# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2021

####################################################################### 
# 
# 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_m135
_database_code_depnum_ccdc_archive 'CCDC 2044963'
loop_
_audit_author_name
_audit_author_address
'Vitalii Suslonov'
;Saint Petersburg State University
Russia
;
_audit_update_record             
;
2020-11-17 deposited with the CCDC.	2021-03-23 downloaded from the CCDC.
;
_audit_creation_date             2019-05-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C6 F3 I3), C10 H20 Cu N2 S4'
_chemical_formula_sum            'C22 H20 Cu F6 I6 N2 S4'
_chemical_formula_weight         1379.58
_chemical_melting_point          ?
_chemical_oxdiff_formula         C16H20CuF3I3N2S4
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'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 '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'
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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.6789(3)
_cell_length_b                   9.4436(3)
_cell_length_c                   12.4868(2)
_cell_angle_alpha                107.682(2)
_cell_angle_beta                 90.978(2)
_cell_angle_gamma                114.817(3)
_cell_volume                     872.57(5)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    8196
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.1970
_cell_measurement_theta_min      3.7590
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    45.254
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.10727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.50a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    2.625
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             631
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14534
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.480
_diffrn_reflns_theta_max         67.480
_diffrn_reflns_theta_min         3.768
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -16.00  20.00   0.50    0.30    --   38.95 -98.00   7.00   72
  2  ω     27.00  67.00   0.50    0.30    --   38.95 -98.00   7.00   80
  3  ω     44.00  69.00   0.50    1.19    --  100.00 -98.00   7.00   50
  4  ω     81.00 152.00   0.50    1.19    --  100.00  98.00 115.00  142
  5  ω     -5.00  20.00   0.50    0.30    --  -38.95  98.00 115.00   50
  6  ω    -73.00  -9.00   0.50    0.30    --  -38.95  98.00 115.00  128
  7  ω    -44.00 -13.00   0.50    0.30    --  -38.95 138.00 150.00   62
  8  ω    -85.00 -59.00   0.50    0.30    --  -38.95 -77.00   0.00   52
  9  ω    -41.00 -11.00   0.50    0.30    --  -38.95  43.00 120.00   60
 10  ω    -44.00 -12.00   0.50    0.30    --  -38.95 -77.00   0.00   64
 11  ω     -8.00  18.00   0.50    0.30    --  -38.95  43.00 120.00   52
 12  ω    -96.00 -49.00   0.50    0.30    --  -38.95 138.00 150.00   94
 13  ω     28.00  54.00   0.50    0.30    --   38.95-104.00-180.00   52
 14  ω     32.00  73.00   0.50    0.30    --   38.95  32.00 -30.00   82
 15  ω     41.00 104.00   0.50    0.30    --   38.95  43.00-120.00  126
 16  ω     43.00  69.00   0.50    0.30    --   38.95  32.00  90.00   52
 17  ω      4.00  45.00   0.50    0.30    --   38.95  11.00 120.00   82
 18  ω    -21.00  29.00   0.50    0.30    --   38.95 -43.00-120.00  100
 19  ω     34.00  59.00   0.50    0.30    --   38.95 -54.00  30.00   50
 20  ω    -14.00  16.00   0.50    0.30    --   38.95-104.00-180.00   60
 21  ω     90.00 115.00   0.50    0.30    --   38.95  11.00 120.00   50
 22  ω     46.00  91.00   0.50    0.30    --   38.95-138.00 -30.00   90
 23  ω    -12.00  30.00   0.50    0.30    --   38.95 -77.00-180.00   84
 24  ω     19.00  95.00   0.50    0.30    --   38.95  54.00   0.00  152
 25  ω     72.00 100.00   0.50    0.30    --   38.95  32.00  90.00   56
 26  ω     83.00 108.00   0.50    0.30    --   38.95  32.00 -30.00   50
 27  ω     84.00 124.00   0.50    1.19    --  100.00 111.00  90.00   80
 28  ω     43.00 129.00   0.50    1.19    --  100.00 -89.00  33.28  172
 29  ω     86.00 157.00   0.50    1.19    --  100.00  93.00 150.00  142
 30  ω     76.00 103.00   0.50    1.19    --  100.00-111.00 120.00   54
 31  ω     32.00 105.00   0.50    1.19    --  100.00-111.00  30.00  146
 32  ω     82.00 107.00   0.50    1.19    --  100.00  45.00  60.00   50
 33  ω    122.00 155.00   0.50    1.19    --  100.00  45.00  60.00   66
 34  ω     44.00  73.00   0.50    1.19    --  100.00 -93.00 -30.00   58
 35  ω     78.00 120.00   0.50    1.19    --  100.00 -86.00 -60.00   84
 36  ω     37.00 108.00   0.50    1.19    --  100.00 -30.00-150.00  142
 37  ω     88.00 141.00   0.50    1.19    --  100.00  30.00 120.00  106
 38  ω     96.00 121.00   0.50    1.19    --  100.00-133.00-120.00   50
 39  ω     98.00 146.00   0.50    1.19    --  100.00 133.00  60.00   96
 40  ω     96.00 144.00   0.50    1.19    --  100.00  77.00-180.00   96
 41  ω    107.00 141.00   0.50    1.19    --  100.00 111.00 -30.00   68
 42  ω     59.00  98.00   0.50    1.19    --  100.00-133.00 -30.00   78
 43  ω     34.00 112.00   0.50    1.19    --  100.00 -30.00   0.00  156
 44  ω    120.00 153.00   0.50    1.19    --  100.00 111.00-180.00   66
 45  ω     81.00 117.00   0.50    1.19    --  100.00 111.00-180.00   72
 46  ω     87.00 146.00   0.50    1.19    --  100.00 111.00 -60.00  118
 47  ω     46.00 115.00   0.50    1.19    --  100.00 -53.00  30.00  138
 48  ω     60.00 109.00   0.50    1.19    --  100.00-133.00 -60.00   98
 49  ω     91.00 123.00   0.50    1.19    --  100.00 -77.00 150.00   64
 50  ω     89.00 144.00   0.50    1.19    --  100.00  30.00 -90.00  110
 51  ω     70.00 124.00   0.50    1.19    --  100.00 -77.00 120.00  108
 52  ω     71.00 115.00   0.50    1.19    --  100.00  15.00 -90.00   88
 53  ω     55.00 122.00   0.50    1.19    --  100.00-133.00   0.00  134
 54  ω    132.00 157.00   0.50    1.19    --  100.00  61.00 -30.00   50
 55  ω     97.00 122.00   0.50    1.19    --  100.00-133.00 150.00   50
 56  ω     64.00  90.00   0.50    1.19    --  100.00-133.00 150.00   52
 57  ω    128.00 153.00   0.50    1.19    --  100.00 111.00  90.00   50
 58  ω     45.00 108.00   0.50    1.19    --  100.00 -45.00 150.00  126
 59  ω     91.00 117.00   0.50    1.19    --  100.00 -53.00  90.00   52
 60  ω     69.00  94.00   0.50    1.19    --  100.00 -61.00   0.00   50
 61  ω     40.00  82.00   0.50    1.19    --  100.00 -77.00 150.00   84
 62  ω     35.00  60.00   0.50    0.30    --   38.95  77.00-180.00   50
 63  ω    -40.00 -15.00   0.50    0.30    --   12.00 128.00 147.49   50
 64  ω    -27.00  -2.00   0.50    0.30    --   16.00 113.00  61.93   50
 65  ω    -20.00   5.00   0.50    0.30    --   24.00 114.00 -29.50   50
 66  ω     -8.00  17.00   0.50    0.30    --   28.00 100.00-110.45   50
 67  ω     -1.00  24.00   0.50    0.30    --   32.00  94.00 165.42   50
 68  ω      0.00  25.00   0.50    0.30    --   32.00  91.00 143.81   50
 69  ω      4.00  29.00   0.50    0.30    --   36.00  90.00 -77.20   50
 70  ω      5.00  30.00   0.50    0.30    --   36.00  88.00 -29.16   50
 71  ω      5.00  30.00   0.50    0.30    --   36.00  88.00  90.55   50
 72  ω      4.00  29.00   0.50    0.30    --   36.00  90.00  65.71   50
 73  ω    -55.00 -11.00   0.50    0.30    --  -38.95  43.00  30.00   88
 74  ω     17.00  42.00   0.50    0.30    --   44.00  79.00  30.68   50
 75  ω     16.00  41.00   0.50    0.30    --   44.00  82.00 154.51   50
 76  ω     16.00  41.00   0.50    0.30    --   44.00  81.00  -8.50   50
 77  ω     17.00  42.00   0.50    0.30    --   44.00  79.00 129.08   50
 78  ω     16.00  41.00   0.50    0.30    --   44.00  81.00-146.92   50
 79  ω     16.00  41.00   0.50    0.30    --   44.00  82.00  91.37   50
 80  ω     17.00  42.00   0.50    0.30    --   44.00  79.00 -39.89   50
 81  ω     17.00  42.00   0.50    0.30    --   44.00  80.00-175.05   50
 82  ω     82.00 111.00   0.50    0.30    --   48.00  76.00-117.38   58
 83  ω     23.00  49.00   0.50    0.30    --   48.00  76.00-117.38   52
 84  ω     97.00 123.00   0.50    0.30    --   56.00  76.00  41.78   52
 85  ω     31.00  57.00   0.50    0.30    --   56.00  77.00 -96.64   52
 86  ω     34.00  60.00   0.50    0.30    --   56.00  76.00  41.78   52
 87  ω     34.00  60.00   0.50    0.30    --   60.00  77.00   8.05   52
 88  ω     98.00 123.00   0.50    0.30    --   60.00  77.00  99.62   50
 89  ω     33.00  59.00   0.50    0.30    --   60.00  77.00  99.62   52
 90  ω     34.00  65.00   0.50    0.30    --   60.00  74.00-162.35   62
 91  ω     38.00  65.00   0.50    0.30    --   64.00  76.00 109.82   54
 92  ω     46.00  72.00   0.50    0.30    --   64.00  75.00 -58.49   52
 93  ω     91.00 116.00   0.50    0.30    --   64.00  76.00 -20.95   50
 94  ω     38.00  68.00   0.50    0.30    --   64.00  76.00 -20.95   60
 95  ω     43.00  80.00   0.50    0.30    --   64.00  69.00  62.71   74
 96  ω     84.00 109.00   0.50    0.30    --   68.00  77.00 -81.20   50
 97  ω     41.00  66.00   0.50    0.30    --   68.00  77.00 -81.20   50
 98  ω     46.00  92.00   0.50    1.19    --   72.00  76.00 170.57   92
 99  ω     96.00 137.00   0.50    1.19    --   72.00  76.00 170.57   82
100  ω     54.00  80.00   0.50    1.19    --   72.00  59.00  26.14   52
101  ω     46.00  86.00   0.50    1.19    --   72.00  74.00 142.24   80
102  ω     53.00  79.00   0.50    1.19    --   76.00  66.00-130.42   52
103  ω     58.00  84.00   0.50    1.19    --   76.00  52.00 -27.08   52
104  ω     59.00  85.00   0.50    1.19    --   80.00  56.00-146.87   52
105  ω     73.00 109.00   0.50    1.19    --  100.00  77.00 150.00   72
106  ω     73.00  98.00   0.50    1.19    --  100.00  77.00-120.00   50
107  ω     79.00 117.00   0.50    1.19    --  100.00  61.00  90.00   76
108  ω     73.00 104.00   0.50    1.19    --  100.00  77.00  90.00   62
109  ω     73.00 118.00   0.50    1.19    --  100.00  77.00 -90.00   90
110  ω     76.00 157.00   0.50    1.19    --  100.00  69.00 -60.00  162
111  ω    123.00 155.00   0.50    1.19    --  100.00  61.00 -90.00   64
112  ω     77.00 103.00   0.50    1.19    --  100.00  77.00-150.00   52
113  ω    107.00 133.00   0.50    1.19    --  100.00  69.00-120.00   52
114  ω     76.00 104.00   0.50    1.19    --  100.00  69.00-120.00   56
115  ω     79.00 117.00   0.50    1.19    --  100.00  61.00 -90.00   76
116  ω    132.00 157.00   0.50    1.19    --  100.00  77.00-150.00   50
117  ω     73.00  99.00   0.50    1.19    --  100.00  77.00 -30.00   52
118  ω    125.00 156.00   0.50    1.19    --  100.00  77.00 -90.00   62
119  ω    132.00 157.00   0.50    1.19    --  100.00  61.00  60.00   50
120  ω     78.00 117.00   0.50    1.19    --  100.00  61.00  60.00   78
121  ω    120.00 157.00   0.50    1.19    --  100.00  69.00 -30.00   74
122  ω    131.00 157.00   0.50    1.19    --  100.00  77.00-180.00   52
123  ω     89.00 114.00   0.50    1.19    --  100.00 -30.00 120.00   50
124  ω     76.00 114.00   0.50    1.19    --  100.00  77.00 -60.00   76
125  ω     74.00 100.00   0.50    1.19    --  100.00  77.00-180.00   52
126  ω    113.00 140.00   0.50    1.19    --  100.00  69.00 150.00   54
127  ω     76.00 101.00   0.50    1.19    --  100.00  69.00 150.00   50
128  ω     76.00 102.00   0.50    1.19    --  100.00  69.00 -30.00   52
129  ω    113.00 148.00   0.50    1.19    --  100.00 111.00 -90.00   70
130  ω     78.00 147.00   0.50    1.19    --  100.00  61.00  30.00  138
131  ω    110.00 152.00   0.50    1.19    --  100.00  77.00   0.00   84
132  ω    132.00 157.00   0.50    1.19    --  100.00  77.00  60.00   50
133  ω     79.00 123.00   0.50    1.19    --  100.00  61.00   0.00   88
134  ω    117.00 157.00   0.50    1.19    --  100.00  61.00-120.00   80
135  ω     73.00  98.00   0.50    1.19    --  100.00  77.00 120.00   50
136  ω     78.00 104.00   0.50    1.19    --  100.00  61.00-120.00   52
137  ω    116.00 153.00   0.50    1.19    --  100.00 111.00 150.00   74
138  ω     73.00  99.00   0.50    1.19    --  100.00  77.00   0.00   52
139  ω    132.00 157.00   0.50    1.19    --  100.00  61.00-150.00   50
140  ω    126.00 151.00   0.50    1.19    --  100.00  77.00  30.00   50
141  ω     74.00 100.00   0.50    1.19    --  100.00  77.00  30.00   52
142  ω     82.00 108.00   0.50    1.19    --  100.00  61.00-150.00   52
143  ω     73.00  99.00   0.50    1.19    --  100.00  77.00  60.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1094365000
_diffrn_orient_matrix_UB_12      0.1207332000
_diffrn_orient_matrix_UB_13      -0.0591242000
_diffrn_orient_matrix_UB_21      -0.1373740000
_diffrn_orient_matrix_UB_22      -0.1003762000
_diffrn_orient_matrix_UB_23      -0.1085681000
_diffrn_orient_matrix_UB_31      -0.0921846000
_diffrn_orient_matrix_UB_32      0.1092994000
_diffrn_orient_matrix_UB_33      0.0443601000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2919
_reflns_number_total             3146
_reflns_odcompleteness_completeness 95.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     72.42
_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 1.171.40.50a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.50a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.50a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.412
_refine_diff_density_min         -0.997
_refine_diff_density_rms         0.196
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         3146
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0346
_refine_ls_restrained_S_all      1.032
_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)+(0.0647P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0899
_refine_special_details          ?
_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.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C5(H5A,H5B,H5C)
;
_atom_sites_solution_hydrogens   geom
_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
I2S I 0.27867(4) 0.24944(4) 0.72616(2) 0.02271(12) Uani 1 1 d . . . . .
I1S I 0.17095(4) -0.29597(4) 0.28055(3) 0.02566(12) Uani 1 1 d . . . . .
I3S I 0.75523(4) 0.39400(5) 0.38679(3) 0.03095(13) Uani 1 1 d . . . . .
Cu1 Cu 1.0000 0.5000 1.0000 0.0198(2) Uani 1 2 d S T P . .
S1 S 1.06409(16) 0.69338(16) 0.91092(10) 0.0218(3) Uani 1 1 d . . . . .
S2 S 0.76023(16) 0.54995(16) 1.00685(10) 0.0216(3) Uani 1 1 d . . . . .
F1S F 0.1229(4) -0.0993(4) 0.5229(3) 0.0274(7) Uani 1 1 d . . . . .
F2S F 0.5686(4) 0.4365(4) 0.6013(3) 0.0268(7) Uani 1 1 d . . . . .
F3S F 0.4978(4) 0.0125(4) 0.2603(3) 0.0330(7) Uani 1 1 d . . . . .
N1 N 0.7950(5) 0.7629(5) 0.8960(4) 0.0217(9) Uani 1 1 d . . . . .
C3S C 0.3446(6) 0.1687(7) 0.5666(4) 0.0210(10) Uani 1 1 d . . . . .
C1S C 0.3065(7) -0.0486(6) 0.3891(4) 0.0230(10) Uani 1 1 d . . . . .
C4S C 0.4844(7) 0.2773(7) 0.5321(4) 0.0238(11) Uani 1 1 d . . . . .
C5S C 0.5417(7) 0.2286(7) 0.4309(5) 0.0247(11) Uani 1 1 d . . . . .
C1 C 0.8632(6) 0.6810(6) 0.9335(4) 0.0194(10) Uani 1 1 d . . . . .
C2S C 0.2598(7) 0.0084(7) 0.4927(4) 0.0234(11) Uani 1 1 d . . . . .
C2 C 0.8939(7) 0.8832(7) 0.8399(5) 0.0253(11) Uani 1 1 d . . . . .
H2A H 1.0154 0.9331 0.8706 0.030 Uiso 1 1 calc R . . . .
H2B H 0.8582 0.9711 0.8569 0.030 Uiso 1 1 calc R . . . .
C6S C 0.4482(7) 0.0639(7) 0.3608(4) 0.0248(11) Uani 1 1 d . . . . .
C3 C 0.8677(7) 0.8019(7) 0.7119(5) 0.0287(12) Uani 1 1 d . . . . .
H3A H 0.9306 0.8843 0.6788 0.043 Uiso 1 1 calc GR . . . .
H3B H 0.7474 0.7511 0.6812 0.043 Uiso 1 1 calc GR . . . .
H3C H 0.9085 0.7187 0.6946 0.043 Uiso 1 1 calc GR . . . .
C4 C 0.6134(7) 0.7284(7) 0.8985(5) 0.0255(11) Uani 1 1 d . . . . .
H4A H 0.5500 0.6186 0.9033 0.031 Uiso 1 1 calc R . . . .
H4B H 0.5650 0.7278 0.8277 0.031 Uiso 1 1 calc R . . . .
C5 C 0.5896(8) 0.8536(7) 0.9972(6) 0.0338(13) Uani 1 1 d . . . . .
H5A H 0.6482 0.9620 0.9914 0.051 Uiso 1 1 calc GR . . . .
H5B H 0.6365 0.8543 1.0677 0.051 Uiso 1 1 calc GR . . . .
H5C H 0.4691 0.8239 0.9953 0.051 Uiso 1 1 calc GR . . . .


