# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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/. 
# 
# Audit and citation data items have may 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 980827'
_audit_update_record             
;
2014-01-09 deposited with the CCDC.
2014-11-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C56 H36 Cl6 N6 Ni S'
_chemical_formula_weight         1096.38

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.0020(9)
_cell_length_b                   14.6553(10)
_cell_length_c                   15.1609(13)
_cell_angle_alpha                79.909(6)
_cell_angle_beta                 70.047(7)
_cell_angle_gamma                81.089(6)
_cell_volume                     2454.8(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    7539
_cell_measurement_theta_min      3.0037
_cell_measurement_theta_max      29.7437

_exptl_crystal_description       ORTHORHOMBIC
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1120
_exptl_absorpt_coefficient_mu    0.811
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_correction_T_min  0.7929
_exptl_absorpt_correction_T_max  0.8546
_exptl_absorpt_process_details   'CrysAlisPro 1.171.34.40 (2006)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Sapphire-3 CCD detector'
_diffrn_measurement_method       'OMEGA SCAN'
_diffrn_detector_area_resol_mean 15.9853
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            34800
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0345
_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       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         26.37
_reflns_number_total             10014
_reflns_number_gt                8306
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_cell_refinement       'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_structure_solution    SIR-92
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  'WINGX V1.80.01'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1616P)²+4.4066P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10014
_refine_ls_number_parameters     631
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0844
_refine_ls_wR_factor_ref         0.2611
_refine_ls_wR_factor_gt          0.2479
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.003
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.35152(4) 0.16453(3) 0.13155(3) 0.03187(19) Uani 1 1 d . . .
S1 S 0.70446(18) 0.04867(14) 0.51870(14) 0.0853(5) Uani 1 1 d . . .
Cl2 Cl 0.8457(4) 0.2780(3) 0.1460(2) 0.1613(13) Uani 1 1 d . . .
Cl1 Cl 0.7891(3) 0.34579(19) 0.3207(2) 0.1213(8) Uani 1 1 d . . .
N2 N 0.2595(3) 0.1307(2) 0.0629(2) 0.0342(7) Uani 1 1 d . . .
N3 N 0.4122(3) 0.0365(2) 0.1517(3) 0.0363(7) Uani 1 1 d . . .
N1 N 0.3113(3) 0.2941(2) 0.0948(2) 0.0354(7) Uani 1 1 d . . .
N4 N 0.4279(3) 0.1967(2) 0.2142(2) 0.0363(7) Uani 1 1 d . . .
N6 N 0.4358(3) 0.3196(3) 0.4029(3) 0.0440(8) Uani 1 1 d . . .
Cl4 Cl 0.8828(5) 0.4251(3) 0.4911(3) 0.1964(18) Uani 1 1 d . . .
N5 N 0.5788(4) 0.1469(3) 0.3913(3) 0.0500(9) Uani 1 1 d . . .
Cl3 Cl 0.9964(4) 0.2189(4) 0.2538(4) 0.237(3) Uani 1 1 d . . .
C3 C 0.4500(4) 0.2676(3) 0.3303(3) 0.0396(9) Uani 1 1 d . . .
Cl5 Cl 1.0052(7) 0.3048(4) 0.5919(5) 0.289(4) Uani 1 1 d . . .
C14 C 0.2304(4) 0.0426(3) 0.0638(3) 0.0361(8) Uani 1 1 d . . .
C15 C 0.2908(4) -0.0398(3) 0.0913(3) 0.0366(8) Uani 1 1 d . . .
C10 C 0.2124(4) 0.2832(3) -0.0200(3) 0.0391(9) Uani 1 1 d . . .
C16 C 0.3857(4) -0.0398(3) 0.1241(3) 0.0377(9) Uani 1 1 d . . .
C8 C 0.2870(4) 0.4275(3) -0.0045(3) 0.0429(10) Uani 1 1 d . . .
H8 H 0.2697 0.4672 -0.0541 0.051 Uiso 1 1 calc R . .
C19 C 0.5081(4) 0.0034(3) 0.1840(3) 0.0402(9) Uani 1 1 d . . .
C20 C 0.5510(4) 0.0507(3) 0.2346(3) 0.0418(9) Uani 1 1 d . . .
C9 C 0.2697(4) 0.3314(3) 0.0198(3) 0.0377(9) Uani 1 1 d . . .
C13 C 0.1454(4) 0.0482(3) 0.0152(4) 0.0452(10) Uani 1 1 d . . .
H13 H 0.1088 -0.0009 0.0094 0.054 Uiso 1 1 calc R . .
C40 C 0.1556(4) -0.1657(3) 0.1369(4) 0.0487(11) Uani 1 1 d . . .
H40 H 0.1035 -0.1327 0.1845 0.058 Uiso 1 1 calc R . .
C39 C 0.2611(4) -0.1300(3) 0.0781(3) 0.0396(9) Uani 1 1 d . . .
C37 C 0.1638(5) 0.3580(4) -0.2561(4) 0.0556(12) Uani 1 1 d . . .
H37 H 0.1935 0.3407 -0.3167 0.067 Uiso 1 1 calc R . .
C45 C 0.5733(4) 0.2001(4) 0.4547(3) 0.0494(11) Uani 1 1 d . . .
Cl6 Cl 1.0990(4) 0.3476(6) 0.3852(5) 0.346(5) Uani 1 1 d . . .
C1 C 0.5008(4) 0.1379(3) 0.2578(3) 0.0387(9) Uani 1 1 d . . .
C33 C 0.1636(4) 0.3337(3) -0.0952(3) 0.0388(9) Uani 1 1 d . . .
C4 C 0.4078(4) 0.2817(3) 0.2501(3) 0.0367(8) Uani 1 1 d . . .
C27 C 0.4066(5) 0.4557(3) 0.2193(3) 0.0465(11) Uani 1 1 d . . .
C44 C 0.3363(5) -0.1806(3) 0.0085(4) 0.0527(12) Uani 1 1 d . . .
H44 H 0.4059 -0.1569 -0.0325 0.063 Uiso 1 1 calc R . .
C21 C 0.6553(4) 0.0029(3) 0.2642(3) 0.0458(10) Uani 1 1 d . . .
C2 C 0.5145(4) 0.1825(3) 0.3313(3) 0.0414(9) Uani 1 1 d . . .
C54 C 0.3642(5) 0.3981(4) 0.4313(3) 0.0526(11) Uani 1 1 d . . .
H54 H 0.3122 0.4332 0.4018 0.063 Uiso 1 1 calc R . .
C22 C 0.6437(5) -0.0725(4) 0.3322(5) 0.0656(15) Uani 1 1 d . . .
H22 H 0.5695 -0.0943 0.3631 0.079 Uiso 1 1 calc R . .
C38 C 0.2062(4) 0.3091(3) -0.1856(3) 0.0467(10) Uani 1 1 d . . .
H38 H 0.2642 0.2589 -0.1992 0.056 Uiso 1 1 calc R . .
C11 C 0.1994(4) 0.1891(3) 0.0077(3) 0.0370(9) Uani 1 1 d . . .
C5 C 0.3808(4) 0.3654(3) 0.1994(3) 0.0386(9) Uani 1 1 d . . .
C7 C 0.3327(5) 0.4505(3) 0.0565(3) 0.0457(10) Uani 1 1 d . . .
H7 H 0.3526 0.5092 0.0572 0.055 Uiso 1 1 calc R . .
C18 C 0.5460(5) -0.0910(3) 0.1682(4) 0.0519(12) Uani 1 1 d . . .
H18 H 0.6127 -0.1266 0.1785 0.062 Uiso 1 1 calc R . .
C34 C 0.0740(5) 0.4070(3) -0.0763(4) 0.0502(11) Uani 1 1 d . . .
H34 H 0.0416 0.4231 -0.0153 0.060 Uiso 1 1 calc R . .
C51 C 0.4989(4) 0.2857(4) 0.4668(3) 0.0506(11) Uani 1 1 d . . .
C6 C 0.3455(4) 0.3684(3) 0.1208(3) 0.0385(9) Uani 1 1 d . . .
C32 C 0.3227(6) 0.5323(3) 0.2310(4) 0.0605(14) Uani 1 1 d . . .
H32 H 0.2463 0.5284 0.2306 0.073 Uiso 1 1 calc R . .
C43 C 0.3098(6) -0.2672(4) -0.0015(5) 0.0642(14) Uani 1 1 d . . .
H43 H 0.3628 -0.3022 -0.0469 0.077 Uiso 1 1 calc R . .
C41 C 0.1282(5) -0.2502(4) 0.1248(4) 0.0599(14) Uani 1 1 d . . .
H41 H 0.0570 -0.2730 0.1636 0.072 Uiso 1 1 calc R . .
C28 C 0.5198(5) 0.4619(4) 0.2225(3) 0.0529(12) Uani 1 1 d . . .
H28 H 0.5768 0.4106 0.2145 0.064 Uiso 1 1 calc R . .
C26 C 0.7656(5) 0.0334(4) 0.2190(4) 0.0562(12) Uani 1 1 d . . .
H26 H 0.7746 0.0842 0.1718 0.067 Uiso 1 1 calc R . .
C35 C 0.0325(6) 0.4564(3) -0.1476(4) 0.0613(14) Uani 1 1 d . . .
H35 H -0.0263 0.5062 -0.1348 0.074 Uiso 1 1 calc R . .
C12 C 0.1287(4) 0.1377(3) -0.0203(3) 0.0445(10) Uani 1 1 d . . .
H12 H 0.0797 0.1619 -0.0566 0.053 Uiso 1 1 calc R . .
C53 C 0.3819(6) 0.4161(4) 0.5105(4) 0.0630(14) Uani 1 1 d . . .
H53 H 0.3447 0.4660 0.5439 0.076 Uiso 1 1 calc R . .
