data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Jiwen Cai' _publ_contact_author_address ; School of Chemistry and Chemical Engineering Sun Yat-Sen University Guangzhou 510275 CHINA ; _publ_contact_author_email PUSCJW@ZSU.EDU.CN _publ_section_title ; Reversible and Selective Amine Interactions of [Cd(µ2-p-N,O-NH2C6H4SO3)2(H2O)2]n ; loop_ _publ_author_name 'Jiwen Cai' 'Seik Weng Ng' 'Li Wang' 'Jin-Sen Zhou' data_compound_1 _database_code_depnum_ccdc_archive 'CCDC 222142' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Cd(mu2-NH2C6H4SO3)2(H2O)2)n _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H16 Cd N2 O8 S2' _chemical_formula_weight 492.79 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' S S 0.1246 0.1234 '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.210(4) _cell_length_b 5.962(3) _cell_length_c 18.975(10) _cell_angle_alpha 90.00 _cell_angle_beta 99.336(9) _cell_angle_gamma 90.00 _cell_volume 804.9(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.033 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 492 _exptl_absorpt_coefficient_mu 1.663 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4903 _exptl_absorpt_correction_T_max 0.6532 _exptl_absorpt_process_details sadabs _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 Smart 1000 CCD' _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 4696 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0379 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 27.03 _reflns_number_total 1732 _reflns_number_gt 1626 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Saint+' _computing_cell_refinement 'Bruker Saint+' _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^)+(0.0298P)^2^+0.5091P] 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 0.332(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1732 _refine_ls_number_parameters 118 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0295 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0752 _refine_ls_wR_factor_gt 0.0735 _refine_ls_goodness_of_fit_ref 1.195 _refine_ls_restrained_S_all 1.195 _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 Cd1 Cd 0.0000 0.0000 0.0000 0.02375(18) Uani 1 2 d S . . S1 S 0.38751(8) 0.22852(12) 0.10875(3) 0.0285(2) Uani 1 1 d . . . O1 O 0.1970(3) 0.1414(4) 0.09692(10) 0.0442(6) Uani 1 1 d . . . O2 O 0.3990(5) 0.4559(5) 0.08275(15) 0.0579(7) Uani 1 1 d . . . O3 O 0.5179(3) 0.0813(5) 0.08163(11) 0.0473(6) Uani 1 1 d . . . N1 N -0.1520(3) -0.2236(4) 0.07697(10) 0.0267(4) Uani 1 1 d . . . H1A H -0.2721 -0.1767 0.0721 0.032 Uiso 1 1 calc R . . H1B H -0.1548 -0.3649 0.0602 0.032 Uiso 1 1 calc R . . C1 C -0.0819(3) -0.2342(4) 0.15226(12) 0.0229(5) Uani 1 1 d . . . C2 C -0.1097(4) -0.0546(5) 0.19557(15) 0.0281(5) Uani 1 1 d . . . H2A H -0.1703 0.0736 0.1756 0.034 Uiso 1 1 calc R . . C3 C -0.0475(4) -0.0649(5) 0.26840(14) 0.0277(5) Uani 1 1 d . . . H3A H -0.0678 0.0552 0.2975 0.033 Uiso 1 1 calc R . . C4 C 0.0449(3) -0.2545(4) 0.29774(12) 0.0230(5) Uani 1 1 d . . . C5 C 0.0778(4) -0.4329(5) 0.25469(14) 0.0280(5) Uani 1 1 d . . . H5A H 0.1420 -0.5590 0.2746 0.034 Uiso 1 1 calc R . . C6 C 0.0145(4) -0.4223(5) 0.18177(13) 0.0278(5) Uani 1 1 d . . . H6A H 0.0366 -0.5413 0.1526 0.033 Uiso 1 1 calc R . . OW1 O -0.2058(3) 0.2838(3) 0.01606(10) 0.0330(4) Uani 1 1 d . . . HW1 H -0.2616 0.3327 -0.0251 0.059(12) Uiso 1 1 d R . . HW2 H -0.2893 0.2450 0.0381 0.050(10) 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 Cd1 0.0240(2) 0.0318(2) 0.0150(2) -0.00156(8) 0.00175(11) 0.00190(8) S1 0.0253(3) 0.0455(4) 0.0137(3) -0.0008(2) 0.0005(2) 0.0040(3) O1 0.0267(9) 0.0810(17) 0.0236(10) -0.0169(10) -0.0001(7) -0.0047(10) O2 0.085(2) 0.0551(14) 0.0287(13) 0.0155(11) -0.0050(13) 0.0030(14) O3 0.0375(11) 0.0788(16) 0.0264(11) -0.0108(12) 0.0074(9) 0.0159(12) N1 0.0293(10) 0.0338(11) 0.0162(10) -0.0004(8) 0.0013(8) -0.0002(8) C1 0.0240(10) 0.0299(12) 0.0149(10) 0.0011(9) 0.0034(8) -0.0004(9) C2 0.0304(13) 0.0296(11) 0.0236(13) 0.0017(11) 0.0018(10) 0.0075(11) C3 0.0314(13) 0.0292(12) 0.0223(12) -0.0037(11) 0.0044(10) 0.0052(11) C4 0.0222(10) 0.0328(12) 