# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_mo_grumi1_0m-auto
_database_code_depnum_ccdc_archive 'CCDC 1538675'
_audit_update_record             
;
2017-08-10 deposited with the CCDC.
2018-02-20 downloaded from the CCDC.
;

#===============================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
;
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H33 N8 Ni, C F3 O3 S, C H2 Cl2'
# Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)'
_chemical_formula_structural     ?
_chemical_formula_sum            'C35 H35 Cl2 F3 N8 Ni O3 S'
_chemical_formula_iupac          ?
_chemical_formula_weight         834.36
_chemical_compound_source        'see text'

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

#===============================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_symmetry_Int_Tables_number      2

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,-y,-z

_cell_length_a                   10.0222(8)
_cell_length_b                   12.1506(11)
_cell_length_c                   16.0254(14)
_cell_angle_alpha                69.063(4)
_cell_angle_beta                 75.075(4)
_cell_angle_gamma                81.389(4)
_cell_volume                     1757.6(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100
_cell_measurement_reflns_used    9931
_cell_measurement_theta_min      2.4827
_cell_measurement_theta_max      25.8517
_cell_special_details            
;
;

_exptl_crystal_description       fragment
_exptl_crystal_colour            'clear yellow'

_exptl_crystal_size_max          0.245
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.110
_exptl_crystal_size_rad          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_F_000             860
_exptl_absorpt_coefficient_mu    0.830
_exptl_crystal_density_meas_temp ?

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5, Bruker, 2014'
_exptl_absorpt_correction_T_min  0.6956
_exptl_absorpt_correction_T_max  0.7453

#===============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
;
Diffractometer operator             Philipp J. Altmann
scanspeed                           30 s per frame
dx                                  34 mm
1843 frames measured in 6 data sets
phi-scans with delta_phi         = 0.4
omega-scans with delta_omega     = 0.4
shutterless mode
;
_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'IMS microsource'
_diffrn_radiation_monochromator  'Helios optic'


_diffrn_measurement_device       ' κ-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker Photon CMOS '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_detector                 ' CMOS plate '
_diffrn_detector_area_resol_mean 16

# number of measured reflections (redundant set)
_diffrn_reflns_number            39797
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.48
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_full        25.24
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_reduction_process 
;
;

# number of unique reflections
_reflns_number_total             6667
# number of observed reflections (> n sig(I))
_reflns_number_gt                5772
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'APEX III Control Software (Bruker, 2015)'
_computing_cell_refinement       'SAINT (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2015)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  
'SHELXL2014 (Sheldrick, 2014), SHELXLE (Huebschle, 2011)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2014)'

#===============================================================================

# 8. REFINEMENT DATA

_refine_special_details          
;
 Refinement on F² for ALL reflections except those
 flagged by the user for potential systematic errors.
 Weighted R-factors wR and all goodnesses of fit S
 are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The
 observed criterion of F² > 2sigma(F²) is used only
 for calculating -R-factor-obs etc. and is not
 relevant to the choice of reflections for refinement.
 R-factors based on F² are statistically about twice
 as large as those based on F, and R-factors based on
 ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'W=1/[Σ²(FO²)+(0.0390P)²+0.9346P] 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_abs_structure_details ?
_refine_ls_abs_structure_Flack   .
_refine_ls_number_reflns         6667
_refine_ls_number_parameters     725
_refine_ls_number_restraints     381
_refine_ls_number_constraints    ?
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0288
_refine_ls_wR_factor_ref         0.0755
_refine_ls_wR_factor_gt          0.0711
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.053

#===============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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 0.23036(2) 0.33215(2) 0.62373(2) 0.01533(7) Uani 1 1 d . . . . .
N1 N 0.30836(15) 0.48029(12) 0.57645(10) 0.0163(3) Uani 1 1 d . . . . .
N2 N 0.32625(15) 0.65572(12) 0.44399(10) 0.0190(3) Uani 1 1 d . . . . .
N3 N 0.40712(19) 0.46765(15) 0.69972(11) 0.0297(4) Uani 1 1 d . . . . .
N4 N 0.29768(17) 0.29150(13) 0.72943(12) 0.0250(4) Uani 1 1 d . . . . .
N5 N 0.14870(16) 0.18934(12) 0.66264(11) 0.0227(4) Uani 1 1 d . . . . .
N6 N 0.04475(19) 0.21753(14) 0.53771(10) 0.0278(4) Uani 1 1 d . . . . .
N7 N 0.16607(15) 0.38383(12) 0.51433(10) 0.0151(3) Uani 1 1 d . . . . .
N8 N 0.17450(16) 0.55070(12) 0.37619(11) 0.0201(3) Uani 1 1 d . . . . .
C1 C 0.28616(18) 0.55067(15) 0.49144(12) 0.0170(4) Uani 1 1 d . . . . .
C2 C 0.39853(18) 0.70439(15) 0.48268(12) 0.0190(4) Uani 1 1 d . . . . .
C3 C 0.4428(2) 0.81938(16) 0.43443(13) 0.0232(4) Uani 1 1 d . . . . .
H3 H 0.4232 0.8622 0.3760 0.028 Uiso 1 1 calc R U . . .
C4 C 0.5145(2) 0.86869(17) 0.47297(13) 0.0285(5) Uani 1 1 d . . . . .
H4 H 0.5446 0.9462 0.4408 0.034 Uiso 1 1 calc R U . . .
C5 C 0.5441(2) 0.80644(19) 0.55915(14) 0.0327(5) Uani 1 1 d . . . . .
H5 H 0.5947 0.8421 0.5843 0.039 Uiso 1 1 calc R U . . .
C6 C 0.5012(2) 0.69484(18) 0.60756(13) 0.0278(5) Uani 1 1 d . . . . .
H6 H 0.5208 0.6536 0.6662 0.033 Uiso 1 1 calc R U . . .
C7 C 0.42742(19) 0.64174(16) 0.56933(12) 0.0205(4) Uani 1 1 d . . . . .
C8 C 0.37871(18) 0.52542(16) 0.61639(12) 0.0190(4) Uani 1 1 d . . . . .
C9 C 0.37053(18) 0.36258(16) 0.74918(12) 0.0181(4) Uani 1 1 d . . . . .
C10 C 0.4289(5) 0.2866(4) 0.8406(4) 0.0154(8) Uani 0.505(2) 1 d D U P A 1
C11 C 0.5623(4) 0.2145(4) 0.8098(3) 0.0211(8) Uani 0.505(2) 1 d D U P A 1
H11A H 0.5392 0.1600 0.7837 0.032 Uiso 0.505(2) 1 calc R U P A 1
H11B H 0.6026 0.1695 0.8627 0.032 Uiso 0.505(2) 1 calc R U P A 1
H11C H 0.6293 0.2686 0.7634 0.032 Uiso 0.505(2) 1 calc R U P A 1
C12 C 0.4649(6) 0.3662(6) 0.8858(4) 0.0204(13) Uani 0.505(2) 1 d D U P A 1
H12A H 0.5449 0.4105 0.8458 0.031 Uiso 0.505(2) 1 calc R U P A 1
H12B H 0.4874 0.3177 0.9446 0.031 Uiso 0.505(2) 1 calc R U P A 1
H12C H 0.3857 0.4215 0.8959 0.031 Uiso 0.505(2) 1 calc R U P A 1
C13 C 0.3085(3) 0.2061(3) 0.8957(2) 0.0140(7) Uani 0.505(2) 1 d D U P A 1
C14 C 0.349(2) 0.0857(12) 0.9603(9) 0.018(2) Uani 0.505(2) 1 d D U P A 1
H14A H 0.4048 0.0379 0.9244 0.027 Uiso 0.505(2) 1 calc R U P A 1
H14B H 0.2646 0.0456 0.9981 0.027 Uiso 0.505(2) 1 calc R U P A 1
H14C H 0.4018 0.0963 1.0000 0.027 Uiso 0.505(2) 1 calc R U P A 1
C15 C 0.1939(4) 0.2679(3) 0.9513(2) 0.0186(8) Uani 0.505(2) 1 d D U P A 1
H15A H 0.2258 0.2722 1.0029 0.028 Uiso 0.505(2) 1 calc R U P A 1
H15B H 0.1109 0.2229 0.9746 0.028 Uiso 0.505(2) 1 calc R U P A 1
H15C H 0.1720 0.3479 0.9119 0.028 Uiso 0.505(2) 1 calc R U P A 1
C16 C 0.1188(4) 0.1061(3) 0.7579(3) 0.0119(7) Uani 0.505(2) 1 d D U P A 1
C17 C 0.1709(3) 0.1112(3) 0.8282(2) 0.0141(7) Uani 0.505(2) 1 d D U P A 1
H17 H 0.1493 0.0512 0.8863 0.017 Uiso 0.505(2) 1 calc R U P A 1
C18 C 0.2524(4) 0.1983(3) 0.8186(3) 0.0127(7) Uani 0.505(2) 1 d D U P A 1
C19 C 0.0253(3) 0.0131(3) 0.7675(2) 0.0136(7) Uani 0.505(2) 1 d D U P A 1
C20 C 0.057(2) -0.1102(11) 0.8314(9) 0.019(2) Uani 0.505(2) 1 d D U P A 1
H20A H 0.0015 -0.1665 0.8263 0.028 Uiso 0.505(2) 1 calc R U P A 1
H20B H 0.0341 -0.1102 0.8947 0.028 Uiso 0.505(2) 1 calc R U P A 1
H20C H 0.1554 -0.1332 0.8144 0.028 Uiso 0.505(2) 1 calc R U P A 1
C21 C -0.1232(4) 0.0559(3) 0.8051(3) 0.0192(8) Uani 0.505(2) 1 d D U P A 1
H21A H -0.1463 0.1338 0.7633 0.029 Uiso 0.505(2) 1 calc R U P A 1
H21B H -0.1294 0.0612 0.8656 0.029 Uiso 0.505(2) 1 calc R U P A 1
H21C H -0.1883 -0.0002 0.8104 0.029 Uiso 0.505(2) 1 calc R U P A 1
C22 C 0.0464(5) 0.0229(4) 0.6664(3) 0.0138(10) Uani 0.505(2) 1 d D U P A 1
C23 C -0.0760(12) -0.0078(14) 0.6409(9) 0.016(2) Uani 0.505(2) 1 d D U P A 1
H23A H -0.1530 0.0513 0.6459 0.024 Uiso 0.505(2) 1 calc R U P A 1
H23B H -0.1049 -0.0859 0.6825 0.024 Uiso 0.505(2) 1 calc R U P A 1
H23C H -0.0489 -0.0085 0.5778 0.024 Uiso 0.505(2) 1 calc R U P A 1
C24 C 0.1762(5) -0.0533(4) 0.6361(3) 0.0169(9) Uani 0.505(2) 1 d D U P A 1
H24A H 0.2017 -0.0285 0.5691 0.025 Uiso 0.505(2) 1 calc R U P A 1
H24B H 0.1554 -0.1367 0.6611 0.025 Uiso 0.505(2) 1 calc R U P A 1
H24C H 0.2533 -0.0427 0.6592 0.025 Uiso 0.505(2) 1 calc R U P A 1
C10A C 0.3831(5) 0.3146(4) 0.8404(4) 0.0154(8) Uani 0.495(2) 1 d D U P A 2
C11A C 0.2491(4) 0.3432(3) 0.9058(2) 0.0187(8) Uani 0.495(2) 1 d D U P A 2
H11D H 0.2331 0.4290 0.8907 0.028 Uiso 0.495(2) 1 calc R U P A 2
H11E H 0.2596 0.3075 0.9693 0.028 Uiso 0.495(2) 1 calc R U P A 2
H11F H 0.1703 0.3111 0.8986 0.028 Uiso 0.495(2) 1 calc R U P A 2
C12A C 0.5049(6) 0.3607(6) 0.8566(4) 0.0197(13) Uani 0.495(2) 1 d D U P A 2
H12D H 0.5878 0.3551 0.8096 0.030 Uiso 0.495(2) 1 calc R U P A 2
H12E H 0.5216 0.3131 0.9173 0.030 Uiso 0.495(2) 1 calc R U P A 2
H12F H 0.4832 0.4433 0.8534 0.030 Uiso 0.495(2) 1 calc R U P A 2
C13A C 0.3968(3) 0.1813(3) 0.8511(2) 0.0118(7) Uani 0.495(2) 1 d D U P A 2
C14A C 0.3424(19) 0.0967(12) 0.9472(9) 0.018(2) Uani 0.495(2) 1 d D U P A 2
H14D H 0.3668 0.0151 0.9482 0.027 Uiso 0.495(2) 1 calc R U P A 2
H14E H 0.2416 0.1093 0.9640 0.027 Uiso 0.495(2) 1 calc R U P A 2
H14F H 0.3840 0.1113 0.9910 0.027 Uiso 0.495(2) 1 calc R U P A 2
C15A C 0.5489(3) 0.1425(4) 0.8166(2) 0.0146(8) Uani 0.495(2) 1 d D U P A 2
H15D H 0.5534 0.0634 0.8124 0.022 Uiso 0.495(2) 1 calc R U P A 2
H15E H 0.6040 0.1409 0.8595 0.022 Uiso 0.495(2) 1 calc R U P A 2
H15F H 0.5859 0.1984 0.7560 0.022 Uiso 0.495(2) 1 calc R U P A 2
C16A C 0.1837(4) 0.0906(3) 0.7212(3) 0.0113(7) Uani 0.495(2) 1 d D U P A 2
C17A C 0.2630(4) 0.0850(3) 0.7820(2) 0.0134(7) Uani 0.495(2) 1 d D U P A 2
H17B H 0.2798 0.0107 0.8261 0.016 Uiso 0.495(2) 1 calc R U P A 2
C18A C 0.3186(4) 0.1830(3) 0.7812(3) 0.0116(7) Uani 0.495(2) 1 d D U P A 2
C19A C 0.1135(4) -0.0128(3) 0.7233(2) 0.0133(8) Uani 0.495(2) 1 d D U P A 2
C20A C 0.069(2) -0.1010(11) 0.8195(8) 0.019(2) Uani 0.495(2) 1 d D U P A 2
H20D H 0.0083 -0.1561 0.8183 0.028 Uiso 0.495(2) 1 calc R U P A 2
H20E H 0.0200 -0.0585 0.8613 0.028 Uiso 0.495(2) 1 calc R U P A 2
H20F H 0.1515 -0.1450 0.8406 0.028 Uiso 0.495(2) 1 calc R U P A 2
C21A C 0.2192(5) -0.0758(4) 0.6637(3) 0.0177(10) Uani 0.495(2) 1 d D U P A 2
H21D H 0.1781 -0.1439 0.6633 0.026 Uiso 0.495(2) 1 calc R U P A 2
H21E H 0.3021 -0.1028 0.6890 0.026 Uiso 0.495(2) 1 calc R U P A 2
H21F H 0.2444 -0.0209 0.6010 0.026 Uiso 0.495(2) 1 calc R U P A 2
C22A C -0.0047(5) 0.0533(4) 0.6744(3) 0.0145(10) Uani 0.495(2) 1 d D U P A 2
C23A C -0.0563(13) -0.0078(15) 0.6219(9) 0.016(2) Uani 0.495(2) 1 d D U P A 2
H23D H -0.1316 0.0417 0.5951 0.024 Uiso 0.495(2) 1 calc R U P A 2
H23E H -0.0904 -0.0842 0.6637 0.024 Uiso 0.495(2) 1 calc R U P A 2
H23F H 0.0197 -0.0201 0.5729 0.024 Uiso 0.495(2) 1 calc R U P A 2
C24A C -0.1298(4) 0.0904(3) 0.7410(3) 0.0198(8) Uani 0.495(2) 1 d D U P A 2
H24D H -0.1919 0.1477 0.7059 0.030 Uiso 0.495(2) 1 calc R U P A 2
H24E H -0.0968 0.1263 0.7773 0.030 Uiso 0.495(2) 1 calc R U P A 2
H24F H -0.1798 0.0207 0.7821 0.030 Uiso 0.495(2) 1 calc R U P A 2
C25 C 0.07269(18) 0.15816(15) 0.61616(12) 0.0175(4) Uani 1 1 d . . . . .
C26 C 0.08877(18) 0.32655(15) 0.48769(12) 0.0164(4) Uani 1 1 d . . . . .
C27 C 0.04942(18) 0.38153(14) 0.40183(12) 0.0157(3) Uani 1 1 d . . . . .
C28 C -0.03289(19) 0.32630(15) 0.37050(12) 0.0187(4) Uani 1 1 d . . . . .
H28 H -0.0670 0.2513 0.4077 0.022 Uiso 1 1 calc R U . . .
C29 C -0.06295(19) 0.38211(15) 0.28592(12) 0.0200(4) Uani 1 1 d . . . . .
H29 H -0.1171 0.3451 0.2641 0.024 Uiso 1 1 calc R U . . .
C30 C -0.0142(2) 0.49362(16) 0.23140(14) 0.0243(4) Uani 1 1 d . . . . .
H30 H -0.0346 0.5307 0.1725 0.029 Uiso 1 1 calc R U . . .
C31 C 0.0622(2) 0.54979(16) 0.26163(14) 0.0246(4) Uani 1 1 d . . . . .
H31 H 0.0922 0.6263 0.2248 0.030 Uiso 1 1 calc R U . . .
C32 C 0.09603(18) 0.49391(15) 0.34726(13) 0.0187(4) Uani 1 1 d . . . . .
C33 C 0.20387(18) 0.49459(14) 0.45529(12) 0.0176(4) Uani 1 1 d . . . . .
S1 S 0.4628(4) 0.1864(4) 0.1880(2) 0.0194(5) Uani 0.558(11) 1 d D U P B 5
O1 O 0.4896(11) 0.1614(9) 0.1039(5) 0.0230(14) Uani 0.558(11) 1 d D U P B 5
O2 O 0.5734(7) 0.2435(5) 0.1968(5) 0.0265(11) Uani 0.558(11) 1 d D U P B 5
O3 O 0.3993(6) 0.0983(5) 0.2710(3) 0.0311(11) Uani 0.558(11) 1 d D U P B 5
C34 C 0.3293(6) 0.3059(7) 0.1717(5) 0.0221(13) Uani 0.558(11) 1 d D U P B 5
F1 F 0.3720(6) 0.3969(5) 0.0970(4) 0.0374(10) Uani 0.558(11) 1 d D U P B 5
F2 F 0.2921(4) 0.3457(5) 0.2423(4) 0.0410(11) Uani 0.558(11) 1 d D U P B 5
F3 F 0.2159(8) 0.2721(6) 0.1607(6) 0.0357(13) Uani 0.558(11) 1 d D U P B 5
S1A S 0.4841(5) 0.1556(4) 0.2003(3) 0.0220(6) Uani 0.442(11) 1 d D U P B 6
O1A O 0.5145(16) 0.1413(13) 0.1124(8) 0.034(3) Uani 0.442(11) 1 d D U P B 6
O2A O 0.5899(9) 0.2059(8) 0.2171(7) 0.0337(17) Uani 0.442(11) 1 d D U P B 6
O3A O 0.4254(9) 0.0567(6) 0.2735(5) 0.0514(19) Uani 0.442(11) 1 d D U P B 6
C34A C 0.3464(8) 0.2678(7) 0.1938(5) 0.0212(16) Uani 0.442(11) 1 d D U P B 6
F1A F 0.3828(9) 0.3702(6) 0.1284(6) 0.0489(16) Uani 0.442(11) 1 d D U P B 6
F2A F 0.2993(6) 0.2907(8) 0.2726(4) 0.0447(14) Uani 0.442(11) 1 d D U P B 6
F3A F 0.2341(10) 0.2382(8) 0.1766(8) 0.0385(18) Uani 0.442(11) 1 d D U P B 6
Cl1 Cl 0.1836(3) 0.7701(2) 0.0358(2) 0.0239(6) Uani 0.558(11) 1 d D U P B 3
Cl2 Cl 0.1348(4) 0.5846(4) -0.0279(3) 0.0299(6) Uani 0.558(11) 1 d D U P B 3
C35 C 0.2546(6) 0.6435(6) 0.0057(4) 0.0258(12) Uani 0.558(11) 1 d D U P B 3
H35A H 0.3369 0.6647 -0.0453 0.031 Uiso 0.558(11) 1 calc R U P B 3
H35B H 0.2850 0.5826 0.0587 0.031 Uiso 0.558(11) 1 calc R U P B 3
Cl1A Cl 0.1341(8) 0.7907(3) 0.0584(3) 0.0370(10) Uani 0.442(11) 1 d D U P B 4
Cl2A Cl 0.1096(5) 0.6093(4) -0.0164(3) 0.0257(6) Uani 0.442(11) 1 d D U P B 4
C35A C 0.2246(8) 0.6873(7) 0.0056(6) 0.0305(18) Uani 0.442(11) 1 d D U P B 4
H35C H 0.2871 0.7292 -0.0528 0.037 Uiso 0.442(11) 1 calc R U P B 4
H35D H 0.2821 0.6306 0.0460 0.037 Uiso 0.442(11) 1 calc R U P B 4


