# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1450384'
_audit_update_record             
;
2016-01-28 deposited with the CCDC.
2016-08-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        Ni-SSC
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C75 H92 N18 Ni3 O4 S12'
_chemical_formula_weight         1870.52

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
O O 0.0106 0.0060 '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                   18.28(2)
_cell_length_b                   18.49(2)
_cell_length_c                   19.33(2)
_cell_angle_alpha                112.371(12)
_cell_angle_beta                 114.135(11)
_cell_angle_gamma                95.882(11)
_cell_volume                     5250(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    504
_cell_measurement_theta_min      2.74
_cell_measurement_theta_max      16.85

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            'dark blue'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1952
_exptl_absorpt_coefficient_mu    0.819
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_correction_T_min  0.8277
_exptl_absorpt_correction_T_max  0.8404
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      200(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_number            25723
_diffrn_reflns_av_R_equivalents  0.1686
_diffrn_reflns_av_sigmaI/netI    0.7172
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.66
_diffrn_reflns_theta_max         25.00
_reflns_number_total             18178
_reflns_number_gt                2841
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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 
 [0.00000+1.00000exp(7.00(sinθ/λ)²)]/ 
   [σ²(Fo²)+0.0000+0.0000*P+(0.0000P)²+0.0000sinθ/λ] 
 where P = 0.33333Fo² + 0.66667Fc² 
;
_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         18178
_refine_ls_number_parameters     1060
_refine_ls_number_restraints     198
_refine_ls_R_factor_all          0.3250
_refine_ls_R_factor_gt           0.1082
_refine_ls_wR_factor_ref         0.3951
_refine_ls_wR_factor_gt          0.2445
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_restrained_S_all      0.996
_refine_ls_shift/su_max          0.036
_refine_ls_shift/su_mean         0.001

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 0.62065(6) 0.48273(6) 0.23041(6) 0.0613(4) Uani 1 1 d . . .
Ni2 Ni 0.12102(6) -0.18503(7) -0.23309(6) 0.0680(4) Uani 1 1 d . . .
Ni3 Ni 0.34694(6) 0.10873(6) 0.52582(6) 0.0642(4) Uani 1 1 d . . .
S1 S 0.10693(14) -0.31416(14) -0.29117(15) 0.0815(9) Uani 1 1 d . . .
S2 S 0.19465(17) -0.40792(17) -0.20899(19) 0.1127(12) Uani 1 1 d U . .
S3 S 0.53327(13) 0.45118(13) 0.10100(12) 0.0677(8) Uani 1 1 d . . .
S4 S 0.39568(15) 0.28926(15) -0.02359(14) 0.0814(10) Uani 1 1 d . . .
S5 S 0.68283(13) 0.59958(13) 0.25119(12) 0.0667(7) Uani 1 1 d . . .
S6 S 0.80613(13) 0.74112(14) 0.42638(13) 0.0807(8) Uani 1 1 d . . .
S7 S 0.38709(15) 0.10572(14) 0.64445(14) 0.0796(9) Uani 1 1 d . . .
S8 S 0.45922(15) 0.24424(15) 0.81564(14) 0.0849(9) Uani 1 1 d . . .
S9 S 0.04556(13) -0.19018(15) -0.35324(13) 0.0759(9) Uani 1 1 d . . .
S10 S -0.03700(14) -0.06910(16) -0.38668(13) 0.0849(9) Uani 1 1 d . . .
S11 S 0.31467(16) -0.02207(14) 0.46240(14) 0.0852(10) Uani 1 1 d . . .
S12 S 0.23757(16) -0.13226(16) 0.28039(15) 0.0905(11) Uani 1 1 d . . .
N1 N 0.6105(3) 0.0140(4) 0.1796(4) 0.063(2) Uani 1 1 d . . .
N2 N 0.2317(4) -0.2469(4) -0.1327(4) 0.077(2) Uani 1 1 d . . .
N3 N 0.2129(3) -0.1778(3) -0.1382(3) 0.066(2) Uani 1 1 d . . .
N4 N 0.5115(4) 0.3183(4) 0.1256(4) 0.064(2) Uani 1 1 d . . .
N5 N 0.5802(3) 0.3689(3) 0.1962(3) 0.0399(18) Uani 1 1 d . . .
N6 N 0.6395(4) 0.5877(4) 0.6969(4) 0.086(3) Uani 1 1 d . . .
N7 N 0.7246(3) 0.6082(3) 0.4047(3) 0.062(2) Uani 1 1 d D . .
N8 N 0.6702(3) 0.5245(3) 0.3505(3) 0.062(2) Uani 1 1 d D . .
N9 N 0.4338(4) 0.2642(4) 0.6796(3) 0.072(2) Uani 1 1 d . . .
N10 N 0.4055(3) 0.2287(4) 0.5926(3) 0.059(2) Uani 1 1 d . . .
N11 N 0.0413(3) 0.1884(4) 0.1199(3) 0.065(2) Uani 1 1 d . . .
N12 N 0.0490(3) -0.0517(4) -0.2332(4) 0.078(3) Uani 1 1 d D . .
N13 N 0.0980(3) -0.0852(3) -0.1815(3) 0.060(2) Uani 1 1 d D . .
N14 N 0.2579(4) 0.0243(3) 0.3412(3) 0.056(2) Uani 1 1 d . . .
N15 N 0.2828(3) 0.1012(4) 0.4162(3) 0.064(2) Uani 1 1 d . . .
C1 C 0.5329(4) -0.0314(5) 0.1120(5) 0.081(3) Uani 1 1 d . . .
C2 C 0.4865(5) -0.1167(4) 0.0632(4) 0.061(3) Uani 1 1 d . . .
H2B H 0.5115 -0.1553 0.0742 0.073 Uiso 1 1 calc R . .
C3 C 0.4066(4) -0.1407(5) 0.0016(4) 0.069(3) Uani 1 1 d . . .
H3B H 0.3793 -0.1969 -0.0318 0.082 Uiso 1 1 calc R . .
C4 C 0.3601(4) -0.0876(4) -0.0168(4) 0.053(2) Uani 1 1 d U . .
C5 C 0.4088(3) -0.0022(5) 0.0272(4) 0.058(2) Uani 1 1 d . . .
H5B H 0.3851 0.0353 0.0122 0.070 Uiso 1 1 calc R . .
C6 C 0.4924(4) 0.0239(5) 0.0928(4) 0.064(2) Uani 1 1 d U . .
C7 C 0.5507(4) 0.1074(4) 0.1510(4) 0.055(3) Uani 1 1 d . . .
C8 C 0.5498(4) 0.1854(5) 0.1593(4) 0.055(3) Uani 1 1 d . . .
H8A H 0.5021 0.1924 0.1229 0.066 Uiso 1 1 calc R . .
C9 C 0.6191(4) 0.2516(4) 0.2211(4) 0.054(2) Uani 1 1 d . . .
C10 C 0.6918(4) 0.2321(5) 0.2703(5) 0.068(3) Uani 1 1 d . . .
H10A H 0.7404 0.2760 0.3118 0.082 Uiso 1 1 calc R . .
C11 C 0.6966(4) 0.1524(5) 0.2617(4) 0.071(3) Uani 1 1 d . . .
H11A H 0.7443 0.1420 0.2938 0.086 Uiso 1 1 calc R . .
