First examples of hybrids based on polyoxometalates, metal halide clusters and organic ligands
Wang, La-Mei; Fan, Yong; Wang, Yan; Xiao, Li-Na; Hu, Yang-Yang; Peng, Yu; Wang, Tie-Gang; Gao, Zhong-Min; Zheng, Da-Fang; Cui, Xiao-Bing; Xu, Ji-Qing; Journal of Solid State Chemistry 191 (2012) 257–262; doi:10.1016/j.jssc.2012.03.033

data_1562985
_publ_section_title
;
 First examples of hybrids based on polyoxometalates, metal halide
 clusters and organic ligands
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              257
_journal_page_last               262
_journal_paper_doi               10.1016/j.jssc.2012.03.033
_journal_volume                  191
_journal_year                    2012
_chemical_formula_sum            'C88 H85 B2 Cl Cu2 N16 O86 W24'
_chemical_formula_weight         7339.27
_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                100.00(3)
_cell_angle_beta                 91.58(3)
_cell_angle_gamma                115.88(3)
_cell_formula_units_Z            1
_cell_length_a                   12.044(2)
_cell_length_b                   12.814(3)
_cell_length_c                   23.915(5)
_cell_measurement_temperature    293(2)
_cell_volume                     3247.9(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0600
_diffrn_reflns_av_sigmaI/netI    0.0825
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            31818
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    21.603
_exptl_absorpt_correction_T_max  0.0985
_exptl_absorpt_correction_T_min  0.0434
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    3.752
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3274
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_refine_diff_density_max         3.940
_refine_diff_density_min         -2.425
_refine_diff_density_rms         0.360
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     973
_refine_ls_number_reflns         14671
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0572
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0595P)^2^+43.8006P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1328
_refine_ls_wR_factor_ref         0.1457
_reflns_number_gt                10455
_reflns_number_total             14671
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2012-191-257.cif
_cod_data_source_block           k1
_cod_original_cell_volume        3247.7(11)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1562985