_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
I2S C3S 2.088(5) . ?
I1S C1S 2.096(5) . ?
I3S C5S 2.074(5) . ?
Cu1 S1 2.2988(12) . ?
Cu1 S1 2.2988(12) 2_767 ?
Cu1 S2 2.3164(13) 2_767 ?
Cu1 S2 2.3164(13) . ?
S1 C1 1.732(5) . ?
S2 C1 1.720(5) . ?
F1S C2S 1.351(6) . ?
F2S C4S 1.345(6) . ?
F3S C6S 1.348(6) . ?
N1 C1 1.328(7) . ?
N1 C2 1.485(6) . ?
N1 C4 1.472(7) . ?
C3S C4S 1.397(7) . ?
C3S C2S 1.371(8) . ?
C1S C2S 1.380(7) . ?
C1S C6S 1.383(8) . ?
C4S C5S 1.385(8) . ?
C5S C6S 1.390(8) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.513(8) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.513(9) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?

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
S1 Cu1 S1 180.0 . 2_767 ?
S1 Cu1 S2 102.64(4) . 2_767 ?
S1 Cu1 S2 77.36(4) 2_767 2_767 ?
S1 Cu1 S2 102.64(4) 2_767 . ?
S1 Cu1 S2 77.36(4) . . ?
S2 Cu1 S2 180.0 2_767 . ?
C1 S1 Cu1 84.74(16) . . ?
C1 S2 Cu1 84.46(18) . . ?
C1 N1 C2 121.4(4) . . ?
C1 N1 C4 121.8(4) . . ?
C4 N1 C2 116.5(4) . . ?
C4S C3S I2S 120.5(4) . . ?
C2S C3S I2S 122.9(4) . . ?
C2S C3S C4S 116.5(5) . . ?
C2S C1S I1S 121.4(4) . . ?
C2S C1S C6S 117.1(5) . . ?
C6S C1S I1S 121.4(4) . . ?
F2S C4S C3S 118.3(5) . . ?
F2S C4S C5S 118.4(5) . . ?
C5S C4S C3S 123.3(5) . . ?
C4S C5S I3S 121.5(4) . . ?
C4S C5S C6S 116.4(5) . . ?
C6S C5S I3S 122.1(4) . . ?
S2 C1 S1 113.4(3) . . ?
N1 C1 S1 123.0(4) . . ?
N1 C1 S2 123.6(4) . . ?
F1S C2S C3S 118.0(4) . . ?
F1S C2S C1S 118.3(5) . . ?
C3S C2S C1S 123.6(5) . . ?
N1 C2 H2A 109.2 . . ?
N1 C2 H2B 109.2 . . ?
N1 C2 C3 112.1(4) . . ?
H2A C2 H2B 107.9 . . ?
C3 C2 H2A 109.2 . . ?
C3 C2 H2B 109.2 . . ?
F3S C6S C1S 118.8(5) . . ?
F3S C6S C5S 118.2(5) . . ?
C1S C6S C5S 123.0(5) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 H4A 108.9 . . ?
N1 C4 H4B 108.9 . . ?
N1 C4 C5 113.2(5) . . ?
H4A C4 H4B 107.8 . . ?
C5 C4 H4A 108.9 . . ?
C5 C4 H4B 108.9 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?

# start Validation Reply Form
_vrf_PLAT431_m135                
;
PROBLEM: Short Inter HL..A Contact  I1S      ..S1       .       3.45 Ang.  
RESPONSE: Short contact is the investigated feature of this structure.
;
# end Validation Reply Form

_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 5.309
_oxdiff_exptl_absorpt_empirical_full_min 0.462
####################################################################### 
# 
# 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_eaa-162
_database_code_depnum_ccdc_archive 'CCDC 2044965'
loop_
_audit_author_name
_audit_author_address
'Vitalii Suslonov'
;Saint Petersburg State University
Russia
;
_audit_update_record             
;
2020-11-17 deposited with the CCDC.	2021-03-23 downloaded from the CCDC.
;
_audit_creation_date             2019-09-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C10 H20 N2 Pt S4, 2(C6 F3 I3)'
_chemical_formula_sum            'C22 H20 F6 I6 N2 Pt S4'
_chemical_formula_weight         1511.13
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C16 H20 N2 S4 Pt1 F3 I3'
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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 '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'
Pt Pt -4.5932 6.9264 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.6611(2)
_cell_length_b                   9.6024(2)
_cell_length_c                   12.1690(2)
_cell_angle_alpha                107.288(2)
_cell_angle_beta                 89.909(2)
_cell_angle_gamma                113.544(2)
_cell_volume                     877.93(3)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    4715
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.3920
_cell_measurement_theta_min      3.8560
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    51.576
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.35a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.858
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.438
_diffrn_reflns_theta_min         3.839
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     18.00  65.00   0.50    0.20    --   38.82  58.00-151.00   94
  2  ω     21.00  47.00   0.50    0.20    --   38.82 -58.00  67.00   52
  3  ω     81.00 107.00   0.50    0.29    --  100.00 -58.00  67.00   52
  4  ω    111.00 144.00   0.50    0.29    --  100.00  58.00-151.00   66
  5  ω     79.00 106.00   0.50    0.29    --  100.00  58.00-151.00   54
  6  ω     37.00  74.00   0.50    0.29    --  100.00 -58.00  67.00   74
  7  ω   -104.00 -48.00   0.50    0.20    --  -38.82 -58.00  67.00  112
  8  ω    -95.00 -58.00   0.50    0.20    --  -38.82 138.00 -60.00   74
  9  ω    -55.00  21.00   0.50    0.20    --  -38.82  54.00 120.00  152
 10  ω    -53.00 -28.00   0.50    0.20    --  -38.82  58.00-151.00   50
 11  ω    -69.00 -16.00   0.50    0.20    --  -38.82 -65.00-180.00  106
 12  ω    -55.00 -13.00   0.50    0.20    --  -38.82 138.00 -60.00   84
 13  ω   -103.00 -78.00   0.50    0.20    --  -38.82 -65.00-180.00   50
 14  ω    -21.00  32.00   0.50    0.20    --  -38.82  21.00 -60.00  106
 15  ω    -53.00 -27.00   0.50    0.20    --  -38.82  21.00 -60.00   52
 16  ω      1.00  26.00   0.50    0.20    --  -38.82  58.00-151.00   50
 17  ω    -26.00   5.00   0.50    0.20    --  -38.82  77.00-120.00   62
 18  ω   -101.00 -53.00   0.50    0.20    --  -38.82 -54.00 -60.00   96
 19  ω    -63.00 -37.00   0.50    0.20    --  -38.82  77.00-120.00   52
 20  ω    -47.00 -20.00   0.50    0.20    --  -38.82 -54.00 -60.00   54
 21  ω     73.00 105.00   0.50    0.20    --   38.82  43.00-180.00   64
 22  ω     42.00  70.00   0.50    0.20    --   38.82 -89.00  60.00   56
 23  ω      9.00  68.00   0.50    0.20    --   38.82-104.00 -90.00  118
 24  ω     38.00  66.00   0.50    0.20    --   38.82  43.00-180.00   56
 25  ω      3.00  28.00   0.50    0.20    --   38.82 -89.00  60.00   50
 26  ω     80.00 105.00   0.50    0.20    --   38.82  43.00 -30.00   50
 27  ω     31.00  64.00   0.50    0.20    --   38.82  43.00 -30.00   66
 28  ω     26.00  56.00   0.50    0.20    --   38.82  43.00   0.00   60
 29  ω    -31.00  -3.00   0.50    0.20    --   38.82 -89.00  60.00   56
 30  ω     31.00  84.00   0.50    0.29    --  100.00 -30.00  60.00  106
 31  ω     86.00 111.00   0.50    0.29    --  100.00-111.00 -60.00   50
 32  ω     87.00 150.00   0.50    0.29    --  100.00  22.00 120.00  126
 33  ω    125.00 151.00   0.50    0.29    --  100.00  15.00 -30.00   52
 34  ω     49.00 104.00   0.50    0.29    --  100.00 -93.00  60.00  110
 35  ω     84.00 115.00   0.50    0.29    --  100.00 -22.00 -60.00   62
 36  ω     36.00  78.00   0.50    0.29    --  100.00 178.00 -90.00   84
 37  ω     29.00  77.00   0.50    0.29    --  100.00 -22.00 -60.00   96
 38  ω    109.00 135.00   0.50    0.29    --  100.00  37.00 -90.00   52
 39  ω     65.00 111.00   0.50    0.29    --  100.00-111.00-120.00   92
 40  ω     32.00 103.00   0.50    0.29    --  100.00 -30.00-120.00  142
 41  ω     93.00 119.00   0.50    0.29    --  100.00  15.00 -30.00   52
 42  ω    121.00 151.00   0.50    0.29    --  100.00  37.00-120.00   60
 43  ω     57.00 120.00   0.50    0.29    --  100.00 -86.00 -90.00  126
 44  ω     91.00 116.00   0.50    0.29    --  100.00  37.00-180.00   50
 45  ω     91.00 117.00   0.50    0.29    --  100.00 -61.00 -90.00   52
 46  ω     39.00  65.00   0.50    0.29    --  100.00 -61.00 -90.00   52
 47  ω     38.00  63.00   0.50    0.29    --  100.00 -69.00 120.00   50
 48  ω     60.00  96.00   0.50    0.29    --  100.00-111.00-150.00   72
 49  ω     78.00 137.00   0.50    0.29    --  100.00  61.00-120.00  118
 50  ω     90.00 115.00   0.50    0.29    --  100.00  37.00-120.00   50
 51  ω     85.00 118.00   0.50    0.29    --  100.00 -61.00-120.00   66
 52  ω     95.00 121.00   0.50    0.29    --  100.00-133.00-180.00   52
 53  ω     39.00 118.00   0.50    0.29    --  100.00 -45.00 -30.00  158
 54  ω     88.00 118.00   0.50    0.29    --  100.00  15.00   0.00   60
 55  ω     36.00 116.00   0.50    0.29    --  100.00 -53.00 150.00  160
 56  ω     77.00 120.00   0.50    0.29    --  100.00-133.00  90.00   86
 57  ω     85.00 157.00   0.50    0.29    --  100.00  37.00 -60.00  144
 58  ω    120.00 145.00   0.50    0.29    --  100.00 178.00 -90.00   50
 59  ω    101.00 156.00   0.50    0.29    --  100.00 111.00 -60.00  110
 60  ω     56.00 104.00   0.50    0.29    --  100.00-111.00 -90.00   96
 61  ω     88.00 153.00   0.50    0.29    --  100.00  53.00-180.00  130
 62  ω     36.00  70.00   0.50    0.29    --  100.00-133.00  90.00   68
 63  ω     41.00 100.00   0.50    0.29    --  100.00 -69.00  60.00  118
 64  ω     35.00  62.00   0.50    0.29    --  100.00 -61.00-120.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0354416000
_diffrn_orient_matrix_UB_12      -0.0978936000
_diffrn_orient_matrix_UB_13      -0.0686317000
_diffrn_orient_matrix_UB_21      -0.1570815000
_diffrn_orient_matrix_UB_22      0.0072900000
_diffrn_orient_matrix_UB_23      0.0617989000
_diffrn_orient_matrix_UB_31      -0.1113569000
_diffrn_orient_matrix_UB_32      0.1567425000
_diffrn_orient_matrix_UB_33      -0.0968009000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3052
_reflns_number_total             3352
_reflns_odcompleteness_completeness 96.49
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     72.42
_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 1.171.39.35a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.704
_refine_diff_density_min         -1.865
_refine_diff_density_rms         0.264
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         3352
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0348
_refine_ls_restrained_S_all      1.011
_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)+(0.0461P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.0871
_refine_special_details          ?
_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. Uiso/Uaniso restraints and constraints
Uanis(C2) = Uanis(C4)
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B)
3.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C5(H5A,H5B,H5C)
;
_atom_sites_solution_hydrogens   geom
_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
Pt1 Pt 0.0000 0.5000 0.0000 0.00724(11) Uani 1 2 d S T P . .
I2S I 0.71400(5) 0.75281(5) 0.26512(3) 0.01438(12) Uani 1 1 d . . . . .
I3S I 0.22353(5) 0.56896(5) 0.60225(4) 0.01915(12) Uani 1 1 d . . . . .
I1S I 0.79078(6) 1.23205(5) 0.74426(4) 0.01970(13) Uani 1 1 d . . . . .
S1 S -0.06597(19) 0.29928(19) 0.08509(13) 0.0112(3) Uani 1 1 d . . . . .
S2 S 0.24443(18) 0.45538(18) 0.00611(13) 0.0101(3) Uani 1 1 d . . . . .
F2S F 0.4124(5) 0.5568(4) 0.3785(3) 0.0145(8) Uani 1 1 d . . . . .
F3S F 0.4597(5) 0.9304(5) 0.7422(3) 0.0206(9) Uani 1 1 d . . . . .
F1S F 0.8495(5) 1.0780(5) 0.4834(3) 0.0189(8) Uani 1 1 d . . . . .
N1 N 0.2059(6) 0.2367(6) 0.1140(5) 0.0094(10) Uani 1 1 d . . . . .
C1S C 0.6577(9) 1.0104(8) 0.6152(6) 0.0140(13) Uani 1 1 d . . . . .
C6S C 0.5165(8) 0.8942(8) 0.6382(5) 0.0131(13) Uani 1 1 d . . . . .
C3S C 0.6325(8) 0.8180(8) 0.4263(6) 0.0134(13) Uani 1 1 d . . . . .
C5S C 0.4306(8) 0.7400(8) 0.5598(6) 0.0158(14) Uani 1 1 d . . . . .
C3 C 0.1151(9) 0.1909(9) 0.2985(6) 0.0188(14) Uani 1 1 d . . . . .
H3A H 0.0578 0.2607 0.3136 0.028 Uiso 1 1 calc GR . . . .
H3B H 0.2321 0.2515 0.3321 0.028 Uiso 1 1 calc GR . . . .
H3C H 0.0620 0.1075 0.3322 0.028 Uiso 1 1 calc GR . . . .
C4S C 0.4935(9) 0.7060(9) 0.4567(5) 0.0151(13) Uani 1 1 d . . . . .
C2S C 0.7112(9) 0.9673(8) 0.5079(6) 0.0175(14) Uani 1 1 d . . . . .
C2 C 0.1047(8) 0.1171(8) 0.1692(6) 0.0134(9) Uani 1 1 d . . . . .
H2A H 0.1454 0.0335 0.1543 0.016 Uiso 1 1 calc R . . . .
H2B H -0.0131 0.0676 0.1345 0.016 Uiso 1 1 calc R . . . .
C5 C 0.4248(9) 0.1540(9) 0.0203(7) 0.0212(15) Uani 1 1 d . . . . .
H5A H 0.3911 0.1579 -0.0535 0.032 Uiso 1 1 calc GR . . . .
H5B H 0.3619 0.0481 0.0246 0.032 Uiso 1 1 calc GR . . . .
H5C H 0.5442 0.1795 0.0285 0.032 Uiso 1 1 calc GR . . . .
C4 C 0.3891(8) 0.2745(8) 0.1168(6) 0.0134(9) Uani 1 1 d . . . . .
H4A H 0.4322 0.2765 0.1911 0.016 Uiso 1 1 calc R . . . .
H4B H 0.4491 0.3806 0.1101 0.016 Uiso 1 1 calc R . . . .
C1 C 0.1382(8) 0.3161(7) 0.0752(5) 0.0099(12) Uani 1 1 d . . . . .