C42 C 0.2042(6) -0.2997(3) 0.0568(5) 0.0655(16) Uani 1 1 d . . .
H42 H 0.1848 -0.3564 0.0496 0.079 Uiso 1 1 calc R . .
C24 C 0.8505(6) -0.0858(5) 0.3124(5) 0.0759(18) Uani 1 1 d . . .
H24 H 0.9161 -0.1150 0.3294 0.091 Uiso 1 1 calc R . .
C36 C 0.0787(6) 0.4314(4) -0.2372(4) 0.0614(14) Uani 1 1 d . . .
H36 H 0.0516 0.4649 -0.2853 0.074 Uiso 1 1 calc R . .
C17 C 0.4678(5) -0.1194(3) 0.1354(4) 0.0505(11) Uani 1 1 d . . .
H17 H 0.4672 -0.1791 0.1226 0.061 Uiso 1 1 calc R . .
C23 C 0.7440(6) -0.1173(4) 0.3558(5) 0.0749(18) Uani 1 1 d . . .
H23 H 0.7361 -0.1692 0.4017 0.090 Uiso 1 1 calc R . .
C30 C 0.4658(8) 0.6215(4) 0.2466(4) 0.080(2) Uani 1 1 d . . .
H30 H 0.4860 0.6775 0.2547 0.096 Uiso 1 1 calc R . .
C25 C 0.8636(5) -0.0107(5) 0.2432(5) 0.0728(17) Uani 1 1 d . . .
H25 H 0.9382 0.0106 0.2126 0.087 Uiso 1 1 calc R . .
C46 C 0.6468(5) 0.1629(4) 0.5158(4) 0.0608(14) Uani 1 1 d . . .
C31 C 0.3544(7) 0.6166(4) 0.2436(4) 0.0763(19) Uani 1 1 d . . .
H31 H 0.2992 0.6691 0.2499 0.092 Uiso 1 1 calc R . .
C29 C 0.5468(6) 0.5460(4) 0.2379(4) 0.0693(17) Uani 1 1 d . . .
H29 H 0.6213 0.5498 0.2423 0.083 Uiso 1 1 calc R . .
C48 C 0.7549(7) 0.1480(7) 0.6195(5) 0.093(2) Uani 1 1 d . . .
H48 H 0.7853 0.1679 0.6609 0.111 Uiso 1 1 calc R . .
C52 C 0.4650(6) 0.3471(5) 0.5329(4) 0.0678(16) Uani 1 1 d . . .
H52 H 0.4929 0.3430 0.5837 0.081 Uiso 1 1 calc R . .
C47 C 0.6841(7) 0.2051(5) 0.5732(5) 0.0815(19) Uani 1 1 d . . .
H47 H 0.6631 0.2679 0.5803 0.098 Uiso 1 1 calc R . .
C49 C 0.7755(7) 0.0592(7) 0.5982(5) 0.095(3) Uani 1 1 d . . .
C50 C 0.8466(9) -0.0213(8) 0.6352(6) 0.138(4) Uani 1 1 d . . .
H50A H 0.8463 -0.0753 0.6075 0.207 Uiso 1 1 calc R . .
H50B H 0.8123 -0.0336 0.7027 0.207 Uiso 1 1 calc R . .
H50C H 0.9271 -0.0070 0.6192 0.207 Uiso 1 1 calc R . .
C55 C 0.8533(8) 0.2520(7) 0.2603(6) 0.099(2) Uani 1 1 d . . .
H55 H 0.8071 0.1992 0.2924 0.119 Uiso 1 1 calc R . .
C56 C 0.9839(11) 0.3237(8) 0.4819(10) 0.139(4) Uani 1 1 d . . .
H56 H 0.9465 0.2718 0.4747 0.167 Uiso 1 1 calc R . .


_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 N3 1.916(3) . ?
Ni1 N1 1.917(3) . ?
Ni1 N2 1.919(3) . ?
Ni1 N4 1.937(3) . ?
S1 C46 1.709(6) . ?
S1 C49 1.734(8) . ?
Cl2 C55 1.739(9) . ?
Cl1 C55 1.719(9) . ?
N2 C14 1.385(5) . ?
N2 C11 1.387(5) . ?
N3 C16 1.375(5) . ?
N3 C19 1.388(5) . ?
N1 C6 1.383(5) . ?
N1 C9 1.387(5) . ?
N4 C1 1.381(5) . ?
N4 C4 1.401(5) . ?
N6 C54 1.365(6) . ?
N6 C3 1.395(5) . ?
N6 C51 1.406(6) . ?
Cl4 C56 1.760(12) . ?
N5 C45 1.318(6) . ?
N5 C2 1.372(6) . ?
Cl3 C55 1.684(10) . ?
C3 C2 1.362(6) . ?
C3 C4 1.442(6) . ?
Cl5 C56 1.740(13) . ?
C14 C15 1.385(5) . ?
C14 C13 1.435(6) . ?
C15 C16 1.390(6) . ?
C15 C39 1.483(5) . ?
C10 C9 1.385(6) . ?
C10 C11 1.386(6) . ?
C10 C33 1.489(6) . ?
C16 C17 1.431(6) . ?
C8 C7 1.335(6) . ?
C8 C9 1.420(6) . ?
C8 H8 0.9300 . ?
C19 C20 1.379(6) . ?
C19 C18 1.423(6) . ?
C20 C1 1.376(6) . ?
C20 C21 1.503(6) . ?
C13 C12 1.339(6) . ?
C13 H13 0.9300 . ?
C40 C41 1.387(7) . ?
C40 C39 1.394(6) . ?
C40 H40 0.9300 . ?
C39 C44 1.376(7) . ?
C37 C36 1.361(8) . ?
C37 C38 1.380(7) . ?
C37 H37 0.9300 . ?
C45 C51 1.424(7) . ?
C45 C46 1.471(7) . ?
Cl6 C56 1.663(14) . ?
C1 C2 1.454(6) . ?
C33 C38 1.382(6) . ?
C33 C34 1.390(6) . ?
C4 C5 1.385(6) . ?
C27 C32 1.381(7) . ?
C27 C28 1.393(7) . ?
C27 C5 1.505(6) . ?
C44 C43 1.400(7) . ?
C44 H44 0.9300 . ?
C21 C22 1.362(7) . ?
C21 C26 1.371(7) . ?
C54 C53 1.364(7) . ?
C54 H54 0.9300 . ?
C22 C23 1.404(8) . ?
C22 H22 0.9300 . ?
C38 H38 0.9300 . ?
C11 C12 1.422(6) . ?
C5 C6 1.386(6) . ?
C7 C6 1.433(6) . ?
C7 H7 0.9300 . ?
C18 C17 1.346(7) . ?
C18 H18 0.9300 . ?
C34 C35 1.386(7) . ?
C34 H34 0.9300 . ?
C51 C52 1.380(7) . ?
C32 C31 1.408(8) . ?
C32 H32 0.9300 . ?
C43 C42 1.375(9) . ?
C43 H43 0.9300 . ?
C41 C42 1.356(9) . ?
C41 H41 0.9300 . ?
C28 C29 1.398(7) . ?
C28 H28 0.9300 . ?
C26 C25 1.382(7) . ?
C26 H26 0.9300 . ?
C35 C36 1.372(8) . ?
C35 H35 0.9300 . ?
C12 H12 0.9300 . ?
C53 C52 1.390(8) . ?
C53 H53 0.9300 . ?
C42 H42 0.9300 . ?
C24 C23 1.335(10) . ?
C24 C25 1.369(10) . ?
C24 H24 0.9300 . ?
C36 H36 0.9300 . ?
C17 H17 0.9300 . ?
C23 H23 0.9300 . ?
C30 C29 1.348(10) . ?
C30 C31 1.367(11) . ?
C30 H30 0.9300 . ?
C25 H25 0.9300 . ?
C46 C47 1.371(8) . ?
C31 H31 0.9300 . ?
C29 H29 0.9300 . ?
C48 C49 1.360(12) . ?
C48 C47 1.378(9) . ?
C48 H48 0.9300 . ?
C52 H52 0.9300 . ?
C47 H47 0.9300 . ?
C49 C50 1.490(11) . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C55 H55 0.9800 . ?
C56 H56 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
N3 Ni1 N1 171.42(15) . . ?
N3 Ni1 N2 89.77(14) . . ?
N1 Ni1 N2 90.48(14) . . ?
N3 Ni1 N4 90.42(14) . . ?
N1 Ni1 N4 90.35(14) . . ?
N2 Ni1 N4 173.16(15) . . ?
C46 S1 C49 92.4(4) . . ?
C14 N2 C11 104.4(3) . . ?
C14 N2 Ni1 127.3(3) . . ?
C11 N2 Ni1 128.1(3) . . ?
C16 N3 C19 104.6(3) . . ?
C16 N3 Ni1 128.7(3) . . ?
C19 N3 Ni1 126.0(3) . . ?
C6 N1 C9 105.5(3) . . ?
C6 N1 Ni1 126.4(3) . . ?
C9 N1 Ni1 126.4(3) . . ?
C1 N4 C4 106.6(3) . . ?
C1 N4 Ni1 127.1(3) . . ?
C4 N4 Ni1 125.9(3) . . ?
C54 N6 C3 133.0(4) . . ?
C54 N6 C51 108.8(4) . . ?
C3 N6 C51 118.1(4) . . ?
C45 N5 C2 115.6(4) . . ?
C2 C3 N6 117.9(4) . . ?
C2 C3 C4 107.9(4) . . ?
N6 C3 C4 134.2(4) . . ?
C15 C14 N2 124.6(4) . . ?
C15 C14 C13 124.0(4) . . ?
N2 C14 C13 110.3(3) . . ?
C14 C15 C16 121.3(4) . . ?
