# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _publ_contact_author_name 'Yao, Yuan-Gen' _publ_contact_author_email yyg@fjirsm.ac.cn loop_ _publ_author_name 'Yuan-Gen Yao' 'Pei-Xiu Yin' 'Jian Zhang' 'Ye-Yan Qin' 'Jian-kai Cheng' ; Zhao-Ji Li ; data_a _database_code_depnum_ccdc_archive 'CCDC 798302' #TrackingRef '- CEC-YPX(revision).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H5 N3 O2 Zn ' _chemical_formula_sum 'C4 H5 N3 O2 Zn ' _chemical_formula_weight 192.50 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pmn2(1) _symmetry_space_group_name_Hall 'P 2ac -2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y, z+1/2' '-x, y, z' _cell_length_a 9.303(6) _cell_length_b 8.413(6) _cell_length_c 8.161(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 638.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 785 _cell_measurement_theta_min 2.1891 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.1400 _exptl_crystal_size_min 0.1200 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.002 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 384 _exptl_absorpt_coefficient_mu 3.778 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 0.635 _exptl_absorpt_correction_T_min 0.535 _exptl_absorpt_process_details crystalclear _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 4776 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 27.50 _reflns_number_total 1556 _reflns_number_gt 1403 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0361P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(2) _refine_ls_number_reflns 1556 _refine_ls_number_parameters 108 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0300 _refine_ls_R_factor_gt 0.0276 _refine_ls_wR_factor_ref 0.0645 _refine_ls_wR_factor_gt 0.0628 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 0.5000 1.38548(7) 0.83553(6) 0.02048(14) Uani 1 2 d S . . Zn2 Zn 0.0000 1.01665(6) 1.17566(6) 0.01756(13) Uani 1 2 d S . . O1 O 0.5000 1.7656(4) 0.8113(4) 0.0275(8) Uani 1 2 d S . . O2 O 0.5000 1.5627(4) 0.9844(5) 0.0374(10) Uani 1 2 d S . . O3 O 0.0000 0.7971(4) 1.0290(5) 0.0283(8) Uani 1 2 d S . . O4 O 0.0000 0.5462(5) 1.1090(5) 0.0405(11) Uani 1 2 d S . . N1 N 0.1629(3) 1.1028(3) 1.0165(4) 0.0216(6) Uani 1 1 d . . . N2 N 0.3382(3) 1.0881(3) 0.8319(4) 0.0210(5) Uani 1 1 d . . . N3 N 0.3353(3) 1.2393(3) 0.8931(3) 0.0222(6) Uani 1 1 d . . . C1 C 0.2286(4) 1.2427(4) 1.0026(4) 0.0240(7) Uani 1 1 d . . . H1 H 0.2031 1.3326 1.0623 0.029 Uiso 1 1 calc R . . C2 C 0.2347(5) 1.0121(4) 0.9081(5) 0.0237(8) Uani 1 1 d . . . H2 H 0.2131 0.9058 0.8889 0.028 Uiso 1 1 calc R . . C3 C 0.5000 1.7105(6) 0.9518(6) 0.0227(10) Uani 1 2 d S . . C4 C 0.5000 1.8144(6) 1.1006(7) 0.0377(14) Uani 1 2 d S . . H43 H 0.5950 1.8177 1.1464 0.057 Uiso 0.50 1 calc PR . . H42 H 0.4343 1.7722 1.1802 0.057 Uiso 0.50 1 calc PR . . H41 H 0.4707 1.9199 1.0706 0.057 Uiso 0.50 1 calc PR . . C5 C 0.0000 0.6522(6) 1.0027(7) 0.0279(11) Uani 1 2 d S . . C6 C 0.0000 0.5964(9) 0.8273(9) 0.089(4) Uani 1 2 d S . . H63 H -0.0544 0.6692 0.7613 0.134 Uiso 0.50 1 calc PR . . H62 H -0.0426 0.4926 0.8211 0.134 Uiso 0.50 1 calc PR . . H61 H 0.0971 0.5917 0.7876 0.134 Uiso 0.50 1 calc PR . . 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 0.0218(3) 0.0180(3) 0.0216(3) 0.0011(2) 0.000 0.000 Zn2 0.0143(2) 0.0226(3) 0.0158(2) 0.0015(2) 0.000 0.000 O1 0.040(2) 0.0249(17) 0.0178(19) 0.0016(14) 0.000 0.000 O2 0.069(3) 0.0198(17) 0.0229(19) 0.0007(16) 0.000 0.000 O3 0.036(2) 0.0183(17) 0.0302(19) -0.0043(15) 0.000 0.000 O4 0.075(3) 0.0254(19) 0.0215(18) -0.0041(17) 0.000 0.000 N1 0.0176(14) 0.0259(14) 0.0213(14) 0.0027(12) 0.0035(11) 0.0015(10) N2 0.0187(13) 0.0228(13) 0.0216(13) -0.0037(13) 0.0026(12) -0.0019(10) N3 0.0214(15) 0.0180(14) 0.0273(15) -0.0007(11) 0.0040(10) -0.0016(11) C1 0.0217(17) 0.0250(16) 0.0253(16) -0.0013(15) 0.0058(14) 0.0006(12) C2 0.020(2) 0.0242(16) 0.0273(19) -0.0027(14) 0.0071(14) -0.0020(13) C3 0.024(2) 0.024(2) 0.020(2) 0.001(2) 0.000 0.000 C4 0.061(4) 0.026(3) 0.026(3) -0.007(3) 0.000 0.000 C5 0.039(3) 0.028(3) 0.017(2) -0.004(2) 0.000 0.000 C6 0.202(12) 0.042(4) 