0.0138(10) 0.0017(9) 0.0024(8) -0.0008(9) C5 0.0304(12) 0.0280(12) 0.0255(13) 0.0031(11) 0.0040(10) 0.0057(11) C6 0.0345(13) 0.0285(13) 0.0206(12) -0.0024(10) 0.0056(10) 0.0046(11) OW1 0.0303(9) 0.0383(11) 0.0304(10) 0.0008(8) 0.0047(8) 0.0067(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 Cd1 O1 2.294(2) . ? Cd1 O1 2.294(2) 3 ? Cd1 OW1 2.303(2) 3 ? Cd1 OW1 2.303(2) . ? Cd1 N1 2.373(2) 3 ? Cd1 N1 2.373(2) . ? S1 O3 1.441(2) . ? S1 O2 1.450(3) . ? S1 O1 1.451(2) . ? S1 C4 1.765(3) 2 ? N1 C1 1.438(3) . ? C1 C2 1.384(4) . ? C1 C6 1.388(4) . ? C2 C3 1.383(4) . ? C3 C4 1.383(4) . ? C4 C5 1.385(4) . ? C4 S1 1.765(3) 2_545 ? C5 C6 1.386(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 O1 Cd1 O1 180.00(7) . 3 ? O1 Cd1 OW1 92.73(8) . 3 ? O1 Cd1 OW1 87.27(8) 3 3 ? O1 Cd1 OW1 87.27(8) . . ? O1 Cd1 OW1 92.73(8) 3 . ? OW1 Cd1 OW1 180.00(9) 3 . ? O1 Cd1 N1 89.95(8) . 3 ? O1 Cd1 N1 90.05(8) 3 3 ? OW1 Cd1 N1 87.68(8) 3 3 ? OW1 Cd1 N1 92.32(8) . 3 ? O1 Cd1 N1 90.05(8) . . ? O1 Cd1 N1 89.95(8) 3 . ? OW1 Cd1 N1 92.32(8) 3 . ? OW1 Cd1 N1 87.68(8) . . ? N1 Cd1 N1 180.00(13) 3 . ? O3 S1 O2 111.81(19) . . ? O3 S1 O1 112.49(15) . . ? O2 S1 O1 112.77(18) . . ? O3 S1 C4 107.72(12) . 2 ? O2 S1 C4 105.47(15) . 2 ? O1 S1 C4 106.02(11) . 2 ? S1 O1 Cd1 134.66(11) . . ? C1 N1 Cd1 120.88(15) . . ? C2 C1 C6 119.8(2) . . ? C2 C1 N1 119.6(2) . . ? C6 C1 N1 120.6(2) . . ? C3 C2 C1 120.3(3) . . ? C4 C3 C2 119.7(2) . . ? C3 C4 C5 120.5(2) . . ? C3 C4 S1 119.21(19) . 2_545 ? C5 C4 S1 120.21(19) . 2_545 ? C4 C5 C6 119.6(2) . . ? C5 C6 C1 120.1(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 S1 O1 Cd1 -49.8(3) . . . . ? O2 S1 O1 Cd1 77.8(2) . . . . ? C4 S1 O1 Cd1 -167.31(18) 2 . . . ? O1 Cd1 O1 S1 9(42) 3 . . . ? OW1 Cd1 O1 S1 59.2(2) 3 . . . ? OW1 Cd1 O1 S1 -120.8(2) . . . . ? N1 Cd1 O1 S1 -28.5(2) 3 . . . ? N1 Cd1 O1 S1 151.5(2) . . . . ? O1 Cd1 N1 C1 -6.22(18) . . . . ? O1 Cd1 N1 C1 173.78(18) 3 . . . ? OW1 Cd1 N1 C1 86.51(18) 3 . . . ? OW1 Cd1 N1 C1 -93.49(18) . . . . ? N1 Cd1 N1 C1 -88(100) 3 . . . ? Cd1 N1 C1 C2 74.7(3) . . . . ? Cd1 N1 C1 C6 -104.9(2) . . . . ? C6 C1 C2 C3 -2.2(4) . . . . ? N1 C1 C2 C3 178.2(2) . . . . ? C1 C2 C3 C4 0.9(4) . . . . ? C2 C3 C4 C5 0.8(4) . . . . ? C2 C3 C4 S1 -176.7(2) . . . 2_545 ? C3 C4 C5 C6 -1.1(4) . . . . ? S1 C4 C5 C6 176.4(2) 2_545 . . . ? C4 C5 C6 C1 -0.2(4) . . . . ? C2 C1 C6 C5 1.9(4) . . . . ? N1 C1 C6 C5 -178.5(2) . . . . ? 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 N1 H1A O3 0.90 2.19 3.008(3) 151.3 1_455 N1 H1B OW1 0.90 2.26 3.157(3) 172.0 1_545 OW1 HW1 O2 0.87 1.85 2.649(3) 152.5 3_565 OW1 HW2 O3 0.82 1.98 2.789(3) 166.5 1_455 _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.03 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.258 _refine_diff_density_min -0.892 _refine_diff_density_rms 0.132 #==============================================end data_compound_4 _database_code_depnum_ccdc_archive 'CCDC 222143' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Cd(NH2C6H4SO3)2(C3H7NH2)4)(C3H7NH2) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H57 Cd N7 O6 S2' _chemical_formula_weight 752.32 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' S S 0.1246 0.1234 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.9686(9) _cell_length_b 15.4694(19) _cell_length_c 15.7489(19) _cell_angle_alpha 88.932(2) _cell_angle_beta 88.548(2) _cell_angle_gamma 78.565(2) _cell_volume 1902.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colour _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 0.728 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7449 _exptl_absorpt_correction_T_max 0.9177 _exptl_absorpt_process_details sadabs _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 Smart 1000 CCD' _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 14060 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0429 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6686 _reflns_number_gt 4441 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Saint+' _computing_cell_refinement 'Bruker Saint+' _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. The included amine