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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_D620
_database_code_depnum_ccdc_archive 'CCDC 1019251'
_audit_update_record             
;
2014-08-13 deposited with the CCDC.
2015-02-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C136 H142 N4 Ni O2'
_chemical_formula_weight         1923.24

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'
O O 0.0106 0.0060 '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'

_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                   12.8361(14)
_cell_length_b                   15.5717(18)
_cell_length_c                   15.9281(17)
_cell_angle_alpha                100.921(4)
_cell_angle_beta                 109.976(4)
_cell_angle_gamma                108.180(4)
_cell_volume                     2682.0(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9830
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      27.56

_exptl_crystal_description       Block
_exptl_crystal_colour            Red
_exptl_crystal_density_meas      'Not Measured'
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_F_000             1030
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    0.237
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7150
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'Sadabs, (Sheldrick 2012)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Microfocusing Source'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            147706
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_av_R_equivalents  0.0918
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.128
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             12338
_reflns_number_gt                9448
_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.bruker_data_scaling   'SADABS V2012/1 (Bruker AXS Inc.)'
_computing.cell_refinement       'APEX2 v2013.6--2 (Bruker AXS)'
_computing.data_collection       'APEX2 (Bruker AXS)'
_computing.data_reduction        'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing.molecular_graphics    'Bruker SHELXTL'
_computing.publication_material  'Bruker SHELXTL'
_computing.structure_refinement  'SHELXL--2013 (Sheldrick 2013)'
_computing.structure_solution    'SHELXS--97 (Sheldrick 2008)'

_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)+(0.0424P)²+2.3179P] 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         12338
_refine_ls_number_parameters     644
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0506
_refine_ls_wR_factor_ref         0.1184
_refine_ls_wR_factor_gt          0.1087
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_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_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
C14S C 0.867(2) 0.2072(12) 1.0006(10) 0.050(2) Uani 0.5 1 d D . P A 1
H14A H 0.8197 0.2390 1.0200 0.075 Uiso 0.5 1 calc R U P A 1
H14B H 0.9287 0.2062 1.0568 0.075 Uiso 0.5 1 calc R U P A 1
H14C H 0.8124 0.1414 0.9585 0.075 Uiso 0.5 1 calc R U P A 1
C8S C 0.9271(5) 0.2607(3) 0.9497(4) 0.0486(5) Uani 0.5 1 d DG . P A 1
C9S C 0.9931(6) 0.2240(2) 0.9118(4) 0.0486(5) Uani 0.5 1 d G . P A 1
H9S H 0.9916 0.1627 0.9122 0.058 Uiso 0.5 1 calc R U P A 1
C10S C 1.0612(5) 0.2769(3) 0.8731(4) 0.0486(5) Uani 0.5 1 d G . P A 1
H10S H 1.1063 0.2517 0.8472 0.058 Uiso 0.5 1 calc R U P A 1
C11S C 1.0634(4) 0.3665(3) 0.8725(3) 0.0607(10) Uani 0.5 1 d G . P A 1
H11S H 1.1099 0.4027 0.8461 0.073 Uiso 0.5 1 calc R U P A 1
C12S C 0.9974(5) 0.4033(2) 0.9104(4) 0.0607(10) Uani 0.5 1 d G . P A 1
H12S H 0.9988 0.4646 0.9099 0.073 Uiso 0.5 1 calc R U P A 1
C13S C 0.9292(4) 0.3504(3) 0.9490(4) 0.0607(10) Uani 0.5 1 d G . P A 1
H13S H 0.8841 0.3755 0.9750 0.073 Uiso 0.5 1 calc R U P A 1
C14X C 0.842(2) 0.1816(11) 0.9854(10) 0.050(2) Uani 0.5 1 d D . P B 2
H14X H 0.7918 0.2058 1.0086 0.075 Uiso 0.5 1 calc R U P B 2
H14Y H 0.9023 0.1737 1.0375 0.075 Uiso 0.5 1 calc R U P B 2
H14Z H 0.7906 0.1197 0.9349 0.075 Uiso 0.5 1 calc R U P B 2
C8X C 0.9058(5) 0.2512(3) 0.9477(4) 0.0486(5) Uani 0.5 1 d DG . P B 2
C9X C 0.9950(5) 0.2413(3) 0.9211(4) 0.0486(5) Uani 0.5 1 d G . P B 2
H9X H 1.0200 0.1910 0.9296 0.058 Uiso 0.5 1 calc R U P B 2
C10X C 1.0476(4) 0.3051(3) 0.8820(4) 0.0486(5) Uani 0.5 1 d G . P B 2
H10X H 1.1086 0.2983 0.8637 0.058 Uiso 0.5 1 calc R U P B 2
C11X C 1.0110(4) 0.3787(3) 0.8695(3) 0.0607(10) Uani 0.5 1 d G . P B 2
H11X H 1.0470 0.4222 0.8428 0.073 Uiso 0.5 1 calc R U P B 2
C12X C 0.9218(4) 0.3886(3) 0.8962(4) 0.0607(10) Uani 0.5 1 d G . P B 2
H12X H 0.8968 0.4389 0.8877 0.073 Uiso 0.5 1 calc R U P B 2
C13X C 0.8692(4) 0.3248(3) 0.9353(4) 0.0607(10) Uani 0.5 1 d G . P B 2
H13X H 0.8083 0.3316 0.9535 0.073 Uiso 0.5 1 calc R U P B 2
Ni1 Ni 0.0000 0.0000 0.0000 0.01042(9) Uani 1 2 d S . P . .
N1 N -0.11833(13) -0.04305(10) 0.05138(10) 0.0122(3) Uani 1 1 d . . . . .
N2 N 0.08797(13) 0.12300(10) 0.10293(10) 0.0125(3) Uani 1 1 d . . . . .
O1 O -0.3675(3) -0.20476(19) 0.0724(2) 0.0292(7) Uani 0.5 1 d . . P C 1
O2 O 0.3340(3) 0.3497(2) 0.2536(2) 0.0300(7) Uani 0.5 1 d . . P D 2
C1 C -0.22046(16) -0.13162(12) 0.01645(13) 0.0139(4) Uani 1 1 d . . . . .
C2 C -0.28075(17) -0.13615(13) 0.07789(13) 0.0165(4) Uani 1 1 d . . . . .
H2 H -0.3496 -0.1884 0.0707 0.020 Uiso 0.5 1 calc R U P C 2
C3 C -0.21501(16) -0.04526(13) 0.15215(13) 0.0154(4) Uani 1 1 d . . . . .
C4 C -0.23173(16) -0.00684(13) 0.22920(13) 0.0156(4) Uani 1 1 d . . . . .
C5 C -0.14851(16) 0.08866(12) 0.29165(13) 0.0140(4) Uani 1 1 d . . . . .
C6 C -0.05100(16) 0.14023(12) 0.27245(12) 0.0127(4) Uani 1 1 d . . . . .
C7 C -0.03659(16) 0.09890(12) 0.19153(12) 0.0125(3) Uani 1 1 d . . . . .
C8 C -0.11838(16) 0.00693(12) 0.13106(12) 0.0126(3) Uani 1 1 d . . . . .
C9 C -0.16044(16) 0.13209(13) 0.37167(13) 0.0148(4) Uani 1 1 d . . . . .
H9 H -0.2263 0.0976 0.3835 0.018 Uiso 1 1 calc R U . . .
C10 C -0.07974(16) 0.22338(13) 0.43405(12) 0.0142(4) Uani 1 1 d . . . . .
C11 C 0.01532(16) 0.27319(13) 0.41444(13) 0.0154(4) Uani 1 1 d . . . . .
H11 H 0.0707 0.3362 0.4559 0.019 Uiso 1 1 calc R U . . .
C12 C 0.03217(16) 0.23406(12) 0.33647(12) 0.0141(4) Uani 1 1 d . . . . .
C13 C 0.13396(16) 0.28645(13) 0.32044(13) 0.0159(4) Uani 1 1 d . . . . .
C14 C 0.14603(16) 0.24361(12) 0.24254(13) 0.0153(4) Uani 1 1 d . . . . .
C15 C 0.06075(16) 0.15084(12) 0.17564(12) 0.0128(4) Uani 1 1 d . . . . .
C16 C 0.23569(17) 0.27568(13) 0.20825(13) 0.0166(4) Uani 1 1 d . . . . .
H16 H 0.3061 0.3342 0.2366 0.020 Uiso 0.5 1 calc R U P D 1
C17 C 0.19684(16) 0.20091(12) 0.12219(13) 0.0139(4) Uani 1 1 d . . . . .
C18 C -0.33417(17) -0.06274(12) 0.24845(13) 0.0174(4) Uani 1 1 d . . . . .
