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


data_z

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H21 N4 Ni O5'
_chemical_formula_sum            'C25 H21 N4 Ni O5'
_chemical_formula_weight         516.17

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   17.073(11)
_cell_length_b                   15.507(11)
_cell_length_c                   18.110(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.765(13)
_cell_angle_gamma                90.00
_cell_volume                     4739(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1555
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      20.58

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2136
_exptl_absorpt_coefficient_mu    0.863
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7296
_exptl_absorpt_correction_T_max  0.8961
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11691
_diffrn_reflns_av_R_equivalents  0.0740
_diffrn_reflns_av_unetI/netI     0.0927
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.01
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4129
_reflns_number_gt                2718
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0910P)²+3.5018P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4129
_refine_ls_number_parameters     322
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.1002
_refine_ls_R_factor_gt           0.0623
_refine_ls_wR_factor_ref         0.1740
_refine_ls_wR_factor_gt          0.1509
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.001
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.002

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4849(3) 0.1032(3) 0.4603(3) 0.0362(13) Uani 1 1 d . . .
H1 H 0.5154 0.0872 0.5053 0.043 Uiso 1 1 calc R . .
C2 C 0.4068(3) 0.0861(3) 0.4397(3) 0.0369(13) Uani 1 1 d . . .
H2 H 0.3743 0.0567 0.4679 0.044 Uiso 1 1 calc R . .
C3 C 0.4504(3) 0.1565(3) 0.3507(3) 0.0338(12) Uani 1 1 d . . .
H3 H 0.4519 0.1842 0.3053 0.041 Uiso 1 1 calc R . .
C4 C 0.3054(3) 0.1166(4) 0.3275(3) 0.0440(15) Uani 1 1 d . . .
H4A H 0.2910 0.0569 0.3164 0.053 Uiso 1 1 calc R . .
H4B H 0.3052 0.1465 0.2804 0.053 Uiso 1 1 calc R . .
C5 C 0.2448(3) 0.1572(4) 0.3692(3) 0.0343(12) Uani 1 1 d . . .
C6 C 0.2419(3) 0.2437(4) 0.3803(3) 0.0407(14) Uani 1 1 d . . .
H6 H 0.2773 0.2790 0.3603 0.049 Uiso 1 1 calc R . .
C7 C 0.1880(3) 0.2811(4) 0.4206(3) 0.0446(14) Uani 1 1 d . . .
H7 H 0.1872 0.3405 0.4278 0.053 Uiso 1 1 calc R . .
C8 C 0.1351(3) 0.2280(4) 0.4501(4) 0.0465(15) Uani 1 1 d . . .
H8 H 0.0969 0.2520 0.4754 0.056 Uiso 1 1 calc R . .
C9 C 0.1389(3) 0.1383(4) 0.4418(4) 0.0442(14) Uani 1 1 d . . .
C10 C 0.1931(3) 0.1037(4) 0.4003(3) 0.0435(14) Uani 1 1 d . . .
H10 H 0.1950 0.0443 0.3932 0.052 Uiso 1 1 calc R . .
C11 C 0.4134(3) 0.4214(4) 0.5206(4) 0.0549(17) Uani 1 1 d . . .
H11A H 0.3869 0.4347 0.4706 0.066 Uiso 1 1 calc R . .
H11B H 0.4205 0.4751 0.5484 0.066 Uiso 1 1 calc R . .
C12 C 0.5114(4) 0.3427(4) 0.4563(4) 0.0477(15) Uani 1 1 d . . .
H12 H 0.4804 0.3405 0.4094 0.057 Uiso 1 1 calc R . .
C13 C 0.6057(4) 0.3255(4) 0.5479(4) 0.0495(15) Uani 1 1 d . . .
H13 H 0.6534 0.3087 0.5760 0.059 Uiso 1 1 calc R . .
C14 C 0.5502(4) 0.3726(4) 0.5731(4) 0.0525(16) Uani 1 1 d . . .
H14 H 0.5522 0.3935 0.6215 0.063 Uiso 1 1 calc R . .
C15 C 0.6952(3) 0.0341(3) 0.3745(3) 0.0306(12) Uani 1 1 d . . .
C16 C 0.7224(3) -0.0266(3) 0.3178(3) 0.0275(11) Uani 1 1 d . . .
C17 C 0.6714(3) -0.0743(3) 0.2646(3) 0.0256(11) Uani 1 1 d . . .
C18 C 0.7056(3) -0.1277(3) 0.2167(3) 0.0263(11) Uani 1 1 d . . .
H18 H 0.6728 -0.1604 0.1816 0.032 Uiso 1 1 calc R . .
C19 C 0.7872(3) -0.1339(3) 0.2195(3) 0.0287(11) Uani 1 1 d . . .
C20 C 0.8362(3) -0.0858(4) 0.2710(3) 0.0370(13) Uani 1 1 d . . .
H20 H 0.8909 -0.0894 0.2734 0.044 Uiso 1 1 calc R . .
C21 C 0.8038(3) -0.0322(3) 0.3191(3) 0.0354(13) Uani 1 1 d . . .
H21 H 0.8372 0.0010 0.3532 0.042 Uiso 1 1 calc R . .
C22 C 0.8212(3) -0.1951(3) 0.1687(3) 0.0244(10) Uani 1 1 d . . .
C23 C 0.5836(3) -0.0707(3) 0.2582(3) 0.0288(11) Uani 1 1 d . . .
C24 C 0.5444(3) -0.0696(3) 0.3205(3) 0.0318(12) Uani 1 1 d . . .
H24 H 0.5735 -0.0681 0.3682 0.038 Uiso 1 1 calc R . .
C25 C 0.4625(3) -0.0709(3) 0.3115(3) 0.0308(12) Uani 1 1 d . . .
H25 H 0.4377 -0.0718 0.3538 0.037 Uiso 1 1 calc R . .
N1 N 0.5117(2) 0.1485(3) 0.4032(2) 0.0333(10) Uani 1 1 d . . .
N2 N 0.3846(2) 0.1198(3) 0.3701(2) 0.0320(10) Uani 1 1 d . . .
N3 N 0.5815(3) 0.3051(3) 0.4727(3) 0.0389(11) Uani 1 1 d . . .
N4 N 0.4902(3) 0.3847(3) 0.5158(3) 0.0419(12) Uani 1 1 d . . .
Ni1 Ni 0.62106(3) 0.20307(4) 0.41189(3) 0.0274(2) Uani 1 1 d D . .
O1 O 0.66269(19) 0.1030(2) 0.35083(18) 0.0329(8) Uani 1 1 d . . .
O2 O 0.7096(3) 0.0100(3) 0.44091(19) 0.0526(11) Uani 1 1 d . . .
O3 O 0.77926(18) -0.2224(2) 0.10971(18) 0.0315(8) Uani 1 1 d . . .
O4 O 0.89220(19) -0.2203(2) 0.18594(19) 0.0338(8) Uani 1 1 d . . .
O5 O 0.66423(18) 0.1423(2) 0.51060(18) 0.0345(8) Uani 1 1 d D . .
H1W H 0.677(3) 0.0914(8) 0.5090(6) 0.080 Uiso 1 1 d D . .
H2W H 0.691(2) 0.1705(8) 0.5434(11) 0.080 Uiso 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.355(7) . ?
C1 N1 1.385(6) . ?
C1 H1 0.9300 . ?
C2 N2 1.363(7) . ?
C2 H2 0.9300 . ?
C3 N1 1.308(6) . ?
C3 N2 1.354(6) . ?
C3 H3 0.9300 . ?
C4 N2 1.452(6) . ?
C4 C5 1.508(7) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.359(8) . ?
C5 C10 1.391(8) . ?
C6 C7 1.386(7) . ?
C6 H6 0.9300 . ?
C7 C8 1.387(8) . ?
C7 H7 0.9300 . ?
C8 C9 1.401(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.386(7) . ?
C9 C11 1.518(8) 7_556 ?
C10 H10 0.9300 . ?
C11 N4 1.445(7) . ?
C11 C9 1.518(8) 7_556 ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 N3 1.323(7) . ?
C12 N4 1.355(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.332(8) . ?
C13 N3 1.397(8) . ?
C13 H13 0.9300 . ?
C14 N4 1.355(8) . ?
C14 H14 0.9300 . ?
C15 O2 1.248(6) . ?
C15 O1 1.248(6) . ?
C15 C16 1.517(6) . ?
C16 C21 1.388(7) . ?
C16 C17 1.407(7) . ?
C17 C18 1.391(6) . ?
C17 C23 1.486(6) . ?
C18 C19 1.390(6) . ?
C18 H18 0.9300 . ?
C19 C20 1.373(7) . ?
C19 C22 1.500(6) . ?
C20 C21 1.380(7) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 O4 1.266(6) . ?
C22 O3 1.265(6) . ?
C22 Ni1 2.455(5) 4_645 ?
C23 C25 1.382(7) 2_655 ?
C23 C24 1.397(6) . ?
C24 C25 1.383(7) . ?
C24 H24 0.9300 . ?
C25 C23 1.382(7) 2_655 ?
C25 H25 0.9300 . ?
N1 Ni1 2.035(4) . ?
N3 Ni1 2.097(4) . ?
Ni1 O5 2.055(4) . ?
Ni1 O1 2.092(3) . ?
Ni1 O4 2.117(4) 4_655 ?
Ni1 O3 2.142(3) 4_655 ?
Ni1 C22 2.455(5) 4_655 ?
O3 Ni1 2.142(3) 4_645 ?
O4 Ni1 2.117(4) 4_645 ?
O5 H1W 0.8201(12) . ?
O5 H2W 0.8201(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 N1 108.4(5) . . ?
C2 C1 H1 125.8 . . ?
N1 C1 H1 125.8 . . ?
C1 C2 N2 107.7(4) . . ?
C1 C2 H2 126.1 . . ?
N2 C2 H2 126.2 . . ?
N1 C3 N2 112.0(4) . . ?
N1 C3 H3 124.0 . . ?
N2 C3 H3 124.0 . . ?
N2 C4 C5 112.0(4) . . ?
N2 C4 H4A 109.2 . . ?
C5 C4 H4A 109.2 . . ?
N2 C4 H4B 109.2 . . ?
C5 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
C6 C5 C10 119.3(5) . . ?
C6 C5 C4 122.0(5) . . ?
C10 C5 C4 118.6(5) . . ?
C5 C6 C7 122.2(5) . . ?
C5 C6 H6 118.9 . . ?
C7 C6 H6 118.9 . . ?
C6 C7 C8 118.5(6) . . ?
C6 C7 H7 120.8 . . ?
C8 C7 H7 120.8 . . ?
C7 C8 C9 120.3(5) . . ?
C7 C8 H8 119.8 . . ?
C9 C8 H8 119.8 . . ?
C10 C9 C8 119.2(5) . . ?
C10 C9 C11 119.6(5) . 7_556 ?
C8 C9 C11 121.1(5) . 7_556 ?
C9 C10 C5 120.4(6) . . ?
C9 C10 H10 119.8 . . ?
C5 C10 H10 119.8 . . ?
N4 C11 C9 112.8(5) . 7_556 ?
N4 C11 H11A 109.0 . . ?
C9 C11 H11A 109.0 7_556 . ?
N4 C11 H11B 109.0 . . ?
C9 C11 H11B 109.0 7_556 . ?
H11A C11 H11B 107.8 . . ?
N3 C12 N4 112.1(6) . . ?
N3 C12 H12 124.0 . . ?
N4 C12 H12 124.0 . . ?
C14 C13 N3 109.8(6) . . ?
C14 C13 H13 125.1 . . ?
N3 C13 H13 125.1 . . ?
C13 C14 N4 107.9(5) . . ?
C13 C14 H14 126.1 . . ?
N4 C14 H14 126.1 . . ?
O2 C15 O1 126.8(5) . . ?
O2 C15 C16 115.5(5) . . ?
O1 C15 C16 117.7(4) . . ?
C21 C16 C17 119.5(4) . . ?
C21 C16 C15 115.8(4) . . ?
C17 C16 C15 124.6(4) . . ?
C16 C17 C18 117.7(4) . . ?
C16 C17 C23 123.1(4) . . ?
C18 C17 C23 119.2(4) . . ?
C19 C18 C17 122.2(4) . . ?
C19 C18 H18 118.9 . . ?
C17 C18 H18 118.9 . . ?
C20 C19 C18 119.4(4) . . ?
C20 C19 C22 120.5(4) . . ?
C18 C19 C22 120.0(4) . . ?
C19 C20 C21 119.6(5) . . ?
C19 C20 H20 120.2 . . ?
C21 C20 H20 120.2 . . ?
C16 C21 C20 121.5(5) . . ?
C16 C21 H21 119.2 . . ?
C20 C21 H21 119.2 . . ?
O4 C22 O3 120.3(4) . . ?
O4 C22 C19 119.3(4) . . ?
O3 C22 C19 120.5(4) . . ?
O4 C22 Ni1 59.5(2) . 4_645 ?
O3 C22 Ni1 60.7(2) . 4_645 ?
C19 C22 Ni1 178.6(4) . 4_645 ?
C25 C23 C24 117.5(4) 2_655 . ?
C25 C23 C17 119.9(4) 2_655 . ?
C24 C23 C17 122.6(4) . . ?
C25 C24 C23 120.3(5) . . ?
C25 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
C24 C25 C23 122.2(4) . 2_655 ?
C24 C25 H25 118.9 . . ?
C23 C25 H25 118.9 2_655 . ?
C3 N1 C1 105.9(4) . . ?
C3 N1 Ni1 129.8(3) . . ?
C1 N1 Ni1 123.8(4) . . ?
C3 N2 C2 106.0(4) . . ?
C3 N2 C4 128.2(4) . . ?
C2 N2 C4 125.7(4) . . ?
C12 N3 C13 104.0(5) . . ?
C12 N3 Ni1 124.5(4) . . ?
C13 N3 Ni1 127.7(4) . . ?
C14 N4 C12 106.3(5) . . ?
C14 N4 C11 126.6(5) . . ?
C12 N4 C11 126.3(6) . . ?
N1 Ni1 O5 94.60(15) . . ?
N1 Ni1 O1 91.85(16) . . ?
O5 Ni1 O1 90.80(14) . . ?
N1 Ni1 N3 89.39(17) . . ?
O5 Ni1 N3 89.46(17) . . ?
O1 Ni1 N3 178.71(15) . . ?
N1 Ni1 O4 100.88(15) . 4_655 ?
O5 Ni1 O4 164.52(13) . 4_655 ?
O1 Ni1 O4 88.62(14) . 4_655 ?
N3 Ni1 O4 90.80(17) . 4_655 ?
N1 Ni1 O3 162.90(15) . 4_655 ?
O5 Ni1 O3 102.51(13) . 4_655 ?
O1 Ni1 O3 87.75(14) . 4_655 ?
N3 Ni1 O3 90.96(15) . 4_655 ?
O4 Ni1 O3 62.01(13) 4_655 4_655 ?
N1 Ni1 C22 131.91(16) . 4_655 ?
O5 Ni1 C22 133.49(15) . 4_655 ?
O1 Ni1 C22 87.92(15) . 4_655 ?
N3 Ni1 C22 90.99(16) . 4_655 ?
O4 Ni1 C22 31.03(14) 4_655 4_655 ?
O3 Ni1 C22 30.98(14) 4_655 4_655 ?
C15 O1 Ni1 128.5(3) . . ?
C22 O3 Ni1 88.3(3) . 4_645 ?
C22 O4 Ni1 89.4(3) . 4_645 ?
Ni1 O5 H1W 118.2(6) . . ?
Ni1 O5 H2W 118.3(6) . . ?
H1W O5 H2W 114.6(2) . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.998
_refine_diff_density_min         -0.887
_refine_diff_density_rms         0.101
_database_code_depnum_ccdc_archive 'CCDC 973827'

