# Supplementary Information (SI) for Physical Chemistry Chemical Physics.
# This journal is © the Owner Societies 2025

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_tref
_database_code_depnum_ccdc_archive 'CCDC 2378911'
loop_
_audit_author_name
_audit_author_address
'huimin liu'
;ningbo university
China
;
_audit_update_record             
;
2024-08-21 deposited with the CCDC.	2025-06-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/2
_shelx_SHELXL_version_number     2019/2
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H2 Cl2 O2 S3'
_chemical_formula_sum            'C8 H2 Cl2 O2 S3'
_chemical_formula_weight         297.18

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'
O O 0.0106 0.0060 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   16.031(3)
_cell_length_b                   6.9802(14)
_cell_length_c                   9.3455(19)
_cell_angle_alpha                90
_cell_angle_beta                 101.26(3)
_cell_angle_gamma                90
_cell_volume                     1025.6(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4193
_cell_measurement_theta_min      3.5
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.925
_exptl_crystal_F_000             592
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.22
_exptl_absorpt_coefficient_mu    1.213
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.723
_exptl_absorpt_correction_T_max  0.812
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            3862
_diffrn_reflns_av_unetI/netI     0.1067
_diffrn_reflns_av_R_equivalents  0.0722
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.193
_diffrn_reflns_theta_max         25.013
_diffrn_reflns_theta_full        25.013
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             902
_reflns_number_gt                837
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_cell_refinement       RAPID-AUTO
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2004)'
_computing_structure_solution    'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0432P)²+0.2085P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_extinction_coef       0.055(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         902
_refine_ls_number_parameters     70
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0353
_refine_ls_wR_factor_ref         0.0874
_refine_ls_wR_factor_gt          0.0855
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.59438(3) 0.65073(7) 0.41405(6) 0.0326(3) Uani 1 1 d . . . . .
S2 S 0.500000 0.12256(9) 0.250000 0.0324(3) Uani 1 2 d S T P . .
Cl1 Cl 0.73330(4) 0.54439(9) 0.65848(6) 0.0470(3) Uani 1 1 d . . . . .
O1 O 0.44641(11) 0.0155(2) 0.32667(19) 0.0519(5) Uani 1 1 d . . . . .
C1 C 0.62805(13) 0.2930(3) 0.4813(2) 0.0309(5) Uani 1 1 d . . . . .
H1A H 0.652268 0.182504 0.527255 0.037 Uiso 1 1 calc R U . . .
C2 C 0.65291(13) 0.4761(3) 0.5202(2) 0.0314(5) Uani 1 1 d . . . . .
C3 C 0.53457(12) 0.4782(3) 0.3125(2) 0.0267(5) Uani 1 1 d . . . . .
C4 C 0.56042(13) 0.2980(3) 0.3615(2) 0.0285(5) Uani 1 1 d . . . . .

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 0.0336(4) 0.0245(4) 0.0393(4) -0.00346(19) 0.0063(3) -0.00369(19)
S2 0.0405(5) 0.0201(4) 0.0337(5) 0.000 0.0005(4) 0.000
Cl1 0.0409(4) 0.0543(5) 0.0418(4) -0.0064(2) -0.0022(3) -0.0109(3)
O1 0.0604(11) 0.0394(9) 0.0519(10) 0.0123(7) 0.0008(9) -0.0222(8)
C1 0.0314(11) 0.0300(10) 0.0319(12) 0.0034(8) 0.0075(9) 0.0006(8)
C2 0.0277(10) 0.0369(11) 0.0296(11) -0.0003(9) 0.0059(9) -0.0040(9)
C3 0.0271(10) 0.0229(10) 0.0314(11) -0.0009(7) 0.0086(9) -0.0013(8)
C4 0.0305(11) 0.0243(10) 0.0311(11) 0.0007(8) 0.0072(9) -0.0012(8)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 C3 1.707(2) . ?
S1 C2 1.728(2) . ?
S2 O1 1.4319(15) . ?
S2 O1 1.4320(15) 2_655 ?
S2 C4 1.769(2) . ?
S2 C4 1.769(2) 2_655 ?
Cl1 C2 1.705(2) . ?
C1 C2 1.367(3) . ?
C1 C4 1.399(3) . ?
C1 H1A 0.9300 . ?
C3 C4 1.375(3) . ?
C3 C3 1.445(4) 2_655 ?

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
C3 S1 C2 90.26(10) . . ?
O1 S2 O1 117.07(15) . 2_655 ?
O1 S2 C4 112.32(9) . . ?
O1 S2 C4 110.06(10) 2_655 . ?
O1 S2 C4 110.06(10) . 2_655 ?
O1 S2 C4 112.32(9) 2_655 2_655 ?
C4 S2 C4 92.37(13) . 2_655 ?
C2 C1 C4 109.26(18) . . ?
C2 C1 H1A 125.4 . . ?
C4 C1 H1A 125.4 . . ?
C1 C2 Cl1 126.95(17) . . ?
C1 C2 S1 114.17(17) . . ?
Cl1 C2 S1 118.89(11) . . ?
C4 C3 C3 113.76(12) . 2_655 ?
C4 C3 S1 111.12(16) . . ?
C3 C3 S1 135.10(7) 2_655 . ?
C3 C4 C1 115.18(17) . . ?
C3 C4 S2 110.04(16) . . ?
C1 C4 S2 134.74(14) . . ?

