Ratiometric radio-photoluminescence dosimeter based on a radical excimer for X-Ray detection
Lu, Huangjie; Ma, Jingqi; Yang, Junpu; Hou, Huiliang; Lu, Jiacheng; Wang, Jian-Qiang; Wang, Yaxing; Lin, Jian; Chemical Communications  (2023) –; doi:10.1039/D3CC03824F

data_7132157
_publ_section_title
;
 Ratiometric radio-photoluminescence dosimeter based on a radical excimer
 for X-Ray detection
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC03824F
_journal_year                    2023
_chemical_formula_moiety
'C170 H121 N29 O38 Th6, 12.5(H2 O), 1.25(O), 0.5(C3 H6 N O)'
_chemical_formula_sum            'C171.5 H149 N29.5 O52.25 Th6'
_chemical_formula_weight         4851.43
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-19
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2023-08-01 deposited with the CCDC.	2023-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                80.4910(9)
_cell_angle_beta                 89.9651(9)
_cell_angle_gamma                76.2585(9)
_cell_formula_units_Z            2
_cell_length_a                   20.2226(2)
_cell_length_b                   20.2409(2)
_cell_length_c                   23.3410(3)
_cell_measurement_reflns_used    52244
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      28.8650
_cell_measurement_theta_min      1.6480
_cell_volume                     9145.60(18)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      273.15
_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  \f   -350.61   9.39   0.50    4.00  12.27 -11.30 -28.85    --   720
  2  \w    -64.97  -6.47   0.50    4.00    --  -11.35 102.22 -99.09  117
  3  \w   -106.96  17.54   0.50    4.00    --  -11.30 -59.25 -51.92  249
  4  \w    -52.58  27.42   0.50    4.00    --  -11.35  79.34  91.89  160
  5  \f     -9.39 350.61   0.50    4.00  79.56 -11.30  28.85    --   720
  6  \f   -339.92  20.08   0.50    4.00  17.79 -11.30 -59.25    --   720
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            334528
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.761
_exptl_absorpt_coefficient_mu    4.950
_exptl_absorpt_correction_T_max  0.26749
_exptl_absorpt_correction_T_min  0.24249
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_description       block
_exptl_crystal_F_000             4685
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         2.088
_refine_diff_density_min         -1.451
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2483
_refine_ls_number_reflns         32183
_refine_ls_number_restraints     396
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0180P)^2^+72.4685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0921
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26239
_reflns_number_total             32183
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03824f2.cif
_cod_data_source_block           Th105
_cod_original_cell_volume        9145.58(17)
_cod_original_formula_sum        'C171.50 H149 N29.50 O52.25 Th6'
_cod_database_code               7132157
_shelx_shelxl_version_number     2018/3
_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,H) groups
2. Restrained distances
 Th6-H22A \\sim Th6-H22B
 with sigma of 0.02
3. Rigid bond restraints
 N29, C135, C162, C163, C164, C165
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O50, N30, C172, C173, C174
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(C132) \\sim Ueq, Uanis(C139) \\sim Ueq, Uanis(C155) \\sim Ueq,
Uanis(C171) \\sim Ueq, Uanis(C1A) \\sim Ueq, Uanis(C1B) \\sim Ueq, Uanis(C98)
\\sim Ueq, Uanis(C168) \\sim Ueq, Uanis(C169) \\sim Ueq, Uanis(C170) \\sim Ueq,
Uanis(C98A) \\sim Ueq, Uanis(C1F) \\sim Ueq, Uanis(C1C) \\sim Ueq, Uanis(C1D)
