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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 1060103'
_audit_update_record             
;
2015-04-17 deposited with the CCDC.
2015-08-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H44 N2 Ni'
_chemical_formula_weight         491.38

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C2/c  '

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

_cell_length_a                   16.404(3)
_cell_length_b                   9.3422(18)
_cell_length_c                   19.045(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.067(2)
_cell_angle_gamma                90.00
_cell_volume                     2914.5(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.120
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1064
_exptl_absorpt_coefficient_mu    0.684
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8477
_exptl_absorpt_correction_T_max  0.8754
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8809
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2566
_reflns_number_gt                2355
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART APEX II'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0580P)²+1.0393P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2566
_refine_ls_number_parameters     155
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0319
_refine_ls_wR_factor_ref         0.0910
_refine_ls_wR_factor_gt          0.0885
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.0000 0.86720(3) 0.2500 0.03692(14) Uani 1 2 d S . .
N1 N 0.02271(8) 0.71103(14) 0.18871(6) 0.0326(3) Uani 1 1 d . . .
C1 C 0.01290(10) 0.58335(18) 0.21372(8) 0.0339(3) Uani 1 1 d . . .
C3 C 0.02573(15) 0.4472(2) 0.17482(10) 0.0556(5) Uani 1 1 d . . .
H3A H 0.0424 0.4686 0.1284 0.083 Uiso 1 1 calc R . .
H3B H -0.0243 0.3937 0.1715 0.083 Uiso 1 1 calc R . .
H3C H 0.0673 0.3916 0.1995 0.083 Uiso 1 1 calc R . .
C5 C 0.04532(10) 0.73556(17) 0.11736(8) 0.0357(4) Uani 1 1 d . . .
C6 C -0.01494(11) 0.72922(18) 0.06260(8) 0.0413(4) Uani 1 1 d . . .
C7 C 0.00778(15) 0.7700(2) -0.00462(10) 0.0583(5) Uani 1 1 d . . .
H7 H -0.0309 0.7683 -0.0421 0.070 Uiso 1 1 calc R . .
C8 C 0.08603(16) 0.8121(3) -0.01583(11) 0.0689(6) Uani 1 1 d . . .
H8 H 0.0997 0.8393 -0.0607 0.083 Uiso 1 1 calc R . .
C9 C 0.14405(14) 0.8145(3) 0.03813(11) 0.0643(6) Uani 1 1 d . . .
H9 H 0.1971 0.8415 0.0292 0.077 Uiso 1 1 calc R . .
C10 C 0.12546(12) 0.7772(2) 0.10672(9) 0.0492(5) Uani 1 1 d . . .
C11 C -0.10213(12) 0.6867(2) 0.07494(10) 0.0511(5) Uani 1 1 d . . .
H11 H -0.1003 0.6207 0.1150 0.061 Uiso 1 1 calc R . .
C12 C -0.15193(17) 0.8174(4) 0.09559(17) 0.0890(8) Uani 1 1 d . . .
H12A H -0.1560 0.8836 0.0570 0.133 Uiso 1 1 calc R . .
H12B H -0.1253 0.8631 0.1357 0.133 Uiso 1 1 calc R . .
H12C H -0.2056 0.7874 0.1070 0.133 Uiso 1 1 calc R . .
C13 C -0.14374(17) 0.6073(3) 0.01216(15) 0.0795(8) Uani 1 1 d . . .
H13A H -0.1505 0.6714 -0.0271 0.119 Uiso 1 1 calc R . .
H13B H -0.1962 0.5733 0.0247 0.119 Uiso 1 1 calc R . .
H13C H -0.1105 0.5276 -0.0004 0.119 Uiso 1 1 calc R . .
C14 C 0.18993(14) 0.7796(3) 0.16602(12) 0.0753(8) Uani 1 1 d . . .
H14 H 0.1624 0.7899 0.2102 0.090 Uiso 1 1 calc R . .
C15 C 0.2368(2) 0.6380(5) 0.1688(3) 0.1361(18) Uani 1 1 d . . .
H15A H 0.2670 0.6284 0.1273 0.204 Uiso 1 1 calc R . .
H15B H 0.1990 0.5600 0.1712 0.204 Uiso 1 1 calc R . .
H15C H 0.2738 0.6368 0.2096 0.204 Uiso 1 1 calc R . .
C16 C 0.2506(2) 0.9039(5) 0.1611(2) 0.1249(14) Uani 1 1 d . . .
H16A H 0.2212 0.9926 0.1571 0.187 Uiso 1 1 calc R . .
H16B H 0.2821 0.8910 0.1205 0.187 Uiso 1 1 calc R . .
H16C H 0.2865 0.9057 0.2026 0.187 Uiso 1 1 calc R . .
C29 C 0.0142(2) 1.0594(2) 0.21623(14) 0.0841(8) Uani 1 1 d . . .
H29A H -0.0235 1.0915 0.1786 0.101 Uiso 1 1 d R . .
H29B H 0.0699 1.0915 0.2115 0.101 Uiso 1 1 d R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 1.9174(13) 2 ?
Ni1 N1 1.9174(13) . ?
Ni1 C29 1.926(2) . ?
Ni1 C29 1.926(2) 2 ?
N1 C1 1.298(2) . ?
N1 C5 1.4458(18) . ?
C1 C1 1.467(3) 2 ?
C1 C3 1.493(2) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C5 C10 1.396(3) . ?
C5 C6 1.399(2) . ?
C6 C7 1.405(2) . ?
C6 C11 1.515(3) . ?
C7 C8 1.370(3) . ?
C7 H7 0.9300 . ?
C8 C9 1.363(3) . ?
C8 H8 0.9300 . ?
C9 C10 1.401(3) . ?
C9 H9 0.9300 . ?
C10 C14 1.506(3) . ?
C11 C12 1.532(3) . ?
C11 C13 1.536(3) . ?
C11 H11 0.9800 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.529(5) . ?
C14 C16 1.535(4) . ?
C14 H14 0.9800 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C29 C29 1.392(5) 2 ?
C29 H29A 0.9695 . ?
C29 H29B 0.9695 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N1 80.91(7) 2 . ?
N1 Ni1 C29 160.70(9) 2 . ?
N1 Ni1 C29 118.37(9) . . ?
N1 Ni1 C29 118.37(9) 2 2 ?
N1 Ni1 C29 160.70(9) . 2 ?
C29 Ni1 C29 42.37(17) . 2 ?
C1 N1 C5 122.26(13) . . ?
C1 N1 Ni1 116.36(10) . . ?
C5 N1 Ni1 121.30(10) . . ?
N1 C1 C1 113.18(8) . 2 ?
N1 C1 C3 125.28(14) . . ?
C1 C1 C3 121.54(10) 2 . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C10 C5 C6 122.45(15) . . ?
C10 C5 N1 118.14(15) . . ?
C6 C5 N1 119.16(14) . . ?
C5 C6 C7 117.16(17) . . ?
C5 C6 C11 122.05(15) . . ?
C7 C6 C11 120.74(17) . . ?
C8 C7 C6 121.1(2) . . ?
C8 C7 H7 119.5 . . ?
C6 C7 H7 119.5 . . ?
C9 C8 C7 120.63(18) . . ?
C9 C8 H8 119.7 . . ?
C7 C8 H8 119.7 . . ?
C8 C9 C10 121.4(2) . . ?
C8 C9 H9 119.3 . . ?
C10 C9 H9 119.3 . . ?
C5 C10 C9 117.28(18) . . ?
C5 C10 C14 121.63(16) . . ?
C9 C10 C14 121.08(18) . . ?
C6 C11 C12 110.58(19) . . ?
C6 C11 C13 112.95(18) . . ?
C12 C11 C13 111.3(2) . . ?
C6 C11 H11 107.2 . . ?
C12 C11 H11 107.2 . . ?
C13 C11 H11 107.2 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C10 C14 C15 110.1(3) . . ?
C10 C14 C16 113.4(3) . . ?
C15 C14 C16 109.3(3) . . ?
C10 C14 H14 108.0 . . ?
C15 C14 H14 108.0 . . ?
C16 C14 H14 108.0 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C29 C29 Ni1 68.82(8) 2 . ?
C29 C29 H29A 116.8 2 . ?
Ni1 C29 H29A 116.8 . . ?
C29 C29 H29B 116.7 2 . ?
Ni1 C29 H29B 116.8 . . ?
H29A C29 H29B 113.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Ni1 N1 C1 0.42(9) 2 . . . ?
C29 Ni1 N1 C1 179.52(15) . . . . ?
C29 Ni1 N1 C1 -177.2(3) 2 . . . ?
N1 Ni1 N1 C5 177.27(15) 2 . . . ?
C29 Ni1 N1 C5 -3.63(18) . . . . ?
C29 Ni1 N1 C5 -0.3(4) 2 . . . ?
C5 N1 C1 C1 -177.88(16) . . . 2 ?
Ni1 N1 C1 C1 -1.1(2) . . . 2 ?
C5 N1 C1 C3 2.1(3) . . . . ?
Ni1 N1 C1 C3 178.93(15) . . . . ?
C1 N1 C5 C10 -105.1(2) . . . . ?
Ni1 N1 C5 C10 78.26(18) . . . . ?
C1 N1 C5 C6 80.5(2) . . . . ?
Ni1 N1 C5 C6 -96.17(16) . . . . ?
C10 C5 C6 C7 -1.4(3) . . . . ?
N1 C5 C6 C7 172.79(16) . . . . ?
C10 C5 C6 C11 -178.79(18) . . . . ?
N1 C5 C6 C11 -4.6(2) . . . . ?
C5 C6 C7 C8 0.9(3) . . . . ?
C11 C6 C7 C8 178.3(2) . . . . ?
C6 C7 C8 C9 0.5(4) . . . . ?
C7 C8 C9 C10 -1.3(4) . . . . ?
C6 C5 C10 C9 0.6(3) . . . . ?
N1 C5 C10 C9 -173.66(18) . . . . ?
C6 C5 C10 C14 -178.4(2) . . . . ?
N1 C5 C10 C14 7.4(3) . . . . ?
C8 C9 C10 C5 0.8(4) . . . . ?
C8 C9 C10 C14 179.8(3) . . . . ?
C5 C6 C11 C12 86.6(2) . . . . ?
C7 C6 C11 C12 -90.7(2) . . . . ?
C5 C6 C11 C13 -147.8(2) . . . . ?
C7 C6 C11 C13 34.9(3) . . . . ?
C5 C10 C14 C15 93.5(3) . . . . ?
C9 C10 C14 C15 -85.4(3) . . . . ?
C5 C10 C14 C16 -143.7(3) . . . . ?
C9 C10 C14 C16 37.4(4) . . . . ?
N1 Ni1 C29 C29 -4.3(6) 2 . . 2 ?
N1 Ni1 C29 C29 178.4(2) . . . 2 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.239
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.052
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1060104'
_audit_update_record             
;
2015-04-17 deposited with the CCDC.
2015-08-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H48 N2 Ni'
_chemical_formula_weight         567.47

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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

