%!PS-Adobe-3.1 data_publication_text _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Katharina M. Fromm' _publ_contact_author_address ;Universit\'e de Fribourg D\'epartement de Chimie Chemin du Mus\'ee 8 1700 Fribourg Suisse ; _publ_contact_author_email katharina.fromm@unifr.ch _publ_contact_author_phone ;+41 26 300 87 32 ; _publ_contact_author_fax ;+41 26 300 97 32 ; _publ_author_address ;Universit\'e de Fribourg D\'epartement de Chimie Chemin du Mus\'ee 8 1700 Fribourg Suisse ; loop_ _publ_author_name 'Katharina Fromm' 'Ines Chevrier' 'Jorge L.Sague' 'Priscilla Brunetto' 'Nina Khanna' 'Zarco Rajacic' # Attachment 'compound 4 [Ag(L3i)PF6]24.cif' data_comp4 _database_code_depnum_ccdc_archive 'CCDC 765998' #TrackingRef 'compound 4 [Ag(L3i)PF6]24.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'bisisonicotinate triethyleneglycol' _chemical_melting_point ? _chemical_formula_moiety 'C36 H40 Ag2 N4 O12, (P F6)2' _chemical_formula_sum 'C36 H40 Ag2 F12 N4 O12 P2' _chemical_formula_weight 1226.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7123(17) _cell_length_b 9.806(2) _cell_length_c 14.257(3) _cell_angle_alpha 75.58(3) _cell_angle_beta 79.75(3) _cell_angle_gamma 72.74(3) _cell_volume 1119.4(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour 'yellow grey' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.819 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 612 _exptl_absorpt_coefficient_mu 1.060 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; The absorption correction is low (mu x r is near 1) and with/without absorption correction after a verification in this case does not change the R values. After 45 L.S. the R values are stable. EADP are made on the carbon and oxygen atoms of the ligand for a better anisotropic model of the ligand. Cell measurement_felns_used, cell measurement_theta_min and max are missing because the measure was made in 2004 and lxr and cfx are lost. The R values are high because of a too short time of the measurement which was counted (only one XR machine was accessible for all the departement). ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3709 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.3355 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3709 _reflns_number_gt 1094 _reflns_threshold_expression >2\s(I) _computing_data_collection Xarea _computing_cell_refinement Xarea _computing_data_reduction Xarea _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics diamond _computing_publication_material word _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1433P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3709 _refine_ls_number_parameters 205 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2747 _refine_ls_R_factor_gt 0.1096 _refine_ls_wR_factor_ref 0.3211 _refine_ls_wR_factor_gt 0.2360 _refine_ls_goodness_of_fit_ref 0.823 _refine_ls_restrained_S_all 0.823 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.0530(3) 0.9190(3) 0.73989(12) 0.0718(9) Uani 1 1 d . . . O1 O 0.839(2) 1.0249(19) 0.5848(10) 0.074(4) Uani 1 1 d . . . O2 O 0.6946(17) 1.2229(16) 0.4929(9) 0.054(3) Uani 1 1 d . . . O3 O 0.7910(18) 1.3669(17) 0.2912(9) 0.062(3) Uani 1 1 d . . . O4 O 0.8796(19) 1.3740(17) 0.0920(9) 0.062(3) Uani 1 1 d . . . O5 O -0.7034(17) 0.8064(17) 0.9584(9) 0.054(3) Uani 1 1 d . . . O6 O -0.771(2) 1.046(2) 0.9373(10) 0.074(4) Uani 1 1 d . . . N1 N 0.268(2) 0.985(2) 0.6782(11) 0.063(4) Uani 1 1 d . . . N2 N -0.188(2) 0.917(2) 0.8175(12) 0.063(4) Uani 1 1 d . . . C1 C 0.410(3) 0.883(3) 0.6741(13) 0.055(3) Uani 1 1 d . . . H1 H 0.4127 0.7851 0.6960 0.066 Uiso 1 1 calc R . . C2 C 0.556(3) 0.922(3) 0.6373(12) 0.052(3) Uani 1 1 d . . . H2 H 0.6539 0.8511 0.6409 0.062 Uiso 1 1 calc R . . C3 C 0.553(2) 1.065(3) 0.5961(11) 0.046(4) Uani 1 1 d . . . C4 C 0.406(3) 1.170(3) 0.5911(12) 0.052(3) Uani 1 1 d . . . H4 H 0.4009 1.2665 0.5611 0.062 Uiso 1 1 calc R . . C5 C 0.268(3) 1.127(3) 0.6317(13) 0.055(3) Uani 1 1 d . . . H5 H 0.1696 1.1969 0.6278 0.066 Uiso 1 1 calc R . . C6 C 0.708(3) 1.094(3) 0.5602(14) 0.050(4) Uani 1 1 d . . . C7 C 0.840(3) 1.270(3) 0.4583(12) 0.062(3) Uani 1 1 d . . . H7A H 0.9229 1.1954 0.4306 0.075 Uiso 1 1 calc R . . H7B H 0.8815 1.2880 0.5118 0.075 Uiso 1 1 calc R . . C8 C 0.800(3) 1.409(3) 0.3818(12) 0.062(3) Uani 1 1 d . . . H8A H 0.6980 1.4727 0.4021 0.075 Uiso 1 1 calc R . . H8B H 0.8838 1.4597 0.3719 0.075 Uiso 1 1 calc R . . C9 C 0.749(3) 1.495(3) 0.2188(13) 0.062(3) Uani 1 1 d . . . H9A H 0.8315 1.5472 0.2067 0.075 Uiso 1 1 calc R . . H9B H 0.6475 1.5587 0.2415 0.075 Uiso 1 1 calc R . . C10 C 0.731(3) 1.458(3) 0.1265(13) 0.062(3) Uani 1 1 d . . . H10A H 0.6505 1.4032 0.1387 0.075 Uiso 1 1 calc R . . H10B H 0.6959 1.5463 0.0783 0.075 Uiso 1 1 calc R . . C11 C -0.890(3) 0.660(3) 1.0040(13) 0.062(3) Uani 1 1 d . . . H11A H -0.9961 0.6577 1.0391 0.075 Uiso 1 1 calc R . . H11B H -0.8094 0.5867 1.0414 0.075 Uiso 1 1 calc R . . C12 C -0.866(3) 0.799(3) 0.9935(13) 0.062(3) Uani 1 1 d . . . H12A H -0.8951 0.8277 1.0561 0.075 Uiso 1 1 calc R . . H12B H -0.9379 0.8695 0.9487 0.075 Uiso 1 1 calc R . . C13 C -0.669(3) 0.924(3) 0.9338(14) 0.050(4) Uani 1 1 d . . . C16 C -0.500(2) 0.924(3) 0.8912(11) 0.046(4) Uani 1 1 d . . . C17 C -0.450(3) 1.045(3) 0.8562(12) 0.052(3) Uani 1 1 d . . . H17 H -0.5257 1.1351 0.8556 0.062 Uiso 1 1 calc R . . C18 C -0.294(3) 1.045(3) 0.8214(13) 0.055(3) Uani 1 1 d . . . H18 H -0.2626 1.1319 0.8010 0.066 Uiso 1 1 calc R . . C14 C -0.230(3) 0.792(3) 0.8517(13) 0.055(3) Uani 1 1 d . . . H14 H -0.1524 0.7035 0.8510 0.066 Uiso 1 1 calc R . . C15 C -0.383(3) 0.793(3) 0.8869(12) 0.052(3) Uani 1 1 d . . . H15 H -0.4118 0.7052 0.9087 0.062 Uiso 1 1 calc R . . P1 P 0.7574(9) 0.4501(9) 0.7036(4) 0.065(2) Uani 1 1 d . . . F4 F 0.669(2) 0.361(2) 0.6663(11) 0.135(8) Uani 1 1 d . . . F6 F 0.673(2) 0.394(2) 0.8084(10) 0.132(7) Uani 1 1 d . . . F3 F 0.611(3) 0.578(2) 0.693(2) 0.210(13) Uani 1 1 d . . . F2 F 0.844(3) 0.538(3) 0.7420(15) 0.191(12) Uani 1 1 d . . . F5 F 0.842(3) 0.494(3) 0.6033(13) 0.190(12) Uani 1 1 d . . . F1 F 0.895(2) 0.315(3) 0.7230(19) 0.181(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0692(14) 0.110(2) 0.0434(9) -0.0198(10) 0.0022(8) -0.0363(14) O1 0.068(8) 0.083(10) 0.064(6) -0.021(6) -0.003(6) -0.008(8) O2 0.060(7) 0.060(8) 0.047(5) -0.018(5) 0.004(5) -0.025(7) O3 0.079(8) 0.064(8) 0.043(5) -0.013(5) -0.014(5) -0.012(7) O4 0.079(8) 0.064(8) 0.043(5) -0.013(5) -0.014(5) -0.012(7) O5 0.060(7) 0.060(8) 0.047(5) -0.018(5) 0.004(5) -0.025(7) O6 0.068(8) 0.083(10) 0.064(6) -0.021(6) -0.003(6) -0.008(8) N1 0.077(10) 0.064(12) 0.054(7) -0.008(7) -0.032(7) -0.018(10) N2 0.077(10) 0.064(12) 0.054(7) -0.008(7) -0.032(7) -0.018(10) C1 0.062(8) 0.055(9) 0.046(5) -0.009(6) -0.013(5) -0.010(8) C2 0.062(8) 0.057(9) 0.034(5) -0.007(5) -0.016(5) -0.009(7) C3 0.049(10) 0.067(13) 0.026(6) -0.009(7) -0.011(6) -0.018(10) C4 0.062(8) 0.057(9) 0.034(5) -0.007(5) -0.016(5) -0.009(7) C5 0.062(8) 0.055(9) 0.046(5) -0.009(6) -0.013(5) -0.010(8) C6 0.055(11) 0.045(12) 0.052(8) -0.025(8) -0.009(7) 0.000(10) C7 0.075(7) 0.074(9) 0.035(4) -0.007(5) -0.005(4) -0.019(7) C8 0.075(7) 0.074(9) 0.035(4) -0.007(5) -0.005(4) -0.019(7) C9 0.075(7) 0.074(9) 0.035(4) -0.007(5) -0.005(4) -0.019(7) C10 0.075(7) 0.074(9) 0.035(4) -0.007(5) -0.005(4) -0.019(7) C11 0.075(7) 0.074(9) 0.035(4) -0.007(5) -0.005(4) -0.019(7) C12 0.075(7) 0.074(9) 0.035(4) -0.007(5) -0.005(4) -0.019(7) C13 0.055(11) 0.045(12) 0.052(8) -0.025(8) -0.009(7) 0.000(10) C16 0.049(10) 0.067(13) 0.026(6) -0.009(7) -0.011(6) -0.018(10) C17 0.062(8) 0.057(9) 0.034(5) -0.007(5) -0.016(5) -0.009(7) C18 0.062(8) 0.055(9) 0.046(5) -0.009(6) -0.013(5) -0.010(8) C14 0.062(8) 0.055(9) 0.046(5) -0.009(6) -0.013(5) -0.010(8) C15 0.062(8) 0.057(9) 0.034(5) -0.007(5) -0.016(5) -0.009(7) P1 0.066(5) 0.064(6) 0.067(4) -0.028(4) -0.008(3) -0.009(5) F4 0.178(18) 0.19(2) 0.085(10) -0.055(11) 0.021(11) -0.115(17) F6 0.146(16) 0.21(2) 0.064(9) -0.062(11) 0.017(9) -0.072(16) F3 0.13(2) 0.076(16) 0.36(4) 0.00(2) -0.04(2) 0.032(16) F2 0.19(2) 0.30(3) 0.174(17) -0.19(2) 0.071(15) -0.15(2) F5 0.29(3) 0.25(3) 0.084(12) -0.025(14) 0.018(15) -0.18(3) F1 0.092(15) 0.13(2) 0.26(3) -0.007(19) -0.001(16) 0.026(16) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.129(19) . ? Ag1 N2 2.20(2) . ? O1 C6 1.20(2) . ? O2 C6 1.37(2) . ? O2 C7 1.45(2) . ? O3 C9 1.41(2) . ? O3 C8 1.47(2) . ? O4 C10 1.39(3) . ? O4 C11 1.47(2) 2_576 ? O5 C13 1.22(2) . ? O5 C12 1.43(2) . ? O6 C13 1.27(2) . ? N1 C1 1.34(3) . ? N1 C5 1.39(3) . ? N2 C14 1.34(3) . ? N2 C18 1.33(3) . ? C1 C2 1.41(3) . ? C1 H1 0.9300 . ? C2 C3 1.37(3) . ? C2 H2 0.9300 . ? C3 C4 1.38(3) . ? C3 C6 1.44(3) . ? C4 C5 1.37(3) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C7 C8 1.51(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.50(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.41(3) . ? C11 O4 1.47(2) 2_576 ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C16 1.50(3) . ? C16 C17 1.34(3) . ? C16 C15 1.39(3) . ? C17 C18 1.36(3) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C14 C15 1.34(3) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? P1 F5 1.510(18) . ? P1 F3 1.50(2) . ? P1 F1 1.51(2) . ? P1 F2 1.547(17) . ? P1 F4 1.558(16) . ? P1 F6 1.585(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N2 162.0(8) . . ? C6 O2 C7 117.0(17) . . ? C9 O3 C8 108.5(16) . . ? C10 O4 C11 116.6(15) . 2_576 ? C13 O5 C12 121(2) . . ? C1 N1 C5 117(2) . . ? C1 N1 Ag1 119.6(15) . . ? C5 N1 Ag1 123.5(17) . . ? C14 N2 C18 122(2) . . ? C14 N2 Ag1 120.8(18) . . ? C18 N2 Ag1 117.4(15) . . ? N1 C1 C2 121(2) . . ? N1 C1 H1 119.3 . . ? C2 C1 H1 119.3 . . ? C3 C2 C1 120(2) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 119(2) . . ? C2 C3 C6 116(2) . . ? C4 C3 C6 125(2) . . ? C5 C4 C3 118(2) . . ? C5 C4 H4 121.0 . . ? C3 C4 H4 121.0 . . ? C4 C5 N1 124(2) . . ? C4 C5 H5 118.0 . . ? N1 C5 H5 118.0 . . ? O1 C6 O2 119(2) . . ? O1 C6 C3 129(2) . . ? O2 C6 C3 112(2) . . ? O2 C7 C8 108.2(18) . . ? O2 C7 H7A 110.0 . . ? C8 C7 H7A 110.0 . . ? O2 C7 H7B 110.0 . . ? C8 C7 H7B 110.0 . . ? H7A C7 H7B 108.4 . . ? O3 C8 C7 107.3(18) . . ? O3 C8 H8A 110.2 . . ? C7 C8 H8A 110.2 . . ? O3 C8 H8B 110.2 . . ? C7 C8 H8B 110.2 . . ? H8A C8 H8B 108.5 . . ? O3 C9 C10 110.2(19) . . ? O3 C9 H9A 109.6 . . ? C10 C9 H9A 109.6 . . ? O3 C9 H9B 109.6 . . ? C10 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? O4 C10 C9 108.8(18) . . ? O4 C10 H10A 109.9 . . ? C9 C10 H10A 109.9 . . ? O4 C10 H10B 109.9 . . ? C9 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? C12 C11 O4 110.3(16) . 2_576 ? C12 C11 H11A 109.6 . . ? O4 C11 H11A 109.6 2_576 . ? C12 C11 H11B 109.6 . . ? O4 C11 H11B 109.6 2_576 . ? H11A C11 H11B 108.1 . . ? C11 C12 O5 114(2) . . ? C11 C12 H12A 108.8 . . ? O5 C12 H12A 108.8 . . ? C11 C12 H12B 108.8 . . ? O5 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? O5 C13 O6 124(2) . . ? O5 C13 C16 118(2) . . ? O6 C13 C16 118(2) . . ? C17 C16 C15 116(2) . . ? C17 C16 C13 124(2) . . ? C15 C16 C13 120(2) . . ? C18 C17 C16 124(2) . . ? C18 C17 H17 118.1 . . ? C16 C17 H17 118.1 . . ? N2 C18 C17 118(2) . . ? N2 C18 H18 121.2 . . ? C17 C18 H18 121.2 . . ? N2 C14 C15 120(3) . . ? N2 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C14 C15 C16 120(2) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? F5 P1 F3 95.8(17) . . ? F5 P1 F1 89.7(15) . . ? F3 P1 F1 174.3(15) . . ? F5 P1 F2 88.5(11) . . ? F3 P1 F2 90.3(16) . . ? F1 P1 F2 91.3(15) . . ? F5 P1 F4 92.3(10) . . ? F3 P1 F4 89.5(14) . . ? F1 P1 F4 88.8(14) . . ? F2 P1 F4 179.2(10) . . ? F5 P1 F6 176.7(14) . . ? F3 P1 F6 86.9(14) . . ? F1 P1 F6 87.5(12) . . ? F2 P1 F6 93.4(10) . . ? F4 P1 F6 85.8(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ag1 N1 C1 146.7(19) . . . . ? N2 Ag1 N1 C5 -40(3) . . . . ? N1 Ag1 N2 C14 -158.5(18) . . . . ? N1 Ag1 N2 C18 27(3) . . . . ? C5 N1 C1 C2 9(3) . . . . ? Ag1 N1 C1 C2 -177.6(13) . . . . ? N1 C1 C2 C3 -6(3) . . . . ? C1 C2 C3 C4 0(3) . . . . ? C1 C2 C3 C6 -179.8(16) . . . . ? C2 C3 C4 C5 3(3) . . . . ? C6 C3 C4 C5 -177.6(16) . . . . ? C3 C4 C5 N1 1(3) . . . . ? C1 N1 C5 C4 -6(3) . . . . ? Ag1 N1 C5 C4 -179.5(14) . . . . ? C7 O2 C6 O1 -2(3) . . . . ? C7 O2 C6 C3 174.5(16) . . . . ? C2 C3 C6 O1 -24(3) . . . . ? C4 C3 C6 O1 156(2) . . . . ? C2 C3 C6 O2 159.5(15) . . . . ? C4 C3 C6 O2 -20(3) . . . . ? C6 O2 C7 C8 177.0(16) . . . . ? C9 O3 C8 C7 178.2(18) . . . . ? O2 C7 C8 O3 -78(2) . . . . ? C8 O3 C9 C10 -177.7(18) . . . . ? C11 O4 C10 C9 -173.5(17) 2_576 . . . ? O3 C9 C10 O4 -63(2) . . . . ? O4 C11 C12 O5 -70(2) 2_576 . . . ? C13 O5 C12 C11 170.3(17) . . . . ? C12 O5 C13 O6 0(3) . . . . ? C12 O5 C13 C16 -175.7(14) . . . . ? O5 C13 C16 C17 175.9(17) . . . . ? O6 C13 C16 C17 -1(3) . . . . ? O5 C13 C16 C15 -4(2) . . . . ? O6 C13 C16 C15 179.0(16) . . . . ? C15 C16 C17 C18 -3(3) . . . . ? C13 C16 C17 C18 177.1(17) . . . . ? C14 N2 C18 C17 -4(3) . . . . ? Ag1 N2 C18 C17 170.4(12) . . . . ? C16 C17 C18 N2 4(3) . . . . ? C18 N2 C14 C15 3(3) . . . . ? Ag1 N2 C14 C15 -170.9(13) . . . . ? N2 C14 C15 C16 -2(3) . . . . ? C17 C16 C15 C14 2(2) . . . . ? C13 C16 C15 C14 -178.0(16) . . . . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 1.157 _refine_diff_density_min -1.291 _refine_diff_density_rms 0.161 data_l3iagno3 _database_code_depnum_ccdc_archive 'CCDC 849905' #TrackingRef 'compound 1 [{Ag(L3i)]NO3}(H2O)2]4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'bisisonicotinate triethyleneglycol' _chemical_melting_point ? _chemical_formula_moiety 'C18 H20 Ag1 N2 O6, N O3, 2(H2 O)' _chemical_formula_sum 'C18 H24 Ag1 N3 O11' _chemical_formula_weight 566.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8970 1.1020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1377(18) _cell_length_b 10.794(2) _cell_length_c 11.988(2) _cell_angle_alpha 100.062(15) _cell_angle_beta 107.033(15) _cell_angle_gamma 99.711(15) _cell_volume 1082.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 13382 _cell_measurement_theta_min 1.82 _cell_measurement_theta_max 27.19 _exptl_crystal_description bloc _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.737 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 0.985 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.887 _exptl_absorpt_correction_T_max 0.951 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22829 _diffrn_reflns_av_R_equivalents 0.1485 _diffrn_reflns_av_sigmaI/netI 0.0767 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 26.71 _reflns_number_total 4584 _reflns_number_gt 4070 _reflns_threshold_expression >2\s(I) _computing_data_collection Xarea _computing_cell_refinement Xarea _computing_data_reduction Xarea _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics diamond _computing_publication_material word _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. 3 restraints were given (two DFIX for H11A O11 and H11B O11 and one DANG for H11A H11B) to improve the molecule of water. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1026P)^2^+0.2873P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4584 _refine_ls_number_parameters 304 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0653 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.1561 _refine_ls_wR_factor_gt 0.1517 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.71217(3) 0.26282(3) 0.73150(3) 0.04495(15) Uani 1 1 d . . . O3 O 0.3489(3) 0.7120(3) 0.0387(3) 0.0430(6) Uani 1 1 d . . . O2 O 0.5972(3) 0.8095(3) 0.2580(3) 0.0414(6) Uani 1 1 d . . . O4 O 0.0380(3) 0.7443(3) -0.0837(3) 0.0395(6) Uani 1 1 d . . . O5 O -0.1967(3) 0.6918(3) -0.0576(3) 0.0474(7) Uani 1 1 d . . . O1 O 0.6892(3) 0.8251(3) 0.5133(3) 0.0444(6) Uani 1 1 d . . . O6 O 0.4650(4) 0.8190(4) 0.5566(4) 0.0650(10) Uani 1 1 d . . . N1 N 0.6685(4) 0.4433(3) 0.6868(3) 0.0411(7) Uani 1 1 d . . . N2 N -0.2227(4) 1.0911(3) -0.2169(3) 0.0414(7) Uani 1 1 d . . . C8 C 0.4989(4) 0.6821(4) 0.0568(4) 0.0413(8) Uani 1 1 d . . . H8A H 0.5191 0.6667 -0.0189 0.050 Uiso 1 1 calc R . . H8B H 0.4998 0.6040 0.0863 0.050 Uiso 1 1 calc R . . C7 C 0.6247(4) 0.7920(4) 0.1458(4) 0.0442(9) Uani 1 1 d . . . H7A H 0.7273 0.7732 0.1556 0.053 Uiso 1 1 calc R . . H7B H 0.6231 0.8706 0.1171 0.053 Uiso 1 1 calc R . . C11 C -0.1036(4) 0.7635(4) -0.0873(3) 0.0368(8) Uani 1 1 d . . . C12 C -0.1393(4) 0.8790(4) -0.1318(3) 0.0358(7) Uani 1 1 d . . . C1 C 0.7744(5) 0.5150(4) 0.6523(4) 0.0426(9) Uani 1 1 d . . . H1 H 0.8677 0.4894 0.6565 0.051 Uiso 1 1 calc R . . C2 C 0.7532(4) 0.6239(4) 0.6112(4) 0.0427(9) Uani 1 1 d . . . H2 H 0.8288 0.6695 0.5865 0.051 Uiso 1 1 calc R . . C3 C 0.6149(4) 0.6644(3) 0.6076(3) 0.0348(7) Uani 1 1 d . . . C17 C 0.5062(4) 0.5940(4) 0.6464(4) 0.0401(8) Uani 1 1 d . . . H17 H 0.4144 0.6202 0.6468 0.048 Uiso 1 1 calc R . . C18 C 0.5360(4) 0.4850(4) 0.6843(4) 0.0425(9) Uani 1 1 d . . . H18 H 0.4619 0.4377 0.7093 0.051 Uiso 1 1 calc R . . C14 C -0.0855(4) 1.0585(4) -0.2158(4) 0.0421(8) Uani 1 1 d . . . H14 H -0.0187 1.1088 -0.2447 0.050 Uiso 1 1 calc R . . C13 C -0.0396(4) 0.9557(4) -0.1747(4) 0.0399(8) Uani 1 1 d . . . H13 H 0.0560 0.9374 -0.1753 0.048 Uiso 1 1 calc R . . C15 C -0.3174(4) 1.0154(4) -0.1752(4) 0.0414(8) Uani 1 1 d . . . H15 H -0.4129 1.0350 -0.1758 0.050 Uiso 1 1 calc R . . C16 C -0.2803(4) 0.9114(4) -0.1323(4) 0.0414(8) Uani 1 1 d . . . H16 H -0.3488 0.8626 -0.1037 0.050 Uiso 1 1 calc R . . C4 C 0.5793(4) 0.7778(4) 0.5580(4) 0.0408(8) Uani 1 1 d . . . C5 C 0.6690(5) 0.9331(4) 0.4589(4) 0.0454(9) Uani 1 1 d . . . H5A H 0.7347 1.0130 0.5147 0.054 Uiso 1 1 calc R . . H5B H 0.5602 0.9397 0.4382 0.054 Uiso 1 1 calc R . . C9 C 0.2270(5) 0.6097(4) -0.0486(4) 0.0453(9) Uani 1 1 d . . . H9A H 0.2409 0.5269 -0.0317 0.054 Uiso 1 1 calc R . . H9B H 0.2327 0.6096 -0.1281 0.054 Uiso 1 1 calc R . . C6 C 0.7148(4) 0.9115(4) 0.3480(4) 0.0418(8) Uani 1 1 d . . . H6A H 0.7239 0.9901 0.3193 0.050 Uiso 1 1 calc R . . H6B H 0.8159 0.8885 0.3660 0.050 Uiso 1 1 calc R . . C10 C 0.0694(5) 0.6287(4) -0.0445(4) 0.0443(9) Uani 1 1 d . . . H10A H -0.0121 0.5539 -0.0960 0.053 Uiso 1 1 calc R . . H10B H 0.0676 0.6362 0.0369 0.053 Uiso 1 1 calc R . . O7 O -0.0515(5) 0.2390(4) 0.5756(4) 0.0773(11) Uani 1 1 d . . . O8 O 0.1208(5) 0.4182(4) 0.6183(4) 0.0796(12) Uani 1 1 d . . . O9 O 0.0507(4) 0.3482(4) 0.7579(3) 0.0634(9) Uani 1 1 d . . . N3 N 0.0414(4) 0.3351(4) 0.6505(4) 0.0498(9) Uani 1 1 d . . . O10 O 0.8463(5) 0.3054(4) 0.3450(4) 0.0718(10) Uani 1 1 d . . . O11 O 0.6483(4) 0.1179(4) 0.1395(4) 0.0623(9) Uani 1 1 d D . . H12A H 0.8588 0.2912 0.4149 0.050 Uiso 1 1 d . . . H12B H 0.8618 0.3890 0.3556 0.050 Uiso 1 1 d . . . H11A H 0.717(5) 0.175(4) 0.200(2) 0.050 Uiso 1 1 d D . . H11B H 0.655(5) 0.144(4) 0.077(2) 0.050 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0409(2) 0.0368(2) 0.0560(2) 0.01348(15) 0.01294(15) 0.00921(13) O3 0.0325(13) 0.0387(14) 0.0525(16) 0.0052(12) 0.0117(11) 0.0047(10) O2 0.0322(12) 0.0418(14) 0.0472(15) 0.0068(12) 0.0151(11) 0.0011(11) O4 0.0302(12) 0.0370(14) 0.0535(16) 0.0153(12) 0.0156(11) 0.0062(10) O5 0.0395(14) 0.0453(16) 0.0660(19) 0.0230(14) 0.0257(14) 0.0076(12) O1 0.0442(14) 0.0431(15) 0.0540(17) 0.0196(13) 0.0224(13) 0.0124(12) O6 0.0503(18) 0.057(2) 0.108(3) 0.038(2) 0.040(2) 0.0240(16) N1 0.0353(15) 0.0398(17) 0.0492(19) 0.0121(14) 0.0138(14) 0.0101(13) N2 0.0327(15) 0.0419(18) 0.052(2) 0.0108(15) 0.0178(14) 0.0087(13) C8 0.0338(17) 0.041(2) 0.049(2) 0.0051(17) 0.0176(16) 0.0084(15) C7 0.0313(17) 0.052(2) 0.049(2) 0.0071(18) 0.0180(16) 0.0082(16) C11 0.0299(16) 0.0386(19) 0.040(2) 0.0085(15) 0.0125(14) 0.0030(14) C12 0.0320(16) 0.0328(17) 0.042(2) 0.0085(15) 0.0137(14) 0.0030(13) C1 0.0340(18) 0.040(2) 0.058(2) 0.0156(18) 0.0171(16) 0.0110(15) C2 0.0333(18) 0.042(2) 0.055(2) 0.0129(18) 0.0179(16) 0.0078(15) C3 0.0323(16) 0.0287(17) 0.0410(19) 0.0053(14) 0.0114(14) 0.0052(13) C17 0.0305(17) 0.040(2) 0.050(2) 0.0096(16) 0.0148(15) 0.0059(14) C18 0.0347(18) 0.039(2) 0.051(2) 0.0059(17) 0.0147(16) 0.0040(15) C14 0.0345(17) 0.041(2) 0.055(2) 0.0150(18) 0.0199(16) 0.0082(15) C13 0.0278(16) 0.043(2) 0.052(2) 0.0144(17) 0.0174(15) 0.0049(14) C15 0.0302(17) 0.040(2) 0.056(2) 0.0102(17) 0.0174(16) 0.0080(14) C16 0.0339(18) 0.041(2) 0.052(2) 0.0110(17) 0.0207(16) 0.0034(15) C4 0.0351(18) 0.0359(19) 0.049(2) 0.0057(16) 0.0147(16) 0.0060(14) C5 0.051(2) 0.0353(19) 0.049(2) 0.0098(17) 0.0168(18) 0.0106(16) C9 0.042(2) 0.039(2) 0.050(2) 0.0057(17) 0.0122(17) 0.0061(16) C6 0.0350(17) 0.0384(19) 0.049(2) 0.0104(16) 0.0131(15) 0.0018(14) C10 0.0342(18) 0.039(2) 0.055(2) 0.0148(18) 0.0100(16) 0.0024(15) O7 0.079(3) 0.064(2) 0.067(2) 0.0129(19) 0.0043(19) -0.0063(19) O8 0.074(2) 0.071(2) 0.107(3) 0.023(2) 0.058(2) 0.0004(19) O9 0.066(2) 0.056(2) 0.067(2) 0.0135(17) 0.0243(17) 0.0083(16) N3 0.0387(17) 0.0427(19) 0.074(3) 0.0179(18) 0.0226(17) 0.0131(14) O10 0.059(2) 0.083(3) 0.064(2) 0.013(2) 0.0184(17) 0.0018(18) O11 0.058(2) 0.057(2) 0.073(2) 0.0193(18) 0.0260(18) 0.0016(15) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.175(4) 1_646 ? Ag1 N1 2.178(4) . ? O3 C8 1.424(4) . ? O3 C9 1.433(5) . ? O2 C7 1.426(5) . ? O2 C6 1.427(5) . ? O4 C11 1.334(4) . ? O4 C10 1.452(5) . ? O5 C11 1.225(4) . ? O1 C4 1.339(5) . ? O1 C5 1.445(5) . ? O6 C4 1.199(5) . ? N1 C1 1.341(5) . ? N1 C18 1.355(5) . ? N2 C15 1.351(5) . ? N2 C14 1.355(5) . ? N2 Ag1 2.175(4) 1_464 ? C8 C7 1.499(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C11 C12 1.487(5) . ? C12 C16 1.389(5) . ? C12 C13 1.396(5) . ? C1 C2 1.373(6) . ? C1 H1 0.9300 . ? C2 C3 1.397(5) . ? C2 H2 0.9300 . ? C3 C17 1.386(5) . ? C3 C4 1.494(6) . ? C17 C18 1.373(6) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C14 C13 1.371(6) . ? C14 H14 0.9300 . ? C13 H13 0.9300 . ? C15 C16 1.367(6) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C5 C6 1.499(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C9 C10 1.502(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? O7 N3 1.239(5) . ? O8 N3 1.244(5) . ? O9 N3 1.246(5) . ? O10 H12A 0.857(4) . ? O10 H12B 0.870(5) . ? O11 H11A 0.866(19) . ? O11 H11B 0.866(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N1 175.01(11) 1_646 . ? C8 O3 C9 110.9(3) . . ? C7 O2 C6 112.0(3) . . ? C11 O4 C10 113.7(3) . . ? C4 O1 C5 118.0(3) . . ? C1 N1 C18 117.1(4) . . ? C1 N1 Ag1 118.5(3) . . ? C18 N1 Ag1 124.3(3) . . ? C15 N2 C14 116.5(4) . . ? C15 N2 Ag1 119.4(2) . 1_464 ? C14 N2 Ag1 124.0(3) . 1_464 ? O3 C8 C7 109.9(3) . . ? O3 C8 H8A 109.7 . . ? C7 C8 H8A 109.7 . . ? O3 C8 H8B 109.7 . . ? C7 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? O2 C7 C8 109.0(3) . . ? O2 C7 H7A 109.9 . . ? C8 C7 H7A 109.9 . . ? O2 C7 H7B 109.9 . . ? C8 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? O5 C11 O4 123.1(4) . . ? O5 C11 C12 122.9(3) . . ? O4 C11 C12 114.1(3) . . ? C16 C12 C13 118.1(4) . . ? C16 C12 C11 118.4(3) . . ? C13 C12 C11 123.5(3) . . ? N1 C1 C2 123.8(3) . . ? N1 C1 H1 118.1 . . ? C2 C1 H1 118.1 . . ? C1 C2 C3 118.2(3) . . ? C1 C2 H2 120.9 . . ? C3 C2 H2 120.9 . . ? C17 C3 C2 118.8(4) . . ? C17 C3 C4 119.8(3) . . ? C2 C3 C4 121.4(3) . . ? C18 C17 C3 119.0(3) . . ? C18 C17 H17 120.5 . . ? C3 C17 H17 120.5 . . ? N1 C18 C17 123.0(4) . . ? N1 C18 H18 118.5 . . ? C17 C18 H18 118.5 . . ? N2 C14 C13 123.8(3) . . ? N2 C14 H14 118.1 . . ? C13 C14 H14 118.1 . . ? C14 C13 C12 118.7(3) . . ? C14 C13 H13 120.7 . . ? C12 C13 H13 120.7 . . ? N2 C15 C16 123.4(3) . . ? N2 C15 H15 118.3 . . ? C16 C15 H15 118.3 . . ? C15 C16 C12 119.5(3) . . ? C15 C16 H16 120.3 . . ? C12 C16 H16 120.3 . . ? O6 C4 O1 124.7(4) . . ? O6 C4 C3 123.9(4) . . ? O1 C4 C3 111.4(3) . . ? O1 C5 C6 108.3(3) . . ? O1 C5 H5A 110.0 . . ? C6 C5 H5A 110.0 . . ? O1 C5 H5B 110.0 . . ? C6 C5 H5B 110.0 . . ? H5A C5 H5B 108.4 . . ? O3 C9 C10 109.5(3) . . ? O3 C9 H9A 109.8 . . ? C10 C9 H9A 109.8 . . ? O3 C9 H9B 109.8 . . ? C10 C9 H9B 109.8 . . ? H9A C9 H9B 108.2 . . ? O2 C6 C5 108.9(3) . . ? O2 C6 H6A 109.9 . . ? C5 C6 H6A 109.9 . . ? O2 C6 H6B 109.9 . . ? C5 C6 H6B 109.9 . . ? H6A C6 H6B 108.3 . . ? O4 C10 C9 110.7(3) . . ? O4 C10 H10A 109.5 . . ? C9 C10 H10A 109.5 . . ? O4 C10 H10B 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? O7 N3 O8 120.3(5) . . ? O7 N3 O9 118.8(4) . . ? O8 N3 O9 120.9(4) . . ? H12A O10 H12B 105.3(4) . . ? H11A O11 H11B 105(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ag1 N1 C1 37.7(15) 1_646 . . . ? N2 Ag1 N1 C18 -146.5(12) 1_646 . . . ? C9 O3 C8 C7 178.4(3) . . . . ? C6 O2 C7 C8 178.9(3) . . . . ? O3 C8 C7 O2 61.9(4) . . . . ? C10 O4 C11 O5 1.6(5) . . . . ? C10 O4 C11 C12 -177.8(3) . . . . ? O5 C11 C12 C16 4.2(6) . . . . ? O4 C11 C12 C16 -176.3(4) . . . . ? O5 C11 C12 C13 -174.8(4) . . . . ? O4 C11 C12 C13 4.6(5) . . . . ? C18 N1 C1 C2 -2.4(6) . . . . ? Ag1 N1 C1 C2 173.7(3) . . . . ? N1 C1 C2 C3 1.5(7) . . . . ? C1 C2 C3 C17 0.6(6) . . . . ? C1 C2 C3 C4 -176.8(4) . . . . ? C2 C3 C17 C18 -1.7(6) . . . . ? C4 C3 C17 C18 175.7(4) . . . . ? C1 N1 C18 C17 1.2(6) . . . . ? Ag1 N1 C18 C17 -174.6(3) . . . . ? C3 C17 C18 N1 0.8(6) . . . . ? C15 N2 C14 C13 -0.5(6) . . . . ? Ag1 N2 C14 C13 174.9(3) 1_464 . . . ? N2 C14 C13 C12 0.4(7) . . . . ? C16 C12 C13 C14 -0.4(6) . . . . ? C11 C12 C13 C14 178.7(4) . . . . ? C14 N2 C15 C16 0.7(6) . . . . ? Ag1 N2 C15 C16 -174.9(3) 1_464 . . . ? N2 C15 C16 C12 -0.7(7) . . . . ? C13 C12 C16 C15 0.5(6) . . . . ? C11 C12 C16 C15 -178.5(4) . . . . ? C5 O1 C4 O6 -0.2(6) . . . . ? C5 O1 C4 C3 178.3(3) . . . . ? C17 C3 C4 O6 5.3(6) . . . . ? C2 C3 C4 O6 -177.4(5) . . . . ? C17 C3 C4 O1 -173.3(4) . . . . ? C2 C3 C4 O1 4.1(5) . . . . ? C4 O1 C5 C6 -139.2(4) . . . . ? C8 O3 C9 C10 166.7(3) . . . . ? C7 O2 C6 C5 174.2(3) . . . . ? O1 C5 C6 O2 71.6(4) . . . . ? C11 O4 C10 C9 177.1(3) . . . . ? O3 C9 C10 O4 66.4(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O10 H12A O7 0.857(4) 2.076(4) 2.904(6) 162.4(3) 1_655 O10 H12B O8 0.870(5) 2.021(4) 2.888(6) 175.0(3) 2_666 O11 H11A O10 0.866(19) 1.94(2) 2.802(5) 171(5) . O11 H11B O3 0.866(18) 2.25(3) 3.052(5) 155(4) 2_665 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.71 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.676 _refine_diff_density_min -2.073 _refine_diff_density_rms 0.149 # Attachment 'compound 5 [Ag(L3n)NO3]4.cif' data_280810 _database_code_depnum_ccdc_archive 'CCDC 849908' #TrackingRef 'compound 5 [Ag(L3n)NO3]4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; L3nAgNO3 11 ; _chemical_name_common 'L3nAgNO3 11' _chemical_melting_point ? _chemical_formula_moiety 'C18 H20 Ag N3 O9' _chemical_formula_sum 'C18 H20 Ag N3 O9' _chemical_formula_weight 530.