# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C11 H14 Cl N5 Ni O'
_chemical_formula_weight         326.43

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           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   9.4997(3)
_cell_length_b                   12.1258(4)
_cell_length_c                   11.8494(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.933(3)
_cell_angle_gamma                90.00
_cell_volume                     1340.18(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7111
_cell_measurement_theta_min      3.0284
_cell_measurement_theta_max      32.2397

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             672
_exptl_absorpt_coefficient_mu    1.646
_exptl_absorpt_correction_T_min  0.6127
_exptl_absorpt_correction_T_max  0.7135
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Micro-Focus (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'OXFORD DIFFRACTION SUPER NOVA'
_diffrn_measurement_method       ω/q-scan
_diffrn_detector_area_resol_mean 15.9948
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8391
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_sigmaI/netI    0.0181
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.03
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2357
_reflns_number_gt                2222
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.,'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.,'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.,'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Ortep3
_computing_publication_material  Shelx97

_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)+(0.0515P)²+8.2043P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    riding
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2357
_refine_ls_number_parameters     174
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0478
_refine_ls_wR_factor_ref         0.1416
_refine_ls_wR_factor_gt          0.1408
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_restrained_S_all      1.153
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.23915(6) 0.24569(5) 0.26591(5) 0.0155(2) Uani 1 1 d . . .
Cl1 Cl -0.33334(13) 0.05185(11) 0.53107(11) 0.0287(3) Uani 1 1 d . . .
O1 O 0.1017(3) 0.2974(3) 0.3426(3) 0.0218(7) Uani 1 1 d . . .
N1 N 0.3931(4) 0.1931(3) 0.1912(3) 0.0194(8) Uani 1 1 d . . .
N2 N 0.1571(4) 0.1070(3) 0.2390(3) 0.0187(8) Uani 1 1 d . . .
N3 N 0.3269(4) 0.3871(3) 0.2815(4) 0.0240(9) Uani 1 1 d . . .
N4 N 0.2938(4) 0.4568(3) 0.3443(3) 0.0217(9) Uani 1 1 d . . .
N5 N 0.2683(5) 0.5275(4) 0.4024(4) 0.0328(11) Uani 1 1 d . . .
C1 C 0.0087(5) 0.2371(4) 0.3850(4) 0.0174(9) Uani 1 1 d . . .
C2 C -0.0653(5) 0.2863(4) 0.4648(4) 0.0224(10) Uani 1 1 d . . .
H2 H -0.0443 0.3606 0.4873 0.027 Uiso 1 1 calc R . .
C3 C -0.1664(5) 0.2302(4) 0.5107(4) 0.0238(10) Uani 1 1 d . . .
H3 H -0.2149 0.2654 0.5640 0.029 Uiso 1 1 calc R . .
C4 C -0.1972(5) 0.1209(4) 0.4785(4) 0.0213(10) Uani 1 1 d . . .
C5 C -0.1274(5) 0.0683(4) 0.4029(4) 0.0199(10) Uani 1 1 d . . .
H5 H -0.1494 -0.0063 0.3821 0.024 Uiso 1 1 calc R . .
C6 C -0.0224(5) 0.1255(4) 0.3558(4) 0.0178(9) Uani 1 1 d . . .
C7 C 0.0514(5) 0.0669(4) 0.2796(4) 0.0198(10) Uani 1 1 d . . .
H7 H 0.0205 -0.0058 0.2576 0.024 Uiso 1 1 calc R . .
C8 C 0.2281(5) 0.0376(4) 0.1637(4) 0.0255(11) Uani 1 1 d . . .
H8A H 0.1855 0.0508 0.0819 0.031 Uiso 1 1 calc R . .
H8B H 0.2175 -0.0415 0.1810 0.031 Uiso 1 1 calc R . .
C9 C 0.3838(5) 0.0702(4) 0.1881(4) 0.0247(11) Uani 1 1 d . . .
H9A H 0.4318 0.0392 0.2628 0.030 Uiso 1 1 calc R . .
H9B H 0.4322 0.0409 0.1274 0.030 Uiso 1 1 calc R . .
C10 C 0.5394(5) 0.2248(5) 0.2534(5) 0.0293(12) Uani 1 1 d . . .
H10A H 0.6118 0.1875 0.2181 0.044 Uiso 1 1 calc R . .
H10B H 0.5510 0.2027 0.3342 0.044 Uiso 1 1 calc R . .
H10C H 0.5514 0.3048 0.2487 0.044 Uiso 1 1 calc R . .
C11 C 0.3711(6) 0.2384(4) 0.0727(4) 0.0273(11) Uani 1 1 d . . .
H11A H 0.3860 0.3183 0.0761 0.041 Uiso 1 1 calc R . .
H11B H 0.2732 0.2223 0.0328 0.041 Uiso 1 1 calc R . .
H11C H 0.4396 0.2043 0.0310 0.041 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 1.836(3) . ?
Ni1 N2 1.855(4) . ?
Ni1 N3 1.900(4) . ?
Ni1 N1 1.955(4) . ?
Cl1 C4 1.751(5) . ?
O1 C1 1.318(6) . ?
N1 C11 1.485(6) . ?
N1 C9 1.493(6) . ?
N1 C10 1.495(6) . ?
N2 C7 1.288(6) . ?
N2 C8 1.479(6) . ?
N3 N4 1.206(6) . ?
N4 N5 1.154(6) . ?
C1 C2 1.413(7) . ?
C1 C6 1.414(7) . ?
C2 C3 1.371(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.395(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.369(7) . ?
C5 C6 1.414(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.432(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.505(7) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 N2 94.55(16) . . ?
O1 Ni1 N3 89.08(16) . . ?
N2 Ni1 N3 175.39(17) . . ?
O1 Ni1 N1 176.99(15) . . ?
N2 Ni1 N1 87.28(17) . . ?
N3 Ni1 N1 89.21(17) . . ?
C1 O1 Ni1 126.2(3) . . ?
C11 N1 C9 110.4(4) . . ?
C11 N1 C10 108.8(4) . . ?
C9 N1 C10 108.3(4) . . ?
C11 N1 Ni1 108.9(3) . . ?
C9 N1 Ni1 106.9(3) . . ?
C10 N1 Ni1 113.5(3) . . ?
C7 N2 C8 119.2(4) . . ?
C7 N2 Ni1 127.6(3) . . ?
C8 N2 Ni1 113.2(3) . . ?
N4 N3 Ni1 122.1(3) . . ?
N5 N4 N3 175.9(5) . . ?
O1 C1 C2 118.4(4) . . ?
O1 C1 C6 124.1(4) . . ?
C2 C1 C6 117.5(4) . . ?
C3 C2 C1 122.1(5) . . ?
C3 C2 H2 119.0 . . ?
C1 C2 H2 119.0 . . ?
C2 C3 C4 119.3(5) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C5 C4 C3 121.3(4) . . ?
C5 C4 Cl1 119.5(4) . . ?
C3 C4 Cl1 119.2(4) . . ?
C4 C5 C6 119.7(4) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C5 C6 C1 120.2(4) . . ?
C5 C6 C7 118.2(4) . . ?
C1 C6 C7 121.7(4) . . ?
N2 C7 C6 123.9(4) . . ?
N2 C7 H7 118.1 . . ?
C6 C7 H7 118.1 . . ?
N2 C8 C9 106.2(4) . . ?
N2 C8 H8A 110.5 . . ?
C9 C8 H8A 110.5 . . ?
N2 C8 H8B 110.5 . . ?
C9 C8 H8B 110.5 . . ?
H8A C8 H8B 108.7 . . ?
N1 C9 C8 108.6(4) . . ?
N1 C9 H9A 110.0 . . ?
C8 C9 H9A 110.0 . . ?
N1 C9 H9B 110.0 . . ?
C8 C9 H9B 110.0 . . ?
H9A C9 H9B 108.4 . . ?
N1 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 H11A 109.5 . . ?
N1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 Ni1 O1 C1 15.7(4) . . . . ?
N3 Ni1 O1 C1 -167.1(4) . . . . ?
N1 Ni1 O1 C1 -112(3) . . . . ?
O1 Ni1 N1 C11 -130(3) . . . . ?
N2 Ni1 N1 C11 102.8(3) . . . . ?
N3 Ni1 N1 C11 -74.2(3) . . . . ?
O1 Ni1 N1 C9 111(3) . . . . ?
N2 Ni1 N1 C9 -16.5(3) . . . . ?
N3 Ni1 N1 C9 166.4(3) . . . . ?
O1 Ni1 N1 C10 -8(3) . . . . ?
N2 Ni1 N1 C10 -135.8(4) . . . . ?
N3 Ni1 N1 C10 47.1(4) . . . . ?
O1 Ni1 N2 C7 -8.2(4) . . . . ?
N3 Ni1 N2 C7 -150(2) . . . . ?
N1 Ni1 N2 C7 169.4(4) . . . . ?
O1 Ni1 N2 C8 173.2(3) . . . . ?
N3 Ni1 N2 C8 31(2) . . . . ?
N1 Ni1 N2 C8 -9.2(3) . . . . ?
O1 Ni1 N3 N4 12.1(4) . . . . ?
N2 Ni1 N3 N4 154.2(19) . . . . ?
N1 Ni1 N3 N4 -165.4(4) . . . . ?
Ni1 N3 N4 N5 180(100) . . . . ?
Ni1 O1 C1 C2 164.7(3) . . . . ?
Ni1 O1 C1 C6 -15.2(6) . . . . ?
O1 C1 C2 C3 178.3(4) . . . . ?
C6 C1 C2 C3 -1.7(7) . . . . ?
C1 C2 C3 C4 0.3(7) . . . . ?
C2 C3 C4 C5 0.7(7) . . . . ?
C2 C3 C4 Cl1 -176.5(4) . . . . ?
C3 C4 C5 C6 -0.3(7) . . . . ?
Cl1 C4 C5 C6 176.9(3) . . . . ?
C4 C5 C6 C1 -1.1(7) . . . . ?
C4 C5 C6 C7 178.2(4) . . . . ?
O1 C1 C6 C5 -177.9(4) . . . . ?
C2 C1 C6 C5 2.1(6) . . . . ?
O1 C1 C6 C7 2.7(7) . . . . ?
C2 C1 C6 C7 -177.3(4) . . . . ?
C8 N2 C7 C6 178.1(4) . . . . ?
Ni1 N2 C7 C6 -0.4(7) . . . . ?
C5 C6 C7 N2 -173.9(4) . . . . ?
C1 C6 C7 N2 5.4(7) . . . . ?
C7 N2 C8 C9 -146.5(4) . . . . ?
Ni1 N2 C8 C9 32.3(5) . . . . ?
C11 N1 C9 C8 -80.1(5) . . . . ?
C10 N1 C9 C8 160.9(4) . . . . ?
Ni1 N1 C9 C8 38.3(4) . . . . ?
N2 C8 C9 N1 -45.4(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         2.069
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.120
_database_code_depnum_ccdc_archive 'CCDC 961048'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_4a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H31 Cl N11 Ni1.50 O2'
_chemical_formula_weight         677.15

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                   11.0194(11)
_cell_length_b                   12.2772(12)
_cell_length_c                   12.3400(13)
_cell_angle_alpha                79.470(8)
_cell_angle_beta                 76.251(9)
_cell_angle_gamma                79.852(8)
_cell_volume                     1578.8(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4392
_cell_measurement_theta_min      3.1435
_cell_measurement_theta_max      26.3096

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            PINK
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             702
_exptl_absorpt_coefficient_mu    1.033
_exptl_absorpt_correction_T_min  0.7334
_exptl_absorpt_correction_T_max  0.8123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Micro-Focus (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'OXFORD DIFFRACTION SUPER NOVA'
_diffrn_measurement_method       ω/q-scan
_diffrn_detector_area_resol_mean 15.9948
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10777
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_unetI/netI     0.0696
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.15
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5547
_reflns_number_gt                4188
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.,'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.,'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.,'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Ortep3
_computing_publication_material  Shelx97