C19 C -0.31052(19) -0.10131(13) 0.32174(14) 0.0214(4) Uani 1 1 d . . . . .
C20 C -0.4061(2) -0.14781(14) 0.34237(16) 0.0271(5) Uani 1 1 d . . . . .
H20 H -0.3904 -0.1740 0.3923 0.032 Uiso 1 1 calc R U . . .
C21 C -0.5227(2) -0.15689(14) 0.29236(17) 0.0293(5) Uani 1 1 d . . . . .
C22 C -0.54440(19) -0.12095(15) 0.21824(17) 0.0287(5) Uani 1 1 d . . . . .
H22 H -0.6248 -0.1286 0.1821 0.034 Uiso 1 1 calc R U . . .
C23 C -0.45234(18) -0.07381(14) 0.19463(15) 0.0219(4) Uani 1 1 d . . . . .
C24 C -0.1861(2) -0.09636(16) 0.37601(17) 0.0323(5) Uani 1 1 d . . . . .
H24A H -0.1593 -0.1255 0.3319 0.048 Uiso 1 1 calc R U . . .
H24B H -0.1887 -0.1311 0.4211 0.048 Uiso 1 1 calc R U . . .
H24C H -0.1290 -0.0292 0.4105 0.048 Uiso 1 1 calc R U . . .
C25 C -0.6235(2) -0.20276(17) 0.3193(2) 0.0446(7) Uani 1 1 d . . . . .
H25A H -0.5950 -0.2322 0.3666 0.067 Uiso 1 1 calc R U . . .
H25B H -0.6937 -0.2520 0.2629 0.067 Uiso 1 1 calc R U . . .
H25C H -0.6471 -0.1538 0.3457 0.067 Uiso 1 1 calc R U . . .
C26 C -0.4815(2) -0.03535(17) 0.11346(17) 0.0327(5) Uani 1 1 d . . . . .
H26A H -0.4852 -0.0784 0.0579 0.049 Uiso 1 1 calc R U . . .
H26B H -0.4183 0.0285 0.1314 0.049 Uiso 1 1 calc R U . . .
H26C H -0.5602 -0.0312 0.0982 0.049 Uiso 1 1 calc R U . . .
C27 C 0.22340(16) 0.38426(13) 0.38718(13) 0.0152(4) Uani 1 1 d . . . . .
C28 C 0.22204(16) 0.46463(13) 0.36018(13) 0.0177(4) Uani 1 1 d . . . . .
C29 C 0.30261(18) 0.55517(14) 0.42550(15) 0.0233(4) Uani 1 1 d . . . . .
H29 H 0.3029 0.6100 0.4075 0.028 Uiso 1 1 calc R U . . .
C30 C 0.38230(18) 0.56794(14) 0.51593(15) 0.0256(5) Uani 1 1 d . . . . .
C31 C 0.38349(18) 0.48728(15) 0.54013(14) 0.0253(5) Uani 1 1 d . . . . .
H31 H 0.4390 0.4950 0.6014 0.030 Uiso 1 1 calc R U . . .
C32 C 0.30571(17) 0.39534(14) 0.47729(13) 0.0196(4) Uani 1 1 d . . . . .
C33 C 0.3120(2) 0.31029(15) 0.50785(15) 0.0284(5) Uani 1 1 d . . . . .
H33A H 0.2550 0.2918 0.5360 0.043 Uiso 1 1 calc R U . . .
H33B H 0.3946 0.3274 0.5547 0.043 Uiso 1 1 calc R U . . .
H33C H 0.2904 0.2565 0.4527 0.043 Uiso 1 1 calc R U . . .
C34 C 0.4643(2) 0.66695(16) 0.58636(19) 0.0430(7) Uani 1 1 d . . . . .
H34A H 0.4436 0.6758 0.6403 0.065 Uiso 1 1 calc R U . . .
H34B H 0.4537 0.7147 0.5560 0.065 Uiso 1 1 calc R U . . .
H34C H 0.5490 0.6747 0.6086 0.065 Uiso 1 1 calc R U . . .
C35 C 0.13469(19) 0.45534(16) 0.26435(15) 0.0280(5) Uani 1 1 d . . . . .
H35A H 0.1356 0.5184 0.2637 0.042 Uiso 1 1 calc R U . . .
H35B H 0.0527 0.4114 0.2506 0.042 Uiso 1 1 calc R U . . .
H35C H 0.1587 0.4301 0.2162 0.042 Uiso 1 1 calc R U . . .
C36 C -0.08709(17) 0.27054(13) 0.52439(13) 0.0165(4) Uani 1 1 d . . . . .
C37 C -0.08723(18) 0.36946(14) 0.52670(14) 0.0215(4) Uani 1 1 d . . . . .
H37A H -0.1605 0.3620 0.4738 0.032 Uiso 1 1 calc R U . . .
H37B H -0.0152 0.4087 0.5211 0.032 Uiso 1 1 calc R U . . .
H37C H -0.0861 0.4009 0.5866 0.032 Uiso 1 1 calc R U . . .
C38 C 0.02426(19) 0.28187(15) 0.60989(14) 0.0250(4) Uani 1 1 d . . . . .
H38A H 0.0211 0.3117 0.6684 0.037 Uiso 1 1 calc R U . . .
H38B H 0.0983 0.3224 0.6076 0.037 Uiso 1 1 calc R U . . .
H38C H 0.0246 0.2187 0.6083 0.037 Uiso 1 1 calc R U . . .
C39 C -0.20177(19) 0.21087(14) 0.53093(15) 0.0251(5) Uani 1 1 d . . . . .
H39A H -0.2734 0.2028 0.4762 0.038 Uiso 1 1 calc R U . . .
H39B H -0.2031 0.2436 0.5893 0.038 Uiso 1 1 calc R U . . .
H39C H -0.2024 0.1479 0.5316 0.038 Uiso 1 1 calc R U . . .
C40 C 0.25878(15) 0.20497(12) 0.06580(12) 0.0126(3) Uani 1 1 d . . . . .
C41 C 0.37476(16) 0.29134(12) 0.09919(12) 0.0128(4) Uani 1 1 d . . . . .
C42 C 0.48409(16) 0.28160(13) 0.13417(13) 0.0152(4) Uani 1 1 d . . . . .
H42 H 0.4834 0.2200 0.1319 0.018 Uiso 1 1 calc R U . . .
C43 C 0.59414(16) 0.36061(13) 0.17233(13) 0.0169(4) Uani 1 1 d . . . . .
C44 C 0.59101(17) 0.45002(13) 0.17613(13) 0.0184(4) Uani 1 1 d . . . . .
H44 H 0.6657 0.5049 0.2033 0.022 Uiso 1 1 calc R U . . .
C45 C 0.48354(17) 0.46220(13) 0.14191(13) 0.0170(4) Uani 1 1 d . . . . .
C46 C 0.37481(16) 0.38031(12) 0.10142(12) 0.0148(4) Uani 1 1 d . . . . .
H46 H 0.2998 0.3860 0.0750 0.018 Uiso 1 1 calc R U . . .
C47 C 0.71559(17) 0.35077(14) 0.20623(15) 0.0220(4) Uani 1 1 d . . . . .
C48 C 0.7033(2) 0.25546(17) 0.2217(2) 0.0468(7) Uani 1 1 d . . . . .
H48A H 0.7838 0.2542 0.2474 0.070 Uiso 1 1 calc R U . . .
H48B H 0.6512 0.2033 0.1612 0.070 Uiso 1 1 calc R U . . .
H48C H 0.6672 0.2474 0.2663 0.070 Uiso 1 1 calc R U . . .
C49 C 0.7614(2) 0.3571(2) 0.12955(18) 0.0483(7) Uani 1 1 d . . . . .
H49A H 0.8391 0.3509 0.1494 0.072 Uiso 1 1 calc R U . . .
H49B H 0.7726 0.4192 0.1200 0.072 Uiso 1 1 calc R U . . .
H49C H 0.7019 0.3055 0.0702 0.072 Uiso 1 1 calc R U . . .
C50 C 0.8094(2) 0.43066(17) 0.29825(17) 0.0348(5) Uani 1 1 d . . . . .
H50A H 0.7767 0.4320 0.3456 0.052 Uiso 1 1 calc R U . . .
H50B H 0.8286 0.4922 0.2870 0.052 Uiso 1 1 calc R U . . .
H50C H 0.8833 0.4192 0.3215 0.052 Uiso 1 1 calc R U . . .
C51 C 0.48054(18) 0.56114(13) 0.15108(14) 0.0203(4) Uani 1 1 d . . . . .
C52 C 0.6074(2) 0.64186(15) 0.1932(2) 0.0406(6) Uani 1 1 d . . . . .
H52A H 0.6551 0.6427 0.2566 0.061 Uiso 1 1 calc R U . . .
H52B H 0.6007 0.7034 0.1976 0.061 Uiso 1 1 calc R U . . .
H52C H 0.6479 0.6312 0.1525 0.061 Uiso 1 1 calc R U . . .
C53 C 0.4189(2) 0.57938(16) 0.21573(17) 0.0344(5) Uani 1 1 d . . . . .
H53A H 0.3360 0.5298 0.1880 0.052 Uiso 1 1 calc R U . . .
H53B H 0.4162 0.6424 0.2222 0.052 Uiso 1 1 calc R U . . .
H53C H 0.4651 0.5776 0.2782 0.052 Uiso 1 1 calc R U . . .
C54 C 0.4075(2) 0.56435(17) 0.05456(16) 0.0386(6) Uani 1 1 d . . . . .
H54A H 0.4463 0.5532 0.0126 0.058 Uiso 1 1 calc R U . . .
H54B H 0.4045 0.6273 0.0617 0.058 Uiso 1 1 calc R U . . .
H54C H 0.3248 0.5146 0.0272 0.058 Uiso 1 1 calc R U . . .
C1S C 0.2292(3) 0.01247(18) 0.3383(2) 0.0414(6) Uani 1 1 d . . . . .
C2S C 0.3394(3) 0.03335(17) 0.41146(18) 0.0424(6) Uani 1 1 d . . . . .
H2S H 0.3417 0.0246 0.4694 0.051 Uiso 1 1 calc R U . . .
C3S C 0.4463(3) 0.06667(17) 0.4018(2) 0.0477(7) Uani 1 1 d . . . . .
H3S H 0.5210 0.0794 0.4526 0.057 Uiso 1 1 calc R U . . .
C4S C 0.4452(3) 0.08152(17) 0.3192(2) 0.0473(7) Uani 1 1 d . . . . .
H4S H 0.5190 0.1055 0.3129 0.057 Uiso 1 1 calc R U . . .
C5S C 0.3363(3) 0.06120(19) 0.2457(2) 0.0462(7) Uani 1 1 d . . . . .
H5S H 0.3346 0.0713 0.1883 0.055 Uiso 1 1 calc R U . . .
C6S C 0.2295(3) 0.0263(2) 0.2551(2) 0.0470(7) Uani 1 1 d . . . . .
H6S H 0.1547 0.0114 0.2034 0.056 Uiso 1 1 calc R U . . .
C7S C 0.1124(3) -0.0236(3) 0.3479(3) 0.0657(9) Uani 1 1 d . . . . .
H7S1 H 0.1294 -0.0272 0.4117 0.099 Uiso 1 1 calc R U . . .
H7S2 H 0.0589 -0.0875 0.3010 0.099 Uiso 1 1 calc R U . . .
H7S3 H 0.0725 0.0203 0.3373 0.099 Uiso 1 1 calc R U . . .


