# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 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
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# 
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#  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            'C44 H46 N4 Ni3 S30'
_chemical_formula_weight         1768.78

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           ?
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   11.6986(12)
_cell_length_b                   12.1197(12)
_cell_length_c                   14.0622(14)
_cell_angle_alpha                109.910(3)
_cell_angle_beta                 105.249(3)
_cell_angle_gamma                103.361(3)
_cell_volume                     1691.9(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.736
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             902
_exptl_absorpt_coefficient_mu    1.790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7160
_exptl_absorpt_correction_T_max  0.9158
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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            34520
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_sigmaI/netI    0.0433
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.92
_diffrn_reflns_theta_max         27.55
_reflns_number_total             7788
_reflns_number_gt                5220
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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)+(0.0295P)²+1.0249P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00148(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         7788
_refine_ls_number_parameters     369
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0423
_refine_ls_wR_factor_ref         0.0894
_refine_ls_wR_factor_gt          0.0760
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_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
Ni1 Ni 0.35830(3) 0.03764(3) 0.67495(3) 0.03346(10) Uani 1 1 d . . .
S1 S 0.29448(7) 0.19530(7) 0.72001(6) 0.04118(18) Uani 1 1 d . . .
S2 S 0.39366(7) 0.06585(6) 0.54034(6) 0.03872(18) Uani 1 1 d . . .
S3 S 0.34057(8) 0.02319(7) 0.81926(6) 0.0460(2) Uani 1 1 d . . .
S4 S 0.41068(8) -0.12791(7) 0.62542(6) 0.04071(18) Uani 1 1 d . . .
S5 S 0.38557(8) -0.16070(7) 0.91279(6) 0.0480(2) Uani 1 1 d . . .
S6 S 0.44706(8) -0.30103(7) 0.73522(6) 0.04338(19) Uani 1 1 d . . .
S7 S 0.45523(9) -0.38104(8) 0.91375(7) 0.0578(2) Uani 1 1 d . . .
S8 S 0.27380(7) 0.38160(6) 0.62363(6) 0.03864(18) Uani 1 1 d . . .
S9 S 0.36955(8) 0.26513(7) 0.46106(6) 0.04246(19) Uani 1 1 d . . .
S10 S 0.29917(9) 0.48596(8) 0.46488(7) 0.0560(2) Uani 1 1 d . . .
C1 C 0.3128(3) 0.3827(2) 0.5140(2) 0.0376(6) Uani 1 1 d . . .
C2 C 0.3110(2) 0.2511(2) 0.6266(2) 0.0325(6) Uani 1 1 d . . .
C3 C 0.3542(2) 0.1955(2) 0.5488(2) 0.0335(6) Uani 1 1 d . . .
C4 C 0.3797(3) -0.1072(3) 0.8122(2) 0.0369(6) Uani 1 1 d . . .
C5 C 0.4098(3) -0.1717(2) 0.7293(2) 0.0342(6) Uani 1 1 d . . .
C6 C 0.4307(3) -0.2852(3) 0.8572(2) 0.0395(7) Uani 1 1 d . . .
Ni2 Ni 0.0000 1.0000 0.5000 0.03743(14) Uani 1 2 d S . .
S11 S -0.03404(8) 0.97838(7) 0.63645(7) 0.0469(2) Uani 1 1 d . . .
S12 S 0.05807(7) 0.83957(7) 0.45833(6) 0.04487(19) Uani 1 1 d . . .
S13 S 0.08137(8) 0.66063(7) 0.56120(7) 0.0497(2) Uani 1 1 d . . .
S14 S -0.00211(9) 0.79132(8) 0.72888(7) 0.0550(2) Uani 1 1 d . . .
S15 S 0.06435(11) 0.57012(10) 0.72978(9) 0.0783(3) Uani 1 1 d . . .
C7 C 0.0052(3) 0.8516(3) 0.6344(2) 0.0394(7) Uani 1 1 d . . .
C8 C 0.0454(2) 0.7902(2) 0.5553(2) 0.0371(7) Uani 1 1 d . . .
