#------------------------------------------------------------------------------ #$Date: 2025-08-19 11:43:10 +0100 (Tue, 19 Aug 2025) $ #$Revision: 301803 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/24/2202413.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2202413 loop_ _publ_author_name 'Jian-Fang Ma' 'Jin Yang' 'Jing-Fu Liu' _publ_section_title ; Hexaaquacopper(II) 3-carboxy-4-hydroxybenzenesulfonate dihydrate ; _journal_issue 7 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m485 _journal_page_last m486 _journal_paper_doi 10.1107/S1600536803013084 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac '[Cu (H2 O)6] (C7 H5 O6 S)2, 2H2 O' _chemical_formula_moiety 'H12 Cu O6 2+, 2C7 H5 O6 S 1-, 2H2 O' _chemical_formula_sum 'C14 H26 Cu O20 S2' _chemical_formula_weight 642.01 _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 92.16(2) _cell_angle_beta 90.259(18) _cell_angle_gamma 112.236(12) _cell_formula_units_Z 1 _cell_length_a 7.0298(9) _cell_length_b 7.0749(15) _cell_length_c 13.288(4) _cell_measurement_reflns_used 20 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 9.92 _cell_measurement_theta_min 5.36 _cell_volume 611.2(2) _computing_cell_refinement XSCANS _computing_data_collection 'XSCANS (Siemens, 1994)' _computing_data_reduction XSCANS _computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 1990)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method \w _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 0.0166 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 3134 _diffrn_reflns_theta_full 26.01 _diffrn_reflns_theta_max 26.01 _diffrn_reflns_theta_min 1.53 _diffrn_standards_decay_% none _diffrn_standards_interval_count 97 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.157 _exptl_absorpt_correction_type none _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.744 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 331 _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.34 _refine_diff_density_max 0.298 _refine_diff_density_min -0.524 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 193 _refine_ls_number_reflns 2413 _refine_ls_number_restraints 8 _refine_ls_restrained_S_all 1.111 _refine_ls_R_factor_all 0.0362 _refine_ls_R_factor_gt 0.0322 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0566P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0911 _refine_ls_wR_factor_ref 0.0926 _reflns_number_gt 2140 _reflns_number_total 2413 _reflns_threshold_expression I>2\s(I) _cod_data_source_file cf6252.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2202413 _cod_database_fobs_code 2202413 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol C1 0.2205(3) 0.4403(3) 0.65438(15) 0.0244(4) Uani d . 1 . . C C2 0.2004(3) 0.3313(3) 0.56410(15) 0.0243(4) Uani d . 1 . . C H2 0.1638 0.1904 0.5634 0.029 Uiso calc R 1 . . H C3 0.2352(3) 0.4327(3) 0.47369(15) 0.0241(4) Uani d . 1 . . C C4 0.2928(4) 0.6457(4) 0.47607(17) 0.0284(5) Uani d . 1 . . C C5 0.3103(4) 0.7531(3) 0.56800(18) 0.0322(5) Uani d . 1 . . C H5 0.3472 0.8941 0.5695 0.039 Uiso calc R 1 . . H C6 0.2734(4) 0.6517(3) 0.65644(17) 0.0301(5) Uani d . 