molecules are located on the inversion centers and therefore disordered. They were refined isotropically and the hydrogen atoms were not located. ; _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^)+(0.0693P)^2^+1.3615P] 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 6686 _refine_ls_number_parameters 371 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0799 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1383 _refine_ls_wR_factor_gt 0.1178 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.068 _refine_ls_shift/su_mean 0.007 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 0.5000 0.5000 0.05497(17) Uani 1 2 d S . . Cd2 Cd 0.5000 0.0000 0.0000 0.05740(18) Uani 1 2 d S . . S1 S 0.89649(16) 0.38598(9) 0.41199(9) 0.0607(3) Uani 1 1 d . . . S2 S 0.11563(17) 0.09987(10) -0.10563(8) 0.0640(4) Uani 1 1 d . . . O1 O 0.7362(4) 0.4475(2) 0.3969(2) 0.0647(9) Uani 1 1 d . . . O2 O 0.8842(6) 0.3333(3) 0.4881(2) 0.0874(12) Uani 1 1 d . . . O3 O 1.0374(5) 0.4310(3) 0.4104(3) 0.0999(15) Uani 1 1 d . . . O4 O 0.2465(4) 0.1065(2) -0.0457(2) 0.0667(9) Uani 1 1 d . . . O5 O -0.0523(5) 0.1204(4) -0.0672(3) 0.1131(18) Uani 1 1 d . . . O6 O 0.1513(7) 0.0154(3) -0.1484(3) 0.0989(14) Uani 1 1 d . . . N1 N 1.0326(7) 0.1313(4) 0.1302(3) 0.0943(17) Uani 1 1 d . . . H1A H 1.0181 0.0782 0.1385 0.113 Uiso 1 1 calc R . . H1B H 1.0705 0.1466 0.0817 0.113 Uiso 1 1 calc R . . N2 N 0.5378(7) 0.6444(3) 0.4988(3) 0.0877(15) Uani 1 1 d . . . H2B H 0.6313 0.6460 0.4661 0.105 Uiso 1 1 calc R . . H2C H 0.4481 0.6765 0.4715 0.105 Uiso 1 1 calc R . . N3 N 0.6721(7) 0.4674(4) 0.6173(3) 0.0970(17) Uani 1 1 d . . . H3B H 0.7680 0.4301 0.6003 0.116 Uiso 1 1 calc R . . H3C H 0.7037 0.5177 0.6323 0.116 Uiso 1 1 calc R . . N4 N 0.1356(7) 0.3691(3) -0.3764(3) 0.0873(15) Uani 1 1 d . . . H4A H 0.1134 0.3577 -0.4277 0.105 Uiso 1 1 calc R . . H4B H 0.1615 0.4190 -0.3650 0.105 Uiso 1 1 calc R . . N5 N 0.3861(10) -0.0027(4) 0.1349(4) 0.144(3) Uani 1 1 d . . . H5B H 0.4180 0.0419 0.1621 0.172 Uiso 1 1 calc R . . H5C H 0.2719 0.0129 0.1293 0.172 Uiso 1 1 calc R . . N6 N 0.3915(8) -0.1243(5) -0.0309(4) 0.118(2) Uani 1 1 d . . . H6B H 0.3619 -0.1462 0.0194 0.142 Uiso 1 1 calc R . . H6C H 0.2933 -0.1046 -0.0583 0.142 Uiso 1 1 calc R . . C1 C 0.9318(6) 0.3110(3) 0.3274(3) 0.0521(11) Uani 1 1 d . . . C2 C 0.9033(6) 0.2266(3) 0.3380(3) 0.0617(13) Uani 1 1 d . . . H2A H 0.8626 0.2090 0.3900 0.074 Uiso 1 1 calc R . . C3 C 0.9342(7) 0.1685(3) 0.2725(3) 0.0661(14) Uani 1 1 d . . . H3A H 0.9138 0.1117 0.2806 0.079 Uiso 1 1 calc R . . C4 C 0.9948(7) 0.1923(4) 0.1949(3) 0.0642(14) Uani 1 1 d . . . C5 C 1.0232(8) 0.2769(4) 0.1850(4) 0.0752(16) Uani 1 1 d . . . H5A H 1.0649 0.2943 0.1331 0.090 Uiso 1 1 calc R . . C6 C 0.9915(7) 0.3355(4) 0.2498(4) 0.0692(15) Uani 1 1 d . . . H6A H 1.0105 0.3925 0.2414 0.083 Uiso 1 1 calc R . . C7 C 0.5561(8) 0.6905(3) 0.5744(4) 0.0766(16) Uani 1 1 d D . . H7A H 0.6557 0.6585 0.6036 0.092 Uiso 1 1 calc R . . H7B H 0.4570 0.6890 0.6110 0.092 Uiso 1 1 calc R . . C8 C 0.5746(11) 0.7843(4) 0.5640(5) 0.111(2) Uani 1 1 d D . . H8A H 0.4773 0.8167 0.5334 0.133 Uiso 1 1 calc R . . H8B H 0.6770 0.7864 0.5299 0.133 Uiso 1 1 calc R . . C9 C 0.5859(13) 0.8285(5) 0.6467(6) 0.142(3) Uani 1 1 d D . . H9A H 0.5960 0.8886 0.6362 0.214 Uiso 1 1 calc R . . H9B H 0.6845 0.7981 0.6764 0.214 Uiso 1 1 calc R . . H9C H 0.4845 0.8272 0.6805 0.214 Uiso 1 1 calc R . . C10 C 0.6081(12) 0.4299(8) 0.6930(5) 0.173(5) Uani 1 1 d D . . H10A H 0.5020 0.4696 0.7085 0.207 Uiso 1 1 calc R . . H10B H 0.5765 0.3756 0.6756 0.207 Uiso 1 1 calc R . . C11 C 0.6972(13) 0.4094(8) 0.7688(6) 0.176(4) Uani 1 1 d D . . H11A H 0.7083 0.4647 0.7938 0.211 Uiso 1 1 calc R . . H11B H 0.8119 0.3787 0.7535 0.211 Uiso 1 1 calc R . . C12 C 0.6329(17) 0.3574(10) 0.8353(7) 0.222(6) Uani 1 1 d D . . H12A H 0.7071 0.3516 0.8830 0.333 Uiso 1 1 calc R . . H12B H 0.6296 0.3000 0.8142 0.333 Uiso 1 1 calc R . . H12C H 0.5196 0.3863 0.8526 0.333 Uiso 1 1 calc R . . C13 C 0.1248(6) 0.1801(3) -0.1856(3) 0.0520(11) Uani 1 1 d . . . C14 C 0.1662(7) 0.2601(4) -0.1675(3) 0.0655(14) Uani 1 1 d . . . H14 