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

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

data_1
_database_code_depnum_ccdc_archive 'CCDC 1038632'
_audit_update_record             
;
2015-01-29 deposited with the CCDC.
2015-01-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H26 N10 Ni2'
_chemical_formula_sum            'C16 H32 N10 Ni2 O3'
_chemical_formula_weight         529.93

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   R-3c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'-x, -x+y, -z+1/2'
'x-y, -y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'x, x-y, z-1/2'
'-x+y, y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'

_cell_length_a                   28.9962(9)
_cell_length_b                   28.9962(9)
_cell_length_c                   32.8782(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     23939.8(16)
_cell_formula_units_Z            36
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    4456
_cell_measurement_theta_min      3.28
_cell_measurement_theta_max      24.58

_exptl_crystal_description       block
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             10008
_exptl_absorpt_coefficient_mu    1.449
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.704
_exptl_absorpt_correction_T_max  0.780
_exptl_absorpt_process_details   'SADABS (Bruker, 2013)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'TRIUMPH curved crystal monochromator'
_diffrn_measurement_device_type  'PHOTON100 CMOS detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            34812
_diffrn_reflns_av_R_equivalents  0.0880
_diffrn_reflns_av_sigmaI/netI    0.0670
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_theta_min         3.18
_diffrn_reflns_theta_max         26.37
_reflns_number_total             5370
_reflns_number_gt                3373
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          SQUEEZE

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0761P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5370
_refine_ls_number_parameters     425
_refine_ls_number_restraints     896
_refine_ls_R_factor_all          0.0913
_refine_ls_R_factor_gt           0.0516
_refine_ls_wR_factor_ref         0.1429
_refine_ls_wR_factor_gt          0.1305
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      0.988
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.002