_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)+(0.0844P)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    riding
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5547
_refine_ls_number_parameters     417
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0536
_refine_ls_wR_factor_ref         0.1617
_refine_ls_wR_factor_gt          0.1420
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.72787(4) 0.65946(3) -0.10407(4) 0.03807(19) Uani 1 1 d . A .
Ni2 Ni 0.5000 0.5000 0.0000 0.0364(2) Uani 1 2 d S . .
Cl1 Cl 0.6930(2) 0.5902(3) 0.49901(15) 0.1591(10) Uani 1 1 d . . .
O1 O 0.6153(2) 0.59664(19) 0.0444(2) 0.0400(6) Uani 1 1 d . . .
O2 O 0.6785(3) 0.8208(2) -0.0453(3) 0.0574(8) Uani 1 1 d . . .
N1 N 0.8740(3) 0.6373(3) -0.0288(3) 0.0504(9) Uani 1 1 d . . .
N2 N 0.8632(3) 0.7224(3) -0.2481(3) 0.0481(8) Uani 1 1 d . . .
N3 N 0.5737(3) 0.6920(2) -0.1748(3) 0.0417(8) Uani 1 1 d . . .
N4 N 0.4848(3) 0.6274(2) -0.1341(3) 0.0416(8) Uani 1 1 d . A .
N5 N 0.5450(3) 0.7647(2) -0.2622(3) 0.0480(8) Uani 1 1 d . A .
N6 N 0.3946(3) 0.6558(3) -0.1939(3) 0.0479(8) Uani 1 1 d . . .
N7 N 0.7591(3) 0.4913(2) -0.1387(3) 0.0408(8) Uani 1 1 d . . .
N8 N 0.6715(3) 0.4297(2) -0.0871(3) 0.0416(8) Uani 1 1 d . A .
N9 N 0.8608(3) 0.4270(2) -0.1885(3) 0.0445(8) Uani 1 1 d . A .
N10 N 0.7112(3) 0.3230(2) -0.0998(3) 0.0477(8) Uani 1 1 d . . .
N11 N 0.5583(4) 0.8976(3) 0.1039(4) 0.0714(11) Uani 1 1 d . . .
C1 C 0.6354(4) 0.5978(3) 0.1455(4) 0.0439(9) Uani 1 1 d . A .
C2 C 0.5366(4) 0.5937(4) 0.2401(4) 0.0575(11) Uani 1 1 d . . .
H2 H 0.4545 0.5911 0.2297 0.069 Uiso 1 1 calc R . .
C3 C 0.5514(5) 0.5933(5) 0.3473(4) 0.0733(14) Uani 1 1 d . . .
H3 H 0.4814 0.5912 0.4094 0.088 Uiso 1 1 calc R . .
C4 C 0.6724(6) 0.5959(5) 0.3627(5) 0.0808(16) Uani 1 1 d . . .
C5 C 0.7702(5) 0.6018(4) 0.2744(4) 0.0694(14) Uani 1 1 d . A .
H5 H 0.8515 0.6031 0.2873 0.083 Uiso 1 1 calc R . .
C6 C 0.7569(4) 0.6060(3) 0.1636(4) 0.0509(10) Uani 1 1 d . . .
C7 C 0.8672(4) 0.6206(4) 0.0763(4) 0.0585(12) Uani 1 1 d . A .
H7 H 0.9438 0.6173 0.1003 0.070 Uiso 1 1 calc R . .
C8A C 0.983(2) 0.6834(13) -0.0969(18) 0.048(3) Uani 0.50 1 d PU A 1
H8A1 H 1.0604 0.6440 -0.0726 0.057 Uiso 0.50 1 calc PR A 1
H8A2 H 0.9755 0.7640 -0.0923 0.057 Uiso 0.50 1 calc PR A 1
C9 C 0.9841(7) 0.6648(7) -0.2209(7) 0.0501(18) Uani 0.60 1 d PU A 1
H9A H 1.0557 0.6964 -0.2749 0.060 Uiso 0.60 1 calc PR A 1
H9B H 0.9931 0.5840 -0.2251 0.060 Uiso 0.60 1 calc PR A 1
C8 C 0.999(2) 0.6448(14) -0.115(2) 0.063(5) Uani 0.50 1 d PU A 2
H8A H 1.0645 0.6582 -0.0782 0.075 Uiso 0.50 1 calc PR A 2
H8B H 1.0273 0.5744 -0.1472 0.075 Uiso 0.50 1 calc PR A 2
C9A C 0.9753(12) 0.7337(13) -0.1979(13) 0.069(4) Uani 0.40 1 d PU A 2
H9A1 H 1.0519 0.7375 -0.2590 0.083 Uiso 0.40 1 calc PR A 2
H9A2 H 0.9573 0.8044 -0.1656 0.083 Uiso 0.40 1 calc PR A 2
C10 C 0.8411(5) 0.8431(4) -0.2767(5) 0.0873(18) Uani 1 1 d . A .
H10A H 0.8394 0.8778 -0.2108 0.131 Uiso 1 1 calc R . .
H10B H 0.7601 0.8653 -0.2999 0.131 Uiso 1 1 calc R . .
H10C H 0.9089 0.8677 -0.3388 0.131 Uiso 1 1 calc R . .
C11 C 0.8679(7) 0.6756(5) -0.3487(5) 0.104(2) Uani 1 1 d . A .
H11A H 0.7942 0.7097 -0.3806 0.156 Uiso 1 1 calc R . .
H11B H 0.8676 0.5946 -0.3294 0.156 Uiso 1 1 calc R . .
H11C H 0.9451 0.6909 -0.4042 0.156 Uiso 1 1 calc R . .
C12 C 0.4348(3) 0.7388(3) -0.2723(4) 0.0435(9) Uani 1 1 d . A .
C13 C 0.3691(4) 0.7913(3) -0.3633(4) 0.0511(10) Uani 1 1 d . . .
C14 C 0.3830(4) 0.8995(4) -0.4169(4) 0.0631(12) Uani 1 1 d . A .
H14 H 0.4342 0.9418 -0.3938 0.076 Uiso 1 1 calc R . .
C15 C 0.3219(5) 0.9455(5) -0.5042(5) 0.0771(15) Uani 1 1 d . . .
H15 H 0.3319 1.0194 -0.5411 0.092 Uiso 1 1 calc R A .
C16 C 0.2480(5) 0.8862(5) -0.5376(5) 0.0792(16) Uani 1 1 d . A .
H16 H 0.2048 0.9194 -0.5961 0.095 Uiso 1 1 calc R . .
C17 C 0.2355(5) 0.7783(5) -0.4867(5) 0.0768(15) Uani 1 1 d . . .
H17 H 0.1856 0.7359 -0.5113 0.092 Uiso 1 1 calc R A .
C18 C 0.2956(4) 0.7319(4) -0.3996(4) 0.0633(13) Uani 1 1 d . A .
H18 H 0.2862 0.6575 -0.3641 0.076 Uiso 1 1 calc R . .
C19 C 0.8273(3) 0.3243(3) -0.1623(4) 0.0425(9) Uani 1 1 d . A .
C20 C 0.9117(4) 0.2239(3) -0.1970(4) 0.0502(11) Uani 1 1 d . . .
C21 C 0.9947(4) 0.2290(4) -0.3004(5) 0.0709(14) Uani 1 1 d . A .
H21 H 0.9974 0.2972 -0.3512 0.085 Uiso 1 1 calc R . .
C22 C 1.0743(5) 0.1325(5) -0.3290(6) 0.0890(18) Uani 1 1 d . . .
H22 H 1.1315 0.1352 -0.4001 0.107 Uiso 1 1 calc R A .
C23 C 1.0719(5) 0.0346(4) -0.2573(7) 0.0888(19) Uani 1 1 d . A .
H23 H 1.1265 -0.0305 -0.2787 0.107 Uiso 1 1 calc R . .
C24 C 0.9908(6) 0.0295(4) -0.1541(7) 0.0868(19) Uani 1 1 d . . .
H24 H 0.9904 -0.0388 -0.1034 0.104 Uiso 1 1 calc R A .
C25 C 0.9089(4) 0.1242(3) -0.1232(5) 0.0669(13) Uani 1 1 d . A .
H25 H 0.8516 0.1205 -0.0521 0.080 Uiso 1 1 calc R . .
C26 C 0.6586(7) 0.9447(6) 0.1231(7) 0.124(3) Uani 1 1 d . . .
H26A H 0.6742 0.9132 0.1983 0.186 Uiso 1 1 calc R . .
H26B H 0.6359 1.0260 0.1185 0.186 Uiso 1 1 calc R . .
H26C H 0.7350 0.9275 0.0660 0.186 Uiso 1 1 calc R . .
C27 C 0.4397(6) 0.9064(5) 0.1851(6) 0.108(2) Uani 1 1 d . . .
H27A H 0.3774 0.8749 0.1596 0.162 Uiso 1 1 calc R . .
H27B H 0.4094 0.9852 0.1924 0.162 Uiso 1 1 calc R . .
H27C H 0.4518 0.8649 0.2584 0.162 Uiso 1 1 calc R . .
C28 C 0.5776(5) 0.8371(3) 0.0231(4) 0.0590(12) Uani 1 1 d . . .
H28 H 0.5091 0.8032 0.0165 0.071 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 1.998(3) . ?
Ni1 N3 2.036(3) . ?
Ni1 O1 2.056(3) . ?
Ni1 N7 2.137(3) . ?
Ni1 N2 2.150(3) . ?
Ni1 O2 2.169(3) . ?
Ni2 N8 2.067(3) . ?
Ni2 N8 2.067(3) 2_665 ?
Ni2 N4 2.075(3) . ?
Ni2 N4 2.075(3) 2_665 ?
Ni2 O1 2.103(2) 2_665 ?
Ni2 O1 2.103(2) . ?
Cl1 C4 1.737(5) . ?
O1 C1 1.321(5) . ?
O2 C28 1.235(5) . ?
N1 C7 1.262(6) . ?
N1 C8A 1.43(2) . ?
N1 C8 1.53(2) . ?
N2 C11 1.446(6) . ?
N2 C10 1.449(5) . ?
N2 C9 1.478(8) . ?
N2 C9A 1.545(13) . ?
N3 N4 1.318(4) . ?
N3 N5 1.331(4) . ?
N4 N6 1.336(4) . ?
N5 C12 1.346(4) . ?
N6 C12 1.329(5) . ?
N7 N8 1.303(4) . ?
N7 N9 1.340(4) . ?
N8 N10 1.331(4) . ?
N9 C19 1.337(4) . ?
N10 C19 1.328(5) . ?
N11 C28 1.305(6) . ?
N11 C26 1.419(7) . ?
N11 C27 1.447(7) . ?
C1 C2 1.395(6) . ?
C1 C6 1.432(5) . ?
C2 C3 1.369(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.398(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.340(7) . ?
C5 C6 1.399(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.433(6) . ?
C7 H7 0.9500 . ?
C8A C9 1.58(2) . ?
C8A H8A1 0.9900 . ?
C8A H8A2 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C8 C9A 1.39(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9A H9A1 0.9900 . ?
C9A H9A2 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.470(5) . ?
C13 C18 1.375(6) . ?
C13 C14 1.388(6) . ?
C14 C15 1.386(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.357(7) . ?
C15 H15 0.9500 . ?
C16 C17 1.374(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.378(6) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.473(5) . ?
C20 C21 1.380(7) . ?
C20 C25 1.386(6) . ?
C21 C22 1.393(6) . ?
C21 H21 0.9500 . ?
C22 C23 1.356(8) . ?
C22 H22 0.9500 . ?
C23 C24 1.369(9) . ?
C23 H23 0.9500 . ?
C24 C25 1.393(7) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N3 175.75(13) . . ?
N1 Ni1 O1 90.56(12) . . ?
N3 Ni1 O1 88.39(11) . . ?
N1 Ni1 N7 94.03(12) . . ?
N3 Ni1 N7 89.96(11) . . ?
O1 Ni1 N7 84.34(11) . . ?
N1 Ni1 N2 82.58(14) . . ?
N3 Ni1 N2 98.44(13) . . ?
O1 Ni1 N2 173.13(10) . . ?
N7 Ni1 N2 96.32(12) . . ?
N1 Ni1 O2 85.94(13) . . ?
N3 Ni1 O2 89.89(12) . . ?
O1 Ni1 O2 87.08(11) . . ?
N7 Ni1 O2 171.43(13) . . ?
N2 Ni1 O2 92.18(12) . . ?
N8 Ni2 N8 180.0 . 2_665 ?
N8 Ni2 N4 91.18(12) . . ?
N8 Ni2 N4 88.82(12) 2_665 . ?
N8 Ni2 N4 88.82(12) . 2_665 ?
N8 Ni2 N4 91.18(12) 2_665 2_665 ?
N4 Ni2 N4 180.00(19) . 2_665 ?
N8 Ni2 O1 97.85(10) . 2_665 ?
N8 Ni2 O1 82.15(11) 2_665 2_665 ?
N4 Ni2 O1 94.30(10) . 2_665 ?
N4 Ni2 O1 85.70(10) 2_665 2_665 ?
N8 Ni2 O1 82.15(11) . . ?
N8 Ni2 O1 97.85(11) 2_665 . ?
N4 Ni2 O1 85.70(10) . . ?
N4 Ni2 O1 94.30(10) 2_665 . ?
O1 Ni2 O1 180.00(13) 2_665 . ?
C1 O1 Ni1 124.1(2) . . ?
C1 O1 Ni2 128.0(2) . . ?
Ni1 O1 Ni2 106.24(11) . . ?
C28 O2 Ni1 117.5(3) . . ?
C7 N1 C8A 116.2(9) . . ?
C7 N1 C8 122.7(10) . . ?
C8A N1 C8 20.8(8) . . ?
C7 N1 Ni1 125.6(3) . . ?
C8A N1 Ni1 114.3(9) . . ?
C8 N1 Ni1 111.7(10) . . ?
C11 N2 C10 107.2(4) . . ?
C11 N2 C9 99.3(5) . . ?
C10 N2 C9 121.1(4) . . ?
C11 N2 C9A 127.5(7) . . ?
C10 N2 C9A 89.4(6) . . ?
C9 N2 C9A 35.4(5) . . ?
C11 N2 Ni1 113.6(3) . . ?
C10 N2 Ni1 112.9(3) . . ?
C9 N2 Ni1 102.2(4) . . ?
C9A N2 Ni1 103.8(6) . . ?
N4 N3 N5 109.9(3) . . ?
N4 N3 Ni1 117.6(2) . . ?
N5 N3 Ni1 132.4(2) . . ?
N3 N4 N6 109.9(3) . . ?
N3 N4 Ni2 120.9(2) . . ?
N6 N4 Ni2 129.2(2) . . ?
N3 N5 C12 103.7(3) . . ?
C12 N6 N4 104.0(3) . . ?
N8 N7 N9 109.6(3) . . ?
N8 N7 Ni1 116.3(2) . . ?
N9 N7 Ni1 133.0(2) . . ?
N7 N8 N10 110.4(3) . . ?
N7 N8 Ni2 120.8(2) . . ?
N10 N8 Ni2 128.8(2) . . ?
C19 N9 N7 103.6(3) . . ?
C19 N10 N8 103.8(3) . . ?
C28 N11 C26 120.6(5) . . ?
C28 N11 C27 121.2(5) . . ?
C26 N11 C27 117.8(5) . . ?
O1 C1 C2 120.7(3) . . ?
O1 C1 C6 122.5(4) . . ?
C2 C1 C6 116.7(4) . . ?
C3 C2 C1 123.6(4) . . ?
C3 C2 H2 118.2 . . ?
C1 C2 H2 118.2 . . ?