C12 C 0.6231(4) 0.0955(4) 0.2015(4) 0.053(3) Uani 1 1 d . . .
C13 C 0.6688(5) -0.0240(6) 0.2158(6) 0.101(4) Uani 1 1 d . . .
H13A H 0.6381 -0.0661 0.2208 0.122 Uiso 1 1 calc R . .
H13B H 0.7099 0.0172 0.2736 0.122 Uiso 1 1 calc R . .
C14 C 0.7169(4) -0.0631(5) 0.1721(5) 0.073(3) Uani 1 1 d . . .
H14A H 0.6772 -0.1052 0.1143 0.087 Uiso 1 1 calc R . .
H14B H 0.7501 -0.0217 0.1684 0.087 Uiso 1 1 calc R . .
C15 C 0.7724(5) -0.0997(5) 0.2175(6) 0.091(4) Uani 1 1 d . . .
H15A H 0.7392 -0.1384 0.2241 0.109 Uiso 1 1 calc R . .
H15B H 0.8134 -0.0567 0.2744 0.109 Uiso 1 1 calc R . .
C16 C 0.8190(6) -0.1437(6) 0.1743(7) 0.114(6) Uani 1 1 d . . .
H16A H 0.8525 -0.1676 0.2071 0.171 Uiso 1 1 calc R . .
H16B H 0.8549 -0.1052 0.1707 0.171 Uiso 1 1 calc R . .
H16C H 0.7791 -0.1862 0.1177 0.171 Uiso 1 1 calc R . .
C17 C 0.2749(4) -0.1127(5) -0.0858(4) 0.058(2) Uani 1 1 d U . .
H17A H 0.2619 -0.0683 -0.0942 0.070 Uiso 1 1 calc R . .
C18 C 0.1814(4) -0.3111(5) -0.2024(5) 0.073(3) Uani 1 1 d . . .
C19 C 0.2698(6) -0.3834(5) -0.1068(6) 0.114(4) Uani 1 1 d U . .
H19A H 0.2833 -0.4319 -0.1056 0.172 Uiso 1 1 calc R . .
H19B H 0.2484 -0.3615 -0.0680 0.172 Uiso 1 1 calc R . .
H19C H 0.3196 -0.3431 -0.0899 0.172 Uiso 1 1 calc R . .
C20 C 0.6310(4) 0.3408(4) 0.2388(4) 0.063(3) Uani 1 1 d . . .
H20A H 0.6812 0.3790 0.2861 0.076 Uiso 1 1 calc R . .
C21 C 0.4833(4) 0.3502(4) 0.0773(4) 0.057(2) Uani 1 1 d . . .
C22 C 0.3599(6) 0.3564(5) -0.0658(6) 0.106(5) Uani 1 1 d . . .
H22A H 0.3118 0.3252 -0.1218 0.159 Uiso 1 1 calc R . .
H22B H 0.4040 0.3850 -0.0694 0.159 Uiso 1 1 calc R . .
H22C H 0.3445 0.3954 -0.0289 0.159 Uiso 1 1 calc R . .
C23 C 0.6897(4) 0.6399(5) 0.6184(4) 0.072(3) Uani 1 1 d . . .
H23A H 0.7173 0.6941 0.6609 0.087 Uiso 1 1 calc R . .
C24 C 0.6865(5) 0.6086(6) 0.5353(5) 0.090(4) Uani 1 1 d . . .
H24A H 0.7145 0.6455 0.5256 0.108 Uiso 1 1 calc R . .
C25 C 0.6443(4) 0.5264(4) 0.4674(4) 0.055(2) Uani 1 1 d . . .
C26 C 0.6337(6) 0.4927(5) 0.3825(5) 0.083(4) Uani 1 1 d . . .
H26A H 0.5953 0.4404 0.3446 0.100 Uiso 1 1 calc R . .
C27 C 0.5989(4) 0.4686(5) 0.4777(4) 0.075(3) Uani 1 1 d . . .
H27A H 0.5695 0.4150 0.4343 0.091 Uiso 1 1 calc R . .
C28 C 0.6002(4) 0.4971(4) 0.5603(5) 0.065(3) Uani 1 1 d . . .
C29 C 0.6466(4) 0.5797(5) 0.6275(4) 0.063(3) Uani 1 1 d . . .
C30 C 0.5634(5) 0.4528(5) 0.5915(4) 0.062(3) Uani 1 1 d . . .
C31 C 0.5092(4) 0.3747(4) 0.5581(4) 0.049(2) Uani 1 1 d . . .
H31A H 0.4907 0.3368 0.5016 0.059 Uiso 1 1 calc R . .
C32 C 0.4825(5) 0.3522(5) 0.6058(5) 0.070(3) Uani 1 1 d . . .
C33 C 0.5122(5) 0.4135(4) 0.6931(5) 0.065(3) Uani 1 1 d . . .
H33A H 0.4996 0.3980 0.7284 0.078 Uiso 1 1 calc R . .
C34 C 0.5584(5) 0.4939(6) 0.7265(5) 0.092(4) Uani 1 1 d . . .
H34A H 0.5713 0.5345 0.7801 0.110 Uiso 1 1 calc R . .
C35 C 0.5847(5) 0.5095(5) 0.6722(5) 0.081(3) Uani 1 1 d . . .
C36 C 0.6771(5) 0.6635(5) 0.7789(5) 0.090(3) Uani 1 1 d . . .
H36A H 0.7313 0.6937 0.7913 0.108 Uiso 1 1 calc R . .
H36B H 0.6856 0.6501 0.8249 0.108 Uiso 1 1 calc R . .
C37 C 0.6177(5) 0.7160(5) 0.7723(6) 0.099(4) Uani 1 1 d . . .
H37A H 0.5704 0.6911 0.7752 0.119 Uiso 1 1 calc R . .
H37B H 0.5957 0.7133 0.7161 0.119 Uiso 1 1 calc R . .
C38 C 0.6550(6) 0.8099(7) 0.8415(7) 0.140(6) Uani 1 1 d . . .
H38A H 0.6938 0.8391 0.8316 0.168 Uiso 1 1 calc R . .
H38B H 0.6098 0.8343 0.8364 0.168 Uiso 1 1 calc R . .
C39 C 0.6982(6) 0.8172(7) 0.9259(5) 0.113(5) Uani 1 1 d . . .
H39A H 0.7223 0.8742 0.9674 0.170 Uiso 1 1 calc R . .
H39B H 0.7421 0.7919 0.9303 0.170 Uiso 1 1 calc R . .
H39C H 0.6591 0.7903 0.9364 0.170 Uiso 1 1 calc R . .
C40 C 0.7341(4) 0.6437(4) 0.3607(4) 0.056(3) Uani 1 1 d . . .
C41 C 0.7888(6) 0.7838(5) 0.3529(5) 0.103(4) Uani 1 1 d . . .
H41A H 0.8262 0.8388 0.3832 0.154 Uiso 1 1 calc R . .
H41B H 0.7316 0.7846 0.3284 0.154 Uiso 1 1 calc R . .
H41C H 0.7995 0.7507 0.3081 0.154 Uiso 1 1 calc R . .
C42 C 0.4305(4) 0.2668(4) 0.5622(4) 0.059(2) Uani 1 1 d . . .
