# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global #TrackingRef '- cif.cif' _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Yan Bai' _publ_contact_author_email baiyan@henu.edu.cn _publ_section_title ; Assembly of four d10-metal inorganic Corganic hybrid c oordination polymers based on bipyrazine imine-based ligand: synthesis, crystal structures and luminescent properties ; loop_ _publ_author_name 'Yan Bai' 'Jun-Li Wang' 'Dong-Bin Dang' 'Meng-Meng Li' 'Jingyang Niu' # Attachment '1.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 838959' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H14 Ag2 N8 O7' _chemical_formula_weight 598.05 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 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 12.2040(10) _cell_length_b 8.1960(10) _cell_length_c 18.415(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.230(10) _cell_angle_gamma 90.00 _cell_volume 1777.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1198 _cell_measurement_theta_min 3.07 _cell_measurement_theta_max 23.29 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.235 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 2.262 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6997 _exptl_absorpt_correction_T_max 0.8054 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4609 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 25.50 _reflns_number_total 1652 _reflns_number_gt 1255 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0344P)^2^+9.1151P] 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 1652 _refine_ls_number_parameters 132 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0529 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0901 _refine_ls_wR_factor_gt 0.0837 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.074 _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 0.96733(4) 0.25920(5) 0.61100(3) 0.04693(19) Uani 1 1 d . . . N1 N 1.1146(4) 0.0865(5) 0.6010(3) 0.0355(10) Uani 1 1 d . . . N2 N 1.0242(4) 0.0720(5) 0.7193(2) 0.0340(10) Uani 1 1 d . . . N3 N 1.3022(4) -0.1045(6) 0.6000(3) 0.0393(11) Uani 1 1 d . . . C1 C 1.1598(5) 0.0849(7) 0.5433(3) 0.0405(13) Uani 1 1 d . . . H1A H 1.1280 0.1508 0.5020 0.049 Uiso 1 1 calc R . . C2 C 1.2529(4) -0.0113(7) 0.5417(3) 0.0412(13) Uani 1 1 d . . . H2A H 1.2809 -0.0103 0.4994 0.049 Uiso 1 1 calc R . . C3 C 1.2568(4) -0.1026(7) 0.6584(3) 0.0378(13) Uani 1 1 d . . . H3A H 1.2895 -0.1672 0.6999 0.045 Uiso 1 1 calc R . . C4 C 1.1633(4) -0.0092(6) 0.6600(3) 0.0307(11) Uani 1 1 d . . . C5 C 1.1126(4) -0.0146(6) 0.7254(3) 0.0299(11) Uani 1 1 d . . . C6 C 1.1642(5) -0.1234(9) 0.7899(4) 0.0558(17) Uani 1 1 d . . . H6A H 1.1224 -0.1146 0.8272 0.084 Uiso 1 1 calc R . . H6B H 1.2417 -0.0916 0.8115 0.084 Uiso 1 1 calc R . . H6C H 1.1620 -0.2342 0.7727 0.084 Uiso 1 1 calc R . . N4 N 1.0550(5) 0.6289(7) 0.5846(4) 0.0638(14) Uani 1 1 d U . . O1 O 1.0969(4) 0.4924(6) 0.5926(3) 0.0813(13) Uani 1 1 d U . . O2 O 0.9887(5) 0.6830(8) 0.6187(3) 0.0903(18) Uani 1 1 d . . . O3 O 1.0765(5) 