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_1572575
_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 H46 P2'
_chemical_formula_sum            'C44 H46 Br4 Mn P2'
_chemical_formula_weight         1011.33
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.4957(10)
_cell_length_b                   33.2381(11)
_cell_length_c                   16.6711(5)
_cell_measurement_reflns_used    11783
_cell_measurement_temperature    101(1)
_cell_measurement_theta_max      25.5790
_cell_measurement_theta_min      2.4200
_cell_volume                     8586.4(7)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      101(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -14.00  13.00   0.50    3.00    --    6.23  88.00 -65.00   54
  2  \w    -18.00  27.00   0.50    3.00    --   -5.44 -99.00   0.00   90
  3  \w    -15.00  39.00   0.50    3.00    --    6.23 -99.00   0.00  108
  4  \w    -16.00  28.00   0.50    3.00    --   -5.44 -99.00  30.00   88
  5  \w    -15.00  30.00   0.50    3.00    --    6.23 -88.00 178.00   90
;
_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      -0.0182705000
_diffrn_orient_matrix_UB_12      -0.0344606000
_diffrn_orient_matrix_UB_13      0.0106565000
_diffrn_orient_matrix_UB_21      0.0276323000
_diffrn_orient_matrix_UB_22      0.0058074000
_diffrn_orient_matrix_UB_23      0.0159937000
_diffrn_orient_matrix_UB_31      -0.0267131000
_diffrn_orient_matrix_UB_32      0.0295501000
_diffrn_orient_matrix_UB_33      0.0092749000
_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  0.0639
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            50137
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.173
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.134
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26728
_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    1.565
_exptl_crystal_description       block
_exptl_crystal_F_000             4040
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.672
_refine_diff_density_min         -0.871
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         7565
_refine_ls_number_restraints     327
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.1148
_refine_ls_R_factor_gt           0.0810
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1098P)^2^+55.2052P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2132
_refine_ls_wR_factor_ref         0.2368
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5330
_reflns_number_total             7565
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04229h2.cif
_cod_data_source_block           b
_cod_depositor_comments
'Adding full bibliography for 1572573--1572580.cif.'
_cod_database_code               1572575
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         chonMnBr
_shelx_estimated_absorpt_t_max   0.733
_shelx_estimated_absorpt_t_min   0.576
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Mn1-Br4 \\sim Mn1-Br4A
 with sigma of 0.02
 Mn1-Br1 \\sim Mn1-Br1A
 with sigma of 0.02
 Br2-Mn1 \\sim Br2A-Mn1
 with sigma of 0.02
3. 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
4. Others
 Sof(Br4A)=1-FVAR(1)
 Sof(Br4)=FVAR(1)
 Sof(Br1A)=1-FVAR(2)
 Sof(Br1)=FVAR(2)
 Sof(Br2A)=1-FVAR(3)
 Sof(Br2)=FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C18(H18A,H18B), C1(H1A,H1B), C3(H3A,H3B), C2(H2A,H2B), C4(H4A,
 H4B), C5(H5A,H5B), C44(H44A,H44B)
5.b Aromatic/amide H refined with riding coordinates:
 C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C39(H39), C40(H40),
 C41(H41), C42(H42), C43(H43), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17),
  C11(H11), C10(H10), C9(H9), C8(H8), C7(H7), C26(H26), C27(H27), C28(H28),
 C29(H29), C30(H30), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24)
5.c Fitted hexagon refined as free rotating group:
 C31(C32,C33,C34,C35,C36), C38(C39,C40,C41,C42,C43), C12(C13,C14,C15,C16,C17),
 C6(C11,C10,C9,C8,C7), C25(C26,C27,C28,C29,C30), C19(C20,C21,C22,C23,C24)
;
_shelx_res_checksum              15460
_shelx_hkl_checksum              80873
_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 1.945
_oxdiff_exptl_absorpt_empirical_full_min 0.639