#Supplementary Material (ESI) for Dalton Transactions #This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Cai, Jiwen' 'Chen, Cai-Hong' 'Chen, Xiao-Ming' 'Feng, Xiao-Long' _publ_contact_author_name 'Dr Jiwen Cai' _publ_contact_author_address ; Dr Jiwen Cai Instrumentation Analysis & Research Center Zhongshan University Guangzhou 510275 CHINA ; _publ_contact_author_email 'PUSCJW@ZSU.EDU.CN' data_compound1 _database_code_CSD 162417 _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(N,N'-dimethylethylenediamine)-cadmium(II) naphthalene-2,6-disulfonate ; _chemical_name_common Cd(N,N'-meen)2(2,6nds) _chemical_melting_point ? _chemical_formula_moiety 'Cd C8 H24 N4 2+, C10 H6 S2 O6 2-' _chemical_formula_sum 'C18 H30 Cd N4 O6 S2' _chemical_formula_weight 574.98 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 7.6548(12) _cell_length_b 11.9968(18) _cell_length_c 12.832(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.836(3) _cell_angle_gamma 90.00 _cell_volume 1144.2(3) _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 plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.669 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 588 _exptl_absorpt_coefficient_mu 1.179 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.6971 _exptl_absorpt_correction_T_max 0.9013 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8020 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_sigmaI/netI 0.0249 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.43 _diffrn_reflns_theta_max 29.99 _reflns_number_total 3256 _reflns_number_gt 2731 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0401P)^2^+0.0954P] 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 3256 _refine_ls_number_parameters 137 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0328 _refine_ls_R_factor_gt 0.0255 _refine_ls_wR_factor_ref 0.0740 _refine_ls_wR_factor_gt 0.0710 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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 0.5000 0.0000 0.03250(7) Uani 1 2 d S . . S1 S 0.45154(6) 0.55185(4) 0.16421(3) 0.02888(10) Uani 1 1 d . . . O1 O 0.49263(18) 0.44010(12) 0.13403(10) 0.0360(3) Uani 1 1 d . . . O2 O 0.5769(2) 0.63600(13) 0.14660(11) 0.0443(3) Uani 1 1 d . . . O3 O 0.26416(17) 0.58340(13) 0.11795(10) 0.0419(3) Uani 1 1 d . . . N1 N 0.1439(2) 0.32710(14) 0.02799(13) 0.0377(4) Uani 1 1 d . . . H1A H 0.2635 0.3391 0.0351 0.045 Uiso 1 1 calc R . . N2 N -0.1077(2) 0.43099(17) 0.14072(13) 0.0434(4) Uani 1 1 d . . . H2A H -0.2296 0.4384 0.1219 0.052 Uiso 1 1 calc R . . C1 C 0.5282(2) 0.34801(14) 0.53322(14) 0.0311(4) Uani 1 1 d . . . H1C H 0.5354 0.2806 0.4987 0.037 Uiso 1 1 calc R . . C2 C 0.5058(2) 0.44890(15) 0.47322(13) 0.0263(3) Uani 1 1 d . . . C3 C 0.4948(2) 0.45006(15) 0.36116(13) 0.0279(3) Uani 1 1 d . . . H3A H 0.5034 0.3837 0.3253 0.033 Uiso 1 1 calc R . . C4 C 0.4714(2) 0.54887(15) 0.30547(13) 0.0263(3) Uani 1 1 d . . . C5 C 0.4607(2) 0.65094(15) 0.35897(14) 0.0313(4) Uani 1 1 d . . . H5A H 0.4462 0.7174 0.3206 0.038 Uiso 1 1 calc R . . C6 C 0.1194(3) 0.28962(19) 0.13393(18) 0.0484(5) Uani 1 1 d . . . H6A H 0.2035 0.3288 0.1907 0.058 Uiso 1 1 calc R . . H6B H 0.1447 0.2105 0.1425 0.058 Uiso 1 1 calc R . . C7 C -0.0687(3) 0.3117(2) 0.14277(19) 0.0532(6) Uani 1 1 d . . . H7A H -0.1525 0.2755 0.0838 0.064 Uiso 1 1 calc R . . H7B H -0.0856 0.2800 0.2092 0.064 Uiso 1 1 calc R . . C8 C -0.0443(4) 0.4845(2) 0.2465(2) 0.0563(7) Uani 1 1 d . . . H8A H -0.0983 0.4485 0.2977 0.084 Uiso 1 1 calc R . . H8B H -0.0774 0.5619 0.2412 0.084 Uiso 1 1 calc R . . H8C H 0.0842 0.4781 0.2692 0.084 Uiso 1 1 calc R . . C9 C 0.0862(3) 0.2444(2) -0.05656(19) 0.0536(6) Uiso 1 1 d . . . H9A H 0.1534 0.1769 -0.0372 0.080 Uiso 1 1 calc R . . H9B H 0.1068 0.2725 -0.1226 0.080 Uiso 1 1 calc R . . H9C H -0.0397 0.2293 -0.0655 0.080 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03706(12) 0.03331(11) 0.02531(11) 0.00248(7) 0.00386(7) 0.00575(8) S1 0.0292(2) 0.0342(2) 0.02139(19) 0.00138(17) 0.00241(15) -0.00087(18) O1 0.0408(7) 0.0372(7) 0.0298(6) -0.0028(6) 0.0079(5) 