New organic-inorganic hybrid compounds constructed from polyoxometalates and transition metal mixed-organic-ligand complexes.
Hu, Yang-Yang; Zhang, Ting-Ting; Zhang, Xiao; Zhao, De-Chuan; Cui, Xiao-Bing; Huo, Qi-Sheng; Xu, Ji-Qing; Dalton transactions (Cambridge, England : 2003) 45 (2016) 2562–2573; doi:10.1039/c5dt04413h

data_7037673
_publ_section_title
;
 New organic-inorganic hybrid compounds constructed from polyoxometalates
 and transition metal mixed-organic-ligand complexes.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2562
_journal_page_last               2573
_journal_paper_doi               10.1039/c5dt04413h
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C52 H40 Cl2 Cu4 Ge N10 O46 W12'
_chemical_formula_weight         4144.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-12-07 deposited with the CCDC.
2015-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 128.069(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.1378(9)
_cell_length_b                   13.5053(8)
_cell_length_c                   23.9776(11)
_cell_measurement_reflns_used    8933
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.2080
_cell_measurement_theta_min      3.2330
_cell_volume                     3859.2(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Diamond 3.2'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            19015
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         2.939
_exptl_absorpt_coefficient_mu    19.433
_exptl_absorpt_correction_T_max  0.098
_exptl_absorpt_correction_T_min  0.043
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    3.567
_exptl_crystal_description       block
_exptl_crystal_F_000             3720
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_refine_diff_density_max         3.271
_refine_diff_density_min         -2.801
_refine_diff_density_rms         0.463
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         7059
_refine_ls_number_restraints     702
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1101
_refine_ls_R_factor_gt           0.1040
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+1294.9978P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2274
_refine_ls_wR_factor_ref         0.2306
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6455
_reflns_number_total             7059
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04413h2.cif
_cod_data_source_block           shelx_4
_cod_depositor_comments
'Adding full bibliography for 7037670--7037674.cif.'
_cod_database_code               7037673
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.058
_shelx_estimated_absorpt_t_max   0.112
_exptl_absorpt_special_details
;
 R(int) was 0.0478 before and 0.0456 after correction.
;
_shelx_res_checksum              64522
_shelx_hkl_checksum              8694