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

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

data_mcbc160928
_database_code_depnum_ccdc_archive 'CCDC 1585953'
_audit_update_record             
;
2017-11-16 deposited with the CCDC.
2017-12-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H13 N3 Ni'

_chemical_formula_sum            'C12 H13 N3 Ni'
_chemical_formula_weight         257.96

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   8.4784(2)
_cell_length_b                   17.3913(5)
_cell_length_c                   8.5806(2)
_cell_angle_alpha                90
_cell_angle_beta                 118.3620(10)
_cell_angle_gamma                90
_cell_volume                     1113.34(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    8234
_cell_measurement_theta_min      2.73
_cell_measurement_theta_max      32.97

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_F_000             536
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    1.716
_shelx_estimated_absorpt_T_min   0.610
_shelx_estimated_absorpt_T_max   0.795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6698
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  triumph
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16574
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.342
_diffrn_reflns_theta_max         33.049
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4192
_reflns_number_gt                3557
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0325P)²+0.2627P] 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         4192
_refine_ls_number_parameters     146
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0260
_refine_ls_wR_factor_ref         0.0648
_refine_ls_wR_factor_gt          0.0617
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.42580(14) 0.88558(6) 0.94762(14) 0.01858(19) Uani 1 1 d . . . . .
C2 C 0.49196(17) 0.93028(8) 1.21935(16) 0.0275(2) Uani 1 1 d . . . . .
H2 H 0.4797 0.9555 1.3113 0.033 Uiso 1 1 calc R U . . .
C3 C 0.63753(16) 0.89275(8) 1.23588(16) 0.0275(2) Uani 1 1 d . . . . .
H3 H 0.7475 0.8857 1.3415 0.033 Uiso 1 1 calc R U . . .
C4 C 0.18406(16) 0.95817(8) 0.97201(18) 0.0310(3) Uani 1 1 d . . . . .
H4A H 0.1734 1.0023 0.8967 0.046 Uiso 1 1 calc R U . . .
H4B H 0.1636 0.9750 1.0700 0.046 Uiso 1 1 calc R U . . .
H4C H 0.0948 0.9193 0.9018 0.046 Uiso 1 1 calc R U . . .
C5 C 0.69809(16) 0.81853(8) 1.00978(17) 0.0283(2) Uani 1 1 d . . . . .
H5A H 0.7092 0.7657 1.0568 0.034 Uiso 1 1 calc R U . . .
H5B H 0.8199 0.8399 1.0524 0.034 Uiso 1 1 calc R U . . .
C6 C 0.59669(16) 0.81762(7) 0.80673(17) 0.0238(2) Uani 1 1 d . . . . .
H6 H 0.5971 0.7642 0.7637 0.029 Uiso 1 1 calc R U . . .
C7 C 0.67437(16) 0.86968(7) 0.72994(17) 0.0244(2) Uani 1 1 d . . . . .
C8 C 0.07013(17) 0.81962(8) 0.58680(17) 0.0301(3) Uani 1 1 d . . . . .
H8 H 0.0054 0.8007 0.6437 0.036 Uiso 1 1 calc R U . . .
C9 C 0.1606(2) 0.77531(8) 0.51920(18) 0.0351(3) Uani 1 1 d . . . . .
H9 H 0.1671 0.7208 0.5199 0.042 Uiso 1 1 calc R U . . .
C10 C 0.2421(2) 0.82698(9) 0.44838(18) 0.0353(3) Uani 1 1 d . . . . .
H10 H 0.3185 0.8125 0.4007 0.042 Uiso 1 1 calc R U . . .
C11 C 0.19024(18) 0.90299(8) 0.46109(16) 0.0308(3) Uani 1 1 d . . . . .
H11 H 0.2165 0.9481 0.4151 0.037 Uiso 1 1 calc R U . . .
C12 C 0.09216(16) 0.89893(8) 0.55514(16) 0.0272(2) Uani 1 1 d . . . . .
H12 H 0.0479 0.9417 0.5916 0.033 Uiso 1 1 calc R U . . .
N1 N 0.36264(13) 0.92541(6) 1.04261(13) 0.02165(18) Uani 1 1 d . . . . .
N2 N 0.59545(13) 0.86647(6) 1.06877(13) 0.02165(18) Uani 1 1 d . . . . .
N3 N 0.73503(16) 0.91200(7) 0.67011(16) 0.0339(2) Uani 1 1 d . . . . .
Ni1 Ni 0.34723(2) 0.85190(2) 0.71830(2) 0.01819(5) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N2 1.3563(14) . ?
C1 N1 1.3585(14) . ?
C1 Ni1 1.8475(11) . ?
C2 C3 1.3429(19) . ?
C2 N1 1.3890(15) . ?
C2 H2 0.9500 . ?
C3 N2 1.3807(16) . ?
C3 H3 0.9500 . ?
C4 N1 1.4534(15) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 N2 1.4585(15) . ?
C5 C6 1.5336(18) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.4491(17) . ?
C6 Ni1 1.9697(11) . ?
C6 H6 1.0000 . ?
C7 N3 1.1491(17) . ?
C8 C9 1.393(2) . ?
C8 C12 1.4350(19) . ?
C8 Ni1 2.1423(12) . ?
C8 H8 0.9500 . ?
C9 C10 1.433(2) . ?
C9 Ni1 2.1514(13) . ?
C9 H9 0.9500 . ?
C10 C11 1.413(2) . ?
C10 Ni1 2.0941(13) . ?
C10 H10 0.9500 . ?
C11 C12 1.4090(19) . ?
C11 Ni1 2.1543(12) . ?
C11 H11 0.9500 . ?
C12 Ni1 2.1045(12) . ?
C12 H12 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
N2 C1 N1 104.00(9) . . ?
