# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_ydkr
_database_code_depnum_ccdc_archive 'CCDC 1536337'
_audit_update_record             
;
2017-03-07 deposited with the CCDC.
2017-05-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C38.50 H10 Cl F15 N4 Ni'
_chemical_formula_sum            'C38.50 H10 Cl F15 N4 Ni'
_chemical_formula_weight         907.66

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0041 0.0020 '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 0.0215 0.0127 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0078 0.0041 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3231 1.3236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1720 0.1930 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   31.4500(12)
_cell_length_b                   7.5523(3)
_cell_length_c                   29.4499(10)
_cell_angle_alpha                90
_cell_angle_beta                 111.954(3)
_cell_angle_gamma                90
_cell_volume                     6487.7(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    16661
_cell_measurement_theta_min      2.634
_cell_measurement_theta_max      27.958

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.859
_exptl_crystal_F_000             3592
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.005
_exptl_absorpt_coefficient_mu    1.040
_shelx_estimated_absorpt_T_min   0.921
_shelx_estimated_absorpt_T_max   0.990
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.767
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'ABSCOR (T.Higashi, 2001)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.78201
_diffrn_radiation_type           Synchrotron
_diffrn_source                   'synchrotron radiation SPring-8 BL40XU'
_diffrn_radiation_monochromator  'Si(111) Channel Cut'
_diffrn_measurement_device_type  'Rigaku Saturn 724'
_diffrn_measurement_method       'Oscillation Photograph'
_diffrn_detector_area_resol_mean 29
_diffrn_reflns_number            16661
_diffrn_reflns_av_unetI/netI     0.0574
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         2.634
_diffrn_reflns_theta_max         27.958
_diffrn_reflns_theta_full        27.958
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measured_fraction_theta_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_point_group_measured_fraction_full 0.979
_reflns_number_total             5733
_reflns_number_gt                4772
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Rapid Auto(Rigaku)'
_computing_cell_refinement       'Rapid Auto(Rigaku)'
_computing_data_reduction        'Rapid Auto(Rigaku)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0322P)²+16.9616P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5733
_refine_ls_number_parameters     537
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0400
_refine_ls_wR_factor_ref         0.0990
_refine_ls_wR_factor_gt          0.0917
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.56889(9) 0.9024(3) 0.45698(10) 0.0154(6) Uani 1 1 d . . . . .
H1 H 0.5886 0.9578 0.4435 0.018 Uiso 1 1 calc R U . . .
C2 C 0.52297(9) 0.8915(3) 0.43647(10) 0.0161(6) Uani 1 1 d . . . . .
H2 H 0.5041 0.9350 0.4051 0.019 Uiso 1 1 calc R U . . .
C3 C 0.50750(9) 0.8024(3) 0.47050(9) 0.0141(6) Uani 1 1 d . . . . .
C4 C 0.46239(9) 0.7785(4) 0.46350(10) 0.0155(6) Uani 1 1 d . . . . .
H3 H 0.4399 0.8088 0.4325 0.019 Uiso 1 1 calc R U . . .
C5 C 0.44773(9) 0.7132(3) 0.49880(10) 0.0148(6) Uani 1 1 d . . . . .
C6 C 0.40066(9) 0.7070(4) 0.49407(10) 0.0176(6) Uani 1 1 d . . . . .
H4 H 0.3747 0.7325 0.4654 0.021 Uiso 1 1 calc R U . . .
C7 C 0.40008(9) 0.6581(3) 0.53787(10) 0.0156(6) Uani 1 1 d . . . . .
H5 H 0.3738 0.6444 0.5460 0.019 Uiso 1 1 calc R U . . .
C8 C 0.44714(9) 0.6308(3) 0.56989(10) 0.0138(6) Uani 1 1 d . . . . .
C9 C 0.46120(9) 0.5739(3) 0.61806(10) 0.0148(6) Uani 1 1 d . . . . .
C10 C 0.50525(9) 0.5150(3) 0.64406(10) 0.0151(6) Uani 1 1 d . . . . .
C11 C 0.51941(10) 0.4246(4) 0.69038(10) 0.0188(6) Uani 1 1 d . . . . .
H6 H 0.5027 0.4166 0.7113 0.023 Uiso 1 1 calc R U . . .
C12 C 0.56086(9) 0.3535(4) 0.69841(10) 0.0173(6) Uani 1 1 d . . . . .
H7 H 0.5783 0.2813 0.7254 0.021 Uiso 1 1 calc R U . . .
C13 C 0.57382(9) 0.4072(4) 0.65868(10) 0.0154(6) Uani 1 1 d . . . . .
C14 C 0.61579(9) 0.3676(3) 0.65520(9) 0.0142(6) Uani 1 1 d . . . . .
C15 C 0.63167(9) 0.4575(3) 0.62366(9) 0.0136(5) Uani 1 1 d . . . . .
C16 C 0.67771(9) 0.4460(4) 0.62496(10) 0.0161(6) Uani 1 1 d . . . . .
H8 H 0.7006 0.3639 0.6432 0.019 Uiso 1 1 calc R U . . .
C17 C 0.68216(9) 0.5747(4) 0.59509(10) 0.0179(6) Uani 1 1 d . . . . .
H9 H 0.7093 0.6052 0.5899 0.021 Uiso 1 1 calc R U . . .
C18 C 0.63808(9) 0.6560(3) 0.57277(9) 0.0138(6) Uani 1 1 d . . . . .
C19 C 0.62724(9) 0.7767(4) 0.53414(10) 0.0159(6) Uani 1 1 d . . . . .
C20 C 0.58236(9) 0.8128(3) 0.50376(9) 0.0140(6) Uani 1 1 d . . . . .
C21 C 0.42533(9) 0.5618(4) 0.63990(9) 0.0148(6) Uani 1 1 d . . . . .
C22 C 0.40330(10) 0.7128(4) 0.64696(10) 0.0191(6) Uani 1 1 d . . . . .
C23 C 0.36707(10) 0.7058(4) 0.66265(11) 0.0226(6) Uani 1 1 d . . . . .
C24 C 0.35209(10) 0.5439(4) 0.67216(11) 0.0227(6) Uani 1 1 d . . . . .
C25 C 0.37342(10) 0.3918(4) 0.66651(10) 0.0206(6) Uani 1 1 d . . . . .
C26 C 0.40953(9) 0.4020(3) 0.65072(10) 0.0165(6) Uani 1 1 d . . . . .
C27 C 0.64496(9) 0.2303(4) 0.68902(10) 0.0162(6) Uani 1 1 d . . . . .
C28 C 0.63168(9) 0.0542(4) 0.68453(10) 0.0197(6) Uani 1 1 d . . . . .
C29 C 0.65663(10) -0.0748(4) 0.71652(10) 0.0194(6) Uani 1 1 d . . . . .
C30 C 0.69656(9) -0.0278(4) 0.75475(10) 0.0192(6) Uani 1 1 d . . . . .
C31 C 0.71080(9) 0.1456(4) 0.76048(10) 0.0168(6) Uani 1 1 d . . . . .
C32 C 0.68513(9) 0.2721(3) 0.72784(10) 0.0145(6) Uani 1 1 d . . . . .
C33 C 0.66612(9) 0.8592(4) 0.52425(10) 0.0165(6) Uani 1 1 d . . . . .
C34 C 0.69539(9) 0.9782(4) 0.55762(10) 0.0197(6) Uani 1 1 d . . . . .
C35 C 0.73235(10) 1.0547(4) 0.55061(11) 0.0252(7) Uani 1 1 d . . . . .
C36 C 0.74059(10) 1.0147(4) 0.50888(12) 0.0257(7) Uani 1 1 d . . . . .
C37 C 0.71216(10) 0.8999(4) 0.47478(11) 0.0236(7) Uani 1 1 d . . . . .
C38 C 0.67597(10) 0.8226(4) 0.48312(10) 0.0193(6) Uani 1 1 d . . . . .
N1 N 0.54434(7) 0.7521(3) 0.51185(8) 0.0135(5) Uani 1 1 d . . . . .
N2 N 0.47631(7) 0.6615(3) 0.54538(8) 0.0139(5) Uani 1 1 d . . . . .
N3 N 0.54012(7) 0.5104(3) 0.62587(8) 0.0138(5) Uani 1 1 d . . . . .
N4 N 0.60702(7) 0.5840(3) 0.59039(8) 0.0134(5) Uani 1 1 d . . . . .
F1 F 0.41697(6) 0.8736(2) 0.63788(6) 0.0254(4) Uani 1 1 d . . . . .
F2 F 0.34657(7) 0.8554(2) 0.66809(8) 0.0358(5) Uani 1 1 d . . . . .
F3 F 0.31606(6) 0.5344(2) 0.68594(7) 0.0353(5) Uani 1 1 d . . . . .
F4 F 0.35917(6) 0.2341(2) 0.67637(7) 0.0304(4) Uani 1 1 d . . . . .
F5 F 0.42846(6) 0.2486(2) 0.64453(6) 0.0229(4) Uani 1 1 d . . . . .
F6 F 0.59309(6) 0.0035(2) 0.64730(6) 0.0275(4) Uani 1 1 d . . . . .
F7 F 0.64247(6) -0.2439(2) 0.71124(7) 0.0301(4) Uani 1 1 d . . . . .
F8 F 0.72096(5) -0.1523(2) 0.78616(6) 0.0241(4) Uani 1 1 d . . . . .
F9 F 0.74896(5) 0.1930(2) 0.79807(6) 0.0241(4) Uani 1 1 d . . . . .
F10 F 0.69983(5) 0.4404(2) 0.73490(6) 0.0185(3) Uani 1 1 d . . . . .
F11 F 0.68784(6) 1.0216(2) 0.59826(6) 0.0268(4) Uani 1 1 d . . . . .
F12 F 0.75988(6) 1.1684(2) 0.58363(7) 0.0358(5) Uani 1 1 d . . . . .
F13 F 0.77696(6) 1.0866(2) 0.50213(8) 0.0358(5) Uani 1 1 d . . . . .
F14 F 0.72032(6) 0.8599(2) 0.43426(7) 0.0321(4) Uani 1 1 d . . . . .
F15 F 0.65049(6) 0.7046(2) 0.44983(6) 0.0238(4) Uani 1 1 d . . . . .
C39 C 0.5000 1.0032(7) 0.7500 0.0518(15) Uani 1 2 d S T P . .
H10 H 0.4811 1.0804 0.7227 0.062 Uiso 0.5 1 calc R U P . .
H11 H 0.5189 1.0804 0.7773 0.062 Uiso 0.5 1 calc R U P . .
Cl1 Cl 0.46372(4) 0.87299(14) 0.76965(4) 0.0648(3) Uani 1 1 d . . . . .
Ni1 Ni 0.54191(2) 0.62849(4) 0.56841(2) 0.01233(11) 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
C1 C2 1.343(4) . ?
C1 C20 1.449(4) . ?
C1 H1 0.9500 . ?
C2 C3 1.435(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.367(4) . ?
C3 N1 1.384(3) . ?
C4 C5 1.377(4) . ?
C4 H3 0.9500 . ?
C5 N2 1.386(3) . ?
C5 C6 1.435(4) . ?
C6 C7 1.348(4) . ?
C6 H4 0.9500 . ?
C7 C8 1.442(4) . ?
C7 H5 0.9500 . ?
C8 N2 1.383(3) . ?
C8 C9 1.387(4) . ?
C9 C10 1.382(4) . ?
C9 C21 1.496(4) . ?
C10 N3 1.389(3) . ?
C10 C11 1.439(4) . ?
C11 C12 1.346(4) . ?
C11 H6 0.9500 . ?
C12 C13 1.434(4) . ?
C12 H7 0.9500 . ?
C13 N3 1.378(3) . ?
C13 C14 1.394(4) . ?
C14 C15 1.386(4) . ?
C14 C27 1.492(4) . ?
C15 N4 1.381(3) . ?
C15 C16 1.437(4) . ?
C16 C17 1.353(4) . ?
C16 H8 0.9500 . ?
C17 C18 1.432(4) . ?
C17 H9 0.9500 . ?
C18 N4 1.378(3) . ?
C18 C19 1.397(4) . ?
C19 C20 1.387(4) . ?
C19 C33 1.495(4) . ?
C20 N1 1.382(3) . ?
C21 C26 1.387(4) . ?
C21 C22 1.390(4) . ?
C22 F1 1.348(3) . ?
C22 C23 1.381(4) . ?
C23 F2 1.339(3) . ?
C23 C24 1.377(4) . ?
C24 F3 1.341(3) . ?
C24 C25 1.371(4) . ?
C25 F4 1.341(3) . ?
C25 C26 1.381(4) . ?
C26 F5 1.346(3) . ?
C27 C28 1.386(4) . ?
C27 C32 1.387(4) . ?
C28 F6 1.352(3) . ?
C28 C29 1.378(4) . ?
C29 F7 1.342(3) . ?
C29 C30 1.383(4) . ?
C30 F8 1.341(3) . ?
C30 C31 1.374(4) . ?
C31 F9 1.342(3) . ?
C31 C32 1.381(4) . ?
C32 F10 1.342(3) . ?
C33 C38 1.386(4) . ?
C33 C34 1.394(4) . ?
C34 F11 1.345(3) . ?
C34 C35 1.381(4) . ?
C35 F12 1.343(3) . ?
C35 C36 1.381(5) . ?
C36 F13 1.347(3) . ?
C36 C37 1.374(4) . ?
C37 F14 1.346(3) . ?
C37 C38 1.380(4) . ?
C38 F15 1.346(3) . ?
N1 Ni1 1.936(2) . ?
N2 Ni1 1.932(2) . ?
N3 Ni1 1.932(2) . ?
N4 Ni1 1.932(2) . ?
C39 Cl1 1.760(3) 2_656 ?
C39 Cl1 1.760(3) . ?
C39 H10 0.9900 . ?
C39 H11 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
C2 C1 C20 106.4(2) . . ?
C2 C1 H1 126.8 . . ?
C20 C1 H1 126.8 . . ?
C1 C2 C3 107.6(2) . . ?
C1 C2 H2 126.2 . . ?
C3 C2 H2 126.2 . . ?
C4 C3 N1 125.2(2) . . ?
C4 C3 C2 124.1(2) . . ?
N1 C3 C2 110.6(2) . . ?
C3 C4 C5 123.7(2) . . ?
C3 C4 H3 118.1 . . ?
