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

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H31 N3 Ni O7'
_chemical_formula_weight         676.35

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           Orthorhombic
_symmetry_space_group_name_H-M   Pbca

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

_cell_length_a                   9.574(3)
_cell_length_b                   22.596(7)
_cell_length_c                   30.900(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6685(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1519
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      17.93

_exptl_crystal_description       block
_exptl_crystal_colour            yellow-green
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      1.342
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2816
_exptl_absorpt_coefficient_mu    0.633
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_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 APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            35667
_diffrn_reflns_av_R_equivalents  0.1344
_diffrn_reflns_av_sigmaI/netI    0.0942
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         1.80
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5888
_reflns_number_gt                2892
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_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)+(0.1133P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5888
_refine_ls_number_parameters     424
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1526
_refine_ls_R_factor_gt           0.0695
_refine_ls_wR_factor_ref         0.2221
_refine_ls_wR_factor_gt          0.1866
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      1.003
_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 0.60869(8) 0.11685(3) 0.15198(2) 0.0478(3) Uani 1 1 d . . .
C7 C 0.9058(7) 0.1352(3) 0.13958(19) 0.0570(16) Uani 1 1 d . . .
N2 N 0.6004(5) 0.06484(19) 0.20711(14) 0.0456(11) Uani 1 1 d . . .
O4 O 0.5978(4) 0.16976(18) 0.09738(13) 0.0607(11) Uani 1 1 d . . .
N1 N 0.7356(5) 0.16926(18) 0.19293(14) 0.0478(12) Uani 1 1 d . . .
O1 O 0.4261(4) 0.15431(18) 0.17388(13) 0.0574(11) Uani 1 1 d . . .
O3 O 0.5112(4) 0.05955(16) 0.11277(12) 0.0585(11) Uani 1 1 d . . .
N3 N 0.8099(5) 0.0938(2) 0.13067(15) 0.0540(12) Uani 1 1 d . . .
C20 C 0.3785(7) 0.2050(3) 0.17092(19) 0.0547(15) Uani 1 1 d . . .
O2 O 0.2526(5) 0.21820(19) 0.17678(16) 0.0759(13) Uani 1 1 d . . .
O5 O 0.3611(5) 0.0877(2) 0.00654(13) 0.0737(13) Uani 1 1 d . . .
C14 C 0.6033(7) 0.2638(3) 0.18032(18) 0.0553(16) Uani 1 1 d . . .
C27 C 0.5220(7) 0.1458(3) 0.0694(2) 0.0581(16) Uani 1 1 d . . .
C28 C 0.3988(8) 0.1447(4) 0.0007(2) 0.074(2) Uani 1 1 d . . .
C22 C 0.3977(6) 0.0581(3) 0.04378(19) 0.0595(16) Uani 1 1 d . . .
C13 C 0.6624(7) 0.2208(2) 0.21248(18) 0.0538(15) Uani 1 1 d . . .
H13A H 0.7274 0.2417 0.2311 0.065 Uiso 1 1 calc R . .
H13B H 0.5869 0.2062 0.2305 0.065 Uiso 1 1 calc R . .
C6 C 0.7841(6) 0.1306(3) 0.22903(18) 0.0549(16) Uani 1 1 d . . .
H6A H 0.8713 0.1119 0.2209 0.066 Uiso 1 1 calc R . .
H6B H 0.8014 0.1548 0.2544 0.066 Uiso 1 1 calc R . .
C21 C 0.4748(6) 0.0852(3) 0.07646(18) 0.0527(15) Uani 1 1 d . . .
C12 C 0.8553(6) 0.1874(3) 0.16552(19) 0.0576(16) Uani 1 1 d . . .
H12A H 0.9304 0.2021 0.1836 0.069 Uiso 1 1 calc R . .
H12B H 0.8268 0.2190 0.1462 0.069 Uiso 1 1 calc R . .
C5 C 0.5107(7) 0.0212(3) 0.2146(2) 0.0595(16) Uani 1 1 d . . .
H5A H 0.4550 0.0078 0.1920 0.071 Uiso 1 1 calc R . .
C1 C 0.6799(6) 0.0843(2) 0.23986(18) 0.0487(14) Uani 1 1 d . . .
C17 C 0.5079(8) 0.3478(3) 0.1209(2) 0.078(2) Uani 1 1 d . . .
H17A H 0.4768 0.3752 0.1006 0.093 Uiso 1 1 calc R . .
O6 O 0.7067(5) 0.4058(2) 0.13004(18) 0.0911(16) Uani 1 1 d . . .
C2 C 0.6692(7) 0.0618(3) 0.2808(2) 0.0607(17) Uani 1 1 d . . .
H2A H 0.7233 0.0772 0.3031 0.073 Uiso 1 1 calc R . .
C19 C 0.6849(8) 0.3144(3) 0.1710(2) 0.0660(18) Uani 1 1 d . . .
H19A H 0.7703 0.3204 0.1847 0.079 Uiso 1 1 calc R . .
C30 C 0.3473(7) -0.0024(3) 0.0436(2) 0.0624(17) Uani 1 1 d . . .
C29 C 0.4808(7) 0.1752(3) 0.0293(2) 0.0656(18) Uani 1 1 d . . .
C4 C 0.4973(8) -0.0051(3) 0.2552(3) 0.074(2) Uani 1 1 d . . .
H4A H 0.4356 -0.0363 0.2596 0.089 Uiso 1 1 calc R . .
C15 C 0.4729(6) 0.2569(3) 0.16057(19) 0.0544(15) Uani 1 1 d . . .
C31 C 0.3681(7) -0.0417(3) 0.0772(2) 0.076(2) Uani 1 1 d . . .
H31A H 0.4128 -0.0279 0.1020 0.091 Uiso 1 1 calc R . .
C33 C 0.2551(10) -0.1210(4) 0.0411(3) 0.100(3) Uani 1 1 d . . .
H33A H 0.2253 -0.1601 0.0400 0.121 Uiso 1 1 calc R . .
C18 C 0.6342(8) 0.3550(3) 0.1410(2) 0.071(2) Uani 1 1 d . . .
C16 C 0.4272(7) 0.2991(3) 0.1312(2) 0.0689(19) Uani 1 1 d . . .
H16A H 0.3404 0.2945 0.1182 0.083 Uiso 1 1 calc R . .
C26 C 0.5199(9) 0.2343(3) 0.0205(2) 0.086(2) Uani 1 1 d . . .
H26A H 0.5734 0.2557 0.0401 0.104 Uiso 1 1 calc R . .
C3 C 0.5782(8) 0.0166(3) 0.2885(3) 0.077(2) Uani 1 1 d . . .
H3A H 0.5709 0.0004 0.3161 0.092 Uiso 1 1 calc R . .
C35 C 0.2754(9) -0.0256(4) 0.0076(2) 0.091(2) Uani 1 1 d . . .