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni2 Ni 0.3375(3) 0.1633(3) 0.0388(2) 0.041(2) Uani 0.49(3) 1 d P A 1
N5A N 0.4496(7) 0.2569(8) 0.0072(5) 0.042(3) Uani 0.49(3) 1 d PDU A 1
C5A C 0.4527(10) 0.2134(9) 0.0259(6) 0.046(4) Uani 0.49(3) 1 d PDU A 1
H5AA H 0.4892 0.2253 0.0356 0.056 Uiso 0.49(3) 1 calc PR A 1
H5AB H 0.4422 0.1838 0.0064 0.056 Uiso 0.49(3) 1 calc PR A 1
N6A N 0.4154(8) 0.1968(7) 0.0599(6) 0.031(3) Uani 0.49(3) 1 d PDU A 1
C6A C 0.4364(8) 0.2492(7) 0.0792(5) 0.032(3) Uani 0.49(3) 1 d PDU A 1
H6AA H 0.4693 0.2589 0.0947 0.039 Uiso 0.49(3) 1 calc PR A 1
H6AB H 0.4098 0.2497 0.0978 0.039 Uiso 0.49(3) 1 calc PR A 1
C7A C 0.4480(10) 0.2873(7) 0.0433(6) 0.049(4) Uani 0.49(3) 1 d PDU A 1
H7AA H 0.4196 0.2965 0.0404 0.059 Uiso 0.49(3) 1 calc PR A 1
H7AB H 0.4826 0.3205 0.0471 0.059 Uiso 0.49(3) 1 calc PR A 1
C8A C 0.4073(7) 0.2435(11) -0.0225(5) 0.039(3) Uani 0.49(3) 1 d PDU A 1
H8AA H 0.4166 0.2756 -0.0389 0.047 Uiso 0.49(3) 1 calc PR A 1
H8AB H 0.4061 0.2161 -0.0411 0.047 Uiso 0.49(3) 1 calc PR A 1
N7A N 0.3545(7) 0.2238(14) -0.0057(6) 0.031(4) Uani 0.49(3) 1 d PDU A 1
H7AC H 0.3527 0.2518 0.0065 0.037 Uiso 0.49(3) 1 calc PR A 1
C9A C 0.3098(7) 0.1971(10) -0.0365(6) 0.044(4) Uani 0.49(3) 1 d PDU A 1
H9AA H 0.3145 0.1714 -0.0532 0.052 Uiso 0.49(3) 1 calc PR A 1
H9AB H 0.3092 0.2240 -0.0548 0.052 Uiso 0.49(3) 1 calc PR A 1
C10A C 0.4150(7) 0.1550(7) 0.0857(6) 0.038(3) Uani 0.49(3) 1 d PDU A 1
H10A H 0.4473 0.1706 0.1030 0.045 Uiso 0.49(3) 1 calc PR A 1
H10B H 0.4153 0.1272 0.0683 0.045 Uiso 0.49(3) 1 calc PR A 1
N5B N 0.2266(7) 0.0710(8) 0.0747(6) 0.039(3) Uani 0.49(3) 1 d PDU A 1
C5B C 0.2680(8) 0.0987(10) 0.1048(6) 0.037(3) Uani 0.49(3) 1 d PDU A 1
H5BA H 0.2603 0.0770 0.1297 0.045 Uiso 0.49(3) 1 calc PR A 1
H5BB H 0.2709 0.1332 0.1120 0.045 Uiso 0.49(3) 1 calc PR A 1
N6B N 0.3171(7) 0.1070(8) 0.0856(7) 0.038(3) Uani 0.49(3) 1 d PDU A 1
C6B C 0.2988(8) 0.0518(9) 0.0721(9) 0.045(4) Uani 0.49(3) 1 d PDU A 1
H6BA H 0.2990 0.0295 0.0948 0.054 Uiso 0.49(3) 1 calc PR A 1
H6BB H 0.3212 0.0510 0.0497 0.054 Uiso 0.49(3) 1 calc PR A 1
C7B C 0.2421(9) 0.0332(8) 0.0576(8) 0.050(4) Uani 0.49(3) 1 d PDU A 1
H7BA H 0.2408 0.0334 0.0275 0.060 Uiso 0.49(3) 1 calc PR A 1
H7BB H 0.2175 -0.0034 0.0673 0.060 Uiso 0.49(3) 1 calc PR A 1
C8B C 0.2171(8) 0.1028(9) 0.0452(7) 0.043(4) Uani 0.49(3) 1 d PDU A 1
H8BA H 0.2130 0.1304 0.0598 0.052 Uiso 0.49(3) 1 calc PR A 1
H8BB H 0.1833 0.0796 0.0307 0.052 Uiso 0.49(3) 1 calc PR A 1
N7B N 0.2605(10) 0.1289(11) 0.0153(8) 0.030(3) Uani 0.49(3) 1 d PDU A 1
H7BC H 0.2571 0.1018 -0.0018 0.036 Uiso 0.49(3) 1 calc PR A 1
C9B C 0.2568(7) 0.1678(8) -0.0114(7) 0.026(3) Uani 0.49(3) 1 d PDU A 1
H9BA H 0.2521 0.1937 0.0051 0.031 Uiso 0.49(3) 1 calc PR A 1
H9BB H 0.2259 0.1493 -0.0300 0.031 Uiso 0.49(3) 1 calc PR A 1
C10B C 0.3649(8) 0.1302(9) 0.1125(6) 0.046(4) Uani 0.49(3) 1 d PDU A 1
H10C H 0.3643 0.1020 0.1299 0.055 Uiso 0.49(3) 1 calc PR A 1
H10D H 0.3650 0.1577 0.1303 0.055 Uiso 0.49(3) 1 calc PR A 1
Ni2' Ni 0.3404(3) 0.1654(3) 0.03877(19) 0.0284(16) Uani 0.51(3) 1 d P A 2
N5C N 0.4529(6) 0.2605(7) -0.0023(5) 0.031(3) Uani 0.51(3) 1 d PDU A 2
C5C C 0.4554(8) 0.2166(7) 0.0160(5) 0.028(3) Uani 0.51(3) 1 d PDU A 2
H5CA H 0.4926 0.2273 0.0233 0.034 Uiso 0.51(3) 1 calc PR A 2
H5CB H 0.4415 0.1859 -0.0028 0.034 Uiso 0.51(3) 1 calc PR A 2
N6C N 0.4219(8) 0.2032(7) 0.0527(6) 0.034(3) Uani 0.51(3) 1 d PDU A 2
C6C C 0.4449(9) 0.2573(7) 0.0699(5) 0.044(4) Uani 0.51(3) 1 d PDU A 2
H6CA H 0.4778 0.2668 0.0854 0.053 Uiso 0.51(3) 1 calc PR A 2
H6CB H 0.4192 0.2597 0.0883 0.053 Uiso 0.51(3) 1 calc PR A 2
C7C C 0.4572(8) 0.2940(7) 0.0336(6) 0.039(3) Uani 0.51(3) 1 d PDU A 2
H7CA H 0.4313 0.3066 0.0317 0.046 Uiso 0.51(3) 1 calc PR A 2
H7CB H 0.4935 0.3252 0.0357 0.046 Uiso 0.51(3) 1 calc PR A 2
C8C C 0.4050(7) 0.2460(11) -0.0274(5) 0.044(4) Uani 0.51(3) 1 d PDU A 2
H8CA H 0.4029 0.2221 -0.0497 0.053 Uiso 0.51(3) 1 calc PR A 2
H8CB H 0.4082 0.2786 -0.0398 0.053 Uiso 0.51(3) 1 calc PR A 2
N7C N 0.3553(7) 0.2190(13) -0.0029(6) 0.034(4) Uani 0.51(3) 1 d PDU A 2
H7CC H 0.3541 0.2464 0.0108 0.041 Uiso 0.51(3) 1 calc PR A 2
C9C C 0.3063(6) 0.1946(9) -0.0296(6) 0.028(3) Uani 0.51(3) 1 d PDU A 2
H9CA H 0.3084 0.1702 -0.0496 0.033 Uiso 0.51(3) 1 calc PR A 2
H9CB H 0.3039 0.2229 -0.0447 0.033 Uiso 0.51(3) 1 calc PR A 2
C10C C 0.4267(8) 0.1649(8) 0.0795(6) 0.046(4) Uani 0.51(3) 1 d PDU A 2
H10E H 0.4606 0.1833 0.0948 0.055 Uiso 0.51(3) 1 calc PR A 2
H10F H 0.4267 0.1364 0.0630 0.055 Uiso 0.51(3) 1 calc PR A 2