_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
C14S C8S 1.495(5) . ?
C14S H14A 0.9800 . ?
C14S H14B 0.9800 . ?
C14S H14C 0.9800 . ?
C8S C9S 1.3900 . ?
C8S C13S 1.3900 . ?
C9S C10S 1.3900 . ?
C9S H9S 0.9500 . ?
C10S C11S 1.3900 . ?
C10S H10S 0.9500 . ?
C11S C12S 1.3900 . ?
C11S H11S 0.9500 . ?
C12S C13S 1.3900 . ?
C12S H12S 0.9500 . ?
C13S H13S 0.9500 . ?
C14X C8X 1.494(5) . ?
C14X H14X 0.9800 . ?
C14X H14Y 0.9800 . ?
C14X H14Z 0.9800 . ?
C8X C9X 1.3900 . ?
C8X C13X 1.3900 . ?
C9X C10X 1.3900 . ?
C9X H9X 0.9500 . ?
C10X C11X 1.3900 . ?
C10X H10X 0.9500 . ?
C11X C12X 1.3900 . ?
C11X H11X 0.9500 . ?
C12X C13X 1.3900 . ?
C12X H12X 0.9500 . ?
C13X H13X 0.9500 . ?
Ni1 N2 1.9563(14) . ?
Ni1 N2 1.9563(14) 2 ?
Ni1 N1 1.9615(14) 2 ?
Ni1 N1 1.9616(14) . ?
N1 C8 1.358(2) . ?
N1 C1 1.419(2) . ?
N2 C15 1.353(2) . ?
N2 C17 1.424(2) . ?
O1 C2 1.243(3) . ?
O2 C16 1.264(3) . ?
C1 C40 1.380(2) 2 ?
C1 C2 1.439(2) . ?
C2 C3 1.433(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.375(2) . ?
C3 C8 1.439(2) . ?
C4 C5 1.437(2) . ?
C4 C18 1.498(2) . ?
C5 C9 1.406(2) . ?
C5 C6 1.426(2) . ?
C6 C12 1.426(2) . ?
C6 C7 1.426(2) . ?
C7 C8 1.389(2) . ?
C7 C15 1.394(2) . ?
C9 C10 1.387(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.396(2) . ?
C10 C36 1.534(2) . ?
C11 C12 1.393(2) . ?
C11 H11 0.9500 . ?
C12 C13 1.442(2) . ?
C13 C14 1.375(2) . ?
C13 C27 1.493(2) . ?
C14 C16 1.431(2) . ?
C14 C15 1.433(2) . ?
C16 C17 1.432(2) . ?
C16 H16 0.9500 . ?
C17 C40 1.386(2) . ?
C18 C19 1.398(3) . ?
C18 C23 1.399(3) . ?
C19 C20 1.396(3) . ?
C19 C24 1.503(3) . ?
C20 C21 1.381(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.381(3) . ?
C21 C25 1.511(3) . ?
C22 C23 1.394(3) . ?
C22 H22 0.9500 . ?
C23 C26 1.508(3) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C32 1.401(3) . ?
C27 C28 1.401(3) . ?
C28 C29 1.392(3) . ?
C28 C35 1.501(3) . ?
C29 C30 1.385(3) . ?
C29 H29 0.9500 . ?
C30 C31 1.385(3) . ?
C30 C34 1.506(3) . ?
C31 C32 1.389(3) . ?
C31 H31 0.9500 . ?
C32 C33 1.510(3) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C39 1.526(2) . ?
C36 C38 1.533(3) . ?
C36 C37 1.534(3) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 C1 1.380(2) 2 ?
C40 C41 1.499(2) . ?
C41 C46 1.379(2) . ?
C41 C42 1.390(3) . ?
C42 C43 1.387(2) . ?
C42 H42 0.9500 . ?
C43 C44 1.396(3) . ?
C43 C47 1.533(3) . ?
C44 C45 1.387(3) . ?
C44 H44 0.9500 . ?
C45 C46 1.397(2) . ?
C45 C51 1.534(3) . ?
C46 H46 0.9500 . ?
C47 C48 1.519(3) . ?
C47 C50 1.521(3) . ?
C47 C49 1.532(3) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 C54 1.523(3) . ?
C51 C52 1.530(3) . ?
C51 C53 1.534(3) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C1S C2S 1.382(4) . ?
C1S C6S 1.383(4) . ?
C1S C7S 1.501(4) . ?
C2S C3S 1.380(4) . ?
C2S H2S 0.9500 . ?
C3S C4S 1.375(4) . ?
C3S H3S 0.9500 . ?
C4S C5S 1.375(4) . ?
C4S H4S 0.9500 . ?
C5S C6S 1.379(4) . ?
C5S H5S 0.9500 . ?
C6S H6S 0.9500 . ?
C7S H7S1 0.9800 . ?
C7S H7S2 0.9800 . ?
C7S H7S3 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
C8S C14S H14A 109.5 . . ?
C8S C14S H14B 109.5 . . ?
H14A C14S H14B 109.5 . . ?
C8S C14S H14C 109.5 . . ?
H14A C14S H14C 109.5 . . ?
H14B C14S H14C 109.5 . . ?
C9S C8S C13S 120.0 . . ?
C9S C8S C14S 118.4(11) . . ?
C13S C8S C14S 121.2(11) . . ?
C8S C9S C10S 120.0 . . ?
C8S C9S H9S 120.0 . . ?
C10S C9S H9S 120.0 . . ?
C11S C10S C9S 120.0 . . ?
C11S C10S H10S 120.0 . . ?
C9S C10S H10S 120.0 . . ?
C10S C11S C12S 120.0 . . ?
C10S C11S H11S 120.0 . . ?
C12S C11S H11S 120.0 . . ?
C11S C12S C13S 120.0 . . ?
C11S C12S H12S 120.0 . . ?
C13S C12S H12S 120.0 . . ?
C12S C13S C8S 120.0 . . ?
C12S C13S H13S 120.0 . . ?
C8S C13S H13S 120.0 . . ?
C8X C14X H14X 109.5 . . ?
C8X C14X H14Y 109.5 . . ?
H14X C14X H14Y 109.5 . . ?
C8X C14X H14Z 109.5 . . ?
H14X C14X H14Z 109.5 . . ?
H14Y C14X H14Z 109.5 . . ?
C9X C8X C13X 120.0 . . ?
C9X C8X C14X 122.0(12) . . ?
C13X C8X C14X 118.0(12) . . ?
C10X C9X C8X 120.0 . . ?
C10X C9X H9X 120.0 . . ?
C8X C9X H9X 120.0 . . ?
C9X C10X C11X 120.0 . . ?
C9X C10X H10X 120.0 . . ?
C11X C10X H10X 120.0 . . ?
C12X C11X C10X 120.0 . . ?
C12X C11X H11X 120.0 . . ?
C10X C11X H11X 120.0 . . ?
C13X C12X C11X 120.0 . . ?
C13X C12X H12X 120.0 . . ?
C11X C12X H12X 120.0 . . ?
C12X C13X C8X 120.0 . . ?
C12X C13X H13X 120.0 . . ?
C8X C13X H13X 120.0 . . ?
N2 Ni1 N2 180.0 . 2 ?
N2 Ni1 N1 89.00(6) . 2 ?
N2 Ni1 N1 91.00(6) 2 2 ?
N2 Ni1 N1 91.00(6) . . ?
N2 Ni1 N1 89.00(6) 2 . ?
N1 Ni1 N1 180.0 2 . ?
C8 N1 C1 104.38(13) . . ?
C8 N1 Ni1 126.55(11) . . ?
C1 N1 Ni1 129.06(11) . . ?
C15 N2 C17 104.16(14) . . ?
C15 N2 Ni1 126.76(11) . . ?
C17 N2 Ni1 129.00(11) . . ?
C40 C1 N1 125.14(15) 2 . ?
C40 C1 C2 123.46(16) 2 . ?
N1 C1 C2 111.40(15) . . ?
O1 C2 C3 125.9(2) . . ?
O1 C2 C1 128.6(2) . . ?
C3 C2 C1 105.45(15) . . ?
C3 C2 H2 127.3 . . ?
C1 C2 H2 127.3 . . ?
C4 C3 C2 132.22(16) . . ?
C4 C3 C8 122.55(16) . . ?
C2 C3 C8 105.22(15) . . ?
C3 C4 C5 118.66(16) . . ?
C3 C4 C18 121.17(16) . . ?
C5 C4 C18 120.17(15) . . ?
C9 C5 C6 119.26(16) . . ?
C9 C5 C4 121.52(16) . . ?
C6 C5 C4 119.21(15) . . ?
C5 C6 C12 118.34(15) . . ?
C5 C6 C7 120.88(16) . . ?
C12 C6 C7 120.78(15) . . ?
C8 C7 C15 121.24(16) . . ?
C8 C7 C6 119.39(15) . . ?
C15 C7 C6 119.35(16) . . ?
N1 C8 C7 127.20(16) . . ?
N1 C8 C3 113.52(15) . . ?
C7 C8 C3 119.28(15) . . ?
C10 C9 C5 122.54(16) . . ?
C10 C9 H9 118.7 . . ?
C5 C9 H9 118.7 . . ?
C9 C10 C11 117.65(16) . . ?
C9 C10 C36 123.59(15) . . ?
C11 C10 C36 118.73(15) . . ?
C12 C11 C10 122.55(16) . . ?
C12 C11 H11 118.7 . . ?
C10 C11 H11 118.7 . . ?
C11 C12 C6 119.64(16) . . ?
C11 C12 C13 120.91(16) . . ?
C6 C12 C13 119.44(15) . . ?
C14 C13 C12 118.11(16) . . ?
C14 C13 C27 121.38(15) . . ?
C12 C13 C27 120.51(15) . . ?
C13 C14 C16 131.50(17) . . ?
C13 C14 C15 123.11(16) . . ?
C16 C14 C15 105.38(15) . . ?
N2 C15 C7 127.23(16) . . ?
N2 C15 C14 113.61(15) . . ?
C7 C15 C14 119.14(15) . . ?
O2 C16 C14 124.6(2) . . ?
O2 C16 C17 129.5(2) . . ?
C14 C16 C17 105.41(15) . . ?
C14 C16 H16 127.3 . . ?
C17 C16 H16 127.3 . . ?
C40 C17 N2 125.00(16) . . ?
C40 C17 C16 123.58(16) . . ?
N2 C17 C16 111.41(15) . . ?
C19 C18 C23 120.46(17) . . ?
C19 C18 C4 119.72(18) . . ?
C23 C18 C4 119.80(17) . . ?
C20 C19 C18 118.7(2) . . ?
C20 C19 C24 119.85(19) . . ?
C18 C19 C24 121.39(17) . . ?
C21 C20 C19 121.9(2) . . ?
C21 C20 H20 119.0 . . ?
C19 C20 H20 119.0 . . ?
C20 C21 C22 118.15(18) . . ?
C20 C21 C25 121.1(2) . . ?
C22 C21 C25 120.8(2) . . ?
C21 C22 C23 122.3(2) . . ?
C21 C22 H22 118.9 . . ?
C23 C22 H22 118.9 . . ?
C22 C23 C18 118.39(19) . . ?
C22 C23 C26 119.79(19) . . ?
C18 C23 C26 121.82(17) . . ?
C19 C24 H24A 109.5 . . ?
C19 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C19 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C21 C25 H25A 109.5 . . ?
C21 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C21 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C32 C27 C28 120.42(17) . . ?
C32 C27 C13 119.88(17) . . ?
C28 C27 C13 119.68(17) . . ?
C29 C28 C27 118.43(18) . . ?
C29 C28 C35 119.77(18) . . ?
C27 C28 C35 121.79(17) . . ?
C30 C29 C28 122.15(19) . . ?
C30 C29 H29 118.9 . . ?
C28 C29 H29 118.9 . . ?
C31 C30 C29 118.22(18) . . ?
C31 C30 C34 121.0(2) . . ?
C29 C30 C34 120.8(2) . . ?
C30 C31 C32 121.9(2) . . ?
C30 C31 H31 119.1 . . ?
C32 C31 H31 119.1 . . ?
C31 C32 C27 118.87(18) . . ?
C31 C32 C33 119.27(18) . . ?
C27 C32 C33 121.85(17) . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C30 C34 H34A 109.5 . . ?
C30 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C30 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C28 C35 H35A 109.5 . . ?
C28 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C28 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C39 C36 C38 108.97(16) . . ?
C39 C36 C10 112.13(15) . . ?
C38 C36 C10 108.23(15) . . ?
C39 C36 C37 107.98(16) . . ?
C38 C36 C37 109.45(16) . . ?
C10 C36 C37 110.04(15) . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C36 C39 H39A 109.5 . . ?
C36 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C36 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C1 C40 C17 122.67(16) 2 . ?
C1 C40 C41 119.66(15) 2 . ?
C17 C40 C41 117.61(15) . . ?
C46 C41 C42 119.98(16) . . ?
C46 C41 C40 121.26(16) . . ?
C42 C41 C40 118.62(16) . . ?
C43 C42 C41 120.88(17) . . ?
C43 C42 H42 119.6 . . ?
C41 C42 H42 119.6 . . ?
C42 C43 C44 117.68(17) . . ?
C42 C43 C47 121.73(17) . . ?
C44 C43 C47 120.55(16) . . ?
C45 C44 C43 122.86(17) . . ?
C45 C44 H44 118.6 . . ?
C43 C44 H44 118.6 . . ?
C44 C45 C46 117.54(17) . . ?
C44 C45 C51 122.61(16) . . ?
C46 C45 C51 119.79(17) . . ?
C41 C46 C45 120.99(17) . . ?
C41 C46 H46 119.5 . . ?
C45 C46 H46 119.5 . . ?
C48 C47 C50 108.28(19) . . ?
C48 C47 C49 108.2(2) . . ?
C50 C47 C49 108.92(19) . . ?
C48 C47 C43 112.38(16) . . ?
C50 C47 C43 111.19(17) . . ?
C49 C47 C43 107.81(17) . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C47 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C47 C50 H50A 109.5 . . ?
C47 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C47 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C54 C51 C52 108.10(19) . . ?
C54 C51 C45 110.38(16) . . ?
C52 C51 C45 112.58(17) . . ?
C54 C51 C53 108.61(19) . . ?
C52 C51 C53 108.57(18) . . ?
C45 C51 C53 108.51(16) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C2S C1S C6S 117.8(3) . . ?
C2S C1S C7S 121.6(2) . . ?
C6S C1S C7S 120.5(3) . . ?
C3S C2S C1S 121.1(2) . . ?
C3S C2S H2S 119.4 . . ?
C1S C2S H2S 119.4 . . ?
C4S C3S C2S 120.4(3) . . ?
C4S C3S H3S 119.8 . . ?
C2S C3S H3S 119.8 . . ?
C5S C4S C3S 119.2(3) . . ?
C5S C4S H4S 120.4 . . ?
C3S C4S H4S 120.4 . . ?
C4S C5S C6S 120.2(3) . . ?
C4S C5S H5S 119.9 . . ?
C6S C5S H5S 119.9 . . ?
C5S C6S C1S 121.3(3) . . ?
C5S C6S H6S 119.3 . . ?
C1S C6S H6S 119.3 . . ?
C1S C7S H7S1 109.5 . . ?
C1S C7S H7S2 109.5 . . ?
H7S1 C7S H7S2 109.5 . . ?
C1S C7S H7S3 109.5 . . ?
H7S1 C7S H7S3 109.5 . . ?
H7S2 C7S H7S3 109.5 . . ?