_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
Pt1 S1 2.3276(14) . ?
Pt1 S1 2.3277(14) 2_565 ?
Pt1 S2 2.3270(15) . ?
Pt1 S2 2.3270(15) 2_565 ?
I2S C3S 2.087(7) . ?
I3S C5S 2.081(7) . ?
I1S C1S 2.094(7) . ?
S1 C1 1.718(6) . ?
S2 C1 1.739(6) . ?
F2S C4S 1.356(8) . ?
F3S C6S 1.355(7) . ?
F1S C2S 1.351(8) . ?
N1 C2 1.481(8) . ?
N1 C4 1.477(8) . ?
N1 C1 1.311(8) . ?
C1S C6S 1.383(10) . ?
C1S C2S 1.386(10) . ?
C6S C5S 1.393(10) . ?
C3S C4S 1.394(10) . ?
C3S C2S 1.372(10) . ?
C5S C4S 1.369(9) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C3 C2 1.508(10) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C5 C4 1.514(9) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?

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
S1 Pt1 S1 180.0 . 2_565 ?
S2 Pt1 S1 105.01(5) 2_565 . ?
S2 Pt1 S1 105.01(5) . 2_565 ?
S2 Pt1 S1 74.99(5) . . ?
S2 Pt1 S1 74.99(5) 2_565 2_565 ?
S2 Pt1 S2 180.0 . 2_565 ?
C1 S1 Pt1 87.7(2) . . ?
C1 S2 Pt1 87.2(2) . . ?
C4 N1 C2 116.9(5) . . ?
C1 N1 C2 120.8(5) . . ?
C1 N1 C4 122.0(5) . . ?
C6S C1S I1S 120.0(5) . . ?
C6S C1S C2S 116.7(6) . . ?
C2S C1S I1S 123.1(5) . . ?
F3S C6S C1S 118.9(6) . . ?
F3S C6S C5S 118.1(6) . . ?
C1S C6S C5S 123.0(6) . . ?
C4S C3S I2S 120.0(5) . . ?
C2S C3S I2S 123.5(5) . . ?
C2S C3S C4S 116.5(6) . . ?
C6S C5S I3S 120.9(5) . . ?
C4S C5S I3S 122.3(5) . . ?
C4S C5S C6S 116.7(6) . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
F2S C4S C3S 118.4(6) . . ?
F2S C4S C5S 118.0(6) . . ?
C5S C4S C3S 123.6(7) . . ?
F1S C2S C1S 118.0(6) . . ?
F1S C2S C3S 118.5(6) . . ?
C3S C2S C1S 123.5(7) . . ?
N1 C2 C3 112.3(5) . . ?
N1 C2 H2A 109.1 . . ?
N1 C2 H2B 109.1 . . ?
C3 C2 H2A 109.1 . . ?
C3 C2 H2B 109.1 . . ?
H2A C2 H2B 107.9 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
N1 C4 C5 112.5(5) . . ?
N1 C4 H4A 109.1 . . ?
N1 C4 H4B 109.1 . . ?
C5 C4 H4A 109.1 . . ?
C5 C4 H4B 109.1 . . ?
H4A C4 H4B 107.8 . . ?
S1 C1 S2 110.1(3) . . ?
N1 C1 S1 125.6(5) . . ?
N1 C1 S2 124.4(5) . . ?

# start Validation Reply Form
_vrf_PLAT431_eaa-162             
;
PROBLEM: Short Inter HL..A Contact  I2S      ..S2       .       3.42 Ang.  
RESPONSE: Short contact is the investigated feature of this structure.
;
# end Validation Reply Form