H 0.1931 0.2717 -0.1123 0.079 Uiso 1 1 calc R . . C15 C 0.1681(7) 0.3225(4) -0.2302(4) 0.0692(14) Uani 1 1 d . . . H15 H 0.1959 0.3761 -0.2165 0.083 Uiso 1 1 calc R . . C16 C 0.1298(6) 0.3080(3) -0.3129(3) 0.0608(13) Uani 1 1 d . . . C17 C 0.0886(7) 0.2279(4) -0.3301(3) 0.0689(14) Uani 1 1 d . . . H17 H 0.0620 0.2161 -0.3853 0.083 Uiso 1 1 calc R . . C18 C 0.0861(6) 0.1650(4) -0.2675(3) 0.0612(13) Uani 1 1 d . . . H18 H 0.0576 0.1115 -0.2810 0.073 Uiso 1 1 calc R . . C19 C 0.4108(9) -0.0710(5) 0.1898(4) 0.111(2) Uani 1 1 d D . . H19A H 0.5335 -0.0930 0.1893 0.133 Uiso 1 1 calc R . . H19B H 0.3616 -0.1161 0.1634 0.133 Uiso 1 1 calc R . . C20 C 0.3580(13) -0.0720(6) 0.2776(4) 0.144(3) Uani 1 1 d D . . H20A H 0.2346 -0.0526 0.2804 0.173 Uiso 1 1 calc R . . H20B H 0.4067 -0.0282 0.3063 0.173 Uiso 1 1 calc R . . C21 C 0.3998(14) -0.1538(7) 0.3263(6) 0.183(5) Uani 1 1 d D . . H21A H 0.3621 -0.1434 0.3843 0.274 Uiso 1 1 calc R . . H21B H 0.5215 -0.1751 0.3242 0.274 Uiso 1 1 calc R . . H21C H 0.3436 -0.1969 0.3027 0.274 Uiso 1 1 calc R . . C22 C 0.4775(12) -0.1944(6) -0.0756(8) 0.166(5) Uani 1 1 d D . . H22A H 0.5913 -0.2093 -0.0524 0.199 Uiso 1 1 calc R . . H22B H 0.4913 -0.1731 -0.1332 0.199 Uiso 1 1 calc R . . C23 C 0.4186(14) -0.2764(7) -0.0827(8) 0.177(5) Uani 1 1 d D . . H23A H 0.2964 -0.2628 -0.0923 0.213 Uiso 1 1 calc R . . H23B H 0.4360 -0.3080 -0.0289 0.213 Uiso 1 1 calc R . . C24 C 0.5014(19) -0.3349(8) -0.1501(10) 0.246(8) Uani 1 1 d D . . H24A H 0.4569 -0.3882 -0.1485 0.368 Uiso 1 1 calc R . . H24B H 0.6227 -0.3489 -0.1416 0.368 Uiso 1 1 calc R . . H24C H 0.4789 -0.3060 -0.2042 0.368 Uiso 1 1 calc R . . C91 C 0.215(2) 0.0069(10) -0.4641(10) 0.250(6) Uiso 0.50 1 d P A 1 N91 N 0.215(2) 0.0069(10) -0.4641(10) 0.250(6) Uiso 0.50 1 d P A 2 C92 C 0.046(3) 0.0243(14) -0.4896(15) 0.263(9) Uiso 1 1 d . . . C93 C 0.194(3) -0.4984(14) -0.0407(15) 0.346(11) Uiso 0.50 1 d P . 1 N93 N 0.194(3) -0.4984(14) -0.0407(15) 0.346(11) Uiso 0.50 1 d P . 2 C94 C 0.043(6) -0.487(3) 0.016(3) 0.405(17) 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 0.0556(3) 0.0521(3) 0.0581(3) -0.0033(2) -0.0008(2) -0.0125(2) Cd2 0.0560(3) 0.0637(4) 0.0520(3) 0.0007(2) 0.0014(2) -0.0111(3) S1 0.0512(7) 0.0610(8) 0.0673(8) -0.0143(6) -0.0026(6) -0.0036(6) S2 0.0551(8) 0.0845(10) 0.0546(7) 0.0111(7) -0.0079(6) -0.0199(7) O1 0.056(2) 0.065(2) 0.068(2) -0.0032(17) 0.0077(16) 0.0000(17) O2 0.113(3) 0.082(3) 0.057(2) -0.007(2) -0.015(2) 0.009(2) O3 0.063(2) 0.099(3) 0.142(4) -0.060(3) 0.009(2) -0.023(2) O4 0.059(2) 0.076(2) 0.063(2) 0.0081(18) -0.0133(17) -0.0065(18) O5 0.057(2) 0.184(5) 0.094(3) 0.053(3) 0.003(2) -0.020(3) O6 0.157(4) 0.073(3) 0.077(3) 0.007(2) -0.026(3) -0.047(3) N1 0.122(4) 0.100(4) 0.068(3) -0.033(3) 0.031(3) -0.039(3) N2 0.127(4) 0.065(3) 0.080(3) -0.006(3) 0.009(3) -0.040(3) N3 0.105(4) 0.099(4) 0.092(4) 0.014(3) -0.032(3) -0.031(3) N4 0.108(4) 0.075(3) 0.083(3) 0.021(3) -0.017(3) -0.026(3) N5 0.208(7) 0.087(4) 0.103(4) 0.033(4) 0.081(5) 0.036(4) N6 0.104(5) 0.136(6) 0.131(5) -0.042(4) 0.016(4) -0.061(4) C1 0.043(3) 0.053(3) 0.060(3) -0.005(2) 0.001(2) -0.009(2) C2 0.066(3) 0.058(3) 0.060(3) -0.003(2) 0.013(2) -0.012(3) C3 0.073(3) 0.052(3) 0.076(4) -0.010(3) 0.012(3) -0.018(3) C4 0.059(3) 0.076(4) 0.059(3) -0.013(3) 0.007(2) -0.019(3) C5 0.090(4) 0.080(4) 0.059(3) 0.001(3) 0.014(3) -0.030(3) C6 0.077(4) 0.062(3) 0.070(4) 0.000(3) 0.009(3) -0.022(3) C7 0.068(4) 0.067(4) 0.096(4) -0.018(3) 0.001(3) -0.016(3) C8 0.147(7) 0.074(5) 0.118(6) -0.020(4) -0.006(5) -0.036(5) C9 0.155(8) 0.100(6) 0.180(9) -0.046(6) -0.032(7) -0.035(6) C10 0.124(7) 0.300(15) 0.074(5) 0.001(7) -0.027(5) 0.009(8) C11 0.157(10) 0.200(12) 0.151(9) 0.025(8) 0.014(8) 0.009(8) C12 0.223(13) 0.343(19) 0.127(9) 0.076(10) -0.015(9) -0.126(13) C13 0.043(2) 0.059(3) 0.053(3) 0.002(2) -0.003(2) -0.007(2) C14 0.065(3) 0.076(4) 0.055(3) -0.009(3) -0.011(2) -0.010(3) C15 0.078(4) 0.056(3) 0.076(4) -0.009(3) -0.014(3) -0.017(3) C16 0.049(3) 0.065(3) 0.066(3) 0.004(3) -0.005(2) -0.005(2) C17 0.078(4) 0.079(4) 0.055(3) 0.000(3) -0.016(3) -0.025(3) C18 0.068(3) 0.070(3) 