# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_js124b
_database_code_depnum_ccdc_archive 'CCDC 2330491'
loop_
_audit_author_name
_audit_author_address
'Dr. Richard J. Staples'
;Michigan State University
United States of America
;
_audit_update_record             
;
2024-02-02 deposited with the CCDC.	2024-03-26 downloaded from the CCDC.
;
_audit_creation_date             2024-01-29
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
staples@chemistry.msu.edu
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C8 H5 Cl2 N7 O2, 1.327(C1.507 H4.52 O0.753 S0.753)'
_chemical_formula_sum            'C10 H11 Cl2 N7 O3 S'
_chemical_formula_weight         380.22
_chemical_melting_point          351
_chemical_oxdiff_formula         C8H5Cl2N7O2(CH3SOCH3)
_chemical_oxdiff_usercomment     Sohan-163
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   20.9148(9)
_cell_length_b                   17.5238(6)
_cell_length_c                   4.21488(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1544.78(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2737
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.9330
_cell_measurement_theta_min      4.2070
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.303
_exptl_absorpt_correction_T_max  0.964
_exptl_absorpt_correction_T_min  0.696
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.104a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             776
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 -1 0.0524
1 -11 0 0.0143
-2 11 0 0.0077
-14 0 0 0.0307
14 0 0 0.0106
2 3 3 0.0571

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DMSO'
_exptl_crystal_size_max          0.121
_exptl_crystal_size_mid          0.047
_exptl_crystal_size_min          0.026
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0104 -1.0002 -1.0013 -0.0904 -0.3229 -0.1708
0.8778 -11.2869 0.2819 -0.9916 0.1294 -0.0098
-2.3730 11.0508 -0.4279 0.9848 -0.1284 -0.1141
-13.5735 0.2031 -0.0349 0.1472 0.4204 -0.8952
13.5897 -0.2673 0.0124 -0.1530 -0.4279 0.8920
2.4209 3.2217 2.5788 0.2663 0.7515 0.6036

