Controllable Assembly of Vanadium-Containing Polyoxoniobate-Based Three-Dimensional Organic-Inorganic Hybrid Compounds and Their Photocatalytic Properties.
Hu, Jufang; Wang, Yin; Zhang, Xinning; Chi, Yingnan; Yang, Song; Li, Jikun; Hu, Changwen; Inorganic chemistry 55 (2016) 7501–7507; doi:10.1021/acs.inorgchem.6b00823

data_4347987
_publ_section_title
;
 Controllable Assembly of Vanadium-Containing Polyoxoniobate-Based
 Three-Dimensional Organic-Inorganic Hybrid Compounds and Their
 Photocatalytic Properties.
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7501
_journal_page_last               7507
_journal_paper_doi               10.1021/acs.inorgchem.6b00823
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C30 H122 Co5 N20 Nb12 O58 P V6'
_chemical_formula_weight         3439.68
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                77.1710(10)
_cell_angle_beta                 80.038(2)
_cell_angle_gamma                63.0880(10)
_cell_formula_units_Z            1
_cell_length_a                   13.3030(11)
_cell_length_b                   14.1260(12)
_cell_length_c                   14.3554(13)
_cell_measurement_reflns_used    3246
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.962
_cell_measurement_theta_min      2.845
_cell_volume                     2337.3(3)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0793
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            11295
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.017
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.84
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.957
_exptl_absorpt_correction_T_max  0.701
_exptl_absorpt_correction_T_min  0.593
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    2.444
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1686
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_refine_diff_density_max         2.332
_refine_diff_density_min         -1.451
_refine_diff_density_rms         0.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     636
_refine_ls_number_reflns         8234
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1099
_refine_ls_R_factor_gt           0.0612
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0862P)^2^+34.6029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1588
_refine_ls_wR_factor_ref         0.1986
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4982
_reflns_number_total             8234
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00823_si_002.cif
_cod_data_source_block           2
_cod_database_code               4347987
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.593
_shelx_estimated_absorpt_t_max   0.701
_shelx_res_checksum              40624
_shelx_hkl_checksum              77856