H35A H 0.2593 -0.0018 -0.0164 0.110 Uiso 1 1 calc R . .
C24 C 0.3971(12) 0.2285(5) -0.0472(3) 0.127(4) Uani 1 1 d . . .
H24A H 0.3706 0.2460 -0.0732 0.152 Uiso 1 1 calc R . .
C34 C 0.2286(10) -0.0832(4) 0.0077(3) 0.107(3) Uani 1 1 d . . .
H34A H 0.1772 -0.0968 -0.0158 0.128 Uiso 1 1 calc R . .
C32 C 0.3266(9) -0.1001(4) 0.0764(3) 0.097(3) Uani 1 1 d . . .
H32A H 0.3469 -0.1251 0.0995 0.117 Uiso 1 1 calc R . .
C23 C 0.3582(10) 0.1733(4) -0.0380(3) 0.110(3) Uani 1 1 d . . .
H23A H 0.3026 0.1529 -0.0577 0.132 Uiso 1 1 calc R . .
C36 C 0.8352(9) 0.4162(4) 0.1517(3) 0.110(3) Uani 1 1 d . . .
H36A H 0.8757 0.4524 0.1413 0.165 Uiso 1 1 calc R . .
H36B H 0.8980 0.3840 0.1461 0.165 Uiso 1 1 calc R . .
H36C H 0.8188 0.4192 0.1823 0.165 Uiso 1 1 calc R . .
C25 C 0.4772(12) 0.2593(4) -0.0176(3) 0.118(3) Uani 1 1 d . . .
H25A H 0.5028 0.2981 -0.0238 0.141 Uiso 1 1 calc R . .
C11 C 0.8483(7) 0.0466(3) 0.10687(19) 0.0684(19) Uani 1 1 d . . .
H11A H 0.7816 0.0180 0.1005 0.082 Uiso 1 1 calc R . .
C8 C 1.0415(7) 0.1313(3) 0.1253(2) 0.077(2) Uani 1 1 d . . .
H8A H 1.1068 0.1603 0.1322 0.093 Uiso 1 1 calc R . .
C10 C 0.9815(9) 0.0390(4) 0.0917(2) 0.086(2) Uani 1 1 d . . .
H10A H 1.0068 0.0054 0.0761 0.103 Uiso 1 1 calc R . .
C9 C 1.0775(8) 0.0836(4) 0.1006(3) 0.091(2) Uani 1 1 d . . .
H9A H 1.1676 0.0809 0.0895 0.109 Uiso 1 1 calc R . .
O7 O 0.1125(11) 0.3253(5) 0.1919(3) 0.264(7) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O3 2.004(4) . ?
Ni1 O1 2.057(4) . ?
Ni1 O4 2.070(4) . ?
Ni1 N2 2.071(5) . ?
Ni1 N3 2.101(5) . ?
Ni1 N1 2.117(4) . ?
C7 N3 1.339(8) . ?
C7 C8 1.376(9) . ?
C7 C12 1.506(8) . ?
N2 C5 1.328(7) . ?
N2 C1 1.340(7) . ?
O4 C27 1.252(7) . ?
N1 C12 1.483(7) . ?
N1 C13 1.487(7) . ?
N1 C6 1.490(6) . ?
O1 C20 1.237(7) . ?
O3 C21 1.310(6) . ?
N3 C11 1.347(7) . ?
C20 O2 1.254(7) . ?
C20 C15 1.514(8) . ?
O5 C28 1.350(9) . ?
O5 C22 1.376(7) . ?
C14 C15 1.398(8) . ?
C14 C19 1.414(8) . ?
C14 C13 1.500(8) . ?
C27 C21 1.459(9) . ?
C27 C29 1.461(8) . ?
C28 C29 1.368(10) . ?
C28 C23 1.414(10) . ?
C22 C21 1.392(8) . ?
C22 C30 1.449(9) . ?
C6 C1 1.484(8) . ?
C5 C4 1.393(9) . ?
C1 C2 1.368(8) . ?
C17 C18 1.369(9) . ?
C17 C16 1.381(9) . ?
O6 C18 1.383(7) . ?
O6 C36 1.420(9) . ?
C2 C3 1.365(9) . ?
C19 C18 1.394(9) . ?
C30 C31 1.381(9) . ?
C30 C35 1.410(9) . ?
C29 C26 1.415(9) . ?
C4 C3 1.379(10) . ?
C15 C16 1.387(8) . ?
C31 C32 1.380(9) . ?
C33 C34 1.364(11) . ?
C33 C32 1.370(10) . ?
C26 C25 1.368(10) . ?
C35 C34 1.376(11) . ?
C24 C23 1.332(12) . ?
C24 C25 1.382(13) . ?
C11 C10 1.370(9) . ?
C8 C9 1.364(10) . ?
C10 C9 1.392(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
O3 Ni1 O1 93.95(17) . . ?
O3 Ni1 O4 81.78(16) . . ?
O1 Ni1 O4 89.31(16) . . ?
O3 Ni1 N2 96.48(17) . . ?
O1 Ni1 N2 86.02(16) . . ?
O4 Ni1 N2 174.89(17) . . ?
O3 Ni1 N3 94.44(18) . . ?
O1 Ni1 N3 169.81(18) . . ?
O4 Ni1 N3 86.18(17) . . ?
N2 Ni1 N3 98.76(18) . . ?
O3 Ni1 N1 172.03(17) . . ?
O1 Ni1 N1 93.50(17) . . ?
O4 Ni1 N1 101.12(17) . . ?
N2 Ni1 N1 81.24(17) . . ?
N3 Ni1 N1 78.44(18) . . ?
N3 C7 C8 122.4(6) . . ?
N3 C7 C12 115.9(6) . . ?
C8 C7 C12 121.7(6) . . ?
C5 N2 C1 118.6(5) . . ?
C5 N2 Ni1 126.1(4) . . ?
C1 N2 Ni1 114.4(4) . . ?
C27 O4 Ni1 110.0(4) . . ?
C12 N1 C13 112.3(4) . . ?
C12 N1 C6 110.4(4) . . ?
C13 N1 C6 107.5(4) . . ?
C12 N1 Ni1 104.9(3) . . ?
C13 N1 Ni1 114.2(3) . . ?
C6 N1 Ni1 107.4(3) . . ?
C20 O1 Ni1 132.1(4) . . ?
C21 O3 Ni1 110.9(4) . . ?
C7 N3 C11 118.6(6) . . ?
C7 N3 Ni1 113.0(4) . . ?
C11 N3 Ni1 128.1(4) . . ?
O1 C20 O2 124.3(6) . . ?
O1 C20 C15 120.8(6) . . ?
O2 C20 C15 114.9(6) . . ?
C28 O5 C22 120.5(5) . . ?
C15 C14 C19 119.7(6) . . ?
C15 C14 C13 123.6(6) . . ?
C19 C14 C13 116.7(6) . . ?
O4 C27 C21 118.9(5) . . ?
O4 C27 C29 123.1(6) . . ?
C21 C27 C29 118.0(6) . . ?
O5 C28 C29 123.2(6) . . ?
O5 C28 C23 118.4(8) . . ?
C29 C28 C23 118.3(8) . . ?
O5 C22 C21 121.9(6) . . ?
O5 C22 C30 111.7(6) . . ?
C21 C22 C30 126.4(6) . . ?
N1 C13 C14 114.6(4) . . ?
C1 C6 N1 111.9(5) . . ?
O3 C21 C22 124.6(6) . . ?
O3 C21 C27 117.4(5) . . ?
C22 C21 C27 118.0(6) . . ?
N1 C12 C7 109.6(5) . . ?
N2 C5 C4 122.2(6) . . ?
N2 C1 C2 122.3(6) . . ?
N2 C1 C6 116.3(5) . . ?
C2 C1 C6 121.4(6) . . ?
C18 C17 C16 119.0(6) . . ?
C18 O6 C36 117.2(6) . . ?
C3 C2 C1 119.2(6) . . ?
C18 C19 C14 118.4(6) . . ?
C31 C30 C35 115.1(7) . . ?
C31 C30 C22 123.8(6) . . ?
C35 C30 C22 121.1(7) . . ?
C28 C29 C26 120.2(7) . . ?
C28 C29 C27 118.3(7) . . ?
C26 C29 C27 121.4(7) . . ?
C3 C4 C5 118.0(7) . . ?
C16 C15 C14 119.3(6) . . ?
C16 C15 C20 118.8(6) . . ?
C14 C15 C20 121.8(5) . . ?
C30 C31 C32 124.0(7) . . ?
C34 C33 C32 118.6(8) . . ?
C17 C18 O6 115.6(6) . . ?
C17 C18 C19 122.0(6) . . ?
O6 C18 C19 122.4(6) . . ?
C17 C16 C15 121.5(6) . . ?
C25 C26 C29 118.5(8) . . ?
C2 C3 C4 119.6(7) . . ?
C34 C35 C30 120.6(8) . . ?
C23 C24 C25 119.1(8) . . ?
C33 C34 C35 122.2(8) . . ?
C33 C32 C31 119.2(8) . . ?
C24 C23 C28 122.1(9) . . ?
C26 C25 C24 121.8(9) . . ?
N3 C11 C10 122.7(7) . . ?
C9 C8 C7 118.0(7) . . ?
C11 C10 C9 117.1(7) . . ?
C8 C9 C10 121.1(7) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.083