H42A H 0.4142 0.2376 0.5044 0.071 Uiso 1 1 calc R . .
C43 C 0.4251(4) 0.2133(5) 0.7079(4) 0.059(3) Uani 1 1 d . . .
C44 C 0.5184(5) 0.3509(5) 0.8654(5) 0.087(4) Uani 1 1 d . . .
H44A H 0.5413 0.3743 0.9263 0.130 Uiso 1 1 calc R . .
H44B H 0.4820 0.3800 0.8441 0.130 Uiso 1 1 calc R . .
H44C H 0.5635 0.3552 0.8523 0.130 Uiso 1 1 calc R . .
C45 C 0.0530(4) 0.1323(5) 0.0543(4) 0.064(3) Uani 1 1 d . . .
C46 C 0.0166(4) 0.1163(5) -0.0311(4) 0.062(3) Uani 1 1 d . . .
H46A H -0.0194 0.1440 -0.0517 0.075 Uiso 1 1 calc R . .
C47 C 0.0369(5) 0.0569(4) -0.0837(5) 0.069(3) Uani 1 1 d . . .
H47A H 0.0169 0.0469 -0.1401 0.083 Uiso 1 1 calc R . .
C48 C 0.0864(5) 0.0117(4) -0.0542(5) 0.064(3) Uani 1 1 d . . .
C49 C 0.1237(4) 0.0263(4) 0.0319(4) 0.053(3) Uani 1 1 d . . .
H49A H 0.1568 -0.0043 0.0507 0.064 Uiso 1 1 calc R . .
C50 C 0.1073(4) 0.0918(5) 0.0894(4) 0.068(3) Uani 1 1 d . . .
C51 C 0.1306(4) 0.1232(4) 0.1786(3) 0.046(2) Uani 1 1 d U . .
C52 C 0.1800(4) 0.1122(4) 0.2457(3) 0.044(2) Uani 1 1 d U . .
H52A H 0.2066 0.0719 0.2373 0.053 Uiso 1 1 calc R . .
C53 C 0.1912(4) 0.1580(4) 0.3237(4) 0.048(2) Uani 1 1 d U . .
C54 C 0.1469(4) 0.2179(4) 0.3399(5) 0.062(3) Uani 1 1 d . . .
H54A H 0.1544 0.2481 0.3946 0.075 Uiso 1 1 calc R . .
C55 C 0.0934(4) 0.2293(4) 0.2725(4) 0.051(3) Uani 1 1 d . . .
H55A H 0.0630 0.2663 0.2800 0.061 Uiso 1 1 calc R . .
C56 C 0.0868(4) 0.1837(4) 0.1938(4) 0.049(2) Uani 1 1 d . . .
C57 C -0.0173(5) 0.2395(4) 0.1055(6) 0.110(3) Uani 1 1 d DU . .
H57A H -0.0433 0.2473 0.1416 0.132 Uiso 1 1 calc R . .
H57B H -0.0611 0.2141 0.0461 0.132 Uiso 1 1 calc R . .
C58 C 0.0463(5) 0.3281(4) 0.1325(7) 0.148(4) Uani 1 1 d DU B .
H58A H 0.0944 0.3512 0.1894 0.178 Uiso 1 1 calc R . .
H58B H 0.0653 0.3233 0.0913 0.178 Uiso 1 1 calc R . .
C59 C -0.0228(4) 0.3803(5) 0.1283(7) 0.195(5) Uani 1 1 d DU . .
H59C H -0.0062 0.4262 0.1203 0.234 Uiso 0.50 1 d PR A 1
H59D H -0.0220 0.4011 0.1823 0.234 Uiso 0.50 1 d PR A 1
H59A H 0.0102 0.4371 0.1591 0.234 Uiso 0.50 1 d PR A 2
H59B H -0.0462 0.3716 0.1618 0.234 Uiso 0.50 1 d PR A 2
C60 C -0.1209(7) 0.3213(6) 0.0502(8) 0.226(9) Uani 0.54(2) 1 d PDU B 1
H60A H -0.1491 0.2979 0.0726 0.340 Uiso 0.54(2) 1 calc PR B 1
H60B H -0.1185 0.2782 0.0045 0.340 Uiso 0.54(2) 1 calc PR B 1
H60C H -0.1513 0.3542 0.0289 0.340 Uiso 0.54(2) 1 calc PR B 1
C60' C -0.1058(9) 0.3704(7) 0.0413(7) 0.185(5) Uiso 0.46(2) 1 d PDU B 2
H60D H -0.0867 0.3907 0.0107 0.277 Uiso 0.46(2) 1 calc PR B 2
H60E H -0.1400 0.4013 0.0581 0.277 Uiso 0.46(2) 1 calc PR B 2
H60F H -0.1383 0.3135 0.0049 0.277 Uiso 0.46(2) 1 calc PR B 2
C61 C 0.1107(4) -0.0533(4) -0.1034(4) 0.069(3) Uani 1 1 d . . .
H61A H 0.1422 -0.0771 -0.0720 0.083 Uiso 1 1 calc R . .
C62 C 0.0259(4) -0.0924(5) -0.3109(4) 0.070(3) Uani 1 1 d . . .
C63 C -0.0596(5) 0.0165(6) -0.3236(5) 0.084(4) Uani 1 1 d . . .
H63A H -0.0956 0.0361 -0.3599 0.126 Uiso 1 1 calc R . .
H63B H -0.0079 0.0598 -0.2802 0.126 Uiso 1 1 calc R . .
H63C H -0.0872 -0.0006 -0.2971 0.126 Uiso 1 1 calc R . .
C64 C 0.2486(4) 0.1640(4) 0.4078(4) 0.057(2) Uani 1 1 d . . .
H64A H 0.2625 0.2115 0.4572 0.069 Uiso 1 1 calc R . .
C65 C 0.2687(4) -0.0328(4) 0.3569(5) 0.059(3) Uani 1 1 d . . .
C66 C 0.1590(6) -0.1250(6) 0.1900(6) 0.112(5) Uani 1 1 d . . .
H66A H 0.1337 -0.1778 0.1402 0.168 Uiso 1 1 calc R . .
H66B H 0.1853 -0.0859 0.1792 0.168 Uiso 1 1 calc R . .
H66C H 0.1163 -0.1074 0.2027 0.168 Uiso 1 1 calc R . .
O101 O -0.0352(9) 0.2059(11) -0.2988(12) 0.197(8) Uani 0.50 1 d P . .
N101 N -0.0937(4) 0.1368(6) -0.4434(6) 0.065(3) Uani 0.50 1 d P . .
C101 C -0.1094(4) 0.1899(8) -0.3752(5) 0.242(6) Uani 0.50 1 d PD . .
H10B H -0.1559 0.2084 -0.3804 0.290 Uiso 0.50 1 calc PR . .
C102 C -0.0156(5) 0.1442(9) -0.4185(7) 0.097(5) Uani 0.50 1 d PDU . .
H10E H -0.0095 0.1058 -0.4645 0.146 Uiso 0.50 1 calc PR . .
H10F H 0.0075 0.1332 -0.3705 0.146 Uiso 0.50 1 calc PR . .
H10G H 0.0138 0.1991 -0.4019 0.146 Uiso 0.50 1 calc PR . .
