Self-Assembly and Photocatalytic Properties of Polyoxoniobates: {Nb24O72}, {Nb32O96}, and {K12Nb96O288} Clusters
Peng Huang; Chao Qin; Zhong-Min Su; Yan Xing; Xin-Long Wang; Kui-Zhan Shao; Ya-Qian Lan; En-Bo Wang; Journal of the American Chemical Society 134 (2012) 14004–14010; doi:10.1021/ja303723u

data_4118535
_publ_section_title
;
 Self-Assembly and Photocatalytic Properties of Polyoxoniobates:
 {Nb24O72}, {Nb32O96}, and {K12Nb96O288} Clusters
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14004
_journal_page_last               14010
_journal_paper_doi               10.1021/ja303723u
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'H298 K12 Nb96 O395'
_chemical_formula_weight         16008.95
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            12
_cell_length_a                   39.2527(14)
_cell_length_b                   39.2527(14)
_cell_length_c                   106.905(7)
_cell_measurement_reflns_used    163466
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.86
_cell_measurement_theta_min      1.04
_cell_volume                     142649(12)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL-PLUS (Sheldrick, 1990)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1529
_diffrn_reflns_av_sigmaI/netI    0.1653
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       91
_diffrn_reflns_limit_l_min       -106
_diffrn_reflns_number            163466
_diffrn_reflns_theta_full        20.86
_diffrn_reflns_theta_max         20.86
_diffrn_reflns_theta_min         1.04
_exptl_absorpt_coefficient_mu    2.420
_exptl_absorpt_correction_T_max  0.918
_exptl_absorpt_correction_T_min  0.902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.236
_exptl_crystal_description       block
_exptl_crystal_F_000             91464
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_platon_squeeze_details
;
;
_refine_diff_density_max         1.276
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1461
_refine_ls_number_reflns         33175
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1320
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0143P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.0999
_reflns_number_gt                14511
_reflns_number_total             33175
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja303723u_si_004.cif
_cod_data_source_block           www
_cod_original_cell_volume        142648(12)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4118535