# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_complex_1
_database_code_depnum_ccdc_archive 'CCDC 985705'
_audit_update_record             
;
2016-04-29 deposited with the CCDC.
2016-05-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H44 Cl2 N8 Ni O2'
_chemical_formula_weight         630.30

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   10.8400(7)
_cell_length_b                   11.2885(10)
_cell_length_c                   14.2205(7)
_cell_angle_alpha                85.293(5)
_cell_angle_beta                 77.072(5)
_cell_angle_gamma                73.587(7)
_cell_volume                     1626.57(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4695
_cell_measurement_theta_min      3.4670
_cell_measurement_theta_max      28.4230

_exptl_crystal_description       cube
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             668
_exptl_absorpt_coefficient_mu    0.796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.37736
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'face installed'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11016
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_sigmaI/netI    0.0826
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.00
_diffrn_reflns_theta_max         25.50
_reflns_number_total             6030
_reflns_number_gt                4214
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1400P)²+0.0800P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6030
_refine_ls_number_parameters     390
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_gt           0.0655
_refine_ls_wR_factor_ref         0.2249
_refine_ls_wR_factor_gt          0.1797
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni2 Ni 1.0000 1.0000 0.5000 0.0341(2) Uani 1 2 d S . .
Ni1 Ni 1.0000 0.5000 1.0000 0.0334(2) Uani 1 2 d S . .
Cl1 Cl 0.66454(12) 0.15941(15) 0.98451(9) 0.0706(4) Uani 1 1 d . . .
Cl2 Cl 0.5173(2) 0.65470(19) 0.61925(11) 0.1008(7) Uani 1 1 d . . .
N1 N 0.8296(3) 0.5679(3) 0.9742(2) 0.0368(8) Uani 1 1 d . . .
N7 N 1.0491(3) 0.9634(3) 0.3667(2) 0.0396(8) Uani 1 1 d . . .
N5 N 0.8644(3) 0.9220(3) 0.5084(2) 0.0399(8) Uani 1 1 d . . .
N6 N 0.7212(4) 0.8150(4) 0.5436(3) 0.0503(10) Uani 1 1 d . . .
N3 N 1.0572(3) 0.4651(3) 0.8671(2) 0.0392(8) Uani 1 1 d . . .
N2 N 0.6294(4) 0.6723(4) 0.9689(3) 0.0453(9) Uani 1 1 d . . .
N4 N 1.1477(4) 0.4559(4) 0.7146(3) 0.0460(9) Uani 1 1 d D . .
N8 N 1.1450(4) 0.9153(4) 0.2188(3) 0.0470(10) Uani 1 1 d . . .
O1 O 0.3197(6) 0.5178(7) 0.5562(3) 0.127(2) Uani 1 1 d G . .
H1OB H 0.3252 0.5918 0.5507 0.190 Uiso 1 1 d G . .
H1OA H 0.3547 0.4818 0.5027 0.190 Uiso 1 1 d G . .
C21 C 0.9540(4) 0.9923(4) 0.3106(3) 0.0375(9) Uani 1 1 d . . .
C4 C 0.6525(4) 0.5649(4) 0.9203(3) 0.0415(10) Uani 1 1 d . . .
C17 C 0.6938(4) 0.8855(4) 0.4633(3) 0.0453(11) Uani 1 1 d . . .
C20 C 0.8118(4) 1.0391(4) 0.3587(3) 0.0418(10) Uani 1 1 d . . .
H20A H 0.7563 1.0421 0.3132 0.050 Uiso 1 1 calc R . .
H20B H 0.7943 1.1217 0.3823 0.050 Uiso 1 1 calc R . .
C19 C 0.7834(4) 0.9517(4) 0.4416(3) 0.0414(10) Uani 1 1 d . . .
C3 C 0.7376(4) 0.6733(4) 1.0007(3) 0.0410(10) Uani 1 1 d . . .
C7 C 0.8629(4) 0.3842(4) 0.8754(3) 0.0417(10) Uani 1 1 d . . .
H7A H 0.8188 0.3572 0.8323 0.050 Uiso 1 1 calc R . .
H7B H 0.8823 0.3194 0.9234 0.050 Uiso 1 1 calc R . .
C6 C 0.7771(4) 0.5004(4) 0.9232(3) 0.0387(10) Uani 1 1 d . . .
C11 C 1.1527(4) 0.4926(4) 0.7997(3) 0.0411(10) Uani 1 1 d . . .
C22 C 1.0134(4) 0.9637(4) 0.2184(3) 0.0394(10) Uani 1 1 d . . .
C8 C 0.9878(4) 0.4101(4) 0.8195(3) 0.0381(9) Uani 1 1 d . . .
O2 O 0.5639(7) 0.1202(6) 0.2229(5) 0.1128(17) Uani 1 1 d D . .
C12 C 1.2460(4) 0.5600(5) 0.8144(3) 0.0510(12) Uani 1 1 d . . .
H12A H 1.3167 0.5519 0.7578 0.061 Uiso 1 1 calc R . .
H12B H 1.2842 0.5235 0.8691 0.061 Uiso 1 1 calc R . .
C24 C 1.1657(4) 0.9149(4) 0.3076(3) 0.0430(10) Uani 1 1 d . . .
C5 C 0.5521(4) 0.5379(5) 0.8745(3) 0.0553(13) Uani 1 1 d . . .
H5A H 0.5574 0.5748 0.8109 0.083 Uiso 1 1 calc R . .
H5B H 0.4658 0.5715 0.9129 0.083 Uiso 1 1 calc R . .
H5C H 0.5686 0.4502 0.8702 0.083 Uiso 1 1 calc R . .
C9 C 1.0441(4) 0.4039(4) 0.7249(3) 0.0448(11) Uani 1 1 d . . .
C23 C 0.9599(5) 0.9743(5) 0.1291(3) 0.0593(13) Uani 1 1 d . . .
H23A H 0.8678 1.0167 0.1433 0.089 Uiso 1 1 calc R . .
H23B H 0.9718 0.8932 0.1064 0.089 Uiso 1 1 calc R . .
H23C H 1.0055 1.0197 0.0803 0.089 Uiso 1 1 calc R . .
C2 C 0.7490(5) 0.7800(5) 1.0488(4) 0.0588(13) Uani 1 1 d . . .
H2A H 0.7380 0.8510 1.0051 0.071 Uiso 1 1 calc R . .
H2B H 0.8370 0.7614 1.0613 0.071 Uiso 1 1 calc R . .
C16 C 0.8248(4) 0.8364(5) 0.5695(3) 0.0461(11) Uani 1 1 d . . .
C25 C 1.2950(4) 0.8646(5) 0.3342(4) 0.0564(13) Uani 1 1 d . . .
H25A H 1.3574 0.9036 0.2932 0.068 Uiso 1 1 calc R . .
H25B H 1.2872 0.8864 0.4003 0.068 Uiso 1 1 calc R . .
C18 C 0.5879(5) 0.8769(6) 0.4142(4) 0.0605(14) Uani 1 1 d . . .
H18A H 0.5694 0.9467 0.3712 0.091 Uiso 1 1 calc R . .
H18B H 0.5098 0.8763 0.4618 0.091 Uiso 1 1 calc R . .
H18C H 0.6168 0.8022 0.3781 0.091 Uiso 1 1 calc R . .
C10 C 1.0101(5) 0.3565(6) 0.6404(4) 0.0644(15) Uani 1 1 d . . .
H10A H 0.9818 0.2833 0.6599 0.097 Uiso 1 1 calc R . .
H10B H 1.0862 0.3376 0.5887 0.097 Uiso 1 1 calc R . .
H10C H 0.9406 0.4186 0.6189 0.097 Uiso 1 1 calc R . .
C15 C 0.8877(6) 0.7690(6) 0.6486(4) 0.0739(18) Uani 1 1 d . . .
H15A H 0.9533 0.6956 0.6211 0.089 Uiso 1 1 calc R . .
H15B H 0.9344 0.8210 0.6685 0.089 Uiso 1 1 calc R . .
C13 C 1.1771(7) 0.6971(6) 0.8326(5) 0.089(2) Uani 1 1 d . . .
H13A H 1.1363 0.7325 0.7797 0.133 Uiso 1 1 calc R . .
H13B H 1.2406 0.7392 0.8383 0.133 Uiso 1 1 calc R . .
H13C H 1.1113 0.7055 0.8913 0.133 Uiso 1 1 calc R . .
C1 C 0.6521(8) 0.8134(8) 1.1412(6) 0.120(3) Uani 1 1 d . . .
H1A H 0.5646 0.8327 1.1296 0.179 Uiso 1 1 calc R . .
H1B H 0.6644 0.8839 1.1674 0.179 Uiso 1 1 calc R . .
H1C H 0.6648 0.7450 1.1861 0.179 Uiso 1 1 calc R . .
C26 C 1.3465(10) 0.7335(9) 0.3260(10) 0.188(6) Uani 1 1 d . . .
H26A H 1.2765 0.6974 0.3251 0.282 Uiso 1 1 calc R . .
H26B H 1.3859 0.7005 0.3800 0.282 Uiso 1 1 calc R . .
H26C H 1.4116 0.7147 0.2672 0.282 Uiso 1 1 calc R . .
C14 C 0.8115(9) 0.7323(11) 0.7309(6) 0.168(5) Uani 1 1 d . . .
H14A H 0.7552 0.8038 0.7657 0.252 Uiso 1 1 calc R . .
H14B H 0.8675 0.6819 0.7709 0.252 Uiso 1 1 calc R . .
H14C H 0.7589 0.6855 0.7132 0.252 Uiso 1 1 calc R . .
H2N H 0.559(4) 0.728(4) 0.979(3) 0.039(12) Uiso 1 1 d . . .
H4N H 1.194(4) 0.465(5) 0.660(2) 0.065(16) Uiso 1 1 d D . .
H6N H 0.670(5) 0.775(5) 0.570(3) 0.052(14) Uiso 1 1 d . . .
H8N H 1.192(4) 0.899(3) 0.171(3) 0.019(10) Uiso 1 1 d . . .
H2OA H 0.583(12) 0.176(9) 0.253(7) 0.22(6) Uiso 1 1 d D . .
H3OA H 0.534(9) 0.141(9) 0.169(4) 0.14(4) 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
Ni2 N5 1.894(3) 2_776 ?
Ni2 N5 1.894(3) . ?
Ni2 N7 1.897(3) . ?
Ni2 N7 1.897(3) 2_776 ?
Ni1 N3 1.890(3) 2_767 ?
Ni1 N3 1.890(3) . ?
Ni1 N1 1.895(3) 2_767 ?
Ni1 N1 1.895(3) . ?
N1 C3 1.337(5) . ?
N1 C6 1.397(5) . ?
N7 C24 1.346(5) . ?
N7 C21 1.394(5) . ?
N5 C16 1.343(5) . ?
N5 C19 1.393(5) . ?
N6 C16 1.345(5) . ?
N6 C17 1.376(6) . ?
N3 C11 1.333(5) . ?
N3 C8 1.404(5) . ?
N2 C3 1.351(5) . ?
N2 C4 1.378(6) . ?
N4 C11 1.328(5) . ?
N4 C9 1.384(5) . ?
N8 C24 1.332(6) . ?
N8 C22 1.376(6) . ?
C21 C22 1.346(5) . ?
C21 C20 1.500(6) . ?
C4 C6 1.350(6) . ?
C4 C5 1.497(5) . ?
C17 C19 1.355(5) . ?
C17 C18 1.499(6) . ?
C20 C19 1.508(6) . ?
C3 C2 1.481(6) . ?
C7 C6 1.490(6) . ?
C7 C8 1.502(5) . ?
C11 C12 1.483(5) . ?
C22 C23 1.494(6) . ?
C8 C9 1.345(6) . ?
C12 C13 1.531(8) . ?
C24 C25 1.477(7) . ?
C9 C10 1.510(6) . ?
C2 C1 1.487(8) . ?
C16 C15 1.489(7) . ?
C25 C26 1.430(10) . ?
C15 C14 1.380(8) . ?