C5 C4 H3 118.1 . . ?
C4 C5 N2 124.9(2) . . ?
C4 C5 C6 124.3(2) . . ?
N2 C5 C6 110.5(2) . . ?
C7 C6 C5 107.4(2) . . ?
C7 C6 H4 126.3 . . ?
C5 C6 H4 126.3 . . ?
C6 C7 C8 106.7(2) . . ?
C6 C7 H5 126.7 . . ?
C8 C7 H5 126.7 . . ?
N2 C8 C9 124.5(2) . . ?
N2 C8 C7 110.7(2) . . ?
C9 C8 C7 124.8(2) . . ?
C10 C9 C8 122.4(2) . . ?
C10 C9 C21 120.2(2) . . ?
C8 C9 C21 117.1(2) . . ?
C9 C10 N3 124.5(2) . . ?
C9 C10 C11 124.7(2) . . ?
N3 C10 C11 110.1(2) . . ?
C12 C11 C10 107.0(2) . . ?
C12 C11 H6 126.5 . . ?
C10 C11 H6 126.5 . . ?
C11 C12 C13 107.2(2) . . ?
C11 C12 H7 126.4 . . ?
C13 C12 H7 126.4 . . ?
N3 C13 C14 124.8(2) . . ?
N3 C13 C12 110.7(2) . . ?
C14 C13 C12 124.4(2) . . ?
C15 C14 C13 122.2(2) . . ?
C15 C14 C27 120.1(2) . . ?
C13 C14 C27 117.6(2) . . ?
N4 C15 C14 124.6(2) . . ?
N4 C15 C16 110.7(2) . . ?
C14 C15 C16 124.4(2) . . ?
C17 C16 C15 106.7(2) . . ?
C17 C16 H8 126.6 . . ?
C15 C16 H8 126.6 . . ?
C16 C17 C18 106.8(2) . . ?
C16 C17 H9 126.6 . . ?
C18 C17 H9 126.6 . . ?
N4 C18 C19 124.9(2) . . ?
N4 C18 C17 111.0(2) . . ?
C19 C18 C17 123.6(2) . . ?
C20 C19 C18 122.2(3) . . ?
C20 C19 C33 120.1(2) . . ?
C18 C19 C33 117.5(2) . . ?
N1 C20 C19 124.2(2) . . ?
N1 C20 C1 110.8(2) . . ?
C19 C20 C1 124.8(2) . . ?
C26 C21 C22 116.0(2) . . ?
C26 C21 C9 123.0(2) . . ?
C22 C21 C9 120.8(2) . . ?
F1 C22 C23 117.7(2) . . ?
F1 C22 C21 119.7(2) . . ?
C23 C22 C21 122.6(3) . . ?
F2 C23 C24 120.6(3) . . ?
F2 C23 C22 120.1(3) . . ?
C24 C23 C22 119.3(3) . . ?
F3 C24 C25 119.9(3) . . ?
F3 C24 C23 120.1(3) . . ?
C25 C24 C23 120.0(3) . . ?
F4 C25 C24 119.9(2) . . ?
F4 C25 C26 120.4(3) . . ?
C24 C25 C26 119.7(3) . . ?
F5 C26 C25 117.3(2) . . ?
F5 C26 C21 120.2(2) . . ?
C25 C26 C21 122.4(2) . . ?
C28 C27 C32 116.5(2) . . ?
C28 C27 C14 121.0(2) . . ?
C32 C27 C14 122.4(2) . . ?
F6 C28 C29 117.6(2) . . ?
F6 C28 C27 119.7(2) . . ?
C29 C28 C27 122.6(3) . . ?
F7 C29 C28 120.9(2) . . ?
F7 C29 C30 119.9(3) . . ?
C28 C29 C30 119.1(3) . . ?
F8 C30 C31 120.5(2) . . ?
F8 C30 C29 119.5(3) . . ?
C31 C30 C29 120.0(3) . . ?
F9 C31 C30 120.4(2) . . ?
F9 C31 C32 119.9(2) . . ?
C30 C31 C32 119.7(2) . . ?
F10 C32 C31 118.0(2) . . ?
F10 C32 C27 119.9(2) . . ?
C31 C32 C27 122.1(3) . . ?
C38 C33 C34 116.1(3) . . ?
C38 C33 C19 123.6(2) . . ?
C34 C33 C19 120.2(2) . . ?
F11 C34 C35 118.0(3) . . ?
F11 C34 C33 119.7(2) . . ?
C35 C34 C33 122.3(3) . . ?
F12 C35 C34 120.7(3) . . ?
F12 C35 C36 120.0(3) . . ?
C34 C35 C36 119.3(3) . . ?
F13 C36 C37 120.2(3) . . ?
F13 C36 C35 119.7(3) . . ?
C37 C36 C35 120.1(3) . . ?
F14 C37 C36 120.1(3) . . ?
F14 C37 C38 120.4(3) . . ?
C36 C37 C38 119.4(3) . . ?
F15 C38 C37 117.2(3) . . ?
F15 C38 C33 120.1(2) . . ?
C37 C38 C33 122.7(3) . . ?
C20 N1 C3 104.5(2) . . ?
C20 N1 Ni1 128.56(18) . . ?
C3 N1 Ni1 126.88(18) . . ?
C8 N2 C5 104.6(2) . . ?
C8 N2 Ni1 128.68(18) . . ?
C5 N2 Ni1 126.61(18) . . ?
C13 N3 C10 104.8(2) . . ?
C13 N3 Ni1 127.49(17) . . ?
C10 N3 Ni1 127.72(18) . . ?
C18 N4 C15 104.6(2) . . ?
C18 N4 Ni1 128.10(17) . . ?
C15 N4 Ni1 126.98(17) . . ?
Cl1 C39 Cl1 112.0(3) 2_656 . ?
Cl1 C39 H10 109.2 2_656 . ?
Cl1 C39 H10 109.2 . . ?
Cl1 C39 H11 109.2 2_656 . ?
Cl1 C39 H11 109.2 . . ?
H10 C39 H11 107.9 . . ?
N2 Ni1 N3 89.44(9) . . ?
N2 Ni1 N4 177.28(9) . . ?
N3 Ni1 N4 90.03(9) . . ?
N2 Ni1 N1 90.93(9) . . ?
N3 Ni1 N1 178.53(10) . . ?
N4 Ni1 N1 89.67(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C20 C1 C2 C3 2.1(3) . . . . ?
C1 C2 C3 C4 175.2(3) . . . . ?
C1 C2 C3 N1 -2.1(3) . . . . ?
N1 C3 C4 C5 5.4(4) . . . . ?
C2 C3 C4 C5 -171.5(3) . . . . ?
C3 C4 C5 N2 -0.8(4) . . . . ?
C3 C4 C5 C6 172.3(3) . . . . ?
C4 C5 C6 C7 -171.7(3) . . . . ?
N2 C5 C6 C7 2.2(3) . . . . ?
C5 C6 C7 C8 -1.0(3) . . . . ?
C6 C7 C8 N2 -0.5(3) . . . . ?
C6 C7 C8 C9 -177.9(3) . . . . ?
N2 C8 C9 C10 -10.6(4) . . . . ?
C7 C8 C9 C10 166.4(3) . . . . ?
N2 C8 C9 C21 175.1(2) . . . . ?
C7 C8 C9 C21 -7.9(4) . . . . ?
C8 C9 C10 N3 1.8(4) . . . . ?
C21 C9 C10 N3 175.8(2) . . . . ?
C8 C9 C10 C11 -167.9(3) . . . . ?
C21 C9 C10 C11 6.2(4) . . . . ?
C9 C10 C11 C12 166.1(3) . . . . ?
N3 C10 C11 C12 -4.8(3) . . . . ?
C10 C11 C12 C13 3.1(3) . . . . ?
C11 C12 C13 N3 -0.5(3) . . . . ?
C11 C12 C13 C14 176.5(3) . . . . ?
N3 C13 C14 C15 13.4(4) . . . . ?
C12 C13 C14 C15 -163.1(3) . . . . ?
N3 C13 C14 C27 -170.1(2) . . . . ?
C12 C13 C14 C27 13.4(4) . . . . ?
C13 C14 C15 N4 -4.9(4) . . . . ?
C27 C14 C15 N4 178.7(2) . . . . ?
C13 C14 C15 C16 167.8(3) . . . . ?
C27 C14 C15 C16 -8.6(4) . . . . ?
N4 C15 C16 C17 4.4(3) . . . . ?
C14 C15 C16 C17 -169.2(3) . . . . ?
C15 C16 C17 C18 -4.2(3) . . . . ?
C16 C17 C18 N4 2.8(3) . . . . ?
C16 C17 C18 C19 -170.1(3) . . . . ?
N4 C18 C19 C20 -11.7(4) . . . . ?
C17 C18 C19 C20 160.1(3) . . . . ?
N4 C18 C19 C33 172.1(2) . . . . ?
C17 C18 C19 C33 -16.0(4) . . . . ?
C18 C19 C20 N1 8.3(4) . . . . ?
C33 C19 C20 N1 -175.6(2) . . . . ?
C18 C19 C20 C1 -164.8(3) . . . . ?
C33 C19 C20 C1 11.3(4) . . . . ?
C2 C1 C20 N1 -1.5(3) . . . . ?
C2 C1 C20 C19 172.4(3) . . . . ?
C10 C9 C21 C26 -64.7(4) . . . . ?
C8 C9 C21 C26 109.7(3) . . . . ?
C10 C9 C21 C22 120.4(3) . . . . ?
C8 C9 C21 C22 -65.2(4) . . . . ?
C26 C21 C22 F1 179.2(2) . . . . ?
C9 C21 C22 F1 -5.6(4) . . . . ?
C26 C21 C22 C23 -1.5(4) . . . . ?
C9 C21 C22 C23 173.7(3) . . . . ?
F1 C22 C23 F2 0.4(4) . . . . ?
C21 C22 C23 F2 -178.9(3) . . . . ?
F1 C22 C23 C24 179.8(3) . . . . ?
C21 C22 C23 C24 0.5(5) . . . . ?
F2 C23 C24 F3 1.5(5) . . . . ?
C22 C23 C24 F3 -177.9(3) . . . . ?
F2 C23 C24 C25 -179.9(3) . . . . ?
C22 C23 C24 C25 0.7(5) . . . . ?
F3 C24 C25 F4 -2.2(4) . . . . ?
C23 C24 C25 F4 179.2(3) . . . . ?
F3 C24 C25 C26 177.8(3) . . . . ?
C23 C24 C25 C26 -0.8(5) . . . . ?
F4 C25 C26 F5 1.8(4) . . . . ?
C24 C25 C26 F5 -178.3(3) . . . . ?
F4 C25 C26 C21 179.7(2) . . . . ?
C24 C25 C26 C21 -0.3(4) . . . . ?
C22 C21 C26 F5 179.3(2) . . . . ?
C9 C21 C26 F5 4.2(4) . . . . ?
C22 C21 C26 C25 1.4(4) . . . . ?
C9 C21 C26 C25 -173.7(3) . . . . ?
C15 C14 C27 C28 -115.5(3) . . . . ?
C13 C14 C27 C28 67.9(3) . . . . ?
C15 C14 C27 C32 68.0(4) . . . . ?
C13 C14 C27 C32 -108.6(3) . . . . ?
C32 C27 C28 F6 -179.4(2) . . . . ?
C14 C27 C28 F6 3.9(4) . . . . ?
C32 C27 C28 C29 -0.1(4) . . . . ?
C14 C27 C28 C29 -176.8(3) . . . . ?
F6 C28 C29 F7 -1.2(4) . . . . ?
C27 C28 C29 F7 179.4(3) . . . . ?
F6 C28 C29 C30 179.3(2) . . . . ?
C27 C28 C29 C30 0.0(4) . . . . ?
F7 C29 C30 F8 0.3(4) . . . . ?
C28 C29 C30 F8 179.7(3) . . . . ?
F7 C29 C30 C31 -179.3(3) . . . . ?
C28 C29 C30 C31 0.1(4) . . . . ?
F8 C30 C31 F9 -1.1(4) . . . . ?
C29 C30 C31 F9 178.6(2) . . . . ?
F8 C30 C31 C32 -179.8(2) . . . . ?
C29 C30 C31 C32 -0.2(4) . . . . ?
F9 C31 C32 F10 0.5(4) . . . . ?
C30 C31 C32 F10 179.3(2) . . . . ?
F9 C31 C32 C27 -178.6(2) . . . . ?
C30 C31 C32 C27 0.1(4) . . . . ?
C28 C27 C32 F10 -179.1(2) . . . . ?
C14 C27 C32 F10 -2.5(4) . . . . ?
C28 C27 C32 C31 0.0(4) . . . . ?
C14 C27 C32 C31 176.7(2) . . . . ?
C20 C19 C33 C38 -65.7(4) . . . . ?
C18 C19 C33 C38 110.6(3) . . . . ?
C20 C19 C33 C34 115.3(3) . . . . ?
C18 C19 C33 C34 -68.4(3) . . . . ?
C38 C33 C34 F11 179.4(2) . . . . ?
C19 C33 C34 F11 -1.5(4) . . . . ?
C38 C33 C34 C35 -0.5(4) . . . . ?
C19 C33 C34 C35 178.5(3) . . . . ?
F11 C34 C35 F12 0.3(4) . . . . ?
C33 C34 C35 F12 -179.8(3) . . . . ?
F11 C34 C35 C36 -179.1(3) . . . . ?
C33 C34 C35 C36 0.9(4) . . . . ?
F12 C35 C36 F13 1.7(4) . . . . ?
C34 C35 C36 F13 -179.0(3) . . . . ?
F12 C35 C36 C37 -179.3(3) . . . . ?
C34 C35 C36 C37 0.0(4) . . . . ?
F13 C36 C37 F14 -0.5(4) . . . . ?
C35 C36 C37 F14 -179.6(3) . . . . ?
F13 C36 C37 C38 177.8(3) . . . . ?
C35 C36 C37 C38 -1.3(4) . . . . ?
F14 C37 C38 F15 1.5(4) . . . . ?
C36 C37 C38 F15 -176.8(3) . . . . ?
F14 C37 C38 C33 179.9(3) . . . . ?
C36 C37 C38 C33 1.7(4) . . . . ?
C34 C33 C38 F15 177.7(2) . . . . ?
C19 C33 C38 F15 -1.4(4) . . . . ?
