# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_cypi_nis
_database_code_depnum_ccdc_archive 'CCDC 939713'
_audit_update_record             
;
2013-05-16 deposited with the CCDC.	2020-08-05 downloaded from the CCDC.
;

_audit_creation_date             2012-02-24T08:44:55-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C7 H13 Ni1.5 S4'
_chemical_formula_sum            'C7 H13 Ni1.5 S4'
_chemical_formula_weight         313.48
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_Int_Tables_number      60
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y, z-1/2'

_cell_length_a                   16.0517(3)
_cell_length_b                   12.6900(2)
_cell_length_c                   11.0788(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2256.71(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    17268
_cell_measurement_theta_min      3.52
_cell_measurement_theta_max      28.98
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_crystal_density_diffrn    1.845
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1288
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    3.216
_exptl_absorpt_correction_type   none

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'Omega + Phi scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_number            17268
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.52
_diffrn_reflns_theta_max         28.98
_diffrn_reflns_theta_full        28.98
_diffrn_measured_fraction_theta_full 0.96
_diffrn_measured_fraction_theta_max 0.96
_reflns_number_total             2877
_reflns_number_gt                2432
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)²+1.9103P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         2877
_refine_ls_number_parameters     115
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0262
_refine_ls_wR_factor_ref         0.0531
_refine_ls_wR_factor_gt          0.0483
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.29
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.062

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 1.07630(13) 0.27231(17) -0.02385(19) 0.0409(5) Uani 1 1 d . . .
C2 C 1.11005(16) 0.2432(2) -0.1498(2) 0.0577(6) Uani 1 1 d . . .
H2A H 1.1105 0.3048 -0.2002 0.087 Uiso 1 1 calc R . .
H2B H 1.0749 0.1904 -0.1855 0.087 Uiso 1 1 calc R . .
H2C H 1.1657 0.2162 -0.1423 0.087 Uiso 1 1 calc R . .
C3 C 0.98614(14) 0.3110(2) -0.0420(2) 0.0476(5) Uani 1 1 d . . .
H3A H 0.9536 0.251 -0.0688 0.057 Uiso 1 1 calc R . .
H3B H 0.9869 0.3611 -0.1081 0.057 Uiso 1 1 calc R . .
C4 C 1.13214(13) 0.36167(18) 0.0224(2) 0.0464(5) Uani 1 1 d . . .
H4A H 1.1206 0.4235 -0.0263 0.056 Uiso 1 1 calc R . .
H4B H 1.1895 0.3417 0.0067 0.056 Uiso 1 1 calc R . .
C5 C 1.07711(12) 0.17397(17) 0.05763(18) 0.0381(4) Uani 1 1 d . . .
H5A H 1.0713 0.1116 0.0077 0.046 Uiso 1 1 calc R . .
H5B H 1.0296 0.1767 0.1116 0.046 Uiso 1 1 calc R . .
C6 C 1.16098(15) 0.03037(17) 0.2093(2) 0.0454(5) Uani 1 1 d . . .
H6A H 1.1026 0.0109 0.2138 0.054 Uiso 1 1 calc R . .
H6B H 1.1898 -0.0206 0.1591 0.054 Uiso 1 1 calc R . .
C7 C 1.19889(14) 0.03371(18) 0.3336(2) 0.0459(5) Uani 1 1 d . . .
H7A H 1.2577 0.0506 0.3277 0.055 Uiso 1 1 calc R . .
H7B H 1.1936 -0.0348 0.3717 0.055 Uiso 1 1 calc R . .
S1 S 0.92931(3) 0.37226(4) 0.08193(5) 0.04426(14) Uani 1 1 d . . .
S2 S 1.12534(3) 0.40062(4) 0.17888(6) 0.04483(14) Uani 1 1 d . . .
S3 S 1.17227(3) 0.16258(4) 0.14705(5) 0.03774(12) Uani 1 1 d . . .
S4 S 1.14602(4) 0.13299(5) 0.42452(5) 0.04604(14) Uani 1 1 d . . .
Ni1 Ni 1 0.39038(3) 0.25 0.03950(10) Uani 1 2 d S . .
Ni2 Ni 1.134647(15) 0.26188(2) 0.29720(2) 0.03586(8) Uani 1 1 d . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 C4 1.534(3) . ?
C1 C5 1.540(3) . ?
C1 C3 1.541(3) . ?
C1 C2 1.542(3) . ?
C2 H2A 0.96 . ?
C2 H2B 0.96 . ?
C2 H2C 0.96 . ?
C3 S1 1.823(2) . ?
C3 H3A 0.97 . ?
C3 H3B 0.97 . ?
C4 S2 1.806(2) . ?
C4 H4A 0.97 . ?
C4 H4B 0.97 . ?
C5 S3 1.8264(19) . ?
C5 H5A 0.97 . ?
C5 H5B 0.97 . ?
C6 C7 1.506(3) . ?
C6 S3 1.823(2) . ?
C6 H6A 0.97 . ?
C6 H6B 0.97 . ?
C7 S4 1.823(2) . ?
C7 H7A 0.97 . ?
C7 H7B 0.97 . ?
S1 Ni1 2.1926(6) . ?
S1 Ni2 2.1930(6) 4_755 ?
S2 Ni1 2.1647(5) . ?
S2 Ni2 2.2000(6) . ?
S3 Ni2 2.1725(6) . ?
S4 Ni2 2.1675(6) . ?
Ni1 S2 2.1647(5) 4_755 ?
Ni1 S1 2.1926(6) 4_755 ?
Ni1 Ni2 2.7574(3) 4_755 ?
Ni1 Ni2 2.7574(3) . ?
Ni2 S1 2.1930(6) 4_755 ?

