# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H29 Co4 N5 O3 S10'
_chemical_formula_weight         1184.00

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'
Co Co 0.3494 0.9721 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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                   12.582(3)
_cell_length_b                   18.775(4)
_cell_length_c                   21.716(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 116.95(2)
_cell_angle_gamma                90.00
_cell_volume                     4573(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.720
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2384
_exptl_absorpt_coefficient_mu    1.927
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.714
_exptl_absorpt_correction_T_max  0.778
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            47391
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         27.48
_reflns_number_total             10482
_reflns_number_gt                8336
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       PROCESS-AUTO
_computing_cell_refinement       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_structure_solution    DirectMethod
_computing_structure_refinement  SHELXL
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_molecular_graphics    ?

_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)+(0.0254P)²+4.4569P] 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         10482
_refine_ls_number_parameters     562
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0452
_refine_ls_wR_factor_ref         0.0871
_refine_ls_wR_factor_gt          0.0810
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.087
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5761(3) 0.16615(15) 0.42335(15) 0.0313(6) Uani 1 1 d . . .
C2 C 0.6367(3) 0.18178(16) 0.38550(16) 0.0358(7) Uani 1 1 d . . .
H2 H 0.5986 0.2048 0.3431 0.043 Uiso 1 1 calc R . .
C3 C 0.7548(3) 0.16235(17) 0.41220(18) 0.0407(8) Uani 1 1 d . . .
H3 H 0.7969 0.1726 0.3875 0.049 Uiso 1 1 calc R . .
C4 C 0.8115(3) 0.12804(17) 0.47475(18) 0.0427(8) Uani 1 1 d . . .
H4 H 0.8915 0.1160 0.4918 0.051 Uiso 1 1 calc R . .
C5 C 0.7525(3) 0.1112(2) 0.51239(19) 0.0527(9) Uani 1 1 d . . .
H5 H 0.7909 0.0876 0.5545 0.063 Uiso 1 1 calc R . .
C6 C 0.6342(3) 0.13041(18) 0.48597(17) 0.0420(8) Uani 1 1 d . . .
C7 C 0.4298(3) 0.16680(18) 0.45466(16) 0.0382(7) Uani 1 1 d . . .
C8 C -0.2081(3) 0.18596(16) 0.15119(16) 0.0369(7) Uani 1 1 d . . .
C9 C -0.2267(3) 0.2069(2) 0.08601(18) 0.0506(9) Uani 1 1 d . . .
H9 H -0.1667 0.2291 0.0793 0.061 Uiso 1 1 calc R . .
C10 C -0.3363(3) 0.1940(2) 0.0315(2) 0.0597(10) Uani 1 1 d . . .
H10 H -0.3491 0.2062 -0.0129 0.072 Uiso 1 1 calc R . .
C11 C -0.4273(3) 0.1637(2) 0.0404(2) 0.0598(10) Uani 1 1 d . . .
H11 H -0.5010 0.1568 0.0023 0.072 Uiso 1 1 calc R . .
C12 C -0.4114(3) 0.1435(2) 0.1044(2) 0.0531(9) Uani 1 1 d . . .
H12 H -0.4732 0.1233 0.1107 0.064 Uiso 1 1 calc R . .
C13 C -0.2998(3) 0.15406(17) 0.15970(17) 0.0410(8) Uani 1 1 d . . .
C14 C -0.1111(3) 0.16526(17) 0.26504(17) 0.0381(7) Uani 1 1 d . . .
C15 C 0.4169(3) 0.34827(15) 0.24491(16) 0.0334(7) Uani 1 1 d . . .
C16 C 0.4230(3) 0.40618(18) 0.2857(2) 0.0489(9) Uani 1 1 d . . .
H16 H 0.4131 0.4007 0.3254 0.059 Uiso 1 1 calc R . .
C17 C 0.4441(3) 0.47216(18) 0.2659(2) 0.0572(10) Uani 1 1 d . . .
H17 H 0.4482 0.5116 0.2928 0.069 Uiso 1 1 calc R . .
C18 C 0.4591(3) 0.48131(19) 0.2079(2) 0.0551(10) Uani 1 1 d . . .
H18 H 0.4717 0.5268 0.1956 0.066 Uiso 1 1 calc R . .
C19 C 0.4558(3) 0.42508(18) 0.1680(2) 0.0521(9) Uani 1 1 d . . .
H19 H 0.4658 0.4312 0.1285 0.062 Uiso 1 1 calc R . .
C20 C 0.4372(3) 0.35817(16) 0.18803(17) 0.0373(7) Uani 1 1 d . . .
C21 C 0.4029(3) 0.23477(15) 0.21072(15) 0.0317(6) Uani 1 1 d . . .
C22 C 0.0849(3) 0.33687(16) 0.12481(17) 0.0389(7) Uani 1 1 d . . .
C23 C 0.0766(4) 0.39971(19) 0.1545(2) 0.0588(10) Uani 1 1 d . . .
H23 H 0.0553 0.4003 0.1904 0.071 Uiso 1 1 calc R . .
C24 C 0.1010(4) 0.4623(2) 0.1296(3) 0.0811(15) Uani 1 1 d . . .
H24 H 0.0960 0.5058 0.1486 0.097 Uiso 1 1 calc R . .
C25 C 0.1325(4) 0.4601(3) 0.0766(3) 0.0832(16) Uani 1 1 d . . .
H25 H 0.1505 0.5026 0.0614 0.100 Uiso 1 1 calc R . .
C26 C 0.1384(4) 0.3991(3) 0.0460(3) 0.0735(13) Uani 1 1 d . . .
H26 H 0.1584 0.3992 0.0097 0.088 Uiso 1 1 calc R . .
C27 C 0.1139(3) 0.3363(2) 0.07002(19) 0.0494(9) Uani 1 1 d . . .
C28 C 0.0715(3) 0.22037(17) 0.10297(16) 0.0378(7) Uani 1 1 d . . .
C29 C 0.2244(3) -0.03927(15) 0.18314(17) 0.0374(7) Uani 1 1 d . . .
C30 C 0.2150(3) -0.02457(19) 0.11881(19) 0.0521(9) Uani 1 1 d . . .
H30 H 0.2131 0.0223 0.1044 0.063 Uiso 1 1 calc R . .
C31 C 0.2083(4) -0.0804(2) 0.0762(2) 0.0671(12) Uani 1 1 d . . .
H31 H 0.2014 -0.0712 0.0324 0.081 Uiso 1 1 calc R . .
C32 C 0.2117(5) -0.1500(2) 0.0978(2) 0.0749(13) Uani 1 1 d . . .
H32 H 0.2057 -0.1871 0.0680 0.090 Uiso 1 1 calc R . .
C33 C 0.2237(4) -0.16529(19) 0.1618(2) 0.0675(12) Uani 1 1 d . . .
H33 H 0.2276 -0.2122 0.1764 0.081 Uiso 1 1 calc R . .
C34 C 0.2300(3) -0.10970(17) 0.20469(19) 0.0468(8) Uani 1 1 d . . .
C35 C 0.2375(3) -0.01947(16) 0.28821(16) 0.0374(7) Uani 1 1 d . . .
C36 C 0.1824(3) 0.34949(17) 0.33593(17) 0.0386(7) Uani 1 1 d . . .
C37 C 0.1702(3) 0.41490(19) 0.37467(19) 0.0496(9) Uani 1 1 d . . .
C38 C 0.0858(5) 0.4677(3) 0.3227(3) 0.1029(19) Uani 1 1 d . . .
H38A H 0.0665 0.5046 0.3465 0.154 Uiso 1 1 calc R . .
H38B H 0.0142 0.4436 0.2916 0.154 Uiso 1 1 calc R . .
H38C H 0.1233 0.4883 0.2970 0.154 Uiso 1 1 calc R . .
C39 C 0.2865(4) 0.4512(3) 0.4143(3) 0.123(3) Uani 1 1 d . . .
H39A H 0.2738 0.4962 0.4309 0.184 Uiso 1 1 calc R . .
H39B H 0.3237 0.4589 0.3848 0.184 Uiso 1 1 calc R . .
H39C H 0.3372 0.4220 0.4527 0.184 Uiso 1 1 calc R . .
C40 C 0.1166(8) 0.3901(3) 0.4189(4) 0.148(3) Uani 1 1 d . . .
H40A H 0.1753 0.3646 0.4578 0.221 Uiso 1 1 calc R . .
H40B H 0.0506 0.3592 0.3928 0.221 Uiso 1 1 calc R . .
H40C H 0.0892 0.4304 0.4350 0.221 Uiso 1 1 calc R . .
Co1 Co 0.33790(3) 0.23990(2) 0.32412(2) 0.02933(10) Uani 1 1 d . . .
Co4 Co 0.21783(4) 0.11632(2) 0.21284(2) 0.03176(10) Uani 1 1 d . . .
Co2 Co 0.05519(4) 0.23871(2) 0.23048(2) 0.03267(10) Uani 1 1 d . . .
Co3 Co 0.17516(4) 0.13165(2) 0.34846(2) 0.03355(10) Uani 1 1 d . . .
N1 N 0.4599(2) 0.18656(13) 0.40681(12) 0.0315(5) Uani 1 1 d . . .
N2 N -0.1016(2) 0.19300(14) 0.21256(13) 0.0366(6) Uani 1 1 d . . .
N3 N 0.3958(2) 0.27730(12) 0.25650(13) 0.0310(5) Uani 1 1 d . . .
N4 N 0.0628(2) 0.26969(13) 0.14311(13) 0.0345(6) Uani 1 1 d . . .
N5 N 0.2285(2) 0.01094(12) 0.23166(13) 0.0348(6) Uani 1 1 d . . .
O1 O 0.19747(17) 0.17976(10) 0.27641(10) 0.0287(4) Uani 1 1 d . . .
O2 O 0.2844(2) 0.32608(11) 0.35258(12) 0.0444(6) Uani 1 1 d . . .
O3 O 0.0885(2) 0.32272(12) 0.29045(12) 0.0463(6) Uani 1 1 d . . .
S1 S 0.29544(8) 0.18325(6) 0.45401(4) 0.0497(2) Uani 1 1 d . . .
S2 S 0.53888(8) 0.12096(6) 0.52266(5) 0.0593(3) Uani 1 1 d . . .
S3 S -0.00152(8) 0.16266(6) 0.34874(5) 0.0511(2) Uani 1 1 d . . .
S4 S -0.25070(8) 0.13140(6) 0.24535(5) 0.0519(2) Uani 1 1 d . . .
S5 S 0.43349(10) 0.27680(5) 0.15006(5) 0.0499(2) Uani 1 1 d . . .
S6 S 0.39359(8) 0.14340(4) 0.21036(5) 0.0423(2) Uani 1 1 d . . .
S7 S 0.10724(11) 0.25119(6) 0.04026(6) 0.0628(3) Uani 1 1 d . . .
S8 S 0.04911(9) 0.13094(5) 0.11024(5) 0.0507(2) Uani 1 1 d . . .
S9 S 0.24015(9) -0.11165(4) 0.28652(5) 0.0507(2) Uani 1 1 d . . .
S10 S 0.25336(11) 0.01976(5) 0.36287(5) 0.0603(3) 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
C1 C2 1.382(4) . ?
C1 C6 1.390(4) . ?
C1 N1 1.392(4) . ?
C2 C3 1.377(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.375(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.367(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.377(5) . ?
C5 H5 0.9300 . ?
C6 S2 1.724(3) . ?
C7 N1 1.311(4) . ?
C7 S1 1.712(3) . ?
C7 S2 1.723(3) . ?
C8 C9 1.383(5) . ?
C8 C13 1.385(4) . ?
C8 N2 1.403(4) . ?
C9 C10 1.372(5) . ?
C9 H9 0.9300 . ?
C10 C11 1.369(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.365(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.387(5) . ?
C12 H12 0.9300 . ?
C13 S4 1.726(4) . ?
C14 N2 1.307(4) . ?
C14 S3 1.713(3) . ?
C14 S4 1.729(3) . ?
C15 C20 1.382(4) . ?
C15 C16 1.383(4) . ?
C15 N3 1.404(4) . ?
C16 C17 1.376(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.367(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.354(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.384(4) . ?
C19 H19 0.9300 . ?
C20 S5 1.727(3) . ?
C21 N3 1.309(4) . ?
C21 S6 1.719(3) . ?
C21 S5 1.722(3) . ?
C22 C23 1.371(5) . ?
C22 N4 1.388(4) . ?
C22 C27 1.394(5) . ?
C23 C24 1.385(6) . ?
C23 H23 0.9300 . ?
C24 C25 1.377(7) . ?
C24 H24 0.9300 . ?
C25 C26 1.342(7) . ?
C25 H25 0.9300 . ?
C26 C27 1.380(5) . ?
C26 H26 0.9300 . ?
C27 S7 1.711(4) . ?
C28 N4 1.310(4) . ?
C28 S7 1.716(3) . ?
C28 S8 1.722(3) . ?
C29 C30 1.375(5) . ?
C29 C34 1.394(4) . ?
C29 N5 1.397(4) . ?
C30 C31 1.376(5) . ?
C30 H30 0.9300 . ?
C31 C32 1.384(6) . ?
C31 H31 0.9300 . ?
C32 C33 1.359(6) . ?
C32 H32 0.9300 . ?
C33 C34 1.376(5) . ?
C33 H33 0.9300 . ?
C34 S9 1.723(4) . ?
C35 N5 1.312(4) . ?
C35 S10 1.708(3) . ?
C35 S9 1.732(3) . ?
C36 O2 1.244(4) . ?
C36 O3 1.252(4) . ?
C36 C37 1.535(4) . ?
C37 C40 1.478(6) . ?
C37 C39 1.485(6) . ?
C37 C38 1.516(6) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
Co1 O1 1.952(2) . ?
Co1 O2 1.957(2) . ?
Co1 N1 2.021(2) . ?
Co1 N3 2.037(2) . ?
Co4 O1 1.9262(19) . ?
Co4 N5 2.012(2) . ?
Co4 S8 2.2933(12) . ?
Co4 S6 2.2935(11) . ?
Co2 O1 1.951(2) . ?
Co2 O3 1.966(2) . ?
Co2 N2 2.021(3) . ?
Co2 N4 2.028(3) . ?
Co3 O1 1.9342(19) . ?
Co3 S10 2.2804(11) . ?
Co3 S3 2.3007(11) . ?
Co3 S1 2.3104(12) . ?

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
C2 C1 C6 119.8(3) . . ?
C2 C1 N1 125.9(3) . . ?
C6 C1 N1 114.2(3) . . ?
C3 C2 C1 118.3(3) . . ?
C3 C2 H2 120.9 . . ?
C1 C2 H2 120.9 . . ?
C4 C3 C2 121.2(3) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C5 C4 C3 121.3(3) . . ?
C5 C4 H4 119.3 . . ?
C3 C4 H4 119.3 . . ?
C4 C5 C6 117.8(3) . . ?
C4 C5 H5 121.1 . . ?
C6 C5 H5 121.1 . . ?
C5 C6 C1 121.6(3) . . ?
C5 C6 S2 128.8(3) . . ?
C1 C6 S2 109.5(2) . . ?
N1 C7 S1 125.6(2) . . ?
N1 C7 S2 114.6(2) . . ?
S1 C7 S2 119.81(18) . . ?
C9 C8 C13 119.6(3) . . ?
C9 C8 N2 126.3(3) . . ?
C13 C8 N2 114.1(3) . . ?
C10 C9 C8 118.1(3) . . ?
C10 C9 H9 120.9 . . ?
C8 C9 H9 120.9 . . ?
C11 C10 C9 122.0(4) . . ?
C11 C10 H10 119.0 . . ?
C9 C10 H10 119.0 . . ?
C12 C11 C10 120.8(4) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C11 C12 C13 117.8(3) . . ?
C11 C12 H12 121.1 . . ?
C13 C12 H12 121.1 . . ?
C8 C13 C12 121.6(3) . . ?
C8 C13 S4 109.7(2) . . ?
C12 C13 S4 128.7(3) . . ?
N2 C14 S3 126.1(2) . . ?
N2 C14 S4 114.5(2) . . ?
S3 C14 S4 119.39(19) . . ?
C20 C15 C16 119.2(3) . . ?
C20 C15 N3 114.5(3) . . ?
C16 C15 N3 126.3(3) . . ?
C17 C16 C15 118.1(3) . . ?
C17 C16 H16 121.0 . . ?
C15 C16 H16 121.0 . . ?
C18 C17 C16 121.8(3) . . ?
C18 C17 H17 119.1 . . ?
C16 C17 H17 119.1 . . ?
C19 C18 C17 121.0(3) . . ?
C19 C18 H18 119.5 . . ?
C17 C18 H18 119.5 . . ?
C18 C19 C20 117.9(3) . . ?
C18 C19 H19 121.1 . . ?
C20 C19 H19 121.1 . . ?
C15 C20 C19 121.9(3) . . ?
C15 C20 S5 109.4(2) . . ?
C19 C20 S5 128.7(3) . . ?
N3 C21 S6 125.7(2) . . ?
N3 C21 S5 114.6(2) . . ?
S6 C21 S5 119.48(17) . . ?
C23 C22 N4 125.4(3) . . ?
C23 C22 C27 120.9(3) . . ?
N4 C22 C27 113.6(3) . . ?
C22 C23 C24 117.9(4) . . ?
C22 C23 H23 121.1 . . ?
C24 C23 H23 121.1 . . ?
C25 C24 C23 120.0(4) . . ?
C25 C24 H24 120.0 . . ?
C23 C24 H24 120.0 . . ?
C26 C25 C24 122.7(4) . . ?
C26 C25 H25 118.6 . . ?
C24 C25 H25 118.6 . . ?
C25 C26 C27 118.0(4) . . ?
C25 C26 H26 121.0 . . ?
C27 C26 H26 121.0 . . ?
C26 C27 C22 120.4(4) . . ?
C26 C27 S7 129.5(4) . . ?
C22 C27 S7 110.1(2) . . ?
N4 C28 S7 114.9(2) . . ?
N4 C28 S8 124.2(2) . . ?
S7 C28 S8 120.95(19) . . ?
C30 C29 C34 120.0(3) . . ?
C30 C29 N5 126.0(3) . . ?
C34 C29 N5 114.1(3) . . ?
C29 C30 C31 118.8(3) . . ?
C29 C30 H30 120.6 . . ?
C31 C30 H30 120.6 . . ?
C30 C31 C32 120.6(4) . . ?
C30 C31 H31 119.7 . . ?
C32 C31 H31 119.7 . . ?
C33 C32 C31 121.2(4) . . ?
C33 C32 H32 119.4 . . ?
C31 C32 H32 119.4 . . ?
C32 C33 C34 118.5(4) . . ?
C32 C33 H33 120.7 . . ?
C34 C33 H33 120.7 . . ?
C33 C34 C29 120.9(3) . . ?
C33 C34 S9 129.5(3) . . ?
C29 C34 S9 109.6(3) . . ?
N5 C35 S10 128.6(2) . . ?
N5 C35 S9 114.2(2) . . ?
S10 C35 S9 117.14(18) . . ?
O2 C36 O3 124.6(3) . . ?
O2 C36 C37 118.0(3) . . ?
O3 C36 C37 117.4(3) . . ?
C40 C37 C39 112.9(5) . . ?
C40 C37 C38 108.6(5) . . ?
C39 C37 C38 107.8(4) . . ?
C40 C37 C36 107.0(3) . . ?
C39 C37 C36 111.6(3) . . ?
C38 C37 C36 109.0(3) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C37 C40 H40A 109.5 . . ?
C37 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C37 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
O1 Co1 O2 106.71(9) . . ?
O1 Co1 N1 108.99(9) . . ?
O2 Co1 N1 111.14(10) . . ?
O1 Co1 N3 110.50(9) . . ?
O2 Co1 N3 103.26(10) . . ?
N1 Co1 N3 115.81(10) . . ?
O1 Co4 N5 118.73(9) . . ?
O1 Co4 S8 104.90(7) . . ?
N5 Co4 S8 105.19(8) . . ?
O1 Co4 S6 108.82(6) . . ?
N5 Co4 S6 104.28(8) . . ?
S8 Co4 S6 115.37(4) . . ?
O1 Co2 O3 104.22(9) . . ?
O1 Co2 N2 116.55(9) . . ?
O3 Co2 N2 111.39(11) . . ?
O1 Co2 N4 102.68(9) . . ?
O3 Co2 N4 107.66(10) . . ?
N2 Co2 N4 113.43(10) . . ?
O1 Co3 S10 109.23(6) . . ?
O1 Co3 S3 112.25(6) . . ?
S10 Co3 S3 126.17(4) . . ?
O1 Co3 S1 109.68(7) . . ?
S10 Co3 S1 101.67(4) . . ?
S3 Co3 S1 95.20(4) . . ?
C7 N1 C1 111.4(3) . . ?
C7 N1 Co1 117.9(2) . . ?
C1 N1 Co1 130.68(19) . . ?
C14 N2 C8 111.5(3) . . ?
C14 N2 Co2 117.9(2) . . ?
C8 N2 Co2 130.6(2) . . ?
C21 N3 C15 111.1(2) . . ?
C21 N3 Co1 120.44(19) . . ?
C15 N3 Co1 127.97(19) . . ?
C28 N4 C22 111.3(3) . . ?
C28 N4 Co2 118.3(2) . . ?
C22 N4 Co2 129.0(2) . . ?
C35 N5 C29 111.7(3) . . ?
C35 N5 Co4 126.0(2) . . ?
C29 N5 Co4 122.3(2) . . ?
Co4 O1 Co3 113.96(10) . . ?
Co4 O1 Co2 111.94(9) . . ?
Co3 O1 Co2 104.04(9) . . ?
Co4 O1 Co1 110.83(9) . . ?
Co3 O1 Co1 105.61(9) . . ?
Co2 O1 Co1 110.07(9) . . ?
C36 O2 Co1 131.1(2) . . ?
C36 O3 Co2 133.4(2) . . ?
C7 S1 Co3 97.64(11) . . ?
C7 S2 C6 90.19(15) . . ?
C14 S3 Co3 108.57(11) . . ?
C13 S4 C14 90.19(16) . . ?
C21 S5 C20 90.41(15) . . ?
C21 S6 Co4 106.59(10) . . ?
C27 S7 C28 90.05(16) . . ?
C28 S8 Co4 95.04(11) . . ?
C34 S9 C35 90.44(16) . . ?
C35 S10 Co3 114.17(11) . . ?

