# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 2048855'
loop_
_audit_author_name
_audit_author_address
'Narcis Avarvari'
;CNRS, University of Angers
France
;
_audit_update_record             
;
2020-12-07 deposited with the CCDC.	2021-02-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H8 S5'
_chemical_formula_sum            'C7 H8 S5'
_chemical_formula_weight         252.43

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'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   7.4413(2)
_cell_length_b                   15.6747(4)
_cell_length_c                   8.6991(2)
_cell_angle_alpha                90
_cell_angle_beta                 92.916(2)
_cell_angle_gamma                90
_cell_volume                     1013.35(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.0(3)
_cell_measurement_reflns_used    4510
_cell_measurement_theta_min      5.0780
_cell_measurement_theta_max      73.1580

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_F_000             520
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    10.060
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.55344
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.677
_oxdiff_exptl_absorpt_empirical_full_max 1.518
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150.0(3)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_reflns_number            6956
_diffrn_reflns_av_unetI/netI     0.0629
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         5.091
_diffrn_reflns_theta_max         73.592
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_point_group_measured_fraction_full 0.984
_reflns_number_total             3887
_reflns_number_gt                3670
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.869
_reflns_Friedel_fraction_max     0.921
_reflns_Friedel_fraction_full    0.967

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

_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0819P)²+0.2242P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1568 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.07(5)
_chemical_absolute_configuration syn
_refine_ls_number_reflns         3887
_refine_ls_number_parameters     217
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0449
_refine_ls_wR_factor_ref         0.1378
_refine_ls_wR_factor_gt          0.1246
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5643(11) 0.8447(5) -0.2877(9) 0.0280(16) Uani 1 1 d . . . . .
H1 H 0.548576 0.898845 -0.343013 0.034 Uiso 1 1 calc R U . . .
C2 C 0.4086(11) 0.7869(5) -0.3462(9) 0.0284(16) Uani 1 1 d . . . . .
H2 H 0.413199 0.785251 -0.458539 0.034 Uiso 1 1 calc R U . . .
C3 C 0.5516(9) 0.7654(4) -0.0110(8) 0.0204(14) Uani 1 1 d . . . . .
C4 C 0.5056(9) 0.6934(5) -0.0862(9) 0.0253(16) Uani 1 1 d . . . . .
C5 C 0.5833(10) 0.6453(6) 0.1996(10) 0.0287(17) Uani 1 1 d . . . . .
C6 C 0.7491(10) 0.8104(5) -0.3274(10) 0.0294(16) Uani 1 1 d . . . . .
H6A H 0.841052 0.848799 -0.288367 0.044 Uiso 1 1 calc R U . . .
H6B H 0.767507 0.755227 -0.281523 0.044 Uiso 1 1 calc R U . . .
H6C H 0.754418 0.805864 -0.437096 0.044 Uiso 1 1 calc R U . . .
C7 C 0.2247(11) 0.8216(6) -0.3122(11) 0.0341(18) Uani 1 1 d . . . . .
H7A H 0.133442 0.782836 -0.351360 0.051 Uiso 1 1 calc R U . . .
H7B H 0.216265 0.827645 -0.203012 0.051 Uiso 1 1 calc R U . . .
H7C H 0.207746 0.876175 -0.360788 0.051 Uiso 1 1 calc R U . . .
C8 C 0.0057(10) 0.4938(4) -0.3789(9) 0.0221(14) Uani 1 1 d . . . . .
H8 H -0.039243 0.492215 -0.486747 0.026 Uiso 1 1 calc R U . . .
C9 C -0.0951(11) 0.4232(5) -0.2963(8) 0.0244(15) Uani 1 1 d . . . . .
H9 H -0.076362 0.370562 -0.354024 0.029 Uiso 1 1 calc R U . . .
C10 C 0.0014(9) 0.5826(4) -0.1102(8) 0.0169(12) Uani 1 1 d . . . . .
C11 C 0.0178(10) 0.5093(5) -0.0330(9) 0.0264(16) Uani 1 1 d . . . . .
C12 C 0.0692(10) 0.6293(5) 0.1764(9) 0.0234(15) Uani 1 1 d . . . . .
C13 C 0.2075(11) 0.4806(5) -0.3802(10) 0.0310(17) Uani 1 1 d . . . . .
H13A H 0.260789 0.527003 -0.433618 0.046 Uiso 1 1 calc R U . . .
H13B H 0.257360 0.478339 -0.276355 0.046 Uiso 1 1 calc R U . . .
H13C H 0.232029 0.427940 -0.431603 0.046 Uiso 1 1 calc R U . . .
C14 C -0.2978(11) 0.4367(6) -0.2970(10) 0.0333(18) Uani 1 1 d . . . . .
H14A H -0.351991 0.390518 -0.243685 0.050 Uiso 1 1 calc R U . . .
H14B H -0.322842 0.489546 -0.246441 0.050 Uiso 1 1 calc R U . . .
H14C H -0.346339 0.438672 -0.401313 0.050 Uiso 1 1 calc R U . . .
S1 S 0.5540(3) 0.86984(11) -0.0847(2) 0.0258(4) Uani 1 1 d . . . . .
S2 S 0.4419(2) 0.67754(12) -0.2795(2) 0.0266(4) Uani 1 1 d . . . . .
S3 S 0.6176(3) 0.75398(12) 0.1844(2) 0.0264(4) Uani 1 1 d . . . . .
S4 S 0.5164(3) 0.60008(11) 0.0233(2) 0.0256(4) Uani 1 1 d . . . . .
S5 S 0.6103(3) 0.59167(15) 0.3604(2) 0.0370(5) Uani 1 1 d . . . . .
S6 S -0.0514(2) 0.59940(11) -0.30667(19) 0.0222(4) Uani 1 1 d . . . . .
S7 S 0.0017(3) 0.40484(12) -0.1024(2) 0.0307(4) Uani 1 1 d . . . . .
S8 S 0.0274(2) 0.67653(10) -0.0019(2) 0.0217(4) Uani 1 1 d . . . . .
S9 S 0.0672(3) 0.51963(12) 0.1657(2) 0.0274(4) Uani 1 1 d . . . . .
S10 S 0.1084(3) 0.68266(13) 0.3371(2) 0.0306(4) 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
C1 C6 1.531(11) . ?
C1 C2 1.537(11) . ?
C1 S1 1.815(8) . ?
C2 C7 1.516(11) . ?
C2 S2 1.822(8) . ?
C3 C4 1.341(11) . ?
C3 S3 1.754(7) . ?
C3 S1 1.758(7) . ?
C4 S2 1.742(8) . ?
C4 S4 1.745(8) . ?
C5 S5 1.635(8) . ?
C5 S3 1.729(9) . ?
C5 S4 1.739(9) . ?
C8 C13 1.517(11) . ?
C8 C9 1.536(10) . ?
C8 S6 1.828(7) . ?
C9 C14 1.523(12) . ?
C9 S7 1.822(7) . ?
C10 C11 1.333(11) . ?
C10 S8 1.754(7) . ?
C10 S6 1.754(7) . ?
C11 S7 1.748(9) . ?
C11 S9 1.756(8) . ?
C12 S10 1.642(8) . ?
C12 S9 1.722(8) . ?
C12 S8 1.733(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 C1 C2 112.9(7) . . ?
C6 C1 S1 112.2(6) . . ?
C2 C1 S1 112.4(6) . . ?
C7 C2 C1 113.4(7) . . ?
C7 C2 S2 112.6(6) . . ?
C1 C2 S2 111.2(5) . . ?
C4 C3 S3 116.0(6) . . ?
C4 C3 S1 127.8(6) . . ?
S3 C3 S1 116.2(4) . . ?
C3 C4 S2 129.9(6) . . ?
C3 C4 S4 115.9(6) . . ?
S2 C4 S4 114.2(5) . . ?
S5 C5 S3 124.0(5) . . ?
S5 C5 S4 124.2(6) . . ?
S3 C5 S4 111.7(5) . . ?
C13 C8 C9 114.3(6) . . ?
C13 C8 S6 112.0(5) . . ?
C9 C8 S6 111.3(5) . . ?
C14 C9 C8 113.9(6) . . ?
C14 C9 S7 111.7(5) . . ?
C8 C9 S7 111.6(5) . . ?
C11 C10 S8 116.6(5) . . ?
C11 C10 S6 129.1(5) . . ?
S8 C10 S6 114.2(4) . . ?
C10 C11 S7 129.1(6) . . ?
C10 C11 S9 115.2(6) . . ?
S7 C11 S9 115.7(5) . . ?
S10 C12 S9 123.7(5) . . ?
S10 C12 S8 124.1(5) . . ?
S9 C12 S8 112.2(4) . . ?
C3 S1 C1 98.9(3) . . ?
C4 S2 C2 101.5(4) . . ?
C5 S3 C3 98.1(4) . . ?
C5 S4 C4 98.2(4) . . ?
C10 S6 C8 98.9(3) . . ?
C11 S7 C9 100.9(4) . . ?
C12 S8 C10 97.6(4) . . ?
C12 S9 C11 98.4(4) . . ?

_refine_diff_density_max         0.495
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.113

####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2048859'
loop_
_audit_author_name
_audit_author_address
'Narcis Avarvari'
;CNRS, University of Angers
France
;
_audit_update_record             
;
2020-12-07 deposited with the CCDC.	2021-02-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H48 N Ni S8'
_chemical_formula_sum            'C26 H48 N Ni S8'
_chemical_formula_weight         689.84

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'
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'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_H-M_alt        'P 1'
_space_group_name_Hall           'P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'

_cell_length_a                   9.3629(7)
_cell_length_b                   13.5340(7)
_cell_length_c                   13.7348(7)
_cell_angle_alpha                83.774(4)
_cell_angle_beta                 77.788(5)
_cell_angle_gamma                87.427(5)
_cell_volume                     1690.59(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    150.01(10)
_cell_measurement_reflns_used    6029
_cell_measurement_theta_min      3.2530
_cell_measurement_theta_max      72.9880

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_F_000             734
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    5.567
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.62421
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.689
_oxdiff_exptl_absorpt_empirical_full_max 1.651
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150.01(10)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_reflns_number            27719
_diffrn_reflns_av_unetI/netI     0.0693
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.286
_diffrn_reflns_theta_max         74.116
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_point_group_measured_fraction_full 0.950
_reflns_number_total             12475
_reflns_number_gt                8028
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.878
_reflns_Friedel_fraction_max     0.848
_reflns_Friedel_fraction_full    0.907

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

_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1024P)²+1.1256P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2642 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.12(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         12475
_refine_ls_number_parameters     649
_refine_ls_number_restraints     78
_refine_ls_R_factor_all          0.1120
_refine_ls_R_factor_gt           0.0744
_refine_ls_wR_factor_ref         0.2255
_refine_ls_wR_factor_gt          0.1935
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.173
_refine_ls_shift/su_mean         0.018

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
C3 C 0.927(3) 0.1064(14) 0.1288(16) 0.099(7) Uani 1 1 d . . . . .
C4 C 0.788(2) 0.1557(11) 0.1368(13) 0.071(4) Uani 1 1 d . . . . .
C5 C 1.0981(18) 0.3783(11) 0.3952(11) 0.064(4) Uani 1 1 d . . . . .
C6 C 0.9818(18) 0.4303(13) 0.3978(14) 0.074(4) Uani 1 1 d . . . . .
C13 C 1.2592(19) 0.6448(11) 0.7150(12) 0.068(4) Uani 1 1 d . . . . .
C14 C 1.2681(18) 0.7153(11) 0.6395(12) 0.065(4) Uani 1 1 d . . . . .
C15 C 0.659(2) 0.8048(11) 0.8880(14) 0.075(5) Uani 1 1 d . . . . .
C16 C 0.6729(17) 0.8753(12) 0.8088(13) 0.069(4) Uani 1 1 d . . . . .
C21 C 0.5388(18) 0.4869(13) 0.9775(12) 0.069(4) Uani 1 1 d . . . . .
H21A H 0.511052 0.486676 0.913398 0.083 Uiso 1 1 calc R U . . .
H21B H 0.563967 0.554304 0.983837 0.083 Uiso 1 1 calc R U . . .
C22 C 0.6719(19) 0.4198(15) 0.9789(14) 0.090(6) Uani 1 1 d . . . . .
H22A H 0.706028 0.425563 1.039967 0.108 Uiso 1 1 calc R U . . .
H22B H 0.644226 0.351461 0.979873 0.108 Uiso 1 1 calc R U . . .
C23 C 0.790(2) 0.4429(15) 0.8939(17) 0.100(7) Uani 1 1 d . . . . .
H23A H 0.817373 0.511553 0.891597 0.120 Uiso 1 1 calc R U . . .
H23B H 0.758265 0.434772 0.832600 0.120 Uiso 1 1 calc R U . . .
C24 C 0.921(2) 0.3751(17) 0.9016(17) 0.112(8) Uani 1 1 d . . . . .
H24A H 0.998860 0.391272 0.844754 0.169 Uiso 1 1 calc R U . . .
H24B H 0.953633 0.383877 0.961872 0.169 Uiso 1 1 calc R U . . .
H24C H 0.894634 0.307238 0.902984 0.169 Uiso 1 1 calc R U . . .
C25 C 0.362(2) 0.3522(11) 1.0626(13) 0.077(5) Uani 1 1 d . . . . .
H25A H 0.444367 0.307903 1.070598 0.092 Uiso 1 1 calc R U . . .
H25B H 0.284657 0.337809 1.120935 0.092 Uiso 1 1 calc R U . . .
C26 C 0.311(2) 0.3296(13) 0.9735(17) 0.096(6) Uani 1 1 d . . . . .
H26A H 0.208615 0.349200 0.982045 0.115 Uiso 1 1 calc R U . . .
H26B H 0.363772 0.370945 0.916203 0.115 Uiso 1 1 calc R U . . .
C27 C 0.326(4) 0.2254(19) 0.949(2) 0.140(10) Uani 1 1 d . . . . .
H27A H 0.428341 0.204697 0.939622 0.168 Uiso 1 1 calc R U . . .
H27B H 0.272056 0.183049 1.005148 0.168 Uiso 1 1 calc R U . . .
C28 C 0.273(3) 0.2132(17) 0.860(2) 0.139(11) Uani 1 1 d . . . . .
H28A H 0.284401 0.144805 0.846543 0.209 Uiso 1 1 calc R U . . .
H28B H 0.171319 0.232501 0.869726 0.209 Uiso 1 1 calc R U . . .
H28C H 0.327490 0.254134 0.804247 0.209 Uiso 1 1 calc R U . . .
C29 C 0.2844(18) 0.5291(11) 1.0474(11) 0.066(4) Uani 1 1 d . . . . .
H29A H 0.268019 0.528114 0.980145 0.079 Uiso 1 1 calc R U . . .
H29B H 0.315376 0.595351 1.052918 0.079 Uiso 1 1 calc R U . . .
C30 C 0.1395(18) 0.5106(11) 1.1210(12) 0.075(4) Uani 1 1 d . . . . .
H30A H 0.100170 0.448884 1.109236 0.090 Uiso 1 1 calc R U . . .
H30B H 0.156717 0.502955 1.188630 0.090 Uiso 1 1 calc R U . . .
C31 C 0.031(2) 0.5914(14) 1.1124(17) 0.094(6) Uani 1 1 d . . . . .
H31A H -0.064182 0.567773 1.147595 0.112 Uiso 1 1 calc R U . . .
H31B H 0.027130 0.606179 1.042323 0.112 Uiso 1 1 calc R U . . .
C32 C 0.059(3) 0.6876(19) 1.153(3) 0.164(13) Uani 1 1 d . . . . .
H32A H -0.017242 0.735469 1.143963 0.245 Uiso 1 1 calc R U . . .
H32B H 0.059965 0.674681 1.222838 0.245 Uiso 1 1 calc R U . . .
H32C H 0.151500 0.713180 1.117308 0.245 Uiso 1 1 calc R U . . .
C33 C 0.446(2) 0.4632(13) 1.1663(11) 0.089(6) Uani 1 1 d . . . . .
H33A H 0.361610 0.444193 1.218418 0.107 Uiso 1 1 calc R U . . .
H33B H 0.525600 0.416927 1.174680 0.107 Uiso 1 1 calc R U . . .
C34 C 0.489(3) 0.5678(15) 1.1775(14) 0.094(6) Uani 1 1 d . . . . .
H34A H 0.555204 0.594066 1.116783 0.113 Uiso 1 1 calc R U . . .
H34B H 0.403039 0.610911 1.188035 0.113 Uiso 1 1 calc R U . . .
C35 C 0.561(2) 0.5658(15) 1.2627(16) 0.103(6) Uani 1 1 d . . . . .
H35A H 0.639277 0.515741 1.255976 0.124 Uiso 1 1 calc R U . . .
H35B H 0.491077 0.546741 1.323946 0.124 Uiso 1 1 calc R U . . .
C36 C 0.622(3) 0.662(2) 1.2702(19) 0.127(9) Uani 1 1 d . . . . .
H36A H 0.668104 0.657061 1.326920 0.191 Uiso 1 1 calc R U . . .
H36B H 0.693503 0.680809 1.210346 0.191 Uiso 1 1 calc R U . . .
H36C H 0.545302 0.711809 1.278316 0.191 Uiso 1 1 calc R U . . .
C37 C 0.541(2) 1.1779(12) 1.4775(13) 0.074(4) Uani 1 1 d . . . . .
H37A H 0.622646 1.195396 1.422657 0.089 Uiso 1 1 calc R U . . .
H37B H 0.460586 1.223496 1.469177 0.089 Uiso 1 1 calc R U . . .
C38 C 0.585(3) 1.1938(13) 1.5754(15) 0.094(6) Uani 1 1 d . . . . .
H38A H 0.518453 1.157817 1.630073 0.112 Uiso 1 1 calc R U . . .
H38B H 0.682081 1.164537 1.574113 0.112 Uiso 1 1 calc R U . . .
C39 C 0.587(4) 1.2928(16) 1.596(2) 0.175(16) Uani 1 1 d . . . . .
H39A H 0.488509 1.320292 1.600296 0.210 Uiso 1 1 calc R U . . .
H39B H 0.648653 1.329001 1.538849 0.210 Uiso 1 1 calc R U . . .
C40 C 0.638(3) 1.3149(17) 1.6893(17) 0.116(8) Uani 1 1 d . . . . .
H40A H 0.632885 1.385364 1.693572 0.174 Uiso 1 1 calc R U . . .
H40B H 0.575616 1.282291 1.747535 0.174 Uiso 1 1 calc R U . . .
H40C H 0.736556 1.291044 1.685782 0.174 Uiso 1 1 calc R U . . .
C41 C 0.3671(17) 1.0460(10) 1.5561(11) 0.059(4) Uani 1 1 d . . . . .
H41A H 0.351033 0.975121 1.561566 0.071 Uiso 1 1 calc R U . . .
H41B H 0.394824 1.060169 1.617254 0.071 Uiso 1 1 calc R U . . .
C42 C 0.226(2) 1.0995(16) 1.5500(16) 0.097(7) Uani 1 1 d . . . . .
H42A H 0.247322 1.168165 1.525020 0.117 Uiso 1 1 calc R U . . .
H42B H 0.184665 1.070891 1.500570 0.117 Uiso 1 1 calc R U . . .
C43 C 0.115(2) 1.0989(14) 1.6414(12) 0.080(5) Uani 1 1 d . . . . .
H43A H 0.157530 1.126420 1.690719 0.096 Uiso 1 1 calc R U . . .
H43B H 0.093977 1.029972 1.665746 0.096 Uiso 1 1 calc R U . . .
C44 C -0.029(2) 1.1520(14) 1.640(2) 0.111(8) Uani 1 1 d . . . . .
H44A H -0.089395 1.144387 1.706410 0.166 Uiso 1 1 calc R U . . .
H44B H -0.012483 1.221331 1.619671 0.166 Uiso 1 1 calc R U . . .
H44C H -0.076412 1.124313 1.594550 0.166 Uiso 1 1 calc R U . . .
C45 C 0.4496(18) 1.0662(12) 1.3728(11) 0.066(4) Uani 1 1 d . . . . .
H45A H 0.530489 1.088121 1.319177 0.080 Uiso 1 1 calc R U . . .
H45B H 0.369246 1.113415 1.369743 0.080 Uiso 1 1 calc R U . . .
C46 C 0.402(2) 0.9648(13) 1.3518(13) 0.085(6) Uani 1 1 d . . . . .
H46A H 0.488090 0.922187 1.335279 0.102 Uiso 1 1 calc R U . . .
H46B H 0.340119 0.933881 1.412131 0.102 Uiso 1 1 calc R U . . .
C47 C 0.321(2) 0.972(2) 1.2684(16) 0.123(9) Uani 1 1 d . . . . .
H47A H 0.382258 1.005245 1.208794 0.148 Uiso 1 1 calc R U . . .
H47B H 0.233855 1.012976 1.286046 0.148 Uiso 1 1 calc R U . . .
C48 C 0.276(3) 0.867(2) 1.2434(17) 0.116(7) Uani 1 1 d . . . . .
H48A H 0.224967 0.876325 1.189438 0.174 Uiso 1 1 calc R U . . .
H48B H 0.362531 0.826386 1.224302 0.174 Uiso 1 1 calc R U . . .
H48C H 0.214042 0.834122 1.301599 0.174 Uiso 1 1 calc R U . . .
C49 C 0.6167(16) 0.9968(10) 1.4815(12) 0.067(4) Uani 1 1 d . . . . .
H49A H 0.585633 0.931121 1.474109 0.080 Uiso 1 1 calc R U . . .
H49B H 0.633430 0.995963 1.548891 0.080 Uiso 1 1 calc R U . . .
C50 C 0.761(2) 1.0180(15) 1.4072(16) 0.117(9) Uani 1 1 d . . . . .
H50A H 0.794166 1.082895 1.415596 0.140 Uiso 1 1 calc R U . . .
H50B H 0.744597 1.020278 1.339581 0.140 Uiso 1 1 calc R U . . .
C51 C 0.882(2) 0.9401(12) 1.4201(13) 0.084(5) Uani 1 1 d . . . . .
H51A H 0.975209 0.964185 1.382173 0.101 Uiso 1 1 calc R U . . .
H51B H 0.887392 0.928783 1.490132 0.101 Uiso 1 1 calc R U . . .
C52 C 0.850(3) 0.8491(19) 1.386(3) 0.180(15) Uani 1 1 d . . . . .
H52A H 0.925611 0.800550 1.393875 0.270 Uiso 1 1 calc R U . . .
H52B H 0.757842 0.825221 1.423869 0.270 Uiso 1 1 calc R U . . .
H52C H 0.845443 0.860536 1.316177 0.270 Uiso 1 1 calc R U . . .
N1 N 0.4081(15) 0.4561(8) 1.0609(8) 0.063(3) Uani 1 1 d . . . . .
N2 N 0.4946(13) 1.0709(9) 1.4691(10) 0.062(3) Uani 1 1 d . . . . .
S1 S 0.9777(11) 0.0002(6) 0.0674(8) 0.181(5) Uani 1 1 d . . . . .
S2 S 0.6420(6) 0.1286(3) 0.0837(4) 0.0902(15) Uani 1 1 d . . . . .
S3 S 1.0500(5) 0.1424(4) 0.1920(4) 0.0884(15) Uani 1 1 d . . . . .
S4 S 0.7573(4) 0.2554(3) 0.2052(3) 0.0631(9) Uani 1 1 d . . . . .
S5 S 1.1366(4) 0.2731(3) 0.3292(3) 0.0601(9) Uani 1 1 d . . . . .
S6 S 0.8490(5) 0.3925(3) 0.3367(3) 0.0776(12) Uani 1 1 d . . . . .
S7 S 1.2483(5) 0.4014(3) 0.4509(4) 0.0745(11) Uani 1 1 d . . . . .
S8 S 0.9226(7) 0.5386(5) 0.4558(6) 0.127(2) Uani 1 1 d . . . . .
S9 S 1.3817(6) 0.5473(3) 0.7306(4) 0.0890(13) Uani 1 1 d . . . . .
S10 S 1.4161(6) 0.7287(4) 0.5334(5) 0.115(2) Uani 1 1 d . . . . .
S11 S 1.0980(6) 0.6405(3) 0.8081(3) 0.0884(15) Uani 1 1 d . . . . .
S12 S 1.1266(5) 0.8024(3) 0.6325(4) 0.0803(12) Uani 1 1 d . . . . .
S13 S 0.8004(6) 0.7233(3) 0.8977(3) 0.0866(15) Uani 1 1 d . . . . .
S14 S 0.8273(5) 0.8802(3) 0.7153(3) 0.0800(12) Uani 1 1 d . . . . .
S15 S 0.5042(7) 0.7904(3) 0.9851(4) 0.1033(18) Uani 1 1 d . . . . .
S16 S 0.5330(6) 0.9628(6) 0.7896(4) 0.125(2) Uani 1 1 d . . . . .
NI1 Ni 0.9484(3) 0.2649(2) 0.2661(2) 0.0554(4) Uani 1 1 d . . . . .
NI2 Ni 0.9629(4) 0.7626(2) 0.7638(2) 0.0626(5) Uani 1 1 d . . . . .
C1 C 0.839(2) -0.0102(15) -0.0052(15) 0.103(5) Uani 1 1 d D U . . .
H1 H 0.847689 -0.076927 -0.027549 0.123 Uiso 1 1 calc R U . . .
C2 C 0.693(2) 0.0060(14) 0.0444(16) 0.112(6) Uani 1 1 d . U . . .
H2A H 0.672099 -0.041762 0.103224 0.135 Uiso 1 1 calc R U . . .
H2B H 0.629771 -0.008620 0.000348 0.135 Uiso 1 1 calc R U . . .
C7 C 1.160(2) 0.4931(13) 0.5366(12) 0.093(5) Uani 1 1 d . U . . .
H7 H 1.239701 0.517404 0.563480 0.112 Uiso 1 1 calc R U . . .
C8 C 1.103(3) 0.5875(16) 0.4752(18) 0.133(7) Uani 1 1 d . U . . .
H8A H 1.170139 0.604688 0.411940 0.159 Uiso 1 1 calc R U . . .
H8B H 1.086927 0.644643 0.513410 0.159 Uiso 1 1 calc R U . . .
C9 C 0.858(5) 0.068(3) -0.101(2) 0.25(2) Uani 1 1 d D U . . .
H9A H 0.955406 0.062849 -0.140294 0.380 Uiso 1 1 calc R U . . .
H9B H 0.788992 0.055139 -0.140758 0.380 Uiso 1 1 calc R U . . .
H9C H 0.840614 0.134059 -0.080820 0.380 Uiso 1 1 calc R U . . .
C10 C 1.060(2) 0.4443(17) 0.6236(13) 0.114(7) Uani 1 1 d . U . . .
H10A H 1.110060 0.388911 0.652786 0.171 Uiso 1 1 calc R U . . .
H10B H 1.028557 0.490901 0.672151 0.171 Uiso 1 1 calc R U . . .
H10C H 0.977251 0.421243 0.602745 0.171 Uiso 1 1 calc R U . . .
C11 C 1.555(2) 0.5904(15) 0.6438(15) 0.108(5) Uani 1 1 d . U . . .
H11 H 1.632965 0.540362 0.647886 0.130 Uiso 1 1 calc R U . . .
C12 C 1.537(3) 0.612(2) 0.5323(19) 0.157(9) Uani 1 1 d . U . . .
H12A H 1.490697 0.557390 0.512027 0.188 Uiso 1 1 calc R U . . .
H12B H 1.630912 0.623658 0.487331 0.188 Uiso 1 1 calc R U . . .
C17 C 0.354(3) 0.859(2) 0.948(2) 0.161(10) Uani 1 1 d D U . . .
H17A H 0.263830 0.825062 0.978064 0.193 Uiso 1 1 calc R U . . .
H17B H 0.348148 0.924562 0.969938 0.193 Uiso 1 1 calc R U . . .
C18 C 0.377(3) 0.865(2) 0.841(2) 0.155(9) Uani 1 1 d D U . . .
H18 H 0.390678 0.801842 0.811062 0.186 Uiso 1 1 calc R U . . .
C19 C 1.606(4) 0.686(2) 0.653(3) 0.230(16) Uani 1 1 d . U . . .
H19A H 1.623934 0.687798 0.719376 0.344 Uiso 1 1 calc R U . . .
H19B H 1.694943 0.699460 0.604767 0.344 Uiso 1 1 calc R U . . .
H19C H 1.533351 0.736159 0.642004 0.344 Uiso 1 1 calc R U . . .
C20 C 0.218(3) 0.917(3) 0.848(2) 0.215(15) Uani 1 1 d D U . . .
H20A H 0.199207 0.931740 0.781554 0.323 Uiso 1 1 calc R U . . .
H20B H 0.145635 0.872402 0.886622 0.323 Uiso 1 1 calc R U . . .
H20C H 0.214546 0.977128 0.879019 0.323 Uiso 1 1 calc R U . . .


_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
C3 C4 1.42(3) . ?
C3 S3 1.70(2) . ?
C3 S1 1.742(18) . ?
C4 S4 1.706(17) . ?
C4 S2 1.751(18) . ?
C5 C6 1.27(2) . ?
C5 S5 1.753(15) . ?
C5 S7 1.790(17) . ?
C6 S8 1.756(17) . ?
C6 S6 1.762(17) . ?
C13 C14 1.32(2) . ?
C13 S9 1.736(15) . ?
C13 S11 1.758(19) . ?
C14 S12 1.744(16) . ?
C14 S10 1.785(18) . ?
C15 C16 1.35(2) . ?
C15 S13 1.705(18) . ?
C15 S15 1.750(19) . ?
C16 S14 1.717(17) . ?
C16 S16 1.769(17) . ?
C21 C22 1.51(2) . ?
C21 N1 1.53(2) . ?
C22 C23 1.45(3) . ?
C23 C24 1.51(2) . ?
C25 C26 1.47(3) . ?
C25 N1 1.485(19) . ?
C26 C27 1.48(3) . ?
C27 C28 1.45(3) . ?
C29 N1 1.516(18) . ?
C29 C30 1.52(2) . ?
C30 C31 1.47(2) . ?
C31 C32 1.52(3) . ?
C33 C34 1.52(3) . ?
C33 N1 1.58(2) . ?
C34 C35 1.46(3) . ?
C35 C36 1.47(3) . ?
C37 C38 1.53(3) . ?
C37 N2 1.55(2) . ?
C38 C39 1.40(3) . ?
C39 C40 1.52(3) . ?
C41 C42 1.49(2) . ?
C41 N2 1.521(19) . ?
C42 C43 1.45(2) . ?
C43 C44 1.50(2) . ?
C45 N2 1.48(2) . ?
C45 C46 1.54(2) . ?
C46 C47 1.49(3) . ?
C47 C48 1.60(3) . ?
C49 N2 1.512(16) . ?
C49 C50 1.53(2) . ?
C50 C51 1.53(2) . ?
C51 C52 1.43(3) . ?
S1 C1 1.814(19) . ?
S2 C2 1.813(19) . ?
S3 NI1 2.122(5) . ?
S4 NI1 2.144(5) . ?
S5 NI1 2.134(5) . ?
S6 NI1 2.151(5) . ?
S7 C7 1.849(17) . ?
S8 C8 1.92(2) . ?
S9 C11 1.87(2) . ?
S10 C12 1.90(3) . ?
S11 NI2 2.149(5) . ?
S12 NI2 2.141(6) . ?
S13 NI2 2.158(6) . ?
S14 NI2 2.130(5) . ?
S15 C17 1.78(3) . ?
S16 C18 1.98(3) . ?
C1 C2 1.42(3) . ?
C1 C9 1.58(2) . ?
C7 C10 1.47(2) . ?
C7 C8 1.59(3) . ?
C11 C19 1.43(3) . ?
C11 C12 1.57(3) . ?
C17 C18 1.44(3) . ?
C18 C20 1.60(2) . ?