N5D N 0.2361(7) 0.0677(7) 0.0815(6) 0.037(3) Uani 0.51(3) 1 d PDU A 2
C5D C 0.2807(8) 0.1006(10) 0.1084(6) 0.043(4) Uani 0.51(3) 1 d PDU A 2
H5DA H 0.2787 0.0810 0.1336 0.051 Uiso 0.51(3) 1 calc PR A 2
H5DB H 0.2806 0.1336 0.1158 0.051 Uiso 0.51(3) 1 calc PR A 2
N6D N 0.3289(7) 0.1132(8) 0.0852(7) 0.040(3) Uani 0.51(3) 1 d PDU A 2
C6D C 0.3143(8) 0.0581(8) 0.0733(9) 0.043(3) Uani 0.51(3) 1 d PDU A 2
H6DA H 0.3197 0.0389 0.0961 0.052 Uiso 0.51(3) 1 calc PR A 2
H6DB H 0.3353 0.0581 0.0495 0.052 Uiso 0.51(3) 1 calc PR A 2
C7D C 0.2553(8) 0.0336(7) 0.0627(7) 0.044(4) Uani 0.51(3) 1 d PDU A 2
H7DA H 0.2506 0.0324 0.0328 0.053 Uiso 0.51(3) 1 calc PR A 2
H7DB H 0.2349 -0.0031 0.0734 0.053 Uiso 0.51(3) 1 calc PR A 2
C8D C 0.2211(8) 0.0964(9) 0.0526(6) 0.031(3) Uani 0.51(3) 1 d PDU A 2
H8DA H 0.2150 0.1226 0.0674 0.038 Uiso 0.51(3) 1 calc PR A 2
H8DB H 0.1875 0.0709 0.0389 0.038 Uiso 0.51(3) 1 calc PR A 2
N7D N 0.2633(11) 0.1244(11) 0.0217(8) 0.036(4) Uani 0.51(3) 1 d PDU A 2
H7DC H 0.2604 0.0985 0.0035 0.043 Uiso 0.51(3) 1 calc PR A 2
C9D C 0.2567(7) 0.1637(9) -0.0025(7) 0.039(4) Uani 0.51(3) 1 d PDU A 2
H9DA H 0.2527 0.1886 0.0158 0.046 Uiso 0.51(3) 1 calc PR A 2
H9DB H 0.2244 0.1452 -0.0197 0.046 Uiso 0.51(3) 1 calc PR A 2
C10D C 0.3794(7) 0.1406(8) 0.1094(5) 0.040(3) Uani 0.51(3) 1 d PDU A 2
H10G H 0.3820 0.1147 0.1275 0.048 Uiso 0.51(3) 1 calc PR A 2
H10H H 0.3798 0.1689 0.1264 0.048 Uiso 0.51(3) 1 calc PR A 2
C1 C 0.23862(16) 0.30409(16) 0.13986(12) 0.0331(9) Uani 1 1 d . A .
C2 C 0.30457(16) 0.23907(15) 0.08799(10) 0.0289(9) Uani 1 1 d . A .
C3 C 0.33296(17) 0.31463(16) 0.14442(12) 0.0312(9) Uani 1 1 d . A .
C4 C 0.21555(19) 0.24124(18) 0.07546(12) 0.0418(11) Uani 1 1 d . A .
N1 N 0.21468(14) 0.31520(15) 0.16200(10) 0.0410(9) Uani 1 1 d . . .
N2 N 0.32177(14) 0.21372(13) 0.07548(10) 0.0363(8) Uani 1 1 d . . .
N3 N 0.36842(15) 0.33885(15) 0.16537(11) 0.0467(10) Uani 1 1 d . . .
N4 N 0.17961(18) 0.22008(18) 0.05399(12) 0.0620(12) Uani 1 1 d . . .
Ni1 Ni 0.27404(2) 0.27647(2) 0.110496(14) 0.02911(17) 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
Ni2 N6A 2.08(2) . ?
Ni2 N7B 2.09(3) . ?
Ni2 N1 2.098(7) 28 ?
Ni2 N6B 2.10(2) . ?
Ni2 N2 2.115(7) . ?
Ni2 N7A 2.14(3) . ?
N5A C5A 1.446(11) . ?
N5A C8A 1.460(12) . ?
N5A C7A 1.494(11) . ?
C5A N6A 1.460(11) . ?
C5A H5AA 0.9900 . ?
C5A H5AB 0.9900 . ?
N6A C6A 1.468(10) . ?
N6A C10A 1.475(12) . ?
C6A C7A 1.533(11) . ?
C6A H6AA 0.9900 . ?
C6A H6AB 0.9900 . ?
C7A H7AA 0.9900 . ?
C7A H7AB 0.9900 . ?
C8A N7A 1.449(14) . ?
C8A H8AA 0.9900 . ?
C8A H8AB 0.9900 . ?
N7A C9A 1.515(14) . ?
N7A H7AC 0.9300 . ?
C9A C9B 1.567(13) . ?
C9A H9AA 0.9900 . ?
C9A H9AB 0.9900 . ?
C10A C10B 1.537(13) . ?
C10A H10A 0.9900 . ?
C10A H10B 0.9900 . ?
N5B C5B 1.449(10) . ?
N5B C8B 1.456(11) . ?
N5B C7B 1.486(11) . ?
C5B N6B 1.463(10) . ?
C5B H5BA 0.9900 . ?
C5B H5BB 0.9900 . ?
N6B C6B 1.483(10) . ?
N6B C10B 1.490(13) . ?
C6B C7B 1.528(12) . ?
C6B H6BA 0.9900 . ?
C6B H6BB 0.9900 . ?
C7B H7BA 0.9900 . ?
C7B H7BB 0.9900 . ?
C8B N7B 1.475(14) . ?
C8B H8BA 0.9900 . ?
C8B H8BB 0.9900 . ?
N7B C9B 1.475(13) . ?
N7B H7BC 0.9300 . ?
C9B H9BA 0.9900 . ?
C9B H9BB 0.9900 . ?
C10B H10C 0.9900 . ?
C10B H10D 0.9900 . ?
Ni2' N7C 1.95(3) . ?
Ni2' N7D 2.02(3) . ?
Ni2' N6D 2.06(3) . ?
Ni2' N6C 2.10(2) . ?
Ni2' N1 2.100(6) 28 ?
Ni2' N2 2.115(6) . ?
N5C C5C 1.444(10) . ?
N5C C8C 1.484(11) . ?
N5C C7C 1.493(10) . ?
C5C N6C 1.474(10) . ?
C5C H5CA 0.9900 . ?
C5C H5CB 0.9900 . ?
N6C C6C 1.477(10) . ?
N6C C10C 1.477(13) . ?
C6C C7C 1.517(11) . ?
C6C H6CA 0.9900 . ?
C6C H6CB 0.9900 . ?
C7C H7CA 0.9900 . ?
C7C H7CB 0.9900 . ?
C8C N7C 1.486(15) . ?
C8C H8CA 0.9900 . ?
C8C H8CB 0.9900 . ?
N7C C9C 1.513(13) . ?
N7C H7CC 0.9300 . ?
C9C C9D 1.540(12) . ?
C9C H9CA 0.9900 . ?
C9C H9CB 0.9900 . ?
C10C C10D 1.540(12) . ?
C10C H10E 0.9900 . ?
C10C H10F 0.9900 . ?
N5D C5D 1.459(10) . ?
N5D C8D 1.465(11) . ?
N5D C7D 1.489(11) . ?
C5D N6D 1.468(11) . ?
C5D H5DA 0.9900 . ?
C5D H5DB 0.9900 . ?
N6D C6D 1.486(11) . ?
N6D C10D 1.498(13) . ?
C6D C7D 1.529(11) . ?
C6D H6DA 0.9900 . ?
C6D H6DB 0.9900 . ?
C7D H7DA 0.9900 . ?
C7D H7DB 0.9900 . ?
C8D N7D 1.481(13) . ?
C8D H8DA 0.9900 . ?
C8D H8DB 0.9900 . ?
N7D C9D 1.478(14) . ?
N7D H7DC 0.9300 . ?
C9D H9DA 0.9900 . ?
C9D H9DB 0.9900 . ?
C10D H10G 0.9900 . ?
C10D H10H 0.9900 . ?
C1 N1 1.157(5) . ?
C1 Ni1 1.858(4) . ?
C2 N2 1.151(5) . ?
C2 Ni1 1.862(4) . ?
C3 N3 1.141(5) . ?
C3 Ni1 1.870(4) . ?
C4 N4 1.149(5) . ?
C4 Ni1 1.875(4) . ?
N1 Ni2 2.098(7) 34 ?
N1 Ni2' 2.100(6) 34 ?

