Engineering Chiral Polyoxometalate Hybrid Metal-Organic Frameworks for Asymmetric Dihydroxylation of Olefins
Qiuxia Han; Cheng He; Min Zhao; Bo Qi; Jingyang Niu; Chunying Duan; Journal of the American Chemical Society 135 (2013) 10186–10189; doi:10.1021/ja401758c

data_4120097
_publ_section_title
;
 Engineering Chiral Polyoxometalate Hybrid Metal-Organic Frameworks for
 Asymmetric Dihydroxylation of Olefins
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10186
_journal_page_last               10189
_journal_paper_doi               10.1021/ja401758c
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C50 H45.5 B Cl0.5 N10 Ni2 O42 W12'
_chemical_formula_weight         3810.62
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
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_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 102.665(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.4140(3)
_cell_length_b                   14.9239(4)
_cell_length_c                   20.0622(5)
_cell_measurement_temperature    296(2)
_cell_volume                     3918.52(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0621
_diffrn_reflns_av_sigmaI/netI    0.1037
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18409
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    18.111
_exptl_absorpt_correction_T_max  0.1390
_exptl_absorpt_correction_T_min  0.1031
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    3.230
_exptl_crystal_description       block
_exptl_crystal_F_000             3418
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         3.080
_refine_diff_density_min         -1.601
_refine_diff_density_rms         0.365
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.375(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1067
_refine_ls_number_reflns         10227
_refine_ls_number_restraints     352
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0665P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1286
_refine_ls_wR_factor_ref         0.1412
_reflns_number_gt                7722
_reflns_number_total             10227
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja401758c_si_004.cif
_cod_data_source_block           1
_cod_original_cell_volume        3918.51(17)
_cod_original_formula_sum        'C50 H45.50 B Cl0.50 N10 Ni2 O42 W12'
_cod_database_code               4120097