# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 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_ic17394
_database_code_depnum_ccdc_archive 'CCDC 1486165'
_audit_update_record             
;
2016-06-17 deposited with the CCDC.
2016-09-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C81 H60 Cl10 F3 N16 Ni4 O3 S'
_chemical_formula_weight         1983.85

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   14.6069(5)
_cell_length_b                   17.1511(5)
_cell_length_c                   17.8766(4)
_cell_angle_alpha                76.392(2)
_cell_angle_beta                 86.344(2)
_cell_angle_gamma                69.1391(14)
_cell_volume                     4066.5(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    54086
_cell_measurement_theta_min      1.30
_cell_measurement_theta_max      25.00

_exptl_crystal_description       needle
_exptl_crystal_colour            dark-brown
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2014
_exptl_absorpt_coefficient_mu    1.334
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6903
_exptl_absorpt_correction_T_max  0.9363
_exptl_absorpt_process_details   'SORTAV (Blessing, 1995)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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  'NONIUS KappaCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            54086
_diffrn_reflns_av_R_equivalents  0.0768
_diffrn_reflns_av_sigmaI/netI    0.0912
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.30
_diffrn_reflns_theta_max         25.00
_reflns_number_total             14281
_reflns_number_gt                7012
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'NONIUS COLLECT'
_computing_cell_refinement       DENZO-SMN
_computing_data_reduction        DENZO-SMN
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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. 
 The distance restraints are used to the CH2Cl2 solvents. The isotropice 
 restraints are applied to a CF3SO3 anion and the atoms of C19, C46 and 
 C80.
;

_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)+(0.1695P)²+20.5751P] 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         14281
_refine_ls_number_parameters     1157
_refine_ls_number_restraints     78
_refine_ls_R_factor_all          0.1874
_refine_ls_R_factor_gt           0.0969
_refine_ls_wR_factor_ref         0.3369
_refine_ls_wR_factor_gt          0.2648
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.004
_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 0.85736(12) -0.32798(8) 0.77885(8) 0.0671(5) Uani 1 1 d . A 7
Ni2 Ni 0.79572(9) -0.17904(7) 0.73442(7) 0.0452(4) Uani 1 1 d . A 7
Ni3 Ni 0.73376(8) -0.02850(7) 0.69006(6) 0.0366(3) Uani 1 1 d . A 7
Ni4 Ni 0.66625(8) 0.12663(7) 0.64567(6) 0.0375(3) Uani 1 1 d . A 7
Cl1 Cl 0.9196(3) -0.48144(19) 0.8225(2) 0.1031(14) Uani 1 1 d . A 7
Cl2 Cl 0.59819(18) 0.27578(15) 0.59877(15) 0.0539(7) Uani 1 1 d . A 7
N1 N 0.9843(7) -0.3193(5) 0.7161(5) 0.062(3) Uani 1 1 d . A 7
N2 N 0.8987(5) -0.1794(5) 0.6529(4) 0.0413(19) Uani 1 1 d . A 7
N3 N 0.8024(5) -0.0414(4) 0.5969(4) 0.0372(18) Uani 1 1 d . A 7
N4 N 0.7020(5) 0.0966(5) 0.5371(4) 0.0370(18) Uani 1 1 d . A 7
N5 N 0.7864(7) -0.3291(6) 0.6779(5) 0.064(3) Uani 1 1 d . A 7
N6 N 0.7028(6) -0.1836(5) 0.6598(4) 0.047(2) Uani 1 1 d . A 7
N7 N 0.6218(6) -0.0375(5) 0.6479(4) 0.044(2) Uani 1 1 d . A 7
N8 N 0.5350(5) 0.1036(5) 0.6492(4) 0.0402(18) Uani 1 1 d . A 7
N9 N 0.7080(13) -0.3044(18) 0.8313(17) 0.054(5) Uani 0.599(5) 1 d P A 1
N10 N 0.680(2) -0.159(2) 0.8071(19) 0.032(5) Uani 0.599(5) 1 d P A 1
N9' N 0.748(2) -0.320(3) 0.850(3) 0.054(5) Uani 0.401(5) 1 d P A 2
N10' N 0.708(3) -0.172(4) 0.824(3) 0.032(5) Uani 0.401(5) 1 d P A 2
N11 N 0.6695(6) -0.0202(5) 0.7841(4) 0.0422(19) Uani 1 1 d . . .
N12 N 0.6515(6) 0.1228(5) 0.7640(4) 0.046(2) Uani 1 1 d . . .
N13 N 0.9137(8) -0.3008(6) 0.8723(5) 0.072(3) Uani 1 1 d . . .
N14 N 0.8838(6) -0.1597(5) 0.8057(4) 0.048(2) Uani 1 1 d . . .
N15 N 0.8460(5) -0.0213(5) 0.7341(4) 0.0405(19) Uani 1 1 d . . .
N16 N 0.8118(5) 0.1155(5) 0.6575(4) 0.0380(18) Uani 1 1 d . . .
C1 C 1.0671(9) -0.3857(8) 0.7292(7) 0.081(4) Uani 1 1 d . . .
H1 H 1.0679 -0.4356 0.7664 0.097 Uiso 1 1 calc R A 7
C2 C 1.1537(10) -0.3859(8) 0.6907(8) 0.096(5) Uani 1 1 d . A .
H2 H 1.2120 -0.4346 0.7031 0.115 Uiso 1 1 calc R . .
C3 C 1.1541(8) -0.3161(8) 0.6354(7) 0.076(4) Uani 1 1 d . . .
H3 H 1.2119 -0.3170 0.6075 0.091 Uiso 1 1 calc R A .
C4 C 1.0687(7) -0.2428(7) 0.6197(6) 0.058(3) Uani 1 1 d . A .
C5 C 0.9842(7) -0.2475(6) 0.6625(6) 0.052(3) Uani 1 1 d . . .
C6 C 1.0590(7) -0.1659(6) 0.5657(5) 0.047(2) Uani 1 1 d . . .
H6 H 1.1140 -0.1600 0.5369 0.056 Uiso 1 1 calc R A .
C7 C 0.9721(7) -0.1002(6) 0.5545(5) 0.042(2) Uani 1 1 d . A .
H7 H 0.9657 -0.0491 0.5169 0.050 Uiso 1 1 calc R . .
C8 C 0.8891(6) -0.1081(6) 0.6000(5) 0.039(2) Uani 1 1 d . . .
C9 C 0.7665(6) 0.0195(6) 0.5298(5) 0.036(2) Uani 1 1 d . . .
C10 C 0.7904(7) 0.0027(7) 0.4557(5) 0.047(2) Uani 1 1 d . A .
H10 H 0.8331 -0.0523 0.4506 0.057 Uiso 1 1 calc R . .
C11 C 0.7517(8) 0.0659(7) 0.3919(6) 0.051(3) Uani 1 1 d . . .
H11 H 0.7694 0.0549 0.3423 0.061 Uiso 1 1 calc R A .
C12 C 0.6877(8) 0.1452(7) 0.3981(6) 0.050(3) Uani 1 1 d . A .
C13 C 0.6655(7) 0.1562(6) 0.4724(6) 0.046(2) Uani 1 1 d . . .
H13 H 0.6206 0.2103 0.4779 0.055 Uiso 1 1 calc RD A 7
C14 C 0.6689(17) 0.2100(17) 0.3261(14) 0.063(6) Uani 0.599(5) 1 d P A 1
C15 C 0.7325(18) 0.2052(14) 0.2621(11) 0.084(6) Uani 0.599(5) 1 d P A 1
H15 H 0.7885 0.1557 0.2609 0.101 Uiso 0.599(5) 1 calc PR A 1
C16 C 0.706(3) 0.281(2) 0.1987(14) 0.125(10) Uani 0.599(5) 1 d P A 1
H16 H 0.7485 0.2817 0.1560 0.150 Uiso 0.599(5) 1 calc PR A 1
C17 C 0.624(3) 0.3502(18) 0.1982(17) 0.121(9) Uani 0.599(5) 1 d P A 1
H17 H 0.6081 0.3969 0.1545 0.146 Uiso 0.599(5) 1 calc PR A 1
C18 C 0.560(2) 0.3539(18) 0.2636(17) 0.096(8) Uani 0.599(5) 1 d P A 1
H18 H 0.5014 0.4020 0.2633 0.115 Uiso 0.599(5) 1 calc PR A 1
C19 C 0.5861(19) 0.2857(15) 0.3259(12) 0.064(6) Uani 0.599(5) 1 d PU A 1
H19 H 0.5477 0.2891 0.3708 0.077 Uiso 0.599(5) 1 calc PR A 1
C14' C 0.616(3) 0.217(3) 0.337(2) 0.063(6) Uani 0.401(5) 1 d P A 2
C15' C 0.611(3) 0.194(2) 0.2654(16) 0.084(6) Uani 0.401(5) 1 d P A 2
H15' H 0.6482 0.1386 0.2582 0.101 Uiso 0.401(5) 1 calc PR A 2
C16' C 0.550(3) 0.257(3) 0.206(2) 0.125(10) Uani 0.401(5) 1 d P A 2
H16' H 0.5460 0.2451 0.1570 0.150 Uiso 0.401(5) 1 calc PR A 2
C17' C 0.497(4) 0.335(3) 0.219(3) 0.121(9) Uani 0.401(5) 1 d P A 2
H17' H 0.4545 0.3744 0.1780 0.146 Uiso 0.401(5) 1 calc PR A 2
C18' C 0.497(3) 0.363(3) 0.285(3) 0.096(8) Uani 0.401(5) 1 d P A 2
H18' H 0.4571 0.4192 0.2889 0.115 Uiso 0.401(5) 1 calc PR A 2
C19' C 0.559(3) 0.3046(18) 0.3447(18) 0.064(6) Uani 0.401(5) 1 d P A 2
H19' H 0.5652 0.3216 0.3906 0.077 Uiso 0.401(5) 1 calc PRD A 2
C20 C 0.7973(10) -0.4030(7) 0.6572(8) 0.077(4) Uani 1 1 d U . .
H20 H 0.8460 -0.4538 0.6841 0.092 Uiso 1 1 calc R A 7
C21 C 0.7434(13) -0.4105(10) 0.6001(9) 0.091(4) Uani 1 1 d U A .
H21 H 0.7563 -0.4644 0.5879 0.109 Uiso 1 1 calc R . .
C22 C 0.6738(11) -0.3413(9) 0.5633(8) 0.078(4) Uani 1 1 d . . .
H22 H 0.6357 -0.3452 0.5241 0.094 Uiso 1 1 calc R A .
C23 C 0.6557(9) -0.2628(7) 0.5810(7) 0.058(3) Uani 1 1 d . A .
C24 C 0.7120(9) -0.2575(7) 0.6380(7) 0.059(3) Uani 1 1 d . . .
C25 C 0.5809(9) -0.1862(8) 0.5458(7) 0.063(3) Uani 1 1 d . . .
H25 H 0.5407 -0.1861 0.5060 0.076 Uiso 1 1 calc R A .
C26 C 0.5663(8) -0.1131(7) 0.5688(6) 0.055(3) Uani 1 1 d . A .
H26 H 0.5138 -0.0623 0.5469 0.066 Uiso 1 1 calc R . .
C27 C 0.6301(8) -0.1118(7) 0.6264(6) 0.050(3) Uani 1 1 d . . .
C28 C 0.5318(7) 0.0265(6) 0.6509(5) 0.041(2) Uani 1 1 d . . .
C29 C 0.4444(7) 0.0101(7) 0.6635(6) 0.051(3) Uani 1 1 d . A .
H29 H 0.4435 -0.0459 0.6675 0.061 Uiso 1 1 calc R . .
C30 C 0.3586(8) 0.0775(7) 0.6698(6) 0.057(3) Uani 1 1 d . . .
H30 H 0.2982 0.0677 0.6752 0.069 Uiso 1 1 calc R A .
C31 C 0.3586(7) 0.1595(7) 0.6685(6) 0.053(3) Uani 1 1 d . A .
C32 C 0.4496(6) 0.1675(6) 0.6586(6) 0.045(2) Uani 1 1 d . . .
H32 H 0.4533 0.2218 0.6583 0.053 Uiso 1 1 calc R A 7
C33 C 0.2711(8) 0.2314(8) 0.6792(7) 0.063(3) Uani 1 1 d . . .
C34 C 0.1894(9) 0.2168(9) 0.7184(8) 0.081(4) Uani 1 1 d . A .
H34 H 0.1903 0.1600 0.7374 0.097 Uiso 1 1 calc R . .
C35 C 0.1084(9) 0.2856(11) 0.7290(10) 0.102(5) Uani 1 1 d . . .
H35 H 0.0553 0.2749 0.7575 0.122 Uiso 1 1 calc R A .
C36 C 0.1023(10) 0.3681(11) 0.6997(11) 0.113(6) Uani 1 1 d . A .
H36 H 0.0445 0.4143 0.7057 0.136 Uiso 1 1 calc R . .
C37 C 0.1835(10) 0.3846(9) 0.6599(10) 0.098(5) Uani 1 1 d . . .
H37 H 0.1827 0.4416 0.6419 0.117 Uiso 1 1 calc R A .
C38 C 0.2646(8) 0.3147(8) 0.6483(8) 0.079(4) Uani 1 1 d . A .
H38 H 0.3167 0.3251 0.6181 0.095 Uiso 1 1 calc R . .
C39 C 0.6778(17) -0.3718(13) 0.8593(12) 0.064(6) Uani 0.599(5) 1 d P A 1
H39 H 0.7173 -0.4268 0.8518 0.077 Uiso 0.599(5) 1 calc PR A 1
C40 C 0.5919(18) -0.3625(15) 0.8980(13) 0.080(6) Uani 0.599(5) 1 d P A 1
H40 H 0.5716 -0.4104 0.9151 0.096 Uiso 0.599(5) 1 calc PR A 1
C41 C 0.5350(17) -0.2847(14) 0.9125(13) 0.073(6) Uani 0.599(5) 1 d P A 1
H41 H 0.4766 -0.2785 0.9408 0.088 Uiso 0.599(5) 1 calc PR A 1
C42 C 0.5656(14) -0.2135(13) 0.8839(11) 0.051(5) Uani 0.599(5) 1 d P A 1
C43 C 0.6497(19) -0.226(2) 0.8416(16) 0.046(6) Uani 0.599(5) 1 d P A 1
C44 C 0.5109(15) -0.1307(14) 0.8948(11) 0.054(5) Uani 0.599(5) 1 d P A 1
H44 H 0.4541 -0.1212 0.9254 0.065 Uiso 0.599(5) 1 calc PR A 1
C45 C 0.5407(19) -0.066(2) 0.8616(17) 0.046(7) Uani 0.599(5) 1 d P A 1
H45 H 0.5019 -0.0097 0.8650 0.055 Uiso 0.599(5) 1 calc PR A 1
C46 C 0.633(2) -0.082(3) 0.820(2) 0.043(6) Uani 0.599(5) 1 d PU A 1
C39' C 0.728(3) -0.384(2) 0.8969(19) 0.064(6) Uani 0.401(5) 1 d P A 2
H39' H 0.7698 -0.4393 0.8915 0.077 Uiso 0.401(5) 1 calc PR A 2
C40' C 0.659(3) -0.384(2) 0.9510(19) 0.080(6) Uani 0.401(5) 1 d P A 2
H40' H 0.6549 -0.4360 0.9810 0.096 Uiso 0.401(5) 1 calc PR A 2
C41' C 0.596(3) -0.306(2) 0.961(2) 0.073(6) Uani 0.401(5) 1 d P A 2
H41' H 0.5431 -0.3021 0.9956 0.088 Uiso 0.401(5) 1 calc PR A 2
C42' C 0.611(2) -0.232(2) 0.9187(18) 0.051(5) Uani 0.401(5) 1 d P A 2
C43' C 0.686(3) -0.240(4) 0.864(3) 0.046(6) Uani 0.401(5) 1 d P A 2
C44' C 0.559(2) -0.151(2) 0.9266(19) 0.054(5) Uani 0.401(5) 1 d P A 2
H44' H 0.5081 -0.1446 0.9631 0.065 Uiso 0.401(5) 1 calc PR A 2
C45' C 0.575(3) -0.076(4) 0.883(3) 0.046(7) Uani 0.401(5) 1 d P A 2
H45' H 0.5371 -0.0198 0.8895 0.055 Uiso 0.401(5) 1 calc PR A 2
C46' C 0.654(4) -0.092(4) 0.831(4) 0.043(6) Uani 0.401(5) 1 d P A 2
C47 C 0.6604(7) 0.0483(6) 0.8152(5) 0.046(3) Uani 1 1 d . A .
C48 C 0.6672(9) 0.0426(8) 0.8950(6) 0.068(3) Uani 1 1 d . . .
H48 H 0.6768 -0.0106 0.9305 0.081 Uiso 1 1 calc R A .
C49 C 0.6601(10) 0.1124(8) 0.9214(6) 0.072(4) Uani 1 1 d . A .
H49 H 0.6655 0.1078 0.9751 0.086 Uiso 1 1 calc R . .
C50 C 0.6451(10) 0.1896(8) 0.8704(7) 0.074(4) Uani 1 1 d . . .
C51 C 0.6436(8) 0.1928(7) 0.7916(6) 0.054(3) Uani 1 1 d . A .
H51 H 0.6368 0.2454 0.7559 0.065 Uiso 1 1 calc R . .
C52 C 0.642(2) 0.2602(17) 0.9048(17) 0.052(7) Uani 0.599(5) 1 d P A 1
C53 C 0.7038(16) 0.2578(14) 0.9622(13) 0.059(5) Uani 0.599(5) 1 d P A 1
H53 H 0.7557 0.2056 0.9819 0.071 Uiso 0.599(5) 1 calc PR A 1
C54 C 0.693(2) 0.3292(16) 0.9925(15) 0.077(7) Uani 0.599(5) 1 d P A 1
H54 H 0.7359 0.3267 1.0313 0.092 Uiso 0.599(5) 1 calc PR A 1
C55 C 0.615(3) 0.4039(17) 0.962(2) 0.106(12) Uani 0.599(5) 1 d P A 1
H55 H 0.6010 0.4522 0.9838 0.127 Uiso 0.599(5) 1 calc PR A 1
C56 C 0.562(2) 0.4095(17) 0.9073(17) 0.079(7) Uani 0.599(5) 1 d P A 1
H56 H 0.5153 0.4642 0.8863 0.095 Uiso 0.599(5) 1 calc PR A 1
C57 C 0.5677(17) 0.3380(16) 0.8724(14) 0.059(5) Uani 0.599(5) 1 d P A 1
H57 H 0.5249 0.3440 0.8320 0.071 Uiso 0.599(5) 1 calc PR A 1
C52' C 0.603(4) 0.288(3) 0.883(3) 0.052(7) Uani 0.401(5) 1 d P A 2
C53' C 0.640(2) 0.292(2) 0.950(2) 0.059(5) Uani 0.401(5) 1 d P A 2
H53' H 0.6765 0.2391 0.9834 0.071 Uiso 0.401(5) 1 calc PR A 2
C54' C 0.630(4) 0.367(3) 0.972(3) 0.077(7) Uani 0.401(5) 1 d P A 2
H54' H 0.6693 0.3699 1.0101 0.092 Uiso 0.401(5) 1 calc PR A 2
C55' C 0.543(4) 0.447(2) 0.924(3) 0.106(12) Uani 0.401(5) 1 d P A 2
H55' H 0.5181 0.5000 0.9396 0.127 Uiso 0.401(5) 1 calc PR A 2
C56' C 0.508(3) 0.435(2) 0.861(2) 0.079(7) Uani 0.401(5) 1 d P A 2
H56' H 0.4640 0.4852 0.8285 0.095 Uiso 0.401(5) 1 calc PR A 2
C57' C 0.526(2) 0.363(2) 0.839(2) 0.059(5) Uani 0.401(5) 1 d P A 2
H57' H 0.4913 0.3598 0.7970 0.071 Uiso 0.401(5) 1 calc PR A 2
C58 C 0.9489(12) -0.3623(9) 0.9360(8) 0.092(5) Uani 1 1 d . A .
H58 H 0.9400 -0.4154 0.9404 0.110 Uiso 1 1 calc R . .
C59 C 0.9969(13) -0.3535(11) 0.9952(9) 0.112(6) Uani 1 1 d . . .
H59 H 1.0219 -0.4011 1.0374 0.135 Uiso 1 1 calc R A .
C60 C 1.0096(12) -0.2784(11) 0.9952(8) 0.101(5) Uani 1 1 d . A .
H60 H 1.0411 -0.2714 1.0368 0.121 Uiso 1 1 calc R . .
C61 C 0.9716(10) -0.2098(9) 0.9272(7) 0.076(4) Uani 1 1 d . . .
C62 C 0.9246(9) -0.2242(8) 0.8697(6) 0.064(3) Uani 1 1 d . A .
C63 C 0.9784(10) -0.1285(10) 0.9189(7) 0.086(4) Uani 1 1 d . A .
H63 H 1.0116 -0.1177 0.9572 0.103 Uiso 1 1 calc R . .
C64 C 0.9372(9) -0.0646(8) 0.8554(6) 0.065(3) Uani 1 1 d . . .
H64 H 0.9392 -0.0088 0.8505 0.078 Uiso 1 1 calc R A .
C65 C 0.8917(7) -0.0826(6) 0.7973(5) 0.046(2) Uani 1 1 d . A .
C66 C 0.8785(7) 0.0456(6) 0.7000(5) 0.038(2) Uani 1 1 d . A .
C67 C 0.9767(6) 0.0406(6) 0.7045(5) 0.043(2) Uani 1 1 d . . .
H67 H 1.0247 -0.0099 0.7326 0.052 Uiso 1 1 calc R A .
C68 C 1.0022(7) 0.1104(6) 0.6676(6) 0.048(2) Uani 1 1 d . A .
H68 H 1.0673 0.1086 0.6727 0.057 Uiso 1 1 calc R . .
C69 C 0.9341(7) 0.1821(6) 0.6236(5) 0.042(2) Uani 1 1 d . . .
C70 C 0.8385(7) 0.1822(6) 0.6184(5) 0.042(2) Uani 1 1 d . A .
H70 H 0.7911 0.2301 0.5867 0.050 Uiso 1 1 calc R . .
C71 C 0.9591(7) 0.2567(7) 0.5775(6) 0.051(3) Uani 1 1 d . A .
C72 C 1.0551(8) 0.2457(7) 0.5532(7) 0.062(3) Uani 1 1 d . . .
H72 H 1.1057 0.1913 0.5676 0.074 Uiso 1 1 calc R A .
C73 C 1.0757(10) 0.3156(9) 0.5075(8) 0.081(4) Uani 1 1 d . A .
H73 H 1.1408 0.3076 0.4908 0.098 Uiso 1 1 calc R . .
C74 C 1.0093(10) 0.3904(8) 0.4873(8) 0.079(4) Uani 1 1 d . . .
H74 H 1.0263 0.4364 0.4568 0.095 Uiso 1 1 calc R A .
C75 C 0.9123(10) 0.4047(7) 0.5098(8) 0.084(4) Uani 1 1 d . A .
H75 H 0.8632 0.4596 0.4937 0.101 Uiso 1 1 calc R . .
C76 C 0.8890(9) 0.3380(7) 0.5558(7) 0.068(3) Uani 1 1 d . . .
H76 H 0.8238 0.3479 0.5729 0.082 Uiso 1 1 calc R A .
S1 S 0.2228(4) -0.0271(4) 0.8576(3) 0.1162(15) Uani 1 1 d U . .
O1 O 0.1916(7) 0.0018(6) 0.7798(5) 0.088(3) Uani 1 1 d U . .
O2 O 0.3124(11) -0.0057(11) 0.8695(9) 0.179(6) Uani 1 1 d U . .
O3 O 0.2340(14) -0.1072(12) 0.8972(10) 0.193(7) Uani 1 1 d U . .
C77 C 0.1385(15) 0.0320(14) 0.9084(11) 0.120(6) Uani 1 1 d U . .
F1 F 0.0461(9) 0.0427(8) 0.9039(7) 0.156(4) Uani 1 1 d U . .
F2 F 0.1571(11) 0.0167(10) 0.9841(8) 0.210(6) Uani 1 1 d U . .
F3 F 0.1233(9) 0.1179(9) 0.8848(8) 0.170(5) Uani 1 1 d U . .
C78 C 0.7054(11) 0.799(2) 0.1116(8) 0.29(2) Uani 1 1 d D . .
H78A H 0.7448 0.7431 0.1443 0.347 Uiso 1 1 calc R . .
H78B H 0.7177 0.8445 0.1302 0.347 Uiso 1 1 calc R . .
Cl3 Cl 0.7429(5) 0.8034(5) 0.0160(4) 0.181(3) Uani 1 1 d D . .
Cl4 Cl 0.5818(5) 0.8124(5) 0.1206(4) 0.202(3) Uani 1 1 d D . .
C79 C 0.1947(12) 0.6355(7) 0.2021(7) 0.186(13) Uani 1 1 d D . .
H79A H 0.2302 0.6234 0.1547 0.223 Uiso 1 1 calc R . .
H79B H 0.1486 0.6038 0.2130 0.223 Uiso 1 1 calc R . .
Cl5 Cl 0.1299(4) 0.7469(4) 0.1897(4) 0.163(2) Uani 1 1 d D . .
Cl6 Cl 0.2797(5) 0.6026(4) 0.2813(4) 0.178(3) Uani 1 1 d D . .
C80 C 0.5414(14) 0.514(2) 0.4030(10) 0.252(15) Uani 1 1 d DU . .
H80A H 0.4857 0.5635 0.4141 0.302 Uiso 1 1 calc R . .
H80B H 0.5201 0.4649 0.4066 0.302 Uiso 1 1 calc R . .
Cl7 Cl 0.6434(6) 0.4881(5) 0.4628(6) 0.215(3) Uani 1 1 d D . .
Cl8 Cl 0.5929(6) 0.5414(9) 0.3139(8) 0.330(7) Uani 1 1 d D . .
C81 C 0.783(4) 0.5866(18) 0.0651(13) 0.25(3) Uani 0.599(5) 1 d PD A 1
H81A H 0.8483 0.5909 0.0556 0.303 Uiso 0.599(5) 1 calc PR A 1
H81B H 0.7353 0.6326 0.0271 0.303 Uiso 0.599(5) 1 calc PR A 1
Cl9 Cl 0.7844(11) 0.4863(7) 0.0587(7) 0.191(5) Uani 0.599(5) 1 d PD A 1
Cl10 Cl 0.7471(10) 0.5945(5) 0.1581(5) 0.190(6) Uani 0.599(5) 1 d PD A 1
C82 C 0.776(3) 0.2771(15) 0.159(3) 0.14(2) Uani 0.401(5) 1 d PD A 2
H82A H 0.7094 0.2787 0.1749 0.170 Uiso 0.401(5) 1 calc PR A 2
H82B H 0.7918 0.2520 0.1133 0.170 Uiso 0.401(5) 1 calc PR A 2
Cl11 Cl 0.8585(6) 0.2091(6) 0.2335(5) 0.086(3) Uani 0.401(5) 1 d PD A 2
Cl12 Cl 0.7742(13) 0.3829(9) 0.1320(9) 0.165(6) Uani 0.401(5) 1 d PD A 2


