Ionothermal syntheses of three transition-metal-containing polyoxotungstate hybrids exhibiting the photocatalytic and electrocatalytic properties
Chen, Wei-Lin; Chen, Bao-Wang; Tan, Hua-Qiao; Li, Yang-Guang; Wang, Yong-Hui; Wang, En-Bo; Journal of Solid State Chemistry 183 (2010) 310–321; doi:10.1016/j.jssc.2009.11.016

data_1563728
_publ_section_title
;
 Ionothermal syntheses of three transition-metal-containing
 polyoxotungstate hybrids exhibiting the photocatalytic and
 electrocatalytic properties
;
_journal_issue                   2
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              310
_journal_page_last               321
_journal_paper_doi               10.1016/j.jssc.2009.11.016
_journal_volume                  183
_journal_year                    2010
_chemical_formula_sum            'C54 H106 Fe9 N18 Na8 O115.5 Si3 W28'
_chemical_formula_weight         8774.21
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                87.59(3)
_cell_angle_beta                 87.04(3)
_cell_angle_gamma                87.15(3)
_cell_formula_units_Z            2
_cell_length_a                   15.364(3)
_cell_length_b                   20.866(4)
_cell_length_c                   30.156(6)
_cell_measurement_reflns_used    53451
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      55.08
_cell_measurement_theta_min      6.05
_cell_volume                     9635(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.01
_diffrn_measured_fraction_theta_full 0.921
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_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  0.1094
_diffrn_reflns_av_sigmaI/netI    0.1577
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            67155
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.02
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.413
_exptl_absorpt_correction_T_max  0.026
_exptl_absorpt_correction_T_min  0.008
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'ABSCOR by T.Higashi 8 March, 1995'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    3.024
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7832
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.21
_refine_diff_density_max         3.216
_refine_diff_density_min         -3.102
_refine_diff_density_rms         0.408
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1996
_refine_ls_number_reflns         31226
_refine_ls_number_restraints     1235
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1198
_refine_ls_R_factor_gt           0.0693
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1495
_refine_ls_wR_factor_ref         0.1655
_reflns_number_gt                18054
_reflns_number_total             31226
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2010-183-310.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the built-in table derived from the
CIF Core dictionary named 'cif_core.dic' version 2.4.5 last updated
on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 8369 2020-08-20 11:38:08Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C54 H106 Fe9 N18 Na8 O115.50 Si3 W28'
_cod_database_code               1563728