An anti-thermal-quenching organic–inorganic hybrid manganese-based single-crystal scintillator for high-temperature X-ray imaging
Chen, Jing-Hua; Luo, Jian-Bin; He, Zi-Lin; Peng, Qing-Peng; Wei, Jun-Hua; Zhang, Zhi-Zhong; Guo, Xiu-Xian; Kuang, Dai-Bin; Chemical Science 16 (2025) 9375–9384; doi:10.1039/D4SC08499C

data_1575039
_publ_section_title
;
 An anti-thermal-quenching organic--inorganic hybrid manganese-based
 single-crystal scintillator for high-temperature X-ray imaging
;
_journal_issue                   21
_journal_name_full               'Chemical Science'
_journal_page_first              9375
_journal_page_last               9384
_journal_paper_doi               10.1039/D4SC08499C
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         '2(Br), C22 H26 N P'
_chemical_formula_sum            'C22 H26 Br2 N P'
_chemical_formula_weight         495.23
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-03-16
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-08-23 deposited with the CCDC.	2025-04-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.8011(10)
_cell_length_b                   13.8575(10)
_cell_length_c                   26.5401(17)
_cell_measurement_reflns_used    4264
_cell_measurement_temperature    149.98(10)
_cell_measurement_theta_max      26.4270
_cell_measurement_theta_min      2.9330
_cell_volume                     4340.2(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.92a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.92a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.92a (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 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.98(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2913
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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   -107.00 -71.00   1.00   90.00    --  -18.96-178.00 -60.00   36
  2  \w    -42.00  18.00   1.00   90.00    --   19.90 -77.00 -60.00   60
  3  \w    -31.00  21.00   1.00   90.00    --   19.90 -77.00-180.00   52
  4  \w   -104.00 -69.00   1.00   90.00    --  -18.96 178.00   0.00   35
  5  \w     11.00  78.00   1.00   90.00    --   19.90  38.00  60.00   67
  6  \w    -37.00 -11.00   1.00   90.00    --   19.90 -77.00  60.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0292503000
_diffrn_orient_matrix_UB_12      0.0031647000
_diffrn_orient_matrix_UB_13      0.0232887000
_diffrn_orient_matrix_UB_21      -0.0371597000
_diffrn_orient_matrix_UB_22      -0.0348318000
_diffrn_orient_matrix_UB_23      0.0105137000
_diffrn_orient_matrix_UB_31      0.0371107000
_diffrn_orient_matrix_UB_32      -0.0373671000
_diffrn_orient_matrix_UB_33      -0.0078279000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0826
_diffrn_reflns_av_unetI/netI     0.1061
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            26678
_diffrn_reflns_point_group_measured_fraction_full 0.920
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         2.393
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           3.57
_diffrn_source_power             0.24947159999999996
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_source_voltage           69.88
_exptl_absorpt_coefficient_mu    3.815
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69397
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.92a (Rigaku Oxford Diffraction, 2023)
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    1.516
_exptl_crystal_description       block
_exptl_crystal_F_000             2000
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details
;
 Flack x determined using 2010 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.031(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         8723
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0534
_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^)+(0.0208P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0999
_reflns_Friedel_coverage         0.782
_reflns_Friedel_fraction_full    0.837
_reflns_Friedel_fraction_max     0.817
_reflns_number_gt                6547
_reflns_number_total             8723
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc08499c2.cif
_cod_data_source_block           a24031215a0084
_cod_database_code               1575039
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         CHNBrP
_chemical_oxdiff_usercomment     1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C21(H21A,H21B), C00D(H00D,H00E), C00G(H00H,H00I), C00M(H00V,
 H00W), C00T(H00,H), C00V(H00M,H00O), C013(H01A,H01B)
2.b Aromatic/amide H refined with riding coordinates:
 C00E(H00F), C00F(H00G), C00H(H00T), C00I(H00U), C00J(H00J), C00K(H00K),
 C00L(H00L), C00N(H00N), C00O(H00X), C00Q(H00Y), C00R(H00Z), C00S(H00S),
 C00U(H1), C00X(H2), C00Y(H3), C00Z(H4), C012(H012), C014(H014), C015(H015),
 C016(H016), C017(H017), C018(H018), C019(H019), C01A(H01H), C01B(H01C),
 C01C(H01I), C01D(H01D), C01E(H01E), C01F(H01F), C01G(H01G)
2.c Idealised Me refined as rotating group:
 N007(H00P,H00Q,H00R), N008(H00A,H00B,H00C)
;
_shelx_res_checksum              66829
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.543
_oxdiff_exptl_absorpt_empirical_full_min 0.708