0.024(3) -0.014(3) 0.000 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 Zn1 O2 1.923(4) . ? Zn1 O4 1.936(4) 2_574 ? Zn1 N3 2.020(3) . ? Zn1 N3 2.020(3) 4_655 ? Zn2 N1 2.124(3) . ? Zn2 N1 2.124(3) 4 ? Zn2 O1 2.140(4) 2_585 ? Zn2 N2 2.161(3) 2_575 ? Zn2 N2 2.161(3) 3_475 ? Zn2 O3 2.201(4) . ? O1 C3 1.237(6) . ? O1 Zn2 2.140(4) 2_584 ? O2 C3 1.271(7) . ? O3 C5 1.238(6) . ? O4 C5 1.245(7) . ? O4 Zn1 1.936(4) 2_575 ? N1 C1 1.331(4) . ? N1 C2 1.346(5) . ? N2 C2 1.312(5) . ? N2 N3 1.366(4) . ? N2 Zn2 2.161(3) 2_574 ? N3 C1 1.336(4) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 C4 1.496(7) . ? C4 H43 0.9600 . ? C4 H42 0.9600 . ? C4 H41 0.9600 . ? C5 C6 1.507(9) . ? C6 H63 0.9600 . ? C6 H62 0.9600 . ? C6 H61 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 O2 Zn1 O4 111.88(17) . 2_574 ? O2 Zn1 N3 108.99(11) . . ? O4 Zn1 N3 113.76(10) 2_574 . ? O2 Zn1 N3 108.99(11) . 4_655 ? O4 Zn1 N3 113.76(10) 2_574 4_655 ? N3 Zn1 N3 98.65(18) . 4_655 ? N1 Zn2 N1 91.07(16) . 4 ? N1 Zn2 O1 91.40(11) . 2_585 ? N1 Zn2 O1 91.40(11) 4 2_585 ? N1 Zn2 N2 90.17(12) . 2_575 ? N1 Zn2 N2 175.86(11) 4 2_575 ? O1 Zn2 N2 92.52(11) 2_585 2_575 ? N1 Zn2 N2 175.86(11) . 3_475 ? N1 Zn2 N2 90.17(12) 4 3_475 ? O1 Zn2 N2 92.52(11) 2_585 3_475 ? N2 Zn2 N2 88.32(16) 2_575 3_475 ? N1 Zn2 O3 87.34(11) . . ? N1 Zn2 O3 87.34(11) 4 . ? O1 Zn2 O3 178.21(14) 2_585 . ? N2 Zn2 O3 88.77(11) 2_575 . ? N2 Zn2 O3 88.77(11) 3_475 . ? C3 O1 Zn2 143.2(3) . 2_584 ? C3 O2 Zn1 128.8(4) . . ? C5 O3 Zn2 157.0(4) . . ? C5 O4 Zn1 116.9(3) . 2_575 ? C1 N1 C2 102.6(3) . . ? C1 N1 Zn2 133.0(2) . . ? C2 N1 Zn2 124.3(2) . . ? C2 N2 N3 105.4(3) . . ? C2 N2 Zn2 126.3(2) . 2_574 ? N3 N2 Zn2 127.5(2) . 2_574 ? C1 N3 N2 106.2(3) . . ? C1 N3 Zn1 134.9(2) . . ? N2 N3 Zn1 117.8(2) . . ? N1 C1 N3 112.3(3) . . ? N1 C1 H1 123.9 . . ? N3 C1 H1 123.9 . . ? N2 C2 N1 113.5(3) . . ? N2 C2 H2 123.2 . . ? N1 C2 H2 123.2 . . ? O1 C3 O2 124.1(5) . . ? O1 C3 C4 122.2(4) . . ? O2 C3 C4 113.7(4) . . ? C3 C4 H43 109.5 . . ? C3 C4 H42 109.5 . . ? H43 C4 H42 109.5 . . ? C3 C4 H41 109.5 . . ? H43 C4 H41 109.5 . . ? H42 C4 H41 109.5 . . ? O3 C5 O4 125.8(5) . . ? O3 C5 C6 118.2(5) . . ? O4 C5 C6 116.0(5) . . ? C5 C6 H63 109.5 . . ? C5 C6 H62 109.5 . . ? H63 C6 H62 109.5 . . ? C5 C6 H61 109.5 . . ? H63 C6 H61 109.5 . . ? H62 C6 H61 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.450 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.086 #===END ## Crystallographic Data for compound 2 data_2 _database_code_depnum_ccdc_archive 'CCDC 798303' #TrackingRef '- CEC-YPX(revision).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H9 N9 O2 Zn2' _chemical_formula_sum 'C8 H9 N9 O2 Zn2' _chemical_formula_weight 394.02 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma _symmetry_space_group_name_Hall '-P 2ac 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 7.663(3) _cell_length_b 10.104(4) _cell_length_c 17.426(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1349.2(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1428 _cell_measurement_theta_min 2.3296 _cell_measurement_theta_max 27.4719 _exptl_crystal_description Needle _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.1800 _exptl_crystal_size_mid 0.1400 _exptl_crystal_size_min 0.1300 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.940 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 3.575 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 0.628 _exptl_absorpt_correction_T_min 0.554 _exptl_absorpt_process_details crystalclear _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 9697 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0213 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 27.45 _reflns_number_total 1620 _reflns_number_gt 1453 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0349P)^2^+1.8093P] 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 0.0022(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1620 _refine_ls_number_parameters 119 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0349 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0761 _refine_ls_wR_factor_gt 0.0738 