# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_ss1892fneu
_database_code_depnum_ccdc_archive 'CCDC 1506855'
_audit_update_record             
;
2016-09-27 deposited with the CCDC.
2016-10-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H36 N6 Ni O8 S2'
_chemical_formula_sum            'C34 H36 N6 Ni O8 S2'
_chemical_formula_weight         779.52

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'
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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   11.0327(3)
_cell_length_b                   14.2185(3)
_cell_length_c                   11.9259(4)
_cell_angle_alpha                90
_cell_angle_beta                 95.618(2)
_cell_angle_gamma                90
_cell_volume                     1861.81(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    27836
_cell_measurement_theta_min      1.716
_cell_measurement_theta_max      27.350

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_F_000             812
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.1510
_exptl_crystal_size_mid          0.0856
_exptl_crystal_size_min          0.053
_exptl_absorpt_coefficient_mu    0.690
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.917
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_process_details   'X-Shape and X-Red 32 (STOE, 2008)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS-2'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27836
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.716
_diffrn_reflns_theta_max         27.350
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8365
_reflns_number_gt                7689
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.919
_reflns_Friedel_fraction_max     0.993
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0431P)²+0.0897P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 3405 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8365
_refine_ls_number_parameters     502
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0305
_refine_ls_wR_factor_ref         0.0767
_refine_ls_wR_factor_gt          0.0754
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.58216(3) 0.92501(2) 0.70993(3) 0.03173(9) Uani 1 1 d . . . . .
N1 N 0.6557(2) 1.05489(18) 0.6936(2) 0.0376(5) Uani 1 1 d . . . . .
C1 C 0.6979(3) 1.1268(2) 0.7200(3) 0.0382(6) Uani 1 1 d . . . . .
S1 S 0.75320(11) 1.22770(7) 0.76337(12) 0.0717(3) Uani 1 1 d . . . . .
N2 N 0.5108(2) 0.79227(18) 0.7203(2) 0.0387(5) Uani 1 1 d . . . . .
C2 C 0.4800(3) 0.7160(2) 0.6964(3) 0.0395(6) Uani 1 1 d . . . . .
S2 S 0.43783(12) 0.60961(7) 0.66234(11) 0.0711(3) Uani 1 1 d . . . . .
N11 N 0.6170(2) 0.89216(17) 0.5418(2) 0.0360(5) Uani 1 1 d . . . . .
C11 C 0.5366(3) 0.8447(2) 0.4708(3) 0.0392(6) Uani 1 1 d . . . . .
H11 H 0.4580 0.8324 0.4936 0.047 Uiso 1 1 calc R U . . .
C12 C 0.5628(3) 0.8132(2) 0.3667(3) 0.0417(6) Uani 1 1 d . . . . .
H12 H 0.5030 0.7811 0.3184 0.050 Uiso 1 1 calc R U . . .
C13 C 0.6779(3) 0.8293(2) 0.3337(2) 0.0388(6) Uani 1 1 d . . . . .
C14 C 0.7610(3) 0.8801(2) 0.4053(3) 0.0410(7) Uani 1 1 d . . . . .
H14 H 0.8402 0.8934 0.3845 0.049 Uiso 1 1 calc R U . . .
C15 C 0.7259(3) 0.9110(2) 0.5075(2) 0.0387(6) Uani 1 1 d . . . . .
H15 H 0.7820 0.9472 0.5553 0.046 Uiso 1 1 calc R U . . .
C16 C 0.7095(3) 0.7901(2) 0.2242(3) 0.0426(7) Uani 1 1 d . . . . .
C17 C 0.8673(4) 0.7626(3) 0.1065(3) 0.0602(10) Uani 1 1 d . . . . .
H17A H 0.9395 0.7982 0.0870 0.072 Uiso 1 1 calc R U . . .
H17B H 0.8017 0.7711 0.0445 0.072 Uiso 1 1 calc R U . . .
C18 C 0.8987(4) 0.6612(4) 0.1170(4) 0.0654(11) Uani 1 1 d . . . . .
H18A H 0.9645 0.6526 0.1775 0.098 Uiso 1 1 calc R U . . .
H18B H 0.9254 0.6386 0.0458 0.098 Uiso 1 1 calc R U . . .
H18C H 0.8269 0.6256 0.1346 0.098 Uiso 1 1 calc R U . . .
O11 O 0.6357(2) 0.75243(19) 0.1575(2) 0.0561(6) Uani 1 1 d . . . . .