0.0029(6) O2 0.0498(8) 0.0490(8) 0.0340(7) 0.0069(6) 0.0098(6) -0.0146(7) O3 0.0334(7) 0.0523(8) 0.0329(7) -0.0035(6) -0.0062(5) 0.0066(6) N1 0.0329(8) 0.0361(8) 0.0420(9) -0.0024(7) 0.0049(7) 0.0018(7) N2 0.0321(8) 0.0640(12) 0.0338(8) 0.0061(8) 0.0076(7) 0.0040(8) C1 0.0402(9) 0.0232(8) 0.0283(8) -0.0018(7) 0.0050(7) 0.0009(7) C2 0.0275(8) 0.0254(8) 0.0246(8) -0.0012(6) 0.0036(6) -0.0009(7) C3 0.0318(8) 0.0266(8) 0.0237(8) -0.0032(6) 0.0036(6) 0.0005(7) C4 0.0242(7) 0.0307(8) 0.0220(7) -0.0008(7) 0.0015(6) -0.0015(7) C5 0.0377(9) 0.0260(8) 0.0287(8) 0.0035(7) 0.0047(7) 0.0001(7) C6 0.0509(12) 0.0415(11) 0.0484(12) 0.0113(10) 0.0030(10) 0.0022(10) C7 0.0521(13) 0.0612(14) 0.0461(12) 0.0091(11) 0.0112(10) -0.0141(12) C8 0.0598(15) 0.0762(18) 0.0350(12) 0.0015(10) 0.0155(11) 0.0098(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 2.3106(17) . ? Cd1 N2 2.3106(17) 3_565 ? Cd1 N1 2.3356(16) . ? Cd1 N1 2.3356(16) 3_565 ? Cd1 O3 2.4324(13) 3_565 ? Cd1 O3 2.4324(13) . ? S1 O2 1.4473(15) . ? S1 O1 1.4507(15) . ? S1 O3 1.4649(13) . ? S1 C4 1.7828(17) . ? N1 C9 1.459(3) . ? N1 C6 1.486(3) . ? N2 C7 1.460(3) . ? N2 C8 1.474(3) . ? C1 C5 1.366(2) 3_666 ? C1 C2 1.423(2) . ? C2 C2 1.419(3) 3_666 ? C2 C3 1.420(2) . ? C3 C4 1.373(3) . ? C4 C5 1.416(2) . ? C5 C1 1.366(2) 3_666 ? C6 C7 1.495(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cd1 N2 180.00(9) . 3_565 ? N2 Cd1 N1 78.75(6) . . ? N2 Cd1 N1 101.25(6) 3_565 . ? N2 Cd1 N1 101.25(6) . 3_565 ? N2 Cd1 N1 78.75(6) 3_565 3_565 ? N1 Cd1 N1 180.00(8) . 3_565 ? N2 Cd1 O3 86.56(6) . 3_565 ? N2 Cd1 O3 93.45(6) 3_565 3_565 ? N1 Cd1 O3 91.24(5) . 3_565 ? N1 Cd1 O3 88.76(5) 3_565 3_565 ? N2 Cd1 O3 93.44(6) . . ? N2 Cd1 O3 86.56(6) 3_565 . ? N1 Cd1 O3 88.76(5) . . ? N1 Cd1 O3 91.24(5) 3_565 . ? O3 Cd1 O3 180.00(8) 3_565 . ? O2 S1 O1 114.13(9) . . ? O2 S1 O3 112.21(9) . . ? O1 S1 O3 112.60(8) . . ? O2 S1 C4 105.92(8) . . ? O1 S1 C4 106.36(8) . . ? O3 S1 C4 104.73(8) . . ? S1 O3 Cd1 137.19(9) . . ? C9 N1 C6 113.13(17) . . ? C9 N1 Cd1 116.22(13) . . ? C6 N1 Cd1 104.58(12) . . ? C7 N2 C8 112.90(18) . . ? C7 N2 Cd1 104.80(14) . . ? C8 N2 Cd1 117.55(15) . . ? C5 C1 C2 120.71(16) 3_666 . ? C2 C2 C3 119.1(2) 3_666 . ? C2 C2 C1 119.11(19) 3_666 . ? C3 C2 C1 121.78(16) . . ? C4 C3 C2 120.27(16) . . ? C3 C4 C5 120.64(15) . . ? C3 C4 S1 121.00(14) . . ? C5 C4 S1 118.35(13) . . ? C1 C5 C4 120.15(16) 3_666 . ? N1 C6 C7 110.49(17) . . ? N2 C7 C6 111.65(19) . . ? 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 O2 S1 O3 Cd1 129.00(12) . . . . ? O1 S1 O3 Cd1 -1.41(15) . . . . ? C4 S1 O3 Cd1 -116.55(12) . . . . ? N2 Cd1 O3 S1 93.76(13) . . . . ? N2 Cd1 O3 S1 -86.24(13) 3_565 . . . ? N1 Cd1 O3 S1 15.11(13) . . . . ? N1 Cd1 O3 S1 -164.89(13) 3_565 . . . ? O3 Cd1 O3 S1 149(100) 3_565 . . . ? N2 Cd1 N1 C9 111.51(16) . . . . ? N2 Cd1 N1 C9 -68.49(16) 3_565 . . . ? N1 Cd1 N1 C9 165(100) 3_565 . . . ? O3 Cd1 N1 C9 25.27(15) 3_565 . . . ? O3 Cd1 N1 C9 -154.73(15) . . . . ? N2 Cd1 N1 C6 -13.98(12) . . . . ? N2 Cd1 N1 C6 166.02(12) 3_565 . . . ? N1 Cd1 N1 C6 39(100) 3_565 . . . ? O3 Cd1 N1 C6 -100.21(12) 3_565 . . . ? O3 Cd1 N1 C6 79.79(12) . . . . ? N2 Cd1 N2 C7 -79(77) 3_565 . . . ? N1 Cd1 N2 C7 -16.38(12) . . . . ? N1 Cd1 N2 C7 163.62(12) 3_565 . . . ? O3 Cd1 N2 C7 75.58(13) 3_565 . . . ? O3 Cd1 N2 C7 -104.42(13) . . . . ? N2 Cd1 N2 C8 47(77) 3_565 . . . ? N1 Cd1 N2 C8 109.90(16) . . . . ? N1 Cd1 N2 C8 -70.10(16) 3_565 . . . ? O3 Cd1 N2 C8 -158.15(16) 3_565 . . . ? O3 Cd1 N2 C8 21.85(16) . . . . ? C5 C1 C2 C2 -0.3(3) 3_666 . . 3_666 ? C5 C1 C2 C3 179.70(16) 3_666 . . . ? C2 C2 C3 C4 -0.6(3) 3_666 . . . ? C1 C2 C3 C4 179.37(16) . . . . ? C2 C3 C4 C5 1.0(2) . . . . ? C2 C3 C4 S1 -178.42(12) . . . . ? O2 S1 C4 C3 -130.30(15) . . . . ? O1 S1 C4 C3 -8.51(16) . . . . ? O3 S1 C4 C3 110.92(15) . . . . ? O2 S1 C4 C5 50.29(16) . . . . ? O1 S1 C4 C5 172.07(13) . . . . ? O3 S1 C4 C5 -68.50(15) . . . . ? C3 C4 C5 C1 -0.7(3) . . . 3_666 ? S1 C4 C5 C1 178.74(14) . . . 