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _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 Zn1 Zn 0.15692(6) -0.2500 -0.08445(2) 0.02024(15) Uani 1 2 d S . . Zn2 Zn -0.00750(5) 0.2500 -0.26119(2) 0.01578(14) Uani 1 2 d S . . N1 N 0.1500(3) 0.0971(2) -0.20757(13) 0.0213(5) Uani 1 1 d . . . N2 N 0.3258(3) 0.0983(2) -0.19236(13) 0.0199(4) Uani 1 1 d . . . N3 N 0.2123(3) -0.0836(2) -0.14095(13) 0.0220(5) Uani 1 1 d . . . N4 N 0.3390(4) -0.2500 0.14161(17) 0.0198(6) Uani 1 2 d S . . N5 N 0.1621(4) -0.2500 0.15229(17) 0.0229(7) Uani 1 2 d S . . N6 N 0.2130(4) -0.2500 0.02704(17) 0.0225(7) Uani 1 2 d S . . C1 C 0.0894(4) -0.0117(3) -0.17613(16) 0.0276(6) Uani 1 1 d . . . H1 H -0.0275 -0.0364 -0.1781 0.033 Uiso 1 1 calc R . . C2 C 0.3576(3) -0.0111(3) -0.15323(16) 0.0261(6) Uani 1 1 d . . . H2 H 0.4679 -0.0355 -0.1360 0.031 Uiso 1 1 calc R . . C3 C 0.3633(5) -0.2500 0.0668(2) 0.0253(8) Uani 1 2 d S . . H3 H 0.4729 -0.2500 0.0439 0.030 Uiso 1 2 calc SR . . C4 C 0.0931(5) -0.2500 0.0832(2) 0.0272(9) Uani 1 2 d S . . H4 H -0.0266 -0.2500 0.0742 0.033 Uiso 1 2 calc SR . . C6 C -0.2252(15) -0.0891(11) -0.0332(7) 0.080(3) Uani 0.50 1 d P . . H6A H -0.1048 -0.0656 -0.0266 0.120 Uiso 0.50 1 calc PR . . H6B H -0.2800 -0.0966 0.0162 0.120 Uiso 0.50 1 calc PR . . H6C H -0.2831 -0.0220 -0.0627 0.120 Uiso 0.50 1 calc PR . . C5 C -0.2374(9) -0.2197(6) -0.0746(5) 0.045(2) Uani 0.50 1 d P . . O1 O -0.1005(5) -0.2500 -0.0897(2) 0.0643(12) Uani 1 2 d S . . O2 O -0.3850(6) -0.2500 -0.0834(3) 0.0719(14) Uani 1 2 d S . . 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 0.0294(3) 0.0156(2) 0.0158(2) 0.000 -0.00019(16) 0.000 Zn2 0.0119(2) 0.0173(2) 0.0181(2) 0.000 -0.00031(14) 0.000 N1 0.0125(10) 0.0210(10) 0.0304(12) 0.0076(9) -0.0009(8) -0.0001(8) N2 0.0129(10) 0.0210(10) 0.0259(11) 0.0047(9) -0.0015(8) -0.0007(8) N3 0.0245(11) 0.0183(10) 0.0232(11) 0.0047(9) -0.0011(9) 0.0002(9) N4 0.0132(14) 0.0286(16) 0.0176(14) 0.000 0.0004(11) 0.000 N5 0.0144(15) 0.0377(18) 0.0165(14) 0.000 0.0000(11) 0.000 N6 0.0249(16) 0.0267(16) 0.0160(15) 0.000 0.0006(12) 0.000 C1 0.0194(13) 0.0250(13) 0.0384(16) 0.0115(12) -0.0016(11) -0.0038(11) C2 0.0196(12) 0.0256(13) 0.0331(14) 0.0092(11) -0.0027(11) 0.0021(11) C3 0.0178(18) 0.038(2) 0.0197(17) 0.000 0.0041(14) 0.000 C4 0.0182(19) 0.045(2) 0.0180(18) 0.000 -0.0024(14) 0.000 C6 0.086(8) 0.067(6) 0.087(8) -0.014(6) 0.000(6) 0.011(6) C5 0.028(3) 0.038(6) 0.068(4) 0.012(3) 0.002(3) -0.001(2) O1 0.029(2) 0.099(4) 0.064(3) 0.000 -0.0036(18) 0.000 O2 0.038(2) 0.091(4) 0.087(4) 0.000 0.002(2) 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 Zn1 O1 1.975(4) . ? Zn1 N6 1.990(3) . ? Zn1 N3 1.994(2) 8 ? Zn1 N3 1.994(2) . ? Zn2 N4 2.130(3) 2_554 ? Zn2 N2 2.153(2) 6 ? Zn2 N2 2.153(2) 3_454 ? Zn2 N1 2.171(2) 8_565 ? Zn2 N1 2.171(2) . ? Zn2 N5 2.237(3) 5 ? N1 C1 1.314(3) . ? N1 N2 1.373(3) . ? N2 C2 1.321(3) . ? N2 Zn2 2.153(2) 6_655 ? N3 C1 1.338(3) . ? N3 C2 1.350(3) . ? N4 C3 1.316(5) . ? N4 N5 1.369(4) . ? N4 Zn2 2.130(3) 2 ? N5 C4 1.314(5) . ? N5 Zn2 2.237(3) 5 ? N6 C3 1.344(5) . ? N6 C4 1.343(5) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C6 C5 1.507(12) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C5 C5 0.612(13) 8 ? C5 O1 1.124(8) . ? C5 O2 1.182(8) . ? O1 C5 1.124(8) 8 ? O2 C5 1.182(8) 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 O1 Zn1 N6 105.11(16) . . ? O1 Zn1 N3 100.93(9) . 8 ? N6 Zn1 N3 115.86(8) . 8 ? O1 Zn1 N3 100.93(9) . . ? N6 Zn1 N3 115.86(8) . . ? N3 Zn1 N3 114.97(13) 8 . ? N4 Zn2 N2 93.48(8) 2_554 6 ? N4 Zn2 N2 93.48(8) 2_554 3_454 ? N2 Zn2 N2 90.76(12) 6 3_454 ? N4 Zn2 N1 90.30(8) 2_554 8_565 ? N2 Zn2 N1 176.21(8) 6 8_565 ? N2 Zn2 N1 89.15(9) 3_454 8_565 ? N4 Zn2 N1 90.30(8) 2_554 . ? N2 Zn2 N1 89.15(9) 6 . ? N2 Zn2 N1 176.21(8) 3_454 . ? N1 Zn2 N1 90.68(12) 8_565 . ? N4 Zn2 N5 174.65(11) 2_554 5 ? N2 Zn2 N5 90.28(8) 6 5 ? N2 Zn2 N5 90.28(8) 3_454 5 ? N1 Zn2 N5 85.94(8) 8_565 5 ? N1 Zn2 N5 85.94(8) . 5 ? C1 N1 N2 105.9(2) . . ? C1 N1 Zn2 125.34(18) . . ? N2 N1 Zn2 128.48(16) . . ? C2 N2 N1 105.9(2) . . ? C2 N2 Zn2 132.85(18) . 6_655 ? N1 N2 Zn2 121.04(15) . 