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N13 2.121(11) . ?
Ni1 N1 2.139(9) . ?
Ni1 N5 2.144(11) . ?
Ni1 Ni2 2.3378(18) . ?
Ni1 Cl1 2.405(3) . ?
Ni2 N6 1.995(9) . ?
Ni2 N14 2.025(9) . ?
Ni2 N2 2.026(7) . ?
Ni2 Ni3 2.3619(16) . ?
Ni3 N11 1.882(7) . ?
Ni3 N3 1.905(7) . ?
Ni3 N7 1.912(8) . ?
Ni3 N15 1.918(8) . ?
Ni3 Ni4 2.4329(16) . ?
Ni4 N8 2.085(8) . ?
Ni4 N16 2.086(8) . ?
Ni4 N12 2.100(8) . ?
Ni4 N4 2.110(7) . ?
Ni4 Cl2 2.350(3) . ?
N1 C1 1.320(13) . ?
N1 C5 1.370(12) . ?
N2 C8 1.326(11) . ?
N2 C5 1.360(12) . ?
N3 C8 1.364(11) . ?
N3 C9 1.380(11) . ?
N4 C13 1.343(11) . ?
N4 C9 1.354(11) . ?
N5 C20 1.356(14) . ?
N5 C24 1.392(14) . ?
N6 C27 1.344(13) . ?
N6 C24 1.372(13) . ?
N7 C27 1.378(12) . ?
N7 C28 1.388(11) . ?
N8 C28 1.334(11) . ?
N8 C32 1.367(11) . ?
N9 C39 1.36(3) . ?
N9 C43 1.36(5) . ?
N10 C46 1.32(6) . ?
N10 C43 1.38(5) . ?
N9' C39' 1.32(5) . ?
N9' C43' 1.42(8) . ?
N10' C46' 1.35(10) . ?
N10' C43' 1.35(8) . ?
N11 C46 1.36(4) . ?
N11 C47 1.377(12) . ?
N11 C46' 1.40(7) . ?
N12 C47 1.354(12) . ?
N12 C51 1.369(12) . ?
N13 C58 1.340(15) . ?
N13 C62 1.370(15) . ?
N14 C65 1.340(12) . ?
N14 C62 1.382(13) . ?
N15 C65 1.366(12) . ?
N15 C66 1.391(11) . ?
N16 C66 1.341(11) . ?
N16 C70 1.362(11) . ?
C1 C2 1.400(18) . ?
C2 C3 1.364(17) . ?
C3 C4 1.407(14) . ?
C4 C6 1.405(14) . ?
C4 C5 1.426(13) . ?
C6 C7 1.352(13) . ?
C7 C8 1.446(12) . ?
C9 C10 1.416(13) . ?
C10 C11 1.364(13) . ?
C11 C12 1.374(14) . ?
C12 C13 1.386(14) . ?
C12 C14 1.46(3) . ?
C12 C14' 1.55(4) . ?
C14 C19 1.42(3) . ?
C14 C15 1.43(3) . ?
C15 C16 1.46(3) . ?
C16 C17 1.36(4) . ?
C17 C18 1.45(4) . ?
C18 C19 1.37(3) . ?
C14' C15' 1.43(6) . ?
C14' C19' 1.48(6) . ?
C15' C16' 1.41(4) . ?
C16' C17' 1.35(6) . ?
C17' C18' 1.37(7) . ?
C18' C19' 1.40(5) . ?
C20 C21 1.38(2) . ?
C21 C22 1.318(19) . ?
C22 C23 1.385(15) . ?
C23 C24 1.388(16) . ?
C23 C25 1.411(16) . ?
C25 C26 1.353(15) . ?
C26 C27 1.441(15) . ?
C28 C29 1.397(13) . ?
C29 C30 1.390(14) . ?
C30 C31 1.402(14) . ?
C31 C32 1.380(13) . ?
C31 C33 1.465(14) . ?
C33 C38 1.377(17) . ?
C33 C34 1.414(16) . ?
C34 C35 1.382(17) . ?
C35 C36 1.36(2) . ?
C36 C37 1.42(2) . ?
C37 C38 1.400(17) . ?
C39 C40 1.37(3) . ?
C40 C41 1.37(3) . ?
C41 C42 1.42(3) . ?
C42 C43 1.38(4) . ?
C42 C44 1.41(3) . ?
C44 C45 1.32(4) . ?
C45 C46 1.47(5) . ?
C39' C40' 1.35(4) . ?
C40' C41' 1.38(4) . ?
C41' C42' 1.39(4) . ?
C42' C44' 1.35(5) . ?
C42' C43' 1.42(6) . ?
C44' C45' 1.44(7) . ?
C45' C46' 1.43(8) . ?
C47 C48 1.414(14) . ?
C48 C49 1.355(15) . ?
C49 C50 1.373(17) . ?
C50 C51 1.399(15) . ?
C50 C52 1.47(4) . ?
C50 C52' 1.65(6) . ?
C52 C53 1.39(4) . ?
C52 C57 1.41(3) . ?
C53 C54 1.41(3) . ?
C54 C55 1.40(4) . ?
C55 C56 1.24(5) . ?
C56 C57 1.48(3) . ?
C52' C53' 1.36(7) . ?
C52' C57' 1.47(5) . ?
C53' C54' 1.38(6) . ?
C54' C55' 1.60(7) . ?
C55' C56' 1.36(7) . ?
C56' C57' 1.32(5) . ?
C58 C59 1.37(2) . ?
C59 C60 1.37(2) . ?
C60 C61 1.455(18) . ?
C61 C62 1.385(18) . ?
C61 C63 1.407(19) . ?
C63 C64 1.372(16) . ?
C64 C65 1.416(15) . ?
C66 C67 1.413(12) . ?
C67 C68 1.385(13) . ?
C68 C69 1.377(13) . ?
C69 C70 1.406(13) . ?
C69 C71 1.498(13) . ?
C71 C76 1.386(15) . ?
C71 C72 1.401(14) . ?
C72 C73 1.401(15) . ?
C73 C74 1.287(17) . ?
C74 C75 1.398(17) . ?
C75 C76 1.378(15) . ?
S1 O3 1.347(18) . ?
S1 O1 1.409(9) . ?
S1 O2 1.520(17) . ?
S1 C77 1.66(2) . ?
C77 F1 1.30(2) . ?
C77 F2 1.34(2) . ?
C77 F3 1.37(2) . ?
C78 Cl4 1.739(10) . ?
C78 Cl3 1.754(10) . ?
C79 Cl5 1.770(9) . ?
C79 Cl6 1.792(10) . ?
C80 Cl7 1.750(10) . ?
C80 Cl8 1.751(10) . ?
C81 Cl10 1.730(10) . ?
C81 Cl9 1.742(10) . ?
C82 Cl11 1.747(10) . ?
C82 Cl12 1.755(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
N13 Ni1 N1 88.2(4) . . ?
N13 Ni1 N5 168.9(3) . . ?
N1 Ni1 N5 92.1(3) . . ?
N13 Ni1 Ni2 84.2(3) . . ?
N1 Ni1 Ni2 84.2(2) . . ?
N5 Ni1 Ni2 84.8(2) . . ?
N13 Ni1 Cl1 96.8(3) . . ?
N1 Ni1 Cl1 95.8(2) . . ?
N5 Ni1 Cl1 94.2(3) . . ?
Ni2 Ni1 Cl1 178.97(14) . . ?
N6 Ni2 N14 173.4(3) . . ?
N6 Ni2 N2 91.5(3) . . ?
N14 Ni2 N2 88.1(3) . . ?
N6 Ni2 Ni1 92.8(2) . . ?
N14 Ni2 Ni1 93.7(2) . . ?
N2 Ni2 Ni1 93.5(2) . . ?
N6 Ni2 Ni3 87.4(2) . . ?
N14 Ni2 Ni3 86.0(2) . . ?
N2 Ni2 Ni3 86.5(2) . . ?
Ni1 Ni2 Ni3 179.73(9) . . ?
N11 Ni3 N3 177.7(3) . . ?
N11 Ni3 N7 90.0(3) . . ?
N3 Ni3 N7 90.8(3) . . ?
N11 Ni3 N15 89.3(3) . . ?
N3 Ni3 N15 89.8(3) . . ?
N7 Ni3 N15 178.9(3) . . ?
N11 Ni3 Ni2 89.0(2) . . ?
N3 Ni3 Ni2 88.9(2) . . ?
N7 Ni3 Ni2 89.0(2) . . ?
N15 Ni3 Ni2 90.1(2) . . ?
N11 Ni3 Ni4 90.0(2) . . ?
N3 Ni3 Ni4 92.2(2) . . ?
N7 Ni3 Ni4 90.1(2) . . ?
N15 Ni3 Ni4 90.8(2) . . ?
Ni2 Ni3 Ni4 178.65(6) . . ?
N8 Ni4 N16 164.8(3) . . ?
N8 Ni4 N12 87.5(3) . . ?
N16 Ni4 N12 88.0(3) . . ?
N8 Ni4 N4 93.0(3) . . ?
N16 Ni4 N4 87.7(3) . . ?
N12 Ni4 N4 165.2(3) . . ?
N8 Ni4 Cl2 96.4(2) . . ?
N16 Ni4 Cl2 98.6(2) . . ?
N12 Ni4 Cl2 98.6(2) . . ?
N4 Ni4 Cl2 96.1(2) . . ?
N8 Ni4 Ni3 82.3(2) . . ?
N16 Ni4 Ni3 82.7(2) . . ?
N12 Ni4 Ni3 83.2(2) . . ?
N4 Ni4 Ni3 82.24(19) . . ?
Cl2 Ni4 Ni3 177.79(10) . . ?
C1 N1 C5 117.9(10) . . ?
C1 N1 Ni1 119.1(8) . . ?
C5 N1 Ni1 123.0(6) . . ?
C8 N2 C5 121.1(8) . . ?
C8 N2 Ni2 119.4(6) . . ?
C5 N2 Ni2 118.3(6) . . ?
C8 N3 C9 122.2(7) . . ?
C8 N3 Ni3 118.4(6) . . ?
C9 N3 Ni3 119.3(6) . . ?
C13 N4 C9 117.7(8) . . ?
C13 N4 Ni4 120.3(6) . . ?
C9 N4 Ni4 121.9(6) . . ?
C20 N5 C24 114.4(11) . . ?
C20 N5 Ni1 122.1(9) . . ?
C24 N5 Ni1 122.4(7) . . ?
C27 N6 C24 117.3(10) . . ?
C27 N6 Ni2 120.1(7) . . ?
C24 N6 Ni2 122.6(8) . . ?
C27 N7 C28 122.1(8) . . ?
C27 N7 Ni3 119.5(7) . . ?
C28 N7 Ni3 117.7(6) . . ?
C28 N8 C32 118.3(8) . . ?
C28 N8 Ni4 122.5(6) . . ?
C32 N8 Ni4 118.7(6) . . ?
C39 N9 C43 118(2) . . ?
C46 N10 C43 120(4) . . ?
C39' N9' C43' 112(4) . . ?
C46' N10' C43' 121(6) . . ?
C46 N11 C47 121.5(19) . . ?
C46 N11 C46' 14(4) . . ?
C47 N11 C46' 119(3) . . ?
C46 N11 Ni3 119.3(19) . . ?
C47 N11 Ni3 119.2(6) . . ?
C46' N11 Ni3 120(3) . . ?
C47 N12 C51 118.5(8) . . ?
C47 N12 Ni4 120.5(6) . . ?
C51 N12 Ni4 120.7(6) . . ?
C58 N13 C62 115.9(12) . . ?
C58 N13 Ni1 120.3(10) . . ?
C62 N13 Ni1 123.5(7) . . ?
C65 N14 C62 120.2(10) . . ?
C65 N14 Ni2 120.9(6) . . ?
C62 N14 Ni2 118.2(8) . . ?
C65 N15 C66 122.5(8) . . ?
C65 N15 Ni3 118.7(7) . . ?
C66 N15 Ni3 118.8(6) . . ?
C66 N16 C70 120.1(8) . . ?
C66 N16 Ni4 122.7(6) . . ?
C70 N16 Ni4 117.2(6) . . ?
N1 C1 C2 123.1(11) . . ?
C3 C2 C1 119.8(11) . . ?
C2 C3 C4 119.8(11) . . ?
C6 C4 C3 126.0(10) . . ?
C6 C4 C5 117.4(9) . . ?
C3 C4 C5 116.6(10) . . ?
N2 C5 N1 116.1(8) . . ?
N2 C5 C4 121.1(9) . . ?
N1 C5 C4 122.7(9) . . ?
C7 C6 C4 120.6(9) . . ?
C6 C7 C8 119.8(8) . . ?
N2 C8 N3 117.2(8) . . ?
N2 C8 C7 119.9(8) . . ?
N3 C8 C7 122.6(8) . . ?
N4 C9 N3 117.0(8) . . ?
N4 C9 C10 120.0(8) . . ?
N3 C9 C10 122.9(8) . . ?
C11 C10 C9 119.7(9) . . ?
C10 C11 C12 121.1(9) . . ?
C11 C12 C13 116.0(9) . . ?
C11 C12 C14 114.0(13) . . ?
C13 C12 C14 128.8(14) . . ?
C11 C12 C14' 129.2(19) . . ?
C13 C12 C14' 112.7(17) . . ?
C14 C12 C14' 29.0(13) . . ?
N4 C13 C12 125.4(9) . . ?
C19 C14 C15 120(2) . . ?
C19 C14 C12 115.1(18) . . ?
C15 C14 C12 124(2) . . ?
C14 C15 C16 116(2) . . ?
C17 C16 C15 122(3) . . ?
C16 C17 C18 121(3) . . ?
C19 C18 C17 118(3) . . ?
C18 C19 C14 123(2) . . ?
C15' C14' C19' 119(4) . . ?
C15' C14' C12 115(3) . . ?
C19' C14' C12 126(3) . . ?
C16' C15' C14' 118(4) . . ?
C17' C16' C15' 119(4) . . ?
C16' C17' C18' 128(4) . . ?
C17' C18' C19' 116(4) . . ?
C18' C19' C14' 120(4) . . ?
N5 C20 C21 125.5(13) . . ?
C22 C21 C20 118.4(13) . . ?
C21 C22 C23 120.7(15) . . ?
C22 C23 C24 119.3(13) . . ?
C22 C23 C25 124.1(13) . . ?
C24 C23 C25 116.5(10) . . ?
N6 C24 C23 125.0(11) . . ?
N6 C24 N5 113.3(11) . . ?
C23 C24 N5 121.7(10) . . ?
C26 C25 C23 120.0(12) . . ?
C25 C26 C27 120.4(11) . . ?
N6 C27 N7 117.1(10) . . ?
N6 C27 C26 120.6(9) . . ?
N7 C27 C26 122.2(10) . . ?
N8 C28 N7 115.6(8) . . ?
N8 C28 C29 121.4(8) . . ?
N7 C28 C29 122.7(9) . . ?
C30 C29 C28 118.5(10) . . ?
C29 C30 C31 121.9(10) . . ?
C32 C31 C30 114.5(9) . . ?
C32 C31 C33 121.5(10) . . ?
C30 C31 C33 123.9(10) . . ?
N8 C32 C31 125.3(9) . . ?
C38 C33 C34 118.3(11) . . ?
C38 C33 C31 120.8(10) . . ?
C34 C33 C31 120.9(11) . . ?
C35 C34 C33 119.8(13) . . ?
C36 C35 C34 122.0(13) . . ?
C35 C36 C37 119.3(12) . . ?
C38 C37 C36 118.2(14) . . ?
C33 C38 C37 122.1(13) . . ?
N9 C39 C40 122(2) . . ?
C39 C40 C41 120.8(19) . . ?
C40 C41 C42 118.3(18) . . ?
C43 C42 C44 120(2) . . ?
C43 C42 C41 118(2) . . ?
C44 C42 C41 122.3(18) . . ?
N9 C43 C42 123(3) . . ?
N9 C43 N10 116(3) . . ?
C42 C43 N10 122(3) . . ?
C45 C44 C42 119(2) . . ?
C44 C45 C46 121(3) . . ?
N10 C46 N11 115(3) . . ?
N10 C46 C45 119(4) . . ?
N11 C46 C45 125(3) . . ?
N9' C39' C40' 131(4) . . ?
C39' C40' C41' 118(3) . . ?
C40' C41' C42' 118(3) . . ?
C44' C42' C41' 125(3) . . ?
C44' C42' C43' 116(3) . . ?
C41' C42' C43' 119(3) . . ?
N10' C43' N9' 115(5) . . ?
N10' C43' C42' 122(5) . . ?
N9' C43' C42' 122(5) . . ?
C42' C44' C45' 125(4) . . ?
C46' C45' C44' 114(5) . . ?
N10' C46' N11 121(5) . . ?
N10' C46' C45' 122(6) . . ?
N11 C46' C45' 117(5) . . ?
N12 C47 N11 115.8(8) . . ?
N12 C47 C48 120.1(10) . . ?
N11 C47 C48 123.9(9) . . ?
C49 C48 C47 120.7(11) . . ?
C48 C49 C50 119.8(11) . . ?
C49 C50 C51 118.5(10) . . ?
C49 C50 C52 115.4(14) . . ?
C51 C50 C52 125.7(14) . . ?
C49 C50 C52' 131(2) . . ?
C51 C50 C52' 109(2) . . ?
C52 C50 C52' 24.0(19) . . ?
N12 C51 C50 122.2(10) . . ?
C53 C52 C57 119(3) . . ?
C53 C52 C50 127.7(19) . . ?
C57 C52 C50 113(2) . . ?
C52 C53 C54 123(2) . . ?
C55 C54 C53 116(3) . . ?
C56 C55 C54 122(3) . . ?
C55 C56 C57 125(3) . . ?
C52 C57 C56 114(2) . . ?
C53' C52' C57' 121(5) . . ?
C53' C52' C50 111(3) . . ?
C57' C52' C50 128(4) . . ?
C52' C53' C54' 125(4) . . ?
C53' C54' C55' 112(4) . . ?
C56' C55' C54' 116(4) . . ?
C57' C56' C55' 128(4) . . ?
C56' C57' C52' 115(4) . . ?
N13 C58 C59 124.3(15) . . ?
C60 C59 C58 121.9(14) . . ?
C59 C60 C61 115.4(15) . . ?
C62 C61 C63 118.7(11) . . ?
C62 C61 C60 119.0(14) . . ?
C63 C61 C60 122.2(14) . . ?
N13 C62 N14 115.6(11) . . ?
N13 C62 C61 123.4(11) . . ?
N14 C62 C61 120.9(12) . . ?
C64 C63 C61 120.0(13) . . ?
C63 C64 C65 119.3(12) . . ?
N14 C65 N15 116.7(9) . . ?
N14 C65 C64 120.7(9) . . ?
N15 C65 C64 122.3(10) . . ?
N16 C66 N15 116.0(8) . . ?
N16 C66 C67 120.3(8) . . ?
N15 C66 C67 123.5(8) . . ?
C68 C67 C66 119.2(9) . . ?
C69 C68 C67 120.6(9) . . ?
C68 C69 C70 117.7(9) . . ?
C68 C69 C71 123.1(9) . . ?
C70 C69 C71 119.1(9) . . ?
N16 C70 C69 121.9(9) . . ?
C76 C71 C72 117.5(10) . . ?
C76 C71 C69 122.1(9) . . ?
C72 C71 C69 120.4(9) . . ?
C73 C72 C71 119.3(11) . . ?
C74 C73 C72 122.1(12) . . ?
C73 C74 C75 120.7(11) . . ?
C76 C75 C74 119.1(12) . . ?
C75 C76 C71 121.2(11) . . ?
O3 S1 O1 121.5(10) . . ?
O3 S1 O2 110.2(12) . . ?
O1 S1 O2 110.6(8) . . ?
O3 S1 C77 101.9(11) . . ?
O1 S1 C77 108.0(8) . . ?
O2 S1 C77 102.5(10) . . ?
F1 C77 F2 104.4(17) . . ?
F1 C77 F3 94.1(16) . . ?
F2 C77 F3 102.0(17) . . ?
F1 C77 S1 122.3(16) . . ?
F2 C77 S1 117.1(15) . . ?
F3 C77 S1 113.0(15) . . ?
Cl4 C78 Cl3 111.9(8) . . ?
Cl5 C79 Cl6 107.8(7) . . ?
Cl7 C80 Cl8 99.0(10) . . ?
Cl10 C81 Cl9 105.2(10) . . ?
Cl11 C82 Cl12 116.0(12) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.359
_refine_diff_density_min         -1.352
_refine_diff_density_rms         0.165
####################################################################### 
# 
# 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_ic17383
_database_code_depnum_ccdc_archive 'CCDC 1486166'
_audit_update_record             
;
2016-06-17 deposited with the CCDC.
2016-09-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C86 H73 B2 Cl12 F8 N16 Ni4'
_chemical_formula_weight         2164.46