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
C4 C1 C2 Cl1 -179.37(14) . . . . ?
C4 C1 C2 S1 0.6(2) . . . . ?
C3 S1 C2 C1 -0.36(15) . . . . ?
C3 S1 C2 Cl1 179.60(13) . . . . ?
C2 S1 C3 C4 0.01(14) . . . . ?
C2 S1 C3 C3 -178.5(3) . . . 2_655 ?
C3 C3 C4 C1 179.21(18) 2_655 . . . ?
S1 C3 C4 C1 0.3(2) . . . . ?
C3 C3 C4 S2 1.1(2) 2_655 . . . ?
S1 C3 C4 S2 -177.81(8) . . . . ?
C2 C1 C4 C3 -0.6(3) . . . . ?
C2 C1 C4 S2 176.95(14) . . . . ?
O1 S2 C4 C3 -113.23(15) . . . . ?
O1 S2 C4 C3 114.43(15) 2_655 . . . ?
C4 S2 C4 C3 -0.39(9) 2_655 . . . ?
O1 S2 C4 C1 69.1(2) . . . . ?
O1 S2 C4 C1 -63.2(2) 2_655 . . . ?
C4 S2 C4 C1 -178.0(2) 2_655 . . . ?

_refine_diff_density_max         0.599
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.105

_shelx_res_file                  
;
TITL tref_a.res in C2/c
    tref.res
    created by SHELXL-2019/2 at 15:42:43 on 15-Dec-2023
REM Old TITL tref in C2/c
REM SHELXT solution in C2/c: R1 0.130, Rweak 0.004, Alpha 0.026
REM <I/s> 0.940 for 89 systematic absences, Orientation as input
REM Formula found by SHELXT: C8 N2 S2 Cl3
CELL 0.71073 16.031 6.9802 9.3455 90 101.261 90
ZERR 4 0.0032 0.0014 0.0019 0 0.03 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H O S Cl
UNIT 32 8 8 12 8

L.S. 20
PLAN  5
ACTA
CONF
HTAB
BOND $H
SHEL 999 0.84
OMIT   -16   0   8
OMIT     1   3  11
OMIT    -5   1   3
OMIT    -4   2   1
OMIT     4   0   4
list 4
fmap 2
MORE -1
REM <olex2.extras>
REM <HklSrc "%.\\tref.hkl">
REM </olex2.extras>
WGHT    0.043200    0.208500
EXTI    0.055064
FVAR       0.23107
S1    4    0.594381    0.650731    0.414054    11.00000    0.03361    0.02454 =
         0.03934   -0.00346    0.00628   -0.00369
S2    4    0.500000    0.122562    0.250000    10.50000    0.04049    0.02014 =
         0.03367    0.00000    0.00049    0.00000
CL1   5    0.733298    0.544394    0.658484    11.00000    0.04087    0.05429 =
         0.04177   -0.00640   -0.00217   -0.01094
O1    3    0.446412    0.015473    0.326665    11.00000    0.06038    0.03945 =
         0.05186    0.01230    0.00083   -0.02217
C1    1    0.628046    0.292994    0.481303    11.00000    0.03144    0.02996 =
         0.03191    0.00336    0.00749    0.00056
AFIX  43
H1A   2    0.652268    0.182504    0.527255    11.00000   -1.20000
AFIX   0
C2    1    0.652910    0.476093    0.520215    11.00000    0.02771    0.03687 =
         0.02964   -0.00033    0.00593   -0.00397
C3    1    0.534566    0.478199    0.312504    11.00000    0.02710    0.02289 =
         0.03141   -0.00087    0.00861   -0.00132
C4    1    0.560419    0.297995    0.361462    11.00000    0.03048    0.02432 =
         0.03112    0.00066    0.00720   -0.00124

HKLF 4




REM  tref_a.res in C2/c
REM wR2 = 0.0874, GooF = S = 1.086, Restrained GooF = 1.086 for all data
REM R1 = 0.0353 for 837 Fo > 4sig(Fo) and 0.0386 for all 902 data
REM 70 parameters refined using 0 restraints

END

WGHT      0.0463      0.1878

REM No hydrogen bonds found for HTAB generation

REM Highest difference peak  0.599,  deepest hole -0.440,  1-sigma level  0.105
Q1    1   0.6321  0.5620  0.4684  11.00000  0.05    0.60
Q2    1   0.5604  0.5616  0.3492  11.00000  0.05    0.54
Q3    1   0.5343  0.2101  0.3081  11.00000  0.05    0.48
Q4    1   0.5493  0.3686  0.3383  11.00000  0.05    0.41
Q5    1   0.5000  0.5401  0.2500  10.50000  0.05    0.39
;
_shelx_res_checksum              2283

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DCM'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_tref_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2378965'
loop_
_audit_author_name
_audit_author_address
'huimin liu'
;ningbo university
China
;
_audit_update_record             
;
2024-08-21 deposited with the CCDC.	2025-06-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/2
_shelx_SHELXL_version_number     2019/2
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H2 Br2 O2 S3'
_chemical_formula_sum            'C8 H2 Br2 O2 S3'
_chemical_formula_weight         386.10

