# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_04
_database_code_depnum_ccdc_archive 'CCDC 1982923'
loop_
_audit_author_name
_audit_author_address
Duan
;Nanjingxiaozhuang university
China
;
_audit_update_record             
;
2020-02-10 deposited with the CCDC.	2022-11-01 downloaded from the CCDC.
;
_audit_creation_date             2019-03-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C8 N4 Ni S4, C8 H15 N2'
_chemical_formula_sum            'C16 H15 N6 Ni S4'
_chemical_formula_weight         478.29
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   10.5716(7)
_cell_length_b                   7.2583(4)
_cell_length_c                   26.5198(14)
_cell_angle_alpha                90
_cell_angle_beta                 93.924(6)
_cell_angle_gamma                90
_cell_volume                     2030.1(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3459
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      28.8460
_cell_measurement_theta_min      2.9180
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.381
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85163
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            9365
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.386
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -18.00  11.00   1.00    2.50    --  -11.59 -99.00   0.00   29
  2  ω    -59.00  13.00   1.00    2.50    --   11.74 -57.00   0.00   72
  3  ω    -21.00  88.00   1.00    2.50    --   11.74  77.00 120.00  109
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0549982000
_diffrn_orient_matrix_UB_12      -0.0217415000
_diffrn_orient_matrix_UB_13      -0.0127378000
_diffrn_orient_matrix_UB_21      -0.0384023000
_diffrn_orient_matrix_UB_22      -0.0177568000
_diffrn_orient_matrix_UB_23      -0.0224405000
_diffrn_orient_matrix_UB_31      0.0054391000
_diffrn_orient_matrix_UB_32      0.0936026000
_diffrn_orient_matrix_UB_33      -0.0072012000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3107
_reflns_number_total             3579
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         3579
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0309
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0187P)²+1.2592P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0600
_refine_ls_wR_factor_ref         0.0644
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C12(H12A,H12B), C14(H14A,H14B)
2.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C15(H15A,H15B,H15C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.90332(3) 0.70956(4) 0.49738(2) 0.01037(10) Uani 1 1 d . . . . .
S2 S 1.09785(6) 0.79471(8) 0.50721(2) 0.01227(15) Uani 1 1 d . . . . .
S1 S 0.87084(6) 0.76546(8) 0.57482(2) 0.01281(15) Uani 1 1 d . . . . .
S4 S 0.93487(6) 0.65517(8) 0.41974(2) 0.01285(15) Uani 1 1 d . . . . .
S3 S 0.71067(6) 0.61425(8) 0.48860(2) 0.01336(15) Uani 1 1 d . . . . .
N6 N 0.22102(19) 0.7452(3) 0.34018(7) 0.0126(5) Uani 1 1 d . . . . .
N5 N 0.33725(19) 0.8567(3) 0.40297(7) 0.0122(5) Uani 1 1 d . . . . .
N2 N 1.3346(2) 0.9825(3) 0.60263(8) 0.0231(5) Uani 1 1 d . . . . .
N1 N 1.0248(2) 0.9644(3) 0.69187(8) 0.0236(5) Uani 1 1 d . . . . .
N3 N 0.4750(2) 0.4155(3) 0.39518(9) 0.0249(6) Uani 1 1 d . . . . .
C4 C 1.0219(2) 0.9122(3) 0.65096(10) 0.0139(6) Uani 1 1 d . . . . .
N4 N 0.7830(2) 0.4544(3) 0.30320(8) 0.0273(6) Uani 1 1 d . . . . .
C1 C 1.0140(2) 0.8503(3) 0.59924(9) 0.0116(5) Uani 1 1 d . . . . .
C3 C 1.2367(3) 0.9290(3) 0.58847(9) 0.0142(6) Uani 1 1 d . . . . .
C2 C 1.1149(2) 0.8600(3) 0.56975(9) 0.0120(5) Uani 1 1 d . . . . .
C6 C 0.7927(2) 0.5629(3) 0.39609(9) 0.0132(6) Uani 1 1 d . . . . .
C9 C 0.2608(2) 0.7194(3) 0.38833(9) 0.0135(6) Uani 1 1 d . . . . .