data_z

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H21 Mn N4 O5'
_chemical_formula_sum            'C25 H21 Mn N4 O5'
_chemical_formula_weight         512.40

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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   16.3353(12)
_cell_length_b                   16.0464(12)
_cell_length_c                   18.4433(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.6790(10)
_cell_angle_gamma                90.00
_cell_volume                     4734.3(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5003
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      27.39

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.38
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2112
_exptl_absorpt_coefficient_mu    0.602
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7734
_exptl_absorpt_correction_T_max  0.8036
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11955
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_av_sigmaI/netI    0.0273
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.80
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4167
_reflns_number_gt                3473
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0550P)²+2.6246P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4167
_refine_ls_number_parameters     322
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0328
_refine_ls_wR_factor_ref         0.0928
_refine_ls_wR_factor_gt          0.0857
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_restrained_S_all      0.999
_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
C2 C 0.70401(12) 0.13995(12) 0.77025(10) 0.0301(4) Uani 1 1 d . . .
C3 C 0.78841(11) 0.12569(11) 0.77599(10) 0.0282(4) Uani 1 1 d . . .
H3 H 0.8260 0.1526 0.8132 0.034 Uiso 1 1 calc R . .
C4 C 0.81946(11) 0.07260(11) 0.72817(10) 0.0268(4) Uani 1 1 d . . .
C5 C 0.76133(12) 0.03345(11) 0.67177(10) 0.0297(4) Uani 1 1 d . . .
C6 C 0.67681(12) 0.04778(14) 0.66633(12) 0.0393(5) Uani 1 1 d . . .
H6 H 0.6388 0.0217 0.6288 0.047 Uiso 1 1 calc R . .
C7 C 0.64728(12) 0.09985(14) 0.71517(12) 0.0399(5) Uani 1 1 d . . .
H7 H 0.5901 0.1078 0.7111 0.048 Uiso 1 1 calc R . .
C8 C 0.78624(12) -0.02644(12) 0.61660(11) 0.0323(4) Uani 1 1 d . . .
C9 C 0.95279(12) 0.06120(12) 0.67891(10) 0.0302(4) Uani 1 1 d . . .
H9 H 0.9217 0.0594 0.6307 0.036 Uiso 1 1 calc R . .
C10 C 0.96129(12) 0.06186(12) 0.80938(11) 0.0304(4) Uani 1 1 d . . .
H10 H 0.9356 0.0615 0.8500 0.037 Uiso 1 1 calc R . .
C11 C 0.91152(11) 0.06312(11) 0.73821(10) 0.0272(4) Uani 1 1 d . . .
C12 C 0.52915(19) 0.14517(18) 0.94712(17) 0.0720(9) Uani 1 1 d . . .
H12 H 0.5150 0.1332 0.8968 0.086 Uiso 1 1 calc R . .
C13 C 0.4914(2) 0.11246(19) 0.99897(18) 0.0764(9) Uani 1 1 d . . .
H13 H 0.4467 0.0754 0.9913 0.092 Uiso 1 1 calc R . .
C14 C 0.59005(14) 0.19525(15) 1.04919(14) 0.0475(6) Uani 1 1 d . . .
H14 H 0.6264 0.2254 1.0851 0.057 Uiso 1 1 calc R . .
C15 C 0.50337(16) 0.1363(2) 1.13471(15) 0.0673(8) Uani 1 1 d . . .
H15A H 0.5425 0.1648 1.1733 0.081 Uiso 1 1 calc R . .
H15B H 0.5026 0.0779 1.1482 0.081 Uiso 1 1 calc R . .
C16 C 0.41709(14) 0.17295(16) 1.12913(13) 0.0476(6) Uani 1 1 d . . .
C17 C 0.39542(16) 0.24783(16) 1.09327(14) 0.0527(6) Uani 1 1 d . . .
H17 H 0.4349 0.2768 1.0733 0.063 Uiso 1 1 calc R . .
C18 C 0.43784(13) 0.34863(14) 0.84551(12) 0.0384(5) Uani 1 1 d . . .
H18 H 0.4394 0.3222 0.8009 0.046 Uiso 1 1 calc R . .
C19 C 0.39135(14) 0.41549(14) 0.93141(12) 0.0418(5) Uani 1 1 d . . .
H19 H 0.3568 0.4436 0.9576 0.050 Uiso 1 1 calc R . .
C20 C 0.47291(13) 0.39849(13) 0.95460(12) 0.0388(5) Uani 1 1 d . . .
H20 H 0.5046 0.4130 1.0006 0.047 Uiso 1 1 calc R . .
C21 C 0.28591(13) 0.38536(17) 0.81450(13) 0.0504(6) Uani 1 1 d . . .
H21A H 0.2885 0.3621 0.7665 0.060 Uiso 1 1 calc R . .
H21B H 0.2678 0.4429 0.8072 0.060 Uiso 1 1 calc R . .
C22 C 0.22255(13) 0.33721(14) 0.84718(12) 0.0390(5) Uani 1 1 d . . .
C23 C 0.24258(15) 0.26203(14) 0.88328(12) 0.0447(5) Uani 1 1 d . . .
H23 H 0.2959 0.2398 0.8873 0.054 Uiso 1 1 calc R . .
C24 C 0.18370(16) 0.22006(15) 0.91331(14) 0.0513(6) Uani 1 1 d . . .
H24 H 0.1976 0.1699 0.9381 0.062 Uiso 1 1 calc R . .
C25 C 0.14286(13) 0.36897(15) 0.84159(12) 0.0448(5) Uani 1 1 d . . .
H25 H 0.1292 0.4196 0.8176 0.054 Uiso 1 1 calc R . .
C26 C 0.67460(12) 0.19987(12) 0.82170(11) 0.0302(4) Uani 1 1 d . . .
H1W H 0.7021(11) 0.4111(7) 1.0086(4) 0.080 Uiso 1 1 d D . .
H2W H 0.7069(11) 0.3358(4) 1.0453(5) 0.080 Uiso 1 1 d D . .
Mn1 Mn 0.628962(17) 0.306734(18) 0.912974(16) 0.02946(11) Uani 1 1 d D . .
N1 N 0.50263(10) 0.35652(11) 0.90025(10) 0.0372(4) Uani 1 1 d . . .
N2 N 0.36926(10) 0.38318(11) 0.86172(10) 0.0384(4) Uani 1 1 d . . .
N3 N 0.53120(12) 0.14411(13) 1.06430(12) 0.0520(5) Uani 1 1 d . . .
N4 N 0.59119(12) 0.19841(11) 0.97886(11) 0.0447(5) Uani 1 1 d . . .
O1 O 0.82325(9) -0.09157(9) 0.64207(7) 0.0378(3) Uani 1 1 d . . .
O2 O 0.76659(12) -0.00636(10) 0.54985(8) 0.0583(5) Uani 1 1 d . . .
O3 O 0.72666(8) 0.22604(8) 0.87772(7) 0.0332(3) Uani 1 1 d . . .
O4 O 0.60046(8) 0.22501(10) 0.80806(8) 0.0418(4) Uani 1 1 d . . .
O1W O 0.67787(9) 0.36858(9) 1.01709(8) 0.0410(4) Uani 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C2 C3 1.380(3) . ?
C2 C7 1.387(3) . ?
C2 C26 1.497(3) . ?
C3 C4 1.393(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.407(3) . ?
C4 C11 1.485(3) . ?
C5 C6 1.383(3) . ?
C5 C8 1.514(3) . ?
C6 C7 1.385(3) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 O2 1.250(2) . ?
C8 O1 1.250(2) . ?
C9 C10 1.376(3) 2_756 ?
C9 C11 1.396(3) . ?
C9 H9 0.9300 . ?
C10 C9 1.376(3) 2_756 ?
C10 C11 1.397(3) . ?
C10 H10 0.9300 . ?
C12 C13 1.345(4) . ?
C12 N4 1.364(3) . ?
C12 H12 0.9300 . ?
C13 N3 1.347(4) . ?
C13 H13 0.9300 . ?
C14 N4 1.302(3) . ?
C14 N3 1.336(3) . ?
C14 H14 0.9300 . ?
C15 N3 1.466(3) . ?
C15 C16 1.512(3) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.383(3) . ?
C16 C25 1.385(3) 7_557 ?
C17 C24 1.374(4) 7_557 ?
C17 H17 0.9300 . ?
C18 N1 1.312(3) . ?
C18 N2 1.337(3) . ?
C18 H18 0.9300 . ?
C19 C20 1.342(3) . ?
C19 N2 1.365(3) . ?
C19 H19 0.9300 . ?
C20 N1 1.375(3) . ?
C20 H20 0.9300 . ?
C21 N2 1.461(3) . ?
C21 C22 1.511(3) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C25 1.382(3) . ?
C22 C23 1.385(3) . ?
C23 C24 1.379(3) . ?
C23 H23 0.9300 . ?
C24 C17 1.374(4) 7_557 ?
C24 H24 0.9300 . ?
C25 C16 1.385(3) 7_557 ?
C25 H25 0.9300 . ?
C26 O4 1.253(2) . ?
C26 O3 1.269(2) . ?
C26 Mn1 2.615(2) . ?
Mn1 O1 2.1503(14) 4_656 ?
Mn1 O1W 2.1655(15) . ?
Mn1 N1 2.1808(17) . ?
Mn1 O3 2.2508(13) . ?
Mn1 N4 2.2765(19) . ?
Mn1 O4 2.3056(15) . ?
O1 Mn1 2.1503(14) 4_646 ?
O1W H1W 0.8202(11) . ?
O1W H2W 0.8199(10) . ?

