# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_Compound_4
_database_code_depnum_ccdc_archive 'CCDC 1513676'
_audit_update_record             
;
2017-01-30 deposited with the CCDC.
2017-02-17 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         ?
_chemical_formula_sum            'C12 H16 N2 Ni2 O4 S4'
_chemical_formula_weight         497.93

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'
O O 0.0106 0.0060 '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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   12.670(19)
_cell_length_b                   9.658(14)
_cell_length_c                   16.44(2)
_cell_angle_alpha                90
_cell_angle_beta                 112.87(6)
_cell_angle_gamma                90
_cell_volume                     1854(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2149
_cell_measurement_theta_min      2.679
_cell_measurement_theta_max      27.465

_exptl_crystal_description       blade
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_F_000             1016
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    2.500
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1968
_exptl_absorpt_correction_T_max  0.2617
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0901 before and 0.0468 after correction.
The Ratio of minimum to maximum transmission is 0.7520.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_reflns_number            6339
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.344
_diffrn_reflns_theta_max         27.689
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2151
_reflns_number_gt                1812
_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       'APEX2 v2013.6-2 (Bruker, 2013)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
Reflection -14 4 5 was affected by the beam stop and was omitted 
from the refinement. Twinning by pseudo-merohedry by a 180 degree 
rotation around the [1 0 2] direct lattice direction was handled using 
the twin matrix -1 0 0 0 -1 0 1 0 1 resulting in a BASF value of 
0.413(3). Both thioacetate anions were refined using a two part 
disorder model with a common occupancy ratio. The four disordered 
moieties were restrained to have similar geometries (SAME restraint), 
and Uij components of ADPs were restrained to be similar for atoms 
closer to each other than 1.7 Angstrom (SIMU restraint). 
The shared occupancy ratio refined to 0.815(7) to 0.185(5). 
The ADPs of C5 and C6 were constrained to be identical (EADP). 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0589P)²+21.5929P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2151
_refine_ls_number_parameters     182
_refine_ls_number_restraints     228
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0575
_refine_ls_wR_factor_ref         0.1464
_refine_ls_wR_factor_gt          0.1383
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.017
_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 0.5000 0.50565(14) 0.7500 0.0206(3) Uani 1 2 d S T P . .
Ni2 Ni 0.5000 0.76868(14) 0.7500 0.0181(3) Uani 1 2 d S T P A .
S1 S 0.5981(3) 0.5153(3) 0.6627(2) 0.0295(7) Uani 0.815(7) 1 d D U P A 1
O1 O 0.5412(7) 0.7739(6) 0.6402(5) 0.0175(14) Uani 0.815(7) 1 d D U P A 1
C1 C 0.585(3) 0.6783(10) 0.6194(16) 0.0258(17) Uani 0.815(7) 1 d D U P A 1
C2 C 0.6277(10) 0.7024(12) 0.5463(8) 0.030(3) Uani 0.815(7) 1 d D U P A 1
H2A H 0.6893 0.6367 0.5526 0.045 Uiso 0.815(7) 1 calc R U P A 1
H2B H 0.6569 0.7972 0.5502 0.045 Uiso 0.815(7) 1 calc R U P A 1
H2C H 0.5646 0.6889 0.4888 0.045 Uiso 0.815(7) 1 calc R U P A 1
S2 S 0.3395(3) 0.5113(3) 0.6322(2) 0.0300(8) Uani 0.815(7) 1 d D U P A 1
O2 O 0.3288(6) 0.7686(6) 0.6731(5) 0.0155(13) Uani 0.815(7) 1 d D U P A 1
C3 C 0.2829(12) 0.6724(10) 0.6277(13) 0.0292(18) Uani 0.815(7) 1 d D U P A 1
C4 C 0.1630(10) 0.6913(12) 0.5619(6) 0.032(3) Uani 0.815(7) 1 d D U P A 1
H4A H 0.1622 0.7600 0.5178 0.048 Uiso 0.815(7) 1 calc R U P A 1
H4B H 0.1144 0.7233 0.5921 0.048 Uiso 0.815(7) 1 calc R U P A 1
H4C H 0.1338 0.6028 0.5326 0.048 Uiso 0.815(7) 1 calc R U P A 1
S1' S 0.5388(15) 0.5145(14) 0.6296(11) 0.034(3) Uani 0.185(7) 1 d D U P A 2
O1' O 0.589(3) 0.771(3) 0.661(2) 0.017(4) Uani 0.185(7) 1 d D U P A 2
C1' C 0.586(11) 0.674(3) 0.616(7) 0.026(3) Uani 0.185(7) 1 d D U P A 2
C2' C 0.653(6) 0.678(5) 0.557(4) 0.038(8) Uani 0.185(7) 1 d D U P A 2
H2A' H 0.6408 0.5914 0.5237 0.057 Uiso 0.185(7) 1 calc R U P A 2
H2B' H 0.6258 0.7560 0.5156 0.057 Uiso 0.185(7) 1 calc R U P A 2
H2C' H 0.7342 0.6898 0.5932 0.057 Uiso 0.185(7) 1 calc R U P A 2
S2' S 0.3180(11) 0.5102(13) 0.6698(11) 0.030(3) Uani 0.185(7) 1 d D U P A 2
O2' O 0.340(3) 0.765(3) 0.639(2) 0.020(4) Uani 0.185(7) 1 d D U P A 2
C3' C 0.276(4) 0.670(3) 0.625(5) 0.026(3) Uani 0.185(7) 1 d D U P A 2
C4' C 0.169(4) 0.669(5) 0.541(3) 0.035(8) Uani 0.185(7) 1 d D U P A 2
H4A' H 0.1254 0.5847 0.5385 0.052 Uiso 0.185(7) 1 calc R U P A 2
H4B' H 0.1225 0.7504 0.5393 0.052 Uiso 0.185(7) 1 calc R U P A 2
H4C' H 0.1915 0.6713 0.4898 0.052 Uiso 0.185(7) 1 calc R U P A 2
N1 N 0.5000 0.2737(9) 0.7500 0.0181(18) Uani 1 2 d S T P A .
N2 N 0.5000 -0.0112(9) 0.7500 0.024(2) Uani 1 2 d S T P . .
C5 C 0.4083(7) 0.2017(6) 0.7475(7) 0.0272(9) Uani 1 1 d . . . . .
H5 H 0.3420 0.2497 0.7457 0.033 Uiso 1 1 calc R U . A .
C6 C 0.4089(7) 0.0589(6) 0.7475(7) 0.0272(9) Uani 1 1 d . . . . .
H6 H 0.3430 0.0100 0.7457 0.033 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' 2.167(14) . ?
Ni1 S2' 2.167(14) 2_656 ?
Ni1 S2 2.197(4) 2_656 ?
Ni1 S2 2.197(4) . ?
Ni1 S1' 2.219(15) . ?
Ni1 S1' 2.219(15) 2_656 ?
Ni1 S1 2.236(4) . ?
Ni1 S1 2.236(4) 2_656 ?
Ni1 N1 2.240(10) . ?
Ni1 Ni2 2.540(4) . ?
Ni2 O2 2.043(7) 2_656 ?
Ni2 O2 2.043(7) . ?
Ni2 O1 2.066(8) 2_656 ?
Ni2 O1 2.066(8) . ?
Ni2 N2 2.126(10) 1_565 ?
Ni2 O2' 2.13(3) . ?
Ni2 O2' 2.13(3) 2_656 ?
Ni2 O1' 2.16(3) . ?
Ni2 O1' 2.16(3) 2_656 ?
S1 C1 1.709(14) . ?
O1 C1 1.191(14) . ?
C1 C2 1.519(11) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
S2 C3 1.703(13) . ?
O2 C3 1.191(13) . ?
C3 C4 1.495(11) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
S1' C1' 1.704(17) . ?
O1' C1' 1.19(2) . ?
C1' C2' 1.508(19) . ?
C2' H2A' 0.9800 . ?
C2' H2B' 0.9800 . ?
C2' H2C' 0.9800 . ?
S2' C3' 1.708(17) . ?
O2' C3' 1.19(2) . ?
C3' C4' 1.507(19) . ?
C4' H4A' 0.9800 . ?
C4' H4B' 0.9800 . ?
C4' H4C' 0.9800 . ?
N1 C5 1.341(9) 2_656 ?
N1 C5 1.341(9) . ?
N2 C6 1.324(8) . ?
N2 C6 1.324(8) 2_656 ?
N2 Ni2 2.126(10) 1_545 ?
C5 C6 1.379(8) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S2' Ni1 S2' 177.7(7) . 2_656 ?
S2 Ni1 S2 177.13(15) 2_656 . ?
S2' Ni1 S1' 90.5(6) . . ?
S2' Ni1 S1' 89.4(6) 2_656 . ?
S2' Ni1 S1' 89.4(6) . 2_656 ?
S2' Ni1 S1' 90.5(6) 2_656 2_656 ?
S1' Ni1 S1' 175.6(7) . 2_656 ?
S2 Ni1 S1 90.60(18) 2_656 . ?
S2 Ni1 S1 89.28(18) . . ?
S2 Ni1 S1 89.28(18) 2_656 2_656 ?
S2 Ni1 S1 90.60(18) . 2_656 ?
S1 Ni1 S1 175.24(15) . 2_656 ?
S2' Ni1 N1 91.2(3) . . ?
S2' Ni1 N1 91.2(3) 2_656 . ?
S2 Ni1 N1 91.44(8) 2_656 . ?
S2 Ni1 N1 91.44(8) . . ?
S1' Ni1 N1 92.2(3) . . ?
S1' Ni1 N1 92.2(3) 2_656 . ?
S1 Ni1 N1 92.38(7) . . ?
S1 Ni1 N1 92.38(7) 2_656 . ?
S2' Ni1 Ni2 88.8(3) . . ?
S2' Ni1 Ni2 88.8(3) 2_656 . ?
S2 Ni1 Ni2 88.56(8) 2_656 . ?
S2 Ni1 Ni2 88.56(8) . . ?
S1' Ni1 Ni2 87.8(3) . . ?
S1' Ni1 Ni2 87.8(3) 2_656 . ?
S1 Ni1 Ni2 87.62(7) . . ?
S1 Ni1 Ni2 87.62(7) 2_656 . ?
N1 Ni1 Ni2 180.0 . . ?
O2 Ni2 O2 179.9(3) 2_656 . ?
O2 Ni2 O1 91.6(3) 2_656 2_656 ?
O2 Ni2 O1 88.4(3) . 2_656 ?
O2 Ni2 O1 88.4(3) 2_656 . ?
O2 Ni2 O1 91.6(3) . . ?
O1 Ni2 O1 177.2(4) 2_656 . ?
O2 Ni2 N2 90.03(17) 2_656 1_565 ?
O2 Ni2 N2 90.03(17) . 1_565 ?
O1 Ni2 N2 88.60(18) 2_656 1_565 ?
O1 Ni2 N2 88.60(18) . 1_565 ?
N2 Ni2 O2' 90.9(7) 1_565 . ?
N2 Ni2 O2' 90.9(7) 1_565 2_656 ?
O2' Ni2 O2' 178.3(14) . 2_656 ?
N2 Ni2 O1' 89.5(7) 1_565 . ?
O2' Ni2 O1' 89.7(12) . . ?
O2' Ni2 O1' 90.3(13) 2_656 . ?
N2 Ni2 O1' 89.5(7) 1_565 2_656 ?
O2' Ni2 O1' 90.3(13) . 2_656 ?
O2' Ni2 O1' 89.7(12) 2_656 2_656 ?
O1' Ni2 O1' 179.0(14) . 2_656 ?
O2 Ni2 Ni1 89.97(17) 2_656 . ?
O2 Ni2 Ni1 89.97(17) . . ?
O1 Ni2 Ni1 91.40(18) 2_656 . ?
O1 Ni2 Ni1 91.40(18) . . ?
N2 Ni2 Ni1 180.0 1_565 . ?
O2' Ni2 Ni1 89.1(7) . . ?
O2' Ni2 Ni1 89.1(7) 2_656 . ?
O1' Ni2 Ni1 90.5(7) . . ?
O1' Ni2 Ni1 90.5(7) 2_656 . ?
C1 S1 Ni1 108.4(5) . . ?
C1 O1 Ni2 122.2(9) . . ?
O1 C1 C2 117.1(11) . . ?
O1 C1 S1 125.3(8) . . ?
C2 C1 S1 117.5(9) . . ?
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 . . ?
C3 S2 Ni1 106.9(4) . . ?
C3 O2 Ni2 122.0(8) . . ?
O2 C3 C4 118.0(11) . . ?
O2 C3 S2 126.2(8) . . ?
C4 C3 S2 115.8(8) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C1' S1' Ni1 111.6(16) . . ?
C1' O1' Ni2 122(2) . . ?
O1' C1' C2' 120(3) . . ?
O1' C1' S1' 123(2) . . ?
C2' C1' S1' 115(2) . . ?
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 . . ?
C3' S2' Ni1 111.3(15) . . ?
C3' O2' Ni2 122(2) . . ?
O2' C3' C4' 119(4) . . ?
O2' C3' S2' 122(2) . . ?
C4' C3' S2' 114(2) . . ?
C3' C4' H4A' 109.5 . . ?
C3' C4' H4B' 109.5 . . ?
H4A' C4' H4B' 109.5 . . ?
C3' C4' H4C' 109.5 . . ?
H4A' C4' H4C' 109.5 . . ?
H4B' C4' H4C' 109.5 . . ?
C5 N1 C5 117.5(9) 2_656 . ?
C5 N1 Ni1 121.3(4) 2_656 . ?
C5 N1 Ni1 121.3(4) . . ?
C6 N2 C6 118.5(9) . 2_656 ?
C6 N2 Ni2 120.7(5) . 1_545 ?
C6 N2 Ni2 120.7(5) 2_656 1_545 ?
N1 C5 C6 120.9(8) . . ?
N1 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
N2 C6 C5 121.0(8) . . ?
N2 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?

