# Electronic Supplementary Material (ESI) for RSC Advances
# This journal is © The Royal Society of Chemistry 2012


data_global
_journal_name_full               'Dalton Trans.'
_journal_coden_cambridge         0222
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
_publ_contact_author_name        'Shizheng Liu'
_publ_contact_author_email       interlsz@sina.com
loop_
_publ_author_name
'Jianmin Dou'
'Shizheng Liu'
'Suna Wang'
'Fan Cao'
'Haiying Fu'
;
Dacheng Li
;

data_100108b
_database_code_depnum_ccdc_archive 'CCDC 795063'
#TrackingRef '- 795063.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H52 N4 Ni4 O10'
_chemical_formula_weight         1007.72

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/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                   13.0082(15)
_cell_length_b                   12.0689(12)
_cell_length_c                   13.7934(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.5830(10)
_cell_angle_gamma                90.00
_cell_volume                     2064.3(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2484
_cell_measurement_theta_min      2.295
_cell_measurement_theta_max      24.811

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1048
_exptl_absorpt_coefficient_mu    1.860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6434
_exptl_absorpt_correction_T_max  0.7678
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10464
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_sigmaI/netI    0.0578
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.64
_diffrn_reflns_theta_max         25.01
_reflns_number_total             3643
_reflns_number_gt                2408
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0725P)^2^+2.2934P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3643
_refine_ls_number_parameters     275
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0431
_refine_ls_wR_factor_ref         0.1406
_refine_ls_wR_factor_gt          0.1028
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.000
_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 0.02732(5) 0.59716(5) 0.07707(5) 0.0315(2) Uani 1 1 d . . .
Ni2 Ni 0.20149(5) 0.44817(6) 0.05082(5) 0.0361(2) Uani 1 1 d . . .
N1 N -0.0193(3) 0.6407(3) 0.1982(3) 0.0342(10) Uani 1 1 d . . .
N2 N 0.3161(4) 0.3456(4) 0.0372(3) 0.0443(12) Uani 1 1 d . . .
O1 O -0.1036(3) 0.6827(3) -0.0040(2) 0.0361(9) Uani 1 1 d . . .
O2 O 0.1384(3) 0.4925(3) 0.1624(2) 0.0354(8) Uani 1 1 d . . .
O3 O 0.3031(3) 0.5730(3) 0.0750(3) 0.0503(11) Uani 1 1 d . . .
O4 O -0.0786(3) 0.4634(3) 0.0385(2) 0.0309(8) Uani 1 1 d . . .
O5 O 0.1514(3) 0.7193(3) 0.0945(3) 0.0433(9) Uani 1 1 d . . .
H5 H 0.2056 0.6925 0.0852 0.065 Uiso 1 1 d R . .
C1 C -0.1282(4) 0.6841(5) 0.1636(4) 0.0412(13) Uani 1 1 d . . .
H1A H -0.1392 0.7355 0.2137 0.049 Uiso 1 1 calc R . .
H1B H -0.1795 0.6240 0.1559 0.049 Uiso 1 1 calc R . .
C2 C -0.1473(4) 0.7436(5) 0.0618(4) 0.0415(14) Uani 1 1 d . . .
H2 H -0.1127 0.8165 0.0741 0.050 Uiso 1 1 calc R . .
C3 C 0.2686(4) 0.2408(5) -0.0096(4) 0.0492(15) Uani 1 1 d . . .
H3A H 0.2798 0.1837 0.0420 0.059 Uiso 1 1 calc R . .
H3B H 0.3034 0.2173 -0.0593 0.059 Uiso 1 1 calc R . .
C4 C -0.0365(5) 0.6080(5) 0.3677(4) 0.0483(15) Uani 1 1 d . . .
H4A H -0.0385 0.6817 0.3931 0.073 Uiso 1 1 calc R . .
H4B H -0.0013 0.5595 0.4229 0.073 Uiso 1 1 calc R . .
H4C H -0.1087 0.5825 0.3359 0.073 Uiso 1 1 calc R . .
C5 C 0.0253(5) 0.6083(4) 0.2904(4) 0.0375(13) Uani 1 1 d . . .
C6 C 0.1379(4) 0.5672(4) 0.3239(4) 0.0373(13) Uani 1 1 d . . .
C7 C 0.1896(4) 0.5132(4) 0.2596(4) 0.0351(12) Uani 1 1 d . . .
C8 C 0.2965(4) 0.4813(5) 0.3005(4) 0.0432(14) Uani 1 1 d . . .
H8 H 0.3302 0.4439 0.2595 0.052 Uiso 1 1 calc R . .
C9 C 0.3539(5) 0.5035(5) 0.3996(4) 0.0540(16) Uani 1 1 d . . .
H9 H 0.4262 0.4834 0.4243 0.065 Uiso 1 1 calc R . .
C10 C 0.3044(5) 0.5556(5) 0.4626(4) 0.0575(18) Uani 1 1 d . . .
H10 H 0.3428 0.5700 0.5301 0.069 Uiso 1 1 calc R . .
C11 C 0.1991(5) 0.5856(5) 0.4251(4) 0.0474(15) Uani 1 1 d . . .
H11 H 0.1663 0.6197 0.4686 0.057 Uiso 1 1 calc R . .
C12 C 0.4958(5) 0.2694(6) 0.0606(5) 0.070(2) Uani 1 1 d . . .
H12A H 0.5115 0.2228 0.1197 0.105 Uiso 1 1 calc R . .
H12B H 0.5616 0.3012 0.0553 0.105 Uiso 1 1 calc R . .
H12C H 0.4626 0.2260 0.0010 0.105 Uiso 1 1 calc R . .
C13 C 0.4198(5) 0.3611(5) 0.0698(4) 0.0449(14) Uani 1 1 d . . .
C14 C 0.4660(4) 0.4640(5) 0.1203(4) 0.0460(15) Uani 1 1 d . . .
C15 C 0.4067(4) 0.5633(5) 0.1186(4) 0.0458(15) Uani 1 1 d . . .
C16 C 0.4628(5) 0.6570(6) 0.1677(5) 0.0593(18) Uani 1 1 d . . .
H16 H 0.4250 0.7226 0.1662 0.071 Uiso 1 1 calc R . .
C17 C 0.5715(6) 0.6554(7) 0.2178(5) 0.073(2) Uani 1 1 d . . .
H17 H 0.6063 0.7195 0.2482 0.088 Uiso 1 1 calc R . .
C18 C 0.6281(6) 0.5594(9) 0.2226(7) 0.091(3) Uani 1 1 d . . .
H18 H 0.7010 0.5568 0.2590 0.109 Uiso 1 1 calc R . .
C19 C 0.5772(5) 0.4671(7) 0.1737(5) 0.071(2) Uani 1 1 d . . .
H19 H 0.6178 0.4032 0.1756 0.086 Uiso 1 1 calc R . .
C20 C -0.0939(5) 0.3943(5) 0.1160(4) 0.0423(14) Uani 1 1 d . . .
H20A H -0.1290 0.4356 0.1565 0.063 Uiso 1 1 calc R . .
H20B H -0.0253 0.3684 0.1583 0.063 Uiso 1 1 calc R . .
H20C H -0.1380 0.3321 0.0856 0.063 Uiso 1 1 calc R . .
C21 C 0.1820(5) 0.7966(5) 0.1762(4) 0.0603(18) Uani 1 1 d . . .
H21A H 0.2208 0.7588 0.2376 0.090 Uiso 1 1 calc R . .
H21B H 0.1186 0.8304 0.1850 0.090 Uiso 1 1 calc R . .