6_655 ? C1 N3 C2 102.3(2) . . ? C1 N3 Zn1 122.29(18) . . ? C2 N3 Zn1 135.33(18) . . ? C3 N4 N5 105.9(3) . . ? C3 N4 Zn2 134.6(3) . 2 ? N5 N4 Zn2 119.5(2) . 2 ? C4 N5 N4 105.9(3) . . ? C4 N5 Zn2 124.3(3) . 5 ? N4 N5 Zn2 129.8(2) . 5 ? C3 N6 C4 102.1(3) . . ? C3 N6 Zn1 133.5(3) . . ? C4 N6 Zn1 124.3(3) . . ? N1 C1 N3 113.4(2) . . ? N1 C1 H1 123.3 . . ? N3 C1 H1 123.3 . . ? N2 C2 N3 112.6(2) . . ? N2 C2 H2 123.7 . . ? N3 C2 H2 123.7 . . ? N4 C3 N6 112.9(3) . . ? N4 C3 H3 123.5 . . ? N6 C3 H3 123.5 . . ? N5 C4 N6 113.1(3) . . ? N5 C4 H4 123.5 . . ? N6 C4 H4 123.5 . . ? 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 . . ? C5 C5 O1 74.2(3) 8 . ? C5 C5 O2 75.0(3) 8 . ? O1 C5 O2 142.4(7) . . ? C5 C5 C6 151.1(5) 8 . ? O1 C5 C6 107.0(7) . . ? O2 C5 C6 110.4(7) . . ? C5 O1 C5 31.6(7) 8 . ? C5 O1 Zn1 157.2(5) 8 . ? C5 O1 Zn1 157.2(5) . . ? C5 O2 C5 30.0(6) . 8 ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 1.208 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.097 #===END ## Crystallographic Data for compound 3 data_3 _database_code_depnum_ccdc_archive 'CCDC 798304' #TrackingRef '- CEC-YPX(revision).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H20 Cd3 Cl3 N11 O2' _chemical_formula_sum 'C12 H20 Cd3 Cl3 N11 O2' _chemical_formula_weight 793.97 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' Cd Cd -0.8075 1.2024 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'C m c 21' _symmetry_space_group_name_Hall 'C 2c -2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, 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' '-x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 11.856(8) _cell_length_b 12.019(8) _cell_length_c 16.688(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2378(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1247 _cell_measurement_theta_min 2.4120 _cell_measurement_theta_max 27.4410 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.1400 _exptl_crystal_size_mid 0.1200 _exptl_crystal_size_min 0.1000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.218 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 3.029 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 0.739 _exptl_absorpt_correction_T_min 0.661 _exptl_absorpt_process_details crystalclear _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 8644 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 27.40 _reflns_number_total 2840 _reflns_number_gt 2306 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0393P)^2^+20.3521P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(6) _refine_ls_number_reflns 2448 _refine_ls_number_parameters 163 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0463 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.0956 _refine_ls_wR_factor_gt 0.0929 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.006 _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 -1.0000 0.06145(6) -0.32061(5) 0.02564(19) Uani 1 2 d S . . Cd2 Cd -1.0000 -0.30719(6) -0.17980(5) 0.02559(18) Uani 1 2 d S . . Cd3 Cd -1.0000 0.37937(6) -0.28458(5) 0.02484(18) Uani 1 2 d S . . Cl1 Cl -1.0000 -0.0761(2) -0.2006(2) 0.0355(7) Uani 1 2 d S . . Cl2 Cl -1.0000 0.5688(3) -0.3437(2) 0.0391(7) Uani 1 2 d S . . Cl3 Cl -1.0000 -0.5200(2) -0.1428(2) 0.0434(8) Uani 1 2 d S . . N1 N -0.8498(5) 0.1616(5) -0.2692(5) 0.0274(14) Uani 1 1 d . . . N2 N -0.8523(6) 0.2737(5) -0.2473(5) 0.0314(16) Uani 1 1 d . . . N3 N -0.6824(6) 0.2060(5) -0.2177(5) 0.0282(14) Uani 1 1 d . . . N4 N -1.0000 0.2982(8) -0.4133(6) 0.035(2) Uani 1 2 d S . . N5 N -1.0000 0.1872(7) -0.4284(7) 0.030(2) Uani 1 2 d S . . N6 N -1.0000 0.2720(8) -0.5455(6) 0.031(2) Uani 1 2 d S . . N7 N -1.1702(8) -0.1779(8) -0.4782(6) 0.050(2) Uani 1 1 d . . . O1 O -1.1338(9) -0.0416(6) -0.3905(7) 0.080(3) Uani 1 1 d . . . C1 C -0.7473(7) 0.1258(8) -0.2500(6) 0.0294(16) Uani 1 1 d . . . H1 H -0.7229 0.0531 -0.2581 0.035 Uiso 1 1 calc R . . C2 C -0.7503(8) 0.2957(6) -0.2181(5) 0.0282(17) Uani 1 1 d . . . H2 H -0.7283 0.3655 -0.1999 0.034 Uiso 1 1 calc R . . C3 C -1.0000 0.3474(10) -0.4825(7) 0.035(3) Uani 1 2 d S . . H3 H -1.0000 0.4242 -0.4891 0.042 