C2 C3 C4 118.2(5) . . ?
C2 C3 H3 120.9 . . ?
C4 C3 H3 120.9 . . ?
C5 C4 C3 120.6(5) . . ?
C5 C4 Cl1 120.9(4) . . ?
C3 C4 Cl1 118.5(5) . . ?
C4 C5 C6 122.3(4) . . ?
C4 C5 H5 118.8 . . ?
C6 C5 H5 118.8 . . ?
C5 C6 C1 118.4(4) . . ?
C5 C6 C7 116.6(4) . . ?
C1 C6 C7 125.0(4) . . ?
N1 C7 C6 127.2(4) . . ?
N1 C7 H7 116.4 . . ?
C6 C7 H7 116.4 . . ?
N1 C8A C9 104.5(12) . . ?
N1 C8A H8A1 110.8 . . ?
C9 C8A H8A1 110.8 . . ?
N1 C8A H8A2 110.8 . . ?
C9 C8A H8A2 110.8 . . ?
H8A1 C8A H8A2 108.9 . . ?
N2 C9 C8A 107.1(9) . . ?
N2 C9 H9A 110.3 . . ?
C8A C9 H9A 110.3 . . ?
N2 C9 H9B 110.3 . . ?
C8A C9 H9B 110.3 . . ?
H9A C9 H9B 108.6 . . ?
C9A C8 N1 106.4(14) . . ?
C9A C8 H8A 110.5 . . ?
N1 C8 H8A 110.5 . . ?
C9A C8 H8B 110.5 . . ?
N1 C8 H8B 110.5 . . ?
H8A C8 H8B 108.6 . . ?
C8 C9A N2 112.2(14) . . ?
C8 C9A H9A1 109.2 . . ?
N2 C9A H9A1 109.2 . . ?
C8 C9A H9A2 109.2 . . ?
N2 C9A H9A2 109.2 . . ?
H9A1 C9A H9A2 107.9 . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C11 H11A 109.5 . . ?
N2 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N2 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N6 C12 N5 112.5(3) . . ?
N6 C12 C13 123.2(3) . . ?
N5 C12 C13 124.2(3) . . ?
C18 C13 C14 118.7(4) . . ?
C18 C13 C12 120.0(4) . . ?
C14 C13 C12 121.3(4) . . ?
C15 C14 C13 119.7(5) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C16 C15 C14 120.7(5) . . ?
C16 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
C15 C16 C17 120.1(4) . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C16 C17 C18 119.6(5) . . ?
C16 C17 H17 120.2 . . ?
C18 C17 H17 120.2 . . ?
C13 C18 C17 121.2(5) . . ?
C13 C18 H18 119.4 . . ?
C17 C18 H18 119.4 . . ?
N10 C19 N9 112.6(3) . . ?
N10 C19 C20 124.1(3) . . ?
N9 C19 C20 123.3(3) . . ?
C21 C20 C25 120.2(4) . . ?
C21 C20 C19 120.7(4) . . ?
C25 C20 C19 119.1(4) . . ?
C20 C21 C22 118.8(5) . . ?
C20 C21 H21 120.6 . . ?
C22 C21 H21 120.6 . . ?
C23 C22 C21 121.3(6) . . ?
C23 C22 H22 119.3 . . ?
C21 C22 H22 119.3 . . ?
C22 C23 C24 120.1(5) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C23 C24 C25 120.2(5) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C20 C25 C24 119.5(5) . . ?
C20 C25 H25 120.3 . . ?
C24 C25 H25 120.3 . . ?
N11 C26 H26A 109.5 . . ?
N11 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
N11 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N11 C27 H27A 109.5 . . ?
N11 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N11 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O2 C28 N11 124.7(5) . . ?
O2 C28 H28 117.6 . . ?
N11 C28 H28 117.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Ni1 O1 C1 24.6(3) . . . . ?
N3 Ni1 O1 C1 -151.2(3) . . . . ?
N7 Ni1 O1 C1 118.6(3) . . . . ?
N2 Ni1 O1 C1 22.7(10) . . . . ?
O2 Ni1 O1 C1 -61.3(3) . . . . ?
N1 Ni1 O1 Ni2 -141.58(13) . . . . ?
N3 Ni1 O1 Ni2 42.54(12) . . . . ?
N7 Ni1 O1 Ni2 -47.59(11) . . . . ?
N2 Ni1 O1 Ni2 -143.5(9) . . . . ?
O2 Ni1 O1 Ni2 132.51(12) . . . . ?
N8 Ni2 O1 C1 -114.6(3) . . . . ?
N8 Ni2 O1 C1 65.4(3) 2_665 . . . ?
N4 Ni2 O1 C1 153.6(3) . . . . ?
N4 Ni2 O1 C1 -26.4(3) 2_665 . . . ?
O1 Ni2 O1 C1 7(100) 2_665 . . . ?
N8 Ni2 O1 Ni1 50.88(12) . . . . ?
N8 Ni2 O1 Ni1 -129.12(12) 2_665 . . . ?
N4 Ni2 O1 Ni1 -40.91(12) . . . . ?
N4 Ni2 O1 Ni1 139.09(12) 2_665 . . . ?
O1 Ni2 O1 Ni1 173(100) 2_665 . . . ?
N1 Ni1 O2 C28 -116.1(3) . . . . ?
N3 Ni1 O2 C28 63.0(3) . . . . ?
O1 Ni1 O2 C28 -25.4(3) . . . . ?
N7 Ni1 O2 C28 -26.0(9) . . . . ?
N2 Ni1 O2 C28 161.5(3) . . . . ?
N3 Ni1 N1 C7 59.7(19) . . . . ?
O1 Ni1 N1 C7 -15.9(4) . . . . ?
N7 Ni1 N1 C7 -100.3(4) . . . . ?
N2 Ni1 N1 C7 163.9(4) . . . . ?
O2 Ni1 N1 C7 71.2(4) . . . . ?
N3 Ni1 N1 C8A -97.0(19) . . . . ?
O1 Ni1 N1 C8A -172.6(6) . . . . ?
N7 Ni1 N1 C8A 103.0(6) . . . . ?
N2 Ni1 N1 C8A 7.1(6) . . . . ?
O2 Ni1 N1 C8A -85.6(6) . . . . ?
N3 Ni1 N1 C8 -119.4(18) . . . . ?
O1 Ni1 N1 C8 165.0(7) . . . . ?
N7 Ni1 N1 C8 80.6(7) . . . . ?
N2 Ni1 N1 C8 -15.3(7) . . . . ?
O2 Ni1 N1 C8 -108.0(7) . . . . ?
N1 Ni1 N2 C11 131.1(4) . . . . ?
N3 Ni1 N2 C11 -53.1(4) . . . . ?
O1 Ni1 N2 C11 133.0(9) . . . . ?
N7 Ni1 N2 C11 37.8(4) . . . . ?
O2 Ni1 N2 C11 -143.3(4) . . . . ?
N1 Ni1 N2 C10 -106.6(3) . . . . ?
N3 Ni1 N2 C10 69.3(3) . . . . ?
O1 Ni1 N2 C10 -104.7(9) . . . . ?
N7 Ni1 N2 C10 160.2(3) . . . . ?
O2 Ni1 N2 C10 -21.0(3) . . . . ?
N1 Ni1 N2 C9 25.1(4) . . . . ?
N3 Ni1 N2 C9 -159.1(4) . . . . ?
O1 Ni1 N2 C9 27.0(11) . . . . ?
N7 Ni1 N2 C9 -68.2(4) . . . . ?
O2 Ni1 N2 C9 110.7(4) . . . . ?
N1 Ni1 N2 C9A -11.2(6) . . . . ?
N3 Ni1 N2 C9A 164.6(6) . . . . ?
O1 Ni1 N2 C9A -9.3(12) . . . . ?
N7 Ni1 N2 C9A -104.5(6) . . . . ?
O2 Ni1 N2 C9A 74.4(6) . . . . ?
N1 Ni1 N3 N4 -104.4(17) . . . . ?
O1 Ni1 N3 N4 -28.7(3) . . . . ?
N7 Ni1 N3 N4 55.7(3) . . . . ?
N2 Ni1 N3 N4 152.0(3) . . . . ?
O2 Ni1 N3 N4 -115.8(3) . . . . ?
N1 Ni1 N3 N5 80.3(19) . . . . ?
O1 Ni1 N3 N5 155.9(4) . . . . ?
N7 Ni1 N3 N5 -119.7(4) . . . . ?
N2 Ni1 N3 N5 -23.3(4) . . . . ?
O2 Ni1 N3 N5 68.9(4) . . . . ?
N5 N3 N4 N6 0.0(4) . . . . ?
Ni1 N3 N4 N6 -176.4(2) . . . . ?
N5 N3 N4 Ni2 178.0(2) . . . . ?
Ni1 N3 N4 Ni2 1.7(4) . . . . ?
N8 Ni2 N4 N3 -56.3(3) . . . . ?
N8 Ni2 N4 N3 123.7(3) 2_665 . . . ?
N4 Ni2 N4 N3 141(100) 2_665 . . . ?
O1 Ni2 N4 N3 -154.2(3) 2_665 . . . ?
O1 Ni2 N4 N3 25.8(3) . . . . ?
N8 Ni2 N4 N6 121.4(3) . . . . ?
N8 Ni2 N4 N6 -58.6(3) 2_665 . . . ?
N4 Ni2 N4 N6 -41(100) 2_665 . . . ?
O1 Ni2 N4 N6 23.4(3) 2_665 . . . ?
O1 Ni2 N4 N6 -156.6(3) . . . . ?
N4 N3 N5 C12 -0.7(4) . . . . ?
Ni1 N3 N5 C12 174.9(3) . . . . ?
N3 N4 N6 C12 0.8(4) . . . . ?
Ni2 N4 N6 C12 -177.0(3) . . . . ?
N1 Ni1 N7 N8 114.7(3) . . . . ?
N3 Ni1 N7 N8 -63.8(3) . . . . ?
O1 Ni1 N7 N8 24.6(2) . . . . ?
N2 Ni1 N7 N8 -162.3(2) . . . . ?
O2 Ni1 N7 N8 25.2(9) . . . . ?
N1 Ni1 N7 N9 -51.9(4) . . . . ?
N3 Ni1 N7 N9 129.6(3) . . . . ?
O1 Ni1 N7 N9 -142.1(3) . . . . ?
N2 Ni1 N7 N9 31.1(4) . . . . ?
O2 Ni1 N7 N9 -141.4(7) . . . . ?
N9 N7 N8 N10 0.4(4) . . . . ?
Ni1 N7 N8 N10 -169.2(2) . . . . ?
N9 N7 N8 Ni2 180.0(2) . . . . ?
Ni1 N7 N8 Ni2 10.3(3) . . . . ?
N8 Ni2 N8 N7 -129(100) 2_665 . . . ?
N4 Ni2 N8 N7 47.1(3) . . . . ?
N4 Ni2 N8 N7 -132.9(3) 2_665 . . . ?
O1 Ni2 N8 N7 141.6(3) 2_665 . . . ?
O1 Ni2 N8 N7 -38.4(3) . . . . ?
N8 Ni2 N8 N10 50(100) 2_665 . . . ?
N4 Ni2 N8 N10 -133.5(3) . . . . ?
N4 Ni2 N8 N10 46.5(3) 2_665 . . . ?
O1 Ni2 N8 N10 -39.0(3) 2_665 . . . ?
O1 Ni2 N8 N10 141.0(3) . . . . ?
N8 N7 N9 C19 -0.4(4) . . . . ?
Ni1 N7 N9 C19 166.9(3) . . . . ?
N7 N8 N10 C19 -0.3(4) . . . . ?
Ni2 N8 N10 C19 -179.8(3) . . . . ?
Ni1 O1 C1 C2 156.1(3) . . . . ?
Ni2 O1 C1 C2 -40.8(5) . . . . ?
Ni1 O1 C1 C6 -22.4(5) . . . . ?
Ni2 O1 C1 C6 140.8(3) . . . . ?
O1 C1 C2 C3 179.1(4) . . . . ?
C6 C1 C2 C3 -2.3(7) . . . . ?
C1 C2 C3 C4 -0.7(8) . . . . ?
C2 C3 C4 C5 1.8(9) . . . . ?
C2 C3 C4 Cl1 -177.7(4) . . . . ?
C3 C4 C5 C6 0.3(9) . . . . ?
Cl1 C4 C5 C6 179.8(4) . . . . ?
C4 C5 C6 C1 -3.3(7) . . . . ?
C4 C5 C6 C7 175.5(5) . . . . ?
O1 C1 C6 C5 -177.3(4) . . . . ?
C2 C1 C6 C5 4.2(6) . . . . ?
O1 C1 C6 C7 4.0(6) . . . . ?
C2 C1 C6 C7 -174.5(4) . . . . ?
C8A N1 C7 C6 161.1(7) . . . . ?
C8 N1 C7 C6 -176.2(8) . . . . ?
Ni1 N1 C7 C6 4.7(7) . . . . ?
C5 C6 C7 N1 -172.7(5) . . . . ?
C1 C6 C7 N1 6.1(8) . . . . ?
C7 N1 C8A C9 165.4(7) . . . . ?
C8 N1 C8A C9 52(4) . . . . ?
Ni1 N1 C8A C9 -35.6(10) . . . . ?
C11 N2 C9 C8A -167.1(9) . . . . ?
C10 N2 C9 C8A 76.2(10) . . . . ?
C9A N2 C9 C8A 46.4(13) . . . . ?
Ni1 N2 C9 C8A -50.3(9) . . . . ?
N1 C8A C9 N2 58.4(11) . . . . ?
C7 N1 C8 C9A -137.3(13) . . . . ?
C8A N1 C8 C9A -60(4) . . . . ?
Ni1 N1 C8 C9A 41.8(15) . . . . ?
N1 C8 C9A N2 -53.9(17) . . . . ?
C11 N2 C9A C8 -95.1(14) . . . . ?
C10 N2 C9A C8 153.5(13) . . . . ?
C9 N2 C9A C8 -51.7(13) . . . . ?
Ni1 N2 C9A C8 40.0(14) . . . . ?
N4 N6 C12 N5 -1.3(5) . . . . ?
N4 N6 C12 C13 175.4(4) . . . . ?
N3 N5 C12 N6 1.3(5) . . . . ?
N3 N5 C12 C13 -175.4(4) . . . . ?
N6 C12 C13 C18 -26.3(7) . . . . ?
N5 C12 C13 C18 150.0(4) . . . . ?
N6 C12 C13 C14 156.0(4) . . . . ?
N5 C12 C13 C14 -27.7(7) . . . . ?
C18 C13 C14 C15 0.8(7) . . . . ?
C12 C13 C14 C15 178.5(4) . . . . ?
C13 C14 C15 C16 0.4(8) . . . . ?
C14 C15 C16 C17 -1.7(9) . . . . ?
C15 C16 C17 C18 1.8(9) . . . . ?
C14 C13 C18 C17 -0.7(7) . . . . ?
C12 C13 C18 C17 -178.4(4) . . . . ?
C16 C17 C18 C13 -0.6(8) . . . . ?
N8 N10 C19 N9 0.0(4) . . . . ?
N8 N10 C19 C20 178.6(4) . . . . ?
N7 N9 C19 N10 0.2(4) . . . . ?
N7 N9 C19 C20 -178.4(4) . . . . ?
N10 C19 C20 C21 145.7(4) . . . . ?
N9 C19 C20 C21 -35.8(6) . . . . ?
N10 C19 C20 C25 -35.8(6) . . . . ?
N9 C19 C20 C25 142.7(4) . . . . ?
C25 C20 C21 C22 0.4(7) . . . . ?
C19 C20 C21 C22 178.9(4) . . . . ?
C20 C21 C22 C23 -0.3(8) . . . . ?
C21 C22 C23 C24 -0.6(9) . . . . ?
C22 C23 C24 C25 1.2(9) . . . . ?
C21 C20 C25 C24 0.2(7) . . . . ?
C19 C20 C25 C24 -178.3(4) . . . . ?
C23 C24 C25 C20 -1.1(8) . . . . ?
Ni1 O2 C28 N11 146.1(4) . . . . ?
C26 N11 C28 O2 -4.0(8) . . . . ?
C27 N11 C28 O2 -175.8(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.929
_refine_diff_density_min         -0.855
_refine_diff_density_rms         0.088
_database_code_depnum_ccdc_archive 'CCDC 961049'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_4b