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N5 1.8599(15) . ?
Ni1 N4 1.8599(16) . ?
Ni1 N7 1.8861(15) . ?
Ni1 N1 1.8885(14) . ?
N1 C8 1.344(2) . ?
N1 C1 1.380(2) . ?
N2 C1 1.293(2) . ?
N2 C2 1.371(2) . ?
N3 C9 1.288(2) . ?
N3 C8 1.350(2) . ?
N4 C18A 1.302(4) . ?
N4 C9 1.372(2) . ?
N4 C18 1.481(4) . ?
N5 C16A 1.297(4) . ?
N5 C25 1.363(2) . ?
N5 C16 1.482(4) . ?
N6 C25 1.285(2) . ?
N6 C26 1.351(2) . ?
N7 C26 1.346(2) . ?
N7 C33 1.381(2) . ?
N8 C33 1.293(2) . ?
N8 C32 1.374(2) . ?
C1 C33 1.475(2) . ?
C2 C7 1.406(3) . ?
C2 C3 1.408(2) . ?
C3 C4 1.371(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.402(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.370(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.413(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.435(2) . ?
C9 C10A 1.399(6) . ?
C9 C10 1.629(6) . ?
C10 C12 1.526(7) . ?
C10 C13 1.543(6) . ?
C10 C11 1.556(6) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C18 1.519(4) . ?
C13 C14 1.526(10) . ?
C13 C15 1.540(5) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.381(4) . ?
C16 C19 1.516(4) . ?
C17 C18 1.375(5) . ?
C17 H17 0.9500 . ?
C19 C20 1.524(10) . ?
C19 C22 1.542(5) . ?
C19 C21 1.543(5) . ?
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 C23 1.522(9) . ?
C22 C24 1.556(6) . ?
C22 C25 1.579(5) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C10A C12A 1.531(7) . ?
C10A C11A 1.555(6) . ?
C10A C13A 1.555(5) . ?
C11A H11D 0.9800 . ?
C11A H11E 0.9800 . ?
C11A H11F 0.9800 . ?
C12A H12D 0.9800 . ?
C12A H12E 0.9800 . ?
C12A H12F 0.9800 . ?
C13A C18A 1.517(4) . ?
C13A C14A 1.526(11) . ?
C13A C15A 1.546(5) . ?
C14A H14D 0.9800 . ?
C14A H14E 0.9800 . ?
C14A H14F 0.9800 . ?
C15A H15D 0.9800 . ?
C15A H15E 0.9800 . ?
C15A H15F 0.9800 . ?
C16A C17A 1.386(4) . ?
C16A C19A 1.515(4) . ?
C17A C18A 1.383(5) . ?
C17A H17B 0.9500 . ?
C19A C20A 1.527(10) . ?
C19A C21A 1.542(6) . ?
C19A C22A 1.550(5) . ?
C20A H20D 0.9800 . ?
C20A H20E 0.9800 . ?
C20A H20F 0.9800 . ?
C21A H21D 0.9800 . ?
C21A H21E 0.9800 . ?
C21A H21F 0.9800 . ?
C22A C25 1.473(6) . ?
C22A C23A 1.521(9) . ?
C22A C24A 1.549(6) . ?
C23A H23D 0.9800 . ?
C23A H23E 0.9800 . ?
C23A H23F 0.9800 . ?
C24A H24D 0.9800 . ?
C24A H24E 0.9800 . ?
C24A H24F 0.9800 . ?
C26 C27 1.428(2) . ?
C27 C32 1.405(2) . ?
C27 C28 1.415(2) . ?
C28 C29 1.371(3) . ?
C28 H28 0.9500 . ?
C29 C30 1.404(3) . ?
C29 H29 0.9500 . ?
C30 C31 1.368(3) . ?
C30 H30 0.9500 . ?
C31 C32 1.401(3) . ?
C31 H31 0.9500 . ?
S1 O1 1.437(6) . ?
S1 O3 1.439(5) . ?
S1 O2 1.453(6) . ?
S1 C34 1.814(6) . ?
C34 F2 1.330(6) . ?
C34 F1 1.331(7) . ?
C34 F3 1.337(7) . ?
S1A O3A 1.420(7) . ?
S1A O2A 1.425(8) . ?
S1A O1A 1.430(9) . ?
S1A C34A 1.785(7) . ?
C34A F1A 1.336(7) . ?
C34A F2A 1.341(8) . ?
C34A F3A 1.352(9) . ?
Cl1 C35 1.770(5) . ?
Cl2 C35 1.763(6) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
Cl1A C35A 1.772(7) . ?
Cl2A C35A 1.768(7) . ?
C35A H35C 0.9900 . ?
C35A H35D 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 Ni1 N4 92.70(7) . . ?
N5 Ni1 N7 91.17(6) . . ?
N4 Ni1 N7 176.09(6) . . ?
N5 Ni1 N1 175.85(6) . . ?
N4 Ni1 N1 91.45(6) . . ?
N7 Ni1 N1 84.68(6) . . ?
C8 N1 C1 117.05(15) . . ?
C8 N1 Ni1 127.97(13) . . ?
C1 N1 Ni1 114.96(11) . . ?
C1 N2 C2 116.56(16) . . ?
C9 N3 C8 123.43(16) . . ?
C18A N4 C9 108.3(2) . . ?
C9 N4 C18 104.09(18) . . ?
C18A N4 Ni1 123.62(18) . . ?
C9 N4 Ni1 125.33(13) . . ?
C18 N4 Ni1 128.27(15) . . ?
C16A N5 C25 104.86(19) . . ?
C25 N5 C16 106.48(17) . . ?
C16A N5 Ni1 126.81(18) . . ?
C25 N5 Ni1 125.51(12) . . ?
C16 N5 Ni1 125.79(16) . . ?
C25 N6 C26 122.97(15) . . ?
C26 N7 C33 117.03(15) . . ?
C26 N7 Ni1 128.09(12) . . ?
C33 N7 Ni1 114.88(11) . . ?
C33 N8 C32 116.40(15) . . ?
N2 C1 N1 127.91(16) . . ?
N2 C1 C33 119.42(16) . . ?
N1 C1 C33 112.66(14) . . ?
N2 C2 C7 121.02(16) . . ?
N2 C2 C3 118.84(17) . . ?
C7 C2 C3 120.14(17) . . ?
C4 C3 C2 119.09(19) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C3 C4 C5 121.01(17) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C6 C5 C4 120.87(18) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C5 C6 C7 119.31(19) . . ?
C5 C6 H6 120.3 . . ?
C7 C6 H6 120.3 . . ?
C2 C7 C6 119.58(16) . . ?
C2 C7 C8 118.13(16) . . ?
C6 C7 C8 122.28(17) . . ?
N1 C8 N3 123.83(16) . . ?
N1 C8 C7 119.33(17) . . ?
N3 C8 C7 116.85(16) . . ?
N3 C9 N4 127.96(17) . . ?
N3 C9 C10A 120.7(3) . . ?
N4 C9 C10A 110.6(3) . . ?
N3 C9 C10 122.1(2) . . ?
N4 C9 C10 109.3(2) . . ?
C12 C10 C13 116.8(5) . . ?
C12 C10 C11 108.9(4) . . ?
C13 C10 C11 111.4(4) . . ?
C12 C10 C9 111.9(4) . . ?
C13 C10 C9 100.2(3) . . ?
C11 C10 C9 106.9(4) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C18 C13 C14 113.3(7) . . ?
C18 C13 C15 107.4(3) . . ?
C14 C13 C15 108.4(8) . . ?
C18 C13 C10 100.8(3) . . ?
C14 C13 C10 115.5(7) . . ?
C15 C13 C10 111.1(3) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 N5 124.7(3) . . ?
C17 C16 C19 124.5(3) . . ?
N5 C16 C19 110.8(2) . . ?
C18 C17 C16 123.5(3) . . ?
C18 C17 H17 118.3 . . ?
C16 C17 H17 118.3 . . ?
C17 C18 N4 122.0(3) . . ?
C17 C18 C13 124.1(3) . . ?
N4 C18 C13 113.9(2) . . ?
C16 C19 C20 115.1(7) . . ?
C16 C19 C22 100.5(3) . . ?
C20 C19 C22 114.6(7) . . ?
C16 C19 C21 106.3(3) . . ?
C20 C19 C21 108.6(8) . . ?
C22 C19 C21 111.2(3) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 C19 115.6(6) . . ?
C23 C22 C24 108.2(6) . . ?
C19 C22 C24 111.7(4) . . ?
C23 C22 C25 110.2(7) . . ?
C19 C22 C25 101.2(3) . . ?
C24 C22 C25 109.7(3) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C9 C10A C12A 112.5(5) . . ?
C9 C10A C11A 110.9(3) . . ?
C12A C10A C11A 108.1(4) . . ?
C9 C10A C13A 99.1(4) . . ?
C12A C10A C13A 115.7(4) . . ?
C11A C10A C13A 110.4(4) . . ?
C10A C11A H11D 109.5 . . ?
C10A C11A H11E 109.5 . . ?
H11D C11A H11E 109.5 . . ?
C10A C11A H11F 109.5 . . ?
H11D C11A H11F 109.5 . . ?
H11E C11A H11F 109.5 . . ?
C10A C12A H12D 109.5 . . ?
C10A C12A H12E 109.5 . . ?
H12D C12A H12E 109.5 . . ?
C10A C12A H12F 109.5 . . ?
H12D C12A H12F 109.5 . . ?
H12E C12A H12F 109.5 . . ?
C18A C13A C14A 113.7(7) . . ?
C18A C13A C15A 106.5(3) . . ?
C14A C13A C15A 109.0(7) . . ?
C18A C13A C10A 100.6(3) . . ?
C14A C13A C10A 116.1(8) . . ?
C15A C13A C10A 110.4(3) . . ?
C13A C14A H14D 109.5 . . ?
C13A C14A H14E 109.5 . . ?
H14D C14A H14E 109.5 . . ?
C13A C14A H14F 109.5 . . ?
H14D C14A H14F 109.5 . . ?
H14E C14A H14F 109.5 . . ?
C13A C15A H15D 109.5 . . ?
C13A C15A H15E 109.5 . . ?
H15D C15A H15E 109.5 . . ?
C13A C15A H15F 109.5 . . ?
H15D C15A H15F 109.5 . . ?
H15E C15A H15F 109.5 . . ?
N5 C16A C17A 122.5(3) . . ?
N5 C16A C19A 112.4(3) . . ?
C17A C16A C19A 124.6(3) . . ?
C18A C17A C16A 122.8(3) . . ?
C18A C17A H17B 118.6 . . ?
C16A C17A H17B 118.6 . . ?
N4 C18A C17A 126.0(3) . . ?
N4 C18A C13A 109.5(3) . . ?
C17A C18A C13A 123.9(3) . . ?
C16A C19A C20A 113.3(6) . . ?
C16A C19A C21A 106.6(3) . . ?
C20A C19A C21A 109.0(8) . . ?
C16A C19A C22A 100.5(3) . . ?
C20A C19A C22A 116.2(8) . . ?
C21A C19A C22A 110.6(3) . . ?
C19A C20A H20D 109.5 . . ?
C19A C20A H20E 109.5 . . ?
H20D C20A H20E 109.5 . . ?
C19A C20A H20F 109.5 . . ?
H20D C20A H20F 109.5 . . ?
H20E C20A H20F 109.5 . . ?
C19A C21A H21D 109.5 . . ?
C19A C21A H21E 109.5 . . ?
H21D C21A H21E 109.5 . . ?
C19A C21A H21F 109.5 . . ?
H21D C21A H21F 109.5 . . ?
H21E C21A H21F 109.5 . . ?
C25 C22A C23A 114.4(7) . . ?
C25 C22A C24A 108.7(3) . . ?
C23A C22A C24A 109.0(6) . . ?
C25 C22A C19A 95.2(3) . . ?
C23A C22A C19A 117.1(7) . . ?
C24A C22A C19A 111.7(4) . . ?
C22A C23A H23D 109.5 . . ?
C22A C23A H23E 109.5 . . ?
H23D C23A H23E 109.5 . . ?
C22A C23A H23F 109.5 . . ?
H23D C23A H23F 109.5 . . ?
H23E C23A H23F 109.5 . . ?
C22A C24A H24D 109.5 . . ?
C22A C24A H24E 109.5 . . ?
H24D C24A H24E 109.5 . . ?
C22A C24A H24F 109.5 . . ?
H24D C24A H24F 109.5 . . ?
H24E C24A H24F 109.5 . . ?
N6 C25 N5 128.40(16) . . ?
N6 C25 C22A 118.7(2) . . ?
N5 C25 C22A 111.8(2) . . ?
N6 C25 C22 123.2(2) . . ?
N5 C25 C22 107.5(2) . . ?
N7 C26 N6 123.83(16) . . ?
N7 C26 C27 119.62(15) . . ?
N6 C26 C27 116.54(15) . . ?
C32 C27 C28 119.80(16) . . ?
C32 C27 C26 117.95(15) . . ?
C28 C27 C26 122.25(16) . . ?
C29 C28 C27 119.34(16) . . ?
C29 C28 H28 120.3 . . ?
C27 C28 H28 120.3 . . ?
C28 C29 C30 120.38(17) . . ?
C28 C29 H29 119.8 . . ?
C30 C29 H29 119.8 . . ?
C31 C30 C29 121.08(18) . . ?
C31 C30 H30 119.5 . . ?
C29 C30 H30 119.5 . . ?
C30 C31 C32 119.64(17) . . ?
C30 C31 H31 120.2 . . ?
C32 C31 H31 120.2 . . ?
N8 C32 C31 119.00(16) . . ?
N8 C32 C27 121.28(16) . . ?
C31 C32 C27 119.73(16) . . ?
N8 C33 N7 127.71(16) . . ?
N8 C33 C1 119.48(15) . . ?
N7 C33 C1 112.81(15) . . ?
O1 S1 O3 117.9(5) . . ?
O1 S1 O2 114.0(6) . . ?
O3 S1 O2 114.7(4) . . ?
O1 S1 C34 102.3(4) . . ?
O3 S1 C34 103.3(3) . . ?
O2 S1 C34 101.5(3) . . ?
F2 C34 F1 107.4(5) . . ?
F2 C34 F3 107.8(6) . . ?
F1 C34 F3 106.5(5) . . ?
F2 C34 S1 112.0(4) . . ?
F1 C34 S1 111.3(4) . . ?
F3 C34 S1 111.5(5) . . ?
O3A S1A O2A 115.4(5) . . ?
O3A S1A O1A 114.0(8) . . ?
O2A S1A O1A 114.7(8) . . ?
O3A S1A C34A 103.8(4) . . ?
O2A S1A C34A 103.2(4) . . ?
O1A S1A C34A 103.6(5) . . ?
F1A C34A F2A 106.9(6) . . ?
F1A C34A F3A 106.3(7) . . ?
F2A C34A F3A 104.8(8) . . ?
F1A C34A S1A 112.8(6) . . ?
F2A C34A S1A 112.5(5) . . ?
F3A C34A S1A 113.0(6) . . ?
Cl2 C35 Cl1 112.2(3) . . ?
Cl2 C35 H35A 109.2 . . ?
Cl1 C35 H35A 109.2 . . ?
Cl2 C35 H35B 109.2 . . ?
Cl1 C35 H35B 109.2 . . ?
H35A C35 H35B 107.9 . . ?
Cl2A C35A Cl1A 111.4(4) . . ?
Cl2A C35A H35C 109.3 . . ?
Cl1A C35A H35C 109.3 . . ?
Cl2A C35A H35D 109.3 . . ?
Cl1A C35A H35D 109.3 . . ?
H35C C35A H35D 108.0 . . ?

