Structure, stability and photocatalytic H2 production by Cr-, Mn-, Fe-, Co-, and Ni-substituted decaniobate clusters.
Son, Jung-Ho; Wang, Jiarui; Casey, William H.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 17928–17933; doi:10.1039/c4dt02020k

data_7031894
_publ_section_title
;
 Structure, stability and photocatalytic H2 production by Cr-, Mn-, Fe-,
 Co-, and Ni-substituted decaniobate clusters.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17928
_journal_page_last               17933
_journal_paper_doi               10.1039/c4dt02020k
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'Mn Nb9 O28 8(C4 H12 N) 29(H2 O)'
_chemical_formula_sum            'C33 H60 Mn N8 Nb9 O57'
_chemical_formula_weight         2372.02
_chemical_name_common            'Tetramethylammonium nonaniobomanganate'
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 129.353(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.846(6)
_cell_length_b                   13.767(4)
_cell_length_c                   17.970(5)
_cell_measurement_reflns_used    6920
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.79
_cell_volume                     4370(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.996
_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_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_av_unetI/netI     0.0138
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23936
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.543
_diffrn_reflns_theta_min         2.795
_exptl_absorpt_coefficient_mu    1.374
_exptl_absorpt_correction_T_max  0.7426
_exptl_absorpt_correction_T_min  0.5855
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2003)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.803
_exptl_crystal_description       block
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.447
_exptl_crystal_size_mid          0.423
_exptl_crystal_size_min          0.236
_refine_diff_density_max         0.928
_refine_diff_density_min         -1.207
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.242
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         5199
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.242
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+53.9487P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1285
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5048
_reflns_number_total             5199
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt02020k2.cif
_cod_data_source_block           TMA-MnNb9
_cod_depositor_comments
'Adding full bibliography for 7031894--7031896.cif.'
_cod_database_code               7031894
_shelx_estimated_absorpt_t_min   0.579
_shelx_estimated_absorpt_t_max   0.738