1 . . C H6 0.2835 0.7237 0.7176 0.036 Uiso calc R 1 . . H C7 0.2117(4) 0.3171(4) 0.37601(17) 0.0305(5) Uani d . 1 . . C O1 0.3123(3) 0.1933(3) 0.76643(13) 0.0416(5) Uani d . 1 . . O O2 -0.0378(3) 0.1691(2) 0.76838(12) 0.0308(4) Uani d . 1 . . O O3 0.2249(3) 0.4634(3) 0.84896(12) 0.0444(5) Uani d . 1 . . O O4 0.1564(3) 0.1200(3) 0.38535(12) 0.0418(5) Uani d . 1 . . O H4 0.1452 0.0634 0.3294 0.063 Uiso calc R 1 . . H O5 0.2416(4) 0.3988(3) 0.29508(12) 0.0467(5) Uani d . 1 . . O O6 0.3330(3) 0.7531(3) 0.39242(14) 0.0448(5) Uani d . 1 . . O H6A 0.3181 0.6754 0.3431 0.067 Uiso calc R 1 . . H OW1 0.6723(3) 0.2571(3) 0.88095(12) 0.0317(4) Uani d D 1 . . O OW2 0.4356(3) 0.1959(3) 1.08673(14) 0.0378(4) Uani d D 1 . . O OW3 0.2426(3) -0.0653(3) 0.92333(14) 0.0378(4) Uani d D 1 . . O OW4 0.8673(3) 0.6598(3) 0.95578(13) 0.0338(4) Uani d D 1 . . O S1 0.17750(9) 0.30792(8) 0.76709(4) 0.02569(16) Uani d . 1 . . S Cu1 0.5000 0.0000 1.0000 0.02392(14) Uani d S 1 . . Cu H1A 0.766(4) 0.237(4) 0.8420(19) 0.036 Uiso d D 1 . . H H1B 0.577(4) 0.252(4) 0.8364(18) 0.036 Uiso d D 1 . . H H2A 0.540(4) 0.304(3) 1.109(2) 0.036 Uiso d D 1 . . H H2B 0.339(4) 0.239(4) 1.071(2) 0.036 Uiso d D 1 . . H H3A 0.121(3) -0.157(4) 0.936(2) 0.036 Uiso d D 1 . . H H3B 0.222(4) -0.015(4) 0.8674(16) 0.036 Uiso d D 1 . . H H4A 0.854(4) 0.621(4) 1.0185(15) 0.036 Uiso d D 1 . . H H4B 0.819(4) 0.545(3) 0.9187(18) 0.036 Uiso d D 1 . . H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 C1 0.0243(11) 0.0238(10) 0.0227(10) 0.0063(9) -0.0005(8) 0.0025(8) C2 0.0254(11) 0.0200(10) 0.0252(10) 0.0057(9) -0.0013(9) 0.0012(8) C3 0.0234(11) 0.0242(11) 0.0225(10) 0.0064(9) 0.0005(8) 0.0020(8) C4 0.0256(12) 0.0290(11) 0.0301(11) 0.0092(9) 0.0015(9) 0.0091(9) C5 0.0387(14) 0.0182(10) 0.0387(12) 0.0095(10) -0.0005(11) 0.0009(9) C6 0.0343(13) 0.0247(11) 0.0283(11) 0.0084(10) -0.0016(10) -0.0053(8) C7 0.0265(12) 0.0334(12) 0.0261(11) 0.0052(10) -0.0003(9) 0.0004(9) O1 0.0390(11) 0.0545(12) 0.0377(9) 0.0231(9) 0.0038(8) 0.0196(8) O2 0.0283(9) 0.0295(8) 0.0276(8) 0.0034(7) 0.0025(7) -0.0023(6) O3 0.0568(13) 0.0339(9) 0.0229(8) -0.0043(9) -0.0022(8) -0.0050(7) O4 0.0582(13) 0.0291(9) 0.0278(8) 0.0058(9) 0.0037(8) -0.0083(7) O5 0.0675(14) 0.0458(11) 0.0217(8) 0.0155(10) 0.0049(8) 0.0043(7) O6 0.0637(14) 0.0354(10) 0.0351(9) 0.0171(10) 0.0081(9) 0.0148(7) OW1 0.0306(9) 0.0335(9) 0.0317(8) 0.0130(8) 0.0021(7) 0.0023(7) OW2 0.0317(10) 0.0322(9) 0.0490(10) 0.0132(8) -0.0053(8) -0.0143(8) OW3 0.0268(9) 0.0374(10) 0.0413(9) 0.0021(8) -0.0092(8) 0.0139(8) OW4 0.0344(10) 0.0301(9) 0.0315(8) 0.0067(8) 0.0005(7) -0.0037(7) S1 0.0267(3) 0.0267(3) 0.0189(3) 0.0047(2) -0.0018(2) 0.0008(2) Cu1 0.0228(2) 0.0199(2) 0.0276(2) 0.00665(16) -0.00385(15) -0.00162(14) 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' 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' Cu Cu 0.3201 1.2651 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 C1 C6 . . 120.6(2) ? C2 C1 S1 . . 118.77(17) ? C6 C1 S1 . . 120.64(17) ? C1 C2 C3 . . 119.9(2) ? C1 C2 H2 . . 120.0 ? C3 C2 H2 . . 120.0 ? C2 C3 C4 . . 119.39(19) ? C2 C3 C7 . . 120.5(2) ? C4 C3 C7 . . 