H21C H 0.2271 0.8527 0.1611 0.090 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.0370(4) 0.0284(4) 0.0273(4) -0.0018(3) 0.0071(3) 0.0025(3)
Ni2 0.0350(4) 0.0344(4) 0.0363(4) -0.0034(3) 0.0067(3) 0.0051(3)
N1 0.037(3) 0.034(3) 0.032(2) -0.004(2) 0.011(2) 0.002(2)
N2 0.044(3) 0.044(3) 0.042(3) 0.000(2) 0.008(2) 0.009(2)
O1 0.042(2) 0.030(2) 0.0346(19) -0.0001(16) 0.0093(16) 0.0066(16)
O2 0.038(2) 0.037(2) 0.0268(18) -0.0027(16) 0.0038(15) 0.0063(16)
O3 0.036(2) 0.047(3) 0.061(3) -0.003(2) 0.0032(19) -0.0007(18)
O4 0.037(2) 0.0273(19) 0.0284(17) 0.0028(15) 0.0103(15) 0.0033(15)
O5 0.047(2) 0.039(2) 0.043(2) -0.0090(18) 0.0114(18) -0.0037(18)
C1 0.051(4) 0.039(3) 0.036(3) -0.005(3) 0.017(3) 0.006(3)
C2 0.042(3) 0.032(3) 0.046(3) -0.009(3) 0.008(3) 0.005(3)
C3 0.051(4) 0.047(4) 0.050(3) 0.003(3) 0.015(3) 0.020(3)
C4 0.059(4) 0.053(4) 0.037(3) -0.004(3) 0.020(3) -0.004(3)
C5 0.053(3) 0.028(3) 0.032(3) -0.005(2) 0.012(3) -0.005(3)
C6 0.044(3) 0.030(3) 0.034(3) 0.002(2) 0.007(2) -0.004(2)
C7 0.042(3) 0.030(3) 0.028(3) -0.002(2) 0.003(2) -0.006(2)
C8 0.042(3) 0.046(4) 0.037(3) 0.005(3) 0.004(3) -0.001(3)
C9 0.046(4) 0.056(4) 0.048(4) 0.012(3) -0.004(3) 0.001(3)
C10 0.070(5) 0.059(4) 0.033(3) -0.003(3) -0.001(3) -0.006(4)
C11 0.067(4) 0.041(3) 0.029(3) -0.005(3) 0.007(3) -0.008(3)
C12 0.052(4) 0.086(6) 0.070(4) 0.007(4) 0.018(3) 0.028(4)
C13 0.041(4) 0.057(4) 0.038(3) 0.011(3) 0.014(3) 0.015(3)
C14 0.033(3) 0.066(4) 0.039(3) 0.009(3) 0.012(3) 0.005(3)
C15 0.033(3) 0.063(4) 0.042(3) 0.005(3) 0.012(3) -0.004(3)
C16 0.053(4) 0.064(5) 0.060(4) -0.007(4) 0.016(3) -0.017(3)
C17 0.052(5) 0.100(7) 0.063(4) 0.000(4) 0.011(4) -0.031(4)
C18 0.038(4) 0.130(8) 0.094(6) 0.018(6) 0.004(4) -0.011(5)
C19 0.035(4) 0.098(6) 0.076(5) 0.014(5) 0.009(3) 0.005(4)
C20 0.060(4) 0.038(3) 0.030(3) -0.001(2) 0.016(3) -0.001(3)
C21 0.078(5) 0.050(4) 0.052(4) -0.019(3) 0.019(3) -0.023(4)

_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 O2 2.010(3) . ?
Ni1 N1 2.011(4) . ?
Ni1 O1 2.016(3) . ?
Ni1 O4 2.041(3) 3_565 ?
Ni1 O4 2.084(3) . ?
Ni1 O5 2.145(4) . ?
Ni2 O3 1.965(4) . ?
Ni2 N2 1.990(5) . ?
Ni2 O4 2.006(3) 3_565 ?
Ni2 O1 2.010(3) 3_565 ?
Ni2 O2 2.023(3) . ?
N1 C5 1.288(6) . ?
N1 C1 1.451(6) . ?
N2 C13 1.301(7) . ?
N2 C3 1.469(7) . ?
O1 C2 1.414(6) . ?
O1 Ni2 2.010(3) 3_565 ?
O2 C7 1.327(6) . ?
O3 C15 1.304(6) . ?
O4 C20 1.416(6) . ?
O4 Ni2 2.006(3) 3_565 ?
O4 Ni1 2.041(3) 3_565 ?
O5 C21 1.425(6) . ?
O5 H5 0.8200 . ?
C1 C2 1.528(7) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.535(7) 3_565 ?
C2 H2 0.9800 . ?
C3 C2 1.535(7) 3_565 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.516(7) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 C6 1.483(8) . ?
C6 C11 1.401(7) . ?
C6 C7 1.423(7) . ?
C7 C8 1.388(7) . ?
C8 C9 1.372(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.380(9) . ?
C9 H9 0.9300 . ?
C10 C11 1.359(8) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 C13 1.514(8) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.462(8) . ?
C14 C19 1.412(8) . ?
C14 C15 1.421(8) . ?
C15 C16 1.405(8) . ?
C16 C17 1.373(9) . ?
C16 H16 0.9300 . ?
C17 C18 1.364(11) . ?
C17 H17 0.9300 . ?
C18 C19 1.365(11) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ni1 N1 91.21(15) . . ?
O2 Ni1 O1 169.65(14) . . ?
N1 Ni1 O1 84.91(15) . . ?
O2 Ni1 O4 83.45(13) . 3_565 ?
N1 Ni1 O4 173.79(15) . 3_565 ?
O1 Ni1 O4 99.81(13) . 3_565 ?
O2 Ni1 O4 88.03(13) . . ?
N1 Ni1 O4 94.14(15) . . ?
O1 Ni1 O4 82.70(13) . . ?
O4 Ni1 O4 82.54(13) 3_565 . ?
O2 Ni1 O5 88.99(14) . . ?
N1 Ni1 O5 97.64(15) . . ?
O1 Ni1 O5 101.01(14) . . ?
O4 Ni1 O5 85.47(13) 3_565 . ?
O4 Ni1 O5 167.90(13) . . ?
O3 Ni2 N2 90.49(18) . . ?
O3 Ni2 O4 93.83(15) . 3_565 ?
N2 Ni2 O4 138.93(16) . 3_565 ?
O3 Ni2 O1 170.35(16) . 3_565 ?
N2 Ni2 O1 84.30(17) . 3_565 ?
O4 Ni2 O1 84.87(13) 3_565 3_565 ?
O3 Ni2 O2 94.26(16) . . ?
N2 Ni2 O2 136.37(16) . . ?
O4 Ni2 O2 84.02(13) 3_565 . ?
O1 Ni2 O2 95.11(14) 3_565 . ?
C5 N1 C1 122.5(4) . . ?
C5 N1 Ni1 125.6(4) . . ?
C1 N1 Ni1 109.3(3) . . ?
C13 N2 C3 122.0(5) . . ?
C13 N2 Ni2 127.4(4) . . ?
C3 N2 Ni2 110.5(3) . . ?
C2 O1 Ni2 106.0(3) . 3_565 ?
C2 O1 Ni1 110.2(3) . . ?
Ni2 O1 Ni1 97.05(14) 3_565 . ?
C7 O2 Ni1 121.7(3) . . ?
C7 O2 Ni2 128.5(3) . . ?
Ni1 O2 Ni2 96.05(14) . . ?
C15 O3 Ni2 123.9(4) . . ?
C20 O4 Ni2 120.6(3) . 3_565 ?
C20 O4 Ni1 122.2(3) . 3_565 ?
Ni2 O4 Ni1 95.64(13) 3_565 3_565 ?
C20 O4 Ni1 119.8(3) . . ?
Ni2 O4 Ni1 95.00(13) 3_565 . ?
Ni1 O4 Ni1 97.46(13) 3_565 . ?
C21 O5 Ni1 124.0(3) . . ?
C21 O5 H5 109.5 . . ?
Ni1 O5 H5 111.5 . . ?
N1 C1 C2 110.1(4) . . ?
N1 C1 H1A 109.6 . . ?
C2 C1 H1A 109.6 . . ?
N1 C1 H1B 109.6 . . ?
C2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.2 . . ?
O1 C2 C1 111.2(4) . . ?
O1 C2 C3 108.6(4) . 3_565 ?
C1 C2 C3 110.3(5) . 3_565 ?
O1 C2 H2 108.9 . . ?
C1 C2 H2 108.9 . . ?
C3 C2 H2 108.9 3_565 . ?
N2 C3 C2 109.6(4) . 3_565 ?
N2 C3 H3A 109.7 . . ?
C2 C3 H3A 109.7 3_565 . ?
N2 C3 H3B 109.7 . . ?
C2 C3 H3B 109.7 3_565 . ?
H3A C3 H3B 108.2 . . ?
C5 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C5 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N1 C5 C6 121.1(5) . . ?
N1 C5 C4 121.3(5) . . ?
C6 C5 C4 117.6(5) . . ?
C11 C6 C7 117.5(5) . . ?
C11 C6 C5 117.9(5) . . ?
C7 C6 C5 124.6(5) . . ?
O2 C7 C8 119.6(5) . . ?
O2 C7 C6 121.9(5) . . ?
C8 C7 C6 118.5(5) . . ?
C9 C8 C7 121.9(6) . . ?
C9 C8 H8 119.1 . . ?
C7 C8 H8 119.1 . . ?
C8 C9 C10 120.0(6) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
C11 C10 C9 119.4(5) . . ?
C11 C10 H10 120.3 . . ?
C9 C10 H10 120.3 . . ?
C10 C11 C6 122.7(6) . . ?
C10 C11 H11 118.6 . . ?
C6 C11 H11 118.6 . . ?
C13 C12 H12A 109.5 . . ?
C13 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C13 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N2 C13 C14 121.4(5) . . ?
N2 C13 C12 120.1(6) . . ?
C14 C13 C12 118.4(5) . . ?
C19 C14 C15 116.9(6) . . ?
C19 C14 C13 118.7(6) . . ?
C15 C14 C13 124.4(5) . . ?
O3 C15 C16 117.6(6) . . ?
O3 C15 C14 124.3(6) . . ?
C16 C15 C14 118.0(5) . . ?
C17 C16 C15 122.5(7) . . ?
C17 C16 H16 118.7 . . ?
C15 C16 H16 118.7 . . ?
C18 C17 C16 119.7(7) . . ?
C18 C17 H17 120.2 . . ?
C16 C17 H17 120.2 . . ?
C17 C18 C19 119.7(7) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
C18 C19 C14 123.2(7) . . ?
C18 C19 H19 118.4 . . ?
C14 C19 H19 118.4 . . ?
O4 C20 H20A 109.5 . . ?