C14 C15 C39 119.7(4) . . ?
C16 C15 C39 118.8(4) . . ?
C9 C10 C11 122.1(4) . . ?
C9 C10 C33 119.2(4) . . ?
C11 C10 C33 118.7(4) . . ?
N3 C16 C15 124.4(4) . . ?
N3 C16 C17 110.8(4) . . ?
C15 C16 C17 124.7(4) . . ?
C7 C8 C9 107.9(4) . . ?
C7 C8 H8 126.1 . . ?
C9 C8 H8 126.1 . . ?
C20 C19 N3 125.1(4) . . ?
C20 C19 C18 124.3(4) . . ?
N3 C19 C18 110.1(4) . . ?
C1 C20 C19 121.8(4) . . ?
C1 C20 C21 121.0(4) . . ?
C19 C20 C21 117.2(4) . . ?
C10 C9 N1 124.6(4) . . ?
C10 C9 C8 125.7(4) . . ?
N1 C9 C8 109.6(4) . . ?
C12 C13 C14 106.9(4) . . ?
C12 C13 H13 126.5 . . ?
C14 C13 H13 126.5 . . ?
C41 C40 C39 120.2(5) . . ?
C41 C40 H40 119.9 . . ?
C39 C40 H40 119.9 . . ?
C44 C39 C40 118.4(4) . . ?
C44 C39 C15 121.4(4) . . ?
C40 C39 C15 120.2(4) . . ?
C36 C37 C38 120.2(5) . . ?
C36 C37 H37 119.9 . . ?
C38 C37 H37 119.9 . . ?
N5 C45 C51 123.4(4) . . ?
N5 C45 C46 115.1(5) . . ?
C51 C45 C46 121.5(5) . . ?
C20 C1 N4 124.6(4) . . ?
C20 C1 C2 126.2(4) . . ?
N4 C1 C2 109.3(4) . . ?
C38 C33 C34 118.2(4) . . ?
C38 C33 C10 121.0(4) . . ?
C34 C33 C10 120.8(4) . . ?
C5 C4 N4 122.2(4) . . ?
C5 C4 C3 127.8(4) . . ?
N4 C4 C3 108.1(3) . . ?
C32 C27 C28 119.8(5) . . ?
C32 C27 C5 121.6(5) . . ?
C28 C27 C5 118.5(4) . . ?
C39 C44 C43 121.1(5) . . ?
C39 C44 H44 119.4 . . ?
C43 C44 H44 119.4 . . ?
C22 C21 C26 119.1(5) . . ?
C22 C21 C20 121.5(5) . . ?
C26 C21 C20 119.3(4) . . ?
C3 C2 N5 125.9(4) . . ?
C3 C2 C1 106.7(4) . . ?
N5 C2 C1 127.4(4) . . ?
C53 C54 N6 108.3(5) . . ?
C53 C54 H54 125.9 . . ?
N6 C54 H54 125.9 . . ?
C21 C22 C23 119.9(6) . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C37 C38 C33 120.9(4) . . ?
C37 C38 H38 119.5 . . ?
C33 C38 H38 119.5 . . ?
C10 C11 N2 124.1(4) . . ?
C10 C11 C12 125.4(4) . . ?
N2 C11 C12 110.4(3) . . ?
C4 C5 C6 121.6(4) . . ?
C4 C5 C27 120.4(4) . . ?
C6 C5 C27 117.4(4) . . ?
C8 C7 C6 107.6(4) . . ?
C8 C7 H7 126.2 . . ?
C6 C7 H7 126.2 . . ?
C17 C18 C19 107.5(4) . . ?
C17 C18 H18 126.2 . . ?
C19 C18 H18 126.2 . . ?
C35 C34 C33 120.6(5) . . ?
C35 C34 H34 119.7 . . ?
C33 C34 H34 119.7 . . ?
C52 C51 N6 106.2(5) . . ?
C52 C51 C45 135.1(5) . . ?
N6 C51 C45 118.5(4) . . ?
N1 C6 C5 125.5(4) . . ?
N1 C6 C7 109.3(4) . . ?
C5 C6 C7 125.1(4) . . ?
C27 C32 C31 119.1(6) . . ?
C27 C32 H32 120.5 . . ?
C31 C32 H32 120.5 . . ?
C42 C43 C44 119.0(5) . . ?
C42 C43 H43 120.5 . . ?
C44 C43 H43 120.5 . . ?
C42 C41 C40 120.5(5) . . ?
C42 C41 H41 119.7 . . ?
C40 C41 H41 119.7 . . ?
C27 C28 C29 119.4(6) . . ?
C27 C28 H28 120.3 . . ?
C29 C28 H28 120.3 . . ?
C21 C26 C25 120.6(5) . . ?
C21 C26 H26 119.7 . . ?
C25 C26 H26 119.7 . . ?
C36 C35 C34 119.7(5) . . ?
C36 C35 H35 120.2 . . ?
C34 C35 H35 120.2 . . ?
C13 C12 C11 107.8(4) . . ?
C13 C12 H12 126.1 . . ?
C11 C12 H12 126.1 . . ?
C54 C53 C52 108.3(5) . . ?
C54 C53 H53 125.8 . . ?
C52 C53 H53 125.8 . . ?
C41 C42 C43 120.7(5) . . ?
C41 C42 H42 119.6 . . ?
C43 C42 H42 119.6 . . ?
C23 C24 C25 120.4(5) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 H24 119.8 . . ?
C37 C36 C35 120.4(5) . . ?
C37 C36 H36 119.8 . . ?
C35 C36 H36 119.8 . . ?
C18 C17 C16 106.6(4) . . ?
C18 C17 H17 126.7 . . ?
C16 C17 H17 126.7 . . ?
C24 C23 C22 120.3(6) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C29 C30 C31 120.7(5) . . ?
C29 C30 H30 119.7 . . ?
C31 C30 H30 119.7 . . ?
C24 C25 C26 119.7(6) . . ?
C24 C25 H25 120.2 . . ?
C26 C25 H25 120.2 . . ?
C47 C46 C45 131.4(6) . . ?
C47 C46 S1 109.3(4) . . ?
C45 C46 S1 119.3(4) . . ?
C30 C31 C32 120.3(6) . . ?
C30 C31 H31 119.8 . . ?
C32 C31 H31 119.8 . . ?
C30 C29 C28 120.6(6) . . ?
C30 C29 H29 119.7 . . ?
C28 C29 H29 119.7 . . ?
C49 C48 C47 112.7(6) . . ?
C49 C48 H48 123.7 . . ?
C47 C48 H48 123.7 . . ?
C51 C52 C53 108.4(5) . . ?
C51 C52 H52 125.8 . . ?
C53 C52 H52 125.8 . . ?
C46 C47 C48 115.2(7) . . ?
C46 C47 H47 122.4 . . ?
C48 C47 H47 122.4 . . ?
C48 C49 C50 127.7(8) . . ?
C48 C49 S1 110.4(5) . . ?
C50 C49 S1 121.9(8) . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
Cl3 C55 Cl1 114.4(6) . . ?
Cl3 C55 Cl2 108.6(5) . . ?
Cl1 C55 Cl2 109.3(5) . . ?
Cl3 C55 H55 108.1 . . ?
Cl1 C55 H55 108.1 . . ?
Cl2 C55 H55 108.1 . . ?
Cl6 C56 Cl5 119.0(7) . . ?
Cl6 C56 Cl4 106.0(7) . . ?
Cl5 C56 Cl4 101.9(8) . . ?
Cl6 C56 H56 109.8 . . ?
Cl5 C56 H56 109.8 . . ?
Cl4 C56 H56 109.8 . . ?

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
N3 Ni1 N2 C14 17.3(4) . . . . ?
N1 Ni1 N2 C14 -171.3(4) . . . . ?
N4 Ni1 N2 C14 -74.3(12) . . . . ?
N3 Ni1 N2 C11 -168.4(4) . . . . ?
N1 Ni1 N2 C11 3.1(4) . . . . ?
N4 Ni1 N2 C11 100.1(11) . . . . ?
N1 Ni1 N3 C16 -93.4(10) . . . . ?
N2 Ni1 N3 C16 -1.7(4) . . . . ?
N4 Ni1 N3 C16 171.5(4) . . . . ?
N1 Ni1 N3 C19 75.1(10) . . . . ?
N2 Ni1 N3 C19 166.8(4) . . . . ?
N4 Ni1 N3 C19 -20.0(4) . . . . ?
N3 Ni1 N1 C6 -90.0(10) . . . . ?
N2 Ni1 N1 C6 178.4(4) . . . . ?
N4 Ni1 N1 C6 5.2(4) . . . . ?
N3 Ni1 N1 C9 72.5(10) . . . . ?
N2 Ni1 N1 C9 -19.1(4) . . . . ?
N4 Ni1 N1 C9 167.6(4) . . . . ?
N3 Ni1 N4 C1 3.5(4) . . . . ?
N1 Ni1 N4 C1 -167.9(4) . . . . ?
N2 Ni1 N4 C1 95.1(11) . . . . ?
N3 Ni1 N4 C4 -168.2(4) . . . . ?
N1 Ni1 N4 C4 20.3(4) . . . . ?
N2 Ni1 N4 C4 -76.7(12) . . . . ?
C54 N6 C3 C2 -168.3(5) . . . . ?
C51 N6 C3 C2 6.5(6) . . . . ?
C54 N6 C3 C4 9.7(9) . . . . ?
C51 N6 C3 C4 -175.4(5) . . . . ?
C11 N2 C14 C15 164.2(4) . . . . ?
Ni1 N2 C14 C15 -20.4(6) . . . . ?
C11 N2 C14 C13 -4.4(5) . . . . ?
Ni1 N2 C14 C13 171.0(3) . . . . ?
N2 C14 C15 C16 2.3(7) . . . . ?
