# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_complex_1
_database_code_depnum_ccdc_archive 'CCDC 1402077'
_audit_update_record             
;
2015-12-10 deposited with the CCDC.
2015-12-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H36 N4 Ni2 O2, 2(Cl O4)'
_chemical_formula_sum            'C21 H36 Cl2 N4 Ni2 O10'
_chemical_formula_weight         692.86

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

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

_cell_length_a                   7.5074(6)
_cell_length_b                   15.9840(13)
_cell_length_c                   23.982(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.482(3)
_cell_angle_gamma                90.00
_cell_volume                     2859.4(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    295
_cell_measurement_reflns_used    32360
_cell_measurement_theta_min      1.53
_cell_measurement_theta_max      25.00

_exptl_crystal_description       needle
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1440
_exptl_absorpt_coefficient_mu    1.562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.615
_exptl_absorpt_correction_T_max  0.740
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      295
_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       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            32360
_diffrn_reflns_av_R_equivalents  0.0990
_diffrn_reflns_av_sigmaI/netI    0.0650
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.53
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4886
_reflns_number_gt                3285
_reflns_threshold_expression     I>2sigma(I)

_computing_data_collection       'Brucker SMART'
_computing_cell_refinement       'Brucker SMART'
_computing_data_reduction        'Brucker SAINT'
_computing_structure_solution    'SIR97(Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Diamond
_computing_publication_material  
'SHELXL-97 (Sheldrick, 1997), PLATON (Spek, 2009)'

_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)+(0.0797P)²+21.9136P] 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         4886
_refine_ls_number_parameters     356
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1263
_refine_ls_R_factor_gt           0.0863
_refine_ls_wR_factor_ref         0.2280
_refine_ls_wR_factor_gt          0.2066
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_restrained_S_all      1.116
_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 0.19870(16) 0.24264(7) 0.57207(4) 0.0369(3) Uani 1 1 d . . .
Ni2 Ni 0.16389(16) 0.10874(7) 0.65153(4) 0.0376(3) Uani 1 1 d . . .
O1 O 0.1923(9) 0.1265(4) 0.5741(2) 0.0445(16) Uani 1 1 d . . .
C1 C 0.2223(12) 0.0721(6) 0.5319(4) 0.037(2) Uani 1 1 d . . .
C2 C 0.2271(14) -0.0146(6) 0.5434(4) 0.047(2) Uani 1 1 d . . .
C3 C 0.2546(13) -0.0700(6) 0.4985(4) 0.051(3) Uani 1 1 d . . .
H3 H 0.2544 -0.1271 0.5058 0.061 Uiso 1 1 calc R . .
C4 C 0.2819(14) -0.0447(7) 0.4437(4) 0.055(3) Uani 1 1 d . . .
C5 C 0.2774(13) 0.0407(7) 0.4319(4) 0.052(3) Uani 1 1 d . . .
H5 H 0.2930 0.0598 0.3962 0.062 Uiso 1 1 calc R . .
C6 C 0.2479(12) 0.0997(6) 0.4764(4) 0.041(2) Uani 1 1 d . . .
C7 C 0.3169(16) -0.1081(7) 0.3961(4) 0.069(3) Uani 1 1 d . . .
H7A H 0.3162 -0.1641 0.4104 0.103 Uiso 1 1 calc R . .
H7B H 0.4314 -0.0965 0.3835 0.103 Uiso 1 1 calc R . .
H7C H 0.2246 -0.1023 0.3652 0.103 Uiso 1 1 calc R . .
C8 C 0.2473(12) 0.1872(6) 0.4609(4) 0.043(2) Uani 1 1 d . . .
H8 H 0.2630 0.2004 0.4240 0.051 Uiso 1 1 calc R . .
N1 N 0.2261(10) 0.2489(5) 0.4952(3) 0.0422(19) Uani 1 1 d . . .
C9 C 0.2186(15) 0.3346(6) 0.4738(4) 0.050(3) Uani 1 1 d . . .
H9A H 0.2867 0.3388 0.4418 0.060 Uiso 1 1 calc R . .
H9B H 0.0953 0.3498 0.4615 0.060 Uiso 1 1 calc R . .
C10 C 0.2913(14) 0.3901(6) 0.5170(4) 0.051(3) Uani 1 1 d . . .
H10A H 0.2591 0.4475 0.5074 0.062 Uiso 1 1 calc R . .
H10B H 0.4209 0.3857 0.5226 0.062 Uiso 1 1 calc R . .
N2 N 0.2065(11) 0.3622(5) 0.5731(3) 0.0441(19) Uani 1 1 d . . .
C11 C 0.0122(13) 0.3880(6) 0.5848(4) 0.048(2) Uani 1 1 d . . .
H11A H -0.0721 0.3653 0.5551 0.058 Uiso 1 1 calc R . .
H11B H -0.0124 0.3617 0.6196 0.058 Uiso 1 1 calc R . .
C12 C -0.0239(18) 0.4803(7) 0.5892(6) 0.080(4) Uani 1 1 d . . .
H12A H -0.1458 0.4887 0.5964 0.121 Uiso 1 1 calc R . .
H12B H -0.0044 0.5072 0.5546 0.121 Uiso 1 1 calc R . .
H12C H 0.0555 0.5037 0.6194 0.121 Uiso 1 1 calc R . .
C13 C 0.3142(15) 0.3969(6) 0.6172(4) 0.056(3) Uani 1 1 d . . .
H13A H 0.2656 0.3859 0.6522 0.068 Uiso 1 1 calc R . .
H13B H 0.3227 0.4569 0.6123 0.068 Uiso 1 1 calc R . .
C14 C 0.4967(16) 0.3569(8) 0.6175(5) 0.076(4) Uani 1 1 d . . .
H14A H 0.5765 0.3795 0.6479 0.113 Uiso 1 1 calc R . .
H14B H 0.5431 0.3682 0.5826 0.113 Uiso 1 1 calc R . .
H14C H 0.4863 0.2975 0.6224 0.113 Uiso 1 1 calc R . .
C15 C 0.1957(13) -0.0481(6) 0.5993(4) 0.052(3) Uani 1 1 d . . .
H15 H 0.1960 -0.1060 0.6027 0.063 Uiso 1 1 calc R . .
