# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1856112'
loop_
_audit_author_name
_audit_author_address
'Lingyi Shen'
;Northwest University
China
;
_audit_update_record             
;
2018-07-14 deposited with the CCDC.	2019-03-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H72 Br6 N6 Ni3'
_chemical_formula_weight         1532.82

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'
Br Br -0.2901 2.4595 '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      hexagonal
_space_group_IT_number           176
_space_group_name_H-M_alt        'P 63/m'
_space_group_name_Hall           '-P 6c'

_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, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'-x, -y, -z'
'-x+y, -x, -z-1/2'
'y, -x+y, -z'
'x, y, -z-1/2'
'x-y, x, -z'
'-y, x-y, -z-1/2'

_cell_length_a                   13.198(5)
_cell_length_b                   13.198(5)
_cell_length_c                   23.606(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3561(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5285
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      23.04

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            BLACK
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_F_000             1536
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    4.188
_shelx_estimated_absorpt_T_min   0.421
_shelx_estimated_absorpt_T_max   0.488
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.4208
_exptl_absorpt_correction_T_max  0.4880
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16357
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_av_R_equivalents  0.0969
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.980
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             2136
_reflns_number_gt                1313
_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 SMART APEX II'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0080P)²+45.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2136
_refine_ls_number_parameters     120
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1348
_refine_ls_R_factor_gt           0.0952
_refine_ls_wR_factor_ref         0.1967
_refine_ls_wR_factor_gt          0.1830
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_restrained_S_all      1.144
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.52241(15) 0.21397(16) 0.2500 0.0416(5) Uani 1 2 d S T P . .
Br1 Br 0.6667 0.3333 0.17251(17) 0.1244(13) Uani 1 3 d S T P . .
Br2 Br 0.62682(14) 0.08944(14) 0.2500 0.0565(5) Uani 1 2 d S T P . .
Br3 Br 0.0000 0.0000 0.2500 0.1062(14) Uani 1 6 d S T P . .
N1 N 0.3953(7) 0.1012(7) 0.1945(4) 0.051(2) Uani 1 1 d . . . . .
C1 C 0.3079(9) 0.0151(9) 0.2182(5) 0.052(3) Uani 1 1 d . . . . .
C2 C 0.2093(11) -0.0831(11) 0.1883(6) 0.086(4) Uani 1 1 d . . . . .
H2A H 0.1384 -0.0821 0.1962 0.129 Uiso 1 1 calc R U . . .
H2B H 0.2014 -0.1557 0.2011 0.129 Uiso 1 1 calc R U . . .
H2C H 0.2239 -0.0752 0.1483 0.129 Uiso 1 1 calc R U . . .
C3 C 0.4045(10) 0.1173(11) 0.1339(5) 0.059(3) Uani 1 1 d . . . . .
C4 C 0.4829(14) 0.0921(15) 0.1072(5) 0.099(5) Uani 1 1 d . . . . .
H4 H 0.5215 0.0595 0.1262 0.119 Uiso 1 1 calc R U . . .
C5 C 0.5004(17) 0.1203(16) 0.0466(6) 0.110(6) Uani 1 1 d . . . . .
H5 H 0.5573 0.1116 0.0276 0.132 Uiso 1 1 calc R U . . .
C6 C 0.4409(15) 0.1569(16) 0.0181(6) 0.099(5) Uani 1 1 d . . . . .
C7 C 0.3627(14) 0.1789(14) 0.0465(7) 0.097(5) Uani 1 1 d . . . . .
H7 H 0.3217 0.2070 0.0260 0.117 Uiso 1 1 calc R U . . .
C8 C 0.3415(12) 0.1598(12) 0.1072(6) 0.074(4) Uani 1 1 d . . . . .
C9 C 0.2561(16) 0.1814(16) 0.1331(7) 0.112(6) Uani 1 1 d . . . . .
H9A H 0.2005 0.1129 0.1534 0.168 Uiso 1 1 calc R U . . .
H9B H 0.2163 0.1998 0.1044 0.168 Uiso 1 1 calc R U . . .
H9C H 0.2942 0.2459 0.1590 0.168 Uiso 1 1 calc R U . . .
C10 C 0.4600(18) 0.1850(18) -0.0445(6) 0.150(9) Uani 1 1 d . . . . .
H10A H 0.5147 0.2668 -0.0494 0.226 Uiso 1 1 calc R U . . .
H10B H 0.3869 0.1661 -0.0619 0.226 Uiso 1 1 calc R U . . .
H10C H 0.4903 0.1398 -0.0617 0.226 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 2.062(8) 10_556 ?
Ni1 N1 2.062(8) . ?
Ni1 Br1 2.540(3) . ?
Ni1 Br1 2.540(3) 8_666 ?
Ni1 Br2 2.588(3) 8_666 ?
Ni1 Br2 2.620(3) . ?
Br1 Ni1 2.540(3) 3_655 ?
Br1 Ni1 2.540(3) 8_666 ?
Br2 Ni1 2.588(3) 3_655 ?
N1 C1 1.275(13) . ?
N1 C3 1.441(13) . ?
C1 C2 1.477(14) . ?
C1 C1 1.50(2) 10_556 ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C8 1.369(16) . ?
C3 C4 1.387(17) . ?
C4 C5 1.47(2) . ?
C4 H4 0.9300 . ?
C5 C6 1.30(2) . ?
C5 H5 0.9300 . ?
C6 C7 1.38(2) . ?
C6 C10 1.51(2) . ?
C7 C8 1.458(19) . ?
C7 H7 0.9300 . ?
C8 C9 1.431(19) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?

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 79.0(5) 10_556 . ?
N1 Ni1 Br1 173.0(3) 10_556 . ?
N1 Ni1 Br1 94.4(3) . . ?
N1 Ni1 Br1 94.4(3) 10_556 8_666 ?
N1 Ni1 Br1 173.0(3) . 8_666 ?
Br1 Ni1 Br1 92.12(14) . 8_666 ?
N1 Ni1 Br2 96.8(2) 10_556 8_666 ?
N1 Ni1 Br2 96.8(2) . 8_666 ?
Br1 Ni1 Br2 86.26(6) . 8_666 ?
Br1 Ni1 Br2 86.26(6) 8_666 8_666 ?
N1 Ni1 Br2 92.3(2) 10_556 . ?
N1 Ni1 Br2 92.3(2) . . ?
Br1 Ni1 Br2 85.57(5) . . ?
Br1 Ni1 Br2 85.57(5) 8_666 . ?
Br2 Ni1 Br2 168.22(8) 8_666 . ?
Ni1 Br1 Ni1 73.87(11) 3_655 . ?
Ni1 Br1 Ni1 73.87(11) 3_655 8_666 ?
Ni1 Br1 Ni1 73.87(11) . 8_666 ?
Ni1 Br2 Ni1 71.78(8) 3_655 . ?
C1 N1 C3 122.6(9) . . ?
C1 N1 Ni1 114.3(7) . . ?
C3 N1 Ni1 123.1(7) . . ?
N1 C1 C2 125.5(10) . . ?
N1 C1 C1 116.0(6) . 10_556 ?
C2 C1 C1 118.5(7) . 10_556 ?
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 . . ?
C8 C3 C4 124.6(11) . . ?
C8 C3 N1 119.6(11) . . ?
C4 C3 N1 115.8(11) . . ?
C3 C4 C5 115.2(14) . . ?
C3 C4 H4 122.4 . . ?
C5 C4 H4 122.4 . . ?
C6 C5 C4 123.5(16) . . ?
C6 C5 H5 118.2 . . ?
C4 C5 H5 118.2 . . ?
C5 C6 C7 118.9(15) . . ?
C5 C6 C10 122.7(18) . . ?
C7 C6 C10 118.3(18) . . ?
C6 C7 C8 122.7(15) . . ?
C6 C7 H7 118.6 . . ?
C8 C7 H7 118.6 . . ?
C3 C8 C9 125.8(13) . . ?
C3 C8 C7 114.9(13) . . ?
C9 C8 C7 119.3(14) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C10 H10A 109.5 . . ?
C6 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C6 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 N1 C1 C2 4.3(18) . . . . ?
Ni1 N1 C1 C2 -175.1(10) . . . . ?
C3 N1 C1 C1 -176.2(8) . . . 10_556 ?
Ni1 N1 C1 C1 4.4(8) . . . 10_556 ?
C1 N1 C3 C8 77.2(15) . . . . ?
Ni1 N1 C3 C8 -103.5(12) . . . . ?
C1 N1 C3 C4 -105.5(14) . . . . ?
Ni1 N1 C3 C4 73.9(14) . . . . ?
C8 C3 C4 C5 3(2) . . . . ?
N1 C3 C4 C5 -173.9(13) . . . . ?
C3 C4 C5 C6 -6(3) . . . . ?
C4 C5 C6 C7 5(3) . . . . ?
C4 C5 C6 C10 -179.6(16) . . . . ?
C5 C6 C7 C8 -2(3) . . . . ?
C10 C6 C7 C8 -177.3(14) . . . . ?
C4 C3 C8 C9 176.9(15) . . . . ?
N1 C3 C8 C9 -6(2) . . . . ?
C4 C3 C8 C7 0(2) . . . . ?
N1 C3 C8 C7 176.6(11) . . . . ?
C6 C7 C8 C3 -1(2) . . . . ?
C6 C7 C8 C9 -178.1(16) . . . . ?

