Hydrothermal synthesis and structural characterization of the first mixed molybdenum‒tungsten capped-keggin polyoxometal complex: {[Co(dien)]4[(AsVO4)MoV8WVI4O33(µ2‒OH)3]}·2H2O
Yu, Hai-Hui; Cui, Xiao-Bing; Cui, Ji-Wen; Kong, Li; Duan, Wei-Jie; Xu, Ji-Qing; Wang, Tie-Gang; Dalton Transactions  (2008) 195–197; doi:10.1039/b711604g

data_7003083
_publ_section_title
;
 Hydrothermal synthesis and structural characterization of the first
 mixed molybdenum--tungsten capped-keggin polyoxometal complex:
 {[Co(dien)]4[(AsVO4)MoV8WVI4O33(&#x00B5;2--OH)3]}&#x00B7;2H2O
;
_journal_issue                   2
_journal_name_full               'Dalton Transactions'
_journal_page_first              195
_journal_page_last               197
_journal_paper_doi               10.1039/b711604g
_journal_year                    2008
_chemical_formula_sum            'C16 H59 As Co4 Mo8 N12 O42 W4'
_chemical_formula_weight         2905.31
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                93.89(3)
_cell_angle_beta                 94.50(3)
_cell_angle_gamma                109.70(3)
_cell_formula_units_Z            2
_cell_length_a                   11.906(2)
_cell_length_b                   13.363(3)
_cell_length_c                   19.406(4)
_cell_measurement_temperature    293(2)
_cell_volume                     2883.2(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28267
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.14
_exptl_absorpt_coefficient_mu    11.410
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2696
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         3.292
_refine_diff_density_min         -2.815
_refine_diff_density_rms         0.312
_refine_ls_extinction_coef       0.00010(4)
_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    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     785
_refine_ls_number_reflns         12941
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0433
_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^)+(0.0483P)^2^+63.7339P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1188
_reflns_number_gt                11307
_reflns_number_total             12941
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b711604g.txt
_cod_data_source_block           xjq
_cod_original_cell_volume        2883.1(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7003083