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

_cell_length_a                   9.649(2)
_cell_length_b                   10.406(2)
_cell_length_c                   18.470(4)
_cell_angle_alpha                81.915(3)
_cell_angle_beta                 83.476(2)
_cell_angle_gamma                65.495(2)
_cell_volume                     1667.6(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.130
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             612
_exptl_absorpt_coefficient_mu    0.606
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8159
_exptl_absorpt_correction_T_max  0.8884
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10374
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0464
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.16
_diffrn_reflns_theta_max         25.02
_reflns_number_total             5702
_reflns_number_gt                4889
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART APEX II'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0100P)²+3.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5702
_refine_ls_number_parameters     362
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0489
_refine_ls_wR_factor_ref         0.1341
_refine_ls_wR_factor_gt          0.1284
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.68346(5) 0.07605(5) 0.28579(2) 0.03989(15) Uani 1 1 d . . .
N1 N 0.7691(3) 0.2141(3) 0.25579(13) 0.0318(5) Uani 1 1 d . . .
N2 N 0.8914(3) -0.0402(3) 0.30731(13) 0.0336(6) Uani 1 1 d . . .
C1 C 0.9106(3) 0.1741(3) 0.27114(16) 0.0325(7) Uani 1 1 d . . .
C2 C 0.9831(4) 0.0243(3) 0.29868(16) 0.0342(7) Uani 1 1 d . . .
C3 C 0.9967(4) 0.2664(4) 0.2599(2) 0.0506(9) Uani 1 1 d . . .
H3A H 0.9306 0.3608 0.2416 0.076 Uiso 1 1 calc R . .
H3B H 1.0818 0.2290 0.2252 0.076 Uiso 1 1 calc R . .
H3C H 1.0332 0.2690 0.3057 0.076 Uiso 1 1 calc R . .
C4 C 1.1516(4) -0.0454(4) 0.3103(2) 0.0501(9) Uani 1 1 d . . .
H4A H 1.1803 -0.1445 0.3260 0.075 Uiso 1 1 calc R . .
H4B H 1.1738 -0.0013 0.3471 0.075 Uiso 1 1 calc R . .
H4C H 1.2078 -0.0347 0.2652 0.075 Uiso 1 1 calc R . .
C5 C 0.6845(3) 0.3562(3) 0.22149(18) 0.0392(7) Uani 1 1 d . . .
C6 C 0.6057(4) 0.4674(4) 0.2638(2) 0.0504(9) Uani 1 1 d . . .
C7 C 0.5169(5) 0.5991(5) 0.2255(3) 0.0746(13) Uani 1 1 d . . .
H7 H 0.4605 0.6767 0.2515 0.090 Uiso 1 1 calc R . .
C8 C 0.5126(6) 0.6143(5) 0.1518(3) 0.0859(16) Uani 1 1 d . . .
H8 H 0.4517 0.7016 0.1282 0.103 Uiso 1 1 calc R . .
C9 C 0.5951(5) 0.5051(5) 0.1119(3) 0.0719(13) Uani 1 1 d . . .
H9 H 0.5930 0.5194 0.0611 0.086 Uiso 1 1 calc R . .
C10 C 0.6820(4) 0.3733(4) 0.1449(2) 0.0519(9) Uani 1 1 d . . .
C11 C 0.6145(5) 0.4516(5) 0.3456(2) 0.0625(11) Uani 1 1 d . . .
H11 H 0.6998 0.3612 0.3588 0.075 Uiso 1 1 calc R . .
C12 C 0.4726(10) 0.4451(11) 0.3855(4) 0.171(4) Uani 1 1 d . . .
H12A H 0.3851 0.5270 0.3690 0.256 Uiso 1 1 calc R . .
H12B H 0.4786 0.4433 0.4372 0.256 Uiso 1 1 calc R . .
H12C H 0.4635 0.3607 0.3758 0.256 Uiso 1 1 calc R . .
C13 C 0.6440(7) 0.5675(7) 0.3731(3) 0.1021(18) Uani 1 1 d . . .
H13A H 0.7274 0.5803 0.3442 0.153 Uiso 1 1 calc R . .
H13B H 0.6692 0.5412 0.4234 0.153 Uiso 1 1 calc R . .
H13C H 0.5542 0.6546 0.3693 0.153 Uiso 1 1 calc R . .
C14 C 0.7802(5) 0.2498(5) 0.0992(2) 0.0756(14) Uani 1 1 d . . .
H14 H 0.8168 0.1622 0.1326 0.091 Uiso 1 1 calc R . .
C15 C 0.9162(7) 0.2724(11) 0.0628(4) 0.172(4) Uani 1 1 d . . .
H15A H 0.9937 0.1833 0.0499 0.258 Uiso 1 1 calc R . .
H15B H 0.9552 0.3110 0.0958 0.258 Uiso 1 1 calc R . .
H15C H 0.8868 0.3373 0.0193 0.258 Uiso 1 1 calc R . .
C16 C 0.6965(7) 0.2291(9) 0.0415(4) 0.124(3) Uani 1 1 d . . .
H16A H 0.6812 0.3032 0.0019 0.185 Uiso 1 1 calc R . .
H16B H 0.5994 0.2321 0.0620 0.185 Uiso 1 1 calc R . .
H16C H 0.7554 0.1387 0.0233 0.185 Uiso 1 1 calc R . .
C17 C 0.9518(4) -0.1918(3) 0.32503(17) 0.0361(7) Uani 1 1 d . . .
C18 C 0.9750(4) -0.2759(4) 0.26715(19) 0.0426(8) Uani 1 1 d . . .
C19 C 1.0418(5) -0.4218(4) 0.2830(2) 0.0576(10) Uani 1 1 d . . .
H19 H 1.0615 -0.4795 0.2457 0.069 Uiso 1 1 calc R . .
C20 C 1.0794(5) -0.4827(4) 0.3522(3) 0.0638(11) Uani 1 1 d . . .
H20 H 1.1262 -0.5811 0.3613 0.077 Uiso 1 1 calc R . .
C21 C 1.0490(5) -0.4011(4) 0.4079(2) 0.0613(11) Uani 1 1 d . . .
H21 H 1.0723 -0.4449 0.4551 0.074 Uiso 1 1 calc R . .
C22 C 0.9837(4) -0.2530(4) 0.39635(19) 0.0475(8) Uani 1 1 d . . .
C23 C 0.9308(5) -0.2056(5) 0.1905(2) 0.0577(10) Uani 1 1 d . . .
H23 H 0.8489 -0.1115 0.1958 0.069 Uiso 1 1 calc R . .
C24 C 1.0629(7) -0.1832(7) 0.1460(3) 0.0920(17) Uani 1 1 d . . .
H24A H 1.0967 -0.1279 0.1714 0.138 Uiso 1 1 calc R . .
H24B H 1.0301 -0.1338 0.0990 0.138 Uiso 1 1 calc R . .
H24C H 1.1455 -0.2735 0.1396 0.138 Uiso 1 1 calc R . .
C25 C 0.8688(7) -0.2858(7) 0.1493(3) 0.0946(17) Uani 1 1 d . . .
H25A H 0.9513 -0.3703 0.1343 0.142 Uiso 1 1 calc R . .
H25B H 0.8203 -0.2264 0.1069 0.142 Uiso 1 1 calc R . .
H25C H 0.7959 -0.3112 0.1808 0.142 Uiso 1 1 calc R . .
C26 C 0.9452(6) -0.1630(4) 0.4596(2) 0.0696(13) Uani 1 1 d . . .
H26 H 0.9341 -0.0673 0.4392 0.083 Uiso 1 1 calc R . .
C27 C 0.7923(7) -0.1517(8) 0.4969(3) 0.122(3) Uani 1 1 d . . .
H27A H 0.7159 -0.1140 0.4615 0.184 Uiso 1 1 calc R . .
H27B H 0.7642 -0.0898 0.5350 0.184 Uiso 1 1 calc R . .
H27C H 0.8002 -0.2442 0.5178 0.184 Uiso 1 1 calc R . .
C28 C 1.0663(7) -0.2173(6) 0.5149(3) 0.0968(18) Uani 1 1 d . . .
H28A H 1.0762 -0.3094 0.5374 0.145 Uiso 1 1 calc R . .
H28B H 1.0375 -0.1529 0.5519 0.145 Uiso 1 1 calc R . .
H28C H 1.1621 -0.2238 0.4907 0.145 Uiso 1 1 calc R . .
C29 C 0.5353(5) -0.0043(6) 0.3188(3) 0.0823(16) Uani 1 1 d . . .
H29A H 0.5441 -0.0854 0.2953 0.099 Uiso 1 1 calc R . .
H29B H 0.5094 -0.0116 0.3710 0.099 Uiso 1 1 calc R . .
C30 C 0.4635(4) 0.1337(5) 0.2786(2) 0.0623(11) Uani 1 1 d . . .
H30 H 0.3991 0.2082 0.3097 0.075 Uiso 1 1 calc R . .
C31 C 0.4174(4) 0.1602(5) 0.2040(2) 0.0553(10) Uani 1 1 d . . .
C32 C 0.3469(4) 0.2993(6) 0.1727(3) 0.0745(13) Uani 1 1 d . . .
H32 H 0.3339 0.3734 0.1993 0.089 Uiso 1 1 calc R . .
C33 C 0.2962(6) 0.3297(9) 0.1036(4) 0.114(3) Uani 1 1 d . . .
H33 H 0.2504 0.4238 0.0839 0.137 Uiso 1 1 calc R . .
C34 C 0.3118(8) 0.2245(13) 0.0636(4) 0.127(3) Uani 1 1 d . . .
H34 H 0.2780 0.2457 0.0164 0.152 Uiso 1 1 calc R . .
C35 C 0.3783(9) 0.0859(10) 0.0936(4) 0.119(2) Uani 1 1 d . . .
H35 H 0.3876 0.0129 0.0671 0.142 Uiso 1 1 calc R . .
C36 C 0.4308(6) 0.0549(6) 0.1622(3) 0.0806(14) Uani 1 1 d . . .
H36 H 0.4769 -0.0396 0.1814 0.097 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N2 1.918(3) . ?
Ni1 N1 1.926(3) . ?
Ni1 C29 1.940(4) . ?
Ni1 C30 1.966(4) . ?
N1 C1 1.305(4) . ?
N1 C5 1.452(4) . ?
N2 C2 1.300(4) . ?
N2 C17 1.439(4) . ?
C1 C2 1.460(4) . ?
C1 C3 1.491(4) . ?
C2 C4 1.507(4) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 C6 1.385(5) . ?
C5 C10 1.402(5) . ?
C6 C7 1.416(5) . ?
C6 C11 1.504(6) . ?
C7 C8 1.351(7) . ?
C7 H7 0.9300 . ?
C8 C9 1.349(7) . ?
C8 H8 0.9300 . ?
C9 C10 1.372(6) . ?
C9 H9 0.9300 . ?
C10 C14 1.541(6) . ?
C11 C12 1.502(7) . ?
C11 C13 1.512(7) . ?
C11 H11 0.9800 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C16 1.497(7) . ?
C14 C15 1.497(8) . ?
C14 H14 0.9800 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C22 1.389(5) . ?
C17 C18 1.416(5) . ?
C18 C19 1.383(5) . ?
C18 C23 1.519(5) . ?
C19 C20 1.362(6) . ?
C19 H19 0.9300 . ?
