Crystal structures of two new divalent transition-metal salts of carboxybenzenesulfonate anions
Bettinger, Reuben T.; Squattrito, Philip J.; Aulakh, Darpandeep; Gianopoulos, Christopher G.; Acta Crystallographica Section E 78 (2022) 961–965; doi:10.1107/S2056989022008295

data_2244155
_publ_section_title
;
 Crystal structures of two new divalent transition-metal salts of
 carboxybenzenesulfonate anions
;
_journal_coeditor_code           MW2190
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              961
_journal_page_last               965
_journal_paper_doi               10.1107/S2056989022008295
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac          '[Ni (H2 O1)6] (C7 H5 O6 S)2, 2H2 O'
_chemical_formula_moiety         'H12 Ni O6 2+, 2(C7 H5 O6 S -), 2(H2 O)'
_chemical_formula_sum            'C14 H26 Ni O20 S2'
_chemical_formula_weight         637.18
_chemical_name_common
;
Hexaaquanickel(II) bis(3-carboxy-4-hydroxybenzenesulfonate) dihydrate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                74.1712(14)
_cell_angle_beta                 88.6035(14)
_cell_angle_gamma                77.9200(13)
_cell_formula_units_Z            1
_cell_length_a                   6.5986(7)
_cell_length_b                   7.4183(8)
_cell_length_c                   13.2847(14)
_cell_measurement_reflns_used    4943
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.92
_cell_volume                     611.41(11)
_computing_cell_refinement       'SAINT (Bruker, 2015)'
_computing_data_collection       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2015)'
_computing_molecular_graphics    'CrystalMaker (Palmer, 2014)'
_computing_structure_refinement  '<i>SHELXL2018/3</i> (Sheldrick, 2015b)'
_computing_structure_solution    '<i>SHELXT2014/5</i> (Sheldrick, 2015a)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Duo with APEXII CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0193
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8656
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.403
_diffrn_reflns_theta_min         2.919
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.057
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Krause et al., 2015)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_description       block
_exptl_crystal_F_000             330
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.413
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3047
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0228
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0284P)^2^+0.2223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0578
_refine_ls_wR_factor_ref         0.0592
_reflns_number_gt                2779
_reflns_number_total             3047
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            mw2190sup1.cif
_cod_data_source_block           I
_cod_database_code               2244155
_shelx_hkl_checksum              80308
_shelx_res_checksum              43234
_cod_database_fobs_code 2244155