Chiral Nanoporous Metal-Metallosalen Frameworks for Hydrolytic Kinetic Resolution of Epoxides
Chengfeng Zhu; Guozan Yuan; Xu Chen; Zhiwei Yang; Yong Cui; Journal of the American Chemical Society 134 (2012) 8058–8061; doi:10.1021/ja302340b

data_4117936
_publ_contact_author             'Yong Cui'
_publ_contact_author_email       yongcui@sjtu.edu.cn
_publ_contact_author_fax         +86-21-54741297
_publ_contact_author_phone       +86-21-54747687
_publ_section_title
;
 Chiral Nanoporous Metal-Metallosalen Frameworks for Hydrolytic Kinetic
 Resolution of Epoxides
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8058
_journal_page_last               8061
_journal_paper_doi               10.1021/ja302340b
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C132 H172 Cd4 N12 Ni4 O32'
_chemical_formula_weight         3123.26
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 101.996(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.430(3)
_cell_length_b                   40.910(9)
_cell_length_c                   30.645(6)
_cell_measurement_reflns_used    26898
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.04
_cell_volume                     17696(6)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL-PLUS (Sheldrick, 1990)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0880
_diffrn_reflns_av_sigmaI/netI    0.1592
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            45624
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.947
_exptl_absorpt_correction_T_max  0.910
_exptl_absorpt_correction_T_min  0.890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_description       Block
_exptl_crystal_F_000             6432
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.681
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.152
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.29(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1212
_refine_ls_number_reflns         26898
_refine_ls_number_restraints     371
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1838
_refine_ls_R_factor_gt           0.1072
_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^)+(0.1214P)^2^+305.2712P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2559
_refine_ls_wR_factor_ref         0.3104
_reflns_number_gt                13953
_reflns_number_total             26898
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja302340b_si_002_1.cif
_cod_data_source_block           '[Cd4(NiL)4(DMF)4]4H2O_1'
_cod_database_code               4117936