C13 C14 C15 C16 169.4(4) . . . . ?
N2 C14 C15 C39 -172.4(4) . . . . ?
C13 C14 C15 C39 -5.3(7) . . . . ?
C19 N3 C16 C15 176.6(4) . . . . ?
Ni1 N3 C16 C15 -13.0(6) . . . . ?
C19 N3 C16 C17 -2.4(5) . . . . ?
Ni1 N3 C16 C17 168.0(3) . . . . ?
C14 C15 C16 N3 14.6(7) . . . . ?
C39 C15 C16 N3 -170.7(4) . . . . ?
C14 C15 C16 C17 -166.5(5) . . . . ?
C39 C15 C16 C17 8.2(7) . . . . ?
C16 N3 C19 C20 -167.4(4) . . . . ?
Ni1 N3 C19 C20 21.9(6) . . . . ?
C16 N3 C19 C18 5.1(5) . . . . ?
Ni1 N3 C19 C18 -165.6(3) . . . . ?
N3 C19 C20 C1 -0.2(7) . . . . ?
C18 C19 C20 C1 -171.7(5) . . . . ?
N3 C19 C20 C21 179.5(4) . . . . ?
C18 C19 C20 C21 8.0(7) . . . . ?
C11 C10 C9 N1 -5.0(7) . . . . ?
C33 C10 C9 N1 175.2(4) . . . . ?
C11 C10 C9 C8 179.8(4) . . . . ?
C33 C10 C9 C8 0.1(7) . . . . ?
C6 N1 C9 C10 -171.3(4) . . . . ?
Ni1 N1 C9 C10 23.3(6) . . . . ?
C6 N1 C9 C8 4.5(5) . . . . ?
Ni1 N1 C9 C8 -160.9(3) . . . . ?
C7 C8 C9 C10 172.8(4) . . . . ?
C7 C8 C9 N1 -3.0(5) . . . . ?
C15 C14 C13 C12 -164.8(4) . . . . ?
N2 C14 C13 C12 3.9(5) . . . . ?
C41 C40 C39 C44 -0.1(7) . . . . ?
C41 C40 C39 C15 -179.7(4) . . . . ?
C14 C15 C39 C44 106.6(5) . . . . ?
C16 C15 C39 C44 -68.2(6) . . . . ?
C14 C15 C39 C40 -73.8(6) . . . . ?
C16 C15 C39 C40 111.3(5) . . . . ?
C2 N5 C45 C51 4.9(7) . . . . ?
C2 N5 C45 C46 -177.4(4) . . . . ?
C19 C20 C1 N4 -18.2(7) . . . . ?
C21 C20 C1 N4 162.1(4) . . . . ?
C19 C20 C1 C2 161.3(4) . . . . ?
C21 C20 C1 C2 -18.4(7) . . . . ?
C4 N4 C1 C20 -173.0(4) . . . . ?
Ni1 N4 C1 C20 14.0(6) . . . . ?
C4 N4 C1 C2 7.4(5) . . . . ?
Ni1 N4 C1 C2 -165.6(3) . . . . ?
C9 C10 C33 C38 117.3(5) . . . . ?
C11 C10 C33 C38 -62.4(6) . . . . ?
C9 C10 C33 C34 -62.6(6) . . . . ?
C11 C10 C33 C34 117.7(5) . . . . ?
C1 N4 C4 C5 153.9(4) . . . . ?
Ni1 N4 C4 C5 -33.0(6) . . . . ?
C1 N4 C4 C3 -11.5(5) . . . . ?
Ni1 N4 C4 C3 161.6(3) . . . . ?
C2 C3 C4 C5 -152.7(4) . . . . ?
N6 C3 C4 C5 29.1(8) . . . . ?
C2 C3 C4 N4 11.6(5) . . . . ?
N6 C3 C4 N4 -166.6(5) . . . . ?
C40 C39 C44 C43 -1.8(8) . . . . ?
C15 C39 C44 C43 177.7(5) . . . . ?
C1 C20 C21 C22 109.2(6) . . . . ?
C19 C20 C21 C22 -70.5(7) . . . . ?
C1 C20 C21 C26 -73.4(6) . . . . ?
C19 C20 C21 C26 106.9(5) . . . . ?
N6 C3 C2 N5 -7.9(7) . . . . ?
C4 C3 C2 N5 173.6(4) . . . . ?
N6 C3 C2 C1 171.7(4) . . . . ?
C4 C3 C2 C1 -6.8(5) . . . . ?
C45 N5 C2 C3 2.1(7) . . . . ?
C45 N5 C2 C1 -177.5(5) . . . . ?
C20 C1 C2 C3 -179.9(4) . . . . ?
N4 C1 C2 C3 -0.3(5) . . . . ?
C20 C1 C2 N5 -0.3(8) . . . . ?
N4 C1 C2 N5 179.3(4) . . . . ?
C3 N6 C54 C53 176.5(5) . . . . ?
C51 N6 C54 C53 1.2(6) . . . . ?
C26 C21 C22 C23 0.5(9) . . . . ?
C20 C21 C22 C23 177.9(6) . . . . ?
C36 C37 C38 C33 -0.2(8) . . . . ?
C34 C33 C38 C37 2.1(7) . . . . ?
C10 C33 C38 C37 -177.7(4) . . . . ?
C9 C10 C11 N2 -12.5(7) . . . . ?
C33 C10 C11 N2 167.2(4) . . . . ?
C9 C10 C11 C12 171.2(4) . . . . ?
C33 C10 C11 C12 -9.1(7) . . . . ?
C14 N2 C11 C10 -173.4(4) . . . . ?
Ni1 N2 C11 C10 11.3(6) . . . . ?
C14 N2 C11 C12 3.4(5) . . . . ?
Ni1 N2 C11 C12 -172.0(3) . . . . ?
N4 C4 C5 C6 15.0(7) . . . . ?
C3 C4 C5 C6 177.3(4) . . . . ?
N4 C4 C5 C27 -155.8(4) . . . . ?
C3 C4 C5 C27 6.5(7) . . . . ?
C32 C27 C5 C4 -132.3(5) . . . . ?
C28 C27 C5 C4 50.0(6) . . . . ?
C32 C27 C5 C6 56.5(6) . . . . ?
C28 C27 C5 C6 -121.2(5) . . . . ?
C9 C8 C7 C6 0.2(5) . . . . ?
C20 C19 C18 C17 166.5(5) . . . . ?
N3 C19 C18 C17 -6.0(6) . . . . ?
C38 C33 C34 C35 -2.7(7) . . . . ?
C10 C33 C34 C35 177.1(5) . . . . ?
C54 N6 C51 C52 -1.2(6) . . . . ?
C3 N6 C51 C52 -177.3(5) . . . . ?
C54 N6 C51 C45 175.7(5) . . . . ?
C3 N6 C51 C45 -0.4(7) . . . . ?
N5 C45 C51 C52 170.1(6) . . . . ?
C46 C45 C51 C52 -7.5(10) . . . . ?
N5 C45 C51 N6 -5.7(8) . . . . ?
C46 C45 C51 N6 176.7(5) . . . . ?
C9 N1 C6 C5 172.7(4) . . . . ?
Ni1 N1 C6 C5 -21.9(6) . . . . ?
C9 N1 C6 C7 -4.3(5) . . . . ?
Ni1 N1 C6 C7 161.1(3) . . . . ?
C4 C5 C6 N1 13.0(7) . . . . ?
C27 C5 C6 N1 -175.9(4) . . . . ?
C4 C5 C6 C7 -170.4(4) . . . . ?
C27 C5 C6 C7 0.7(7) . . . . ?
C8 C7 C6 N1 2.6(5) . . . . ?
C8 C7 C6 C5 -174.4(5) . . . . ?
C28 C27 C32 C31 1.6(8) . . . . ?
C5 C27 C32 C31 -176.0(5) . . . . ?
C39 C44 C43 C42 2.8(9) . . . . ?
C39 C40 C41 C42 1.1(8) . . . . ?
C32 C27 C28 C29 0.2(7) . . . . ?
C5 C27 C28 C29 178.0(4) . . . . ?
C22 C21 C26 C25 -1.0(8) . . . . ?
C20 C21 C26 C25 -178.5(5) . . . . ?
C33 C34 C35 C36 1.3(8) . . . . ?
C14 C13 C12 C11 -1.7(6) . . . . ?
C10 C11 C12 C13 175.7(5) . . . . ?
N2 C11 C12 C13 -1.1(6) . . . . ?
N6 C54 C53 C52 -0.7(7) . . . . ?
C40 C41 C42 C43 -0.2(9) . . . . ?
C44 C43 C42 C41 -1.8(9) . . . . ?
C38 C37 C36 C35 -1.3(8) . . . . ?
C34 C35 C36 C37 0.7(8) . . . . ?
C19 C18 C17 C16 4.3(6) . . . . ?
N3 C16 C17 C18 -1.2(6) . . . . ?
C15 C16 C17 C18 179.8(5) . . . . ?
C25 C24 C23 C22 -1.4(11) . . . . ?
C21 C22 C23 C24 0.7(10) . . . . ?
C23 C24 C25 C26 0.9(11) . . . . ?
C21 C26 C25 C24 0.4(10) . . . . ?
N5 C45 C46 C47 163.7(7) . . . . ?
C51 C45 C46 C47 -18.6(10) . . . . ?
N5 C45 C46 S1 -14.0(7) . . . . ?
C51 C45 C46 S1 163.7(4) . . . . ?
C49 S1 C46 C47 0.9(6) . . . . ?
C49 S1 C46 C45 179.0(5) . . . . ?
C29 C30 C31 C32 -0.2(10) . . . . ?
C27 C32 C31 C30 -1.7(9) . . . . ?
C31 C30 C29 C28 2.1(9) . . . . ?