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   16.412(3)
_cell_length_b                   6.9676(14)
_cell_length_c                   9.5683(19)
_cell_angle_alpha                90
_cell_angle_beta                 99.34(3)
_cell_angle_gamma                90
_cell_volume                     1079.6(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3203
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.375
_exptl_crystal_F_000             736
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    8.060
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.745
_exptl_absorpt_correction_T_max  0.832
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4131
_diffrn_reflns_av_unetI/netI     0.0709
_diffrn_reflns_av_R_equivalents  0.0898
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.183
_diffrn_reflns_theta_max         24.858
_diffrn_reflns_theta_full        24.858
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             933
_reflns_number_gt                687
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_cell_refinement       RAPID-AUTO
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2004)'
_computing_structure_solution    'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0523P)²+19.9813P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_extinction_coef       0.0095(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         933
_refine_ls_number_parameters     70
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0525
_refine_ls_wR_factor_ref         0.1686
_refine_ls_wR_factor_gt          0.1169
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_restrained_S_all      1.168
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Br1 Br 0.26978(6) 0.55212(18) 0.34636(12) 0.0510(6) Uani 1 1 d . . . . .
C1 C 0.3543(6) 0.4748(13) 0.4908(10) 0.032(2) Uani 1 1 d . . . . .
C2 C 0.3778(6) 0.2971(16) 0.5258(11) 0.041(2) Uani 1 1 d . . . . .
H2 H 0.355186 0.187873 0.478837 0.049 Uiso 1 1 calc R U . . .
C3 C 0.4417(6) 0.2956(13) 0.6440(10) 0.033(2) Uani 1 1 d . . . . .
C4 C 0.4676(6) 0.4792(14) 0.6883(9) 0.033(2) Uani 1 1 d . . . . .
O1 O 0.4469(5) 0.0153(12) 0.8245(9) 0.058(2) Uani 1 1 d . . . . .
S1 S 0.41010(14) 0.6512(3) 0.5920(3) 0.0375(7) Uani 1 1 d . . . . .
S2 S 0.500000 0.1228(5) 0.750000 0.0401(10) Uani 1 2 d S T P . .

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
Br1 0.0367(8) 0.0633(10) 0.0481(9) 0.0020(5) -0.0079(5) 0.0085(5)
C1 0.032(5) 0.025(5) 0.037(5) 0.015(4) -0.004(4) 0.011(4)
C2 0.029(5) 0.059(7) 0.034(5) 0.003(5) 0.002(4) -0.005(5)
C3 0.032(5) 0.029(5) 0.039(5) 0.000(4) 0.007(4) 0.004(4)
C4 0.038(5) 0.039(5) 0.020(4) -0.004(4) 0.001(4) 0.003(4)
O1 0.058(5) 0.055(5) 0.059(5) 0.018(4) 0.002(4) -0.028(4)
S1 0.0257(12) 0.0344(14) 0.0500(16) 0.0007(11) -0.0012(10) 0.0004(10)
S2 0.040(2) 0.0329(18) 0.044(2) 0.000 -0.0056(16) 0.000

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Br1 C1 1.872(8) . ?
C1 C2 1.324(13) . ?
C1 S1 1.731(10) . ?
C2 C3 1.412(13) . ?
C2 H2 0.9300 . ?
C3 C4 1.392(13) . ?
C3 S2 1.755(9) . ?
C4 C4 1.456(17) 2_656 ?
C4 S1 1.701(9) . ?
O1 S2 1.424(8) . ?

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
C2 C1 S1 114.6(7) . . ?
C2 C1 Br1 127.3(8) . . ?
S1 C1 Br1 118.0(5) . . ?
C1 C2 C3 110.9(10) . . ?
C1 C2 H2 124.5 . . ?
C3 C2 H2 124.5 . . ?
C4 C3 C2 112.8(9) . . ?
C4 C3 S2 110.1(7) . . ?
C2 C3 S2 137.1(8) . . ?
C3 C4 C4 113.2(5) . 2_656 ?
C3 C4 S1 111.6(7) . . ?
C4 C4 S1 135.0(3) 2_656 . ?
C4 S1 C1 90.0(4) . . ?
O1 S2 O1 116.6(8) . 2_656 ?
O1 S2 C3 113.1(5) . 2_656 ?
O1 S2 C3 109.2(5) 2_656 2_656 ?
O1 S2 C3 109.2(5) . . ?
O1 S2 C3 113.1(5) 2_656 . ?
C3 S2 C3 93.3(6) 2_656 . ?

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 C1 C2 C3 2.7(12) . . . . ?
Br1 C1 C2 C3 -177.8(7) . . . . ?
C1 C2 C3 C4 -3.8(12) . . . . ?
C1 C2 C3 S2 177.9(9) . . . . ?
C2 C3 C4 C4 179.0(10) . . . 2_656 ?
S2 C3 C4 C4 -2.3(13) . . . 2_656 ?
C2 C3 C4 S1 3.3(11) . . . . ?
S2 C3 C4 S1 -177.9(5) . . . . ?
C3 C4 S1 C1 -1.5(8) . . . . ?
C4 C4 S1 C1 -175.9(14) 2_656 . . . ?
C2 C1 S1 C4 -0.7(9) . . . . ?
Br1 C1 S1 C4 179.7(6) . . . . ?
C4 C3 S2 O1 116.7(8) . . . . ?
C2 C3 S2 O1 -65.0(12) . . . . ?
C4 C3 S2 O1 -111.7(8) . . . 2_656 ?
C2 C3 S2 O1 66.6(12) . . . 2_656 ?
C4 C3 S2 C3 0.8(5) . . . 2_656 ?
C2 C3 S2 C3 179.2(13) . . . 2_656 ?

