# 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_ms7
_database_code_depnum_ccdc_archive 'CCDC 1434556'
_audit_update_record             
;
2015-11-02 deposited with the CCDC.
2016-02-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'2(C78 H52 Cl4 F12 N16 Ni4 O8), 2(C H4 O), H2 O'
_chemical_formula_sum            'C158 H114 Cl8 F24 N32 Ni8 O19'
_chemical_formula_weight         3974.09

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'
Cl Cl 0.1484 0.1585 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   15.825(2)
_cell_length_b                   16.590(2)
_cell_length_c                   17.807(3)
_cell_angle_alpha                75.858(6)
_cell_angle_beta                 69.560(5)
_cell_angle_gamma                68.566(5)
_cell_volume                     4041.0(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9524
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      30.53

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.411
_exptl_crystal_size_mid          0.279
_exptl_crystal_size_min          0.188
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2014
_exptl_absorpt_coefficient_mu    1.147
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6942
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            210698
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.15
_diffrn_reflns_theta_max         30.57
_reflns_number_total             24707
_reflns_number_gt                21043
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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)+(0.0385P)²+4.2452P] 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         24707
_refine_ls_number_parameters     1223
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0353
_refine_ls_wR_factor_ref         0.0910
_refine_ls_wR_factor_gt          0.0844
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.005
_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
O9 O -0.00529(13) 0.95069(13) 0.12241(12) 0.0339(4) Uani 0.75 1 d P A 1
H9A H 0.0374 0.9047 0.1132 0.051 Uiso 0.75 1 calc PR A 1
C79 C 0.0267(3) 1.0199(2) 0.0780(2) 0.0452(7) Uani 0.75 1 d P A 1
H79A H -0.0264 1.0701 0.0715 0.068 Uiso 0.75 1 calc PR A 1
H79B H 0.0675 1.0047 0.0257 0.068 Uiso 0.75 1 calc PR A 1
H79C H 0.0613 1.0332 0.1057 0.068 Uiso 0.75 1 calc PR A 1
O10 O 0.5199(5) 0.4708(5) 0.4065(5) 0.0509(18) Uani 0.25 1 d P B 1
H10A H 0.5699 0.4457 0.4181 0.076 Uiso 0.25 1 calc PR B 1
C80 C 0.4658(6) 0.5216(6) 0.4562(6) 0.0364(18) Uani 0.25 1 d P B 1
H80A H 0.4403 0.4889 0.5061 0.055 Uiso 0.25 1 calc PR B 1
H80B H 0.4150 0.5616 0.4354 0.055 Uiso 0.25 1 calc PR B 1
H80C H 0.5001 0.5536 0.4655 0.055 Uiso 0.25 1 calc PR B 1
O1W O 0.0779(9) 0.9934(8) 0.0083(7) 0.091(3) Uani 0.25 1 d P C 2
O2W O 0.4354(10) 0.4998(7) 0.5251(8) 0.042(3) Uani 0.13 1 d P D 2
O3W O 0.4158(11) 0.5463(9) 0.4184(9) 0.049(4) Uani 0.12 1 d P E 2
Ni1 Ni 0.556752(13) 0.145659(13) 0.432490(12) 0.01456(4) Uani 1 1 d U . .
Ni2 Ni 0.567665(13) -0.041212(12) 0.419912(11) 0.01309(4) Uani 1 1 d . . .
Cl2 Cl 0.88653(4) 0.11055(4) 0.74144(4) 0.03989(12) Uani 1 1 d . . .
F4 F 0.92415(10) -0.01385(11) 0.62235(12) 0.0618(5) Uani 1 1 d . . .
F5 F 0.84973(13) -0.05976(9) 0.74291(11) 0.0588(5) Uani 1 1 d . . .
F6 F 0.81000(10) -0.06303(8) 0.63964(9) 0.0429(3) Uani 1 1 d . . .
O1 O 0.65606(7) 0.02483(7) 0.42718(6) 0.0145(2) Uani 1 1 d . . .
O2 O 0.81093(8) 0.03459(8) 0.36639(7) 0.0198(2) Uani 1 1 d . . .
O3 O 0.46398(7) 0.07025(7) 0.45355(6) 0.01377(19) Uani 1 1 d . . .
O4 O 0.32212(8) 0.07978(8) 0.43483(7) 0.0192(2) Uani 1 1 d . . .
H4A H 0.3230 0.0471 0.4775 0.029 Uiso 1 1 calc R . .
N1 N 0.62785(9) 0.14657(9) 0.30721(8) 0.0180(3) Uani 1 1 d . . .
N2 N 0.70139(9) -0.12230(9) 0.37244(8) 0.0162(2) Uani 1 1 d . . .
N4 N 0.53155(9) 0.02013(9) 0.31110(8) 0.0169(2) Uani 1 1 d . . .
N3 N 0.43076(9) 0.23980(9) 0.42068(8) 0.0174(2) Uani 1 1 d . . .
N5 N 0.62423(11) 0.22598(10) 0.43527(10) 0.0248(3) Uani 1 1 d U . .
N6 N 0.68730(14) 0.33932(12) 0.43664(13) 0.0378(4) Uani 1 1 d . . .
N7 N 0.50640(9) 0.12679(9) 0.56217(8) 0.0168(2) Uani 1 1 d U . .
N8 N 0.53609(10) 0.20921(9) 0.64217(9) 0.0213(3) Uani 1 1 d U . .
C1 C 0.60455(12) 0.21144(11) 0.24851(10) 0.0226(3) Uani 1 1 d . . .
H1 H 0.5492 0.2577 0.2622 0.027 Uiso 1 1 calc R . .
C2 C 0.66004(13) 0.21193(13) 0.16835(11) 0.0272(4) Uani 1 1 d . . .
H2 H 0.6420 0.2575 0.1291 0.033 Uiso 1 1 calc R . .
C3 C 0.74282(13) 0.14333(13) 0.14799(11) 0.0280(4) Uani 1 1 d . . .
H3 H 0.7809 0.1418 0.0947 0.034 Uiso 1 1 calc R . .
C4 C 0.76818(12) 0.07667(12) 0.20852(10) 0.0230(3) Uani 1 1 d . . .
H4 H 0.8237 0.0303 0.1965 0.028 Uiso 1 1 calc R . .
C5 C 0.70894(11) 0.08092(10) 0.28722(9) 0.0176(3) Uani 1 1 d . . .
C6 C 0.73375(10) 0.01438(10) 0.35943(9) 0.0160(3) Uani 1 1 d . . .
C7 C 0.76809(11) -0.08115(10) 0.34293(9) 0.0169(3) Uani 1 1 d . . .
C8 C 0.86176(12) -0.12361(12) 0.30295(11) 0.0230(3) Uani 1 1 d . . .
H8 H 0.9064 -0.0937 0.2819 0.028 Uiso 1 1 calc R . .
C9 C 0.88734(12) -0.21137(12) 0.29504(11) 0.0260(4) Uani 1 1 d . . .
H9 H 0.9491 -0.2407 0.2677 0.031 Uiso 1 1 calc R . .
C10 C 0.81962(13) -0.25460(12) 0.32838(11) 0.0245(3) Uani 1 1 d . . .
H10 H 0.8358 -0.3139 0.3258 0.029 Uiso 1 1 calc R . .
C11 C 0.72714(12) -0.20766(11) 0.36575(10) 0.0205(3) Uani 1 1 d . . .
H11 H 0.6814 -0.2363 0.3869 0.025 Uiso 1 1 calc R . .
C12 C 0.83659(13) -0.00330(13) 0.43994(11) 0.0261(4) Uani 1 1 d . . .
H12A H 0.8887 0.0137 0.4391 0.039 Uiso 1 1 calc R . .
H12B H 0.8548 -0.0658 0.4447 0.039 Uiso 1 1 calc R . .
H12C H 0.7834 0.0168 0.4852 0.039 Uiso 1 1 calc R . .
C23 C 0.57613(12) -0.00509(11) 0.23730(10) 0.0223(3) Uani 1 1 d . . .
H23 H 0.6306 -0.0531 0.2308 0.027 Uiso 1 1 calc R . .
C22 C 0.54428(15) 0.03741(13) 0.17046(11) 0.0296(4) Uani 1 1 d . . .
H22 H 0.5771 0.0186 0.1201 0.036 Uiso 1 1 calc R . .
C21 C 0.46216(15) 0.10874(13) 0.18005(11) 0.0300(4) Uani 1 1 d . . .
H21 H 0.4393 0.1387 0.1362 0.036 Uiso 1 1 calc R . .
C20 C 0.41520(13) 0.13427(12) 0.25623(10) 0.0232(3) Uani 1 1 d . . .
H20 H 0.3597 0.1812 0.2644 0.028 Uiso 1 1 calc R . .
C19 C 0.45209(11) 0.08873(10) 0.32034(9) 0.0161(3) Uani 1 1 d . . .
C13 C 0.40518(13) 0.32457(11) 0.42872(11) 0.0235(3) Uani 1 1 d . . .
H13 H 0.4489 0.3459 0.4348 0.028 Uiso 1 1 calc R . .
C14 C 0.31550(13) 0.38141(12) 0.42824(12) 0.0288(4) Uani 1 1 d . . .
H14 H 0.2994 0.4398 0.4342 0.035 Uiso 1 1 calc R . .
C15 C 0.25036(13) 0.34990(12) 0.41874(13) 0.0295(4) Uani 1 1 d . . .
H15 H 0.1902 0.3869 0.4176 0.035 Uiso 1 1 calc R . .
C16 C 0.27639(12) 0.26225(12) 0.41089(11) 0.0225(3) Uani 1 1 d . . .
H16 H 0.2337 0.2395 0.4049 0.027 Uiso 1 1 calc R . .
C17 C 0.36739(11) 0.20885(10) 0.41209(9) 0.0164(3) Uani 1 1 d . . .
C18 C 0.40140(10) 0.11055(10) 0.40741(9) 0.0148(3) Uani 1 1 d . . .
C24 C 0.65651(13) 0.27664(13) 0.43867(12) 0.0267(4) Uani 1 1 d U . .
Cl1 Cl 1.02921(4) 0.27453(5) 0.53817(4) 0.04085(13) Uani 0.90 1 d P F 1
F1 F 0.86756(12) 0.52574(10) 0.42424(12) 0.0495(4) Uani 0.90 1 d P F 1
F2 F 1.00920(10) 0.43742(10) 0.41030(9) 0.0416(3) Uani 0.90 1 d P F 1
F3 F 0.91921(11) 0.47244(11) 0.52820(10) 0.0478(4) Uani 0.90 1 d P F 1
C25 C 0.76840(16) 0.31983(15) 0.46049(14) 0.0261(4) Uani 0.90 1 d P F 1
C26 C 0.80370(15) 0.38942(14) 0.45106(14) 0.0280(4) Uani 0.90 1 d P F 1
H26 H 0.7731 0.4448 0.4288 0.034 Uiso 0.90 1 calc PR F 1
C27 C 0.88309(16) 0.37712(16) 0.47421(14) 0.0277(4) Uani 0.90 1 d P F 1
C28 C 0.92886(15) 0.29408(17) 0.50835(13) 0.0284(4) Uani 0.90 1 d P F 1
C29 C 0.89576(17) 0.22445(16) 0.51743(13) 0.0301(4) Uani 0.90 1 d P F 1
H29 H 0.9267 0.1692 0.5396 0.036 Uiso 0.90 1 calc PR F 1
C30 C 0.81707(16) 0.23682(15) 0.49371(13) 0.0277(4) Uani 0.90 1 d P F 1
H30 H 0.7959 0.1895 0.4998 0.033 Uiso 0.90 1 calc PR F 1
C31 C 0.91959(17) 0.45284(16) 0.45933(16) 0.0354(5) Uani 0.90 1 d P F 1
Cl1' Cl 1.0030(5) 0.3552(6) 0.5223(4) 0.0538(17) Uani 0.10 1 d P F 2
F1' F 0.9299(13) 0.1228(11) 0.5242(12) 0.062(4) Uani 0.10 1 d P F 2
F2' F 1.0425(10) 0.1788(11) 0.4665(9) 0.052(4) Uani 0.10 1 d P F 2
F3' F 0.9722(14) 0.1813(16) 0.5953(9) 0.079(6) Uani 0.10 1 d P F 2
C25' C 0.7430(10) 0.3572(11) 0.4667(11) 0.036(2) Uani 0.10 1 d PG F 2
C26' C 0.7627(10) 0.4339(9) 0.4612(10) 0.036(2) Uani 0.10 1 d PG F 2
H26' H 0.7219 0.4875 0.4461 0.043 Uiso 0.10 1 calc PR F 2
C27' C 0.8433(11) 0.4305(9) 0.4782(10) 0.036(2) Uani 0.10 1 d PG F 2
H27' H 0.8564 0.4818 0.4746 0.043 Uiso 0.10 1 calc PR F 2
C28' C 0.9043(9) 0.3503(11) 0.5008(10) 0.036(2) Uani 0.10 1 d PG F 2
C29' C 0.8846(10) 0.2736(9) 0.5063(10) 0.036(2) Uani 0.10 1 d PG F 2
C30' C 0.8040(11) 0.2771(9) 0.4892(11) 0.036(2) Uani 0.10 1 d PG F 2
H30' H 0.7909 0.2257 0.4929 0.043 Uiso 0.10 1 calc PR F 2
C31' C 0.9554(17) 0.1872(16) 0.5236(14) 0.041(5) Uani 0.10 1 d P F 2
C32 C 0.52371(11) 0.16351(10) 0.60209(10) 0.0174(3) Uani 1 1 d U . .