N3 N 0.1672(11) -0.0054(5) 0.6451(3) 0.045(2) Uani 1 1 d . . .
C16 C 0.1293(17) -0.0501(6) 0.6994(4) 0.060(3) Uani 1 1 d . . .
H16A H 0.0026 -0.0624 0.6989 0.072 Uiso 1 1 calc R . .
H16B H 0.1965 -0.1019 0.7044 0.072 Uiso 1 1 calc R . .
C17 C 0.1868(17) 0.0081(6) 0.7430(4) 0.059(3) Uani 1 1 d . . .
H17A H 0.3167 0.0072 0.7492 0.071 Uiso 1 1 calc R . .
H17B H 0.1423 -0.0104 0.7774 0.071 Uiso 1 1 calc R . .
N4 N 0.1278(10) 0.0950(5) 0.7317(3) 0.0419(19) Uani 1 1 d . . .
C18 C -0.0657(13) 0.1089(7) 0.7487(4) 0.049(3) Uani 1 1 d . . .
H18A H -0.1417 0.0710 0.7251 0.059 Uiso 1 1 calc R . .
H18B H -0.0992 0.1648 0.7357 0.059 Uiso 1 1 calc R . .
C19 C -0.1340(17) 0.1020(9) 0.8095(4) 0.078(4) Uani 1 1 d . . .
H19A H -0.2600 0.1141 0.8066 0.117 Uiso 1 1 calc R . .
H19B H -0.0699 0.1413 0.8345 0.117 Uiso 1 1 calc R . .
H19C H -0.1130 0.0463 0.8238 0.117 Uiso 1 1 calc R . .
C20 C 0.2334(13) 0.1555(7) 0.7638(4) 0.050(3) Uani 1 1 d . . .
H20A H 0.2483 0.1391 0.8030 0.060 Uiso 1 1 calc R . .
H20B H 0.1730 0.2093 0.7609 0.060 Uiso 1 1 calc R . .
C21 C 0.4245(15) 0.1637(8) 0.7417(5) 0.072(4) Uani 1 1 d . . .
H21A H 0.4947 0.2047 0.7636 0.108 Uiso 1 1 calc R . .
H21B H 0.4095 0.1806 0.7030 0.108 Uiso 1 1 calc R . .
H21C H 0.4846 0.1106 0.7450 0.108 Uiso 1 1 calc R . .
O2 O 0.1645(12) 0.2250(4) 0.6490(3) 0.055(2) Uani 1 1 d . . .
H2 H 0.092(15) 0.244(7) 0.672(5) 0.07(4) Uiso 1 1 d . . .
Cl1 Cl 0.2349(4) 0.19540(19) 0.92799(12) 0.0629(8) Uani 1 1 d . . .
O3 O 0.1115(14) 0.2550(6) 0.9131(6) 0.128(5) Uani 1 1 d . . .
O4 O 0.1633(15) 0.1163(6) 0.9178(5) 0.114(4) Uani 1 1 d . . .
O5 O 0.3989(14) 0.2064(9) 0.8963(4) 0.125(4) Uani 1 1 d . . .
O6 O 0.2506(17) 0.2027(9) 0.9847(4) 0.141(5) Uani 1 1 d . . .
Cl2 Cl -0.1303(4) 0.36702(18) 0.76209(12) 0.0593(7) Uani 1 1 d . . .
O7 O -0.1330(18) 0.4478(7) 0.7803(7) 0.167(6) Uani 1 1 d . . .
O8 O -0.240(2) 0.3568(17) 0.7241(7) 0.270(12) Uani 1 1 d . . .
O9 O 0.0421(11) 0.3433(6) 0.7382(4) 0.087(3) Uani 1 1 d . . .
O10 O -0.200(2) 0.3195(9) 0.8056(6) 0.171(6) 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 O1 1.858(6) . ?
Ni1 N1 1.881(8) . ?
Ni1 N2 1.911(8) . ?
Ni1 O2 1.913(7) . ?
Ni1 Ni2 2.8971(16) . ?
Ni2 N3 1.831(8) . ?
Ni2 O2 1.859(7) . ?
Ni2 O1 1.914(6) . ?
Ni2 N4 1.984(8) . ?
O1 C1 1.370(10) . ?
C1 C2 1.413(13) . ?
C1 C6 1.437(13) . ?
C2 C3 1.427(13) . ?
C2 C15 1.487(14) . ?
C3 C4 1.410(15) . ?
C3 H3 0.9300 . ?
C4 C5 1.393(15) . ?
C4 C7 1.572(13) . ?
C5 C6 1.460(13) . ?
C5 H5 0.9300 . ?
C6 C8 1.447(13) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 N1 1.304(12) . ?
C8 H8 0.9300 . ?
N1 C9 1.462(11) . ?
C9 C10 1.426(13) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.613(13) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
N2 C13 1.374(11) . ?
N2 C11 1.572(12) . ?
C11 C12 1.505(14) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.511(15) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 N3 1.331(12) . ?
C15 H15 0.9300 . ?
N3 C16 1.540(12) . ?
C16 C17 1.429(14) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 N4 1.474(12) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
N4 C20 1.421(12) . ?
N4 C18 1.569(12) . ?
C18 C19 1.603(14) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 C21 1.589(15) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
O2 H2 0.88(11) . ?
Cl1 O3 1.348(9) . ?
Cl1 O6 1.356(10) . ?
Cl1 O4 1.385(10) . ?
Cl1 O5 1.529(11) . ?
Cl2 O8 1.166(12) . ?
Cl2 O7 1.365(11) . ?
Cl2 O10 1.436(13) . ?
Cl2 O9 1.521(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
O1 Ni1 N1 94.8(3) . . ?
O1 Ni1 N2 177.8(3) . . ?
N1 Ni1 N2 87.3(3) . . ?
O1 Ni1 O2 79.7(3) . . ?
N1 Ni1 O2 174.4(3) . . ?
N2 Ni1 O2 98.2(3) . . ?
O1 Ni1 Ni2 40.54(18) . . ?
N1 Ni1 Ni2 135.4(2) . . ?
N2 Ni1 Ni2 137.3(2) . . ?
O2 Ni1 Ni2 39.1(2) . . ?
N3 Ni2 O2 173.2(3) . . ?