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.0308(16) _cell_length_b 13.192(2) _cell_length_c 20.531(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.866(16) _cell_angle_gamma 90.00 _cell_volume 2128.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 4788 _cell_measurement_theta_min 1.85 _cell_measurement_theta_max 27.33 _exptl_crystal_description diamond _exptl_crystal_colour white _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.655 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 1.002 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.58963 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20319 _diffrn_reflns_av_R_equivalents 0.1256 _diffrn_reflns_av_sigmaI/netI 0.0929 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 27.33 _reflns_number_total 4788 _reflns_number_gt 2979 _reflns_threshold_expression >2\s(I) _computing_data_collection Xarea _computing_cell_refinement Xarea _computing_data_reduction Xarea _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics diamond _computing_publication_material word _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0621P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4788 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1004 _refine_ls_R_factor_gt 0.0591 _refine_ls_wR_factor_ref 0.1272 _refine_ls_wR_factor_gt 0.1137 _refine_ls_goodness_of_fit_ref 0.939 _refine_ls_restrained_S_all 0.939 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 1.13394(4) 0.00819(3) 0.066634(18) 0.04914(14) Uani 1 1 d . . . O8 O 1.0534(7) 0.1710(4) 0.1279(2) 0.1028(17) Uani 1 1 d . . . O7 O 0.9179(5) 0.1708(3) 0.0283(2) 0.0787(12) Uani 1 1 d . . . O9 O 0.9228(8) 0.3039(3) 0.0891(3) 0.1190(19) Uani 1 1 d . . . O5 O 0.8401(4) -0.3676(2) 0.07673(18) 0.0543(8) Uani 1 1 d . . . O4 O 0.6287(4) -0.4152(2) -0.05707(17) 0.0551(8) Uani 1 1 d . . . O3 O 0.4949(5) -0.2717(3) -0.16977(19) 0.0680(10) Uani 1 1 d . . . O2 O 0.3909(5) -0.0625(3) -0.15910(18) 0.0663(10) Uani 1 1 d . . . O1 O 0.5357(7) 0.0693(4) -0.1872(2) 0.0974(16) Uani 1 1 d . . . O6 O 0.7855(8) -0.4048(3) 0.1754(2) 0.1082(19) Uani 1 1 d . . . N3 N 0.9629(6) 0.2181(3) 0.0804(3) 0.0595(11) Uani 1 1 d . . . N2 N 1.0455(5) -0.0932(3) 0.13635(19) 0.0448(9) Uani 1 1 d . . . N1 N 1.2927(4) 0.0782(3) 0.00472(18) 0.0400(8) Uani 1 1 d . . . C18 C 0.9838(5) -0.1863(3) 0.1187(2) 0.0446(10) Uani 1 1 d . . . H20 H 0.9894 -0.2111 0.0768 0.054 Uiso 1 1 calc R . . C14 C 0.9117(6) -0.2468(3) 0.1615(2) 0.0472(11) Uani 1 1 d . . . C13 C 0.8395(7) -0.3478(4) 0.1388(3) 0.0596(14) Uani 1 1 d . . . C12 C 0.7710(8) -0.4650(4) 0.0507(3) 0.0630(14) Uani 1 1 d . . . H15 H 0.6563 -0.4729 0.0582 0.076 Uiso 1 1 calc R . . H16 H 0.8403 -0.5195 0.0736 0.076 Uiso 1 1 calc R . . C11 C 0.7686(7) -0.4703(4) -0.0215(3) 0.0650(14) Uani 1 1 d . . . H13 H 0.8735 -0.4424 -0.0303 0.078 Uiso 1 1 calc R . . H14 H 0.7604 -0.5405 -0.0359 0.078 Uiso 1 1 calc R . . C10 C 0.6042(8) -0.4301(4) -0.1258(3) 0.0685(15) Uani 1 1 d . . . H11 H 0.5892 -0.5019 -0.1356 0.082 Uiso 1 1 calc R . . H12 H 0.7044 -0.4075 -0.1413 0.082 Uiso 1 1 calc R . . C9 C 0.4522(8) -0.3734(4) -0.1619(3) 0.0679(15) Uani 1 1 d . . . H9 H 0.4111 -0.4039 -0.2052 0.082 Uiso 1 1 calc R . . H10 H 0.3620 -0.3772 -0.1370 0.082 Uiso 1 1 calc R . . C8 C 0.3628(9) -0.2209(4) -0.2131(3) 0.0752(17) Uani 1 1 d . . . H8 H 0.2592 -0.2244 -0.1959 0.090 Uiso 1 1 calc R . . H7 H 0.3416 -0.2532 -0.2565 0.090 Uiso 1 1 calc R . . C7 C 0.4107(11) -0.1146(5) -0.2195(3) 0.086(2) Uani 1 1 d . . . H6 H 0.5277 -0.1102 -0.2248 0.104 Uiso 1 1 calc R . . H5 H 0.3380 -0.0840 -0.2580 0.104 Uiso 1 1 calc R . . C6 C 0.4579(7) 0.0293(4) -0.1501(3) 0.0560(13) Uani 1 1 d . . . C2 C 0.4284(5) 0.0771(3) -0.0881(2) 0.0424(10) Uani 1 1 d . . . C1 C 1.3224(5) 0.0342(3) -0.0509(2) 0.0384(9) Uani 1 1 d . . . H1 H 1.2696 -0.0271 -0.0646 0.046 Uiso 1 1 calc R . . C5 C 1.3691(6) 0.1667(3) 0.0243(2) 0.0476(11) Uani 1 1 d . . . H4 H 1.3474 0.1983 0.0622 0.057 Uiso 1 1 calc R . . C4 C 1.4790(6) 0.2119(4) -0.0104(3) 0.0571(14) Uani 1 1 d . . . H3 H 1.5322 0.2725 0.0048 0.069 Uiso 1 1 calc R . . C3 C 0.5095(6) 0.1681(4) -0.0664(3) 0.0568(13) Uani 1 1 d . . . H2 H 0.5833 0.1983 -0.0901 0.068 Uiso 1 1 calc R . . C15 C 0.9067(7) -0.2101(4) 0.2239(3) 0.0590(13) Uani 1 1 d . . . H17 H 0.8600 -0.2490 0.2534 0.071 Uiso 1 1 calc R . . C16 C 0.9708(7) -0.1167(4) 0.2418(3) 0.0607(14) Uani 1 1 d . . . H18 H 0.9699 -0.0914 0.2840 0.073 Uiso 1 1 calc R . . C17 C 1.0372(6) -0.0595(4) 0.1968(2) 0.0519(12) Uani 1 1 d . . . H19 H 1.0779 0.0051 0.2093 0.062 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0543(2) 0.0509(2) 0.0448(2) 0.00254(19) 0.01620(14) -0.00289(18) O8 0.155(5) 0.089(3) 0.064(3) -0.007(3) 0.022(3) 0.038(3) O7 0.080(3) 0.091(3) 0.068(3) -0.024(2) 0.021(2) -0.002(2) O9 0.175(5) 0.040(2) 0.157(5) -0.002(3) 0.071(4) 0.023(3) O5 0.068(2) 0.0436(18) 0.050(2) 0.0054(15) 0.0105(17) -0.0032(15) O4 0.068(2) 0.0491(19) 0.048(2) -0.0053(15) 0.0132(16) 0.0087(16) O3 0.094(3) 0.056(2) 0.051(2) -0.0030(18) 0.007(2) -0.0051(19) O2 0.107(3) 0.051(2) 0.047(2) 0.0008(17) 0.032(2) 0.0058(19) O1 0.131(4) 0.112(4) 0.067(3) -0.007(3) 0.062(3) -0.033(3) O6 0.190(5) 0.073(3) 0.063(3) 0.009(2) 0.027(3) -0.053(3) N3 0.076(3) 0.041(2) 0.072(3) -0.003(2) 0.039(3) 0.004(2) N2 0.049(2) 0.047(2) 0.037(2) -0.0008(17) 0.0051(17) 0.0044(16) N1 0.0441(19) 0.0396(19) 0.036(2) 0.0022(16) 0.0069(16) 0.0052(15) C18 0.047(2) 0.045(2) 0.041(3) 0.003(2) 0.006(2) 0.0045(19) C14 0.051(2) 0.046(2) 0.041(3) 0.014(2) 0.003(2) 0.004(2) C13 0.080(4) 0.050(3) 0.047(3) 0.018(2) 0.008(3) -0.003(2) C12 0.079(3) 0.038(2) 0.067(4) 0.003(2) 0.004(3) 0.000(2) C11 0.079(4) 0.047(3) 0.070(4) -0.006(3) 0.017(3) 0.011(2) C10 0.095(4) 0.061(3) 0.054(3) -0.013(3) 0.028(3) 0.008(3) C9 0.097(4) 0.064(3) 0.042(3) -0.009(3) 0.011(3) -0.011(3) C8 0.106(5) 0.071(4) 0.046(3) -0.011(3) 0.008(3) 0.000(3) C7 0.155(6) 0.066(4) 0.044(3) 0.003(3) 0.035(4) 0.021(4) C6 0.062(3) 0.063(3) 0.045(3) 0.005(2) 0.015(2) 0.012(2) C2 0.041(2) 0.043(2) 0.045(3) 0.007(2) 0.0124(19) 0.0076(18) C1 0.039(2) 0.039(2) 0.036(2) 0.0015(18) 0.0057(17) 0.0069(16) C5 0.056(3) 0.040(2) 0.047(3) -0.002(2) 0.009(2) 0.006(2) C4 0.056(3) 0.037(2) 0.077(4) -0.004(2) 0.011(3) -0.006(2) C3 0.058(3) 0.054(3) 0.063(4) 0.013(3) 0.024(3) 0.002(2) C15 0.073(3) 0.062(3) 0.042(3) 0.016(2) 0.013(2) 0.002(3) C16 0.079(4) 0.069(3) 0.034(3) -0.001(2) 0.011(2) 0.000(3) C17 0.063(3) 0.053(3) 0.038(3) 0.000(2) 0.009(2) -0.004(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.182(4) . ? Ag1 N1 2.182(4) . ? Ag1 Ag1 3.1209(10) 3_755 ? O8 N3 1.255(6) . ? O7 N3 1.226(6) . ? O9 N3 1.200(6) . ? O5 C13 1.301(6) . ? O5 C12 1.458(6) . ? O4 C10 1.399(6) . ? O4 C11 1.410(6) . ? O3 C9 1.403(6) . ? O3 C8 1.406(7) . ? O2 C6 1.323(7) . ? O2 C7 1.454(7) . ? O1 C6 1.201(6) . ? O6 C13 1.206(6) . ? N2 C17 1.333(6) . ? N2 C18 1.346(6) . ? N1 C5 1.341(6) . ? N1 C1 1.345(5) . ? C18 C14 1.397(6) . ? C18 H20 0.9300 . ? C14 C15 1.379(7) . ? C14 C13 1.488(7) . ? C12 C11 1.479(8) . ? C12 H15 0.9700 . ? C12 H16 0.9700 . ? C11 H13 0.9700 . ? C11 H14 0.9700 . ? C10 C9 1.493(8) . ? C10 H11 0.9700 . ? C10 H12 0.9700 . ? C9 H9 0.9700 . ? C9 H10 0.9700 . ? C8 C7 1.467(8) . ? C8 H8 0.9700 . ? C8 H7 0.9700 . ? C7 H6 0.9700 . ? C7 H5 0.9700 . ? C6 C2 1.483(7) . ? C2 C1 1.376(6) 1_455 ? C2 C3 1.395(7) . ? C1 C2 1.376(6) 1_655 ? C1 H1 0.9300 . ? C5 C4 1.378(7) . ? C5 H4 0.9300 . ? C4 C3 1.354(7) 1_655 ? C4 H3 0.9300 . ? C3 C4 1.354(7) 1_455 ? C3 H2 0.9300 . ? C15 C16 1.357(7) . ? C15 H17 0.9300 . ? C16 C17 1.382(7) . ? C16 H18 0.9300 . ? C17 H19 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N1 161.77(13) . . ? N2 Ag1 Ag1 105.91(10) . 3_755 ? N1 Ag1 Ag1 84.18(9) . 3_755 ? C13 O5 C12 117.3(4) . . ? C10 O4 C11 112.5(4) . . ? C9 O3 C8 111.0(5) . . ? C6 O2 C7 116.1(5) . . ? O9 N3 O7 124.7(6) . . ? O9 N3 O8 118.8(6) . . ? O7 N3 O8 116.5(5) . . ? C17 N2 C18 117.9(4) . . ? C17 N2 Ag1 119.5(3) . . ? C18 N2 Ag1 122.3(3) . . ? C5 N1 C1 118.7(4) . . ? C5 N1 Ag1 118.7(3) . . ? C1 N1 Ag1 122.6(3) . . ? N2 C18 C14 122.0(5) . . ? N2 C18 H20 119.0 . . ? C14 C18 H20 119.0 . . ? C15 C14 C18 118.6(5) . . ? C15 C14 C13 121.4(5) . . ? C18 C14 C13 120.0(5) . . ? O6 C13 O5 124.0(5) . . ? O6 C13 C14 122.0(5) . . ? O5 C13 C14 114.0(4) . . ? O5 C12 C11 109.6(4) . . ? O5 C12 H15 109.8 . . ? C11 C12 H15 109.8 . . ? O5 C12 H16 109.8 . . ? C11 C12 H16 109.8 . . ? H15 C12 H16 108.2 . . ? O4 C11 C12 109.9(5) . . ? O4 C11 H13 109.7 . . ? C12 C11 H13 109.7 . . ? O4 C11 H14 109.7 . . ? C12 C11 H14 109.7 . . ? H13 C11 H14 108.2 . . ? O4 C10 C9 111.2(5) . . ? O4 C10 H11 109.4 . . ? C9 C10 H11 109.4 . . ? O4 C10 H12 109.4 . . ? C9 C10 H12 109.4 . . ? H11 C10 H12 108.0 . . ? O3 C9 C10 110.0(5) . . ? O3 C9 H9 109.7 . . ? C10 C9 H9 109.7 . . ? O3 C9 H10 109.7 . . ? C10 C9 H10 109.7 . . ? H9 C9 H10 108.2 . . ? O3 C8 C7 109.5(6) . . ? O3 C8 H8 109.8 . . ? C7 C8 H8 109.8 . . ? O3 C8 H7 109.8 . . ? C7 C8 H7 109.8 . . ? H8 C8 H7 108.2 . . ? O2 C7 C8 107.4(5) . . ? O2 C7 H6 110.2 . . ? C8 C7 H6 110.2 . . ? O2 C7 H5 110.2 . . ? C8 C7 H5 110.2 . . ? H6 C7 H5 108.5 . . ? O1 C6 O2 124.3(5) . . ? O1 C6 C2 123.6(5) . . ? O2 C6 C2 112.1(4) . . ? C1 C2 C3 118.6(5) 1_455 . ? C1 C2 C6 121.9(4) 1_455 . ? C3 C2 C6 119.5(4) . . ? N1 C1 C2 122.1(4) . 1_655 ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 1_655 . ? N1 C5 C4 121.6(5) . . ? N1 C5 H4 119.2 . . ? C4 C5 H4 119.2 . . ? C3 C4 C5 120.1(5) 1_655 . ? C3 C4 H3 119.9 1_655 . ? C5 C4 H3 119.9 . . ? C4 C3 C2 118.9(5) 1_455 . ? C4 C3 H2 120.5 1_455 . ? C2 C3 H2 120.5 . . ? C16 C15 C14 119.3(5) . . ? C16 C15 H17 120.4 . . ? C14 C15 H17 120.4 . . ? C15 C16 C17 119.5(5) . . ? C15 C16 H18 120.3 . . ? C17 C16 H18 120.3 . . ? N2 C17 C16 122.8(5) . . ? N2 C17 H19 118.6 . . ? C16 C17 H19 118.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ag1 N2 C17 107.3(5) . . . . ? Ag1 Ag1 N2 C17 -130.8(3) 3_755 . . . ? N1 Ag1 N2 C18 -78.9(5) . . . . ? Ag1 Ag1 N2 C18 43.0(3) 3_755 . . . ? N2 Ag1 N1 C5 -105.1(5) . . . . ? Ag1 Ag1 N1 C5 130.1(3) 3_755 . . . ? N2 Ag1 N1 C1 72.2(5) . . . . ? Ag1 Ag1 N1 C1 -52.6(3) 3_755 . . . ? C17 N2 C18 C14 0.5(6) . . . . ? Ag1 N2 C18 C14 -173.4(3) . . . . ? N2 C18 C14 C15 -1.1(7) . . . . ? N2 C18 C14 C13 177.7(4) . . . . ? C12 O5 C13 O6 0.0(8) . . . . ? C12 O5 C13 C14 -179.8(4) . . . . ? C15 C14 C13 O6 -5.7(8) . . . . ? C18 C14 C13 O6 175.4(6) . . . . ? C15 C14 C13 O5 174.1(5) . . . . ? C18 C14 C13 O5 -4.7(7) . . . . ? C13 O5 C12 C11 175.1(5) . . . . ? C10 O4 C11 C12 -170.8(5) . . . . ? O5 C12 C11 O4 -78.6(6) . . . . ? C11 O4 C10 C9 178.2(5) . . . . ? C8 O3 C9 C10 170.0(5) . . . . ? O4 C10 C9 O3 81.5(6) . . . . ? C9 O3 C8 C7 179.3(5) . . . . ? C6 O2 C7 C8 167.8(5) . . . . ? O3 C8 C7 O2 -76.3(7) . . . . ? C7 O2 C6 O1 -2.0(8) . . . . ? C7 O2 C6 C2 178.8(5) . . . . ? O1 C6 C2 C1 172.3(5) . . . 1_455 ? O2 C6 C2 C1 -8.6(6) . . . 1_455 ? O1 C6 C2 C3 -7.6(8) . . . . ? O2 C6 C2 C3 171.6(4) . . . . ? C5 N1 C1 C2 0.0(6) . . . 1_655 ? Ag1 N1 C1 C2 -177.2(3) . . . 1_655 ? C1 N1 C5 C4 -1.3(6) . . . . ? Ag1 N1 C5 C4 176.1(3) . . . . ? N1 C5 C4 C3 1.4(7) . . . 1_655 ? C1 C2 C3 C4 -1.1(7) 1_455 . . 1_455 ? C6 C2 C3 C4 178.8(4) . . . 