#------------------------------------------------------------------------------
#$Date: 2022-01-01 06:16:20 +0200 (Sat, 01 Jan 2022) $
#$Revision: 271664 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/10/89/2108903.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_2108903
loop_
_publ_author_name
'Garkul, Ilia'
'Zadesenets, Andrey'
'Filatov, Evgeny'
'Baidina, Iraida'
'Tkachev, Sergey'
'Samsonenko, Denis'
'Korenev, Sergey'
_publ_section_title
;
 Oxonium trans-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_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                95.557(3)
_cell_angle_beta                 98.352(3)
_cell_angle_gamma                98.065(3)
_cell_formula_units_Z            2
_cell_length_a                   6.2055(3)
_cell_length_b                   7.8091(3)
_cell_length_c                   10.7762(4)
_cell_measurement_reflns_used    2269
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.38
_cell_measurement_theta_min      2.63
_cell_volume                     507.88(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2018 (Sheldrick, 2015)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.822
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.822
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3910
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.822
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         28.957
_diffrn_reflns_theta_min         1.924
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.791
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.446
_exptl_crystal_description       plate
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2214
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0217P)²+0.0121P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0570
_refine_ls_wR_factor_ref         0.0591
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2024
_reflns_number_total             2214
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            yh5016sup1.cif
_cod_data_source_block           NaRh-2
_cod_database_code               2108903
_publcif_datablock.id            {181e1b82-4d9a-40b1-87c8-764a472aabf2}
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.727
_shelx_estimated_absorpt_t_max   0.916
_publcif_info_exptl_table_max_cols 5
_publcif_info_exptl_table_use_headnotes n
_publcif_funding_html
;
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.25557(4) 0.69752(3) 0.76733(2) 0.01553(9) Uani 1 1 d . . . . .
Na1 Na 0.8339(2) 0.79886(18) 0.42497(11) 0.0340(3) Uani 1 1 d . . . . .
O1M O 0.0411(3) 0.4743(3) 0.69957(18) 0.0190(4) Uani 1 1 d D . . . .
H11M H 0.001(5) 0.431(4) 0.7628(18) 0.023 Uiso 1 1 d D U . . .
H12M H -0.063(3) 0.512(4) 0.656(2) 0.023 Uiso 1 1 d D U . . .
O2M O 0.4769(4) 0.9138(3) 0.8244(2) 0.0381(6) Uani 1 1 d D . . . .
H21M H 0.451(6) 1.015(2) 0.820(3) 0.046 Uiso 1 1 d D U . . .
H22M H 0.564(5) 0.908(4) 0.890(2) 0.046 Uiso 1 1 d D U . . .
O3M O 1.1219(4) 0.9878(3) 0.37673(19) 0.0278(5) Uani 1 1 d D . . . .
H31M H 1.102(5) 1.019(4) 0.3037(15) 0.033 Uiso 1 1 d D U . . .
H32M H 1.226(4) 0.930(4) 0.379(3) 0.033 Uiso 1 1 d D U . . .
O4M O 0.6437(4) 0.7806(3) 0.19877(19) 0.0282(5) Uani 1 1 d D . . . .
H41M H 0.538(4) 0.697(3) 0.192(3) 0.034 Uiso 1 1 d D U . . .
H42M H 0.709(4) 0.759(3) 0.136(2) 0.034 Uiso 1 1 d D U . . .
O1 O 0.2794(4) 0.6357(3) 0.94445(17) 0.0235(5) Uani 1 1 d . . . . .
O2 O 0.0049(3) 0.8111(3) 0.81852(17) 0.0206(5) Uani 1 1 d . . . . .
O3 O -0.1834(4) 0.8354(3) 0.97744(18) 0.0262(5) Uani 1 1 d . . . . .
O4 O 0.1342(4) 0.6815(3) 1.11812(18) 0.0338(6) Uani 1 1 d . . . . .
O5 O 0.5086(3) 0.5867(3) 0.71829(17) 0.0199(4) Uani 1 1 d . . . . .
O6 O 0.2343(3) 0.7660(3) 0.59134(17) 0.0209(5) Uani 1 1 d . . . . .
O7 O 0.4487(4) 0.7911(3) 0.44324(17) 0.0232(5) Uani 1 1 d . . . . .
O8 O 0.7266(3) 0.6032(2) 0.57151(17) 0.0182(4) Uani 1 1 d . . . . .
C1 C 0.1396(5) 0.6932(4) 1.0064(3) 0.0206(7) Uani 1 1 d . . . . .
C2 C -0.0311(5) 0.7882(4) 0.9304(3) 0.0189(6) Uani 1 1 d . . . . .
C3 C 0.5640(5) 0.6369(4) 0.6165(2) 0.0168(6) Uani 1 1 d . . . . .