N2 C1 Ni1 116.95(8) . . ?
N1 C1 Ni1 139.04(8) . . ?
C3 C2 N1 107.15(11) . . ?
C3 C2 H2 126.4 . . ?
N1 C2 H2 126.4 . . ?
C2 C3 N2 106.26(10) . . ?
C2 C3 H3 126.9 . . ?
N2 C3 H3 126.9 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 C6 107.17(9) . . ?
N2 C5 H5A 110.3 . . ?
C6 C5 H5A 110.3 . . ?
N2 C5 H5B 110.3 . . ?
C6 C5 H5B 110.3 . . ?
H5A C5 H5B 108.5 . . ?
C7 C6 C5 112.31(11) . . ?
C7 C6 Ni1 105.82(8) . . ?
C5 C6 Ni1 110.76(8) . . ?
C7 C6 H6 109.3 . . ?
C5 C6 H6 109.3 . . ?
Ni1 C6 H6 109.3 . . ?
N3 C7 C6 178.84(14) . . ?
C9 C8 C12 107.81(12) . . ?
C9 C8 Ni1 71.42(8) . . ?
C12 C8 Ni1 68.84(7) . . ?
C9 C8 H8 126.1 . . ?
C12 C8 H8 126.1 . . ?
Ni1 C8 H8 125.2 . . ?
C8 C9 C10 107.54(12) . . ?
C8 C9 Ni1 70.71(7) . . ?
C10 C9 Ni1 68.13(7) . . ?
C8 C9 H9 126.2 . . ?
C10 C9 H9 126.2 . . ?
Ni1 C9 H9 126.5 . . ?
C11 C10 C9 108.88(13) . . ?
C11 C10 Ni1 72.88(7) . . ?
C9 C10 Ni1 72.45(8) . . ?
C11 C10 H10 125.6 . . ?
C9 C10 H10 125.6 . . ?
Ni1 C10 H10 120.8 . . ?
C12 C11 C10 106.68(12) . . ?
C12 C11 Ni1 68.78(7) . . ?
C10 C11 Ni1 68.28(7) . . ?
C12 C11 H11 126.7 . . ?
C10 C11 H11 126.7 . . ?
Ni1 C11 H11 127.8 . . ?
C11 C12 C8 108.78(12) . . ?
C11 C12 Ni1 72.60(7) . . ?
C8 C12 Ni1 71.68(7) . . ?
C11 C12 H12 125.6 . . ?
C8 C12 H12 125.6 . . ?
Ni1 C12 H12 121.8 . . ?
C1 N1 C2 110.76(10) . . ?
C1 N1 C4 125.40(10) . . ?
C2 N1 C4 123.83(10) . . ?
C1 N2 C3 111.82(10) . . ?
C1 N2 C5 117.68(10) . . ?
C3 N2 C5 130.33(10) . . ?
C1 Ni1 C6 84.71(5) . . ?
C1 Ni1 C10 172.86(5) . . ?
C6 Ni1 C10 100.28(6) . . ?
C1 Ni1 C12 108.78(5) . . ?
C6 Ni1 C12 161.79(5) . . ?
C10 Ni1 C12 65.27(6) . . ?
C1 Ni1 C8 113.23(5) . . ?
C6 Ni1 C8 146.28(5) . . ?
C10 Ni1 C8 65.10(6) . . ?
C12 Ni1 C8 39.48(5) . . ?
C1 Ni1 C9 143.04(5) . . ?
C6 Ni1 C9 111.63(6) . . ?
C10 Ni1 C9 39.42(6) . . ?
C12 Ni1 C9 64.95(5) . . ?
C8 Ni1 C9 37.87(6) . . ?
C1 Ni1 C11 134.04(5) . . ?
C6 Ni1 C11 123.18(5) . . ?
C10 Ni1 C11 38.83(6) . . ?
C12 Ni1 C11 38.62(5) . . ?
C8 Ni1 C11 65.11(5) . . ?
C9 Ni1 C11 65.07(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
N1 C2 C3 N2 0.73(14) . . . . ?
N2 C5 C6 C7 100.66(12) . . . . ?
N2 C5 C6 Ni1 -17.41(12) . . . . ?
C12 C8 C9 C10 1.10(15) . . . . ?
Ni1 C8 C9 C10 -58.37(9) . . . . ?
C12 C8 C9 Ni1 59.47(8) . . . . ?
C8 C9 C10 C11 -4.26(16) . . . . ?
Ni1 C9 C10 C11 -64.25(9) . . . . ?
C8 C9 C10 Ni1 59.99(9) . . . . ?
C9 C10 C11 C12 5.71(15) . . . . ?
Ni1 C10 C11 C12 -58.27(9) . . . . ?
C9 C10 C11 Ni1 63.97(10) . . . . ?
C10 C11 C12 C8 -5.02(14) . . . . ?
Ni1 C11 C12 C8 -62.96(8) . . . . ?
C10 C11 C12 Ni1 57.95(9) . . . . ?
C9 C8 C12 C11 2.45(14) . . . . ?
Ni1 C8 C12 C11 63.55(9) . . . . ?
C9 C8 C12 Ni1 -61.10(9) . . . . ?
N2 C1 N1 C2 -0.18(13) . . . . ?
Ni1 C1 N1 C2 178.37(11) . . . . ?
N2 C1 N1 C4 -179.53(11) . . . . ?
Ni1 C1 N1 C4 -1.0(2) . . . . ?
C3 C2 N1 C1 -0.36(14) . . . . ?
C3 C2 N1 C4 179.01(12) . . . . ?
N1 C1 N2 C3 0.66(13) . . . . ?
Ni1 C1 N2 C3 -178.28(8) . . . . ?
N1 C1 N2 C5 176.40(10) . . . . ?
Ni1 C1 N2 C5 -2.54(14) . . . . ?