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
Ni2 O1 C1 C2 -170.7(13) . . . . ?
Ni2 O1 C1 S1 12(3) . . . . ?
Ni1 S1 C1 O1 8(3) . . . . ?
Ni1 S1 C1 C2 -170.1(16) . . . . ?
Ni2 O2 C3 C4 -169.1(12) . . . . ?
Ni2 O2 C3 S2 13(3) . . . . ?
Ni1 S2 C3 O2 9(2) . . . . ?
Ni1 S2 C3 C4 -169.4(14) . . . . ?
Ni2 O1' C1' C2' -178(6) . . . . ?
Ni2 O1' C1' S1' -14(15) . . . . ?
Ni1 S1' C1' O1' -5(13) . . . . ?
Ni1 S1' C1' C2' 159(7) . . . . ?
Ni2 O2' C3' C4' -174(5) . . . . ?
Ni2 O2' C3' S2' -19(11) . . . . ?
Ni1 S2' C3' O2' -2(10) . . . . ?
Ni1 S2' C3' C4' 155(5) . . . . ?
C5 N1 C5 C6 0.0(5) 2_656 . . . ?
Ni1 N1 C5 C6 -180.0(5) . . . . ?
C6 N2 C6 C5 0.0(5) 2_656 . . . ?
Ni2 N2 C6 C5 -180.0(5) 1_545 . . . ?
N1 C5 C6 N2 0.0(11) . . . . ?

_refine_diff_density_max         1.352
_refine_diff_density_min         -0.832
_refine_diff_density_rms         0.159

####################################################################### 
# 
# 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_Compound_2
_database_code_depnum_ccdc_archive 'CCDC 1513674'
_audit_update_record             
;
2017-01-30 deposited with the CCDC.
2017-02-17 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         'C16 H12 N Ni O2 S2, C3 H6 O'
_chemical_formula_sum            'C19 H18 N Ni O3 S2'
_chemical_formula_weight         431.17

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'
O O 0.0106 0.0060 '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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   27.620(6)
_cell_length_b                   9.630(2)
_cell_length_c                   18.507(4)
_cell_angle_alpha                90.00(3)
_cell_angle_beta                 127.04(3)
_cell_angle_gamma                90.00(3)
_cell_volume                     3929.6(19)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1105
_cell_measurement_theta_min      2.96
_cell_measurement_theta_max      27.76