O12 O 0.8272(2) 0.8004(2) 0.2103(2) 0.0558(6) Uani 1 1 d . . . . .
N21 N 0.7587(2) 0.87461(17) 0.7738(2) 0.0343(5) Uani 1 1 d . . . . .
C21 C 0.7898(3) 0.7852(2) 0.7574(3) 0.0390(6) Uani 1 1 d . . . . .
H21 H 0.7310 0.7444 0.7198 0.047 Uiso 1 1 calc R U . . .
C22 C 0.9036(3) 0.7493(2) 0.7925(3) 0.0405(7) Uani 1 1 d . . . . .
H22 H 0.9218 0.6851 0.7800 0.049 Uiso 1 1 calc R U . . .
C23 C 0.9902(3) 0.8080(2) 0.8459(2) 0.0363(6) Uani 1 1 d . . . . .
C24 C 0.9587(3) 0.9005(2) 0.8639(3) 0.0398(6) Uani 1 1 d . . . . .
H24 H 1.0162 0.9425 0.9012 0.048 Uiso 1 1 calc R U . . .
C25 C 0.8429(2) 0.9312(2) 0.8273(2) 0.0391(5) Uani 1 1 d . . . . .
H25 H 0.8221 0.9948 0.8404 0.047 Uiso 1 1 calc R U . . .
C26 C 1.1163(3) 0.7751(2) 0.8838(3) 0.0401(6) Uani 1 1 d . . . . .
C27 C 1.2453(3) 0.6412(3) 0.9114(3) 0.0510(8) Uani 1 1 d . . . . .
H27A H 1.2693 0.6519 0.9925 0.061 Uiso 1 1 calc R U . . .
H27B H 1.3076 0.6697 0.8676 0.061 Uiso 1 1 calc R U . . .
C28 C 1.2336(3) 0.5385(3) 0.8871(4) 0.0577(9) Uani 1 1 d . . . . .
H28A H 1.1724 0.5112 0.9317 0.087 Uiso 1 1 calc R U . . .
H28B H 1.3123 0.5077 0.9068 0.087 Uiso 1 1 calc R U . . .
H28C H 1.2085 0.5292 0.8068 0.087 Uiso 1 1 calc R U . . .
O21 O 1.1256(2) 0.68229(18) 0.8784(2) 0.0462(6) Uani 1 1 d . . . . .
O22 O 1.1993(2) 0.8276(2) 0.9125(3) 0.0625(7) Uani 1 1 d . . . . .
N31 N 0.5346(2) 0.95832(17) 0.8758(2) 0.0344(5) Uani 1 1 d . . . . .
C31 C 0.5110(3) 0.8906(2) 0.9488(2) 0.0341(5) Uani 1 1 d . . . . .
H31 H 0.5407 0.8290 0.9373 0.041 Uiso 1 1 calc R U . . .
C32 C 0.4450(2) 0.90641(19) 1.0407(2) 0.0345(6) Uani 1 1 d . . . . .
H32 H 0.4295 0.8568 1.0907 0.041 Uiso 1 1 calc R U . . .
C33 C 0.4024(2) 0.9967(2) 1.0573(2) 0.0339(5) Uani 1 1 d . . . . .
C34 C 0.4320(3) 1.0679(2) 0.9852(3) 0.0385(6) Uani 1 1 d . . . . .
H34 H 0.4072 1.1308 0.9970 0.046 Uiso 1 1 calc R U . . .
C35 C 0.4975(3) 1.0459(2) 0.8966(3) 0.0369(6) Uani 1 1 d . . . . .
H35 H 0.5176 1.0951 0.8478 0.044 Uiso 1 1 calc R U . . .
C36 C 0.3213(3) 1.0204(2) 1.1457(3) 0.0393(6) Uani 1 1 d . . . . .
C37 C 0.2305(4) 0.9677(3) 1.3049(3) 0.0542(8) Uani 1 1 d . . . . .
H37A H 0.2451 1.0325 1.3333 0.065 Uiso 1 1 calc R U . . .
H37B H 0.2523 0.9239 1.3681 0.065 Uiso 1 1 calc R U . . .
C38 C 0.0988(4) 0.9565(3) 1.2660(4) 0.0709(11) Uani 1 1 d . . . . .
H38A H 0.0756 1.0024 1.2064 0.106 Uiso 1 1 calc R U . . .
H38B H 0.0503 0.9672 1.3294 0.106 Uiso 1 1 calc R U . . .