_refine_diff_density_max         2.154
_refine_diff_density_min         -2.704
_refine_diff_density_rms         0.162

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 120 37 ' '
2 0.000 0.000 0.500 120 37 ' '
3 0.333 0.667 0.250 209 58 ' '
4 0.667 0.333 0.750 209 58 ' '
_platon_squeeze_details          
;
;
####################################################################### 
# 
# 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_4a
_database_code_depnum_ccdc_archive 'CCDC 1856114'
loop_
_audit_author_name
_audit_author_address
'Lingyi Shen'
;Northwest University
China
;
_audit_update_record             
;
2018-07-14 deposited with the CCDC.	2019-03-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H29 O6'
_chemical_formula_weight         521.56

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C c'
_space_group_name_Hall           'C -2yc'

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

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

_cell_length_a                   22.007(7)
_cell_length_b                   12.847(7)
_cell_length_c                   11.149(5)
_cell_angle_alpha                90
_cell_angle_beta                 112.394(8)
_cell_angle_gamma                90
_cell_volume                     2914(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    3426
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      21.74

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_F_000             1100
_exptl_transmission_factor_min   0.4536
_exptl_transmission_factor_max   0.7452
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.081
_shelx_estimated_absorpt_T_min   0.980
_shelx_estimated_absorpt_T_max   0.984
_exptl_absorpt_correction_T_min  0.4536
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean 'fine-focus sealed tube'
_diffrn_reflns_number            9581
_diffrn_reflns_av_unetI/netI     0.0674
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.875
_diffrn_reflns_theta_max         25.700
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_point_group_measured_fraction_full 0.885
_reflns_number_total             4614
_reflns_number_gt                3158
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.763
_reflns_Friedel_fraction_max     0.760
_reflns_Friedel_fraction_full    0.773