Uiso 1 2 calc SR . . C4 C -1.0000 0.1744(10) -0.5044(9) 0.033(2) Uani 1 2 d S . . H4 H -1.0000 0.1051 -0.5291 0.040 Uiso 1 2 calc SR . . C5 C -1.1438(11) -0.1400(9) -0.4068(7) 0.056(3) Uani 1 1 d . . . C6 C -1.191(2) -0.1003(13) -0.5414(10) 0.136(11) Uani 1 1 d . . . H6A H -1.2557 -0.1242 -0.5717 0.205 Uiso 1 1 calc R . . H6B H -1.1266 -0.0966 -0.5759 0.205 Uiso 1 1 calc R . . H6C H -1.2057 -0.0281 -0.5190 0.205 Uiso 1 1 calc R . . C7 C -1.1865(13) -0.2962(10) -0.4929(11) 0.079(5) Uani 1 1 d . . . H7A H -1.1269 -0.3234 -0.5266 0.118 Uiso 1 1 calc R . . H7B H -1.2577 -0.3077 -0.5189 0.118 Uiso 1 1 calc R . . H7C H -1.1855 -0.3356 -0.4429 0.118 Uiso 1 1 calc R . . H5 H -1.148(9) -0.214(8) -0.361(6) 0.04(3) 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 Cd1 0.0320(4) 0.0215(3) 0.0234(4) -0.0002(3) 0.000 0.000 Cd2 0.0232(4) 0.0279(4) 0.0257(4) 0.0018(3) 0.000 0.000 Cd3 0.0268(4) 0.0202(3) 0.0275(4) -0.0015(3) 0.000 0.000 Cl1 0.0373(14) 0.0303(13) 0.0388(18) 0.0148(12) 0.000 0.000 Cl2 0.0470(17) 0.0292(13) 0.0411(19) 0.0064(12) 0.000 0.000 Cl3 0.077(2) 0.0254(13) 0.0276(15) -0.0007(12) 0.000 0.000 N1 0.028(3) 0.019(3) 0.035(4) 0.002(3) 0.001(3) -0.001(2) N2 0.030(4) 0.021(3) 0.044(4) 0.004(3) 0.000(3) 0.005(3) N3 0.026(3) 0.024(3) 0.035(4) 0.003(3) -0.006(3) -0.003(2) N4 0.059(7) 0.021(4) 0.025(6) 0.001(4) 0.000 0.000 N5 0.039(5) 0.018(4) 0.031(5) 0.006(4) 0.000 0.000 N6 0.052(6) 0.030(5) 0.012(5) 0.001(4) 0.000 0.000 N7 0.058(5) 0.054(5) 0.038(4) -0.001(4) -0.008(4) -0.015(4) O1 0.119(8) 0.041(4) 0.081(7) -0.022(4) -0.057(6) -0.005(5) C1 0.029(3) 0.023(3) 0.036(4) -0.003(3) -0.006(4) 0.000(3) C2 0.026(4) 0.023(3) 0.036(5) -0.004(4) 0.000(4) 0.001(3) C3 0.077(9) 0.019(4) 0.010(5) 0.005(4) 0.000 0.000 C4 0.045(7) 0.027(5) 0.028(6) -0.007(5) 0.000 0.000 C5 0.076(8) 0.047(5) 0.046(7) -0.012(5) -0.020(6) -0.005(6) C6 0.27(3) 0.089(10) 0.051(9) 0.023(9) -0.069(14) -0.068(14) C7 0.078(9) 0.064(8) 0.095(12) -0.019(7) -0.031(9) 0.012(7) _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 2.314(7) . ? Cd1 N1 2.314(7) 3_355 ? Cd1 O1 2.326(8) . ? Cd1 O1 2.326(8) 3_355 ? Cd1 N5 2.350(10) . ? Cd1 Cl1 2.597(3) . ? Cd2 N3 2.258(7) 5_445 ? Cd2 N3 2.258(7) 7_345 ? Cd2 N6 2.281(10) 2_355 ? Cd2 Cl3 2.631(3) . ? Cd2 Cl1 2.799(3) . ? Cd3 N2 2.251(7) . ? Cd3 N2 2.251(7) 3_355 ? Cd3 N4 2.359(11) . ? Cd3 Cl2 2.481(3) . ? Cd3 Cl3 2.658(4) 1_565 ? Cl3 Cd3 2.658(4) 1_545 ? N1 C1 1.329(11) . ? N1 N2 1.397(9) . ? N2 C2 1.330(12) . ? N3 C1 1.346(11) . ? N3 C2 1.346(10) . ? N3 Cd2 2.258(7) 5 ? N4 C3 1.297(16) . ? N4 N5 1.357(13) . ? N5 C4 1.277(18) . ? N6 C4 1.358(16) . ? N6 C3 1.388(16) . ? N6 Cd2 2.281(10) 2_354 ? N7 C5 1.313(14) . ? N7 C6 1.430(17) . ? N7 C7 1.456(14) . ? O1 C5 1.219(12) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C5 H5 1.17(10) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? 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 100.6(3) . 3_355 ? N1 Cd1 O1 170.9(4) . . ? N1 Cd1 O1 86.4(3) 3_355 . ? N1 Cd1 O1 86.4(3) . 3_355 ? N1 Cd1 O1 170.9(4) 3_355 3_355 ? O1 Cd1 O1 86.0(6) . 3_355 ? N1 Cd1 N5 87.1(2) . . ? N1 Cd1 N5 87.1(2) 3_355 . ? O1 Cd1 N5 87.6(3) . . ? O1 Cd1 N5 87.6(3) 3_355 . ? N1 Cd1 Cl1 92.59(18) . . ? N1 Cd1 Cl1 92.59(18) 3_355 . ? O1 Cd1 Cl1 92.8(3) . . ? O1 Cd1 Cl1 92.8(3) 3_355 . ? N5 Cd1 Cl1 179.5(3) . . ? N3 Cd2 N3 146.5(4) 5_445 7_345 ? N3 Cd2 N6 105.2(2) 5_445 2_355 ? N3 Cd2 N6 105.2(2) 7_345 2_355 ? N3 Cd2 Cl3 97.69(16) 5_445 . ? N3 Cd2 Cl3 97.69(16) 7_345 . ? N6 Cd2 Cl3 87.1(2) 2_355 . ? N3 Cd2 Cl1 84.02(15) 5_445 . ? N3 Cd2 Cl1 84.02(15) 7_345 . ? N6 Cd2 Cl1 86.4(2) 2_355 . ? Cl3 Cd2 Cl1 173.54(11) . . ? N2 Cd3 N2 102.1(4) . 3_355 ? N2 Cd3 N4 91.1(2) . . ? N2 Cd3 N4 91.1(2) 3_355 . ? N2 Cd3 Cl2 128.89(18) . . ? N2 Cd3 Cl2 128.89(18) 3_355 . ? N4 Cd3 Cl2 91.0(2) . . ? N2 Cd3 Cl3 90.6(2) . 1_565 ? N2 Cd3 Cl3 90.6(2) 3_355 1_565 ? N4 Cd3 Cl3 177.3(2) . 1_565 ? Cl2 Cd3 Cl3 86.36(12) . 1_565 ? Cd1 Cl1 Cd2 136.64(14) . . ? Cd2 Cl3 Cd3 103.51(13) . 1_545 ? C1 N1 N2 105.6(6) . . ? C1 N1 Cd1 128.7(5) . . ? N2 N1 Cd1 125.6(5) . . ? C2 N2 N1 105.6(6) . . ? C2 N2 Cd3 134.1(5) . . ? N1 N2 Cd3 119.2(5) . . ? C1 N3 C2 103.2(8) . . ? C1 N3 Cd2 127.6(6) . 