Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Muthu, Sebastian' 'Vittal, Jagadese J.' 'Yip, John H. K.' _publ_contact_author_name 'Dr John H K Yip' _publ_contact_author_address ; Department of Chemistry The National University of Singapore 10 Kent Ridge Crescent 119260 SINGAPORE ; _publ_contact_author_email 'CHMYIPHK@NUS.EDU.SG' _publ_section_title ; Coordination Polymers of d10 Metals and N,N'-Bis(3-Pyridinecarboxamide)-1,2-Ethane ; data_99145 _database_code_CSD 171770 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H14 Ag Cl N4 O6' _chemical_formula_weight 477.61 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' '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' 'Cl' 'Cl' 0.1484 0.1585 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c 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 5.1132(2) _cell_length_b 13.2742(3) _cell_length_c 24.2679(7) _cell_angle_alpha 90.00 _cell_angle_beta 95.284(1) _cell_angle_gamma 90.00 _cell_volume 1640.2(1) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4305 _cell_measurement_theta_min 2.06 _cell_measurement_theta_max 25.0 _exptl_crystal_description 'rectangular shape, cut' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.934 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 1.434 _exptl_absorpt_correction_type 'sadabs (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.7108 _exptl_absorpt_correction_T_max 0.9422 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _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 ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4189 _diffrn_reflns_av_R_equivalents 0.0163 _diffrn_reflns_av_sigmaI/netI 0.0181 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1441 _reflns_number_gt 1376 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS, SMART' _computing_cell_refinement 'Bruker AXS, SAINT' _computing_data_reduction 'Bruker AXS, SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS, SHELXTL' _computing_publication_material 'Bruker AXS, SHELXTL' _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^ > 2sigma(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^)+(0.0263P)^2^+4.2225P] 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 SHELXL _refine_ls_extinction_coef 0.0008(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1441 _refine_ls_number_parameters 137 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0269 _refine_ls_R_factor_gt 0.0253 _refine_ls_wR_factor_ref 0.0634 _refine_ls_wR_factor_gt 0.0625 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.101 _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 0.0000 0.34455(2) 0.2500 0.04085(15) Uani 1 2 d S . . N1 N 0.1992(5) 0.34133(16) 0.17565(9) 0.0298(5) Uani 1 1 d . . . C1 C 0.3893(5) 0.4075(2) 0.16751(11) 0.0326(6) Uani 1 1 d . . . H1 H 0.4109 0.4633 0.1907 0.039 Uiso 1 1 calc R . . C2 C 0.5535(6) 0.3963(2) 0.12626(12) 0.0351(6) Uani 1 1 d . . . H2A H 0.6869 0.4426 0.1223 0.042 Uiso 1 1 calc R . . C3 C 0.5178(5) 0.3150(2) 0.09055(12) 0.0340(6) Uani 1 1 d . . . H3 H 0.6262 0.3061 0.0622 0.041 Uiso 1 1 calc R . . C4 C 0.3181(5) 0.24756(19) 0.09785(11) 0.0264(5) Uani 1 1 d . . . C5 C 0.1638(5) 0.26320(19) 0.14102(11) 0.0280(5) Uani 1 1 d . . . H5 H 0.0302 0.2175 0.1461 0.034 Uiso 1 1 calc R . . C6 C 0.2539(5) 0.1594(2) 0.06064(14) 0.0384(7) Uani 1 1 d . . . O1 O 0.0257(4) 0.13129(17) 0.05020(11) 0.0498(6) Uani 1 1 d . . . N2 N 0.4563(5) 0.1156(3) 0.03988(17) 0.0779(13) Uani 1 1 d D . . H2 H 0.6191 0.1412 0.0496 0.094 Uiso 1 1 calc R . . C7 C 0.4242(10) 0.0458(4) -0.0098(2) 0.0305(10) Uani 0.60 1 d PD . . H7A H 0.485(7) 0.066(3) -0.0424(13) 0.049(10) Uiso 1 1 d D . . H7B H 0.256(7) 0.017(3) -0.0156(17) 0.098(16) Uiso 1 1 d D . . C7A C 0.4351(14) -0.0003(6) 0.0262(3) 0.0344(16) Uani 0.40 1 d PD . . Cl1 Cl 0.0000 0.61579(7) 0.2500 0.0381(2) Uani 1 2 d SD . . O2 O 0.1610(6) 0.5537(2) 0.28707(13) 0.0726(8) Uani 1 1 d D . . O3 O 0.1611(5) 0.6782(2) 0.21943(12) 0.0679(8) Uani 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 0.0474(2) 0.0471(2) 0.0307(2) 0.000 0.01824(14) 0.000 N1 0.0326(12) 0.0296(11) 0.0284(11) -0.0018(9) 0.0093(9) 0.0006(9) C1 0.0374(15) 0.0285(13) 0.0320(14) -0.0080(11) 0.0040(11) -0.0017(11) C2 0.0353(15) 0.0331(14) 0.0381(16) -0.0057(12) 0.0100(12) -0.0108(12) C3 0.0292(14) 0.0391(15) 0.0353(15) -0.0083(12) 0.0124(11) -0.0032(12) C4 0.0219(12) 0.0269(13) 0.0305(13) -0.0056(10) 0.0023(10) 0.0019(10) C5 0.0248(13) 0.0261(12) 0.0334(14) -0.0004(11) 0.0051(10) -0.0010(10) C6 0.0225(13) 0.0393(16) 0.0537(18) -0.0210(14) 0.0057(12) -0.0011(11) O1 0.0224(10) 0.0549(13) 0.0728(16) -0.0333(12) 0.0077(10) -0.0071(9) N2 0.0194(12) 0.078(2) 0.137(3) -0.085(2) 0.0109(15) -0.0056(13) C7 0.031(3) 0.029(2) 0.032(3) -0.009(2) 0.002(2) 0.001(2) C7A 0.030(4) 0.029(4) 0.046(5) -0.016(4) 0.014(4) -0.004(3) Cl1 0.0328(5) 0.0255(5) 0.0546(6) 0.000 -0.0038(4) 0.000 O2 0.0704(17) 0.0533(15) 0.089(2) 0.0187(14) -0.0173(15) 0.0183(13) O3 0.0607(16) 0.0674(17) 0.0754(19) 0.0128(14) 0.0057(14) -0.0208(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 2.153(2) . ? Ag1 N1 2.153(2) 2 ? N1 C5 1.337(3) . ? N1 C1 1.338(4) . ? C1 C2 1.373(4) . ? C2 C3 1.385(4) . ? C3 C4 1.382(4) . ? C4 C5 1.384(4) . ? C4 C6 1.496(4) . ? C6 O1 1.229(3) . ? C6 N2 1.327(4) . ? N2 C7 1.516(5) . ? N2 C7A 1.575(7) . ? C7 C7A 1.047(8) 5_655 ? C7 C7A 1.064(9) . ? C7 C7 1.497(10) 5_655 ? C7A C7 1.047(8) 5_655 ? C7A C7A 1.489(15) 5_655 ? Cl1 O3 1.424(3) . ? Cl1 O3 1.424(3) 2 ? Cl1 O2 1.424(2) 2 ? Cl1 O2 1.424(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 N1 Ag1 N1 177.72(11) . 2 ? C5 N1 C1 118.3(2) . . ? C5 N1 Ag1 119.70(17) . . ? C1 N1 Ag1 121.12(18) . . ? N1 C1 C2 122.5(2) . . ? C1 C2 C3 119.1(3) . . ? C4 C3 C2 118.7(2) . . ? C3 C4 C5 118.6(2) . . ? C3 C4 C6 123.6(2) . . ? C5 C4 C6 117.7(2) . . ? N1 C5 C4 122.6(2) . . ? O1 C6 N2 123.2(3) . . ? O1 C6 C4 120.9(2) . . ? N2 C6 C4 115.9(2) . . ? C6 N2 C7 122.6(3) . . ? C6 N2 C7A 117.9(4) . . ? C7 N2 C7A 40.2(3) . . ? C7A C7 C7A 89.7(8) 5_655 . ? C7A C7 C7 45.3(6) 5_655 5_655 ? C7A C7 C7 44.4(5) . 5_655 ? C7A C7 N2 128.9(6) 5_655 . ? C7A C7 N2 72.8(5) . . ? C7 C7 N2 103.3(5) 5_655 . ? C7 C7A C7 90.3(8) 5_655 . ? C7 C7A C7A 45.6(5) 5_655 5_655 ? C7 C7A C7A 44.7(5) . 5_655 ? C7 C7A N2 127.4(6) 5_655 . ? C7 C7A N2 66.9(5) . . ? C7A C7A N2 98.5(7) 5_655 . ? O3 Cl1 O3 108.8(3) . 2 ? O3 Cl1 O2 109.63(18) . 