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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   14.6577(9)
_cell_length_b                   35.883(2)
_cell_length_c                   17.1139(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.750(2)
_cell_angle_gamma                90.00
_cell_volume                     8997.1(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    36814
_cell_measurement_theta_min      1.13
_cell_measurement_theta_max      25.00

_exptl_crystal_description       needle
_exptl_crystal_colour            dark-red
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4396
_exptl_absorpt_coefficient_mu    1.253
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6341
_exptl_absorpt_correction_T_max  0.8849
_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  'NONIUS KappaCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            36814
_diffrn_reflns_av_R_equivalents  0.0823
_diffrn_reflns_av_sigmaI/netI    0.1199
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.13
_diffrn_reflns_theta_max         25.00
_reflns_number_total             15675
_reflns_number_gt                6932
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'NONIUS COLLECT'
_computing_cell_refinement       DENZO-SMN
_computing_data_reduction        DENZO-SMN
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.0920P)²+40.5360P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         15675
_refine_ls_number_parameters     1135
_refine_ls_number_restraints     145
_refine_ls_R_factor_all          0.2264
_refine_ls_R_factor_gt           0.1185
_refine_ls_wR_factor_ref         0.3467
_refine_ls_wR_factor_gt          0.2984
_refine_ls_goodness_of_fit_ref   1.410
_refine_ls_restrained_S_all      1.448
_refine_ls_shift/su_max          0.033
_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 0.26585(12) 0.26319(4) 0.23714(10) 0.0472(5) Uani 1 1 d . . .
Ni2 Ni 0.26222(11) 0.33071(4) 0.23776(9) 0.0369(4) Uani 1 1 d . . .
Ni3 Ni 0.25830(11) 0.39578(4) 0.23937(8) 0.0329(4) Uani 1 1 d . . .
Ni4 Ni 0.25477(10) 0.46336(4) 0.24275(8) 0.0312(4) Uani 1 1 d . . .
Cl1 Cl 0.2689(3) 0.19886(9) 0.2368(2) 0.0661(11) Uani 1 1 d . . .
Cl2 Cl 0.2523(2) 0.52796(7) 0.24473(16) 0.0361(7) Uani 1 1 d . . .
N1 N 0.1249(8) 0.2703(3) 0.2405(6) 0.048(3) Uani 1 1 d . . .
N2 N 0.1356(7) 0.3316(3) 0.2047(6) 0.040(3) Uani 1 1 d . . .
N3 N 0.1564(6) 0.3945(3) 0.1696(5) 0.034(2) Uani 1 1 d . . .
N4 N 0.1808(7) 0.4558(3) 0.1379(5) 0.034(2) Uani 1 1 d . . .
N5 N 0.2575(7) 0.2710(3) 0.1165(6) 0.051(3) Uani 1 1 d . . .
N6 N 0.3004(7) 0.3328(3) 0.1330(6) 0.040(3) Uani 1 1 d . . .
N7 N 0.3395(7) 0.3948(3) 0.1552(6) 0.043(3) Uani 1 1 d . . .
N8 N 0.3778(6) 0.4571(3) 0.1804(5) 0.032(2) Uani 1 1 d . . .
N9 N 0.4063(7) 0.2715(3) 0.2347(6) 0.048(3) Uani 1 1 d . . .
N10 N 0.3888(7) 0.3338(3) 0.2732(5) 0.041(3) Uani 1 1 d . . .
N11 N 0.3606(7) 0.3944(3) 0.3100(5) 0.036(2) Uani 1 1 d . . .
N12 N 0.3299(6) 0.4551(3) 0.3472(5) 0.034(2) Uani 1 1 d . . .
N13 N 0.2785(8) 0.2706(3) 0.3587(6) 0.053(3) Uani 1 1 d . . .
N14 N 0.2243(7) 0.3310(3) 0.3444(5) 0.041(3) Uani 1 1 d . . .
N15 N 0.1787(7) 0.3928(2) 0.3229(5) 0.034(2) Uani 1 1 d . . .
N16 N 0.1353(6) 0.4545(3) 0.3063(5) 0.032(2) Uani 1 1 d . . .
C1 C 0.0722(11) 0.2405(4) 0.2593(9) 0.064(4) Uani 1 1 d . . .
H1 H 0.1006 0.2194 0.2801 0.077 Uiso 1 1 calc R . .
C2 C -0.0199(11) 0.2403(4) 0.2491(9) 0.061(4) Uani 1 1 d . . .
H2 H -0.0528 0.2193 0.2627 0.073 Uiso 1 1 calc R . .
C3 C -0.0664(10) 0.2717(4) 0.2180(8) 0.057(4) Uani 1 1 d . . .
H3 H -0.1293 0.2717 0.2094 0.068 Uiso 1 1 calc R . .
C4 C -0.0128(10) 0.3028(4) 0.2008(8) 0.050(4) Uani 1 1 d . . .
C5 C 0.0816(9) 0.3016(3) 0.2146(7) 0.040(3) Uani 1 1 d . . .
C6 C -0.0514(10) 0.3363(4) 0.1739(8) 0.056(4) Uani 1 1 d . . .
H6 H -0.1142 0.3382 0.1656 0.067 Uiso 1 1 calc R . .
C7 C 0.0041(10) 0.3667(4) 0.1595(7) 0.051(4) Uani 1 1 d . . .
H7 H -0.0215 0.3886 0.1397 0.061 Uiso 1 1 calc R . .
C8 C 0.1006(9) 0.3647(4) 0.1749(7) 0.045(3) Uani 1 1 d . . .
C9 C 0.1383(8) 0.4231(3) 0.1189(7) 0.036(3) Uani 1 1 d . . .
C10 C 0.0898(9) 0.4201(4) 0.0482(7) 0.048(4) Uani 1 1 d . . .
H10 H 0.0599 0.3980 0.0355 0.057 Uiso 1 1 calc R . .
C11 C 0.0856(9) 0.4504(4) -0.0047(7) 0.052(4) Uani 1 1 d . . .
H11 H 0.0523 0.4484 -0.0516 0.062 Uiso 1 1 calc R . .
C12 C 0.1323(9) 0.4836(4) 0.0146(7) 0.045(3) Uani 1 1 d . . .
C13 C 0.1769(8) 0.4845(3) 0.0863(6) 0.036(3) Uani 1 1 d . . .
H13 H 0.2068 0.5064 0.1006 0.043 Uiso 1 1 calc R . .
C14 C 0.1401(9) 0.5142(4) -0.0413(6) 0.041(3) Uani 1 1 d . . .
C15 C 0.1412(11) 0.5074(4) -0.1215(8) 0.067(4) Uani 1 1 d . . .
H15 H 0.1309 0.4833 -0.1400 0.081 Uiso 1 1 calc R . .
C16 C 0.1576(11) 0.5367(5) -0.1755(8) 0.072(5) Uani 1 1 d . . .
H16A H 0.2073 0.5288 -0.2079 0.086 Uiso 1 1 calc R . .
H16B H 0.1038 0.5389 -0.2096 0.086 Uiso 1 1 calc R . .
C17 C 0.1781(10) 0.5710(4) -0.1482(9) 0.061(4) Uani 1 1 d . . .
H17 H 0.1906 0.5899 -0.1834 0.073 Uiso 1 1 calc R . .
C18 C 0.1807(10) 0.5786(4) -0.0690(8) 0.059(4) Uani 1 1 d . . .
H18 H 0.1953 0.6024 -0.0510 0.070 Uiso 1 1 calc R . .
C19 C 0.1615(10) 0.5505(4) -0.0169(8) 0.056(4) Uani 1 1 d . . .
H19 H 0.1627 0.5559 0.0362 0.067 Uiso 1 1 calc R . .
C20 C 0.2391(11) 0.2425(4) 0.0686(9) 0.064(4) Uani 1 1 d . . .
H20 H 0.2177 0.2206 0.0904 0.077 Uiso 1 1 calc R . .
C21 C 0.2497(11) 0.2434(4) -0.0125(9) 0.071(5) Uani 1 1 d . . .
H21 H 0.2322 0.2232 -0.0435 0.086 Uiso 1 1 calc R . .
C22 C 0.2870(11) 0.2753(4) -0.0456(9) 0.066(4) Uani 1 1 d . . .
H22 H 0.2989 0.2762 -0.0986 0.080 Uiso 1 1 calc R . .
C23 C 0.3059(11) 0.3055(4) 0.0022(8) 0.060(4) Uani 1 1 d . . .
C24 C 0.2854(9) 0.3031(3) 0.0825(8) 0.047(3) Uani 1 1 d . . .
C25 C 0.3442(10) 0.3395(4) -0.0239(8) 0.061(4) Uani 1 1 d . . .
H25 H 0.3577 0.3420 -0.0764 0.074 Uiso 1 1 calc R . .
C26 C 0.3616(10) 0.3682(4) 0.0250(7) 0.055(4) Uani 1 1 d . . .
H26 H 0.3905 0.3895 0.0072 0.066 Uiso 1 1 calc R . .
C27 C 0.3352(9) 0.3656(3) 0.1046(7) 0.041(3) Uani 1 1 d . . .
C28 C 0.4005(8) 0.4239(3) 0.1483(7) 0.035(3) Uani 1 1 d . . .
C29 C 0.4893(9) 0.4204(4) 0.1167(7) 0.050(4) Uani 1 1 d . . .
H29 H 0.5084 0.3977 0.0965 0.060 Uiso 1 1 calc R . .
C30 C 0.5452(9) 0.4503(4) 0.1165(8) 0.050(4) Uani 1 1 d . . .
H30 H 0.6033 0.4480 0.0967 0.060 Uiso 1 1 calc R . .
C31 C 0.5176(8) 0.4841(3) 0.1452(7) 0.038(3) Uani 1 1 d . . .
C32 C 0.4338(8) 0.4857(3) 0.1778(6) 0.036(3) Uani 1 1 d . . .
H32 H 0.4153 0.5082 0.1993 0.043 Uiso 1 1 calc R . .
C33 C 0.5781(8) 0.5175(4) 0.1430(8) 0.046(3) Uani 1 1 d . . .
C34 C 0.6342(10) 0.5244(4) 0.0811(9) 0.067(4) Uani 1 1 d . . .
H34 H 0.6346 0.5083 0.0385 0.080 Uiso 1 1 calc R . .
C35 C 0.6907(11) 0.5560(4) 0.0834(12) 0.080(6) Uani 1 1 d . . .
H35 H 0.7293 0.5603 0.0421 0.096 Uiso 1 1 calc R . .
C36 C 0.6908(10) 0.5798(4) 0.1421(12) 0.079(6) Uani 1 1 d . . .
H36 H 0.7283 0.6007 0.1406 0.095 Uiso 1 1 calc R . .
C37 C 0.6341(10) 0.5742(4) 0.2085(9) 0.061(4) Uani 1 1 d . . .
H37 H 0.6347 0.5908 0.2503 0.073 Uiso 1 1 calc R . .
C38 C 0.5791(9) 0.5432(4) 0.2070(8) 0.053(4) Uani 1 1 d . . .
H38 H 0.5415 0.5387 0.2488 0.063 Uiso 1 1 calc R . .
C39 C 0.4636(10) 0.2427(4) 0.2208(8) 0.052(4) Uani 1 1 d . . .
H39 H 0.4385 0.2206 0.2017 0.062 Uiso 1 1 calc R . .
C40 C 0.5565(11) 0.2444(4) 0.2333(9) 0.063(4) Uani 1 1 d . . .
H40 H 0.5928 0.2242 0.2205 0.075 Uiso 1 1 calc R . .
C41 C 0.5962(10) 0.2766(3) 0.2652(8) 0.055(4) Uani 1 1 d . . .
H41 H 0.6585 0.2776 0.2770 0.066 Uiso 1 1 calc R . .
C42 C 0.5407(9) 0.3069(4) 0.2788(8) 0.046(3) Uani 1 1 d . . .
C43 C 0.4470(10) 0.3042(3) 0.2612(7) 0.048(3) Uani 1 1 d . . .
C44 C 0.5743(9) 0.3420(4) 0.3058(7) 0.050(4) Uani 1 1 d . . .
H44 H 0.6368 0.3457 0.3131 0.060 Uiso 1 1 calc R . .
C45 C 0.5151(10) 0.3706(4) 0.3212(8) 0.051(4) Uani 1 1 d . . .
H45 H 0.5369 0.3926 0.3436 0.061 Uiso 1 1 calc R . .
C46 C 0.4209(9) 0.3664(3) 0.3028(7) 0.040(3) Uani 1 1 d . . .
C47 C 0.3720(8) 0.4227(3) 0.3632(7) 0.032(3) Uani 1 1 d . . .
C48 C 0.4168(9) 0.4178(3) 0.4357(7) 0.049(4) Uani 1 1 d . . .
H48 H 0.4453 0.3952 0.4477 0.059 Uiso 1 1 calc R . .
C49 C 0.4188(9) 0.4473(3) 0.4911(7) 0.046(3) Uani 1 1 d . . .
H49 H 0.4521 0.4450 0.5380 0.055 Uiso 1 1 calc R . .
C50 C 0.3692(8) 0.4802(3) 0.4738(6) 0.036(3) Uani 1 1 d . . .
C51 C 0.3281(8) 0.4825(3) 0.4013(7) 0.033(3) Uani 1 1 d . . .
H51 H 0.2969 0.5043 0.3882 0.039 Uiso 1 1 calc R . .
C52 C 0.3587(8) 0.5098(3) 0.5334(7) 0.037(3) Uani 1 1 d . . .
C53 C 0.3576(11) 0.5011(4) 0.6120(7) 0.066(4) Uani 1 1 d . . .
H53 H 0.3717 0.4770 0.6282 0.079 Uiso 1 1 calc R . .
C54 C 0.3356(12) 0.5281(4) 0.6678(8) 0.072(5) Uani 1 1 d . . .
H54 H 0.3359 0.5218 0.7206 0.086 Uiso 1 1 calc R . .
C55 C 0.3139(10) 0.5631(4) 0.6448(8) 0.056(4) Uani 1 1 d . . .
H55 H 0.2984 0.5809 0.6815 0.067 Uiso 1 1 calc R . .
C56 C 0.3150(10) 0.5720(4) 0.5664(8) 0.056(4) Uani 1 1 d . . .
H56 H 0.3007 0.5961 0.5502 0.067 Uiso 1 1 calc R . .
C57 C 0.3376(9) 0.5452(4) 0.5111(8) 0.052(4) Uani 1 1 d . . .
H57 H 0.3382 0.5516 0.4585 0.062 Uiso 1 1 calc R . .
C58 C 0.3026(12) 0.2427(4) 0.4042(10) 0.074(5) Uani 1 1 d . . .
H58 H 0.3244 0.2212 0.3809 0.089 Uiso 1 1 calc R . .
C59 C 0.2973(13) 0.2434(4) 0.4861(9) 0.083(6) Uani 1 1 d . . .
H59 H 0.3178 0.2234 0.5162 0.100 Uiso 1 1 calc R . .
C60 C 0.2616(12) 0.2740(4) 0.5200(10) 0.081(5) Uani 1 1 d . . .
H60 H 0.2556 0.2750 0.5739 0.097 Uiso 1 1 calc R . .
C61 C 0.2340(11) 0.3041(4) 0.4737(8) 0.059(4) Uani 1 1 d . . .
C62 C 0.2452(9) 0.3018(3) 0.3931(7) 0.045(3) Uani 1 1 d . . .
C63 C 0.1905(10) 0.3366(4) 0.5025(8) 0.057(4) Uani 1 1 d . . .
H63 H 0.1792 0.3385 0.5555 0.068 Uiso 1 1 calc R . .
C64 C 0.1657(10) 0.3646(4) 0.4542(7) 0.052(4) Uani 1 1 d . . .
H64 H 0.1344 0.3850 0.4736 0.062 Uiso 1 1 calc R . .
C65 C 0.1873(9) 0.3634(3) 0.3724(7) 0.041(3) Uani 1 1 d . . .
C66 C 0.1130(8) 0.4203(3) 0.3330(6) 0.034(3) Uani 1 1 d . . .
C67 C 0.0301(9) 0.4142(3) 0.3662(7) 0.042(3) Uani 1 1 d . . .
H67 H 0.0145 0.3904 0.3822 0.050 Uiso 1 1 calc R . .
C68 C -0.0302(9) 0.4433(4) 0.3759(7) 0.044(3) Uani 1 1 d . . .
H68 H -0.0864 0.4389 0.3979 0.052 Uiso 1 1 calc R . .
C69 C -0.0071(8) 0.4791(3) 0.3527(6) 0.036(3) Uani 1 1 d . . .
C70 C 0.0755(7) 0.4826(3) 0.3162(6) 0.030(3) Uani 1 1 d . . .
H70 H 0.0908 0.5059 0.2971 0.036 Uiso 1 1 calc R . .
C71 C -0.0671(8) 0.5109(3) 0.3644(7) 0.041(3) Uani 1 1 d . . .
C72 C -0.1111(10) 0.5157(4) 0.4335(9) 0.062(4) Uani 1 1 d . . .
H72 H -0.1030 0.4985 0.4736 0.075 Uiso 1 1 calc R . .
C73 C -0.1679(10) 0.5464(4) 0.4436(10) 0.071(5) Uani 1 1 d . . .
H73 H -0.1983 0.5491 0.4902 0.085 Uiso 1 1 calc R . .
C74 C -0.1795(10) 0.5724(4) 0.3867(10) 0.063(4) Uani 1 1 d . . .
H74 H -0.2175 0.5927 0.3943 0.076 Uiso 1 1 calc R . .
C75 C -0.1359(10) 0.5686(4) 0.3190(10) 0.063(4) Uani 1 1 d . . .
H75 H -0.1435 0.5866 0.2801 0.076 Uiso 1 1 calc R . .
C76 C -0.0797(9) 0.5382(4) 0.3071(8) 0.054(4) Uani 1 1 d . . .
H76 H -0.0499 0.5360 0.2601 0.064 Uiso 1 1 calc R . .
B1 B 0.8286(12) 0.3357(4) 0.3576(10) 0.051(4) Uani 1 1 d . . .
F1 F 0.7975(6) 0.3024(3) 0.3305(6) 0.091(3) Uani 1 1 d . . .
F2 F 0.7788(7) 0.3443(2) 0.4211(5) 0.087(3) Uani 1 1 d . . .
F3 F 0.9184(7) 0.3347(3) 0.3732(6) 0.100(3) Uani 1 1 d . . .
F4 F 0.8100(9) 0.3626(3) 0.3011(7) 0.134(4) Uani 1 1 d U . .
B2 B 0.2685(12) 0.3239(5) 0.7347(12) 0.057(5) Uani 1 1 d . . .
F5 F 0.2622(6) 0.2874(3) 0.7155(6) 0.095(3) Uani 1 1 d . . .
F6 F 0.3378(8) 0.3291(3) 0.7882(6) 0.100(3) Uani 1 1 d . . .
F7 F 0.2915(12) 0.3463(4) 0.6761(7) 0.172(7) Uani 1 1 d . . .
F8 F 0.1914(11) 0.3364(4) 0.7607(10) 0.172(6) Uani 1 1 d U . .
C77 C 0.6820(12) 0.3945(5) 0.8787(10) 0.112(7) Uani 1 1 d DU . .
H77A H 0.7383 0.4074 0.8680 0.135 Uiso 1 1 calc R . .
H77B H 0.6968 0.3722 0.9087 0.135 Uiso 1 1 calc R . .
C78 C 0.6328(12) 0.3840(6) 0.8027(11) 0.131(8) Uani 1 1 d DU . .
H78A H 0.6743 0.3711 0.7688 0.157 Uiso 1 1 calc R . .
H78B H 0.6107 0.4062 0.7761 0.157 Uiso 1 1 calc R . .
Cl3 Cl 0.6097(4) 0.42373(16) 0.9325(3) 0.1143(18) Uani 1 1 d DU . .
Cl4 Cl 0.5413(5) 0.35495(19) 0.8241(5) 0.163(3) Uani 1 1 d DU . .
C79 C 0.4108(14) 0.1304(8) 0.1749(13) 0.200 Uiso 1 1 d D . .
H79A H 0.4338 0.1102 0.2074 0.240 Uiso 1 1 calc R . .
H79B H 0.3780 0.1475 0.2080 0.240 Uiso 1 1 calc R . .
C80 C 0.3445(14) 0.1146(5) 0.1109(13) 0.133(8) Uani 1 1 d DU . .
H80A H 0.3358 0.1326 0.0689 0.160 Uiso 1 1 calc R . .
H80B H 0.2856 0.1093 0.1327 0.160 Uiso 1 1 calc R . .
Cl5 Cl 0.5027(4) 0.15389(15) 0.1342(3) 0.1138(18) Uani 1 1 d DU . .
Cl6 Cl 0.3924(5) 0.07443(16) 0.0758(4) 0.133(2) Uani 1 1 d DU . .
C81 C 0.9558(15) 0.3412(8) 0.9510(15) 0.214(4) Uani 1 1 d DU . .
H81A H 0.8975 0.3285 0.9510 0.256 Uiso 1 1 calc R . .
H81B H 0.9505 0.3644 0.9796 0.256 Uiso 1 1 calc R . .
C82 C 0.985(3) 0.3488(7) 0.8660(12) 0.345(8) Uani 1 1 d DU . .
H82A H 0.9524 0.3327 0.8293 0.415 Uiso 1 1 calc R . .
H82B H 1.0502 0.3448 0.8611 0.415 Uiso 1 1 calc R . .
Cl7 Cl 1.0449(7) 0.3122(3) 0.9947(6) 0.214(4) Uani 1 1 d DU . .
Cl8 Cl 0.9568(11) 0.3956(5) 0.8496(10) 0.345(8) Uani 1 1 d DU . .
C83 C 0.588(3) 0.3105(6) 0.0140(13) 0.31(2) Uani 1 1 d DU . .
H83A H 0.5415 0.3266 -0.0087 0.370 Uiso 1 1 calc R . .
H83B H 0.6312 0.3047 -0.0264 0.370 Uiso 1 1 calc R . .
C84 C 0.545(2) 0.2749(7) 0.0422(11) 0.258(19) Uani 1 1 d DU . .
H84A H 0.4906 0.2811 0.0703 0.309 Uiso 1 1 calc R . .
H84B H 0.5872 0.2625 0.0785 0.309 Uiso 1 1 calc R . .
Cl9 Cl 0.6464(8) 0.3342(3) 0.0916(7) 0.264(5) Uani 1 1 d DU . .
Cl10 Cl 0.5155(8) 0.2439(3) -0.0340(7) 0.269(5) Uani 1 1 d DU . .
C85 C 0.508(2) 0.3305(8) 0.5769(10) 0.27(2) Uani 1 1 d DU . .
H85A H 0.4510 0.3421 0.5919 0.328 Uiso 1 1 calc R . .
H85B H 0.5246 0.3118 0.6155 0.328 Uiso 1 1 calc R . .
C86 C 0.5844(13) 0.3603(5) 0.5711(10) 0.119(7) Uani 1 1 d DU . .
H86A H 0.5855 0.3706 0.5187 0.143 Uiso 1 1 calc R . .
H86B H 0.6436 0.3494 0.5838 0.143 Uiso 1 1 calc R . .
Cl11 Cl 0.4948(7) 0.3102(3) 0.4836(6) 0.222(4) Uani 1 1 d DU . .
Cl12 Cl 0.5587(9) 0.3938(3) 0.6367(8) 0.281(6) Uani 1 1 d DU . .