H9 H 0.238626 0.621159 0.408418 0.016 Uiso 1 1 calc R . . . .
C5 C 0.6937(2) 0.5480(3) 0.42598(9) 0.0126(5) Uani 1 1 d . . . . .
C7 C 0.5729(3) 0.4743(3) 0.40816(9) 0.0165(6) Uani 1 1 d . . . . .
C10 C 0.3477(2) 0.9753(3) 0.36280(9) 0.0152(6) Uani 1 1 d . . . . .
H10 H 0.395542 1.082769 0.362711 0.018 Uiso 1 1 calc R . . . .
C8 C 0.7851(2) 0.5032(3) 0.34431(10) 0.0172(6) Uani 1 1 d . . . . .
C16 C 0.3994(2) 0.8808(4) 0.45371(9) 0.0166(6) Uani 1 1 d . . . . .
H16A H 0.362470 0.983989 0.469926 0.025 Uiso 1 1 calc GR . . . .
H16B H 0.488302 0.902665 0.451117 0.025 Uiso 1 1 calc GR . . . .
H16C H 0.388177 0.771481 0.473280 0.025 Uiso 1 1 calc GR . . . .
C11 C 0.2750(2) 0.9050(3) 0.32373(9) 0.0148(6) Uani 1 1 d . . . . .
H11 H 0.263333 0.955330 0.291492 0.018 Uiso 1 1 calc R . . . .
C13 C 0.2216(2) 0.4488(3) 0.29417(9) 0.0155(6) Uani 1 1 d . . . . .
H13A H 0.252849 0.385313 0.324708 0.019 Uiso 1 1 calc R . . . .
H13B H 0.167478 0.364023 0.274374 0.019 Uiso 1 1 calc R . . . .
C12 C 0.1429(2) 0.6141(3) 0.30866(9) 0.0169(6) Uani 1 1 d . . . . .
H12A H 0.108743 0.675960 0.278288 0.020 Uiso 1 1 calc R . . . .
H12B H 0.072349 0.572334 0.327208 0.020 Uiso 1 1 calc R . . . .
C14 C 0.3334(3) 0.5008(3) 0.26405(10) 0.0209(6) Uani 1 1 d . . . . .
H14A H 0.302075 0.561032 0.233015 0.025 Uiso 1 1 calc R . . . .
H14B H 0.386337 0.588263 0.283425 0.025 Uiso 1 1 calc R . . . .
C15 C 0.4133(3) 0.3361(4) 0.25108(12) 0.0325(8) Uani 1 1 d . . . . .
H15A H 0.481544 0.376171 0.231650 0.049 Uiso 1 1 calc GR . . . .
H15B H 0.361592 0.249205 0.231715 0.049 Uiso 1 1 calc GR . . . .
H15C H 0.447342 0.278573 0.281666 0.049 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S2 2.1461(7) . ?
Ni1 S1 2.1441(7) . ?
Ni1 S4 2.1448(7) . ?
Ni1 S3 2.1484(7) . ?
S2 C2 1.722(2) . ?
S1 C1 1.719(2) . ?
S4 C6 1.724(3) . ?
S3 C5 1.726(2) . ?
N6 C9 1.330(3) . ?
N6 C11 1.377(3) . ?
N6 C12 1.480(3) . ?
N5 C9 1.324(3) . ?
N5 C10 1.380(3) . ?
N5 C16 1.467(3) . ?
N2 C3 1.144(3) . ?
N1 C4 1.147(3) . ?
N3 C7 1.150(3) . ?
C4 C1 1.440(3) . ?
N4 C8 1.145(3) . ?
C1 C2 1.367(3) . ?
C3 C2 1.439(4) . ?
C6 C5 1.360(4) . ?
C6 C8 1.437(3) . ?
C9 H9 0.9300 . ?
C5 C7 1.434(4) . ?
C10 H10 0.9300 . ?
C10 C11 1.348(3) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C11 H11 0.9300 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C12 1.524(3) . ?
C13 C14 1.519(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.517(4) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 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
S2 Ni1 S3 177.84(3) . . ?
S1 Ni1 S2 92.52(3) . . ?