C2 C3 N2 C1 -0.90(14) . . . . ?
C2 C3 N2 C5 -175.94(12) . . . . ?
C6 C5 N2 C1 13.28(14) . . . . ?
C6 C5 N2 C3 -171.91(12) . . . . ?
N2 C1 Ni1 C6 -6.80(9) . . . . ?
N1 C1 Ni1 C6 174.78(13) . . . . ?
N2 C1 Ni1 C12 -174.25(8) . . . . ?
N1 C1 Ni1 C12 7.33(14) . . . . ?
N2 C1 Ni1 C8 143.58(9) . . . . ?
N1 C1 Ni1 C8 -34.84(14) . . . . ?
N2 C1 Ni1 C9 112.72(11) . . . . ?
N1 C1 Ni1 C9 -65.70(16) . . . . ?
N2 C1 Ni1 C11 -139.25(9) . . . . ?
N1 C1 Ni1 C11 42.33(16) . . . . ?

_refine_diff_density_max         0.419
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.058

_shelxl_version_number           2013-4



_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: thf'
_chemical_properties_physical    Air-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_mcbc161020
_database_code_depnum_ccdc_archive 'CCDC 1585956'
_audit_update_record             
;
2017-11-16 deposited with the CCDC.
2017-12-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H21 N3 Ni'
_chemical_formula_sum            'C20 H21 N3 Ni'
_chemical_formula_weight         362.11

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   9.3425(10)
_cell_length_b                   13.7491(15)
_cell_length_c                   14.2032(15)
_cell_angle_alpha                80.591(6)
_cell_angle_beta                 86.833(7)
_cell_angle_gamma                82.101(7)
_cell_volume                     1781.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    7379
_cell_measurement_theta_min      5.44
_cell_measurement_theta_max      65.39

_exptl_crystal_description       needle
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_F_000             760
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    1.592
_shelx_estimated_absorpt_T_min   0.692
_shelx_estimated_absorpt_T_max   0.911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6172
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  mirror
_diffrn_source                   'Cu-ImuS microfocus tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27037
_diffrn_reflns_av_unetI/netI     0.0639
_diffrn_reflns_av_R_equivalents  0.0760
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.156
_diffrn_reflns_theta_max         67.104
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measured_fraction_theta_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_point_group_measured_fraction_full 0.962
_reflns_number_total             6205
_reflns_number_gt                4232
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1380P)²+4.0164P] 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         6205
_refine_ls_number_parameters     415
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1173
_refine_ls_R_factor_gt           0.0883
_refine_ls_wR_factor_ref         0.2721
_refine_ls_wR_factor_gt          0.2462
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8082(6) 0.1420(4) 0.5436(3) 0.0369(12) Uani 1 1 d . . . . .
C2 C 0.6045(7) 0.0698(4) 0.5762(4) 0.0486(14) Uani 1 1 d . . . . .
H2 H 0.5058 0.0595 0.5773 0.058 Uiso 1 1 calc R U . . .
C3 C 0.7121(6) 0.0076(4) 0.6212(4) 0.0480(14) Uani 1 1 d . . . . .
H3 H 0.7052 -0.0554 0.6591 0.058 Uiso 1 1 calc R U . . .
C4 C 0.5842(6) 0.2327(4) 0.4661(4) 0.0411(12) Uani 1 1 d . . . . .
C5 C 0.5829(6) 0.2268(4) 0.3702(4) 0.0453(13) Uani 1 1 d . . . . .
C6 C 0.5054(7) 0.3062(5) 0.3108(4) 0.0521(14) Uani 1 1 d . . . . .
H6 H 0.5007 0.3036 0.2446 0.063 Uiso 1 1 calc R U . . .
C7 C 0.4361(6) 0.3877(4) 0.3474(5) 0.0511(14) Uani 1 1 d . . . . .
C8 C 0.4427(6) 0.3921(4) 0.4428(5) 0.0501(14) Uani 1 1 d . . . . .
H8 H 0.3972 0.4497 0.4668 0.060 Uiso 1 1 calc R U . . .
C9 C 0.5151(6) 0.3138(4) 0.5058(4) 0.0447(13) Uani 1 1 d . . . . .
C10 C 0.6620(8) 0.1398(5) 0.3278(4) 0.0599(17) Uani 1 1 d . . . . .
H10A H 0.7665 0.1400 0.3307 0.090 Uiso 1 1 calc R U . . .
H10B H 0.6358 0.1453 0.2611 0.090 Uiso 1 1 calc R U . . .
H10C H 0.6351 0.0776 0.3641 0.090 Uiso 1 1 calc R U . . .
C11 C 0.3533(9) 0.4722(5) 0.2807(6) 0.078(2) Uani 1 1 d . . . . .
H11A H 0.4212 0.5149 0.2463 0.116 Uiso 1 1 calc R U . . .
H11B H 0.2832 0.5114 0.3181 0.116 Uiso 1 1 calc R U . . .
H11C H 0.3022 0.4446 0.2348 0.116 Uiso 1 1 calc R U . . .
C12 C 0.5192(8) 0.3169(5) 0.6107(4) 0.0602(17) Uani 1 1 d . . . . .
H12A H 0.4706 0.2629 0.6466 0.090 Uiso 1 1 calc R U . . .
H12B H 0.4697 0.3809 0.6244 0.090 Uiso 1 1 calc R U . . .
H12C H 0.6200 0.3090 0.6296 0.090 Uiso 1 1 calc R U . . .
C13 C 0.9834(6) 0.0185(4) 0.6292(4) 0.0457(13) Uani 1 1 d . . . . .
H13A H 1.0150 -0.0477 0.6105 0.055 Uiso 1 1 calc R U . . .