C9 C 0.0489(3) 0.6683(3) 0.6761(3) 0.0492(8) Uani 1 1 d . . .
N1 N 0.2797(2) 0.8002(2) 0.22088(18) 0.0399(6) Uani 1 1 d . . .
N2 N 0.3849(2) 0.5089(2) 0.2506(2) 0.0539(7) Uani 1 1 d . . .
H2A H 0.4212 0.4736 0.2097 0.065 Uiso 1 1 calc R . .
H2B H 0.3715 0.4839 0.2984 0.065 Uiso 1 1 calc R . .
C10 C 0.3494(3) 0.6024(3) 0.2401(2) 0.0402(7) Uani 1 1 d . . .
C11 C 0.3694(3) 0.6459(3) 0.1638(2) 0.0467(7) Uani 1 1 d . . .
H11 H 0.4065 0.6078 0.1173 0.056 Uiso 1 1 calc R . .
C12 C 0.2907(3) 0.6637(3) 0.3062(3) 0.0514(8) Uani 1 1 d . . .
H12 H 0.2738 0.6375 0.3576 0.062 Uiso 1 1 calc R . .
C13 C 0.3352(3) 0.7431(3) 0.1567(2) 0.0467(8) Uani 1 1 d . . .
H13 H 0.3507 0.7711 0.1059 0.056 Uiso 1 1 calc R . .
C14 C 0.2592(3) 0.7596(3) 0.2954(2) 0.0501(8) Uani 1 1 d . . .
H14 H 0.2219 0.7996 0.3407 0.060 Uiso 1 1 calc R . .
C15 C 0.2498(3) 0.9418(3) 0.1267(2) 0.0450(7) Uani 1 1 d . . .
H15A H 0.1979 0.8689 0.0583 0.054 Uiso 1 1 calc R . .
H15B H 0.3362 0.9660 0.1297 0.054 Uiso 1 1 calc R . .
C16 C 0.2453(3) 0.9103(3) 0.2207(3) 0.0515(8) Uani 1 1 d . . .
H16A H 0.3019 0.9828 0.2880 0.062 Uiso 1 1 calc R . .
H16B H 0.1602 0.8956 0.2208 0.062 Uiso 1 1 calc R . .
C17 C 0.2010(3) 1.0904(3) 0.0433(3) 0.0529(8) Uani 1 1 d . . .
H17A H 0.1513 1.0187 -0.0265 0.063 Uiso 1 1 calc R . .
H17B H 0.2871 1.1192 0.0466 0.063 Uiso 1 1 calc R . .
C18 C 0.2010(3) 1.0494(3) 0.1333(3) 0.0499(8) Uani 1 1 d . . .
H18A H 0.1153 1.0240 0.1316 0.060 Uiso 1 1 calc R . .
H18B H 0.2529 1.1207 0.2028 0.060 Uiso 1 1 calc R . .
C19 C 0.1475(3) 1.1942(3) 0.0501(3) 0.0549(9) Uani 1 1 d . . .
H19A H 0.0607 1.1640 0.0448 0.066 Uiso 1 1 calc R . .
H19B H 0.1954 1.2643 0.1211 0.066 Uiso 1 1 calc R . .
C20 C 0.1493(3) 1.2409(3) -0.0362(3) 0.0630(10) Uani 1 1 d . . .
H20A H 0.1040 1.1706 -0.1075 0.076 Uiso 1 1 calc R . .
H20B H 0.2363 1.2747 -0.0292 0.076 Uiso 1 1 calc R . .
C21 C 0.0902(4) 1.3415(3) -0.0297(3) 0.0731(11) Uani 1 1 d . . .
H21A H 0.0024 1.3070 -0.0388 0.088 Uiso 1 1 calc R . .
H21B H 0.1339 1.4108 0.0423 0.088 Uiso 1 1 calc R . .
C22 C 0.0952(5) 1.3911(4) -0.1143(4) 0.1068(17) Uani 1 1 d . . .