_refine_diff_density_max         0.504
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.058

_shelxl_version_number           2013-3



####################################################################### 
# 
# 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_E180
_database_code_depnum_ccdc_archive 'CCDC 1019261'
_audit_update_record             
;
2014-08-13 deposited with the CCDC.
2015-02-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C136 H142 N4 Ni O2'
_chemical_formula_weight         1923.24

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'
N N 0.0311 0.0180 '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'
Ni Ni -3.0029 0.5091 '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                   12.8500(12)
_cell_length_b                   15.5881(15)
_cell_length_c                   15.9283(15)
_cell_angle_alpha                100.951(5)
_cell_angle_beta                 110.033(5)
_cell_angle_gamma                108.118(5)
_cell_volume                     2687.2(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9897
_cell_measurement_theta_min      3.13
_cell_measurement_theta_max      66.88

_exptl_crystal_description       Block
_exptl_crystal_colour            Dark_Red
_exptl_crystal_density_meas      'Not Measured'
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_F_000             1030
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.684
_shelx_estimated_absorpt_T_min   0.904
_shelx_estimated_absorpt_T_max   0.980
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.4989
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            36244
_diffrn_reflns_av_unetI/netI     0.0750
_diffrn_reflns_av_R_equivalents  0.0839
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.131
_diffrn_reflns_theta_max         66.580
_diffrn_reflns_theta_full        66.500
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measured_fraction_theta_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_point_group_measured_fraction_full 0.961
_reflns_number_total             9117
_reflns_number_gt                6330
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.1538P)²+0.2272P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9117
_refine_ls_number_parameters     682
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.1098
_refine_ls_R_factor_gt           0.0771
_refine_ls_wR_factor_ref         0.2360
_refine_ls_wR_factor_gt          0.2016
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.065
_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
Ni1 Ni 1.0000 1.0000 0.0000 0.0284(2) Uani 1 2 d S . P . .
O1 O 0.6323(3) 0.7940(2) 0.0724(2) 0.0387(11) Uani 0.692(6) 1 d . . P A 1
O2 O 1.3352(7) 1.3502(5) 0.2544(6) 0.042(2) Uani 0.308(6) 1 d . . P A 2
N1 N 0.8807(2) 0.95654(18) 0.05160(19) 0.0294(6) Uani 1 1 d . . . . .
N2 N 1.0877(2) 1.12298(17) 0.10323(18) 0.0280(6) Uani 1 1 d . . . . .
C1 C 0.7799(3) 0.8681(2) 0.0164(2) 0.0291(7) Uani 1 1 d D . . . .
C2 C 0.7137(8) 0.8610(6) 0.0775(6) 0.0278(16) Uani 0.692(6) 1 d D . P A 1
C2A C 0.732(2) 0.8676(13) 0.0824(15) 0.030 Uiso 0.308(6) 1 d D U P A 2
H2A H 0.6697 0.8130 0.0795 0.030 Uiso 0.308(6) 1 calc R U P A 2
C3 C 0.7852(3) 0.9556(2) 0.1531(2) 0.0315(7) Uani 1 1 d D . . . .
C4 C 0.7682(3) 0.9930(2) 0.2297(2) 0.0316(7) Uani 1 1 d . . . . .
C5 C 0.8516(3) 1.0890(2) 0.2927(2) 0.0312(7) Uani 1 1 d . . . . .
C6 C 0.9485(3) 1.1400(2) 0.2728(2) 0.0310(7) Uani 1 1 d . . . . .
C7 C 0.9626(3) 1.0988(2) 0.1916(2) 0.0300(7) Uani 1 1 d . . . . .
C8 C 0.8807(3) 1.0066(2) 0.1312(2) 0.0290(7) Uani 1 1 d . . . . .
C9 C 0.8399(3) 1.1326(2) 0.3727(2) 0.0319(7) Uani 1 1 d . . . . .
H9 H 0.770(3) 1.095(3) 0.380(3) 0.038 Uiso 1 1 d . U . . .
C10 C 0.9203(3) 1.2240(2) 0.4344(2) 0.0324(7) Uani 1 1 d . . . . .
C11 C 1.0151(3) 1.2729(2) 0.4149(2) 0.0316(7) Uani 1 1 d . . . . .
H11 H 1.0707 1.3357 0.4566 0.038 Uiso 1 1 calc R U . . .
C12 C 1.0323(3) 1.2342(2) 0.3367(2) 0.0307(7) Uani 1 1 d . . . . .
C13 C 1.1330(3) 1.2860(2) 0.3200(2) 0.0325(7) Uani 1 1 d . . . . .
C14 C 1.1450(3) 1.2440(2) 0.2415(2) 0.0312(7) Uani 1 1 d D . . . .
C15 C 1.2322(11) 1.2704(4) 0.2075(7) 0.0297(18) Uani 0.692(6) 1 d D . P A 1
H15 H 1.3050 1.3270 0.2376 0.036 Uiso 0.692(6) 1 calc R U P A 1
C15A C 1.236(2) 1.2854(12) 0.2061(17) 0.030 Uiso 0.308(6) 1 d D U P A 2
C16 C 1.1958(3) 1.2012(2) 0.1226(2) 0.0296(7) Uani 1 1 d D . . . .
C17 C 1.0599(3) 1.1507(2) 0.1755(2) 0.0306(7) Uani 1 1 d . . . . .
C18 C 0.9128(3) 1.2712(2) 0.5250(2) 0.0358(7) Uani 1 1 d . . . . .
C19 C 0.9131(3) 1.3699(2) 0.5276(3) 0.0398(8) Uani 1 1 d . . . . .
H19A H 0.8404 1.3627 0.4745 0.060 Uiso 1 1 calc R U . . .
H19B H 0.9855 1.4091 0.5227 0.060 Uiso 1 1 calc R U . . .
H19C H 0.9136 1.4011 0.5874 0.060 Uiso 1 1 calc R U . . .
C20 C 1.0243(3) 1.2827(3) 0.6109(2) 0.0410(8) Uani 1 1 d . . . . .
H20A H 1.0210 1.3125 0.6693 0.061 Uiso 1 1 calc R U . . .
H20B H 1.0982 1.3233 0.6087 0.061 Uiso 1 1 calc R U . . .
H20C H 1.0249 1.2198 0.6093 0.061 Uiso 1 1 calc R U . . .
C21 C 0.7980(3) 1.2122(3) 0.5317(3) 0.0434(8) Uani 1 1 d . . . . .
H21A H 0.7265 1.2044 0.4770 0.065 Uiso 1 1 calc R U . . .
H21B H 0.7971 1.2453 0.5901 0.065 Uiso 1 1 calc R U . . .
H21C H 0.7968 1.1492 0.5324 0.065 Uiso 1 1 calc R U . . .
C22 C 0.6664(3) 0.9379(2) 0.2496(2) 0.0339(7) Uani 1 1 d . . . . .
C23 C 0.5477(3) 0.9267(2) 0.1964(3) 0.0388(8) Uani 1 1 d . . . . .
C24 C 0.4565(3) 0.8803(2) 0.2195(3) 0.0452(9) Uani 1 1 d . . . . .
H24 H 0.3762 0.8728 0.1834 0.054 Uiso 1 1 calc R U . . .
C25 C 0.4784(4) 0.8441(2) 0.2942(3) 0.0469(9) Uani 1 1 d . . . . .
C26 C 0.5952(3) 0.8529(2) 0.3438(3) 0.0440(9) Uani 1 1 d . . . . .
H26 H 0.6112 0.8264 0.3934 0.053 Uiso 1 1 calc R U . . .
C27 C 0.6899(3) 0.8992(2) 0.3232(3) 0.0383(8) Uani 1 1 d . . . . .
C28 C 0.5185(3) 0.9654(3) 0.1149(3) 0.0477(9) Uani 1 1 d . . . . .
H28A H 0.5089 0.9201 0.0581 0.072 Uiso 1 1 calc R U . . .
H28B H 0.5846 1.0270 0.1312 0.072 Uiso 1 1 calc R U . . .
H28C H 0.4429 0.9740 0.1027 0.072 Uiso 1 1 calc R U . . .
C29 C 0.3776(4) 0.7983(3) 0.3212(4) 0.0603(12) Uani 1 1 d . . . . .
H29A H 0.4052 0.7670 0.3670 0.090 Uiso 1 1 calc R U . . .
H29B H 0.3065 0.7507 0.2645 0.090 Uiso 1 1 calc R U . . .
H29C H 0.3560 0.8476 0.3497 0.090 Uiso 1 1 calc R U . . .
C30 C 0.8151(3) 0.9040(3) 0.3769(3) 0.0493(9) Uani 1 1 d . . . . .
H30A H 0.8127 0.8683 0.4212 0.074 Uiso 1 1 calc R U . . .
H30B H 0.8719 0.9709 0.4123 0.074 Uiso 1 1 calc R U . . .
H30C H 0.8418 0.8759 0.3322 0.074 Uiso 1 1 calc R U . . .
C31 C 1.2231(3) 1.3835(2) 0.3872(2) 0.0316(7) Uani 1 1 d . . . . .
C32 C 1.2228(3) 1.4638(2) 0.3606(2) 0.0343(7) Uani 1 1 d . . . . .
C33 C 1.3040(3) 1.5539(2) 0.4260(3) 0.0390(8) Uani 1 1 d . . . . .
H33 H 1.3050 1.6087 0.4079 0.047 Uiso 1 1 calc R U . . .
C34 C 1.3839(3) 1.5666(2) 0.5170(3) 0.0420(9) Uani 1 1 d . . . . .
C35 C 1.3838(3) 1.4858(2) 0.5410(3) 0.0406(8) Uani 1 1 d . . . . .
H35 H 1.4385 1.4932 0.6026 0.049 Uiso 1 1 calc R U . . .
C36 C 1.3062(3) 1.3940(2) 0.4777(2) 0.0353(7) Uani 1 1 d . . . . .
C37 C 1.1346(3) 1.4552(3) 0.2651(3) 0.0425(8) Uani 1 1 d . . . . .
H37A H 1.1560 1.4278 0.2161 0.064 Uiso 1 1 calc R U . . .
H37B H 1.1380 1.5187 0.2643 0.064 Uiso 1 1 calc R U . . .
H37C H 1.0524 1.4134 0.2527 0.064 Uiso 1 1 calc R U . . .
C38 C 1.4657(3) 1.6653(3) 0.5885(3) 0.0574(11) Uani 1 1 d . . . . .
H38A H 1.4511 1.6709 0.6453 0.086 Uiso 1 1 calc R U . . .
H38B H 1.4486 1.7133 0.5611 0.086 Uiso 1 1 calc R U . . .
H38C H 1.5506 1.6757 0.6054 0.086 Uiso 1 1 calc R U . . .
C39 C 1.3116(3) 1.3092(3) 0.5077(3) 0.0446(8) Uani 1 1 d . . . . .
H39A H 1.3928 1.3269 0.5570 0.067 Uiso 1 1 calc R U . . .
H39B H 1.2939 1.2566 0.4530 0.067 Uiso 1 1 calc R U . . .
H39C H 1.2514 1.2889 0.5326 0.067 Uiso 1 1 calc R U . . .
C40 C 0.7414(3) 0.7948(2) -0.0656(2) 0.0293(7) Uani 1 1 d . . . . .
C41 C 0.6262(3) 0.7086(2) -0.0993(2) 0.0302(7) Uani 1 1 d . . . . .
C42 C 0.5156(3) 0.7176(2) -0.1358(2) 0.0322(7) Uani 1 1 d . . . . .
H42 H 0.5159 0.7789 -0.1343 0.039 Uiso 1 1 calc R U . . .
C43 C 0.4066(3) 0.6393(2) -0.1736(2) 0.0346(7) Uani 1 1 d . . . . .
C44 C 0.4088(3) 0.5503(2) -0.1781(2) 0.0364(8) Uani 1 1 d . . . . .
H44 H 0.3340 0.4956 -0.2060 0.044 Uiso 1 1 calc R U . . .
C45 C 0.5171(3) 0.5379(2) -0.1432(2) 0.0344(7) Uani 1 1 d . . . . .
C46 C 0.6255(3) 0.6194(2) -0.1030(2) 0.0322(7) Uani 1 1 d . . . . .
H46 H 0.7004 0.6133 -0.0777 0.039 Uiso 1 1 calc R U . . .
C47 C 0.2844(3) 0.6493(2) -0.2075(3) 0.0393(8) Uani 1 1 d . . . . .
C48 C 0.2957(3) 0.7437(3) -0.2232(4) 0.0607(12) Uani 1 1 d . . . . .
H48A H 0.3281 0.7504 -0.2702 0.091 Uiso 1 1 calc R U . . .
H48B H 0.3506 0.7962 -0.1634 0.091 Uiso 1 1 calc R U . . .
H48C H 0.2156 0.7458 -0.2463 0.091 Uiso 1 1 calc R U . . .
C50 C 0.1900(3) 0.5690(3) -0.2993(3) 0.0531(10) Uani 1 1 d . . . . .
H50A H 0.1156 0.5799 -0.3218 0.080 Uiso 1 1 calc R U . . .
H50B H 0.1721 0.5076 -0.2879 0.080 Uiso 1 1 calc R U . . .
H50C H 0.2215 0.5679 -0.3473 0.080 Uiso 1 1 calc R U . . .
C49 C 0.2408(4) 0.6442(4) -0.1294(3) 0.0630(12) Uani 1 1 d . . . . .
H49A H 0.3008 0.6967 -0.0707 0.095 Uiso 1 1 calc R U . . .
H49B H 0.2310 0.5829 -0.1188 0.095 Uiso 1 1 calc R U . . .
H49C H 0.1629 0.6499 -0.1488 0.095 Uiso 1 1 calc R U . . .
C51 C 0.5202(3) 0.4394(2) -0.1522(2) 0.0363(7) Uani 1 1 d . . . . .
C52 C 0.3933(4) 0.3582(3) -0.1961(3) 0.0561(11) Uani 1 1 d . . . . .
H52A H 0.3521 0.3676 -0.1557 0.084 Uiso 1 1 calc R U . . .
H52B H 0.4003 0.2968 -0.2014 0.084 Uiso 1 1 calc R U . . .
H52C H 0.3463 0.3583 -0.2592 0.084 Uiso 1 1 calc R U . . .
C53 C 0.5910(4) 0.4357(3) -0.0547(3) 0.0544(10) Uani 1 1 d . . . . .
H53A H 0.6746 0.4838 -0.0270 0.082 Uiso 1 1 calc R U . . .
H53B H 0.5913 0.3720 -0.0613 0.082 Uiso 1 1 calc R U . . .
H53C H 0.5523 0.4488 -0.0133 0.082 Uiso 1 1 calc R U . . .
C54 C 0.5844(4) 0.4209(3) -0.2143(3) 0.0523(10) Uani 1 1 d . . . . .
H54A H 0.5438 0.4274 -0.2757 0.078 Uiso 1 1 calc R U . . .
H54B H 0.5815 0.3561 -0.2240 0.078 Uiso 1 1 calc R U . . .
H54C H 0.6692 0.4675 -0.1830 0.078 Uiso 1 1 calc R U . . .
C1X C 0.9155(5) 0.2559(3) 0.9493(3) 0.0696(13) Uani 1 1 d . U . . .
C2X C 0.8939(7) 0.3358(5) 0.9403(4) 0.109(2) Uani 1 1 d . U . . .
H2X H 0.8374 0.3499 0.9600 0.131 Uiso 1 1 calc R U . . .
C3X C 0.9530(9) 0.3940(5) 0.9034(5) 0.131(3) Uani 1 1 d . U . . .
H3X H 0.9375 0.4489 0.8978 0.157 Uiso 1 1 calc R U . . .
C4X C 1.0349(8) 0.3758(5) 0.8740(5) 0.117(3) Uani 1 1 d . U . . .
H4X H 1.0776 0.4191 0.8505 0.141 Uiso 1 1 calc R U . . .