H13B H 0.9907 0.0128 0.6992 0.055 Uiso 1 1 calc R U . . .
C14 C 1.0772(7) 0.0948(4) 0.5773(4) 0.0499(14) Uani 1 1 d . . . . .
H14 H 1.1390 0.0617 0.5289 0.060 Uiso 1 1 calc R U . . .
C15 C 1.1740(7) 0.1253(5) 0.6394(4) 0.0509(14) Uani 1 1 d . . . . .
C16 C 0.9299(9) 0.3717(5) 0.4863(6) 0.076(2) Uani 1 1 d . . . . .
H16 H 0.8668 0.4130 0.5223 0.091 Uiso 1 1 calc R U . . .
C17 C 1.0731(9) 0.3380(5) 0.5043(5) 0.0668(18) Uani 1 1 d . . . . .
H17 H 1.1256 0.3500 0.5557 0.080 Uiso 1 1 calc R U . . .
C18 C 1.1265(8) 0.2825(5) 0.4322(6) 0.0672(19) Uani 1 1 d . . . . .
H18 H 1.2214 0.2479 0.4285 0.081 Uiso 1 1 calc R U . . .
C19 C 1.0214(9) 0.2860(5) 0.3683(5) 0.072(2) Uani 1 1 d . . . . .
H19 H 1.0324 0.2604 0.3098 0.087 Uiso 1 1 calc R U . . .
C20 C 0.8929(8) 0.3350(5) 0.4060(6) 0.074(2) Uani 1 1 d . . . . .
H20 H 0.7990 0.3417 0.3813 0.089 Uiso 1 1 calc R U . . .
C21 C 0.6297(6) 0.1479(4) 1.0397(4) 0.0426(13) Uani 1 1 d . . . . .
C22 C 0.8596(7) 0.0795(4) 1.0681(4) 0.0501(14) Uani 1 1 d . . . . .
H22 H 0.9624 0.0702 1.0664 0.060 Uiso 1 1 calc R U . . .
C23 C 0.7734(7) 0.0169(4) 1.1166(4) 0.0527(15) Uani 1 1 d . . . . .
H23 H 0.8028 -0.0449 1.1555 0.063 Uiso 1 1 calc R U . . .
C24 C 0.8238(6) 0.2412(4) 0.9583(4) 0.0417(12) Uani 1 1 d . . . . .
C25 C 0.8503(7) 0.3249(4) 0.9942(5) 0.0522(15) Uani 1 1 d . . . . .
C26 C 0.9087(7) 0.3998(5) 0.9317(5) 0.0580(16) Uani 1 1 d . . . . .
H26 H 0.9232 0.4591 0.9540 0.070 Uiso 1 1 calc R U . . .
C27 C 0.9460(7) 0.3895(5) 0.8373(5) 0.0565(16) Uani 1 1 d . . . . .
C28 C 0.9139(7) 0.3074(4) 0.8037(4) 0.0520(15) Uani 1 1 d . . . . .
H28 H 0.9342 0.3018 0.7384 0.062 Uiso 1 1 calc R U . . .
C29 C 0.8518(6) 0.2317(4) 0.8632(4) 0.0471(13) Uani 1 1 d . . . . .
C30 C 0.8169(9) 0.3347(6) 1.0980(5) 0.075(2) Uani 1 1 d . . . . .
H30A H 0.7249 0.3099 1.1183 0.113 Uiso 1 1 calc R U . . .
H30B H 0.8101 0.4048 1.1056 0.113 Uiso 1 1 calc R U . . .
H30C H 0.8943 0.2959 1.1373 0.113 Uiso 1 1 calc R U . . .
C31 C 1.0206(9) 0.4669(6) 0.7730(6) 0.084(2) Uani 1 1 d . . . . .
H31A H 1.1254 0.4518 0.7804 0.125 Uiso 1 1 calc R U . . .
H31B H 0.9869 0.5326 0.7902 0.125 Uiso 1 1 calc R U . . .
H31C H 0.9981 0.4666 0.7065 0.125 Uiso 1 1 calc R U . . .
C32 C 0.8159(9) 0.1436(5) 0.8238(4) 0.0642(18) Uani 1 1 d . . . . .
H32A H 0.8672 0.0826 0.8588 0.096 Uiso 1 1 calc R U . . .
H32B H 0.8455 0.1495 0.7561 0.096 Uiso 1 1 calc R U . . .
H32C H 0.7115 0.1411 0.8308 0.096 Uiso 1 1 calc R U . . .
C33 C 0.4967(7) 0.0246(5) 1.1334(4) 0.0552(15) Uani 1 1 d . . . . .
H33A H 0.4823 0.0261 1.2028 0.066 Uiso 1 1 calc R U . . .
H33B H 0.4967 -0.0446 1.1223 0.066 Uiso 1 1 calc R U . . .
C34 C 0.3755(7) 0.0937(5) 1.0783(4) 0.0575(16) Uani 1 1 d . . . . .
H34 H 0.3414 0.0571 1.0303 0.069 Uiso 1 1 calc R U . . .
C35 C 0.2536(7) 0.1219(5) 1.1383(4) 0.0546(15) Uani 1 1 d . . . . .
C36 C 0.3565(10) 0.2835(6) 0.8740(7) 0.0891(12) Uani 1 1 d . . . . .
H36 H 0.3469 0.2543 0.8189 0.107 Uiso 1 1 calc R U . . .
C37 C 0.2604(10) 0.2878(6) 0.9483(7) 0.0891(12) Uani 1 1 d . . . . .
H37 H 0.1751 0.2564 0.9558 0.107 Uiso 1 1 calc R U . . .
C38 C 0.3021(10) 0.3439(6) 1.0120(7) 0.0891(12) Uani 1 1 d . . . . .