C20 C21 1.355(6) . ?
C20 H20 0.9300 . ?
C21 C22 1.397(5) . ?
C21 H21 0.9300 . ?
C22 C26 1.517(5) . ?
C23 C24 1.520(6) . ?
C23 C25 1.527(6) . ?
C23 H23 0.9800 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 C28 1.514(7) . ?
C26 C27 1.521(8) . ?
C26 H26 0.9800 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 C30 1.443(6) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C31 1.450(6) . ?
C30 H30 0.9800 . ?
C31 C36 1.383(7) . ?
C31 C32 1.389(6) . ?
C32 C33 1.366(8) . ?
C32 H32 0.9300 . ?
C33 C34 1.354(11) . ?
C33 H33 0.9300 . ?
C34 C35 1.373(11) . ?
C34 H34 0.9300 . ?
C35 C36 1.364(9) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ni1 N1 81.18(11) . . ?
N2 Ni1 C29 116.64(16) . . ?
N1 Ni1 C29 160.52(18) . . ?
N2 Ni1 C30 159.89(15) . . ?
N1 Ni1 C30 118.90(15) . . ?
C29 Ni1 C30 43.35(18) . . ?
C1 N1 C5 120.4(3) . . ?
C1 N1 Ni1 115.4(2) . . ?
C5 N1 Ni1 124.2(2) . . ?
C2 N2 C17 119.6(3) . . ?
C2 N2 Ni1 115.7(2) . . ?
C17 N2 Ni1 124.4(2) . . ?
N1 C1 C2 113.3(3) . . ?
N1 C1 C3 125.3(3) . . ?
C2 C1 C3 121.4(3) . . ?
N2 C2 C1 113.8(3) . . ?
N2 C2 C4 125.3(3) . . ?
C1 C2 C4 120.8(3) . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 C10 122.3(3) . . ?
C6 C5 N1 120.5(3) . . ?
C10 C5 N1 117.1(3) . . ?
C5 C6 C7 116.0(4) . . ?
C5 C6 C11 122.6(3) . . ?
C7 C6 C11 121.3(4) . . ?
C8 C7 C6 121.3(4) . . ?
C8 C7 H7 119.4 . . ?
C6 C7 H7 119.4 . . ?
C9 C8 C7 121.2(4) . . ?
C9 C8 H8 119.4 . . ?
C7 C8 H8 119.4 . . ?
C8 C9 C10 121.1(4) . . ?
C8 C9 H9 119.4 . . ?
C10 C9 H9 119.4 . . ?
C9 C10 C5 117.9(4) . . ?
C9 C10 C14 121.2(4) . . ?
C5 C10 C14 120.8(3) . . ?
C12 C11 C6 111.8(4) . . ?
C12 C11 C13 108.6(5) . . ?
C6 C11 C13 113.7(4) . . ?
C12 C11 H11 107.5 . . ?
C6 C11 H11 107.5 . . ?
C13 C11 H11 107.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C16 C14 C15 108.2(4) . . ?
C16 C14 C10 114.0(4) . . ?
C15 C14 C10 110.2(5) . . ?
C16 C14 H14 108.1 . . ?
C15 C14 H14 108.1 . . ?
C10 C14 H14 108.1 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C22 C17 C18 121.3(3) . . ?
C22 C17 N2 121.3(3) . . ?
C18 C17 N2 117.4(3) . . ?
C19 C18 C17 117.6(3) . . ?
C19 C18 C23 122.3(3) . . ?
C17 C18 C23 120.1(3) . . ?
C20 C19 C18 121.3(4) . . ?
C20 C19 H19 119.3 . . ?
C18 C19 H19 119.3 . . ?
C21 C20 C19 120.5(4) . . ?
C21 C20 H20 119.8 . . ?
C19 C20 H20 119.8 . . ?
C20 C21 C22 121.7(4) . . ?
C20 C21 H21 119.1 . . ?
C22 C21 H21 119.1 . . ?
C17 C22 C21 117.3(3) . . ?
C17 C22 C26 121.5(3) . . ?
C21 C22 C26 121.1(3) . . ?
C18 C23 C24 111.3(4) . . ?
C18 C23 C25 113.1(4) . . ?
C24 C23 C25 110.5(4) . . ?
C18 C23 H23 107.2 . . ?
C24 C23 H23 107.2 . . ?
C25 C23 H23 107.2 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C28 C26 C22 113.8(4) . . ?
C28 C26 C27 110.4(4) . . ?
C22 C26 C27 109.2(4) . . ?
C28 C26 H26 107.8 . . ?
C22 C26 H26 107.8 . . ?
C27 C26 H26 107.8 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 Ni1 69.3(2) . . ?
C30 C29 H29A 116.7 . . ?
Ni1 C29 H29A 116.7 . . ?
C30 C29 H29B 116.7 . . ?
Ni1 C29 H29B 116.7 . . ?
H29A C29 H29B 113.7 . . ?
C29 C30 C31 125.7(5) . . ?
C29 C30 Ni1 67.4(2) . . ?
C31 C30 Ni1 113.9(3) . . ?
C29 C30 H30 113.8 . . ?
C31 C30 H30 113.8 . . ?
Ni1 C30 H30 113.8 . . ?
C36 C31 C32 116.5(5) . . ?
C36 C31 C30 124.0(4) . . ?
C32 C31 C30 119.4(4) . . ?
C33 C32 C31 121.6(6) . . ?
C33 C32 H32 119.2 . . ?
C31 C32 H32 119.2 . . ?
C34 C33 C32 120.8(7) . . ?
C34 C33 H33 119.6 . . ?
C32 C33 H33 119.6 . . ?
C33 C34 C35 119.1(7) . . ?
C33 C34 H34 120.5 . . ?
C35 C34 H34 120.5 . . ?
C36 C35 C34 120.3(7) . . ?
C36 C35 H35 119.8 . . ?
C34 C35 H35 119.8 . . ?
C35 C36 C31 121.8(6) . . ?
C35 C36 H36 119.1 . . ?
C31 C36 H36 119.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 Ni1 N1 C1 -7.7(2) . . . . ?
C29 Ni1 N1 C1 149.6(5) . . . . ?
C30 Ni1 N1 C1 171.2(2) . . . . ?
N2 Ni1 N1 C5 175.2(3) . . . . ?
C29 Ni1 N1 C5 -27.6(6) . . . . ?
C30 Ni1 N1 C5 -6.0(3) . . . . ?
N1 Ni1 N2 C2 5.3(2) . . . . ?
C29 Ni1 N2 C2 -166.4(3) . . . . ?
C30 Ni1 N2 C2 -171.8(4) . . . . ?
N1 Ni1 N2 C17 -168.7(2) . . . . ?
C29 Ni1 N2 C17 19.6(3) . . . . ?
C30 Ni1 N2 C17 14.2(6) . . . . ?
C5 N1 C1 C2 -174.3(3) . . . . ?
Ni1 N1 C1 C2 8.4(3) . . . . ?
C5 N1 C1 C3 3.4(5) . . . . ?
Ni1 N1 C1 C3 -173.9(3) . . . . ?
C17 N2 C2 C1 172.0(3) . . . . ?
Ni1 N2 C2 C1 -2.3(3) . . . . ?
C17 N2 C2 C4 -4.1(5) . . . . ?
Ni1 N2 C2 C4 -178.3(3) . . . . ?
N1 C1 C2 N2 -4.1(4) . . . . ?
C3 C1 C2 N2 178.1(3) . . . . ?
N1 C1 C2 C4 172.2(3) . . . . ?
C3 C1 C2 C4 -5.6(5) . . . . ?
C1 N1 C5 C6 -87.8(4) . . . . ?
Ni1 N1 C5 C6 89.2(4) . . . . ?
C1 N1 C5 C10 94.6(4) . . . . ?
Ni1 N1 C5 C10 -88.4(3) . . . . ?
C10 C5 C6 C7 2.4(5) . . . . ?
N1 C5 C6 C7 -175.1(3) . . . . ?
C10 C5 C6 C11 -176.7(4) . . . . ?
N1 C5 C6 C11 5.8(5) . . . . ?
C5 C6 C7 C8 -1.1(7) . . . . ?
C11 C6 C7 C8 178.0(4) . . . . ?
C6 C7 C8 C9 -1.3(8) . . . . ?
C7 C8 C9 C10 2.4(8) . . . . ?
C8 C9 C10 C5 -1.1(7) . . . . ?
C8 C9 C10 C14 -178.1(5) . . . . ?
C6 C5 C10 C9 -1.4(6) . . . . ?
N1 C5 C10 C9 176.2(3) . . . . ?
C6 C5 C10 C14 175.6(4) . . . . ?
N1 C5 C10 C14 -6.8(5) . . . . ?
C5 C6 C11 C12 -104.7(6) . . . . ?
C7 C6 C11 C12 76.2(7) . . . . ?
C5 C6 C11 C13 131.8(4) . . . . ?
C7 C6 C11 C13 -47.3(6) . . . . ?
C9 C10 C14 C16 -49.1(7) . . . . ?
C5 C10 C14 C16 134.0(5) . . . . ?
C9 C10 C14 C15 72.8(6) . . . . ?
C5 C10 C14 C15 -104.1(5) . . . . ?
C2 N2 C17 C22 80.8(4) . . . . ?
Ni1 N2 C17 C22 -105.4(3) . . . . ?
C2 N2 C17 C18 -100.3(3) . . . . ?
Ni1 N2 C17 C18 73.5(3) . . . . ?
C22 C17 C18 C19 -5.0(5) . . . . ?
N2 C17 C18 C19 176.1(3) . . . . ?
C22 C17 C18 C23 176.6(3) . . . . ?
N2 C17 C18 C23 -2.3(5) . . . . ?
C17 C18 C19 C20 2.2(6) . . . . ?
C23 C18 C19 C20 -179.4(4) . . . . ?
C18 C19 C20 C21 1.4(7) . . . . ?
C19 C20 C21 C22 -2.3(7) . . . . ?
C18 C17 C22 C21 4.2(5) . . . . ?
N2 C17 C22 C21 -177.0(3) . . . . ?
C18 C17 C22 C26 -174.1(4) . . . . ?
N2 C17 C22 C26 4.7(6) . . . . ?
C20 C21 C22 C17 -0.5(6) . . . . ?
C20 C21 C22 C26 177.8(4) . . . . ?
C19 C18 C23 C24 -87.9(5) . . . . ?
C17 C18 C23 C24 90.5(4) . . . . ?
C19 C18 C23 C25 37.3(5) . . . . ?
C17 C18 C23 C25 -144.4(4) . . . . ?
C17 C22 C26 C28 -139.9(4) . . . . ?
C21 C22 C26 C28 41.8(6) . . . . ?
C17 C22 C26 C27 96.3(5) . . . . ?
C21 C22 C26 C27 -82.0(5) . . . . ?
N2 Ni1 C29 C30 -177.3(2) . . . . ?
N1 Ni1 C29 C30 28.0(7) . . . . ?
Ni1 C29 C30 C31 103.9(4) . . . . ?
N2 Ni1 C30 C29 7.0(6) . . . . ?
N1 Ni1 C30 C29 -169.7(3) . . . . ?
N2 Ni1 C30 C31 -113.4(4) . . . . ?
N1 Ni1 C30 C31 69.9(4) . . . . ?
C29 Ni1 C30 C31 -120.4(5) . . . . ?
C29 C30 C31 C36 3.0(6) . . . . ?
Ni1 C30 C31 C36 81.4(5) . . . . ?
C29 C30 C31 C32 178.9(4) . . . . ?
Ni1 C30 C31 C32 -102.7(4) . . . . ?
C36 C31 C32 C33 -1.2(6) . . . . ?
C30 C31 C32 C33 -177.4(4) . . . . ?
C31 C32 C33 C34 0.7(8) . . . . ?
C32 C33 C34 C35 0.6(10) . . . . ?
C33 C34 C35 C36 -1.4(10) . . . . ?
C34 C35 C36 C31 0.9(9) . . . . ?
C32 C31 C36 C35 0.4(7) . . . . ?
C30 C31 C36 C35 176.4(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.969
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.969
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.071
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1060105'
_audit_update_record             
;
2015-04-17 deposited with the CCDC.
2015-08-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C37 H50 N2 Ni'
_chemical_formula_weight         581.50

