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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/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 1055737'
_audit_update_record             
;
2015-03-24 deposited with the CCDC.
2015-06-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H20 Ni5 S10'
_chemical_formula_weight         754.41

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'
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   C2/C

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

_cell_length_a                   10.906(3)
_cell_length_b                   14.095(3)
_cell_length_c                   14.294(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.160(12)
_cell_angle_gamma                90.00
_cell_volume                     2120.9(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1032
_cell_measurement_theta_min      2.8902
_cell_measurement_theta_max      27.4063

_exptl_crystal_description       NEEDLE
_exptl_crystal_colour            BLACK
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.363
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1520
_exptl_absorpt_coefficient_mu    5.337
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6779
_exptl_absorpt_correction_T_max  1.0000
_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  'Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 13.6612
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8227
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_av_sigmaI/netI    0.0549
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.41
_diffrn_reflns_theta_max         27.51
_reflns_number_total             2439
_reflns_number_gt                1855
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_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)+(0.0305P)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_number_reflns         2439
_refine_ls_number_parameters     114
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0413
_refine_ls_wR_factor_ref         0.0792
_refine_ls_wR_factor_gt          0.0713
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.003

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 0.5000 0.07881(5) 0.2500 0.0276(2) Uani 1 2 d S . .
Ni2 Ni 0.34505(5) 0.20426(4) 0.31800(4) 0.02877(16) Uani 1 1 d . . .
Ni3 Ni 0.40348(5) 0.39061(4) 0.29508(4) 0.02937(16) Uani 1 1 d . . .
S1 S 0.70144(10) 0.10188(8) 0.30570(9) 0.0330(3) Uani 1 1 d . . .
S2 S 0.46295(11) 0.08501(8) 0.39132(8) 0.0330(3) Uani 1 1 d . . .
S3 S 0.40867(12) 0.31355(8) 0.43044(8) 0.0355(3) Uani 1 1 d . . .
S4 S 0.21648(11) 0.31908(8) 0.24708(9) 0.0354(3) Uani 1 1 d . . .
S5 S 0.59178(11) 0.45759(9) 0.34377(8) 0.0351(3) Uani 1 1 d . . .
C1 C 0.6991(5) 0.1687(3) 0.4152(3) 0.0407(12) Uani 1 1 d . . .
H1A H 0.7849 0.1736 0.4566 0.049 Uiso 1 1 calc R . .
H1B H 0.6681 0.2324 0.3972 0.049 Uiso 1 1 calc R . .
C2 C 0.6163(4) 0.1217(3) 0.4697(3) 0.0391(11) Uani 1 1 d . . .
H2A H 0.6021 0.1652 0.5184 0.047 Uiso 1 1 calc R . .
H2B H 0.6599 0.0664 0.5030 0.047 Uiso 1 1 calc R . .
C3 C 0.2591(5) 0.3639(4) 0.4415(4) 0.0470(13) Uani 1 1 d . . .
H3A H 0.2372 0.3362 0.4971 0.056 Uiso 1 1 calc R . .
H3B H 0.2691 0.4318 0.4522 0.056 Uiso 1 1 calc R . .
C4 C 0.1528(4) 0.3456(3) 0.3512(4) 0.0452(13) Uani 1 1 d . . .
H4A H 0.0983 0.4010 0.3369 0.054 Uiso 1 1 calc R . .
H4B H 0.1019 0.2925 0.3626 0.054 Uiso 1 1 calc R . .
C5 C 0.5377(4) 0.5765(3) 0.3037(4) 0.0415(12) Uani 1 1 d . . .
H5A H 0.4844 0.6005 0.3431 0.050 Uiso 1 1 calc R . .
H5B H 0.6105 0.6183 0.3123 0.050 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 S1 2.1567(12) . ?
Ni1 S1 2.1567(12) 2_655 ?
Ni1 S2 2.1629(12) . ?
Ni1 S2 2.1629(12) 2_655 ?
Ni1 Ni2 2.7903(8) . ?
Ni1 Ni2 2.7903(8) 2_655 ?
Ni2 S3 2.2034(13) . ?
Ni2 S2 2.2073(12) . ?
Ni2 S4 2.2068(13) . ?
Ni2 S1 2.2354(13) 2_655 ?
Ni2 Ni3 2.7426(9) . ?
Ni3 S5 2.2012(13) . ?
Ni3 S3 2.2066(13) . ?
Ni3 S5 2.2107(13) 2_655 ?
Ni3 S4 2.2169(13) . ?
Ni3 Ni3 2.7409(13) 2_655 ?
S1 C1 1.832(5) . ?
S1 Ni2 2.2354(13) 2_655 ?
S2 C2 1.828(4) . ?
S3 C3 1.823(5) . ?
S4 C4 1.838(5) . ?
S5 C5 1.819(5) . ?
S5 Ni3 2.2107(13) 2_655 ?
C1 C2 1.494(6) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.514(7) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C5 1.541(9) 2_655 ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?

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
S1 Ni1 S1 162.66(7) . 2_655 ?
S1 Ni1 S2 94.02(5) . . ?
S1 Ni1 S2 85.28(5) 2_655 . ?
S1 Ni1 S2 85.28(5) . 2_655 ?
S1 Ni1 S2 94.02(5) 2_655 2_655 ?
S2 Ni1 S2 175.37(7) . 2_655 ?
S1 Ni1 Ni2 115.28(4) . . ?
S1 Ni1 Ni2 51.82(3) 2_655 . ?
S2 Ni1 Ni2 51.03(3) . . ?
S2 Ni1 Ni2 125.30(4) 2_655 . ?
S1 Ni1 Ni2 51.82(3) . 2_655 ?
S1 Ni1 Ni2 115.28(4) 2_655 2_655 ?
S2 Ni1 Ni2 125.30(4) . 2_655 ?
S2 Ni1 Ni2 51.03(3) 2_655 2_655 ?
Ni2 Ni1 Ni2 101.36(4) . 2_655 ?
S3 Ni2 S2 98.79(5) . . ?
S3 Ni2 S4 82.15(5) . . ?
S2 Ni2 S4 176.26(5) . . ?
S3 Ni2 S1 172.47(5) . 2_655 ?
S2 Ni2 S1 82.39(5) . 2_655 ?
S4 Ni2 S1 97.16(5) . 2_655 ?
S3 Ni2 Ni3 51.60(4) . . ?
S2 Ni2 Ni3 131.40(4) . . ?
S4 Ni2 Ni3 51.85(4) . . ?
S1 Ni2 Ni3 122.38(4) 2_655 . ?
S3 Ni2 Ni1 126.39(4) . . ?
S2 Ni2 Ni1 49.62(3) . . ?
S4 Ni2 Ni1 132.43(4) . . ?
S1 Ni2 Ni1 49.32(3) 2_655 . ?
Ni3 Ni2 Ni1 112.61(3) . . ?
S5 Ni3 S3 97.24(5) . . ?
S5 Ni3 S5 82.05(6) . 2_655 ?
S3 Ni3 S5 175.00(5) . 2_655 ?
S5 Ni3 S4 178.35(5) . . ?
S3 Ni3 S4 81.84(5) . . ?
S5 Ni3 S4 98.74(5) 2_655 . ?
S5 Ni3 Ni3 51.75(4) . 2_655 ?
S3 Ni3 Ni3 124.44(4) . 2_655 ?
S5 Ni3 Ni3 51.44(4) 2_655 2_655 ?
S4 Ni3 Ni3 127.73(5) . 2_655 ?
S5 Ni3 Ni2 126.85(4) . . ?
S3 Ni3 Ni2 51.49(3) . . ?
S5 Ni3 Ni2 125.24(4) 2_655 . ?
S4 Ni3 Ni2 51.52(3) . . ?
Ni3 Ni3 Ni2 106.690(17) 2_655 . ?
C1 S1 Ni1 98.78(16) . . ?
C1 S1 Ni2 107.03(16) . 2_655 ?
Ni1 S1 Ni2 78.86(4) . 2_655 ?
C2 S2 Ni1 102.69(16) . . ?
C2 S2 Ni2 113.69(16) . . ?
Ni1 S2 Ni2 79.35(4) . . ?
C3 S3 Ni2 102.55(18) . . ?
C3 S3 Ni3 93.78(17) . . ?
Ni2 S3 Ni3 76.91(5) . . ?
C4 S4 Ni2 96.10(16) . . ?
C4 S4 Ni3 99.70(17) . . ?
Ni2 S4 Ni3 76.63(4) . . ?
C5 S5 Ni3 95.57(15) . . ?
C5 S5 Ni3 101.10(16) . 2_655 ?
Ni3 S5 Ni3 76.81(5) . 2_655 ?
C2 C1 S1 111.3(3) . . ?
C2 C1 H1A 109.4 . . ?
S1 C1 H1A 109.4 . . ?
C2 C1 H1B 109.4 . . ?
S1 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
C1 C2 S2 112.7(3) . . ?
C1 C2 H2A 109.0 . . ?
S2 C2 H2A 109.0 . . ?
C1 C2 H2B 109.0 . . ?
S2 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
C4 C3 S3 111.2(3) . . ?
C4 C3 H3A 109.4 . . ?
S3 C3 H3A 109.4 . . ?
C4 C3 H3B 109.4 . . ?
S3 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
C3 C4 S4 111.0(3) . . ?
C3 C4 H4A 109.4 . . ?
S4 C4 H4A 109.4 . . ?
C3 C4 H4B 109.4 . . ?
S4 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
C5 C5 S5 111.01(17) 2_655 . ?
C5 C5 H5A 109.4 2_655 . ?
S5 C5 H5A 109.4 . . ?
C5 C5 H5B 109.4 2_655 . ?
S5 C5 H5B 109.4 . . ?
H5A C5 H5B 108.0 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.51
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.588
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.124
####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1055738'
_audit_update_record             
;
2015-03-24 deposited with the CCDC.
2015-06-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H132 Ni6 S12'
_chemical_formula_weight         1590.64