H38C H 0.0840 0.8928 1.2367 0.106 Uiso 1 1 calc R U . . .
O31 O 0.2713(3) 1.09581(17) 1.1498(2) 0.0565(6) Uani 1 1 d . . . . .
O32 O 0.3082(2) 0.94952(14) 1.21596(18) 0.0419(5) Uani 1 1 d . . . . .
N41 N 0.4067(2) 0.97860(18) 0.6544(2) 0.0360(5) Uani 1 1 d . . . . .
C41 C 0.3094(2) 0.9402(2) 0.6959(3) 0.0446(7) Uani 1 1 d . . . . .
H41 H 0.3210 0.8879 0.7454 0.054 Uiso 1 1 calc R U . . .
C42 C 0.1928(3) 0.9744(3) 0.6691(3) 0.0500(8) Uani 1 1 d . . . . .
H42 H 0.1256 0.9461 0.7002 0.060 Uiso 1 1 calc R U . . .
C43 C 0.1750(3) 1.0493(3) 0.5975(3) 0.0455(7) Uani 1 1 d . . . . .
C44 C 0.2750(3) 1.0909(2) 0.5564(3) 0.0412(6) Uani 1 1 d . . . . .
H44 H 0.2656 1.1446 0.5089 0.049 Uiso 1 1 calc R U . . .
C45 C 0.3889(3) 1.0525(2) 0.5860(2) 0.0371(6) Uani 1 1 d . . . . .
H45 H 0.4575 1.0801 0.5564 0.045 Uiso 1 1 calc R U . . .
C46 C 0.0462(4) 1.0792(4) 0.5659(4) 0.0735(13) Uani 1 1 d . . . . .
O41 O -0.0389(7) 1.0550(7) 0.6111(6) 0.080(2) Uani 0.6 1 d D . P A 1
O42 O 0.0322(7) 1.1413(5) 0.4944(9) 0.065(2) Uani 0.6 1 d D . P A 1
C47 C -0.0909(7) 1.1720(7) 0.4602(10) 0.073(3) Uani 0.6 1 d D . P A 1
H47A H -0.1469 1.1420 0.5095 0.088 Uiso 0.6 1 calc R U P A 1
H47B H -0.1145 1.1505 0.3821 0.088 Uiso 0.6 1 calc R U P A 1
C48 C -0.1052(9) 1.2732(7) 0.4652(11) 0.093(3) Uani 0.6 1 d D . P A 1
H48A H -0.0968 1.2936 0.5441 0.140 Uiso 0.6 1 calc R U P A 1
H48B H -0.1860 1.2908 0.4300 0.140 Uiso 0.6 1 calc R U P A 1
H48C H -0.0425 1.3036 0.4251 0.140 Uiso 0.6 1 calc R U P A 1
O41' O -0.0345(9) 1.0125(9) 0.5660(14) 0.092(4) Uani 0.4 1 d D . P A 2
O42' O 0.0495(10) 1.1785(8) 0.5214(11) 0.062(3) Uani 0.4 1 d D . P A 2
C47' C -0.0635(11) 1.2395(12) 0.5091(13) 0.080(4) Uani 0.4 1 d D . P A 2
H47C H -0.1035 1.2412 0.5799 0.096 Uiso 0.4 1 calc R U P A 2
H47D H -0.0441 1.3046 0.4872 0.096 Uiso 0.4 1 calc R U P A 2
C48' C -0.1383(16) 1.1928(15) 0.4210(13) 0.095(5) Uani 0.4 1 d D . P A 2
H48D H -0.0972 1.1934 0.3517 0.143 Uiso 0.4 1 calc R U P A 2
H48E H -0.2166 1.2255 0.4076 0.143 Uiso 0.4 1 calc R U P A 2
H48F H -0.1522 1.1277 0.4432 0.143 Uiso 0.4 1 calc R U 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 N1 2.034(3) . ?
Ni1 N2 2.054(3) . ?
Ni1 N41 2.125(2) . ?
Ni1 N11 2.130(2) . ?
Ni1 N21 2.144(2) . ?
Ni1 N31 2.148(2) . ?
N1 C1 1.154(4) . ?
C1 S1 1.624(3) . ?
N2 C2 1.163(4) . ?
C2 S2 1.622(3) . ?
N11 C15 1.334(4) . ?
N11 C11 1.346(4) . ?
C11 C12 1.377(5) . ?
C12 C13 1.385(4) . ?
C13 C14 1.392(4) . ?