C34 C33 C38 C37 -0.7(4) . . . . ?
C19 C33 C38 C37 -179.8(3) . . . . ?
C19 C20 N1 C3 -173.7(3) . . . . ?
C1 C20 N1 C3 0.3(3) . . . . ?
C19 C20 N1 Ni1 7.4(4) . . . . ?
C1 C20 N1 Ni1 -178.60(18) . . . . ?
C4 C3 N1 C20 -176.2(3) . . . . ?
C2 C3 N1 C20 1.1(3) . . . . ?
C4 C3 N1 Ni1 2.7(4) . . . . ?
C2 C3 N1 Ni1 179.95(17) . . . . ?
C9 C8 N2 C5 179.2(3) . . . . ?
C7 C8 N2 C5 1.9(3) . . . . ?
C9 C8 N2 Ni1 2.4(4) . . . . ?
C7 C8 N2 Ni1 -175.01(17) . . . . ?
C4 C5 N2 C8 171.4(3) . . . . ?
C6 C5 N2 C8 -2.5(3) . . . . ?
C4 C5 N2 Ni1 -11.6(4) . . . . ?
C6 C5 N2 Ni1 174.49(18) . . . . ?
C14 C13 N3 C10 -179.4(3) . . . . ?
C12 C13 N3 C10 -2.4(3) . . . . ?
C14 C13 N3 Ni1 -1.1(4) . . . . ?
C12 C13 N3 Ni1 175.86(18) . . . . ?
C9 C10 N3 C13 -166.6(3) . . . . ?
C11 C10 N3 C13 4.4(3) . . . . ?
C9 C10 N3 Ni1 15.1(4) . . . . ?
C11 C10 N3 Ni1 -173.90(18) . . . . ?
C19 C18 N4 C15 172.7(2) . . . . ?
C17 C18 N4 C15 -0.1(3) . . . . ?
C19 C18 N4 Ni1 -0.8(4) . . . . ?
C17 C18 N4 Ni1 -173.54(18) . . . . ?
C14 C15 N4 C18 171.0(2) . . . . ?
C16 C15 N4 C18 -2.6(3) . . . . ?
C14 C15 N4 Ni1 -15.5(4) . . . . ?
C16 C15 N4 Ni1 170.97(18) . . . . ?

_refine_diff_density_max         0.371
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.072

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1536338'
_audit_update_record             
;
2017-03-07 deposited with the CCDC.
2017-05-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H21.50 F15 N4 Ni O3'
_chemical_formula_weight         997.86

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 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'
O O 0.0105 0.0059 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0059 0.0032 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0170 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3420 1.0892 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.309(3)
_cell_length_b                   14.459(6)
_cell_length_c                   20.126(8)
_cell_angle_alpha                72.365(5)
_cell_angle_beta                 80.781(6)
_cell_angle_gamma                78.319(6)
_cell_volume                     1974.0(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    19562
_cell_measurement_theta_min      1.052
_cell_measurement_theta_max      27.060

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_F_000             1001
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.586
_shelx_estimated_absorpt_T_min   0.944
_shelx_estimated_absorpt_T_max   0.944
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7006
_diffrn_radiation_type           synchrotron
_diffrn_radiation_monochromator  'Si 311'
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku MercuryCCD2'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19562
_diffrn_reflns_av_unetI/netI     0.2367
_diffrn_reflns_av_R_equivalents  0.1536
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.052
_diffrn_reflns_theta_max         27.060
_diffrn_reflns_theta_full        24.857
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             8927
_reflns_number_gt                3605
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       RAPID-AUTO
_computing_cell_refinement       RAPID-AUTO
_computing_data_reduction        RAPID-AUTO
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.2000P)²]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8927
_refine_ls_number_parameters     616
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.2688
_refine_ls_R_factor_gt           0.1424
_refine_ls_wR_factor_ref         0.4202
_refine_ls_wR_factor_gt          0.3412
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_restrained_S_all      1.072
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2077(14) 0.5675(8) 0.4862(6) 0.029(2) Uani 1 1 d . . . . .
C2 C 0.2274(16) 0.6590(8) 0.4416(6) 0.035(3) Uani 1 1 d . . . . .
C3 C 0.1443(16) 0.7479(8) 0.4592(7) 0.042(3) Uani 1 1 d . . . . .
H3 H 0.0575 0.7544 0.4987 0.051 Uiso 1 1 calc R U . . .
C4 C 0.2139(16) 0.8206(8) 0.4085(6) 0.038(3) Uani 1 1 d . . . . .
H4 H 0.1907 0.8883 0.4067 0.045 Uiso 1 1 calc R U . . .
C5 C 0.3303(15) 0.7769(8) 0.3574(5) 0.029(2) Uani 1 1 d . . . . .
C6 C 0.4100(14) 0.8295(8) 0.2952(6) 0.031(2) Uani 1 1 d . . . . .
C7 C 0.4936(15) 0.7864(7) 0.2430(5) 0.027(2) Uani 1 1 d . . . . .
C8 C 0.5511(17) 0.8421(10) 0.1742(7) 0.045(3) Uani 1 1 d . . . . .
H8 H 0.5506 0.9111 0.1585 0.054 Uiso 1 1 calc R U . . .
C9 C 0.6060(15) 0.7786(8) 0.1359(7) 0.038(3) Uani 1 1 d . . . . .
H9 H 0.6533 0.7934 0.0877 0.045 Uiso 1 1 calc R U . . .
C10 C 0.5802(14) 0.6851(8) 0.1807(6) 0.032(3) Uani 1 1 d . . . . .
C11 C 0.6259(14) 0.5991(8) 0.1613(6) 0.032(3) Uani 1 1 d . . . . .
C12 C 0.6260(16) 0.5080(9) 0.2092(6) 0.034(3) Uani 1 1 d . . . . .
C13 C 0.6960(15) 0.4211(8) 0.1911(6) 0.033(3) Uani 1 1 d . . . . .
H13 H 0.7376 0.4159 0.1449 0.039 Uiso 1 1 calc R U . . .
C14 C 0.6951(14) 0.3486(8) 0.2474(5) 0.026(2) Uani 1 1 d . . . . .
H14 H 0.7421 0.2812 0.2508 0.031 Uiso 1 1 calc R U . . .
C15 C 0.6091(14) 0.3893(8) 0.3041(6) 0.028(2) Uani 1 1 d . . . . .
C16 C 0.5718(14) 0.3382(8) 0.3716(6) 0.030(2) Uani 1 1 d . . . . .
C17 C 0.4656(15) 0.3796(8) 0.4220(6) 0.035(3) Uani 1 1 d . . . . .
C18 C 0.4044(16) 0.3268(8) 0.4890(6) 0.035(3) Uani 1 1 d . . . . .
H18 H 0.4315 0.2576 0.5086 0.043 Uiso 1 1 calc R U . . .
C19 C 0.3027(15) 0.3902(7) 0.5199(6) 0.028(2) Uani 1 1 d . . . . .
H19 H 0.2426 0.3750 0.5665 0.034 Uiso 1 1 calc R U . . .
C20 C 0.2969(14) 0.4836(8) 0.4733(5) 0.027(2) Uani 1 1 d . . . . .
C21 C 0.4001(15) 0.9365(8) 0.2814(6) 0.032(3) Uani 1 1 d . . . . .
C22 C 0.2379(15) 1.0010(8) 0.2722(6) 0.035(3) Uani 1 1 d . . . . .
C23 C 0.2290(15) 1.1014(8) 0.2572(6) 0.036(3) Uani 1 1 d . . . . .
C24 C 0.3911(18) 1.1372(9) 0.2497(7) 0.043(3) Uani 1 1 d . . . . .
C25 C 0.5547(17) 1.0765(8) 0.2574(7) 0.039(3) Uani 1 1 d . . . . .
C26 C 0.5626(13) 0.9697(9) 0.2791(6) 0.030(3) Uani 1 1 d . . . . .
C27 C 0.6843(16) 0.6069(7) 0.0863(6) 0.030(2) Uani 1 1 d . . . . .
C28 C 0.5662(16) 0.6066(10) 0.0400(7) 0.048(3) Uani 1 1 d . . . . .
C29 C 0.6206(18) 0.6145(11) -0.0267(6) 0.046(3) Uani 1 1 d . . . . .
C30 C 0.8036(17) 0.6175(10) -0.0522(6) 0.041(3) Uani 1 1 d . . . . .
C31 C 0.9234(17) 0.6184(10) -0.0099(7) 0.046(3) Uani 1 1 d . . . . .
C32 C 0.8684(15) 0.6128(9) 0.0571(6) 0.036(3) Uani 1 1 d . . . . .
C33 C 0.6230(15) 0.2304(8) 0.3885(6) 0.033(3) Uani 1 1 d . . . . .
C34 C 0.8121(15) 0.1881(8) 0.3930(6) 0.032(3) Uani 1 1 d . . . . .
C35 C 0.8636(15) 0.0882(9) 0.4112(6) 0.035(3) Uani 1 1 d . . . . .
C36 C 0.7351(17) 0.0285(8) 0.4223(6) 0.033(3) Uani 1 1 d . . . . .
C37 C 0.5540(17) 0.0668(8) 0.4168(6) 0.035(3) Uani 1 1 d . . . . .
C38 C 0.4990(15) 0.1685(8) 0.4010(6) 0.033(3) Uani 1 1 d . . . . .
C39 C 0.0359(17) 0.5613(10) 0.2878(7) 0.042(3) Uani 1 1 d . . . . .
C40 C 0.0985(19) 0.4612(9) 0.2797(7) 0.051(4) Uani 1 1 d . . . . .
H40A H -0.0039 0.4400 0.2649 0.076 Uiso 1 1 calc R U . . .
H40B H 0.1337 0.4157 0.3245 0.076 Uiso 1 1 calc R U . . .
H40C H 0.2072 0.4614 0.2441 0.076 Uiso 1 1 calc R U . . .
C41 C 0.0189(18) 0.7301(8) 0.2386(7) 0.044(3) Uani 1 1 d . . . . .
H41A H -0.1182 0.7431 0.2518 0.052 Uiso 1 1 calc R U . . .
H41B H 0.0842 0.7411 0.2743 0.052 Uiso 1 1 calc R U . . .
C42 C 0.068(2) 0.7939(10) 0.1707(7) 0.055(4) Uani 1 1 d . . . . .
H42A H 0.0066 0.7804 0.1356 0.083 Uiso 1 1 calc R U . . .
H42B H 0.2044 0.7824 0.1591 0.083 Uiso 1 1 calc R U . . .
H42C H 0.0258 0.8626 0.1711 0.083 Uiso 1 1 calc R U . . .
O1 O 0.1036(11) 0.5700(6) 0.5473(4) 0.0367(19) Uani 1 1 d . . . . .
H1 H -0.0086 0.5936 0.5399 0.055 Uiso 1 1 calc R U . . .
O2 O -0.0471(12) 0.5778(5) 0.3433(5) 0.046(2) Uani 1 1 d . . . . .
O3 O 0.0759(11) 0.6309(6) 0.2342(4) 0.0381(19) Uani 1 1 d . . . . .
N1 N 0.3338(12) 0.6773(6) 0.3762(5) 0.029(2) Uani 1 1 d . . . . .
N2 N 0.5097(12) 0.6901(6) 0.2483(5) 0.032(2) Uani 1 1 d . . . . .
N3 N 0.5741(12) 0.4916(6) 0.2774(5) 0.032(2) Uani 1 1 d . . . . .
N4 N 0.4041(12) 0.4785(6) 0.4115(5) 0.031(2) Uani 1 1 d . . . . .
F1 F 0.0771(8) 0.9689(4) 0.2769(4) 0.0440(18) Uani 1 1 d . . . . .
F2 F 0.0663(9) 1.1605(5) 0.2501(4) 0.053(2) Uani 1 1 d . . . . .
F3 F 0.3838(10) 1.2339(5) 0.2346(4) 0.0511(19) Uani 1 1 d . . . . .
F4 F 0.7148(9) 1.1118(5) 0.2502(4) 0.0487(19) Uani 1 1 d . . . . .
F5 F 0.7261(9) 0.9188(5) 0.2826(4) 0.0452(18) Uani 1 1 d . . . . .
F6 F 0.3878(10) 0.5997(7) 0.0657(4) 0.074(3) Uani 1 1 d . . . . .
F7 F 0.4979(11) 0.6123(9) -0.0692(4) 0.089(3) Uani 1 1 d . . . . .
F8 F 0.8568(11) 0.6234(7) -0.1199(4) 0.068(2) Uani 1 1 d . . . . .
F9 F 1.1044(9) 0.6240(7) -0.0352(4) 0.062(2) Uani 1 1 d . . . . .
F10 F 0.9935(9) 0.6113(6) 0.0993(4) 0.059(2) Uani 1 1 d . . . . .
F11 F 0.9412(8) 0.2427(4) 0.3816(3) 0.0353(15) Uani 1 1 d . . . . .
F12 F 1.0449(9) 0.0502(5) 0.4165(4) 0.0427(17) Uani 1 1 d . . . . .
F13 F 0.7850(9) -0.0679(5) 0.4400(4) 0.0480(18) Uani 1 1 d . . . . .
F14 F 0.4234(9) 0.0103(5) 0.4271(4) 0.0444(17) Uani 1 1 d . . . . .
F15 F 0.3189(8) 0.2041(5) 0.3939(4) 0.0426(17) Uani 1 1 d . . . . .
Ni1 Ni 0.45636(19) 0.58408(10) 0.32880(8) 0.0296(4) Uani 1 1 d . . . . .