2 ? O3 Cl1 O2 109.70(18) 2 2 ? O3 Cl1 O2 109.70(18) . . ? O3 Cl1 O2 109.63(18) 2 . ? O2 Cl1 O2 109.3(3) 2 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.525 _refine_diff_density_min -0.541 _refine_diff_density_rms 0.062 data_019 _database_code_CSD 171771 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H14 Ag Cl N4 O6' _chemical_formula_weight 477.61 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' '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' 'Cl' 'Cl' 0.1484 0.1585 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c 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 24.0654(6) _cell_length_b 5.1239(1) _cell_length_c 13.9276(2) _cell_angle_alpha 90.00 _cell_angle_beta 110.757(1) _cell_angle_gamma 90.00 _cell_volume 1605.92(6) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 4030 _cell_measurement_theta_min 2.06 _cell_measurement_theta_max 25.0 _exptl_crystal_description 'hexagonal plates' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.975 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 1.465 _exptl_absorpt_correction_type 'sadabs (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.6300 _exptl_absorpt_correction_T_max 0.8971 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3923 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0268 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1408 _reflns_number_gt 1321 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS, SMART' _computing_cell_refinement 'Bruker AXS, SAINT' _computing_data_reduction 'Bruker AXS, SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS, SHELXTL' _computing_publication_material 'Bruker AXS, SHELXTL' _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^ > 2sigma(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^)+(0.0341P)^2^+2.7290P] 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 SHELXL _refine_ls_extinction_coef 0.0009(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1408 _refine_ls_number_parameters 121 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0254 _refine_ls_R_factor_gt 0.0231 _refine_ls_wR_factor_ref 0.0637 _refine_ls_wR_factor_gt 0.0625 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 0.0000 0.0000 0.0000 0.02665(15) Uani 1 2 d S . . Cl1 Cl 0.0000 -0.08795(18) 0.2500 0.0245(2) Uani 1 2 d S . . O1 O -0.03943(14) 0.0727(6) 0.1725(2) 0.0662(8) Uani 1 1 d . . . O2 O 0.03288(10) -0.2454(4) 0.20424(18) 0.0467(6) Uani 1 1 d . . . O3 O -0.20160(9) -0.2368(3) -0.34653(14) 0.0302(4) Uani 1 1 d . . . N1 N -0.06955(9) -0.3008(4) -0.05949(15) 0.0199(4) Uani 1 1 d . . . C1 C -0.07715(12) -0.4887(4) 0.0023(2) 0.0226(6) Uani 1 1 d . . . H1 H -0.0525 -0.4891 0.0710 0.027 Uiso 1 1 calc R . . C2 C -0.11990(11) -0.6807(5) -0.03192(19) 0.0234(5) Uani 1 1 d . . . H2 H -0.1240 -0.8070 0.0131 0.028 Uiso 1 1 calc R . . C3 C -0.15666(10) -0.6824(5) -0.13435(18) 0.0205(5) Uani 1 1 d . . . H3 H -0.1853 -0.8119 -0.1594 0.025 Uiso 1 1 calc R . . C4 C -0.15011(11) -0.4879(4) -0.19892(19) 0.0172(5) Uani 1 1 d . . . C5 C -0.10593(10) -0.3023(5) -0.15820(17) 0.0186(5) Uani 1 1 d . . . H5 H -0.1013 -0.1725 -0.2015 0.022 Uiso 1 1 calc R . . C6 C -0.19071(11) -0.4567(4) -0.30880(19) 0.0197(5) Uani 1 1 d . . . C7 C -0.26013(12) -0.6717(5) -0.46309(18) 0.0259(6) Uani 1 1 d . . . H7A H -0.2677 -0.4930 -0.4871 0.031 Uiso 1 1 calc R . . H7B H -0.2969 -0.7444 -0.4611 0.031 Uiso 1 1 calc R . . N2 N -0.21507(10) -0.6746(4) -0.35944(15) 0.0254(5) Uani 1 1 d . . . H2A H -0.2038 -0.8226 -0.3299 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 Ag1 0.0275(2) 0.0274(2) 0.01919(19) -0.00448(10) 0.00111(13) -0.01338(11) Cl1 0.0328(5) 0.0250(4) 0.0148(4) 0.000 0.0074(4) 0.000 O1 0.080(2) 0.0789(17) 0.0385(14) 0.0333(14) 0.0200(14) 0.0403(16) O2 0.0456(13) 0.0486(13) 0.0518(14) -0.0137(11) 0.0247(11) 0.0052(11) O3 0.0392(11) 0.0152(9) 0.0232(9) 0.0024(7) -0.0050(8) -0.0018(8) N1 0.0206(10) 0.0191(10) 0.0165(10) -0.0016(8) 0.0021(8) -0.0025(8) C1 0.0227(13) 0.0237(13) 0.0152(12) 0.0006(9) -0.0009(10) 0.0012(9) C2 0.0260(13) 0.0211(12) 0.0200(12) 0.0046(10) 0.0046(10) -0.0029(10) C3 0.0200(12) 0.0165(11) 0.0211(12) -0.0009(9) 0.0023(10) -0.0035(9) C4 0.0180(12) 0.0158(12) 0.0152(12) -0.0023(8) 0.0027(10) 0.0018(8) C5 0.0219(12) 0.0156(11) 0.0158(11) -0.0004(9) 0.0037(9) -0.0007(9) C6 0.0214(13) 0.0172(12) 0.0160(12) 0.0006(9) 0.0010(10) 0.0000(9) C7 0.0293(13) 0.0218(12) 0.0182(12) -0.0004(10) -0.0019(10) -0.0017(11) N2 0.0377(12) 0.0136(10) 0.0144(10) -0.0006(8) -0.0038(9) -0.0009(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 2.2092(19) . ? Ag1 N1 2.2092(19) 5 ? Cl1 O1 1.420(2) 2 ? Cl1 O1 1.420(2) . ? Cl1 O2 1.429(2) . ? Cl1 O2 1.429(2) 2 ? O3 C6 1.231(3) . ? N1 C5 1.343(3) . ? N1 C1 1.346(3) . ? C1 C2 1.381(4) . ? C2 C3 1.387(3) . ? C3 C4 1.388(3) . ? C4 C5 1.389(3) . ? C4 C6 1.504(3) . ? C6 N2 1.340(3) . ? C7 N2 1.466(3) . ? C7 C7 1.514(5) 7_434 ? 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 N1 180.00(8) . 5 ? O1 Cl1 O1 109.2(3) 2 . ? O1 Cl1 O2 109.86(16) 2 . ? O1 Cl1 O2 108.35(15) . . ? O1 Cl1 O2 108.35(15) 2 2 ? O1 Cl1 O2 109.86(16) . 2 ? O2 Cl1 O2 111.2(2) . 2 ? C5 N1 C1 117.6(2) . . ? C5 N1 Ag1 121.36(15) . . ? C1 N1 Ag1 121.05(16) . . ? N1 C1 C2 122.9(2) . . ? C1 C2 C3 119.0(2) . . ? C2 C3 C4 119.0(2) . . ? C3 C4 C5 118.3(2) . . ? C3 C4 C6 123.6(2) . . ? C5 C4 C6 118.0(2) . . ? N1 C5 C4 123.3(2) . . ? O3 C6 N2 123.4(2) . . ? O3 C6 C4 119.7(2) . . ? N2 C6 C4 116.9(2) . . ? N2 C7 C7 111.1(3) . 7_434 ? C6 N2 C7 122.9(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.418 _refine_diff_density_min -0.274 _refine_diff_density_rms 0.073 data_030 _database_code_CSD 171772 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H14 Ag F3 N4 O5 S' _chemical_formula_weight 527.23 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' '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' 'F' 'F' 0.0171 0.0103 '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' 'Ag' 'Ag' -0.8971 1.1015 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1297(1) _cell_length_b 9.6318(1) _cell_length_c 9.8647(1) _cell_angle_alpha 86.833(1) _cell_angle_beta 87.100(1) _cell_angle_gamma 89.493(1) _cell_volume 865.01(2) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.06 _cell_measurement_theta_max 25.0 _exptl_crystal_description 'plate, cut' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.024 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 524 _exptl_absorpt_coefficient_mu 1.357 _exptl_absorpt_correction_type 'sadabs (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.3957 _exptl_absorpt_correction_T_max 0.8100 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6364 _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_av_sigmaI/netI 0.0361 _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 -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3021 _reflns_number_gt 2801 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS, SMART' _computing_cell_refinement 'Bruker AXS, SAINT' _computing_data_reduction 'Bruker AXS, SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS, SHELXTL' _computing_publication_material 'Bruker AXS, SHELXTL' _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^ > 2sigma(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^)+(0.0444P)^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 SHELXL _refine_ls_extinction_coef 0.0016(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3021 _refine_ls_number_parameters 319 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0268 _refine_ls_R_factor_gt 0.0253 _refine_ls_wR_factor_ref 0.0670 _refine_ls_wR_factor_gt 0.0666 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.009 _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 0.48153(2) 0.497689(16) 0.247036(16) 0.02126(10) Uani 1 1 d . . . S1 S 0.06453(7) 0.59077(6) 0.23022(6) 0.02178(15) Uani 1 1 d . . . O1 O 0.72147(18) 0.06785(18) -0.22514(16) 0.0224(4) Uani 1 1 d . . . O2 O 0.27562(18) 