C13 C16 1.492(4) . ?
C14 C15 1.386(4) . ?
C16 O11 1.206(4) . ?
C16 O12 1.334(4) . ?
C17 O12 1.458(4) . ?
C17 C18 1.485(7) . ?
N21 C21 1.336(4) . ?
N21 C25 1.342(4) . ?
C21 C22 1.382(4) . ?
C22 C23 1.377(4) . ?
C23 C24 1.382(4) . ?
C23 C26 1.495(4) . ?
C24 C25 1.380(4) . ?
C26 O22 1.205(4) . ?
C26 O21 1.325(4) . ?
C27 O21 1.462(4) . ?
C27 C28 1.492(5) . ?
N31 C31 1.341(4) . ?
N31 C35 1.342(4) . ?
C31 C32 1.392(4) . ?
C32 C33 1.388(4) . ?
C33 C34 1.387(4) . ?
C33 C36 1.487(4) . ?
C34 C35 1.374(4) . ?
C36 O31 1.209(4) . ?
C36 O32 1.327(4) . ?
C37 O32 1.451(4) . ?
C37 C38 1.489(6) . ?
N41 C45 1.333(4) . ?
N41 C41 1.341(4) . ?
C41 C42 1.383(4) . ?
C42 C43 1.366(5) . ?
C43 C44 1.384(5) . ?
C43 C46 1.496(5) . ?
C44 C45 1.385(4) . ?
C46 O41 1.178(9) . ?
C46 O42 1.226(10) . ?
C46 O41' 1.301(13) . ?
C46 O42' 1.511(13) . ?
O42 C47 1.447(9) . ?
C47 C48 1.450(12) . ?
O42' C47' 1.514(15) . ?
C47' C48' 1.434(17) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N2 177.62(11) . . ?
N1 Ni1 N41 90.25(10) . . ?
N2 Ni1 N41 90.29(10) . . ?
N1 Ni1 N11 89.91(10) . . ?
N2 Ni1 N11 87.75(10) . . ?
N41 Ni1 N11 91.61(9) . . ?
N1 Ni1 N21 88.88(10) . . ?
N2 Ni1 N21 90.68(10) . . ?
N41 Ni1 N21 177.13(10) . . ?
N11 Ni1 N21 91.12(9) . . ?
N1 Ni1 N31 91.36(10) . . ?
N2 Ni1 N31 91.00(10) . . ?
N41 Ni1 N31 84.88(9) . . ?
N11 Ni1 N31 176.28(9) . . ?
N21 Ni1 N31 92.40(9) . . ?
C1 N1 Ni1 158.8(3) . . ?
N1 C1 S1 176.8(3) . . ?
C2 N2 Ni1 161.1(3) . . ?
N2 C2 S2 179.6(3) . . ?
C15 N11 C11 117.8(3) . . ?
C15 N11 Ni1 119.72(19) . . ?
C11 N11 Ni1 122.2(2) . . ?
N11 C11 C12 123.1(3) . . ?
C11 C12 C13 118.8(3) . . ?
C12 C13 C14 118.5(3) . . ?
C12 C13 C16 119.1(3) . . ?
C14 C13 C16 122.4(3) . . ?
C15 C14 C13 118.7(3) . . ?
N11 C15 C14 122.9(3) . . ?
O11 C16 O12 124.7(3) . . ?
O11 C16 C13 122.9(3) . . ?
O12 C16 C13 112.4(3) . . ?
O12 C17 C18 112.0(3) . . ?
C16 O12 C17 116.4(3) . . ?
C21 N21 C25 117.6(3) . . ?
C21 N21 Ni1 120.3(2) . . ?
C25 N21 Ni1 122.1(2) . . ?
N21 C21 C22 123.1(3) . . ?
C23 C22 C21 119.0(3) . . ?
C22 C23 C24 118.3(3) . . ?
C22 C23 C26 122.2(3) . . ?
C24 C23 C26 119.5(3) . . ?
C25 C24 C23 119.4(3) . . ?
N21 C25 C24 122.5(3) . . ?
O22 C26 O21 124.8(3) . . ?
O22 C26 C23 123.4(3) . . ?
O21 C26 C23 111.8(3) . . ?
O21 C27 C28 106.3(3) . . ?
C26 O21 C27 117.2(3) . . ?
C31 N31 C35 117.6(2) . . ?
C31 N31 Ni1 121.37(19) . . ?
C35 N31 Ni1 118.8(2) . . ?