0.7177(7) 0.5361(3) 0.0761(15) Uani 1 1 d . . . O1W O 1.0000 0.4756(10) 0.7500 0.127(4) Uani 1 2 d S . . H1WA H 0.9967 0.5352 0.7117 0.153 Uiso 1 1 d 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 0.0395(3) 0.0456(3) 0.0621(3) 0.0105(2) 0.0248(2) 0.0194(2) N1 0.033(2) 0.036(2) 0.042(3) 0.005(2) 0.018(2) 0.0076(19) N2 0.034(2) 0.032(2) 0.042(3) 0.0031(19) 0.0200(19) 0.0024(19) N3 0.034(2) 0.048(3) 0.039(3) 0.005(2) 0.016(2) 0.010(2) C1 0.041(3) 0.042(3) 0.044(3) 0.014(3) 0.020(3) 0.012(2) C2 0.036(3) 0.051(3) 0.042(3) 0.007(3) 0.020(3) 0.011(3) C3 0.030(3) 0.042(3) 0.043(3) 0.007(3) 0.015(2) 0.007(2) C4 0.027(3) 0.028(3) 0.039(3) 0.002(2) 0.012(2) -0.002(2) C5 0.027(3) 0.031(3) 0.032(3) -0.001(2) 0.008(2) -0.002(2) C6 0.039(3) 0.081(5) 0.049(4) 0.017(3) 0.015(3) 0.018(3) N4 0.047(3) 0.040(3) 0.106(4) 0.003(3) 0.024(3) 0.001(2) O1 0.060(3) 0.056(2) 0.126(4) 0.012(3) 0.021(3) 0.006(2) O2 0.106(4) 0.086(4) 0.103(5) -0.009(3) 0.071(4) -0.003(3) O3 0.084(4) 0.078(4) 0.067(3) -0.004(3) 0.020(3) -0.006(3) O1W 0.187(10) 0.073(6) 0.090(7) 0.000 -0.021(6) 0.000 _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 2.266(4) 3_455 ? Ag1 N1 2.333(4) . ? Ag1 N2 2.467(4) . ? Ag1 O1 2.559(5) . ? N1 C1 1.320(7) . ? N1 C4 1.346(6) . ? N2 C5 1.271(6) . ? N2 N2 1.406(8) 2_756 ? N3 C2 1.326(7) . ? N3 C3 1.334(7) . ? N3 Ag1 2.266(4) 3_545 ? C1 C2 1.389(7) . ? C1 H1A 0.9300 . ? C2 H2A 0.9300 . ? C3 C4 1.381(7) . ? C3 H3A 0.9300 . ? C4 C5 1.491(7) . ? C5 C6 1.487(7) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? N4 O1 1.223(7) . ? N4 O2 1.229(7) . ? N4 O3 1.234(7) . ? O1W H1WA 0.8500 . ? 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 167.83(16) 3_455 . ? N3 Ag1 N2 115.70(15) 3_455 . ? N1 Ag1 N2 68.12(14) . . ? N3 Ag1 O1 100.71(16) 3_455 . ? N1 Ag1 O1 85.82(16) . . ? N2 Ag1 O1 121.28(16) . . ? C1 N1 C4 117.1(4) . . ? C1 N1 Ag1 124.3(3) . . ? C4 N1 Ag1 118.4(3) . . ? C5 N2 N2 117.1(5) . 2_756 ? C5 N2 Ag1 118.1(3) . . ? N2 N2 Ag1 124.1(3) 2_756 . ? C2 N3 C3 116.7(5) . . ? C2 N3 Ag1 124.1(4) . 3_545 ? C3 N3 Ag1 118.8(4) . 3_545 ? N1 C1 C2 122.6(5) . . ? N1 C1 H1A 118.7 . . ? C2 C1 H1A 118.7 . . ? N3 C2 C1 120.7(5) . . ? N3 C2 H2A 119.7 . . ? C1 C2 H2A 119.7 . . ? N3 C3 C4 123.1(5) . . ? N3 C3 H3A 118.5 . . ? C4 C3 H3A 118.5 . . ? N1 C4 C3 119.8(5) . . ? N1 C4 C5 118.7(4) . . ? C3 C4 C5 121.5(5) . . ? N2 C5 C6 125.2(5) . . ? N2 C5 C4 115.8(4) . . ? C6 C5 C4 118.9(5) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O1 N4 O2 125.4(7) . . ? O1 N4 O3 117.7(7) . . ? O2 N4 O3 116.8(6) . . ? N4 O1 Ag1 116.5(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.966 _refine_diff_density_min -0.701 _refine_diff_density_rms 0.102 # Attachment '2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 838960' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H12 Ag2 N8 S2' _chemical_formula_weight 572.18 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' 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 Orthorhombic _symmetry_space_group_name_H-M