_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 SMART APEX II'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0200P)²+2.0402P] 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_abs_structure_details 
;
 Flack x determined using 1033 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.8(10)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4614
_refine_ls_number_parameters     358
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0620
_refine_ls_wR_factor_ref         0.1446
_refine_ls_wR_factor_gt          0.1312
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_restrained_S_all      1.127
_refine_ls_shift/su_max          0.004
_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 0.9939(2) 0.0544(4) 0.1370(5) 0.0474(12) Uani 1 1 d . . . A 1
C2 C 0.9321(2) 0.0827(4) 0.1328(5) 0.0494(12) Uani 1 1 d . . . A 1
C3 C 0.9150(2) 0.1873(4) 0.1363(6) 0.0529(14) Uani 1 1 d . . . A 1
C4 C 0.9607(2) 0.2645(4) 0.1424(6) 0.0524(14) Uani 1 1 d . . . A 1
C5 C 1.0229(3) 0.2387(4) 0.1451(5) 0.0496(13) Uani 1 1 d . . . A 1
C6 C 1.0401(2) 0.1337(4) 0.1448(5) 0.0463(12) Uani 1 1 d . . . A 1
C7 C 1.0119(2) -0.0570(4) 0.1272(6) 0.0501(13) Uani 1 1 d . . . A 1
C8 C 1.0068(4) -0.0976(5) 0.0104(7) 0.084(2) Uani 1 1 d . . . A 1
H8 H 0.9914 -0.0548 -0.0647 0.101 Uiso 1 1 calc R U . A 1
C9 C 1.0237(4) -0.2000(6) -0.0008(9) 0.105(3) Uani 1 1 d . . . A 1
H9 H 1.0208 -0.2263 -0.0824 0.126 Uiso 1 1 calc R U . A 1
C10 C 1.0446(3) -0.2629(5) 0.1058(10) 0.086(2) Uani 1 1 d . . . A 1
H10 H 1.0547 -0.3339 0.0982 0.104 Uiso 1 1 calc R U . A 1
C11 C 1.0507(4) -0.2240(6) 0.2219(9) 0.096(2) Uani 1 1 d . . . A 1
H11 H 1.0661 -0.2672 0.2966 0.116 Uiso 1 1 calc R U . A 1
C12 C 1.0347(4) -0.1208(5) 0.2328(7) 0.083(2) Uani 1 1 d . . . A 1
H12 H 1.0397 -0.0942 0.3155 0.100 Uiso 1 1 calc R U . A 1
C13 C 0.8821(3) -0.0013(4) 0.1169(7) 0.0612(16) Uani 1 1 d . . . A 1
C14 C 0.8482(4) -0.1357(6) 0.2261(13) 0.143(5) Uani 1 1 d . . . A 1
H14A H 0.8259 -0.1193 0.2861 0.171 Uiso 1 1 calc R U . A 1
H14B H 0.8141 -0.1434 0.1378 0.171 Uiso 1 1 calc R U . A 1
C15 C 0.8826(6) -0.2276(7) 0.2633(13) 0.151(5) Uani 1 1 d . . . A 1
H15A H 0.8947 -0.2533 0.1927 0.227 Uiso 1 1 calc R U . A 1
H15B H 0.8550 -0.2794 0.2830 0.227 Uiso 1 1 calc R U . A 1
H15C H 0.9224 -0.2156 0.3406 0.227 Uiso 1 1 calc R U . A 1
C16 C 0.8483(3) 0.2145(4) 0.1426(6) 0.0560(15) Uani 1 1 d . . . A 1
C17 C 0.8339(3) 0.1807(4) 0.2459(7) 0.0644(16) Uani 1 1 d . . . A 1
H17 H 0.8649 0.1396 0.3120 0.077 Uiso 1 1 calc R U . A 1
C18 C 0.7748(3) 0.2060(5) 0.2539(8) 0.079(2) Uani 1 1 d . . . A 1
H18 H 0.7654 0.1828 0.3260 0.095 Uiso 1 1 calc R U . A 1
C19 C 0.7296(3) 0.2639(6) 0.1599(10) 0.090(2) Uani 1 1 d . . . A 1
H19 H 0.6887 0.2801 0.1658 0.108 Uiso 1 1 calc R U . A 1
C20 C 0.7430(3) 0.2983(6) 0.0577(9) 0.090(2) Uani 1 1 d . . . A 1
H20 H 0.7116 0.3398 -0.0073 0.107 Uiso 1 1 calc R U . A 1
C21 C 0.8031(3) 0.2732(5) 0.0469(7) 0.0722(17) Uani 1 1 d . . . A 1
H21 H 0.8122 0.2965 -0.0254 0.087 Uiso 1 1 calc R U . A 1
C22 C 0.9453(3) 0.3792(4) 0.1516(9) 0.0685(18) Uani 1 1 d . . . A 1
C23 C 0.9004(6) 0.5333(6) 0.0383(14) 0.156(5) Uani 1 1 d . . . A 1
C24 C 0.8619(10) 0.5625(17) -0.067(2) 0.118(4) Uani 0.5 1 d . U P A 1
C25 C 1.0719(3) 0.3237(4) 0.1483(6) 0.0578(15) Uani 1 1 d . . . A 1
C26 C 1.0613(3) 0.3822(5) 0.0370(8) 0.0784(19) Uani 1 1 d . . . A 1
H26 H 1.0233 0.3707 -0.0393 0.094 Uiso 1 1 calc R U . A 1
C27 C 1.1068(5) 0.4574(6) 0.0389(12) 0.109(3) Uani 1 1 d . . . A 1
H27 H 1.0995 0.4976 -0.0369 0.130 Uiso 1 1 calc R U . A 1
C28 C 1.1605(5) 0.4745(6) 0.1443(14) 0.120(4) Uani 1 1 d . . . A 1
H28 H 1.1912 0.5261 0.1430 0.144 Uiso 1 1 calc R U . A 1
C29 C 1.1717(4) 0.4176(7) 0.2556(12) 0.116(3) Uani 1 1 d . . . A 1
H29 H 1.2103 0.4301 0.3305 0.139 Uiso 1 1 calc R U . A 1
C30 C 1.1266(3) 0.3410(5) 0.2595(8) 0.085(2) Uani 1 1 d . . . A 1
H30 H 1.1337 0.3024 0.3364 0.102 Uiso 1 1 calc R U . A 1
C31 C 1.1084(3) 0.1029(4) 0.1607(7) 0.0581(14) Uani 1 1 d . . . A 1
C32 C 1.1847(5) 0.0907(9) 0.0614(12) 0.149(4) Uani 1 1 d D . . A 1
H32A H 1.2118 0.0670 0.1503 0.178 Uiso 1 1 calc R U . A 1
H32B H 1.1825 0.0333 0.0005 0.178 Uiso 1 1 calc R U . A 1
C33 C 1.2136(6) 0.1764(11) 0.031(2) 0.249(11) Uani 1 1 d D . . A 1
H33A H 1.2427 0.1539 -0.0119 0.374 Uiso 1 1 calc R U . A 1
H33B H 1.2391 0.2143 0.1107 0.374 Uiso 1 1 calc R U . A 1
