Assembly of two novel 3D organic‒inorganic hybrids based on Keggin-type polyoxometalates: syntheses, crystal structures and properties
Zhou, En-Long; Qin, Chao; Wang, Xin-Long; Shao, Kui-Zhan; Su, Zhong-Min; CrystEngComm 18 (2016) 6370–; doi:10.1039/C6CE00021E

data_7225009
_publ_section_title
;
 Assembly of two novel 3D organic--inorganic hybrids based on Keggin-type
 polyoxometalates: syntheses, crystal structures and properties
;
_journal_issue                   34
_journal_name_full               CrystEngComm
_journal_page_first              6370
_journal_paper_doi               10.1039/C6CE00021E
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C34 H52 N51 O89 Si2 W24 Zn12.5'
_chemical_formula_weight         7884.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-03-07 deposited with the CCDC.
2016-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 120.8360(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.5590(16)
_cell_length_b                   27.6534(16)
_cell_length_c                   21.9738(12)
_cell_measurement_reflns_used    29585
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.622
_cell_measurement_theta_min      1.786
_cell_volume                     13857.2(14)
_computing_cell_refinement       'Bruker SAINT v8.34a'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT v8.34a'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL & local programs'
_computing_structure_refinement  'SHELXL-2015/1 (Sheldrick, 2015)'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 0.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart Apex II CCD'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0724
_diffrn_reflns_av_unetI/netI     0.0728
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            27843
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        21.999
_diffrn_reflns_theta_max         21.999
_diffrn_reflns_theta_min         1.786
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    22.070
_exptl_absorpt_correction_T_max  0.076
_exptl_absorpt_correction_T_min  0.061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/4 Bruker AXS Madison WI USA'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.779
_exptl_crystal_description       block
_exptl_crystal_F_000             14016
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.240
_refine_diff_density_max         2.916
_refine_diff_density_min         -3.494
_refine_diff_density_rms         0.352
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1031
_refine_ls_number_reflns         8711
_refine_ls_number_restraints     2154
_refine_ls_restrained_S_all      0.910
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.105
_refine_ls_shift/su_mean         0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0562P)^2^+1798.0880P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1268
_refine_ls_wR_factor_ref         0.1462
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6099
_reflns_number_total             8711
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce00021e2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7225009--7225010.cif.'
_cod_original_formula_sum        'C34 H52 N51 O89 Si2 W24 Zn12.50'
_cod_database_code               7225009
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.060
_shelx_estimated_absorpt_t_max   0.076
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              93226