#------------------------------------------------------------------------------
#$Date: 2022-01-15 00:48:57 +0200 (Sat, 15 Jan 2022) $
#$Revision: 272040 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/95/7129567.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7129567
loop_
_publ_author_name
'Tang, Shuxuan'
'Ruan, Huapeng'
'Hu, Zhao-Bo'
'Zhao, Yue'
'Song, You'
'Wang, Xinping'
_publ_section_title
;
 A Cationic Sulfur-Hydrocarbon Triradical with an Excited Quartet State
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06904G
_journal_year                    2022
_chemical_formula_moiety         'C38 H20 S6'
_chemical_formula_sum            'C38 H20 S6'
_chemical_formula_weight         668.90
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-22 deposited with the CCDC.	2022-01-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   12.143(3)
_cell_length_b                   12.143(3)
_cell_length_c                   11.827(4)
_cell_measurement_reflns_used    2452
_cell_measurement_temperature    193
_cell_measurement_theta_max      27.251
_cell_measurement_theta_min      2.592
_cell_volume                     1510.3(7)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0761
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8648
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.320
_diffrn_reflns_theta_min         2.592
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.482
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4918
_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 0.0838 after correction.
The Ratio of minimum to maximum transmission is 0.6596.
The λ/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_description       block
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     67
_refine_ls_number_reflns         975
_refine_ls_number_restraints     83
_refine_ls_restrained_S_all      1.266
_refine_ls_R_factor_all          0.1841
_refine_ls_R_factor_gt           0.1345
_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/[σ²(Fo²)+(0.0500P)²+15.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2684
_refine_ls_wR_factor_ref         0.2978
_reflns_Friedel_coverage         0.000
_reflns_number_gt                558
_reflns_number_total             975
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1cc06904g2.cif
_cod_data_source_block           a
_cod_original_cell_volume        1510.2(9)
_cod_database_code               7129567
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.944
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C2) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(S1)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4.a Ternary CH refined with riding coordinates:
 C1(H1)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7)
;
_shelx_res_file
;
TITL a_a.res in P6(3)/m
    a.res
    created by SHELXL-2018/3 at 12:31:04 on 01-Apr-2021
REM Old TITL A in P6(3)/m
REM SHELXT solution in P6(3)/m
REM R1 0.517, Rweak 0.037, Alpha 0.113, Orientation as input
REM Formula found by SHELXT: C27 N8 S6
CELL 0.71073 12.1427 12.1427 11.8269 90 90 120
ZERR 2 0.0028 0.0028 0.0043 0 0 0
LATT 1
SYMM -Y,+X-Y,+Z
SYMM +Y-X,-X,+Z
SYMM -X,-Y,0.5+Z
SYMM +Y,-X+Y,0.5+Z
SYMM -Y+X,+X,0.5+Z
SFAC C H S
UNIT 76 40 12
RIGU 0.001 0.001
ISOR 0.01 0.02 C2 C4 C1 C3 C5 C6 C7 S1

L.S. 20
PLAN  5
SIZE 0.1 0.12 0.1
TEMP 23
CONF
BOND $H
list 4
MORE -1
fmap 2
acta
SHEL 999 0.83
REM <olex2.extras>
REM <HklSrc "%.\\A.hkl">
REM </olex2.extras>

WGHT    0.050000   15.000000
FVAR       0.65308
S1    3    0.546986   -0.152706    0.614642    11.00000    0.07676    0.03522 =
         0.21147   -0.01736   -0.03009    0.03007
C2    1    0.630473    0.204336    0.693494    11.00000    0.02814    0.03825 =
         0.12715    0.00214   -0.00009    0.01835
C4    1    0.577710   -0.013079    0.693129    11.00000    0.03292    0.03708 =
         0.14238   -0.00199   -0.00826    0.01817
C1    1    0.666667    0.333333    0.639245    10.33333    0.04137    0.04137 =
         0.10359    0.00000    0.00000    0.02069
AFIX  13
H1    2    0.666666    0.333332    0.556383    10.33333   -1.20000
AFIX   0
C3    1    0.604908    0.095970    0.630261    11.00000    0.04146    0.04305 =
         0.13323   -0.00254   -0.00542    0.02577
AFIX  43
H3    2    0.605930    0.096408    0.551632    11.00000   -1.20000
AFIX   0
C5    1    0.644644   -0.194800    0.692837    11.00000    0.08324    0.04660 =
         0.15026   -0.00686   -0.00613    0.04275
C6    1    0.723337   -0.227438    0.629758    11.00000    0.12485    0.09143 =
         0.15843   -0.00599    0.00214    0.08287
AFIX  43
H6    2    0.726801   -0.223864    0.551207    11.00000   -1.20000
AFIX   0
C7    1    0.796009   -0.265689    0.694153    11.00000    0.14446    0.10998 =
         0.17331   -0.00687    0.00052    0.10616
AFIX  43
H7    2    0.846064   -0.292039    0.656468    11.00000   -1.20000
AFIX   0
HKLF 4




REM  a_a.res in P6(3)/m
REM wR2 = 0.2978, GooF = S = 1.044, Restrained GooF = 1.266 for all data
REM R1 = 0.1345 for 558 Fo > 4sig(Fo) and 0.1841 for all 975 data
REM 67 parameters refined using 83 restraints

