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_7055519
_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            'C36.5 H29.5 N3 O7 Zn'
_chemical_formula_weight         687.50
_space_group_crystal_system      hexagonal
_space_group_IT_number           179
_space_group_name_Hall           'P 65 2 (0 0 1)'
_space_group_name_H-M_alt        'P 65 2 2'
_symmetry_space_group_name_Hall  'P 65 2 (0 0 1)'
_symmetry_space_group_name_H-M   'P 65 2 2'
_atom_sites_solution_hydrogens   mixed
_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                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   11.1967(4)
_cell_length_b                   11.1967(4)
_cell_length_c                   44.0828(16)
_cell_measurement_reflns_used    9977
_cell_measurement_temperature    273
_cell_measurement_theta_max      66.77
_cell_measurement_theta_min      4.56
_cell_volume                     4786.1(3)
_computing_cell_refinement       'APEX2 v2015.5 (Bruker AXS)'
_computing_data_collection
'Bruker Instrument Service V4.2.7 (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'XSHELL V6.3.1 (Bruker AXS Inc., 2004)'
_computing_publication_material
'Generate Report V2014.1 (Bruker AXS Inc., 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2013)'
_diffrn_ambient_temperature      273
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0277
_diffrn_reflns_av_unetI/netI     0.0134
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            35785
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.765
_diffrn_reflns_theta_min         4.560
_diffrn_source                   'rotating anode'
_diffrn_source_type              'Bruker Turbo X-ray Source'
_exptl_absorpt_coefficient_mu    1.534
_exptl_absorpt_correction_T_max  0.896
_exptl_absorpt_correction_T_min  0.831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_description       block
_exptl_crystal_F_000             2133
_exptl_crystal_size_max          0.147
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.073
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 1034 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         2840
_refine_ls_number_restraints     325
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0269
_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^)+(0.0391P)^2^+3.0319P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0731
_reflns_Friedel_coverage         0.584
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2819
_reflns_number_total             2840
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj00090h2.cif
_cod_data_source_block           p6522
_cod_depositor_comments
'Adding full bibliography for 7055519--7055520.cif.'
_cod_original_cell_volume        4786.1(4)
_cod_original_formula_sum        'C36.50 H29.50 N3 O7 Zn'
_cod_database_code               7055519
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.806
_shelx_estimated_absorpt_t_max   0.896
_shelx_res_checksum              21606