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_1572579
_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, C43 H44 P2'
_chemical_formula_sum            'C43 H44 Br4 Mn P2'
_chemical_formula_weight         997.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_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                 102.6600(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.01730(10)
_cell_length_b                   13.33120(10)
_cell_length_c                   27.3180(3)
_cell_measurement_reflns_used    35417
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      76.8890
_cell_measurement_theta_min      3.3010
_cell_volume                     4270.08(7)
_computing_cell_refinement       'CrysAlisPro 1.171.43.94a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.94a (Rigaku OD, 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_temperature      293(2)
_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 1.000
_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   -177.00 -89.00   0.50    1.00    -- -104.98 -34.00 101.00  176
  2  \w    -71.00 -32.00   0.50    1.00    -- -104.98  61.00 120.00   78
  3  \w   -114.00 -34.00   0.50    1.00    -- -104.98 128.00 121.00  160
  4  \w    -22.00  78.00   0.50    0.20    --   49.71 -88.00 -65.00  200
  5  \w     35.00 137.00   0.50    1.00    --  108.10 -88.00 -65.00  204
  6  \w     74.00 120.00   0.50    0.20    --   49.71 125.00  90.00   92
  7  \w     74.00 120.00   0.50    0.20    --   49.71 125.00   0.00   92
  8  \w     74.00 120.00   0.50    0.20    --   49.71 125.00 -30.00   92
  9  \w     41.00  67.00   0.50    1.00    --  108.10 -61.00  90.00   52
 10  \w     35.00 105.00   0.50    1.00    --  108.10 -77.00  60.00  140
 11  \w    -26.00  26.00   0.50    0.20    --   49.71 -19.00 150.00  104
 12  \w     35.00  71.00   0.50    1.00    --  108.10 -61.00   0.00   72
 13  \w     44.00 103.00   0.50    1.00    --  108.10 -77.00 -60.00  118
 14  \w     35.00  60.00   0.50    1.00    --  108.10 -61.00-180.00   50
 15  \w    -40.00 -13.00   0.50    0.20    --  -46.49  38.00  30.00   54
 16  \w    -91.00 -41.00   0.50    0.20    --  -46.49 125.00 150.00  100
 17  \w     80.00 117.00   0.50    0.20    --   49.62 125.00-150.00   74
 18  \w    -21.00  39.00   0.50    0.20    --   49.62 -38.00  30.00  120
 19  \w      6.00  40.00   0.50    0.20    --   49.62 -38.00 -60.00   68
 20  \w     77.00 112.00   0.50    0.20    --   49.62 125.00-120.00   70
 21  \w     83.00 109.00   0.50    0.20    --   49.62 125.00  30.00   52
 22  \w   -108.00 -81.00   0.50    1.00    -- -104.82 109.00  37.64   54
 23  \w   -124.00 -94.00   0.50    1.00    -- -104.82 142.00-104.89   60
 24  \w   -166.00-139.00   0.50    1.00    -- -104.82 -46.00-105.41   54
 25  \w   -124.00 -99.00   0.50    1.00    -- -104.82 141.00  85.97   50
 26  \w   -127.00-100.00   0.50    1.00    -- -104.82 -46.00-105.41   54
 27  \w   -175.00-102.00   0.50    1.00    -- -104.82 -46.00 -10.42  146
 28  \w    -62.00 -36.00   0.50    1.00    -- -104.82 143.00 156.38   52
 29  \w   -177.00 -87.00   0.50    1.00    -- -104.82 -65.00  23.65  180
 30  \w    -64.00 -32.00   0.50    1.00    -- -104.82 142.00-104.89   64
 31  \w   -124.00 -67.00   0.50    1.00    -- -104.82 143.00 156.38  114
 32  \w    -66.00 -39.00   0.50    1.00    -- -104.82  61.00   0.00   54
 33  \w    -82.00 -54.00   0.50    1.00    -- -104.82 141.00  85.97   56
 34  \w     38.00 108.00   0.50    1.00    --  107.94-125.00 -90.00  140
 35  \w     80.00 105.00   0.50    1.00    --  107.94 -77.00 -90.00   50
 36  \w     84.00 110.00   0.50    1.00    --  107.94-125.00  60.00   52