C27 C28 C29 C30 -2.2(8) . . . . ?
N6 C51 C52 C53 0.8(7) . . . . ?
C45 C51 C52 C53 -175.3(6) . . . . ?
C54 C53 C52 C51 -0.1(7) . . . . ?
C45 C46 C47 C48 -178.9(7) . . . . ?
S1 C46 C47 C48 -1.0(9) . . . . ?
C49 C48 C47 C46 0.7(11) . . . . ?
C47 C48 C49 C50 -179.4(9) . . . . ?
C47 C48 C49 S1 0.0(10) . . . . ?
C46 S1 C49 C48 -0.5(7) . . . . ?
C46 S1 C49 C50 179.0(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.779
_refine_diff_density_min         -1.117
_refine_diff_density_rms         0.112
####################################################################### 
# 
# 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/. 
# 
# Audit and citation data items have may 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 980828'
_audit_update_record             
;
2014-01-09 deposited with the CCDC.
2014-11-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C54 H33 Cl3 N6 Ni S'
_chemical_formula_sum            'C54 H33 Cl3 N6 Ni S'
_chemical_formula_weight         962.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'

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

_cell_length_a                   13.3636(13)
_cell_length_b                   29.0621(18)
_cell_length_c                   12.7286(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 116.573(12)
_cell_angle_gamma                90.00
_cell_volume                     4421.3(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    11326
_cell_measurement_theta_min      3.0476
_cell_measurement_theta_max      29.7510

_exptl_crystal_description       Trangular
_exptl_crystal_colour            brown
_exptl_crystal_size_max          .30
_exptl_crystal_size_mid          .28
_exptl_crystal_size_min          .24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1976
_exptl_absorpt_coefficient_mu    0.714
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_correction_T_min  0.76749
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'CrysAlisPro 1.171.34.40 (2006)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Sapphire-3 CCD detector'
_diffrn_measurement_method       'OMEGA SCAN'
_diffrn_detector_area_resol_mean 15.9853
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            65192
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         26.37
_reflns_number_total             9018
_reflns_number_gt                7754
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_cell_refinement       'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_structure_solution    SIR-92
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  'WINGX V1.80.01'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0786P)²+8.4006P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9018
_refine_ls_number_parameters     586
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0776
_refine_ls_wR_factor_ref         0.1978
_refine_ls_wR_factor_gt          0.1907
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_restrained_S_all      1.141
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni01 Ni 0.10463(4) 0.100261(15) 0.61474(4) 0.03261(16) Uani 1 1 d . . .
Cl1 Cl 0.3958(3) 0.05526(11) 0.9820(2) 0.1522(11) Uani 1 1 d . . .
S1 S 0.5105(3) 0.10244(11) 0.2892(4) 0.1653(15) Uani 1 1 d . . .
Cl3 Cl 0.4264(2) 0.03743(17) 0.7817(3) 0.2062(19) Uani 1 1 d . . .
N1 N 0.0434(3) 0.15886(11) 0.6217(3) 0.0371(7) Uani 1 1 d . . .
N2 N 0.0390(3) 0.07419(10) 0.7083(3) 0.0352(7) Uani 1 1 d . . .
Cl2 Cl 0.4178(3) 0.13070(14) 0.8540(4) 0.2005(16) Uani 1 1 d . . .
N3 N 0.1474(3) 0.04019(10) 0.5883(3) 0.0341(7) Uani 1 1 d . . .
N6 N 0.3912(3) 0.12623(12) 0.4222(3) 0.0444(8) Uani 1 1 d . . .
N5 N 0.3913(3) 0.21151(12) 0.5300(3) 0.0474(9) Uani 1 1 d . . .
N4 N 0.1899(3) 0.12777(11) 0.5412(3) 0.0361(7) Uani 1 1 d . . .
C45 C 0.2279(3) 0.05915(13) 0.4538(3) 0.0364(8) Uani 1 1 d . . .
C13 C 0.1793(4) 0.25844(14) 0.5472(4) 0.0422(9) Uani 1 1 d . . .
C12 C 0.1606(4) 0.20895(13) 0.5666(3) 0.0391(9) Uani 1 1 d . . .
C11 C 0.2238(3) 0.17402(13) 0.5524(3) 0.0369(8) Uani 1 1 d . . .
C24 C -0.1755(4) 0.15265(14) 0.7343(4) 0.0425(9) Uani 1 1 d . . .
C10 C 0.3135(3) 0.17751(13) 0.5194(3) 0.0385(8) Uani 1 1 d . . .
C3 C 0.6371(4) 0.17482(16) 0.3800(4) 0.0517(11) Uani 1 1 d . . .
H3 H 0.6681 0.2018 0.4211 0.062 Uiso 1 1 calc R . .
C41 C 0.1359(3) -0.00120(13) 0.6355(3) 0.0370(8) Uani 1 1 d . . .
C53 C 0.3197(3) 0.13614(13) 0.4697(3) 0.0390(9) Uani 1 1 d . . .
C34 C 0.1073(3) -0.00550(13) 0.7269(4) 0.0399(9) Uani 1 1 d . . .
C32 C 0.0090(4) 0.02740(15) 0.8372(4) 0.0461(10) Uani 1 1 d . . .
H32 H 0.0150 0.0027 0.8860 0.055 Uiso 1 1 calc R . .
C47 C 0.3501(4) 0.00814(16) 0.4001(4) 0.0529(11) Uani 1 1 d . . .
H47 H 0.3893 -0.0003 0.4786 0.063 Uiso 1 1 calc R . .
C22 C -0.0479(3) 0.16715(14) 0.6431(3) 0.0397(9) Uani 1 1 d . . .
C51 C 0.2075(4) 0.05238(15) 0.2502(4) 0.0486(10) Uani 1 1 d . . .
H51 H 0.1506 0.0741 0.2268 0.058 Uiso 1 1 calc R . .
C31 C -0.0505(4) 0.06577(15) 0.8251(4) 0.0462(10) Uani 1 1 d . . .
H31 H -0.0949 0.0724 0.8624 0.055 Uiso 1 1 calc R . .
C18 C 0.2063(5) 0.29041(15) 0.6367(4) 0.0567(12) Uani 1 1 d . . .
H18 H 0.2147 0.2810 0.7101 0.068 Uiso 1 1 calc R . .
C20 C -0.0129(4) 0.23394(15) 0.5800(4) 0.0494(11) Uani 1 1 d . . .
H20 H -0.0153 0.2645 0.5571 0.059 Uiso 1 1 calc R . .
C46 C 0.2639(4) 0.04014(13) 0.3670(4) 0.0408(9) Uani 1 1 d . . .
C44 C 0.1827(3) 0.02858(13) 0.5051(3) 0.0354(8) Uani 1 1 d . . .
C35 C 0.1179(4) -0.05157(15) 0.7839(4) 0.0456(10) Uani 1 1 d . . .
C23 C -0.0840(3) 0.13740(14) 0.7046(3) 0.0392(9) Uani 1 1 d . . .
C43 C 0.1821(4) -0.02037(13) 0.4929(4) 0.0432(9) Uani 1 1 d . . .
H43 H 0.1956 -0.0366 0.4376 0.052 Uiso 1 1 calc R . .
C19 C 0.0686(4) 0.20022(13) 0.5875(3) 0.0403(9) Uani 1 1 d . . .
C30 C -0.0330(3) 0.09469(13) 0.7441(3) 0.0366(8) Uani 1 1 d . . .
C40 C 0.0514(4) -0.08859(16) 0.7228(5) 0.0565(12) Uani 1 1 d . . .
H40 H -0.0008 -0.0849 0.6448 0.068 Uiso 1 1 calc R . .
C14 C 0.1659(4) 0.27297(16) 0.4381(4) 0.0489(10) Uani 1 1 d . . .
H14 H 0.1469 0.2520 0.3770 0.059 Uiso 1 1 calc R . .
C33 C 0.0621(3) 0.03133(13) 0.7613(3) 0.0377(8) Uani 1 1 d . . .
C25 C -0.1613(4) 0.19054(16) 0.8054(4) 0.0518(11) Uani 1 1 d . . .
H25 H -0.0935 0.2062 0.8374 0.062 Uiso 1 1 calc R . .
C52 C 0.2430(3) 0.10555(12) 0.4854(3) 0.0355(8) Uani 1 1 d . . .
C29 C -0.2760(4) 0.12886(16) 0.6914(4) 0.0519(11) Uani 1 1 d . . .
H29 H -0.2858 0.1028 0.6453 0.062 Uiso 1 1 calc R . .
C50 C 0.2350(5) 0.03252(19) 0.1672(4) 0.0604(13) Uani 1 1 d . . .
H50 H 0.1958 0.0406 0.0884 0.072 Uiso 1 1 calc R . .
C26 C -0.2480(5) 0.20530(18) 0.8291(4) 0.0611(13) Uani 1 1 d . . .
H26 H -0.2387 0.2314 0.8748 0.073 Uiso 1 1 calc R . .
C28 C -0.3618(4) 0.14324(18) 0.7162(5) 0.0589(12) Uani 1 1 d . . .
H28 H -0.4290 0.1271 0.6862 0.071 Uiso 1 1 calc R . .
C49 C 0.3191(5) 0.0012(2) 0.2015(5) 0.0685(15) Uani 1 1 d . . .
H49 H 0.3376 -0.0120 0.1459 0.082 Uiso 1 1 calc R . .
C42 C 0.1586(4) -0.03848(14) 0.5757(4) 0.0451(10) Uani 1 1 d . . .
H42 H 0.1571 -0.0696 0.5916 0.054 Uiso 1 1 calc R . .
C7 C 0.5284(5) 0.24220(19) 0.4974(6) 0.0741(16) Uani 1 1 d . . .