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 Ni2 N5 179.999(1) 2_776 . ?
N5 Ni2 N7 92.62(13) 2_776 . ?
N5 Ni2 N7 87.38(13) . . ?
N5 Ni2 N7 87.39(13) 2_776 2_776 ?
N5 Ni2 N7 92.61(13) . 2_776 ?
N7 Ni2 N7 180.0(2) . 2_776 ?
N3 Ni1 N3 180.00(7) 2_767 . ?
N3 Ni1 N1 86.64(13) 2_767 2_767 ?
N3 Ni1 N1 93.36(13) . 2_767 ?
N3 Ni1 N1 93.36(13) 2_767 . ?
N3 Ni1 N1 86.64(13) . . ?
N1 Ni1 N1 180.0(2) 2_767 . ?
C3 N1 C6 107.7(3) . . ?
C3 N1 Ni1 132.0(3) . . ?
C6 N1 Ni1 120.2(3) . . ?
C24 N7 C21 107.1(3) . . ?
C24 N7 Ni2 132.9(3) . . ?
C21 N7 Ni2 119.9(3) . . ?
C16 N5 C19 107.2(3) . . ?
C16 N5 Ni2 132.7(3) . . ?
C19 N5 Ni2 120.1(3) . . ?
C16 N6 C17 110.2(4) . . ?
C11 N3 C8 106.6(3) . . ?
C11 N3 Ni1 131.9(3) . . ?
C8 N3 Ni1 121.2(3) . . ?
C3 N2 C4 109.9(4) . . ?
C11 N4 C9 109.8(3) . . ?
C24 N8 C22 110.4(4) . . ?
C22 C21 N7 108.8(4) . . ?
C22 C21 C20 131.9(4) . . ?
N7 C21 C20 119.2(3) . . ?
C6 C4 N2 105.9(3) . . ?
C6 C4 C5 131.4(4) . . ?
N2 C4 C5 122.6(4) . . ?
C19 C17 N6 105.5(4) . . ?
C19 C17 C18 131.8(4) . . ?
N6 C17 C18 122.7(4) . . ?
C21 C20 C19 107.7(4) . . ?
C17 C19 N5 109.0(4) . . ?
C17 C19 C20 131.8(4) . . ?
N5 C19 C20 119.1(3) . . ?
N1 C3 N2 107.8(4) . . ?
N1 C3 C2 128.4(4) . . ?
N2 C3 C2 123.5(4) . . ?
C6 C7 C8 107.9(3) . . ?
C4 C6 N1 108.6(4) . . ?
C4 C6 C7 131.4(4) . . ?
N1 C6 C7 119.7(3) . . ?
N4 C11 N3 109.2(3) . . ?
N4 C11 C12 124.4(4) . . ?
N3 C11 C12 126.3(4) . . ?
C21 C22 N8 105.7(4) . . ?
C21 C22 C23 131.6(4) . . ?
N8 C22 C23 122.7(4) . . ?
C9 C8 N3 108.8(3) . . ?
C9 C8 C7 132.1(4) . . ?
N3 C8 C7 118.6(3) . . ?
C11 C12 C13 111.3(4) . . ?
N8 C24 N7 108.0(4) . . ?
N8 C24 C25 124.4(4) . . ?
N7 C24 C25 127.5(4) . . ?
C8 C9 N4 105.5(4) . . ?
C8 C9 C10 131.9(4) . . ?
N4 C9 C10 122.5(4) . . ?
C3 C2 C1 114.2(5) . . ?
N5 C16 N6 108.1(4) . . ?
N5 C16 C15 127.1(4) . . ?
N6 C16 C15 124.7(4) . . ?
C26 C25 C24 114.4(5) . . ?
C14 C15 C16 119.9(6) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.153
_refine_diff_density_min         -1.075
_refine_diff_density_rms         0.107