C33 C 0.62027(12) 0.18179(11) 0.66474(10) 0.0199(3) Uani 1 1 d . . .
C34 C 0.68645(12) 0.09846(11) 0.65709(10) 0.0208(3) Uani 1 1 d . . .
H34 H 0.6754 0.0582 0.6363 0.025 Uiso 1 1 calc R . .
C35 C 0.76868(13) 0.07519(12) 0.68027(11) 0.0240(3) Uani 1 1 d . . .
C36 C 0.78513(13) 0.13527(13) 0.71182(11) 0.0258(3) Uani 1 1 d . . .
C37 C 0.71967(13) 0.21747(13) 0.72037(11) 0.0257(3) Uani 1 1 d . . .
H37 H 0.7305 0.2572 0.7420 0.031 Uiso 1 1 calc R . .
C38 C 0.63812(13) 0.24096(12) 0.69696(11) 0.0244(3) Uani 1 1 d . . .
H38 H 0.5948 0.2965 0.7027 0.029 Uiso 1 1 calc R . .
C39 C 0.83787(16) -0.01472(14) 0.67111(16) 0.0379(5) Uani 1 1 d . . .
Ni3 Ni 0.969715(14) 0.347174(13) 0.002015(13) 0.01628(4) Uani 1 1 d U . .
Ni4 Ni 1.053409(13) 0.507421(13) -0.093268(12) 0.01451(4) Uani 1 1 d . . .
Cl3 Cl 0.55327(4) 0.52334(5) -0.24685(4) 0.05117(17) Uani 1 1 d . . .
Cl4 Cl 0.46050(3) 0.29102(4) -0.10899(4) 0.03728(11) Uani 1 1 d . . .
F7 F 0.57066(10) 0.66983(10) -0.18357(10) 0.0515(4) Uani 1 1 d . . .
F8 F 0.64914(9) 0.63027(9) -0.09719(9) 0.0418(3) Uani 1 1 d . . .
F9 F 0.54603(9) 0.56845(11) -0.08414(10) 0.0520(4) Uani 1 1 d . . .
F10 F 0.56475(10) 0.10170(9) -0.14479(7) 0.0387(3) Uani 1 1 d . . .
F11 F 0.50280(10) 0.10112(10) -0.01639(8) 0.0421(3) Uani 1 1 d . . .
F12 F 0.64451(11) 0.01895(9) -0.06332(10) 0.0489(4) Uani 1 1 d . . .
O5 O 0.86089(7) 0.44415(7) 0.05769(7) 0.0155(2) Uani 1 1 d . . .
O6 O 0.72096(8) 0.40360(8) 0.11286(8) 0.0212(2) Uani 1 1 d . . .
O7 O 1.05364(7) 0.41752(7) 0.01225(7) 0.0145(2) Uani 1 1 d . . .
O8 O 1.20559(8) 0.39568(8) 0.01731(8) 0.0205(2) Uani 1 1 d . . .
H8A H 1.1883 0.4474 -0.0013 0.031 Uiso 1 1 calc R . .
N11 N 1.10398(10) 0.25950(9) -0.02573(9) 0.0200(3) Uani 1 1 d U . .
N12 N 1.01350(10) 0.38772(10) 0.16854(8) 0.0199(3) Uani 1 1 d . . .
N9 N 0.92917(10) 0.28550(10) 0.12255(9) 0.0220(3) Uani 1 1 d . . .
N10 N 0.81543(10) 0.53708(10) 0.17302(8) 0.0202(3) Uani 1 1 d . . .
N13 N 0.90615(11) 0.28403(10) -0.03262(10) 0.0263(3) Uani 1 1 d U . .
N14 N 0.83976(11) 0.18424(10) -0.05769(9) 0.0228(3) Uani 1 1 d U . .
N15 N 0.98973(9) 0.42906(9) -0.11282(8) 0.0181(3) Uani 1 1 d . . .
N16 N 0.94684(11) 0.40672(10) -0.22394(9) 0.0233(3) Uani 1 1 d . . .
C52 C 1.13144(13) 0.18899(12) -0.06270(12) 0.0262(4) Uani 1 1 d . . .
H52 H 1.0867 0.1763 -0.0766 0.031 Uiso 1 1 calc R . .
C53 C 1.22408(14) 0.13432(13) -0.08091(14) 0.0335(4) Uani 1 1 d . . .
H53 H 1.2412 0.0854 -0.1061 0.040 Uiso 1 1 calc R . .
C54 C 1.29110(13) 0.15393(14) -0.06078(15) 0.0349(4) Uani 1 1 d . . .
H54 H 1.3540 0.1188 -0.0732 0.042 Uiso 1 1 calc R . .
C55 C 1.26275(12) 0.22669(12) -0.02190(12) 0.0266(4) Uani 1 1 d . . .
H55 H 1.3063 0.2408 -0.0076 0.032 Uiso 1 1 calc R . .
C56 C 1.16810(11) 0.27798(11) -0.00483(10) 0.0191(3) Uani 1 1 d . . .
C57 C 1.13094(10) 0.36018(10) 0.03698(10) 0.0165(3) Uani 1 1 d . . .
C58 C 1.09996(11) 0.33878(11) 0.12981(10) 0.0192(3) Uani 1 1 d . . .
C59 C 1.16016(13) 0.27514(12) 0.17091(12) 0.0261(4) Uani 1 1 d . . .
H59 H 1.2204 0.2436 0.1427 0.031 Uiso 1 1 calc R . .
C60 C 1.12900(16) 0.25947(14) 0.25442(12) 0.0327(4) Uani 1 1 d . . .
H60 H 1.1680 0.2171 0.2832 0.039 Uiso 1 1 calc R . .
C61 C 1.03952(16) 0.30749(15) 0.29425(12) 0.0351(4) Uani 1 1 d . . .
H61 H 1.0164 0.2967 0.3502 0.042 Uiso 1 1 calc R . .
C62 C 0.98395(14) 0.37239(13) 0.24969(11) 0.0280(4) Uani 1 1 d . . .
H62 H 0.9245 0.4062 0.2770 0.034 Uiso 1 1 calc R . .
C40 C 0.97362(13) 0.20553(12) 0.15408(13) 0.0288(4) Uani 1 1 d . . .
H40 H 1.0326 0.1748 0.1231 0.035 Uiso 1 1 calc R . .
C41 C 0.93562(14) 0.16662(13) 0.23080(13) 0.0318(4) Uani 1 1 d . . .
H41 H 0.9682 0.1108 0.2505 0.038 Uiso 1 1 calc R . .
C42 C 0.84870(14) 0.21223(13) 0.27723(12) 0.0297(4) Uani 1 1 d . . .
H42 H 0.8215 0.1876 0.3288 0.036 Uiso 1 1 calc R . .
C43 C 0.80240(13) 0.29537(12) 0.24580(11) 0.0249(3) Uani 1 1 d . . .
H43 H 0.7439 0.3277 0.2761 0.030 Uiso 1 1 calc R . .
C44 C 0.84486(11) 0.32958(11) 0.16820(10) 0.0202(3) Uani 1 1 d . . .
C45 C 0.79697(11) 0.41896(11) 0.12696(10) 0.0178(3) Uani 1 1 d . . .
C46 C 0.75667(11) 0.49153(12) 0.18167(10) 0.0203(3) Uani 1 1 d . . .
C47 C 0.66537(12) 0.51168(14) 0.23467(11) 0.0286(4) Uani 1 1 d . . .
H47 H 0.6266 0.4780 0.2418 0.034 Uiso 1 1 calc R . .
C48 C 0.63293(13) 0.58239(17) 0.27665(13) 0.0369(5) Uani 1 1 d . . .
H48 H 0.5719 0.5972 0.3119 0.044 Uiso 1 1 calc R . .
C49 C 0.69256(14) 0.63069(17) 0.26550(14) 0.0386(5) Uani 1 1 d . . .
H49 H 0.6717 0.6793 0.2920 0.046 Uiso 1 1 calc R . .
C50 C 0.78388(13) 0.60536(14) 0.21408(12) 0.0289(4) Uani 1 1 d . . .
H50 H 0.8246 0.6367 0.2078 0.035 Uiso 1 1 calc R . .
C51 C 0.67843(12) 0.46787(12) 0.05602(11) 0.0235(3) Uani 1 1 d . . .
H51A H 0.6282 0.4525 0.0505 0.035 Uiso 1 1 calc R . .
H51B H 0.7253 0.4704 0.0045 0.035 Uiso 1 1 calc R . .
H51C H 0.6532 0.5239 0.0748 0.035 Uiso 1 1 calc R . .
C63 C 0.96553(11) 0.42123(10) -0.16635(10) 0.0181(3) Uani 1 1 d . . .
C64 C 0.85364(13) 0.44002(12) -0.22957(10) 0.0224(3) Uani 1 1 d . . .
C65 C 0.78198(12) 0.50430(11) -0.18433(10) 0.0218(3) Uani 1 1 d . . .
H65 H 0.7964 0.5289 -0.1505 0.026 Uiso 1 1 calc R . .
C66 C 0.68948(13) 0.53174(12) -0.18937(11) 0.0261(4) Uani 1 1 d . . .
C67 C 0.66865(14) 0.49486(14) -0.24090(13) 0.0324(4) Uani 1 1 d . . .
C68 C 0.73941(17) 0.43407(14) -0.28789(13) 0.0354(5) Uani 1 1 d . . .
H68 H 0.7253 0.4115 -0.3234 0.042 Uiso 1 1 calc R . .
C69 C 0.83143(16) 0.40627(13) -0.28274(12) 0.0306(4) Uani 1 1 d . . .
H69 H 0.8785 0.3652 -0.3146 0.037 Uiso 1 1 calc R . .
C70 C 0.61447(14) 0.59981(14) -0.13866(14) 0.0345(4) Uani 1 1 d . . .
C71 C 0.87113(11) 0.24031(11) -0.04537(10) 0.0203(3) Uani 1 1 d U . .
C72 C 0.74950(11) 0.21207(11) -0.06763(10) 0.0188(3) Uani 1 1 d . . .
C73 C 0.71128(12) 0.14771(11) -0.06768(10) 0.0214(3) Uani 1 1 d . . .
H73 H 0.7463 0.0891 -0.0604 0.026 Uiso 1 1 calc R . .
C74 C 0.62208(13) 0.17013(12) -0.07836(10) 0.0224(3) Uani 1 1 d . . .
C75 C 0.56973(12) 0.25821(13) -0.08999(11) 0.0247(3) Uani 1 1 d . . .
C76 C 0.60527(13) 0.32254(12) -0.08839(11) 0.0253(3) Uani 1 1 d . . .
H76 H 0.5694 0.3810 -0.0946 0.030 Uiso 1 1 calc R . .
C77 C 0.69417(12) 0.30001(11) -0.07750(11) 0.0220(3) Uani 1 1 d . . .
H77 H 0.7174 0.3437 -0.0767 0.026 Uiso 1 1 calc R . .
C78 C 0.58411(15) 0.09862(14) -0.07656(12) 0.0299(4) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O9 C79 1.380(4) . ?
O9 H9A 0.8200 . ?
C79 H79A 0.9600 . ?
C79 H79B 0.9600 . ?
C79 H79C 0.9600 . ?
O10 C80 1.238(11) . ?
O10 H10A 0.8200 . ?
C80 H80A 0.9600 . ?
C80 H80B 0.9600 . ?
C80 H80C 0.9600 . ?
Ni1 N5 2.0068(15) . ?
Ni1 O1 2.0453(11) . ?
Ni1 N3 2.0774(13) . ?
Ni1 N1 2.1180(14) . ?
Ni1 O3 2.1423(11) . ?
Ni1 N7 2.1469(14) . ?
Ni2 O3 2.0268(11) . ?
Ni2 N7 2.0554(14) 2_656 ?
Ni2 N2 2.0563(13) . ?
Ni2 O3 2.1019(11) 2_656 ?
Ni2 O1 2.1189(11) . ?
Ni2 N4 2.1217(14) . ?
Cl2 C36 1.7395(18) . ?
F4 C39 1.341(3) . ?
F5 C39 1.352(3) . ?
F6 C39 1.342(2) . ?
O1 C6 1.3811(18) . ?
O2 C6 1.4299(19) . ?
O2 C12 1.435(2) . ?
O3 C18 1.3852(17) . ?
O3 Ni2 2.1018(11) 2_656 ?