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_F_000             1784
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    1.218
_shelx_estimated_absorpt_T_min   0.751
_shelx_estimated_absorpt_T_max   0.848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0219
_exptl_absorpt_correction_T_max  0.0526
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0631 before and 0.0383 after correction.
The Ratio of minimum to maximum transmission is 0.4163.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4474
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.209
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_full        24.996
_diffrn_measured_fraction_theta_max 0.841
_diffrn_measured_fraction_theta_full 0.841
_diffrn_reflns_Laue_measured_fraction_max 0.841
_diffrn_reflns_Laue_measured_fraction_full 0.841
_diffrn_reflns_point_group_measured_fraction_max 0.841
_diffrn_reflns_point_group_measured_fraction_full 0.841
_reflns_number_total             2914
_reflns_number_gt                2161
_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       'APEX2 v2013.6-2 (Bruker, 2013)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_structure_solution    'XM (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;Reflections -3 5 0 and 2 0 0 were affected by the beam stop and were 
omitted from the refinement.
The structure exhibits disorder induced by a 180 degree rotation of the 
thiocarboxylate ligand, inducing a ca. 0.7 Angstrom shift of the two Ni 
ions of the paddlewheel and the bridging pyrazine ligand. The occupancy 
ratio refined to 0.914(2) to 0.086(2). The ADPs of Ni and pyrazine atoms 
were each constrained to be identical between major and minor moieties. 
An enhanced rigid bond restraint with an effective standard deviation of
0.002 Angstrom squared was used for the Ni and disordered thiocarboxylate 
atoms., Twin
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1511P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2914
_refine_ls_number_parameters     286
_refine_ls_number_restraints     192
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0691
_refine_ls_wR_factor_ref         0.2071
_refine_ls_wR_factor_gt          0.1844
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      0.994
_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
Ni4 Ni 0.5000 0.35027(15) 0.7500 0.0180(4) Uani 0.914(2) 2 d S TU P A 1
Ni3 Ni 0.5000 0.08739(15) 0.7500 0.0182(4) Uani 0.914(2) 2 d S TU P A 1
S3 S 0.39958(6) 0.09043(17) 0.66956(11) 0.0246(4) Uani 0.914(2) 1 d . U P A 1
S1 S 0.49265(7) 0.09398(17) 0.62302(10) 0.0244(4) Uani 0.914(2) 1 d . U P A 1
O4 O 0.41548(18) 0.3524(5) 0.7173(3) 0.0261(10) Uani 0.914(2) 1 d . U P A 1
O2 O 0.46204(18) 0.3530(4) 0.6174(3) 0.0243(9) Uani 0.914(2) 1 d . U P A 1
N1 N 0.5000 0.5638(7) 0.7500 0.0187(12) Uani 0.914(2) 2 d DS TU P A 1
N2 N 0.5000 0.8525(8) 0.7500 0.0216(15) Uani 0.914(2) 2 d DS TU P A 1
C1 C 0.5413(3) 0.6367(7) 0.8235(4) 0.0243(13) Uani 0.914(2) 1 d D U P A 1
H1 H 0.5722 0.5886 0.8769 0.029 Uiso 0.914(2) 1 calc R U P A 1
C2 C 0.5407(3) 0.7795(7) 0.8245(4) 0.0237(13) Uani 0.914(2) 1 d D U P A 1
H2 H 0.5698 0.8274 0.8792 0.028 Uiso 0.914(2) 1 calc R U P A 1
Ni1 Ni 0.5000 0.1592(17) 0.7500 0.0182(4) Uani 0.086(2) 2 d S TU P A 2
Ni2 Ni 0.5000 0.4228(17) 0.7500 0.0180(4) Uani 0.086(2) 2 d DS TU P A 2
S4 S 0.4005(6) 0.4104(18) 0.6665(10) 0.017(2) Uani 0.086(2) 1 d . U P A 2
S2 S 0.4932(6) 0.4143(19) 0.6226(10) 0.020(2) Uani 0.086(2) 1 d . U P A 2
O3 O 0.4169(18) 0.151(5) 0.720(3) 0.021(4) Uani 0.086(2) 1 d . U P A 2
O1 O 0.4626(17) 0.154(5) 0.616(3) 0.019(4) Uani 0.086(2) 1 d . U P A 2
N3 N 0.5000 0.630(3) 0.7500 0.0187(12) Uani 0.086(2) 2 d DS TU P A 2
N4 N 0.5000 0.927(6) 0.7500 0.0216(15) Uani 0.086(2) 2 d DS TU P A 2
C3 C 0.540(2) 0.708(4) 0.821(3) 0.0243(13) Uani 0.086(2) 1 d D U P A 2
H3 H 0.5714 0.6613 0.8750 0.029 Uiso 0.086(2) 1 calc R U P A 2
C4 C 0.541(2) 0.850(4) 0.822(3) 0.0237(13) Uani 0.086(2) 1 d D U P A 2
H4 H 0.5722 0.8966 0.8765 0.028 Uiso 0.086(2) 1 calc R U P A 2
C5 C 0.4657(2) 0.2540(6) 0.5770(4) 0.0214(11) Uani 1 1 d . U . . .
C6 C 0.4453(2) 0.2778(7) 0.4822(4) 0.0276(14) Uani 1 1 d . . . . .
C7 C 0.4372(3) 0.1717(8) 0.4275(4) 0.0393(16) Uani 1 1 d . . . . .
H7 H 0.4464 0.0791 0.4496 0.047 Uiso 1 1 calc R U . . .
C8 C 0.4150(3) 0.2005(8) 0.3373(5) 0.0420(18) Uani 1 1 d . . . . .
H8 H 0.4085 0.1268 0.2983 0.050 Uiso 1 1 calc R U . . .
C9 C 0.4031(3) 0.3310(9) 0.3070(5) 0.0447(18) Uani 1 1 d . . . . .
H9 H 0.3882 0.3487 0.2464 0.054 Uiso 1 1 calc R U . . .
C10 C 0.4120(3) 0.4417(9) 0.3621(5) 0.052(2) Uani 1 1 d . . . . .
H10 H 0.4040 0.5345 0.3402 0.062 Uiso 1 1 calc R U . . .
C11 C 0.4323(3) 0.4132(8) 0.4469(5) 0.0458(18) Uani 1 1 d . . . . .
H11 H 0.4381 0.4879 0.4849 0.055 Uiso 1 1 calc R U . . .
C12 C 0.3801(2) 0.2519(6) 0.6805(4) 0.0223(11) Uani 1 1 d . U . . .
C13 C 0.3151(3) 0.2750(7) 0.6388(4) 0.0350(16) Uani 1 1 d . . . . .
C14 C 0.2739(3) 0.1736(8) 0.6181(5) 0.0406(17) Uani 1 1 d . . . . .
H14 H 0.2869 0.0796 0.6305 0.049 Uiso 1 1 calc R U . . .
C15 C 0.2136(3) 0.2032(9) 0.5796(5) 0.0459(19) Uani 1 1 d . . . . .
H15 H 0.1863 0.1300 0.5662 0.055 Uiso 1 1 calc R U . . .
C16 C 0.1941(3) 0.3338(10) 0.5615(5) 0.056(2) Uani 1 1 d . . . . .
H16 H 0.1532 0.3537 0.5373 0.067 Uiso 1 1 calc R U . . .
C17 C 0.2334(3) 0.4429(9) 0.5780(5) 0.052(2) Uani 1 1 d . . . . .
H17 H 0.2189 0.5356 0.5615 0.063 Uiso 1 1 calc R U . . .
C18 C 0.2931(3) 0.4130(8) 0.6182(5) 0.0455(19) Uani 1 1 d . . . . .
H18 H 0.3204 0.4869 0.6326 0.055 Uiso 1 1 calc R U . . .
C19 C 0.2703(4) 0.6869(13) 0.3102(6) 0.089(4) Uani 1 1 d . . . . .
H19A H 0.2521 0.6138 0.3237 0.134 Uiso 1 1 calc R U . . .
H19B H 0.2760 0.6523 0.2660 0.134 Uiso 1 1 calc R U . . .
H19C H 0.2433 0.7678 0.2851 0.134 Uiso 1 1 calc R U . . .
C20 C 0.3310(3) 0.7282(9) 0.3961(5) 0.051(2) Uani 1 1 d . . . . .
C21 C 0.3694(4) 0.8173(11) 0.3877(6) 0.077(3) Uani 1 1 d . . . . .
H21A H 0.3458 0.8966 0.3489 0.115 Uiso 1 1 calc R U . . .
H21B H 0.3854 0.7650 0.3608 0.115 Uiso 1 1 calc R U . . .
H21C H 0.4032 0.8509 0.4477 0.115 Uiso 1 1 calc R U . . .
O5 O 0.3461(3) 0.6856(8) 0.4677(4) 0.0752(19) 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
Ni4 O2 2.006(4) 2_656 ?
Ni4 O2 2.006(4) . ?
Ni4 O4 2.029(4) . ?
Ni4 O4 2.029(4) 2_656 ?
Ni4 N1 2.057(7) . ?
Ni4 Ni3 2.5316(18) . ?
Ni3 S3 2.2218(17) . ?
Ni3 S3 2.2218(17) 2_656 ?
Ni3 S1 2.2345(17) . ?
Ni3 S1 2.2345(17) 2_656 ?
Ni3 N2 2.262(8) 1_545 ?
S3 C12 1.697(6) . ?
S1 C5 1.700(6) . ?
O4 C12 1.247(7) . ?
O2 C5 1.252(7) . ?
N1 C1 1.333(7) . ?
N1 C1 1.333(7) 2_656 ?
N2 C2 1.339(7) . ?
N2 C2 1.339(7) 2_656 ?
N2 Ni3 2.262(8) 1_565 ?
C1 C2 1.376(9) . ?
C1 H1 0.9500 . ?
C2 H2 0.9500 . ?
Ni1 O3 2.01(4) 2_656 ?
Ni1 O3 2.01(4) . ?
Ni1 O1 2.04(4) . ?
Ni1 O1 2.04(4) 2_656 ?
Ni1 N4 2.24(6) 1_545 ?
Ni1 Ni2 2.538(19) . ?
Ni2 N3 1.99(2) . ?
Ni2 S4 2.200(13) . ?
Ni2 S4 2.200(13) 2_656 ?
Ni2 S2 2.251(15) 2_656 ?
Ni2 S2 2.251(15) . ?
S4 C12 1.700(18) . ?
S2 C5 1.702(18) . ?
O3 C12 1.27(4) . ?
O1 C5 1.23(4) . ?
N3 C3 1.33(2) 2_656 ?
N3 C3 1.33(2) . ?
N4 C4 1.34(2) 2_656 ?
N4 C4 1.34(2) . ?
N4 Ni1 2.24(6) 1_565 ?
C3 C4 1.37(2) . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C5 C6 1.502(8) . ?
C6 C7 1.358(9) . ?
C6 C11 1.405(10) . ?
C7 C8 1.417(9) . ?
C7 H7 0.9500 . ?
C8 C9 1.334(11) . ?
C8 H8 0.9500 . ?
C9 C10 1.390(11) . ?
C9 H9 0.9500 . ?
C10 C11 1.340(10) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 C13 1.481(8) . ?
C13 C14 1.369(9) . ?
C13 C18 1.415(10) . ?
C14 C15 1.390(9) . ?
C14 H14 0.9500 . ?
C15 C16 1.329(13) . ?
C15 H15 0.9500 . ?
C16 C17 1.406(12) . ?
C16 H16 0.9500 . ?
C17 C18 1.369(9) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.512(11) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 O5 1.196(9) . ?
C20 C21 1.445(12) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ni4 O2 178.5(3) 2_656 . ?
O2 Ni4 O4 91.37(18) 2_656 . ?
O2 Ni4 O4 88.61(18) . . ?
O2 Ni4 O4 88.61(18) 2_656 2_656 ?
O2 Ni4 O4 91.37(18) . 2_656 ?
O4 Ni4 O4 178.8(3) . 2_656 ?
O2 Ni4 N1 89.26(13) 2_656 . ?
O2 Ni4 N1 89.26(13) . . ?
O4 Ni4 N1 89.41(14) . . ?
O4 Ni4 N1 89.41(14) 2_656 . ?
O2 Ni4 Ni3 90.74(13) 2_656 . ?
O2 Ni4 Ni3 90.74(13) . . ?
O4 Ni4 Ni3 90.59(14) . . ?
O4 Ni4 Ni3 90.59(14) 2_656 . ?
N1 Ni4 Ni3 180.0 . . ?
S3 Ni3 S3 178.49(11) . 2_656 ?
S3 Ni3 S1 90.52(7) . . ?
S3 Ni3 S1 89.44(7) 2_656 . ?
S3 Ni3 S1 89.44(7) . 2_656 ?
S3 Ni3 S1 90.52(7) 2_656 2_656 ?
S1 Ni3 S1 176.74(11) . 2_656 ?
S3 Ni3 N2 90.76(7) . 1_545 ?
S3 Ni3 N2 90.76(7) 2_656 1_545 ?
S1 Ni3 N2 91.63(6) . 1_545 ?
S1 Ni3 N2 91.63(6) 2_656 1_545 ?
S3 Ni3 Ni4 89.24(7) . . ?
S3 Ni3 Ni4 89.24(7) 2_656 . ?
S1 Ni3 Ni4 88.37(6) . . ?
S1 Ni3 Ni4 88.37(6) 2_656 . ?
N2 Ni3 Ni4 180.0 1_545 . ?
C12 S3 Ni3 106.9(2) . . ?
C5 S1 Ni3 106.7(2) . . ?
C12 O4 Ni4 122.5(4) . . ?
C5 O2 Ni4 123.3(4) . . ?
C1 N1 C1 116.4(8) . 2_656 ?
C1 N1 Ni4 121.8(4) . . ?
C1 N1 Ni4 121.8(4) 2_656 . ?
C2 N2 C2 116.7(8) . 2_656 ?
C2 N2 Ni3 121.7(4) . 1_565 ?
C2 N2 Ni3 121.7(4) 2_656 1_565 ?
N1 C1 C2 122.0(6) . . ?
N1 C1 H1 119.0 . . ?
C2 C1 H1 119.0 . . ?
N2 C2 C1 121.4(6) . . ?
N2 C2 H2 119.3 . . ?
C1 C2 H2 119.3 . . ?
O3 Ni1 O3 175(3) 2_656 . ?
O3 Ni1 O1 89.7(17) 2_656 . ?
O3 Ni1 O1 90.2(17) . . ?
O3 Ni1 O1 90.2(17) 2_656 2_656 ?
O3 Ni1 O1 89.7(17) . 2_656 ?
O1 Ni1 O1 177(3) . 2_656 ?
O3 Ni1 N4 87.7(14) 2_656 1_545 ?
O3 Ni1 N4 87.7(14) . 1_545 ?
O1 Ni1 N4 88.7(13) . 1_545 ?
O1 Ni1 N4 88.7(13) 2_656 1_545 ?
O3 Ni1 Ni2 92.3(14) 2_656 . ?
O3 Ni1 Ni2 92.3(14) . . ?
O1 Ni1 Ni2 91.3(13) . . ?
O1 Ni1 Ni2 91.3(13) 2_656 . ?
N4 Ni1 Ni2 180.000(12) 1_545 . ?
N3 Ni2 S4 93.1(6) . . ?
N3 Ni2 S4 93.1(6) . 2_656 ?
S4 Ni2 S4 173.8(12) . 2_656 ?
N3 Ni2 S2 92.1(6) . 2_656 ?
S4 Ni2 S2 90.9(5) . 2_656 ?
S4 Ni2 S2 88.9(5) 2_656 2_656 ?
N3 Ni2 S2 92.1(6) . . ?
S4 Ni2 S2 88.9(5) . . ?
S4 Ni2 S2 90.9(5) 2_656 . ?
S2 Ni2 S2 175.8(12) 2_656 . ?
N3 Ni2 Ni1 180.000(10) . . ?
S4 Ni2 Ni1 86.9(6) . . ?
S4 Ni2 Ni1 86.9(6) 2_656 . ?
S2 Ni2 Ni1 87.9(6) 2_656 . ?
S2 Ni2 Ni1 87.9(6) . . ?
C12 S4 Ni2 109.3(9) . . ?
C5 S2 Ni2 106.5(9) . . ?
C12 O3 Ni1 121(3) . . ?
C5 O1 Ni1 122(3) . . ?
C3 N3 C3 111(4) 2_656 . ?
C3 N3 Ni2 124(2) 2_656 . ?
C3 N3 Ni2 124(2) . . ?
C4 N4 C4 113(4) 2_656 . ?
C4 N4 Ni1 123(2) 2_656 1_565 ?
C4 N4 Ni1 123(2) . 1_565 ?
N3 C3 C4 125(3) . . ?
N3 C3 H3 117.4 . . ?
C4 C3 H3 117.4 . . ?
N4 C4 C3 123(3) . . ?
N4 C4 H4 118.7 . . ?
C3 C4 H4 118.7 . . ?
O1 C5 C6 134(2) . . ?
O2 C5 C6 118.2(5) . . ?
O2 C5 S1 124.0(4) . . ?
C6 C5 S1 117.8(4) . . ?
O1 C5 S2 126(2) . . ?
C6 C5 S2 100.5(7) . . ?
C7 C6 C11 118.0(6) . . ?
C7 C6 C5 122.2(6) . . ?
C11 C6 C5 119.7(6) . . ?
C6 C7 C8 119.4(7) . . ?
C6 C7 H7 120.3 . . ?
C8 C7 H7 120.3 . . ?
C9 C8 C7 120.1(7) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C8 C9 C10 121.6(7) . . ?
C8 C9 H9 119.2 . . ?
C10 C9 H9 119.2 . . ?
C11 C10 C9 117.8(8) . . ?
C11 C10 H10 121.1 . . ?
C9 C10 H10 121.1 . . ?
C10 C11 C6 123.0(8) . . ?
C10 C11 H11 118.5 . . ?
C6 C11 H11 118.5 . . ?
O4 C12 C13 118.2(5) . . ?
O3 C12 C13 136(2) . . ?
O4 C12 S3 125.1(4) . . ?
C13 C12 S3 116.6(4) . . ?
O3 C12 S4 123(2) . . ?
C13 C12 S4 101.2(6) . . ?
C14 C13 C18 116.3(6) . . ?
C14 C13 C12 125.6(6) . . ?
C18 C13 C12 118.1(6) . . ?
C13 C14 C15 122.4(7) . . ?
C13 C14 H14 118.8 . . ?
C15 C14 H14 118.8 . . ?
C16 C15 C14 120.1(8) . . ?
C16 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
C15 C16 C17 120.7(7) . . ?
C15 C16 H16 119.7 . . ?
C17 C16 H16 119.7 . . ?
C18 C17 C16 118.7(8) . . ?
C18 C17 H17 120.6 . . ?
C16 C17 H17 120.6 . . ?
C17 C18 C13 121.7(7) . . ?
C17 C18 H18 119.1 . . ?
C13 C18 H18 119.1 . . ?
C20 C19 H19A 109.5 . . ?
C20 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C20 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O5 C20 C21 122.3(8) . . ?
O5 C20 C19 120.1(8) . . ?
C21 C20 C19 117.7(8) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?