C4 C 0.4051(5) 0.7423(4) 0.5420(3) 0.0179(6) Uani 1 1 d . . . . .
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'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2M Rh1 O1M 176.23(9) . . ?
O2M Rh1 O2 93.06(10) . . ?
O2M Rh1 O5 86.17(10) . . ?
O2M Rh1 O6 87.82(10) . . ?
O1 Rh1 O1M 91.82(8) . . ?
O1 Rh1 O2M 90.84(10) . . ?
O1 Rh1 O2 82.14(8) . . ?
O1 Rh1 O5 97.47(8) . . ?
O1 Rh1 O6 178.53(8) . . ?
O2 Rh1 O1M 89.95(9) . . ?
O5 Rh1 O1M 90.84(8) . . ?
O5 Rh1 O2 179.14(8) . . ?
O5 Rh1 O6 83.03(8) . . ?
O6 Rh1 O1M 89.54(8) . . ?
O6 Rh1 O2 97.34(8) . . ?
Na1 Na1 H32M 53.7(6) 2_776 . ?
O1M Na1 Na1 128.76(8) 2_666 2_776 ?
O1M Na1 H32M 77.3(6) 2_666 . ?
O1M Na1 O6 79.17(7) 2_666 1_655 ?
O1M Na1 C3 104.19(8) 2_666 . ?
O1M Na1 C4 118.98(8) 2_666 . ?
O3M Na1 Na1 39.58(6) 2_776 2_776 ?
O3M Na1 Na1 44.46(6) . 2_776 ?
O3M Na1 O1M 91.83(8) . 2_666 ?
O3M Na1 O1M 149.32(9) 2_776 2_666 ?
O3M Na1 O3M 84.04(9) . 2_776 ?
O3M Na1 H32M 17.9(4) . . ?
O3M Na1 H32M 91.4(6) 2_776 . ?
O3M Na1 O4M 88.89(8) . . ?
O3M Na1 O6 70.68(7) 2_776 1_655 ?
O3M Na1 O6 71.42(8) . 1_655 ?
O3M Na1 O7 139.07(10) . . ?
O3M Na1 O8 144.52(9) . . ?
O3M Na1 C3 70.27(8) 2_776 . ?
O3M Na1 C3 151.77(9) . . ?
O3M Na1 C4 71.21(8) 2_776 . ?
O3M Na1 C4 149.00(9) . . ?
O4M Na1 Na1 119.52(8) . 2_776 ?
O4M Na1 O1M 74.20(7) . 2_666 ?
O4M Na1 O3M 135.83(9) . 2_776 ?
O4M Na1 H32M 94.9(6) . . ?
O4M Na1 O6 146.23(9) . 1_655 ?
O4M Na1 C3 117.58(9) . . ?
O4M Na1 C4 95.93(9) . . ?
O6 Na1 Na1 64.08(6) 1_655 2_776 ?
O6 Na1 H32M 58.7(5) 1_655 . ?
O6 Na1 C3 88.69(7) 1_655 . ?
O6 Na1 C4 115.20(8) 1_655 . ?
O7 Na1 Na1 112.09(8) . 2_776 ?
O7 Na1 O1M 119.14(9) . 2_666 ?
O7 Na1 O3M 81.18(8) . 2_776 ?
O7 Na1 H32M 156.9(4) . . ?
O7 Na1 O4M 76.13(8) . . ?
O7 Na1 O6 136.19(8) . 1_655 ?
O7 Na1 C3 49.66(7) . . ?
O7 Na1 C4 21.24(7) . . ?
O8 Na1 Na1 113.47(7) . 2_776 ?
O8 Na1 O1M 86.35(7) . 2_666 ?
O8 Na1 O3M 79.91(8) . 2_776 ?
O8 Na1 H32M 131.4(5) . . ?
O8 Na1 O4M 124.22(9) . . ?
O8 Na1 O6 73.45(7) . 1_655 ?
O8 Na1 O7 68.98(8) . . ?
O8 Na1 C3 21.45(7) . . ?
O8 Na1 C4 49.70(7) . . ?
C3 Na1 Na1 109.07(7) . 2_776 ?
C3 Na1 H32M 146.9(6) . . ?
C3 Na1 C4 29.08(7) . . ?
C4 Na1 Na1 108.80(7) . 2_776 ?
C4 Na1 H32M 162.4(6) . . ?
Rh1 O1M Na1 122.09(10) . 2_666 ?
Rh1 O1M H11M 107(2) . . ?
Rh1 O1M H12M 103(2) . . ?
Na1 O1M H11M 102(2) 2_666 . ?
Na1 O1M H12M 112(2) 2_666 . ?
H11M O1M H12M 112(2) . . ?