####################################################################### 
# 
# 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_complex_2
_database_code_depnum_ccdc_archive 'CCDC 1456771'
_audit_update_record             
;
2016-04-29 deposited with the CCDC.
2016-05-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H44 Cl N9 Ni O4'
_chemical_formula_weight         640.86

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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           monoclinic
_symmetry_space_group_name_H-M   'P 2/c'

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

_cell_length_a                   9.4536(3)
_cell_length_b                   9.3089(3)
_cell_length_c                   18.4419(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.025(2)
_cell_angle_gamma                90.00
_cell_volume                     1622.68(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1602
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      25.81

_exptl_crystal_description       cube
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             680
_exptl_absorpt_coefficient_mu    0.725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.682
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'face installed'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18479
_diffrn_reflns_av_R_equivalents  0.0658
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.15
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2828
_reflns_number_gt                2406
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0102P)²+10.0043P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2828
_refine_ls_number_parameters     197
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0599
_refine_ls_wR_factor_ref         0.1596
_refine_ls_wR_factor_gt          0.1572
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 1.0000 0.67819(10) 0.7500 0.0291(3) Uani 1 2 d S . .
O1 O 1.1047(4) 0.4690(4) 0.7706(2) 0.0437(9) Uani 1 1 d . . .
N1 N 1.0755(4) 0.6612(4) 0.6453(2) 0.0312(9) Uani 1 1 d . . .
N2 N 1.2057(5) 0.6527(5) 0.5487(2) 0.0414(11) Uani 1 1 d . . .
H2 H 1.2791 0.6443 0.5221 0.050 Uiso 1 1 d R . .
N3 N 0.8544(4) 0.8302(4) 0.7132(2) 0.0321(9) Uani 1 1 d . . .
N4 N 0.7371(5) 1.0292(5) 0.6911(2) 0.0398(11) Uani 1 1 d . . .
H4 H 0.6999 1.1123 0.6977 0.048 Uiso 1 1 d R . .
N9 N 1.0000 0.3932(7) 0.7500 0.0499(17) Uani 1 2 d S . .
C1 C 1.4586(7) 0.7068(8) 0.6521(4) 0.0646(19) Uani 1 1 d . . .
H1A H 1.4761 0.7090 0.6010 0.097 Uiso 1 1 calc R . .
H1B H 1.5409 0.6713 0.6775 0.097 Uiso 1 1 calc R . .
H1C H 1.4377 0.8021 0.6687 0.097 Uiso 1 1 calc R . .
C2 C 1.3336(5) 0.6089(6) 0.6666(3) 0.0432(13) Uani 1 1 d . . .
H2A H 1.3076 0.6095 0.7158 0.052 Uiso 1 1 d R . .
H2B H 1.3591 0.5083 0.6540 0.052 Uiso 1 1 d R . .
C3 C 1.2055(5) 0.6420(6) 0.6213(3) 0.0351(12) Uani 1 1 d . . .
C4 C 1.0705(6) 0.6794(6) 0.5236(3) 0.0384(12) Uani 1 1 d . . .
C5 C 1.0355(7) 0.6981(7) 0.4449(3) 0.0560(17) Uani 1 1 d . . .
H5A H 1.0466 0.7892 0.4306 0.067 Uiso 1 1 d R . .
H5B H 0.9267 0.7123 0.4397 0.067 Uiso 1 1 d R . .
H5C H 1.0551 0.6176 0.4162 0.067 Uiso 1 1 d R . .
C6 C 0.9902(5) 0.6833(5) 0.5840(3) 0.0328(11) Uani 1 1 d . . .
C7 C 0.8338(5) 0.7058(6) 0.5920(3) 0.0367(12) Uani 1 1 d . . .
H7A H 0.7910 0.7245 0.5447 0.044 Uiso 1 1 calc R . .
H7B H 0.7916 0.6191 0.6112 0.044 Uiso 1 1 calc R . .
C8 C 0.8042(5) 0.8287(5) 0.6414(3) 0.0312(11) Uani 1 1 d . . .
C9 C 0.7320(5) 0.9512(6) 0.6275(3) 0.0371(12) Uani 1 1 d . . .
C10 C 0.6556(7) 1.0030(7) 0.5606(3) 0.0551(16) Uani 1 1 d . . .
H10A H 0.7209 1.0520 0.5299 0.083 Uiso 1 1 calc R . .
H10B H 0.5815 1.0678 0.5740 0.083 Uiso 1 1 calc R . .
H10C H 0.6155 0.9225 0.5350 0.083 Uiso 1 1 calc R . .
C11 C 0.8115(5) 0.9532(6) 0.7415(3) 0.0359(12) Uani 1 1 d . . .
C12 C 0.8429(7) 1.0106(7) 0.8159(3) 0.0502(15) Uani 1 1 d . . .
H12A H 0.8617 0.9359 0.8481 0.060 Uiso 1 1 d R . .
H12B H 0.9329 1.0690 0.8122 0.060 Uiso 1 1 d R . .
C13 C 0.7309(8) 1.1037(9) 0.8475(4) 0.076(2) Uani 1 1 d . . .
H13A H 0.7196 1.1887 0.8185 0.114 Uiso 1 1 calc R . .
H13B H 0.7580 1.1303 0.8961 0.114 Uiso 1 1 calc R . .
H13C H 0.6430 1.0520 0.8482 0.114 Uiso 1 1 calc R . .
Cl1 Cl 0.4808(3) 0.3637(3) 0.95614(14) 0.0461(7) Uani 0.50 1 d P . .
O4 O 0.6196(5) 0.3223(5) 0.7008(2) 0.0533(11) Uani 1 1 d GD . .
H4A H 0.6899 0.3730 0.7147 0.080 Uiso 1 1 d G . .
H4B H 0.6000 0.3407 0.6566 0.080 Uiso 1 1 d GD . .


_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 2.077(4) . ?
Ni1 N1 2.077(4) 2_756 ?
Ni1 N3 2.079(4) 2_756 ?
Ni1 N3 2.079(4) . ?
Ni1 O1 2.214(4) . ?
Ni1 O1 2.214(4) 2_756 ?
O1 N9 1.268(5) . ?
N1 C3 1.326(6) . ?
N1 C6 1.393(6) . ?
N2 C3 1.343(6) . ?
N2 C4 1.375(7) . ?
N2 H2 0.8601 . ?
N3 C11 1.325(6) . ?
N3 C8 1.399(6) . ?
N4 C11 1.356(6) . ?
N4 C9 1.378(7) . ?
N4 H4 0.8594 . ?
N9 O1 1.268(5) 2_756 ?
C1 C2 1.520(8) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.491(7) . ?
C2 H2A 0.9449 . ?
C2 H2B 0.9957 . ?
C4 C6 1.359(7) . ?
C4 C5 1.493(7) . ?
C5 H5A 0.8952 . ?
C5 H5B 1.0402 . ?
C5 H5C 0.9379 . ?
C6 C7 1.503(7) . ?
C7 C8 1.492(7) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.352(7) . ?
C9 C10 1.499(7) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.497(7) . ?
C12 C13 1.495(8) . ?
C12 H12A 0.9287 . ?
C12 H12B 1.0132 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
O4 H4A 0.8500 . ?
O4 H4B 0.8499 . ?