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
N6A Ni2 N7B 177.5(10) . . ?
N6A Ni2 N1 91.0(6) . 28 ?
N7B Ni2 N1 86.7(9) . 28 ?
N6A Ni2 N6B 86.4(7) . . ?
N7B Ni2 N6B 94.7(8) . . ?
N1 Ni2 N6B 94.9(6) 28 . ?
N6A Ni2 N2 92.6(6) . . ?
N7B Ni2 N2 89.6(8) . . ?
N1 Ni2 N2 171.9(4) 28 . ?
N6B Ni2 N2 92.5(6) . . ?
N6A Ni2 N7A 95.4(7) . . ?
N7B Ni2 N7A 83.7(7) . . ?
N1 Ni2 N7A 90.3(9) 28 . ?
N6B Ni2 N7A 174.5(11) . . ?
N2 Ni2 N7A 82.2(9) . . ?
C5A N5A C8A 117.4(10) . . ?
C5A N5A C7A 102.2(9) . . ?
C8A N5A C7A 114.8(10) . . ?
N5A C5A N6A 104.7(10) . . ?
N5A C5A H5AA 110.8 . . ?
N6A C5A H5AA 110.8 . . ?
N5A C5A H5AB 110.8 . . ?
N6A C5A H5AB 110.8 . . ?
H5AA C5A H5AB 108.9 . . ?
C5A N6A C6A 97.8(10) . . ?
C5A N6A C10A 114.2(11) . . ?
C6A N6A C10A 115.5(10) . . ?
C5A N6A Ni2 110.5(13) . . ?
C6A N6A Ni2 114.8(13) . . ?
C10A N6A Ni2 104.4(10) . . ?
N6A C6A C7A 104.0(9) . . ?
N6A C6A H6AA 111.0 . . ?
C7A C6A H6AA 111.0 . . ?
N6A C6A H6AB 111.0 . . ?
C7A C6A H6AB 111.0 . . ?
H6AA C6A H6AB 109.0 . . ?
N5A C7A C6A 104.3(9) . . ?
N5A C7A H7AA 110.9 . . ?
C6A C7A H7AA 110.9 . . ?
N5A C7A H7AB 110.9 . . ?
C6A C7A H7AB 110.9 . . ?
H7AA C7A H7AB 108.9 . . ?
N7A C8A N5A 115.7(11) . . ?
N7A C8A H8AA 108.3 . . ?
N5A C8A H8AA 108.4 . . ?
N7A C8A H8AB 108.4 . . ?
N5A C8A H8AB 108.4 . . ?
H8AA C8A H8AB 107.4 . . ?
C8A N7A C9A 114.4(13) . . ?
C8A N7A Ni2 110(2) . . ?
C9A N7A Ni2 104.5(16) . . ?
C8A N7A H7AC 109.2 . . ?
C9A N7A H7AC 109.2 . . ?
Ni2 N7A H7AC 109.2 . . ?
N7A C9A C9B 106.4(11) . . ?
N7A C9A H9AA 110.4 . . ?
C9B C9A H9AA 110.4 . . ?
N7A C9A H9AB 110.4 . . ?
C9B C9A H9AB 110.4 . . ?
H9AA C9A H9AB 108.6 . . ?
N6A C10A C10B 109.3(10) . . ?
N6A C10A H10A 109.8 . . ?
C10B C10A H10A 109.8 . . ?
N6A C10A H10B 109.8 . . ?
C10B C10A H10B 109.8 . . ?
H10A C10A H10B 108.3 . . ?
C5B N5B C8B 118.0(10) . . ?
C5B N5B C7B 101.2(9) . . ?
C8B N5B C7B 116.0(10) . . ?
N5B C5B N6B 105.4(10) . . ?
N5B C5B H5BA 110.7 . . ?
N6B C5B H5BA 110.6 . . ?
N5B C5B H5BB 110.7 . . ?
N6B C5B H5BB 110.7 . . ?
H5BA C5B H5BB 108.8 . . ?
C5B N6B C6B 99.0(10) . . ?
C5B N6B C10B 115.4(11) . . ?
C6B N6B C10B 114.5(11) . . ?
C5B N6B Ni2 108.5(14) . . ?
C6B N6B Ni2 115.4(14) . . ?
C10B N6B Ni2 104.4(10) . . ?
N6B C6B C7B 102.4(10) . . ?
N6B C6B H6BA 111.3 . . ?
C7B C6B H6BA 111.3 . . ?
N6B C6B H6BB 111.3 . . ?
C7B C6B H6BB 111.3 . . ?
H6BA C6B H6BB 109.2 . . ?
N5B C7B C6B 106.9(9) . . ?
N5B C7B H7BA 110.3 . . ?
C6B C7B H7BA 110.3 . . ?
N5B C7B H7BB 110.3 . . ?
C6B C7B H7BB 110.3 . . ?
H7BA C7B H7BB 108.6 . . ?
N5B C8B N7B 112.6(11) . . ?
N5B C8B H8BA 109.1 . . ?
N7B C8B H8BA 109.1 . . ?
N5B C8B H8BB 109.1 . . ?
N7B C8B H8BB 109.1 . . ?
H8BA C8B H8BB 107.8 . . ?
C9B N7B C8B 114.7(13) . . ?
C9B N7B Ni2 109.0(14) . . ?
C8B N7B Ni2 115.7(14) . . ?
C9B N7B H7BC 105.5 . . ?
C8B N7B H7BC 105.5 . . ?
Ni2 N7B H7BC 105.5 . . ?
N7B C9B C9A 107.5(10) . . ?
N7B C9B H9BA 110.2 . . ?
C9A C9B H9BA 110.2 . . ?
N7B C9B H9BB 110.2 . . ?
C9A C9B H9BB 110.2 . . ?
H9BA C9B H9BB 108.5 . . ?
N6B C10B C10A 108.6(10) . . ?
N6B C10B H10C 110.0 . . ?
C10A C10B H10C 110.0 . . ?
N6B C10B H10D 110.0 . . ?
C10A C10B H10D 110.0 . . ?
H10C C10B H10D 108.4 . . ?
N7C Ni2' N7D 90.7(7) . . ?
N7C Ni2' N6D 175.8(10) . . ?
N7D Ni2' N6D 92.8(7) . . ?
N7C Ni2' N6C 89.7(8) . . ?
N7D Ni2' N6C 174.4(10) . . ?
N6D Ni2' N6C 87.1(7) . . ?
N7C Ni2' N1 89.6(9) . 28 ?
N7D Ni2' N1 85.0(9) . 28 ?
N6D Ni2' N1 92.9(6) . 28 ?
N6C Ni2' N1 89.4(6) . 28 ?
N7C Ni2' N2 84.3(9) . . ?
N7D Ni2' N2 88.5(9) . . ?
N6D Ni2' N2 93.6(7) . . ?
N6C Ni2' N2 97.1(6) . . ?
N1 Ni2' N2 171.0(4) 28 . ?
C5C N5C C8C 115.8(9) . . ?
C5C N5C C7C 102.5(8) . . ?
C8C N5C C7C 112.9(9) . . ?
N5C C5C N6C 104.9(9) . . ?
N5C C5C H5CA 110.8 . . ?
N6C C5C H5CA 110.8 . . ?
N5C C5C H5CB 110.8 . . ?
N6C C5C H5CB 110.8 . . ?
H5CA C5C H5CB 108.8 . . ?
C5C N6C C6C 98.3(9) . . ?
C5C N6C C10C 113.0(11) . . ?
C6C N6C C10C 114.0(11) . . ?
C5C N6C Ni2' 112.4(12) . . ?
C6C N6C Ni2' 115.5(13) . . ?
C10C N6C Ni2' 104.0(10) . . ?
N6C C6C C7C 105.5(8) . . ?
N6C C6C H6CA 110.6 . . ?
C7C C6C H6CA 110.6 . . ?
N6C C6C H6CB 110.6 . . ?
C7C C6C H6CB 110.6 . . ?
H6CA C6C H6CB 108.8 . . ?
N5C C7C C6C 104.7(8) . . ?
N5C C7C H7CA 110.8 . . ?
C6C C7C H7CA 110.8 . . ?
N5C C7C H7CB 110.8 . . ?
C6C C7C H7CB 110.8 . . ?
H7CA C7C H7CB 108.9 . . ?
N5C C8C N7C 111.7(11) . . ?
N5C C8C H8CA 109.3 . . ?
N7C C8C H8CA 109.3 . . ?
N5C C8C H8CB 109.3 . . ?
N7C C8C H8CB 109.3 . . ?
H8CA C8C H8CB 107.9 . . ?
C8C N7C C9C 111.6(12) . . ?
C8C N7C Ni2' 124.8(19) . . ?
C9C N7C Ni2' 104.7(14) . . ?
C8C N7C H7CC 104.7 . . ?
C9C N7C H7CC 104.7 . . ?
Ni2' N7C H7CC 104.7 . . ?
N7C C9C C9D 108.8(9) . . ?
N7C C9C H9CA 109.9 . . ?
C9D C9C H9CA 109.9 . . ?
N7C C9C H9CB 109.9 . . ?
C9D C9C H9CB 109.9 . . ?
H9CA C9C H9CB 108.3 . . ?
N6C C10C C10D 109.2(10) . . ?
N6C C10C H10E 109.8 . . ?
C10D C10C H10E 109.8 . . ?
N6C C10C H10F 109.8 . . ?
C10D C10C H10F 109.8 . . ?
H10E C10C H10F 108.3 . . ?
C5D N5D C8D 116.0(10) . . ?
C5D N5D C7D 100.6(9) . . ?
C8D N5D C7D 115.0(9) . . ?
N5D C5D N6D 105.6(10) . . ?
N5D C5D H5DA 110.6 . . ?
N6D C5D H5DA 110.6 . . ?
N5D C5D H5DB 110.6 . . ?
N6D C5D H5DB 110.6 . . ?
H5DA C5D H5DB 108.7 . . ?
C5D N6D C6D 98.5(10) . . ?
C5D N6D C10D 114.5(11) . . ?
C6D N6D C10D 112.7(11) . . ?
C5D N6D Ni2' 110.6(14) . . ?
C6D N6D Ni2' 116.7(14) . . ?
C10D N6D Ni2' 104.3(10) . . ?
N6D C6D C7D 102.1(9) . . ?
N6D C6D H6DA 111.4 . . ?
C7D C6D H6DA 111.4 . . ?
N6D C6D H6DB 111.4 . . ?
C7D C6D H6DB 111.4 . . ?
H6DA C6D H6DB 109.2 . . ?
N5D C7D C6D 107.5(9) . . ?
N5D C7D H7DA 110.2 . . ?
C6D C7D H7DA 110.2 . . ?
N5D C7D H7DB 110.2 . . ?
C6D C7D H7DB 110.2 . . ?
H7DA C7D H7DB 108.5 . . ?
N5D C8D N7D 111.0(10) . . ?
N5D C8D H8DA 109.4 . . ?
N7D C8D H8DA 109.4 . . ?
N5D C8D H8DB 109.4 . . ?
N7D C8D H8DB 109.4 . . ?
H8DA C8D H8DB 108.0 . . ?
C9D N7D C8D 113.7(13) . . ?
C9D N7D Ni2' 103.2(14) . . ?
C8D N7D Ni2' 120.0(15) . . ?
C9D N7D H7DC 106.3 . . ?
C8D N7D H7DC 106.3 . . ?
Ni2' N7D H7DC 106.3 . . ?
N7D C9D C9C 108.5(11) . . ?
N7D C9D H9DA 110.0 . . ?
C9C C9D H9DA 110.0 . . ?
N7D C9D H9DB 110.0 . . ?
C9C C9D H9DB 110.0 . . ?
H9DA C9D H9DB 108.4 . . ?
N6D C10D C10C 108.4(9) . . ?
N6D C10D H10G 110.0 . . ?
C10C C10D H10G 110.0 . . ?
N6D C10D H10H 110.0 . . ?
C10C C10D H10H 110.0 . . ?
H10G C10D H10H 108.4 . . ?
N1 C1 Ni1 170.0(4) . . ?
N2 C2 Ni1 176.3(4) . . ?
N3 C3 Ni1 178.1(4) . . ?
N4 C4 Ni1 179.3(4) . . ?
C1 N1 Ni2 174.6(4) . 34 ?
C1 N1 Ni2' 173.0(4) . 34 ?
Ni2 N1 Ni2' 2.0(5) 34 34 ?
C2 N2 Ni2 163.3(4) . . ?
C2 N2 Ni2' 164.4(4) . . ?
Ni2 N2 Ni2' 2.0(5) . . ?
C1 Ni1 C2 169.72(17) . . ?
C1 Ni1 C3 88.48(17) . . ?
C2 Ni1 C3 91.25(16) . . ?
C1 Ni1 C4 90.56(18) . . ?
C2 Ni1 C4 90.14(18) . . ?
C3 Ni1 C4 177.33(18) . . ?