0.92010(18) 0.72522(16) 0.0231(4) Uani 1 1 d . . . O3 O -0.0132(2) 0.69171(19) 0.3088(2) 0.0357(5) Uani 1 1 d . . . O4 O 0.0683(3) 0.6153(3) 0.0869(2) 0.0613(8) Uani 1 1 d . . . O5 O 0.2023(2) 0.5462(2) 0.2832(3) 0.0519(6) Uani 1 1 d . . . C1 C 0.3402(3) 0.3371(3) 0.0280(2) 0.0212(5) Uani 1 1 d . . . H1 H 0.263(3) 0.392(3) 0.054(3) 0.016(6) Uiso 1 1 d . . . C2 C 0.3249(3) 0.2455(3) -0.0730(3) 0.0220(5) Uani 1 1 d . . . H2 H 0.236(4) 0.237(3) -0.109(3) 0.042(9) Uiso 1 1 d . . . C3 C 0.4440(3) 0.1671(3) -0.1157(2) 0.0193(5) Uani 1 1 d . . . H3 H 0.439(3) 0.102(3) -0.179(3) 0.021(7) Uiso 1 1 d . . . C4 C 0.5780(2) 0.1827(2) -0.0554(2) 0.0149(4) Uani 1 1 d . . . C5 C 0.5846(3) 0.2772(2) 0.0450(2) 0.0167(5) Uani 1 1 d . . . H5 H 0.675(3) 0.284(3) 0.081(3) 0.021(7) Uiso 1 1 d . . . C6 C 0.7103(2) 0.1029(2) -0.1061(2) 0.0159(5) Uani 1 1 d . . . N1 N 0.4692(2) 0.3534(2) 0.0877(2) 0.0185(4) Uani 1 1 d . . . C7 C 0.9495(3) 0.0050(3) -0.0583(2) 0.0188(5) Uani 1 1 d . . . H7A H 0.996(3) 0.065(3) -0.133(3) 0.019(6) Uiso 1 1 d . . . H7B H 0.928(3) -0.080(3) -0.085(3) 0.023(7) Uiso 1 1 d . . . C8 C 0.6531(3) 0.6627(3) 0.4528(3) 0.0221(5) Uani 1 1 d . . . H8 H 0.732(3) 0.616(3) 0.423(3) 0.026(7) Uiso 1 1 d . . . C9 C 0.6731(3) 0.7549(3) 0.5525(3) 0.0239(5) Uani 1 1 d . . . H9 H 0.763(4) 0.769(3) 0.572(3) 0.045(10) Uiso 1 1 d . . . C10 C 0.5552(3) 0.8296(3) 0.6039(2) 0.0198(5) Uani 1 1 d . . . H10 H 0.563(3) 0.898(3) 0.667(3) 0.011(6) Uiso 1 1 d . . . C11 C 0.4179(2) 0.8097(2) 0.5512(2) 0.0148(5) Uani 1 1 d . . . C12 C 0.4057(3) 0.7146(2) 0.4522(2) 0.0162(5) Uani 1 1 d . . . H12 H 0.308(3) 0.704(3) 0.422(3) 0.017(6) Uiso 1 1 d . . . C13 C 0.2858(3) 0.8870(2) 0.6055(2) 0.0159(5) Uani 1 1 d . . . N2 N 0.5209(2) 0.6409(2) 0.4024(2) 0.0176(4) Uani 1 1 d . . . C14 C 0.0467(3) 0.9870(3) 0.5606(2) 0.0185(5) Uani 1 1 d . . . H14A H 0.075(3) 1.072(3) 0.598(3) 0.028(7) Uiso 1 1 d . . . H14B H -0.007(3) 0.923(3) 0.629(3) 0.020(7) Uiso 1 1 d . . . C15 C -0.0450(3) 0.4328(3) 0.2625(3) 0.0240(5) Uani 1 1 d D . . F1 F -0.0613(2) 0.3990(2) 0.39380(18) 0.0524(5) Uani 1 1 d D . . F2 F -0.17894(17) 0.45088(19) 0.2161(2) 0.0463(5) Uani 1 1 d D . . F3 F 0.01571(18) 0.32440(15) 0.20220(17) 0.0350(4) Uani 1 1 d D . . N3 N 0.8125(2) 0.0721(2) -0.0169(2) 0.0167(4) Uani 1 1 d . . . H3' H 0.799(3) 0.085(3) 0.051(3) 0.006(7) Uiso 1 1 d . . . N4 N 0.1822(2) 0.9172(2) 0.5177(2) 0.0174(4) Uani 1 1 d . . . H4 H 0.199(3) 0.907(3) 0.447(3) 0.013(7) 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 0.02690(14) 0.01981(13) 0.01740(14) -0.00614(8) 0.00020(8) 0.00501(8) S1 0.0189(3) 0.0217(3) 0.0251(3) -0.0075(2) 0.0020(2) -0.0033(2) O1 0.0243(9) 0.0306(9) 0.0128(9) -0.0061(7) -0.0020(7) 0.0045(7) O2 0.0247(9) 0.0327(10) 0.0125(9) -0.0066(7) -0.0019(7) 0.0063(7) O3 0.0327(11) 0.0244(10) 0.0503(13) -0.0135(9) 0.0071(9) 0.0030(8) O4 0.108(2) 0.0474(14) 0.0277(12) -0.0010(10) 0.0084(13) -0.0374(14) O5 0.0186(10) 0.0514(14) 0.0900(19) -0.0347(13) -0.0133(11) 0.0030(9) C1 0.0180(12) 0.0214(12) 0.0235(13) 0.0000(10) 0.0025(10) 0.0035(10) C2 0.0127(12) 0.0274(13) 0.0260(13) 0.0000(10) -0.0040(10) -0.0003(9) C3 0.0213(13) 0.0200(12) 0.0171(12) -0.0011(10) -0.0042(9) -0.0017(9) C4 0.0156(11) 0.0156(11) 0.0131(11) 0.0019(9) -0.0003(8) 0.0001(8) C5 0.0189(12) 0.0170(11) 0.0143(11) -0.0017(9) -0.0025(9) 0.0007(9) C6 0.0174(11) 0.0159(11) 0.0143(12) -0.0011(9) 0.0001(9) -0.0006(9) N1 0.0208(10) 0.0174(10) 0.0172(10) -0.0010(8) -0.0004(8) 0.0028(8) C7 0.0185(12) 0.0226(13) 0.0158(12) -0.0070(10) -0.0005(10) 0.0063(9) C8 0.0168(12) 0.0239(12) 0.0253(13) -0.0014(10) 0.0016(10) 0.0039(10) C9 0.0147(13) 0.0287(14) 0.0286(14) -0.0011(11) -0.0045(10) -0.0006(10) C10 0.0212(13) 0.0198(12) 0.0190(12) -0.0012(10) -0.0058(10) -0.0006(9) C11 0.0160(11) 0.0160(11) 0.0123(11) 0.0008(9) -0.0007(8) 0.0010(9) C12 0.0165(12) 0.0180(11) 0.0141(11) -0.0005(9) -0.0022(9) 0.0026(9) C13 0.0172(12) 0.0156(11) 0.0150(12) -0.0014(9) -0.0005(9) 0.0000(9) N2 0.0178(10) 0.0186(10) 0.0164(10) -0.0015(8) -0.0008(7) 0.0025(7) C14 0.0170(12) 0.0243(13) 0.0146(12) -0.0056(10) -0.0007(10) 0.0080(9) C15 0.0212(13) 0.0227(13) 0.0278(14) -0.0032(10) 0.0016(10) 0.0007(10) F1 0.0878(15) 0.0410(10) 0.0265(9) 0.0018(8) 0.0139(9) -0.0151(10) F2 0.0185(8) 0.0473(11) 0.0756(13) -0.0191(9) -0.0079(8) -0.0052(7) F3 0.0394(9) 0.0223(8) 0.0435(10) -0.0112(7) 0.0051(7) 0.0021(7) N3 0.0193(11) 0.0232(11) 0.0079(11) -0.0041(8) 0.0005(8) 0.0045(8) N4 0.0181(10) 0.0260(11) 0.0083(11) -0.0052(8) -0.0003(8) 0.0066(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 2.162(2) . ? Ag1 N2 2.163(2) . ? Ag1 O5 2.598(2) . ? S1 O4 1.419(2) . ? S1 O3 1.4371(19) . ? S1 O5 1.440(2) . ? S1 C15 1.832(3) . ? O1 C6 1.239(3) . ? O2 C13 1.239(3) . ? C1 N1 1.357(3) . ? C1 C2 1.380(4) . ? C2 C3 1.380(4) . ? C3 C4 1.400(3) . ? C4 C5 1.385(3) . ? C4 C6 1.505(3) . ? C5 N1 1.343(3) . ? C6 N3 1.335(3) . ? C7 N3 1.453(3) . ? C7 C7 1.509(5) 2_755 ? C8 N2 1.351(3) . ? C8 C9 1.382(4) . ? C9 C10 1.379(4) . ? C10 C11 1.400(3) . ? C11 C12 1.384(3) . ? C11 C13 1.502(3) . ? C12 N2 1.351(3) . ? C13 N4 1.334(3) . ? C14 N4 1.458(3) . ? C14 C14 1.512(4) 2_576 ? C15 F1 1.320(3) . ? C15 F3 1.332(3) . ? C15 F2 1.334(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 N1 Ag1 N2 173.44(6) . . ? N1 Ag1 O5 97.77(7) . . ? N2 Ag1 O5 88.75(7) . . ? O4 S1 O3 116.35(16) . . ? O4 S1 O5 114.38(18) . . ? O3 S1 O5 114.29(14) . . ? O4 S1 C15 104.52(13) . . ? O3 S1 C15 103.65(12) . . ? O5 S1 C15 101.14(13) . . ? S1 O5 Ag1 150.21(17) . . ? N1 C1 C2 122.3(2) . . ? C1 C2 C3 119.5(2) . . ? C2 C3 C4 119.0(2) . . ? C5 C4 C3 118.0(2) . . ? C5 C4 C6 122.5(2) . . ? C3 C4 C6 119.4(2) . . ? N1 C5 C4 123.4(2) . . ? O1 C6 N3 122.5(2) . . ? O1 C6 C4 120.7(2) . . ? N3 C6 C4 116.8(2) . . ? C5 N1 C1 117.8(2) . . ? C5 N1 Ag1 122.65(16) . . ? C1 N1 Ag1 119.57(16) . . ? N3 C7 C7 110.1(2) . 2_755 ? N2 C8 C9 122.6(2) . . ? C10 C9 C8 119.9(2) . . ? C9 C10 C11 118.2(2) . . ? C12 C11 C10 118.8(2) . . ? C12 C11 C13 121.0(2) . . ? C10 C11 C13 120.1(2) . . ? N2 C12 C11 123.0(2) . . ? O2 C13 N4 122.7(2) . . ? O2 C13 C11 121.1(2) . . ? N4 C13 C11 116.2(2) . . ? C12 N2 C8 117.5(2) . . ? C12 N2 Ag1 117.96(15) . . ? C8 N2 Ag1 124.55(17) . . ? N4 C14 C14 109.3(2) . 