New heteropolyniobates based on a bicapped Keggin-type {VNb14} cluster with selective adsorption and photocatalytic properties
Huang, Peng; Zhou, En-Long; Wang, Xin-Long; Sun, Chun-Yi; Wang, Hai-Ning; Xing, Yan; Shao, Kui-Zhan; Su, Zhong-Min; CrystEngComm 16 (2014) 9582–; doi:10.1039/C4CE00960F

data_7216732
_publ_section_title
;
 New heteropolyniobates based on a bicapped Keggin-type {VNb14} cluster
 with selective adsorption and photocatalytic properties
;
_journal_issue                   41
_journal_name_full               CrystEngComm
_journal_page_first              9582
_journal_paper_doi               10.1039/C4CE00960F
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C10 H64 N12 Na Nb14 O60 V'
_chemical_formula_weight         2687.40
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.812(5)
_cell_angle_beta                 78.200(5)
_cell_angle_gamma                66.431(5)
_cell_formula_units_Z            2
_cell_length_a                   13.041(5)
_cell_length_b                   14.260(5)
_cell_length_c                   20.450(5)
_cell_measurement_reflns_used    17006
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.72
_cell_volume                     3376.4(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker SMART Apex II CCD Detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17006
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    2.540
_exptl_absorpt_correction_T_max  0.5693
_exptl_absorpt_correction_T_min  0.5263
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick (2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.643
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_platon_squeeze_details
;
;
_refine_diff_density_max         2.234
_refine_diff_density_min         -1.620
_refine_diff_density_rms         0.193
_refine_ls_extinction_coef       0.00012(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     911
_refine_ls_number_reflns         11691
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0801P)^2^+8.6730P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1298
_refine_ls_wR_factor_ref         0.1405
_reflns_number_gt                8720
_reflns_number_total             11691
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce00960f2.cif
_cod_data_source_block           mm
_cod_depositor_comments
'Adding full bibliography for 7216732--7216733.cif.'
_cod_database_code               7216732