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
C6 C1 C2 C3 -1.3(5) . . . . ?
N1 C1 C2 C3 174.8(3) . . . . ?
C1 C2 C3 C4 0.2(5) . . . . ?
C2 C3 C4 C5 0.7(5) . . . . ?
C3 C4 C5 C6 -0.6(5) . . . . ?
C4 C5 C6 C1 -0.5(5) . . . . ?
C4 C5 C6 S2 -176.4(3) . . . . ?
C2 C1 C6 C5 1.4(5) . . . . ?
N1 C1 C6 C5 -175.1(3) . . . . ?
C2 C1 C6 S2 178.0(2) . . . . ?
N1 C1 C6 S2 1.5(3) . . . . ?
C13 C8 C9 C10 -1.0(5) . . . . ?
N2 C8 C9 C10 178.3(3) . . . . ?
C8 C9 C10 C11 2.3(6) . . . . ?
C9 C10 C11 C12 -1.6(7) . . . . ?
C10 C11 C12 C13 -0.6(6) . . . . ?
C9 C8 C13 C12 -1.1(5) . . . . ?
N2 C8 C13 C12 179.5(3) . . . . ?
C9 C8 C13 S4 178.3(3) . . . . ?
N2 C8 C13 S4 -1.0(4) . . . . ?
C11 C12 C13 C8 1.9(5) . . . . ?
C11 C12 C13 S4 -177.4(3) . . . . ?
C20 C15 C16 C17 2.8(5) . . . . ?
N3 C15 C16 C17 -179.7(3) . . . . ?
C15 C16 C17 C18 -0.1(6) . . . . ?
C16 C17 C18 C19 -1.2(6) . . . . ?
C17 C18 C19 C20 -0.2(6) . . . . ?
C16 C15 C20 C19 -4.3(5) . . . . ?
N3 C15 C20 C19 177.9(3) . . . . ?
C16 C15 C20 S5 176.2(3) . . . . ?
N3 C15 C20 S5 -1.6(3) . . . . ?
C18 C19 C20 C15 2.9(5) . . . . ?
C18 C19 C20 S5 -177.6(3) . . . . ?
N4 C22 C23 C24 -179.5(4) . . . . ?
C27 C22 C23 C24 -1.6(6) . . . . ?
C22 C23 C24 C25 -0.1(7) . . . . ?
C23 C24 C25 C26 1.6(8) . . . . ?
C24 C25 C26 C27 -1.3(7) . . . . ?
C25 C26 C27 C22 -0.4(6) . . . . ?
C25 C26 C27 S7 176.8(4) . . . . ?
C23 C22 C27 C26 1.9(5) . . . . ?
N4 C22 C27 C26 -179.9(3) . . . . ?
C23 C22 C27 S7 -175.8(3) . . . . ?
N4 C22 C27 S7 2.3(4) . . . . ?
C34 C29 C30 C31 1.6(6) . . . . ?
N5 C29 C30 C31 -178.0(4) . . . . ?
C29 C30 C31 C32 -0.4(7) . . . . ?
C30 C31 C32 C33 -1.1(7) . . . . ?
C31 C32 C33 C34 1.3(7) . . . . ?
C32 C33 C34 C29 -0.1(6) . . . . ?
C32 C33 C34 S9 177.6(4) . . . . ?
C30 C29 C34 C33 -1.4(6) . . . . ?
N5 C29 C34 C33 178.2(3) . . . . ?
C30 C29 C34 S9 -179.5(3) . . . . ?
N5 C29 C34 S9 0.1(4) . . . . ?
O2 C36 C37 C40 -109.1(5) . . . . ?
O3 C36 C37 C40 69.7(5) . . . . ?
O2 C36 C37 C39 14.8(5) . . . . ?
O3 C36 C37 C39 -166.4(4) . . . . ?
O2 C36 C37 C38 133.7(4) . . . . ?
O3 C36 C37 C38 -47.5(5) . . . . ?
S1 C7 N1 C1 178.8(2) . . . . ?
S2 C7 N1 C1 -0.9(3) . . . . ?
S1 C7 N1 Co1 -0.9(4) . . . . ?
S2 C7 N1 Co1 179.39(14) . . . . ?
C2 C1 N1 C7 -176.7(3) . . . . ?
C6 C1 N1 C7 -0.4(4) . . . . ?
C2 C1 N1 Co1 3.0(4) . . . . ?
C6 C1 N1 Co1 179.3(2) . . . . ?
O1 Co1 N1 C7 -60.4(2) . . . . ?
O2 Co1 N1 C7 56.9(3) . . . . ?
N3 Co1 N1 C7 174.3(2) . . . . ?
O1 Co1 N1 C1 119.9(2) . . . . ?
O2 Co1 N1 C1 -122.8(2) . . . . ?
N3 Co1 N1 C1 -5.4(3) . . . . ?
S3 C14 N2 C8 179.8(2) . . . . ?
S4 C14 N2 C8 -2.3(4) . . . . ?
S3 C14 N2 Co2 -0.9(4) . . . . ?
S4 C14 N2 Co2 176.95(15) . . . . ?
C9 C8 N2 C14 -177.2(3) . . . . ?
C13 C8 N2 C14 2.2(4) . . . . ?
C9 C8 N2 Co2 3.7(5) . . . . ?
C13 C8 N2 Co2 -177.0(2) . . . . ?
O1 Co2 N2 C14 54.7(3) . . . . ?
O3 Co2 N2 C14 -64.6(3) . . . . ?
N4 Co2 N2 C14 173.7(2) . . . . ?
O1 Co2 N2 C8 -126.2(3) . . . . ?
O3 Co2 N2 C8 114.4(3) . . . . ?
N4 Co2 N2 C8 -7.2(3) . . . . ?
S6 C21 N3 C15 175.0(2) . . . . ?
S5 C21 N3 C15 -0.8(3) . . . . ?
S6 C21 N3 Co1 -12.7(4) . . . . ?
S5 C21 N3 Co1 171.50(14) . . . . ?
C20 C15 N3 C21 1.6(4) . . . . ?
C16 C15 N3 C21 -176.1(3) . . . . ?
C20 C15 N3 Co1 -170.0(2) . . . . ?
C16 C15 N3 Co1 12.4(5) . . . . ?
O1 Co1 N3 C21 -44.5(2) . . . . ?
O2 Co1 N3 C21 -158.2(2) . . . . ?
N1 Co1 N3 C21 80.1(2) . . . . ?
O1 Co1 N3 C15 126.4(2) . . . . ?
O2 Co1 N3 C15 12.6(3) . . . . ?
N1 Co1 N3 C15 -109.1(2) . . . . ?
S7 C28 N4 C22 0.1(3) . . . . ?
S8 C28 N4 C22 -179.6(2) . . . . ?
S7 C28 N4 Co2 -167.54(14) . . . . ?
S8 C28 N4 Co2 12.7(4) . . . . ?
C23 C22 N4 C28 176.5(3) . . . . ?
C27 C22 N4 C28 -1.6(4) . . . . ?
C23 C22 N4 Co2 -17.5(5) . . . . ?
C27 C22 N4 Co2 164.4(2) . . . . ?
O1 Co2 N4 C28 54.5(2) . . . . ?
O3 Co2 N4 C28 164.1(2) . . . . ?
N2 Co2 N4 C28 -72.2(3) . . . . ?
O1 Co2 N4 C22 -110.7(3) . . . . ?
O3 Co2 N4 C22 -1.0(3) . . . . ?
N2 Co2 N4 C22 122.7(3) . . . . ?
S10 C35 N5 C29 176.1(3) . . . . ?
S9 C35 N5 C29 -0.6(3) . . . . ?
S10 C35 N5 Co4 -5.2(4) . . . . ?
S9 C35 N5 Co4 178.11(15) . . . . ?
C30 C29 N5 C35 179.9(3) . . . . ?
C34 C29 N5 C35 0.3(4) . . . . ?
C30 C29 N5 Co4 1.1(5) . . . . ?
C34 C29 N5 Co4 -178.5(2) . . . . ?
O1 Co4 N5 C35 -8.9(3) . . . . ?
S8 Co4 N5 C35 -125.8(2) . . . . ?
S6 Co4 N5 C35 112.4(3) . . . . ?
O1 Co4 N5 C29 169.7(2) . . . . ?
S8 Co4 N5 C29 52.8(2) . . . . ?
S6 Co4 N5 C29 -69.0(2) . . . . ?
N5 Co4 O1 Co3 -5.29(14) . . . . ?
S8 Co4 O1 Co3 111.78(9) . . . . ?
S6 Co4 O1 Co3 -124.23(8) . . . . ?
N5 Co4 O1 Co2 -123.01(11) . . . . ?
S8 Co4 O1 Co2 -5.95(10) . . . . ?
S6 Co4 O1 Co2 118.04(8) . . . . ?
N5 Co4 O1 Co1 113.67(11) . . . . ?
S8 Co4 O1 Co1 -129.26(8) . . . . ?
S6 Co4 O1 Co1 -5.27(10) . . . . ?
S10 Co3 O1 Co4 22.97(11) . . . . ?
S3 Co3 O1 Co4 -121.91(8) . . . . ?
S1 Co3 O1 Co4 133.60(8) . . . . ?
S10 Co3 O1 Co2 145.16(7) . . . . ?
S3 Co3 O1 Co2 0.27(10) . . . . ?
S1 Co3 O1 Co2 -104.22(8) . . . . ?
S10 Co3 O1 Co1 -98.92(8) . . . . ?
S3 Co3 O1 Co1 116.20(8) . . . . ?
S1 Co3 O1 Co1 11.71(10) . . . . ?
O3 Co2 O1 Co4 -155.99(10) . . . . ?
N2 Co2 O1 Co4 80.82(12) . . . . ?
N4 Co2 O1 Co4 -43.79(12) . . . . ?
O3 Co2 O1 Co3 80.49(11) . . . . ?
N2 Co2 O1 Co3 -42.69(13) . . . . ?
N4 Co2 O1 Co3 -167.30(9) . . . . ?
O3 Co2 O1 Co1 -32.25(12) . . . . ?
N2 Co2 O1 Co1 -155.43(10) . . . . ?
N4 Co2 O1 Co1 79.95(11) . . . . ?
O2 Co1 O1 Co4 155.08(10) . . . . ?
N1 Co1 O1 Co4 -84.83(11) . . . . ?
N3 Co1 O1 Co4 43.49(12) . . . . ?
O2 Co1 O1 Co3 -81.04(11) . . . . ?
N1 Co1 O1 Co3 39.05(11) . . . . ?
N3 Co1 O1 Co3 167.38(9) . . . . ?
O2 Co1 O1 Co2 30.69(12) . . . . ?
N1 Co1 O1 Co2 150.78(10) . . . . ?
N3 Co1 O1 Co2 -80.89(11) . . . . ?
O3 C36 O2 Co1 -6.0(5) . . . . ?
C37 C36 O2 Co1 172.7(2) . . . . ?
O1 Co1 O2 C36 -12.6(3) . . . . ?
N1 Co1 O2 C36 -131.3(3) . . . . ?
N3 Co1 O2 C36 103.9(3) . . . . ?
O2 C36 O3 Co2 1.8(5) . . . . ?
C37 C36 O3 Co2 -176.9(2) . . . . ?
O1 Co2 O3 C36 19.7(3) . . . . ?
N2 Co2 O3 C36 146.1(3) . . . . ?
N4 Co2 O3 C36 -88.9(3) . . . . ?
N1 C7 S1 Co3 56.0(3) . . . . ?
S2 C7 S1 Co3 -124.25(19) . . . . ?
O1 Co3 S1 C7 -60.56(14) . . . . ?
S10 Co3 S1 C7 54.97(12) . . . . ?
S3 Co3 S1 C7 -176.43(12) . . . . ?
N1 C7 S2 C6 1.5(3) . . . . ?
S1 C7 S2 C6 -178.3(2) . . . . ?
C5 C6 S2 C7 174.7(4) . . . . ?
C1 C6 S2 C7 -1.6(3) . . . . ?
N2 C14 S3 Co3 -43.1(3) . . . . ?
S4 C14 S3 Co3 139.10(16) . . . . ?
O1 Co3 S3 C14 42.20(14) . . . . ?
S10 Co3 S3 C14 -95.52(13) . . . . ?
S1 Co3 S3 C14 155.94(13) . . . . ?
C8 C13 S4 C14 -0.2(3) . . . . ?
C12 C13 S4 C14 179.2(3) . . . . ?
N2 C14 S4 C13 1.5(3) . . . . ?
S3 C14 S4 C13 179.5(2) . . . . ?
N3 C21 S5 C20 -0.1(3) . . . . ?
S6 C21 S5 C20 -176.2(2) . . . . ?
C15 C20 S5 C21 1.0(2) . . . . ?
C19 C20 S5 C21 -178.6(3) . . . . ?
N3 C21 S6 Co4 54.9(3) . . . . ?
S5 C21 S6 Co4 -129.55(16) . . . . ?
O1 Co4 S6 C21 -41.30(13) . . . . ?
N5 Co4 S6 C21 -168.95(13) . . . . ?
S8 Co4 S6 C21 76.22(12) . . . . ?
C26 C27 S7 C28 -179.3(4) . . . . ?
C22 C27 S7 C28 -1.9(3) . . . . ?
N4 C28 S7 C27 1.0(3) . . . . ?
S8 C28 S7 C27 -179.2(2) . . . . ?
N4 C28 S8 Co4 -69.3(3) . . . . ?
S7 C28 S8 Co4 111.00(19) . . . . ?
O1 Co4 S8 C28 60.13(13) . . . . ?
N5 Co4 S8 C28 -173.87(14) . . . . ?
S6 Co4 S8 C28 -59.57(12) . . . . ?
C33 C34 S9 C35 -178.3(4) . . . . ?
C29 C34 S9 C35 -0.4(3) . . . . ?
N5 C35 S9 C34 0.6(3) . . . . ?
S10 C35 S9 C34 -176.5(2) . . . . ?
N5 C35 S10 Co3 27.2(4) . . . . ?
S9 C35 S10 Co3 -156.12(14) . . . . ?
O1 Co3 S10 C35 -35.21(15) . . . . ?
S3 Co3 S10 C35 103.53(14) . . . . ?
S1 Co3 S10 C35 -151.07(13) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.795
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.067
_database_code_depnum_ccdc_archive 'CCDC 1013607'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H22 N4 Ni3 O2 S10'
_chemical_formula_sum            'C30 H22 N4 Ni3 O2 S10'
_chemical_formula_weight         967.29

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'

_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                   7.6972(15)
_cell_length_b                   9.965(2)
_cell_length_c                   12.372(3)
_cell_angle_alpha                94.89(3)
_cell_angle_beta                 96.17(3)
_cell_angle_gamma                110.77(3)
_cell_volume                     874.4(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.837
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             490
_exptl_absorpt_coefficient_mu    2.234
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.646
_exptl_absorpt_correction_T_max  0.699
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  SCX-MINI
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7439
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_sigmaI/netI    0.0510
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.09
_diffrn_reflns_theta_max         24.99
_reflns_number_total             3071
_reflns_number_gt                2652
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       PROCESS-AUTO
_computing_cell_refinement       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_structure_solution    DirectMethod
_computing_structure_refinement  SHELXL
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_molecular_graphics    ?

_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)+(0.0536P)²+1.4371P] 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         3064
_refine_ls_number_parameters     227
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0487
_refine_ls_wR_factor_ref         0.1240
_refine_ls_wR_factor_gt          0.1194
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.066
_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
Ni1 Ni 1.0000 0.5000 0.5000 0.0283(2) Uani 1 2 d S . .
Ni2 Ni 0.84741(9) 0.52452(7) 0.23219(5) 0.0380(2) Uani 1 1 d . A .
S3 S 1.11656(18) 0.62217(12) 0.36351(9) 0.0377(3) Uani 1 1 d . . .
S4 S 0.79398(19) 0.08249(13) 0.28541(10) 0.0412(3) Uani 1 1 d . . .
S5 S 0.64865(17) 0.32944(14) 0.30815(10) 0.0420(3) Uani 1 1 d . . .
S2 S 1.29031(18) 0.53006(15) 0.29547(10) 0.0460(3) Uani 1 1 d . . .
S1 S 1.21508(19) 0.29502(17) 0.10574(11) 0.0520(4) Uani 1 1 d . . .
N2 N 0.9640(5) 0.3174(4) 0.4201(3) 0.0312(8) Uani 1 1 d . . .
N1 N 0.9716(5) 0.4102(4) 0.1489(3) 0.0353(9) Uani 1 1 d . . .
C2 C 0.8109(6) 0.2535(5) 0.3457(3) 0.0321(10) Uani 1 1 d . . .
C3 C 1.1404(7) 0.4145(5) 0.1827(4) 0.0381(11) Uani 1 1 d . . .
C4 C 1.0025(7) 0.0983(5) 0.3649(3) 0.0329(10) Uani 1 1 d . . .
C5 C 0.9979(7) 0.2314(6) 0.0210(4) 0.0421(12) Uani 1 1 d . . .
O1 O 0.7456(6) 0.6361(5) 0.1904(4) 0.0718(12) Uani 1 1 d . . .
C7 C 0.8851(7) 0.3045(5) 0.0567(4) 0.0368(11) Uani 1 1 d . . .
C8 C 0.7043(8) 0.2680(6) 0.0047(4) 0.0528(14) Uani 1 1 d . . .
H8A H 0.6293 0.3171 0.0277 0.063 Uiso 1 1 calc R . .
C9 C 0.9295(8) 0.1193(6) -0.0680(4) 0.0503(14) Uani 1 1 d . . .
H9A H 1.0048 0.0711 -0.0920 0.060 Uiso 1 1 calc R . .
C10 C 0.7495(9) 0.0840(7) -0.1177(4) 0.0611(16) Uani 1 1 d . . .
H10A H 0.7009 0.0098 -0.1763 0.073 Uiso 1 1 calc R . .
C11 C 0.6354(9) 0.1576(7) -0.0821(5) 0.0681(18) Uani 1 1 d . . .
H11A H 0.5129 0.1317 -0.1173 0.082 Uiso 1 1 calc R . .
C12 C 1.0765(6) 0.2334(4) 0.4328(3) 0.0298(10) Uani 1 1 d . . .
C13 C 1.2452(6) 0.2740(5) 0.5024(4) 0.0379(11) Uani 1 1 d . . .
H13A H 1.2955 0.3637 0.5458 0.046 Uiso 1 1 calc R . .
C14 C 1.2632(7) 0.0419(5) 0.4388(4) 0.0442(12) Uani 1 1 d . . .
H14A H 1.3285 -0.0206 0.4425 0.053 Uiso 1 1 calc R . .
C15 C 1.0969(8) 0.0013(5) 0.3689(4) 0.0420(12) Uani 1 1 d . . .
H15A H 1.0482 -0.0882 0.3252 0.050 Uiso 1 1 calc R . .
C16 C 1.3358(7) 0.1775(6) 0.5052(4) 0.0451(12) Uani 1 1 d . . .
H16A H 1.4482 0.2023 0.5523 0.054 Uiso 1 1 calc R . .
C21 C 0.6527(13) 0.6943(10) 0.1550(8) 0.0295(14) Uani 0.50 1 d PU A 1
H21A H 0.7018 0.7937 0.1878 0.044 Uiso 0.50 1 calc PR A 1
H21B H 0.5271 0.6482 0.1705 0.044 Uiso 0.50 1 calc PR A 1
H21C H 0.6513 0.6897 0.0771 0.044 Uiso 0.50 1 calc PR A 1
C21' C 0.6964(13) 0.7364(10) 0.1960(8) 0.0295(14) Uani 0.50 1 d PU A 2
H21D H 0.6393 0.7431 0.1248 0.044 Uiso 0.50 1 calc PR A 2
H21E H 0.8032 0.8237 0.2213 0.044 Uiso 0.50 1 calc PR A 2
H21F H 0.6070 0.7236 0.2463 0.044 Uiso 0.50 1 calc PR 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 N2 1.908(4) 2_766 ?
Ni1 N2 1.908(4) . ?
Ni1 S3 2.2452(14) . ?
Ni1 S3 2.2452(14) 2_766 ?
Ni2 O1 1.657(5) . ?
Ni2 N1 2.014(4) . ?
Ni2 S3 2.3356(17) . ?
Ni2 S5 2.3484(17) . ?
S3 S2 2.0785(19) . ?
S4 C4 1.739(5) . ?
S4 C2 1.756(4) . ?
S5 C2 1.719(5) . ?
S2 C3 1.744(5) . ?
S1 C5 1.748(5) . ?
S1 C3 1.751(5) . ?
N2 C2 1.332(6) . ?
N2 C12 1.408(6) . ?
N1 C3 1.306(6) . ?
N1 C7 1.410(6) . ?
C4 C15 1.401(6) . ?
C4 C12 1.415(6) . ?
C5 C7 1.398(7) . ?
C5 C9 1.409(7) . ?
O1 C21 1.144(9) . ?
O1 C21' 1.187(9) . ?
C7 C8 1.376(7) . ?
C8 C11 1.380(7) . ?
C9 C10 1.362(8) . ?
C10 C11 1.411(9) . ?
C12 C13 1.385(6) . ?
C13 C16 1.374(7) . ?
C14 C15 1.374(7) . ?
C14 C16 1.410(7) . ?

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 N2 180.00(12) 2_766 . ?
N2 Ni1 S3 87.18(11) 2_766 . ?
N2 Ni1 S3 92.82(11) . . ?
N2 Ni1 S3 92.82(11) 2_766 2_766 ?
N2 Ni1 S3 87.18(11) . 2_766 ?
S3 Ni1 S3 180.00(6) . 2_766 ?
O1 Ni2 N1 130.40(19) . . ?
O1 Ni2 S3 117.48(17) . . ?
N1 Ni2 S3 89.87(12) . . ?
O1 Ni2 S5 113.73(16) . . ?
N1 Ni2 S5 96.32(12) . . ?
S3 Ni2 S5 104.02(6) . . ?
S2 S3 Ni1 108.72(7) . . ?
S2 S3 Ni2 100.37(6) . . ?
Ni1 S3 Ni2 97.82(5) . . ?
C4 S4 C2 91.1(2) . . ?
C2 S5 Ni2 97.61(16) . . ?
C3 S2 S3 102.15(18) . . ?
C5 S1 C3 89.1(2) . . ?
C2 N2 C12 113.2(4) . . ?
C2 N2 Ni1 118.7(3) . . ?
C12 N2 Ni1 128.0(3) . . ?
C3 N1 C7 111.0(4) . . ?
C3 N1 Ni2 122.6(3) . . ?
C7 N1 Ni2 125.9(3) . . ?
N2 C2 S5 124.7(3) . . ?
N2 C2 S4 112.7(3) . . ?
S5 C2 S4 122.6(3) . . ?
N1 C3 S2 124.5(4) . . ?
N1 C3 S1 115.7(4) . . ?
S2 C3 S1 119.8(3) . . ?
C15 C4 C12 120.4(4) . . ?
C15 C4 S4 130.0(4) . . ?
C12 C4 S4 109.6(3) . . ?
C7 C5 C9 121.1(5) . . ?
C7 C5 S1 109.9(4) . . ?
C9 C5 S1 128.9(4) . . ?
C21 O1 C21' 30.3(6) . . ?
C21 O1 Ni2 169.5(6) . . ?
C21' O1 Ni2 157.9(6) . . ?
C8 C7 C5 120.1(5) . . ?
C8 C7 N1 125.6(5) . . ?
C5 C7 N1 114.3(4) . . ?
C7 C8 C11 119.2(5) . . ?
C10 C9 C5 117.8(5) . . ?
C9 C10 C11 121.3(5) . . ?
C8 C11 C10 120.4(5) . . ?
C13 C12 N2 125.6(4) . . ?
C13 C12 C4 121.0(4) . . ?
N2 C12 C4 113.4(4) . . ?
C16 C13 C12 117.8(4) . . ?
C15 C14 C16 120.6(5) . . ?
C14 C15 C4 118.3(4) . . ?
C13 C16 C14 121.9(5) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.963
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.093
_database_code_depnum_ccdc_archive 'CCDC 1013608'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H16 N4 Ni4 S10'
_chemical_formula_sum            'C27 H16 N4 Ni4 S10'
_chemical_formula_weight         951.90

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'
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           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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                   9.5006(19)
_cell_length_b                   16.608(3)
_cell_length_c                   20.842(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.14(3)
_cell_angle_gamma                90.00
_cell_volume                     3255.6(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            'dark brown'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1912
_exptl_absorpt_coefficient_mu    2.949
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.649
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  SCX-MINI
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26348
_diffrn_reflns_av_R_equivalents  0.1328
_diffrn_reflns_av_sigmaI/netI    0.1040
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.98
_diffrn_reflns_theta_max         25.01
_reflns_number_total             5729
_reflns_number_gt                4133
_reflns_threshold_expression     >2sigma(I)


_computing_data_collection       PROCESS-AUTO
_computing_cell_refinement       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_structure_solution    DirectMethod
_computing_structure_refinement  SHELXL
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_molecular_graphics    ?