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'
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                   10.700(8)
_cell_length_b                   14.844(10)
_cell_length_c                   15.567(10)
_cell_angle_alpha                66.82(6)
_cell_angle_beta                 75.32(6)
_cell_angle_gamma                72.64(6)
_cell_volume                     2143(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      2.0185
_cell_measurement_theta_max      27.4719

_exptl_crystal_description       cuboid
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             852
_exptl_absorpt_coefficient_mu    1.613
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6302
_exptl_absorpt_correction_T_max  1.0000
_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  'Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 13.6612
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13364
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_sigmaI/netI    0.0976
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.76
_diffrn_reflns_theta_max         25.00
_reflns_number_total             7359
_reflns_number_gt                3464
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_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)+(0.0126P)²+6.4200P] 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         7359
_refine_ls_number_parameters     352
_refine_ls_number_restraints     160
_refine_ls_R_factor_all          0.1673
_refine_ls_R_factor_gt           0.0821
_refine_ls_wR_factor_ref         0.1640
_refine_ls_wR_factor_gt          0.1361
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.052
_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 0.99433(12) 1.07250(9) 0.15138(8) 0.0846(4) Uani 1 1 d . . .
Ni2 Ni 0.78280(11) 0.98057(9) 0.14500(8) 0.0842(4) Uani 1 1 d . . .
Ni3 Ni 0.78250(12) 0.90720(9) -0.00421(8) 0.0840(4) Uani 1 1 d . . .
S1 S 0.7863(3) 1.1349(2) 0.1285(2) 0.0994(8) Uani 1 1 d . . .
S2 S 0.9140(3) 0.9420(2) 0.24864(16) 0.0964(8) Uani 1 1 d . . .
S3 S 0.6379(2) 1.0200(2) 0.05093(17) 0.0898(7) Uani 1 1 d . . .
S4 S 0.7981(3) 0.8286(2) 0.14682(17) 0.0963(8) Uani 1 1 d . . .
S5 S 0.7923(2) 0.99744(19) -0.15625(17) 0.0921(8) Uani 1 1 d . . .
S6 S 0.9276(3) 0.79427(19) -0.05945(17) 0.0912(7) Uani 1 1 d . . .
C1 C 0.6910(13) 1.1514(10) 0.2363(9) 0.159(5) Uani 1 1 d . . .
H1A H 0.5981 1.1559 0.2383 0.191 Uiso 1 1 calc R . .
H1B H 0.7218 1.0952 0.2906 0.191 Uiso 1 1 calc R . .
C2 C 0.7110(14) 1.2512(11) 0.2367(12) 0.222(7) Uani 1 1 d DU . .
H2A H 0.7980 1.2391 0.2525 0.267 Uiso 1 1 calc R . .
H2B H 0.7083 1.3010 0.1736 0.267 Uiso 1 1 calc R . .
C3 C 0.6086(16) 1.2925(12) 0.3052(11) 0.318(12) Uani 1 1 d DU . .
H3A H 0.6034 1.2412 0.3685 0.382 Uiso 1 1 calc R . .
C4 C 0.4765(14) 1.3284(15) 0.2711(15) 0.327(12) Uani 1 1 d DU . .
H4A H 0.4536 1.2735 0.2652 0.490 Uiso 1 1 calc R . .
H4B H 0.4819 1.3811 0.2106 0.490 Uiso 1 1 calc R . .
H4C H 0.4098 1.3533 0.3157 0.490 Uiso 1 1 calc R . .
C5 C 0.6449(19) 1.3822(14) 0.3067(15) 0.339(13) Uani 1 1 d DU . .
H5A H 0.7283 1.3614 0.3290 0.508 Uiso 1 1 calc R . .
H5B H 0.5776 1.4115 0.3481 0.508 Uiso 1 1 calc R . .
H5C H 0.6518 1.4309 0.2439 0.508 Uiso 1 1 calc R . .
C6 C 1.0333(10) 0.8211(7) 0.2640(7) 0.116(4) Uani 1 1 d DU . .
H6A H 0.9964 0.7736 0.2550 0.139 Uiso 1 1 calc R . .
H6B H 1.1145 0.8293 0.2195 0.139 Uiso 1 1 calc R . .
C7 C 1.0584(18) 0.7860(9) 0.3640(10) 0.246(9) Uani 1 1 d D . .
H7A H 1.1135 0.8252 0.3680 0.295 Uiso 1 1 calc R . .
H7B H 0.9750 0.7962 0.4055 0.295 Uiso 1 1 calc R . .
C8 C 1.1257(19) 0.6776(10) 0.3951(12) 0.341(13) Uani 1 1 d DU . .
H8A H 1.0888 0.6416 0.3700 0.409 Uiso 1 1 calc R . .
C9 C 1.271(2) 0.668(2) 0.358(2) 0.52(2) Uani 1 1 d DU . .
H9A H 1.2832 0.7125 0.2935 0.777 Uiso 1 1 calc R . .
H9B H 1.3107 0.5997 0.3600 0.777 Uiso 1 1 calc R . .
H9C H 1.3125 0.6844 0.3957 0.777 Uiso 1 1 calc R . .
C10 C 1.104(3) 0.6347(18) 0.5008(13) 0.61(3) Uani 1 1 d DU . .
H10A H 1.0157 0.6234 0.5231 0.917 Uiso 1 1 calc R . .
H10B H 1.1151 0.6810 0.5258 0.917 Uiso 1 1 calc R . .
H10C H 1.1670 0.5721 0.5214 0.917 Uiso 1 1 calc R . .
C11 C 0.6181(9) 1.1468(7) -0.0317(6) 0.100(3) Uani 1 1 d . . .
H11A H 0.6992 1.1694 -0.0443 0.120 Uiso 1 1 calc R . .
H11B H 0.6021 1.1483 -0.0909 0.120 Uiso 1 1 calc R . .
C12 C 0.5041(9) 1.2174(7) 0.0059(7) 0.099(3) Uani 1 1 d . . .
H12A H 0.5177 1.2108 0.0676 0.119 Uiso 1 1 calc R . .
H12B H 0.4231 1.1960 0.0148 0.119 Uiso 1 1 calc R . .
C13 C 0.4844(13) 1.3280(10) -0.0556(10) 0.140(4) Uani 1 1 d U . .
H13A H 0.4654 1.3348 -0.1165 0.168 Uiso 1 1 calc R . .
C14 C 0.3586(13) 1.3872(10) -0.0061(9) 0.177(6) Uani 1 1 d U . .
H14A H 0.2838 1.3595 0.0035 0.265 Uiso 1 1 calc R . .
H14B H 0.3405 1.4568 -0.0454 0.265 Uiso 1 1 calc R . .
H14C H 0.3749 1.3816 0.0539 0.265 Uiso 1 1 calc R . .
C15 C 0.5939(16) 1.3706(12) -0.0736(11) 0.215(7) Uani 1 1 d U . .
H15A H 0.6704 1.3333 -0.1028 0.322 Uiso 1 1 calc R . .
H15B H 0.6113 1.3682 -0.0151 0.322 Uiso 1 1 calc R . .
H15C H 0.5748 1.4392 -0.1151 0.322 Uiso 1 1 calc R . .
C16 C 0.6350(11) 0.7999(9) 0.2028(7) 0.133(4) Uani 1 1 d DU . .
H16A H 0.5686 0.8483 0.1650 0.159 Uiso 1 1 calc R . .
H16B H 0.6358 0.7337 0.2045 0.159 Uiso 1 1 calc R . .
C17 C 0.5974(15) 0.8027(10) 0.3025(9) 0.236(8) Uani 1 1 d DU . .
H17A H 0.6128 0.8635 0.3034 0.283 Uiso 1 1 calc R . .
H17B H 0.5041 0.8026 0.3246 0.283 Uiso 1 1 calc R . .
C18 C 0.6792(15) 0.7128(12) 0.3654(9) 0.246(8) Uani 1 1 d DU . .
H18A H 0.7736 0.7112 0.3419 0.295 Uiso 1 1 calc R . .
C19 C 0.645(3) 0.7173(17) 0.4641(11) 0.49(2) Uani 1 1 d DU . .
H19A H 0.6623 0.7776 0.4630 0.739 Uiso 1 1 calc R . .
H19B H 0.6977 0.6598 0.5052 0.739 Uiso 1 1 calc R . .
H19C H 0.5527 0.7173 0.4871 0.739 Uiso 1 1 calc R . .
C20 C 0.647(2) 0.6192(11) 0.3692(15) 0.376(15) Uani 1 1 d DU . .
H20A H 0.6719 0.6132 0.3076 0.565 Uiso 1 1 calc R . .
H20B H 0.5533 0.6232 0.3890 0.565 Uiso 1 1 calc R . .
H20C H 0.6946 0.5615 0.4134 0.565 Uiso 1 1 calc R . .
C21 C 0.7327(10) 0.9329(8) -0.2104(6) 0.106(3) Uani 1 1 d . . .
H21A H 0.7698 0.8612 -0.1863 0.127 Uiso 1 1 calc R . .
H21B H 0.6369 0.9441 -0.1957 0.127 Uiso 1 1 calc R . .
C22 C 0.7760(14) 0.9750(9) -0.3180(7) 0.153(5) Uani 1 1 d D . .
H22A H 0.7448 1.0475 -0.3401 0.183 Uiso 1 1 calc R . .
H22B H 0.8720 0.9600 -0.3318 0.183 Uiso 1 1 calc R . .
C23 C 0.7231(15) 0.9319(11) -0.3705(10) 0.231(8) Uani 1 1 d DU . .
H23A H 0.6270 0.9386 -0.3529 0.277 Uiso 1 1 calc R . .
C24 C 0.796(3) 0.8226(10) -0.3480(16) 0.435(18) Uani 1 1 d DU . .
H24A H 0.7701 0.7857 -0.2826 0.653 Uiso 1 1 calc R . .
H24B H 0.8901 0.8184 -0.3599 0.653 Uiso 1 1 calc R . .
H24C H 0.7751 0.7946 -0.3871 0.653 Uiso 1 1 calc R . .
C25 C 0.762(3) 0.9845(16) -0.4754(9) 0.414(17) Uani 1 1 d DU . .
H25A H 0.7285 0.9585 -0.5106 0.622 Uiso 1 1 calc R . .
H25B H 0.8567 0.9728 -0.4908 0.622 Uiso 1 1 calc R . .
H25C H 0.7249 1.0554 -0.4913 0.622 Uiso 1 1 calc R . .
C26 C 1.0342(10) 0.7004(7) 0.0257(7) 0.111(3) Uani 1 1 d . . .
H26A H 1.1223 0.6819 -0.0075 0.133 Uiso 1 1 calc R . .
H26B H 1.0416 0.7289 0.0701 0.133 Uiso 1 1 calc R . .
C27 C 0.9766(12) 0.6070(8) 0.0793(8) 0.126(4) Uani 1 1 d . . .
H27A H 0.9613 0.5824 0.0344 0.152 Uiso 1 1 calc R . .
H27B H 0.8921 0.6245 0.1170 0.152 Uiso 1 1 calc R . .