_refine_diff_density_max         0.910
_refine_diff_density_min         -1.116
_refine_diff_density_rms         0.236

_shelx_res_file                  
;
TITL tref_a.res in C2/c
    tref.res
    created by SHELXL-2019/2 at 07:41:05 on 26-Dec-2023
REM Old TITL tref in C2/c
REM SHELXT solution in C2/c: R1 0.189, Rweak 0.002, Alpha 0.018
REM <I/s> 0.424 for 95 systematic absences, Orientation as input
REM Formula found by SHELXT: C8 O2 S3 Br2
CELL 0.71073 16.4117 6.9676 9.5683 90 99.339 90
ZERR 4 0.0033 0.0014 0.0019 0 0.03 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H Br O S
UNIT 32 8 8 8 12

L.S. 30
PLAN  5
CONF
HTAB
BOND $H
list 4
MORE -1
BOND $H
fmap 2 53
acta
SHEL 999 0.845
OMIT -12 0 2
OMIT-6 6 6
REM <olex2.extras>
REM <HklSrc "%.\\tref.hkl">
REM </olex2.extras>

WGHT    0.052300   19.981298
EXTI    0.009477
FVAR       0.29491
BR1   3    0.269777    0.552124    0.346365    11.00000    0.03673    0.06327 =
         0.04812    0.00200   -0.00791    0.00847
C1    1    0.354307    0.474850    0.490827    11.00000    0.03157    0.02515 =
         0.03700    0.01458   -0.00373    0.01134
C2    1    0.377773    0.297133    0.525811    11.00000    0.02904    0.05901 =
         0.03365    0.00345    0.00236   -0.00519
AFIX  43
H2    2    0.355186    0.187873    0.478837    11.00000   -1.20000
AFIX   0
C3    1    0.441696    0.295591    0.644005    11.00000    0.03158    0.02934 =
         0.03866    0.00044    0.00674    0.00395
C4    1    0.467551    0.479181    0.688309    11.00000    0.03842    0.03917 =
         0.01994   -0.00396    0.00137    0.00277
O1    4    0.446947    0.015330    0.824488    11.00000    0.05798    0.05514 =
         0.05913    0.01838    0.00151   -0.02775
S1    5    0.410102    0.651185    0.591978    11.00000    0.02569    0.03443 =
         0.04997    0.00069   -0.00118    0.00044
S2    5    0.500000    0.122781    0.750000    10.50000    0.03956    0.03293 =
         0.04357    0.00000   -0.00561    0.00000
HKLF 4




REM  tref_a.res in C2/c
REM wR2 = 0.1686, GooF = S = 1.168, Restrained GooF = 1.168 for all data
REM R1 = 0.0525 for 687 Fo > 4sig(Fo) and 0.0779 for all 933 data
REM 70 parameters refined using 0 restraints

END

WGHT      0.0549     20.2193

REM No hydrogen bonds found for HTAB generation

REM Highest difference peak  0.910,  deepest hole -1.116,  1-sigma level  0.236
Q1    1   0.3420  0.5578  0.4458  11.00000  0.05    0.91
Q2    1   0.2190  0.7186  0.2408  11.00000  0.05    0.90
Q3    1   0.5000 -0.2062  0.7500  10.50000  0.05    0.88
Q4    1   0.2754  0.3335  0.3428  11.00000  0.05    0.85
Q5    1   0.4379  0.7844  0.6423  11.00000  0.05    0.79
;
_shelx_res_checksum              8001
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_tref_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2378966'
loop_
_audit_author_name
_audit_author_address
'huimin liu'
;ningbo university
China
;
_audit_update_record             
;
2024-08-21 deposited with the CCDC.	2025-06-17 downloaded from the CCDC.
;
_audit_creation_date             2024-01-10
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.286(C8 H4 O2 S3)'
_chemical_formula_sum            'C2.29 H1.14 O0.57 S0.86'
_chemical_formula_weight         65.23
_chemical_melting_point          ?
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'
O O 0.0106 0.0060 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   9.756(2)
_cell_length_b                   12.219(2)
_cell_length_c                   7.5175(15)
_cell_angle_alpha                90
_cell_angle_beta                 102.31(3)
_cell_angle_gamma                90
_cell_volume                     875.5(3)
_cell_formula_units_Z            14
_cell_measurement_reflns_used    4193
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.5
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.802
_exptl_absorpt_correction_T_max  0.812
_exptl_absorpt_correction_T_min  0.723
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.588
_exptl_crystal_size_mid          0.376
_exptl_crystal_size_min          0.087
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3495
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.015
_diffrn_reflns_theta_max         25.015
_diffrn_reflns_theta_min         3.335
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                703
_reflns_number_total             773
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_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    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       0.009(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         773
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0334
_refine_ls_restrained_S_all      1.090
_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)+(0.0512P)²+0.5716P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.0966
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
C1 C 0.4241(2) 0.53402(17) 0.2273(3) 0.0279(5) Uani 1 1 d . . . . .
C2 C 0.3659(2) 0.43057(17) 0.2096(3) 0.0279(5) Uani 1 1 d . . . . .
C3 C 0.2179(2) 0.42942(19) 0.1624(3) 0.0338(5) Uani 1 1 d . . . . .
H3 H 0.162797 0.366614 0.144262 0.041 Uiso 1 1 calc R U . . .
C4 C 0.1672(2) 0.53422(18) 0.1472(3) 0.0354(6) Uani 1 1 d . . . . .
H4 H 0.072048 0.550875 0.118278 0.043 Uiso 1 1 calc R U . . .
O1 O 0.50136(17) 0.26845(12) 0.0874(2) 0.0413(5) Uani 1 1 d . . . . .
S1 S 0.29631(6) 0.63174(4) 0.18651(8) 0.0353(3) Uani 1 1 d . . . . .
S2 S 0.500000 0.33054(6) 0.250000 0.0289(3) Uani 1 2 d S T P . .