_database_code_depnum_ccdc_archive 'CCDC 970058'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C35 H26 Br N3 Ni O5'
_chemical_formula_weight         707.18

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   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                   8.9775(6)
_cell_length_b                   17.6982(14)
_cell_length_c                   23.2372(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.817(4)
_cell_angle_gamma                90.00
_cell_volume                     3648.4(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1440
_exptl_absorpt_coefficient_mu    1.668
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15725
_diffrn_reflns_av_R_equivalents  0.0712
_diffrn_reflns_av_sigmaI/netI    0.1104
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.11
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6401
_reflns_number_gt                3646
_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)+(0.0950P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6401
_refine_ls_number_parameters     406
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1228
_refine_ls_R_factor_gt           0.0708
_refine_ls_wR_factor_ref         0.1968
_refine_ls_wR_factor_gt          0.1761
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_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
Br2 Br 0.56064(12) 0.22264(7) -0.13363(4) 0.1081(4) Uani 1 1 d . . .
Ni1 Ni 0.54129(7) 0.17991(4) 0.16048(3) 0.0353(2) Uani 1 1 d . . .
O1 O 0.7210(4) 0.1291(2) 0.12980(19) 0.0459(10) Uani 1 1 d . . .
O2 O 0.8656(5) 0.0940(3) 0.0658(2) 0.0672(13) Uani 1 1 d . . .
O3 O 0.6633(4) 0.26761(19) 0.19865(16) 0.0393(9) Uani 1 1 d . . .
O4 O 0.5168(4) 0.2544(2) 0.09054(17) 0.0449(10) Uani 1 1 d . . .
O5 O 0.7816(5) 0.4382(2) 0.1324(2) 0.0581(12) Uani 1 1 d . . .
N1 N 0.3910(5) 0.0897(2) 0.1294(2) 0.0393(11) Uani 1 1 d . . .
N2 N 0.5875(5) 0.1093(2) 0.2313(2) 0.0408(11) Uani 1 1 d . . .
N3 N 0.3371(4) 0.2193(2) 0.1826(2) 0.0382(11) Uani 1 1 d . . .
C1 C 0.5121(6) 0.0437(3) 0.2274(3) 0.0436(14) Uani 1 1 d . . .
C2 C 0.5471(8) -0.0137(3) 0.2671(3) 0.0616(19) Uani 1 1 d . . .
H2A H 0.4943 -0.0591 0.2632 0.074 Uiso 1 1 calc R . .
C3 C 0.6618(9) -0.0025(4) 0.3129(4) 0.078(2) Uani 1 1 d . . .
H3A H 0.6862 -0.0402 0.3406 0.093 Uiso 1 1 calc R . .
C4 C 0.7391(8) 0.0633(4) 0.3176(3) 0.0651(19) Uani 1 1 d . . .
H4A H 0.8176 0.0711 0.3481 0.078 Uiso 1 1 calc R . .
C5 C 0.6994(7) 0.1191(4) 0.2762(3) 0.0514(16) Uani 1 1 d . . .
H5A H 0.7516 0.1647 0.2797 0.062 Uiso 1 1 calc R . .
C6 C 0.3778(6) 0.0394(3) 0.1781(3) 0.0524(17) Uani 1 1 d . . .
H6A H 0.3679 -0.0121 0.1638 0.063 Uiso 1 1 calc R . .
H6B H 0.2866 0.0519 0.1936 0.063 Uiso 1 1 calc R . .
C7 C 0.2151(5) 0.1837(3) 0.1549(3) 0.0416(14) Uani 1 1 d . . .
C8 C 0.0727(6) 0.1972(3) 0.1685(3) 0.0491(16) Uani 1 1 d . . .
H8A H -0.0093 0.1695 0.1503 0.059 Uiso 1 1 calc R . .
C9 C 0.0524(7) 0.2511(4) 0.2087(3) 0.0562(17) Uani 1 1 d . . .
H9A H -0.0426 0.2607 0.2183 0.067 Uiso 1 1 calc R . .
C10 C 0.1790(7) 0.2917(4) 0.2351(3) 0.0567(17) Uani 1 1 d . . .
H10A H 0.1690 0.3299 0.2617 0.068 Uiso 1 1 calc R . .
C11 C 0.3186(7) 0.2739(3) 0.2209(3) 0.0473(15) Uani 1 1 d . . .
H11A H 0.4026 0.3007 0.2384 0.057 Uiso 1 1 calc R . .
C12 C 0.2447(6) 0.1280(3) 0.1097(3) 0.0443(15) Uani 1 1 d . . .
H12A H 0.1643 0.0909 0.1037 0.053 Uiso 1 1 calc R . .
H12B H 0.2480 0.1537 0.0731 0.053 Uiso 1 1 calc R . .