2_576 ? F1 C15 F3 107.8(2) . . ? F1 C15 F2 107.2(2) . . ? F3 C15 F2 107.4(2) . . ? F1 C15 S1 111.30(18) . . ? F3 C15 S1 112.10(17) . . ? F2 C15 S1 110.90(18) . . ? C6 N3 C7 121.1(2) . . ? C13 N4 C14 120.9(2) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.786 _refine_diff_density_min -0.842 _refine_diff_density_rms 0.093 data_99171 _database_code_CSD 171773 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H16.50 Ag N5 O6.25' _chemical_formula_weight 462.69 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' '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' 'Ag' 'Ag' -0.8971 1.1015 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0861(1) _cell_length_b 9.5617(1) _cell_length_c 10.1841(1) _cell_angle_alpha 92.612(1) _cell_angle_beta 98.041(1) _cell_angle_gamma 97.386(1) _cell_volume 866.997(16) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6805 _cell_measurement_theta_min 2.06 _cell_measurement_theta_max 25.0 _exptl_crystal_description 'distorted hexagnal blocks' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.772 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 465 _exptl_absorpt_coefficient_mu 1.207 _exptl_absorpt_correction_type 'sadabs (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.7182 _exptl_absorpt_correction_T_max 0.8288 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _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 ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6347 _diffrn_reflns_av_R_equivalents 0.0148 _diffrn_reflns_av_sigmaI/netI 0.0216 _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 -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3000 _reflns_number_gt 2758 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS, SMART' _computing_cell_refinement 'Bruker AXS, SAINT' _computing_data_reduction 'Bruker AXS, SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS, SHELXTL' _computing_publication_material 'Bruker AXS, SHELXTL' _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^ > 2sigma(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^)+(0.0420P)^2^+0.4010P] 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 SHELXL _refine_ls_extinction_coef 0.0048(15) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3000 _refine_ls_number_parameters 258 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0284 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0716 _refine_ls_wR_factor_gt 0.0705 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.073 _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 0.52950(3) 0.26904(2) 0.496114(19) 0.05704(13) Uani 1 1 d . . . O1 O 0.7076(2) -0.18595(17) 0.93514(19) 0.0473(4) Uani 1 1 d . . . O2 O 0.2944(2) 0.68769(17) 0.03505(19) 0.0466(4) Uani 1 1 d . . . N1 N 0.4812(2) 0.1064(2) 0.6297(2) 0.0421(5) Uani 1 1 d . . . N2 N 0.8061(2) 0.0442(2) 0.9522(2) 0.0386(5) Uani 1 1 d . . . H2 H 0.7933 0.1283 0.9309 0.046 Uiso 1 1 calc R . . N3 N 0.5540(3) 0.4251(2) 0.3518(2) 0.0444(5) Uani 1 1 d . . . N4 N 0.1963(2) 0.4611(2) 0.0488(2) 0.0370(4) Uani 1 1 d . . . H4 H 0.2094 0.3813 0.0811 0.044 Uiso 1 1 calc R . . C1 C 0.3435(3) 0.0331(3) 0.6271(3) 0.0502(7) Uani 1 1 d . . . H1A H 0.2648 0.0543 0.5659 0.060 Uiso 1 1 calc R . . C2 C 0.3156(3) -0.0717(3) 0.7117(3) 0.0537(7) Uani 1 1 d . . . H2' H 0.2193 -0.1202 0.7072 0.064 Uiso 1 1 calc R . . C3 C 0.4308(3) -0.1051(3) 0.8037(3) 0.0432(6) Uani 1 1 d . . . H3 H 0.4140 -0.1767 0.8609 0.052 Uiso 1 1 calc R . . C4 C 0.5727(3) -0.0283(2) 0.8083(2) 0.0333(5) Uani 1 1 d . . . C5 C 0.5930(3) 0.0751(2) 0.7197(2) 0.0354(5) Uani 1 1 d . . . H5 H 0.6882 0.1252 0.7225 0.042 Uiso 1 1 calc R . . C6 C 0.7014(3) -0.0640(2) 0.9044(2) 0.0337(5) Uani 1 1 d . . . C7 C 0.9416(3) 0.0230(3) 1.0399(3) 0.0419(6) Uani 1 1 d . . . H7A H 0.9168 -0.0485 1.1008 0.050 Uiso 1 1 calc R . . H7B H 0.9824 0.1103 1.0919 0.050 Uiso 1 1 calc R . . C8 C 0.4332(3) 0.4461(2) 0.2663(2) 0.0370(5) Uani 1 1 d . . . H8 H 0.3419 0.3911 0.2701 0.044 Uiso 1 1 calc R . . C9 C 0.4396(3) 0.5468(2) 0.1725(2) 0.0331(5) Uani 1 1 d . . . C10 C 0.5756(3) 0.6308(3) 0.1689(3) 0.0418(5) Uani 1 1 d . . . H10 H 0.5831 0.7009 0.1089 0.050 Uiso 1 1 calc R . . C11 C 0.6994(3) 0.6078(3) 0.2565(3) 0.0521(7) Uani 1 1 d . . . H11A H 0.7917 0.6622 0.2553 0.062 Uiso 1 1 calc R . . C12 C 0.6861(3) 0.5051(3) 0.3448(3) 0.0521(7) Uani 1 1 d . . . H12 H 0.7709 0.4897 0.4019 0.063 Uiso 1 1 calc R . . C13 C 0.3032(3) 0.5710(2) 0.0799(2) 0.0333(5) Uani 1 1 d . . . C14 C 0.0573(3) 0.4725(3) -0.0386(3) 0.0411(5) Uani 1 1 d . . . H14A H 0.0162 0.3804 -0.0815 0.042(7) Uiso 1 1 calc R . . H14B H 0.0785 0.5360 -0.1073 0.054(8) Uiso 1 1 calc R . . O3 O 0.8234(3) 0.3468(4) 0.6315(3) 0.0850(8) Uani 1 1 d D . . H3A H 0.870(4) 0.426(3) 0.622(4) 0.080 Uiso 1 1 d D . . H3B H 0.892(4) 0.295(4) 0.624(4) 0.080 Uiso 1 1 d D . . N5 N 0.9124(3) 0.7450(3) 0.6044(4) 0.0814(10) Uani 1 1 d D . . O4 O 0.9729(4) 0.7997(5) 0.5055(4) 0.0824(11) Uani 0.65 1 d PD . . O5 O 0.8089(5) 0.8009(6) 0.6366(5) 0.0908(13) Uani 0.65 1 d PD . . O6 O 0.9601(7) 0.6393(6) 0.6406(8) 0.131(3) Uani 0.65 1 d PD . . O4A O 0.954(2) 0.6881(17) 0.6984(16) 0.166(4) Uiso 0.35 1 d PD . . O5A O 0.7877(15) 0.7184(17) 0.5726(16) 0.166(4) Uiso 0.35 1 d PD . . O6A O 0.9427(17) 0.8679(14) 0.6244(16) 0.166(4) Uiso 0.35 1 d PD . . O7 O 1.0302(12) 0.8872(12) 0.3565(11) 0.080(3) Uiso 0.25 1 d P . . 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 0.0906(2) 0.04899(16) 0.03583(15) 0.01533(9) 0.00188(10) 0.02935(12) O1 0.0577(10) 0.0278(9) 0.0580(11) 0.0158(8) 0.0038(8) 0.0125(7) O2 0.0589(11) 0.0289(9) 0.0536(11) 0.0144(8) 0.0021(8) 0.0144(7) N1 0.0524(12) 0.0409(11) 0.0343(11) 0.0050(9) -0.0009(9) 0.0183(9) N2 0.0386(10) 0.0275(10) 0.0495(12) 0.0098(8) -0.0028(9) 0.0111(8) N3 0.0547(13) 0.0443(12) 0.0350(11) 0.0068(9) -0.0025(9) 0.0179(10) N4 0.0385(10) 0.0286(10) 0.0449(11) 0.0110(8) -0.0007(8) 0.0123(8) C1 0.0448(14) 0.0598(17) 0.0462(15) 0.0002(13) -0.0057(11) 0.0221(12) C2 0.0371(13) 0.0613(18) 0.0620(18) 0.0028(14) 0.0047(12) 0.0071(12) C3 0.0424(13) 0.0389(13) 0.0494(15) 0.0080(11) 0.0084(11) 0.0055(10) C4 0.0364(11) 0.0281(11) 0.0371(12) 0.0043(9) 0.0056(9) 0.0100(9) C5 0.0393(12) 0.0320(11) 0.0355(12) 0.0067(9) 0.0019(9) 0.0095(9) C6 0.0397(12) 0.0288(11) 0.0361(12) 0.0106(9) 0.0081(9) 0.0125(9) C7 0.0423(13) 0.0417(13) 0.0413(13) 0.0080(11) -0.0040(10) 0.0134(10) C8 0.0458(13) 0.0331(12) 0.0333(12) 0.0065(9) 0.0021(10) 0.0120(9) C9 0.0389(12) 0.0297(11) 0.0328(11) 0.0030(9) 0.0059(9) 0.0120(9) C10 0.0476(13) 0.0394(13) 0.0404(13) 0.0057(10) 0.0102(10) 0.0084(10) C11 0.0378(13) 0.0632(18) 0.0551(16) 0.0016(14) 0.0076(12) 0.0064(12) C12 0.0455(15) 0.0636(18) 0.0467(15) 0.0003(13) -0.0046(11) 0.0188(13) C13 0.0432(12) 0.0288(11) 0.0319(11) 0.0069(9) 0.0077(9) 0.0155(9) C14 0.0411(12) 0.0412(13) 0.0407(13) 0.0066(11) -0.0033(10) 0.0137(10) O3 0.0707(17) 0.094(2) 0.0887(19) 0.0150(17) 0.0087(14) 0.0044(14) N5 0.0545(17) 0.074(2) 0.100(3) 0.0212(18) -0.0231(17) -0.0180(15) O4 0.070(2) 0.100(3) 0.087(3) 0.024(2) 0.033(2) 0.018(2) O5 0.080(3) 0.109(4) 0.098(3) 0.023(3) 0.043(2) 0.029(3) O6 0.096(3) 0.076(3) 0.215(8) 0.072(4) -0.024(4) 0.019(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 N3 2.155(2) . ? Ag1 N1 2.155(2) . ? O1 C6 1.227(3) . ? O2 C13 1.233(3) . ? N1 C5 1.343(3) . ? N1 C1 1.350(4) . ? N2 C6 1.335(3) . ? N2 C7 1.458(3) . ? N3 C8 1.345(3) . ? N3 C12 1.350(4) . ? N4 C13 1.330(3) . ? N4 C14 1.459(3) . ? C1 C2 1.373(4) . ? C2 C3 1.384(4) . ? C3 C4 1.393(4) . ? C4 C5 1.381(3) . ? C4 C6 1.502(3) . ? C7 C7 1.520(5) 2_757 ? C8 C9 1.389(3) . ? C9 C10 1.390(4) . ? C9 C13 1.498(3) . ? C10 C11 1.382(4) . ? C11 C12 1.367(4) . ? C14 C14 1.521(5) 2_565 ? N5 O5A 1.127(13) . ? N5 O4A 1.163(14) . ? N5 O6A 1.174(13) . ? N5 O6 1.202(5) . ? N5 O5 1.215(5) . ? N5 O4 1.311(5) . ? O4 O6A 1.426(16) . ? O5 O5A 0.981(15) . ? O5 O6A 1.324(16) . ? O6 O4A 0.75(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 N3 Ag1 N1 173.95(8) . . ? C5 N1 C1 117.9(2) . . ? C5 N1 Ag1 118.93(17) . . ? C1 N1 Ag1 123.16(17) . . ? C6 N2 C7 121.5(2) . . ? C8 N3 C12 118.2(2) . . ? C8 N3 Ag1 119.21(18) . . ? C12 N3 Ag1 122.56(17) . . ? C13 N4 C14 121.7(2) . . ? N1 C1 C2 122.3(2) . . ? C1 C2 C3 120.0(3) . . ? C2 C3 C4 118.1(2) . . ? C5 C4 C3 118.9(2) . . ? C5 C4 C6 121.4(2) . . ? C3 C4 C6 119.6(2) . . ? N1 C5 C4 122.9(2) . . ? O1 C6 N2 123.3(2) . . ? O1 C6 C4 120.9(2) . . ? N2 C6 C4 115.82(19) . . ? N2 C7 C7 110.8(3) . 