H7 H 0.5816 0.2475 0.4706 0.089 Uiso 1 1 calc R . .
C27 C -0.3477(4) 0.18143(19) 0.7853(5) 0.0603(13) Uani 1 1 d . . .
H27 H -0.4051 0.1911 0.8024 0.072 Uiso 1 1 calc R . .
C6 C 0.4615(4) 0.20363(16) 0.4742(4) 0.0519(11) Uani 1 1 d . . .
C17 C 0.2207(5) 0.33593(17) 0.6174(6) 0.0725(16) Uani 1 1 d . . .
H17 H 0.2394 0.3572 0.6779 0.087 Uiso 1 1 calc R . .
C36 C 0.1963(6) -0.0583(2) 0.8979(5) 0.0783(18) Uani 1 1 d . . .
H36 H 0.2429 -0.0342 0.9396 0.094 Uiso 1 1 calc R . .
C48 C 0.3778(5) -0.01107(18) 0.3184(5) 0.0641(14) Uani 1 1 d . . .
H48 H 0.4358 -0.0323 0.3415 0.077 Uiso 1 1 calc R . .
C9 C 0.4215(4) 0.25240(16) 0.5879(5) 0.0624(13) Uani 1 1 d . . .
H9 H 0.3910 0.2650 0.6343 0.075 Uiso 1 1 calc R . .
C4 C 0.5319(4) 0.14867(17) 0.3689(4) 0.0540(11) Uani 1 1 d . . .
C21 C -0.0847(4) 0.21345(15) 0.6117(4) 0.0480(10) Uani 1 1 d . . .
H21 H -0.1472 0.2269 0.6132 0.058 Uiso 1 1 calc R . .
C39 C 0.0620(5) -0.13094(19) 0.7768(6) 0.0779(17) Uani 1 1 d . . .
H39 H 0.0171 -0.1554 0.7347 0.094 Uiso 1 1 calc R . .
C5 C 0.4578(4) 0.15971(15) 0.4225(4) 0.0465(10) Uani 1 1 d . . .
C16 C 0.2076(5) 0.35020(18) 0.5093(6) 0.0756(17) Uani 1 1 d . . .
H16 H 0.2168 0.3811 0.4964 0.091 Uiso 1 1 calc R . .
C38 C 0.1375(7) -0.1369(2) 0.8905(7) 0.097(2) Uani 1 1 d . . .
H38 H 0.1428 -0.1652 0.9271 0.117 Uiso 1 1 calc R . .
C54 C 0.3739(6) 0.0742(3) 0.8490(6) 0.099(2) Uani 1 1 d . . .
H54 H 0.2926 0.0744 0.8007 0.119 Uiso 1 1 calc R . .
C15 C 0.1810(4) 0.31904(19) 0.4206(5) 0.0663(15) Uani 1 1 d . . .
H15 H 0.1729 0.3288 0.3476 0.080 Uiso 1 1 calc R . .
C1 C 0.6166(7) 0.1107(3) 0.2607(7) 0.105(3) Uani 1 1 d . . .
H1 H 0.6340 0.0913 0.2130 0.126 Uiso 1 1 calc R . .
C37 C 0.2066(8) -0.1010(2) 0.9517(6) 0.111(3) Uani 1 1 d . . .
H37 H 0.2601 -0.1053 1.0290 0.134 Uiso 1 1 calc R . .
C8 C 0.5028(5) 0.27162(19) 0.5673(6) 0.0788(18) Uani 1 1 d . . .
H8 H 0.5362 0.3000 0.5955 0.095 Uiso 1 1 calc R . .
C2 C 0.6747(7) 0.1475(3) 0.3121(9) 0.113(3) Uani 1 1 d . . .
H2 H 0.7385 0.1554 0.3044 0.136 Uiso 1 1 calc R . .


_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
Ni01 N1 1.909(3) . ?
Ni01 N3 1.913(3) . ?
Ni01 N2 1.923(3) . ?
Ni01 N4 1.941(3) . ?
Cl1 C54 1.678(8) . ?
S1 C4 1.630(6) . ?
S1 C1 1.631(8) . ?
Cl3 C54 1.704(8) . ?
N1 C19 1.371(5) . ?
N1 C22 1.385(5) . ?
N2 C30 1.370(5) . ?
N2 C33 1.384(5) . ?
Cl2 C54 1.736(9) . ?
N3 C44 1.380(5) . ?
N3 C41 1.383(5) . ?
N6 C5 1.317(5) . ?
N6 C53 1.371(5) . ?
N5 C9 1.361(6) . ?
N5 C10 1.396(5) . ?
N5 C6 1.426(6) . ?
N4 C52 1.370(5) . ?
N4 C11 1.405(5) . ?
C45 C44 1.391(5) . ?
C45 C52 1.396(5) . ?
C45 C46 1.494(5) . ?
C13 C14 1.384(6) . ?
C13 C18 1.387(6) . ?
C13 C12 1.500(5) . ?
C12 C11 1.384(6) . ?
C12 C19 1.392(6) . ?
C11 C10 1.440(6) . ?
C24 C25 1.383(6) . ?
C24 C29 1.386(6) . ?
C24 C23 1.499(6) . ?
C10 C53 1.378(5) . ?
C3 C2 1.421(10) . ?
C3 C4 1.548(6) . ?
C3 H3 0.9300 . ?
C41 C34 1.383(6) . ?
C41 C42 1.432(6) . ?
C53 C52 1.436(5) . ?
C34 C33 1.392(6) . ?
C34 C35 1.499(5) . ?
C32 C31 1.338(6) . ?
C32 C33 1.437(6) . ?
C32 H32 0.9300 . ?
C47 C48 1.368(7) . ?
C47 C46 1.391(6) . ?
C47 H47 0.9300 . ?
C22 C23 1.390(6) . ?
C22 C21 1.427(6) . ?
C51 C46 1.379(6) . ?
C51 C50 1.390(7) . ?
C51 H51 0.9300 . ?
C31 C30 1.429(6) . ?
C31 H31 0.9300 . ?
C18 C17 1.375(7) . ?
C18 H18 0.9300 . ?
C20 C21 1.336(6) . ?
C20 C19 1.436(6) . ?
C20 H20 0.9300 . ?
C44 C43 1.430(5) . ?
C35 C36 1.372(7) . ?
C35 C40 1.390(7) . ?
C23 C30 1.397(5) . ?
C43 C42 1.336(6) . ?
C43 H43 0.9300 . ?
C40 C39 1.385(7) . ?
C40 H40 0.9300 . ?
C14 C15 1.387(7) . ?
C14 H14 0.9300 . ?
C25 C26 1.388(6) . ?
C25 H25 0.9300 . ?
C29 C28 1.383(7) . ?
C29 H29 0.9300 . ?
C50 C49 1.357(8) . ?
C50 H50 0.9300 . ?
C26 C27 1.379(8) . ?
C26 H26 0.9300 . ?
C28 C27 1.376(7) . ?
C28 H28 0.9300 . ?
C49 C48 1.384(8) . ?
C49 H49 0.9300 . ?
C42 H42 0.9300 . ?
C7 C6 1.380(7) . ?
C7 C8 1.382(9) . ?
C7 H7 0.9300 . ?
C27 H27 0.9300 . ?
C6 C5 1.426(6) . ?
C17 C16 1.371(9) . ?
C17 H17 0.9300 . ?
C36 C37 1.395(8) . ?
C36 H36 0.9300 . ?
C48 H48 0.9300 . ?
C9 C8 1.347(8) . ?
C9 H9 0.9300 . ?
C4 C5 1.468(6) . ?
C21 H21 0.9300 . ?
C39 C38 1.355(9) . ?
C39 H39 0.9300 . ?
C16 C15 1.364(8) . ?
C16 H16 0.9300 . ?
C38 C37 1.381(11) . ?
C38 H38 0.9300 . ?
C54 H54 0.9800 . ?
C15 H15 0.9300 . ?
C1 C2 1.312(11) . ?
C1 H1 0.9300 . ?
C37 H37 0.9300 . ?
C8 H8 0.9300 . ?
C2 H2 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni01 N3 172.11(14) . . ?
N1 Ni01 N2 89.94(13) . . ?
N3 Ni01 N2 90.25(13) . . ?
N1 Ni01 N4 90.64(13) . . ?
N3 Ni01 N4 90.28(13) . . ?
N2 Ni01 N4 171.86(13) . . ?
C4 S1 C1 95.1(4) . . ?
C19 N1 C22 105.9(3) . . ?
C19 N1 Ni01 126.6(3) . . ?
C22 N1 Ni01 126.7(3) . . ?
C30 N2 C33 105.5(3) . . ?
C30 N2 Ni01 128.1(3) . . ?
C33 N2 Ni01 126.3(3) . . ?
C44 N3 C41 105.3(3) . . ?
C44 N3 Ni01 126.1(2) . . ?
C41 N3 Ni01 128.1(3) . . ?
C5 N6 C53 116.5(4) . . ?
C9 N5 C10 134.2(4) . . ?
C9 N5 C6 108.0(4) . . ?
C10 N5 C6 117.7(4) . . ?
C52 N4 C11 106.6(3) . . ?
C52 N4 Ni01 127.5(3) . . ?
C11 N4 Ni01 125.3(3) . . ?
C44 C45 C52 121.3(4) . . ?
C44 C45 C46 117.5(3) . . ?
C52 C45 C46 121.2(3) . . ?
C14 C13 C18 119.3(4) . . ?
C14 C13 C12 120.1(4) . . ?
C18 C13 C12 120.5(4) . . ?
C11 C12 C19 122.3(4) . . ?
C11 C12 C13 121.7(4) . . ?
C19 C12 C13 115.7(3) . . ?
C12 C11 N4 121.8(4) . . ?
C12 C11 C10 128.6(4) . . ?