C13 C 0.4395(6) 0.0435(3) 0.0816(3) 0.0473(16) Uani 1 1 d . . .
H13A H 0.3610 0.0071 0.0681 0.057 Uiso 1 1 calc R . .
H13B H 0.5296 0.0155 0.0972 0.057 Uiso 1 1 calc R . .
C14 C 0.4712(6) 0.0894(3) 0.0311(3) 0.0435(15) Uani 1 1 d . . .
C15 C 0.3626(7) 0.0970(4) -0.0184(3) 0.0614(19) Uani 1 1 d . . .
H15A H 0.2689 0.0746 -0.0188 0.074 Uiso 1 1 calc R . .
C16 C 0.3898(9) 0.1368(4) -0.0669(3) 0.069(2) Uani 1 1 d . . .
H16A H 0.3142 0.1424 -0.0988 0.082 Uiso 1 1 calc R . .
C17 C 0.5275(9) 0.1675(4) -0.0674(3) 0.0630(19) Uani 1 1 d . . .
C18 C 0.6420(7) 0.1602(3) -0.0209(3) 0.0496(16) Uani 1 1 d . . .
H18A H 0.7364 0.1810 -0.0225 0.059 Uiso 1 1 calc R . .
C19 C 0.6143(6) 0.1212(3) 0.0286(3) 0.0437(14) Uani 1 1 d . . .
C20 C 0.7425(6) 0.1135(3) 0.0793(3) 0.0432(15) Uani 1 1 d . . .
C21 C 0.6792(6) 0.3217(3) 0.1618(3) 0.0366(13) Uani 1 1 d . . .
C22 C 0.7641(6) 0.3858(3) 0.1747(3) 0.0415(14) Uani 1 1 d . . .
C27 C 0.5983(6) 0.3113(3) 0.1031(3) 0.0415(14) Uani 1 1 d . . .
C28 C 0.7177(8) 0.4289(3) 0.0766(3) 0.0601(18) Uani 1 1 d . . .
C30 C 0.8468(6) 0.4083(3) 0.2314(3) 0.0415(14) Uani 1 1 d . . .
C31 C 0.8330(6) 0.3712(3) 0.2819(3) 0.0479(16) Uani 1 1 d . . .
H31A H 0.7699 0.3294 0.2800 0.058 Uiso 1 1 calc R . .
C32 C 0.9080(7) 0.3930(4) 0.3349(3) 0.0611(19) Uani 1 1 d . . .
H32A H 0.8953 0.3672 0.3686 0.073 Uiso 1 1 calc R . .
C33 C 1.0061(7) 0.4564(4) 0.3370(4) 0.070(2) Uani 1 1 d . . .
H33A H 1.0588 0.4722 0.3725 0.084 Uiso 1 1 calc R . .
C34 C 1.0226(8) 0.4924(4) 0.2896(4) 0.069(2) Uani 1 1 d . . .
H34A H 1.0877 0.5335 0.2917 0.083 Uiso 1 1 calc R . .
C35 C 0.9455(7) 0.4706(3) 0.2367(3) 0.0619(19) Uani 1 1 d . . .
H35A H 0.9587 0.4975 0.2035 0.074 Uiso 1 1 calc R . .
C24 C 0.5876(11) 0.4113(5) -0.0400(4) 0.093(3) Uani 1 1 d . . .
H24A H 0.5444 0.4068 -0.0789 0.112 Uiso 1 1 calc R . .
C29 C 0.7488(10) 0.4819(4) 0.0364(4) 0.085(3) Uani 1 1 d . . .
H29A H 0.8114 0.5227 0.0480 0.102 Uiso 1 1 calc R . .
C26 C 0.6212(7) 0.3661(3) 0.0589(3) 0.0534(16) Uani 1 1 d . . .
C25 C 0.6868(12) 0.4734(5) -0.0206(5) 0.105(3) Uani 1 1 d . . .
H25A H 0.7089 0.5087 -0.0477 0.126 Uiso 1 1 calc R . .
C23 C 0.5595(8) 0.3597(4) 0.0000(3) 0.0664(19) Uani 1 1 d . . .
H23A H 0.4972 0.3189 -0.0120 0.080 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br2 C17 1.883(7) . ?
Ni1 O3 2.025(3) . ?
Ni1 N2 2.058(5) . ?
Ni1 O1 2.067(4) . ?
Ni1 O4 2.078(4) . ?
Ni1 N3 2.097(4) . ?
Ni1 N1 2.143(4) . ?
O1 C20 1.248(7) . ?
O2 C20 1.244(6) . ?
O3 C21 1.308(6) . ?
O4 C27 1.253(6) . ?
O5 C28 1.345(8) . ?
O5 C22 1.378(7) . ?
N1 C6 1.459(7) . ?
N1 C12 1.486(6) . ?
N1 C13 1.497(7) . ?
N2 C5 1.344(7) . ?
N2 C1 1.340(7) . ?
N3 C11 1.342(7) . ?
N3 C7 1.339(6) . ?
C1 C2 1.376(8) . ?
C1 C6 1.533(8) . ?
C2 C3 1.376(10) . ?
C3 C4 1.351(10) . ?
C4 C5 1.385(9) . ?
C7 C8 1.384(7) . ?
C7 C12 1.495(8) . ?
C8 C9 1.366(8) . ?
C9 C10 1.403(8) . ?
C10 C11 1.380(8) . ?
C13 C14 1.491(8) . ?
C14 C15 1.395(9) . ?
C14 C19 1.412(8) . ?
C15 C16 1.382(10) . ?
C16 C17 1.353(10) . ?
C17 C18 1.379(9) . ?
C18 C19 1.396(8) . ?
C19 C20 1.522(8) . ?
C21 C22 1.374(7) . ?
C21 C27 1.455(8) . ?
C22 C30 1.465(8) . ?
C27 C26 1.449(8) . ?
C28 C29 1.383(9) . ?
C28 C26 1.432(9) . ?
C30 C31 1.365(8) . ?
C30 C35 1.407(8) . ?
C31 C32 1.365(8) . ?
C32 C33 1.422(9) . ?
C33 C34 1.299(10) . ?
C34 C35 1.373(9) . ?
C24 C23 1.354(10) . ?
C24 C25 1.443(12) . ?
C29 C25 1.362(11) . ?
C26 C23 1.398(9) . ?