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
C3 C2 C7 119.22(18) . . ?
C3 C2 C26 120.11(17) . . ?
C7 C2 C26 120.64(17) . . ?
C2 C3 C4 122.60(17) . . ?
C2 C3 H3 118.7 . . ?
C4 C3 H3 118.7 . . ?
C3 C4 C5 117.61(17) . . ?
C3 C4 C11 118.22(16) . . ?
C5 C4 C11 124.14(16) . . ?
C6 C5 C4 119.59(17) . . ?
C6 C5 C8 117.19(16) . . ?
C4 C5 C8 123.20(17) . . ?
C5 C6 C7 121.81(18) . . ?
C5 C6 H6 119.1 . . ?
C7 C6 H6 119.1 . . ?
C6 C7 C2 119.15(18) . . ?
C6 C7 H7 120.4 . . ?
C2 C7 H7 120.4 . . ?
O2 C8 O1 126.42(19) . . ?
O2 C8 C5 116.61(17) . . ?
O1 C8 C5 116.96(17) . . ?
C10 C9 C11 121.04(17) 2_756 . ?
C10 C9 H9 119.5 2_756 . ?
C11 C9 H9 119.5 . . ?
C9 C10 C11 121.91(18) 2_756 . ?
C9 C10 H10 119.0 2_756 . ?
C11 C10 H10 119.0 . . ?
C9 C11 C10 117.00(17) . . ?
C9 C11 C4 122.81(16) . . ?
C10 C11 C4 120.03(17) . . ?
C13 C12 N4 110.3(3) . . ?
C13 C12 H12 124.8 . . ?
N4 C12 H12 124.8 . . ?
C12 C13 N3 106.3(2) . . ?
C12 C13 H13 126.8 . . ?
N3 C13 H13 126.8 . . ?
N4 C14 N3 112.8(2) . . ?
N4 C14 H14 123.6 . . ?
N3 C14 H14 123.6 . . ?
N3 C15 C16 111.0(2) . . ?
N3 C15 H15A 109.4 . . ?
C16 C15 H15A 109.4 . . ?
N3 C15 H15B 109.4 . . ?
C16 C15 H15B 109.4 . . ?
H15A C15 H15B 108.0 . . ?
C17 C16 C25 118.4(2) . 7_557 ?
C17 C16 C15 121.1(2) . . ?
C25 C16 C15 120.5(2) 7_557 . ?
C24 C17 C16 120.9(2) 7_557 . ?
C24 C17 H17 119.6 7_557 . ?
C16 C17 H17 119.6 . . ?
N1 C18 N2 111.70(19) . . ?
N1 C18 H18 124.2 . . ?
N2 C18 H18 124.2 . . ?
C20 C19 N2 106.20(18) . . ?
C20 C19 H19 126.9 . . ?
N2 C19 H19 126.9 . . ?
C19 C20 N1 109.96(19) . . ?
C19 C20 H20 125.0 . . ?
N1 C20 H20 125.0 . . ?
N2 C21 C22 112.39(18) . . ?
N2 C21 H21A 109.1 . . ?
C22 C21 H21A 109.1 . . ?
N2 C21 H21B 109.1 . . ?
C22 C21 H21B 109.1 . . ?
H21A C21 H21B 107.9 . . ?
C25 C22 C23 119.0(2) . . ?
C25 C22 C21 119.5(2) . . ?
C23 C22 C21 121.5(2) . . ?
C24 C23 C22 120.2(2) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C17 C24 C23 120.1(2) 7_557 . ?
C17 C24 H24 119.9 7_557 . ?
C23 C24 H24 119.9 . . ?
C22 C25 C16 121.4(2) . 7_557 ?
C22 C25 H25 119.3 . . ?
C16 C25 H25 119.3 7_557 . ?
O4 C26 O3 121.20(18) . . ?
O4 C26 C2 120.06(17) . . ?
O3 C26 C2 118.71(17) . . ?
O4 C26 Mn1 61.84(10) . . ?
O3 C26 Mn1 59.36(10) . . ?
C2 C26 Mn1 177.84(14) . . ?
O1 Mn1 O1W 88.10(5) 4_656 . ?
O1 Mn1 N1 95.58(6) 4_656 . ?
O1W Mn1 N1 95.67(6) . . ?
O1 Mn1 O3 87.35(5) 4_656 . ?
O1W Mn1 O3 111.34(5) . . ?
N1 Mn1 O3 152.93(6) . . ?
O1 Mn1 N4 174.27(6) 4_656 . ?
O1W Mn1 N4 88.15(6) . . ?
N1 Mn1 N4 89.10(7) . . ?
O3 Mn1 N4 89.98(6) . . ?
O1 Mn1 O4 93.81(6) 4_656 . ?
O1W Mn1 O4 168.65(5) . . ?
N1 Mn1 O4 95.28(6) . . ?
O3 Mn1 O4 57.65(5) . . ?
N4 Mn1 O4 89.04(6) . . ?
O1 Mn1 C26 90.90(6) 4_656 . ?
O1W Mn1 C26 140.29(6) . . ?
N1 Mn1 C26 123.90(6) . . ?
O3 Mn1 C26 29.03(5) . . ?
N4 Mn1 C26 89.22(7) . . ?
O4 Mn1 C26 28.62(5) . . ?
C18 N1 C20 105.03(18) . . ?
C18 N1 Mn1 130.21(14) . . ?
C20 N1 Mn1 124.54(14) . . ?
C18 N2 C19 107.12(17) . . ?
C18 N2 C21 126.8(2) . . ?
C19 N2 C21 126.09(19) . . ?
C14 N3 C13 106.4(2) . . ?
C14 N3 C15 127.1(2) . . ?
C13 N3 C15 125.4(2) . . ?
C14 N4 C12 104.1(2) . . ?
C14 N4 Mn1 128.43(16) . . ?
C12 N4 Mn1 120.49(18) . . ?
C8 O1 Mn1 130.63(13) . 4_646 ?
C26 O3 Mn1 91.61(11) . . ?
C26 O4 Mn1 89.53(12) . . ?
Mn1 O1W H1W 108.5(5) . . ?
Mn1 O1W H2W 109.3(5) . . ?
H1W O1W H2W 114.6(2) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.190
_refine_diff_density_rms         0.047
_database_code_depnum_ccdc_archive 'CCDC 973828'

data_z

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H23 N4 Ni O4, 0.5(H O0.50)'
_chemical_formula_sum            'C27 H23.50 N4 Ni O4.25'
_chemical_formula_weight         530.69

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c
_symmetry_space_group_name_Hall  '-C 2yc'

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

_cell_length_a                   16.388(7)
_cell_length_b                   16.225(7)
_cell_length_c                   19.438(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.373(7)
_cell_angle_gamma                90.00
_cell_volume                     5146(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4354
_cell_measurement_theta_min      2.51
_cell_measurement_theta_max      27.47

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2204
_exptl_absorpt_coefficient_mu    0.795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6968
_exptl_absorpt_correction_T_max  0.8509
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12819
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_av_sigmaI/netI    0.0313
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.77
_diffrn_reflns_theta_max         25.05
_reflns_number_total             4554
_reflns_number_gt                3803
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0780P)²+6.7763P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4554
_refine_ls_number_parameters     329
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0385
_refine_ls_wR_factor_ref         0.1248
_refine_ls_wR_factor_gt          0.1164
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.001
_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
C1 C 0.26483(16) 0.44261(17) 0.43477(13) 0.0281(6) Uani 1 1 d . . .
C2 C 0.26720(16) 0.47359(17) 0.50804(13) 0.0292(6) Uani 1 1 d . . .
C3 C 0.19261(18) 0.4750(2) 0.53554(15) 0.0426(8) Uani 1 1 d . . .
H3 H 0.1456 0.4595 0.5080 0.051 Uiso 1 1 calc R . .
C4 C 0.18597(18) 0.4987(2) 0.60322(15) 0.0413(7) Uani 1 1 d . . .
H4 H 0.1354 0.4977 0.6213 0.050 Uiso 1 1 calc R . .
C5 C 0.25501(17) 0.52395(18) 0.64355(14) 0.0310(6) Uani 1 1 d . . .
C6 C 0.33002(17) 0.52352(18) 0.61674(13) 0.0302(6) Uani 1 1 d . . .
H6 H 0.3763 0.5407 0.6444 0.036 Uiso 1 1 calc R . .
C7 C 0.33847(15) 0.49781(16) 0.54875(13) 0.0262(6) Uani 1 1 d . . .
C8 C 0.42071(16) 0.49840(16) 0.52289(13) 0.0265(6) Uani 1 1 d . . .
C9 C 0.48995(17) 0.48016(18) 0.56734(14) 0.0326(6) Uani 1 1 d . . .
H9 H 0.4838 0.4666 0.6130 0.039 Uiso 1 1 calc R . .
C10 C 0.56738(17) 0.48177(18) 0.54514(14) 0.0324(6) Uani 1 1 d . . .
H10 H 0.6124 0.4694 0.5761 0.039 Uiso 1 1 calc R . .
C11 C 0.24845(17) 0.55568(18) 0.71558(14) 0.0315(6) Uani 1 1 d . . .
C12 C 0.04448(19) 0.38605(19) 0.33385(17) 0.0403(7) Uani 1 1 d . . .
H12 H 0.0419 0.4300 0.3030 0.048 Uiso 1 1 calc R . .
C13 C -0.0196(2) 0.3526(2) 0.3602(2) 0.0522(9) Uani 1 1 d . . .
H13 H -0.0742 0.3676 0.3508 0.063 Uiso 1 1 calc R . .
C14 C 0.09318(19) 0.28926(19) 0.40140(15) 0.0384(7) Uani 1 1 d . . .
C15 C 0.1488(3) 0.2301(3) 0.4390(2) 0.0758(13) Uani 1 1 d . . .
H15A H 0.1373 0.1756 0.4216 0.114 Uiso 1 1 calc R . .
H15B H 0.1409 0.2319 0.4873 0.114 Uiso 1 1 calc R . .
H15C H 0.2045 0.2443 0.4328 0.114 Uiso 1 1 calc R . .
C16 C -0.0384(3) 0.2407(2) 0.4451(2) 0.0659(11) Uani 1 1 d . . .
H16A H -0.0096 0.1892 0.4554 0.079 Uiso 1 1 calc R . .
H16B H -0.0892 0.2276 0.4177 0.079 Uiso 1 1 calc R . .
C17 C -0.0588(2) 0.2788(2) 0.51220(18) 0.0484(8) Uani 1 1 d . . .
C18 C -0.1060(3) 0.2348(2) 0.5538(2) 0.0776(14) Uani 1 1 d . . .
H18 H -0.1236 0.1823 0.5403 0.093 Uiso 1 1 calc R . .
C19 C -0.0331(2) 0.3554(2) 0.5353(2) 0.0628(11) Uani 1 1 d . . .
H19 H -0.0002 0.3867 0.5088 0.075 Uiso 1 1 calc R . .
C20 C 0.1904(2) 0.2150(2) 0.24781(18) 0.0480(8) Uani 1 1 d . . .
H20 H 0.1340 0.2228 0.2447 0.058 Uiso 1 1 calc R . .
C21 C 0.2286(2) 0.1542(2) 0.21704(18) 0.0513(9) Uani 1 1 d . . .
H21 H 0.2041 0.1132 0.1887 0.062 Uiso 1 1 calc R . .
C22 C 0.31951(19) 0.23221(19) 0.27675(15) 0.0379(7) Uani 1 1 d . . .
C23 C 0.3990(2) 0.2639(3) 0.3078(2) 0.0663(11) Uani 1 1 d . . .
H23A H 0.3900 0.3111 0.3358 0.099 Uiso 1 1 calc R . .
H23B H 0.4323 0.2793 0.2718 0.099 Uiso 1 1 calc R . .
H23C H 0.4264 0.2218 0.3360 0.099 Uiso 1 1 calc R . .
C24 C 0.3754(2) 0.11945(19) 0.20561(18) 0.0477(8) Uani 1 1 d . . .
H24A H 0.3581 0.0629 0.1974 0.057 Uiso 1 1 calc R . .
H24B H 0.4238 0.1187 0.2384 0.057 Uiso 1 1 calc R . .
C25 C 0.3977(2) 0.15702(19) 0.13777(17) 0.0414(7) Uani 1 1 d . . .
C26 C 0.3718(3) 0.2333(2) 0.1156(2) 0.0720(13) Uani 1 1 d . . .
H26 H 0.3388 0.2642 0.1422 0.086 Uiso 1 1 calc R . .
C27 C 0.4449(2) 0.1133(2) 0.0967(2) 0.0567(10) Uani 1 1 d . . .
H27 H 0.4628 0.0610 0.1106 0.068 Uiso 1 1 calc R . .
N1 N 0.24751(15) 0.26451(15) 0.28502(12) 0.0359(6) Uani 1 1 d . . .
N2 N 0.31066(16) 0.16437(15) 0.23543(13) 0.0401(6) Uani 1 1 d . . .
N3 N 0.11570(14) 0.34613(15) 0.35886(11) 0.0316(5) Uani 1 1 d . . .
N4 N 0.01089(16) 0.29109(17) 0.40403(14) 0.0452(7) Uani 1 1 d . . .
Ni1 Ni 0.22598(2) 0.37663(2) 0.325280(16) 0.02651(14) Uani 1 1 d . . .
O1 O 0.22804(12) 0.48457(12) 0.38779(9) 0.0354(5) Uani 1 1 d . . .
O2 O 0.29227(13) 0.37221(12) 0.42328(10) 0.0347(5) Uani 1 1 d . . .
O3 O 0.31088(12) 0.56840(13) 0.75575(10) 0.0384(5) Uani 1 1 d . . .
O4 O 0.17794(12) 0.57152(13) 0.73311(9) 0.0362(5) Uani 1 1 d . . .
O1W O 0.5000 0.5099(9) 0.7500 0.140(4) Uiso 0.50 2 d SPD . .
H1W H 0.4628 0.5401 0.7645 0.167 Uiso 0.50 1 d PRD . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.248(3) . ?
C1 O2 1.255(3) . ?
C1 C2 1.507(4) . ?
C1 Ni1 2.414(3) . ?
C2 C3 1.380(4) . ?
C2 C7 1.404(4) . ?
C3 C4 1.385(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.377(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.379(4) . ?
C5 C11 1.505(4) . ?
C6 C7 1.405(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.482(4) . ?
C8 C9 1.392(4) . ?
C8 C10 1.392(4) 5_666 ?
C9 C10 1.378(4) . ?
C9 H9 0.9300 . ?
C10 C8 1.392(4) 5_666 ?
C10 H10 0.9300 . ?
C11 O3 1.245(3) . ?
C11 O4 1.261(3) . ?
C11 Ni1 2.457(3) 6_566 ?
C12 C13 1.326(5) . ?
C12 N3 1.383(4) . ?
C12 H12 0.9300 . ?
C13 N4 1.375(4) . ?
C13 H13 0.9300 . ?
C14 N3 1.315(4) . ?
C14 N4 1.355(4) . ?
C14 C15 1.470(5) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 N4 1.442(4) . ?
C16 C17 1.508(5) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.371(5) . ?
C17 C19 1.375(5) . ?
C18 C26 1.386(5) 8_456 ?
C18 H18 0.9300 . ?
C19 C27 1.377(5) 8_456 ?
C19 H19 0.9300 . ?
C20 C21 1.338(5) . ?
C20 N1 1.385(4) . ?
C20 H20 0.9300 . ?
C21 N2 1.369(4) . ?
C21 H21 0.9300 . ?
C22 N1 1.315(4) . ?
C22 N2 1.362(4) . ?
C22 C23 1.476(5) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 N2 1.452(4) . ?
C24 C25 1.527(5) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 C27 1.362(4) . ?
C25 C26 1.365(5) . ?
C26 C18 1.386(5) 8 ?
C26 H26 0.9300 . ?
C27 C19 1.377(5) 8 ?
C27 H27 0.9300 . ?
N1 Ni1 2.024(2) . ?
N3 Ni1 2.039(2) . ?
Ni1 O4 2.067(2) 6_565 ?
Ni1 O2 2.104(2) . ?
Ni1 O1 2.130(2) . ?
Ni1 O3 2.216(2) 6_565 ?
Ni1 C11 2.457(3) 6_565 ?
O3 Ni1 2.216(2) 6_566 ?
O4 Ni1 2.067(2) 6_566 ?
O1W H1W 0.8503 . ?