_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 1.525
_oxdiff_exptl_absorpt_empirical_full_min 0.749
####################################################################### 
# 
# 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_13298_m153
_database_code_depnum_ccdc_archive 'CCDC 2044966'
loop_
_audit_author_name
_audit_author_address
'Vitalii Suslonov'
;Saint Petersburg State University
Russia
;
_audit_update_record             
;
2020-11-17 deposited with the CCDC.	2021-03-23 downloaded from the CCDC.
;
_audit_creation_date             2019-08-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C6 F3 I3), C10 H20 N2 Pd S4'
_chemical_formula_sum            'C22 H20 F6 I6 N2 Pd S4'
_chemical_formula_weight         1422.44
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C22 H20 F3 I3 N2 Pd S4'
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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 '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'
Pd Pd 0.1215 3.9337 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.6378(2)
_cell_length_b                   9.5068(3)
_cell_length_c                   12.3335(3)
_cell_angle_alpha                107.763(3)
_cell_angle_beta                 89.773(2)
_cell_angle_gamma                113.626(3)
_cell_volume                     875.50(5)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    7404
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.9880
_cell_measurement_theta_min      3.7910
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    48.499
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37595
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.35a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.698
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16237
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.492
_diffrn_reflns_theta_min         3.798
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -55.00  28.00   0.50    0.20    --  -38.95  80.00 171.00  166
  2  ω    -22.00  18.00   0.50    0.20    --   38.95 -80.00  47.00   80
  3  ω    117.00 155.00   0.50    0.76    --  100.00  80.00 171.00   76
  4  ω     37.00 107.00   0.50    0.76    --  100.00 -80.00  47.00  140
  5  ω   -108.00 -33.00   0.50    0.20    --  -38.95 -32.00  30.00  150
  6  ω    -44.00 -19.00   0.50    0.20    --  -38.95 -21.00 150.00   50
  7  ω    -87.00 -45.00   0.50    0.20    --  -38.95 138.00  30.00   84
  8  ω    -56.00 -30.00   0.50    0.20    --  -38.95 138.00-120.00   52
  9  ω    -86.00 -61.00   0.50    0.20    --  -38.95 138.00-120.00   50
 10  ω    -34.00  24.00   0.50    0.20    --  -38.95  32.00-180.00  116
 11  ω     -7.00  28.00   0.50    0.20    --  -38.95  32.00 120.00   70
 12  ω   -100.00 -75.00   0.50    0.20    --  -38.95 -21.00 150.00   50
 13  ω     57.00  93.00   0.50    0.20    --   38.95  54.00 -90.00   72
 14  ω     67.00 104.00   0.50    0.20    --   38.95  54.00 -60.00   74
 15  ω     27.00  57.00   0.50    0.20    --   38.95  54.00 -60.00   60
 16  ω     69.00 101.00   0.50    0.20    --   38.95  77.00 -30.00   64
 17  ω     27.00  60.00   0.50    0.20    --   38.95 -80.00  47.00   66
 18  ω     44.00  80.00   0.50    0.20    --   38.95  32.00-150.00   72
 19  ω     23.00  53.00   0.50    0.20    --   38.95  54.00 -90.00   60
 20  ω     19.00  55.00   0.50    0.20    --   38.95  77.00 -30.00   72
 21  ω    -15.00  52.00   0.50    0.20    --   38.95-104.00  30.00  134
 22  ω      8.00  74.00   0.50    0.20    --   38.95-104.00-120.00  132
 23  ω     48.00 104.00   0.50    0.76    --  100.00-111.00-150.00  112
 24  ω     81.00 123.00   0.50    0.76    --  100.00-133.00  90.00   84
 25  ω     37.00 100.00   0.50    0.76    --  100.00-133.00  60.00  126
 26  ω    116.00 142.00   0.50    0.76    --  100.00  93.00 -30.00   52
 27  ω     82.00 115.00   0.50    0.76    --  100.00  93.00 -30.00   66
 28  ω     37.00 122.00   0.50    0.76    --  100.00 -61.00  60.00  170
 29  ω     32.00  60.00   0.50    0.76    --  100.00-111.00  90.00   56
 30  ω     56.00  82.00   0.50    0.76    --  100.00-111.00   0.00   52
 31  ω    132.00 157.00   0.50    0.76    --  100.00  61.00-150.00   50
 32  ω    124.00 151.00   0.50    0.76    --  100.00  93.00  30.00   54
 33  ω     80.00 156.00   0.50    0.76    --  100.00  53.00-120.00  152
 34  ω     43.00  69.00   0.50    0.76    --  100.00-133.00-150.00   52
 35  ω    109.00 157.00   0.50    0.76    --  100.00  45.00  90.00   96
 36  ω     86.00 157.00   0.50    0.76    --  100.00  37.00-150.00  142
 37  ω     74.00 100.00   0.50    0.76    --  100.00 -93.00-150.00   52
 38  ω     95.00 121.00   0.50    0.76    --  100.00  61.00-150.00   52
 39  ω     34.00  93.00   0.50    0.76    --  100.00-111.00  60.00  118
 40  ω    114.00 139.00   0.50    0.76    --  100.00  69.00 -90.00   50
 41  ω     39.00 120.00   0.50    0.76    --  100.00 -53.00-150.00  162
 42  ω     82.00 107.00   0.50    0.76    --  100.00  93.00  30.00   50
 43  ω    124.00 153.00   0.50    0.76    --  100.00  77.00   0.00   58
 44  ω     81.00 112.00   0.50    0.76    --  100.00  69.00 -90.00   62
 45  ω    122.00 152.00   0.50    0.76    --  100.00  53.00 150.00   60
 46  ω     36.00  70.00   0.50    0.76    --  100.00 -69.00-180.00   68
 47  ω     75.00 103.00   0.50    0.76    --  100.00 -37.00  30.00   56
 48  ω     34.00  84.00   0.50    0.76    --  100.00-111.00 -30.00  100
 49  ω     83.00 153.00   0.50    0.76    --  100.00  22.00 150.00  140
 50  ω     83.00 120.00   0.50    0.76    --  100.00-133.00-150.00   74
 51  ω     38.00  64.00   0.50    0.76    --  100.00-133.00 -30.00   52
 52  ω     77.00 122.00   0.50    0.76    --  100.00-133.00 -30.00   90
 53  ω    105.00 130.00   0.50    0.76    --  100.00  37.00-180.00   50
 54  ω     82.00 108.00   0.50    0.76    --  100.00  61.00 150.00   52
 55  ω     92.00 130.00   0.50    0.76    --  100.00  37.00 -30.00   76
 56  ω     83.00 108.00   0.50    0.76    --  100.00-111.00  90.00   50
 57  ω     33.00  72.00   0.50    0.76    --  100.00 -37.00  30.00   78
 58  ω     54.00 120.00   0.50    0.76    --  100.00-133.00  30.00  132
 59  ω    121.00 147.00   0.50    0.76    --  100.00  93.00 120.00   52
 60  ω     30.00  80.00   0.50    0.76    --  100.00 -93.00-120.00  100
 61  ω     16.00  42.00   0.50    0.20    --   38.95 -80.00  47.00   52
 62  ω    -46.00 -14.00   0.50    0.20    --    0.00 117.00  85.98   64
 63  ω    -19.00   6.00   0.50    0.20    --   24.00 112.00 -60.77   50
 64  ω    -10.00  15.00   0.50    0.20    --   28.00 104.00  21.94   50
 65  ω     -5.00  20.00   0.50    0.20    --   28.00  95.00-154.73   50
 66  ω     -1.00  24.00   0.50    0.20    --   32.00  93.00 -92.25   50
 67  ω     -1.00  24.00   0.50    0.20    --   32.00  94.00 -26.43   50
 68  ω     -1.00  24.00   0.50    0.20    --   32.00  94.00  87.35   50
 69  ω      1.00  26.00   0.50    0.20    --   32.00  88.00 159.83   50
 70  ω      5.00  30.00   0.50    0.20    --   36.00  89.00  10.15   50
 71  ω      5.00  30.00   0.50    0.20    --   36.00  89.00-141.11   50
 72  ω     12.00  37.00   0.50    0.20    --   40.00  82.00-172.28   50
 73  ω     12.00  37.00   0.50    0.20    --   40.00  81.00 139.43   50
 74  ω     11.00  36.00   0.50    0.20    --   40.00  83.00  99.12   50
 75  ω     17.00  42.00   0.50    0.20    --   44.00  79.00 -63.86   50
 76  ω     16.00  41.00   0.50    0.20    --   44.00  81.00 -92.61   50
 77  ω     16.00  41.00   0.50    0.20    --   44.00  82.00  -4.25   50
 78  ω     16.00  41.00   0.50    0.20    --   44.00  82.00  39.69   50
 79  ω     16.00  41.00   0.50    0.20    --   44.00  81.00-150.61   50
 80  ω     16.00  41.00   0.50    0.20    --   44.00  82.00 -60.87   50
 81  ω     16.00  41.00   0.50    0.20    --   44.00  81.00 151.76   50
 82  ω     22.00  48.00   0.50    0.20    --   48.00  75.00-119.77   52
 83  ω     80.00 118.00   0.50    0.20    --   52.00  75.00  89.56   76
 84  ω     26.00  53.00   0.50    0.20    --   52.00  75.00  89.56   54
 85  ω     31.00  58.00   0.50    0.20    --   52.00  75.00  -1.96   54
 86  ω     93.00 118.00   0.50    0.20    --   52.00  75.00  -1.96   50
