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_7225010
_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            'C50 H40 N10 O54 Pb2 Si W12'
_chemical_formula_weight         4293.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_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                90.0000(10)
_cell_angle_beta                 92.7800(10)
_cell_angle_gamma                90.0000(10)
_cell_formula_units_Z            4
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_cell_length_b                   15.8420(11)
_cell_length_c                   26.966(5)
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_cell_measurement_temperature    298(2)
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_cell_measurement_theta_min      1.305
_cell_volume                     7901.1(16)
_computing_cell_refinement       'Bruker SAINT v8.34a'
_computing_data_collection       'Bruker APEX 2'
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_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      298(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     0.71069
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_unetI/netI     0.0568
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            39622
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_diffrn_source                   'fine-focus sealed tube'
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_exptl_absorpt_correction_T_min  0.003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/4 Bruker AXS Madison WI USA'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.609
_exptl_crystal_description       block
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_exptl_crystal_size_min          0.230
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_refine_ls_extinction_method     none
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_refine_ls_number_reflns         13897
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_refine_ls_restrained_S_all      0.946
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0155P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0549
_refine_ls_wR_factor_ref         0.0599
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10731
_reflns_number_total             13897
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           nn
_cod_depositor_comments
'Adding full bibliography for 7225009--7225010.cif.'
_cod_database_code               7225010
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.074
_shelx_estimated_absorpt_t_max   0.082
_shelx_res_checksum              50325