_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. 'Omit' restraint instruction 
was used in the refinement. 
;

_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)+(0.0262P)²+29.8045P] 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         5729
_refine_ls_number_parameters     406
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1356
_refine_ls_R_factor_gt           0.0983
_refine_ls_wR_factor_ref         0.1949
_refine_ls_wR_factor_gt          0.1813
_refine_ls_goodness_of_fit_ref   1.184
_refine_ls_restrained_S_all      1.184
_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
Ni1 Ni 0.24400(15) 0.09625(8) 0.49170(7) 0.0391(4) Uani 1 1 d . . .
Ni2 Ni 0.13332(15) 0.06475(8) 0.60427(7) 0.0386(4) Uani 1 1 d . . .
Ni4 Ni 0.20962(16) 0.22212(9) 0.64855(8) 0.0463(4) Uani 1 1 d . . .
Ni3 Ni 0.09066(15) 0.22926(8) 0.51307(7) 0.0412(4) Uani 1 1 d . . .
S4 S 0.0284(3) 0.10200(17) 0.50862(14) 0.0412(7) Uani 1 1 d . . .
S2 S 0.2774(3) -0.01025(16) 0.55050(14) 0.0391(7) Uani 1 1 d . . .
S1 S 0.6767(3) 0.1041(2) 0.60491(16) 0.0496(8) Uani 1 1 d . . .
S3 S 0.2047(3) 0.19797(18) 0.42834(14) 0.0429(7) Uani 1 1 d . . .
S6 S -0.0037(3) 0.25383(19) 0.59953(17) 0.0507(8) Uani 1 1 d . . .
S8 S 0.3808(4) 0.1607(2) 0.71193(17) 0.0577(9) Uani 1 1 d . . .
S7 S 0.4002(4) 0.0109(2) 0.79266(16) 0.0588(9) Uani 1 1 d . . .
S5 S 0.0199(3) 0.15100(18) 0.65610(16) 0.0464(8) Uani 1 1 d . . .
S10 S 0.3504(4) 0.3152(2) 0.61985(18) 0.0626(10) Uani 1 1 d . . .
S9 S 0.3167(5) 0.4634(2) 0.5387(2) 0.0746(12) Uani 1 1 d . . .
N3 N 0.4495(9) 0.0172(5) 0.5823(4) 0.037(2) Uani 1 1 d . . .
C7 C 0.5109(11) 0.0853(7) 0.5607(5) 0.040(3) Uani 1 1 d . . .
N4 N 0.4388(9) 0.1248(5) 0.5122(4) 0.037(2) Uani 1 1 d . . .
N2 N 0.1542(10) 0.3404(6) 0.5123(5) 0.046(2) Uani 1 1 d . . .
C8 C 0.4823(13) 0.1971(6) 0.4841(5) 0.043(3) Uani 1 1 d . . .
N1 N 0.2215(10) 0.0248(6) 0.6876(5) 0.045(2) Uani 1 1 d . . .
C1 C 0.5395(12) -0.0244(7) 0.6311(5) 0.040(3) Uani 1 1 d . . .
C6 C 0.6668(12) 0.0154(7) 0.6498(5) 0.041(3) Uani 1 1 d . . .
C13 C 0.6223(13) 0.2255(8) 0.4905(6) 0.054(3) Uani 1 1 d . . .
H13 H 0.6940 0.1978 0.5165 0.065 Uiso 1 1 calc R . .
C18 C 0.2915(14) -0.1476(9) 0.7949(7) 0.064(4) Uani 1 1 d . . .
H18 H 0.3509 -0.1599 0.8330 0.077 Uiso 1 1 calc R . .
C14 C 0.2040(12) -0.0533(7) 0.7112(6) 0.047(3) Uani 1 1 d . . .
C16 C 0.1082(15) -0.1860(9) 0.7089(7) 0.065(4) Uani 1 1 d . . .
H16 H 0.0459 -0.2247 0.6891 0.078 Uiso 1 1 calc R . .
C17 C 0.2001(15) -0.2049(8) 0.7658(7) 0.064(4) Uani 1 1 d . . .
H17 H 0.1988 -0.2561 0.7836 0.076 Uiso 1 1 calc R . .
C20 C 0.3213(12) 0.0646(7) 0.7252(6) 0.046(3) Uani 1 1 d . . .
C5 C 0.7672(13) -0.0174(8) 0.6968(6) 0.057(4) Uani 1 1 d . . .
H5 H 0.8534 0.0085 0.7096 0.068 Uiso 1 1 calc R . .
C11 C 0.5505(15) 0.3340(8) 0.4179(7) 0.066(4) Uani 1 1 d . . .
H11 H 0.5736 0.3794 0.3955 0.079 Uiso 1 1 calc R . .
C4 C 0.7370(14) -0.0885(9) 0.7240(7) 0.061(4) Uani 1 1 d . . .
H4 H 0.8030 -0.1104 0.7566 0.073 Uiso 1 1 calc R . .
C10 C 0.4125(14) 0.3071(7) 0.4101(6) 0.054(3) Uani 1 1 d . . .
H10 H 0.3425 0.3347 0.3830 0.065 Uiso 1 1 calc R . .
C21 C 0.1100(14) 0.3969(7) 0.4641(7) 0.054(3) Uani 1 1 d . . .
C3 C 0.6128(15) -0.1290(8) 0.7051(6) 0.060(4) Uani 1 1 d . . .
H3 H 0.5984 -0.1782 0.7245 0.072 Uiso 1 1 calc R . .
C9 C 0.3776(13) 0.2381(7) 0.4432(6) 0.046(3) Uani 1 1 d . . .
C2 C 0.5061(13) -0.0989(7) 0.6576(5) 0.045(3) Uani 1 1 d . . .
H2 H 0.4209 -0.1258 0.6447 0.054 Uiso 1 1 calc R . .
C26 C 0.1869(15) 0.4681(8) 0.4719(7) 0.061(4) Uani 1 1 d . . .
C27 C 0.2615(14) 0.3652(8) 0.5549(6) 0.053(3) Uani 1 1 d . . .
C19 C 0.2960(13) -0.0716(8) 0.7680(6) 0.052(3) Uani 1 1 d . . .
C23 C -0.0283(17) 0.4502(10) 0.3694(8) 0.081(5) Uani 1 1 d . . .
H23 H -0.1013 0.4448 0.3349 0.097 Uiso 1 1 calc R . .
C24 C 0.049(2) 0.5202(10) 0.3770(9) 0.088(5) Uani 1 1 d . . .
H24 H 0.0269 0.5617 0.3473 0.106 Uiso 1 1 calc R . .
C22 C 0.0025(14) 0.3869(8) 0.4134(7) 0.061(4) Uani 1 1 d . . .
H22 H -0.0488 0.3391 0.4084 0.073 Uiso 1 1 calc R . .
C25 C 0.1566(19) 0.5310(9) 0.4266(8) 0.079(5) Uani 1 1 d . . .
H25 H 0.2088 0.5785 0.4306 0.095 Uiso 1 1 calc R . .
C15 C 0.1102(13) -0.1099(7) 0.6823(6) 0.052(3) Uani 1 1 d . . .
H15 H 0.0484 -0.0970 0.6451 0.062 Uiso 1 1 calc R . .
C12 C 0.6549(15) 0.2946(8) 0.4584(7) 0.066(4) Uani 1 1 d . . .
H12 H 0.7475 0.3143 0.4642 0.079 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 N4 1.900(9) . ?
Ni1 S4 2.130(3) . ?
Ni1 S3 2.144(3) . ?
Ni1 S2 2.150(3) . ?
Ni1 Ni3 2.717(2) . ?
Ni1 Ni2 2.754(2) . ?
Ni2 N1 1.935(10) . ?
Ni2 S5 2.170(3) . ?
Ni2 S4 2.188(3) . ?
Ni2 S2 2.262(3) . ?
Ni2 Ni4 2.832(2) . ?
Ni4 S5 2.179(3) . ?
Ni4 S10 2.183(4) . ?
Ni4 S8 2.196(4) . ?
Ni4 S6 2.200(4) . ?
Ni4 Ni3 2.892(2) . ?
Ni3 N2 1.944(10) . ?
Ni3 S6 2.162(4) . ?
Ni3 S4 2.193(3) . ?
Ni3 S3 2.259(3) . ?
S2 N3 1.736(9) . ?
S1 C7 1.736(11) . ?
S1 C6 1.755(12) . ?
S3 C9 1.759(12) . ?
S6 S5 2.069(4) . ?
S8 C20 1.727(12) . ?
S7 C19 1.726(13) . ?
S7 C20 1.743(12) . ?
S10 C27 1.705(13) . ?
S9 C26 1.726(15) . ?
S9 C27 1.762(13) . ?
N3 C7 1.377(14) . ?
N3 C1 1.414(13) . ?
C7 N4 1.315(13) . ?
N4 C8 1.421(14) . ?
N2 C27 1.319(15) . ?
N2 C21 1.395(15) . ?
C8 C9 1.394(16) . ?
C8 C13 1.400(16) . ?
N1 C20 1.319(14) . ?
N1 C14 1.407(14) . ?
C1 C6 1.384(15) . ?
C1 C2 1.409(15) . ?
C6 C5 1.379(15) . ?
C13 C12 1.385(17) . ?
C18 C17 1.370(18) . ?
C18 C19 1.385(17) . ?
C14 C15 1.374(16) . ?
C14 C19 1.402(16) . ?
C16 C15 1.380(17) . ?
C16 C17 1.404(18) . ?
C5 C4 1.358(18) . ?
C11 C10 1.372(17) . ?
C11 C12 1.374(18) . ?
C4 C3 1.367(17) . ?
C10 C9 1.402(16) . ?
C21 C22 1.373(18) . ?
C21 C26 1.386(16) . ?
C3 C2 1.406(16) . ?
C26 C25 1.410(19) . ?
C23 C24 1.37(2) . ?
C23 C22 1.398(18) . ?
C24 C25 1.36(2) . ?

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
N4 Ni1 S4 151.8(3) . . ?
N4 Ni1 S3 91.2(3) . . ?
S4 Ni1 S3 88.78(12) . . ?
N4 Ni1 S2 91.0(3) . . ?
S4 Ni1 S2 90.58(12) . . ?
S3 Ni1 S2 176.52(13) . . ?
N4 Ni1 Ni3 106.7(3) . . ?
S4 Ni1 Ni3 52.11(9) . . ?
S3 Ni1 Ni3 53.83(9) . . ?
S2 Ni1 Ni3 127.93(11) . . ?
N4 Ni1 Ni2 109.5(3) . . ?
S4 Ni1 Ni2 51.33(9) . . ?
S3 Ni1 Ni2 128.33(11) . . ?
S2 Ni1 Ni2 53.22(9) . . ?
Ni3 Ni1 Ni2 74.72(6) . . ?
N1 Ni2 S5 87.8(3) . . ?
N1 Ni2 S4 176.3(3) . . ?
S5 Ni2 S4 94.16(13) . . ?
N1 Ni2 S2 92.3(3) . . ?
S5 Ni2 S2 171.18(13) . . ?
S4 Ni2 S2 86.21(12) . . ?
N1 Ni2 Ni1 131.4(3) . . ?
S5 Ni2 Ni1 125.11(11) . . ?
S4 Ni2 Ni1 49.44(9) . . ?
S2 Ni2 Ni1 49.58(8) . . ?
N1 Ni2 Ni4 88.0(3) . . ?
S5 Ni2 Ni4 49.52(9) . . ?
S4 Ni2 Ni4 95.66(10) . . ?
S2 Ni2 Ni4 121.66(9) . . ?
Ni1 Ni2 Ni4 89.50(6) . . ?
S5 Ni4 S10 161.61(15) . . ?
S5 Ni4 S8 104.73(14) . . ?
S10 Ni4 S8 93.66(15) . . ?
S5 Ni4 S6 56.39(12) . . ?
S10 Ni4 S6 105.25(14) . . ?
S8 Ni4 S6 160.98(14) . . ?
S5 Ni4 Ni2 49.24(9) . . ?
S10 Ni4 Ni2 134.68(12) . . ?
S8 Ni4 Ni2 84.30(10) . . ?
S6 Ni4 Ni2 83.87(10) . . ?
S5 Ni4 Ni3 83.10(10) . . ?
S10 Ni4 Ni3 82.73(11) . . ?
S8 Ni4 Ni3 139.49(12) . . ?
S6 Ni4 Ni3 47.91(10) . . ?
Ni2 Ni4 Ni3 70.91(5) . . ?
N2 Ni3 S6 89.6(3) . . ?
N2 Ni3 S4 176.0(3) . . ?
S6 Ni3 S4 94.36(13) . . ?
N2 Ni3 S3 91.6(3) . . ?
S6 Ni3 S3 174.99(14) . . ?
S4 Ni3 S3 84.35(12) . . ?
N2 Ni3 Ni1 126.6(3) . . ?
S6 Ni3 Ni1 125.82(11) . . ?
S4 Ni3 Ni1 50.02(9) . . ?
S3 Ni3 Ni1 50.01(8) . . ?
N2 Ni3 Ni4 88.2(3) . . ?
S6 Ni3 Ni4 49.06(10) . . ?
S4 Ni3 Ni4 93.88(10) . . ?
S3 Ni3 Ni4 126.13(10) . . ?
Ni1 Ni3 Ni4 88.98(6) . . ?
Ni1 S4 Ni2 79.23(11) . . ?
Ni1 S4 Ni3 77.88(11) . . ?
Ni2 S4 Ni3 98.53(12) . . ?
N3 S2 Ni1 93.3(3) . . ?
N3 S2 Ni2 105.7(3) . . ?
Ni1 S2 Ni2 77.20(10) . . ?
C7 S1 C6 91.1(6) . . ?
C9 S3 Ni1 96.5(4) . . ?
C9 S3 Ni3 108.3(4) . . ?
Ni1 S3 Ni3 76.16(11) . . ?
S5 S6 Ni3 107.16(16) . . ?
S5 S6 Ni4 61.29(13) . . ?
Ni3 S6 Ni4 83.03(12) . . ?
C20 S8 Ni4 107.1(4) . . ?
C19 S7 C20 90.2(6) . . ?
S6 S5 Ni2 106.40(17) . . ?
S6 S5 Ni4 62.32(13) . . ?
Ni2 S5 Ni4 81.23(12) . . ?
C27 S10 Ni4 107.9(5) . . ?
C26 S9 C27 89.9(6) . . ?
C7 N3 C1 113.3(9) . . ?
C7 N3 S2 120.7(8) . . ?
C1 N3 S2 126.0(7) . . ?
N4 C7 N3 117.6(10) . . ?
N4 C7 S1 130.8(9) . . ?
N3 C7 S1 111.7(8) . . ?
C7 N4 C8 126.0(10) . . ?
C7 N4 Ni1 115.7(8) . . ?
C8 N4 Ni1 116.7(8) . . ?
C27 N2 C21 113.6(10) . . ?
C27 N2 Ni3 120.1(9) . . ?
C21 N2 Ni3 125.6(8) . . ?
C9 C8 C13 118.6(11) . . ?
C9 C8 N4 116.1(11) . . ?
C13 C8 N4 125.0(11) . . ?
C20 N1 C14 111.4(10) . . ?
C20 N1 Ni2 123.0(8) . . ?
C14 N1 Ni2 124.9(8) . . ?
C6 C1 C2 123.1(11) . . ?
C6 C1 N3 112.6(10) . . ?
C2 C1 N3 124.3(10) . . ?
C1 C6 C5 120.0(11) . . ?
C1 C6 S1 111.2(8) . . ?
C5 C6 S1 128.8(10) . . ?
C12 C13 C8 120.5(12) . . ?
C17 C18 C19 120.5(12) . . ?
C15 C14 C19 120.7(12) . . ?
C15 C14 N1 125.4(11) . . ?
C19 C14 N1 113.9(11) . . ?
C15 C16 C17 120.1(13) . . ?
C18 C17 C16 119.9(12) . . ?
N1 C20 S8 126.3(9) . . ?
N1 C20 S7 114.5(9) . . ?
S8 C20 S7 119.2(7) . . ?
C4 C5 C6 118.3(13) . . ?
C10 C11 C12 120.9(12) . . ?
C5 C4 C3 122.2(13) . . ?
C11 C10 C9 119.7(12) . . ?
C22 C21 C26 121.0(13) . . ?
C22 C21 N2 126.1(12) . . ?
C26 C21 N2 112.9(12) . . ?
C4 C3 C2 122.3(13) . . ?
C8 C9 C10 120.2(11) . . ?
C8 C9 S3 119.4(9) . . ?
C10 C9 S3 120.2(10) . . ?
C3 C2 C1 114.1(12) . . ?
C21 C26 C25 119.9(14) . . ?
C21 C26 S9 111.1(11) . . ?
C25 C26 S9 128.9(12) . . ?
N2 C27 S10 129.2(10) . . ?
N2 C27 S9 112.4(10) . . ?
S10 C27 S9 118.4(7) . . ?
C18 C19 C14 119.2(12) . . ?
C18 C19 S7 130.7(11) . . ?
C14 C19 S7 110.0(9) . . ?
C24 C23 C22 120.2(16) . . ?
C25 C24 C23 122.1(16) . . ?
C21 C22 C23 118.5(14) . . ?
C24 C25 C26 118.2(15) . . ?
C14 C15 C16 119.7(12) . . ?
C11 C12 C13 120.0(12) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.798
_refine_diff_density_min         -0.693
_refine_diff_density_rms         0.138
_database_code_depnum_ccdc_archive 'CCDC 1013609'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_4

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H32 N8 Ni4 S8'
_chemical_formula_weight         1260.18

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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                   13.969(3)
_cell_length_b                   25.511(5)
_cell_length_c                   15.810(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 120.22(2)
_cell_angle_gamma                90.00
_cell_volume                     4868(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2560
_exptl_absorpt_coefficient_mu    1.915
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.729
_exptl_absorpt_correction_T_max  0.826
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  SCX-MINI
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            47568
_diffrn_reflns_av_R_equivalents  0.1634
_diffrn_reflns_av_sigmaI/netI    0.1593
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.03
_diffrn_reflns_theta_max         27.48
_reflns_number_total             11150
_reflns_number_gt                5884
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       PROCESS-AUTO
_computing_cell_refinement       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_structure_solution    DirectMethod
_computing_structure_refinement  SHELXL
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_molecular_graphics    ?