C103 C -0.1518(7) 0.1190(13) -0.5199(5) 0.163(10) Uani 0.50 1 d PD . .
H10H H -0.1403 0.0815 -0.5617 0.244 Uiso 0.50 1 calc PR . .
H10I H -0.1523 0.1683 -0.5255 0.244 Uiso 0.50 1 calc PR . .
H10J H -0.2057 0.0939 -0.5288 0.244 Uiso 0.50 1 calc PR . .
N121 N 0.5248(5) 1.1368(6) 0.3859(5) 0.136(4) Uani 1 1 d . . .
O121 O 0.4252(4) 1.1972(5) 0.3727(4) 0.130(4) Uani 1 1 d . . .
C121 C 0.5001(5) 1.1865(5) 0.3713(6) 0.247(10) Uani 1 1 d D . .
H12A H 0.5290 1.2195 0.3587 0.296 Uiso 1 1 calc R . .
C122 C 0.5956(5) 1.1107(5) 0.3805(6) 0.186(7) Uani 1 1 d D . .
H12D H 0.6141 1.1342 0.3517 0.279 Uiso 1 1 calc R . .
H12E H 0.5785 1.0518 0.3491 0.279 Uiso 1 1 calc R . .
H12F H 0.6410 1.1287 0.4372 0.279 Uiso 1 1 calc R . .
C123 C 0.4983(5) 1.0945(6) 0.4287(6) 0.246(9) Uani 1 1 d D . .
H12G H 0.4492 1.1067 0.4307 0.369 Uiso 1 1 calc R . .
H12H H 0.5432 1.1137 0.4858 0.369 Uiso 1 1 calc R . .
H12I H 0.4857 1.0362 0.3967 0.369 Uiso 1 1 calc R . .
N111 N 0.3291(5) -0.1042(6) 0.1486(5) 0.153(4) Uani 1 1 d . C 1
O111 O 0.2109(4) -0.1147(4) 0.0396(4) 0.113(3) Uani 1 1 d . C 1
C111 C 0.2579(6) -0.1519(5) 0.0719(5) 0.198(8) Uani 1 1 d D C 1
H11C H 0.2446 -0.2088 0.0446 0.238 Uiso 1 1 calc R C 1
C112 C 0.3932(6) -0.1382(5) 0.1928(7) 0.400(6) Uani 1 1 d D C 1
H11D H 0.3702 -0.1968 0.1664 0.600 Uiso 1 1 calc R C 1
H11E H 0.4078 -0.1148 0.2521 0.600 Uiso 1 1 calc R C 1
H11F H 0.4426 -0.1247 0.1882 0.600 Uiso 1 1 calc R C 1
C113 C 0.3571(7) -0.0109(6) 0.1881(7) 0.252(10) Uani 1 1 d D C 1
H11G H 0.3139 0.0064 0.1555 0.378 Uiso 1 1 calc R C 1
H11H H 0.4080 0.0073 0.1877 0.378 Uiso 1 1 calc R C 1
H11I H 0.3671 0.0124 0.2460 0.378 Uiso 1 1 calc R C 1
O1W O 0.3090(8) 0.6772(8) 0.2651(12) 0.349(13) Uani 1 1 d . . .
N141 N 0.8524(9) 0.4934(10) 0.5376(19) 0.234(7) Uani 0.50 1 d PDU . .
C143 C 0.8722(10) 0.5581(7) 0.6050(6) 0.196(6) Uani 0.50 1 d PDU . .
H14C H 0.8583 0.5442 0.6421 0.295 Uiso 0.50 1 calc PR . .
H14D H 0.8416 0.5940 0.5902 0.295 Uiso 0.50 1 calc PR . .
H14E H 0.9315 0.5854 0.6338 0.295 Uiso 0.50 1 calc PR . .
C142 C 0.8786(8) 0.5149(7) 0.4796(6) 0.235(9) Uani 0.50 1 d PDU . .
H14F H 0.8635 0.4656 0.4286 0.352 Uiso 0.50 1 calc PR . .
H14G H 0.9384 0.5407 0.5098 0.352 Uiso 0.50 1 calc PR . .
H14H H 0.8502 0.5519 0.4645 0.352 Uiso 0.50 1 calc PR . .
C141 C 0.8148(12) 0.4210(6) 0.5062(9) 0.245(7) Uani 0.50 1 d PDU . .
H14I H 0.8428 0.3879 0.5259 0.293 Uiso 0.50 1 calc PR . .
O141 O 0.7371(10) 0.3890(11) 0.4462(19) 0.268(9) Uani 0.50 1 d PDU . .


_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 N8 1.892(6) . ?
Ni1 N5 1.907(6) . ?
Ni1 S3 2.140(3) . ?
Ni1 S5 2.141(4) . ?
Ni2 N3 1.858(6) . ?
Ni2 N13 1.918(6) . ?
Ni2 S9 2.119(4) . ?
Ni2 S1 2.151(4) . ?
Ni3 N15 1.895(7) . ?
Ni3 N10 1.984(6) . ?
Ni3 S7 2.129(4) . ?
Ni3 S11 2.135(4) . ?
S1 C18 1.674(9) . ?
S2 C19 1.722(10) . ?
S2 C18 1.794(10) . ?
S3 C21 1.785(8) . ?
S4 C21 1.744(6) . ?
S4 C22 1.771(11) . ?
S5 C40 1.712(8) . ?
S6 C40 1.731(6) . ?
S6 C41 1.811(11) . ?
S7 C43 1.762(8) . ?
S8 C43 1.735(8) . ?
S8 C44 1.803(9) . ?
S9 C62 1.820(9) . ?
S10 C62 1.692(9) . ?
S10 C63 1.800(10) . ?
S11 C65 1.779(9) . ?
S12 C65 1.709(7) . ?
S12 C66 1.818(11) . ?
N1 C1 1.352(8) . ?
N1 C12 1.367(10) . ?
N1 C13 1.428(13) . ?
N2 C18 1.271(8) . ?
N2 N3 1.387(10) . ?
N3 C17 1.270(7) . ?
N4 C21 1.254(11) . ?
N4 N5 1.305(6) . ?
N5 C20 1.267(9) . ?
N6 C29 1.354(12) . ?
N6 C35 1.452(12) . ?
N6 C36 1.474(9) . ?
N7 C40 1.307(11) . ?
N7 N8 1.442(7) . ?
N8 C26 1.306(13) . ?
N9 C43 1.282(12) . ?
N9 N10 1.381(8) . ?
N10 C42 1.233(11) . ?
N11 C56 1.370(10) . ?
N11 C45 1.413(10) . ?
N11 C57 1.511(11) . ?
N12 C62 1.247(9) . ?
N12 N13 1.428(9) . ?
N13 C61 1.299(10) . ?
N14 C65 1.218(10) . ?
N14 N15 1.445(8) . ?
N15 C64 1.406(10) . ?
C1 C6 1.396(13) . ?
C1 C2 1.427(10) . ?
C2 C3 1.339(9) . ?
C3 C4 1.416(11) . ?
C4 C5 1.441(9) . ?
C4 C17 1.449(8) . ?
C5 C6 1.406(8) . ?
C6 C7 1.464(9) . ?
C7 C12 1.385(10) . ?
C7 C8 1.392(12) . ?
C8 C9 1.364(8) . ?