H33C H 1.1794 0.2222 -0.0272 0.374 Uiso 1 1 calc R U . A 1
C24A C 0.8319(10) 0.5355(16) -0.119(2) 0.118(4) Uani 0.5 1 d . U P A 2
O1 O 0.8376(3) -0.0190(4) 0.0158(6) 0.0977(16) Uani 1 1 d . . . A 1
O2 O 0.8927(2) -0.0501(3) 0.2274(5) 0.0835(14) Uani 1 1 d . . . A 1
O3 O 0.9597(3) 0.4234(3) 0.2521(6) 0.1061(18) Uani 1 1 d . . . A 1
O4 O 0.9153(2) 0.4196(3) 0.0363(6) 0.0904(15) Uani 1 1 d . . . A 1
O5 O 1.1496(2) 0.0720(4) 0.2602(5) 0.0919(15) Uani 1 1 d . . . A 1
O6 O 1.1188(2) 0.1157(4) 0.0533(5) 0.0890(14) Uani 1 1 d . . . A 1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.391(7) . ?
C1 C6 1.418(7) . ?
C1 C7 1.500(7) . ?
C2 C3 1.400(7) . ?
C2 C13 1.504(7) . ?
C3 C4 1.396(7) . ?
C3 C16 1.535(7) . ?
C4 C5 1.397(7) . ?
C4 C22 1.525(8) . ?
C5 C6 1.401(7) . ?
C5 C25 1.527(7) . ?
C6 C31 1.497(7) . ?
C7 C12 1.364(8) . ?
C7 C8 1.368(9) . ?
C8 C9 1.385(9) . ?
C8 H8 0.9500 . ?
C9 C10 1.365(11) . ?
C9 H9 0.9500 . ?
C10 C11 1.345(11) . ?
C10 H10 0.9500 . ?
C11 C12 1.389(10) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 O1 1.200(8) . ?
C13 O2 1.321(8) . ?
C14 C15 1.379(12) . ?
C14 O2 1.468(8) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C21 1.374(8) . ?
C16 C17 1.377(9) . ?
C17 C18 1.377(8) . ?
C17 H17 0.9500 . ?
C18 C19 1.358(11) . ?
C18 H18 0.9500 . ?
C19 C20 1.356(12) . ?
C19 H19 0.9500 . ?
C20 C21 1.410(9) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 O3 1.186(9) . ?
C22 O4 1.308(9) . ?
C23 C24 1.21(2) . ?
C23 O4 1.500(8) . ?
C24 C24A 0.78(3) . ?
C25 C30 1.377(9) . ?
C25 C26 1.392(9) . ?
C26 C27 1.387(10) . ?
C26 H26 0.9500 . ?
C27 C28 1.329(14) . ?
C27 H27 0.9500 . ?
C28 C29 1.379(14) . ?
C28 H28 0.9500 . ?
C29 C30 1.410(11) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 O5 1.202(7) . ?
C31 O6 1.312(7) . ?
C32 C33 1.376(13) . ?
C32 O6 1.456(9) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 118.9(4) . . ?
C2 C1 C7 121.9(4) . . ?
C6 C1 C7 119.2(4) . . ?
C1 C2 C3 121.4(4) . . ?
C1 C2 C13 118.6(4) . . ?
C3 C2 C13 119.9(4) . . ?
C4 C3 C2 119.1(4) . . ?
C4 C3 C16 121.3(4) . . ?
C2 C3 C16 119.5(4) . . ?
C3 C4 C5 121.0(4) . . ?
C3 C4 C22 121.1(5) . . ?
C5 C4 C22 117.9(4) . . ?
C4 C5 C6 119.5(4) . . ?
C4 C5 C25 120.6(4) . . ?
C6 C5 C25 120.0(5) . . ?
C5 C6 C1 120.2(4) . . ?
C5 C6 C31 120.9(4) . . ?
C1 C6 C31 118.7(4) . . ?
C12 C7 C8 117.5(5) . . ?
C12 C7 C1 122.1(5) . . ?
C8 C7 C1 120.4(5) . . ?
C7 C8 C9 121.4(7) . . ?
C7 C8 H8 119.3 . . ?
C9 C8 H8 119.3 . . ?
C10 C9 C8 119.8(7) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C11 C10 C9 119.6(6) . . ?
C11 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
C10 C11 C12 120.3(7) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C7 C12 C11 121.3(7) . . ?
C7 C12 H12 119.3 . . ?
C11 C12 H12 119.3 . . ?
O1 C13 O2 125.2(6) . . ?
O1 C13 C2 123.0(7) . . ?
O2 C13 C2 111.7(5) . . ?
C15 C14 O2 110.6(7) . . ?
C15 C14 H14A 109.5 . . ?
O2 C14 H14A 109.5 . . ?
C15 C14 H14B 109.5 . . ?
O2 C14 H14B 109.5 . . ?
H14A C14 H14B 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 . . ?
C21 C16 C17 119.6(6) . . ?
C21 C16 C3 120.8(6) . . ?
C17 C16 C3 119.6(5) . . ?
C18 C17 C16 120.3(6) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
C19 C18 C17 120.7(7) . . ?
C19 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
C20 C19 C18 119.9(7) . . ?
C20 C19 H19 120.1 . . ?
C18 C19 H19 120.1 . . ?
C19 C20 C21 120.5(7) . . ?
C19 C20 H20 119.7 . . ?
C21 C20 H20 119.7 . . ?
C16 C21 C20 119.0(7) . . ?
C16 C21 H21 120.5 . . ?
C20 C21 H21 120.5 . . ?
O3 C22 O4 126.3(6) . . ?
O3 C22 C4 122.6(7) . . ?
O4 C22 C4 111.1(6) . . ?
C24 C23 O4 111.3(15) . . ?
C30 C25 C26 120.5(6) . . ?
C30 C25 C5 120.2(6) . . ?
C26 C25 C5 119.2(6) . . ?
C27 C26 C25 119.2(8) . . ?
C27 C26 H26 120.4 . . ?
C25 C26 H26 120.4 . . ?
C28 C27 C26 121.5(9) . . ?
C28 C27 H27 119.3 . . ?
C26 C27 H27 119.3 . . ?
C27 C28 C29 120.1(8) . . ?
C27 C28 H28 119.9 . . ?
C29 C28 H28 119.9 . . ?
C28 C29 C30 120.7(8) . . ?
C28 C29 H29 119.6 . . ?
C30 C29 H29 119.6 . . ?
C25 C30 C29 117.9(8) . . ?
C25 C30 H30 121.0 . . ?
C29 C30 H30 121.0 . . ?
O5 C31 O6 123.4(6) . . ?
O5 C31 C6 124.6(6) . . ?
O6 C31 C6 112.0(5) . . ?
C33 C32 O6 110.5(8) . . ?
C33 C32 H32A 109.5 . . ?
O6 C32 H32A 109.5 . . ?
C33 C32 H32B 109.5 . . ?
O6 C32 H32B 109.5 . . ?
H32A C32 H32B 108.1 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C13 O2 C14 117.8(6) . . ?
C22 O4 C23 113.7(7) . . ?
C31 O6 C32 115.7(6) . . ?

