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_7247362
_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         'C39 H39 Cd3 N3 O15'
_chemical_formula_sum            'C39 H39 Cd3 N3 O15'
_chemical_formula_weight         1126.93
_chemical_melting_point          ?
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-12-22
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-06 deposited with the CCDC.	2023-09-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5668(3)
_cell_length_b                   23.3692(6)
_cell_length_c                   17.0992(3)
_cell_measurement_reflns_used    226
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      72.3980
_cell_measurement_theta_min      5.9860
_cell_volume                     3822.84(17)
_computing_cell_refinement       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5861
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -21.00  37.00   1.00    1.00    --  -40.07  38.00-120.00   58
  2  \w   -116.00 -69.00   1.00    1.00    --  -40.07-138.00 174.00   47
  3  \w    -21.00  37.00   1.00    1.00    --  -40.07  38.00  90.00   58
  4  \w      6.00  82.00   1.00    1.00    --   40.07 -99.00  90.00   76
  5  \w     61.00 131.00   1.00    1.00    --   40.07 178.00 -30.00   70
  6  \w     30.00 178.00   1.00    4.00    --  107.62  15.00-180.00  148
  7  \w     31.00 109.00   1.00    4.00    --  107.62-112.00 -90.00   78
  8  \w     31.00  72.00   1.00    4.00    --  107.62 -45.00   0.00   41
  9  \w     31.00  93.00   1.00    4.00    --  107.62 -61.00-120.00   62
 10  \w     28.00  57.00   1.00    4.00    --  107.62 -30.00 -60.00   29
 11  \w    104.00 178.00   1.00    4.00    --  107.62 112.00  90.00   74
 12  \w     28.00  57.00   1.00    4.00    --  107.62 -30.00-120.00   29
 13  \w     31.00  72.00   1.00    4.00    --  107.62 -45.00 -90.00   41
 14  \w     23.00 106.00   1.00    4.00    --  107.62 -95.00  30.00   83
 15  \w   -116.00 -84.00   1.00    1.00    --  -40.07 -57.00  90.00   32
 16  \w   -116.00  -9.00   1.00    1.00    --  -40.07 -57.00 -60.00  107
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0583366000
_diffrn_orient_matrix_UB_12      -0.0183771000
_diffrn_orient_matrix_UB_13      0.0600268000
_diffrn_orient_matrix_UB_21      -0.1314252000
_diffrn_orient_matrix_UB_22      0.0360989000
_diffrn_orient_matrix_UB_23      0.0273936000
_diffrn_orient_matrix_UB_31      -0.0723412000
_diffrn_orient_matrix_UB_32      -0.0804904000
_diffrn_orient_matrix_UB_33      -0.0013699000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1205
_diffrn_reflns_av_unetI/netI     0.1091
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19674
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.478
_diffrn_reflns_theta_min         2.584
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.928
_exptl_absorpt_correction_T_max  0.307
_exptl_absorpt_correction_T_min  0.079
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.67a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.958
_exptl_crystal_description       block
_exptl_crystal_F_000             2232
_exptl_crystal_recrystallization_method 'Solvothermal reaction'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.043
_refine_diff_density_max         1.835
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.202
_refine_ls_abs_structure_details
;
 Flack x determined using 1975 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.026(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         7285
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0621P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1182
_refine_ls_wR_factor_ref         0.1266
_reflns_Friedel_coverage         0.747
_reflns_Friedel_fraction_full    0.965
_reflns_Friedel_fraction_max     0.935
_reflns_number_gt                5623
_reflns_number_total             7285
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00784g1.cif
_cod_data_source_block           cjk22_s2577_sn952_auto
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7247360--7247362.cif.
;
_cod_original_cell_volume        3822.85(16)
_cod_database_code               7247362
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C10 H10 N4 O3 Cd2'
_chemical_oxdiff_usercomment     10b
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C13(H13), C14(H14), C15(H15),
 C24(H24), C25(H25), C26(H26), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33),
  C35(H35)
2.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C19(H19), C37(H37)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C)
;
_shelx_res_checksum              87113
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.219
_oxdiff_exptl_absorpt_empirical_full_min 0.512