_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)+(0.0330P)²+2.4059P] 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         11150
_refine_ls_number_parameters     649
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1845
_refine_ls_R_factor_gt           0.0875
_refine_ls_wR_factor_ref         0.1329
_refine_ls_wR_factor_gt          0.1106
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.074
_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 0.33099(6) 0.17360(3) -0.08134(6) 0.0309(2) Uani 1 1 d . . .
Ni4 Ni 0.35078(6) 0.22696(3) 0.09016(6) 0.0311(2) Uani 1 1 d . . .
Ni2 Ni 0.28905(7) 0.07817(3) -0.00609(6) 0.0316(2) Uani 1 1 d . . .
Ni3 Ni 0.27055(6) 0.13602(3) 0.14207(6) 0.0313(2) Uani 1 1 d . . .
S6 S 0.31031(14) 0.05086(6) 0.13025(13) 0.0369(4) Uani 1 1 d . . .
S7 S 0.42935(14) 0.24338(6) 0.00606(12) 0.0352(4) Uani 1 1 d . . .
S5 S 0.25097(13) 0.10281(6) -0.15757(12) 0.0360(4) Uani 1 1 d . . .
S2 S -0.05822(14) 0.07141(7) -0.07823(14) 0.0455(5) Uani 1 1 d . . .
S8 S 0.25329(13) 0.21641(6) 0.16911(12) 0.0344(4) Uani 1 1 d . . .
S4 S 0.60543(15) 0.17031(7) 0.38486(13) 0.0463(5) Uani 1 1 d . . .
S1 S 0.08190(15) 0.29977(7) -0.17470(13) 0.0469(5) Uani 1 1 d . . .
S3 S 0.58908(16) 0.05697(7) -0.01250(15) 0.0494(5) Uani 1 1 d . . .
N1 N 0.2367(4) 0.26823(19) -0.0069(4) 0.0326(13) Uani 1 1 d . . .
N3 N 0.4601(4) 0.13670(18) -0.0581(4) 0.0295(12) Uani 1 1 d . . .
N6 N 0.4463(4) 0.08096(19) 0.0529(4) 0.0325(13) Uani 1 1 d . . .
N4 N 0.4059(4) 0.14318(18) 0.2591(4) 0.0313(13) Uani 1 1 d . . .
N8 N 0.4853(4) 0.19175(19) 0.1850(4) 0.0316(13) Uani 1 1 d . . .
N7 N 0.1213(4) 0.13747(19) 0.0326(4) 0.0312(13) Uani 1 1 d . . .
N5 N 0.1863(4) 0.20318(19) -0.1268(4) 0.0320(13) Uani 1 1 d . . .
C7 C 0.0769(5) 0.0968(2) -0.0287(5) 0.0321(16) Uani 1 1 d . . .
C51 C 0.6494(5) 0.2271(3) 0.0708(5) 0.0415(18) Uani 1 1 d . . .
H51 H 0.6365 0.2434 0.0133 0.050 Uiso 1 1 calc R . .
C34 C 0.5099(6) 0.0589(2) 0.1464(5) 0.0369(17) Uani 1 1 d . . .
C27 C 0.5138(5) 0.1419(2) -0.1106(5) 0.0324(16) Uani 1 1 d . . .
N2 N 0.1398(4) 0.06554(19) -0.0494(4) 0.0320(13) Uani 1 1 d . . .
C33 C 0.4913(5) 0.0950(2) -0.0011(5) 0.0307(16) Uani 1 1 d . . .
C45 C 0.5286(5) 0.1379(2) 0.4273(5) 0.0333(16) Uani 1 1 d . . .
C50 C 0.7534(6) 0.2095(3) 0.1366(6) 0.050(2) Uani 1 1 d . . .
H50 H 0.8118 0.2141 0.1248 0.060 Uiso 1 1 calc R . .
C10 C -0.0570(6) 0.1890(3) -0.0424(5) 0.048(2) Uani 1 1 d . . .
H10 H -0.0962 0.1625 -0.0869 0.058 Uiso 1 1 calc R . .
C40 C 0.4228(5) 0.1273(2) 0.3501(5) 0.0321(16) Uani 1 1 d . . .
C39 C 0.4546(6) 0.0435(2) 0.1950(5) 0.0374(17) Uani 1 1 d . . .
C14 C 0.2148(5) 0.3199(2) 0.0077(5) 0.0330(16) Uani 1 1 d . . .
C9 C 0.0563(5) 0.1820(2) 0.0247(5) 0.0329(16) Uani 1 1 d . . .
C6 C -0.0234(6) 0.0168(2) -0.1226(5) 0.0414(18) Uani 1 1 d . . .
C8 C 0.1113(5) 0.2239(2) 0.0856(4) 0.0313(16) Uani 1 1 d . . .
C32 C 0.5890(5) 0.1022(3) -0.0950(5) 0.0381(17) Uani 1 1 d . . .
C25 C -0.1001(6) 0.1574(3) -0.3013(5) 0.056(2) Uani 1 1 d . . .
H25 H -0.1732 0.1684 -0.3276 0.067 Uiso 1 1 calc R . .
C46 C 0.4913(5) 0.1681(2) 0.2642(5) 0.0315(16) Uani 1 1 d . . .
C1 C 0.0862(5) 0.0203(2) -0.0980(5) 0.0338(16) Uani 1 1 d . . .
C48 C 0.6849(5) 0.1778(3) 0.2383(5) 0.0428(18) Uani 1 1 d . . .
H48 H 0.6984 0.1602 0.2947 0.051 Uiso 1 1 calc R . .
C21 C 0.0930(5) 0.1746(3) -0.1945(5) 0.0352(17) Uani 1 1 d . . .
C13 C 0.0564(6) 0.2692(3) 0.0839(5) 0.0469(19) Uani 1 1 d . . .
H13 H 0.0951 0.2963 0.1272 0.056 Uiso 1 1 calc R . .
C17 C 0.1399(7) 0.4184(3) 0.0158(6) 0.064(2) Uani 1 1 d . . .
H17 H 0.1149 0.4515 0.0202 0.077 Uiso 1 1 calc R . .
C22 C 0.1130(5) 0.1252(2) -0.2199(5) 0.0349(16) Uani 1 1 d . . .
C16 C 0.2265(7) 0.3957(3) 0.0971(6) 0.054(2) Uani 1 1 d . . .
H16 H 0.2594 0.4140 0.1560 0.065 Uiso 1 1 calc R . .
C29 C 0.5650(6) 0.1817(3) -0.2172(5) 0.049(2) Uani 1 1 d . . .
H29 H 0.5570 0.2088 -0.2597 0.058 Uiso 1 1 calc R . .
C35 C 0.6254(6) 0.0547(3) 0.1994(5) 0.049(2) Uani 1 1 d . . .
H35 H 0.6663 0.0665 0.1715 0.058 Uiso 1 1 calc R . .
C18 C 0.0902(6) 0.3922(3) -0.0721(6) 0.057(2) Uani 1 1 d . . .
H18 H 0.0316 0.4073 -0.1276 0.069 Uiso 1 1 calc R . .
C26 C -0.0176(6) 0.1891(3) -0.2351(5) 0.0459(19) Uani 1 1 d . . .
H26 H -0.0354 0.2206 -0.2170 0.055 Uiso 1 1 calc R . .
C5 C -0.0876(6) -0.0259(3) -0.1712(6) 0.058(2) Uani 1 1 d . . .
H5 H -0.1621 -0.0274 -0.1897 0.070 Uiso 1 1 calc R . .
C47 C 0.5790(5) 0.1964(2) 0.1744(5) 0.0308(16) Uani 1 1 d . . .
C52 C 0.5632(5) 0.2208(2) 0.0896(5) 0.0343(16) Uani 1 1 d . . .
C20 C 0.1748(5) 0.2513(3) -0.0971(5) 0.0345(17) Uani 1 1 d . . .
C30 C 0.6396(6) 0.1425(3) -0.2003(5) 0.052(2) Uani 1 1 d . . .
H30 H 0.6816 0.1436 -0.2309 0.063 Uiso 1 1 calc R . .
C28 C 0.5017(5) 0.1821(3) -0.1733(5) 0.0399(18) Uani 1 1 d . . .
H28 H 0.4515 0.2090 -0.1857 0.048 Uiso 1 1 calc R . .
C49 C 0.7701(6) 0.1851(3) 0.2199(5) 0.050(2) Uani 1 1 d . . .
H49 H 0.8407 0.1731 0.2651 0.060 Uiso 1 1 calc R . .
C2 C 0.1341(5) -0.0194(3) -0.1222(5) 0.0453(19) Uani 1 1 d . . .
H2 H 0.2068 -0.0165 -0.1087 0.054 Uiso 1 1 calc R . .
C31 C 0.6532(6) 0.1013(3) -0.1378(5) 0.052(2) Uani 1 1 d . . .
H31 H 0.7034 0.0744 -0.1257 0.062 Uiso 1 1 calc R . .
C19 C 0.1290(6) 0.3429(3) -0.0763(5) 0.0415(18) Uani 1 1 d . . .
C24 C -0.0798(6) 0.1102(3) -0.3306(6) 0.062(2) Uani 1 1 d . . .
H24 H -0.1373 0.0899 -0.3777 0.075 Uiso 1 1 calc R . .
C38 C 0.5092(6) 0.0225(3) 0.2878(6) 0.052(2) Uani 1 1 d . . .
H38 H 0.4694 0.0113 0.3171 0.063 Uiso 1 1 calc R . .
C15 C 0.2659(6) 0.3467(3) 0.0943(5) 0.0460(19) Uani 1 1 d . . .
H15 H 0.3257 0.3323 0.1497 0.055 Uiso 1 1 calc R . .
C23 C 0.0297(6) 0.0937(3) -0.2875(5) 0.048(2) Uani 1 1 d . . .
H23 H 0.0466 0.0615 -0.3044 0.058 Uiso 1 1 calc R . .
C12 C -0.0552(6) 0.2747(3) 0.0186(6) 0.056(2) Uani 1 1 d . . .
H12 H -0.0924 0.3053 0.0167 0.068 Uiso 1 1 calc R . .
C37 C 0.6232(7) 0.0181(3) 0.3374(6) 0.059(2) Uani 1 1 d . . .
H37 H 0.6612 0.0047 0.4008 0.071 Uiso 1 1 calc R . .
C3 C 0.0723(6) -0.0638(3) -0.1670(6) 0.062(2) Uani 1 1 d . . .
H3 H 0.1049 -0.0919 -0.1805 0.074 Uiso 1 1 calc R . .
C11 C -0.1103(6) 0.2335(3) -0.0439(6) 0.057(2) Uani 1 1 d . . .
H11 H -0.1859 0.2364 -0.0879 0.068 Uiso 1 1 calc R . .
C4 C -0.0368(7) -0.0665(3) -0.1916(6) 0.064(2) Uani 1 1 d . . .
H4 H -0.0776 -0.0964 -0.2228 0.076 Uiso 1 1 calc R . .
C36 C 0.6793(6) 0.0337(3) 0.2913(6) 0.060(2) Uani 1 1 d . . .
H36 H 0.7559 0.0300 0.3234 0.072 Uiso 1 1 calc R . .
C41 C 0.3469(6) 0.1022(3) 0.3675(5) 0.0459(19) Uani 1 1 d . . .
H41 H 0.2756 0.0952 0.3166 0.055 Uiso 1 1 calc R . .
C43 C 0.4826(7) 0.0975(3) 0.5368(6) 0.058(2) Uani 1 1 d . . .
H43 H 0.5022 0.0866 0.5996 0.070 Uiso 1 1 calc R . .
C42 C 0.3788(6) 0.0878(3) 0.4615(6) 0.055(2) Uani 1 1 d . . .
H42 H 0.3281 0.0710 0.4740 0.065 Uiso 1 1 calc R . .
C44 C 0.5598(6) 0.1234(3) 0.5215(5) 0.054(2) Uani 1 1 d . . .
H44 H 0.6304 0.1307 0.5733 0.065 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 1.898(5) . ?
Ni1 N5 1.926(5) . ?
Ni1 S5 2.1465(18) . ?
Ni1 S7 2.2483(18) . ?
Ni1 Ni2 2.8961(12) . ?
Ni1 Ni4 2.9201(16) . ?
Ni4 N1 1.882(5) . ?
Ni4 N8 1.936(5) . ?
Ni4 S7 2.1487(19) . ?
Ni4 S8 2.2795(19) . ?
Ni4 Ni3 2.8700(12) . ?
Ni2 N2 1.866(5) . ?
Ni2 N6 1.908(5) . ?
Ni2 S6 2.139(2) . ?
Ni2 S5 2.265(2) . ?
Ni2 Ni3 2.8883(15) . ?
Ni3 N4 1.874(5) . ?
Ni3 N7 1.927(5) . ?
Ni3 S8 2.1330(18) . ?
Ni3 S6 2.2733(18) . ?
S6 C39 1.752(7) . ?
S7 C52 1.756(6) . ?
S5 C22 1.760(6) . ?
S2 C6 1.735(7) . ?
S2 C7 1.763(6) . ?
S8 C8 1.754(6) . ?
S4 C45 1.736(6) . ?
S4 C46 1.768(6) . ?
S1 C19 1.742(7) . ?
S1 C20 1.765(6) . ?
S3 C32 1.740(7) . ?
S3 C33 1.758(6) . ?
N1 C20 1.314(7) . ?
N1 C14 1.399(7) . ?
N3 C33 1.318(7) . ?
N3 C27 1.377(7) . ?
N6 C33 1.338(7) . ?
N6 C34 1.403(8) . ?
N4 C46 1.317(7) . ?
N4 C40 1.396(7) . ?
N8 C46 1.353(7) . ?
N8 C47 1.405(7) . ?
N7 C7 1.339(7) . ?
N7 C9 1.420(7) . ?
N5 C20 1.352(7) . ?
N5 C21 1.404(7) . ?
C7 N2 1.343(7) . ?
C51 C50 1.369(9) . ?
C51 C52 1.387(8) . ?
C51 H51 0.9300 . ?
C34 C39 1.392(8) . ?
C34 C35 1.398(8) . ?
C27 C28 1.378(8) . ?
C27 C32 1.388(8) . ?
N2 C1 1.379(7) . ?
C45 C44 1.375(8) . ?
C45 C40 1.390(8) . ?
C50 C49 1.368(9) . ?
C50 H50 0.9300 . ?
C10 C11 1.351(9) . ?
C10 C9 1.404(8) . ?
C10 H10 0.9300 . ?
C40 C41 1.380(8) . ?
C39 C38 1.377(9) . ?
C14 C15 1.366(8) . ?
C14 C19 1.393(8) . ?
C9 C8 1.384(8) . ?
C6 C5 1.374(8) . ?
C6 C1 1.379(8) . ?
C8 C13 1.381(8) . ?
C32 C31 1.370(8) . ?
C25 C26 1.364(9) . ?
C25 C24 1.372(9) . ?
C25 H25 0.9300 . ?
C1 C2 1.370(8) . ?
C48 C49 1.372(8) . ?
C48 C47 1.389(8) . ?
C48 H48 0.9300 . ?
C21 C22 1.394(8) . ?
C21 C26 1.392(8) . ?
C13 C12 1.377(9) . ?
C13 H13 0.9300 . ?
C17 C16 1.374(10) . ?
C17 C18 1.374(10) . ?
C17 H17 0.9300 . ?
C22 C23 1.374(8) . ?
C16 C15 1.375(9) . ?
C16 H16 0.9300 . ?
C29 C30 1.370(9) . ?
C29 C28 1.371(8) . ?
C29 H29 0.9300 . ?
C35 C36 1.365(9) . ?
C35 H35 0.9300 . ?
C18 C19 1.385(9) . ?
C18 H18 0.9300 . ?
C26 H26 0.9300 . ?
C5 C4 1.383(9) . ?
C5 H5 0.9300 . ?
C47 C52 1.394(8) . ?
C30 C31 1.389(9) . ?
C30 H30 0.9300 . ?
C28 H28 0.9300 . ?
C49 H49 0.9300 . ?
C2 C3 1.384(9) . ?
C2 H2 0.9300 . ?
C31 H31 0.9300 . ?
C24 C23 1.390(9) . ?
C24 H24 0.9300 . ?
C38 C37 1.381(9) . ?
C38 H38 0.9300 . ?
C15 H15 0.9300 . ?
C23 H23 0.9300 . ?
C12 C11 1.381(9) . ?
C12 H12 0.9300 . ?
C37 C36 1.372(9) . ?
C37 H37 0.9300 . ?
C3 C4 1.372(9) . ?
C3 H3 0.9300 . ?
C11 H11 0.9300 . ?
C4 H4 0.9300 . ?
C36 H36 0.9300 . ?
C41 C42 1.369(9) . ?
C41 H41 0.9300 . ?
C43 C42 1.358(9) . ?
C43 C44 1.385(9) . ?
C43 H43 0.9300 . ?
C42 H42 0.9300 . ?
C44 H44 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
N3 Ni1 N5 169.3(2) . . ?
N3 Ni1 S5 82.36(15) . . ?
N5 Ni1 S5 88.16(16) . . ?
N3 Ni1 S7 92.66(15) . . ?
N5 Ni1 S7 96.95(16) . . ?
S5 Ni1 S7 174.68(7) . . ?
N3 Ni1 Ni2 82.66(15) . . ?
N5 Ni1 Ni2 95.23(15) . . ?
S5 Ni1 Ni2 50.77(6) . . ?
S7 Ni1 Ni2 126.91(6) . . ?
N3 Ni1 Ni4 114.48(15) . . ?
N5 Ni1 Ni4 75.80(15) . . ?
S5 Ni1 Ni4 133.84(6) . . ?
S7 Ni1 Ni4 46.94(5) . . ?
Ni2 Ni1 Ni4 87.40(4) . . ?
N1 Ni4 N8 169.9(2) . . ?
N1 Ni4 S7 82.72(16) . . ?
N8 Ni4 S7 88.35(16) . . ?
N1 Ni4 S8 91.04(16) . . ?
N8 Ni4 S8 97.77(16) . . ?
S7 Ni4 S8 173.65(7) . . ?
N1 Ni4 Ni3 113.13(16) . . ?
N8 Ni4 Ni3 76.70(15) . . ?
S7 Ni4 Ni3 136.81(6) . . ?
S8 Ni4 Ni3 47.24(5) . . ?
N1 Ni4 Ni1 81.85(16) . . ?
N8 Ni4 Ni1 96.00(15) . . ?
S7 Ni4 Ni1 49.86(5) . . ?
S8 Ni4 Ni1 130.54(6) . . ?
Ni3 Ni4 Ni1 91.18(4) . . ?
N2 Ni2 N6 170.0(2) . . ?
N2 Ni2 S6 82.90(16) . . ?
N6 Ni2 S6 88.73(17) . . ?
N2 Ni2 S5 92.03(16) . . ?
N6 Ni2 S5 96.11(17) . . ?
S6 Ni2 S5 174.50(8) . . ?
N2 Ni2 Ni3 81.16(16) . . ?
N6 Ni2 Ni3 97.79(16) . . ?
S6 Ni2 Ni3 51.16(5) . . ?
S5 Ni2 Ni3 130.27(6) . . ?
N2 Ni2 Ni1 114.46(15) . . ?
N6 Ni2 Ni1 75.42(15) . . ?
S6 Ni2 Ni1 137.18(6) . . ?
S5 Ni2 Ni1 47.22(5) . . ?
Ni3 Ni2 Ni1 91.30(4) . . ?
N4 Ni3 N7 169.5(2) . . ?
N4 Ni3 S8 82.43(15) . . ?
N7 Ni3 S8 88.93(15) . . ?
N4 Ni3 S6 90.41(15) . . ?
N7 Ni3 S6 98.23(15) . . ?
S8 Ni3 S6 172.83(7) . . ?
N4 Ni3 Ni4 81.84(15) . . ?
N7 Ni3 Ni4 97.44(15) . . ?
S8 Ni3 Ni4 51.69(5) . . ?
S6 Ni3 Ni4 127.03(6) . . ?
N4 Ni3 Ni2 113.11(16) . . ?
N7 Ni3 Ni2 77.25(15) . . ?
S8 Ni3 Ni2 135.98(6) . . ?
S6 Ni3 Ni2 47.13(5) . . ?
Ni4 Ni3 Ni2 88.50(4) . . ?
C39 S6 Ni2 99.1(2) . . ?
C39 S6 Ni3 108.1(2) . . ?
Ni2 S6 Ni3 81.72(6) . . ?
C52 S7 Ni4 98.8(2) . . ?
C52 S7 Ni1 107.0(2) . . ?
Ni4 S7 Ni1 83.19(7) . . ?
C22 S5 Ni1 99.0(2) . . ?
C22 S5 Ni2 106.9(2) . . ?
Ni1 S5 Ni2 82.01(7) . . ?
C6 S2 C7 91.1(3) . . ?
C8 S8 Ni3 98.8(2) . . ?
C8 S8 Ni4 109.6(2) . . ?
Ni3 S8 Ni4 81.07(6) . . ?
C45 S4 C46 90.3(3) . . ?
C19 S1 C20 90.4(3) . . ?
C32 S3 C33 90.2(3) . . ?
C20 N1 C14 114.2(5) . . ?
C20 N1 Ni4 121.7(4) . . ?
C14 N1 Ni4 124.0(4) . . ?
C33 N3 C27 113.3(5) . . ?
C33 N3 Ni1 119.2(4) . . ?
C27 N3 Ni1 126.0(4) . . ?
C33 N6 C34 121.9(5) . . ?
C33 N6 Ni2 119.5(4) . . ?
C34 N6 Ni2 117.6(4) . . ?
C46 N4 C40 113.5(5) . . ?
C46 N4 Ni3 122.7(4) . . ?
C40 N4 Ni3 123.5(4) . . ?
C46 N8 C47 121.3(5) . . ?
C46 N8 Ni4 120.5(4) . . ?
C47 N8 Ni4 117.9(4) . . ?
C7 N7 C9 120.9(5) . . ?
C7 N7 Ni3 122.2(4) . . ?
C9 N7 Ni3 116.7(4) . . ?
C20 N5 C21 120.7(5) . . ?
C20 N5 Ni1 120.7(4) . . ?
C21 N5 Ni1 118.5(4) . . ?
N7 C7 N2 121.0(6) . . ?
N7 C7 S2 127.5(5) . . ?
N2 C7 S2 111.0(5) . . ?
C50 C51 C52 120.2(7) . . ?
C50 C51 H51 119.9 . . ?
C52 C51 H51 119.9 . . ?
C39 C34 C35 116.2(6) . . ?
C39 C34 N6 117.5(6) . . ?
C35 C34 N6 126.1(6) . . ?
N3 C27 C28 126.9(6) . . ?
N3 C27 C32 114.6(6) . . ?
C28 C27 C32 118.5(6) . . ?
C7 N2 C1 113.2(5) . . ?
C7 N2 Ni2 123.7(4) . . ?
C1 N2 Ni2 122.8(4) . . ?
N3 C33 N6 123.5(5) . . ?
N3 C33 S3 112.5(5) . . ?
N6 C33 S3 123.8(5) . . ?
C44 C45 C40 121.1(6) . . ?
C44 C45 S4 128.8(6) . . ?
C40 C45 S4 110.1(5) . . ?
C51 C50 C49 118.9(7) . . ?
C51 C50 H50 120.6 . . ?
C49 C50 H50 120.6 . . ?
C11 C10 C9 121.5(7) . . ?
C11 C10 H10 119.2 . . ?
C9 C10 H10 119.2 . . ?
C41 C40 C45 119.9(6) . . ?
C41 C40 N4 126.4(6) . . ?
C45 C40 N4 113.7(5) . . ?
C38 C39 C34 122.3(7) . . ?
C38 C39 S6 121.5(5) . . ?
C34 C39 S6 116.2(5) . . ?
C15 C14 C19 120.7(6) . . ?
C15 C14 N1 126.1(6) . . ?
C19 C14 N1 113.2(6) . . ?
C8 C9 C10 116.5(6) . . ?
C8 C9 N7 116.7(6) . . ?
C10 C9 N7 126.6(6) . . ?
C5 C6 C1 121.9(6) . . ?
C5 C6 S2 128.7(6) . . ?
C1 C6 S2 109.3(5) . . ?
C13 C8 C9 121.7(6) . . ?
C13 C8 S8 120.8(5) . . ?
C9 C8 S8 117.5(5) . . ?
C31 C32 C27 123.3(6) . . ?
C31 C32 S3 127.3(6) . . ?
C27 C32 S3 109.4(5) . . ?
C26 C25 C24 122.7(7) . . ?
C26 C25 H25 118.6 . . ?
C24 C25 H25 118.6 . . ?
N4 C46 N8 121.7(6) . . ?
N4 C46 S4 112.3(5) . . ?
N8 C46 S4 125.9(5) . . ?
C2 C1 N2 124.7(6) . . ?
C2 C1 C6 120.1(6) . . ?
N2 C1 C6 115.2(6) . . ?
C49 C48 C47 121.4(7) . . ?
C49 C48 H48 119.3 . . ?
C47 C48 H48 119.3 . . ?
C22 C21 C26 116.3(6) . . ?
C22 C21 N5 116.5(6) . . ?
C26 C21 N5 127.1(6) . . ?
C12 C13 C8 120.5(7) . . ?
C12 C13 H13 119.7 . . ?
C8 C13 H13 119.7 . . ?
C16 C17 C18 120.0(7) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C23 C22 C21 122.6(6) . . ?
C23 C22 S5 120.4(5) . . ?
C21 C22 S5 117.0(5) . . ?
C17 C16 C15 122.1(7) . . ?
C17 C16 H16 119.0 . . ?
C15 C16 H16 119.0 . . ?
C30 C29 C28 121.8(7) . . ?
C30 C29 H29 119.1 . . ?
C28 C29 H29 119.1 . . ?
C36 C35 C34 121.3(7) . . ?
C36 C35 H35 119.4 . . ?
C34 C35 H35 119.4 . . ?
C17 C18 C19 118.6(7) . . ?
C17 C18 H18 120.7 . . ?
C19 C18 H18 120.7 . . ?
C25 C26 C21 120.7(7) . . ?
C25 C26 H26 119.7 . . ?
C21 C26 H26 119.7 . . ?
C6 C5 C4 117.3(7) . . ?
C6 C5 H5 121.4 . . ?
C4 C5 H5 121.4 . . ?
C48 C47 C52 116.5(6) . . ?
C48 C47 N8 126.9(6) . . ?
C52 C47 N8 116.6(6) . . ?
C51 C52 C47 121.7(6) . . ?
C51 C52 S7 120.8(5) . . ?
C47 C52 S7 117.6(5) . . ?
N1 C20 N5 123.2(6) . . ?
N1 C20 S1 112.1(5) . . ?
N5 C20 S1 124.6(5) . . ?
C29 C30 C31 120.6(7) . . ?
C29 C30 H30 119.7 . . ?
C31 C30 H30 119.7 . . ?
C29 C28 C27 118.9(6) . . ?
C29 C28 H28 120.5 . . ?
C27 C28 H28 120.5 . . ?
C50 C49 C48 121.3(7) . . ?
C50 C49 H49 119.4 . . ?
C48 C49 H49 119.4 . . ?
C1 C2 C3 118.8(6) . . ?
C1 C2 H2 120.6 . . ?
C3 C2 H2 120.6 . . ?
C32 C31 C30 116.8(7) . . ?
C32 C31 H31 121.6 . . ?
C30 C31 H31 121.6 . . ?
C18 C19 C14 120.4(7) . . ?
C18 C19 S1 129.5(6) . . ?
C14 C19 S1 110.0(5) . . ?
C25 C24 C23 117.7(7) . . ?
C25 C24 H24 121.2 . . ?
C23 C24 H24 121.2 . . ?
C39 C38 C37 120.0(7) . . ?
C39 C38 H38 120.0 . . ?
C37 C38 H38 120.0 . . ?
C14 C15 C16 118.1(7) . . ?
C14 C15 H15 120.9 . . ?
C16 C15 H15 120.9 . . ?
C22 C23 C24 119.8(7) . . ?
C22 C23 H23 120.1 . . ?
C24 C23 H23 120.1 . . ?
C13 C12 C11 118.2(7) . . ?
C13 C12 H12 120.9 . . ?
C11 C12 H12 120.9 . . ?
C36 C37 C38 118.5(7) . . ?
