Efficient HPLC enantiomer separation using a pillared homochiral metal‒organic framework as a novel chiral stationary phase
Tanaka, Koichi; Hotta, Naoki; Nagase, Shohei; Yoza, Kenji; New J. Chem. 40 (2016) 4891–; doi:10.1039/C6NJ00090H

data_7055520
_publ_section_title
;
 Efficient HPLC enantiomer separation using a pillared homochiral
 metal--organic framework as a novel chiral stationary phase
;
_journal_issue                   6
_journal_name_full               'New J. Chem.'
_journal_page_first              4891
_journal_paper_doi               10.1039/C6NJ00090H
_journal_volume                  40
_journal_year                    2016
_chemical_formula_sum            'C72 H53 N5 O13 Zn2'
_chemical_formula_weight         1326.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-12-28 deposited with the CCDC.
2016-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.217(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.9801(10)
_cell_length_b                   13.6765(6)
_cell_length_c                   25.5651(11)
_cell_measurement_reflns_used    8074
_cell_measurement_temperature    93
_cell_measurement_theta_max      67.058
_cell_measurement_theta_min      3.538
_cell_volume                     7511.1(6)
_computing_cell_refinement       'APEX2 (Bruker AXS)'
_computing_data_collection
'Bruker Instrument Service (Bruker AXS Inc., 2014)'
_computing_data_reduction        'SAINT (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'XSHELL V6.3.1 (Bruker AXS Inc., 2004)'
_computing_publication_material  'Generate Report (Bruker AXS Inc., 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2013)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'multilayered conforcal mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            26112
_diffrn_reflns_point_group_measured_fraction_full 0.906
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         67.023
_diffrn_reflns_theta_min         3.538
_diffrn_source                   'rotating anode'
_diffrn_source_type              'Bruker Turbo X-ray Source'
_exptl_absorpt_coefficient_mu    1.273
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_description       plate
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Flack x determined using 4569 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.036(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     869
_refine_ls_number_reflns         12129
_refine_ls_number_restraints     1950
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+4.7534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0902
_reflns_Friedel_coverage         0.738
_reflns_Friedel_fraction_full    0.807
_reflns_Friedel_fraction_max     0.804
_reflns_number_gt                11470
_reflns_number_total             12129
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj00090h2.cif
_cod_data_source_block           c2_a
_cod_depositor_comments
'Adding full bibliography for 7055519--7055520.cif.'
_cod_database_code               7055520
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.822
_shelx_estimated_absorpt_t_max   0.928
_shelx_res_checksum              39752