O4 C18 1.4111(18) . ?
O4 H4A 0.8200 . ?
N1 C5 1.345(2) . ?
N1 C1 1.348(2) . ?
N2 C11 1.346(2) . ?
N2 C7 1.349(2) . ?
N4 C19 1.343(2) . ?
N4 C23 1.344(2) . ?
N3 C13 1.343(2) . ?
N3 C17 1.347(2) . ?
N5 C24 1.154(2) . ?
N6 C24 1.288(3) . ?
N6 C25' 1.323(11) . ?
N6 C25 1.394(3) . ?
N7 C32 1.192(2) . ?
N7 Ni2 2.0554(14) 2_656 ?
N8 C32 1.262(2) . ?
N8 C33 1.409(2) . ?
C1 C2 1.390(2) . ?
C1 H1 0.9300 . ?
C2 C3 1.387(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.393(2) . ?
C3 H3 0.9300 . ?
C4 C5 1.389(2) . ?
C4 H4 0.9300 . ?
C5 C6 1.539(2) . ?
C6 C7 1.543(2) . ?
C7 C8 1.395(2) . ?
C8 C9 1.390(3) . ?
C8 H8 0.9300 . ?
C9 C10 1.387(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.390(2) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C23 C22 1.385(2) . ?
C23 H23 0.9300 . ?
C22 C21 1.392(3) . ?
C22 H22 0.9300 . ?
C21 C20 1.385(3) . ?
C21 H21 0.9300 . ?
C20 C19 1.392(2) . ?
C20 H20 0.9300 . ?
C19 C18 1.540(2) . ?
C13 C14 1.389(2) . ?
C13 H13 0.9300 . ?
C14 C15 1.387(3) . ?
C14 H14 0.9300 . ?
C15 C16 1.387(3) . ?
C15 H15 0.9300 . ?
C16 C17 1.392(2) . ?
C16 H16 0.9300 . ?
C17 C18 1.533(2) . ?
Cl1 C28 1.743(2) . ?
F1 C31 1.339(3) . ?
F2 C31 1.348(3) . ?
F3 C31 1.341(3) . ?
C25 C26 1.408(3) . ?
C25 C30 1.409(3) . ?
C26 C27 1.387(3) . ?
C26 H26 0.9300 . ?
C27 C28 1.400(3) . ?
C27 C31 1.498(3) . ?
C28 C29 1.388(3) . ?
C29 C30 1.382(3) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
Cl1' C28' 1.766(13) . ?
F1' C31' 1.27(3) . ?
F2' C31' 1.38(3) . ?
F3' C31' 1.37(3) . ?
C25' C26' 1.3900 . ?
C25' C30' 1.3900 . ?
C26' C27' 1.3900 . ?
C26' H26' 0.9300 . ?
C27' C28' 1.3900 . ?
C27' H27' 0.9300 . ?
C28' C29' 1.3900 . ?
C29' C30' 1.3900 . ?
C29' C31' 1.50(3) . ?
C30' H30' 0.9300 . ?
C33 C34 1.400(2) . ?
C33 C38 1.401(2) . ?
C34 C35 1.394(2) . ?
C34 H34 0.9300 . ?
C35 C36 1.394(3) . ?
C35 C39 1.500(3) . ?
C36 C37 1.384(3) . ?
C37 C38 1.385(3) . ?
C37 H37 0.9300 . ?
C38 H38 0.9300 . ?
Ni3 N13 2.0021(15) . ?
Ni3 O5 2.0246(12) . ?
Ni3 N11 2.0575(14) . ?
Ni3 N9 2.1238(15) . ?
Ni3 O7 2.1365(11) . ?
Ni3 N15 2.1522(14) . ?
Ni4 O7 2.0324(11) 2_765 ?
Ni4 N10 2.0502(14) 2_765 ?
Ni4 N15 2.0617(14) . ?
Ni4 O7 2.0944(11) . ?
Ni4 N12 2.1094(14) 2_765 ?
Ni4 O5 2.1287(11) 2_765 ?
Cl3 C67 1.7460(19) . ?
Cl4 C75 1.7406(18) . ?
F7 C70 1.347(2) . ?
F8 C70 1.330(3) . ?
F9 C70 1.348(2) . ?
F10 C78 1.338(2) . ?
F11 C78 1.351(2) . ?
F12 C78 1.341(3) . ?
O5 C45 1.3802(18) . ?
O5 Ni4 2.1287(11) 2_765 ?
O6 C51 1.428(2) . ?
O6 C45 1.4286(18) . ?
O7 C57 1.3844(18) . ?
O7 Ni4 2.0325(11) 2_765 ?
O8 C57 1.4084(18) . ?
O8 H8A 0.8200 . ?
N11 C52 1.340(2) . ?
N11 C56 1.345(2) . ?
N12 C62 1.344(2) . ?
N12 C58 1.345(2) . ?
N12 Ni4 2.1094(14) 2_765 ?
N9 C44 1.340(2) . ?
N9 C40 1.342(2) . ?
N10 C50 1.343(2) . ?
N10 C46 1.347(2) . ?
N10 Ni4 2.0502(14) 2_765 ?
N13 C71 1.161(2) . ?
N14 C71 1.294(2) . ?
N14 C72 1.393(2) . ?
N15 C63 1.193(2) . ?
N16 C63 1.258(2) . ?
N16 C64 1.404(2) . ?
C52 C53 1.385(3) . ?
C52 H52 0.9300 . ?
C53 C54 1.391(3) . ?
C53 H53 0.9300 . ?
C54 C55 1.390(3) . ?
C54 H54 0.9300 . ?
C55 C56 1.392(2) . ?
C55 H55 0.9300 . ?
C56 C57 1.538(2) . ?
C57 C58 1.541(2) . ?
C58 C59 1.390(2) . ?
C59 C60 1.384(3) . ?
C59 H59 0.9300 . ?
C60 C61 1.376(3) . ?
C60 H60 0.9300 . ?
C61 C62 1.393(3) . ?
C61 H61 0.9300 . ?
C62 H62 0.9300 . ?
C40 C41 1.387(3) . ?
C40 H40 0.9300 . ?
C41 C42 1.378(3) . ?
C41 H41 0.9300 . ?
C42 C43 1.387(3) . ?
C42 H42 0.9300 . ?
C43 C44 1.389(2) . ?
C43 H43 0.9300 . ?
C44 C45 1.532(2) . ?
C45 C46 1.544(2) . ?
C46 C47 1.392(2) . ?
C47 C48 1.385(3) . ?
C47 H47 0.9300 . ?
C48 C49 1.384(3) . ?
C48 H48 0.9300 . ?
C49 C50 1.387(3) . ?
C49 H49 0.9300 . ?
C50 H50 0.9300 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C64 C69 1.403(2) . ?
C64 C65 1.404(3) . ?
C65 C66 1.394(2) . ?
C65 H65 0.9300 . ?
C66 C67 1.399(3) . ?
C66 C70 1.507(3) . ?
C67 C68 1.380(3) . ?
C68 C69 1.387(3) . ?
C68 H68 0.9300 . ?
C69 H69 0.9300 . ?
C72 C77 1.405(2) . ?
C72 C73 1.407(2) . ?
C73 C74 1.391(2) . ?
C73 H73 0.9300 . ?
C74 C75 1.397(3) . ?
C74 C78 1.503(2) . ?
C75 C76 1.386(3) . ?
C76 C77 1.388(2) . ?
C76 H76 0.9300 . ?
C77 H77 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O9 C79 H79A 109.5 . . ?
O9 C79 H79B 109.5 . . ?
H79A C79 H79B 109.5 . . ?
O9 C79 H79C 109.5 . . ?
H79A C79 H79C 109.5 . . ?
H79B C79 H79C 109.5 . . ?
O10 C80 H80A 109.5 . . ?
O10 C80 H80B 109.5 . . ?
H80A C80 H80B 109.5 . . ?
O10 C80 H80C 109.5 . . ?
H80A C80 H80C 109.5 . . ?
H80B C80 H80C 109.5 . . ?
N5 Ni1 O1 105.22(6) . . ?
N5 Ni1 N3 98.03(6) . . ?
O1 Ni1 N3 155.60(5) . . ?
N5 Ni1 N1 88.29(6) . . ?
O1 Ni1 N1 77.14(5) . . ?
N3 Ni1 N1 96.53(5) . . ?
N5 Ni1 O3 167.52(5) . . ?
O1 Ni1 O3 81.85(4) . . ?
N3 Ni1 O3 76.72(5) . . ?
N1 Ni1 O3 103.45(5) . . ?
N5 Ni1 N7 90.91(6) . . ?
O1 Ni1 N7 93.52(5) . . ?
N3 Ni1 N7 93.40(5) . . ?
N1 Ni1 N7 170.05(5) . . ?
O3 Ni1 N7 78.24(5) . . ?
O3 Ni2 N7 103.09(5) . 2_656 ?
O3 Ni2 N2 158.65(5) . . ?
N7 Ni2 N2 98.05(5) 2_656 . ?
O3 Ni2 O3 79.42(5) . 2_656 ?
N7 Ni2 O3 81.23(5) 2_656 2_656 ?
N2 Ni2 O3 107.10(5) . 2_656 ?
O3 Ni2 O1 82.86(4) . . ?
N7 Ni2 O1 164.92(5) 2_656 . ?
N2 Ni2 O1 77.40(5) . . ?
O3 Ni2 O1 86.36(4) 2_656 . ?
O3 Ni2 N4 77.55(5) . . ?
N7 Ni2 N4 90.68(5) 2_656 . ?
N2 Ni2 N4 99.36(5) . . ?
O3 Ni2 N4 153.14(5) 2_656 . ?
O1 Ni2 N4 104.20(5) . . ?
C6 O1 Ni1 117.08(9) . . ?
C6 O1 Ni2 108.23(9) . . ?
Ni1 O1 Ni2 96.22(4) . . ?
C6 O2 C12 115.44(12) . . ?
C18 O3 Ni2 117.33(9) . . ?
C18 O3 Ni2 128.10(9) . 2_656 ?
Ni2 O3 Ni2 100.59(4) . 2_656 ?
C18 O3 Ni1 109.85(9) . . ?
Ni2 O3 Ni1 96.05(4) . . ?
Ni2 O3 Ni1 99.16(4) 2_656 . ?
C18 O4 H4A 109.5 . . ?
C5 N1 C1 118.32(14) . . ?
C5 N1 Ni1 115.66(10) . . ?
C1 N1 Ni1 125.56(12) . . ?
C11 N2 C7 118.81(14) . . ?
C11 N2 Ni2 127.78(11) . . ?
C7 N2 Ni2 113.37(10) . . ?
C19 N4 C23 118.41(14) . . ?
C19 N4 Ni2 114.30(10) . . ?
C23 N4 Ni2 127.19(11) . . ?
C13 N3 C17 118.98(14) . . ?
C13 N3 Ni1 125.75(12) . . ?
C17 N3 Ni1 114.93(10) . . ?
C24 N5 Ni1 174.92(16) . . ?
C24 N6 C25' 140.8(8) . . ?
C24 N6 C25 119.01(19) . . ?
C32 N7 Ni2 138.03(12) . 2_656 ?
C32 N7 Ni1 121.47(12) . . ?
Ni2 N7 Ni1 100.49(6) 2_656 . ?
C32 N8 C33 120.19(14) . . ?
N1 C1 C2 122.52(16) . . ?
N1 C1 H1 118.7 . . ?
C2 C1 H1 118.7 . . ?
C3 C2 C1 118.82(16) . . ?
C3 C2 H2 120.6 . . ?
C1 C2 H2 120.6 . . ?
C2 C3 C4 119.04(16) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C5 C4 C3 118.68(16) . . ?
C5 C4 H4 120.7 . . ?
C3 C4 H4 120.7 . . ?
N1 C5 C4 122.61(15) . . ?
N1 C5 C6 114.43(13) . . ?
C4 C5 C6 122.85(14) . . ?
O1 C6 O2 113.96(13) . . ?
O1 C6 C5 110.38(12) . . ?
O2 C6 C5 102.11(12) . . ?
O1 C6 C7 108.48(12) . . ?
O2 C6 C7 109.01(12) . . ?
C5 C6 C7 112.89(13) . . ?
N2 C7 C8 121.87(15) . . ?
N2 C7 C6 115.11(13) . . ?
C8 C7 C6 122.99(14) . . ?
C9 C8 C7 118.89(16) . . ?
C9 C8 H8 120.6 . . ?
C7 C8 H8 120.6 . . ?
C10 C9 C8 119.20(16) . . ?
C10 C9 H9 120.4 . . ?
C8 C9 H9 120.4 . . ?
C9 C10 C11 118.75(16) . . ?
C9 C10 H10 120.6 . . ?
C11 C10 H10 120.6 . . ?
N2 C11 C10 122.40(16) . . ?
N2 C11 H11 118.8 . . ?
C10 C11 H11 118.8 . . ?
O2 C12 H12A 109.5 . . ?
O2 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O2 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N4 C23 C22 122.72(16) . . ?