C28 C 1.0734(15) 0.5222(11) 0.1452(11) 0.159(5) Uani 1 1 d U . .
H28A H 1.1608 0.5089 0.1076 0.191 Uiso 1 1 calc R . .
C29 C 1.0176(18) 0.4282(14) 0.1850(13) 0.255(9) Uani 1 1 d U . .
H29A H 1.0771 0.3735 0.2233 0.383 Uiso 1 1 calc R . .
H29B H 1.0079 0.4113 0.1339 0.383 Uiso 1 1 calc R . .
H29C H 0.9327 0.4405 0.2230 0.383 Uiso 1 1 calc R . .
C30 C 1.0859(16) 0.5521(12) 0.2198(12) 0.215(7) Uani 1 1 d U . .
H30A H 1.1478 0.5001 0.2581 0.323 Uiso 1 1 calc R . .
H30B H 1.0011 0.5629 0.2583 0.323 Uiso 1 1 calc R . .
H30C H 1.1173 0.6132 0.1927 0.323 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 S6 2.193(3) 2_775 ?
Ni1 S2 2.193(3) . ?
Ni1 S1 2.202(3) . ?
Ni1 S5 2.215(3) 2_775 ?
Ni1 Ni3 2.856(3) 2_775 ?
Ni2 S3 2.197(3) . ?
Ni2 S2 2.201(3) . ?
Ni2 S4 2.201(3) . ?
Ni2 S1 2.214(3) . ?
Ni2 Ni3 2.929(2) . ?
Ni3 S4 2.200(3) . ?
Ni3 S3 2.201(3) . ?
Ni3 S6 2.206(3) . ?
Ni3 S5 2.207(3) . ?
Ni3 Ni1 2.856(3) 2_775 ?
S1 C1 1.794(12) . ?
S2 C6 1.833(10) . ?
S3 C11 1.799(9) . ?
S4 C16 1.835(10) . ?
S5 C21 1.818(9) . ?
S5 Ni1 2.215(3) 2_775 ?
S6 C26 1.834(10) . ?
S6 Ni1 2.193(3) 2_775 ?
C1 C2 1.562(16) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.495(10) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C5 1.504(10) . ?
C3 C4 1.508(10) . ?
C3 H3A 0.9800 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C7 1.503(9) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.488(9) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C10 1.495(10) . ?
C8 C9 1.501(10) . ?
C8 H8A 0.9800 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.513(11) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.521(13) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C15 1.410(16) . ?
C13 C14 1.575(15) . ?
C13 H13A 0.9800 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.516(9) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.488(9) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C20 1.506(9) . ?
C18 C19 1.510(9) . ?
C18 H18A 0.9800 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.538(12) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.504(9) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C25 1.515(9) . ?
C23 C24 1.517(9) . ?
C23 H23A 0.9800 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 C27 1.530(12) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.567(15) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C30 1.443(17) . ?
C28 C29 1.522(18) . ?
C28 H28A 0.9800 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 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
S6 Ni1 S2 177.37(11) 2_775 . ?
S6 Ni1 S1 97.93(13) 2_775 . ?
S2 Ni1 S1 81.97(13) . . ?
S6 Ni1 S5 82.13(13) 2_775 2_775 ?
S2 Ni1 S5 98.36(13) . 2_775 ?
S1 Ni1 S5 171.53(11) . 2_775 ?
S6 Ni1 Ni3 49.71(9) 2_775 2_775 ?
S2 Ni1 Ni3 132.38(10) . 2_775 ?
S1 Ni1 Ni3 124.49(11) . 2_775 ?
S5 Ni1 Ni3 49.65(9) 2_775 2_775 ?
S3 Ni2 S2 175.25(11) . . ?
S3 Ni2 S4 81.80(12) . . ?
S2 Ni2 S4 99.10(12) . . ?
S3 Ni2 S1 98.14(12) . . ?
S2 Ni2 S1 81.53(12) . . ?
S4 Ni2 S1 173.20(11) . . ?
S3 Ni2 Ni3 48.31(8) . . ?
S2 Ni2 Ni3 135.28(10) . . ?
S4 Ni2 Ni3 48.27(8) . . ?
S1 Ni2 Ni3 127.21(10) . . ?
S4 Ni3 S3 81.72(12) . . ?
S4 Ni3 S6 98.27(13) . . ?
S3 Ni3 S6 179.92(12) . . ?
S4 Ni3 S5 170.68(12) . . ?
S3 Ni3 S5 97.96(13) . . ?
S6 Ni3 S5 82.03(12) . . ?
S4 Ni3 Ni1 123.83(11) . 2_775 ?
S3 Ni3 Ni1 130.61(10) . 2_775 ?
S6 Ni3 Ni1 49.33(9) . 2_775 ?
S5 Ni3 Ni1 49.91(9) . 2_775 ?
S4 Ni3 Ni2 48.30(9) . . ?
S3 Ni3 Ni2 48.17(9) . . ?
S6 Ni3 Ni2 131.77(10) . . ?
S5 Ni3 Ni2 125.28(10) . . ?
Ni1 Ni3 Ni2 114.83(7) 2_775 . ?
C1 S1 Ni1 107.4(5) . . ?
C1 S1 Ni2 104.1(4) . . ?
Ni1 S1 Ni2 85.93(12) . . ?
C6 S2 Ni1 114.3(4) . . ?
C6 S2 Ni2 114.1(4) . . ?
Ni1 S2 Ni2 86.47(12) . . ?
C11 S3 Ni2 114.0(3) . . ?
C11 S3 Ni3 114.6(3) . . ?
Ni2 S3 Ni3 83.51(11) . . ?
C16 S4 Ni3 104.9(4) . . ?
C16 S4 Ni2 105.8(4) . . ?
Ni3 S4 Ni2 83.43(12) . . ?
C21 S5 Ni3 106.9(3) . . ?
C21 S5 Ni1 106.8(4) . 2_775 ?
Ni3 S5 Ni1 80.45(12) . 2_775 ?
C26 S6 Ni1 114.8(4) . 2_775 ?
C26 S6 Ni3 113.6(3) . . ?
Ni1 S6 Ni3 80.96(12) 2_775 . ?
C2 C1 S1 106.3(10) . . ?
C2 C1 H1A 110.5 . . ?
S1 C1 H1A 110.5 . . ?
C2 C1 H1B 110.5 . . ?
S1 C1 H1B 110.5 . . ?
H1A C1 H1B 108.7 . . ?
C3 C2 C1 113.0(12) . . ?
C3 C2 H2A 109.0 . . ?
C1 C2 H2A 109.0 . . ?
C3 C2 H2B 109.0 . . ?
C1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
C2 C3 C5 108.5(9) . . ?
C2 C3 C4 109.1(9) . . ?
C5 C3 C4 107.6(9) . . ?
C2 C3 H3A 110.5 . . ?
C5 C3 H3A 110.5 . . ?
C4 C3 H3A 110.5 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 S2 104.3(7) . . ?
C7 C6 H6A 110.9 . . ?
S2 C6 H6A 110.9 . . ?
C7 C6 H6B 110.9 . . ?
S2 C6 H6B 110.9 . . ?
H6A C6 H6B 108.9 . . ?
C8 C7 C6 110.3(8) . . ?
C8 C7 H7A 109.6 . . ?
C6 C7 H7A 109.6 . . ?
C8 C7 H7B 109.6 . . ?
C6 C7 H7B 109.6 . . ?
H7A C7 H7B 108.1 . . ?
C7 C8 C10 109.3(10) . . ?
C7 C8 C9 108.8(10) . . ?
C10 C8 C9 110.3(10) . . ?
C7 C8 H8A 109.5 . . ?
C10 C8 H8A 109.5 . . ?
C9 C8 H8A 109.5 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 S3 111.5(7) . . ?
C12 C11 H11A 109.3 . . ?
S3 C11 H11A 109.3 . . ?
C12 C11 H11B 109.3 . . ?
S3 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
C11 C12 C13 115.8(9) . . ?
C11 C12 H12A 108.3 . . ?
C13 C12 H12A 108.3 . . ?
C11 C12 H12B 108.3 . . ?
C13 C12 H12B 108.3 . . ?
H12A C12 H12B 107.4 . . ?
C15 C13 C12 114.9(12) . . ?
C15 C13 C14 110.1(12) . . ?
C12 C13 C14 107.7(10) . . ?
C15 C13 H13A 108.0 . . ?
C12 C13 H13A 108.0 . . ?
C14 C13 H13A 108.0 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 S4 112.0(9) . . ?
C17 C16 H16A 109.2 . . ?
S4 C16 H16A 109.2 . . ?
C17 C16 H16B 109.2 . . ?
S4 C16 H16B 109.2 . . ?
H16A C16 H16B 107.9 . . ?
C18 C17 C16 108.9(8) . . ?
C18 C17 H17A 109.9 . . ?
C16 C17 H17A 109.9 . . ?
C18 C17 H17B 109.9 . . ?
C16 C17 H17B 109.9 . . ?
H17A C17 H17B 108.3 . . ?
C17 C18 C20 109.4(9) . . ?
C17 C18 C19 108.9(9) . . ?
C20 C18 C19 108.1(9) . . ?
C17 C18 H18A 110.1 . . ?
C20 C18 H18A 110.1 . . ?
C19 C18 H18A 110.1 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 S5 108.0(7) . . ?
C22 C21 H21A 110.1 . . ?
S5 C21 H21A 110.1 . . ?
C22 C21 H21B 110.1 . . ?
S5 C21 H21B 110.1 . . ?
H21A C21 H21B 108.4 . . ?
C23 C22 C21 112.3(10) . . ?
C23 C22 H22A 109.1 . . ?
C21 C22 H22A 109.1 . . ?
C23 C22 H22B 109.1 . . ?
C21 C22 H22B 109.1 . . ?
H22A C22 H22B 107.9 . . ?
C22 C23 C25 107.9(9) . . ?
C22 C23 C24 106.6(9) . . ?
C25 C23 C24 107.0(9) . . ?
C22 C23 H23A 111.7 . . ?
C25 C23 H23A 111.7 . . ?
C24 C23 H23A 111.7 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 S6 110.3(8) . . ?
C27 C26 H26A 109.6 . . ?
S6 C26 H26A 109.6 . . ?
C27 C26 H26B 109.6 . . ?
S6 C26 H26B 109.6 . . ?
H26A C26 H26B 108.1 . . ?
C26 C27 C28 110.8(10) . . ?
C26 C27 H27A 109.5 . . ?
C28 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C28 C27 H27B 109.5 . . ?
H27A C27 H27B 108.1 . . ?
C30 C28 C29 111.3(14) . . ?
C30 C28 C27 110.8(13) . . ?
C29 C28 C27 107.1(13) . . ?
C30 C28 H28A 109.2 . . ?
C29 C28 H28A 109.2 . . ?
C27 C28 H28A 109.2 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.074
####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1055739'
_audit_update_record             
;
2015-03-24 deposited with the CCDC.
2015-06-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H60 Ni6 S12'
_chemical_formula_weight         1133.74