N31 C31 C32 123.1(3) . . ?
C33 C32 C31 118.1(3) . . ?
C34 C33 C32 118.9(3) . . ?
C34 C33 C36 117.9(3) . . ?
C32 C33 C36 123.1(3) . . ?
C35 C34 C33 119.0(3) . . ?
N31 C35 C34 123.1(3) . . ?
O31 C36 O32 124.8(3) . . ?
O31 C36 C33 122.5(3) . . ?
O32 C36 C33 112.7(2) . . ?
O32 C37 C38 112.5(3) . . ?
C36 O32 C37 115.7(2) . . ?
C45 N41 C41 118.1(3) . . ?
C45 N41 Ni1 123.2(2) . . ?
C41 N41 Ni1 118.5(2) . . ?
N41 C41 C42 122.1(3) . . ?
C43 C42 C41 119.4(3) . . ?
C42 C43 C44 119.0(3) . . ?
C42 C43 C46 117.0(3) . . ?
C44 C43 C46 124.0(3) . . ?
C43 C44 C45 118.4(3) . . ?
N41 C45 C44 122.9(3) . . ?
O41 C46 O42 118.5(6) . . ?
O41 C46 C43 125.5(5) . . ?
O42 C46 C43 115.6(5) . . ?
O41' C46 C43 115.2(7) . . ?
O41' C46 O42' 136.2(8) . . ?
C43 C46 O42' 107.4(5) . . ?
C46 O42 C47 117.6(8) . . ?
O42 C47 C48 113.0(9) . . ?
C46 O42' C47' 121.5(11) . . ?
C48' C47' O42' 102.4(15) . . ?

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
C12 H12 S1 0.95 3.00 3.871(3) 153.7 2_646
C15 H15 O41 0.95 2.54 3.439(10) 158.2 1_655
C15 H15 O41' 0.95 2.22 3.032(11) 142.9 1_655
C21 H21 N2 0.95 2.52 3.069(4) 116.6 .
C25 H25 N1 0.95 2.56 3.043(4) 112.0 .
C34 H34 O11 0.95 2.54 3.177(4) 124.8 2_656
C35 H35 N1 0.95 2.56 3.122(4) 117.8 .
C38 H38C S1 0.98 2.96 3.673(5) 130.9 2_647
C41 H41 N2 0.95 2.54 3.053(4) 114.1 .
C41 H41 O22 0.95 2.65 3.365(4) 132.3 1_455
C45 H45 N1 0.95 2.62 3.094(4) 110.9 .
C45 H45 S2 0.95 2.98 3.768(3) 140.7 2_656
C47' H47C S1 0.99 2.83 3.809(16) 170.8 1_455
C48' H48E S2 0.98 3.00 3.559(16) 117.7 2_556
C48' H48F O41' 0.98 2.48 3.24(2) 134.3 .

_refine_diff_density_max         0.269
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.038

_shelxl_version_number           2014-3

####################################################################### 
# 
# 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_jw1783neu
_database_code_depnum_ccdc_archive 'CCDC 1506856'
_audit_update_record             
;
2016-09-27 deposited with the CCDC.
2016-10-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H18 N4 Ni O4 S2'
_chemical_formula_sum            'C18 H18 N4 Ni O4 S2'
_chemical_formula_weight         477.19

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'
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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   14.8063(9)
_cell_length_b                   9.5965(3)
_cell_length_c                   15.7820(8)
_cell_angle_alpha                90
_cell_angle_beta                 113.010(4)
_cell_angle_gamma                90
_cell_volume                     2064.03(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    29475
_cell_measurement_theta_min      1.494
_cell_measurement_theta_max      27.242

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_F_000             984
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.1600
_exptl_crystal_size_mid          0.1142
_exptl_crystal_size_min          0.0617
_exptl_absorpt_coefficient_mu    1.175
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.832
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_process_details   'X-Shape and X-Red 32 (STOE, 2008)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS-2'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29475
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_av_R_equivalents  0.0741
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.494
_diffrn_reflns_theta_max         27.242
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4603
_reflns_number_gt                3878
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0456P)²+1.7354P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0048(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4603
_refine_ls_number_parameters     353
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0497
_refine_ls_wR_factor_ref         0.1162
_refine_ls_wR_factor_gt          0.1100
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.50519(3) 0.83105(4) 0.35666(3) 0.04297(14) Uani 1 1 d . . . . .
N1 N 0.5296(2) 0.9751(2) 0.61158(17) 0.0470(6) Uani 1 1 d . . . . .