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H58 Cl2 N26 Ni3 O4'
_chemical_formula_weight         1358.27

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                   15.6896(18)
_cell_length_b                   15.8934(17)
_cell_length_c                   16.5290(15)
_cell_angle_alpha                76.751(9)
_cell_angle_beta                 89.705(9)
_cell_angle_gamma                69.725(10)
_cell_volume                     3750.9(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6979
_cell_measurement_theta_min      3.1405
_cell_measurement_theta_max      26.3142

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1404
_exptl_absorpt_coefficient_mu    0.871
_exptl_absorpt_correction_T_min  0.8248
_exptl_absorpt_correction_T_max  0.8952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Micro-Focus (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'OXFORD DIFFRACTION SUPER NOVA'
_diffrn_measurement_method       ω/q-scan
_diffrn_detector_area_resol_mean 15.9948
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            30207
_diffrn_reflns_av_R_equivalents  0.0830
_diffrn_reflns_av_unetI/netI     0.1039
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.15
_diffrn_reflns_theta_max         25.00
_reflns_number_total             13183
_reflns_number_gt                8092
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.,'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.,'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.,'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Ortep3
_computing_publication_material  Shelx97

_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)+(0.1290P)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    RIDING
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         13183
_refine_ls_number_parameters     833
_refine_ls_number_restraints     78
_refine_ls_R_factor_all          0.1108
_refine_ls_R_factor_gt           0.0780
_refine_ls_wR_factor_ref         0.2328
_refine_ls_wR_factor_gt          0.2066
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_restrained_S_all      0.965
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.92118(4) 0.86674(5) 0.14347(4) 0.0446(2) Uani 1 1 d . A .
Ni2 Ni 1.0000 1.0000 0.0000 0.0400(2) Uani 1 2 d S . .
Ni3 Ni 0.5000 0.0000 0.5000 0.0399(2) Uani 1 2 d S . .
Ni4 Ni 0.32873(4) 0.13360(5) 0.35728(4) 0.0454(2) Uani 1 1 d . . .
Cl1 Cl 1.37221(11) 0.78689(16) 0.32578(13) 0.0923(6) Uani 1 1 d . . .
Cl2 Cl 0.73208(13) 0.20656(16) 0.17792(13) 0.0922(6) Uani 1 1 d . . .
O1 O 1.0234(2) 0.9208(2) 0.1240(2) 0.0438(8) Uani 1 1 d . . .
O2 O 0.9031(3) 0.9130(3) 0.2558(2) 0.0613(11) Uani 1 1 d . . .
O3 O 0.4683(2) 0.0779(2) 0.3745(2) 0.0451(8) Uani 1 1 d . . .
O4 O 0.3392(3) 0.0852(3) 0.2454(3) 0.0632(11) Uani 1 1 d . . .
N1 N 1.0098(4) 0.7465(3) 0.2059(3) 0.0641(14) Uani 1 1 d . . .
N2 N 0.8239(3) 0.7980(4) 0.1780(4) 0.0670(15) Uani 1 1 d . . .
N3 N 0.8312(3) 0.9913(3) 0.0775(3) 0.0482(11) Uani 1 1 d . . .
N4 N 0.8630(3) 1.0454(3) 0.0234(3) 0.0439(10) Uani 1 1 d . A .
N5 N 0.7955(3) 1.1205(3) -0.0153(3) 0.0510(11) Uani 1 1 d . . .
N6 N 0.7412(3) 1.0288(3) 0.0744(3) 0.0540(12) Uani 1 1 d . A .
N7 N 0.4692(5) 1.2298(6) 0.0129(6) 0.121(3) Uani 1 1 d U . .
N8 N 0.9556(3) 0.8278(3) 0.0304(3) 0.0459(10) Uani 1 1 d . . .
N9 N 0.9904(3) 0.8786(3) -0.0244(3) 0.0444(10) Uani 1 1 d . A .
N10 N 0.9659(3) 0.7502(3) 0.0088(3) 0.0523(11) Uani 1 1 d . A .
N11 N 1.0243(3) 0.8348(3) -0.0836(3) 0.0500(11) Uani 1 1 d . . .
N12 N 1.1165(5) 0.6127(5) -0.2114(5) 0.096(2) Uani 1 1 d . . .
N13 N 0.9291(3) 1.0025(4) 0.3336(3) 0.0670(14) Uani 1 1 d . . .
N14 N 0.3341(3) 0.2511(3) 0.2879(3) 0.0613(13) Uani 1 1 d . . .
N15 N 0.1848(3) 0.2059(4) 0.3316(3) 0.0649(14) Uani 1 1 d . . .
N16 N 0.5916(3) -0.1213(3) 0.4764(3) 0.0461(10) Uani 1 1 d . . .
N17 N 0.6610(3) -0.1739(3) 0.5313(3) 0.0509(11) Uani 1 1 d . . .
N18 N 0.5877(3) -0.1644(3) 0.4160(3) 0.0500(11) Uani 1 1 d . . .
N19 N 0.7039(3) -0.2516(3) 0.5085(3) 0.0538(12) Uani 1 1 d . . .
N20 N 0.7877(5) -0.4525(4) 0.3648(5) 0.091(2) Uani 1 1 d . . .
N21 N 0.6056(3) 0.0440(3) 0.5215(3) 0.0445(10) Uani 1 1 d . . .
N22 N 0.6756(3) -0.0109(3) 0.5749(3) 0.0459(10) Uani 1 1 d . . .
N23 N 0.7400(3) 0.0277(3) 0.5714(3) 0.0524(12) Uani 1 1 d . . .
N24 N 0.6208(3) 0.1194(3) 0.4823(3) 0.0482(11) Uani 1 1 d . . .
N25 N 0.8678(4) 0.2333(5) 0.5047(5) 0.101(2) Uani 1 1 d . . .
N26 N 0.4253(4) -0.0047(4) 0.1673(3) 0.0735(15) Uani 1 1 d . . .
C1 C 1.0989(3) 0.8892(4) 0.1730(3) 0.0432(12) Uani 1 1 d . A .
C2 C 1.1473(4) 0.9472(4) 0.1805(4) 0.0540(14) Uani 1 1 d . . .
H2 H 1.1219 1.0107 0.1521 0.065 Uiso 1 1 calc R . .
C3 C 1.2289(4) 0.9169(5) 0.2265(4) 0.0594(15) Uani 1 1 d . . .
H3 H 1.2598 0.9583 0.2289 0.071 Uiso 1 1 calc R . .
C4 C 1.2655(4) 0.8264(5) 0.2691(4) 0.0645(17) Uani 1 1 d . . .
C5 C 1.2200(4) 0.7679(5) 0.2681(4) 0.0640(16) Uani 1 1 d . A .
H5 H 1.2459 0.7054 0.2990 0.077 Uiso 1 1 calc R . .
C6 C 1.1358(4) 0.7978(4) 0.2226(3) 0.0506(13) Uani 1 1 d . . .
C7 C 1.0905(4) 0.7297(5) 0.2313(4) 0.0665(17) Uani 1 1 d . A .
H7 H 1.1254 0.6676 0.2585 0.080 Uiso 1 1 calc R . .
C8 C 0.9740(11) 0.668(2) 0.2163(12) 0.055(4) Uani 0.50 1 d PDU A 1
H8A H 0.9669 0.6525 0.1624 0.066 Uiso 0.50 1 calc PR A 1
H8B H 1.0140 0.6114 0.2567 0.066 Uiso 0.50 1 calc PR A 1
C9 C 0.8862(10) 0.7078(12) 0.2481(8) 0.057(4) Uani 0.50 1 d PDU A 1
H9A H 0.8951 0.7257 0.3000 0.069 Uiso 0.50 1 calc PR A 1
H9B H 0.8555 0.6619 0.2609 0.069 Uiso 0.50 1 calc PR A 1
C8A C 0.9647(19) 0.682(2) 0.240(2) 0.161(14) Uani 0.50 1 d PDU A 2
H8A1 H 0.9596 0.6801 0.2999 0.194 Uiso 0.50 1 calc PR A 2
H8A2 H 1.0042 0.6200 0.2352 0.194 Uiso 0.50 1 calc PR A 2
C9A C 0.8743(16) 0.7017(19) 0.202(2) 0.194(15) Uani 0.50 1 d PDU A 2
H9A1 H 0.8803 0.6762 0.1517 0.232 Uiso 0.50 1 calc PR A 2
H9A2 H 0.8408 0.6708 0.2415 0.232 Uiso 0.50 1 calc PR A 2
C10 C 0.7755(6) 0.7902(8) 0.1070(6) 0.117(4) Uani 1 1 d . A .
H10A H 0.8195 0.7568 0.0726 0.176 Uiso 1 1 calc R . .
H10B H 0.7395 0.8521 0.0736 0.176 Uiso 1 1 calc R . .
H10C H 0.7348 0.7562 0.1269 0.176 Uiso 1 1 calc R . .
C11 C 0.7554(5) 0.8429(6) 0.2302(5) 0.092(3) Uani 1 1 d . A .
H11A H 0.7186 0.9055 0.1988 0.138 Uiso 1 1 calc R . .
H11B H 0.7860 0.8463 0.2803 0.138 Uiso 1 1 calc R . .
H11C H 0.7158 0.8069 0.2465 0.138 Uiso 1 1 calc R . .
C12 C 0.7214(3) 1.1095(4) 0.0169(3) 0.0507(13) Uani 1 1 d . A .
C13 C 0.6291(4) 1.1741(5) -0.0082(4) 0.0634(16) Uani 1 1 d U . .
C14 C 0.6080(5) 1.2420(6) -0.0829(5) 0.092(2) Uani 1 1 d U A .
H14 H 0.6561 1.2459 -0.1170 0.110 Uiso 1 1 calc R . .
C15 C 0.5241(5) 1.3015(6) -0.1090(6) 0.109(3) Uani 1 1 d U . .
H15 H 0.5128 1.3476 -0.1598 0.130 Uiso 1 1 calc R A .
C16 C 0.4573(6) 1.2949(7) -0.0628(7) 0.125(4) Uani 1 1 d U A .
H16 H 0.3974 1.3369 -0.0820 0.150 Uiso 1 1 calc R . .
C17 C 0.5565(4) 1.1692(5) 0.0403(5) 0.080(2) Uani 1 1 d U A .
H17 H 0.5675 1.1243 0.0918 0.096 Uiso 1 1 calc R . .
C18 C 1.0083(3) 0.7558(4) -0.0606(3) 0.0475(13) Uani 1 1 d . A .
C19 C 1.0341(4) 0.6825(4) -0.1054(3) 0.0502(13) Uani 1 1 d . . .
C20 C 0.9986(5) 0.6137(4) -0.0867(4) 0.0680(18) Uani 1 1 d . A .
H20 H 0.9570 0.6134 -0.0447 0.082 Uiso 1 1 calc R . .
C21 C 1.0239(6) 0.5432(5) -0.1300(5) 0.089(2) Uani 1 1 d . . .
H21 H 1.0009 0.4941 -0.1173 0.106 Uiso 1 1 calc R A .
C22 C 1.0803(6) 0.5473(5) -0.1887(5) 0.093(3) Uani 1 1 d . A .
H22 H 1.0968 0.4993 -0.2174 0.112 Uiso 1 1 calc R . .
C23 C 1.0915(4) 0.6798(4) -0.1678(4) 0.0664(17) Uani 1 1 d . A .
H23 H 1.1157 0.7279 -0.1820 0.080 Uiso 1 1 calc R . .
C24 C 0.9252(4) 0.9783(4) 0.2624(4) 0.0581(15) Uani 1 1 d . . .
H24 H 0.9403 1.0136 0.2137 0.070 Uiso 1 1 calc R . .
C25 C 0.9075(5) 0.9508(6) 0.4107(4) 0.090(2) Uani 1 1 d . . .
H25A H 0.8796 0.9085 0.3978 0.135 Uiso 1 1 calc R . .
H25B H 0.8649 0.9939 0.4389 0.135 Uiso 1 1 calc R . .
H25C H 0.9636 0.9153 0.4471 0.135 Uiso 1 1 calc R . .
C26 C 0.9565(6) 1.0808(7) 0.3366(6) 0.108(3) Uani 1 1 d . . .
H26A H 0.9786 1.1021 0.2830 0.162 Uiso 1 1 calc R . .
H26B H 1.0053 1.0616 0.3811 0.162 Uiso 1 1 calc R . .
H26C H 0.9041 1.1312 0.3476 0.162 Uiso 1 1 calc R . .
C27 C 0.5248(3) 0.1080(4) 0.3259(3) 0.0428(12) Uani 1 1 d . B .
C28 C 0.6137(4) 0.0494(4) 0.3218(4) 0.0552(14) Uani 1 1 d . . .
H28 H 0.6323 -0.0136 0.3517 0.066 Uiso 1 1 calc R . .
C29 C 0.6748(4) 0.0795(5) 0.2760(4) 0.0620(16) Uani 1 1 d . . .
H29 H 0.7351 0.0379 0.2753 0.074 Uiso 1 1 calc R . .
C30 C 0.6494(4) 0.1691(5) 0.2313(4) 0.0636(17) Uani 1 1 d . . .
C31 C 0.5636(4) 0.2279(5) 0.2287(4) 0.0624(16) Uani 1 1 d . B .
H31 H 0.5472 0.2899 0.1967 0.075 Uiso 1 1 calc R . .
C32 C 0.4972(4) 0.1989(4) 0.2730(3) 0.0545(14) Uani 1 1 d . . .
C33 C 0.4048(4) 0.2655(4) 0.2581(4) 0.0643(17) Uani 1 1 d . B .
H33 H 0.3959 0.3248 0.2232 0.077 Uiso 1 1 calc R . .
C34 C 0.250(2) 0.330(3) 0.2807(19) 0.076(8) Uani 0.40 1 d PDU B 1
H34A H 0.2470 0.3803 0.2310 0.091 Uiso 0.40 1 calc PR B 1
H34B H 0.2441 0.3551 0.3311 0.091 Uiso 0.40 1 calc PR B 1
C35 C 0.1784(16) 0.2892(17) 0.272(2) 0.091(8) Uani 0.40 1 d PDU B 1
H35A H 0.1182 0.3364 0.2748 0.109 Uiso 0.40 1 calc PR B 1
H35B H 0.1796 0.2772 0.2159 0.109 Uiso 0.40 1 calc PR B 1
C34A C 0.2423(12) 0.3165(14) 0.2508(10) 0.068(5) Uani 0.60 1 d PDU B 2
H34C H 0.2259 0.3016 0.1995 0.082 Uiso 0.60 1 calc PR B 2
H34D H 0.2419 0.3807 0.2362 0.082 Uiso 0.60 1 calc PR B 2
C35A C 0.1747(8) 0.3073(9) 0.3151(9) 0.063(4) Uani 0.60 1 d PDU B 2
H35C H 0.1118 0.3481 0.2928 0.076 Uiso 0.60 1 calc PR B 2
H35D H 0.1899 0.3226 0.3666 0.076 Uiso 0.60 1 calc PR B 2
C36 C 0.1455(5) 0.1679(6) 0.2716(5) 0.093(3) Uani 1 1 d . B .
H36A H 0.1572 0.1021 0.2954 0.140 Uiso 1 1 calc R . .
H36B H 0.1740 0.1753 0.2188 0.140 Uiso 1 1 calc R . .
H36C H 0.0795 0.2014 0.2614 0.140 Uiso 1 1 calc R . .
C37 C 0.1326(4) 0.1986(6) 0.4046(5) 0.094(3) Uani 1 1 d . B .
H37A H 0.1523 0.2256 0.4454 0.141 Uiso 1 1 calc R . .
H37B H 0.1430 0.1334 0.4297 0.141 Uiso 1 1 calc R . .
H37C H 0.0676 0.2320 0.3878 0.141 Uiso 1 1 calc R . .
C38 C 0.6566(4) -0.2442(4) 0.4384(3) 0.0496(13) Uani 1 1 d . . .
C39 C 0.6793(4) -0.3166(4) 0.3921(4) 0.0507(13) Uani 1 1 d . . .
C40 C 0.6201(5) -0.3171(5) 0.3327(5) 0.0714(18) Uani 1 1 d . . .
H40 H 0.5616 -0.2698 0.3209 0.086 Uiso 1 1 calc R . .
C41 C 0.6433(6) -0.3843(5) 0.2899(5) 0.085(2) Uani 1 1 d . . .
H41 H 0.6019 -0.3840 0.2480 0.101 Uiso 1 1 calc R . .
C42 C 0.7260(6) -0.4509(5) 0.3082(5) 0.087(2) Uani 1 1 d . . .
H42 H 0.7414 -0.4991 0.2797 0.105 Uiso 1 1 calc R . .
C43 C 0.7622(4) -0.3863(4) 0.4055(4) 0.0703(18) Uani 1 1 d . . .
H43 H 0.8045 -0.3874 0.4470 0.084 Uiso 1 1 calc R . .
C44 C 0.7032(3) 0.1078(4) 0.5136(3) 0.0470(12) Uani 1 1 d . . .
C45 C 0.7498(4) 0.1736(4) 0.4856(4) 0.0594(15) Uani 1 1 d . . .
C46 C 0.7215(5) 0.2369(5) 0.4088(5) 0.080(2) Uani 1 1 d . . .
H46 H 0.6709 0.2400 0.3753 0.096 Uiso 1 1 calc R . .
C47 C 0.7697(6) 0.2951(6) 0.3829(6) 0.100(3) Uani 1 1 d . . .
H47 H 0.7518 0.3391 0.3307 0.120 Uiso 1 1 calc R . .
C48 C 0.8397(7) 0.2907(6) 0.4292(6) 0.101(3) Uani 1 1 d . . .
H48 H 0.8722 0.3305 0.4078 0.121 Uiso 1 1 calc R . .
C49 C 0.8226(4) 0.1742(5) 0.5316(5) 0.0704(18) Uani 1 1 d . . .
H49 H 0.8421 0.1315 0.5844 0.084 Uiso 1 1 calc R . .
C50 C 0.4054(4) 0.0192(5) 0.2375(4) 0.0585(15) Uani 1 1 d . . .
H50 H 0.4449 -0.0171 0.2859 0.070 Uiso 1 1 calc R . .
C51 C 0.5054(6) -0.0798(7) 0.1624(6) 0.118(3) Uani 1 1 d . . .
H51A H 0.5366 -0.0613 0.1137 0.177 Uiso 1 1 calc R . .
H51B H 0.4888 -0.1324 0.1569 0.177 Uiso 1 1 calc R . .
H51C H 0.5460 -0.0976 0.2131 0.177 Uiso 1 1 calc R . .
C52 C 0.3645(5) 0.0462(6) 0.0921(4) 0.096(3) Uani 1 1 d . . .
H52A H 0.3392 0.0050 0.0732 0.145 Uiso 1 1 calc R . .
H52B H 0.3987 0.0696 0.0483 0.145 Uiso 1 1 calc R . .
H52C H 0.3148 0.0983 0.1043 0.145 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 1.979(5) . ?
Ni1 N3 2.047(5) . ?
Ni1 O1 2.058(3) . ?
Ni1 N8 2.111(4) . ?
Ni1 O2 2.132(4) . ?
Ni1 N2 2.170(4) . ?
Ni2 N4 2.082(4) . ?
Ni2 N4 2.082(4) 2_775 ?
Ni2 O1 2.104(3) . ?
Ni2 O1 2.104(3) 2_775 ?
Ni2 N9 2.113(4) . ?
Ni2 N9 2.113(4) 2_775 ?
Ni3 N21 2.069(4) 2_656 ?
Ni3 N21 2.069(4) . ?
Ni3 N16 2.086(4) 2_656 ?
Ni3 N16 2.086(4) . ?
Ni3 O3 2.119(3) 2_656 ?
Ni3 O3 2.119(3) . ?
Ni4 N14 1.983(5) . ?
Ni4 N22 2.038(4) 2_656 ?
Ni4 O3 2.051(3) . ?
Ni4 N17 2.108(5) 2_656 ?
Ni4 N15 2.142(4) . ?
Ni4 O4 2.145(4) . ?