_refine_diff_density_max         1.816
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.149

####################################################################### 
# 
# 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_Compound_5
_database_code_depnum_ccdc_archive 'CCDC 1513677'
_audit_update_record             
;
2017-01-30 deposited with the CCDC.
2017-02-17 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         'C70 H66 N2 Ni4 O8 S8, 0.582(C H2 Cl2)'
_chemical_formula_sum            'C70.58 H67.16 Cl1.16 N2 Ni4 O8 S8'
_chemical_formula_weight         1603.72

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'
O O 0.0106 0.0060 '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'
Cl Cl 0.1484 0.1585 '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                   10.9952(5)
_cell_length_b                   11.5241(6)
_cell_length_c                   14.5257(6)
_cell_angle_alpha                82.221(2)
_cell_angle_beta                 71.5160(10)
_cell_angle_gamma                88.952(2)
_cell_volume                     1728.94(14)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6737
_cell_measurement_theta_min      2.478
_cell_measurement_theta_max      28.250

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_F_000             828.4
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.416
_shelx_estimated_absorpt_T_min   0.676
_shelx_estimated_absorpt_T_max   0.871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2169
_exptl_absorpt_correction_T_max  0.2627
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0586 before and 0.0453 after correction.
The Ratio of minimum to maximum transmission is 0.8257.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_detector                 'Bruker APEX CCD'
_diffrn_detector_area_resol_mean 8.0
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_number            27583
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.478
_diffrn_reflns_theta_max         28.326
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             8545
_reflns_number_gt                6551
_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       'APEX2 v2013.6-2 (Bruker, 2013)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_structure_solution    'XT (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
Reflection 0 0 1 was affected by the beam stop and was omitted from the 
refinement. 

The thiocarboxylate units of all four thiobenzoate ligands are disordered 
by a ca. 30 degree rotation around their C-C axes. The thiocarboxylate units 
rotate in concert and the occupancy ratio is shared between the four 
thiobenzoate ligands. For one ligand the disorder extends out to the phenyl 
unit. All C-s and C-O distances were each restrained to be similar in length
(SADI commands) and minor thiocarboxylate units were restrained to be planar 
(FLAT command). ADPs of major and minor moiety oxygen and carbon atoms were 
constrained to be pairwise identical. For the completely disordered 
thiobenzoate ligand the geometry of the major and minor moiety were restrained 
to be similar. 

A solvate site is occupied by a disordered and partially occupied methylene 
chloride molecule. Two symmetry equivalent moieties are disordered around an 
inversion center. The two C-Cl distances were restrained to be similar (SADI 
command). The disorder extends to the immediately neighboring phenyl ring, 
with the major moiety phenyl position having the same occupancy as the total 
of the methylene chloride solvate occupancy. The geometries of the two phenyl 
units were restrained to be similar (SAME command). 