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
N4 Ni1 N1 C8 -2.02(16) . . . . ?
N7 Ni1 N1 C8 177.44(15) . . . . ?
N4 Ni1 N1 C1 179.82(13) . . . . ?
N7 Ni1 N1 C1 -0.73(12) . . . . ?
N5 Ni1 N4 C18A 23.0(3) . . . . ?
N1 Ni1 N4 C18A -157.0(3) . . . . ?
N5 Ni1 N4 C9 -178.16(16) . . . . ?
N1 Ni1 N4 C9 1.83(16) . . . . ?
N5 Ni1 N4 C18 -18.3(2) . . . . ?
N1 Ni1 N4 C18 161.7(2) . . . . ?
N4 Ni1 N5 C16A -23.9(3) . . . . ?
N7 Ni1 N5 C16A 156.6(3) . . . . ?
N4 Ni1 N5 C25 178.03(16) . . . . ?
N7 Ni1 N5 C25 -1.43(16) . . . . ?
N4 Ni1 N5 C16 17.3(2) . . . . ?
N7 Ni1 N5 C16 -162.2(2) . . . . ?
N5 Ni1 N7 C26 1.10(15) . . . . ?
N1 Ni1 N7 C26 -178.93(15) . . . . ?
N5 Ni1 N7 C33 -179.10(12) . . . . ?
N1 Ni1 N7 C33 0.87(12) . . . . ?
C2 N2 C1 N1 -0.7(3) . . . . ?
C2 N2 C1 C33 177.96(15) . . . . ?
C8 N1 C1 N2 0.8(3) . . . . ?
Ni1 N1 C1 N2 179.21(14) . . . . ?
C8 N1 C1 C33 -177.93(14) . . . . ?
Ni1 N1 C1 C33 0.44(18) . . . . ?
C1 N2 C2 C7 0.4(2) . . . . ?
C1 N2 C2 C3 -179.05(16) . . . . ?
N2 C2 C3 C4 179.69(17) . . . . ?
C7 C2 C3 C4 0.2(3) . . . . ?
C2 C3 C4 C5 0.0(3) . . . . ?
C3 C4 C5 C6 -0.5(3) . . . . ?
C4 C5 C6 C7 0.7(3) . . . . ?
N2 C2 C7 C6 -179.50(17) . . . . ?
C3 C2 C7 C6 -0.1(3) . . . . ?
N2 C2 C7 C8 -0.2(3) . . . . ?
C3 C2 C7 C8 179.23(16) . . . . ?
C5 C6 C7 C2 -0.4(3) . . . . ?
C5 C6 C7 C8 -179.67(19) . . . . ?
C1 N1 C8 N3 179.29(17) . . . . ?
Ni1 N1 C8 N3 1.2(3) . . . . ?
C1 N1 C8 C7 -0.6(2) . . . . ?
Ni1 N1 C8 C7 -178.70(12) . . . . ?
C9 N3 C8 N1 0.6(3) . . . . ?
C9 N3 C8 C7 -179.51(18) . . . . ?
C2 C7 C8 N1 0.3(3) . . . . ?
C6 C7 C8 N1 179.58(17) . . . . ?
C2 C7 C8 N3 -179.56(17) . . . . ?
C6 C7 C8 N3 -0.3(3) . . . . ?
C8 N3 C9 N4 -0.8(3) . . . . ?
C8 N3 C9 C10A -169.7(3) . . . . ?
C8 N3 C9 C10 169.1(3) . . . . ?
C18A N4 C9 N3 160.6(3) . . . . ?
C18 N4 C9 N3 -164.7(2) . . . . ?
Ni1 N4 C9 N3 -0.9(3) . . . . ?
C18A N4 C9 C10A -29.5(4) . . . . ?
Ni1 N4 C9 C10A 169.0(2) . . . . ?
C18 N4 C9 C10 24.4(3) . . . . ?
Ni1 N4 C9 C10 -171.8(2) . . . . ?
N3 C9 C10 C12 28.6(5) . . . . ?
N4 C9 C10 C12 -159.8(4) . . . . ?
N3 C9 C10 C13 153.2(2) . . . . ?
N4 C9 C10 C13 -35.2(3) . . . . ?
N3 C9 C10 C11 -90.6(4) . . . . ?
N4 C9 C10 C11 81.0(3) . . . . ?
C12 C10 C13 C18 149.5(4) . . . . ?
C11 C10 C13 C18 -84.5(4) . . . . ?
C9 C10 C13 C18 28.4(3) . . . . ?
C12 C10 C13 C14 -88.1(9) . . . . ?
C11 C10 C13 C14 38.0(9) . . . . ?
C9 C10 C13 C14 150.8(8) . . . . ?
C12 C10 C13 C15 35.9(5) . . . . ?
C11 C10 C13 C15 162.0(3) . . . . ?
C9 C10 C13 C15 -85.2(3) . . . . ?
C25 N5 C16 C17 -177.0(3) . . . . ?
Ni1 N5 C16 C17 -13.2(5) . . . . ?
C25 N5 C16 C19 4.1(3) . . . . ?
Ni1 N5 C16 C19 167.9(2) . . . . ?
N5 C16 C17 C18 3.1(6) . . . . ?
C19 C16 C17 C18 -178.2(4) . . . . ?
C16 C17 C18 N4 -3.4(6) . . . . ?
C16 C17 C18 C13 178.9(4) . . . . ?
C9 N4 C18 C17 177.5(3) . . . . ?
Ni1 N4 C18 C17 14.3(5) . . . . ?
C9 N4 C18 C13 -4.6(3) . . . . ?
Ni1 N4 C18 C13 -167.8(2) . . . . ?
C14 C13 C18 C17 36.4(9) . . . . ?
C15 C13 C18 C17 -83.3(4) . . . . ?
C10 C13 C18 C17 160.4(4) . . . . ?
C14 C13 C18 N4 -141.5(8) . . . . ?
C15 C13 C18 N4 98.9(3) . . . . ?
C10 C13 C18 N4 -17.5(4) . . . . ?
C17 C16 C19 C20 -36.1(9) . . . . ?
N5 C16 C19 C20 142.7(8) . . . . ?
C17 C16 C19 C22 -159.9(4) . . . . ?
N5 C16 C19 C22 19.0(4) . . . . ?
C17 C16 C19 C21 84.2(4) . . . . ?
N5 C16 C19 C21 -97.0(3) . . . . ?
C16 C19 C22 C23 -150.5(8) . . . . ?
C20 C19 C22 C23 85.4(11) . . . . ?
C21 C19 C22 C23 -38.3(8) . . . . ?
C16 C19 C22 C24 85.2(4) . . . . ?
C20 C19 C22 C24 -38.9(9) . . . . ?
C21 C19 C22 C24 -162.6(3) . . . . ?
C16 C19 C22 C25 -31.5(3) . . . . ?
C20 C19 C22 C25 -155.5(8) . . . . ?
C21 C19 C22 C25 80.8(3) . . . . ?
N3 C9 C10A C12A -31.2(5) . . . . ?
N4 C9 C10A C12A 158.1(4) . . . . ?
N3 C9 C10A C11A 90.0(4) . . . . ?
N4 C9 C10A C11A -80.7(4) . . . . ?
N3 C9 C10A C13A -154.0(2) . . . . ?
N4 C9 C10A C13A 35.3(3) . . . . ?
C9 C10A C13A C18A -27.3(4) . . . . ?
C12A C10A C13A C18A -147.8(5) . . . . ?
C11A C10A C13A C18A 89.1(4) . . . . ?
C9 C10A C13A C14A -150.5(7) . . . . ?
C12A C10A C13A C14A 89.1(9) . . . . ?
C11A C10A C13A C14A -34.1(8) . . . . ?
C9 C10A C13A C15A 84.9(3) . . . . ?
C12A C10A C13A C15A -35.6(6) . . . . ?
C11A C10A C13A C15A -158.7(3) . . . . ?
C25 N5 C16A C17A 179.9(3) . . . . ?
Ni1 N5 C16A C17A 18.2(5) . . . . ?
C25 N5 C16A C19A -7.4(4) . . . . ?
Ni1 N5 C16A C19A -169.1(2) . . . . ?
N5 C16A C17A C18A -4.3(6) . . . . ?
C19A C16A C17A C18A -176.1(4) . . . . ?
C9 N4 C18A C17A 179.9(4) . . . . ?
Ni1 N4 C18A C17A -18.2(5) . . . . ?
C9 N4 C18A C13A 8.2(4) . . . . ?
Ni1 N4 C18A C13A 170.1(2) . . . . ?
C16A C17A C18A N4 4.8(7) . . . . ?
C16A C17A C18A C13A 175.3(4) . . . . ?
C14A C13A C18A N4 137.5(8) . . . . ?
C15A C13A C18A N4 -102.5(4) . . . . ?
C10A C13A C18A N4 12.7(4) . . . . ?
C14A C13A C18A C17A -34.4(9) . . . . ?
C15A C13A C18A C17A 85.6(4) . . . . ?
C10A C13A C18A C17A -159.2(4) . . . . ?
N5 C16A C19A C20A -141.4(9) . . . . ?
C17A C16A C19A C20A 31.1(10) . . . . ?
N5 C16A C19A C21A 98.7(4) . . . . ?
C17A C16A C19A C21A -88.8(5) . . . . ?
N5 C16A C19A C22A -16.7(4) . . . . ?
C17A C16A C19A C22A 155.8(4) . . . . ?
C16A C19A C22A C25 30.4(3) . . . . ?
C20A C19A C22A C25 153.2(7) . . . . ?
C21A C19A C22A C25 -81.9(3) . . . . ?
C16A C19A C22A C23A 151.2(7) . . . . ?
C20A C19A C22A C23A -86.0(10) . . . . ?
C21A C19A C22A C23A 38.9(7) . . . . ?
C16A C19A C22A C24A -82.0(4) . . . . ?
C20A C19A C22A C24A 40.7(8) . . . . ?
C21A C19A C22A C24A 165.6(3) . . . . ?
C26 N6 C25 N5 -0.7(3) . . . . ?
C26 N6 C25 C22A 166.3(3) . . . . ?
C26 N6 C25 C22 -168.2(3) . . . . ?
C16A N5 C25 N6 -160.5(3) . . . . ?
C16 N5 C25 N6 165.4(2) . . . . ?
Ni1 N5 C25 N6 1.5(3) . . . . ?
C16A N5 C25 C22A 31.8(3) . . . . ?
Ni1 N5 C25 C22A -166.2(2) . . . . ?
C16 N5 C25 C22 -25.6(3) . . . . ?
Ni1 N5 C25 C22 170.6(2) . . . . ?
C23A C22A C25 N6 28.2(7) . . . . ?
C24A C22A C25 N6 -93.9(3) . . . . ?
C19A C22A C25 N6 151.1(2) . . . . ?
C23A C22A C25 N5 -162.7(7) . . . . ?
C24A C22A C25 N5 75.2(3) . . . . ?
C19A C22A C25 N5 -39.8(3) . . . . ?
C23 C22 C25 N6 -30.0(6) . . . . ?
C19 C22 C25 N6 -152.9(2) . . . . ?
C24 C22 C25 N6 89.0(4) . . . . ?
C23 C22 C25 N5 160.2(5) . . . . ?
C19 C22 C25 N5 37.4(3) . . . . ?
C24 C22 C25 N5 -80.8(3) . . . . ?
C33 N7 C26 N6 179.53(16) . . . . ?
Ni1 N7 C26 N6 -0.7(3) . . . . ?
C33 N7 C26 C27 -0.3(2) . . . . ?
Ni1 N7 C26 C27 179.50(12) . . . . ?
C25 N6 C26 N7 0.2(3) . . . . ?
C25 N6 C26 C27 -179.98(18) . . . . ?
N7 C26 C27 C32 1.2(2) . . . . ?
N6 C26 C27 C32 -178.67(16) . . . . ?
N7 C26 C27 C28 -179.35(15) . . . . ?
N6 C26 C27 C28 0.8(3) . . . . ?
C32 C27 C28 C29 1.8(3) . . . . ?
C26 C27 C28 C29 -177.70(16) . . . . ?
C27 C28 C29 C30 -0.9(3) . . . . ?
C28 C29 C30 C31 -1.0(3) . . . . ?
C29 C30 C31 C32 1.9(3) . . . . ?
C33 N8 C32 C31 -179.29(17) . . . . ?
C33 N8 C32 C27 0.7(2) . . . . ?
C30 C31 C32 N8 179.10(17) . . . . ?
C30 C31 C32 C27 -0.9(3) . . . . ?
C28 C27 C32 N8 179.08(16) . . . . ?
C26 C27 C32 N8 -1.4(2) . . . . ?
C28 C27 C32 C31 -0.9(3) . . . . ?
C26 C27 C32 C31 178.62(17) . . . . ?
C32 N8 C33 N7 0.2(3) . . . . ?
C32 N8 C33 C1 -179.18(15) . . . . ?
C26 N7 C33 N8 -0.4(3) . . . . ?
Ni1 N7 C33 N8 179.73(15) . . . . ?
C26 N7 C33 C1 178.99(14) . . . . ?
Ni1 N7 C33 C1 -0.84(18) . . . . ?
N2 C1 C33 N8 0.9(2) . . . . ?
N1 C1 C33 N8 179.74(15) . . . . ?
N2 C1 C33 N7 -178.63(15) . . . . ?
N1 C1 C33 N7 0.3(2) . . . . ?
O1 S1 C34 F2 -177.9(6) . . . . ?
O3 S1 C34 F2 59.1(5) . . . . ?
O2 S1 C34 F2 -59.9(6) . . . . ?
O1 S1 C34 F1 -57.7(6) . . . . ?
O3 S1 C34 F1 179.4(4) . . . . ?
O2 S1 C34 F1 60.4(5) . . . . ?
O1 S1 C34 F3 61.2(8) . . . . ?
O3 S1 C34 F3 -61.8(6) . . . . ?
O2 S1 C34 F3 179.2(6) . . . . ?
O3A S1A C34A F1A 179.1(7) . . . . ?
O2A S1A C34A F1A 58.4(7) . . . . ?
O1A S1A C34A F1A -61.5(10) . . . . ?
O3A S1A C34A F2A 58.2(7) . . . . ?
O2A S1A C34A F2A -62.6(7) . . . . ?
O1A S1A C34A F2A 177.6(9) . . . . ?
O3A S1A C34A F3A -60.2(8) . . . . ?
O2A S1A C34A F3A 179.1(7) . . . . ?
O1A S1A C34A F3A 59.2(10) . . . . ?