2_757 ? N3 C8 C9 122.5(2) . . ? C8 C9 C10 118.6(2) . . ? C8 C9 C13 121.8(2) . . ? C10 C9 C13 119.6(2) . . ? C11 C10 C9 118.5(2) . . ? C12 C11 C10 119.9(3) . . ? N3 C12 C11 122.2(2) . . ? O2 C13 N4 123.0(2) . . ? O2 C13 C9 120.3(2) . . ? N4 C13 C9 116.76(19) . . ? N4 C14 C14 111.1(3) . 2_565 ? O5A N5 O4A 112.1(11) . . ? O5A N5 O6A 109.0(10) . . ? O4A N5 O6A 110.2(10) . . ? O5A N5 O6 108.1(9) . . ? O4A N5 O6 36.8(10) . . ? O6A N5 O6 138.7(8) . . ? O5A N5 O5 49.4(8) . . ? O4A N5 O5 103.4(11) . . ? O6A N5 O5 67.3(8) . . ? O6 N5 O5 130.3(5) . . ? O5A N5 O4 108.7(9) . . ? O4A N5 O4 136.1(11) . . ? O6A N5 O4 69.8(9) . . ? O6 N5 O4 114.0(5) . . ? O5 N5 O4 115.3(4) . . ? N5 O4 O6A 50.6(6) . . ? O5A O5 N5 60.6(9) . . ? O5A O5 O6A 107.8(12) . . ? N5 O5 O6A 54.9(6) . . ? O4A O6 N5 68.7(12) . . ? O6 O4A N5 74.5(14) . . ? O5 O5A N5 70.0(9) . . ? N5 O6A O5 57.9(7) . . ? N5 O6A O4 59.7(7) . . ? O5 O6A O4 101.9(9) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.397 _refine_diff_density_min -0.576 _refine_diff_density_rms 0.055 data_99210 _database_code_CSD 171774 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H39 Cl2 N9 O16 Zn' _chemical_formula_weight 917.97 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' '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tricliniic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.8536(2) _cell_length_b 12.2091(3) _cell_length_c 12.3860(2) _cell_angle_alpha 64.587(1) _cell_angle_beta 77.101(1) _cell_angle_gamma 80.065(1) _cell_volume 1041.67(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4940 _cell_measurement_theta_min 2.06 _cell_measurement_theta_max 25.0 _exptl_crystal_description 'rectangular shape, cut' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 474 _exptl_absorpt_coefficient_mu 0.795 _exptl_absorpt_correction_type 'sadabs (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.4445 _exptl_absorpt_correction_T_max 0.8880 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _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 ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6800 _diffrn_reflns_av_R_equivalents 0.0451 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 26.37 _reflns_number_total 4030 _reflns_number_gt 3593 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS, SMART' _computing_cell_refinement 'Bruker AXS, SAINT' _computing_data_reduction 'Bruker AXS, SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS, SHELXTL' _computing_publication_material 'Bruker AXS, SHELXTL' _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^ > 2sigma(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^)+(0.1098P)^2^+1.9220P] 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 4030 _refine_ls_number_parameters 293 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0711 _refine_ls_R_factor_gt 0.0646 _refine_ls_wR_factor_ref 0.1874 _refine_ls_wR_factor_gt 0.1798 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.060 _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 Zn1 Zn 0.0000 0.0000 0.0000 0.0252(2) Uani 1 2 d S . . O1 O -0.2647(4) -0.0329(3) 0.0103(3) 0.0304(6) Uani 1 1 d D . . H1A H -0.331(8) -0.084(5) 0.065(4) 0.08(2) Uiso 1 1 d D . . H1B H -0.283(7) -0.044(5) -0.050(4) 0.044(14) Uiso 1 1 d D . . O2 O -0.2863(4) -0.4347(3) 0.1845(3) 0.0437(7) Uani 1 1 d . . . O3 O 0.3315(5) -0.2269(4) 0.4022(3) 0.0694(13) Uani 1 1 d . . . N1 N 0.0966(4) -0.1948(3) 0.0399(3) 0.0280(7) Uani 1 1 d . . . N2 N -0.0533(4) -0.0479(3) 0.1924(3) 0.0278(7) Uani 1 1 d . . . N3 N -0.0972(5) -0.5936(3) 0.1763(3) 0.0328(7) Uani 1 1 d . . . H3 H 0.0095 -0.6195 0.1578 0.039 Uiso 1 1 calc R . . N4 N 0.1652(4) -0.2224(3) 0.5714(3) 0.0317(7) Uani 1 1 d . . . H4 H 0.0655 -0.2005 0.6054 0.038 Uiso 1 1 calc R . . C1 C 0.2655(5) -0.2395(4) 0.0474(4) 0.0339(8) Uani 1 1 d . . . H1 H 0.3504 -0.1852 0.0229 0.041 Uiso 1 1 calc R . . C2 C 0.3168(6) -0.3622(4) 0.0898(5) 0.0432(10) Uani 1 1 d . . . H2 H 0.4343 -0.3897 0.0932 0.052 Uiso 1 1 calc R . . C3 C 0.1913(6) -0.4446(4) 0.1278(5) 0.0424(10) Uani 1 1 d . . . H3' H 0.2236 -0.5279 0.1575 0.051 Uiso 1 1 calc R . . C4 C 0.0174(5) -0.4008(4) 0.1205(4) 0.0309(8) Uani 1 1 d . . . C5 C -0.0213(5) -0.2757(4) 0.0747(3) 0.0301(8) Uani 1 1 d . . . H5 H -0.1374 -0.2458 0.0676 0.036 Uiso 1 1 calc R . . C6 C -0.1343(5) -0.4771(4) 0.1627(4) 0.0324(8) Uani 1 1 d . . . C7 C -0.2347(5) -0.6774(4) 0.2218(3) 0.0335(8) Uani 1 1 d . . . H7A H -0.1883 -0.7497 0.2072 0.040 Uiso 1 1 calc R . . H7B H -0.3309 -0.6388 0.1769 0.040 Uiso 1 1 calc R . . C8 C -0.2107(5) -0.0148(4) 0.2447(4) 0.0341(9) Uani 1 1 d . . . H8 H -0.2960 0.0273 0.1966 0.041 Uiso 1 1 calc R . . C9 C -0.2509(6) -0.0405(5) 0.3669(4) 0.0473(12) Uani 1 1 d . . . H9 H -0.3617 -0.0172 0.4002 0.057 Uiso 1 1 calc R . . C10 C -0.1243(6) -0.1015(5) 0.4392(4) 0.0456(11) Uani 1 1 d . . . H10 H -0.1486 -0.1191 0.5217 0.055 Uiso 1 1 calc R . . C11 C 0.0394(5) -0.1360(3) 0.3868(3) 0.0302(8) Uani 1 1 d . . . C12 C 0.0685(5) -0.1082(3) 0.2634(3) 0.0273(7) Uani 1 1 d . . . H12 H 0.1774 -0.1323 0.2283 0.033 Uiso 1 1 calc R . . C13 C 0.1906(5) -0.1986(4) 0.4536(3) 0.0334(9) Uani 1 1 d . . . C14 C 0.3046(5) -0.2850(4) 0.6434(4) 0.0353(9) Uani 1 1 d . . . H14A H 0.3972 -0.2317 0.6188 0.042 Uiso 1 1 calc R . . H14B H 0.3541 -0.3568 0.6285 0.042 Uiso 1 1 calc R . . Cl1 Cl -0.69716(13) -0.82832(10) 0.20629(9) 0.0368(3) Uani 1 1 d D . . O4 O -0.5998(6) -0.8245(6) 0.2869(5) 0.0949(19) Uani 1 1 d D . . O5 O -0.8727(5) -0.8551(4) 0.2652(4) 0.0619(11) Uani 1 1 d D . . O6 O -0.6160(4) -0.9165(4) 0.1593(4) 0.0534(9) Uani 1 1 d D . . O7 O -0.7115(8) -0.7132(4) 0.1049(5) 0.103(2) Uani 1 1 d D . . O8 O -0.4390(5) -0.2080(3) 0.1944(3) 0.0535(9) Uani 1 1 d D . . H8A H -0.407(8) -0.283(3) 0.211(5) 0.065(19) Uiso 1 1 d D . . H8B H -0.504(7) -0.217(5) 0.261(4) 0.070(19) Uiso 1 1 d D . . N1S N 0.271(2) -0.578(2) 0.499(2) 0.163(10) Uani 0.50 1 d P A -1 C1S C 0.150(3) -0.541(2) 0.514(3) 0.145(10) Uani 0.50 1 d P A -1 C2S C 0.004(3) -0.4659(16) 0.512(3) 0.121(9) Uani 0.50 1 d P A -1 H2SB H -0.0957 -0.5128 0.5533 0.181 Uiso 0.50 1 calc PR A -1 H2SC H -0.0104 -0.4159 0.4294 0.181 Uiso 0.50 1 calc PR A -1 H2SD H 0.0120 -0.4151 0.5517 0.181 Uiso 0.50 1 calc PR A -1 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 Zn1 0.0228(3) 0.0307(3) 0.0197(3) -0.0084(2) -0.0040(2) -0.0008(2) O1 0.0252(13) 0.0358(14) 0.0292(14) -0.0107(12) -0.0061(11) -0.0049(11) O2 0.0269(15) 0.0384(16) 0.058(2) -0.0148(14) -0.0049(13) -0.0008(12) O3 0.046(2) 0.110(3) 0.0268(16) -0.0186(18) -0.0045(14) 0.032(2) N1 0.0256(16) 0.0307(16) 0.0239(15) -0.0087(12) -0.0022(12) -0.0016(12) N2 0.0268(16) 0.0314(16) 0.0231(14) -0.0095(12) -0.0029(12) -0.0029(12) N3 0.0329(18) 0.0318(16) 0.0301(16) -0.0096(13) -0.0061(13) -0.0007(13) N4 0.0282(16) 0.0408(18) 0.0234(15) -0.0111(13) -0.0064(12) 0.0009(13) C1 0.0257(19) 0.037(2) 