_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 N9 2.081(11) . ?
Ni1 N5 2.083(11) . ?
Ni1 N1 2.084(11) . ?
Ni1 N13 2.100(11) . ?
Ni1 Cl1 2.309(4) . ?
Ni1 Ni2 2.423(2) . ?
Ni2 N6 1.896(10) . ?
Ni2 N2 1.923(10) . ?
Ni2 N14 1.924(9) . ?
Ni2 N10 1.937(11) . ?
Ni2 Ni3 2.336(2) . ?
Ni3 N15 1.875(9) . ?
Ni3 N3 1.884(10) . ?
Ni3 N11 1.898(10) . ?
Ni3 N7 1.897(9) . ?
Ni3 Ni4 2.4263(19) . ?
Ni4 N4 2.086(9) . ?
Ni4 N12 2.092(9) . ?
Ni4 N16 2.114(9) . ?
Ni4 N8 2.135(9) . ?
Ni4 Cl2 2.319(3) . ?
N1 C5 1.359(15) . ?
N1 C1 1.363(16) . ?
N2 C5 1.351(14) . ?
N2 C8 1.384(15) . ?
N3 C8 1.351(16) . ?
N3 C9 1.366(14) . ?
N4 C13 1.357(14) . ?
N4 C9 1.362(14) . ?
N5 C20 1.333(15) . ?
N5 C24 1.361(15) . ?
N6 C27 1.380(15) . ?
N6 C24 1.383(15) . ?
N7 C27 1.357(14) . ?
N7 C28 1.383(14) . ?
N8 C32 1.317(13) . ?
N8 C28 1.357(13) . ?
N9 C39 1.358(15) . ?
N9 C43 1.387(16) . ?
N10 C46 1.356(15) . ?
N10 C43 1.380(15) . ?
N11 C46 1.344(14) . ?
N11 C47 1.372(14) . ?
N12 C47 1.340(13) . ?
N12 C51 1.350(13) . ?
N13 C58 1.311(17) . ?
N13 C62 1.360(15) . ?
N14 C62 1.368(15) . ?
N14 C65 1.376(14) . ?
N15 C65 1.358(14) . ?
N15 C66 1.392(14) . ?
N16 C70 1.349(13) . ?
N16 C66 1.354(13) . ?
C1 C2 1.356(19) . ?
C2 C3 1.41(2) . ?
C3 C4 1.401(17) . ?
C4 C5 1.397(18) . ?
C4 C6 1.403(18) . ?
C6 C7 1.387(17) . ?
C7 C8 1.432(18) . ?
C9 C10 1.389(16) . ?
C10 C11 1.413(18) . ?
C11 C12 1.410(17) . ?
C12 C13 1.373(16) . ?
C12 C14 1.463(16) . ?
C14 C15 1.393(17) . ?
C14 C19 1.401(17) . ?
C15 C16 1.426(19) . ?
C16 C17 1.347(19) . ?
C17 C18 1.382(18) . ?
C18 C19 1.379(18) . ?
C20 C21 1.401(19) . ?
C21 C22 1.396(19) . ?
C22 C23 1.379(18) . ?
C23 C24 1.418(18) . ?
C23 C25 1.422(18) . ?
C25 C26 1.347(17) . ?
C26 C27 1.430(16) . ?
C28 C29 1.430(16) . ?
C29 C30 1.350(17) . ?
C30 C31 1.375(16) . ?
C31 C32 1.367(15) . ?
C31 C33 1.492(17) . ?
C33 C34 1.384(17) . ?
C33 C38 1.431(18) . ?
C34 C35 1.41(2) . ?
C35 C36 1.32(2) . ?
C36 C37 1.44(2) . ?
C37 C38 1.375(18) . ?
C39 C40 1.372(19) . ?
C40 C41 1.398(19) . ?
C41 C42 1.381(17) . ?
C42 C43 1.401(18) . ?
C42 C44 1.426(18) . ?
C44 C45 1.373(17) . ?
C45 C46 1.414(18) . ?
C47 C48 1.397(16) . ?
C48 C49 1.423(16) . ?
C49 C50 1.414(16) . ?
C50 C51 1.365(15) . ?
C50 C52 1.482(15) . ?
C52 C57 1.359(16) . ?
C52 C53 1.381(17) . ?
C53 C54 1.404(18) . ?
C54 C55 1.351(18) . ?
C55 C56 1.381(18) . ?
C56 C57 1.396(17) . ?
C58 C59 1.41(2) . ?
C59 C60 1.35(2) . ?
C60 C61 1.390(19) . ?
C61 C62 1.396(17) . ?
C61 C63 1.425(18) . ?
C63 C64 1.345(17) . ?
C64 C65 1.445(16) . ?
C66 C67 1.375(16) . ?
C67 C68 1.380(16) . ?
C68 C69 1.389(16) . ?
C69 C70 1.385(15) . ?
C69 C71 1.458(16) . ?
C71 C72 1.376(17) . ?
C71 C76 1.395(17) . ?
C72 C73 1.392(18) . ?
C73 C74 1.36(2) . ?
C74 C75 1.35(2) . ?
C75 C76 1.386(18) . ?
B1 F3 1.336(19) . ?
B1 F1 1.354(18) . ?
B1 F2 1.363(17) . ?
B1 F4 1.389(17) . ?
B2 F8 1.31(2) . ?
B2 F7 1.34(2) . ?
B2 F5 1.354(18) . ?
B2 F6 1.36(2) . ?
C77 C78 1.515(10) . ?
C77 Cl3 1.769(9) . ?
C78 Cl4 1.746(10) . ?
C79 C80 1.550(10) . ?
C79 Cl5 1.751(10) . ?
C80 Cl6 1.720(9) . ?
C81 C82 1.553(10) . ?
C81 Cl7 1.814(10) . ?
C82 Cl8 1.752(10) . ?
C83 C84 1.514(10) . ?
C83 Cl9 1.773(10) . ?
C84 Cl10 1.757(10) . ?
C85 C86 1.557(10) . ?
C85 Cl11 1.761(10) . ?
C86 Cl12 1.697(9) . ?

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
N9 Ni1 N5 89.4(4) . . ?
N9 Ni1 N1 164.7(4) . . ?
N5 Ni1 N1 89.0(4) . . ?
N9 Ni1 N13 86.8(4) . . ?
N5 Ni1 N13 164.8(4) . . ?
N1 Ni1 N13 90.9(4) . . ?
N9 Ni1 Cl1 97.1(3) . . ?
N5 Ni1 Cl1 97.6(3) . . ?
N1 Ni1 Cl1 98.1(3) . . ?
N13 Ni1 Cl1 97.4(3) . . ?
N9 Ni1 Ni2 83.0(3) . . ?
N5 Ni1 Ni2 82.5(3) . . ?
N1 Ni1 Ni2 81.7(3) . . ?
N13 Ni1 Ni2 82.5(3) . . ?
Cl1 Ni1 Ni2 179.83(15) . . ?
N6 Ni2 N2 91.8(4) . . ?
N6 Ni2 N14 177.5(4) . . ?
N2 Ni2 N14 88.5(4) . . ?
N6 Ni2 N10 89.2(4) . . ?
N2 Ni2 N10 175.6(4) . . ?
N14 Ni2 N10 90.3(4) . . ?
N6 Ni2 Ni3 88.9(3) . . ?
N2 Ni2 Ni3 87.8(3) . . ?
N14 Ni2 Ni3 88.6(3) . . ?
N10 Ni2 Ni3 87.9(3) . . ?
N6 Ni2 Ni1 91.6(3) . . ?
N2 Ni2 Ni1 92.1(3) . . ?
N14 Ni2 Ni1 90.9(3) . . ?
N10 Ni2 Ni1 92.1(3) . . ?
Ni3 Ni2 Ni1 179.55(9) . . ?
N15 Ni3 N3 89.0(4) . . ?
N15 Ni3 N11 90.6(4) . . ?
N3 Ni3 N11 177.0(4) . . ?
N15 Ni3 N7 175.7(4) . . ?
N3 Ni3 N7 91.3(4) . . ?
N11 Ni3 N7 88.9(4) . . ?
N15 Ni3 Ni2 88.2(3) . . ?
N3 Ni3 Ni2 89.2(3) . . ?
N11 Ni3 Ni2 87.8(3) . . ?
N7 Ni3 Ni2 87.5(3) . . ?
N15 Ni3 Ni4 91.4(3) . . ?
N3 Ni3 Ni4 91.3(3) . . ?
N11 Ni3 Ni4 91.7(3) . . ?
N7 Ni3 Ni4 93.0(3) . . ?
Ni2 Ni3 Ni4 179.29(10) . . ?
N4 Ni4 N12 164.3(3) . . ?
N4 Ni4 N16 90.4(4) . . ?
N12 Ni4 N16 87.8(3) . . ?
N4 Ni4 N8 88.9(3) . . ?
N12 Ni4 N8 88.9(3) . . ?
N16 Ni4 N8 165.2(4) . . ?
N4 Ni4 Cl2 97.8(3) . . ?
N12 Ni4 Cl2 97.9(3) . . ?
N16 Ni4 Cl2 97.4(3) . . ?
N8 Ni4 Cl2 97.3(3) . . ?
N4 Ni4 Ni3 81.9(3) . . ?
N12 Ni4 Ni3 82.4(3) . . ?
N16 Ni4 Ni3 83.2(3) . . ?
N8 Ni4 Ni3 82.1(3) . . ?
Cl2 Ni4 Ni3 179.36(11) . . ?
C5 N1 C1 117.5(13) . . ?
C5 N1 Ni1 123.1(8) . . ?
C1 N1 Ni1 118.8(10) . . ?
C5 N2 C8 121.1(11) . . ?
C5 N2 Ni2 120.9(9) . . ?
C8 N2 Ni2 117.9(9) . . ?
C8 N3 C9 122.1(11) . . ?
C8 N3 Ni3 116.6(8) . . ?
C9 N3 Ni3 121.2(8) . . ?
C13 N4 C9 119.2(10) . . ?
C13 N4 Ni4 118.1(8) . . ?
C9 N4 Ni4 122.7(8) . . ?
C20 N5 C24 116.4(12) . . ?
C20 N5 Ni1 120.8(10) . . ?
C24 N5 Ni1 121.9(8) . . ?
C27 N6 C24 119.3(10) . . ?
C27 N6 Ni2 119.3(8) . . ?
C24 N6 Ni2 121.0(8) . . ?
C27 N7 C28 123.0(10) . . ?
C27 N7 Ni3 118.8(8) . . ?
C28 N7 Ni3 118.2(8) . . ?
C32 N8 C28 120.7(10) . . ?
C32 N8 Ni4 118.0(7) . . ?
C28 N8 Ni4 121.1(8) . . ?
C39 N9 C43 116.0(12) . . ?
C39 N9 Ni1 120.8(9) . . ?
C43 N9 Ni1 122.1(9) . . ?
C46 N10 C43 120.7(12) . . ?
C46 N10 Ni2 119.0(8) . . ?
C43 N10 Ni2 120.0(9) . . ?
C46 N11 C47 123.1(10) . . ?
C46 N11 Ni3 118.1(8) . . ?
C47 N11 Ni3 118.7(8) . . ?
C47 N12 C51 120.6(10) . . ?
C47 N12 Ni4 121.6(8) . . ?
C51 N12 Ni4 117.5(8) . . ?
C58 N13 C62 117.6(12) . . ?
C58 N13 Ni1 120.3(10) . . ?
C62 N13 Ni1 120.8(8) . . ?
C62 N14 C65 121.3(10) . . ?
C62 N14 Ni2 120.6(8) . . ?
C65 N14 Ni2 117.6(8) . . ?
C65 N15 C66 121.6(10) . . ?
C65 N15 Ni3 118.1(8) . . ?
C66 N15 Ni3 120.3(7) . . ?
C70 N16 C66 118.0(10) . . ?
C70 N16 Ni4 120.3(7) . . ?
C66 N16 Ni4 121.5(8) . . ?
C2 C1 N1 122.9(15) . . ?
C1 C2 C3 120.8(14) . . ?
C4 C3 C2 116.5(14) . . ?
C5 C4 C3 120.0(13) . . ?
C5 C4 C6 118.0(12) . . ?
C3 C4 C6 122.0(14) . . ?
N2 C5 N1 115.5(12) . . ?
N2 C5 C4 122.4(12) . . ?
N1 C5 C4 122.1(11) . . ?
C7 C6 C4 120.0(14) . . ?
C6 C7 C8 120.5(14) . . ?
N3 C8 N2 118.9(12) . . ?
N3 C8 C7 123.0(12) . . ?
N2 C8 C7 117.7(12) . . ?
N4 C9 N3 114.6(10) . . ?
N4 C9 C10 119.6(11) . . ?
N3 C9 C10 125.4(11) . . ?
C9 C10 C11 120.6(12) . . ?
C12 C11 C10 119.3(12) . . ?
C13 C12 C11 116.3(11) . . ?
C13 C12 C14 121.5(12) . . ?
C11 C12 C14 122.0(12) . . ?
N4 C13 C12 125.0(11) . . ?
C15 C14 C19 116.6(12) . . ?
C15 C14 C12 121.0(12) . . ?
C19 C14 C12 121.6(11) . . ?
C14 C15 C16 121.0(14) . . ?
C17 C16 C15 119.3(14) . . ?
C16 C17 C18 121.3(14) . . ?
C19 C18 C17 119.3(14) . . ?
C18 C19 C14 122.3(13) . . ?
N5 C20 C21 124.4(14) . . ?
C22 C21 C20 118.5(14) . . ?
C23 C22 C21 118.5(14) . . ?
C22 C23 C24 118.9(14) . . ?
C22 C23 C25 124.2(13) . . ?
C24 C23 C25 116.9(12) . . ?
N5 C24 N6 115.3(11) . . ?
N5 C24 C23 122.7(12) . . ?
N6 C24 C23 121.7(12) . . ?
C26 C25 C23 122.0(12) . . ?
C25 C26 C27 119.4(13) . . ?
N7 C27 N6 116.4(10) . . ?
N7 C27 C26 123.3(12) . . ?
N6 C27 C26 120.3(11) . . ?
N8 C28 N7 117.4(10) . . ?
N8 C28 C29 117.9(11) . . ?
N7 C28 C29 124.4(11) . . ?
C30 C29 C28 119.3(12) . . ?
C29 C30 C31 121.1(12) . . ?
C32 C31 C30 117.5(12) . . ?
C32 C31 C33 121.3(11) . . ?
C30 C31 C33 121.2(11) . . ?
N8 C32 C31 123.3(11) . . ?
C34 C33 C38 118.7(12) . . ?
C34 C33 C31 122.0(13) . . ?
C38 C33 C31 119.3(11) . . ?
C33 C34 C35 119.1(14) . . ?
C36 C35 C34 122.1(15) . . ?
C35 C36 C37 121.6(14) . . ?
C38 C37 C36 116.8(14) . . ?
C37 C38 C33 121.8(13) . . ?
N9 C39 C40 123.7(13) . . ?
C39 C40 C41 119.8(13) . . ?
C42 C41 C40 118.4(14) . . ?
C41 C42 C43 119.3(13) . . ?
C41 C42 C44 123.5(13) . . ?
C43 C42 C44 117.1(12) . . ?
N10 C43 N9 115.9(12) . . ?
N10 C43 C42 121.5(12) . . ?
N9 C43 C42 122.5(12) . . ?
C45 C44 C42 120.6(13) . . ?
C44 C45 C46 119.8(13) . . ?
N11 C46 N10 117.1(12) . . ?
N11 C46 C45 122.8(11) . . ?
N10 C46 C45 120.0(11) . . ?
N12 C47 N11 117.5(10) . . ?
N12 C47 C48 119.5(11) . . ?
N11 C47 C48 122.6(10) . . ?
C47 C48 C49 119.8(11) . . ?
C50 C49 C48 118.9(12) . . ?
C51 C50 C49 116.7(11) . . ?
C51 C50 C52 122.1(11) . . ?
C49 C50 C52 121.1(11) . . ?
N12 C51 C50 124.3(11) . . ?
C57 C52 C53 118.3(12) . . ?
C57 C52 C50 120.2(11) . . ?
C53 C52 C50 120.9(11) . . ?
C52 C53 C54 121.2(13) . . ?
C55 C54 C53 119.9(13) . . ?
C54 C55 C56 119.3(13) . . ?
C55 C56 C57 120.5(13) . . ?
C52 C57 C56 120.8(13) . . ?
N13 C58 C59 123.8(14) . . ?
C60 C59 C58 118.4(14) . . ?
C59 C60 C61 119.6(15) . . ?
C60 C61 C62 118.4(14) . . ?
C60 C61 C63 124.3(13) . . ?
C62 C61 C63 117.2(12) . . ?
N13 C62 N14 116.2(11) . . ?
N13 C62 C61 122.1(12) . . ?
N14 C62 C61 121.7(12) . . ?
C64 C63 C61 121.0(12) . . ?
C63 C64 C65 120.6(12) . . ?
N15 C65 N14 118.1(10) . . ?
N15 C65 C64 124.2(11) . . ?
N14 C65 C64 117.6(11) . . ?
N16 C66 C67 120.5(11) . . ?
N16 C66 N15 115.2(10) . . ?
C67 C66 N15 124.3(10) . . ?
C66 C67 C68 120.5(11) . . ?
C67 C68 C69 120.1(12) . . ?
C70 C69 C68 115.9(11) . . ?
C70 C69 C71 122.0(11) . . ?
C68 C69 C71 122.2(11) . . ?
N16 C70 C69 124.7(11) . . ?
C72 C71 C76 117.4(12) . . ?
C72 C71 C69 121.1(12) . . ?
C76 C71 C69 121.4(11) . . ?
C71 C72 C73 120.2(14) . . ?
C74 C73 C72 121.1(14) . . ?
C75 C74 C73 119.8(14) . . ?
C74 C75 C76 120.3(15) . . ?
C75 C76 C71 121.1(14) . . ?
F3 B1 F1 111.3(13) . . ?
F3 B1 F2 113.3(14) . . ?
F1 B1 F2 106.8(13) . . ?
F3 B1 F4 109.2(14) . . ?
F1 B1 F4 108.5(15) . . ?
F2 B1 F4 107.5(13) . . ?
F8 B2 F7 106.8(17) . . ?
F8 B2 F5 111.3(15) . . ?
F7 B2 F5 114.7(16) . . ?
F8 B2 F6 111.1(18) . . ?
F7 B2 F6 102.8(14) . . ?
F5 B2 F6 109.9(14) . . ?
C78 C77 Cl3 108.5(13) . . ?
C77 C78 Cl4 108.5(13) . . ?
C80 C79 Cl5 111.5(15) . . ?
C79 C80 Cl6 107.4(16) . . ?
C82 C81 Cl7 105.6(9) . . ?
C81 C82 Cl8 104.2(18) . . ?
C84 C83 Cl9 111.3(10) . . ?
C83 C84 Cl10 113.2(10) . . ?
C86 C85 Cl11 106.5(9) . . ?
C85 C86 Cl12 105.5(14) . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         2.254
_refine_diff_density_min         -1.561
_refine_diff_density_rms         0.175
####################################################################### 
# 
# 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_ic17195
_database_code_depnum_ccdc_archive 'CCDC 1486167'
_audit_update_record             
;
2016-06-17 deposited with the CCDC.
2016-09-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C84.50 H65 Cl8 N18 Ni4 O4 S2'
_chemical_formula_weight         1979.10

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 '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(1)/n

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

_cell_length_a                   14.7684(6)
_cell_length_b                   21.7310(10)
_cell_length_c                   26.4842(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.361(2)
_cell_angle_gamma                90.00
_cell_volume                     8386.4(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    36558
_cell_measurement_theta_min      1.22
_cell_measurement_theta_max      25.00