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
O3 Ni1 N2 94.94(17) . . ?
O3 Ni1 O1 94.94(15) . . ?
N2 Ni1 O1 86.52(16) . . ?
O3 Ni1 O4 80.88(14) . . ?
N2 Ni1 O4 174.36(16) . . ?
O1 Ni1 O4 90.05(16) . . ?
O3 Ni1 N3 94.17(15) . . ?
N2 Ni1 N3 94.73(18) . . ?
O1 Ni1 N3 170.66(16) . . ?
O4 Ni1 N3 89.38(16) . . ?
O3 Ni1 N1 171.66(16) . . ?
N2 Ni1 N1 81.76(18) . . ?
O1 Ni1 N1 92.51(16) . . ?
O4 Ni1 N1 102.89(16) . . ?
N3 Ni1 N1 78.53(16) . . ?
C20 O1 Ni1 131.4(4) . . ?
C21 O3 Ni1 112.4(3) . . ?
C27 O4 Ni1 109.9(4) . . ?
C28 O5 C22 121.8(4) . . ?
C6 N1 C12 110.1(4) . . ?
C6 N1 C13 108.0(4) . . ?
C12 N1 C13 111.4(4) . . ?
C6 N1 Ni1 108.4(3) . . ?
C12 N1 Ni1 104.2(3) . . ?
C13 N1 Ni1 114.7(3) . . ?
C5 N2 C1 118.3(5) . . ?
C5 N2 Ni1 125.3(4) . . ?
C1 N2 Ni1 115.7(4) . . ?
C11 N3 C7 118.8(5) . . ?
C11 N3 Ni1 127.1(4) . . ?
C7 N3 Ni1 114.1(4) . . ?
N2 C1 C2 122.2(6) . . ?
N2 C1 C6 115.1(5) . . ?
C2 C1 C6 122.5(5) . . ?
C1 C2 C3 118.5(6) . . ?
C4 C3 C2 120.1(7) . . ?
C3 C4 C5 118.9(7) . . ?
N2 C5 C4 121.9(6) . . ?
N1 C6 C1 113.7(4) . . ?
N3 C7 C8 121.7(5) . . ?
N3 C7 C12 115.3(5) . . ?
C8 C7 C12 123.0(5) . . ?
C9 C8 C7 120.1(5) . . ?
C8 C9 C10 118.2(6) . . ?
C11 C10 C9 118.9(6) . . ?
N3 C11 C10 122.1(5) . . ?
N1 C12 C7 109.2(4) . . ?
N1 C13 C14 113.5(4) . . ?
C15 C14 C19 116.9(6) . . ?
C15 C14 C13 120.5(6) . . ?
C19 C14 C13 122.3(5) . . ?
C16 C15 C14 122.2(7) . . ?
C17 C16 C15 119.2(7) . . ?
C16 C17 C18 121.8(7) . . ?
C16 C17 Br2 118.3(6) . . ?
C18 C17 Br2 119.8(6) . . ?
C19 C18 C17 119.1(6) . . ?
C18 C19 C14 120.6(5) . . ?
C18 C19 C20 118.3(5) . . ?
C14 C19 C20 121.2(5) . . ?
O2 C20 O1 124.8(5) . . ?
O2 C20 C19 115.1(6) . . ?
O1 C20 C19 120.0(5) . . ?
O3 C21 C22 125.0(5) . . ?
O3 C21 C27 115.7(4) . . ?
C22 C21 C27 119.4(5) . . ?
C21 C22 O5 121.3(5) . . ?
C21 C22 C30 127.5(5) . . ?
O5 C22 C30 111.2(5) . . ?
O4 C27 C26 120.9(5) . . ?
O4 C27 C21 120.6(5) . . ?
C26 C27 C21 118.4(5) . . ?
O5 C28 C29 117.9(6) . . ?
O5 C28 C26 121.6(6) . . ?
C29 C28 C26 120.5(7) . . ?
C31 C30 C35 116.2(6) . . ?
C31 C30 C22 122.8(5) . . ?
C35 C30 C22 121.1(6) . . ?
C30 C31 C32 122.8(6) . . ?
C31 C32 C33 118.1(7) . . ?
C34 C33 C32 120.6(7) . . ?
C33 C34 C35 120.9(7) . . ?
C34 C35 C30 121.5(7) . . ?
C23 C24 C25 118.0(8) . . ?
C25 C29 C28 119.2(7) . . ?
C23 C26 C28 118.4(6) . . ?
C23 C26 C27 124.2(6) . . ?
C28 C26 C27 117.4(6) . . ?
C29 C25 C24 121.9(7) . . ?
C24 C23 C26 122.0(7) . . ?