O4 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O4 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O5 C21 H21A 109.5 . . ?
O5 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O5 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 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
O2 Ni1 N1 C5 4.7(5) . . . . ?
O1 Ni1 N1 C5 175.1(5) . . . . ?
O4 Ni1 N1 C5 92.8(4) . . . . ?
O5 Ni1 N1 C5 -84.4(4) . . . . ?
O2 Ni1 N1 C1 -157.4(3) . . . . ?
O1 Ni1 N1 C1 13.0(3) . . . . ?
O4 Ni1 N1 C1 -69.3(3) . . . . ?
O5 Ni1 N1 C1 113.4(3) . . . . ?
O3 Ni2 N2 C13 19.7(5) . . . . ?
O4 Ni2 N2 C13 116.1(4) 3_565 . . . ?
O1 Ni2 N2 C13 -168.5(5) 3_565 . . . ?
O2 Ni2 N2 C13 -77.0(5) . . . . ?
O3 Ni2 N2 C3 -164.7(4) . . . . ?
O4 Ni2 N2 C3 -68.3(4) 3_565 . . . ?
O1 Ni2 N2 C3 7.1(3) 3_565 . . . ?
O2 Ni2 N2 C3 98.6(4) . . . . ?
O2 Ni1 O1 C2 78.8(8) . . . . ?
N1 Ni1 O1 C2 10.5(3) . . . . ?
O4 Ni1 O1 C2 -173.6(3) 3_565 . . . ?
O4 Ni1 O1 C2 105.4(3) . . . . ?
O5 Ni1 O1 C2 -86.3(3) . . . . ?
O2 Ni1 O1 Ni2 -31.2(8) . . . 3_565 ?
N1 Ni1 O1 Ni2 -99.45(16) . . . 3_565 ?
O4 Ni1 O1 Ni2 76.49(15) 3_565 . . 3_565 ?
O4 Ni1 O1 Ni2 -4.60(13) . . . 3_565 ?
O5 Ni1 O1 Ni2 163.74(13) . . . 3_565 ?
N1 Ni1 O2 C7 -33.0(4) . . . . ?
O1 Ni1 O2 C7 -100.7(8) . . . . ?
O4 Ni1 O2 C7 150.2(4) 3_565 . . . ?
O4 Ni1 O2 C7 -127.1(4) . . . . ?
O5 Ni1 O2 C7 64.7(4) . . . . ?
N1 Ni1 O2 Ni2 -176.28(16) . . . . ?
O1 Ni1 O2 Ni2 116.0(7) . . . . ?
O4 Ni1 O2 Ni2 6.90(13) 3_565 . . . ?
O4 Ni1 O2 Ni2 89.62(14) . . . . ?
O5 Ni1 O2 Ni2 -78.65(15) . . . . ?
O3 Ni2 O2 C7 -53.1(4) . . . . ?
N2 Ni2 O2 C7 42.1(5) . . . . ?
O4 Ni2 O2 C7 -146.5(4) 3_565 . . . ?
O1 Ni2 O2 C7 129.2(4) 3_565 . . . ?
O3 Ni2 O2 Ni1 86.40(16) . . . . ?
N2 Ni2 O2 Ni1 -178.4(2) . . . . ?
O4 Ni2 O2 Ni1 -7.02(14) 3_565 . . . ?
O1 Ni2 O2 Ni1 -91.30(15) 3_565 . . . ?
N2 Ni2 O3 C15 -30.3(4) . . . . ?
O4 Ni2 O3 C15 -169.5(4) 3_565 . . . ?
O2 Ni2 O3 C15 106.3(4) . . . . ?
O2 Ni1 O4 C20 50.3(3) . . . . ?
N1 Ni1 O4 C20 -40.8(4) . . . . ?
O1 Ni1 O4 C20 -125.1(4) . . . . ?
O4 Ni1 O4 C20 133.9(4) 3_565 . . . ?
O5 Ni1 O4 C20 126.1(6) . . . . ?
O2 Ni1 O4 Ni2 179.98(13) . . . 3_565 ?
N1 Ni1 O4 Ni2 88.91(16) . . . 3_565 ?
O1 Ni1 O4 Ni2 4.59(13) . . . 3_565 ?
O4 Ni1 O4 Ni2 -96.37(15) 3_565 . . 3_565 ?
O5 Ni1 O4 Ni2 -104.2(6) . . . 3_565 ?
O2 Ni1 O4 Ni1 -83.65(14) . . . 3_565 ?
N1 Ni1 O4 Ni1 -174.72(15) . . . 3_565 ?
O1 Ni1 O4 Ni1 100.96(14) . . . 3_565 ?
O4 Ni1 O4 Ni1 0.0 3_565 . . 3_565 ?
O5 Ni1 O4 Ni1 -7.8(7) . . . 3_565 ?
O2 Ni1 O5 C21 -88.5(4) . . . . ?
N1 Ni1 O5 C21 2.6(4) . . . . ?
O1 Ni1 O5 C21 88.8(4) . . . . ?
O4 Ni1 O5 C21 -172.0(4) 3_565 . . . ?
O4 Ni1 O5 C21 -164.3(6) . . . . ?
C5 N1 C1 C2 164.7(5) . . . . ?
Ni1 N1 C1 C2 -32.5(5) . . . . ?
Ni2 O1 C2 C1 73.0(4) 3_565 . . . ?
Ni1 O1 C2 C1 -31.0(5) . . . . ?
Ni2 O1 C2 C3 -48.5(5) 3_565 . . 3_565 ?
Ni1 O1 C2 C3 -152.5(4) . . . 3_565 ?
N1 C1 C2 O1 42.7(6) . . . . ?
N1 C1 C2 C3 163.3(4) . . . 3_565 ?
C13 N2 C3 C2 -167.0(5) . . . 3_565 ?
Ni2 N2 C3 C2 17.1(5) . . . 3_565 ?
C1 N1 C5 C6 -178.3(5) . . . . ?
Ni1 N1 C5 C6 21.8(7) . . . . ?
C1 N1 C5 C4 3.4(8) . . . . ?
Ni1 N1 C5 C4 -156.6(4) . . . . ?
N1 C5 C6 C11 148.5(5) . . . . ?
C4 C5 C6 C11 -33.1(7) . . . . ?
N1 C5 C6 C7 -29.5(8) . . . . ?
C4 C5 C6 C7 148.9(5) . . . . ?
Ni1 O2 C7 C8 -145.2(4) . . . . ?
Ni2 O2 C7 C8 -14.6(7) . . . . ?
Ni1 O2 C7 C6 35.0(6) . . . . ?
Ni2 O2 C7 C6 165.6(4) . . . . ?
C11 C6 C7 O2 -179.8(5) . . . . ?
C5 C6 C7 O2 -1.8(8) . . . . ?
C11 C6 C7 C8 0.4(8) . . . . ?
C5 C6 C7 C8 178.4(5) . . . . ?
O2 C7 C8 C9 178.2(5) . . . . ?
C6 C7 C8 C9 -2.0(8) . . . . ?
C7 C8 C9 C10 2.2(9) . . . . ?
C8 C9 C10 C11 -0.8(10) . . . . ?
C9 C10 C11 C6 -0.8(10) . . . . ?
C7 C6 C11 C10 1.0(8) . . . . ?
C5 C6 C11 C10 -177.2(6) . . . . ?
C3 N2 C13 C14 -177.3(5) . . . . ?
Ni2 N2 C13 C14 -2.1(8) . . . . ?
C3 N2 C13 C12 -0.4(8) . . . . ?
Ni2 N2 C13 C12 174.7(4) . . . . ?
N2 C13 C14 C19 166.0(5) . . . . ?
C12 C13 C14 C19 -10.9(8) . . . . ?
N2 C13 C14 C15 -14.8(9) . . . . ?
C12 C13 C14 C15 168.3(6) . . . . ?
Ni2 O3 C15 C16 -154.9(4) . . . . ?
Ni2 O3 C15 C14 24.6(8) . . . . ?
C19 C14 C15 O3 -178.1(5) . . . . ?
C13 C14 C15 O3 2.8(9) . . . . ?
C19 C14 C15 C16 1.4(8) . . . . ?
C13 C14 C15 C16 -177.8(5) . . . . ?
O3 C15 C16 C17 178.6(6) . . . . ?
C14 C15 C16 C17 -0.9(9) . . . . ?
C15 C16 C17 C18 -1.3(11) . . . . ?
C16 C17 C18 C19 3.0(12) . . . . ?
C17 C18 C19 C14 -2.5(12) . . . . ?
C15 C14 C19 C18 0.2(10) . . . . ?
C13 C14 C19 C18 179.4(7) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5 O3 0.82 1.95 2.720(5) 155.4 .

