Two Rh(III)-substituted polyoxoniobates and their base-induced transformation: [H2RhNb9O28](6-) and [Rh2(OH)4Nb10O30](8.).
Son, Jung-Ho; Casey, Willam H.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 20330–20333; doi:10.1039/c5dt03797b

data_7037198
_publ_section_title
;
 Two Rh(III)-substituted polyoxoniobates and their base-induced
 transformation: [H2RhNb9O28](6-) and [Rh2(OH)4Nb10O30](8.).
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              20330
_journal_page_last               20333
_journal_paper_doi               10.1039/c5dt03797b
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'H4 Nb10 O34 Rh2, 8(C4 H12 N), 18(H2 O)'
_chemical_formula_sum            'C32 H136 N8 Nb10 O52 Rh2'
_chemical_formula_weight         2600.40
_chemical_name_common            'tetramethylammonium bis-rhodium decaniobate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-08-07 deposited with the CCDC.
2015-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.748(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.0911(15)
_cell_length_b                   15.379(2)
_cell_length_c                   24.327(3)
_cell_measurement_reflns_used    9151
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.75
_cell_volume                     4140.6(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            44814
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.541
_diffrn_reflns_theta_min         2.844
_exptl_absorpt_coefficient_mu    1.815
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2003)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.086
_exptl_crystal_description       block
_exptl_crystal_F_000             2600
_exptl_crystal_size_max          0.443
_exptl_crystal_size_mid          0.249
_exptl_crystal_size_min          0.244
_refine_diff_density_max         1.628
_refine_diff_density_min         -1.394
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         9483
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0203
_refine_ls_R_factor_gt           0.0190
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0152P)^2^+6.8050P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0454
_refine_ls_wR_factor_ref         0.0460
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9099
_reflns_number_total             9483
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03797b2.cif
_cod_data_source_block           TMA-Rh2Nb10
_cod_depositor_comments
'Adding full bibliography for 7037197--7037198.cif.'
_cod_original_cell_volume        4140.6(10)
_cod_database_code               7037198
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.500
_shelx_estimated_absorpt_t_max   0.666
_shelx_res_checksum              44653