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
C1 0.0244(11) 0.0256(11) 0.0327(11) -0.0002(9) 0.0036(8) 0.0016(8)
C2 0.0212(11) 0.0266(11) 0.0339(11) -0.0008(9) 0.0011(8) 0.0014(8)
C3 0.0228(11) 0.0324(11) 0.0433(13) -0.0017(10) 0.0005(9) -0.0032(9)
C4 0.0204(11) 0.0407(13) 0.0425(12) -0.0016(11) 0.0008(9) 0.0038(9)
O1 0.0366(10) 0.0319(8) 0.0519(10) -0.0116(8) 0.0018(7) 0.0022(7)
S1 0.0270(4) 0.0281(4) 0.0480(5) -0.0012(2) 0.0014(3) 0.0056(2)
S2 0.0216(4) 0.0224(5) 0.0398(5) 0.000 0.0000(3) 0.000

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
C1 C1 1.448(4) 2_655 ?
C1 C2 1.380(3) . ?
C1 S1 1.706(2) . ?
C2 C3 1.412(3) . ?
C2 S2 1.769(2) . ?
C3 H3 0.9300 . ?
C3 C4 1.368(3) . ?
C4 H4 0.9300 . ?
C4 S1 1.713(2) . ?
O1 S2 1.4413(16) . ?

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
C1 C1 S1 135.57(7) 2_655 . ?
C2 C1 C1 113.68(12) . 2_655 ?
C2 C1 S1 110.74(16) . . ?
C1 C2 C3 114.25(18) . . ?
C1 C2 S2 110.03(15) . . ?
C3 C2 S2 135.71(16) . . ?
C2 C3 H3 125.0 . . ?
C4 C3 C2 110.08(19) . . ?
C4 C3 H3 125.0 . . ?
C3 C4 H4 123.3 . . ?
C3 C4 S1 113.42(16) . . ?
S1 C4 H4 123.3 . . ?
C1 S1 C4 91.50(11) . . ?
C2 S2 C2 92.57(14) 2_655 . ?
O1 S2 C2 110.99(10) 2_655 2_655 ?
O1 S2 C2 111.68(10) 2_655 . ?
O1 S2 C2 110.99(10) . . ?
O1 S2 C2 111.68(10) . 2_655 ?
O1 S2 O1 116.48(14) . 2_655 ?

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
C1 C1 C2 C3 -179.0(2) 2_655 . . . ?
C1 C1 C2 S2 0.1(3) 2_655 . . . ?
C1 C1 S1 C4 179.2(3) 2_655 . . . ?
C1 C2 C3 C4 -0.6(3) . . . . ?
C1 C2 S2 C2 -0.05(11) . . . 2_655 ?
C1 C2 S2 O1 113.75(17) . . . 2_655 ?
C1 C2 S2 O1 -114.46(16) . . . . ?
C2 C1 S1 C4 0.17(16) . . . . ?
C2 C3 C4 S1 0.7(3) . . . . ?
C3 C2 S2 C2 178.9(3) . . . 2_655 ?
C3 C2 S2 O1 64.5(3) . . . . ?
C3 C2 S2 O1 -67.3(3) . . . 2_655 ?
C3 C4 S1 C1 -0.53(17) . . . . ?
S1 C1 C2 C3 0.2(3) . . . . ?
S1 C1 C2 S2 179.40(9) . . . . ?
S2 C2 C3 C4 -179.51(17) . . . . ?

_shelx_res_file                  
;
TITL tref in C2/c #15
    tref.res
    created by SHELXL-2018/3 at 09:30:23 on 10-Jan-2024
REM reset to C2/c #15
CELL 0.71073 9.7556 12.2185 7.5175 90 102.305 90
ZERR 14 0.002 0.0024 0.0015 0 0.03 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H O S
UNIT 32 16 8 12

L.S. 4 0 0
PLAN  5
CONF
BOND $H
HTAB
MORE -1
fmap 2 53
ACTA
SHEL 999 0.84
OMIT 1 11 4
REM <olex2.extras>
REM <HklSrc "%.\\tref.hkl">
REM </olex2.extras>

WGHT    0.051200    0.571600
EXTI    0.008754
FVAR       0.19432
C1    1    0.424054    0.534021    0.227257    11.00000    0.02440    0.02561 =
         0.03267   -0.00019    0.00357    0.00164
C2    1    0.365906    0.430573    0.209563    11.00000    0.02125    0.02656 =
         0.03385   -0.00080    0.00107    0.00143
C3    1    0.217863    0.429423    0.162368    11.00000    0.02278    0.03238 =
         0.04326   -0.00172    0.00053   -0.00323
AFIX  43
H3    2    0.162797    0.366614    0.144262    11.00000   -1.20000
AFIX   0
C4    1    0.167235    0.534225    0.147159    11.00000    0.02041    0.04074 =
         0.04246   -0.00159    0.00075    0.00377
AFIX  43
H4    2    0.072048    0.550875    0.118278    11.00000   -1.20000
AFIX   0
O1    3    0.501362    0.268452    0.087363    11.00000    0.03663    0.03186 =
         0.05191   -0.01165    0.00185    0.00215
S1    4    0.296307    0.631743    0.186510    11.00000    0.02697    0.02809 =
         0.04798   -0.00120    0.00142    0.00560
S2    4    0.500000    0.330543    0.250000    10.50000    0.02160    0.02236 =
         0.03981    0.00000    0.00005    0.00000
HKLF 4