N3 Ni2 O1 93.6(3) . . ?
O2 Ni2 O1 79.6(3) . . ?
N3 Ni2 N4 88.6(3) . . ?
O2 Ni2 N4 98.2(3) . . ?
O1 Ni2 N4 177.4(3) . . ?
N3 Ni2 Ni1 132.7(3) . . ?
O2 Ni2 Ni1 40.5(2) . . ?
O1 Ni2 Ni1 39.13(18) . . ?
N4 Ni2 Ni1 138.7(2) . . ?
C1 O1 Ni1 127.4(6) . . ?
C1 O1 Ni2 131.9(6) . . ?
Ni1 O1 Ni2 100.3(3) . . ?
O1 C1 C2 118.8(8) . . ?
O1 C1 C6 122.7(8) . . ?
C2 C1 C6 118.6(8) . . ?
C1 C2 C3 117.6(9) . . ?
C1 C2 C15 121.7(8) . . ?
C3 C2 C15 120.6(9) . . ?
C4 C3 C2 125.0(10) . . ?
C4 C3 H3 117.5 . . ?
C2 C3 H3 117.5 . . ?
C5 C4 C3 117.9(9) . . ?
C5 C4 C7 119.1(10) . . ?
C3 C4 C7 123.1(10) . . ?
C4 C5 C6 119.1(10) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
C1 C6 C8 122.5(8) . . ?
C1 C6 C5 121.8(9) . . ?
C8 C6 C5 115.7(9) . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 C6 124.5(8) . . ?
N1 C8 H8 117.8 . . ?
C6 C8 H8 117.8 . . ?
C8 N1 C9 119.3(8) . . ?
C8 N1 Ni1 127.8(7) . . ?
C9 N1 Ni1 112.9(6) . . ?
C10 C9 N1 109.3(7) . . ?
C10 C9 H9A 109.8 . . ?
N1 C9 H9A 109.8 . . ?
C10 C9 H9B 109.8 . . ?
N1 C9 H9B 109.8 . . ?
H9A C9 H9B 108.3 . . ?
C9 C10 N2 106.2(8) . . ?
C9 C10 H10A 110.5 . . ?
N2 C10 H10A 110.5 . . ?
C9 C10 H10B 110.5 . . ?
N2 C10 H10B 110.5 . . ?
H10A C10 H10B 108.7 . . ?
C13 N2 C11 103.5(8) . . ?
C13 N2 C10 106.0(8) . . ?
C11 N2 C10 122.5(7) . . ?
C13 N2 Ni1 115.3(6) . . ?
C11 N2 Ni1 103.7(6) . . ?
C10 N2 Ni1 106.3(6) . . ?
C12 C11 N2 116.6(9) . . ?
C12 C11 H11A 108.1 . . ?
N2 C11 H11A 108.1 . . ?
C12 C11 H11B 108.1 . . ?
N2 C11 H11B 108.1 . . ?
H11A C11 H11B 107.3 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N2 C13 C14 106.7(9) . . ?
N2 C13 H13A 110.4 . . ?
C14 C13 H13A 110.4 . . ?
N2 C13 H13B 110.4 . . ?
C14 C13 H13B 110.4 . . ?
H13A C13 H13B 108.6 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N3 C15 C2 128.1(9) . . ?
N3 C15 H15 116.0 . . ?
C2 C15 H15 116.0 . . ?
C15 N3 C16 121.5(8) . . ?
C15 N3 Ni2 125.8(7) . . ?
C16 N3 Ni2 112.7(6) . . ?
C17 C16 N3 104.3(8) . . ?
C17 C16 H16A 110.9 . . ?
N3 C16 H16A 110.9 . . ?
C17 C16 H16B 110.9 . . ?
N3 C16 H16B 110.9 . . ?
H16A C16 H16B 108.9 . . ?
C16 C17 N4 114.8(8) . . ?
C16 C17 H17A 108.6 . . ?
N4 C17 H17A 108.6 . . ?
C16 C17 H17B 108.6 . . ?
N4 C17 H17B 108.6 . . ?
H17A C17 H17B 107.5 . . ?
C20 N4 C17 113.8(7) . . ?
C20 N4 C18 103.8(7) . . ?
C17 N4 C18 110.7(8) . . ?
C20 N4 Ni2 108.7(6) . . ?
C17 N4 Ni2 102.2(6) . . ?
C18 N4 Ni2 117.9(5) . . ?
N4 C18 C19 128.9(8) . . ?
N4 C18 H18A 105.1 . . ?
C19 C18 H18A 105.1 . . ?
N4 C18 H18B 105.1 . . ?
C19 C18 H18B 105.1 . . ?
H18A C18 H18B 105.9 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N4 C20 C21 110.2(8) . . ?
N4 C20 H20A 109.6 . . ?
C21 C20 H20A 109.6 . . ?
N4 C20 H20B 109.6 . . ?
C21 C20 H20B 109.6 . . ?
H20A C20 H20B 108.1 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Ni2 O2 Ni1 100.3(3) . . ?
Ni2 O2 H2 109(7) . . ?
Ni1 O2 H2 136(7) . . ?
O3 Cl1 O6 100.6(9) . . ?
O3 Cl1 O4 110.9(7) . . ?
O6 Cl1 O4 104.1(8) . . ?
O3 Cl1 O5 110.8(8) . . ?
O6 Cl1 O5 120.4(7) . . ?
O4 Cl1 O5 109.6(8) . . ?
O8 Cl2 O7 110.3(15) . . ?
O8 Cl2 O10 102.1(14) . . ?
O7 Cl2 O10 104.3(9) . . ?
O8 Cl2 O9 103.0(10) . . ?
O7 Cl2 O9 113.6(7) . . ?
O10 Cl2 O9 122.6(8) . . ?

_diffrn_measured_fraction_theta_max 0.975
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.975
_refine_diff_density_max         1.352
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.125
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_complex_2a
_database_code_depnum_ccdc_archive 'CCDC 1402078'
_audit_update_record             
;
2015-11-03 deposited with the CCDC.