C43 C 1.9142(16) 0.118(4) 0.063(3) 0.083(8) Uiso 0.25 1 d D . P A 1
H43A H 1.9819 0.0839 0.1037 0.125 Uiso 0.25 1 calc R U P A 1
H43B H 1.9639 0.1791 0.0374 0.125 Uiso 0.25 1 calc R U P A 1
H43C H 1.9307 0.0760 0.0314 0.125 Uiso 0.25 1 calc R U P A 1
C44 C 1.7064(19) 0.143(3) 0.0860(19) 0.083(8) Uiso 0.25 1 d D . P A 1
H44A H 1.6776 0.2157 0.0766 0.100 Uiso 0.25 1 calc R U P A 1
H44B H 1.6906 0.1154 0.1375 0.100 Uiso 0.25 1 calc R U P A 1
C45 C 1.5535(16) 0.113(3) 0.0576(13) 0.083(8) Uiso 0.25 1 d D . P A 1
H45A H 1.6067 0.0494 0.0483 0.100 Uiso 0.25 1 calc R U P A 1
H45B H 1.5334 0.1617 0.0114 0.100 Uiso 0.25 1 calc R U P A 1
C46 C 1.3601(18) 0.103(2) 0.0972(11) 0.083(8) Uiso 0.25 1 d D . P A 1
H46A H 1.3756 0.0410 0.1355 0.100 Uiso 0.25 1 calc R U P A 1
H46B H 1.3247 0.1570 0.1200 0.100 Uiso 0.25 1 calc R U P A 1
C47 C 1.1911(15) 0.1029(12) 0.0621(15) 0.083(8) Uiso 0.25 1 d D . P A 1
H47A H 1.2025 0.1500 0.0149 0.100 Uiso 0.25 1 calc R U P A 1
H47B H 1.0790 0.1312 0.0886 0.100 Uiso 0.25 1 calc R U P A 1
C48 C 1.146(2) 0.0101(14) 0.0523(17) 0.083(8) Uiso 0.25 1 d D . P A 1
H48A H 1.1867 -0.0486 0.0907 0.100 Uiso 0.25 1 calc R U P A 1
H48B H 1.2048 -0.0003 0.0068 0.100 Uiso 0.25 1 calc R U P A 1
C49 C 0.933(2) 0.033(2) 0.055(3) 0.083(8) Uiso 0.25 1 d D . P A 1
H49A H 0.9016 0.0265 0.0101 0.100 Uiso 0.25 1 calc R U P A 1
H49B H 0.8838 -0.0210 0.0926 0.100 Uiso 0.25 1 calc R U P A 1
C50 C 0.8181(15) 0.1285(19) 0.065(3) 0.083(8) Uiso 0.25 1 d D . P A 1
H50A H 0.8535 0.1409 0.1057 0.125 Uiso 0.25 1 calc R U P A 1
H50B H 0.6841 0.1239 0.0716 0.125 Uiso 0.25 1 calc R U P A 1
H50C H 0.8429 0.1827 0.0229 0.125 Uiso 0.25 1 calc R U P A 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
C1 C20 1.334(15) . ?
C1 O1 1.346(13) . ?
C1 C2 1.376(15) . ?
C2 N1 1.398(14) . ?
C2 C3 1.427(15) . ?
C3 C4 1.343(17) . ?
C3 H3 0.9500 . ?
C4 C5 1.442(15) . ?
C4 H4 0.9500 . ?
C5 C6 1.362(15) . ?
C5 N1 1.370(13) . ?
C6 C7 1.379(15) . ?
C6 C21 1.475(15) . ?
C7 N2 1.346(13) . ?
C7 C8 1.420(16) . ?
C8 C9 1.334(16) . ?
C8 H8 0.9500 . ?
C9 C10 1.409(16) . ?
C9 H9 0.9500 . ?
C10 C11 1.377(15) . ?
C10 N2 1.393(14) . ?
C11 C12 1.377(16) . ?
C11 C27 1.478(15) . ?
C12 N3 1.325(14) . ?
C12 C13 1.390(15) . ?
C13 C14 1.290(15) . ?
C13 H13 0.9500 . ?
C14 C15 1.439(14) . ?
C14 H14 0.9500 . ?
C15 C16 1.349(15) . ?
C15 N3 1.398(13) . ?
C16 C17 1.385(16) . ?
C16 C33 1.473(15) . ?
C17 N4 1.370(14) . ?
C17 C18 1.386(16) . ?
C18 C19 1.305(15) . ?
C18 H18 0.9500 . ?
C19 C20 1.388(15) . ?
C19 H19 0.9500 . ?
C20 N4 1.374(13) . ?
C21 C22 1.352(15) . ?
C21 C26 1.357(13) . ?
C22 F1 1.328(11) . ?
C22 C23 1.381(15) . ?
C23 F2 1.317(12) . ?
C23 C24 1.355(15) . ?
C24 F3 1.330(13) . ?
C24 C25 1.332(16) . ?
C25 F4 1.339(12) . ?
C25 C26 1.465(16) . ?
C26 F5 1.271(11) . ?
C27 C28 1.370(15) . ?
C27 C32 1.388(15) . ?
C28 C29 1.313(17) . ?
C28 F6 1.335(13) . ?
C29 F7 1.347(13) . ?
C29 C30 1.358(16) . ?
C30 C31 1.319(16) . ?
C30 F8 1.339(13) . ?
C31 C32 1.326(16) . ?
C31 F9 1.349(13) . ?
C32 F10 1.337(12) . ?
C33 C38 1.344(15) . ?
C33 C34 1.399(15) . ?
C34 F11 1.300(11) . ?
C34 C35 1.366(16) . ?
C35 F12 1.335(12) . ?
C35 C36 1.350(15) . ?
C36 F13 1.317(12) . ?
C36 C37 1.336(16) . ?
C37 F14 1.331(12) . ?
C37 C38 1.394(15) . ?
C38 F15 1.327(12) . ?
C39 O2 1.249(14) . ?
C39 O3 1.274(14) . ?
C39 C40 1.477(18) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 C42 1.434(17) . ?
C41 O3 1.437(13) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
O1 H1 0.8400 . ?
N1 Ni1 1.882(9) . ?
N2 Ni1 1.913(9) . ?
N3 Ni1 1.919(9) . ?
N4 Ni1 1.934(9) . ?
C43 C44 1.5199(12) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 C45 1.5200(11) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 C46 1.5200(12) . ?
C45 C50 2.021(9) 1_655 ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.5199(11) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.5200(12) . ?
C47 C43 1.989(7) 1_455 ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 C49 1.5200(12) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 C50 1.5200(12) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?

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
C20 C1 O1 122.4(10) . . ?
C20 C1 C2 123.6(10) . . ?
O1 C1 C2 113.7(10) . . ?
C1 C2 N1 125.4(10) . . ?
C1 C2 C3 122.7(11) . . ?
N1 C2 C3 111.8(10) . . ?
C4 C3 C2 106.0(11) . . ?
C4 C3 H3 127.0 . . ?
C2 C3 H3 127.0 . . ?
C3 C4 C5 107.4(10) . . ?
C3 C4 H4 126.3 . . ?
C5 C4 H4 126.3 . . ?
C6 C5 N1 124.5(10) . . ?
C6 C5 C4 123.9(10) . . ?
N1 C5 C4 111.2(10) . . ?
C5 C6 C7 121.8(10) . . ?
C5 C6 C21 119.6(10) . . ?
C7 C6 C21 118.6(10) . . ?
N2 C7 C6 124.6(10) . . ?
N2 C7 C8 112.4(10) . . ?
C6 C7 C8 122.6(10) . . ?
C9 C8 C7 106.5(11) . . ?
C9 C8 H8 126.7 . . ?
C7 C8 H8 126.7 . . ?
C8 C9 C10 106.8(11) . . ?
C8 C9 H9 126.6 . . ?
C10 C9 H9 126.6 . . ?
C11 C10 N2 124.1(10) . . ?
C11 C10 C9 124.6(11) . . ?
N2 C10 C9 111.3(10) . . ?
C12 C11 C10 122.4(11) . . ?
C12 C11 C27 120.0(10) . . ?
C10 C11 C27 117.5(10) . . ?
N3 C12 C11 125.6(10) . . ?
N3 C12 C13 111.9(10) . . ?
C11 C12 C13 122.4(10) . . ?
C14 C13 C12 108.6(10) . . ?
C14 C13 H13 125.7 . . ?
C12 C13 H13 125.7 . . ?
C13 C14 C15 106.8(10) . . ?
C13 C14 H14 126.6 . . ?
C15 C14 H14 126.6 . . ?
C16 C15 N3 125.6(10) . . ?
C16 C15 C14 126.3(10) . . ?
N3 C15 C14 108.1(9) . . ?
C15 C16 C17 123.8(10) . . ?
C15 C16 C33 116.6(10) . . ?
C17 C16 C33 118.9(10) . . ?
N4 C17 C16 124.1(11) . . ?
N4 C17 C18 111.2(10) . . ?
C16 C17 C18 124.7(11) . . ?
C19 C18 C17 107.0(10) . . ?
C19 C18 H18 126.5 . . ?
C17 C18 H18 126.5 . . ?
C18 C19 C20 108.5(10) . . ?
C18 C19 H19 125.7 . . ?
C20 C19 H19 125.7 . . ?
C1 C20 N4 123.8(10) . . ?
C1 C20 C19 126.1(10) . . ?
N4 C20 C19 110.0(9) . . ?
C22 C21 C26 119.7(10) . . ?
C22 C21 C6 122.9(10) . . ?
C26 C21 C6 117.3(10) . . ?
F1 C22 C21 120.2(10) . . ?
F1 C22 C23 116.7(10) . . ?
C21 C22 C23 123.1(10) . . ?
F2 C23 C24 121.2(11) . . ?
F2 C23 C22 120.3(10) . . ?
C24 C23 C22 118.5(10) . . ?
F3 C24 C25 120.6(11) . . ?
F3 C24 C23 118.8(11) . . ?
C25 C24 C23 120.6(11) . . ?
C24 C25 F4 120.7(10) . . ?
C24 C25 C26 121.0(10) . . ?
F4 C25 C26 118.2(10) . . ?
F5 C26 C21 126.6(11) . . ?
F5 C26 C25 115.7(9) . . ?
C21 C26 C25 116.6(10) . . ?
C28 C27 C32 114.0(10) . . ?
C28 C27 C11 124.0(10) . . ?
C32 C27 C11 122.0(10) . . ?
C29 C28 F6 120.6(11) . . ?
C29 C28 C27 123.0(11) . . ?
F6 C28 C27 116.4(11) . . ?
C28 C29 F7 120.1(12) . . ?
C28 C29 C30 120.5(11) . . ?
F7 C29 C30 119.2(10) . . ?
C31 C30 F8 121.6(11) . . ?
C31 C30 C29 118.9(11) . . ?
F8 C30 C29 119.5(10) . . ?
C30 C31 C32 120.9(12) . . ?
C30 C31 F9 119.4(11) . . ?
C32 C31 F9 119.7(11) . . ?
C31 C32 F10 119.7(11) . . ?
C31 C32 C27 122.6(11) . . ?
F10 C32 C27 117.7(10) . . ?
C38 C33 C34 116.8(11) . . ?
C38 C33 C16 124.3(10) . . ?
C34 C33 C16 118.9(9) . . ?
F11 C34 C35 118.8(10) . . ?
F11 C34 C33 120.8(10) . . ?
C35 C34 C33 120.3(10) . . ?
F12 C35 C36 120.2(11) . . ?
F12 C35 C34 118.8(10) . . ?
C36 C35 C34 121.0(10) . . ?
F13 C36 C37 119.1(10) . . ?
F13 C36 C35 120.9(11) . . ?
C37 C36 C35 120.0(10) . . ?
F14 C37 C36 121.7(10) . . ?
F14 C37 C38 118.8(10) . . ?
C36 C37 C38 119.5(10) . . ?
F15 C38 C33 119.8(10) . . ?
F15 C38 C37 117.8(10) . . ?
C33 C38 C37 122.3(11) . . ?
O2 C39 O3 121.6(13) . . ?
O2 C39 C40 123.2(12) . . ?
O3 C39 C40 115.2(11) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C42 C41 O3 107.1(11) . . ?
C42 C41 H41A 110.3 . . ?
O3 C41 H41A 110.3 . . ?
C42 C41 H41B 110.3 . . ?
O3 C41 H41B 110.3 . . ?
H41A C41 H41B 108.5 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C1 O1 H1 109.5 . . ?
C39 O3 C41 118.1(10) . . ?
C5 N1 C2 103.2(8) . . ?
C5 N1 Ni1 129.7(8) . . ?
C2 N1 Ni1 127.1(7) . . ?
C7 N2 C10 103.0(9) . . ?
C7 N2 Ni1 129.2(8) . . ?
C10 N2 Ni1 127.8(7) . . ?
C12 N3 C15 104.4(9) . . ?
C12 N3 Ni1 128.9(8) . . ?
C15 N3 Ni1 126.5(8) . . ?
C17 N4 C20 103.2(9) . . ?
C17 N4 Ni1 127.8(8) . . ?
C20 N4 Ni1 129.0(7) . . ?
N1 Ni1 N2 88.8(4) . . ?
N1 Ni1 N3 177.5(4) . . ?
N2 Ni1 N3 89.8(4) . . ?
N1 Ni1 N4 90.2(4) . . ?
N2 Ni1 N4 178.7(4) . . ?
N3 Ni1 N4 91.1(4) . . ?
C44 C43 H43A 109.5 . . ?
C44 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C44 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C43 C44 C45 122.89(13) . . ?
C43 C44 H44A 106.6 . . ?
C45 C44 H44A 106.6 . . ?
C43 C44 H44B 106.6 . . ?
C45 C44 H44B 106.6 . . ?
H44A C44 H44B 106.6 . . ?
C44 C45 C46 122.87(13) . . ?
C44 C45 C50 23.7(15) . 1_655 ?
C46 C45 C50 144.9(18) . 1_655 ?
C44 C45 H45A 106.6 . . ?
C46 C45 H45A 106.6 . . ?
C50 C45 H45A 87.8 1_655 . ?
C44 C45 H45B 106.6 . . ?
C46 C45 H45B 106.6 . . ?
C50 C45 H45B 99.2 1_655 . ?
H45A C45 H45B 106.6 . . ?
C47 C46 C45 122.89(13) . . ?
C47 C46 H46A 106.6 . . ?
C45 C46 H46A 106.6 . . ?
C47 C46 H46B 106.6 . . ?
C45 C46 H46B 106.6 . . ?
H46A C46 H46B 106.6 . . ?
C46 C47 C48 122.88(13) . . ?
C46 C47 C43 150(2) . 1_455 ?
C48 C47 C43 71.6(14) . 1_455 ?
C46 C47 H47A 106.6 . . ?
C48 C47 H47A 106.6 . . ?
C43 C47 H47A 91.6 1_455 . ?
C46 C47 H47B 106.6 . . ?
C48 C47 H47B 106.6 . . ?
C43 C47 H47B 44.2 1_455 . ?
H47A C47 H47B 106.6 . . ?
C47 C48 C49 102.02(10) . . ?
C47 C48 H48A 111.4 . . ?
C49 C48 H48A 111.4 . . ?