Aba2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/2, -y+1, z+1/2' '-x+1/2, y+1, z+1/2' _cell_length_a 12.2275(7) _cell_length_b 21.7867(13) _cell_length_c 7.0262(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1871.76(19) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2533 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 27.33 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.030 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 2.331 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4958 _exptl_absorpt_correction_T_max 0.6528 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4468 _diffrn_reflns_av_R_equivalents 0.0165 _diffrn_reflns_av_sigmaI/netI 0.0214 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.48 _reflns_number_total 1714 _reflns_number_gt 1611 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0271P)^2^+1.1935P] 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 SHELXL _refine_ls_extinction_coef 0.0078(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(4) _refine_ls_number_reflns 1714 _refine_ls_number_parameters 120 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0247 _refine_ls_R_factor_gt 0.0228 _refine_ls_wR_factor_ref 0.0551 _refine_ls_wR_factor_gt 0.0537 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.059 _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 -0.285478(18) -0.259011(12) 0.40460(7) 0.06012(14) Uani 1 1 d . . . S1 S -0.65391(7) -0.17889(4) 0.59900(13) 0.0450(2) Uani 1 1 d . . . C1 C -0.5386(3) -0.2145(2) 0.5443(5) 0.0465(9) Uani 1 1 d . . . N1 N -0.4563(3) -0.2370(2) 0.5110(7) 0.0752(13) Uani 1 1 d . . . N2 N -0.1740(3) -0.03403(14) 0.2691(4) 0.0447(8) Uani 1 1 d . . . N3 N -0.2273(2) -0.15584(14) 0.3520(4) 0.0423(7) Uani 1 1 d . . . N4 N -0.4605(2) -0.02260(14) 0.3232(4) 0.0466(7) Uani 1 1 d . . . C2 C -0.0973(3) -0.07710(19) 0.2937(5) 0.0485(9) Uani 1 1 d . . . H2A H -0.0241 -0.0663 0.2800 0.058 Uiso 1 1 calc R . . C3 C -0.1232(3) -0.13670(18) 0.3385(5) 0.0435(9) Uani 1 1 d . . . H3A H -0.0670 -0.1646 0.3601 0.052 Uiso 1 1 calc R . . C4 C -0.3033(3) -0.11331(17) 0.3247(5) 0.0403(8) Uani 1 1 d . . . H4A H -0.3765 -0.1248 0.3298 0.048 Uiso 1 1 calc R . . C5 C -0.2777(2) -0.05226(17) 0.2889(5) 0.0363(7) Uani 1 1 d . . . C6 C -0.3651(3) -0.00497(16) 0.2683(4) 0.0371(7) Uani 1 1 d . . . C7 C -0.3385(3) 0.05671(18) 0.1901(6) 0.0558(10) Uani 1 1 d . . . H7A H -0.4038 0.0811 0.1844 0.084 Uiso 1 1 calc R . . H7B H -0.3086 0.0523 0.0645 0.084 Uiso 1 1 calc R . . H7C H -0.2859 0.0765 0.2709 0.084 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 0.03399(16) 0.05349(19) 0.0929(3) -0.0051(3) -0.00620(19) 0.00698(10) S1 0.0361(4) 0.0467(5) 0.0522(5) -0.0025(4) -0.0010(4) 0.0050(4) C1 0.0346(19) 0.060(3) 0.045(2) -0.0140(18) -0.0004(15) -0.0084(17) N1 0.033(2) 0.103(3) 0.089(3) -0.046(2) 0.0041(17) -0.0012(18) N2 0.0394(16) 0.0456(19) 0.0491(19) -0.0050(14) 0.0044(12) 0.0007(13) N3 0.0434(16) 0.0414(16) 0.0421(18) -0.0053(12) 0.0004(12) 0.0066(12) N4 0.0391(16) 0.0368(16) 0.0639(18) 0.0013(14) 0.0002(13) 0.0091(12) C2 0.0329(18) 0.055(2) 