Two new hybrid compounds assembled from Keggin-type polyoxometalates and transition metal coordination complexes
Wang, Yan; Zou, Bo; Xiao, Li-Na; Jin, Ning; Peng, Yu; Wu, Feng-Qing; Ding, Hong; Wang, Tie-Gang; Gao, Zhong-Min; Zheng, Da-Fang; Cui, Xiao-Bing; Xu, Ji-Qing; Journal of Solid State Chemistry 184 (2011) 557–562; doi:10.1016/j.jssc.2011.01.009

data_1563290
_publ_section_title
;
 Two new hybrid compounds assembled from Keggin-type polyoxometalates and
 transition metal coordination complexes
;
_journal_issue                   3
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              557
_journal_page_last               562
_journal_paper_doi               10.1016/j.jssc.2011.01.009
_journal_volume                  184
_journal_year                    2011
_chemical_formula_sum            'C48 H38 K Mo12 N8 Ni2 O44 P'
_chemical_formula_weight         2769.59
_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                69.4980(10)
_cell_angle_beta                 71.7970(10)
_cell_angle_gamma                79.0790(10)
_cell_formula_units_Z            1
_cell_length_a                   10.7462(6)
_cell_length_b                   13.2324(7)
_cell_length_c                   13.6528(8)
_cell_measurement_temperature    210(2)
_cell_volume                     1720.43(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      210(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0538
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9545
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    2.834
_exptl_absorpt_correction_T_max  0.9300
_exptl_absorpt_correction_T_min  0.4122
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    2.673
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1327
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.653
_refine_diff_density_min         -2.734
_refine_diff_density_rms         0.274
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         6667
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0674
_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^)+(0.0814P)^2^+46.4138P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1773
_refine_ls_wR_factor_ref         0.1899
_reflns_number_gt                5267
_reflns_number_total             6667
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2011-184-557.cif
_cod_data_source_block           k
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1563290