C9 C10 1.460(11) . ?
C9 C20 1.524(11) . ?
C10 C11 1.434(13) . ?
C11 C12 1.328(8) . ?
C13 C14 1.510(14) . ?
C14 C15 1.457(13) . ?
C15 C16 1.514(16) . ?
C23 C29 1.406(13) . ?
C23 C24 1.459(13) . ?
C24 C25 1.429(10) . ?
C25 C27 1.409(13) . ?
C25 C26 1.436(11) . ?
C27 C28 1.466(12) . ?
C28 C29 1.436(9) . ?
C28 C30 1.443(13) . ?
C30 C35 1.364(10) . ?
C30 C31 1.399(10) . ?
C31 C32 1.372(13) . ?
C32 C33 1.448(10) . ?
C32 C42 1.460(10) . ?
C33 C34 1.380(12) . ?
C34 C35 1.425(15) . ?
C36 C37 1.527(14) . ?
C37 C38 1.585(13) . ?
C38 C39 1.436(15) . ?
C45 C46 1.396(11) . ?
C45 C50 1.412(12) . ?
C46 C47 1.386(12) . ?
C47 C48 1.391(12) . ?
C48 C49 1.415(11) . ?
C48 C61 1.460(11) . ?
C49 C50 1.453(11) . ?
C50 C51 1.443(10) . ?
C51 C52 1.348(10) . ?
C51 C56 1.450(11) . ?
C52 C53 1.333(9) . ?
C53 C54 1.452(11) . ?
C53 C64 1.483(10) . ?
C54 C55 1.381(11) . ?
C55 C56 1.377(10) . ?
C57 C58 1.665(10) . ?
C58 C59 1.662(10) . ?
C59 C60' 1.669(12) . ?
C59 C60 1.678(10) . ?
O101 C101 1.435(19) . ?
N101 C102 1.278(11) . ?
N101 C103 1.303(13) . ?
N101 C101 1.471(14) . ?
N121 C121 1.143(16) . ?
N121 C122 1.455(14) . ?
N121 C123 1.508(17) . ?
O121 C121 1.412(13) . ?
N111 C111 1.364(10) . ?
N111 C112 1.497(14) . ?
N111 C113 1.522(14) . ?
O111 C111 1.269(13) . ?
N141 C141 1.217(19) . ?
N141 C143 1.26(2) . ?
N141 C142 1.54(4) . ?
C141 O141 1.29(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
N8 Ni1 N5 99.2(3) . . ?
N8 Ni1 S3 161.1(2) . . ?
N5 Ni1 S3 85.30(16) . . ?
N8 Ni1 S5 88.8(2) . . ?
N5 Ni1 S5 165.4(2) . . ?
S3 Ni1 S5 91.09(10) . . ?
N3 Ni2 N13 100.5(3) . . ?
N3 Ni2 S9 161.8(2) . . ?
N13 Ni2 S9 87.5(2) . . ?
N3 Ni2 S1 85.8(2) . . ?
N13 Ni2 S1 159.6(2) . . ?
S9 Ni2 S1 92.25(11) . . ?
N15 Ni3 N10 99.4(3) . . ?
N15 Ni3 S7 164.9(2) . . ?
N10 Ni3 S7 87.8(2) . . ?
N15 Ni3 S11 87.0(2) . . ?
N10 Ni3 S11 165.9(2) . . ?
S7 Ni3 S11 89.06(12) . . ?
C18 S1 Ni2 95.0(3) . . ?
C19 S2 C18 104.1(4) . . ?
C21 S3 Ni1 93.3(3) . . ?
C21 S4 C22 106.6(4) . . ?
C40 S5 Ni1 95.8(3) . . ?
C40 S6 C41 102.4(4) . . ?
C43 S7 Ni3 95.2(3) . . ?
C43 S8 C44 102.5(4) . . ?
C62 S9 Ni2 96.3(3) . . ?
C62 S10 C63 101.1(4) . . ?
C65 S11 Ni3 95.6(2) . . ?
C65 S12 C66 98.7(4) . . ?
C1 N1 C12 110.7(7) . . ?
C1 N1 C13 121.1(7) . . ?
C12 N1 C13 128.1(5) . . ?
C18 N2 N3 110.0(7) . . ?
C17 N3 N2 112.9(6) . . ?
C17 N3 Ni2 122.3(6) . . ?
N2 N3 Ni2 122.1(4) . . ?
C21 N4 N5 111.7(6) . . ?
C20 N5 N4 119.7(6) . . ?
C20 N5 Ni1 115.8(4) . . ?
N4 N5 Ni1 123.6(5) . . ?
C29 N6 C35 106.6(6) . . ?
C29 N6 C36 125.4(8) . . ?
C35 N6 C36 127.9(8) . . ?
C40 N7 N8 112.2(5) . . ?
C26 N8 N7 117.0(6) . . ?
C26 N8 Ni1 119.7(4) . . ?
N7 N8 Ni1 118.5(5) . . ?
C43 N9 N10 114.8(6) . . ?
C42 N10 N9 120.1(6) . . ?
C42 N10 Ni3 121.5(5) . . ?
N9 N10 Ni3 116.9(6) . . ?
C56 N11 C45 108.8(7) . . ?
C56 N11 C57 127.6(6) . . ?
C45 N11 C57 123.4(7) . . ?
C62 N12 N13 113.7(7) . . ?
C61 N13 N12 115.4(7) . . ?
C61 N13 Ni2 123.1(6) . . ?
N12 N13 Ni2 120.2(4) . . ?
C65 N14 N15 113.6(7) . . ?
C64 N15 N14 119.9(5) . . ?
C64 N15 Ni3 120.5(4) . . ?
N14 N15 Ni3 118.7(5) . . ?
N1 C1 C6 106.6(7) . . ?
N1 C1 C2 135.3(9) . . ?
C6 C1 C2 118.0(6) . . ?
C3 C2 C1 119.3(8) . . ?
C2 C3 C4 125.4(7) . . ?
C3 C4 C5 114.9(6) . . ?
C3 C4 C17 125.9(6) . . ?
C5 C4 C17 118.0(7) . . ?
C6 C5 C4 119.5(7) . . ?
C1 C6 C5 122.1(7) . . ?
C1 C6 C7 108.9(6) . . ?
C5 C6 C7 129.1(8) . . ?
C12 C7 C8 120.5(6) . . ?
C12 C7 C6 103.4(7) . . ?
C8 C7 C6 135.8(6) . . ?
C9 C8 C7 119.9(7) . . ?
C8 C9 C10 114.8(7) . . ?
C8 C9 C20 127.7(7) . . ?
C10 C9 C20 117.3(5) . . ?
C11 C10 C9 127.0(6) . . ?
C12 C11 C10 110.4(7) . . ?
C11 C12 N1 122.5(7) . . ?
C11 C12 C7 127.2(8) . . ?
N1 C12 C7 110.2(5) . . ?
N1 C13 C14 120.0(9) . . ?
C15 C14 C13 112.3(9) . . ?
C14 C15 C16 114.7(10) . . ?
N3 C17 C4 138.3(8) . . ?
N2 C18 S1 126.3(8) . . ?
N2 C18 S2 117.3(7) . . ?
S1 C18 S2 116.3(4) . . ?
N5 C20 C9 127.3(5) . . ?