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 C1 O2 121.5(2) . . ?
O1 C1 C2 118.5(2) . . ?
O2 C1 C2 119.6(2) . . ?
O1 C1 Ni1 61.80(14) . . ?
O2 C1 Ni1 60.59(14) . . ?
C2 C1 Ni1 164.21(19) . . ?
C3 C2 C7 119.8(2) . . ?
C3 C2 C1 115.2(2) . . ?
C7 C2 C1 124.9(2) . . ?
C2 C3 C4 121.6(3) . . ?
C2 C3 H3 119.2 . . ?
C4 C3 H3 119.2 . . ?
C5 C4 C3 119.3(3) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C4 C5 C6 119.8(2) . . ?
C4 C5 C11 120.3(2) . . ?
C6 C5 C11 119.8(2) . . ?
C5 C6 C7 121.8(2) . . ?
C5 C6 H6 119.1 . . ?
C7 C6 H6 119.1 . . ?
C6 C7 C2 117.6(2) . . ?
C6 C7 C8 119.3(2) . . ?
C2 C7 C8 123.1(2) . . ?
C9 C8 C10 117.4(2) . 5_666 ?
C9 C8 C7 120.2(2) . . ?
C10 C8 C7 122.4(2) 5_666 . ?
C10 C9 C8 121.5(3) . . ?
C10 C9 H9 119.2 . . ?
C8 C9 H9 119.2 . . ?
C9 C10 C8 121.1(3) . 5_666 ?
C9 C10 H10 119.4 . . ?
C8 C10 H10 119.4 5_666 . ?
O3 C11 O4 121.1(2) . . ?
O3 C11 C5 120.9(2) . . ?
O4 C11 C5 117.9(2) . . ?
O3 C11 Ni1 64.07(14) . 6_566 ?
O4 C11 Ni1 57.24(13) . 6_566 ?
C5 C11 Ni1 171.9(2) . 6_566 ?
C13 C12 N3 110.2(3) . . ?
C13 C12 H12 124.9 . . ?
N3 C12 H12 124.9 . . ?
C12 C13 N4 106.4(3) . . ?
C12 C13 H13 126.8 . . ?
N4 C13 H13 126.8 . . ?
N3 C14 N4 110.3(3) . . ?
N3 C14 C15 125.0(3) . . ?
N4 C14 C15 124.6(3) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N4 C16 C17 115.3(3) . . ?
N4 C16 H16A 108.4 . . ?
C17 C16 H16A 108.4 . . ?
N4 C16 H16B 108.4 . . ?
C17 C16 H16B 108.4 . . ?
H16A C16 H16B 107.5 . . ?
C18 C17 C19 116.7(3) . . ?
C18 C17 C16 118.7(3) . . ?
C19 C17 C16 124.5(3) . . ?
C17 C18 C26 121.7(3) . 8_456 ?
C17 C18 H18 119.1 . . ?
C26 C18 H18 119.1 8_456 . ?
C17 C19 C27 121.3(3) . 8_456 ?
C17 C19 H19 119.3 . . ?
C27 C19 H19 119.3 8_456 . ?
C21 C20 N1 109.9(3) . . ?
C21 C20 H20 125.1 . . ?
N1 C20 H20 125.1 . . ?
C20 C21 N2 106.5(3) . . ?
C20 C21 H21 126.8 . . ?
N2 C21 H21 126.8 . . ?
N1 C22 N2 110.3(3) . . ?
N1 C22 C23 125.4(3) . . ?
N2 C22 C23 124.3(3) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N2 C24 C25 112.7(3) . . ?
N2 C24 H24A 109.0 . . ?
C25 C24 H24A 109.0 . . ?
N2 C24 H24B 109.0 . . ?
C25 C24 H24B 109.0 . . ?
H24A C24 H24B 107.8 . . ?
C27 C25 C26 117.6(3) . . ?
C27 C25 C24 119.5(3) . . ?
C26 C25 C24 122.9(3) . . ?
C25 C26 C18 120.9(3) . 8 ?
C25 C26 H26 119.6 . . ?
C18 C26 H26 119.6 8 . ?
C25 C27 C19 121.7(3) . 8 ?
C25 C27 H27 119.2 . . ?
C19 C27 H27 119.1 8 . ?
C22 N1 C20 106.0(3) . . ?
C22 N1 Ni1 126.6(2) . . ?
C20 N1 Ni1 126.1(2) . . ?
C22 N2 C21 107.4(3) . . ?
C22 N2 C24 126.8(3) . . ?
C21 N2 C24 124.9(3) . . ?
C14 N3 C12 105.8(2) . . ?
C14 N3 Ni1 132.9(2) . . ?
C12 N3 Ni1 121.20(19) . . ?
C14 N4 C13 107.3(3) . . ?
C14 N4 C16 128.3(3) . . ?
C13 N4 C16 124.4(3) . . ?
N1 Ni1 N3 95.59(10) . . ?
N1 Ni1 O4 95.55(9) . 6_565 ?
N3 Ni1 O4 95.69(9) . 6_565 ?
N1 Ni1 O2 103.03(9) . . ?
N3 Ni1 O2 95.73(9) . . ?
O4 Ni1 O2 157.08(8) 6_565 . ?
N1 Ni1 O1 164.88(9) . . ?
N3 Ni1 O1 89.09(9) . . ?
O4 Ni1 O1 98.29(8) 6_565 . ?
O2 Ni1 O1 62.12(7) . . ?
N1 Ni1 O3 89.07(9) . 6_565 ?
N3 Ni1 O3 156.76(8) . 6_565 ?
O4 Ni1 O3 61.15(8) 6_565 6_565 ?
O2 Ni1 O3 105.39(8) . 6_565 ?
O1 Ni1 O3 92.27(8) . 6_565 ?
N1 Ni1 C1 134.29(10) . . ?
N3 Ni1 C1 89.65(9) . . ?
O4 Ni1 C1 129.14(9) 6_565 . ?
O2 Ni1 C1 31.31(8) . . ?
O1 Ni1 C1 31.09(8) . . ?
O3 Ni1 C1 103.32(9) 6_565 . ?
N1 Ni1 C11 91.17(10) . 6_565 ?
N3 Ni1 C11 126.56(9) . 6_565 ?
O4 Ni1 C11 30.87(9) 6_565 6_565 ?
O2 Ni1 C11 133.98(9) . 6_565 ?
O1 Ni1 C11 97.58(9) . 6_565 ?
O3 Ni1 C11 30.34(8) 6_565 6_565 ?
C1 Ni1 C11 121.22(10) . 6_565 ?
C1 O1 Ni1 87.11(16) . . ?
C1 O2 Ni1 88.10(16) . . ?
C11 O3 Ni1 85.59(16) . 6_566 ?
C11 O4 Ni1 91.89(16) . 6_566 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.05
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.818
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.069
_database_code_depnum_ccdc_archive 'CCDC 973829'

data_z

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C47 H37 N8 Ni O6'
_chemical_formula_weight         868.56

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

_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                   11.9535(5)
_cell_length_b                   12.9115(6)
_cell_length_c                   13.8933(6)
_cell_angle_alpha                83.9270(10)
_cell_angle_beta                 80.9780(10)
_cell_angle_gamma                86.0030(10)
_cell_volume                     2102.76(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4070
_cell_measurement_theta_min      2.49
_cell_measurement_theta_max      26.65

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             902
_exptl_absorpt_coefficient_mu    0.522
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8344
_exptl_absorpt_correction_T_max  0.9448
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11185
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.28
_diffrn_reflns_theta_max         25.25
_reflns_number_total             7575
_reflns_number_gt                6208
_reflns_threshold_expression     >2sigma(I)

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

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

1. Fixed Uiso
  At 1.2 times of:
  All C(H) groups, All O(H,H) groups
2. Restrained distances
 C24-C25 = C25-C26 = C26-C27 = C27-C28 = C28-C29 = C29-C24
 1.41 with sigma of 0.01
 C24-C25' = C25'-C26' = C26'-C27' = C27'-C28' = C28'-C29' = C29'-C24
 1.41 with sigma of 0.01
 C24-C26 = C25-C27 = C26-C28 = C27-C29 = C28-C24 = C29-C25
 2.45 with sigma of 0.02
 C24-C26' = C25'-C27' = C26'-C28' = C27'-C29' = C28'-C24 = C29'-C25'
 2.45 with sigma of 0.02
 H1WA-H1WB = H2WA-H2WB = H3WA-H3WB
 1.34 with sigma of 0.001
 H1WA-O1W = H1WB-O1W = H2WA-O2W = H2WB-O2W = H3WA-O3W = H3WB-O3W
 0.83 with sigma of 0.001
3. Restrained planarity
 C24, C25, C26, C27, C28, C29, C24_$1, C25_$1, C26_$1, C27_$1, C28_$1, C29_$1
 with sigma of 0.01
 C24, C25', C26', C27', C28', C29', C24_$1, C25'_$1, C26'_$1, C27'_$1, C28'_$1
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
O4 ∼ C8: within 1.3A with sigma of 0.01 and sigma for terminal atoms of 0.02
O3 ∼ C8: within 1.3A with sigma of 0.001 and sigma for terminal atoms of
0.002
Uanis(O3W) ∼ Ueq, Uanis(C25) ∼ Ueq, Uanis(C26) ∼ Ueq, Uanis(C27)
∼ Ueq, Uanis(C28) ∼ Ueq, Uanis(C29) ∼ Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.005
Uanis(C25) = Uanis(C25')
Uanis(C26) = Uanis(C26')
Uanis(C27) = Uanis(C27')
Uanis(C28) = Uanis(C28')
Uanis(C29) = Uanis(C29') 

;