0.053(3) -0.001(3) -0.007(2) -0.030(3) C19 0.088(5) 0.151(7) 0.080(4) 0.020(5) 0.013(4) 0.003(5) C20 0.198(10) 0.137(8) 0.092(6) 0.011(5) 0.042(6) -0.027(7) C21 0.184(10) 0.201(11) 0.125(8) 0.067(8) 0.025(7) 0.040(8) C22 0.126(8) 0.093(6) 0.286(14) -0.055(8) 0.005(8) -0.035(6) C23 0.160(10) 0.153(10) 0.219(13) -0.063(9) -0.009(9) -0.024(8) C24 0.255(17) 0.179(13) 0.31(2) -0.079(13) 0.072(15) -0.060(12) _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 N2 2.312(4) . ? Cd1 N2 2.312(4) 2_666 ? Cd1 N3 2.317(5) 2_666 ? Cd1 N3 2.317(5) . ? Cd1 O1 2.475(3) . ? Cd1 O1 2.475(3) 2_666 ? Cd2 N5 2.292(5) 2_655 ? Cd2 N5 2.292(5) . ? Cd2 N6 2.322(6) 2_655 ? Cd2 N6 2.322(6) . ? Cd2 O4 2.453(3) . ? Cd2 O4 2.453(3) 2_655 ? S1 O3 1.433(4) . ? S1 O2 1.449(4) . ? S1 O1 1.455(3) . ? S1 C1 1.762(5) . ? S2 O5 1.434(4) . ? S2 O4 1.444(3) . ? S2 O6 1.456(4) . ? S2 C13 1.761(5) . ? N1 C4 1.388(7) . ? N2 C7 1.423(7) . ? N3 C10 1.443(10) . ? N4 C16 1.369(6) . ? N5 C19 1.340(8) . ? N6 C22 1.361(10) . ? C1 C6 1.374(7) . ? C1 C2 1.376(7) . ? C2 C3 1.366(7) . ? C3 C4 1.374(7) . ? C4 C5 1.376(8) . ? C5 C6 1.364(7) . ? C7 C8 1.494(6) . ? C8 C9 1.496(7) . ? C10 C11 1.403(8) . ? C11 C12 1.452(8) . ? C13 C18 1.369(6) . ? C13 C14 1.379(7) . ? C14 C15 1.371(7) . ? C15 C16 1.378(7) . ? C16 C17 1.376(7) . ? C17 C18 1.376(7) . ? C19 C20 1.435(7) . ? C20 C21 1.452(7) . ? C22 C23 1.444(8) . ? C23 C24 1.464(8) . ? C91 C92 1.39(2) . ? C92 C92 1.21(3) 2_554 ? C93 C94 1.46(5) . ? C93 C94 1.98(5) 2_545 ? C94 C94 1.01(8) 2_545 ? C94 C93 1.98(5) 2_545 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cd1 N2 180.000(1) . 2_666 ? N2 Cd1 N3 89.17(19) . 2_666 ? N2 Cd1 N3 90.83(19) 2_666 2_666 ? N2 Cd1 N3 90.83(19) . . ? N2 Cd1 N3 89.17(19) 2_666 . ? N3 Cd1 N3 180.000(1) 2_666 . ? N2 Cd1 O1 95.15(15) . . ? N2 Cd1 O1 84.85(15) 2_666 . ? N3 Cd1 O1 86.03(17) 2_666 . ? N3 Cd1 O1 93.97(18) . . ? N2 Cd1 O1 84.85(15) . 2_666 ? N2 Cd1 O1 95.15(15) 2_666 2_666 ? N3 Cd1 O1 93.97(18) 2_666 2_666 ? N3 Cd1 O1 86.03(18) . 2_666 ? O1 Cd1 O1 180.000(1) . 2_666 ? N5 Cd2 N5 180.0(3) 2_655 . ? N5 Cd2 N6 89.2(3) 2_655 2_655 ? N5 Cd2 N6 90.8(3) . 2_655 ? N5 Cd2 N6 90.8(3) 2_655 . ? N5 Cd2 N6 89.2(3) . . ? N6 Cd2 N6 180.00(15) 2_655 . ? N5 Cd2 O4 89.29(19) 2_655 . ? N5 Cd2 O4 90.71(19) . . ? N6 Cd2 O4 84.6(2) 2_655 . ? N6 Cd2 O4 95.4(2) . . ? N5 Cd2 O4 90.71(19) 2_655 2_655 ? N5 Cd2 O4 89.29(19) . 2_655 ? N6 Cd2 O4 95.4(2) 2_655 2_655 ? N6 Cd2 O4 84.6(2) . 2_655 ? O4 Cd2 O4 180.0(2) . 2_655 ? O3 S1 O2 114.2(3) . . ? O3 S1 O1 110.8(2) . . ? O2 S1 O1 111.1(2) . . ? O3 S1 C1 106.8(2) . . ? O2 S1 C1 105.8(2) . . ? O1 S1 C1 107.7(2) . . ? O5 S2 O4 111.6(3) . . ? O5 S2 O6 113.4(3) . . ? O4 S2 O6 111.6(3) . . ? O5 S2 C13 107.0(2) . . ? O4 S2 C13 106.9(2) . . ? O6 S2 C13 105.8(2) . . ? S1 O1 Cd1 128.0(2) . . ? S2 O4 Cd2 131.7(2) . . ? C7 N2 Cd1 122.7(4) . . ? C10 N3 Cd1 120.1(5) . . ? C19 N5 Cd2 126.8(4) . . ? C22 N6 Cd2 124.8(5) . . ? C6 C1 C2 118.6(5) . . ? C6 C1 S1 120.4(4) . . ? C2 C1 S1 120.9(4) . . ? C3 C2 C1 120.5(5) . . ? C2 C3 C4 121.2(5) . . ? C3 C4 C5 117.9(5) . . ? C3 C4 N1 120.4(5) . . ? C5 C4 N1 121.6(5) . . ? C6 C5 C4 121.4(5) . . ? C5 C6 C1 120.5(5) . . ? N2 C7 C8 116.8(5) . . ? C7 C8 C9 113.1(6) . . ? C11 C10 N3 125.7(9) . . ? C10 C11 C12 120.7(10) . . ? C18 C13 C14 118.3(5) . . ? C18 C13 S2 120.3(4) . . ? C14 C13 S2 121.4(4) . . ? C15 C14 C13 120.5(5) . . ? C14 C15 C16 121.8(5) . . ? N4 C16 C17 120.7(5) . . ? N4 C16 C15 122.2(5) . . ? C17 C16 C15 117.1(5) . . ? C16 C17 C18 121.5(5) . . ? C13 C18 C17 120.9(5) . . ? N5 C19 C20 128.1(7) . . ? C19 C20 C21 119.2(7) . . ? N6 C22 C23 123.6(9) . . ? C22 C23 C24 115.6(10) . . ? C92 C92 C91 131(3) 2_554 . ? C94 C93 C94 30(3) . 2_545 ? C94 C94 C93 105(6) 2_545 . ? C94 C94 C93 45(5) 2_545 2_545 ? C93 C94 C93 150(3) . 