Aggregation-induced emission organic metal halide complex for X-ray scintillation.
Shonde, Tunde Blessed; Liu, He; Olasupo, Oluwadara Joshua; Bouchard, Alexander; Bouchard, Sara; Franklin, Annaliese; Lin, Xinsong; Stand, Luis M.; Ma, Biwu; Materials horizons 11 (2024) 3076–3081; doi:10.1039/d4mh00142g

data_1571437
_publ_section_title
;
 Aggregation-induced emission organic metal halide complex for X-ray
 scintillation.
;
_journal_issue                   13
_journal_name_full               'Materials horizons'
_journal_page_first              3076
_journal_page_last               3081
_journal_paper_doi               10.1039/d4mh00142g
_journal_volume                  11
_journal_year                    2024
_chemical_formula_moiety         'C46 H36 Cl2 N4 Zn'
_chemical_formula_sum            'C46 H36 Cl2 N4 Zn'
_chemical_formula_weight         781.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-08-19
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_audit_update_record
;
2023-06-06 deposited with the CCDC.	2024-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.6460(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.9901(3)
_cell_length_b                   11.7699(2)
_cell_length_c                   15.3428(2)
_cell_measurement_reflns_used    28286
_cell_measurement_temperature    149.95(15)
_cell_measurement_theta_max      77.7220
_cell_measurement_theta_min      4.1790
_cell_volume                     3804.63(10)
_computing_cell_refinement       'CrysAlisPro 1.171.42.61a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.61a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.61a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.95(15)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.942
_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  24.00   0.50    0.99    --  -48.74  55.00 -97.00  132
  2  \w   -121.00 -35.00   0.50    0.99    --  -48.74 -55.00 119.00  172
  3  \w    -22.00  62.00   0.50    0.99    --   48.74 -55.00 119.00  168
  4  \w     36.00 121.00   0.50    0.99    --   48.74  55.00 -97.00  170
  5  \w   -158.00 -73.00   0.50    4.50    --  -86.25 -55.00 119.00  170
  6  \w    -42.00 -14.00   0.50    4.50    --  -86.25  55.00 -97.00   56
  7  \w     95.00 178.00   0.50    4.50    --  107.75  55.00 -97.00  166
  8  \w     36.00  84.00   0.50    4.50    --  107.75 -55.00 119.00   96
  9  \w   -118.00 -87.00   0.50    0.99    --  -48.74-125.00-120.00   62
 10  \w   -118.00 -87.00   0.50    0.99    --  -48.74-125.00   0.00   62
 11  \w    -19.00  24.00   0.50    0.99    --  -48.74  37.00  30.00   86
 12  \w    -19.00  24.00   0.50    0.99    --  -48.74  37.00  60.00   86
 13  \w     36.00  71.00   0.50    4.50    --  107.75 -45.00-180.00   70
 14  \w     36.00  71.00   0.50    4.50    --  107.75 -45.00 -30.00   70
 15  \w     36.00 166.00   0.50    4.50    --  107.75   0.00  30.00  260
 16  \w     36.00 106.00   0.50    4.50    --  107.75 -94.00  60.00  140
 17  \w     36.00 166.00   0.50    4.50    --  107.75   0.00-180.00  260
 18  \w     36.00 106.00   0.50    4.50    --  107.75 -94.00-150.00  140
 19  \w     93.00 178.00   0.50    4.50    --  107.75  61.00-180.00  170
 20  \w    100.00 164.00   0.50    4.50    --  107.75   0.00 -90.00  128
 21  \w     36.00  94.00   0.50    4.50    --  107.75 -61.00 -30.00  116
 22  \w     36.00  74.00   0.50    4.50    --  107.75 -61.00  60.00   76
 23  \w     97.00 139.00   0.50    4.50    --  107.75  45.00 150.00   84
 24  \w     46.00  71.00   0.50    4.50    --  107.75 -45.00  60.00   50
 25  \w     50.00  93.00   0.50    4.50    --  107.75 -61.00-180.00   86
 26  \w     36.00  61.00   0.50    4.50    --  107.75 -45.00-150.00   50
 27  \w    129.00 177.00   0.50    4.50    --  107.75  15.00  30.00   96
 28  \w    126.00 178.00   0.50    4.50    --  107.75  45.00-150.00  104
 29  \w     44.00  71.00   0.50    4.50    --  107.75 -45.00   0.00   54
 30  \w     36.00  67.00   0.50    4.50    --  107.75 -45.00 -60.00   62
 31  \w    140.00 174.00   0.50    4.50    --  107.75 125.00  90.00   68
 32  \w     56.00 105.00   0.50    4.50    --  107.75 -94.00 120.00   98
 33  \w     36.00  68.00   0.50    4.50    --  107.75 -45.00 -90.00   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0028671000
_diffrn_orient_matrix_UB_12      -0.0844334000
_diffrn_orient_matrix_UB_13      -0.0778645000
_diffrn_orient_matrix_UB_21      0.0721747000
_diffrn_orient_matrix_UB_22      -0.0190971000
_diffrn_orient_matrix_UB_23      0.0369286000
_diffrn_orient_matrix_UB_31      -0.0115750000
_diffrn_orient_matrix_UB_32      -0.0981681000
_diffrn_orient_matrix_UB_33      0.0595905000
_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  0.0623
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            46301
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         82.935
_diffrn_reflns_theta_min         4.303
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.483
_exptl_absorpt_correction_T_max  0.620
_exptl_absorpt_correction_T_min  0.059
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.61a (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_description       plate
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.457
_exptl_crystal_size_mid          0.279
_exptl_crystal_size_min          0.029
_refine_diff_density_max         1.064
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         8007
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0471
_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^)+(0.1005P)^2^+0.7619P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1334
_refine_ls_wR_factor_ref         0.1378
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7337
_reflns_number_total             8007
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4mh00142g2.cif
_cod_data_source_block           tpapy-zncl-lc_auto
_cod_depositor_comments          'Adding full bibliography for 1571437.cif.'
_cod_database_code               1571437
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         CHNZnCl
_chemical_oxdiff_usercomment     150
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.397
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13),
 C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22),
  C23(H23), C24(H24), C25(H25), C27(H27), C28(H28), C30(H30), C31(H31),
 C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C42(H42),
  C43(H43), C44(H44), C45(H45), C46(H46)
;
_shelx_res_checksum              89034
_shelx_hkl_checksum              6530
_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 2.344
_oxdiff_exptl_absorpt_empirical_full_min 0.292