#------------------------------------------------------------------------------ #$Date: 2025-08-23 01:36:08 +0200 (Sat, 23 Aug 2025) $ #$Revision: 301880 $ #$URL: svn://www.crystallography.net/cod/cif/8/10/16/8101699.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_8101699 loop_ _publ_author_name 'S.-R. Fan' 'L.-P. Zhang' 'H.-P. Xiao' 'G.-Q. Cai' 'L.-G. Zhu' _publ_section_title ; Crystal structure of bis[diaqua(1,10-phenanthroline)(\m-4-sulfobenzoato) cadmium(II)], [Cd(H~2~O)~2~(C~12~H~8~N~2~)(C~7~H~4~O~5~S)]~2~ ; _journal_issue 1 _journal_name_full 'Zeitschrift f\"ur Kristallographie - New Crystal Structures' _journal_page_first 69 _journal_page_last 70 _journal_volume 220 _journal_year 2005 _chemical_formula_moiety 'C38 H32 Cd2 N4 O14 S2' _chemical_formula_sum 'C38 H32 Cd2 N4 O14 S2' _chemical_formula_weight 1057.60 _chemical_name_systematic ; bis[diaqua(1,10-phenanthroline)(\m-4-sulfobenzoato)cadmium(II)] ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 102.000(2) _cell_angle_beta 101.049(2) _cell_angle_gamma 113.4530(10) _cell_formula_units_Z 1 _cell_length_a 8.2384(8) _cell_length_b 10.1299(9) _cell_length_c 12.9685(12) _cell_measurement_reflns_used 8023 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 56.4 _cell_measurement_theta_min 3.4 _cell_volume 924.65(15) _computing_cell_refinement SMART _computing_data_collection 'SMART (Bruker, 1997)' _computing_data_reduction 'SHELXTL (Bruker, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 6782 _diffrn_reflns_theta_full 25.10 _diffrn_reflns_theta_max 25.10 _diffrn_reflns_theta_min 1.69 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.343 _exptl_absorpt_correction_T_max 0.9002 _exptl_absorpt_correction_T_min 0.811 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.899 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 528 _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.770 _refine_diff_density_min -1.168 _refine_diff_density_rms 0.098 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.261 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 283 _refine_ls_number_reflns 3274 _refine_ls_number_restraints 4 _refine_ls_restrained_S_all 1.261 _refine_ls_R_factor_all 0.0533 _refine_ls_R_factor_gt 0.0518 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0211P)^2^+3.3727P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0995 _refine_ls_wR_factor_ref 0.1001 _reflns_number_gt 3208 _reflns_number_total 3274 _reflns_threshold_expression >2sigma(I) _cod_data_source_file 1267-1429.cff _cod_data_source_block x59-lgzhu _cod_original_sg_symbol_H-M P-1 _cod_database_code 8101699 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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_Wyckoff_symbol _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.75349(6) 0.65201(4) 0.21276(3) 0.03123(14) Uani 1 2 i d . . . S1 S 0.7912(2) 1.25926(16) -0.18994(12) 