2015-12-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H44 F6 N5 Ni2 O7, C2 F3 O2, H2 O'
_chemical_formula_sum            'C30 H46 F9 N5 Ni2 O10'
_chemical_formula_weight         925.14

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
F F 0.0171 0.0103 '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           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   11.6655(1)
_cell_length_b                   16.9475(1)
_cell_length_c                   22.7678(2)
_cell_angle_alpha                74.2190(4)
_cell_angle_beta                 87.0926(4)
_cell_angle_gamma                75.7040(4)
_cell_volume                     4196.77(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    295
_cell_measurement_reflns_used    54669
_cell_measurement_theta_min      2.49
_cell_measurement_theta_max      28.00

_exptl_crystal_description       prismatic
_exptl_crystal_colour            'light green'
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1912
_exptl_absorpt_coefficient_mu    0.991
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.613
_exptl_absorpt_correction_T_max  0.753
_exptl_absorpt_process_details   'SORTAV (Blessing, 1995)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      295
_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  'Nonius Kappa CCD'
_diffrn_measurement_method       'φ scans and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            54669
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.49
_diffrn_reflns_theta_max         28.00
_reflns_number_total             19828
_reflns_number_gt                14370
_reflns_threshold_expression     I>2sigma(I)

_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_cell_refinement       'Denzo-SMN (otwinowski & Minor, 1997)'
_computing_data_reduction        'Denzo-SMN (otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP III (Burnett & Johnson, 1996)'
_computing_publication_material  
'SHELXL-97 (Sheldrick, 1997), PARST (Nardelli, 1995)'

_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)+(0.1159P)²+1.8363P] 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         19828
_refine_ls_number_parameters     1051
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0618
_refine_ls_wR_factor_ref         0.1964
_refine_ls_wR_factor_gt          0.1803
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_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 0.05608(4) 0.27637(3) 0.386588(17) 0.04511(11) Uani 1 1 d . . .
Ni2 Ni -0.18361(4) 0.25867(3) 0.48202(2) 0.05232(12) Uani 1 1 d . . .
O1A O -0.0613(2) 0.20585(14) 0.42527(10) 0.0508(5) Uani 1 1 d . . .
C1A C -0.0671(3) 0.1357(2) 0.41234(16) 0.0500(7) Uani 1 1 d . . .
C2A C -0.1129(3) 0.0720(2) 0.45450(17) 0.0562(8) Uani 1 1 d . . .
C3A C -0.1232(4) 0.0002(2) 0.4384(2) 0.0652(9) Uani 1 1 d . . .
H3A H -0.1513 -0.0409 0.4673 0.078 Uiso 1 1 calc R . .
C4A C -0.0935(4) -0.0126(2) 0.3814(2) 0.0676(10) Uani 1 1 d . . .
C5A C -0.0456(3) 0.0472(2) 0.34124(19) 0.0625(9) Uani 1 1 d . . .
H5A H -0.0222 0.0388 0.3033 0.075 Uiso 1 1 calc R . .
C6A C -0.0304(3) 0.1196(2) 0.35471(16) 0.0533(8) Uani 1 1 d . . .
C7A C -0.1105(6) -0.0901(3) 0.3652(3) 0.0975(17) Uani 1 1 d . . .
H7A1 H -0.0775 -0.0915 0.3259 0.146 Uiso 1 1 calc R . .
H7A2 H -0.1934 -0.0879 0.3641 0.146 Uiso 1 1 calc R . .
H7A3 H -0.0712 -0.1401 0.3953 0.146 Uiso 1 1 calc R . .
C8A C -0.1513(3) 0.0763(3) 0.51517(18) 0.0634(9) Uani 1 1 d . . .
H8A H -0.1616 0.0267 0.5424 0.076 Uiso 1 1 calc R . .
N1A N -0.1725(3) 0.1427(2) 0.53468(14) 0.0605(7) Uani 1 1 d . . .
C9A C -0.2211(5) 0.1384(3) 0.5957(2) 0.0780(12) Uani 1 1 d . . .
H9A1 H -0.1652 0.0974 0.6258 0.094 Uiso 1 1 calc R . .
H9A2 H -0.2937 0.1196 0.5986 0.094 Uiso 1 1 calc R . .
C10A C -0.2460(6) 0.2231(4) 0.6095(3) 0.1025(17) Uani 1 1 d . . .
H10A H -0.1726 0.2348 0.6188 0.123 Uiso 1 1 calc R . .
H10B H -0.2967 0.2229 0.6446 0.123 Uiso 1 1 calc R . .
N2A N -0.3069(3) 0.2910(2) 0.55374(17) 0.0747(9) Uani 1 1 d . . .
C11A C -0.2968(5) 0.3711(5) 0.5682(3) 0.115(2) Uani 1 1 d . . .
H11A H -0.3213 0.4176 0.5321 0.138 Uiso 1 1 calc R . .
H11B H -0.2139 0.3661 0.5758 0.138 Uiso 1 1 calc R . .
C12A C -0.3664(8) 0.3946(6) 0.6218(4) 0.154(3) Uani 1 1 d . . .
H12A H -0.4472 0.3927 0.6180 0.230 Uiso 1 1 calc R . .
H12B H -0.3635 0.4507 0.6219 0.230 Uiso 1 1 calc R . .
H12C H -0.3325 0.3554 0.6592 0.230 Uiso 1 1 calc R . .
C13A C -0.4246(5) 0.2900(7) 0.5448(4) 0.136(3) Uani 1 1 d . . .
H13A H -0.4641 0.2856 0.5837 0.164 Uiso 1 1 calc R . .
H13B H -0.4243 0.2394 0.5325 0.164 Uiso 1 1 calc R . .
C14A C -0.4931(8) 0.3609(6) 0.5009(4) 0.144(3) Uani 1 1 d . . .
H14A H -0.5580 0.3898 0.5208 0.215 Uiso 1 1 calc R . .
H14B H -0.5231 0.3418 0.4702 0.215 Uiso 1 1 calc R . .
H14C H -0.4443 0.3986 0.4823 0.215 Uiso 1 1 calc R . .
C15A C 0.0219(3) 0.1747(2) 0.30728(15) 0.0555(8) Uani 1 1 d . . .
H15A H 0.0359 0.1605 0.2705 0.067 Uiso 1 1 calc R . .
N3A N 0.0507(3) 0.24096(18) 0.31085(12) 0.0533(6) Uani 1 1 d . . .