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 171.3(2) . 2_756 ?
N1 Ni1 N3 96.80(16) . 2_756 ?
N1 Ni1 N3 89.15(16) 2_756 2_756 ?
N1 Ni1 N3 89.15(16) . . ?
N1 Ni1 N3 96.79(16) 2_756 . ?
N3 Ni1 N3 94.2(2) 2_756 . ?
N1 Ni1 O1 86.12(15) . . ?
N1 Ni1 O1 86.21(15) 2_756 . ?
N3 Ni1 O1 104.56(15) 2_756 . ?
N3 Ni1 O1 161.02(15) . . ?
N1 Ni1 O1 86.21(15) . 2_756 ?
N1 Ni1 O1 86.12(15) 2_756 2_756 ?
N3 Ni1 O1 161.02(15) 2_756 2_756 ?
N3 Ni1 O1 104.56(15) . 2_756 ?
O1 Ni1 O1 56.8(2) . 2_756 ?
N9 O1 Ni1 95.4(3) . . ?
C3 N1 C6 106.0(4) . . ?
C3 N1 Ni1 131.0(3) . . ?
C6 N1 Ni1 122.7(3) . . ?
C3 N2 C4 109.4(4) . . ?
C3 N2 H2 125.3 . . ?
C4 N2 H2 125.3 . . ?
C11 N3 C8 106.3(4) . . ?
C11 N3 Ni1 131.7(3) . . ?
C8 N3 Ni1 120.9(3) . . ?
C11 N4 C9 108.6(4) . . ?
C11 N4 H4 125.5 . . ?
C9 N4 H4 125.9 . . ?
O1 N9 O1 112.4(6) 2_756 . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 C1 113.8(5) . . ?
C3 C2 H2A 108.3 . . ?
C1 C2 H2A 112.5 . . ?
C3 C2 H2B 105.1 . . ?
C1 C2 H2B 109.3 . . ?
H2A C2 H2B 107.4 . . ?
N1 C3 N2 109.9(4) . . ?
N1 C3 C2 126.2(5) . . ?
N2 C3 C2 123.9(5) . . ?
C6 C4 N2 105.0(4) . . ?
C6 C4 C5 132.5(5) . . ?
N2 C4 C5 122.5(5) . . ?
C4 C5 H5A 111.9 . . ?
C4 C5 H5B 107.9 . . ?
H5A C5 H5B 88.4 . . ?
C4 C5 H5C 114.5 . . ?
H5A C5 H5C 124.4 . . ?
H5B C5 H5C 104.7 . . ?
C4 C6 N1 109.7(4) . . ?
C4 C6 C7 130.5(5) . . ?
N1 C6 C7 119.8(4) . . ?
C8 C7 C6 111.2(4) . . ?
C8 C7 H7A 109.4 . . ?
C6 C7 H7A 109.4 . . ?
C8 C7 H7B 109.4 . . ?
C6 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
C9 C8 N3 109.4(4) . . ?
C9 C8 C7 129.1(5) . . ?
N3 C8 C7 121.5(4) . . ?
C8 C9 N4 105.9(4) . . ?
C8 C9 C10 131.5(5) . . ?
N4 C9 C10 122.6(5) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C11 N4 109.8(4) . . ?
N3 C11 C12 127.8(5) . . ?
N4 C11 C12 122.3(5) . . ?
C13 C12 C11 115.7(5) . . ?
C13 C12 H12A 108.4 . . ?
C11 C12 H12A 110.5 . . ?
C13 C12 H12B 108.5 . . ?
C11 C12 H12B 106.3 . . ?
H12A C12 H12B 107.1 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
H4A O4 H4B 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.500
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.111

####################################################################### 
# 
# 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_complex_3
_database_code_depnum_ccdc_archive 'CCDC 1456772'
_audit_update_record             
;
2016-04-29 deposited with the CCDC.
2016-05-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H80 Cl2 N18 Ni2 O7'
_chemical_formula_weight         1257.66

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'
Cl Cl 0.1484 0.1585 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21'

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

_cell_length_a                   9.7243(4)
_cell_length_b                   33.0698(17)
_cell_length_c                   9.7619(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.492(3)
_cell_angle_gamma                90.00
_cell_volume                     3112.4(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7503
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      26.26