N4 C23 H23 118.6 . . ?
C22 C23 H23 118.6 . . ?
C23 C22 C21 118.81(16) . . ?
C23 C22 H22 120.6 . . ?
C21 C22 H22 120.6 . . ?
C20 C21 C22 118.70(16) . . ?
C20 C21 H21 120.6 . . ?
C22 C21 H21 120.6 . . ?
C21 C20 C19 119.13(16) . . ?
C21 C20 H20 120.4 . . ?
C19 C20 H20 120.4 . . ?
N4 C19 C20 122.22(15) . . ?
N4 C19 C18 115.62(13) . . ?
C20 C19 C18 122.07(14) . . ?
N3 C13 C14 122.08(17) . . ?
N3 C13 H13 119.0 . . ?
C14 C13 H13 119.0 . . ?
C15 C14 C13 119.07(17) . . ?
C15 C14 H14 120.5 . . ?
C13 C14 H14 120.5 . . ?
C14 C15 C16 118.98(16) . . ?
C14 C15 H15 120.5 . . ?
C16 C15 H15 120.5 . . ?
C15 C16 C17 118.96(17) . . ?
C15 C16 H16 120.5 . . ?
C17 C16 H16 120.5 . . ?
N3 C17 C16 121.93(15) . . ?
N3 C17 C18 115.19(13) . . ?
C16 C17 C18 122.83(15) . . ?
O3 C18 O4 112.61(12) . . ?
O3 C18 C17 107.68(12) . . ?
O4 C18 C17 109.10(12) . . ?
O3 C18 C19 108.87(12) . . ?
O4 C18 C19 105.92(12) . . ?
C17 C18 C19 112.74(12) . . ?
N5 C24 N6 173.3(2) . . ?
N6 C25 C26 116.9(2) . . ?
N6 C25 C30 125.42(19) . . ?
C26 C25 C30 117.7(2) . . ?
C27 C26 C25 121.4(2) . . ?
C27 C26 H26 119.3 . . ?
C25 C26 H26 119.3 . . ?
C26 C27 C28 119.53(19) . . ?
C26 C27 C31 118.8(2) . . ?
C28 C27 C31 121.6(2) . . ?
C29 C28 C27 120.0(2) . . ?
C29 C28 Cl1 118.37(18) . . ?
C27 C28 Cl1 121.61(18) . . ?
C30 C29 C28 120.3(2) . . ?
C30 C29 H29 119.9 . . ?
C28 C29 H29 119.9 . . ?
C29 C30 C25 121.1(2) . . ?
C29 C30 H30 119.4 . . ?
C25 C30 H30 119.4 . . ?
F1 C31 F3 106.4(2) . . ?
F1 C31 F2 106.2(2) . . ?
F3 C31 F2 107.05(19) . . ?
F1 C31 C27 112.5(2) . . ?
F3 C31 C27 111.9(2) . . ?
F2 C31 C27 112.34(19) . . ?
N6 C25' C26' 132.0(11) . . ?
N6 C25' C30' 106.0(11) . . ?
C26' C25' C30' 120.0 . . ?
C27' C26' C25' 120.0 . . ?
C27' C26' H26' 120.0 . . ?
C25' C26' H26' 120.0 . . ?
C28' C27' C26' 120.0 . . ?
C28' C27' H27' 120.0 . . ?
C26' C27' H27' 120.0 . . ?
C29' C28' C27' 120.0 . . ?
C29' C28' Cl1' 124.5(10) . . ?
C27' C28' Cl1' 115.5(10) . . ?
C28' C29' C30' 120.0 . . ?
C28' C29' C31' 119.3(15) . . ?
C30' C29' C31' 120.4(15) . . ?
C29' C30' C25' 120.0 . . ?
C29' C30' H30' 120.0 . . ?
C25' C30' H30' 120.0 . . ?
F1' C31' F3' 110(2) . . ?
F1' C31' F2' 107(2) . . ?
F3' C31' F2' 105(2) . . ?
F1' C31' C29' 113(2) . . ?
F3' C31' C29' 111(2) . . ?
F2' C31' C29' 111.1(17) . . ?
N7 C32 N8 174.29(17) . . ?
C34 C33 C38 118.51(16) . . ?
C34 C33 N8 123.37(15) . . ?
C38 C33 N8 118.12(15) . . ?
C35 C34 C33 120.74(16) . . ?
C35 C34 H34 119.6 . . ?
C33 C34 H34 119.6 . . ?
C36 C35 C34 119.73(17) . . ?
C36 C35 C39 121.13(16) . . ?
C34 C35 C39 119.14(16) . . ?
C37 C36 C35 119.93(16) . . ?
C37 C36 Cl2 118.05(14) . . ?
C35 C36 Cl2 122.02(15) . . ?
C36 C37 C38 120.47(16) . . ?
C36 C37 H37 119.8 . . ?
C38 C37 H37 119.8 . . ?
C37 C38 C33 120.61(17) . . ?
C37 C38 H38 119.7 . . ?
C33 C38 H38 119.7 . . ?
F4 C39 F6 106.0(2) . . ?
F4 C39 F5 106.69(18) . . ?
F6 C39 F5 106.55(19) . . ?
F4 C39 C35 112.89(19) . . ?
F6 C39 C35 112.51(16) . . ?
F5 C39 C35 111.8(2) . . ?
N13 Ni3 O5 103.85(6) . . ?
N13 Ni3 N11 97.34(6) . . ?
O5 Ni3 N11 157.13(5) . . ?
N13 Ni3 N9 89.94(6) . . ?
O5 Ni3 N9 77.42(5) . . ?
N11 Ni3 N9 94.26(6) . . ?
N13 Ni3 O7 167.78(6) . . ?
O5 Ni3 O7 83.07(4) . . ?
N11 Ni3 O7 77.72(5) . . ?
N9 Ni3 O7 101.49(5) . . ?
N13 Ni3 N15 91.76(6) . . ?
O5 Ni3 N15 92.52(5) . . ?
N11 Ni3 N15 95.38(6) . . ?
N9 Ni3 N15 169.91(6) . . ?
O7 Ni3 N15 77.73(5) . . ?
O7 Ni4 N10 158.95(5) 2_765 2_765 ?
O7 Ni4 N15 102.88(5) 2_765 . ?
N10 Ni4 N15 98.03(6) 2_765 . ?
O7 Ni4 O7 80.42(5) 2_765 . ?
N10 Ni4 O7 105.58(5) 2_765 . ?
N15 Ni4 O7 80.71(5) . . ?
O7 Ni4 N12 77.44(5) 2_765 2_765 ?
N10 Ni4 N12 100.41(6) 2_765 2_765 ?
N15 Ni4 N12 89.83(6) . 2_765 ?
O7 Ni4 N12 153.30(5) . 2_765 ?
O7 Ni4 O5 83.08(4) 2_765 2_765 ?
N10 Ni4 O5 77.30(5) 2_765 2_765 ?
N15 Ni4 O5 164.51(5) . 2_765 ?
O7 Ni4 O5 86.30(4) . 2_765 ?
N12 Ni4 O5 105.49(5) 2_765 2_765 ?
C45 O5 Ni3 116.63(10) . . ?
C45 O5 Ni4 107.69(9) . 2_765 ?
Ni3 O5 Ni4 95.45(4) . 2_765 ?
C51 O6 C45 115.18(12) . . ?
C57 O7 Ni4 118.01(9) . 2_765 ?
C57 O7 Ni4 128.09(9) . . ?
Ni4 O7 Ni4 99.58(5) 2_765 . ?
C57 O7 Ni3 110.18(9) . . ?
Ni4 O7 Ni3 94.98(4) 2_765 . ?
Ni4 O7 Ni3 99.97(5) . . ?
C57 O8 H8A 109.5 . . ?
C52 N11 C56 119.24(15) . . ?
C52 N11 Ni3 126.05(12) . . ?
C56 N11 Ni3 114.70(11) . . ?
C62 N12 C58 118.37(15) . . ?
C62 N12 Ni4 126.86(13) . 2_765 ?
C58 N12 Ni4 114.25(11) . 2_765 ?
C44 N9 C40 117.95(15) . . ?
C44 N9 Ni3 114.45(11) . . ?
C40 N9 Ni3 127.25(13) . . ?
C50 N10 C46 119.20(15) . . ?
C50 N10 Ni4 127.18(12) . 2_765 ?
C46 N10 Ni4 113.60(11) . 2_765 ?
C71 N13 Ni3 172.28(15) . . ?
C71 N14 C72 119.09(15) . . ?
C63 N15 Ni4 137.44(13) . . ?
C63 N15 Ni3 122.05(12) . . ?
Ni4 N15 Ni3 100.50(6) . . ?
C63 N16 C64 119.97(15) . . ?
N11 C52 C53 122.37(17) . . ?
N11 C52 H52 118.8 . . ?
C53 C52 H52 118.8 . . ?
C52 C53 C54 118.70(18) . . ?
C52 C53 H53 120.7 . . ?
C54 C53 H53 120.7 . . ?
C55 C54 C53 119.11(17) . . ?
C55 C54 H54 120.4 . . ?
C53 C54 H54 120.4 . . ?
C54 C55 C56 118.83(17) . . ?
C54 C55 H55 120.6 . . ?
C56 C55 H55 120.6 . . ?
N11 C56 C55 121.75(16) . . ?
N11 C56 C57 115.97(13) . . ?
C55 C56 C57 122.27(15) . . ?
O7 C57 O8 112.95(12) . . ?
O7 C57 C56 108.44(13) . . ?
O8 C57 C56 108.28(13) . . ?
O7 C57 C58 108.76(12) . . ?
O8 C57 C58 106.50(12) . . ?
C56 C57 C58 111.96(13) . . ?
N12 C58 C59 122.27(16) . . ?
N12 C58 C57 116.20(13) . . ?
C59 C58 C57 121.47(15) . . ?
C60 C59 C58 118.97(18) . . ?
C60 C59 H59 120.5 . . ?
C58 C59 H59 120.5 . . ?
C61 C60 C59 119.02(17) . . ?
C61 C60 H60 120.5 . . ?
C59 C60 H60 120.5 . . ?
C60 C61 C62 119.16(18) . . ?
C60 C61 H61 120.4 . . ?
C62 C61 H61 120.4 . . ?
N12 C62 C61 122.14(19) . . ?
N12 C62 H62 118.9 . . ?
C61 C62 H62 118.9 . . ?
N9 C40 C41 122.96(18) . . ?
N9 C40 H40 118.5 . . ?
C41 C40 H40 118.5 . . ?
C42 C41 C40 118.73(17) . . ?
C42 C41 H41 120.6 . . ?
C40 C41 H41 120.6 . . ?
C41 C42 C43 118.96(17) . . ?
C41 C42 H42 120.5 . . ?
C43 C42 H42 120.5 . . ?
C42 C43 C44 118.85(18) . . ?
C42 C43 H43 120.6 . . ?
C44 C43 H43 120.6 . . ?
N9 C44 C43 122.54(16) . . ?
N9 C44 C45 114.87(14) . . ?
C43 C44 C45 122.54(16) . . ?
O5 C45 O6 114.29(13) . . ?
O5 C45 C44 110.38(13) . . ?
O6 C45 C44 102.30(12) . . ?
O5 C45 C46 107.49(13) . . ?
O6 C45 C46 109.66(13) . . ?
C44 C45 C46 112.81(14) . . ?
N10 C46 C47 121.33(17) . . ?
N10 C46 C45 115.17(13) . . ?
C47 C46 C45 123.46(16) . . ?
C48 C47 C46 119.26(18) . . ?
C48 C47 H47 120.4 . . ?
C46 C47 H47 120.4 . . ?
C49 C48 C47 119.11(17) . . ?
C49 C48 H48 120.4 . . ?
C47 C48 H48 120.4 . . ?
C48 C49 C50 118.8(2) . . ?
C48 C49 H49 120.6 . . ?
C50 C49 H49 120.6 . . ?
N10 C50 C49 122.18(18) . . ?
N10 C50 H50 118.9 . . ?
C49 C50 H50 118.9 . . ?
O6 C51 H51A 109.5 . . ?
O6 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
O6 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
N15 C63 N16 174.57(18) . . ?
C69 C64 C65 118.74(17) . . ?
C69 C64 N16 117.86(17) . . ?
C65 C64 N16 123.39(15) . . ?
C66 C65 C64 120.87(17) . . ?
C66 C65 H65 119.6 . . ?
C64 C65 H65 119.6 . . ?
C65 C66 C67 119.14(19) . . ?
C65 C66 C70 119.07(17) . . ?
C67 C66 C70 121.79(17) . . ?
C68 C67 C66 120.35(17) . . ?
C68 C67 Cl3 118.36(16) . . ?
C66 C67 Cl3 121.28(18) . . ?
C67 C68 C69 120.65(18) . . ?
C67 C68 H68 119.7 . . ?
C69 C68 H68 119.7 . . ?
C68 C69 C64 120.2(2) . . ?