C16A C 0.1076(4) 0.2890(3) 0.25917(17) 0.0673(10) Uani 1 1 d . . .
H16A H 0.0530 0.3419 0.2394 0.081 Uiso 1 1 calc R . .
H16B H 0.1318 0.2568 0.2294 0.081 Uiso 1 1 calc R . .
C17A C 0.2133(4) 0.3055(3) 0.2839(2) 0.0744(11) Uani 1 1 d . . .
H17A H 0.2711 0.2524 0.2995 0.089 Uiso 1 1 calc R . .
H17B H 0.2495 0.3409 0.2513 0.089 Uiso 1 1 calc R . .
N4A N 0.1797(3) 0.34826(19) 0.33396(13) 0.0542(6) Uani 1 1 d . . .
C18A C 0.2906(4) 0.3339(3) 0.3706(2) 0.0766(11) Uani 1 1 d . . .
H18A H 0.2685 0.3551 0.4061 0.092 Uiso 1 1 calc R . .
H18B H 0.3231 0.2734 0.3852 0.092 Uiso 1 1 calc R . .
C19A C 0.3858(5) 0.3725(4) 0.3391(3) 0.0968(16) Uani 1 1 d . . .
H19A H 0.4175 0.3461 0.3075 0.145 Uiso 1 1 calc R . .
H19B H 0.4475 0.3647 0.3680 0.145 Uiso 1 1 calc R . .
H19C H 0.3540 0.4319 0.3214 0.145 Uiso 1 1 calc R . .
C20A C 0.1281(4) 0.4386(3) 0.3075(2) 0.0788(12) Uani 1 1 d . . .
H20A H 0.0558 0.4450 0.2856 0.095 Uiso 1 1 calc R . .
H20B H 0.1827 0.4614 0.2781 0.095 Uiso 1 1 calc R . .
C21A C 0.1008(5) 0.4888(3) 0.3522(3) 0.0994(16) Uani 1 1 d . . .
H21A H 0.0599 0.4606 0.3859 0.149 Uiso 1 1 calc R . .
H21B H 0.0518 0.5436 0.3332 0.149 Uiso 1 1 calc R . .
H21C H 0.1731 0.4950 0.3668 0.149 Uiso 1 1 calc R . .
O2A O 0.1936(3) 0.16682(18) 0.41800(15) 0.0644(7) Uani 1 1 d . . .
H21 H 0.233(4) 0.156(3) 0.445(2) 0.061(13) Uiso 1 1 d . . .
H22 H 0.233(6) 0.143(4) 0.392(3) 0.13(3) Uiso 1 1 d . . .
O3A O 0.0845(2) 0.31095(18) 0.46090(12) 0.0625(6) Uani 1 1 d . . .
O4A O -0.0525(2) 0.27983(19) 0.52919(12) 0.0664(7) Uani 1 1 d . . .
C22A C 0.0352(3) 0.3055(2) 0.51056(15) 0.0519(7) Uani 1 1 d . . .
C23A C 0.0955(4) 0.3360(3) 0.5557(2) 0.0764(12) Uani 1 1 d . . .
F1A F 0.2026(4) 0.2901(4) 0.5702(2) 0.1553(19) Uani 1 1 d . . .
F2A F 0.1044(7) 0.4105(3) 0.5354(2) 0.195(3) Uani 1 1 d . . .
F3A F 0.0454(4) 0.3280(3) 0.60857(16) 0.1430(16) Uani 1 1 d . . .
O5A O -0.0860(2) 0.38034(17) 0.35452(13) 0.0655(7) Uani 1 1 d . . .
O6A O -0.2178(3) 0.37939(17) 0.42912(14) 0.0717(7) Uani 1 1 d . . .
C24A C -0.1760(3) 0.4093(2) 0.37967(18) 0.0584(8) Uani 1 1 d . . .
C25A C -0.2488(5) 0.4941(4) 0.3442(3) 0.0951(16) Uani 1 1 d . . .
F4A F -0.2029(6) 0.5359(4) 0.3032(3) 0.272(5) Uani 1 1 d . . .
F5A F -0.2860(8) 0.5464(3) 0.3783(3) 0.229(4) Uani 1 1 d . . .
F6A F -0.3473(6) 0.4925(4) 0.3290(4) 0.259(5) Uani 1 1 d . . .
O7A O -0.3174(2) 0.2416(2) 0.43021(15) 0.0743(8) Uani 1 1 d . . .
C26A C -0.3106(4) 0.2442(3) 0.3767(3) 0.0832(13) Uani 1 1 d . . .
H26A H -0.2640 0.2780 0.3534 0.100 Uiso 1 1 calc R . .
N5A N -0.3610(4) 0.2050(3) 0.3482(2) 0.0885(12) Uani 1 1 d . . .
C27A C -0.3489(8) 0.2101(8) 0.2851(4) 0.169(4) Uani 1 1 d . . .
H27A H -0.3136 0.2560 0.2656 0.253 Uiso 1 1 calc R . .
H27B H -0.4254 0.2198 0.2670 0.253 Uiso 1 1 calc R . .
H27C H -0.2994 0.1581 0.2799 0.253 Uiso 1 1 calc R . .
C28A C -0.4242(6) 0.1434(5) 0.3838(5) 0.143(3) Uani 1 1 d . . .
H28A H -0.3742 0.0874 0.3901 0.214 Uiso 1 1 calc R . .
H28B H -0.4947 0.1476 0.3620 0.214 Uiso 1 1 calc R . .
H28C H -0.4450 0.1547 0.4225 0.214 Uiso 1 1 calc R . .
O8A O 0.3194(3) 0.0774(2) 0.33796(17) 0.0913(10) Uani 1 1 d . . .
O9A O 0.4245(4) -0.0084(3) 0.41891(19) 0.1043(12) Uani 1 1 d D . .
C29A C 0.3988(4) 0.0192(3) 0.3638(2) 0.0737(11) Uani 1 1 d . . .
C30A C 0.4773(5) -0.0274(4) 0.3227(3) 0.0928(15) Uani 1 1 d . . .
F7A F 0.5273(6) 0.0196(4) 0.2818(3) 0.208(3) Uani 1 1 d . . .