0.0347(3) Uani 1 2 i d . . . O1 O 0.6528(6) 0.7159(5) 0.0561(4) 0.0466(11) Uani 1 2 i d . . . O2 O 0.8334(6) 0.9152(5) 0.2016(3) 0.0501(11) Uani 1 2 i d . . . O3 O 0.9279(6) 1.2497(5) -0.2426(3) 0.0441(10) Uani 1 2 i d . . . O4 O 0.6105(7) 1.1973(6) -0.2678(5) 0.0757(17) Uani 1 2 i d . . . O5 O 0.8554(7) 1.4128(5) -0.1185(4) 0.0569(13) Uani 1 2 i d . . . O6 O 0.4268(6) 0.4814(5) 0.1612(4) 0.0405(10) Uani 1 2 i d D . . O7 O 0.7259(6) 0.4484(5) 0.0724(4) 0.0422(10) Uani 1 2 i d D . . N1 N 0.7601(6) 0.7553(5) 0.3910(4) 0.0322(10) Uani 1 2 i d . . . N2 N 0.7840(6) 0.4925(5) 0.3210(4) 0.0326(10) Uani 1 2 i d . . . C1 C 0.7558(9) 0.8860(7) 0.4274(5) 0.0433(15) Uani 1 2 i d . . . H1 H 0.7562 0.9430 0.3797 0.052 Uiso 1 2 i calc R . . C2 C 0.7508(10) 0.9413(8) 0.5328(5) 0.0530(17) Uani 1 2 i d . . . H2 H 0.7530 1.0354 0.5558 0.064 Uiso 1 2 i calc R . . C3 C 0.7426(9) 0.8580(8) 0.6023(5) 0.0523(17) Uani 1 2 i d . . . H3 H 0.7378 0.8940 0.6732 0.063 Uiso 1 2 i calc R . . C4 C 0.7415(8) 0.7178(7) 0.5673(5) 0.0410(15) Uani 1 2 i d . . . C5 C 0.7246(9) 0.6200(9) 0.6333(5) 0.0521(18) Uani 1 2 i d . . . H5 H 0.7104 0.6484 0.7027 0.063 Uiso 1 2 i calc R . . C6 C 0.7289(9) 0.4868(9) 0.5972(6) 0.057(2) Uani 1 2 i d . . . H6 H 0.7162 0.4246 0.6418 0.068 Uiso 1 2 i calc R . . C7 C 0.7526(8) 0.4398(7) 0.4920(5) 0.0439(15) Uani 1 2 i d . . . C8 C 0.7680(9) 0.3069(8) 0.4526(6) 0.0546(19) Uani 1 2 i d . . . H8 H 0.7604 0.2429 0.4955 0.066 Uiso 1 2 i calc R . . C9 C 0.7938(9) 0.2714(7) 0.3529(6) 0.0514(17) Uani 1 2 i d . . . H9 H 0.8069 0.1845 0.3274 0.062 Uiso 1 2 i calc R . . C10 C 0.8006(8) 0.3670(7) 0.2887(5) 0.0428(15) Uani 1 2 i d . . . H10 H 0.8176 0.3413 0.2199 0.051 Uiso 1 2 i calc R . . C11 C 0.7541(7) 0.6712(6) 0.4596(4) 0.0326(12) Uani 1 2 i d . . . C12 C 0.7628(7) 0.5303(6) 0.4218(4) 0.0317(12) Uani 1 2 i d . . . C13 C 0.7466(8) 0.8594(7) 0.1019(5) 0.0355(13) Uani 1 2 i d . . . C14 C 0.7534(8) 0.9596(6) 0.0305(4) 0.0313(12) Uani 1 2 i d . . . C15 C 0.6231(8) 0.9069(7) -0.0719(5) 0.0420(15) Uani 1 2 i d . . . H15 H 0.5278 0.8081 -0.0969 0.050 Uiso 1 2 i calc R . . C16 C 0.6327(8) 0.9994(6) -0.1378(5) 0.0396(14) Uani 1 2 i d . . . H16 H 0.5430 0.9636 -0.2061 0.047 Uiso 1 2 i calc R . . C17 C 0.7754(7) 1.1444(6) -0.1018(4) 0.0296(12) Uani 1 2 i d . . . C18 C 0.9062(8) 1.1988(6) 0.0009(5) 0.0369(13) Uani 1 2 i d . . . H18 H 1.0022 1.2972 0.0254 0.044 Uiso 1 2 i calc R . . C19 C 0.8941(8) 1.1071(6) 0.0665(5) 0.0361(13) Uani 1 2 i d . . . H19 H 0.9813 1.1445 0.1359 0.043 Uiso 1 2 i calc R . . H7A H 0.624(4) 0.396(6) 0.026(4) 0.050 Uiso 1 2 i d D . . H6B H 0.400(9) 0.420(6) 0.101(3) 0.050 Uiso 1 2 i d D . . H6A H 0.372(8) 0.533(6) 0.157(6) 0.050 Uiso 1 2 i d D . . H7B H 0.821(5) 0.466(7) 0.055(5) 0.050 Uiso 1 2 i d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0436(3) 0.0278(2) 0.0243(2) 0.01262(16) 0.01072(17) 0.01583(18) S1 