H38 H 0.2506 0.3611 1.0678 0.107 Uiso 1 1 calc R U . . .
C39 C 0.4378(10) 0.3701(6) 0.9761(7) 0.0891(12) Uani 1 1 d . . . . .
H39 H 0.4963 0.4087 1.0035 0.107 Uiso 1 1 calc R U . . .
C40 C 0.4702(10) 0.3292(6) 0.8932(7) 0.0891(12) Uani 1 1 d . . . . .
H40 H 0.5574 0.3323 0.8558 0.107 Uiso 1 1 calc R U . . .
N1 N 0.6635(5) 0.1513(3) 0.5279(3) 0.0403(10) Uani 1 1 d . . . . .
N2 N 0.8354(5) 0.0542(3) 0.6010(3) 0.0392(10) Uani 1 1 d . . . . .
N3 N 1.2496(8) 0.1509(5) 0.6882(5) 0.0803(18) Uani 1 1 d . . . . .
N4 N 0.7714(5) 0.1603(3) 1.0210(3) 0.0430(11) Uani 1 1 d . . . . .
N5 N 0.6340(5) 0.0600(3) 1.0989(3) 0.0444(11) Uani 1 1 d . . . . .
N6 N 0.1543(7) 0.1442(5) 1.1835(5) 0.087(2) Uani 1 1 d . . . . .
Ni1 Ni 0.96197(10) 0.21224(6) 0.50708(6) 0.0449(3) Uani 1 1 d . . . . .
Ni2 Ni 0.44963(10) 0.21411(7) 1.00770(7) 0.0514(4) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N2 1.343(6) . ?
C1 N1 1.367(7) . ?
C1 Ni1 1.844(5) . ?
C2 C3 1.344(8) . ?
C2 N1 1.381(7) . ?
C2 H2 0.9500 . ?
C3 N2 1.387(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.379(8) . ?
C4 C9 1.395(8) . ?
C4 N1 1.447(7) . ?
C5 C6 1.406(8) . ?
C5 C10 1.512(8) . ?
C6 C7 1.378(9) . ?
C6 H6 0.9500 . ?
C7 C8 1.372(9) . ?
C7 C11 1.523(8) . ?
C8 C9 1.403(8) . ?
C8 H8 0.9500 . ?
C9 C12 1.500(8) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
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 N2 1.458(7) . ?
C13 C14 1.530(8) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.444(9) . ?
C14 Ni1 1.969(6) . ?
C14 H14 1.0000 . ?
C15 N3 1.142(8) . ?
C16 C17 1.378(11) . ?
C16 C20 1.397(12) . ?
C16 Ni1 2.145(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.405(10) . ?
C17 Ni1 2.130(7) . ?
C17 H17 0.9500 . ?
C18 C19 1.364(11) . ?
C18 Ni1 2.078(7) . ?
C18 H18 0.9500 . ?
C19 C20 1.417(11) . ?
C19 Ni1 2.145(6) . ?
C19 H19 0.9500 . ?
C20 Ni1 2.082(6) . ?
C20 H20 0.9500 . ?
C21 N5 1.352(7) . ?
C21 N4 1.364(7) . ?
C21 Ni2 1.842(6) . ?
C22 C23 1.342(9) . ?
C22 N4 1.389(7) . ?
C22 H22 0.9500 . ?
C23 N5 1.373(7) . ?
C23 H23 0.9500 . ?
C24 C29 1.386(8) . ?
C24 C25 1.389(8) . ?
C24 N4 1.431(7) . ?
C25 C26 1.397(9) . ?
C25 C30 1.514(9) . ?
C26 C27 1.391(9) . ?
C26 H26 0.9500 . ?
C27 C28 1.370(9) . ?
C27 C31 1.506(9) . ?
C28 C29 1.400(8) . ?
C28 H28 0.9500 . ?
C29 C32 1.499(9) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 N5 1.465(8) . ?
C33 C34 1.536(9) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.432(9) . ?
C34 Ni2 1.980(7) . ?
C34 H34 1.0000 . ?
C35 N6 1.135(8) . ?
C36 C37 1.350(12) . ?
C36 C40 1.366(13) . ?
C36 Ni2 2.153(9) . ?
C36 H36 0.9500 . ?
C37 C38 1.385(13) . ?
C37 Ni2 2.064(8) . ?
C37 H37 0.9500 . ?
C38 C39 1.412(12) . ?
C38 Ni2 2.107(8) . ?
C38 H38 0.9500 . ?
C39 C40 1.387(13) . ?
C39 Ni2 2.107(8) . ?
C39 H39 0.9500 . ?
C40 Ni2 2.096(8) . ?
C40 H40 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
N2 C1 N1 104.3(4) . . ?
N2 C1 Ni1 117.4(4) . . ?
N1 C1 Ni1 138.3(4) . . ?
C3 C2 N1 107.5(5) . . ?
C3 C2 H2 126.3 . . ?
N1 C2 H2 126.3 . . ?
C2 C3 N2 105.9(5) . . ?
C2 C3 H3 127.0 . . ?
N2 C3 H3 127.0 . . ?
C5 C4 C9 123.2(5) . . ?
C5 C4 N1 118.1(5) . . ?
C9 C4 N1 118.8(5) . . ?
C4 C5 C6 117.6(5) . . ?
C4 C5 C10 122.6(5) . . ?
C6 C5 C10 119.8(5) . . ?
C7 C6 C5 120.8(6) . . ?
C7 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
C8 C7 C6 119.9(5) . . ?
C8 C7 C11 120.8(6) . . ?
C6 C7 C11 119.2(6) . . ?
C7 C8 C9 121.7(5) . . ?
C7 C8 H8 119.2 . . ?
C9 C8 H8 119.2 . . ?
C4 C9 C8 116.7(5) . . ?
C4 C9 C12 121.3(5) . . ?