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.094

# Attachment '- 795064.cif'

data_100310b
_database_code_depnum_ccdc_archive 'CCDC 795064'
#TrackingRef '- 795064.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C73 H93 N11 Ni6 O17'
_chemical_formula_weight         1748.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'Pbcn '

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

_cell_length_a                   27.556(3)
_cell_length_b                   16.8879(16)
_cell_length_c                   17.3304(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     8065.0(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    4338
_cell_measurement_theta_min      2.2385
_cell_measurement_theta_max      26.1435

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3648
_exptl_absorpt_coefficient_mu    1.443
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5825
_exptl_absorpt_correction_T_max  0.8020
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            32407
_diffrn_reflns_av_R_equivalents  0.1438
_diffrn_reflns_av_sigmaI/netI    0.1178
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.41
_diffrn_reflns_theta_max         25.02
_reflns_number_total             7131
_reflns_number_gt                3284
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.1366P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7131
_refine_ls_number_parameters     505
_refine_ls_number_restraints     1276
_refine_ls_R_factor_all          0.1612
_refine_ls_R_factor_gt           0.0829
_refine_ls_wR_factor_ref         0.2639
_refine_ls_wR_factor_gt          0.2091
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      0.949
_refine_ls_shift/su_max          0.006
_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
C33 C 0.2837(10) 0.5123(12) 0.8325(11) 0.289(10) Uani 1 1 d DU . .
H33 H 0.2940 0.5132 0.8836 0.346 Uiso 1 1 calc R . .
O8 O 0.2604(7) 0.5694(10) 0.8081(11) 0.283(9) Uani 1 1 d DU . .
Ni1 Ni 0.44652(4) 0.18866(5) 0.20495(6) 0.0480(3) Uani 1 1 d . . .
Ni2 Ni 0.51792(4) 0.31211(6) 0.15945(7) 0.0501(4) Uani 1 1 d . . .
Ni3 Ni 0.33324(4) 0.24910(6) 0.18005(7) 0.0566(4) Uani 1 1 d . . .
N1 N 0.4419(3) 0.0690(4) 0.1982(4) 0.0573(17) Uani 1 1 d U . .
N2 N 0.3188(3) 0.1697(3) 0.1093(5) 0.0564(17) Uani 1 1 d U . .
N3 N 0.3495(3) 0.3257(3) 0.2588(4) 0.0591(18) Uani 1 1 d U . .
H3A H 0.3216 0.3451 0.2781 0.071 Uiso 1 1 calc R . .
H3B H 0.3647 0.3001 0.2973 0.071 Uiso 1 1 calc R . .
N4 N 0.5005(3) 0.4266(4) 0.1412(4) 0.0552(16) Uani 1 1 d U . .
O1 O 0.3733(2) 0.1785(3) 0.2323(3) 0.0541(14) Uani 1 1 d U . .
O2 O 0.52000(18) 0.1847(3) 0.1806(3) 0.0430(12) Uani 1 1 d U . .
O3 O 0.2974(2) 0.3251(3) 0.1318(4) 0.0700(16) Uani 1 1 d U . .
O4 O 0.45333(19) 0.3096(3) 0.2238(3) 0.0489(13) Uani 1 1 d U . .
O5 O 0.5822(2) 0.3291(3) 0.1125(4) 0.0666(15) Uani 1 1 d U . .
O6 O 0.4300(2) 0.1991(3) 0.0911(3) 0.0560(14) Uani 1 1 d U . .
O7 O 0.4859(2) 0.2883(3) 0.0539(3) 0.0578(14) Uani 1 1 d U . .
N5 N 0.2949(7) 0.4499(9) 0.7899(10) 0.260(9) Uani 1 1 d DU . .
N6 N 0.3734(9) 0.7758(16) 0.1979(15) 0.230(13) Uani 0.50 1 d PDU . .
C1 C 0.3969(3) 0.0408(5) 0.2366(6) 0.063(2) Uani 1 1 d U . .
H1A H 0.4015 0.0388 0.2921 0.075 Uiso 1 1 calc R . .
H1B H 0.3886 -0.0118 0.2186 0.075 Uiso 1 1 calc R . .
C2 C 0.3571(3) 0.0991(4) 0.2162(6) 0.058(2) Uani 1 1 d U . .
H2 H 0.3285 0.0878 0.2478 0.070 Uiso 1 1 calc R . .
C3 C 0.3430(3) 0.0943(5) 0.1320(5) 0.062(2) Uani 1 1 d U . .
H3C H 0.3717 0.0860 0.1006 0.074 Uiso 1 1 calc R . .
H3D H 0.3211 0.0501 0.1239 0.074 Uiso 1 1 calc R . .
C4 C 0.4645(4) -0.0677(5) 0.1700(6) 0.082(3) Uani 1 1 d U . .
H4A H 0.4489 -0.0812 0.2177 0.123 Uiso 1 1 calc R . .
H4B H 0.4950 -0.0948 0.1665 0.123 Uiso 1 1 calc R . .
H4C H 0.4442 -0.0832 0.1276 0.123 Uiso 1 1 calc R . .
C5 C 0.4731(3) 0.0220(5) 0.1669(5) 0.057(2) Uani 1 1 d U . .
C6 C 0.5150(3) 0.0516(5) 0.1258(5) 0.0551(19) Uani 1 1 d U . .
C7 C 0.5358(3) 0.1290(5) 0.1288(5) 0.0557(19) Uani 1 1 d U . .
C8 C 0.5754(4) 0.1479(5) 0.0837(6) 0.064(2) Uani 1 1 d U . .
H8 H 0.5886 0.1984 0.0875 0.077 Uiso 1 1 calc R . .
C9 C 0.5960(4) 0.0945(6) 0.0330(6) 0.079(3) Uani 1 1 d U . .
H9 H 0.6225 0.1084 0.0028 0.094 Uiso 1 1 calc R . .
C10 C 0.5753(4) 0.0178(6) 0.0286(6) 0.081(3) Uani 1 1 d U . .
H10 H 0.5884 -0.0194 -0.0050 0.097 Uiso 1 1 calc R . .
C11 C 0.5376(4) -0.0013(6) 0.0720(6) 0.071(2) Uani 1 1 d U . .
H11 H 0.5249 -0.0521 0.0673 0.085 Uiso 1 1 calc R . .
C12 C 0.2979(4) 0.1068(5) -0.0127(6) 0.080(3) Uani 1 1 d U . .
H12A H 0.3259 0.0744 -0.0032 0.120 Uiso 1 1 calc R . .
H12B H 0.2989 0.1260 -0.0648 0.120 Uiso 1 1 calc R . .
H12C H 0.2691 0.0759 -0.0052 0.120 Uiso 1 1 calc R . .
C13 C 0.2978(3) 0.1764(4) 0.0427(6) 0.060(2) Uani 1 1 d U . .
C14 C 0.2735(4) 0.2480(5) 0.0179(6) 0.067(2) Uani 1 1 d U . .
C15 C 0.2752(3) 0.3182(5) 0.0645(6) 0.066(2) Uani 1 1 d U . .
C16 C 0.2496(4) 0.3867(5) 0.0365(7) 0.076(2) Uani 1 1 d U . .
H16 H 0.2493 0.4327 0.0660 0.091 Uiso 1 1 calc R . .
C17 C 0.2259(4) 0.3854(6) -0.0327(7) 0.083(3) Uani 1 1 d U . .
H17 H 0.2107 0.4313 -0.0499 0.100 Uiso 1 1 calc R . .
C18 C 0.2237(4) 0.3182(6) -0.0778(7) 0.086(3) Uani 1 1 d U . .
H18 H 0.2065 0.3174 -0.1240 0.103 Uiso 1 1 calc R . .
C19 C 0.2484(4) 0.2518(5) -0.0515(7) 0.077(2) Uani 1 1 d U . .
H19 H 0.2480 0.2067 -0.0824 0.092 Uiso 1 1 calc R . .
C20 C 0.3801(3) 0.3934(4) 0.2354(5) 0.055(2) Uani 1 1 d U . .
H20A H 0.3906 0.4214 0.2814 0.066 Uiso 1 1 calc R . .
H20B H 0.3607 0.4296 0.2049 0.066 Uiso 1 1 calc R . .
C21 C 0.4242(3) 0.3698(4) 0.1894(5) 0.0559(19) Uani 1 1 d U . .
H21 H 0.4135 0.3513 0.1386 0.067 Uiso 1 1 calc R . .
C22 C 0.4533(3) 0.4447(4) 0.1788(5) 0.0546(19) Uani 1 1 d U . .
H22A H 0.4352 0.4817 0.1472 0.065 Uiso 1 1 calc R . .
H22B H 0.4591 0.4692 0.2286 0.065 Uiso 1 1 calc R . .
C23 C 0.5083(4) 0.5680(5) 0.1080(6) 0.087(3) Uani 1 1 d U . .
H23A H 0.4807 0.5719 0.1416 0.131 Uiso 1 1 calc R . .
H23B H 0.4992 0.5840 0.0569 0.131 Uiso 1 1 calc R . .
H23C H 0.5337 0.6018 0.1267 0.131 Uiso 1 1 calc R . .
C24 C 0.5264(4) 0.4817(5) 0.1063(6) 0.062(2) Uani 1 1 d U . .
C25 C 0.5700(4) 0.4641(5) 0.0649(6) 0.067(2) Uani 1 1 d U . .
C26 C 0.5965(4) 0.3890(5) 0.0696(6) 0.067(2) Uani 1 1 d U . .
C27 C 0.6389(4) 0.3791(6) 0.0271(6) 0.081(3) Uani 1 1 d U . .
H27 H 0.6555 0.3313 0.0301 0.097 Uiso 1 1 calc R . .