C1 C 0.5622(2) 0.8963(3) 0.57676(19) 0.0426(6) Uani 1 1 d . . . . .
S1 S 0.61108(7) 0.78629(8) 0.52642(6) 0.0535(2) Uani 1 1 d . . . . .
N2 N 0.4578(2) 1.1333(2) 0.16571(19) 0.0511(7) Uani 1 1 d . . . . .
C2 C 0.4349(3) 1.0217(3) 0.1759(2) 0.0462(7) Uani 1 1 d . . . . .
S2 S 0.40348(8) 0.86159(7) 0.18964(6) 0.0536(2) Uani 1 1 d . . . . .
N11 N 0.3806(2) 0.7518(3) 0.37579(18) 0.0498(6) Uani 1 1 d . . . . .
C11 C 0.2924(5) 0.8248(9) 0.3411(5) 0.0460(16) Uani 0.75 1 d D . P A 1
H11 H 0.2880 0.9045 0.3039 0.055 Uiso 0.75 1 calc R U P A 1
C12 C 0.2112(5) 0.7873(7) 0.3580(4) 0.0514(15) Uani 0.75 1 d D . P A 1
H12 H 0.1533 0.8425 0.3355 0.062 Uiso 0.75 1 calc R U P A 1
C13 C 0.2153(5) 0.6678(8) 0.4083(5) 0.0538(17) Uani 0.75 1 d D . P A 1
C14 C 0.3001(6) 0.5886(9) 0.4373(5) 0.0508(18) Uani 0.75 1 d D . P A 1
H14 H 0.3048 0.5051 0.4712 0.061 Uiso 0.75 1 calc R U P A 1
C15 C 0.3785(5) 0.6328(10) 0.4162(5) 0.0452(19) Uani 0.75 1 d D . P A 1
H15 H 0.4339 0.5732 0.4320 0.054 Uiso 0.75 1 calc R U P A 1
C16 C 0.1285(5) 0.6188(6) 0.4280(4) 0.0597(13) Uani 0.75 1 d D . P A 1
O11 O 0.1299(4) 0.5110(4) 0.4677(3) 0.0815(12) Uani 0.75 1 d D . P A 1
O12 O 0.0539(3) 0.7072(4) 0.3975(3) 0.0756(11) Uani 0.75 1 d D . P A 1
C17 C -0.0347(5) 0.6735(7) 0.4123(5) 0.0849(18) Uani 0.75 1 d D . P A 1
H17A H -0.0677 0.7616 0.4159 0.102 Uiso 0.75 1 calc R U P A 1
H17B H -0.0154 0.6261 0.4725 0.102 Uiso 0.75 1 calc R U P A 1
C18 C -0.1066(5) 0.5836(8) 0.3405(5) 0.095(2) Uani 0.75 1 d D . P A 1
H18A H -0.1635 0.5666 0.3562 0.143 Uiso 0.75 1 calc R U P A 1
H18B H -0.1280 0.6304 0.2806 0.143 Uiso 0.75 1 calc R U P A 1
H18C H -0.0756 0.4945 0.3374 0.143 Uiso 0.75 1 calc R U P A 1
C11' C 0.3095(16) 0.819(2) 0.3706(10) 0.039(5) Uani 0.25 1 d D . P A 2
H11' H 0.3043 0.9125 0.3491 0.047 Uiso 0.25 1 calc R U P A 2
C12' C 0.2352(13) 0.7668(19) 0.3947(12) 0.045(4) Uani 0.25 1 d D . P A 2
H12' H 0.1755 0.8166 0.3801 0.054 Uiso 0.25 1 calc R U P A 2
C13' C 0.2503(13) 0.6409(18) 0.4401(14) 0.044(4) Uani 0.25 1 d D . P A 2
C14' C 0.3372(13) 0.571(2) 0.4618(14) 0.043(5) Uani 0.25 1 d D . P A 2
H14' H 0.3478 0.4840 0.4924 0.052 Uiso 0.25 1 calc R U P A 2
C15' C 0.4094(14) 0.631(3) 0.4383(14) 0.039(5) Uani 0.25 1 d D . P A 2
H15' H 0.4745 0.5960 0.4614 0.046 Uiso 0.25 1 calc R U P A 2
C16' C 0.1747(9) 0.5925(13) 0.4756(10) 0.052(4) Uani 0.25 1 d D . P A 2
O11' O 0.0998(8) 0.6530(12) 0.4647(9) 0.066(3) Uani 0.25 1 d D . P A 2
O12' O 0.2013(7) 0.4703(11) 0.5183(6) 0.056(2) Uani 0.25 1 d D . P A 2
C17' C 0.1349(13) 0.411(2) 0.5567(10) 0.088(7) Uani 0.25 1 d D . P A 2
H17C H 0.0668 0.4413 0.5202 0.106 Uiso 0.25 1 calc R U P A 2
H17D H 0.1371 0.3078 0.5546 0.106 Uiso 0.25 1 calc R U P A 2
C18' C 0.1644(13) 0.457(2) 0.6502(10) 0.091(7) Uani 0.25 1 d D . P A 2
H18D H 0.1201 0.4169 0.6766 0.137 Uiso 0.25 1 calc R U P A 2
H18E H 0.2316 0.4254 0.6862 0.137 Uiso 0.25 1 calc R U P A 2
H18F H 0.1615 0.5585 0.6519 0.137 Uiso 0.25 1 calc R U P A 2
N21 N 0.6283(2) 0.9101(2) 0.33754(18) 0.0472(6) Uani 1 1 d . . . . .