C8 C9 C12 121.9(5) . . ?
C5 C10 H10A 109.5 . . ?
C5 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C5 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C7 C11 H11A 109.5 . . ?
C7 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C7 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N2 C13 C14 106.5(4) . . ?
N2 C13 H13A 110.4 . . ?
C14 C13 H13A 110.4 . . ?
N2 C13 H13B 110.4 . . ?
C14 C13 H13B 110.4 . . ?
H13A C13 H13B 108.6 . . ?
C15 C14 C13 113.2(5) . . ?
C15 C14 Ni1 110.1(4) . . ?
C13 C14 Ni1 112.5(4) . . ?
C15 C14 H14 106.9 . . ?
C13 C14 H14 106.9 . . ?
Ni1 C14 H14 106.9 . . ?
N3 C15 C14 179.0(7) . . ?
C17 C16 C20 108.7(6) . . ?
C17 C16 Ni1 70.6(4) . . ?
C20 C16 Ni1 68.3(4) . . ?
C17 C16 H16 125.7 . . ?
C20 C16 H16 125.7 . . ?
Ni1 C16 H16 127.0 . . ?
C16 C17 C18 106.9(7) . . ?
C16 C17 Ni1 71.8(4) . . ?
C18 C17 Ni1 68.5(4) . . ?
C16 C17 H17 126.6 . . ?
C18 C17 H17 126.6 . . ?
Ni1 C17 H17 124.7 . . ?
C19 C18 C17 109.7(7) . . ?
C19 C18 Ni1 73.8(4) . . ?
C17 C18 Ni1 72.5(4) . . ?
C19 C18 H18 125.1 . . ?
C17 C18 H18 125.1 . . ?
Ni1 C18 H18 120.2 . . ?
C18 C19 C20 106.9(7) . . ?
C18 C19 Ni1 68.5(4) . . ?
C20 C19 Ni1 68.1(4) . . ?
C18 C19 H19 126.6 . . ?
C20 C19 H19 126.6 . . ?
Ni1 C19 H19 128.4 . . ?
C16 C20 C19 107.3(7) . . ?
C16 C20 Ni1 73.2(4) . . ?
C19 C20 Ni1 72.8(4) . . ?
C16 C20 H20 126.4 . . ?
C19 C20 H20 126.4 . . ?
Ni1 C20 H20 119.6 . . ?
N5 C21 N4 104.4(5) . . ?
N5 C21 Ni2 117.0(4) . . ?
N4 C21 Ni2 138.6(4) . . ?
C23 C22 N4 107.5(5) . . ?
C23 C22 H22 126.3 . . ?
N4 C22 H22 126.3 . . ?
C22 C23 N5 106.4(5) . . ?
C22 C23 H23 126.8 . . ?
N5 C23 H23 126.8 . . ?
C29 C24 C25 121.8(5) . . ?
C29 C24 N4 118.4(5) . . ?
C25 C24 N4 119.8(5) . . ?
C24 C25 C26 118.0(6) . . ?
C24 C25 C30 121.1(6) . . ?
C26 C25 C30 120.9(6) . . ?
C27 C26 C25 121.3(6) . . ?
C27 C26 H26 119.3 . . ?
C25 C26 H26 119.3 . . ?
C28 C27 C26 118.8(6) . . ?
C28 C27 C31 120.4(6) . . ?
C26 C27 C31 120.8(7) . . ?
C27 C28 C29 121.6(6) . . ?
C27 C28 H28 119.2 . . ?
C29 C28 H28 119.2 . . ?
C24 C29 C28 118.2(5) . . ?
C24 C29 C32 121.5(5) . . ?
C28 C29 C32 120.3(5) . . ?
C25 C30 H30A 109.5 . . ?
C25 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C25 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C27 C31 H31A 109.5 . . ?
C27 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C27 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N5 C33 C34 107.5(5) . . ?
N5 C33 H33A 110.2 . . ?
C34 C33 H33A 110.2 . . ?
N5 C33 H33B 110.2 . . ?
C34 C33 H33B 110.2 . . ?
H33A C33 H33B 108.5 . . ?
C35 C34 C33 113.0(5) . . ?
C35 C34 Ni2 109.8(4) . . ?
C33 C34 Ni2 110.7(5) . . ?
C35 C34 H34 107.7 . . ?
C33 C34 H34 107.7 . . ?
Ni2 C34 H34 107.7 . . ?
N6 C35 C34 177.8(8) . . ?
C37 C36 C40 107.0(10) . . ?
C37 C36 Ni2 67.8(5) . . ?
C40 C36 Ni2 69.0(5) . . ?
C37 C36 H36 126.5 . . ?
C40 C36 H36 126.5 . . ?
Ni2 C36 H36 128.3 . . ?
C36 C37 C38 111.2(10) . . ?
C36 C37 Ni2 74.9(5) . . ?
C38 C37 Ni2 72.3(5) . . ?
C36 C37 H37 124.4 . . ?
C38 C37 H37 124.4 . . ?
Ni2 C37 H37 119.9 . . ?
C37 C38 C39 105.0(9) . . ?
C37 C38 Ni2 68.9(5) . . ?
C39 C38 Ni2 70.4(5) . . ?
C37 C38 H38 127.5 . . ?
C39 C38 H38 127.5 . . ?
Ni2 C38 H38 124.8 . . ?
C40 C39 C38 107.4(10) . . ?
C40 C39 Ni2 70.3(5) . . ?
C38 C39 Ni2 70.4(5) . . ?
C40 C39 H39 126.3 . . ?
C38 C39 H39 126.3 . . ?
Ni2 C39 H39 124.6 . . ?
C36 C40 C39 109.1(9) . . ?
C36 C40 Ni2 73.5(5) . . ?