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'
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   C222(1)

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

_cell_length_a                   15.028(17)
_cell_length_b                   23.16(2)
_cell_length_c                   13.417(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4670(9)
_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       needle
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2352
_exptl_absorpt_coefficient_mu    2.926
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.5712
_exptl_absorpt_correction_T_max  1.0000
_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  'Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 13.6612
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17500
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_sigmaI/netI    0.0500
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.22
_diffrn_reflns_theta_max         27.27
_reflns_number_total             5240
_reflns_number_gt                3625
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_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)+(0.1108P)²+4.6779P] 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   0.47(4)
_refine_ls_number_reflns         5240
_refine_ls_number_parameters     209
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.1030
_refine_ls_R_factor_gt           0.0754
_refine_ls_wR_factor_ref         0.2100
_refine_ls_wR_factor_gt          0.1878
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.073
_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
S1 S -0.00763(16) 0.19191(10) -0.08513(18) 0.0687(6) Uani 1 1 d . . .
S2 S 0.14519(16) 0.17686(10) -0.2165(2) 0.0729(7) Uani 1 1 d . . .
S3 S 0.09305(19) 0.30563(14) 0.02198(18) 0.0831(7) Uani 1 1 d . . .
S4 S 0.23229(16) 0.29962(12) -0.1176(2) 0.0775(6) Uani 1 1 d . . .
S5 S 0.0140(2) 0.42681(11) -0.0860(2) 0.0871(8) Uani 1 1 d . . .
S6 S 0.14710(18) 0.41318(10) -0.2440(2) 0.0767(7) Uani 1 1 d . . .
Ni1 Ni 0.0000 0.18053(6) -0.2500 0.0639(4) Uani 1 2 d S . .
Ni2 Ni 0.11797(8) 0.24080(5) -0.09916(9) 0.0653(3) Uani 1 1 d . A .
Ni3 Ni 0.12223(9) 0.36407(5) -0.10419(9) 0.0715(4) Uani 1 1 d . A .
Ni4 Ni 0.0000 0.42324(6) -0.2500 0.0702(5) Uani 1 2 d S . .
C1 C 0.0091(9) 0.1218(5) -0.0142(10) 0.098(4) Uani 1 1 d . . .
C2 C -0.0016(16) 0.1432(9) 0.1012(12) 0.162(7) Uani 1 1 d . . .
H2A H 0.0059 0.1109 0.1451 0.243 Uiso 1 1 calc R . .
H2B H -0.0597 0.1595 0.1106 0.243 Uiso 1 1 calc R . .
H2C H 0.0428 0.1718 0.1157 0.243 Uiso 1 1 calc R . .
C3 C -0.0692(13) 0.0867(8) -0.0338(16) 0.158(7) Uani 1 1 d U . .
H3A H -0.0639 0.0505 0.0008 0.237 Uiso 1 1 calc R . .
H3B H -0.0740 0.0796 -0.1041 0.237 Uiso 1 1 calc R . .
H3C H -0.1213 0.1066 -0.0110 0.237 Uiso 1 1 calc R . .
C4 C 0.1010(12) 0.0964(9) -0.0194(16) 0.153(6) Uani 1 1 d U . .
H4A H 0.1033 0.0618 0.0200 0.230 Uiso 1 1 calc R . .
H4B H 0.1433 0.1238 0.0058 0.230 Uiso 1 1 calc R . .
H4C H 0.1151 0.0873 -0.0874 0.230 Uiso 1 1 calc R . .
C5 C 0.2167(7) 0.2043(5) -0.3166(9) 0.086(3) Uani 1 1 d . A .
H5A H 0.2761 0.1890 -0.3066 0.103 Uiso 1 1 calc R . .
H5B H 0.1949 0.1890 -0.3793 0.103 Uiso 1 1 calc R . .
C6 C 0.2237(7) 0.2686(5) -0.3262(9) 0.088(3) Uani 1 1 d . . .
H6A H 0.1645 0.2852 -0.3240 0.105 Uiso 1 1 calc R A .
H6B H 0.2498 0.2780 -0.3902 0.105 Uiso 1 1 calc R . .
C7 C 0.2811(7) 0.2956(4) -0.2420(9) 0.087(3) Uani 1 1 d . A .
H7A H 0.2971 0.3345 -0.2623 0.104 Uiso 1 1 calc R . .
H7B H 0.3359 0.2736 -0.2373 0.104 Uiso 1 1 calc R . .
C8 C -0.0209(10) 0.3091(7) 0.0679(10) 0.116(4) Uani 0.50 1 d P A 1
H8A H -0.0421 0.2701 0.0793 0.140 Uiso 0.50 1 calc PR A 1
H8B H -0.0210 0.3290 0.1315 0.140 Uiso 0.50 1 calc PR A 1
C9 C -0.0883(17) 0.341(2) -0.006(3) 0.159(18) Uani 0.50 1 d P A 1
H9A H -0.0807 0.3242 -0.0711 0.191 Uiso 0.50 1 calc PR A 1
H9B H -0.1481 0.3317 0.0162 0.191 Uiso 0.50 1 calc PR A 1
C10 C -0.0841(11) 0.3994(8) -0.0163(11) 0.121(5) Uani 0.50 1 d P A 1
H10A H -0.0840 0.4167 0.0495 0.145 Uiso 0.50 1 calc PR A 1
H10B H -0.1375 0.4122 -0.0502 0.145 Uiso 0.50 1 calc PR A 1
C8A C -0.0209(10) 0.3091(7) 0.0679(10) 0.116(4) Uani 0.50 1 d P A 2
H8AA H -0.0574 0.2870 0.0221 0.140 Uiso 0.50 1 calc PR A 2
H8AB H -0.0222 0.2889 0.1312 0.140 Uiso 0.50 1 calc PR A 2
C9A C -0.0632(16) 0.3621(10) 0.0824(17) 0.082(5) Uiso 0.50 1 d P A 2
H9C H -0.0264 0.3853 0.1262 0.098 Uiso 0.50 1 calc PR A 2
H9D H -0.1190 0.3551 0.1167 0.098 Uiso 0.50 1 calc PR A 2
C10A C -0.0841(11) 0.3994(8) -0.0163(11) 0.121(5) Uani 0.50 1 d P A 2
H10C H -0.1205 0.4321 0.0028 0.145 Uiso 0.50 1 calc PR A 2
H10D H -0.1192 0.3757 -0.0611 0.145 Uiso 0.50 1 calc PR A 2
C11 C 0.2051(8) 0.4845(5) -0.2296(10) 0.097(3) Uani 1 1 d DU A .
C12 C 0.1511(13) 0.5296(8) -0.1739(17) 0.201(10) Uani 1 1 d DU . .
H12A H 0.1853 0.5645 -0.1679 0.301 Uiso 1 1 calc R A .
H12B H 0.1365 0.5154 -0.1087 0.301 Uiso 1 1 calc R . .
H12C H 0.0973 0.5375 -0.2100 0.301 Uiso 1 1 calc R . .
C13 C 0.2166(14) 0.5094(9) -0.3351(11) 0.162(7) Uani 1 1 d DU . .
H13A H 0.2462 0.5460 -0.3312 0.243 Uiso 1 1 calc R A .
H13B H 0.1592 0.5144 -0.3654 0.243 Uiso 1 1 calc R . .
H13C H 0.2515 0.4833 -0.3747 0.243 Uiso 1 1 calc R . .
C14 C 0.3023(11) 0.4725(11) -0.208(2) 0.217(11) Uiso 1 1 d D . .
H14A H 0.3331 0.5083 -0.1982 0.326 Uiso 1 1 calc R A .
H14B H 0.3282 0.4521 -0.2630 0.326 Uiso 1 1 calc R . .
H14C H 0.3071 0.4494 -0.1487 0.326 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
S1 C1 1.899(11) . ?
S1 Ni2 2.209(3) . ?
S1 Ni1 2.231(3) . ?
S2 C5 1.834(10) . ?
S2 Ni2 2.199(3) . ?
S2 Ni1 2.229(3) . ?
S3 C8 1.821(14) . ?
S3 Ni3 2.211(3) . ?
S3 Ni2 2.244(4) . ?
S4 C7 1.826(12) . ?
S4 Ni2 2.206(3) . ?
S4 Ni3 2.235(4) . ?
S5 C10 1.858(18) . ?
S5 Ni3 2.195(4) . ?
S5 Ni4 2.212(4) . ?
S6 C11 1.877(11) . ?
S6 Ni4 2.224(4) . ?
S6 Ni3 2.225(3) . ?
Ni1 S2 2.229(3) 3_554 ?
Ni1 S1 2.231(3) 3_554 ?
Ni2 Ni3 2.857(3) . ?
Ni4 S5 2.212(4) 3_554 ?
Ni4 S6 2.224(4) 3_554 ?
C1 C3 1.45(2) . ?
C1 C4 1.50(2) . ?
C1 C2 1.63(2) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 C6 1.499(17) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C7 1.553(17) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.60(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.36(6) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C9A H9C 0.9700 . ?
C9A H9D 0.9700 . ?
C11 C14 1.514(10) . ?
C11 C12 1.521(10) . ?
C11 C13 1.539(9) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 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
C1 S1 Ni2 111.6(4) . . ?
C1 S1 Ni1 112.9(4) . . ?
Ni2 S1 Ni1 86.11(9) . . ?
C5 S2 Ni2 113.6(4) . . ?
C5 S2 Ni1 114.4(4) . . ?
Ni2 S2 Ni1 86.38(10) . . ?
C8 S3 Ni3 114.7(5) . . ?
C8 S3 Ni2 115.6(5) . . ?
Ni3 S3 Ni2 79.75(12) . . ?
C7 S4 Ni2 112.6(3) . . ?
C7 S4 Ni3 113.9(4) . . ?
Ni2 S4 Ni3 80.05(13) . . ?
C10 S5 Ni3 114.7(5) . . ?
C10 S5 Ni4 114.4(5) . . ?
Ni3 S5 Ni4 86.29(11) . . ?
C11 S6 Ni4 111.9(4) . . ?
C11 S6 Ni3 116.2(4) . . ?
Ni4 S6 Ni3 85.26(11) . . ?
S2 Ni1 S2 175.64(14) . 3_554 ?
S2 Ni1 S1 81.64(10) . . ?
S2 Ni1 S1 98.88(10) 3_554 . ?
S2 Ni1 S1 98.88(10) . 3_554 ?
S2 Ni1 S1 81.64(10) 3_554 3_554 ?
S1 Ni1 S1 166.43(14) . 3_554 ?
S2 Ni2 S4 101.00(12) . . ?
S2 Ni2 S1 82.80(11) . . ?
S4 Ni2 S1 172.43(11) . . ?
S2 Ni2 S3 178.78(12) . . ?
S4 Ni2 S3 78.35(12) . . ?
S1 Ni2 S3 97.97(12) . . ?
S2 Ni2 Ni3 130.69(10) . . ?
S4 Ni2 Ni3 50.42(9) . . ?
S1 Ni2 Ni3 122.24(9) . . ?
S3 Ni2 Ni3 49.62(9) . . ?
S5 Ni3 S3 99.98(14) . . ?
S5 Ni3 S6 83.08(12) . . ?
S3 Ni3 S6 172.50(12) . . ?
S5 Ni3 S4 178.22(12) . . ?
S3 Ni3 S4 78.44(12) . . ?
S6 Ni3 S4 98.59(12) . . ?
S5 Ni3 Ni2 129.99(11) . . ?
S3 Ni3 Ni2 50.63(9) . . ?
S6 Ni3 Ni2 122.32(9) . . ?
S4 Ni3 Ni2 49.53(9) . . ?
S5 Ni4 S5 175.71(16) . 3_554 ?
S5 Ni4 S6 97.75(12) . 3_554 ?
S5 Ni4 S6 82.70(11) 3_554 3_554 ?
S5 Ni4 S6 82.70(11) . . ?
S5 Ni4 S6 97.75(12) 3_554 . ?
S6 Ni4 S6 167.97(14) 3_554 . ?
C3 C1 C4 121.0(14) . . ?
C3 C1 C2 105.2(14) . . ?
C4 C1 C2 104.7(15) . . ?
C3 C1 S1 106.3(11) . . ?
C4 C1 S1 115.7(10) . . ?
C2 C1 S1 101.7(9) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 S2 116.6(8) . . ?
C6 C5 H5A 108.1 . . ?
S2 C5 H5A 108.1 . . ?
C6 C5 H5B 108.1 . . ?
S2 C5 H5B 108.1 . . ?
H5A C5 H5B 107.3 . . ?
C5 C6 C7 112.1(10) . . ?
C5 C6 H6A 109.2 . . ?
C7 C6 H6A 109.2 . . ?
C5 C6 H6B 109.2 . . ?
C7 C6 H6B 109.2 . . ?
H6A C6 H6B 107.9 . . ?
C6 C7 S4 117.5(7) . . ?
C6 C7 H7A 107.9 . . ?
S4 C7 H7A 107.9 . . ?
C6 C7 H7B 107.9 . . ?
S4 C7 H7B 107.9 . . ?
H7A C7 H7B 107.2 . . ?
C9 C8 S3 114.1(14) . . ?
C9 C8 H8A 108.7 . . ?
S3 C8 H8A 108.7 . . ?
C9 C8 H8B 108.7 . . ?
S3 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
C10 C9 C8 120(3) . . ?
C10 C9 H9A 107.4 . . ?
C8 C9 H9A 107.4 . . ?
C10 C9 H9B 107.4 . . ?
C8 C9 H9B 107.4 . . ?
H9A C9 H9B 106.9 . . ?
C9 C10 S5 115.5(15) . . ?
C9 C10 H10A 108.4 . . ?
S5 C10 H10A 108.4 . . ?
C9 C10 H10B 108.4 . . ?
S5 C10 H10B 108.4 . . ?
H10A C10 H10B 107.5 . . ?
H9C C9A H9D 107.3 . . ?
C14 C11 C12 123.1(16) . . ?
C14 C11 C13 97.9(15) . . ?
C12 C11 C13 104.7(15) . . ?
C14 C11 S6 107.8(12) . . ?
C12 C11 S6 114.0(11) . . ?
C13 C11 S6 106.7(10) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.27
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.881
_refine_diff_density_min         -0.941
_refine_diff_density_rms         0.283
####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1055740'
_audit_update_record             
;
2015-03-24 deposited with the CCDC.
2015-06-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H36 Ni6 S12'
_chemical_formula_weight         1157.59