H22A H 0.1816 1.4237 -0.1070 0.160 Uiso 1 1 calc R . .
H22B H 0.0603 1.4567 -0.1037 0.160 Uiso 1 1 calc R . .
H22C H 0.0469 1.3243 -0.1858 0.160 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 S3 2.1537(8) . ?
Ni1 S2 2.1585(8) . ?
Ni1 S1 2.1665(8) . ?
Ni1 S4 2.1742(8) . ?
S1 C2 1.703(3) . ?
S2 C3 1.712(3) . ?
S3 C4 1.723(3) . ?
S4 C5 1.717(3) . ?
S5 C6 1.717(3) . ?
S5 C4 1.737(3) . ?
S6 C6 1.727(3) . ?
S6 C5 1.744(3) . ?
S7 C6 1.651(3) . ?
S8 C1 1.722(3) . ?
S8 C2 1.746(3) . ?
S9 C1 1.732(3) . ?
S9 C3 1.738(3) . ?
S10 C1 1.641(3) . ?
C2 C3 1.361(4) . ?
C4 C5 1.349(4) . ?
Ni2 S11 2.1459(8) . ?
Ni2 S11 2.1459(8) 2_576 ?
Ni2 S12 2.1515(8) 2_576 ?
Ni2 S12 2.1516(8) . ?
S11 C7 1.695(3) . ?
S12 C8 1.692(3) . ?
S13 C9 1.732(3) . ?
S13 C8 1.739(3) . ?
S14 C7 1.732(3) . ?
S14 C9 1.738(3) . ?
S15 C9 1.631(3) . ?
C7 C8 1.372(4) . ?
N1 C13 1.344(3) . ?
N1 C14 1.351(4) . ?
N1 C16 1.481(4) . ?
N2 C10 1.333(4) . ?
N2 H2A 0.8600 . ?
N2 H2B 0.8600 . ?
C10 C11 1.394(4) . ?
C10 C12 1.410(4) . ?
C11 C13 1.353(4) . ?
C11 H11 0.9300 . ?
C12 C14 1.341(4) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 C16 1.505(4) . ?
C15 C18 1.525(4) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.510(4) . ?
C17 C19 1.515(4) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.507(4) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.524(5) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.512(5) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 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
S3 Ni1 S2 174.51(4) . . ?
S3 Ni1 S1 86.09(3) . . ?
S2 Ni1 S1 93.20(3) . . ?
S3 Ni1 S4 93.44(3) . . ?
S2 Ni1 S4 87.58(3) . . ?
S1 Ni1 S4 176.60(3) . . ?
C2 S1 Ni1 101.96(9) . . ?
C3 S2 Ni1 101.94(9) . . ?
C4 S3 Ni1 101.84(9) . . ?
C5 S4 Ni1 101.53(10) . . ?
C6 S5 C4 97.41(13) . . ?
C6 S6 C5 97.40(13) . . ?
C1 S8 C2 97.24(13) . . ?
C1 S9 C3 97.04(13) . . ?
S10 C1 S8 123.42(17) . . ?
S10 C1 S9 122.97(17) . . ?
S8 C1 S9 113.60(15) . . ?
C3 C2 S1 121.5(2) . . ?
C3 C2 S8 115.8(2) . . ?
S1 C2 S8 122.68(16) . . ?
C2 C3 S2 121.4(2) . . ?
C2 C3 S9 116.3(2) . . ?
S2 C3 S9 122.35(16) . . ?
C5 C4 S3 121.6(2) . . ?
C5 C4 S5 116.5(2) . . ?
S3 C4 S5 121.89(16) . . ?
C4 C5 S4 121.6(2) . . ?
C4 C5 S6 115.5(2) . . ?
S4 C5 S6 122.91(16) . . ?
S7 C6 S5 123.72(17) . . ?
S7 C6 S6 123.12(17) . . ?
S5 C6 S6 113.17(15) . . ?
S11 Ni2 S11 180.0 . 2_576 ?