_exptl_crystal_description       needle
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4040
_exptl_absorpt_coefficient_mu    1.253
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5732
_exptl_absorpt_correction_T_max  0.9400
_exptl_absorpt_process_details   'SORTAV (Blessing, 1995)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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  'NONIUS KappaCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            36558
_diffrn_reflns_av_R_equivalents  0.0953
_diffrn_reflns_av_sigmaI/netI    0.1355
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.22
_diffrn_reflns_theta_max         25.00
_reflns_number_total             14696
_reflns_number_gt                7684
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'NONIUS COLLECT'
_computing_cell_refinement       DENZO-SMN
_computing_data_reduction        DENZO-SMN
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.1246P)²+15.1008P] 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         14696
_refine_ls_number_parameters     1086
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.1672
_refine_ls_R_factor_gt           0.0791
_refine_ls_wR_factor_ref         0.2496
_refine_ls_wR_factor_gt          0.2038
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.014
_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 0.76453(7) 0.20438(5) 0.01322(4) 0.0297(3) Uani 1 1 d . . .
Ni2 Ni 0.76581(7) 0.29595(5) 0.05906(4) 0.0252(3) Uani 1 1 d . . .
Ni3 Ni 0.76694(7) 0.38804(5) 0.10595(4) 0.0250(3) Uani 1 1 d . . .
Ni4 Ni 0.76926(7) 0.48252(5) 0.15363(4) 0.0266(3) Uani 1 1 d . . .
S1 S 0.8366(2) 0.03411(15) -0.08387(12) 0.0713(9) Uani 1 1 d . . .
S2 S 0.7573(3) 0.68608(14) 0.21138(13) 0.0836(11) Uani 1 1 d . . .
N1 N 0.8937(4) 0.1878(3) 0.0601(3) 0.0266(16) Uani 1 1 d . . .
N2 N 0.8670(4) 0.2669(3) 0.1148(2) 0.0276(16) Uani 1 1 d . . .
N3 N 0.8313(4) 0.3469(3) 0.1646(2) 0.0276(16) Uani 1 1 d . . .
N4 N 0.7865(4) 0.4250(3) 0.2163(2) 0.0249(16) Uani 1 1 d . . .
N5 N 0.8344(4) 0.2566(3) -0.0374(3) 0.0312(17) Uani 1 1 d . . .
N6 N 0.8613(4) 0.3347(3) 0.0225(2) 0.0243(15) Uani 1 1 d . . .
N7 N 0.8821(4) 0.4088(3) 0.0857(2) 0.0253(16) Uani 1 1 d . . .
N8 N 0.9079(4) 0.4812(3) 0.1517(2) 0.0269(16) Uani 1 1 d . . .
N9 N 0.6363(4) 0.2356(3) -0.0269(2) 0.0300(17) Uani 1 1 d . . .
N10 N 0.6628(4) 0.3335(3) 0.0085(2) 0.0241(15) Uani 1 1 d . . .
N11 N 0.7008(4) 0.4273(3) 0.0469(2) 0.0254(16) Uani 1 1 d . . .
N12 N 0.7510(4) 0.5219(3) 0.0812(2) 0.0263(16) Uani 1 1 d . . .
N13 N 0.7000(4) 0.1675(3) 0.0726(3) 0.0320(17) Uani 1 1 d . . .
N14 N 0.6733(4) 0.2654(3) 0.1013(2) 0.0264(16) Uani 1 1 d . . .
N15 N 0.6537(4) 0.3653(3) 0.1256(2) 0.0230(15) Uani 1 1 d . . .
N16 N 0.6295(4) 0.4677(3) 0.1456(2) 0.0265(16) Uani 1 1 d . . .
N17 N 0.7621(5) 0.1229(4) -0.0278(3) 0.0342(19) Uani 1 1 d . . .
N18 N 0.7695(4) 0.5624(4) 0.1928(3) 0.0317(17) Uani 1 1 d . . .
C1 C 0.9468(5) 0.1421(4) 0.0498(3) 0.031(2) Uani 1 1 d . . .
H1 H 0.9284 0.1201 0.0188 0.038 Uiso 1 1 calc R . .
C2 C 1.0280(6) 0.1235(4) 0.0807(4) 0.035(2) Uani 1 1 d . . .
H2 H 1.0634 0.0906 0.0705 0.041 Uiso 1 1 calc R . .
C3 C 1.0554(6) 0.1536(4) 0.1260(4) 0.038(2) Uani 1 1 d . . .
H3 H 1.1093 0.1412 0.1483 0.046 Uiso 1 1 calc R . .
C4 C 1.0022(5) 0.2032(4) 0.1389(3) 0.030(2) Uani 1 1 d . . .
C5 C 0.9222(5) 0.2185(4) 0.1046(3) 0.029(2) Uani 1 1 d . . .
C6 C 1.0244(6) 0.2389(4) 0.1842(3) 0.034(2) Uani 1 1 d . . .
H6 H 1.0792 0.2305 0.2073 0.041 Uiso 1 1 calc R . .
C7 C 0.9684(5) 0.2847(4) 0.1946(3) 0.030(2) Uani 1 1 d . . .
H7 H 0.9826 0.3077 0.2254 0.036 Uiso 1 1 calc R . .
C8 C 0.8876(5) 0.2981(4) 0.1589(3) 0.029(2) Uani 1 1 d . . .
C9 C 0.8149(5) 0.3659(4) 0.2122(3) 0.029(2) Uani 1 1 d . . .
C10 C 0.8185(5) 0.3253(4) 0.2546(3) 0.032(2) Uani 1 1 d . . .
H10 H 0.8395 0.2843 0.2522 0.038 Uiso 1 1 calc R . .
C11 C 0.7915(6) 0.3455(4) 0.2994(3) 0.037(2) Uani 1 1 d . . .
H11 H 0.7933 0.3181 0.3275 0.045 Uiso 1 1 calc R . .
C12 C 0.7616(5) 0.4063(4) 0.3033(3) 0.030(2) Uani 1 1 d . . .
C13 C 0.7610(5) 0.4434(4) 0.2600(3) 0.031(2) Uani 1 1 d . . .
H13 H 0.7409 0.4847 0.2619 0.037 Uiso 1 1 calc R . .
C14 C 0.7293(6) 0.4299(4) 0.3498(4) 0.038(2) Uani 1 1 d . . .
C15 C 0.7692(8) 0.4102(5) 0.3972(4) 0.052(3) Uani 1 1 d . . .
H15 H 0.8190 0.3820 0.4008 0.063 Uiso 1 1 calc R . .
C16 C 0.7356(9) 0.4321(5) 0.4411(4) 0.062(3) Uani 1 1 d . . .
H16 H 0.7630 0.4184 0.4742 0.074 Uiso 1 1 calc R . .
C17 C 0.6645(9) 0.4726(5) 0.4364(5) 0.067(4) Uani 1 1 d . . .
H17 H 0.6416 0.4859 0.4661 0.080 Uiso 1 1 calc R . .
C18 C 0.6262(8) 0.4940(5) 0.3901(5) 0.064(3) Uani 1 1 d . . .
H18 H 0.5781 0.5235 0.3873 0.077 Uiso 1 1 calc R . .
C19 C 0.6579(7) 0.4723(5) 0.3460(4) 0.052(3) Uani 1 1 d . . .
H19 H 0.6302 0.4869 0.3133 0.062 Uiso 1 1 calc R . .
C20 C 0.8456(6) 0.2343(4) -0.0825(3) 0.036(2) Uani 1 1 d . . .
H20 H 0.8145 0.1970 -0.0930 0.044 Uiso 1 1 calc R . .
C21 C 0.8979(6) 0.2597(4) -0.1153(4) 0.041(2) Uani 1 1 d . . .
H21 H 0.9021 0.2411 -0.1473 0.049 Uiso 1 1 calc R . .
C22 C 0.9442(6) 0.3134(5) -0.1000(4) 0.045(3) Uani 1 1 d . . .
H22 H 0.9826 0.3320 -0.1212 0.054 Uiso 1 1 calc R . .
C23 C 0.9344(5) 0.3411(4) -0.0523(3) 0.034(2) Uani 1 1 d . . .
C24 C 0.8762(5) 0.3118(4) -0.0227(3) 0.027(2) Uani 1 1 d . . .
C25 C 0.9777(6) 0.3966(4) -0.0331(4) 0.036(2) Uani 1 1 d . . .
H25 H 1.0167 0.4181 -0.0523 0.043 Uiso 1 1 calc R . .
C26 C 0.9631(5) 0.4188(4) 0.0129(3) 0.035(2) Uani 1 1 d . . .
H26 H 0.9927 0.4556 0.0261 0.042 Uiso 1 1 calc R . .
C27 C 0.9040(5) 0.3873(4) 0.0412(3) 0.0255(19) Uani 1 1 d . . .
C28 C 0.9453(5) 0.4443(4) 0.1188(3) 0.0274(19) Uani 1 1 d . . .
C29 C 1.0400(6) 0.4405(4) 0.1227(3) 0.034(2) Uani 1 1 d . . .
H29 H 1.0661 0.4107 0.1031 0.041 Uiso 1 1 calc R . .
C30 C 1.0972(6) 0.4796(4) 0.1549(3) 0.039(2) Uani 1 1 d . . .
H30 H 1.1618 0.4784 0.1561 0.047 Uiso 1 1 calc R . .
C31 C 1.0575(5) 0.5209(4) 0.1854(3) 0.031(2) Uani 1 1 d . . .
C32 C 0.9644(6) 0.5178(4) 0.1832(3) 0.032(2) Uani 1 1 d . . .
H32 H 0.9377 0.5436 0.2058 0.038 Uiso 1 1 calc R . .
C33 C 1.1125(6) 0.5671(5) 0.2182(3) 0.040(2) Uani 1 1 d . . .
C34 C 1.2044(7) 0.5553(5) 0.2386(4) 0.058(3) Uani 1 1 d . . .
H34 H 1.2317 0.5170 0.2325 0.069 Uiso 1 1 calc R . .
C35 C 1.2558(7) 0.6007(6) 0.2684(5) 0.078(4) Uani 1 1 d . . .
H35 H 1.3180 0.5926 0.2825 0.093 Uiso 1 1 calc R . .
C36 C 1.2188(7) 0.6554(5) 0.2774(4) 0.064(3) Uani 1 1 d . . .
H36 H 1.2552 0.6854 0.2974 0.076 Uiso 1 1 calc R . .
C37 C 1.1281(6) 0.6682(5) 0.2578(3) 0.043(2) Uani 1 1 d . . .
H37 H 1.1016 0.7064 0.2650 0.052 Uiso 1 1 calc R . .
C38 C 1.0770(6) 0.6252(4) 0.2278(3) 0.038(2) Uani 1 1 d . . .
H38 H 1.0157 0.6350 0.2130 0.045 Uiso 1 1 calc R . .
C39 C 0.5832(6) 0.1986(4) -0.0583(3) 0.036(2) Uani 1 1 d . . .
H39 H 0.6021 0.1569 -0.0600 0.043 Uiso 1 1 calc R . .
C40 C 0.5024(6) 0.2157(5) -0.0889(4) 0.044(2) Uani 1 1 d . . .
H40 H 0.4687 0.1869 -0.1115 0.052 Uiso 1 1 calc R . .
C41 C 0.4713(6) 0.2752(5) -0.0860(3) 0.042(2) Uani 1 1 d . . .
H41 H 0.4147 0.2876 -0.1058 0.050 Uiso 1 1 calc R . .
C42 C 0.5248(5) 0.3173(4) -0.0533(3) 0.031(2) Uani 1 1 d . . .
C43 C 0.6069(5) 0.2949(4) -0.0237(3) 0.031(2) Uani 1 1 d . . .
C44 C 0.5026(6) 0.3795(4) -0.0471(3) 0.032(2) Uani 1 1 d . . .
H44 H 0.4468 0.3952 -0.0655 0.038 Uiso 1 1 calc R . .
C45 C 0.5588(5) 0.4175(4) -0.0158(3) 0.034(2) Uani 1 1 d . . .
H45 H 0.5432 0.4596 -0.0125 0.041 Uiso 1 1 calc R . .
C46 C 0.6423(5) 0.3929(4) 0.0125(3) 0.0264(19) Uani 1 1 d . . .
C47 C 0.7153(5) 0.4895(4) 0.0390(3) 0.030(2) Uani 1 1 d . . .
C48 C 0.7016(6) 0.5179(4) -0.0094(3) 0.037(2) Uani 1 1 d . . .
H48 H 0.6754 0.4954 -0.0390 0.044 Uiso 1 1 calc R . .
C49 C 0.7267(6) 0.5788(4) -0.0135(3) 0.033(2) Uani 1 1 d . . .
H49 H 0.7152 0.5985 -0.0459 0.039 Uiso 1 1 calc R . .
C50 C 0.7686(5) 0.6119(4) 0.0292(3) 0.032(2) Uani 1 1 d . . .
C51 C 0.7777(5) 0.5815(4) 0.0757(3) 0.028(2) Uani 1 1 d . . .
H51 H 0.8041 0.6033 0.1056 0.033 Uiso 1 1 calc R . .
C52 C 0.8046(6) 0.6752(4) 0.0271(3) 0.034(2) Uani 1 1 d . . .
C53 C 0.8403(6) 0.6944(4) -0.0160(4) 0.040(2) Uani 1 1 d . . .
H53 H 0.8378 0.6675 -0.0444 0.048 Uiso 1 1 calc R . .
C54 C 0.8790(6) 0.7519(5) -0.0176(4) 0.046(3) Uani 1 1 d . . .
H54 H 0.9026 0.7643 -0.0474 0.056 Uiso 1 1 calc R . .
C55 C 0.8838(6) 0.7909(4) 0.0225(4) 0.046(3) Uani 1 1 d . . .
H55 H 0.9120 0.8300 0.0212 0.055 Uiso 1 1 calc R . .
C56 C 0.8472(6) 0.7735(4) 0.0660(4) 0.044(2) Uani 1 1 d . . .
H56 H 0.8484 0.8012 0.0939 0.053 Uiso 1 1 calc R . .
C57 C 0.8096(6) 0.7160(4) 0.0677(3) 0.037(2) Uani 1 1 d . . .
H57 H 0.7863 0.7037 0.0975 0.044 Uiso 1 1 calc R . .
C58 C 0.6932(6) 0.1069(4) 0.0772(3) 0.037(2) Uani 1 1 d . . .
H58 H 0.7183 0.0819 0.0535 0.045 Uiso 1 1 calc R . .
C59 C 0.6516(6) 0.0775(4) 0.1142(4) 0.046(3) Uani 1 1 d . . .
H59 H 0.6504 0.0338 0.1164 0.055 Uiso 1 1 calc R . .
C60 C 0.6125(6) 0.1133(4) 0.1475(4) 0.046(3) Uani 1 1 d . . .
H60 H 0.5829 0.0946 0.1729 0.055 Uiso 1 1 calc R . .
C61 C 0.6163(6) 0.1785(4) 0.1440(3) 0.036(2) Uani 1 1 d . . .
C62 C 0.6620(5) 0.2030(4) 0.1064(3) 0.029(2) Uani 1 1 d . . .
C63 C 0.5779(6) 0.2190(4) 0.1754(3) 0.036(2) Uani 1 1 d . . .
H63 H 0.5471 0.2035 0.2015 0.043 Uiso 1 1 calc R . .
C64 C 0.5843(6) 0.2801(4) 0.1689(3) 0.034(2) Uani 1 1 d . . .
H64 H 0.5549 0.3075 0.1889 0.041 Uiso 1 1 calc R . .
C65 C 0.6359(5) 0.3039(4) 0.1315(3) 0.028(2) Uani 1 1 d . . .
C66 C 0.5926(5) 0.4115(4) 0.1351(3) 0.028(2) Uani 1 1 d . . .
C67 C 0.4976(5) 0.4023(4) 0.1314(3) 0.031(2) Uani 1 1 d . . .
H67 H 0.4709 0.3631 0.1231 0.037 Uiso 1 1 calc R . .
C68 C 0.4432(6) 0.4533(4) 0.1406(3) 0.034(2) Uani 1 1 d . . .
H68 H 0.3792 0.4479 0.1401 0.040 Uiso 1 1 calc R . .
C69 C 0.4814(6) 0.5106(4) 0.1502(3) 0.030(2) Uani 1 1 d . . .
C70 C 0.5746(5) 0.5153(4) 0.1517(3) 0.030(2) Uani 1 1 d . . .
H70 H 0.6018 0.5548 0.1574 0.036 Uiso 1 1 calc R . .
C71 C 0.4272(6) 0.5670(5) 0.1577(3) 0.039(2) Uani 1 1 d . . .
C72 C 0.3352(6) 0.5713(5) 0.1361(3) 0.049(3) Uani 1 1 d . . .
H72 H 0.3059 0.5368 0.1184 0.059 Uiso 1 1 calc R . .
C73 C 0.2852(7) 0.6241(5) 0.1395(4) 0.063(3) Uani 1 1 d . . .
H73 H 0.2219 0.6256 0.1253 0.076 Uiso 1 1 calc R . .
C74 C 0.3278(7) 0.6747(5) 0.1637(4) 0.060(3) Uani 1 1 d . . .
H74 H 0.2944 0.7119 0.1645 0.073 Uiso 1 1 calc R . .
C75 C 0.4184(7) 0.6723(5) 0.1867(4) 0.048(3) Uani 1 1 d . . .
H75 H 0.4466 0.7069 0.2046 0.057 Uiso 1 1 calc R . .
C76 C 0.4682(7) 0.6182(4) 0.1832(4) 0.045(2) Uani 1 1 d . . .
H76 H 0.5309 0.6164 0.1986 0.053 Uiso 1 1 calc R . .
C77 C 0.7906(7) 0.0872(5) -0.0505(4) 0.051(3) Uani 1 1 d . . .
C78 C 0.7628(6) 0.6132(5) 0.2009(3) 0.038(2) Uani 1 1 d . . .
Cl1 Cl 0.25961(18) 0.33048(14) 0.16665(11) 0.0588(7) Uani 1 1 d . . .
O1 O 0.1963(5) 0.2823(4) 0.1465(4) 0.097(3) Uani 1 1 d . . .
O2 O 0.2485(5) 0.3798(3) 0.1318(3) 0.062(2) Uani 1 1 d . . .
O3 O 0.3510(5) 0.3071(4) 0.1715(3) 0.078(2) Uani 1 1 d . . .
O4 O 0.2423(8) 0.3474(6) 0.2151(3) 0.135(4) Uani 1 1 d . . .
C79 C 0.4461(9) 0.3989(7) 0.3074(5) 0.098(5) Uani 1 1 d . . .
H79A H 0.4852 0.4017 0.3414 0.117 Uiso 1 1 calc R . .
H79B H 0.3906 0.3746 0.3104 0.117 Uiso 1 1 calc R . .
C80 C 0.4943(9) 0.3731(7) 0.2713(5) 0.089(4) Uani 1 1 d . . .
H80A H 0.5442 0.4010 0.2649 0.107 Uiso 1 1 calc R . .
H80B H 0.4526 0.3662 0.2385 0.107 Uiso 1 1 calc R . .
Cl2 Cl 0.4151(2) 0.47652(17) 0.28094(14) 0.0902(11) Uani 1 1 d . . .
Cl3 Cl 0.54224(19) 0.29932(14) 0.29757(11) 0.0611(8) Uani 1 1 d . . .
C81 C 0.6071(9) 0.0376(7) -0.1700(6) 0.099(5) Uani 1 1 d . . .
H81A H 0.6299 0.0441 -0.1331 0.119 Uiso 1 1 calc R . .
H81B H 0.6241 -0.0046 -0.1789 0.119 Uiso 1 1 calc R . .
C82 C 0.6514(10) 0.0821(6) -0.2000(5) 0.087(4) Uani 1 1 d . . .
H82A H 0.6239 0.0785 -0.2365 0.105 Uiso 1 1 calc R . .
H82B H 0.7175 0.0721 -0.1968 0.105 Uiso 1 1 calc R . .
Cl4 Cl 0.4859(2) 0.0449(2) -0.18150(18) 0.1215(15) Uani 1 1 d . . .
Cl5 Cl 0.6389(3) 0.15988(18) -0.17893(14) 0.1010(12) Uani 1 1 d . . .
C83 C 0.3437(14) 0.1839(6) 0.0934(7) 0.095(6) Uani 0.715(13) 1 d PD A 1
H83A H 0.3001 0.2150 0.1026 0.114 Uiso 0.715(13) 1 calc PR A 1
H83B H 0.3991 0.1838 0.1201 0.114 Uiso 0.715(13) 1 calc PR A 1
C84 C 0.3683(13) 0.1975(7) 0.0428(7) 0.117(8) Uani 0.715(13) 1 d PD A 1
H84A H 0.3123 0.1993 0.0167 0.140 Uiso 0.715(13) 1 calc PR A 1
H84B H 0.4086 0.1647 0.0330 0.140 Uiso 0.715(13) 1 calc PR A 1
C83' C 0.387(2) 0.141(2) 0.0611(17) 0.095(6) Uani 0.285(13) 1 d PD A 2
H83C H 0.4355 0.1267 0.0889 0.114 Uiso 0.285(13) 1 calc PR A 2
H83D H 0.3873 0.1090 0.0342 0.114 Uiso 0.285(13) 1 calc PR A 2
C84' C 0.443(3) 0.1875(6) 0.0388(17) 0.117(8) Uani 0.285(13) 1 d PD A 2
H84C H 0.4347 0.1794 0.0016 0.140 Uiso 0.285(13) 1 calc PR A 2
H84D H 0.5077 0.1788 0.0527 0.140 Uiso 0.285(13) 1 calc PR A 2
Cl6 Cl 0.2914(3) 0.1089(2) 0.08750(17) 0.1246(15) Uani 1 1 d D . .
Cl7 Cl 0.4262(3) 0.2692(3) 0.04625(18) 0.150(2) Uani 1 1 d D . .
C85 C 0.5000 0.0000 0.0000 0.350 Uiso 1 2 d SD . .
H85A H 0.5494 -0.0168 0.0261 0.420 Uiso 0.50 1 calc PR B .
H85B H 0.4516 -0.0315 -0.0088 0.420 Uiso 0.50 1 calc PR . .
Cl8 Cl 0.5434(15) 0.0251(10) -0.0549(6) 0.330(11) Uiso 0.50 1 d PD B -1
Cl9 Cl 0.4542(16) 0.0697(7) 0.0214(8) 0.350 Uiso 0.50 1 d PD B -1