_refine_diff_density_max         0.222
_refine_diff_density_min         -0.168
_refine_diff_density_rms         0.039

####################################################################### 
# 
# 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 1856113'
loop_
_audit_author_name
_audit_author_address
'Lingyi Shen'
;Northwest University
China
;
_audit_update_record             
;
2018-07-14 deposited with the CCDC.	2019-03-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H72 N6 Ni3'
_chemical_formula_weight         1053.36

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/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   13.1720(18)
_cell_length_b                   20.129(3)
_cell_length_c                   21.285(3)
_cell_angle_alpha                90
_cell_angle_beta                 103.793(2)
_cell_angle_gamma                90
_cell_volume                     5480.9(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9903
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      25.20

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_F_000             2232
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.063
_shelx_estimated_absorpt_T_min   0.741
_shelx_estimated_absorpt_T_max   0.816
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7410
_exptl_absorpt_correction_T_max  0.8156
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus 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            34680
_diffrn_reflns_av_unetI/netI     0.0625
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.660
_diffrn_reflns_theta_max         25.197
_diffrn_reflns_theta_full        25.197
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             9824
_reflns_number_gt                7050
_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 SMART APEX II'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0746P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9824
_refine_ls_number_parameters     640
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0419
_refine_ls_wR_factor_ref         0.1279
_refine_ls_wR_factor_gt          0.1092
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.41343(3) 0.87606(2) 0.19291(2) 0.03303(12) Uani 1 1 d . . . . .
Ni3 Ni 0.53054(3) 0.76245(2) 0.21334(2) 0.03359(12) Uani 1 1 d . . . . .
Ni2 Ni 0.45277(3) 0.81569(2) 0.31046(2) 0.03376(12) Uani 1 1 d . . . . .
C5 C 0.2262(3) 0.83854(17) 0.09447(16) 0.0432(8) Uani 1 1 d . . . . .
C10 C 0.1780(3) 0.89728(19) 0.06594(19) 0.0526(9) Uani 1 1 d . . . . .
C6 C 0.1623(3) 0.7866(2) 0.10478(19) 0.0566(10) Uani 1 1 d . . . . .
H6 H 0.1929 0.7472 0.1229 0.068 Uiso 1 1 calc R U . . .
C8 C 0.0074(3) 0.8493(2) 0.0620(2) 0.0642(12) Uani 1 1 d . . . . .
C9 C 0.0697(3) 0.9000(2) 0.0509(2) 0.0671(12) Uani 1 1 d . . . . .
H9 H 0.0376 0.9387 0.0321 0.080 Uiso 1 1 calc R U . . .
C7 C 0.0558(3) 0.7919(2) 0.0889(2) 0.0667(12) Uani 1 1 d . . . . .
H7 H 0.0154 0.7562 0.0964 0.080 Uiso 1 1 calc R U . . .
C2 C 0.5036(3) 0.78909(16) 0.12095(15) 0.0379(7) Uani 1 1 d . . . . .
C1 C 0.3917(3) 0.79085(16) 0.09300(16) 0.0390(8) Uani 1 1 d . . . . .
C53 C 0.6825(2) 0.79432(16) 0.34131(15) 0.0357(7) Uani 1 1 d . . . . .
C55 C 0.8041(3) 0.88167(19) 0.3871(2) 0.0602(11) Uani 1 1 d . . . . .
H55 H 0.8150 0.9255 0.4008 0.072 Uiso 1 1 calc R U . . .
C54 C 0.7029(3) 0.85890(18) 0.36263(19) 0.0492(9) Uani 1 1 d . . . . .
H54 H 0.6472 0.8879 0.3605 0.059 Uiso 1 1 calc R U . . .
C56 C 0.8891(3) 0.83993(19) 0.3915(2) 0.0519(9) Uani 1 1 d . . . . .
C58 C 0.7676(3) 0.75090(17) 0.34724(18) 0.0439(8) Uani 1 1 d . . . . .
C57 C 0.8682(3) 0.77562(18) 0.37171(19) 0.0493(9) Uani 1 1 d . . . . .
H57 H 0.9243 0.7467 0.3748 0.059 Uiso 1 1 calc R U . . .
C60 C 0.9990(3) 0.8649(2) 0.4175(3) 0.0823(15) Uani 1 1 d . . . . .
H60A H 1.0441 0.8282 0.4339 0.123 Uiso 1 1 calc R U . . .
H60B H 0.9999 0.8962 0.4516 0.123 Uiso 1 1 calc R U . . .
H60C H 1.0231 0.8862 0.3834 0.123 Uiso 1 1 calc R U . . .
C38 C 0.2463(3) 0.76471(17) 0.39089(18) 0.0445(9) Uani 1 1 d . . . . .
C33 C 0.2428(3) 0.77320(17) 0.32491(17) 0.0409(8) Uani 1 1 d . . . . .
C37 C 0.1876(3) 0.71298(19) 0.4081(2) 0.0530(10) Uani 1 1 d . . . . .
H37 H 0.1899 0.7068 0.4517 0.064 Uiso 1 1 calc R U . . .
C35 C 0.1228(3) 0.6803(2) 0.2991(2) 0.0573(10) Uani 1 1 d . . . . .
H35 H 0.0810 0.6532 0.2680 0.069 Uiso 1 1 calc R U . . .
C34 C 0.1813(3) 0.73077(18) 0.2803(2) 0.0506(9) Uani 1 1 d . . . . .
H34 H 0.1792 0.7362 0.2367 0.061 Uiso 1 1 calc R U . . .
C36 C 0.1265(3) 0.67061(19) 0.3637(2) 0.0530(10) Uani 1 1 d . . . . .
N2 N 0.5389(2) 0.84041(13) 0.16694(13) 0.0346(6) Uani 1 1 d . . . . .
N1 N 0.3365(2) 0.83467(13) 0.11547(13) 0.0397(7) Uani 1 1 d . . . . .
C3 C 0.3456(3) 0.74364(19) 0.03835(19) 0.0571(10) Uani 1 1 d . . . . .
H3A H 0.2711 0.7492 0.0260 0.086 Uiso 1 1 calc R U . . .
H3B H 0.3619 0.6987 0.0524 0.086 Uiso 1 1 calc R U . . .
H3C H 0.3746 0.7530 0.0020 0.086 Uiso 1 1 calc R U . . .
C45 C 0.4236(3) 0.63397(16) 0.18732(18) 0.0433(8) Uani 1 1 d . . . . .
C50 C 0.4831(3) 0.59679(18) 0.1534(2) 0.0552(10) Uani 1 1 d . . . . .
C46 C 0.3161(3) 0.62901(18) 0.1696(2) 0.0539(10) Uani 1 1 d . . . . .
H46 H 0.2760 0.6524 0.1927 0.065 Uiso 1 1 calc R U . . .
C22 C 0.3327(2) 0.91993(15) 0.24883(15) 0.0362(7) Uani 1 1 d . . . . .
C21 C 0.2631(3) 0.87347(16) 0.26912(16) 0.0371(7) Uani 1 1 d . . . . .
N3 N 0.3067(2) 0.82340(13) 0.30543(13) 0.0374(6) Uani 1 1 d . . . . .
N4 N 0.44145(19) 0.90899(12) 0.27770(13) 0.0335(6) Uani 1 1 d . . . . .
C24 C 0.1475(3) 0.88591(19) 0.2504(2) 0.0553(10) Uani 1 1 d . . . . .
H24A H 0.1124 0.8530 0.2700 0.083 Uiso 1 1 calc R U . . .
H24B H 0.1232 0.8835 0.2042 0.083 Uiso 1 1 calc R U . . .
H24C H 0.1330 0.9293 0.2649 0.083 Uiso 1 1 calc R U . . .
C23 C 0.2933(3) 0.98965(17) 0.22943(17) 0.0485(9) Uani 1 1 d . . . . .
H23A H 0.2809 1.0125 0.2665 0.073 Uiso 1 1 calc R U . . .
H23B H 0.2294 0.9872 0.1965 0.073 Uiso 1 1 calc R U . . .
H23C H 0.3448 1.0134 0.2131 0.073 Uiso 1 1 calc R U . . .
C13 C 0.6322(3) 0.87639(15) 0.16504(16) 0.0372(8) Uani 1 1 d . . . . .
C14 C 0.7273(3) 0.86310(19) 0.20703(19) 0.0510(9) Uani 1 1 d . . . . .
H14 H 0.7325 0.8274 0.2354 0.061 Uiso 1 1 calc R U . . .
C18 C 0.6276(3) 0.92886(18) 0.12137(18) 0.0495(9) Uani 1 1 d . . . . .
C17 C 0.7177(3) 0.96612(19) 0.1240(2) 0.0580(11) Uani 1 1 d . . . . .
H17 H 0.7143 1.0011 0.0950 0.070 Uiso 1 1 calc R U . . .
