A Cationic Sulfur-Hydrocarbon Triradical with an Excited Quartet State
Tang, Shuxuan; Ruan, Huapeng; Hu, Zhao-Bo; Zhao, Yue; Song, You; Wang, Xinping; Chemical Communications  (2022) –; doi:10.1039/D1CC06904G

data_7129568
_publ_section_title
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 A Cationic Sulfur-Hydrocarbon Triradical with an Excited Quartet State
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06904G
_journal_year                    2022
_chemical_formula_moiety         'C38 H20 S6, 3(Al C16 F36 O4), C2 H4 Cl2'
_chemical_formula_sum            'C88 H24 Al3 Cl2 F108 O12 S6'
_chemical_formula_weight         3669.27
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
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2021-07-22 deposited with the CCDC.	2022-01-13 downloaded from the CCDC.
;
_cell_angle_alpha                88.353(5)
_cell_angle_beta                 88.861(5)
_cell_angle_gamma                81.464(5)
_cell_formula_units_Z            2
_cell_length_a                   12.318(2)
_cell_length_b                   17.946(3)
_cell_length_c                   27.986(5)
_cell_measurement_reflns_used    9860
_cell_measurement_temperature    193
_cell_measurement_theta_max      27.441
_cell_measurement_theta_min      2.184
_cell_volume                     6114.7(18)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      193
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_unetI/netI     0.0784
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            49934
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.574
_diffrn_reflns_theta_min         2.200
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.400
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6300
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1297 before and 0.0604 after correction.
The Ratio of minimum to maximum transmission is 0.8450.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.993
_exptl_crystal_description       block
_exptl_crystal_F_000             3578
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.647
_refine_diff_density_min         -1.633
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2331
_refine_ls_number_reflns         27753
_refine_ls_number_restraints     406
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1171
_refine_ls_R_factor_gt           0.0839
_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^)+(0.1340P)^2^+15.6552P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2325
_refine_ls_wR_factor_ref         0.2620
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18738
_reflns_number_total             27753
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06904g2.cif
_cod_data_source_block           a_a
_cod_original_cell_volume        6114.6(18)
_cod_database_code               7129568
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C40A-C39 \\sim C40-C39
 with sigma of 0.02
 C42-C39 \\sim C42A-C39
 with sigma of 0.02
 C41-C39 \\sim C39-C41A
 with sigma of 0.02
 F71A-C41A \\sim F72A-C41A \\sim F70A-C41A
 with sigma of 0.02
 F39-C46 \\sim F39A-C46
 with sigma of 0.02
 F37-C46 \\sim F37A-C46
 with sigma of 0.02
 F44A-C44A \\sim F45A-C44A \\sim F43A-C44A
 with sigma of 0.02
 F37A-C46 \\sim F38-C46 \\sim F39A-C46
 with sigma of 0.02
 F42A-C45A \\sim F41A-C45A \\sim F40A-C45A
 with sigma of 0.02
 O12-C39 \\sim O12A-C39
 with sigma of 0.02
 Al3-O12 \\sim Al3-O12A
 with sigma of 0.02
 C65A-C63 \\sim C65-C63 \\sim C66A-C63 \\sim C66-C63 \\sim C64-C63 \\sim
C64A-C63
 with sigma of 0.02
 F84-C64A \\sim F83A-C64A \\sim F82A-C64A
 with sigma of 0.02
 F60-C52 \\sim F59-C52 \\sim F58-C52
 with sigma of 0.02
 F115-C90 \\sim F118-C90 \\sim F117-C90
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C42 \\sim C42A: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
C41 \\sim C41A: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
C45A \\sim C45: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
C44A \\sim C44: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
F44A \\sim F44 \\sim F43A \\sim F43 \\sim F45 \\sim F45A \\sim F42 \\sim F42A
\\sim F41 \\sim F52 \\sim F40 \\sim F40A: within 2A with sigma of 0.002 and
sigma for terminal atoms of 0.004 within 2A
F39 \\sim F39A: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
F37 \\sim F37A: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
C66A \\sim C66: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
C90 \\sim C52: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
Uanis(C45A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F62) \\sim Ueq, Uanis(F63) \\sim Ueq, Uanis(F61) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 F90, F84, F89, C63, F88, C65, C66, C64, F82, F87, F86, F85, F83
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F83A, F85A, C63, C66A, C64A, F88A, F87A, C65A, F84A, F82A, F90A, F89A, F86A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F80, C68, F81, F79
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(F70A)=Sof(C41A)=Sof(F72A)=Sof(F71A)=1-FVAR(1)
 Sof(F72)=Sof(F70)=Sof(F71)=Sof(C41)=FVAR(1)
 Sof(F66A)=Sof(C40A)=Sof(F64A)=Sof(F65A)=1-FVAR(2)
 Sof(F64)=Sof(F66)=Sof(F65)=Sof(C40)=FVAR(2)
 Sof(C42A)=Sof(F67A)=Sof(F68A)=Sof(F69A)=1-FVAR(3)
 Sof(F67)=Sof(F69)=Sof(F68)=Sof(C42)=FVAR(3)
 Sof(F39A)=Sof(F37A)=1-FVAR(4)
 Sof(F37)=Sof(F39)=FVAR(4)
 Sof(F42A)=Sof(F40A)=Sof(F41A)=Sof(C45A)=Sof(F44A)=Sof(F43A)=Sof(F45A)=
 Sof(C44A)=1-FVAR(5)
 Sof(F45)=Sof(F44)=Sof(F43)=Sof(C44)=Sof(F42)=Sof(F40)=Sof(F41)=Sof(C45)=FVAR(5)
 Sof(O12)=1-FVAR(6)
 Sof(O12A)=FVAR(6)
 Sof(F83A)=Sof(F86A)=Sof(F85A)=Sof(C66A)=Sof(C64A)=Sof(F88A)=Sof(F87A)=
 Sof(C65A)=Sof(F84A)=Sof(F82A)=Sof(F90A)=Sof(F89A)=1-FVAR(7)
 Sof(F90)=Sof(F84)=Sof(F89)=Sof(F88)=Sof(C65)=Sof(C66)=Sof(C64)=Sof(F82)=
 Sof(F87)=Sof(F86)=Sof(F85)=Sof(F83)=FVAR(7)
 Sof(F117)=Sof(F115)=Sof(F118)=Sof(C90)=1-FVAR(8)
 Sof(F59)=Sof(F58)=Sof(F60)=Sof(C52)=FVAR(8)
6.a Ternary CH refined with riding coordinates:
 C14(H14), C13(H13)
6.b Secondary CH2 refined with riding coordinates:
 C87(H87A,H87B), C88(H88A,H88B)
6.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C32(H32), C20(H20), C29(H29), C17(H17), C9(H9), C35(H35), C38(H38),
 C4(H4), C36(H36), C1(H1), C25(H25), C37(H37), C2(H2), C3(H3), C24(H24),
 C22(H22), C23(H23)
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_shelx_res_checksum              27360
_olex2_submission_special_instructions 'No special instructions were received'