Polyoxometalate-based organic-inorganic hybrid compounds containing transition metal mixed-organic-ligand complexes of N-containing and pyridinecarboxylate ligands.
Zhao, De-Chuan; Hu, Yang-Yang; Ding, Hong; Guo, Hai-Yang; Cui, Xiao-Bing; Zhang, Xiao; Huo, Qi-Sheng; Xu, Ji-Qing; Dalton transactions (Cambridge, England : 2003) 44 (2015) 8971–8983; doi:10.1039/c5dt00201j

data_7034664
_publ_section_title
;
 Polyoxometalate-based organic-inorganic hybrid compounds containing
 transition metal mixed-organic-ligand complexes of N-containing and
 pyridinecarboxylate ligands.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8971
_journal_page_last               8983
_journal_paper_doi               10.1039/c5dt00201j
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C52 H40 Cl2 Cu4 N10 O46 Si W12'
_chemical_formula_weight         4100.29
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-03-09 deposited with the CCDC.
2015-03-30 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.953(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.070(4)
_cell_length_b                   13.496(3)
_cell_length_c                   18.814(5)
_cell_measurement_reflns_used    10087
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      35.28
_cell_measurement_theta_min      2.20
_cell_volume                     3826.0(17)
_computing_data_collection       'Bruker XSCANS'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker P4'
_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  0.0379
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15229
_diffrn_reflns_theta_full        25.84
_diffrn_reflns_theta_max         25.84
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    19.232
_exptl_absorpt_correction_T_max  0.1071
_exptl_absorpt_correction_T_min  0.0687
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    3.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3684
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         3.604
_refine_diff_density_min         -2.689
_refine_diff_density_rms         0.493
_refine_ls_extinction_coef       0.00025(2)
_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    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     593
_refine_ls_number_reflns         7252
_refine_ls_number_restraints     542
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1086
_refine_ls_R_factor_gt           0.1076
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+1223.2614P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2300
_refine_ls_wR_factor_ref         0.2304
_reflns_number_gt                7110
_reflns_number_total             7252
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt00201j2.cif
_cod_data_source_block           k3
_cod_depositor_comments
'Adding full bibliography for 7034662--7034666.cif.'
_cod_original_cell_volume        3825.9(16)
_cod_original_sg_symbol_H-M      p2(1)/n
_cod_database_code               7034664