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 -0.003 2591 463 ' '
2 0.667 0.333 0.478 2599 464 ' '
3 0.333 0.667 0.310 2600 464 ' '
_platon_squeeze_details          
;
;

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.090
_exptl_crystal_preparation       'Magnetic properties, Gas adsorption'
####################################################################### 
# 
# 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 1038633'
_audit_update_record             
;
2015-01-29 deposited with the CCDC.
2015-01-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H35 N11 Ni2 O'
_chemical_formula_weight         563.01

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'
O O 0.0106 0.0060 '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                   9.812(2)
_cell_length_b                   13.179(3)
_cell_length_c                   20.122(4)
_cell_angle_alpha                90
_cell_angle_beta                 102.78(3)
_cell_angle_gamma                90
_cell_volume                     2537.5(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_F_000             1184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.4550
_exptl_crystal_size_mid          0.1650
_exptl_crystal_size_min          0.1150
_exptl_absorpt_coefficient_mu    1.520
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8391
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30130
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.861
_diffrn_reflns_theta_max         31.492
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             8372
_reflns_number_gt                7436
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0889P)²+2.7369P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8372
_refine_ls_number_parameters     316
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0721
_refine_ls_wR_factor_ref         0.1978
_refine_ls_wR_factor_gt          0.1849
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_restrained_S_all      1.170
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.74619(4) 0.72176(3) 0.10251(2) 0.02188(12) Uani 1 1 d . . . . .
Ni2 Ni 0.49857(4) 0.73355(3) -0.14898(2) 0.02552(12) Uani 1 1 d . . . . .
C4 C 0.5902(3) 0.7198(3) -0.05790(16) 0.0288(6) Uani 1 1 d . . . . .
C2 C 0.4031(3) 0.7515(3) -0.23878(16) 0.0276(6) Uani 1 1 d . . . . .
C3 C 0.3332(4) 0.7649(3) -0.12193(17) 0.0323(7) Uani 1 1 d . . . . .
C1 C 0.6605(4) 0.6977(3) -0.17900(17) 0.0380(8) Uani 1 1 d . . . . .
N2 N 0.6450(3) 0.7145(2) -0.00116(14) 0.0309(6) Uani 1 1 d . . . . .
N3 N 0.7581(4) 0.6778(4) -0.19915(19) 0.0575(11) Uani 1 1 d . . . . .
N1 N 0.2267(4) 0.7800(3) -0.10872(19) 0.0480(9) Uani 1 1 d . . . . .
N7 N 0.6697(4) 0.5747(3) 0.12033(15) 0.0407(7) Uani 1 1 d . . . . .
N4 N 0.5724(3) 0.7955(3) 0.12281(15) 0.0339(6) Uani 1 1 d D . . . .
N5 N 0.8178(3) 0.8647(3) 0.08563(15) 0.0383(7) Uani 1 1 d D . . . .
N9 N 1.0609(3) 0.8077(4) 0.09333(17) 0.0512(10) Uani 1 1 d . . . . .
N6 N 0.9252(4) 0.6501(3) 0.08115(15) 0.0443(9) Uani 1 1 d . . . . .
N8 N 0.4308(4) 0.6377(3) 0.11093(17) 0.0479(9) Uani 1 1 d . . . . .
C10 C 0.5809(5) 0.8995(3) 0.0967(2) 0.0472(10) Uani 1 1 d . . . . .
H10A H 0.5231 0.9447 0.1168 0.057 Uiso 1 1 calc R U . . .
H10B H 0.5465 0.9003 0.0477 0.057 Uiso 1 1 calc R U . . .
C7 C 1.0542(4) 0.7050(5) 0.1171(2) 0.0572(14) Uani 1 1 d . . . . .
H7A H 1.0570 0.7062 0.1656 0.069 Uiso 1 1 calc R U . . .
H7B H 1.1357 0.6681 0.1105 0.069 Uiso 1 1 calc R U . . .
C8 C 0.9713(4) 0.8827(4) 0.1119(2) 0.0523(12) Uani 1 1 d . . . . .
H8A H 0.9949 0.9480 0.0952 0.063 Uiso 1 1 calc R U . . .
H8B H 0.9900 0.8867 0.1612 0.063 Uiso 1 1 calc R U . . .
C5 C 0.9551(4) 0.7428(4) -0.0247(2) 0.0504(11) Uani 1 1 d . . . . .
H5A H 0.9776 0.7321 -0.0688 0.060 Uiso 1 1 calc R U . . .
H5B H 0.8671 0.7792 -0.0320 0.060 Uiso 1 1 calc R U . . .
C6 C 0.9385(5) 0.6391(4) 0.0082(2) 0.0518(12) Uani 1 1 d . . . . .
H6A H 0.8561 0.6053 -0.0179 0.062 Uiso 1 1 calc R U . . .
H6B H 1.0190 0.5971 0.0067 0.062 Uiso 1 1 calc R U . . .
C12 C 0.5190(5) 0.5687(4) 0.08395(19) 0.0519(12) Uani 1 1 d . . . . .
H12A H 0.5113 0.5837 0.0361 0.062 Uiso 1 1 calc R U . . .
H12B H 0.4858 0.5000 0.0873 0.062 Uiso 1 1 calc R U . . .
C9 C 0.7308(5) 0.9355(3) 0.1144(2) 0.0496(10) Uani 1 1 d . . . . .
H9A H 0.7371 1.0029 0.0959 0.060 Uiso 1 1 calc R U . . .
H9B H 0.7635 0.9389 0.1635 0.060 Uiso 1 1 calc R U . . .
C13 C 0.6735(5) 0.5390(3) 0.1915(2) 0.0472(10) Uani 1 1 d . . . . .