####################################################################### 
# 
# 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_grumi20_0ma-auto
_database_code_depnum_ccdc_archive 'CCDC 1586948'
_audit_update_record             
;
2017-11-21 deposited with the CCDC.
2018-02-20 downloaded from the CCDC.
;

#===============================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
;
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H35 N'
# Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)'
_chemical_formula_structural     ?
_chemical_formula_sum            'C22 H35 N'
_chemical_formula_iupac          ?
_chemical_formula_weight         313.51
_chemical_compound_source        'see text'

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'

#===============================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_Int_Tables_number      14

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,1/2+y,1/2-z
3 -x,-y,-z
4 x,1/2-y,1/2+z

_cell_length_a                   17.6983(15)
_cell_length_b                   6.2954(6)
_cell_length_c                   17.4420(15)
_cell_angle_alpha                90
_cell_angle_beta                 102.677(3)
_cell_angle_gamma                90
_cell_volume                     1896.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    135
_cell_measurement_reflns_used    9845
_cell_measurement_theta_min      2.3591
_cell_measurement_theta_max      29.0516
_cell_special_details            
;
;

_exptl_crystal_description       fragment
_exptl_crystal_colour            'clear colourless'

_exptl_crystal_size_max          0.174
_exptl_crystal_size_mid          0.139
_exptl_crystal_size_min          0.136
_exptl_crystal_size_rad          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.098
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_F_000             696
_exptl_absorpt_coefficient_mu    0.062
_exptl_crystal_density_meas_temp ?

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5, Bruker, 2014'
_exptl_absorpt_correction_T_min  0.6749
_exptl_absorpt_correction_T_max  0.7458

#===============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
;
Diffractometer operator             Philipp J. Altmann	
scanspeed                           5 s per frame
dx                                  36 mm
1272 frames measured in 8 data sets
phi-scans with delta_phi         = 0.5
omega-scans with delta_omega     = 0.5
shutterless mode
;
_diffrn_ambient_temperature      135
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'TXS rotating anode'
_diffrn_radiation_monochromator  'Helios optic'


_diffrn_measurement_device       ' κ-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker Photon CMOS '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_detector                 ' CMOS plate '
_diffrn_detector_area_resol_mean 16

# number of measured reflections (redundant set)
_diffrn_reflns_number            33127
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.36
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_reduction_process 
;
;

# number of unique reflections
_reflns_number_total             3359
# number of observed reflections (> n sig(I))
_reflns_number_gt                2978
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'APEX III Control Software (Bruker, 2015)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  
'SHELXL2014 (Sheldrick, 2014), SHELXLE (Huebschle, 2011)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2014)'

#===============================================================================

# 8. REFINEMENT DATA

_refine_special_details          
;
 Refinement on F² for ALL reflections except those
 flagged by the user for potential systematic errors.
 Weighted R-factors wR and all goodnesses of fit S
 are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The
 observed criterion of F² > 2sigma(F²) is used only
 for calculating -R-factor-obs etc. and is not
 relevant to the choice of reflections for refinement.
 R-factors based on F² are statistically about twice
 as large as those based on F, and R-factors based on
 ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'W=1/[Σ²(FO²)+(0.0455P)²+0.7786P] 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_abs_structure_details ?
_refine_ls_abs_structure_Flack   .
_refine_ls_number_reflns         3359
_refine_ls_number_parameters     211
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0392
_refine_ls_wR_factor_ref         0.1002
_refine_ls_wR_factor_gt          0.0964
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.180
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.038

