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_2108901
_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 H11 Na2 O14 Rh'
_chemical_formula_sum            'C4 H11 Na2 O14 Rh'
_chemical_formula_weight         432.02
_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
_audit_creation_date             2021-06-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                94.20(3)
_cell_angle_beta                 99.40(3)
_cell_angle_gamma                98.10(3)
_cell_formula_units_Z            1
_cell_length_a                   5.5500(11)
_cell_length_b                   6.4400(13)
_cell_length_c                   8.5900(17)
_cell_measurement_reflns_used    3338
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.52
_cell_measurement_theta_min      3.21
_cell_volume                     298.42(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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                 CCD
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'Bruker APEXII CCD area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX diffractometer'
_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  0.0233
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3654
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.531
_diffrn_reflns_theta_min         2.415
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.585
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6611
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0409 before and 0.0312 after correction. The Ratio of minimum to maximum transmission is 0.8860. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.404
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             214
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.814
_refine_diff_density_min         -1.148
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         1984
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0172
_refine_ls_R_factor_gt           0.0170
_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^)+0.2058P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0421
_refine_ls_wR_factor_ref         0.0426
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1975
_reflns_number_total             1984
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yh5016sup1.cif
_cod_data_source_block           Na2Rh
_cod_database_code               2108901
_publcif_datablock.id            {ffbded9b-fb91-462b-a3ca-93c3f3fc7256}
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.911
_shelx_estimated_absorpt_t_min   0.742
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O2W-H2WA = O2W-H2WB
 0.84 with sigma of 0.02
 O3W-H3WA = O3W-H3WB
 0.84 with sigma of 0.02
 O1W-H1WA = O1W-H1W
 0.84 with sigma of 0.02
3. Others
 Fixed Sof: H1W(0.5)
;
_shelx_res_checksum              97735
_shelx_hkl_checksum              95863
_olex2_submission_special_instructions 'No special instructions were received'
_cod_database_fobs_code 2108901