H13A H 0.7688 0.5424 0.2180 0.057 Uiso 1 1 calc R U . . .
H13B H 0.6437 0.4687 0.1901 0.057 Uiso 1 1 calc R U . . .
C11 C 0.4368(4) 0.7447(4) 0.0955(2) 0.0430(9) Uani 1 1 d . . . . .
H11A H 0.3651 0.7795 0.1131 0.052 Uiso 1 1 calc R U . . .
H11B H 0.4140 0.7527 0.0463 0.052 Uiso 1 1 calc R U . . .
C14 C 0.5805(4) 0.6020(3) 0.22589(18) 0.0405(8) Uani 1 1 d . . . . .
H14A H 0.6209 0.6691 0.2352 0.049 Uiso 1 1 calc R U . . .
H14B H 0.5766 0.5709 0.2691 0.049 Uiso 1 1 calc R U . . .
C15 C 0.4328(5) 0.6121(4) 0.1826(2) 0.0537(12) Uani 1 1 d . . . . .
H15A H 0.3834 0.5487 0.1841 0.064 Uiso 1 1 calc R U . . .
H15B H 0.3838 0.6645 0.2019 0.064 Uiso 1 1 calc R U . . .
C16 C 1.0696(5) 0.8068(6) 0.0198(2) 0.0655(17) Uani 1 1 d . . . . .
H16A H 1.1601 0.7804 0.0164 0.079 Uiso 1 1 calc R U . . .
H16B H 1.0627 0.8759 0.0028 0.079 Uiso 1 1 calc R U . . .
C17 C 0.9124(5) 0.5485(4) 0.1091(2) 0.0566(13) Uani 1 1 d . . . . .
H17A H 0.9422 0.5507 0.1583 0.068 Uiso 1 1 calc R U . . .
H17B H 0.9734 0.5019 0.0921 0.068 Uiso 1 1 calc R U . . .
C18 C 0.7619(6) 0.5097(4) 0.0892(2) 0.0576(13) Uani 1 1 d . . . . .
H18A H 0.7301 0.5104 0.0400 0.069 Uiso 1 1 calc R U . . .
H18B H 0.7579 0.4403 0.1048 0.069 Uiso 1 1 calc R U . . .
N10 N 0.3447(3) 0.7634(2) -0.29446(14) 0.0283(6) Uani 1 1 d . . . . .
O1W O 0.0349(3) 0.6501(3) 0.77325(17) 0.0550(8) Uani 1 1 d . . . . .
N1W N 0.7442(5) 0.9603(4) 0.9388(2) 0.0657(12) Uani 1 1 d . . . . .
C1W C 0.7303(5) 0.9645(4) 0.8808(2) 0.0505(10) Uani 1 1 d . . . . .
C2W C 0.7138(7) 0.9732(5) 0.8077(3) 0.0744(17) Uani 1 1 d . . . . .
H2W1 H 0.7469 1.0384 0.7969 0.112 Uiso 1 1 calc R U . . .
H2W2 H 0.6168 0.9662 0.7859 0.112 Uiso 1 1 calc R U . . .
H2W3 H 0.7667 0.9208 0.7919 0.112 Uiso 1 1 calc R U . . .
H2N H 0.791(5) 0.876(4) 0.0401(7) 0.057(15) Uiso 1 1 d D . . . .
H1N H 0.580(4) 0.805(3) 0.1679(7) 0.040(12) Uiso 1 1 d D . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N5 2.065(3) . ?
Ni1 N4 2.080(3) . ?
Ni1 N10 2.094(3) 4_676 ?
Ni1 N2 2.105(3) . ?
Ni1 N6 2.121(3) . ?
Ni1 N7 2.136(3) . ?
Ni2 C2 1.857(3) . ?
Ni2 C4 1.863(3) . ?
Ni2 C3 1.868(4) . ?
Ni2 C1 1.880(4) . ?
C4 N2 1.152(4) . ?
C2 N10 1.151(4) . ?
C3 N1 1.151(5) . ?
C1 N3 1.150(5) . ?
N7 C18 1.482(6) . ?
N7 C13 1.499(5) . ?
N7 C12 1.500(6) . ?
N4 C10 1.477(5) . ?
N4 C11 1.483(5) . ?
N5 C9 1.467(6) . ?
N5 C8 1.501(5) . ?
N9 C8 1.427(7) . ?
N9 C7 1.441(7) . ?
N9 C16 1.500(5) . ?
N6 C17 1.468(6) . ?
N6 C7 1.498(6) . ?
N6 C6 1.510(5) . ?
N8 C12 1.441(6) . ?
N8 C11 1.448(6) . ?
N8 C15 1.478(5) . ?
C10 C9 1.510(6) . ?
C5 C16 1.528(6) . ?
C5 C6 1.542(7) . ?
C13 C14 1.510(6) . ?
C14 C15 1.522(6) . ?
C17 C18 1.530(7) . ?
N10 Ni1 2.094(3) 4_575 ?
N1W C1W 1.144(6) . ?
C1W C2W 1.448(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 Ni1 N4 85.95(14) . . ?
N5 Ni1 N10 88.74(12) . 4_676 ?
N4 Ni1 N10 88.90(12) . 4_676 ?
N5 Ni1 N2 88.92(12) . . ?
N4 Ni1 N2 89.33(12) . . ?
N10 Ni1 N2 177.16(12) 4_676 . ?
N5 Ni1 N6 92.64(15) . . ?
N4 Ni1 N6 178.58(15) . . ?
N10 Ni1 N6 91.19(12) 4_676 . ?
N2 Ni1 N6 90.52(12) . . ?
N5 Ni1 N7 179.23(14) . . ?
N4 Ni1 N7 93.29(14) . . ?
N10 Ni1 N7 91.21(12) 4_676 . ?
N2 Ni1 N7 91.10(12) . . ?
N6 Ni1 N7 88.13(15) . . ?
C2 Ni2 C4 177.70(16) . . ?
C2 Ni2 C3 88.37(15) . . ?
C4 Ni2 C3 89.78(15) . . ?
C2 Ni2 C1 89.98(15) . . ?
C4 Ni2 C1 91.92(15) . . ?
C3 Ni2 C1 177.43(16) . . ?
N2 C4 Ni2 177.7(3) . . ?
N10 C2 Ni2 179.4(4) . . ?
N1 C3 Ni2 175.4(4) . . ?
N3 C1 Ni2 177.8(4) . . ?
C4 N2 Ni1 173.9(3) . . ?
C18 N7 C13 109.4(3) . . ?
C18 N7 C12 113.1(3) . . ?
C13 N7 C12 105.2(3) . . ?
C18 N7 Ni1 100.6(3) . . ?
C13 N7 Ni1 120.6(3) . . ?
C12 N7 Ni1 108.1(3) . . ?
C10 N4 C11 113.8(3) . . ?
C10 N4 Ni1 104.5(2) . . ?
C11 N4 Ni1 115.0(3) . . ?
C9 N5 C8 112.8(3) . . ?
C9 N5 Ni1 105.5(2) . . ?
C8 N5 Ni1 116.0(3) . . ?
C8 N9 C7 119.2(4) . . ?
C8 N9 C16 115.8(4) . . ?
C7 N9 C16 109.7(4) . . ?
C17 N6 C7 113.0(4) . . ?
C17 N6 C6 108.6(4) . . ?
C7 N6 C6 105.7(3) . . ?
C17 N6 Ni1 100.6(3) . . ?
C7 N6 Ni1 109.6(3) . . ?
C6 N6 Ni1 119.6(2) . . ?
C12 N8 C11 118.5(3) . . ?
C12 N8 C15 110.2(4) . . ?
C11 N8 C15 116.1(4) . . ?
N4 C10 C9 109.7(3) . . ?
N9 C7 N6 112.9(3) . . ?
N9 C8 N5 115.3(4) . . ?
C16 C5 C6 111.8(4) . . ?
N6 C6 C5 111.9(4) . . ?
N8 C12 N7 113.1(3) . . ?
N5 C9 C10 109.2(4) . . ?
N7 C13 C14 112.0(3) . . ?
N8 C11 N4 115.9(3) . . ?
C13 C14 C15 112.4(4) . . ?
N8 C15 C14 112.6(3) . . ?
N9 C16 C5 112.8(4) . . ?
N6 C17 C18 111.4(4) . . ?
N7 C18 C17 109.9(4) . . ?
C2 N10 Ni1 176.6(3) . 4_575 ?
N1W C1W C2W 178.2(6) . . ?