#===============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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
N1 N 0.22046(5) 0.43600(16) 0.28787(6) 0.0159(2) Uani 1 1 d . . . . .
C1 C 0.14052(7) 0.42585(19) 0.24058(7) 0.0165(3) Uani 1 1 d . . . . .
H1 H 0.1065 0.4816 0.2748 0.020 Uiso 1 1 calc R U . . .
C2 C 0.13009(7) 0.5763(2) 0.17012(7) 0.0202(3) Uani 1 1 d . . . . .
H2A H 0.1475 0.7204 0.1887 0.024 Uiso 1 1 calc R U . . .
H2B H 0.1628 0.5274 0.1343 0.024 Uiso 1 1 calc R U . . .
C3 C 0.04571(7) 0.5862(2) 0.12516(7) 0.0252(3) Uani 1 1 d . . . . .
H3A H 0.0139 0.6508 0.1591 0.030 Uiso 1 1 calc R U . . .
H3B H 0.0418 0.6778 0.0783 0.030 Uiso 1 1 calc R U . . .
C4 C 0.01420(7) 0.3668(2) 0.09933(7) 0.0272(3) Uani 1 1 d . . . . .
H4A H 0.0416 0.3092 0.0601 0.033 Uiso 1 1 calc R U . . .
H4B H -0.0415 0.3777 0.0741 0.033 Uiso 1 1 calc R U . . .
C5 C 0.02466(7) 0.2161(2) 0.16935(8) 0.0264(3) Uani 1 1 d . . . . .
H5A H 0.0066 0.0725 0.1507 0.032 Uiso 1 1 calc R U . . .
H5B H -0.0075 0.2656 0.2057 0.032 Uiso 1 1 calc R U . . .
C6 C 0.10950(7) 0.2040(2) 0.21360(7) 0.0218(3) Uani 1 1 d . . . . .
H6A H 0.1411 0.1420 0.1789 0.026 Uiso 1 1 calc R U . . .
H6B H 0.1139 0.1101 0.2599 0.026 Uiso 1 1 calc R U . . .
C7 C 0.22710(6) 0.45336(18) 0.37318(7) 0.0153(3) Uani 1 1 d . . . . .
H7 H 0.2832 0.4341 0.3981 0.018 Uiso 1 1 calc R U . . .
C8 C 0.18288(7) 0.28653(19) 0.41043(7) 0.0180(3) Uani 1 1 d . . . . .
H8A H 0.1266 0.3022 0.3888 0.022 Uiso 1 1 calc R U . . .
H8B H 0.1984 0.1424 0.3972 0.022 Uiso 1 1 calc R U . . .
C9 C 0.19980(7) 0.3126(2) 0.49987(7) 0.0223(3) Uani 1 1 d . . . . .
H9A H 0.1688 0.2084 0.5224 0.027 Uiso 1 1 calc R U . . .
H9B H 0.2552 0.2830 0.5220 0.027 Uiso 1 1 calc R U . . .
C10 C 0.18053(9) 0.5363(2) 0.52297(8) 0.0295(3) Uani 1 1 d . . . . .
H10A H 0.1239 0.5589 0.5071 0.035 Uiso 1 1 calc R U . . .
H10B H 0.1960 0.5515 0.5808 0.035 Uiso 1 1 calc R U . . .
C11 C 0.22167(8) 0.7043(2) 0.48448(7) 0.0262(3) Uani 1 1 d . . . . .
H11A H 0.2782 0.6948 0.5062 0.031 Uiso 1 1 calc R U . . .
H11B H 0.2042 0.8470 0.4970 0.031 Uiso 1 1 calc R U . . .
C12 C 0.20545(7) 0.67665(19) 0.39514(7) 0.0191(3) Uani 1 1 d . . . . .
H12A H 0.1498 0.7022 0.3726 0.023 Uiso 1 1 calc R U . . .
H12B H 0.2357 0.7826 0.3725 0.023 Uiso 1 1 calc R U . . .
C13 C 0.27609(7) 0.2870(2) 0.26556(7) 0.0194(3) Uani 1 1 d . . . . .
H13A H 0.2659 0.2755 0.2076 0.023 Uiso 1 1 calc R U . . .
H13B H 0.2693 0.1444 0.2870 0.023 Uiso 1 1 calc R U . . .
C14 C 0.35870(7) 0.3623(2) 0.29677(7) 0.0199(3) Uani 1 1 d . . . . .
C15 C 0.40763(7) 0.2629(2) 0.36120(7) 0.0218(3) Uani 1 1 d . . . . .
C16 C 0.48000(7) 0.3534(2) 0.39339(8) 0.0253(3) Uani 1 1 d . . . . .
H16 H 0.5125 0.2876 0.4376 0.030 Uiso 1 1 calc R U . . .
C17 C 0.50561(7) 0.5356(2) 0.36268(8) 0.0262(3) Uani 1 1 d . . . . .
C18 C 0.45852(7) 0.6244(2) 0.29613(8) 0.0263(3) Uani 1 1 d . . . . .
H18 H 0.4765 0.7449 0.2725 0.032 Uiso 1 1 calc R U . . .
C19 C 0.38569(7) 0.5415(2) 0.26313(7) 0.0238(3) Uani 1 1 d . . . . .
C20 C 0.38475(8) 0.0628(2) 0.39846(8) 0.0285(3) Uani 1 1 d . . . . .
H20A H 0.3716 -0.0485 0.3585 0.043 Uiso 1 1 calc R U . . .
H20B H 0.3398 0.0921 0.4210 0.043 Uiso 1 1 calc R U . . .
H20C H 0.4281 0.0151 0.4401 0.043 Uiso 1 1 calc R U . . .
C21 C 0.58204(8) 0.6371(3) 0.39992(9) 0.0364(4) Uani 1 1 d . . . . .
H21A H 0.6182 0.6207 0.3650 0.055 Uiso 1 1 calc R U . . .
H21B H 0.6035 0.5682 0.4504 0.055 Uiso 1 1 calc R U . . .
H21C H 0.5741 0.7886 0.4086 0.055 Uiso 1 1 calc R U . . .
C22 C 0.33729(8) 0.6508(3) 0.19222(9) 0.0338(3) Uani 1 1 d . . . . .
H22A H 0.3688 0.7574 0.1727 0.051 Uiso 1 1 calc R U . . .
H22B H 0.2929 0.7203 0.2069 0.051 Uiso 1 1 calc R U . . .
H22C H 0.3187 0.5456 0.1510 0.051 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
N1 C7 1.4707(14) . ?
N1 C13 1.4728(15) . ?
N1 C1 1.4744(15) . ?
C1 C2 1.5304(16) . ?
C1 C6 1.5363(17) . ?
C1 H1 1.0000 . ?
C2 C3 1.5282(17) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.520(2) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.5252(19) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.5320(17) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C12 1.5278(16) . ?
C7 C8 1.5365(16) . ?
C7 H7 1.0000 . ?
C8 C9 1.5314(16) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.5240(18) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.5210(19) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.5312(17) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.5196(17) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C19 1.4031(18) . ?
C14 C15 1.4062(18) . ?
C15 C16 1.4017(18) . ?
C15 C20 1.5126(19) . ?
C16 C17 1.384(2) . ?
C16 H16 0.9500 . ?
C17 C18 1.389(2) . ?
C17 C21 1.5081(19) . ?
C18 C19 1.3926(18) . ?
C18 H18 0.9500 . ?
C19 C22 1.5073(19) . ?
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 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 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
C7 N1 C13 113.89(9) . . ?
C7 N1 C1 115.03(9) . . ?
C13 N1 C1 116.08(9) . . ?
N1 C1 C2 110.74(9) . . ?
N1 C1 C6 116.44(10) . . ?
C2 C1 C6 110.16(10) . . ?
N1 C1 H1 106.3 . . ?
C2 C1 H1 106.3 . . ?
C6 C1 H1 106.3 . . ?
C3 C2 C1 111.67(10) . . ?
C3 C2 H2A 109.3 . . ?
C1 C2 H2A 109.3 . . ?
C3 C2 H2B 109.3 . . ?
C1 C2 H2B 109.3 . . ?
H2A C2 H2B 107.9 . . ?
C4 C3 C2 111.64(11) . . ?
C4 C3 H3A 109.3 . . ?
C2 C3 H3A 109.3 . . ?
C4 C3 H3B 109.3 . . ?
C2 C3 H3B 109.3 . . ?
H3A C3 H3B 108.0 . . ?
C3 C4 C5 110.82(10) . . ?
C3 C4 H4A 109.5 . . ?
C5 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C5 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
C4 C5 C6 111.58(10) . . ?
C4 C5 H5A 109.3 . . ?
C6 C5 H5A 109.3 . . ?
C4 C5 H5B 109.3 . . ?
C6 C5 H5B 109.3 . . ?
H5A C5 H5B 108.0 . . ?
C5 C6 C1 110.72(10) . . ?
C5 C6 H6A 109.5 . . ?
C1 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C1 C6 H6B 109.5 . . ?
H6A C6 H6B 108.1 . . ?
N1 C7 C12 110.69(9) . . ?
N1 C7 C8 116.23(9) . . ?
C12 C7 C8 110.11(9) . . ?
N1 C7 H7 106.4 . . ?
C12 C7 H7 106.4 . . ?
C8 C7 H7 106.4 . . ?
C9 C8 C7 110.71(10) . . ?
C9 C8 H8A 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?
C10 C9 C8 111.30(10) . . ?
C10 C9 H9A 109.4 . . ?
C8 C9 H9A 109.4 . . ?
C10 C9 H9B 109.4 . . ?
C8 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
C11 C10 C9 111.66(10) . . ?
C11 C10 H10A 109.3 . . ?
C9 C10 H10A 109.3 . . ?
C11 C10 H10B 109.3 . . ?
C9 C10 H10B 109.3 . . ?
H10A C10 H10B 107.9 . . ?
C10 C11 C12 111.67(11) . . ?
C10 C11 H11A 109.3 . . ?
C12 C11 H11A 109.3 . . ?
C10 C11 H11B 109.3 . . ?
C12 C11 H11B 109.3 . . ?
H11A C11 H11B 107.9 . . ?
C7 C12 C11 111.00(10) . . ?
C7 C12 H12A 109.4 . . ?
C11 C12 H12A 109.4 . . ?
C7 C12 H12B 109.4 . . ?
C11 C12 H12B 109.4 . . ?
H12A C12 H12B 108.0 . . ?
N1 C13 C14 110.68(10) . . ?
N1 C13 H13A 109.5 . . ?
C14 C13 H13A 109.5 . . ?
N1 C13 H13B 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 108.1 . . ?
C19 C14 C15 119.06(11) . . ?
C19 C14 C13 119.35(11) . . ?
C15 C14 C13 121.52(11) . . ?
C16 C15 C14 119.18(12) . . ?
C16 C15 C20 118.26(12) . . ?
C14 C15 C20 122.55(11) . . ?
C17 C16 C15 122.01(12) . . ?
C17 C16 H16 119.0 . . ?
C15 C16 H16 119.0 . . ?
C16 C17 C18 118.01(12) . . ?
C16 C17 C21 121.58(13) . . ?
C18 C17 C21 120.41(13) . . ?
C17 C18 C19 121.70(13) . . ?
C17 C18 H18 119.1 . . ?
C19 C18 H18 119.1 . . ?
C18 C19 C14 119.86(12) . . ?
C18 C19 C22 118.42(12) . . ?
C14 C19 C22 121.72(12) . . ?
C15 C20 H20A 109.5 . . ?
C15 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C15 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C17 C21 H21A 109.5 . . ?
C17 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C17 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 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
C7 N1 C1 C2 133.71(10) . . . . ?
C13 N1 C1 C2 -89.73(12) . . . . ?
C7 N1 C1 C6 -99.43(12) . . . . ?
C13 N1 C1 C6 37.14(14) . . . . ?
N1 C1 C2 C3 -173.97(10) . . . . ?
C6 C1 C2 C3 55.77(13) . . . . ?
C1 C2 C3 C4 -55.55(14) . . . . ?
C2 C3 C4 C5 54.82(14) . . . . ?
C3 C4 C5 C6 -55.69(15) . . . . ?
C4 C5 C6 C1 56.68(14) . . . . ?
N1 C1 C6 C5 176.72(9) . . . . ?
C2 C1 C6 C5 -56.12(13) . . . . ?
C13 N1 C7 C12 148.36(10) . . . . ?
C1 N1 C7 C12 -74.12(12) . . . . ?
C13 N1 C7 C8 -85.07(12) . . . . ?
C1 N1 C7 C8 52.45(13) . . . . ?
N1 C7 C8 C9 175.64(9) . . . . ?
C12 C7 C8 C9 -57.50(13) . . . . ?
C7 C8 C9 C10 56.26(13) . . . . ?
C8 C9 C10 C11 -54.43(15) . . . . ?
C9 C10 C11 C12 54.02(15) . . . . ?
N1 C7 C12 C11 -173.05(10) . . . . ?
C8 C7 C12 C11 57.05(13) . . . . ?
C10 C11 C12 C7 -55.57(14) . . . . ?
C7 N1 C13 C14 -63.20(13) . . . . ?
C1 N1 C13 C14 159.75(10) . . . . ?
N1 C13 C14 C19 -70.96(14) . . . . ?
N1 C13 C14 C15 105.86(13) . . . . ?
C19 C14 C15 C16 4.20(17) . . . . ?
C13 C14 C15 C16 -172.63(11) . . . . ?
C19 C14 C15 C20 -176.89(11) . . . . ?
C13 C14 C15 C20 6.28(18) . . . . ?
C14 C15 C16 C17 -1.39(18) . . . . ?
C20 C15 C16 C17 179.66(12) . . . . ?
C15 C16 C17 C18 -2.45(19) . . . . ?
C15 C16 C17 C21 177.25(12) . . . . ?
C16 C17 C18 C19 3.51(19) . . . . ?
C21 C17 C18 C19 -176.19(12) . . . . ?
C17 C18 C19 C14 -0.71(19) . . . . ?
C17 C18 C19 C22 178.36(13) . . . . ?
C15 C14 C19 C18 -3.20(18) . . . . ?
C13 C14 C19 C18 173.70(11) . . . . ?
C15 C14 C19 C22 177.77(12) . . . . ?
C13 C14 C19 C22 -5.33(18) . . . . ?


####################################################################### 
# 
# 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_mo_grumi3_0m-auto
_database_code_depnum_ccdc_archive 'CCDC 1538676'
_audit_update_record             
;
2017-08-10 deposited with the CCDC.
2018-02-20 downloaded from the CCDC.
;

#===============================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
;
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H33 N8 Ni'
# Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)'
_chemical_formula_structural     ?
_chemical_formula_sum            'C33 H33 N8 Ni'
_chemical_formula_iupac          ?
_chemical_formula_weight         600.36
_chemical_compound_source        'see text'

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'

#===============================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_Int_Tables_number      19

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 1/2-x,-y,1/2+z
3 1/2+x,1/2-y,-z
4 -x,1/2+y,1/2-z

_cell_length_a                   10.1802(7)
_cell_length_b                   20.4136(17)
_cell_length_c                   26.689(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5546.4(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    100
_cell_measurement_reflns_used    9615
_cell_measurement_theta_min      2.3622
_cell_measurement_theta_max      25.2668
_cell_special_details            
;
;

_exptl_crystal_description       needle
_exptl_crystal_colour            green

_exptl_crystal_size_max          0.417
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.040
_exptl_crystal_size_rad          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_F_000             2520
_exptl_absorpt_coefficient_mu    0.739
_exptl_crystal_density_meas_temp ?

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5, Bruker, 2014'
_exptl_absorpt_correction_T_min  0.6534
_exptl_absorpt_correction_T_max  0.7452

#===============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
;
Diffractometer operator             Philipp J. Altmann
scanspeed                           90 s per frame
dx                                  53 mm
2322 frames measured in 10 data sets
phi-scans with delta_phi         = 0.6
omega-scans with delta_omega     = 0.6
shutterless mode
;
_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'IMS microsource'
_diffrn_radiation_monochromator  'Helios optic'


_diffrn_measurement_device       ' κ-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker Photon CMOS '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_detector                 ' CMOS plate '
_diffrn_detector_area_resol_mean 16

# number of measured reflections (redundant set)
_diffrn_reflns_number            192057
_diffrn_reflns_av_R_equivalents  0.0857
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.24
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_reduction_process 
;
;

# number of unique reflections
_reflns_number_total             9767
# number of observed reflections (> n sig(I))
_reflns_number_gt                8669
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'APEX III Control Software (Bruker, 2015)'
_computing_cell_refinement       'SAINT (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2015)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  
'SHELXL2014 (Sheldrick, 2014), SHELXLE (Huebschle, 2011)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2014)'

#===============================================================================

# 8. REFINEMENT DATA

_refine_special_details          
;
 Refinement on F² for ALL reflections except those
 flagged by the user for potential systematic errors.
 Weighted R-factors wR and all goodnesses of fit S
 are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The
 observed criterion of F² > 2sigma(F²) is used only
 for calculating -R-factor-obs etc. and is not
 relevant to the choice of reflections for refinement.
 R-factors based on F² are statistically about twice
 as large as those based on F, and R-factors based on
 ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'W=1/[Σ²(FO²)+(0.0248P)²+6.2581P] 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_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.000

_chemical_absolute_configuration ?

_refine_ls_number_reflns         9767
_refine_ls_number_parameters     773
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0308
_refine_ls_wR_factor_ref         0.0711
_refine_ls_wR_factor_gt          0.0692
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_restrained_S_all      0.946
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.221
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.052