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'
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   P2/n

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

_cell_length_a                   11.621(2)
_cell_length_b                   12.8025(18)
_cell_length_c                   14.234(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.641(10)
_cell_angle_gamma                90.00
_cell_volume                     2058.0(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      2.4050
_cell_measurement_theta_max      27.4410

_exptl_crystal_description       cuboid
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.868
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1176
_exptl_absorpt_coefficient_mu    3.323
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6777
_exptl_absorpt_correction_T_max  1.0000
_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  'Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 13.6612
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15849
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.04
_diffrn_reflns_theta_max         27.51
_reflns_number_total             4724
_reflns_number_gt                3422
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_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)+(0.0759P)²+0.9669P] 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         4724
_refine_ls_number_parameters     227
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0547
_refine_ls_wR_factor_ref         0.1659
_refine_ls_wR_factor_gt          0.1374
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_restrained_S_all      1.144
_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 0.7500 -0.45823(8) 0.2500 0.0380(2) Uani 1 2 d S . .
Ni2 Ni 0.94131(6) -0.54707(6) 0.16413(5) 0.0421(2) Uani 1 1 d . . .
Ni3 Ni 0.7500 -0.84358(8) 0.2500 0.0433(3) Uani 1 2 d S . .
Ni4 Ni 0.91869(6) -0.75526(6) 0.14146(5) 0.0441(2) Uani 1 1 d . . .
S5 S 0.78712(13) -0.45112(11) 0.10535(10) 0.0437(3) Uani 1 1 d . . .
S6 S 0.91361(14) -0.63526(13) 0.02902(11) 0.0508(4) Uani 1 1 d . . .
S7 S 0.55772(14) -0.85564(14) 0.23396(12) 0.0576(4) Uani 1 1 d . . .
S8 S 0.55398(13) -0.46849(12) 0.19742(11) 0.0449(3) Uani 1 1 d . . .
S9 S 0.74576(13) -0.83354(12) 0.09266(11) 0.0476(4) Uani 1 1 d . . .
S10 S 1.07895(14) -0.66655(14) 0.20693(15) 0.0625(5) Uani 1 1 d . . .
C6 C 0.7828(5) -0.9623(5) 0.0605(4) 0.0469(14) Uani 1 1 d . . .
C5 C 0.5053(5) -0.3387(5) 0.2088(4) 0.0486(14) Uani 1 1 d . . .
C10 C 0.6974(5) -0.5487(5) 0.0274(4) 0.0528(15) Uani 1 1 d . . .
H10A H 0.6733 -0.6026 0.0667 0.063 Uiso 1 1 calc R . .
H10B H 0.6267 -0.5161 -0.0113 0.063 Uiso 1 1 calc R . .
C9 C 0.7672(6) -0.5966(6) -0.0373(4) 0.0586(16) Uani 1 1 d . . .
H9A H 0.7742 -0.5467 -0.0870 0.070 Uiso 1 1 calc R . .
H9B H 0.7254 -0.6573 -0.0690 0.070 Uiso 1 1 calc R . .
C4 C 0.7585(8) -1.0497(5) 0.1105(6) 0.072(2) Uani 1 1 d . . .
H4A H 0.7207 -1.0428 0.1610 0.087 Uiso 1 1 calc R . .
C15 C 0.8382(6) -1.1610(6) 0.0072(6) 0.074(2) Uani 1 1 d . . .
H15A H 0.8557 -1.2279 -0.0108 0.088 Uiso 1 1 calc R . .
C3 C 0.5223(7) -0.2631(6) 0.1434(6) 0.071(2) Uani 1 1 d . . .
H3A H 0.5624 -0.2797 0.0960 0.085 Uiso 1 1 calc R . .
C14 C 0.7916(8) -1.1474(6) 0.0839(7) 0.083(2) Uani 1 1 d . . .
H14A H 0.7811 -1.2053 0.1204 0.099 Uiso 1 1 calc R . .
C2 C 0.4478(7) -0.3123(6) 0.2786(5) 0.0665(19) Uani 1 1 d . . .
H2A H 0.4363 -0.3617 0.3234 0.080 Uiso 1 1 calc R . .
C1 C 0.8296(8) -0.9773(7) -0.0165(6) 0.088(3) Uani 1 1 d . . .
H1A H 0.8423 -0.9197 -0.0526 0.105 Uiso 1 1 calc R . .
C13 C 0.8597(9) -1.0767(8) -0.0440(6) 0.094(3) Uani 1 1 d . . .
H13A H 0.8939 -1.0849 -0.0964 0.113 Uiso 1 1 calc R . .
C20 C 1.1120(8) -0.7041(7) 0.3307(6) 0.088(3) Uani 1 1 d . . .
H20A H 1.1828 -0.7469 0.3437 0.105 Uiso 1 1 calc R . .
H20B H 1.1296 -0.6417 0.3701 0.105 Uiso 1 1 calc R . .
C8 C 0.4784(8) -0.7594(10) 0.1408(5) 0.115(4) Uani 1 1 d . . .
H8A H 0.5356 -0.7099 0.1272 0.138 Uiso 1 1 calc R . .
H8B H 0.4445 -0.7966 0.0814 0.138 Uiso 1 1 calc R . .
C12 C 0.4227(9) -0.1368(7) 0.2181(8) 0.090(3) Uani 1 1 d . . .
H12A H 0.3952 -0.0690 0.2214 0.108 Uiso 1 1 calc R . .
C11 C 0.4793(8) -0.1623(6) 0.1490(8) 0.086(3) Uani 1 1 d . . .
H11A H 0.4898 -0.1121 0.1045 0.103 Uiso 1 1 calc R . .
C16 C 0.4057(8) -0.2085(8) 0.2822(7) 0.091(3) Uani 1 1 d . . .
H16A H 0.3661 -0.1902 0.3294 0.109 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 S5 2.2028(14) 2_655 ?
Ni1 S5 2.2028(14) . ?
Ni1 S8 2.2277(15) . ?
Ni1 S8 2.2277(15) 2_655 ?
Ni2 S5 2.1709(16) . ?
Ni2 S6 2.1873(17) . ?
Ni2 S10 2.1931(18) . ?
Ni2 S8 2.2018(17) 2_655 ?
Ni2 Ni4 2.6903(11) . ?
Ni3 S7 2.1974(16) . ?
Ni3 S7 2.1974(16) 2_655 ?
Ni3 S9 2.2322(16) 2_655 ?
Ni3 S9 2.2322(16) . ?
Ni3 Ni4 2.9895(9) 2_655 ?
Ni3 Ni4 2.9895(9) . ?
Ni4 S7 2.1545(19) 2_655 ?