_exptl_crystal_description       block
_exptl_crystal_colour            deep-blue
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1328
_exptl_absorpt_coefficient_mu    0.753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7645
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'face installed'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26834
_diffrn_reflns_av_R_equivalents  0.0824
_diffrn_reflns_av_sigmaI/netI    0.0873
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.10
_diffrn_reflns_theta_max         25.00
_reflns_number_total             9833
_reflns_number_gt                6257
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0750P)²+8.5000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.11(3)
_refine_ls_number_reflns         9833
_refine_ls_number_parameters     746
_refine_ls_number_restraints     27
_refine_ls_R_factor_all          0.1297
_refine_ls_R_factor_gt           0.0760
_refine_ls_wR_factor_ref         0.2342
_refine_ls_wR_factor_gt          0.1873
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_restrained_S_all      1.182
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni2 Ni 0.63555(13) 0.16573(4) 0.10814(14) 0.0446(4) Uani 1 1 d . . .
O6 O 0.6646(17) 0.0940(5) 0.4174(17) 0.158(7) Uani 1 1 d U . .
O4 O 0.5511(10) 0.1398(3) 0.2903(9) 0.066(2) Uani 1 1 d . . .
O5 O 0.7465(9) 0.1200(3) 0.2377(11) 0.071(3) Uani 1 1 d . . .
N14 N 0.5360(9) 0.1188(3) -0.0032(10) 0.049(2) Uani 1 1 d . . .
N15 N 0.3829(11) 0.0778(3) -0.1138(11) 0.063(3) Uani 1 1 d . . .
H15 H 0.3047 0.0664 -0.1408 0.076 Uiso 1 1 calc R . .
N12 N 0.4927(9) 0.2088(3) 0.0262(9) 0.048(2) Uani 1 1 d . . .
N13 N 0.3407(11) 0.2459(3) -0.1080(10) 0.047(3) Uani 1 1 d . . .
H13 H 0.2891 0.2548 -0.1798 0.057 Uiso 1 1 calc R . .
N10 N 0.7210(9) 0.2076(3) 0.2486(10) 0.051(3) Uani 1 1 d . . .
N11 N 0.8478(10) 0.2441(4) 0.3935(11) 0.055(3) Uani 1 1 d . . .
H11 H 0.9201 0.2530 0.4447 0.066 Uiso 1 1 calc R . .
N16 N 0.7683(9) 0.1724(3) -0.0386(10) 0.049(2) Uani 1 1 d . . .
N17 N 0.8785(10) 0.1961(3) -0.2023(11) 0.058(3) Uani 1 1 d . . .
H17 H 0.9169 0.2128 -0.2533 0.070 Uiso 1 1 calc R . .
N18 N 0.6543(16) 0.1168(4) 0.3138(13) 0.077(4) Uani 1 1 d U . .
C40 C 0.847(2) 0.2837(5) -0.108(2) 0.108(6) Uani 1 1 d . . .
H40A H 0.9431 0.2825 -0.1211 0.162 Uiso 1 1 calc R . .
H40B H 0.8307 0.3074 -0.0560 0.162 Uiso 1 1 calc R . .
H40C H 0.7908 0.2848 -0.1967 0.162 Uiso 1 1 calc R . .
C41 C 0.8111(18) 0.2480(4) -0.0345(18) 0.084(5) Uani 1 1 d . . .
H41A H 0.7155 0.2515 -0.0182 0.101 Uiso 1 1 calc R . .
H41B H 0.8669 0.2489 0.0554 0.101 Uiso 1 1 calc R . .
C42 C 0.8223(12) 0.2065(4) -0.0866(13) 0.061(3) Uani 1 1 d . . .
C43 C 0.8657(12) 0.1557(4) -0.2262(12) 0.059(3) Uani 1 1 d . . .
C44 C 0.9200(15) 0.1366(4) -0.3457(16) 0.081(4) Uani 1 1 d . . .
H44A H 0.9030 0.1080 -0.3448 0.121 Uiso 1 1 calc R . .
H44B H 1.0179 0.1414 -0.3397 0.121 Uiso 1 1 calc R . .
H44C H 0.8741 0.1480 -0.4299 0.121 Uiso 1 1 calc R . .
C45 C 0.7934(13) 0.1401(4) -0.1296(15) 0.064(4) Uani 1 1 d . . .
C46 C 0.7532(11) 0.0987(4) -0.1009(15) 0.057(3) Uani 1 1 d . . .
H46A H 0.8056 0.0900 -0.0146 0.068 Uiso 1 1 calc R . .
H46B H 0.7775 0.0812 -0.1735 0.068 Uiso 1 1 calc R . .
C47 C 0.6047(12) 0.0943(4) -0.0910(12) 0.051(3) Uani 1 1 d . . .
C48 C 0.5074(13) 0.0689(4) -0.1608(13) 0.055(3) Uani 1 1 d . . .
C49 C 0.5199(16) 0.0349(4) -0.2586(17) 0.079(4) Uani 1 1 d . . .
H49A H 0.5063 0.0448 -0.3517 0.118 Uiso 1 1 calc R . .
H49B H 0.4509 0.0148 -0.2474 0.118 Uiso 1 1 calc R . .
H49C H 0.6105 0.0230 -0.2395 0.118 Uiso 1 1 calc R . .
C50 C 0.4041(11) 0.1076(4) -0.0180(12) 0.048(3) Uani 1 1 d . . .
C51 C 0.2954(12) 0.1247(5) 0.0581(14) 0.069(4) Uani 1 1 d . . .
H51A H 0.2710 0.1046 0.1232 0.083 Uiso 1 1 calc R . .
H51B H 0.3335 0.1478 0.1109 0.083 Uiso 1 1 calc R . .
C52 C 0.1687(15) 0.1373(6) -0.0297(16) 0.091(5) Uani 1 1 d . . .
H52A H 0.1825 0.1636 -0.0674 0.136 Uiso 1 1 calc R . .
H52B H 0.0932 0.1383 0.0245 0.136 Uiso 1 1 calc R . .
H52C H 0.1476 0.1182 -0.1036 0.136 Uiso 1 1 calc R . .
C39 C 0.4882(17) 0.2120(5) -0.3467(17) 0.089(5) Uani 1 1 d . . .
H39A H 0.4219 0.2328 -0.3761 0.133 Uiso 1 1 calc R . .
H39B H 0.4940 0.1935 -0.4214 0.133 Uiso 1 1 calc R . .
H39C H 0.5774 0.2240 -0.3194 0.133 Uiso 1 1 calc R . .
C38 C 0.4439(16) 0.1901(5) -0.2287(13) 0.066(4) Uani 1 1 d . . .
H38A H 0.5094 0.1683 -0.2042 0.080 Uiso 1 1 calc R . .
H38B H 0.3547 0.1777 -0.2591 0.080 Uiso 1 1 calc R . .
C37 C 0.4312(12) 0.2137(3) -0.1016(11) 0.043(3) Uani 1 1 d . . .
C34 C 0.4415(10) 0.2376(3) 0.1083(11) 0.044(3) Uani 1 1 d . . .
C33 C 0.4887(11) 0.2384(4) 0.2600(12) 0.053(3) Uani 1 1 d . . .
H33A H 0.4510 0.2624 0.2982 0.064 Uiso 1 1 calc R . .
H33B H 0.4491 0.2152 0.3013 0.064 Uiso 1 1 calc R . .
C32 C 0.6403(10) 0.2380(3) 0.3022(11) 0.043(3) Uani 1 1 d . . .
C30 C 0.7209(13) 0.2605(4) 0.3927(12) 0.053(3) Uani 1 1 d . . .
C31 C 0.6853(16) 0.2945(5) 0.4804(14) 0.078(4) Uani 1 1 d . . .
H31A H 0.5992 0.2889 0.5148 0.117 Uiso 1 1 calc R . .
H31B H 0.6762 0.3189 0.4266 0.117 Uiso 1 1 calc R . .
H31C H 0.7573 0.2979 0.5567 0.117 Uiso 1 1 calc R . .
C35 C 0.3505(12) 0.2616(4) 0.0305(13) 0.055(3) Uani 1 1 d . . .
C36 C 0.2643(14) 0.2976(5) 0.0662(16) 0.082(5) Uani 1 1 d . . .
H36A H 0.2815 0.3026 0.1638 0.123 Uiso 1 1 calc R . .