1_455 ? C18 C14 C15 C16 0.4(7) . . . . ? C13 C14 C15 C16 -178.5(5) . . . . ? C14 C15 C16 C17 1.0(8) . . . . ? C18 N2 C17 C16 1.0(7) . . . . ? Ag1 N2 C17 C16 175.1(4) . . . . ? C15 C16 C17 N2 -1.7(8) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.33 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.685 _refine_diff_density_min -0.905 _refine_diff_density_rms 0.099 # Attachment 'compound 6 [Ag2(L3n)(NO3)2]5.cif' data_l3nagno321 _database_code_depnum_ccdc_archive 'CCDC 849909' #TrackingRef 'compound 6 [Ag2(L3n)(NO3)2]5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'bisnicotinate triethyleneglycol' _chemical_melting_point ? _chemical_formula_moiety 'C18 H20 Ag2 N2 O6,2 (N O3)' _chemical_formula_sum 'C18 H20 Ag2 N4 O12' _chemical_formula_weight 700.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8970 1.1020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 8.5066(17) _cell_length_b 23.887(5) _cell_length_c 10.917(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.47(3) _cell_angle_gamma 90.00 _cell_volume 2218.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 15030 _cell_measurement_theta_min 3.4 _cell_measurement_theta_max 55.9 _exptl_crystal_description bloc _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.096 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 1.841 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8046 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18136 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0208 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 27.90 _reflns_number_total 2657 _reflns_number_gt 2400 _reflns_threshold_expression >2\s(I) _computing_data_collection Xarea _computing_cell_refinement Xarea _computing_data_reduction Xarea _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics diamond _computing_publication_material word _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0210P)^2^+4.0635P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2657 _refine_ls_number_parameters 165 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0310 _refine_ls_R_factor_gt 0.0254 _refine_ls_wR_factor_ref 0.0534 _refine_ls_wR_factor_gt 0.0518 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.139 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag2 Ag 0.0000 0.155691(10) 0.7500 0.01981(7) Uani 1 2 d S . . Ag1 Ag 0.0000 0.0000 0.5000 0.02537(8) Uani 1 2 d S . . O2 O 0.32639(19) 0.13887(7) 0.82280(15) 0.0200(3) Uani 1 1 d . . . O1 O 0.4336(2) 0.08956(7) 0.97766(17) 0.0325(4) Uani 1 1 d . . . O3 O 0.1444(2) 0.24234(6) 0.81998(15) 0.0222(3) Uani 1 1 d . . . O4 O 0.0256(2) 0.11915(7) 0.95275(16) 0.0265(4) Uani 1 1 d . . . O6 O -0.0619(2) 0.15500(8) 1.12214(16) 0.0324(4) Uani 1 1 d . . . O5 O 0.1763(3) 0.17457(10) 0.55094(19) 0.0441(5) Uani 1 1 d . . . N01 N 0.1625(2) -0.00403(8) 0.65279(18) 0.0207(4) Uani 1 1 d . . . N02 N -0.0727(2) 0.15029(8) 1.00985(18) 0.0214(4) Uani 1 1 d . . . C2 C 0.3082(3) 0.04043(9) 0.8148(2) 0.0183(4) Uani 1 1 d . . . C7 C 0.3653(3) 0.18963(10) 0.8905(2) 0.0249(5) Uani 1 1 d . . . H6 H 0.4802 0.1918 0.9051 0.030 Uiso 1 1 calc R . . H5 H 0.3119 0.1896 0.9707 0.030 Uiso 1 1 calc R . . C6 C 0.3639(3) 0.09146(9) 0.8808(2) 0.0207(4) Uani 1 1 d . . . C8 C 0.3115(3) 0.23869(10) 0.8150(2) 0.0249(5) Uani 1 1 d . . . H7 H 0.3590 0.2736 0.8473 0.030 Uiso 1 1 calc R . . H8 H 0.3452 0.2339 0.7291 0.030 Uiso 1 1 calc R . . C3 C 0.3413(3) -0.01189(10) 0.8661(2) 0.0229(5) Uani 1 1 d . . . H2 H 0.4011 -0.0146 0.9397 0.027 Uiso 1 1 calc R . . C1 C 0.2211(3) 0.04243(9) 0.7065(2) 0.0194(4) Uani 1 1 d . . . H1 H 0.2022 0.0777 0.6690 0.023 Uiso 1 1 calc R . . C4 C 0.2862(3) -0.05966(10) 0.8087(2) 0.0242(5) Uani 1 1 d . . . H3 H 0.3101 -0.0957 0.8409 0.029 Uiso 1 1 calc R . . C5 C 0.1951(3) -0.05409(10) 0.7033(2) 0.0242(5) Uani 1 1 d . . . H4 H 0.1542 -0.0869 0.6654 0.029 Uiso 1 1 calc R . . C9 C 0.0882(3) 0.28894(9) 0.7495(2) 0.0260(5) Uani 1 1 d . . . H10 H 0.1261 0.2860 0.6643 0.031 Uiso 1 1 calc R . . H9 H 0.1285 0.3243 0.7850 0.031 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag2 0.02324(13) 0.01872(12) 0.01745(12) 0.000 -0.00174(9) 0.000 Ag1 0.02563(14) 0.03198(15) 0.01835(13) -0.00473(9) -0.00886(10) 0.00238(10) O2 0.0219(8) 0.0167(7) 0.0214(8) -0.0001(6) -0.0057(6) -0.0007(6) O1 0.0410(11) 0.0243(9) 0.0317(10) 0.0001(7) -0.0221(8) -0.0008(8) O3 0.0223(8) 0.0173(7) 0.0268(8) 0.0024(6) -0.0038(7) -0.0015(6) O4 0.0294(9) 0.0273(9) 0.0229(8) -0.0006(7) 0.0016(7) 0.0012(7) O6 0.0446(11) 0.0357(10) 0.0169(8) -0.0050(7) -0.0024(8) -0.0060(9) O5 0.0451(13) 0.0533(13) 0.0337(11) -0.0012(9) -0.0093(9) -0.0215(10) N01 0.0217(10) 0.0215(9) 0.0190(9) -0.0022(7) -0.0050(8) 0.0024(7) N02 0.0265(10) 0.0192(9) 0.0186(9) 0.0003(7) -0.0024(8) -0.0046(8) C2 0.0164(10) 0.0188(10) 0.0196(10) -0.0014(8) -0.0029(8) 0.0003(8) C7 0.0267(12) 0.0195(10) 0.0283(12) -0.0020(9) -0.0075(10) -0.0029(9) C6 0.0181(10) 0.0212(11) 0.0226(11) -0.0003(9) -0.0035(9) 0.0007(8) C8 0.0217(12) 0.0201(11) 0.0328(13) -0.0001(9) -0.0023(10) -0.0044(9) C3 0.0219(11) 0.0237(11) 0.0230(11) 0.0015(9) -0.0067(9) 0.0023(9) C1 0.0213(11) 0.0187(10) 0.0181(10) -0.0002(8) -0.0030(9) 0.0026(8) C4 0.0251(12) 0.0196(11) 0.0278(12) 0.0023(9) -0.0055(10) 0.0020(9) C5 0.0261(12) 0.0202(11) 0.0262(12) -0.0048(9) -0.0048(10) 0.0008(9) C9 0.0310(13) 0.0155(10) 0.0314(12) 0.0039(9) -0.0065(10) -0.0022(9) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag2 O4 2.3876(18) 2_556 ? Ag2 O4 2.3876(18) . ? Ag2 O3 2.5223(17) . ? Ag2 O3 2.5223(16) 2_556 ? Ag2 O5 2.689(2) 2_556 ? Ag2 O5 2.689(2) . ? Ag1 N01 2.160(2) . ? Ag1 N01 2.160(2) 5_556 ? O2 C6 1.335(3) . ? O2 C7 1.456(3) . ? O1 C6 1.208(3) . ? O3 C8 1.425(3) . ? O3 C9 1.433(3) . ? O4 N02 1.285(3) . ? O6 N02 1.234(3) . ? O5 N02 1.242(3) 2_556 ? N01 C5 1.344(3) . ? N01 C1 1.348(3) . ? N02 O5 1.242(3) 2_556 ? C2 C1 1.392(3) . ? C2 C3 1.397(3) . ? C2 C6 1.491(3) . ? C7 C8 1.502(3) . ? C7 H6 0.9900 . ? C7 H5 0.9900 . ? C8 H7 0.9900 . ? C8 H8 0.9900 . ? C3 C4 1.382(3) . ? C3 H2 0.9500 . ? C1 H1 0.9500 . ? C4 C5 1.389(3) . ? C4 H3 0.9500 . ? C5 H4 0.9500 . ? C9 C9 1.500(5) 2_556 ? C9 H10 0.9900 . ? C9 H9 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Ag2 O4 137.11(8) 2_556 . ? O4 Ag2 O3 128.41(6) 2_556 . ? O4 Ag2 O3 88.78(6) . . ? O4 Ag2 O3 88.78(6) 2_556 2_556 ? O4 Ag2 O3 128.41(6) . 2_556 ? O3 Ag2 O3 69.71(8) . 2_556 ? O4 Ag2 O5 139.76(7) 2_556 2_556 ? O4 Ag2 O5 50.16(6) . 2_556 ? O3 Ag2 O5 83.75(7) . 2_556 ? O3 Ag2 O5 80.42(6) 2_556 2_556 ? O4 Ag2 O5 50.16(6) 2_556 . ? O4 Ag2 O5 139.76(7) . . ? O3 Ag2 O5 80.42(6) . . ? O3 Ag2 O5 83.75(7) 2_556 . ? O5 Ag2 O5 160.69(10) 2_556 . ? N01 Ag1 N01 180.0 . 5_556 ? C6 O2 C7 114.39(18) . . ? C8 O3 C9 110.85(18) . . ? C8 O3 Ag2 114.94(13) . . ? C9 O3 Ag2 108.37(13) . . ? N02 O4 Ag2 100.57(13) . . ? N02 O5 Ag2 87.45(14) 2_556 . ? C5 N01 C1 118.7(2) . . ? C5 N01 Ag1 118.97(16) . . ? C1 N01 Ag1 122.05(15) . . ? O6 N02 O5 122.3(2) . 2_556 ? O6 N02 O4 119.4(2) . . ? O5 N02 O4 118.2(2) 2_556 . ? C1 C2 C3 118.4(2) . . ? C1 C2 C6 123.2(2) . . ? C3 C2 C6 118.4(2) . . ? O2 C7 C8 107.73(19) . . ? O2 C7 H6 110.2 . . ? C8 C7 H6 110.2 . . ? O2 C7 H5 110.2 . . ? C8 C7 H5 110.2 . . ? H6 C7 H5 108.5 . . ? O1 C6 O2 124.1(2) . . ? O1 C6 C2 122.9(2) . . ? O2 C6 C2 112.97(19) . . ? O3 C8 C7 109.1(2) . . ? O3 C8 H7 109.9 . . ? C7 C8 H7 109.9 . . ? O3 C8 H8 109.9 . . ? C7 C8 H8 109.9 . . ? H7 C8 H8 108.3 . . ? C4 C3 C2 119.4(2) . . ? C4 C3 H2 120.3 . . ? C2 C3 H2 120.3 . . ? N01 C1 C2 122.2(2) . . ? N01 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C3 C4 C5 118.8(2) . . ? C3 C4 H3 120.6 . . ? C5 C4 H3 120.6 . . ? N01 C5 C4 122.4(2) . . ? N01 C5 H4 118.8 . . ? C4 C5 H4 118.8 . . ? O3 C9 C9 109.01(19) . 2_556 ? O3 C9 H10 109.9 . . ? C9 C9 H10 109.9 2_556 . ? O3 C9 H9 109.9 . . ? C9 C9 H9 109.9 2_556 . ? H10 C9 H9 108.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Ag2 O3 C8 -70.60(17) 2_556 . . . ? O4 Ag2 O3 C8 86.09(16) . . . . ? O3 Ag2 O3 C8 -141.81(19) 2_556 . . . ? O5 Ag2 O3 C8 136.12(16) 2_556 . . . ? O5 Ag2 O3 C8 -54.98(16) . . . . ? O4 Ag2 O3 C9 54.01(17) 2_556 . . . ? O4 Ag2 O3 C9 -149.30(15) . . . . ? O3 Ag2 O3 C9 -17.20(12) 2_556 . . . ? O5 Ag2 O3 C9 -99.27(15) 2_556 . . . ? O5 Ag2 O3 C9 69.63(15) . . . . ? O4 Ag2 O4 N02 -134.91(14) 2_556 . . . ? O3 Ag2 O4 N02 72.19(13) . . . . ? O3 Ag2 O4 N02 9.55(16) 2_556 . . . ? O5 Ag2 O4 N02 -10.68(13) 2_556 . . . ? O5 Ag2 O4 N02 145.76(13) . . . . ? O4 Ag2 O5 N02 10.87(13) 2_556 . . 2_556 ? O4 Ag2 O5 N02 130.29(14) . . . 2_556 ? O3 Ag2 O5 N02 -153.18(15) . . . 2_556 ? O3 Ag2 O5 N02 -82.77(15) 2_556 . . 2_556 ? O5 Ag2 O5 N02 -117.81(15) 2_556 . . 2_556 ? N01 Ag1 N01 C5 16(4) 5_556 . . . ? N01 Ag1 N01 C1 -158(4) 5_556 . . . ? Ag2 O4 N02 O6 -159.73(17) . . . . ? Ag2 O4 N02 O5 20.5(2) . . . 2_556 ? C6 O2 C7 C8 -178.3(2) . . . . ? C7 O2 C6 O1 -4.6(3) . . . . ? C7 O2 C6 C2 174.27(19) . . . . ? C1 C2 C6 O1 176.6(2) . . . . ? C3 C2 C6 O1 -1.5(4) . . . . ? C1 C2 C6 O2 -2.3(3) . . . . ? C3 C2 C6 O2 179.6(2) . . . . ? C9 O3 C8 C7 179.69(19) . . . . ? Ag2 O3 C8 C7 -57.0(2) . . . . ? O2 C7 C8 O3 73.7(2) . . . . ? C1 C2 C3 C4 -0.4(4) . . . . ? C6 C2 C3 C4 177.8(2) . . . . ? C5 N01 C1 C2 -2.8(4) . . . . ? Ag1 N01 C1 C2 170.95(17) . . . . ? C3 C2 C1 N01 2.9(3) . . . . ? C6 C2 C1 N01 -175.3(2) . . . . ? C2 C3 C4 C5 -1.9(4) . . . . ? C1 N01 C5 C4 0.2(4) . . . . ? Ag1 N01 C5 C4 -173.66(19) . . . . ? C3 C4 C5 N01 2.1(4) . . . . ? C8 O3 C9 C9 176.3(2) . . . 2_556 ? Ag2 O3 C9 C9 49.3(3) . . . 2_556 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.90 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.744 _refine_diff_density_min -0.807 _refine_diff_density_rms 0.081 # Attachment 'compound 7 [Ag(L4i)O3SCF3]25.cif' data_l4icf3so3 _database_code_depnum_ccdc_archive 'CCDC 849910' #TrackingRef 'compound 7 [Ag(L4i)O3SCF3]25.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'bisisonicotinate tretaethyleneglycol' _chemical_melting_point ? _chemical_formula_moiety 'C40 H48 Ag2 N4 O14, 2(C F3 O3 S)' _chemical_formula_sum 'C42 H48 Ag2 F6 N4 O20 S2' _chemical_formula_weight 1322.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8970 1.1020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0170 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1250 0.1230 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0591(14) _cell_length_b 10.3383(14) _cell_length_c 14.054(2) _cell_angle_alpha 76.820(12) _cell_angle_beta 83.149(12) _cell_angle_gamma 64.790(10) _cell_volume 1287.1(3) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 23195 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 23.96 _exptl_crystal_description bloc _exptl_crystal_colour colorless _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.707 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 668 _exptl_absorpt_coefficient_mu 0.943 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.974 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; the time of the measurement was counted because only one XR machine was accessible for all the departement so the parameter/data ratio is low ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6167 _diffrn_reflns_av_R_equivalents 0.3048 _diffrn_reflns_av_sigmaI/netI 0.2366 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 27.99 _reflns_number_total 6167 _reflns_number_gt 1145 _reflns_threshold_expression >2\s(I) _computing_data_collection Xarea _computing_cell_refinement Xarea _computing_data_reduction Xarea _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics diamond _computing_publication_material word _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1069P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6167 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2093 _refine_ls_R_factor_gt 0.0834 _refine_ls_wR_factor_ref 0.2328 _refine_ls_wR_factor_gt 0.2006 _refine_ls_goodness_of_fit_ref 0.754 _refine_ls_restrained_S_all 0.754 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.21307(11) 0.27698(11) 0.21674(8) 0.0431(3) Uani 1 1 d . . . O4 O 0.3262(9) -0.0015(8) 0.2671(6) 0.045(2) Uani 1 1 d . . . O3 O 0.3587(8) 0.1672(8) 0.3924(5) 0.041(2) Uani 1 1 d . . . O2 O 0.4988(8) 0.3440(8) 0.3973(6) 0.044(2) Uani 1 1 d . . . O1 O 0.4705(9) 0.5737(8) 0.3860(7) 0.059(3) Uani 1 1 d . . . O5 O 0.2955(9) 0.1218(8) 0.0699(5) 0.043(2) Uani 1 1 d . . . O6 O 0.2870(8) 0.3821(8) -0.0673(6) 0.046(2) Uani 1 1 d . . . O7 O 0.1306(10) 0.6184(10) -0.0721(7) 0.068(3) Uani 1 1 d . . . N1 N 0.9976(10) 0.3165(10) 0.2866(7) 0.040(2) Uani 1 1 d . . . N2 N 0.6171(10) 0.6475(10) -0.1588(7) 0.043(2) Uani 1 1 d . . . C10 C 0.4040(13) -0.0647(12) 0.3577(9) 0.044(3) Uani 1 1 d . . . H11 H 0.5066 -0.0817 0.3456 0.053 Uiso 1 1 calc R . . H12 H 0.3992 -0.1576 0.3857 0.053 Uiso 1 1 calc R . . C9 C 0.3372(12) 0.0349(12) 0.4256(9) 0.041(3) Uani 1 1 d . . . H9 H 0.2328 0.0586 0.4324 0.050 Uiso 1 1 calc R . . H10 H 0.3801 -0.0128 0.4893 0.050 Uiso 1 1 calc