Solvothermal Assembly of a Series of Organic‒Inorganic Hybrid Materials Constructed from Keggin Polyoxometalate Clusters and Copper(I)‒Organic Frameworks
Liu, Hai-Yan; Wu, Hua; Yang, Jin; Liu, Ying-Ying; Ma, Jian-Fang; Bai, Hong-Ye; Crystal Growth & Design 11 (2011) 1786–; doi:10.1021/cg1017246

data_4500564
_publ_section_title
;
 Solvothermal Assembly of a Series of Organic--Inorganic Hybrid Materials
 Constructed from Keggin Polyoxometalate Clusters and Copper(I)--Organic
 Frameworks
;
_journal_issue                   5
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1786
_journal_paper_doi               10.1021/cg1017246
_journal_volume                  11
_journal_year                    2011
_chemical_formula_moiety         'C35 H48 Cu4 N10 O40 Si W12'
_chemical_formula_sum            'C35 H48 Cu4 N10 O40 Si W12'
_chemical_formula_weight         3737.28
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 91.791(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.9036(5)
_cell_length_b                   11.9095(3)
_cell_length_c                   22.3016(10)
_cell_measurement_reflns_used    6247
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.4
_cell_measurement_theta_min      4.3
_cell_volume                     3425.5(2)
_computing_cell_refinement       CrysAlis
_computing_data_collection       'CrysAlis (Oxford Diffraction, 2006)'
_computing_data_reduction        CrysAlis
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Oxford Diffraction Gemini R Ultra'
_diffrn_measurement_method       '\w scan'
_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  0.1012
_diffrn_reflns_av_sigmaI/netI    0.1275
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            27325
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         4.29
_exptl_absorpt_coefficient_mu    21.378
_exptl_absorpt_correction_T_max  0.12
_exptl_absorpt_correction_T_min  0.07
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis (Oxford Diffraction, 2006)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.623
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3332
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.780
_refine_diff_density_min         -3.087
_refine_diff_density_rms         0.236
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.874
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         6247
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      0.880
_refine_ls_R_factor_all          0.1604
_refine_ls_R_factor_gt           0.0582
_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^)+(0.0708P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1212
_refine_ls_wR_factor_ref         0.1477
_reflns_number_gt                2675
_reflns_number_total             6247
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            cg1017246_si_002.cif
_cod_data_source_block           1
_cod_original_sg_symbol_Hall     '-P 2yn  '
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4500564