C36 C37 H37 120.7 . . ?
C38 C37 H37 120.7 . . ?
C4 C3 C2 120.3(7) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C10 C11 C12 121.5(7) . . ?
C10 C11 H11 119.2 . . ?
C12 C11 H11 119.2 . . ?
C3 C4 C5 121.5(7) . . ?
C3 C4 H4 119.3 . . ?
C5 C4 H4 119.3 . . ?
C35 C36 C37 121.6(7) . . ?
C35 C36 H36 119.2 . . ?
C37 C36 H36 119.2 . . ?
C42 C41 C40 118.6(7) . . ?
C42 C41 H41 120.7 . . ?
C40 C41 H41 120.7 . . ?
C42 C43 C44 121.0(7) . . ?
C42 C43 H43 119.5 . . ?
C44 C43 H43 119.5 . . ?
C43 C42 C41 121.6(7) . . ?
C43 C42 H42 119.2 . . ?
C41 C42 H42 119.2 . . ?
C45 C44 C43 117.8(7) . . ?
C45 C44 H44 121.1 . . ?
C43 C44 H44 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 Ni1 Ni4 N1 156.5(2) . . . . ?
N5 Ni1 Ni4 N1 -26.7(2) . . . . ?
S5 Ni1 Ni4 N1 -99.92(17) . . . . ?
S7 Ni1 Ni4 N1 87.33(16) . . . . ?
Ni2 Ni1 Ni4 N1 -122.77(16) . . . . ?
N3 Ni1 Ni4 N8 -13.5(2) . . . . ?
N5 Ni1 Ni4 N8 163.2(2) . . . . ?
S5 Ni1 Ni4 N8 90.03(17) . . . . ?
S7 Ni1 Ni4 N8 -82.72(16) . . . . ?
Ni2 Ni1 Ni4 N8 67.18(15) . . . . ?
N3 Ni1 Ni4 S7 69.18(17) . . . . ?
N5 Ni1 Ni4 S7 -114.03(16) . . . . ?
S5 Ni1 Ni4 S7 172.76(10) . . . . ?
Ni2 Ni1 Ni4 S7 149.90(7) . . . . ?
N3 Ni1 Ni4 S8 -119.14(17) . . . . ?
N5 Ni1 Ni4 S8 57.64(17) . . . . ?
S5 Ni1 Ni4 S8 -15.57(11) . . . . ?
S7 Ni1 Ni4 S8 171.68(9) . . . . ?
Ni2 Ni1 Ni4 S8 -38.42(7) . . . . ?
N3 Ni1 Ni4 Ni3 -90.29(16) . . . . ?
N5 Ni1 Ni4 Ni3 86.49(15) . . . . ?
S5 Ni1 Ni4 Ni3 13.28(8) . . . . ?
S7 Ni1 Ni4 Ni3 -159.47(7) . . . . ?
Ni2 Ni1 Ni4 Ni3 -9.57(3) . . . . ?
N3 Ni1 Ni2 N2 -154.5(2) . . . . ?
N5 Ni1 Ni2 N2 14.9(2) . . . . ?
S5 Ni1 Ni2 N2 -68.42(18) . . . . ?
S7 Ni1 Ni2 N2 117.66(18) . . . . ?
Ni4 Ni1 Ni2 N2 90.39(18) . . . . ?
N3 Ni1 Ni2 N6 26.9(2) . . . . ?
N5 Ni1 Ni2 N6 -163.7(2) . . . . ?
S5 Ni1 Ni2 N6 112.99(17) . . . . ?
S7 Ni1 Ni2 N6 -60.93(18) . . . . ?
Ni4 Ni1 Ni2 N6 -88.20(16) . . . . ?
N3 Ni1 Ni2 S6 98.55(17) . . . . ?
N5 Ni1 Ni2 S6 -92.01(18) . . . . ?
S5 Ni1 Ni2 S6 -175.34(11) . . . . ?
S7 Ni1 Ni2 S6 10.74(12) . . . . ?
Ni4 Ni1 Ni2 S6 -16.53(9) . . . . ?
N3 Ni1 Ni2 S5 -86.11(16) . . . . ?
N5 Ni1 Ni2 S5 83.32(17) . . . . ?
S7 Ni1 Ni2 S5 -173.93(9) . . . . ?
Ni4 Ni1 Ni2 S5 158.80(7) . . . . ?
N3 Ni1 Ni2 Ni3 124.60(15) . . . . ?
N5 Ni1 Ni2 Ni3 -65.97(16) . . . . ?
S5 Ni1 Ni2 Ni3 -149.29(7) . . . . ?
S7 Ni1 Ni2 Ni3 36.78(7) . . . . ?
Ni4 Ni1 Ni2 Ni3 9.51(3) . . . . ?
N1 Ni4 Ni3 N4 -155.2(2) . . . . ?
N8 Ni4 Ni3 N4 27.3(2) . . . . ?
S7 Ni4 Ni3 N4 100.12(17) . . . . ?
S8 Ni4 Ni3 N4 -86.77(16) . . . . ?
Ni1 Ni4 Ni3 N4 123.19(15) . . . . ?
N1 Ni4 Ni3 N7 14.3(2) . . . . ?
N8 Ni4 Ni3 N7 -163.2(2) . . . . ?
S7 Ni4 Ni3 N7 -90.41(17) . . . . ?
S8 Ni4 Ni3 N7 82.69(16) . . . . ?
Ni1 Ni4 Ni3 N7 -67.35(15) . . . . ?
N1 Ni4 Ni3 S8 -68.39(19) . . . . ?
N8 Ni4 Ni3 S8 114.07(17) . . . . ?
S7 Ni4 Ni3 S8 -173.10(10) . . . . ?
Ni1 Ni4 Ni3 S8 -150.04(7) . . . . ?
N1 Ni4 Ni3 S6 120.52(19) . . . . ?
N8 Ni4 Ni3 S6 -57.02(17) . . . . ?
S7 Ni4 Ni3 S6 15.81(12) . . . . ?
S8 Ni4 Ni3 S6 -171.09(9) . . . . ?
Ni1 Ni4 Ni3 S6 38.87(7) . . . . ?
N1 Ni4 Ni3 Ni2 91.23(18) . . . . ?
N8 Ni4 Ni3 Ni2 -86.30(15) . . . . ?
S7 Ni4 Ni3 Ni2 -13.48(9) . . . . ?
S8 Ni4 Ni3 Ni2 159.63(7) . . . . ?
Ni1 Ni4 Ni3 Ni2 9.59(3) . . . . ?
N2 Ni2 Ni3 N4 155.3(2) . . . . ?
N6 Ni2 Ni3 N4 -14.7(2) . . . . ?
S6 Ni2 Ni3 N4 67.33(17) . . . . ?
S5 Ni2 Ni3 N4 -119.56(17) . . . . ?
Ni1 Ni2 Ni3 N4 -90.14(16) . . . . ?
N2 Ni2 Ni3 N7 -26.3(2) . . . . ?
N6 Ni2 Ni3 N7 163.8(2) . . . . ?
S6 Ni2 Ni3 N7 -114.22(16) . . . . ?
S5 Ni2 Ni3 N7 58.88(16) . . . . ?
Ni1 Ni2 Ni3 N7 88.30(15) . . . . ?
N2 Ni2 Ni3 S8 -101.08(17) . . . . ?
N6 Ni2 Ni3 S8 88.93(17) . . . . ?
S6 Ni2 Ni3 S8 170.95(10) . . . . ?
S5 Ni2 Ni3 S8 -15.94(12) . . . . ?
Ni1 Ni2 Ni3 S8 13.48(9) . . . . ?
N2 Ni2 Ni3 S6 87.97(16) . . . . ?
N6 Ni2 Ni3 S6 -82.02(16) . . . . ?
S5 Ni2 Ni3 S6 173.11(10) . . . . ?
Ni1 Ni2 Ni3 S6 -157.47(7) . . . . ?
N2 Ni2 Ni3 Ni4 -124.22(15) . . . . ?
N6 Ni2 Ni3 Ni4 65.79(15) . . . . ?
S6 Ni2 Ni3 Ni4 147.80(7) . . . . ?
S5 Ni2 Ni3 Ni4 -39.09(8) . . . . ?
Ni1 Ni2 Ni3 Ni4 -9.67(3) . . . . ?
N2 Ni2 S6 C39 168.5(3) . . . . ?
N6 Ni2 S6 C39 -6.1(3) . . . . ?
S5 Ni2 S6 C39 145.6(8) . . . . ?
Ni3 Ni2 S6 C39 -107.2(2) . . . . ?
Ni1 Ni2 S6 C39 -72.9(2) . . . . ?
N2 Ni2 S6 Ni3 -84.35(16) . . . . ?
N6 Ni2 S6 Ni3 101.07(15) . . . . ?
S5 Ni2 S6 Ni3 -107.2(8) . . . . ?
Ni1 Ni2 S6 Ni3 34.30(10) . . . . ?
N4 Ni3 S6 C39 -25.0(3) . . . . ?
N7 Ni3 S6 C39 161.0(3) . . . . ?
S8 Ni3 S6 C39 -21.9(7) . . . . ?
Ni4 Ni3 S6 C39 55.1(3) . . . . ?
Ni2 Ni3 S6 C39 97.0(2) . . . . ?
N4 Ni3 S6 Ni2 -121.92(16) . . . . ?
N7 Ni3 S6 Ni2 63.99(16) . . . . ?
S8 Ni3 S6 Ni2 -118.8(6) . . . . ?
Ni4 Ni3 S6 Ni2 -41.85(8) . . . . ?
N1 Ni4 S7 C52 168.3(3) . . . . ?
N8 Ni4 S7 C52 -7.0(3) . . . . ?
S8 Ni4 S7 C52 157.4(7) . . . . ?
Ni3 Ni4 S7 C52 -75.4(2) . . . . ?
Ni1 Ni4 S7 C52 -106.3(2) . . . . ?
N1 Ni4 S7 Ni1 -85.46(17) . . . . ?
N8 Ni4 S7 Ni1 99.28(15) . . . . ?
S8 Ni4 S7 Ni1 -96.4(7) . . . . ?
Ni3 Ni4 S7 Ni1 30.82(10) . . . . ?
N3 Ni1 S7 C52 -24.4(3) . . . . ?
N5 Ni1 S7 C52 160.3(3) . . . . ?
S5 Ni1 S7 C52 -3.8(9) . . . . ?
Ni2 Ni1 S7 C52 58.4(2) . . . . ?
Ni4 Ni1 S7 C52 97.2(2) . . . . ?
N3 Ni1 S7 Ni4 -121.61(16) . . . . ?
N5 Ni1 S7 Ni4 63.12(16) . . . . ?
S5 Ni1 S7 Ni4 -101.0(8) . . . . ?
Ni2 Ni1 S7 Ni4 -38.79(8) . . . . ?
N3 Ni1 S5 C22 -167.3(3) . . . . ?
N5 Ni1 S5 C22 7.7(3) . . . . ?
S7 Ni1 S5 C22 171.9(8) . . . . ?
Ni2 Ni1 S5 C22 105.9(2) . . . . ?
Ni4 Ni1 S5 C22 75.9(2) . . . . ?
N3 Ni1 S5 Ni2 86.74(16) . . . . ?
N5 Ni1 S5 Ni2 -98.27(15) . . . . ?
S7 Ni1 S5 Ni2 65.9(8) . . . . ?
Ni4 Ni1 S5 Ni2 -30.06(9) . . . . ?
N2 Ni2 S5 C22 25.1(3) . . . . ?
N6 Ni2 S5 C22 -160.6(3) . . . . ?
S6 Ni2 S5 C22 47.8(8) . . . . ?
Ni3 Ni2 S5 C22 -55.0(2) . . . . ?
Ni1 Ni2 S5 C22 -97.0(2) . . . . ?
N2 Ni2 S5 Ni1 122.12(16) . . . . ?
N6 Ni2 S5 Ni1 -63.63(15) . . . . ?
S6 Ni2 S5 Ni1 144.8(8) . . . . ?
Ni3 Ni2 S5 Ni1 41.99(8) . . . . ?
N4 Ni3 S8 C8 -165.8(3) . . . . ?
N7 Ni3 S8 C8 8.3(3) . . . . ?
S6 Ni3 S8 C8 -169.0(6) . . . . ?
Ni4 Ni3 S8 C8 108.6(2) . . . . ?
Ni2 Ni3 S8 C8 78.6(2) . . . . ?
N4 Ni3 S8 Ni4 85.56(16) . . . . ?
N7 Ni3 S8 Ni4 -100.36(15) . . . . ?
S6 Ni3 S8 Ni4 82.4(6) . . . . ?
Ni2 Ni3 S8 Ni4 -30.05(9) . . . . ?
N1 Ni4 S8 C8 25.0(3) . . . . ?
N8 Ni4 S8 C8 -159.9(3) . . . . ?
S7 Ni4 S8 C8 35.9(7) . . . . ?
Ni3 Ni4 S8 C8 -96.2(2) . . . . ?
Ni1 Ni4 S8 C8 -55.1(2) . . . . ?
N1 Ni4 S8 Ni3 121.23(17) . . . . ?
N8 Ni4 S8 Ni3 -63.74(15) . . . . ?
S7 Ni4 S8 Ni3 132.0(6) . . . . ?
Ni1 Ni4 S8 Ni3 41.07(8) . . . . ?
N8 Ni4 N1 C20 98.7(13) . . . . ?
S7 Ni4 N1 C20 70.6(5) . . . . ?
S8 Ni4 N1 C20 -110.6(5) . . . . ?
Ni3 Ni4 N1 C20 -67.5(5) . . . . ?
Ni1 Ni4 N1 C20 20.3(5) . . . . ?
N8 Ni4 N1 C14 -76.8(14) . . . . ?
S7 Ni4 N1 C14 -104.8(5) . . . . ?
S8 Ni4 N1 C14 74.0(5) . . . . ?
Ni3 Ni4 N1 C14 117.0(4) . . . . ?
Ni1 Ni4 N1 C14 -155.2(5) . . . . ?
N5 Ni1 N3 C33 -95.6(12) . . . . ?
S5 Ni1 N3 C33 -67.6(4) . . . . ?
S7 Ni1 N3 C33 110.6(4) . . . . ?
Ni2 Ni1 N3 C33 -16.3(4) . . . . ?
Ni4 Ni1 N3 C33 67.4(5) . . . . ?
N5 Ni1 N3 C27 69.7(13) . . . . ?
S5 Ni1 N3 C27 97.7(5) . . . . ?
S7 Ni1 N3 C27 -84.1(5) . . . . ?
Ni2 Ni1 N3 C27 149.0(5) . . . . ?
Ni4 Ni1 N3 C27 -127.3(4) . . . . ?
N2 Ni2 N6 C33 144.9(12) . . . . ?
S6 Ni2 N6 C33 177.6(4) . . . . ?
S5 Ni2 N6 C33 0.2(5) . . . . ?
Ni3 Ni2 N6 C33 -131.9(4) . . . . ?
Ni1 Ni2 N6 C33 -42.6(4) . . . . ?
N2 Ni2 N6 C34 -23.7(16) . . . . ?
S6 Ni2 N6 C34 9.1(4) . . . . ?
S5 Ni2 N6 C34 -168.3(4) . . . . ?
Ni3 Ni2 N6 C34 59.6(4) . . . . ?
Ni1 Ni2 N6 C34 148.9(5) . . . . ?
N7 Ni3 N4 C46 -109.6(12) . . . . ?
S8 Ni3 N4 C46 -75.0(5) . . . . ?
S6 Ni3 N4 C46 104.6(5) . . . . ?
Ni4 Ni3 N4 C46 -22.8(5) . . . . ?
Ni2 Ni3 N4 C46 62.0(5) . . . . ?
N7 Ni3 N4 C40 64.0(13) . . . . ?
S8 Ni3 N4 C40 98.5(5) . . . . ?
S6 Ni3 N4 C40 -81.8(5) . . . . ?
Ni4 Ni3 N4 C40 150.8(5) . . . . ?
Ni2 Ni3 N4 C40 -124.4(4) . . . . ?
N1 Ni4 N8 C46 154.6(11) . . . . ?
S7 Ni4 N8 C46 -177.6(5) . . . . ?
S8 Ni4 N8 C46 4.1(5) . . . . ?
Ni3 Ni4 N8 C46 -38.4(4) . . . . ?
Ni1 Ni4 N8 C46 -128.2(4) . . . . ?
N1 Ni4 N8 C47 -18.9(15) . . . . ?
S7 Ni4 N8 C47 9.0(4) . . . . ?
S8 Ni4 N8 C47 -169.3(4) . . . . ?
Ni3 Ni4 N8 C47 148.1(4) . . . . ?
Ni1 Ni4 N8 C47 58.3(4) . . . . ?
N4 Ni3 N7 C7 -151.8(10) . . . . ?
S8 Ni3 N7 C7 174.0(5) . . . . ?
S6 Ni3 N7 C7 -6.4(5) . . . . ?
Ni4 Ni3 N7 C7 122.9(5) . . . . ?
Ni2 Ni3 N7 C7 36.1(4) . . . . ?
N4 Ni3 N7 C9 22.6(14) . . . . ?
S8 Ni3 N7 C9 -11.6(4) . . . . ?
S6 Ni3 N7 C9 168.0(4) . . . . ?
Ni4 Ni3 N7 C9 -62.7(4) . . . . ?
Ni2 Ni3 N7 C9 -149.5(4) . . . . ?
N3 Ni1 N5 C20 -156.9(10) . . . . ?
S5 Ni1 N5 C20 175.3(5) . . . . ?
S7 Ni1 N5 C20 -3.3(5) . . . . ?
Ni2 Ni1 N5 C20 125.0(5) . . . . ?
Ni4 Ni1 N5 C20 39.0(4) . . . . ?
N3 Ni1 N5 C21 20.5(14) . . . . ?
S5 Ni1 N5 C21 -7.3(4) . . . . ?
S7 Ni1 N5 C21 174.2(4) . . . . ?
Ni2 Ni1 N5 C21 -57.6(4) . . . . ?
Ni4 Ni1 N5 C21 -143.6(4) . . . . ?
C9 N7 C7 N2 153.2(6) . . . . ?
Ni3 N7 C7 N2 -32.6(8) . . . . ?
C9 N7 C7 S2 -36.0(8) . . . . ?
Ni3 N7 C7 S2 138.2(4) . . . . ?
C6 S2 C7 N7 -169.4(6) . . . . ?
C6 S2 C7 N2 2.1(5) . . . . ?
C33 N6 C34 C39 -177.3(6) . . . . ?
Ni2 N6 C34 C39 -9.0(7) . . . . ?
C33 N6 C34 C35 8.3(10) . . . . ?
Ni2 N6 C34 C35 176.5(5) . . . . ?
C33 N3 C27 C28 -177.6(6) . . . . ?
Ni1 N3 C27 C28 16.3(9) . . . . ?
C33 N3 C27 C32 0.9(8) . . . . ?
Ni1 N3 C27 C32 -165.2(4) . . . . ?
N7 C7 N2 C1 168.3(5) . . . . ?
S2 C7 N2 C1 -3.9(7) . . . . ?
N7 C7 N2 Ni2 -5.8(8) . . . . ?
S2 C7 N2 Ni2 -178.0(3) . . . . ?
N6 Ni2 N2 C7 108.5(13) . . . . ?
S6 Ni2 N2 C7 75.4(5) . . . . ?
S5 Ni2 N2 C7 -106.7(5) . . . . ?
Ni3 Ni2 N2 C7 23.8(5) . . . . ?
Ni1 Ni2 N2 C7 -63.6(5) . . . . ?
N6 Ni2 N2 C1 -65.0(15) . . . . ?
S6 Ni2 N2 C1 -98.1(5) . . . . ?
S5 Ni2 N2 C1 79.8(5) . . . . ?
Ni3 Ni2 N2 C1 -149.7(5) . . . . ?
Ni1 Ni2 N2 C1 122.9(4) . . . . ?
C27 N3 C33 N6 -176.7(5) . . . . ?
Ni1 N3 C33 N6 -9.6(8) . . . . ?
C27 N3 C33 S3 -2.2(7) . . . . ?
Ni1 N3 C33 S3 164.9(3) . . . . ?
C34 N6 C33 N3 -143.4(6) . . . . ?
Ni2 N6 C33 N3 48.6(8) . . . . ?
C34 N6 C33 S3 42.7(8) . . . . ?
Ni2 N6 C33 S3 -125.3(4) . . . . ?
C32 S3 C33 N3 2.3(5) . . . . ?
C32 S3 C33 N6 176.8(5) . . . . ?
C46 S4 C45 C44 -179.8(7) . . . . ?
C46 S4 C45 C40 -0.1(5) . . . . ?
C52 C51 C50 C49 0.9(10) . . . . ?
C44 C45 C40 C41 0.6(10) . . . . ?
S4 C45 C40 C41 -179.1(5) . . . . ?
C44 C45 C40 N4 -178.1(6) . . . . ?
S4 C45 C40 N4 2.2(7) . . . . ?
C46 N4 C40 C41 177.5(6) . . . . ?
Ni3 N4 C40 C41 3.4(9) . . . . ?
C46 N4 C40 C45 -3.9(8) . . . . ?
Ni3 N4 C40 C45 -178.0(4) . . . . ?
C35 C34 C39 C38 -3.5(10) . . . . ?
N6 C34 C39 C38 -178.5(6) . . . . ?
C35 C34 C39 S6 177.9(5) . . . . ?
N6 C34 C39 S6 2.8(8) . . . . ?
Ni2 S6 C39 C38 -175.2(5) . . . . ?
Ni3 S6 C39 C38 100.6(6) . . . . ?
Ni2 S6 C39 C34 3.4(5) . . . . ?
Ni3 S6 C39 C34 -80.8(5) . . . . ?
C20 N1 C14 C15 179.1(6) . . . . ?
Ni4 N1 C14 C15 -5.1(9) . . . . ?
C20 N1 C14 C19 1.7(8) . . . . ?
Ni4 N1 C14 C19 177.5(4) . . . . ?
C11 C10 C9 C8 -3.2(10) . . . . ?
C11 C10 C9 N7 -179.4(7) . . . . ?
C7 N7 C9 C8 -174.6(6) . . . . ?
Ni3 N7 C9 C8 10.9(7) . . . . ?
C7 N7 C9 C10 1.5(10) . . . . ?
Ni3 N7 C9 C10 -172.9(5) . . . . ?
C7 S2 C6 C5 177.6(7) . . . . ?
C7 S2 C6 C1 0.2(5) . . . . ?
C10 C9 C8 C13 3.3(9) . . . . ?
N7 C9 C8 C13 179.8(6) . . . . ?
C10 C9 C8 S8 -179.3(5) . . . . ?
N7 C9 C8 S8 -2.7(8) . . . . ?
Ni3 S8 C8 C13 172.3(5) . . . . ?
Ni4 S8 C8 C13 -104.2(5) . . . . ?
Ni3 S8 C8 C9 -5.3(5) . . . . ?
Ni4 S8 C8 C9 78.3(5) . . . . ?
N3 C27 C32 C31 -177.7(6) . . . . ?
C28 C27 C32 C31 0.9(10) . . . . ?
N3 C27 C32 S3 0.8(7) . . . . ?
C28 C27 C32 S3 179.5(5) . . . . ?
C33 S3 C32 C31 176.8(7) . . . . ?
C33 S3 C32 C27 -1.7(5) . . . . ?
C40 N4 C46 N8 -172.1(5) . . . . ?
Ni3 N4 C46 N8 2.1(8) . . . . ?
C40 N4 C46 S4 3.7(7) . . . . ?
Ni3 N4 C46 S4 177.9(3) . . . . ?
C47 N8 C46 N4 -149.8(6) . . . . ?
Ni4 N8 C46 N4 37.0(8) . . . . ?
C47 N8 C46 S4 35.0(8) . . . . ?
Ni4 N8 C46 S4 -138.2(4) . . . . ?
C45 S4 C46 N4 -2.1(5) . . . . ?
C45 S4 C46 N8 173.5(6) . . . . ?
C7 N2 C1 C2 -175.9(6) . . . . ?
Ni2 N2 C1 C2 -1.8(9) . . . . ?
C7 N2 C1 C6 4.3(8) . . . . ?
Ni2 N2 C1 C6 178.4(5) . . . . ?
C5 C6 C1 C2 0.1(11) . . . . ?
S2 C6 C1 C2 177.7(5) . . . . ?
C5 C6 C1 N2 179.9(6) . . . . ?
S2 C6 C1 N2 -2.5(7) . . . . ?
C20 N5 C21 C22 -179.4(6) . . . . ?
Ni1 N5 C21 C22 3.2(7) . . . . ?
C20 N5 C21 C26 -3.0(10) . . . . ?
Ni1 N5 C21 C26 179.5(5) . . . . ?
C9 C8 C13 C12 -2.1(10) . . . . ?
S8 C8 C13 C12 -179.5(5) . . . . ?
C26 C21 C22 C23 5.3(10) . . . . ?
N5 C21 C22 C23 -177.9(6) . . . . ?
C26 C21 C22 S5 -172.2(5) . . . . ?
N5 C21 C22 S5 4.5(8) . . . . ?
Ni1 S5 C22 C23 173.8(5) . . . . ?
Ni2 S5 C22 C23 -101.9(5) . . . . ?
Ni1 S5 C22 C21 -8.6(5) . . . . ?
Ni2 S5 C22 C21 75.7(5) . . . . ?
C18 C17 C16 C15 -0.3(12) . . . . ?
C39 C34 C35 C36 3.7(10) . . . . ?
N6 C34 C35 C36 178.3(7) . . . . ?
C16 C17 C18 C19 0.2(12) . . . . ?
C24 C25 C26 C21 0.6(12) . . . . ?
C22 C21 C26 C25 -4.4(10) . . . . ?
N5 C21 C26 C25 179.3(6) . . . . ?
C1 C6 C5 C4 2.4(11) . . . . ?
S2 C6 C5 C4 -174.6(6) . . . . ?
C49 C48 C47 C52 2.3(9) . . . . ?
C49 C48 C47 N8 -179.7(6) . . . . ?
C46 N8 C47 C48 1.2(9) . . . . ?
Ni4 N8 C47 C48 174.5(5) . . . . ?
C46 N8 C47 C52 179.2(5) . . . . ?
Ni4 N8 C47 C52 -7.4(7) . . . . ?
C50 C51 C52 C47 -0.4(10) . . . . ?
C50 C51 C52 S7 179.8(5) . . . . ?
C48 C47 C52 C51 -1.1(9) . . . . ?
N8 C47 C52 C51 -179.4(5) . . . . ?
C48 C47 C52 S7 178.6(5) . . . . ?
N8 C47 C52 S7 0.4(7) . . . . ?
Ni4 S7 C52 C51 -174.8(5) . . . . ?
Ni1 S7 C52 C51 99.7(5) . . . . ?
Ni4 S7 C52 C47 5.5(5) . . . . ?
Ni1 S7 C52 C47 -80.0(5) . . . . ?
C14 N1 C20 N5 177.3(5) . . . . ?
Ni4 N1 C20 N5 1.4(8) . . . . ?
C14 N1 C20 S1 0.5(7) . . . . ?
Ni4 N1 C20 S1 -175.3(3) . . . . ?
C21 N5 C20 N1 142.3(6) . . . . ?
Ni1 N5 C20 N1 -40.3(8) . . . . ?
C21 N5 C20 S1 -41.3(8) . . . . ?
Ni1 N5 C20 S1 136.1(4) . . . . ?
C19 S1 C20 N1 -2.0(5) . . . . ?
C19 S1 C20 N5 -178.7(6) . . . . ?
C28 C29 C30 C31 0.4(11) . . . . ?
C30 C29 C28 C27 0.0(11) . . . . ?
N3 C27 C28 C29 177.9(6) . . . . ?
C32 C27 C28 C29 -0.6(10) . . . . ?
C51 C50 C49 C48 0.3(11) . . . . ?
C47 C48 C49 C50 -1.9(11) . . . . ?
N2 C1 C2 C3 177.0(7) . . . . ?
C6 C1 C2 C3 -3.2(11) . . . . ?
C27 C32 C31 C30 -0.6(11) . . . . ?
S3 C32 C31 C30 -178.9(5) . . . . ?
C29 C30 C31 C32 -0.1(11) . . . . ?
C17 C18 C19 C14 1.7(11) . . . . ?
C17 C18 C19 S1 178.2(6) . . . . ?
C15 C14 C19 C18 -3.6(10) . . . . ?
N1 C14 C19 C18 174.0(6) . . . . ?
C15 C14 C19 S1 179.3(5) . . . . ?
N1 C14 C19 S1 -3.2(7) . . . . ?
C20 S1 C19 C18 -173.9(7) . . . . ?
C20 S1 C19 C14 2.9(5) . . . . ?
C26 C25 C24 C23 2.5(12) . . . . ?
C34 C39 C38 C37 2.5(11) . . . . ?
S6 C39 C38 C37 -178.9(5) . . . . ?
C19 C14 C15 C16 3.4(10) . . . . ?
N1 C14 C15 C16 -173.8(6) . . . . ?
C17 C16 C15 C14 -1.5(11) . . . . ?
C21 C22 C23 C24 -2.4(10) . . . . ?
S5 C22 C23 C24 175.0(5) . . . . ?
C25 C24 C23 C22 -1.5(11) . . . . ?
C8 C13 C12 C11 0.7(11) . . . . ?
C39 C38 C37 C36 -1.5(11) . . . . ?
C1 C2 C3 C4 3.7(12) . . . . ?
C9 C10 C11 C12 2.0(12) . . . . ?
C13 C12 C11 C10 -0.7(12) . . . . ?
C2 C3 C4 C5 -1.1(13) . . . . ?
C6 C5 C4 C3 -1.9(13) . . . . ?
C34 C35 C36 C37 -3.0(12) . . . . ?
C38 C37 C36 C35 1.8(12) . . . . ?
C45 C40 C41 C42 -0.7(10) . . . . ?
N4 C40 C41 C42 177.8(6) . . . . ?
C44 C43 C42 C41 1.3(12) . . . . ?
C40 C41 C42 C43 -0.2(11) . . . . ?
C40 C45 C44 C43 0.5(11) . . . . ?
S4 C45 C44 C43 -179.9(6) . . . . ?
C42 C43 C44 C45 -1.4(12) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.113
_database_code_depnum_ccdc_archive 'CCDC 1013610'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_5