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
C4 C3 S3 120.2(13) . . ?
C4 C3 S1 124.5(16) . . ?
S3 C3 S1 115.0(13) . . ?
C3 C4 S4 117.2(13) . . ?
C3 C4 S2 128.4(14) . . ?
S4 C4 S2 114.4(9) . . ?
C6 C5 S5 123.0(13) . . ?
C6 C5 S7 126.9(12) . . ?
S5 C5 S7 110.1(9) . . ?
C5 C6 S8 130.9(14) . . ?
C5 C6 S6 118.6(13) . . ?
S8 C6 S6 110.6(9) . . ?
C14 C13 S9 128.2(14) . . ?
C14 C13 S11 117.7(12) . . ?
S9 C13 S11 113.9(9) . . ?
C13 C14 S12 121.5(13) . . ?
C13 C14 S10 125.2(13) . . ?
S12 C14 S10 113.2(9) . . ?
C16 C15 S13 119.3(14) . . ?
C16 C15 S15 125.0(14) . . ?
S13 C15 S15 115.7(10) . . ?
C15 C16 S14 121.2(14) . . ?
C15 C16 S16 123.4(14) . . ?
S14 C16 S16 115.2(10) . . ?
C22 C21 N1 113.4(12) . . ?
C23 C22 C21 113.2(14) . . ?
C22 C23 C24 110.4(16) . . ?
C26 C25 N1 115.4(14) . . ?
C27 C26 C25 117.2(18) . . ?
C28 C27 C26 112(2) . . ?
N1 C29 C30 115.9(13) . . ?
C31 C30 C29 112.8(15) . . ?
C30 C31 C32 116(2) . . ?
C34 C33 N1 111.7(12) . . ?
C35 C34 C33 109.9(16) . . ?
C34 C35 C36 112.7(19) . . ?
C38 C37 N2 115.6(13) . . ?
C39 C38 C37 115.8(18) . . ?
C38 C39 C40 118.8(19) . . ?
C42 C41 N2 116.1(12) . . ?
C43 C42 C41 117.5(16) . . ?
C42 C43 C44 120.0(16) . . ?
N2 C45 C46 117.0(13) . . ?
C47 C46 C45 112.9(17) . . ?
C46 C47 C48 113(2) . . ?
N2 C49 C50 114.4(12) . . ?
C49 C50 C51 113.1(14) . . ?
C52 C51 C50 110(2) . . ?
C25 N1 C29 110.9(13) . . ?
C25 N1 C21 114.4(12) . . ?
C29 N1 C21 106.6(11) . . ?
C25 N1 C33 105.5(12) . . ?
C29 N1 C33 109.2(11) . . ?
C21 N1 C33 110.2(14) . . ?
C45 N2 C49 111.5(12) . . ?
C45 N2 C41 110.3(13) . . ?
C49 N2 C41 107.1(11) . . ?
C45 N2 C37 110.4(12) . . ?
C49 N2 C37 110.5(12) . . ?
C41 N2 C37 107.0(11) . . ?
C3 S1 C1 104.8(10) . . ?
C4 S2 C2 102.4(9) . . ?
C3 S3 NI1 105.2(7) . . ?
C4 S4 NI1 105.7(6) . . ?
C5 S5 NI1 102.9(6) . . ?
C6 S6 NI1 104.0(6) . . ?
C5 S7 C7 99.7(8) . . ?
C6 S8 C8 101.9(9) . . ?
C13 S9 C11 103.1(9) . . ?
C14 S10 C12 109.1(10) . . ?
C13 S11 NI2 105.5(5) . . ?
C14 S12 NI2 104.5(6) . . ?
C15 S13 NI2 104.1(7) . . ?
C16 S14 NI2 103.6(6) . . ?
C15 S15 C17 109.3(11) . . ?
C16 S16 C18 93.0(10) . . ?
S3 NI1 S5 88.6(2) . . ?
S3 NI1 S4 91.6(2) . . ?
S5 NI1 S4 178.9(3) . . ?
S3 NI1 S6 178.0(3) . . ?
S5 NI1 S6 91.4(2) . . ?
S4 NI1 S6 88.43(19) . . ?
S14 NI2 S12 88.6(2) . . ?
S14 NI2 S11 177.7(3) . . ?
S12 NI2 S11 90.7(2) . . ?
S14 NI2 S13 91.8(2) . . ?
S12 NI2 S13 179.0(3) . . ?
S11 NI2 S13 88.9(2) . . ?
C2 C1 C9 103(2) . . ?
C2 C1 S1 116.2(14) . . ?
C9 C1 S1 113(2) . . ?
C1 C2 S2 117.6(14) . . ?
C10 C7 C8 119.0(19) . . ?
C10 C7 S7 110.8(13) . . ?
C8 C7 S7 110.3(12) . . ?
C7 C8 S8 100.5(15) . . ?
C19 C11 C12 97(2) . . ?
C19 C11 S9 117.8(19) . . ?
C12 C11 S9 112.4(16) . . ?
C11 C12 S10 103.8(17) . . ?
C18 C17 S15 108(2) . . ?
C17 C18 C20 89.2(18) . . ?
C17 C18 S16 106(2) . . ?
C20 C18 S16 111(2) . . ?

_refine_diff_density_max         1.010
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.079

####################################################################### 
# 
# 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_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2048856'
loop_
_audit_author_name
_audit_author_address
'Narcis Avarvari'
;CNRS, University of Angers
France
;
_audit_update_record             
;
2020-12-07 deposited with the CCDC.	2021-02-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H8 S5'
_chemical_formula_sum            'C7 H8 S5'
_chemical_formula_weight         252.43

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'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   7.4434(2)
_cell_length_b                   15.6819(4)
_cell_length_c                   8.7048(2)
_cell_angle_alpha                90
_cell_angle_beta                 92.980(2)
_cell_angle_gamma                90
_cell_volume                     1014.71(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    149.4(4)
_cell_measurement_reflns_used    3514
_cell_measurement_theta_min      5.0610
_cell_measurement_theta_max      73.1420

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_F_000             520
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    10.046
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.55566
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.697
_oxdiff_exptl_absorpt_empirical_full_max 1.685
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      149.4(4)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_reflns_number            7411
_diffrn_reflns_av_unetI/netI     0.0693
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         5.088
_diffrn_reflns_theta_max         73.415
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             3915
_reflns_number_gt                3581
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.880
_reflns_Friedel_fraction_max     0.935
_reflns_Friedel_fraction_full    0.988

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

_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0500P)²+0.0892P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1515 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.08(3)
_chemical_absolute_configuration syn
_refine_ls_number_reflns         3915
_refine_ls_number_parameters     217
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0419
_refine_ls_wR_factor_ref         0.1153
_refine_ls_wR_factor_gt          0.1062
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5960(11) 0.6860(4) 0.2971(8) 0.0282(15) Uani 1 1 d . . . . .
H1 H 0.576731 0.738484 0.354986 0.034 Uiso 1 1 calc R U . . .
C2 C 0.4924(10) 0.6155(5) 0.3779(8) 0.0275(14) Uani 1 1 d . . . . .
H2 H 0.536137 0.616928 0.485974 0.033 Uiso 1 1 calc R U . . .
C3 C 0.4810(10) 0.6003(5) 0.0325(8) 0.0266(14) Uani 1 1 d . . . . .
C4 C 0.4984(9) 0.5266(4) 0.1100(7) 0.0225(13) Uani 1 1 d . . . . .
C5 C 0.4303(9) 0.4804(4) -0.1753(7) 0.0215(14) Uani 1 1 d . . . . .
C6 C 0.7964(11) 0.6731(6) 0.2988(10) 0.0401(19) Uani 1 1 d . . . . .
H6A H 0.850419 0.719656 0.246371 0.060 Uiso 1 1 calc R U . . .
H6B H 0.844243 0.671005 0.403335 0.060 Uiso 1 1 calc R U . . .
H6C H 0.822349 0.620591 0.247975 0.060 Uiso 1 1 calc R U . . .
C7 C 0.2906(11) 0.6283(5) 0.3786(10) 0.0384(18) Uani 1 1 d . . . . .
H7A H 0.237563 0.581499 0.431091 0.058 Uiso 1 1 calc R U . . .
H7B H 0.265336 0.680590 0.430457 0.058 Uiso 1 1 calc R U . . .
H7C H 0.241138 0.630789 0.274600 0.058 Uiso 1 1 calc R U . . .
C8 C 1.0907(11) 0.3221(5) 0.3470(9) 0.0337(16) Uani 1 1 d . . . . .
H8 H 1.087338 0.323835 0.459394 0.040 Uiso 1 1 calc R U . . .
C9 C 0.9364(10) 0.2648(5) 0.2904(9) 0.0302(15) Uani 1 1 d . . . . .
H9 H 0.952200 0.210666 0.345737 0.036 Uiso 1 1 calc R U . . .
C10 C 0.9933(10) 0.4167(5) 0.0867(8) 0.0268(15) Uani 1 1 d . . . . .
C11 C 0.9480(9) 0.3442(5) 0.0120(8) 0.0258(15) Uani 1 1 d . . . . .
C12 C 0.9168(9) 0.4641(5) -0.1981(9) 0.0294(16) Uani 1 1 d . . . . .
C13 C 1.2741(11) 0.2881(6) 0.3118(10) 0.0375(17) Uani 1 1 d . . . . .
H13A H 1.365232 0.327039 0.350319 0.056 Uiso 1 1 calc R U . . .
H13B H 1.292270 0.233523 0.360077 0.056 Uiso 1 1 calc R U . . .
H13C H 1.281394 0.282132 0.202498 0.056 Uiso 1 1 calc R U . . .
C14 C 0.7510(10) 0.2987(5) 0.3277(9) 0.0335(16) Uani 1 1 d . . . . .
H14A H 0.659872 0.259792 0.289071 0.050 Uiso 1 1 calc R U . . .
H14B H 0.744586 0.304127 0.437132 0.050 Uiso 1 1 calc R U . . .
H14C H 0.732115 0.353476 0.280321 0.050 Uiso 1 1 calc R U . . .
S1 S 0.4976(3) 0.70469(11) 0.1026(2) 0.0345(4) Uani 1 1 d . . . . .
S2 S 0.5515(2) 0.51034(11) 0.30660(18) 0.0259(4) Uani 1 1 d . . . . .
S3 S 0.4323(3) 0.59005(12) -0.16556(19) 0.0307(4) Uani 1 1 d . . . . .
S4 S 0.4727(2) 0.43325(10) 0.00202(19) 0.0252(3) Uani 1 1 d . . . . .
S5 S 0.3907(3) 0.42694(13) -0.3370(2) 0.0351(4) Uani 1 1 d . . . . .
S6 S 1.0577(2) 0.43196(11) 0.2801(2) 0.0301(4) Uani 1 1 d . . . . .
S7 S 0.9456(3) 0.23959(11) 0.0844(2) 0.0301(4) Uani 1 1 d . . . . .
S8 S 0.9830(2) 0.50947(11) -0.0229(2) 0.0294(4) Uani 1 1 d . . . . .
S9 S 0.8824(3) 0.35562(12) -0.18444(19) 0.0294(4) Uani 1 1 d . . . . .
S10 S 0.8900(3) 0.51782(14) -0.3601(2) 0.0408(5) 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
C1 C6 1.504(12) . ?
C1 C2 1.538(10) . ?
C1 S1 1.833(7) . ?
C2 C7 1.515(11) . ?
C2 S2 1.824(7) . ?
C3 C4 1.341(10) . ?
C3 S1 1.750(8) . ?
C3 S3 1.750(7) . ?
C4 S4 1.744(7) . ?
C4 S2 1.755(7) . ?
C5 S5 1.652(7) . ?
C5 S3 1.721(7) . ?
C5 S4 1.726(7) . ?
C8 C13 1.513(12) . ?
C8 C9 1.520(11) . ?
C8 S6 1.831(8) . ?
C9 C14 1.530(11) . ?
C9 S7 1.841(8) . ?
C10 C11 1.344(11) . ?
C10 S8 1.739(8) . ?
C10 S6 1.742(7) . ?
C11 S7 1.758(8) . ?
C11 S9 1.763(7) . ?
C12 S10 1.646(8) . ?
C12 S9 1.725(9) . ?
C12 S8 1.731(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 C1 C2 114.8(6) . . ?
C6 C1 S1 112.3(5) . . ?
C2 C1 S1 110.6(5) . . ?
C7 C2 C1 115.3(6) . . ?
C7 C2 S2 112.2(5) . . ?
C1 C2 S2 111.0(5) . . ?
C4 C3 S1 128.9(5) . . ?
C4 C3 S3 115.2(5) . . ?
S1 C3 S3 115.9(4) . . ?
C3 C4 S4 116.5(5) . . ?
C3 C4 S2 128.8(5) . . ?
S4 C4 S2 114.6(4) . . ?
S5 C5 S3 123.4(4) . . ?
S5 C5 S4 124.1(4) . . ?
S3 C5 S4 112.5(4) . . ?
C13 C8 C9 113.6(7) . . ?
C13 C8 S6 112.0(6) . . ?
C9 C8 S6 111.5(5) . . ?
C8 C9 C14 113.6(6) . . ?
C8 C9 S7 112.2(5) . . ?
C14 C9 S7 111.2(5) . . ?
C11 C10 S8 116.1(5) . . ?
C11 C10 S6 129.3(6) . . ?
S8 C10 S6 114.6(4) . . ?
C10 C11 S7 128.5(6) . . ?
C10 C11 S9 115.7(6) . . ?
S7 C11 S9 115.8(4) . . ?
S10 C12 S9 123.5(5) . . ?
S10 C12 S8 124.1(5) . . ?
S9 C12 S8 112.4(4) . . ?
C3 S1 C1 100.9(3) . . ?
C4 S2 C2 98.9(3) . . ?
C5 S3 C3 98.1(3) . . ?
C5 S4 C4 97.6(3) . . ?
C10 S6 C8 101.8(4) . . ?
C11 S7 C9 98.7(3) . . ?
C12 S8 C10 98.2(4) . . ?
C12 S9 C11 97.6(4) . . ?

_refine_diff_density_max         0.333
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.087

####################################################################### 
# 
# 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_shelx_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 2048857'
loop_
_audit_author_name
_audit_author_address
'Narcis Avarvari'
;CNRS, University of Angers
France
;
_audit_update_record             
;
2020-12-07 deposited with the CCDC.	2021-02-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H8 S5'
_chemical_formula_sum            'C7 H8 S5'
_chemical_formula_weight         252.43

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'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   13.2577(9)
_cell_length_b                   5.9544(4)
_cell_length_c                   13.8006(8)
_cell_angle_alpha                90
_cell_angle_beta                 106.797(7)
_cell_angle_gamma                90
_cell_volume                     1042.96(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.00(10)
_cell_measurement_reflns_used    1477
_cell_measurement_theta_min      4.0770
_cell_measurement_theta_max      72.4000

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_F_000             520
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    9.774
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.76488
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.727
_oxdiff_exptl_absorpt_empirical_full_max 1.562
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150.00(10)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_reflns_number            3768
_diffrn_reflns_av_unetI/netI     0.0650
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         4.073
_diffrn_reflns_theta_max         72.898
_diffrn_reflns_theta_full        70.000
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             2027
_reflns_number_gt                1624
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0562P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2027
_refine_ls_number_parameters     129
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0444
_refine_ls_wR_factor_ref         0.1188
_refine_ls_wR_factor_gt          0.1102
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1A C 0.5465(6) -0.0279(14) 0.2514(6) 0.0269(17) Uani 0.5 1 d . . P A 1
H1A H 0.606796 0.037655 0.302226 0.032 Uiso 0.5 1 calc R U P A 1
C2A C 0.5339(6) -0.2824(12) 0.2748(5) 0.0240(14) Uani 0.5 1 d . . P A 1
H2A H 0.475833 -0.352569 0.222955 0.029 Uiso 0.5 1 calc R U P A 1
C1B C 0.5033(9) -0.0871(16) 0.2169(8) 0.0400(19) Uani 0.5 1 d . . P A 2
H1B H 0.453981 -0.203811 0.182098 0.048 Uiso 0.5 1 calc R U P A 2
C2B C 0.5763(9) -0.1913(18) 0.3035(7) 0.0410(19) Uani 0.5 1 d . . P A 2
H2B H 0.626936 -0.076215 0.337827 0.049 Uiso 0.5 1 calc R U P A 2
C3 C 0.3789(3) 0.0353(6) 0.3351(3) 0.0283(7) Uani 1 1 d . . . . .
C4 C 0.4125(3) -0.1434(6) 0.3954(2) 0.0276(7) Uani 1 1 d . . . . .
C5 C 0.2478(3) 0.0036(6) 0.4450(3) 0.0321(7) Uani 1 1 d . . . . .
C6 C 0.5598(4) -0.0010(8) 0.1421(3) 0.0443(10) Uani 1 1 d . . . . .
H6A H 0.627189 -0.058810 0.141517 0.066 Uiso 1 1 calc R U . A 1
H6B H 0.555152 0.154988 0.123828 0.066 Uiso 1 1 calc R U . A 1
H6C H 0.505036 -0.082938 0.094382 0.066 Uiso 1 1 calc R U . A 1
C7 C 0.6406(4) -0.3943(8) 0.2810(3) 0.0455(10) Uani 1 1 d . . . . .
H7A H 0.650739 -0.397209 0.214903 0.068 Uiso 1 1 calc R U . A 1
H7B H 0.640882 -0.545093 0.305709 0.068 Uiso 1 1 calc R U . A 1
H7C H 0.696433 -0.310241 0.326227 0.068 Uiso 1 1 calc R U . A 1
S1 S 0.42715(8) 0.13947(17) 0.23954(7) 0.0366(3) Uani 1 1 d . . . . .
S2 S 0.51924(7) -0.31790(16) 0.39950(7) 0.0345(2) Uani 1 1 d . . . . .
S3 S 0.26792(7) 0.17294(15) 0.35013(6) 0.0331(2) Uani 1 1 d . . . . .
S4 S 0.33758(7) -0.21275(15) 0.47649(6) 0.0309(2) Uani 1 1 d . . . . .
S5 S 0.15325(8) 0.0413(2) 0.49838(7) 0.0433(3) 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
C1Aa C2A 1.568(11) . ?
C1Aa C6 1.576(9) . ?
C1Aa S1 1.837(8) . ?
C2Aa C7 1.544(8) . ?
C2Aa S2 1.799(7) . ?
C1Bb C2B 1.443(14) . ?
C1Bb C6 1.528(9) . ?
C1Bb S1 1.766(9) . ?
C2Bb C7 1.561(9) . ?
C2Bb S2 1.864(8) . ?
C3 C4 1.345(5) . ?
C3 S1 1.738(4) . ?
C3 S3 1.748(3) . ?
C4 S2 1.743(3) . ?
C4 S4 1.747(3) . ?
C5 S5 1.642(4) . ?
C5 S4 1.722(4) . ?
C5 S3 1.734(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2Aa C1Aa C6 110.1(6) . . ?
C2Aa C1Aa S1 113.7(5) . . ?
C6 C1Aa S1 101.0(5) . . ?
C7 C2Aa C1A 106.1(6) . . ?
C7 C2Aa S2 104.3(4) . . ?
C1Aa C2Aa S2 111.0(5) . . ?
C2Bb C1Bb C6 111.2(8) . . ?
C2Bb C1Bb S1 117.6(7) . . ?
C6 C1Bb S1 106.3(5) . . ?
C1Bb C2Bb C7 116.3(8) . . ?
C1Bb C2Bb S2 116.7(7) . . ?
C7 C2Bb S2 100.7(5) . . ?
C4 C3 S1 128.6(3) . . ?
C4 C3 S3 115.9(3) . . ?
S1 C3 S3 115.4(2) . . ?
C3 C4 S2 127.8(3) . . ?
C3 C4 S4 115.8(3) . . ?
S2 C4 S4 116.4(2) . . ?
S5 C5 S4 123.4(2) . . ?
S5 C5 S3 124.3(2) . . ?
S4 C5 S3 112.3(2) . . ?
C3 S1 C1B 102.5(3) . . ?
C3 S1 C1A 103.6(3) . . ?
C4 S2 C2A 102.1(3) . . ?
C4 S2 C2B 103.2(3) . . ?
C5 S3 C3 97.79(17) . . ?
C5 S4 C4 98.13(17) . . ?

_refine_diff_density_max         0.409
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.098

####################################################################### 
# 
# 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_shelx_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 2048860'
loop_
_audit_author_name
_audit_author_address
'Narcis Avarvari'
;CNRS, University of Angers
France
;
_audit_update_record             
;
2020-12-07 deposited with the CCDC.	2021-02-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H36 N, Ni C10 H12 S8'
_chemical_formula_sum            'C26 H48 N Ni S8'
_chemical_formula_weight         689.84

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'
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'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.3679(7)
_cell_length_b                   13.5115(10)
_cell_length_c                   13.8074(9)
_cell_angle_alpha                83.771(6)
_cell_angle_beta                 76.905(6)
_cell_angle_gamma                87.281(6)
_cell_volume                     1691.7(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    150.03(13)
_cell_measurement_reflns_used    3440
_cell_measurement_theta_min      3.2420
_cell_measurement_theta_max      70.6580

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_F_000             734
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    5.564
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.73783
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.732
_oxdiff_exptl_absorpt_empirical_full_max 1.520
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150.03(13)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_reflns_number            12886
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.291
_diffrn_reflns_theta_max         73.612
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             6561
_reflns_number_gt                4648
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1018P)²+3.4634P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6561
_refine_ls_number_parameters     346
_refine_ls_number_restraints     27
_refine_ls_R_factor_all          0.1093
_refine_ls_R_factor_gt           0.0824
_refine_ls_wR_factor_ref         0.2421
_refine_ls_wR_factor_gt          0.2162
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.074
_refine_ls_shift/su_mean         0.002

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1073(17) 0.1892(12) 1.3578(9) 0.175(6) Uani 1 1 d . . . . .
H1A H 0.155629 0.134822 1.389171 0.263 Uiso 1 1 calc R U . A 1
H1B H 0.078628 0.239540 1.402903 0.263 Uiso 1 1 calc R U . A 1
H1C H 0.021940 0.165633 1.340777 0.263 Uiso 1 1 calc R U . A 1
C4 C 0.1529(7) 0.1122(4) 1.1293(5) 0.0644(14) Uani 1 1 d . . . . .
C5 C 0.0273(8) 0.1650(5) 1.1308(6) 0.0810(19) Uani 1 1 d . . . . .
C6 C 0.308(3) 0.612(2) 0.5801(13) 0.337(19) Uani 1 1 d D . . . .
H6A H 0.299427 0.639457 0.514571 0.505 Uiso 1 1 calc R U . . .
H6B H 0.338317 0.543210 0.578628 0.505 Uiso 1 1 calc R U . . .
H6C H 0.215190 0.617447 0.626177 0.505 Uiso 1 1 calc R U . . .
C7 C 0.4082(14) 0.6158(18) 0.7015(16) 0.313(18) Uani 1 1 d D . . . .
H7A H 0.318221 0.578831 0.718507 0.376 Uiso 1 1 calc R U . . .
H7B H 0.396041 0.666346 0.747781 0.376 Uiso 1 1 calc R U . . .
C8 C 0.4131(13) 0.6647(16) 0.6109(15) 0.271(14) Uani 1 1 d D . . . .
H8 H 0.359021 0.726640 0.628073 0.325 Uiso 1 1 calc R U . . .
C9 C 0.6937(7) 0.5471(5) 0.6257(5) 0.0676(15) Uani 1 1 d . . . . .
C10 C 0.7067(7) 0.6161(5) 0.5469(5) 0.0705(16) Uani 1 1 d . . . . .
C11 C 0.4132(8) 0.0866(5) 0.7927(6) 0.0794(19) Uani 1 1 d . . . . .
H11A H 0.495270 0.041946 0.799520 0.095 Uiso 1 1 calc R U . . .
H11B H 0.334014 0.070430 0.850299 0.095 Uiso 1 1 calc R U . . .
C12 C 0.3641(11) 0.0666(6) 0.7009(8) 0.106(3) Uani 1 1 d . . . . .
H12A H 0.262510 0.088654 0.708248 0.127 Uiso 1 1 calc R U . . .
H12B H 0.421142 0.107169 0.644339 0.127 Uiso 1 1 calc R U . . .
C13 C 0.3757(19) -0.0343(8) 0.6778(10) 0.167(6) Uani 1 1 d . . . . .
H13A H 0.322797 -0.075361 0.735517 0.201 Uiso 1 1 calc R U . . .
H13B H 0.478090 -0.055280 0.666936 0.201 Uiso 1 1 calc R U . . .
C14 C 0.3197(12) -0.0544(8) 0.5888(10) 0.140(4) Uani 1 1 d . . . . .
H14A H 0.332493 -0.124001 0.579755 0.210 Uiso 1 1 calc R U . . .
H14B H 0.217485 -0.036172 0.599132 0.210 Uiso 1 1 calc R U . . .
H14C H 0.373205 -0.016037 0.530361 0.210 Uiso 1 1 calc R U . . .
C15 C 0.5889(7) 0.2198(5) 0.7095(4) 0.0636(14) Uani 1 1 d . . . . .
H15A H 0.561822 0.210494 0.647386 0.076 Uiso 1 1 calc R U . . .
H15B H 0.608432 0.289892 0.708007 0.076 Uiso 1 1 calc R U . . .
C16 C 0.7286(8) 0.1607(7) 0.7136(6) 0.095(3) Uani 1 1 d . . . . .
H16A H 0.767550 0.181611 0.767346 0.114 Uiso 1 1 calc R U . . .
H16B H 0.704396 0.091003 0.730650 0.114 Uiso 1 1 calc R U . . .
C17 C 0.8417(8) 0.1691(6) 0.6239(6) 0.091(2) Uani 1 1 d . . . . .
H17A H 0.865196 0.238786 0.606333 0.109 Uiso 1 1 calc R U . . .
H17B H 0.803476 0.147099 0.570380 0.109 Uiso 1 1 calc R U . . .
C18 C 0.9811(9) 0.1109(7) 0.6296(8) 0.114(3) Uani 1 1 d . . . . .
H18A H 1.049971 0.120943 0.566526 0.171 Uiso 1 1 calc R U . . .
H18B H 1.021976 0.133220 0.680956 0.171 Uiso 1 1 calc R U . . .
H18C H 0.960121 0.041333 0.644924 0.171 Uiso 1 1 calc R U . . .
C19 C 0.4989(8) 0.2004(5) 0.8949(4) 0.0754(18) Uani 1 1 d . . . . .
H19A H 0.414814 0.181174 0.947979 0.090 Uiso 1 1 calc R U . . .
H19B H 0.577854 0.152782 0.901230 0.090 Uiso 1 1 calc R U . . .
C20 C 0.5456(9) 0.3022(6) 0.9103(5) 0.086(2) Uani 1 1 d . . . . .
H20A H 0.611813 0.329515 0.849662 0.103 Uiso 1 1 calc R U . . .
H20B H 0.459977 0.346199 0.922653 0.103 Uiso 1 1 calc R U . . .
C21 C 0.6202(10) 0.2987(8) 0.9959(7) 0.105(3) Uani 1 1 d . . . . .
H21A H 0.703076 0.252260 0.984788 0.126 Uiso 1 1 calc R U . . .
H21B H 0.552345 0.273870 1.056825 0.126 Uiso 1 1 calc R U . . .
C22 C 0.6734(10) 0.3989(8) 1.0096(8) 0.117(3) Uani 1 1 d . . . . .
H22A H 0.720023 0.392267 1.065203 0.175 Uiso 1 1 calc R U . . .
H22B H 0.742379 0.423324 0.950122 0.175 Uiso 1 1 calc R U . . .
H22C H 0.591596 0.444943 1.022184 0.175 Uiso 1 1 calc R U . . .
C23 C 0.3354(7) 0.2671(5) 0.7823(5) 0.0671(15) Uani 1 1 d . . . . .
H23A H 0.318551 0.265759 0.715716 0.080 Uiso 1 1 calc R U . . .
H23B H 0.366278 0.333561 0.787275 0.080 Uiso 1 1 calc R U . . .
C24 C 0.1913(8) 0.2472(6) 0.8583(6) 0.088(2) Uani 1 1 d . . . . .
H24A H 0.156267 0.182584 0.850907 0.105 Uiso 1 1 calc R U . . .
H24B H 0.207987 0.245397 0.925237 0.105 Uiso 1 1 calc R U . . .
C25 C 0.0756(8) 0.3262(6) 0.8448(6) 0.087(2) Uani 1 1 d . . . . .
H25A H 0.071451 0.335756 0.774779 0.104 Uiso 1 1 calc R U . . .
H25B H -0.019173 0.302899 0.882631 0.104 Uiso 1 1 calc R U . . .
C26 C 0.1024(12) 0.4215(8) 0.8766(13) 0.176(7) Uani 1 1 d . . . . .
H26A H 0.025687 0.468380 0.866264 0.263 Uiso 1 1 calc R U . . .
H26B H 0.104281 0.413079 0.946260 0.263 Uiso 1 1 calc R U . . .
H26C H 0.194956 0.445955 0.838348 0.263 Uiso 1 1 calc R U . . .
N1 N 0.4593(5) 0.1933(4) 0.7953(4) 0.0637(12) Uani 1 1 d . . . . .
S1 S 0.2989(2) 0.13736(13) 1.18298(15) 0.0766(5) Uani 1 1 d . . . . .
S2 S -0.0279(3) 0.2741(2) 1.1885(3) 0.1334(12) Uani 1 1 d . . . . .
S3 S 0.18832(16) 0.00820(11) 1.06272(11) 0.0608(4) Uani 1 1 d . . . . .
S4 S -0.10077(19) 0.12724(13) 1.07046(15) 0.0783(5) Uani 1 1 d . . . . .
S5 S 0.5439(2) 0.53384(17) 0.73084(19) 0.1009(7) Uani 1 1 d . . . . .
S6 S 0.5751(3) 0.7100(2) 0.52967(18) 0.1192(10) Uani 1 1 d . . . . .
S7 S 0.8360(2) 0.46292(12) 0.63486(13) 0.0760(5) Uani 1 1 d . . . . .
S8 S 0.8638(2) 0.61864(14) 0.45283(13) 0.0823(5) Uani 1 1 d . . . . .
NI1 Ni 0.000000 0.000000 1.000000 0.0549(3) Uani 1 2 d S . P . .
NI2 Ni 1.000000 0.500000 0.500000 0.0574(4) Uani 1 2 d S . P . .
C2A C 0.2097(19) 0.2324(11) 1.2649(11) 0.071(4) Uani 0.5 1 d D U P B 1
H2A H 0.289828 0.258678 1.288782 0.085 Uiso 0.5 1 calc R U P B 1
C3A C 0.158(2) 0.3189(12) 1.2027(14) 0.090(4) Uani 0.5 1 d D U P B 1
H3A1 H 0.225791 0.331116 1.138234 0.108 Uiso 0.5 1 calc R U P B 1
H3A2 H 0.146514 0.379029 1.236541 0.108 Uiso 0.5 1 calc R U P B 1
C2B C 0.251(3) 0.261(3) 1.224(3) 0.162(13) Uani 0.5 1 d . U P B 2
H2B1 H 0.304401 0.269397 1.275334 0.195 Uiso 0.5 1 calc R U P B 2
H2B2 H 0.287621 0.309464 1.168156 0.195 Uiso 0.5 1 calc R U P B 2
C3B C 0.104(2) 0.2859(19) 1.2625(19) 0.114(6) Uani 0.5 1 d . U P B 2
H3B H 0.094806 0.351007 1.288746 0.136 Uiso 0.5 1 calc R U P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2A 1.50(2) . ?
C1 C3B 1.75(3) . ?
C4 C5 1.345(9) . ?
C4 S3 1.740(6) . ?
C4 S1 1.759(6) . ?
C5 S4 1.731(7) . ?
C5 S2 1.752(7) . ?
C6 C8 1.405(16) . ?
C7 C8 1.342(15) . ?
C7 S5 1.735(14) . ?
C8 S6 1.762(15) . ?
C9 C10 1.340(9) . ?
C9 S7 1.728(7) . ?
C9 S5 1.776(7) . ?
C10 S8 1.727(7) . ?
C10 S6 1.763(6) . ?
C11 C12 1.497(12) . ?
C11 N1 1.530(9) . ?
C12 C13 1.428(12) . ?
C13 C14 1.495(16) . ?
C15 C16 1.509(8) . ?
C15 N1 1.518(7) . ?
C16 C17 1.434(10) . ?
C17 C18 1.505(10) . ?
C19 C20 1.513(11) . ?
C19 N1 1.517(8) . ?
C20 C21 1.499(10) . ?
C21 C22 1.510(13) . ?
C23 N1 1.523(7) . ?
C23 C24 1.526(9) . ?
C24 C25 1.513(9) . ?
C25 C26 1.456(14) . ?
S1 C2B 1.83(3) . ?
S1 C2A 1.847(15) . ?
S2 C3B 1.80(2) . ?
S2 C3A 1.932(19) . ?
S3 NI1 2.1462(14) . ?
S4 NI1 2.1415(17) . ?
S7 NI2 2.1573(17) . ?
S8 NI2 2.1395(17) . ?
NI1 S4 2.1415(17) 2_557 ?
NI1 S3 2.1462(14) 2_557 ?
NI2 S8 2.1395(17) 2_766 ?
NI2 S7 2.1573(17) 2_766 ?
C2Aa C3A 1.502(16) . ?
C2Bb C3B 1.39(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C5 C4 S3 119.4(5) . . ?
C5 C4 S1 128.1(5) . . ?
S3 C4 S1 112.4(3) . . ?
C4 C5 S4 120.1(6) . . ?
C4 C5 S2 127.3(6) . . ?
S4 C5 S2 112.6(4) . . ?
C8 C7 S5 124.5(14) . . ?
C6 C8 C7 99.9(19) . . ?
C6 C8 S6 123.5(17) . . ?
C7 C8 S6 123.9(10) . . ?
C10 C9 S7 120.1(5) . . ?
C10 C9 S5 126.8(5) . . ?
S7 C9 S5 113.0(4) . . ?
C9 C10 S8 119.9(5) . . ?
C9 C10 S6 125.4(6) . . ?
S8 C10 S6 114.7(4) . . ?
C12 C11 N1 115.8(6) . . ?
C13 C12 C11 116.4(8) . . ?
C12 C13 C14 116.1(10) . . ?
C16 C15 N1 115.3(5) . . ?
C17 C16 C15 115.9(6) . . ?
C16 C17 C18 115.4(7) . . ?
C20 C19 N1 115.1(5) . . ?
C21 C20 C19 112.3(7) . . ?
C20 C21 C22 113.1(8) . . ?
N1 C23 C24 114.4(5) . . ?
C25 C24 C23 111.7(6) . . ?
C26 C25 C24 113.4(9) . . ?
C19 N1 C15 110.7(5) . . ?
C19 N1 C23 110.2(5) . . ?
C15 N1 C23 107.0(4) . . ?
C19 N1 C11 108.3(5) . . ?
C15 N1 C11 110.1(5) . . ?
C23 N1 C11 110.6(5) . . ?
C4 S1 C2B 103.2(11) . . ?
C4 S1 C2A 99.9(5) . . ?
C5 S2 C3B 104.2(8) . . ?
C5 S2 C3A 100.7(6) . . ?
C4 S3 NI1 104.4(2) . . ?
C5 S4 NI1 104.5(2) . . ?
C7 S5 C9 105.6(5) . . ?
C10 S6 C8 103.2(6) . . ?
C9 S7 NI2 104.1(2) . . ?
C10 S8 NI2 104.7(2) . . ?
S4 NI1 S4 180.00(9) 2_557 . ?
S4 NI1 S3 88.55(6) 2_557 . ?
S4 NI1 S3 91.45(6) . . ?
S4 NI1 S3 91.45(6) 2_557 2_557 ?
S4 NI1 S3 88.55(6) . 2_557 ?
S3 NI1 S3 180.0 . 2_557 ?
S8 NI2 S8 180.00(8) 2_766 . ?
S8 NI2 S7 88.83(7) 2_766 . ?
S8 NI2 S7 91.17(7) . . ?
S8 NI2 S7 91.17(7) 2_766 2_766 ?
S8 NI2 S7 88.83(7) . 2_766 ?
S7 NI2 S7 180.00(7) . 2_766 ?
C1 C2Aa C3A 119.3(16) . . ?
C1 C2Aa S1 113.2(10) . . ?
C3Aa C2Aa S1 109.3(11) . . ?
C2Aa C3Aa S2 102.1(12) . . ?
C3Bb C2Bb S1 119(2) . . ?
C2Bb C3Bb C1 87(2) . . ?
C2Bb C3Bb S2 119(2) . . ?
C1 C3Bb S2 115.3(14) . . ?