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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

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

_cell_length_a                   9.7243(18)
_cell_length_b                   10.4129(19)
_cell_length_c                   18.679(3)
_cell_angle_alpha                83.031(3)
_cell_angle_beta                 87.778(3)
_cell_angle_gamma                63.827(3)
_cell_volume                     1684.7(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             628
_exptl_absorpt_coefficient_mu    0.601
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8642
_exptl_absorpt_correction_T_max  0.8892
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8313
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0516
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.34
_diffrn_reflns_theta_max         25.17
_reflns_number_total             5916
_reflns_number_gt                5102
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART APEX II'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0100P)²+6.9650P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5916
_refine_ls_number_parameters     372
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0564
_refine_ls_wR_factor_ref         0.1746
_refine_ls_wR_factor_gt          0.1508
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.22848(6) 0.07283(6) 0.28502(3) 0.03283(18) Uani 1 1 d . . .
C2 C 0.4522(5) 0.1669(4) 0.2671(2) 0.0284(8) Uani 1 1 d . . .
C1 C 0.5314(5) 0.0154(4) 0.2968(2) 0.0291(9) Uani 1 1 d . . .
C17 C 0.2216(5) 0.3490(4) 0.2127(2) 0.0328(9) Uani 1 1 d . . .
C22 C 0.1385(5) 0.4692(5) 0.2497(3) 0.0397(10) Uani 1 1 d . . .
C3 C 0.7021(5) -0.0558(5) 0.3059(3) 0.0429(11) Uani 1 1 d . . .
H3A H 0.7368 -0.1569 0.3207 0.064 Uiso 1 1 calc R . .
H3B H 0.7311 -0.0135 0.3419 0.064 Uiso 1 1 calc R . .
H3C H 0.7480 -0.0426 0.2609 0.064 Uiso 1 1 calc R . .
C4 C 0.5374(6) 0.2581(5) 0.2533(3) 0.0464(12) Uani 1 1 d . . .
H4A H 0.4696 0.3515 0.2303 0.070 Uiso 1 1 calc R . .
H4B H 0.6225 0.2128 0.2226 0.070 Uiso 1 1 calc R . .
H4C H 0.5742 0.2679 0.2983 0.070 Uiso 1 1 calc R . .
C18 C 0.2163(6) 0.3586(5) 0.1370(2) 0.0441(11) Uani 1 1 d . . .
C19 C 0.1224(7) 0.4934(6) 0.0996(3) 0.0579(15) Uani 1 1 d . . .
H19 H 0.1162 0.5028 0.0495 0.070 Uiso 1 1 calc R . .
C20 C 0.0397(7) 0.6113(6) 0.1350(3) 0.0641(16) Uani 1 1 d . . .
H20 H -0.0220 0.6994 0.1091 0.077 Uiso 1 1 calc R . .
C21 C 0.0483(6) 0.5989(5) 0.2093(3) 0.0558(14) Uani 1 1 d . . .
H21 H -0.0079 0.6797 0.2328 0.067 Uiso 1 1 calc R . .
C5 C 0.5065(5) -0.2018(4) 0.3280(2) 0.0294(9) Uani 1 1 d . . .
C10 C 0.5171(5) -0.2862(5) 0.2719(2) 0.0347(10) Uani 1 1 d . . .
C6 C 0.5515(5) -0.2650(5) 0.3995(2) 0.0372(10) Uani 1 1 d . . .
C9 C 0.5807(6) -0.4348(5) 0.2900(3) 0.0426(11) Uani 1 1 d . . .
H9 H 0.5928 -0.4928 0.2538 0.051 Uiso 1 1 calc R . .
C7 C 0.6102(6) -0.4157(5) 0.4129(3) 0.0451(12) Uani 1 1 d . . .
H7 H 0.6388 -0.4601 0.4597 0.054 Uiso 1 1 calc R . .
C8 C 0.6264(6) -0.4989(5) 0.3589(3) 0.0475(12) Uani 1 1 d . . .
H8 H 0.6682 -0.5987 0.3690 0.057 Uiso 1 1 calc R . .
C14 C 0.4626(6) -0.2149(6) 0.1954(3) 0.0474(12) Uani 1 1 d . . .
H14 H 0.3832 -0.1170 0.1994 0.057 Uiso 1 1 calc R . .
C11 C 0.5433(7) -0.1783(5) 0.4612(3) 0.0532(14) Uani 1 1 d . . .
H11 H 0.4955 -0.0759 0.4423 0.064 Uiso 1 1 calc R . .
C12 C 0.4422(9) -0.2017(8) 0.5211(3) 0.082(2) Uani 1 1 d . . .
H12A H 0.4951 -0.2967 0.5462 0.123 Uiso 1 1 calc R . .
H12B H 0.3485 -0.1913 0.5003 0.123 Uiso 1 1 calc R . .
H12C H 0.4193 -0.1317 0.5543 0.123 Uiso 1 1 calc R . .
C16 C 0.3901(8) -0.2906(8) 0.1562(4) 0.0767(19) Uani 1 1 d . . .
H16A H 0.4660 -0.3858 0.1494 0.115 Uiso 1 1 calc R . .
H16B H 0.3504 -0.2369 0.1102 0.115 Uiso 1 1 calc R . .
H16C H 0.3082 -0.2969 0.1845 0.115 Uiso 1 1 calc R . .
N1 N 0.4425(4) -0.0481(3) 0.30885(17) 0.0275(7) Uani 1 1 d . . .
N2 N 0.3095(4) 0.2085(4) 0.25108(17) 0.0277(7) Uani 1 1 d . . .
C32 C -0.0478(5) 0.1580(6) 0.2022(3) 0.0449(12) Uani 1 1 d . . .
C31 C 0.0057(5) 0.1347(6) 0.2774(3) 0.0501(13) Uani 1 1 d . . .
H31 H -0.0559 0.2138 0.3056 0.060 Uiso 1 1 calc R . .
C30 C 0.0807(6) -0.0009(7) 0.3195(3) 0.0599(16) Uani 1 1 d . . .
H30 H 0.0876 -0.0826 0.2959 0.072 Uiso 1 1 calc R . .
C37 C -0.1237(6) 0.2981(7) 0.1677(4) 0.0631(16) Uani 1 1 d . . .
H37 H -0.1338 0.3743 0.1922 0.076 Uiso 1 1 calc R . .
C33 C -0.0333(7) 0.0459(7) 0.1641(3) 0.0646(16) Uani 1 1 d . . .
H33 H 0.0177 -0.0489 0.1853 0.078 Uiso 1 1 calc R . .
C29 C 0.0609(10) -0.0167(13) 0.4000(4) 0.124(4) Uani 1 1 d . . .
H29A H 0.0366 0.0732 0.4180 0.186 Uiso 1 1 calc R . .
H29B H 0.1543 -0.0898 0.4224 0.186 Uiso 1 1 calc R . .
H29C H -0.0208 -0.0438 0.4108 0.186 Uiso 1 1 calc R . .
C26 C 0.1464(6) 0.4596(5) 0.3313(3) 0.0463(12) Uani 1 1 d . . .
H26 H 0.2257 0.3637 0.3490 0.056 Uiso 1 1 calc R . .
C23 C 0.3091(7) 0.2304(7) 0.0967(3) 0.0632(16) Uani 1 1 d . . .
H23 H 0.3515 0.1451 0.1325 0.076 Uiso 1 1 calc R . .
C27 C -0.0017(7) 0.4753(8) 0.3649(3) 0.0714(18) Uani 1 1 d . . .
H27A H -0.0768 0.5739 0.3562 0.107 Uiso 1 1 calc R . .
H27B H 0.0137 0.4469 0.4159 0.107 Uiso 1 1 calc R . .
H27C H -0.0369 0.4150 0.3440 0.107 Uiso 1 1 calc R . .
C13 C 0.7013(8) -0.2151(7) 0.4899(3) 0.0718(18) Uani 1 1 d . . .
H13A H 0.7528 -0.3163 0.5062 0.108 Uiso 1 1 calc R . .
H13B H 0.6922 -0.1610 0.5294 0.108 Uiso 1 1 calc R . .
H13C H 0.7592 -0.1914 0.4523 0.108 Uiso 1 1 calc R . .
C15 C 0.5933(8) -0.2009(8) 0.1526(3) 0.0730(19) Uani 1 1 d . . .
H15A H 0.6295 -0.1447 0.1764 0.110 Uiso 1 1 calc R . .
H15B H 0.5571 -0.1543 0.1049 0.110 Uiso 1 1 calc R . .
H15C H 0.6756 -0.2950 0.1495 0.110 Uiso 1 1 calc R . .
C28 C 0.1930(10) 0.5710(9) 0.3551(4) 0.089(2) Uani 1 1 d . . .
H28A H 0.2866 0.5612 0.3322 0.133 Uiso 1 1 calc R . .
H28B H 0.2079 0.5553 0.4066 0.133 Uiso 1 1 calc R . .
H28C H 0.1136 0.6662 0.3416 0.133 Uiso 1 1 calc R . .
C25 C 0.2176(8) 0.2019(10) 0.0424(4) 0.095(3) Uani 1 1 d . . .
H25A H 0.1289 0.1985 0.0652 0.142 Uiso 1 1 calc R . .
H25B H 0.2799 0.1115 0.0246 0.142 Uiso 1 1 calc R . .
H25C H 0.1859 0.2778 0.0030 0.142 Uiso 1 1 calc R . .
C24 C 0.4414(9) 0.2456(13) 0.0597(5) 0.133(4) Uani 1 1 d . . .
H24A H 0.4042 0.3193 0.0194 0.199 Uiso 1 1 calc R . .
H24B H 0.5098 0.1558 0.0429 0.199 Uiso 1 1 calc R . .
H24C H 0.4951 0.2715 0.0930 0.199 Uiso 1 1 calc R . .
C34 C -0.0945(10) 0.0745(11) 0.0945(4) 0.089(2) Uani 1 1 d . . .
H34 H -0.0850 -0.0009 0.0695 0.107 Uiso 1 1 calc R . .
C35 C -0.1699(10) 0.2162(14) 0.0627(4) 0.105(3) Uani 1 1 d . . .
H35 H -0.2110 0.2352 0.0163 0.126 Uiso 1 1 calc R . .
C36 C -0.1843(8) 0.3281(10) 0.0992(4) 0.090(2) Uani 1 1 d . . .
H36 H -0.2343 0.4228 0.0777 0.108 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 1.934(3) . ?
Ni1 N2 1.935(3) . ?
Ni1 C30 1.962(5) . ?
Ni1 C31 1.974(5) . ?
C2 N2 1.294(5) . ?
C2 C1 1.463(5) . ?
C2 C4 1.507(6) . ?
C1 N1 1.299(5) . ?
C1 C3 1.496(6) . ?
C17 C22 1.403(6) . ?
C17 C18 1.406(6) . ?
C17 N2 1.441(5) . ?
C22 C21 1.387(6) . ?
C22 C26 1.519(7) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C18 C19 1.405(7) . ?
C18 C23 1.514(8) . ?
C19 C20 1.370(8) . ?
C19 H19 0.9300 . ?
C20 C21 1.380(8) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C5 C6 1.410(6) . ?
C5 C10 1.420(6) . ?
C5 N1 1.441(5) . ?
C10 C9 1.391(6) . ?
C10 C14 1.526(7) . ?
C6 C7 1.406(6) . ?
C6 C11 1.528(7) . ?
C9 C8 1.370(7) . ?
C9 H9 0.9300 . ?
C7 C8 1.368(7) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C14 C16 1.525(7) . ?
C14 C15 1.527(8) . ?
C14 H14 0.9800 . ?
C11 C13 1.513(9) . ?
C11 C12 1.528(8) . ?
C11 H11 0.9800 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C32 C33 1.392(8) . ?
C32 C37 1.395(7) . ?
C32 C31 1.472(7) . ?
C31 C30 1.418(8) . ?
C31 H31 0.9800 . ?
C30 C29 1.506(9) . ?
C30 H30 0.9800 . ?
C37 C36 1.373(10) . ?
C37 H37 0.9300 . ?
C33 C34 1.394(9) . ?
C33 H33 0.9300 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C26 C27 1.497(8) . ?
C26 C28 1.534(8) . ?
C26 H26 0.9800 . ?
C23 C24 1.498(10) . ?
C23 C25 1.511(9) . ?
C23 H23 0.9800 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C34 C35 1.391(12) . ?
C34 H34 0.9300 . ?
C35 C36 1.372(12) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N2 81.16(14) . . ?
N1 Ni1 C30 117.6(2) . . ?
N2 Ni1 C30 159.8(2) . . ?
N1 Ni1 C31 159.70(19) . . ?
N2 Ni1 C31 119.10(19) . . ?
C30 Ni1 C31 42.2(2) . . ?
N2 C2 C1 113.6(4) . . ?
N2 C2 C4 125.3(4) . . ?
C1 C2 C4 120.9(4) . . ?
N1 C1 C2 114.2(4) . . ?
N1 C1 C3 125.7(4) . . ?
C2 C1 C3 120.0(4) . . ?
C22 C17 C18 121.7(4) . . ?
C22 C17 N2 121.2(4) . . ?
C18 C17 N2 117.0(4) . . ?
C21 C22 C17 117.9(5) . . ?
C21 C22 C26 120.3(5) . . ?
C17 C22 C26 121.8(4) . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C19 C18 C17 117.3(5) . . ?
C19 C18 C23 120.7(5) . . ?
C17 C18 C23 122.0(4) . . ?
C20 C19 C18 121.6(5) . . ?
C20 C19 H19 119.2 . . ?
C18 C19 H19 119.2 . . ?
C19 C20 C21 119.8(5) . . ?
C19 C20 H20 120.1 . . ?
C21 C20 H20 120.1 . . ?
C20 C21 C22 121.7(5) . . ?
C20 C21 H21 119.2 . . ?
C22 C21 H21 119.2 . . ?
C6 C5 C10 121.6(4) . . ?
C6 C5 N1 121.5(4) . . ?
C10 C5 N1 116.8(4) . . ?
C9 C10 C5 117.0(4) . . ?
C9 C10 C14 122.4(4) . . ?
C5 C10 C14 120.6(4) . . ?
C7 C6 C5 117.2(4) . . ?
C7 C6 C11 119.6(4) . . ?
C5 C6 C11 123.2(4) . . ?
C8 C9 C10 122.6(4) . . ?
C8 C9 H9 118.7 . . ?
C10 C9 H9 118.7 . . ?
C8 C7 C6 121.9(5) . . ?
C8 C7 H7 119.0 . . ?
C6 C7 H7 119.0 . . ?
C7 C8 C9 119.7(4) . . ?
C7 C8 H8 120.2 . . ?
C9 C8 H8 120.2 . . ?
C16 C14 C10 113.0(5) . . ?
C16 C14 C15 111.8(5) . . ?
C10 C14 C15 110.3(4) . . ?
C16 C14 H14 107.1 . . ?
C10 C14 H14 107.1 . . ?
C15 C14 H14 107.1 . . ?
C13 C11 C6 111.5(5) . . ?
C13 C11 C12 111.3(5) . . ?
C6 C11 C12 110.2(5) . . ?
C13 C11 H11 107.9 . . ?
C6 C11 H11 107.9 . . ?
C12 C11 H11 107.9 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C1 N1 C5 120.5(3) . . ?
C1 N1 Ni1 115.0(3) . . ?
C5 N1 Ni1 123.8(3) . . ?
C2 N2 C17 120.1(3) . . ?
C2 N2 Ni1 115.2(3) . . ?
C17 N2 Ni1 124.7(3) . . ?
C33 C32 C37 117.5(6) . . ?
C33 C32 C31 122.8(5) . . ?
C37 C32 C31 119.6(5) . . ?
C30 C31 C32 125.7(5) . . ?
C30 C31 Ni1 68.4(3) . . ?
C32 C31 Ni1 112.5(3) . . ?
C30 C31 H31 113.9 . . ?
C32 C31 H31 113.9 . . ?
Ni1 C31 H31 113.9 . . ?
C31 C30 C29 121.2(7) . . ?
C31 C30 Ni1 69.4(3) . . ?
C29 C30 Ni1 116.1(4) . . ?
C31 C30 H30 114.3 . . ?
C29 C30 H30 114.3 . . ?
Ni1 C30 H30 114.3 . . ?
C36 C37 C32 122.7(7) . . ?
C36 C37 H37 118.6 . . ?
C32 C37 H37 118.6 . . ?
C32 C33 C34 120.5(7) . . ?
C32 C33 H33 119.7 . . ?
C34 C33 H33 119.7 . . ?
C30 C29 H29A 109.5 . . ?
C30 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C30 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C26 C22 111.6(5) . . ?
C27 C26 C28 110.5(5) . . ?
C22 C26 C28 111.5(5) . . ?
C27 C26 H26 107.7 . . ?
C22 C26 H26 107.7 . . ?
C28 C26 H26 107.7 . . ?
C24 C23 C25 109.1(5) . . ?
C24 C23 C18 111.0(6) . . ?
C25 C23 C18 114.4(5) . . ?
C24 C23 H23 107.3 . . ?
C25 C23 H23 107.3 . . ?
C18 C23 H23 107.3 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C35 C34 C33 119.7(8) . . ?
C35 C34 H34 120.2 . . ?
C33 C34 H34 120.2 . . ?
C36 C35 C34 120.6(7) . . ?
C36 C35 H35 119.7 . . ?
C34 C35 H35 119.7 . . ?
C35 C36 C37 118.9(8) . . ?
C35 C36 H36 120.5 . . ?
C37 C36 H36 120.5 . . ?