Ni4 S10 2.1928(18) . ?
Ni4 S9 2.2061(17) . ?
Ni4 S6 2.2091(18) . ?
S5 C10 1.826(6) . ?
S6 C9 1.809(7) . ?
S7 C8 1.884(10) . ?
S7 Ni4 2.1545(19) 2_655 ?
S8 C5 1.776(6) . ?
S8 Ni2 2.2018(17) 2_655 ?
S9 C6 1.791(6) . ?
S10 C20 1.778(8) . ?
C6 C1 1.347(9) . ?
C6 C4 1.391(9) . ?
C5 C2 1.364(9) . ?
C5 C3 1.389(9) . ?
C10 C9 1.495(8) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C4 C14 1.388(10) . ?
C4 H4A 0.9300 . ?
C15 C14 1.338(12) . ?
C15 C13 1.358(12) . ?
C15 H15A 0.9300 . ?
C3 C11 1.392(10) . ?
C3 H3A 0.9300 . ?
C14 H14A 0.9300 . ?
C2 C16 1.420(11) . ?
C2 H2A 0.9300 . ?
C1 C13 1.400(11) . ?
C1 H1A 0.9300 . ?
C13 H13A 0.9300 . ?
C20 C8 1.403(12) 2_655 ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C8 C20 1.403(12) 2_655 ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C12 C11 1.347(14) . ?
C12 C16 1.341(13) . ?
C12 H12A 0.9300 . ?
C11 H11A 0.9300 . ?
C16 H16A 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
S5 Ni1 S5 175.26(9) 2_655 . ?
S5 Ni1 S8 84.62(5) 2_655 . ?
S5 Ni1 S8 95.66(5) . . ?
S5 Ni1 S8 95.66(5) 2_655 2_655 ?
S5 Ni1 S8 84.62(5) . 2_655 ?
S8 Ni1 S8 173.24(9) . 2_655 ?
S5 Ni2 S6 90.93(6) . . ?
S5 Ni2 S10 169.53(7) . . ?
S6 Ni2 S10 80.25(7) . . ?
S5 Ni2 S8 86.01(6) . 2_655 ?
S6 Ni2 S8 171.96(7) . 2_655 ?
S10 Ni2 S8 101.98(7) . 2_655 ?
S5 Ni2 Ni4 117.77(5) . . ?
S6 Ni2 Ni4 52.64(5) . . ?
S10 Ni2 Ni4 52.16(5) . . ?
S8 Ni2 Ni4 122.76(5) 2_655 . ?
S7 Ni3 S7 171.94(11) . 2_655 ?
S7 Ni3 S9 83.66(6) . 2_655 ?
S7 Ni3 S9 96.81(6) 2_655 2_655 ?
S7 Ni3 S9 96.81(6) . . ?
S7 Ni3 S9 83.66(6) 2_655 . ?
S9 Ni3 S9 173.40(9) 2_655 . ?
S7 Ni3 Ni4 46.02(5) . 2_655 ?
S7 Ni3 Ni4 138.38(5) 2_655 2_655 ?
S9 Ni3 Ni4 47.29(4) 2_655 2_655 ?
S9 Ni3 Ni4 129.40(5) . 2_655 ?
S7 Ni3 Ni4 138.38(5) . . ?
S7 Ni3 Ni4 46.02(5) 2_655 . ?
S9 Ni3 Ni4 129.40(5) 2_655 . ?
S9 Ni3 Ni4 47.29(4) . . ?
Ni4 Ni3 Ni4 135.55(5) 2_655 . ?
S7 Ni4 S10 91.64(8) 2_655 . ?
S7 Ni4 S9 85.29(7) 2_655 . ?
S10 Ni4 S9 171.27(7) . . ?
S7 Ni4 S6 170.94(7) 2_655 . ?
S10 Ni4 S6 79.78(7) . . ?
S9 Ni4 S6 102.77(7) . . ?
S7 Ni4 Ni2 120.16(6) 2_655 . ?
S10 Ni4 Ni2 52.17(5) . . ?
S9 Ni4 Ni2 122.95(5) . . ?
S6 Ni4 Ni2 51.91(5) . . ?
S7 Ni4 Ni3 47.21(5) 2_655 . ?
S10 Ni4 Ni3 124.82(7) . . ?
S9 Ni4 Ni3 48.03(4) . . ?
S6 Ni4 Ni3 136.77(5) . . ?
Ni2 Ni4 Ni3 111.73(3) . . ?
C10 S5 Ni2 98.5(2) . . ?
C10 S5 Ni1 109.3(2) . . ?
Ni2 S5 Ni1 86.69(6) . . ?
C9 S6 Ni2 104.1(2) . . ?
C9 S6 Ni4 115.4(2) . . ?
Ni2 S6 Ni4 75.45(6) . . ?
C8 S7 Ni4 97.8(3) . 2_655 ?
C8 S7 Ni3 110.1(3) . . ?
Ni4 S7 Ni3 86.77(6) 2_655 . ?
C5 S8 Ni2 106.7(2) . 2_655 ?
C5 S8 Ni1 103.7(2) . . ?
Ni2 S8 Ni1 85.33(6) 2_655 . ?
C6 S9 Ni4 104.06(19) . . ?
C6 S9 Ni3 104.7(2) . . ?
Ni4 S9 Ni3 84.68(6) . . ?
C20 S10 Ni4 104.1(3) . . ?
C20 S10 Ni2 115.9(3) . . ?
Ni4 S10 Ni2 75.67(6) . . ?
C1 C6 C4 118.2(7) . . ?
C1 C6 S9 120.4(6) . . ?
C4 C6 S9 121.3(5) . . ?
C2 C5 C3 119.2(6) . . ?
C2 C5 S8 121.3(5) . . ?
C3 C5 S8 119.5(5) . . ?
C9 C10 S5 109.9(4) . . ?
C9 C10 H10A 109.7 . . ?
S5 C10 H10A 109.7 . . ?
C9 C10 H10B 109.7 . . ?
S5 C10 H10B 109.7 . . ?
H10A C10 H10B 108.2 . . ?
C10 C9 S6 111.7(4) . . ?
C10 C9 H9A 109.3 . . ?
S6 C9 H9A 109.3 . . ?
C10 C9 H9B 109.3 . . ?
S6 C9 H9B 109.3 . . ?
H9A C9 H9B 107.9 . . ?
C6 C4 C14 118.8(7) . . ?
C6 C4 H4A 120.6 . . ?
C14 C4 H4A 120.6 . . ?
C14 C15 C13 119.7(7) . . ?
C14 C15 H15A 120.2 . . ?
C13 C15 H15A 120.2 . . ?
C5 C3 C11 119.8(8) . . ?
C5 C3 H3A 120.1 . . ?
C11 C3 H3A 120.1 . . ?
C15 C14 C4 122.2(8) . . ?
C15 C14 H14A 118.9 . . ?
C4 C14 H14A 118.9 . . ?
C5 C2 C16 119.3(7) . . ?
C5 C2 H2A 120.3 . . ?
C16 C2 H2A 120.3 . . ?
C6 C1 C13 122.1(8) . . ?
C6 C1 H1A 118.9 . . ?
C13 C1 H1A 118.9 . . ?
C15 C13 C1 118.9(7) . . ?
C15 C13 H13A 120.6 . . ?
C1 C13 H13A 120.6 . . ?
C8 C20 S10 114.9(6) 2_655 . ?
C8 C20 H20A 108.5 2_655 . ?
S10 C20 H20A 108.5 . . ?
C8 C20 H20B 108.5 2_655 . ?
S10 C20 H20B 108.5 . . ?
H20A C20 H20B 107.5 . . ?
C20 C8 S7 113.7(6) 2_655 . ?
C20 C8 H8A 108.8 2_655 . ?
S7 C8 H8A 108.8 . . ?
C20 C8 H8B 108.8 2_655 . ?
S7 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
C11 C12 C16 120.4(8) . . ?
C11 C12 H12A 119.8 . . ?
C16 C12 H12A 119.8 . . ?
C12 C11 C3 120.7(8) . . ?
C12 C11 H11A 119.7 . . ?
C3 C11 H11A 119.7 . . ?
C12 C16 C2 120.6(8) . . ?
C12 C16 H16A 119.7 . . ?
C2 C16 H16A 119.7 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.51
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.176
_refine_diff_density_min         -0.889
_refine_diff_density_rms         0.190
####################################################################### 
# 
# 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_6
_database_code_depnum_ccdc_archive 'CCDC 1055741'
_audit_update_record             
;
2015-03-24 deposited with the CCDC.
2015-06-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H44 Ni6 S12'
_chemical_formula_weight         1213.69

