Ultrafast preparation of amine-free 0D metal halides with near-unity emission for X-ray scintillators.
Li, Hao; Wang, Zhaoyu; Wu, Junhong; Zhang, Tianyong; Long, Guankui; Jiang, Shuang; Nanoscale 17 (2025) 27474–27481; doi:10.1039/d5nr03995a

data_1576134
_publ_section_title
;
 Ultrafast preparation of amine-free 0D metal halides with near-unity
 emission for X-ray scintillators.
;
_journal_issue                   47
_journal_name_full               Nanoscale
_journal_page_first              27474
_journal_page_last               27481
_journal_paper_doi               10.1039/d5nr03995a
_journal_volume                  17
_journal_year                    2025
_chemical_formula_moiety         'Cl6 Sb, C12 H36 Al O6 S6'
_chemical_formula_sum            'C12 H36 Al Cl6 O6 S6 Sb'
_chemical_formula_weight         830.20
_chemical_name_systematic        CCD
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-06-09
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7224)
;
_audit_update_record
;
2025-09-22 deposited with the CCDC.	2025-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   13.4727(4)
_cell_length_b                   13.4727(4)
_cell_length_c                   15.2171(4)
_cell_measurement_reflns_used    2443
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.8810
_cell_measurement_theta_min      4.7660
_cell_volume                     2392.06(12)
_computing_cell_refinement       'CrysAlisPro 1.171.42.99a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.99a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.99a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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     33.00 106.00   0.50    0.05    --  105.43 -77.00  90.00  146
  2  \w     34.00  75.00   0.50    0.05    --  105.43 -61.00-120.00   82
  3  \w     36.00  92.00   0.50    0.05    --  105.43 -71.00-119.00  112
  4  \w    -10.00  15.00   0.50    0.05    --  -47.26  19.00-180.00   50
  5  \w    -60.00 -35.00   0.50    0.05    -- -104.50  61.00-180.00   50
  6  \w    -68.00 -37.00   0.50    0.05    -- -104.50  61.00 -90.00   62
  7  \w    -22.00  25.00   0.50    0.05    --  -47.26  19.00 120.00   94
  8  \w    -41.00  26.00   0.50    0.05    --  -47.26  95.00 107.00  134
  9  \w   -170.00-138.00   0.50    0.05    -- -104.50 -45.00 120.00   64
 10  \w   -164.00-137.00   0.50    0.05    -- -104.50 -31.00 125.00   54
 11  \w   -131.00 -95.00   0.50    0.05    -- -104.50 -31.00 125.00   72
 12  \w   -133.00-108.00   0.50    0.05    -- -104.50 -45.00 120.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0616174000
_diffrn_orient_matrix_UB_12      0.0470123000
_diffrn_orient_matrix_UB_13      0.0572734000
_diffrn_orient_matrix_UB_21      0.0851221000
_diffrn_orient_matrix_UB_22      0.0222837000
_diffrn_orient_matrix_UB_23      0.0753394000
_diffrn_orient_matrix_UB_31      0.0799582000
_diffrn_orient_matrix_UB_32      0.1212539000
_diffrn_orient_matrix_UB_33      -0.0359644000
_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  0.1518
_diffrn_reflns_av_unetI/netI     0.0923
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            2129
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        66.506
_diffrn_reflns_theta_max         66.506
_diffrn_reflns_theta_min         6.571
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.665
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.03932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.99a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_description       block
_exptl_crystal_F_000             1254
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.033
_refine_diff_density_min         -0.014
_refine_diff_density_rms         0.002
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.287
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     55
_refine_ls_number_reflns         914
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.315
_refine_ls_R_factor_all          0.1164
_refine_ls_R_factor_gt           0.1119
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2727
_refine_ls_wR_factor_ref         0.2770
_reflns_Friedel_coverage         0.000
_reflns_number_gt                885
_reflns_number_total             914
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nr03995a4.cif
_cod_data_source_block           p20250607tju4_auto
_cod_depositor_comments          'Adding full bibliography for 1576134.cif.'
_cod_original_cell_volume        2392.06(16)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               1576134
_shelx_shelxl_version_number     2014/7
_cell_oxdiff_angle_alpha         90.037(3)
_cell_oxdiff_angle_beta          90.010(3)
_cell_oxdiff_angle_gamma         119.940(4)
_cell_oxdiff_length_a            13.4640(6)
_cell_oxdiff_length_b            13.4740(5)
_cell_oxdiff_length_c            15.2164(6)
_cell_oxdiff_measurement_reflns_used 2569
_cell_oxdiff_volume              2392.07(16)
_shelx_estimated_absorpt_t_max   0.303
_shelx_estimated_absorpt_t_min   0.303
_diffrn_oxdiff_digest_hkl
;
01fd4943dbd8559bbf8b7b0fb1b9c2a4951fe8
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9987(3)
 0.0013(3)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 S002, C007
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(Sb01) \\sim Ueq, Uanis(C007) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.001
5.a Idealised Me refined as rotating group:
 C006(H00A,H00B,H00C), C007(H00D,H00E,H00F)
;
_shelx_res_checksum              58552
_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 8.490
_oxdiff_exptl_absorpt_empirical_full_min 0.239