#===============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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 0.08690(4) 0.62951(2) 0.68103(2) 0.01110(11) Uani 1 1 d . . . . .
N1 N 0.1713(3) 0.58441(15) 0.73404(11) 0.0116(7) Uani 1 1 d . . . . .
N2 N 0.1683(3) 0.57832(15) 0.82395(12) 0.0158(7) Uani 1 1 d . . . . .
N3 N 0.3001(3) 0.50861(15) 0.68689(12) 0.0156(7) Uani 1 1 d . . . . .
N4 N 0.1898(3) 0.58606(15) 0.63330(11) 0.0119(7) Uani 1 1 d . . . . .
N5 N -0.0054(3) 0.67678(15) 0.63237(11) 0.0114(7) Uani 1 1 d . . . . .
N6 N -0.1685(3) 0.72830(15) 0.68450(12) 0.0152(7) Uani 1 1 d . . . . .
N7 N -0.0112(3) 0.66952(15) 0.73284(11) 0.0116(7) Uani 1 1 d . . . . .
N8 N -0.0182(3) 0.67473(15) 0.82282(12) 0.0155(7) Uani 1 1 d . . . . .
C1 C 0.1316(4) 0.60228(18) 0.78125(14) 0.0136(9) Uani 1 1 d . . . . .
C2 C 0.2572(4) 0.52727(18) 0.82161(15) 0.0141(8) Uani 1 1 d . . . . .
C3 C 0.2961(4) 0.49685(19) 0.86639(15) 0.0180(9) Uani 1 1 d . . . . .
H3 H 0.2635 0.5124 0.8976 0.022 Uiso 1 1 calc R U . . .
C4 C 0.3806(4) 0.44498(19) 0.86523(15) 0.0203(10) Uani 1 1 d . . . . .
H4 H 0.4051 0.4239 0.8956 0.024 Uiso 1 1 calc R U . . .
C5 C 0.4318(4) 0.42242(18) 0.81922(15) 0.0220(9) Uani 1 1 d . . . . .
H5 H 0.4922 0.3870 0.8188 0.026 Uiso 1 1 calc R U . . .
C6 C 0.3950(4) 0.45126(19) 0.77534(15) 0.0196(9) Uani 1 1 d . . . . .
H6 H 0.4301 0.4360 0.7445 0.023 Uiso 1 1 calc R U . . .
C7 C 0.3046(4) 0.50388(19) 0.77555(15) 0.0149(9) Uani 1 1 d . . . . .
C8 C 0.2578(4) 0.53364(19) 0.73036(15) 0.0129(8) Uani 1 1 d . . . . .
C9 C 0.2670(4) 0.53382(19) 0.64344(14) 0.0138(9) Uani 1 1 d . . . . .
C10 C 0.3132(4) 0.50136(19) 0.59562(15) 0.0158(9) Uani 1 1 d . . . . .
C11 C 0.2092(5) 0.44893(19) 0.58261(16) 0.0231(10) Uani 1 1 d . . . . .
H11A H 0.1244 0.4702 0.5767 0.035 Uiso 1 1 calc R U . . .
H11B H 0.2010 0.4180 0.6105 0.035 Uiso 1 1 calc R U . . .
H11C H 0.2363 0.4253 0.5524 0.035 Uiso 1 1 calc R U . . .
C12 C 0.4470(4) 0.4690(2) 0.60113(15) 0.0211(9) Uani 1 1 d . . . . .
H12A H 0.4774 0.4538 0.5683 0.032 Uiso 1 1 calc R U . . .
H12B H 0.4400 0.4316 0.6240 0.032 Uiso 1 1 calc R U . . .
H12C H 0.5099 0.5008 0.6147 0.032 Uiso 1 1 calc R U . . .
C13 C 0.3067(4) 0.55979(18) 0.55868(14) 0.0133(8) Uani 1 1 d . . . . .
C14 C 0.2806(4) 0.5410(2) 0.50410(14) 0.0166(9) Uani 1 1 d . . . . .
H14A H 0.2838 0.5804 0.4831 0.025 Uiso 1 1 calc R U . . .
H14B H 0.1936 0.5208 0.5014 0.025 Uiso 1 1 calc R U . . .
H14C H 0.3477 0.5099 0.4928 0.025 Uiso 1 1 calc R U . . .
C15 C 0.4333(4) 0.60022(18) 0.56160(15) 0.0172(9) Uani 1 1 d . . . . .
H15A H 0.5062 0.5750 0.5474 0.026 Uiso 1 1 calc R U . . .
H15B H 0.4526 0.6106 0.5967 0.026 Uiso 1 1 calc R U . . .
H15C H 0.4222 0.6409 0.5426 0.026 Uiso 1 1 calc R U . . .
C16 C 0.1975(4) 0.59950(18) 0.58233(14) 0.0137(8) Uani 1 1 d . . . . .
C17 C 0.1195(4) 0.64472(18) 0.55880(14) 0.0150(9) Uani 1 1 d . . . . .
H17 H 0.1333 0.6515 0.5240 0.018 Uiso 1 1 calc R U . . .
C18 C 0.0228(4) 0.68103(18) 0.58155(14) 0.0127(8) Uani 1 1 d . . . . .
C19 C -0.0630(4) 0.73268(18) 0.55715(13) 0.0138(8) Uani 1 1 d . . . . .
C20 C -0.0944(4) 0.71974(19) 0.50244(13) 0.0161(8) Uani 1 1 d . . . . .
H20A H -0.1599 0.7515 0.4908 0.024 Uiso 1 1 calc R U . . .
H20B H -0.1295 0.6753 0.4988 0.024 Uiso 1 1 calc R U . . .
H20C H -0.0142 0.7241 0.4824 0.024 Uiso 1 1 calc R U . . .
C21 C 0.0075(4) 0.79918(19) 0.56186(15) 0.0188(9) Uani 1 1 d . . . . .
H21A H 0.0921 0.7971 0.5444 0.028 Uiso 1 1 calc R U . . .
H21B H 0.0222 0.8092 0.5973 0.028 Uiso 1 1 calc R U . . .
H21C H -0.0470 0.8335 0.5468 0.028 Uiso 1 1 calc R U . . .
C22 C -0.1831(4) 0.73006(19) 0.59273(14) 0.0158(9) Uani 1 1 d . . . . .
C23 C -0.2746(4) 0.6723(2) 0.58002(15) 0.0205(10) Uani 1 1 d . . . . .
H23A H -0.3235 0.6822 0.5493 0.031 Uiso 1 1 calc R U . . .
H23B H -0.3363 0.6653 0.6077 0.031 Uiso 1 1 calc R U . . .
H23C H -0.2220 0.6326 0.5750 0.031 Uiso 1 1 calc R U . . .
C24 C -0.2637(4) 0.7925(2) 0.59722(15) 0.0208(10) Uani 1 1 d . . . . .
H24A H -0.2968 0.8050 0.5641 0.031 Uiso 1 1 calc R U . . .
H24B H -0.2084 0.8277 0.6106 0.031 Uiso 1 1 calc R U . . .
H24C H -0.3379 0.7849 0.6199 0.031 Uiso 1 1 calc R U . . .
C25 C -0.1158(4) 0.71155(18) 0.64146(14) 0.0128(8) Uani 1 1 d . . . . .
C26 C -0.1157(4) 0.71060(18) 0.72817(14) 0.0140(8) Uani 1 1 d . . . . .
C27 C -0.1743(4) 0.73682(19) 0.77307(15) 0.0140(8) Uani 1 1 d . . . . .
C28 C -0.2806(4) 0.7806(2) 0.77124(16) 0.0208(9) Uani 1 1 d . . . . .
H28 H -0.3174 0.7929 0.7399 0.025 Uiso 1 1 calc R U . . .
C29 C -0.3310(4) 0.80556(19) 0.81494(16) 0.0222(9) Uani 1 1 d . . . . .
H29 H -0.4030 0.8352 0.8138 0.027 Uiso 1 1 calc R U . . .
C30 C -0.2772(4) 0.7877(2) 0.86111(15) 0.0187(9) Uani 1 1 d . . . . .
H30 H -0.3128 0.8053 0.8911 0.022 Uiso 1 1 calc R U . . .
C31 C -0.1742(4) 0.7451(2) 0.86356(15) 0.0188(9) Uani 1 1 d . . . . .
H31 H -0.1383 0.7332 0.8951 0.023 Uiso 1 1 calc R U . . .
C32 C -0.1210(4) 0.71877(17) 0.81917(15) 0.0148(8) Uani 1 1 d . . . . .
C33 C 0.0286(4) 0.65314(18) 0.78066(14) 0.0133(8) Uani 1 1 d . . . . .
Ni2 Ni 0.94859(4) 0.37812(2) 0.33110(2) 0.01138(11) Uani 1 1 d . . . . .
N9 N 1.0280(3) 0.33509(15) 0.27593(11) 0.0126(7) Uani 1 1 d . . . . .
N10 N 1.0171(3) 0.33276(15) 0.18621(12) 0.0150(7) Uani 1 1 d . . . . .
N11 N 1.1601(3) 0.25726(14) 0.31951(12) 0.0152(7) Uani 1 1 d . . . . .
N12 N 1.0553(3) 0.33236(14) 0.37657(11) 0.0118(7) Uani 1 1 d . . . . .
N13 N 0.8597(3) 0.42340(15) 0.38191(11) 0.0126(7) Uani 1 1 d . . . . .
N14 N 0.6931(3) 0.47721(15) 0.33295(12) 0.0151(7) Uani 1 1 d . . . . .
N15 N 0.8475(3) 0.42097(15) 0.28141(11) 0.0124(7) Uani 1 1 d . . . . .
N16 N 0.8391(3) 0.43352(16) 0.19217(12) 0.0171(7) Uani 1 1 d . . . . .
C34 C 0.9851(4) 0.35573(18) 0.22969(14) 0.0134(8) Uani 1 1 d . . . . .
C35 C 1.1003(4) 0.27922(17) 0.18603(14) 0.0135(8) Uani 1 1 d . . . . .
C36 C 1.1323(4) 0.24974(19) 0.14005(14) 0.0153(9) Uani 1 1 d . . . . .
H36 H 1.1001 0.2679 0.1097 0.018 Uiso 1 1 calc R U . . .
C37 C 1.2096(4) 0.19510(19) 0.13894(15) 0.0175(9) Uani 1 1 d . . . . .
H37 H 1.2295 0.1748 0.1078 0.021 Uiso 1 1 calc R U . . .
C38 C 1.2600(4) 0.1686(2) 0.18369(16) 0.0214(9) Uani 1 1 d . . . . .
H38 H 1.3146 0.1309 0.1825 0.026 Uiso 1 1 calc R U . . .
C39 C 1.2308(4) 0.1968(2) 0.22890(16) 0.0199(9) Uani 1 1 d . . . . .
H39 H 1.2657 0.1789 0.2589 0.024 Uiso 1 1 calc R U . . .
C40 C 1.1489(4) 0.25252(19) 0.23078(14) 0.0145(8) Uani 1 1 d . . . . .
C41 C 1.1114(4) 0.28301(19) 0.27742(14) 0.0151(9) Uani 1 1 d . . . . .
C42 C 1.1334(4) 0.28105(18) 0.36407(14) 0.0137(9) Uani 1 1 d . . . . .
C43 C 1.1872(4) 0.24748(18) 0.41029(14) 0.0147(8) Uani 1 1 d . . . . .
C44 C 1.3238(4) 0.2187(2) 0.40223(15) 0.0223(10) Uani 1 1 d . . . . .
H44A H 1.3191 0.1835 0.3773 0.033 Uiso 1 1 calc R U . . .
H44B H 1.3569 0.2011 0.4340 0.033 Uiso 1 1 calc R U . . .
H44C H 1.3832 0.2531 0.3902 0.033 Uiso 1 1 calc R U . . .
C45 C 1.0907(4) 0.19177(18) 0.42272(15) 0.0221(9) Uani 1 1 d . . . . .
H45A H 1.0035 0.2102 0.4293 0.033 Uiso 1 1 calc R U . . .
H45B H 1.1215 0.1682 0.4525 0.033 Uiso 1 1 calc R U . . .
H45C H 1.0856 0.1615 0.3943 0.033 Uiso 1 1 calc R U . . .
C46 C 1.1785(4) 0.30386(18) 0.44933(14) 0.0142(8) Uani 1 1 d . . . . .
C47 C 1.3020(4) 0.34669(19) 0.44771(15) 0.0183(9) Uani 1 1 d . . . . .
H47A H 1.3203 0.3594 0.4130 0.027 Uiso 1 1 calc R U . . .
H47B H 1.3767 0.3220 0.4611 0.027 Uiso 1 1 calc R U . . .
H47C H 1.2879 0.3861 0.4680 0.027 Uiso 1 1 calc R U . . .
C48 C 1.1559(4) 0.28091(19) 0.50310(14) 0.0180(9) Uani 1 1 d . . . . .
H48A H 1.0706 0.2589 0.5054 0.027 Uiso 1 1 calc R U . . .
H48B H 1.1570 0.3188 0.5257 0.027 Uiso 1 1 calc R U . . .
H48C H 1.2257 0.2503 0.5128 0.027 Uiso 1 1 calc R U . . .
C49 C 1.0666(4) 0.34343(17) 0.42755(13) 0.0132(8) Uani 1 1 d . . . . .
C50 C 0.9900(4) 0.38787(18) 0.45320(14) 0.0157(9) Uani 1 1 d . . . . .
H50 H 1.0062 0.3930 0.4880 0.019 Uiso 1 1 calc R U . . .
C51 C 0.8920(4) 0.42524(18) 0.43238(14) 0.0137(8) Uani 1 1 d . . . . .
C52 C 0.8063(4) 0.47460(19) 0.45937(15) 0.0157(9) Uani 1 1 d . . . . .
C53 C 0.8728(4) 0.54220(19) 0.45800(16) 0.0238(10) Uani 1 1 d . . . . .
H53A H 0.8895 0.5547 0.4231 0.036 Uiso 1 1 calc R U . . .
H53B H 0.9562 0.5403 0.4763 0.036 Uiso 1 1 calc R U . . .
H53C H 0.8152 0.5747 0.4737 0.036 Uiso 1 1 calc R U . . .
C54 C 0.7797(4) 0.4572(2) 0.51402(14) 0.0213(10) Uani 1 1 d . . . . .
H54A H 0.7539 0.4111 0.5164 0.032 Uiso 1 1 calc R U . . .
H54B H 0.7088 0.4849 0.5270 0.032 Uiso 1 1 calc R U . . .
H54C H 0.8595 0.4645 0.5338 0.032 Uiso 1 1 calc R U . . .
C55 C 0.6845(4) 0.47406(18) 0.42468(14) 0.0146(8) Uani 1 1 d . . . . .
C56 C 0.6033(4) 0.5368(2) 0.42316(15) 0.0225(9) Uani 1 1 d . . . . .
H56A H 0.6573 0.5727 0.4100 0.034 Uiso 1 1 calc R U . . .
H56B H 0.5737 0.5478 0.4571 0.034 Uiso 1 1 calc R U . . .
H56C H 0.5268 0.5304 0.4014 0.034 Uiso 1 1 calc R U . . .
C57 C 0.5925(4) 0.41632(19) 0.43667(15) 0.0208(9) Uani 1 1 d . . . . .
H57A H 0.5317 0.4096 0.4087 0.031 Uiso 1 1 calc R U . . .
H57B H 0.5424 0.4261 0.4671 0.031 Uiso 1 1 calc R U . . .
H57C H 0.6447 0.3766 0.4418 0.031 Uiso 1 1 calc R U . . .
C58 C 0.7489(4) 0.45814(18) 0.37515(15) 0.0132(9) Uani 1 1 d . . . . .
C59 C 0.7436(4) 0.46183(19) 0.28826(14) 0.0129(9) Uani 1 1 d . . . . .
C60 C 0.6822(4) 0.49079(19) 0.24472(15) 0.0146(8) Uani 1 1 d . . . . .
C61 C 0.5735(4) 0.53336(19) 0.24862(15) 0.0181(9) Uani 1 1 d . . . . .
H61 H 0.5341 0.5415 0.2803 0.022 Uiso 1 1 calc R U . . .
C62 C 0.5252(4) 0.56295(19) 0.20627(15) 0.0197(9) Uani 1 1 d . . . . .
H62 H 0.4522 0.5918 0.2087 0.024 Uiso 1 1 calc R U . . .
C63 C 0.5827(4) 0.55096(19) 0.15954(15) 0.0210(9) Uani 1 1 d . . . . .
H63 H 0.5500 0.5726 0.1306 0.025 Uiso 1 1 calc R U . . .
C64 C 0.6853(4) 0.50846(19) 0.15515(15) 0.0197(9) Uani 1 1 d . . . . .
