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_7248828
_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 rm
_chemical_formula_moiety         'Cl, C7 H13 Cl N'
_chemical_formula_sum            'C7 H13 Cl2 N'
_chemical_formula_weight         182.08
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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                90
_cell_formula_units_Z            4
_cell_length_a                   8.3125(9)
_cell_length_b                   9.4931(9)
_cell_length_c                   11.6083(11)
_cell_measurement_reflns_used    1379
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.5720
_cell_measurement_theta_min      3.0020
_cell_volume                     916.03(16)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.971
_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     58.00  85.00   0.50    1.00    --   20.00  54.00-120.00   54
  2  \w    -73.00 -29.00   0.50    1.00    --   20.00  54.00-180.00   88
  3  \w      7.00  33.00   0.50    1.00    --   20.00  54.00-180.00   52
  4  \w     48.00  80.00   0.50    1.00    --   20.00  54.00-180.00   64
  5  \w    -74.00   2.00   0.50    1.00    --   20.00  54.00  90.00  152
  6  \w     11.00  57.00   0.50    1.00    --   20.00  54.00  90.00   92
  7  \w     51.00  76.00   0.50    1.00    --   20.00  54.00 -30.00   50
  8  \w    -72.00  36.00   0.50    1.00    --   20.00  54.00-120.00  216
;
_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      0.0670270000
_diffrn_orient_matrix_UB_12      0.0461914000
_diffrn_orient_matrix_UB_13      0.0031403000
_diffrn_orient_matrix_UB_21      0.0059410000
_diffrn_orient_matrix_UB_22      -0.0127129000
_diffrn_orient_matrix_UB_23      0.0600610000
_diffrn_orient_matrix_UB_31      0.0525000000
_diffrn_orient_matrix_UB_32      -0.0573233000
_diffrn_orient_matrix_UB_33      -0.0107614000
_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  0.0395
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5864
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.902
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.919
_diffrn_reflns_theta_min         2.772
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.639
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62847
_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    1.320
_exptl_crystal_description       block
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.200
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Flack x determined using 513 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         2394
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0487
_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^)+(0.0708P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1255
_refine_ls_wR_factor_ref         0.1381
_reflns_Friedel_coverage         0.603
_reflns_Friedel_fraction_full    0.932
_reflns_Friedel_fraction_max     0.808
_reflns_number_gt                1680
_reflns_number_total             2394
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00504j2.cif
_cod_data_source_block           R-TCQ_HCl
_cod_depositor_comments
'Adding full bibliography for 7248826--7248829.cif.'
_cod_database_code               7248828
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H N Cl'
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.883
_reflns_odcompleteness_completeness 100.00
_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
2.a Ternary CH refined with riding coordinates:
 C4(H4), C7(H7)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C1(H1A,H1B), C3(H3A,H3B), C6(H6A,H6B), C5(H5A,H5B)
;
_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 1.415
_oxdiff_exptl_absorpt_empirical_full_min 0.833