_refine_diff_density_max         1.107
_refine_diff_density_min         -0.887
_refine_diff_density_rms         0.085

####################################################################### 
# 
# 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_shelx_CCDC5
_database_code_depnum_ccdc_archive 'CCDC 2048861'
loop_
_audit_author_name
_audit_author_address
'Narcis Avarvari'
;CNRS, University of Angers
France
;
_audit_update_record             
;
2020-12-07 deposited with the CCDC.	2021-02-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H36 N, Ni C10 H12 S8'
_chemical_formula_sum            'C26 H48 N Ni S8'
_chemical_formula_weight         689.84

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'
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'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.3463(5)
_cell_length_b                   13.4804(8)
_cell_length_c                   13.8283(7)
_cell_angle_alpha                83.785(4)
_cell_angle_beta                 76.530(5)
_cell_angle_gamma                87.594(5)
_cell_volume                     1684.12(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    150.00(10)
_cell_measurement_reflns_used    9482
_cell_measurement_theta_min      3.2400
_cell_measurement_theta_max      70.7970

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_F_000             734
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    5.589
_shelx_estimated_absorpt_T_min   0.554
_shelx_estimated_absorpt_T_max   0.850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.69013
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.700
_oxdiff_exptl_absorpt_empirical_full_max 1.628
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150.00(10)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_reflns_number            26519
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.298
_diffrn_reflns_theta_max         73.189
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measured_fraction_theta_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_point_group_measured_fraction_full 0.984
_reflns_number_total             6435
_reflns_number_gt                5140
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1267P)²+9.4714P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6435
_refine_ls_number_parameters     346
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.1192
_refine_ls_R_factor_gt           0.1046
_refine_ls_wR_factor_ref         0.3208
_refine_ls_wR_factor_gt          0.3103
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_restrained_S_all      1.136
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.001

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
C3 C 0.9721(10) 0.3334(7) 0.3705(8) 0.072(2) Uani 1 1 d . . . . .
C4 C 0.8462(9) 0.3882(6) 0.3715(6) 0.0585(19) Uani 1 1 d . . . . .
C5 C 0.886(2) 0.3149(14) 0.1423(11) 0.149(6) Uani 1 1 d D . . . .
H5A H 0.836715 0.368953 0.108299 0.223 Uiso 1 1 calc R U . A 1
H5B H 0.971155 0.341129 0.160357 0.223 Uiso 1 1 calc R U . A 1
H5C H 0.918396 0.262620 0.097511 0.223 Uiso 1 1 calc R U . A 1
C8 C 0.2937(10) -0.1135(7) 0.9535(7) 0.065(2) Uani 1 1 d . . . . .
C9 C 0.3063(10) -0.0476(6) 0.8731(6) 0.0600(19) Uani 1 1 d . . . . .
C11 C 0.5855(11) 0.4135(6) 0.7082(8) 0.073(2) Uani 1 1 d . . . . .
H11A H 0.666182 0.430870 0.648931 0.088 Uiso 1 1 calc R U . . .
H11B H 0.501127 0.458869 0.702290 0.088 Uiso 1 1 calc R U . . .
C12 C 0.6349(15) 0.4327(8) 0.7986(11) 0.097(4) Uani 1 1 d . . . . .
H12A H 0.577054 0.390197 0.856116 0.117 Uiso 1 1 calc R U . . .
H12B H 0.739055 0.410609 0.789836 0.117 Uiso 1 1 calc R U . . .
C13 C 0.623(3) 0.5348(11) 0.8241(14) 0.164(8) Uani 1 1 d . . . . .
H13A H 0.674604 0.577824 0.764544 0.197 Uiso 1 1 calc R U . . .
H13B H 0.518051 0.554960 0.837638 0.197 Uiso 1 1 calc R U . . .
C14 C 0.6808(17) 0.5563(11) 0.9083(14) 0.132(6) Uani 1 1 d . . . . .
H14A H 0.666152 0.627403 0.917382 0.197 Uiso 1 1 calc R U . . .
H14B H 0.628855 0.516515 0.968906 0.197 Uiso 1 1 calc R U . . .
H14C H 0.786088 0.539478 0.895494 0.197 Uiso 1 1 calc R U . . .
C15 C 0.4084(9) 0.2804(6) 0.7912(6) 0.0585(19) Uani 1 1 d . . . . .
H15A H 0.389122 0.208329 0.794055 0.070 Uiso 1 1 calc R U . . .
H15B H 0.434696 0.291675 0.854443 0.070 Uiso 1 1 calc R U . . .
C16 C 0.2688(11) 0.3382(9) 0.7852(8) 0.089(3) Uani 1 1 d . . . . .
H16A H 0.293472 0.409239 0.764953 0.107 Uiso 1 1 calc R U . . .
H16B H 0.228768 0.313840 0.731924 0.107 Uiso 1 1 calc R U . . .
C17 C 0.1541(11) 0.3317(9) 0.8772(8) 0.085(3) Uani 1 1 d . . . . .
H17A H 0.192622 0.358114 0.930082 0.102 Uiso 1 1 calc R U . . .
H17B H 0.130953 0.260596 0.898642 0.102 Uiso 1 1 calc R U . . .
C18 C 0.0157(12) 0.3870(9) 0.8686(11) 0.106(4) Uani 1 1 d . . . . .
H18A H -0.055656 0.379215 0.933091 0.159 Uiso 1 1 calc R U . . .
H18B H 0.036758 0.457937 0.849221 0.159 Uiso 1 1 calc R U . . .
H18C H -0.025003 0.360273 0.817734 0.159 Uiso 1 1 calc R U . . .
C19 C 0.5004(10) 0.2998(7) 0.6057(6) 0.068(2) Uani 1 1 d . . . . .
H19A H 0.586582 0.320137 0.551454 0.081 Uiso 1 1 calc R U . . .
H19B H 0.419251 0.347973 0.599743 0.081 Uiso 1 1 calc R U . . .
C20 C 0.4538(12) 0.1964(8) 0.5902(7) 0.082(3) Uani 1 1 d . . . . .
H20A H 0.541584 0.151801 0.576996 0.098 Uiso 1 1 calc R U . . .
H20B H 0.385518 0.167788 0.651957 0.098 Uiso 1 1 calc R U . . .
C21 C 0.3799(13) 0.2015(10) 0.5046(8) 0.095(3) Uani 1 1 d . . . . .
H21A H 0.450652 0.225704 0.442136 0.114 Uiso 1 1 calc R U . . .
H21B H 0.296592 0.250003 0.515586 0.114 Uiso 1 1 calc R U . . .
C22 C 0.3236(13) 0.1013(11) 0.4928(10) 0.107(4) Uani 1 1 d . . . . .
H22A H 0.276181 0.107675 0.436263 0.160 Uiso 1 1 calc R U . . .
H22B H 0.406096 0.053413 0.480628 0.160 Uiso 1 1 calc R U . . .
H22C H 0.252104 0.077701 0.554045 0.160 Uiso 1 1 calc R U . . .
C23 C 0.6634(9) 0.2332(6) 0.7177(6) 0.0587(19) Uani 1 1 d . . . . .
H23A H 0.679764 0.234155 0.785822 0.070 Uiso 1 1 calc R U . . .
H23B H 0.631856 0.165210 0.712234 0.070 Uiso 1 1 calc R U . . .
C24 C 0.8079(10) 0.2536(8) 0.6427(8) 0.080(3) Uani 1 1 d . . . . .
H24A H 0.844115 0.319409 0.650923 0.096 Uiso 1 1 calc R U . . .
H24B H 0.791702 0.256220 0.574192 0.096 Uiso 1 1 calc R U . . .
C25 C 0.9237(11) 0.1736(8) 0.6557(8) 0.081(3) Uani 1 1 d . . . . .
H25A H 1.021629 0.197632 0.618085 0.097 Uiso 1 1 calc R U . . .
H25B H 0.925862 0.161780 0.727257 0.097 Uiso 1 1 calc R U . . .
C26 C 0.8943(17) 0.0791(11) 0.6204(18) 0.168(9) Uani 1 1 d . . . . .
H26A H 0.971103 0.029821 0.630045 0.252 Uiso 1 1 calc R U . . .
H26B H 0.798266 0.054404 0.658348 0.252 Uiso 1 1 calc R U . . .
H26C H 0.894004 0.090245 0.549210 0.252 Uiso 1 1 calc R U . . .
N1 N 0.5395(7) 0.3067(5) 0.7053(5) 0.0578(16) Uani 1 1 d . . . . .
S1 S 1.0256(4) 0.2247(3) 0.3134(3) 0.1131(13) Uani 1 1 d . . . . .
S2 S 0.7009(3) 0.36299(17) 0.31744(19) 0.0699(6) Uani 1 1 d . . . . .
S3 S 1.1002(2) 0.37243(17) 0.43042(19) 0.0701(6) Uani 1 1 d . . . . .
S4 S 0.8120(2) 0.49216(14) 0.43712(15) 0.0551(5) Uani 1 1 d . . . . .
S5 S 0.4281(3) -0.2056(3) 0.9715(2) 0.1200(14) Uani 1 1 d . . . . .
S6 S 0.4552(3) -0.0351(2) 0.7664(2) 0.0873(8) Uani 1 1 d . . . . .
S7 S 0.1383(3) -0.11614(19) 1.04842(18) 0.0760(7) Uani 1 1 d . . . . .
S8 S 0.1627(3) 0.03588(15) 0.86363(17) 0.0666(6) Uani 1 1 d . . . . .
NI1 Ni 1.000000 0.500000 0.500000 0.0502(5) Uani 1 2 d S . P . .
NI2 Ni 0.000000 0.000000 1.000000 0.0525(5) Uani 1 2 d S . P . .
C6 C 0.588(3) -0.1727(18) 0.8811(18) 0.200(10) Uani 1 1 d D U . . .
H6 H 0.650526 -0.234424 0.869051 0.240 Uiso 1 1 calc R U . . .
C7 C 0.593(3) -0.1189(18) 0.7906(16) 0.198(9) Uani 1 1 d D U . . .
H7A H 0.604401 -0.168203 0.741031 0.238 Uiso 1 1 calc R U . . .
H7B H 0.685045 -0.080830 0.773987 0.238 Uiso 1 1 calc R U . . .
C10 C 0.671(3) -0.102(2) 0.9235(18) 0.245(12) Uani 1 1 d D U . . .
H10A H 0.678937 -0.129503 0.990635 0.367 Uiso 1 1 calc R U . . .
H10B H 0.769856 -0.092788 0.880348 0.367 Uiso 1 1 calc R U . . .
H10C H 0.618537 -0.037625 0.927112 0.367 Uiso 1 1 calc R U . . .
C1A C 0.855(2) 0.1840(13) 0.2927(16) 0.072(5) Uani 0.5 1 d . . P B 1
H1A1 H 0.872884 0.125112 0.254205 0.086 Uiso 0.5 1 calc R U P B 1
H1A2 H 0.785959 0.164714 0.357561 0.086 Uiso 0.5 1 calc R U P B 1
C2A C 0.784(2) 0.2733(14) 0.2319(14) 0.056(4) Uani 0.5 1 d . . P B 1
H2A H 0.701789 0.244174 0.209593 0.068 Uiso 0.5 1 calc R U P B 1
C2B C 0.758(5) 0.240(3) 0.281(3) 0.146(15) Uani 0.5 1 d . U P B 2
H2B1 H 0.745575 0.194713 0.343424 0.175 Uiso 0.5 1 calc R U P B 2
H2B2 H 0.686856 0.219837 0.244476 0.175 Uiso 0.5 1 calc R U P B 2
C1B C 0.889(6) 0.222(3) 0.227(3) 0.181(19) Uani 0.5 1 d D U P B 2
H1B H 0.893815 0.156879 0.199013 0.217 Uiso 0.5 1 calc R U P B 2


_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
C3 C4 1.361(12) . ?
C3 S3 1.734(9) . ?
C3 S1 1.740(10) . ?
C4 S4 1.730(9) . ?
C4 S2 1.757(8) . ?
C5 C2A 1.45(3) . ?
C5 C1B 1.622(19) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C8 C9 1.331(12) . ?
C8 S7 1.715(9) . ?
C8 S5 1.768(9) . ?
C9 S8 1.735(9) . ?
C9 S6 1.776(9) . ?
C11 C12 1.480(15) . ?
C11 N1 1.527(11) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.452(17) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.45(2) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.506(12) . ?
C15 N1 1.518(10) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.458(13) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.488(14) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 N1 1.517(11) . ?
C19 C20 1.529(14) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.499(13) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.508(18) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.514(12) . ?
C23 N1 1.520(10) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.522(13) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.470(19) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
S1 C1A 1.80(2) . ?
S1 C1B 1.94(5) . ?
S2 C2B 1.80(4) . ?
S2 C2A 1.807(16) . ?
S3 NI1 2.136(2) . ?
S4 NI1 2.1453(19) . ?
S5 C6 1.75(2) . ?
S6 C7 1.74(2) . ?
S7 NI2 2.139(2) . ?
S8 NI2 2.152(2) . ?
NI1 S3 2.136(2) 2_766 ?
NI1 S4 2.1453(19) 2_766 ?
NI2 S7 2.139(2) 2_557 ?
NI2 S8 2.152(2) 2_557 ?
C6 C7 1.370(17) . ?
C6 C10 1.497(17) . ?
C6 H6 1.0000 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C1Aa C2A 1.60(3) . ?
C1Aa H1A1 0.9900 . ?
C1Aa H1A2 0.9900 . ?
C2Aa H2A 1.0000 . ?
C2Bb C1B 1.30(6) . ?
C2Bb H2B1 0.9900 . ?
C2Bb H2B2 0.9900 . ?
C1Bb H1B 1.0000 . ?

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
C4 C3 S3 119.3(7) . . ?
C4 C3 S1 127.5(7) . . ?
S3 C3 S1 113.2(5) . . ?
C3 C4 S4 119.8(7) . . ?
C3 C4 S2 127.4(7) . . ?
S4 C4 S2 112.7(5) . . ?
C2Aa C5 H5A 109.5 . . ?
C2Aa C5 H5B 109.5 . . ?
H5Aa C5 H5B 109.5 . . ?
C2Aa C5 H5C 109.5 . . ?
H5Aa C5 H5C 109.5 . . ?
H5Ba C5 H5C 109.5 . . ?
C9 C8 S7 120.9(7) . . ?
C9 C8 S5 124.6(7) . . ?
S7 C8 S5 114.5(5) . . ?
C8 C9 S8 119.6(7) . . ?
C8 C9 S6 127.7(7) . . ?
S8 C9 S6 112.7(5) . . ?
C12 C11 N1 115.6(8) . . ?
C12 C11 H11A 108.4 . . ?
N1 C11 H11A 108.4 . . ?
C12 C11 H11B 108.4 . . ?
N1 C11 H11B 108.4 . . ?
H11A C11 H11B 107.4 . . ?
C13 C12 C11 117.0(12) . . ?
C13 C12 H12A 108.0 . . ?
C11 C12 H12A 108.0 . . ?
C13 C12 H12B 108.0 . . ?
C11 C12 H12B 108.0 . . ?
H12A C12 H12B 107.3 . . ?
C14 C13 C12 117.8(14) . . ?
C14 C13 H13A 107.9 . . ?
C12 C13 H13A 107.9 . . ?
C14 C13 H13B 107.9 . . ?
C12 C13 H13B 107.9 . . ?
H13A C13 H13B 107.2 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 N1 115.1(7) . . ?
C16 C15 H15A 108.5 . . ?
N1 C15 H15A 108.5 . . ?
C16 C15 H15B 108.5 . . ?
N1 C15 H15B 108.5 . . ?
H15A C15 H15B 107.5 . . ?
C17 C16 C15 115.3(8) . . ?
C17 C16 H16A 108.5 . . ?
C15 C16 H16A 108.5 . . ?
C17 C16 H16B 108.5 . . ?
C15 C16 H16B 108.5 . . ?
H16A C16 H16B 107.5 . . ?
C16 C17 C18 114.3(9) . . ?
C16 C17 H17A 108.7 . . ?
C18 C17 H17A 108.7 . . ?
C16 C17 H17B 108.7 . . ?
C18 C17 H17B 108.7 . . ?
H17A C17 H17B 107.6 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N1 C19 C20 114.8(7) . . ?
N1 C19 H19A 108.6 . . ?
C20 C19 H19A 108.6 . . ?
N1 C19 H19B 108.6 . . ?
C20 C19 H19B 108.6 . . ?
H19A C19 H19B 107.5 . . ?
C21 C20 C19 111.2(9) . . ?
C21 C20 H20A 109.4 . . ?
C19 C20 H20A 109.4 . . ?
C21 C20 H20B 109.4 . . ?
C19 C20 H20B 109.4 . . ?
H20A C20 H20B 108.0 . . ?
C20 C21 C22 111.9(11) . . ?
C20 C21 H21A 109.2 . . ?
C22 C21 H21A 109.2 . . ?
C20 C21 H21B 109.2 . . ?
C22 C21 H21B 109.2 . . ?
H21A C21 H21B 107.9 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 N1 114.7(7) . . ?
C24 C23 H23A 108.6 . . ?
N1 C23 H23A 108.6 . . ?
C24 C23 H23B 108.6 . . ?
N1 C23 H23B 108.6 . . ?
H23A C23 H23B 107.6 . . ?
C23 C24 C25 111.7(8) . . ?
C23 C24 H24A 109.3 . . ?
C25 C24 H24A 109.3 . . ?
C23 C24 H24B 109.3 . . ?
C25 C24 H24B 109.3 . . ?
H24A C24 H24B 107.9 . . ?
C26 C25 C24 112.1(11) . . ?
C26 C25 H25A 109.2 . . ?
C24 C25 H25A 109.2 . . ?
C26 C25 H25B 109.2 . . ?
C24 C25 H25B 109.2 . . ?
H25A C25 H25B 107.9 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C19 N1 C15 110.6(7) . . ?
C19 N1 C23 110.2(6) . . ?
C15 N1 C23 107.4(6) . . ?
C19 N1 C11 108.2(7) . . ?
C15 N1 C11 109.6(6) . . ?
C23 N1 C11 110.7(7) . . ?
C3 S1 C1A 102.3(6) . . ?
C3 S1 C1B 102.2(15) . . ?
C4 S2 C2B 99.4(15) . . ?
C4 S2 C2A 102.4(6) . . ?
C3 S3 NI1 104.8(3) . . ?
C4 S4 NI1 104.5(3) . . ?
C6 S5 C8 106.3(9) . . ?
C7 S6 C9 106.9(8) . . ?
C8 S7 NI2 104.3(3) . . ?
C9 S8 NI2 103.9(3) . . ?
S3 NI1 S3 180.0 . 2_766 ?
S3 NI1 S4 91.59(8) . . ?
S3 NI1 S4 88.41(8) 2_766 . ?
S3 NI1 S4 88.41(8) . 2_766 ?
S3 NI1 S4 91.59(8) 2_766 2_766 ?
S4 NI1 S4 180.00(8) . 2_766 ?
S7 NI2 S7 180.0 . 2_557 ?
S7 NI2 S8 88.70(9) . 2_557 ?
S7 NI2 S8 91.30(9) 2_557 2_557 ?
S7 NI2 S8 91.30(9) . . ?
S7 NI2 S8 88.70(9) 2_557 . ?
S8 NI2 S8 180.0 2_557 . ?
C7 C6 C10 98.1(15) . . ?
C7 C6 S5 125(2) . . ?
C10 C6 S5 107.8(19) . . ?
C7 C6 H6 108.2 . . ?
C10 C6 H6 108.1 . . ?
S5 C6 H6 108.2 . . ?
C6 C7 S6 124(2) . . ?
C6 C7 H7A 106.3 . . ?
S6 C7 H7A 106.2 . . ?
C6 C7 H7B 106.3 . . ?
S6 C7 H7B 106.3 . . ?
H7A C7 H7B 106.4 . . ?
C6 C10 H10A 109.5 . . ?
C6 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C6 C10 H10C 109.4 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C2Aa C1Aa S1 109.0(14) . . ?
C2Aa C1Aa H1A1 109.9 . . ?
S1 C1Aa H1A1 109.9 . . ?
C2Aa C1Aa H1A2 109.9 . . ?
S1 C1Aa H1A2 109.9 . . ?
H1A1a C1Aa H1A2 108.3 . . ?
C5 C2Aa C1A 113.1(16) . . ?
C5 C2Aa S2 114.9(14) . . ?
C1Aa C2Aa S2 108.4(12) . . ?
C5 C2Aa H2A 106.6 . . ?
C1Aa C2Aa H2A 106.6 . . ?
S2 C2Aa H2A 106.6 . . ?
C1Bb C2Bb S2 122(3) . . ?
C1Bb C2Bb H2B1 106.8 . . ?
S2 C2Bb H2B1 106.8 . . ?
C1Bb C2Bb H2B2 106.8 . . ?
S2 C2Bb H2B2 106.8 . . ?
H2B1b C2Bb H2B2 106.7 . . ?
C2Bb C1Bb C5 95(3) . . ?
C2Bb C1Bb S1 107(4) . . ?
C5 C1Bb S1 119(3) . . ?
C2Bb C1Bb H1B 111.3 . . ?
C5 C1Bb H1B 111.3 . . ?
S1 C1Bb H1B 111.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S3 C3 C4 S4 -2.9(12) . . . . ?
S1 C3 C4 S4 177.7(6) . . . . ?
S3 C3 C4 S2 -179.3(5) . . . . ?
S1 C3 C4 S2 1.3(15) . . . . ?
S7 C8 C9 S8 -0.7(11) . . . . ?
S5 C8 C9 S8 177.8(5) . . . . ?
S7 C8 C9 S6 -178.3(5) . . . . ?
S5 C8 C9 S6 0.2(13) . . . . ?
N1 C11 C12 C13 -156.2(14) . . . . ?
C11 C12 C13 C14 -175.7(15) . . . . ?
N1 C15 C16 C17 -165.6(9) . . . . ?
C15 C16 C17 C18 -178.3(11) . . . . ?
N1 C19 C20 C21 164.9(8) . . . . ?
C19 C20 C21 C22 -175.9(9) . . . . ?
N1 C23 C24 C25 -176.5(8) . . . . ?
C23 C24 C25 C26 73.1(14) . . . . ?
C20 C19 N1 C15 -60.7(9) . . . . ?
C20 C19 N1 C23 58.0(10) . . . . ?
C20 C19 N1 C11 179.1(8) . . . . ?
C16 C15 N1 C19 -53.0(10) . . . . ?
C16 C15 N1 C23 -173.4(9) . . . . ?
C16 C15 N1 C11 66.3(11) . . . . ?
C24 C23 N1 C19 64.1(10) . . . . ?
C24 C23 N1 C15 -175.3(8) . . . . ?
C24 C23 N1 C11 -55.6(10) . . . . ?
C12 C11 N1 C19 -177.0(9) . . . . ?
C12 C11 N1 C15 62.2(11) . . . . ?
C12 C11 N1 C23 -56.1(11) . . . . ?
C4 C3 S1 C1Aa -17.2(13) . . . . ?
S3 C3 S1 C1Aa 163.4(9) . . . . ?
C4 C3 S1 C1Bb 13.7(16) . . . . ?
S3 C3 S1 C1Bb -165.7(13) . . . . ?
C3 C4 S2 C2Bb 8.0(17) . . . . ?
S4 C4 S2 C2Bb -168.6(15) . . . . ?
C3 C4 S2 C2Aa -16.7(12) . . . . ?
S4 C4 S2 C2Aa 166.7(8) . . . . ?
C4 C3 S3 NI1 4.0(9) . . . . ?
S1 C3 S3 NI1 -176.6(5) . . . . ?
C3 C4 S4 NI1 0.3(8) . . . . ?
S2 C4 S4 NI1 177.2(3) . . . . ?
C9 C8 S5 C6 13.5(13) . . . . ?
S7 C8 S5 C6 -167.9(9) . . . . ?
C8 C9 S6 C7 -5.3(13) . . . . ?
S8 C9 S6 C7 177.0(9) . . . . ?
C9 C8 S7 NI2 0.4(9) . . . . ?
S5 C8 S7 NI2 -178.2(4) . . . . ?
C8 C9 S8 NI2 0.6(8) . . . . ?
S6 C9 S8 NI2 178.5(4) . . . . ?
C8 S5 C6 C7 -27(2) . . . . ?
C8 S5 C6 C10 87.2(18) . . . . ?
C10 C6 C7 S6 -93(3) . . . . ?
S5 C6 C7 S6 25(3) . . . . ?
C9 S6 C7 C6 -8(2) . . . . ?
C3 S1 C1Aa C2Aa 54.2(14) . . . . ?
S1 C1Aa C2Aa C5 51.6(16) . . . . ?
S1 C1Aa C2Aa S2 -77.0(15) . . . . ?
C4 S2 C2Aa C5 -74.4(14) . . . . ?
C4 S2 C2Aa C1Aa 53.2(14) . . . . ?
C4 S2 C2Bb C1Bb -53(4) . . . . ?
S2 C2Bb C1Bb C5 -50(5) . . . . ?
S2 C2Bb C1Bb S1 73(4) . . . . ?