C47 C48 H48B 111.4 . . ?
C49 C48 H48B 111.4 . . ?
H48A C48 H48B 109.2 . . ?
C50 C49 C48 122.88(13) . . ?
C50 C49 H49A 106.6 . . ?
C48 C49 H49A 106.6 . . ?
C50 C49 H49B 106.6 . . ?
C48 C49 H49B 106.6 . . ?
H49A C49 H49B 106.6 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C20 C1 C2 N1 3.4(18) . . . . ?
O1 C1 C2 N1 177.5(10) . . . . ?
C20 C1 C2 C3 -174.1(10) . . . . ?
O1 C1 C2 C3 -0.1(15) . . . . ?
C1 C2 C3 C4 171.7(11) . . . . ?
N1 C2 C3 C4 -6.2(13) . . . . ?
C2 C3 C4 C5 3.7(13) . . . . ?
C3 C4 C5 C6 173.5(11) . . . . ?
C3 C4 C5 N1 -0.2(13) . . . . ?
N1 C5 C6 C7 3.9(17) . . . . ?
C4 C5 C6 C7 -169.0(10) . . . . ?
N1 C5 C6 C21 -178.8(9) . . . . ?
C4 C5 C6 C21 8.3(16) . . . . ?
C5 C6 C7 N2 -1.8(17) . . . . ?
C21 C6 C7 N2 -179.1(10) . . . . ?
C5 C6 C7 C8 169.9(11) . . . . ?
C21 C6 C7 C8 -7.4(16) . . . . ?
N2 C7 C8 C9 -0.6(14) . . . . ?
C6 C7 C8 C9 -173.2(10) . . . . ?
C7 C8 C9 C10 0.6(13) . . . . ?
C8 C9 C10 C11 -178.0(10) . . . . ?
C8 C9 C10 N2 -0.6(13) . . . . ?
N2 C10 C11 C12 -7.6(16) . . . . ?
C9 C10 C11 C12 169.6(11) . . . . ?
N2 C10 C11 C27 175.1(9) . . . . ?
C9 C10 C11 C27 -7.7(16) . . . . ?
C10 C11 C12 N3 3.8(18) . . . . ?
C27 C11 C12 N3 -179.0(10) . . . . ?
C10 C11 C12 C13 -171.1(10) . . . . ?
C27 C11 C12 C13 6.1(16) . . . . ?
N3 C12 C13 C14 -1.9(14) . . . . ?
C11 C12 C13 C14 173.7(10) . . . . ?
C12 C13 C14 C15 3.9(12) . . . . ?
C13 C14 C15 C16 176.5(10) . . . . ?
C13 C14 C15 N3 -4.7(12) . . . . ?
N3 C15 C16 C17 10.8(17) . . . . ?
C14 C15 C16 C17 -170.6(10) . . . . ?
N3 C15 C16 C33 -179.0(9) . . . . ?
C14 C15 C16 C33 -0.4(15) . . . . ?
C15 C16 C17 N4 -7.7(17) . . . . ?
C33 C16 C17 N4 -177.6(10) . . . . ?
C15 C16 C17 C18 170.9(11) . . . . ?
C33 C16 C17 C18 1.0(16) . . . . ?
N4 C17 C18 C19 1.4(13) . . . . ?
C16 C17 C18 C19 -177.4(10) . . . . ?
C17 C18 C19 C20 0.3(12) . . . . ?
O1 C1 C20 N4 179.9(9) . . . . ?
C2 C1 C20 N4 -6.6(17) . . . . ?
O1 C1 C20 C19 -2.7(17) . . . . ?
C2 C1 C20 C19 170.8(11) . . . . ?
C18 C19 C20 C1 -179.5(11) . . . . ?
C18 C19 C20 N4 -1.8(12) . . . . ?
C5 C6 C21 C22 -68.5(15) . . . . ?
C7 C6 C21 C22 108.8(13) . . . . ?
C5 C6 C21 C26 110.5(12) . . . . ?
C7 C6 C21 C26 -72.2(14) . . . . ?
C26 C21 C22 F1 -177.5(10) . . . . ?
C6 C21 C22 F1 1.5(18) . . . . ?
C26 C21 C22 C23 3.1(19) . . . . ?
C6 C21 C22 C23 -177.9(11) . . . . ?
F1 C22 C23 F2 1.8(17) . . . . ?
C21 C22 C23 F2 -178.8(11) . . . . ?
F1 C22 C23 C24 -177.8(11) . . . . ?
C21 C22 C23 C24 1.6(19) . . . . ?
F2 C23 C24 F3 -0.2(19) . . . . ?
C22 C23 C24 F3 179.4(11) . . . . ?
F2 C23 C24 C25 179.7(11) . . . . ?
C22 C23 C24 C25 -1(2) . . . . ?
F3 C24 C25 F4 0(2) . . . . ?
C23 C24 C25 F4 -179.8(12) . . . . ?
F3 C24 C25 C26 175.4(11) . . . . ?
C23 C24 C25 C26 -5(2) . . . . ?
C22 C21 C26 F5 -175.4(11) . . . . ?
C6 C21 C26 F5 5.5(17) . . . . ?
C22 C21 C26 C25 -7.9(16) . . . . ?
C6 C21 C26 C25 173.1(10) . . . . ?
C24 C25 C26 F5 177.7(11) . . . . ?
F4 C25 C26 F5 -6.8(15) . . . . ?
C24 C25 C26 C21 8.8(17) . . . . ?
F4 C25 C26 C21 -175.7(10) . . . . ?
C12 C11 C27 C28 85.7(15) . . . . ?
C10 C11 C27 C28 -97.0(13) . . . . ?
C12 C11 C27 C32 -92.6(13) . . . . ?
C10 C11 C27 C32 84.8(13) . . . . ?
C32 C27 C28 C29 -2.3(19) . . . . ?
C11 C27 C28 C29 179.3(13) . . . . ?
C32 C27 C28 F6 179.1(11) . . . . ?
C11 C27 C28 F6 0.7(18) . . . . ?
F6 C28 C29 F7 -2(2) . . . . ?
C27 C28 C29 F7 179.1(12) . . . . ?
F6 C28 C29 C30 -177.3(13) . . . . ?
C27 C28 C29 C30 4(2) . . . . ?
C28 C29 C30 C31 -4(2) . . . . ?
F7 C29 C30 C31 -179.1(13) . . . . ?
C28 C29 C30 F8 178.5(13) . . . . ?
F7 C29 C30 F8 4(2) . . . . ?
F8 C30 C31 C32 179.8(12) . . . . ?
C29 C30 C31 C32 3(2) . . . . ?
F8 C30 C31 F9 -1(2) . . . . ?
C29 C30 C31 F9 -178.2(12) . . . . ?
C30 C31 C32 F10 178.3(12) . . . . ?
F9 C31 C32 F10 -1.0(19) . . . . ?
C30 C31 C32 C27 -1(2) . . . . ?
F9 C31 C32 C27 179.9(10) . . . . ?
C28 C27 C32 C31 0.6(18) . . . . ?
C11 C27 C32 C31 179.0(12) . . . . ?
C28 C27 C32 F10 -178.5(11) . . . . ?
C11 C27 C32 F10 -0.1(16) . . . . ?
C15 C16 C33 C38 -104.9(13) . . . . ?
C17 C16 C33 C38 65.8(15) . . . . ?
C15 C16 C33 C34 75.9(13) . . . . ?
C17 C16 C33 C34 -113.4(12) . . . . ?
C38 C33 C34 F11 179.9(10) . . . . ?
C16 C33 C34 F11 -0.8(16) . . . . ?
C38 C33 C34 C35 -1.7(16) . . . . ?
C16 C33 C34 C35 177.5(10) . . . . ?
F11 C34 C35 F12 -0.2(16) . . . . ?
C33 C34 C35 F12 -178.6(10) . . . . ?
F11 C34 C35 C36 -178.7(10) . . . . ?
C33 C34 C35 C36 2.9(18) . . . . ?
F12 C35 C36 F13 1.7(17) . . . . ?
C34 C35 C36 F13 -179.9(10) . . . . ?
F12 C35 C36 C37 -179.9(10) . . . . ?
C34 C35 C36 C37 -1.4(18) . . . . ?
F13 C36 C37 F14 -1.7(17) . . . . ?
C35 C36 C37 F14 179.8(10) . . . . ?
F13 C36 C37 C38 177.3(10) . . . . ?
C35 C36 C37 C38 -1.2(18) . . . . ?
C34 C33 C38 F15 -176.4(10) . . . . ?
C16 C33 C38 F15 4.4(17) . . . . ?
C34 C33 C38 C37 -0.8(17) . . . . ?
C16 C33 C38 C37 179.9(11) . . . . ?
F14 C37 C38 F15 -3.0(16) . . . . ?
C36 C37 C38 F15 177.9(10) . . . . ?
F14 C37 C38 C33 -178.6(10) . . . . ?
C36 C37 C38 C33 2.3(18) . . . . ?
O2 C39 O3 C41 -1.4(16) . . . . ?
C40 C39 O3 C41 180.0(10) . . . . ?
C42 C41 O3 C39 -175.9(10) . . . . ?
C6 C5 N1 C2 -177.1(10) . . . . ?
C4 C5 N1 C2 -3.4(11) . . . . ?
C6 C5 N1 Ni1 4.7(16) . . . . ?
C4 C5 N1 Ni1 178.4(7) . . . . ?
C1 C2 N1 C5 -171.9(11) . . . . ?
C3 C2 N1 C5 5.8(12) . . . . ?
C1 C2 N1 Ni1 6.3(16) . . . . ?
C3 C2 N1 Ni1 -175.9(7) . . . . ?
C6 C7 N2 C10 172.7(10) . . . . ?
C8 C7 N2 C10 0.2(12) . . . . ?
C6 C7 N2 Ni1 -8.8(16) . . . . ?
C8 C7 N2 Ni1 178.7(7) . . . . ?
C11 C10 N2 C7 177.7(10) . . . . ?
C9 C10 N2 C7 0.2(12) . . . . ?
C11 C10 N2 Ni1 -0.8(15) . . . . ?
C9 C10 N2 Ni1 -178.3(7) . . . . ?
C11 C12 N3 C15 -176.6(10) . . . . ?
C13 C12 N3 C15 -1.2(12) . . . . ?
C11 C12 N3 Ni1 8.5(17) . . . . ?
C13 C12 N3 Ni1 -176.1(7) . . . . ?
C16 C15 N3 C12 -177.7(10) . . . . ?
C14 C15 N3 C12 3.5(11) . . . . ?
C16 C15 N3 Ni1 -2.6(15) . . . . ?
C14 C15 N3 Ni1 178.6(7) . . . . ?
C16 C17 N4 C20 176.4(10) . . . . ?
C18 C17 N4 C20 -2.4(11) . . . . ?
C16 C17 N4 Ni1 -3.4(15) . . . . ?
C18 C17 N4 Ni1 177.8(7) . . . . ?
C1 C20 N4 C17 -179.7(10) . . . . ?
C19 C20 N4 C17 2.5(11) . . . . ?
C1 C20 N4 Ni1 0.0(15) . . . . ?
C19 C20 N4 Ni1 -177.7(7) . . . . ?
C5 N1 Ni1 N2 -10.4(9) . . . . ?
C2 N1 Ni1 N2 171.8(9) . . . . ?
C5 N1 Ni1 N4 168.7(9) . . . . ?
C2 N1 Ni1 N4 -9.1(9) . . . . ?
C43 C44 C45 C46 157(4) . . . . ?
C43 C44 C45 C50 -5(4) . . . 1_655 ?
C44 C45 C46 C47 162(2) . . . . ?
C50 C45 C46 C47 174(3) 1_655 . . . ?
C45 C46 C47 C48 87(2) . . . . ?
C45 C46 C47 C43 -161(4) . . . 1_455 ?
C46 C47 C48 C49 150(3) . . . . ?
C43 C47 C48 C49 -1(3) 1_455 . . . ?
C47 C48 C49 C50 0(5) . . . . ?

_refine_diff_density_max         1.568
_refine_diff_density_min         -1.112
_refine_diff_density_rms         0.197

_shelxl_version_number           2013-2

####################################################################### 
# 
# 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_70106m_a
_database_code_depnum_ccdc_archive 'CCDC 1536339'
_audit_update_record             
;
2017-03-07 deposited with the CCDC.
2017-05-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H8 F15 N4 Ni O, C16 H36 N, C H2 Cl2 '
_chemical_formula_sum            'C55 H46 Cl2 F15 N5 Ni O'
_chemical_formula_weight         1207.58

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   22.0408(14)
_cell_length_b                   16.8646(12)
_cell_length_c                   27.985(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10402.3(12)
_cell_formula_units_Z            8
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    9278
_cell_measurement_theta_min      25.20
_cell_measurement_theta_max      68.25

_exptl_crystal_description       Prism
_exptl_crystal_colour            Green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_F_000             4928
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    2.373
_shelx_estimated_absorpt_T_min   0.536
_shelx_estimated_absorpt_T_max   0.977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.611
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     1.54187
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 5.8140
_diffrn_reflns_number            62909
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         6.750
_diffrn_reflns_theta_max         68.308
_diffrn_reflns_theta_full        67.687
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             9440
_reflns_number_gt                8178
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0817P)²+16.1556P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9440
_refine_ls_number_parameters     728
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0504
_refine_ls_wR_factor_ref         0.1497
_refine_ls_wR_factor_gt          0.1414
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.76764(11) 0.39863(14) 0.22320(9) 0.0198(5) Uani 1 1 d . . . . .
C2 C 0.82318(11) 0.41056(15) 0.19958(9) 0.0219(5) Uani 1 1 d . . . . .
H1 H 0.8625 0.4088 0.2135 0.026 Uiso 1 1 calc R U . . .
C3 C 0.80988(11) 0.42521(15) 0.15275(9) 0.0220(5) Uani 1 1 d . . . . .
H2 H 0.8380 0.4364 0.1279 0.026 Uiso 1 1 calc R U . . .
C4 C 0.74583(11) 0.42055(14) 0.14838(8) 0.0198(5) Uani 1 1 d . . . . .
N1 N 0.71939(9) 0.40705(12) 0.19249(7) 0.0180(4) Uani 1 1 d . . . . .
C5 C 0.71393(11) 0.41619(15) 0.10488(8) 0.0210(5) Uani 1 1 d . . . . .