C21 C 0.6581(3) 0.8523(3) 0.2756(2) 0.0539(8) Uani 1 1 d . . . . .
H21 H 0.6207 0.7778 0.2389 0.065 Uiso 1 1 calc R U . . .
C22 C 0.7403(3) 0.8959(4) 0.2627(2) 0.0563(8) Uani 1 1 d . . . . .
H22 H 0.7591 0.8518 0.2182 0.068 Uiso 1 1 calc R U . . .
C23 C 0.7955(3) 1.0049(3) 0.3152(2) 0.0535(8) Uani 1 1 d . . . . .
C24 C 0.7633(3) 1.0681(3) 0.3772(3) 0.0565(8) Uani 1 1 d . . . . .
H24 H 0.7980 1.1452 0.4129 0.068 Uiso 1 1 calc R U . . .
C25 C 0.6806(3) 1.0178(3) 0.3866(2) 0.0528(8) Uani 1 1 d . . . . .
H25 H 0.6596 1.0614 0.4298 0.063 Uiso 1 1 calc R U . . .
C26 C 0.8870(3) 1.0470(4) 0.3038(3) 0.0640(9) Uani 1 1 d . . . . .
C27 C 1.0190(3) 1.2083(5) 0.3454(4) 0.0932(16) Uani 1 1 d . . . . .
H27A H 1.0284 1.3088 0.3606 0.112 Uiso 1 1 calc R U . . .
H27B H 1.0142 1.1962 0.2815 0.112 Uiso 1 1 calc R U . . .
C28 C 1.1046(4) 1.1291(7) 0.4091(5) 0.124(2) Uani 1 1 d . . . . .
H28A H 1.1645 1.1628 0.4035 0.186 Uiso 1 1 calc R U . . .
H28B H 1.1101 1.1423 0.4725 0.186 Uiso 1 1 calc R U . . .
H28C H 1.0958 1.0298 0.3935 0.186 Uiso 1 1 calc R U . . .
O21 O 0.9198(2) 0.9835(3) 0.2563(2) 0.0801(9) Uani 1 1 d . . . . .
O22 O 0.9281(2) 1.1608(3) 0.3519(2) 0.0746(8) 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
Ni1 N2 2.043(2) 2_645 ?
Ni1 N1 2.045(2) 3_676 ?
Ni1 N21 2.102(3) . ?
Ni1 N11 2.124(3) . ?
Ni1 S2 2.4896(10) . ?
Ni1 S1 2.5568(10) . ?
N1 C1 1.146(4) . ?
N1 Ni1 2.045(2) 3_676 ?
C1 S1 1.649(3) . ?
N2 C2 1.154(4) . ?
N2 Ni1 2.043(2) 2_655 ?
C2 S2 1.644(3) . ?
N11 C11' 1.21(3) . ?
N11 C15 1.315(9) . ?
N11 C11 1.391(8) . ?
N11 C15' 1.47(2) . ?
C11 C12 1.379(8) . ?
C12 C13 1.382(8) . ?
C13 C14 1.383(9) . ?
C13 C16 1.511(8) . ?
C14 C15 1.393(8) . ?
C16 O11 1.206(6) . ?
C16 O12 1.325(7) . ?
O12 C17 1.455(7) . ?
C17 C18 1.489(9) . ?
C11' C12' 1.391(15) . ?