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H36 N6 O2 Ni6 S15'
_chemical_formula_sum            'C46 H36 N6 O2 Ni6 S15'
_chemical_formula_weight         1537.95

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

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

_cell_length_a                   15.384(3)
_cell_length_b                   15.673(3)
_cell_length_c                   25.018(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.45(3)
_cell_angle_gamma                90.00
_cell_volume                     5867(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2904
_exptl_absorpt_coefficient_mu    2.455
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.649
_exptl_absorpt_correction_T_max  0.727
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_measurement_device_type  'Saturn70 (4x4 bin mode)'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            50528
_diffrn_reflns_av_R_equivalents  0.1125
_diffrn_reflns_av_sigmaI/netI    0.1087
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         2.30
_diffrn_reflns_theta_max         27.84
_reflns_number_total             13854
_reflns_number_gt                8562
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0561P)²+0.0000P] 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     SHELXL
_refine_ls_extinction_coef       0.00251(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         13854
_refine_ls_number_parameters     623
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0508
_refine_ls_wR_factor_ref         0.1381
_refine_ls_wR_factor_gt          0.1208
_refine_ls_goodness_of_fit_ref   0.908
_refine_ls_restrained_S_all      0.908
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni4 Ni 0.43625(4) 0.82332(3) 0.16706(2) 0.03286(15) Uani 1 1 d . . .
Ni3 Ni 0.32014(4) 0.81648(3) 0.06474(2) 0.03435(15) Uani 1 1 d . . .
Ni1 Ni 0.18610(4) 0.76126(4) 0.11249(2) 0.03490(15) Uani 1 1 d . . .
Ni2 Ni 0.29420(4) 0.64593(3) 0.07870(2) 0.03303(15) Uani 1 1 d . . .
Ni5 Ni 0.30518(4) 0.77079(3) 0.21658(2) 0.03393(15) Uani 1 1 d . . .
Ni6 Ni 0.41214(4) 0.65185(3) 0.18364(2) 0.03282(15) Uani 1 1 d . . .
S13 S 0.26552(7) 0.65772(6) 0.16091(4) 0.0317(2) Uani 1 1 d . . .
S14 S 0.41979(7) 0.71990(6) 0.10641(4) 0.0311(2) Uani 1 1 d . . .
S15 S 0.29129(7) 0.85416(6) 0.14434(4) 0.0320(2) Uani 1 1 d . . .
S10 S 0.35754(10) 0.87537(8) 0.27768(5) 0.0528(4) Uani 1 1 d . . .
S4 S 0.44327(10) 1.04774(8) 0.27789(5) 0.0530(4) Uani 1 1 d . . .
S2 S 0.39576(10) 0.63400(8) -0.07542(5) 0.0524(3) Uani 1 1 d . . .
S8 S 0.33776(11) 0.78327(8) -0.01920(5) 0.0561(4) Uani 1 1 d . . .
S11 S 0.40584(10) 0.57905(10) 0.25951(6) 0.0589(4) Uani 1 1 d . . .
S12 S 0.58174(9) 0.80058(8) 0.19983(6) 0.0544(4) Uani 1 1 d . . .
S5 S 0.28752(10) 0.56303(9) 0.33681(5) 0.0570(4) Uani 1 1 d . . .
S3 S 0.11574(10) 1.02012(9) 0.00362(7) 0.0682(5) Uani 1 1 d . . .
S1 S -0.01602(10) 0.55472(11) 0.05921(6) 0.0677(4) Uani 1 1 d . . .
S6 S 0.71158(9) 0.66079(9) 0.23163(6) 0.0574(4) Uani 1 1 d . . .
S7 S 0.16996(9) 0.57102(9) 0.04541(6) 0.0568(4) Uani 1 1 d . . .
N6 N 0.5420(2) 0.6309(2) 0.19967(14) 0.0345(8) Uani 1 1 d . . .
N2 N 0.3379(3) 0.6172(2) 0.01302(14) 0.0365(9) Uani 1 1 d . . .
N5 N 0.2846(3) 0.6972(2) 0.27627(14) 0.0399(9) Uani 1 1 d . . .
N3 N 0.2499(3) 0.9187(2) 0.03356(14) 0.0393(9) Uani 1 1 d . . .
C22 C 0.4992(3) 1.0022(3) 0.19279(18) 0.0367(10) Uani 1 1 d . . .
N4 N 0.4519(3) 0.9330(2) 0.20591(14) 0.0372(9) Uani 1 1 d . . .
C28 C 0.4178(3) 0.9460(3) 0.24898(17) 0.0399(11) Uani 1 1 d . . .
C14 C 0.3544(3) 0.6759(3) -0.02146(17) 0.0409(11) Uani 1 1 d . . .
C35 C 0.3233(3) 0.6225(3) 0.28700(18) 0.0433(12) Uani 1 1 d . . .
C15 C 0.2812(3) 0.9905(3) 0.01034(18) 0.0415(11) Uani 1 1 d . . .
C29 C 0.2240(3) 0.7126(3) 0.30966(18) 0.0429(11) Uani 1 1 d . . .
C7 C 0.0848(3) 0.6109(3) 0.07127(19) 0.0466(12) Uani 1 1 d . . .
N1 N 0.0840(2) 0.6820(2) 0.09899(15) 0.0403(9) Uani 1 1 d . . .
C23 C 0.5407(3) 1.0067(3) 0.1485(2) 0.0476(12) Uani 1 1 d . . .
H23 H 0.5379 0.9610 0.1245 0.057 Uiso 1 1 calc R . .
C36 C 0.5839(3) 0.5504(3) 0.21083(17) 0.0390(11) Uani 1 1 d . . .
C34 C 0.2176(3) 0.6463(3) 0.34570(19) 0.0468(12) Uani 1 1 d . . .
C2 C -0.0193(4) 0.7671(4) 0.1411(2) 0.0630(16) Uani 1 1 d . . .
H2 H 0.0231 0.8089 0.1542 0.076 Uiso 1 1 calc R . .
C25 C 0.5907(4) 1.1483(3) 0.1773(2) 0.0556(14) Uani 1 1 d . . .
H25 H 0.6215 1.1973 0.1716 0.067 Uiso 1 1 calc R . .
C8 C 0.3574(3) 0.5339(3) -0.00216(17) 0.0370(10) Uani 1 1 d . . .
C21 C 0.1650(3) 0.9261(3) 0.03281(19) 0.0468(12) Uani 1 1 d . . .
C42 C 0.5998(3) 0.6937(3) 0.20728(18) 0.0399(11) Uani 1 1 d . . .
C20 C 0.2172(4) 1.0510(3) -0.0083(2) 0.0537(14) Uani 1 1 d . . .
C9 C 0.3465(3) 0.4597(3) 0.0252(2) 0.0464(12) Uani 1 1 d . . .
H9 H 0.3243 0.4614 0.0567 0.056 Uiso 1 1 calc R . .
C24 C 0.5857(4) 1.0805(3) 0.1414(2) 0.0529(13) Uani 1 1 d . . .
H24 H 0.6131 1.0847 0.1120 0.063 Uiso 1 1 calc R . .
C27 C 0.5041(3) 1.0708(3) 0.22881(18) 0.0422(11) Uani 1 1 d . . .
C1 C 0.0018(3) 0.6961(4) 0.1121(2) 0.0489(13) Uani 1 1 d . . .
C13 C 0.3895(3) 0.5314(3) -0.05001(18) 0.0419(11) Uani 1 1 d . . .
C6 C -0.0612(4) 0.6315(4) 0.0925(2) 0.0580(15) Uani 1 1 d . . .
C32 C 0.1146(4) 0.7242(4) 0.3825(2) 0.0676(17) Uani 1 1 d . . .
H32 H 0.0767 0.7288 0.4064 0.081 Uiso 1 1 calc R . .
C31 C 0.1217(4) 0.7932(4) 0.3476(2) 0.0612(15) Uani 1 1 d . . .
H31 H 0.0897 0.8429 0.3496 0.073 Uiso 1 1 calc R . .
C33 C 0.1622(4) 0.6508(4) 0.3820(2) 0.0594(15) Uani 1 1 d . . .
H33 H 0.1576 0.6055 0.4052 0.071 Uiso 1 1 calc R . .
C41 C 0.6773(3) 0.5552(3) 0.2295(2) 0.0464(12) Uani 1 1 d . . .
C30 C 0.1750(4) 0.7882(4) 0.3105(2) 0.0532(13) Uani 1 1 d . . .
H30 H 0.1785 0.8332 0.2868 0.064 Uiso 1 1 calc R . .
C12 C 0.4145(4) 0.4545(3) -0.0696(2) 0.0542(14) Uani 1 1 d . . .
H12 H 0.4381 0.4530 -0.1006 0.065 Uiso 1 1 calc R . .
C11 C 0.4036(4) 0.3801(3) -0.0419(2) 0.0578(14) Uani 1 1 d . . .
H11 H 0.4193 0.3280 -0.0547 0.069 Uiso 1 1 calc R . .
C26 C 0.5512(4) 1.1451(3) 0.2214(2) 0.0536(14) Uani 1 1 d . . .
H26 H 0.5556 1.1908 0.2456 0.064 Uiso 1 1 calc R . .
C10 C 0.3692(4) 0.3827(3) 0.0051(2) 0.0545(14) Uani 1 1 d . . .
H10 H 0.3614 0.3322 0.0230 0.065 Uiso 1 1 calc R . .
S9 S 0.09885(9) 0.85261(10) 0.05590(6) 0.0637(4) Uani 1 1 d . . .
C37 C 0.5413(4) 0.4720(3) 0.2048(2) 0.0496(13) Uani 1 1 d . . .
H37 H 0.4796 0.4678 0.1926 0.060 Uiso 1 1 calc R . .
C38 C 0.5942(4) 0.4002(3) 0.2175(2) 0.0625(16) Uani 1 1 d . . .
H38 H 0.5667 0.3470 0.2131 0.075 Uiso 1 1 calc R . .
C16 C 0.3680(4) 1.0031(3) 0.0068(2) 0.0564(14) Uani 1 1 d . . .
H16 H 0.4113 0.9618 0.0194 0.068 Uiso 1 1 calc R . .
C17 C 0.3898(4) 1.0786(4) -0.0160(3) 0.0694(17) Uani 1 1 d . . .
H17 H 0.4484 1.0882 -0.0185 0.083 Uiso 1 1 calc R . .
C40 C 0.7295(4) 0.4811(3) 0.2423(2) 0.0607(15) Uani 1 1 d . . .
H40 H 0.7913 0.4842 0.2544 0.073 Uiso 1 1 calc R . .
C39 C 0.6858(4) 0.4039(4) 0.2364(2) 0.0675(17) Uani 1 1 d . . .
H39 H 0.7183 0.3538 0.2452 0.081 Uiso 1 1 calc R . .
C18 C 0.3247(5) 1.1401(4) -0.0352(3) 0.0771(19) Uani 1 1 d . . .
H18 H 0.3402 1.1904 -0.0504 0.092 Uiso 1 1 calc R . .
C3 C -0.1052(5) 0.7731(5) 0.1498(3) 0.082(2) Uani 1 1 d . . .
H3 H -0.1207 0.8191 0.1692 0.098 Uiso 1 1 calc R . .
C4 C -0.1689(5) 0.7091(6) 0.1291(3) 0.094(3) Uani 1 1 d . . .
H4 H -0.2265 0.7141 0.1344 0.112 Uiso 1 1 calc R . .
C19 C 0.2377(5) 1.1269(4) -0.0320(3) 0.0723(18) Uani 1 1 d . . .
H19 H 0.1937 1.1673 -0.0453 0.087 Uiso 1 1 calc R . .
C5 C -0.1474(4) 0.6392(5) 0.1010(3) 0.076(2) Uani 1 1 d . . .
H5 H -0.1901 0.5976 0.0878 0.092 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
Ni4 N4 1.961(3) . ?
Ni4 S14 2.1945(11) . ?
Ni4 S15 2.2226(13) . ?
Ni4 S12 2.2260(15) . ?
Ni4 Ni5 2.7277(10) . ?
Ni4 Ni6 2.7577(9) . ?
Ni4 Ni3 2.7620(12) . ?
Ni3 N3 1.987(3) . ?
Ni3 S15 2.2188(12) . ?
Ni3 S14 2.2326(12) . ?
Ni3 S8 2.2404(14) . ?
Ni3 Ni2 2.7371(9) . ?
Ni3 Ni1 2.7523(10) . ?
Ni1 N1 1.969(4) . ?
Ni1 S15 2.1849(13) . ?
Ni1 S13 2.2148(12) . ?
Ni1 S9 2.2298(14) . ?
Ni1 Ni2 2.7207(9) . ?
Ni1 Ni5 2.8178(12) . ?
Ni2 N2 1.967(4) . ?
Ni2 S13 2.2092(13) . ?
Ni2 S14 2.2214(13) . ?
Ni2 S7 2.2326(15) . ?
Ni2 Ni6 2.8245(12) . ?
Ni5 N5 1.970(4) . ?
Ni5 S15 2.1998(12) . ?
Ni5 S13 2.2490(12) . ?
Ni5 S10 2.2581(14) . ?
Ni5 Ni6 2.7373(9) . ?
Ni6 N6 1.972(4) . ?
Ni6 S13 2.1961(13) . ?
Ni6 S14 2.2341(12) . ?
Ni6 S11 2.2360(14) . ?
S10 C28 1.706(5) . ?
S4 C27 1.747(5) . ?
S4 C28 1.757(4) . ?
S2 C13 1.740(5) . ?
S2 C14 1.749(5) . ?
S8 C14 1.705(5) . ?
S11 C35 1.718(5) . ?
S12 C42 1.701(5) . ?
S5 C34 1.738(6) . ?
S5 C35 1.745(5) . ?
S3 C20 1.725(6) . ?
S3 C21 1.739(5) . ?
S1 C6 1.702(6) . ?
S1 C7 1.748(5) . ?
S6 C41 1.733(5) . ?
S6 C42 1.763(5) . ?
S7 C7 1.709(6) . ?
N6 C42 1.310(6) . ?
N6 C36 1.415(5) . ?
N2 C14 1.325(6) . ?
N2 C8 1.411(5) . ?
N5 C35 1.313(6) . ?
N5 C29 1.410(6) . ?
N3 C21 1.307(6) . ?
N3 C15 1.402(6) . ?
C22 N4 1.388(5) . ?
C22 C27 1.394(6) . ?
C22 C23 1.403(7) . ?
N4 C28 1.319(6) . ?
C15 C20 1.368(7) . ?
C15 C16 1.373(7) . ?
C29 C34 1.394(6) . ?
C29 C30 1.407(7) . ?
C7 N1 1.314(6) . ?
N1 C1 1.395(6) . ?
C23 C24 1.382(6) . ?
C36 C37 1.384(6) . ?
C36 C41 1.406(6) . ?
C34 C33 1.385(7) . ?
C2 C3 1.390(8) . ?
C2 C1 1.408(8) . ?
C25 C26 1.380(8) . ?
C25 C24 1.381(7) . ?
C8 C9 1.380(6) . ?
C8 C13 1.398(6) . ?
C21 S9 1.723(5) . ?
C20 C19 1.398(7) . ?
C9 C10 1.383(6) . ?
C27 C26 1.406(6) . ?
C1 C6 1.408(7) . ?
C13 C12 1.389(6) . ?
C6 C5 1.396(8) . ?
C32 C33 1.365(8) . ?
C32 C31 1.411(8) . ?
C31 C30 1.377(7) . ?
C41 C40 1.406(7) . ?
C12 C11 1.387(7) . ?
C11 C10 1.399(7) . ?
C37 C38 1.380(7) . ?
C38 C39 1.381(8) . ?
C16 C17 1.388(7) . ?
C17 C18 1.392(8) . ?
C40 C39 1.374(7) . ?
C18 C19 1.375(9) . ?
C3 C4 1.414(11) . ?
C4 C5 1.382(10) . ?

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
N4 Ni4 S14 166.16(11) . . ?
N4 Ni4 S15 86.35(11) . . ?
S14 Ni4 S15 92.07(5) . . ?
N4 Ni4 S12 87.76(12) . . ?
S14 Ni4 S12 94.64(5) . . ?
S15 Ni4 S12 172.78(5) . . ?
N4 Ni4 Ni5 93.31(12) . . ?
S14 Ni4 Ni5 96.46(4) . . ?
S15 Ni4 Ni5 51.54(3) . . ?
S12 Ni4 Ni5 124.79(5) . . ?
N4 Ni4 Ni6 141.69(11) . . ?
S14 Ni4 Ni6 52.13(3) . . ?
S15 Ni4 Ni6 95.06(3) . . ?
S12 Ni4 Ni6 86.99(4) . . ?
Ni5 Ni4 Ni6 59.87(2) . . ?
N4 Ni4 Ni3 118.14(10) . . ?
S14 Ni4 Ni3 52.02(3) . . ?
S15 Ni4 Ni3 51.49(4) . . ?
S12 Ni4 Ni3 135.50(5) . . ?
Ni5 Ni4 Ni3 91.27(3) . . ?
Ni6 Ni4 Ni3 91.20(2) . . ?
N3 Ni3 S15 86.21(11) . . ?
N3 Ni3 S14 168.90(12) . . ?
S15 Ni3 S14 91.16(5) . . ?
N3 Ni3 S8 89.58(11) . . ?
S15 Ni3 S8 175.04(6) . . ?
S14 Ni3 S8 93.47(5) . . ?
N3 Ni3 Ni2 139.03(12) . . ?
S15 Ni3 Ni2 94.58(4) . . ?
S14 Ni3 Ni2 51.90(3) . . ?
S8 Ni3 Ni2 86.89(4) . . ?
N3 Ni3 Ni1 91.71(12) . . ?
S15 Ni3 Ni1 50.77(4) . . ?
S14 Ni3 Ni1 94.96(4) . . ?
S8 Ni3 Ni1 126.88(5) . . ?
Ni2 Ni3 Ni1 59.42(2) . . ?
N3 Ni3 Ni4 120.52(11) . . ?
S15 Ni3 Ni4 51.61(3) . . ?
S14 Ni3 Ni4 50.78(3) . . ?
S8 Ni3 Ni4 133.21(5) . . ?
Ni2 Ni3 Ni4 90.10(2) . . ?
Ni1 Ni3 Ni4 89.90(3) . . ?
N1 Ni1 S15 167.56(12) . . ?
N1 Ni1 S13 87.04(11) . . ?
S15 Ni1 S13 91.22(5) . . ?
N1 Ni1 S9 87.57(12) . . ?
S15 Ni1 S9 95.11(6) . . ?
S13 Ni1 S9 172.64(6) . . ?
N1 Ni1 Ni2 92.78(12) . . ?
S15 Ni1 Ni2 95.83(4) . . ?
S13 Ni1 Ni2 51.96(3) . . ?
S9 Ni1 Ni2 123.40(5) . . ?
N1 Ni1 Ni3 140.55(12) . . ?
S15 Ni1 Ni3 51.87(3) . . ?
S13 Ni1 Ni3 95.40(4) . . ?
S9 Ni1 Ni3 85.62(5) . . ?
Ni2 Ni1 Ni3 60.01(2) . . ?
N1 Ni1 Ni5 120.88(11) . . ?
S15 Ni1 Ni5 50.24(3) . . ?
S13 Ni1 Ni5 51.40(3) . . ?
S9 Ni1 Ni5 135.95(5) . . ?
Ni2 Ni1 Ni5 90.54(3) . . ?
Ni3 Ni1 Ni5 89.59(3) . . ?
N2 Ni2 S13 167.95(11) . . ?
N2 Ni2 S14 86.47(11) . . ?
S13 Ni2 S14 90.77(5) . . ?
N2 Ni2 S7 89.86(11) . . ?
S13 Ni2 S7 92.99(6) . . ?
S14 Ni2 S7 176.24(5) . . ?
N2 Ni2 Ni1 139.82(11) . . ?
S13 Ni2 Ni1 52.14(3) . . ?
S14 Ni2 Ni1 96.11(4) . . ?
S7 Ni2 Ni1 86.17(5) . . ?
N2 Ni2 Ni3 91.62(11) . . ?
S13 Ni2 Ni3 95.96(3) . . ?
S14 Ni2 Ni3 52.27(3) . . ?
S7 Ni2 Ni3 127.12(5) . . ?
Ni1 Ni2 Ni3 60.57(2) . . ?
N2 Ni2 Ni6 120.90(11) . . ?
S13 Ni2 Ni6 49.92(4) . . ?
S14 Ni2 Ni6 50.86(3) . . ?
S7 Ni2 Ni6 132.31(5) . . ?
Ni1 Ni2 Ni6 89.79(3) . . ?
Ni3 Ni2 Ni6 90.31(2) . . ?
N5 Ni5 S15 165.59(12) . . ?
N5 Ni5 S13 86.54(11) . . ?
S15 Ni5 S13 89.93(4) . . ?
N5 Ni5 S10 90.39(11) . . ?
S15 Ni5 S10 94.37(5) . . ?
S13 Ni5 S10 173.67(5) . . ?
N5 Ni5 Ni4 141.91(12) . . ?
S15 Ni5 Ni4 52.30(4) . . ?
S13 Ni5 Ni4 94.55(4) . . ?
S10 Ni5 Ni4 84.45(4) . . ?
N5 Ni5 Ni6 92.47(12) . . ?
S15 Ni5 Ni6 96.17(4) . . ?
S13 Ni5 Ni6 51.12(4) . . ?
S10 Ni5 Ni6 123.60(5) . . ?
Ni4 Ni5 Ni6 60.61(2) . . ?
N5 Ni5 Ni1 119.01(11) . . ?
S15 Ni5 Ni1 49.78(3) . . ?
S13 Ni5 Ni1 50.32(3) . . ?
S10 Ni5 Ni1 135.80(4) . . ?
Ni4 Ni5 Ni1 89.24(3) . . ?
Ni6 Ni5 Ni1 89.59(3) . . ?
N6 Ni6 S13 172.22(11) . . ?
N6 Ni6 S14 90.03(11) . . ?
S13 Ni6 S14 90.78(5) . . ?
N6 Ni6 S11 89.11(11) . . ?
S13 Ni6 S11 89.81(6) . . ?
S14 Ni6 S11 177.79(6) . . ?
N6 Ni6 Ni5 134.72(10) . . ?
S13 Ni6 Ni5 52.87(3) . . ?
S14 Ni6 Ni5 95.25(4) . . ?
S11 Ni6 Ni5 86.80(5) . . ?
N6 Ni6 Ni4 91.56(10) . . ?
S13 Ni6 Ni4 94.94(3) . . ?
S14 Ni6 Ni4 50.85(3) . . ?
S11 Ni6 Ni4 131.22(5) . . ?
Ni5 Ni6 Ni4 59.52(2) . . ?
N6 Ni6 Ni2 125.81(10) . . ?
S13 Ni6 Ni2 50.33(4) . . ?
S14 Ni6 Ni2 50.46(3) . . ?
S11 Ni6 Ni2 128.83(5) . . ?
Ni5 Ni6 Ni2 90.06(3) . . ?
Ni4 Ni6 Ni2 88.40(2) . . ?
Ni6 S13 Ni2 79.76(5) . . ?
Ni6 S13 Ni1 125.11(5) . . ?
Ni2 S13 Ni1 75.90(4) . . ?
Ni6 S13 Ni5 76.01(4) . . ?
Ni2 S13 Ni5 123.94(5) . . ?
Ni1 S13 Ni5 78.28(4) . . ?
Ni4 S14 Ni2 123.60(6) . . ?
Ni4 S14 Ni3 77.20(4) . . ?
Ni2 S14 Ni3 75.83(4) . . ?
Ni4 S14 Ni6 77.02(4) . . ?
Ni2 S14 Ni6 78.68(5) . . ?
Ni3 S14 Ni6 123.98(6) . . ?
Ni1 S15 Ni5 79.98(5) . . ?
Ni1 S15 Ni3 77.36(4) . . ?
Ni5 S15 Ni3 125.30(5) . . ?
Ni1 S15 Ni4 124.22(5) . . ?
Ni5 S15 Ni4 76.16(4) . . ?
Ni3 S15 Ni4 76.91(5) . . ?
C28 S10 Ni5 109.23(15) . . ?
C27 S4 C28 90.2(2) . . ?
C13 S2 C14 90.2(2) . . ?
C14 S8 Ni3 108.20(16) . . ?
C35 S11 Ni6 108.63(16) . . ?
C42 S12 Ni4 108.83(17) . . ?
C34 S5 C35 89.9(2) . . ?
C20 S3 C21 89.2(3) . . ?
C6 S1 C7 90.4(3) . . ?
C41 S6 C42 90.2(2) . . ?
C7 S7 Ni2 109.35(16) . . ?
C42 N6 C36 112.3(4) . . ?
C42 N6 Ni6 121.7(3) . . ?
C36 N6 Ni6 125.5(3) . . ?
C14 N2 C8 112.4(4) . . ?
C14 N2 Ni2 122.7(3) . . ?
C8 N2 Ni2 124.9(3) . . ?
C35 N5 C29 111.3(4) . . ?
C35 N5 Ni5 122.1(3) . . ?
C29 N5 Ni5 126.4(3) . . ?
C21 N3 C15 111.2(4) . . ?
C21 N3 Ni3 121.8(3) . . ?
C15 N3 Ni3 127.0(3) . . ?
N4 C22 C27 113.8(4) . . ?
N4 C22 C23 125.8(4) . . ?
C27 C22 C23 120.4(4) . . ?
C28 N4 C22 113.7(4) . . ?
C28 N4 Ni4 120.9(3) . . ?
C22 N4 Ni4 125.4(3) . . ?
N4 C28 S10 127.0(3) . . ?
N4 C28 S4 112.6(3) . . ?
S10 C28 S4 120.4(3) . . ?
N2 C14 S8 127.6(4) . . ?
N2 C14 S2 113.6(3) . . ?
S8 C14 S2 118.7(3) . . ?
N5 C35 S11 127.8(4) . . ?
N5 C35 S5 114.7(4) . . ?
S11 C35 S5 117.4(3) . . ?
C20 C15 C16 120.8(5) . . ?
C20 C15 N3 114.1(5) . . ?
C16 C15 N3 125.1(4) . . ?
C34 C29 N5 114.3(5) . . ?
C34 C29 C30 120.0(5) . . ?
N5 C29 C30 125.6(4) . . ?
N1 C7 S7 127.8(4) . . ?
N1 C7 S1 113.7(4) . . ?
S7 C7 S1 118.5(3) . . ?
C7 N1 C1 112.2(4) . . ?
C7 N1 Ni1 121.3(3) . . ?
C1 N1 Ni1 126.2(4) . . ?
C24 C23 C22 118.5(5) . . ?
C37 C36 C41 120.3(4) . . ?
C37 C36 N6 126.1(4) . . ?
C41 C36 N6 113.6(4) . . ?
C29 C34 C33 122.2(5) . . ?
C29 C34 S5 109.7(4) . . ?
C33 C34 S5 128.1(4) . . ?
C3 C2 C1 118.5(6) . . ?
C26 C25 C24 121.6(5) . . ?
C9 C8 C13 120.6(4) . . ?
C9 C8 N2 126.0(4) . . ?
C13 C8 N2 113.3(4) . . ?
N3 C21 S9 127.0(4) . . ?
N3 C21 S3 114.7(4) . . ?
S9 C21 S3 118.3(3) . . ?
N6 C42 S12 129.5(4) . . ?
N6 C42 S6 113.9(3) . . ?
S12 C42 S6 116.6(3) . . ?
C15 C20 C19 121.3(6) . . ?
C15 C20 S3 110.8(4) . . ?
C19 C20 S3 127.9(5) . . ?
C8 C9 C10 119.1(5) . . ?
C25 C24 C23 121.0(5) . . ?
C22 C27 C26 120.4(5) . . ?
C22 C27 S4 109.7(3) . . ?
C26 C27 S4 129.9(4) . . ?
N1 C1 C2 125.2(5) . . ?
N1 C1 C6 113.2(5) . . ?
C2 C1 C6 121.6(5) . . ?
C12 C13 C8 120.6(5) . . ?
C12 C13 S2 129.0(4) . . ?
C8 C13 S2 110.3(3) . . ?
C5 C6 C1 119.2(6) . . ?
C5 C6 S1 130.2(5) . . ?
C1 C6 S1 110.6(4) . . ?
C33 C32 C31 121.4(6) . . ?
C30 C31 C32 121.2(6) . . ?
C32 C33 C34 117.6(6) . . ?
C36 C41 C40 121.0(5) . . ?
C36 C41 S6 110.0(3) . . ?
C40 C41 S6 128.9(4) . . ?
C31 C30 C29 117.5(5) . . ?
C11 C12 C13 118.5(5) . . ?
C12 C11 C10 120.6(5) . . ?
C25 C26 C27 118.1(5) . . ?
C9 C10 C11 120.5(5) . . ?
C21 S9 Ni1 109.06(17) . . ?
C38 C37 C36 117.4(5) . . ?
C39 C38 C37 123.0(5) . . ?
C15 C16 C17 118.8(5) . . ?
C16 C17 C18 120.5(6) . . ?
C39 C40 C41 117.7(5) . . ?
C38 C39 C40 120.5(5) . . ?
C19 C18 C17 120.5(6) . . ?
C2 C3 C4 119.8(7) . . ?
C5 C4 C3 121.5(7) . . ?
C18 C19 C20 118.1(6) . . ?
C4 C5 C6 119.5(7) . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.84
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.732
_refine_diff_density_min         -0.967
_refine_diff_density_rms         0.157

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.041 0.237 0.111 303 54 ' '
2 0.041 -0.237 0.889 303 54 ' '
3 0.541 0.737 0.389 303 53 ' '
4 0.459 0.263 0.611 303 54 ' '
_platon_squeeze_details          
;
The PLATON SQUEEZE procedure was used to treat 
regions of diffuse solvent which could not be modeled 
properly in terms of atomic sites. Their contribution to 
the diffraction pattern was removed and modified F² was
written to a new HKL file. The number of located electrons, 
215 in four voids per unit cell, is included in the formula, formula weight, 
calculated density, and F(000). There are four formula units 
in one unit cell. On base of charge balance considerations, volume/count_electrons 
analysis, TG analyses and elemental analyses, this residual electron density 
was assigned to two  ethanol molecules. So SQUEEZE removed these 
disordered units per unit cell. The tentative formula for compound 1 
is presented as in the text.
See refs. (a) O. V. Dolomanov, D. B. Cordes, N. R. Champness, A. J. Blake,
L. R. Hanton, G. B. Jameson, M. Schroder and C. Wilson. Chem. Commun.
2004, 642; (b) Y. Du, A. L. Thompson and D. O. Hare. Chem. Commun. 2008, 5987;
(c) Y. F. Bi, X. T. Wang, W. P. Liao, X. F. Wang, X. W. Wang, H. J. Zhang,
and S. Gao, J. Am. Chem. Soc. 2009, 131, 11650.
;
_database_code_depnum_ccdc_archive 'CCDC 1013611'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_6

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H30 Co4 N13 O4 S6'
_chemical_formula_sum            'C42 H30 Co4 N13 O4 S6'
_chemical_formula_weight         1208.93

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'
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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   'P 21 3'

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

_cell_length_a                   18.737(2)
_cell_length_b                   18.737(2)
_cell_length_c                   18.737(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6578.3(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2436
_exptl_absorpt_coefficient_mu    1.223
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.802
_exptl_absorpt_correction_T_max  0.832
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  SCX-MINI
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            57198
_diffrn_reflns_av_R_equivalents  0.0821
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.08
_diffrn_reflns_theta_max         24.93
_reflns_number_total             3866
_reflns_number_gt                3635
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       PROCESS-AUTO
_computing_cell_refinement       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_structure_solution    DirectMethod
_computing_structure_refinement  SHELXL
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_molecular_graphics    ?