Uij components of ADPs of all disordered atoms were restrained to be similar 
for atoms closer to each other than 1.7 Angstrom (SIMU restraint). Given these 
conditions the occupancy ratio for the thiocarboxylate units refined to 
0.9182(11) to 0.818(11), and the occupancy for the methylene chloride molecule
(both disordered moieties combined) to 0.582(3). 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0245P)²+0.7037P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8545
_refine_ls_number_parameters     603
_refine_ls_number_restraints     542
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0336
_refine_ls_wR_factor_ref         0.0732
_refine_ls_wR_factor_gt          0.0662
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.008
_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
Ni2 Ni 0.24539(2) 0.36321(2) 0.27224(2) 0.01312(7) Uani 1 1 d . . . . .
Ni1 Ni 0.33058(2) 0.46767(2) 0.09500(2) 0.01516(7) Uani 1 1 d . . . . .
C1 C 0.2266(3) 0.2082(2) 0.13258(19) 0.0177(4) Uani 0.9182(11) 1 d D . P A 1
S1 S 0.33228(7) 0.29695(5) 0.03903(4) 0.02233(16) Uani 0.9182(11) 1 d D . P A 1
S2 S 0.52985(6) 0.44028(6) 0.10051(5) 0.01450(14) Uani 0.9182(11) 1 d D . P A 1
C8 C 0.5187(3) 0.3209(2) 0.18826(18) 0.0139(4) Uani 0.9182(11) 1 d D . P A 1
S3 S 0.32894(6) 0.63808(5) 0.14588(4) 0.01734(14) Uani 0.9182(11) 1 d D U P A 1
O3 O 0.31101(16) 0.50498(13) 0.31270(12) 0.0150(3) Uani 0.9182(11) 1 d D U P A
1
C15 C 0.3265(3) 0.6061(2) 0.26460(17) 0.0154(5) Uani 0.9182(11) 1 d D U P A 1
C16 C 0.3438(6) 0.7062(3) 0.3154(2) 0.0197(6) Uani 0.9182(11) 1 d D U P A 1
C17 C 0.3022(4) 0.6930(3) 0.4167(2) 0.0265(7) Uani 0.9182(11) 1 d D U P A 1
H17 H 0.2613 0.6215 0.4526 0.032 Uiso 0.9182(11) 1 calc R U P A 1
C18 C 0.3191(5) 0.7827(3) 0.4669(3) 0.0367(9) Uani 0.9182(11) 1 d D U P A 1
H18 H 0.2908 0.7721 0.5365 0.044 Uiso 0.9182(11) 1 calc R U P A 1
C19 C 0.3773(6) 0.8874(3) 0.4151(3) 0.0433(10) Uani 0.9182(11) 1 d D U P A 1
H19 H 0.3902 0.9487 0.4490 0.052 Uiso 0.9182(11) 1 calc R U P A 1
C20 C 0.4164(4) 0.9025(4) 0.3142(4) 0.0554(13) Uani 0.9182(11) 1 d D U P A 1
H20 H 0.4552 0.9749 0.2786 0.066 Uiso 0.9182(11) 1 calc R U P A 1
C21 C 0.3997(4) 0.8127(3) 0.2641(3) 0.0425(11) Uani 0.9182(11) 1 d D U P A 1
H21 H 0.4266 0.8242 0.1945 0.051 Uiso 0.9182(11) 1 calc R U P A 1
C22 C 0.0387(3) 0.4803(2) 0.21413(19) 0.0166(5) Uani 0.9182(11) 1 d D . P A 1
S4 S 0.13001(6) 0.49176(6) 0.09275(4) 0.02101(16) Uani 0.9182(11) 1 d D . P A 1
O1 O 0.17850(16) 0.23017(14) 0.21852(11) 0.0166(4) Uani 0.9182(11) 1 d D . P A
1
O2 O 0.41364(14) 0.27936(13) 0.24601(11) 0.0144(3) Uani 0.9182(11) 1 d D . P A
1
O4 O 0.07888(18) 0.44475(15) 0.28420(14) 0.0172(4) Uani 0.9182(11) 1 d D . P A
1
N1 N 0.18762(16) 0.28277(14) 0.42043(12) 0.0142(4) Uani 1 1 d . . . . .
C2 C 0.1920(2) 0.09437(19) 0.10940(16) 0.0211(5) Uani 0.582(3) 1 d D U P A 1
C3 C 0.1684(18) 0.0001(9) 0.1841(8) 0.0157(15) Uani 0.582(3) 1 d D U P A 1
H3 H 0.1736 0.0099 0.2466 0.019 Uiso 0.582(3) 1 calc R U P A 1
C4 C 0.1372(19) -0.1081(11) 0.1657(9) 0.0213(16) Uani 0.582(3) 1 d D U P A 1
H4 H 0.1290 -0.1750 0.2134 0.026 Uiso 0.582(3) 1 calc R U P A 1
C5 C 0.1180(8) -0.1190(7) 0.0775(6) 0.0298(17) Uani 0.582(3) 1 d D U P A 1
H5 H 0.0939 -0.1930 0.0659 0.036 Uiso 0.582(3) 1 calc R U P A 1
C6 C 0.1337(5) -0.0222(5) 0.0056(5) 0.0312(12) Uani 0.582(3) 1 d D U P A 1
H6 H 0.1209 -0.0304 -0.0549 0.037 Uiso 0.582(3) 1 calc R U P A 1
C7 C 0.1681(5) 0.0859(5) 0.0226(4) 0.0250(12) Uani 0.582(3) 1 d D U P A 1
H7 H 0.1751 0.1533 -0.0246 0.030 Uiso 0.582(3) 1 calc R U P A 1
C2' C 0.1920(2) 0.09437(19) 0.10940(16) 0.0211(5) Uani 0.418(3) 1 d D U P A 2
C3' C 0.156(3) -0.0066(13) 0.1780(12) 0.020(2) Uani 0.418(3) 1 d D U P A 2
H3' H 0.1508 -0.0015 0.2439 0.024 Uiso 0.418(3) 1 calc R U P A 2
C4' C 0.128(3) -0.1129(14) 0.1551(12) 0.022(2) Uani 0.418(3) 1 d D U P A 2
H4' H 0.0951 -0.1759 0.2061 0.026 Uiso 0.418(3) 1 calc R U P A 2
C5' C 0.1480(11) -0.1294(10) 0.0596(8) 0.0239(18) Uani 0.418(3) 1 d D U P A 2
H5' H 0.1326 -0.2041 0.0440 0.029 Uiso 0.418(3) 1 calc R U P A 2
C6' C 0.1902(7) -0.0358(7) -0.0130(6) 0.0269(15) Uani 0.418(3) 1 d D U P A 2
H6' H 0.2016 -0.0450 -0.0792 0.032 Uiso 0.418(3) 1 calc R U P A 2
C7' C 0.2162(8) 0.0718(7) 0.0100(6) 0.0263(16) Uani 0.418(3) 1 d D U P A 2
H7' H 0.2515 0.1334 -0.0420 0.032 Uiso 0.418(3) 1 calc R U P A 2
C9 C 0.63830(19) 0.26614(17) 0.19953(14) 0.0136(4) Uani 1 1 d . . . . .
C10 C 0.6263(2) 0.17389(18) 0.27461(15) 0.0188(5) Uani 1 1 d . . . . .
H10 H 0.5434 0.1477 0.3168 0.023 Uiso 1 1 calc R U . . .
C11 C 0.7338(2) 0.11994(19) 0.28837(16) 0.0218(5) Uani 1 1 d . . . . .
H11 H 0.7246 0.0563 0.3392 0.026 Uiso 1 1 calc R U . . .
C12 C 0.8549(2) 0.15879(19) 0.22800(16) 0.0216(5) Uani 1 1 d . . . . .
H12 H 0.9288 0.1224 0.2379 0.026 Uiso 1 1 calc R U . . .
C13 C 0.8683(2) 0.25058(19) 0.15320(17) 0.0229(5) Uani 1 1 d . . . . .
H13 H 0.9513 0.2774 0.1119 0.027 Uiso 1 1 calc R U . . .
C14 C 0.7605(2) 0.30343(18) 0.13853(15) 0.0177(4) Uani 1 1 d . . . . .
H14 H 0.7700 0.3656 0.0864 0.021 Uiso 1 1 calc R U . . .
C23 C -0.0997(2) 0.50825(18) 0.23865(16) 0.0177(4) Uani 1 1 d . . . . .
C24 C -0.1841(2) 0.45369(19) 0.32650(16) 0.0211(5) Uani 1 1 d . . . . .
H24 H -0.1523 0.4007 0.3690 0.025 Uiso 1 1 calc R U . . .
C25 C -0.3137(2) 0.4760(2) 0.35242(17) 0.0259(5) Uani 1 1 d . . . . .
H25 H -0.3708 0.4379 0.4122 0.031 Uiso 1 1 calc R U . . .
C26 C -0.3597(2) 0.5536(2) 0.29120(18) 0.0281(6) Uani 1 1 d . . . . .
H26 H -0.4487 0.5692 0.3091 0.034 Uiso 1 1 calc R U . . .
C27 C -0.2773(2) 0.6087(2) 0.20414(18) 0.0295(6) Uani 1 1 d . . . . .
H27 H -0.3099 0.6623 0.1626 0.035 Uiso 1 1 calc R U . . .
C28 C -0.1475(2) 0.5865(2) 0.17691(17) 0.0241(5) Uani 1 1 d . . . . .
H28 H -0.0911 0.6243 0.1166 0.029 Uiso 1 1 calc R U . . .
C29 C 0.1539(2) 0.15692(18) 0.42760(16) 0.0256(5) Uani 1 1 d . . . . .
H29A H 0.2312 0.1154 0.3935 0.031 Uiso 1 1 calc R U . . .
H29B H 0.0892 0.1495 0.3942 0.031 Uiso 1 1 calc R U . . .
C30 C 0.0999(2) 0.0986(2) 0.53498(16) 0.0257(5) Uani 1 1 d . . . . .
H30A H 0.0072 0.0805 0.5516 0.031 Uiso 1 1 calc R U . . .
H30B H 0.1440 0.0243 0.5441 0.031 Uiso 1 1 calc R U . . .
C31 C 0.2935(2) 0.2916(2) 0.46315(16) 0.0268(5) Uani 1 1 d . . . . .
H31A H 0.3083 0.3748 0.4677 0.032 Uiso 1 1 calc R U . . .
H31B H 0.3734 0.2631 0.4191 0.032 Uiso 1 1 calc R U . . .
C32 C 0.2627(2) 0.2201(2) 0.56540(16) 0.0244(5) Uani 1 1 d . . . . .
H32A H 0.3169 0.1503 0.5622 0.029 Uiso 1 1 calc R U . . .
H32B H 0.2808 0.2683 0.6113 0.029 Uiso 1 1 calc R U . . .
C33 C 0.0748(2) 0.3396(2) 0.48243(15) 0.0260(5) Uani 1 1 d . . . . .
H33A H -0.0001 0.3274 0.4607 0.031 Uiso 1 1 calc R U . . .
H33B H 0.0926 0.4250 0.4737 0.031 Uiso 1 1 calc R U . . .
C34 C 0.0420(2) 0.2909(2) 0.59150(16) 0.0269(5) Uani 1 1 d . . . . .
H34A H 0.0618 0.3510 0.6277 0.032 Uiso 1 1 calc R U . . .
H34B H -0.0506 0.2701 0.6195 0.032 Uiso 1 1 calc R U . . .
C35 C 0.1212(2) 0.18221(19) 0.60161(15) 0.0202(5) Uani 1 1 d . . . . .
H35 H 0.0955 0.1438 0.6712 0.024 Uiso 1 1 calc R U . . .
C1' C 0.2281(18) 0.2119(13) 0.1353(13) 0.0177(4) Uani 0.0818(11) 1 d D . P A 2
S1' S 0.2499(7) 0.3397(6) 0.0514(5) 0.0166(15) Uani 0.0818(11) 1 d D . P A 2
C8' C 0.525(3) 0.3314(19) 0.1934(12) 0.0139(4) Uani 0.0818(11) 1 d D . P A 2
S2' S 0.5178(7) 0.3916(7) 0.0805(6) 0.0134(15) Uani 0.0818(11) 1 d D . P A 2
S3' S 0.4047(7) 0.6267(5) 0.1611(5) 0.0145(14) Uani 0.0818(11) 1 d D U P A 2
O3' O 0.2532(17) 0.5264(15) 0.3310(13) 0.0150(3) Uani 0.0818(11) 1 d D U P A 2
C15' C 0.322(3) 0.613(2) 0.2833(12) 0.0154(5) Uani 0.0818(11) 1 d D U P A 2
C16' C 0.343(8) 0.717(4) 0.327(2) 0.025(3) Uani 0.0818(11) 1 d D U P A 2
C17' C 0.316(6) 0.712(4) 0.427(2) 0.028(3) Uani 0.0818(11) 1 d D U P A 2
H17' H 0.2858 0.6419 0.4700 0.033 Uiso 0.0818(11) 1 calc R U P A 2
C18' C 0.335(6) 0.813(4) 0.463(3) 0.033(3) Uani 0.0818(11) 1 d D U P A 2
H18' H 0.3038 0.8163 0.5311 0.040 Uiso 0.0818(11) 1 calc R U P A 2
C19' C 0.397(8) 0.910(4) 0.400(4) 0.042(3) Uani 0.0818(11) 1 d D U P A 2
H19' H 0.3976 0.9833 0.4235 0.051 Uiso 0.0818(11) 1 calc R U P A 2
C20' C 0.458(5) 0.900(4) 0.303(4) 0.043(3) Uani 0.0818(11) 1 d D U P A 2
H20' H 0.5177 0.9591 0.2621 0.052 Uiso 0.0818(11) 1 calc R U P A 2
C21' C 0.432(5) 0.802(3) 0.265(3) 0.036(3) Uani 0.0818(11) 1 d D U P A 2
H21' H 0.4731 0.7937 0.1987 0.043 Uiso 0.0818(11) 1 calc R U P A 2
S4' S 0.1436(6) 0.5685(5) 0.1327(5) 0.0151(15) Uani 0.0818(11) 1 d D . P A 2
C22' C 0.033(3) 0.4820(19) 0.2252(14) 0.0166(5) Uani 0.0818(11) 1 d D . P A 2
O1' O 0.2439(19) 0.2223(17) 0.2181(12) 0.0166(4) Uani 0.0818(11) 1 d D . P A 2
O2' O 0.4368(16) 0.3392(15) 0.2724(13) 0.0144(3) Uani 0.0818(11) 1 d D . P A 2
O4' O 0.067(2) 0.4009(19) 0.2779(19) 0.0172(4) Uani 0.0818(11) 1 d D . P A 2
C38 C 0.4733(8) -0.0597(7) 0.0215(6) 0.028(2) Uani 0.2910(15) 1 d D . P A -1
H38A H 0.3830 -0.0730 0.0639 0.034 Uiso 0.2910(15) 1 calc R U P A -1
H38B H 0.5221 -0.1289 0.0360 0.034 Uiso 0.2910(15) 1 calc R U P A -1
Cl1 Cl 0.4792(3) -0.0463(3) -0.1015(2) 0.0383(8) Uani 0.2910(15) 1 d D . P A -1
Cl2 Cl 0.5356(4) 0.0630(4) 0.0494(4) 0.0759(16) Uani 0.2910(15) 1 d D . P A -1