0.036(2) -0.0125(17) -0.0066(16) -0.0014(15) C2 0.026(2) 0.038(2) 0.065(3) -0.019(2) -0.018(2) 0.0051(17) C3 0.036(2) 0.034(2) 0.055(3) -0.0149(19) -0.014(2) 0.0030(17) C4 0.030(2) 0.0314(19) 0.0291(18) -0.0101(15) -0.0058(15) -0.0011(15) C5 0.0247(18) 0.0327(19) 0.0279(18) -0.0093(15) -0.0040(14) 0.0016(14) C6 0.034(2) 0.0300(18) 0.0283(18) -0.0071(15) -0.0095(15) 0.0008(15) C7 0.036(2) 0.036(2) 0.0281(19) -0.0072(16) -0.0141(16) -0.0064(16) C8 0.030(2) 0.042(2) 0.0259(18) -0.0107(16) -0.0067(15) 0.0040(16) C9 0.038(2) 0.067(3) 0.030(2) -0.021(2) -0.0045(18) 0.016(2) C10 0.039(2) 0.068(3) 0.0224(19) -0.0184(19) -0.0045(17) 0.012(2) C11 0.031(2) 0.0322(19) 0.0224(17) -0.0075(14) -0.0057(14) 0.0010(15) C12 0.0285(19) 0.0312(18) 0.0182(16) -0.0080(13) -0.0027(13) 0.0007(14) C13 0.031(2) 0.039(2) 0.0231(17) -0.0074(15) -0.0057(15) 0.0026(16) C14 0.029(2) 0.045(2) 0.0268(19) -0.0079(17) -0.0088(15) -0.0049(17) Cl1 0.0302(5) 0.0487(6) 0.0384(5) -0.0258(5) -0.0013(4) -0.0049(4) O4 0.065(3) 0.160(5) 0.114(4) -0.102(4) -0.027(3) -0.006(3) O5 0.0353(18) 0.090(3) 0.077(3) -0.055(2) 0.0088(17) -0.0132(18) O6 0.0389(18) 0.073(2) 0.064(2) -0.047(2) -0.0065(16) 0.0055(16) O7 0.120(5) 0.061(3) 0.081(3) -0.007(2) 0.019(3) 0.001(3) O8 0.052(2) 0.048(2) 0.0454(19) -0.0163(16) 0.0206(16) -0.0114(16) N1S 0.071(11) 0.152(18) 0.25(3) -0.087(18) -0.025(13) 0.042(11) C1S 0.074(14) 0.13(2) 0.24(3) -0.09(2) -0.033(16) 0.002(13) C2S 0.072(10) 0.077(14) 0.19(2) -0.032(15) -0.026(12) 0.008(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 Zn1 O1 2.150(3) . ? Zn1 O1 2.150(3) 2 ? Zn1 N2 2.154(3) . ? Zn1 N2 2.154(3) 2 ? Zn1 N1 2.239(3) 2 ? Zn1 N1 2.239(3) . ? O2 C6 1.236(5) . ? O3 C13 1.221(5) . ? N1 C5 1.338(5) . ? N1 C1 1.353(5) . ? N2 C8 1.344(5) . ? N2 C12 1.344(5) . ? N3 C6 1.345(5) . ? N3 C7 1.464(5) . ? N4 C13 1.334(5) . ? N4 C14 1.463(5) . ? C1 C2 1.375(6) . ? C2 C3 1.391(7) . ? C3 C4 1.386(6) . ? C4 C5 1.386(5) . ? C4 C6 1.499(6) . ? C7 C14 1.523(5) 2_546 ? C8 C9 1.378(6) . ? C9 C10 1.384(6) . ? C10 C11 1.388(6) . ? C11 C12 1.388(5) . ? C11 C13 1.504(5) . ? C14 C7 1.523(5) 2_546 ? Cl1 O4 1.406(4) . ? Cl1 O6 1.429(3) . ? Cl1 O5 1.429(4) . ? Cl1 O7 1.435(5) . ? N1S C1S 0.99(2) . ? C1S C2S 1.34(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 O1 Zn1 O1 180.00(18) . 2 ? O1 Zn1 N2 88.91(11) . . ? O1 Zn1 N2 91.09(11) 2 . ? O1 Zn1 N2 91.09(11) . 2 ? O1 Zn1 N2 88.91(11) 2 2 ? N2 Zn1 N2 180.00(19) . 2 ? O1 Zn1 N1 87.86(11) . 2 ? O1 Zn1 N1 92.14(11) 2 2 ? N2 Zn1 N1 91.75(11) . 2 ? N2 Zn1 N1 88.25(11) 2 2 ? O1 Zn1 N1 92.14(11) . . ? O1 Zn1 N1 87.86(11) 2 . ? N2 Zn1 N1 88.25(11) . . ? N2 Zn1 N1 91.75(11) 2 . ? N1 Zn1 N1 180.00(18) 2 . ? C5 N1 C1 117.0(3) . . ? C5 N1 Zn1 118.5(2) . . ? C1 N1 Zn1 123.8(3) . . ? C8 N2 C12 117.8(3) . . ? C8 N2 Zn1 120.1(3) . . ? C12 N2 Zn1 122.0(2) . . ? C6 N3 C7 121.4(3) . . ? C13 N4 C14 121.0(3) . . ? N1 C1 C2 122.6(4) . . ? C1 C2 C3 119.4(4) . . ? C4 C3 C2 119.0(4) . . ? C3 C4 C5 117.4(4) . . ? C3 C4 C6 125.7(4) . . ? C5 C4 C6 116.8(3) . . ? N1 C5 C4 124.6(3) . . ? O2 C6 N3 121.7(4) . . ? O2 C6 C4 121.3(4) . . ? N3 C6 C4 117.0(4) . . ? N3 C7 C14 113.0(3) . 2_546 ? N2 C8 C9 122.7(4) . . ? C8 C9 C10 119.2(4) . . ? C9 C10 C11 119.0(4) . . ? C12 C11 C10 118.2(4) . . ? C12 C11 C13 117.2(3) . . ? C10 C11 C13 124.6(4) . . ? N2 C12 C11 123.1(3) . . ? O3 C13 N4 121.1(4) . . ? O3 C13 C11 121.4(4) . . ? N4 C13 C11 117.5(3) . . ? N4 C14 C7 111.1(3) . 2_546 ? O4 Cl1 O6 110.7(3) . . ? O4 Cl1 O5 110.5(3) . . ? O6 Cl1 O5 110.1(2) . . ? O4 Cl1 O7 111.9(4) . . ? O6 Cl1 O7 107.4(3) . . ? O5 Cl1 O7 106.0(3) . . ? N1S C1S C2S 165(4) . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 0.778 _refine_diff_density_min -0.582 _refine_diff_density_rms 0.108 data_1149 _database_code_CSD 171775 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H19 Cd Cl2 N4 O13' _chemical_formula_weight 634.63 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' '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 '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 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 17.8353(19) _cell_length_b 7.5368(8) _cell_length_c 17.1661(17) _cell_angle_alpha 90.00 _cell_angle_beta 112.487(2) _cell_angle_gamma 90.00 _cell_volume 2132.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5645 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 24.5 _exptl_crystal_description blocks _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.977 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1268 _exptl_absorpt_coefficient_mu 1.353 _exptl_absorpt_correction_type 'sadabs (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.6500 _exptl_absorpt_correction_T_max 0.9321 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5977 _diffrn_reflns_av_R_equivalents 0.0605 _diffrn_reflns_av_sigmaI/netI 0.0563 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1884 _reflns_number_gt 1413 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS, SMART' _computing_cell_refinement 'Bruker AXS, SAINT' _computing_data_reduction 'Bruker AXS, SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS, SHELXTL' _computing_publication_material 'Bruker AXS, SHELXTL' _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^ > 2sigma(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^)+(0.0600P)^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 1884 _refine_ls_number_parameters 168 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.0684 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1191 _refine_ls_wR_factor_gt 0.1088 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.046 _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 Cd1 Cd 0.5000 0.20885(8) 0.2500 0.0604(3) Uani 1 2 d S . . O1 O 0.4280(2) 0.2540(5) 0.6100(2) 0.0510(11) Uani 1 1 d . . . O2 O 0.5000 0.5084(7) 0.2500 0.0510(14) Uani 1 2 d SD . . H2 H 0.478(9) 0.592(16) 0.205(7) 0.111 Uiso 0.50 1 d PD . . O3 O 0.5911(2) -0.0144(6) 0.2718(3) 0.0586(11) Uani 1 1 d D . . H3A H 0.597(3) -0.118(4) 0.305(2) 0.032 Uiso 1 1 d D . . H3B H 0.643(3) -0.013(11) 0.268(7) 0.213 Uiso 1 1 d D . . N1 N 0.5275(3) 0.2311(5) 0.3899(3) 0.0393(11) Uani 1 1 d . . . N2 N 0.3421(3) 0.1761(7) 0.4819(3) 0.0521(14) Uani 1 1 d . . . H2A H 0.331(4) 0.171(9) 0.431(4) 0.07(2) Uiso 1 1 d . . . C1 C 0.6019(4) 0.2661(8) 0.4441(4) 0.0505(16) Uani 1 1 d . . . H1 H 0.6441 0.2756 0.4241 0.061 Uiso 1 1 calc R . . C2B C 0.6196(4) 0.2893(8) 0.5293(4) 0.0520(15) Uani 1 1 d . . . H2' H 0.6729 0.3137 0.5667 0.062 Uiso 1 1 calc R . . C3 C 0.5579(3) 0.2759(7) 0.5584(3) 0.0374(12) Uani 1 1 d . . . H3 H 0.5687 0.2910 0.6160 0.045 Uiso 1 1 calc R . . C4 C 0.4807(3) 0.2404(6) 0.5032(3) 0.0308(11) Uani 1 1 d . . . C5 C 0.4677(3) 0.2191(7) 0.4180(3) 0.0378(12) Uani 1 1 d . . . H5 H 0.4148 0.1953 0.3792 0.045 Uiso 1 1 calc R . . C6 C 0.4140(3) 0.2240(7) 0.5352(3) 0.0340(12) Uani 1 1 d . . . C7 C 0.2710(3) 0.1627(9) 0.5040(4) 0.0523(15) Uani 1 1 d . . . H7A H 0.2879 0.1199 0.5621 0.063 Uiso 1 1 calc R . . H7B H 0.2331 0.0760 0.4669 0.063 Uiso 1 1 calc R . . Cl1 Cl 0.70928(7) 0.47008(17) 0.26897(7) 0.0377(3) Uani 1 1 d D . . O4 O 0.6733(3) 0.6301(6) 0.2821(3) 0.0703(13) Uani 1 1 d