H64 H 0.7219 0.4998 0.1231 0.024 Uiso 1 1 calc R U . . .
C65 C 0.7369(4) 0.47750(19) 0.19765(15) 0.0160(9) Uani 1 1 d . . . . .
C66 C 0.8846(4) 0.40798(18) 0.23290(14) 0.0129(8) 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
Ni1 N5 1.871(3) . ?
Ni1 N4 1.873(3) . ?
Ni1 N7 1.891(3) . ?
Ni1 N1 1.894(3) . ?
N1 C8 1.363(5) . ?
N1 C1 1.373(5) . ?
N2 C1 1.295(5) . ?
N2 C2 1.381(5) . ?
N3 C9 1.313(5) . ?
N3 C8 1.339(5) . ?
N4 C9 1.352(5) . ?
N4 C16 1.390(5) . ?
N5 C25 1.351(5) . ?
N5 C18 1.389(5) . ?
N6 C25 1.314(5) . ?
N6 C26 1.333(5) . ?
N7 C26 1.360(5) . ?
N7 C33 1.380(5) . ?
N8 C33 1.299(5) . ?
N8 C32 1.383(5) . ?
C1 C33 1.475(5) . ?
C2 C3 1.404(5) . ?
C2 C7 1.404(6) . ?
C3 C4 1.365(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.411(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.363(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.414(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.432(5) . ?
C9 C10 1.513(5) . ?
C10 C12 1.521(6) . ?
C10 C11 1.545(6) . ?
C10 C13 1.549(5) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C16 1.513(5) . ?
C13 C14 1.530(5) . ?
C13 C15 1.533(5) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.370(5) . ?
C17 C18 1.374(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.516(5) . ?
C19 C20 1.518(5) . ?
C19 C21 1.541(5) . ?
C19 C22 1.549(5) . ?
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 C25 1.518(5) . ?
C22 C24 1.520(5) . ?
C22 C23 1.541(5) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C26 C27 1.442(5) . ?
C27 C32 1.394(6) . ?
C27 C28 1.405(6) . ?
C28 C29 1.372(6) . ?
C28 H28 0.9500 . ?
C29 C30 1.397(6) . ?
C29 H29 0.9500 . ?
C30 C31 1.364(6) . ?
C30 H30 0.9500 . ?
C31 C32 1.409(5) . ?
C31 H31 0.9500 . ?
Ni2 N13 1.874(3) . ?
Ni2 N12 1.878(3) . ?
Ni2 N15 1.893(3) . ?
Ni2 N9 1.896(3) . ?
N9 C41 1.361(5) . ?
N9 C34 1.375(5) . ?
N10 C34 1.293(5) . ?
N10 C35 1.383(5) . ?
N11 C42 1.313(5) . ?
N11 C41 1.336(5) . ?
N12 C42 1.356(5) . ?
N12 C49 1.384(5) . ?
N13 C58 1.344(5) . ?
N13 C51 1.387(5) . ?
N14 C58 1.320(5) . ?
N14 C59 1.336(5) . ?
N15 C59 1.360(5) . ?
N15 C66 1.375(5) . ?
N16 C66 1.292(5) . ?
N16 C65 1.382(5) . ?
C34 C66 1.480(5) . ?
C35 C40 1.403(5) . ?
C35 C36 1.405(5) . ?
C36 C37 1.366(6) . ?
C36 H36 0.9500 . ?
C37 C38 1.408(6) . ?
C37 H37 0.9500 . ?
C38 C39 1.370(6) . ?
C38 H38 0.9500 . ?
C39 C40 1.410(6) . ?
C39 H39 0.9500 . ?
C40 C41 1.443(5) . ?
C42 C43 1.514(5) . ?
C43 C44 1.524(6) . ?
C43 C45 1.539(5) . ?
C43 C46 1.555(5) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 C49 1.513(5) . ?
C46 C48 1.527(5) . ?
C46 C47 1.532(6) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 C50 1.378(5) . ?
C50 C51 1.373(5) . ?
C50 H50 0.9500 . ?
C51 C52 1.515(5) . ?
C52 C54 1.525(5) . ?
C52 C53 1.538(5) . ?
C52 C55 1.548(6) . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 C58 1.511(5) . ?
C55 C56 1.525(5) . ?
C55 C57 1.539(5) . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C59 C60 1.446(5) . ?
C60 C65 1.401(6) . ?
C60 C61 1.410(6) . ?
C61 C62 1.373(5) . ?
C61 H61 0.9500 . ?
C62 C63 1.399(6) . ?
C62 H62 0.9500 . ?
C63 C64 1.362(6) . ?
C63 H63 0.9500 . ?
C64 C65 1.401(5) . ?
C64 H64 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 Ni1 N4 93.03(13) . . ?
N5 Ni1 N7 91.12(12) . . ?
N4 Ni1 N7 175.83(14) . . ?
N5 Ni1 N1 175.56(14) . . ?
N4 Ni1 N1 91.38(13) . . ?
N7 Ni1 N1 84.47(13) . . ?
C8 N1 C1 117.3(3) . . ?
C8 N1 Ni1 127.5(3) . . ?
C1 N1 Ni1 115.0(2) . . ?
C1 N2 C2 115.7(3) . . ?
C9 N3 C8 122.2(3) . . ?
C9 N4 C16 108.6(3) . . ?
C9 N4 Ni1 124.2(3) . . ?
C16 N4 Ni1 127.2(3) . . ?
C25 N5 C18 108.3(3) . . ?
C25 N5 Ni1 124.3(2) . . ?
C18 N5 Ni1 127.3(3) . . ?
C25 N6 C26 121.9(3) . . ?
C26 N7 C33 117.6(3) . . ?
C26 N7 Ni1 127.8(3) . . ?
C33 N7 Ni1 114.6(2) . . ?
C33 N8 C32 115.9(3) . . ?
N2 C1 N1 128.5(4) . . ?
N2 C1 C33 118.7(3) . . ?
N1 C1 C33 112.7(3) . . ?
N2 C2 C3 118.7(4) . . ?
N2 C2 C7 121.4(4) . . ?
C3 C2 C7 119.8(3) . . ?
C4 C3 C2 120.1(4) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 120.4(4) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C6 C5 C4 120.3(4) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C5 C6 C7 120.2(4) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 H6 119.9 . . ?
C2 C7 C6 119.0(4) . . ?
C2 C7 C8 118.6(4) . . ?
C6 C7 C8 122.4(4) . . ?
N3 C8 N1 124.1(3) . . ?
N3 C8 C7 117.4(3) . . ?
N1 C8 C7 118.5(3) . . ?
N3 C9 N4 129.4(4) . . ?
N3 C9 C10 119.6(3) . . ?
N4 C9 C10 110.9(3) . . ?
C9 C10 C12 112.8(3) . . ?
C9 C10 C11 106.3(3) . . ?
C12 C10 C11 109.6(3) . . ?
C9 C10 C13 100.7(3) . . ?
C12 C10 C13 115.7(3) . . ?
C11 C10 C13 111.2(3) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C16 C13 C14 113.8(3) . . ?
C16 C13 C15 107.9(3) . . ?
C14 C13 C15 109.2(3) . . ?
C16 C13 C10 100.3(3) . . ?
C14 C13 C10 114.9(3) . . ?
C15 C13 C10 110.3(3) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 N4 123.3(3) . . ?
C17 C16 C13 126.5(3) . . ?
N4 C16 C13 110.1(3) . . ?
C16 C17 C18 125.2(4) . . ?
C16 C17 H17 117.4 . . ?
C18 C17 H17 117.4 . . ?
C17 C18 N5 123.1(3) . . ?
C17 C18 C19 126.7(3) . . ?
N5 C18 C19 110.1(3) . . ?
C18 C19 C20 114.4(3) . . ?
C18 C19 C21 108.0(3) . . ?
C20 C19 C21 109.3(3) . . ?
C18 C19 C22 99.6(3) . . ?
C20 C19 C22 114.7(3) . . ?
C21 C19 C22 110.4(3) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C25 C22 C24 112.6(3) . . ?
C25 C22 C23 105.7(3) . . ?
C24 C22 C23 109.4(3) . . ?
C25 C22 C19 100.2(3) . . ?
C24 C22 C19 116.5(3) . . ?
C23 C22 C19 111.6(3) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N6 C25 N5 129.3(3) . . ?
N6 C25 C22 120.0(3) . . ?
N5 C25 C22 110.6(3) . . ?
N6 C26 N7 124.2(3) . . ?
N6 C26 C27 117.3(3) . . ?
N7 C26 C27 118.4(3) . . ?
C32 C27 C28 119.9(4) . . ?
C32 C27 C26 118.3(4) . . ?
C28 C27 C26 121.8(4) . . ?
C29 C28 C27 119.7(4) . . ?
C29 C28 H28 120.2 . . ?
C27 C28 H28 120.2 . . ?
C28 C29 C30 120.4(4) . . ?
C28 C29 H29 119.8 . . ?
C30 C29 H29 119.8 . . ?
C31 C30 C29 120.7(4) . . ?
C31 C30 H30 119.7 . . ?
C29 C30 H30 119.7 . . ?
C30 C31 C32 119.9(4) . . ?
C30 C31 H31 120.1 . . ?
C32 C31 H31 120.1 . . ?
N8 C32 C27 121.9(3) . . ?
N8 C32 C31 118.7(4) . . ?
C27 C32 C31 119.4(3) . . ?
N8 C33 N7 127.6(3) . . ?
N8 C33 C1 119.4(3) . . ?
N7 C33 C1 112.9(3) . . ?
N13 Ni2 N12 93.27(13) . . ?
N13 Ni2 N15 90.94(13) . . ?
N12 Ni2 N15 175.79(14) . . ?
N13 Ni2 N9 175.25(14) . . ?
N12 Ni2 N9 91.41(13) . . ?
N15 Ni2 N9 84.38(14) . . ?
C41 N9 C34 117.6(3) . . ?
C41 N9 Ni2 127.3(3) . . ?
C34 N9 Ni2 114.8(2) . . ?
C34 N10 C35 116.3(3) . . ?
C42 N11 C41 122.6(3) . . ?
C42 N12 C49 108.6(3) . . ?
C42 N12 Ni2 124.3(3) . . ?
C49 N12 Ni2 127.0(3) . . ?
C58 N13 C51 108.4(3) . . ?
C58 N13 Ni2 124.6(3) . . ?
C51 N13 Ni2 127.0(3) . . ?
C58 N14 C59 121.8(3) . . ?
C59 N15 C66 117.3(3) . . ?
C59 N15 Ni2 127.8(3) . . ?
C66 N15 Ni2 114.9(3) . . ?
C66 N16 C65 116.3(3) . . ?
N10 C34 N9 127.9(3) . . ?
N10 C34 C66 119.1(3) . . ?
N9 C34 C66 112.9(3) . . ?
N10 C35 C40 121.4(3) . . ?
N10 C35 C36 118.9(3) . . ?
C40 C35 C36 119.7(3) . . ?
C37 C36 C35 120.2(4) . . ?
C37 C36 H36 119.9 . . ?
C35 C36 H36 119.9 . . ?
C36 C37 C38 120.4(4) . . ?
C36 C37 H37 119.8 . . ?
C38 C37 H37 119.8 . . ?
C39 C38 C37 120.5(4) . . ?
C39 C38 H38 119.8 . . ?
C37 C38 H38 119.8 . . ?
C38 C39 C40 119.9(4) . . ?
C38 C39 H39 120.1 . . ?
C40 C39 H39 120.1 . . ?
C35 C40 C39 119.4(4) . . ?
C35 C40 C41 118.2(4) . . ?
C39 C40 C41 122.3(4) . . ?
N11 C41 N9 124.3(3) . . ?
N11 C41 C40 117.2(4) . . ?
N9 C41 C40 118.5(3) . . ?
N11 C42 N12 129.0(4) . . ?
N11 C42 C43 119.7(3) . . ?
N12 C42 C43 111.2(3) . . ?
C42 C43 C44 112.9(3) . . ?
C42 C43 C45 106.2(3) . . ?
C44 C43 C45 109.2(3) . . ?
C42 C43 C46 101.0(3) . . ?
C44 C43 C46 115.5(3) . . ?
C45 C43 C46 111.5(3) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C49 C46 C48 114.3(3) . . ?
C49 C46 C47 107.6(3) . . ?
C48 C46 C47 109.0(3) . . ?
C49 C46 C43 100.4(3) . . ?
C48 C46 C43 114.3(3) . . ?
C47 C46 C43 110.9(3) . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C46 C48 H48A 109.5 . . ?
C46 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C46 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C50 C49 N12 123.3(3) . . ?
C50 C49 C46 125.9(3) . . ?
N12 C49 C46 110.7(3) . . ?
C51 C50 C49 125.2(4) . . ?
C51 C50 H50 117.4 . . ?
C49 C50 H50 117.4 . . ?
C50 C51 N13 123.4(3) . . ?
C50 C51 C52 126.5(3) . . ?
N13 C51 C52 110.1(3) . . ?
C51 C52 C54 113.7(3) . . ?
C51 C52 C53 109.4(3) . . ?
C54 C52 C53 108.0(3) . . ?
C51 C52 C55 99.9(3) . . ?
C54 C52 C55 115.4(3) . . ?
C53 C52 C55 110.2(3) . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C52 C54 H54A 109.5 . . ?
C52 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C52 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C58 C55 C56 113.1(3) . . ?
C58 C55 C57 106.3(3) . . ?
C56 C55 C57 108.6(3) . . ?
C58 C55 C52 100.2(3) . . ?
C56 C55 C52 116.3(3) . . ?
C57 C55 C52 111.6(3) . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C55 C57 H57A 109.5 . . ?
C55 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C55 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
N14 C58 N13 129.1(4) . . ?
N14 C58 C55 119.7(3) . . ?
N13 C58 C55 111.1(3) . . ?
N14 C59 N15 124.3(3) . . ?
N14 C59 C60 117.1(3) . . ?
N15 C59 C60 118.6(3) . . ?
C65 C60 C61 119.8(4) . . ?
C65 C60 C59 118.0(4) . . ?
C61 C60 C59 122.1(4) . . ?
C62 C61 C60 119.4(4) . . ?
C62 C61 H61 120.3 . . ?
C60 C61 H61 120.3 . . ?
C61 C62 C63 120.5(4) . . ?
C61 C62 H62 119.8 . . ?
C63 C62 H62 119.8 . . ?
C64 C63 C62 120.6(4) . . ?
C64 C63 H63 119.7 . . ?
C62 C63 H63 119.7 . . ?
C63 C64 C65 120.3(4) . . ?
C63 C64 H64 119.8 . . ?
C65 C64 H64 119.8 . . ?
N16 C65 C60 121.3(4) . . ?
N16 C65 C64 119.3(4) . . ?
C60 C65 C64 119.3(4) . . ?
N16 C66 N15 128.0(4) . . ?
N16 C66 C34 119.4(3) . . ?
N15 C66 C34 112.5(3) . . ?