 87  ω     29.00  73.00   0.50    0.20    --   52.00  77.00 -91.44   88
 88  ω     32.00  58.00   0.50    0.20    --   52.00  77.00 -49.08   52
 89  ω     28.00  68.00   0.50    0.20    --   52.00  73.00 131.87   80
 90  ω     46.00  72.00   0.50    0.20    --   56.00  57.00-116.08   52
 91  ω     90.00 116.00   0.50    0.20    --   56.00  57.00-116.08   52
 92  ω     35.00  61.00   0.50    0.20    --   56.00  66.00-167.11   52
 93  ω     37.00  63.00   0.50    0.20    --   56.00  59.00 103.92   52
 94  ω     35.00  65.00   0.50    0.20    --   60.00  72.00 -58.85   60
 95  ω     43.00  81.00   0.50    0.20    --   68.00  73.00-111.20   76
 96  ω     52.00  77.00   0.50    0.20    --   68.00  47.00 178.96   50
 97  ω     98.00 133.00   0.50    0.20    --   68.00  77.00  44.86   70
 98  ω     41.00  67.00   0.50    0.20    --   68.00  77.00  44.86   52
 99  ω     88.00 113.00   0.50    0.20    --   68.00  67.00 118.44   50
100  ω     52.00  77.00   0.50    0.20    --   68.00  67.00 118.44   50
101  ω     46.00  92.00   0.50    0.76    --   72.00  76.00-175.41   92
102  ω     96.00 122.00   0.50    0.76    --   76.00  67.00 103.99   52
103  ω     51.00  81.00   0.50    0.76    --   76.00  73.00  13.25   60
104  ω     52.00  78.00   0.50    0.76    --   76.00  67.00 103.99   52
105  ω     50.00  76.00   0.50    0.76    --   76.00  77.00  63.11   52
106  ω     52.00  78.00   0.50    0.76    --   76.00  67.00 -29.14   52
107  ω     60.00  85.00   0.50    0.76    --   80.00  57.00 -35.02   50
108  ω     67.00  92.00   0.50    0.76    --   88.00  62.00-118.13   50
109  ω    106.00 131.00   0.50    0.76    --   92.00  61.00 103.48   50
110  ω     71.00  99.00   0.50    0.76    --   92.00  61.00 103.48   56
111  ω     73.00 105.00   0.50    0.76    --  100.00  77.00  90.00   64
112  ω     88.00 114.00   0.50    0.76    --  100.00 -45.00 -60.00   52
113  ω     78.00 112.00   0.50    0.76    --  100.00  69.00 120.00   68
114  ω     55.00  80.00   0.50    0.76    --  100.00 -45.00 -60.00   50
115  ω     84.00 110.00   0.50    0.76    --  100.00 -30.00  30.00   52
116  ω     40.00  66.00   0.50    0.76    --  100.00 -30.00  30.00   52
117  ω     80.00 106.00   0.50    0.76    --  100.00 -15.00  60.00   52
118  ω     25.00  75.00   0.50    0.76    --  100.00 -15.00  60.00  100
119  ω    125.00 151.00   0.50    0.76    --  100.00  77.00-120.00   52
120  ω     78.00 104.00   0.50    0.76    --  100.00  61.00 120.00   52
121  ω     73.00 111.00   0.50    0.76    --  100.00  77.00 -90.00   76
122  ω     73.00 126.00   0.50    0.76    --  100.00  77.00   0.00  106
123  ω    121.00 149.00   0.50    0.76    --  100.00  77.00  60.00   56
124  ω     73.00 118.00   0.50    0.76    --  100.00  77.00-120.00   90
125  ω     75.00 114.00   0.50    0.76    --  100.00  77.00  60.00   78
126  ω     73.00 134.00   0.50    0.76    --  100.00  77.00  30.00  122
127  ω     36.00  84.00   0.50    0.76    --  100.00 -30.00 -90.00   96
128  ω     78.00 119.00   0.50    0.76    --  100.00  61.00 150.00   82
129  ω     73.00 123.00   0.50    0.76    --  100.00  77.00 -60.00  100
130  ω     76.00 101.00   0.50    0.76    --  100.00  69.00-180.00   50
131  ω    119.00 145.00   0.50    0.76    --  100.00  30.00-180.00   52
132  ω     75.00 104.00   0.50    0.76    --  100.00  77.00 -30.00   58
133  ω     75.00 101.00   0.50    0.76    --  100.00  71.00-167.22   52
134  ω     77.00 128.00   0.50    0.76    --  100.00  69.00  60.00  102
135  ω     76.00 118.00   0.50    0.76    --  100.00  69.00-150.00   84
136  ω    108.00 156.00   0.50    0.76    --  100.00  93.00 -60.00   96
137  ω     75.00 104.00   0.50    0.76    --  100.00  77.00 150.00   58
138  ω    111.00 138.00   0.50    0.76    --  100.00  69.00 -30.00   54
139  ω     88.00 114.00   0.50    0.76    --  100.00 -30.00 120.00   52
140  ω    118.00 144.00   0.50    0.76    --  100.00  61.00  30.00   52
141  ω     49.00  84.00   0.50    0.76    --  100.00 -30.00 120.00   70
142  ω    131.00 157.00   0.50    0.76    --  100.00  77.00  90.00   52
143  ω     78.00 104.00   0.50    0.76    --  100.00  61.00  30.00   52
144  ω     76.00 101.00   0.50    0.76    --  100.00  69.00 -30.00   50
145  ω    -44.00 -19.00   0.50    0.20    --  -38.95  80.00 171.00   50
146  ω     44.00  70.00   0.50    0.20    --   68.00  68.00 147.45   52
147  ω     47.00  73.00   0.50    0.20    --   68.00  60.00 -36.93   52
148  ω     50.00  75.00   0.50    0.76    --   76.00  76.00 -37.27   50
149  ω     54.00  79.00   0.50    0.76    --   80.00  75.00-162.28   50
150  ω     57.00  83.00   0.50    0.76    --   84.00  77.00-106.50   52
151  ω     78.00 104.00   0.50    0.76    --  100.00  70.00  15.43   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1847906107
_diffrn_orient_matrix_UB_12      0.1307412037
_diffrn_orient_matrix_UB_13      0.0383141450
_diffrn_orient_matrix_UB_21      -0.0088335938
_diffrn_orient_matrix_UB_22      0.0493541699
_diffrn_orient_matrix_UB_23      -0.1069582540
_diffrn_orient_matrix_UB_31      -0.0661863096
_diffrn_orient_matrix_UB_32      0.1249466720
_diffrn_orient_matrix_UB_33      0.0679537744
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3076
_reflns_number_total             3340
_reflns_odcompleteness_completeness 98.35
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.14
_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 1.171.39.35a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.275
_refine_diff_density_min         -2.171
_refine_diff_density_rms         0.171
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         3340
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0352
_refine_ls_restrained_S_all      1.072
_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)+(0.0486P)²+3.1622P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0916
_refine_ls_wR_factor_ref         0.0941
_refine_special_details          ?
_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.a Secondary CH4 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C5(H5A,H5B,H5C)
;
_atom_sites_solution_hydrogens   geom
_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
I2S I 0.21682(5) -0.24971(4) 0.26659(3) 0.02873(12) Uani 1 1 d . . . . .
Pd1 Pd 0.5000 0.5000 1.0000 0.01930(14) Uani 1 2 d S T P . .
I1S I 0.29815(6) 0.24865(6) 0.73491(4) 0.05151(17) Uani 1 1 d . . . . .
I3S I -0.27220(5) -0.42334(6) 0.60269(4) 0.04255(14) Uani 1 1 d . . . . .
S2 S 0.74450(16) 0.45258(16) 1.00344(11) 0.0226(3) Uani 1 1 d . . . . .
S1 S 0.43463(17) 0.30221(16) 1.08794(12) 0.0241(3) Uani 1 1 d . . . . .
F2S F -0.0814(4) -0.4437(4) 0.3828(3) 0.0318(8) Uani 1 1 d . . . . .
F1S F 0.3561(5) 0.0824(4) 0.4808(3) 0.0400(9) Uani 1 1 d . . . . .
F3S F -0.0296(6) -0.0558(6) 0.7398(3) 0.0467(10) Uani 1 1 d . . . . .
N1 N 0.7058(6) 0.2354(6) 1.1117(4) 0.0252(10) Uani 1 1 d . . . . .
C5S C 0.1374(7) -0.1810(7) 0.4275(5) 0.0246(11) Uani 1 1 d . . . . .
C2 C 0.6060(7) 0.1151(7) 1.1660(5) 0.0287(13) Uani 1 1 d . . . . .
H2A H 0.6463 0.0301 1.1501 0.034 Uiso 1 1 calc R . . . .
H2B H 0.4872 0.0652 1.1329 0.034 Uiso 1 1 calc R . . . .
C1S C 0.1668(9) 0.0179(8) 0.6115(5) 0.0341(14) Uani 1 1 d . . . . .
C1 C 0.6398(7) 0.3145(6) 1.0734(5) 0.0241(11) Uani 1 1 d . . . . .
C4S C 0.2199(8) -0.0274(8) 0.5069(5) 0.0290(12) Uani 1 1 d . . . . .
C2S C -0.0009(8) -0.2924(8) 0.4570(5) 0.0272(12) Uani 1 1 d . . . . .
C4 C 0.8894(7) 0.2712(7) 1.1111(6) 0.0288(13) Uani 1 1 d . . . . .
H4A H 0.9338 0.2687 1.1823 0.035 Uiso 1 1 calc R . . . .
H4B H 0.9509 0.3800 1.1077 0.035 Uiso 1 1 calc R . . . .
C6S C 0.0250(9) -0.0959(9) 0.6371(5) 0.0355(15) Uani 1 1 d . . . . .
C3S C -0.0615(8) -0.2532(8) 0.5613(5) 0.0303(13) Uani 1 1 d . . . . .
C3 C 0.6203(8) 0.1916(8) 1.2941(6) 0.0356(14) Uani 1 1 d . . . . .
H3A H 0.5808 0.2760 1.3102 0.053 Uiso 1 1 calc GR . . . .
H3B H 0.7372 0.2372 1.3276 0.053 Uiso 1 1 calc GR . . . .
H3C H 0.5518 0.1103 1.3262 0.053 Uiso 1 1 calc GR . . . .
C5 C 0.9209(9) 0.1518(8) 1.0114(7) 0.0421(16) Uani 1 1 d . . . . .
H5A H 0.8799 0.1557 0.9406 0.063 Uiso 1 1 calc GR . . . .
H5B H 0.8620 0.0440 1.0151 0.063 Uiso 1 1 calc GR . . . .
H5C H 1.0410 0.1796 1.0149 0.063 Uiso 1 1 calc GR . . . .