S1 Ni1 S4 179.59(3) . . ?
S1 Ni1 S3 87.25(3) . . ?
S4 Ni1 S2 87.65(3) . . ?
S4 Ni1 S3 92.59(3) . . ?
C2 S2 Ni1 103.43(9) . . ?
C1 S1 Ni1 103.54(9) . . ?
C6 S4 Ni1 103.41(9) . . ?
C5 S3 Ni1 103.27(9) . . ?
C9 N6 C11 108.2(2) . . ?
C9 N6 C12 125.4(2) . . ?
C11 N6 C12 126.1(2) . . ?
C9 N5 C10 108.8(2) . . ?
C9 N5 C16 125.8(2) . . ?
C10 N5 C16 125.4(2) . . ?
N1 C4 C1 177.9(3) . . ?
C4 C1 S1 117.60(19) . . ?
C2 C1 S1 120.28(19) . . ?
C2 C1 C4 122.1(2) . . ?
N2 C3 C2 178.8(3) . . ?
C1 C2 S2 120.17(19) . . ?
C1 C2 C3 122.4(2) . . ?
C3 C2 S2 117.39(19) . . ?
C5 C6 S4 120.37(19) . . ?
C5 C6 C8 122.5(2) . . ?
C8 C6 S4 117.09(19) . . ?
N6 C9 H9 125.6 . . ?
N5 C9 N6 108.8(2) . . ?
N5 C9 H9 125.6 . . ?
C6 C5 S3 120.32(19) . . ?
C6 C5 C7 122.8(2) . . ?
C7 C5 S3 116.91(19) . . ?
N3 C7 C5 178.1(3) . . ?
N5 C10 H10 126.7 . . ?
C11 C10 N5 106.6(2) . . ?
C11 C10 H10 126.7 . . ?
N4 C8 C6 177.8(3) . . ?
N5 C16 H16A 109.5 . . ?
N5 C16 H16B 109.5 . . ?
N5 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N6 C11 H11 126.2 . . ?
C10 C11 N6 107.6(2) . . ?
C10 C11 H11 126.2 . . ?
H13A C13 H13B 107.7 . . ?
C12 C13 H13A 108.9 . . ?
C12 C13 H13B 108.9 . . ?
C14 C13 H13A 108.9 . . ?
C14 C13 H13B 108.9 . . ?
C14 C13 C12 113.3(2) . . ?
N6 C12 C13 110.8(2) . . ?
N6 C12 H12A 109.5 . . ?
N6 C12 H12B 109.5 . . ?
C13 C12 H12A 109.5 . . ?
C13 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
C13 C14 H14A 109.0 . . ?
C13 C14 H14B 109.0 . . ?
H14A C14 H14B 107.8 . . ?
C15 C14 C13 112.9(2) . . ?
C15 C14 H14A 109.0 . . ?
C15 C14 H14B 109.0 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.309
_oxdiff_exptl_absorpt_empirical_full_min 0.799
####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 2209474'
loop_
_audit_author_name
_audit_author_address
'Xiu-Ni Hua'
;Nanjing Xiaozhuang University
China
;
_audit_update_record             
;
2022-09-24 deposited with the CCDC.	2022-11-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 N4 Ni S4, C8 H15 N2'
_chemical_formula_sum            'C16 H15 N6 Ni S4'
_chemical_formula_weight         478.29

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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                   10.7039(5)
_cell_length_b                   7.4586(4)
_cell_length_c                   26.8087(14)
_cell_angle_alpha                90
_cell_angle_beta                 93.095(2)
_cell_angle_gamma                90
_cell_volume                     2137.18(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    353(2)
_cell_measurement_reflns_used    2350
_cell_measurement_theta_min      2.918
_cell_measurement_theta_max      28.846

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_F_000             980
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    1.312
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.854
_exptl_absorpt_correction_T_max  0.900
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      353(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  AtlasS2
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21768
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.502
_diffrn_reflns_theta_max         27.677
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             4923
_reflns_number_gt                3076
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0466P)²+0.4575P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0030(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4923
_refine_ls_number_parameters     247
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0411
_refine_ls_wR_factor_ref         0.1010
_refine_ls_wR_factor_gt          0.0867
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.001
_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
Ni1 Ni 0.09974(3) 0.20557(4) 0.00387(2) 0.04853(14) Uani 1 1 d . . . . .
