Spontaneous resolution of two chiral metal–organic frameworks through local geometric and lattice frustration effects
Windsor, Hunter J.; Kepert, Cameron J.; Macreadie, Lauren K.; CrystEngComm 25 (2023) 5428–5435; doi:10.1039/D3CE00784G

data_7247361
_publ_section_title
;
 Spontaneous resolution of two chiral metal--organic frameworks through
 local geometric and lattice frustration effects
;
_journal_issue                   38
_journal_name_full               CrystEngComm
_journal_page_first              5428
_journal_page_last               5435
_journal_paper_doi               10.1039/D3CE00784G
_journal_volume                  25
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C10 H13 Cd N O5'
_chemical_formula_sum            'C10 H13 Cd N O5'
_chemical_formula_weight         339.61
_space_group_crystal_system      hexagonal
_space_group_IT_number           170
_space_group_name_Hall           'P 65'
_space_group_name_H-M_alt        'P 65'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-04-15
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-04-16 deposited with the CCDC.	2023-09-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   9.3938(3)
_cell_length_b                   9.3938(3)
_cell_length_c                   22.5064(8)
_cell_measurement_reflns_used    8860
_cell_measurement_temperature    100.02
_cell_measurement_theta_max      33.13
_cell_measurement_theta_min      2.50
_cell_volume                     1719.96(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.02
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0606
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            14182
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.144
_diffrn_reflns_theta_min         2.504
_diffrn_source                   'FR591 rotating anode'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.913
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.5385
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1355 before and 0.0788 after correction.
The Ratio of minimum to maximum transmission is 0.7214.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.967
_exptl_crystal_description       prism
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details
;
 Flack x determined using 1652 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.06(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         4334
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0277
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+0.1434P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0465
_refine_ls_wR_factor_ref         0.0474
_reflns_Friedel_coverage         0.939
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                4014
_reflns_number_total             4334
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00784g1.cif
_cod_data_source_block           s2532_2
_cod_depositor_comments
'Adding full bibliography for 7247360--7247362.cif.'
_cod_original_cell_volume        1719.96(13)
_cod_database_code               7247361
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C4B-C2 \\sim C4A-C2 \\sim C6-C4B \\sim C6-C4A \\sim C6-C5A \\sim C6-C5B \\sim
C6-C3A \\sim C6-C3B \\sim C3B-
 C2 \\sim C3A-C2 \\sim C5B-C2 \\sim C5A-C2
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C5A) = Uanis(C5B)
Uanis(C3B) = Uanis(C3A)
Uanis(C4A) = Uanis(C4B)
4. Others
 Sof(C5B)=Sof(H5BA)=Sof(H5BB)=Sof(C4B)=Sof(H4BA)=Sof(H4BB)=Sof(C3B)=Sof(H3BA)=
 Sof(H3BB)=1-FVAR(1)
 Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(C3A)=Sof(H3AA)=
 Sof(H3AB)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C5A(H5AA,H5AB), C4A(H4AA,H4AB), C3A(H3AA,H3AB), C5B(H5BA,H5BB), C4B(H4BA,
 H4BB), C3B(H3BA,H3BB)
5.b Aromatic/amide H refined with riding coordinates:
 C8(H8)
5.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              5018
_olex2_submission_special_instructions 'No special instructions were received'