3_666 ? C9 N1 C6 C7 -84.3(2) . . . . ? Cd1 N1 C6 C7 43.16(19) . . . . ? C8 N2 C7 C6 -82.8(2) . . . . ? Cd1 N2 C7 C6 46.4(2) . . . . ? N1 C6 C7 N2 -64.7(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 O1 0.91 2.26 3.013(2) 140.3 . N2 H2A O1 0.91 2.17 3.042(2) 160.4 1_455 _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 29.99 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.565 _refine_diff_density_min -0.541 _refine_diff_density_rms 0.065 #==================================================end data_compound2 _database_code_CSD 162418 _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(N,N'-dimethylethylenediamine)-cadmium(II) naphthalene-1,5-disulfonate ; _chemical_name_common Cd(N,N'-meen)2(1,5nds) _chemical_melting_point ? _chemical_formula_moiety 'Cd C8 H24 N4 2+, C10 H6 S2 O6 2-' _chemical_formula_sum 'C18 H30 Cd N4 O6 S2' _chemical_formula_weight 574.98 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 8.4306(14) _cell_length_b 8.5243(14) _cell_length_c 8.5607(14) _cell_angle_alpha 87.652(3) _cell_angle_beta 67.476(2) _cell_angle_gamma 88.910(3) _cell_volume 567.80(16) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.682 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 588 _exptl_absorpt_coefficient_mu 1.188 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.6480 _exptl_absorpt_correction_T_max 0.9540 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4608 _diffrn_reflns_av_R_equivalents 0.0572 _diffrn_reflns_av_sigmaI/netI 0.0494 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 4.32 _diffrn_reflns_theta_max 30.00 _reflns_number_total 3130 _reflns_number_gt 2903 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0608P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3130 _refine_ls_number_parameters 142 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0402 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.0934 _refine_ls_wR_factor_gt 0.0915 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 0.5000 1.0000 0.5000 0.02804(9) Uani 1 2 d S . . S1 S 0.75686(8) 0.81217(7) 0.71305(8) 0.03234(14) Uani 1 1 d . . . N1 N 0.2832(3) 0.8169(3) 0.6512(3) 0.0370(5) Uani 1 1 d . . . H1A H 0.1921 0.8379 0.6214 0.044 Uiso 1 1 calc R . . N2 N 0.3721(3) 1.1117(3) 0.7669(3) 0.0391(5) Uani 1 1 d . . . H2A H 0.4397 1.0892 0.8261 0.047 Uiso 1 1 calc R . . O1 O 0.9019(3) 0.8994(2) 0.7152(3) 0.0455(5) Uani 1 1 d . . . O2 O 0.7079(3) 0.8628(3) 0.5727(3) 0.0466(5) Uani 1 1 d . . . O3 O 0.6123(3) 0.8054(3) 0.8737(3) 0.0481(5) Uani 1 1 d . . . C1 C 0.8049(4) 0.3403(3) 0.7537(3) 0.0390(6) Uani 1 1 d . . . H1B H 0.7482 0.2617 0.8330 0.047 Uiso 1 1 calc R . . C2 C 0.7501(3) 0.4974(3) 0.7837(3) 0.0368(5) Uani 1 1 d . . . H2B H 0.6585 0.5217 0.8827 0.044 Uiso 1 1 calc R . . C3 C 0.8311(3) 0.6142(3) 0.6676(3) 0.0290(4) Uani 1 1 d . . . C4 C 0.9726(3) 0.5801(3) 0.5139(3) 0.0262(4) Uani 1 1 d . . . C5 C 1.0604(3) 0.6984(3) 0.3898(3) 0.0325(5) Uani 1 1 d . . . H5A H 1.0255 0.8026 0.4068 0.039 Uiso 1 1 calc R . . C6 C 0.3184(5) 0.6492(4) 0.6330(6) 0.0580(9) Uani 1 1 d . . . H6A H 0.2177 0.5915 0.7024 0.087 Uiso 1 1 calc R . . H6B H 0.4112 0.6220 0.6679 0.087 Uiso 1 1 calc R . . H6C H 0.3495 0.6237 0.5168 0.087 Uiso 1 1 calc R . . C7 C 0.2298(4) 0.8543(4) 0.8306(4) 0.0462(7) Uani 1 1 d . . . H7A H 0.3159 0.8164 0.8725 0.055 Uiso 1 1 calc R . . H7B H 0.1225 0.8018 0.8964 0.055 Uiso 1 1 calc R . . C8 C 0.2072(4) 1.0277(4) 0.8521(4) 0.0476(7) Uani 1 1 d . . . H8A H 0.1252 1.0662 0.8051 0.057 Uiso 1 1 calc R . . H8B H 0.1614 1.0491 0.9717 0.057 Uiso 1 1 calc R . . C9 C 0.3401(5) 1.2811(4) 0.7706(5) 0.0587(9) Uani 1 1 d . . . H9A H 0.2880 1.3120 0.8859 0.088 Uiso 1 1 calc R . . H9B H 0.2645 1.3067 0.7132 0.088 Uiso 1 1 calc R . . H9C H 0.4468 1.3356 0.7150 0.088 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.02680(13) 0.03171(14) 0.02258(13) -0.00243(8) -0.00635(9) 0.00876(8) S1 0.0310(3) 0.0374(3) 0.0329(3) -0.0115(2) -0.0167(2) 0.0148(2) N1 0.0312(10) 0.0406(12) 0.0399(12) 0.0034(9) -0.0151(9) 0.0019(9) N2 0.0353(11) 0.0524(13) 0.0313(11) -0.0110(10) -0.0140(9) 0.0074(9) O1 0.0442(11) 0.0422(11) 0.0569(13) -0.0162(9) -0.0260(10) 0.0076(8) O2 0.0495(11) 0.0544(12) 