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'
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           ORTHORHOMBIC
_symmetry_space_group_name_H-M   pccn

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

_cell_length_a                   11.997(7)
_cell_length_b                   14.360(9)
_cell_length_c                   26.228(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4518(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6917
_cell_measurement_theta_min      2.1063
_cell_measurement_theta_max      27.6375

_exptl_crystal_description       black
_exptl_crystal_colour            block
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2480
_exptl_absorpt_coefficient_mu    3.032
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8877
_exptl_absorpt_correction_T_max  1.0000
_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  'Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 14.6306
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            33264
_diffrn_reflns_av_R_equivalents  0.0875
_diffrn_reflns_av_sigmaI/netI    0.0657
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         2.10
_diffrn_reflns_theta_max         27.52
_reflns_number_total             5172
_reflns_number_gt                3464
_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)+(0.0947P)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_number_reflns         5172
_refine_ls_number_parameters     245
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.1122
_refine_ls_R_factor_gt           0.0697
_refine_ls_wR_factor_ref         0.1998
_refine_ls_wR_factor_gt          0.1708
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.111
_refine_ls_shift/su_max          0.101
_refine_ls_shift/su_mean         0.009

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 0.7500 -0.2500 -0.41538(5) 0.0443(3) Uani 1 2 d S . .
Ni2 Ni 0.57511(7) -0.13552(6) -0.36774(3) 0.0424(3) Uani 1 1 d . . .
Ni3 Ni 0.56595(7) -0.14718(6) -0.26148(3) 0.0416(3) Uani 1 1 d . . .
Ni4 Ni 0.7500 -0.2500 -0.21175(5) 0.0463(3) Uani 1 2 d S . .
S1 S 0.56916(16) -0.24140(13) -0.42596(7) 0.0503(5) Uani 1 1 d . . .
S2 S 0.73362(16) -0.09896(13) -0.40609(6) 0.0480(5) Uani 1 1 d . . .
S3 S 0.43811(14) -0.18061(13) -0.31902(7) 0.0467(4) Uani 1 1 d . . .
S4 S 0.57338(15) -0.02459(12) -0.31011(7) 0.0467(4) Uani 1 1 d . . .
S5 S 0.56976(15) -0.28051(13) -0.21939(7) 0.0511(5) Uani 1 1 d . . .
S6 S 0.68471(17) -0.10889(14) -0.20307(7) 0.0529(5) Uani 1 1 d . . .
C1 C 0.4040(7) -0.3044(6) -0.3240(3) 0.062(2) Uani 1 1 d . . .
H1A H 0.3956 -0.3291 -0.2898 0.074 Uiso 1 1 calc R . .
H1B H 0.3323 -0.3100 -0.3408 0.074 Uiso 1 1 calc R . .
C2 C 0.4857(8) -0.3646(6) -0.3520(4) 0.073(2) Uani 1 1 d . . .
H2A H 0.5587 -0.3562 -0.3368 0.088 Uiso 1 1 calc R . .
H2B H 0.4646 -0.4292 -0.3472 0.088 Uiso 1 1 calc R . .
C3 C 0.4945(7) -0.3460(6) -0.4076(3) 0.064(2) Uani 1 1 d . . .
H3A H 0.4197 -0.3423 -0.4215 0.077 Uiso 1 1 calc R . .
H3B H 0.5309 -0.3989 -0.4235 0.077 Uiso 1 1 calc R . .
C4 C 0.7148(6) -0.0536(5) -0.4683(3) 0.0520(18) Uani 1 1 d . . .
C5 C 0.6457(8) 0.0203(7) -0.4771(4) 0.090(3) Uani 1 1 d . . .
H5A H 0.6030 0.0442 -0.4506 0.109 Uiso 1 1 calc R . .
C6 C 0.6386(11) 0.0596(8) -0.5244(5) 0.113(4) Uani 1 1 d . . .
H6A H 0.5906 0.1097 -0.5295 0.136 Uiso 1 1 calc R . .
C7 C 0.6988(10) 0.0281(8) -0.5637(4) 0.091(3) Uani 1 1 d . . .
H7A H 0.6924 0.0557 -0.5957 0.110 Uiso 1 1 calc R . .
C8 C 0.7713(9) -0.0465(8) -0.5563(3) 0.085(3) Uani 1 1 d . . .
H8A H 0.8146 -0.0692 -0.5830 0.102 Uiso 1 1 calc R . .
C9 C 0.7768(8) -0.0854(6) -0.5088(3) 0.074(2) Uani 1 1 d . . .
H9A H 0.8245 -0.1356 -0.5037 0.088 Uiso 1 1 calc R . .
C10 C 0.7034(7) 0.0397(5) -0.3060(3) 0.060(2) Uani 1 1 d . . .
H10A H 0.7283 0.0538 -0.3404 0.073 Uiso 1 1 calc R . .
H10B H 0.6890 0.0984 -0.2890 0.073 Uiso 1 1 calc R . .
C11 C 0.7981(7) -0.0101(6) -0.2779(4) 0.067(2) Uani 1 1 d . . .
H11A H 0.8075 -0.0716 -0.2927 0.081 Uiso 1 1 calc R . .
H11B H 0.8667 0.0241 -0.2836 0.081 Uiso 1 1 calc R . .
C12 C 0.7809(6) -0.0203(5) -0.2223(3) 0.059(2) Uani 1 1 d . . .
H12A H 0.7549 0.0388 -0.2089 0.070 Uiso 1 1 calc R . .
H12B H 0.8524 -0.0334 -0.2066 0.070 Uiso 1 1 calc R . .
C13 C 0.5167(6) -0.2574(5) -0.1570(3) 0.0538(19) Uani 1 1 d . . .
C14 C 0.4259(10) -0.2072(9) -0.1506(5) 0.120(4) Uani 1 1 d U . .
H14A H 0.3899 -0.1821 -0.1788 0.145 Uiso 1 1 calc R . .
C15 C 0.3825(12) -0.1910(10) -0.1010(5) 0.136(5) Uani 1 1 d U . .
H15A H 0.3162 -0.1584 -0.0966 0.163 Uiso 1 1 calc R . .
C16 C 0.4395(11) -0.2239(9) -0.0603(5) 0.108(4) Uani 1 1 d U . .
H16A H 0.4181 -0.2071 -0.0275 0.130 Uiso 1 1 calc R . .
C17 C 0.5231(10) -0.2783(8) -0.0670(4) 0.093(3) Uani 1 1 d . . .
H17A H 0.5560 -0.3070 -0.0390 0.111 Uiso 1 1 calc R . .
C18 C 0.5652(8) -0.2950(7) -0.1156(3) 0.080(3) Uani 1 1 d . . .
H18A H 0.6277 -0.3326 -0.1195 0.096 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 S1 2.191(2) 2_645 ?
Ni1 S1 2.191(2) . ?
Ni1 S2 2.191(2) . ?
Ni1 S2 2.191(2) 2_645 ?
Ni1 Ni2 2.9439(15) . ?
Ni1 Ni2 2.9439(15) 2_645 ?
Ni2 S1 2.156(2) . ?
Ni2 S3 2.180(2) . ?
Ni2 S4 2.196(2) . ?
Ni2 S2 2.214(2) . ?
Ni2 Ni3 2.794(2) . ?