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
N4 Ni1 N1 C8 -8.3(3) . . . . ?
N7 Ni1 N1 C8 171.3(3) . . . . ?
N4 Ni1 N1 C1 177.2(3) . . . . ?
N7 Ni1 N1 C1 -3.1(3) . . . . ?
N5 Ni1 N4 C9 -168.1(3) . . . . ?
N1 Ni1 N4 C9 11.4(3) . . . . ?
N5 Ni1 N4 C16 9.6(3) . . . . ?
N1 Ni1 N4 C16 -170.9(3) . . . . ?
N4 Ni1 N5 C25 167.9(3) . . . . ?
N7 Ni1 N5 C25 -11.7(3) . . . . ?
N4 Ni1 N5 C18 -9.9(3) . . . . ?
N7 Ni1 N5 C18 170.5(3) . . . . ?
N5 Ni1 N7 C26 5.9(3) . . . . ?
N1 Ni1 N7 C26 -173.6(3) . . . . ?
N5 Ni1 N7 C33 -175.4(3) . . . . ?
N1 Ni1 N7 C33 5.0(3) . . . . ?
C2 N2 C1 N1 -1.4(6) . . . . ?
C2 N2 C1 C33 175.0(3) . . . . ?
C8 N1 C1 N2 2.2(6) . . . . ?
Ni1 N1 C1 N2 177.2(3) . . . . ?
C8 N1 C1 C33 -174.4(3) . . . . ?
Ni1 N1 C1 C33 0.7(4) . . . . ?
C1 N2 C2 C3 -176.9(3) . . . . ?
C1 N2 C2 C7 0.6(5) . . . . ?
N2 C2 C3 C4 178.0(4) . . . . ?
C7 C2 C3 C4 0.5(6) . . . . ?
C2 C3 C4 C5 1.4(6) . . . . ?
C3 C4 C5 C6 -1.5(6) . . . . ?
C4 C5 C6 C7 -0.3(6) . . . . ?
N2 C2 C7 C6 -179.7(3) . . . . ?
C3 C2 C7 C6 -2.3(6) . . . . ?
N2 C2 C7 C8 -0.7(6) . . . . ?
C3 C2 C7 C8 176.7(4) . . . . ?
C5 C6 C7 C2 2.2(6) . . . . ?
C5 C6 C7 C8 -176.8(4) . . . . ?
C9 N3 C8 N1 4.1(6) . . . . ?
C9 N3 C8 C7 -177.4(4) . . . . ?
C1 N1 C8 N3 176.5(4) . . . . ?
Ni1 N1 C8 N3 2.1(6) . . . . ?
C1 N1 C8 C7 -2.0(5) . . . . ?
Ni1 N1 C8 C7 -176.4(3) . . . . ?
C2 C7 C8 N3 -177.2(4) . . . . ?
C6 C7 C8 N3 1.8(6) . . . . ?
C2 C7 C8 N1 1.4(6) . . . . ?
C6 C7 C8 N1 -179.6(4) . . . . ?
C8 N3 C9 N4 0.0(6) . . . . ?
C8 N3 C9 C10 -177.3(4) . . . . ?
C16 N4 C9 N3 172.0(4) . . . . ?
Ni1 N4 C9 N3 -9.9(6) . . . . ?
C16 N4 C9 C10 -10.5(4) . . . . ?
Ni1 N4 C9 C10 167.6(3) . . . . ?
N3 C9 C10 C12 -32.5(5) . . . . ?
N4 C9 C10 C12 149.8(3) . . . . ?
N3 C9 C10 C11 87.6(4) . . . . ?
N4 C9 C10 C11 -90.2(4) . . . . ?
N3 C9 C10 C13 -156.4(4) . . . . ?
N4 C9 C10 C13 25.8(4) . . . . ?
C9 C10 C13 C16 -28.7(4) . . . . ?
C12 C10 C13 C16 -150.6(3) . . . . ?
C11 C10 C13 C16 83.6(4) . . . . ?
C9 C10 C13 C14 -151.2(3) . . . . ?
C12 C10 C13 C14 87.0(4) . . . . ?
C11 C10 C13 C14 -38.9(5) . . . . ?
C9 C10 C13 C15 84.9(4) . . . . ?
C12 C10 C13 C15 -37.0(4) . . . . ?
C11 C10 C13 C15 -162.8(3) . . . . ?
C9 N4 C16 C17 172.3(4) . . . . ?
Ni1 N4 C16 C17 -5.8(5) . . . . ?
C9 N4 C16 C13 -10.4(4) . . . . ?
Ni1 N4 C16 C13 171.6(2) . . . . ?
C14 C13 C16 C17 -34.1(5) . . . . ?
C15 C13 C16 C17 87.4(5) . . . . ?
C10 C13 C16 C17 -157.2(4) . . . . ?
C14 C13 C16 N4 148.7(3) . . . . ?
C15 C13 C16 N4 -89.9(4) . . . . ?
C10 C13 C16 N4 25.5(4) . . . . ?
N4 C16 C17 C18 -1.7(6) . . . . ?
C13 C16 C17 C18 -178.6(4) . . . . ?
C16 C17 C18 N5 1.4(6) . . . . ?
C16 C17 C18 C19 178.3(4) . . . . ?
C25 N5 C18 C17 -171.8(4) . . . . ?
Ni1 N5 C18 C17 6.3(5) . . . . ?
C25 N5 C18 C19 10.9(4) . . . . ?
Ni1 N5 C18 C19 -171.0(2) . . . . ?
C17 C18 C19 C20 32.5(5) . . . . ?
N5 C18 C19 C20 -150.3(3) . . . . ?
C17 C18 C19 C21 -89.5(4) . . . . ?
N5 C18 C19 C21 87.8(4) . . . . ?
C17 C18 C19 C22 155.3(4) . . . . ?
N5 C18 C19 C22 -27.5(4) . . . . ?
C18 C19 C22 C25 31.1(3) . . . . ?
C20 C19 C22 C25 153.7(3) . . . . ?
C21 C19 C22 C25 -82.4(3) . . . . ?
C18 C19 C22 C24 152.9(3) . . . . ?
C20 C19 C22 C24 -84.5(4) . . . . ?
C21 C19 C22 C24 39.4(4) . . . . ?
C18 C19 C22 C23 -80.5(4) . . . . ?
C20 C19 C22 C23 42.2(4) . . . . ?
C21 C19 C22 C23 166.1(3) . . . . ?
C26 N6 C25 N5 -1.0(6) . . . . ?
C26 N6 C25 C22 177.1(4) . . . . ?
C18 N5 C25 N6 -170.0(4) . . . . ?
Ni1 N5 C25 N6 11.8(6) . . . . ?
C18 N5 C25 C22 11.8(4) . . . . ?
Ni1 N5 C25 C22 -166.4(3) . . . . ?
C24 C22 C25 N6 28.8(5) . . . . ?
C23 C22 C25 N6 -90.6(4) . . . . ?
C19 C22 C25 N6 153.3(3) . . . . ?
C24 C22 C25 N5 -152.7(3) . . . . ?
C23 C22 C25 N5 87.8(4) . . . . ?
C19 C22 C25 N5 -28.3(4) . . . . ?
C25 N6 C26 N7 -6.1(6) . . . . ?
C25 N6 C26 C27 174.2(4) . . . . ?
C33 N7 C26 N6 -176.9(4) . . . . ?
Ni1 N7 C26 N6 1.7(5) . . . . ?
C33 N7 C26 C27 2.8(5) . . . . ?
Ni1 N7 C26 C27 -178.6(3) . . . . ?
N6 C26 C27 C32 179.7(3) . . . . ?
N7 C26 C27 C32 0.0(5) . . . . ?
N6 C26 C27 C28 -1.6(6) . . . . ?
N7 C26 C27 C28 178.6(4) . . . . ?
C32 C27 C28 C29 0.2(6) . . . . ?
C26 C27 C28 C29 -178.4(4) . . . . ?
C27 C28 C29 C30 0.0(6) . . . . ?
C28 C29 C30 C31 -0.2(6) . . . . ?
C29 C30 C31 C32 0.0(6) . . . . ?
C33 N8 C32 C27 2.4(5) . . . . ?
C33 N8 C32 C31 -178.6(4) . . . . ?
C28 C27 C32 N8 178.6(4) . . . . ?
C26 C27 C32 N8 -2.8(5) . . . . ?
C28 C27 C32 C31 -0.4(6) . . . . ?
C26 C27 C32 C31 178.3(4) . . . . ?
C30 C31 C32 N8 -178.7(4) . . . . ?
C30 C31 C32 C27 0.2(6) . . . . ?
C32 N8 C33 N7 0.7(6) . . . . ?
C32 N8 C33 C1 -175.4(3) . . . . ?
C26 N7 C33 N8 -3.4(6) . . . . ?
Ni1 N7 C33 N8 177.8(3) . . . . ?
C26 N7 C33 C1 172.9(3) . . . . ?
Ni1 N7 C33 C1 -5.8(4) . . . . ?
N2 C1 C33 N8 3.1(6) . . . . ?
N1 C1 C33 N8 -180.0(3) . . . . ?
N2 C1 C33 N7 -173.6(3) . . . . ?
N1 C1 C33 N7 3.3(5) . . . . ?
N12 Ni2 N9 C41 10.2(3) . . . . ?
N15 Ni2 N9 C41 -169.9(3) . . . . ?
N12 Ni2 N9 C34 -176.6(3) . . . . ?
N15 Ni2 N9 C34 3.3(3) . . . . ?
N13 Ni2 N12 C42 169.1(3) . . . . ?
N9 Ni2 N12 C42 -10.1(3) . . . . ?
N13 Ni2 N12 C49 -9.5(3) . . . . ?
N9 Ni2 N12 C49 171.3(3) . . . . ?
N12 Ni2 N13 C58 -167.5(3) . . . . ?
N15 Ni2 N13 C58 12.5(3) . . . . ?
N12 Ni2 N13 C51 9.9(3) . . . . ?
N15 Ni2 N13 C51 -170.1(3) . . . . ?
N13 Ni2 N15 C59 -6.2(3) . . . . ?
N9 Ni2 N15 C59 172.9(3) . . . . ?
N13 Ni2 N15 C66 174.4(3) . . . . ?
N9 Ni2 N15 C66 -6.4(3) . . . . ?
C35 N10 C34 N9 3.0(6) . . . . ?
C35 N10 C34 C66 -173.0(3) . . . . ?
C41 N9 C34 N10 -2.2(6) . . . . ?
Ni2 N9 C34 N10 -176.1(3) . . . . ?
C41 N9 C34 C66 174.0(3) . . . . ?
Ni2 N9 C34 C66 0.1(4) . . . . ?
C34 N10 C35 C40 -1.3(5) . . . . ?
C34 N10 C35 C36 176.3(3) . . . . ?
N10 C35 C36 C37 -177.2(3) . . . . ?
C40 C35 C36 C37 0.5(6) . . . . ?
C35 C36 C37 C38 -1.3(6) . . . . ?
C36 C37 C38 C39 0.8(6) . . . . ?
C37 C38 C39 C40 0.5(6) . . . . ?
N10 C35 C40 C39 178.4(3) . . . . ?
C36 C35 C40 C39 0.8(6) . . . . ?
N10 C35 C40 C41 -0.9(5) . . . . ?
C36 C35 C40 C41 -178.4(4) . . . . ?
C38 C39 C40 C35 -1.3(6) . . . . ?
C38 C39 C40 C41 177.9(4) . . . . ?
C42 N11 C41 N9 -1.3(6) . . . . ?
C42 N11 C41 C40 179.7(4) . . . . ?
C34 N9 C41 N11 -179.4(4) . . . . ?
Ni2 N9 C41 N11 -6.3(6) . . . . ?
C34 N9 C41 C40 -0.3(5) . . . . ?
Ni2 N9 C41 C40 172.8(3) . . . . ?
C35 C40 C41 N11 -179.2(3) . . . . ?
C39 C40 C41 N11 1.6(6) . . . . ?
C35 C40 C41 N9 1.7(5) . . . . ?
C39 C40 C41 N9 -177.6(4) . . . . ?
C41 N11 C42 N12 0.9(6) . . . . ?
C41 N11 C42 C43 177.3(4) . . . . ?
C49 N12 C42 N11 -174.3(4) . . . . ?
Ni2 N12 C42 N11 6.9(6) . . . . ?
C49 N12 C42 C43 9.1(4) . . . . ?
Ni2 N12 C42 C43 -169.7(2) . . . . ?
N11 C42 C43 C44 35.4(5) . . . . ?
N12 C42 C43 C44 -147.6(3) . . . . ?
N11 C42 C43 C45 -84.2(4) . . . . ?
N12 C42 C43 C45 92.7(4) . . . . ?
N11 C42 C43 C46 159.4(3) . . . . ?
N12 C42 C43 C46 -23.7(4) . . . . ?
C42 C43 C46 C49 26.8(4) . . . . ?
C44 C43 C46 C49 149.0(3) . . . . ?
C45 C43 C46 C49 -85.7(3) . . . . ?
C42 C43 C46 C48 149.6(3) . . . . ?
C44 C43 C46 C48 -88.2(4) . . . . ?
C45 C43 C46 C48 37.1(5) . . . . ?
C42 C43 C46 C47 -86.7(4) . . . . ?
C44 C43 C46 C47 35.5(4) . . . . ?
C45 C43 C46 C47 160.8(3) . . . . ?
C42 N12 C49 C50 -173.2(4) . . . . ?
Ni2 N12 C49 C50 5.6(5) . . . . ?
C42 N12 C49 C46 10.5(4) . . . . ?
Ni2 N12 C49 C46 -170.7(2) . . . . ?
C48 C46 C49 C50 36.7(5) . . . . ?
C47 C46 C49 C50 -84.4(4) . . . . ?
C43 C46 C49 C50 159.5(4) . . . . ?
C48 C46 C49 N12 -147.1(3) . . . . ?
C47 C46 C49 N12 91.7(4) . . . . ?
C43 C46 C49 N12 -24.3(4) . . . . ?
N12 C49 C50 C51 1.6(6) . . . . ?
C46 C49 C50 C51 177.3(4) . . . . ?
C49 C50 C51 N13 -1.2(6) . . . . ?
C49 C50 C51 C52 -179.8(4) . . . . ?
C58 N13 C51 C50 171.3(3) . . . . ?
Ni2 N13 C51 C50 -6.5(5) . . . . ?
C58 N13 C51 C52 -9.9(4) . . . . ?
Ni2 N13 C51 C52 172.4(2) . . . . ?
C50 C51 C52 C54 -31.5(5) . . . . ?
N13 C51 C52 C54 149.7(3) . . . . ?
C50 C51 C52 C53 89.3(5) . . . . ?
N13 C51 C52 C53 -89.5(4) . . . . ?
C50 C51 C52 C55 -155.0(4) . . . . ?
N13 C51 C52 C55 26.2(4) . . . . ?
C51 C52 C55 C58 -30.0(3) . . . . ?
C54 C52 C55 C58 -152.3(3) . . . . ?
C53 C52 C55 C58 85.0(4) . . . . ?
C51 C52 C55 C56 -152.3(3) . . . . ?
C54 C52 C55 C56 85.4(4) . . . . ?
C53 C52 C55 C56 -37.3(5) . . . . ?
C51 C52 C55 C57 82.2(4) . . . . ?
C54 C52 C55 C57 -40.1(5) . . . . ?
C53 C52 C55 C57 -162.7(3) . . . . ?
C59 N14 C58 N13 1.3(6) . . . . ?
C59 N14 C58 C55 -177.1(3) . . . . ?
C51 N13 C58 N14 169.4(4) . . . . ?
Ni2 N13 C58 N14 -12.7(6) . . . . ?
C51 N13 C58 C55 -12.1(4) . . . . ?
Ni2 N13 C58 C55 165.8(2) . . . . ?
C56 C55 C58 N14 -29.0(5) . . . . ?
C57 C55 C58 N14 90.1(4) . . . . ?
C52 C55 C58 N14 -153.6(3) . . . . ?
C56 C55 C58 N13 152.3(3) . . . . ?
C57 C55 C58 N13 -88.5(4) . . . . ?
C52 C55 C58 N13 27.8(4) . . . . ?
C58 N14 C59 N15 6.4(6) . . . . ?
C58 N14 C59 C60 -173.8(4) . . . . ?
C66 N15 C59 N14 177.5(4) . . . . ?
Ni2 N15 C59 N14 -1.8(5) . . . . ?
C66 N15 C59 C60 -2.3(5) . . . . ?
Ni2 N15 C59 C60 178.4(3) . . . . ?
N14 C59 C60 C65 177.4(3) . . . . ?
N15 C59 C60 C65 -2.8(5) . . . . ?
N14 C59 C60 C61 -0.2(6) . . . . ?
N15 C59 C60 C61 179.6(3) . . . . ?
C65 C60 C61 C62 -2.1(6) . . . . ?
C59 C60 C61 C62 175.5(4) . . . . ?
C60 C61 C62 C63 0.2(6) . . . . ?
C61 C62 C63 C64 1.7(6) . . . . ?
C62 C63 C64 C65 -1.7(6) . . . . ?
C66 N16 C65 C60 -3.1(5) . . . . ?
C66 N16 C65 C64 178.2(4) . . . . ?
C61 C60 C65 N16 -176.7(4) . . . . ?
C59 C60 C65 N16 5.7(6) . . . . ?
C61 C60 C65 C64 2.0(6) . . . . ?
C59 C60 C65 C64 -175.6(4) . . . . ?
C63 C64 C65 N16 178.6(4) . . . . ?
C63 C64 C65 C60 -0.1(6) . . . . ?
C65 N16 C66 N15 -2.7(6) . . . . ?
C65 N16 C66 C34 174.1(3) . . . . ?
C59 N15 C66 N16 5.5(6) . . . . ?
Ni2 N15 C66 N16 -175.1(3) . . . . ?
C59 N15 C66 C34 -171.5(3) . . . . ?
Ni2 N15 C66 C34 7.9(4) . . . . ?
N10 C34 C66 N16 -5.9(5) . . . . ?
N9 C34 C66 N16 177.6(3) . . . . ?
N10 C34 C66 N15 171.4(3) . . . . ?
N9 C34 C66 N15 -5.1(5) . . . . ?



