# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 2144097'
loop_
_audit_author_name
_audit_author_address
'Michael G. B. Drew'
;Department of Chemistry, University of Reading, Whiteknights, Reading, UK
United Kingdom
;
_audit_update_record             
;
2022-01-24 deposited with the CCDC.	2022-08-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H22 N4 Ni S6'
_chemical_formula_weight         617.52

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'

_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                   6.191(3)
_cell_length_b                   10.226(4)
_cell_length_c                   10.769(5)
_cell_angle_alpha                77.765(10)
_cell_angle_beta                 73.925(10)
_cell_angle_gamma                87.279(11)
_cell_volume                     640.2(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7039
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      27.50

_exptl_crystal_description       Needle
_exptl_crystal_colour            Brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_F_000             318
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    1.270
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7039
_diffrn_reflns_av_unetI/netI     0.0998
_diffrn_reflns_av_R_equivalents  0.0738
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.550
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             2889
_reflns_number_gt                1834
_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-2016/6 (Sheldrick, 2016)'
_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)+(0.1158P)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         2889
_refine_ls_number_parameters     161
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1299
_refine_ls_R_factor_gt           0.0827
_refine_ls_wR_factor_ref         0.2446
_refine_ls_wR_factor_gt          0.2205
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_restrained_S_all      1.162
_refine_ls_shift/su_max          0.002
_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 0.500000 0.500000 0.500000 0.0336(4) Uani 1 2 d S . P . .
S11 S 0.3342(3) 0.30675(16) 0.52762(14) 0.0354(4) Uani 1 1 d . . . . .
C12 C 0.2074(10) 0.3891(6) 0.4108(5) 0.0352(13) Uani 1 1 d . . . . .
S13 S 0.2972(3) 0.55178(16) 0.35946(14) 0.0369(4) Uani 1 1 d . . . . .
N14 N 0.0601(8) 0.3325(5) 0.3682(5) 0.0373(12) Uani 1 1 d . . . . .
C21 C -0.0447(10) 0.4131(6) 0.2695(6) 0.0384(14) Uani 1 1 d . . . . .
H21A H 0.003191 0.505782 0.251996 0.046 Uiso 1 1 calc R U . . .
H21B H -0.206793 0.409382 0.305386 0.046 Uiso 1 1 calc R U . . .
C22 C 0.0165(10) 0.3647(6) 0.1429(6) 0.0364(14) Uani 1 1 d . . . . .
C23 C 0.2453(10) 0.3620(6) 0.0614(7) 0.0411(15) Uani 1 1 d . . . . .
H23 H 0.362430 0.392879 0.086450 0.049 Uiso 1 1 calc R U . . .
C24 C 0.2852(16) 0.3193(9) -0.0401(9) 0.076(3) Uani 1 1 d . . . . .
H24 H 0.433499 0.314396 -0.089451 0.091 Uiso 1 1 calc R U . . .
C25 C 0.119(2) 0.2790(9) -0.0822(8) 0.077(3) Uani 1 1 d . . . . .
H25 H 0.158474 0.249451 -0.161384 0.092 Uiso 1 1 calc R U . . .
N26 N -0.0961(15) 0.2786(7) -0.0190(7) 0.072(2) Uani 1 1 d . . . . .
C27 C -0.1424(11) 0.3201(7) 0.0939(6) 0.0447(16) Uani 1 1 d . . . . .
H27 H -0.291934 0.318913 0.143187 0.054 Uiso 1 1 calc R U . . .
C31 C -0.0101(9) 0.1940(6) 0.4196(6) 0.0346(13) Uani 1 1 d . . . . .
H31A H -0.167007 0.185905 0.422553 0.042 Uiso 1 1 calc R U . . .
H31B H 0.001722 0.168210 0.509502 0.042 Uiso 1 1 calc R U . . .
C32 C 0.1247(10) 0.0985(6) 0.3401(6) 0.0354(13) Uani 1 1 d . . . . .
S33 S 0.3901(4) 0.0653(3) 0.3392(3) 0.0569(9) Uani 0.672(8) 1 d . . P A 1
C33 C 0.3901(4) 0.0653(3) 0.3392(3) 0.0569(9) Uani 0.328(8) 1 d . . P A 2
H33 H 0.484492 0.092931 0.382772 0.068 Uiso 0.328(8) 1 calc R U P A 2
C34 C 0.4254(13) -0.0326(8) 0.2352(8) 0.065(2) Uani 1 1 d . . . . .
H34 H 0.561835 -0.073436 0.205259 0.078 Uiso 1 1 calc R U . A 2
C35 C 0.2387(18) -0.0511(8) 0.1942(8) 0.073(3) Uani 1 1 d . . . . .
H35 H 0.238771 -0.107227 0.136603 0.088 Uiso 1 1 calc R U . A 1
C36 C 0.0336(9) 0.0272(5) 0.2501(5) 0.0806(19) Uani 0.672(8) 1 d . . P A 1
H36 H -0.107525 0.031487 0.234908 0.097 Uiso 0.672(8) 1 calc R U P A 1
S36 S 0.0336(9) 0.0272(5) 0.2501(5) 0.0806(19) Uani 0.328(8) 1 d . . P A 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
Ni1 S13 2.1900(15) 2_666 ?
Ni1 S13 2.1900(15) . ?
Ni1 S11 2.1959(18) . ?
Ni1 S11 2.1959(18) 2_666 ?
S11 C12 1.715(6) . ?
C12 N14 1.332(8) . ?
C12 S13 1.706(6) . ?
N14 C31 1.447(7) . ?
N14 C21 1.480(7) . ?
C21 C22 1.493(8) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C27 1.373(8) . ?
C22 C23 1.448(8) . ?
C23 C24 1.220(11) . ?
C23 H23 0.9300 . ?
C24 C25 1.347(13) . ?
C24 H24 0.9300 . ?
C25 N26 1.316(12) . ?
C25 H25 0.9300 . ?
N26 C27 1.325(8) . ?
C27 H27 0.9300 . ?
C31 C32 1.505(8) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 C36 1.559(7) . ?
C32 C33 1.659(6) . ?
C33 C34 1.619(8) . ?
C33 H33 0.9300 . ?
C34 C35 1.381(11) . ?
C34 H34 0.9300 . ?
C35 C36 1.517(11) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?