C28 C 0.6567(4) 0.4377(7) -0.0190(6) 0.089(3) Uani 1 1 d U . .
H28 H 0.6844 0.4283 -0.0481 0.107 Uiso 1 1 calc R . .
C29 C 0.6344(4) 0.5106(7) -0.0232(7) 0.091(3) Uani 1 1 d U . .
H29 H 0.6477 0.5510 -0.0528 0.109 Uiso 1 1 calc R . .
C30 C 0.5916(4) 0.5226(6) 0.0173(6) 0.076(2) Uani 1 1 d U . .
H30 H 0.5764 0.5715 0.0130 0.091 Uiso 1 1 calc R . .
C31 C 0.4523(3) 0.2400(5) 0.0410(5) 0.055(2) Uani 1 1 d U . .
C32 C 0.4329(4) 0.2315(5) -0.0401(6) 0.084(3) Uani 1 1 d U . .
H32A H 0.4087 0.2712 -0.0492 0.126 Uiso 1 1 calc R . .
H32B H 0.4189 0.1799 -0.0464 0.126 Uiso 1 1 calc R . .
H32C H 0.4590 0.2381 -0.0763 0.126 Uiso 1 1 calc R . .
C34 C 0.2787(7) 0.4350(12) 0.7106(10) 0.255(10) Uani 1 1 d DU . .
H34A H 0.2464 0.4551 0.7040 0.383 Uiso 1 1 calc R . .
H34B H 0.2789 0.3790 0.7008 0.383 Uiso 1 1 calc R . .
H34C H 0.3002 0.4610 0.6752 0.383 Uiso 1 1 calc R . .
C35 C 0.3308(8) 0.3902(13) 0.8160(13) 0.289(11) Uani 1 1 d DU . .
H35A H 0.3630 0.4093 0.8061 0.434 Uiso 1 1 calc R . .
H35B H 0.3257 0.3415 0.7885 0.434 Uiso 1 1 calc R . .
H35C H 0.3269 0.3810 0.8703 0.434 Uiso 1 1 calc R . .
O9 O 0.4403(10) 0.7414(16) 0.2415(19) 0.269(13) Uani 0.50 1 d PDU . .
C36 C 0.4159(11) 0.742(2) 0.1808(16) 0.252(14) Uani 0.50 1 d PDU . .
H36 H 0.4256 0.7233 0.1329 0.302 Uiso 0.50 1 calc PR . .
C37 C 0.3668(13) 0.8128(17) 0.2738(16) 0.239(14) Uani 0.50 1 d PDU . .
H37A H 0.3650 0.7725 0.3127 0.358 Uiso 0.50 1 calc PR . .
H37B H 0.3373 0.8431 0.2739 0.358 Uiso 0.50 1 calc PR . .
H37C H 0.3938 0.8471 0.2844 0.358 Uiso 0.50 1 calc PR . .
C38 C 0.3371(12) 0.790(2) 0.139(2) 0.255(15) Uani 0.50 1 d PDU . .
H38A H 0.3503 0.7771 0.0895 0.382 Uiso 0.50 1 calc PR . .
H38B H 0.3275 0.8443 0.1403 0.382 Uiso 0.50 1 calc PR . .
H38C H 0.3093 0.7568 0.1492 0.382 Uiso 0.50 1 calc PR . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C33 0.30(2) 0.27(2) 0.295(18) -0.068(17) 0.164(16) -0.117(18)
O8 0.260(18) 0.272(19) 0.317(17) -0.088(15) 0.146(13) -0.100(15)
Ni1 0.0591(7) 0.0287(5) 0.0563(7) -0.0014(5) 0.0004(5) 0.0004(5)
Ni2 0.0599(7) 0.0342(6) 0.0564(8) 0.0041(5) 0.0028(6) 0.0007(5)
Ni3 0.0586(7) 0.0355(6) 0.0757(9) -0.0092(5) -0.0013(6) 0.0005(5)
N1 0.067(4) 0.038(3) 0.067(4) -0.005(3) -0.001(3) 0.002(3)
N2 0.062(4) 0.029(3) 0.078(4) -0.001(3) -0.001(3) -0.003(3)
N3 0.064(4) 0.038(4) 0.075(4) -0.006(3) 0.000(4) -0.003(3)
N4 0.061(4) 0.038(3) 0.067(4) 0.000(3) -0.001(3) -0.002(3)
O1 0.059(3) 0.031(3) 0.072(3) -0.006(2) 0.001(3) -0.006(2)
O2 0.052(3) 0.029(2) 0.048(3) -0.003(2) 0.009(2) 0.004(2)
O3 0.079(4) 0.037(3) 0.094(4) -0.008(3) -0.018(3) 0.009(3)
O4 0.058(3) 0.026(2) 0.063(3) 0.004(2) 0.008(3) 0.006(2)
O5 0.071(4) 0.052(3) 0.076(4) 0.005(3) 0.010(3) 0.002(3)
O6 0.067(3) 0.038(3) 0.063(3) 0.000(2) 0.002(3) -0.001(2)
O7 0.069(3) 0.045(3) 0.060(3) 0.005(2) -0.006(3) -0.001(3)
N5 0.284(19) 0.217(18) 0.280(17) -0.071(15) 0.164(16) -0.110(15)
N6 0.32(3) 0.16(2) 0.21(2) 0.099(17) -0.12(2) -0.16(2)
C1 0.068(5) 0.036(4) 0.084(5) -0.005(4) -0.010(4) -0.005(4)
C2 0.064(5) 0.035(4) 0.076(5) -0.005(4) -0.003(4) -0.008(3)
C3 0.068(5) 0.033(4) 0.084(5) -0.001(4) -0.004(4) 0.003(3)
C4 0.110(8) 0.035(5) 0.101(8) -0.013(5) -0.013(6) 0.009(5)
C5 0.073(5) 0.033(4) 0.066(4) -0.010(3) -0.014(4) 0.005(4)
C6 0.062(4) 0.043(4) 0.061(4) -0.005(3) -0.002(4) 0.017(3)
C7 0.067(4) 0.038(4) 0.062(4) -0.009(3) -0.001(4) 0.011(3)
C8 0.065(5) 0.055(4) 0.073(5) -0.002(4) 0.008(4) 0.004(4)
C9 0.075(5) 0.085(5) 0.077(6) -0.013(5) 0.007(5) 0.017(5)
C10 0.085(6) 0.077(5) 0.079(6) -0.031(5) 0.002(5) 0.016(5)
C11 0.071(5) 0.059(4) 0.081(5) -0.019(4) -0.002(4) 0.012(4)
C12 0.091(7) 0.061(6) 0.089(7) -0.012(5) -0.025(6) 0.002(5)
C13 0.061(4) 0.035(4) 0.084(5) -0.003(4) -0.009(4) -0.005(3)
C14 0.074(5) 0.035(4) 0.091(5) 0.004(4) -0.006(4) -0.003(4)
C15 0.067(5) 0.036(4) 0.096(5) 0.006(4) -0.012(5) 0.004(4)
C16 0.080(5) 0.040(4) 0.107(6) 0.000(4) -0.009(5) 0.008(4)
C17 0.084(6) 0.049(5) 0.116(6) 0.010(5) -0.023(5) 0.008(4)
C18 0.094(6) 0.061(5) 0.103(6) 0.009(5) -0.030(5) 0.001(5)
C19 0.087(5) 0.050(4) 0.092(6) 0.000(4) -0.020(5) -0.007(4)
C20 0.059(5) 0.034(4) 0.073(5) -0.003(4) -0.002(4) -0.001(3)
C21 0.064(4) 0.030(3) 0.074(4) 0.003(3) -0.003(4) 0.004(3)
C22 0.064(5) 0.035(4) 0.064(5) 0.005(3) -0.008(4) 0.007(3)
C23 0.112(8) 0.034(5) 0.116(8) 0.014(5) -0.001(7) -0.010(5)
C24 0.072(5) 0.043(4) 0.072(5) 0.012(4) -0.004(4) -0.009(4)
C25 0.074(5) 0.056(4) 0.070(5) 0.022(4) -0.005(4) -0.013(4)
C26 0.069(5) 0.065(4) 0.066(5) 0.016(4) 0.007(4) -0.011(4)
C27 0.074(6) 0.082(5) 0.087(6) 0.028(5) 0.007(5) -0.006(5)
C28 0.078(6) 0.102(6) 0.086(6) 0.020(5) 0.015(5) -0.011(5)
C29 0.089(6) 0.096(6) 0.088(6) 0.032(5) -0.003(5) -0.019(5)
C30 0.079(5) 0.070(5) 0.077(5) 0.024(4) 0.002(5) -0.011(4)
C31 0.074(5) 0.034(4) 0.057(5) 0.003(4) 0.003(4) 0.013(4)
C32 0.125(9) 0.053(6) 0.074(7) 0.004(5) -0.019(6) -0.018(5)
C34 0.245(19) 0.281(19) 0.239(18) -0.143(17) 0.116(16) -0.124(15)
C35 0.28(2) 0.28(2) 0.32(2) -0.088(19) 0.151(16) -0.101(17)
O9 0.38(3) 0.23(2) 0.19(2) 0.093(18) -0.11(2) -0.14(2)
C36 0.35(3) 0.18(2) 0.23(2) 0.090(18) -0.10(2) -0.15(2)
C37 0.35(3) 0.16(2) 0.21(3) 0.109(19) -0.09(3) -0.13(2)
C38 0.35(3) 0.18(2) 0.23(3) 0.10(2) -0.08(2) -0.14(2)

_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
C33 O8 1.233(9) . ?