_refine_diff_density_max         1.127
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.153

_shelxl_version_number           2014-3



_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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 1038634'
_audit_update_record             
;
2015-01-29 deposited with the CCDC.
2015-01-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H32 N10 Ni2 O3'
_chemical_formula_weight         529.93

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'
O O 0.0106 0.0060 '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                   8.6927(17)
_cell_length_b                   9.6891(19)
_cell_length_c                   14.739(3)
_cell_angle_alpha                100.47(3)
_cell_angle_beta                 93.41(3)
_cell_angle_gamma                110.83(3)
_cell_volume                     1130.5(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_F_000             556
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_exptl_absorpt_coefficient_mu    1.705
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.606
_exptl_absorpt_correction_T_max  0.676
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11219
_diffrn_reflns_av_unetI/netI     0.0647
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.063
_diffrn_reflns_theta_max         27.446
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5139
_reflns_number_gt                3584
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0370P)²+1.7901P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5139
_refine_ls_number_parameters     283
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0462
_refine_ls_wR_factor_ref         0.1246
_refine_ls_wR_factor_gt          0.0987
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_restrained_S_all      1.094
_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 -0.03914(6) 0.68438(6) 0.27961(3) 0.03003(15) Uani 1 1 d . . . . .
Ni2 Ni 0.5000 1.0000 0.5000 0.02415(17) Uani 1 2 d S . P . .
Ni3 Ni -0.5000 0.5000 0.0000 0.02695(18) Uani 1 2 d S . P . .
N1 N 0.0918(6) 0.9506(6) 0.1904(4) 0.0797(17) Uani 1 1 d . . . . .
N2 N -0.3180(4) 0.5698(4) 0.1200(2) 0.0337(8) Uani 1 1 d . . . . .
N3 N -0.1966(5) 0.4418(5) 0.3856(3) 0.0595(12) Uani 1 1 d . . . . .
N4 N 0.2685(4) 0.8430(4) 0.4196(2) 0.0327(8) Uani 1 1 d . . . . .
N5 N -0.4280(4) 0.3217(4) -0.0417(2) 0.0319(8) Uani 1 1 d . . . . .
H1N H -0.3538 0.3304 -0.0010 0.038 Uiso 1 1 d R U . . .
N6 N -0.3150(4) 0.6210(4) -0.0755(2) 0.0308(8) Uani 1 1 d . . . . .
N7 N -0.6688(4) 0.1466(4) 0.0158(3) 0.0399(9) Uani 1 1 d . . . . .
N8 N 0.6346(4) 0.8899(4) 0.4198(2) 0.0358(8) Uani 1 1 d . . . . .
N9 N 0.5382(4) 1.1361(4) 0.4058(2) 0.0299(7) Uani 1 1 d . . . . .
H2N H 0.6210 1.2079 0.4269 0.036 Uiso 1 1 d R U . . .
N10 N 0.3430(5) 1.2503(4) 0.4724(2) 0.0402(9) Uani 1 1 d . . . . .
C1 C 0.0470(5) 0.8470(6) 0.2236(3) 0.0439(12) Uani 1 1 d . . . . .
C2 C -0.2154(5) 0.6065(5) 0.1826(3) 0.0311(9) Uani 1 1 d . . . . .
C3 C -0.1360(5) 0.5301(5) 0.3430(3) 0.0390(10) Uani 1 1 d . . . . .
C4 C 0.1480(5) 0.7753(5) 0.3692(3) 0.0299(9) Uani 1 1 d . . . . .
C5 C -0.5599(5) 0.1695(5) -0.0564(3) 0.0399(10) Uani 1 1 d . . . . .
H5A H -0.6277 0.1497 -0.1155 0.048 Uiso 1 1 calc R U . . .
H5B H -0.5078 0.0954 -0.0612 0.048 Uiso 1 1 calc R U . . .
C6 C -0.3393(6) 0.3557(5) -0.1225(3) 0.0437(11) Uani 1 1 d . . . . .
H6A H -0.4186 0.3377 -0.1766 0.052 Uiso 1 1 calc R U . . .
H6B H -0.2776 0.2903 -0.1367 0.052 Uiso 1 1 calc R U . . .
C7 C -0.2204(5) 0.5211(5) -0.0990(3) 0.0438(11) Uani 1 1 d . . . . .
H7A H -0.1382 0.5377 -0.0466 0.053 Uiso 1 1 calc R U . . .
H7B H -0.1628 0.5451 -0.1519 0.053 Uiso 1 1 calc R U . . .
C8 C -0.3748(6) 0.6682(5) -0.1577(3) 0.0404(11) Uani 1 1 d . . . . .
H8A H -0.4718 0.5873 -0.1945 0.049 Uiso 1 1 calc R U . . .
H8B H -0.2885 0.6981 -0.1970 0.049 Uiso 1 1 calc R U . . .
C9 C -0.5822(6) 0.1973(5) 0.1128(3) 0.0426(11) Uani 1 1 d . . . . .
H9A H -0.4631 0.2275 0.1131 0.051 Uiso 1 1 calc R U . . .
H9B H -0.6202 0.1165 0.1463 0.051 Uiso 1 1 calc R U . . .
C10 C -0.2167(5) 0.7749(5) -0.0164(3) 0.0409(11) Uani 1 1 d . . . . .
H10A H -0.1829 0.7684 0.0461 0.049 Uiso 1 1 calc R U . . .
H10B H -0.1186 0.8257 -0.0434 0.049 Uiso 1 1 calc R U . . .
C11 C 0.4063(6) 1.1956(5) 0.3885(3) 0.0380(10) Uani 1 1 d . . . . .
H11A H 0.4495 1.2780 0.3568 0.046 Uiso 1 1 calc R U . . .
H11B H 0.3141 1.1162 0.3470 0.046 Uiso 1 1 calc R U . . .
C12 C 0.4719(6) 1.3559(5) 0.5497(3) 0.0433(11) Uani 1 1 d . . . . .
H12A H 0.4503 1.4474 0.5704 0.052 Uiso 1 1 calc R U . . .
H12B H 0.5814 1.3831 0.5302 0.052 Uiso 1 1 calc R U . . .
C13 C 0.5405(6) 0.7323(5) 0.3714(3) 0.0399(11) Uani 1 1 d . . . . .
H13A H 0.5990 0.6990 0.3233 0.048 Uiso 1 1 calc R U . . .
H13B H 0.4312 0.7199 0.3435 0.048 Uiso 1 1 calc R U . . .
C14 C 0.7045(6) 0.9889(6) 0.3544(3) 0.0467(12) Uani 1 1 d . . . . .
H14A H 0.7318 0.9312 0.3012 0.056 Uiso 1 1 calc R U . . .
H14B H 0.8056 1.0715 0.3853 0.056 Uiso 1 1 calc R U . . .
C15 C 0.5785(6) 1.0523(5) 0.3214(3) 0.0384(10) Uani 1 1 d . . . . .
H15A H 0.6252 1.1197 0.2804 0.046 Uiso 1 1 calc R U . . .
H15B H 0.4789 0.9707 0.2876 0.046 Uiso 1 1 calc R U . . .
C16 C 0.7592(6) 0.8688(5) 0.4826(3) 0.0413(11) Uani 1 1 d . . . . .
H16A H 0.8213 0.9614 0.5282 0.050 Uiso 1 1 calc R U . . .
H16B H 0.8362 0.8361 0.4479 0.050 Uiso 1 1 calc R U . . .
O1 O 0.8067(5) 0.2032(4) 0.0414(3) 0.0675(11) Uani 1 1 d . . . . .
O2 O 0.1191(8) 0.3605(7) 0.3833(4) 0.130(2) Uani 1 1 d . . . . .
O3 O 0.9394(6) 0.1807(6) 0.2129(3) 0.0834(13) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 C1 1.853(5) . ?
Ni1 C4 1.862(4) . ?
Ni1 C2 1.867(4) . ?
Ni1 C3 1.877(5) . ?
Ni2 N9 2.046(3) 2_676 ?
Ni2 N9 2.046(3) . ?
Ni2 N8 2.121(3) 2_676 ?
Ni2 N8 2.121(4) . ?
Ni2 N4 2.157(3) 2_676 ?
Ni2 N4 2.157(3) . ?
Ni3 N5 2.045(3) . ?
Ni3 N5 2.045(3) 2_465 ?
Ni3 N6 2.132(3) . ?
Ni3 N6 2.132(3) 2_465 ?
Ni3 N2 2.136(3) 2_465 ?
Ni3 N2 2.136(3) . ?
N1 C1 1.149(6) . ?
N2 C2 1.153(5) . ?
N3 C3 1.147(6) . ?
N4 C4 1.150(5) . ?
N5 C5 1.479(5) . ?
N5 C6 1.481(5) . ?
N5 H1N 0.8241 . ?
N6 C7 1.487(6) . ?
N6 C8 1.498(5) . ?
N6 C10 1.498(5) . ?
N7 C10 1.452(6) 2_465 ?
N7 C5 1.460(6) . ?
N7 C9 1.485(5) . ?
N8 C13 1.468(5) . ?
N8 C16 1.476(5) . ?
N8 C14 1.488(6) . ?
N9 C11 1.483(5) . ?
N9 C15 1.489(5) . ?
N9 H2N 0.7988 . ?
N10 C11 1.470(6) . ?
N10 C16 1.477(6) 2_676 ?
N10 C12 1.487(5) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C7 1.528(6) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.529(7) 2_465 ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C8 1.529(7) 2_465 ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N7 1.452(6) 2_465 ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.551(6) 2_676 ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C12 1.551(6) 2_676 ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.528(7) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 N10 1.477(6) 2_676 ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?