_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
I2S C5S 2.096(6) . ?
Pd1 S2 2.3325(13) . ?
Pd1 S2 2.3325(13) 2_667 ?
Pd1 S1 2.3280(13) 2_667 ?
Pd1 S1 2.3280(13) . ?
I1S C1S 2.097(6) . ?
I3S C3S 2.080(6) . ?
S2 C1 1.738(6) . ?
S1 C1 1.741(6) . ?
F2S C2S 1.337(7) . ?
F1S C4S 1.340(7) . ?
F3S C6S 1.348(7) . ?
N1 C2 1.474(7) . ?
N1 C1 1.295(8) . ?
N1 C4 1.483(7) . ?
C5S C4S 1.378(8) . ?
C5S C2S 1.378(9) . ?
C2 C3 1.507(9) . ?
C1S C4S 1.370(9) . ?
C1S C6S 1.384(11) . ?
C2S C3S 1.388(9) . ?
C4 C5 1.506(10) . ?
C6S C3S 1.387(10) . ?

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
S2 Pd1 S2 180.0 2_667 . ?
S1 Pd1 S2 104.65(5) 2_667 . ?
S1 Pd1 S2 104.65(5) . 2_667 ?
S1 Pd1 S2 75.35(5) 2_667 2_667 ?
S1 Pd1 S2 75.35(5) . . ?
S1 Pd1 S1 180.00(7) 2_667 . ?
C1 S2 Pd1 87.3(2) . . ?
C1 S1 Pd1 87.4(2) . . ?
C2 N1 C4 116.8(5) . . ?
C1 N1 C2 121.8(5) . . ?
C1 N1 C4 121.3(5) . . ?
C4S C5S I2S 122.4(4) . . ?
C4S C5S C2S 117.9(5) . . ?
C2S C5S I2S 119.7(4) . . ?
N1 C2 C3 111.8(5) . . ?
C4S C1S I1S 122.3(5) . . ?
C4S C1S C6S 118.1(6) . . ?
C6S C1S I1S 119.5(5) . . ?
S2 C1 S1 110.0(3) . . ?
N1 C1 S2 125.1(4) . . ?
N1 C1 S1 124.9(4) . . ?
F1S C4S C5S 119.1(5) . . ?
F1S C4S C1S 118.6(6) . . ?
C1S C4S C5S 122.4(6) . . ?
F2S C2S C5S 119.4(5) . . ?
F2S C2S C3S 118.3(5) . . ?
C5S C2S C3S 122.3(6) . . ?
N1 C4 C5 112.5(5) . . ?
F3S C6S C1S 119.6(6) . . ?
F3S C6S C3S 118.3(7) . . ?
C1S C6S C3S 122.1(6) . . ?
C2S C3S I3S 121.4(5) . . ?
C6S C3S I3S 121.4(5) . . ?
C6S C3S C2S 117.2(6) . . ?

# start Validation Reply Form
_vrf_PLAT431_13298_m153          
;
PROBLEM: Short Inter HL..A Contact  I2S      ..S2       .       3.39 Ang.  
RESPONSE: Short contact is the investigated feature of this structure.
;
# end Validation Reply Form