S11 Ni2 S12 87.40(3) . 2_576 ?
S11 Ni2 S12 92.60(3) 2_576 2_576 ?
S11 Ni2 S12 92.60(3) . . ?
S11 Ni2 S12 87.40(3) 2_576 . ?
S12 Ni2 S12 180.00(5) 2_576 . ?
C7 S11 Ni2 102.96(10) . . ?
C8 S12 Ni2 102.82(10) . . ?
C9 S13 C8 97.06(14) . . ?
C7 S14 C9 97.39(15) . . ?
C8 C7 S11 120.7(2) . . ?
C8 C7 S14 115.9(2) . . ?
S11 C7 S14 123.42(18) . . ?
C7 C8 S12 120.9(2) . . ?
C7 C8 S13 116.3(2) . . ?
S12 C8 S13 122.77(17) . . ?
S15 C9 S13 123.5(2) . . ?
S15 C9 S14 123.1(2) . . ?
S13 C9 S14 113.36(17) . . ?
C13 N1 C14 118.4(3) . . ?
C13 N1 C16 124.8(2) . . ?
C14 N1 C16 116.7(2) . . ?
C10 N2 H2A 120.0 . . ?
C10 N2 H2B 120.0 . . ?
H2A N2 H2B 120.0 . . ?
N2 C10 C11 121.9(3) . . ?
N2 C10 C12 121.9(3) . . ?
C11 C10 C12 116.2(3) . . ?
C13 C11 C10 120.6(3) . . ?
C13 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C14 C12 C10 120.3(3) . . ?
C14 C12 H12 119.8 . . ?
C10 C12 H12 119.8 . . ?
N1 C13 C11 122.0(3) . . ?
N1 C13 H13 119.0 . . ?
C11 C13 H13 119.0 . . ?
C12 C14 N1 122.3(3) . . ?
C12 C14 H14 118.8 . . ?
N1 C14 H14 118.8 . . ?
C16 C15 C18 109.2(2) . . ?
C16 C15 H15A 109.8 . . ?
C18 C15 H15A 109.8 . . ?
C16 C15 H15B 109.8 . . ?
C18 C15 H15B 109.8 . . ?
H15A C15 H15B 108.3 . . ?
N1 C16 C15 115.8(2) . . ?
N1 C16 H16A 108.3 . . ?
C15 C16 H16A 108.3 . . ?
N1 C16 H16B 108.3 . . ?
C15 C16 H16B 108.3 . . ?
H16A C16 H16B 107.4 . . ?
C18 C17 C19 113.0(3) . . ?
C18 C17 H17A 109.0 . . ?
C19 C17 H17A 109.0 . . ?
C18 C17 H17B 109.0 . . ?
C19 C17 H17B 109.0 . . ?
H17A C17 H17B 107.8 . . ?
C17 C18 C15 114.5(3) . . ?
C17 C18 H18A 108.6 . . ?
C15 C18 H18A 108.6 . . ?
C17 C18 H18B 108.6 . . ?
C15 C18 H18B 108.6 . . ?
H18A C18 H18B 107.6 . . ?
C20 C19 C17 114.9(3) . . ?
C20 C19 H19A 108.6 . . ?
C17 C19 H19A 108.6 . . ?
C20 C19 H19B 108.6 . . ?
C17 C19 H19B 108.6 . . ?
H19A C19 H19B 107.5 . . ?
C19 C20 C21 113.4(3) . . ?
C19 C20 H20A 108.9 . . ?
C21 C20 H20A 108.9 . . ?
C19 C20 H20B 108.9 . . ?
C21 C20 H20B 108.9 . . ?
H20A C20 H20B 107.7 . . ?
C22 C21 C20 113.5(4) . . ?
C22 C21 H21A 108.9 . . ?
C20 C21 H21A 108.9 . . ?
C22 C21 H21B 108.9 . . ?
C20 C21 H21B 108.9 . . ?
H21A C21 H21B 107.7 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.55
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.096
_database_code_depnum_ccdc_archive 'CCDC 956073'