REM  tref in C2/c #15
REM wR2 = 0.0966, GooF = S = 1.090, Restrained GooF = 1.090 for all data
REM R1 = 0.0334 for 703 Fo > 4sig(Fo) and 0.0354 for all 773 data
REM 61 parameters refined using 0 restraints

END

WGHT      0.0512      0.5714

REM No hydrogen bonds found for HTAB generation

REM Highest difference peak  0.380,  deepest hole -0.345,  1-sigma level  0.062
Q1    1   0.4239  0.3792  0.2247  11.00000  0.05    0.38
Q2    1   0.2299  0.5814  0.1627  11.00000  0.05    0.32
Q3    1   0.3743  0.5814  0.2112  11.00000  0.05    0.30
Q4    1   0.3929  0.4874  0.2716  11.00000  0.05    0.28
Q5    1   0.3961  0.4802  0.1736  11.00000  0.05    0.26
;
_shelx_res_checksum              24830
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_tref_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 2378958'
loop_
_audit_author_name
_audit_author_address
'huimin liu'
;ningbo university
China
;
_audit_update_record             
;
2024-08-21 deposited with the CCDC.	2025-06-17 downloaded from the CCDC.
;
_audit_creation_date             2024-01-10
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.333(C8 H2 I2 O2 S3)'
_chemical_formula_sum            'C2.67 H0.67 I0.67 O0.67 S'
_chemical_formula_weight         160.03
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y, z+1/2'
'x+1/2, -y, z'

_cell_length_a                   18.519(4)
_cell_length_b                   4.9155(10)
_cell_length_c                   12.812(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1166.2(4)
_cell_formula_units_Z            12
_cell_measurement_reflns_used    4193
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.5
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.904
_exptl_absorpt_correction_T_max  0.812
_exptl_absorpt_correction_T_min  0.723
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.734
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.417
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.070
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1098
_diffrn_reflns_av_unetI/netI     0.1255
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8041
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.013
_diffrn_reflns_theta_max         25.013
_diffrn_reflns_theta_min         3.180
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.906
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                1752
_reflns_number_total             2043
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_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    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         1.277
_refine_diff_density_min         -1.084
_refine_diff_density_rms         0.206
_refine_ls_abs_structure_details 
;
 Flack x determined using 617 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(5)
_refine_ls_extinction_coef       0.0040(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         2043
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0524
_refine_ls_restrained_S_all      1.030
_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)+(0.0004P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1010
_refine_ls_wR_factor_ref         0.1135
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
C1 C -0.6679(8) -1.214(3) -0.0273(15) 0.033(4) Uani 1 1 d . . . . .
C2 C -0.6659(8) -1.187(3) -0.1333(15) 0.035(4) Uani 1 1 d . . . . .
H2 H -0.698712 -1.267598 -0.178658 0.042 Uiso 1 1 calc R U . . .
C3 C -0.6073(8) -1.019(3) -0.1660(13) 0.029(4) Uani 1 1 d . . . . .
C4 C -0.5679(9) -0.923(3) -0.0860(15) 0.032(4) Uani 1 1 d . . . . .
C5 C -0.5106(8) -0.733(3) -0.1187(13) 0.028(4) Uani 1 1 d . . . . .
C6 C -0.5111(9) -0.690(3) -0.2241(15) 0.032(4) Uani 1 1 d . . . . .
C7 C -0.4562(8) -0.503(3) -0.2586(15) 0.033(4) Uani 1 1 d . . . . .
H7 H -0.448255 -0.449585 -0.327310 0.039 Uiso 1 1 calc R U . . .
C8 C -0.4178(8) -0.417(3) -0.1739(15) 0.033(4) Uani 1 1 d . . . . .
I1 I -0.74317(7) -1.41191(18) 0.06344(9) 0.0427(4) Uani 1 1 d . . . . .
I2 I -0.33049(6) -0.14587(19) -0.17830(12) 0.0442(4) Uani 1 1 d . . . . .
O1 O -0.5528(6) -1.065(2) -0.3609(10) 0.035(3) Uani 1 1 d . . . . .
O2 O -0.6368(7) -0.688(2) -0.3194(11) 0.045(3) Uani 1 1 d . . . . .
S1 S -0.5981(2) -1.0349(9) 0.0326(4) 0.0362(11) Uani 1 1 d . . . . .
S2 S -0.5810(2) -0.8697(8) -0.2852(4) 0.0299(10) Uani 1 1 d . . . . .
S3 S -0.4445(2) -0.5501(9) -0.0561(4) 0.0356(11) Uani 1 1 d . . . . .