5 ? C2 N3 Cd2 129.1(5) . 5 ? C3 N4 N5 106.4(10) . . ? C3 N4 Cd3 128.5(8) . . ? N5 N4 Cd3 125.1(8) . . ? C4 N5 N4 107.6(10) . . ? C4 N5 Cd1 133.1(9) . . ? N4 N5 Cd1 119.3(8) . . ? C4 N6 C3 100.4(10) . . ? C4 N6 Cd2 131.0(8) . 2_354 ? C3 N6 Cd2 128.5(7) . 2_354 ? C5 N7 C6 119.0(10) . . ? C5 N7 C7 121.6(11) . . ? C6 N7 C7 119.3(11) . . ? C5 O1 Cd1 134.0(8) . . ? N1 C1 N3 112.8(8) . . ? N1 C1 H1 123.6 . . ? N3 C1 H1 123.6 . . ? N2 C2 N3 112.8(7) . . ? N2 C2 H2 123.6 . . ? N3 C2 H2 123.6 . . ? N4 C3 N6 112.1(9) . . ? N4 C3 H3 123.9 . . ? N6 C3 H3 123.9 . . ? N5 C4 N6 113.4(11) . . ? N5 C4 H4 123.3 . . ? N6 C4 H4 123.3 . . ? O1 C5 N7 124.2(12) . . ? O1 C5 H5 126(5) . . ? N7 C5 H5 109(5) . . ? N7 C6 H6A 109.5 . . ? N7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N7 C7 H7A 109.5 . . ? N7 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N7 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.40 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.158 _refine_diff_density_min -1.005 _refine_diff_density_rms 0.153 #===END ## Crystallographic Data for compound 4 data_4 _database_code_depnum_ccdc_archive 'CCDC 798305' #TrackingRef '- CEC-YPX(revision).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C2 H3 Cd Cl2 N3, 0.5(H2O), 0.5(H2O)' _chemical_formula_sum 'C2 H5 Cd Cl2 N3 O ' _chemical_formula_weight 270.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Imma _symmetry_space_group_name_Hall '-I 2b 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' 'x, -y, -z' '-x, y+1/2, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1, -z+1/2' '-x, -y, -z' 'x, y-1/2, -z' '-x, y, z' 'x, -y-1/2, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y, z+1/2' _cell_length_a 7.09(2) _cell_length_b 7.24(2) _cell_length_c 11.96(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 614(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 357 _cell_measurement_theta_min 3.2864 _cell_measurement_theta_max 27.4179 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.1600 _exptl_crystal_size_min 0.1000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.903 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 504 _exptl_absorpt_coefficient_mu 4.334 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 0.648 _exptl_absorpt_correction_T_min 0.439 _exptl_absorpt_process_details crystalclear _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 2310 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.0284 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 27.64 _reflns_number_total 421 _reflns_number_gt 389 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.1554P)^2^+13.7156P] 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 412 _refine_ls_number_parameters 35 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0636 _refine_ls_R_factor_gt 0.0624 _refine_ls_wR_factor_ref 0.2198 _refine_ls_wR_factor_gt 0.2184 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _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 Cd1 Cd -0.2500 0.7500 -0.2500 0.0319(7) Uani 1 4 d S . . Cl1 Cl 0.0000 0.5058(4) -0.3196(3) 0.0313(8) Uani 1 2 d S . . N1 N -0.0997(12) 0.7500 -0.0799(8) 0.029(2) Uani 1 2 d S . . N2 N 0.0000 0.7500 0.0891(14) 0.074(8) Uani 1 4 d S . . H2 H 0.0000 0.7500 0.1610 0.089 Uiso 1 4 d SR . . C1 C -0.153(2) 0.7500 0.0244(12) 0.043(3) Uani 1 2 d S . . H1 H -0.2771 0.7500 0.0496 0.051 Uiso 1 2 calc SR . . O2W O -0.5000 0.7500 -0.002(7) 0.11(3) Uani 0.50 4 d SP . . O1W O 0.2500 0.7500 0.2500 0.061(15) Uani 0.50 4 d SP . . 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 0.0216(9) 0.0456(10) 0.0285(9) 0.000 -0.0022(4) 0.000 Cl1 0.0259(15) 0.0331(15) 0.0348(15) -0.0047(11) 0.000 0.000 N1 0.010(4) 0.055(6) 0.023(4) 0.000 0.003(3) 0.000 N2 0.13(3) 0.080(16) 0.013(7) 0.000 0.000 0.000 C1 0.036(7) 0.057(9) 0.035(7) 0.000 0.021(6) 0.000 O2W 0.026(18) 0.06(3) 0.25(9) 0.000 0.000 0.000 O1W 0.03(2) 0.026(14) 0.12(5) 0.000 0.008(16) 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 Cd1 N1 2.296(10) . ? Cd1 N1 2.296(10) 13_464 ? Cd1 Cl1 2.638(5) 14_454 ? Cd1 Cl1 2.638(5) 13_464 ? Cd1 Cl1 2.638(5) 2_565 ? Cd1 Cl1 2.638(5) . ? Cl1 Cd1 2.638(5) 2_565 ? N1 C1 1.304(16) . ? N1 N1 1.414(18) 2_565 ? N2 C1 1.332(19) . ? N2 C1 1.332(19) 2_565 ? N2 H2 0.8600 . ? C1 H1 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd1 N1 180.0 . 