0.058(2) -0.0085(19) 0.0056(15) 0.0041(16) C3 0.0368(19) 0.049(2) 0.044(2) -0.0060(14) 0.0005(14) 0.0125(14) C4 0.0382(17) 0.040(2) 0.0428(17) -0.0038(15) -0.0010(13) 0.0047(14) C5 0.0401(19) 0.0387(19) 0.0303(17) -0.0075(14) 0.0016(13) 0.0041(13) C6 0.0388(17) 0.0366(18) 0.0359(19) -0.0059(13) -0.0036(14) 0.0016(14) C7 0.055(2) 0.040(2) 0.073(3) 0.0048(19) 0.011(2) 0.0048(17) _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 2.270(3) . ? Ag1 N3 2.386(3) . ? Ag1 S1 2.5068(10) 3_545 ? Ag1 S1 2.6440(11) 6_444 ? S1 C1 1.655(4) . ? S1 Ag1 2.5069(10) 3_445 ? S1 Ag1 2.6440(11) 6_445 ? C1 N1 1.143(4) . ? N2 C5 1.336(5) . ? N2 C2 1.338(5) . ? N3 C4 1.326(4) . ? N3 C3 1.343(4) . ? N4 C6 1.287(4) . ? N4 N4 1.380(5) 2_455 ? C2 C3 1.373(5) . ? C2 H2A 0.9300 . ? C3 H3A 0.9300 . ? C4 C5 1.390(5) . ? C4 H4A 0.9300 . ? C5 C6 1.492(5) . ? C6 C7 1.488(5) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? 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 N3 97.25(14) . . ? N1 Ag1 S1 121.68(14) . 3_545 ? N3 Ag1 S1 113.67(7) . 3_545 ? N1 Ag1 S1 96.76(11) . 6_444 ? N3 Ag1 S1 116.10(7) . 6_444 ? S1 Ag1 S1 110.25(4) 3_545 6_444 ? C1 S1 Ag1 99.61(13) . 3_445 ? C1 S1 Ag1 100.81(15) . 6_445 ? Ag1 S1 Ag1 89.22(3) 3_445 6_445 ? N1 C1 S1 176.8(4) . . ? C1 N1 Ag1 165.4(5) . . ? C5 N2 C2 116.3(3) . . ? C4 N3 C3 115.9(3) . . ? C4 N3 Ag1 118.1(2) . . ? C3 N3 Ag1 125.9(2) . . ? C6 N4 N4 115.0(4) . 2_455 ? N2 C2 C3 122.1(3) . . ? N2 C2 H2A 118.9 . . ? C3 C2 H2A 118.9 . . ? N3 C3 C2 121.9(3) . . ? N3 C3 H3A 119.1 . . ? C2 C3 H3A 119.1 . . ? N3 C4 C5 122.5(3) . . ? N3 C4 H4A 118.8 . . ? C5 C4 H4A 118.8 . . ? N2 C5 C4 121.2(3) . . ? N2 C5 C6 117.7(3) . . ? C4 C5 C6 121.1(3) . . ? N4 C6 C7 125.3(3) . . ? N4 C6 C5 114.5(3) . . ? C7 C6 C5 120.2(3) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.402 _refine_diff_density_min -0.534 _refine_diff_density_rms 0.079 # Attachment '3.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 838961' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H12 Cd N8 S2' _chemical_formula_weight 468.84 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' Cd Cd -0.8075 1.2024 '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' S S 0.1246 0.1234 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.8963(4) _cell_length_b 7.1928(4) _cell_length_c 10.9481(7) _cell_angle_alpha 73.6100(10) _cell_angle_beta 86.5760(10) _cell_angle_gamma 87.0680(10) _cell_volume 444.37(5) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2155 _cell_measurement_theta_min 2.95 _cell_measurement_theta_max 27.94 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.752 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 232 _exptl_absorpt_coefficient_mu 1.478 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6572 _exptl_absorpt_correction_T_max 0.7465 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2387 _diffrn_reflns_av_R_equivalents 0.0102 _diffrn_reflns_av_sigmaI/netI 0.0170 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.50 _reflns_number_total 1640 _reflns_number_gt 