Cl1 C4 1.759(6) . ?
Cl2 C30 1.760(5) . ?
O1 C1 1.312(6) . ?
O2 C24 1.229(7) . ?
O3 C27 1.331(6) . ?
O4 C50 1.225(7) . ?
N1 C7 1.254(7) . ?
N1 C8A 1.45(3) . ?
N1 C8 1.52(3) . ?
N2 C9A 1.42(3) . ?
N2 C10 1.453(10) . ?
N2 C11 1.467(9) . ?
N2 C9 1.623(17) . ?
N3 N4 1.316(6) . ?
N3 N6 1.325(6) . ?
N4 N5 1.317(6) . ?
N5 C12 1.325(6) . ?
N6 C12 1.346(7) . ?
N7 C17 1.379(10) . ?
N7 C16 1.394(12) . ?
N8 N10 1.317(6) . ?
N8 N9 1.319(5) . ?
N9 N11 1.332(6) . ?
N10 C18 1.324(7) . ?
N11 C18 1.336(7) . ?
N12 C22 1.330(9) . ?
N12 C23 1.367(8) . ?
N13 C24 1.327(8) . ?
N13 C25 1.456(8) . ?
N13 C26 1.461(9) . ?
N14 C33 1.283(7) . ?
N14 C34 1.46(4) . ?
N14 C34A 1.49(2) . ?
N15 C35 1.43(3) . ?
N15 C37 1.460(8) . ?
N15 C36 1.507(9) . ?
N15 C35A 1.522(15) . ?
N16 N17 1.319(6) . ?
N16 N18 1.347(6) . ?
N17 N19 1.324(6) . ?
N17 Ni4 2.108(5) 2_656 ?
N18 C38 1.324(7) . ?
N19 C38 1.339(7) . ?
N20 C43 1.322(9) . ?
N20 C42 1.340(10) . ?
N21 N22 1.320(6) . ?
N21 N24 1.324(6) . ?
N22 N23 1.346(6) . ?
N22 Ni4 2.038(4) 2_656 ?
N23 C44 1.344(7) . ?
N24 C44 1.331(7) . ?
N25 C48 1.338(11) . ?
N25 C49 1.360(8) . ?
N26 C50 1.306(8) . ?
N26 C51 1.419(9) . ?
N26 C52 1.458(9) . ?
C1 C2 1.407(7) . ?
C1 C6 1.413(7) . ?
C2 C3 1.365(8) . ?
C2 H2 0.9500 . ?
C3 C4 1.365(9) . ?
C3 H3 0.9500 . ?
C4 C5 1.357(9) . ?
C5 C6 1.396(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.468(8) . ?
C7 H7 0.9500 . ?
C8 C9 1.455(17) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C8A C9A 1.457(18) . ?
C8A H8A1 0.9900 . ?
C8A H8A2 0.9900 . ?
C9A H9A1 0.9900 . ?
C9A H9A2 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.451(8) . ?
C13 C14 1.394(10) . ?
C13 C17 1.403(9) . ?
C14 C15 1.330(10) . ?
C14 H14 0.9500 . ?
C15 C16 1.314(12) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 C19 1.462(8) . ?
C19 C23 1.364(8) . ?
C19 C20 1.366(8) . ?
C20 C21 1.407(9) . ?
C20 H20 0.9500 . ?
C21 C22 1.315(10) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.394(7) . ?
C27 C32 1.425(8) . ?
C28 C29 1.366(7) . ?
C28 H28 0.9500 . ?
C29 C30 1.364(9) . ?
C29 H29 0.9500 . ?
C30 C31 1.341(9) . ?
C31 C32 1.417(7) . ?
C31 H31 0.9500 . ?
C32 C33 1.450(8) . ?
C33 H33 0.9500 . ?
C34 C35 1.505(18) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C34A C35A 1.516(15) . ?
C34A H34C 0.9900 . ?
C34A H34D 0.9900 . ?
C35A H35C 0.9900 . ?
C35A H35D 0.9900 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C39 1.468(8) . ?
C39 C40 1.357(9) . ?
C39 C43 1.364(8) . ?
C40 C41 1.358(9) . ?
C40 H40 0.9500 . ?
C41 C42 1.342(10) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C43 H43 0.9500 . ?
C44 C45 1.465(8) . ?
C45 C49 1.380(9) . ?
C45 C46 1.389(9) . ?
C46 C47 1.382(9) . ?
C46 H46 0.9500 . ?
C47 C48 1.315(12) . ?
C47 H47 0.9500 . ?
C48 H48 0.9500 . ?
C49 H49 0.9500 . ?
C50 H50 0.9500 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N3 179.01(19) . . ?
N1 Ni1 O1 90.58(17) . . ?
N3 Ni1 O1 88.66(15) . . ?
N1 Ni1 N8 89.8(2) . . ?
N3 Ni1 N8 89.47(17) . . ?
O1 Ni1 N8 84.56(15) . . ?
N1 Ni1 O2 89.6(2) . . ?
N3 Ni1 O2 90.99(18) . . ?
O1 Ni1 O2 86.97(14) . . ?
N8 Ni1 O2 171.50(15) . . ?
N1 Ni1 N2 83.0(2) . . ?
N3 Ni1 N2 97.82(19) . . ?
O1 Ni1 N2 172.78(19) . . ?
N8 Ni1 N2 98.61(19) . . ?
O2 Ni1 N2 89.74(19) . . ?
N4 Ni2 N4 180.0(2) . 2_775 ?
N4 Ni2 O1 85.69(14) . . ?
N4 Ni2 O1 94.31(14) 2_775 . ?
N4 Ni2 O1 94.31(14) . 2_775 ?
N4 Ni2 O1 85.69(14) 2_775 2_775 ?
O1 Ni2 O1 180.0(2) . 2_775 ?
N4 Ni2 N9 90.76(16) . . ?
N4 Ni2 N9 89.24(16) 2_775 . ?
O1 Ni2 N9 82.57(15) . . ?
O1 Ni2 N9 97.43(15) 2_775 . ?
N4 Ni2 N9 89.24(16) . 2_775 ?
N4 Ni2 N9 90.76(16) 2_775 2_775 ?
O1 Ni2 N9 97.43(15) . 2_775 ?
O1 Ni2 N9 82.57(15) 2_775 2_775 ?
N9 Ni2 N9 180.0(2) . 2_775 ?
N21 Ni3 N21 180.00(9) 2_656 . ?
N21 Ni3 N16 91.10(17) 2_656 2_656 ?
N21 Ni3 N16 88.90(17) . 2_656 ?
N21 Ni3 N16 88.90(17) 2_656 . ?
N21 Ni3 N16 91.10(17) . . ?
N16 Ni3 N16 180.000(1) 2_656 . ?
N21 Ni3 O3 94.65(15) 2_656 2_656 ?
N21 Ni3 O3 85.35(15) . 2_656 ?
N16 Ni3 O3 97.18(15) 2_656 2_656 ?
N16 Ni3 O3 82.82(15) . 2_656 ?
N21 Ni3 O3 85.35(15) 2_656 . ?
N21 Ni3 O3 94.65(15) . . ?
N16 Ni3 O3 82.82(15) 2_656 . ?
N16 Ni3 O3 97.18(15) . . ?
O3 Ni3 O3 180.000(1) 2_656 . ?
N14 Ni4 N22 178.0(2) . 2_656 ?
N14 Ni4 O3 90.90(16) . . ?
N22 Ni4 O3 88.69(15) 2_656 . ?
N14 Ni4 N17 92.2(2) . 2_656 ?
N22 Ni4 N17 89.72(18) 2_656 2_656 ?
O3 Ni4 N17 84.23(16) . 2_656 ?
N14 Ni4 N15 82.63(19) . . ?
N22 Ni4 N15 97.78(18) 2_656 . ?
O3 Ni4 N15 173.52(17) . . ?
N17 Ni4 N15 95.7(2) 2_656 . ?
N14 Ni4 O4 87.4(2) . . ?
N22 Ni4 O4 90.60(17) 2_656 . ?
O3 Ni4 O4 87.58(15) . . ?
N17 Ni4 O4 171.79(16) 2_656 . ?
N15 Ni4 O4 92.4(2) . . ?
C1 O1 Ni1 123.3(3) . . ?
C1 O1 Ni2 127.8(3) . . ?
Ni1 O1 Ni2 106.51(15) . . ?
C24 O2 Ni1 120.2(3) . . ?
C27 O3 Ni4 125.0(3) . . ?
C27 O3 Ni3 125.9(3) . . ?
Ni4 O3 Ni3 106.12(14) . . ?
C50 O4 Ni4 120.6(4) . . ?
C7 N1 C8A 119.8(11) . . ?
C7 N1 C8 119.4(9) . . ?
C8A N1 C8 19.0(19) . . ?
C7 N1 Ni1 127.2(4) . . ?
C8A N1 Ni1 111.2(11) . . ?
C8 N1 Ni1 113.3(8) . . ?
C9A N2 C10 92.9(15) . . ?
C9A N2 C11 121.2(17) . . ?
C10 N2 C11 107.5(6) . . ?
C9A N2 C9 30.6(17) . . ?
C10 N2 C9 121.9(8) . . ?
C11 N2 C9 99.5(7) . . ?
C9A N2 Ni1 107.0(10) . . ?
C10 N2 Ni1 113.6(4) . . ?
C11 N2 Ni1 113.2(4) . . ?
C9 N2 Ni1 100.5(6) . . ?
N4 N3 N6 109.7(4) . . ?
N4 N3 Ni1 118.3(3) . . ?
N6 N3 Ni1 131.8(3) . . ?
N3 N4 N5 110.0(4) . . ?
N3 N4 Ni2 120.1(3) . . ?
N5 N4 Ni2 129.5(3) . . ?
N4 N5 C12 104.6(4) . . ?
N3 N6 C12 103.8(4) . . ?
C17 N7 C16 117.6(7) . . ?
N10 N8 N9 109.6(4) . . ?
N10 N8 Ni1 131.1(3) . . ?
N9 N8 Ni1 117.8(3) . . ?
N8 N9 N11 109.6(4) . . ?
N8 N9 Ni2 119.2(3) . . ?
N11 N9 Ni2 130.7(3) . . ?
N8 N10 C18 104.8(4) . . ?
N9 N11 C18 103.7(4) . . ?
C22 N12 C23 114.9(6) . . ?
C24 N13 C25 120.8(6) . . ?
C24 N13 C26 120.6(6) . . ?
C25 N13 C26 118.6(6) . . ?
C33 N14 C34 118.1(12) . . ?
C33 N14 C34A 118.9(7) . . ?
C34 N14 C34A 24.0(12) . . ?
C33 N14 Ni4 127.0(4) . . ?
C34 N14 Ni4 114.3(12) . . ?
C34A N14 Ni4 111.8(6) . . ?
C35 N15 C37 126.3(13) . . ?
C35 N15 C36 95.0(12) . . ?
C37 N15 C36 104.9(5) . . ?
C35 N15 C35A 32.0(11) . . ?
C37 N15 C35A 100.0(7) . . ?
C36 N15 C35A 122.8(8) . . ?
C35 N15 Ni4 103.4(10) . . ?
C37 N15 Ni4 114.2(4) . . ?
C36 N15 Ni4 111.0(4) . . ?
C35A N15 Ni4 103.8(5) . . ?
N17 N16 N18 109.7(4) . . ?
N17 N16 Ni3 119.6(4) . . ?
N18 N16 Ni3 130.3(3) . . ?
N16 N17 N19 109.3(5) . . ?
N16 N17 Ni4 117.8(3) . 2_656 ?
N19 N17 Ni4 132.0(3) . 2_656 ?
C38 N18 N16 103.9(4) . . ?
N17 N19 C38 104.8(4) . . ?
C43 N20 C42 116.7(6) . . ?
N22 N21 N24 110.1(4) . . ?
N22 N21 Ni3 120.1(3) . . ?
N24 N21 Ni3 129.3(3) . . ?
N21 N22 N23 109.5(4) . . ?
N21 N22 Ni4 118.4(3) . 2_656 ?
N23 N22 Ni4 132.1(3) . 2_656 ?
C44 N23 N22 103.4(4) . . ?
N21 N24 C44 104.5(4) . . ?
C48 N25 C49 116.6(7) . . ?
C50 N26 C51 121.3(7) . . ?
C50 N26 C52 119.8(6) . . ?
C51 N26 C52 118.8(7) . . ?
O1 C1 C2 120.8(5) . . ?
O1 C1 C6 123.5(5) . . ?
C2 C1 C6 115.6(5) . . ?
C3 C2 C1 123.3(6) . . ?
C3 C2 H2 118.3 . . ?
C1 C2 H2 118.3 . . ?
C4 C3 C2 119.2(6) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C5 C4 C3 120.5(6) . . ?
C5 C4 Cl1 120.5(5) . . ?
C3 C4 Cl1 119.0(5) . . ?
C4 C5 C6 121.3(6) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C5 C6 C1 119.8(5) . . ?
C5 C6 C7 116.0(5) . . ?
C1 C6 C7 124.2(5) . . ?
N1 C7 C6 125.7(6) . . ?
N1 C7 H7 117.2 . . ?
C6 C7 H7 117.2 . . ?
C9 C8 N1 100.7(18) . . ?
C9 C8 H8A 111.6 . . ?
N1 C8 H8A 111.6 . . ?
C9 C8 H8B 111.6 . . ?
N1 C8 H8B 111.6 . . ?
H8A C8 H8B 109.4 . . ?
C8 C9 N2 108.8(14) . . ?
C8 C9 H9A 109.9 . . ?
N2 C9 H9A 109.9 . . ?
C8 C9 H9B 109.9 . . ?
N2 C9 H9B 109.9 . . ?
H9A C9 H9B 108.3 . . ?
N1 C8A C9A 117(3) . . ?
N1 C8A H8A1 108.1 . . ?
C9A C8A H8A1 108.1 . . ?
N1 C8A H8A2 108.1 . . ?
C9A C8A H8A2 108.1 . . ?
H8A1 C8A H8A2 107.3 . . ?
N2 C9A C8A 112(2) . . ?
N2 C9A H9A1 109.3 . . ?
C8A C9A H9A1 109.3 . . ?
N2 C9A H9A2 109.3 . . ?
C8A C9A H9A2 109.3 . . ?
H9A1 C9A H9A2 108.0 . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C11 H11A 109.5 . . ?
N2 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N2 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N5 C12 N6 111.9(5) . . ?
N5 C12 C13 124.8(5) . . ?
N6 C12 C13 123.2(5) . . ?
C14 C13 C17 117.0(6) . . ?
C14 C13 C12 121.5(6) . . ?
C17 C13 C12 121.5(6) . . ?
C15 C14 C13 123.5(8) . . ?
C15 C14 H14 118.3 . . ?
C13 C14 H14 118.3 . . ?
C16 C15 C14 118.3(9) . . ?
C16 C15 H15 120.9 . . ?
C14 C15 H15 120.9 . . ?
C15 C16 N7 123.9(8) . . ?
C15 C16 H16 118.0 . . ?
N7 C16 H16 118.0 . . ?
N7 C17 C13 119.8(7) . . ?
N7 C17 H17 120.1 . . ?
C13 C17 H17 120.1 . . ?
N10 C18 N11 112.3(5) . . ?
N10 C18 C19 122.7(5) . . ?
N11 C18 C19 125.0(5) . . ?
C23 C19 C20 117.1(6) . . ?
C23 C19 C18 123.0(5) . . ?
C20 C19 C18 119.9(5) . . ?
C19 C20 C21 119.6(6) . . ?
C19 C20 H20 120.2 . . ?
C21 C20 H20 120.2 . . ?
C22 C21 C20 118.1(7) . . ?
C22 C21 H21 121.0 . . ?
C20 C21 H21 121.0 . . ?
C21 C22 N12 125.8(7) . . ?
C21 C22 H22 117.1 . . ?
N12 C22 H22 117.1 . . ?
C19 C23 N12 124.5(6) . . ?
C19 C23 H23 117.8 . . ?
N12 C23 H23 117.8 . . ?
O2 C24 N13 123.8(6) . . ?
O2 C24 H24 118.1 . . ?
N13 C24 H24 118.1 . . ?
N13 C25 H25A 109.5 . . ?
N13 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
N13 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N13 C26 H26A 109.5 . . ?
N13 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
N13 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O3 C27 C28 120.8(5) . . ?
O3 C27 C32 122.4(4) . . ?
C28 C27 C32 116.8(4) . . ?
C29 C28 C27 122.1(6) . . ?
C29 C28 H28 118.9 . . ?
C27 C28 H28 118.9 . . ?
C30 C29 C28 120.2(5) . . ?
C30 C29 H29 119.9 . . ?
C28 C29 H29 119.9 . . ?
C31 C30 C29 120.9(5) . . ?
C31 C30 Cl2 120.5(5) . . ?
C29 C30 Cl2 118.6(5) . . ?
C30 C31 C32 120.8(6) . . ?
C30 C31 H31 119.6 . . ?
C32 C31 H31 119.6 . . ?
C31 C32 C27 118.7(5) . . ?
C31 C32 C33 115.7(5) . . ?
C27 C32 C33 125.6(4) . . ?
N14 C33 C32 125.6(5) . . ?
N14 C33 H33 117.2 . . ?
C32 C33 H33 117.2 . . ?
N14 C34 C35 102(2) . . ?
N14 C34 H34A 111.3 . . ?
C35 C34 H34A 111.3 . . ?
N14 C34 H34B 111.3 . . ?
C35 C34 H34B 111.3 . . ?
H34A C34 H34B 109.2 . . ?
N15 C35 C34 118(2) . . ?
N15 C35 H35A 107.9 . . ?
C34 C35 H35A 107.9 . . ?
N15 C35 H35B 107.9 . . ?
C34 C35 H35B 107.9 . . ?
H35A C35 H35B 107.2 . . ?
N14 C34A C35A 107.7(12) . . ?
N14 C34A H34C 110.2 . . ?
C35A C34A H34C 110.2 . . ?
N14 C34A H34D 110.2 . . ?
C35A C34A H34D 110.2 . . ?
H34C C34A H34D 108.5 . . ?
C34A C35A N15 103.6(12) . . ?
C34A C35A H35C 111.0 . . ?
N15 C35A H35C 111.0 . . ?
C34A C35A H35D 111.0 . . ?
N15 C35A H35D 111.0 . . ?
H35C C35A H35D 109.0 . . ?
N15 C36 H36A 109.5 . . ?
N15 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
N15 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N15 C37 H37A 109.5 . . ?
N15 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
N15 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N18 C38 N19 112.3(5) . . ?
N18 C38 C39 124.2(5) . . ?
N19 C38 C39 123.5(5) . . ?
C40 C39 C43 116.4(6) . . ?
C40 C39 C38 122.2(5) . . ?
C43 C39 C38 121.4(6) . . ?
C39 C40 C41 121.0(7) . . ?
C39 C40 H40 119.5 . . ?
C41 C40 H40 119.5 . . ?
C42 C41 C40 118.4(8) . . ?
C42 C41 H41 120.8 . . ?
C40 C41 H41 120.8 . . ?
N20 C42 C41 122.9(7) . . ?
N20 C42 H42 118.5 . . ?
C41 C42 H42 118.5 . . ?
N20 C43 C39 124.5(7) . . ?
N20 C43 H43 117.8 . . ?
C39 C43 H43 117.8 . . ?
N24 C44 N23 112.5(5) . . ?
N24 C44 C45 123.6(5) . . ?
N23 C44 C45 123.9(5) . . ?
C49 C45 C46 118.1(6) . . ?
C49 C45 C44 122.7(6) . . ?
C46 C45 C44 119.2(6) . . ?
C47 C46 C45 117.5(7) . . ?
C47 C46 H46 121.3 . . ?
C45 C46 H46 121.3 . . ?
C48 C47 C46 121.3(8) . . ?
C48 C47 H47 119.3 . . ?
C46 C47 H47 119.3 . . ?
C47 C48 N25 123.6(7) . . ?
C47 C48 H48 118.2 . . ?
N25 C48 H48 118.2 . . ?
N25 C49 C45 122.8(7) . . ?
N25 C49 H49 118.6 . . ?
C45 C49 H49 118.6 . . ?
O4 C50 N26 124.6(6) . . ?
O4 C50 H50 117.7 . . ?
N26 C50 H50 117.7 . . ?
N26 C51 H51A 109.5 . . ?
N26 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
N26 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
N26 C52 H52A 109.5 . . ?
N26 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
N26 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Ni1 O1 C1 -25.0(4) . . . . ?
N3 Ni1 O1 C1 155.6(4) . . . . ?
N8 Ni1 O1 C1 -114.8(4) . . . . ?
O2 Ni1 O1 C1 64.6(4) . . . . ?
N2 Ni1 O1 C1 1.6(16) . . . . ?
N1 Ni1 O1 Ni2 138.5(2) . . . . ?
N3 Ni1 O1 Ni2 -40.88(18) . . . . ?