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
O3 Ni1 O1 C20 -119.9(5) . . . . ?
N2 Ni1 O1 C20 145.4(5) . . . . ?
O4 Ni1 O1 C20 -39.0(5) . . . . ?
N3 Ni1 O1 C20 47.4(13) . . . . ?
N1 Ni1 O1 C20 63.9(5) . . . . ?
N2 Ni1 O3 C21 170.1(3) . . . . ?
O1 Ni1 O3 C21 83.2(3) . . . . ?
O4 Ni1 O3 C21 -6.0(3) . . . . ?
N3 Ni1 O3 C21 -94.7(3) . . . . ?
N1 Ni1 O3 C21 -123.6(11) . . . . ?
O3 Ni1 O4 C27 6.8(4) . . . . ?
N2 Ni1 O4 C27 -35.7(18) . . . . ?
O1 Ni1 O4 C27 -88.2(4) . . . . ?
N3 Ni1 O4 C27 101.1(4) . . . . ?
N1 Ni1 O4 C27 179.2(4) . . . . ?
O3 Ni1 N1 C6 -54.3(12) . . . . ?
N2 Ni1 N1 C6 12.9(3) . . . . ?
O1 Ni1 N1 C6 99.0(3) . . . . ?
O4 Ni1 N1 C6 -170.4(3) . . . . ?
N3 Ni1 N1 C6 -83.7(3) . . . . ?
O3 Ni1 N1 C12 63.0(12) . . . . ?
N2 Ni1 N1 C12 130.1(4) . . . . ?
O1 Ni1 N1 C12 -143.7(4) . . . . ?
O4 Ni1 N1 C12 -53.1(4) . . . . ?
N3 Ni1 N1 C12 33.6(4) . . . . ?
O3 Ni1 N1 C13 -175.0(9) . . . . ?
N2 Ni1 N1 C13 -107.8(4) . . . . ?
O1 Ni1 N1 C13 -21.7(4) . . . . ?
O4 Ni1 N1 C13 68.9(4) . . . . ?
N3 Ni1 N1 C13 155.6(4) . . . . ?
O3 Ni1 N2 C5 -16.7(5) . . . . ?
O1 Ni1 N2 C5 77.9(5) . . . . ?
O4 Ni1 N2 C5 25.3(19) . . . . ?
N3 Ni1 N2 C5 -111.4(5) . . . . ?
N1 Ni1 N2 C5 171.0(5) . . . . ?
O3 Ni1 N2 C1 172.9(4) . . . . ?
O1 Ni1 N2 C1 -92.5(4) . . . . ?
O4 Ni1 N2 C1 -145.1(16) . . . . ?
N3 Ni1 N2 C1 78.3(4) . . . . ?
N1 Ni1 N2 C1 0.6(4) . . . . ?
O3 Ni1 N3 C11 -13.4(5) . . . . ?
N2 Ni1 N3 C11 81.9(5) . . . . ?
O1 Ni1 N3 C11 179(47) . . . . ?
O4 Ni1 N3 C11 -94.2(5) . . . . ?
N1 Ni1 N3 C11 162.5(5) . . . . ?
O3 Ni1 N3 C7 167.4(4) . . . . ?
N2 Ni1 N3 C7 -97.3(4) . . . . ?
O1 Ni1 N3 C7 0.1(13) . . . . ?
O4 Ni1 N3 C7 86.6(4) . . . . ?
N1 Ni1 N3 C7 -16.7(4) . . . . ?
C5 N2 C1 C2 -1.0(9) . . . . ?
Ni1 N2 C1 C2 170.1(5) . . . . ?
C5 N2 C1 C6 175.0(5) . . . . ?
Ni1 N2 C1 C6 -13.9(6) . . . . ?
N2 C1 C2 C3 1.1(10) . . . . ?
C6 C1 C2 C3 -174.6(6) . . . . ?
C1 C2 C3 C4 -1.0(11) . . . . ?
C2 C3 C4 C5 0.9(11) . . . . ?
C1 N2 C5 C4 0.8(9) . . . . ?
Ni1 N2 C5 C4 -169.4(5) . . . . ?
C3 C4 C5 N2 -0.7(10) . . . . ?
C12 N1 C6 C1 -136.7(5) . . . . ?
C13 N1 C6 C1 101.4(6) . . . . ?
Ni1 N1 C6 C1 -23.4(6) . . . . ?
N2 C1 C6 N1 25.7(7) . . . . ?
C2 C1 C6 N1 -158.3(6) . . . . ?
C11 N3 C7 C8 -5.8(8) . . . . ?
Ni1 N3 C7 C8 173.4(4) . . . . ?
C11 N3 C7 C12 175.4(5) . . . . ?
Ni1 N3 C7 C12 -5.4(6) . . . . ?
N3 C7 C8 C9 3.9(9) . . . . ?
C12 C7 C8 C9 -177.4(6) . . . . ?
C7 C8 C9 C10 0.1(10) . . . . ?
C8 C9 C10 C11 -2.0(10) . . . . ?
C7 N3 C11 C10 3.8(9) . . . . ?
Ni1 N3 C11 C10 -175.4(4) . . . . ?
C9 C10 C11 N3 0.1(10) . . . . ?
C6 N1 C12 C7 70.3(6) . . . . ?
C13 N1 C12 C7 -170.0(4) . . . . ?
Ni1 N1 C12 C7 -45.8(5) . . . . ?
N3 C7 C12 N1 35.7(7) . . . . ?
C8 C7 C12 N1 -143.0(5) . . . . ?
C6 N1 C13 C14 -174.6(5) . . . . ?
C12 N1 C13 C14 64.3(6) . . . . ?
Ni1 N1 C13 C14 -53.7(5) . . . . ?
N1 C13 C14 C15 -98.0(6) . . . . ?
N1 C13 C14 C19 87.7(6) . . . . ?
C19 C14 C15 C16 -3.1(9) . . . . ?
C13 C14 C15 C16 -177.6(6) . . . . ?
C14 C15 C16 C17 2.2(10) . . . . ?
C15 C16 C17 C18 0.1(10) . . . . ?
C15 C16 C17 Br2 -179.1(5) . . . . ?
C16 C17 C18 C19 -1.2(9) . . . . ?
Br2 C17 C18 C19 178.0(4) . . . . ?
C17 C18 C19 C14 0.2(8) . . . . ?
C17 C18 C19 C20 179.7(5) . . . . ?
C15 C14 C19 C18 1.8(8) . . . . ?
C13 C14 C19 C18 176.3(5) . . . . ?
C15 C14 C19 C20 -177.7(5) . . . . ?
C13 C14 C19 C20 -3.2(8) . . . . ?
Ni1 O1 C20 O2 167.7(4) . . . . ?
Ni1 O1 C20 C19 -9.6(8) . . . . ?
C18 C19 C20 O2 -46.5(7) . . . . ?
C14 C19 C20 O2 133.1(6) . . . . ?
C18 C19 C20 O1 131.1(6) . . . . ?
C14 C19 C20 O1 -49.4(7) . . . . ?
Ni1 O3 C21 C22 -175.8(4) . . . . ?
Ni1 O3 C21 C27 4.5(5) . . . . ?
O3 C21 C22 O5 176.3(5) . . . . ?
C27 C21 C22 O5 -4.0(8) . . . . ?
O3 C21 C22 C30 -3.0(9) . . . . ?
C27 C21 C22 C30 176.7(5) . . . . ?
C28 O5 C22 C21 -0.5(8) . . . . ?
C28 O5 C22 C30 178.9(5) . . . . ?
Ni1 O4 C27 C26 169.8(4) . . . . ?
Ni1 O4 C27 C21 -6.6(6) . . . . ?
O3 C21 C27 O4 1.7(7) . . . . ?
C22 C21 C27 O4 -178.0(5) . . . . ?
O3 C21 C27 C26 -174.9(5) . . . . ?
C22 C21 C27 C26 5.4(8) . . . . ?
C22 O5 C28 C29 -176.0(6) . . . . ?
C22 O5 C28 C26 3.5(9) . . . . ?
C21 C22 C30 C31 -9.0(9) . . . . ?
O5 C22 C30 C31 171.6(5) . . . . ?
C21 C22 C30 C35 171.4(6) . . . . ?
O5 C22 C30 C35 -8.0(7) . . . . ?
C35 C30 C31 C32 0.9(8) . . . . ?
C22 C30 C31 C32 -178.8(5) . . . . ?
C30 C31 C32 C33 -1.0(9) . . . . ?
C31 C32 C33 C34 0.3(10) . . . . ?
C32 C33 C34 C35 0.4(11) . . . . ?
C33 C34 C35 C30 -0.5(11) . . . . ?
C31 C30 C35 C34 -0.1(9) . . . . ?
C22 C30 C35 C34 179.5(6) . . . . ?
O5 C28 C29 C25 179.4(8) . . . . ?
C26 C28 C29 C25 -0.2(12) . . . . ?
O5 C28 C26 C23 -179.6(6) . . . . ?
C29 C28 C26 C23 -0.1(10) . . . . ?
O5 C28 C26 C27 -1.8(9) . . . . ?
C29 C28 C26 C27 177.7(6) . . . . ?
O4 C27 C26 C23 -1.5(9) . . . . ?
C21 C27 C26 C23 175.0(6) . . . . ?
O4 C27 C26 C28 -179.1(6) . . . . ?
C21 C27 C26 C28 -2.6(8) . . . . ?
C28 C29 C25 C24 0.8(14) . . . . ?
C23 C24 C25 C29 -1.3(14) . . . . ?
C25 C24 C23 C26 1.1(13) . . . . ?
C28 C26 C23 C24 -0.5(11) . . . . ?
C27 C26 C23 C24 -178.0(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.734
_refine_diff_density_min         -1.150
_refine_diff_density_rms         0.090