1610 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0305P)^2^+0.1184P] 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 1640 _refine_ls_number_parameters 116 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0189 _refine_ls_R_factor_gt 0.0185 _refine_ls_wR_factor_ref 0.0496 _refine_ls_wR_factor_gt 0.0493 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 0.0000 0.5000 0.5000 0.03691(9) Uani 1 2 d S . . S1 S -0.24558(9) 0.80546(8) 0.34892(6) 0.04573(14) Uani 1 1 d . . . C1 C -0.5009(3) 0.7210(3) 0.39058(19) 0.0369(4) Uani 1 1 d . . . N1 N -0.6806(3) 0.6643(3) 0.4178(2) 0.0523(5) Uani 1 1 d . . . N2 N 0.0704(3) 0.1802(3) 0.12904(17) 0.0455(4) Uani 1 1 d . . . N3 N 0.0284(3) 0.3443(3) 0.33209(17) 0.0443(4) Uani 1 1 d . . . N4 N -0.4213(3) 0.4802(3) 0.04794(17) 0.0462(4) Uani 1 1 d . . . C2 C 0.2225(4) 0.1461(3) 0.2179(2) 0.0507(5) Uani 1 1 d . . . H2A H 0.3473 0.0640 0.2119 0.061 Uiso 1 1 calc R . . C3 C 0.2050(4) 0.2257(4) 0.3181(2) 0.0496(5) Uani 1 1 d . . . H3A H 0.3174 0.1970 0.3774 0.060 Uiso 1 1 calc R . . C4 C -0.1269(4) 0.3787(3) 0.2439(2) 0.0432(5) Uani 1 1 d . . . H4A H -0.2529 0.4589 0.2508 0.052 Uiso 1 1 calc R . . C5 C -0.1064(4) 0.2989(3) 0.14219(19) 0.0376(4) Uani 1 1 d . . . C6 C -0.2771(4) 0.3427(3) 0.04258(19) 0.0404(4) Uani 1 1 d . . . C7 C -0.2667(6) 0.2276(4) -0.0511(3) 0.0681(8) Uani 1 1 d . . . H7A H -0.3998 0.2570 -0.1005 0.102 Uiso 1 1 calc R . . H7B H -0.2598 0.0919 -0.0068 0.102 Uiso 1 1 calc R . . H7C H -0.1336 0.2596 -0.1068 0.102 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 Cd1 0.02426(12) 0.04793(14) 0.04013(13) -0.01410(9) -0.00674(8) 0.00013(8) S1 0.0299(3) 0.0453(3) 0.0544(3) -0.0006(2) -0.0053(2) -0.0037(2) C1 0.0318(11) 0.0372(10) 0.0390(10) -0.0063(8) -0.0097(8) 0.0066(8) N1 0.0295(9) 0.0547(11) 0.0626(12) 0.0012(10) -0.0080(8) -0.0006(8) N2 0.0500(11) 0.0415(9) 0.0438(9) -0.0113(8) -0.0028(8) 0.0081(8) N3 0.0390(10) 0.0516(10) 0.0450(10) -0.0176(8) -0.0089(8) 0.0052(8) N4 0.0488(11) 0.0484(10) 0.0466(10) -0.0207(8) -0.0158(8) 0.0074(8) C2 0.0477(13) 0.0485(12) 0.0525(13) -0.0109(10) -0.0031(10) 0.0137(10) C3 0.0417(12) 0.0566(13) 0.0495(12) -0.0137(10) -0.0099(10) 0.0100(10) C4 0.0382(11) 0.0479(12) 0.0469(11) -0.0195(9) -0.0082(9) 0.0080(9) C5 0.0422(11) 0.0330(9) 0.0376(10) -0.0096(8) -0.0034(8) 0.0004(8) C6 0.0462(12) 0.0391(10) 0.0365(10) -0.0115(8) -0.0045(9) 0.0010(9) C7 0.087(2) 0.0693(17) 0.0612(16) -0.0393(14) -0.0257(14) 0.0255(15) _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 N1 2.2754(19) 1_655 ? Cd1 N1 2.2754(19) 2_466 ? Cd1 N3 2.4016(18) 2_566 ? Cd1 N3 2.4016(18) . ? Cd1 S1 2.7513(5) . ? Cd1 S1 2.7513(5) 2_566 ? S1 C1 1.643(2) . ? C1 N1 1.147(3) . ? N1 Cd1 2.2754(19) 1_455 ? N2 C2 1.326(3) . ? N2 C5 1.340(3) . ? N3 C4 1.334(3) . ? N3 C3 1.342(3) . ? N4 C6 1.283(3) . ? N4 N4 1.402(3) 2_465 ? C2 C3 1.370(3) . ? C2 H2A 0.9300 . ? C3 H3A 0.9300 . ? C4 C5 1.386(3) . ? C4 H4A 0.9300 . ? C5 C6 1.486(3) . ? C6 C7 1.486(3) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? 