_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 N17 2.074(8) . ?
Ni1 N13 2.124(7) . ?
Ni1 N9 2.126(7) . ?
Ni1 N1 2.130(7) . ?
Ni1 N5 2.145(7) . ?
Ni1 Ni2 2.3296(15) . ?
Ni2 N14 2.015(6) . ?
Ni2 N6 2.019(6) . ?
Ni2 N2 2.024(6) . ?
Ni2 N10 2.028(6) . ?
Ni2 Ni3 2.3537(15) . ?
Ni3 N15 1.896(6) . ?
Ni3 N11 1.906(6) . ?
Ni3 N3 1.907(7) . ?
Ni3 N7 1.919(6) . ?
Ni3 Ni4 2.4077(15) . ?
Ni4 N18 2.022(8) . ?
Ni4 N8 2.056(6) . ?
Ni4 N4 2.060(7) . ?
Ni4 N16 2.065(6) . ?
Ni4 N12 2.076(6) . ?
S1 C77 1.665(13) . ?
S2 C78 1.612(10) . ?
N1 C1 1.322(10) . ?
N1 C5 1.360(10) . ?
N2 C8 1.343(10) . ?
N2 C5 1.384(10) . ?
N3 C8 1.370(10) . ?
N3 C9 1.384(10) . ?
N4 C13 1.336(10) . ?
N4 C9 1.361(10) . ?
N5 C20 1.324(10) . ?
N5 C24 1.376(10) . ?
N6 C24 1.348(10) . ?
N6 C27 1.358(10) . ?
N7 C27 1.356(10) . ?
N7 C28 1.402(10) . ?
N8 C32 1.341(10) . ?
N8 C28 1.366(10) . ?
N9 C39 1.319(10) . ?
N9 C43 1.367(11) . ?
N10 C46 1.334(10) . ?
N10 C43 1.372(10) . ?
N11 C46 1.371(10) . ?
N11 C47 1.389(10) . ?
N12 C47 1.354(10) . ?
N12 C51 1.369(10) . ?
N13 C58 1.328(10) . ?
N13 C62 1.367(10) . ?
N14 C65 1.336(10) . ?
N14 C62 1.375(10) . ?
N15 C65 1.374(10) . ?
N15 C66 1.399(10) . ?
N16 C70 1.339(10) . ?
N16 C66 1.348(10) . ?
N17 C77 1.105(12) . ?
N18 C78 1.133(11) . ?
C1 C2 1.397(11) . ?
C2 C3 1.368(12) . ?
C3 C4 1.409(11) . ?
C4 C5 1.409(11) . ?
C4 C6 1.420(12) . ?
C6 C7 1.351(11) . ?
C7 C8 1.427(11) . ?
C9 C10 1.422(11) . ?
C10 C11 1.382(11) . ?
C11 C12 1.402(12) . ?
C12 C13 1.401(11) . ?
C12 C14 1.483(12) . ?
C14 C15 1.367(13) . ?
C14 C19 1.392(13) . ?
C15 C16 1.419(14) . ?
C16 C17 1.359(16) . ?
C17 C18 1.346(16) . ?
C18 C19 1.408(14) . ?
C20 C21 1.369(12) . ?
C21 C22 1.380(13) . ?
C22 C23 1.430(12) . ?
C23 C24 1.404(11) . ?
C23 C25 1.421(12) . ?
C25 C26 1.359(11) . ?
C26 C27 1.416(11) . ?
C28 C29 1.388(11) . ?
C29 C30 1.390(12) . ?
C30 C31 1.401(12) . ?
C31 C32 1.368(11) . ?
C31 C33 1.479(12) . ?
C33 C34 1.400(12) . ?
C33 C38 1.407(12) . ?
C34 C35 1.406(14) . ?
C35 C36 1.345(14) . ?
C36 C37 1.384(13) . ?
C37 C38 1.371(12) . ?
C39 C40 1.379(12) . ?
C40 C41 1.378(13) . ?
C41 C42 1.411(12) . ?
C42 C44 1.406(12) . ?
C42 C43 1.419(11) . ?
C44 C45 1.356(12) . ?
C45 C46 1.438(11) . ?
C47 C48 1.407(11) . ?
C48 C49 1.384(12) . ?
C49 C50 1.397(12) . ?
C50 C51 1.385(11) . ?
C50 C52 1.479(12) . ?
C52 C57 1.385(12) . ?
C52 C53 1.396(11) . ?
C53 C54 1.378(12) . ?
C54 C55 1.353(13) . ?
C55 C56 1.401(13) . ?
C56 C57 1.372(12) . ?
C58 C59 1.395(12) . ?
C59 C60 1.373(13) . ?
C60 C61 1.421(12) . ?
C61 C63 1.394(12) . ?
C61 C62 1.397(11) . ?
C63 C64 1.342(11) . ?
C64 C65 1.441(11) . ?
C66 C67 1.405(11) . ?
C67 C68 1.413(11) . ?
C68 C69 1.373(12) . ?
C69 C70 1.374(11) . ?
C69 C71 1.496(12) . ?
C71 C76 1.388(13) . ?
C71 C72 1.389(12) . ?
C72 C73 1.376(13) . ?
C73 C74 1.372(15) . ?
C74 C75 1.378(13) . ?
C75 C76 1.398(12) . ?
Cl1 O4 1.397(9) . ?
Cl1 O2 1.406(7) . ?
Cl1 O3 1.428(7) . ?
Cl1 O1 1.447(9) . ?
C79 C80 1.399(16) . ?
C79 Cl2 1.854(15) . ?
C80 Cl3 1.843(15) . ?
C81 C82 1.470(17) . ?
C81 Cl4 1.774(13) . ?
C82 Cl5 1.799(13) . ?
C83 C84 1.475(10) . ?
C83 Cl6 1.800(9) . ?
C84 Cl7 1.773(9) . ?
C83' C84' 1.495(10) . ?
C83' Cl6 1.805(10) . ?
C84' Cl7 1.806(10) . ?
C85 Cl8 1.769(9) 3_655 ?
C85 Cl8 1.769(9) . ?
C85 Cl9 1.788(9) 3_655 ?
C85 Cl9 1.788(9) . ?

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
N17 Ni1 N13 95.5(3) . . ?
N17 Ni1 N9 94.1(3) . . ?
N13 Ni1 N9 91.2(3) . . ?
N17 Ni1 N1 95.7(3) . . ?
N13 Ni1 N1 88.4(2) . . ?
N9 Ni1 N1 170.2(3) . . ?
N17 Ni1 N5 95.3(3) . . ?
N13 Ni1 N5 169.0(3) . . ?
N9 Ni1 N5 89.9(3) . . ?
N1 Ni1 N5 88.7(2) . . ?
N17 Ni1 Ni2 179.5(2) . . ?
N13 Ni1 Ni2 84.40(19) . . ?
N9 Ni1 Ni2 85.38(19) . . ?
N1 Ni1 Ni2 84.84(18) . . ?
N5 Ni1 Ni2 84.8(2) . . ?
N14 Ni2 N6 173.4(3) . . ?
N14 Ni2 N2 88.8(3) . . ?
N6 Ni2 N2 89.4(3) . . ?
N14 Ni2 N10 89.8(2) . . ?
N6 Ni2 N10 91.3(2) . . ?
N2 Ni2 N10 173.4(3) . . ?
N14 Ni2 Ni1 93.4(2) . . ?
N6 Ni2 Ni1 93.09(19) . . ?
N2 Ni2 Ni1 93.2(2) . . ?
N10 Ni2 Ni1 93.31(19) . . ?
N14 Ni2 Ni3 86.2(2) . . ?
N6 Ni2 Ni3 87.27(19) . . ?
N2 Ni2 Ni3 86.5(2) . . ?
N10 Ni2 Ni3 86.94(19) . . ?
Ni1 Ni2 Ni3 179.55(6) . . ?
N15 Ni3 N11 89.2(3) . . ?
N15 Ni3 N3 89.9(3) . . ?
N11 Ni3 N3 178.5(3) . . ?
N15 Ni3 N7 178.5(3) . . ?
N11 Ni3 N7 91.4(3) . . ?
N3 Ni3 N7 89.5(3) . . ?
N15 Ni3 Ni2 89.61(19) . . ?
N11 Ni3 Ni2 89.4(2) . . ?
N3 Ni3 Ni2 89.5(2) . . ?
N7 Ni3 Ni2 89.1(2) . . ?
N15 Ni3 Ni4 90.89(19) . . ?
N11 Ni3 Ni4 90.6(2) . . ?
N3 Ni3 Ni4 90.6(2) . . ?
N7 Ni3 Ni4 90.4(2) . . ?
Ni2 Ni3 Ni4 179.50(6) . . ?
N18 Ni4 N8 96.1(3) . . ?
N18 Ni4 N4 96.7(3) . . ?
N8 Ni4 N4 91.0(2) . . ?
N18 Ni4 N16 96.0(3) . . ?
N8 Ni4 N16 167.9(3) . . ?
N4 Ni4 N16 88.8(2) . . ?
N18 Ni4 N12 96.3(3) . . ?
N8 Ni4 N12 87.9(2) . . ?
N4 Ni4 N12 166.9(3) . . ?
N16 Ni4 N12 89.5(3) . . ?
N18 Ni4 Ni3 179.1(2) . . ?
N8 Ni4 Ni3 84.53(19) . . ?
N4 Ni4 Ni3 83.94(18) . . ?
N16 Ni4 Ni3 83.38(18) . . ?
N12 Ni4 Ni3 83.01(19) . . ?
C1 N1 C5 115.9(7) . . ?
C1 N1 Ni1 120.8(6) . . ?
C5 N1 Ni1 123.0(5) . . ?
C8 N2 C5 119.8(7) . . ?
C8 N2 Ni2 120.9(5) . . ?
C5 N2 Ni2 118.9(6) . . ?
C8 N3 C9 122.0(7) . . ?
C8 N3 Ni3 120.2(5) . . ?
C9 N3 Ni3 117.6(5) . . ?
C13 N4 C9 119.1(7) . . ?
C13 N4 Ni4 120.1(5) . . ?
C9 N4 Ni4 120.5(5) . . ?
C20 N5 C24 117.3(7) . . ?
C20 N5 Ni1 120.8(6) . . ?
C24 N5 Ni1 121.6(5) . . ?
C24 N6 C27 120.0(7) . . ?
C24 N6 Ni2 120.0(5) . . ?
C27 N6 Ni2 119.7(5) . . ?
C27 N7 C28 120.3(7) . . ?
C27 N7 Ni3 120.5(5) . . ?
C28 N7 Ni3 119.0(5) . . ?
C32 N8 C28 118.0(7) . . ?
C32 N8 Ni4 119.9(5) . . ?
C28 N8 Ni4 122.1(5) . . ?
C39 N9 C43 116.9(7) . . ?
C39 N9 Ni1 120.7(6) . . ?
C43 N9 Ni1 122.4(6) . . ?
C46 N10 C43 121.3(7) . . ?
C46 N10 Ni2 119.5(5) . . ?
C43 N10 Ni2 118.3(5) . . ?
C46 N11 C47 121.8(7) . . ?
C46 N11 Ni3 119.0(5) . . ?
C47 N11 Ni3 119.2(5) . . ?
C47 N12 C51 118.9(7) . . ?
C47 N12 Ni4 121.6(6) . . ?
C51 N12 Ni4 119.5(6) . . ?
C58 N13 C62 117.0(7) . . ?
C58 N13 Ni1 119.4(6) . . ?
C62 N13 Ni1 123.6(6) . . ?
C65 N14 C62 119.5(7) . . ?
C65 N14 Ni2 120.5(6) . . ?
C62 N14 Ni2 118.8(5) . . ?
C65 N15 C66 122.4(6) . . ?
C65 N15 Ni3 118.5(5) . . ?
C66 N15 Ni3 119.1(5) . . ?
C70 N16 C66 119.4(7) . . ?
C70 N16 Ni4 118.8(5) . . ?
C66 N16 Ni4 121.7(5) . . ?
C77 N17 Ni1 155.2(8) . . ?
C78 N18 Ni4 160.3(7) . . ?
N1 C1 C2 125.3(8) . . ?
C3 C2 C1 118.6(8) . . ?
C2 C3 C4 118.8(8) . . ?
C3 C4 C5 117.7(8) . . ?
C3 C4 C6 124.2(8) . . ?
C5 C4 C6 118.0(8) . . ?
N1 C5 N2 115.7(7) . . ?
N1 C5 C4 123.6(7) . . ?
N2 C5 C4 120.8(8) . . ?
C7 C6 C4 120.7(8) . . ?
C6 C7 C8 119.2(8) . . ?
N2 C8 N3 115.6(7) . . ?
N2 C8 C7 121.3(8) . . ?
N3 C8 C7 122.8(8) . . ?
N4 C9 N3 117.1(7) . . ?
N4 C9 C10 119.6(8) . . ?
N3 C9 C10 123.0(8) . . ?
C11 C10 C9 120.2(8) . . ?
C10 C11 C12 120.0(8) . . ?
C13 C12 C11 116.2(8) . . ?
C13 C12 C14 121.4(8) . . ?
C11 C12 C14 122.4(8) . . ?
N4 C13 C12 124.9(8) . . ?
C15 C14 C19 118.9(9) . . ?
C15 C14 C12 120.4(9) . . ?
C19 C14 C12 120.7(9) . . ?
C14 C15 C16 119.4(11) . . ?
C17 C16 C15 120.6(11) . . ?
C18 C17 C16 120.8(11) . . ?
C17 C18 C19 119.5(11) . . ?
C14 C19 C18 120.8(10) . . ?
N5 C20 C21 126.2(9) . . ?
C20 C21 C22 117.4(9) . . ?
C21 C22 C23 119.8(9) . . ?
C24 C23 C25 117.8(8) . . ?
C24 C23 C22 117.6(9) . . ?
C25 C23 C22 124.7(8) . . ?
N6 C24 N5 116.3(7) . . ?
N6 C24 C23 122.1(8) . . ?
N5 C24 C23 121.6(8) . . ?
C26 C25 C23 119.6(8) . . ?
C25 C26 C27 120.3(9) . . ?
N7 C27 N6 116.4(7) . . ?
N7 C27 C26 123.2(8) . . ?
N6 C27 C26 120.3(7) . . ?
N8 C28 C29 119.7(8) . . ?
N8 C28 N7 115.1(7) . . ?
C29 C28 N7 125.0(7) . . ?
C28 C29 C30 120.9(8) . . ?
C29 C30 C31 118.5(8) . . ?
C32 C31 C30 117.2(8) . . ?
C32 C31 C33 120.7(8) . . ?
C30 C31 C33 122.1(7) . . ?
N8 C32 C31 125.1(8) . . ?
C34 C33 C38 117.4(9) . . ?
C34 C33 C31 120.6(9) . . ?
C38 C33 C31 121.9(8) . . ?
C33 C34 C35 119.3(10) . . ?
C36 C35 C34 121.4(10) . . ?
C35 C36 C37 120.6(10) . . ?
C38 C37 C36 119.2(9) . . ?
C37 C38 C33 122.0(8) . . ?
N9 C39 C40 125.0(8) . . ?
C41 C40 C39 119.1(9) . . ?
C40 C41 C42 118.9(9) . . ?
C44 C42 C41 125.2(8) . . ?
C44 C42 C43 117.4(8) . . ?
C41 C42 C43 117.4(8) . . ?
N9 C43 N10 116.8(7) . . ?
N9 C43 C42 122.7(8) . . ?
N10 C43 C42 120.5(8) . . ?
C45 C44 C42 121.8(8) . . ?
C44 C45 C46 118.6(8) . . ?
N10 C46 N11 117.0(7) . . ?
N10 C46 C45 120.4(8) . . ?
N11 C46 C45 122.5(8) . . ?
N12 C47 N11 115.5(7) . . ?
N12 C47 C48 120.3(8) . . ?
N11 C47 C48 124.1(8) . . ?
C49 C48 C47 119.3(8) . . ?
C48 C49 C50 121.2(8) . . ?
C51 C50 C49 116.1(8) . . ?
C51 C50 C52 119.6(8) . . ?
C49 C50 C52 124.3(8) . . ?
N12 C51 C50 124.0(8) . . ?
C57 C52 C53 117.6(8) . . ?
C57 C52 C50 122.7(8) . . ?
C53 C52 C50 119.6(8) . . ?
C54 C53 C52 120.7(9) . . ?
C55 C54 C53 120.7(9) . . ?
C54 C55 C56 120.0(9) . . ?
C57 C56 C55 119.0(9) . . ?
C56 C57 C52 121.9(9) . . ?
N13 C58 C59 124.5(8) . . ?
C60 C59 C58 118.1(9) . . ?
C59 C60 C61 119.9(9) . . ?
C63 C61 C62 118.4(8) . . ?
C63 C61 C60 124.5(8) . . ?
C62 C61 C60 117.1(8) . . ?
N13 C62 N14 115.0(7) . . ?
N13 C62 C61 123.3(8) . . ?
N14 C62 C61 121.7(8) . . ?
C64 C63 C61 120.2(8) . . ?
C63 C64 C65 120.0(8) . . ?
N14 C65 N15 115.9(7) . . ?
N14 C65 C64 120.0(8) . . ?
N15 C65 C64 124.0(7) . . ?
N16 C66 N15 115.8(7) . . ?
N16 C66 C67 120.6(8) . . ?
N15 C66 C67 123.5(8) . . ?
C66 C67 C68 117.8(8) . . ?
C69 C68 C67 121.0(8) . . ?
C68 C69 C70 116.9(8) . . ?
C68 C69 C71 123.7(8) . . ?
C70 C69 C71 119.4(8) . . ?
N16 C70 C69 124.2(8) . . ?
C76 C71 C72 117.8(9) . . ?
C76 C71 C69 121.4(8) . . ?
C72 C71 C69 120.6(9) . . ?
C73 C72 C71 121.9(10) . . ?
C74 C73 C72 119.2(10) . . ?
C73 C74 C75 121.0(10) . . ?
C74 C75 C76 119.1(10) . . ?
C71 C76 C75 120.9(9) . . ?
N17 C77 S1 178.4(10) . . ?
N18 C78 S2 177.5(9) . . ?
O4 Cl1 O2 112.5(6) . . ?
O4 Cl1 O3 108.8(6) . . ?
O2 Cl1 O3 109.7(5) . . ?
O4 Cl1 O1 109.0(7) . . ?
O2 Cl1 O1 108.1(5) . . ?
O3 Cl1 O1 108.7(5) . . ?
C80 C79 Cl2 103.2(10) . . ?
C79 C80 Cl3 107.3(10) . . ?
C82 C81 Cl4 111.9(11) . . ?
C81 C82 Cl5 111.9(9) . . ?
C84 C83 Cl6 105.5(8) . . ?
C83 C84 Cl7 108.5(9) . . ?
C84' C83' Cl6 158(4) . . ?
C83' C84' Cl7 122(3) . . ?
C83 Cl6 C83' 48.6(16) . . ?
C84 Cl7 C84' 37.1(11) . . ?
Cl8 C85 Cl8 179.999(1) 3_655 . ?
Cl8 C85 Cl9 101.9(6) 3_655 3_655 ?
Cl8 C85 Cl9 78.1(6) . 3_655 ?
Cl8 C85 Cl9 78.1(6) 3_655 . ?
Cl8 C85 Cl9 101.9(6) . . ?
Cl9 C85 Cl9 180.0(13) 3_655 . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.257
_refine_diff_density_min         -1.228
_refine_diff_density_rms         0.166
####################################################################### 
# 
# 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_ic17446
_database_code_depnum_ccdc_archive 'CCDC 1486168'
_audit_update_record             
;
2016-06-17 deposited with the CCDC.
2016-09-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C88 H62 Cl24 F6 N18 Ni4 O7 S4'
_chemical_formula_weight         2811.44

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   14.4138(4)
_cell_length_b                   37.0360(11)
_cell_length_c                   21.1405(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.6332(16)
_cell_angle_gamma                90.00
_cell_volume                     11230.9(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    45601
_cell_measurement_theta_min      1.10
_cell_measurement_theta_max      25.00