_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
Ni2 O1' 1.900(18) . ?
Ni2 O4' 1.98(3) . ?
Ni2 O4 2.0112(18) . ?
Ni2 O2 2.0220(15) . ?
Ni2 O3 2.0266(16) . ?
Ni2 O1 2.0565(16) . ?
Ni2 O2' 2.118(17) . ?
Ni2 N1 2.1238(16) . ?
Ni2 O3' 2.181(18) . ?
Ni2 Ni1 2.5746(4) . ?
Ni1 S1' 2.005(7) . ?
Ni1 S2' 2.181(7) . ?
Ni1 S3 2.1878(6) . ?
Ni1 S1 2.2258(7) . ?
Ni1 S4 2.2277(6) . ?
Ni1 S2 2.2328(7) . ?
Ni1 S4' 2.291(6) . ?
Ni1 S3' 2.444(6) . ?
C1 O1 1.251(3) . ?
C1 C2 1.482(3) . ?
C1 S1 1.706(3) . ?
S2 C8 1.721(3) . ?
C8 O2 1.251(3) . ?
C8 C9 1.494(4) . ?
S3 C15 1.706(3) . ?
O3 C15 1.260(3) . ?
C15 C16 1.495(3) . ?
C16 C17 1.383(4) . ?
C16 C21 1.389(4) . ?
C17 C18 1.390(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.380(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.378(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.390(4) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 O4 1.251(3) . ?
C22 C23 1.489(4) . ?
C22 S4 1.718(3) . ?
N1 C33 1.483(3) . ?
N1 C29 1.485(3) . ?
N1 C31 1.493(3) . ?
C2 C7 1.384(6) . ?
C2 C3 1.392(8) . ?
C3 C4 1.381(9) . ?
C3 H3 0.9500 . ?
C4 C5 1.385(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.393(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.385(7) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C2' C3' 1.398(11) . ?
C2' C7' 1.442(8) . ?
C2' C1' 1.544(16) . ?
C3' C4' 1.377(12) . ?
C3' H3' 0.9500 . ?
C4' C5' 1.374(12) . ?
C4' H4' 0.9500 . ?
C5' C6' 1.375(10) . ?
C5' H5' 0.9500 . ?
C6' C7' 1.384(9) . ?
C6' H6' 0.9500 . ?
C7' H7' 0.9500 . ?
C9 C10 1.392(3) . ?
C9 C14 1.392(3) . ?
C9 C8' 1.47(3) . ?
C10 C11 1.383(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.385(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.384(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.385(3) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C23 C24 1.392(3) . ?
C23 C28 1.399(3) . ?
C23 C22' 1.44(3) . ?
C24 C25 1.382(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.379(3) . ?
C25 H25 0.9500 . ?
C26 C27 1.379(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.384(3) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C30 1.543(3) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C35 1.524(3) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.536(3) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C35 1.527(3) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.536(3) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.530(3) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35 1.0000 . ?
C1' O1' 1.290(14) . ?
C1' S1' 1.748(14) . ?
C8' O2' 1.257(16) . ?
C8' S2' 1.716(16) . ?
S3' C15' 1.704(14) . ?
O3' C15' 1.250(14) . ?
C15' C16' 1.483(17) . ?
C16' C17' 1.377(18) . ?
C16' C21' 1.403(19) . ?
C17' C18' 1.379(18) . ?
C17' H17' 0.9500 . ?
C18' C19' 1.380(18) . ?
C18' H18' 0.9500 . ?
C19' C20' 1.376(19) . ?
C19' H19' 0.9500 . ?
C20' C21' 1.388(18) . ?
C20' H20' 0.9500 . ?
C21' H21' 0.9500 . ?
S4' C22' 1.712(16) . ?
C22' O4' 1.255(16) . ?
C38 Cl2 1.732(8) . ?
C38 Cl1 1.752(8) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?

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
O1' Ni2 O4' 93.9(9) . . ?
O4 Ni2 O2 174.11(7) . . ?
O4 Ni2 O3 88.79(6) . . ?
O2 Ni2 O3 94.61(6) . . ?
O4 Ni2 O1 88.81(7) . . ?
O2 Ni2 O1 87.36(6) . . ?
O3 Ni2 O1 174.18(6) . . ?
O1' Ni2 O2' 92.1(8) . . ?
O4' Ni2 O2' 174.0(8) . . ?
O1' Ni2 N1 95.5(5) . . ?
O4' Ni2 N1 92.6(8) . . ?
O4 Ni2 N1 94.66(7) . . ?
O2 Ni2 N1 90.19(6) . . ?
O3 Ni2 N1 89.50(6) . . ?
O1 Ni2 N1 95.97(6) . . ?
O2' Ni2 N1 86.9(5) . . ?
O1' Ni2 O3' 178.2(8) . . ?
O4' Ni2 O3' 87.4(8) . . ?
O2' Ni2 O3' 86.6(7) . . ?
N1 Ni2 O3' 85.7(5) . . ?
O1' Ni2 Ni1 87.1(5) . . ?
O4' Ni2 Ni1 90.8(8) . . ?
O4 Ni2 Ni1 87.88(6) . . ?
O2 Ni2 Ni1 87.51(4) . . ?
O3 Ni2 Ni1 86.86(5) . . ?
O1 Ni2 Ni1 87.75(4) . . ?
O2' Ni2 Ni1 89.4(5) . . ?
N1 Ni2 Ni1 175.53(5) . . ?
O3' Ni2 Ni1 91.6(5) . . ?
S1' Ni1 S2' 98.9(3) . . ?
S3 Ni1 S1 178.35(2) . . ?
S3 Ni1 S4 90.19(3) . . ?
S1 Ni1 S4 89.25(3) . . ?
S3 Ni1 S2 90.22(3) . . ?
S1 Ni1 S2 90.38(3) . . ?
S4 Ni1 S2 178.59(3) . . ?
S1' Ni1 S4' 91.9(2) . . ?
S2' Ni1 S4' 168.2(3) . . ?
S1' Ni1 S3' 173.5(2) . . ?
S2' Ni1 S3' 86.5(3) . . ?
S4' Ni1 S3' 82.5(2) . . ?
S1' Ni1 Ni2 89.19(18) . . ?
S2' Ni1 Ni2 89.74(19) . . ?
S3 Ni1 Ni2 91.503(19) . . ?
S1 Ni1 Ni2 90.052(18) . . ?
S4 Ni1 Ni2 89.967(18) . . ?
S2 Ni1 Ni2 88.677(19) . . ?
S4' Ni1 Ni2 85.74(15) . . ?
S3' Ni1 Ni2 87.12(15) . . ?
O1 C1 C2 117.9(2) . . ?
O1 C1 S1 125.6(2) . . ?
C2 C1 S1 116.46(19) . . ?
C1 S1 Ni1 105.05(9) . . ?
C8 S2 Ni1 105.48(11) . . ?
O2 C8 C9 117.7(2) . . ?
O2 C8 S2 122.7(2) . . ?
C9 C8 S2 119.58(19) . . ?
C15 S3 Ni1 104.85(9) . . ?
C15 O3 Ni2 124.54(16) . . ?
O3 C15 C16 117.6(2) . . ?
O3 C15 S3 125.06(19) . . ?
C16 C15 S3 117.3(2) . . ?
C17 C16 C21 118.7(3) . . ?
C17 C16 C15 119.2(2) . . ?
C21 C16 C15 122.1(3) . . ?
C16 C17 C18 121.1(3) . . ?
C16 C17 H17 119.4 . . ?
C18 C17 H17 119.4 . . ?
C19 C18 C17 119.7(3) . . ?
C19 C18 H18 120.1 . . ?
C17 C18 H18 120.1 . . ?
C20 C19 C18 119.7(3) . . ?
C20 C19 H19 120.2 . . ?
C18 C19 H19 120.2 . . ?
C19 C20 C21 120.6(3) . . ?
C19 C20 H20 119.7 . . ?
C21 C20 H20 119.7 . . ?
C16 C21 C20 120.2(3) . . ?
C16 C21 H21 119.9 . . ?
C20 C21 H21 119.9 . . ?
O4 C22 C23 117.0(2) . . ?
O4 C22 S4 124.6(3) . . ?
C23 C22 S4 118.4(2) . . ?
C22 S4 Ni1 104.59(12) . . ?
C1 O1 Ni2 123.19(16) . . ?
C8 O2 Ni2 124.78(17) . . ?
C22 O4 Ni2 125.0(2) . . ?
C33 N1 C29 108.04(17) . . ?
C33 N1 C31 107.07(17) . . ?
C29 N1 C31 108.45(16) . . ?
C33 N1 Ni2 112.05(12) . . ?
C29 N1 Ni2 110.75(12) . . ?
C31 N1 Ni2 110.34(13) . . ?
C7 C2 C3 121.4(6) . . ?
C7 C2 C1 121.4(3) . . ?
C3 C2 C1 116.7(5) . . ?
C4 C3 C2 118.8(9) . . ?
C4 C3 H3 120.6 . . ?
C2 C3 H3 120.6 . . ?
C3 C4 C5 119.9(9) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 C6 120.6(7) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C7 C6 C5 119.8(6) . . ?
C7 C6 H6 120.1 . . ?
C5 C6 H6 120.1 . . ?
C2 C7 C6 118.9(5) . . ?
C2 C7 H7 120.5 . . ?
C6 C7 H7 120.5 . . ?
C3' C2' C7' 113.0(8) . . ?
C3' C2' C1' 122.9(10) . . ?
C7' C2' C1' 123.0(7) . . ?
C4' C3' C2' 123.5(13) . . ?
C4' C3' H3' 118.3 . . ?
C2' C3' H3' 118.3 . . ?
C5' C4' C3' 121.1(13) . . ?
C5' C4' H4' 119.5 . . ?
C3' C4' H4' 119.5 . . ?
C4' C5' C6' 118.7(10) . . ?
C4' C5' H5' 120.6 . . ?
C6' C5' H5' 120.6 . . ?
C5' C6' C7' 120.3(8) . . ?
C5' C6' H6' 119.9 . . ?
C7' C6' H6' 119.9 . . ?
C6' C7' C2' 122.8(7) . . ?
C6' C7' H7' 118.6 . . ?
C2' C7' H7' 118.6 . . ?
C10 C9 C14 118.88(18) . . ?
C10 C9 C8' 119.7(7) . . ?
C14 C9 C8' 121.0(7) . . ?
C10 C9 C8 118.20(19) . . ?
C14 C9 C8 122.92(19) . . ?
C11 C10 C9 120.6(2) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C10 C11 C12 120.0(2) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C13 C12 C11 120.00(19) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C12 C13 C14 120.0(2) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C13 C14 C9 120.50(19) . . ?
C13 C14 H14 119.7 . . ?
C9 C14 H14 119.7 . . ?
C24 C23 C28 119.2(2) . . ?
C24 C23 C22' 113.8(8) . . ?
C28 C23 C22' 126.8(8) . . ?
C24 C23 C22 118.24(19) . . ?
C28 C23 C22 122.5(2) . . ?
C25 C24 C23 120.5(2) . . ?
C25 C24 H24 119.7 . . ?
C23 C24 H24 119.7 . . ?
C26 C25 C24 119.8(2) . . ?
C26 C25 H25 120.1 . . ?
C24 C25 H25 120.1 . . ?
C25 C26 C27 120.4(2) . . ?
C25 C26 H26 119.8 . . ?
C27 C26 H26 119.8 . . ?
C26 C27 C28 120.5(2) . . ?
C26 C27 H27 119.8 . . ?
C28 C27 H27 119.8 . . ?
C27 C28 C23 119.6(2) . . ?
C27 C28 H28 120.2 . . ?
C23 C28 H28 120.2 . . ?
N1 C29 C30 112.01(17) . . ?
N1 C29 H29A 109.2 . . ?
C30 C29 H29A 109.2 . . ?
N1 C29 H29B 109.2 . . ?
C30 C29 H29B 109.2 . . ?
H29A C29 H29B 107.9 . . ?
C35 C30 C29 108.82(18) . . ?
C35 C30 H30A 109.9 . . ?
C29 C30 H30A 109.9 . . ?
C35 C30 H30B 109.9 . . ?
C29 C30 H30B 109.9 . . ?
H30A C30 H30B 108.3 . . ?
N1 C31 C32 111.96(18) . . ?
N1 C31 H31A 109.2 . . ?
C32 C31 H31A 109.2 . . ?
N1 C31 H31B 109.2 . . ?
C32 C31 H31B 109.2 . . ?
H31A C31 H31B 107.9 . . ?
C35 C32 C31 108.87(17) . . ?
C35 C32 H32A 109.9 . . ?
C31 C32 H32A 109.9 . . ?
C35 C32 H32B 109.9 . . ?
C31 C32 H32B 109.9 . . ?
H32A C32 H32B 108.3 . . ?
N1 C33 C34 112.20(17) . . ?
N1 C33 H33A 109.2 . . ?
C34 C33 H33A 109.2 . . ?
N1 C33 H33B 109.2 . . ?
C34 C33 H33B 109.2 . . ?
H33A C33 H33B 107.9 . . ?
C35 C34 C33 108.92(18) . . ?
C35 C34 H34A 109.9 . . ?
C33 C34 H34A 109.9 . . ?
C35 C34 H34B 109.9 . . ?
C33 C34 H34B 109.9 . . ?
H34A C34 H34B 108.3 . . ?
C30 C35 C32 108.32(19) . . ?
C30 C35 C34 107.97(18) . . ?
C32 C35 C34 108.10(19) . . ?
C30 C35 H35 110.8 . . ?
C32 C35 H35 110.8 . . ?
C34 C35 H35 110.8 . . ?
O1' C1' C2' 123.1(14) . . ?
O1' C1' S1' 116.3(13) . . ?
C2' C1' S1' 120.6(11) . . ?
C1' S1' Ni1 110.6(7) . . ?
O2' C8' C9 117.3(15) . . ?
O2' C8' S2' 124(2) . . ?
C9 C8' S2' 119.0(15) . . ?
C8' S2' Ni1 110.0(11) . . ?
C15' S3' Ni1 107.4(8) . . ?
C15' O3' Ni2 123.5(15) . . ?
O3' C15' C16' 123.5(17) . . ?
O3' C15' S3' 124.7(17) . . ?
C16' C15' S3' 111.7(15) . . ?
C17' C16' C21' 118(3) . . ?
C17' C16' C15' 121(2) . . ?
C21' C16' C15' 117(2) . . ?
C16' C17' C18' 118(2) . . ?
C16' C17' H17' 121.0 . . ?
C18' C17' H17' 121.0 . . ?
C17' C18' C19' 121(2) . . ?
C17' C18' H18' 119.5 . . ?
C19' C18' H18' 119.5 . . ?
C20' C19' C18' 119(2) . . ?
C20' C19' H19' 120.4 . . ?
C18' C19' H19' 120.4 . . ?
C19' C20' C21' 119(2) . . ?
C19' C20' H20' 120.5 . . ?
C21' C20' H20' 120.5 . . ?
C20' C21' C16' 119(2) . . ?
C20' C21' H21' 120.3 . . ?
C16' C21' H21' 120.3 . . ?
C22' S4' Ni1 107.0(12) . . ?
O4' C22' C23 122.8(18) . . ?
O4' C22' S4' 121(3) . . ?
C23 C22' S4' 116.3(18) . . ?
C1' O1' Ni2 127.0(14) . . ?
C8' O2' Ni2 119.8(16) . . ?
C22' O4' Ni2 126(2) . . ?
Cl2 C38 Cl1 112.7(5) . . ?
Cl2 C38 H38A 109.1 . . ?
Cl1 C38 H38A 109.1 . . ?
Cl2 C38 H38B 109.1 . . ?
Cl1 C38 H38B 109.1 . . ?
H38A C38 H38B 107.8 . . ?