0.0451(11) -0.0105(9) -0.0287(9) 0.0264(9) O3 0.0390(10) 0.0615(13) 0.0394(11) -0.0184(10) -0.0092(8) 0.0194(9) C1 0.0417(14) 0.0411(14) 0.0289(12) 0.0057(10) -0.0083(10) 0.0000(11) C2 0.0342(12) 0.0446(14) 0.0262(11) -0.0039(10) -0.0055(9) 0.0052(10) C3 0.0271(10) 0.0343(11) 0.0267(11) -0.0062(9) -0.0116(8) 0.0092(8) C4 0.0253(10) 0.0306(11) 0.0243(10) -0.0038(8) -0.0112(8) 0.0072(8) C5 0.0352(12) 0.0298(11) 0.0326(12) 0.0002(9) -0.0136(9) 0.0058(9) C6 0.056(2) 0.0402(16) 0.081(3) 0.0045(16) -0.0304(18) 0.0004(14) C7 0.0357(13) 0.0661(19) 0.0330(13) 0.0096(13) -0.0099(10) -0.0042(12) C8 0.0318(13) 0.079(2) 0.0273(12) -0.0141(13) -0.0047(10) 0.0049(13) C9 0.070(2) 0.0567(19) 0.052(2) -0.0194(16) -0.0238(17) 0.0112(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O2 2.3504(19) 2_676 ? Cd1 O2 2.3504(19) . ? Cd1 N2 2.354(2) 2_676 ? Cd1 N2 2.354(2) . ? Cd1 N1 2.363(2) 2_676 ? Cd1 N1 2.363(2) . ? S1 O3 1.446(2) . ? S1 O1 1.450(2) . ? S1 O2 1.460(2) . ? S1 C3 1.794(2) . ? N1 C6 1.457(4) . ? N1 C7 1.473(4) . ? N2 C9 1.463(4) . ? N2 C8 1.482(4) . ? C1 C5 1.363(4) 2_766 ? C1 C2 1.410(4) . ? C2 C3 1.368(4) . ? C3 C4 1.433(3) . ? C4 C5 1.425(3) . ? C4 C4 1.433(4) 2_766 ? C5 C1 1.363(4) 2_766 ? C7 C8 1.496(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cd1 O2 180.0 2_676 . ? O2 Cd1 N2 93.46(8) 2_676 2_676 ? O2 Cd1 N2 86.54(8) . 2_676 ? O2 Cd1 N2 86.54(8) 2_676 . ? O2 Cd1 N2 93.46(8) . . ? N2 Cd1 N2 180.0 2_676 . ? O2 Cd1 N1 92.62(8) 2_676 2_676 ? O2 Cd1 N1 87.38(8) . 2_676 ? N2 Cd1 N1 77.42(9) 2_676 2_676 ? N2 Cd1 N1 102.58(9) . 2_676 ? O2 Cd1 N1 87.38(8) 2_676 . ? O2 Cd1 N1 92.62(8) . . ? N2 Cd1 N1 102.58(9) 2_676 . ? N2 Cd1 N1 77.42(9) . . ? N1 Cd1 N1 180.0 2_676 . ? O3 S1 O1 113.88(14) . . ? O3 S1 O2 112.66(14) . . ? O1 S1 O2 112.30(15) . . ? O3 S1 C3 106.69(13) . . ? O1 S1 C3 106.03(12) . . ? O2 S1 C3 104.40(11) . . ? C6 N1 C7 109.2(3) . . ? C6 N1 Cd1 119.9(2) . . ? C7 N1 Cd1 105.59(17) . . ? C9 N2 C8 109.4(3) . . ? C9 N2 Cd1 117.5(2) . . ? C8 N2 Cd1 105.22(17) . . ? S1 O2 Cd1 144.37(13) . . ? C5 C1 C2 121.1(2) 2_766 . ? C3 C2 C1 120.2(2) . . ? C2 C3 C4 121.1(2) . . ? C2 C3 S1 118.28(18) . . ? C4 C3 S1 120.64(18) . . ? C5 C4 C3 122.8(2) . . ? C5 C4 C4 119.3(3) . 2_766 ? C3 C4 C4 117.9(3) . 2_766 ? C1 C5 C4 120.4(2) 2_766 . ? N1 C7 C8 110.7(2) . . ? N2 C8 C7 111.4(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 O2 Cd1 N1 C6 133.9(2) 2_676 . . . ? O2 Cd1 N1 C6 -46.1(2) . . . . ? N2 Cd1 N1 C6 40.9(2) 2_676 . . . ? N2 Cd1 N1 C6 -139.1(2) . . . . ? N1 Cd1 N1 C6 -98(100) 2_676 . . . ? O2 Cd1 N1 C7 -102.40(18) 2_676 . . . ? O2 Cd1 N1 C7 77.60(18) . . . . ? N2 Cd1 N1 C7 164.63(17) 2_676 . . . ? N2 Cd1 N1 C7 -15.37(17) . . . . ? N1 Cd1 N1 C7 26(100) 2_676 . . . ? O2 Cd1 N2 C9 -48.9(2) 2_676 . . . ? O2 Cd1 N2 C9 131.1(2) . . . . ? N2 Cd1 N2 C9 -170(100) 2_676 . . . ? N1 Cd1 N2 C9 43.0(2) 2_676 . . . ? N1 Cd1 N2 C9 -137.0(2) . . . . ? O2 Cd1 N2 C8 73.05(19) 2_676 . . . ? O2 Cd1 N2 C8 -106.95(19) . . . . ? N2 Cd1 N2 C8 -48(100) 2_676 . . . ? N1 Cd1 N2 C8 164.97(18) 2_676 . . . ? N1 Cd1 N2 C8 -15.03(18) . . . . ? O3 S1 O2 Cd1 22.7(3) . . . . ? O1 S1 O2 Cd1 -107.5(3) . . . . ? C3 S1 O2 Cd1 138.0(2) . . . . ? O2 Cd1 O2 S1 138(100) 2_676 . . . ? N2 Cd1 O2 S1 -166.8(3) 2_676 . . . ? N2 Cd1 O2 S1 13.2(3) . . . . ? N1 Cd1 O2 S1 115.7(3) 2_676 . . . ? N1 Cd1 O2 S1 -64.3(3) . . . . ? C5 C1 C2 C3 0.6(4) 2_766 . . . ? C1 C2 C3 C4 0.0(4) . . . . ? C1 C2 C3 S1 -179.6(2) . . . . ? O3 S1 C3 C2 -1.6(2) . . . . ? O1 S1 C3 C2 120.1(2) . . . . ? O2 S1 C3 C2 -121.1(2) . . . . ? O3 S1 C3 C4 178.76(19) . . . . ? O1 S1 C3 C4 -59.5(2) . . . . ? O2 S1 C3 C4 59.3(2) . . . . ? C2 C3 C4 C5 180.0(2) . . . . ? S1 C3 C4 C5 -0.4(3) . . . . ? C2 C3 C4 C4 -0.5(4) . . . 2_766 ? S1 C3 C4 C4 179.1(2) . . . 2_766 ? C3 C4 C5 C1 179.4(2) . . . 2_766 ? C4 C4 C5 C1 0.0(4) 2_766 . . 2_766 ? C6 N1 C7 C8 175.1(3) . . . . ? Cd1 N1 C7 C8 44.9(3) . . . . ? C9 N2 C8 C7 172.1(3) . . . . ? Cd1 N2 C8 C7 45.0(3) . . . . ? N1 C7 C8 N2 -64.6(3) . . . . ? 