N8 Ni1 O1 Ni2 48.72(17) . . . . ?
O2 Ni1 O1 Ni2 -131.94(18) . . . . ?
N2 Ni1 O1 Ni2 165.1(14) . . . . ?
N4 Ni2 O1 C1 -156.0(4) . . . . ?
N4 Ni2 O1 C1 24.0(4) 2_775 . . . ?
O1 Ni2 O1 C1 41(100) 2_775 . . . ?
N9 Ni2 O1 C1 112.7(4) . . . . ?
N9 Ni2 O1 C1 -67.3(4) 2_775 . . . ?
N4 Ni2 O1 Ni1 41.49(17) . . . . ?
N4 Ni2 O1 Ni1 -138.51(17) 2_775 . . . ?
O1 Ni2 O1 Ni1 -122(100) 2_775 . . . ?
N9 Ni2 O1 Ni1 -49.85(17) . . . . ?
N9 Ni2 O1 Ni1 130.15(17) 2_775 . . . ?
N1 Ni1 O2 C24 116.2(5) . . . . ?
N3 Ni1 O2 C24 -63.0(5) . . . . ?
O1 Ni1 O2 C24 25.6(5) . . . . ?
N8 Ni1 O2 C24 30.0(14) . . . . ?
N2 Ni1 O2 C24 -160.9(5) . . . . ?
N14 Ni4 O3 C27 -20.4(4) . . . . ?
N22 Ni4 O3 C27 157.6(4) 2_656 . . . ?
N17 Ni4 O3 C27 -112.6(4) 2_656 . . . ?
N15 Ni4 O3 C27 -23.3(18) . . . . ?
O4 Ni4 O3 C27 66.9(4) . . . . ?
N14 Ni4 O3 Ni3 140.9(2) . . . . ?
N22 Ni4 O3 Ni3 -41.07(19) 2_656 . . . ?
N17 Ni4 O3 Ni3 48.78(18) 2_656 . . . ?
N15 Ni4 O3 Ni3 138.1(16) . . . . ?
O4 Ni4 O3 Ni3 -131.72(18) . . . . ?
N21 Ni3 O3 C27 -156.8(4) 2_656 . . . ?
N21 Ni3 O3 C27 23.2(4) . . . . ?
N16 Ni3 O3 C27 111.5(4) 2_656 . . . ?
N16 Ni3 O3 C27 -68.5(4) . . . . ?
O3 Ni3 O3 C27 -17(100) 2_656 . . . ?
N21 Ni3 O3 Ni4 42.09(18) 2_656 . . . ?
N21 Ni3 O3 Ni4 -137.91(18) . . . . ?
N16 Ni3 O3 Ni4 -49.61(18) 2_656 . . . ?
N16 Ni3 O3 Ni4 130.39(18) . . . . ?
O3 Ni3 O3 Ni4 -178(100) 2_656 . . . ?
N14 Ni4 O4 C50 116.2(5) . . . . ?
N22 Ni4 O4 C50 -63.4(4) 2_656 . . . ?
O3 Ni4 O4 C50 25.2(4) . . . . ?
N17 Ni4 O4 C50 28.7(14) 2_656 . . . ?
N15 Ni4 O4 C50 -161.3(5) . . . . ?
N3 Ni1 N1 C7 51(13) . . . . ?
O1 Ni1 N1 C7 11.4(6) . . . . ?
N8 Ni1 N1 C7 96.0(6) . . . . ?
O2 Ni1 N1 C7 -75.5(6) . . . . ?
N2 Ni1 N1 C7 -165.3(6) . . . . ?
N3 Ni1 N1 C8A -144(13) . . . . ?
O1 Ni1 N1 C8A 175.9(17) . . . . ?
N8 Ni1 N1 C8A -99.6(17) . . . . ?
O2 Ni1 N1 C8A 88.9(17) . . . . ?
N2 Ni1 N1 C8A -0.9(17) . . . . ?
N3 Ni1 N1 C8 -124(12) . . . . ?
O1 Ni1 N1 C8 -163.7(7) . . . . ?
N8 Ni1 N1 C8 -79.2(7) . . . . ?
O2 Ni1 N1 C8 109.3(7) . . . . ?
N2 Ni1 N1 C8 19.5(7) . . . . ?
N1 Ni1 N2 C9A -17.6(18) . . . . ?
N3 Ni1 N2 C9A 161.8(18) . . . . ?
O1 Ni1 N2 C9A -44(2) . . . . ?
N8 Ni1 N2 C9A 71.1(18) . . . . ?
O2 Ni1 N2 C9A -107.2(18) . . . . ?
N1 Ni1 N2 C10 -118.6(6) . . . . ?
N3 Ni1 N2 C10 60.8(6) . . . . ?
O1 Ni1 N2 C10 -145.5(13) . . . . ?
N8 Ni1 N2 C10 -29.9(6) . . . . ?
O2 Ni1 N2 C10 151.7(6) . . . . ?
N1 Ni1 N2 C11 118.4(5) . . . . ?
N3 Ni1 N2 C11 -62.2(5) . . . . ?
O1 Ni1 N2 C11 91.5(15) . . . . ?
N8 Ni1 N2 C11 -152.9(5) . . . . ?
O2 Ni1 N2 C11 28.8(5) . . . . ?
N1 Ni1 N2 C9 13.2(6) . . . . ?
N3 Ni1 N2 C9 -167.4(6) . . . . ?
O1 Ni1 N2 C9 -13.7(17) . . . . ?
N8 Ni1 N2 C9 102.0(6) . . . . ?
O2 Ni1 N2 C9 -76.4(6) . . . . ?
N1 Ni1 N3 N4 -16(13) . . . . ?
O1 Ni1 N3 N4 24.0(4) . . . . ?
N8 Ni1 N3 N4 -60.6(4) . . . . ?
O2 Ni1 N3 N4 110.9(4) . . . . ?
N2 Ni1 N3 N4 -159.2(4) . . . . ?
N1 Ni1 N3 N6 159(12) . . . . ?
O1 Ni1 N3 N6 -160.7(5) . . . . ?
N8 Ni1 N3 N6 114.7(5) . . . . ?
O2 Ni1 N3 N6 -73.8(5) . . . . ?
N2 Ni1 N3 N6 16.1(5) . . . . ?
N6 N3 N4 N5 1.4(6) . . . . ?
Ni1 N3 N4 N5 177.6(3) . . . . ?
N6 N3 N4 Ni2 -171.8(3) . . . . ?
Ni1 N3 N4 Ni2 4.5(5) . . . . ?
N4 Ni2 N4 N3 87(100) 2_775 . . . ?
O1 Ni2 N4 N3 -29.7(4) . . . . ?
O1 Ni2 N4 N3 150.3(4) 2_775 . . . ?
N9 Ni2 N4 N3 52.7(4) . . . . ?
N9 Ni2 N4 N3 -127.3(4) 2_775 . . . ?
N4 Ni2 N4 N5 -85(100) 2_775 . . . ?
O1 Ni2 N4 N5 158.6(5) . . . . ?
O1 Ni2 N4 N5 -21.4(5) 2_775 . . . ?
N9 Ni2 N4 N5 -118.9(5) . . . . ?
N9 Ni2 N4 N5 61.1(5) 2_775 . . . ?
N3 N4 N5 C12 -0.5(6) . . . . ?
Ni2 N4 N5 C12 171.8(4) . . . . ?
N4 N3 N6 C12 -1.6(6) . . . . ?
Ni1 N3 N6 C12 -177.2(4) . . . . ?
N1 Ni1 N8 N10 45.8(5) . . . . ?
N3 Ni1 N8 N10 -134.9(5) . . . . ?
O1 Ni1 N8 N10 136.4(5) . . . . ?
O2 Ni1 N8 N10 131.9(10) . . . . ?
N2 Ni1 N8 N10 -37.0(5) . . . . ?
N1 Ni1 N8 N9 -118.8(4) . . . . ?
N3 Ni1 N8 N9 60.5(4) . . . . ?
O1 Ni1 N8 N9 -28.2(4) . . . . ?
O2 Ni1 N8 N9 -32.6(13) . . . . ?
N2 Ni1 N8 N9 158.4(4) . . . . ?
N10 N8 N9 N11 0.1(6) . . . . ?
Ni1 N8 N9 N11 167.9(3) . . . . ?
N10 N8 N9 Ni2 -172.3(3) . . . . ?
Ni1 N8 N9 Ni2 -4.6(5) . . . . ?
N4 Ni2 N9 N8 -51.5(4) . . . . ?
N4 Ni2 N9 N8 128.5(4) 2_775 . . . ?
O1 Ni2 N9 N8 34.0(4) . . . . ?
O1 Ni2 N9 N8 -146.0(4) 2_775 . . . ?
N9 Ni2 N9 N8 -171(100) 2_775 . . . ?
N4 Ni2 N9 N11 137.8(4) . . . . ?
N4 Ni2 N9 N11 -42.2(4) 2_775 . . . ?
O1 Ni2 N9 N11 -136.6(5) . . . . ?
O1 Ni2 N9 N11 43.4(5) 2_775 . . . ?
N9 Ni2 N9 N11 18(100) 2_775 . . . ?
N9 N8 N10 C18 0.2(6) . . . . ?
Ni1 N8 N10 C18 -165.3(4) . . . . ?
N8 N9 N11 C18 -0.4(6) . . . . ?
Ni2 N9 N11 C18 170.9(4) . . . . ?
N22 Ni4 N14 C33 -67(5) 2_656 . . . ?
O3 Ni4 N14 C33 11.8(6) . . . . ?
N17 Ni4 N14 C33 96.0(6) 2_656 . . . ?
N15 Ni4 N14 C33 -168.5(6) . . . . ?
O4 Ni4 N14 C33 -75.8(6) . . . . ?
N22 Ni4 N14 C34 122(5) 2_656 . . . ?
O3 Ni4 N14 C34 -159.6(11) . . . . ?
N17 Ni4 N14 C34 -75.4(11) 2_656 . . . ?
N15 Ni4 N14 C34 20.0(11) . . . . ?
O4 Ni4 N14 C34 112.8(11) . . . . ?
N22 Ni4 N14 C34A 96(5) 2_656 . . . ?
O3 Ni4 N14 C34A 174.3(8) . . . . ?
N17 Ni4 N14 C34A -101.4(8) 2_656 . . . ?
N15 Ni4 N14 C34A -6.0(8) . . . . ?
O4 Ni4 N14 C34A 86.8(8) . . . . ?
N14 Ni4 N15 C35 7.2(13) . . . . ?
N22 Ni4 N15 C35 -170.8(13) 2_656 . . . ?
O3 Ni4 N15 C35 10(2) . . . . ?
N17 Ni4 N15 C35 98.7(13) 2_656 . . . ?
O4 Ni4 N15 C35 -79.8(13) . . . . ?
N14 Ni4 N15 C37 -133.5(6) . . . . ?
N22 Ni4 N15 C37 48.5(5) 2_656 . . . ?
O3 Ni4 N15 C37 -130.7(15) . . . . ?
N17 Ni4 N15 C37 -42.0(5) 2_656 . . . ?
O4 Ni4 N15 C37 139.4(5) . . . . ?
N14 Ni4 N15 C36 108.1(5) . . . . ?
N22 Ni4 N15 C36 -69.9(5) 2_656 . . . ?
O3 Ni4 N15 C36 110.9(17) . . . . ?
N17 Ni4 N15 C36 -160.4(5) 2_656 . . . ?
O4 Ni4 N15 C36 21.0(5) . . . . ?
N14 Ni4 N15 C35A -25.7(6) . . . . ?
N22 Ni4 N15 C35A 156.3(6) 2_656 . . . ?
O3 Ni4 N15 C35A -23(2) . . . . ?
N17 Ni4 N15 C35A 65.8(6) 2_656 . . . ?
O4 Ni4 N15 C35A -112.8(6) . . . . ?
N21 Ni3 N16 N17 -127.3(4) 2_656 . . . ?
N21 Ni3 N16 N17 52.7(4) . . . . ?
N16 Ni3 N16 N17 156(100) 2_656 . . . ?
O3 Ni3 N16 N17 -32.5(4) 2_656 . . . ?
O3 Ni3 N16 N17 147.5(4) . . . . ?
N21 Ni3 N16 N18 43.8(4) 2_656 . . . ?
N21 Ni3 N16 N18 -136.2(4) . . . . ?
N16 Ni3 N16 N18 -33(100) 2_656 . . . ?
O3 Ni3 N16 N18 138.6(4) 2_656 . . . ?
O3 Ni3 N16 N18 -41.4(4) . . . . ?
N18 N16 N17 N19 0.2(6) . . . . ?
Ni3 N16 N17 N19 173.0(3) . . . . ?
N18 N16 N17 Ni4 -170.3(3) . . . 2_656 ?
Ni3 N16 N17 Ni4 2.5(5) . . . 2_656 ?
N17 N16 N18 C38 0.7(5) . . . . ?
Ni3 N16 N18 C38 -171.1(3) . . . . ?
N16 N17 N19 C38 -0.9(6) . . . . ?
Ni4 N17 N19 C38 167.7(4) 2_656 . . . ?
N21 Ni3 N21 N22 -172(100) 2_656 . . . ?
N16 Ni3 N21 N22 128.0(4) 2_656 . . . ?
N16 Ni3 N21 N22 -52.0(4) . . . . ?
O3 Ni3 N21 N22 30.7(4) 2_656 . . . ?
O3 Ni3 N21 N22 -149.3(4) . . . . ?
N21 Ni3 N21 N24 0(100) 2_656 . . . ?
N16 Ni3 N21 N24 -60.0(4) 2_656 . . . ?
N16 Ni3 N21 N24 120.0(4) . . . . ?
O3 Ni3 N21 N24 -157.2(4) 2_656 . . . ?
O3 Ni3 N21 N24 22.8(4) . . . . ?
N24 N21 N22 N23 -0.6(6) . . . . ?
Ni3 N21 N22 N23 172.9(3) . . . . ?
N24 N21 N22 Ni4 -179.0(3) . . . 2_656 ?
Ni3 N21 N22 Ni4 -5.5(5) . . . 2_656 ?
N21 N22 N23 C44 0.4(6) . . . . ?
Ni4 N22 N23 C44 178.5(4) 2_656 . . . ?
N22 N21 N24 C44 0.5(6) . . . . ?
Ni3 N21 N24 C44 -172.2(4) . . . . ?
Ni1 O1 C1 C2 -152.9(4) . . . . ?
Ni2 O1 C1 C2 47.3(7) . . . . ?
Ni1 O1 C1 C6 25.6(7) . . . . ?
Ni2 O1 C1 C6 -134.3(4) . . . . ?
O1 C1 C2 C3 -175.9(5) . . . . ?
C6 C1 C2 C3 5.5(8) . . . . ?
C1 C2 C3 C4 -1.3(9) . . . . ?
C2 C3 C4 C5 -2.2(9) . . . . ?
C2 C3 C4 Cl1 178.1(5) . . . . ?
C3 C4 C5 C6 1.2(10) . . . . ?
Cl1 C4 C5 C6 -179.2(5) . . . . ?
C4 C5 C6 C1 3.3(9) . . . . ?
C4 C5 C6 C7 -175.8(6) . . . . ?
O1 C1 C6 C5 175.1(5) . . . . ?
C2 C1 C6 C5 -6.4(8) . . . . ?
O1 C1 C6 C7 -5.8(9) . . . . ?
C2 C1 C6 C7 172.7(6) . . . . ?
C8A N1 C7 C6 -160.8(19) . . . . ?
C8 N1 C7 C6 177.4(9) . . . . ?
Ni1 N1 C7 C6 2.5(10) . . . . ?
C5 C6 C7 N1 169.0(6) . . . . ?
C1 C6 C7 N1 -10.2(11) . . . . ?
C7 N1 C8 C9 134.3(11) . . . . ?
C8A N1 C8 C9 38(4) . . . . ?
Ni1 N1 C8 C9 -50.1(14) . . . . ?
N1 C8 C9 N2 62.5(15) . . . . ?
C9A N2 C9 C8 59(3) . . . . ?
C10 N2 C9 C8 79.9(16) . . . . ?
C11 N2 C9 C8 -162.6(15) . . . . ?
Ni1 N2 C9 C8 -46.7(16) . . . . ?
C7 N1 C8A C9A -174(3) . . . . ?
C8 N1 C8A C9A -80(6) . . . . ?
Ni1 N1 C8A C9A 20(4) . . . . ?
C10 N2 C9A C8A 148(3) . . . . ?
C11 N2 C9A C8A -100(3) . . . . ?
C9 N2 C9A C8A -50(2) . . . . ?
Ni1 N2 C9A C8A 32(4) . . . . ?
N1 C8A C9A N2 -37(5) . . . . ?
N4 N5 C12 N6 -0.5(6) . . . . ?
N4 N5 C12 C13 -178.2(5) . . . . ?
N3 N6 C12 N5 1.3(6) . . . . ?
N3 N6 C12 C13 179.0(5) . . . . ?
N5 C12 C13 C14 16.6(10) . . . . ?
N6 C12 C13 C14 -160.9(7) . . . . ?
N5 C12 C13 C17 -165.4(6) . . . . ?
N6 C12 C13 C17 17.1(10) . . . . ?
C17 C13 C14 C15 0.7(13) . . . . ?
C12 C13 C14 C15 178.8(8) . . . . ?
C13 C14 C15 C16 -1.3(16) . . . . ?
C14 C15 C16 N7 0.9(19) . . . . ?
C17 N7 C16 C15 0.1(17) . . . . ?
C16 N7 C17 C13 -0.7(13) . . . . ?
C14 C13 C17 N7 0.3(11) . . . . ?
C12 C13 C17 N7 -177.8(7) . . . . ?
N8 N10 C18 N11 -0.5(6) . . . . ?
N8 N10 C18 C19 179.3(5) . . . . ?
N9 N11 C18 N10 0.6(6) . . . . ?
N9 N11 C18 C19 -179.2(5) . . . . ?
N10 C18 C19 C23 -167.9(6) . . . . ?
N11 C18 C19 C23 11.9(9) . . . . ?
N10 C18 C19 C20 13.6(9) . . . . ?
N11 C18 C19 C20 -166.6(6) . . . . ?
C23 C19 C20 C21 1.6(10) . . . . ?
C18 C19 C20 C21 -179.8(6) . . . . ?
C19 C20 C21 C22 -1.2(13) . . . . ?
C20 C21 C22 N12 0.0(15) . . . . ?
C23 N12 C22 C21 0.6(14) . . . . ?
C20 C19 C23 N12 -1.0(11) . . . . ?
C18 C19 C23 N12 -179.5(7) . . . . ?
C22 N12 C23 C19 0.0(12) . . . . ?
Ni1 O2 C24 N13 -169.5(5) . . . . ?
C25 N13 C24 O2 0.5(10) . . . . ?
C26 N13 C24 O2 179.6(7) . . . . ?
Ni4 O3 C27 C28 -156.0(4) . . . . ?
Ni3 O3 C27 C28 46.3(7) . . . . ?
Ni4 O3 C27 C32 20.9(7) . . . . ?
Ni3 O3 C27 C32 -136.8(4) . . . . ?
O3 C27 C28 C29 -176.4(5) . . . . ?
C32 C27 C28 C29 6.5(9) . . . . ?
C27 C28 C29 C30 -1.1(10) . . . . ?
C28 C29 C30 C31 -2.8(10) . . . . ?
C28 C29 C30 Cl2 176.5(5) . . . . ?
C29 C30 C31 C32 0.7(10) . . . . ?
Cl2 C30 C31 C32 -178.6(5) . . . . ?
C30 C31 C32 C27 5.0(9) . . . . ?
C30 C31 C32 C33 -173.5(6) . . . . ?
O3 C27 C32 C31 174.7(5) . . . . ?
C28 C27 C32 C31 -8.3(8) . . . . ?
O3 C27 C32 C33 -7.0(9) . . . . ?
C28 C27 C32 C33 170.0(6) . . . . ?
C34 N14 C33 C32 167.7(13) . . . . ?
C34A N14 C33 C32 -164.9(10) . . . . ?
Ni4 N14 C33 C32 -3.4(11) . . . . ?
C31 C32 C33 N14 175.6(7) . . . . ?
C27 C32 C33 N14 -2.7(11) . . . . ?
C33 N14 C34 C35 147.8(18) . . . . ?
C34A N14 C34 C35 49(3) . . . . ?
Ni4 N14 C34 C35 -40(2) . . . . ?
C37 N15 C35 C34 100(3) . . . . ?
C36 N15 C35 C34 -147(3) . . . . ?
C35A N15 C35 C34 60(3) . . . . ?
Ni4 N15 C35 C34 -34(3) . . . . ?
N14 C34 C35 N15 50(3) . . . . ?
C33 N14 C34A C35A -158.4(11) . . . . ?
C34 N14 C34A C35A -64(4) . . . . ?
Ni4 N14 C34A C35A 37.5(15) . . . . ?
N14 C34A C35A N15 -58.9(15) . . . . ?
C35 N15 C35A C34A -42.5(19) . . . . ?
C37 N15 C35A C34A 169.1(11) . . . . ?
C36 N15 C35A C34A -75.8(12) . . . . ?
Ni4 N15 C35A C34A 50.9(12) . . . . ?
N16 N18 C38 N19 -1.3(6) . . . . ?
N16 N18 C38 C39 178.8(5) . . . . ?
N17 N19 C38 N18 1.4(6) . . . . ?
N17 N19 C38 C39 -178.7(5) . . . . ?
N18 C38 C39 C40 -15.1(9) . . . . ?
N19 C38 C39 C40 165.1(6) . . . . ?
N18 C38 C39 C43 163.7(5) . . . . ?
N19 C38 C39 C43 -16.2(8) . . . . ?
C43 C39 C40 C41 0.3(10) . . . . ?
C38 C39 C40 C41 179.1(6) . . . . ?
C39 C40 C41 C42 0.6(11) . . . . ?
C43 N20 C42 C41 2.7(12) . . . . ?
C40 C41 C42 N20 -2.2(12) . . . . ?
C42 N20 C43 C39 -1.7(11) . . . . ?
C40 C39 C43 N20 0.3(10) . . . . ?
C38 C39 C43 N20 -178.5(6) . . . . ?
N21 N24 C44 N23 -0.2(6) . . . . ?
N21 N24 C44 C45 177.6(5) . . . . ?
N22 N23 C44 N24 -0.1(6) . . . . ?
N22 N23 C44 C45 -177.9(5) . . . . ?
N24 C44 C45 C49 162.7(6) . . . . ?
N23 C44 C45 C49 -19.8(9) . . . . ?
N24 C44 C45 C46 -19.0(9) . . . . ?
N23 C44 C45 C46 158.6(6) . . . . ?
C49 C45 C46 C47 1.3(11) . . . . ?
C44 C45 C46 C47 -177.2(7) . . . . ?
C45 C46 C47 C48 0.1(14) . . . . ?
C46 C47 C48 N25 -2.4(17) . . . . ?
C49 N25 C48 C47 3.1(15) . . . . ?
C48 N25 C49 C45 -1.7(12) . . . . ?
C46 C45 C49 N25 -0.5(11) . . . . ?
C44 C45 C49 N25 177.9(6) . . . . ?
Ni4 O4 C50 N26 -167.4(5) . . . . ?
C51 N26 C50 O4 177.3(7) . . . . ?
C52 N26 C50 O4 -2.9(10) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         2.022
_refine_diff_density_min         -0.899
_refine_diff_density_rms         0.107


# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.188 0.500 0.546 1001 117 ' '
_platon_squeeze_details          
;
;
_database_code_depnum_ccdc_archive 'CCDC 961050'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_4C

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C76 H72 Cl4 N28 Ni5 O8'
_chemical_formula_weight         1940.97

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           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   10.5420(10)
_cell_length_b                   22.598(3)
_cell_length_c                   21.861(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.357(9)
_cell_angle_gamma                90.00
_cell_volume                     5206.5(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5912
_cell_measurement_theta_min      2.9319
_cell_measurement_theta_max      26.3152

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1992
_exptl_absorpt_coefficient_mu    1.048
_exptl_absorpt_correction_T_min  0.7722
_exptl_absorpt_correction_T_max  0.8337
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      150(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  'OXFORD DIFFRACTION SUPER NOVA'
_diffrn_measurement_method       ω/q-scan
_diffrn_detector_area_resol_mean 15.9948
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            41030
_diffrn_reflns_av_R_equivalents  0.1139
_diffrn_reflns_av_unetI/netI     0.0869
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.94
_diffrn_reflns_theta_max         25.00
_reflns_number_total             9170
_reflns_number_gt                5348
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.,'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.,'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.,'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Ortep3
_computing_publication_material  Shelx97

_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)+(0.1204P)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    riding
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9170
_refine_ls_number_parameters     570
_refine_ls_number_restraints     38
_refine_ls_R_factor_all          0.1059
_refine_ls_R_factor_gt           0.0763
_refine_ls_wR_factor_ref         0.2367
_refine_ls_wR_factor_gt          0.2070
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_restrained_S_all      0.985
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.0000 0.5000 0.0000 0.0536(3) Uani 1 2 d S . .
Ni2 Ni 0.00718(6) 0.34154(3) 0.01089(3) 0.0554(2) Uani 1 1 d . . .
Ni3 Ni -0.13063(6) 0.42139(3) -0.12183(3) 0.0542(2) Uani 1 1 d . . .
Cl1 Cl -0.4449(4) 0.1247(2) 0.1194(2) 0.294(3) Uani 1 1 d . . .
Cl2 Cl 0.2498(3) 0.42471(13) -0.39871(12) 0.1393(10) Uani 1 1 d . . .
O1 O -0.1652(3) 0.33809(19) 0.0516(2) 0.0777(12) Uani 1 1 d . . .
O2 O 0.0487(3) 0.43155(16) -0.15063(19) 0.0641(10) Uani 1 1 d . . .
O3 O -0.0695(3) 0.42030(14) -0.03057(18) 0.0554(9) Uani 1 1 d . . .
O4 O -0.1595(3) 0.5172(2) 0.0551(2) 0.0839(13) Uani 1 1 d . . .
N1 N 0.0821(4) 0.45605(18) 0.07264(19) 0.0538(10) Uani 1 1 d . . .
N2 N 0.0773(4) 0.3979(2) 0.0849(2) 0.0540(10) Uani 1 1 d . . .
N3 N 0.1349(4) 0.4845(2) 0.1185(2) 0.0576(11) Uani 1 1 d . . .
N4 N 0.1685(4) 0.4457(2) 0.1632(2) 0.0624(11) Uani 1 1 d . . .
N5 N 0.4687(6) 0.3889(4) 0.1714(4) 0.119(2) Uani 1 1 d . . .
N6 N 0.2073(4) 0.3256(3) -0.0223(3) 0.0829(16) Uani 1 1 d . . .
N7 N 0.0488(4) 0.2620(2) 0.0498(3) 0.0709(13) Uani 1 1 d . . .
N8 N -0.0627(4) 0.3007(2) -0.0688(2) 0.0621(11) Uani 1 1 d . . .
N9 N -0.1071(4) 0.33063(19) -0.1171(2) 0.0564(11) Uani 1 1 d . . .
N10 N -0.1340(4) 0.2928(2) -0.1635(2) 0.0659(12) Uani 1 1 d . . .
N11 N -0.0581(4) 0.2424(2) -0.0822(2) 0.0680(13) Uani 1 1 d . . .
N12 N -0.3903(8) 0.2506(4) -0.2344(5) 0.170(4) Uani 1 1 d . . .
N13 N -0.3383(4) 0.4175(2) -0.1041(2) 0.0665(13) Uani 1 1 d U . .
N14 N -0.1928(4) 0.4194(2) -0.2103(2) 0.0653(13) Uani 1 1 d . . .
C1 C 0.1327(4) 0.3933(3) 0.1399(2) 0.0584(14) Uani 1 1 d . . .
C2 C 0.1555(5) 0.3383(3) 0.1741(3) 0.0647(14) Uani 1 1 d . . .
C3 C 0.2755(6) 0.3220(3) 0.1973(3) 0.087(2) Uani 1 1 d . . .
C4 C 0.3828(7) 0.3599(4) 0.1825(4) 0.104(3) Uani 1 1 d . . .
C5 C 0.2964(7) 0.2711(3) 0.2305(4) 0.097(2) Uani 1 1 d U . .
H5 H 0.3786 0.2619 0.2465 0.117 Uiso 1 1 calc R . .
C6 C 0.1964(9) 0.2341(4) 0.2400(4) 0.108(2) Uani 1 1 d U . .
H6 H 0.2103 0.1981 0.2617 0.129 Uiso 1 1 calc R . .
C7 C 0.0761(7) 0.2479(3) 0.2189(4) 0.090(2) Uani 1 1 d U . .
H7 H 0.0071 0.2223 0.2272 0.108 Uiso 1 1 calc R . .
C8 C 0.0558(5) 0.3001(3) 0.1851(3) 0.0699(15) Uani 1 1 d . . .
H8 H -0.0269 0.3093 0.1697 0.084 Uiso 1 1 calc R . .
C9 C -0.2250(5) 0.2896(4) 0.0667(3) 0.089(2) Uani 1 1 d . . .
C10 C -0.3576(7) 0.2928(5) 0.0770(4) 0.131(4) Uani 1 1 d . . .
H10 H -0.4023 0.3290 0.0721 0.157 Uiso 1 1 calc R . .
C11 C -0.4207(9) 0.2412(7) 0.0946(5) 0.154(5) Uani 1 1 d . . .
H11 H -0.5092 0.2432 0.1013 0.185 Uiso 1 1 calc R . .
C12 C -0.3610(11) 0.1887(7) 0.1023(6) 0.175(6) Uani 1 1 d . . .
C13 C -0.2348(9) 0.1840(4) 0.0900(4) 0.134(4) Uani 1 1 d . . .
H13 H -0.1945 0.1464 0.0925 0.161 Uiso 1 1 calc R . .
C14 C -0.1632(6) 0.2344(4) 0.0734(4) 0.096(2) Uani 1 1 d . . .
C15 C -0.0331(6) 0.2232(3) 0.0666(4) 0.092(2) Uani 1 1 d . . .
H15 H -0.0033 0.1843 0.0750 0.110 Uiso 1 1 calc R . .
C16 C 0.1800(7) 0.2421(4) 0.0489(4) 0.107(3) Uani 1 1 d . . .
H16A H 0.2297 0.2602 0.0830 0.129 Uiso 1 1 calc R . .
H16B H 0.1841 0.1985 0.0533 0.129 Uiso 1 1 calc R . .
C17 C 0.2290(7) 0.2594(5) -0.0075(5) 0.126(3) Uani 1 1 d . . .
H17A H 0.1888 0.2352 -0.0403 0.151 Uiso 1 1 calc R . .
H17B H 0.3212 0.2511 -0.0072 0.151 Uiso 1 1 calc R . .
C18 C 0.3052(6) 0.3586(5) 0.0105(4) 0.141(4) Uani 1 1 d . . .
H18A H 0.3888 0.3455 -0.0026 0.212 Uiso 1 1 calc R . .
H18B H 0.2978 0.3519 0.0545 0.212 Uiso 1 1 calc R . .
H18C H 0.2951 0.4009 0.0018 0.212 Uiso 1 1 calc R . .
C19 C 0.2251(6) 0.3295(4) -0.0891(3) 0.098(2) Uani 1 1 d . . .
H19A H 0.2184 0.3709 -0.1021 0.147 Uiso 1 1 calc R . .
H19B H 0.1596 0.3060 -0.1104 0.147 Uiso 1 1 calc R . .
H19C H 0.3091 0.3142 -0.0990 0.147 Uiso 1 1 calc R . .
C38 C -0.1038(5) 0.2406(3) -0.1397(3) 0.0635(14) Uani 1 1 d . . .
C20 C -0.1152(6) 0.1845(3) -0.1751(3) 0.0784(17) Uani 1 1 d . . .
C21 C -0.2123(6) 0.1769(3) -0.2192(3) 0.0834(19) Uani 1 1 d . . .
C22 C -0.3082(8) 0.2185(4) -0.2270(4) 0.111(3) Uani 1 1 d . . .
C23 C -0.2210(9) 0.1258(4) -0.2538(5) 0.127(3) Uani 1 1 d . . .
H23 H -0.2898 0.1195 -0.2819 0.152 Uiso 1 1 calc R . .
C24 C -0.1279(11) 0.0849(4) -0.2462(5) 0.124(3) Uani 1 1 d . . .
H24 H -0.1299 0.0506 -0.2713 0.149 Uiso 1 1 calc R . .
C25 C -0.0330(10) 0.0909(3) -0.2045(5) 0.123(3) Uani 1 1 d . . .
H25 H 0.0290 0.0606 -0.1998 0.148 Uiso 1 1 calc R . .
C26 C -0.0254(8) 0.1407(3) -0.1689(4) 0.100(2) Uani 1 1 d . . .
H26 H 0.0422 0.1449 -0.1397 0.120 Uiso 1 1 calc R . .
C27 C 0.0910(5) 0.4294(2) -0.2066(3) 0.0607(14) Uani 1 1 d . A .
C28 C 0.2219(5) 0.4347(3) -0.2160(3) 0.0703(16) Uani 1 1 d . . .
H28 H 0.2781 0.4404 -0.1819 0.084 Uiso 1 1 calc R . .
C29 C 0.2696(7) 0.4318(3) -0.2741(4) 0.088(2) Uani 1 1 d . . .
H29 H 0.3588 0.4337 -0.2791 0.105 Uiso 1 1 calc R . .
C30 C 0.1895(7) 0.4260(3) -0.3258(4) 0.0838(19) Uani 1 1 d . . .
C31 C 0.0617(7) 0.4218(3) -0.3172(3) 0.0824(19) Uani 1 1 d . A .
H31 H 0.0067 0.4182 -0.3520 0.099 Uiso 1 1 calc R . .
C32 C 0.0092(6) 0.4225(2) -0.2593(3) 0.0648(15) Uani 1 1 d . . .
C33 C -0.1266(6) 0.4188(3) -0.2582(3) 0.0666(15) Uani 1 1 d . A .
H33 H -0.1707 0.4155 -0.2964 0.080 Uiso 1 1 calc R . .
C34 C -0.3364(14) 0.4156(9) -0.2141(6) 0.065(4) Uani 0.60 1 d PU A 1
H34A H -0.3680 0.4359 -0.2516 0.077 Uiso 0.60 1 calc PR A 1
H34B H -0.3629 0.3736 -0.2165 0.077 Uiso 0.60 1 calc PR A 1
C35 C -0.3910(16) 0.4430(7) -0.1607(7) 0.064(3) Uani 0.60 1 d PU A 1
H35A H -0.4841 0.4374 -0.1621 0.077 Uiso 0.60 1 calc PR A 1
H35B H -0.3736 0.4861 -0.1613 0.077 Uiso 0.60 1 calc PR A 1
C34A C -0.309(3) 0.407(2) -0.2265(18) 0.154(15) Uani 0.40 1 d PDU A 2
H34C H -0.3165 0.3646 -0.2381 0.185 Uiso 0.40 1 calc PR A 2
H34D H -0.3362 0.4312 -0.2622 0.185 Uiso 0.40 1 calc PR A 2
C35A C -0.390(3) 0.4195(18) -0.1743(15) 0.150(14) Uani 0.40 1 d PDU A 2
H35C H -0.4627 0.3916 -0.1772 0.179 Uiso 0.40 1 calc PR A 2
H35D H -0.4261 0.4596 -0.1810 0.179 Uiso 0.40 1 calc PR A 2
C36 C -0.3830(6) 0.4606(4) -0.0600(4) 0.115(3) Uani 1 1 d . A .
H36A H -0.4751 0.4651 -0.0649 0.172 Uiso 1 1 calc R . .
H36B H -0.3417 0.4988 -0.0671 0.172 Uiso 1 1 calc R . .
H36C H -0.3622 0.4469 -0.0184 0.172 Uiso 1 1 calc R . .
C37 C -0.3782(6) 0.3585(3) -0.0886(4) 0.104(3) Uani 1 1 d . A .
H37A H -0.4701 0.3582 -0.0827 0.156 Uiso 1 1 calc R . .
H37B H -0.3345 0.3459 -0.0508 0.156 Uiso 1 1 calc R . .
H37C H -0.3574 0.3314 -0.1219 0.156 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 2.048(4) 3_565 ?
Ni1 N1 2.048(4) . ?
Ni1 O3 2.051(3) 3_565 ?
Ni1 O3 2.051(3) . ?
Ni1 O4 2.127(4) . ?
Ni1 O4 2.127(4) 3_565 ?
Ni2 N7 2.031(5) . ?
Ni2 O1 2.044(4) . ?
Ni2 N8 2.091(5) . ?
Ni2 O3 2.147(3) . ?
Ni2 N2 2.175(4) . ?
Ni2 N6 2.276(5) . ?
Ni3 O2 2.020(4) . ?
Ni3 N14 2.027(5) . ?
Ni3 N9 2.068(4) . ?
Ni3 O3 2.082(4) . ?
Ni3 N3 2.128(5) 3_565 ?
Ni3 N13 2.234(4) . ?
Cl1 C12 1.741(11) . ?
Cl2 C30 1.731(8) . ?
O1 C9 1.311(8) . ?
O2 C27 1.312(7) . ?
N1 N3 1.304(6) . ?
N1 N2 1.342(6) . ?
N2 C1 1.329(6) . ?
N3 N4 1.354(6) . ?
N3 Ni3 2.128(5) 3_565 ?
N4 C1 1.340(7) . ?
N5 C4 1.148(9) . ?
N6 C18 1.449(9) . ?
N6 C19 1.479(8) . ?
N6 C17 1.547(11) . ?
N7 C15 1.290(8) . ?
N7 C16 1.456(8) . ?
N8 N9 1.330(6) . ?
N8 N11 1.350(6) . ?
N9 N10 1.351(6) . ?
N10 C38 1.325(7) . ?
N11 C38 1.337(7) . ?
N12 C22 1.139(10) . ?
N13 C37 1.440(8) . ?
N13 C36 1.457(9) . ?
N13 C35 1.463(16) . ?
N13 C35A 1.62(3) . ?
N14 C33 1.273(8) . ?
N14 C34A 1.30(4) . ?
N14 C34 1.517(15) . ?
C1 C2 1.467(8) . ?
C2 C8 1.386(8) . ?
C2 C3 1.402(8) . ?
C3 C5 1.375(9) . ?
C3 C4 1.461(10) . ?
C5 C6 1.365(11) . ?
C5 H5 0.9500 . ?
C6 C7 1.375(10) . ?
C6 H6 0.9500 . ?
C7 C8 1.406(9) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C14 1.413(10) . ?
C9 C10 1.424(9) . ?
C10 C11 1.399(13) . ?
C10 H10 0.9500 . ?
C11 C12 1.353(17) . ?
C11 H11 0.9500 . ?
C12 C13 1.368(15) . ?
C13 C14 1.418(10) . ?
C13 H13 0.9500 . ?
C14 C15 1.406(10) . ?
C15 H15 0.9500 . ?
C16 C17 1.403(12) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C38 C20 1.488(8) . ?
C20 C26 1.375(9) . ?
C20 C21 1.400(9) . ?
C21 C23 1.382(10) . ?
C21 C22 1.387(11) . ?
C23 C24 1.355(12) . ?
C23 H23 0.9500 . ?
C24 C25 1.344(13) . ?
C24 H24 0.9500 . ?
C25 C26 1.368(10) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28 1.405(8) . ?
C27 C32 1.431(8) . ?
C28 C29 1.379(10) . ?
C28 H28 0.9500 . ?
C29 C30 1.401(10) . ?
C29 H29 0.9500 . ?
C30 C31 1.368(10) . ?
C31 C32 1.395(9) . ?
C31 H31 0.9500 . ?
C32 C33 1.435(9) . ?
C33 H33 0.9500 . ?
C34 C35 1.452(17) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C34A C35A 1.471(18) . ?
C34A H34C 0.9900 . ?
C34A H34D 0.9900 . ?
C35A H35C 0.9900 . ?
C35A H35D 0.9900 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N1 180.0(3) 3_565 . ?
N1 Ni1 O3 88.17(15) 3_565 3_565 ?
N1 Ni1 O3 91.83(15) . 3_565 ?
N1 Ni1 O3 91.83(15) 3_565 . ?
N1 Ni1 O3 88.17(15) . . ?
O3 Ni1 O3 180.0(2) 3_565 . ?
N1 Ni1 O4 91.43(17) 3_565 . ?
N1 Ni1 O4 88.57(17) . . ?
O3 Ni1 O4 86.35(16) 3_565 . ?
O3 Ni1 O4 93.65(16) . . ?
N1 Ni1 O4 88.57(17) 3_565 3_565 ?
N1 Ni1 O4 91.43(17) . 3_565 ?
O3 Ni1 O4 93.65(16) 3_565 3_565 ?
O3 Ni1 O4 86.35(16) . 3_565 ?
O4 Ni1 O4 180.0(3) . 3_565 ?
N7 Ni2 O1 88.24(19) . . ?
N7 Ni2 N8 91.54(19) . . ?
O1 Ni2 N8 92.65(18) . . ?
N7 Ni2 O3 170.25(16) . . ?
O1 Ni2 O3 83.42(15) . . ?
N8 Ni2 O3 83.82(16) . . ?
N7 Ni2 N2 98.06(18) . . ?
O1 Ni2 N2 89.36(17) . . ?
N8 Ni2 N2 170.25(18) . . ?
O3 Ni2 N2 86.93(15) . . ?
N7 Ni2 N6 78.5(2) . . ?
O1 Ni2 N6 166.7(2) . . ?
N8 Ni2 N6 88.61(19) . . ?
O3 Ni2 N6 109.84(19) . . ?
N2 Ni2 N6 91.62(18) . . ?
O2 Ni3 N14 89.39(19) . . ?
O2 Ni3 N9 90.93(16) . . ?
N14 Ni3 N9 93.48(18) . . ?
O2 Ni3 O3 91.68(15) . . ?
N14 Ni3 O3 177.85(16) . . ?
N9 Ni3 O3 84.64(16) . . ?
O2 Ni3 N3 85.30(16) . 3_565 ?
N14 Ni3 N3 92.79(17) . 3_565 ?
N9 Ni3 N3 172.65(17) . 3_565 ?
O3 Ni3 N3 89.16(15) . 3_565 ?
O2 Ni3 N13 170.72(17) . . ?
N14 Ni3 N13 82.44(19) . . ?
N9 Ni3 N13 93.95(17) . . ?
O3 Ni3 N13 96.63(16) . . ?
N3 Ni3 N13 90.67(17) 3_565 . ?
C9 O1 Ni2 125.4(4) . . ?
C27 O2 Ni3 128.8(3) . . ?
Ni1 O3 Ni3 113.70(15) . . ?
Ni1 O3 Ni2 117.55(16) . . ?
Ni3 O3 Ni2 121.29(16) . . ?
N3 N1 N2 110.3(4) . . ?
N3 N1 Ni1 121.4(3) . . ?
N2 N1 Ni1 127.7(3) . . ?
C1 N2 N1 103.8(4) . . ?
C1 N2 Ni2 139.7(4) . . ?
N1 N2 Ni2 116.0(3) . . ?
N1 N3 N4 109.5(4) . . ?
N1 N3 Ni3 120.7(3) . 3_565 ?
N4 N3 Ni3 128.9(4) . 3_565 ?
C1 N4 N3 103.4(4) . . ?
C18 N6 C19 110.6(6) . . ?
C18 N6 C17 107.2(6) . . ?
C19 N6 C17 104.1(6) . . ?
C18 N6 Ni2 114.5(5) . . ?
C19 N6 Ni2 116.4(4) . . ?
C17 N6 Ni2 102.7(4) . . ?
C15 N7 C16 115.8(6) . . ?
C15 N7 Ni2 125.6(4) . . ?
C16 N7 Ni2 117.7(5) . . ?
N9 N8 N11 109.8(4) . . ?
N9 N8 Ni2 123.2(4) . . ?
N11 N8 Ni2 126.7(3) . . ?
N8 N9 N10 109.8(4) . . ?
N8 N9 Ni3 125.7(3) . . ?
N10 N9 Ni3 124.6(4) . . ?
C38 N10 N9 103.0(5) . . ?
C38 N11 N8 102.7(4) . . ?
C37 N13 C36 111.2(6) . . ?
C37 N13 C35 117.2(7) . . ?
C36 N13 C35 100.0(8) . . ?
C37 N13 C35A 98.8(15) . . ?
C36 N13 C35A 120.0(13) . . ?
C35 N13 C35A 22.1(15) . . ?