C5X C 1.0555(5) 0.2937(5) 0.8786(4) 0.0976(19) Uani 1 1 d . U . . .
H5X H 1.1097 0.2789 0.8564 0.117 Uiso 1 1 calc R U . . .
C6X C 0.9943(4) 0.2347(4) 0.9164(4) 0.0699(13) Uani 1 1 d . U . . .
H6X H 1.0067 0.1782 0.9199 0.084 Uiso 1 1 calc R U . . .
C7X C 0.8528(5) 0.1940(4) 0.9916(4) 0.0787(14) Uani 1 1 d . . . . .
H7X1 H 0.9032 0.2148 1.0599 0.118 Uiso 1 1 calc R U . . .
H7X2 H 0.8384 0.1276 0.9624 0.118 Uiso 1 1 calc R U . . .
H7X3 H 0.7750 0.1983 0.9807 0.118 Uiso 1 1 calc R U . . .
C1Y C 0.2292(4) 0.0124(3) 0.3379(3) 0.0577(11) Uani 1 1 d . . . . .
C2Y C 0.3406(4) 0.0330(3) 0.4113(3) 0.0585(11) Uani 1 1 d . . . . .
H2Y H 0.3432 0.0231 0.4689 0.070 Uiso 1 1 calc R U . . .
C3Y C 0.4467(4) 0.0675(3) 0.4018(3) 0.0642(12) Uani 1 1 d . . . . .
H3Y H 0.5215 0.0810 0.4527 0.077 Uiso 1 1 calc R U . . .
C4Y C 0.4456(4) 0.0827(3) 0.3197(4) 0.0632(12) Uani 1 1 d . . . . .
H4Y H 0.5194 0.1071 0.3138 0.076 Uiso 1 1 calc R U . . .
C5Y C 0.3350(5) 0.0620(3) 0.2444(4) 0.0626(12) Uani 1 1 d . . . . .
H5Y H 0.3326 0.0720 0.1869 0.075 Uiso 1 1 calc R U . . .
C6Y C 0.2297(4) 0.0267(3) 0.2555(3) 0.0621(11) Uani 1 1 d . . . . .
H6Y H 0.1545 0.0118 0.2042 0.074 Uiso 1 1 calc R U . . .
C7Y C 0.1119(5) -0.0256(4) 0.3464(4) 0.0826(16) Uani 1 1 d . . . . .
H7Y1 H 0.0662 0.0129 0.3281 0.124 Uiso 1 1 calc R U . . .
H7Y2 H 0.1290 -0.0223 0.4121 0.124 Uiso 1 1 calc R U . . .
H7Y3 H 0.0639 -0.0923 0.3047 0.124 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N2 1.959(2) . ?
Ni1 N2 1.959(2) 2_775 ?
Ni1 N1 1.978(2) 2_775 ?
Ni1 N1 1.978(2) . ?
O1 C2 1.192(7) . ?
O2 C15A 1.21(2) . ?
N1 C8 1.356(4) . ?
N1 C1 1.411(4) . ?
N2 C17 1.353(4) . ?
N2 C16 1.422(4) . ?
C1 C40 1.376(4) . ?
C1 C2A 1.389(10) . ?
C1 C2 1.495(6) . ?
C2 C3 1.481(6) . ?
C2A C3 1.385(10) . ?
C2A H2A 0.9500 . ?
C3 C4 1.366(4) . ?
C3 C8 1.433(4) . ?
C4 C5 1.446(4) . ?
C4 C22 1.496(4) . ?
C5 C9 1.404(5) . ?
C5 C6 1.426(4) . ?
C6 C7 1.427(5) . ?
C6 C12 1.432(4) . ?
C7 C8 1.392(4) . ?
C7 C17 1.396(4) . ?
C9 C10 1.386(5) . ?
C9 H9 0.97(3) . ?
C10 C11 1.391(4) . ?
C10 C18 1.539(5) . ?
C11 C12 1.397(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.437(4) . ?
C13 C14 1.378(5) . ?
C13 C31 1.495(4) . ?
C14 C15 1.391(6) . ?
C14 C17 1.435(4) . ?
C14 C15A 1.489(10) . ?
C15 C16 1.381(7) . ?
C15 H15 0.9500 . ?
C15A C16 1.484(10) . ?
C16 C40 1.406(4) 2_775 ?
C18 C21 1.528(4) . ?
C18 C19 1.531(5) . ?
C18 C20 1.536(5) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C27 1.402(5) . ?
C22 C23 1.403(5) . ?
C23 C24 1.380(5) . ?
C23 C28 1.514(5) . ?
C24 C25 1.392(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.384(5) . ?
C25 C29 1.516(5) . ?
C26 C27 1.388(5) . ?
C26 H26 0.9500 . ?
C27 C30 1.511(5) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.397(5) . ?
C31 C36 1.411(5) . ?
C32 C33 1.391(5) . ?
C32 C37 1.504(5) . ?
C33 C34 1.393(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.384(5) . ?
C34 C38 1.509(5) . ?
C35 C36 1.391(5) . ?
C35 H35 0.9500 . ?
C36 C39 1.501(5) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 C16 1.406(4) 2_775 ?
C40 C41 1.493(4) . ?
C41 C46 1.377(4) . ?
C41 C42 1.402(4) . ?
C42 C43 1.376(4) . ?
C42 H42 0.9500 . ?
C43 C44 1.386(5) . ?
C43 C47 1.544(5) . ?
C44 C45 1.400(5) . ?
C44 H44 0.9500 . ?
C45 C46 1.395(4) . ?
C45 C51 1.529(5) . ?
C46 H46 0.9500 . ?
C47 C48 1.512(5) . ?
C47 C50 1.524(5) . ?
C47 C49 1.534(5) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C51 C54 1.530(5) . ?
C51 C53 1.531(5) . ?
C51 C52 1.533(5) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C1X C2X 1.380(7) . ?
C1X C6X 1.384(7) . ?
C1X C7X 1.473(7) . ?
C2X C3X 1.351(10) . ?
C2X H2X 0.9500 . ?
C3X C4X 1.371(11) . ?
C3X H3X 0.9500 . ?
C4X C5X 1.394(10) . ?
C4X H4X 0.9500 . ?
C5X C6X 1.384(7) . ?
C5X H5X 0.9500 . ?
C6X H6X 0.9500 . ?
C7X H7X1 0.9800 . ?
C7X H7X2 0.9800 . ?
C7X H7X3 0.9800 . ?
C1Y C6Y 1.374(6) . ?
C1Y C2Y 1.393(6) . ?
C1Y C7Y 1.503(6) . ?
C2Y C3Y 1.373(6) . ?
C2Y H2Y 0.9500 . ?
C3Y C4Y 1.369(7) . ?
C3Y H3Y 0.9500 . ?
C4Y C5Y 1.401(7) . ?
C4Y H4Y 0.9500 . ?
C5Y C6Y 1.380(6) . ?
C5Y H5Y 0.9500 . ?
C6Y H6Y 0.9500 . ?
C7Y H7Y1 0.9800 . ?
C7Y H7Y2 0.9800 . ?
C7Y H7Y3 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
N2 Ni1 N2 180.0 . 2_775 ?
N2 Ni1 N1 89.05(10) . 2_775 ?
N2 Ni1 N1 90.95(10) 2_775 2_775 ?
N2 Ni1 N1 90.95(10) . . ?
N2 Ni1 N1 89.05(10) 2_775 . ?
N1 Ni1 N1 180.0 2_775 . ?
C8 N1 C1 105.0(2) . . ?
C8 N1 Ni1 126.4(2) . . ?
C1 N1 Ni1 128.6(2) . . ?
C17 N2 C16 104.1(2) . . ?
C17 N2 Ni1 126.7(2) . . ?
C16 N2 Ni1 129.2(2) . . ?
C40 C1 C2A 127.0(6) . . ?
C40 C1 N1 125.9(3) . . ?
C2A C1 N1 107.0(6) . . ?
C40 C1 C2 121.5(3) . . ?
N1 C1 C2 112.6(3) . . ?
O1 C2 C3 128.7(4) . . ?
O1 C2 C1 129.3(4) . . ?
C3 C2 C1 101.6(4) . . ?
C3 C2A C1 112.5(11) . . ?
C3 C2A H2A 123.8 . . ?
C1 C2A H2A 123.8 . . ?
C4 C3 C2A 135.4(6) . . ?
C4 C3 C8 123.6(3) . . ?
C2A C3 C8 100.8(6) . . ?
C4 C3 C2 129.7(3) . . ?
C8 C3 C2 106.7(3) . . ?
C3 C4 C5 118.4(3) . . ?
C3 C4 C22 122.1(3) . . ?
C5 C4 C22 119.6(3) . . ?
C9 C5 C6 119.6(3) . . ?
C9 C5 C4 121.8(3) . . ?
C6 C5 C4 118.6(3) . . ?
C5 C6 C7 121.4(3) . . ?
C5 C6 C12 118.3(3) . . ?
C7 C6 C12 120.4(3) . . ?
C8 C7 C17 121.3(3) . . ?
C8 C7 C6 119.2(3) . . ?
C17 C7 C6 119.4(3) . . ?
N1 C8 C7 127.2(3) . . ?
N1 C8 C3 114.1(3) . . ?
C7 C8 C3 118.8(3) . . ?
C10 C9 C5 122.4(3) . . ?
C10 C9 H9 123(2) . . ?
C5 C9 H9 115(2) . . ?
C9 C10 C11 117.7(3) . . ?
C9 C10 C18 123.2(3) . . ?
C11 C10 C18 119.1(3) . . ?
C10 C11 C12 123.1(3) . . ?
C10 C11 H11 118.5 . . ?
C12 C11 H11 118.5 . . ?
C11 C12 C6 119.0(3) . . ?
C11 C12 C13 121.5(3) . . ?
C6 C12 C13 119.5(3) . . ?
C14 C13 C12 118.8(3) . . ?
C14 C13 C31 120.9(3) . . ?
C12 C13 C31 120.3(3) . . ?
C13 C14 C15 133.9(4) . . ?
C13 C14 C17 122.3(3) . . ?
C15 C14 C17 103.8(3) . . ?
C13 C14 C15A 128.7(5) . . ?
C17 C14 C15A 108.9(5) . . ?
C16 C15 C14 109.0(6) . . ?
C16 C15 H15 125.5 . . ?
C14 C15 H15 125.5 . . ?
O2 C15A C16 130.1(14) . . ?
O2 C15A C14 125.1(13) . . ?
C16 C15A C14 98.8(8) . . ?
C15 C16 C40 125.2(4) . 2_775 ?
C15 C16 N2 110.0(3) . . ?
C40 C16 N2 124.7(3) 2_775 . ?
C40 C16 C15A 120.1(5) 2_775 . ?
N2 C16 C15A 115.0(5) . . ?
N2 C17 C7 127.5(3) . . ?
N2 C17 C14 112.9(3) . . ?
C7 C17 C14 119.6(3) . . ?
C21 C18 C19 107.7(3) . . ?
C21 C18 C20 109.1(3) . . ?
C19 C18 C20 109.1(3) . . ?
C21 C18 C10 112.5(3) . . ?
C19 C18 C10 110.1(3) . . ?
C20 C18 C10 108.3(3) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C27 C22 C23 119.7(3) . . ?
C27 C22 C4 120.0(3) . . ?
C23 C22 C4 120.3(3) . . ?
C24 C23 C22 119.2(3) . . ?
C24 C23 C28 119.7(3) . . ?
C22 C23 C28 121.2(3) . . ?
C23 C24 C25 122.1(4) . . ?
C23 C24 H24 119.0 . . ?
C25 C24 H24 119.0 . . ?
C26 C25 C24 117.9(3) . . ?
C26 C25 C29 121.3(4) . . ?
C24 C25 C29 120.7(4) . . ?
C25 C26 C27 121.9(4) . . ?
C25 C26 H26 119.0 . . ?
C27 C26 H26 119.0 . . ?
C26 C27 C22 119.1(3) . . ?
C26 C27 C30 120.1(3) . . ?
C22 C27 C30 120.8(3) . . ?
C23 C28 H28A 109.5 . . ?
C23 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C23 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C25 C29 H29A 109.5 . . ?
C25 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C25 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32 C31 C36 120.4(3) . . ?
C32 C31 C13 119.6(3) . . ?
C36 C31 C13 119.9(3) . . ?
C33 C32 C31 118.5(3) . . ?
C33 C32 C37 119.7(3) . . ?
C31 C32 C37 121.8(3) . . ?
C32 C33 C34 122.3(3) . . ?
C32 C33 H33 118.8 . . ?
C34 C33 H33 118.8 . . ?
C35 C34 C33 118.0(3) . . ?
C35 C34 C38 120.7(4) . . ?
C33 C34 C38 121.2(4) . . ?
C34 C35 C36 121.9(3) . . ?
C34 C35 H35 119.0 . . ?
C36 C35 H35 119.0 . . ?
C35 C36 C31 118.7(3) . . ?
C35 C36 C39 119.4(3) . . ?
C31 C36 C39 121.9(3) . . ?
C32 C37 H37A 109.5 . . ?
C32 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C32 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C34 C38 H38A 109.5 . . ?
C34 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C34 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C36 C39 H39A 109.5 . . ?
C36 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C36 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C1 C40 C16 122.4(3) . 2_775 ?
C1 C40 C41 120.2(3) . . ?
C16 C40 C41 117.3(3) 2_775 . ?
C46 C41 C42 119.3(3) . . ?
C46 C41 C40 121.7(3) . . ?
C42 C41 C40 118.8(3) . . ?
C43 C42 C41 121.2(3) . . ?
C43 C42 H42 119.4 . . ?
C41 C42 H42 119.4 . . ?
C42 C43 C44 118.1(3) . . ?
C42 C43 C47 121.7(3) . . ?
C44 C43 C47 120.1(3) . . ?
C43 C44 C45 122.6(3) . . ?
C43 C44 H44 118.7 . . ?
C45 C44 H44 118.7 . . ?
C46 C45 C44 117.5(3) . . ?
C46 C45 C51 119.7(3) . . ?
C44 C45 C51 122.8(3) . . ?
C41 C46 C45 121.3(3) . . ?
C41 C46 H46 119.3 . . ?
C45 C46 H46 119.3 . . ?
C48 C47 C50 108.3(3) . . ?
C48 C47 C49 107.8(3) . . ?
C50 C47 C49 109.5(3) . . ?
C48 C47 C43 112.6(3) . . ?
C50 C47 C43 111.2(3) . . ?
C49 C47 C43 107.3(3) . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C47 C50 H50A 109.5 . . ?
C47 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C47 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C47 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C45 C51 C54 109.3(3) . . ?
C45 C51 C53 110.3(3) . . ?
C54 C51 C53 108.2(3) . . ?
C45 C51 C52 112.7(3) . . ?
C54 C51 C52 108.5(3) . . ?
C53 C51 C52 107.8(3) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C2X C1X C6X 118.9(6) . . ?
C2X C1X C7X 119.8(6) . . ?
C6X C1X C7X 121.3(4) . . ?
C3X C2X C1X 120.1(8) . . ?
C3X C2X H2X 120.0 . . ?
C1X C2X H2X 120.0 . . ?
C2X C3X C4X 121.5(7) . . ?
C2X C3X H3X 119.2 . . ?
C4X C3X H3X 119.2 . . ?
C3X C4X C5X 120.0(6) . . ?
C3X C4X H4X 120.0 . . ?
C5X C4X H4X 120.0 . . ?
C6X C5X C4X 117.8(7) . . ?
C6X C5X H5X 121.1 . . ?
C4X C5X H5X 121.1 . . ?
C5X C6X C1X 121.6(6) . . ?
C5X C6X H6X 119.2 . . ?
C1X C6X H6X 119.2 . . ?
C1X C7X H7X1 109.5 . . ?
C1X C7X H7X2 109.5 . . ?
H7X1 C7X H7X2 109.5 . . ?
C1X C7X H7X3 109.5 . . ?
H7X1 C7X H7X3 109.5 . . ?
H7X2 C7X H7X3 109.5 . . ?
C6Y C1Y C2Y 117.4(4) . . ?
C6Y C1Y C7Y 120.4(4) . . ?
C2Y C1Y C7Y 122.2(4) . . ?
C3Y C2Y C1Y 121.1(4) . . ?
C3Y C2Y H2Y 119.4 . . ?
C1Y C2Y H2Y 119.4 . . ?
C4Y C3Y C2Y 120.7(4) . . ?
C4Y C3Y H3Y 119.7 . . ?
C2Y C3Y H3Y 119.7 . . ?
C3Y C4Y C5Y 119.5(4) . . ?
C3Y C4Y H4Y 120.2 . . ?
C5Y C4Y H4Y 120.2 . . ?
C6Y C5Y C4Y 118.6(4) . . ?
C6Y C5Y H5Y 120.7 . . ?
C4Y C5Y H5Y 120.7 . . ?
C1Y C6Y C5Y 122.6(5) . . ?
C1Y C6Y H6Y 118.7 . . ?
C5Y C6Y H6Y 118.7 . . ?
C1Y C7Y H7Y1 109.5 . . ?
C1Y C7Y H7Y2 109.5 . . ?
H7Y1 C7Y H7Y2 109.5 . . ?
C1Y C7Y H7Y3 109.5 . . ?
H7Y1 C7Y H7Y3 109.5 . . ?
H7Y2 C7Y H7Y3 109.5 . . ?