Rh1 O2M H21M 125(2) . . ?
Rh1 O2M H22M 114(2) . . ?
H21M O2M H22M 111(2) . . ?
Na1 O3M Na1 95.96(9) . 2_776 ?
Na1 O3M H31M 115(2) . . ?
Na1 O3M H31M 122(2) 2_776 . ?
Na1 O3M H32M 104(2) . . ?
Na1 O3M H32M 111(2) 2_776 . ?
H31M O3M H32M 106(2) . . ?
Na1 O4M H41M 104(2) . . ?
Na1 O4M H42M 122(2) . . ?
H41M O4M H42M 106(2) . . ?
C1 O1 Rh1 113.96(18) . . ?
C2 O2 Rh1 113.72(18) . . ?
C3 O5 Rh1 111.54(17) . . ?
Rh1 O6 Na1 126.56(9) . 1_455 ?
C4 O6 Rh1 111.93(17) . . ?
C4 O6 Na1 118.36(16) . 1_455 ?
C4 O7 Na1 112.74(19) . . ?
C3 O8 Na1 113.01(18) . . ?
O1 C1 C2 115.4(2) . . ?
O4 C1 O1 125.0(3) . . ?
O4 C1 C2 119.6(3) . . ?
O2 C2 C1 114.5(3) . . ?
O3 C2 O2 124.8(3) . . ?
O3 C2 C1 120.7(2) . . ?
O5 C3 Na1 162.3(2) . . ?
O5 C3 C4 116.3(2) . . ?
O8 C3 Na1 45.53(14) . . ?
O8 C3 O5 125.3(3) . . ?
O8 C3 C4 118.4(2) . . ?
C4 C3 Na1 75.69(16) . . ?
O6 C4 Na1 163.7(2) . . ?
O6 C4 C3 115.1(2) . . ?
O7 C4 Na1 46.01(15) . . ?
O7 C4 O6 126.0(3) . . ?
O7 C4 C3 118.9(3) . . ?
C3 C4 Na1 75.23(16) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 O1M 2.040(2) . yes
Rh1 O2M 2.005(2) . yes
Rh1 O1 2.0037(19) . yes
Rh1 O2 2.013(2) . yes
Rh1 O5 2.007(2) . yes
Rh1 O6 2.0109(18) . yes
Na1 Na1 3.601(3) 2_776 ?
Na1 O1M 2.677(2) 2_666 yes
Na1 O3M 2.307(3) . yes
Na1 O3M 2.536(2) 2_776 yes
Na1 H32M 2.64(3) . ?
Na1 O4M 2.531(3) . yes
Na1 O6 2.903(2) 1_655 yes
Na1 O7 2.419(3) . yes
Na1 O8 2.400(2) . yes
Na1 C3 3.095(3) . ?
Na1 C4 3.101(3) . ?
O1M H11M 0.843(10) . ?
O1M H12M 0.843(10) . ?
O2M H21M 0.833(9) . ?
O2M H22M 0.836(10) . ?
O3M H31M 0.844(10) . ?
O3M H32M 0.838(10) . ?
O4M H41M 0.849(10) . ?
O4M H42M 0.852(10) . ?
O1 C1 1.273(4) . ?
O2 C2 1.283(3) . ?
O3 C2 1.219(4) . ?
O4 C1 1.221(3) . ?
O5 C3 1.277(3) . ?
O6 C4 1.281(3) . ?
O7 C4 1.219(3) . ?
O8 C3 1.230(3) . ?
C1 C2 1.558(4) . ?
C3 C4 1.556(4) . ?
loop_
_publcif_info_tables.block_id
_publcif_info_tables.reference_item
{7243f9a5-1d7c-4548-ab8d-f8cd242d8136} '_publcif_info_datablock.publ_exptl'
{7243f9a5-1d7c-4548-ab8d-f8cd242d8136} '_geom_hbond_atom_site_label_D'
{181e1b82-4d9a-40b1-87c8-764a472aabf2} '_geom_bond_atom_site_label_1'
loop_
_publcif_info_cif.paper_type
CB
loop_
_publcif_info_datablock.id
_publcif_info_datablock.publ_exptl
_publcif_info_datablock.publ_geom
_publcif_info_datablock.structure
{7243f9a5-1d7c-4548-ab8d-f8cd242d8136} y y y
{ffbded9b-fb91-462b-a3ca-93c3f3fc7256} y y y
{c5f56b33-ec02-4492-8bc1-214dcdc4e2cb} y y y
{181e1b82-4d9a-40b1-87c8-764a472aabf2} y y y
loop_
_publcif_info_exptl_table_extra_item
sin_theta_over_lambda_max
loop_
_publcif_info_exptl_table_header_item
?

_cod_database_fobs_code 2108903