0.0387(8) 0.0361(8) 0.0407(8) 0.0246(7) 0.0177(7) 0.0196(7) O1 0.060(3) 0.036(2) 0.048(3) 0.025(2) 0.019(2) 0.019(2) O2 0.062(3) 0.054(3) 0.034(2) 0.024(2) 0.009(2) 0.024(2) O3 0.055(3) 0.042(2) 0.043(2) 0.018(2) 0.024(2) 0.022(2) O4 0.043(3) 0.097(4) 0.090(4) 0.073(4) 0.007(3) 0.020(3) O5 0.095(4) 0.041(3) 0.065(3) 0.031(2) 0.049(3) 0.043(3) O6 0.048(3) 0.045(3) 0.040(2) 0.021(2) 0.020(2) 0.027(2) O7 0.042(3) 0.043(3) 0.045(3) 0.014(2) 0.022(2) 0.019(2) N1 0.037(3) 0.032(3) 0.029(2) 0.013(2) 0.010(2) 0.016(2) N2 0.035(3) 0.029(2) 0.035(3) 0.014(2) 0.011(2) 0.013(2) C1 0.049(4) 0.042(4) 0.038(3) 0.016(3) 0.008(3) 0.021(3) C2 0.073(5) 0.049(4) 0.042(4) 0.010(3) 0.022(4) 0.033(4) C3 0.057(4) 0.067(5) 0.034(3) 0.008(3) 0.021(3) 0.030(4) C4 0.034(3) 0.059(4) 0.030(3) 0.020(3) 0.009(3) 0.018(3) C5 0.039(4) 0.076(5) 0.037(4) 0.031(4) 0.011(3) 0.016(4) C6 0.048(4) 0.076(5) 0.048(4) 0.050(4) 0.011(3) 0.018(4) C7 0.034(3) 0.049(4) 0.045(4) 0.030(3) 0.006(3) 0.010(3) C8 0.047(4) 0.044(4) 0.069(5) 0.038(4) 0.006(4) 0.011(3) C9 0.049(4) 0.035(4) 0.061(5) 0.013(3) -0.001(3) 0.020(3) C10 0.041(4) 0.037(3) 0.049(4) 0.014(3) 0.005(3) 0.019(3) C11 0.023(3) 0.039(3) 0.032(3) 0.016(3) 0.006(2) 0.009(2) C12 0.022(3) 0.038(3) 0.034(3) 0.020(3) 0.005(2) 0.009(2) C13 0.041(3) 0.035(3) 0.041(4) 0.025(3) 0.017(3) 0.018(3) C14 0.040(3) 0.032(3) 0.029(3) 0.016(2) 0.014(2) 0.019(3) C15 0.042(3) 0.029(3) 0.041(3) 0.015(3) 0.003(3) 0.004(3) C16 0.041(3) 0.035(3) 0.032(3) 0.016(3) 0.002(3) 0.010(3) C17 0.030(3) 0.030(3) 0.034(3) 0.017(2) 0.013(2) 0.014(2) C18 0.039(3) 0.026(3) 0.039(3) 0.013(3) 0.009(3) 0.008(3) C19 0.037(3) 0.034(3) 0.030(3) 0.010(2) 0.000(2) 0.015(3) 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' 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 O3 98.20(15) . 2_775 ? N1 Cd1 O7 150.58(16) . . ? O3 Cd1 O7 86.16(14) 2_775 . ? N1 Cd1 O1 126.10(15) . . ? O3 Cd1 O1 102.79(15) 2_775 . ? O7 Cd1 O1 80.39(15) . . ? N1 Cd1 N2 70.63(15) . . ? O3 Cd1 N2 86.96(15) 2_775 . ? O7 Cd1 N2 80.64(16) . . ? O1 Cd1 N2 157.99(15) . . ? N1 Cd1 O6 91.71(15) . . ? O3 Cd1 O6 163.13(14) 2_775 . ? O7 Cd1 O6 78.60(14) . . ? O1 Cd1 O6 81.92(14) . . ? N2 Cd1 O6 83.48(15) . . ? N1 Cd1 O2 83.89(15) . . ? O3 Cd1 O2 78.98(15) 2_775 . ? O7 Cd1 O2 125.37(15) . . ? O1 Cd1 O2 53.20(14) . . ? N2 Cd1 O2 148.81(15) . . ? O6 Cd1 O2 115.82(14) . . ? O4 S1 O3 112.4(3) . . ? O4 S1 O5 113.5(3) . . ? O3 S1 O5 111.0(3) . . ? O4 S1 C17 107.0(3) . . ? O3 S1 C17 105.9(2) . . ? O5 S1 C17 106.4(3) . . ? C13 O1 Cd1 95.8(3) . . ? C13 O2 Cd1 89.2(3) . . ? S1 O3 Cd1 142.2(3) . 