_exptl_crystal_description       plate
_exptl_crystal_colour            red-brown
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5640
_exptl_absorpt_coefficient_mu    1.375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6230
_exptl_absorpt_correction_T_max  0.9220
_exptl_absorpt_process_details   'SORTAV (Blessing, 1995)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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  'NONIUS KappaCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            45601
_diffrn_reflns_av_R_equivalents  0.0741
_diffrn_reflns_av_sigmaI/netI    0.1237
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.10
_diffrn_reflns_theta_max         25.00
_reflns_number_total             19695
_reflns_number_gt                9951
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'NONIUS COLLECT'
_computing_cell_refinement       DENZO-SMN
_computing_data_reduction        DENZO-SMNP
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.1217P)²+36.0712P] 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         19695
_refine_ls_number_parameters     1388
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.1762
_refine_ls_R_factor_gt           0.0806
_refine_ls_wR_factor_ref         0.2595
_refine_ls_wR_factor_gt          0.2016
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.76060(8) 0.34763(3) 0.58632(5) 0.0287(3) Uani 1 1 d . . .
Ni2 Ni 0.76671(7) 0.28274(3) 0.59594(5) 0.0240(3) Uani 1 1 d . . .
Ni3 Ni 0.77387(7) 0.22000(3) 0.60446(5) 0.0238(3) Uani 1 1 d . . .
Ni4 Ni 0.78251(7) 0.15513(3) 0.61110(5) 0.0248(3) Uani 1 1 d . . .
S1 S 0.7752(3) 0.47307(8) 0.54522(15) 0.0745(10) Uani 1 1 d . . .
S2 S 0.7750(2) 0.03198(8) 0.56720(15) 0.0632(8) Uani 1 1 d . . .
N1 N 0.8552(5) 0.34556(18) 0.6678(3) 0.0286(17) Uani 1 1 d . . .
N2 N 0.8197(4) 0.28511(17) 0.6827(3) 0.0221(15) Uani 1 1 d . . .
N3 N 0.7781(5) 0.22477(18) 0.6932(3) 0.0281(17) Uani 1 1 d . . .
N4 N 0.7364(5) 0.16502(19) 0.7002(3) 0.0275(17) Uani 1 1 d . . .
N5 N 0.6515(5) 0.34260(19) 0.6428(3) 0.0284(17) Uani 1 1 d . . .
N6 N 0.6441(5) 0.28081(18) 0.6223(3) 0.0249(16) Uani 1 1 d . . .
N7 N 0.6424(5) 0.21985(19) 0.5987(3) 0.0266(16) Uani 1 1 d . . .
N8 N 0.6463(5) 0.16023(18) 0.5658(3) 0.0257(16) Uani 1 1 d . . .
N9 N 0.6657(5) 0.33671(19) 0.5079(3) 0.0290(17) Uani 1 1 d . . .
N10 N 0.7141(5) 0.27697(18) 0.5094(3) 0.0236(16) Uani 1 1 d . . .
N11 N 0.7696(5) 0.21800(18) 0.5146(3) 0.0245(16) Uani 1 1 d . . .
N12 N 0.8296(4) 0.15996(19) 0.5211(3) 0.0268(16) Uani 1 1 d . . .
N13 N 0.8691(5) 0.33922(18) 0.5286(3) 0.0282(17) Uani 1 1 d . . .
N14 N 0.8901(5) 0.28120(18) 0.5701(3) 0.0257(16) Uani 1 1 d . . .
N15 N 0.9047(5) 0.22320(18) 0.6107(3) 0.0264(16) Uani 1 1 d . . .
N16 N 0.9179(5) 0.16482(19) 0.6512(3) 0.0260(16) Uani 1 1 d . . .
N17 N 0.7575(5) 0.4017(2) 0.5772(3) 0.0372(19) Uani 1 1 d . . .
N18 N 0.7874(5) 0.1011(2) 0.6160(3) 0.0297(17) Uani 1 1 d . . .
C1 C 0.8999(7) 0.3754(3) 0.6885(4) 0.041(2) Uani 1 1 d . . .
H1 H 0.8958 0.3959 0.6613 0.050 Uiso 1 1 calc R . .
C2 C 0.9523(7) 0.3787(3) 0.7469(4) 0.046(3) Uani 1 1 d . . .
H2 H 0.9829 0.4007 0.7590 0.055 Uiso 1 1 calc R . .
C3 C 0.9586(6) 0.3494(3) 0.7868(4) 0.040(2) Uani 1 1 d . . .
H3 H 0.9931 0.3508 0.8274 0.047 Uiso 1 1 calc R . .
C4 C 0.9134(6) 0.3175(2) 0.7667(4) 0.030(2) Uani 1 1 d . . .
C5 C 0.8640(6) 0.3166(2) 0.7058(4) 0.030(2) Uani 1 1 d . . .
C6 C 0.9145(6) 0.2857(2) 0.8041(4) 0.032(2) Uani 1 1 d . . .
H6 H 0.9482 0.2855 0.8450 0.039 Uiso 1 1 calc R . .
C7 C 0.8686(6) 0.2556(2) 0.7826(4) 0.030(2) Uani 1 1 d . . .
H7 H 0.8685 0.2347 0.8088 0.036 Uiso 1 1 calc R . .
C8 C 0.8197(6) 0.2554(2) 0.7197(4) 0.028(2) Uani 1 1 d . . .
C9 C 0.7438(6) 0.1977(2) 0.7288(4) 0.027(2) Uani 1 1 d . . .
C10 C 0.7131(6) 0.2027(2) 0.7893(4) 0.032(2) Uani 1 1 d . . .
H10 H 0.7144 0.2260 0.8082 0.039 Uiso 1 1 calc R . .
C11 C 0.6816(6) 0.1739(3) 0.8200(4) 0.036(2) Uani 1 1 d . . .
H11 H 0.6642 0.1770 0.8619 0.044 Uiso 1 1 calc R . .
C12 C 0.6736(6) 0.1395(2) 0.7921(4) 0.031(2) Uani 1 1 d . . .
C13 C 0.7008(6) 0.1371(2) 0.7317(4) 0.030(2) Uani 1 1 d . . .
H13 H 0.6943 0.1144 0.7106 0.036 Uiso 1 1 calc R . .
C14 C 0.6394(6) 0.1086(2) 0.8262(4) 0.034(2) Uani 1 1 d . . .
C15 C 0.6769(7) 0.0997(3) 0.8871(4) 0.040(2) Uani 1 1 d . . .
H15 H 0.7251 0.1144 0.9075 0.048 Uiso 1 1 calc R . .
C16 C 0.6458(7) 0.0699(3) 0.9192(5) 0.047(3) Uani 1 1 d . . .
H16 H 0.6727 0.0643 0.9608 0.057 Uiso 1 1 calc R . .
C17 C 0.5764(8) 0.0488(3) 0.8903(5) 0.059(3) Uani 1 1 d . . .
H17 H 0.5564 0.0280 0.9116 0.071 Uiso 1 1 calc R . .
C18 C 0.5361(9) 0.0571(3) 0.8321(6) 0.066(3) Uani 1 1 d . . .
H18 H 0.4853 0.0432 0.8134 0.079 Uiso 1 1 calc R . .
C19 C 0.5690(8) 0.0861(3) 0.7997(5) 0.056(3) Uani 1 1 d . . .
H19 H 0.5423 0.0909 0.7576 0.067 Uiso 1 1 calc R . .
C20 C 0.6142(7) 0.3722(2) 0.6665(4) 0.036(2) Uani 1 1 d . . .
H20 H 0.6476 0.3943 0.6656 0.043 Uiso 1 1 calc R . .
C21 C 0.5287(7) 0.3723(3) 0.6922(4) 0.043(2) Uani 1 1 d . . .
H21 H 0.5059 0.3940 0.7090 0.051 Uiso 1 1 calc R . .
C22 C 0.4782(6) 0.3413(2) 0.6931(4) 0.034(2) Uani 1 1 d . . .
H22 H 0.4190 0.3412 0.7092 0.041 Uiso 1 1 calc R . .
C23 C 0.5160(6) 0.3093(2) 0.6694(4) 0.029(2) Uani 1 1 d . . .
C24 C 0.6031(6) 0.3111(2) 0.6456(3) 0.0260(19) Uani 1 1 d . . .
C25 C 0.4680(6) 0.2760(2) 0.6672(4) 0.033(2) Uani 1 1 d . . .
H25 H 0.4085 0.2743 0.6827 0.039 Uiso 1 1 calc R . .
C26 C 0.5067(6) 0.2469(2) 0.6431(4) 0.033(2) Uani 1 1 d . . .
H26 H 0.4739 0.2246 0.6411 0.039 Uiso 1 1 calc R . .
C27 C 0.5984(6) 0.2488(2) 0.6201(3) 0.0239(19) Uani 1 1 d . . .
C28 C 0.5963(7) 0.1910(2) 0.5662(4) 0.033(2) Uani 1 1 d . . .
C29 C 0.5098(6) 0.1943(3) 0.5319(4) 0.039(2) Uani 1 1 d . . .
H29 H 0.4753 0.2161 0.5324 0.047 Uiso 1 1 calc R . .
C30 C 0.4746(7) 0.1645(3) 0.4966(4) 0.044(3) Uani 1 1 d . . .
H30 H 0.4147 0.1661 0.4736 0.053 Uiso 1 1 calc R . .
C31 C 0.5243(7) 0.1333(2) 0.4943(4) 0.038(2) Uani 1 1 d . . .
C32 C 0.6108(6) 0.1324(2) 0.5309(4) 0.034(2) Uani 1 1 d . . .
H32 H 0.6463 0.1107 0.5309 0.041 Uiso 1 1 calc R . .
C33 C 0.4896(7) 0.1015(3) 0.4569(5) 0.052(3) Uani 1 1 d . . .
C34 C 0.3948(8) 0.0913(3) 0.4566(6) 0.070(4) Uani 1 1 d . . .
H34 H 0.3536 0.1046 0.4801 0.084 Uiso 1 1 calc R . .
C35 C 0.3634(11) 0.0612(4) 0.4208(7) 0.096(5) Uani 1 1 d . . .
H35 H 0.2994 0.0546 0.4186 0.115 Uiso 1 1 calc R . .
C36 C 0.4238(13) 0.0407(4) 0.3887(8) 0.111(7) Uani 1 1 d . . .
H36 H 0.4019 0.0194 0.3671 0.133 Uiso 1 1 calc R . .
C37 C 0.5144(12) 0.0508(4) 0.3877(8) 0.102(6) Uani 1 1 d . . .
H37 H 0.5538 0.0375 0.3627 0.122 Uiso 1 1 calc R . .
C38 C 0.5506(10) 0.0806(3) 0.4233(6) 0.080(4) Uani 1 1 d . . .
H38 H 0.6149 0.0866 0.4248 0.096 Uiso 1 1 calc R . .
C39 C 0.6160(6) 0.3635(3) 0.4790(4) 0.037(2) Uani 1 1 d . . .
H39 H 0.6167 0.3863 0.4997 0.044 Uiso 1 1 calc R . .
C40 C 0.5637(7) 0.3602(3) 0.4209(4) 0.044(3) Uani 1 1 d . . .
H40 H 0.5295 0.3802 0.4024 0.053 Uiso 1 1 calc R . .
C41 C 0.5621(6) 0.3272(3) 0.3901(4) 0.035(2) Uani 1 1 d . . .
H41 H 0.5270 0.3243 0.3500 0.042 Uiso 1 1 calc R . .
C42 C 0.6124(6) 0.2984(2) 0.4184(4) 0.027(2) Uani 1 1 d . . .
C43 C 0.6640(6) 0.3039(2) 0.4790(4) 0.028(2) Uani 1 1 d . . .
C44 C 0.6162(6) 0.2633(3) 0.3909(4) 0.031(2) Uani 1 1 d . . .
H44 H 0.5816 0.2582 0.3513 0.037 Uiso 1 1 calc R . .
C45 C 0.6687(6) 0.2374(2) 0.4210(4) 0.030(2) Uani 1 1 d . . .
H45 H 0.6721 0.2143 0.4020 0.036 Uiso 1 1 calc R . .
C46 C 0.7196(6) 0.2442(2) 0.4815(4) 0.026(2) Uani 1 1 d . . .
C47 C 0.8125(6) 0.1900(2) 0.4858(4) 0.0261(19) Uani 1 1 d . . .
C48 C 0.8434(6) 0.1924(2) 0.4249(4) 0.027(2) Uani 1 1 d . . .
H48 H 0.8326 0.2137 0.4004 0.032 Uiso 1 1 calc R . .
C49 C 0.8893(6) 0.1638(2) 0.4007(4) 0.033(2) Uani 1 1 d . . .
H49 H 0.9085 0.1651 0.3590 0.040 Uiso 1 1 calc R . .
C50 C 0.9078(6) 0.1328(2) 0.4368(4) 0.030(2) Uani 1 1 d . . .
C51 C 0.8781(6) 0.1330(2) 0.4982(4) 0.027(2) Uani 1 1 d . . .
H51 H 0.8934 0.1128 0.5249 0.032 Uiso 1 1 calc R . .
C52 C 0.9612(6) 0.1014(2) 0.4152(4) 0.031(2) Uani 1 1 d . . .
C53 C 1.0258(6) 0.1060(3) 0.3702(4) 0.043(2) Uani 1 1 d . . .
H53 H 1.0353 0.1293 0.3532 0.051 Uiso 1 1 calc R . .
C54 C 1.0760(7) 0.0767(3) 0.3504(4) 0.044(3) Uani 1 1 d . . .
H54 H 1.1189 0.0801 0.3195 0.052 Uiso 1 1 calc R . .
C55 C 1.0639(7) 0.0435(3) 0.3749(5) 0.051(3) Uani 1 1 d . . .
H55 H 1.0992 0.0237 0.3613 0.061 Uiso 1 1 calc R . .
C56 C 1.0012(8) 0.0377(3) 0.4192(5) 0.055(3) Uani 1 1 d . . .
H56 H 0.9930 0.0143 0.4361 0.066 Uiso 1 1 calc R . .
C57 C 0.9496(7) 0.0673(3) 0.4390(4) 0.041(2) Uani 1 1 d . . .
H57 H 0.9060 0.0636 0.4693 0.049 Uiso 1 1 calc R . .
C58 C 0.8954(7) 0.3657(3) 0.4917(4) 0.039(2) Uani 1 1 d . . .
H58 H 0.8563 0.3863 0.4859 0.046 Uiso 1 1 calc R . .
C59 C 0.9762(7) 0.3650(3) 0.4612(4) 0.041(2) Uani 1 1 d . . .
H59 H 0.9916 0.3842 0.4342 0.049 Uiso 1 1 calc R . .
C60 C 1.0326(7) 0.3357(3) 0.4718(4) 0.039(2) Uani 1 1 d . . .
H60 H 1.0905 0.3351 0.4538 0.047 Uiso 1 1 calc R . .
C61 C 1.0082(6) 0.3065(2) 0.5079(4) 0.032(2) Uani 1 1 d . . .
C62 C 0.9230(6) 0.3092(2) 0.5346(4) 0.028(2) Uani 1 1 d . . .
C63 C 1.0617(7) 0.2747(3) 0.5196(4) 0.039(2) Uani 1 1 d . . .
H63 H 1.1195 0.2725 0.5020 0.046 Uiso 1 1 calc R . .
C64 C 1.0325(6) 0.2476(3) 0.5552(4) 0.035(2) Uani 1 1 d . . .
H64 H 1.0698 0.2267 0.5634 0.042 Uiso 1 1 calc R . .
C65 C 0.9430(6) 0.2510(2) 0.5808(4) 0.028(2) Uani 1 1 d . . .
C66 C 0.9575(6) 0.1978(2) 0.6460(4) 0.029(2) Uani 1 1 d . . .
C67 C 1.0426(6) 0.2056(3) 0.6810(4) 0.033(2) Uani 1 1 d . . .
H67 H 1.0678 0.2293 0.6799 0.040 Uiso 1 1 calc R . .
C68 C 1.0898(7) 0.1796(3) 0.7168(4) 0.038(2) Uani 1 1 d . . .
H68 H 1.1479 0.1852 0.7398 0.046 Uiso 1 1 calc R . .
C69 C 1.0532(6) 0.1448(2) 0.7198(4) 0.034(2) Uani 1 1 d . . .
C70 C 0.9661(6) 0.1400(2) 0.6868(4) 0.031(2) Uani 1 1 d . . .
H70 H 0.9380 0.1170 0.6898 0.037 Uiso 1 1 calc R . .
C71 C 1.1021(7) 0.1151(3) 0.7556(4) 0.040(2) Uani 1 1 d . . .
C72 C 1.1986(8) 0.1158(3) 0.7667(6) 0.063(3) Uani 1 1 d . . .
H72 H 1.2329 0.1348 0.7496 0.075 Uiso 1 1 calc R . .
C73 C 1.2454(9) 0.0885(4) 0.8032(6) 0.074(4) Uani 1 1 d . . .
H73 H 1.3115 0.0892 0.8104 0.089 Uiso 1 1 calc R . .
C74 C 1.1995(10) 0.0616(4) 0.8280(7) 0.086(4) Uani 1 1 d . . .
H74 H 1.2327 0.0437 0.8533 0.103 Uiso 1 1 calc R . .
C75 C 1.1018(9) 0.0596(3) 0.8167(6) 0.072(4) Uani 1 1 d . . .
H75 H 1.0685 0.0401 0.8329 0.086 Uiso 1 1 calc R . .
C76 C 1.0559(8) 0.0864(3) 0.7819(4) 0.048(3) Uani 1 1 d . . .
H76 H 0.9898 0.0855 0.7754 0.058 Uiso 1 1 calc R . .
C77 C 0.7643(7) 0.4313(3) 0.5638(4) 0.040(2) Uani 1 1 d . . .
C78 C 0.7827(6) 0.0722(3) 0.5964(4) 0.036(2) Uani 1 1 d . . .
S3 S 0.70961(18) 0.20360(8) 0.25543(11) 0.0451(7) Uani 1 1 d . A .
O1 O 0.8069(5) 0.1960(2) 0.2623(3) 0.064(2) Uani 1 1 d . . .
O2 O 0.6886(7) 0.2408(2) 0.2468(5) 0.096(3) Uani 1 1 d . . .
O3 O 0.6577(5) 0.1856(2) 0.2999(3) 0.077(3) Uani 1 1 d . . .
C79 C 0.6666(6) 0.1843(3) 0.1795(4) 0.071(4) Uani 1 1 d D . .
F1 F 0.6756(16) 0.1489(3) 0.1762(18) 0.139(6) Uani 0.733(3) 1 d PD A 1
F2 F 0.5761(6) 0.1928(3) 0.1672(9) 0.060(4) Uani 0.733(3) 1 d PD A 1
F3 F 0.7137(15) 0.1989(12) 0.1348(11) 0.111(4) Uani 0.733(3) 1 d PD A 1
F1' F 0.705(3) 0.1519(7) 0.182(6) 0.139(6) Uani 0.267(3) 1 d PD A 2
F2' F 0.5767(11) 0.1784(11) 0.163(3) 0.060(4) Uani 0.267(3) 1 d PD A 2
F3' F 0.698(4) 0.200(3) 0.129(3) 0.111(4) Uani 0.267(3) 1 d PD A 2
S4 S 0.32814(18) 0.26833(8) 0.46903(12) 0.0456(7) Uani 1 1 d . . .
O4 O 0.3254(6) 0.2510(2) 0.5301(3) 0.066(2) Uani 1 1 d . . .
O5 O 0.2392(4) 0.27121(19) 0.4321(3) 0.0492(18) Uani 1 1 d . . .
O6 O 0.4024(5) 0.2576(2) 0.4341(3) 0.068(2) Uani 1 1 d . . .
C80 C 0.3552(8) 0.3141(3) 0.4913(5) 0.058(3) Uani 1 1 d . . .
F4 F 0.2909(6) 0.3284(2) 0.5231(4) 0.096(3) Uani 1 1 d . . .
F5 F 0.3569(4) 0.33506(19) 0.4389(3) 0.0733(19) Uani 1 1 d . . .
F6 F 0.4368(5) 0.3173(2) 0.5241(3) 0.088(2) Uani 1 1 d . . .
C81 C 0.3305(7) 0.44402(19) 0.7873(4) 0.073(4) Uani 1 1 d D . .
H81 H 0.3912 0.4417 0.8142 0.088 Uiso 0.733(3) 1 calc PR A 1
H81' H 0.3920 0.4407 0.8128 0.088 Uiso 0.267(3) 1 calc PR A 2
Cl1 Cl 0.3537(4) 0.45106(18) 0.7059(2) 0.115(2) Uani 0.733(3) 1 d PD A 1
Cl2 Cl 0.2735(4) 0.48023(17) 0.8116(3) 0.125(2) Uani 0.733(3) 1 d PD A 1
Cl3 Cl 0.2725(5) 0.40279(15) 0.7867(3) 0.121(3) Uani 0.733(3) 1 d PD A 1
Cl1' Cl 0.3240(11) 0.4874(3) 0.7560(7) 0.115(2) Uani 0.267(3) 1 d PD A 2
Cl2' Cl 0.2399(10) 0.4471(5) 0.8400(8) 0.125(2) Uani 0.267(3) 1 d PD A 2
Cl3' Cl 0.3101(14) 0.4085(4) 0.7377(8) 0.121(3) Uani 0.267(3) 1 d PD A 2
C82 C 0.8817(9) 0.5503(2) 0.3689(4) 0.071(5) Uani 0.733(3) 1 d PD A 1
H82 H 0.8200 0.5587 0.3484 0.085 Uiso 0.733(3) 1 calc PR A 1
C82' C 0.9525(11) 0.5405(3) 0.3925(5) 0.071(5) Uani 0.267(3) 1 d PD A 2
H82' H 1.0143 0.5321 0.4129 0.085 Uiso 0.267(3) 1 calc PR A 2
Cl4 Cl 0.9331(3) 0.58563(10) 0.41220(17) 0.1089(15) Uani 1 1 d D . .
Cl5 Cl 0.8619(3) 0.51449(9) 0.41977(17) 0.1008(14) Uani 1 1 d D . .
Cl6 Cl 0.9478(3) 0.53622(9) 0.30980(16) 0.1039(14) Uani 1 1 d D . .
C83 C 0.4110(7) 0.4515(4) 0.5087(4) 0.139(7) Uani 1 1 d DU . .
H83 H 0.3777 0.4745 0.5167 0.167 Uiso 0.733(3) 1 calc PR A 1
H83' H 0.4183 0.4252 0.5186 0.167 Uiso 0.267(3) 1 calc PR A 2
Cl7 Cl 0.4006(3) 0.44291(11) 0.4261(2) 0.1160(15) Uani 1 1 d D A .
Cl8 Cl 0.3545(5) 0.4156(2) 0.5436(3) 0.140(2) Uani 0.733(3) 1 d PD A 1
Cl9 Cl 0.5290(6) 0.4561(10) 0.5375(8) 0.247(7) Uani 0.733(3) 1 d PD A 1
Cl8' Cl 0.3822(14) 0.4608(6) 0.5850(6) 0.140(2) Uani 0.267(3) 1 d PD A 2
Cl9' Cl 0.5321(12) 0.457(3) 0.5108(18) 0.247(7) Uani 0.267(3) 1 d PD A 2
C84 C 0.7017(7) 0.3094(3) 0.8793(4) 0.049(3) Uani 1 1 d . . .
H84 H 0.7482 0.2896 0.8890 0.058 Uiso 1 1 calc R . .
Cl10 Cl 0.6204(3) 0.30897(10) 0.93608(16) 0.0959(13) Uani 1 1 d . . .
Cl11 Cl 0.6430(2) 0.30243(9) 0.80339(14) 0.0699(9) Uani 1 1 d . . .
Cl12 Cl 0.7590(2) 0.35052(9) 0.88061(18) 0.0773(10) Uani 1 1 d . . .
C85 C 0.7121(10) 0.4964(4) 0.7036(6) 0.083(4) Uani 1 1 d . . .
H85 H 0.7313 0.5014 0.6602 0.100 Uiso 1 1 calc R . .
Cl13 Cl 0.7145(4) 0.53641(15) 0.7456(3) 0.148(2) Uani 1 1 d . . .
Cl14 Cl 0.7838(4) 0.46287(16) 0.7390(2) 0.150(2) Uani 1 1 d . . .
Cl15 Cl 0.5981(3) 0.47896(13) 0.6956(2) 0.1255(16) Uani 1 1 d . . .
C86 C 0.3848(7) 0.2095(3) 0.8034(5) 0.056(3) Uani 1 1 d . . .
H86 H 0.3448 0.2245 0.7723 0.067 Uiso 1 1 calc R . .
Cl16 Cl 0.4307(3) 0.17395(13) 0.7636(2) 0.1255(18) Uani 1 1 d . . .
Cl17 Cl 0.3177(2) 0.19351(10) 0.86054(15) 0.0760(10) Uani 1 1 d . . .
Cl18 Cl 0.4778(2) 0.23641(9) 0.83815(15) 0.0686(8) Uani 1 1 d . . .
C87 C 0.1426(9) 0.0727(4) 0.5972(6) 0.093(5) Uani 1 1 d . . .
H87 H 0.1794 0.0727 0.6399 0.112 Uiso 1 1 calc R . .
Cl19 Cl 0.1459(4) 0.11718(14) 0.5663(3) 0.1335(17) Uani 1 1 d . . .
Cl20 Cl 0.1944(3) 0.04186(13) 0.54993(19) 0.1139(15) Uani 1 1 d . . .
Cl21 Cl 0.0292(2) 0.06103(9) 0.60853(15) 0.0775(10) Uani 1 1 d . . .
C88 C 0.4302(9) 0.0653(3) 0.6221(6) 0.072(4) Uani 1 1 d . . .
H88 H 0.3956 0.0589 0.5803 0.086 Uiso 1 1 calc R . .
Cl22 Cl 0.4133(3) 0.11256(11) 0.63607(18) 0.0998(12) Uani 1 1 d . . .
Cl23 Cl 0.5487(2) 0.05749(9) 0.61736(18) 0.0822(10) Uani 1 1 d . . .
Cl24 Cl 0.3860(3) 0.04023(11) 0.67994(16) 0.0887(11) Uani 1 1 d . . .
O7 O 0.7768(10) 0.2867(5) 0.1486(7) 0.202(7) Uani 1 1 d . . .
H7A H 0.7317 0.2814 0.1724 0.303 Uiso 1 1 d R . .
H7B H 0.8020 0.2690 0.1300 0.303 Uiso 1 1 d 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 N17 2.011(9) . ?
Ni1 N5 2.074(7) . ?
Ni1 N9 2.083(7) . ?
Ni1 N1 2.091(7) . ?
Ni1 N13 2.100(7) . ?
Ni1 Ni2 2.4130(15) . ?
Ni2 N6 1.906(7) . ?
Ni2 N14 1.912(7) . ?
Ni2 N2 1.918(6) . ?
Ni2 N10 1.922(6) . ?
Ni2 Ni3 2.3321(15) . ?
Ni3 N3 1.880(6) . ?
Ni3 N15 1.881(7) . ?
Ni3 N7 1.887(7) . ?
Ni3 N11 1.897(6) . ?
Ni3 Ni4 2.4091(15) . ?
Ni4 N18 2.004(8) . ?
Ni4 N16 2.082(7) . ?
Ni4 N12 2.089(7) . ?
Ni4 N4 2.090(7) . ?
Ni4 N8 2.106(7) . ?
S1 C77 1.609(11) . ?
S2 C78 1.612(10) . ?
N1 C1 1.331(11) . ?
N1 C5 1.339(10) . ?
N2 C8 1.351(10) . ?
N2 C5 1.394(10) . ?
N3 C9 1.375(10) . ?
N3 C8 1.375(11) . ?
N4 C9 1.352(10) . ?
N4 C13 1.358(10) . ?
N5 C20 1.339(10) . ?
N5 C24 1.363(10) . ?
N6 C27 1.355(10) . ?
N6 C24 1.381(10) . ?
N7 C27 1.346(10) . ?
N7 C28 1.402(10) . ?
N8 C32 1.342(10) . ?
N8 C28 1.349(11) . ?
N9 C39 1.336(11) . ?
N9 C43 1.358(10) . ?
N10 C43 1.357(10) . ?
N10 C46 1.357(10) . ?
N11 C46 1.359(10) . ?
N11 C47 1.379(10) . ?
N12 C51 1.336(10) . ?
N12 C47 1.350(10) . ?
N13 C58 1.330(11) . ?
N13 C62 1.356(11) . ?
N14 C65 1.361(10) . ?
N14 C62 1.390(10) . ?
N15 C65 1.352(10) . ?
N15 C66 1.382(10) . ?
N16 C70 1.338(10) . ?
N16 C66 1.358(11) . ?
N17 C77 1.138(11) . ?
N18 C78 1.148(11) . ?
C1 C2 1.389(13) . ?
C2 C3 1.373(13) . ?
C3 C4 1.395(12) . ?
C4 C5 1.409(11) . ?
C4 C6 1.418(12) . ?
C6 C7 1.352(12) . ?
C7 C8 1.444(11) . ?
C9 C10 1.406(11) . ?
C10 C11 1.350(12) . ?
C11 C12 1.403(12) . ?
C12 C13 1.376(11) . ?
C12 C14 1.464(12) . ?
C14 C15 1.385(12) . ?
C14 C19 1.388(13) . ?
C15 C16 1.394(13) . ?
C16 C17 1.366(15) . ?
C17 C18 1.344(15) . ?
C18 C19 1.383(14) . ?
C20 C21 1.394(12) . ?
C21 C22 1.360(12) . ?
C22 C23 1.417(12) . ?
C23 C24 1.399(11) . ?
C23 C25 1.414(12) . ?
C25 C26 1.336(12) . ?
C26 C27 1.454(11) . ?
C28 C29 1.385(12) . ?
C29 C30 1.398(12) . ?
C30 C31 1.364(13) . ?
C31 C32 1.401(12) . ?
C31 C33 1.480(13) . ?
C33 C38 1.412(16) . ?
C33 C34 1.417(15) . ?
C34 C35 1.398(16) . ?
C35 C36 1.38(2) . ?
C36 C37 1.36(2) . ?
C37 C38 1.408(16) . ?
C39 C40 1.383(12) . ?
C40 C41 1.383(13) . ?
C41 C42 1.393(12) . ?
C42 C44 1.426(12) . ?
C42 C43 1.431(11) . ?
C44 C45 1.341(12) . ?
C45 C46 1.432(11) . ?
C47 C48 1.406(11) . ?
C48 C49 1.374(12) . ?
C49 C50 1.389(12) . ?
C50 C51 1.405(11) . ?
C50 C52 1.492(12) . ?
C52 C57 1.377(12) . ?
C52 C53 1.405(12) . ?
C53 C54 1.390(13) . ?
C54 C55 1.354(14) . ?
C55 C56 1.381(15) . ?
C56 C57 1.410(13) . ?
C58 C59 1.386(12) . ?
C59 C60 1.363(13) . ?
C60 C61 1.387(12) . ?
C61 C62 1.403(11) . ?
C61 C63 1.416(13) . ?
C63 C64 1.346(12) . ?
C64 C65 1.453(11) . ?
C66 C67 1.400(12) . ?
C67 C68 1.364(12) . ?
C68 C69 1.396(13) . ?
C69 C70 1.387(12) . ?
C69 C71 1.474(12) . ?
C71 C72 1.388(14) . ?
C71 C76 1.399(14) . ?
C72 C73 1.406(15) . ?
C73 C74 1.332(17) . ?
C74 C75 1.407(17) . ?
C75 C76 1.365(14) . ?
S3 O2 1.419(9) . ?
S3 O3 1.423(7) . ?
S3 O1 1.424(7) . ?
S3 C79 1.809(10) . ?
C79 F1 1.319(9) . ?
C79 F1' 1.325(10) . ?
C79 F2' 1.328(10) . ?
C79 F3' 1.330(10) . ?
C79 F3 1.331(9) . ?
C79 F2 1.343(9) . ?
S4 O6 1.417(7) . ?
S4 O5 1.439(7) . ?
S4 O4 1.445(7) . ?
S4 C80 1.793(12) . ?
C80 F6 1.309(12) . ?
C80 F4 1.310(12) . ?
C80 F5 1.355(12) . ?
C81 Cl2 1.679(8) . ?
C81 Cl3' 1.690(9) . ?
C81 Cl1' 1.735(9) . ?
C81 Cl3 1.740(8) . ?
C81 Cl2' 1.802(9) . ?
C81 Cl1 1.803(8) . ?
C82 Cl4 1.723(9) . ?
C82 Cl6 1.724(9) . ?
C82 Cl5 1.747(8) . ?
C82' Cl6 1.750(10) . ?
C82' Cl4 1.753(10) . ?
C82' Cl5 1.763(10) . ?
C83 Cl8' 1.739(9) . ?
C83 Cl9' 1.755(10) . ?
C83 Cl9 1.758(9) . ?
C83 Cl8 1.760(9) . ?
C83 Cl7 1.766(8) . ?
C84 Cl12 1.732(11) . ?
C84 Cl10 1.758(10) . ?
C84 Cl11 1.759(10) . ?
C85 Cl13 1.727(14) . ?
C85 Cl14 1.737(14) . ?
C85 Cl15 1.759(14) . ?
C86 Cl17 1.725(11) . ?
C86 Cl16 1.730(12) . ?
C86 Cl18 1.770(11) . ?
C87 Cl21 1.730(15) . ?
C87 Cl20 1.733(14) . ?
C87 Cl19 1.776(16) . ?
C88 Cl24 1.708(13) . ?
C88 Cl23 1.745(13) . ?
C88 Cl22 1.795(13) . ?