C12' C13' 1.378(15) . ?
C13' C14' 1.368(16) . ?
C13' C16' 1.507(13) . ?
C14' C15' 1.386(16) . ?
C16' O11' 1.203(14) . ?
C16' O12' 1.333(14) . ?
O12' C17' 1.458(12) . ?
C17' C18' 1.434(16) . ?
N21 C21 1.341(4) . ?
N21 C25 1.341(4) . ?
C21 C22 1.376(5) . ?
C22 C23 1.385(5) . ?
C23 C24 1.384(5) . ?
C23 C26 1.490(5) . ?
C24 C25 1.378(5) . ?
C26 O21 1.206(5) . ?
C26 O22 1.333(5) . ?
C27 O22 1.463(5) . ?
C27 C28 1.483(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ni1 N1 175.97(10) 2_645 3_676 ?
N2 Ni1 N21 90.26(11) 2_645 . ?
N1 Ni1 N21 91.29(10) 3_676 . ?
N2 Ni1 N11 89.93(11) 2_645 . ?
N1 Ni1 N11 88.54(11) 3_676 . ?
N21 Ni1 N11 179.79(11) . . ?
N2 Ni1 S2 91.06(8) 2_645 . ?
N1 Ni1 S2 92.66(8) 3_676 . ?
N21 Ni1 S2 90.29(8) . . ?
N11 Ni1 S2 89.60(8) . . ?
N2 Ni1 S1 85.93(8) 2_645 . ?
N1 Ni1 S1 90.35(8) 3_676 . ?
N21 Ni1 S1 90.01(8) . . ?
N11 Ni1 S1 90.11(8) . . ?
S2 Ni1 S1 176.98(3) . . ?
C1 N1 Ni1 155.7(2) . 3_676 ?
N1 C1 S1 178.4(3) . . ?
C1 S1 Ni1 101.10(11) . . ?
C2 N2 Ni1 178.1(3) . 2_655 ?
N2 C2 S2 179.0(3) . . ?
C2 S2 Ni1 99.47(12) . . ?
C15 N11 C11 115.6(5) . . ?
C11' N11 C15' 118.8(11) . . ?
C11' N11 Ni1 125.5(9) . . ?
C15 N11 Ni1 124.5(4) . . ?
C11 N11 Ni1 119.8(3) . . ?
C15' N11 Ni1 109.7(8) . . ?
C12 C11 N11 123.2(6) . . ?
C11 C12 C13 118.8(6) . . ?
C12 C13 C14 118.5(6) . . ?
C12 C13 C16 121.7(6) . . ?
C14 C13 C16 119.7(6) . . ?
C13 C14 C15 119.1(6) . . ?
N11 C15 C14 124.1(8) . . ?
O11 C16 O12 125.4(6) . . ?
O11 C16 C13 122.1(6) . . ?
O12 C16 C13 112.5(5) . . ?
C16 O12 C17 118.4(5) . . ?
O12 C17 C18 115.4(6) . . ?
N11 C11' C12' 123.3(17) . . ?
C13' C12' C11' 118.3(15) . . ?
C14' C13' C12' 120.2(13) . . ?
C14' C13' C16' 121.3(14) . . ?
C12' C13' C16' 118.0(15) . . ?
C13' C14' C15' 118.6(17) . . ?
C14' C15' N11 117.0(16) . . ?
O11' C16' O12' 124.8(11) . . ?
O11' C16' C13' 125.1(12) . . ?
O12' C16' C13' 110.1(11) . . ?
C16' O12' C17' 116.2(12) . . ?
C18' C17' O12' 109.0(10) . . ?
C21 N21 C25 117.4(3) . . ?
C21 N21 Ni1 120.5(2) . . ?
C25 N21 Ni1 122.2(2) . . ?
N21 C21 C22 123.0(3) . . ?
C21 C22 C23 119.3(3) . . ?
C24 C23 C22 118.0(3) . . ?
C24 C23 C26 123.1(3) . . ?
C22 C23 C26 118.9(3) . . ?
C25 C24 C23 119.3(3) . . ?
N21 C25 C24 123.0(3) . . ?
O21 C26 O22 124.3(4) . . ?
O21 C26 C23 122.9(4) . . ?
O22 C26 C23 112.8(3) . . ?
O22 C27 C28 111.0(5) . . ?
C26 O22 C27 116.3(4) . . ?

_refine_diff_density_max         0.391
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.064

_shelxl_version_number           2014-3