C68 C69 H69 119.9 . . ?
C64 C69 H69 119.9 . . ?
F8 C70 F7 106.21(18) . . ?
F8 C70 F9 106.58(19) . . ?
F7 C70 F9 106.42(16) . . ?
F8 C70 C66 112.77(15) . . ?
F7 C70 C66 112.34(18) . . ?
F9 C70 C66 112.06(18) . . ?
N13 C71 N14 173.63(19) . . ?
N14 C72 C77 124.39(15) . . ?
N14 C72 C73 117.69(15) . . ?
C77 C72 C73 117.92(15) . . ?
C74 C73 C72 121.26(16) . . ?
C74 C73 H73 119.4 . . ?
C72 C73 H73 119.4 . . ?
C73 C74 C75 119.47(16) . . ?
C73 C74 C78 118.98(17) . . ?
C75 C74 C78 121.54(16) . . ?
C76 C75 C74 120.13(16) . . ?
C76 C75 Cl4 117.97(14) . . ?
C74 C75 Cl4 121.88(14) . . ?
C75 C76 C77 120.27(17) . . ?
C75 C76 H76 119.9 . . ?
C77 C76 H76 119.9 . . ?
C76 C77 C72 120.91(16) . . ?
C76 C77 H77 119.5 . . ?
C72 C77 H77 119.5 . . ?
F10 C78 F12 106.73(17) . . ?
F10 C78 F11 106.12(15) . . ?
F12 C78 F11 105.63(16) . . ?
F10 C78 C74 113.76(15) . . ?
F12 C78 C74 112.15(16) . . ?
F11 C78 C74 111.91(17) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        30.57
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.956
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.080
####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1434557'
_audit_update_record             
;
2015-11-02 deposited with the CCDC.
2016-02-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C80 H56 Cl4 F12 N16 Ni4 O8, 2(C2 H6 O)'
_chemical_formula_sum            'C84 H68 Cl4 F12 N16 Ni4 O10'
_chemical_formula_weight         2066.18

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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                   11.4251(11)
_cell_length_b                   13.5149(12)
_cell_length_c                   14.9081(14)
_cell_angle_alpha                70.643(4)
_cell_angle_beta                 84.372(4)
_cell_angle_gamma                84.460(4)
_cell_volume                     2156.3(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1052
_exptl_absorpt_coefficient_mu    1.079
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            43053
_diffrn_reflns_av_R_equivalents  0.0642
_diffrn_reflns_av_sigmaI/netI    0.0631
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.37
_diffrn_reflns_theta_max         28.58
_reflns_number_total             10428
_reflns_number_gt                7918
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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)+(0.0000P)²+23.0529P] 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         10428
_refine_ls_number_parameters     592
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.1205
_refine_ls_R_factor_gt           0.0891
_refine_ls_wR_factor_ref         0.1859
_refine_ls_wR_factor_gt          0.1699
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_restrained_S_all      1.111
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.35919(6) 0.83945(5) 0.01337(5) 0.01383(15) Uani 1 1 d . . .
Ni2 Ni 0.60624(6) 0.92857(5) -0.02388(5) 0.01355(15) Uani 1 1 d . . .
Cl1 Cl 0.1553(2) 0.47536(18) 0.61898(13) 0.0536(5) Uani 1 1 d . . .
Cl2 Cl 0.6880(2) 1.24763(19) -0.64741(14) 0.0613(6) Uani 1 1 d . . .
N1 N 0.4508(4) 0.7286(3) -0.0445(3) 0.0164(9) Uani 1 1 d . . .
N2 N 0.7396(4) 0.8266(3) 0.0410(3) 0.0144(9) Uani 1 1 d . . .
N3 N 0.2535(4) 0.9096(3) -0.0993(3) 0.0168(9) Uani 1 1 d . . .
N4 N 0.6093(4) 0.8947(3) -0.1517(3) 0.0158(9) Uani 1 1 d . . .
N5 N 0.2479(4) 0.7299(4) 0.0891(3) 0.0193(9) Uani 1 1 d . . .
N6 N 0.1960(4) 0.5566(4) 0.2001(3) 0.0244(11) Uani 1 1 d D . .
N7 N 0.7018(4) 1.0604(3) -0.0961(3) 0.0142(9) Uani 1 1 d . . .
N8 N 0.8225(4) 1.0837(4) -0.2459(3) 0.0217(10) Uani 1 1 d . . .
F1 F 0.1121(4) 0.2689(4) 0.5827(3) 0.0575(13) Uani 1 1 d . . .
F2 F 0.2978(5) 0.2893(4) 0.5756(3) 0.0642(14) Uani 1 1 d . . .
F3 F 0.2270(5) 0.2368(3) 0.4725(3) 0.0632(15) Uani 1 1 d . . .
F4 F 0.9607(5) 1.2515(4) -0.6418(3) 0.0707(16) Uani 1 1 d . . .
F5 F 0.9110(5) 1.1017(4) -0.6404(3) 0.0667(15) Uani 1 1 d . . .
F6 F 1.0399(4) 1.1089(4) -0.5478(3) 0.0537(12) Uani 1 1 d . . .
O1 O 0.5132(3) 0.8056(3) 0.0793(2) 0.0135(7) Uani 1 1 d . . .
O2 O 0.5399(3) 0.6245(3) 0.1620(3) 0.0171(8) Uani 1 1 d . . .
O3 O 0.4436(3) 0.9816(3) -0.0657(2) 0.0137(7) Uani 1 1 d . . .
O4 O 0.4471(3) 1.1142(3) -0.2127(3) 0.0175(8) Uani 1 1 d D . .
H4A H 0.460(6) 1.142(5) -0.171(3) 0.026 Uiso 1 1 d D . .
C1 C 0.4160(5) 0.6994(5) -0.1147(4) 0.0228(12) Uani 1 1 d . . .
H1 H 0.3455 0.7322 -0.1436 0.027 Uiso 1 1 calc R . .
C2 C 0.4783(5) 0.6234(5) -0.1469(4) 0.0244(12) Uani 1 1 d . . .
H2 H 0.4515 0.6047 -0.1970 0.029 Uiso 1 1 calc R . .
C3 C 0.5808(5) 0.5751(5) -0.1045(4) 0.0257(13) Uani 1 1 d . . .
H3 H 0.6255 0.5228 -0.1254 0.031 Uiso 1 1 calc R . .
C4 C 0.6169(5) 0.6038(4) -0.0317(4) 0.0230(12) Uani 1 1 d . . .
H4 H 0.6869 0.5716 -0.0017 0.028 Uiso 1 1 calc R . .
C5 C 0.5497(5) 0.6807(4) -0.0025(4) 0.0180(11) Uani 1 1 d . . .
C6 C 0.5755(4) 0.7120(4) 0.0831(4) 0.0172(11) Uani 1 1 d . . .
C7 C 0.7070(4) 0.7282(4) 0.0865(4) 0.0165(10) Uani 1 1 d . . .
C8 C 0.7847(5) 0.6506(4) 0.1389(4) 0.0221(12) Uani 1 1 d . . .
H8 H 0.7611 0.5811 0.1692 0.027 Uiso 1 1 calc R . .
C9 C 0.8971(5) 0.6751(5) 0.1468(4) 0.0248(12) Uani 1 1 d . . .
H9 H 0.9512 0.6228 0.1831 0.030 Uiso 1 1 calc R . .
C10 C 0.9302(5) 0.7769(5) 0.1011(4) 0.0225(12) Uani 1 1 d . . .
H10 H 1.0065 0.7961 0.1063 0.027 Uiso 1 1 calc R . .
C11 C 0.8486(5) 0.8495(4) 0.0477(4) 0.0187(11) Uani 1 1 d . . .
H11 H 0.8713 0.9188 0.0144 0.022 Uiso 1 1 calc R . .
C12 C 0.5204(6) 0.6433(5) 0.2526(4) 0.0255(13) Uani 1 1 d . . .
H12A H 0.4486 0.6904 0.2531 0.031 Uiso 1 1 calc R . .
H12B H 0.5883 0.6768 0.2640 0.031 Uiso 1 1 calc R . .
C13 C 0.5063(6) 0.5376(5) 0.3289(5) 0.0351(15) Uani 1 1 d . . .
H13A H 0.4927 0.5473 0.3915 0.053 Uiso 1 1 calc R . .
H13B H 0.5781 0.4919 0.3278 0.053 Uiso 1 1 calc R . .
H13C H 0.4390 0.5052 0.3168 0.053 Uiso 1 1 calc R . .
C14 C 0.1398(5) 0.8919(4) -0.0989(4) 0.0195(11) Uani 1 1 d . . .
H14 H 0.1084 0.8334 -0.0503 0.023 Uiso 1 1 calc R . .
C15 C 0.0667(5) 0.9558(5) -0.1669(4) 0.0238(12) Uani 1 1 d . . .
H15 H -0.0137 0.9422 -0.1651 0.029 Uiso 1 1 calc R . .
C16 C 0.1140(5) 1.0397(5) -0.2372(4) 0.0260(13) Uani 1 1 d . . .
H16 H 0.0654 1.0862 -0.2836 0.031 Uiso 1 1 calc R . .
C17 C 0.2316(5) 1.0563(4) -0.2404(4) 0.0210(11) Uani 1 1 d . . .
H17 H 0.2654 1.1123 -0.2904 0.025 Uiso 1 1 calc R . .
C18 C 0.2994(4) 0.9909(4) -0.1705(4) 0.0161(10) Uani 1 1 d . . .
C19 C 0.4279(4) 1.0093(4) -0.1615(4) 0.0150(10) Uani 1 1 d . . .
C20 C 0.5191(5) 0.9421(4) -0.2055(4) 0.0179(11) Uani 1 1 d . . .
C21 C 0.5124(5) 0.9379(5) -0.2964(4) 0.0242(12) Uani 1 1 d . . .
H21 H 0.4467 0.9709 -0.3321 0.029 Uiso 1 1 calc R . .
C22 C 0.6033(6) 0.8847(5) -0.3348(4) 0.0312(14) Uani 1 1 d . . .
H22 H 0.6012 0.8813 -0.3973 0.037 Uiso 1 1 calc R . .
C23 C 0.6968(6) 0.8369(5) -0.2799(5) 0.0300(14) Uani 1 1 d . . .
H23 H 0.7602 0.7999 -0.3042 0.036 Uiso 1 1 calc R . .
C24 C 0.6966(5) 0.8436(5) -0.1887(4) 0.0233(12) Uani 1 1 d . . .
H24 H 0.7609 0.8106 -0.1514 0.028 Uiso 1 1 calc R . .
C25 C 0.2228(5) 0.6496(4) 0.1440(4) 0.0205(11) Uani 1 1 d . . .
C26 C 0.1843(5) 0.5413(5) 0.2982(4) 0.0265(13) Uani 1 1 d . . .
C27 C 0.1930(6) 0.4374(5) 0.3606(4) 0.0299(14) Uani 1 1 d . . .
H27 H 0.2039 0.3812 0.3351 0.036 Uiso 1 1 calc R . .
C28 C 0.1861(6) 0.4150(5) 0.4589(4) 0.0312(14) Uani 1 1 d . . .
C29 C 0.1664(6) 0.4971(6) 0.4968(4) 0.0357(16) Uani 1 1 d . . .
C30 C 0.1555(6) 0.5999(6) 0.4363(5) 0.0367(16) Uani 1 1 d . . .
H30 H 0.1414 0.6558 0.4621 0.044 Uiso 1 1 calc R . .
C31 C 0.1649(6) 0.6215(5) 0.3388(4) 0.0295(14) Uani 1 1 d . . .
H31 H 0.1581 0.6926 0.2984 0.035 Uiso 1 1 calc R . .
C32 C 0.2058(7) 0.3028(6) 0.5223(5) 0.0445(18) Uani 1 1 d . . .
C33 C 0.7555(4) 1.0765(4) -0.1713(4) 0.0168(10) Uani 1 1 d . . .
C34 C 0.7852(5) 1.1221(4) -0.3389(4) 0.0206(11) Uani 1 1 d . . .
C35 C 0.8692(5) 1.1175(5) -0.4132(4) 0.0276(13) Uani 1 1 d . . .
H35 H 0.9465 1.0875 -0.3984 0.033 Uiso 1 1 calc R . .
C36 C 0.8414(6) 1.1560(5) -0.5078(5) 0.0332(15) Uani 1 1 d . . .
C37 C 0.7284(6) 1.1978(6) -0.5294(5) 0.0368(16) Uani 1 1 d . . .
C38 C 0.6443(6) 1.2012(6) -0.4577(5) 0.0356(15) Uani 1 1 d . . .
H38 H 0.5666 1.2295 -0.4730 0.043 Uiso 1 1 calc R . .
C39 C 0.6720(5) 1.1637(5) -0.3632(5) 0.0288(13) Uani 1 1 d . . .
H39 H 0.6130 1.1664 -0.3144 0.035 Uiso 1 1 calc R . .
C40 C 0.9370(7) 1.1540(7) -0.5846(5) 0.0467(19) Uani 1 1 d . . .