N4 C21 S4 118.2(6) . . ?
N4 C21 S3 124.0(5) . . ?
S4 C21 S3 117.5(5) . . ?
C29 C23 C24 113.0(7) . . ?
C25 C24 C23 125.9(9) . . ?
C27 C25 C24 119.4(8) . . ?
C27 C25 C26 111.4(6) . . ?
C24 C25 C26 128.9(8) . . ?
N8 C26 C25 129.6(7) . . ?
C25 C27 C28 116.8(6) . . ?
C29 C28 C30 108.5(7) . . ?
C29 C28 C27 121.3(8) . . ?
C30 C28 C27 130.1(6) . . ?
N6 C29 C23 127.9(6) . . ?
N6 C29 C28 108.5(8) . . ?
C23 C29 C28 123.5(8) . . ?
C35 C30 C31 117.9(9) . . ?
C35 C30 C28 104.9(7) . . ?
C31 C30 C28 136.8(6) . . ?
C32 C31 C30 122.2(6) . . ?
C31 C32 C33 117.0(7) . . ?
C31 C32 C42 114.6(7) . . ?
C33 C32 C42 128.3(9) . . ?
C34 C33 C32 123.2(9) . . ?
C33 C34 C35 114.5(8) . . ?
C30 C35 C34 124.6(8) . . ?
C30 C35 N6 111.3(9) . . ?
C34 C35 N6 124.1(7) . . ?
N6 C36 C37 108.7(6) . . ?
C36 C37 C38 117.5(7) . . ?
C39 C38 C37 109.8(11) . . ?
N7 C40 S5 124.6(5) . . ?
N7 C40 S6 111.9(5) . . ?
S5 C40 S6 123.5(5) . . ?
N10 C42 C32 127.9(7) . . ?
N9 C43 S8 122.5(5) . . ?
N9 C43 S7 123.9(6) . . ?
S8 C43 S7 113.3(5) . . ?
C46 C45 N11 127.5(8) . . ?
C46 C45 C50 124.6(8) . . ?
N11 C45 C50 107.9(7) . . ?
C47 C46 C45 116.4(8) . . ?
C46 C47 C48 121.7(8) . . ?
C47 C48 C49 122.8(8) . . ?
C47 C48 C61 126.9(8) . . ?
C49 C48 C61 110.2(7) . . ?
C48 C49 C50 116.3(7) . . ?
C45 C50 C51 108.7(7) . . ?
C45 C50 C49 117.9(7) . . ?
C51 C50 C49 133.2(8) . . ?
C52 C51 C50 137.8(7) . . ?
C52 C51 C56 117.6(6) . . ?
C50 C51 C56 104.6(6) . . ?
C53 C52 C51 121.1(7) . . ?
C52 C53 C54 122.1(7) . . ?
C52 C53 C64 131.0(7) . . ?
C54 C53 C64 106.8(6) . . ?
C55 C54 C53 118.7(7) . . ?
C56 C55 C54 117.3(7) . . ?
N11 C56 C55 126.9(7) . . ?
N11 C56 C51 110.0(6) . . ?
C55 C56 C51 123.1(7) . . ?
N11 C57 C58 103.1(6) . . ?
C59 C58 C57 96.9(7) . . ?
C58 C59 C60' 127.7(10) . . ?
C58 C59 C60 112.2(7) . . ?
C60' C59 C60 35.5(6) . . ?
N13 C61 C48 134.1(8) . . ?
N12 C62 S10 123.3(7) . . ?
N12 C62 S9 121.9(7) . . ?
S10 C62 S9 114.3(4) . . ?
N15 C64 C53 123.0(6) . . ?
N14 C65 S12 124.0(6) . . ?
N14 C65 S11 123.3(5) . . ?
S12 C65 S11 112.6(5) . . ?
C102 N101 C103 126.9(12) . . ?
C102 N101 C101 113.3(8) . . ?
C103 N101 C101 113.1(10) . . ?
O101 C101 N101 102.6(11) . . ?
C121 N121 C122 128.3(11) . . ?
C121 N121 C123 125.4(10) . . ?
C122 N121 C123 105.6(9) . . ?
N121 C121 O121 119.3(11) . . ?
C111 N111 C112 123.2(9) . . ?
C111 N111 C113 121.9(9) . . ?
C112 N111 C113 114.0(6) . . ?
O111 C111 N111 116.7(8) . . ?
C141 N141 C143 136(3) . . ?
C141 N141 C142 114(2) . . ?
C143 N141 C142 109.7(17) . . ?
N141 C141 O141 122(2) . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.103
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1450385'
_audit_update_record             
;
2016-01-28 deposited with the CCDC.
2016-08-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        Ni-MSSC-cis
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H40 N6 Ni S4'
_chemical_formula_weight         767.71

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

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P2(1)2(1)2(1) '

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'

_cell_length_a                   8.454(2)
_cell_length_b                   18.860(4)
_cell_length_c                   23.003(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3667.7(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    1889
_cell_measurement_theta_min      2.57
_cell_measurement_theta_max      18.90

_exptl_crystal_description       block
_exptl_crystal_colour            'dark blue'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1608
_exptl_absorpt_coefficient_mu    0.794
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      200(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_number            19072
_diffrn_reflns_av_R_equivalents  0.0854
_diffrn_reflns_av_sigmaI/netI    0.0965
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.77
_diffrn_reflns_theta_max         24.99
_reflns_number_total             6452
_reflns_number_gt                4686
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0522P)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     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_number_reflns         6452
_refine_ls_number_parameters     437
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0556
_refine_ls_wR_factor_ref         0.1268
_refine_ls_wR_factor_gt          0.1143
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.012
_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 0.52933(8) 0.16347(3) 0.80446(3) 0.02822(18) Uani 1 1 d . . .
S1 S 0.51068(17) 0.04911(7) 0.80947(6) 0.0339(3) Uani 1 1 d . . .
S2 S 0.37244(18) -0.03792(7) 0.71627(7) 0.0376(4) Uani 1 1 d . . .
S3 S 0.5521(2) 0.17178(8) 0.89765(6) 0.0401(4) Uani 1 1 d . . .
S4 S 0.6613(3) 0.30992(9) 0.95527(7) 0.0562(5) Uani 1 1 d . . .
N5 N 0.4854(5) 0.2634(2) 0.80494(18) 0.0301(10) Uani 1 1 d . . .
N2 N 0.5638(5) 0.1511(2) 0.72297(19) 0.0282(10) Uani 1 1 d . . .
N6 N 0.5523(6) 0.3032(2) 0.8516(2) 0.0358(11) Uani 1 1 d . . .
N3 N 0.4949(5) 0.08994(19) 0.69696(19) 0.0288(10) Uani 1 1 d . . .
C18 C 0.4652(7) 0.0413(3) 0.7356(2) 0.0285(12) Uani 1 1 d . . .
C13 C 0.7267(6) 0.2537(3) 0.6936(2) 0.0269(12) Uani 1 1 d . . .
C11 C 0.8967(6) 0.3310(3) 0.7482(2) 0.0259(12) Uani 1 1 d . . .
C10 C 0.9938(6) 0.3641(3) 0.7934(2) 0.0298(13) Uani 1 1 d . . .
N4 N 0.0515(6) 0.2207(2) 0.5745(2) 0.0366(12) Uani 1 1 d . . .