R . . C8 C 0.3094(13) 0.2608(13) 0.4553(9) 0.047(3) Uani 1 1 d . . . H7 H 0.3573 0.2120 0.5174 0.056 Uiso 1 1 calc R . . H8 H 0.2044 0.2906 0.4667 0.056 Uiso 1 1 calc R . . C7 C 0.3396(11) 0.3887(11) 0.4158(8) 0.033(3) Uani 1 1 d . . . H5 H 0.3050 0.4540 0.4618 0.040 Uiso 1 1 calc R . . H6 H 0.2878 0.4404 0.3553 0.040 Uiso 1 1 calc R . . C6 C 0.5485(12) 0.4470(12) 0.3796(9) 0.041(3) Uani 1 1 d . . . C3 C 0.7077(11) 0.4000(10) 0.3510(8) 0.032(3) Uani 1 1 d . . . C2 C 0.7688(12) 0.4957(12) 0.3311(8) 0.038(3) Uani 1 1 d . . . H1 H 0.7127 0.5913 0.3384 0.046 Uiso 1 1 calc R . . C1 C 0.9114(12) 0.4556(12) 0.3002(8) 0.039(3) Uani 1 1 d . . . H2 H 0.9514 0.5241 0.2880 0.047 Uiso 1 1 calc R . . C5 C 0.9392(12) 0.2220(12) 0.3089(9) 0.043(3) Uani 1 1 d . . . H3 H 0.9994 0.1264 0.3030 0.052 Uiso 1 1 calc R . . C4 C 0.7934(12) 0.2521(11) 0.3410(9) 0.042(3) Uani 1 1 d . . . H4 H 0.7556 0.1818 0.3546 0.051 Uiso 1 1 calc R . . C11 C 0.3962(16) -0.0881(13) 0.1938(10) 0.058(4) Uani 1 1 d . . . H13 H 0.4076 -0.1877 0.2189 0.070 Uiso 1 1 calc R . . H14 H 0.4931 -0.0893 0.1774 0.070 Uiso 1 1 calc R . . C12 C 0.3061(17) -0.0262(12) 0.1055(10) 0.059(4) Uani 1 1 d . . . H16 H 0.3518 -0.0846 0.0559 0.071 Uiso 1 1 calc R . . H15 H 0.2090 -0.0247 0.1213 0.071 Uiso 1 1 calc R . . C13 C 0.2144(16) 0.1827(13) -0.0180(10) 0.059(4) Uani 1 1 d . . . H17 H 0.1299 0.1587 -0.0112 0.070 Uiso 1 1 calc R . . H18 H 0.2758 0.1436 -0.0722 0.070 Uiso 1 1 calc R . . C14 C 0.1652(13) 0.3448(14) -0.0363(10) 0.053(3) Uani 1 1 d . . . H20 H 0.0914 0.3911 -0.0862 0.063 Uiso 1 1 calc R . . H19 H 0.1212 0.3803 0.0231 0.063 Uiso 1 1 calc R . . C15 C 0.2548(14) 0.5284(13) -0.0805(9) 0.041(3) Uani 1 1 d . . . C16 C 0.3798(12) 0.5676(12) -0.1101(8) 0.037(3) Uani 1 1 d . . . C17 C 0.5253(12) 0.4616(13) -0.1208(8) 0.041(3) Uani 1 1 d . . . H21 H 0.5447 0.3633 -0.1110 0.049 Uiso 1 1 calc R . . C18 C 0.6340(12) 0.5065(13) -0.1455(8) 0.041(3) Uani 1 1 d . . . H22 H 0.7280 0.4362 -0.1542 0.049 Uiso 1 1 calc R . . C19 C 0.4741(13) 0.7453(14) -0.1527(9) 0.048(3) Uani 1 1 d . . . H23 H 0.4559 0.8436 -0.1668 0.058 Uiso 1 1 calc R . . C20 C 0.3578(14) 0.7123(14) -0.1282(9) 0.047(3) Uani 1 1 d . . . H24 H 0.2641 0.7853 -0.1235 0.056 Uiso 1 1 calc R . . S1 S 0.0686(3) 0.1666(3) 0.7495(3) 0.0504(9) Uani 1 1 d . . . F1 F -0.1552(9) 0.2062(10) 0.6527(7) 0.087(3) Uani 1 1 d . . . F2 F 0.0518(10) 0.0994(9) 0.5832(6) 0.079(2) Uani 1 1 d . . . F3 F -0.0347(8) 0.3296(8) 0.5800(6) 0.075(2) Uani 1 1 d . . . O8 O 0.0743(11) 0.0275(8) 0.7971(7) 0.062(3) Uani 1 1 d . . . O9 O 0.2068(10) 0.1746(11) 0.7176(8) 0.079(3) Uani 1 1 d . . . O10 O -0.0293(10) 0.2864(9) 0.7966(7) 0.071(3) Uani 1 1 d . . . C21 C -0.0249(14) 0.2058(15) 0.6366(11) 0.056(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0366(5) 0.0387(5) 0.0549(7) -0.0165(4) 0.0083(4) -0.0153(4) O4 0.051(5) 0.038(4) 0.048(5) -0.022(4) -0.005(4) -0.014(4) O3 0.045(5) 0.046(5) 0.033(5) -0.021(4) 0.008(4) -0.015(4) O2 0.023(4) 0.038(4) 0.067(6) -0.019(4) 0.007(4) -0.006(3) O1 0.046(5) 0.024(4) 0.096(7) -0.020(5) 0.011(5) -0.003(4) O5 0.065(5) 0.032(4) 0.032(5) -0.001(4) -0.004(4) -0.022(4) O6 0.048(5) 0.045(5) 0.045(5) -0.004(4) 0.004(4) -0.025(4) O7 0.049(6) 0.055(6) 0.087(8) -0.009(5) 0.002(5) -0.013(5) N1 0.044(6) 0.040(6) 0.044(6) -0.020(5) 0.004(5) -0.020(5) N2 0.033(6) 0.033(5) 0.051(7) -0.003(5) 0.006(5) -0.006(4) C10 0.047(7) 0.034(6) 0.054(8) -0.011(6) -0.011(6) -0.016(6) C9 0.033(6) 0.040(7) 0.052(8) -0.001(6) -0.007(6) -0.018(5) C8 0.043(7) 0.054(8) 0.041(8) -0.016(6) 0.014(6) -0.019(6) C7 0.023(6) 0.031(6) 0.047(7) -0.012(5) 0.001(5) -0.010(5) C6 0.036(7) 0.034(7) 0.057(8) -0.003(6) -0.002(6) -0.022(6) C3 0.033(6) 0.020(5) 0.041(7) -0.007(5) -0.005(5) -0.007(5) C2 0.041(7) 0.031(6) 0.048(7) -0.022(6) 0.003(6) -0.013(5) C1 0.035(7) 0.045(7) 0.049(8) -0.026(6) 0.001(6) -0.019(6) C5 0.031(6) 0.033(6) 0.067(9) -0.023(6) 0.004(6) -0.010(5) C4 0.036(7) 0.024(6) 0.067(9) -0.007(6) 0.002(6) -0.013(5) C11 0.080(10) 0.027(7) 0.060(9) -0.012(6) 0.004(8) -0.015(7) C12 0.094(11) 0.033(7) 0.059(9) -0.013(7) 0.004(8) -0.035(7) C13 0.079(10) 0.047(8) 0.054(9) -0.026(7) 0.022(8) -0.028(7) C14 0.034(7) 0.063(9) 0.063(9) -0.003(7) 0.003(6) -0.028(7) C15 0.049(8) 0.042(7) 0.042(7) -0.006(6) 0.006(6) -0.030(6) C16 0.045(7) 0.041(7) 0.029(7) -0.012(5) 0.005(5) -0.020(6) C17 0.037(7) 0.049(7) 0.025(6) -0.008(5) 0.003(5) -0.009(6) C18 0.032(6) 0.043(7) 0.049(8) -0.014(6) 0.011(5) -0.017(6) C19 0.041(7) 0.045(7) 0.055(8) -0.019(6) 0.008(6) -0.012(6) C20 0.038(7) 0.049(8) 0.043(8) -0.008(6) 0.006(6) -0.010(6) S1 0.0416(19) 0.0358(18) 0.073(2) -0.0181(17) 0.0007(17) -0.0122(15) F1 0.049(5) 0.114(7) 0.099(7) -0.021(6) -0.010(5) -0.031(5) F2 0.093(6) 0.062(5) 0.071(6) -0.026(5) 0.006(5) -0.018(5) F3 0.066(5) 0.041(4) 0.086(6) 0.009(4) 0.004(4) -0.005(4) O8 0.082(7) 0.026(4) 0.076(7) -0.006(4) -0.009(5) -0.021(4) O9 0.039(5) 0.082(7) 0.125(9) -0.063(7) 0.009(5) -0.015(5) O10 0.077(7) 0.041(5) 0.092(8) -0.046(5) 0.019(6) -0.010(5) C21 0.034(7) 0.054(9) 0.072(10) -0.013(8) 0.009(7) -0.013(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.169(9) 2_665 ? Ag1 N1 2.179(9) 1_455 ? Ag1 O4 2.561(8) . ? Ag1 O5 2.736(7) . ? O4 C11 1.439(14) . ? O4 C10 1.443(14) . ? O3 C8 1.357(13) . ? O3 C9 1.439(13) . ? O2 C6 1.322(12) . ? O2 C7 1.474(12) . ? O1 C6 1.225(13) . ? O5 C13 1.427(15) . ? O5 C12 1.459(13) . ? O6 C15 1.377(13) . ? O6 C14 1.427(13) . ? O7 C15 1.210(14) . ? N1 C5 1.306(14) . ? N1 C1 1.371(13) . ? N1 Ag1 2.179(9) 1_655 ? N2 C18 1.364(14) . ? N2 C19 1.368(14) . ? N2 Ag1 2.169(9) 2_665 ? C10 C9 1.459(15) . ? C10 H11 0.9700 . ? C10 H12 0.9700 . ? C9 H9 0.9700 . ? C9 H10 0.9700 . ? C8 C7 1.455(15) . ? C8 H7 0.9700 . ? C8 H8 0.9700 . ? C7 H5 0.9700 . ? C7 H6 0.9700 . ? C6 C3 1.495(15) . ? C3 C2 1.335(14) . ? C3 C4 1.431(14) . ? C2 C1 1.358(15) . ? C2 H1 0.9300 . ? C1 H2 0.9300 . ? C5 C4 1.403(15) . ? C5 H3 0.9300 . ? C4 H4 0.9300 . ? C11 C12 1.478(18) . ? C11 H13 0.9700 . ? C11 H14 0.9700 . ? C12 H16 0.9700 . ? C12 H15 0.9700 . ? C13 C14 1.499(17) . ? C13 H17 0.9700 . ? C13 H18 0.9700 . ? C14 H20 0.9700 . ? C14 H19 0.9700 . ? C15 C16 1.467(16) . ? C16 C20 1.382(16) . ? C16 C17 1.422(15) . ? C17 C18 1.342(15) . ? C17 H21 0.9300 . ? C18 H22 0.9300 . ? C19 C20 1.338(16) . ? C19 H23 0.9300 . ? C20 H24 0.9300 . ? S1 O8 1.421(8) . ? S1 O9 1.439(10) . ? S1 O10 1.456(8) . ? S1 C21 1.818(15) . ? F1 C21 1.302(14) . ? F2 C21 1.373(14) . ? F3 C21 1.315(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N1 150.1(3) 2_665 1_455 ? N2 Ag1 O4 110.0(3) 2_665 . ? N1 Ag1 O4 97.4(3) 1_455 . ? N2 Ag1 O5 86.3(3) 2_665 . ? N1 Ag1 O5 117.7(3) 1_455 . ? O4 Ag1 O5 62.9(2) . . ? C11 O4 C10 111.6(9) . . ? C11 O4 Ag1 119.3(7) . . ? C10 O4 Ag1 117.3(6) . . ? C8 O3 C9 115.1(9) . . ? C6 O2 C7 117.6(8) . . ? C13 O5 C12 108.7(9) . . ? C13 O5 Ag1 118.7(6) . . ? C12 O5 Ag1 111.4(7) . . ? C15 O6 C14 114.9(9) . . ? C5 N1 C1 117.3(10) . . ? C5 N1 Ag1 125.2(7) . 1_655 ? C1 N1 Ag1 117.2(7) . 1_655 ? C18 N2 C19 113.7(10) . . ? C18 N2 Ag1 124.6(7) . 2_665 ? C19 N2 Ag1 120.3(8) . 2_665 ? O4 C10 C9 109.1(9) . . ? O4 C10 H11 109.9 . . ? C9 C10 H11 109.9 . . ? O4 C10 H12 109.9 . . ? C9 C10 H12 109.9 . . ? H11 C10 H12 108.3 . . ? O3 C9 C10 111.6(10) . . ? O3 C9 H9 109.3 . . ? C10 C9 H9 109.3 . . ? O3 C9 H10 109.3 . . ? C10 C9 H10 109.3 . . ? H9 C9 H10 108.0 . . ? O3 C8 C7 110.5(10) . . ? O3 C8 H7 109.5 . . ? C7 C8 H7 109.5 . . ? O3 C8 H8 109.5 . . ? C7 C8 H8 109.5 . . ? H7 C8 H8 108.1 . . ? C8 C7 O2 109.8(8) . . ? C8 C7 H5 109.7 . . ? O2 C7 H5 109.7 . . ? C8 C7 H6 109.7 . . ? O2 C7 H6 109.7 . . ? H5 C7 H6 108.2 . . ? O1 C6 O2 122.9(10) . . ? O1 C6 C3 121.2(10) . . ? O2 C6 C3 116.0(9) . . ? C2 C3 C4 119.9(10) . . ? C2 C3 C6 120.8(9) . . ? C4 C3 C6 119.3(9) . . ? C3 C2 C1 121.2(10) . . ? C3 C2 H1 119.4 . . ? C1 C2 H1 119.4 . . ? C2 C1 N1 121.5(10) . . ? C2 C1 H2 119.2 . . ? N1 C1 H2 119.2 . . ? N1 C5 C4 125.6(10) . . ? N1 C5 H3 117.2 . . ? C4 C5 H3 117.2 . . ? C5 C4 C3 114.4(10) . . ? C5 C4 H4 122.8 . . ? C3 C4 H4 122.8 . . ? O4 C11 C12 109.7(10) . . ? O4 C11 H13 109.7 . . ? C12 C11 H13 109.7 . . ? O4 C11 H14 109.7 . . ? C12 C11 H14 109.7 . . ? H13 C11 H14 108.2 . . ? O5 C12 C11 107.3(10) . . ? O5 C12 H16 110.3 . . ? C11 C12 H16 110.3 . . ? O5 C12 H15 110.3 . . ? C11 C12 H15 110.3 . . ? H16 C12 H15 108.5 . . ? O5 C13 C14 107.7(10) . . ? O5 C13 H17 110.2 . . ? C14 C13 H17 110.2 . . ? O5 C13 H18 110.2 . . ? C14 C13 H18 110.2 . . ? H17 C13 H18 108.5 . . ? O6 C14 C13 110.3(10) . . ? O6 C14 H20 109.6 . . ? C13 C14 H20 109.6 . . ? O6 C14 H19 109.6 . . ? C13 C14 H19 109.6 . . ? H20 C14 H19 108.1 . . ? O7 C15 O6 122.0(11) . . ? O7 C15 C16 122.6(11) . . ? O6 C15 C16 115.3(10) . . ? C20 C16 C17 117.8(11) . . ? C20 C16 C15 119.7(11) . . ? C17 C16 C15 122.5(10) . . ? C18 C17 C16 118.6(11) . . ? C18 C17 H21 120.7 . . ? C16 C17 H21 120.7 . . ? C17 C18 N2 125.0(11) . . ? C17 C18 H22 117.5 . . ? N2 C18 H22 117.5 . . ? C20 C19 N2 125.9(12) . . ? C20 C19 H23 117.0 . . ? N2 C19 H23 117.0 . . ? C19 C20 C16 118.7(11) . . ? C19 C20 H24 120.6 . . ? C16 C20 H24 120.6 . . ? O8 S1 O9 116.7(6) . . ? O8 S1 O10 114.6(6) . . ? O9 S1 O10 112.9(6) . . ? O8 S1 C21 103.8(6) . . ? O9 S1 C21 104.2(6) . . ? O10 S1 C21 102.3(6) . . ? F1 C21 F3 109.6(11) . . ? F1 C21 F2 105.9(11) . . ? F3 C21 F2 106.2(11) . . ? F1 C21 S1 112.1(10) . . ? F3 C21 S1 112.5(10) . . ? F2 C21 S1 110.2(9) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.99 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.168 _refine_diff_density_min -1.523 _refine_diff_density_rms 0.191 # Attachment 'compound 8 [Ag(L4n)NO3(CH3OH)]24.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 849911' #TrackingRef 'compound 8 [Ag(L4n)NO3(CH3OH)]24.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'bisnicotinate tetraethyleneglycol' _chemical_melting_point ? _chemical_formula_moiety 'C40 H48 Ag2 N4 O14,2(N1 O3), 2(C1 H4 O1)' _chemical_formula_sum 'C42 H56 Ag2 N6 O22' _chemical_formula_weight 1212.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.5480(5) _cell_length_b 8.1661(3) _cell_length_c 31.3729(15) _cell_angle_alpha 90.00 _cell_angle_beta 91.197(4) _cell_angle_gamma 90.00 _cell_volume 2445.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 56351 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 29.62 _exptl_crystal_description diamond _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.647 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 0.889 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.71579 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; after 50 cycles of LS nothing changes, the time of the measurement was counted because only one XR machine was accessible for all the departement, _refine_ls_shift/su_max 3.442 refine_ls_shift/su_mean and max are high probably due to the motion of the methanol molecules ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 69921 _diffrn_reflns_av_R_equivalents 0.0684 _diffrn_reflns_av_sigmaI/netI 0.0303 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 29.26 _reflns_number_total 6585 _reflns_number_gt 5297 _reflns_threshold_expression >2\s(I) _computing_data_collection Xarea _computing_cell_refinement Xarea _computing_data_reduction Xarea _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics diamond _computing_publication_material word _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0509P)^2^+0.0416P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6585 _refine_ls_number_parameters 341 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0382 _refine_ls_R_factor_gt 0.0279 _refine_ls_wR_factor_ref 0.0717 _refine_ls_wR_factor_gt 0.0684 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.952 _refine_ls_shift/su_max 0.040 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.997511(14) -0.287906(18) -0.014395(4) 0.02116(5) Uani 1 1 d . . . O2 O 0.90248(12) -0.01972(15) 0.13810(3) 0.0179(2) Uani 1 1 d . . . O1 O 0.68116(13) -0.03929(18) 0.16076(4) 0.0227(3) Uani 1 1 d . . . O7 O 0.64818(16) 0.5318(2) 0.18434(5) 0.0385(4) Uani 1 1 d . . . O4 O 1.34308(13) 0.31978(15) 0.19310(4) 0.0173(2) Uani 1 1 d . . . O5 O 1.13604(12) 0.53568(15) 0.22115(4) 0.0173(2) Uani 1 1 d . . . O6 O 0.87794(13) 0.53695(15) 0.17101(4) 0.0181(2) Uani 1 1 d . . . O3 O 1.17845(13) 0.01323(15) 0.17800(4) 0.0200(2) Uani 1 1 d . . . N1 N 0.83004(15) -0.28725(17) 0.03154(4) 0.0160(3) Uani 1 1 d . . . N2 N 0.82726(15) 0.30202(17) 0.05690(4) 0.0160(3) Uani 1 1 d . . . C7 C 0.93767(18) 0.0845(2) 0.17430(5) 0.0162(3) Uani 1 1 d . . . H5 H 0.9310 0.0231 0.2006 0.019 Uiso 1 1 calc R . . H6 H 0.8733 0.1763 0.1754 0.019 Uiso 1 1 calc R . . C6 C 