C16 C 0.8107(3) 0.9540(2) 0.1670(2) 0.0611(11) Uani 1 1 d . . . . .
C15 C 0.8148(3) 0.9009(2) 0.2083(2) 0.0644(11) Uani 1 1 d . . . . .
H15 H 0.8774 0.8905 0.2374 0.077 Uiso 1 1 calc R U . . .
C20 C 0.9062(4) 0.9970(2) 0.1672(3) 0.0877(16) Uani 1 1 d . . . . .
H20A H 0.9518 0.9971 0.2098 0.132 Uiso 1 1 calc R U . . .
H20B H 0.8841 1.0416 0.1551 0.132 Uiso 1 1 calc R U . . .
H20C H 0.9427 0.9794 0.1369 0.132 Uiso 1 1 calc R U . . .
C11 C 0.2401(4) 0.9536(2) 0.0515(2) 0.0822(14) Uani 1 1 d . . . . .
H11A H 0.1940 0.9875 0.0292 0.123 Uiso 1 1 calc R U . . .
H11B H 0.2848 0.9387 0.0247 0.123 Uiso 1 1 calc R U . . .
H11C H 0.2819 0.9714 0.0911 0.123 Uiso 1 1 calc R U . . .
C12 C -0.1116(3) 0.8551(3) 0.0429(3) 0.104(2) Uani 1 1 d . . . . .
H12A H -0.1317 0.8999 0.0494 0.155 Uiso 1 1 calc R U . . .
H12B H -0.1414 0.8256 0.0691 0.155 Uiso 1 1 calc R U . . .
H12C H -0.1366 0.8433 -0.0018 0.155 Uiso 1 1 calc R U . . .
C4 C 0.5760(3) 0.76217(18) 0.08136(19) 0.0527(10) Uani 1 1 d . . . . .
H4A H 0.5717 0.7897 0.0440 0.079 Uiso 1 1 calc R U . . .
H4B H 0.5557 0.7176 0.0678 0.079 Uiso 1 1 calc R U . . .
H4C H 0.6466 0.7621 0.1072 0.079 Uiso 1 1 calc R U . . .
C49 C 0.4307(4) 0.55733(19) 0.1021(2) 0.0685(12) Uani 1 1 d . . . . .
H49 H 0.4704 0.5325 0.0799 0.082 Uiso 1 1 calc R U . . .
C47 C 0.2671(4) 0.5893(2) 0.1177(2) 0.0680(12) Uani 1 1 d . . . . .
H47 H 0.1945 0.5872 0.1064 0.082 Uiso 1 1 calc R U . . .
C48 C 0.3232(4) 0.5530(2) 0.0825(2) 0.0681(12) Uani 1 1 d . . . . .
C51 C 0.6012(3) 0.5977(2) 0.1718(2) 0.0749(13) Uani 1 1 d . . . . .
H51A H 0.6253 0.6429 0.1753 0.112 Uiso 1 1 calc R U . . .
H51B H 0.6275 0.5752 0.1392 0.112 Uiso 1 1 calc R U . . .
H51C H 0.6258 0.5757 0.2126 0.112 Uiso 1 1 calc R U . . .
C52 C 0.2705(5) 0.5107(3) 0.0252(3) 0.1024(19) Uani 1 1 d . . . . .
H52A H 0.2474 0.4698 0.0404 0.154 Uiso 1 1 calc R U . . .
H52B H 0.3192 0.5014 -0.0008 0.154 Uiso 1 1 calc R U . . .
H52C H 0.2114 0.5342 -0.0003 0.154 Uiso 1 1 calc R U . . .
C19 C 0.5265(3) 0.9442(2) 0.0740(2) 0.0727(13) Uani 1 1 d . . . . .
H19A H 0.5102 0.9092 0.0426 0.109 Uiso 1 1 calc R U . . .
H19B H 0.5330 0.9854 0.0526 0.109 Uiso 1 1 calc R U . . .
H19C H 0.4717 0.9479 0.0965 0.109 Uiso 1 1 calc R U . . .
C25 C 0.5025(2) 0.96720(15) 0.30078(16) 0.0369(7) Uani 1 1 d . . . . .
C26 C 0.5615(3) 0.99881(17) 0.26461(18) 0.0473(9) Uani 1 1 d . . . . .
H26 H 0.5664 0.9805 0.2253 0.057 Uiso 1 1 calc R U . . .
C30 C 0.5005(3) 0.99327(18) 0.36107(18) 0.0480(9) Uani 1 1 d . . . . .
C29 C 0.5531(3) 1.0531(2) 0.3806(2) 0.0594(11) Uani 1 1 d . . . . .
H29 H 0.5503 1.0710 0.4205 0.071 Uiso 1 1 calc R U . . .
C28 C 0.6083(3) 1.08628(19) 0.3434(2) 0.0610(11) Uani 1 1 d . . . . .
C27 C 0.6139(3) 1.05772(19) 0.2855(2) 0.0584(11) Uani 1 1 d . . . . .
H27 H 0.6533 1.0781 0.2601 0.070 Uiso 1 1 calc R U . . .
N6 N 0.58008(19) 0.77414(12) 0.30859(13) 0.0331(6) Uani 1 1 d . . . . .
N5 N 0.4766(2) 0.67929(12) 0.23549(14) 0.0376(6) Uani 1 1 d . . . . .
C41 C 0.4687(2) 0.67772(16) 0.29610(17) 0.0390(8) Uani 1 1 d . . . . .
C42 C 0.5222(3) 0.72966(15) 0.33878(17) 0.0378(8) Uani 1 1 d . . . . .
C44 C 0.4088(3) 0.62493(16) 0.3225(2) 0.0496(9) Uani 1 1 d . . . . .
H44A H 0.3482 0.6444 0.3327 0.074 Uiso 1 1 calc R U . . .
H44B H 0.4526 0.6060 0.3608 0.074 Uiso 1 1 calc R U . . .
H44C H 0.3873 0.5908 0.2906 0.074 Uiso 1 1 calc R U . . .
C43 C 0.5529(3) 0.7176(2) 0.41049(18) 0.0533(10) Uani 1 1 d . . . . .
H43A H 0.6006 0.6808 0.4195 0.080 Uiso 1 1 calc R U . . .
H43B H 0.4917 0.7077 0.4258 0.080 Uiso 1 1 calc R U . . .
H43C H 0.5861 0.7566 0.4319 0.080 Uiso 1 1 calc R U . . .
C39 C 0.3105(4) 0.8102(2) 0.4406(2) 0.0713(13) Uani 1 1 d . . . . .
H39A H 0.3804 0.8124 0.4347 0.107 Uiso 1 1 calc R U . . .
H39B H 0.3120 0.7935 0.4831 0.107 Uiso 1 1 calc R U . . .
H39C H 0.2801 0.8538 0.4359 0.107 Uiso 1 1 calc R U . . .
C31 C 0.4445(4) 0.9581(2) 0.4039(2) 0.0726(13) Uani 1 1 d . . . . .
H31A H 0.3718 0.9545 0.3827 0.109 Uiso 1 1 calc R U . . .
H31B H 0.4520 0.9825 0.4435 0.109 Uiso 1 1 calc R U . . .
H31C H 0.4736 0.9144 0.4133 0.109 Uiso 1 1 calc R U . . .
C32 C 0.6597(4) 1.1523(2) 0.3655(3) 0.0991(19) Uani 1 1 d . . . . .
H32A H 0.6101 1.1811 0.3782 0.149 Uiso 1 1 calc R U . . .
H32B H 0.6834 1.1724 0.3306 0.149 Uiso 1 1 calc R U . . .
H32C H 0.7182 1.1453 0.4016 0.149 Uiso 1 1 calc R U . . .
C40 C 0.0674(4) 0.6153(2) 0.3870(3) 0.0791(14) Uani 1 1 d . . . . .
H40A H 0.1153 0.5808 0.4060 0.119 Uiso 1 1 calc R U . . .
H40B H 0.0161 0.5976 0.3511 0.119 Uiso 1 1 calc R U . . .
H40C H 0.0332 0.6323 0.4187 0.119 Uiso 1 1 calc R U . . .
C59 C 0.7525(3) 0.6806(2) 0.3255(3) 0.0786(15) Uani 1 1 d . . . . .
H59A H 0.8193 0.6599 0.3293 0.118 Uiso 1 1 calc R U . . .
H59B H 0.7137 0.6792 0.2812 0.118 Uiso 1 1 calc R U . . .
H59C H 0.7146 0.6572 0.3520 0.118 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 1.908(3) . ?
Ni1 C22 1.983(3) . ?
Ni1 N2 1.996(3) . ?
Ni3 N5 1.920(3) . ?
Ni3 C2 1.987(3) . ?
Ni3 N6 1.990(3) . ?
Ni2 N3 1.908(3) . ?
Ni2 C42 1.984(3) . ?
Ni2 N4 1.997(3) . ?
C5 C6 1.392(5) . ?
C5 C10 1.409(5) . ?
C5 N1 1.416(4) . ?
C10 C9 1.387(6) . ?
C10 C11 1.473(6) . ?
C6 C7 1.368(5) . ?
C8 C9 1.365(6) . ?
C8 C7 1.377(6) . ?
C8 C12 1.528(6) . ?
C2 N2 1.423(4) . ?
C2 C1 1.452(5) . ?
C2 C4 1.516(5) . ?
C1 N1 1.305(4) . ?
C1 C3 1.513(5) . ?
C53 C54 1.382(5) . ?
C53 C58 1.403(4) . ?
C53 N6 1.422(4) . ?
C55 C56 1.385(5) . ?
C55 C54 1.389(5) . ?
C56 C57 1.369(5) . ?
C56 C60 1.508(5) . ?
C58 C57 1.395(5) . ?
C58 C59 1.488(5) . ?
C38 C37 1.396(5) . ?
C38 C33 1.405(5) . ?
C38 C39 1.499(5) . ?
C33 C34 1.385(5) . ?
C33 N3 1.438(4) . ?
C37 C36 1.380(6) . ?
C35 C36 1.379(6) . ?
C35 C34 1.390(5) . ?
C36 C40 1.508(5) . ?
N2 C13 1.435(4) . ?
C45 C46 1.380(5) . ?
C45 C50 1.402(5) . ?
C45 N5 1.425(4) . ?
C50 C49 1.392(6) . ?
C50 C51 1.511(6) . ?
C46 C47 1.392(6) . ?
C22 N4 1.435(4) . ?
C22 C21 1.446(4) . ?
C22 C23 1.519(4) . ?
C21 N3 1.316(4) . ?
C21 C24 1.500(5) . ?
N4 C25 1.440(4) . ?
C13 C14 1.381(5) . ?
C13 C18 1.399(5) . ?
C14 C15 1.375(5) . ?
C18 C17 1.394(5) . ?
C18 C19 1.498(5) . ?
C17 C16 1.365(6) . ?
C16 C15 1.376(6) . ?
C16 C20 1.525(5) . ?
C49 C48 1.381(6) . ?
C47 C48 1.381(6) . ?
C48 C52 1.513(6) . ?
C25 C26 1.373(5) . ?
C25 C30 1.393(5) . ?
C26 C27 1.391(5) . ?
C30 C29 1.401(5) . ?
C30 C31 1.483(5) . ?
C29 C28 1.370(6) . ?
C28 C27 1.377(6) . ?
C28 C32 1.515(6) . ?
N6 C42 1.425(4) . ?
N5 C41 1.319(4) . ?
C41 C42 1.452(5) . ?
C41 C44 1.510(4) . ?
C42 C43 1.502(5) . ?