C6 C 0.65300(12) 0.40250(15) 0.10207(8) 0.0210(5) Uani 1 1 d . . . . .
C7 C 0.62003(12) 0.38351(16) 0.05930(9) 0.0246(5) Uani 1 1 d . . . . .
H3 H 0.6366 0.3779 0.0282 0.030 Uiso 1 1 calc R U . . .
C8 C 0.56150(12) 0.37511(16) 0.07140(9) 0.0242(5) Uani 1 1 d . . . . .
H4 H 0.5292 0.3604 0.0507 0.029 Uiso 1 1 calc R U . . .
C9 C 0.55680(11) 0.39266(14) 0.12186(8) 0.0204(5) Uani 1 1 d . . . . .
N2 N 0.61355(9) 0.40510(12) 0.14095(7) 0.0186(4) Uani 1 1 d . . . . .
C10 C 0.50297(11) 0.40612(15) 0.14582(9) 0.0209(5) Uani 1 1 d . . . . .
C11 C 0.50158(11) 0.43398(15) 0.19249(9) 0.0200(5) Uani 1 1 d . . . . .
C12 C 0.44822(11) 0.46429(16) 0.21593(9) 0.0239(5) Uani 1 1 d . . . . .
H5 H 0.4087 0.4684 0.2026 0.029 Uiso 1 1 calc R U . . .
C13 C 0.46496(11) 0.48561(16) 0.26034(9) 0.0239(5) Uani 1 1 d . . . . .
H6 H 0.4399 0.5099 0.2838 0.029 Uiso 1 1 calc R U . . .
C14 C 0.52779(11) 0.46480(15) 0.26575(8) 0.0209(5) Uani 1 1 d . . . . .
N3 N 0.55066(9) 0.43671(12) 0.22256(7) 0.0187(4) Uani 1 1 d . . . . .
C15 C 0.55773(11) 0.45989(16) 0.30837(9) 0.0238(5) Uani 1 1 d . . . . .
C16 C 0.61579(12) 0.42680(16) 0.31311(9) 0.0245(5) Uani 1 1 d . . . . .
C17 C 0.64400(13) 0.40635(19) 0.35682(9) 0.0314(6) Uani 1 1 d . . . . .
H7 H 0.6273 0.4122 0.3879 0.038 Uiso 1 1 calc R U . . .
C18 C 0.69985(12) 0.37658(19) 0.34580(9) 0.0311(6) Uani 1 1 d . . . . .
H8 H 0.7289 0.3563 0.3677 0.037 Uiso 1 1 calc R U . . .
C19 C 0.70627(12) 0.38160(16) 0.29571(9) 0.0232(5) Uani 1 1 d . . . . .
N4 N 0.65384(9) 0.41056(12) 0.27506(7) 0.0204(4) Uani 1 1 d . . . . .
C20 C 0.76389(11) 0.37393(14) 0.27243(8) 0.0211(5) Uani 1 1 d . . . . .
Ni1 Ni 0.63416(2) 0.41396(2) 0.20771(2) 0.01660(13) Uani 1 1 d . . . . .
C21 C 0.75096(12) 0.41956(17) 0.06009(8) 0.0251(5) Uani 1 1 d . . . . .
C22 C 0.76475(12) 0.49030(18) 0.03770(10) 0.0313(6) Uani 1 1 d . . . . .
C23 C 0.80181(13) 0.4934(2) -0.00247(11) 0.0406(7) Uani 1 1 d . . . . .
C24 C 0.82523(13) 0.4250(2) -0.02087(10) 0.0405(8) Uani 1 1 d . . . . .
C25 C 0.81372(14) 0.3538(2) 0.00094(10) 0.0391(7) Uani 1 1 d . . . . .
C26 C 0.77664(13) 0.35133(19) 0.04088(9) 0.0318(6) Uani 1 1 d . . . . .
F1 F 0.74246(9) 0.55823(11) 0.05494(7) 0.0443(4) Uani 1 1 d . . . . .
F2 F 0.81600(10) 0.56300(14) -0.02221(8) 0.0625(6) Uani 1 1 d . . . . .
F3 F 0.86110(9) 0.42779(16) -0.05930(7) 0.0609(6) Uani 1 1 d . . . . .
F4 F 0.84002(10) 0.28728(14) -0.01516(7) 0.0590(6) Uani 1 1 d . . . . .
F5 F 0.76700(9) 0.28118(11) 0.06149(7) 0.0449(4) Uani 1 1 d . . . . .
C27 C 0.44417(11) 0.39441(16) 0.12031(8) 0.0221(5) Uani 1 1 d . . . . .
C28 C 0.42068(12) 0.44963(17) 0.08833(10) 0.0294(6) Uani 1 1 d . . . . .
C29 C 0.36631(13) 0.43759(19) 0.06483(10) 0.0322(6) Uani 1 1 d . . . . .
C30 C 0.33407(12) 0.36918(19) 0.07274(9) 0.0317(6) Uani 1 1 d . . . . .
C31 C 0.35532(12) 0.31392(18) 0.10463(9) 0.0292(6) Uani 1 1 d . . . . .
C32 C 0.40946(12) 0.32699(16) 0.12789(9) 0.0258(5) Uani 1 1 d . . . . .
F6 F 0.45126(8) 0.51664(11) 0.07928(7) 0.0451(5) Uani 1 1 d . . . . .
F7 F 0.34576(9) 0.49118(13) 0.03338(7) 0.0517(5) Uani 1 1 d . . . . .
F8 F 0.28202(7) 0.35676(13) 0.04935(6) 0.0433(4) Uani 1 1 d . . . . .
F9 F 0.32336(8) 0.24785(11) 0.11291(6) 0.0401(4) Uani 1 1 d . . . . .
F10 F 0.42888(8) 0.27237(10) 0.15884(6) 0.0354(4) Uani 1 1 d . . . . .
C33 C 0.52666(11) 0.48526(18) 0.35335(9) 0.0285(6) Uani 1 1 d . . . . .
C34 C 0.48755(14) 0.4361(2) 0.37812(11) 0.0417(8) Uani 1 1 d . . . . .
C35 C 0.46166(14) 0.4582(3) 0.42097(11) 0.0500(9) Uani 1 1 d . . . . .
C36 C 0.47310(14) 0.5315(3) 0.43959(10) 0.0469(9) Uani 1 1 d . . . . .
C37 C 0.51078(15) 0.5831(2) 0.41577(11) 0.0426(8) Uani 1 1 d . . . . .
C38 C 0.53750(13) 0.55905(19) 0.37319(9) 0.0324(6) Uani 1 1 d . . . . .
F11 F 0.47460(10) 0.36408(15) 0.36124(7) 0.0621(6) Uani 1 1 d . . . . .
F12 F 0.42481(11) 0.40817(19) 0.44429(8) 0.0763(8) Uani 1 1 d . . . . .
F13 F 0.44780(9) 0.55326(17) 0.48106(7) 0.0663(7) Uani 1 1 d . . . . .
F14 F 0.52222(11) 0.65502(13) 0.43359(7) 0.0615(6) Uani 1 1 d . . . . .
F15 F 0.57541(10) 0.60895(11) 0.35150(6) 0.0440(4) Uani 1 1 d . . . . .
O1 O 0.80988(8) 0.35068(12) 0.29415(6) 0.0275(4) Uani 1 1 d . . . . .
N5 N 0.33369(10) 0.16097(12) 0.29881(8) 0.0247(5) Uani 1 1 d . . . . .
C39 C 0.38081(12) 0.22170(16) 0.28325(9) 0.0262(5) Uani 1 1 d . . . . .
H9 H 0.3633 0.2543 0.2573 0.031 Uiso 1 1 calc R U . . .
H10 H 0.3893 0.2575 0.3105 0.031 Uiso 1 1 calc R U . . .
C40 C 0.44049(13) 0.18691(17) 0.26597(10) 0.0311(6) Uani 1 1 d . . . . .
H11 H 0.4347 0.1626 0.2341 0.037 Uiso 1 1 calc R U . . .
H12 H 0.4539 0.1449 0.2883 0.037 Uiso 1 1 calc R U . . .
C41 C 0.48900(13) 0.25125(18) 0.26289(11) 0.0353(6) Uani 1 1 d . . . . .
H13 H 0.4733 0.2959 0.2436 0.042 Uiso 1 1 calc R U . . .
H14 H 0.4976 0.2715 0.2954 0.042 Uiso 1 1 calc R U . . .
C42 C 0.54721(17) 0.2217(2) 0.24090(18) 0.0611(11) Uani 1 1 d . . . . .
H33 H 0.5768 0.2650 0.2397 0.092 Uiso 1 1 calc R U . . .
H34 H 0.5635 0.1782 0.2603 0.092 Uiso 1 1 calc R U . . .
H35 H 0.5392 0.2026 0.2084 0.092 Uiso 1 1 calc R U . . .
C43 C 0.31676(13) 0.10751(16) 0.25701(10) 0.0287(6) Uani 1 1 d . . . . .
H15 H 0.2858 0.0691 0.2680 0.034 Uiso 1 1 calc R U . . .
H16 H 0.3531 0.0769 0.2475 0.034 Uiso 1 1 calc R U . . .
C44 C 0.29232(18) 0.1503(2) 0.21309(12) 0.0465(8) Uani 1 1 d . . . . .
H17 H 0.3252 0.1819 0.1983 0.056 Uiso 1 1 calc R U . . .
H18 H 0.2597 0.1872 0.2228 0.056 Uiso 1 1 calc R U . . .
C45 C 0.26739(15) 0.0912(2) 0.17643(12) 0.0418(7) Uani 1 1 d . . . . .
H19 H 0.2685 0.1157 0.1443 0.050 Uiso 1 1 calc R U . . .
H20 H 0.2937 0.0437 0.1758 0.050 Uiso 1 1 calc R U . . .
C46 C 0.20441(19) 0.0668(3) 0.18744(16) 0.0616(10) Uani 1 1 d . . . . .
H36 H 0.1903 0.0292 0.1632 0.092 Uiso 1 1 calc R U . . .
H37 H 0.2032 0.0416 0.2190 0.092 Uiso 1 1 calc R U . . .
H38 H 0.1780 0.1136 0.1875 0.092 Uiso 1 1 calc R U . . .
C47 C 0.27868(12) 0.20651(16) 0.31654(10) 0.0276(6) Uani 1 1 d . . . . .
H21 H 0.2629 0.2392 0.2899 0.033 Uiso 1 1 calc R U . . .
H22 H 0.2919 0.2432 0.3421 0.033 Uiso 1 1 calc R U . . .
C48 C 0.22718(14) 0.15584(18) 0.33574(13) 0.0387(7) Uani 1 1 d . . . . .
H23 H 0.2145 0.1172 0.3110 0.046 Uiso 1 1 calc R U . . .
H24 H 0.2414 0.1258 0.3640 0.046 Uiso 1 1 calc R U . . .
C49 C 0.17370(13) 0.20708(18) 0.34960(12) 0.0356(6) Uani 1 1 d . . . . .
H25 H 0.1572 0.2327 0.3206 0.043 Uiso 1 1 calc R U . . .
H26 H 0.1878 0.2495 0.3714 0.043 Uiso 1 1 calc R U . . .
C50 C 0.12348(15) 0.1605(2) 0.37393(14) 0.0485(8) Uani 1 1 d . . . . .
H39 H 0.0901 0.1963 0.3821 0.073 Uiso 1 1 calc R U . . .
H40 H 0.1087 0.1191 0.3523 0.073 Uiso 1 1 calc R U . . .
H41 H 0.1393 0.1359 0.4031 0.073 Uiso 1 1 calc R U . . .
C51 C 0.35857(12) 0.10839(15) 0.33832(9) 0.0252(5) Uani 1 1 d . . . . .
H27 H 0.3262 0.0714 0.3485 0.030 Uiso 1 1 calc R U . . .
H28 H 0.3921 0.0761 0.3250 0.030 Uiso 1 1 calc R U . . .
C52 C 0.38187(14) 0.15175(17) 0.38201(10) 0.0317(6) Uani 1 1 d . . . . .
H29 H 0.3479 0.1800 0.3978 0.038 Uiso 1 1 calc R U . . .
H30 H 0.4124 0.1916 0.3722 0.038 Uiso 1 1 calc R U . . .
C53 C 0.41027(13) 0.09370(18) 0.41693(10) 0.0333(6) Uani 1 1 d . . . . .
H31 H 0.3790 0.0552 0.4273 0.040 Uiso 1 1 calc R U . . .
H32 H 0.4426 0.0637 0.4003 0.040 Uiso 1 1 calc R U . . .
C54 C 0.43704(17) 0.1334(2) 0.46066(11) 0.0461(8) Uani 1 1 d . . . . .
H42 H 0.4546 0.0930 0.4817 0.069 Uiso 1 1 calc R U . . .
H43 H 0.4688 0.1707 0.4508 0.069 Uiso 1 1 calc R U . . .
H44 H 0.4051 0.1621 0.4778 0.069 Uiso 1 1 calc R U . . .
Cl1 Cl 0.07488(7) 0.28278(8) 0.03994(5) 0.0737(4) Uani 0.848(2) 1 d D . P A 1
Cl2 Cl 0.18029(8) 0.18842(15) 0.06765(6) 0.1065(7) Uani 0.848(2) 1 d D . P A 1
C55 C 0.1068(2) 0.2192(4) 0.0819(2) 0.0761(15) Uani 0.848(2) 1 d D . P A 1
H45 H 0.0805 0.1718 0.0850 0.091 Uiso 0.848(2) 1 calc R U P A 1
H46 H 0.1076 0.2463 0.1132 0.091 Uiso 0.848(2) 1 calc R U P A 1
Cl1A Cl 0.1579(4) 0.2439(5) 0.0472(3) 0.0737(4) Uani 0.152(2) 1 d D . P A 2
Cl2A Cl 0.0645(3) 0.2067(5) 0.1288(2) 0.065(2) Uani 0.152(2) 1 d D . P A 2
C55A C 0.1373(10) 0.206(2) 0.1034(8) 0.0761(15) Uani 0.152(2) 1 d D . P A 2
H47 H 0.1502 0.1500 0.1033 0.091 Uiso 0.152(2) 1 calc R U P A 2
H48 H 0.1638 0.2335 0.1267 0.091 Uiso 0.152(2) 1 calc R U P 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
C1 N1 1.375(3) . ?
C1 C2 1.406(3) . ?