_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 3.222
_oxdiff_exptl_absorpt_empirical_full_min 0.603
####################################################################### 
# 
# 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_13229_m150
_database_code_depnum_ccdc_archive 'CCDC 2044964'
loop_
_audit_author_name
_audit_author_address
'Vitalii Suslonov'
;Saint Petersburg State University
Russia
;
_audit_update_record             
;
2020-11-17 deposited with the CCDC.	2021-03-23 downloaded from the CCDC.
;
_audit_creation_date             2019-07-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C6 F3 I3), C10 H20 N2 Ni S4'
_chemical_formula_sum            'C22 H20 F6 I6 N2 Ni S4'
_chemical_formula_weight         1374.75
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C16 H20 F3 I3 N2 Ni S4'
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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 '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'
Ni Ni -3.0029 0.5091 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.6870(2)
_cell_length_b                   9.4313(2)
_cell_length_c                   12.2577(2)
_cell_angle_alpha                106.930(2)
_cell_angle_beta                 91.1590(10)
_cell_angle_gamma                113.553(2)
_cell_volume                     869.96(3)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    13304
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.2460
_cell_measurement_theta_min      3.8040
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    45.309
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.12157
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.50a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.624
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             630
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14447
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        62.455
_diffrn_reflns_theta_max         62.455
_diffrn_reflns_theta_min         3.816
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -107.00 -82.00   0.50    2.20    --  -38.95 -33.00  91.00   50
  2  ω     -9.00  30.00   0.50    2.20    --  -38.95  33.00-109.00   78
  3  ω    -50.00 -25.00   0.50    2.20    --  -38.95 -33.00  91.00   50
  4  ω    -29.00   0.00   0.50    2.20    --   38.95 -33.00  91.00   58
  5  ω     34.00 109.00   0.50    2.29    --  100.00 -33.00  91.00  150
  6  ω    108.00 134.00   0.50    2.29    --  100.00  33.00-109.00   52
  7  ω    -58.00  24.00   0.50    2.20    --  -38.95  54.00  30.00  164
  8  ω   -107.00 -66.00   0.50    2.20    --  -38.95 -32.00 -60.00   82
  9  ω     -3.00  23.00   0.50    2.20    --  -38.95  65.00-120.00   52
 10  ω    -27.00  16.00   0.50    2.20    --  -38.95 104.00 150.00   86
 11  ω    -62.00  -7.00   0.50    2.20    --  -38.95  65.00-120.00  110
 12  ω    -77.00 -41.00   0.50    2.20    --  -38.95 104.00 150.00   72
 13  ω    -57.00 -12.00   0.50    2.20    --  -38.95  54.00 120.00   90
 14  ω     -2.00  24.00   0.50    2.20    --  -38.95  54.00 120.00   52
 15  ω    -57.00 -31.00   0.50    2.20    --  -38.95 -32.00 -60.00   52
 16  ω     13.00  86.00   0.50    2.20    --   38.95-138.00 -30.00  146
 17  ω     -7.00  62.00   0.50    2.20    --   38.95 -77.00  60.00  138
 18  ω     24.00  58.00   0.50    2.20    --   38.95 -21.00 -30.00   68
 19  ω     42.00  67.00   0.50    2.20    --   38.95-138.00  60.00   50
 20  ω     20.00  53.00   0.50    2.20    --   38.95 -33.00  91.00   66
 21  ω     52.00  77.00   0.50    2.20    --   38.95-104.00 -30.00   50
 22  ω      0.00  32.00   0.50    2.20    --   38.95-104.00 -30.00   64
 23  ω     78.00 103.00   0.50    2.20    --   38.95  33.00-109.00   50
 24  ω    -29.00  12.00   0.50    2.20    --   38.95 -21.00 -30.00   82
 25  ω    107.00 132.00   0.50    2.29    --  100.00  30.00  60.00   50
 26  ω     31.00 105.00   0.50    2.29    --  100.00-111.00 -60.00  148
 27  ω     35.00 103.00   0.50    2.29    --  100.00 -77.00 120.00  136
 28  ω     27.00  87.00   0.50    2.29    --  100.00 -20.00  20.70  120
 29  ω     83.00 108.00   0.50    2.29    --  100.00 -93.00-150.00   50
 30  ω     97.00 122.00   0.50    2.29    --  100.00  30.00   0.00   50
 31  ω     86.00 111.00   0.50    2.29    --  100.00-111.00 -90.00   50
 32  ω     81.00 157.00   0.50    2.29    --  100.00  22.00 -30.00  152
 33  ω     36.00  90.00   0.50    2.29    --  100.00 -53.00-150.00  108
 34  ω     65.00 108.00   0.50    2.29    --  100.00 -93.00 120.00   86
 35  ω     32.00  58.00   0.50    2.29    --  100.00 -93.00 120.00   52
 36  ω     56.00  81.00   0.50    2.29    --  100.00-111.00 -90.00   50
 37  ω     88.00 118.00   0.50    2.29    --  100.00-133.00 120.00   60
 38  ω     38.00  75.00   0.50    2.29    --  100.00-133.00 120.00   74
 39  ω     79.00 136.00   0.50    2.29    --  100.00  61.00 -90.00  114
 40  ω     36.00 111.00   0.50    2.29    --  100.00 -37.00 -60.00  150
 41  ω     70.00 108.00   0.50    2.29    --  100.00 -53.00 120.00   76
 42  ω     37.00 103.00   0.50    2.29    --  100.00 -53.00 -90.00  132
 43  ω     39.00 119.00   0.50    2.29    --  100.00-133.00 -90.00  160
 44  ω    112.00 137.00   0.50    2.29    --  100.00  61.00 -30.00   50
 45  ω     97.00 152.00   0.50    2.29    --  100.00  22.00  30.00  110
 46  ω     82.00 130.00   0.50    2.29    --  100.00 -15.00  60.00   96
 47  ω     71.00 105.00   0.50    2.29    --  100.00-111.00   0.00   68
 48  ω     89.00 115.00   0.50    2.29    --  100.00 -53.00  60.00   52
 49  ω     29.00  76.00   0.50    2.29    --  100.00 -15.00  60.00   94
 50  ω     82.00 154.00   0.50    2.29    --  100.00  53.00-120.00  144
 51  ω     78.00 113.00   0.50    2.29    --  100.00  61.00  30.00   70
 52  ω    128.00 153.00   0.50    2.29    --  100.00  61.00  30.00   50
 53  ω     80.00 106.00   0.50    2.29    --  100.00  61.00 -30.00   52
 54  ω     84.00 109.00   0.50    2.29    --  100.00-111.00  60.00   50
 55  ω     70.00 101.00   0.50    2.29    --  100.00 -53.00 -60.00   62
 56  ω     46.00 109.00   0.50    2.29    --  100.00 -61.00  30.00  126
 57  ω     31.00 130.00   0.50    2.29    --  100.00 -86.00 -60.00  198
 58  ω     32.00 105.00   0.50    2.29    --  100.00-111.00 120.00  146
 59  ω    -78.00 -52.00   0.50    2.20    --  -38.95 -33.00  91.00   52
 60  ω    -29.00  -4.00   0.50    2.20    --   12.00 110.00  47.86   50
 61  ω    -26.00  -1.00   0.50    2.20    --   20.00 118.00 -17.90   50
 62  ω    -21.00   4.00   0.50    2.20    --   24.00 116.00-176.88   50
 63  ω     -7.00  18.00   0.50    2.20    --   28.00  99.00  47.23   50
 64  ω     -1.00  24.00   0.50    2.20    --   32.00  94.00 -35.22   50
 65  ω     -1.00  24.00   0.50    2.20    --   32.00  94.00 114.64   50
 66  ω      6.00  31.00   0.50    2.20    --   36.00  86.00 -11.67   50
 67  ω      5.00  30.00   0.50    2.20    --   36.00  88.00-161.08   50
 68  ω      4.00  29.00   0.50    2.20    --   36.00  90.00-130.96   50
 69  ω      6.00  31.00   0.50    2.20    --   36.00  87.00  77.49   50
 70  ω     -4.00  22.00   0.50    2.20    --   38.95 -33.00  91.00   52
 71  ω     11.00  36.00   0.50    2.20    --   40.00  84.00 117.81   50
 72  ω     11.00  36.00   0.50    2.20    --   40.00  83.00  44.20   50
 73  ω     16.00  41.00   0.50    2.20    --   44.00  81.00 161.64   50
 74  ω     16.00  41.00   0.50    2.20    --   44.00  81.00  13.09   50
 75  ω     17.00  43.00   0.50    2.20    --   44.00  82.00 -87.92   52
 76  ω     16.00  41.00   0.50    2.20    --   44.00  80.00-113.27   50
 77  ω     16.00  41.00   0.50    2.20    --   44.00  80.00  83.28   50
 78  ω     27.00  63.00   0.50    2.20    --   52.00  75.00 -48.75   72
 79  ω     27.00  60.00   0.50    2.20    --   52.00  76.00 -35.67   66
 80  ω     29.00  55.00   0.50    2.20    --   52.00  71.00-160.96   52
 81  ω     25.00  50.00   0.50    2.20    --   52.00  77.00 142.70   50
 82  ω     30.00  56.00   0.50    2.20    --   52.00  61.00 110.82   52
 83  ω     27.00  53.00   0.50    2.20    --   52.00  75.00   5.76   52
 84  ω     34.00  61.00   0.50    2.20    --   56.00  68.00-101.92   54
 85  ω     82.00 109.00   0.50    2.20    --   56.00  65.00  47.24   54
 86  ω     33.00  58.00   0.50    2.20    --   56.00  65.00  47.24   50
 87  ω     36.00  87.00   0.50    2.20    --   60.00  75.00 152.71  102
 88  ω    104.00 130.00   0.50    2.20    --   64.00  68.00  67.32   52
 89  ω     41.00  72.00   0.50    2.20    --   64.00  68.00  67.32   62
 90  ω     40.00 130.00   0.50    2.20    --   64.00  69.00 112.89  180
 91  ω     96.00 122.00   0.50    2.20    --   68.00  76.00-138.62   52
 92  ω     42.00  74.00   0.50    2.20    --   68.00  76.00-138.62   64
 93  ω     44.00  69.00   0.50    2.20    --   68.00  70.00-172.61   50
 94  ω    112.00 137.00   0.50    2.29    --   72.00  59.00 -85.31   50
 95  ω     53.00  85.00   0.50    2.29    --   72.00  59.00 -85.31   64
 96  ω     46.00  86.00   0.50    2.29    --   72.00  76.00  -5.80   80
 97  ω     56.00  82.00   0.50    2.29    --   76.00  61.00  42.47   52
 98  ω     50.00  91.00   0.50    2.29    --   76.00  74.00  70.17   82
 99  ω     55.00  80.00   0.50    2.29    --   76.00  62.00 -20.63   50
100  ω     55.00  89.00   0.50    2.29    --   80.00  77.00-150.51   68
101  ω     64.00  91.00   0.50    2.29    --   84.00  64.00  14.83   54
102  ω     66.00  96.00   0.50    2.29    --   88.00  59.00 167.86   60
103  ω     73.00 120.00   0.50    2.29    --  100.00  77.00-120.00   94
104  ω     74.00 148.00   0.50    2.29    --  100.00  77.00  90.00  148
105  ω     73.00 114.00   0.50    2.29    --  100.00  77.00-180.00   82
106  ω     74.00 100.00   0.50    2.29    --  100.00  77.00 -60.00   52
107  ω    112.00 152.00   0.50    2.29    --  100.00  77.00 120.00   80
108  ω    127.00 153.00   0.50    2.29    --  100.00  93.00   0.00   52
109  ω    109.00 135.00   0.50    2.29    --  100.00  77.00-150.00   52
110  ω    126.00 152.00   0.50    2.29    --  100.00  77.00  30.00   52
111  ω     73.00 101.00   0.50    2.29    --  100.00  77.00-150.00   56
112  ω     73.00 117.00   0.50    2.29    --  100.00  77.00  30.00   88
113  ω    109.00 144.00   0.50    2.29    --  100.00  61.00-180.00   70
114  ω     76.00 107.00   0.50    2.29    --  100.00  69.00   0.00   62
115  ω     73.00 103.00   0.50    2.29    --  100.00  77.00 120.00   60
116  ω     78.00 131.00   0.50    2.29    --  100.00  61.00  90.00  106
117  ω     80.00 105.00   0.50    2.29    --  100.00  61.00 120.00   50
118  ω     78.00 105.00   0.50    2.29    --  100.00  61.00-180.00   54
119  ω    104.00 144.00   0.50    2.29    --  100.00 111.00  90.00   80
120  ω    122.00 151.00   0.50    2.29    --  100.00  53.00  60.00   58
121  ω     78.00 104.00   0.50    2.29    --  100.00  61.00 -60.00   52
122  ω     73.00  99.00   0.50    2.29    --  100.00  77.00 -30.00   52
123  ω    123.00 152.00   0.50    2.29    --  100.00  77.00 150.00   58
124  ω    114.00 143.00   0.50    2.29    --  100.00  45.00-150.00   58
125  ω     73.00 118.00   0.50    2.29    --  100.00  77.00 150.00   90
126  ω    121.00 148.00   0.50    2.29    --  100.00  93.00  60.00   54
127  ω    100.00 156.00   0.50    2.29    --  100.00  30.00 150.00  112
128  ω     61.00 126.00   0.50    2.29    --  100.00 -15.00 -90.00  130
129  ω     73.00  98.00   0.50    2.29    --  100.00  77.00 -90.00   50
130  ω     76.00 102.00   0.50    2.29    --  100.00  69.00 120.00   52
131  ω     78.00 103.00   0.50    2.29    --  100.00  61.00-120.00   50
132  ω     76.00 126.00   0.50    2.29    --  100.00  69.00  60.00  100
133  ω    -36.00 -11.00   0.50    2.20    --  -38.95  33.00-109.00   50
134  ω     40.00  66.00   0.50    2.20    --   64.00  73.00 -80.54   52
135  ω     50.00  76.00   0.50    2.29    --   76.00  75.00 -80.14   52
136  ω     51.00  77.00   0.50    2.29    --   76.00  75.00 170.40   52
137  ω     50.00  75.00   0.50    2.29    --   76.00  74.00 143.77   50
138  ω     63.00  89.00   0.50    2.29    --   88.00  74.00-127.36   52
139  ω     62.00  88.00   0.50    2.29    --   88.00  74.00 -50.03   52
140  ω    -36.00 -11.00   0.50    2.20    --  -38.95  33.00-109.00   50
141  ω     -6.00  19.00   0.50    2.20    --   28.00  97.00 -97.24   50
142  ω     49.00  75.00   0.50    2.29    --   76.00  77.00-125.23   52
143  ω     63.00  89.00   0.50    2.29    --   84.00  72.00  87.09   52
144  ω     96.00 143.00   0.50    2.29    --  100.00  30.00-180.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1537541000
_diffrn_orient_matrix_UB_12      -0.0125043000
_diffrn_orient_matrix_UB_13      -0.0553002000
_diffrn_orient_matrix_UB_21      -0.0549072000
_diffrn_orient_matrix_UB_22      -0.1725619000
_diffrn_orient_matrix_UB_23      0.0089064000
_diffrn_orient_matrix_UB_31      -0.1081741000
_diffrn_orient_matrix_UB_32      -0.0748855000
_diffrn_orient_matrix_UB_33      -0.1206279000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2695
_reflns_number_total             2765
_reflns_odcompleteness_completeness 96.04
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     72.42
_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 1.171.40.50a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.50a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.50a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.728
_refine_diff_density_min         -2.566
_refine_diff_density_rms         0.198
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         2765
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0366
_refine_ls_restrained_S_all      1.096
_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)+(0.0600P)²+4.2700P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.0990
_refine_special_details          ?
_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.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C5(H5A,H5B,H5C)
;
_atom_sites_solution_hydrogens   geom
_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
I2S I 0.21773(5) 0.24935(4) 0.26816(3) 0.02189(15) Uani 1 1 d . . . . .
I3S I -0.26656(6) 0.08737(6) 0.60432(4) 0.03777(17) Uani 1 1 d . . . . .
I1S I 0.31108(7) 0.76169(6) 0.73079(4) 0.04312(19) Uani 1 1 d . . . . .
Ni1 Ni 0.5000 1.0000 0.0000 0.0159(3) Uani 1 2 d S T P . .
S2 S 0.73282(18) 0.95740(18) -0.00247(12) 0.0181(3) Uani 1 1 d . . . . .
S1 S 0.43328(18) 0.81188(17) 0.08553(13) 0.0190(3) Uani 1 1 d . . . . .
F1S F 0.3630(5) 0.5862(4) 0.4793(3) 0.0294(9) Uani 1 1 d . . . . .
F2S F -0.0782(5) 0.0575(4) 0.3861(3) 0.0267(8) Uani 1 1 d . . . . .
F3S F -0.0175(6) 0.4573(6) 0.7392(3) 0.0421(11) Uani 1 1 d . . . . .
N1 N 0.7004(6) 0.7397(6) 0.1086(4) 0.0191(10) Uani 1 1 d . . . . .
C5S C -0.0554(9) 0.2548(8) 0.5622(6) 0.0247(14) Uani 1 1 d . . . . .
C2S C 0.2278(8) 0.4779(8) 0.5071(6) 0.0234(14) Uani 1 1 d . . . . .
C1S C 0.1744(9) 0.5260(8) 0.6116(5) 0.0261(15) Uani 1 1 d . . . . .
C3S C 0.1423(8) 0.3211(8) 0.4282(5) 0.0207(13) Uani 1 1 d . . . . .
C4S C 0.0043(8) 0.2121(8) 0.4593(5) 0.0228(13) Uani 1 1 d . . . . .
C1 C 0.6343(7) 0.8218(7) 0.0697(5) 0.0167(12) Uani 1 1 d . . . . .
C2 C 0.6016(8) 0.6191(7) 0.1633(6) 0.0225(13) Uani 1 1 d . . . . .
H2A H 0.6402 0.5305 0.1469 0.027 Uiso 1 1 calc R . . . .
H2B H 0.4800 0.5698 0.1297 0.027 Uiso 1 1 calc R . . . .
C6S C 0.0349(9) 0.4130(9) 0.6370(6) 0.0297(16) Uani 1 1 d . . . . .
C4 C 0.8820(8) 0.7743(7) 0.1077(6) 0.0231(14) Uani 1 1 d . . . . .
H4A H 0.9320 0.7830 0.1840 0.028 Uiso 1 1 calc R . . . .
H4B H 0.9423 0.8812 0.0957 0.028 Uiso 1 1 calc R . . . .
C3 C 0.6213(9) 0.6974(8) 0.2941(6) 0.0266(14) Uani 1 1 d . . . . .
H3A H 0.5769 0.7807 0.3106 0.040 Uiso 1 1 calc GR . . . .
H3B H 0.7419 0.7485 0.3274 0.040 Uiso 1 1 calc GR . . . .
H3C H 0.5578 0.6131 0.3280 0.040 Uiso 1 1 calc GR . . . .
C5 C 0.9100(8) 0.6453(8) 0.0155(7) 0.0293(15) Uani 1 1 d . . . . .
H5A H 0.8775 0.6479 -0.0607 0.044 Uiso 1 1 calc GR . . . .
H5B H 0.8406 0.5373 0.0214 0.044 Uiso 1 1 calc GR . . . .
H5C H 1.0304 0.6666 0.0256 0.044 Uiso 1 1 calc GR . . . .