F8A F 0.5587(5) -0.0922(4) 0.3532(3) 0.204(3) Uani 1 1 d . . .
F9A F 0.4204(4) -0.0613(3) 0.2924(2) 0.1457(17) Uani 1 1 d . . .
O10A O 0.3717(5) 0.0927(4) 0.5038(2) 0.155(2) Uani 1 1 d D . .
H101 H 0.397(8) 0.064(4) 0.470(2) 0.232 Uiso 1 1 d D . .
H102 H 0.429(7) 0.067(6) 0.539(3) 0.232 Uiso 1 1 d D . .
Ni3 Ni -0.14066(3) 0.78068(3) -0.008406(18) 0.04530(12) Uani 1 1 d . . .
Ni4 Ni -0.37440(3) 0.71570(3) 0.073745(19) 0.04899(12) Uani 1 1 d . . .
O1B O -0.29022(18) 0.81293(14) 0.04073(10) 0.0465(5) Uani 1 1 d . . .
C1B C -0.3250(3) 0.8851(2) 0.05549(13) 0.0470(7) Uani 1 1 d . . .
C2B C -0.4455(3) 0.9189(2) 0.06734(16) 0.0562(8) Uani 1 1 d . . .
C3B C -0.4793(4) 0.9932(3) 0.08532(19) 0.0699(11) Uani 1 1 d . . .
H3B H -0.5592 1.0142 0.0916 0.084 Uiso 1 1 calc R . .
C4B C -0.4001(4) 1.0375(3) 0.0943(2) 0.0728(11) Uani 1 1 d . . .
C5B C -0.2846(4) 1.0060(2) 0.08272(19) 0.0662(10) Uani 1 1 d . . .
H5B H -0.2295 1.0345 0.0888 0.079 Uiso 1 1 calc R . .
C6B C -0.2432(3) 0.9329(2) 0.06202(15) 0.0522(7) Uani 1 1 d . . .
C7B C -0.4410(6) 1.1164(3) 0.1158(3) 0.1063(19) Uani 1 1 d . . .
H7B1 H -0.4388 1.1015 0.1596 0.159 Uiso 1 1 calc R . .
H7B2 H -0.5205 1.1443 0.1013 0.159 Uiso 1 1 calc R . .
H7B3 H -0.3899 1.1535 0.1001 0.159 Uiso 1 1 calc R . .
C8B C -0.5406(3) 0.8785(3) 0.06177(18) 0.0657(10) Uani 1 1 d . . .
H8B H -0.6179 0.9107 0.0608 0.079 Uiso 1 1 calc R . .
N1B N -0.5264(2) 0.8036(2) 0.05818(15) 0.0621(8) Uani 1 1 d . . .
C9B C -0.6285(3) 0.7688(4) 0.0584(2) 0.0840(14) Uani 1 1 d . . .
H9B1 H -0.6348 0.7549 0.0203 0.101 Uiso 1 1 calc R . .
H9B2 H -0.7006 0.8091 0.0638 0.101 Uiso 1 1 calc R . .
C10B C -0.6083(4) 0.6889(4) 0.1120(3) 0.1003(18) Uani 1 1 d . . .
H10C H -0.6096 0.7047 0.1500 0.120 Uiso 1 1 calc R . .
H10D H -0.6722 0.6614 0.1127 0.120 Uiso 1 1 calc R . .
N2B N -0.4934(3) 0.6284(3) 0.10782(16) 0.0714(9) Uani 1 1 d . . .
C11B C -0.5049(5) 0.5759(4) 0.0675(3) 0.0902(15) Uani 1 1 d . . .
H11C H -0.5274 0.6128 0.0270 0.108 Uiso 1 1 calc R . .
H11D H -0.5689 0.5488 0.0822 0.108 Uiso 1 1 calc R . .
C12B C -0.3970(6) 0.5091(4) 0.0623(4) 0.115(2) Uani 1 1 d . . .
H12D H -0.3287 0.5321 0.0579 0.172 Uiso 1 1 calc R . .
H12E H -0.4052 0.4896 0.0273 0.172 Uiso 1 1 calc R . .
H12F H -0.3879 0.4626 0.0984 0.172 Uiso 1 1 calc R . .
C13B C -0.4522(6) 0.5718(4) 0.1709(2) 0.109(2) Uani 1 1 d . . .
H13C H -0.4436 0.6071 0.1967 0.131 Uiso 1 1 calc R . .
H13D H -0.3747 0.5359 0.1675 0.131 Uiso 1 1 calc R . .
C14B C -0.5349(9) 0.5155(7) 0.2023(4) 0.174(4) Uani 1 1 d . . .
H14D H -0.6155 0.5476 0.1959 0.261 Uiso 1 1 calc R . .
H14E H -0.5169 0.4955 0.2453 0.261 Uiso 1 1 calc R . .
H14F H -0.5238 0.4682 0.1853 0.261 Uiso 1 1 calc R . .
C15B C -0.1181(3) 0.9108(2) 0.05077(17) 0.0577(8) Uani 1 1 d . . .
H15B H -0.0716 0.9418 0.0622 0.069 Uiso 1 1 calc R . .
N3B N -0.0660(2) 0.85232(19) 0.02652(13) 0.0518(6) Uani 1 1 d . . .
C16B C 0.0614(3) 0.8371(3) 0.0173(2) 0.0659(10) Uani 1 1 d . . .
H16C H 0.1023 0.7880 0.0486 0.079 Uiso 1 1 calc R . .
H16D H 0.0890 0.8855 0.0200 0.079 Uiso 1 1 calc R . .
C17B C 0.0868(3) 0.8222(3) -0.0455(2) 0.0668(10) Uani 1 1 d . . .
H17C H 0.0522 0.8735 -0.0765 0.080 Uiso 1 1 calc R . .
H17D H 0.1716 0.8085 -0.0513 0.080 Uiso 1 1 calc R . .
N4B N 0.0379(2) 0.7528(2) -0.05231(14) 0.0576(7) Uani 1 1 d . . .
C18B C 0.0250(4) 0.7585(4) -0.11864(19) 0.0822(14) Uani 1 1 d . . .
H18C H -0.0258 0.8132 -0.1383 0.099 Uiso 1 1 calc R . .
H18D H -0.0143 0.7157 -0.1220 0.099 Uiso 1 1 calc R . .
