The design, syntheses and characterization of a series of hybrids based on polyoxometalates and metal complexes
Wang, La-Mei; Wang, Yan; Fan, Yong; Xiao, Li-Na; Hu, Yang-Yang; Gao, Zhong-Min; Zheng, Da-Fang; Cui, Xiao-Bing; Xu, Ji-Qing; CrystEngComm 16 (2014) 430–; doi:10.1039/c3ce41611a

data_7213775
_publ_section_title
;
 The design, syntheses and characterization of a series of hybrids based
 on polyoxometalates and metal complexes
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              430
_journal_paper_doi               10.1039/c3ce41611a
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C68 H48 Cu4 Mo12 N12 O42 Si V2'
_chemical_formula_weight         3240.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           72
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-I 2 2c'
_symmetry_space_group_name_H-M   'I b a m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2145(11)
_cell_length_b                   24.934(2)
_cell_length_c                   27.184(2)
_cell_measurement_temperature    296(2)
_cell_volume                     8956.9(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0413
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            23450
_diffrn_reflns_theta_full        25.77
_diffrn_reflns_theta_max         25.77
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    2.851
_exptl_absorpt_correction_T_max  0.6279
_exptl_absorpt_correction_T_min  0.4530
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    2.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6224
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.867
_refine_diff_density_min         -1.219
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         4396
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0518
_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^)+(0.0668P)^2^+121.7090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1347
_refine_ls_wR_factor_ref         0.1477
_reflns_number_gt                3341
_reflns_number_total             4396
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41611a.txt
_cod_data_source_block           k
_cod_original_cell_volume        8956.8(13)
_cod_original_sg_symbol_H-M      Ibam
_cod_database_code               7213775