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 O1 0.91 2.32 3.118(3) 146.2 1_455 N2 H2A O3 0.91 2.63 3.237(3) 124.8 2_677 _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 1.336 _refine_diff_density_min -1.452 _refine_diff_density_rms 0.118 #========================================end data_compound3 _database_code_CSD 162419 _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(N,N'-dimethylethylenediamine)-cadmium(II) 4,4'-biphenyldisulfonate ; _chemical_name_common Cd(N,N'-meen)2(bpds) _chemical_melting_point ? _chemical_formula_moiety 'Cd C8 H24 N4 2+, C12 H8 S2 O6 2-' _chemical_formula_sum 'C20 H32 Cd N4 O6 S2' _chemical_formula_weight 601.02 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' '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 7.6031(10) _cell_length_b 9.0127(12) _cell_length_c 9.5933(13) _cell_angle_alpha 73.237(2) _cell_angle_beta 84.119(2) _cell_angle_gamma 72.192(2) _cell_volume 599.21(14) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.666 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 1.129 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7139 _exptl_absorpt_correction_T_max 0.8954 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4330 _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 4.25 _diffrn_reflns_theta_max 30.01 _reflns_number_total 3319 _reflns_number_gt 3096 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0610P)^2^+0.0610P] 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 3319 _refine_ls_number_parameters 151 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0348 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0880 _refine_ls_wR_factor_gt 0.0862 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 0.5000 1.0000 1.0000 0.03122(8) Uani 1 2 d S . . S1 S 0.97352(6) 0.83448(6) 0.88331(5) 0.03000(11) Uani 1 1 d . . . O1 O 0.8035(2) 0.8278(2) 0.96798(19) 0.0414(4) Uani 1 1 d . . . O2 O 0.9705(3) 0.9974(2) 0.7981(2) 0.0426(4) Uani 1 1 d . . . O3 O 1.1378(2) 0.7502(2) 0.97066(19) 0.0428(4) Uani 1 1 d . . . N1 N 0.3769(3) 1.0005(3) 0.7888(2) 0.0426(4) Uani 1 1 d . . . H1A H 0.2583 0.9983 0.8107 0.051 Uiso 1 1 calc R . . N2 N 0.4274(3) 0.7783(2) 1.1690(2) 0.0418(4) Uani 1 1 d . . . H2A H 0.3042 0.7939 1.1621 0.050 Uiso 1 1 calc R . . C1 C 0.9811(3) 0.7239(2) 0.7552(2) 0.0293(4) Uani 1 1 d . . . C2 C 0.9298(3) 0.5817(3) 0.7975(2) 0.0356(4) Uani 1 1 d . . . H2B H 0.8898 0.5450 0.8925 0.043 Uiso 1 1 calc R . . C3 C 0.9384(3) 0.4949(3) 0.6980(2) 0.0363(4) Uani 1 1 d . . . H3A H 0.9044 0.3997 0.7280 0.044 Uiso 1 1 calc R . . C4 C 0.9967(3) 0.5463(2) 0.5536(2) 0.0284(4) Uani 1 1 d . . . C5 C 1.0472(3) 0.6893(3) 0.5143(2) 0.0388(5) Uani 1 1 d . . . H5A H 1.0863 0.7271 0.4191 0.047 Uiso 1 1 calc R . . C6 C 1.0404(3) 0.7768(3) 0.6138(2) 0.0376(4) Uani 1 1 d . . . H6A H 1.0760 0.8713 0.5850 0.045 Uiso 1 1 calc R . . C7 C 0.4645(4) 0.8682(4) 0.7233(4) 0.0586(7) Uani 1 1 d . . . H7A H 0.3991 0.8836 0.6373 0.088 Uiso 1 1 calc R . . H7B H 0.4616 0.7673 0.7915 0.088 Uiso 1 1 calc R . . H7C H 0.5904 0.8665 0.6977 0.088 Uiso 1 1 calc R . . C8 C 0.3674(4) 1.1609(4) 0.6884(3) 0.0535(7) Uani 1 1 d . . . H8A H 0.2649 1.2419 0.7171 0.064 Uiso 1 1 calc R . . H8B H 0.3448 1.1608 0.5907 0.064 Uiso 1 1 calc R . . C9 C 0.4567(4) 0.7957(4) 1.3118(3) 0.0530(6) Uani 1 1 d . . . H9A H 0.4626 0.6949 1.3857 0.064 Uiso 1 1 calc R . . H9B H 0.3532 0.8795 1.3357 0.064 Uiso 1 1 calc R . . C10 C 0.5226(4) 0.6173(3) 1.1507(4) 0.0606(8) Uani 1 1 d . . . H10A H 0.4824 0.5374 1.2257 0.091 Uiso 1 1 calc R . . H10B H 0.6535 0.5966 1.1571 0.091 Uiso 1 1 calc R . . H10C H 0.4944 0.6123 1.0572 0.091 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03794(13) 0.03250(12) 0.02605(12) -0.01083(8) 0.00399(7) -0.01301(8) S1 0.0283(2) 0.0312(2) 0.0333(2) -0.01379(19) 0.00313(17) -0.00912(18) O1 0.0345(8) 0.0456(9) 0.0485(9) -0.0230(7) 0.0130(6) -0.0127(7) O2 0.0497(9) 0.0328(8) 0.0475(9) -0.0123(7) 0.0039(7) -0.0154(7) O3 0.0395(8) 0.0491(9) 0.0422(9) -0.0180(7) -0.0069(7) -0.0090(7) N1 0.0344(9) 0.0625(13) 0.0417(10) -0.0273(9) 0.0049(7) -0.0189(9) N2 0.0355(9) 0.0359(9) 0.0505(11) -0.0031(8) -0.0015(8) -0.0134(7) C1 