_exptl_special_details           
;
Data was collected using a Rigaku Synergy S Diffractometer diffractometer equipped 
with an Oxford 800 low-temperature apparatus.  A suitable 
crystal was chosen and mounted on a nylon loop using Paratone oil.  Data  were 
measured based on the Pre-Experiment plugin of CrysAlisPro software.  Cell 
parameters were retrieved using CrysAlisPro software and data reduction was 
performed using the intergration software inside the CrysAlisPro which 
corrects for Lp.  The structure was solved by the direct method using the 
SHELXT program and refined by least squares method on F2, SHELXL,
 incorporated in OLEX2. 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0642
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            6062
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.063
_diffrn_reflns_theta_min         4.228
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -42.00 -13.00   0.50    1.20    --  -86.25  36.00 151.00   58
  2  ω    -73.00 -35.00   0.50    0.30    --  -47.36  87.00 -31.00   76
  3  ω    -15.00  11.00   0.50    0.30    --  -47.36  87.00 -31.00   52
  4  ω    -29.00  25.00   0.50    0.30    --  -47.36  19.00-120.00  108
  5  ω    -34.00  20.00   0.50    0.30    --  -47.36  37.00-180.00  108
  6  ω    123.00 163.00   0.50    1.20    --  107.75  61.00-150.00   80
  7  ω    103.00 171.00   0.50    1.20    --  107.75  87.00 -31.00  136
  8  ω     98.00 177.00   0.50    1.20    --  107.75 125.00 -90.00  158
  9  ω     81.00 142.00   0.50    1.20    --  107.75 153.00  16.00  122
 10  ω    126.00 151.00   0.50    1.20    --  107.75  36.00 151.00   50
 11  ω     96.00 121.00   0.50    1.20    --  107.75  36.00 151.00   50
 12  ω     41.00  66.00   0.50    1.20    --  107.75 -61.00  60.00   50
 13  ω     42.00  68.00   0.50    1.20    --  107.75 -61.00 -60.00   52
 14  ω     42.00  67.00   0.50    1.20    --  107.75 -61.00 -90.00   50
 15  ω     49.00  99.00   0.50    1.20    --  107.75 -77.00-150.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0095489000
_diffrn_orient_matrix_UB_12      0.0871946000
_diffrn_orient_matrix_UB_13      0.0032784000
_diffrn_orient_matrix_UB_21      -0.0319033000
_diffrn_orient_matrix_UB_22      -0.0057441000
_diffrn_orient_matrix_UB_23      0.3285239000
_diffrn_orient_matrix_UB_31      0.0656890000
_diffrn_orient_matrix_UB_32      0.0099723000
_diffrn_orient_matrix_UB_33      0.1599395000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           1
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_source_voltage           50
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1312
_reflns_number_total             1674
_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       'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.647
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         1674
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0447
_refine_ls_restrained_S_all      1.033
_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/[σ²(Fo²)+(0.0538P)²+1.0442P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1214
_refine_special_details          
;
The structure was refined by Least Squares SHELXL incorporated 
in Olex2 software program. All non-hydrogen atoms were refined anisotropically. 
Hydrogen atom positions were calculated geometrically and refined using the 
riding model, except for the hydrogen atom on the non-carbon atom(s) which were found 
by difference Fourier methods and refined isotropically when data permits.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 S1-C5B \\sim S1-C5
 with sigma of 0.02
 C5B-S1B \\sim C5-S1B
 with sigma of 0.02
 S1-C5 \\sim S1B-C5B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(S1B) = Uanis(S1)
Uanis(C5B) = Uanis(C5)
4. Others
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=1-FVAR(1)
 Sof(S1)=Sof(O2B)=0.5*(1-FVAR(2))
 Sof(S1B)=Sof(O2)=0.5*FVAR(2)
 Sof(C5B)=Sof(H5BA)=Sof(H5BB)=Sof(H5BC)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B)
5.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C5B(H5BA,H5BB,H5BC)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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
Cl1 Cl 0.32418(3) 0.53307(4) 0.66099(18) 0.0348(2) Uani 1 1 d . . . . .
O1 O 0.39290(8) 0.40761(10) 1.0847(5) 0.0265(4) Uani 1 1 d . . . . .
N1 N 0.59759(15) 0.250000 0.5301(8) 0.0259(7) Uani 1 2 d S T P . .
H1 H 0.634(3) 0.250000 0.408(14) 0.053(15) Uiso 1 2 d S . P . .
N2 N 0.56826(10) 0.31404(11) 0.6096(5) 0.0246(5) Uani 1 1 d . . . . .
N4 N 0.42392(10) 0.33598(12) 1.0669(6) 0.0270(5) Uani 1 1 d . . . . .
N5 N 0.47159(10) 0.42164(11) 0.7409(5) 0.0247(5) Uani 1 1 d . . . . .
C1 C 0.51470(11) 0.29020(13) 0.7554(6) 0.0205(5) Uani 1 1 d . . . . .
C2 C 0.46896(11) 0.34801(13) 0.8613(6) 0.0210(5) Uani 1 1 d . . . . .
C3 C 0.42443(11) 0.45364(13) 0.8838(6) 0.0220(5) Uani 1 1 d . . . . .
C4 C 0.40106(13) 0.53369(14) 0.8484(7) 0.0260(5) Uani 1 1 d . . . . .
H4A H 0.431622 0.563434 0.718434 0.031 Uiso 1 1 calc R U . . .
H4B H 0.397882 0.558137 1.059566 0.031 Uiso 1 1 calc R U . . .
S1 S 0.73169(6) 0.250000 -0.0395(3) 0.0292(3) Uani 0.753(2) 2 d DS T P A 2
O2B O 0.71606(18) 0.250000 0.3102(10) 0.0365(9) Uani 0.753(2) 2 d S T P A 2
C5 C 0.7809(4) 0.1698(4) -0.093(3) 0.064(3) Uani 0.753(2) 1 d D . P A 2
H5A H 0.820036 0.175842 0.032254 0.095 Uiso 0.753(2) 1 calc R U P A 2
H5B H 0.792084 0.165011 -0.318312 0.095 Uiso 0.753(2) 1 calc R U P A 2
H5C H 0.758143 0.123886 -0.024098 0.095 Uiso 0.753(2) 1 calc R U P A 2
S1B S 0.75933(19) 0.250000 0.1495(10) 0.0292(3) Uani 0.247(2) 2 d DS T P A 1
O2 O 0.6871(5) 0.250000 0.100(3) 0.029(2) Uani 0.247(2) 2 d S T P A 1
C5B C 0.7998(18) 0.1855(16) -0.089(10) 0.064(3) Uani 0.247(2) 1 d D . P A 1
H5BA H 0.782583 0.187607 -0.304591 0.095 Uiso 0.247(2) 1 calc R U P A 1
H5BB H 0.794379 0.133845 -0.003304 0.095 Uiso 0.247(2) 1 calc R U P A 1
H5BC H 0.845385 0.198455 -0.092428 0.095 Uiso 0.247(2) 1 calc R U P A 1