_refine_diff_density_max         1.390
_refine_diff_density_min         -1.074
_refine_diff_density_rms         0.126

####################################################################### 
# 
# 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_shelx_CCDC6
_database_code_depnum_ccdc_archive 'CCDC 2048863'
loop_
_audit_author_name
_audit_author_address
'Narcis Avarvari'
;CNRS, University of Angers
France
;
_audit_update_record             
;
2020-12-07 deposited with the CCDC.	2021-02-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H52 N Ni S8'
_chemical_formula_sum            'C28 H52 N Ni S8'
_chemical_formula_weight         717.89

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'
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'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.9129(2)
_cell_length_b                   12.6872(4)
_cell_length_c                   15.3643(5)
_cell_angle_alpha                81.603(3)
_cell_angle_beta                 80.128(2)
_cell_angle_gamma                68.888(3)
_cell_volume                     1768.45(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    150.0(3)
_cell_measurement_reflns_used    23237
_cell_measurement_theta_min      3.7080
_cell_measurement_theta_max      75.8560

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_F_000             766
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.420
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    5.343
_shelx_estimated_absorpt_T_min   0.197
_shelx_estimated_absorpt_T_max   0.591
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.43264
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.635
_oxdiff_exptl_absorpt_empirical_full_max 1.739
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150.0(3)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_reflns_number            29990
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.932
_diffrn_reflns_theta_max         76.323
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measured_fraction_theta_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_point_group_measured_fraction_full 0.984
_reflns_number_total             7142
_reflns_number_gt                6981
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0746P)²+2.0911P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7142
_refine_ls_number_parameters     382
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0451
_refine_ls_wR_factor_ref         0.1268
_refine_ls_wR_factor_gt          0.1262
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_restrained_S_all      0.995
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C3 C -0.3538(3) 0.3970(2) 0.82321(18) 0.0361(5) Uani 1 1 d . . . . .
C4 C -0.2429(3) 0.41326(19) 0.85377(17) 0.0318(5) Uani 1 1 d . . . . .
C5 C -0.0717(7) 0.1552(3) 0.7691(3) 0.122(3) Uani 1 1 d . . . . .
H5A H -0.121833 0.099873 0.777045 0.183 Uiso 1 1 calc R U . A 1
H5B H 0.030908 0.118867 0.745767 0.183 Uiso 1 1 calc R U . A 1
H5C H -0.077736 0.183215 0.826272 0.183 Uiso 1 1 calc R U . A 1
C6 C -0.1344(8) 0.4379(4) 0.6209(3) 0.120(3) Uani 1 1 d . . . . .
H6A H -0.085697 0.494271 0.611415 0.180 Uiso 1 1 calc R U . B 1
H6B H -0.124412 0.405583 0.565006 0.180 Uiso 1 1 calc R U . B 1
H6C H -0.237975 0.474281 0.641914 0.180 Uiso 1 1 calc R U . B 1
C9 C 0.1773(3) 0.1476(2) 1.52255(16) 0.0333(5) Uani 1 1 d . . . . .
C10 C 0.2245(3) 0.0575(2) 1.58204(16) 0.0323(5) Uani 1 1 d . . . . .
C11 C 0.4978(4) 0.2873(3) 1.5010(3) 0.0585(8) Uani 1 1 d . . . . .
H11A H 0.491300 0.317323 1.438803 0.088 Uiso 1 1 calc R U . C 1
H11B H 0.444596 0.348512 1.539400 0.088 Uiso 1 1 calc R U . C 1
H11C H 0.600337 0.256134 1.511124 0.088 Uiso 1 1 calc R U . C 1
C12 C 0.6007(3) 0.0873(2) 1.6337(2) 0.0441(6) Uani 1 1 d . . . . .
H12A H 0.607536 0.056352 1.695682 0.066 Uiso 1 1 calc R U . D 1
H12B H 0.647103 0.025623 1.594908 0.066 Uiso 1 1 calc R U . D 1
H12C H 0.650198 0.143133 1.619131 0.066 Uiso 1 1 calc R U . D 1
C13 C 0.1560(3) 0.1989(2) 1.20150(17) 0.0347(5) Uani 1 1 d . . . . .
H13A H 0.225261 0.128309 1.177138 0.042 Uiso 1 1 calc R U . . .
H13B H 0.112780 0.177447 1.261410 0.042 Uiso 1 1 calc R U . . .
C14 C 0.2411(3) 0.2745(2) 1.2108(2) 0.0439(6) Uani 1 1 d . . . . .
H14A H 0.267931 0.309319 1.151423 0.053 Uiso 1 1 calc R U . . .
H14B H 0.178744 0.336457 1.247616 0.053 Uiso 1 1 calc R U . . .
C15 C 0.3775(3) 0.2081(2) 1.25276(19) 0.0390(6) Uani 1 1 d . . . . .
H15A H 0.436186 0.142899 1.218271 0.047 Uiso 1 1 calc R U . . .
H15B H 0.350065 0.177915 1.313679 0.047 Uiso 1 1 calc R U . . .
C16 C 0.4691(3) 0.2803(3) 1.2565(2) 0.0470(7) Uani 1 1 d . . . . .
H16A H 0.556376 0.234231 1.284183 0.071 Uiso 1 1 calc R U . . .
H16B H 0.498066 0.309224 1.196244 0.071 Uiso 1 1 calc R U . . .
H16C H 0.411975 0.344229 1.291619 0.071 Uiso 1 1 calc R U . . .
C17 C 0.0954(3) 0.2854(2) 1.04991(18) 0.0414(6) Uani 1 1 d . . . . .
H17A H 0.013285 0.321235 1.014378 0.050 Uiso 1 1 calc R U . . .
H17B H 0.138530 0.343574 1.053732 0.050 Uiso 1 1 calc R U . . .
C18 C 0.2094(4) 0.1902(3) 1.0009(2) 0.0509(7) Uani 1 1 d . . . . .
H18A H 0.282538 0.143426 1.040345 0.061 Uiso 1 1 calc R U . . .
H18B H 0.162609 0.140830 0.983427 0.061 Uiso 1 1 calc R U . . .
C19 C 0.2831(5) 0.2386(4) 0.9199(3) 0.0723(11) Uani 1 1 d . . . . .
H19A H 0.327645 0.288754 0.938502 0.087 Uiso 1 1 calc R U . . .
H19B H 0.208204 0.286137 0.881799 0.087 Uiso 1 1 calc R U . . .
C20 C 0.3994(5) 0.1512(5) 0.8656(2) 0.0848(15) Uani 1 1 d . . . . .
H20A H 0.441970 0.189456 0.814158 0.127 Uiso 1 1 calc R U . . .
H20B H 0.475665 0.104948 0.902117 0.127 Uiso 1 1 calc R U . . .
H20C H 0.356023 0.102326 0.845317 0.127 Uiso 1 1 calc R U . . .
C21 C -0.0338(3) 0.16162(19) 1.14135(17) 0.0330(5) Uani 1 1 d . . . . .
H21A H -0.072909 0.141844 1.202811 0.040 Uiso 1 1 calc R U . . .
H21B H 0.043349 0.092290 1.119999 0.040 Uiso 1 1 calc R U . . .
C22 C -0.1559(3) 0.1973(2) 1.08346(19) 0.0397(6) Uani 1 1 d . . . . .
H22A H -0.233829 0.266833 1.103874 0.048 Uiso 1 1 calc R U . . .
H22B H -0.117598 0.214783 1.021310 0.048 Uiso 1 1 calc R U . . .
C23 C -0.2191(3) 0.1036(2) 1.0877(2) 0.0446(6) Uani 1 1 d . . . . .
H23A H -0.259212 0.087135 1.149663 0.053 Uiso 1 1 calc R U . . .
H23B H -0.140776 0.033555 1.068453 0.053 Uiso 1 1 calc R U . . .
C24 C -0.3392(4) 0.1381(3) 1.0284(2) 0.0568(8) Uani 1 1 d . . . . .
H24A H -0.378343 0.076605 1.032075 0.085 Uiso 1 1 calc R U . . .
H24B H -0.417429 0.206758 1.047980 0.085 Uiso 1 1 calc R U . . .
H24C H -0.299149 0.153248 0.966877 0.085 Uiso 1 1 calc R U . . .
C25 C -0.0775(3) 0.3589(2) 1.1789(2) 0.0415(6) Uani 1 1 d . . . . .
H25A H -0.027134 0.412940 1.181142 0.050 Uiso 1 1 calc R U . . .
H25B H -0.149779 0.393930 1.136612 0.050 Uiso 1 1 calc R U . . .
C26 C -0.1578(4) 0.3428(3) 1.2694(2) 0.0574(8) Uani 1 1 d . . . . .
H26A H -0.227854 0.305216 1.264724 0.069 Uiso 1 1 calc R U . . .
H26B H -0.087221 0.292259 1.309030 0.069 Uiso 1 1 calc R U . . .
C27 C -0.2381(7) 0.4523(4) 1.3092(3) 0.106(2) Uani 1 1 d D . . . .
H27A H -0.168955 0.493435 1.305170 0.127 Uiso 1 1 calc R U . . .
H27B H -0.314739 0.498193 1.271820 0.127 Uiso 1 1 calc R U . . .
C28 C -0.2998(10) 0.4491(6) 1.3912(5) 0.077(2) Uani 0.5 1 d D U P . .
H28A H -0.348244 0.526624 1.408455 0.116 Uiso 0.5 1 calc R U P . .
H28B H -0.372054 0.411542 1.396621 0.116 Uiso 0.5 1 calc R U P . .
H28C H -0.225570 0.406762 1.430130 0.116 Uiso 0.5 1 calc R U P . .
N1 N 0.0348(2) 0.25078(16) 1.14301(14) 0.0329(4) Uani 1 1 d . . . . .
S1 S -0.34678(9) 0.33617(9) 0.72631(6) 0.0617(2) Uani 1 1 d . . . . .
S2 S -0.06066(7) 0.37809(6) 0.80473(5) 0.04573(18) Uani 1 1 d . . . . .
S3 S -0.52601(7) 0.43824(6) 0.88398(4) 0.03881(16) Uani 1 1 d . . . . .
S4 S -0.27496(6) 0.47526(5) 0.95235(4) 0.02866(13) Uani 1 1 d . . . . .
S5 S 0.23866(8) 0.26400(5) 1.50112(5) 0.04143(16) Uani 1 1 d . . . . .
S6 S 0.35690(7) 0.03599(6) 1.65154(4) 0.04151(16) Uani 1 1 d . . . . .
S7 S 0.04574(7) 0.15463(5) 1.45864(4) 0.03671(15) Uani 1 1 d . . . . .
S8 S 0.15467(6) -0.05212(5) 1.59399(4) 0.03435(15) Uani 1 1 d . . . . .
NI1 Ni -0.500000 0.500000 1.000000 0.02528(13) Uani 1 2 d S . P . .
NI2 Ni 0.000000 0.000000 1.500000 0.03178(15) Uani 1 2 d S . P . .
C1A C -0.1492(8) 0.2617(6) 0.6990(5) 0.0494(15) Uani 0.5 1 d . . P E 1
H1A H -0.132626 0.232419 0.639603 0.059 Uiso 0.5 1 calc R U P E 1
C2A C -0.0609(6) 0.3389(6) 0.6936(4) 0.0430(12) Uani 0.5 1 d . . P E 1
H2A H 0.041949 0.297514 0.668754 0.052 Uiso 0.5 1 calc R U P E 1
C7A C 0.4302(6) 0.1927(5) 1.5228(4) 0.0327(10) Uani 0.5 1 d . . P F 1
H7A H 0.481453 0.130854 1.482645 0.039 Uiso 0.5 1 calc R U P F 1
C8A C 0.4394(6) 0.1447(5) 1.6199(4) 0.0334(11) Uani 0.5 1 d . . P F 1
H8A H 0.391687 0.207660 1.659415 0.040 Uiso 0.5 1 calc R U P F 1
C8B C 0.4715(6) 0.1110(5) 1.5820(5) 0.0367(12) Uani 0.5 1 d . . P F 2
H8B H 0.509336 0.075147 1.524788 0.044 Uiso 0.5 1 calc R U P F 2
C7B C 0.3895(7) 0.2339(6) 1.5616(5) 0.0451(13) Uani 0.5 1 d . . P F 2
H7B H 0.354482 0.271520 1.618107 0.054 Uiso 0.5 1 calc R U P F 2
C2B C -0.0498(7) 0.2743(6) 0.7307(4) 0.0501(15) Uani 0.5 1 d . . P E 2
H2B H 0.046516 0.256894 0.692310 0.060 Uiso 0.5 1 calc R U P E 2
C1B C -0.1694(8) 0.3227(7) 0.6698(5) 0.0530(16) Uani 0.5 1 d . . P E 2
H1B H -0.146937 0.268901 0.623477 0.064 Uiso 0.5 1 calc R U P E 2


_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
C3 C4 1.356(4) . ?
C3 S3 1.736(3) . ?
C3 S1 1.755(3) . ?
C4 S4 1.737(2) . ?
C4 S2 1.755(2) . ?
C5 C2B 1.616(8) . ?
C5 C1A 1.639(10) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C2A 1.601(8) . ?
C6 C1B 1.666(9) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C9 C10 1.348(4) . ?
C9 S7 1.733(3) . ?
C9 S5 1.759(3) . ?
C10 S8 1.738(3) . ?
C10 S6 1.754(2) . ?
C11 C7A 1.546(6) . ?
C11 C7B 1.573(7) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C8B 1.537(6) . ?
C12 C8A 1.537(6) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 N1 1.520(3) . ?
C13 C14 1.523(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.508(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.516(4) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.514(5) . ?
C17 N1 1.520(3) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.500(4) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.508(7) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 N1 1.520(3) . ?
C21 C22 1.523(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.520(3) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.523(4) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.504(5) . ?
C25 N1 1.528(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.491(5) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.304(8) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
S1 C1B 1.783(7) . ?
S1 C1A 1.845(7) . ?
S2 C2B 1.825(7) . ?
S2 C2A 1.848(6) . ?
S3 NI1 2.1375(6) . ?
S4 NI1 2.1479(5) . ?
S5 C7B 1.791(6) . ?
S5 C7A 1.850(5) . ?
S6 C8A 1.814(6) . ?
S6 C8B 1.845(6) . ?
S7 NI2 2.1532(7) . ?
S8 NI2 2.1502(6) . ?
NI1 S3 2.1374(6) 2_467 ?
NI1 S4 2.1479(5) 2_467 ?
NI2 S8 2.1502(6) 2_558 ?
NI2 S7 2.1532(7) 2_558 ?
C1Aa C2A 1.518(9) . ?
C1Aa H1A 1.0000 . ?
C2Aa H2A 1.0000 . ?
C7Aa C8A 1.532(8) . ?
C7Aa H7A 1.0000 . ?
C8Aa H8A 1.0000 . ?
C8Bb C7B 1.491(9) . ?
C8Bb H8B 1.0000 . ?
C7Bb H7B 1.0000 . ?
C2Bb C1B 1.532(11) . ?
C2Bb H2B 1.0000 . ?
C1Bb H1B 1.0000 . ?

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
C4 C3 S3 119.2(2) . . ?
C4 C3 S1 127.7(2) . . ?
S3 C3 S1 113.14(15) . . ?
C3 C4 S4 119.81(19) . . ?
C3 C4 S2 127.4(2) . . ?
S4 C4 S2 112.74(14) . . ?
C1Aa C5 H5A 109.5 . . ?
C1Aa C5 H5B 109.5 . . ?
H5Aa C5 H5B 109.5 . . ?
C1Aa C5 H5C 109.5 . . ?
H5Aa C5 H5C 109.5 . . ?
H5Ba C5 H5C 109.5 . . ?
C2Aa C6 H6A 109.5 . . ?
C2Aa C6 H6B 109.5 . . ?
H6Aa C6 H6B 109.5 . . ?
C2Aa C6 H6C 109.5 . . ?
H6Aa C6 H6C 109.5 . . ?
H6Ba C6 H6C 109.5 . . ?
C10 C9 S7 119.9(2) . . ?
C10 C9 S5 125.8(2) . . ?
S7 C9 S5 114.35(14) . . ?
C9 C10 S8 120.08(19) . . ?
C9 C10 S6 126.1(2) . . ?
S8 C10 S6 113.86(14) . . ?
C7Aa C11 H11A 109.5 . . ?
C7Aa C11 H11B 109.5 . . ?
H11Aa C11 H11B 109.5 . . ?
C7Aa C11 H11C 109.5 . . ?
H11Aa C11 H11C 109.5 . . ?
H11Ba C11 H11C 109.5 . . ?
C8Aa C12 H12A 109.5 . . ?
C8Aa C12 H12B 109.5 . . ?
H12Aa C12 H12B 109.5 . . ?
C8Aa C12 H12C 109.5 . . ?
H12Aa C12 H12C 109.5 . . ?
H12Ba C12 H12C 109.5 . . ?
N1 C13 C14 115.49(19) . . ?
N1 C13 H13A 108.4 . . ?
C14 C13 H13A 108.4 . . ?
N1 C13 H13B 108.4 . . ?
C14 C13 H13B 108.4 . . ?
H13A C13 H13B 107.5 . . ?
C15 C14 C13 111.3(2) . . ?
C15 C14 H14A 109.4 . . ?
C13 C14 H14A 109.4 . . ?
C15 C14 H14B 109.4 . . ?
C13 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
C14 C15 C16 112.0(2) . . ?
C14 C15 H15A 109.2 . . ?
C16 C15 H15A 109.2 . . ?
C14 C15 H15B 109.2 . . ?
C16 C15 H15B 109.2 . . ?
H15A C15 H15B 107.9 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 N1 115.5(2) . . ?
C18 C17 H17A 108.4 . . ?
N1 C17 H17A 108.4 . . ?
C18 C17 H17B 108.4 . . ?
N1 C17 H17B 108.4 . . ?
H17A C17 H17B 107.5 . . ?
C19 C18 C17 109.8(3) . . ?
C19 C18 H18A 109.7 . . ?
C17 C18 H18A 109.7 . . ?
C19 C18 H18B 109.7 . . ?
C17 C18 H18B 109.7 . . ?
H18A C18 H18B 108.2 . . ?
C18 C19 C20 114.5(4) . . ?
C18 C19 H19A 108.6 . . ?
C20 C19 H19A 108.6 . . ?
C18 C19 H19B 108.6 . . ?
C20 C19 H19B 108.6 . . ?
H19A C19 H19B 107.6 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N1 C21 C22 114.80(18) . . ?
N1 C21 H21A 108.6 . . ?
C22 C21 H21A 108.6 . . ?
N1 C21 H21B 108.6 . . ?
C22 C21 H21B 108.6 . . ?
H21A C21 H21B 107.5 . . ?
C23 C22 C21 110.7(2) . . ?
C23 C22 H22A 109.5 . . ?
C21 C22 H22A 109.5 . . ?
C23 C22 H22B 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 108.1 . . ?
C22 C23 C24 110.8(2) . . ?
C22 C23 H23A 109.5 . . ?
C24 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C24 C23 H23B 109.5 . . ?
H23A C23 H23B 108.1 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 N1 115.3(2) . . ?
C26 C25 H25A 108.4 . . ?
N1 C25 H25A 108.4 . . ?
C26 C25 H25B 108.4 . . ?
N1 C25 H25B 108.4 . . ?
H25A C25 H25B 107.5 . . ?
C27 C26 C25 112.3(3) . . ?
C27 C26 H26A 109.1 . . ?
C25 C26 H26A 109.1 . . ?
C27 C26 H26B 109.1 . . ?
C25 C26 H26B 109.1 . . ?
H26A C26 H26B 107.9 . . ?
C28 C27 C26 118.4(5) . . ?
C28 C27 H27A 107.7 . . ?
C26 C27 H27A 107.7 . . ?
C28 C27 H27B 107.7 . . ?
C26 C27 H27B 107.7 . . ?
H27A C27 H27B 107.1 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C17 N1 C21 110.83(19) . . ?
C17 N1 C13 110.6(2) . . ?
C21 N1 C13 107.08(17) . . ?
C17 N1 C25 106.4(2) . . ?
C21 N1 C25 111.4(2) . . ?
C13 N1 C25 110.61(19) . . ?
C3 S1 C1B 103.5(3) . . ?
C3 S1 C1A 102.0(2) . . ?
C4 S2 C2B 101.1(2) . . ?
C4 S2 C2A 104.6(2) . . ?
C3 S3 NI1 105.05(9) . . ?
C4 S4 NI1 104.45(8) . . ?
C9 S5 C7B 108.2(2) . . ?
C9 S5 C7A 99.95(18) . . ?
C10 S6 C8A 108.8(2) . . ?
C10 S6 C8B 100.5(2) . . ?
C9 S7 NI2 104.33(9) . . ?
C10 S8 NI2 104.16(8) . . ?
S3 NI1 S3 180.0 2_467 . ?
S3 NI1 S4 91.35(2) 2_467 2_467 ?
S3 NI1 S4 88.65(2) . 2_467 ?
S3 NI1 S4 88.65(2) 2_467 . ?
S3 NI1 S4 91.35(2) . . ?
S4 NI1 S4 180.0 2_467 . ?
S8 NI2 S8 180.00(2) 2_558 . ?
S8 NI2 S7 88.46(2) 2_558 . ?
S8 NI2 S7 91.54(2) . . ?
S8 NI2 S7 91.54(2) 2_558 2_558 ?
S8 NI2 S7 88.46(2) . 2_558 ?
S7 NI2 S7 180.0 . 2_558 ?
C2Aa C1Aa C5 103.3(6) . . ?
C2Aa C1Aa S1 112.6(5) . . ?
C5 C1Aa S1 116.6(4) . . ?
C2Aa C1Aa H1A 108.0 . . ?
C5 C1Aa H1A 108.0 . . ?
S1 C1Aa H1A 108.0 . . ?
C1Aa C2Aa C6 101.7(6) . . ?
C1Aa C2Aa S2 110.9(4) . . ?
C6 C2Aa S2 118.1(4) . . ?
C1Aa C2Aa H2A 108.6 . . ?
C6 C2Aa H2A 108.6 . . ?
S2 C2Aa H2A 108.6 . . ?
C8Aa C7Aa C11 110.2(4) . . ?
C8Aa C7Aa S5 111.5(4) . . ?
C11 C7Aa S5 104.4(3) . . ?
C8Aa C7Aa H7A 110.2 . . ?
C11 C7Aa H7A 110.2 . . ?
S5 C7Aa H7A 110.2 . . ?
C7Aa C8Aa C12 109.0(4) . . ?
C7Aa C8Aa S6 112.8(4) . . ?
C12 C8Aa S6 106.0(3) . . ?
C7Aa C8Aa H8A 109.7 . . ?
C12 C8Aa H8A 109.7 . . ?
S6 C8Aa H8A 109.7 . . ?
C7Bb C8Bb C12 114.1(5) . . ?
C7Bb C8Bb S6 112.6(5) . . ?
C12 C8Bb S6 104.6(4) . . ?
C7Bb C8Bb H8B 108.5 . . ?
C12 C8Bb H8B 108.5 . . ?
S6 C8Bb H8B 108.5 . . ?
C8Bb C7Bb C11 107.6(5) . . ?
C8Bb C7Bb S5 115.0(5) . . ?
C11 C7Bb S5 106.0(4) . . ?
C8Bb C7Bb H7B 109.4 . . ?
C11 C7Bb H7B 109.4 . . ?
S5 C7Bb H7B 109.4 . . ?
C1Bb C2Bb C5 100.5(6) . . ?
C1Bb C2Bb S2 111.1(4) . . ?
C5 C2Bb S2 121.2(4) . . ?
C1Bb C2Bb H2B 107.8 . . ?
C5 C2Bb H2B 107.8 . . ?
S2 C2Bb H2B 107.8 . . ?
C2Bb C1Bb C6 100.6(6) . . ?
C2Bb C1Bb S1 113.2(5) . . ?
C6 C1Bb S1 119.7(5) . . ?
C2Bb C1Bb H1B 107.5 . . ?
C6 C1Bb H1B 107.5 . . ?
S1 C1Bb H1B 107.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S3 C3 C4 S4 -0.3(3) . . . . ?
S1 C3 C4 S4 -179.79(15) . . . . ?
S3 C3 C4 S2 179.61(14) . . . . ?
S1 C3 C4 S2 0.1(4) . . . . ?
S7 C9 C10 S8 0.5(3) . . . . ?
S5 C9 C10 S8 -178.94(13) . . . . ?
S7 C9 C10 S6 179.66(13) . . . . ?
S5 C9 C10 S6 0.2(4) . . . . ?
N1 C13 C14 C15 -167.7(2) . . . . ?
C13 C14 C15 C16 176.0(3) . . . . ?
N1 C17 C18 C19 -167.4(2) . . . . ?
C17 C18 C19 C20 180.0(3) . . . . ?
N1 C21 C22 C23 -178.9(2) . . . . ?
C21 C22 C23 C24 -178.9(3) . . . . ?
N1 C25 C26 C27 166.3(3) . . . . ?
C25 C26 C27 C28 -173.0(7) . . . . ?
C18 C17 N1 C21 -58.4(3) . . . . ?
C18 C17 N1 C13 60.2(3) . . . . ?
C18 C17 N1 C25 -179.7(2) . . . . ?
C22 C21 N1 C17 -57.7(3) . . . . ?
C22 C21 N1 C13 -178.4(2) . . . . ?
C22 C21 N1 C25 60.6(3) . . . . ?
C14 C13 N1 C17 58.1(3) . . . . ?
C14 C13 N1 C21 179.0(2) . . . . ?
C14 C13 N1 C25 -59.5(3) . . . . ?
C26 C25 N1 C17 176.7(2) . . . . ?
C26 C25 N1 C21 55.8(3) . . . . ?
C26 C25 N1 C13 -63.1(3) . . . . ?
C4 C3 S1 C1Bb -9.1(4) . . . . ?
S3 C3 S1 C1Bb 171.4(3) . . . . ?
C4 C3 S1 C1Aa 17.3(4) . . . . ?
S3 C3 S1 C1Aa -162.2(3) . . . . ?
C3 C4 S2 C2Bb -19.2(3) . . . . ?
S4 C4 S2 C2Bb 160.7(3) . . . . ?
C3 C4 S2 C2Aa 10.0(3) . . . . ?
S4 C4 S2 C2Aa -170.1(2) . . . . ?
C4 C3 S3 NI1 -2.5(2) . . . . ?
S1 C3 S3 NI1 177.02(12) . . . . ?
C3 C4 S4 NI1 2.9(2) . . . . ?
S2 C4 S4 NI1 -176.97(10) . . . . ?
C10 C9 S5 C7Bb 7.0(4) . . . . ?
S7 C9 S5 C7Bb -172.5(3) . . . . ?
C10 C9 S5 C7Aa 32.0(3) . . . . ?
S7 C9 S5 C7Aa -147.6(2) . . . . ?
C9 C10 S6 C8Aa -8.0(3) . . . . ?
S8 C10 S6 C8Aa 171.2(2) . . . . ?
C9 C10 S6 C8Bb -30.2(3) . . . . ?
S8 C10 S6 C8Bb 149.0(3) . . . . ?
C10 C9 S7 NI2 -0.5(2) . . . . ?
S5 C9 S7 NI2 178.99(10) . . . . ?
C9 C10 S8 NI2 -0.2(2) . . . . ?
S6 C10 S8 NI2 -179.46(10) . . . . ?
C3 S1 C1Aa C2Aa -53.5(6) . . . . ?
C3 S1 C1Aa C5 65.7(5) . . . . ?
C5 C1Aa C2Aa C6 177.1(4) . . . . ?
S1 C1Aa C2Aa C6 -56.2(5) . . . . ?
C5 C1Aa C2Aa S2 -56.4(5) . . . . ?
S1 C1Aa C2Aa S2 70.3(6) . . . . ?
C4 S2 C2Aa C1Aa -45.0(5) . . . . ?
C4 S2 C2Aa C6 71.7(5) . . . . ?
C9 S5 C7Aa C8Aa -63.9(4) . . . . ?
C9 S5 C7Aa C11 177.2(3) . . . . ?
C11 C7Aa C8Aa C12 -64.4(6) . . . . ?
S5 C7Aa C8Aa C12 -179.8(3) . . . . ?
C11 C7Aa C8Aa S6 178.2(3) . . . . ?
S5 C7Aa C8Aa S6 62.8(5) . . . . ?
C10 S6 C8Aa C7Aa -25.4(5) . . . . ?
C10 S6 C8Aa C12 -144.6(3) . . . . ?
C10 S6 C8Bb C7Bb 60.9(5) . . . . ?
C10 S6 C8Bb C12 -174.7(3) . . . . ?
C12 C8Bb C7Bb C11 62.0(7) . . . . ?
S6 C8Bb C7Bb C11 -179.0(4) . . . . ?
C12 C8Bb C7Bb S5 179.8(4) . . . . ?
S6 C8Bb C7Bb S5 -61.2(7) . . . . ?
C9 S5 C7Bb C8Bb 25.5(6) . . . . ?
C9 S5 C7Bb C11 144.2(3) . . . . ?
C4 S2 C2Bb C1Bb 53.8(5) . . . . ?
C4 S2 C2Bb C5 -63.6(5) . . . . ?
C5 C2Bb C1Bb C6 -173.5(4) . . . . ?
S2 C2Bb C1Bb C6 57.0(5) . . . . ?
C5 C2Bb C1Bb S1 57.5(5) . . . . ?
S2 C2Bb C1Bb S1 -72.0(6) . . . . ?
C3 S1 C1Bb C2Bb 45.2(6) . . . . ?
C3 S1 C1Bb C6 -73.2(5) . . . . ?