H36B H 0.1677 0.2918 0.0403 0.123 Uiso 1 1 calc R . .
H36C H 0.2894 0.3210 0.0170 0.123 Uiso 1 1 calc R . .
C29 C 0.8511(11) 0.2134(4) 0.3092(11) 0.046(3) Uani 1 1 d . . .
C28 C 0.9755(12) 0.1883(4) 0.2931(15) 0.062(4) Uani 1 1 d . . .
H28A H 0.9931 0.1708 0.3732 0.074 Uiso 1 1 calc R . .
H28B H 0.9524 0.1711 0.2131 0.074 Uiso 1 1 calc R . .
C27 C 1.1040(16) 0.2093(6) 0.277(2) 0.118(8) Uani 1 1 d . . .
H27A H 1.1082 0.2143 0.1809 0.177 Uiso 1 1 calc R . .
H27B H 1.1815 0.1930 0.3142 0.177 Uiso 1 1 calc R . .
H27C H 1.1069 0.2346 0.3259 0.177 Uiso 1 1 calc R . .
Ni1 Ni 0.87240(13) 0.47213(4) 0.86997(14) 0.0458(4) Uani 1 1 d . . .
O2 O 0.9789(10) 0.5185(3) 1.0077(11) 0.074(3) Uani 1 1 d . . .
O1 O 0.7788(10) 0.4960(3) 1.0575(10) 0.072(3) Uani 1 1 d . . .
O3 O 0.8847(17) 0.5398(6) 1.1844(17) 0.168(7) Uani 1 1 d U . .
N7 N 0.9586(9) 0.4298(3) 1.0075(10) 0.044(2) Uani 1 1 d . . .
N8 N 1.0947(10) 0.3928(3) 1.1620(10) 0.052(3) Uani 1 1 d . . .
H8 H 1.1666 0.3842 1.2147 0.062 Uiso 1 1 calc R . .
N5 N 0.7320(9) 0.4294(3) 0.7816(9) 0.045(2) Uani 1 1 d . . .
N6 N 0.5877(11) 0.3937(4) 0.6560(11) 0.058(3) Uani 1 1 d . . .
H6 H 0.5360 0.3849 0.5840 0.070 Uiso 1 1 calc R . .
N1 N 1.0078(9) 0.4671(3) 0.7269(10) 0.054(2) Uani 1 1 d . . .
N2 N 1.1207(12) 0.4439(4) 0.5616(13) 0.080(4) Uani 1 1 d . . .
H2 H 1.1632 0.4277 0.5122 0.096 Uiso 1 1 calc R . .
N3 N 0.7706(10) 0.5193(3) 0.7604(11) 0.048(2) Uani 1 1 d . . .
N4 N 0.6159(11) 0.5594(3) 0.6528(11) 0.056(3) Uani 1 1 d . . .
H4 H 0.5361 0.5701 0.6272 0.068 Uiso 1 1 calc R . .
N9 N 0.8793(16) 0.5181(4) 1.0846(13) 0.078(4) Uani 1 1 d U . .
C1 C 1.006(3) 0.3624(6) 0.640(2) 0.150(10) Uani 1 1 d . . .
H1A H 1.0190 0.3696 0.5469 0.226 Uiso 1 1 calc R . .
H1B H 0.9088 0.3612 0.6472 0.226 Uiso 1 1 calc R . .
H1C H 1.0475 0.3365 0.6619 0.226 Uiso 1 1 calc R . .
C2 C 1.0696(19) 0.3917(4) 0.7321(16) 0.083(5) Uani 1 1 d . . .
H2A H 1.1666 0.3847 0.7570 0.099 Uiso 1 1 calc R . .
H2B H 1.0257 0.3913 0.8158 0.099 Uiso 1 1 calc R . .
C3 C 1.0598(13) 0.4335(3) 0.6718(14) 0.055(3) Uani 1 1 d . . .
C26 C 1.3459(13) 0.4271(6) 1.0453(18) 0.096(6) Uani 1 1 d . . .
H26A H 1.3760 0.4146 1.1328 0.145 Uiso 1 1 calc R . .
H26B H 1.4168 0.4451 1.0218 0.145 Uiso 1 1 calc R . .
H26C H 1.3283 0.4067 0.9755 0.145 Uiso 1 1 calc R . .
C5 C 1.1536(18) 0.5070(6) 0.4190(15) 0.097(5) Uani 1 1 d . . .
H5A H 1.2251 0.4909 0.3870 0.146 Uiso 1 1 calc R . .
H5B H 1.1901 0.5332 0.4465 0.146 Uiso 1 1 calc R . .
H5C H 1.0780 0.5100 0.3460 0.146 Uiso 1 1 calc R . .
C4 C 1.1028(14) 0.4865(5) 0.5406(15) 0.068(4) Uani 1 1 d . . .
C6 C 1.0317(12) 0.4994(4) 0.6389(13) 0.056(3) Uani 1 1 d . . .
C7 C 0.9878(12) 0.5406(4) 0.6705(15) 0.058(3) Uani 1 1 d . . .
H7A H 1.0155 0.5590 0.6018 0.070 Uiso 1 1 calc R . .
H7B H 1.0359 0.5486 0.7597 0.070 Uiso 1 1 calc R . .
C8 C 0.8319(12) 0.5447(4) 0.6735(13) 0.052(3) Uani 1 1 d . . .
C9 C 0.7390(13) 0.5709(4) 0.6055(14) 0.057(3) Uani 1 1 d . . .
C10 C 0.7467(17) 0.6033(5) 0.5013(17) 0.087(5) Uani 1 1 d . . .
H10A H 0.7309 0.6291 0.5418 0.130 Uiso 1 1 calc R . .
H10B H 0.6773 0.5987 0.4236 0.130 Uiso 1 1 calc R . .
H10C H 0.8369 0.6031 0.4713 0.130 Uiso 1 1 calc R . .
C11 C 0.6396(13) 0.5290(4) 0.7443(13) 0.055(3) Uani 1 1 d . . .
C12 C 0.5280(13) 0.5121(5) 0.8227(14) 0.068(4) Uani 1 1 d . . .
H12A H 0.5012 0.5326 0.8852 0.081 Uiso 1 1 calc R . .
H12B H 0.5649 0.4892 0.8776 0.081 Uiso 1 1 calc R . .
C25 C 1.2116(11) 0.4513(4) 1.0547(15) 0.059(3) Uani 1 1 d . . .
H25A H 1.2280 0.4702 1.1311 0.071 Uiso 1 1 calc R . .
H25B H 1.1893 0.4669 0.9706 0.071 Uiso 1 1 calc R . .
C24 C 1.0894(12) 0.4251(4) 1.0748(13) 0.050(3) Uani 1 1 d . . .
C22 C 0.9602(11) 0.3760(4) 1.1499(11) 0.048(3) Uani 1 1 d . . .
C23 C 0.9365(14) 0.3390(4) 1.2369(14) 0.066(3) Uani 1 1 d . . .
H23A H 0.8444 0.3289 1.2103 0.099 Uiso 1 1 calc R . .
H23B H 0.9474 0.3464 1.3328 0.099 Uiso 1 1 calc R . .
H23C H 1.0028 0.3185 1.2224 0.099 Uiso 1 1 calc R . .
C21 C 0.8830(10) 0.3987(4) 1.0581(11) 0.046(3) Uani 1 1 d . . .
C20 C 0.7240(10) 0.3969(4) 1.0145(11) 0.044(3) Uani 1 1 d . . .
H20A H 0.6890 0.3719 1.0489 0.052 Uiso 1 1 calc R . .
H20B H 0.6812 0.4191 1.0582 0.052 Uiso 1 1 calc R . .
C19 C 0.6812(11) 0.3991(3) 0.8643(12) 0.047(3) Uani 1 1 d . . .
C17 C 0.5905(12) 0.3768(4) 0.7809(13) 0.054(3) Uani 1 1 d . . .
C18 C 0.5040(13) 0.3402(4) 0.8076(16) 0.069(4) Uani 1 1 d . . .
H18A H 0.4396 0.3475 0.8701 0.104 Uiso 1 1 calc R . .
H18B H 0.5637 0.3190 0.8476 0.104 Uiso 1 1 calc R . .
H18C H 0.4539 0.3310 0.7220 0.104 Uiso 1 1 calc R . .
C16 C 0.6713(11) 0.4249(3) 0.6535(11) 0.042(2) Uani 1 1 d . . .
C15 C 0.6875(13) 0.4498(4) 0.5347(12) 0.058(3) Uani 1 1 d . . .
H15A H 0.7661 0.4676 0.5592 0.070 Uiso 1 1 calc R . .
H15B H 0.6057 0.4667 0.5153 0.070 Uiso 1 1 calc R . .
C14 C 0.7088(17) 0.4275(6) 0.4023(16) 0.099(6) Uani 1 1 d . . .
H14A H 0.7858 0.4093 0.4207 0.148 Uiso 1 1 calc R . .
H14B H 0.7274 0.4467 0.3333 0.148 Uiso 1 1 calc R . .
H14C H 0.6265 0.4125 0.3694 0.148 Uiso 1 1 calc R . .
C13 C 0.401(2) 0.4988(9) 0.726(3) 0.196(15) Uani 1 1 d . . .
H13C H 0.3382 0.5211 0.7094 0.294 Uiso 1 1 calc R . .
H13D H 0.3561 0.4770 0.7682 0.294 Uiso 1 1 calc R . .
H13E H 0.4288 0.4897 0.6406 0.294 Uiso 1 1 calc R . .
Cl1 Cl 0.3289(3) 0.38807(12) 0.4117(3) 0.0706(10) Uani 1 1 d . . .
Cl2 Cl 0.0950(3) 0.25098(13) 0.6502(3) 0.0703(9) Uani 1 1 d . . .