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
Cl1 0.0282(3) 0.0292(3) 0.0470(4) 0.0036(3) -0.0037(3) 0.0055(2)
O1 0.0269(9) 0.0185(8) 0.0342(10) 0.0011(7) 0.0063(8) 0.0036(7)
N1 0.0241(15) 0.0190(13) 0.0345(17) 0.000 0.0070(14) 0.000
N2 0.0244(11) 0.0181(9) 0.0312(11) 0.0005(8) 0.0037(9) 0.0006(8)
N4 0.0271(11) 0.0168(9) 0.0371(12) 0.0009(9) 0.0051(10) 0.0042(8)
N5 0.0257(10) 0.0179(9) 0.0304(11) 0.0006(8) 0.0016(10) 0.0018(8)
C1 0.0187(11) 0.0191(11) 0.0238(11) -0.0002(9) -0.0002(10) 0.0004(9)
C2 0.0204(11) 0.0171(10) 0.0254(12) -0.0010(9) -0.0024(10) -0.0001(9)
C3 0.0207(11) 0.0191(11) 0.0263(12) 0.0009(9) -0.0020(10) -0.0010(9)
C4 0.0263(12) 0.0201(11) 0.0316(13) -0.0004(10) 0.0005(11) 0.0022(10)
S1 0.0259(6) 0.0294(6) 0.0322(6) 0.000 -0.0035(5) 0.000
O2B 0.0261(18) 0.041(2) 0.042(2) 0.000 0.0155(19) 0.000
C5 0.073(7) 0.067(4) 0.050(2) 0.026(3) 0.035(5) 0.044(4)
S1B 0.0259(6) 0.0294(6) 0.0322(6) 0.000 -0.0035(5) 0.000
O2 0.019(5) 0.046(6) 0.021(5) 0.000 0.008(5) 0.000
C5B 0.073(7) 0.067(4) 0.050(2) 0.026(3) 0.035(5) 0.044(4)

_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
Cl1 C4 1.792(3) . ?
O1 N4 1.415(3) . ?
O1 C3 1.343(3) . ?
N1 H1 0.93(6) . ?
N1 N2 1.322(3) 7_565 ?
N1 N2 1.322(3) . ?
N2 C1 1.344(3) . ?
N4 C2 1.297(3) . ?
N5 C2 1.388(3) . ?
N5 C3 1.285(3) . ?
C1 C1 1.409(4) 7_565 ?
C1 C2 1.463(3) . ?
C3 C4 1.493(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
S1 O2B 1.510(4) . ?
S1 C5 1.757(7) . ?
S1 C5 1.757(7) 7_565 ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
S1B O2 1.525(11) . ?
S1B C5B 1.733(17) 7_565 ?
S1B C5B 1.733(17) . ?
C5B H5BA 0.9800 . ?
C5B H5BB 0.9800 . ?
C5B H5BC 0.9800 . ?

