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_2108902
_publ_section_title
;
 Oxonium <i>trans</i>-bis(oxalato)rhodate and related sodium salts: a rare
 example of crystalline complex acid
;
_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 H8 Na O12 Rh'
_chemical_formula_sum            'C4 H8 Na O12 Rh'
_chemical_formula_weight         374.00
_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
_audit_creation_date             2021-05-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                97.7960(10)
_cell_angle_beta                 92.0990(10)
_cell_angle_gamma                112.1130(10)
_cell_formula_units_Z            1
_cell_length_a                   5.2554(2)
_cell_length_b                   6.4584(2)
_cell_length_c                   8.2102(2)
_cell_measurement_reflns_used    5321
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.22
_cell_measurement_theta_min      3.93
_cell_volume                     254.612(14)
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            5308
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.217
_diffrn_reflns_theta_min         3.929
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.786
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6330
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0452 before and 0.0317 after correction. The Ratio of minimum to maximum transmission is 0.8480. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.439
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             184
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.671
_refine_diff_density_min         -1.283
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     85
_refine_ls_number_reflns         1912
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0157
_refine_ls_R_factor_gt           0.0156
_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^)+(0.0172P)^2^+0.1339P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0416
_refine_ls_wR_factor_ref         0.0420
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1909
_reflns_number_total             1912
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yh5016sup1.cif
_cod_data_source_block           NaRh-1
_cod_database_code               2108902
_publcif_datablock.id            {c5f56b33-ec02-4492-8bc1-214dcdc4e2cb}
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.717
_shelx_estimated_absorpt_t_min   0.574
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2.a Riding coordinates:
 O1W(H1WA,H1WB), O3W(H3WA,H3WB)
;
_shelx_res_checksum              86582
_shelx_hkl_checksum              94753
_olex2_submission_special_instructions 'No special instructions were received'
_cod_database_fobs_code 2108902