_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)+(0.0920P)²+5.9400P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7575
_refine_ls_number_parameters     584
_refine_ls_number_restraints     98
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0639
_refine_ls_wR_factor_ref         0.1801
_refine_ls_wR_factor_gt          0.1673
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.004
_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 0.33041(15) 0.25970(15) 0.42696(14) 0.0208(7) Uani 1 1 d . . .
C1 C 0.0770(13) 0.2990(12) 0.4117(11) 0.023(3) Uani 1 1 d . . .
C2 C -0.0378(12) 0.3006(12) 0.4759(11) 0.023(3) Uani 1 1 d . . .
C3 C -0.0918(14) 0.3986(12) 0.4879(13) 0.029(4) Uani 1 1 d . . .
H3 H -0.0636 0.4565 0.4483 0.035 Uiso 1 1 calc R . .
C4 C -0.1867(14) 0.4113(13) 0.5576(13) 0.033(4) Uani 1 1 d . . .
H4 H -0.2198 0.4777 0.5663 0.040 Uiso 1 1 calc R . .
C5 C -0.2325(14) 0.3257(13) 0.6142(13) 0.032(4) Uani 1 1 d . . .
C6 C -0.1820(14) 0.2271(13) 0.5986(13) 0.032(4) Uani 1 1 d . . .
H6 H -0.2146 0.1691 0.6348 0.038 Uiso 1 1 calc R . .
C7 C -0.0847(13) 0.2119(12) 0.5312(12) 0.024(3) Uani 1 1 d . . .
C8 C -0.337(2) 0.3374(16) 0.690(2) 0.083(7) Uani 1 1 d U . .
C9 C -0.0389(13) 0.1037(12) 0.5151(12) 0.024(3) Uani 1 1 d . . .
C10 C -0.0030(13) 0.0743(12) 0.4213(12) 0.026(3) Uani 1 1 d . . .
H10 H -0.0050 0.1236 0.3676 0.031 Uiso 1 1 calc R . .
C11 C 0.0355(13) -0.0273(12) 0.4066(12) 0.027(3) Uani 1 1 d . . .
H11 H 0.0595 -0.0449 0.3431 0.032 Uiso 1 1 calc R . .
C12 C 0.3739(14) 0.1432(13) 0.6252(12) 0.028(3) Uani 1 1 d . . .
H12 H 0.4284 0.1886 0.6325 0.034 Uiso 1 1 calc R . .
C13 C 0.2537(18) 0.0210(17) 0.6572(15) 0.050(5) Uani 1 1 d . . .
H13 H 0.2101 -0.0330 0.6886 0.060 Uiso 1 1 calc R . .
C14 C 0.2549(16) 0.0639(15) 0.5641(14) 0.038(4) Uani 1 1 d . . .
H14 H 0.2107 0.0445 0.5203 0.046 Uiso 1 1 calc R . .
C15 C 0.3658(15) 0.0519(16) 0.7901(13) 0.039(4) Uani 1 1 d . . .
C16 C 0.378(2) -0.048(2) 0.8309(18) 0.072(8) Uani 1 1 d . . .
H16 H 0.3523 -0.1025 0.8032 0.086 Uiso 1 1 calc R . .
C17 C 0.430(3) -0.068(2) 0.915(2) 0.085(10) Uani 1 1 d . . .
H17 H 0.4380 -0.1359 0.9423 0.101 Uiso 1 1 calc R . .
C18 C 0.4690(17) 0.0112(18) 0.9571(13) 0.047(5) Uani 1 1 d . . .
C19 C 0.451(2) 0.1118(19) 0.9166(16) 0.058(6) Uani 1 1 d . . .
H19 H 0.4737 0.1669 0.9458 0.070 Uiso 1 1 calc R . .
C20 C 0.400(2) 0.1329(19) 0.8334(16) 0.056(6) Uani 1 1 d . . .
H20 H 0.3886 0.2013 0.8069 0.067 Uiso 1 1 calc R . .
C21 C 0.2678(15) 0.1534(13) 0.2629(13) 0.032(4) Uani 1 1 d . . .
H21 H 0.2250 0.2133 0.2451 0.038 Uiso 1 1 calc R . .
C22 C 0.3814(14) 0.0467(13) 0.3322(13) 0.033(4) Uani 1 1 d . . .
H22 H 0.4330 0.0192 0.3730 0.040 Uiso 1 1 calc R . .
C23 C 0.3413(15) -0.0061(14) 0.2682(13) 0.035(4) Uani 1 1 d . . .
H23 H 0.3595 -0.0752 0.2562 0.042 Uiso 1 1 calc R . .
C24 C 0.1966(16) 0.0412(12) 0.1566(12) 0.041(5) Uani 1 1 d D . .
C25 C 0.205(3) -0.043(3) 0.107(3) 0.036(7) Uani 0.45(3) 1 d PDU A 1
H25 H 0.2644 -0.0930 0.1130 0.044 Uiso 0.45(3) 1 calc PR A 1
C26 C 0.127(3) -0.058(3) 0.046(3) 0.039(7) Uani 0.45(3) 1 d PDU A 1
H26 H 0.1362 -0.1178 0.0122 0.047 Uiso 0.45(3) 1 calc PR A 1
C27 C 0.037(3) 0.012(3) 0.032(3) 0.058(6) Uani 0.45(3) 1 d PDU . 1
C28 C 0.022(4) 0.103(4) 0.085(3) 0.080(12) Uani 0.45(3) 1 d PDU A 1
H28 H -0.0389 0.1511 0.0780 0.096 Uiso 0.45(3) 1 calc PR A 1
C29 C 0.101(3) 0.117(3) 0.146(3) 0.066(10) Uani 0.45(3) 1 d PDU A 1
H29 H 0.0930 0.1752 0.1810 0.079 Uiso 0.45(3) 1 calc PR A 1
C25' C 0.168(3) -0.059(2) 0.149(2) 0.036(7) Uani 0.55(3) 1 d PD A 2
H25' H 0.2002 -0.1150 0.1848 0.044 Uiso 0.55(3) 1 calc PR A 2
C26' C 0.091(3) -0.077(3) 0.088(2) 0.039(7) Uani 0.55(3) 1 d PD A 2
H26' H 0.0716 -0.1442 0.0828 0.047 Uiso 0.55(3) 1 calc PR A 2
C27' C 0.042(3) 0.006(3) 0.034(2) 0.058(6) Uani 0.55(3) 1 d PD . 2
C28' C 0.074(3) 0.108(3) 0.042(3) 0.080(12) Uani 0.55(3) 1 d PD A 2
H28' H 0.0416 0.1638 0.0063 0.096 Uiso 0.55(3) 1 calc PR A 2
C29' C 0.154(3) 0.127(3) 0.101(3) 0.066(10) Uani 0.55(3) 1 d PD A 2
H29' H 0.1769 0.1934 0.1040 0.079 Uiso 0.55(3) 1 calc PR A 2
C30 C 0.5922(15) 0.2517(19) 0.4455(14) 0.047(5) Uani 1 1 d . . .
H30 H 0.5840 0.2294 0.5120 0.056 Uiso 1 1 calc R . .
C31 C 0.6917(16) 0.2663(19) 0.3879(14) 0.048(5) Uani 1 1 d . . .
H31 H 0.7633 0.2571 0.4066 0.058 Uiso 1 1 calc R . .
C32 C 0.5529(13) 0.3015(14) 0.3039(12) 0.032(4) Uani 1 1 d . . .
H32 H 0.5130 0.3217 0.2520 0.039 Uiso 1 1 calc R . .
C33 C 0.7462(13) 0.3200(13) 0.2085(12) 0.029(4) Uani 1 1 d . . .
C34 C 0.8565(15) 0.3374(16) 0.2143(13) 0.040(4) Uani 1 1 d . . .
H34 H 0.8797 0.3364 0.2753 0.048 Uiso 1 1 calc R . .
C35 C 0.9334(15) 0.3566(17) 0.1305(14) 0.043(5) Uani 1 1 d . . .
H35 H 1.0074 0.3700 0.1360 0.052 Uiso 1 1 calc R . .
C36 C 0.9033(15) 0.3565(14) 0.0373(13) 0.033(4) Uani 1 1 d . . .
C37 C 0.7912(17) 0.3404(18) 0.0339(15) 0.048(5) Uani 1 1 d . . .
H37 H 0.7673 0.3422 -0.0268 0.058 Uiso 1 1 calc R . .
C38 C 0.7133(16) 0.3218(18) 0.1176(14) 0.047(5) Uani 1 1 d . . .
H38 H 0.6386 0.3106 0.1125 0.057 Uiso 1 1 calc R . .
C39 C 0.9882(15) 0.3716(14) -0.0528(13) 0.034(4) Uani 1 1 d . . .
C40 C 1.1032(16) 0.3715(17) -0.0491(14) 0.043(5) Uani 1 1 d . . .
H40 H 1.1277 0.3654 0.0117 0.052 Uiso 1 1 calc R . .
C41 C 1.1831(16) 0.3800(16) -0.1330(13) 0.041(4) Uani 1 1 d . . .
H41 H 1.2599 0.3788 -0.1283 0.049 Uiso 1 1 calc R . .
C42 C 1.1477(15) 0.3904(14) -0.2234(13) 0.035(4) Uani 1 1 d . . .
C43 C 1.0341(18) 0.396(2) -0.2299(15) 0.055(6) Uani 1 1 d . . .
H43 H 1.0100 0.4055 -0.2908 0.066 Uiso 1 1 calc R . .
C44 C 0.9553(17) 0.386(2) -0.1450(15) 0.055(6) Uani 1 1 d . . .
H44 H 0.8784 0.3894 -0.1501 0.066 Uiso 1 1 calc R . .
C45 C 1.2160(15) 0.3538(14) -0.3939(12) 0.032(4) Uani 1 1 d . . .
H45 H 1.1503 0.3240 -0.4029 0.038 Uiso 1 1 calc R . .
C46 C 1.3835(15) 0.4103(13) -0.4174(13) 0.034(4) Uani 1 1 d . . .
H46 H 1.4560 0.4270 -0.4475 0.041 Uiso 1 1 calc R . .
C47 C 1.3374(16) 0.4297(15) -0.3253(14) 0.039(4) Uani 1 1 d . . .
H47 H 1.3717 0.4607 -0.2808 0.047 Uiso 1 1 calc R . .
N1 N 0.3312(11) 0.1404(10) 0.5442(10) 0.027(3) Uani 1 1 d . . .
N2 N 0.3295(12) 0.0728(12) 0.6962(10) 0.034(3) Uani 1 1 d . . .
N3 N 0.3351(11) 0.1478(10) 0.3289(10) 0.027(3) Uani 1 1 d . . .
N4 N 0.2674(12) 0.0629(11) 0.2237(10) 0.032(3) Uani 1 1 d . A .
N5 N 0.5046(11) 0.2739(11) 0.3933(10) 0.028(3) Uani 1 1 d . . .
N6 N 0.6667(11) 0.2975(11) 0.2955(10) 0.030(3) Uani 1 1 d . . .
N7 N 1.2295(12) 0.3941(11) -0.3109(10) 0.032(3) Uani 1 1 d . . .
N8 N 1.3070(11) 0.3620(11) -0.4602(10) 0.029(3) Uani 1 1 d . . .
O1 O 0.1558(9) 0.2518(9) 0.4514(8) 0.027(2) Uani 1 1 d . . .
O2 O 0.0865(10) 0.3478(10) 0.3287(9) 0.037(3) Uani 1 1 d . . .
O3 O -0.3841(16) 0.2582(12) 0.7275(17) 0.093(6) Uani 1 1 d U . .
O4 O -0.3730(13) 0.4278(11) 0.7077(13) 0.063(5) Uani 1 1 d U . .
O1W O 0.3099(9) 0.3762(9) 0.3085(8) 0.030(3) Uani 1 1 d D . .
H1W H 0.2395 0.3781 0.3182 0.036 Uiso 1 1 d RD . .
H2W H 0.3296 0.4368 0.3073 0.036 Uiso 1 1 d RD . .
O2W O 0.429(4) 0.357(4) 0.086(3) 0.089(12) Uani 0.50 1 d PD . .
H3W H 0.3636 0.3503 0.0752 0.106 Uiso 0.50 1 d PRD . .
H4W H 0.4335 0.4233 0.0923 0.106 Uiso 0.50 1 d PRD . .
O3W O 0.523(3) 0.561(4) 0.120(3) 0.089(12) Uani 0.50 1 d PDU . .
H5W H 0.4685 0.5206 0.1265 0.106 Uiso 0.50 1 d PRD . .
H6W H 0.5135 0.6392 0.1148 0.106 Uiso 0.50 1 d PRD . .