_refine_diff_density_max         0.985
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.083

_shelxl_version_number           2013-4



####################################################################### 
# 
# 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_E248
_database_code_depnum_ccdc_archive 'CCDC 1019262'
_audit_update_record             
;
2014-08-13 deposited with the CCDC.
2015-02-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C85.50 H87 N5 Ni'
_chemical_formula_weight         1243.31

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'
Ni Ni 0.3393 1.1124 '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                   15.0498(12)
_cell_length_b                   15.6708(13)
_cell_length_c                   17.4668(15)
_cell_angle_alpha                111.901(3)
_cell_angle_beta                 107.076(3)
_cell_angle_gamma                102.416(3)
_cell_volume                     3400.2(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9557
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      27.90

_exptl_crystal_description       Needle
_exptl_crystal_colour            Dark_Red
_exptl_crystal_density_meas      'Not Measured'
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_F_000             1326
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    0.336
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7138
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'Sadabs, (Sheldrick 2012)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            123595
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.118
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             12000
_reflns_number_gt                10101
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0476P)²+4.6525P] 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         12000
_refine_ls_number_parameters     893
_refine_ls_number_restraints     71
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0423
_refine_ls_wR_factor_ref         0.1095
_refine_ls_wR_factor_gt          0.1027
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_restrained_S_all      1.015
_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
C28 C 1.0762(7) 0.1197(3) 0.5249(5) 0.0285(13) Uani 0.482(7) 1 d D U P A 1
H28A H 1.0526 0.1180 0.5712 0.043 Uiso 0.482(7) 1 calc R U P A 1
H28B H 1.1242 0.0863 0.5232 0.043 Uiso 0.482(7) 1 calc R U P A 1
H28C H 1.0193 0.0859 0.4656 0.043 Uiso 0.482(7) 1 calc R U P A 1
C29 C 1.2168(5) 0.2795(6) 0.6393(4) 0.0503(16) Uani 0.482(7) 1 d D U P A 1
H29A H 1.2518 0.3468 0.6515 0.075 Uiso 0.482(7) 1 calc R U P A 1
H29B H 1.2623 0.2431 0.6379 0.075 Uiso 0.482(7) 1 calc R U P A 1
H29C H 1.1942 0.2825 0.6871 0.075 Uiso 0.482(7) 1 calc R U P A 1
C30 C 1.1645(6) 0.2248(5) 0.4739(4) 0.0319(11) Uani 0.482(7) 1 d D U P A 1
H30A H 1.1078 0.1896 0.4145 0.048 Uiso 0.482(7) 1 calc R U P A 1
H30B H 1.2121 0.1909 0.4741 0.048 Uiso 0.482(7) 1 calc R U P A 1
H30C H 1.1975 0.2926 0.4864 0.048 Uiso 0.482(7) 1 calc R U P A 1
C28A C 1.0655(6) 0.1155(3) 0.4965(5) 0.0304(12) Uani 0.518(7) 1 d D U P A 2
H28D H 1.0223 0.0994 0.5255 0.046 Uiso 0.518(7) 1 calc R U P A 2
H28E H 1.1109 0.0791 0.4977 0.046 Uiso 0.518(7) 1 calc R U P A 2
H28F H 1.0244 0.0969 0.4336 0.046 Uiso 0.518(7) 1 calc R U P A 2
C29A C 1.1837(6) 0.2530(6) 0.6481(3) 0.0474(15) Uani 0.518(7) 1 d D U P A 2
H29D H 1.2155 0.3249 0.6850 0.071 Uiso 0.518(7) 1 calc R U P A 2
H29E H 1.2349 0.2233 0.6528 0.071 Uiso 0.518(7) 1 calc R U P A 2
H29F H 1.1367 0.2271 0.6700 0.071 Uiso 0.518(7) 1 calc R U P A 2
C30A C 1.2039(5) 0.2536(5) 0.5129(5) 0.0326(11) Uani 0.518(7) 1 d D U P A 2
H30D H 1.1702 0.2400 0.4501 0.049 Uiso 0.518(7) 1 calc R U P A 2
H30E H 1.2462 0.2142 0.5158 0.049 Uiso 0.518(7) 1 calc R U P A 2
H30F H 1.2455 0.3240 0.5505 0.049 Uiso 0.518(7) 1 calc R U P A 2
N1X N 0.1472(3) 0.9442(3) 0.7059(2) 0.0634(10) Uani 0.865(3) 1 d D . P B 1
C1X C 0.1162(2) 0.8688(3) 0.7017(2) 0.0371(8) Uani 0.865(3) 1 d D . P B 1
C2X C 0.0786(12) 0.7746(7) 0.6973(8) 0.0444(14) Uani 0.865(3) 1 d D . P B 1
H2X1 H 0.0491 0.7231 0.6341 0.067 Uiso 0.865(3) 1 calc R U P B 1
H2X2 H 0.0275 0.7736 0.7214 0.067 Uiso 0.865(3) 1 calc R U P B 1
H2X3 H 0.1333 0.7625 0.7332 0.067 Uiso 0.865(3) 1 calc R U P B 1
C1Y C 0.0715(15) 0.8445(15) 0.7630(13) 0.0371(8) Uani 0.135(3) 1 d D . P B 2
N1Y N 0.0564(17) 0.9023(14) 0.8158(14) 0.0634(10) Uani 0.135(3) 1 d D . P B 2
C2Y C 0.069(8) 0.765(5) 0.687(5) 0.0444(14) Uani 0.135(3) 1 d D . P B 2
H2Y1 H 0.0040 0.7382 0.6359 0.067 Uiso 0.135(3) 1 calc R U P B 2
H2Y2 H 0.0784 0.7125 0.7029 0.067 Uiso 0.135(3) 1 calc R U P B 2
H2Y3 H 0.1222 0.7885 0.6704 0.067 Uiso 0.135(3) 1 calc R U P B 2
C1S C 0.0687(4) 0.4886(3) 0.9686(3) 0.0601(14) Uani 0.5 1 d G . P C -1
C2S C 0.1662(3) 0.4996(3) 0.9784(3) 0.0676(17) Uani 0.5 1 d G . P C -1
H2S H 0.2190 0.5320 1.0372 0.081 Uiso 0.5 1 calc R U P C -1
C3S C 0.1863(3) 0.4633(3) 0.9023(4) 0.067(2) Uani 0.5 1 d G . P C -1
H3S H 0.2529 0.4708 0.9090 0.080 Uiso 0.5 1 calc R U P C -1
C4S C 0.1090(4) 0.4159(3) 0.8163(3) 0.0601(14) Uani 0.5 1 d G . P C -1
H4S H 0.1228 0.3911 0.7642 0.072 Uiso 0.5 1 calc R U P C -1
C5S C 0.0115(4) 0.4049(3) 0.8064(3) 0.0676(17) Uani 0.5 1 d G . P C -1
H5S H -0.0413 0.3725 0.7476 0.081 Uiso 0.5 1 calc R U P C -1
C6S C -0.0086(3) 0.4412(3) 0.8825(4) 0.077(3) Uani 0.5 1 d G . P C -1
H6S H -0.0753 0.4337 0.8758 0.093 Uiso 0.5 1 calc R U P C -1
C7S C 0.0405(7) 0.5221(5) 1.0437(5) 0.071(2) Uani 0.5 1 d . . P C -1
H7S1 H 0.0847 0.5168 1.0942 0.106 Uiso 0.5 1 calc R U P C -1
H7S2 H -0.0287 0.4810 1.0249 0.106 Uiso 0.5 1 calc R U P C -1
H7S3 H 0.0464 0.5911 1.0630 0.106 Uiso 0.5 1 calc R U P C -1
Ni1 Ni 0.72198(2) 0.59837(2) 0.59057(2) 0.01103(8) Uani 1 1 d . . . . .
N1 N 0.84070(13) 0.59748(12) 0.67243(11) 0.0137(4) Uani 1 1 d . . . . .
N2 N 0.71542(12) 0.48113(12) 0.49246(11) 0.0124(4) Uani 1 1 d . . . . .
N3 N 0.60683(12) 0.60256(12) 0.50758(11) 0.0124(4) Uani 1 1 d . . . . .
N4 N 0.72659(12) 0.71351(12) 0.68904(11) 0.0128(4) Uani 1 1 d . . . . .
C1 C 0.88807(16) 0.65441(15) 0.76522(14) 0.0155(4) Uani 1 1 d . . . . .
C2 C 0.97576(16) 0.63496(16) 0.80125(15) 0.0187(5) Uani 1 1 d . . . . .
H2 H 1.0211 0.6653 0.8631 0.022 Uiso 1 1 calc R U . . .
C3 C 0.98148(16) 0.56551(16) 0.73082(15) 0.0200(5) Uani 1 1 d . . . . .
H3 H 1.0322 0.5382 0.7335 0.024 Uiso 1 1 calc R U . . .
C4 C 0.89692(15) 0.54031(15) 0.65109(14) 0.0150(4) Uani 1 1 d . . . . .
C5 C 0.87043(15) 0.46127(15) 0.56731(14) 0.0145(4) Uani 1 1 d . . . . .
C6 C 0.78263(15) 0.43279(15) 0.49324(14) 0.0125(4) Uani 1 1 d . . . . .
C7 C 0.75034(15) 0.34971(15) 0.40643(14) 0.0147(4) Uani 1 1 d . . . . .
H7 H 0.7839 0.3056 0.3901 0.018 Uiso 1 1 calc R U . . .
C8 C 0.66258(15) 0.34616(15) 0.35195(14) 0.0133(4) Uani 1 1 d . . . . .
C9 C 0.64246(15) 0.42764(15) 0.40509(14) 0.0123(4) Uani 1 1 d . . . . .
C10 C 0.56237(15) 0.45099(15) 0.36705(14) 0.0123(4) Uani 1 1 d . . . . .
C11 C 0.54981(15) 0.53587(15) 0.41765(13) 0.0120(4) Uani 1 1 d . . . . .
C12 C 0.47815(15) 0.56918(15) 0.37566(14) 0.0131(4) Uani 1 1 d . . . . .
C13 C 0.49327(15) 0.65925(15) 0.43952(14) 0.0141(4) Uani 1 1 d . . . . .
H13 H 0.4593 0.7018 0.4314 0.017 Uiso 1 1 calc R U . . .
C14 C 0.57021(15) 0.67834(15) 0.52173(14) 0.0135(4) Uani 1 1 d . . . . .
C15 C 0.59876(15) 0.75950(15) 0.60509(14) 0.0128(4) Uani 1 1 d . . . . .
C16 C 0.66867(15) 0.77060(15) 0.68401(14) 0.0137(4) Uani 1 1 d . . . . .
C17 C 0.68698(16) 0.84177(16) 0.77299(14) 0.0161(4) Uani 1 1 d . . . . .
H17 H 0.6567 0.8895 0.7872 0.019 Uiso 1 1 calc R U . . .
C18 C 0.75511(16) 0.82826(16) 0.83256(14) 0.0159(4) Uani 1 1 d . . . . .
H18 H 0.7807 0.8634 0.8967 0.019 Uiso 1 1 calc R U . . .
C19 C 0.78178(15) 0.75078(15) 0.78080(14) 0.0141(4) Uani 1 1 d . . . . .
C20 C 0.85806(15) 0.72282(15) 0.81864(14) 0.0144(4) Uani 1 1 d . . . . .
C21 C 0.93508(15) 0.40087(15) 0.55914(14) 0.0141(4) Uani 1 1 d . . . . .