# SQUEEZE RESULTS (APPEND TO CIF) 
# Note: Data are Listed for all Voids in the P1 Unit Cell 
# i.e. Centre of Gravity, Solvent Accessible Volume, 
# Recovered number of Electrons in the Void and 
# Details about the Squeezed Material 
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.090 0.301 0.952 225 49 ' '
2 0.090 0.198 0.452 225 49 ' '
3 -0.091 0.805 0.549 223 48 ' '
4 -0.091 0.695 0.049 223 47 ' '
_platon_squeeze_details          
; 
;

_database_code_depnum_ccdc_archive 'CCDC 970057'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C35 H28 N4 Ni O8'
_chemical_formula_weight         691.32

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   P2(1)

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

_cell_length_a                   8.813(2)
_cell_length_b                   17.454(5)
_cell_length_c                   11.745(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.292(4)
_cell_angle_gamma                90.00
_cell_volume                     1782.9(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow-green
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             716
_exptl_absorpt_coefficient_mu    0.598
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10703
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0709
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.76
_diffrn_reflns_theta_max         26.00
_reflns_number_total             6644
_reflns_number_gt                5000
_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)+(0.1189P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(2)
_refine_ls_number_reflns         6644
_refine_ls_number_parameters     430
_refine_ls_number_restraints     73
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0664
_refine_ls_wR_factor_ref         0.1883
_refine_ls_wR_factor_gt          0.1748
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_restrained_S_all      1.027
_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 0.08368(7) 0.24749(4) 0.37684(5) 0.0517(2) Uani 1 1 d . . .
C7 C -0.2454(6) 0.2488(4) 0.3827(4) 0.0561(11) Uani 1 1 d . . .
N1 N -0.0759(5) 0.3204(3) 0.2752(4) 0.0523(10) Uani 1 1 d . . .
O4 O 0.0248(6) 0.1488(3) 0.2835(5) 0.0795(13) Uani 1 1 d . . .
C8 C -0.3887(6) 0.2360(4) 0.4138(6) 0.0680(16) Uani 1 1 d . . .
H8A H -0.4783 0.2497 0.3648 0.082 Uiso 1 1 calc R . .
O3 O 0.2129(5) 0.1734(3) 0.4821(4) 0.0733(13) Uani 1 1 d . . .
C21 C 0.1956(8) 0.1028(3) 0.4372(7) 0.0703(15) Uani 1 1 d U . .
N12 N 0.1449(6) 0.3476(3) 0.4660(4) 0.0544(11) Uani 1 1 d . . .
C2 C 0.1094(9) 0.4821(4) 0.4617(6) 0.0699(16) Uani 1 1 d . . .
H2A H 0.0563 0.5249 0.4291 0.084 Uiso 1 1 calc R . .
C1 C 0.0649(7) 0.4092(3) 0.4235(5) 0.0563(14) Uani 1 1 d . . .
N3 N -0.1135(5) 0.2291(2) 0.4517(4) 0.0591(12) Uani 1 1 d . . .
C3 C 0.2342(12) 0.4904(5) 0.5491(7) 0.096(3) Uani 1 1 d . . .
H3A H 0.2633 0.5386 0.5783 0.115 Uiso 1 1 calc R . .
C5 C 0.2670(8) 0.3560(4) 0.5469(6) 0.0730(17) Uani 1 1 d . . .
H12A H 0.3232 0.3129 0.5745 0.088 Uiso 1 1 calc R . .
C27 C 0.0962(9) 0.0936(4) 0.3305(7) 0.0730(15) Uani 1 1 d U . .
C6 C -0.0793(7) 0.3935(3) 0.3402(5) 0.0602(14) Uani 1 1 d . . .
H6A H -0.1652 0.3920 0.3824 0.072 Uiso 1 1 calc R . .
H6B H -0.0969 0.4354 0.2856 0.072 Uiso 1 1 calc R . .
C12 C -0.2257(7) 0.2814(4) 0.2674(5) 0.0666(15) Uani 1 1 d . . .
H12B H -0.2321 0.2405 0.2110 0.080 Uiso 1 1 calc R . .
H12C H -0.3078 0.3176 0.2421 0.080 Uiso 1 1 calc R . .
C13 C -0.0369(7) 0.3396(3) 0.1595(5) 0.0599(14) Uani 1 1 d . . .
H13A H 0.0566 0.3699 0.1699 0.072 Uiso 1 1 calc R . .
H13B H -0.1186 0.3708 0.1178 0.072 Uiso 1 1 calc R . .
C4 C 0.3133(10) 0.4272(5) 0.5915(6) 0.085(2) Uani 1 1 d . . .
H21A H 0.3977 0.4316 0.6499 0.102 Uiso 1 1 calc R . .
O5 O 0.2535(8) -0.0323(3) 0.4415(6) 0.1086(18) Uani 1 1 d U . .
C29 C 0.0710(12) 0.0151(4) 0.2801(8) 0.095(3) Uani 1 1 d . . .
C22 C 0.2726(10) 0.0398(4) 0.4954(8) 0.0920(17) Uani 1 1 d U . .
O1 O 0.2571(4) 0.2736(2) 0.2834(3) 0.0602(10) Uani 1 1 d . . .
C15 C 0.1320(7) 0.2333(4) 0.0967(5) 0.0626(16) Uani 1 1 d . . .
C20 C 0.2726(7) 0.2598(5) 0.1802(5) 0.0726(18) Uani 1 1 d . . .
C14 C -0.0143(7) 0.2689(3) 0.0874(5) 0.0626(15) Uani 1 1 d . . .
C16 C 0.1506(8) 0.1713(4) 0.0252(6) 0.0724(17) Uani 1 1 d . . .
H16A H 0.2463 0.1487 0.0264 0.087 Uiso 1 1 calc R . .
C17 C 0.0211(8) 0.1442(4) -0.0482(5) 0.0673(16) Uani 1 1 d . . .
C18 C -0.1177(9) 0.1760(5) -0.0569(6) 0.082(2) Uani 1 1 d . . .
H18A H -0.2007 0.1557 -0.1067 0.098 Uiso 1 1 calc R . .
C28 C 0.1434(17) -0.0427(5) 0.3341(10) 0.126(3) Uani 1 1 d U . .
O2 O 0.3899(5) 0.2687(4) 0.1400(4) 0.106(2) Uani 1 1 d . . .
O7 O 0.1581(9) 0.0364(5) -0.0954(7) 0.140(3) Uani 1 1 d . . .
N4 N 0.0402(11) 0.0741(5) -0.1179(6) 0.099(2) Uani 1 1 d . . .
O6 O -0.0613(10) 0.0580(6) -0.1924(8) 0.169(4) Uani 1 1 d . . .
C10 C -0.2627(8) 0.1802(4) 0.5889(6) 0.0724(17) Uani 1 1 d . . .
H10A H -0.2665 0.1545 0.6577 0.087 Uiso 1 1 calc R . .
C9 C -0.3947(8) 0.2027(4) 0.5189(7) 0.0780(18) Uani 1 1 d . . .
H9A H -0.4892 0.1953 0.5428 0.094 Uiso 1 1 calc R . .
C11 C -0.1244(8) 0.1966(3) 0.5546(5) 0.0668(16) Uani 1 1 d . . .
H11A H -0.0343 0.1848 0.6043 0.080 Uiso 1 1 calc R . .
C19 C -0.1366(7) 0.2414(5) 0.0110(5) 0.0757(16) Uani 1 1 d . . .
H19A H -0.2317 0.2656 0.0039 0.091 Uiso 1 1 calc R . .
C26 C -0.0245(14) 0.0007(5) 0.1804(8) 0.115(4) Uani 1 1 d U . .
H26A H -0.0760 0.0405 0.1377 0.138 Uiso 1 1 calc R . .
C30 C 0.3703(6) 0.0350(4) 0.6020(5) 0.101(2) Uani 1 1 d GU . .
C31 C 0.3728(7) 0.0931(3) 0.6832(6) 0.104(2) Uani 1 1 d GU . .
H31A H 0.3138 0.1370 0.6655 0.125 Uiso 1 1 calc R . .
C32 C 0.4634(9) 0.0856(5) 0.7911(6) 0.159(5) Uani 1 1 d G . .
H32A H 0.4650 0.1245 0.8455 0.191 Uiso 1 1 calc R . .
C33 C 0.5515(7) 0.0200(6) 0.8176(7) 0.167(6) Uani 1 1 d GU . .
H33A H 0.6121 0.0150 0.8898 0.201 Uiso 1 1 calc R . .
C34 C 0.5490(7) -0.0380(5) 0.7364(9) 0.155(6) Uani 1 1 d GU . .
H34A H 0.6080 -0.0819 0.7541 0.186 Uiso 1 1 calc R . .
C35 C 0.4584(8) -0.0305(3) 0.6285(8) 0.148(5) Uani 1 1 d GU . .
H35A H 0.4568 -0.0694 0.5741 0.177 Uiso 1 1 calc R . .
C23 C 0.119(2) -0.1182(5) 0.2979(12) 0.151(5) Uani 1 1 d U . .
H23A H 0.1690 -0.1572 0.3432 0.182 Uiso 1 1 calc R . .
C24 C 0.027(2) -0.1361(7) 0.2012(15) 0.177(6) Uani 1 1 d U . .
H24A H 0.0134 -0.1866 0.1764 0.213 Uiso 1 1 calc R . .
C25 C -0.045(2) -0.0786(10) 0.1411(13) 0.161(6) Uani 1 1 d U . .
H25A H -0.1101 -0.0891 0.0723 0.194 Uiso 1 1 calc R . .
O9 O 0.4773(19) 0.2892(18) -0.0816(18) 0.236(12) Uani 0.50 1 d PU . .
O8 O 0.546(3) 0.0925(13) 0.171(2) 0.254(13) Uani 0.50 1 d PU . .


