New compounds constructed from polyoxometalates and transition metal coordination complexes with lower positive charge
Wang, Yan; Peng, Yu; Xiao, Li-Na; Hu, Yang-Yang; Wang, La-Mei; Gao, Zhong-Min; Wang, Tie-Gang; Wu, Feng-Qing; Cui, Xiao-Bing; Xu, Ji-Qing; CrystEngComm 14 (2012) 1049–; doi:10.1039/c1ce05633f

data_7206939
_publ_section_title
;
 New compounds constructed from polyoxometalates and transition metal
 coordination complexes with lower positive charge
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              1049
_journal_paper_doi               10.1039/c1ce05633f
_journal_volume                  14
_journal_year                    2012
_chemical_formula_sum            'C96 H72 B Cu5 N16 O44 W12'
_chemical_formula_weight         4688.34
_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                78.45(3)
_cell_angle_beta                 82.58(3)
_cell_angle_gamma                87.87(3)
_cell_formula_units_Z            2
_cell_length_a                   12.506(3)
_cell_length_b                   14.025(3)
_cell_length_c                   31.972(6)
_cell_measurement_temperature    293(2)
_cell_volume                     5448(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_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  0.0543
_diffrn_reflns_av_sigmaI/netI    0.0747
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            49714
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    13.657
_exptl_absorpt_correction_T_max  0.0935
_exptl_absorpt_correction_T_min  0.0618
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.858
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4298
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.33
_refine_diff_density_max         3.158
_refine_diff_density_min         -3.537
_refine_diff_density_rms         0.369
_refine_ls_extinction_coef       0.00060(5)
_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   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1607
_refine_ls_number_reflns         23595
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0645
_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^)+(0.1060P)^2^+41.8057P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1694
_refine_ls_wR_factor_ref         0.1989
_reflns_number_gt                16452
_reflns_number_total             23595
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ce05633f.txt
_cod_data_source_block           k_3
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7206939