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
S13 Ni1 S13 180.0 2_666 . ?
S13 Ni1 S11 100.52(6) 2_666 . ?
S13 Ni1 S11 79.48(6) . . ?
S13 Ni1 S11 79.48(6) 2_666 2_666 ?
S13 Ni1 S11 100.52(6) . 2_666 ?
S11 Ni1 S11 180.0 . 2_666 ?
C12 S11 Ni1 85.0(2) . . ?
N14 C12 S13 125.8(4) . . ?
N14 C12 S11 124.1(5) . . ?
S13 C12 S11 110.1(3) . . ?
C12 S13 Ni1 85.4(2) . . ?
C12 N14 C31 122.0(5) . . ?
C12 N14 C21 120.0(5) . . ?
C31 N14 C21 118.0(5) . . ?
N14 C21 C22 112.1(5) . . ?
N14 C21 H21A 109.2 . . ?
C22 C21 H21A 109.2 . . ?
N14 C21 H21B 109.2 . . ?
C22 C21 H21B 109.2 . . ?
H21A C21 H21B 107.9 . . ?
C27 C22 C23 114.6(6) . . ?
C27 C22 C21 122.1(6) . . ?
C23 C22 C21 123.3(5) . . ?
C24 C23 C22 120.3(7) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C23 C24 C25 121.4(9) . . ?
C23 C24 H24 119.3 . . ?
C25 C24 H24 119.3 . . ?
N26 C25 C24 124.5(8) . . ?
N26 C25 H25 117.8 . . ?
C24 C25 H25 117.8 . . ?
C25 N26 C27 115.1(7) . . ?
N26 C27 C22 124.1(7) . . ?
N26 C27 H27 117.9 . . ?
C22 C27 H27 117.9 . . ?
N14 C31 C32 113.9(5) . . ?
N14 C31 H31A 108.8 . . ?
C32 C31 H31A 108.8 . . ?
N14 C31 H31B 108.8 . . ?
C32 C31 H31B 108.8 . . ?
H31A C31 H31B 107.7 . . ?
C31 C32 C36 123.9(5) . . ?
C31 C32 C33 121.2(4) . . ?
C34 C33 C32 94.3(4) . . ?
C34 C33 H33 132.9 . . ?
C32 C33 H33 132.9 . . ?
C35 C34 C33 115.3(6) . . ?
C35 C34 H34 122.4 . . ?
C33 C34 H34 122.4 . . ?
C34 C35 C36 114.9(7) . . ?
C34 C35 H35 122.6 . . ?
C36 C35 H35 122.6 . . ?
C35 C36 C32 100.7(5) . . ?
C35 C36 H36 129.6 . . ?
C32 C36 H36 129.6 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C21 H21A S13 0.97 2.52 3.071(6) 116.0 .
C24 H24 S13 0.93 2.99 3.705(9) 134.6 2_665
C31 H31B S36 0.97 2.88 3.758(7) 151.5 2_556

_refine_diff_density_max         0.985
_refine_diff_density_min         -1.026
_refine_diff_density_rms         0.143