2_545 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 S1 O1 Cd1 -108.5(3) . . . . ? O2 S1 O1 Cd1 19.7(3) . . . . ? C1 S1 O1 Cd1 135.1(3) . . . . ? N2 Cd1 O1 S1 113.2(3) . . . . ? N2 Cd1 O1 S1 -66.8(3) 2_666 . . . ? N3 Cd1 O1 S1 -158.0(3) 2_666 . . . ? N3 Cd1 O1 S1 22.0(3) . . . . ? O1 Cd1 O1 S1 -163(100) 2_666 . . . ? O5 S2 O4 Cd2 124.2(3) . . . . ? O6 S2 O4 Cd2 -3.9(4) . . . . ? C13 S2 O4 Cd2 -119.1(3) . . . . ? N5 Cd2 O4 S2 65.1(3) 2_655 . . . ? N5 Cd2 O4 S2 -114.9(3) . . . . ? N6 Cd2 O4 S2 154.4(3) 2_655 . . . ? N6 Cd2 O4 S2 -25.6(3) . . . . ? O4 Cd2 O4 S2 -67(75) 2_655 . . . ? N2 Cd1 N2 C7 31(100) 2_666 . . . ? N3 Cd1 N2 C7 146.2(5) 2_666 . . . ? N3 Cd1 N2 C7 -33.8(5) . . . . ? O1 Cd1 N2 C7 -127.8(5) . . . . ? O1 Cd1 N2 C7 52.2(5) 2_666 . . . ? N2 Cd1 N3 C10 124.9(7) . . . . ? N2 Cd1 N3 C10 -55.1(7) 2_666 . . . ? N3 Cd1 N3 C10 -24(100) 2_666 . . . ? O1 Cd1 N3 C10 -139.9(7) . . . . ? O1 Cd1 N3 C10 40.1(7) 2_666 . . . ? N5 Cd2 N5 C19 13(100) 2_655 . . . ? N6 Cd2 N5 C19 -126.4(8) 2_655 . . . ? N6 Cd2 N5 C19 53.6(8) . . . . ? O4 Cd2 N5 C19 148.9(8) . . . . ? O4 Cd2 N5 C19 -31.1(8) 2_655 . . . ? N5 Cd2 N6 C22 42.2(9) 2_655 . . . ? N5 Cd2 N6 C22 -137.8(9) . . . . ? N6 Cd2 N6 C22 -96(100) 2_655 . . . ? O4 Cd2 N6 C22 131.5(9) . . . . ? O4 Cd2 N6 C22 -48.5(9) 2_655 . . . ? O3 S1 C1 C6 -41.6(5) . . . . ? O2 S1 C1 C6 -163.7(4) . . . . ? O1 S1 C1 C6 77.4(5) . . . . ? O3 S1 C1 C2 137.3(4) . . . . ? O2 S1 C1 C2 15.2(5) . . . . ? O1 S1 C1 C2 -103.7(4) . . . . ? C6 C1 C2 C3 0.2(8) . . . . ? S1 C1 C2 C3 -178.8(4) . . . . ? C1 C2 C3 C4 0.2(8) . . . . ? C2 C3 C4 C5 -0.1(9) . . . . ? C2 C3 C4 N1 177.2(5) . . . . ? C3 C4 C5 C6 -0.4(9) . . . . ? N1 C4 C5 C6 -177.6(6) . . . . ? C4 C5 C6 C1 0.8(9) . . . . ? C2 C1 C6 C5 -0.6(8) . . . . ? S1 C1 C6 C5 178.3(5) . . . . ? Cd1 N2 C7 C8 -178.3(5) . . . . ? N2 C7 C8 C9 177.6(7) . . . . ? Cd1 N3 C10 C11 -178.2(9) . . . . ? N3 C10 C11 C12 -168.8(11) . . . . ? O5 S2 C13 C18 -92.9(5) . . . . ? O4 S2 C13 C18 147.4(4) . . . . ? O6 S2 C13 C18 28.4(5) . . . . ? O5 S2 C13 C14 85.4(5) . . . . ? O4 S2 C13 C14 -34.3(5) . . . . ? O6 S2 C13 C14 -153.3(4) . . . . ? C18 C13 C14 C15 0.1(7) . . . . ? S2 C13 C14 C15 -178.2(4) . . . . ? C13 C14 C15 C16 -0.3(8) . . . . ? C14 C15 C16 N4 -178.3(5) . . . . ? C14 C15 C16 C17 0.3(8) . . . . ? N4 C16 C17 C18 178.5(5) . . . . ? C15 C16 C17 C18 -0.1(8) . . . . ? C14 C13 C18 C17 0.1(7) . . . . ? S2 C13 C18 C17 178.4(4) . . . . ? C16 C17 C18 C13 -0.1(8) . . . . ? Cd2 N5 C19 C20 172.1(8) . . . . ? N5 C19 C20 C21 -179.3(10) . . . . ? Cd2 N6 C22 C23 170.0(9) . . . . ? N6 C22 C23 C24 164.7(13) . . . . ? C94 C93 C94 C93 0.000(16) 2_545 . . 2_545 ? 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 H4B O1 0.86 2.41 3.208(6) 155.3 2_665 N4 H4B O3 0.86 2.64 3.168(7) 121.2 2_665 N4 H4A O2 0.86 2.38 3.095(7) 141.2 1_454 N5 H5C N1 0.90 2.37 3.151(9) 145.5 1_455 N6 H6B O5 0.90 2.52 3.069(7) 120.1 2 N6 H6C O6 0.90 2.43 3.186(9) 142.1 . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.637 _refine_diff_density_min -0.406 _refine_diff_density_rms 0.070 #=============================================end data_compound_3 _database_code_depnum_ccdc_archive 'CCDC 222144' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Cd(C2H5NH2)4(H2O)2)(NH2C6H4SO3)2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H44 Cd N6 O8 S2' _chemical_formula_weight 673.13 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' S S 0.1246 0.1234 '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.680(3) _cell_length_b 7.863(2) _cell_length_c 18.906(6) _cell_angle_alpha 90.00 _cell_angle_beta 100.152(6) _cell_angle_gamma 90.00 _cell_volume 1562.8(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 700 _exptl_absorpt_coefficient_mu 0.880 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6824 _exptl_absorpt_correction_T_max 0.8436 _exptl_absorpt_process_details sadabs _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 Smart 1000 CCD' _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 10887 _diffrn_reflns_av_R_equivalents 0.0170 _diffrn_reflns_av_sigmaI/netI 0.0216 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 29.87 _reflns_number_total 4171 _reflns_number_gt 2995 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Saint+' _computing_cell_refinement 'Bruker Saint+' _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^)+(0.0439P)^2^+0.4578P] 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 4171 _refine_ls_number_parameters 177 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0473 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0882 _refine_ls_wR_factor_gt 0.0791 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 1.0000 0.5000 0.5000 0.04160(8) Uani 1 2 d S . . S1 S 0.77662(5) 0.01054(6) 0.39095(3) 0.03972(12) Uani 1 1 d . . . O1 O 0.85209(15) 0.1475(2) 0.36811(10) 0.0607(4) Uani 1 1 d . . . O2 O 0.79427(15) -0.1466(2) 0.35411(9) 0.0517(4) Uani 1 1 d . . . O3 O 0.79887(19) -0.0098(2) 0.46873(9) 0.0610(5) Uani 1 1 d . . . OW1 O 1.07981(17) 0.2607(2) 0.43656(10) 0.0473(4) Uani 1 1 d . . . N1 N 0.93431(19) 0.2898(2) 0.57394(10) 0.0502(4) Uani 1 1 d . . . H1C H 0.8685 0.2340 0.5477 0.060 Uiso 1 1 calc R . . H1D H 0.9984 0.2145 0.5846 0.060 Uiso 1 1 calc R . . N2 N 0.80047(19) 0.5047(2) 0.42597(11) 0.0474(4) Uani 1 1 d . . . H2D H 0.7959 0.5987 0.3985 0.057 Uiso 1 1 calc R . . H2E H 0.7954 0.4145 0.3963 0.057 Uiso 1 1 calc R . . N3 N 0.2446(2) 0.2438(4) 0.30478(13) 0.0801(8) Uani 1 1 d . . . H3A H 0.2202 0.2865 0.2627 0.096 Uiso 1 1 calc R . . H3B H 0.1925 0.2380 0.3346 0.096 Uiso 1 1 calc R . . C1 C 0.8956(4) 0.3407(4) 0.64197(19) 0.1017(12) Uani 1 1 d . . . H1A H 0.9603 0.4155 0.6677 0.122 Uiso 1 1 calc R . . H1B H 0.8172 0.4053 0.6309 0.122 Uiso 1 1 calc R . . C2 C 0.8762(5) 0.1999(7) 0.6892(2) 0.1384(19) Uani 1 1 d . . . H2A H 0.8455 0.2432 0.7304 0.208 Uiso 1 1 calc R . . H2B H 0.9553 0.1416 0.7044 0.208 Uiso 1 1 calc R . . H2C H 0.8149 0.1223 0.6637 0.208 Uiso 1 1 calc R . . C3 C 0.6890(2) 0.5023(3) 0.46148(14) 0.0575(6) Uani 1 1 d . . . H3C H 0.7040 0.5793 0.5022 0.069 Uiso 1 1 calc R . . H3D H 0.6795 0.3888 0.4799 0.069 Uiso 1 1 calc R . . C4 C 0.5661(3) 0.5522(4) 0.41319(16) 0.0686(7) Uani 1 1 d . . . H4A H 0.4979 0.5498 0.4402 0.103 Uiso 1 1 calc R . . H4B H 0.5482 0.4736 0.3738 0.103 Uiso 1 1 calc R . . H4C H 0.5741 0.6648 0.3949 0.103 Uiso 1 1 calc R . . C5 C 0.4516(2) 0.1933(3) 0.27710(12) 0.0533(6) Uani 1 1 d . . . H5A H 0.4247 0.2363 0.2311 0.064 Uiso 1 1 calc R . . C6 C 0.3667(2) 0.1850(3) 0.32431(12) 0.0511(5) Uani 1 1 d . . . C7 C 0.4091(2) 0.1173(4) 0.39196(13) 0.0629(7) Uani 1 1 d . . . H7A H 0.3532 0.1081 0.4243 0.075 Uiso 1 1 calc R . . C8 C 0.5335(2) 0.0635(4) 0.41199(12) 0.0563(6) Uani 1 1 d . . . H8A H 0.5604 0.0191 0.4577 0.068 Uiso 1 1 calc R . . C9 C 0.61753(19) 0.0746(3) 0.36527(10) 0.0391(4) Uani 1 1 d . . . C10 C 0.5754(2) 0.1391(3) 0.29696(11) 0.0501(5) Uani 1 1 d . . . H10A H 0.6311 0.1457 0.2644 0.060 Uiso 1 1 calc R . . HW1 H 1.114(2) 0.201(3) 0.4635(13) 0.052(8) Uiso 1 1 d . . . HW2 H 1.012(3) 0.205(4) 0.4162(16) 0.084(10) 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 0.03701(12) 0.03797(12) 0.04994(14) 0.00156(9) 0.00798(9) 0.00409(9) S1 0.0365(3) 0.0382(3) 0.0408(3) -0.0014(2) -0.0032(2) 0.0046(2) O1 0.0442(9) 0.0506(9) 0.0829(12) 0.0060(8) -0.0008(8) -0.0073(8) O2 0.0475(9) 0.0437(8) 0.0608(9) -0.0090(7) 0.0008(7) 0.0089(7) O3 0.0593(11) 0.0765(13) 0.0415(9) 0.0033(7) -0.0069(8) 0.0181(8) OW1 0.0415(9) 0.0426(8) 0.0558(10) -0.0011(8) 0.0030(8) 0.0022(7) N1 0.0481(11) 0.0472(10) 0.0558(11) 0.0066(8) 0.0102(9) 0.0065(9) N2 0.0445(10) 0.0425(10) 0.0538(11) -0.0013(8) 0.0044(8) 0.0017(8) N3 0.0515(13) 0.120(2) 0.0695(14) 0.0281(14) 0.0114(11) 0.0370(13) C1 0.143(3) 0.079(2) 0.101(2) 0.0223(19) 0.071(2) 0.036(2) C2 0.173(5) 0.146(4) 0.116(3) 0.029(3) 0.082(4) 0.007(3) C3 0.0460(13) 0.0700(17) 0.0552(14) 0.0022(11) 0.0055(11) -0.0026(11) C4 0.0467(14) 0.0824(17) 0.0747(18) 0.0066(15) 0.0056(13) 0.0025(14) C5 0.0500(13) 0.0669(15) 0.0397(11) 0.0063(10) -0.0012(10) 0.0164(11) C6 0.0422(12) 0.0586(13) 0.0506(12) 0.0075(10) 0.0031(10) 0.0135(10) C7 0.0456(13) 0.0895(19) 0.0567(14) 0.0222(13) 0.0172(11) 0.0166(13) C8 0.0490(13) 0.0768(15) 0.0421(12) 0.0204(11) 0.0055(10) 0.0138(12) C9 0.0379(10) 0.0387(10) 0.0383(10) 0.0002(8) 0.0003(8) 0.0073(9) C10 0.0482(12) 0.0657(15) 0.0365(10) 0.0058(9) 0.0081(9) 0.0143(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 Cd1 N2 2.334(2) 3_766 ? Cd1 N2 2.334(2) . ? Cd1 N1 2.3505(19) . ? Cd1 N1 2.3505(19) 3_766 ? Cd1 OW1 