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 O1 N4 105.93(18) . . ?
N2 N1 H1 121.8(3) . . ?
N2 N1 H1 121.8(2) 7_565 . ?
N2 N1 N2 116.2(3) . 7_565 ?
N1 N2 C1 103.8(2) . . ?
C2 N4 O1 102.96(18) . . ?
C3 N5 C2 101.8(2) . . ?
N2 C1 C1 108.11(13) . 7_565 ?
N2 C1 C2 118.0(2) . . ?
C1 C1 C2 133.82(13) 7_565 . ?
N4 C2 N5 115.1(2) . . ?
N4 C2 C1 124.5(2) . . ?
N5 C2 C1 120.4(2) . . ?
O1 C3 C4 117.8(2) . . ?
N5 C3 O1 114.2(2) . . ?
N5 C3 C4 127.9(2) . . ?
Cl1 C4 H4A 109.8 . . ?
Cl1 C4 H4B 109.8 . . ?
C3 C4 Cl1 109.40(17) . . ?
C3 C4 H4A 109.8 . . ?
C3 C4 H4B 109.8 . . ?
H4A C4 H4B 108.2 . . ?
O2B S1 C5 104.7(4) . . ?
C5 S1 C5 106.2(5) 7_565 . ?
S1 C5 H5A 109.5 . . ?
S1 C5 H5B 109.5 . . ?
S1 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O2 S1B C5B 113.9(16) . 7_565 ?
O2 S1B C5B 113.9(16) . . ?
C5B S1B C5B 81(2) 7_565 . ?
S1B C5B H5BA 109.5 . . ?
S1B C5B H5BB 109.5 . . ?
S1B C5B H5BC 109.5 . . ?
H5BA C5B H5BB 109.5 . . ?
H5BA C5B H5BC 109.5 . . ?
H5BB C5B H5BC 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1 O2B 0.93(6) 1.76(6) 2.645(5) 160(5) . yes
N1 H1 O2 0.93(6) 1.70(6) 2.606(10) 164(5) . yes

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
O1 N4 C2 N5 0.6(3) . . . . ?
O1 N4 C2 C1 -179.2(2) . . . . ?
O1 C3 C4 Cl1 -67.3(3) . . . . ?
N1 N2 C1 C1 -0.1(2) . . . 7_565 ?
N1 N2 C1 C2 -177.0(2) . . . . ?
N2 N1 N2 C1 0.1(4) 7_565 . . . ?
N2 C1 C2 N4 -162.8(2) . . . . ?
N2 C1 C2 N5 17.4(4) . . . . ?
N4 O1 C3 N5 -0.4(3) . . . . ?
N4 O1 C3 C4 178.8(2) . . . . ?
N5 C3 C4 Cl1 111.7(3) . . . . ?
C1 C1 C2 N4 21.2(3) 7_565 . . . ?
C1 C1 C2 N5 -158.59(15) 7_565 . . . ?
C2 N5 C3 O1 0.7(3) . . . . ?
C2 N5 C3 C4 -178.4(3) . . . . ?
C3 O1 N4 C2 -0.2(3) . . . . ?
C3 N5 C2 N4 -0.8(3) . . . . ?
C3 N5 C2 C1 179.0(2) . . . . ?

_shelx_res_file                  
;
TITL js124b_a.res in Pnma
    js124b.res
    created by SHELXL-2018/3 at 10:38:09 on 29-Jan-2024
REM Old TITL JS124B in Pnma
REM SHELXT solution in Pnma: R1 0.161, Rweak 0.023, Alpha 0.016
REM <I/s> 0.336 for 265 systematic absences, Orientation as input
REM Formula found by SHELXT: C19 N1 O1 Cl2
CELL 1.54184 20.914799 17.523805 4.214875 90 90 90
ZERR 4 0.000866 0.000631 0.00017 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,0.5-Z
SFAC C H Cl N O S
UNIT 40 44 8 28 12 4
EADP S1B S1
SADI S1 C5B S1 C5
SADI C5B S1B C5 S1B
EADP C5B C5
SADI S1 C5 S1B C5B

L.S. 4
PLAN  3
TEMP -173
CONF
HTAB N1 O2B
HTAB N1 O2
BOND
MORE -1
BOND $H
fmap 2
ACTA
REM <olex2.extras>
REM <HklSrc "%.\\JS124B.hkl">
REM </olex2.extras>