C19B C 0.1400(5) 0.7474(5) -0.1530(2) 0.123(3) Uani 1 1 d . . .
H19D H 0.1686 0.7976 -0.1602 0.185 Uiso 1 1 calc R . .
H19E H 0.1267 0.7374 -0.1913 0.185 Uiso 1 1 calc R . .
H19F H 0.1976 0.7001 -0.1292 0.185 Uiso 1 1 calc R . .
C20B C 0.1172(3) 0.6697(3) -0.0202(2) 0.0710(11) Uani 1 1 d . . .
H20C H 0.1198 0.6664 0.0230 0.085 Uiso 1 1 calc R . .
H20D H 0.1966 0.6679 -0.0355 0.085 Uiso 1 1 calc R . .
C21B C 0.0813(5) 0.5933(3) -0.0270(3) 0.0973(16) Uani 1 1 d . . .
H21D H -0.0004 0.5976 -0.0167 0.146 Uiso 1 1 calc R . .
H21E H 0.1292 0.5433 -0.0002 0.146 Uiso 1 1 calc R . .
H21F H 0.0923 0.5901 -0.0684 0.146 Uiso 1 1 calc R . .
O2B O -0.2117(2) 0.88419(18) -0.08117(12) 0.0629(6) Uani 1 1 d D . .
H23 H -0.239(6) 0.873(4) -0.1183(19) 0.14(2) Uiso 1 1 d D . .
H24 H -0.172(5) 0.932(3) -0.093(3) 0.12(2) Uiso 1 1 d D . .
O3B O -0.0744(2) 0.68062(17) 0.06613(12) 0.0607(6) Uani 1 1 d . . .
O4B O -0.2250(2) 0.62074(16) 0.09863(13) 0.0622(6) Uani 1 1 d . . .
C22B C -0.1217(3) 0.6268(2) 0.09822(16) 0.0540(8) Uani 1 1 d . . .
C23B C -0.0403(4) 0.5590(3) 0.1469(2) 0.0781(12) Uani 1 1 d . . .
F1B F -0.0397(5) 0.5840(3) 0.19568(19) 0.174(2) Uani 1 1 d . . .
F2B F 0.0672(4) 0.5418(4) 0.1326(3) 0.207(3) Uani 1 1 d . . .
F3B F -0.0737(5) 0.4898(2) 0.1658(3) 0.179(2) Uani 1 1 d . . .
O5B O -0.2062(2) 0.71190(18) -0.05303(12) 0.0609(6) Uani 1 1 d . . .
O6B O -0.3809(2) 0.69679(18) -0.01112(11) 0.0612(6) Uani 1 1 d . . .
C24B C -0.3035(3) 0.6937(2) -0.04988(15) 0.0530(8) Uani 1 1 d . . .
C25B C -0.3316(4) 0.6621(3) -0.1030(2) 0.0749(12) Uani 1 1 d . . .
F4B F -0.3418(5) 0.7231(3) -0.15546(17) 0.1504(17) Uani 1 1 d . . .
F5B F -0.4359(4) 0.6498(4) -0.1026(2) 0.175(2) Uani 1 1 d . . .
F6B F -0.2557(6) 0.6060(4) -0.1139(3) 0.248(4) Uani 1 1 d . . .
O7B O -0.3706(2) 0.73170(19) 0.16111(11) 0.0651(7) Uani 1 1 d . . .
C26B C -0.2913(4) 0.7500(3) 0.18296(17) 0.0646(9) Uani 1 1 d . . .
H26B H -0.2242 0.7549 0.1597 0.078 Uiso 1 1 calc R . .
N5B N -0.2937(5) 0.7631(3) 0.23634(18) 0.0944(14) Uani 1 1 d . . .
C27B C -0.1899(11) 0.7831(9) 0.2582(5) 0.236(7) Uani 1 1 d . . .
H27D H -0.1638 0.7445 0.2972 0.354 Uiso 1 1 calc R . .
H27E H -0.2113 0.8399 0.2621 0.354 Uiso 1 1 calc R . .
H27F H -0.1271 0.7780 0.2295 0.354 Uiso 1 1 calc R . .
C28B C -0.3907(9) 0.7506(6) 0.2766(3) 0.153(3) Uani 1 1 d . . .
H28D H -0.4639 0.7829 0.2558 0.229 Uiso 1 1 calc R . .
H28E H -0.3820 0.7688 0.3122 0.229 Uiso 1 1 calc R . .
H28F H -0.3907 0.6917 0.2885 0.229 Uiso 1 1 calc R . .
O8B O -0.1407(5) 1.0322(3) -0.1132(2) 0.1237(15) Uani 1 1 d . . .
O9B O -0.0997(8) 1.0084(5) -0.2053(4) 0.207(4) Uani 1 1 d . . .
C29B C -0.1250(7) 1.0523(4) -0.1673(3) 0.1076(18) Uani 1 1 d . . .
C30B C -0.1238(11) 1.1414(6) -0.1974(3) 0.145(3) Uani 1 1 d . . .
F7B F -0.1034(11) 1.1843(4) -0.1646(3) 0.252(5) Uani 1 1 d . . .
F8B F -0.2441(11) 1.1877(6) -0.2070(5) 0.321(6) Uani 1 1 d . . .
F9B F -0.0950(8) 1.1630(4) -0.2508(2) 0.208(3) Uani 1 1 d . . .
O10B O -0.2303(5) 0.8958(3) -0.20684(18) 0.1087(13) Uani 1 1 d D . .
H103 H -0.283(6) 0.890(5) -0.238(3) 0.163 Uiso 1 1 d D . .
H104 H -0.184(6) 0.939(4) -0.223(4) 0.163 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
Ni1 N3A 1.982(3) . ?
Ni1 O3A 2.002(2) . ?
Ni1 O1A 2.048(2) . ?
Ni1 O5A 2.090(3) . ?
Ni1 O2A 2.110(3) . ?
Ni1 N4A 2.213(3) . ?
Ni2 N1A 1.982(3) . ?
Ni2 O6A 2.025(3) . ?
Ni2 O4A 2.066(3) . ?
Ni2 O1A 2.078(2) . ?
Ni2 O7A 2.123(3) . ?
Ni2 N2A 2.212(3) . ?
