Assembly of Fe-substituted Dawson-type nanoscale selenotungstate clusters with photocatalytic H2 evolution activity
Wei-Chao Chen; Chao Qin; Xin-Long Wang; Yang-Guang Li; Hong-Ying Zang; Yan-Qing Jiao; Peng Huang; Kui-Zhan Shao; Zhong-Min Su; En-Bo Wang; Chem.Commun. 50 (2014) 13265–; doi:10.1039/C4cc06447J

data_7115857
_publ_section_title
;
 Assembly of Fe-substituted Dawson-type nanoscale selenotungstate clusters
 with photocatalytic H2 evolution activity
;
_journal_name_full               Chem.Commun.
_journal_page_first              13265
_journal_paper_doi               10.1039/C4cc06447J
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'Fe10 H146 N9 Na19 O286 Se8 W62'
_chemical_formula_weight         17874.95
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.5020(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.6237(10)
_cell_length_b                   25.6225(15)
_cell_length_c                   37.073(2)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.9553
_cell_measurement_theta_min      2.1873
_cell_volume                     16735.1(16)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 0.01
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX area-detector diffractometer'
_diffrn_measurement_method       '\f and \w scan'
_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  0.0701
_diffrn_reflns_av_sigmaI/netI    0.0849
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            85907
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.83
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    22.620
_exptl_absorpt_correction_T_max  0.0788
_exptl_absorpt_correction_T_min  0.0707
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             15652
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_platon_squeeze_details
;
;
_refine_diff_density_max         2.525
_refine_diff_density_min         -4.454
_refine_diff_density_rms         0.305
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1632
_refine_ls_number_reflns         29399
_refine_ls_number_restraints     203
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0455
_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^)+(0.0557P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1214
_reflns_number_gt                18170
_reflns_number_total             29399
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc06447j2.cif
_cod_data_source_block           1a
_cod_original_cell_volume        16735.0(17)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'H146 Fe10 N9 Na19 O286 Se8 W62'
_cod_database_code               7115857