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
C1 0.024(9) 0.034(8) 0.041(12) 0.001(8) -0.002(7) -0.006(7)
C2 0.037(10) 0.036(9) 0.033(11) -0.007(7) -0.001(8) 0.007(7)
C3 0.023(9) 0.042(8) 0.022(10) 0.009(7) -0.002(7) 0.000(6)
C4 0.032(10) 0.027(8) 0.036(12) 0.004(8) 0.003(8) -0.011(7)
C5 0.025(8) 0.040(9) 0.021(9) -0.010(7) 0.002(7) 0.006(7)
C6 0.030(9) 0.029(8) 0.038(11) -0.002(7) 0.000(8) -0.006(7)
C7 0.024(9) 0.036(9) 0.039(11) 0.001(8) 0.007(8) 0.016(7)
C8 0.033(9) 0.032(7) 0.034(11) -0.009(9) 0.001(9) 0.004(6)
I1 0.0366(7) 0.0522(7) 0.0392(8) 0.0056(8) 0.0051(6) -0.0116(5)
I2 0.0409(7) 0.0397(6) 0.0519(9) 0.0022(7) -0.0014(7) -0.0123(5)
O1 0.032(7) 0.039(6) 0.035(8) -0.003(5) 0.007(6) 0.003(5)
O2 0.032(7) 0.048(7) 0.056(10) 0.014(6) -0.011(6) 0.016(6)
S1 0.031(2) 0.048(3) 0.030(3) -0.0001(19) 0.0015(19) -0.0072(19)
S2 0.031(2) 0.035(2) 0.024(2) 0.0040(16) -0.0009(19) -0.0011(17)
S3 0.033(2) 0.043(2) 0.031(3) -0.002(2) -0.002(2) -0.0093(18)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
C1 C2 1.37(3) . ?
C1 I1 2.059(16) . ?
C1 S1 1.743(15) . ?
C2 H2 0.9300 . ?
C2 C3 1.43(2) . ?
C3 C4 1.34(2) . ?
C3 S2 1.764(16) . ?
C4 C5 1.47(2) . ?
C4 S1 1.710(18) . ?
C5 C6 1.37(2) . ?
C5 S3 1.717(16) . ?
C6 C7 1.44(2) . ?
C6 S2 1.753(17) . ?
C7 H7 0.9300 . ?
C7 C8 1.37(2) . ?
C8 I2 2.095(14) . ?
C8 S3 1.718(19) . ?
O1 S2 1.460(12) . ?
O2 S2 1.436(11) . ?

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
C2 C1 I1 128.8(12) . . ?
C2 C1 S1 111.6(13) . . ?
S1 C1 I1 119.5(10) . . ?
C1 C2 H2 124.1 . . ?
C1 C2 C3 111.7(15) . . ?
C3 C2 H2 124.1 . . ?
C2 C3 S2 134.9(12) . . ?
C4 C3 C2 113.2(15) . . ?
C4 C3 S2 111.3(12) . . ?
C3 C4 C5 113.4(15) . . ?
C3 C4 S1 112.7(12) . . ?
C5 C4 S1 133.8(14) . . ?
C4 C5 S3 135.4(13) . . ?
C6 C5 C4 112.0(16) . . ?
C6 C5 S3 112.6(14) . . ?
C5 C6 C7 113.5(17) . . ?
C5 C6 S2 111.6(14) . . ?
C7 C6 S2 134.9(15) . . ?
C6 C7 H7 125.6 . . ?
C8 C7 C6 108.7(17) . . ?
C8 C7 H7 125.6 . . ?
C7 C8 I2 125.3(14) . . ?
C7 C8 S3 115.5(12) . . ?
S3 C8 I2 119.2(10) . . ?
C4 S1 C1 90.8(8) . . ?
C6 S2 C3 91.6(8) . . ?
O1 S2 C3 113.5(7) . . ?
O1 S2 C6 111.4(7) . . ?
O2 S2 C3 108.9(8) . . ?
O2 S2 C6 110.7(7) . . ?
O2 S2 O1 117.7(8) . . ?
C5 S3 C8 89.7(8) . . ?

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
C1 C2 C3 C4 -1(2) . . . . ?
C1 C2 C3 S2 -170.3(13) . . . . ?
C2 C1 S1 C4 0.7(14) . . . . ?
C2 C3 C4 C5 -175.6(12) . . . . ?
C2 C3 C4 S1 1.5(19) . . . . ?
C2 C3 S2 C6 173.2(16) . . . . ?
C2 C3 S2 O1 -72.6(17) . . . . ?
C2 C3 S2 O2 60.7(17) . . . . ?
C3 C4 C5 C6 2(2) . . . . ?
C3 C4 C5 S3 -179.4(13) . . . . ?
C3 C4 S1 C1 -1.3(14) . . . . ?
C4 C3 S2 C6 3.7(13) . . . . ?
C4 C3 S2 O1 117.9(13) . . . . ?
C4 C3 S2 O2 -108.8(13) . . . . ?
C4 C5 C6 C7 179.4(12) . . . . ?
C4 C5 C6 S2 1(2) . . . . ?
C4 C5 S3 C8 -179.0(18) . . . . ?
C5 C4 S1 C1 175.1(17) . . . . ?
C5 C6 C7 C8 0(2) . . . . ?
C5 C6 S2 C3 -2.7(14) . . . . ?
C5 C6 S2 O1 -118.8(14) . . . . ?
C5 C6 S2 O2 108.2(14) . . . . ?
C6 C5 S3 C8 -0.1(14) . . . . ?
C6 C7 C8 I2 179.3(10) . . . . ?
C6 C7 C8 S3 0.1(16) . . . . ?
C7 C6 S2 C3 179.6(16) . . . . ?
C7 C6 S2 O1 63.5(17) . . . . ?
C7 C6 S2 O2 -69.5(18) . . . . ?
C7 C8 S3 C5 0.0(12) . . . . ?
I1 C1 C2 C3 176.2(10) . . . . ?
I1 C1 S1 C4 -175.9(9) . . . . ?
I2 C8 S3 C5 -179.2(8) . . . . ?
S1 C1 C2 C3 0.0(18) . . . . ?
S1 C4 C5 C6 -174.6(14) . . . . ?
S1 C4 C5 S3 4(3) . . . . ?
S2 C3 C4 C5 -3.7(19) . . . . ?
S2 C3 C4 S1 173.4(8) . . . . ?
S2 C6 C7 C8 177.4(13) . . . . ?
S3 C5 C6 C7 0(2) . . . . ?
S3 C5 C6 S2 -178.0(7) . . . . ?

