Bisphosphonium cation based metal halide glass scintillators with tunable melting points.
Luo, Jian-Bin; Wei, Jun-Hua; He, Zi-Lin; Chen, Jing-Hua; Peng, Qing-Peng; Zhang, Zhi-Zhong; Kuang, Dai-Bin; Chemical science 15 (2024) 16338–16346; doi:10.1039/d4sc04229h

data_1572573
_publ_section_title
;
 Bisphosphonium cation based metal halide glass scintillators with tunable
 melting points.
;
_journal_issue                   39
_journal_name_full               'Chemical science'
_journal_page_first              16338
_journal_page_last               16346
_journal_paper_doi               10.1039/d4sc04229h
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'Br4 Mn, C42 H42 P2'
_chemical_formula_sum            'C42 H42 Br4 Mn P2'
_chemical_formula_weight         983.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-26
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-04-18 deposited with the CCDC.	2024-09-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.908(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1667(7)
_cell_length_b                   13.9159(5)
_cell_length_c                   18.6147(8)
_cell_measurement_reflns_used    7926
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.9720
_cell_measurement_theta_min      1.9980
_cell_volume                     4006.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.94a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.94a 64-bit (release 20-10-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.94a (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 2018/2 (Sheldrick, 2018)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.809
_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    -30.00  11.00   0.50    0.50    --   -5.60  79.00  -8.00   82
  2  \w    -79.00   9.00   0.50    0.50    --   -5.60 -38.00 150.00  176
  3  \w    -18.00   9.00   0.50    0.50    --   -5.60 -99.00  90.00   54
  4  \w    -17.00  14.00   0.50    0.50    --   -5.60 -99.00  30.00   62
  5  \w     -8.00  40.00   0.50    0.50    --    6.38 -99.00   0.00   96
  6  \w    -18.00  40.00   0.50    0.50    --    6.38 -99.00 150.00  116
  7  \w    -14.00  17.00   0.50    0.50    --    6.38  79.00  -8.00   62
  8  \w    -24.00   2.00   0.50    0.50    --    6.38 -79.00-132.00   52
;
_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      0.0407263000
_diffrn_orient_matrix_UB_12      0.0142044000
_diffrn_orient_matrix_UB_13      0.0242740000
_diffrn_orient_matrix_UB_21      0.0002634000
_diffrn_orient_matrix_UB_22      -0.0409210000
_diffrn_orient_matrix_UB_23      0.0227523000
_diffrn_orient_matrix_UB_31      0.0211507000
_diffrn_orient_matrix_UB_32      -0.0268324000
_diffrn_orient_matrix_UB_33      -0.0218707000
_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  0.0470
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.809
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23506
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.809
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.901
_diffrn_reflns_theta_min         1.969
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.427
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55257
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.94a (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    1.630
_exptl_crystal_description       block
_exptl_crystal_F_000             1956
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         5132
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0300
_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^)+(0.0226P)^2^+2.1084P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0563
_refine_ls_wR_factor_ref         0.0602
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4008
_reflns_number_total             5132
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04229h2.cif
_cod_data_source_block           9962-1_auto
_cod_depositor_comments
'Adding full bibliography for 1572573--1572580.cif.'
_cod_database_code               1572573
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         CHOMnBr
_shelx_estimated_absorpt_t_max   0.666
_shelx_estimated_absorpt_t_min   0.666
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C1(H1A,H1B), C15(H15A,H15B)
1.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C10(H10), C14(H14), C17(H17), C12(H12), C4(H4), C18(H18), C20(H20),
 C11(H11), C6(H6), C13(H13), C5(H5), C7(H7), C8(H8), C19(H19)
;
_shelx_res_checksum              90027
_shelx_hkl_checksum              19875
_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 1.809
_oxdiff_exptl_absorpt_empirical_full_min 0.640