C22 C 1.03032(16) 0.43758(16) 0.56366(15) 0.0181(5) Uani 1 1 d . . . . .
H22 H 1.0550 0.5023 0.5706 0.022 Uiso 1 1 calc R U . . .
C23 C 1.08977(16) 0.38095(16) 0.55820(15) 0.0196(5) Uani 1 1 d . . . . .
H23 H 1.1543 0.4078 0.5610 0.024 Uiso 1 1 calc R U . . .
C24 C 1.05753(16) 0.28587(16) 0.54873(14) 0.0173(5) Uani 1 1 d . . . . .
C25 C 0.96222(17) 0.24967(16) 0.54432(16) 0.0210(5) Uani 1 1 d . . . . .
H25 H 0.9375 0.1849 0.5374 0.025 Uiso 1 1 calc R U . . .
C26 C 0.90245(16) 0.30603(16) 0.54974(15) 0.0196(5) Uani 1 1 d . . . . .
H26 H 0.8380 0.2793 0.5470 0.024 Uiso 1 1 calc R U . . .
C27 C 1.12662(15) 0.22681(15) 0.54782(15) 0.0254(5) Uani 1 1 d D . . . .
C31 C 0.59013(15) 0.27124(15) 0.25701(14) 0.0147(4) Uani 1 1 d . . . . .
H31 H 0.5513 0.2148 0.2622 0.018 Uiso 1 1 calc R U . . .
C32 C 0.63953(15) 0.22767(16) 0.19498(14) 0.0157(4) Uani 1 1 d . . . . .
C33 C 0.70252(16) 0.28871(17) 0.17563(15) 0.0195(5) Uani 1 1 d . . . . .
C34 C 0.74375(17) 0.24666(18) 0.11614(15) 0.0231(5) Uani 1 1 d . . . . .
H34 H 0.7871 0.2884 0.1039 0.028 Uiso 1 1 calc R U . . .
C35 C 0.72351(18) 0.14593(19) 0.07424(16) 0.0260(5) Uani 1 1 d . . . . .
C36 C 0.6596(2) 0.08671(18) 0.09310(16) 0.0282(6) Uani 1 1 d . . . . .
H36 H 0.6445 0.0174 0.0646 0.034 Uiso 1 1 calc R U . . .
C37 C 0.61681(18) 0.12535(17) 0.15249(15) 0.0219(5) Uani 1 1 d . . . . .
C38 C 0.72540(19) 0.39842(18) 0.21499(18) 0.0296(6) Uani 1 1 d . . . . .
H38A H 0.6629 0.4105 0.1991 0.044 Uiso 1 1 calc R U . . .
H38B H 0.7674 0.4266 0.1904 0.044 Uiso 1 1 calc R U . . .
H38C H 0.7608 0.4295 0.2811 0.044 Uiso 1 1 calc R U . . .
C39 C 0.7696(2) 0.1021(2) 0.0104(2) 0.0403(7) Uani 1 1 d . . . . .
H39A H 0.8162 0.0757 0.0373 0.060 Uiso 1 1 calc R U . . .
H39B H 0.8056 0.1535 -0.0003 0.060 Uiso 1 1 calc R U . . .
H39C H 0.7169 0.0487 -0.0472 0.060 Uiso 1 1 calc R U . . .
C40 C 0.5450(2) 0.05552(17) 0.16698(18) 0.0340(6) Uani 1 1 d . . . . .
H40A H 0.5400 -0.0123 0.1323 0.051 Uiso 1 1 calc R U . . .
H40B H 0.4791 0.0601 0.1465 0.051 Uiso 1 1 calc R U . . .
H40C H 0.5696 0.0735 0.2315 0.051 Uiso 1 1 calc R U . . .
C41 C 0.51363(15) 0.30907(15) 0.21538(14) 0.0144(4) Uani 1 1 d . . . . .
C42 C 0.45888(15) 0.25921(15) 0.12236(14) 0.0158(4) Uani 1 1 d . . . . .
H42 H 0.4699 0.2027 0.0875 0.019 Uiso 1 1 calc R U . . .
C43 C 0.38817(15) 0.28876(15) 0.07798(14) 0.0150(4) Uani 1 1 d . . . . .
C44 C 0.37076(15) 0.36862(15) 0.13236(14) 0.0152(4) Uani 1 1 d . . . . .
H44 H 0.3202 0.3882 0.1045 0.018 Uiso 1 1 calc R U . . .
C45 C 0.42449(15) 0.42090(15) 0.22585(14) 0.0142(4) Uani 1 1 d . . . . .
C46 C 0.49805(15) 0.39205(15) 0.26908(14) 0.0133(4) Uani 1 1 d . . . . .
C47 C 0.33518(16) 0.23535(16) -0.02562(14) 0.0186(5) Uani 1 1 d . . . . .
C48 C 0.40701(19) 0.2036(2) -0.06665(16) 0.0281(6) Uani 1 1 d . . . . .
H48A H 0.4678 0.2611 -0.0422 0.042 Uiso 1 1 calc R U . . .
H48B H 0.3748 0.1760 -0.1326 0.042 Uiso 1 1 calc R U . . .
H48C H 0.4243 0.1535 -0.0513 0.042 Uiso 1 1 calc R U . . .
C49 C 0.24596(17) 0.14288(17) -0.05616(15) 0.0236(5) Uani 1 1 d . . . . .
H49A H 0.2147 0.1061 -0.1225 0.035 Uiso 1 1 calc R U . . .
H49B H 0.1971 0.1626 -0.0340 0.035 Uiso 1 1 calc R U . . .
H49C H 0.2690 0.1009 -0.0315 0.035 Uiso 1 1 calc R U . . .
C50 C 0.29874(18) 0.30222(18) -0.06217(15) 0.0250(5) Uani 1 1 d . . . . .
H50A H 0.3552 0.3629 -0.0400 0.038 Uiso 1 1 calc R U . . .
H50B H 0.2480 0.3190 -0.0414 0.038 Uiso 1 1 calc R U . . .
H50C H 0.2697 0.2676 -0.1285 0.038 Uiso 1 1 calc R U . . .
C51 C 0.40306(15) 0.50986(15) 0.27894(14) 0.0138(4) Uani 1 1 d . . . . .
H51 H 0.3380 0.4824 0.2812 0.017 Uiso 1 1 calc R U . . .
C52 C 0.38845(16) 0.57817(15) 0.23625(14) 0.0150(4) Uani 1 1 d . . . . .
C53 C 0.45267(17) 0.60805(16) 0.19918(15) 0.0194(5) Uani 1 1 d . . . . .
C54 C 0.4355(2) 0.66957(18) 0.16074(16) 0.0274(6) Uani 1 1 d . . . . .
H54 H 0.4776 0.6874 0.1336 0.033 Uiso 1 1 calc R U . . .
C55 C 0.3593(2) 0.70580(18) 0.16054(16) 0.0287(6) Uani 1 1 d . . . . .
C56 C 0.30054(18) 0.68066(17) 0.20231(16) 0.0251(5) Uani 1 1 d . . . . .
H56 H 0.2499 0.7074 0.2055 0.030 Uiso 1 1 calc R U . . .
C57 C 0.31316(16) 0.61732(16) 0.23997(14) 0.0188(5) Uani 1 1 d . . . . .
C58 C 0.54246(18) 0.57908(18) 0.20129(17) 0.0261(5) Uani 1 1 d . . . . .
H58A H 0.5736 0.5782 0.2586 0.039 Uiso 1 1 calc R U . . .
H58B H 0.5907 0.6270 0.1958 0.039 Uiso 1 1 calc R U . . .
H58C H 0.5213 0.5132 0.1507 0.039 Uiso 1 1 calc R U . . .
C59 C 0.3422(3) 0.7729(2) 0.1183(2) 0.0450(8) Uani 1 1 d . . . . .
H59A H 0.3745 0.8419 0.1655 0.068 Uiso 1 1 calc R U . . .
H59B H 0.2703 0.7573 0.0887 0.068 Uiso 1 1 calc R U . . .
H59C H 0.3708 0.7628 0.0733 0.068 Uiso 1 1 calc R U . . .
C60 C 0.24584(17) 0.59466(17) 0.28477(17) 0.0241(5) Uani 1 1 d . . . . .
H60A H 0.2117 0.6418 0.2947 0.036 Uiso 1 1 calc R U . . .
H60B H 0.2859 0.6001 0.3430 0.036 Uiso 1 1 calc R U . . .
H60C H 0.1962 0.5274 0.2456 0.036 Uiso 1 1 calc R U . . .
C61 C 0.54811(15) 0.83239(15) 0.60919(13) 0.0137(4) Uani 1 1 d . . . . .
C62 C 0.60124(16) 0.93190(16) 0.64105(14) 0.0169(5) Uani 1 1 d . . . . .
H62 H 0.6721 0.9555 0.6650 0.020 Uiso 1 1 calc R U . . .
C63 C 0.55255(16) 0.99763(16) 0.63852(15) 0.0182(5) Uani 1 1 d . . . . .
H63 H 0.5910 1.0650 0.6601 0.022 Uiso 1 1 calc R U . . .
C64 C 0.44911(16) 0.96716(16) 0.60518(14) 0.0164(5) Uani 1 1 d . . . . .
C65 C 0.39660(16) 0.86799(16) 0.57714(14) 0.0173(5) Uani 1 1 d . . . . .
H65 H 0.3260 0.8452 0.5567 0.021 Uiso 1 1 calc R U . . .
C66 C 0.44447(16) 0.80220(15) 0.57832(14) 0.0152(4) Uani 1 1 d . . . . .
H66 H 0.4061 0.7351 0.5577 0.018 Uiso 1 1 calc R U . . .
C67 C 0.39317(17) 1.03738(17) 0.59970(16) 0.0218(5) Uani 1 1 d . . . . .
C68 C 0.3667(2) 1.0710(2) 0.6820(2) 0.0378(7) Uani 1 1 d . . . . .
H68A H 0.3220 1.0136 0.6796 0.057 Uiso 1 1 calc R U . . .
H68B H 0.3333 1.1181 0.6810 0.057 Uiso 1 1 calc R U . . .
H68C H 0.4279 1.1029 0.7379 0.057 Uiso 1 1 calc R U . . .
C69 C 0.45622(18) 1.12846(17) 0.60026(16) 0.0243(5) Uani 1 1 d . . . . .
H69A H 0.5147 1.1677 0.6584 0.036 Uiso 1 1 calc R U . . .
H69B H 0.4162 1.1686 0.5918 0.036 Uiso 1 1 calc R U . . .
H69C H 0.4782 1.1075 0.5510 0.036 Uiso 1 1 calc R U . . .
C70 C 0.29742(18) 0.9843(2) 0.51201(19) 0.0329(6) Uani 1 1 d . . . . .
H70A H 0.3139 0.9563 0.4600 0.049 Uiso 1 1 calc R U . . .
H70B H 0.2659 1.0315 0.5063 0.049 Uiso 1 1 calc R U . . .
H70C H 0.2512 0.9310 0.5137 0.049 Uiso 1 1 calc R U . . .
C71 C 0.91132(15) 0.76733(16) 0.91938(14) 0.0158(4) Uani 1 1 d . . . . .
C72 C 0.96975(16) 0.86714(16) 0.97333(15) 0.0180(5) Uani 1 1 d . . . . .
H72 H 0.9766 0.9089 0.9459 0.022 Uiso 1 1 calc R U . . .
C73 C 1.01850(16) 0.90693(17) 1.06699(15) 0.0198(5) Uani 1 1 d . . . . .
H73 H 1.0580 0.9754 1.1022 0.024 Uiso 1 1 calc R U . . .
C74 C 1.01069(16) 0.84881(17) 1.11015(15) 0.0197(5) Uani 1 1 d . . . . .
C75 C 0.95449(16) 0.74817(17) 1.05525(15) 0.0213(5) Uani 1 1 d . . . . .
H75 H 0.9495 0.7061 1.0825 0.026 Uiso 1 1 calc R U . . .
C76 C 0.90587(16) 0.70792(17) 0.96221(15) 0.0186(5) Uani 1 1 d . . . . .
H76 H 0.8683 0.6390 0.9269 0.022 Uiso 1 1 calc R U . . .
C77 C 1.06283(17) 0.89074(19) 1.21324(15) 0.0258(5) Uani 1 1 d . . . . .
C78 C 1.10929(19) 1.0038(2) 1.26201(16) 0.0330(6) Uani 1 1 d . . . . .
H78A H 1.1594 1.0255 1.2411 0.049 Uiso 1 1 calc R U . . .
H78B H 1.1412 1.0275 1.3275 0.049 Uiso 1 1 calc R U . . .
H78C H 1.0570 1.0307 1.2486 0.049 Uiso 1 1 calc R U . . .
C79 C 0.9875(2) 0.8606(2) 1.25031(17) 0.0379(7) Uani 1 1 d . . . . .
H79A H 0.9353 0.8877 1.2374 0.057 Uiso 1 1 calc R U . . .
H79B H 1.0219 0.8865 1.3159 0.057 Uiso 1 1 calc R U . . .
H79C H 0.9573 0.7884 1.2213 0.057 Uiso 1 1 calc R U . . .
C80 C 1.14511(19) 0.8492(2) 1.23381(17) 0.0351(6) Uani 1 1 d . . . . .
H80A H 1.1154 0.7769 1.2050 0.053 Uiso 1 1 calc R U . . .
H80B H 1.1795 0.8754 1.2995 0.053 Uiso 1 1 calc R U . . .
H80C H 1.1931 0.8687 1.2102 0.053 Uiso 1 1 calc R U . . .