_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 2.070(10) . ?
Ni1 N5 2.078(13) . ?
Ni1 N3 2.081(13) . ?
Ni1 N1 2.121(13) . ?
Ni1 N8 2.128(14) 1_456 ?
Ni1 O1W 2.141(11) . ?
C1 O2 1.248(19) . ?
C1 O1 1.254(18) . ?
C1 C2 1.52(2) . ?
C2 C3 1.39(2) . ?
C2 C7 1.41(2) . ?
C3 C4 1.38(2) . ?
C3 H3 0.9300 . ?
C4 C5 1.38(2) . ?
C4 H4 0.9300 . ?
C5 C6 1.39(2) . ?
C5 C8 1.51(3) . ?
C6 C7 1.39(2) . ?
C6 H6 0.9300 . ?
C7 C9 1.49(2) . ?
C8 O3 1.23(3) . ?
C8 O4 1.25(2) . ?
C9 C10 1.39(2) . ?
C9 C11 1.39(2) 2_556 ?
C10 C11 1.38(2) . ?
C10 H10 0.9300 . ?
C11 C9 1.39(2) 2_556 ?
C11 H11 0.9300 . ?
C12 N1 1.31(2) . ?
C12 N2 1.34(2) . ?
C12 H12 0.9300 . ?
C13 C14 1.35(3) . ?
C13 N2 1.37(2) . ?
C13 H13 0.9300 . ?
C14 N1 1.37(2) . ?
C14 H14 0.9300 . ?
C15 C16 1.36(3) . ?
C15 C20 1.37(3) . ?
C15 N2 1.43(2) . ?
C16 C17 1.39(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.37(3) . ?
C17 H17 0.9300 . ?
C18 C19 1.38(3) . ?
C18 C18 1.49(4) 2_657 ?
C19 C20 1.39(3) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 N3 1.30(2) . ?
C21 N4 1.34(2) . ?
C21 H21 0.9300 . ?
C22 C23 1.34(2) . ?
C22 N3 1.38(2) . ?
C22 H22 0.9300 . ?
C23 N4 1.38(2) . ?
C23 H23 0.9300 . ?
C24 C25 1.35(3) . ?
C24 C25' 1.38(3) . ?
C24 C29' 1.39(3) . ?
C24 N4 1.41(2) . ?
C24 C29 1.46(3) . ?
C25 C26 1.39(3) . ?
C25 H25 0.9300 . ?
C26 C27 1.39(4) . ?
C26 H26 0.9300 . ?
C27 C28 1.42(4) . ?
C27 C27 1.43(10) 2 ?
C28 C29 1.41(4) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C25' C26' 1.40(3) . ?
C25' H25' 0.9300 . ?
C26' C27' 1.38(3) . ?
C26' H26' 0.9300 . ?
C27' C28' 1.41(3) . ?
C27' C27' 1.51(9) 2 ?
C28' C29' 1.41(3) . ?
C28' H28' 0.9300 . ?
C29' H29' 0.9300 . ?
C30 C31 1.34(3) . ?
C30 N5 1.36(2) . ?
C30 H30 0.9300 . ?
C31 N6 1.38(2) . ?
C31 H31 0.9300 . ?
C32 N5 1.31(2) . ?
C32 N6 1.35(2) . ?
C32 H32 0.9300 . ?
C33 C34 1.37(2) . ?
C33 C38 1.38(3) . ?
C33 N6 1.43(2) . ?
C34 C35 1.38(2) . ?
C34 H34 0.9300 . ?
C35 C36 1.40(3) . ?
C35 H35 0.9300 . ?
C36 C37 1.38(3) . ?
C36 C39 1.49(2) . ?
C37 C38 1.38(3) . ?
C37 H37 0.9300 . ?
C38 H38 0.9300 . ?
C39 C40 1.38(3) . ?
C39 C44 1.39(3) . ?
C40 C41 1.39(2) . ?
C40 H40 0.9300 . ?
C41 C42 1.38(3) . ?
C41 H41 0.9300 . ?
C42 C43 1.37(3) . ?
C42 N7 1.43(2) . ?
C43 C44 1.39(3) . ?
C43 H43 0.9300 . ?
C44 H44 0.9300 . ?
C45 N8 1.31(2) . ?
C45 N7 1.35(2) . ?
C45 H45 0.9300 . ?
C46 C47 1.35(2) . ?
C46 N8 1.38(2) . ?
C46 H46 0.9300 . ?
C47 N7 1.38(2) . ?
C47 H47 0.9300 . ?
N8 Ni1 2.128(14) 1_654 ?
O1W H1W 0.8300 . ?
O1W H2W 0.8301 . ?
O2W H3W 0.8305 . ?
O2W H4W 0.8755 . ?
O3W H5W 0.8469 . ?
O3W H6W 1.0080 . ?

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 N5 176.0(5) . . ?
O1 Ni1 N3 87.5(5) . . ?
N5 Ni1 N3 91.6(5) . . ?
O1 Ni1 N1 86.0(5) . . ?
N5 Ni1 N1 98.0(5) . . ?
N3 Ni1 N1 90.2(5) . . ?
O1 Ni1 N8 86.2(5) . 1_456 ?
N5 Ni1 N8 95.0(5) . 1_456 ?
N3 Ni1 N8 171.9(5) . 1_456 ?
N1 Ni1 N8 84.3(5) . 1_456 ?
O1 Ni1 O1W 87.7(4) . . ?
N5 Ni1 O1W 88.4(5) . . ?
N3 Ni1 O1W 88.0(5) . . ?
N1 Ni1 O1W 173.4(5) . . ?
N8 Ni1 O1W 96.9(5) 1_456 . ?
O2 C1 O1 126.3(14) . . ?
O2 C1 C2 118.8(13) . . ?
O1 C1 C2 114.8(13) . . ?
C3 C2 C7 119.6(14) . . ?
C3 C2 C1 116.2(14) . . ?
C7 C2 C1 123.8(13) . . ?
C4 C3 C2 121.2(15) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C5 C4 C3 120.2(15) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 118.6(15) . . ?
C4 C5 C8 121.1(16) . . ?
C6 C5 C8 120.3(16) . . ?
C7 C6 C5 122.7(15) . . ?
C7 C6 H6 118.6 . . ?
C5 C6 H6 118.6 . . ?
C6 C7 C2 117.7(14) . . ?
C6 C7 C9 119.5(14) . . ?
C2 C7 C9 122.6(14) . . ?
O3 C8 O4 124(2) . . ?
O3 C8 C5 118.2(18) . . ?
O4 C8 C5 117.7(18) . . ?
C10 C9 C11 117.7(14) . 2_556 ?
C10 C9 C7 121.2(14) . . ?
C11 C9 C7 121.0(15) 2_556 . ?
C11 C10 C9 121.0(15) . . ?
C11 C10 H10 119.5 . . ?
C9 C10 H10 119.5 . . ?
C10 C11 C9 121.3(15) . 2_556 ?
C10 C11 H11 119.3 . . ?
C9 C11 H11 119.3 2_556 . ?
N1 C12 N2 111.9(15) . . ?
N1 C12 H12 124.1 . . ?
N2 C12 H12 124.1 . . ?
C14 C13 N2 106.5(16) . . ?
C14 C13 H13 126.8 . . ?
N2 C13 H13 126.8 . . ?
C13 C14 N1 109.5(16) . . ?
C13 C14 H14 125.3 . . ?
N1 C14 H14 125.2 . . ?
C16 C15 C20 120.3(18) . . ?
C16 C15 N2 120.3(19) . . ?
C20 C15 N2 119.0(18) . . ?
C15 C16 C17 119(2) . . ?
C15 C16 H16 120.3 . . ?
C17 C16 H16 120.3 . . ?
C18 C17 C16 122(2) . . ?
C18 C17 H17 119.1 . . ?
C16 C17 H17 119.1 . . ?
C17 C18 C19 117.6(19) . . ?
C17 C18 C18 121(3) . 2_657 ?
C19 C18 C18 121(3) . 2_657 ?
C18 C19 C20 121(2) . . ?
C18 C19 H19 119.3 . . ?
C20 C19 H19 119.3 . . ?
C15 C20 C19 120(2) . . ?
C15 C20 H20 120.2 . . ?
C19 C20 H20 120.2 . . ?
N3 C21 N4 112.2(15) . . ?
N3 C21 H21 123.9 . . ?
N4 C21 H21 123.9 . . ?
C23 C22 N3 110.2(15) . . ?
C23 C22 H22 124.9 . . ?
N3 C22 H22 124.9 . . ?
C22 C23 N4 106.0(15) . . ?
C22 C23 H23 127.0 . . ?
N4 C23 H23 127.0 . . ?
C25 C24 C25' 29.7(13) . . ?
C25 C24 C29' 110(2) . . ?
C25' C24 C29' 122(2) . . ?
C25 C24 N4 127(2) . . ?
C25' C24 N4 121.8(18) . . ?
C29' C24 N4 116(2) . . ?
C25 C24 C29 118(3) . . ?
C25' C24 C29 112(2) . . ?
C29' C24 C29 33.2(16) . . ?
N4 C24 C29 115(2) . . ?
C24 C25 C26 121(3) . . ?
C24 C25 H25 119.3 . . ?
C26 C25 H25 119.3 . . ?
C27 C26 C25 122(3) . . ?
C27 C26 H26 118.8 . . ?
C25 C26 H26 118.8 . . ?
C26 C27 C28 119(4) . . ?
C26 C27 C27 117(5) . 2 ?
C28 C27 C27 124(5) . 2 ?
C29 C28 C27 118(4) . . ?
C29 C28 H28 121.1 . . ?
C27 C28 H28 121.2 . . ?
C28 C29 C24 121(3) . . ?
C28 C29 H29 119.3 . . ?
C24 C29 H29 119.3 . . ?
C24 C25' C26' 120(3) . . ?
C24 C25' H25' 119.9 . . ?
C26' C25' H25' 119.9 . . ?
C27' C26' C25' 120(3) . . ?
C27' C26' H26' 119.8 . . ?
C25' C26' H26' 119.8 . . ?
C26' C27' C28' 118(3) . . ?
C26' C27' C27' 124(4) . 2 ?
C28' C27' C27' 118(4) . 2 ?
C27' C28' C29' 122(4) . . ?
C27' C28' H28' 119.0 . . ?
C29' C28' H28' 119.0 . . ?
C24 C29' C28' 117(3) . . ?
C24 C29' H29' 121.4 . . ?
C28' C29' H29' 121.4 . . ?
C31 C30 N5 110.7(16) . . ?
C31 C30 H30 124.7 . . ?
N5 C30 H30 124.7 . . ?
C30 C31 N6 106.3(16) . . ?
C30 C31 H31 126.9 . . ?
N6 C31 H31 126.9 . . ?
N5 C32 N6 112.4(15) . . ?
N5 C32 H32 123.8 . . ?
N6 C32 H32 123.8 . . ?
C34 C33 C38 119.0(16) . . ?
C34 C33 N6 120.6(15) . . ?
C38 C33 N6 120.4(15) . . ?
C33 C34 C35 120.4(17) . . ?
C33 C34 H34 119.8 . . ?
C35 C34 H34 119.8 . . ?
C34 C35 C36 121.9(17) . . ?
C34 C35 H35 119.1 . . ?
C36 C35 H35 119.1 . . ?
C37 C36 C35 116.2(16) . . ?
C37 C36 C39 122.2(17) . . ?
C35 C36 C39 121.6(16) . . ?
C36 C37 C38 122.3(18) . . ?
C36 C37 H37 118.9 . . ?
C38 C37 H37 118.9 . . ?
C33 C38 C37 120.1(18) . . ?
C33 C38 H38 119.9 . . ?
C37 C38 H38 119.9 . . ?
C40 C39 C44 116.9(17) . . ?
C40 C39 C36 121.9(17) . . ?
C44 C39 C36 121.2(17) . . ?
C39 C40 C41 122.1(18) . . ?
C39 C40 H40 118.9 . . ?
C41 C40 H40 118.9 . . ?
C42 C41 C40 119.5(18) . . ?
C42 C41 H41 120.3 . . ?
C40 C41 H41 120.3 . . ?
C43 C42 C41 120.0(16) . . ?
C43 C42 N7 119.9(17) . . ?
C41 C42 N7 120.1(16) . . ?
C42 C43 C44 119.7(19) . . ?
C42 C43 H43 120.1 . . ?
C44 C43 H43 120.1 . . ?
C39 C44 C43 121.7(19) . . ?
C39 C44 H44 119.1 . . ?
C43 C44 H44 119.1 . . ?
N8 C45 N7 111.7(15) . . ?
N8 C45 H45 124.1 . . ?
N7 C45 H45 124.1 . . ?
C47 C46 N8 109.9(15) . . ?
C47 C46 H46 125.0 . . ?
N8 C46 H46 125.0 . . ?
C46 C47 N7 106.0(16) . . ?
C46 C47 H47 127.0 . . ?
N7 C47 H47 127.0 . . ?
C12 N1 C14 105.6(14) . . ?
C12 N1 Ni1 127.2(11) . . ?
C14 N1 Ni1 123.8(11) . . ?
C12 N2 C13 106.5(14) . . ?
C12 N2 C15 124.7(15) . . ?
C13 N2 C15 128.5(16) . . ?
C21 N3 C22 105.0(14) . . ?
C21 N3 Ni1 122.9(11) . . ?
C22 N3 Ni1 130.3(11) . . ?
C21 N4 C23 106.6(14) . . ?
C21 N4 C24 125.9(15) . . ?
C23 N4 C24 127.3(14) . . ?
C32 N5 C30 104.9(14) . . ?
C32 N5 Ni1 121.4(11) . . ?
C30 N5 Ni1 133.5(12) . . ?
C32 N6 C31 105.8(14) . . ?
C32 N6 C33 127.4(14) . . ?
C31 N6 C33 126.8(14) . . ?
C45 N7 C47 106.9(14) . . ?
C45 N7 C42 124.5(15) . . ?
C47 N7 C42 128.3(15) . . ?
C45 N8 C46 105.4(14) . . ?
C45 N8 Ni1 118.1(11) . 1_654 ?
C46 N8 Ni1 131.7(11) . 1_654 ?
C1 O1 Ni1 133.7(10) . . ?
Ni1 O1W H1W 95.2 . . ?
Ni1 O1W H2W 122.6 . . ?
H1W O1W H2W 107.6 . . ?
H3W O2W H4W 106.2 . . ?
H5W O3W H6W 124.3 . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.442
_refine_diff_density_min         -1.180
_refine_diff_density_rms         0.094
_database_code_depnum_ccdc_archive 'CCDC 973830'

data_z

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C41 H36 N6 Ni O6'
_chemical_formula_weight         767.47

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

_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                   12.785(3)
_cell_length_b                   13.443(4)
_cell_length_c                   14.029(4)
_cell_angle_alpha                96.636(4)
_cell_angle_beta                 114.001(4)
_cell_angle_gamma                115.893(4)
_cell_volume                     1851.2(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2557
_cell_measurement_theta_min      2.80
_cell_measurement_theta_max      23.09