END

WGHT      0.1007     11.4794

REM Highest difference peak  0.714,  deepest hole -0.500,  1-sigma level  0.119
Q1    1   0.5166 -0.1749  0.6987  11.00000  0.05    0.71
Q2    1   0.5529 -0.1543  0.5360  11.00000  0.05    0.70
Q3    1   0.6667  0.3333  0.7108  10.33333  0.05    0.69
Q4    1   0.6253  0.2052  0.7500  10.50000  0.05    0.69
Q5    1   0.5758 -0.0268  0.7500  10.50000  0.05    0.60
;
_shelx_res_checksum              20282
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.5470(3) -0.1527(2) 0.6146(4) 0.1069(15) Uani 1 1 d . U . . .
C2 C 0.6305(6) 0.2043(7) 0.6935(8) 0.064(2) Uani 1 1 d . U . . .
C4 C 0.5777(7) -0.0131(7) 0.6931(8) 0.070(2) Uani 1 1 d . U . . .
C1 C 0.666667 0.333333 0.6392(16) 0.062(3) Uani 1 3 d S TU P . .
H1 H 0.666666 0.333332 0.556383 0.075 Uiso 1 3 calc R U P . .
C3 C 0.6049(7) 0.0960(7) 0.6303(10) 0.071(2) Uani 1 1 d . U . . .
H3 H 0.605930 0.096408 0.551632 0.085 Uiso 1 1 calc R U . . .
C5 C 0.6446(10) -0.1948(8) 0.6928(10) 0.089(3) Uani 1 1 d . U . . .
C6 C 0.7233(12) -0.2274(11) 0.6298(13) 0.112(4) Uani 1 1 d . U . . .
H6 H 0.726801 -0.223864 0.551207 0.135 Uiso 1 1 calc R U . . .
C7 C 0.7960(13) -0.2657(12) 0.6942(11) 0.124(5) Uani 1 1 d . U . . .
H7 H 0.846064 -0.292039 0.656468 0.148 Uiso 1 1 calc R U . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S1 0.0768(18) 0.0352(12) 0.211(4) -0.0174(17) -0.030(2) 0.0301(11)
C2 0.028(3) 0.038(2) 0.127(5) 0.002(3) 0.000(3) 0.018(2)
C4 0.033(3) 0.037(3) 0.142(6) -0.002(3) -0.008(4) 0.018(3)
C1 0.041(3) 0.041(3) 0.104(8) 0.000 0.000 0.0207(13)
C3 0.041(4) 0.043(3) 0.133(6) -0.003(3) -0.005(4) 0.026(3)
C5 0.083(5) 0.047(4) 0.150(7) -0.007(4) -0.006(5) 0.043(4)
C6 0.125(7) 0.091(6) 0.158(7) -0.006(5) 0.002(5) 0.083(6)
C7 0.144(8) 0.110(7) 0.173(9) -0.007(5) 0.001(6) 0.106(6)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C5 S1 C4 98.6(4) . . ?
C2 C2 C1 114.6(8) 10_557 . ?
C2 C2 C3 122.1(6) 10_557 . ?
C3 C2 C1 123.2(10) . . ?
C4 C4 S1 121.0(3) 10_557 . ?
C4 C4 C3 121.9(6) 10_557 . ?
C3 C4 S1 117.0(8) . . ?
C2 C1 C2 103.9(9) . 3_665 ?
C2 C1 C2 103.9(9) 2_655 3_665 ?
C2 C1 C2 103.9(9) . 2_655 ?
C2 C1 H1 114.6 . . ?
C2 C1 H1 114.6 2_655 . ?
C2 C1 H1 114.6 3_665 . ?
C2 C3 H3 122.0 . . ?
C4 C3 C2 116.0(10) . . ?
C4 C3 H3 122.0 . . ?
C5 C5 S1 121.5(4) 10_557 . ?
C5 C5 C6 121.8(8) 10_557 . ?
C6 C5 S1 116.7(10) . . ?
C5 C6 H6 122.3 . . ?
C7 C6 C5 115.4(13) . . ?
C7 C6 H6 122.3 . . ?
C6 C7 H7 118.6 . . ?
C7 C7 C6 122.7(8) 10_557 . ?
C7 C7 H7 118.6 10_557 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C4 1.801(8) . ?
S1 C5 1.769(10) . ?
C2 C2 1.34(2) 10_557 ?
C2 C1 1.539(11) . ?
C2 C3 1.407(11) . ?
C4 C4 1.35(2) 10_557 ?
C4 C3 1.406(12) . ?
C1 H1 0.9800 . ?
C3 H3 0.9300 . ?
C5 C5 1.35(2) 10_557 ?
C5 C6 1.416(15) . ?
C6 H6 0.9300 . ?
C6 C7 1.409(16) . ?
C7 C7 1.32(3) 10_557 ?
C7 H7 0.9300 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S1 C4 C3 C2 -179.1(5) . . . . ?
S1 C5 C6 C7 -177.4(9) . . . . ?
C2 C2 C1 C2 54.2(8) 10_557 . . 2_655 ?
C2 C2 C1 C2 -54.2(8) 10_557 . . 3_665 ?
C2 C2 C3 C4 0.8(8) 10_557 . . . ?
C4 S1 C5 C5 45.2(4) . . . 10_557 ?
C4 S1 C5 C6 -134.3(8) . . . . ?
C4 C4 C3 C2 -0.8(8) 10_557 . . . ?
C1 C2 C3 C4 177.8(5) . . . . ?
C3 C2 C1 C2 -123.0(11) . . . 2_655 ?
C3 C2 C1 C2 128.6(10) . . . 3_665 ?
C5 S1 C4 C4 -44.9(4) . . . 10_557 ?
C5 S1 C4 C3 133.4(6) . . . . ?
C5 C5 C6 C7 3.0(14) 10_557 . . . ?
C5 C6 C7 C7 -3.1(14) . . . 10_557 ?
