Sorption discrimination between secondary alcohol enantiomers by chiral alkyl-dicarboxylate MOFs
Satska, Yulia A.; Mikhalyova, Elena A.; Chernenko, Zhanna V.; Kolotilov, Sergey V.; Zeller, Matthias; Komarov, Igor V.; Tymtsunik, Andriy V.; Tolmachev, Andrey; Gavrilenko, Konstantin S.; Addison, Anthony W.; RSC Advances 6 (2016) 93707–93714; doi:10.1039/C6RA09353A

data_1544178
_publ_section_title
;
 Sorption discrimination between secondary alcohol enantiomers by chiral
 alkyl-dicarboxylate MOFs
;
_journal_issue                   96
_journal_name_full               'RSC Advances'
_journal_page_first              93707
_journal_page_last               93714
_journal_paper_doi               10.1039/C6RA09353A
_journal_volume                  6
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C30 H30 Co2 N4 O9, C5 H5 N'
_chemical_formula_sum            'C35 H35 Co2 N5 O9'
_chemical_formula_weight         787.54
_chemical_properties_physical    Efflorescent
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-02-19 deposited with the CCDC.
2016-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8480(5)
_cell_length_b                   10.8480(5)
_cell_length_c                   29.771(3)
_cell_measurement_reflns_used    3234
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.29
_cell_measurement_theta_min      2.66
_cell_volume                     3503.4(4)
_computing_cell_refinement       'SAINT V7.53A (Bruker, 2008)'
_computing_data_collection       'Apex2 v2008.2-4 (Bruker, 2008)'
_computing_data_reduction        'SAINT V7.53A (Bruker, 2008)'
_computing_structure_refinement
;  
SHELXL-2014/7 (Sheldrick, 2014), 
SHELXLE Rev758 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker AXS SMART APEX CCD diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            22289
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.098
_diffrn_reflns_theta_min         1.998
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.009
_exptl_absorpt_correction_T_max  0.801
_exptl_absorpt_correction_T_min  0.687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 v2008.2-4 (Bruker, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_description       block
_exptl_crystal_F_000             1624
_exptl_crystal_preparation       'Sorption of chiral 2-butanol'
_exptl_crystal_recrystallization_method
'Diffusion of pyridine vapor into solution of reagents'
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.220
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 1623 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.004(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         5432
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0353P)^2^+1.4300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0945
_reflns_Friedel_coverage         0.676
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.940
_reflns_number_gt                4732
_reflns_number_total             5432
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra09353a2.cif
_cod_data_source_block           09mz101_0m
_cod_original_cell_volume        3503.4(5)
_cod_database_code               1544178
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.671
_shelx_estimated_absorpt_t_max   0.809
_shelx_res_checksum              53373