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
N2 C2 C1 N1 -6.5(5) . . . . ?
C4 C2 C1 N1 177.1(4) . . . . ?
N2 C2 C1 C3 169.3(4) . . . . ?
C4 C2 C1 C3 -7.2(6) . . . . ?
C18 C17 C22 C21 0.9(7) . . . . ?
N2 C17 C22 C21 -175.7(4) . . . . ?
C18 C17 C22 C26 -178.9(4) . . . . ?
N2 C17 C22 C26 4.6(7) . . . . ?
C22 C17 C18 C19 -0.9(7) . . . . ?
N2 C17 C18 C19 175.8(4) . . . . ?
C22 C17 C18 C23 178.2(5) . . . . ?
N2 C17 C18 C23 -5.1(7) . . . . ?
C17 C18 C19 C20 0.3(8) . . . . ?
C23 C18 C19 C20 -178.8(6) . . . . ?
C18 C19 C20 C21 0.3(9) . . . . ?
C19 C20 C21 C22 -0.3(9) . . . . ?
C17 C22 C21 C20 -0.2(8) . . . . ?
C26 C22 C21 C20 179.5(5) . . . . ?
C6 C5 C10 C9 -3.0(6) . . . . ?
N1 C5 C10 C9 179.1(4) . . . . ?
C6 C5 C10 C14 178.0(4) . . . . ?
N1 C5 C10 C14 0.0(6) . . . . ?
C10 C5 C6 C7 1.1(7) . . . . ?
N1 C5 C6 C7 179.0(4) . . . . ?
C10 C5 C6 C11 179.4(4) . . . . ?
N1 C5 C6 C11 -2.8(7) . . . . ?
C5 C10 C9 C8 2.5(7) . . . . ?
C14 C10 C9 C8 -178.4(5) . . . . ?
C5 C6 C7 C8 1.3(7) . . . . ?
C11 C6 C7 C8 -177.0(5) . . . . ?
C6 C7 C8 C9 -1.8(8) . . . . ?
C10 C9 C8 C7 -0.2(8) . . . . ?
C9 C10 C14 C16 36.4(7) . . . . ?
C5 C10 C14 C16 -144.5(5) . . . . ?
C9 C10 C14 C15 -89.6(6) . . . . ?
C5 C10 C14 C15 89.5(6) . . . . ?
C7 C6 C11 C13 64.2(6) . . . . ?
C5 C6 C11 C13 -114.1(5) . . . . ?
C7 C6 C11 C12 -59.9(7) . . . . ?
C5 C6 C11 C12 121.9(5) . . . . ?
C2 C1 N1 C5 170.8(3) . . . . ?
C3 C1 N1 C5 -4.6(6) . . . . ?
C2 C1 N1 Ni1 -0.3(4) . . . . ?
C3 C1 N1 Ni1 -175.7(3) . . . . ?
C6 C5 N1 C1 82.6(5) . . . . ?
C10 C5 N1 C1 -99.5(5) . . . . ?
C6 C5 N1 Ni1 -107.1(4) . . . . ?
C10 C5 N1 Ni1 70.8(4) . . . . ?
N2 Ni1 N1 C1 4.3(3) . . . . ?
C30 Ni1 N1 C1 -167.7(3) . . . . ?
C31 Ni1 N1 C1 -172.7(5) . . . . ?
N2 Ni1 N1 C5 -166.5(3) . . . . ?
C30 Ni1 N1 C5 21.6(4) . . . . ?
C31 Ni1 N1 C5 16.5(7) . . . . ?
C1 C2 N2 C17 -171.9(3) . . . . ?
C4 C2 N2 C17 4.4(6) . . . . ?
C1 C2 N2 Ni1 10.1(4) . . . . ?
C4 C2 N2 Ni1 -173.7(4) . . . . ?
C22 C17 N2 C2 -91.2(5) . . . . ?
C18 C17 N2 C2 92.1(5) . . . . ?
C22 C17 N2 Ni1 86.6(5) . . . . ?
C18 C17 N2 Ni1 -90.1(4) . . . . ?
N1 Ni1 N2 C2 -8.1(3) . . . . ?
C30 Ni1 N2 C2 150.9(6) . . . . ?
C31 Ni1 N2 C2 170.7(3) . . . . ?
N1 Ni1 N2 C17 173.9(3) . . . . ?
C30 Ni1 N2 C17 -27.0(7) . . . . ?
C31 Ni1 N2 C17 -7.2(4) . . . . ?
C33 C32 C31 C30 1.8(8) . . . . ?
C37 C32 C31 C30 178.3(5) . . . . ?
C33 C32 C31 Ni1 80.7(5) . . . . ?
C37 C32 C31 Ni1 -102.8(5) . . . . ?
N1 Ni1 C31 C30 6.7(8) . . . . ?
N2 Ni1 C31 C30 -170.0(3) . . . . ?
N1 Ni1 C31 C32 -114.4(5) . . . . ?
N2 Ni1 C31 C32 69.0(4) . . . . ?
C30 Ni1 C31 C32 -121.1(6) . . . . ?
C32 C31 C30 C29 -148.4(5) . . . . ?
Ni1 C31 C30 C29 108.8(5) . . . . ?
C32 C31 C30 Ni1 102.8(5) . . . . ?
N1 Ni1 C30 C31 -177.4(3) . . . . ?
N2 Ni1 C30 C31 26.1(8) . . . . ?
N1 Ni1 C30 C29 67.0(7) . . . . ?
N2 Ni1 C30 C29 -89.4(8) . . . . ?
C31 Ni1 C30 C29 -115.6(8) . . . . ?
C33 C32 C37 C36 0.5(8) . . . . ?
C31 C32 C37 C36 -176.2(5) . . . . ?
C37 C32 C33 C34 -0.7(8) . . . . ?
C31 C32 C33 C34 175.9(5) . . . . ?
C21 C22 C26 C27 69.5(6) . . . . ?
C17 C22 C26 C27 -110.8(5) . . . . ?
C21 C22 C26 C28 -54.7(7) . . . . ?
C17 C22 C26 C28 125.0(6) . . . . ?
C19 C18 C23 C24 72.5(8) . . . . ?
C17 C18 C23 C24 -106.6(7) . . . . ?
C19 C18 C23 C25 -51.5(8) . . . . ?
C17 C18 C23 C25 129.4(6) . . . . ?
C32 C33 C34 C35 0.4(10) . . . . ?
C33 C34 C35 C36 0.1(12) . . . . ?
C34 C35 C36 C37 -0.3(12) . . . . ?
C32 C37 C36 C35 0.0(10) . . . . ?