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 C22 117.54(13) . . ?
N1 Ni1 N2 84.74(11) . . ?
C22 Ni1 N2 157.53(12) . . ?
N5 Ni3 C2 119.28(13) . . ?
N5 Ni3 N6 84.46(11) . . ?
C2 Ni3 N6 156.08(12) . . ?
N3 Ni2 C42 118.27(12) . . ?
N3 Ni2 N4 85.04(11) . . ?
C42 Ni2 N4 156.62(12) . . ?
C6 C5 C10 118.1(3) . . ?
C6 C5 N1 121.4(3) . . ?
C10 C5 N1 120.3(3) . . ?
C9 C10 C5 117.8(4) . . ?
C9 C10 C11 120.9(4) . . ?
C5 C10 C11 121.4(4) . . ?
C7 C6 C5 121.7(4) . . ?
C9 C8 C7 117.5(4) . . ?
C9 C8 C12 121.3(5) . . ?
C7 C8 C12 121.2(5) . . ?
C8 C9 C10 123.9(4) . . ?
C6 C7 C8 121.0(4) . . ?
N2 C2 C1 113.4(3) . . ?
N2 C2 C4 119.8(3) . . ?
C1 C2 C4 119.5(3) . . ?
N2 C2 Ni3 64.10(16) . . ?
C1 C2 Ni3 109.7(2) . . ?
C4 C2 Ni3 117.8(2) . . ?
N1 C1 C2 117.8(3) . . ?
N1 C1 C3 123.3(3) . . ?
C2 C1 C3 118.8(3) . . ?
C54 C53 C58 117.9(3) . . ?
C54 C53 N6 121.1(3) . . ?
C58 C53 N6 120.7(3) . . ?
C56 C55 C54 120.9(4) . . ?
C53 C54 C55 121.8(3) . . ?
C57 C56 C55 116.9(3) . . ?
C57 C56 C60 122.2(4) . . ?
C55 C56 C60 120.8(4) . . ?
C57 C58 C53 118.6(3) . . ?
C57 C58 C59 120.1(3) . . ?
C53 C58 C59 121.3(3) . . ?
C56 C57 C58 123.8(3) . . ?
C37 C38 C33 117.7(4) . . ?
C37 C38 C39 121.6(3) . . ?
C33 C38 C39 120.7(3) . . ?
C34 C33 C38 118.9(3) . . ?
C34 C33 N3 121.5(3) . . ?
C38 C33 N3 119.5(3) . . ?
C36 C37 C38 123.5(4) . . ?
C36 C35 C34 120.0(4) . . ?
C33 C34 C35 121.8(4) . . ?
C35 C36 C37 118.1(4) . . ?
C35 C36 C40 122.3(4) . . ?
C37 C36 C40 119.7(4) . . ?
C2 N2 C13 119.2(3) . . ?
C2 N2 Ni1 107.2(2) . . ?
C13 N2 Ni1 126.7(2) . . ?
C1 N1 C5 122.8(3) . . ?
C1 N1 Ni1 112.6(2) . . ?
C5 N1 Ni1 122.8(2) . . ?
C46 C45 C50 118.9(4) . . ?
C46 C45 N5 122.5(3) . . ?
C50 C45 N5 118.3(3) . . ?
C49 C50 C45 118.4(4) . . ?
C49 C50 C51 119.9(4) . . ?
C45 C50 C51 121.8(4) . . ?
C45 C46 C47 120.7(4) . . ?
N4 C22 C21 114.3(3) . . ?
N4 C22 C23 120.0(3) . . ?
C21 C22 C23 118.6(3) . . ?
N4 C22 Ni1 64.22(16) . . ?
C21 C22 Ni1 111.1(2) . . ?
C23 C22 Ni1 116.5(2) . . ?
N3 C21 C22 116.9(3) . . ?
N3 C21 C24 123.8(3) . . ?
C22 C21 C24 119.2(3) . . ?
C21 N3 C33 120.3(3) . . ?
C21 N3 Ni2 112.8(2) . . ?
C33 N3 Ni2 125.3(2) . . ?
C22 N4 C25 116.2(2) . . ?
C22 N4 Ni2 106.13(19) . . ?
C25 N4 Ni2 131.1(2) . . ?
C14 C13 C18 117.7(3) . . ?
C14 C13 N2 122.4(3) . . ?
C18 C13 N2 119.9(3) . . ?
C15 C14 C13 122.2(4) . . ?
C17 C18 C13 118.6(4) . . ?
C17 C18 C19 121.9(3) . . ?
C13 C18 C19 119.6(3) . . ?
C16 C17 C18 123.4(4) . . ?
C17 C16 C15 117.3(4) . . ?
C17 C16 C20 120.5(4) . . ?
C15 C16 C20 122.2(4) . . ?
C14 C15 C16 120.8(4) . . ?
C48 C49 C50 123.6(4) . . ?
C48 C47 C46 121.9(4) . . ?
C47 C48 C49 116.5(4) . . ?
C47 C48 C52 122.2(5) . . ?
C49 C48 C52 121.3(5) . . ?
C26 C25 C30 118.6(3) . . ?
C26 C25 N4 122.0(3) . . ?
C30 C25 N4 119.3(3) . . ?
C25 C26 C27 121.3(3) . . ?
C25 C30 C29 118.7(4) . . ?
C25 C30 C31 120.5(3) . . ?
C29 C30 C31 120.7(3) . . ?
C28 C29 C30 122.7(4) . . ?
C29 C28 C27 117.5(4) . . ?
C29 C28 C32 120.5(4) . . ?
C27 C28 C32 121.9(4) . . ?
C28 C27 C26 120.9(4) . . ?
C53 N6 C42 120.4(3) . . ?
C53 N6 Ni3 125.1(2) . . ?
C42 N6 Ni3 107.7(2) . . ?
C41 N5 C45 123.3(3) . . ?
C41 N5 Ni3 112.4(2) . . ?
C45 N5 Ni3 121.9(2) . . ?
N5 C41 C42 117.1(3) . . ?
N5 C41 C44 123.4(3) . . ?
C42 C41 C44 119.5(3) . . ?
N6 C42 C41 113.7(3) . . ?
N6 C42 C43 121.1(3) . . ?
C41 C42 C43 119.5(3) . . ?
N6 C42 Ni2 64.66(15) . . ?
C41 C42 Ni2 108.6(2) . . ?
C43 C42 Ni2 116.3(2) . . ?