0.76910(17) -0.0690(2) 0.13492(5) 0.0147(3) Uani 1 1 d . . . C18 C 0.58778(19) 0.2421(2) 0.07337(6) 0.0195(3) Uani 1 1 d . . . H22 H 0.5038 0.1912 0.0658 0.023 Uiso 1 1 calc R . . C10 C 1.39376(18) 0.1577(2) 0.19975(5) 0.0185(3) Uani 1 1 d . . . H11 H 1.3746 0.1227 0.2286 0.022 Uiso 1 1 calc R . . H12 H 1.4943 0.1545 0.1959 0.022 Uiso 1 1 calc R . . C12 C 1.28194(19) 0.5765(2) 0.22199(6) 0.0203(3) Uani 1 1 d . . . H15 H 1.3018 0.6540 0.2448 0.024 Uiso 1 1 calc R . . H16 H 1.3070 0.6269 0.1952 0.024 Uiso 1 1 calc R . . C9 C 1.32185(18) 0.0449(2) 0.16818(5) 0.0194(3) Uani 1 1 d . . . H9 H 1.3258 0.0933 0.1400 0.023 Uiso 1 1 calc R . . H10 H 1.3723 -0.0581 0.1675 0.023 Uiso 1 1 calc R . . C19 C 0.70269(19) 0.2310(2) 0.04725(5) 0.0178(3) Uani 1 1 d . . . H23 H 0.6937 0.1721 0.0220 0.021 Uiso 1 1 calc R . . C8 C 1.08498(18) 0.1452(2) 0.16893(5) 0.0173(3) Uani 1 1 d . . . H7 H 1.0973 0.1834 0.1400 0.021 Uiso 1 1 calc R . . H8 H 1.1039 0.2356 0.1883 0.021 Uiso 1 1 calc R . . C3 C 0.60780(18) -0.2198(2) 0.08500(5) 0.0165(3) Uani 1 1 d . . . H1 H 0.5335 -0.1964 0.1027 0.020 Uiso 1 1 calc R . . C16 C 0.72913(17) 0.4025(2) 0.12147(5) 0.0154(3) Uani 1 1 d . . . C14 C 0.90036(18) 0.6258(2) 0.21090(5) 0.0183(3) Uani 1 1 d . . . H19 H 0.8774 0.5565 0.2349 0.022 Uiso 1 1 calc R . . H20 H 0.8408 0.7220 0.2115 0.022 Uiso 1 1 calc R . . C4 C 0.58665(18) -0.3094(2) 0.04765(5) 0.0183(3) Uani 1 1 d . . . H2 H 0.4978 -0.3476 0.0401 0.022 Uiso 1 1 calc R . . C15 C 0.74455(19) 0.4960(2) 0.16218(5) 0.0183(3) Uani 1 1 d . . . C2 C 0.74272(17) -0.1661(2) 0.09521(5) 0.0136(3) Uani 1 1 d . . . C17 C 0.60022(18) 0.3305(2) 0.11112(5) 0.0180(3) Uani 1 1 d . . . H21 H 0.5245 0.3415 0.1291 0.022 Uiso 1 1 calc R . . C1 C 0.85076(17) -0.2013(2) 0.06762(5) 0.0153(3) Uani 1 1 d . . . H4 H 0.9405 -0.1640 0.0744 0.018 Uiso 1 1 calc R . . C5 C 0.69942(18) -0.3407(2) 0.02197(5) 0.0167(3) Uani 1 1 d . . . H3 H 0.6847 -0.4010 -0.0029 0.020 Uiso 1 1 calc R . . C11 C 1.36554(18) 0.4234(2) 0.22901(5) 0.0193(3) Uani 1 1 d . . . H13 H 1.4643 0.4498 0.2322 0.023 Uiso 1 1 calc R . . H14 H 1.3360 0.3687 0.2547 0.023 Uiso 1 1 calc R . . C20 C 0.83946(17) 0.3853(2) 0.09371(5) 0.0152(3) Uani 1 1 d . . . H24 H 0.9251 0.4333 0.1009 0.018 Uiso 1 1 calc R . . C13 C 1.0516(2) 0.6757(2) 0.21384(5) 0.0192(3) Uani 1 1 d . . . H17 H 1.0783 0.7285 0.1875 0.023 Uiso 1 1 calc R . . H18 H 1.0653 0.7532 0.2370 0.023 Uiso 1 1 calc R . . O9 O 0.23289(14) 0.17597(15) 0.06456(4) 0.0216(3) Uani 1 1 d . . . O8 O 0.11348(14) -0.01660(17) 0.03283(4) 0.0250(3) Uani 1 1 d . . . O10 O 0.32320(15) -0.06649(18) 0.05773(5) 0.0301(3) Uani 1 1 d . . . N3 N 0.22300(15) 0.03100(18) 0.05196(4) 0.0174(3) Uani 1 1 d . . . O11 O 0.21868(18) 0.6065(2) 0.05552(5) 0.0329(4) Uani 1 1 d . . . C21 C 0.2299(2) 0.5647(3) 0.09933(7) 0.0299(4) Uani 1 1 d . . . H21C H 0.324(3) 0.595(3) 0.1135(9) 0.043(7) Uiso 1 1 d . . . H21A H 0.160(3) 0.613(4) 0.1177(9) 0.046(8) Uiso 1 1 d . . . H11B H 0.227(4) 0.690(4) 0.0541(11) 0.049(10) Uiso 1 1 d . . . H21B H 0.216(3) 0.446(4) 0.1025(9) 0.046(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01923(8) 0.02859(8) 0.01587(7) -0.00351(5) 0.00502(5) 0.00415(5) O2 0.0153(6) 0.0226(6) 0.0158(5) -0.0059(5) 0.0010(4) -0.0036(5) O1 0.0162(6) 0.0333(7) 0.0186(6) -0.0072(5) 0.0033(5) -0.0006(5) O7 0.0238(7) 0.0608(11) 0.0315(7) -0.0203(7) 0.0132(6) -0.0101(7) O4 0.0190(6) 0.0186(6) 0.0143(5) -0.0012(4) -0.0022(4) -0.0019(4) O5 0.0164(6) 0.0150(6) 0.0206(5) -0.0013(4) 0.0002(4) -0.0024(4) O6 0.0168(6) 0.0227(6) 0.0147(5) -0.0042(4) 0.0001(4) 0.0018(5) O3 0.0154(6) 0.0165(6) 0.0280(6) 0.0047(5) -0.0007(5) -0.0005(4) N1 0.0160(7) 0.0181(7) 0.0138(6) -0.0008(5) 0.0016(5) 0.0000(5) N2 0.0160(7) 0.0179(7) 0.0142(6) -0.0004(5) 0.0013(5) 0.0030(5) C7 0.0177(8) 0.0170(8) 0.0137(7) -0.0032(6) -0.0015(6) -0.0012(6) C6 0.0149(8) 0.0152(7) 0.0139(7) 0.0014(5) -0.0008(6) 0.0011(6) C18 0.0184(8) 0.0188(8) 0.0211(8) 0.0020(6) -0.0019(6) -0.0038(6) C10 0.0151(8) 0.0222(8) 0.0181(7) 0.0032(6) 0.0006(6) 0.0016(6) C12 0.0196(8) 0.0224(9) 0.0191(8) -0.0046(6) 0.0020(6) -0.0079(7) C9 0.0174(8) 0.0198(8) 0.0211(8) -0.0002(6) 0.0030(6) 0.0017(6) C19 0.0202(8) 0.0165(8) 0.0166(7) -0.0003(6) -0.0019(6) -0.0007(6) C8 0.0188(8) 0.0143(7) 0.0188(7) 0.0009(6) -0.0019(6) -0.0013(6) C3 0.0134(8) 0.0192(8) 0.0169(7) 0.0012(6) 0.0007(6) 0.0009(6) C16 0.0169(8) 0.0159(7) 0.0135(7) 0.0022(6) 0.0014(6) 0.0010(6) C14 0.0243(9) 0.0179(8) 0.0128(7) -0.0023(6) 0.0004(6) 0.0036(7) C4 0.0144(8) 0.0207(8) 0.0197(8) 0.0018(6) -0.0032(6) -0.0034(6) C15 0.0197(9) 0.0195(8) 0.0158(7) 0.0004(6) 0.0034(6) -0.0009(6) C2 0.0143(8) 0.0134(7) 0.0131(7) 0.0005(5) 0.0001(6) 0.0005(6) C17 0.0163(8) 0.0183(8) 0.0196(8) 0.0035(6) 0.0036(6) -0.0006(6) C1 0.0143(7) 0.0163(8) 0.0154(7) -0.0004(6) 0.0002(6) -0.0010(6) C5 0.0202(8) 0.0146(7) 0.0153(7) -0.0001(6) -0.0026(6) 0.0004(6) C11 0.0156(8) 0.0278(9) 0.0145(7) -0.0038(6) -0.0002(6) -0.0060(7) C20 0.0143(7) 0.0166(8) 0.0147(7) 0.0005(6) -0.0009(6) 0.0011(6) C13 0.0268(9) 0.0142(8) 0.0167(7) -0.0015(6) 0.0002(6) -0.0005(6) O9 0.0267(7) 0.0181(6) 0.0200(6) -0.0022(4) -0.0035(5) -0.0020(5) O8 0.0169(6) 0.0257(7) 0.0322(7) -0.0034(6) -0.0066(5) -0.0046(5) O10 0.0235(7) 0.0287(7) 0.0378(8) -0.0040(6) -0.0089(6) 0.0102(6) N3 0.0161(7) 0.0213(7) 0.0147(6) 0.0011(5) 0.0004(5) -0.0009(5) O11 0.0466(10) 0.0277(8) 0.0242(7) -0.0067(6) -0.0059(6) 0.0054(7) C21 0.0317(11) 0.0329(11) 0.0252(9) -0.0024(8) 0.0038(8) -0.0059(9) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.1643(15) 3_755 ? Ag1 N1 2.1749(15) . ? O2 C6 1.337(2) . ? O2 C7 1.4531(19) . ? O1 C6 1.204(2) . ? O7 C15 1.201(2) . ? O4 C11 1.422(2) . ? O4 C10 1.423(2) . ? O5 C13 1.415(2) . ? O5 C12 1.432(2) . ? O6 C15 1.340(2) . ? O6 C14 1.4587(19) . ? O3 C8 1.424(2) . ? O3 C9 1.433(2) . ? N1 C1 1.343(2) . ? N1 C5 1.349(2) . ? N2 C20 1.343(2) . ? N2 C19 1.352(2) . ? N2 Ag1 2.1643(15) 3_755 ? C7 C8 1.504(2) . ? C7 H5 0.9700 . ? C7 H6 0.9700 . ? C6 C2 1.494(2) . ? C18 C19 1.386(3) . ? C18 C17 1.390(2) . ? C18 H22 0.9300 . ? C10 C9 1.507(2) . ? C10 H11 0.9700 . ? C10 H12 0.9700 . ? C12 C11 1.497(3) . ? C12 H15 0.9700 . ? C12 H16 0.9700 . ? C9 H9 0.9700 . ? C9 H10 0.9700 . ? C19 H23 0.9300 . ? C8 H7 0.9700 . ? C8 H8 0.9700 . ? C3 C4 1.393(2) . ? C3 C2 1.392(2) . ? C3 H1 0.9300 . ? C16 C20 1.388(2) . ? C16 C17 1.396(2) . ? C16 C15 1.493(2) . ? C14 C13 1.501(3) . ? C14 H19 0.9700 . ? C14 H20 0.9700 . ? C4 C5 1.382(3) . ? C4 H2 0.9300 . ? C2 C1 1.390(2) . ? C17 H21 0.9300 . ? C1 H4 0.9300 . ? C5 H3 0.9300 . ? C11 H13 0.9700 . ? C11 H14 0.9700 . ? C20 H24 0.9300 . ? C13 H17 0.9700 . ? C13 H18 0.9700 . ? O9 N3 1.251(2) . ? O8 N3 1.2564(18) . ? O10 N3 1.255(2) . ? O11 C21 1.418(3) . ? O11 H11B 0.69(3) . ? C21 H21C 1.03(3) . ? C21 H21A 0.97(3) . ? C21 H21B 0.98(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N1 175.53(5) 3_755 . ? C6 O2 C7 116.04(13) . . ? C11 O4 C10 113.08(13) . . ? C13 O5 C12 111.44(13) . . ? C15 O6 C14 115.05(13) . . ? C8 O3 C9 114.71(13) . . ? C1 N1 C5 118.42(15) . . ? C1 N1 Ag1 117.54(11) . . ? C5 N1 Ag1 122.73(11) . . ? C20 N2 C19 118.03(15) . . ? C20 N2 Ag1 120.16(11) . 3_755 ? C19 N2 Ag1 121.80(11) . 3_755 ? O2 C7 C8 107.87(13) . . ? O2 C7 H5 110.1 . . ? C8 C7 H5 110.1 . . ? O2 C7 H6 110.1 . . ? C8 C7 H6 110.1 . . ? H5 C7 H6 108.4 . . ? O1 C6 O2 124.44(15) . . ? O1 C6 C2 124.11(15) . . ? O2 C6 C2 111.45(14) . . ? C19 C18 C17 118.87(16) . . ? C19 C18 H22 120.6 . . ? C17 C18 H22 120.6 . . ? O4 C10 C9 108.84(13) . . ? O4 C10 H11 109.9 . . ? C9 C10 H11 109.9 . . ? O4 C10 H12 109.9 . . ? C9 C10 H12 109.9 . . ? H11 C10 H12 108.3 . . ? O5 C12 C11 108.86(14) . . ? O5 C12 H15 109.9 . . ? C11 C12 H15 109.9 . . ? O5 C12 H16 109.9 . . ? C11 C12 H16 109.9 . . ? H15 C12 H16 108.3 . . ? O3 C9 C10 113.14(14) . . ? O3 C9 H9 109.0 . . ? C10 C9 H9 109.0 . . ? O3 C9 H10 109.0 . . ? C10 C9 H10 109.0 . . ? H9 C9 H10 107.8 . . ? N2 C19 C18 122.91(16) . . ? N2 C19 H23 118.5 . . ? C18 C19 H23 118.5 . . ? O3 C8 C7 108.19(14) . . ? O3 C8 H7 110.1 . . ? C7 C8 H7 110.1 . . ? O3 C8 H8 110.1 . . ? C7 C8 H8 110.1 . . ? H7 C8 H8 108.4 . . ? C4 C3 C2 118.44(16) . . ? C4 C3 H1 120.8 . . ? C2 C3 H1 120.8 . . ? C20 C16 C17 119.25(15) . . ? C20 C16 C15 121.73(15) . . ? C17 C16 C15 119.02(15) . . ? O6 C14 C13 108.14(13) . . ? O6 C14 H19 110.1 . . ? C13 C14 H19 110.1 . . ? O6 C14 H20 110.1 . . ? C13 C14 H20 110.1 . . ? H19 C14 H20 108.4 . . ? C5 C4 C3 119.13(15) . . ? C5 C4 H2 120.4 . . ? C3 C4 H2 120.4 . . ? O7 C15 O6 123.78(16) . . ? O7 C15 C16 123.83(17) . . ? O6 C15 C16 112.39(14) . . ? C1 C2 C3 119.15(15) . . ? C1 C2 C6 120.97(14) . . ? C3 C2 C6 119.87(15) . . ? C18 C17 C16 118.43(16) . . ? C18 C17 H21 120.8 . . ? C16 C17 H21 120.8 . . ? N1 C1 C2 122.31(15) . . ? N1 C1 H4 118.8 . . ? C2 C1 H4 118.8 . . ? N1 C5 C4 122.54(15) . . ? N1 C5 H3 118.7 . . ? C4 C5 H3 118.7 . . ? O4 C11 C12 108.03(13) . . ? O4 C11 H13 110.1 . . ? C12 C11 H13 110.1 . . ? O4 C11 H14 110.1 . . ? C12 C11 H14 110.1 . . ? H13 C11 H14 108.4 . . ? N2 C20 C16 122.50(15) . . ? N2 C20 H24 118.8 . . ? C16 C20 H24 118.8 . . ? O5 C13 C14 109.58(14) . . ? O5 C13 H17 109.8 . . ? C14 C13 H17 109.8 . . ? O5 C13 H18 109.8 . . ? C14 C13 H18 109.8 . . ? H17 C13 H18 108.2 . . ? O9 N3 O10 120.16(14) . . ? O9 N3 O8 120.02(15) . . ? O10 N3 O8 119.81(15) . . ? C21 O11 H11B 107(3) . . ? O11 C21 H21C 114.2(15) . . ? O11 C21 H21A 115.9(17) . . ? H21C C21 H21A 104(2) . . ? O11 C21 H21B 109.1(16) . . ? H21C C21 H21B 108(2) . . ? H21A C21 H21B 104(2) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 29.26 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.502 _refine_diff_density_min -1.064 _refine_diff_density_rms 0.090 # Attachment 'compound 9 [Ag2(L4n)(NO3)2]25.cif' data_l4nagno3 _database_code_depnum_ccdc_archive 'CCDC 849912' #TrackingRef 'compound 9 [Ag2(L4n)(NO3)2]25.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'bisnicotinate tetraethyleneglycol' _chemical_melting_point ? _chemical_formula_moiety 'C40 H48 Ag4 N4 O14,4(N1 O3)' _chemical_formula_sum 'C40 H48 Ag4 N8 O26' _chemical_formula_weight 1488.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.9254(16) _cell_length_b 7.9338(10) _cell_length_c 31.910(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.243(13) _cell_angle_gamma 90.00 _cell_volume 2512.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9663 _cell_measurement_theta_min 1.95 _cell_measurement_theta_max 27.07 _exptl_crystal_description needle _exptl_crystal_colour white _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.968 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 1.635 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8208 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; after another XR measurement with a bigger exposition time, it is not possible to avoid the disordered part of the molecule ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17935 _diffrn_reflns_av_R_equivalents 0.1859 _diffrn_reflns_av_sigmaI/netI 0.1690 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 26.74 _reflns_number_total 5298 _reflns_number_gt 2635 _reflns_threshold_expression >2\s(I) _computing_data_collection Xarea _computing_cell_refinement Xarea _computing_data_reduction Xarea _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics diamond _computing_publication_material word _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. atoms C8, C9, C10, C11 and O3 are refined isotropically because of the disorder induced by the big torsion angle in this part of the molecule ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5298 _refine_ls_number_parameters 327 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1907 _refine_ls_R_factor_gt 0.0961 _refine_ls_wR_factor_ref 0.1782 _refine_ls_wR_factor_gt 0.1530 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.126 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag -0.56094(9) 0.83541(14) -0.02466(3) 0.0420(3) Uani 1 1 d . . . Ag2 Ag 0.38239(10) 0.10284(14) 0.16733(3) 0.0473(3) Uani 1 1 d . . . O2 O -0.0112(8) 0.5317(15) 0.0734(3) 0.067(3) Uani 1 1 d . . . O1 O -0.0159(8) 0.6890(15) 0.0140(3) 0.064(3) Uani 1 1 d . . . O3 O 0.1762(17) 0.388(2) 0.1388(6) 0.123(5) Uiso 1 1 d . . . O4 O 0.1524(8) 0.0902(12) 0.1917(3) 0.048(2) Uani 1 1 d . . . O5 O 0.3525(8) -0.1517(13) 0.2121(2) 0.049(2) Uani 1 1 d . . . O6 O 0.6187(7) -0.1925(10) 0.1702(2) 0.0313(18) Uani 1 1 d . . . O7 O 0.8328(8) -0.2045(12) 0.1948(3) 0.052(3) Uani 1 1 d . . . O8 O 0.7376(9) 0.3717(13) 0.1761(3) 0.062(3) Uani 1 1 d . . . O9 O 0.6467(11) 0.1486(13) 0.1981(3) 0.069(3) Uani 1 1 d . . . O10 O 0.5259(10) 0.3291(15) 0.1669(4) 0.089(4) Uani 1 1 d . . . O11 O -0.3796(11) 0.878(2) -0.0829(3) 0.082(4) Uani 1 1 d . . . O12 O -0.2814(9) 1.0598(17) -0.0439(3) 0.079(4) Uani 1 1 d . . . O13 O -0.3010(12) 1.0997(16) -0.1095(3) 0.079(4) Uani 1 1 d . . . N1 N -0.4359(9) 0.7082(12) 0.0207(3) 0.034(2) Uani 1 1 d . . . N2 N 0.7191(9) 0.0662(12) 0.0654(3) 0.033(2) Uani 1 1 d . . . N3 N -0.3192(12) 1.014(2) -0.0787(4) 0.063(4) Uani 1 1 d . . . N4 N 0.6381(11) 0.2827(15) 0.1802(3) 0.044(3) Uani 1 1 d . . . C1 C -0.3009(10) 0.6974(15) 0.0174(3) 0.031(3) Uani 1 1 d . . . H1 H -0.2602 0.7504 -0.0051 0.038 Uiso 1 1 calc R . . C2 C -0.2201(10) 0.6099(15) 0.0463(3) 0.030(3) Uani 1 1 d . . . C3 C -0.2810(11) 0.5302(15) 0.0798(3) 0.032(3) Uani 1 1 d . . . H2 H -0.2297 0.4727 0.0999 0.038 Uiso 1 1 calc R . . C4 C -0.4183(12) 0.5386(17) 0.0824(4) 0.043(3) Uani 1 1 d . . . H3 H -0.4622 0.4839 0.1040 0.051 Uiso 1 1 calc R . . C5 C -0.4905(11) 0.6286(18) 0.0529(4) 0.044(3) Uani 1 1 d . . . H4 H -0.5835 0.6344 0.0556 0.053 Uiso 1 1 calc R . . C6 C -0.0730(11) 0.6162(18) 0.0417(4) 0.043(3) Uani 1 1 d . . . C9 C 0.084(2) 0.345(3) 0.1498(6) 0.096(6) Uiso 1 1 d . . . H9 H 0.0473 0.2671 0.1291 0.115 Uiso 1 1 calc R . . H10 H 0.0235 0.4404 0.1507 0.115 Uiso 1 1 calc R . . C10 C 0.0796(15) 0.246(2) 0.1976(5) 0.063(4) Uiso 1 1 d . . . H11 H -0.0125 0.2246 0.2055 0.075 Uiso 1 1 calc R . . H12 H 0.1231 0.3149 0.2191 0.075 Uiso 1 1 calc R . . C11 C 0.1378(14) -0.028(2) 0.2244(4) 0.061(4) Uani 1 1 d . . . H13 H 0.0431 -0.0508 0.2287 0.073 Uiso 1 1 calc R . . H14 H 0.1766 0.0164 0.2503 0.073 Uiso 1 1 calc R . . C12 C 0.2089(12) -0.187(2) 0.2124(4) 0.060(5) Uani 1 1 d . . . H15 H 0.1905 -0.2755 0.2325 0.072 Uiso 1 1 calc R . . H16 H 0.1778 -0.2241 0.1849 0.072 Uiso 1 1 calc R . . C13 C 0.4273(13) -0.3028(18) 0.2043(4) 0.051(4) Uani 1 1 d . . . H17 H 0.4064 -0.3430 0.1762 0.061 Uiso 1 1 calc R . . H18 H 0.4013 -0.3895 0.2239 0.061 Uiso 1 1 calc R . . C14 C 0.5749(12) -0.2709(17) 0.2087(4) 0.044(3) Uani 1 1 d . . . H19 H 0.5933 -0.1970 0.2324 0.053 Uiso 1 1 calc R . . H20 H 0.6227 -0.3761 0.2134 0.053 Uiso 1 1 calc R . . C15 C 0.7511(12) -0.1631(16) 0.1684(4) 0.040(3) Uani 1 1 d . . . C16 C 0.7862(10) -0.0787(15) 0.1293(3) 0.031(3) Uani 1 1 d . . . C17 C 0.9211(11) -0.0635(16) 0.1172(4) 0.041(3) Uani 1 1 d . . . H21 H 0.9902 -0.1050 0.1344 0.049 Uiso 1 1 calc R . . C18 C 0.9510(12) 0.0132(18) 0.0794(4) 0.049(4) Uani 1 1 d . . . H22 H 1.0398 0.0215 0.0710 0.059 Uiso 1 1 calc R . . C19 C 0.8483(10) 0.0767(16) 0.0547(4) 0.035(3) Uani 1 1 d . . . H23 H 0.8692 0.1290 0.0296 0.042 Uiso 1 1 calc R . . C20 C 0.6881(10) -0.0092(14) 0.1019(3) 0.027(3) Uani 1 1 d . . . H24 H 0.5981 -0.0155 0.1092 0.032 Uiso 1 1 calc R . . C8 C 0.186(3) 0.448(4) 0.1033(9) 0.137(9) Uiso 1 1 d . . . H7 H 0.2202 0.3492 0.0892 0.165 Uiso 1 1 calc R . . H8 H 0.2650 0.5174 0.1082 0.165 Uiso 1 1 calc R . . C7 C 0.1355(18) 0.526(3) 0.0711(6) 0.091(6) Uiso 1 1 d . . . H5 H 0.1611 0.4684 0.0457 0.109 Uiso 1 1 calc R . . H6 H 0.1710 0.6399 0.0702 0.109 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0331(5) 0.0577(7) 0.0349(5) 0.0050(5) -0.0087(4) 0.0081(5) Ag2 0.0502(6) 0.0495(7) 0.0427(6) -0.0059(5) 0.0102(4) -0.0189(5) O2 0.031(5) 0.131(10) 0.039(5) 0.040(6) 0.008(4) 0.031(5) O1 0.032(5) 0.105(9) 0.054(6) 0.039(6) -0.003(4) 0.005(5) O4 0.040(5) 0.061(6) 0.043(5) -0.011(5) 0.009(4) -0.015(5) O5 0.037(5) 0.076(7) 0.034(5) 0.008(5) -0.004(4) -0.019(5) O6 0.034(4) 0.031(5) 0.029(4) 0.008(4) -0.009(3) -0.001(4) O7 0.044(5) 0.066(7) 0.045(5) 0.019(5) -0.030(4) -0.012(5) O8 0.051(6) 0.075(8) 0.059(6) 0.005(5) -0.005(5) -0.024(5) O9 0.107(8) 0.028(6) 0.072(7) 0.014(5) 0.010(6) 0.001(5) O10 0.056(6) 0.065(8) 0.144(11) 0.054(8) -0.030(7) -0.024(6) O11 0.051(7) 0.142(13) 0.051(7) 0.019(8) -0.002(5) 0.010(7) O12 0.052(6) 0.151(12) 0.033(5) -0.011(6) -0.015(4) 0.030(6) O13 0.120(9) 0.097(9) 0.019(5) 0.022(6) 0.016(5) 0.022(7) N1 0.036(5) 0.036(6) 0.030(5) 0.002(5) -0.006(4) -0.010(5) N2 0.034(5) 0.032(6) 0.031(5) -0.002(5) -0.007(4) -0.001(4) N3 0.029(7) 0.124(14) 0.035(7) -0.013(8) -0.007(5) 0.030(7) N4 0.048(7) 0.048(8) 0.036(6) 0.004(5) -0.001(5) -0.012(6) C1 0.021(5) 0.038(8) 0.034(6) 0.010(5) 0.004(5) 0.002(5) C2 0.029(6) 0.031(7) 0.031(6) -0.001(5) 0.003(5) 0.007(5) C3 0.041(7) 0.034(7) 0.019(6) 0.006(5) -0.002(5) -0.001(5) C4 0.038(7) 0.049(9) 0.041(7) 0.009(6) 0.003(6) -0.006(6) C5 0.027(6) 0.064(10) 0.042(7) -0.001(7) -0.007(5) -0.001(6) C6 0.031(6) 0.062(10) 0.035(7) 0.021(7) -0.001(5) 0.012(6) C11 0.054(9) 0.105(14) 0.024(7) 0.008(8) -0.001(6) -0.017(9) C12 0.035(7) 0.092(13) 0.053(8) 0.030(9) -0.015(6) -0.036(8) C13 0.058(9) 0.052(10) 0.041(8) 0.006(7) -0.003(6) -0.012(8) C14 0.055(8) 0.035(8) 0.041(7) 0.011(6) 0.000(6) -0.007(6) C15 0.048(7) 0.021(7) 0.049(8) 0.005(6) -0.016(6) -0.008(6) C16 0.029(6) 0.032(7) 0.032(6) -0.007(5) -0.010(5) -0.002(5) C17 0.023(6) 0.041(8) 0.059(8) 0.007(7) -0.015(6) -0.003(5) C18 0.024(6) 0.069(10) 0.053(8) 0.018(8) 0.001(6) -0.006(6) C19 0.021(6) 0.043(8) 0.040(7) -0.012(6) 0.002(5) -0.003(5) C20 0.020(5) 0.024(7) 0.036(6) 0.005(5) -0.006(5) -0.003(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.140(9) . ? Ag1 N2 2.163(9) 3_565 ? Ag1 Ag1 3.268(2) 3_475 ? Ag2 O10 2.292(10) . ? Ag2 O4 2.430(8) . ? Ag2 O5 2.495(9) . ? Ag2 O13 2.565(12) 3_565 ? O2 C6 1.351(14) . ? O2 C7 1.460(19) . ? O1 C6 1.208(14) . ? O3 C9 1.04(2) . ? O3 C8 1.23(3) . ? O4 C11 1.414(16) . ? O4 C10 1.449(17) . ? O5 C13 1.435(16) . ? O5 C12 1.452(13) . ? O6 C15 1.337(13) . ? O6 C14 1.452(13) . ? O7 C15 1.203(13) . ? O8 N4 1.224(12) . ? O9 N4 1.210(13) . ? O10 N4 1.239(14) . ? O11 N3 1.240(18) . ? O12 N3 1.222(14) . ? O13 N3 1.211(16) . ? O13 Ag2 2.565(12) 3_565 ? N1 C5 1.331(15) . ? N1 C1 1.349(13) . ? N2 C19 1.337(13) . ? N2 C20 1.349(14) . ? N2 Ag1 2.163(9) 3_565 ? C1 C2 1.394(15) . ? C1 H1 0.9300 . ? C2 C3 1.392(15) . ? C2 C6 1.471(15) . ? C3 C4 1.369(15) . ? C3 H2 0.9300 . ? C4 C5 1.371(17) . ? C4 H3 0.9300 . ? C5 H4 0.9300 . ? C9 C10 1.71(2) . ? C9 H9 0.9700 . ? C9 H10 0.9700 . ? C10 H11 0.9700 . ? C10 H12 0.9700 . ? C11 C12 1.50(2) . ? C11 H13 0.9700 . ? C11 H14 0.9700 . ? C12 H15 0.9700 . ? C12 H16 0.9700 . ? C13 C14 1.490(17) . ? C13 H17 0.9700 . ? C13 H18 0.9700 . ? C14 H19 0.9700 . ? C14 H20 0.9700 . ? C15 C16 1.464(16) . ? C16 C20 1.407(14) . ? C16 C17 1.407(15) . ? C17 C18 1.387(17) . ? C17 H21 0.9300 . ? C18 C19 1.371(16) . ? C18 H22 0.9300 . ? C19 H23 0.9300 . ? C20 H24 0.9300 . ? C8 C7 1.29(3) . ? C8 H7 0.9700 . ? C8 H8 0.9700 . ? C7 H5 0.9700 . ? C7 H6 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N2 168.6(4) . 3_565 ? N1 Ag1 Ag1 81.2(2) . 3_475 ? N2 Ag1 Ag1 104.9(3) 3_565 3_475 ? O10 Ag2 O4 128.5(4) . . ? O10 Ag2 O5 136.0(3) . . ? O4 Ag2 O5 70.1(3) . . ? O10 Ag2 O13 132.3(4) . 3_565 ? O4 Ag2 O13 85.5(3) . 3_565 ? O5 Ag2 O13 82.2(3) . 3_565 ? C6 O2 C7 114.5(11) . . ? C9 O3 C8 121(2) . . ? C11 O4 C10 114.4(10) . . ? C11 O4 Ag2 112.1(8) . . ? C10 O4 Ag2 118.7(8) . . ? C13 O5 C12 110.6(11) . . ? C13 O5 Ag2 120.6(7) . . ? C12 O5 Ag2 106.8(7) . . ? C15 O6 C14 115.1(9) . . ? N4 O10 Ag2 108.6(8) . . ? N3 O13 Ag2 100.4(10) . 3_565 ? C5 N1 C1 117.0(10) . . ? C5 N1 Ag1 120.4(8) . . ? C1 N1 Ag1 122.6(8) . . ? C19 N2 C20 119.1(9) . . ? C19 N2 Ag1 120.7(8) . 3_565 ? C20 N2 Ag1 120.2(7) . 3_565 ? O13 N3 O12 121.6(17) . . ? O13 N3 O11 118.8(13) . . ? O12 N3 O11 119.7(16) . . ? O9 N4 O8 120.6(12) . . ? O9 N4 O10 118.5(11) . . ? O8 N4 O10 120.9(12) . . ? N1 C1 C2 122.5(10) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C3 C2 C1 118.8(9) . . ? C3 C2 C6 122.7(10) . . ? C1 C2 C6 118.4(10) . . ? C4 C3 C2 118.3(10) . . ? C4 C3 H2 120.8 . . ? C2 C3 H2 120.8 . . ? C5 C4 C3 119.3(11) . . ? C5 C4 H3 120.3 . . ? C3 C4 H3 120.3 . . ? N1 C5 C4 124.1(11) . . ? N1 C5 H4 117.9 . . ? C4 C5 H4 117.9 . . ? O1 C6 O2 125.0(10) . . ? O1 C6 C2 124.9(10) . . ? O2 C6 C2 110.1(10) . . ? O3 C9 C10 119(2) . . ? O3 C9 H9 107.5 . . ? C10 C9 H9 107.5 . . ? O3 C9 H10 107.5 . . ? C10 C9 H10 107.5 . . ? H9 C9 H10 107.0 . . ? C9 C10 O4 104.5(12) . . ? C9 C10 H11 110.8 . . ? O4 C10 H11 110.8 . . ? C9 C10 H12 110.8 . . ? O4 C10 H12 110.8 . . ? H11 C10 H12 108.9 . . ? O4 C11 C12 108.3(11) . . ? O4 C11 H13 110.0 . . ? C12 C11 H13 110.0 . . ? O4 C11 H14 110.0 . . ? C12 C11 H14 110.0 . . ? H13 C11 H14 108.4 . . ? O5 C12 C11 107.9(12) . . ? O5 C12 H15 110.1 . . ? C11 C12 H15 110.1 . . ? O5 C12 H16 110.1 . . ? C11 C12 H16 110.1 . . ? H15 C12 H16 108.4 . . ? O5 C13 C14 110.7(11) . . ? O5 C13 H17 109.5 . . ? C14 C13 H17 109.5 . . ? O5 C13 H18 109.5 . . ? C14 C13 H18 109.5 . . ? H17 C13 H18 108.1 . . ? O6 C14 C13 107.7(10) . . ? O6 C14 H19 110.2 . . ? C13 C14 H19 110.2 . . ? O6 C14 H20 110.2 . . ? C13 C14 H20 110.2 . . ? H19 C14 H20 108.5 . . ? O7 C15 O6 124.7(11) . . ? O7 C15 C16 123.6(11) . . ? O6 C15 C16 111.6(9) . . ? C20 C16 C17 116.4(10) . . ? C20 C16 C15 122.3(10) . . ? C17 C16 C15 121.3(10) . . ? C18 C17 C16 120.0(11) . . ? C18 C17 H21 120.0 . . ? C16 C17 H21 120.0 . . ? C19 C18 C17 119.4(11) . . ? C19 C18 H22 120.3 . . ? C17 C18 H22 120.3 . . ? N2 C19 C18 122.3(11) . . ? N2 C19 H23 118.8 . . ? C18 C19 H23 118.8 . . ? N2 C20 C16 122.8(10) . . ? N2 C20 H24 118.6 . . ? C16 C20 H24 118.6 . . ? O3 C8 C7 152(3) . . ? O3 C8 H7 98.7 . . ? C7 C8 H7 98.7 . . ? O3 C8 H8 98.7 . . ? C7 C8 H8 98.7 . . ? H7 C8 H8 103.9 . . ? C8 C7 O2 110.0(18) . . ? C8 C7 H5 109.7 . . ? O2 C7 H5 109.7 . . ? C8 C7 H6 109.7 . . ? O2 C7 H6 109.7 . . ? H5 C7 H6 108.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O10 Ag2 O4 C11 -120.1(9) . . . . ? O5 Ag2 O4 C11 13.4(8) . . . . ? O13 Ag2 O4 C11 96.8(9) 3_565 . . . ? O10 Ag2 O4 C10 16.8(10) . . . . ? O5 Ag2 O4 C10 150.4(9) . . . . ? O13 Ag2 O4 C10 -126.3(9) 3_565 . . . ? O10 Ag2 O5 C13 -86.5(10) . . . . ? O4 Ag2 O5 C13 148.2(8) . . . . ? O13 Ag2 O5 C13 60.2(8) 3_565 . . . ? O10 Ag2 O5 C12 146.2(9) . . . . ? O4 Ag2 O5 C12 20.9(8) . . . . ? O13 Ag2 O5 C12 -67.1(9) 3_565 . . . ? O4 Ag2 O10 N4 134.9(9) . . . . ? O5 Ag2 O10 N4 33.5(13) . . . . ? O13 Ag2 O10 N4 -99.2(10) 3_565 . . . ? N2 Ag1 N1 C5 -17(2) 3_565 . . . ? Ag1 Ag1 N1 C5 106.2(9) 3_475 . . . ? N2 Ag1 N1 C1 159.4(16) 3_565 . . . ? Ag1 Ag1 N1 C1 -77.0(9) 3_475 . . . ? Ag2 O13 N3 O12 173.4(10) 3_565 . . . ? Ag2 O13 N3 O11 -7.8(14) 3_565 . . . ? Ag2 O10 N4 O9 -14.6(15) . . . . ? Ag2 O10 N4 O8 166.9(9) . . . . ? C5 N1 C1 C2 -1.0(17) . . . . ? Ag1 N1 C1 C2 -177.9(9) . . . . ? N1 C1 C2 C3 0.2(18) . . . . ? N1 C1 C2 C6 -175.4(11) . . . . ? C1 C2 C3 C4 1.3(17) . . . . ? C6 C2 C3 C4 176.6(12) . . . . ? C2 C3 C4 C5 -1.9(18) . . . . ? C1 N1 C5 C4 0.4(18) . . . . ? Ag1 N1 C5 C4 177.3(10) . . . . ? C3 C4 C5 N1 1(2) . . . . ? C7 O2 C6 O1 -3(2) . . . . ? C7 O2 C6 C2 178.2(13) . . . . ? C3 C2 C6 O1 -177.2(13) . . . . ? C1 C2 C6 O1 -2(2) . . . . ? C3 C2 C6 O2 1.6(18) . . . . ? C1 C2 C6 O2 177.0(11) . . . . ? C8 O3 C9 C10 174(2) . . . . ? O3 C9 C10 O4 -67(3) . . . . ? C11 O4 C10 C9 -167.4(11) . . . . ? Ag2 O4 C10 C9 56.6(13) . . . . ? C10 O4 C11 C12 175.5(10) . . . . ? Ag2 O4 C11 C12 -45.6(12) . . . . ? C13 O5 C12 C11 175.1(10) . . . . ? Ag2 O5 C12 C11 -51.9(11) . . . . ? O4 C11 C12 O5 67.4(13) . . . . ? C12 O5 C13 C14 -173.5(10) . . . . ? Ag2 O5 C13 C14 60.9(12) . . . . ? C15 O6 C14 C13 -176.9(11) . . . . ? O5 C13 C14 O6 -80.1(13) . . . . ? C14 O6 C15 O7 4.1(18) . . . . ? C14 O6 C15 C16 -178.0(10) . . . . ? O7 C15 C16 C20 -170.3(12) . . . . ? O6 C15 C16 C20 11.8(16) . . . . ? O7 C15 C16 C17 9.9(19) . . . . ? O6 C15 C16 C17 -168.1(11) . . . . ? C20 C16 C17 C18 -1.5(18) . . . . ? C15 C16 C17 C18 178.4(12) . . . . ? C16 C17 C18 C19 1(2) . . . . ? C20 N2 C19 C18 0.1(17) . . . . ? Ag1 N2 C19 C18 -178.8(10) 3_565 . . . ? C17 C18 C19 N2 -1(2) . . . . ? C19 N2 C20 C16 -0.3(16) . . . . ? Ag1 N2 C20 C16 178.6(8) 3_565 . . . ? C17 C16 C20 N2 1.0(17) . . . . ? C15 C16 C20 N2 -178.8(11) . . . . ? C9 O3 C8 C7 28(7) . . . . ? O3 C8 C7 O2 -14(7) . . . . ? C6 O2 C7 C8 177.9(19) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.74 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.314 _refine_diff_density_min -1.166 _refine_diff_density_rms 0.181 # Attachment 'compound 3 [Ag(L3i)OSCF3]4.cif' data_comp3defp21np21c _database_code_depnum_ccdc_archive 'CCDC 884807' #TrackingRef 'compound 3 [Ag(L3i)OSCF3]4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'bisisonicotinate triethyleneglycol' _chemical_melting_point ? _chemical_formula_moiety 'C18 H20 Ag N2 O6,C F3 O3 S' _chemical_formula_sum 'C19 H20 Ag F3 N2 O9 S' _chemical_formula_weight 617.