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
C1 Ni1 C4 87.62(18) . . ?
C1 Ni1 C2 86.87(18) . . ?
C4 Ni1 C2 174.31(18) . . ?
C1 Ni1 C3 174.7(2) . . ?
C4 Ni1 C3 92.25(18) . . ?
C2 Ni1 C3 93.37(19) . . ?
N9 Ni2 N9 180.00(19) 2_676 . ?
N9 Ni2 N8 85.61(14) 2_676 2_676 ?
N9 Ni2 N8 94.39(14) . 2_676 ?
N9 Ni2 N8 94.39(14) 2_676 . ?
N9 Ni2 N8 85.61(14) . . ?
N8 Ni2 N8 180.0 2_676 . ?
N9 Ni2 N4 91.94(13) 2_676 2_676 ?
N9 Ni2 N4 88.06(13) . 2_676 ?
N8 Ni2 N4 90.96(13) 2_676 2_676 ?
N8 Ni2 N4 89.03(13) . 2_676 ?
N9 Ni2 N4 88.06(13) 2_676 . ?
N9 Ni2 N4 91.94(13) . . ?
N8 Ni2 N4 89.03(13) 2_676 . ?
N8 Ni2 N4 90.97(13) . . ?
N4 Ni2 N4 180.0 2_676 . ?
N5 Ni3 N5 180.0 . 2_465 ?
N5 Ni3 N6 86.41(13) . . ?
N5 Ni3 N6 93.59(13) 2_465 . ?
N5 Ni3 N6 93.59(13) . 2_465 ?
N5 Ni3 N6 86.41(13) 2_465 2_465 ?
N6 Ni3 N6 180.0 . 2_465 ?
N5 Ni3 N2 92.36(13) . 2_465 ?
N5 Ni3 N2 87.64(13) 2_465 2_465 ?
N6 Ni3 N2 90.23(13) . 2_465 ?
N6 Ni3 N2 89.77(13) 2_465 2_465 ?
N5 Ni3 N2 87.64(13) . . ?
N5 Ni3 N2 92.36(13) 2_465 . ?
N6 Ni3 N2 89.77(13) . . ?
N6 Ni3 N2 90.23(13) 2_465 . ?
N2 Ni3 N2 180.0 2_465 . ?
C2 N2 Ni3 177.3(3) . . ?
C4 N4 Ni2 169.9(3) . . ?
C5 N5 C6 115.7(3) . . ?
C5 N5 Ni3 115.9(3) . . ?
C6 N5 Ni3 104.9(3) . . ?
C5 N5 H1N 109.6 . . ?
C6 N5 H1N 103.6 . . ?
Ni3 N5 H1N 106.0 . . ?
C7 N6 C8 113.8(3) . . ?
C7 N6 C10 115.6(3) . . ?
C8 N6 C10 98.6(3) . . ?
C7 N6 Ni3 103.7(3) . . ?
C8 N6 Ni3 116.7(2) . . ?
C10 N6 Ni3 108.9(3) . . ?
C10 N7 C5 114.5(4) 2_465 . ?
C10 N7 C9 103.5(3) 2_465 . ?
C5 N7 C9 115.1(3) . . ?
C13 N8 C16 100.2(3) . . ?
C13 N8 C14 112.3(3) . . ?
C16 N8 C14 114.9(4) . . ?
C13 N8 Ni2 116.0(3) . . ?
C16 N8 Ni2 109.3(3) . . ?
C14 N8 Ni2 104.4(3) . . ?
C11 N9 C15 115.3(3) . . ?
C11 N9 Ni2 115.8(3) . . ?
C15 N9 Ni2 106.2(2) . . ?
C11 N9 H2N 106.5 . . ?
C15 N9 H2N 106.1 . . ?
Ni2 N9 H2N 106.3 . . ?
C11 N10 C16 115.1(3) . 2_676 ?
C11 N10 C12 115.5(4) . . ?
C16 N10 C12 103.3(3) 2_676 . ?
N1 C1 Ni1 175.5(5) . . ?
N2 C2 Ni1 174.0(4) . . ?
N3 C3 Ni1 176.2(5) . . ?
N4 C4 Ni1 173.0(4) . . ?
N7 C5 N5 115.5(3) . . ?
N7 C5 H5A 108.4 . . ?
N5 C5 H5A 108.4 . . ?
N7 C5 H5B 108.4 . . ?
N5 C5 H5B 108.4 . . ?
H5A C5 H5B 107.5 . . ?
N5 C6 C7 109.0(4) . . ?
N5 C6 H6A 109.9 . . ?
C7 C6 H6A 109.9 . . ?
N5 C6 H6B 109.9 . . ?
C7 C6 H6B 109.9 . . ?
H6A C6 H6B 108.3 . . ?
N6 C7 C6 109.8(3) . . ?
N6 C7 H7A 109.7 . . ?
C6 C7 H7A 109.7 . . ?
N6 C7 H7B 109.7 . . ?
C6 C7 H7B 109.7 . . ?
H7A C7 H7B 108.2 . . ?
N6 C8 C9 103.0(3) . 2_465 ?
N6 C8 H8A 111.2 . . ?
C9 C8 H8A 111.2 2_465 . ?
N6 C8 H8B 111.2 . . ?
C9 C8 H8B 111.2 2_465 . ?
H8A C8 H8B 109.1 . . ?
N7 C9 C8 106.0(4) . 2_465 ?
N7 C9 H9A 110.5 . . ?
C8 C9 H9A 110.5 2_465 . ?
N7 C9 H9B 110.5 . . ?
C8 C9 H9B 110.5 2_465 . ?
H9A C9 H9B 108.7 . . ?
N7 C10 N6 103.7(3) 2_465 . ?
N7 C10 H10A 111.0 2_465 . ?
N6 C10 H10A 111.0 . . ?
N7 C10 H10B 111.0 2_465 . ?
N6 C10 H10B 111.0 . . ?
H10A C10 H10B 109.0 . . ?
N10 C11 N9 115.0(3) . . ?
N10 C11 H11A 108.5 . . ?
N9 C11 H11A 108.5 . . ?
N10 C11 H11B 108.5 . . ?
N9 C11 H11B 108.5 . . ?
H11A C11 H11B 107.5 . . ?
N10 C12 C13 105.1(4) . 2_676 ?
N10 C12 H12A 110.7 . . ?
C13 C12 H12A 110.7 2_676 . ?
N10 C12 H12B 110.7 . . ?
C13 C12 H12B 110.7 2_676 . ?
H12A C12 H12B 108.8 . . ?
N8 C13 C12 103.1(3) . 2_676 ?
N8 C13 H13A 111.1 . . ?
C12 C13 H13A 111.1 2_676 . ?
N8 C13 H13B 111.1 . . ?
C12 C13 H13B 111.1 2_676 . ?
H13A C13 H13B 109.1 . . ?
N8 C14 C15 110.1(4) . . ?
N8 C14 H14A 109.6 . . ?
C15 C14 H14A 109.6 . . ?
N8 C14 H14B 109.6 . . ?
C15 C14 H14B 109.6 . . ?
H14A C14 H14B 108.2 . . ?
N9 C15 C14 107.2(3) . . ?
N9 C15 H15A 110.3 . . ?
C14 C15 H15A 110.3 . . ?
N9 C15 H15B 110.3 . . ?
C14 C15 H15B 110.3 . . ?
H15A C15 H15B 108.5 . . ?
N8 C16 N10 103.0(3) . 2_676 ?
N8 C16 H16A 111.2 . . ?
N10 C16 H16A 111.2 2_676 . ?
N8 C16 H16B 111.2 . . ?
N10 C16 H16B 111.2 2_676 . ?
H16A C16 H16B 109.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10 N7 C5 N5 71.6(5) 2_465 . . . ?
C9 N7 C5 N5 -48.3(5) . . . . ?
C6 N5 C5 N7 -168.2(4) . . . . ?
Ni3 N5 C5 N7 -44.8(5) . . . . ?
C5 N5 C6 C7 174.4(4) . . . . ?
Ni3 N5 C6 C7 45.4(4) . . . . ?
C8 N6 C7 C6 -90.0(4) . . . . ?
C10 N6 C7 C6 156.8(4) . . . . ?
Ni3 N6 C7 C6 37.8(4) . . . . ?
N5 C6 C7 N6 -58.5(5) . . . . ?
C7 N6 C8 C9 -163.4(3) . . . 2_465 ?
C10 N6 C8 C9 -40.5(4) . . . 2_465 ?
Ni3 N6 C8 C9 75.8(4) . . . 2_465 ?
C10 N7 C9 C8 -13.0(4) 2_465 . . 2_465 ?
C5 N7 C9 C8 112.8(4) . . . 2_465 ?
C7 N6 C10 N7 172.2(4) . . . 2_465 ?
C8 N6 C10 N7 50.5(4) . . . 2_465 ?
Ni3 N6 C10 N7 -71.7(3) . . . 2_465 ?
C16 N10 C11 N9 -70.9(5) 2_676 . . . ?
C12 N10 C11 N9 49.3(5) . . . . ?
C15 N9 C11 N10 168.1(3) . . . . ?
Ni2 N9 C11 N10 43.2(4) . . . . ?
C11 N10 C12 C13 -112.7(4) . . . 2_676 ?
C16 N10 C12 C13 13.8(4) 2_676 . . 2_676 ?
C16 N8 C13 C12 40.6(4) . . . 2_676 ?
C14 N8 C13 C12 163.0(4) . . . 2_676 ?
Ni2 N8 C13 C12 -77.0(4) . . . 2_676 ?
C13 N8 C14 C15 88.3(4) . . . . ?
C16 N8 C14 C15 -158.0(4) . . . . ?
Ni2 N8 C14 C15 -38.2(4) . . . . ?
C11 N9 C15 C14 -175.1(4) . . . . ?
Ni2 N9 C15 C14 -45.4(4) . . . . ?
N8 C14 C15 N9 57.9(5) . . . . ?
C13 N8 C16 N10 -50.9(4) . . . 2_676 ?
C14 N8 C16 N10 -171.4(3) . . . 2_676 ?
Ni2 N8 C16 N10 71.6(3) . . . 2_676 ?

_refine_diff_density_max         0.774
_refine_diff_density_min         -1.065
_refine_diff_density_rms         0.117

_shelxl_version_number           2014-3