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 C1 C5 113.47(17) . . ?
C4 C1 C3 110.90(19) . . ?
C5 C1 C3 110.04(17) . . ?
C4 C1 C2 105.92(18) . . ?
C5 C1 C2 109.47(19) . . ?
C3 C1 C2 106.73(18) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 S1 120.48(16) . . ?
C1 C3 H3A 107.2 . . ?
S1 C3 H3A 107.2 . . ?
C1 C3 H3B 107.2 . . ?
S1 C3 H3B 107.2 . . ?
H3A C3 H3B 106.8 . . ?
C1 C4 S2 119.20(15) . . ?
C1 C4 H4A 107.5 . . ?
S2 C4 H4A 107.5 . . ?
C1 C4 H4B 107.5 . . ?
S2 C4 H4B 107.5 . . ?
H4A C4 H4B 107 . . ?
C1 C5 S3 112.90(14) . . ?
C1 C5 H5A 109 . . ?
S3 C5 H5A 109 . . ?
C1 C5 H5B 109 . . ?
S3 C5 H5B 109 . . ?
H5A C5 H5B 107.8 . . ?
C7 C6 S3 106.24(16) . . ?
C7 C6 H6A 110.5 . . ?
S3 C6 H6A 110.5 . . ?
C7 C6 H6B 110.5 . . ?
S3 C6 H6B 110.5 . . ?
H6A C6 H6B 108.7 . . ?
C6 C7 S4 109.68(15) . . ?
C6 C7 H7A 109.7 . . ?
S4 C7 H7A 109.7 . . ?
C6 C7 H7B 109.7 . . ?
S4 C7 H7B 109.7 . . ?
H7A C7 H7B 108.2 . . ?
C3 S1 Ni1 115.19(7) . . ?
C3 S1 Ni2 114.96(8) . 4_755 ?
Ni1 S1 Ni2 77.92(2) . 4_755 ?
C4 S2 Ni1 112.90(7) . . ?
C4 S2 Ni2 110.42(8) . . ?
Ni1 S2 Ni2 78.36(2) . . ?
C6 S3 C5 101.24(10) . . ?
C6 S3 Ni2 102.51(8) . . ?
C5 S3 Ni2 97.87(7) . . ?
C7 S4 Ni2 101.60(8) . . ?
S2 Ni1 S2 173.12(4) 4_755 . ?
S2 Ni1 S1 100.26(2) 4_755 4_755 ?
S2 Ni1 S1 80.47(2) . 4_755 ?
S2 Ni1 S1 80.47(2) 4_755 . ?
S2 Ni1 S1 100.26(2) . . ?
S1 Ni1 S1 167.96(3) 4_755 . ?
S2 Ni1 Ni2 51.392(17) 4_755 4_755 ?
S2 Ni1 Ni2 134.03(2) . 4_755 ?
S1 Ni1 Ni2 120.309(19) 4_755 4_755 ?
S1 Ni1 Ni2 51.048(16) . 4_755 ?
S2 Ni1 Ni2 134.03(2) 4_755 . ?
S2 Ni1 Ni2 51.392(17) . . ?
S1 Ni1 Ni2 51.048(16) 4_755 . ?
S1 Ni1 Ni2 120.309(19) . . ?
Ni2 Ni1 Ni2 107.497(16) 4_755 . ?
S4 Ni2 S3 92.13(2) . . ?
S4 Ni2 S1 97.13(2) . 4_755 ?
S3 Ni2 S1 165.51(2) . 4_755 ?
S4 Ni2 S2 175.80(3) . . ?
S3 Ni2 S2 91.54(2) . . ?
S1 Ni2 S2 79.69(2) 4_755 . ?
S4 Ni2 Ni1 129.470(19) . . ?
S3 Ni2 Ni1 114.563(16) . . ?
S1 Ni2 Ni1 51.036(16) 4_755 . ?
S2 Ni2 Ni1 50.252(16) . . ?

# END of CIF