\\sim Ueq, Uanis(C166) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(C167) \\sim Ueq,
Uanis(C1G) \\sim Ueq, Uanis(C1E) \\sim Ueq, Uanis(N7A) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C165) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C172) \\sim Ueq, Uanis(C173) \\sim Ueq, Uanis(N30) \\sim Ueq, Uanis(C174)
\\sim Ueq, Uanis(O50) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O49) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O52) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O51) \\sim Ueq, Uanis(O46) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O53) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 N7, N7A, C1A, C1B, C1C, C1D, C1E, C1F, C1G, C2, C49, C49A, C52, C98, C98A,
 C132, C139, C155, C166, C167, C168, C169, C170, C171
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C1A)=Sof(H1A)=Sof(C1B)=Sof(C1G)=Sof(H1G)=Sof(N7A)=Sof(C1E)=Sof(H1E)=
 Sof(C1F)=Sof(H1F)=Sof(C1C)=Sof(C1D)=Sof(H1D)=Sof(C49A)=Sof(H49A)=Sof(C98A)=
 Sof(H98A)=Sof(C171)=Sof(H171)=1-FVAR(1)
 Sof(C49)=Sof(H49)=Sof(C98)=Sof(H98)=Sof(C132)=Sof(H132)=Sof(C139)=Sof(H139)=
 Sof(C155)=Sof(C166)=Sof(H166)=Sof(N7)=Sof(C167)=Sof(H167)=Sof(C168)=Sof(H168)=
 Sof(C169)=Sof(C170)=Sof(H170)=FVAR(1)
 Fixed Sof: O45(0.5) H45A(0.5) H45B(0.5) O46(0.5) H46A(0.5) H46B(0.5) O47(0.5)
 O48(0.5) H48A(0.5) H48B(0.5) O49(0.5) H49B(0.5) H49C(0.5) O50(0.5) N30(0.5)
 C172(0.5) H172(0.5) C173(0.5) H17A(0.5) H17B(0.5) C174(0.5) H17C(0.5)
 H17D(0.5) H17E(0.5) O51(0.5) H51A(0.5) H51B(0.5) O52(0.25) O53(0.5)
7.a Riding coordinates:
 O32(H32A,H32B), O1W(H1WA,H1WB), O2W(H2WA,H2WB), O4W(H4WA,H4WB), O7(H7A,H7B),
 O39(H39A,H39B), O41(H41A,H41B), O42(H42A,H42B), O43(H43A,H43B), O44(H44A,H44B),
  O45(H45A,H45B), O46(H46A,H46B), O48(H48A,H48B), O49(H49B,H49C), O51(H51A,H51B)
7.b Free rotating group:
 O22(H22A,H22B), O3W(H3WA,H3WB)
7.c Rotating group:
 O27(H27A,H27B), O28(H28A,H28B), O37(H37A,H37B), O38(H38A,H38B)
7.d Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C1G(H1G), C1E(H1E), C1F(H1F), C1D(H1D), C3(H3), C12(H12), C14(H14),
 C16(H16), C19(H19), C22(H22), C23(H23), C30(H30), C31(H31), C32(H32), C33(H33),
  C34(H34), C35(H35), C37(H37), C39(H39), C43(H43), C44(H44), C46(H46),
 C48(H48), C49(H49), C49A(H49A), C56(H56), C58(H58), C62(H62), C63(H63),
 C71(H71), C72(H72), C73(H73), C79(H79), C84(H84), C86(H86), C87(H87), C88(H88),
  C89(H89), C90(H90), C91(H91), C92(H92), C93(H93), C94(H94), C95(H95),
 C97(H97), C98(H98), C98A(H98A), C99(H99), C100(H100), C101(H101), C102(H102),
 C104(H104), C106(H106), C107(H107), C108(H108), C109(H109), C110(H110),
 C112(H112), C113(H113), C114(H114), C116(H116), C117(H117), C118(H118),
 C119(H119), C120(H120), C121(H121), C122(H122), C123(H123), C124(H124),
 C125(H125), C126(H126), C127(H127), C128(H128), C129(H129), C130(H130),
 C131(H131), C132(H132), C133(H133), C134(H134), C136(H136), C137(H137),
 C138(H138), C139(H139), C140(H140), C141(H141), C142(H142), C143(H143),
 C144(H144), C145(H145), C146(H146), C147(H147), C148(H148), C149(H149),
 C150(H150), C151(H151), C152(H152), C153(H153), C154(H154), C156(H156),
 C157(H157), C158(H158), C159(H159), C160(H160), C161(H161), C162(H162),
 C163(H163), C164(H164), C165(H165), C166(H166), C167(H167), C168(H168),
 C170(H170), C171(H171), C172(H172)
7.e Fitted hexagon refined as free rotating group:
 C1G(N7A,C1E,C1F,C1C,C1D), C166(N7,C167,C168,C169,C170)
7.f X=CH2 refined with riding coordinates:
 C173(H17A,H17B)
7.g Idealised Me refined as rotating group:
 C96(H96A,H96B,H96C), C174(H17C,H17D,H17E)
;
_shelx_res_checksum              44888
_platon_squeeze_void_probe_radius 1.20
_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
- Detector area scaling
;