Homochiral hybrid hexagonal antiperovskite crystals [R- and S-3-chloroquinuclidinium]3(CdCl3)(CdCl4)
Xu, Zhe-Kun; Zhang, Jia-Mei; Wang, Zhong-Xia; CrystEngComm 26 (2024) 3874–3879; doi:10.1039/D4CE00504J

data_7248829
_publ_section_title
;
 Homochiral hybrid hexagonal antiperovskite crystals [R- and
 S-3-chloroquinuclidinium]3(CdCl3)(CdCl4)
;
_journal_issue                   28
_journal_name_full               CrystEngComm
_journal_page_first              3874
_journal_page_last               3879
_journal_paper_doi               10.1039/D4CE00504J
_journal_volume                  26
_journal_year                    2024
_chemical_absolute_configuration syn
_chemical_formula_moiety         'Cd1 Cl4, Cd1 Cl3, 3(C7 H13 Cl N)'
_chemical_formula_sum            'C21 H39 Cd2 Cl10 N3'
_chemical_formula_weight         912.85
_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_Hall           'P 6c'
_space_group_name_H-M_alt        'P 63'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2024-05-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2024-05-18 deposited with the CCDC.	2024-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   16.8561(13)
_cell_length_b                   16.8561(13)
_cell_length_c                   6.8554(5)
_cell_measurement_reflns_used    2053
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.9880
_cell_measurement_theta_min      2.4170
_cell_volume                     1686.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.60a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.970
_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     -5.00  32.00   0.50    8.00    --   20.00  54.00 150.00   74
  2  \w     73.00 101.00   0.50    8.00    --   20.00  54.00 150.00   56
  3  \w    -72.00  -6.00   0.50    8.00    --   20.00  54.00   0.00  132
  4  \w     -2.00  98.00   0.50    8.00    --   20.00  54.00   0.00  200
  5  \w    -57.00 -31.00   0.50    8.00    --   20.00  54.00-150.00   52
  6  \w     72.00 109.00   0.50    8.00    --   20.00  54.00-150.00   74
  7  \w    -45.00 -19.00   0.50    8.00    --   20.00  54.00 150.00   52
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0120398000
_diffrn_orient_matrix_UB_12      0.0466570000
_diffrn_orient_matrix_UB_13      0.0070983000
_diffrn_orient_matrix_UB_21      -0.0456519000
_diffrn_orient_matrix_UB_22      -0.0134489000
_diffrn_orient_matrix_UB_23      0.0270674000
_diffrn_orient_matrix_UB_31      0.0115997000
_diffrn_orient_matrix_UB_32      0.0003712000
_diffrn_orient_matrix_UB_33      0.0996075000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0619
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            9201
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.176
_diffrn_reflns_theta_min         2.417
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.071
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.60a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.797
_exptl_crystal_description       needle
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.913
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details
;
 Flack x determined using 871 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.08(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         3145
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0514P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.1044
_reflns_Friedel_coverage         0.802
_reflns_Friedel_fraction_full    0.964
_reflns_Friedel_fraction_max     0.907
_reflns_number_gt                2388
_reflns_number_total             3145
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00504j2.cif
_cod_data_source_block           R-1
_cod_depositor_comments
'Adding full bibliography for 7248826--7248829.cif.'
_cod_original_cell_volume        1686.9(3)
_cod_database_code               7248829
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C N H Cd Cl'
_shelx_estimated_absorpt_t_max   0.820
_shelx_estimated_absorpt_t_min   0.491
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Ternary CH refined with riding coordinates:
 C7(H7), N1(H1), C4(H4)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C3(H3A,H3B), C1(H1A,H1B), C2(H2A,H2B)
;
_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 1.085
_oxdiff_exptl_absorpt_empirical_full_min 0.919