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             800
_exptl_absorpt_coefficient_mu    0.581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8052
_exptl_absorpt_correction_T_max  0.9231
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9682
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.70
_diffrn_reflns_theta_max         25.25
_reflns_number_total             6660
_reflns_number_gt                4883
_reflns_threshold_expression     >2sigma(I)

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

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


1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{C14, C14'}
3. Restrained distances
 C11-C12 = C12-C13 = C13-C14 = C14-C15 = C15-C16 = C16-C11
 1.4 with sigma of 0.01
 C11-C12' = C12'-C13' = C13'-C14' = C14'-C15' = C15'-C16' = C16'-C11
 1.4 with sigma of 0.01
 C11-C13 = C12-C14 = C13-C15 = C14-C16 = C15-C11 = C16-C12
 2.45 with sigma of 0.02
 C11-C13' = C12'-C14' = C13'-C15' = C14'-C16' = C15'-C11 = C16'-C12'
 2.45 with sigma of 0.02
 H1WB-H1WA = H2WA-H2WB
 1.38 with sigma of 0.001
 H1WB-O1W = H1WA-O1W = H2WA-O2W = H2WB-O2W
 0.82 with sigma of 0.001
4. Restrained planarity
 C11, C12, C13, C14, C15, C16
 with sigma of 0.01
 C11, C12', C13', C14', C15', C16'
 with sigma of 0.01
5. Uiso/Uaniso restraints and constraints
C13 ∼ C14: within 1.45A with sigma of 0.01 and sigma for terminal atoms of
0.02
C12 ∼ C11: within 1.45A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C12) = Uanis(C12')
Uanis(C13) = Uanis(C13')
Uanis(C14) = Uanis(C14')
Uanis(C15) = Uanis(C15')
Uanis(C16) = Uanis(C16')

;

_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)+(0.0740P)²+1.6507P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6660
_refine_ls_number_parameters     512
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0529
_refine_ls_wR_factor_ref         0.1490
_refine_ls_wR_factor_gt          0.1317
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.005
_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
C1 C 0.3284(5) 0.5770(4) 0.6074(4) 0.0481(11) Uani 1 1 d . . .
H1 H 0.3176 0.6109 0.6615 0.058 Uiso 1 1 calc R . .
C2 C 0.3977(5) 0.5537(4) 0.4969(4) 0.0537(12) Uani 1 1 d . . .
H2 H 0.4463 0.5700 0.4602 0.064 Uiso 1 1 calc R . .
C3 C 0.3005(5) 0.4450(4) 0.4784(4) 0.0530(12) Uani 1 1 d . . .
H3 H 0.2692 0.3738 0.4272 0.064 Uiso 1 1 calc R . .
C4 C 0.1535(6) 0.3614(4) 0.5595(5) 0.0738(17) Uani 1 1 d . . .
H4A H 0.1895 0.3153 0.5914 0.089 Uiso 1 1 calc R . .
H4B H 0.0750 0.3098 0.4858 0.089 Uiso 1 1 calc R . .
C5 C 0.1113(6) 0.4054(4) 0.6312(5) 0.0588(14) Uani 1 1 d . . .
C6 C -0.0032(6) 0.4110(5) 0.5856(5) 0.0708(17) Uani 1 1 d . . .
H6 H -0.0603 0.3798 0.5085 0.085 Uiso 1 1 calc R . .
C7 C -0.0352(6) 0.4620(5) 0.6521(5) 0.0724(17) Uani 1 1 d . . .
H7 H -0.1138 0.4635 0.6192 0.087 Uiso 1 1 calc R . .
C8 C 0.0486(5) 0.5109(4) 0.7673(4) 0.0576(13) Uani 1 1 d . A .
C9 C 0.1605(5) 0.5004(5) 0.8136(4) 0.0605(14) Uani 1 1 d . . .
H9 H 0.2160 0.5290 0.8908 0.073 Uiso 1 1 calc R . .
C10 C 0.1904(6) 0.4482(5) 0.7468(5) 0.0644(14) Uani 1 1 d . . .
H10 H 0.2652 0.4414 0.7798 0.077 Uiso 1 1 calc R . .
C11 C 0.0206(5) 0.5736(4) 0.8373(4) 0.0668(15) Uani 1 1 d DU . .
C12 C -0.0394(7) 0.6341(7) 0.8170(8) 0.060(2) Uani 0.509(4) 1 d PDU A 1
H12 H -0.0668 0.6399 0.7466 0.072 Uiso 0.509(4) 1 calc PR A 1
C13 C -0.0674(8) 0.6882(8) 0.8802(7) 0.059(2) Uani 0.509(4) 1 d PDU A 1
H13 H -0.1199 0.7195 0.8496 0.071 Uiso 0.509(4) 1 calc PR A 1
C14 C -0.0231(5) 0.6972(4) 0.9816(5) 0.085(2) Uani 0.509(4) 1 d PDU A 1
C15 C 0.0298(9) 0.6220(7) 1.0247(7) 0.064(2) Uani 0.509(4) 1 d PD A 1
H15 H 0.0455 0.6142 1.0935 0.076 Uiso 0.509(4) 1 calc PR A 1
C16 C 0.0543(9) 0.5635(7) 0.9526(7) 0.065(2) Uani 0.509(4) 1 d PD A 1
H16 H 0.0912 0.5184 0.9757 0.078 Uiso 0.509(4) 1 calc PR A 1
C12' C -0.0959(9) 0.5655(8) 0.8060(8) 0.060(2) Uani 0.491(4) 1 d PD A 2
H12' H -0.1675 0.5129 0.7347 0.072 Uiso 0.491(4) 1 calc PR A 2
C13' C -0.1208(9) 0.6267(8) 0.8683(7) 0.059(2) Uani 0.491(4) 1 d PD A 2
H13' H -0.2030 0.6222 0.8362 0.071 Uiso 0.491(4) 1 calc PR A 2
C14' C -0.0231(5) 0.6972(4) 0.9816(5) 0.085(2) Uani 0.491(4) 1 d PD A 2
C15' C 0.1087(9) 0.7226(8) 1.0096(8) 0.064(2) Uani 0.491(4) 1 d PD A 2
H15' H 0.1829 0.7839 1.0758 0.076 Uiso 0.491(4) 1 calc PR A 2
C16' C 0.1315(9) 0.6594(7) 0.9419(7) 0.065(2) Uani 0.491(4) 1 d PD A 2
H16' H 0.2177 0.6738 0.9655 0.078 Uiso 0.491(4) 1 calc PR A 2
C17 C -0.0452(6) 0.7605(6) 1.0623(6) 0.097(2) Uani 1 1 d . . .
H17A H -0.0853 0.8028 1.0272 0.117 Uiso 1 1 calc R A 1
H17B H -0.1086 0.7021 1.0775 0.117 Uiso 1 1 calc R A 1
C18 C 0.1383(6) 0.8246(5) 1.2638(6) 0.0707(16) Uani 1 1 d . . .
H18 H 0.1011 0.7556 1.2783 0.085 Uiso 1 1 calc R A .
C19 C 0.2587(6) 0.9240(4) 1.3323(5) 0.0579(13) Uani 1 1 d . A .
H19 H 0.3199 0.9360 1.4042 0.070 Uiso 1 1 calc R . .
C20 C 0.1698(5) 0.9547(4) 1.1824(4) 0.0526(12) Uani 1 1 d . . .
H20 H 0.1554 0.9899 1.1289 0.063 Uiso 1 1 calc R A .
C21 C 0.4229(4) 0.8640(3) 0.6985(4) 0.0341(9) Uani 1 1 d . . .
C22 C 0.3310(4) 0.8865(4) 0.7249(3) 0.0342(9) Uani 1 1 d . . .
C23 C 0.3265(5) 0.8803(4) 0.8207(4) 0.0467(11) Uani 1 1 d . . .
H23 H 0.3844 0.8644 0.8731 0.056 Uiso 1 1 calc R . .
C24 C 0.2369(5) 0.8976(4) 0.8394(4) 0.0468(11) Uani 1 1 d . . .
H24 H 0.2375 0.8959 0.9057 0.056 Uiso 1 1 calc R . .
C25 C 0.1451(4) 0.9176(4) 0.7609(3) 0.0338(9) Uani 1 1 d . . .
C26 C 0.1518(4) 0.9291(3) 0.6644(3) 0.0301(8) Uani 1 1 d . . .
C27 C 0.2452(4) 0.9126(3) 0.6490(3) 0.0329(9) Uani 1 1 d . . .
H27 H 0.2502 0.9194 0.5855 0.039 Uiso 1 1 calc R . .
C28 C 0.0357(4) 0.9158(4) 0.7808(4) 0.0379(10) Uani 1 1 d . . .
C29 C 0.0689(4) 0.9624(3) 0.5800(3) 0.0292(8) Uani 1 1 d . . .
C30 C 0.0398(4) 1.0450(3) 0.6110(3) 0.0308(9) Uani 1 1 d . . .
H30 H 0.0661 1.0763 0.6853 0.037 Uiso 1 1 calc R . .
C31 C -0.0282(4) 1.0811(3) 0.5322(3) 0.0326(9) Uani 1 1 d . . .
H31 H -0.0470 1.1359 0.5548 0.039 Uiso 1 1 calc R . .
C32 C 0.4741(5) 0.7901(4) 0.4074(4) 0.0459(11) Uani 1 1 d . . .
H32 H 0.3904 0.7757 0.3939 0.055 Uiso 1 1 calc R . .
C33 C 0.6389(4) 0.8169(4) 0.3822(4) 0.0466(11) Uani 1 1 d . . .
H33 H 0.6912 0.8245 0.3497 0.056 Uiso 1 1 calc R . .
C34 C 0.6760(4) 0.8267(4) 0.4889(4) 0.0409(10) Uani 1 1 d . . .
H34 H 0.7594 0.8428 0.5434 0.049 Uiso 1 1 calc R . .
C35 C 0.4286(6) 0.7731(6) 0.2124(4) 0.0663(15) Uani 1 1 d . . .
H35A H 0.4587 0.8476 0.1998 0.080 Uiso 1 1 calc R . .
H35B H 0.3343 0.7377 0.1912 0.080 Uiso 1 1 calc R . .
C36 C 0.4434(5) 0.6912(5) 0.1431(4) 0.0594(14) Uani 1 1 d . . .
C37 C 0.3976(6) 0.5780(6) 0.1409(5) 0.0739(17) Uani 1 1 d . . .
H37 H 0.3503 0.5502 0.1773 0.089 Uiso 1 1 calc R . .
C38 C 0.4193(6) 0.5026(5) 0.0859(5) 0.0710(16) Uani 1 1 d . . .
H38 H 0.3875 0.4262 0.0871 0.085 Uiso 1 1 calc R . .
C39 C 0.4875(5) 0.5398(5) 0.0295(4) 0.0544(13) Uani 1 1 d . . .
C40 C 0.5316(7) 0.6536(6) 0.0309(5) 0.0789(18) Uani 1 1 d . . .
H40 H 0.5769 0.6814 -0.0069 0.095 Uiso 1 1 calc R . .
C41 C 0.5108(7) 0.7281(6) 0.0869(5) 0.0766(17) Uani 1 1 d . . .
H41 H 0.5432 0.8048 0.0864 0.092 Uiso 1 1 calc R . .
N1 N 0.4147(3) 0.6370(3) 0.5777(3) 0.0400(8) Uani 1 1 d . . .
N2 N 0.2573(4) 0.4599(3) 0.5495(3) 0.0481(10) Uani 1 1 d . . .
N3 N 0.0808(4) 0.8444(4) 1.1683(4) 0.0645(13) Uani 1 1 d . A .
N4 N 0.2790(4) 1.0061(3) 1.2809(3) 0.0414(9) Uani 1 1 d . . .
N5 N 0.5712(3) 0.8092(3) 0.5042(3) 0.0390(8) Uani 1 1 d . . .
N6 N 0.5109(4) 0.7938(3) 0.3309(3) 0.0468(9) Uani 1 1 d . . .
Ni1 Ni 0.56351(5) 0.81747(5) 0.64694(4) 0.03286(18) Uani 1 1 d . . .
O1 O 0.5025(3) 0.8407(3) 0.7673(2) 0.0395(7) Uani 1 1 d . . .
O2 O 0.4184(3) 0.8658(3) 0.6073(2) 0.0431(7) Uani 1 1 d . . .
O3 O -0.0835(3) 0.8414(3) 0.7059(2) 0.0440(7) Uani 1 1 d . . .
O4 O 0.0717(4) 0.9827(4) 0.8723(3) 0.0689(11) Uani 1 1 d . . .
O1W O 0.7030(3) 0.7714(3) 0.7307(2) 0.0420(7) Uani 1 1 d D . .
O2W O 0.7146(4) 0.8338(3) 0.9362(3) 0.0603(9) Uani 1 1 d D . .
H2W H 0.771(2) 0.796(4) 0.725(3) 0.080 Uiso 1 1 d D . .
H1W H 0.718(4) 0.795(4) 0.7942(14) 0.080 Uiso 1 1 d D . .
H3W H 0.649(3) 0.840(4) 0.904(4) 0.080 Uiso 1 1 d D . .
H4W H 0.778(3) 0.889(3) 0.994(3) 0.080 Uiso 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.309(5) . ?
C1 N2 1.349(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.347(7) . ?
C2 N1 1.372(6) . ?
C2 H2 0.9300 . ?
C3 N2 1.356(6) . ?
C3 H3 0.9300 . ?
C4 N2 1.481(6) . ?
C4 C5 1.494(8) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.380(8) . ?
C5 C10 1.388(7) . ?
C6 C7 1.384(8) . ?
C6 H6 0.9300 . ?
C7 C8 1.387(7) . ?
C7 H7 0.9300 . ?
C8 C9 1.390(7) . ?
C8 C11 1.469(7) . ?
C9 C10 1.374(7) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12' 1.319(8) . ?
C11 C12 1.324(8) . ?
C11 C16' 1.408(8) . ?
C11 C16 1.535(8) . ?
C12 C13 1.334(9) . ?
C12 H12 0.9300 . ?
C13 C14 1.267(8) . ?
C13 H13 0.9300 . ?
C14 C15 1.500(8) . ?
C14 C17 1.529(8) . ?
C15 C16 1.425(9) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C12' C13' 1.353(9) . ?
C12' H12' 0.9300 . ?
C13' H13' 0.9300 . ?
C15' C16' 1.401(9) . ?
C15' H15' 0.9300 . ?
C16' H16' 0.9300 . ?
C17 N3 1.468(7) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.335(8) . ?
C18 N3 1.364(7) . ?
C18 H18 0.9300 . ?
C19 N4 1.375(6) . ?
C19 H19 0.9300 . ?
C20 N4 1.306(6) . ?
C20 N3 1.345(6) . ?
C20 H20 0.9300 . ?
C21 O2 1.260(5) . ?
C21 O1 1.271(5) . ?
C21 C22 1.500(5) . ?
C21 Ni1 2.466(4) . ?
C22 C23 1.379(6) . ?
C22 C27 1.390(5) . ?
C23 C24 1.377(6) . ?
C23 H23 0.9300 . ?
C24 C25 1.398(6) . ?
C24 H24 0.9300 . ?
C25 C26 1.412(5) . ?
C25 C28 1.523(5) . ?
C26 C27 1.397(5) . ?
C26 C29 1.497(5) . ?
C27 H27 0.9300 . ?
C28 O3 1.245(5) . ?
C28 O4 1.250(5) . ?
C29 C31 1.394(5) 2_576 ?
C29 C30 1.395(5) . ?
C30 C31 1.387(5) . ?
C30 H30 0.9300 . ?
C31 C29 1.394(5) 2_576 ?
C31 H31 0.9300 . ?
C32 N5 1.311(5) . ?
C32 N6 1.334(6) . ?
C32 H32 0.9300 . ?
C33 C34 1.343(6) . ?
C33 N6 1.356(6) . ?
C33 H33 0.9300 . ?
C34 N5 1.367(5) . ?
C34 H34 0.9300 . ?
C35 N6 1.471(6) . ?
C35 C36 1.509(8) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 C37 1.361(8) . ?
C36 C41 1.371(7) . ?
C37 C38 1.393(8) . ?
C37 H37 0.9300 . ?
C38 C39 1.381(7) . ?
C38 H38 0.9300 . ?
C39 C40 1.375(8) . ?
C39 C39 1.495(10) 2_665 ?
C40 C41 1.382(8) . ?
C40 H40 0.9300 . ?
C41 H41 0.9300 . ?
N1 Ni1 2.091(3) . ?
N4 Ni1 2.079(4) 2_677 ?
N5 Ni1 2.037(3) . ?
Ni1 N4 2.079(4) 2_677 ?
Ni1 O1W 2.091(3) . ?
Ni1 O2 2.113(3) . ?
Ni1 O1 2.172(3) . ?
O1W H2W 0.8201(14) . ?
O1W H1W 0.8200(12) . ?
O2W H3W 0.8201(12) . ?
O2W H4W 0.8201(13) . ?