0.0270(8) 0.0297(9) 0.0317(9) -0.0110(7) -0.0005(7) -0.0065(7) C2 0.0461(11) 0.0359(10) 0.0281(9) -0.0116(8) 0.0085(8) -0.0168(9) C3 0.0473(12) 0.0340(10) 0.0319(10) -0.0115(8) 0.0069(8) -0.0178(9) C4 0.0281(8) 0.0306(9) 0.0266(9) -0.0078(7) -0.0012(6) -0.0083(7) C5 0.0541(13) 0.0434(11) 0.0262(9) -0.0093(8) 0.0035(8) -0.0262(10) C6 0.0509(12) 0.0372(10) 0.0320(10) -0.0089(8) 0.0019(8) -0.0244(9) C7 0.0519(15) 0.078(2) 0.0620(18) -0.0436(16) 0.0052(12) -0.0212(14) C8 0.0441(13) 0.0702(18) 0.0402(13) -0.0139(12) -0.0090(10) -0.0065(12) C9 0.0523(14) 0.0593(16) 0.0378(13) 0.0009(11) 0.0038(10) -0.0171(12) C10 0.0603(17) 0.0391(13) 0.082(2) -0.0132(13) -0.0060(15) -0.0156(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 N1 2.315(2) 2_677 ? Cd1 N1 2.315(2) . ? Cd1 N2 2.3554(19) 2_677 ? Cd1 N2 2.3554(19) . ? Cd1 O1 2.4018(16) . ? Cd1 O1 2.4018(16) 2_677 ? S1 O3 1.4514(17) . ? S1 O2 1.4546(17) . ? S1 O1 1.4622(16) . ? S1 C1 1.779(2) . ? N1 C7 1.457(4) . ? N1 C8 1.473(4) . ? N2 C10 1.462(4) . ? N2 C9 1.469(4) . ? C1 C6 1.379(3) . ? C1 C2 1.390(3) . ? C2 C3 1.383(3) . ? C3 C4 1.400(3) . ? C4 C5 1.393(3) . ? C4 C4 1.489(4) 2_766 ? C5 C6 1.392(3) . ? C8 C9 1.504(4) 2_677 ? C9 C8 1.504(4) 2_677 ? 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 180.000(1) 2_677 . ? N1 Cd1 N2 101.40(8) 2_677 2_677 ? N1 Cd1 N2 78.60(8) . 2_677 ? N1 Cd1 N2 78.60(8) 2_677 . ? N1 Cd1 N2 101.40(8) . . ? N2 Cd1 N2 180.0 2_677 . ? N1 Cd1 O1 83.39(7) 2_677 . ? N1 Cd1 O1 96.61(7) . . ? N2 Cd1 O1 90.33(7) 2_677 . ? N2 Cd1 O1 89.67(7) . . ? N1 Cd1 O1 96.61(7) 2_677 2_677 ? N1 Cd1 O1 83.39(7) . 2_677 ? N2 Cd1 O1 89.67(7) 2_677 2_677 ? N2 Cd1 O1 90.33(7) . 2_677 ? O1 Cd1 O1 180.0 . 2_677 ? O3 S1 O2 113.28(11) . . ? O3 S1 O1 112.45(11) . . ? O2 S1 O1 113.22(10) . . ? O3 S1 C1 106.18(10) . . ? O2 S1 C1 106.04(10) . . ? O1 S1 C1 104.80(10) . . ? S1 O1 Cd1 140.07(11) . . ? C7 N1 C8 112.9(2) . . ? C7 N1 Cd1 118.43(18) . . ? C8 N1 Cd1 104.88(16) . . ? C10 N2 C9 113.4(2) . . ? C10 N2 Cd1 117.11(18) . . ? C9 N2 Cd1 104.48(15) . . ? C6 C1 C2 119.39(19) . . ? C6 C1 S1 120.47(16) . . ? C2 C1 S1 120.14(16) . . ? C3 C2 C1 119.94(19) . . ? C2 C3 C4 121.93(19) . . ? C5 C4 C3 116.87(19) . . ? C5 C4 C4 121.4(2) . 2_766 ? C3 C4 C4 121.7(2) . 2_766 ? C6 C5 C4 121.6(2) . . ? C1 C6 C5 120.2(2) . . ? N1 C8 C9 111.5(2) . 2_677 ? N2 C9 C8 110.9(2) . 2_677 ? 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 136.71(15) . . . . ? O2 S1 O1 Cd1 6.7(2) . . . . ? C1 S1 O1 Cd1 -108.39(16) . . . . ? N1 Cd1 O1 S1 -103.21(17) 2_677 . . . ? N1 Cd1 O1 S1 76.79(17) . . . . ? N2 Cd1 O1 S1 -1.77(17) 2_677 . . . ? N2 Cd1 O1 S1 178.23(17) . . . . ? O1 Cd1 O1 S1 0(100) 2_677 . . . ? N1 Cd1 N1 C7 -62(100) 2_677 . . . ? N2 Cd1 N1 C7 111.1(2) 2_677 . . . ? N2 Cd1 N1 C7 -68.9(2) . . . . ? O1 Cd1 N1 C7 22.1(2) . . . . ? O1 Cd1 N1 C7 -157.9(2) 2_677 . . . ? N1 Cd1 N1 C8 171(100) 2_677 . . . ? N2 Cd1 N1 C8 -15.97(15) 2_677 . . . ? N2 Cd1 N1 C8 164.03(15) . . . . ? O1 Cd1 N1 C8 -104.97(15) . . . . ? O1 Cd1 N1 C8 75.03(15) 2_677 . . . ? N1 Cd1 N2 C10 -112.0(2) 2_677 . . . ? N1 Cd1 N2 C10 68.0(2) . . . . ? N2 Cd1 N2 C10 -117(100) 2_677 . . . ? O1 Cd1 N2 C10 -28.7(2) . . . . ? O1 Cd1 N2 C10 151.3(2) 2_677 . . . ? N1 Cd1 N2 C9 14.43(15) 2_677 . . . ? N1 Cd1 N2 C9 -165.57(15) . . . . ? N2 Cd1 N2 C9 10(100) 2_677 . . . ? O1 Cd1 N2 C9 97.75(16) . . . . ? O1 Cd1 N2 C9 -82.25(16) 2_677 . . . ? O3 S1 C1 C6 -100.33(19) . . . . ? O2 S1 C1 C6 20.4(2) . . . . ? O1 S1 C1 C6 140.46(18) . . . . ? O3 S1 C1 C2 78.68(19) . . . . ? O2 S1 C1 C2 -160.55(17) . . . . ? O1 S1 C1 C2 -40.53(19) . . . . ? C6 C1 C2 C3 -0.1(3) . . . . ? S1 C1 C2 C3 -179.11(18) . . . . ? C1 C2 C3 C4 -0.4(4) . . . . ? C2 C3 C4 C5 0.4(3) . . . . ? C2 C3 C4 C4 -179.2(2) . . . 2_766 ? C3 C4 C5 C6 0.1(3) . . . . ? C4 C4 C5 C6 179.7(2) 2_766 . . . ? C2 C1 C6 C5 0.6(3) . . . . ? S1 C1 C6 C5 179.60(19) . . . . ? C4 C5 C6 C1 -0.6(4) . . . . ? C7 N1 C8 C9 -84.7(3) . . . 2_677 ? Cd1 N1 C8 C9 45.6(3) . . . 2_677 ? C10 N2 C9 C8 85.0(3) . . . 2_677 ? Cd1 N2 C9 C8 -43.7(3) . . . 2_677 ? 