_refine_diff_density_max         1.887
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.075

####################################################################### 
# 
# 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_shelx_CCDC7
_database_code_depnum_ccdc_archive 'CCDC 2048864'
loop_
_audit_author_name
_audit_author_address
'Narcis Avarvari'
;CNRS, University of Angers
France
;
_audit_update_record             
;
2020-12-07 deposited with the CCDC.	2021-02-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H12 N, C12 H16 Ni S8'
_chemical_formula_sum            'C16 H28 N Ni S8'
_chemical_formula_weight         549.58

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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'I 2'
_space_group_name_Hall           'I 2y'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   17.5736(4)
_cell_length_b                   9.9714(2)
_cell_length_c                   15.7038(4)
_cell_angle_alpha                90
_cell_angle_beta                 119.990(3)
_cell_angle_gamma                90
_cell_volume                     2383.39(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.01(10)
_cell_measurement_reflns_used    8671
_cell_measurement_theta_min      3.0330
_cell_measurement_theta_max      71.9030

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_F_000             1148
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    7.745
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.65254
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.837
_oxdiff_exptl_absorpt_empirical_full_max 1.296
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150.01(10)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_reflns_number            10593
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_av_R_equivalents  0.0186
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.091
_diffrn_reflns_theta_max         72.063
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_point_group_measured_fraction_full 0.982
_reflns_number_total             4505
_reflns_number_gt                4450
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.828
_reflns_Friedel_fraction_max     0.927
_reflns_Friedel_fraction_full    0.964

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

_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0459P)²+3.8163P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1958 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.022(10)
_chemical_absolute_configuration syn
_refine_ls_number_reflns         4505
_refine_ls_number_parameters     226
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0301
_refine_ls_wR_factor_ref         0.0856
_refine_ls_wR_factor_gt          0.0851
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2162(3) 0.1141(5) 0.6271(3) 0.0275(9) Uani 1 1 d . . . . .
H1 H 0.234682 0.068127 0.689605 0.033 Uiso 1 1 calc R U . . .
C2 C 0.2680(3) 0.0580(5) 0.5810(3) 0.0277(9) Uani 1 1 d . . . . .
H2 H 0.251655 0.105657 0.519627 0.033 Uiso 1 1 calc R U . . .
C3 C 0.3391(3) 0.3316(5) 0.6796(3) 0.0249(10) Uani 1 1 d . . . . .
C4 C 0.4013(3) 0.2436(6) 0.6846(3) 0.0228(9) Uani 1 1 d . . . . .
C5 C 0.6020(3) 0.7773(6) 0.8125(3) 0.0222(10) Uani 1 1 d . . . . .
C6 C 0.6639(3) 0.6913(5) 0.8180(3) 0.0243(10) Uani 1 1 d . . . . .
C7 C 0.7241(3) 0.9935(4) 0.8579(3) 0.0269(8) Uani 1 1 d . . . . .
H7 H 0.725833 1.003095 0.796767 0.032 Uiso 1 1 calc R U . . .
C8 C 0.7892(3) 0.8860(4) 0.9203(3) 0.0255(8) Uani 1 1 d . . . . .
H8 H 0.781196 0.865581 0.976439 0.031 Uiso 1 1 calc R U . . .
C9 C 0.1165(3) 0.0976(7) 0.5604(4) 0.0354(12) Uani 1 1 d . . . . .
H9A H 0.086961 0.134266 0.592614 0.053 Uiso 1 1 calc R U . . .
H9B H 0.097795 0.144053 0.499595 0.053 Uiso 1 1 calc R U . . .
H9C H 0.102480 0.004054 0.547412 0.053 Uiso 1 1 calc R U . . .
C10 C 0.2513(3) -0.0924(6) 0.5606(5) 0.0407(13) Uani 1 1 d . . . . .
H10A H 0.284586 -0.125143 0.531632 0.061 Uiso 1 1 calc R U . . .
H10B H 0.268897 -0.139009 0.621125 0.061 Uiso 1 1 calc R U . . .
H10C H 0.189843 -0.107424 0.516140 0.061 Uiso 1 1 calc R U . . .
C11 C 0.7424(4) 1.1306(6) 0.9085(5) 0.0432(14) Uani 1 1 d . . . . .
H11A H 0.699081 1.193925 0.865286 0.065 Uiso 1 1 calc R U . . .
H11B H 0.739766 1.122943 0.967913 0.065 Uiso 1 1 calc R U . . .
H11C H 0.799752 1.160921 0.923984 0.065 Uiso 1 1 calc R U . . .
C12 C 0.8842(3) 0.9249(6) 0.9579(4) 0.0318(11) Uani 1 1 d . . . . .
H12A H 0.922003 0.853074 0.996724 0.048 Uiso 1 1 calc R U . . .
H12B H 0.892826 0.942050 0.903113 0.048 Uiso 1 1 calc R U . . .
H12C H 0.897925 1.004278 0.997507 0.048 Uiso 1 1 calc R U . . .
C13 C 0.4851(4) 0.8064(6) 0.5686(4) 0.0353(11) Uani 1 1 d . U . . .
H13A H 0.434849 0.749918 0.531462 0.053 Uiso 1 1 calc R U . . .
H13B H 0.535911 0.751717 0.607211 0.053 Uiso 1 1 calc R U . . .
H13C H 0.474842 0.863095 0.611266 0.053 Uiso 1 1 calc R U . . .
C14 C 0.5775(5) 0.9774(8) 0.5581(5) 0.069(2) Uani 1 1 d . U . . .
H14A H 0.628288 0.922369 0.596162 0.104 Uiso 1 1 calc R U . . .
H14B H 0.587193 1.033007 0.514492 0.104 Uiso 1 1 calc R U . . .
H14C H 0.567358 1.033008 0.601356 0.104 Uiso 1 1 calc R U . . .
C15 C 0.5181(6) 0.2011(11) 0.9365(6) 0.077(2) Uiso 1 1 d . . . . .
H15A H 0.571958 0.249056 0.976057 0.115 Uiso 1 1 calc R U . . .
H15B H 0.523464 0.147390 0.889023 0.115 Uiso 1 1 calc R U . . .
H15C H 0.470813 0.263803 0.903132 0.115 Uiso 1 1 calc R U . . .
C16 C 0.4232(13) 0.051(3) 0.937(2) 0.365(19) Uiso 1 1 d D . . . .
H16A H 0.379008 0.117643 0.900516 0.548 Uiso 1 1 calc R U . . .
H16B H 0.431725 -0.003545 0.892142 0.548 Uiso 1 1 calc R U . . .
H16C H 0.404764 -0.003550 0.973408 0.548 Uiso 1 1 calc R U . . .
N1 N 0.500000 0.8909(6) 0.500000 0.0268(12) Uani 1 2 d S T P . .
N2 N 0.500000 0.1136(10) 1.000000 0.050(2) Uani 1 2 d DS T P . .
NI1 Ni 0.50210(6) 0.51025(13) 0.75002(6) 0.02145(16) Uani 1 1 d . . . . .
S1 S 0.23139(9) 0.29388(17) 0.64906(14) 0.0474(4) Uani 1 1 d . . . . .
S2 S 0.38620(8) 0.07056(14) 0.66381(10) 0.0309(3) Uani 1 1 d . . . . .
S3 S 0.36465(7) 0.49938(13) 0.70393(9) 0.0274(3) Uani 1 1 d . . . . .
S4 S 0.50585(7) 0.30132(12) 0.71867(8) 0.0247(3) Uani 1 1 d . . . . .
S5 S 0.49890(7) 0.71890(12) 0.78388(8) 0.0240(3) Uani 1 1 d . . . . .
S6 S 0.63840(7) 0.52212(13) 0.79207(9) 0.0273(3) Uani 1 1 d . . . . .
S7 S 0.61177(7) 0.95248(13) 0.82703(10) 0.0293(3) Uani 1 1 d . . . . .
S8 S 0.77097(8) 0.73346(14) 0.84775(10) 0.0318(3) 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
C1 C2 1.525(6) . ?
C1 C9 1.536(6) . ?
C1 S1 1.820(5) . ?
C1 H1 0.9800 . ?
C2 C10 1.531(7) . ?
C2 S2 1.822(4) . ?
C2 H2 0.9800 . ?
C3 C4 1.373(7) . ?
C3 S3 1.725(5) . ?
C3 S1 1.746(5) . ?
C4 S4 1.736(5) . ?
C4 S2 1.752(6) . ?
C5 C6 1.353(7) . ?
C5 S5 1.735(4) . ?
C5 S7 1.759(6) . ?
C6 S6 1.741(5) . ?
C6 S8 1.749(5) . ?
C7 C8 1.516(6) . ?
C7 C11 1.532(7) . ?
C7 S7 1.828(4) . ?
C7 H7 0.9800 . ?
C8 C12 1.518(6) . ?
C8 S8 1.831(4) . ?
C8 H8 0.9800 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 N1 1.491(6) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 N1 1.480(6) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 N2 1.474(11) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 N2 1.360(19) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
N1 C14 1.480(6) 2_656 ?
N1 C13 1.491(6) 2_656 ?
N2 C16 1.360(19) 2_657 ?
N2 C15 1.474(11) 2_657 ?
NI1 S6 2.1462(14) . ?
NI1 S4 2.1493(18) . ?
NI1 S3 2.1499(14) . ?
NI1 S5 2.1551(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C9 112.7(4) . . ?
C2 C1 S1 112.7(3) . . ?
C9 C1 S1 104.1(4) . . ?
C2 C1 H1 109.1 . . ?
C9 C1 H1 109.1 . . ?
S1 C1 H1 109.1 . . ?
C1 C2 C10 111.2(4) . . ?
C1 C2 S2 112.0(3) . . ?
C10 C2 S2 104.4(3) . . ?
C1 C2 H2 109.7 . . ?
C10 C2 H2 109.7 . . ?
S2 C2 H2 109.7 . . ?
C4 C3 S3 119.7(4) . . ?
C4 C3 S1 126.9(4) . . ?
S3 C3 S1 113.4(3) . . ?
C3 C4 S4 119.7(4) . . ?
C3 C4 S2 125.3(4) . . ?
S4 C4 S2 115.0(3) . . ?
C6 C5 S5 120.4(4) . . ?
C6 C5 S7 126.7(4) . . ?
S5 C5 S7 112.9(3) . . ?
C5 C6 S6 119.6(4) . . ?
C5 C6 S8 126.0(4) . . ?
S6 C6 S8 114.4(3) . . ?
C8 C7 C11 113.6(4) . . ?
C8 C7 S7 112.2(3) . . ?
C11 C7 S7 104.8(3) . . ?
C8 C7 H7 108.7 . . ?
C11 C7 H7 108.7 . . ?
S7 C7 H7 108.7 . . ?
C7 C8 C12 113.5(4) . . ?
C7 C8 S8 110.1(3) . . ?
C12 C8 S8 105.7(3) . . ?
C7 C8 H8 109.2 . . ?
C12 C8 H8 109.2 . . ?
S8 C8 H8 109.2 . . ?
C1 C9 H9A 109.5 . . ?
C1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C2 C10 H10A 109.5 . . ?
C2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C7 C11 H11A 109.5 . . ?
C7 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C7 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C8 C12 H12A 109.5 . . ?
C8 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C8 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N1 C13 H13A 109.5 . . ?
N1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N1 C14 H14A 109.5 . . ?
N1 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N1 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N2 C15 H15A 109.5 . . ?
N2 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N2 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N2 C16 H16A 109.5 . . ?
N2 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N2 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 N1 C14 108.7(8) . 2_656 ?
C14 N1 C13 109.6(3) . 2_656 ?
C14 N1 C13 108.9(3) 2_656 2_656 ?
C14 N1 C13 108.9(3) . . ?
C14 N1 C13 109.6(3) 2_656 . ?
C13 N1 C13 111.1(6) 2_656 . ?
C16 N2 C16 126(3) . 2_657 ?
C16 N2 C15 106.9(13) . 2_657 ?
C16 N2 C15 104.3(13) 2_657 2_657 ?
C16 N2 C15 104.3(13) . . ?
C16 N2 C15 106.9(13) 2_657 . ?
C15 N2 C15 107.5(10) 2_657 . ?
S6 NI1 S4 88.09(6) . . ?
S6 NI1 S3 178.48(7) . . ?
S4 NI1 S3 91.83(6) . . ?
S6 NI1 S5 91.93(6) . . ?
S4 NI1 S5 179.06(6) . . ?
S3 NI1 S5 88.18(6) . . ?
C3 S1 C1 107.5(2) . . ?
C4 S2 C2 102.3(2) . . ?
C3 S3 NI1 104.35(18) . . ?
C4 S4 NI1 104.1(2) . . ?
C5 S5 NI1 103.6(2) . . ?
C6 S6 NI1 104.04(17) . . ?
C5 S7 C7 106.2(2) . . ?
C6 S8 C8 101.3(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 C1 C2 C10 -60.7(6) . . . . ?
S1 C1 C2 C10 -178.2(3) . . . . ?
C9 C1 C2 S2 -177.0(4) . . . . ?
S1 C1 C2 S2 65.6(4) . . . . ?
S3 C3 C4 S4 1.8(6) . . . . ?
S1 C3 C4 S4 -178.9(3) . . . . ?
S3 C3 C4 S2 179.0(3) . . . . ?
S1 C3 C4 S2 -1.7(7) . . . . ?
S5 C5 C6 S6 2.3(5) . . . . ?
S7 C5 C6 S6 -175.1(3) . . . . ?
S5 C5 C6 S8 -178.9(3) . . . . ?
S7 C5 C6 S8 3.7(6) . . . . ?
C11 C7 C8 C12 -54.0(6) . . . . ?
S7 C7 C8 C12 -172.7(3) . . . . ?
C11 C7 C8 S8 -172.2(4) . . . . ?
S7 C7 C8 S8 69.1(4) . . . . ?
C4 C3 S1 C1 1.2(5) . . . . ?
S3 C3 S1 C1 -179.5(3) . . . . ?
C2 C1 S1 C3 -34.0(4) . . . . ?
C9 C1 S1 C3 -156.4(3) . . . . ?
C3 C4 S2 C2 27.1(5) . . . . ?
S4 C4 S2 C2 -155.6(3) . . . . ?
C1 C2 S2 C4 -59.6(4) . . . . ?
C10 C2 S2 C4 -179.9(3) . . . . ?
C4 C3 S3 NI1 -5.1(4) . . . . ?
S1 C3 S3 NI1 175.5(2) . . . . ?
C3 C4 S4 NI1 2.5(4) . . . . ?
S2 C4 S4 NI1 -175.0(2) . . . . ?
C6 C5 S5 NI1 -5.9(4) . . . . ?
S7 C5 S5 NI1 171.84(19) . . . . ?
C5 C6 S6 NI1 2.6(4) . . . . ?
S8 C6 S6 NI1 -176.3(2) . . . . ?
C6 C5 S7 C7 -3.1(5) . . . . ?
S5 C5 S7 C7 179.4(2) . . . . ?
C8 C7 S7 C5 -34.7(4) . . . . ?
C11 C7 S7 C5 -158.5(3) . . . . ?
C5 C6 S8 C8 25.4(5) . . . . ?
S6 C6 S8 C8 -155.8(3) . . . . ?
C7 C8 S8 C6 -62.0(3) . . . . ?
C12 C8 S8 C6 175.1(3) . . . . ?

_refine_diff_density_max         1.514
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.074

####################################################################### 
# 
# 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_shelx_CCDC8
_database_code_depnum_ccdc_archive 'CCDC 2048858'
loop_
_audit_author_name
_audit_author_address
'Narcis Avarvari'
;CNRS, University of Angers
France
;
_audit_update_record             
;
2020-12-07 deposited with the CCDC.	2021-02-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H36 N, Ni C10 H12 S8'
_chemical_formula_sum            'C26 H48 N Ni S8'
_chemical_formula_weight         689.84

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'
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'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_H-M_alt        'P 1'
_space_group_name_Hall           'P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'

_cell_length_a                   9.3775(4)
_cell_length_b                   13.5118(4)
_cell_length_c                   13.7352(5)
_cell_angle_alpha                83.682(3)
_cell_angle_beta                 77.681(3)
_cell_angle_gamma                87.481(3)
_cell_volume                     1689.57(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    150.03(13)
_cell_measurement_reflns_used    3440
_cell_measurement_theta_min      3.2420
_cell_measurement_theta_max      70.6580

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_F_000             734
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    5.571
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.86896
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.349
_oxdiff_exptl_absorpt_empirical_full_max 1.495
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150.00(10)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_reflns_number            28197
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.292
_diffrn_reflns_theta_max         73.696
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_point_group_measured_fraction_full 0.953
_reflns_number_total             12527
_reflns_number_gt                9826
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.891
_reflns_Friedel_fraction_max     0.864
_reflns_Friedel_fraction_full    0.915

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

_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1028P)²+1.8006P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 3658 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.105(18)
_chemical_absolute_configuration syn
_refine_ls_number_reflns         12527
_refine_ls_number_parameters     649
_refine_ls_number_restraints     47
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0705
_refine_ls_wR_factor_ref         0.2060
_refine_ls_wR_factor_gt          0.1886
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.850(3) 0.0681(18) -0.1182(12) 0.129(7) Uani 1 1 d . . . . .
H1A H 0.797770 0.123985 -0.143845 0.194 Uiso 1 1 calc R U . . .
H1B H 0.937100 0.090754 -0.101708 0.194 Uiso 1 1 calc R U . . .
H1C H 0.876925 0.022230 -0.168069 0.194 Uiso 1 1 calc R U . . .
C2 C 0.7602(18) 0.0192(12) -0.0302(10) 0.090(4) Uani 1 1 d . . . . .
H2 H 0.679377 -0.005826 -0.054847 0.108 Uiso 1 1 calc R U . . .
C3 C 0.818(3) -0.0757(14) 0.028(2) 0.173(13) Uani 1 1 d . . . . .
H3A H 0.834960 -0.131825 -0.011296 0.207 Uiso 1 1 calc R U . . .
H3B H 0.751745 -0.094681 0.091567 0.207 Uiso 1 1 calc R U . . .
C4 C 0.8193(13) 0.1339(8) 0.1110(9) 0.055(3) Uani 1 1 d . . . . .
C5 C 0.9401(13) 0.0805(10) 0.1105(11) 0.068(3) Uani 1 1 d . . . . .
C6 C 0.9948(19) 0.4024(11) 0.3801(13) 0.086(5) Uani 1 1 d . . . . .
C7 C 1.1287(15) 0.3554(9) 0.3712(11) 0.069(4) Uani 1 1 d . . . . .
C8 C 1.084(2) 0.5188(13) 0.5104(17) 0.121(8) Uani 1 1 d D . . . .
H8 H 1.075162 0.585723 0.532445 0.145 Uiso 1 1 calc R U . . .
C9 C 1.228(2) 0.5041(12) 0.4645(15) 0.107(5) Uani 1 1 d . . . . .
H9A H 1.288692 0.516709 0.510811 0.128 Uiso 1 1 calc R U . . .
H9B H 1.252171 0.553100 0.406656 0.128 Uiso 1 1 calc R U . . .
C10 C 1.051(4) 0.445(2) 0.606(2) 0.193(13) Uani 1 1 d D U . . .
H10A H 0.950627 0.452863 0.639468 0.290 Uiso 1 1 calc R U . . .
H10B H 1.066990 0.377683 0.587764 0.290 Uiso 1 1 calc R U . . .
H10C H 1.113568 0.456835 0.649681 0.290 Uiso 1 1 calc R U . . .
C11 C 0.304(4) 0.820(2) 0.860(3) 0.250(17) Uani 1 1 d . U . . .
H11A H 0.282811 0.816080 0.795668 0.375 Uiso 1 1 calc R U . . .
H11B H 0.374774 0.769054 0.872621 0.375 Uiso 1 1 calc R U . . .
H11C H 0.216339 0.810608 0.910931 0.375 Uiso 1 1 calc R U . . .
C12 C 0.3642(16) 0.9197(13) 0.8637(13) 0.101(4) Uani 1 1 d . U . . .
H12 H 0.287214 0.970609 0.859995 0.121 Uiso 1 1 calc R U . . .
C13 C 0.386(2) 0.9012(16) 0.9762(15) 0.131(6) Uani 1 1 d . U . . .
H13A H 0.293444 0.891971 1.023076 0.157 Uiso 1 1 calc R U . . .
H13B H 0.435847 0.956286 0.993237 0.157 Uiso 1 1 calc R U . . .
C14 C 0.6642(15) 0.8646(10) 0.7916(11) 0.070(4) Uani 1 1 d . . . . .
C15 C 0.6507(14) 0.7952(9) 0.8705(11) 0.066(3) Uani 1 1 d . . . . .
C16 C 1.2608(16) 0.7052(10) 0.6202(11) 0.070(3) Uani 1 1 d . . . . .
C17 C 1.2478(14) 0.6339(10) 0.6980(11) 0.065(3) Uani 1 1 d . . . . .
C21 C 0.5598(15) 0.1588(9) 0.4441(10) 0.066(3) Uani 1 1 d . . . . .
H21A H 0.638045 0.173587 0.386199 0.080 Uiso 1 1 calc R U . . .
H21B H 0.477945 0.203249 0.436471 0.080 Uiso 1 1 calc R U . . .
C22 C 0.609(2) 0.1778(12) 0.5351(16) 0.106(6) Uani 1 1 d . . . . .
H22A H 0.712261 0.159515 0.526413 0.127 Uiso 1 1 calc R U . . .
H22B H 0.557110 0.134467 0.591087 0.127 Uiso 1 1 calc R U . . .
C23 C 0.589(3) 0.2850(17) 0.562(2) 0.151(10) Uani 1 1 d . . . . .
H23A H 0.639771 0.329484 0.506251 0.182 Uiso 1 1 calc R U . . .
H23B H 0.486449 0.303353 0.574258 0.182 Uiso 1 1 calc R U . . .
C24 C 0.646(2) 0.2967(15) 0.6512(19) 0.136(9) Uani 1 1 d . . . . .
H24A H 0.632462 0.364596 0.666398 0.204 Uiso 1 1 calc R U . . .
H24B H 0.595591 0.253589 0.706787 0.204 Uiso 1 1 calc R U . . .
H24C H 0.748734 0.279690 0.638860 0.204 Uiso 1 1 calc R U . . .
C25 C 0.3828(14) 0.0246(10) 0.5293(9) 0.066(3) Uani 1 1 d . . . . .
H25A H 0.357534 -0.042804 0.522663 0.079 Uiso 1 1 calc R U . . .
H25B H 0.409847 0.024190 0.593703 0.079 Uiso 1 1 calc R U . . .
C26 C 0.2495(16) 0.0913(13) 0.5288(13) 0.094(5) Uani 1 1 d . . . . .
H26A H 0.278081 0.159766 0.526542 0.113 Uiso 1 1 calc R U . . .
H26B H 0.215410 0.085064 0.467893 0.113 Uiso 1 1 calc R U . . .
C27 C 0.1291(18) 0.0716(14) 0.6132(14) 0.098(6) Uani 1 1 d . . . . .
H27A H 0.160810 0.081197 0.674144 0.118 Uiso 1 1 calc R U . . .
H27B H 0.102312 0.002425 0.617508 0.118 Uiso 1 1 calc R U . . .
C28 C -0.0022(18) 0.1363(14) 0.6068(15) 0.107(6) Uani 1 1 d . . . . .
H28A H -0.078035 0.119644 0.664647 0.160 Uiso 1 1 calc R U . . .
H28B H 0.022677 0.204804 0.604081 0.160 Uiso 1 1 calc R U . . .
H28C H -0.035857 0.125983 0.547410 0.160 Uiso 1 1 calc R U . . .
C29 C 0.4770(17) 0.0478(11) 0.3415(9) 0.077(4) Uani 1 1 d . . . . .
H29A H 0.397434 0.094307 0.333719 0.092 Uiso 1 1 calc R U . . .
H29B H 0.561146 0.067975 0.289551 0.092 Uiso 1 1 calc R U . . .
C30 C 0.434(2) -0.0546(13) 0.3266(12) 0.091(5) Uani 1 1 d . . . . .
H30A H 0.521863 -0.095918 0.311380 0.109 Uiso 1 1 calc R U . . .
H30B H 0.374475 -0.084043 0.388698 0.109 Uiso 1 1 calc R U . . .
C31 C 0.3545(19) -0.0546(13) 0.2469(15) 0.098(5) Uani 1 1 d . . . . .
H31A H 0.418079 -0.030081 0.184232 0.118 Uiso 1 1 calc R U . . .
H31B H 0.272578 -0.008026 0.259319 0.118 Uiso 1 1 calc R U . . .
C32 C 0.299(2) -0.1518(18) 0.2345(17) 0.123(8) Uani 1 1 d . . . . .
H32A H 0.247829 -0.144163 0.180325 0.184 Uiso 1 1 calc R U . . .
H32B H 0.378789 -0.198285 0.219938 0.184 Uiso 1 1 calc R U . . .
H32C H 0.232930 -0.176176 0.295209 0.184 Uiso 1 1 calc R U . . .
C33 C 0.6388(14) -0.0190(9) 0.4584(9) 0.060(3) Uani 1 1 d . . . . .
H33A H 0.655791 -0.019468 0.525711 0.072 Uiso 1 1 calc R U . . .
H33B H 0.607593 -0.084995 0.451859 0.072 Uiso 1 1 calc R U . . .
C34 C 0.7823(15) 0.0009(10) 0.3847(11) 0.072(4) Uani 1 1 d . . . . .
H34A H 0.764683 0.007986 0.317127 0.087 Uiso 1 1 calc R U . . .
H34B H 0.820216 0.063238 0.396050 0.087 Uiso 1 1 calc R U . . .
C35 C 0.8951(16) -0.0807(12) 0.3931(14) 0.086(5) Uani 1 1 d . . . . .
H35A H 0.900792 -0.095011 0.462995 0.104 Uiso 1 1 calc R U . . .
H35B H 0.989511 -0.056890 0.356428 0.104 Uiso 1 1 calc R U . . .
C36 C 0.864(3) -0.1777(16) 0.353(2) 0.161(11) Uani 1 1 d . . . . .
H36A H 0.939878 -0.226026 0.361226 0.242 Uiso 1 1 calc R U . . .
H36B H 0.771795 -0.202907 0.390514 0.242 Uiso 1 1 calc R U . . .
H36C H 0.860615 -0.164743 0.283827 0.242 Uiso 1 1 calc R U . . .
C37 C 0.4691(13) 0.4438(10) 0.1348(9) 0.061(3) Uani 1 1 d . . . . .
H37A H 0.549322 0.396709 0.138625 0.073 Uiso 1 1 calc R U . . .
H37B H 0.387490 0.422059 0.188060 0.073 Uiso 1 1 calc R U . . .
C38 C 0.5151(16) 0.5460(10) 0.1538(10) 0.072(4) Uani 1 1 d . . . . .
H38A H 0.577361 0.576795 0.093357 0.086 Uiso 1 1 calc R U . . .
H38B H 0.429314 0.588500 0.170562 0.086 Uiso 1 1 calc R U . . .
C39 C 0.5963(16) 0.5359(16) 0.2383(12) 0.100(6) Uani 1 1 d . . . . .
H39A H 0.682630 0.493972 0.220990 0.120 Uiso 1 1 calc R U . . .
H39B H 0.534433 0.504061 0.298305 0.120 Uiso 1 1 calc R U . . .
C40 C 0.642(2) 0.6398(16) 0.2599(15) 0.104(6) Uani 1 1 d . . . . .
H40A H 0.693707 0.631189 0.313865 0.157 Uiso 1 1 calc R U . . .
H40B H 0.705052 0.671028 0.200942 0.157 Uiso 1 1 calc R U . . .
H40C H 0.557020 0.681106 0.278171 0.157 Uiso 1 1 calc R U . . .
C41 C 0.5515(12) 0.4651(9) -0.0493(9) 0.055(3) Uani 1 1 d . . . . .
H41A H 0.566833 0.536213 -0.055490 0.066 Uiso 1 1 calc R U . . .
H41B H 0.523444 0.449977 -0.109944 0.066 Uiso 1 1 calc R U . . .
C42 C 0.6954(15) 0.4114(12) -0.0429(12) 0.084(4) Uani 1 1 d . . . . .
H42A H 0.736763 0.440096 0.006334 0.100 Uiso 1 1 calc R U . . .
H42B H 0.675472 0.342184 -0.018441 0.100 Uiso 1 1 calc R U . . .
C43 C 0.8034(15) 0.4145(11) -0.1355(11) 0.073(4) Uani 1 1 d . . . . .
H43A H 0.824673 0.483716 -0.159079 0.088 Uiso 1 1 calc R U . . .
H43B H 0.761079 0.387219 -0.185038 0.088 Uiso 1 1 calc R U . . .
C44 C 0.9460(17) 0.3594(13) -0.1304(16) 0.102(6) Uani 1 1 d . . . . .
H44A H 1.009825 0.366064 -0.195332 0.152 Uiso 1 1 calc R U . . .
H44B H 0.991264 0.386963 -0.083236 0.152 Uiso 1 1 calc R U . . .
H44C H 0.927495 0.290202 -0.109266 0.152 Uiso 1 1 calc R U . . .
C45 C 0.3775(15) 0.3315(9) 0.0296(11) 0.070(3) Uani 1 1 d . . . . .
H45A H 0.457524 0.285648 0.037909 0.084 Uiso 1 1 calc R U . . .
H45B H 0.296543 0.314637 0.085182 0.084 Uiso 1 1 calc R U . . .
C46 C 0.3319(19) 0.3136(10) -0.0654(12) 0.081(4) Uani 1 1 d . . . . .
H46A H 0.234610 0.342207 -0.062835 0.098 Uiso 1 1 calc R U . . .
H46B H 0.396796 0.350158 -0.120850 0.098 Uiso 1 1 calc R U . . .
C47 C 0.330(4) 0.2160(13) -0.0869(19) 0.158(11) Uani 1 1 d . . . . .
H47A H 0.266589 0.179469 -0.030659 0.190 Uiso 1 1 calc R U . . .
H47B H 0.427836 0.187945 -0.090048 0.190 Uiso 1 1 calc R U . . .
C48 C 0.282(2) 0.1951(15) -0.1832(15) 0.109(6) Uani 1 1 d . . . . .
H48A H 0.286016 0.124634 -0.188168 0.163 Uiso 1 1 calc R U . . .
H48B H 0.183473 0.219530 -0.180875 0.163 Uiso 1 1 calc R U . . .
H48C H 0.345523 0.228048 -0.240560 0.163 Uiso 1 1 calc R U . . .
C49 C 0.3028(13) 0.5136(9) 0.0242(10) 0.063(3) Uani 1 1 d . . . . .
H49A H 0.332098 0.579690 0.032096 0.075 Uiso 1 1 calc R U . . .
H49B H 0.288254 0.514331 -0.043698 0.075 Uiso 1 1 calc R U . . .
C50 C 0.1586(15) 0.4913(12) 0.0963(13) 0.089(5) Uani 1 1 d . . . . .
H50A H 0.124447 0.427841 0.084589 0.107 Uiso 1 1 calc R U . . .
H50B H 0.174131 0.485284 0.164338 0.107 Uiso 1 1 calc R U . . .
C51 C 0.0420(17) 0.5705(10) 0.0861(11) 0.075(4) Uani 1 1 d . . . . .
H51A H 0.036679 0.584136 0.016147 0.091 Uiso 1 1 calc R U . . .
H51B H -0.051906 0.545968 0.123020 0.091 Uiso 1 1 calc R U . . .
C52 C 0.071(2) 0.6608(16) 0.123(2) 0.150(10) Uani 1 1 d . . . . .
H52A H -0.004417 0.709229 0.115446 0.225 Uiso 1 1 calc R U . . .
H52B H 0.075067 0.647789 0.192626 0.225 Uiso 1 1 calc R U . . .
H52C H 0.163580 0.685926 0.085838 0.225 Uiso 1 1 calc R U . . .
N1 N 0.5149(11) 0.0548(7) 0.4468(7) 0.057(2) Uani 1 1 d . . . . .
N2 N 0.4266(10) 0.4400(7) 0.0379(8) 0.058(2) Uani 1 1 d . . . . .
S1 S 0.6717(3) 0.1093(2) 0.0555(3) 0.0702(9) Uani 1 1 d . . . . .
S2 S 0.9990(5) -0.0265(4) 0.0486(5) 0.130(2) Uani 1 1 d . . . . .
S3 S 0.7834(3) 0.2375(2) 0.1774(2) 0.0550(7) Uani 1 1 d . . . . .
S4 S 1.0716(3) 0.1182(3) 0.1696(3) 0.0711(9) Uani 1 1 d . . . . .
S5 S 0.8707(4) 0.3678(3) 0.3154(3) 0.0797(11) Uani 1 1 d . . . . .
S6 S 1.1624(3) 0.2545(2) 0.3018(2) 0.0567(7) Uani 1 1 d . . . . .
S7 S 0.9448(8) 0.5112(5) 0.4375(6) 0.157(3) Uani 1 1 d . . . . .
S8 S 1.2764(4) 0.3812(3) 0.4237(3) 0.0805(11) Uani 1 1 d . . . . .
S9 S 0.5375(5) 0.9637(3) 0.7760(3) 0.0842(10) Uani 1 1 d . . . . .
S10 S 0.5035(4) 0.7826(3) 0.9763(4) 0.1053(16) Uani 1 1 d . . . . .
S11 S 0.8208(5) 0.8702(3) 0.6989(3) 0.0858(12) Uani 1 1 d . . . . .
S12 S 0.7924(4) 0.7082(2) 0.8766(3) 0.0714(9) Uani 1 1 d . . . . .
S13 S 1.1178(5) 0.7874(2) 0.6103(3) 0.0893(13) Uani 1 1 d . . . . .
S14 S 1.0907(4) 0.6298(3) 0.7916(3) 0.0742(9) Uani 1 1 d . . . . .
S15 S 1.4158(5) 0.7200(3) 0.5233(4) 0.1006(14) Uani 1 1 d . . . . .
S16 S 1.3857(5) 0.5474(5) 0.7168(3) 0.122(2) Uani 1 1 d . . . . .
NI1 Ni 0.9715(2) 0.24479(16) 0.24121(18) 0.0495(3) Uani 1 1 d . . . . .
NI2 Ni 0.9554(3) 0.74783(17) 0.74355(19) 0.0570(4) Uani 1 1 d . . . . .
C19 C 1.550(2) 0.6420(18) 0.6659(17) 0.133(6) Uani 1 1 d . U . . .
H19 H 1.534670 0.705832 0.694637 0.160 Uiso 1 1 calc R U . . .
C18 C 1.562(2) 0.6504(16) 0.5574(16) 0.140(7) Uani 1 1 d D U . . .
H18A H 1.564369 0.584417 0.535514 0.168 Uiso 1 1 calc R U . . .
H18B H 1.653308 0.682277 0.524498 0.168 Uiso 1 1 calc R U . . .
C20 C 1.686(3) 0.599(2) 0.664(2) 0.186(11) Uani 1 1 d D U . . .
H20A H 1.701162 0.586871 0.731207 0.279 Uiso 1 1 calc R U . . .
H20B H 1.692522 0.537828 0.634418 0.279 Uiso 1 1 calc R U . . .
H20C H 1.758496 0.643900 0.625220 0.279 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.43(2) . ?
C2 C3 1.58(2) . ?
C2 S1 1.835(15) . ?
C3 S2 1.93(2) . ?
C4 C5 1.316(15) . ?
C4 S3 1.735(11) . ?
C4 S1 1.776(12) . ?
C5 S4 1.736(13) . ?
C5 S2 1.766(13) . ?
C6 C7 1.369(19) . ?
C6 S5 1.717(15) . ?
C6 S7 1.743(14) . ?
C7 S6 1.728(13) . ?
C7 S8 1.756(13) . ?
C8 C9 1.38(3) . ?
C8 C10 1.55(2) . ?
C8 S7 1.815(18) . ?
C9 S8 1.819(15) . ?
C11 C12 1.49(3) . ?
C12 C13 1.59(2) . ?
C12 S9 1.881(18) . ?
C13 S10 1.90(2) . ?
C14 C15 1.341(18) . ?
C14 S11 1.725(16) . ?
C14 S9 1.777(12) . ?
C15 S12 1.744(12) . ?
C15 S10 1.777(15) . ?
C16 C17 1.348(19) . ?
C16 S13 1.721(14) . ?
C16 S15 1.750(15) . ?
C17 S14 1.734(15) . ?
C17 S16 1.745(13) . ?
C21 C22 1.47(2) . ?
C21 N1 1.478(16) . ?
C22 C23 1.53(2) . ?
C23 C24 1.46(3) . ?
C25 C26 1.509(16) . ?
C25 N1 1.526(17) . ?
C26 C27 1.45(2) . ?
C27 C28 1.49(2) . ?
C29 C30 1.50(2) . ?
C29 N1 1.576(16) . ?
C30 C31 1.45(2) . ?
C31 C32 1.47(2) . ?
C33 C34 1.516(19) . ?
C33 N1 1.520(13) . ?
C34 C35 1.506(16) . ?
C35 C36 1.54(3) . ?
C37 N2 1.475(15) . ?
C37 C38 1.529(19) . ?
C38 C39 1.510(19) . ?
C39 C40 1.56(3) . ?
C41 N2 1.506(15) . ?
C41 C42 1.518(15) . ?
C42 C43 1.445(19) . ?
C43 C44 1.513(18) . ?
C45 C46 1.503(19) . ?
C45 N2 1.578(17) . ?
C46 C47 1.38(2) . ?
C47 C48 1.55(3) . ?
C49 C50 1.516(18) . ?
C49 N2 1.524(12) . ?
C50 C51 1.513(17) . ?
C51 C52 1.43(3) . ?
S3 NI1 2.141(3) . ?
S4 NI1 2.148(4) . ?
S5 NI1 2.125(4) . ?
S6 NI1 2.144(3) . ?
S11 NI2 2.152(4) . ?
S12 NI2 2.151(4) . ?
S13 NI2 2.150(5) . ?
S14 NI2 2.130(4) . ?
S15 C18 1.75(2) . ?
S16 C19 2.00(2) . ?
C19 C20 1.37(3) . ?
C19 C18 1.46(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 C2 C3 120.8(19) . . ?
C1 C2 S1 111.2(13) . . ?
C3 C2 S1 111.4(11) . . ?
C2 C3 S2 100.5(14) . . ?
C5 C4 S3 120.9(9) . . ?
C5 C4 S1 127.3(9) . . ?
S3 C4 S1 111.7(6) . . ?
C4 C5 S4 119.9(9) . . ?
C4 C5 S2 128.6(10) . . ?
S4 C5 S2 111.4(6) . . ?
C7 C6 S5 120.3(10) . . ?
C7 C6 S7 125.2(11) . . ?
S5 C6 S7 113.6(8) . . ?
C6 C7 S6 118.2(10) . . ?
C6 C7 S8 128.9(10) . . ?
S6 C7 S8 112.9(7) . . ?
C9 C8 C10 107(2) . . ?
C9 C8 S7 118.4(15) . . ?
C10 C8 S7 109.8(18) . . ?
C8 C9 S8 115.8(13) . . ?
C11 C12 C13 96(2) . . ?
C11 C12 S9 121.5(17) . . ?
C13 C12 S9 110.9(12) . . ?
C12 C13 S10 103.3(12) . . ?
C15 C14 S11 120.8(10) . . ?
C15 C14 S9 125.5(12) . . ?
S11 C14 S9 113.5(8) . . ?
C14 C15 S12 118.9(11) . . ?
C14 C15 S10 127.1(10) . . ?
S12 C15 S10 113.9(7) . . ?
C17 C16 S13 120.0(11) . . ?
C17 C16 S15 124.1(11) . . ?
S13 C16 S15 115.8(9) . . ?
C16 C17 S14 119.7(11) . . ?
C16 C17 S16 124.1(11) . . ?
S14 C17 S16 116.1(8) . . ?
C22 C21 N1 112.8(12) . . ?
C21 C22 C23 115.6(15) . . ?
C24 C23 C22 111.3(18) . . ?
C26 C25 N1 114.6(11) . . ?
C27 C26 C25 115.5(13) . . ?
C26 C27 C28 113.4(14) . . ?
C30 C29 N1 113.7(11) . . ?
C31 C30 C29 113.2(14) . . ?
C30 C31 C32 115.7(16) . . ?
C34 C33 N1 115.7(10) . . ?
C35 C34 C33 112.9(13) . . ?
C34 C35 C36 114.1(16) . . ?
N2 C37 C38 115.3(10) . . ?
C39 C38 C37 110.5(13) . . ?
C38 C39 C40 111.3(15) . . ?
N2 C41 C42 115.6(10) . . ?
C43 C42 C41 115.6(12) . . ?
C42 C43 C44 116.1(13) . . ?
C46 C45 N2 117.2(11) . . ?
C47 C46 C45 117.6(15) . . ?
C46 C47 C48 118.9(17) . . ?
C50 C49 N2 114.7(10) . . ?
C51 C50 C49 113.1(12) . . ?
C52 C51 C50 111.7(16) . . ?
C21 N1 C33 111.7(10) . . ?
C21 N1 C25 114.4(9) . . ?
C33 N1 C25 107.9(9) . . ?
C21 N1 C29 105.0(10) . . ?
C33 N1 C29 108.3(8) . . ?
C25 N1 C29 109.4(11) . . ?
C37 N2 C41 111.8(10) . . ?
C37 N2 C49 112.1(9) . . ?
C41 N2 C49 106.5(9) . . ?
C37 N2 C45 109.9(10) . . ?
C41 N2 C45 107.2(9) . . ?
C49 N2 C45 109.0(10) . . ?
C4 S1 C2 100.1(6) . . ?
C5 S2 C3 102.4(6) . . ?
C4 S3 NI1 103.6(4) . . ?
C5 S4 NI1 103.8(4) . . ?
C6 S5 NI1 104.9(5) . . ?
C7 S6 NI1 105.0(4) . . ?
C6 S7 C8 102.8(7) . . ?
C7 S8 C9 102.7(7) . . ?
C14 S9 C12 103.4(7) . . ?
C15 S10 C13 108.5(8) . . ?
C14 S11 NI2 104.5(4) . . ?
C15 S12 NI2 104.7(5) . . ?
C16 S13 NI2 104.2(6) . . ?
C17 S14 NI2 104.5(5) . . ?
C18 S15 C16 109.9(9) . . ?
C17 S16 C19 95.3(8) . . ?
S5 NI1 S3 88.63(14) . . ?
S5 NI1 S6 91.42(15) . . ?
S3 NI1 S6 178.5(2) . . ?
S5 NI1 S4 178.6(3) . . ?
S3 NI1 S4 91.58(14) . . ?
S6 NI1 S4 88.41(13) . . ?
S14 NI2 S13 91.59(17) . . ?
S14 NI2 S12 88.55(16) . . ?
S13 NI2 S12 179.8(2) . . ?
S14 NI2 S11 177.9(2) . . ?
S13 NI2 S11 88.88(18) . . ?
S12 NI2 S11 90.99(17) . . ?
C20 C19 C18 95.2(17) . . ?
C20 C19 S16 114.0(19) . . ?
C18 C19 S16 103.1(15) . . ?
C19 C18 S15 110.6(15) . . ?

