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_7037197
_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         'Nb8.88 O28 Rh1.12, 6(C4 H12 N), 14(H2 O)'
_chemical_formula_sum            'C24 H100 N6 Nb8.88 O42 Rh1.12'
_chemical_formula_weight         2084.19
_chemical_name_common            'tetramethylammonium rhodium nonaniobate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                85.9610(10)
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_cell_angle_gamma                87.8620(10)
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_cell_length_b                   12.1932(9)
_cell_length_c                   13.3388(10)
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_cell_measurement_temperature    93(2)
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_cell_measurement_theta_min      2.57
_cell_volume                     1673.1(2)
_computing_cell_refinement       'Bruker SAINT'
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_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 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0209
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19423
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.506
_diffrn_reflns_theta_min         2.047
_exptl_absorpt_coefficient_mu    1.816
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6039
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2003)'
_exptl_crystal_colour            orange
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_exptl_crystal_description       prism
_exptl_crystal_F_000             1036
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_exptl_crystal_size_min          0.096
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_refine_ls_extinction_method     none
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_refine_ls_number_parameters     438
_refine_ls_number_reflns         7620
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0330
_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/[\s^2^(Fo^2^)+(0.0290P)^2^+6.5947P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0840
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7099
_reflns_number_total             7620
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03797b2.cif
_cod_data_source_block           TMA-RhNb9
_cod_depositor_comments
'Adding full bibliography for 7037197--7037198.cif.'
_cod_database_code               7037197
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.496
_shelx_estimated_absorpt_t_max   0.845
_shelx_res_checksum              14110