Synthesis, structure, and photocatalytic hydrogen evolution of a trimeric Nb/W addendum cluster
Wang, Haiying; Hou, Lili; Li, Chen; Zhang, Dongdi; Ma, Pengtao; Wang, Jingping; Niu, Jingyang; RSC Adv. 7 (2017) 36416–; doi:10.1039/C7RA06291E

data_7228728
_publ_section_title
;
 Synthesis, structure, and photocatalytic hydrogen evolution of a trimeric
 Nb/W addendum cluster
;
_journal_issue                   58
_journal_name_full               'RSC Adv.'
_journal_page_first              36416
_journal_paper_doi               10.1039/C7RA06291E
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         '0.33(Cs36 Nb27 O372 Si9 W84), 6(O)'
_chemical_formula_sum            'Cs12 H20 Nb9 O130 Si3 W28'
_chemical_formula_weight         9763.34
_space_group_crystal_system      trigonal
_space_group_IT_number           160
_space_group_name_Hall           'R 3 -2"'
_space_group_name_H-M_alt        'R 3 m :H'
_audit_creation_date             2015-12-29
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   30.4555(13)
_cell_length_b                   30.4555(13)
_cell_length_c                   15.9433(13)
_cell_measurement_reflns_used    8059
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.97
_cell_measurement_theta_min      2.41
_cell_volume                     12806.8(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0913
_diffrn_reflns_av_unetI/netI     0.0843
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21257
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.098
_diffrn_reflns_theta_max         25.098
_diffrn_reflns_theta_min         2.004
_exptl_absorpt_coefficient_mu    21.980
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.1948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1788 before and 0.0737 after correction.
The Ratio of minimum to maximum transmission is 0.2612.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.798
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             12609
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.625
_refine_diff_density_min         -3.069
_refine_diff_density_rms         0.351
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.535(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         5324
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0591P)^2^+171.4812P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1213
_reflns_Friedel_coverage         0.994
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4772
_reflns_number_total             5324
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra06291e1.cif
_cod_data_source_block           njy1
_cod_depositor_comments
;
 Updating space group information.

 Antanas Vaitkus,
 2018-07-04
;
_cod_original_cell_volume        12806.8(15)
_cod_database_code               7228728
_shelx_estimated_absorpt_t_max   0.091
_shelx_estimated_absorpt_t_min   0.045
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.465(19) 0.535(19)
2. Others
 Fixed Sof: Cs4(0.2) Cs5(0.13333) O1W(0.25) O2W(0.25) O3W(0.25) O6W(0.25)
;
_shelx_res_checksum              1012
_shelx_hkl_checksum              11714
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'