Oxonium <i>trans</i>-bis(oxalato)rhodate and related sodium salts: a rare example of crystalline complex acid
Garkul, Ilia; Zadesenets, Andrey; Filatov, Evgeny; Baidina, Iraida; Tkachev, Sergey; Samsonenko, Denis; Korenev, Sergey; Acta Crystallographica Section B 77 (2021) 1048–1054; doi:10.1107/S205252062101115X

data_2108900
_publ_section_title
;
 Oxonium <i>trans</i>-bis(oxalato)rhodate and related sodium salts: a rare
 example of crystalline complex acid
;
_journal_coeditor_code           YH5016
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              1048
_journal_page_last               1054
_journal_paper_doi               10.1107/S205252062101115X
_journal_volume                  77
_journal_year                    2021
_chemical_formula_moiety         'C4 H4 O10 Rh, 3(H2 O), (H5 O2)'
_chemical_formula_sum            'C4 H15 O15 Rh'
_chemical_formula_weight         406.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-11-03 # Formatted by IUCr publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 99.572(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.2131(8)
_cell_length_b                   13.0362(6)
_cell_length_c                   6.3015(3)
_cell_measurement_reflns_used    8655
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.48
_cell_measurement_theta_min      2.55
_cell_volume                     1313.32(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 PIXEL
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Incoatec HELIOS multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7956
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.494
_diffrn_reflns_theta_min         2.016
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    1.381
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6314
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0746 before and 0.0555 after correction. The Ratio of minimum to maximum transmission is 0.8463. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.054
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         1996
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0277
_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^)+(0.0165P)^2^+4.4254P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0618
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1774
_reflns_number_total             1996
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yh5016sup1.cif
_cod_data_source_block           HRh
_cod_database_code               2108900
_publcif_datablock.id            {7243f9a5-1d7c-4548-ab8d-f8cd242d8136}
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.898
_shelx_estimated_absorpt_t_min   0.841
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups, All O(H,H,H,H,H) groups
2. Others
 Fixed Sof: H2WB(0.5) H2W(0.5) H3WA(0.5) H3WB(0.5) H4WC(0.5) H4WB(0.5) H4W(0.5)
3.a Riding coordinates:
 O1W(H2WB,H2W,H2WA)
3.b Free rotating group:
 O3W(H3WA,H3WB)
3.c Rotating group:
 O1W(H1WA,H1WB), O4W(H4WC,H4WA,H4WB,H4W)
;
_shelx_res_checksum              48470
_shelx_hkl_checksum              74578
_olex2_submission_special_instructions 'No special instructions were received'
_cod_database_fobs_code 2108900