C37 N13 Ni3 111.8(4) . . ?
C36 N13 Ni3 115.0(4) . . ?
C35 N13 Ni3 101.0(7) . . ?
C35A N13 Ni3 98.5(12) . . ?
C33 N14 C34A 107.8(16) . . ?
C33 N14 C34 121.3(7) . . ?
C34A N14 C34 16(2) . . ?
C33 N14 Ni3 127.9(4) . . ?
C34A N14 Ni3 123.2(17) . . ?
C34 N14 Ni3 110.7(6) . . ?
N2 C1 N4 112.9(5) . . ?
N2 C1 C2 126.2(5) . . ?
N4 C1 C2 120.9(5) . . ?
C8 C2 C3 117.0(6) . . ?
C8 C2 C1 120.1(5) . . ?
C3 C2 C1 122.9(5) . . ?
C5 C3 C2 122.9(6) . . ?
C5 C3 C4 119.5(6) . . ?
C2 C3 C4 117.6(6) . . ?
N5 C4 C3 178.7(8) . . ?
C6 C5 C3 118.6(7) . . ?
C6 C5 H5 120.7 . . ?
C3 C5 H5 120.7 . . ?
C5 C6 C7 121.3(7) . . ?
C5 C6 H6 119.4 . . ?
C7 C6 H6 119.4 . . ?
C6 C7 C8 119.6(7) . . ?
C6 C7 H7 120.2 . . ?
C8 C7 H7 120.2 . . ?
C2 C8 C7 120.5(6) . . ?
C2 C8 H8 119.7 . . ?
C7 C8 H8 119.7 . . ?
O1 C9 C14 122.8(5) . . ?
O1 C9 C10 118.5(8) . . ?
C14 C9 C10 118.7(7) . . ?
C11 C10 C9 118.4(10) . . ?
C11 C10 H10 120.8 . . ?
C9 C10 H10 120.8 . . ?
C12 C11 C10 122.9(9) . . ?
C12 C11 H11 118.6 . . ?
C10 C11 H11 118.6 . . ?
C11 C12 C13 119.7(9) . . ?
C11 C12 Cl1 121.3(10) . . ?
C13 C12 Cl1 118.7(12) . . ?
C12 C13 C14 121.0(10) . . ?
C12 C13 H13 119.5 . . ?
C14 C13 H13 119.5 . . ?
C15 C14 C9 126.5(6) . . ?
C15 C14 C13 114.2(8) . . ?
C9 C14 C13 119.3(7) . . ?
N7 C15 C14 124.7(6) . . ?
N7 C15 H15 117.6 . . ?
C14 C15 H15 117.6 . . ?
C17 C16 N7 107.2(6) . . ?
C17 C16 H16A 110.3 . . ?
N7 C16 H16A 110.3 . . ?
C17 C16 H16B 110.3 . . ?
N7 C16 H16B 110.3 . . ?
H16A C16 H16B 108.5 . . ?
C16 C17 N6 113.5(7) . . ?
C16 C17 H17A 108.9 . . ?
N6 C17 H17A 108.9 . . ?
C16 C17 H17B 108.9 . . ?
N6 C17 H17B 108.9 . . ?
H17A C17 H17B 107.7 . . ?
N6 C18 H18A 109.5 . . ?
N6 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N6 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N6 C19 H19A 109.5 . . ?
N6 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N6 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N10 C38 N11 114.8(5) . . ?
N10 C38 C20 122.6(5) . . ?
N11 C38 C20 122.6(5) . . ?
C26 C20 C21 118.1(6) . . ?
C26 C20 C38 121.0(6) . . ?
C21 C20 C38 120.7(6) . . ?
C23 C21 C22 117.5(7) . . ?
C23 C21 C20 121.1(7) . . ?
C22 C21 C20 121.3(6) . . ?
N12 C22 C21 176.9(9) . . ?
C24 C23 C21 117.7(8) . . ?
C24 C23 H23 121.1 . . ?
C21 C23 H23 121.1 . . ?
C25 C24 C23 122.6(8) . . ?
C25 C24 H24 118.7 . . ?
C23 C24 H24 118.7 . . ?
C24 C25 C26 120.1(8) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
C25 C26 C20 120.3(8) . . ?
C25 C26 H26 119.9 . . ?
C20 C26 H26 119.9 . . ?
O2 C27 C28 119.3(5) . . ?
O2 C27 C32 122.9(5) . . ?
C28 C27 C32 117.8(6) . . ?
C29 C28 C27 120.8(6) . . ?
C29 C28 H28 119.6 . . ?
C27 C28 H28 119.6 . . ?
C28 C29 C30 121.4(6) . . ?
C28 C29 H29 119.3 . . ?
C30 C29 H29 119.3 . . ?
C31 C30 C29 118.2(7) . . ?
C31 C30 Cl2 120.6(6) . . ?
C29 C30 Cl2 121.2(6) . . ?
C30 C31 C32 122.5(7) . . ?
C30 C31 H31 118.8 . . ?
C32 C31 H31 118.8 . . ?
C31 C32 C27 119.2(6) . . ?
C31 C32 C33 115.6(6) . . ?
C27 C32 C33 125.1(6) . . ?
N14 C33 C32 125.5(6) . . ?
N14 C33 H33 117.3 . . ?
C32 C33 H33 117.3 . . ?
C35 C34 N14 110.2(12) . . ?
C35 C34 H34A 109.6 . . ?
N14 C34 H34A 109.6 . . ?
C35 C34 H34B 109.6 . . ?
N14 C34 H34B 109.6 . . ?
H34A C34 H34B 108.1 . . ?
C34 C35 N13 111.2(12) . . ?
C34 C35 H35A 109.4 . . ?
N13 C35 H35A 109.4 . . ?
C34 C35 H35B 109.4 . . ?
N13 C35 H35B 109.4 . . ?
H35A C35 H35B 108.0 . . ?
N14 C34A C35A 108(3) . . ?
N14 C34A H34C 110.1 . . ?
C35A C34A H34C 110.1 . . ?
N14 C34A H34D 110.1 . . ?
C35A C34A H34D 110.1 . . ?
H34C C34A H34D 108.4 . . ?
C34A C35A N13 123(3) . . ?
C34A C35A H35C 106.7 . . ?
N13 C35A H35C 106.7 . . ?
C34A C35A H35D 106.7 . . ?
N13 C35A H35D 106.7 . . ?
H35C C35A H35D 106.6 . . ?
N13 C36 H36A 109.5 . . ?
N13 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
N13 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N13 C37 H37A 109.5 . . ?
N13 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
N13 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N7 Ni2 O1 C9 -26.8(5) . . . . ?
N8 Ni2 O1 C9 64.7(5) . . . . ?
O3 Ni2 O1 C9 148.2(5) . . . . ?
N2 Ni2 O1 C9 -124.8(5) . . . . ?
N6 Ni2 O1 C9 -30.5(11) . . . . ?
N14 Ni3 O2 C27 -6.7(4) . . . . ?
N9 Ni3 O2 C27 86.8(4) . . . . ?
O3 Ni3 O2 C27 171.5(4) . . . . ?
N3 Ni3 O2 C27 -99.5(4) 3_565 . . . ?
N13 Ni3 O2 C27 -35.0(13) . . . . ?
N1 Ni1 O3 Ni3 16.5(2) 3_565 . . . ?
N1 Ni1 O3 Ni3 -163.5(2) . . . . ?
O3 Ni1 O3 Ni3 122(100) 3_565 . . . ?
O4 Ni1 O3 Ni3 108.1(2) . . . . ?
O4 Ni1 O3 Ni3 -71.9(2) 3_565 . . . ?
N1 Ni1 O3 Ni2 166.9(2) 3_565 . . . ?
N1 Ni1 O3 Ni2 -13.1(2) . . . . ?
O3 Ni1 O3 Ni2 -88(100) 3_565 . . . ?
O4 Ni1 O3 Ni2 -101.6(2) . . . . ?
O4 Ni1 O3 Ni2 78.4(2) 3_565 . . . ?
O2 Ni3 O3 Ni1 68.20(19) . . . . ?
N14 Ni3 O3 Ni1 -172(5) . . . . ?
N9 Ni3 O3 Ni1 159.0(2) . . . . ?
N3 Ni3 O3 Ni1 -17.1(2) 3_565 . . . ?
N13 Ni3 O3 Ni1 -107.7(2) . . . . ?
O2 Ni3 O3 Ni2 -80.9(2) . . . . ?
N14 Ni3 O3 Ni2 39(5) . . . . ?
N9 Ni3 O3 Ni2 9.9(2) . . . . ?
N3 Ni3 O3 Ni2 -166.2(2) 3_565 . . . ?
N13 Ni3 O3 Ni2 103.3(2) . . . . ?
N7 Ni2 O3 Ni1 138.5(10) . . . . ?
O1 Ni2 O3 Ni1 107.1(2) . . . . ?
N8 Ni2 O3 Ni1 -159.5(2) . . . . ?
N2 Ni2 O3 Ni1 17.4(2) . . . . ?
N6 Ni2 O3 Ni1 -73.2(2) . . . . ?
N7 Ni2 O3 Ni3 -73.5(12) . . . . ?
O1 Ni2 O3 Ni3 -104.9(2) . . . . ?
N8 Ni2 O3 Ni3 -11.5(2) . . . . ?
N2 Ni2 O3 Ni3 165.4(2) . . . . ?
N6 Ni2 O3 Ni3 74.7(2) . . . . ?
N1 Ni1 N1 N3 -142(100) 3_565 . . . ?
O3 Ni1 N1 N3 8.7(4) 3_565 . . . ?
O3 Ni1 N1 N3 -171.3(4) . . . . ?
O4 Ni1 N1 N3 -77.6(4) . . . . ?
O4 Ni1 N1 N3 102.4(4) 3_565 . . . ?
N1 Ni1 N1 N2 29(100) 3_565 . . . ?
O3 Ni1 N1 N2 179.7(4) 3_565 . . . ?
O3 Ni1 N1 N2 -0.3(4) . . . . ?
O4 Ni1 N1 N2 93.4(4) . . . . ?
O4 Ni1 N1 N2 -86.6(4) 3_565 . . . ?
N3 N1 N2 C1 -1.3(5) . . . . ?
Ni1 N1 N2 C1 -173.2(3) . . . . ?
N3 N1 N2 Ni2 -174.9(3) . . . . ?
Ni1 N1 N2 Ni2 13.2(5) . . . . ?
N7 Ni2 N2 C1 0.8(5) . . . . ?
O1 Ni2 N2 C1 88.9(5) . . . . ?
N8 Ni2 N2 C1 -169.1(9) . . . . ?
O3 Ni2 N2 C1 172.4(5) . . . . ?
N6 Ni2 N2 C1 -77.8(5) . . . . ?
N7 Ni2 N2 N1 171.1(3) . . . . ?
O1 Ni2 N2 N1 -100.7(3) . . . . ?
N8 Ni2 N2 N1 1.3(12) . . . . ?
O3 Ni2 N2 N1 -17.3(3) . . . . ?
N6 Ni2 N2 N1 92.5(3) . . . . ?
N2 N1 N3 N4 0.5(5) . . . . ?
Ni1 N1 N3 N4 173.0(3) . . . . ?
N2 N1 N3 Ni3 -169.6(3) . . . 3_565 ?
Ni1 N1 N3 Ni3 2.9(5) . . . 3_565 ?
N1 N3 N4 C1 0.5(5) . . . . ?
Ni3 N3 N4 C1 169.6(3) 3_565 . . . ?
N7 Ni2 N6 C18 -102.1(6) . . . . ?
O1 Ni2 N6 C18 -98.3(10) . . . . ?
N8 Ni2 N6 C18 166.0(6) . . . . ?
O3 Ni2 N6 C18 83.1(6) . . . . ?
N2 Ni2 N6 C18 -4.2(6) . . . . ?
N7 Ni2 N6 C19 126.6(5) . . . . ?
O1 Ni2 N6 C19 130.4(8) . . . . ?
N8 Ni2 N6 C19 34.8(5) . . . . ?
O3 Ni2 N6 C19 -48.1(5) . . . . ?
N2 Ni2 N6 C19 -135.5(5) . . . . ?
N7 Ni2 N6 C17 13.7(5) . . . . ?
O1 Ni2 N6 C17 17.5(11) . . . . ?
N8 Ni2 N6 C17 -78.2(5) . . . . ?
O3 Ni2 N6 C17 -161.1(5) . . . . ?
N2 Ni2 N6 C17 111.6(5) . . . . ?
O1 Ni2 N7 C15 24.5(6) . . . . ?
N8 Ni2 N7 C15 -68.1(6) . . . . ?
O3 Ni2 N7 C15 -6.7(15) . . . . ?
N2 Ni2 N7 C15 113.6(6) . . . . ?
N6 Ni2 N7 C15 -156.3(6) . . . . ?
O1 Ni2 N7 C16 -167.3(5) . . . . ?
N8 Ni2 N7 C16 100.1(5) . . . . ?
O3 Ni2 N7 C16 161.5(10) . . . . ?
N2 Ni2 N7 C16 -78.2(5) . . . . ?
N6 Ni2 N7 C16 11.8(5) . . . . ?
N7 Ni2 N8 N9 -179.0(4) . . . . ?
O1 Ni2 N8 N9 92.7(4) . . . . ?
O3 Ni2 N8 N9 9.7(4) . . . . ?
N2 Ni2 N8 N9 -9.0(13) . . . . ?
N6 Ni2 N8 N9 -100.5(4) . . . . ?
N7 Ni2 N8 N11 -6.4(5) . . . . ?
O1 Ni2 N8 N11 -94.8(4) . . . . ?
O3 Ni2 N8 N11 -177.8(4) . . . . ?
N2 Ni2 N8 N11 163.5(8) . . . . ?
N6 Ni2 N8 N11 72.0(5) . . . . ?
N11 N8 N9 N10 0.5(6) . . . . ?
Ni2 N8 N9 N10 174.2(3) . . . . ?
N11 N8 N9 Ni3 -179.0(3) . . . . ?
Ni2 N8 N9 Ni3 -5.3(6) . . . . ?
O2 Ni3 N9 N8 88.7(4) . . . . ?
N14 Ni3 N9 N8 178.1(4) . . . . ?
O3 Ni3 N9 N8 -2.9(4) . . . . ?
N3 Ni3 N9 N8 29.6(17) 3_565 . . . ?
N13 Ni3 N9 N8 -99.2(4) . . . . ?
O2 Ni3 N9 N10 -90.7(4) . . . . ?
N14 Ni3 N9 N10 -1.3(4) . . . . ?
O3 Ni3 N9 N10 177.7(4) . . . . ?
N3 Ni3 N9 N10 -149.8(13) 3_565 . . . ?
N13 Ni3 N9 N10 81.4(4) . . . . ?
N8 N9 N10 C38 0.2(5) . . . . ?
Ni3 N9 N10 C38 179.7(3) . . . . ?
N9 N8 N11 C38 -1.0(6) . . . . ?
Ni2 N8 N11 C38 -174.4(4) . . . . ?
O2 Ni3 N13 C37 128.7(10) . . . . ?
N14 Ni3 N13 C37 100.1(5) . . . . ?
N9 Ni3 N13 C37 7.1(5) . . . . ?
O3 Ni3 N13 C37 -77.9(5) . . . . ?
N3 Ni3 N13 C37 -167.1(5) 3_565 . . . ?
O2 Ni3 N13 C36 -103.3(11) . . . . ?
N14 Ni3 N13 C36 -131.8(6) . . . . ?
N9 Ni3 N13 C36 135.2(6) . . . . ?
O3 Ni3 N13 C36 50.1(6) . . . . ?
N3 Ni3 N13 C36 -39.1(6) 3_565 . . . ?
O2 Ni3 N13 C35 3.3(14) . . . . ?
N14 Ni3 N13 C35 -25.2(6) . . . . ?
N9 Ni3 N13 C35 -118.2(6) . . . . ?
O3 Ni3 N13 C35 156.7(6) . . . . ?
N3 Ni3 N13 C35 67.5(6) 3_565 . . . ?
O2 Ni3 N13 C35A 25.6(19) . . . . ?
N14 Ni3 N13 C35A -3.0(14) . . . . ?
N9 Ni3 N13 C35A -96.0(14) . . . . ?
O3 Ni3 N13 C35A 179.0(14) . . . . ?
N3 Ni3 N13 C35A 89.8(14) 3_565 . . . ?
O2 Ni3 N14 C33 6.3(5) . . . . ?
N9 Ni3 N14 C33 -84.5(5) . . . . ?
O3 Ni3 N14 C33 -113(5) . . . . ?
N3 Ni3 N14 C33 91.6(5) 3_565 . . . ?
N13 Ni3 N14 C33 -178.1(5) . . . . ?
O2 Ni3 N14 C34A 172(3) . . . . ?
N9 Ni3 N14 C34A 81(3) . . . . ?
O3 Ni3 N14 C34A 53(6) . . . . ?
N3 Ni3 N14 C34A -102(3) 3_565 . . . ?
N13 Ni3 N14 C34A -12(3) . . . . ?
O2 Ni3 N14 C34 -176.4(9) . . . . ?
N9 Ni3 N14 C34 92.7(9) . . . . ?
O3 Ni3 N14 C34 64(5) . . . . ?
N3 Ni3 N14 C34 -91.1(9) 3_565 . . . ?
N13 Ni3 N14 C34 -0.8(8) . . . . ?
N1 N2 C1 N4 1.7(5) . . . . ?
Ni2 N2 C1 N4 172.8(4) . . . . ?
N1 N2 C1 C2 -178.2(5) . . . . ?
Ni2 N2 C1 C2 -7.1(9) . . . . ?
N3 N4 C1 N2 -1.4(6) . . . . ?
N3 N4 C1 C2 178.5(5) . . . . ?
N2 C1 C2 C8 -54.2(8) . . . . ?
N4 C1 C2 C8 125.9(6) . . . . ?
N2 C1 C2 C3 126.4(7) . . . . ?
N4 C1 C2 C3 -53.5(9) . . . . ?
C8 C2 C3 C5 -0.9(11) . . . . ?
C1 C2 C3 C5 178.5(7) . . . . ?
C8 C2 C3 C4 176.0(7) . . . . ?
C1 C2 C3 C4 -4.6(11) . . . . ?
C5 C3 C4 N5 8(51) . . . . ?
C2 C3 C4 N5 -169(100) . . . . ?
C2 C3 C5 C6 1.6(13) . . . . ?
C4 C3 C5 C6 -175.3(8) . . . . ?
C3 C5 C6 C7 -2.2(13) . . . . ?
C5 C6 C7 C8 2.2(13) . . . . ?
C3 C2 C8 C7 0.8(10) . . . . ?
C1 C2 C8 C7 -178.6(6) . . . . ?
C6 C7 C8 C2 -1.4(11) . . . . ?
Ni2 O1 C9 C14 19.2(10) . . . . ?
Ni2 O1 C9 C10 -161.1(5) . . . . ?
O1 C9 C10 C11 -178.5(8) . . . . ?
C14 C9 C10 C11 1.3(12) . . . . ?
C9 C10 C11 C12 0.2(17) . . . . ?
C10 C11 C12 C13 -3(2) . . . . ?
C10 C11 C12 Cl1 -175.9(8) . . . . ?
C11 C12 C13 C14 4.6(17) . . . . ?
Cl1 C12 C13 C14 177.5(8) . . . . ?
O1 C9 C14 C15 1.5(12) . . . . ?
C10 C9 C14 C15 -178.3(8) . . . . ?
O1 C9 C14 C13 179.9(7) . . . . ?
C10 C9 C14 C13 0.2(11) . . . . ?
C12 C13 C14 C15 175.5(9) . . . . ?
C12 C13 C14 C9 -3.1(13) . . . . ?
C16 N7 C15 C14 176.8(8) . . . . ?
Ni2 N7 C15 C14 -14.9(11) . . . . ?
C9 C14 C15 N7 -3.9(13) . . . . ?
C13 C14 C15 N7 177.6(8) . . . . ?
C15 N7 C16 C17 131.9(8) . . . . ?
Ni2 N7 C16 C17 -37.5(9) . . . . ?
N7 C16 C17 N6 51.1(10) . . . . ?
C18 N6 C17 C16 81.1(8) . . . . ?
C19 N6 C17 C16 -161.7(7) . . . . ?
Ni2 N6 C17 C16 -39.9(8) . . . . ?
N9 N10 C38 N11 -0.9(6) . . . . ?
N9 N10 C38 C20 -178.7(5) . . . . ?
N8 N11 C38 N10 1.2(6) . . . . ?
N8 N11 C38 C20 179.0(5) . . . . ?
N10 C38 C20 C26 141.0(7) . . . . ?
N11 C38 C20 C26 -36.5(10) . . . . ?
N10 C38 C20 C21 -33.9(9) . . . . ?
N11 C38 C20 C21 148.5(6) . . . . ?
C26 C20 C21 C23 2.7(12) . . . . ?
C38 C20 C21 C23 177.8(7) . . . . ?
C26 C20 C21 C22 178.2(8) . . . . ?
C38 C20 C21 C22 -6.7(11) . . . . ?
C23 C21 C22 N12 20(25) . . . . ?
C20 C21 C22 N12 -155(24) . . . . ?
C22 C21 C23 C24 -179.7(10) . . . . ?
C20 C21 C23 C24 -4.0(14) . . . . ?
C21 C23 C24 C25 3.7(17) . . . . ?
C23 C24 C25 C26 -2.0(18) . . . . ?
C24 C25 C26 C20 0.5(15) . . . . ?
C21 C20 C26 C25 -0.9(12) . . . . ?
C38 C20 C26 C25 -176.0(8) . . . . ?
Ni3 O2 C27 C28 -176.7(4) . . . . ?
Ni3 O2 C27 C32 4.0(7) . . . . ?
O2 C27 C28 C29 179.1(5) . . . . ?
C32 C27 C28 C29 -1.6(8) . . . . ?
C27 C28 C29 C30 2.7(10) . . . . ?
C28 C29 C30 C31 -1.6(10) . . . . ?
C28 C29 C30 Cl2 177.9(5) . . . . ?
C29 C30 C31 C32 -0.6(10) . . . . ?
Cl2 C30 C31 C32 179.9(5) . . . . ?
C30 C31 C32 C27 1.7(9) . . . . ?
C30 C31 C32 C33 178.9(5) . . . . ?
O2 C27 C32 C31 178.8(5) . . . . ?
C28 C27 C32 C31 -0.5(8) . . . . ?
O2 C27 C32 C33 1.8(8) . . . . ?
C28 C27 C32 C33 -177.5(5) . . . . ?
C34A N14 C33 C32 -171(3) . . . . ?
C34 N14 C33 C32 179.6(10) . . . . ?
Ni3 N14 C33 C32 -3.5(9) . . . . ?
C31 C32 C33 N14 -179.2(6) . . . . ?
C27 C32 C33 N14 -2.1(9) . . . . ?
C33 N14 C34 C35 -154.3(9) . . . . ?
C34A N14 C34 C35 172(11) . . . . ?
Ni3 N14 C34 C35 28.3(14) . . . . ?
N14 C34 C35 N13 -54.5(16) . . . . ?
C37 N13 C35 C34 -72.6(14) . . . . ?
C36 N13 C35 C34 167.1(11) . . . . ?
C35A N13 C35 C34 -36(4) . . . . ?
Ni3 N13 C35 C34 49.0(12) . . . . ?
C33 N14 C34A C35A -168(3) . . . . ?
C34 N14 C34A C35A -18(7) . . . . ?
Ni3 N14 C34A C35A 23(5) . . . . ?
N14 C34A C35A N13 -27(6) . . . . ?
C37 N13 C35A C34A -97(4) . . . . ?
C36 N13 C35A C34A 142(4) . . . . ?
C35 N13 C35A C34A 115(7) . . . . ?
Ni3 N13 C35A C34A 17(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.013
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.085

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.036 0.000 0.000 618 63 ' '
2 -0.005 0.500 0.500 618 64 ' '
3 0.334 0.949 0.385 19 1 ' '
4 0.334 0.551 0.885 19 1 ' '
5 0.665 0.449 0.115 19 1 ' '
6 0.665 0.051 0.615 19 1 ' '
_platon_squeeze_details          
;
;
_database_code_depnum_ccdc_archive 'CCDC 984713'