Ni3 S6 2.163(2) . ?
Ni3 S4 2.176(2) . ?
Ni3 S3 2.205(2) . ?
Ni3 S5 2.211(2) . ?
Ni3 Ni4 2.9593(15) . ?
Ni4 S6 2.184(2) . ?
Ni4 S6 2.184(2) 2_645 ?
Ni4 S5 2.215(2) . ?
Ni4 S5 2.215(2) 2_645 ?
Ni4 Ni3 2.9593(15) 2_645 ?
S1 C3 1.814(8) . ?
S2 C4 1.771(7) . ?
S3 C1 1.829(8) . ?
S4 C10 1.816(8) . ?
S5 C13 1.786(8) . ?
S6 C12 1.789(8) . ?
C1 C2 1.498(12) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.487(11) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.367(11) . ?
C4 C9 1.376(11) . ?
C5 C6 1.366(13) . ?
C5 H5A 0.9300 . ?
C6 C7 1.337(15) . ?
C6 H6A 0.9300 . ?
C7 C8 1.393(14) . ?
C7 H7A 0.9300 . ?
C8 C9 1.368(11) . ?
C8 H8A 0.9300 . ?
C9 H9A 0.9300 . ?
C10 C11 1.532(11) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.482(11) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.318(12) . ?
C13 C18 1.345(11) . ?
C14 C15 1.421(16) . ?
C14 H14A 0.9300 . ?
C15 C16 1.354(16) . ?
C15 H15A 0.9300 . ?
C16 C17 1.284(15) . ?
C16 H16A 0.9300 . ?
C17 C18 1.392(13) . ?
C17 H17A 0.9300 . ?
C18 H18A 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
S1 Ni1 S1 165.44(12) 2_645 . ?
S1 Ni1 S2 99.13(7) 2_645 . ?
S1 Ni1 S2 82.50(7) . . ?
S1 Ni1 S2 82.50(7) 2_645 2_645 ?
S1 Ni1 S2 99.13(7) . 2_645 ?
S2 Ni1 S2 167.23(11) . 2_645 ?
S1 Ni1 Ni2 142.29(6) 2_645 . ?
S1 Ni1 Ni2 46.88(6) . . ?
S2 Ni1 Ni2 48.41(5) . . ?
S2 Ni1 Ni2 124.71(6) 2_645 . ?
S1 Ni1 Ni2 46.88(6) 2_645 2_645 ?
S1 Ni1 Ni2 142.29(6) . 2_645 ?
S2 Ni1 Ni2 124.71(6) . 2_645 ?
S2 Ni1 Ni2 48.41(5) 2_645 2_645 ?
Ni2 Ni1 Ni2 129.77(6) . 2_645 ?
S1 Ni2 S3 100.41(9) . . ?
S1 Ni2 S4 177.07(8) . . ?
S3 Ni2 S4 78.75(8) . . ?
S1 Ni2 S2 82.75(8) . . ?
S3 Ni2 S2 169.74(8) . . ?
S4 Ni2 S2 98.56(8) . . ?
S1 Ni2 Ni3 131.52(7) . . ?
S3 Ni2 Ni3 50.80(6) . . ?
S4 Ni2 Ni3 49.95(6) . . ?
S2 Ni2 Ni3 120.07(6) . . ?
S1 Ni2 Ni1 47.87(6) . . ?
S3 Ni2 Ni1 128.33(7) . . ?
S4 Ni2 Ni1 134.74(6) . . ?
S2 Ni2 Ni1 47.74(6) . . ?
Ni3 Ni2 Ni1 114.70(4) . . ?
S6 Ni3 S4 100.52(9) . . ?
S6 Ni3 S3 176.73(8) . . ?
S4 Ni3 S3 78.66(8) . . ?
S6 Ni3 S5 81.53(8) . . ?
S4 Ni3 S5 173.08(8) . . ?
S3 Ni3 S5 99.65(8) . . ?
S6 Ni3 Ni2 131.71(7) . . ?
S4 Ni3 Ni2 50.60(6) . . ?
S3 Ni3 Ni2 50.03(6) . . ?
S5 Ni3 Ni2 123.31(6) . . ?
S6 Ni3 Ni4 47.40(6) . . ?
S4 Ni3 Ni4 129.17(6) . . ?
S3 Ni3 Ni4 135.41(7) . . ?
S5 Ni3 Ni4 48.11(5) . . ?
Ni2 Ni3 Ni4 116.12(4) . . ?
S6 Ni4 S6 168.03(12) . 2_645 ?
S6 Ni4 S5 80.96(8) . . ?
S6 Ni4 S5 100.14(8) 2_645 . ?
S6 Ni4 S5 100.14(8) . 2_645 ?
S6 Ni4 S5 80.96(8) 2_645 2_645 ?
S5 Ni4 S5 169.61(12) . 2_645 ?
S6 Ni4 Ni3 46.80(5) . . ?
S6 Ni4 Ni3 140.93(6) 2_645 . ?
S5 Ni4 Ni3 47.97(6) . . ?
S5 Ni4 Ni3 126.14(7) 2_645 . ?
S6 Ni4 Ni3 140.93(6) . 2_645 ?
S6 Ni4 Ni3 46.80(5) 2_645 2_645 ?
S5 Ni4 Ni3 126.14(7) . 2_645 ?
S5 Ni4 Ni3 47.97(6) 2_645 2_645 ?
Ni3 Ni4 Ni3 127.69(6) . 2_645 ?
C3 S1 Ni2 114.4(3) . . ?
C3 S1 Ni1 114.1(3) . . ?
Ni2 S1 Ni1 85.25(7) . . ?
C4 S2 Ni1 105.8(3) . . ?
C4 S2 Ni2 113.3(3) . . ?
Ni1 S2 Ni2 83.85(7) . . ?
C1 S3 Ni2 114.5(3) . . ?
C1 S3 Ni3 114.6(3) . . ?
Ni2 S3 Ni3 79.17(8) . . ?
C10 S4 Ni3 114.3(3) . . ?
C10 S4 Ni2 113.6(3) . . ?
Ni3 S4 Ni2 79.46(8) . . ?
C13 S5 Ni3 106.8(2) . . ?
C13 S5 Ni4 103.2(3) . . ?
Ni3 S5 Ni4 83.92(7) . . ?
C12 S6 Ni3 113.9(3) . . ?
C12 S6 Ni4 113.5(3) . . ?
Ni3 S6 Ni4 85.79(8) . . ?
C2 C1 S3 116.7(6) . . ?
C2 C1 H1A 108.1 . . ?
S3 C1 H1A 108.1 . . ?
C2 C1 H1B 108.1 . . ?
S3 C1 H1B 108.1 . . ?
H1A C1 H1B 107.3 . . ?
C3 C2 C1 115.0(7) . . ?
C3 C2 H2A 108.5 . . ?
C1 C2 H2A 108.5 . . ?
C3 C2 H2B 108.5 . . ?
C1 C2 H2B 108.5 . . ?
H2A C2 H2B 107.5 . . ?
C2 C3 S1 116.4(6) . . ?
C2 C3 H3A 108.2 . . ?
S1 C3 H3A 108.2 . . ?
C2 C3 H3B 108.2 . . ?
S1 C3 H3B 108.2 . . ?
H3A C3 H3B 107.4 . . ?
C5 C4 C9 117.0(8) . . ?
C5 C4 S2 121.3(6) . . ?
C9 C4 S2 121.4(6) . . ?
C4 C5 C6 120.8(10) . . ?
C4 C5 H5A 119.6 . . ?
C6 C5 H5A 119.6 . . ?
C7 C6 C5 121.8(10) . . ?
C7 C6 H6A 119.1 . . ?
C5 C6 H6A 119.1 . . ?
C6 C7 C8 119.3(9) . . ?
C6 C7 H7A 120.3 . . ?
C8 C7 H7A 120.3 . . ?
C9 C8 C7 118.1(9) . . ?
C9 C8 H8A 120.9 . . ?
C7 C8 H8A 120.9 . . ?
C8 C9 C4 122.9(9) . . ?
C8 C9 H9A 118.6 . . ?
C4 C9 H9A 118.6 . . ?
C11 C10 S4 115.3(5) . . ?
C11 C10 H10A 108.4 . . ?
S4 C10 H10A 108.4 . . ?
C11 C10 H10B 108.4 . . ?
S4 C10 H10B 108.4 . . ?
H10A C10 H10B 107.5 . . ?
C12 C11 C10 114.6(7) . . ?
C12 C11 H11A 108.6 . . ?
C10 C11 H11A 108.6 . . ?
C12 C11 H11B 108.6 . . ?
C10 C11 H11B 108.6 . . ?
H11A C11 H11B 107.6 . . ?
C11 C12 S6 115.9(6) . . ?
C11 C12 H12A 108.3 . . ?
S6 C12 H12A 108.3 . . ?
C11 C12 H12B 108.3 . . ?
S6 C12 H12B 108.3 . . ?
H12A C12 H12B 107.4 . . ?
C14 C13 C18 118.3(9) . . ?
C14 C13 S5 120.9(7) . . ?
C18 C13 S5 120.8(7) . . ?
C13 C14 C15 120.7(11) . . ?
C13 C14 H14A 119.7 . . ?
C15 C14 H14A 119.7 . . ?
C16 C15 C14 118.7(12) . . ?
C16 C15 H15A 120.7 . . ?
C14 C15 H15A 120.7 . . ?
C17 C16 C15 119.9(12) . . ?
C17 C16 H16A 120.0 . . ?
C15 C16 H16A 120.0 . . ?
C16 C17 C18 120.9(10) . . ?
C16 C17 H17A 119.5 . . ?
C18 C17 H17A 119.6 . . ?
C13 C18 C17 121.0(9) . . ?
C13 C18 H18A 119.5 . . ?
C17 C18 H18A 119.5 . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.52
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.878
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.177