C33 N5 1.323(9) . ?
C33 H33 0.9300 . ?
Ni1 N1 2.028(6) . ?
Ni1 O6 2.033(6) . ?
Ni1 O2 2.069(5) . ?
Ni1 O4 2.076(5) . ?
Ni1 O1 2.079(6) . ?
Ni1 O2 2.189(5) 3_655 ?
Ni2 O5 1.970(6) . ?
Ni2 N4 2.017(6) . ?
Ni2 O7 2.070(6) . ?
Ni2 O4 2.101(5) . ?
Ni2 O4 2.173(6) 3_655 ?
Ni2 O2 2.183(5) . ?
Ni3 O3 1.822(6) . ?
Ni3 N2 1.861(7) . ?
Ni3 O1 1.861(6) . ?
Ni3 N3 1.933(7) . ?
N1 C5 1.290(10) . ?
N1 C1 1.484(11) . ?
N2 C13 1.296(11) . ?
N2 C3 1.490(10) . ?
N3 C20 1.477(10) . ?
N3 H3A 0.9000 . ?
N3 H3B 0.9000 . ?
N4 C24 1.319(10) . ?
N4 C22 1.486(11) . ?
O1 C2 1.441(9) . ?
O2 C7 1.372(9) . ?
O2 Ni1 2.189(5) 3_655 ?
O3 C15 1.323(11) . ?
O4 C21 1.426(9) . ?
O4 Ni2 2.173(6) 3_655 ?
O5 C26 1.315(10) . ?
O6 C31 1.268(10) . ?
O7 C31 1.256(10) . ?
N5 C34 1.466(9) . ?
N5 C35 1.483(9) . ?
N6 C36 1.333(9) . ?
N6 C38 1.445(9) . ?
N6 C37 1.468(9) . ?
C1 C2 1.518(12) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.512(12) . ?
C2 H2 0.9800 . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C4 C5 1.535(11) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 C6 1.446(12) . ?
C6 C7 1.429(11) . ?
C6 C11 1.434(12) . ?
C7 C8 1.378(12) . ?
C8 C9 1.381(12) . ?
C8 H8 0.9300 . ?
C9 C10 1.416(13) . ?
C9 H9 0.9300 . ?
C10 C11 1.324(14) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 C13 1.517(12) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.448(11) . ?
C14 C19 1.388(14) . ?
C14 C15 1.436(12) . ?
C15 C16 1.439(12) . ?
C16 C17 1.366(14) . ?
C16 H16 0.9300 . ?
C17 C18 1.380(14) . ?
C17 H17 0.9300 . ?
C18 C19 1.388(12) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 C21 1.507(11) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.508(11) . ?
C21 H21 0.9800 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.542(12) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 C25 1.430(13) . ?
C25 C30 1.419(12) . ?
C25 C26 1.465(13) . ?
C26 C27 1.392(13) . ?
C27 C28 1.362(13) . ?
C27 H27 0.9300 . ?
C28 C29 1.378(14) . ?
C28 H28 0.9300 . ?
C29 C30 1.385(14) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
C31 C32 1.509(13) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
O9 C36 1.248(10) . ?
C36 H36 0.9300 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O8 C33 N5 123.5(16) . . ?
O8 C33 H33 118.2 . . ?
N5 C33 H33 118.2 . . ?
N1 Ni1 O6 90.9(2) . . ?
N1 Ni1 O2 91.0(2) . . ?
O6 Ni1 O2 91.4(2) . . ?
N1 Ni1 O4 174.0(3) . . ?
O6 Ni1 O4 95.0(2) . . ?
O2 Ni1 O4 88.58(19) . . ?
N1 Ni1 O1 82.5(2) . . ?
O6 Ni1 O1 90.6(2) . . ?
O2 Ni1 O1 173.26(19) . . ?
O4 Ni1 O1 97.65(19) . . ?
N1 Ni1 O2 92.8(2) . 3_655 ?
O6 Ni1 O2 167.6(2) . 3_655 ?
O2 Ni1 O2 76.8(2) . 3_655 ?
O4 Ni1 O2 81.32(19) . 3_655 ?
O1 Ni1 O2 101.5(2) . 3_655 ?
O5 Ni2 N4 90.5(3) . . ?
O5 Ni2 O7 92.6(3) . . ?
N4 Ni2 O7 86.9(2) . . ?
O5 Ni2 O4 169.7(2) . . ?
N4 Ni2 O4 84.3(2) . . ?
O7 Ni2 O4 96.0(2) . . ?
O5 Ni2 O4 93.4(2) . 3_655 ?
N4 Ni2 O4 104.6(2) . 3_655 ?
O7 Ni2 O4 167.0(2) . 3_655 ?
O4 Ni2 O4 79.3(2) . 3_655 ?
O5 Ni2 O2 100.9(2) . . ?
N4 Ni2 O2 167.7(3) . . ?
O7 Ni2 O2 88.2(2) . . ?
O4 Ni2 O2 85.01(18) . . ?
O4 Ni2 O2 79.32(18) 3_655 . ?
O3 Ni3 N2 95.1(3) . . ?
O3 Ni3 O1 175.0(3) . . ?
N2 Ni3 O1 89.2(3) . . ?
O3 Ni3 N3 88.7(3) . . ?
N2 Ni3 N3 175.9(3) . . ?
O1 Ni3 N3 87.0(3) . . ?
C5 N1 C1 123.2(7) . . ?
C5 N1 Ni1 126.5(6) . . ?
C1 N1 Ni1 110.3(5) . . ?
C13 N2 C3 120.6(7) . . ?
C13 N2 Ni3 128.4(5) . . ?
C3 N2 Ni3 110.2(6) . . ?
C20 N3 Ni3 117.2(6) . . ?
C20 N3 H3A 108.0 . . ?
Ni3 N3 H3A 108.0 . . ?
C20 N3 H3B 108.0 . . ?
Ni3 N3 H3B 108.0 . . ?
H3A N3 H3B 107.2 . . ?
C24 N4 C22 122.0(7) . . ?
C24 N4 Ni2 128.2(6) . . ?
C22 N4 Ni2 109.7(5) . . ?
C2 O1 Ni3 108.5(5) . . ?
C2 O1 Ni1 109.5(5) . . ?
Ni3 O1 Ni1 114.3(3) . . ?
C7 O2 Ni1 117.9(5) . . ?
C7 O2 Ni2 125.0(5) . . ?
Ni1 O2 Ni2 88.67(18) . . ?
C7 O2 Ni1 118.7(5) . 3_655 ?
Ni1 O2 Ni1 103.1(2) . 3_655 ?
Ni2 O2 Ni1 97.65(19) . 3_655 ?
C15 O3 Ni3 126.4(5) . . ?
C21 O4 Ni1 125.8(5) . . ?
C21 O4 Ni2 103.9(4) . . ?
Ni1 O4 Ni2 90.75(19) . . ?
C21 O4 Ni2 125.5(5) . 3_655 ?
Ni1 O4 Ni2 101.5(2) . 3_655 ?
Ni2 O4 Ni2 100.7(2) . 3_655 ?
C26 O5 Ni2 127.9(6) . . ?
C31 O6 Ni1 127.1(6) . . ?
C31 O7 Ni2 126.8(6) . . ?
C33 N5 C34 126.1(12) . . ?
C33 N5 C35 121.8(13) . . ?
C34 N5 C35 111.8(11) . . ?
C36 N6 C38 121.5(14) . . ?
C36 N6 C37 119.2(13) . . ?
C38 N6 C37 118.3(13) . . ?
N1 C1 C2 106.9(7) . . ?
N1 C1 H1A 110.3 . . ?
C2 C1 H1A 110.3 . . ?
N1 C1 H1B 110.3 . . ?
C2 C1 H1B 110.3 . . ?
H1A C1 H1B 108.6 . . ?
O1 C2 C3 108.5(7) . . ?
O1 C2 C1 109.5(7) . . ?
C3 C2 C1 112.1(7) . . ?
O1 C2 H2 108.9 . . ?
C3 C2 H2 108.9 . . ?
C1 C2 H2 108.9 . . ?
N2 C3 C2 108.9(7) . . ?
N2 C3 H3C 109.9 . . ?
C2 C3 H3C 109.9 . . ?
N2 C3 H3D 109.9 . . ?
C2 C3 H3D 109.9 . . ?
H3C C3 H3D 108.3 . . ?
C5 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C5 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N1 C5 C6 121.8(7) . . ?
N1 C5 C4 119.3(9) . . ?
C6 C5 C4 118.8(8) . . ?
C7 C6 C11 114.8(9) . . ?
C7 C6 C5 128.3(8) . . ?
C11 C6 C5 116.8(8) . . ?
O2 C7 C8 117.6(8) . . ?
O2 C7 C6 121.5(8) . . ?
C8 C7 C6 120.6(8) . . ?
C7 C8 C9 122.3(9) . . ?