 37  \w    133.00 160.00   0.50    1.00    --  107.94  45.00  90.00   54
 38  \w     45.00  97.00   0.50    1.00    --  107.94-125.00 -60.00  104
 39  \w     46.00 100.00   0.50    1.00    --  107.94 -95.00  60.00  108
 40  \w     37.00  65.00   0.50    1.00    --  107.94 -61.00-120.00   56
 41  \w     91.00 178.00   0.50    1.00    --  107.94  61.00-180.00  174
 42  \w    120.00 174.00   0.50    1.00    --  107.94  61.00  60.00  108
 43  \w   -119.00 -30.00   0.50    0.20    --  -46.49 -57.00 150.00  178
 44  \w     34.00 123.00   0.50    0.20    --   49.62  57.00  30.00  178
 45  \w     26.00 123.00   0.50    0.20    --   49.62  77.00-150.00  194
 46  \w     26.00 123.00   0.50    0.20    --   49.62  77.00 -90.00  194
 47  \w     26.00 123.00   0.50    0.20    --   49.62  77.00 -60.00  194
 48  \w     26.00 122.00   0.50    0.20    --   49.62  77.00  30.00  192
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0240095000
_diffrn_orient_matrix_UB_12      -0.1031737000
_diffrn_orient_matrix_UB_13      -0.0256070000
_diffrn_orient_matrix_UB_21      -0.1277680000
_diffrn_orient_matrix_UB_22      0.0118601000
_diffrn_orient_matrix_UB_23      -0.0005768000
_diffrn_orient_matrix_UB_31      -0.0188713000
_diffrn_orient_matrix_UB_32      0.0507165000
_diffrn_orient_matrix_UB_33      -0.0518102000
_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  0.0692
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            65295
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.601
_diffrn_reflns_theta_max         66.601
_diffrn_reflns_theta_min         3.316
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.818
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25544
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_description       block
_exptl_crystal_F_000             1988
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.223
_refine_diff_density_min         -1.036
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         7564
_refine_ls_number_restraints     300
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0433
_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^)+(0.0589P)^2^+4.5884P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1152
_refine_ls_wR_factor_ref         0.1181
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6690
_reflns_number_total             7564
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04229h2.cif
_cod_data_source_block           9962-2-cu_auto
_cod_depositor_comments
'Adding full bibliography for 1572573--1572580.cif.'
_cod_database_code               1572579
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         CHONMnBr
_shelx_estimated_absorpt_t_max   0.509
_shelx_estimated_absorpt_t_min   0.509
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
2.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C3(H3A,H3B), C1(H1A,H1B), C37(H37A,H37B), C18(H18A,H18B), C2(H2A,
 H2B), C4(H4A,H4B)
2.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C13(H13), C14(H14),
 C15(H15), C16(H16), C17(H17), C36(H36), C35(H35), C34(H34), C33(H33), C32(H32),
  C43(H43), C42(H42), C41(H41), C40(H40), C39(H39), C20(H20), C21(H21),
 C22(H22), C23(H23), C24(H24), C11(H11), C10(H10), C9(H9), C8(H8), C7(H7)
2.c Fitted hexagon refined as free rotating group:
 C25(C26,C27,C28,C29,C30), C12(C13,C14,C15,C16,C17), C31(C36,C35,C34,C33,C32),
 C38(C43,C42,C41,C40,C39), C19(C20,C21,C22,C23,C24), C6(C11,C10,C9,C8,C7)
;
_shelx_res_checksum              6285
_shelx_hkl_checksum              46186
_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 4.622
_oxdiff_exptl_absorpt_empirical_full_min 0.550