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 O2 0.91 2.21 3.090(3) 163.9 1_455 N2 H2A O2 0.91 2.43 3.126(3) 133.6 2_677 N2 H2A O3 0.91 2.52 3.164(3) 128.6 1_455 _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 30.01 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 1.307 _refine_diff_density_min -0.863 _refine_diff_density_rms 0.089 #============================================end data_compound4 _database_code_CSD 162420 _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(N-methylethylenediamine)-cadmium(II) naphthalene-2,6-disulfonate dihydrate ; _chemical_name_common Cd(N-meen)2(2,6nds).2H2O _chemical_melting_point ? _chemical_formula_moiety 'Cd C6 H20 N4 2+, C10 H6 S2 O6 2-, 2(H2 O)' _chemical_formula_sum 'C16 H30 Cd N4 O8 S2' _chemical_formula_weight 582.96 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 8.4953(11) _cell_length_b 9.6732(13) _cell_length_c 14.0313(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.412(2) _cell_angle_gamma 90.00 _cell_volume 1153.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 4.31 _cell_measurement_theta_max 30.01 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.679 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 596 _exptl_absorpt_coefficient_mu 1.177 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7654 _exptl_absorpt_correction_T_max 0.8073 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8052 _diffrn_reflns_av_R_equivalents 0.0189 _diffrn_reflns_av_sigmaI/netI 0.0203 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 4.31 _diffrn_reflns_theta_max 30.01 _reflns_number_total 3286 _reflns_number_gt 2892 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0442P)^2^+0.4502P] 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 3286 _refine_ls_number_parameters 137 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0328 _refine_ls_R_factor_gt 0.0286 _refine_ls_wR_factor_ref 0.0809 _refine_ls_wR_factor_gt 0.0788 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.0000 0.0000 0.5000 0.03157(8) Uani 1 2 d S . . S1 S 0.35438(5) -0.13087(5) 0.35921(3) 0.02568(10) Uani 1 1 d . . . O1 O 0.49140(18) -0.04613(17) 0.33978(12) 0.0394(3) Uani 1 1 d . . . O2 O 0.24230(19) -0.05887(19) 0.41927(12) 0.0470(4) Uani 1 1 d . . . O3 O 0.2836(2) -0.18948(17) 0.27392(11) 0.0420(4) Uani 1 1 d . . . O1W O 0.9944(2) 0.6643(2) 0.30008(14) 0.0567(5) Uiso 1 1 d . . . N1 N 0.1534(2) 0.0821(2) 0.62294(12) 0.0361(4) Uani 1 1 d . . . H1B H 0.2554 0.0828 0.6061 0.043 Uiso 1 1 calc R . . H1C H 0.1247 0.1688 0.6382 0.043 Uiso 1 1 calc R . . N2 N -0.0094(2) 0.19046(18) 0.39618(13) 0.0364(4) Uani 1 1 d . . . H2A H 0.0823 0.1903 0.3630 0.044 Uiso 1 1 calc R . . C1 C 0.4244(2) -0.65516(19) 0.43470(13) 0.0311(4) Uani 1 1 d . . . H1A H 0.3647 -0.6755 0.3807 0.037 Uiso 1 1 calc R . . C2 C 0.4535(2) -0.51510(17) 0.45915(13) 0.0254(3) Uani 1 1 d . . . C3 C 0.3931(2) -0.40449(19) 0.40339(12) 0.0264(3) Uani 1 1 d . . . H3A H 0.3313 -0.4229 0.3499 0.032 Uiso 1 1 calc R . . C4 C 0.4258(2) -0.27039(18) 0.42841(12) 0.0245(3) Uani 1 1 d . . . C5 C 0.5172(2) -0.2391(2) 0.51066(13) 0.0302(4) Uani 1 1 d . . . H5A H 0.5373 -0.1476 0.5273 0.036 Uiso 1 1 calc R . . C6 C 0.1295(3) -0.0111(3) 0.70427(17) 0.0445(6) Uani 1 1 d . . . H6A H 0.0281 0.0076 0.7329 0.053 Uiso 1 1 calc R . . H6B H 0.2105 0.0054 0.7520 0.053 Uiso 1 1 calc R . . C7 C -0.1359(3) 0.1604(3) 0.32757(17) 0.0448(5) Uani 1 1 d . . . H7A H -0.1257 0.2204 0.2726 0.054 Uiso 1 1 calc R . . H7B H -0.2370 0.1788 0.3567 0.054 Uiso 1 1 calc R . . C8 C -0.0253(4) 0.3285(3) 0.4385(2) 0.0567(7) Uani 1 1 d . . . H8A H -0.0274 0.3967 0.3888 0.085 Uiso 1 1 calc R . . H8B H 0.0624 0.3459 0.4803 0.085 Uiso 1 1 calc R . . H8C H -0.1213 0.3331 0.4740 0.085 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03377(12) 0.03038(12) 0.03052(12) 0.00074(7) -0.00146(8) 0.00534(7) S1 0.0241(2) 0.0254(2) 0.0275(2) 0.00301(15) 0.00070(15) 0.00314(15) O1 0.0328(7) 0.0353(7) 0.0500(9) 0.0141(7) -0.0005(6) -0.0045(6) O2 0.0409(9) 0.0490(10) 0.0514(9) 0.0027(8) 0.0138(7) 0.0205(7) O3 0.0513(9) 0.0403(8) 0.0341(7) 