O5 O 0.1222(5) 0.3939(5) 0.1406(5) 0.0608(17) Uani 1 1 d D . .
H5A H 0.152(8) 0.442(6) 0.156(7) 0.091 Uiso 1 1 d D . .
C41 C -0.0553(9) 0.3387(8) 0.1130(7) 0.067(3) Uani 1 1 d . . .
H41A H -0.1404 0.3564 0.1108 0.101 Uiso 1 1 calc R . .
H41B H -0.0407 0.2697 0.1611 0.101 Uiso 1 1 calc R . .
H41C H -0.0220 0.3366 0.0505 0.101 Uiso 1 1 calc R . .
C42 C -0.0004(7) 0.4175(7) 0.1377(6) 0.0473(19) Uani 1 1 d . . .
H42A H -0.0166 0.4874 0.0900 0.057 Uiso 1 1 calc R . .
H42B H -0.0343 0.4200 0.2007 0.057 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N5 2.015(5) . ?
Ni1 O1 2.039(3) . ?
Ni1 N3 2.074(4) . ?
Ni1 N1 2.112(4) . ?
Ni1 N7 2.144(4) 2_675 ?
Ni1 O3 2.155(4) . ?
Ni2 O3 2.007(3) . ?
Ni2 N2 2.039(4) . ?
Ni2 O3 2.091(4) 2_675 ?
Ni2 N7 2.098(4) . ?
Ni2 N4 2.098(4) . ?
Ni2 O1 2.141(4) . ?
Cl1 C29 1.740(7) . ?
Cl2 C37 1.754(7) . ?
N1 C1 1.340(7) . ?
N1 C5 1.348(7) . ?
N2 C11 1.334(7) . ?
N2 C7 1.346(7) . ?
N3 C14 1.342(7) . ?
N3 C18 1.356(7) . ?
N4 C24 1.338(7) . ?
N4 C20 1.345(7) . ?
N5 C25 1.164(7) . ?
N6 C25 1.303(7) . ?
N6 C26 1.402(8) . ?
N7 C33 1.187(7) . ?
N7 Ni1 2.144(4) 2_675 ?
N8 C33 1.268(7) . ?
N8 C34 1.405(7) . ?
F1 C32 1.342(9) . ?
F2 C32 1.342(9) . ?
F3 C32 1.329(9) . ?
F4 C40 1.348(9) . ?
F5 C40 1.326(9) . ?
F6 C40 1.350(9) . ?
O1 C6 1.377(6) . ?
O2 C6 1.423(6) . ?
O2 C12 1.448(7) . ?
O3 C19 1.377(6) . ?
O3 Ni2 2.090(4) 2_675 ?
O4 C19 1.397(6) . ?
O4 H4A 0.855(14) . ?
C1 C2 1.382(8) . ?
C1 H1 0.9500 . ?
C2 C3 1.385(8) . ?
C2 H2 0.9500 . ?
C3 C4 1.378(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.392(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.533(8) . ?
C6 C7 1.547(7) . ?
C7 C8 1.382(7) . ?
C8 C9 1.382(8) . ?
C8 H8 0.9500 . ?
C9 C10 1.389(8) . ?
C9 H9 0.9500 . ?
C10 C11 1.385(7) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 C13 1.514(8) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.385(8) . ?
C14 H14 0.9500 . ?
C15 C16 1.376(8) . ?
C15 H15 0.9500 . ?
C16 C17 1.377(8) . ?
C16 H16 0.9500 . ?
C17 C18 1.372(7) . ?
C17 H17 0.9500 . ?
C18 C19 1.539(7) . ?
C19 C20 1.555(7) . ?
C20 C21 1.385(8) . ?
C21 C22 1.390(8) . ?
C21 H21 0.9500 . ?
C22 C23 1.384(9) . ?
C22 H22 0.9500 . ?
C23 C24 1.392(8) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C26 C31 1.398(9) . ?
C26 C27 1.404(8) . ?
C27 C28 1.390(9) . ?
C27 H27 0.9500 . ?
C28 C29 1.393(10) . ?
C28 C32 1.507(9) . ?
C29 C30 1.384(9) . ?
C30 C31 1.380(9) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C34 C39 1.391(8) . ?
C34 C35 1.406(8) . ?
C35 C36 1.389(9) . ?
C35 H35 0.9500 . ?
C36 C37 1.381(10) . ?
C36 C40 1.508(10) . ?
C37 C38 1.375(10) . ?
C38 C39 1.388(9) . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
O5 C42 1.409(9) . ?
O5 H5A 0.863(17) . ?
C41 C42 1.448(12) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?

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
N5 Ni1 O1 107.39(17) . . ?
N5 Ni1 N3 96.22(19) . . ?
O1 Ni1 N3 155.20(16) . . ?
N5 Ni1 N1 89.54(18) . . ?
O1 Ni1 N1 76.96(15) . . ?
N3 Ni1 N1 96.16(17) . . ?
N5 Ni1 N7 91.61(18) . 2_675 ?
O1 Ni1 N7 89.64(15) . 2_675 ?
N3 Ni1 N7 97.32(16) . 2_675 ?
N1 Ni1 N7 166.26(17) . 2_675 ?
N5 Ni1 O3 166.68(16) . . ?
O1 Ni1 O3 81.64(14) . . ?
N3 Ni1 O3 76.55(16) . . ?
N1 Ni1 O3 102.24(15) . . ?
N7 Ni1 O3 78.44(15) 2_675 . ?
O3 Ni2 N2 159.14(16) . . ?
O3 Ni2 O3 80.41(15) . 2_675 ?
N2 Ni2 O3 104.54(15) . 2_675 ?
O3 Ni2 N7 101.21(15) . . ?
N2 Ni2 N7 99.58(17) . . ?
O3 Ni2 N7 80.94(15) 2_675 . ?
O3 Ni2 N4 78.14(15) . . ?
N2 Ni2 N4 100.64(17) . . ?
O3 Ni2 N4 154.12(15) 2_675 . ?
N7 Ni2 N4 89.17(17) . . ?
O3 Ni2 O1 82.75(14) . . ?
N2 Ni2 O1 77.41(15) . . ?
O3 Ni2 O1 86.56(13) 2_675 . ?
N7 Ni2 O1 166.01(15) . . ?
N4 Ni2 O1 104.80(15) . . ?
C1 N1 C5 118.6(5) . . ?
C1 N1 Ni1 125.8(4) . . ?
C5 N1 Ni1 115.5(4) . . ?
C11 N2 C7 119.1(4) . . ?
C11 N2 Ni2 126.9(4) . . ?
C7 N2 Ni2 113.8(3) . . ?
C14 N3 C18 118.9(5) . . ?
C14 N3 Ni1 124.8(4) . . ?
C18 N3 Ni1 115.4(3) . . ?
C24 N4 C20 118.3(5) . . ?
C24 N4 Ni2 127.0(4) . . ?
C20 N4 Ni2 114.1(3) . . ?
C25 N5 Ni1 155.1(4) . . ?
C25 N6 C26 116.8(5) . . ?
C33 N7 Ni2 126.2(4) . . ?
C33 N7 Ni1 132.3(4) . 2_675 ?
Ni2 N7 Ni1 100.19(18) . 2_675 ?
C33 N8 C34 124.5(5) . . ?
C6 O1 Ni1 117.5(3) . . ?
C6 O1 Ni2 107.2(3) . . ?
Ni1 O1 Ni2 95.85(14) . . ?
C6 O2 C12 115.4(4) . . ?
C19 O3 Ni2 117.3(3) . . ?
C19 O3 Ni2 127.4(3) . 2_675 ?
Ni2 O3 Ni2 99.59(15) . 2_675 ?
C19 O3 Ni1 110.9(3) . . ?
Ni2 O3 Ni1 96.36(15) . . ?
Ni2 O3 Ni1 100.03(14) 2_675 . ?
C19 O4 H4A 105(5) . . ?
N1 C1 C2 122.7(5) . . ?
N1 C1 H1 118.6 . . ?
C2 C1 H1 118.6 . . ?
C1 C2 C3 118.7(5) . . ?
C1 C2 H2 120.6 . . ?
C3 C2 H2 120.6 . . ?
C4 C3 C2 119.1(5) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C3 C4 C5 119.2(5) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
N1 C5 C4 121.6(5) . . ?
N1 C5 C6 114.6(4) . . ?
C4 C5 C6 123.7(5) . . ?
O1 C6 O2 114.3(4) . . ?
O1 C6 C5 109.3(4) . . ?
O2 C6 C5 102.7(4) . . ?
O1 C6 C7 107.0(4) . . ?
O2 C6 C7 110.0(4) . . ?
C5 C6 C7 113.8(4) . . ?
N2 C7 C8 121.4(5) . . ?
N2 C7 C6 115.3(4) . . ?
C8 C7 C6 123.1(5) . . ?
C9 C8 C7 119.3(5) . . ?
C9 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
C8 C9 C10 119.4(5) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
C11 C10 C9 117.9(5) . . ?
C11 C10 H10 121.0 . . ?
C9 C10 H10 121.0 . . ?
N2 C11 C10 122.8(5) . . ?
N2 C11 H11 118.6 . . ?
C10 C11 H11 118.6 . . ?
O2 C12 C13 107.1(5) . . ?
O2 C12 H12A 110.3 . . ?
C13 C12 H12A 110.3 . . ?
O2 C12 H12B 110.3 . . ?
C13 C12 H12B 110.3 . . ?
H12A C12 H12B 108.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N3 C14 C15 122.3(5) . . ?
N3 C14 H14 118.8 . . ?
C15 C14 H14 118.8 . . ?
C16 C15 C14 117.9(5) . . ?
C16 C15 H15 121.0 . . ?
C14 C15 H15 121.0 . . ?
C15 C16 C17 120.3(5) . . ?
C15 C16 H16 119.9 . . ?
C17 C16 H16 119.9 . . ?
C18 C17 C16 119.1(5) . . ?
C18 C17 H17 120.5 . . ?
C16 C17 H17 120.5 . . ?
N3 C18 C17 121.5(5) . . ?
N3 C18 C19 115.1(4) . . ?
C17 C18 C19 123.2(5) . . ?
O3 C19 O4 113.9(4) . . ?
O3 C19 C18 107.1(4) . . ?
O4 C19 C18 108.2(4) . . ?
O3 C19 C20 108.5(4) . . ?
O4 C19 C20 106.2(4) . . ?
C18 C19 C20 113.0(4) . . ?
N4 C20 C21 122.5(5) . . ?
N4 C20 C19 115.1(4) . . ?
C21 C20 C19 122.2(5) . . ?
C20 C21 C22 119.1(5) . . ?
C20 C21 H21 120.4 . . ?
C22 C21 H21 120.4 . . ?
C23 C22 C21 118.5(6) . . ?
C23 C22 H22 120.8 . . ?
C21 C22 H22 120.8 . . ?
C22 C23 C24 119.1(5) . . ?
C22 C23 H23 120.5 . . ?
C24 C23 H23 120.5 . . ?
N4 C24 C23 122.6(5) . . ?
N4 C24 H24 118.7 . . ?
C23 C24 H24 118.7 . . ?
N5 C25 N6 175.6(6) . . ?
C31 C26 N6 125.1(5) . . ?
C31 C26 C27 117.3(6) . . ?
N6 C26 C27 117.6(6) . . ?
C28 C27 C26 121.5(6) . . ?
C28 C27 H27 119.2 . . ?
C26 C27 H27 119.2 . . ?
C27 C28 C29 119.5(6) . . ?
C27 C28 C32 119.2(6) . . ?
C29 C28 C32 121.2(6) . . ?
C30 C29 C28 119.8(6) . . ?
C30 C29 Cl1 118.0(6) . . ?
C28 C29 Cl1 122.2(5) . . ?
C31 C30 C29 120.4(7) . . ?
C31 C30 H30 119.8 . . ?
C29 C30 H30 119.8 . . ?
C30 C31 C26 121.5(6) . . ?
C30 C31 H31 119.2 . . ?
C26 C31 H31 119.2 . . ?
F3 C32 F1 106.0(7) . . ?
F3 C32 F2 106.8(7) . . ?
F1 C32 F2 106.7(6) . . ?
F3 C32 C28 112.1(6) . . ?
F1 C32 C28 112.6(6) . . ?
F2 C32 C28 112.2(7) . . ?
N7 C33 N8 172.3(5) . . ?
C39 C34 N8 125.2(5) . . ?
C39 C34 C35 117.7(5) . . ?
N8 C34 C35 117.1(5) . . ?
C36 C35 C34 121.2(6) . . ?
C36 C35 H35 119.4 . . ?
C34 C35 H35 119.4 . . ?
C37 C36 C35 119.5(6) . . ?
C37 C36 C40 121.7(6) . . ?
C35 C36 C40 118.8(6) . . ?
C38 C37 C36 120.2(6) . . ?
C38 C37 Cl2 118.2(5) . . ?
C36 C37 Cl2 121.6(5) . . ?