_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_theta_full        25.17
_diffrn_measured_fraction_theta_full 0.976
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.110
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1060106'
_audit_update_record             
;
2015-04-17 deposited with the CCDC.
2015-08-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H52 N2 Ni'
_chemical_formula_weight         643.57

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'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Fdd2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   19.024(11)
_cell_length_b                   41.19(2)
_cell_length_c                   9.557(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7489(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            dark-blue
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2768
_exptl_absorpt_coefficient_mu    0.547
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8984
_exptl_absorpt_correction_T_max  0.9127
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12565
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.98
_diffrn_reflns_theta_max         26.72
_reflns_number_total             3323
_reflns_number_gt                2920
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART APEX II'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0528P)²+2.2788P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.028(16)
_refine_ls_number_reflns         3323
_refine_ls_number_parameters     209
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0345
_refine_ls_wR_factor_ref         0.0905
_refine_ls_wR_factor_gt          0.0844
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.0000 0.0000 0.76515(5) 0.03506(12) Uani 1 2 d S . .
C15 C 0.03285(14) 0.00884(7) 0.5740(3) 0.0448(6) Uani 1 1 d . . .
H15 H 0.0733 -0.0045 0.5463 0.054 Uiso 1 1 calc R . .
C3 C 0.12808(11) 0.02731(6) 0.9002(3) 0.0365(5) Uani 1 1 d . . .
C8 C 0.18212(11) 0.00666(6) 0.8534(3) 0.0397(6) Uani 1 1 d . . .
C7 C 0.24738(12) 0.02095(8) 0.8285(4) 0.0546(8) Uani 1 1 d . . .
H7 H 0.2846 0.0080 0.7994 0.066 Uiso 1 1 calc R . .
C4 C 0.13772(13) 0.06068(6) 0.9193(3) 0.0429(6) Uani 1 1 d . . .
C6 C 0.25818(14) 0.05369(9) 0.8459(4) 0.0605(8) Uani 1 1 d . . .
H6 H 0.3022 0.0625 0.8276 0.073 Uiso 1 1 calc R . .
C16 C 0.04010(14) 0.04303(7) 0.5354(3) 0.0502(6) Uani 1 1 d . . .
C5 C 0.20456(15) 0.07337(7) 0.8901(4) 0.0549(7) Uani 1 1 d . . .
H5 H 0.2126 0.0955 0.9010 0.066 Uiso 1 1 calc R . .
C21 C 0.10755(19) 0.05705(8) 0.5288(4) 0.0697(9) Uani 1 1 d . . .
H21 H 0.1463 0.0445 0.5530 0.084 Uiso 1 1 calc R . .
C9 C 0.07827(15) 0.08306(7) 0.9672(3) 0.0542(7) Uani 1 1 d . . .
H9 H 0.0423 0.0694 1.0112 0.065 Uiso 1 1 calc R . .
C18 C -0.0053(3) 0.09518(11) 0.4582(5) 0.0992(16) Uani 1 1 d . . .
H18 H -0.0436 0.1082 0.4361 0.119 Uiso 1 1 calc R . .
C19 C 0.0621(4) 0.10808(11) 0.4511(5) 0.1074(18) Uani 1 1 d . . .
H19 H 0.0693 0.1294 0.4222 0.129 Uiso 1 1 calc R . .
C20 C 0.1179(3) 0.08851(11) 0.4879(6) 0.0988(15) Uani 1 1 d . . .
H20 H 0.1633 0.0968 0.4849 0.119 Uiso 1 1 calc R . .
C12 C 0.16917(13) -0.02950(6) 0.8322(3) 0.0467(6) Uani 1 1 d . . .
H12 H 0.1211 -0.0319 0.7968 0.056 Uiso 1 1 calc R . .
C14 C 0.2179(2) -0.04478(9) 0.7245(5) 0.0811(12) Uani 1 1 d . . .
H14A H 0.2174 -0.0320 0.6405 0.122 Uiso 1 1 calc R . .
H14B H 0.2022 -0.0664 0.7039 0.122 Uiso 1 1 calc R . .
H14C H 0.2648 -0.0456 0.7612 0.122 Uiso 1 1 calc R . .
C13 C 0.1732(2) -0.04818(9) 0.9706(4) 0.0689(9) Uani 1 1 d . . .
H13A H 0.2193 -0.0458 1.0100 0.103 Uiso 1 1 calc R . .
H13B H 0.1638 -0.0708 0.9538 0.103 Uiso 1 1 calc R . .
H13C H 0.1389 -0.0397 1.0346 0.103 Uiso 1 1 calc R . .
C11 C 0.0445(3) 0.09997(17) 0.8457(6) 0.145(3) Uani 1 1 d . . .
H11A H 0.0145 0.1170 0.8795 0.218 Uiso 1 1 calc R . .
H11B H 0.0172 0.0847 0.7930 0.218 Uiso 1 1 calc R . .
H11C H 0.0803 0.1091 0.7867 0.218 Uiso 1 1 calc R . .
C10 C 0.1010(3) 0.10786(12) 1.0740(6) 0.1077(17) Uani 1 1 d . . .
H10A H 0.1223 0.1260 1.0272 0.161 Uiso 1 1 calc R . .
H10B H 0.1345 0.0982 1.1368 0.161 Uiso 1 1 calc R . .
H10C H 0.0608 0.1151 1.1260 0.161 Uiso 1 1 calc R . .
N1 N 0.05959(9) 0.01311(5) 0.9194(2) 0.0328(4) Uani 1 1 d . . .
C1 C 0.03552(10) 0.00752(6) 1.0440(3) 0.0363(5) Uani 1 1 d . . .
C2 C 0.07223(13) 0.01391(9) 1.1798(3) 0.0545(7) Uani 1 1 d . . .
H2A H 0.1187 0.0220 1.1616 0.082 Uiso 1 1 calc R . .
H2B H 0.0754 -0.0059 1.2324 0.082 Uiso 1 1 calc R . .
H2C H 0.0462 0.0297 1.2325 0.082 Uiso 1 1 calc R . .
C17 C -0.0164(2) 0.06310(8) 0.4980(4) 0.0687(9) Uani 1 1 d . . .
H17 H -0.0619 0.0549 0.4997 0.082 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 1.937(2) . ?
Ni1 N1 1.937(2) 2 ?
Ni1 C15 1.965(3) . ?
Ni1 C15 1.965(3) 2 ?
C15 C15 1.447(5) 2 ?
C15 C16 1.462(4) . ?
C15 H15 0.9800 . ?
C3 C4 1.399(4) . ?
C3 C8 1.407(3) . ?
C3 N1 1.440(3) . ?
C8 C7 1.394(4) . ?
C8 C12 1.523(4) . ?
C7 C6 1.374(5) . ?
C7 H7 0.9300 . ?
C4 C5 1.403(4) . ?
C4 C9 1.529(4) . ?
C6 C5 1.370(5) . ?
C6 H6 0.9300 . ?
C16 C17 1.403(5) . ?
C16 C21 1.409(4) . ?
C5 H5 0.9300 . ?
C21 C20 1.368(6) . ?
C21 H21 0.9300 . ?
C9 C11 1.499(6) . ?
C9 C10 1.507(5) . ?
C9 H9 0.9800 . ?
C18 C17 1.391(6) . ?
C18 C19 1.389(7) . ?
C18 H18 0.9300 . ?
C19 C20 1.379(8) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C12 C14 1.521(4) . ?
C12 C13 1.532(5) . ?
C12 H12 0.9800 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
N1 C1 1.297(3) . ?
C1 C1 1.487(4) 2 ?
C1 C2 1.497(4) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C17 H17 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N1 80.85(12) . 2 ?
N1 Ni1 C15 118.04(11) . . ?
N1 Ni1 C15 161.02(9) 2 . ?
N1 Ni1 C15 161.03(9) . 2 ?
N1 Ni1 C15 118.03(11) 2 2 ?
C15 Ni1 C15 43.19(16) . 2 ?
C15 C15 C16 124.5(3) 2 . ?
C15 C15 Ni1 68.41(8) 2 . ?
C16 C15 Ni1 116.29(19) . . ?
C15 C15 H15 113.3 2 . ?
C16 C15 H15 113.3 . . ?
Ni1 C15 H15 113.3 . . ?
C4 C3 C8 122.6(2) . . ?
C4 C3 N1 120.1(2) . . ?
C8 C3 N1 117.1(2) . . ?
C7 C8 C3 116.7(2) . . ?
C7 C8 C12 122.3(2) . . ?
C3 C8 C12 121.0(2) . . ?
C6 C7 C8 121.8(3) . . ?
C6 C7 H7 119.1 . . ?
C8 C7 H7 119.1 . . ?
C5 C4 C3 117.3(2) . . ?
C5 C4 C9 120.3(3) . . ?
C3 C4 C9 122.3(2) . . ?
C5 C6 C7 120.5(2) . . ?
C5 C6 H6 119.8 . . ?
C7 C6 H6 119.8 . . ?
C17 C16 C21 116.4(3) . . ?
C17 C16 C15 124.0(3) . . ?
C21 C16 C15 119.5(3) . . ?
C6 C5 C4 121.0(3) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C20 C21 C16 122.2(4) . . ?
C20 C21 H21 118.9 . . ?
C16 C21 H21 118.9 . . ?
C11 C9 C10 109.4(4) . . ?
C11 C9 C4 111.4(3) . . ?
C10 C9 C4 113.5(3) . . ?
C11 C9 H9 107.4 . . ?
C10 C9 H9 107.4 . . ?
C4 C9 H9 107.4 . . ?
C17 C18 C19 121.1(4) . . ?
C17 C18 H18 119.4 . . ?
C19 C18 H18 119.4 . . ?
C20 C19 C18 118.3(4) . . ?
C20 C19 H19 120.8 . . ?
C18 C19 H19 120.8 . . ?
C21 C20 C19 121.0(5) . . ?
C21 C20 H20 119.5 . . ?
C19 C20 H20 119.5 . . ?
C14 C12 C8 113.3(2) . . ?
C14 C12 C13 110.2(3) . . ?
C8 C12 C13 111.6(3) . . ?
C14 C12 H12 107.1 . . ?
C8 C12 H12 107.1 . . ?
C13 C12 H12 107.1 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C1 N1 C3 120.6(2) . . ?
C1 N1 Ni1 116.29(15) . . ?
C3 N1 Ni1 123.09(16) . . ?
N1 C1 C1 113.28(13) . 2 ?
N1 C1 C2 126.9(2) . . ?
C1 C1 C2 119.83(14) 2 . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C18 C17 C16 120.8(4) . . ?
C18 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        26.72
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.057
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
####################################################################### 
# 
# 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_6
_database_code_depnum_ccdc_archive 'CCDC 1060107'
_audit_update_record             
;
2015-04-17 deposited with the CCDC.
2015-08-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H54 N2 Ni'
_chemical_formula_weight         669.60