0.0043(6) -0.0144(6) -0.0014(7) N1 0.0305(8) 0.0400(9) 0.0379(9) -0.0048(7) 0.0016(7) 0.0000(7) N2 0.0343(9) 0.0343(9) 0.0407(9) 0.0048(7) 0.0081(7) 0.0019(7) C1 0.0400(10) 0.0268(9) 0.0263(8) -0.0024(7) -0.0081(7) -0.0018(7) C2 0.0286(9) 0.0256(8) 0.0218(8) -0.0004(6) -0.0015(7) -0.0006(6) C3 0.0296(8) 0.0276(8) 0.0221(7) -0.0010(6) -0.0030(6) 0.0005(6) C4 0.0258(8) 0.0244(8) 0.0232(7) 0.0017(6) 0.0011(6) 0.0020(6) C5 0.0376(10) 0.0253(9) 0.0277(9) -0.0021(6) -0.0049(7) -0.0012(7) C6 0.0410(12) 0.0626(16) 0.0298(10) -0.0004(9) -0.0009(9) 0.0005(10) C7 0.0407(11) 0.0528(14) 0.0408(11) 0.0155(10) -0.0001(9) 0.0056(10) C8 0.0714(18) 0.0338(12) 0.0652(17) 0.0034(11) 0.0142(14) 0.0032(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 N1 2.2961(18) . ? Cd1 N1 2.2961(18) 3_556 ? Cd1 N2 2.3497(17) 3_556 ? Cd1 N2 2.3497(18) . ? Cd1 O2 2.4245(15) 3_556 ? Cd1 O2 2.4245(15) . ? S1 O3 1.4509(15) . ? S1 O1 1.4512(15) . ? S1 O2 1.4537(15) . ? S1 C4 1.7673(17) . ? N1 C6 1.469(3) . ? N2 C7 1.467(3) . ? N2 C8 1.467(3) . ? C1 C5 1.369(3) 3_646 ? C1 C2 1.419(2) . ? C2 C2 1.417(4) 3_646 ? C2 C3 1.420(2) . ? C3 C4 1.372(2) . ? C4 C5 1.419(2) . ? C5 C1 1.369(3) 3_646 ? C6 C7 1.512(4) 3_556 ? C7 C6 1.512(4) 3_556 ? 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 . 3_556 ? N1 Cd1 N2 77.80(7) . 3_556 ? N1 Cd1 N2 102.20(7) 3_556 3_556 ? N1 Cd1 N2 102.20(7) . . ? N1 Cd1 N2 77.80(7) 3_556 . ? N2 Cd1 N2 180.0 3_556 . ? N1 Cd1 O2 92.69(6) . 3_556 ? N1 Cd1 O2 87.31(6) 3_556 3_556 ? N2 Cd1 O2 85.40(6) 3_556 3_556 ? N2 Cd1 O2 94.60(6) . 3_556 ? N1 Cd1 O2 87.31(6) . . ? N1 Cd1 O2 92.69(6) 3_556 . ? N2 Cd1 O2 94.60(6) 3_556 . ? N2 Cd1 O2 85.40(6) . . ? O2 Cd1 O2 180.00(7) 3_556 . ? O3 S1 O1 113.21(10) . . ? O3 S1 O2 113.33(11) . . ? O1 S1 O2 111.58(11) . . ? O3 S1 C4 107.06(9) . . ? O1 S1 C4 105.19(9) . . ? O2 S1 C4 105.72(9) . . ? S1 O2 Cd1 160.94(13) . . ? C6 N1 Cd1 106.90(14) . . ? C7 N2 C8 112.1(2) . . ? C7 N2 Cd1 105.83(13) . . ? C8 N2 Cd1 117.73(15) . . ? C5 C1 C2 121.08(17) 3_646 . ? C2 C2 C1 119.17(19) 3_646 . ? C2 C2 C3 119.19(19) 3_646 . ? C1 C2 C3 121.64(16) . . ? C4 C3 C2 119.99(16) . . ? C3 C4 C5 121.25(16) . . ? C3 C4 S1 120.90(13) . . ? C5 C4 S1 117.86(14) . . ? C1 C5 C4 119.31(17) 3_646 . ? N1 C6 C7 110.53(19) . 3_556 ? N2 C7 C6 110.83(19) . 3_556 ? 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 O2 Cd1 35.1(4) . . . . ? O1 S1 O2 Cd1 164.3(3) . . . . ? C4 S1 O2 Cd1 -81.9(3) . . . . ? N1 Cd1 O2 S1 147.5(3) . . . . ? N1 Cd1 O2 S1 -32.5(3) 3_556 . . . ? N2 Cd1 O2 S1 69.9(3) 3_556 . . . ? N2 Cd1 O2 S1 -110.1(3) . . . . ? O2 Cd1 O2 S1 -42(100) 3_556 . . . ? N1 Cd1 N1 C6 -85(100) 3_556 . . . ? N2 Cd1 N1 C6 -16.49(14) 3_556 . . . ? N2 Cd1 N1 C6 163.51(14) . . . . ? O2 Cd1 N1 C6 68.20(14) 3_556 . . . ? O2 Cd1 N1 C6 -111.80(14) . . . . ? N1 Cd1 N2 C7 -166.21(13) . . . . ? N1 Cd1 N2 C7 13.79(13) 3_556 . . . ? N2 Cd1 N2 C7 53(12) 3_556 . . . ? O2 Cd1 N2 C7 -72.45(14) 3_556 . . . ? O2 Cd1 N2 C7 107.55(14) . . . . ? N1 Cd1 N2 C8 -39.94(19) . . . . ? N1 Cd1 N2 C8 140.06(19) 3_556 . . . ? N2 Cd1 N2 C8 179(12) 3_556 . . . ? O2 Cd1 N2 C8 53.82(18) 3_556 . . . ? O2 Cd1 N2 C8 -126.18(18) . . . . ? C5 C1 C2 C2 0.9(3) 3_646 . . 3_646 ? C5 C1 C2 C3 -179.69(18) 3_646 . . . ? C2 C2 C3 C4 0.5(3) 3_646 . . . ? C1 C2 C3 C4 -178.97(18) . . . . ? C2 C3 C4 C5 -1.2(3) . . . . ? C2 C3 C4 S1 179.05(14) . . . . ? O3 S1 C4 C3 -7.55(18) . . . . ? O1 S1 C4 C3 -128.25(16) . . . . ? O2 S1 C4 C3 113.56(16) . . . . ? O3 S1 C4 C5 172.69(14) . . . . ? O1 S1 C4 C5 51.99(16) . . . . ? O2 S1 C4 C5 -66.20(17) . . . . ? C3 C4 C5 C1 0.9(3) . . . 3_646 ? S1 C4 C5 C1 -179.36(15) . . . 3_646 ? Cd1 N1 C6 C7 45.1(2) . . . 3_556 ? C8 N2 C7 C6 -172.1(2) . . . 3_556 ? Cd1 N2 C7 C6 -42.4(2) . . . 3_556 ? 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 H1B O1 0.90 2.30 3.078(2) 144.2 3_656 N1 H1C O1W 0.90 2.10 2.963(3) 161.6 3_666 N2 H2A O3 0.91 2.53 3.285(2) 141.3 2 _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 30.01 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.096 _refine_diff_density_min -0.645 _refine_diff_density_rms 0.116