N4 C11 C10 108.1(3) . . ?
C25 C24 C29 118.7(4) . . ?
C25 C24 C23 120.8(4) . . ?
C29 C24 C23 120.6(4) . . ?
C53 C10 N5 117.8(4) . . ?
C53 C10 C11 107.5(3) . . ?
N5 C10 C11 134.6(4) . . ?
C2 C3 C4 102.9(5) . . ?
C2 C3 H3 128.5 . . ?
C4 C3 H3 128.5 . . ?
C34 C41 N3 124.8(4) . . ?
C34 C41 C42 125.6(4) . . ?
N3 C41 C42 109.6(3) . . ?
N6 C53 C10 125.6(4) . . ?
N6 C53 C52 127.8(4) . . ?
C10 C53 C52 106.5(3) . . ?
C41 C34 C33 121.1(4) . . ?
C41 C34 C35 119.1(4) . . ?
C33 C34 C35 119.6(4) . . ?
C31 C32 C33 107.7(4) . . ?
C31 C32 H32 126.2 . . ?
C33 C32 H32 126.2 . . ?
C48 C47 C46 120.7(5) . . ?
C48 C47 H47 119.6 . . ?
C46 C47 H47 119.6 . . ?
N1 C22 C23 124.1(4) . . ?
N1 C22 C21 109.4(4) . . ?
C23 C22 C21 125.5(4) . . ?
C46 C51 C50 120.7(5) . . ?
C46 C51 H51 119.7 . . ?
C50 C51 H51 119.7 . . ?
C32 C31 C30 107.0(4) . . ?
C32 C31 H31 126.5 . . ?
C30 C31 H31 126.5 . . ?
C17 C18 C13 120.2(5) . . ?
C17 C18 H18 119.9 . . ?
C13 C18 H18 119.9 . . ?
C21 C20 C19 107.5(4) . . ?
C21 C20 H20 126.2 . . ?
C19 C20 H20 126.2 . . ?
C51 C46 C47 118.6(4) . . ?
C51 C46 C45 120.0(4) . . ?
C47 C46 C45 121.3(4) . . ?
N3 C44 C45 125.0(3) . . ?
N3 C44 C43 109.8(3) . . ?
C45 C44 C43 124.5(4) . . ?
C36 C35 C40 118.4(4) . . ?
C36 C35 C34 120.1(4) . . ?
C40 C35 C34 121.5(4) . . ?
C22 C23 C30 121.2(4) . . ?
C22 C23 C24 119.1(4) . . ?
C30 C23 C24 119.6(4) . . ?
C42 C43 C44 107.4(4) . . ?
C42 C43 H43 126.3 . . ?
C44 C43 H43 126.3 . . ?
N1 C19 C12 125.7(4) . . ?
N1 C19 C20 109.5(4) . . ?
C12 C19 C20 124.8(4) . . ?
N2 C30 C23 124.7(4) . . ?
N2 C30 C31 110.5(3) . . ?
C23 C30 C31 124.8(4) . . ?
C39 C40 C35 120.8(5) . . ?
C39 C40 H40 119.6 . . ?
C35 C40 H40 119.6 . . ?
C13 C14 C15 119.5(5) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
N2 C33 C34 124.9(4) . . ?
N2 C33 C32 109.2(3) . . ?
C34 C33 C32 124.4(4) . . ?
C24 C25 C26 120.3(5) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
N4 C52 C45 124.3(4) . . ?
N4 C52 C53 110.3(3) . . ?
C45 C52 C53 125.3(4) . . ?
C28 C29 C24 121.0(5) . . ?
C28 C29 H29 119.5 . . ?
C24 C29 H29 119.5 . . ?
C49 C50 C51 119.7(5) . . ?
C49 C50 H50 120.1 . . ?
C51 C50 H50 120.1 . . ?
C27 C26 C25 120.4(5) . . ?
C27 C26 H26 119.8 . . ?
C25 C26 H26 119.8 . . ?
C27 C28 C29 119.9(5) . . ?
C27 C28 H28 120.0 . . ?
C29 C28 H28 120.0 . . ?
C50 C49 C48 120.5(5) . . ?
C50 C49 H49 119.7 . . ?
C48 C49 H49 119.7 . . ?
C43 C42 C41 107.6(4) . . ?
C43 C42 H42 126.2 . . ?
C41 C42 H42 126.2 . . ?
C6 C7 C8 108.5(5) . . ?
C6 C7 H7 125.7 . . ?
C8 C7 H7 125.7 . . ?
C28 C27 C26 119.7(4) . . ?
C28 C27 H27 120.1 . . ?
C26 C27 H27 120.1 . . ?
C7 C6 N5 105.6(4) . . ?
C7 C6 C5 135.4(5) . . ?
N5 C6 C5 118.5(4) . . ?
C16 C17 C18 120.4(5) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C35 C36 C37 120.4(6) . . ?
C35 C36 H36 119.8 . . ?
C37 C36 H36 119.8 . . ?
C47 C48 C49 119.8(5) . . ?
C47 C48 H48 120.1 . . ?
C49 C48 H48 120.1 . . ?
C8 C9 N5 109.0(5) . . ?
C8 C9 H9 125.5 . . ?
N5 C9 H9 125.5 . . ?
C5 C4 C3 128.6(4) . . ?
C5 C4 S1 120.2(4) . . ?
C3 C4 S1 111.2(3) . . ?
C20 C21 C22 107.5(4) . . ?
C20 C21 H21 126.2 . . ?
C22 C21 H21 126.2 . . ?
C38 C39 C40 120.4(6) . . ?
C38 C39 H39 119.8 . . ?
C40 C39 H39 119.8 . . ?
N6 C5 C6 123.2(4) . . ?
N6 C5 C4 115.6(4) . . ?
C6 C5 C4 121.2(4) . . ?
C15 C16 C17 119.9(5) . . ?
C15 C16 H16 120.1 . . ?
C17 C16 H16 120.1 . . ?
C39 C38 C37 119.7(5) . . ?
C39 C38 H38 120.1 . . ?
C37 C38 H38 120.1 . . ?
Cl1 C54 Cl3 112.1(5) . . ?
Cl1 C54 Cl2 111.7(5) . . ?
Cl3 C54 Cl2 113.7(5) . . ?
Cl1 C54 H54 106.2 . . ?
Cl3 C54 H54 106.2 . . ?
Cl2 C54 H54 106.2 . . ?
C16 C15 C14 120.7(5) . . ?
C16 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
C2 C1 S1 112.9(6) . . ?
C2 C1 H1 123.6 . . ?
S1 C1 H1 123.6 . . ?
C38 C37 C36 120.1(6) . . ?
C38 C37 H37 119.9 . . ?
C36 C37 H37 119.9 . . ?
C9 C8 C7 108.8(5) . . ?
C9 C8 H8 125.6 . . ?
C7 C8 H8 125.6 . . ?
C1 C2 C3 117.9(7) . . ?
C1 C2 H2 121.1 . . ?
C3 C2 H2 121.1 . . ?

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
N3 Ni01 N1 C19 -99.6(10) . . . . ?
N2 Ni01 N1 C19 169.0(3) . . . . ?
N4 Ni01 N1 C19 -2.9(3) . . . . ?
N3 Ni01 N1 C22 68.6(11) . . . . ?
N2 Ni01 N1 C22 -22.8(3) . . . . ?
N4 Ni01 N1 C22 165.3(3) . . . . ?
N1 Ni01 N2 C30 6.7(3) . . . . ?
N3 Ni01 N2 C30 -165.4(3) . . . . ?
N4 Ni01 N2 C30 100.9(10) . . . . ?
N1 Ni01 N2 C33 -167.9(3) . . . . ?
N3 Ni01 N2 C33 19.9(3) . . . . ?
N4 Ni01 N2 C33 -73.8(10) . . . . ?
N1 Ni01 N3 C44 74.6(11) . . . . ?
N2 Ni01 N3 C44 166.0(3) . . . . ?
N4 Ni01 N3 C44 -22.2(3) . . . . ?
N1 Ni01 N3 C41 -96.0(10) . . . . ?
N2 Ni01 N3 C41 -4.6(3) . . . . ?
N4 Ni01 N3 C41 167.3(3) . . . . ?
N1 Ni01 N4 C52 -166.0(3) . . . . ?
N3 Ni01 N4 C52 6.1(3) . . . . ?
N2 Ni01 N4 C52 99.9(10) . . . . ?
N1 Ni01 N4 C11 25.2(3) . . . . ?
N3 Ni01 N4 C11 -162.7(3) . . . . ?
N2 Ni01 N4 C11 -68.9(10) . . . . ?
C14 C13 C12 C11 60.9(6) . . . . ?
C18 C13 C12 C11 -121.4(5) . . . . ?
C14 C13 C12 C19 -112.7(5) . . . . ?
C18 C13 C12 C19 65.0(6) . . . . ?
C19 C12 C11 N4 9.5(6) . . . . ?
C13 C12 C11 N4 -163.7(4) . . . . ?
C19 C12 C11 C10 173.4(4) . . . . ?
C13 C12 C11 C10 0.3(6) . . . . ?
C52 N4 C11 C12 157.4(4) . . . . ?
Ni01 N4 C11 C12 -31.9(5) . . . . ?
C52 N4 C11 C10 -9.5(4) . . . . ?
Ni01 N4 C11 C10 161.3(3) . . . . ?
C9 N5 C10 C53 -168.3(5) . . . . ?
C6 N5 C10 C53 8.6(6) . . . . ?
C9 N5 C10 C11 9.5(8) . . . . ?
C6 N5 C10 C11 -173.6(4) . . . . ?
C12 C11 C10 C53 -155.4(4) . . . . ?
N4 C11 C10 C53 10.3(4) . . . . ?
C12 C11 C10 N5 26.6(7) . . . . ?