C34 C 0.1511(7) 0.1860(3) 0.6724(2) 0.0329(14) Uani 1 1 d . . .
H34A H 0.1030 0.1417 0.6725 0.040 Uiso 1 1 calc R . .
N1 N 1.0015(5) 0.4339(2) 0.71228(19) 0.0309(11) Uani 1 1 d . . .
C5 C 1.0553(7) 0.4270(3) 0.7682(3) 0.0316(13) Uani 1 1 d . . .
C36 C 0.4046(7) 0.3013(3) 0.7696(2) 0.0323(14) Uani 1 1 d . . .
H36A H 0.4052 0.3500 0.7759 0.039 Uiso 1 1 calc R . .
C9 C 1.0323(7) 0.3471(3) 0.8502(2) 0.0363(13) Uani 1 1 d . . .
H9A H 0.9915 0.3064 0.8674 0.044 Uiso 1 1 calc R . .
C28 C 0.1729(7) 0.4006(3) 0.5472(3) 0.0396(15) Uani 1 1 d . . .
H28A H 0.2345 0.4340 0.5664 0.048 Uiso 1 1 calc R . .
C16 C 0.9046(6) 0.3771(3) 0.6993(2) 0.0278(12) Uani 1 1 d . . .
C24 C 0.0599(7) 0.2823(3) 0.5414(3) 0.0382(15) Uani 1 1 d . . .
C37 C 0.5836(7) 0.2637(3) 0.8952(2) 0.0343(14) Uani 1 1 d . . .
C6 C 1.1557(7) 0.4722(3) 0.7997(3) 0.0370(14) Uani 1 1 d . . .
H6B H 1.1955 0.5136 0.7834 0.044 Uiso 1 1 calc R . .
C14 C 0.7409(6) 0.2997(3) 0.6463(3) 0.0317(14) Uani 1 1 d . . .
H14A H 0.6897 0.2877 0.6119 0.038 Uiso 1 1 calc R . .
C4 C 1.0383(7) 0.4936(3) 0.6736(2) 0.0356(14) Uani 1 1 d . . .
H4A H 1.0141 0.4801 0.6339 0.043 Uiso 1 1 calc R . .
H4B H 1.1507 0.5036 0.6758 0.043 Uiso 1 1 calc R . .
C30 C 0.2057(7) 0.2991(3) 0.6249(2) 0.0316(14) Uani 1 1 d . . .
C17 C 0.6342(6) 0.1901(3) 0.6846(2) 0.0264(12) Uani 1 1 d . . .
H17A H 0.6239 0.1754 0.6462 0.032 Uiso 1 1 calc R . .
C12 C 0.8075(7) 0.2701(3) 0.7453(2) 0.0277(13) Uani 1 1 d . . .
H12A H 0.8008 0.2400 0.7772 0.033 Uiso 1 1 calc R . .
C23 C -0.0492(8) 0.1595(3) 0.5627(3) 0.0507(16) Uani 1 1 d . . .
H23A H -0.1248 0.1729 0.5329 0.061 Uiso 1 1 calc R . .
H23B H -0.1088 0.1490 0.5977 0.061 Uiso 1 1 calc R . .
C31 C 0.2909(6) 0.3221(3) 0.6729(3) 0.0336(14) Uani 1 1 d . . .
H31A H 0.3339 0.3675 0.6737 0.040 Uiso 1 1 calc R . .
C35 C 0.1384(7) 0.2314(3) 0.6252(3) 0.0368(15) Uani 1 1 d . . .
C32 C 0.3116(7) 0.2758(3) 0.7205(3) 0.0314(14) Uani 1 1 d . . .
C38 C 0.6938(9) 0.2426(4) 1.0078(3) 0.060(2) Uani 1 1 d . . .
H38A H 0.7364 0.2634 1.0426 0.090 Uiso 1 1 calc R . .
H38B H 0.7672 0.2084 0.9927 0.090 Uiso 1 1 calc R . .
H38C H 0.5954 0.2196 1.0166 0.090 Uiso 1 1 calc R . .
C8 C 1.1324(8) 0.3916(4) 0.8814(3) 0.0503(17) Uani 1 1 d . . .
H8A H 1.1592 0.3806 0.9195 0.060 Uiso 1 1 calc R . .
C33 C 0.2390(6) 0.2098(3) 0.7196(3) 0.0320(14) Uani 1 1 d . . .
H33A H 0.2497 0.1803 0.7517 0.038 Uiso 1 1 calc R . .
C15 C 0.8265(7) 0.3617(3) 0.6477(2) 0.0310(13) Uani 1 1 d . . .
H15A H 0.8317 0.3918 0.6157 0.037 Uiso 1 1 calc R . .
C29 C 0.1542(7) 0.3330(3) 0.5710(2) 0.0356(14) Uani 1 1 d . . .
C27 C 0.1000(8) 0.4183(4) 0.4949(3) 0.0517(19) Uani 1 1 d . . .
H27A H 0.1118 0.4633 0.4790 0.062 Uiso 1 1 calc R . .
C7 C 1.1926(7) 0.4526(3) 0.8555(3) 0.0455(17) Uani 1 1 d . . .
H7A H 1.2605 0.4812 0.8770 0.055 Uiso 1 1 calc R . .
C2 C 1.0055(8) 0.6239(3) 0.6542(3) 0.0513(17) Uani 1 1 d . . .
H2A H 0.9473 0.6656 0.6665 0.062 Uiso 1 1 calc R . .
H2B H 1.1161 0.6318 0.6633 0.062 Uiso 1 1 calc R . .
C3 C 0.9467(7) 0.5601(3) 0.6889(3) 0.0429(15) Uani 1 1 d . . .
H3B H 0.9581 0.5698 0.7301 0.051 Uiso 1 1 calc R . .
H3C H 0.8353 0.5527 0.6809 0.051 Uiso 1 1 calc R . .
C25 C -0.0133(8) 0.2980(3) 0.4886(2) 0.0460(16) Uani 1 1 d . . .
H25A H -0.0736 0.2643 0.4691 0.055 Uiso 1 1 calc R . .
C26 C 0.0077(8) 0.3663(4) 0.4663(3) 0.0524(18) Uani 1 1 d . . .
H26A H -0.0409 0.3780 0.4313 0.063 Uiso 1 1 calc R . .
C21 C 0.0928(10) 0.0917(5) 0.4883(4) 0.090(3) Uani 1 1 d . . .
H21A H 0.1832 0.1232 0.4860 0.108 Uiso 1 1 calc R . .
H21B H 0.0139 0.1077 0.4607 0.108 Uiso 1 1 calc R . .
C20 C 0.1484(12) 0.0089(5) 0.4722(4) 0.097(3) Uani 1 1 d . . .
H20A H 0.1922 0.0077 0.4337 0.146 Uiso 1 1 calc R . .
H20B H 0.0582 -0.0220 0.4740 0.146 Uiso 1 1 calc R . .
H20C H 0.2267 -0.0067 0.4996 0.146 Uiso 1 1 calc R . .
C22 C 0.0311(12) 0.0929(4) 0.5435(4) 0.093(3) Uani 1 1 d . . .
H22A H 0.1162 0.0830 0.5706 0.111 Uiso 1 1 calc R . .