C37 C38 C39 120.5(6) . . ?
C37 C38 H38 119.8 . . ?
C39 C38 H38 119.8 . . ?
C38 C39 C34 120.8(6) . . ?
C38 C39 H39 119.6 . . ?
C34 C39 H39 119.6 . . ?
F5 C40 F4 106.9(6) . . ?
F5 C40 F6 106.5(7) . . ?
F4 C40 F6 105.7(7) . . ?
F5 C40 C36 113.4(7) . . ?
F4 C40 C36 112.0(7) . . ?
F6 C40 C36 111.9(6) . . ?
C42 O5 H5A 108(7) . . ?
C42 C41 H41A 109.5 . . ?
C42 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C42 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O5 C42 C41 110.3(7) . . ?
O5 C42 H42A 109.6 . . ?
C41 C42 H42A 109.6 . . ?
O5 C42 H42B 109.6 . . ?
C41 C42 H42B 109.6 . . ?
H42A C42 H42B 108.1 . . ?

_diffrn_measured_fraction_theta_max 0.947
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         1.424
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.148
####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1434558'
_audit_update_record             
;
2015-11-02 deposited with the CCDC.
2016-02-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C78 H52 F16 N16 Ni4 O8, 4(C H4 O)'
_chemical_formula_sum            'C82 H68 F16 N16 Ni4 O12'
_chemical_formula_weight         2008.36

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   12.5027(4)
_cell_length_b                   21.7883(7)
_cell_length_c                   15.8999(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.446(2)
_cell_angle_gamma                90.00
_cell_volume                     4132.1(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100.0(1)
_cell_measurement_reflns_used    1887
_cell_measurement_theta_min      2.615
_cell_measurement_theta_max      27.38

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2048
_exptl_absorpt_coefficient_mu    1.006
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8034
_exptl_absorpt_correction_T_max  0.8749
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100.0(1)
_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  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            50699
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_av_sigmaI/netI    0.0649
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.64
_diffrn_reflns_theta_max         30.87
_reflns_number_total             12806
_reflns_number_gt                8788
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'BRUKER APEX2'
_computing_cell_refinement       'BRUKER APEX2'
_computing_data_reduction        'BRUKER APEX2'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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)+(0.0485P)²+3.5212P] 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         12806
_refine_ls_number_parameters     597
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0485
_refine_ls_wR_factor_ref         0.1203
_refine_ls_wR_factor_gt          0.1062
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.108
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O5 O 0.9766(3) 0.23975(14) 0.2036(2) 0.0511(7) Uani 1 1 d D . .
H5A H 0.999(4) 0.2039(14) 0.182(3) 0.077 Uiso 1 1 d D . .
C40 C 0.9312(4) 0.2152(3) 0.2693(3) 0.0613(13) Uani 1 1 d . . .
H40A H 0.9902 0.1969 0.3157 0.092 Uiso 1 1 calc R . .
H40B H 0.8758 0.1847 0.2431 0.092 Uiso 1 1 calc R . .
H40C H 0.8971 0.2477 0.2932 0.092 Uiso 1 1 calc R . .
O6 O 0.0586(3) 0.16687(16) 0.1023(2) 0.0599(9) Uani 1 1 d D . .
H6A H 0.127(2) 0.152(2) 0.118(3) 0.090 Uiso 1 1 d D . .
C41 C 0.0377(3) 0.1854(2) 0.0141(3) 0.0443(10) Uani 1 1 d . . .
H41A H -0.0259 0.2124 -0.0020 0.066 Uiso 1 1 calc R . .
H41B H 0.0225 0.1499 -0.0235 0.066 Uiso 1 1 calc R . .
H41C H 0.1022 0.2064 0.0076 0.066 Uiso 1 1 calc R . .
Ni1 Ni 0.68557(3) 0.442754(15) 0.47343(2) 0.01253(8) Uani 1 1 d . . .
Ni2 Ni 0.44465(3) 0.435344(15) 0.49192(2) 0.01170(8) Uani 1 1 d . . .
F1 F 1.02265(18) 0.34086(11) 0.04442(14) 0.0435(6) Uani 1 1 d . . .
F2 F 0.8775(2) 0.35236(12) -0.06798(14) 0.0496(6) Uani 1 1 d . . .
F3 F 0.99584(19) 0.42598(11) -0.02701(15) 0.0467(6) Uani 1 1 d . . .
F4 F 0.77079(18) 0.46694(10) -0.05509(12) 0.0384(5) Uani 1 1 d . . .
F5 F 0.25601(19) 0.38065(11) 1.02169(13) 0.0468(6) Uani 1 1 d . . .
F6 F 0.1587(2) 0.32190(11) 0.91913(14) 0.0485(6) Uani 1 1 d . . .
F7 F 0.3177(2) 0.29151(13) 1.00291(17) 0.0630(7) Uani 1 1 d U . .
F8 F 0.48165(19) 0.38470(13) 1.01672(13) 0.0522(7) Uani 1 1 d . . .
O1 O 0.52769(15) 0.42201(8) 0.39523(12) 0.0136(4) Uani 1 1 d . . .
O2 O 0.53799(17) 0.35066(9) 0.28760(12) 0.0202(4) Uani 1 1 d . . .
O3 O 0.59193(14) 0.47635(8) 0.55779(11) 0.0114(3) Uani 1 1 d . . .
O4 O 0.60998(16) 0.49352(9) 0.70541(12) 0.0170(4) Uani 1 1 d D . .
H4A H 0.566(2) 0.5219(12) 0.6776(19) 0.025 Uiso 1 1 d D . .
N1 N 0.67663(19) 0.34710(10) 0.48916(15) 0.0162(5) Uani 1 1 d . . .
N2 N 0.33610(19) 0.37936(10) 0.40348(14) 0.0155(4) Uani 1 1 d . . .
N3 N 0.80804(19) 0.45722(10) 0.59158(14) 0.0150(4) Uani 1 1 d . . .
N4 N 0.51777(19) 0.37139(10) 0.59024(15) 0.0148(4) Uani 1 1 d . . .
N5 N 0.7855(2) 0.42853(11) 0.39662(16) 0.0206(5) Uani 1 1 d . . .
N6 N 0.8696(2) 0.38470(12) 0.28918(16) 0.0231(5) Uani 1 1 d . . .
N7 N 0.33496(19) 0.46237(10) 0.56160(14) 0.0146(4) Uani 1 1 d . . .
N8 N 0.2551(2) 0.40507(11) 0.66136(16) 0.0199(5) Uani 1 1 d . . .
C1 C 0.7545(3) 0.31247(14) 0.5457(2) 0.0225(6) Uani 1 1 d . . .
H1 H 0.8162 0.3317 0.5844 0.027 Uiso 1 1 calc R . .
C2 C 0.7466(3) 0.24952(15) 0.5484(2) 0.0288(7) Uani 1 1 d . . .
H2 H 0.8013 0.2267 0.5889 0.035 Uiso 1 1 calc R . .
C3 C 0.6559(3) 0.22081(14) 0.4900(2) 0.0293(7) Uani 1 1 d . . .
H3 H 0.6490 0.1783 0.4903 0.035 Uiso 1 1 calc R . .
C4 C 0.5757(3) 0.25605(14) 0.4311(2) 0.0244(6) Uani 1 1 d . . .
H4 H 0.5139 0.2377 0.3912 0.029 Uiso 1 1 calc R . .
C5 C 0.5889(2) 0.31911(13) 0.43254(18) 0.0176(5) Uani 1 1 d . . .
C6 C 0.5093(2) 0.36237(12) 0.36665(18) 0.0162(5) Uani 1 1 d . . .
C7 C 0.3845(2) 0.34804(13) 0.35133(18) 0.0172(5) Uani 1 1 d . . .
C8 C 0.3234(3) 0.30813(14) 0.2870(2) 0.0251(6) Uani 1 1 d . . .
H8 H 0.3583 0.2864 0.2523 0.030 Uiso 1 1 calc R . .
C9 C 0.2098(3) 0.30096(16) 0.2749(2) 0.0280(7) Uani 1 1 d . . .
H9 H 0.1676 0.2743 0.2321 0.034 Uiso 1 1 calc R . .
C10 C 0.1595(2) 0.33403(15) 0.32757(19) 0.0237(6) Uani 1 1 d . . .
H10 H 0.0832 0.3304 0.3204 0.028 Uiso 1 1 calc R . .
C11 C 0.2265(2) 0.37262(13) 0.39104(18) 0.0189(6) Uani 1 1 d . . .
H11 H 0.1935 0.3948 0.4266 0.023 Uiso 1 1 calc R . .
C12 C 0.5013(3) 0.39599(15) 0.2207(2) 0.0282(7) Uani 1 1 d . . .
H12A H 0.5236 0.3844 0.1702 0.042 Uiso 1 1 calc R . .
H12B H 0.5343 0.4348 0.2426 0.042 Uiso 1 1 calc R . .
H12C H 0.4211 0.3993 0.2042 0.042 Uiso 1 1 calc R . .
C13 C 0.9183(2) 0.46208(13) 0.60272(19) 0.0181(5) Uani 1 1 d . . .
H13 H 0.9438 0.4579 0.5538 0.022 Uiso 1 1 calc R . .
C14 C 0.9954(2) 0.47308(14) 0.6836(2) 0.0216(6) Uani 1 1 d . . .
H14 H 1.0715 0.4760 0.6892 0.026 Uiso 1 1 calc R . .
C15 C 0.9573(2) 0.47968(14) 0.75687(19) 0.0217(6) Uani 1 1 d . . .
H15 H 1.0075 0.4868 0.8123 0.026 Uiso 1 1 calc R . .
C16 C 0.8432(2) 0.47543(13) 0.74591(18) 0.0185(5) Uani 1 1 d . . .
H16 H 0.8158 0.4804 0.7938 0.022 Uiso 1 1 calc R . .
C17 C 0.7707(2) 0.46371(12) 0.66251(17) 0.0144(5) Uani 1 1 d . . .
C18 C 0.6434(2) 0.45780(12) 0.64349(16) 0.0139(5) Uani 1 1 d . . .
C19 C 0.6072(2) 0.39151(12) 0.65449(17) 0.0148(5) Uani 1 1 d . . .
C20 C 0.6593(2) 0.35599(14) 0.72746(19) 0.0208(6) Uani 1 1 d . . .
H20 H 0.7200 0.3713 0.7719 0.025 Uiso 1 1 calc R . .
C21 C 0.6195(3) 0.29697(15) 0.7333(2) 0.0269(7) Uani 1 1 d . . .
H21 H 0.6547 0.2718 0.7807 0.032 Uiso 1 1 calc R . .
C22 C 0.5273(3) 0.27653(14) 0.6677(2) 0.0251(6) Uani 1 1 d . . .
H22 H 0.4986 0.2375 0.6705 0.030 Uiso 1 1 calc R . .
C23 C 0.4779(2) 0.31499(13) 0.5975(2) 0.0204(6) Uani 1 1 d . . .
H23 H 0.4149 0.3013 0.5538 0.024 Uiso 1 1 calc R . .
C24 C 0.8218(2) 0.40855(13) 0.34263(18) 0.0181(5) Uani 1 1 d . . .
C25 C 0.8418(2) 0.40693(13) 0.20337(19) 0.0184(5) Uani 1 1 d . . .
C26 C 0.9017(2) 0.38461(13) 0.14774(18) 0.0189(6) Uani 1 1 d . . .
H26 H 0.9576 0.3554 0.1691 0.023 Uiso 1 1 calc R . .
C27 C 0.8795(2) 0.40507(14) 0.06218(19) 0.0204(6) Uani 1 1 d . . .
C28 C 0.7951(3) 0.44767(15) 0.03027(19) 0.0246(6) Uani 1 1 d . . .
C29 C 0.7344(3) 0.47034(15) 0.0819(2) 0.0279(7) Uani 1 1 d . . .
H29 H 0.6780 0.4990 0.0593 0.033 Uiso 1 1 calc R . .
C30 C 0.7578(2) 0.45022(14) 0.1687(2) 0.0217(6) Uani 1 1 d . . .
H30 H 0.7169 0.4658 0.2040 0.026 Uiso 1 1 calc R . .
C31 C 0.9440(3) 0.38127(17) 0.0035(2) 0.0300(7) Uani 1 1 d . . .
C32 C 0.2987(2) 0.43523(13) 0.61193(17) 0.0158(5) Uani 1 1 d . . .
C33 C 0.3164(2) 0.39992(13) 0.75168(19) 0.0195(6) Uani 1 1 d . . .
C34 C 0.2634(3) 0.37235(13) 0.80808(19) 0.0218(6) Uani 1 1 d . . .
H34 H 0.1906 0.3576 0.7857 0.026 Uiso 1 1 calc R . .
C35 C 0.3196(3) 0.36710(15) 0.8974(2) 0.0255(7) Uani 1 1 d . . .
C36 C 0.4280(3) 0.38933(17) 0.9291(2) 0.0323(8) Uani 1 1 d . . .