_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. 'Omit' restraint instruction 
 was used in the refinement. 
;

_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)+(0.0675P)²+5.2141P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.52(3)
_refine_ls_number_reflns         3866
_refine_ls_number_parameters     208
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0562
_refine_ls_wR_factor_ref         0.1345
_refine_ls_wR_factor_gt          0.1318
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_restrained_S_all      1.183
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.002

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1305(4) 0.2917(4) 0.9631(3) 0.0575(18) Uani 1 1 d . . .
C2 C 0.0591(5) 0.3082(6) 0.9565(5) 0.089(3) Uani 1 1 d . . .
H2A H 0.0380 0.3118 0.9117 0.107 Uiso 1 1 calc R . .
C3 C 0.0195(5) 0.3192(7) 1.0175(6) 0.111(4) Uani 1 1 d . . .
H3 H -0.0288 0.3297 1.0132 0.134 Uiso 1 1 calc R . .
C4 C 0.0490(7) 0.3151(8) 1.0842(6) 0.139(5) Uani 1 1 d . . .
H4A H 0.0209 0.3256 1.1237 0.167 Uiso 1 1 calc R . .
C5 C 0.1205(7) 0.2956(7) 1.0946(4) 0.116(4) Uani 1 1 d . . .
H5 H 0.1397 0.2901 1.1401 0.139 Uiso 1 1 calc R . .
C6 C 0.1625(5) 0.2844(4) 1.0316(4) 0.068(2) Uani 1 1 d . . .
C7 C 0.2440(4) 0.2641(3) 0.9494(3) 0.0453(15) Uani 1 1 d . . .
C8 C 0.0629(5) 0.2488(6) 0.4516(4) 0.089(3) Uani 1 1 d . . .
H8 H 0.0807 0.2541 0.4056 0.106 Uiso 1 1 calc R . .
C9 C -0.0107(5) 0.2528(7) 0.4642(5) 0.107(4) Uani 1 1 d . . .
H9 H -0.0411 0.2604 0.4258 0.129 Uiso 1 1 calc R . .
C10 C -0.0396(4) 0.2459(5) 0.5310(5) 0.083(3) Uani 1 1 d . . .
H10 H -0.0885 0.2495 0.5384 0.099 Uiso 1 1 calc R . .
C11 C 0.0072(3) 0.2334(4) 0.5873(4) 0.0569(18) Uani 1 1 d . . .
C12 C 0.0618(3) 0.2179(3) 0.6921(3) 0.0426(13) Uani 1 1 d . . .
C13 C 0.0090(4) 0.3903(4) 0.7633(5) 0.071(2) Uani 1 1 d . . .
H13 H 0.0018 0.3412 0.7661 0.085 Uiso 1 1 calc R . .
C14 C 0.0756(3) 0.4186(3) 0.7710(4) 0.0483(15) Uani 1 1 d . . .
Co1 Co 0.16816(4) 0.28408(4) 0.80666(4) 0.0338(2) Uani 1 1 d . . .
Co2 Co 0.30863(3) 0.19137(3) 0.80863(3) 0.0348(3) Uani 1 3 d S . .
N1 N 0.1845(3) 0.2773(3) 0.9133(2) 0.0446(12) Uani 1 1 d . . .
N2 N 0.2318(4) 0.2676(3) 1.0212(3) 0.0639(16) Uani 1 1 d . . .
H2 H 0.2629 0.2603 1.0542 0.077 Uiso 1 1 calc R . .
N3 N 0.1429(3) 0.3864(2) 0.7814(3) 0.0431(11) Uani 1 1 d . . .
N4 N -0.0031(3) 0.2273(3) 0.6604(3) 0.0553(14) Uani 1 1 d . . .
H4 H -0.0436 0.2290 0.6820 0.066 Uiso 1 1 calc R . .
N5 N 0.8027(5) 0.1973(5) 0.6973(5) 0.116(5) Uani 1 3 d S . .
O1 O 0.24819(17) 0.25181(17) 0.74819(17) 0.0273(12) Uani 1 3 d S . .
O2 O 0.8529(5) 0.2318(11) 0.7135(10) 0.268(9) Uani 1 1 d . . .
S3 S 0.07299(8) 0.20575(8) 0.78330(8) 0.0456(4) Uani 1 1 d . . .
S4 S 0.32922(9) 0.24682(9) 0.91675(8) 0.0515(4) 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
C1 C2 1.380(11) . ?
C1 N1 1.403(8) . ?
C1 C6 1.423(10) . ?
C2 C3 1.378(11) . ?
C3 C4 1.370(16) . ?
C4 C5 1.401(17) . ?
C5 C6 1.435(11) . ?
C6 N2 1.350(10) . ?
C7 N1 1.326(8) . ?
C7 N2 1.367(7) . ?
C7 S4 1.741(7) . ?
C8 C9 1.401(13) . ?
C8 C13 1.407(10) 12_565 ?
C9 C10 1.369(12) . ?
C10 C11 1.391(10) . ?
C11 N4 1.388(9) . ?
C11 C14 1.409(9) 12_565 ?
C12 N3 1.337(7) 12_565 ?
C12 N4 1.366(8) . ?
C12 S3 1.737(6) . ?
C13 C14 1.363(10) . ?
C13 C8 1.407(10) 6_456 ?
C14 C11 1.409(9) 6_456 ?
C14 N3 1.412(7) . ?
Co1 O1 1.9530(18) . ?
Co1 N1 2.025(4) . ?
Co1 N3 2.031(5) . ?
Co1 S3 2.3507(16) . ?
Co2 O1 1.962(5) . ?
Co2 S4 2.3092(16) . ?
Co2 S4 2.3092(16) 6_456 ?
Co2 S4 2.3092(16) 12_565 ?
N3 C12 1.337(7) 6_456 ?
N5 O2 1.181(12) 10_646 ?
N5 O2 1.181(12) . ?
N5 O2 1.181(12) 7_665 ?
O1 Co1 1.9530(18) 12_565 ?
O1 Co1 1.9530(18) 6_456 ?

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
C2 C1 N1 133.1(7) . . ?
C2 C1 C6 120.8(7) . . ?
N1 C1 C6 106.1(6) . . ?
C3 C2 C1 118.7(9) . . ?
C4 C3 C2 122.2(10) . . ?
C3 C4 C5 121.8(8) . . ?
C4 C5 C6 116.6(9) . . ?
N2 C6 C1 107.3(6) . . ?
N2 C6 C5 132.9(9) . . ?
C1 C6 C5 119.8(9) . . ?
N1 C7 N2 110.7(6) . . ?
N1 C7 S4 128.7(4) . . ?
N2 C7 S4 120.5(5) . . ?
C9 C8 C13 119.6(8) . 12_565 ?
C10 C9 C8 122.5(7) . . ?
C9 C10 C11 117.4(7) . . ?
N4 C11 C10 132.4(7) . . ?
N4 C11 C14 106.6(5) . 12_565 ?
C10 C11 C14 120.9(7) . 12_565 ?
N3 C12 N4 110.2(5) 12_565 . ?
N3 C12 S3 126.3(4) 12_565 . ?
N4 C12 S3 123.5(5) . . ?
C14 C13 C8 118.3(7) . 6_456 ?
C13 C14 C11 121.3(6) . 6_456 ?
C13 C14 N3 131.7(6) . . ?
C11 C14 N3 106.9(6) 6_456 . ?
O1 Co1 N1 114.7(2) . . ?
O1 Co1 N3 109.91(18) . . ?
N1 Co1 N3 108.9(2) . . ?
O1 Co1 S3 106.54(5) . . ?
N1 Co1 S3 105.03(15) . . ?
N3 Co1 S3 111.69(15) . . ?
O1 Co2 S4 110.07(5) . . ?
O1 Co2 S4 110.07(5) . 6_456 ?
S4 Co2 S4 108.86(5) . 6_456 ?
O1 Co2 S4 110.07(5) . 12_565 ?
S4 Co2 S4 108.86(5) . 12_565 ?
S4 Co2 S4 108.86(5) 6_456 12_565 ?
C7 N1 C1 107.6(5) . . ?
C7 N1 Co1 130.0(4) . . ?
C1 N1 Co1 122.3(4) . . ?
C6 N2 C7 108.2(6) . . ?
C12 N3 C14 107.8(5) 6_456 . ?
C12 N3 Co1 121.5(4) 6_456 . ?
C14 N3 Co1 130.1(4) . . ?
C12 N4 C11 108.4(5) . . ?
O2 N5 O2 119.998(16) 10_646 . ?
O2 N5 O2 119.997(18) 10_646 7_665 ?
O2 N5 O2 119.998(17) . 7_665 ?
Co1 O1 Co1 111.51(14) 12_565 6_456 ?
Co1 O1 Co1 111.51(14) 12_565 . ?
Co1 O1 Co1 111.51(14) 6_456 . ?
Co1 O1 Co2 107.35(15) 12_565 . ?
Co1 O1 Co2 107.35(15) 6_456 . ?
Co1 O1 Co2 107.35(15) . . ?
C12 S3 Co1 101.10(19) . . ?
C7 S4 Co2 103.8(2) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        24.93
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.993
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.078

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.017 0.017 0.018 449 67 ' '
2 -0.031 0.031 0.531 103 16 ' '
3 -0.018 0.518 0.482 449 61 ' '
4 0.030 0.531 0.969 103 15 ' '
5 0.482 -0.018 0.517 449 64 ' '
6 0.517 0.482 0.983 449 59 ' '
7 0.469 0.469 0.469 103 14 ' '
8 0.531 0.969 1.031 103 16 ' '
_platon_squeeze_details          
;
The PLATON SQUEEZE procedure was used to treat 
regions of diffuse solvent and triethylamine which could not be modeled 
properly in terms of atomic sites. Their contribution to 
the diffraction pattern was removed and modified F² was
written to a new HKL file. The number of located electrons, 
312 in eight voids per unit cell, is included in the formula, formula weight, 
calculated density, and F(000). There are four formula units 
in one unit cell. On base of charge balance considerations, volume/count_electrons 
analysis, and elemental analyses, this residual electron density 
was assigned to half triethylamine molecule, two methanol molecules and one protonated water molecule. 
So SQUEEZE removed these disordered units per unit cell.
See refs. (a) O. V. Dolomanov, D. B. Cordes, N. R. Champness, A. J. Blake,
L. R. Hanton, G. B. Jameson, M. Schroder and C. Wilson. Chem. Commun.
2004, 642; (b) Y. Du, A. L. Thompson and D. O. Hare. Chem. Commun. 2008, 5987;
(c) Y. F. Bi, X. T. Wang, W. P. Liao, X. F. Wang, X. W. Wang, H. J. Zhang,
and S. Gao, J. Am. Chem. Soc. 2009, 131, 11650.
;

###END
_database_code_depnum_ccdc_archive 'CCDC 1013612'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_7

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H20 N8 Ni2 S4, 2(C H4 O)'
_chemical_formula_sum            'C30 H28 N8 Ni2 O2 S4'
_chemical_formula_weight         778.26

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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                   10.426(2)
_cell_length_b                   18.052(4)
_cell_length_c                   19.622(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 118.48(2)
_cell_angle_gamma                90.00
_cell_volume                     3246.1(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1600
_exptl_absorpt_coefficient_mu    1.460
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.747
_exptl_absorpt_correction_T_max  0.803
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  SCX-MINI
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            32039
_diffrn_reflns_av_R_equivalents  0.0839
_diffrn_reflns_av_sigmaI/netI    0.0725
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.99
_diffrn_reflns_theta_max         27.48
_reflns_number_total             7383
_reflns_number_gt                4778
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       PROCESS-AUTO
_computing_cell_refinement       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_structure_solution    DirectMethod
_computing_structure_refinement  SHELXL
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_molecular_graphics    ?

_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)+(0.0243P)²+4.0825P] 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         7383
_refine_ls_number_parameters     411
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1113
_refine_ls_R_factor_gt           0.0602
_refine_ls_wR_factor_ref         0.1029
_refine_ls_wR_factor_gt          0.0902
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.015
_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 0.26760(5) 0.42995(3) 0.26219(3) 0.02493(13) Uani 1 1 d . . .
Ni2 Ni 0.39935(5) 0.43133(3) 0.41452(3) 0.03146(14) Uani 1 1 d . . .
S3 S 0.40798(13) 0.55493(6) 0.41140(6) 0.0395(3) Uani 1 1 d . . .
S1 S 0.38545(12) 0.30774(6) 0.41408(6) 0.0401(3) Uani 1 1 d . . .
S2 S 0.61519(11) 0.42345(7) 0.41569(6) 0.0389(3) Uani 1 1 d . . .
S4 S 0.18205(12) 0.43894(7) 0.41084(6) 0.0422(3) Uani 1 1 d . . .
C2 C -0.0206(4) 0.3206(2) 0.1268(2) 0.0387(11) Uani 1 1 d . . .
H2 H -0.0106 0.3665 0.1085 0.046 Uiso 1 1 calc R . .
N3 N 0.4335(3) 0.38491(17) 0.26433(17) 0.0268(7) Uani 1 1 d . . .
N7 N 0.1014(3) 0.47534(17) 0.26029(17) 0.0300(8) Uani 1 1 d . . .
C17 C 0.3501(4) 0.5857(2) 0.0826(2) 0.0385(11) Uani 1 1 d . . .
H17 H 0.3230 0.5723 0.0317 0.046 Uiso 1 1 calc R . .
C9 C 0.3441(4) 0.3337(2) 0.1292(2) 0.0350(10) Uani 1 1 d . . .
H9 H 0.2450 0.3399 0.1126 0.042 Uiso 1 1 calc R . .
C19 C 0.4535(5) 0.6770(2) 0.1838(3) 0.0411(11) Uani 1 1 d . . .
H19 H 0.4961 0.7231 0.2019 0.049 Uiso 1 1 calc R . .
C28 C 0.0703(5) 0.4705(2) 0.3186(2) 0.0330(10) Uani 1 1 d . . .
N6 N 0.4484(4) 0.63380(18) 0.30534(19) 0.0389(9) Uani 1 1 d . . .
H6 H 0.4861 0.6709 0.3360 0.047 Uiso 1 1 calc R . .
C12 C 0.6454(5) 0.3139(2) 0.1792(3) 0.0431(11) Uani 1 1 d . . .
H12 H 0.7444 0.3074 0.1957 0.052 Uiso 1 1 calc R . .
C18 C 0.4149(4) 0.6538(2) 0.1096(2) 0.0399(11) Uani 1 1 d . . .
H18 H 0.4328 0.6846 0.0771 0.048 Uiso 1 1 calc R . .
C7 C 0.2403(4) 0.2906(2) 0.3239(2) 0.0317(9) Uani 1 1 d . . .
N5 N 0.3474(3) 0.52438(17) 0.26230(17) 0.0288(8) Uani 1 1 d . . .
C15 C 0.3619(4) 0.5597(2) 0.2035(2) 0.0301(9) Uani 1 1 d . . .
N1 N 0.1894(3) 0.33510(17) 0.26269(17) 0.0297(8) Uani 1 1 d . . .
N2 N 0.1630(4) 0.22686(18) 0.30588(19) 0.0398(9) Uani 1 1 d . . .
H3A H 0.1786 0.1903 0.3369 0.048 Uiso 1 1 calc R . .
C8 C 0.4482(4) 0.3539(2) 0.2033(2) 0.0278(9) Uani 1 1 d . . .
C14 C 0.5684(4) 0.3896(2) 0.3252(2) 0.0302(9) Uani 1 1 d . . .
N4 N 0.6681(4) 0.36491(18) 0.30459(19) 0.0371(9) Uani 1 1 d . . .
H1 H 0.7609 0.3632 0.3345 0.044 Uiso 1 1 calc R . .
C21 C 0.4008(4) 0.5703(2) 0.3232(2) 0.0336(9) Uani 1 1 d . . .
C20 C 0.4264(5) 0.6293(2) 0.2300(2) 0.0350(10) Uani 1 1 d . . .
C13 C 0.5966(4) 0.3430(2) 0.2281(2) 0.0333(10) Uani 1 1 d . . .
C1 C 0.0710(4) 0.2987(2) 0.2023(2) 0.0289(9) Uani 1 1 d . . .
C11 C 0.5411(5) 0.2950(2) 0.1052(2) 0.0445(11) Uani 1 1 d . . .
H11 H 0.5706 0.2759 0.0709 0.053 Uiso 1 1 calc R . .
C6 C 0.0540(5) 0.2300(2) 0.2288(2) 0.0343(10) Uani 1 1 d . . .
C5 C -0.0558(5) 0.1814(2) 0.1824(3) 0.0451(12) Uani 1 1 d . . .
H5 H -0.0689 0.1363 0.2012 0.054 Uiso 1 1 calc R . .
N8 N -0.0689(4) 0.49401(19) 0.2950(2) 0.0403(9) Uani 1 1 d . . .
H8 H -0.1120 0.4951 0.3230 0.048 Uiso 1 1 calc R . .
C27 C -0.1286(4) 0.5158(2) 0.2187(2) 0.0357(10) Uani 1 1 d . . .
C3 C -0.1280(5) 0.2710(3) 0.0796(3) 0.0445(12) Uani 1 1 d . . .
H3 H -0.1902 0.2838 0.0283 0.053 Uiso 1 1 calc R . .
C16 C 0.3245(4) 0.5369(2) 0.1291(2) 0.0347(10) Uani 1 1 d . . .
H16 H 0.2836 0.4906 0.1109 0.042 Uiso 1 1 calc R . .
C10 C 0.3938(5) 0.3038(2) 0.0808(2) 0.0432(11) Uani 1 1 d . . .
H10 H 0.3264 0.2893 0.0309 0.052 Uiso 1 1 calc R . .
C4 C -0.1448(5) 0.2031(3) 0.1069(3) 0.0473(12) Uani 1 1 d . . .
H4 H -0.2180 0.1713 0.0735 0.057 Uiso 1 1 calc R . .
C22 C -0.0205(4) 0.5048(2) 0.1971(2) 0.0324(10) Uani 1 1 d . . .
C23 C -0.0424(5) 0.5248(2) 0.1241(2) 0.0391(11) Uani 1 1 d . . .
H23 H 0.0299 0.5186 0.1097 0.047 Uiso 1 1 calc R . .
C26 C -0.2649(5) 0.5440(3) 0.1673(3) 0.0479(12) Uani 1 1 d . . .
H26 H -0.3378 0.5498 0.1814 0.057 Uiso 1 1 calc R . .
C24 C -0.1775(5) 0.5546(2) 0.0736(3) 0.0456(12) Uani 1 1 d . . .
H24 H -0.1954 0.5692 0.0244 0.055 Uiso 1 1 calc R . .
C25 C -0.2872(3) 0.56313(14) 0.09421(16) 0.0513(12) Uani 1 1 d . . .
H25 H -0.3772 0.5821 0.0581 0.062 Uiso 1 1 calc R . .
O1 O 0.9469(3) 0.30917(14) 0.37998(16) 0.0951(15) Uani 1 1 d R . .
H1A H 1.0215 0.3297 0.3877 0.114 Uiso 1 1 d R . .
O2 O 0.7905(3) 0.54608(14) 0.37405(16) 0.1091(17) Uani 1 1 d R . .
H2A H 0.8121 0.5173 0.4164 0.131 Uiso 1 1 d R . .
C30 C 0.8424(9) 0.6120(4) 0.4130(4) 0.134(3) Uani 1 1 d . . .
H30A H 0.7815 0.6277 0.4347 0.201 Uiso 1 1 calc R . .
H30B H 0.8412 0.6490 0.3776 0.201 Uiso 1 1 calc R . .
H30C H 0.9405 0.6052 0.4538 0.201 Uiso 1 1 calc R . .
C29 C 0.9656(7) 0.2404(4) 0.4110(4) 0.105(2) Uani 1 1 d . . .
H29A H 1.0620 0.2363 0.4542 0.157 Uiso 1 1 calc R . .
H29B H 0.9534 0.2042 0.3725 0.157 Uiso 1 1 calc R . .
H29C H 0.8948 0.2320 0.4282 0.157 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 1.894(3) . ?
Ni1 N5 1.897(3) . ?
Ni1 N1 1.898(3) . ?
Ni1 N7 1.901(3) . ?
Ni1 Ni2 2.6279(11) . ?
Ni2 S3 2.2350(13) . ?
Ni2 S1 2.2355(13) . ?
Ni2 S4 2.2363(13) . ?
Ni2 S2 2.2440(12) . ?
S3 C21 1.719(4) . ?
S1 C7 1.721(4) . ?
S2 C14 1.715(4) . ?
S4 C28 1.717(4) . ?
C2 C1 1.383(5) . ?
C2 C3 1.386(6) . ?
C2 H2 0.9300 . ?
N3 C14 1.345(5) . ?
N3 C8 1.394(4) . ?
N7 C28 1.332(5) . ?
N7 C22 1.390(5) . ?
C17 C18 1.381(6) . ?
C17 C16 1.382(5) . ?
C17 H17 0.9300 . ?
C9 C8 1.386(5) . ?
C9 C10 1.390(5) . ?
C9 H9 0.9300 . ?
C19 C20 1.374(5) . ?
C19 C18 1.378(6) . ?
C19 H19 0.9300 . ?
C28 N8 1.364(5) . ?
N6 C21 1.359(5) . ?
N6 C20 1.387(5) . ?
N6 H6 0.8600 . ?
C12 C11 1.379(6) . ?
C12 C13 1.385(5) . ?
C12 H12 0.9300 . ?
C18 H18 0.9300 . ?
C7 N1 1.327(5) . ?
C7 N2 1.352(5) . ?
N5 C21 1.339(5) . ?
N5 C15 1.387(5) . ?
C15 C16 1.383(5) . ?
C15 C20 1.403(5) . ?
N1 C1 1.401(5) . ?
N2 C6 1.394(5) . ?
N2 H3A 0.8600 . ?
C8 C13 1.397(5) . ?
C14 N4 1.357(5) . ?
N4 C13 1.378(5) . ?
N4 H1 0.8600 . ?
C1 C6 1.389(5) . ?
C11 C10 1.383(6) . ?
C11 H11 0.9300 . ?
C6 C5 1.384(6) . ?
C5 C4 1.377(6) . ?
C5 H5 0.9300 . ?
N8 C27 1.376(5) . ?
N8 H8 0.8600 . ?
C27 C26 1.389(6) . ?
C27 C22 1.395(5) . ?
C3 C4 1.382(6) . ?
C3 H3 0.9300 . ?
C16 H16 0.9300 . ?
C10 H10 0.9300 . ?
C4 H4 0.9300 . ?
C22 C23 1.385(5) . ?
C23 C24 1.387(6) . ?
C23 H23 0.9300 . ?
C26 C25 1.383(5) . ?
C26 H26 0.9300 . ?
C24 C25 1.391(5) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
O1 C29 1.355(6) . ?
O1 H1A 0.8068 . ?
O2 C30 1.378(7) . ?
O2 H2A 0.9124 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?