S1 S -0.09139(6) 0.29087(10) -0.00509(3) 0.0566(2) Uani 1 1 d . . . . .
S2 S 0.13208(6) 0.25923(11) -0.07283(3) 0.0584(2) Uani 1 1 d . . . . .
S3 S 0.06879(7) 0.15791(10) 0.08107(3) 0.0592(2) Uani 1 1 d . . . . .
S4 S 0.28910(7) 0.11087(11) 0.01184(3) 0.0616(2) Uani 1 1 d . . . . .
N1 N -0.3240(3) 0.4695(4) -0.09757(12) 0.0971(10) Uani 1 1 d . . . . .
N2 N -0.0182(3) 0.4419(5) -0.18820(12) 0.1086(11) Uani 1 1 d . . . . .
N3 N 0.2213(4) -0.0258(5) 0.19580(12) 0.1199(13) Uani 1 1 d . . . . .
N4 N 0.5190(3) -0.0804(5) 0.10296(13) 0.1110(11) Uani 1 1 d . . . . .
N5 N 0.6597(2) 0.3615(3) 0.09950(8) 0.0577(6) Uani 1 1 d . . . . .
N6 N 0.7700(2) 0.2543(4) 0.16165(9) 0.0630(6) Uani 1 1 d . . . . .
C1 C -0.2280(3) 0.4184(4) -0.08434(12) 0.0646(8) Uani 1 1 d . . . . .
C2 C -0.1082(2) 0.3528(3) -0.06659(10) 0.0517(7) Uani 1 1 d . . . . .
C3 C -0.0090(2) 0.3411(3) -0.09637(10) 0.0529(7) Uani 1 1 d . . . . .
C4 C -0.0161(3) 0.3959(5) -0.14766(12) 0.0694(8) Uani 1 1 d . . . . .
C5 C 0.2170(3) 0.0159(5) 0.15526(13) 0.0772(9) Uani 1 1 d . . . . .
C6 C 0.2082(3) 0.0694(4) 0.10392(10) 0.0591(7) Uani 1 1 d . . . . .
C7 C 0.3056(3) 0.0495(4) 0.07363(11) 0.0580(7) Uani 1 1 d . . . . .
C8 C 0.4236(3) -0.0239(5) 0.09067(12) 0.0743(9) Uani 1 1 d . . . . .
C9 C 0.6010(3) 0.3840(5) 0.04916(11) 0.0788(9) Uani 1 1 d . . . . .
H9A H 0.6140 0.2778 0.0299 0.118 Uiso 1 1 calc R U . . .
H9B H 0.6377 0.4849 0.0332 0.118 Uiso 1 1 calc R U . . .
H9C H 0.5129 0.4039 0.0514 0.118 Uiso 1 1 calc R U . . .
C10 C 0.6479(3) 0.4767(4) 0.13819(12) 0.0741(9) Uani 1 1 d . . . . .
H10 H 0.6008 0.5815 0.1380 0.089 Uiso 1 1 calc R U . . .
C11 C 0.7178(3) 0.4092(5) 0.17685(12) 0.0762(9) Uani 1 1 d . . . . .
H11 H 0.7285 0.4598 0.2085 0.091 Uiso 1 1 calc R U . . .
C12 C 0.7341(3) 0.2294(4) 0.11450(11) 0.0604(7) Uani 1 1 d . . . . .
H12 H 0.7576 0.1336 0.0948 0.072 Uiso 1 1 calc R U . . .
C13 C 0.8486(3) 0.1308(5) 0.19288(12) 0.0853(10) Uani 1 1 d . . . . .
H13A H 0.8790 0.1927 0.2230 0.102 Uiso 1 1 calc R U . . .
H13B H 0.9205 0.0951 0.1747 0.102 Uiso 1 1 calc R U . . .
C14 C 0.7770(4) -0.0341(5) 0.20707(14) 0.0973(12) Uani 1 1 d . . . . .