C39 C40 Ni2 71.2(5) . . ?
C36 C40 H40 125.5 . . ?
C39 C40 H40 125.5 . . ?
Ni2 C40 H40 121.5 . . ?
C1 N1 C2 110.4(4) . . ?
C1 N1 C4 125.0(4) . . ?
C2 N1 C4 124.5(5) . . ?
C1 N2 C3 111.9(5) . . ?
C1 N2 C13 118.9(5) . . ?
C3 N2 C13 129.1(5) . . ?
C21 N4 C22 109.9(5) . . ?
C21 N4 C24 125.9(4) . . ?
C22 N4 C24 124.1(5) . . ?
C21 N5 C23 111.8(5) . . ?
C21 N5 C33 118.3(5) . . ?
C23 N5 C33 129.9(5) . . ?
C1 Ni1 C14 84.3(2) . . ?
C1 Ni1 C18 165.5(3) . . ?
C14 Ni1 C18 99.9(3) . . ?
C1 Ni1 C20 108.7(3) . . ?
C14 Ni1 C20 163.3(3) . . ?
C18 Ni1 C20 64.9(3) . . ?
C1 Ni1 C17 152.2(3) . . ?
C14 Ni1 C17 108.6(3) . . ?
C18 Ni1 C17 39.0(3) . . ?
C20 Ni1 C17 64.7(3) . . ?
C1 Ni1 C19 129.3(3) . . ?
C14 Ni1 C19 124.3(3) . . ?
C18 Ni1 C19 37.6(3) . . ?
C20 Ni1 C19 39.1(3) . . ?
C17 Ni1 C19 64.0(3) . . ?
C1 Ni1 C16 120.1(3) . . ?
C14 Ni1 C16 142.8(3) . . ?
C18 Ni1 C16 63.9(3) . . ?
C20 Ni1 C16 38.6(3) . . ?
C17 Ni1 C16 37.6(3) . . ?
C19 Ni1 C16 63.8(3) . . ?
C21 Ni2 C34 85.2(3) . . ?
C21 Ni2 C37 170.3(3) . . ?
C34 Ni2 C37 99.3(3) . . ?
C21 Ni2 C40 109.7(3) . . ?
C34 Ni2 C40 156.4(4) . . ?
C37 Ni2 C40 63.3(4) . . ?
C21 Ni2 C38 146.5(3) . . ?
C34 Ni2 C38 112.5(3) . . ?
C37 Ni2 C38 38.8(3) . . ?
C40 Ni2 C38 64.9(4) . . ?
C21 Ni2 C39 115.2(3) . . ?
C34 Ni2 C39 150.2(3) . . ?
C37 Ni2 C39 64.2(4) . . ?
C40 Ni2 C39 38.5(3) . . ?
C38 Ni2 C39 39.1(3) . . ?
C21 Ni2 C36 133.1(3) . . ?
C34 Ni2 C36 119.2(3) . . ?
C37 Ni2 C36 37.3(3) . . ?
C40 Ni2 C36 37.5(3) . . ?
C38 Ni2 C36 64.0(4) . . ?
C39 Ni2 C36 63.5(4) . . ?

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 C2 C3 N2 1.4(6) . . . . ?
C9 C4 C5 C6 -1.2(9) . . . . ?
N1 C4 C5 C6 179.9(5) . . . . ?
C9 C4 C5 C10 178.1(6) . . . . ?
N1 C4 C5 C10 -0.8(8) . . . . ?
C4 C5 C6 C7 1.4(9) . . . . ?
C10 C5 C6 C7 -178.0(6) . . . . ?
C5 C6 C7 C8 0.2(9) . . . . ?
C5 C6 C7 C11 180.0(6) . . . . ?
C6 C7 C8 C9 -2.0(9) . . . . ?
C11 C7 C8 C9 178.2(6) . . . . ?
C5 C4 C9 C8 -0.5(9) . . . . ?
N1 C4 C9 C8 178.4(5) . . . . ?
C5 C4 C9 C12 179.9(6) . . . . ?
N1 C4 C9 C12 -1.2(8) . . . . ?
C7 C8 C9 C4 2.2(9) . . . . ?
C7 C8 C9 C12 -178.2(6) . . . . ?
N2 C13 C14 C15 131.3(5) . . . . ?
N2 C13 C14 Ni1 5.7(5) . . . . ?
C20 C16 C17 C18 2.0(8) . . . . ?
Ni1 C16 C17 C18 59.8(5) . . . . ?
C20 C16 C17 Ni1 -57.8(5) . . . . ?
C16 C17 C18 C19 3.0(8) . . . . ?
Ni1 C17 C18 C19 65.0(5) . . . . ?
C16 C17 C18 Ni1 -61.9(5) . . . . ?
C17 C18 C19 C20 -6.7(8) . . . . ?
Ni1 C18 C19 C20 57.4(5) . . . . ?
C17 C18 C19 Ni1 -64.1(5) . . . . ?
C17 C16 C20 C19 -6.1(8) . . . . ?
Ni1 C16 C20 C19 -65.3(5) . . . . ?
C17 C16 C20 Ni1 59.2(5) . . . . ?
C18 C19 C20 C16 7.9(8) . . . . ?
Ni1 C19 C20 C16 65.5(5) . . . . ?
C18 C19 C20 Ni1 -57.7(5) . . . . ?
N4 C22 C23 N5 -0.1(6) . . . . ?
C29 C24 C25 C26 -0.9(9) . . . . ?
N4 C24 C25 C26 176.7(5) . . . . ?
C29 C24 C25 C30 179.1(6) . . . . ?
N4 C24 C25 C30 -3.4(9) . . . . ?
C24 C25 C26 C27 -3.1(9) . . . . ?
C30 C25 C26 C27 177.0(6) . . . . ?