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 C1 N2 111.5(4) . . ?
N1 C1 H1 124.3 . . ?
N2 C1 H1 124.3 . . ?
C3 C2 N1 110.0(4) . . ?
C3 C2 H2 125.0 . . ?
N1 C2 H2 125.0 . . ?
C2 C3 N2 106.3(4) . . ?
C2 C3 H3 126.8 . . ?
N2 C3 H3 126.8 . . ?
N2 C4 C5 111.8(4) . . ?
N2 C4 H4A 109.3 . . ?
C5 C4 H4A 109.3 . . ?
N2 C4 H4B 109.3 . . ?
C5 C4 H4B 109.3 . . ?
H4A C4 H4B 107.9 . . ?
C6 C5 C10 117.4(6) . . ?
C6 C5 C4 121.7(5) . . ?
C10 C5 C4 120.9(6) . . ?
C5 C6 C7 121.5(5) . . ?
C5 C6 H6 119.2 . . ?
C7 C6 H6 119.2 . . ?
C6 C7 C8 120.7(6) . . ?
C6 C7 H7 119.6 . . ?
C8 C7 H7 119.6 . . ?
C7 C8 C9 117.8(5) . . ?
C7 C8 C11 120.7(5) . . ?
C9 C8 C11 121.5(5) . . ?
C10 C9 C8 120.9(5) . . ?
C10 C9 H9 119.5 . . ?
C8 C9 H9 119.5 . . ?
C9 C10 C5 121.5(5) . . ?
C9 C10 H10 119.2 . . ?
C5 C10 H10 119.2 . . ?
C12' C11 C12 36.7(4) . . ?
C12' C11 C16' 117.0(7) . . ?
C12 C11 C16' 95.0(5) . . ?
C12' C11 C8 125.6(6) . . ?
C12 C11 C8 131.5(6) . . ?
C16' C11 C8 117.0(5) . . ?
C12' C11 C16 99.5(5) . . ?
C12 C11 C16 110.2(6) . . ?
C16' C11 C16 52.6(4) . . ?
C8 C11 C16 118.1(5) . . ?
C11 C12 C13 131.1(8) . . ?
C11 C12 H12 114.5 . . ?
C13 C12 H12 114.5 . . ?
C14 C13 C12 120.5(8) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C13 C14 C15 120.4(7) . . ?
C13 C14 C17 124.8(7) . . ?
C15 C14 C17 113.5(6) . . ?
C16 C15 C14 115.0(7) . . ?
C16 C15 H15 122.5 . . ?
C14 C15 H15 122.5 . . ?
C15 C16 C11 121.0(7) . . ?
C15 C16 H16 119.5 . . ?
C11 C16 H16 119.5 . . ?
C11 C12' C13' 125.9(9) . . ?
C11 C12' H12' 117.1 . . ?
C13' C12' H12' 117.1 . . ?
C12' C13' H13' 119.7 . . ?
C16' C15' H15' 118.5 . . ?
C15' C16' C11 118.4(8) . . ?
C15' C16' H16' 120.8 . . ?
C11 C16' H16' 120.8 . . ?
N3 C17 C14 112.6(4) . . ?
N3 C17 H17A 109.1 . . ?
C14 C17 H17A 109.1 . . ?
N3 C17 H17B 109.1 . . ?
C14 C17 H17B 109.1 . . ?
H17A C17 H17B 107.8 . . ?
C19 C18 N3 106.2(5) . . ?
C19 C18 H18 126.9 . . ?
N3 C18 H18 126.9 . . ?
C18 C19 N4 110.0(5) . . ?
C18 C19 H19 125.0 . . ?
N4 C19 H19 125.0 . . ?
N4 C20 N3 111.1(5) . . ?
N4 C20 H20 124.4 . . ?
N3 C20 H20 124.4 . . ?
O2 C21 O1 120.6(4) . . ?
O2 C21 C22 119.8(3) . . ?
O1 C21 C22 119.6(4) . . ?
O2 C21 Ni1 59.0(2) . . ?
O1 C21 Ni1 61.6(2) . . ?
C22 C21 Ni1 177.0(3) . . ?
C23 C22 C27 118.7(4) . . ?
C23 C22 C21 122.6(4) . . ?
C27 C22 C21 118.8(4) . . ?
C24 C23 C22 120.4(4) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C23 C24 C25 121.5(4) . . ?
C23 C24 H24 119.2 . . ?
C25 C24 H24 119.2 . . ?
C24 C25 C26 118.9(4) . . ?
C24 C25 C28 117.2(4) . . ?
C26 C25 C28 123.7(3) . . ?
C27 C26 C25 117.9(3) . . ?
C27 C26 C29 118.0(3) . . ?
C25 C26 C29 124.1(3) . . ?
C22 C27 C26 122.5(4) . . ?
C22 C27 H27 118.8 . . ?
C26 C27 H27 118.8 . . ?
O3 C28 O4 125.3(4) . . ?
O3 C28 C25 116.3(4) . . ?
O4 C28 C25 118.2(4) . . ?
C31 C29 C30 117.5(3) 2_576 . ?
C31 C29 C26 120.5(3) 2_576 . ?
C30 C29 C26 121.8(3) . . ?
C31 C30 C29 120.7(4) . . ?
C31 C30 H30 119.7 . . ?
C29 C30 H30 119.7 . . ?
C30 C31 C29 121.9(4) . 2_576 ?
C30 C31 H31 119.1 . . ?
C29 C31 H31 119.1 2_576 . ?
N5 C32 N6 111.3(4) . . ?
N5 C32 H32 124.3 . . ?
N6 C32 H32 124.3 . . ?
C34 C33 N6 107.1(4) . . ?
C34 C33 H33 126.4 . . ?
N6 C33 H33 126.4 . . ?
C33 C34 N5 108.8(4) . . ?
C33 C34 H34 125.6 . . ?
N5 C34 H34 125.6 . . ?
N6 C35 C36 108.6(4) . . ?
N6 C35 H35A 110.0 . . ?
C36 C35 H35A 110.0 . . ?
N6 C35 H35B 110.0 . . ?
C36 C35 H35B 110.0 . . ?
H35A C35 H35B 108.4 . . ?
C37 C36 C41 117.0(6) . . ?
C37 C36 C35 120.2(5) . . ?
C41 C36 C35 122.5(6) . . ?
C36 C37 C38 122.2(5) . . ?
C36 C37 H37 118.9 . . ?
C38 C37 H37 118.9 . . ?
C39 C38 C37 120.8(6) . . ?
C39 C38 H38 119.6 . . ?
C37 C38 H38 119.6 . . ?
C40 C39 C38 116.5(5) . . ?
C40 C39 C39 121.9(6) . 2_665 ?
C38 C39 C39 121.6(6) . 2_665 ?
C39 C40 C41 122.1(5) . . ?
C39 C40 H40 118.9 . . ?
C41 C40 H40 118.9 . . ?
C36 C41 C40 121.3(6) . . ?
C36 C41 H41 119.4 . . ?
C40 C41 H41 119.4 . . ?
C1 N1 C2 105.2(4) . . ?
C1 N1 Ni1 129.1(3) . . ?
C2 N1 Ni1 125.4(3) . . ?
C1 N2 C3 107.1(4) . . ?
C1 N2 C4 128.9(4) . . ?
C3 N2 C4 124.0(4) . . ?
C20 N3 C18 107.2(5) . . ?
C20 N3 C17 123.8(6) . . ?
C18 N3 C17 128.6(6) . . ?
C20 N4 C19 105.5(4) . . ?
C20 N4 Ni1 126.9(3) . 2_677 ?
C19 N4 Ni1 127.1(3) . 2_677 ?
C32 N5 C34 105.9(4) . . ?
C32 N5 Ni1 125.3(3) . . ?
C34 N5 Ni1 128.7(3) . . ?
C32 N6 C33 106.8(4) . . ?
C32 N6 C35 127.3(4) . . ?
C33 N6 C35 125.8(4) . . ?
N5 Ni1 N4 89.14(14) . 2_677 ?
N5 Ni1 O1W 99.72(13) . . ?
N4 Ni1 O1W 89.19(13) 2_677 . ?
N5 Ni1 N1 90.61(14) . . ?
N4 Ni1 N1 176.24(14) 2_677 . ?
O1W Ni1 N1 87.15(13) . . ?
N5 Ni1 O2 98.06(12) . . ?
N4 Ni1 O2 91.45(13) 2_677 . ?
O1W Ni1 O2 162.22(12) . . ?
N1 Ni1 O2 92.30(13) . . ?
N5 Ni1 O1 159.77(12) . . ?
N4 Ni1 O1 91.87(13) 2_677 . ?
O1W Ni1 O1 100.49(11) . . ?
N1 Ni1 O1 89.66(12) . . ?
O2 Ni1 O1 61.72(11) . . ?
N5 Ni1 C21 128.78(14) . . ?
N4 Ni1 C21 92.40(14) 2_677 . ?
O1W Ni1 C21 131.48(13) . . ?
N1 Ni1 C21 90.68(13) . . ?
O2 Ni1 C21 30.74(12) . . ?
O1 Ni1 C21 30.99(12) . . ?
C21 O1 Ni1 87.4(2) . . ?
C21 O2 Ni1 90.3(2) . . ?
Ni1 O1W H2W 118(4) . . ?
Ni1 O1W H1W 99(4) . . ?
H2W O1W H1W 114.6(3) . . ?
H3W O2W H4W 114.6(2) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.879
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.065
_database_code_depnum_ccdc_archive 'CCDC 973831'