_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
I2S C3S 2.091(6) . ?
I3S C5S 2.079(7) . ?
I1S C1S 2.101(6) . ?
Ni1 S2 2.2131(14) . ?
Ni1 S2 2.2131(14) 2_675 ?
Ni1 S1 2.2066(14) 2_675 ?
Ni1 S1 2.2065(14) . ?
S2 C1 1.723(6) . ?
S1 C1 1.729(6) . ?
F1S C2S 1.341(7) . ?
F2S C4S 1.350(7) . ?
F3S C6S 1.350(8) . ?
N1 C1 1.309(8) . ?
N1 C2 1.473(8) . ?
N1 C4 1.478(8) . ?
C5S C4S 1.386(9) . ?
C5S C6S 1.386(10) . ?
C2S C1S 1.384(9) . ?
C2S C3S 1.391(9) . ?
C1S C6S 1.370(11) . ?
C3S C4S 1.379(9) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.530(9) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.505(9) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 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
S2 Ni1 S2 180.0 . 2_675 ?
S1 Ni1 S2 100.78(5) . 2_675 ?
S1 Ni1 S2 100.78(5) 2_675 . ?
S1 Ni1 S2 79.22(5) 2_675 2_675 ?
S1 Ni1 S2 79.22(5) . . ?
S1 Ni1 S1 180.0 . 2_675 ?
C1 S2 Ni1 85.6(2) . . ?
C1 S1 Ni1 85.7(2) . . ?
C1 N1 C2 121.6(5) . . ?
C1 N1 C4 121.0(5) . . ?
C2 N1 C4 117.1(5) . . ?
C4S C5S I3S 121.5(5) . . ?
C4S C5S C6S 116.8(6) . . ?
C6S C5S I3S 121.6(5) . . ?
F1S C2S C1S 119.4(6) . . ?
F1S C2S C3S 118.7(6) . . ?
C1S C2S C3S 121.8(6) . . ?
C2S C1S I1S 120.8(5) . . ?
C6S C1S I1S 121.2(5) . . ?
C6S C1S C2S 118.0(6) . . ?
C2S C3S I2S 122.1(5) . . ?
C4S C3S I2S 120.4(5) . . ?
C4S C3S C2S 117.5(6) . . ?
F2S C4S C5S 118.2(6) . . ?
F2S C4S C3S 118.9(6) . . ?
C3S C4S C5S 122.8(6) . . ?
S2 C1 S1 109.4(3) . . ?
N1 C1 S2 126.0(5) . . ?
N1 C1 S1 124.6(4) . . ?
N1 C2 H2A 109.3 . . ?
N1 C2 H2B 109.3 . . ?
N1 C2 C3 111.7(5) . . ?
H2A C2 H2B 107.9 . . ?
C3 C2 H2A 109.3 . . ?
C3 C2 H2B 109.3 . . ?
F3S C6S C5S 118.3(7) . . ?
F3S C6S C1S 118.7(7) . . ?
C1S C6S C5S 123.0(6) . . ?
N1 C4 H4A 108.9 . . ?
N1 C4 H4B 108.9 . . ?
N1 C4 C5 113.2(5) . . ?
H4A C4 H4B 107.8 . . ?
C5 C4 H4A 108.9 . . ?
C5 C4 H4B 108.9 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?

# start Validation Reply Form
_vrf_PLAT431_13229_m150          
;
PROBLEM: Short Inter HL..A Contact  I2S      ..S2       .       3.41 Ang.  
RESPONSE: Short contact is the investigated feature of this structure.
;
# end Validation Reply Form

_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 4.364
_oxdiff_exptl_absorpt_empirical_full_min 0.530