_refine_diff_density_max         1.121
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.081

####################################################################### 
# 
# 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_shelx_CCDC9
_database_code_depnum_ccdc_archive 'CCDC 2048868'
loop_
_audit_author_name
_audit_author_address
'Narcis Avarvari'
;CNRS, University of Angers
France
;
_audit_update_record             
;
2020-12-07 deposited with the CCDC.	2021-02-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H12 Ni S8'
_chemical_formula_sum            'C10 H12 Ni S8'
_chemical_formula_weight         447.39

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'
S S 0.3331 0.5567 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   5.2567(6)
_cell_length_b                   15.0900(19)
_cell_length_c                   10.1421(12)
_cell_angle_alpha                90
_cell_angle_beta                 90.093(11)
_cell_angle_gamma                90
_cell_volume                     804.51(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    150.01(10)
_cell_measurement_reflns_used    2588
_cell_measurement_theta_min      2.8390
_cell_measurement_theta_max      73.9740

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.847
_exptl_crystal_F_000             456
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    11.293
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.47461
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.611
_oxdiff_exptl_absorpt_empirical_full_max 1.873
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150.01(10)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_reflns_number            5115
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         4.359
_diffrn_reflns_theta_max         74.843
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_point_group_measured_fraction_full 0.954
_reflns_number_total             3010
_reflns_number_gt                2679
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.814
_reflns_Friedel_fraction_max     0.846
_reflns_Friedel_fraction_full    0.910

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

_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1025P)²+2.2658P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1045 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.15(6)
_chemical_absolute_configuration syn
_refine_ls_number_reflns         3010
_refine_ls_number_parameters     172
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0647
_refine_ls_wR_factor_ref         0.1802
_refine_ls_wR_factor_gt          0.1746
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.739(2) 0.5538(10) 1.1232(13) 0.044(3) Uani 1 1 d . . . . .
H1 H -0.865538 0.530229 1.061100 0.053 Uiso 1 1 calc R U . . .
C2 C -0.525(2) 0.4903(10) 1.1320(12) 0.044(3) Uani 1 1 d . . . . .
H2A H -0.584620 0.437059 1.175838 0.053 Uiso 1 1 calc R U . . .
H2B H -0.393065 0.516161 1.186607 0.053 Uiso 1 1 calc R U . . .
C3 C -0.401(2) 0.6439(11) 0.9472(11) 0.035(3) Uani 1 1 d . . . . .
C4 C -0.309(3) 0.5653(11) 0.9126(12) 0.038(3) Uani 1 1 d . . . . .
C5 C 0.294(2) 0.8249(9) 0.5711(11) 0.031(2) Uani 1 1 d . . . . .
C6 C 0.392(2) 0.7429(8) 0.5301(12) 0.033(3) Uani 1 1 d . . . . .
C7 C 0.646(2) 0.9061(9) 0.4015(13) 0.039(3) Uani 1 1 d . . . . .
H7A H 0.670724 0.956927 0.344403 0.046 Uiso 1 1 calc R U . . .
H7B H 0.794512 0.901421 0.457762 0.046 Uiso 1 1 calc R U . . .
C8 C 0.632(2) 0.8244(9) 0.3169(11) 0.038(2) Uani 1 1 d . . . . .
H8 H 0.477468 0.825967 0.262557 0.045 Uiso 1 1 calc R U . . .
C9 C -0.872(3) 0.5701(12) 1.2574(14) 0.053(4) Uani 1 1 d . . . . .
H9A H -1.008436 0.611620 1.245799 0.079 Uiso 1 1 calc R U . . .
H9B H -0.938095 0.515224 1.290497 0.079 Uiso 1 1 calc R U . . .
H9C H -0.750653 0.593742 1.319044 0.079 Uiso 1 1 calc R U . . .
C10 C 0.864(2) 0.8169(12) 0.2295(14) 0.046(4) Uani 1 1 d . . . . .
H10A H 0.851720 0.764385 0.176428 0.069 Uiso 1 1 calc R U . . .
H10B H 0.874643 0.867943 0.173248 0.069 Uiso 1 1 calc R U . . .
H10C H 1.014464 0.813613 0.283393 0.069 Uiso 1 1 calc R U . . .
S1 S -0.6370(7) 0.6634(2) 1.0650(3) 0.0428(8) Uani 1 1 d . . . . .
S2 S -0.3897(8) 0.4599(3) 0.9761(3) 0.0459(9) Uani 1 1 d . . . . .
S3 S -0.2862(6) 0.7394(2) 0.8765(3) 0.0369(7) Uani 1 1 d . . . . .
S4 S -0.0833(6) 0.5597(2) 0.7889(3) 0.0362(7) Uani 1 1 d . . . . .
S5 S 0.0684(7) 0.8283(2) 0.6903(3) 0.0387(7) Uani 1 1 d . . . . .
S6 S 0.2726(6) 0.6492(2) 0.6038(3) 0.0350(7) Uani 1 1 d . . . . .
S7 S 0.3731(7) 0.9275(2) 0.5045(3) 0.0409(7) Uani 1 1 d . . . . .
S8 S 0.6344(6) 0.7235(2) 0.4180(3) 0.0395(8) Uani 1 1 d . . . . .
NI1 Ni -0.0072(5) 0.6938(2) 0.7387(2) 0.0327(4) 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
C1 C2 1.48(2) . ?
C1 C9 1.549(19) . ?
C1 S1 1.837(15) . ?
C2 S2 1.796(13) . ?
C3 C4 1.33(2) . ?
C3 S3 1.720(15) . ?
C3 S1 1.748(13) . ?
C4 S4 1.729(14) . ?
C4 S2 1.767(15) . ?
C5 C6 1.404(19) . ?
C5 S5 1.696(12) . ?
C5 S7 1.740(14) . ?
C6 S6 1.719(13) . ?
C6 S8 1.732(14) . ?
C7 C8 1.505(17) . ?
C7 S7 1.803(12) . ?
C8 C10 1.517(17) . ?
C8 S8 1.835(14) . ?
S3 NI1 2.141(4) . ?
S4 NI1 2.125(5) . ?
S5 NI1 2.126(5) . ?
S6 NI1 2.120(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C9 113.1(12) . . ?
C2 C1 S1 112.3(9) . . ?
C9 C1 S1 105.7(11) . . ?
C1 C2 S2 114.5(9) . . ?
C4 C3 S3 120.6(10) . . ?
C4 C3 S1 126.2(11) . . ?
S3 C3 S1 113.2(9) . . ?
C3 C4 S4 119.1(11) . . ?
C3 C4 S2 128.2(11) . . ?
S4 C4 S2 112.7(9) . . ?
C6 C5 S5 119.8(10) . . ?
C6 C5 S7 125.5(9) . . ?
S5 C5 S7 114.7(8) . . ?
C5 C6 S6 117.4(10) . . ?
C5 C6 S8 127.9(10) . . ?
S6 C6 S8 114.6(7) . . ?
C8 C7 S7 116.0(8) . . ?
C7 C8 C10 110.8(11) . . ?
C7 C8 S8 111.2(8) . . ?
C10 C8 S8 105.0(10) . . ?
C3 S1 C1 106.0(7) . . ?
C4 S2 C2 100.8(7) . . ?
C3 S3 NI1 104.2(5) . . ?
C4 S4 NI1 104.9(6) . . ?
C5 S5 NI1 105.5(5) . . ?
C6 S6 NI1 105.9(5) . . ?
C5 S7 C7 104.9(7) . . ?
C6 S8 C8 102.8(6) . . ?
S6 NI1 S4 89.05(17) . . ?
S6 NI1 S5 91.38(15) . . ?
S4 NI1 S5 179.45(17) . . ?
S6 NI1 S3 179.3(2) . . ?
S4 NI1 S3 91.16(15) . . ?
S5 NI1 S3 88.41(17) . . ?

_refine_diff_density_max         1.086
_refine_diff_density_min         -1.156
_refine_diff_density_rms         0.148

####################################################################### 
# 
# 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_shelx_CCDC10
_database_code_depnum_ccdc_archive 'CCDC 2048865'
loop_
_audit_author_name
_audit_author_address
'Narcis Avarvari'
;CNRS, University of Angers
France
;
_audit_update_record             
;
2020-12-07 deposited with the CCDC.	2021-02-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H12 N, C12 H16 Ni S8'
_chemical_formula_sum            'C16 H28 N Ni S8'
_chemical_formula_weight         549.58

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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'I 2'
_space_group_name_Hall           'I 2y'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   17.5730(5)
_cell_length_b                   9.9665(2)
_cell_length_c                   15.7025(5)
_cell_angle_alpha                90
_cell_angle_beta                 119.996(4)
_cell_angle_gamma                90
_cell_volume                     2381.80(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.01(10)
_cell_measurement_reflns_used    8682
_cell_measurement_theta_min      5.2620
_cell_measurement_theta_max      71.7870

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_F_000             1148
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    7.750
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.51844
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.818
_oxdiff_exptl_absorpt_empirical_full_max 1.383
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      150.01(10)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_reflns_number            10384
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_av_R_equivalents  0.0188
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.091
_diffrn_reflns_theta_max         71.946
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_point_group_measured_fraction_full 0.962
_reflns_number_total             4411
_reflns_number_gt                4371
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.791
_reflns_Friedel_fraction_max     0.887
_reflns_Friedel_fraction_full    0.919

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

_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0474P)²+3.8260P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1886 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.038(10)
_chemical_absolute_configuration syn
_refine_ls_number_reflns         4411
_refine_ls_number_parameters     231
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0295
_refine_ls_wR_factor_ref         0.0846
_refine_ls_wR_factor_gt          0.0844
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2108(3) 0.1323(4) 0.5800(3) 0.0257(8) Uani 1 1 d . . . . .
H1 H 0.218809 0.152727 0.523959 0.031 Uiso 1 1 calc R U . . .
C2 C 0.2756(3) 0.0243(5) 0.6420(3) 0.0274(8) Uani 1 1 d . . . . .
H2 H 0.273948 0.014340 0.703144 0.033 Uiso 1 1 calc R U . . .
C3 C 0.3361(3) 0.3274(5) 0.6819(3) 0.0249(10) Uani 1 1 d . . . . .
C4 C 0.3977(3) 0.2408(6) 0.6872(3) 0.0234(10) Uani 1 1 d . . . . .
C5 C 0.5987(3) 0.7751(5) 0.8151(3) 0.0221(9) Uani 1 1 d . . . . .
C6 C 0.6607(3) 0.6868(5) 0.8200(3) 0.0244(10) Uani 1 1 d . . . . .
C7 C 0.7319(3) 0.9603(5) 0.9187(3) 0.0280(9) Uani 1 1 d . . . . .
H7 H 0.748363 0.912568 0.980127 0.034 Uiso 1 1 calc R U . . .
C8 C 0.7837(3) 0.9043(5) 0.8726(3) 0.0271(9) Uani 1 1 d . . . . .
H8 H 0.765166 0.950262 0.810040 0.032 Uiso 1 1 calc R U . . .
C9 C 0.1157(3) 0.0937(6) 0.5421(3) 0.0324(11) Uani 1 1 d . . . . .
H9A H 0.078139 0.165976 0.503518 0.049 Uiso 1 1 calc R U . . .
H9B H 0.101936 0.014733 0.501992 0.049 Uiso 1 1 calc R U . . .
H9C H 0.106925 0.075993 0.596610 0.049 Uiso 1 1 calc R U . . .
C10 C 0.2575(3) -0.1124(6) 0.5913(4) 0.0441(14) Uani 1 1 d . . . . .
H10A H 0.300859 -0.175713 0.634490 0.066 Uiso 1 1 calc R U . . .
H10B H 0.200163 -0.142816 0.575670 0.066 Uiso 1 1 calc R U . . .
H10C H 0.260263 -0.104364 0.531975 0.066 Uiso 1 1 calc R U . . .
C11 C 0.7487(3) 1.1109(6) 0.9393(4) 0.0408(13) Uani 1 1 d . . . . .
H11A H 0.715461 1.143599 0.968247 0.061 Uiso 1 1 calc R U . . .
H11B H 0.810179 1.125821 0.983664 0.061 Uiso 1 1 calc R U . . .
H11C H 0.731084 1.157530 0.878704 0.061 Uiso 1 1 calc R U . . .
C12 C 0.8834(3) 0.9210(6) 0.9395(3) 0.0348(12) Uani 1 1 d . . . . .
H12A H 0.913084 0.884434 0.907346 0.052 Uiso 1 1 calc R U . . .
H12B H 0.897375 1.014598 0.952502 0.052 Uiso 1 1 calc R U . . .
H12C H 0.902107 0.874471 1.000270 0.052 Uiso 1 1 calc R U . . .
C13 C 0.4220(5) 0.0414(8) 0.9414(4) 0.072(2) Uani 1 1 d . . . . .
H13A H 0.371400 0.096955 0.903486 0.108 Uiso 1 1 calc R U . . .
H13B H 0.431967 -0.014182 0.898061 0.108 Uiso 1 1 calc R U . . .
H13C H 0.412050 -0.014186 0.984870 0.108 Uiso 1 1 calc R U . . .
C14 C 0.5153(3) 0.2118(6) 0.9315(3) 0.0345(11) Uani 1 1 d . . . . .
H14A H 0.565672 0.267918 0.968684 0.052 Uiso 1 1 calc R U . . .
H14B H 0.525333 0.154834 0.888783 0.052 Uiso 1 1 calc R U . . .
H14C H 0.464607 0.266849 0.892864 0.052 Uiso 1 1 calc R U . . .
C15 C 0.9812(7) 0.3172(11) 0.0634(6) 0.089(3) Uani 1 1 d . . . . .
H15A H 0.928801 0.266364 0.023288 0.134 Uiso 1 1 calc R U . . .
H15B H 1.029613 0.257042 0.099315 0.134 Uiso 1 1 calc R U . . .
H15C H 0.973001 0.371370 0.108763 0.134 Uiso 1 1 calc R U . . .
N1 N 0.500000 0.1275(6) 1.000000 0.0256(11) Uani 1 2 d S T P . .
N2 N 1.000000 0.4049(9) 0.000000 0.0500(19) Uani 1 2 d S T P . .
NI1 Ni 0.49794(5) 0.50797(13) 0.75002(6) 0.02171(15) Uani 1 1 d . . . . .
S4 S 0.61383(7) 0.94780(14) 0.83623(9) 0.0311(3) Uani 1 1 d . . . . .
S7 S 0.76855(8) 0.72441(17) 0.85079(13) 0.0478(4) Uani 1 1 d . . . . .
S8 S 0.63532(7) 0.51887(14) 0.79604(8) 0.0276(3) Uani 1 1 d . . . . .
S9 S 0.49418(7) 0.71714(12) 0.78129(8) 0.0253(2) Uani 1 1 d . . . . .
S14 S 0.22901(7) 0.28496(14) 0.65223(9) 0.0323(3) Uani 1 1 d . . . . .
S17 S 0.38820(7) 0.06578(13) 0.67299(9) 0.0298(3) Uani 1 1 d . . . . .
S18 S 0.50114(7) 0.29955(12) 0.71616(7) 0.0242(2) Uani 1 1 d . . . . .
S19 S 0.36164(7) 0.49616(13) 0.70799(8) 0.0276(3) Uani 1 1 d . . . . .
C16 C 1.0731(15) 0.471(4) 0.061(2) 0.378(19) Uiso 1 1 d . . . . .
H16A H 1.118864 0.407884 0.099929 0.567 Uiso 1 1 calc R U . . .
H16B H 1.090886 0.526316 0.024430 0.567 Uiso 1 1 calc R U . . .
H16C H 1.062184 0.526317 0.104254 0.567 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.515(6) . ?
C1 C9 1.516(6) . ?
C1 S14 1.828(4) . ?
C1 H1 0.9800 . ?
C2 C10 1.528(7) . ?
C2 S17 1.833(4) . ?
C2 H2 0.9800 . ?
C3 C4 1.355(7) . ?
C3 S19 1.736(5) . ?
C3 S14 1.750(4) . ?
C4 S18 1.740(4) . ?
C4 S17 1.755(6) . ?
C5 C6 1.372(7) . ?
C5 S9 1.736(4) . ?
C5 S4 1.748(5) . ?
C6 S8 1.725(5) . ?
C6 S7 1.747(5) . ?
C7 C8 1.524(6) . ?
C7 C11 1.532(7) . ?
C7 S4 1.820(4) . ?
C7 H7 0.9800 . ?
C8 C12 1.537(6) . ?
C8 S7 1.820(5) . ?
C8 H8 0.9800 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 N1 1.484(6) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 N1 1.491(6) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 N2 1.481(9) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
N1 C13 1.484(6) 2_657 ?
N1 C14 1.491(6) 2_657 ?
N2 C16 1.33(3) . ?
N2 C16 1.33(3) 2_755 ?
N2 C15 1.481(9) 2_755 ?
NI1 S19 2.1460(14) . ?
NI1 S8 2.1489(14) . ?
NI1 S9 2.1503(18) . ?
NI1 S18 2.1519(18) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 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
C2 C1 C9 113.5(4) . . ?
C2 C1 S14 110.5(3) . . ?
C9 C1 S14 105.8(3) . . ?
C2 C1 H1 109.0 . . ?
C9 C1 H1 109.0 . . ?
S14 C1 H1 109.0 . . ?
C1 C2 C10 113.9(4) . . ?
C1 C2 S17 112.1(3) . . ?
C10 C2 S17 104.8(3) . . ?
C1 C2 H2 108.7 . . ?
C10 C2 H2 108.7 . . ?
S17 C2 H2 108.7 . . ?
C4 C3 S19 119.9(4) . . ?
C4 C3 S14 125.6(4) . . ?
S19 C3 S14 114.4(3) . . ?
C3 C4 S18 120.0(4) . . ?
C3 C4 S17 127.1(4) . . ?
S18 C4 S17 112.9(3) . . ?
C6 C5 S9 119.5(4) . . ?
C6 C5 S4 125.4(4) . . ?
S9 C5 S4 115.0(3) . . ?
C5 C6 S8 119.9(4) . . ?
C5 C6 S7 126.8(4) . . ?
S8 C6 S7 113.3(3) . . ?
C8 C7 C11 111.1(4) . . ?
C8 C7 S4 112.1(3) . . ?
C11 C7 S4 104.4(3) . . ?
C8 C7 H7 109.7 . . ?
C11 C7 H7 109.7 . . ?
S4 C7 H7 109.7 . . ?
C7 C8 C12 112.5(4) . . ?
C7 C8 S7 112.6(3) . . ?
C12 C8 S7 104.2(4) . . ?
C7 C8 H8 109.1 . . ?
C12 C8 H8 109.1 . . ?
S7 C8 H8 109.1 . . ?
C1 C9 H9A 109.5 . . ?
C1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C2 C10 H10A 109.5 . . ?
C2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C7 C11 H11A 109.5 . . ?
C7 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C7 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C8 C12 H12A 109.5 . . ?
C8 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C8 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N1 C13 H13A 109.5 . . ?
N1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N1 C14 H14A 109.5 . . ?
N1 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N1 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N2 C15 H15A 109.5 . . ?
N2 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N2 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 N1 C13 109.3(8) . 2_657 ?
C13 N1 C14 109.2(3) . 2_657 ?
C13 N1 C14 108.8(3) 2_657 2_657 ?
C13 N1 C14 108.8(3) . . ?
C13 N1 C14 109.2(3) 2_657 . ?
C14 N1 C14 111.4(6) 2_657 . ?
C16 N2 C16 121(3) . 2_755 ?
C16 N2 C15 105.2(13) . . ?
C16 N2 C15 108.7(13) 2_755 . ?
C16 N2 C15 108.7(13) . 2_755 ?
C16 N2 C15 105.2(13) 2_755 2_755 ?
C15 N2 C15 107.7(10) . 2_755 ?
S19 NI1 S8 178.50(7) . . ?
S19 NI1 S9 88.07(6) . . ?
S8 NI1 S9 91.82(6) . . ?
S19 NI1 S18 91.95(6) . . ?
S8 NI1 S18 88.18(6) . . ?
S9 NI1 S18 179.00(6) . . ?
C5 S4 C7 102.3(2) . . ?
C6 S7 C8 107.4(2) . . ?
C6 S8 NI1 104.29(17) . . ?
C5 S9 NI1 104.12(19) . . ?
C3 S14 C1 101.4(2) . . ?
C4 S17 C2 106.2(2) . . ?
C4 S18 NI1 103.70(19) . . ?
C3 S19 NI1 104.04(16) . . ?
N2 C16 H16A 109.5 . . ?
N2 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N2 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 C1 C2 C10 53.9(5) . . . . ?
S14 C1 C2 C10 172.6(4) . . . . ?
C9 C1 C2 S17 172.6(3) . . . . ?
S14 C1 C2 S17 -68.7(3) . . . . ?
S19 C3 C4 S18 -2.2(5) . . . . ?
S14 C3 C4 S18 179.1(2) . . . . ?
S19 C3 C4 S17 174.8(2) . . . . ?
S14 C3 C4 S17 -3.9(6) . . . . ?
S9 C5 C6 S8 -1.8(5) . . . . ?
S4 C5 C6 S8 -179.4(2) . . . . ?
S9 C5 C6 S7 179.2(3) . . . . ?
S4 C5 C6 S7 1.6(6) . . . . ?
C11 C7 C8 C12 60.7(5) . . . . ?
S4 C7 C8 C12 177.0(4) . . . . ?
C11 C7 C8 S7 178.0(3) . . . . ?
S4 C7 C8 S7 -65.6(4) . . . . ?
C6 C5 S4 C7 -26.8(4) . . . . ?
S9 C5 S4 C7 155.5(2) . . . . ?
C8 C7 S4 C5 59.4(4) . . . . ?
C11 C7 S4 C5 179.8(3) . . . . ?
C5 C6 S7 C8 -1.4(5) . . . . ?
S8 C6 S7 C8 179.6(2) . . . . ?
C7 C8 S7 C6 34.2(4) . . . . ?
C12 C8 S7 C6 156.5(3) . . . . ?
C5 C6 S8 NI1 5.2(4) . . . . ?
S7 C6 S8 NI1 -175.64(19) . . . . ?
C6 C5 S9 NI1 -2.6(4) . . . . ?
S4 C5 S9 NI1 175.24(19) . . . . ?
C4 C3 S14 C1 -25.2(4) . . . . ?
S19 C3 S14 C1 156.1(2) . . . . ?
C2 C1 S14 C3 61.9(3) . . . . ?
C9 C1 S14 C3 -174.8(3) . . . . ?
C3 C4 S17 C2 3.3(5) . . . . ?
S18 C4 S17 C2 -179.5(2) . . . . ?
C1 C2 S17 C4 34.2(4) . . . . ?
C10 C2 S17 C4 158.2(3) . . . . ?
C3 C4 S18 NI1 5.7(4) . . . . ?
S17 C4 S18 NI1 -171.67(18) . . . . ?
C4 C3 S19 NI1 -2.6(4) . . . . ?
S14 C3 S19 NI1 176.21(18) . . . . ?