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 Cd1 N1 180.0 1_655 2_466 ? N1 Cd1 N3 90.03(7) 1_655 2_566 ? N1 Cd1 N3 89.97(7) 2_466 2_566 ? N1 Cd1 N3 89.97(7) 1_655 . ? N1 Cd1 N3 90.03(7) 2_466 . ? N3 Cd1 N3 180.0 2_566 . ? N1 Cd1 S1 87.59(5) 1_655 . ? N1 Cd1 S1 92.41(5) 2_466 . ? N3 Cd1 S1 89.70(5) 2_566 . ? N3 Cd1 S1 90.30(5) . . ? N1 Cd1 S1 92.41(5) 1_655 2_566 ? N1 Cd1 S1 87.59(5) 2_466 2_566 ? N3 Cd1 S1 90.30(5) 2_566 2_566 ? N3 Cd1 S1 89.70(5) . 2_566 ? S1 Cd1 S1 180.0 . 2_566 ? C1 S1 Cd1 98.17(7) . . ? N1 C1 S1 178.8(2) . . ? C1 N1 Cd1 168.29(17) . 1_455 ? C2 N2 C5 116.07(19) . . ? C4 N3 C3 116.34(19) . . ? C4 N3 Cd1 121.35(14) . . ? C3 N3 Cd1 122.24(15) . . ? C6 N4 N4 113.3(2) . 2_465 ? N2 C2 C3 123.2(2) . . ? N2 C2 H2A 118.4 . . ? C3 C2 H2A 118.4 . . ? N3 C3 C2 121.1(2) . . ? N3 C3 H3A 119.5 . . ? C2 C3 H3A 119.5 . . ? N3 C4 C5 122.12(19) . . ? N3 C4 H4A 118.9 . . ? C5 C4 H4A 118.9 . . ? N2 C5 C4 121.18(19) . . ? N2 C5 C6 117.19(18) . . ? C4 C5 C6 121.63(18) . . ? N4 C6 C5 114.54(18) . . ? N4 C6 C7 126.7(2) . . ? C5 C6 C7 118.74(19) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.248 _refine_diff_density_min -0.262 _refine_diff_density_rms 0.054 # Attachment '4.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 838962' #TrackingRef '- cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H12 Cd I2 N6' _chemical_formula_weight 606.48 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 4.1197(2) _cell_length_b 8.0163(4) _cell_length_c 12.4386(8) _cell_angle_alpha 91.739(3) _cell_angle_beta 94.104(3) _cell_angle_gamma 94.716(3) _cell_volume 408.07(4) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1620 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 23.15 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.468 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 280 _exptl_absorpt_coefficient_mu 5.122 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4273 _exptl_absorpt_correction_T_max 0.4945 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5682 _diffrn_reflns_av_R_equivalents 0.0194 _diffrn_reflns_av_sigmaI/netI 0.0151 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1426 _reflns_number_gt 1398 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0245P)^2^+0.1696P] 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 1426 _refine_ls_number_parameters 98 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0165 _refine_ls_R_factor_gt 0.0161 _refine_ls_wR_factor_ref 0.0419 _refine_ls_wR_factor_gt 0.0416 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _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 0.0000 -0.5000 0.0000 0.02978(9) Uani 1 2 d S . . I1 I -0.49220(4) -0.712221(19) 0.097219(13) 0.03347(8) Uani 1 1 d . . . N1 N 0.0589(6) -0.3175(3) 0.16158(17) 0.0334(5) Uani 1 1 d . . . N2 N 0.1125(6) -0.1129(3) 0.34792(18) 0.0419(6) Uani 1 1 d . . . N3 N 0.4423(6) -0.4724(3) 0.44958(17) 0.0404(6) Uani 1 1 d . . . C1 C 0.0160(8) -0.0581(4) 0.2516(2) 0.0475(8) Uani 1 1 d . . . H1A H -0.0373 0.0521 0.2469 0.057 Uiso 1 1 calc R . . C2 C -0.0077(8) -0.1572(3) 