H22B H -0.0445 0.0544 0.5467 0.111 Uiso 1 1 calc R . .
C1 C 0.9888(11) 0.6162(4) 0.5906(3) 0.086(3) Uani 1 1 d . . .
H1A H 1.0284 0.6580 0.5717 0.129 Uiso 1 1 calc R . .
H1B H 0.8792 0.6100 0.5809 0.129 Uiso 1 1 calc R . .
H1C H 1.0479 0.5757 0.5777 0.129 Uiso 1 1 calc R . .
C19 C 0.3378(8) -0.0275(3) 0.6400(2) 0.0454(16) Uiso 1 1 d . . .
H19A H 0.2864 -0.0692 0.6251 0.068 Uiso 1 1 calc R . .
H19B H 0.4369 -0.0210 0.6203 0.068 Uiso 1 1 calc R . .
H19C H 0.2716 0.0131 0.6336 0.068 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 N2 1.911(4) . ?
Ni1 N5 1.922(4) . ?
Ni1 S3 2.1580(16) . ?
Ni1 S1 2.1658(15) . ?
S1 C18 1.749(5) . ?
S2 C18 1.744(5) . ?
S2 C19 1.790(6) . ?
S3 C37 1.755(6) . ?
S4 C37 1.762(6) . ?
S4 C38 1.774(7) . ?
N5 C36 1.279(6) . ?
N5 N6 1.425(6) . ?
N2 C17 1.294(6) . ?
N2 N3 1.424(5) . ?
N6 C37 1.277(7) . ?
N3 C18 1.301(6) . ?
C13 C14 1.397(7) . ?
C13 C12 1.405(7) . ?
C13 C17 1.447(7) . ?
C11 C12 1.376(7) . ?
C11 C16 1.422(7) . ?
C11 C10 1.464(7) . ?
C10 C9 1.384(7) . ?
C10 C5 1.420(7) . ?
N4 C24 1.391(7) . ?
N4 C35 1.393(7) . ?
N4 C23 1.460(7) . ?
C34 C35 1.387(8) . ?
C34 C33 1.388(7) . ?
N1 C5 1.370(7) . ?
N1 C16 1.382(6) . ?
N1 C4 1.467(6) . ?
C5 C6 1.404(7) . ?
C36 C32 1.459(8) . ?
C9 C8 1.391(8) . ?
C28 C27 1.393(8) . ?
C28 C29 1.396(8) . ?
C16 C15 1.390(7) . ?
C24 C25 1.394(8) . ?
C24 C29 1.420(8) . ?
C6 C7 1.372(8) . ?
C14 C15 1.376(7) . ?
C4 C3 1.517(7) . ?
C30 C31 1.389(8) . ?
C30 C35 1.398(8) . ?
C30 C29 1.460(8) . ?
C23 C22 1.495(9) . ?
C31 C32 1.411(7) . ?
C32 C33 1.389(7) . ?
C8 C7 1.391(8) . ?
C27 C26 1.415(9) . ?
C2 C1 1.477(9) . ?
C2 C3 1.528(7) . ?
C25 C26 1.398(8) . ?
C21 C22 1.373(10) . ?
C21 C20 1.672(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
N2 Ni1 N5 98.91(18) . . ?
N2 Ni1 S3 165.82(14) . . ?
N5 Ni1 S3 86.58(13) . . ?
N2 Ni1 S1 86.66(13) . . ?
N5 Ni1 S1 164.31(14) . . ?
S3 Ni1 S1 91.48(6) . . ?
C18 S1 Ni1 92.77(17) . . ?
C18 S2 C19 103.3(3) . . ?
C37 S3 Ni1 93.03(19) . . ?
C37 S4 C38 103.8(3) . . ?
C36 N5 N6 113.3(4) . . ?
C36 N5 Ni1 130.4(4) . . ?
N6 N5 Ni1 116.3(3) . . ?
C17 N2 N3 111.2(4) . . ?
C17 N2 Ni1 132.1(4) . . ?
N3 N2 Ni1 116.7(3) . . ?
C37 N6 N5 111.5(4) . . ?
C18 N3 N2 111.3(4) . . ?
N3 C18 S2 121.1(4) . . ?
N3 C18 S1 124.1(4) . . ?
S2 C18 S1 114.7(3) . . ?
C14 C13 C12 118.7(5) . . ?
C14 C13 C17 116.7(5) . . ?
C12 C13 C17 124.5(5) . . ?
C12 C11 C16 119.8(5) . . ?
C12 C11 C10 134.2(5) . . ?
C16 C11 C10 106.0(4) . . ?
C9 C10 C5 119.5(5) . . ?
C9 C10 C11 134.8(5) . . ?
C5 C10 C11 105.8(5) . . ?
C24 N4 C35 108.1(5) . . ?
C24 N4 C23 126.1(5) . . ?
C35 N4 C23 125.3(5) . . ?
C35 C34 C33 117.1(5) . . ?
C5 N1 C16 109.0(4) . . ?
C5 N1 C4 124.9(4) . . ?
C16 N1 C4 126.1(5) . . ?
N1 C5 C6 128.9(5) . . ?
N1 C5 C10 110.0(5) . . ?
C6 C5 C10 121.2(5) . . ?
N5 C36 C32 126.5(5) . . ?
C10 C9 C8 119.4(5) . . ?
C27 C28 C29 120.6(6) . . ?
N1 C16 C15 128.9(5) . . ?
N1 C16 C11 109.3(5) . . ?
C15 C16 C11 121.8(5) . . ?
N4 C24 C25 129.1(6) . . ?
N4 C24 C29 109.1(5) . . ?
C25 C24 C29 121.7(6) . . ?
N6 C37 S3 124.8(4) . . ?
N6 C37 S4 113.9(4) . . ?
S3 C37 S4 121.3(3) . . ?
C7 C6 C5 117.2(5) . . ?
C15 C14 C13 123.7(5) . . ?
N1 C4 C3 112.7(5) . . ?
C31 C30 C35 119.5(5) . . ?
C31 C30 C29 133.8(5) . . ?
C35 C30 C29 106.4(5) . . ?
N2 C17 C13 128.4(5) . . ?
C11 C12 C13 119.4(5) . . ?
N4 C23 C22 117.1(6) . . ?
C30 C31 C32 119.2(5) . . ?
C34 C35 N4 127.4(6) . . ?
C34 C35 C30 122.4(6) . . ?
N4 C35 C30 110.0(5) . . ?
C33 C32 C31 119.3(5) . . ?
C33 C32 C36 123.1(5) . . ?
C31 C32 C36 117.6(5) . . ?
C9 C8 C7 120.1(6) . . ?
C34 C33 C32 122.5(6) . . ?
C14 C15 C16 116.5(5) . . ?
C28 C29 C24 119.3(5) . . ?
C28 C29 C30 134.4(6) . . ?
C24 C29 C30 106.3(5) . . ?
C28 C27 C26 118.6(6) . . ?
C6 C7 C8 122.7(6) . . ?
C1 C2 C3 114.2(6) . . ?
C4 C3 C2 111.4(5) . . ?
C24 C25 C26 117.3(6) . . ?
C25 C26 C27 122.5(6) . . ?
C22 C21 C20 109.1(8) . . ?
C21 C22 C23 117.4(8) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.830
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.078