_refine_diff_density_max         1.382
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.072

####################################################################### 
# 
# 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_shelx_CCDC11
_database_code_depnum_ccdc_archive 'CCDC 2048869'
loop_
_audit_author_name
_audit_author_address
'Narcis Avarvari'
;CNRS, University of Angers
France
;
_audit_update_record             
;
2020-12-07 deposited with the CCDC.	2021-02-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H12 Ni S8'
_chemical_formula_sum            'C10 H12 Ni S8'
_chemical_formula_weight         447.39

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'
S S 0.3331 0.5567 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   5.2521(2)
_cell_length_b                   15.1161(5)
_cell_length_c                   10.1483(3)
_cell_angle_alpha                90
_cell_angle_beta                 90.181(4)
_cell_angle_gamma                90
_cell_volume                     805.68(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    149.3(6)
_cell_measurement_reflns_used    3054
_cell_measurement_theta_min      2.8260
_cell_measurement_theta_max      72.8160

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.844
_exptl_crystal_F_000             456
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    11.277
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.68741
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.613
_oxdiff_exptl_absorpt_empirical_full_max 1.637
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      149.3(6)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_reflns_number            4209
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         5.250
_diffrn_reflns_theta_max         73.106
_diffrn_reflns_theta_full        67.000
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measured_fraction_theta_full 0.946
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_Laue_measured_fraction_full 0.946
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_point_group_measured_fraction_full 0.946
_reflns_number_total             1476
_reflns_number_gt                1426
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0737P)²+4.7944P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1476
_refine_ls_number_parameters     88
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0631
_refine_ls_wR_factor_ref         0.1709
_refine_ls_wR_factor_gt          0.1615
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_restrained_S_all      1.144
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 1.160(2) -0.1319(6) 0.0888(11) 0.079(3) Uani 1 1 d . . . . .
H1 H 1.008378 -0.131788 0.032184 0.094 Uiso 1 1 calc R U . . .
C2 C 1.137(2) -0.2086(6) 0.1544(11) 0.096(5) Uani 1 1 d . . . . .
H2A H 1.296701 -0.217228 0.200588 0.115 Uiso 1 1 calc R U . . .
H2B H 1.127757 -0.254488 0.087741 0.115 Uiso 1 1 calc R U . . .
C3 C 0.8967(11) -0.0478(4) 0.2921(5) 0.0252(12) Uani 1 1 d . . . . .
C4 C 0.8093(11) -0.1295(4) 0.3327(5) 0.0261(12) Uani 1 1 d . . . . .
C5 C 1.3747(14) -0.1223(5) -0.0097(7) 0.0419(16) Uani 1 1 d . . . . .
H5A H 1.367877 -0.064485 -0.048781 0.063 Uiso 1 1 calc R U . . .
H5B H 1.534985 -0.129849 0.034585 0.063 Uiso 1 1 calc R U . . .
H5C H 1.357066 -0.166358 -0.077183 0.063 Uiso 1 1 calc R U . . .
S1 S 1.1325(3) -0.02832(10) 0.17524(15) 0.0323(4) Uani 1 1 d . . . . .
S2 S 0.8934(3) -0.23346(10) 0.27003(17) 0.0375(4) Uani 1 1 d . . . . .
S3 S 0.7751(3) 0.04557(9) 0.36229(14) 0.0284(4) Uani 1 1 d . . . . .
S4 S 0.5850(3) -0.13438(10) 0.45493(15) 0.0314(4) Uani 1 1 d . . . . .
NI1 Ni 0.500000 0.000000 0.500000 0.0258(4) Uani 1 2 d S . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.342(14) . ?
C1 C5 1.516(10) . ?
C1 S1 1.801(8) . ?
C2 S2 1.778(9) . ?
C3 C4 1.381(9) . ?
C3 S3 1.706(6) . ?
C3 S1 1.743(6) . ?
C4 S4 1.715(6) . ?
C4 S2 1.752(6) . ?
S3 NI1 2.1279(14) . ?
S4 NI1 2.1298(15) . ?
NI1 S3 2.1279(14) 3_656 ?
NI1 S4 2.1298(15) 3_656 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C5 118.6(8) . . ?
C2 C1 S1 120.1(8) . . ?
C5 C1 S1 107.3(6) . . ?
C1 C2 S2 125.2(8) . . ?
C4 C3 S3 119.4(4) . . ?
C4 C3 S1 126.3(4) . . ?
S3 C3 S1 114.3(3) . . ?
C3 C4 S4 118.9(4) . . ?
C3 C4 S2 127.5(4) . . ?
S4 C4 S2 113.5(4) . . ?
C3 S1 C1 104.0(3) . . ?
C4 S2 C2 103.4(3) . . ?
C3 S3 NI1 105.2(2) . . ?
C4 S4 NI1 105.0(2) . . ?
S3 NI1 S3 180.0 . 3_656 ?
S3 NI1 S4 91.40(5) . . ?
S3 NI1 S4 88.60(5) 3_656 . ?
S3 NI1 S4 88.60(5) . 3_656 ?
S3 NI1 S4 91.40(5) 3_656 3_656 ?
S4 NI1 S4 180.0 . 3_656 ?

_refine_diff_density_max         0.856
_refine_diff_density_min         -0.865
_refine_diff_density_rms         0.166

####################################################################### 
# 
# 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_shelx_CCDC12
_database_code_depnum_ccdc_archive 'CCDC 2048870'
loop_
_audit_author_name
_audit_author_address
'Narcis Avarvari'
;CNRS, University of Angers
France
;
_audit_update_record             
;
2020-12-07 deposited with the CCDC.	2021-02-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H16 Ni S8'
_chemical_formula_sum            'C12 H16 Ni S8'
_chemical_formula_weight         475.44

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'
S S 0.3331 0.5567 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_H-M_alt        'P 1'
_space_group_name_Hall           'P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'

_cell_length_a                   6.9052(3)
_cell_length_b                   7.7527(3)
_cell_length_c                   9.1468(3)
_cell_angle_alpha                70.732(4)
_cell_angle_beta                 76.045(3)
_cell_angle_gamma                76.463(4)
_cell_volume                     442.17(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    150.00(10)
_cell_measurement_reflns_used    4473
_cell_measurement_theta_min      5.1630
_cell_measurement_theta_max      71.8950

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_F_000             244
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    10.315
_shelx_estimated_absorpt_T_min   0.210
_shelx_estimated_absorpt_T_max   0.627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.76208
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.863
_oxdiff_exptl_absorpt_empirical_full_max 1.366
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150.00(10)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_reflns_number            5909
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_av_R_equivalents  0.0174
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         5.206
_diffrn_reflns_theta_max         72.040
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measured_fraction_theta_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.881
_diffrn_reflns_point_group_measured_fraction_full 0.919
_reflns_number_total             3083
_reflns_number_gt                3010
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.845
_reflns_Friedel_fraction_max     0.807
_reflns_Friedel_fraction_full    0.857

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

_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0375P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1329 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.038(11)
_chemical_absolute_configuration syn
_refine_ls_number_reflns         3083
_refine_ls_number_parameters     190
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0217
_refine_ls_R_factor_gt           0.0212
_refine_ls_wR_factor_ref         0.0575
_refine_ls_wR_factor_gt          0.0571
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4059(7) 0.6709(6) 0.7631(4) 0.0286(9) Uani 1 1 d . . . . .
H1A H 0.277341 0.755286 0.748855 0.043 Uiso 1 1 calc R U . . .
H1B H 0.401412 0.554150 0.745327 0.043 Uiso 1 1 calc R U . . .
H1C H 0.427931 0.646392 0.870595 0.043 Uiso 1 1 calc R U . . .
C2 C 0.8311(7) 0.5758(5) 0.8275(5) 0.0261(9) Uani 1 1 d . . . . .
H2A H 0.964439 0.496912 0.829981 0.039 Uiso 1 1 calc R U . . .
H2B H 0.830751 0.685584 0.858265 0.039 Uiso 1 1 calc R U . . .
H2C H 0.727765 0.506297 0.900888 0.039 Uiso 1 1 calc R U . . .
C3 C 0.5793(6) 0.7600(5) 0.6455(4) 0.0211(7) Uani 1 1 d . . . . .
H3 H 0.580976 0.881160 0.661413 0.025 Uiso 1 1 calc R U . . .
C4 C 0.7846(6) 0.6362(5) 0.6609(4) 0.0212(7) Uani 1 1 d . . . . .
H4 H 0.790547 0.524036 0.627919 0.025 Uiso 1 1 calc R U . . .
C5 C 0.7337(7) 0.8637(5) 0.3177(4) 0.0190(9) Uani 1 1 d . . . . .
C6 C 0.9206(8) 0.8479(5) 0.3533(5) 0.0197(9) Uani 1 1 d . . . . .
C7 C 1.0574(7) 1.1863(5) -0.3628(5) 0.0183(8) Uani 1 1 d . . . . .
C8 C 1.2371(7) 1.1934(5) -0.3249(4) 0.0186(9) Uani 1 1 d . . . . .
C9 C 1.2329(6) 1.3024(5) -0.6860(4) 0.0212(7) Uani 1 1 d . . . . .
H9 H 1.316589 1.180537 -0.693604 0.025 Uiso 1 1 calc R U . . .
C10 C 1.3543(6) 1.4083(5) -0.6372(4) 0.0202(7) Uani 1 1 d . . . . .
H10 H 1.267454 1.526742 -0.623574 0.024 Uiso 1 1 calc R U . . .
C11 C 1.1649(8) 1.4112(5) -0.8443(5) 0.0287(10) Uani 1 1 d . . . . .
H11A H 1.087625 1.338324 -0.871173 0.043 Uiso 1 1 calc R U . . .
H11B H 1.079612 1.529112 -0.836031 0.043 Uiso 1 1 calc R U . . .
H11C H 1.284164 1.435497 -0.926634 0.043 Uiso 1 1 calc R U . . .
C12 C 1.5447(7) 1.4521(6) -0.7593(4) 0.0274(9) Uani 1 1 d . . . . .
H12A H 1.618701 1.520012 -0.724038 0.041 Uiso 1 1 calc R U . . .
H12B H 1.631289 1.336188 -0.771619 0.041 Uiso 1 1 calc R U . . .
H12C H 1.505952 1.528080 -0.860448 0.041 Uiso 1 1 calc R U . . .
S1 S 0.51713(16) 0.80130(12) 0.45232(10) 0.0223(2) Uani 1 1 d . . . . .
S2 S 0.98873(15) 0.75963(12) 0.53914(10) 0.0233(2) Uani 1 1 d . . . . .
S3 S 0.70211(18) 0.94961(12) 0.12543(10) 0.0219(2) Uani 1 1 d . . . . .
S4 S 1.11551(16) 0.92415(12) 0.20459(10) 0.0212(2) Uani 1 1 d . . . . .
S5 S 0.86820(16) 1.10102(11) -0.21558(10) 0.0209(2) Uani 1 1 d . . . . .
S6 S 1.26900(17) 1.10856(13) -0.13134(10) 0.0214(2) Uani 1 1 d . . . . .
S7 S 0.99599(16) 1.26350(12) -0.54969(10) 0.0236(2) Uani 1 1 d . . . . .
S8 S 1.44830(15) 1.27567(11) -0.45507(10) 0.0225(2) Uani 1 1 d . . . . .
NI1 Ni 0.98847(16) 1.02003(10) -0.00420(10) 0.01804(14) 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
C1 C3 1.531(5) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C4 1.529(5) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.523(5) . ?
C3 S1 1.826(3) . ?
C3 H3 1.0000 . ?
C4 S2 1.821(4) . ?
C4 H4 1.0000 . ?
C5 C6 1.374(7) . ?
C5 S3 1.711(4) . ?
C5 S1 1.745(4) . ?
C6 S4 1.724(4) . ?
C6 S2 1.745(5) . ?
C7 C8 1.384(6) . ?
C7 S5 1.711(4) . ?
C7 S7 1.737(4) . ?
C8 S6 1.722(4) . ?
C8 S8 1.746(4) . ?
C9 C10 1.523(5) . ?
C9 C11 1.538(5) . ?
C9 S7 1.823(4) . ?
C9 H9 1.0000 . ?
C10 C12 1.530(5) . ?
C10 S8 1.825(3) . ?
C10 H10 1.0000 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
S3 NI1 2.1357(17) . ?
S4 NI1 2.1295(15) . ?
S5 NI1 2.1334(15) . ?
S6 NI1 2.1413(17) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 C1 H1A 109.5 . . ?
C3 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C3 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C4 C2 H2A 109.5 . . ?
C4 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C4 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 C1 112.4(3) . . ?
C4 C3 S1 111.2(2) . . ?
C1 C3 S1 104.8(3) . . ?
C4 C3 H3 109.4 . . ?
C1 C3 H3 109.4 . . ?
S1 C3 H3 109.4 . . ?
C3 C4 C2 113.3(3) . . ?
C3 C4 S2 110.9(2) . . ?
C2 C4 S2 104.4(3) . . ?
C3 C4 H4 109.4 . . ?
C2 C4 H4 109.4 . . ?
S2 C4 H4 109.4 . . ?
C6 C5 S3 119.3(3) . . ?
C6 C5 S1 126.0(3) . . ?
S3 C5 S1 114.7(3) . . ?
C5 C6 S4 119.4(3) . . ?
C5 C6 S2 127.1(3) . . ?
S4 C6 S2 113.5(3) . . ?
C8 C7 S5 119.3(3) . . ?
C8 C7 S7 126.4(3) . . ?
S5 C7 S7 114.3(3) . . ?
C7 C8 S6 119.3(3) . . ?
C7 C8 S8 127.0(3) . . ?
S6 C8 S8 113.7(3) . . ?
C10 C9 C11 112.2(3) . . ?
C10 C9 S7 112.6(2) . . ?
C11 C9 S7 103.6(3) . . ?
C10 C9 H9 109.4 . . ?
C11 C9 H9 109.4 . . ?
S7 C9 H9 109.4 . . ?
C9 C10 C12 111.8(3) . . ?
C9 C10 S8 112.7(2) . . ?
C12 C10 S8 104.6(3) . . ?
C9 C10 H10 109.2 . . ?
C12 C10 H10 109.2 . . ?
S8 C10 H10 109.2 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C5 S1 C3 105.1(2) . . ?
C6 S2 C4 103.9(2) . . ?
C5 S3 NI1 104.97(18) . . ?
C6 S4 NI1 104.70(19) . . ?
C7 S5 NI1 105.20(18) . . ?
C8 S6 NI1 104.58(18) . . ?
C7 S7 C9 105.65(19) . . ?
C8 S8 C10 104.40(19) . . ?
S4 NI1 S5 176.73(6) . . ?
S4 NI1 S3 91.60(6) . . ?
S5 NI1 S3 88.73(7) . . ?
S4 NI1 S6 88.29(6) . . ?
S5 NI1 S6 91.60(6) . . ?
S3 NI1 S6 176.13(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C3 C4 C2 -55.0(4) . . . . ?
S1 C3 C4 C2 -172.2(3) . . . . ?
C1 C3 C4 S2 -171.9(3) . . . . ?
S1 C3 C4 S2 70.9(3) . . . . ?
S3 C5 C6 S4 2.8(4) . . . . ?
S1 C5 C6 S4 -177.9(2) . . . . ?
S3 C5 C6 S2 -178.4(2) . . . . ?
S1 C5 C6 S2 1.0(5) . . . . ?
S5 C7 C8 S6 2.3(4) . . . . ?
S7 C7 C8 S6 -179.8(2) . . . . ?
S5 C7 C8 S8 -179.6(2) . . . . ?
S7 C7 C8 S8 -1.8(5) . . . . ?
C11 C9 C10 C12 -59.3(4) . . . . ?
S7 C9 C10 C12 -175.8(3) . . . . ?
C11 C9 C10 S8 -176.8(3) . . . . ?
S7 C9 C10 S8 66.8(3) . . . . ?
C6 C5 S1 C3 11.6(3) . . . . ?
S3 C5 S1 C3 -169.06(18) . . . . ?
C4 C3 S1 C5 -48.0(3) . . . . ?
C1 C3 S1 C5 -169.7(3) . . . . ?
C5 C6 S2 C4 15.7(3) . . . . ?
S4 C6 S2 C4 -165.40(18) . . . . ?
C3 C4 S2 C6 -51.9(3) . . . . ?
C2 C4 S2 C6 -174.2(2) . . . . ?
C6 C5 S3 NI1 -2.6(3) . . . . ?
S1 C5 S3 NI1 178.01(16) . . . . ?
C5 C6 S4 NI1 -1.4(3) . . . . ?
S2 C6 S4 NI1 179.56(14) . . . . ?
C8 C7 S5 NI1 -1.7(3) . . . . ?
S7 C7 S5 NI1 -179.78(15) . . . . ?
C7 C8 S6 NI1 -1.7(3) . . . . ?
S8 C8 S6 NI1 -179.96(15) . . . . ?
C8 C7 S7 C9 13.1(3) . . . . ?
S5 C7 S7 C9 -168.95(19) . . . . ?
C10 C9 S7 C7 -46.0(3) . . . . ?
C11 C9 S7 C7 -167.5(2) . . . . ?
C7 C8 S8 C10 16.0(3) . . . . ?
S6 C8 S8 C10 -165.87(18) . . . . ?
C9 C10 S8 C8 -48.9(3) . . . . ?
C12 C10 S8 C8 -170.5(2) . . . . ?

_refine_diff_density_max         0.320
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.063

####################################################################### 
# 
# 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_shelx_CCDC13
_database_code_depnum_ccdc_archive 'CCDC 2048871'
loop_
_audit_author_name
_audit_author_address
'Narcis Avarvari'
;CNRS, University of Angers
France
;
_audit_update_record             
;
2020-12-07 deposited with the CCDC.	2021-02-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H16 Ni S8'
_chemical_formula_sum            'C12 H16 Ni S8'
_chemical_formula_weight         475.44

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'
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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.9552(7)
_cell_length_b                   7.8717(8)
_cell_length_c                   9.1681(9)
_cell_angle_alpha                69.989(9)
_cell_angle_beta                 74.837(8)
_cell_angle_gamma                72.895(9)
_cell_volume                     443.49(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    150.01(10)
_cell_measurement_reflns_used    1838
_cell_measurement_theta_min      5.1890
_cell_measurement_theta_max      73.2140

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_F_000             244
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_exptl_absorpt_coefficient_mu    10.284
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.76270
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.695
_oxdiff_exptl_absorpt_empirical_full_max 1.458
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150.01(10)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_reflns_number            2933
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         5.219
_diffrn_reflns_theta_max         73.758
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             1716
_reflns_number_gt                1644
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0598P)²+0.6396P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1716
_refine_ls_number_parameters     115
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0374
_refine_ls_wR_factor_ref         0.1140
_refine_ls_wR_factor_gt          0.1034
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_restrained_S_all      1.160
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C3A C 0.1434(8) 0.1139(8) 0.1350(6) 0.0131(10) Uani 0.5 1 d . . P A 1
H3A H 0.229350 -0.005653 0.123109 0.016 Uiso 0.5 1 calc R U P A 1
C4A C 0.2569(9) 0.2222(9) 0.1859(6) 0.0113(11) Uani 0.5 1 d . . P A 1
H4A H 0.168760 0.339062 0.202516 0.014 Uiso 0.5 1 calc R U P A 1
C3B C 0.1036(13) 0.2258(16) 0.1496(9) 0.041(2) Uani 0.5 1 d . . P A 2
H3B H 0.070760 0.342909 0.175988 0.049 Uiso 0.5 1 calc R U P A 2
C4B C 0.3115(14) 0.1250(14) 0.1647(8) 0.0348(17) Uani 0.5 1 d . . P A 2
H4B H 0.340431 0.007258 0.140118 0.042 Uiso 0.5 1 calc R U P A 2
C5 C 0.2524(5) 0.3362(4) -0.1780(3) 0.0205(6) Uani 1 1 d . . . . .
C6 C 0.4340(5) 0.3349(4) -0.1415(3) 0.0198(6) Uani 1 1 d . . . . .
C1 C -0.0516(7) 0.0922(8) 0.2616(5) 0.0552(13) Uani 1 1 d . . . . .
H1A H -0.127620 0.025939 0.235612 0.083 Uiso 1 1 calc R U . A 1
H1B H -0.013775 0.024570 0.362855 0.083 Uiso 1 1 calc R U . A 1
H1C H -0.134550 0.212696 0.264920 0.083 Uiso 1 1 calc R U . A 1
C2 C 0.3435(7) 0.0888(6) 0.3383(4) 0.0414(10) Uani 1 1 d . . . . .
H2A H 0.414423 0.151952 0.372558 0.062 Uiso 1 1 calc R U . A 1
H2B H 0.232490 0.052877 0.420483 0.062 Uiso 1 1 calc R U . A 1
H2C H 0.436179 -0.019714 0.314757 0.062 Uiso 1 1 calc R U . A 1
NI1 Ni 0.500000 0.500000 -0.500000 0.0192(2) Uani 1 2 d S . P . .
S1 S 0.04278(12) 0.26213(12) -0.04511(9) 0.0267(2) Uani 1 1 d . . . . .
S2 S 0.49737(12) 0.25640(12) 0.04569(8) 0.0256(2) Uani 1 1 d . . . . .
S3 S 0.22086(11) 0.41991(11) -0.37120(8) 0.0238(2) Uani 1 1 d . . . . .
S4 S 0.62234(11) 0.41444(11) -0.28953(8) 0.0227(2) 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
C3Aa C1 1.547(6) . ?
C3Aa C4A 1.558(8) . ?
C3Aa S1 1.839(5) . ?
C4Aa C2 1.575(6) . ?
C4Aa S2 1.851(5) . ?
C3Bb C4B 1.447(13) . ?
C3Bb C1 1.636(9) . ?
C3Bb S1 1.849(8) . ?
C4Bb C2 1.582(8) . ?
C4Bb S2 1.791(7) . ?
C5 C6 1.386(5) . ?
C5 S3 1.714(3) . ?
C5 S1 1.742(3) . ?
C6 S4 1.709(3) . ?
C6 S2 1.740(3) . ?
NI1 S4 2.1292(7) 2_664 ?
NI1 S4 2.1292(7) . ?
NI1 S3 2.1383(8) 2_664 ?
NI1 S3 2.1383(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 C3Aa C4A 106.1(4) . . ?
C1 C3Aa S1 103.5(3) . . ?
C4Aa C3Aa S1 109.5(4) . . ?
C3Aa C4Aa C2 107.6(4) . . ?
C3Aa C4Aa S2 111.1(4) . . ?
C2 C4Aa S2 100.7(3) . . ?
C4Bb C3Bb C1 108.7(7) . . ?
C4Bb C3Bb S1 113.3(7) . . ?
C1 C3Bb S1 99.6(5) . . ?
C3Bb C4Bb C2 109.4(7) . . ?
C3Bb C4Bb S2 113.1(6) . . ?
C2 C4Bb S2 103.1(5) . . ?
C6 C5 S3 119.1(2) . . ?
C6 C5 S1 126.5(2) . . ?
S3 C5 S1 114.40(18) . . ?
C5 C6 S4 119.5(2) . . ?
C5 C6 S2 126.5(2) . . ?
S4 C6 S2 114.00(18) . . ?
S4 NI1 S4 180.0 2_664 . ?
S4 NI1 S3 91.60(3) 2_664 2_664 ?
S4 NI1 S3 88.40(3) . 2_664 ?
S4 NI1 S3 88.40(3) 2_664 . ?
S4 NI1 S3 91.60(3) . . ?
S3 NI1 S3 180.0 2_664 . ?
C5 S1 C3A 105.0(2) . . ?
C5 S1 C3B 103.5(3) . . ?
C6 S2 C4B 103.9(3) . . ?
C6 S2 C4A 105.7(2) . . ?
C5 S3 NI1 104.80(11) . . ?
C6 S4 NI1 105.04(11) . . ?