C37 C 0.4817(3) 0.41602(17) 0.8753(2) 0.0304(7) Uani 1 1 d . . .
H37 H 0.5549 0.4301 0.8980 0.036 Uiso 1 1 calc R . .
C38 C 0.4254(2) 0.42172(14) 0.78616(19) 0.0223(6) Uani 1 1 d . . .
H38 H 0.4608 0.4403 0.7490 0.027 Uiso 1 1 calc R . .
C39 C 0.2632(3) 0.34037(18) 0.9599(2) 0.0369(9) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O5 C40 1.433(5) . ?
O5 H5A 0.932(18) . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
O6 C41 1.406(5) . ?
O6 H6A 0.880(17) . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
Ni1 N5 2.015(2) . ?
Ni1 O1 2.0434(19) . ?
Ni1 N3 2.061(2) . ?
Ni1 N1 2.106(2) . ?
Ni1 N7 2.136(2) 3_666 ?
Ni1 O3 2.1558(17) . ?
Ni2 O3 2.0320(18) . ?
Ni2 N2 2.040(2) . ?
Ni2 O3 2.0784(18) 3_666 ?
Ni2 N4 2.089(2) . ?
Ni2 N7 2.090(2) . ?
Ni2 O1 2.1173(17) . ?
F1 C31 1.335(4) . ?
F2 C31 1.347(4) . ?
F3 C31 1.339(4) . ?
F4 C28 1.365(3) . ?
F5 C39 1.340(4) . ?
F6 C39 1.335(5) . ?
F7 C39 1.337(4) . ?
F8 C36 1.356(4) . ?
O1 C6 1.373(3) . ?
O2 C12 1.423(4) . ?
O2 C6 1.430(3) . ?
O3 C18 1.381(3) . ?
O3 Ni2 2.0783(18) 3_666 ?
O4 C18 1.413(3) . ?
O4 H4A 0.857(14) . ?
N1 C5 1.339(4) . ?
N1 C1 1.342(4) . ?
N2 C11 1.332(4) . ?
N2 C7 1.349(3) . ?
N3 C13 1.340(3) . ?
N3 C17 1.351(3) . ?
N4 C19 1.342(4) . ?
N4 C23 1.344(3) . ?
N5 C24 1.169(4) . ?
N6 C24 1.286(4) . ?
N6 C25 1.390(4) . ?
N7 C32 1.189(3) . ?
N7 Ni1 2.136(2) 3_666 ?
N8 C32 1.266(3) . ?
N8 C33 1.415(4) . ?
C1 C2 1.377(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.381(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.382(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.383(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.534(4) . ?
C6 C7 1.536(4) . ?
C7 C8 1.385(4) . ?
C8 C9 1.383(4) . ?
C8 H8 0.9300 . ?
C9 C10 1.389(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.386(4) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.378(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.392(4) . ?
C14 H14 0.9300 . ?
C15 C16 1.387(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.388(4) . ?
C16 H16 0.9300 . ?
C17 C18 1.533(4) . ?
C18 C19 1.539(4) . ?
C19 C20 1.384(4) . ?
C20 C21 1.392(4) . ?
C20 H20 0.9300 . ?
C21 C22 1.377(5) . ?
C21 H21 0.9300 . ?
C22 C23 1.384(4) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C25 C30 1.396(4) . ?
C25 C26 1.407(4) . ?
C26 C27 1.378(4) . ?
C26 H26 0.9300 . ?
C27 C28 1.382(4) . ?
C27 C31 1.497(4) . ?
C28 C29 1.367(4) . ?
C29 C30 1.392(4) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
C33 C38 1.391(4) . ?
C33 C34 1.400(4) . ?
C34 C35 1.387(4) . ?
C34 H34 0.9300 . ?
C35 C36 1.384(5) . ?
C35 C39 1.499(4) . ?
C36 C37 1.366(5) . ?
C37 C38 1.386(4) . ?
C37 H37 0.9300 . ?
C38 H38 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C40 O5 H5A 101(2) . . ?
O5 C40 H40A 109.5 . . ?
O5 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
O5 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C41 O6 H6A 105(3) . . ?
O6 C41 H41A 109.5 . . ?
O6 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
O6 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
N5 Ni1 O1 104.97(9) . . ?
N5 Ni1 N3 98.62(9) . . ?
O1 Ni1 N3 155.04(8) . . ?
N5 Ni1 N1 89.11(9) . . ?
O1 Ni1 N1 77.13(8) . . ?
N3 Ni1 N1 95.42(9) . . ?
N5 Ni1 N7 92.22(9) . 3_666 ?
O1 Ni1 N7 92.11(8) . 3_666 ?
N3 Ni1 N7 95.05(9) . 3_666 ?
N1 Ni1 N7 169.13(9) . 3_666 ?
N5 Ni1 O3 168.54(9) . . ?
O1 Ni1 O3 81.25(7) . . ?
N3 Ni1 O3 76.98(8) . . ?
N1 Ni1 O3 101.77(8) . . ?
N7 Ni1 O3 77.79(7) 3_666 . ?
O3 Ni2 N2 158.56(8) . . ?
O3 Ni2 O3 81.43(7) . 3_666 ?
N2 Ni2 O3 105.45(8) . 3_666 ?
O3 Ni2 N4 77.41(8) . . ?
N2 Ni2 N4 99.69(9) . . ?
O3 Ni2 N4 154.05(8) 3_666 . ?
O3 Ni2 N7 103.90(8) . . ?
N2 Ni2 N7 97.30(9) . . ?
O3 Ni2 N7 80.57(8) 3_666 . ?
N4 Ni2 N7 90.04(9) . . ?
O3 Ni2 O1 82.46(7) . . ?
N2 Ni2 O1 77.71(8) . . ?
O3 Ni2 O1 87.18(7) 3_666 . ?
N4 Ni2 O1 104.60(8) . . ?
N7 Ni2 O1 165.09(8) . . ?
C6 O1 Ni1 116.51(16) . . ?
C6 O1 Ni2 107.46(15) . . ?
Ni1 O1 Ni2 97.03(7) . . ?
C12 O2 C6 115.0(2) . . ?
C18 O3 Ni2 117.51(15) . . ?
C18 O3 Ni2 129.07(16) . 3_666 ?
Ni2 O3 Ni2 98.57(7) . 3_666 ?
C18 O3 Ni1 109.58(14) . . ?
Ni2 O3 Ni1 96.16(7) . . ?
Ni2 O3 Ni1 100.16(7) 3_666 . ?
C18 O4 H4A 108(2) . . ?
C5 N1 C1 118.5(2) . . ?
C5 N1 Ni1 115.65(18) . . ?
C1 N1 Ni1 125.6(2) . . ?
C11 N2 C7 118.9(2) . . ?
C11 N2 Ni2 127.60(19) . . ?
C7 N2 Ni2 113.42(18) . . ?
C13 N3 C17 118.7(2) . . ?
C13 N3 Ni1 125.88(18) . . ?
C17 N3 Ni1 115.36(18) . . ?
C19 N4 C23 118.6(2) . . ?
C19 N4 Ni2 115.43(17) . . ?
C23 N4 Ni2 125.7(2) . . ?
C24 N5 Ni1 161.8(2) . . ?
C24 N6 C25 118.6(3) . . ?
C32 N7 Ni2 131.3(2) . . ?
C32 N7 Ni1 128.1(2) . 3_666 ?
Ni2 N7 Ni1 100.43(9) . 3_666 ?
C32 N8 C33 117.9(2) . . ?
N1 C1 C2 122.4(3) . . ?
N1 C1 H1 118.8 . . ?
C2 C1 H1 118.8 . . ?
C1 C2 C3 118.8(3) . . ?
C1 C2 H2 120.6 . . ?
C3 C2 H2 120.6 . . ?
C2 C3 C4 119.1(3) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C3 C4 C5 118.8(3) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
N1 C5 C4 122.2(3) . . ?
N1 C5 C6 114.4(2) . . ?
C4 C5 C6 123.3(3) . . ?
O1 C6 O2 113.5(2) . . ?
O1 C6 C5 110.2(2) . . ?
O2 C6 C5 102.0(2) . . ?
O1 C6 C7 107.8(2) . . ?
O2 C6 C7 109.6(2) . . ?
C5 C6 C7 113.8(2) . . ?
N2 C7 C8 121.4(3) . . ?
N2 C7 C6 114.9(2) . . ?
C8 C7 C6 123.7(2) . . ?
C9 C8 C7 119.3(3) . . ?
C9 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
C8 C9 C10 119.3(3) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
C11 C10 C9 118.0(3) . . ?
C11 C10 H10 121.0 . . ?
C9 C10 H10 121.0 . . ?
N2 C11 C10 123.0(3) . . ?
N2 C11 H11 118.5 . . ?
C10 C11 H11 118.5 . . ?
O2 C12 H12A 109.5 . . ?
O2 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O2 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N3 C13 C14 122.8(3) . . ?
N3 C13 H13 118.6 . . ?
C14 C13 H13 118.6 . . ?
C13 C14 C15 118.6(3) . . ?
C13 C14 H14 120.7 . . ?
C15 C14 H14 120.7 . . ?
C16 C15 C14 119.0(3) . . ?
C16 C15 H15 120.5 . . ?
C14 C15 H15 120.5 . . ?
C15 C16 C17 119.0(3) . . ?
C15 C16 H16 120.5 . . ?
C17 C16 H16 120.5 . . ?
N3 C17 C16 121.7(2) . . ?
N3 C17 C18 115.1(2) . . ?
C16 C17 C18 123.1(2) . . ?
O3 C18 O4 112.2(2) . . ?
O3 C18 C17 108.6(2) . . ?
O4 C18 C17 108.8(2) . . ?
O3 C18 C19 108.7(2) . . ?
O4 C18 C19 106.2(2) . . ?
C17 C18 C19 112.3(2) . . ?
N4 C19 C20 122.0(3) . . ?
N4 C19 C18 115.2(2) . . ?
C20 C19 C18 122.7(2) . . ?
C19 C20 C21 119.0(3) . . ?
C19 C20 H20 120.5 . . ?
C21 C20 H20 120.5 . . ?
C22 C21 C20 118.9(3) . . ?
C22 C21 H21 120.5 . . ?
C20 C21 H21 120.5 . . ?
C21 C22 C23 119.0(3) . . ?
C21 C22 H22 120.5 . . ?
C23 C22 H22 120.5 . . ?
N4 C23 C22 122.4(3) . . ?
N4 C23 H23 118.8 . . ?
C22 C23 H23 118.8 . . ?
N5 C24 N6 174.6(3) . . ?
N6 C25 C30 124.1(3) . . ?
N6 C25 C26 118.2(3) . . ?
C30 C25 C26 117.7(3) . . ?
C27 C26 C25 121.4(3) . . ?
C27 C26 H26 119.3 . . ?
C25 C26 H26 119.3 . . ?
C26 C27 C28 119.1(3) . . ?
C26 C27 C31 121.0(3) . . ?
C28 C27 C31 119.9(3) . . ?
F4 C28 C29 119.2(3) . . ?
F4 C28 C27 119.3(3) . . ?
C29 C28 C27 121.5(3) . . ?
C28 C29 C30 119.5(3) . . ?
C28 C29 H29 120.3 . . ?
C30 C29 H29 120.3 . . ?
C29 C30 C25 120.9(3) . . ?
C29 C30 H30 119.5 . . ?
C25 C30 H30 119.5 . . ?
F1 C31 F3 106.9(3) . . ?
F1 C31 F2 106.3(3) . . ?
F3 C31 F2 106.1(3) . . ?
F1 C31 C27 112.4(3) . . ?
F3 C31 C27 112.6(3) . . ?
F2 C31 C27 112.1(3) . . ?
N7 C32 N8 176.4(3) . . ?
C38 C33 C34 119.3(3) . . ?
C38 C33 N8 122.8(2) . . ?
C34 C33 N8 117.9(3) . . ?
C35 C34 C33 119.9(3) . . ?
C35 C34 H34 120.0 . . ?
C33 C34 H34 120.0 . . ?
C36 C35 C34 119.0(3) . . ?
C36 C35 C39 119.9(3) . . ?
C34 C35 C39 121.1(3) . . ?
F8 C36 C37 119.4(3) . . ?
F8 C36 C35 118.5(3) . . ?
C37 C36 C35 122.1(3) . . ?
C36 C37 C38 119.0(3) . . ?
C36 C37 H37 120.5 . . ?
C38 C37 H37 120.5 . . ?
C37 C38 C33 120.6(3) . . ?
C37 C38 H38 119.7 . . ?
C33 C38 H38 119.7 . . ?
F6 C39 F7 106.5(3) . . ?
F6 C39 F5 106.4(3) . . ?
F7 C39 F5 106.4(3) . . ?
F6 C39 C35 112.5(3) . . ?
F7 C39 C35 112.3(3) . . ?
F5 C39 C35 112.3(3) . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        30.87
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         1.247
_refine_diff_density_min         -1.028
_refine_diff_density_rms         0.095
