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_1575044
_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         'Br4 Mn, C22 H26 N P'
_chemical_formula_sum            'C22 H26 Br4 Mn N P'
_chemical_formula_weight         709.99
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-04-15
_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                105.646(2)
_cell_angle_beta                 95.716(2)
_cell_angle_gamma                93.676(2)
_cell_formula_units_Z            2
_cell_length_a                   8.5137(2)
_cell_length_b                   12.2993(4)
_cell_length_c                   12.7994(3)
_cell_measurement_reflns_used    12078
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      32.2840
_cell_measurement_theta_min      3.0740
_cell_volume                     1278.38(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      149.99(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 0.917
_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    -42.00  13.00   1.00   10.00    --  -19.11 -77.00  90.00   55
  2  \w   -108.00 -61.00   1.00   10.00    --  -19.11-178.00 -60.00   47
  3  \w   -108.00 -61.00   1.00   10.00    --  -19.11-178.00 120.00   47
  4  \w    -42.00  13.00   1.00   10.00    --  -19.11 -77.00-120.00   55
  5  \w    -68.00 108.00   1.00   10.00    --   19.74   0.00-180.00  176
  6  \w    -55.00  44.00   1.00   10.00    --   19.74 -38.00 -90.00   99
  7  \w    -21.00 100.00   1.00   10.00    --   19.74  19.00  90.00  121
  8  \w    -42.00  13.00   1.00   10.00    --  -19.11 -77.00  30.00   55
  9  \w    -93.00   5.00   1.00   10.00    --  -19.11 -38.00 -90.00   98
 10  \w    -15.00  10.00   1.00   10.00    --   19.74 -99.00 -30.00   25
 11  \w    -15.00  60.00   1.00   10.00    --   19.74 -99.00  30.00   75
 12  \w    -15.00  35.00   1.00   10.00    --   19.74 -99.00 120.00   50
;
_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      0.0125891000
_diffrn_orient_matrix_UB_12      -0.0580612000
_diffrn_orient_matrix_UB_13      -0.0197044000
_diffrn_orient_matrix_UB_21      0.0685055000
_diffrn_orient_matrix_UB_22      0.0085967000
_diffrn_orient_matrix_UB_23      0.0387107000
_diffrn_orient_matrix_UB_31      -0.0471475000
_diffrn_orient_matrix_UB_32      -0.0132031000
_diffrn_orient_matrix_UB_33      0.0384035000
_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  0.0435
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            35977
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.951
_diffrn_reflns_theta_min         2.415
_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    6.840
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42105
_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    1.844
_exptl_crystal_description       block
_exptl_crystal_F_000             690
_refine_diff_density_max         0.620
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       0.00051(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         8800
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0271P)^2^+0.2564P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0711
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7047
_reflns_number_total             8800
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc08499c2.cif
_cod_data_source_block           a24031401a0084_auto
_cod_database_code               1575044
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         PCHNBrMn
_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:
 C009(H00D,H00E), C00A(H00F,H00G), C00H(H00L,H00M), C00M(H00R,H00S)
2.b Aromatic/amide H refined with riding coordinates:
 C00B(H00H), C00C(H00I), C00D(H00J), C00G(H00K), C00I(H00N), C00J(H00O),
 C00K(H00P), C00L(H00Q), C00N(H00T), C00O(H00U), C00P(H00V), C00Q(H00W),
 C00R(H00X), C00S(H00Y), C00T(H00Z)
2.c Idealised Me refined as rotating group:
 N007(H00A,H00B,H00C)
;
_shelx_res_checksum              24934
_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 1.846
_oxdiff_exptl_absorpt_empirical_full_min 0.712