C1 C20 1.442(3) . ?
C2 C3 1.365(4) . ?
C2 H1 0.9500 . ?
C3 C4 1.419(4) . ?
C3 H2 0.9500 . ?
C4 N1 1.384(3) . ?
C4 C5 1.408(3) . ?
N1 Ni1 1.930(2) . ?
C5 C6 1.365(4) . ?
C5 C21 1.497(3) . ?
C6 N2 1.394(3) . ?
C6 C7 1.436(3) . ?
C7 C8 1.341(4) . ?
C7 H3 0.9500 . ?
C8 C9 1.447(3) . ?
C8 H4 0.9500 . ?
C9 N2 1.376(3) . ?
C9 C10 1.382(4) . ?
N2 Ni1 1.928(2) . ?
C10 C11 1.388(3) . ?
C10 C27 1.493(3) . ?
C11 N3 1.371(3) . ?
C11 C12 1.440(3) . ?
C12 C13 1.346(4) . ?
C12 H5 0.9500 . ?
C13 C14 1.436(3) . ?
C13 H6 0.9500 . ?
C14 C15 1.366(4) . ?
C14 N3 1.393(3) . ?
N3 Ni1 1.926(2) . ?
C15 C16 1.402(4) . ?
C15 C33 1.496(3) . ?
C16 N4 1.383(3) . ?
C16 C17 1.415(4) . ?
C17 C18 1.365(4) . ?
C17 H7 0.9500 . ?
C18 C19 1.412(4) . ?
C18 H8 0.9500 . ?
C19 N4 1.381(3) . ?
C19 C20 1.433(4) . ?
N4 Ni1 1.935(2) . ?
C20 O1 1.245(3) . ?
C21 C22 1.381(4) . ?
C21 C26 1.390(4) . ?
C22 F1 1.337(4) . ?
C22 C23 1.391(4) . ?
C23 F2 1.335(4) . ?
C23 C24 1.364(5) . ?
C24 F3 1.336(3) . ?
C24 C25 1.370(5) . ?
C25 F4 1.341(4) . ?
C25 C26 1.385(4) . ?
C26 F5 1.333(4) . ?
C27 C32 1.387(4) . ?
C27 C28 1.391(4) . ?
C28 F6 1.340(3) . ?
C28 C29 1.382(4) . ?
C29 F7 1.340(3) . ?
C29 C30 1.373(4) . ?
C30 F8 1.337(3) . ?
C30 C31 1.373(4) . ?
C31 F9 1.338(3) . ?
C31 C32 1.377(4) . ?
C32 F10 1.335(3) . ?
C33 C34 1.383(4) . ?
C33 C38 1.383(4) . ?
C34 F11 1.334(4) . ?
C34 C35 1.379(4) . ?
C35 F12 1.341(4) . ?
C35 C36 1.365(6) . ?
C36 F13 1.339(3) . ?
C36 C37 1.375(6) . ?
C37 F14 1.336(4) . ?
C37 C38 1.390(4) . ?
C38 F15 1.332(4) . ?
N5 C47 1.519(3) . ?
N5 C51 1.520(3) . ?
N5 C39 1.522(3) . ?
N5 C43 1.523(3) . ?
C39 C40 1.519(4) . ?
C39 H9 0.9900 . ?
C39 H10 0.9900 . ?
C40 C41 1.526(4) . ?
C40 H11 0.9900 . ?
C40 H12 0.9900 . ?
C41 C42 1.508(5) . ?
C41 H13 0.9900 . ?
C41 H14 0.9900 . ?
C42 H33 0.9800 . ?
C42 H34 0.9800 . ?
C42 H35 0.9800 . ?
C43 C44 1.524(4) . ?
C43 H15 0.9900 . ?
C43 H16 0.9900 . ?
C44 C45 1.532(5) . ?
C44 H17 0.9900 . ?
C44 H18 0.9900 . ?
C45 C46 1.480(5) . ?
C45 H19 0.9900 . ?
C45 H20 0.9900 . ?
C46 H36 0.9800 . ?
C46 H37 0.9800 . ?
C46 H38 0.9800 . ?
C47 C48 1.519(4) . ?
C47 H21 0.9900 . ?
C47 H22 0.9900 . ?
C48 C49 1.512(4) . ?
C48 H23 0.9900 . ?
C48 H24 0.9900 . ?
C49 C50 1.519(4) . ?
C49 H25 0.9900 . ?
C49 H26 0.9900 . ?
C50 H39 0.9800 . ?
C50 H40 0.9800 . ?
C50 H41 0.9800 . ?
C51 C52 1.515(4) . ?
C51 H27 0.9900 . ?
C51 H28 0.9900 . ?
C52 C53 1.518(4) . ?
C52 H29 0.9900 . ?
C52 H30 0.9900 . ?
C53 C54 1.514(4) . ?
C53 H31 0.9900 . ?
C53 H32 0.9900 . ?
C54 H42 0.9800 . ?
C54 H43 0.9800 . ?
C54 H44 0.9800 . ?
Cl1 C55 1.738(6) . ?
Cl2 C55 1.748(6) . ?
C55 H45 0.9900 . ?
C55 H46 0.9900 . ?
Cl1A C55A 1.756(15) . ?
Cl2A C55A 1.754(15) . ?
C55A H47 0.9900 . ?
C55A H48 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
N1 C1 C2 111.4(2) . . ?
N1 C1 C20 125.7(2) . . ?
C2 C1 C20 122.7(2) . . ?
C3 C2 C1 106.9(2) . . ?
C3 C2 H1 126.6 . . ?
C1 C2 H1 126.6 . . ?
C2 C3 C4 106.6(2) . . ?
C2 C3 H2 126.7 . . ?
C4 C3 H2 126.7 . . ?
N1 C4 C5 123.5(2) . . ?
N1 C4 C3 110.6(2) . . ?
C5 C4 C3 125.0(2) . . ?
C1 N1 C4 104.42(19) . . ?
C1 N1 Ni1 128.42(16) . . ?
C4 N1 Ni1 126.64(16) . . ?
C6 C5 C4 123.4(2) . . ?
C6 C5 C21 119.7(2) . . ?
C4 C5 C21 116.7(2) . . ?
C5 C6 N2 124.3(2) . . ?
C5 C6 C7 125.7(2) . . ?
N2 C6 C7 110.0(2) . . ?
C8 C7 C6 107.4(2) . . ?
C8 C7 H3 126.3 . . ?
C6 C7 H3 126.3 . . ?
C7 C8 C9 107.1(2) . . ?
C7 C8 H4 126.5 . . ?
C9 C8 H4 126.5 . . ?
N2 C9 C10 124.5(2) . . ?
N2 C9 C8 110.2(2) . . ?
C10 C9 C8 124.7(2) . . ?
C9 N2 C6 105.01(19) . . ?
C9 N2 Ni1 127.02(16) . . ?
C6 N2 Ni1 127.73(16) . . ?
C9 C10 C11 122.1(2) . . ?
C9 C10 C27 119.4(2) . . ?
C11 C10 C27 118.4(2) . . ?
N3 C11 C10 124.8(2) . . ?
N3 C11 C12 110.7(2) . . ?
C10 C11 C12 124.5(2) . . ?
C13 C12 C11 106.9(2) . . ?
C13 C12 H5 126.5 . . ?
C11 C12 H5 126.5 . . ?
C12 C13 C14 107.2(2) . . ?
C12 C13 H6 126.4 . . ?
C14 C13 H6 126.4 . . ?
C15 C14 N3 124.2(2) . . ?
C15 C14 C13 124.9(2) . . ?
N3 C14 C13 109.9(2) . . ?
C11 N3 C14 104.99(19) . . ?
C11 N3 Ni1 127.94(16) . . ?
C14 N3 Ni1 126.95(16) . . ?
C14 C15 C16 123.2(2) . . ?
C14 C15 C33 119.8(2) . . ?
C16 C15 C33 116.9(2) . . ?
N4 C16 C15 124.0(2) . . ?
N4 C16 C17 110.5(2) . . ?
C15 C16 C17 125.4(2) . . ?
C18 C17 C16 106.9(2) . . ?
C18 C17 H7 126.5 . . ?
C16 C17 H7 126.5 . . ?
C17 C18 C19 107.0(2) . . ?
C17 C18 H8 126.5 . . ?
C19 C18 H8 126.5 . . ?
N4 C19 C18 110.7(2) . . ?
N4 C19 C20 125.7(2) . . ?
C18 C19 C20 122.3(2) . . ?
C19 N4 C16 104.8(2) . . ?
C19 N4 Ni1 127.27(16) . . ?
C16 N4 Ni1 127.47(17) . . ?
O1 C20 C19 121.9(2) . . ?
O1 C20 C1 120.7(2) . . ?
C19 C20 C1 117.3(2) . . ?
N3 Ni1 N2 89.97(8) . . ?
N3 Ni1 N1 171.97(9) . . ?
N2 Ni1 N1 90.63(8) . . ?
N3 Ni1 N4 90.57(8) . . ?
N2 Ni1 N4 173.81(9) . . ?
N1 Ni1 N4 89.71(9) . . ?
C22 C21 C26 116.7(2) . . ?
C22 C21 C5 122.2(2) . . ?
C26 C21 C5 120.9(2) . . ?
F1 C22 C21 119.7(2) . . ?
F1 C22 C23 118.4(3) . . ?
C21 C22 C23 121.9(3) . . ?
F2 C23 C24 119.9(3) . . ?
F2 C23 C22 120.3(3) . . ?
C24 C23 C22 119.7(3) . . ?
F3 C24 C23 119.9(3) . . ?
F3 C24 C25 119.9(3) . . ?
C23 C24 C25 120.2(3) . . ?
F4 C25 C24 120.2(3) . . ?
F4 C25 C26 120.0(3) . . ?
C24 C25 C26 119.7(3) . . ?
F5 C26 C25 118.0(3) . . ?
F5 C26 C21 120.1(2) . . ?
C25 C26 C21 121.8(3) . . ?
C32 C27 C28 116.2(2) . . ?
C32 C27 C10 121.0(2) . . ?
C28 C27 C10 122.8(2) . . ?
F6 C28 C29 118.0(2) . . ?
F6 C28 C27 119.9(2) . . ?
C29 C28 C27 122.0(3) . . ?
F7 C29 C30 119.8(2) . . ?
F7 C29 C28 120.4(3) . . ?
C30 C29 C28 119.7(3) . . ?
F8 C30 C31 120.3(3) . . ?
F8 C30 C29 119.8(3) . . ?
C31 C30 C29 119.9(2) . . ?
F9 C31 C30 119.9(2) . . ?
F9 C31 C32 120.5(3) . . ?
C30 C31 C32 119.6(3) . . ?
F10 C32 C31 118.3(2) . . ?
F10 C32 C27 119.2(2) . . ?
C31 C32 C27 122.5(2) . . ?
C34 C33 C38 116.5(2) . . ?
C34 C33 C15 122.4(3) . . ?
C38 C33 C15 121.1(3) . . ?
F11 C34 C35 117.7(3) . . ?
F11 C34 C33 120.1(3) . . ?
C35 C34 C33 122.1(3) . . ?
F12 C35 C36 119.7(3) . . ?
F12 C35 C34 120.3(4) . . ?
C36 C35 C34 120.0(3) . . ?
F13 C36 C35 120.2(4) . . ?
F13 C36 C37 119.9(3) . . ?
C35 C36 C37 120.0(3) . . ?
F14 C37 C36 120.5(3) . . ?
F14 C37 C38 120.3(3) . . ?
C36 C37 C38 119.2(3) . . ?
F15 C38 C33 119.6(2) . . ?
F15 C38 C37 118.2(3) . . ?
C33 C38 C37 122.2(3) . . ?
C47 N5 C51 110.21(19) . . ?
C47 N5 C39 107.33(19) . . ?
C51 N5 C39 110.8(2) . . ?
C47 N5 C43 110.8(2) . . ?
C51 N5 C43 107.56(19) . . ?
C39 N5 C43 110.2(2) . . ?
C40 C39 N5 115.0(2) . . ?
C40 C39 H9 108.5 . . ?
N5 C39 H9 108.5 . . ?
C40 C39 H10 108.5 . . ?
N5 C39 H10 108.5 . . ?
H9 C39 H10 107.5 . . ?
C39 C40 C41 110.5(2) . . ?
C39 C40 H11 109.6 . . ?
C41 C40 H11 109.6 . . ?
C39 C40 H12 109.6 . . ?
C41 C40 H12 109.6 . . ?
H11 C40 H12 108.1 . . ?
C42 C41 C40 112.6(3) . . ?
C42 C41 H13 109.1 . . ?
C40 C41 H13 109.1 . . ?
C42 C41 H14 109.1 . . ?
C40 C41 H14 109.1 . . ?
H13 C41 H14 107.8 . . ?
C41 C42 H33 109.5 . . ?
C41 C42 H34 109.5 . . ?
H33 C42 H34 109.5 . . ?
C41 C42 H35 109.5 . . ?
H33 C42 H35 109.5 . . ?
H34 C42 H35 109.5 . . ?
N5 C43 C44 115.2(2) . . ?
N5 C43 H15 108.5 . . ?
C44 C43 H15 108.5 . . ?
N5 C43 H16 108.5 . . ?
C44 C43 H16 108.5 . . ?
H15 C43 H16 107.5 . . ?
C43 C44 C45 111.0(3) . . ?
C43 C44 H17 109.4 . . ?
C45 C44 H17 109.4 . . ?
C43 C44 H18 109.4 . . ?
C45 C44 H18 109.4 . . ?
H17 C44 H18 108.0 . . ?
C46 C45 C44 112.2(3) . . ?
C46 C45 H19 109.2 . . ?
C44 C45 H19 109.2 . . ?
C46 C45 H20 109.2 . . ?
C44 C45 H20 109.2 . . ?
H19 C45 H20 107.9 . . ?
C45 C46 H36 109.5 . . ?
C45 C46 H37 109.5 . . ?
H36 C46 H37 109.5 . . ?
C45 C46 H38 109.5 . . ?
H36 C46 H38 109.5 . . ?
H37 C46 H38 109.5 . . ?
N5 C47 C48 115.3(2) . . ?
N5 C47 H21 108.4 . . ?
C48 C47 H21 108.4 . . ?
N5 C47 H22 108.4 . . ?
C48 C47 H22 108.4 . . ?
H21 C47 H22 107.5 . . ?