H14A H 0.7472 -0.0956 0.1768 0.117 Uiso 1 1 calc R U . . .
H14B H 0.8334 -0.1146 0.2257 0.117 Uiso 1 1 calc R U . . .
C15 C 0.6686(4) 0.0054(7) 0.2376(2) 0.1392(19) Uani 1 1 d . . . . .
H15A H 0.6988 0.0767 0.2660 0.167 Uiso 1 1 calc R U . . .
H15B H 0.6109 0.0799 0.2176 0.167 Uiso 1 1 calc R U . . .
C16 C 0.6010(6) -0.1373(10) 0.2557(3) 0.225(4) Uani 1 1 d . . . . .
H16A H 0.5578 -0.1982 0.2283 0.337 Uiso 1 1 calc R U . . .
H16B H 0.5413 -0.0931 0.2782 0.337 Uiso 1 1 calc R U . . .
H16C H 0.6571 -0.2193 0.2731 0.337 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
Ni1 S2 2.1412(8) . ?
Ni1 S3 2.1431(8) . ?
Ni1 S1 2.1436(7) . ?
Ni1 S4 2.1462(8) . ?
S1 C2 1.713(3) . ?
S2 C3 1.717(3) . ?
S3 C6 1.715(3) . ?
S4 C7 1.718(3) . ?
N1 C1 1.135(4) . ?
N2 C4 1.139(4) . ?
N3 C5 1.129(4) . ?
N4 C8 1.137(4) . ?
N5 C12 1.316(3) . ?
N5 C10 1.358(4) . ?
N5 C9 1.467(3) . ?
N6 C12 1.314(3) . ?
N6 C11 1.356(4) . ?
N6 C13 1.476(4) . ?
C1 C2 1.429(4) . ?
C2 C3 1.366(4) . ?
C3 C4 1.432(4) . ?
C5 C6 1.431(4) . ?
C6 C7 1.363(4) . ?
C7 C8 1.429(4) . ?
C10 C11 1.343(4) . ?
C13 C14 1.509(5) . ?
C14 C15 1.484(6) . ?
C15 C16 1.390(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
S2 Ni1 S3 178.70(3) . . ?
S2 Ni1 S1 92.28(3) . . ?
S3 Ni1 S1 87.77(3) . . ?
S2 Ni1 S4 87.50(3) . . ?
S3 Ni1 S4 92.50(3) . . ?
S1 Ni1 S4 177.95(3) . . ?
C2 S1 Ni1 103.79(9) . . ?
C3 S2 Ni1 103.60(10) . . ?
C6 S3 Ni1 103.41(10) . . ?
C7 S4 Ni1 103.35(10) . . ?
C12 N5 C10 108.7(2) . . ?
C12 N5 C9 126.1(3) . . ?
C10 N5 C9 125.2(3) . . ?
C12 N6 C11 107.8(3) . . ?
C12 N6 C13 125.8(3) . . ?
C11 N6 C13 126.3(3) . . ?
N1 C1 C2 178.7(4) . . ?
C3 C2 C1 122.6(3) . . ?
C3 C2 S1 120.0(2) . . ?
C1 C2 S1 117.3(2) . . ?
C2 C3 C4 122.7(3) . . ?
C2 C3 S2 120.3(2) . . ?
C4 C3 S2 117.0(2) . . ?
N2 C4 C3 177.9(3) . . ?
N3 C5 C6 178.6(4) . . ?
C7 C6 C5 122.0(3) . . ?
C7 C6 S3 120.5(2) . . ?
C5 C6 S3 117.5(2) . . ?
C6 C7 C8 122.8(3) . . ?
C6 C7 S4 120.2(2) . . ?
C8 C7 S4 117.0(2) . . ?
N4 C8 C7 177.9(4) . . ?
C11 C10 N5 106.3(3) . . ?
C10 C11 N6 108.0(3) . . ?
N6 C12 N5 109.2(3) . . ?
N6 C13 C14 111.7(3) . . ?
C15 C14 C13 113.6(4) . . ?
C16 C15 C14 118.5(5) . . ?

_refine_diff_density_max         0.415
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.055