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
N17 Ni1 N5 97.7(3) . . ?
N17 Ni1 N9 96.4(3) . . ?
N5 Ni1 N9 88.0(3) . . ?
N17 Ni1 N1 97.0(3) . . ?
N5 Ni1 N1 89.5(3) . . ?
N9 Ni1 N1 166.6(3) . . ?
N17 Ni1 N13 95.9(3) . . ?
N5 Ni1 N13 166.3(3) . . ?
N9 Ni1 N13 88.7(3) . . ?
N1 Ni1 N13 90.6(3) . . ?
N17 Ni1 Ni2 178.9(2) . . ?
N5 Ni1 Ni2 83.42(19) . . ?
N9 Ni1 Ni2 83.65(19) . . ?
N1 Ni1 Ni2 83.01(19) . . ?
N13 Ni1 Ni2 82.99(19) . . ?
N6 Ni2 N14 176.1(3) . . ?
N6 Ni2 N2 90.9(3) . . ?
N14 Ni2 N2 88.9(3) . . ?
N6 Ni2 N10 89.0(3) . . ?
N14 Ni2 N10 90.9(3) . . ?
N2 Ni2 N10 176.2(3) . . ?
N6 Ni2 Ni3 88.6(2) . . ?
N14 Ni2 Ni3 87.5(2) . . ?
N2 Ni2 Ni3 87.8(2) . . ?
N10 Ni2 Ni3 88.5(2) . . ?
N6 Ni2 Ni1 92.0(2) . . ?
N14 Ni2 Ni1 91.9(2) . . ?
N2 Ni2 Ni1 92.4(2) . . ?
N10 Ni2 Ni1 91.3(2) . . ?
Ni3 Ni2 Ni1 179.37(6) . . ?
N3 Ni3 N15 89.5(3) . . ?
N3 Ni3 N7 89.9(3) . . ?
N15 Ni3 N7 176.5(3) . . ?
N3 Ni3 N11 176.8(3) . . ?
N15 Ni3 N11 90.4(3) . . ?
N7 Ni3 N11 90.0(3) . . ?
N3 Ni3 Ni2 88.9(2) . . ?
N15 Ni3 Ni2 88.8(2) . . ?
N7 Ni3 Ni2 87.8(2) . . ?
N11 Ni3 Ni2 88.0(2) . . ?
N3 Ni3 Ni4 92.3(2) . . ?
N15 Ni3 Ni4 90.8(2) . . ?
N7 Ni3 Ni4 92.7(2) . . ?
N11 Ni3 Ni4 90.9(2) . . ?
Ni2 Ni3 Ni4 178.79(6) . . ?
N18 Ni4 N16 97.1(3) . . ?
N18 Ni4 N12 96.9(3) . . ?
N16 Ni4 N12 88.9(2) . . ?
N18 Ni4 N4 98.1(3) . . ?
N16 Ni4 N4 88.3(3) . . ?
N12 Ni4 N4 165.0(3) . . ?
N18 Ni4 N8 98.0(3) . . ?
N16 Ni4 N8 164.7(3) . . ?
N12 Ni4 N8 87.2(2) . . ?
N4 Ni4 N8 91.6(3) . . ?
N18 Ni4 Ni3 179.0(2) . . ?
N16 Ni4 Ni3 83.8(2) . . ?
N12 Ni4 Ni3 83.2(2) . . ?
N4 Ni4 Ni3 81.86(19) . . ?
N8 Ni4 Ni3 81.00(18) . . ?
C1 N1 C5 117.0(7) . . ?
C1 N1 Ni1 119.7(6) . . ?
C5 N1 Ni1 122.6(6) . . ?
C8 N2 C5 120.3(7) . . ?
C8 N2 Ni2 119.6(5) . . ?
C5 N2 Ni2 120.0(5) . . ?
C9 N3 C8 123.1(7) . . ?
C9 N3 Ni3 119.9(5) . . ?
C8 N3 Ni3 116.9(5) . . ?
C9 N4 C13 118.6(7) . . ?
C9 N4 Ni4 122.8(5) . . ?
C13 N4 Ni4 118.5(6) . . ?
C20 N5 C24 117.3(8) . . ?
C20 N5 Ni1 119.8(6) . . ?
C24 N5 Ni1 121.4(5) . . ?
C27 N6 C24 120.0(7) . . ?
C27 N6 Ni2 119.0(6) . . ?
C24 N6 Ni2 121.0(6) . . ?
C27 N7 C28 123.8(7) . . ?
C27 N7 Ni3 118.6(6) . . ?
C28 N7 Ni3 117.3(6) . . ?
C32 N8 C28 118.5(7) . . ?
C32 N8 Ni4 118.0(6) . . ?
C28 N8 Ni4 123.3(5) . . ?
C39 N9 C43 118.3(8) . . ?
C39 N9 Ni1 120.0(6) . . ?
C43 N9 Ni1 120.8(6) . . ?
C43 N10 C46 120.2(7) . . ?
C43 N10 Ni2 120.8(6) . . ?
C46 N10 Ni2 118.7(5) . . ?
C46 N11 C47 123.2(7) . . ?
C46 N11 Ni3 116.8(5) . . ?
C47 N11 Ni3 119.9(5) . . ?
C51 N12 C47 119.2(7) . . ?
C51 N12 Ni4 119.7(6) . . ?
C47 N12 Ni4 121.1(5) . . ?
C58 N13 C62 117.8(8) . . ?
C58 N13 Ni1 120.2(6) . . ?
C62 N13 Ni1 121.4(5) . . ?
C65 N14 C62 119.2(7) . . ?
C65 N14 Ni2 119.9(5) . . ?
C62 N14 Ni2 120.6(6) . . ?
C65 N15 C66 122.7(7) . . ?
C65 N15 Ni3 117.9(6) . . ?
C66 N15 Ni3 119.4(6) . . ?
C70 N16 C66 117.7(7) . . ?
C70 N16 Ni4 121.7(6) . . ?
C66 N16 Ni4 120.5(5) . . ?
C77 N17 Ni1 168.6(7) . . ?
C78 N18 Ni4 155.7(7) . . ?
N1 C1 C2 124.7(9) . . ?
C3 C2 C1 118.3(9) . . ?
C2 C3 C4 118.8(9) . . ?
C3 C4 C5 118.6(8) . . ?
C3 C4 C6 123.6(8) . . ?
C5 C4 C6 117.8(8) . . ?
N1 C5 N2 116.5(7) . . ?
N1 C5 C4 122.5(8) . . ?
N2 C5 C4 120.9(8) . . ?
C7 C6 C4 121.3(8) . . ?
C6 C7 C8 119.5(8) . . ?
N2 C8 N3 117.5(7) . . ?
N2 C8 C7 120.1(8) . . ?
N3 C8 C7 122.2(8) . . ?
N4 C9 N3 115.2(7) . . ?
N4 C9 C10 120.5(7) . . ?
N3 C9 C10 124.2(8) . . ?
C11 C10 C9 118.9(8) . . ?
C10 C11 C12 122.1(8) . . ?
C13 C12 C11 115.5(8) . . ?
C13 C12 C14 123.2(8) . . ?
C11 C12 C14 121.3(8) . . ?
N4 C13 C12 124.1(8) . . ?
C15 C14 C19 115.9(8) . . ?
C15 C14 C12 121.6(8) . . ?
C19 C14 C12 122.5(8) . . ?
C14 C15 C16 121.7(10) . . ?
C17 C16 C15 119.6(10) . . ?
C18 C17 C16 120.5(10) . . ?
C17 C18 C19 119.7(11) . . ?
C18 C19 C14 122.5(10) . . ?
N5 C20 C21 123.4(9) . . ?
C22 C21 C20 119.8(9) . . ?
C21 C22 C23 118.5(9) . . ?
C24 C23 C25 118.9(8) . . ?
C24 C23 C22 118.5(8) . . ?
C25 C23 C22 122.6(8) . . ?
N5 C24 N6 116.2(7) . . ?
N5 C24 C23 122.5(8) . . ?
N6 C24 C23 121.3(8) . . ?
C26 C25 C23 119.7(9) . . ?
C25 C26 C27 121.1(9) . . ?
N7 C27 N6 117.7(7) . . ?
N7 C27 C26 123.2(8) . . ?
N6 C27 C26 119.0(8) . . ?
N8 C28 C29 121.8(8) . . ?
N8 C28 N7 114.7(8) . . ?
C29 C28 N7 123.3(8) . . ?
C28 C29 C30 118.1(9) . . ?
C31 C30 C29 121.6(9) . . ?
C30 C31 C32 116.3(8) . . ?
C30 C31 C33 122.9(8) . . ?
C32 C31 C33 120.7(8) . . ?
N8 C32 C31 123.8(8) . . ?
C38 C33 C34 120.0(10) . . ?
C38 C33 C31 120.7(10) . . ?
C34 C33 C31 119.3(10) . . ?
C35 C34 C33 118.4(14) . . ?
C36 C35 C34 121.1(14) . . ?
C37 C36 C35 120.6(13) . . ?
C36 C37 C38 120.8(15) . . ?
C37 C38 C33 118.8(13) . . ?
N9 C39 C40 124.2(9) . . ?
C41 C40 C39 118.5(9) . . ?
C40 C41 C42 119.6(8) . . ?
C41 C42 C44 124.3(8) . . ?
C41 C42 C43 118.4(8) . . ?
C44 C42 C43 117.3(7) . . ?
N10 C43 N9 117.3(7) . . ?
N10 C43 C42 121.6(8) . . ?
N9 C43 C42 121.1(8) . . ?
C45 C44 C42 119.9(8) . . ?
C44 C45 C46 121.0(8) . . ?
N10 C46 N11 117.7(7) . . ?
N10 C46 C45 119.9(7) . . ?
N11 C46 C45 122.3(8) . . ?
N12 C47 N11 116.2(7) . . ?
N12 C47 C48 120.1(8) . . ?
N11 C47 C48 123.6(8) . . ?
C49 C48 C47 120.0(8) . . ?
C48 C49 C50 120.3(8) . . ?
C49 C50 C51 116.4(8) . . ?
C49 C50 C52 123.5(8) . . ?
C51 C50 C52 120.0(8) . . ?
N12 C51 C50 123.9(8) . . ?
C57 C52 C53 118.1(9) . . ?
C57 C52 C50 121.3(8) . . ?
C53 C52 C50 120.6(8) . . ?
C54 C53 C52 120.6(10) . . ?
C55 C54 C53 120.2(9) . . ?
C54 C55 C56 121.2(10) . . ?
C55 C56 C57 118.8(10) . . ?
C52 C57 C56 121.2(9) . . ?
N13 C58 C59 124.1(9) . . ?
C60 C59 C58 116.9(9) . . ?
C59 C60 C61 122.1(9) . . ?
C60 C61 C62 116.5(9) . . ?
C60 C61 C63 125.5(9) . . ?
C62 C61 C63 118.0(8) . . ?
N13 C62 N14 116.0(7) . . ?
N13 C62 C61 122.4(8) . . ?
N14 C62 C61 121.6(8) . . ?
C64 C63 C61 121.6(9) . . ?
C63 C64 C65 118.8(9) . . ?
N15 C65 N14 117.1(7) . . ?
N15 C65 C64 121.8(8) . . ?
N14 C65 C64 120.7(8) . . ?
N16 C66 N15 116.3(7) . . ?
N16 C66 C67 119.8(8) . . ?
N15 C66 C67 123.6(8) . . ?
C68 C67 C66 120.6(9) . . ?
C67 C68 C69 120.6(9) . . ?
C70 C69 C68 114.9(8) . . ?
C70 C69 C71 121.8(9) . . ?
C68 C69 C71 123.3(8) . . ?
N16 C70 C69 126.1(9) . . ?
C72 C71 C76 117.2(10) . . ?
C72 C71 C69 119.5(10) . . ?
C76 C71 C69 123.3(9) . . ?
C71 C72 C73 119.8(12) . . ?
C74 C73 C72 121.7(12) . . ?
C73 C74 C75 120.0(12) . . ?
C76 C75 C74 118.5(12) . . ?
C75 C76 C71 122.8(11) . . ?
N17 C77 S1 179.3(11) . . ?
N18 C78 S2 178.6(9) . . ?
O2 S3 O3 114.8(6) . . ?
O2 S3 O1 113.7(6) . . ?
O3 S3 O1 114.6(5) . . ?
O2 S3 C79 102.7(5) . . ?
O3 S3 C79 104.2(4) . . ?
O1 S3 C79 105.1(4) . . ?
F1 C79 F1' 20(2) . . ?
F1 C79 F2' 85(2) . . ?
F1' C79 F2' 105.0(11) . . ?
F1 C79 F3' 110(8) . . ?
F1' C79 F3' 104.6(11) . . ?
F2' C79 F3' 104.6(11) . . ?
F1 C79 F3 107.9(14) . . ?
F1' C79 F3 99(7) . . ?
F2' C79 F3 115(4) . . ?
F3' C79 F3 11(4) . . ?
F1 C79 F2 108.8(12) . . ?
F1' C79 F2 128(2) . . ?
F2' C79 F2 23(2) . . ?
F3' C79 F2 98(4) . . ?
F3 C79 F2 108.7(12) . . ?
F1 C79 S3 114.4(14) . . ?
F1' C79 S3 103(4) . . ?
F2' C79 S3 123(3) . . ?
F3' C79 S3 115(5) . . ?
F3 C79 S3 108.4(17) . . ?
F2 C79 S3 108.7(9) . . ?
O6 S4 O5 114.6(4) . . ?
O6 S4 O4 115.4(5) . . ?
O5 S4 O4 114.6(4) . . ?
O6 S4 C80 104.3(5) . . ?
O5 S4 C80 103.4(5) . . ?
O4 S4 C80 102.1(5) . . ?
F6 C80 F4 109.7(9) . . ?
F6 C80 F5 107.1(9) . . ?
F4 C80 F5 105.0(10) . . ?
F6 C80 S4 112.6(9) . . ?
F4 C80 S4 111.7(8) . . ?
F5 C80 S4 110.3(7) . . ?
Cl2 C81 Cl3' 138.7(10) . . ?
Cl2 C81 Cl1' 50.8(6) . . ?
Cl3' C81 Cl1' 119.0(10) . . ?
Cl2 C81 Cl3 117.0(6) . . ?
Cl3' C81 Cl3 42.1(7) . . ?
Cl1' C81 Cl3 143.3(9) . . ?
Cl2 C81 Cl2' 49.8(6) . . ?
Cl3' C81 Cl2' 109.9(11) . . ?
Cl1' C81 Cl2' 99.3(9) . . ?
Cl3 C81 Cl2' 71.5(7) . . ?
Cl2 C81 Cl1 108.6(5) . . ?
Cl3' C81 Cl1 63.8(8) . . ?
Cl1' C81 Cl1 60.8(6) . . ?
Cl3 C81 Cl1 104.7(5) . . ?
Cl2' C81 Cl1 142.6(9) . . ?
Cl4 C82 Cl6 112.0(6) . . ?
Cl4 C82 Cl5 109.7(5) . . ?
Cl6 C82 Cl5 110.6(6) . . ?
Cl6 C82' Cl4 109.4(7) . . ?
Cl6 C82' Cl5 108.7(7) . . ?
Cl4 C82' Cl5 107.6(7) . . ?
C82 Cl4 C82' 38.6(7) . . ?
C82 Cl5 C82' 38.2(7) . . ?
C82 Cl6 C82' 38.6(7) . . ?
Cl8' C83 Cl9' 106.3(8) . . ?
Cl8' C83 Cl9 88.3(11) . . ?
Cl9' C83 Cl9 18.8(18) . . ?
Cl8' C83 Cl8 66.3(8) . . ?
Cl9' C83 Cl8 125(4) . . ?
Cl9 C83 Cl8 113.5(12) . . ?
Cl8' C83 Cl7 161.4(9) . . ?
Cl9' C83 Cl7 91.9(10) . . ?
Cl9 C83 Cl7 110.2(8) . . ?
Cl8 C83 Cl7 106.3(6) . . ?
Cl12 C84 Cl10 110.2(6) . . ?
Cl12 C84 Cl11 109.2(5) . . ?
Cl10 C84 Cl11 109.2(6) . . ?
Cl13 C85 Cl14 114.3(8) . . ?
Cl13 C85 Cl15 109.6(7) . . ?
Cl14 C85 Cl15 106.8(8) . . ?
Cl17 C86 Cl16 110.2(7) . . ?
Cl17 C86 Cl18 111.0(6) . . ?
Cl16 C86 Cl18 108.7(6) . . ?
Cl21 C87 Cl20 112.5(9) . . ?
Cl21 C87 Cl19 110.0(8) . . ?
Cl20 C87 Cl19 111.7(8) . . ?
Cl24 C88 Cl23 112.8(7) . . ?
Cl24 C88 Cl22 110.3(7) . . ?
Cl23 C88 Cl22 108.7(7) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.342
_refine_diff_density_min         -1.006
_refine_diff_density_rms         0.172
