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_7034665
_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            'C60 H40 Cl4 Cu4 N10 O44 Si W12'
_chemical_formula_weight         4235.19
_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
_audit_update_record
;
2015-03-09 deposited with the CCDC.
2015-03-30 downloaded from the CCDC.
;
_cell_angle_alpha                102.93(3)
_cell_angle_beta                 91.43(3)
_cell_angle_gamma                102.46(3)
_cell_formula_units_Z            1
_cell_length_a                   12.186(2)
_cell_length_b                   12.977(3)
_cell_length_c                   14.887(3)
_cell_measurement_reflns_used    13048
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      35.33
_cell_measurement_theta_min      1.79
_cell_volume                     2233.8(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_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  0.0303
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16247
_diffrn_reflns_theta_full        25.94
_diffrn_reflns_theta_max         25.94
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    16.531
_exptl_absorpt_correction_T_max  0.1906
_exptl_absorpt_correction_T_min  0.1548
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    3.148
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1907
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.067
_refine_diff_density_min         -4.933
_refine_diff_density_rms         0.445
_refine_ls_extinction_coef       0.00112(7)
_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   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     629
_refine_ls_number_reflns         8463
_refine_ls_number_restraints     157
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1007
_refine_ls_R_factor_gt           0.1001
_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^)+(0.0000P)^2^+525.6360P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2179
_refine_ls_wR_factor_ref         0.2181
_reflns_number_gt                8332
_reflns_number_total             8463
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt00201j2.cif
_cod_data_source_block           k4
_cod_depositor_comments
'Adding full bibliography for 7034662--7034666.cif.'
_cod_original_cell_volume        2233.8(8)
_cod_original_sg_symbol_H-M      p-1
_cod_database_code               7034665