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/c  '

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

_cell_length_a                   19.995(4)
_cell_length_b                   9.4506(17)
_cell_length_c                   20.667(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.609(3)
_cell_angle_gamma                90.00
_cell_volume                     3901.3(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1440
_exptl_absorpt_coefficient_mu    0.528
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8793
_exptl_absorpt_correction_T_max  0.9018
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18490
_diffrn_reflns_av_R_equivalents  0.0658
_diffrn_reflns_av_sigmaI/netI    0.0778
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.97
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6839
_reflns_number_gt                4434
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART APEX II'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0677P)²+6.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6839
_refine_ls_number_parameters     434
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1017
_refine_ls_R_factor_gt           0.0570
_refine_ls_wR_factor_ref         0.1842
_refine_ls_wR_factor_gt          0.1451
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.27007(3) 0.32595(6) 0.77642(3) 0.03190(19) Uani 1 1 d . . .
N1 N 0.32269(16) 0.1573(4) 0.79509(16) 0.0287(8) Uani 1 1 d . . .
N2 N 0.20145(16) 0.1833(4) 0.76015(16) 0.0334(8) Uani 1 1 d . . .
C1 C 0.2913(2) 0.0388(5) 0.7884(2) 0.0329(10) Uani 1 1 d . . .
C2 C 0.2196(2) 0.0554(5) 0.7699(2) 0.0352(10) Uani 1 1 d . . .
C3 C 0.3226(3) -0.1052(5) 0.7957(3) 0.0534(14) Uani 1 1 d . . .
H3A H 0.3697 -0.0954 0.8057 0.080 Uiso 1 1 calc R . .
H3B H 0.3158 -0.1569 0.7559 0.080 Uiso 1 1 calc R . .
H3C H 0.3023 -0.1554 0.8300 0.080 Uiso 1 1 calc R . .
C4 C 0.1746(3) -0.0715(5) 0.7660(3) 0.0534(14) Uani 1 1 d . . .
H4A H 0.1295 -0.0417 0.7556 0.080 Uiso 1 1 calc R . .
H4B H 0.1764 -0.1196 0.8070 0.080 Uiso 1 1 calc R . .
H4C H 0.1891 -0.1343 0.7330 0.080 Uiso 1 1 calc R . .
C5 C 0.3931(2) 0.1662(4) 0.8132(2) 0.0315(9) Uani 1 1 d . . .
C6 C 0.4361(2) 0.2100(4) 0.7661(2) 0.0350(10) Uani 1 1 d . . .
C7 C 0.5033(2) 0.2318(5) 0.7852(3) 0.0513(13) Uani 1 1 d . . .
H7 H 0.5335 0.2593 0.7547 0.062 Uiso 1 1 calc R . .
C8 C 0.5252(3) 0.2133(6) 0.8485(3) 0.0570(15) Uani 1 1 d . . .
H8 H 0.5699 0.2298 0.8606 0.068 Uiso 1 1 calc R . .
C9 C 0.4819(2) 0.1706(6) 0.8940(2) 0.0502(13) Uani 1 1 d . . .
H9 H 0.4976 0.1596 0.9368 0.060 Uiso 1 1 calc R . .
C10 C 0.4147(2) 0.1433(5) 0.8777(2) 0.0382(11) Uani 1 1 d . . .
C11 C 0.4105(3) 0.2332(5) 0.6962(2) 0.0457(12) Uani 1 1 d . . .
H11 H 0.3664 0.2775 0.6981 0.055 Uiso 1 1 calc R . .
C12 C 0.4533(4) 0.3336(7) 0.6588(3) 0.0791(19) Uani 1 1 d . . .
H12A H 0.4617 0.4178 0.6839 0.119 Uiso 1 1 calc R . .
H12B H 0.4304 0.3581 0.6185 0.119 Uiso 1 1 calc R . .
H12C H 0.4951 0.2888 0.6503 0.119 Uiso 1 1 calc R . .
C13 C 0.4000(3) 0.0941(6) 0.6595(3) 0.0665(16) Uani 1 1 d . . .
H13A H 0.3813 0.1132 0.6168 0.100 Uiso 1 1 calc R . .
H13B H 0.3699 0.0349 0.6823 0.100 Uiso 1 1 calc R . .
H13C H 0.4422 0.0467 0.6564 0.100 Uiso 1 1 calc R . .
C14 C 0.3677(3) 0.0979(6) 0.9288(2) 0.0482(13) Uani 1 1 d . . .
H14 H 0.3270 0.0613 0.9065 0.058 Uiso 1 1 calc R . .
C15 C 0.3963(4) -0.0190(8) 0.9717(3) 0.093(2) Uani 1 1 d . . .
H15A H 0.4172 -0.0887 0.9456 0.140 Uiso 1 1 calc R . .
H15B H 0.3609 -0.0624 0.9946 0.140 Uiso 1 1 calc R . .
H15C H 0.4289 0.0199 1.0023 0.140 Uiso 1 1 calc R . .
C16 C 0.3478(5) 0.2181(8) 0.9700(4) 0.133(4) Uani 1 1 d . . .
H16A H 0.3872 0.2655 0.9873 0.199 Uiso 1 1 calc R . .
H16B H 0.3224 0.1832 1.0050 0.199 Uiso 1 1 calc R . .
H16C H 0.3210 0.2834 0.9444 0.199 Uiso 1 1 calc R . .
C17 C 0.1340(2) 0.2222(5) 0.7386(2) 0.0351(11) Uani 1 1 d . . .
C18 C 0.0948(2) 0.2927(6) 0.7826(2) 0.0446(12) Uani 1 1 d . . .
C19 C 0.0321(3) 0.3388(8) 0.7597(3) 0.076(2) Uani 1 1 d . . .
H19 H 0.0045 0.3863 0.7876 0.091 Uiso 1 1 calc R . .
C20 C 0.0101(3) 0.3152(9) 0.6965(3) 0.092(3) Uani 1 1 d . . .
H20 H -0.0316 0.3488 0.6820 0.110 Uiso 1 1 calc R . .
C21 C 0.0483(3) 0.2442(7) 0.6557(3) 0.0648(16) Uani 1 1 d . . .
H21 H 0.0318 0.2277 0.6136 0.078 Uiso 1 1 calc R . .
C22 C 0.1121(2) 0.1942(6) 0.6743(2) 0.0468(13) Uani 1 1 d . . .
C23 C 0.1207(2) 0.3210(6) 0.8518(2) 0.0511(13) Uani 1 1 d . . .
H23 H 0.1690 0.3374 0.8498 0.061 Uiso 1 1 calc R . .
C24 C 0.1126(4) 0.1884(7) 0.8935(3) 0.081(2) Uani 1 1 d . . .
H24A H 0.1378 0.1997 0.9338 0.122 Uiso 1 1 calc R . .
H24B H 0.1289 0.1074 0.8710 0.122 Uiso 1 1 calc R . .
H24C H 0.0662 0.1752 0.9016 0.122 Uiso 1 1 calc R . .
C25 C 0.0918(3) 0.4526(8) 0.8823(3) 0.087(2) Uani 1 1 d . . .
H25A H 0.0453 0.4377 0.8894 0.131 Uiso 1 1 calc R . .
H25B H 0.0967 0.5318 0.8538 0.131 Uiso 1 1 calc R . .
H25C H 0.1154 0.4713 0.9229 0.131 Uiso 1 1 calc R . .
C26 C 0.1555(3) 0.1212(5) 0.6263(2) 0.0468(13) Uani 1 1 d . . .
H26 H 0.1900 0.0680 0.6512 0.056 Uiso 1 1 calc R . .
C27 C 0.1904(4) 0.2279(9) 0.5864(4) 0.112(3) Uani 1 1 d . . .
H27A H 0.1579 0.2876 0.5645 0.169 Uiso 1 1 calc R . .
H27B H 0.2163 0.1801 0.5551 0.169 Uiso 1 1 calc R . .
H27C H 0.2195 0.2846 0.6141 0.169 Uiso 1 1 calc R . .
C28 C 0.1174(4) 0.0171(8) 0.5828(3) 0.097(2) Uani 1 1 d . . .
H28A H 0.0830 0.0662 0.5579 0.146 Uiso 1 1 calc R . .
H28B H 0.0974 -0.0541 0.6088 0.146 Uiso 1 1 calc R . .
H28C H 0.1476 -0.0268 0.5541 0.146 Uiso 1 1 calc R . .
C29 C 0.3835(4) 0.5938(6) 0.9847(3) 0.0688(18) Uani 1 1 d . . .
H29 H 0.3996 0.6126 1.0267 0.083 Uiso 1 1 calc R . .
C30 C 0.4265(3) 0.5638(7) 0.9372(3) 0.0662(16) Uani 1 1 d . . .
H30 H 0.4722 0.5606 0.9473 0.079 Uiso 1 1 calc R . .
C31 C 0.4033(3) 0.5384(6) 0.8748(3) 0.0536(14) Uani 1 1 d . . .
H31 H 0.4338 0.5199 0.8433 0.064 Uiso 1 1 calc R . .
C32 C 0.3350(2) 0.5395(4) 0.8574(2) 0.0391(11) Uani 1 1 d . . .
C33 C 0.2913(3) 0.5704(5) 0.9063(3) 0.0537(14) Uani 1 1 d . . .
H33 H 0.2454 0.5741 0.8965 0.064 Uiso 1 1 calc R . .
C34 C 0.3153(3) 0.5958(6) 0.9692(3) 0.0604(15) Uani 1 1 d . . .
H34 H 0.2854 0.6144 1.0013 0.073 Uiso 1 1 calc R . .
C35 C 0.3133(2) 0.5114(4) 0.7889(2) 0.0377(11) Uani 1 1 d . . .
H35 H 0.3475 0.5324 0.7578 0.045 Uiso 1 1 calc R . .
C36 C 0.2459(2) 0.5272(5) 0.7634(2) 0.0406(12) Uani 1 1 d . . .
H36 H 0.2138 0.5661 0.7932 0.049 Uiso 1 1 calc R . .
C37 C 0.2307(2) 0.5520(4) 0.6948(2) 0.0409(11) Uani 1 1 d . . .