0.1594(2) 0.0404(7) Uani 1 1 d . . . H2A H -0.0715 -0.1122 0.0939 0.049 Uiso 1 1 calc R . . C3 C 0.1557(7) -0.3738(3) 0.2575(2) 0.0340(6) Uani 1 1 d . . . H3A H 0.2034 -0.4848 0.2623 0.041 Uiso 1 1 calc R . . C4 C 0.1875(6) -0.2714(3) 0.3505(2) 0.0306(5) Uani 1 1 d . . . C5 C 0.3115(6) -0.3335(3) 0.4560(2) 0.0319(6) Uani 1 1 d . . . C6 C 0.2707(8) -0.2325(4) 0.5555(2) 0.0469(7) Uani 1 1 d . . . H6A H 0.3008 -0.3000 0.6173 0.070 Uiso 1 1 calc R . . H6B H 0.0552 -0.1946 0.5522 0.070 Uiso 1 1 calc R . . H6C H 0.4296 -0.1375 0.5613 0.070 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 Cd1 0.03304(16) 0.03276(15) 0.02331(15) -0.00051(11) -0.00108(11) 0.00477(11) I1 0.03208(12) 0.03550(12) 0.03369(12) 0.00901(8) 0.00006(8) 0.00719(8) N1 0.0435(12) 0.0317(11) 0.0248(11) 0.0005(9) -0.0020(9) 0.0067(9) N2 0.0633(16) 0.0322(12) 0.0302(12) -0.0025(9) -0.0061(11) 0.0140(11) N3 0.0628(15) 0.0381(12) 0.0219(11) 0.0006(9) -0.0046(10) 0.0202(11) C1 0.076(2) 0.0298(14) 0.0378(16) 0.0008(12) -0.0074(15) 0.0186(14) C2 0.0595(18) 0.0327(14) 0.0288(14) 0.0058(11) -0.0067(12) 0.0089(13) C3 0.0474(15) 0.0276(12) 0.0272(13) 0.0012(10) -0.0030(11) 0.0101(11) C4 0.0387(14) 0.0282(12) 0.0256(13) 0.0006(10) -0.0004(11) 0.0090(11) C5 0.0389(14) 0.0304(13) 0.0262(13) -0.0001(10) -0.0026(11) 0.0074(11) C6 0.074(2) 0.0398(15) 0.0278(14) -0.0050(12) -0.0071(14) 0.0224(15) _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 N1 2.436(2) . ? Cd1 N1 2.436(2) 2_545 ? Cd1 I1 2.8943(2) 2_545 ? Cd1 I1 2.8943(2) . ? Cd1 I1 3.01346(19) 2_445 ? Cd1 I1 3.01346(19) 1_655 ? I1 Cd1 3.0135(2) 1_455 ? N1 C3 1.335(3) . ? N1 C2 1.336(3) . ? N2 C4 1.333(3) . ? N2 C1 1.334(4) . ? N3 C5 1.279(3) . ? N3 N3 1.406(4) 2_646 ? C1 C2 1.369(4) . ? C1 H1A 0.9300 . ? C2 H2A 0.9300 . ? C3 C4 1.389(3) . ? C3 H3A 0.9300 . ? C4 C5 1.489(3) . ? C5 C6 1.485(4) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? 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 Cd1 N1 180.00(14) . 2_545 ? N1 Cd1 I1 90.39(5) . 2_545 ? N1 Cd1 I1 89.61(5) 2_545 2_545 ? N1 Cd1 I1 89.61(5) . . ? N1 Cd1 I1 90.39(5) 2_545 . ? I1 Cd1 I1 180.000(7) 2_545 . ? N1 Cd1 I1 89.69(5) . 2_445 ? N1 Cd1 I1 90.31(5) 2_545 2_445 ? I1 Cd1 I1 88.404(6) 2_545 2_445 ? I1 Cd1 I1 91.596(6) . 2_445 ? N1 Cd1 I1 90.31(5) . 1_655 ? N1 Cd1 I1 89.69(5) 2_545 1_655 ? I1 Cd1 I1 91.596(6) 2_545 1_655 ? I1 Cd1 I1 88.404(6) . 1_655 ? I1 Cd1 I1 180.000(1) 2_445 1_655 ? Cd1 I1 Cd1 88.404(6) . 1_455 ? C3 N1 C2 116.5(2) . . ? C3 N1 Cd1 121.38(16) . . ? C2 N1 Cd1 122.07(17) . . ? C4 N2 C1 116.4(2) . . ? C5 N3 N3 113.1(3) . 2_646 ? N2 C1 C2 122.7(3) . . ? N2 C1 H1A 118.6 . . ? C2 C1 H1A 118.6 . . ? N1 C2 C1 121.3(2) . . ? N1 C2 H2A 119.4 . . ? C1 C2 H2A 119.4 . . ? N1 C3 C4 122.0(2) . . ? N1 C3 H3A 119.0 . . ? C4 C3 H3A 119.0 . . ? N2 C4 C3 121.0(2) . . ? N2 C4 C5 117.6(2) . . ? C3 C4 C5 121.4(2) . . ? N3 C5 C6 127.2(2) . . ? N3 C5 C4 114.5(2) . . ? C6 C5 C4 118.4(2) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.669 _refine_diff_density_min -0.460 _refine_diff_density_rms 0.092