C49 C48 C47 110.6(2) . . ?
C49 C48 H23 109.5 . . ?
C47 C48 H23 109.5 . . ?
C49 C48 H24 109.5 . . ?
C47 C48 H24 109.5 . . ?
H23 C48 H24 108.1 . . ?
C48 C49 C50 112.8(3) . . ?
C48 C49 H25 109.0 . . ?
C50 C49 H25 109.0 . . ?
C48 C49 H26 109.0 . . ?
C50 C49 H26 109.0 . . ?
H25 C49 H26 107.8 . . ?
C49 C50 H39 109.5 . . ?
C49 C50 H40 109.5 . . ?
H39 C50 H40 109.5 . . ?
C49 C50 H41 109.5 . . ?
H39 C50 H41 109.5 . . ?
H40 C50 H41 109.5 . . ?
C52 C51 N5 115.3(2) . . ?
C52 C51 H27 108.4 . . ?
N5 C51 H27 108.4 . . ?
C52 C51 H28 108.4 . . ?
N5 C51 H28 108.4 . . ?
H27 C51 H28 107.5 . . ?
C51 C52 C53 110.4(2) . . ?
C51 C52 H29 109.6 . . ?
C53 C52 H29 109.6 . . ?
C51 C52 H30 109.6 . . ?
C53 C52 H30 109.6 . . ?
H29 C52 H30 108.1 . . ?
C54 C53 C52 113.3(3) . . ?
C54 C53 H31 108.9 . . ?
C52 C53 H31 108.9 . . ?
C54 C53 H32 108.9 . . ?
C52 C53 H32 108.9 . . ?
H31 C53 H32 107.7 . . ?
C53 C54 H42 109.5 . . ?
C53 C54 H43 109.5 . . ?
H42 C54 H43 109.5 . . ?
C53 C54 H44 109.5 . . ?
H42 C54 H44 109.5 . . ?
H43 C54 H44 109.5 . . ?
Cl1 C55 Cl2 113.9(4) . . ?
Cl1 C55 H45 108.8 . . ?
Cl2 C55 H45 108.8 . . ?
Cl1 C55 H46 108.8 . . ?
Cl2 C55 H46 108.8 . . ?
H45 C55 H46 107.7 . . ?
Cl2A C55A Cl1A 126.7(16) . . ?
Cl2A C55A H47 105.6 . . ?
Cl1A C55A H47 105.6 . . ?
Cl2A C55A H48 105.6 . . ?
Cl1A C55A H48 105.6 . . ?
H47 C55A H48 106.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 -1.3(3) . . . . ?
C20 C1 C2 C3 173.7(2) . . . . ?
C1 C2 C3 C4 -1.0(3) . . . . ?
C2 C3 C4 N1 3.0(3) . . . . ?
C2 C3 C4 C5 -166.7(2) . . . . ?
C2 C1 N1 C4 3.0(3) . . . . ?
C20 C1 N1 C4 -171.8(2) . . . . ?
C2 C1 N1 Ni1 -169.02(17) . . . . ?
C20 C1 N1 Ni1 16.2(3) . . . . ?
C5 C4 N1 C1 166.2(2) . . . . ?
C3 C4 N1 C1 -3.6(3) . . . . ?
C5 C4 N1 Ni1 -21.6(3) . . . . ?
C3 C4 N1 Ni1 168.59(16) . . . . ?
N1 C4 C5 C6 3.7(4) . . . . ?
C3 C4 C5 C6 172.1(2) . . . . ?
N1 C4 C5 C21 -170.5(2) . . . . ?
C3 C4 C5 C21 -2.2(4) . . . . ?
C4 C5 C6 N2 11.8(4) . . . . ?
C21 C5 C6 N2 -174.1(2) . . . . ?
C4 C5 C6 C7 -168.2(2) . . . . ?
C21 C5 C6 C7 5.9(4) . . . . ?
C5 C6 C7 C8 -179.6(3) . . . . ?
N2 C6 C7 C8 0.4(3) . . . . ?
C6 C7 C8 C9 2.7(3) . . . . ?
C7 C8 C9 N2 -5.1(3) . . . . ?
C7 C8 C9 C10 166.4(3) . . . . ?
C10 C9 N2 C6 -166.3(2) . . . . ?
C8 C9 N2 C6 5.2(3) . . . . ?
C10 C9 N2 Ni1 19.0(3) . . . . ?
C8 C9 N2 Ni1 -169.54(17) . . . . ?
C5 C6 N2 C9 176.5(2) . . . . ?
C7 C6 N2 C9 -3.5(3) . . . . ?
C5 C6 N2 Ni1 -8.8(4) . . . . ?
C7 C6 N2 Ni1 171.17(17) . . . . ?
N2 C9 C10 C11 -0.1(4) . . . . ?
C8 C9 C10 C11 -170.4(2) . . . . ?
N2 C9 C10 C27 176.8(2) . . . . ?
C8 C9 C10 C27 6.5(4) . . . . ?
C9 C10 C11 N3 -13.1(4) . . . . ?
C27 C10 C11 N3 170.0(2) . . . . ?
C9 C10 C11 C12 166.7(2) . . . . ?
C27 C10 C11 C12 -10.2(4) . . . . ?
N3 C11 C12 C13 0.1(3) . . . . ?
C10 C11 C12 C13 -179.7(2) . . . . ?
C11 C12 C13 C14 -3.1(3) . . . . ?
C12 C13 C14 C15 -164.2(3) . . . . ?
C12 C13 C14 N3 5.1(3) . . . . ?
C10 C11 N3 C14 -177.2(2) . . . . ?
C12 C11 N3 C14 3.0(3) . . . . ?
C10 C11 N3 Ni1 6.7(4) . . . . ?
C12 C11 N3 Ni1 -173.11(17) . . . . ?
C15 C14 N3 C11 164.5(2) . . . . ?
C13 C14 N3 C11 -4.9(3) . . . . ?
C15 C14 N3 Ni1 -19.3(4) . . . . ?
C13 C14 N3 Ni1 171.25(17) . . . . ?
N3 C14 C15 C16 1.1(4) . . . . ?
C13 C14 C15 C16 168.9(3) . . . . ?
N3 C14 C15 C33 -174.4(2) . . . . ?
C13 C14 C15 C33 -6.6(4) . . . . ?
C14 C15 C16 N4 13.7(4) . . . . ?
C33 C15 C16 N4 -170.7(2) . . . . ?
C14 C15 C16 C17 -167.2(3) . . . . ?
C33 C15 C16 C17 8.5(4) . . . . ?
N4 C16 C17 C18 -0.5(3) . . . . ?
C15 C16 C17 C18 -179.7(3) . . . . ?
C16 C17 C18 C19 2.0(3) . . . . ?
C17 C18 C19 N4 -3.0(3) . . . . ?
C17 C18 C19 C20 164.5(3) . . . . ?
C18 C19 N4 C16 2.6(3) . . . . ?
C20 C19 N4 C16 -164.4(3) . . . . ?
C18 C19 N4 Ni1 -169.90(19) . . . . ?
C20 C19 N4 Ni1 23.1(4) . . . . ?
C15 C16 N4 C19 178.0(3) . . . . ?
C17 C16 N4 C19 -1.3(3) . . . . ?
C15 C16 N4 Ni1 -9.6(4) . . . . ?
C17 C16 N4 Ni1 171.17(19) . . . . ?
N4 C19 C20 O1 176.6(2) . . . . ?
C18 C19 C20 O1 11.0(4) . . . . ?
N4 C19 C20 C1 0.1(4) . . . . ?
C18 C19 C20 C1 -165.5(3) . . . . ?
N1 C1 C20 O1 163.5(2) . . . . ?
C2 C1 C20 O1 -10.8(4) . . . . ?
N1 C1 C20 C19 -20.0(4) . . . . ?
C2 C1 C20 C19 165.7(2) . . . . ?
C6 C5 C21 C22 95.7(3) . . . . ?
C4 C5 C21 C22 -89.8(3) . . . . ?
C6 C5 C21 C26 -88.8(3) . . . . ?
C4 C5 C21 C26 85.7(3) . . . . ?
C26 C21 C22 F1 -178.7(2) . . . . ?
C5 C21 C22 F1 -3.0(4) . . . . ?
C26 C21 C22 C23 0.8(4) . . . . ?
C5 C21 C22 C23 176.6(3) . . . . ?
F1 C22 C23 F2 2.0(4) . . . . ?
C21 C22 C23 F2 -177.6(3) . . . . ?
F1 C22 C23 C24 180.0(3) . . . . ?
C21 C22 C23 C24 0.4(4) . . . . ?
F2 C23 C24 F3 -1.6(5) . . . . ?
C22 C23 C24 F3 -179.7(3) . . . . ?
F2 C23 C24 C25 176.1(3) . . . . ?
C22 C23 C24 C25 -1.9(5) . . . . ?
F3 C24 C25 F4 2.3(4) . . . . ?
C23 C24 C25 F4 -175.5(3) . . . . ?
F3 C24 C25 C26 179.8(3) . . . . ?
C23 C24 C25 C26 2.0(5) . . . . ?
F4 C25 C26 F5 -1.7(4) . . . . ?
C24 C25 C26 F5 -179.2(3) . . . . ?
F4 C25 C26 C21 176.8(3) . . . . ?
C24 C25 C26 C21 -0.7(4) . . . . ?
C22 C21 C26 F5 177.8(2) . . . . ?
C5 C21 C26 F5 2.0(4) . . . . ?
C22 C21 C26 C25 -0.7(4) . . . . ?
C5 C21 C26 C25 -176.5(3) . . . . ?
C9 C10 C27 C32 102.4(3) . . . . ?
C11 C10 C27 C32 -80.6(3) . . . . ?
C9 C10 C27 C28 -78.2(3) . . . . ?
C11 C10 C27 C28 98.7(3) . . . . ?
C32 C27 C28 F6 179.5(2) . . . . ?
C10 C27 C28 F6 0.2(4) . . . . ?
C32 C27 C28 C29 -1.0(4) . . . . ?
C10 C27 C28 C29 179.6(3) . . . . ?
F6 C28 C29 F7 1.1(4) . . . . ?
C27 C28 C29 F7 -178.4(3) . . . . ?
F6 C28 C29 C30 179.2(3) . . . . ?
C27 C28 C29 C30 -0.3(4) . . . . ?
F7 C29 C30 F8 -0.7(4) . . . . ?
C28 C29 C30 F8 -178.8(3) . . . . ?
F7 C29 C30 C31 179.4(3) . . . . ?
C28 C29 C30 C31 1.3(4) . . . . ?
F8 C30 C31 F9 -1.0(4) . . . . ?
C29 C30 C31 F9 178.9(3) . . . . ?
F8 C30 C31 C32 179.0(2) . . . . ?
C29 C30 C31 C32 -1.1(4) . . . . ?
F9 C31 C32 F10 -0.2(4) . . . . ?
C30 C31 C32 F10 179.7(2) . . . . ?
F9 C31 C32 C27 179.8(2) . . . . ?
C30 C31 C32 C27 -0.3(4) . . . . ?
C28 C27 C32 F10 -178.7(2) . . . . ?
C10 C27 C32 F10 0.6(4) . . . . ?
C28 C27 C32 C31 1.3(4) . . . . ?
C10 C27 C32 C31 -179.4(2) . . . . ?
C14 C15 C33 C34 82.7(4) . . . . ?
C16 C15 C33 C34 -93.1(3) . . . . ?
C14 C15 C33 C38 -99.5(3) . . . . ?
C16 C15 C33 C38 84.7(3) . . . . ?
C38 C33 C34 F11 179.8(3) . . . . ?
C15 C33 C34 F11 -2.4(5) . . . . ?
C38 C33 C34 C35 -1.6(5) . . . . ?
C15 C33 C34 C35 176.3(3) . . . . ?
F11 C34 C35 F12 -0.1(5) . . . . ?
C33 C34 C35 F12 -178.8(3) . . . . ?
F11 C34 C35 C36 -179.5(3) . . . . ?
C33 C34 C35 C36 1.8(5) . . . . ?
F12 C35 C36 F13 0.2(5) . . . . ?
C34 C35 C36 F13 179.7(3) . . . . ?
F12 C35 C36 C37 -179.9(3) . . . . ?
C34 C35 C36 C37 -0.4(5) . . . . ?
F13 C36 C37 F14 -0.2(4) . . . . ?
C35 C36 C37 F14 179.9(3) . . . . ?
F13 C36 C37 C38 178.9(3) . . . . ?
C35 C36 C37 C38 -1.0(5) . . . . ?
C34 C33 C38 F15 179.1(3) . . . . ?
C15 C33 C38 F15 1.2(4) . . . . ?
C34 C33 C38 C37 0.1(4) . . . . ?
C15 C33 C38 C37 -177.8(3) . . . . ?
F14 C37 C38 F15 1.3(4) . . . . ?
C36 C37 C38 F15 -177.8(3) . . . . ?
F14 C37 C38 C33 -179.7(3) . . . . ?
C36 C37 C38 C33 1.2(4) . . . . ?
C47 N5 C39 C40 177.8(2) . . . . ?
C51 N5 C39 C40 57.5(3) . . . . ?
C43 N5 C39 C40 -61.4(3) . . . . ?
N5 C39 C40 C41 -166.3(2) . . . . ?
C39 C40 C41 C42 -173.8(3) . . . . ?
C47 N5 C43 C44 61.1(3) . . . . ?
C51 N5 C43 C44 -178.4(3) . . . . ?
C39 N5 C43 C44 -57.6(3) . . . . ?
N5 C43 C44 C45 -171.0(3) . . . . ?
C43 C44 C45 C46 83.1(4) . . . . ?
C51 N5 C47 C48 -56.9(3) . . . . ?
C39 N5 C47 C48 -177.6(2) . . . . ?
C43 N5 C47 C48 62.1(3) . . . . ?
N5 C47 C48 C49 -176.7(2) . . . . ?
C47 C48 C49 C50 -173.9(3) . . . . ?
C47 N5 C51 C52 -63.0(3) . . . . ?
C39 N5 C51 C52 55.6(3) . . . . ?
C43 N5 C51 C52 176.1(2) . . . . ?
N5 C51 C52 C53 -175.2(2) . . . . ?
C51 C52 C53 C54 177.5(3) . . . . ?

_refine_diff_density_max         1.008
_refine_diff_density_min         -1.434
_refine_diff_density_rms         0.073

