Highly Stable Crystalline Catalysts Based on a Microporous Metal-Organic Framework and Polyoxometalates
Chun-Yan Sun; Shu-Xia Liu; Da-Dong Liang; Kui-Zhan Shao; Yuan-Hang Ren; Zhong-Min Su; Journal of the American Chemical Society 131 (2009) 1883–1888; doi:10.1021/ja807357r

data_4103877
_publ_section_title
;
 Highly Stable Crystalline Catalysts Based on a Microporous Metal-Organic
 Framework and Polyoxometalates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1883
_journal_page_last               1888
_journal_paper_doi               10.1021/ja807357r
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C76 H36 Cu12 Ge N O112 W12'
_chemical_formula_weight         5795.86
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           225
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-F 4 2 3'
_symmetry_space_group_name_H-M   'F m -3 m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.3189(12)
_cell_length_b                   26.318(12)
_cell_length_c                   26.318(12)
_cell_measurement_reflns_used    4347
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.85
_cell_measurement_theta_min      2.19
_cell_volume                     18229(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0489
_diffrn_reflns_av_sigmaI/netI    0.0134
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            23342
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    9.152
_exptl_absorpt_correction_T_max  0.348
_exptl_absorpt_correction_T_min  0.331
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'
_exptl_crystal_density_diffrn    2.098
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             10400
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.092
_refine_diff_density_min         -2.197
_refine_diff_density_rms         0.612
_refine_ls_extinction_coef       0.000132(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.295
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         874
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.295
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0979P)^2^+171.7548P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1373
_refine_ls_wR_factor_ref         0.1608
_reflns_number_gt                758
_reflns_number_total             874
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja807357r_si_003.cif
_cod_data_source_block           2
_cod_original_cell_volume        18229.0
_cod_database_code               4103877