C7 C8 H8 118.9 . . ?
C9 C8 H8 118.9 . . ?
C8 C9 C10 117.9(10) . . ?
C8 C9 H9 121.1 . . ?
C10 C9 H9 121.1 . . ?
C11 C10 C9 120.5(9) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.7 . . ?
C10 C11 C6 124.0(9) . . ?
C10 C11 H11 118.0 . . ?
C6 C11 H11 118.0 . . ?
C13 C12 H12A 109.5 . . ?
C13 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C13 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N2 C13 C14 122.9(8) . . ?
N2 C13 C12 119.7(8) . . ?
C14 C13 C12 117.4(9) . . ?
C19 C14 C15 117.8(8) . . ?
C19 C14 C13 121.8(9) . . ?
C15 C14 C13 120.5(9) . . ?
O3 C15 C14 125.8(8) . . ?
O3 C15 C16 116.9(8) . . ?
C14 C15 C16 117.3(10) . . ?
C17 C16 C15 121.1(9) . . ?
C17 C16 H16 119.4 . . ?
C15 C16 H16 119.4 . . ?
C16 C17 C18 122.1(9) . . ?
C16 C17 H17 118.9 . . ?
C18 C17 H17 118.9 . . ?
C17 C18 C19 117.2(11) . . ?
C17 C18 H18 121.4 . . ?
C19 C18 H18 121.4 . . ?
C14 C19 C18 124.5(10) . . ?
C14 C19 H19 117.8 . . ?
C18 C19 H19 117.8 . . ?
N3 C20 C21 113.7(6) . . ?
N3 C20 H20A 108.8 . . ?
C21 C20 H20A 108.8 . . ?
N3 C20 H20B 108.8 . . ?
C21 C20 H20B 108.8 . . ?
H20A C20 H20B 107.7 . . ?
O4 C21 C20 114.9(7) . . ?
O4 C21 C22 110.5(7) . . ?
C20 C21 C22 105.8(6) . . ?
O4 C21 H21 108.5 . . ?
C20 C21 H21 108.5 . . ?
C22 C21 H21 108.5 . . ?
N4 C22 C21 110.2(6) . . ?
N4 C22 H22A 109.6 . . ?
C21 C22 H22A 109.6 . . ?
N4 C22 H22B 109.6 . . ?
C21 C22 H22B 109.6 . . ?
H22A C22 H22B 108.1 . . ?
C24 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C24 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N4 C24 C25 122.5(8) . . ?
N4 C24 C23 118.8(9) . . ?
C25 C24 C23 118.6(8) . . ?
C30 C25 C24 120.0(9) . . ?
C30 C25 C26 115.2(9) . . ?
C24 C25 C26 124.7(8) . . ?
O5 C26 C27 117.3(9) . . ?
O5 C26 C25 123.3(9) . . ?
C27 C26 C25 119.5(9) . . ?
C28 C27 C26 121.8(11) . . ?
C28 C27 H27 119.1 . . ?
C26 C27 H27 119.1 . . ?
C27 C28 C29 121.2(11) . . ?
C27 C28 H28 119.4 . . ?
C29 C28 H28 119.4 . . ?
C28 C29 C30 118.9(10) . . ?
C28 C29 H29 120.6 . . ?
C30 C29 H29 120.6 . . ?
C29 C30 C25 123.3(10) . . ?
C29 C30 H30 118.3 . . ?
C25 C30 H30 118.3 . . ?
O7 C31 O6 126.1(9) . . ?
O7 C31 C32 119.2(8) . . ?
O6 C31 C32 114.6(9) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N5 C34 H34A 109.5 . . ?
N5 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
N5 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N5 C35 H35A 109.5 . . ?
N5 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
N5 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
O9 C36 N6 107.0(15) . . ?
O9 C36 H36 126.5 . . ?
N6 C36 H36 126.5 . . ?
N6 C37 H37A 109.5 . . ?
N6 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
N6 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N6 C38 H38A 109.5 . . ?
N6 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
N6 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 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
O6 Ni1 N1 C5 74.5(8) . . . . ?
O2 Ni1 N1 C5 -16.9(8) . . . . ?
O1 Ni1 N1 C5 165.0(8) . . . . ?
O2 Ni1 N1 C5 -93.7(8) 3_655 . . . ?
O6 Ni1 N1 C1 -106.8(6) . . . . ?
O2 Ni1 N1 C1 161.8(6) . . . . ?
O1 Ni1 N1 C1 -16.3(6) . . . . ?
O2 Ni1 N1 C1 85.0(6) 3_655 . . . ?
O3 Ni3 N2 C13 11.0(9) . . . . ?
O1 Ni3 N2 C13 -166.5(8) . . . . ?
O3 Ni3 N2 C3 -179.5(6) . . . . ?
O1 Ni3 N2 C3 3.0(6) . . . . ?
O3 Ni3 N3 C20 -66.8(6) . . . . ?
O1 Ni3 N3 C20 110.6(6) . . . . ?
O5 Ni2 N4 C24 2.9(8) . . . . ?
O7 Ni2 N4 C24 -89.7(8) . . . . ?
O4 Ni2 N4 C24 173.9(8) . . . . ?
O4 Ni2 N4 C24 96.6(8) 3_655 . . . ?
O2 Ni2 N4 C24 -156.2(10) . . . . ?
O5 Ni2 N4 C22 -172.9(6) . . . . ?
O7 Ni2 N4 C22 94.5(5) . . . . ?
O4 Ni2 N4 C22 -1.8(5) . . . . ?
O4 Ni2 N4 C22 -79.2(6) 3_655 . . . ?
O2 Ni2 N4 C22 28.0(15) . . . . ?
N2 Ni3 O1 C2 -24.8(6) . . . . ?
N3 Ni3 O1 C2 153.6(6) . . . . ?
N2 Ni3 O1 Ni1 97.7(3) . . . . ?
N3 Ni3 O1 Ni1 -83.9(3) . . . . ?
N1 Ni1 O1 C2 -12.0(5) . . . . ?
O6 Ni1 O1 C2 78.9(5) . . . . ?
O4 Ni1 O1 C2 174.1(5) . . . . ?
O2 Ni1 O1 C2 -103.3(5) 3_655 . . . ?
N1 Ni1 O1 Ni3 -133.9(3) . . . . ?
O6 Ni1 O1 Ni3 -43.1(3) . . . . ?
O4 Ni1 O1 Ni3 52.1(3) . . . . ?
O2 Ni1 O1 Ni3 134.8(3) 3_655 . . . ?
N1 Ni1 O2 C7 36.7(6) . . . . ?
O6 Ni1 O2 C7 -54.3(5) . . . . ?
O4 Ni1 O2 C7 -149.3(5) . . . . ?
O2 Ni1 O2 C7 129.3(5) 3_655 . . . ?
N1 Ni1 O2 Ni2 166.3(2) . . . . ?
O6 Ni1 O2 Ni2 75.29(19) . . . . ?
O4 Ni1 O2 Ni2 -19.7(2) . . . . ?
O2 Ni1 O2 Ni2 -101.13(16) 3_655 . . . ?
N1 Ni1 O2 Ni1 -96.2(3) . . . 3_655 ?
O6 Ni1 O2 Ni1 172.8(2) . . . 3_655 ?
O4 Ni1 O2 Ni1 77.8(2) . . . 3_655 ?
O2 Ni1 O2 Ni1 -3.6(2) 3_655 . . 3_655 ?
O5 Ni2 O2 C7 -45.3(6) . . . . ?
N4 Ni2 O2 C7 113.4(12) . . . . ?
O7 Ni2 O2 C7 47.1(6) . . . . ?
O4 Ni2 O2 C7 143.2(6) . . . . ?
O4 Ni2 O2 C7 -136.8(6) 3_655 . . . ?
O5 Ni2 O2 Ni1 -169.0(2) . . . . ?
N4 Ni2 O2 Ni1 -10.3(12) . . . . ?
O7 Ni2 O2 Ni1 -76.6(2) . . . . ?
O4 Ni2 O2 Ni1 19.5(2) . . . . ?
O4 Ni2 O2 Ni1 99.6(2) 3_655 . . . ?
O5 Ni2 O2 Ni1 88.0(2) . . . 3_655 ?
N4 Ni2 O2 Ni1 -113.3(11) . . . 3_655 ?
O7 Ni2 O2 Ni1 -179.7(2) . . . 3_655 ?
O4 Ni2 O2 Ni1 -83.5(2) . . . 3_655 ?
O4 Ni2 O2 Ni1 -3.49(19) 3_655 . . 3_655 ?
N2 Ni3 O3 C15 -6.2(8) . . . . ?
N3 Ni3 O3 C15 175.2(8) . . . . ?
O6 Ni1 O4 C21 37.0(6) . . . . ?
O2 Ni1 O4 C21 128.3(6) . . . . ?
O1 Ni1 O4 C21 -54.3(6) . . . . ?
O2 Ni1 O4 C21 -154.9(6) 3_655 . . . ?
O6 Ni1 O4 Ni2 -70.8(2) . . . . ?
O2 Ni1 O4 Ni2 20.5(2) . . . . ?
O1 Ni1 O4 Ni2 -162.1(2) . . . . ?
O2 Ni1 O4 Ni2 97.4(2) 3_655 . . . ?