D . . O5 O 0.6946(2) 0.4501(6) 0.1826(2) 0.0551(11) Uani 1 1 d D . . O6 O 0.6752(3) 0.3206(6) 0.2955(3) 0.0683(13) Uani 1 1 d D . . O7 O 0.7953(2) 0.4760(7) 0.3156(2) 0.0669(13) Uani 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 Cd1 0.1301(7) 0.0338(4) 0.0261(4) 0.000 0.0396(4) 0.000 O1 0.052(2) 0.076(3) 0.030(2) -0.0073(18) 0.0209(18) -0.005(2) O2 0.061(4) 0.033(3) 0.040(3) 0.000 -0.001(3) 0.000 O3 0.056(3) 0.068(3) 0.064(3) 0.009(2) 0.037(2) -0.006(2) N1 0.062(3) 0.035(2) 0.025(2) -0.0009(18) 0.022(2) -0.003(2) N2 0.041(3) 0.078(4) 0.037(3) -0.017(2) 0.014(2) 0.000(3) C1 0.069(4) 0.054(4) 0.045(3) -0.012(3) 0.040(3) -0.023(3) C2B 0.056(4) 0.068(4) 0.038(3) -0.014(3) 0.024(3) -0.024(3) C3 0.049(3) 0.043(3) 0.022(3) -0.005(2) 0.016(2) -0.005(3) C4 0.041(3) 0.029(3) 0.024(2) 0.0007(19) 0.014(2) 0.006(2) C5 0.053(3) 0.037(3) 0.021(2) 0.002(2) 0.012(2) 0.009(3) C6 0.039(3) 0.038(3) 0.025(3) -0.001(2) 0.011(2) 0.008(2) C7 0.043(3) 0.070(4) 0.040(3) -0.014(3) 0.013(3) -0.001(3) Cl1 0.0400(7) 0.0416(8) 0.0340(7) 0.0009(5) 0.0169(6) 0.0044(6) O4 0.065(3) 0.049(3) 0.110(4) -0.011(3) 0.048(3) 0.009(2) O5 0.065(3) 0.063(3) 0.033(2) 0.0013(18) 0.0134(18) -0.006(2) O6 0.087(3) 0.057(3) 0.086(3) 0.028(2) 0.061(3) 0.015(2) O7 0.038(2) 0.099(4) 0.045(2) -0.016(2) -0.0046(18) 0.013(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 Cd1 O2 2.257(5) . ? Cd1 N1 2.266(4) . ? Cd1 N1 2.266(4) 2_655 ? Cd1 O3 2.269(4) 2_655 ? Cd1 O3 2.269(4) . ? O1 C6 1.232(6) . ? N1 C1 1.324(8) . ? N1 C5 1.332(7) . ? N2 C6 1.310(7) . ? N2 C7 1.459(7) . ? C1 C2B 1.385(8) . ? C2B C3 1.374(8) . ? C3 C4 1.366(7) . ? C4 C5 1.399(6) . ? C4 C6 1.495(7) . ? C7 C7 1.495(12) 7_556 ? Cl1 O5 1.412(4) . ? Cl1 O4 1.424(4) . ? Cl1 O7 1.434(4) . ? Cl1 O6 1.435(4) . ? 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 O2 Cd1 N1 85.75(11) . . ? O2 Cd1 N1 85.75(10) . 2_655 ? N1 Cd1 N1 171.5(2) . 2_655 ? O2 Cd1 O3 137.86(11) . 2_655 ? N1 Cd1 O3 94.64(15) . 2_655 ? N1 Cd1 O3 91.66(15) 2_655 2_655 ? O2 Cd1 O3 137.86(11) . . ? N1 Cd1 O3 91.66(15) . . ? N1 Cd1 O3 94.64(15) 2_655 . ? O3 Cd1 O3 84.3(2) 2_655 . ? C1 N1 C5 119.1(4) . . ? C1 N1 Cd1 120.8(3) . . ? C5 N1 Cd1 120.0(4) . . ? C6 N2 C7 123.6(5) . . ? N1 C1 C2B 121.9(5) . . ? C3 C2B C1 119.0(6) . . ? C4 C3 C2B 119.8(5) . . ? C3 C4 C5 117.9(4) . . ? C3 C4 C6 119.6(4) . . ? C5 C4 C6 122.5(5) . . ? N1 C5 C4 122.3(5) . . ? O1 C6 N2 122.2(5) . . ? O1 C6 C4 119.7(5) . . ? N2 C6 C4 118.0(4) . . ? N2 C7 C7 111.8(7) . 7_556 ? O5 Cl1 O4 110.0(3) . . ? O5 Cl1 O7 108.6(2) . . ? O4 Cl1 O7 109.6(3) . . ? O5 Cl1 O6 108.6(3) . . ? O4 Cl1 O6 110.1(3) . . ? O7 Cl1 O6 109.9(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.767 _refine_diff_density_min -1.812 _refine_diff_density_rms 0.122 data_99193 _database_code_CSD 171776 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H17 Ag Cl N5 O6' _chemical_formula_weight 518.67 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' 'H' 'H' 0.0000 0.0000 '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' 'Cl' 'Cl' 0.1484 0.1585 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.1569(2) _cell_length_b 10.6650(2) _cell_length_c 13.2643(2) _cell_angle_alpha 88.4960(10) _cell_angle_beta 88.8160(10) _cell_angle_gamma 76.8810(10) _cell_volume 985.57(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4428 _cell_measurement_theta_min 2.06 _cell_measurement_theta_max 25.0 _exptl_crystal_description 'rectangular plates, cut' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.748 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 1.202 _exptl_absorpt_correction_type 'sadabs (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.6320 _exptl_absorpt_correction_T_max 0.8984 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _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 ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7712 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0479 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 26.37 _reflns_number_total 3903 _reflns_number_gt 2918 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS, SMART' _computing_cell_refinement 'Bruker AXS, SAINT' _computing_data_reduction 'Bruker AXS, SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS, SHELXTL' _computing_publication_material 'Bruker AXS, SHELXTL' _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^ > 2sigma(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^)+(0.0738P)^2^+0.5156P] 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 SHELXL _refine_ls_extinction_coef 0.0003(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3903 _refine_ls_number_parameters 283 _refine_ls_number_restraints 159 _refine_ls_R_factor_all 0.0723 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1391 _refine_ls_wR_factor_gt 0.1280 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.082 _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 0.21314(6) 0.36950(4) 0.44492(3) 0.0611(2) Uani 1 1 d . . . O1 O 0.2929(6) 0.5885(4) 0.4253(3) 0.0647(10) Uani 1 1 d . . . O2 O 0.1463(6) 0.1544(3) 0.4195(3) 0.0654(10) Uani 1 1 d . . . N1 N 0.2104(6) 0.4571(4) 0.5937(3) 0.0481(9) Uani 1 1 d . . . N2 N 0.2379(6) 0.3222(4) 0.2808(3) 0.0457(9) Uani 1 1 d . . . N3 N 0.3338(6) 0.7541(4) 0.5140(3) 0.0534(10) Uani 1 1 d . . . H3 H 0.3448 0.7827 0.5731 0.08(2) Uiso 1 1 calc R . . N4 N 0.1872(6) -0.0019(3) 0.3060(3) 0.0483(9) Uani 1 1 d . . . H4 H 0.2082 -0.0218 0.2437 0.055(15) Uiso 1 1 calc R . . C1 C 0.1783(8) 0.3925(5) 0.6780(4) 0.0611(14) Uani 1 1 d . . . H1 H 0.1422 0.3146 0.6716 0.047(13) Uiso 1 1 calc R . . C2 C 0.1959(9) 0.4352(6) 0.7723(4) 0.0662(15) Uani 1 1 d . . . H2 H 0.1716 0.3874 0.8288 0.068(17) Uiso 1 1 calc R . . C3 C 0.2494(8) 0.5480(6) 0.7831(4) 0.0628(14) Uani 1 1 d . . . H3A H 0.2630 0.5788 0.8469 0.055(14) Uiso 1 1 calc R . . C4 C 0.2832(7) 0.6162(5) 0.6974(4) 0.0540(12) Uani 1 1 d . . . H4A H 0.3200 0.6939 0.7032 0.060(15) Uiso 1 1 calc R . . C5 C 0.2627(6) 0.5702(4) 0.6043(3) 0.0415(10) Uani 1 1 d . . . C6 C 0.2962(7) 0.6384(4) 0.5064(4) 0.0439(10) Uani 1 1 d . . . C7 C 0.3570(8) 0.8344(5) 0.4258(4) 0.0567(13) Uani 1 1 d . . . H7A H 0.4364 0.7818 0.3756 0.078(19) Uiso 1 1 calc R . . H7B H 0.4221 0.9003 0.4453 0.068(16) Uiso 1 1 calc R . . C8 C 0.1663(7) -0.1022(4) 0.3803(4) 0.0521(12) Uani 1 1 d . . . H8A H 0.1133 -0.1667 0.3479 0.059(15) Uiso 1 1 calc R . . H8B H 0.0775 -0.0644 0.4333 0.09(2) Uiso 1 1 calc R . . C9 C 0.1746(7) 0.1193(4) 0.3327(4) 0.0446(10) Uani 1 1 d . . . C10 C 0.2007(7) 0.2124(4) 0.2491(3) 0.0430(10) Uani 1 1 d . . . C11 C 0.1860(10) 0.1912(5) 0.1491(4) 0.0664(15) Uani 1 1 d . . . H11 H 0.1563 0.1154 0.1286 0.070(17) Uiso 1 1 calc R . . C12 C 0.2150(11) 0.2821(6) 0.0783(4) 0.081(2) Uani 1 1 d . . . H12 H 0.2053 0.2686 0.0098 0.058(15) Uiso 1 1 calc R . . C13 C 0.2583(10) 0.3928(5) 0.1110(5) 0.0738(17) Uani 1 1 d . . . H13 H 0.2821 0.4548 0.0650 0.069(17) Uiso 1 1 calc R . . C14 C 0.2659(8) 0.4106(5) 0.2125(4) 0.0557(13) Uani 1 1 d . . . H14 H 0.2915 0.4870 0.2347 0.074(18) Uiso 1 1 calc R . . Cl1 Cl 0.2586(2) 0.76455(12) 0.08821(11) 0.0627(4) Uani 1 1 d D . . O3 O 0.1028(10) 0.7271(8) 0.1385(7) 0.125(3) Uani 0.75 1 d