_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 O3 2.011(4) . ?
Ni1 O4 2.062(5) . ?
Ni1 N12 2.064(5) . ?
Ni1 O1 2.071(4) . ?
Ni1 N3 2.095(5) . ?
Ni1 N1 2.117(5) . ?
C7 N3 1.350(7) . ?
C7 C8 1.389(8) . ?
C7 C12 1.504(8) . ?
N1 C12 1.474(8) . ?
N1 C6 1.490(7) . ?
N1 C13 1.492(7) . ?
O4 C27 1.231(9) . ?
C8 C9 1.374(9) . ?
O3 C21 1.339(9) . ?
C21 C22 1.409(9) . ?
C21 C27 1.417(10) . ?
N12 C5 1.323(8) . ?
N12 C1 1.338(7) . ?
C2 C3 1.386(11) . ?
C2 C1 1.384(8) . ?
C1 C6 1.498(9) . ?
N3 C11 1.353(7) . ?
C3 C4 1.356(12) . ?
C5 C4 1.384(10) . ?
C27 C29 1.496(10) . ?
C13 C14 1.528(8) . ?
O5 C22 1.407(11) . ?
O5 C28 1.473(15) . ?
C29 C28 1.302(14) . ?
C29 C26 1.350(14) . ?
C22 C30 1.402(11) . ?
O1 C20 1.264(7) . ?
C15 C16 1.395(8) . ?
C15 C14 1.419(8) . ?
C15 C20 1.523(8) . ?
C20 O2 1.213(7) . ?
C14 C19 1.373(9) . ?
C16 C17 1.396(9) . ?
C17 C18 1.332(10) . ?
C17 N4 1.497(10) . ?
C18 C19 1.418(11) . ?
C28 C23 1.390(14) . ?
O7 N4 1.222(11) . ?
N4 O6 1.179(9) . ?
C10 C9 1.368(10) . ?
C10 C11 1.374(9) . ?
C26 C25 1.462(17) . ?
C30 C31 1.3900 . ?
C30 C35 1.3900 . ?
C31 C32 1.3900 . ?
C32 C33 1.3900 . ?
C33 C34 1.3900 . ?
C34 C35 1.3900 . ?
C23 C24 1.32(2) . ?
C24 C25 1.33(2) . ?

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
O3 Ni1 O4 81.9(2) . . ?
O3 Ni1 N12 99.0(2) . . ?
O4 Ni1 N12 178.3(2) . . ?
O3 Ni1 O1 94.26(17) . . ?
O4 Ni1 O1 92.63(17) . . ?
N12 Ni1 O1 85.88(17) . . ?
O3 Ni1 N3 93.97(18) . . ?
O4 Ni1 N3 86.60(19) . . ?
N12 Ni1 N3 94.76(19) . . ?
O1 Ni1 N3 171.54(17) . . ?
O3 Ni1 N1 172.82(19) . . ?
O4 Ni1 N1 96.6(2) . . ?
N12 Ni1 N1 82.69(18) . . ?
O1 Ni1 N1 92.81(17) . . ?
N3 Ni1 N1 78.93(18) . . ?
N3 C7 C8 122.2(5) . . ?
N3 C7 C12 115.1(4) . . ?
C8 C7 C12 122.7(5) . . ?
C12 N1 C6 109.6(5) . . ?
C12 N1 C13 112.5(5) . . ?
C6 N1 C13 107.5(4) . . ?
C12 N1 Ni1 105.3(4) . . ?
C6 N1 Ni1 107.0(3) . . ?
C13 N1 Ni1 114.8(3) . . ?
C27 O4 Ni1 110.4(5) . . ?
C9 C8 C7 118.2(6) . . ?
C21 O3 Ni1 109.4(4) . . ?
O3 C21 C22 120.7(8) . . ?
O3 C21 C27 117.8(5) . . ?
C22 C21 C27 121.4(7) . . ?
C5 N12 C1 119.9(5) . . ?
C5 N12 Ni1 125.0(4) . . ?
C1 N12 Ni1 114.3(4) . . ?
C3 C2 C1 119.0(7) . . ?
N12 C1 C2 120.9(6) . . ?
N12 C1 C6 115.9(5) . . ?
C2 C1 C6 123.1(5) . . ?
C7 N3 C11 117.7(5) . . ?
C7 N3 Ni1 113.7(3) . . ?
C11 N3 Ni1 128.5(4) . . ?
C4 C3 C2 119.1(7) . . ?
N12 C5 C4 121.8(7) . . ?
O4 C27 C21 120.4(6) . . ?
O4 C27 C29 120.5(8) . . ?
C21 C27 C29 119.0(7) . . ?
N1 C6 C1 114.0(5) . . ?
N1 C12 C7 110.6(5) . . ?
N1 C13 C14 113.1(5) . . ?
C3 C4 C5 119.3(7) . . ?
C22 O5 C28 120.7(6) . . ?
C28 C29 C26 117.8(9) . . ?
C28 C29 C27 119.2(10) . . ?
C26 C29 C27 123.0(8) . . ?
C30 C22 O5 111.1(6) . . ?
C30 C22 C21 131.1(8) . . ?
O5 C22 C21 117.8(8) . . ?
C20 O1 Ni1 132.0(4) . . ?
C16 C15 C14 119.1(6) . . ?
C16 C15 C20 117.5(6) . . ?
C14 C15 C20 123.4(5) . . ?
O2 C20 O1 125.4(6) . . ?
O2 C20 C15 116.4(5) . . ?
O1 C20 C15 118.2(5) . . ?
C19 C14 C15 120.3(6) . . ?
C19 C14 C13 119.1(6) . . ?
C15 C14 C13 120.6(5) . . ?
C17 C16 C15 118.1(6) . . ?
C18 C17 C16 123.7(6) . . ?
C18 C17 N4 118.8(7) . . ?
C16 C17 N4 117.5(7) . . ?
C17 C18 C19 118.8(6) . . ?
C29 C28 C23 123.1(14) . . ?
C29 C28 O5 121.6(8) . . ?
C23 C28 O5 115.2(11) . . ?
O6 N4 O7 123.2(8) . . ?
O6 N4 C17 117.5(9) . . ?
O7 N4 C17 119.2(7) . . ?
C9 C10 C11 118.2(6) . . ?
C10 C9 C8 120.6(6) . . ?
N3 C11 C10 122.9(6) . . ?
C14 C19 C18 119.9(7) . . ?
C29 C26 C25 118.5(12) . . ?
C31 C30 C35 120.0 . . ?
C31 C30 C22 120.6(6) . . ?
C35 C30 C22 119.3(6) . . ?
C32 C31 C30 120.0 . . ?
C31 C32 C33 120.0 . . ?
C34 C33 C32 120.0 . . ?
C33 C34 C35 120.0 . . ?
C34 C35 C30 120.0 . . ?
C24 C23 C28 122.0(13) . . ?
C23 C24 C25 116.9(12) . . ?
C24 C25 C26 121.6(15) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.094


_database_code_depnum_ccdc_archive 'CCDC 970059'
