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_1572577
_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, C44 H42 F4 P2, C H4 O'
_chemical_formula_sum            'C45 H46 Br4 F4 Mn O P2'
_chemical_formula_weight         1115.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-27
_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                 93.2590(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5253(2)
_cell_length_b                   19.8357(3)
_cell_length_c                   20.0972(3)
_cell_measurement_reflns_used    26519
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.7530
_cell_measurement_theta_min      2.0860
_cell_volume                     4587.04(13)
_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 2014/4 (Sheldrick, 2014)'
_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 0.878
_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     31.00  79.00   0.50    0.50    --    6.38  57.00 120.00   96
  2  \w     31.00  79.00   0.50    0.50    --    6.38  57.00 120.00   96
  3  \w    -63.00   8.00   0.50    0.50    --    6.38 -57.00 120.00  142
  4  \w    -18.00  28.00   0.50    0.50    --   -5.60 -99.00   0.00   92
  5  \w    -65.00  23.00   0.50    0.50    --    6.38 -57.00-150.00  176
  6  \w    -56.00  13.00   0.50    0.50    --   -5.51 -13.00-136.00  138
  7  \w    -18.00  27.00   0.50    0.50    --   -5.51 -99.00-150.00   90
  8  \w     -4.00  22.00   0.50    0.50    --    6.29 -30.00  75.39   52
  9  \w    -50.00  22.00   0.50    0.50    --    6.29 -31.00-110.65  144
 10  \w    -69.00  22.00   0.50    0.50    --    6.29 -34.00  32.11  182
 11  \w    -64.00  -9.00   0.50    0.50    --    6.29 -34.00 177.31  110
 12  \w     -7.00  22.00   0.50    0.50    --    6.29 -34.00 177.31   58
 13  \w    -47.00 -41.00   0.50    0.50    --    6.29 -34.00 -52.17   12
;
_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      -0.0516565000
_diffrn_orient_matrix_UB_12      -0.0186491000
_diffrn_orient_matrix_UB_13      0.0039711000
_diffrn_orient_matrix_UB_21      -0.0332688000
_diffrn_orient_matrix_UB_22      0.0298702000
_diffrn_orient_matrix_UB_23      -0.0047581000
_diffrn_orient_matrix_UB_31      -0.0049195000
_diffrn_orient_matrix_UB_32      -0.0062153000
_diffrn_orient_matrix_UB_33      -0.0348061000
_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  0.0374
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.878
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            54734
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.804
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.851
_diffrn_reflns_theta_min         2.046
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.891
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70725
_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    1.615
_exptl_crystal_description       block
_exptl_crystal_F_000             2220
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.671
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Flack x determined using 4535 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.001(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         11628
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0276
_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^)+(0.0273P)^2^+2.4628P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0545
_refine_ls_wR_factor_ref         0.0556
_reflns_Friedel_coverage         0.830
_reflns_Friedel_fraction_full    0.980
_reflns_Friedel_fraction_max     0.730
_reflns_number_gt                10738
_reflns_number_total             11628
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04229h2.cif
_cod_data_source_block           4-4
_cod_depositor_comments
'Adding full bibliography for 1572573--1572580.cif.'
_cod_database_code               1572577
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         CHONMnPBr
_shelx_estimated_absorpt_t_max   0.697
_shelx_estimated_absorpt_t_min   0.697
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B), C6(H6A,H6B), C2(H2A,H2B), C5(H5A,H5B), C19(H19A,H19B), C1(H1A,
 H1B), C4(H4A,H4B), C3(H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
 C28(H28), C8(H8), C29(H29), C10(H10), C31(H31), C11(H11), C27(H27), C30(H30),
 C22(H22), C9(H9), C37(H37), C14(H14), C33(H33), C15(H15), C12(H12), C36(H36),
 C42(H42), C43(H43), C18(H18), C35(H35), C41(H41), C24(H24), C17(H17), C23(H23),
  C34(H34), C16(H16)
2.c Idealised Me refined as rotating group:
 C45(H45A,H45B,H45C)
2.d Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              58047
_shelx_hkl_checksum              52954
_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 1.619
_oxdiff_exptl_absorpt_empirical_full_min 0.804