_refine_diff_density_max         0.431
_refine_diff_density_min         -0.556
_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. 
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data_Compound_3
_database_code_depnum_ccdc_archive 'CCDC 1513675'
_audit_update_record             
;
2017-01-30 deposited with the CCDC.
2017-02-17 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         ?
_chemical_formula_sum            'C14 H24 N2 Ni2 O4 S4'
_chemical_formula_weight         530.01

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'
O O 0.0106 0.0060 '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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   13.324(6)
_cell_length_b                   9.791(5)
_cell_length_c                   16.613(12)
_cell_angle_alpha                90
_cell_angle_beta                 110.61(3)
_cell_angle_gamma                90
_cell_volume                     2029(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2404
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      26.36

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_F_000             1096
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    2.290
_shelx_estimated_absorpt_T_min   0.577
_shelx_estimated_absorpt_T_max   0.838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0361
_exptl_absorpt_correction_T_max  0.0627
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0576 before and 0.0435 after correction.
The Ratio of minimum to maximum transmission is 0.5758.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Ultra'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_detector_type            'CCD Area Detector'
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6108
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.310
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_full        24.997
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.901
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1783
_reflns_number_gt                1550
_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       'APEX2 v2013.6-2 (Bruker, 2013)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
Reflections -3 5 0, -8 4 1, 1 7 1, -1 7 1, -1 7 3, 1 5 0, -9 1 3, 
-8 2 1 and 10 4 3 were affected by the beam stop and were omitted 
from the refinement. Twinning by pseudo-merohedry by a 180 degree 
rotation around the [1 0 2] direct lattice direction was handled using 
the twin matrix -1 0 0 0 -1 0 1 0 1 resulting in a BASF value of 
0.061(3). Both thioacetate anions were refined using a two part 
disorder model with a common occupancy ratio. The four disordered 
moieties were restrained to have similar geometries (SAME restraint), 
and Uij components of ADPs were restrained to be similar for atoms 
closer to each other than 1.7 Angstrom (SIMU restraint). Minor moiety 
thioacetate anions were restrained to be planar (FLAT restraint). 
The shared occupancy ratio refined to 0.962(5) to 0.038(5). 
The DABCO ligand was also disordered in a 50:50 manner as a result of 
its location across a crystallographic two fold axis. Uij components 
of ADPs of all DABCO carbon and nitrogen atoms were restrained to 
be similar for atoms closer to each other than 1.7 Angstrom. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0760P)²+74.4152P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1783
_refine_ls_number_parameters     223
_refine_ls_number_restraints     284
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0697
_refine_ls_wR_factor_ref         0.1902
_refine_ls_wR_factor_gt          0.1826
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      0.992
_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
Ni2 Ni 0.5000 0.50900(15) 0.2500 0.0189(4) Uani 1 2 d S T P . .
Ni1 Ni 0.5000 0.77405(15) 0.2500 0.0209(4) Uani 1 2 d S T P A .
S1 S 0.6749(2) 0.7650(2) 0.32553(17) 0.0267(6) Uani 0.962(5) 1 d D U P A 1
O1 O 0.6348(5) 0.5130(6) 0.3577(4) 0.0216(15) Uani 0.962(5) 1 d D U P A 1
C1 C 0.7001(7) 0.6094(9) 0.3740(6) 0.0243(18) Uani 0.962(5) 1 d D U P A 1
C2 C 0.8068(8) 0.5880(11) 0.4444(7) 0.032(2) Uani 0.962(5) 1 d D U P A 1
H2A H 0.8591 0.6528 0.4373 0.047 Uiso 0.962(5) 1 calc R U P A 1
H2B H 0.8315 0.4945 0.4414 0.047 Uiso 0.962(5) 1 calc R U P A 1
H2C H 0.7993 0.6027 0.5004 0.047 Uiso 0.962(5) 1 calc R U P A 1
S2 S 0.4636(2) 0.7663(2) 0.37172(16) 0.0265(6) Uani 0.962(5) 1 d D U P A 1
O2 O 0.4071(5) 0.5134(6) 0.3260(4) 0.0217(14) Uani 0.962(5) 1 d D U P A 1
C3 C 0.4104(8) 0.6096(9) 0.3756(6) 0.0243(18) Uani 0.962(5) 1 d D U P A 1
C4 C 0.3641(9) 0.5851(11) 0.4455(7) 0.030(2) Uani 0.962(5) 1 d D U P A 1
H4A H 0.4225 0.5781 0.5012 0.045 Uiso 0.962(5) 1 calc R U P A 1
H4B H 0.3228 0.4999 0.4336 0.045 Uiso 0.962(5) 1 calc R U P A 1
H4C H 0.3170 0.6613 0.4468 0.045 Uiso 0.962(5) 1 calc R U P A 1
S1' S 0.647(5) 0.763(6) 0.369(4) 0.025(4) Uani 0.038(5) 1 d D U P A 2
O1' O 0.613(11) 0.498(8) 0.364(8) 0.023(4) Uani 0.038(5) 1 d D U P A 2
C1' C 0.679(7) 0.594(7) 0.385(3) 0.025(3) Uani 0.038(5) 1 d D U P A 2
C2' C 0.796(9) 0.559(13) 0.428(10) 0.027(8) Uani 0.038(5) 1 d D U P A 2
H2A' H 0.8383 0.6428 0.4409 0.041 Uiso 0.038(5) 1 calc R U P A 2
H2B' H 0.8057 0.5089 0.4812 0.041 Uiso 0.038(5) 1 calc R U P A 2
H2C' H 0.8189 0.5015 0.3892 0.041 Uiso 0.038(5) 1 calc R U P A 2
S2' S 0.396(6) 0.754(6) 0.337(4) 0.026(4) Uani 0.038(5) 1 d D U P A 2
O2' O 0.448(10) 0.496(8) 0.333(9) 0.023(4) Uani 0.038(5) 1 d D U P A 2
C3' C 0.405(5) 0.585(6) 0.363(5) 0.025(3) Uani 0.038(5) 1 d D U P A 2
C4' C 0.356(14) 0.539(13) 0.428(10) 0.026(8) Uani 0.038(5) 1 d D U P A 2
H4A' H 0.3240 0.6182 0.4464 0.039 Uiso 0.038(5) 1 calc R U P A 2
H4B' H 0.2995 0.4715 0.4013 0.039 Uiso 0.038(5) 1 calc R U P A 2
H4C' H 0.4111 0.4987 0.4776 0.039 Uiso 0.038(5) 1 calc R U P A 2
N1 N 0.5000 0.2880(11) 0.2500 0.028(2) Uani 1 2 d S TU P A .
N2 N 0.5000 0.0225(11) 0.2500 0.031(2) Uani 1 2 d S TU P . .
C10 C 0.533(2) 0.0787(19) 0.3390(13) 0.037(4) Uani 0.5 1 d . U P A -1
H10A H 0.6081 0.0508 0.3716 0.044 Uiso 0.5 1 calc R U P A -1
H10B H 0.4869 0.0400 0.3686 0.044 Uiso 0.5 1 calc R U P A -1
C8 C 0.3892(18) 0.080(2) 0.2083(16) 0.038(4) Uani 0.5 1 d . U P A -1
H8A H 0.3448 0.0538 0.2428 0.046 Uiso 0.5 1 calc R U P A -1
H8B H 0.3560 0.0389 0.1504 0.046 Uiso 0.5 1 calc R U P A -1
C9 C 0.5255(19) 0.236(2) 0.3388(14) 0.037(4) Uani 0.5 1 d . U P A -1
H9A H 0.4688 0.2644 0.3610 0.045 Uiso 0.5 1 calc R U P A -1
H9B H 0.5944 0.2752 0.3767 0.045 Uiso 0.5 1 calc R U P A -1
C7 C 0.3896(17) 0.237(2) 0.1999(16) 0.037(4) Uani 0.5 1 d . U P A -1
H7A H 0.3694 0.2628 0.1387 0.045 Uiso 0.5 1 calc R U P A -1
H7B H 0.3370 0.2774 0.2227 0.045 Uiso 0.5 1 calc R U P A -1
C6 C 0.5642(18) 0.076(2) 0.2077(14) 0.034(3) Uani 0.5 1 d . U P A -1
H6A H 0.5336 0.0493 0.1464 0.041 Uiso 0.5 1 calc R U P A -1
H6B H 0.6362 0.0343 0.2321 0.041 Uiso 0.5 1 calc R U P A -1
C5 C 0.5774(19) 0.234(2) 0.2125(16) 0.040(4) Uani 0.5 1 d . U P A -1
H5A H 0.6515 0.2586 0.2491 0.048 Uiso 0.5 1 calc R U P A -1
H5B H 0.5626 0.2721 0.1543 0.048 Uiso 0.5 1 calc R U P A -1


