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_4500568
_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         'C24 H35 Cu4 Mo12 N8 O41.50 P'
_chemical_formula_sum            'C24 H35 Cu4 Mo12 N8 O41.5 P'
_chemical_formula_weight         2536.01
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 112.811(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.4725(7)
_cell_length_b                   12.0745(3)
_cell_length_c                   23.1288(7)
_cell_measurement_reflns_used    6164
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      1.9
_cell_volume                     6042.4(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0879
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            15276
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    3.901
_exptl_absorpt_correction_T_max  0.67
_exptl_absorpt_correction_T_min  0.52
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis (Oxford Diffraction, 2006)
;
_exptl_crystal_colour            blacl
_exptl_crystal_density_diffrn    2.788
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4808
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.966
_refine_diff_density_min         -0.832
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.859
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         6164
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.859
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0475P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.0964
_reflns_number_gt                3413
_reflns_number_total             6164
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            cg1017246_si_002.cif
_cod_data_source_block           5
_cod_original_sg_symbol_Hall     '-C 2yc '
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_original_formula_sum        'C24 H35 Cu4 Mo12 N8 O41.50 P'
_cod_database_code               4500568