O6 Ni1 O4 Ni2 -171.8(2) . . . 3_655 ?
O2 Ni1 O4 Ni2 -80.5(2) . . . 3_655 ?
O1 Ni1 O4 Ni2 96.9(2) . . . 3_655 ?
O2 Ni1 O4 Ni2 -3.7(2) 3_655 . . 3_655 ?
O5 Ni2 O4 C21 87.6(14) . . . . ?
N4 Ni2 O4 C21 27.1(5) . . . . ?
O7 Ni2 O4 C21 -59.1(5) . . . . ?
O4 Ni2 O4 C21 133.2(4) 3_655 . . . ?
O2 Ni2 O4 C21 -146.8(5) . . . . ?
O5 Ni2 O4 Ni1 -145.1(12) . . . . ?
N4 Ni2 O4 Ni1 154.4(3) . . . . ?
O7 Ni2 O4 Ni1 68.2(2) . . . . ?
O4 Ni2 O4 Ni1 -99.53(18) 3_655 . . . ?
O2 Ni2 O4 Ni1 -19.5(2) . . . . ?
O5 Ni2 O4 Ni2 -43.3(13) . . . 3_655 ?
N4 Ni2 O4 Ni2 -103.8(3) . . . 3_655 ?
O7 Ni2 O4 Ni2 170.0(2) . . . 3_655 ?
O4 Ni2 O4 Ni2 2.3(2) 3_655 . . 3_655 ?
O2 Ni2 O4 Ni2 82.4(2) . . . 3_655 ?
N4 Ni2 O5 C26 -15.4(8) . . . . ?
O7 Ni2 O5 C26 71.5(8) . . . . ?
O4 Ni2 O5 C26 -75.4(16) . . . . ?
O4 Ni2 O5 C26 -120.1(8) 3_655 . . . ?
O2 Ni2 O5 C26 160.1(7) . . . . ?
N1 Ni1 O6 C31 -131.1(7) . . . . ?
O2 Ni1 O6 C31 -40.0(6) . . . . ?
O4 Ni1 O6 C31 48.7(6) . . . . ?
O1 Ni1 O6 C31 146.4(6) . . . . ?
O2 Ni1 O6 C31 -23.5(13) 3_655 . . . ?
O5 Ni2 O7 C31 145.2(7) . . . . ?
N4 Ni2 O7 C31 -124.4(7) . . . . ?
O4 Ni2 O7 C31 -40.4(7) . . . . ?
O4 Ni2 O7 C31 27.5(14) 3_655 . . . ?
O2 Ni2 O7 C31 44.3(7) . . . . ?
O8 C33 N5 C34 -5(5) . . . . ?
O8 C33 N5 C35 168(3) . . . . ?
C5 N1 C1 C2 -141.3(8) . . . . ?
Ni1 N1 C1 C2 39.9(8) . . . . ?
Ni3 O1 C2 C3 40.1(8) . . . . ?
Ni1 O1 C2 C3 -85.3(7) . . . . ?
Ni3 O1 C2 C1 162.7(6) . . . . ?
Ni1 O1 C2 C1 37.3(8) . . . . ?
N1 C1 C2 O1 -51.0(9) . . . . ?
N1 C1 C2 C3 69.5(9) . . . . ?
C13 N2 C3 C2 -171.1(8) . . . . ?
Ni3 N2 C3 C2 18.5(8) . . . . ?
O1 C2 C3 N2 -38.1(9) . . . . ?
C1 C2 C3 N2 -159.1(7) . . . . ?
C1 N1 C5 C6 176.2(8) . . . . ?
Ni1 N1 C5 C6 -5.2(13) . . . . ?
C1 N1 C5 C4 -1.0(13) . . . . ?
Ni1 N1 C5 C4 177.6(6) . . . . ?
N1 C5 C6 C7 17.4(15) . . . . ?
C4 C5 C6 C7 -165.5(9) . . . . ?
N1 C5 C6 C11 -159.1(8) . . . . ?
C4 C5 C6 C11 18.1(12) . . . . ?
Ni1 O2 C7 C8 148.1(7) . . . . ?
Ni2 O2 C7 C8 38.3(10) . . . . ?
Ni1 O2 C7 C8 -86.4(9) 3_655 . . . ?
Ni1 O2 C7 C6 -37.1(10) . . . . ?
Ni2 O2 C7 C6 -146.9(6) . . . . ?
Ni1 O2 C7 C6 88.4(8) 3_655 . . . ?
C11 C6 C7 O2 -176.2(8) . . . . ?
C5 C6 C7 O2 7.3(14) . . . . ?
C11 C6 C7 C8 -1.6(13) . . . . ?
C5 C6 C7 C8 -178.1(9) . . . . ?
O2 C7 C8 C9 176.1(8) . . . . ?
C6 C7 C8 C9 1.3(15) . . . . ?
C7 C8 C9 C10 -0.4(15) . . . . ?
C8 C9 C10 C11 0.0(16) . . . . ?
C9 C10 C11 C6 -0.4(17) . . . . ?
C7 C6 C11 C10 1.2(15) . . . . ?
C5 C6 C11 C10 178.1(10) . . . . ?
C3 N2 C13 C14 179.6(8) . . . . ?
Ni3 N2 C13 C14 -11.9(14) . . . . ?
C3 N2 C13 C12 0.0(13) . . . . ?
Ni3 N2 C13 C12 168.4(7) . . . . ?
N2 C13 C14 C19 -175.4(10) . . . . ?
C12 C13 C14 C19 4.2(14) . . . . ?
N2 C13 C14 C15 5.4(15) . . . . ?
C12 C13 C14 C15 -175.0(9) . . . . ?
Ni3 O3 C15 C14 2.7(14) . . . . ?
Ni3 O3 C15 C16 -178.8(7) . . . . ?
C19 C14 C15 O3 -179.9(10) . . . . ?
C13 C14 C15 O3 -0.7(15) . . . . ?
C19 C14 C15 C16 1.5(14) . . . . ?
C13 C14 C15 C16 -179.2(9) . . . . ?
O3 C15 C16 C17 179.5(9) . . . . ?
C14 C15 C16 C17 -1.8(15) . . . . ?
C15 C16 C17 C18 2.2(17) . . . . ?
C16 C17 C18 C19 -2.3(17) . . . . ?
C15 C14 C19 C18 -1.8(17) . . . . ?
C13 C14 C19 C18 179.0(10) . . . . ?
C17 C18 C19 C14 2.1(18) . . . . ?
Ni3 N3 C20 C21 -47.8(9) . . . . ?
Ni1 O4 C21 C20 91.9(8) . . . . ?
Ni2 O4 C21 C20 -166.9(6) . . . . ?
Ni2 O4 C21 C20 -52.7(9) 3_655 . . . ?
Ni1 O4 C21 C22 -148.6(5) . . . . ?
Ni2 O4 C21 C22 -47.4(7) . . . . ?
Ni2 O4 C21 C22 66.9(8) 3_655 . . . ?
N3 C20 C21 O4 -51.8(10) . . . . ?
N3 C20 C21 C22 -174.0(7) . . . . ?
C24 N4 C22 C21 160.7(8) . . . . ?
Ni2 N4 C22 C21 -23.2(8) . . . . ?
O4 C21 C22 N4 49.0(9) . . . . ?
C20 C21 C22 N4 173.9(7) . . . . ?
C22 N4 C24 C25 -175.2(8) . . . . ?
Ni2 N4 C24 C25 9.4(14) . . . . ?
C22 N4 C24 C23 2.9(13) . . . . ?
Ni2 N4 C24 C23 -172.4(6) . . . . ?
N4 C24 C25 C30 168.7(9) . . . . ?
C23 C24 C25 C30 -9.4(14) . . . . ?
N4 C24 C25 C26 -13.7(16) . . . . ?
C23 C24 C25 C26 168.2(9) . . . . ?
Ni2 O5 C26 C27 -164.2(7) . . . . ?
Ni2 O5 C26 C25 15.7(13) . . . . ?
C30 C25 C26 O5 178.4(9) . . . . ?
C24 C25 C26 O5 0.7(16) . . . . ?
C30 C25 C26 C27 -1.7(14) . . . . ?
C24 C25 C26 C27 -179.4(10) . . . . ?
O5 C26 C27 C28 -179.9(10) . . . . ?
C25 C26 C27 C28 0.2(16) . . . . ?
C26 C27 C28 C29 2.4(18) . . . . ?
C27 C28 C29 C30 -3.3(18) . . . . ?
C28 C29 C30 C25 1.7(18) . . . . ?
C24 C25 C30 C29 178.6(10) . . . . ?
C26 C25 C30 C29 0.8(15) . . . . ?
Ni2 O7 C31 O6 3.5(12) . . . . ?
Ni2 O7 C31 C32 179.1(6) . . . . ?
Ni1 O6 C31 O7 -7.9(12) . . . . ?
Ni1 O6 C31 C32 176.4(6) . . . . ?
C38 N6 C36 O9 177(3) . . . . ?
C37 N6 C36 O9 9(6) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3B O5 0.90 2.20 2.921(10) 137.0 3_655
N3 H3A O8 0.90 2.28 3.15(2) 161.2 7_565

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.157
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.154