_refine_diff_density_max         0.497
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.111

####################################################################### 
# 
# 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_shelx_CCDC14
_database_code_depnum_ccdc_archive 'CCDC 2048862'
loop_
_audit_author_name
_audit_author_address
'Narcis Avarvari'
;CNRS, University of Angers
France
;
_audit_update_record             
;
2020-12-07 deposited with the CCDC.	2021-02-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H52 N Ni S8'
_chemical_formula_sum            'C28 H52 N Ni S8'
_chemical_formula_weight         717.89

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'
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'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.9746(3)
_cell_length_b                   12.8587(4)
_cell_length_c                   15.4306(5)
_cell_angle_alpha                81.684(3)
_cell_angle_beta                 80.287(3)
_cell_angle_gamma                69.560(3)
_cell_volume                     1820.05(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    297(1)
_cell_measurement_reflns_used    6633
_cell_measurement_theta_min      3.6180
_cell_measurement_theta_max      72.9330

_exptl_crystal_description       hexagon
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_F_000             766
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    5.192
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.68634
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.737
_oxdiff_exptl_absorpt_empirical_full_max 1.526
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      297(1)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_reflns_number            12621
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.918
_diffrn_reflns_theta_max         73.509
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7089
_reflns_number_gt                6001
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0935P)²+0.3959P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7089
_refine_ls_number_parameters     382
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0516
_refine_ls_wR_factor_ref         0.1639
_refine_ls_wR_factor_gt          0.1455
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1A C 0.4293(8) 0.1866(6) 0.0264(5) 0.0639(16) Uani 0.5 1 d . . P A 1
H1 H 0.476944 0.127310 -0.012972 0.077 Uiso 0.5 1 calc R U P A 1
C2A C 0.4369(9) 0.1403(7) 0.1242(5) 0.0667(19) Uani 0.5 1 d . . P A 1
H2 H 0.392427 0.200606 0.162981 0.080 Uiso 0.5 1 calc R U P A 1
C7A C 0.0732(11) 0.6602(8) 0.8048(5) 0.087(2) Uani 0.5 1 d D . P B 1
H7 H -0.026175 0.699401 0.829380 0.105 Uiso 0.5 1 calc R U P B 1
C8A C 0.1550(13) 0.7409(9) 0.7952(7) 0.096(3) Uani 0.5 1 d D . P B 1
H8 H 0.140751 0.768324 0.853261 0.115 Uiso 0.5 1 calc R U P B 1
C1B C 0.3923(10) 0.2258(8) 0.0637(7) 0.086(2) Uani 0.5 1 d . . P A 2
H1B H 0.359957 0.262227 0.118692 0.103 Uiso 0.5 1 calc R U P A 2
C2B C 0.4659(9) 0.1091(7) 0.0871(7) 0.0745(18) Uani 0.5 1 d . . P A 2
H2B H 0.501654 0.074264 0.031528 0.089 Uiso 0.5 1 calc R U P A 2
C7B C 0.0571(11) 0.7223(9) 0.7679(6) 0.093(3) Uani 0.5 1 d . . P B 2
H7B H -0.036023 0.737940 0.805455 0.112 Uiso 0.5 1 calc R U P B 2
C8B C 0.1776(13) 0.6748(11) 0.8282(7) 0.103(3) Uani 0.5 1 d . . P B 2
H8B H 0.156512 0.726026 0.873777 0.124 Uiso 0.5 1 calc R U P B 2
C3 C 0.1764(3) 0.1443(3) 0.0261(2) 0.0640(7) Uani 1 1 d . . . . .
C4 C 0.2228(3) 0.0550(3) 0.08404(19) 0.0628(7) Uani 1 1 d . . . . .
C5 C 0.4979(6) 0.2808(4) 0.0057(4) 0.0991(13) Uani 1 1 d . . . . .
H5A H 0.493219 0.309638 -0.055099 0.149 Uiso 1 1 calc R U . A 1
H5B H 0.445943 0.339607 0.042878 0.149 Uiso 1 1 calc R U . A 1
H5C H 0.596848 0.251079 0.016513 0.149 Uiso 1 1 calc R U . A 1
C6 C 0.5968(4) 0.0811(4) 0.1366(3) 0.0868(10) Uani 1 1 d . . . . .
H6A H 0.604121 0.051612 0.197044 0.130 Uiso 1 1 calc R U . A 1
H6B H 0.638026 0.021410 0.099043 0.130 Uiso 1 1 calc R U . A 1
H6C H 0.647912 0.133464 0.121301 0.130 Uiso 1 1 calc R U . A 1
C9 C 0.2464(3) 0.5896(2) 0.6436(2) 0.0619(7) Uani 1 1 d . . . . .
C10 C 0.3571(4) 0.6053(3) 0.6735(2) 0.0669(7) Uani 1 1 d . . . . .
C11 C 0.1395(9) 0.5630(6) 0.8751(4) 0.164(3) Uani 1 1 d D . . . .
H11A H 0.089335 0.510099 0.882649 0.247 Uiso 1 1 calc R U . B 1
H11B H 0.239692 0.526790 0.855507 0.247 Uiso 1 1 calc R U . B 1
H11C H 0.129969 0.592535 0.930400 0.247 Uiso 1 1 calc R U . B 1
C12 C 0.0824(9) 0.8424(5) 0.7321(5) 0.165(3) Uani 1 1 d D . . . .
H12A H 0.133021 0.894918 0.725120 0.248 Uiso 1 1 calc R U . B 1
H12B H 0.085070 0.818126 0.675650 0.248 Uiso 1 1 calc R U . B 1
H12C H -0.016057 0.877219 0.756284 0.248 Uiso 1 1 calc R U . B 1
C13 C 0.1640(4) 0.2028(3) 0.7017(2) 0.0713(8) Uani 1 1 d . . . . .
H13A H 0.122237 0.182591 0.760351 0.086 Uiso 1 1 calc R U . . .
H13B H 0.230734 0.134680 0.678481 0.086 Uiso 1 1 calc R U . . .
C14 C 0.2488(5) 0.2774(3) 0.7099(3) 0.0877(11) Uani 1 1 d . . . . .
H14A H 0.275983 0.309395 0.651608 0.105 Uiso 1 1 calc R U . . .
H14B H 0.187907 0.338158 0.744368 0.105 Uiso 1 1 calc R U . . .
C15 C 0.3809(4) 0.2163(3) 0.7527(3) 0.0827(9) Uani 1 1 d . . . . .
H15A H 0.438573 0.152944 0.720106 0.099 Uiso 1 1 calc R U . . .
H15B H 0.352872 0.187887 0.812106 0.099 Uiso 1 1 calc R U . . .
C16 C 0.4716(5) 0.2870(4) 0.7571(4) 0.1000(13) Uani 1 1 d . . . . .
H16A H 0.554960 0.243033 0.785232 0.150 Uiso 1 1 calc R U . . .
H16B H 0.501804 0.314003 0.698391 0.150 Uiso 1 1 calc R U . . .
H16C H 0.416052 0.348967 0.790445 0.150 Uiso 1 1 calc R U . . .
C17 C 0.1038(5) 0.2841(3) 0.5506(2) 0.0798(10) Uani 1 1 d . . . . .
H17A H 0.024153 0.317444 0.515894 0.096 Uiso 1 1 calc R U . . .
H17B H 0.146117 0.340844 0.553257 0.096 Uiso 1 1 calc R U . . .
C18 C 0.2150(6) 0.1910(5) 0.5031(3) 0.1035(14) Uani 1 1 d . . . . .
H18A H 0.289374 0.150753 0.540477 0.124 Uiso 1 1 calc R U . . .
H18B H 0.170041 0.139462 0.491592 0.124 Uiso 1 1 calc R U . . .
C19 C 0.2821(7) 0.2337(7) 0.4179(4) 0.138(2) Uani 1 1 d . . . . .
H19A H 0.319090 0.289975 0.429707 0.165 Uiso 1 1 calc R U . . .
H19B H 0.207660 0.269621 0.379749 0.165 Uiso 1 1 calc R U . . .
C20 C 0.4016(9) 0.1470(7) 0.3697(4) 0.162(3) Uani 1 1 d . . . . .
H20A H 0.438494 0.181327 0.315986 0.243 Uiso 1 1 calc R U . . .
H20B H 0.477446 0.112225 0.406095 0.243 Uiso 1 1 calc R U . . .
H20C H 0.365815 0.091834 0.356047 0.243 Uiso 1 1 calc R U . . .
C21 C -0.0248(4) 0.1634(3) 0.6432(2) 0.0701(8) Uani 1 1 d . . . . .
H21A H 0.049642 0.096617 0.622826 0.084 Uiso 1 1 calc R U . . .
H21B H -0.062259 0.144811 0.703406 0.084 Uiso 1 1 calc R U . . .
C22 C -0.1459(5) 0.1959(3) 0.5863(3) 0.0854(10) Uani 1 1 d . . . . .
H22A H -0.221977 0.261732 0.606914 0.102 Uiso 1 1 calc R U . . .
H22B H -0.109600 0.214664 0.525850 0.102 Uiso 1 1 calc R U . . .
C23 C -0.2070(5) 0.1048(4) 0.5884(3) 0.0961(12) Uani 1 1 d . . . . .
H23A H -0.248100 0.088831 0.648266 0.115 Uiso 1 1 calc R U . . .
H23B H -0.130089 0.037827 0.570679 0.115 Uiso 1 1 calc R U . . .
C24 C -0.3217(6) 0.1359(5) 0.5279(4) 0.1163(17) Uani 1 1 d . . . . .
H24A H -0.358513 0.075540 0.530860 0.174 Uiso 1 1 calc R U . . .
H24B H -0.398806 0.201409 0.545884 0.174 Uiso 1 1 calc R U . . .
H24C H -0.280887 0.150445 0.468358 0.174 Uiso 1 1 calc R U . . .
C25 C -0.0667(4) 0.3578(3) 0.6784(3) 0.0779(9) Uani 1 1 d . . . . .
H25A H -0.018732 0.412070 0.676899 0.093 Uiso 1 1 calc R U . . .
H25B H -0.139607 0.388260 0.638614 0.093 Uiso 1 1 calc R U . . .
C26 C -0.1404(6) 0.3437(4) 0.7699(3) 0.1007(13) Uani 1 1 d . . . . .
H26A H -0.200842 0.298741 0.770272 0.121 Uiso 1 1 calc R U . . .
H26B H -0.068338 0.304569 0.809123 0.121 Uiso 1 1 calc R U . . .
C27 C -0.2301(9) 0.4524(6) 0.8031(5) 0.146(3) Uani 1 1 d . . . . .
H27A H -0.171689 0.500592 0.792941 0.176 Uiso 1 1 calc R U . . .
H27B H -0.308728 0.485908 0.767619 0.176 Uiso 1 1 calc R U . . .
C28 C -0.2860(14) 0.4521(9) 0.8869(8) 0.254(7) Uani 1 1 d . . . . .
H28A H -0.341426 0.526995 0.900129 0.381 Uiso 1 1 calc R U . . .
H28B H -0.347428 0.407182 0.898040 0.381 Uiso 1 1 calc R U . . .
H28C H -0.209856 0.421924 0.923460 0.381 Uiso 1 1 calc R U . . .
N1 N 0.0439(3) 0.2518(2) 0.64360(18) 0.0662(6) Uani 1 1 d . . . . .
S1 S 0.23804(11) 0.25913(8) 0.00773(7) 0.0809(3) Uani 1 1 d . . . . .
S2 S 0.35326(11) 0.03284(10) 0.15368(6) 0.0855(3) Uani 1 1 d . . . . .
S3 S 0.04687(9) 0.15258(7) -0.03870(5) 0.0695(2) Uani 1 1 d . . . . .
S4 S 0.15355(9) -0.05308(7) 0.09368(5) 0.0662(2) Uani 1 1 d . . . . .
S5 S 0.06638(10) 0.62477(10) 0.69306(7) 0.0907(3) Uani 1 1 d . . . . .
S6 S 0.35219(14) 0.66483(13) 0.77009(8) 0.1088(4) Uani 1 1 d . . . . .
S7 S 0.27572(7) 0.52844(6) 0.54635(5) 0.05907(19) Uani 1 1 d . . . . .
S8 S 0.52701(9) 0.56436(8) 0.61350(5) 0.0723(2) Uani 1 1 d . . . . .
NI1 Ni 0.000000 0.000000 0.000000 0.0595(2) Uani 1 2 d S . P . .
NI2 Ni 0.500000 0.500000 0.500000 0.05125(17) Uani 1 2 d S . P . .


_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
C1Aa C2A 1.544(10) . ?
C1Aa C5 1.559(8) . ?
C1Aa S1 1.859(8) . ?
C2Aa C6 1.540(9) . ?
C2Aa S2 1.819(8) . ?
C7Aa C8A 1.507(18) . ?
C7Aa C11 1.566(11) . ?
C7Aa S5 1.863(9) . ?
C8Aa C12 1.544(12) . ?
C8Aa S6 1.867(11) . ?
C1Bb C2B 1.444(13) . ?
C1Bb C5 1.559(10) . ?
C1Bb S1 1.783(9) . ?
C2Bb C6 1.531(9) . ?
C2Bb S2 1.835(8) . ?
C7Bb C8B 1.544(17) . ?
C7Bb C12 1.653(14) . ?
C7Bb S5 1.793(11) . ?
C8Bb C11 1.650(16) . ?
C8Bb S6 1.790(12) . ?
C3 C4 1.343(5) . ?
C3 S3 1.729(3) . ?
C3 S1 1.758(3) . ?
C4 S4 1.735(3) . ?
C4 S2 1.747(3) . ?
C9 C10 1.352(5) . ?
C9 S7 1.729(3) . ?
C9 S5 1.755(3) . ?
C10 S8 1.730(3) . ?
C10 S6 1.757(3) . ?
C13 C14 1.514(5) . ?
C13 N1 1.519(4) . ?
C14 C15 1.486(5) . ?
C15 C16 1.504(6) . ?
C17 C18 1.500(7) . ?
C17 N1 1.517(4) . ?
C18 C19 1.493(6) . ?
C19 C20 1.493(10) . ?
C21 C22 1.517(5) . ?
C21 N1 1.520(4) . ?
C22 C23 1.492(5) . ?
C23 C24 1.508(7) . ?
C25 C26 1.496(6) . ?
C25 N1 1.525(5) . ?
C26 C27 1.481(7) . ?
C27 C28 1.319(13) . ?
S3 NI1 2.1522(9) . ?
S4 NI1 2.1523(7) . ?
S7 NI2 2.1481(7) . ?
S8 NI2 2.1352(7) . ?
NI1 S3 2.1522(9) 2 ?
NI1 S4 2.1523(7) 2 ?
NI2 S8 2.1352(7) 2_666 ?
NI2 S7 2.1480(7) 2_666 ?

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
C2Aa C1Aa C5 109.4(6) . . ?
C2Aa C1Aa S1 109.9(5) . . ?
C5 C1Aa S1 103.8(4) . . ?
C6 C2Aa C1A 108.0(6) . . ?
C6 C2Aa S2 105.2(5) . . ?
C1Aa C2Aa S2 111.6(5) . . ?
C8Aa C7Aa C11 107.6(10) . . ?
C8Aa C7Aa S5 109.0(7) . . ?
C11 C7Aa S5 118.4(6) . . ?
C7Aa C8Aa C12 108.2(11) . . ?
C7Aa C8Aa S6 109.5(7) . . ?
C12 C8Aa S6 118.9(7) . . ?
C2Bb C1Bb C5 110.7(8) . . ?
C2Bb C1Bb S1 116.8(7) . . ?
C5 C1Bb S1 107.4(6) . . ?
C1Bb C2Bb C6 116.5(7) . . ?
C1Bb C2Bb S2 115.5(7) . . ?
C6 C2Bb S2 104.8(5) . . ?
C8Bb C7Bb C12 98.4(10) . . ?
C8Bb C7Bb S5 111.8(7) . . ?
C12 C7Bb S5 121.6(6) . . ?
C7Bb C8Bb C11 99.1(10) . . ?
C7Bb C8Bb S6 112.7(8) . . ?
C11 C8Bb S6 121.5(7) . . ?
C4 C3 S3 120.3(3) . . ?
C4 C3 S1 125.2(3) . . ?
S3 C3 S1 114.45(18) . . ?
C3 C4 S4 120.0(3) . . ?
C3 C4 S2 126.3(3) . . ?
S4 C4 S2 113.74(18) . . ?
C10 C9 S7 119.9(2) . . ?
C10 C9 S5 127.3(2) . . ?
S7 C9 S5 112.86(18) . . ?
C9 C10 S8 119.5(2) . . ?
C9 C10 S6 127.5(3) . . ?
S8 C10 S6 112.99(19) . . ?
C14 C13 N1 115.9(3) . . ?
C15 C14 C13 112.3(3) . . ?
C14 C15 C16 113.4(4) . . ?
C18 C17 N1 115.7(3) . . ?
C19 C18 C17 111.5(5) . . ?
C18 C19 C20 114.9(6) . . ?
C22 C21 N1 115.2(3) . . ?
C23 C22 C21 112.2(3) . . ?
C22 C23 C24 111.7(4) . . ?
C26 C25 N1 115.4(3) . . ?
C27 C26 C25 111.8(5) . . ?
C28 C27 C26 117.5(8) . . ?
C17 N1 C13 110.5(3) . . ?
C17 N1 C21 110.6(3) . . ?
C13 N1 C21 107.3(2) . . ?
C17 N1 C25 106.8(3) . . ?
C13 N1 C25 110.7(3) . . ?
C21 N1 C25 111.1(3) . . ?
C3 S1 C1B 108.4(3) . . ?
C3 S1 C1A 99.4(2) . . ?
C4 S2 C2A 108.9(3) . . ?
C4 S2 C2B 100.5(3) . . ?
C3 S3 NI1 104.13(12) . . ?
C4 S4 NI1 104.09(11) . . ?
C9 S5 C7B 102.2(4) . . ?
C9 S5 C7A 103.7(3) . . ?
C10 S6 C8B 103.5(4) . . ?
C10 S6 C8A 101.2(4) . . ?
C9 S7 NI2 104.38(11) . . ?
C10 S8 NI2 104.85(11) . . ?
S3 NI1 S3 180.0 2 . ?
S3 NI1 S4 91.48(3) 2 2 ?
S3 NI1 S4 88.52(3) . 2 ?
S3 NI1 S4 88.52(3) 2 . ?
S3 NI1 S4 91.48(3) . . ?
S4 NI1 S4 180.00(3) 2 . ?
S8 NI2 S8 180.00(5) . 2_666 ?
S8 NI2 S7 88.63(3) . 2_666 ?
S8 NI2 S7 91.38(3) 2_666 2_666 ?
S8 NI2 S7 91.37(3) . . ?
S8 NI2 S7 88.62(3) 2_666 . ?
S7 NI2 S7 180.0 2_666 . ?

_refine_diff_density_max         0.577
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.064

####################################################################### 
# 
# 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_shelx_CCDC15
_database_code_depnum_ccdc_archive 'CCDC 2048866'
loop_
_audit_author_name
_audit_author_address
'Narcis Avarvari'
;CNRS, University of Angers
France
;
_audit_update_record             
;
2020-12-07 deposited with the CCDC.	2021-02-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H28 N Ni S8'
_chemical_formula_sum            'C16 H28 N Ni S8'
_chemical_formula_weight         549.58

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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   27.1336(11)
_cell_length_b                   9.9785(3)
_cell_length_c                   15.7836(7)
_cell_angle_alpha                90
_cell_angle_beta                 145.935(3)
_cell_angle_gamma                90
_cell_volume                     2393.70(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    148.70(10)
_cell_measurement_reflns_used    3087
_cell_measurement_theta_min      5.2650
_cell_measurement_theta_max      73.1550

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_F_000             1148
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    7.712
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.58126
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.616
_oxdiff_exptl_absorpt_empirical_full_max 1.787
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      148.70(10)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_reflns_number            4853
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         5.303
_diffrn_reflns_theta_max         73.476
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             2329
_reflns_number_gt                2084
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0538P)²+5.8700P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2329
_refine_ls_number_parameters     138
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0387
_refine_ls_wR_factor_ref         0.1147
_refine_ls_wR_factor_gt          0.1020
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.106
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1A C 0.4815(4) 0.3004(6) 0.5428(7) 0.0282(11) Uani 0.5 1 d . . P A 1
H1A H 0.499179 0.345443 0.515490 0.034 Uiso 0.5 1 calc R U P A 1
C2A C 0.5321(4) 0.3512(7) 0.6935(7) 0.0282(13) Uani 0.5 1 d . . P A 1
H2A H 0.515636 0.299948 0.720515 0.034 Uiso 0.5 1 calc R U P A 1
C1B C 0.4744(4) 0.2675(7) 0.5867(9) 0.0452(17) Uani 0.5 1 d . . P A 2
H1B H 0.475731 0.244424 0.648893 0.054 Uiso 0.5 1 calc R U P A 2
C2B C 0.5392(4) 0.3715(7) 0.6592(8) 0.0368(15) Uani 0.5 1 d . . P A 2
H2B H 0.537206 0.391721 0.595680 0.044 Uiso 0.5 1 calc R U P A 2
C3 C 0.34947(19) 0.4825(3) 0.3855(3) 0.0304(6) Uani 1 1 d . . . . .
C4 C 0.41074(18) 0.5686(3) 0.5049(3) 0.0310(6) Uani 1 1 d . . . . .
C5 C 0.4966(3) 0.1417(4) 0.5617(5) 0.0765(17) Uani 1 1 d . . . . .
H5A H 0.466385 0.104588 0.470641 0.115 Uiso 1 1 calc R U . A 1
H5B H 0.558433 0.123127 0.644988 0.115 Uiso 1 1 calc R U . A 1
H5C H 0.474197 0.102140 0.580792 0.115 Uiso 1 1 calc R U . A 1
C6 C 0.6334(2) 0.3364(4) 0.8189(4) 0.0499(9) Uani 1 1 d . . . . .
H6A H 0.666475 0.367357 0.913998 0.075 Uiso 1 1 calc R U . A 1
H6B H 0.647016 0.243969 0.827729 0.075 Uiso 1 1 calc R U . A 1
H6C H 0.648463 0.388916 0.791505 0.075 Uiso 1 1 calc R U . A 1
C7 C 0.1738(6) 0.2820(10) 0.4082(9) 0.185(5) Uani 1 1 d . . . . .
H7A H 0.124610 0.339845 0.348938 0.278 Uiso 1 1 calc R U . . .
H7B H 0.161296 0.226466 0.342199 0.278 Uiso 1 1 calc R U . . .
H7C H 0.184208 0.226461 0.471669 0.278 Uiso 1 1 calc R U . . .
C8 C 0.2332(3) 0.4473(5) 0.4007(5) 0.0591(10) Uani 1 1 d . . . . .
H8A H 0.284305 0.500698 0.461990 0.089 Uiso 1 1 calc R U . . .
H8B H 0.220388 0.391848 0.334341 0.089 Uiso 1 1 calc R U . . .
H8C H 0.183935 0.504906 0.341790 0.089 Uiso 1 1 calc R U . . .
N1 N 0.250000 0.3609(4) 0.500000 0.0424(9) Uani 1 2 d S T P . .
NI1 Ni 0.250000 0.750000 0.250000 0.0276(2) Uani 1 2 d S . P . .
S1 S 0.36261(5) 0.30871(8) 0.39311(9) 0.0401(2) Uani 1 1 d . . . . .
S2 S 0.51729(5) 0.52721(9) 0.68965(9) 0.0516(3) Uani 1 1 d . . . . .
S3 S 0.24637(4) 0.54142(7) 0.21033(8) 0.0316(2) Uani 1 1 d . . . . .
S4 S 0.38588(5) 0.73691(7) 0.47985(8) 0.0352(2) 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
C1Aa C2A 1.545(9) . ?
C1Aa C5 1.601(7) . ?
C1Aa S1 1.835(6) . ?
C2Aa C6 1.574(7) . ?
C2Aa S2 1.792(7) . ?
C1Bb C2B 1.463(11) . ?
C1Bb C5 1.578(9) . ?
C1Bb S1 1.831(7) . ?
C2Bb C6 1.528(7) . ?
C2Bb S2 1.863(7) . ?
C3 C4 1.364(4) . ?
C3 S3 1.732(3) . ?
C3 S1 1.755(3) . ?
C4 S4 1.730(3) . ?
C4 S2 1.751(3) . ?
C7 N1 1.425(6) . ?
C8 N1 1.490(5) . ?
N1 C7 1.425(6) 2_556 ?
N1 C8 1.490(5) 2_556 ?
NI1 S4 2.1473(7) 7_565 ?
NI1 S4 2.1474(7) . ?
NI1 S3 2.1521(7) 7_565 ?
NI1 S3 2.1522(7) . ?

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
C2Aa C1Aa C5 105.9(5) . . ?
C2Aa C1Aa S1 109.9(4) . . ?
C5 C1Aa S1 101.0(4) . . ?
C1Aa C2Aa C6 107.8(5) . . ?
C1Aa C2Aa S2 112.4(5) . . ?
C6 C2Aa S2 104.1(4) . . ?
C2Bb C1Bb C5 107.5(6) . . ?
C2Bb C1Bb S1 113.7(6) . . ?
C5 C1Bb S1 102.1(5) . . ?
C1Bb C2Bb C6 114.3(6) . . ?
C1Bb C2Bb S2 111.1(6) . . ?
C6 C2Bb S2 102.8(4) . . ?
C4 C3 S3 120.0(2) . . ?
C4 C3 S1 125.6(2) . . ?
S3 C3 S1 114.35(17) . . ?
C3 C4 S4 119.8(2) . . ?
C3 C4 S2 126.4(2) . . ?
S4 C4 S2 113.75(17) . . ?
C7 N1 C7 112.9(10) . 2_556 ?
C7 N1 C8 109.1(4) . . ?
C7 N1 C8 108.1(4) 2_556 . ?
C7 N1 C8 108.1(4) . 2_556 ?
C7 N1 C8 109.1(4) 2_556 2_556 ?
C8 N1 C8 109.4(4) . 2_556 ?
S4 NI1 S4 180.0 7_565 . ?
S4 NI1 S3 91.92(3) 7_565 7_565 ?
S4 NI1 S3 88.08(3) . 7_565 ?
S4 NI1 S3 88.08(3) 7_565 . ?
S4 NI1 S3 91.92(3) . . ?
S3 NI1 S3 180.0 7_565 . ?
C3 S1 C1B 107.3(3) . . ?
C3 S1 C1A 100.0(2) . . ?
C4 S2 C2A 107.6(2) . . ?
C4 S2 C2B 101.9(2) . . ?
C3 S3 NI1 103.85(10) . . ?
C4 S4 NI1 104.11(10) . . ?

_refine_diff_density_max         0.600
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.084

####################################################################### 
# 
# 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_shelx_CCDC16
_database_code_depnum_ccdc_archive 'CCDC 2048867'
loop_
_audit_author_name
_audit_author_address
'Narcis Avarvari'
;CNRS, University of Angers
France
;
_audit_update_record             
;
2020-12-07 deposited with the CCDC.	2021-02-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H12 Ni S8'
_chemical_formula_sum            'C10 H12 Ni S8'
_chemical_formula_weight         447.39

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'
S S 0.3331 0.5567 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   5.2529(2)
_cell_length_b                   15.0859(4)
_cell_length_c                   10.1409(3)
_cell_angle_alpha                90
_cell_angle_beta                 90.135(3)
_cell_angle_gamma                90
_cell_volume                     803.61(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    150.00(10)
_cell_measurement_reflns_used    3880
_cell_measurement_theta_min      4.3790
_cell_measurement_theta_max      73.2360

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.849
_exptl_crystal_F_000             456
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    11.306
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.59863
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.740
_oxdiff_exptl_absorpt_empirical_full_max 1.834
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150.00(10)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_reflns_number            7587
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         4.360
_diffrn_reflns_theta_max         73.517
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measured_fraction_theta_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_point_group_measured_fraction_full 0.950
_reflns_number_total             2969
_reflns_number_gt                2777
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.844
_reflns_Friedel_fraction_max     0.875
_reflns_Friedel_fraction_full    0.925

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

_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND 3.2k (Crystal Impact GbR, 2014)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0123P)²+3.0995P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1162 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(3)
_chemical_absolute_configuration syn
_refine_ls_number_reflns         2969
_refine_ls_number_parameters     172
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0363
_refine_ls_wR_factor_ref         0.0963
_refine_ls_wR_factor_gt          0.0883
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_restrained_S_all      1.127
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.871(3) 0.9029(9) 1.2552(11) 0.041(3) Uani 1 1 d . . . . .
H1A H -1.006893 0.861031 1.244114 0.061 Uiso 1 1 calc R U . . .
H1B H -0.749376 0.879901 1.317342 0.061 Uiso 1 1 calc R U . . .
H1C H -0.938134 0.957883 1.287445 0.061 Uiso 1 1 calc R U . . .
C2 C -0.7420(18) 0.9182(6) 1.1245(9) 0.031(2) Uani 1 1 d . . . . .
H2 H -0.868846 0.941030 1.062236 0.037 Uiso 1 1 calc R U . . .
C3 C -0.5257(19) 0.9827(6) 1.1312(9) 0.032(2) Uani 1 1 d . . . . .
H3A H -0.392632 0.957504 1.186077 0.038 Uiso 1 1 calc R U . . .
H3B H -0.585216 1.036216 1.174435 0.038 Uiso 1 1 calc R U . . .
C4 C -0.402(2) 0.8277(8) 0.9508(9) 0.026(2) Uani 1 1 d . . . . .
C5 C -0.305(2) 0.9088(8) 0.9128(9) 0.025(2) Uani 1 1 d . . . . .
C6 C 0.295(2) 0.6479(8) 0.5737(9) 0.026(2) Uani 1 1 d . . . . .
C7 C 0.393(2) 0.7292(7) 0.5335(10) 0.024(2) Uani 1 1 d . . . . .
C8 C 0.6450(18) 0.5655(6) 0.4040(9) 0.030(2) Uani 1 1 d . . . . .
H8A H 0.793998 0.569350 0.460395 0.035 Uiso 1 1 calc R U . . .
H8B H 0.669033 0.515051 0.345945 0.035 Uiso 1 1 calc R U . . .
C9 C 0.6321(16) 0.6490(6) 0.3200(8) 0.0249(17) Uani 1 1 d . . . . .
H9 H 0.476204 0.647762 0.266721 0.030 Uiso 1 1 calc R U . . .
C10 C 0.862(2) 0.6563(9) 0.2289(10) 0.036(3) Uani 1 1 d . . . . .
H10A H 0.848426 0.709488 0.177295 0.053 Uiso 1 1 calc R U . . .
H10B H 1.014931 0.658285 0.280730 0.053 Uiso 1 1 calc R U . . .
H10C H 0.866907 0.605850 0.171305 0.053 Uiso 1 1 calc R U . . .
S1 S -0.6381(6) 0.80862(18) 1.0672(3) 0.0330(7) Uani 1 1 d . . . . .
S2 S -0.3901(6) 1.01280(19) 0.9761(3) 0.0352(7) Uani 1 1 d . . . . .
S3 S -0.2866(6) 0.73366(17) 0.8792(3) 0.0284(6) Uani 1 1 d . . . . .
S4 S -0.0816(6) 0.91314(17) 0.7899(2) 0.0298(6) Uani 1 1 d . . . . .
S5 S 0.0678(6) 0.64390(17) 0.6926(2) 0.0303(6) Uani 1 1 d . . . . .
S6 S 0.2727(6) 0.82323(17) 0.6062(2) 0.0280(6) Uani 1 1 d . . . . .
S7 S 0.3720(6) 0.54426(18) 0.5060(3) 0.0323(6) Uani 1 1 d . . . . .
S8 S 0.6335(6) 0.74825(17) 0.4213(3) 0.0306(6) Uani 1 1 d . . . . .
NI1 Ni -0.0072(4) 0.77859(19) 0.74157(18) 0.0248(3) 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
C1 C2 1.507(15) . ?
C2 C3 1.498(14) . ?
C2 S1 1.835(9) . ?
C3 S2 1.787(10) . ?
C4 C5 1.382(18) . ?
C4 S3 1.706(12) . ?
C4 S1 1.737(12) . ?
C5 S4 1.714(12) . ?
C5 S2 1.754(12) . ?
C6 C7 1.392(17) . ?
C6 S5 1.701(12) . ?
C6 S7 1.754(12) . ?
C7 S6 1.720(11) . ?
C7 S8 1.724(12) . ?
C8 C9 1.522(12) . ?
C8 S7 1.799(10) . ?
C9 C10 1.526(14) . ?
C9 S8 1.816(9) . ?
S3 NI1 2.138(4) . ?
S4 NI1 2.125(4) . ?
S5 NI1 2.129(4) . ?
S6 NI1 2.124(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 C2 C1 113.7(8) . . ?
C3 C2 S1 112.0(7) . . ?
C1 C2 S1 106.0(7) . . ?
C2 C3 S2 115.4(6) . . ?
C5 C4 S3 119.0(9) . . ?
C5 C4 S1 127.0(9) . . ?
S3 C4 S1 114.0(7) . . ?
C4 C5 S4 119.4(9) . . ?
C4 C5 S2 126.5(9) . . ?
S4 C5 S2 114.1(7) . . ?
C7 C6 S5 120.0(9) . . ?
C7 C6 S7 125.9(9) . . ?
S5 C6 S7 114.1(7) . . ?
C6 C7 S6 117.7(9) . . ?
C6 C7 S8 127.7(9) . . ?
S6 C7 S8 114.6(6) . . ?
C9 C8 S7 115.7(6) . . ?
C8 C9 C10 111.4(8) . . ?
C8 C9 S8 111.5(6) . . ?
C10 C9 S8 106.3(7) . . ?
C4 S1 C2 106.2(6) . . ?
C5 S2 C3 101.4(5) . . ?
C4 S3 NI1 105.1(4) . . ?
C5 S4 NI1 104.9(4) . . ?
C6 S5 NI1 105.2(4) . . ?
C7 S6 NI1 105.8(4) . . ?
C6 S7 C8 104.5(5) . . ?
C7 S8 C9 103.5(5) . . ?
S6 NI1 S4 88.52(15) . . ?
S6 NI1 S5 91.32(14) . . ?
S4 NI1 S5 179.82(19) . . ?
S6 NI1 S3 179.50(15) . . ?
S4 NI1 S3 91.46(14) . . ?
S5 NI1 S3 88.71(15) . . ?

_refine_diff_density_max         0.489
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.102