13_464 ? N1 Cd1 Cl1 91.8(2) . 14_454 ? N1 Cd1 Cl1 88.2(2) 13_464 14_454 ? N1 Cd1 Cl1 91.8(2) . 13_464 ? N1 Cd1 Cl1 88.2(2) 13_464 13_464 ? Cl1 Cd1 Cl1 84.1(2) 14_454 13_464 ? N1 Cd1 Cl1 88.2(2) . 2_565 ? N1 Cd1 Cl1 91.8(2) 13_464 2_565 ? Cl1 Cd1 Cl1 180.0 14_454 2_565 ? Cl1 Cd1 Cl1 95.9(2) 13_464 2_565 ? N1 Cd1 Cl1 88.2(2) . . ? N1 Cd1 Cl1 91.8(2) 13_464 . ? Cl1 Cd1 Cl1 95.9(2) 14_454 . ? Cl1 Cd1 Cl1 180.00(17) 13_464 . ? Cl1 Cd1 Cl1 84.1(2) 2_565 . ? Cd1 Cl1 Cd1 84.4(2) 2_565 . ? C1 N1 N1 106.8(8) . 2_565 ? C1 N1 Cd1 135.5(10) . . ? N1 N1 Cd1 117.6(2) 2_565 . ? C1 N2 C1 109.0(16) . 2_565 ? C1 N2 H2 125.5 . . ? C1 N2 H2 125.5 2_565 . ? N1 C1 N2 108.7(13) . . ? N1 C1 H1 125.7 . . ? N2 C1 H1 125.7 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.64 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.523 _refine_diff_density_min -2.732 _refine_diff_density_rms 0.366 #===END ## Crystallographic Data for compound 5 data_5 _database_code_depnum_ccdc_archive 'CCDC 798306' #TrackingRef '- CEC-YPX(revision).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H9 Cd2 Cl N12' _chemical_formula_sum 'C6 H9 Cd2 Cl N12' _chemical_formula_weight 509.52 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' Cd Cd -0.8075 1.2024 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n m a ' _symmetry_space_group_name_Hall '-P 2ac 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 16.562(7) _cell_length_b 10.103(4) _cell_length_c 7.904(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1322.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1487 _cell_measurement_theta_min 2.0156 _cell_measurement_theta_max 27.4797 _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.2300 _exptl_crystal_size_mid 0.1800 _exptl_crystal_size_min 0.1600 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 3.432 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 0.577 _exptl_absorpt_correction_T_min 0.481 _exptl_absorpt_process_details crystalclear _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time 0 _diffrn_standards_decay_% none _diffrn_reflns_number 9763 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_sigmaI/netI 0.0188 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 27.47 _reflns_number_total 1606 _reflns_number_gt 1525 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0272P)^2^+3.7331P] 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 1606 _refine_ls_number_parameters 123 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0274 _refine_ls_R_factor_gt 0.0254 _refine_ls_wR_factor_ref 0.0592 _refine_ls_wR_factor_gt 0.0579 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.230079(19) 0.2500 -0.10997(4) 0.01348(10) Uani 1 2 d S . . Cd2 Cd 0.461414(19) 0.2500 -0.03966(4) 0.01543(10) Uani 1 2 d S . . Cl1 Cl 0.36764(7) 0.2500 -0.30756(15) 0.0214(2) Uani 1 2 d S . . C1 C 0.39159(19) -0.0270(3) 0.1675(4) 0.0154(6) Uani 1 1 d . . . C2 C 0.2666(2) -0.0035(3) 0.1374(4) 0.0207(7) Uani 1 1 d . . . H2 H 0.2111 -0.0164 0.1455 0.025 Uiso 1 1 calc R . . C3 C 0.0484(3) 0.2500 0.0204(5) 0.0149(9) Uani 1 2 d S . . H3 H 0.0336 0.2500 -0.0931 0.018 Uiso 1 2 calc SR . . C4 C 0.1189(3) 0.2500 0.2517(6) 0.0196(9) Uani 1 2 d S . . N1 N 0.29955(16) 0.0929(3) 0.0494(4) 0.0203(6) Uani 1 1 d . . . N2 N 0.38237(16) 0.0782(3) 0.0687(4) 0.0180(6) Uani 1 1 d . . . N3 N 0.32141(17) -0.0822(3) 0.2151(4) 0.0190(6) Uani 1 1 d . . . N4 N 0.46733(17) -0.0799(3) 0.2100(4) 0.0183(6) Uani 1 1 d . . . N5 N 0.0002(3) 0.2500 0.1497(7) 0.0389(12) Uani 1 2 d S . . N6 N 0.0404(2) 0.2500 0.3009(5) 0.0235(9) Uani 1 2 d S . . N7 N 0.1258(3) 0.2500 0.0839(5) 0.0216(9) Uani 1 2 d S . . N8 N 0.1825(3) 0.2500 0.3599(7) 0.0353(12) Uani 1 2 d S . . HN81 H 0.228(3) 0.2500 0.319(7) 0.016(14) Uiso 1 2 d S . . HN41 H 0.505(3) -0.020(4) 0.199(5) 0.028(11) Uiso 1 1 d . . . HN42 H 0.461(3) -0.113(5) 0.302(6) 0.036(13) Uiso 1 1 d . . . HN82 H 0.184(4) 0.2500 0.464(9) 0.034(18) Uiso 1 2 d S . . 