O7 O 0.297(2) 0.2953(4) 0.4594(19) 0.174(8) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni2 N10 2.048(10) . ?
Ni2 N16 2.061(9) . ?
Ni2 N14 2.063(10) . ?
Ni2 N12 2.075(9) . ?
Ni2 O5 2.167(10) . ?
Ni2 O4 2.226(8) . ?
O6 N18 1.254(17) . ?
O4 N18 1.257(15) . ?
O5 N18 1.241(16) . ?
N14 C50 1.324(14) . ?
N14 C47 1.409(15) . ?
N15 C50 1.355(15) . ?
N15 C48 1.382(15) . ?
N15 H15 0.8600 . ?
N12 C37 1.322(14) . ?
N12 C34 1.381(14) . ?
N13 C37 1.379(15) . ?
N13 C35 1.439(16) . ?
N13 H13 0.8600 . ?
N10 C29 1.339(14) . ?
N10 C32 1.416(14) . ?
N11 C29 1.311(16) . ?
N11 C30 1.346(16) . ?
N11 H11 0.8600 . ?
N16 C42 1.352(15) . ?
N16 C45 1.432(15) . ?
N17 C43 1.357(17) . ?
N17 C42 1.362(15) . ?
N17 H17 0.8600 . ?
C40 C41 1.448(19) . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 C42 1.47(2) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C43 C45 1.351(16) . ?
C43 C44 1.483(16) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 C46 1.459(18) . ?
C46 C47 1.467(16) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C47 C48 1.376(17) . ?
C48 C49 1.492(17) . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C50 C51 1.480(15) . ?
C51 C52 1.467(19) . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C39 C38 1.472(19) . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C38 C37 1.484(17) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C34 C35 1.347(16) . ?
C34 C33 1.492(15) . ?
C33 C32 1.478(14) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C32 C30 1.329(15) . ?
C30 C31 1.483(18) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C35 C36 1.521(17) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C29 C28 1.491(16) . ?
C28 C27 1.456(18) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
Ni1 N7 2.043(10) . ?
Ni1 N1 2.047(8) . ?
Ni1 N3 2.069(10) . ?
Ni1 N5 2.072(9) . ?
Ni1 O2 2.206(9) . ?
Ni1 O1 2.288(9) . ?
O2 N9 1.301(16) . ?
O1 N9 1.222(16) . ?
O3 N9 1.207(16) . ?
N7 C24 1.362(15) . ?
N7 C21 1.390(14) . ?
N8 C24 1.363(16) . ?
N8 C22 1.411(14) . ?
N8 H8 0.8600 . ?
N5 C16 1.320(14) . ?
N5 C19 1.416(13) . ?
N6 C16 1.316(15) . ?
N6 C17 1.338(16) . ?
N6 H6 0.8600 . ?
N1 C3 1.359(14) . ?
N1 C6 1.408(16) . ?
N2 C3 1.338(15) . ?
N2 C4 1.432(18) . ?
N2 H2 0.8600 . ?
N3 C11 1.302(15) . ?
N3 C8 1.383(15) . ?
N4 C11 1.345(15) . ?
N4 C9 1.392(15) . ?
N4 H4 0.8600 . ?
C1 C2 1.41(2) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.503(18) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C26 C25 1.544(18) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C5 C4 1.506(18) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C4 C6 1.324(17) . ?
C6 C7 1.473(17) . ?
C7 C8 1.526(16) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.361(17) . ?
C9 C10 1.485(19) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.514(17) . ?
C12 C13 1.51(2) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C25 C24 1.504(17) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C22 C21 1.324(15) . ?
C22 C23 1.524(16) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C21 C20 1.551(14) . ?
C20 C19 1.473(15) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C19 C17 1.340(16) . ?
C17 C18 1.514(16) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C16 C15 1.447(16) . ?
C15 C14 1.526(18) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C13 H13C 0.9600 . ?
C13 H13D 0.9600 . ?
C13 H13E 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
N10 Ni2 N16 99.0(4) . . ?
N10 Ni2 N14 169.6(4) . . ?
N16 Ni2 N14 90.5(4) . . ?
N10 Ni2 N12 89.2(4) . . ?
N16 Ni2 N12 96.1(4) . . ?
N14 Ni2 N12 93.9(4) . . ?
N10 Ni2 O5 87.4(4) . . ?
N16 Ni2 O5 99.9(4) . . ?
N14 Ni2 O5 86.9(4) . . ?
N12 Ni2 O5 164.0(4) . . ?
N10 Ni2 O4 83.4(4) . . ?
N16 Ni2 O4 157.9(4) . . ?
N14 Ni2 O4 86.2(4) . . ?
N12 Ni2 O4 105.9(4) . . ?
O5 Ni2 O4 58.1(4) . . ?
N18 O4 Ni2 90.6(7) . . ?
N18 O5 Ni2 93.7(8) . . ?
C50 N14 C47 107.7(10) . . ?
C50 N14 Ni2 130.4(8) . . ?
C47 N14 Ni2 121.7(8) . . ?
C50 N15 C48 108.9(10) . . ?
C50 N15 H15 125.6 . . ?
C48 N15 H15 125.6 . . ?
C37 N12 C34 108.1(9) . . ?
C37 N12 Ni2 130.3(8) . . ?
C34 N12 Ni2 121.6(7) . . ?
C37 N13 C35 105.9(9) . . ?
C37 N13 H13 127.1 . . ?
C35 N13 H13 127.1 . . ?
C29 N10 C32 105.9(10) . . ?
C29 N10 Ni2 132.1(8) . . ?
C32 N10 Ni2 122.1(7) . . ?
C29 N11 C30 113.9(11) . . ?
C29 N11 H11 123.0 . . ?
C30 N11 H11 123.0 . . ?
C42 N16 C45 107.6(9) . . ?
C42 N16 Ni2 129.6(8) . . ?
C45 N16 Ni2 121.6(7) . . ?
C43 N17 C42 110.7(11) . . ?
C43 N17 H17 124.6 . . ?
C42 N17 H17 124.6 . . ?
O5 N18 O6 123.1(17) . . ?
O5 N18 O4 117.5(12) . . ?
O6 N18 O4 119.2(17) . . ?
C41 C40 H40A 109.5 . . ?
C41 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C41 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C40 C41 C42 123.6(14) . . ?
C40 C41 H41A 106.4 . . ?
C42 C41 H41A 106.4 . . ?
C40 C41 H41B 106.4 . . ?
C42 C41 H41B 106.4 . . ?
H41A C41 H41B 106.5 . . ?
N16 C42 N17 107.0(12) . . ?
N16 C42 C41 127.4(10) . . ?
N17 C42 C41 125.3(11) . . ?
C45 C43 N17 107.5(11) . . ?
C45 C43 C44 131.0(13) . . ?
N17 C43 C44 121.4(11) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C43 C45 N16 107.0(11) . . ?
C43 C45 C46 132.1(12) . . ?
N16 C45 C46 120.6(10) . . ?
C45 C46 C47 113.4(10) . . ?
C45 C46 H46A 108.9 . . ?
C47 C46 H46A 108.9 . . ?
C45 C46 H46B 108.9 . . ?
C47 C46 H46B 108.9 . . ?