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
C6 C5 C10 C9 1.1(5) . . . . ?
N1 C5 C10 C9 -175.1(3) . . . . ?
C6 C5 C10 C11 -177.9(4) . . . . ?
N1 C5 C10 C11 5.9(6) . . . . ?
C10 C5 C6 C7 -1.0(6) . . . . ?
N1 C5 C6 C7 175.1(4) . . . . ?
C7 C8 C9 C10 -1.0(7) . . . . ?
C12 C8 C9 C10 -178.6(4) . . . . ?
C5 C10 C9 C8 0.0(6) . . . . ?
C11 C10 C9 C8 179.0(4) . . . . ?
C5 C6 C7 C8 -0.1(6) . . . . ?
C9 C8 C7 C6 1.1(6) . . . . ?
C12 C8 C7 C6 178.7(4) . . . . ?
N2 C2 C1 N1 -4.6(4) . . . . ?
C4 C2 C1 N1 -154.7(3) . . . . ?
Ni3 C2 C1 N1 64.9(3) . . . . ?
N2 C2 C1 C3 173.6(3) . . . . ?
C4 C2 C1 C3 23.5(5) . . . . ?
Ni3 C2 C1 C3 -116.9(3) . . . . ?
C58 C53 C54 C55 2.3(6) . . . . ?
N6 C53 C54 C55 -171.6(4) . . . . ?
C56 C55 C54 C53 -0.4(6) . . . . ?
C54 C55 C56 C57 -1.2(6) . . . . ?
C54 C55 C56 C60 179.4(4) . . . . ?
C54 C53 C58 C57 -2.6(5) . . . . ?
N6 C53 C58 C57 171.3(3) . . . . ?
C54 C53 C58 C59 180.0(4) . . . . ?
N6 C53 C58 C59 -6.1(5) . . . . ?
C55 C56 C57 C58 0.8(6) . . . . ?
C60 C56 C57 C58 -179.8(4) . . . . ?
C53 C58 C57 C56 1.1(6) . . . . ?
C59 C58 C57 C56 178.6(4) . . . . ?
C37 C38 C33 C34 0.6(5) . . . . ?
C39 C38 C33 C34 -179.0(3) . . . . ?
C37 C38 C33 N3 -176.5(3) . . . . ?
C39 C38 C33 N3 3.9(5) . . . . ?
C33 C38 C37 C36 -0.5(5) . . . . ?
C39 C38 C37 C36 179.1(4) . . . . ?
C38 C33 C34 C35 0.3(5) . . . . ?
N3 C33 C34 C35 177.3(3) . . . . ?
C36 C35 C34 C33 -1.3(6) . . . . ?
C34 C35 C36 C37 1.4(5) . . . . ?
C34 C35 C36 C40 -177.9(3) . . . . ?
C38 C37 C36 C35 -0.5(5) . . . . ?
C38 C37 C36 C40 178.9(3) . . . . ?
C1 C2 N2 C13 -135.8(3) . . . . ?
C4 C2 N2 C13 14.2(4) . . . . ?
Ni3 C2 N2 C13 122.8(3) . . . . ?
C1 C2 N2 Ni1 17.0(3) . . . . ?
C4 C2 N2 Ni1 167.0(3) . . . . ?
Ni3 C2 N2 Ni1 -84.42(13) . . . . ?
C2 C1 N1 C5 -176.4(3) . . . . ?
C3 C1 N1 C5 5.5(5) . . . . ?
C2 C1 N1 Ni1 -11.4(4) . . . . ?
C3 C1 N1 Ni1 170.5(3) . . . . ?
C6 C5 N1 C1 63.4(5) . . . . ?
C10 C5 N1 C1 -120.6(4) . . . . ?
C6 C5 N1 Ni1 -100.1(4) . . . . ?
C10 C5 N1 Ni1 76.0(4) . . . . ?
C46 C45 C50 C49 1.3(5) . . . . ?
N5 C45 C50 C49 -173.9(3) . . . . ?
C46 C45 C50 C51 -177.6(4) . . . . ?
N5 C45 C50 C51 7.2(5) . . . . ?
C50 C45 C46 C47 -1.9(6) . . . . ?
N5 C45 C46 C47 173.1(3) . . . . ?
N4 C22 C21 N3 -6.9(4) . . . . ?
C23 C22 C21 N3 -157.6(3) . . . . ?
Ni1 C22 C21 N3 63.4(3) . . . . ?
N4 C22 C21 C24 170.7(3) . . . . ?
C23 C22 C21 C24 20.1(5) . . . . ?
Ni1 C22 C21 C24 -119.0(3) . . . . ?
C22 C21 N3 C33 -176.8(3) . . . . ?
C24 C21 N3 C33 5.6(5) . . . . ?
C22 C21 N3 Ni2 -10.2(4) . . . . ?
C24 C21 N3 Ni2 172.3(3) . . . . ?
C34 C33 N3 C21 66.3(4) . . . . ?
C38 C33 N3 C21 -116.7(4) . . . . ?
C34 C33 N3 Ni2 -98.5(4) . . . . ?
C38 C33 N3 Ni2 78.4(4) . . . . ?
C21 C22 N4 C25 -135.7(3) . . . . ?
C23 C22 N4 C25 14.5(4) . . . . ?
Ni1 C22 N4 C25 121.6(3) . . . . ?
C21 C22 N4 Ni2 19.0(3) . . . . ?
C23 C22 N4 Ni2 169.3(2) . . . . ?
Ni1 C22 N4 Ni2 -83.73(13) . . . . ?
C2 N2 C13 C14 -101.0(4) . . . . ?
Ni1 N2 C13 C14 112.0(3) . . . . ?
C2 N2 C13 C18 81.8(4) . . . . ?
Ni1 N2 C13 C18 -65.2(4) . . . . ?
C18 C13 C14 C15 2.2(5) . . . . ?
N2 C13 C14 C15 -175.0(3) . . . . ?
C14 C13 C18 C17 -2.2(5) . . . . ?
N2 C13 C18 C17 175.1(3) . . . . ?
C14 C13 C18 C19 178.8(4) . . . . ?
N2 C13 C18 C19 -3.9(5) . . . . ?
C13 C18 C17 C16 0.3(6) . . . . ?
C19 C18 C17 C16 179.3(4) . . . . ?
C18 C17 C16 C15 1.7(6) . . . . ?
C18 C17 C16 C20 -179.9(4) . . . . ?
C13 C14 C15 C16 -0.3(6) . . . . ?
C17 C16 C15 C14 -1.7(6) . . . . ?
C20 C16 C15 C14 179.9(4) . . . . ?
C45 C50 C49 C48 0.4(6) . . . . ?
C51 C50 C49 C48 179.3(4) . . . . ?
C45 C46 C47 C48 0.8(6) . . . . ?
C46 C47 C48 C49 1.0(6) . . . . ?
C46 C47 C48 C52 -178.9(4) . . . . ?
C50 C49 C48 C47 -1.6(7) . . . . ?
C50 C49 C48 C52 178.3(4) . . . . ?
C22 N4 C25 C26 -97.2(4) . . . . ?
Ni2 N4 C25 C26 115.8(3) . . . . ?
C22 N4 C25 C30 81.5(4) . . . . ?
Ni2 N4 C25 C30 -65.5(4) . . . . ?
C30 C25 C26 C27 -3.5(5) . . . . ?
N4 C25 C26 C27 175.2(3) . . . . ?
C26 C25 C30 C29 4.2(5) . . . . ?
N4 C25 C30 C29 -174.6(3) . . . . ?
C26 C25 C30 C31 -175.4(4) . . . . ?
N4 C25 C30 C31 5.9(5) . . . . ?
C25 C30 C29 C28 -1.5(6) . . . . ?
C31 C30 C29 C28 178.1(4) . . . . ?
C30 C29 C28 C27 -2.0(6) . . . . ?
C30 C29 C28 C32 177.3(4) . . . . ?
C29 C28 C27 C26 2.7(6) . . . . ?
C32 C28 C27 C26 -176.5(4) . . . . ?
C25 C26 C27 C28 0.0(6) . . . . ?
C54 C53 N6 C42 -111.0(4) . . . . ?
C58 C53 N6 C42 75.3(4) . . . . ?
C54 C53 N6 Ni3 101.5(3) . . . . ?
C58 C53 N6 Ni3 -72.2(4) . . . . ?
C46 C45 N5 C41 60.6(5) . . . . ?
C50 C45 N5 C41 -124.3(4) . . . . ?
C46 C45 N5 Ni3 -100.3(4) . . . . ?
C50 C45 N5 Ni3 74.7(4) . . . . ?
C45 N5 C41 C42 -176.3(3) . . . . ?
Ni3 N5 C41 C42 -13.8(4) . . . . ?
C45 N5 C41 C44 4.4(5) . . . . ?
Ni3 N5 C41 C44 166.9(2) . . . . ?
C53 N6 C42 C41 -136.2(3) . . . . ?
Ni3 N6 C42 C41 16.3(3) . . . . ?
C53 N6 C42 C43 16.9(4) . . . . ?
Ni3 N6 C42 C43 169.5(3) . . . . ?
C53 N6 C42 Ni2 123.5(3) . . . . ?
Ni3 N6 C42 Ni2 -83.90(13) . . . . ?
N5 C41 C42 N6 -2.4(4) . . . . ?
C44 C41 C42 N6 176.9(3) . . . . ?
N5 C41 C42 C43 -156.0(3) . . . . ?
C44 C41 C42 C43 23.3(4) . . . . ?
N5 C41 C42 Ni2 67.4(3) . . . . ?
C44 C41 C42 Ni2 -113.3(3) . . . . ?

_refine_diff_density_max         0.516
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.094