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 0.01318(17) 0.01379(17) 0.01347(16) 0.000 -0.00134(11) 0.000 Cd2 0.01375(17) 0.01749(18) 0.01504(17) 0.000 -0.00047(12) 0.000 Cl1 0.0160(5) 0.0300(6) 0.0183(5) 0.000 0.0000(4) 0.000 C1 0.0147(14) 0.0163(15) 0.0152(14) 0.0008(12) 0.0005(12) 0.0012(11) C2 0.0165(16) 0.0173(16) 0.0285(18) 0.0049(14) 0.0013(13) 0.0007(12) C3 0.009(2) 0.029(2) 0.0060(19) 0.000 -0.0031(15) 0.000 C4 0.020(2) 0.023(2) 0.015(2) 0.000 0.0030(18) 0.000 N1 0.0144(14) 0.0189(14) 0.0275(16) 0.0072(12) -0.0018(11) 0.0009(11) N2 0.0129(13) 0.0177(14) 0.0234(14) 0.0046(12) 0.0006(11) -0.0002(10) N3 0.0160(13) 0.0182(13) 0.0227(14) 0.0057(12) 0.0022(11) 0.0004(11) N4 0.0165(14) 0.0199(14) 0.0185(15) 0.0040(12) 0.0006(11) 0.0016(11) N5 0.039(3) 0.049(3) 0.029(3) 0.000 0.000(2) 0.000 N6 0.018(2) 0.035(2) 0.017(2) 0.000 0.0027(16) 0.000 N7 0.017(2) 0.033(2) 0.0151(19) 0.000 0.0012(15) 0.000 N8 0.018(2) 0.068(4) 0.020(2) 0.000 -0.0017(19) 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 Cd1 N7 2.309(4) . ? Cd1 N1 2.330(3) 8_565 ? Cd1 N1 2.330(3) . ? Cd1 N3 2.348(3) 2_554 ? Cd1 N3 2.348(3) 7_665 ? Cd1 Cl1 2.7622(15) . ? Cd2 N6 2.296(4) 6_656 ? Cd2 N2 2.337(3) . ? Cd2 N2 2.337(3) 8_565 ? Cd2 N4 2.481(3) 5_655 ? Cd2 N4 2.481(3) 4_655 ? Cd2 Cl1 2.6259(14) . ? C1 N2 1.327(4) . ? C1 N3 1.343(4) . ? C1 N4 1.405(4) . ? C2 N1 1.316(4) . ? C2 N3 1.354(4) . ? C2 H2 0.9300 . ? C3 N5 1.297(7) . ? C3 N7 1.377(6) . ? C3 H3 0.9300 . ? C4 N7 1.331(6) . ? C4 N6 1.356(6) . ? C4 N8 1.357(7) . ? N1 N2 1.388(4) . ? N3 Cd1 2.348(3) 2 ? N4 Cd2 2.481(3) 5_655 ? N4 HN41 0.87(5) . ? N4 HN42 0.81(5) . ? N5 N6 1.368(7) . ? N6 Cd2 2.296(4) 6_556 ? N8 HN81 0.83(6) . ? N8 HN82 0.82(7) . ? 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 N7 Cd1 N1 90.60(11) . 8_565 ? N7 Cd1 N1 90.60(11) . . ? N1 Cd1 N1 85.86(15) 8_565 . ? N7 Cd1 N3 96.85(10) . 2_554 ? N1 Cd1 N3 171.68(10) 8_565 2_554 ? N1 Cd1 N3 90.34(10) . 2_554 ? N7 Cd1 N3 96.85(10) . 7_665 ? N1 Cd1 N3 90.34(10) 8_565 7_665 ? N1 Cd1 N3 171.68(10) . 7_665 ? N3 Cd1 N3 92.44(14) 2_554 7_665 ? N7 Cd1 Cl1 172.84(11) . . ? N1 Cd1 Cl1 84.17(8) 8_565 . ? N1 Cd1 Cl1 84.17(8) . . ? N3 Cd1 Cl1 88.09(7) 2_554 . ? N3 Cd1 Cl1 88.09(7) 7_665 . ? N6 Cd2 N2 91.02(10) 6_656 . ? N6 Cd2 N2 91.02(10) 6_656 8_565 ? N2 Cd2 N2 95.94(14) . 8_565 ? N6 Cd2 N4 100.07(10) 6_656 5_655 ? N2 Cd2 N4 87.19(10) . 5_655 ? N2 Cd2 N4 168.44(10) 8_565 5_655 ? N6 Cd2 N4 100.07(10) 6_656 4_655 ? N2 Cd2 N4 168.44(10) . 4_655 ? N2 Cd2 N4 87.19(10) 8_565 4_655 ? N4 Cd2 N4 87.65(15) 5_655 4_655 ? N6 Cd2 Cl1 178.47(11) 6_656 . ? N2 Cd2 Cl1 87.96(7) . . ? N2 Cd2 Cl1 87.96(7) 8_565 . ? N4 Cd2 Cl1 81.02(7) 5_655 . ? N4 Cd2 Cl1 81.02(7) 4_655 . ? Cd2 Cl1 Cd1 91.83(5) . . ? N2 C1 N3 113.4(3) . . ? N2 C1 N4 123.3(3) . . ? N3 C1 N4 123.2(3) . . ? N1 C2 N3 113.4(3) . . ? N1 C2 H2 123.3 . . ? N3 C2 H2 123.3 . . ? N5 C3 N7 106.6(4) . . ? N5 C3 H3 126.7 . . ? N7 C3 H3 126.7 . . ? N7 C4 N6 111.6(4) . . ? N7 C4 N8 124.1(5) . . ? N6 C4 N8 124.3(5) . . ? C2 N1 N2 105.8(3) . . ? C2 N1 Cd1 125.8(2) . . ? N2 N1 Cd1 128.4(2) . . ? C1 N2 N1 105.3(3) . . ? C1 N2 Cd2 138.2(2) . . ? N1 N2 Cd2 115.69(19) . . ? C1 N3 C2 102.1(3) . . ? C1 N3 Cd1 141.2(2) . 2 ? C2 N3 Cd1 116.6(2) . 2 ? C1 N4 Cd2 124.0(2) . 5_655 ? C1 N4 HN41 110(3) . . ? Cd2 N4 HN41 95(3) 5_655 . ? C1 N4 HN42 104(3) . . ? Cd2 N4 HN42 106(3) 5_655 . ? HN41 N4 HN42 118(4) . . ? C3 N5 N6 112.9(5) . . ? C4 N6 N5 102.5(4) . . ? C4 N6 Cd2 141.4(3) . 6_556 ? N5 N6 Cd2 116.1(3) . 6_556 ? C4 N7 C3 106.4(4) . . ? C4 N7 Cd1 136.6(3) . . ? C3 N7 Cd1 117.0(3) . . ? C4 N8 HN81 118(4) . . ? C4 N8 HN82 131(5) . . ? HN81 N8 HN82 111(6) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 HN41 N2 0.87(5) 2.89(4) 3.324(4) 113(3) 5_655 N4 HN42 Cl1 0.81(5) 3.16(4) 3.319(3) 94(3) 5_655 N8 HN82 N3 0.82(7) 2.61(5) 3.280(5) 139.3(12) 7_666 N8 HN82 N3 0.82(7) 2.61(5) 3.280(5) 139.3(12) 2 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.014 _refine_diff_density_min -1.082 _refine_diff_density_rms 0.138 #===end