Creation of bismuth‒tungsten oxide nanoclusters using lacunary polyoxometalates
Hanaya, Takumi; Suzuki, Kosuke; Sato, Rinta; Yamaguchi, Kazuya; Mizuno, Noritaka; Dalton Trans.  (2017) –; doi:10.1039/C7DT01587A

data_7042970
_publ_section_title
;
 Creation of bismuth--tungsten oxide nanoclusters using lacunary
 polyoxometalates
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01587A
_journal_year                    2017
_chemical_formula_sum            'C114 H255 Bi4 N7 O75 Si2 W20'
_chemical_formula_weight         7493.33
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2017-05-10 deposited with the CCDC.
2017-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.8709(2)
_cell_length_b                   33.9407(3)
_cell_length_c                   19.39360(10)
_cell_measurement_reflns_used    29900
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      24.99
_cell_measurement_theta_min      1.20
_cell_volume                     20320.2(2)
_computing_cell_refinement       HKL2000
_computing_data_collection       'Rigaku CrystalClear'
_computing_data_reduction        HKL2000
_computing_molecular_graphics    'CrystalMaker 9.2'
_computing_publication_material
'SHELXL-2014/6 (Sheldrick, 2014), WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.093
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            18469
_diffrn_reflns_point_group_measured_fraction_full 0.502
_diffrn_reflns_point_group_measured_fraction_max 0.516
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.200
_exptl_absorpt_coefficient_mu    14.800
_exptl_absorpt_correction_T_max  0.400
_exptl_absorpt_correction_T_min  0.310
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL2000 DENZO SCALEPACK'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.449
_exptl_crystal_description       plate
_exptl_crystal_F_000             13712
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.256
_refine_diff_density_min         -1.365
_refine_diff_density_rms         0.213
_refine_ls_abs_structure_details
;
No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   0.009(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     908
_refine_ls_number_reflns         18469
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0251
_refine_ls_R_factor_gt           0.0240
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0585P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0785
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    0.000
_reflns_Friedel_fraction_max     0.000
_reflns_number_gt                17095
_reflns_number_total             18469
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01587a2.cif
_cod_data_source_block           SiW10Bi4
_cod_database_code               7042970
_shelx_estimated_absorpt_t_min   0.319
_shelx_estimated_absorpt_t_max   0.319
_shelxl_version_number           2014/6
_shelx_res_checksum              88712
_platon_squeeze_void_probe_radius 1.20