WGHT    0.053800    1.044200
FVAR       1.87058   0.24665
CL1   3    0.324181    0.533073    0.660995    11.00000    0.02816    0.02923 =
         0.04699    0.00358   -0.00365    0.00548
O1    5    0.392902    0.407605    1.084679    11.00000    0.02690    0.01851 =
         0.03422    0.00107    0.00635    0.00361
N1    4    0.597590    0.250000    0.530114    10.50000    0.02412    0.01896 =
         0.03453    0.00000    0.00704    0.00000
H1    2    0.634455    0.250000    0.408409    10.50000    0.05266
N2    4    0.568259    0.314041    0.609602    11.00000    0.02435    0.01812 =
         0.03120    0.00051    0.00366    0.00062
N4    4    0.423917    0.335985    1.066869    11.00000    0.02713    0.01683 =
         0.03709    0.00087    0.00507    0.00420
N5    4    0.471592    0.421641    0.740855    11.00000    0.02574    0.01785 =
         0.03037    0.00063    0.00158    0.00178
C1    1    0.514696    0.290196    0.755377    11.00000    0.01866    0.01910 =
         0.02384   -0.00021   -0.00024    0.00044
C2    1    0.468957    0.348007    0.861349    11.00000    0.02045    0.01713 =
         0.02536   -0.00104   -0.00245   -0.00013
C3    1    0.424426    0.453642    0.883802    11.00000    0.02070    0.01907 =
         0.02635    0.00093   -0.00198   -0.00105
C4    1    0.401064    0.533694    0.848395    11.00000    0.02634    0.02012 =
         0.03155   -0.00041    0.00053    0.00223
AFIX  23
H4A   2    0.431622    0.563434    0.718434    11.00000   -1.20000
H4B   2    0.397882    0.558137    1.059566    11.00000   -1.20000
AFIX   0

PART 2
S1    6    0.731691    0.250000   -0.039519   -20.50000    0.02592    0.02943 =
         0.03225    0.00000   -0.00350    0.00000
O2B   5    0.716060    0.250000    0.310195   -20.50000    0.02609    0.04087 =
         0.04246    0.00000    0.01548    0.00000
C5    1    0.780932    0.169822   -0.093372   -21.00000    0.07347    0.06736 =
         0.04968    0.02639    0.03453    0.04360
AFIX 137
H5A   2    0.820036    0.175842    0.032254   -21.00000   -1.50000
H5B   2    0.792084    0.165011   -0.318312   -21.00000   -1.50000
H5C   2    0.758143    0.123886   -0.024098   -21.00000   -1.50000
AFIX   0

PART 1
S1B   6    0.759325    0.250000    0.149525    20.50000    0.02592    0.02943 =
         0.03225    0.00000   -0.00350    0.00000
O2    5    0.687101    0.250000    0.100157    20.50000    0.01872    0.04627 =
         0.02060    0.00000    0.00755    0.00000
C5B   1    0.799816    0.185467   -0.088560    21.00000    0.07347    0.06736 =
         0.04968    0.02639    0.03453    0.04360
AFIX 137
H5BA  2    0.782583    0.187607   -0.304591    21.00000   -1.50000
H5BB  2    0.794379    0.133845   -0.003304    21.00000   -1.50000
H5BC  2    0.845385    0.198455   -0.092428    21.00000   -1.50000
AFIX   0
HKLF 4




REM  js124b_a.res in Pnma
REM wR2 = 0.1214, GooF = S = 1.033, Restrained GooF = 1.033 for all data
REM R1 = 0.0447 for 1312 Fo > 4sig(Fo) and 0.0614 for all 1674 data
REM 126 parameters refined using 1 restraints

END

WGHT      0.0538      1.0438

REM Highest difference peak  0.647,  deepest hole -0.487,  1-sigma level  0.079
Q1    1   0.7617  0.2207  0.1496  11.00000  0.05    0.65
Q2    1   0.5080  0.2500  0.7912  10.50000  0.05    0.35
Q3    1   0.3786  0.5418  0.6982  11.00000  0.05    0.34
;
_shelx_res_checksum              34674
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a nylon loop with paratone oil'
_olex2_submission_original_sample_id JMS-SOHAN-163
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.254
_oxdiff_exptl_absorpt_empirical_full_min 0.797
