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_1572574
_publ_section_title
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 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, C H4 O'
_chemical_formula_sum            'C45 H50 Br4 Mn O P2'
_chemical_formula_weight         1043.37
_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                 94.1160(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7943(3)
_cell_length_b                   19.8244(6)
_cell_length_c                   19.3722(7)
_cell_measurement_reflns_used    9994
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      57.162
_cell_measurement_theta_min      3.801
_cell_volume                     4517.8(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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      150.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_unetI/netI     0.0596
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22413
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.435
_diffrn_reflns_theta_min         2.013
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.933
_exptl_absorpt_correction_T_max  0.7512
_exptl_absorpt_correction_T_min  0.5348
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1468 before and 0.0572 after correction.
The Ratio of minimum to maximum transmission is 0.7119.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_description       block
_exptl_crystal_F_000             2092
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.510(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         8596
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0412
_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^)+(0.0303P)^2^+17.4526P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0993
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                7459
_reflns_number_total             8596
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04229h2.cif
_cod_data_source_block           11
_cod_depositor_comments
'Adding full bibliography for 1572573--1572580.cif.'
_cod_database_code               1572574
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.694
_shelx_estimated_absorpt_t_min   0.694
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.490(12)
 0.510(12)
2. 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
3.a Secondary CH2 refined with riding coordinates:
 C00B(H00A,H00B), C00G(H00F,H00G), C00N(H00K,H00L), C00S(H00N,H00R), C00U(H00S,
 H00T), C00W(H00U,H00W), C00Z(H00Z,H), C01D(H01D,H01E)
3.b Aromatic/amide H refined with riding coordinates:
 C008(H008), C009(H009), C00C(H00C), C00D(H00D), C00E(H00E), C00H(H00H),
 C00I(H00I), C00J(H00J), C00M(H00M), C00O(H00O), C00P(H00P), C00Q(H00Q),
 C00V(H00V), C00X(H00X), C00Y(H00Y), C010(H010), C011(H011), C012(H012),
 C013(H013), C014(H014), C015(H015), C016(H016), C017(H017), C018(H018),
 C019(H019), C01A(H01A), C01B(H01B), C01C(H01C), C01E(H01F), C01G(H01G)
3.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C)
3.d Idealised tetrahedral OH refined as rotating group:
 O01F(H01H)
;
_shelx_res_checksum              66468
_shelx_hkl_checksum              49566
_olex2_submission_special_instructions 'No special instructions were received'