Polyoxometalate-Based Metal−Organic Frameworks Assembled under the Ionothermal Conditions
Fu, Hai; Li, Yangguang; Lu, Ying; Chen, Weilin; Wu, Qiong; Meng, Jingxin; Wang, Xiaolan; Zhang, Zhiming; Wang, Enbo; Crystal Growth & Design 11 (2011) 458–; doi:10.1021/cg101224r

data_4500182
_publ_section_title
;
 Polyoxometalate-Based Metal&#x2212;Organic Frameworks Assembled under the
 Ionothermal Conditions
;
_journal_issue                   2
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              458
_journal_paper_doi               10.1021/cg101224r
_journal_volume                  11
_journal_year                    2011
_chemical_formula_sum            'C76 H108 Cu5 N32 O130 P4 W36'
_chemical_formula_weight         10610.12
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 113.68(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.540(4)
_cell_length_b                   13.302(3)
_cell_length_c                   43.600(12)
_cell_measurement_temperature    150(2)
_cell_volume                     9847(5)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX area-detector diffractometer'
_diffrn_measurement_method       '\f and \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  0.1907
_diffrn_reflns_av_sigmaI/netI    0.1531
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            46526
_diffrn_reflns_theta_full        21.98
_diffrn_reflns_theta_max         21.98
_diffrn_reflns_theta_min         3.04
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    21.588
_exptl_absorpt_correction_T_max  0.0986
_exptl_absorpt_correction_T_min  0.0785
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.578
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             9394
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_platon_squeeze_details          ' '
_refine_diff_density_max         3.660
_refine_diff_density_min         -3.378
_refine_diff_density_rms         0.545
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     753
_refine_ls_number_reflns         11980
_refine_ls_number_restraints     292
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1376
_refine_ls_R_factor_gt           0.0873
_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^)+(0.0000P)^2^+1504.9878P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1598
_refine_ls_wR_factor_ref         0.1822
_reflns_number_gt                7825
_reflns_number_total             11980
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg101224r_si_004.cif
_cod_data_source_block           1
_cod_original_cell_volume        9847(4)
_cod_original_sg_symbol_H-M      p21/c
_cod_database_code               4500182