H37 H 0.2662 0.5468 0.6674 0.049 Uiso 1 1 calc R . .
C38 C 0.1704(3) 0.5815(5) 0.6674(2) 0.0490(13) Uani 1 1 d . . .
H38 H 0.1352 0.5860 0.6953 0.059 Uiso 1 1 calc R . .
C39 C 0.1532(3) 0.6076(5) 0.5990(3) 0.0519(14) Uani 1 1 d . . .
C40 C 0.1994(3) 0.6176(6) 0.5518(3) 0.0684(17) Uani 1 1 d . . .
H40 H 0.2446 0.6077 0.5634 0.082 Uiso 1 1 calc R . .
C41 C 0.1802(4) 0.6420(7) 0.4876(3) 0.080(2) Uani 1 1 d . . .
H41 H 0.2125 0.6470 0.4567 0.096 Uiso 1 1 calc R . .
C42 C 0.1144(4) 0.6589(8) 0.4693(3) 0.091(2) Uani 1 1 d . . .
H42 H 0.1019 0.6789 0.4264 0.109 Uiso 1 1 calc R . .
C43 C 0.0669(4) 0.6463(8) 0.5143(3) 0.086(2) Uani 1 1 d . . .
H43 H 0.0218 0.6538 0.5017 0.103 Uiso 1 1 calc R . .
C44 C 0.0859(3) 0.6221(7) 0.5791(3) 0.078(2) Uani 1 1 d . . .
H44 H 0.0532 0.6156 0.6095 0.093 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 1.939(3) . ?
Ni1 N2 1.942(4) . ?
Ni1 C35 1.967(4) . ?
Ni1 C36 1.978(4) . ?
N1 C1 1.288(5) . ?
N1 C5 1.442(5) . ?
N2 C2 1.276(5) . ?
N2 C17 1.448(5) . ?
C1 C2 1.475(6) . ?
C1 C3 1.503(6) . ?
C2 C4 1.499(6) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 C6 1.391(6) . ?
C5 C10 1.399(6) . ?
C6 C7 1.399(6) . ?
C6 C11 1.526(6) . ?
C7 C8 1.371(7) . ?
C7 H7 0.9300 . ?
C8 C9 1.368(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.394(6) . ?
C9 H9 0.9300 . ?
C10 C14 1.507(7) . ?
C11 C12 1.514(7) . ?
C11 C13 1.527(7) . ?
C11 H11 0.9800 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C16 1.485(8) . ?
C14 C15 1.513(7) . ?
C14 H14 0.9800 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.396(6) . ?
C17 C22 1.406(6) . ?
C18 C19 1.390(7) . ?
C18 C23 1.523(6) . ?
C19 C20 1.377(8) . ?
C19 H19 0.9300 . ?
C20 C21 1.344(8) . ?
C20 H20 0.9300 . ?
C21 C22 1.397(7) . ?
C21 H21 0.9300 . ?
C22 C26 1.514(7) . ?
C23 C25 1.520(8) . ?
C23 C24 1.533(8) . ?
C23 H23 0.9800 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 C27 1.495(8) . ?
C26 C28 1.515(7) . ?
C26 H26 0.9800 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 C30 1.363(8) . ?
C29 C34 1.385(8) . ?
C29 H29 0.9300 . ?
C30 C31 1.371(7) . ?
C30 H30 0.9300 . ?
C31 C32 1.396(6) . ?
C31 H31 0.9300 . ?
C32 C33 1.396(7) . ?
C32 C35 1.485(6) . ?
C33 C34 1.387(7) . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
C35 C36 1.434(6) . ?
C35 H35 0.9800 . ?
C36 C37 1.455(6) . ?
C36 H36 0.9800 . ?
C37 C38 1.336(6) . ?
C37 H37 0.9300 . ?
C38 C39 1.460(7) . ?
C38 H38 0.9300 . ?
C39 C40 1.376(8) . ?
C39 C44 1.396(8) . ?
C40 C41 1.385(8) . ?
C40 H40 0.9300 . ?
C41 C42 1.361(9) . ?
C41 H41 0.9300 . ?
C42 C43 1.363(10) . ?
C42 H42 0.9300 . ?
C43 C44 1.394(8) . ?
C43 H43 0.9300 . ?
C44 H44 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N2 80.60(15) . . ?
N1 Ni1 C35 118.35(16) . . ?
N2 Ni1 C35 160.85(17) . . ?
N1 Ni1 C36 160.87(17) . . ?
N2 Ni1 C36 118.50(17) . . ?
C35 Ni1 C36 42.65(18) . . ?
C1 N1 C5 122.9(3) . . ?
C1 N1 Ni1 115.9(3) . . ?
C5 N1 Ni1 121.2(3) . . ?
C2 N2 C17 122.9(4) . . ?
C2 N2 Ni1 115.9(3) . . ?
C17 N2 Ni1 121.2(3) . . ?
N1 C1 C2 113.5(4) . . ?
N1 C1 C3 125.4(4) . . ?
C2 C1 C3 121.1(4) . . ?
N2 C2 C1 114.1(4) . . ?
N2 C2 C4 125.7(4) . . ?
C1 C2 C4 120.2(4) . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 C10 122.6(4) . . ?
C6 C5 N1 117.5(4) . . ?
C10 C5 N1 119.6(4) . . ?
C5 C6 C7 117.5(4) . . ?
C5 C6 C11 121.0(4) . . ?
C7 C6 C11 121.5(4) . . ?
C8 C7 C6 120.8(5) . . ?
C8 C7 H7 119.6 . . ?
C6 C7 H7 119.6 . . ?
C9 C8 C7 120.6(5) . . ?
C9 C8 H8 119.7 . . ?
C7 C8 H8 119.7 . . ?
C8 C9 C10 121.4(5) . . ?
C8 C9 H9 119.3 . . ?
C10 C9 H9 119.3 . . ?
C9 C10 C5 117.1(4) . . ?
C9 C10 C14 120.5(4) . . ?
C5 C10 C14 122.4(4) . . ?
C12 C11 C6 113.6(4) . . ?
C12 C11 C13 110.8(5) . . ?
C6 C11 C13 112.3(4) . . ?
C12 C11 H11 106.5 . . ?
C6 C11 H11 106.5 . . ?
C13 C11 H11 106.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C16 C14 C10 112.1(5) . . ?
C16 C14 C15 109.0(6) . . ?
C10 C14 C15 112.8(5) . . ?
C16 C14 H14 107.5 . . ?
C10 C14 H14 107.5 . . ?
C15 C14 H14 107.5 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 C22 123.0(4) . . ?
C18 C17 N2 117.6(4) . . ?
C22 C17 N2 119.3(4) . . ?
C19 C18 C17 117.0(4) . . ?
C19 C18 C23 121.8(4) . . ?
C17 C18 C23 121.2(4) . . ?
C20 C19 C18 121.0(5) . . ?
C20 C19 H19 119.5 . . ?
C18 C19 H19 119.5 . . ?
C21 C20 C19 120.7(5) . . ?
C21 C20 H20 119.6 . . ?
C19 C20 H20 119.6 . . ?
C20 C21 C22 122.2(5) . . ?
C20 C21 H21 118.9 . . ?
C22 C21 H21 118.9 . . ?
C21 C22 C17 116.0(5) . . ?
C21 C22 C26 121.1(4) . . ?
C17 C22 C26 122.8(4) . . ?
C25 C23 C18 114.5(5) . . ?
C25 C23 C24 112.6(5) . . ?
C18 C23 C24 110.1(5) . . ?
C25 C23 H23 106.4 . . ?
C18 C23 H23 106.4 . . ?
C24 C23 H23 106.4 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 C22 110.5(5) . . ?
C27 C26 C28 110.2(5) . . ?
C22 C26 C28 113.4(5) . . ?
C27 C26 H26 107.5 . . ?
C22 C26 H26 107.5 . . ?
C28 C26 H26 107.5 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 C34 118.9(5) . . ?
C30 C29 H29 120.6 . . ?
C34 C29 H29 120.6 . . ?
C29 C30 C31 121.0(6) . . ?
C29 C30 H30 119.5 . . ?
C31 C30 H30 119.5 . . ?
C30 C31 C32 121.7(6) . . ?
C30 C31 H31 119.1 . . ?
C32 C31 H31 119.1 . . ?
C31 C32 C33 116.9(5) . . ?
C31 C32 C35 118.9(5) . . ?
C33 C32 C35 124.2(4) . . ?
C34 C33 C32 120.8(5) . . ?
C34 C33 H33 119.6 . . ?
C32 C33 H33 119.6 . . ?
C29 C34 C33 120.6(6) . . ?
C29 C34 H34 119.7 . . ?
C33 C34 H34 119.7 . . ?
C36 C35 C32 124.1(4) . . ?
C36 C35 Ni1 69.1(2) . . ?
C32 C35 Ni1 113.1(3) . . ?
C36 C35 H35 114.1 . . ?
C32 C35 H35 114.1 . . ?
Ni1 C35 H35 114.1 . . ?
C35 C36 C37 121.8(5) . . ?
C35 C36 Ni1 68.3(2) . . ?
C37 C36 Ni1 109.1(3) . . ?
C35 C36 H36 116.0 . . ?
C37 C36 H36 116.0 . . ?
Ni1 C36 H36 116.0 . . ?
C38 C37 C36 126.1(5) . . ?
C38 C37 H37 116.9 . . ?
C36 C37 H37 116.9 . . ?
C37 C38 C39 127.8(5) . . ?
C37 C38 H38 116.1 . . ?
C39 C38 H38 116.1 . . ?
C40 C39 C44 116.9(5) . . ?
C40 C39 C38 124.2(5) . . ?
C44 C39 C38 118.9(5) . . ?
C39 C40 C41 121.7(6) . . ?
C39 C40 H40 119.1 . . ?
C41 C40 H40 119.1 . . ?
C42 C41 C40 120.5(7) . . ?
C42 C41 H41 119.8 . . ?
C40 C41 H41 119.8 . . ?
C41 C42 C43 119.7(6) . . ?
C41 C42 H42 120.2 . . ?
C43 C42 H42 120.2 . . ?
C42 C43 C44 120.1(6) . . ?
C42 C43 H43 120.0 . . ?
C44 C43 H43 120.0 . . ?
C43 C44 C39 121.1(7) . . ?
C43 C44 H44 119.4 . . ?
C39 C44 H44 119.4 . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.089
_chemical_properties_physical    
'Air-sensitive, Moisture-sensitive, Photo-sensitive'