H46A C46 H46B 107.7 . . ?
C48 C47 N14 107.5(10) . . ?
C48 C47 C46 130.3(11) . . ?
N14 C47 C46 122.1(11) . . ?
C47 C48 N15 106.3(10) . . ?
C47 C48 C49 132.0(12) . . ?
N15 C48 C49 121.4(11) . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
N14 C50 N15 109.6(10) . . ?
N14 C50 C51 125.7(11) . . ?
N15 C50 C51 124.7(10) . . ?
C52 C51 C50 114.6(11) . . ?
C52 C51 H51A 108.6 . . ?
C50 C51 H51A 108.6 . . ?
C52 C51 H51B 108.6 . . ?
C50 C51 H51B 108.6 . . ?
H51A C51 H51B 107.6 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C39 C38 C37 117.3(13) . . ?
C39 C38 H38A 108.0 . . ?
C37 C38 H38A 108.0 . . ?
C39 C38 H38B 108.0 . . ?
C37 C38 H38B 108.0 . . ?
H38A C38 H38B 107.2 . . ?
N12 C37 N13 110.2(10) . . ?
N12 C37 C38 130.3(11) . . ?
N13 C37 C38 119.5(11) . . ?
C35 C34 N12 109.9(9) . . ?
C35 C34 C33 130.1(10) . . ?
N12 C34 C33 120.0(10) . . ?
C32 C33 C34 116.3(9) . . ?
C32 C33 H33A 108.2 . . ?
C34 C33 H33A 108.2 . . ?
C32 C33 H33B 108.2 . . ?
C34 C33 H33B 108.2 . . ?
H33A C33 H33B 107.4 . . ?
C30 C32 N10 109.6(10) . . ?
C30 C32 C33 131.4(11) . . ?
N10 C32 C33 118.9(10) . . ?
C32 C30 N11 103.9(11) . . ?
C32 C30 C31 130.3(12) . . ?
N11 C30 C31 125.8(12) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C34 C35 N13 106.0(10) . . ?
C34 C35 C36 132.2(12) . . ?
N13 C35 C36 121.8(11) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N11 C29 N10 106.8(10) . . ?
N11 C29 C28 125.8(11) . . ?
N10 C29 C28 127.4(12) . . ?
C27 C28 C29 117.7(13) . . ?
C27 C28 H28A 107.9 . . ?
C29 C28 H28A 107.9 . . ?
C27 C28 H28B 107.9 . . ?
C29 C28 H28B 107.9 . . ?
H28A C28 H28B 107.2 . . ?
C28 C27 H27A 109.5 . . ?
C28 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C28 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N7 Ni1 N1 98.5(4) . . ?
N7 Ni1 N3 169.8(4) . . ?
N1 Ni1 N3 90.9(4) . . ?
N7 Ni1 N5 89.9(4) . . ?
N1 Ni1 N5 96.2(4) . . ?
N3 Ni1 N5 93.1(4) . . ?
N7 Ni1 O2 87.5(3) . . ?
N1 Ni1 O2 100.3(4) . . ?
N3 Ni1 O2 86.9(4) . . ?
N5 Ni1 O2 163.4(4) . . ?
N7 Ni1 O1 83.3(3) . . ?
N1 Ni1 O1 158.7(4) . . ?
N3 Ni1 O1 86.6(4) . . ?
N5 Ni1 O1 105.0(4) . . ?
O2 Ni1 O1 58.5(4) . . ?
N9 O2 Ni1 91.1(8) . . ?
N9 O1 Ni1 89.4(8) . . ?
C24 N7 C21 104.4(9) . . ?
C24 N7 Ni1 132.2(8) . . ?
C21 N7 Ni1 123.3(7) . . ?
C24 N8 C22 107.2(10) . . ?
C24 N8 H8 126.4 . . ?
C22 N8 H8 126.4 . . ?
C16 N5 C19 108.3(9) . . ?
C16 N5 Ni1 131.3(8) . . ?
C19 N5 Ni1 120.4(7) . . ?
C16 N6 C17 113.9(10) . . ?
C16 N6 H6 123.0 . . ?
C17 N6 H6 123.0 . . ?
C3 N1 C6 106.1(9) . . ?
C3 N1 Ni1 129.9(8) . . ?
C6 N1 Ni1 121.8(8) . . ?
C3 N2 C4 107.9(11) . . ?
C3 N2 H2 126.1 . . ?
C4 N2 H2 126.1 . . ?
C11 N3 C8 105.7(10) . . ?
C11 N3 Ni1 129.9(8) . . ?
C8 N3 Ni1 124.0(8) . . ?
C11 N4 C9 110.2(10) . . ?
C11 N4 H4 124.9 . . ?
C9 N4 H4 124.9 . . ?
O3 N9 O1 118.8(17) . . ?
O3 N9 O2 120.2(17) . . ?
O1 N9 O2 121.1(12) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C1 C2 C3 112.4(15) . . ?
C1 C2 H2A 109.1 . . ?
C3 C2 H2A 109.1 . . ?
C1 C2 H2B 109.1 . . ?
C3 C2 H2B 109.1 . . ?
H2A C2 H2B 107.9 . . ?
N2 C3 N1 109.7(11) . . ?
N2 C3 C2 122.5(11) . . ?
N1 C3 C2 127.2(11) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C6 C4 N2 106.2(12) . . ?
C6 C4 C5 133.0(15) . . ?
N2 C4 C5 120.7(13) . . ?
C4 C6 N1 110.0(12) . . ?
C4 C6 C7 130.0(12) . . ?
N1 C6 C7 119.9(10) . . ?
C6 C7 C8 113.7(10) . . ?
C6 C7 H7A 108.8 . . ?
C8 C7 H7A 108.8 . . ?
C6 C7 H7B 108.8 . . ?
C8 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
C9 C8 N3 112.0(10) . . ?
C9 C8 C7 130.2(11) . . ?
N3 C8 C7 117.8(11) . . ?
C8 C9 N4 102.0(10) . . ?
C8 C9 C10 134.7(12) . . ?
N4 C9 C10 123.2(12) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C11 N4 110.1(10) . . ?
N3 C11 C12 127.1(11) . . ?
N4 C11 C12 122.6(11) . . ?
C11 C12 C13 111.9(14) . . ?
C11 C12 H12A 109.2 . . ?
C13 C12 H12A 109.2 . . ?
C11 C12 H12B 109.2 . . ?
C13 C12 H12B 109.2 . . ?
H12A C12 H12B 107.9 . . ?
C24 C25 C26 113.4(12) . . ?
C24 C25 H25A 108.9 . . ?
C26 C25 H25A 108.9 . . ?
C24 C25 H25B 108.9 . . ?
C26 C25 H25B 108.9 . . ?
H25A C25 H25B 107.7 . . ?
N7 C24 N8 110.3(10) . . ?
N7 C24 C25 125.2(11) . . ?
N8 C24 C25 124.5(12) . . ?
C21 C22 N8 105.8(10) . . ?
C21 C22 C23 135.9(10) . . ?
N8 C22 C23 118.3(10) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C21 N7 112.3(9) . . ?
C22 C21 C20 128.4(10) . . ?
N7 C21 C20 119.1(10) . . ?
C19 C20 C21 114.4(8) . . ?
C19 C20 H20A 108.7 . . ?
C21 C20 H20A 108.7 . . ?
C19 C20 H20B 108.7 . . ?
C21 C20 H20B 108.7 . . ?
H20A C20 H20B 107.6 . . ?
C17 C19 N5 107.1(10) . . ?
C17 C19 C20 131.0(10) . . ?
N5 C19 C20 121.8(10) . . ?
N6 C17 C19 104.9(10) . . ?
N6 C17 C18 123.0(12) . . ?
C19 C17 C18 132.1(12) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N6 C16 N5 105.8(10) . . ?
N6 C16 C15 126.4(11) . . ?
N5 C16 C15 127.8(11) . . ?
C16 C15 C14 116.4(13) . . ?
C16 C15 H15A 108.2 . . ?
C14 C15 H15A 108.2 . . ?
C16 C15 H15B 108.2 . . ?
C14 C15 H15B 108.2 . . ?
H15A C15 H15B 107.3 . . ?
C15 C14 H14A 109.5 . . ?
C15 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C15 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C13 H13C 109.5 . . ?
C12 C13 H13D 109.5 . . ?
H13C C13 H13D 109.5 . . ?
C12 C13 H13E 109.5 . . ?
H13C C13 H13E 109.5 . . ?
H13D C13 H13E 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         0.837
_refine_diff_density_min         -1.034
_refine_diff_density_rms         0.160