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.930(5) _cell_length_b 14.200(5) _cell_length_c 20.264(5) _cell_angle_alpha 90.00 _cell_angle_beta 116.134(15) _cell_angle_gamma 90.00 _cell_volume 2306.9(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour 'transparent yellow grey' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.777 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 1.042 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; cell measurement_felns_used, cell measurement_theta_min and max are missing because the measure was made in 2004 and lxr and cfx are lost, the time of the measurement was counted because only one XR machine was accessible for all the departement so the completness is only of 0.986 and the coverage of 22.61. The absorption correction is low (mu x r is near 1) and after verification with/without absorption correction in this case does not change the R values. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5859 _diffrn_reflns_av_R_equivalents 0.1645 _diffrn_reflns_av_sigmaI/netI 0.1732 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 22.61 _reflns_number_total 3017 _reflns_number_gt 1485 _reflns_threshold_expression >2\s(I) _computing_data_collection Xarea _computing_cell_refinement Xarea _computing_data_reduction Xarea _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics diamond _computing_publication_material word _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+9.0600P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3017 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1910 _refine_ls_R_factor_gt 0.0810 _refine_ls_wR_factor_ref 0.1354 _refine_ls_wR_factor_gt 0.1033 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.022 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag -1.88800(13) -0.23947(9) -0.92913(7) 0.0595(4) Uani 1 1 d . . . O5 O -0.4969(10) -0.3810(7) -0.8189(5) 0.055(3) Uani 1 1 d . . . O6 O -0.6033(13) -0.4607(9) -0.9245(6) 0.086(4) Uani 1 1 d . . . O4 O -0.6687(10) -0.2648(8) -0.7660(5) 0.056(3) Uani 1 1 d . . . O3 O -0.8181(13) -0.0975(8) -0.8009(7) 0.081(4) Uani 1 1 d . . . O2 O -1.1392(11) -0.0398(7) -0.9002(5) 0.053(3) Uani 1 1 d . . . O1 O -1.2580(12) -0.0615(7) -1.0235(6) 0.061(3) Uani 1 1 d . . . N2 N -0.0959(12) -0.2953(7) -0.9156(7) 0.041(3) Uani 1 1 d . . . N1 N -1.6733(13) -0.1841(8) -0.9387(6) 0.046(3) Uani 1 1 d . . . C14 C -0.2222(17) -0.3403(11) -0.9683(8) 0.055(4) Uani 1 1 d . . . H14 H -0.2216 -0.3469 -1.0139 0.065 Uiso 1 1 calc R . . C15 C -0.3556(15) -0.3782(10) -0.9591(7) 0.044(4) Uani 1 1 d . . . H15 H -0.4422 -0.4088 -0.9977 0.052 Uiso 1 1 calc R . . C16 C -0.3565(16) -0.3695(9) -0.8920(8) 0.035(4) Uani 1 1 d . . . C17 C -0.2278(15) -0.3227(9) -0.8378(7) 0.043(4) Uani 1 1 d . . . H17 H -0.2270 -0.3144 -0.7921 0.051 Uiso 1 1 calc R . . C18 C -0.0982(15) -0.2874(9) -0.8504(8) 0.046(4) Uani 1 1 d . . . H18 H -0.0100 -0.2572 -0.8122 0.055 Uiso 1 1 calc R . . C13 C -0.5008(18) -0.4093(11) -0.8811(9) 0.048(4) Uani 1 1 d . . . C12 C -0.6364(16) -0.4121(11) -0.8061(8) 0.059(4) Uani 1 1 d . . . H12A H -0.6287 -0.4791 -0.7958 0.070 Uiso 1 1 calc R . . H12B H -0.7411 -0.3994 -0.8487 0.070 Uiso 1 1 calc R . . C11 C -0.6251(19) -0.3573(13) -0.7413(9) 0.070(5) Uani 1 1 d . . . H11A H -0.7012 -0.3826 -0.7234 0.084 Uiso 1 1 calc R . . H11B H -0.5127 -0.3597 -0.7019 0.084 Uiso 1 1 calc R . . C10 C -0.6688(18) -0.2094(13) -0.7108(9) 0.069(5) Uani 1 1 d . . . H10A H -0.5645 -0.2172 -0.6669 0.083 Uiso 1 1 calc R . . H10B H -0.7592 -0.2282 -0.6993 0.083 Uiso 1 1 calc R . . C9 C -0.690(2) -0.1115(16) -0.7340(11) 0.099(7) Uani 1 1 d . . . H9A H -0.7075 -0.0739 -0.6981 0.119 Uiso 1 1 calc R . . H9B H -0.5875 -0.0898 -0.7348 0.119 Uiso 1 1 calc R . . C8 C -0.848(2) 0.0003(13) -0.8265(9) 0.083(6) Uani 1 1 d . . . H8A H -0.7483 0.0270 -0.8269 0.099 Uiso 1 1 calc R . . H8B H -0.8787 0.0382 -0.7945 0.099 Uiso 1 1 calc R . . C7 C -0.9889(17) -0.0025(10) -0.9035(9) 0.060(5) Uani 1 1 d . . . H7A H -1.0106 0.0604 -0.9244 0.072 Uiso 1 1 calc R . . H7B H -0.9585 -0.0423 -0.9346 0.072 Uiso 1 1 calc R . . C6 C -1.2624(17) -0.0652(10) -0.9647(9) 0.046(4) Uani 1 1 d . . . C3 C -1.4070(16) -0.1069(8) -0.9535(9) 0.040(4) Uani 1 1 d . . . C4 C -1.4061(17) -0.1139(11) -0.8869(8) 0.053(4) Uani 1 1 d . . . H4 H -1.3141 -0.0926 -0.8454 0.063 Uiso 1 1 calc R . . C5 C -1.5382(18) -0.1517(11) -0.8798(8) 0.053(4) Uani 1 1 d . . . H5 H -1.5354 -0.1553 -0.8334 0.064 Uiso 1 1 calc R . . C1 C -1.6736(14) -0.1786(9) -1.0046(8) 0.048(4) Uani 1 1 d . . . H1 H -1.7663 -0.2004 -1.0456 0.057 Uiso 1 1 calc R . . C2 C -1.5406(16) -0.1417(10) -1.0140(8) 0.051(4) Uani 1 1 d . . . H2 H -1.5419 -0.1405 -1.0601 0.061 Uiso 1 1 calc R . . S1 S -1.0974(4) -0.3030(3) -1.1451(2) 0.0542(11) Uani 1 1 d . . . F3 F -1.0246(14) -0.4613(8) -1.0764(8) 0.137(5) Uani 1 1 d . . . F1 F -0.8195(10) -0.3973(7) -1.0848(6) 0.107(4) Uani 1 1 d . . . F2 F -1.0074(17) -0.4640(10) -1.1784(9) 0.165(7) Uani 1 1 d . . . O7 O -1.0708(12) -0.2662(9) -1.0758(6) 0.091(4) Uani 1 1 d . . . O9 O -1.2621(11) -0.3325(9) -1.1935(6) 0.102(4) Uani 1 1 d . . . O8 O -1.0100(10) -0.2510(8) -1.1773(5) 0.079(3) Uani 1 1 d . . . C19 C -0.982(2) -0.4135(14) -1.1241(14) 0.085(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0511(6) 0.0587(8) 0.0845(9) 0.0098(9) 0.0445(6) -0.0039(7) O5 0.044(6) 0.064(7) 0.069(8) 0.000(6) 0.035(6) -0.009(5) O6 0.091(9) 0.104(10) 0.074(9) -0.037(8) 0.047(7) -0.067(8) O4 0.065(6) 0.074(8) 0.040(6) -0.014(7) 0.034(5) -0.016(6) O3 0.067(8) 0.057(9) 0.087(10) -0.011(7) 0.005(7) 0.015(6) O2 0.041(6) 0.055(7) 0.062(7) 0.005(6) 0.023(6) -0.012(5) O1 0.077(7) 0.070(8) 0.055(7) 0.000(6) 0.045(6) -0.014(6) N2 0.039(7) 0.036(7) 0.059(8) 0.011(7) 0.031(7) 0.008(6) N1 0.061(8) 0.056(9) 0.034(8) 0.008(7) 0.032(7) 0.007(7) C14 0.050(10) 0.068(12) 0.039(10) -0.007(9) 0.013(9) -0.005(9) C15 0.025(8) 0.053(10) 0.029(10) -0.010(8) -0.009(7) -0.014(7) C16 0.039(9) 0.038(9) 0.027(9) -0.006(7) 0.012(8) 0.004(7) C17 0.041(8) 0.052(10) 0.043(10) -0.012(8) 0.026(8) -0.012(8) C18 0.048(9) 0.036(10) 0.059(10) -0.001(8) 0.028(8) -0.018(7) C13 0.053(11) 0.051(11) 0.057(12) -0.006(9) 0.040(10) -0.013(9) C12 0.066(11) 0.054(11) 0.072(12) 0.014(10) 0.046(9) -0.001(8) C11 0.077(12) 0.073(14) 0.069(13) 0.021(11) 0.041(11) 0.010(10) C10 0.054(10) 0.085(15) 0.083(14) 0.017(12) 0.043(10) 0.014(9) C9 0.087(15) 0.13(2) 0.070(15) -0.040(15) 0.024(13) -0.026(15) C8 0.081(13) 0.078(15) 0.093(15) -0.028(12) 0.040(12) -0.028(11) C7 0.063(10) 0.028(10) 0.095(15) -0.002(9) 0.041(10) 0.001(8) C6 0.037(9) 0.039(10) 0.055(12) 0.001(9) 0.015(9) 0.001(7) C3 0.032(8) 0.017(8) 0.084(13) 0.011(8) 0.037(10) 0.011(7) C4 0.047(10) 0.081(12) 0.040(10) 0.008(9) 0.028(9) -0.004(9) C5 0.063(11) 0.068(12) 0.037(11) 0.003(9) 0.029(9) -0.001(9) C1 0.026(8) 0.046(10) 0.058(11) -0.006(8) 0.006(7) -0.004(7) C2 0.043(9) 0.061(11) 0.046(11) 0.018(9) 0.016(8) -0.011(8) S1 0.049(2) 0.072(3) 0.047(3) 0.011(2) 0.025(2) 0.003(2) F3 0.133(10) 0.092(9) 0.177(13) 0.059(10) 0.059(9) 0.002(7) F1 0.050(6) 0.086(8) 0.152(10) 0.031(8) 0.013(6) 0.020(5) F2 0.169(13) 0.114(12) 0.218(17) -0.080(12) 0.091(12) 0.000(10) O7 0.112(9) 0.103(10) 0.073(7) -0.009(9) 0.056(7) -0.011(8) O9 0.040(6) 0.134(11) 0.101(9) 0.007(9) 0.003(7) 0.002(7) O8 0.074(6) 0.087(8) 0.086(7) 0.041(8) 0.043(6) 0.015(7) C19 0.032(11) 0.082(16) 0.13(2) 0.031(15) 0.021(12) 0.010(10) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.145(10) 1_355 ? Ag1 N1 2.158(10) . ? O5 C13 1.308(16) . ? O5 C12 1.448(13) . ? O6 C13 1.197(16) . ? O4 C10 1.368(16) . ? O4 C11 1.398(18) . ? O3 C9 1.351(19) . ? O3 C8 1.466(18) . ? O2 C6 1.334(16) . ? O2 C7 1.472(14) . ? O1 C6 1.212(16) . ? N2 C14 1.327(15) . ? N2 C18 1.335(15) . ? N2 Ag1 2.145(9) 1_755 ? N1 C1 1.337(15) . ? N1 C5 1.350(16) . ? C14 C15 1.393(16) . ? C14 H14 0.9300 . ? C15 C16 1.371(17) . ? C15 H15 0.9300 . ? C16 C17 1.362(16) . ? C16 C13 1.510(17) . ? C17 C18 1.384(15) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C12 C11 1.490(19) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C10 C9 1.45(2) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C8 C7 1.515(19) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C6 C3 1.525(17) . ? C3 C4 1.350(18) . ? C3 C2 1.372(17) . ? C4 C5 1.361(17) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C1 C2 1.386(16) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? S1 O7 1.417(10) . ? S1 O9 1.425(10) . ? S1 O8 1.424(9) . ? S1 C19 1.824(18) . ? F3 C19 1.37(2) . ? F1 C19 1.329(17) . ? F2 C19 1.25(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N1 178.0(5) 1_355 . ? C13 O5 C12 114.7(11) . . ? C10 O4 C11 110.3(12) . . ? C9 O3 C8 115.8(15) . . ? C6 O2 C7 115.3(11) . . ? C14 N2 C18 117.4(11) . . ? C14 N2 Ag1 123.5(10) . 1_755 ? C18 N2 Ag1 119.1(9) . 1_755 ? C1 N1 C5 118.1(12) . . ? C1 N1 Ag1 120.0(10) . . ? C5 N1 Ag1 121.9(9) . . ? N2 C14 C15 123.5(13) . . ? N2 C14 H14 118.2 . . ? C15 C14 H14 118.2 . . ? C16 C15 C14 118.5(13) . . ? C16 C15 H15 120.8 . . ? C14 C15 H15 120.8 . . ? C17 C16 C15 118.2(13) . . ? C17 C16 C13 122.5(13) . . ? C15 C16 C13 119.3(13) . . ? C16 C17 C18 120.4(13) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? N2 C18 C17 122.0(13) . . ? N2 C18 H18 119.0 . . ? C17 C18 H18 119.0 . . ? O6 C13 O5 125.7(13) . . ? O6 C13 C16 123.1(14) . . ? O5 C13 C16 111.3(13) . . ? O5 C12 C11 105.6(12) . . ? O5 C12 H12A 110.6 . . ? C11 C12 H12A 110.6 . . ? O5 C12 H12B 110.6 . . ? C11 C12 H12B 110.6 . . ? H12A C12 H12B 108.7 . . ? O4 C11 C12 105.9(13) . . ? O4 C11 H11A 110.5 . . ? C12 C11 H11A 110.5 . . ? O4 C11 H11B 110.5 . . ? C12 C11 H11B 110.5 . . ? H11A C11 H11B 108.7 . . ? O4 C10 C9 109.4(15) . . ? O4 C10 H10A 109.8 . . ? C9 C10 H10A 109.8 . . ? O4 C10 H10B 109.8 . . ? C9 C10 H10B 109.8 . . ? H10A C10 H10B 108.3 . . ? O3 C9 C10 113.3(16) . . ? O3 C9 H9A 108.9 . . ? C10 C9 H9A 108.9 . . ? O3 C9 H9B 108.9 . . ? C10 C9 H9B 108.9 . . ? H9A C9 H9B 107.7 . . ? O3 C8 C7 106.2(13) . . ? O3 C8 H8A 110.5 . . ? C7 C8 H8A 110.5 . . ? O3 C8 H8B 110.5 . . ? C7 C8 H8B 110.5 . . ? H8A C8 H8B 108.7 . . ? O2 C7 C8 108.9(12) . . ? O2 C7 H7A 109.9 . . ? C8 C7 H7A 109.9 . . ? O2 C7 H7B 109.9 . . ? C8 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? O1 C6 O2 125.6(13) . . ? O1 C6 C3 124.0(14) . . ? O2 C6 C3 110.3(13) . . ? C4 C3 C2 119.1(13) . . ? C4 C3 C6 123.0(14) . . ? C2 C3 C6 117.8(14) . . ? C5 C4 C3 120.8(15) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 N1 121.3(14) . . ? C4 C5 H5 119.3 . . ? N1 C5 H5 119.3 . . ? N1 C1 C2 122.3(13) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C3 C2 C1 118.3(13) . . ? C3 C2 H2 120.9 . . ? C1 C2 H2 120.9 . . ? O7 S1 O9 117.5(7) . . ? O7 S1 O8 112.1(7) . . ? O9 S1 O8 116.4(7) . . ? O7 S1 C19 104.8(10) . . ? O9 S1 C19 102.4(9) . . ? O8 S1 C19 100.6(8) . . ? F2 C19 F1 111.0(18) . . ? F2 C19 F3 109.8(18) . . ? F1 C19 F3 103.5(17) . . ? F2 C19 S1 115.0(16) . . ? F1 C19 S1 110.3(14) . . ? F3 C19 S1 106.5(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ag1 N1 C1 162(12) 1_355 . . . ? N2 Ag1 N1 C5 -20(13) 1_355 . . . ? C18 N2 C14 C15 1(2) . . . . ? Ag1 N2 C14 C15 178.7(10) 1_755 . . . ? N2 C14 C15 C16 -1(2) . . . . ? C14 C15 C16 C17 1(2) . . . . ? C14 C15 C16 C13 179.4(13) . . . . ? C15 C16 C17 C18 -2(2) . . . . ? C13 C16 C17 C18 -180.0(12) . . . . ? C14 N2 C18 C17 -1.2(19) . . . . ? Ag1 N2 C18 C17 -179.3(10) 1_755 . . . ? C16 C17 C18 N2 2(2) . . . . ? C12 O5 C13 O6 -4(2) . . . . ? C12 O5 C13 C16 176.8(11) . . . . ? C17 C16 C13 O6 -170.2(15) . . . . ? C15 C16 C13 O6 12(2) . . . . ? C17 C16 C13 O5 9(2) . . . . ? C15 C16 C13 O5 -168.9(13) . . . . ? C13 O5 C12 C11 -169.1(13) . . . . ? C10 O4 C11 C12 177.5(11) . . . . ? O5 C12 C11 O4 71.2(14) . . . . ? C11 O4 C10 C9 171.5(13) . . . . ? C8 O3 C9 C10 178.5(14) . . . . ? O4 C10 C9 O3 50(2) . . . . ? C9 O3 C8 C7 176.6(14) . . . . ? C6 O2 C7 C8 -166.2(13) . . . . ? O3 C8 C7 O2 62.4(16) . . . . ? C7 O2 C6 O1 1(2) . . . . ? C7 O2 C6 C3 177.3(10) . . . . ? O1 C6 C3 C4 177.1(15) . . . . ? O2 C6 C3 C4 1.3(18) . . . . ? O1 C6 C3 C2 0(2) . . . . ? O2 C6 C3 C2 -176.3(12) . . . . ? C2 C3 C4 C5 -2(2) . . . . ? C6 C3 C4 C5 -180.0(13) . . . . ? C3 C4 C5 N1 1(2) . . . . ? C1 N1 C5 C4 0(2) . . . . ? Ag1 N1 C5 C4 -177.6(11) . . . . ? C5 N1 C1 C2 0(2) . . . . ? Ag1 N1 C1 C2 178.5(10) . . . . ? C4 C3 C2 C1 3(2) . . . . ? C6 C3 C2 C1 -179.2(12) . . . . ? N1 C1 C2 C3 -2(2) . . . . ? O7 S1 C19 F2 170.4(15) . . . . ? O9 S1 C19 F2 47.2(18) . . . . ? O8 S1 C19 F2 -73.2(17) . . . . ? O7 S1 C19 F1 -63.2(17) . . . . ? O9 S1 C19 F1 173.6(15) . . . . ? O8 S1 C19 F1 53.3(17) . . . . ? O7 S1 C19 F3 48.5(15) . . . . ? O9 S1 C19 F3 -74.7(16) . . . . ? O8 S1 C19 F3 165.0(13) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 22.61 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.785 _refine_diff_density_min -0.635 _refine_diff_density_rms 0.117