_shelx_res_file                  
;
TITL tref in Pca21 #29
    tref.res
    created by SHELXL-2018/3 at 10:45:44 on 10-Jan-2024
REM reset to Pca21 #29
CELL 0.71073 18.5189 4.9155 12.8116 90 90 90
ZERR 12 0.0037 0.001 0.0026 0 0 0
LATT -1
SYMM -X,-Y,0.5+Z
SYMM 0.5-X,+Y,0.5+Z
SYMM 0.5+X,-Y,+Z
SFAC C H I O S
UNIT 32 8 8 8 12

L.S. 4 0 0
PLAN  2
CONF
BOND $H
HTAB
MORE -1
fmap 2 53
acta
SHEL 999 0.84
OMIT 13 4 2
OMIT 11 5 0
REM <olex2.extras>
REM <HklSrc "%.\\tref.hkl">
REM </olex2.extras>

WGHT    0.000400
EXTI    0.003994
FVAR       0.27972
C1    1   -0.667917   -1.214043   -0.027281    11.00000    0.02412    0.03353 =
         0.04128    0.00052   -0.00195   -0.00560
C2    1   -0.665874   -1.186787   -0.133325    11.00000    0.03691    0.03584 =
         0.03324   -0.00669   -0.00107    0.00665
AFIX  43
H2    2   -0.698712   -1.267598   -0.178658    11.00000   -1.20000
AFIX   0
C3    1   -0.607263   -1.019359   -0.166007    11.00000    0.02299    0.04155 =
         0.02226    0.00853   -0.00176   -0.00007
C4    1   -0.567899   -0.922628   -0.086009    11.00000    0.03241    0.02668 =
         0.03637    0.00380    0.00319   -0.01115
C5    1   -0.510617   -0.732807   -0.118696    11.00000    0.02513    0.03954 =
         0.02072   -0.01024    0.00188    0.00624
C6    1   -0.511061   -0.689587   -0.224082    11.00000    0.02978    0.02855 =
         0.03794   -0.00227    0.00033   -0.00572
C7    1   -0.456223   -0.502825   -0.258612    11.00000    0.02400    0.03579 =
         0.03894    0.00077    0.00659    0.01575
AFIX  43
H7    2   -0.448255   -0.449585   -0.327310    11.00000   -1.20000
AFIX   0
C8    1   -0.417819   -0.416670   -0.173887    11.00000    0.03283    0.03217 =
         0.03375   -0.00922    0.00067    0.00399
I1    3   -0.743173   -1.411914    0.063438    11.00000    0.03660    0.05224 =
         0.03918    0.00558    0.00511   -0.01160
I2    3   -0.330492   -0.145866   -0.178296    11.00000    0.04089    0.03966 =
         0.05192    0.00217   -0.00135   -0.01230
O1    4   -0.552828   -1.065003   -0.360891    11.00000    0.03216    0.03931 =
         0.03452   -0.00251    0.00737    0.00318
O2    4   -0.636819   -0.687632   -0.319351    11.00000    0.03238    0.04788 =
         0.05604    0.01406   -0.01057    0.01559
S1    5   -0.598059   -1.034914    0.032589    11.00000    0.03069    0.04753 =
         0.03050   -0.00005    0.00150   -0.00716
S2    5   -0.580962   -0.869691   -0.285237    11.00000    0.03073    0.03489 =
         0.02393    0.00398   -0.00087   -0.00106
S3    5   -0.444530   -0.550052   -0.056142    11.00000    0.03272    0.04263 =
         0.03136   -0.00232   -0.00153   -0.00925
HKLF 4




REM  tref in Pca21 #29
REM wR2 = 0.1135, GooF = S = 1.030, Restrained GooF = 1.030 for all data
REM R1 = 0.0524 for 1752 Fo > 4sig(Fo) and 0.0615 for all 2043 data
REM 137 parameters refined using 1 restraints

END

WGHT      0.0001      0.0000

REM No hydrogen bonds found for HTAB generation

REM Highest difference peak  1.277,  deepest hole -1.084,  1-sigma level  0.206
Q1    1  -0.7425 -1.2649  0.0633  11.00000  0.05    1.28
Q2    1  -0.7405 -1.6489  0.0617  11.00000  0.05    1.19
;
_shelx_res_checksum              59294
_olex2_submission_special_instructions 'No special instructions were received'