2_775 ? Cd1 O6 H6B 107(5) . . ? Cd1 O6 H6A 107(5) . . ? H6B O6 H6A 112(7) . . ? Cd1 O7 H7A 116(5) . . ? Cd1 O7 H7B 113(5) . . ? H7A O7 H7B 121(7) . . ? C1 N1 C11 118.1(5) . . ? C1 N1 Cd1 124.4(4) . . ? C11 N1 Cd1 117.3(4) . . ? C10 N2 C12 118.0(5) . . ? C10 N2 Cd1 127.4(4) . . ? C12 N2 Cd1 114.3(3) . . ? N1 C1 C2 123.1(6) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C3 C2 C1 119.7(6) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 119.6(6) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C3 C4 C11 117.4(5) . . ? C3 C4 C5 123.2(6) . . ? C11 C4 C5 119.3(6) . . ? C6 C5 C4 121.2(6) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C5 C6 C7 121.2(6) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C8 C7 C12 116.7(6) . . ? C8 C7 C6 123.8(6) . . ? C12 C7 C6 119.6(6) . . ? C9 C8 C7 120.4(6) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C10 119.0(6) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? N2 C10 C9 123.2(6) . . ? N2 C10 H10 118.4 . . ? C9 C10 H10 118.4 . . ? N1 C11 C4 122.0(5) . . ? N1 C11 C12 118.6(5) . . ? C4 C11 C12 119.4(5) . . ? N2 C12 C7 122.8(5) . . ? N2 C12 C11 118.1(5) . . ? C7 C12 C11 119.1(5) . . ? O2 C13 O1 121.4(5) . . ? O2 C13 C14 120.3(5) . . ? O1 C13 C14 118.3(5) . . ? C15 C14 C19 118.8(5) . . ? C15 C14 C13 121.2(5) . . ? C19 C14 C13 119.9(5) . . ? C14 C15 C16 120.7(5) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C17 C16 C15 119.7(5) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C18 120.1(5) . . ? C16 C17 S1 119.2(4) . . ? C18 C17 S1 120.7(4) . . ? C19 C18 C17 119.8(5) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C14 120.8(5) . . ? C18 C19 H19 119.6 . . ? C14 C19 H19 119.6 . . ? 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 2.311(4) . ? Cd1 O3 2.324(4) 2_775 ? Cd1 O7 2.350(4) . ? Cd1 O1 2.359(4) . ? Cd1 N2 2.403(4) . ? Cd1 O6 2.409(5) . ? Cd1 O2 2.522(4) . ? S1 O4 1.431(5) . ? S1 O3 1.448(4) . ? S1 O5 1.454(5) . ? S1 C17 1.780(5) . ? O1 C13 1.278(7) . ? O2 C13 1.234(7) . ? O3 Cd1 2.324(4) 2_775 ? O6 H6B 0.82(4) . ? O6 H6A 0.82(7) . ? O7 H7A 0.82(5) . ? O7 H7B 0.82(5) . ? N1 C1 1.326(7) . ? N1 C11 1.349(7) . ? N2 C10 1.323(7) . ? N2 C12 1.348(7) . ? C1 C2 1.380(8) . ? C1 H1 0.9300 . ? C2 C3 1.351(9) . ? C2 H2 0.9300 . ? C3 C4 1.394(9) . ? C3 H3 0.9300 . ? C4 C11 1.416(8) . ? C4 C5 1.422(9) . ? C5 C6 1.350(10) . ? C5 H5 0.9300 . ? C6 C7 1.426(10) . ? C6 H6 0.9300 . ? C7 C8 1.401(10) . ? C7 C12 1.411(7) . ? C8 C9 1.349(10) . ? C8 H8 0.9300 . ? C9 C10 1.394(9) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.444(8) . ? C13 C14 1.503(7) . ? C14 C15 1.379(8) . ? C14 C19 1.385(8) . ? C15 C16 1.383(8) . ? C15 H15 0.9300 . ? C16 C17 1.374(8) . ? C16 H16 0.9300 . ? C17 C18 1.382(8) . ? C18 C19 1.372(8) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? 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 O7 H7A O1 0.82(5) 2.03(5) 2.829(6) 165(7) 2_665 O6 H6A O5 0.82(7) 2.15(7) 2.933(6) 159(6) 2_675 O6 H6A S1 0.82(7) 2.92(7) 3.725(4) 169(6) 2_675 O6 H6B O1 0.82(4) 2.06(4) 2.876(6) 174(7) 2_665 O7 H7B O5 0.82(5) 2.30(5) 2.889(6) 129(6) 1_545 O7 H7B O5 0.82(5) 2.33(4) 3.038(7) 145(6) 2_775 loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 168344149