Engineering a homochiral metal-organic framework based on an amino acid for enantioselective separation.
Tang, Haitong; Yang, Keke; Wang, Kun-Yu; Meng, Qi; Wu, Fan; Fang, Yu; Wu, Xiang; Li, Yougui; Zhang, WenCheng; Luo, Yunfei; Zhu, Chengfeng; Zhou, Hong-Cai; Chemical communications (Cambridge, England) 56 (2020) 9016–9019; doi:10.1039/d0cc00897d

data_7126797
_publ_section_title
;
 Engineering a homochiral metal-organic framework based on an amino acid
 for enantioselective separation.
;
_journal_issue                   63
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9016
_journal_page_last               9019
_journal_paper_doi               10.1039/d0cc00897d
_journal_volume                  56
_journal_year                    2020
_chemical_absolute_configuration rm
_chemical_formula_moiety         '0.5(C186 H156 N18 O38 Zn8)'
_chemical_formula_sum            'C93 H78 N9 O19 Zn4'
_chemical_formula_weight         1887.12
_space_group_crystal_system      trigonal
_space_group_IT_number           150
_space_group_name_Hall           'P 3 2"'
_space_group_name_H-M_alt        'P 3 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-11-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-26 deposited with the CCDC.	2020-06-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   25.6587(8)
_cell_length_b                   25.6587(8)
_cell_length_c                   10.1334(5)
_cell_measurement_reflns_used    9678
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.750
_cell_measurement_theta_min      2.224
_cell_volume                     5777.7(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  Synchrotron
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.65247
_diffrn_reflns_av_R_equivalents  0.0872
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            103649
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        23.047
_diffrn_reflns_theta_max         27.869
_diffrn_reflns_theta_min         2.497
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.697
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4433
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1372 before and 0.1069 after correction. The Ratio of minimum to maximum transmission is 0.5946. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.085
_exptl_crystal_description       block
_exptl_crystal_F_000             1942
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.891
_refine_diff_density_min         -1.325
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
;
 Flack x determined using 4257 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.079(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         11693
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0663
_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^)+(0.1289P)^2^+1.9347P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1837
_refine_ls_wR_factor_ref         0.1905
_reflns_Friedel_coverage         0.882
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.980
_reflns_number_gt                10197
_reflns_number_total             11693
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc00897d2.cif
_cod_data_source_block           ld3056c115mm_0m
_cod_depositor_comments          'Adding full bibliography for 7126797.cif.'
_cod_original_cell_volume        5777.7(5)
_cod_database_code               7126797
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.973
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Restrained distances
 C22-C21 = C21-C26 = C25-C26 = C24-C25 = C24-C23 = C23-C22
 1.395 with sigma of 0.002
 C21-C23 = C23-C25
 2.45 with sigma of 0.002
 C24-C22 = C22-C26
 2.45 with sigma of 0.002
 C20-C21 = C20-C19 = C19-C18
 1.52 with sigma of 0.02
 C16A-C11 = C16A-C15A = C15A-C14 = C14B-C14 = C14B-C15B = C15B-C11 = C12B-C11 =
  C12A-C11 = C12A-C13A = C13B-C12B = C13B-C14 = C13A-C14
 1.395 with sigma of 0.002
 C5-C4 = C9-C4 = C8-C9 = C8-C7 = C6-C7 = C6-C5
 1.395 with sigma of 0.002
 C4-C6 = C6-C8
 2.45 with sigma of 0.002
 C7-C5 = C5-C9
 2.45 with sigma of 0.002
 C5-C4 = C9-C4 = C9-C8 = C8-C7 = C7-C6 = C6-C5
 1.395 with sigma of 0.002
3. Restrained planarity
 C21, C26, C25, C24, C23, C22
 with sigma of 0.002
 C4, C5, C9, C7, C6, C8
 with sigma of 0.002
 C13A, C12A, C14, C15A, C16A, C11
 with sigma of 0.02
 C4, C5, H5, C9, H9, C7, H7, C6, H6, C8, H8
 with sigma of 0.02
4. Others
 Fixed Sof: C15B(0.5) H15B(0.5) C12B(0.5) H12B(0.5) C14B(0.5) H14B(0.5)
 C13B(0.5) H13B(0.5) C13A(0.5) H13A(0.5) C12A(0.5) H12A(0.5) C15A(0.5)
 H15A(0.5) C16A(0.5) H16A(0.5)
5.a Ternary CH refined with riding coordinates:
 C2(H2A), C19(H19)
5.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C20(H20A,H20B)
5.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N1(H1), C31(H31), C27(H27), C30(H30), C28(H28), C26(H26), C22(H22),
 C23(H23), C15B(H15B), C25(H25), C24(H24), C5(H5), C12B(H12B), C9(H9),
 C14B(H14B), C7(H7), C13B(H13B), C13A(H13A), C12A(H12A), C15A(H15A), C16A(H16A),
  C6(H6), C8(H8)
;
_shelx_res_checksum              59254
_shelx_fab_checksum              12780
_olex2_submission_special_instructions 'No special instructions were received'