_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
C28 C27 1.526(4) . ?
C29 C27 1.529(4) . ?
C30 C27 1.550(4) . ?
C28A C27 1.533(4) . ?
C29A C27 1.551(4) . ?
C30A C27 1.516(3) . ?
N1X C1X 1.140(4) . ?
C1X C2X 1.426(15) . ?
C1Y N1Y 1.145(11) . ?
C1Y C2Y 1.426(17) . ?
C1S C2S 1.3900 . ?
C1S C6S 1.3900 . ?
C1S C7S 1.445(9) . ?
C2S C3S 1.3900 . ?
C3S C4S 1.3900 . ?
C4S C5S 1.3900 . ?
C5S C6S 1.3900 . ?
Ni1 N3 1.9374(17) . ?
Ni1 N1 1.9395(17) . ?
Ni1 N4 1.9441(17) . ?
Ni1 N2 1.9483(17) . ?
N1 C1 1.378(3) . ?
N1 C4 1.386(3) . ?
N2 C9 1.379(3) . ?
N2 C6 1.388(3) . ?
N3 C11 1.376(3) . ?
N3 C14 1.385(3) . ?
N4 C19 1.382(3) . ?
N4 C16 1.385(3) . ?
C1 C20 1.390(3) . ?
C1 C2 1.435(3) . ?
C2 C3 1.345(3) . ?
C3 C4 1.431(3) . ?
C4 C5 1.388(3) . ?
C5 C6 1.389(3) . ?
C5 C21 1.496(3) . ?
C6 C7 1.433(3) . ?
C7 C8 1.358(3) . ?
C8 C9 1.425(3) . ?
C8 C31 1.501(3) . ?
C9 C10 1.389(3) . ?
C10 C11 1.384(3) . ?
C10 C46 1.477(3) . ?
C11 C12 1.427(3) . ?
C12 C13 1.352(3) . ?
C12 C51 1.500(3) . ?
C13 C14 1.430(3) . ?
C14 C15 1.392(3) . ?
C15 C16 1.389(3) . ?
C15 C61 1.495(3) . ?
C16 C17 1.435(3) . ?
C17 C18 1.345(3) . ?
C18 C19 1.434(3) . ?
C19 C20 1.391(3) . ?
C20 C71 1.497(3) . ?
C21 C26 1.391(3) . ?
C21 C22 1.392(3) . ?
C22 C23 1.388(3) . ?
C23 C24 1.393(3) . ?
C24 C25 1.392(3) . ?
C24 C27 1.533(3) . ?
C25 C26 1.388(3) . ?
C31 C41 1.526(3) . ?
C31 C32 1.527(3) . ?
C32 C37 1.402(3) . ?
C32 C33 1.403(3) . ?
C33 C34 1.394(3) . ?
C33 C38 1.507(3) . ?
C34 C35 1.386(3) . ?
C35 C36 1.387(4) . ?
C35 C39 1.511(3) . ?
C36 C37 1.396(3) . ?
C37 C40 1.512(3) . ?
C41 C42 1.385(3) . ?
C41 C46 1.406(3) . ?
C42 C43 1.394(3) . ?
C43 C44 1.392(3) . ?
C43 C47 1.532(3) . ?
C44 C45 1.390(3) . ?
C45 C46 1.407(3) . ?
C45 C51 1.520(3) . ?
C47 C50 1.532(3) . ?
C47 C48 1.533(3) . ?
C47 C49 1.534(3) . ?
C51 C52 1.533(3) . ?
C52 C53 1.404(3) . ?
C52 C57 1.406(3) . ?
C53 C54 1.391(3) . ?
C53 C58 1.510(3) . ?
C54 C55 1.385(4) . ?
C55 C56 1.383(4) . ?
C55 C59 1.516(3) . ?
C56 C57 1.396(3) . ?
C57 C60 1.511(3) . ?
C61 C62 1.391(3) . ?
C61 C66 1.395(3) . ?
C62 C63 1.393(3) . ?
C63 C64 1.390(3) . ?
C64 C65 1.399(3) . ?
C64 C67 1.536(3) . ?
C65 C66 1.382(3) . ?
C67 C69 1.530(3) . ?
C67 C70 1.534(3) . ?
C67 C68 1.538(3) . ?
C71 C72 1.389(3) . ?
C71 C76 1.398(3) . ?
C72 C73 1.393(3) . ?
C73 C74 1.389(3) . ?
C74 C75 1.394(3) . ?
C74 C77 1.535(3) . ?
C75 C76 1.383(3) . ?
C77 C78 1.531(4) . ?
C77 C80 1.532(3) . ?
C77 C79 1.535(4) . ?

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
N1X C1X C2X 179.3(8) . . ?
N1Y C1Y C2Y 168(5) . . ?
C2S C1S C6S 120.0 . . ?
C2S C1S C7S 123.8(5) . . ?
C6S C1S C7S 116.2(5) . . ?
C1S C2S C3S 120.0 . . ?
C4S C3S C2S 120.0 . . ?
C3S C4S C5S 120.0 . . ?
C6S C5S C4S 120.0 . . ?
C5S C6S C1S 120.0 . . ?
N3 Ni1 N1 177.68(7) . . ?
N3 Ni1 N4 89.78(7) . . ?
N1 Ni1 N4 90.30(7) . . ?
N3 Ni1 N2 90.21(7) . . ?
N1 Ni1 N2 89.76(7) . . ?
N4 Ni1 N2 178.75(7) . . ?
C1 N1 C4 104.68(17) . . ?
C1 N1 Ni1 127.32(14) . . ?
C4 N1 Ni1 127.99(14) . . ?
C9 N2 C6 103.97(16) . . ?
C9 N2 Ni1 127.44(14) . . ?
C6 N2 Ni1 128.59(14) . . ?
C11 N3 C14 104.00(16) . . ?
C11 N3 Ni1 127.61(13) . . ?
C14 N3 Ni1 128.01(14) . . ?
C19 N4 C16 104.41(16) . . ?
C19 N4 Ni1 127.39(14) . . ?
C16 N4 Ni1 127.93(14) . . ?
N1 C1 C20 126.13(19) . . ?
N1 C1 C2 110.65(18) . . ?
C20 C1 C2 123.21(19) . . ?
C3 C2 C1 106.93(19) . . ?
C2 C3 C4 107.28(19) . . ?
N1 C4 C5 125.80(19) . . ?
N1 C4 C3 110.39(18) . . ?
C5 C4 C3 123.37(19) . . ?
C4 C5 C6 121.99(19) . . ?
C4 C5 C21 118.46(18) . . ?
C6 C5 C21 119.39(18) . . ?
N2 C6 C5 125.07(19) . . ?
N2 C6 C7 110.87(17) . . ?
C5 C6 C7 124.05(19) . . ?
C8 C7 C6 106.86(18) . . ?
C7 C8 C9 106.59(18) . . ?
C7 C8 C31 131.04(19) . . ?
C9 C8 C31 122.19(18) . . ?
N2 C9 C10 126.74(19) . . ?
N2 C9 C8 111.70(17) . . ?
C10 C9 C8 121.34(19) . . ?
C11 C10 C9 120.37(19) . . ?
C11 C10 C46 119.57(18) . . ?
C9 C10 C46 119.58(18) . . ?
N3 C11 C10 127.28(18) . . ?
N3 C11 C12 111.62(17) . . ?
C10 C11 C12 120.78(19) . . ?
C13 C12 C11 106.45(18) . . ?
C13 C12 C51 130.10(19) . . ?
C11 C12 C51 123.44(18) . . ?
C12 C13 C14 107.01(18) . . ?
N3 C14 C15 125.40(19) . . ?
N3 C14 C13 110.80(18) . . ?
C15 C14 C13 123.68(19) . . ?
C16 C15 C14 121.31(19) . . ?
C16 C15 C61 120.05(18) . . ?
C14 C15 C61 118.55(18) . . ?
N4 C16 C15 125.87(19) . . ?
N4 C16 C17 110.63(18) . . ?
C15 C16 C17 123.44(19) . . ?
C18 C17 C16 107.11(18) . . ?
C17 C18 C19 106.98(19) . . ?
N4 C19 C20 125.17(19) . . ?
N4 C19 C18 110.80(18) . . ?
C20 C19 C18 123.87(19) . . ?
C1 C20 C19 121.74(19) . . ?
C1 C20 C71 118.03(18) . . ?
C19 C20 C71 120.23(19) . . ?
C26 C21 C22 117.50(19) . . ?
C26 C21 C5 120.39(19) . . ?
C22 C21 C5 122.08(19) . . ?
C23 C22 C21 121.0(2) . . ?
C22 C23 C24 121.8(2) . . ?
C25 C24 C23 116.9(2) . . ?
C25 C24 C27 122.20(19) . . ?
C23 C24 C27 120.87(19) . . ?
C26 C25 C24 121.5(2) . . ?
C25 C26 C21 121.3(2) . . ?
C28 C27 C29 109.9(5) . . ?
C30A C27 C24 114.2(3) . . ?
C28 C27 C24 114.4(4) . . ?
C29 C27 C24 109.5(3) . . ?
C30A C27 C28A 111.5(4) . . ?
C24 C27 C28A 110.7(4) . . ?
C28 C27 C30 107.1(4) . . ?
C29 C27 C30 108.3(4) . . ?
C24 C27 C30 107.5(3) . . ?
C30A C27 C29A 107.4(4) . . ?
C24 C27 C29A 105.7(3) . . ?
C28A C27 C29A 107.0(4) . . ?
C8 C31 C41 112.28(17) . . ?
C8 C31 C32 114.04(17) . . ?
C41 C31 C32 112.44(17) . . ?
C37 C32 C33 119.7(2) . . ?
C37 C32 C31 119.9(2) . . ?
C33 C32 C31 120.28(19) . . ?
C34 C33 C32 119.2(2) . . ?
C34 C33 C38 118.4(2) . . ?
C32 C33 C38 122.4(2) . . ?
C35 C34 C33 122.1(2) . . ?
C34 C35 C36 117.7(2) . . ?
C34 C35 C39 121.2(2) . . ?
C36 C35 C39 121.1(2) . . ?
C35 C36 C37 122.3(2) . . ?
C36 C37 C32 118.9(2) . . ?
C36 C37 C40 119.1(2) . . ?
C32 C37 C40 121.9(2) . . ?
C42 C41 C46 120.19(19) . . ?
C42 C41 C31 118.25(18) . . ?
C46 C41 C31 121.56(18) . . ?
C41 C42 C43 122.5(2) . . ?
C44 C43 C42 116.62(19) . . ?
C44 C43 C47 123.13(19) . . ?
C42 C43 C47 120.24(19) . . ?
C45 C44 C43 122.53(19) . . ?
C44 C45 C46 119.92(19) . . ?
C44 C45 C51 118.60(18) . . ?
C46 C45 C51 121.47(18) . . ?
C41 C46 C45 118.14(19) . . ?
C41 C46 C10 120.48(18) . . ?
C45 C46 C10 121.24(18) . . ?
C43 C47 C50 111.59(18) . . ?
C43 C47 C48 110.11(18) . . ?
C50 C47 C48 107.59(19) . . ?
C43 C47 C49 109.27(18) . . ?
C50 C47 C49 109.48(19) . . ?
C48 C47 C49 108.73(19) . . ?
C12 C51 C45 112.59(17) . . ?
C12 C51 C52 110.05(17) . . ?
C45 C51 C52 115.91(17) . . ?
C53 C52 C57 119.1(2) . . ?
C53 C52 C51 121.65(19) . . ?
C57 C52 C51 119.09(19) . . ?
C54 C53 C52 119.2(2) . . ?
C54 C53 C58 117.7(2) . . ?
C52 C53 C58 123.1(2) . . ?
C55 C54 C53 122.4(2) . . ?
C56 C55 C54 117.6(2) . . ?
C56 C55 C59 121.0(2) . . ?
C54 C55 C59 121.4(2) . . ?
C55 C56 C57 122.2(2) . . ?
C56 C57 C52 119.3(2) . . ?
C56 C57 C60 118.4(2) . . ?
C52 C57 C60 122.4(2) . . ?
C62 C61 C66 117.20(19) . . ?
C62 C61 C15 121.91(19) . . ?
C66 C61 C15 120.86(18) . . ?
C61 C62 C63 121.3(2) . . ?
C64 C63 C62 121.6(2) . . ?
C63 C64 C65 116.67(19) . . ?
C63 C64 C67 122.8(2) . . ?
C65 C64 C67 120.5(2) . . ?
C66 C65 C64 121.9(2) . . ?
C65 C66 C61 121.2(2) . . ?
C69 C67 C70 107.59(19) . . ?
C69 C67 C64 112.01(19) . . ?
C70 C67 C64 110.21(19) . . ?
C69 C67 C68 108.9(2) . . ?
C70 C67 C68 109.8(2) . . ?
C64 C67 C68 108.28(18) . . ?
C72 C71 C76 117.6(2) . . ?
C72 C71 C20 122.09(19) . . ?
C76 C71 C20 120.31(19) . . ?
C71 C72 C73 121.1(2) . . ?
C74 C73 C72 121.6(2) . . ?
C73 C74 C75 117.0(2) . . ?
C73 C74 C77 122.7(2) . . ?
C75 C74 C77 120.3(2) . . ?
C76 C75 C74 121.9(2) . . ?
C75 C76 C71 120.9(2) . . ?
C78 C77 C80 109.1(2) . . ?
C78 C77 C79 107.4(2) . . ?
C80 C77 C79 109.7(2) . . ?
C78 C77 C74 112.1(2) . . ?
C80 C77 C74 108.3(2) . . ?
C79 C77 C74 110.23(19) . . ?

_refine_diff_density_max         1.003
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.057

_shelxl_version_number           2013-4