_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
Ni2 O2' 1.75(13) 2_655 ?
Ni2 O2' 1.75(13) . ?
Ni2 O1' 1.96(11) 2_655 ?
Ni2 O1' 1.96(11) . ?
Ni2 O1 2.041(7) 2_655 ?
Ni2 O1 2.041(7) . ?
Ni2 O2 2.056(6) . ?
Ni2 O2 2.056(6) 2_655 ?
Ni2 N1 2.164(11) . ?
Ni2 Ni1 2.595(2) . ?
Ni1 S1 2.226(3) 2_655 ?
Ni1 S1 2.226(3) . ?
Ni1 S1' 2.24(6) . ?
Ni1 S1' 2.24(6) 2_655 ?
Ni1 S2 2.240(3) 2_655 ?
Ni1 S2 2.240(3) . ?
Ni1 S2' 2.35(6) 2_655 ?
Ni1 S2' 2.35(6) . ?
Ni1 N2 2.432(11) 1_565 ?
S1 C1 1.700(9) . ?
O1 C1 1.247(10) . ?
C1 C2 1.504(11) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
S2 C3 1.700(8) . ?
O2 C3 1.243(10) . ?
C3 C4 1.514(11) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
S1' C1' 1.701(18) . ?
O1' C1' 1.245(18) . ?
C1' C2' 1.510(19) . ?
C2' H2A' 0.9800 . ?
C2' H2B' 0.9800 . ?
C2' H2C' 0.9800 . ?
S2' C3' 1.702(18) . ?
O2' C3' 1.246(18) . ?
C3' C4' 1.511(19) . ?
C4' H4A' 0.9800 . ?
C4' H4B' 0.9800 . ?
C4' H4C' 0.9800 . ?
N1 C5 1.48(2) . ?
N1 C9 1.48(2) . ?
N1 C7 1.50(2) . ?
N2 C6 1.39(2) . ?
N2 C10 1.49(2) . ?
N2 C8 1.50(2) . ?
N2 Ni1 2.432(11) 1_545 ?
C10 C9 1.54(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C8 C7 1.54(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C6 C5 1.55(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?

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
O2' Ni2 O2' 171(5) 2_655 . ?
O2' Ni2 O1' 68(6) 2_655 2_655 ?
O2' Ni2 O1' 112(7) . 2_655 ?
O2' Ni2 O1' 112(7) 2_655 . ?
O2' Ni2 O1' 68(6) . . ?
O1' Ni2 O1' 174(4) 2_655 . ?
O1 Ni2 O1 177.8(4) 2_655 . ?
O1 Ni2 O2 90.2(3) 2_655 . ?
O1 Ni2 O2 89.7(3) . . ?
O1 Ni2 O2 89.7(3) 2_655 2_655 ?
O1 Ni2 O2 90.2(3) . 2_655 ?
O2 Ni2 O2 177.6(3) . 2_655 ?
O2' Ni2 N1 86(2) 2_655 . ?
O2' Ni2 N1 86(2) . . ?
O1' Ni2 N1 87(2) 2_655 . ?
O1' Ni2 N1 87(2) . . ?
O1 Ni2 N1 91.11(18) 2_655 . ?
O1 Ni2 N1 91.11(18) . . ?
O2 Ni2 N1 91.19(17) . . ?
O2 Ni2 N1 91.19(17) 2_655 . ?
O2' Ni2 Ni1 94(2) 2_655 . ?
O2' Ni2 Ni1 94(2) . . ?
O1' Ni2 Ni1 93(2) 2_655 . ?
O1' Ni2 Ni1 93(2) . . ?
O1 Ni2 Ni1 88.89(18) 2_655 . ?
O1 Ni2 Ni1 88.89(18) . . ?
O2 Ni2 Ni1 88.81(17) . . ?
O2 Ni2 Ni1 88.81(17) 2_655 . ?
N1 Ni2 Ni1 180.0 . . ?
S1 Ni1 S1 175.44(14) 2_655 . ?
S1' Ni1 S1' 174(3) . 2_655 ?
S1 Ni1 S2 90.35(11) 2_655 2_655 ?
S1 Ni1 S2 89.50(11) . 2_655 ?
S1 Ni1 S2 89.50(11) 2_655 . ?
S1 Ni1 S2 90.34(11) . . ?
S2 Ni1 S2 176.10(14) 2_655 . ?
S1' Ni1 S2' 91(2) . 2_655 ?
S1' Ni1 S2' 88(2) 2_655 2_655 ?
S1' Ni1 S2' 88(2) . . ?
S1' Ni1 S2' 91(2) 2_655 . ?
S2' Ni1 S2' 170(3) 2_655 . ?
S1 Ni1 N2 92.28(7) 2_655 1_565 ?
S1 Ni1 N2 92.28(7) . 1_565 ?
S1' Ni1 N2 92.8(15) . 1_565 ?
S1' Ni1 N2 92.8(15) 2_655 1_565 ?
S2 Ni1 N2 91.95(7) 2_655 1_565 ?
S2 Ni1 N2 91.95(7) . 1_565 ?
S2' Ni1 N2 94.8(14) 2_655 1_565 ?
S2' Ni1 N2 94.8(14) . 1_565 ?
S1 Ni1 Ni2 87.72(7) 2_655 . ?
S1 Ni1 Ni2 87.72(7) . . ?
S1' Ni1 Ni2 87.2(15) . . ?
S1' Ni1 Ni2 87.2(15) 2_655 . ?
S2 Ni1 Ni2 88.05(7) 2_655 . ?
S2 Ni1 Ni2 88.05(7) . . ?
S2' Ni1 Ni2 85.2(14) 2_655 . ?
S2' Ni1 Ni2 85.2(14) . . ?
N2 Ni1 Ni2 180.0 1_565 . ?
C1 S1 Ni1 107.2(3) . . ?
C1 O1 Ni2 122.4(6) . . ?
O1 C1 C2 117.3(8) . . ?
O1 C1 S1 124.7(7) . . ?
C2 C1 S1 117.9(7) . . ?
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 . . ?
C3 S2 Ni1 106.9(3) . . ?
C3 O2 Ni2 122.3(6) . . ?
O2 C3 C4 117.4(8) . . ?
O2 C3 S2 125.2(7) . . ?
C4 C3 S2 117.4(7) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C1' S1' Ni1 106(3) . . ?
C1' O1' Ni2 117(6) . . ?
O1' C1' C2' 117(3) . . ?
O1' C1' S1' 125(3) . . ?
C2' C1' S1' 117(2) . . ?
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 . . ?
C3' S2' Ni1 103(4) . . ?
C3' O2' Ni2 129(5) . . ?
O2' C3' C4' 117(3) . . ?
O2' C3' S2' 126(3) . . ?
C4' C3' S2' 117(2) . . ?
C3' C4' H4A' 109.5 . . ?
C3' C4' H4B' 109.5 . . ?
H4A' C4' H4B' 109.5 . . ?
C3' C4' H4C' 109.5 . . ?
H4A' C4' H4C' 109.5 . . ?
H4B' C4' H4C' 109.5 . . ?
C5 N1 C9 110.3(14) . . ?
C5 N1 C7 109.8(13) . . ?
C9 N1 C7 105.9(13) . . ?
C5 N1 Ni2 111.1(9) . . ?
C9 N1 Ni2 110.1(9) . . ?
C7 N1 Ni2 109.6(9) . . ?
C6 N2 C10 109.9(13) . . ?
C6 N2 C8 107.8(13) . . ?
C10 N2 C8 102.8(13) . . ?
C6 N2 Ni1 112.3(9) . 1_545 ?
C10 N2 Ni1 111.7(8) . 1_545 ?
C8 N2 Ni1 111.9(9) . 1_545 ?
N2 C10 C9 111.7(16) . . ?
N2 C10 H10A 109.3 . . ?
C9 C10 H10A 109.3 . . ?
N2 C10 H10B 109.3 . . ?
C9 C10 H10B 109.3 . . ?
H10A C10 H10B 108.0 . . ?
N2 C8 C7 112.2(17) . . ?
N2 C8 H8A 109.2 . . ?
C7 C8 H8A 109.2 . . ?
N2 C8 H8B 109.2 . . ?
C7 C8 H8B 109.2 . . ?
H8A C8 H8B 107.9 . . ?
N1 C9 C10 109.7(16) . . ?
N1 C9 H9A 109.7 . . ?
C10 C9 H9A 109.7 . . ?
N1 C9 H9B 109.7 . . ?
C10 C9 H9B 109.7 . . ?
H9A C9 H9B 108.2 . . ?
N1 C7 C8 108.6(16) . . ?
N1 C7 H7A 110.0 . . ?
C8 C7 H7A 110.0 . . ?
N1 C7 H7B 110.0 . . ?
C8 C7 H7B 110.0 . . ?
H7A C7 H7B 108.4 . . ?
N2 C6 C5 115.4(17) . . ?
N2 C6 H6A 108.4 . . ?
C5 C6 H6A 108.4 . . ?
N2 C6 H6B 108.4 . . ?
C5 C6 H6B 108.4 . . ?
H6A C6 H6B 107.5 . . ?
N1 C5 C6 107.2(17) . . ?
N1 C5 H5A 110.3 . . ?
C6 C5 H5A 110.3 . . ?
N1 C5 H5B 110.3 . . ?
C6 C5 H5B 110.3 . . ?
H5A C5 H5B 108.5 . . ?

_refine_diff_density_max         1.969
_refine_diff_density_min         -1.826
_refine_diff_density_rms         0.194