PD A . O4 O 0.4320(12) 0.6940(10) 0.1306(8) 0.1001(19) Uiso 0.50 1 d PD A . O5 O 0.2391(16) 0.8969(8) 0.0959(9) 0.1001(19) Uiso 0.50 1 d PD A . O6 O 0.2604(17) 0.7329(11) -0.0163(6) 0.1001(19) Uiso 0.50 1 d PD A . O4A O 0.346(3) 0.693(2) 0.0177(15) 0.115(4) Uiso 0.25 1 d PD A 1 O5A O 0.386(2) 0.795(2) 0.1632(14) 0.115(4) Uiso 0.25 1 d PD A 1 O6A O 0.159(3) 0.8992(15) 0.0512(16) 0.115(4) Uiso 0.25 1 d PD A 1 O3B O 0.326(3) 0.8755(15) 0.1030(15) 0.091(3) Uiso 0.25 1 d PD A 2 O4B O 0.436(2) 0.6603(16) 0.0704(16) 0.091(3) Uiso 0.25 1 d PD A 2 O5B O 0.150(3) 0.7670(18) 0.0035(12) 0.091(3) Uiso 0.25 1 d PD A 2 O6B O 0.174(3) 0.726(2) 0.1758(12) 0.091(3) Uiso 0.25 1 d PD A 2 C1S C 0.7034(13) -0.0309(10) 0.1381(7) 0.120(3) Uani 1 1 d . . . H1S1 H 0.7632 -0.1211 0.1405 0.181 Uiso 1 1 calc R . . H1S2 H 0.7791 0.0139 0.0963 0.181 Uiso 1 1 calc R . . H1S3 H 0.5773 -0.0188 0.1107 0.181 Uiso 1 1 calc R . . C2S C 0.6893(9) 0.0189(6) 0.2383(5) 0.0691(16) Uani 1 1 d . . . N1S N 0.6762(10) 0.0601(6) 0.3154(5) 0.100(2) 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 0.0756(3) 0.0501(3) 0.0601(3) -0.01091(18) -0.0092(2) -0.0173(2) O1 0.104(3) 0.055(2) 0.0422(19) -0.0028(16) 0.0032(19) -0.033(2) O2 0.109(3) 0.0438(19) 0.048(2) -0.0045(16) 0.015(2) -0.028(2) N1 0.055(2) 0.042(2) 0.050(2) 0.0053(18) -0.0009(18) -0.0189(18) N2 0.050(2) 0.0372(19) 0.051(2) 0.0044(17) -0.0053(18) -0.0141(17) N3 0.077(3) 0.042(2) 0.046(2) 0.0057(18) -0.004(2) -0.025(2) N4 0.065(3) 0.0346(19) 0.047(2) -0.0013(17) 0.0096(19) -0.0151(18) C1 0.069(4) 0.051(3) 0.068(4) 0.013(3) -0.002(3) -0.023(3) C2 0.074(4) 0.073(4) 0.053(3) 0.017(3) -0.001(3) -0.021(3) C3 0.071(4) 0.074(4) 0.043(3) 0.004(3) -0.003(3) -0.016(3) C4 0.062(3) 0.054(3) 0.048(3) -0.001(2) -0.001(2) -0.018(2) C5 0.039(2) 0.043(2) 0.043(2) 0.0064(19) -0.0031(19) -0.0106(19) C6 0.045(3) 0.040(2) 0.046(3) 0.0004(19) -0.001(2) -0.009(2) C7 0.069(3) 0.050(3) 0.057(3) 0.008(2) 0.002(3) -0.027(3) C8 0.061(3) 0.039(2) 0.058(3) 0.004(2) 0.010(3) -0.016(2) C9 0.050(3) 0.037(2) 0.047(3) -0.0008(19) 0.004(2) -0.012(2) C10 0.050(3) 0.033(2) 0.046(2) -0.0007(18) 0.002(2) -0.0080(19) C11 0.110(5) 0.044(3) 0.048(3) -0.003(2) 0.004(3) -0.026(3) C12 0.140(6) 0.056(3) 0.047(3) 0.004(3) 0.006(3) -0.025(4) C13 0.109(5) 0.050(3) 0.064(4) 0.015(3) 0.018(3) -0.025(3) C14 0.066(3) 0.038(2) 0.065(3) 0.008(2) -0.003(3) -0.018(2) Cl1 0.0732(9) 0.0470(7) 0.0699(8) -0.0072(6) -0.0018(7) -0.0170(6) O3 0.083(5) 0.116(6) 0.182(9) 0.033(6) 0.019(5) -0.043(5) C1S 0.118(7) 0.135(8) 0.103(6) -0.036(6) 0.019(5) -0.015(6) C2S 0.065(4) 0.057(3) 0.088(5) -0.012(3) 0.000(3) -0.018(3) N1S 0.110(5) 0.093(4) 0.103(5) -0.029(4) -0.012(4) -0.032(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 2.203(4) . ? Ag1 N2 2.242(4) . ? Ag1 O2 2.480(3) . ? Ag1 O1 2.533(4) . ? O1 C6 1.216(6) . ? O2 C9 1.220(6) . ? N1 C1 1.340(7) . ? N1 C5 1.353(6) . ? N2 C14 1.336(6) . ? N2 C10 1.338(6) . ? N3 C6 1.327(6) . ? N3 C7 1.461(6) . ? N4 C9 1.332(6) . ? N4 C8 1.466(6) . ? C1 C2 1.361(8) . ? C2 C3 1.355(8) . ? C3 C4 1.381(7) . ? C4 C5 1.364(7) . ? C5 C6 1.513(7) . ? C7 C8 1.509(7) 1_565 ? C8 C7 1.509(7) 1_545 ? C9 C10 1.506(6) . ? C10 C11 1.362(7) . ? C11 C12 1.378(8) . ? C12 C13 1.370(9) . ? C13 C14 1.368(8) . ? Cl1 O4A 1.285(14) . ? Cl1 O5B 1.377(14) . ? Cl1 O5 1.393(8) . ? Cl1 O6B 1.395(15) . ? Cl1 O3B 1.395(14) . ? Cl1 O3 1.416(6) . ? Cl1 O4 1.416(8) . ? Cl1 O6 1.435(8) . ? Cl1 O5A 1.454(15) . ? Cl1 O4B 1.503(14) . ? Cl1 O6A 1.523(14) . ? O3 O6B 0.72(2) . ? O4 O4B 0.883(18) . ? O4 O5A 1.14(2) . ? O4 O4A 1.63(2) . ? O5 O3B 0.62(2) . ? O5 O6A 0.83(2) . ? O5 O5A 1.60(2) . ? O6 O4A 0.80(2) . ? O6 O5B 0.834(18) . ? O6 O4B 1.751(19) . ? C1S C2S 1.436(10) . ? C2S N1S 1.117(8) . ? 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 166.47(13) . . ? N1 Ag1 O2 123.73(13) . . ? N2 Ag1 O2 69.77(12) . . ? N1 Ag1 O1 70.06(12) . . ? N2 Ag1 O1 96.43(12) . . ? O2 Ag1 O1 166.20(11) . . ? C6 O1 Ag1 111.6(3) . . ? C9 O2 Ag1 112.7(3) . . ? C1 N1 C5 117.6(4) . . ? C1 N1 Ag1 120.6(3) . . ? C5 N1 Ag1 121.3(3) . . ? C14 N2 C10 119.0(4) . . ? C14 N2 Ag1 119.9(3) . . ? C10 N2 Ag1 120.5(3) . . ? C6 N3 C7 122.4(4) . . ? C9 N4 C8 121.6(4) . . ? N1 C1 C2 123.2(5) . . ? C3 C2 C1 119.3(5) . . ? C2 C3 C4 118.5(5) . . ? C5 C4 C3 120.2(5) . . ? N1 C5 C4 121.1(4) . . ? N1 C5 C6 115.0(4) . . ? C4 C5 C6 123.9(4) . . ? O1 C6 N3 121.9(4) . . ? O1 C6 C5 121.6(4) . . ? N3 C6 C5 116.5(4) . . ? N3 C7 C8 111.7(4) . 1_565 ? N4 C8 C7 111.1(4) . 1_545 ? O2 C9 N4 122.8(4) . . ? O2 C9 C10 121.0(4) . . ? N4 C9 C10 116.2(4) . . ? N2 C10 C11 121.2(4) . . ? N2 C10 C9 114.3(4) . . ? C11 C10 C9 124.5(4) . . ? C10 C11 C12 120.0(5) . . ? C13 C12 C11 118.6(6) . . ? C14 C13 C12 118.9(5) . . ? N2 C14 C13 122.3(5) . . ? O4A Cl1 O5B 66.6(11) . . ? O4A Cl1 O5 126.8(11) . . ? O5B Cl1 O5 97.8(9) . . ? O4A Cl1 O6B 127.5(13) . . ? O5B Cl1 O6B 113.6(10) . . ? O5 Cl1 O6B 105.5(11) . . ? O4A Cl1 O3B 114.5(12) . . ? O5B Cl1 O3B 115.3(10) . . ? O5 Cl1 O3B 25.7(8) . . ? O6B Cl1 O3B 111.5(10) . . ? O4A Cl1 O3 118.0(9) . . ? O5B Cl1 O3 84.1(9) . . ? O5 Cl1 O3 109.7(5) . . ? O6B Cl1 O3 29.5(8) . . ? O3B Cl1 O3 127.5(9) . . ? O4A Cl1 O4 74.2(11) . . ? O5B Cl1 O4 140.0(9) . . ? O5 Cl1 O4 111.9(6) . . ? O6B Cl1 O4 84.4(9) . . ? O3B Cl1 O4 87.3(9) . . ? O3 Cl1 O4 108.8(5) . . ? O4A Cl1 O6 33.8(10) . . ? O5B Cl1 O6 34.4(7) . . ? O5 Cl1 O6 109.1(6) . . ? O6B Cl1 O6 134.9(10) . . ? O3B Cl1 O6 112.3(10) . . ? O3 Cl1 O6 109.5(5) . . ? O4 Cl1 O6 107.8(6) . . ? O4A Cl1 O5A 113.6(10) . . ? O5B Cl1 O5A 163.4(11) . . ? O5 Cl1 O5A 68.4(9) . . ? O6B Cl1 O5A 80.0(11) . . ? O3B Cl1 O5A 48.6(10) . . ? O3 Cl1 O5A 108.8(8) . . ? O4 Cl1 O5A 46.8(8) . . ? O6 Cl1 O5A 139.7(9) . . ? O4A Cl1 O4B 39.3(10) . . ? O5B Cl1 O4B 105.1(9) . . ? O5 Cl1 O4B 129.7(8) . . ? O6B Cl1 O4B 105.1(10) . . ? O3B Cl1 O4B 105.0(9) . . ? O3 Cl1 O4B 116.6(8) . . ? O4 Cl1 O4B 35.0(7) . . ? O6 Cl1 O4B 73.1(8) . . ? O5A Cl1 O4B 78.9(10) . . ? O4A Cl1 O6A 113.4(10) . . ? O5B Cl1 O6A 65.6(11) . . ? O5 Cl1 O6A 32.6(8) . . ? O6B Cl1 O6A 112.8(12) . . ? O3B Cl1 O6A 55.2(10) . . ? O3 Cl1 O6A 100.1(7) . . ? O4 Cl1 O6A 142.0(9) . . ? O6 Cl1 O6A 84.3(9) . . ? O5A Cl1 O6A 101.0(9) . . ? O4B Cl1 O6A 141.5(10) . . ? O6B O3 Cl1 73.6(13) . . ? O4B O4 O5A 136.2(19) . . ? O4B O4 Cl1 77.9(11) . . ? O5A O4 Cl1 68.3(8) . . ? O4B O4 O4A 29.0(11) . . ? O5A O4 O4A 110.3(13) . . ? Cl1 O4 O4A 49.2(6) . . ? O3B O5 O6A 139(3) . . ? O3B O5 Cl1 77.4(16) . . ? O6A O5 Cl1 82.4(12) . . ? O3B O5 O5A 38(2) . . ? O6A O5 O5A 140.0(15) . . ? Cl1 O5 O5A 57.6(7) . . ? O4A O6 O5B 126.5(18) . . ? O4A O6 Cl1 62.8(11) . . ? O5B O6 Cl1 69.0(11) . . ? O4A O6 O4B 7.7(12) . . ? O5B O6 O4B 120.3(14) . . ? Cl1 O6 O4B 55.2(6) . . ? O6 O4A Cl1 83.4(14) . . ? O6 O4A O4 139.5(16) . . ? Cl1 O4A O4 56.6(8) . . ? O4 O5A Cl1 64.8(8) . . ? O4 O5A O5 115.1(12) . . ? Cl1 O5A O5 54.0(6) . . ? O5 O6A Cl1 65.0(11) . . ? O5 O3B Cl1 76.9(16) . . ? O4 O4B Cl1 67.1(10) . . ? O4 O4B O6 118.2(13) . . ? Cl1 O4B O6 51.7(5) . . ? O6 O5B Cl1 76.6(11) . . ? O3 O6B Cl1 76.9(14) . . ? N1S C2S C1S 178.5(9) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.784 _refine_diff_density_min -0.683 _refine_diff_density_rms 0.086