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 N5 89.43(13) . . ?
N3 Ni1 N1 90.15(13) . . ?
N5 Ni1 N1 179.48(15) . . ?
N3 Ni1 N7 179.83(16) . . ?
N5 Ni1 N7 90.45(14) . . ?
N1 Ni1 N7 89.97(14) . . ?
N3 Ni1 Ni2 90.14(9) . . ?
N5 Ni1 Ni2 89.95(9) . . ?
N1 Ni1 Ni2 89.75(9) . . ?
N7 Ni1 Ni2 89.74(9) . . ?
S3 Ni2 S1 178.33(4) . . ?
S3 Ni2 S4 89.50(5) . . ?
S1 Ni2 S4 89.91(5) . . ?
S3 Ni2 S2 90.59(5) . . ?
S1 Ni2 S2 89.98(5) . . ?
S4 Ni2 S2 178.88(4) . . ?
S3 Ni2 Ni1 89.11(3) . . ?
S1 Ni2 Ni1 89.33(3) . . ?
S4 Ni2 Ni1 89.53(4) . . ?
S2 Ni2 Ni1 89.36(4) . . ?
C21 S3 Ni2 101.90(15) . . ?
C7 S1 Ni2 101.92(14) . . ?
C14 S2 Ni2 102.91(14) . . ?
C28 S4 Ni2 102.83(15) . . ?
C1 C2 C3 117.2(4) . . ?
C1 C2 H2 121.4 . . ?
C3 C2 H2 121.4 . . ?
C14 N3 C8 106.9(3) . . ?
C14 N3 Ni1 123.4(3) . . ?
C8 N3 Ni1 128.8(2) . . ?
C28 N7 C22 107.4(3) . . ?
C28 N7 Ni1 123.2(3) . . ?
C22 N7 Ni1 128.3(3) . . ?
C18 C17 C16 121.7(4) . . ?
C18 C17 H17 119.1 . . ?
C16 C17 H17 119.1 . . ?
C8 C9 C10 117.4(4) . . ?
C8 C9 H9 121.3 . . ?
C10 C9 H9 121.3 . . ?
C20 C19 C18 117.2(4) . . ?
C20 C19 H19 121.4 . . ?
C18 C19 H19 121.4 . . ?
N7 C28 N8 110.0(3) . . ?
N7 C28 S4 127.4(3) . . ?
N8 C28 S4 122.6(3) . . ?
C21 N6 C20 109.3(3) . . ?
C21 N6 H6 125.4 . . ?
C20 N6 H6 125.4 . . ?
C11 C12 C13 117.2(4) . . ?
C11 C12 H12 121.4 . . ?
C13 C12 H12 121.4 . . ?
C19 C18 C17 121.4(4) . . ?
C19 C18 H18 119.3 . . ?
C17 C18 H18 119.3 . . ?
N1 C7 N2 110.3(3) . . ?
N1 C7 S1 126.7(3) . . ?
N2 C7 S1 123.0(3) . . ?
C21 N5 C15 107.1(3) . . ?
C21 N5 Ni1 123.6(3) . . ?
C15 N5 Ni1 129.3(3) . . ?
C16 C15 N5 130.9(4) . . ?
C16 C15 C20 120.0(4) . . ?
N5 C15 C20 109.1(3) . . ?
C7 N1 C1 107.0(3) . . ?
C7 N1 Ni1 124.3(3) . . ?
C1 N1 Ni1 128.8(2) . . ?
C7 N2 C6 109.0(3) . . ?
C7 N2 H3A 125.5 . . ?
C6 N2 H3A 125.5 . . ?
C9 C8 N3 131.0(4) . . ?
C9 C8 C13 120.7(4) . . ?
N3 C8 C13 108.3(3) . . ?
N3 C14 N4 109.9(3) . . ?
N3 C14 S2 127.0(3) . . ?
N4 C14 S2 123.0(3) . . ?
C14 N4 C13 109.0(3) . . ?
C14 N4 H1 125.5 . . ?
C13 N4 H1 125.5 . . ?
N5 C21 N6 109.8(3) . . ?
N5 C21 S3 126.8(3) . . ?
N6 C21 S3 123.4(3) . . ?
C19 C20 N6 133.2(4) . . ?
C19 C20 C15 122.1(4) . . ?
N6 C20 C15 104.7(3) . . ?
N4 C13 C12 132.6(4) . . ?
N4 C13 C8 105.8(3) . . ?
C12 C13 C8 121.6(4) . . ?
C2 C1 C6 120.6(4) . . ?
C2 C1 N1 130.6(4) . . ?
C6 C1 N1 108.7(3) . . ?
C12 C11 C10 121.6(4) . . ?
C12 C11 H11 119.2 . . ?
C10 C11 H11 119.2 . . ?
C5 C6 C1 122.2(4) . . ?
C5 C6 N2 132.8(4) . . ?
C1 C6 N2 105.0(3) . . ?
C4 C5 C6 116.7(4) . . ?
C4 C5 H5 121.7 . . ?
C6 C5 H5 121.7 . . ?
C28 N8 C27 108.4(3) . . ?
C28 N8 H8 125.8 . . ?
C27 N8 H8 125.8 . . ?
N8 C27 C26 132.1(4) . . ?
N8 C27 C22 106.1(4) . . ?
C26 C27 C22 121.8(4) . . ?
C4 C3 C2 121.7(4) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
C17 C16 C15 117.6(4) . . ?
C17 C16 H16 121.2 . . ?
C15 C16 H16 121.2 . . ?
C11 C10 C9 121.5(4) . . ?
C11 C10 H10 119.3 . . ?
C9 C10 H10 119.3 . . ?
C5 C4 C3 121.6(4) . . ?
C5 C4 H4 119.2 . . ?
C3 C4 H4 119.2 . . ?
C23 C22 N7 130.7(4) . . ?
C23 C22 C27 121.2(4) . . ?
N7 C22 C27 108.1(4) . . ?
C22 C23 C24 116.8(4) . . ?
C22 C23 H23 121.6 . . ?
C24 C23 H23 121.6 . . ?
C25 C26 C27 116.9(4) . . ?
C25 C26 H26 121.6 . . ?
C27 C26 H26 121.6 . . ?
C23 C24 C25 122.1(4) . . ?
C23 C24 H24 119.0 . . ?
C25 C24 H24 119.0 . . ?
C26 C25 C24 121.2(3) . . ?
C26 C25 H25 119.4 . . ?
C24 C25 H25 119.4 . . ?
C29 O1 H1A 114.6 . . ?
C30 O2 H2A 97.1 . . ?
O2 C30 H30A 109.5 . . ?
O2 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
O2 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O1 C29 H29A 109.5 . . ?
O1 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
O1 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?

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
N3 Ni1 Ni2 S3 112.39(10) . . . . ?
N5 Ni1 Ni2 S3 22.96(10) . . . . ?
N1 Ni1 Ni2 S3 -157.47(10) . . . . ?
N7 Ni1 Ni2 S3 -67.50(10) . . . . ?
N3 Ni1 Ni2 S1 -68.20(10) . . . . ?
N5 Ni1 Ni2 S1 -157.63(10) . . . . ?
N1 Ni1 Ni2 S1 21.95(10) . . . . ?
N7 Ni1 Ni2 S1 111.92(10) . . . . ?
N3 Ni1 Ni2 S4 -158.11(10) . . . . ?
N5 Ni1 Ni2 S4 112.46(10) . . . . ?
N1 Ni1 Ni2 S4 -67.96(10) . . . . ?
N7 Ni1 Ni2 S4 22.01(10) . . . . ?
N3 Ni1 Ni2 S2 21.79(10) . . . . ?
N5 Ni1 Ni2 S2 -67.64(10) . . . . ?
N1 Ni1 Ni2 S2 111.94(10) . . . . ?
N7 Ni1 Ni2 S2 -158.10(10) . . . . ?
S1 Ni2 S3 C21 -45.2(17) . . . . ?
S4 Ni2 S3 C21 -114.28(14) . . . . ?
S2 Ni2 S3 C21 64.60(14) . . . . ?
Ni1 Ni2 S3 C21 -24.74(14) . . . . ?
S3 Ni2 S1 C7 -3.3(17) . . . . ?
S4 Ni2 S1 C7 65.70(14) . . . . ?
S2 Ni2 S1 C7 -113.19(14) . . . . ?
Ni1 Ni2 S1 C7 -23.83(14) . . . . ?
S3 Ni2 S2 C14 -109.20(14) . . . . ?
S1 Ni2 S2 C14 69.23(14) . . . . ?
S4 Ni2 S2 C14 -15(3) . . . . ?
Ni1 Ni2 S2 C14 -20.10(14) . . . . ?
S3 Ni2 S4 C28 69.48(14) . . . . ?
S1 Ni2 S4 C28 -108.96(15) . . . . ?
S2 Ni2 S4 C28 -25(3) . . . . ?
Ni1 Ni2 S4 C28 -19.63(14) . . . . ?
N5 Ni1 N3 C14 67.1(3) . . . . ?
N1 Ni1 N3 C14 -112.5(3) . . . . ?
N7 Ni1 N3 C14 20(63) . . . . ?
Ni2 Ni1 N3 C14 -22.8(3) . . . . ?
N5 Ni1 N3 C8 -100.4(3) . . . . ?
N1 Ni1 N3 C8 79.9(3) . . . . ?
N7 Ni1 N3 C8 -148(100) . . . . ?
Ni2 Ni1 N3 C8 169.6(3) . . . . ?
N3 Ni1 N7 C28 -67(63) . . . . ?
N5 Ni1 N7 C28 -114.0(3) . . . . ?
N1 Ni1 N7 C28 65.7(3) . . . . ?
Ni2 Ni1 N7 C28 -24.1(3) . . . . ?
N3 Ni1 N7 C22 127(69) . . . . ?
N5 Ni1 N7 C22 80.2(3) . . . . ?
N1 Ni1 N7 C22 -100.1(3) . . . . ?
Ni2 Ni1 N7 C22 170.1(3) . . . . ?
C22 N7 C28 N8 1.5(4) . . . . ?
Ni1 N7 C28 N8 -166.9(3) . . . . ?
C22 N7 C28 S4 -179.1(3) . . . . ?
Ni1 N7 C28 S4 12.5(5) . . . . ?
Ni2 S4 C28 N7 11.1(4) . . . . ?
Ni2 S4 C28 N8 -169.6(3) . . . . ?
C20 C19 C18 C17 0.7(6) . . . . ?
C16 C17 C18 C19 -1.7(7) . . . . ?
Ni2 S1 C7 N1 22.1(4) . . . . ?
Ni2 S1 C7 N2 -159.3(3) . . . . ?
N3 Ni1 N5 C21 -108.6(3) . . . . ?
N1 Ni1 N5 C21 -73(15) . . . . ?
N7 Ni1 N5 C21 71.3(3) . . . . ?
Ni2 Ni1 N5 C21 -18.4(3) . . . . ?
N3 Ni1 N5 C15 72.0(3) . . . . ?
N1 Ni1 N5 C15 108(15) . . . . ?
N7 Ni1 N5 C15 -108.1(3) . . . . ?
Ni2 Ni1 N5 C15 162.2(3) . . . . ?
C21 N5 C15 C16 179.9(4) . . . . ?
Ni1 N5 C15 C16 -0.6(6) . . . . ?
C21 N5 C15 C20 0.0(4) . . . . ?
Ni1 N5 C15 C20 179.5(3) . . . . ?
N2 C7 N1 C1 1.3(4) . . . . ?
S1 C7 N1 C1 -180.0(3) . . . . ?
N2 C7 N1 Ni1 -179.3(3) . . . . ?
S1 C7 N1 Ni1 -0.6(5) . . . . ?
N3 Ni1 N1 C7 72.6(3) . . . . ?
N5 Ni1 N1 C7 37(15) . . . . ?
N7 Ni1 N1 C7 -107.3(3) . . . . ?
Ni2 Ni1 N1 C7 -17.5(3) . . . . ?
N3 Ni1 N1 C1 -108.2(3) . . . . ?
N5 Ni1 N1 C1 -144(15) . . . . ?
N7 Ni1 N1 C1 71.9(3) . . . . ?
Ni2 Ni1 N1 C1 161.6(3) . . . . ?
N1 C7 N2 C6 -0.8(5) . . . . ?
S1 C7 N2 C6 -179.6(3) . . . . ?
C10 C9 C8 N3 179.8(4) . . . . ?
C10 C9 C8 C13 -1.2(6) . . . . ?
C14 N3 C8 C9 176.4(4) . . . . ?
Ni1 N3 C8 C9 -14.4(6) . . . . ?
C14 N3 C8 C13 -2.6(4) . . . . ?
Ni1 N3 C8 C13 166.6(3) . . . . ?
C8 N3 C14 N4 1.8(4) . . . . ?
Ni1 N3 C14 N4 -168.1(2) . . . . ?
C8 N3 C14 S2 -179.9(3) . . . . ?
Ni1 N3 C14 S2 10.2(5) . . . . ?
Ni2 S2 C14 N3 12.8(4) . . . . ?
Ni2 S2 C14 N4 -169.1(3) . . . . ?
N3 C14 N4 C13 -0.4(5) . . . . ?
S2 C14 N4 C13 -178.7(3) . . . . ?
C15 N5 C21 N6 0.2(4) . . . . ?
Ni1 N5 C21 N6 -179.3(3) . . . . ?
C15 N5 C21 S3 179.2(3) . . . . ?
Ni1 N5 C21 S3 -0.3(5) . . . . ?
C20 N6 C21 N5 -0.4(5) . . . . ?
C20 N6 C21 S3 -179.4(3) . . . . ?
Ni2 S3 C21 N5 22.8(4) . . . . ?
Ni2 S3 C21 N6 -158.4(3) . . . . ?
C18 C19 C20 N6 -179.2(4) . . . . ?
C18 C19 C20 C15 -0.1(6) . . . . ?
C21 N6 C20 C19 179.6(5) . . . . ?
C21 N6 C20 C15 0.4(4) . . . . ?
C16 C15 C20 C19 0.5(6) . . . . ?
N5 C15 C20 C19 -179.6(4) . . . . ?
C16 C15 C20 N6 179.8(4) . . . . ?
N5 C15 C20 N6 -0.3(4) . . . . ?
C14 N4 C13 C12 -179.9(4) . . . . ?
C14 N4 C13 C8 -1.2(4) . . . . ?
C11 C12 C13 N4 177.5(4) . . . . ?
C11 C12 C13 C8 -1.0(6) . . . . ?
C9 C8 C13 N4 -176.8(4) . . . . ?
N3 C8 C13 N4 2.4(4) . . . . ?
C9 C8 C13 C12 2.0(6) . . . . ?
N3 C8 C13 C12 -178.8(4) . . . . ?
C3 C2 C1 C6 -0.2(6) . . . . ?
C3 C2 C1 N1 178.7(4) . . . . ?
C7 N1 C1 C2 179.6(4) . . . . ?
Ni1 N1 C1 C2 0.3(6) . . . . ?
C7 N1 C1 C6 -1.3(4) . . . . ?
Ni1 N1 C1 C6 179.4(3) . . . . ?
C13 C12 C11 C10 -0.8(7) . . . . ?
C2 C1 C6 C5 -1.7(6) . . . . ?
N1 C1 C6 C5 179.1(4) . . . . ?
C2 C1 C6 N2 180.0(4) . . . . ?
N1 C1 C6 N2 0.8(4) . . . . ?
C7 N2 C6 C5 -178.1(5) . . . . ?
C7 N2 C6 C1 0.0(4) . . . . ?
C1 C6 C5 C4 2.7(6) . . . . ?
N2 C6 C5 C4 -179.5(4) . . . . ?
N7 C28 N8 C27 -0.8(5) . . . . ?
S4 C28 N8 C27 179.8(3) . . . . ?
C28 N8 C27 C26 -179.9(5) . . . . ?
C28 N8 C27 C22 -0.2(5) . . . . ?
C1 C2 C3 C4 1.0(6) . . . . ?
C18 C17 C16 C15 2.0(6) . . . . ?
N5 C15 C16 C17 178.7(4) . . . . ?
C20 C15 C16 C17 -1.4(6) . . . . ?
C12 C11 C10 C9 1.6(7) . . . . ?
C8 C9 C10 C11 -0.5(6) . . . . ?
C6 C5 C4 C3 -1.9(7) . . . . ?
C2 C3 C4 C5 0.1(7) . . . . ?
C28 N7 C22 C23 176.0(4) . . . . ?
Ni1 N7 C22 C23 -16.4(6) . . . . ?
C28 N7 C22 C27 -1.6(4) . . . . ?
Ni1 N7 C22 C27 166.0(3) . . . . ?
N8 C27 C22 C23 -176.8(4) . . . . ?
C26 C27 C22 C23 3.0(6) . . . . ?
N8 C27 C22 N7 1.1(4) . . . . ?
C26 C27 C22 N7 -179.2(4) . . . . ?
N7 C22 C23 C24 -178.7(4) . . . . ?
C27 C22 C23 C24 -1.4(6) . . . . ?
N8 C27 C26 C25 177.6(4) . . . . ?
C22 C27 C26 C25 -2.1(6) . . . . ?
C22 C23 C24 C25 -0.9(6) . . . . ?
C27 C26 C25 C24 -0.2(6) . . . . ?
C23 C24 C25 C26 1.7(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.080
_database_code_depnum_ccdc_archive 'CCDC 1013613'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_8

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H36 N12 Ni5 O2 S6 (C H4 O)3 (H3 0)2'
_chemical_formula_sum            'C47 H54 N12 Ni5 O7 S6'
_chemical_formula_weight         1384.86

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'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   'R -3 c'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   18.546(3)
_cell_length_b                   18.546(3)
_cell_length_c                   29.647(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     8831(2)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3816
_exptl_absorpt_coefficient_mu    1.826
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.681
_exptl_absorpt_correction_T_max  0.747
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  SCX-MINI
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24321
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_av_sigmaI/netI    0.0245
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         25.01
_reflns_number_total             1734
_reflns_number_gt                1619
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       PROCESS-AUTO
_computing_cell_refinement       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_structure_solution    DirectMethod
_computing_structure_refinement  SHELXL
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_molecular_graphics    ?

_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. 'Omit' restraint instruction 
was used in the refinement. 'Isor' restraint instruction 
was used for C19 in the refinement.
;

_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)+(0.0576P)²+57.5496P] 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         1734
_refine_ls_number_parameters     106
_refine_ls_number_restraints     84
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0548
_refine_ls_wR_factor_ref         0.1360
_refine_ls_wR_factor_gt          0.1328
_refine_ls_goodness_of_fit_ref   1.220
_refine_ls_restrained_S_all      1.224
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.002

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 0.6667 0.22025(4) 0.0833 0.0302(3) Uani 1 2 d SU . .
Ni2 Ni 0.6667 0.3333 -0.01663(4) 0.0350(3) Uani 1 3 d SU . .
S3 S 0.72621(7) 0.26230(7) 0.01593(4) 0.0342(3) Uani 1 1 d U . .
N1 N 0.5634(2) 0.1533(2) 0.05325(13) 0.0311(9) Uani 1 1 d U . .
N2 N 0.8948(3) 0.3375(3) 0.01797(14) 0.0388(10) Uani 1 1 d U . .
H2 H 0.8955 0.2988 0.0023 0.047 Uiso 1 1 calc R . .
C1 C 0.5374(4) 0.0130(3) 0.08164(19) 0.0468(13) Uani 1 1 d U . .
H1 H 0.5880 0.0326 0.0964 0.056 Uiso 1 1 calc R . .
C2 C 0.8264(3) 0.3422(3) 0.02922(16) 0.0319(10) Uani 1 1 d U . .
C3 C 0.9636(3) 0.4066(3) 0.03629(17) 0.0386(12) Uani 1 1 d U . .
C4 C 0.5189(3) 0.0672(3) 0.05824(16) 0.0348(11) Uani 1 1 d U . .
C5 C 1.0482(4) 0.4315(4) 0.0365(2) 0.0561(15) Uani 1 1 d U . .
H5 H 1.0686 0.4012 0.0216 0.067 Uiso 1 1 calc R . .
C6 C 0.4788(4) -0.0698(4) 0.0822(2) 0.0609(17) Uani 1 1 d U . .
H6 H 0.4896 -0.1069 0.0978 0.073 Uiso 1 1 calc R . .
C7 C 1.0994(4) 0.5028(5) 0.0598(2) 0.0658(18) Uani 1 1 d U . .
H7 H 1.1561 0.5212 0.0607 0.079 Uiso 1 1 calc R . .
O1 O 0.6667 0.3333 -0.0716(3) 0.083(3) Uani 1 3 d SU . .
C9 C 0.6667 0.3333 -0.1104(6) 0.133(6) Uani 1 3 d SU . .
H9A H 0.6125 0.2929 -0.1212 0.199 Uiso 0.33 1 calc PR . .
H9B H 0.7071 0.3196 -0.1212 0.199 Uiso 0.33 1 calc PR . .
H9C H 0.6804 0.3875 -0.1212 0.199 Uiso 0.33 1 calc PR . .


_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 1.905(4) . ?
Ni1 N1 1.905(4) 18_654 ?
Ni1 S3 2.2269(13) 18_654 ?
Ni1 S3 2.2270(13) . ?
Ni2 O1 1.629(9) . ?
Ni2 S3 2.3113(14) . ?
Ni2 S3 2.3113(14) 2_655 ?
Ni2 S3 2.3113(14) 3_665 ?
S3 C2 1.746(5) . ?
N1 C2 1.326(6) 3_665 ?
N1 C4 1.390(6) . ?
N2 C2 1.356(6) . ?
N2 C3 1.388(7) . ?
C1 C6 1.367(8) . ?
C1 C4 1.398(7) . ?
C2 N1 1.326(6) 2_655 ?
C3 C4 1.388(7) 2_655 ?
C3 C5 1.397(7) . ?
C4 C3 1.388(7) 3_665 ?
C5 C7 1.369(9) . ?
C6 C7 1.389(9) 3_665 ?
C7 C6 1.389(9) 2_655 ?
O1 C9 1.150(18) . ?

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 N1 162.9(2) . 18_654 ?
N1 Ni1 S3 93.51(12) . 18_654 ?
N1 Ni1 S3 88.24(12) 18_654 18_654 ?
N1 Ni1 S3 88.24(12) . . ?
N1 Ni1 S3 93.51(12) 18_654 . ?
S3 Ni1 S3 168.27(7) 18_654 . ?
O1 Ni2 S3 114.69(4) . . ?
O1 Ni2 S3 114.69(4) . 2_655 ?
S3 Ni2 S3 103.79(5) . 2_655 ?
O1 Ni2 S3 114.69(4) . 3_665 ?
S3 Ni2 S3 103.79(5) . 3_665 ?
S3 Ni2 S3 103.79(5) 2_655 3_665 ?
C2 S3 Ni1 103.04(16) . . ?
C2 S3 Ni2 102.67(16) . . ?
Ni1 S3 Ni2 106.24(6) . . ?
C2 N1 C4 106.6(4) 3_665 . ?
C2 N1 Ni1 131.4(3) 3_665 . ?
C4 N1 Ni1 121.6(3) . . ?
C2 N2 C3 107.6(4) . . ?
C6 C1 C4 118.1(6) . . ?
N1 C2 N2 111.2(4) 2_655 . ?
N1 C2 S3 127.1(4) 2_655 . ?
N2 C2 S3 121.5(4) . . ?
N2 C3 C4 105.9(4) . 2_655 ?
N2 C3 C5 132.0(5) . . ?
C4 C3 C5 122.1(5) 2_655 . ?
C3 C4 N1 108.7(4) 3_665 . ?
C3 C4 C1 119.9(5) 3_665 . ?
N1 C4 C1 131.4(5) . . ?
C7 C5 C3 116.3(6) . . ?
C1 C6 C7 121.0(6) . 3_665 ?
C5 C7 C6 122.5(5) . 2_655 ?
C9 O1 Ni2 180.0 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.085

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.013 0.215 -0.003 2617 448 ' '
_platon_squeeze_details          
;
The PLATON SQUEEZE procedure was used to treat 
regions of diffuse solvent which could not be modeled 
properly in terms of atomic sites. Their contribution to 
the diffraction pattern was removed and modified F² was
written to a new HKL file. The number of located electrons, 
448 in one void per unit cell, is included in the formula, formula weight, 
calculated density, and F(000). There are six formula units 
in one unit cell. On base of charge balance considerations, volume/count_electrons 
analysis, elemental analyses, this residual electron density 
was assigned to three methanol molecules and two protonated water molecules. 
So SQUEEZE removed these disordered units per unit cell. 
The tentative formula for compound 1 is presented as in the text.
See refs. (a) O. V. Dolomanov, D. B. Cordes, N. R. Champness, A. J. Blake,
L. R. Hanton, G. B. Jameson, M. Schroder and C. Wilson. Chem. Commun.
2004, 642; (b) Y. Du, A. L. Thompson and D. O. Hare. Chem. Commun. 2008, 5987;
(c) Y. F. Bi, X. T. Wang, W. P. Liao, X. F. Wang, X. W. Wang, H. J. Zhang,
and S. Gao, J. Am. Chem. Soc. 2009, 131, 11650.
;

_database_code_depnum_ccdc_archive 'CCDC 1013614'