2.4629(17) . ? Cd1 OW1 2.4629(17) 3_766 ? S1 O2 1.4468(16) . ? S1 O1 1.4556(17) . ? S1 O3 1.4564(18) . ? S1 C9 1.757(2) . ? OW1 HW1 0.74(3) . ? OW1 HW2 0.88(3) . ? N1 C1 1.474(4) . ? N1 H1C 0.9000 . ? N1 H1D 0.9000 . ? N2 C3 1.467(3) . ? N2 H2D 0.9000 . ? N2 H2E 0.9000 . ? N3 C6 1.371(3) . ? N3 H3A 0.8600 . ? N3 H3B 0.8600 . ? C1 C2 1.459(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C4 1.513(4) . ? C3 H3C 0.9700 . ? C3 H3D 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C10 1.376(3) . ? C5 C6 1.382(3) . ? C5 H5A 0.9300 . ? C6 C7 1.386(3) . ? C7 C8 1.382(3) . ? C7 H7A 0.9300 . ? C8 C9 1.369(3) . ? C8 H8A 0.9300 . ? C9 C10 1.386(3) . ? C10 H10A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cd1 N2 180.0 3_766 . ? N2 Cd1 N1 88.21(7) 3_766 . ? N2 Cd1 N1 91.79(7) . . ? N2 Cd1 N1 91.79(7) 3_766 3_766 ? N2 Cd1 N1 88.21(7) . 3_766 ? N1 Cd1 N1 180.000(1) . 3_766 ? N2 Cd1 OW1 85.54(6) 3_766 . ? N2 Cd1 OW1 94.46(6) . . ? N1 Cd1 OW1 85.26(7) . . ? N1 Cd1 OW1 94.74(7) 3_766 . ? N2 Cd1 OW1 94.46(6) 3_766 3_766 ? N2 Cd1 OW1 85.54(6) . 3_766 ? N1 Cd1 OW1 94.74(7) . 3_766 ? N1 Cd1 OW1 85.26(7) 3_766 3_766 ? OW1 Cd1 OW1 180.00(7) . 3_766 ? O2 S1 O1 111.30(11) . . ? O2 S1 O3 112.36(9) . . ? O1 S1 O3 112.35(11) . . ? O2 S1 C9 108.27(9) . . ? O1 S1 C9 105.36(10) . . ? O3 S1 C9 106.76(11) . . ? Cd1 OW1 HW1 109(2) . . ? Cd1 OW1 HW2 105(2) . . ? HW1 OW1 HW2 105(3) . . ? C1 N1 Cd1 119.14(18) . . ? C1 N1 H1C 107.5 . . ? Cd1 N1 H1C 107.5 . . ? C1 N1 H1D 107.5 . . ? Cd1 N1 H1D 107.5 . . ? H1C N1 H1D 107.0 . . ? C3 N2 Cd1 117.02(15) . . ? C3 N2 H2D 108.0 . . ? Cd1 N2 H2D 108.0 . . ? C3 N2 H2E 108.0 . . ? Cd1 N2 H2E 108.0 . . ? H2D N2 H2E 107.3 . . ? C6 N3 H3A 120.0 . . ? C6 N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? C2 C1 N1 114.8(3) . . ? C2 C1 H1A 108.6 . . ? N1 C1 H1A 108.6 . . ? C2 C1 H1B 108.6 . . ? N1 C1 H1B 108.6 . . ? H1A C1 H1B 107.5 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N2 C3 C4 114.1(2) . . ? N2 C3 H3C 108.7 . . ? C4 C3 H3C 108.7 . . ? N2 C3 H3D 108.7 . . ? C4 C3 H3D 108.7 . . ? H3C C3 H3D 107.6 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C10 C5 C6 121.2(2) . . ? C10 C5 H5A 119.4 . . ? C6 C5 H5A 119.4 . . ? N3 C6 C5 120.8(2) . . ? N3 C6 C7 121.3(2) . . ? C5 C6 C7 118.0(2) . . ? C8 C7 C6 120.9(2) . . ? C8 C7 H7A 119.6 . . ? C6 C7 H7A 119.6 . . ? C9 C8 C7 120.8(2) . . ? C9 C8 H8A 119.6 . . ? C7 C8 H8A 119.6 . . ? C8 C9 C10 118.83(19) . . ? C8 C9 S1 121.05(16) . . ? C10 C9 S1 120.12(17) . . ? C5 C10 C9 120.4(2) . . ? C5 C10 H10A 119.8 . . ? C9 C10 H10A 119.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Cd1 N1 C1 81.0(2) 3_766 . . . ? N2 Cd1 N1 C1 -99.0(2) . . . . ? N1 Cd1 N1 C1 -42(100) 3_766 . . . ? OW1 Cd1 N1 C1 166.6(2) . . . . ? OW1 Cd1 N1 C1 -13.4(2) 3_766 . . . ? N2 Cd1 N2 C3 -105(100) 3_766 . . . ? N1 Cd1 N2 C3 43.39(16) . . . . ? N1 Cd1 N2 C3 -136.61(16) 3_766 . . . ? OW1 Cd1 N2 C3 128.77(15) . . . . ? OW1 Cd1 N2 C3 -51.23(15) 3_766 . . . ? Cd1 N1 C1 C2 -170.7(3) . . . . ? Cd1 N2 C3 C4 164.54(18) . . . . ? C10 C5 C6 N3 178.1(3) . . . . ? C10 C5 C6 C7 -1.2(4) . . . . ? N3 C6 C7 C8 -177.9(3) . . . . ? C5 C6 C7 C8 1.4(4) . . . . ? C6 C7 C8 C9 -0.4(5) . . . . ? C7 C8 C9 C10 -0.8(4) . . . . ? C7 C8 C9 S1 178.7(2) . . . . ? O2 S1 C9 C8 107.9(2) . . . . ? O1 S1 C9 C8 -132.9(2) . . . . ? O3 S1 C9 C8 -13.3(2) . . . . ? O2 S1 C9 C10 -72.6(2) . . . . ? O1 S1 C9 C10 46.5(2) . . . . ? O3 S1 C9 C10 166.17(18) . . . . ? C6 C5 C10 C9 0.0(4) . . . . ? C8 C9 C10 C5 1.0(4) . . . . ? S1 C9 C10 C5 -178.44(19) . . . . ? 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 N1 H1C O3 0.90 2.46 3.253(3) 146.8 . N1 H1D O2 0.90 2.37 3.183(3) 149.9 3_756 N2 H2D O2 0.90 2.17 3.056(3) 167.7 1_565 N2 H2E O1 0.90 2.27 3.099(3) 152.2 . N3 H3A O2 0.86 2.25 3.082(3) 163.0 2_655 N3 H3B OW1 0.86 2.45 3.297(3) 167.1 1_455 OW1 HW1 O3 0.74(3) 2.09(3) 2.821(2) 173(3) 3_756 OW1 HW2 O1 0.88(3) 1.84(3) 2.697(2) 164(3) . _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 29.87 _diffrn_measured_fraction_theta_full 0.927 _refine_diff_density_max 0.691 _refine_diff_density_min -0.290 _refine_diff_density_rms 0.057