C25 C26 C27 C28 5.2(9) . . . . ?
C25 C26 C27 C31 -174.7(6) . . . . ?
C26 C27 C28 C29 -3.5(9) . . . . ?
C31 C27 C28 C29 176.5(6) . . . . ?
C25 C24 C29 C28 2.6(8) . . . . ?
N4 C24 C29 C28 -175.0(5) . . . . ?
C25 C24 C29 C32 -176.8(6) . . . . ?
N4 C24 C29 C32 5.6(8) . . . . ?
C27 C28 C29 C24 -0.4(9) . . . . ?
C27 C28 C29 C32 179.1(6) . . . . ?
N5 C33 C34 C35 -135.9(6) . . . . ?
N5 C33 C34 Ni2 -12.3(6) . . . . ?
C40 C36 C37 C38 5.8(9) . . . . ?
Ni2 C36 C37 C38 63.8(5) . . . . ?
C40 C36 C37 Ni2 -58.0(5) . . . . ?
C36 C37 C38 C39 -3.7(8) . . . . ?
Ni2 C37 C38 C39 61.7(5) . . . . ?
C36 C37 C38 Ni2 -65.4(5) . . . . ?
C37 C38 C39 C40 0.2(8) . . . . ?
Ni2 C38 C39 C40 60.9(5) . . . . ?
C37 C38 C39 Ni2 -60.6(5) . . . . ?
C37 C36 C40 C39 -5.5(8) . . . . ?
Ni2 C36 C40 C39 -62.7(5) . . . . ?
C37 C36 C40 Ni2 57.2(5) . . . . ?
C38 C39 C40 C36 3.2(8) . . . . ?
Ni2 C39 C40 C36 64.2(6) . . . . ?
C38 C39 C40 Ni2 -61.0(5) . . . . ?
N2 C1 N1 C2 0.4(5) . . . . ?
Ni1 C1 N1 C2 178.9(4) . . . . ?
N2 C1 N1 C4 -177.0(4) . . . . ?
Ni1 C1 N1 C4 1.5(8) . . . . ?
C3 C2 N1 C1 -1.1(6) . . . . ?
C3 C2 N1 C4 176.3(5) . . . . ?
C5 C4 N1 C1 85.5(7) . . . . ?
C9 C4 N1 C1 -93.4(6) . . . . ?
C5 C4 N1 C2 -91.6(6) . . . . ?
C9 C4 N1 C2 89.5(7) . . . . ?
N1 C1 N2 C3 0.5(5) . . . . ?
Ni1 C1 N2 C3 -178.4(3) . . . . ?
N1 C1 N2 C13 177.5(4) . . . . ?
Ni1 C1 N2 C13 -1.4(6) . . . . ?
C2 C3 N2 C1 -1.2(6) . . . . ?
C2 C3 N2 C13 -177.9(5) . . . . ?
C14 C13 N2 C1 -3.0(6) . . . . ?
C14 C13 N2 C3 173.5(5) . . . . ?
N5 C21 N4 C22 0.7(6) . . . . ?
Ni2 C21 N4 C22 -179.3(5) . . . . ?
N5 C21 N4 C24 177.4(5) . . . . ?
Ni2 C21 N4 C24 -2.6(9) . . . . ?
C23 C22 N4 C21 -0.4(6) . . . . ?
C23 C22 N4 C24 -177.2(5) . . . . ?
C29 C24 N4 C21 -90.1(6) . . . . ?
C25 C24 N4 C21 92.2(7) . . . . ?
C29 C24 N4 C22 86.1(7) . . . . ?
C25 C24 N4 C22 -91.5(6) . . . . ?
N4 C21 N5 C23 -0.8(6) . . . . ?
Ni2 C21 N5 C23 179.2(4) . . . . ?
N4 C21 N5 C33 179.6(5) . . . . ?
Ni2 C21 N5 C33 -0.4(6) . . . . ?
C22 C23 N5 C21 0.6(7) . . . . ?
C22 C23 N5 C33 -179.9(6) . . . . ?
C34 C33 N5 C21 8.6(7) . . . . ?
C34 C33 N5 C23 -170.9(5) . . . . ?
N2 C1 Ni1 C14 3.9(4) . . . . ?
N1 C1 Ni1 C14 -174.5(6) . . . . ?
N2 C1 Ni1 C18 111.5(10) . . . . ?
N1 C1 Ni1 C18 -66.8(12) . . . . ?
N2 C1 Ni1 C20 173.0(4) . . . . ?
N1 C1 Ni1 C20 -5.4(6) . . . . ?
N2 C1 Ni1 C17 -116.0(6) . . . . ?
N1 C1 Ni1 C17 65.6(8) . . . . ?
N2 C1 Ni1 C19 134.4(4) . . . . ?
N1 C1 Ni1 C19 -44.0(7) . . . . ?
N2 C1 Ni1 C16 -146.3(4) . . . . ?
N1 C1 Ni1 C16 35.3(7) . . . . ?
N5 C21 Ni2 C34 -5.9(4) . . . . ?
N4 C21 Ni2 C34 174.1(6) . . . . ?
N5 C21 Ni2 C40 -167.2(4) . . . . ?
N4 C21 Ni2 C40 12.8(7) . . . . ?
N5 C21 Ni2 C38 118.8(6) . . . . ?
N4 C21 Ni2 C38 -61.2(9) . . . . ?
N5 C21 Ni2 C39 151.4(5) . . . . ?
N4 C21 Ni2 C39 -28.6(7) . . . . ?
N5 C21 Ni2 C36 -132.2(5) . . . . ?
N4 C21 Ni2 C36 47.8(8) . . . . ?

_refine_diff_density_max         1.163
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.104

_shelxl_version_number           2013-4



_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_chemical_properties_physical    Air-sensitive