120.11(19) ? O6 C4 C5 . . 117.6(2) ? O6 C4 C3 . . 122.5(2) ? C5 C4 C3 . . 119.9(2) ? C6 C5 C4 . . 120.3(2) ? C6 C5 H5 . . 119.8 ? C4 C5 H5 . . 119.8 ? C5 C6 C1 . . 119.9(2) ? C5 C6 H6 . . 120.1 ? C1 C6 H6 . . 120.1 ? O5 C7 O4 . . 123.6(2) yes O5 C7 C3 . . 123.0(2) ? O4 C7 C3 . . 113.37(19) ? C7 O4 H4 . . 109.5 ? C4 O6 H6A . . 109.5 ? Cu1 OW1 H1A . . 117.9(18) ? Cu1 OW1 H1B . . 105.7(19) ? H1A OW1 H1B . . 102(3) ? Cu1 OW2 H2A . . 116(2) ? Cu1 OW2 H2B . . 122.3(19) ? H2A OW2 H2B . . 106(3) ? Cu1 OW3 H3A . . 127.8(19) ? Cu1 OW3 H3B . . 128.5(19) ? H3A OW3 H3B . . 104(3) ? H4A OW4 H4B . . 105(3) ? O2 S1 O3 . . 111.03(11) yes O2 S1 O1 . . 110.55(11) yes O3 S1 O1 . . 113.44(13) yes O2 S1 C1 . . 108.60(10) ? O3 S1 C1 . . 106.18(10) ? O1 S1 C1 . . 106.73(11) ? OW2 Cu1 OW2 2_657 . 180.0 ? OW2 Cu1 OW3 2_657 . 89.33(8) ? OW2 Cu1 OW3 . . 90.67(8) yes OW2 Cu1 OW3 2_657 2_657 90.67(8) ? OW2 Cu1 OW3 . 2_657 89.33(8) ? OW3 Cu1 OW3 . 2_657 180.0 ? OW2 Cu1 OW1 2_657 . 87.81(7) ? OW2 Cu1 OW1 . . 92.19(7) yes OW3 Cu1 OW1 . . 89.13(7) yes OW3 Cu1 OW1 2_657 . 90.87(7) ? OW2 Cu1 OW1 2_657 2_657 92.19(7) ? OW2 Cu1 OW1 . 2_657 87.81(7) ? OW3 Cu1 OW1 . 2_657 90.87(7) ? OW3 Cu1 OW1 2_657 2_657 89.13(7) ? OW1 Cu1 OW1 . 2_657 180.0 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 C2 . 1.379(3) ? C1 C6 . 1.397(3) ? C1 S1 . 1.763(2) ? C2 C3 . 1.397(3) ? C2 H2 . 0.930 ? C3 C4 . 1.403(3) ? C3 C7 . 1.482(3) ? C4 O6 . 1.340(3) yes C4 C5 . 1.394(3) ? C5 C6 . 1.374(3) ? C5 H5 . 0.930 ? C6 H6 . 0.930 ? C7 O5 . 1.221(3) yes C7 O4 . 1.310(3) yes O1 S1 . 1.462(2) yes O2 S1 . 1.4600(17) yes O3 S1 . 1.4608(18) yes O4 H4 . 0.820 ? O6 H6A . 0.820 ? OW1 Cu1 . 2.4175(18) yes OW1 H1A . 0.888(18) ? OW1 H1B . 0.884(18) ? OW2 Cu1 . 1.9527(18) yes OW2 H2A . 0.876(18) ? OW2 H2B . 0.873(17) ? OW3 Cu1 . 1.9596(18) yes OW3 H3A . 0.879(18) ? OW3 H3B . 0.871(17) ? OW4 H4A . 0.882(17) ? OW4 H4B . 0.879(18) ? Cu1 OW2 2_657 1.9527(18) ? Cu1 OW3 2_657 1.9596(18) ? Cu1 OW1 2_657 2.4175(18) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA OW1 H1A O2 1_655 0.888(18) 1.890(18) 2.774(2) 173(3) OW1 H1B O1 . 0.884(18) 1.965(18) 2.824(3) 164(3) OW2 H2A O3 2_667 0.876(18) 1.902(18) 2.777(3) 177(3) OW2 H2B OW4 2_667 0.873(17) 1.880(18) 2.752(3) 177(3) OW3 H3A OW4 1_445 0.879(18) 1.790(18) 2.668(3) 177(3) OW3 H3B O1 . 0.871(17) 1.953(18) 2.748(3) 151(3) OW4 H4A O3 2_667 0.882(17) 1.898(18) 2.770(3) 169(3) OW4 H4B OW1 . 0.879(18) 1.950(19) 2.794(3) 160(3) O4 H4 O2 2_556 0.82 1.96 2.726(2) 154 O6 H6A O5 . 0.82 1.91 2.627(3) 146 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 C6 C1 C2 C3 0.7(4) S1 C1 C2 C3 -179.52(17) C1 C2 C3 C4 0.8(3) C1 C2 C3 C7 -179.2(2) C2 C3 C4 O6 178.5(2) C7 C3 C4 O6 -1.5(4) C2 C3 C4 C5 -1.4(4) C7 C3 C4 C5 178.6(2) O6 C4 C5 C6 -179.3(2) C3 C4 C5 C6 0.6(4) C4 C5 C6 C1 0.8(4) C2 C1 C6 C5 -1.5(4) S1 C1 C6 C5 178.72(19) C2 C3 C7 O5 -179.5(2) C4 C3 C7 O5 0.5(4) C2 C3 C7 O4 0.3(3) C4 C3 C7 O4 -179.7(2) C2 C1 S1 O2 -64.7(2) C6 C1 S1 O2 115.0(2) C2 C1 S1 O3 175.79(19) C6 C1 S1 O3 -4.4(2) C2 C1 S1 O1 54.5(2) C6 C1 S1 O1 -125.7(2) loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 168308669