N4 C11 C10 N5 -167.7(4) . . . . ?
C44 N3 C41 C34 176.6(4) . . . . ?
Ni01 N3 C41 C34 -11.3(6) . . . . ?
C44 N3 C41 C42 -3.2(4) . . . . ?
Ni01 N3 C41 C42 168.9(3) . . . . ?
C5 N6 C53 C10 -1.4(6) . . . . ?
C5 N6 C53 C52 -176.7(4) . . . . ?
N5 C10 C53 N6 -4.6(6) . . . . ?
C11 C10 C53 N6 177.0(4) . . . . ?
N5 C10 C53 C52 171.5(3) . . . . ?
C11 C10 C53 C52 -6.9(4) . . . . ?
N3 C41 C34 C33 15.3(6) . . . . ?
C42 C41 C34 C33 -165.0(4) . . . . ?
N3 C41 C34 C35 -169.0(4) . . . . ?
C42 C41 C34 C35 10.7(6) . . . . ?
C19 N1 C22 C23 -164.6(4) . . . . ?
Ni01 N1 C22 C23 25.2(6) . . . . ?
C19 N1 C22 C21 5.0(4) . . . . ?
Ni01 N1 C22 C21 -165.2(3) . . . . ?
C33 C32 C31 C30 -1.6(5) . . . . ?
C14 C13 C18 C17 -0.7(8) . . . . ?
C12 C13 C18 C17 -178.4(5) . . . . ?
C50 C51 C46 C47 1.2(6) . . . . ?
C50 C51 C46 C45 -175.5(4) . . . . ?
C48 C47 C46 C51 -0.5(7) . . . . ?
C48 C47 C46 C45 176.1(4) . . . . ?
C44 C45 C46 C51 112.7(4) . . . . ?
C52 C45 C46 C51 -69.5(5) . . . . ?
C44 C45 C46 C47 -63.8(5) . . . . ?
C52 C45 C46 C47 113.9(5) . . . . ?
C41 N3 C44 C45 -165.3(4) . . . . ?
Ni01 N3 C44 C45 22.4(5) . . . . ?
C41 N3 C44 C43 5.8(4) . . . . ?
Ni01 N3 C44 C43 -166.5(3) . . . . ?
C52 C45 C44 N3 1.0(6) . . . . ?
C46 C45 C44 N3 178.7(4) . . . . ?
C52 C45 C44 C43 -168.8(4) . . . . ?
C46 C45 C44 C43 8.9(6) . . . . ?
C41 C34 C35 C36 112.6(5) . . . . ?
C33 C34 C35 C36 -71.6(6) . . . . ?
C41 C34 C35 C40 -65.7(6) . . . . ?
C33 C34 C35 C40 110.0(5) . . . . ?
N1 C22 C23 C30 -3.9(6) . . . . ?
C21 C22 C23 C30 -171.9(4) . . . . ?
N1 C22 C23 C24 172.9(4) . . . . ?
C21 C22 C23 C24 4.9(6) . . . . ?
C25 C24 C23 C22 -61.7(6) . . . . ?
C29 C24 C23 C22 118.6(5) . . . . ?
C25 C24 C23 C30 115.1(5) . . . . ?
C29 C24 C23 C30 -64.5(5) . . . . ?
N3 C44 C43 C42 -6.4(5) . . . . ?
C45 C44 C43 C42 164.7(4) . . . . ?
C22 N1 C19 C12 174.3(4) . . . . ?
Ni01 N1 C19 C12 -15.5(6) . . . . ?
C22 N1 C19 C20 -3.9(4) . . . . ?
Ni01 N1 C19 C20 166.3(3) . . . . ?
C11 C12 C19 N1 15.0(6) . . . . ?
C13 C12 C19 N1 -171.4(4) . . . . ?
C11 C12 C19 C20 -167.0(4) . . . . ?
C13 C12 C19 C20 6.5(6) . . . . ?
C21 C20 C19 N1 1.4(5) . . . . ?
C21 C20 C19 C12 -176.8(4) . . . . ?
C33 N2 C30 C23 -175.3(4) . . . . ?
Ni01 N2 C30 C23 9.1(6) . . . . ?
C33 N2 C30 C31 3.3(4) . . . . ?
Ni01 N2 C30 C31 -172.3(3) . . . . ?
C22 C23 C30 N2 -13.5(6) . . . . ?
C24 C23 C30 N2 169.8(4) . . . . ?
C22 C23 C30 C31 168.1(4) . . . . ?
C24 C23 C30 C31 -8.7(6) . . . . ?
C32 C31 C30 N2 -1.1(5) . . . . ?
C32 C31 C30 C23 177.6(4) . . . . ?
C36 C35 C40 C39 1.7(8) . . . . ?
C34 C35 C40 C39 -179.9(5) . . . . ?
C18 C13 C14 C15 0.8(7) . . . . ?
C12 C13 C14 C15 178.5(4) . . . . ?
C30 N2 C33 C34 162.5(4) . . . . ?
Ni01 N2 C33 C34 -21.9(5) . . . . ?
C30 N2 C33 C32 -4.2(4) . . . . ?
Ni01 N2 C33 C32 171.4(3) . . . . ?
C41 C34 C33 N2 1.7(6) . . . . ?
C35 C34 C33 N2 -174.0(4) . . . . ?
C41 C34 C33 C32 166.4(4) . . . . ?
C35 C34 C33 C32 -9.3(6) . . . . ?
C31 C32 C33 N2 3.7(5) . . . . ?
C31 C32 C33 C34 -163.1(4) . . . . ?
C29 C24 C25 C26 -2.5(7) . . . . ?
C23 C24 C25 C26 177.8(4) . . . . ?
C11 N4 C52 C45 -177.5(4) . . . . ?
Ni01 N4 C52 C45 12.0(6) . . . . ?
C11 N4 C52 C53 5.3(4) . . . . ?
Ni01 N4 C52 C53 -165.2(3) . . . . ?
C44 C45 C52 N4 -18.6(6) . . . . ?
C46 C45 C52 N4 163.8(4) . . . . ?
C44 C45 C52 C53 158.2(4) . . . . ?
C46 C45 C52 C53 -19.4(6) . . . . ?
N6 C53 C52 N4 177.1(4) . . . . ?
C10 C53 C52 N4 1.1(5) . . . . ?
N6 C53 C52 C45 0.0(7) . . . . ?
C10 C53 C52 C45 -176.1(4) . . . . ?
C25 C24 C29 C28 1.7(7) . . . . ?
C23 C24 C29 C28 -178.6(4) . . . . ?
C46 C51 C50 C49 -1.0(7) . . . . ?
C24 C25 C26 C27 2.2(8) . . . . ?
C24 C29 C28 C27 -0.6(7) . . . . ?
C51 C50 C49 C48 0.1(8) . . . . ?
C44 C43 C42 C41 4.2(5) . . . . ?
C34 C41 C42 C43 179.5(4) . . . . ?
N3 C41 C42 C43 -0.7(5) . . . . ?
C29 C28 C27 C26 0.3(8) . . . . ?
C25 C26 C27 C28 -1.1(8) . . . . ?
C8 C7 C6 N5 1.8(6) . . . . ?
C8 C7 C6 C5 -170.0(6) . . . . ?
C9 N5 C6 C7 -2.9(5) . . . . ?
C10 N5 C6 C7 179.5(4) . . . . ?
C9 N5 C6 C5 170.6(4) . . . . ?
C10 N5 C6 C5 -7.1(6) . . . . ?
C13 C18 C17 C16 0.5(9) . . . . ?
C40 C35 C36 C37 -1.7(10) . . . . ?
C34 C35 C36 C37 179.9(6) . . . . ?
C46 C47 C48 C49 -0.3(8) . . . . ?
C50 C49 C48 C47 0.6(8) . . . . ?
C10 N5 C9 C8 180.0(5) . . . . ?
C6 N5 C9 C8 2.8(6) . . . . ?
C2 C3 C4 C5 178.5(5) . . . . ?
C2 C3 C4 S1 0.8(6) . . . . ?
C1 S1 C4 C5 -179.5(5) . . . . ?
C1 S1 C4 C3 -1.5(5) . . . . ?
C19 C20 C21 C22 1.7(5) . . . . ?
N1 C22 C21 C20 -4.3(5) . . . . ?
C23 C22 C21 C20 165.2(4) . . . . ?
C35 C40 C39 C38 0.1(9) . . . . ?
C53 N6 C5 C6 3.1(6) . . . . ?
C53 N6 C5 C4 -178.7(4) . . . . ?
C7 C6 C5 N6 172.2(6) . . . . ?
N5 C6 C5 N6 1.1(7) . . . . ?
C7 C6 C5 C4 -5.9(9) . . . . ?
N5 C6 C5 C4 -177.0(4) . . . . ?
C3 C4 C5 N6 -164.2(5) . . . . ?
S1 C4 C5 N6 13.4(6) . . . . ?
C3 C4 C5 C6 14.1(7) . . . . ?
S1 C4 C5 C6 -168.4(4) . . . . ?
C18 C17 C16 C15 -0.5(10) . . . . ?
C40 C39 C38 C37 -2.0(12) . . . . ?
C17 C16 C15 C14 0.6(9) . . . . ?
C13 C14 C15 C16 -0.8(8) . . . . ?
C4 S1 C1 C2 1.9(7) . . . . ?
C39 C38 C37 C36 2.0(13) . . . . ?
C35 C36 C37 C38 -0.1(13) . . . . ?
N5 C9 C8 C7 -1.7(7) . . . . ?
C6 C7 C8 C9 -0.2(8) . . . . ?
S1 C1 C2 C3 -1.8(11) . . . . ?
C4 C3 C2 C1 0.6(9) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.782
_refine_diff_density_min         -0.947
_refine_diff_density_rms         0.077