O1A C1A 1.317(4) . ?
C1A C2A 1.428(5) . ?
C1A C6A 1.435(5) . ?
C2A C3A 1.397(5) . ?
C2A C8A 1.446(6) . ?
C3A C4A 1.386(6) . ?
C3A H3A 0.9300 . ?
C4A C5A 1.378(6) . ?
C4A C7A 1.518(6) . ?
C5A C6A 1.397(5) . ?
C5A H5A 0.9300 . ?
C6A C15A 1.441(5) . ?
C7A H7A1 0.9600 . ?
C7A H7A2 0.9600 . ?
C7A H7A3 0.9600 . ?
C8A N1A 1.283(5) . ?
C8A H8A 0.9300 . ?
N1A C9A 1.463(5) . ?
C9A C10A 1.508(8) . ?
C9A H9A1 0.9700 . ?
C9A H9A2 0.9700 . ?
C10A N2A 1.528(7) . ?
C10A H10A 0.9700 . ?
C10A H10B 0.9700 . ?
N2A C13A 1.404(7) . ?
N2A C11A 1.513(7) . ?
C11A C12A 1.520(8) . ?
C11A H11A 0.9700 . ?
C11A H11B 0.9700 . ?
C12A H12A 0.9600 . ?
C12A H12B 0.9600 . ?
C12A H12C 0.9600 . ?
C13A C14A 1.425(11) . ?
C13A H13A 0.9700 . ?
C13A H13B 0.9700 . ?
C14A H14A 0.9600 . ?
C14A H14B 0.9600 . ?
C14A H14C 0.9600 . ?
C15A N3A 1.272(5) . ?
C15A H15A 0.9300 . ?
N3A C16A 1.468(5) . ?
C16A C17A 1.499(6) . ?
C16A H16A 0.9700 . ?
C16A H16B 0.9700 . ?
C17A N4A 1.496(5) . ?
C17A H17A 0.9700 . ?
C17A H17B 0.9700 . ?
N4A C20A 1.466(5) . ?
N4A C18A 1.507(5) . ?
C18A C19A 1.483(7) . ?
C18A H18A 0.9700 . ?
C18A H18B 0.9700 . ?
C19A H19A 0.9600 . ?
C19A H19B 0.9600 . ?
C19A H19C 0.9600 . ?
C20A C21A 1.472(7) . ?
C20A H20A 0.9700 . ?
C20A H20B 0.9700 . ?
C21A H21A 0.9600 . ?
C21A H21B 0.9600 . ?
C21A H21C 0.9600 . ?
O2A H21 0.74(5) . ?
O2A H22 0.85(8) . ?
O3A C22A 1.233(4) . ?
O4A C22A 1.221(4) . ?
C22A C23A 1.536(5) . ?
C23A F2A 1.249(6) . ?
C23A F3A 1.299(6) . ?
C23A F1A 1.303(6) . ?
O5A C24A 1.229(5) . ?
O6A C24A 1.232(5) . ?
C24A C25A 1.508(6) . ?
C25A F4A 1.198(7) . ?
C25A F6A 1.225(8) . ?
C25A F5A 1.313(8) . ?
O7A C26A 1.206(6) . ?
C26A N5A 1.295(6) . ?
C26A H26A 0.9300 . ?
N5A C27A 1.417(9) . ?
N5A C28A 1.466(9) . ?
C27A H27A 0.9600 . ?
C27A H27B 0.9600 . ?
C27A H27C 0.9600 . ?
C28A H28A 0.9600 . ?
C28A H28B 0.9600 . ?
C28A H28C 0.9600 . ?
O8A C29A 1.211(5) . ?
O9A C29A 1.238(6) . ?
C29A C30A 1.515(7) . ?
C30A F7A 1.269(8) . ?
C30A F9A 1.303(7) . ?
C30A F8A 1.315(7) . ?
O10A H101 1.009(10) . ?
O10A H102 1.002(10) . ?
Ni3 N3B 1.995(3) . ?
Ni3 O5B 2.034(2) . ?
Ni3 O1B 2.063(2) . ?
Ni3 O3B 2.067(3) . ?
Ni3 O2B 2.085(3) . ?
Ni3 N4B 2.263(3) . ?
Ni4 N1B 1.990(3) . ?
Ni4 O4B 2.041(3) . ?
Ni4 O6B 2.051(2) . ?
Ni4 O1B 2.072(2) . ?
Ni4 O7B 2.083(2) . ?
Ni4 N2B 2.236(3) . ?
O1B C1B 1.318(4) . ?
C1B C2B 1.423(5) . ?
C1B C6B 1.432(5) . ?
C2B C3B 1.389(6) . ?
C2B C8B 1.467(6) . ?
C3B C4B 1.380(7) . ?
C3B H3B 0.9300 . ?
C4B C5B 1.362(6) . ?
C4B C7B 1.506(6) . ?
C5B C6B 1.410(5) . ?
C5B H5B 0.9300 . ?
C6B C15B 1.443(5) . ?
C7B H7B1 0.9600 . ?
C7B H7B2 0.9600 . ?
C7B H7B3 0.9600 . ?
C8B N1B 1.263(6) . ?
C8B H8B 0.9300 . ?
N1B C9B 1.453(5) . ?
C9B C10B 1.534(8) . ?
C9B H9B1 0.9700 . ?
C9B H9B2 0.9700 . ?
C10B N2B 1.489(7) . ?
C10B H10C 0.9700 . ?
C10B H10D 0.9700 . ?
N2B C11B 1.472(6) . ?
N2B C13B 1.518(6) . ?
C11B C12B 1.494(8) . ?
C11B H11C 0.9700 . ?
C11B H11D 0.9700 . ?
C12B H12D 0.9600 . ?
C12B H12E 0.9600 . ?
C12B H12F 0.9600 . ?
C13B C14B 1.538(8) . ?
C13B H13C 0.9700 . ?
C13B H13D 0.9700 . ?
C14B H14D 0.9600 . ?
C14B H14E 0.9600 . ?
C14B H14F 0.9600 . ?
C15B N3B 1.274(5) . ?
C15B H15B 0.9300 . ?
N3B C16B 1.459(4) . ?
C16B C17B 1.521(6) . ?
C16B H16C 0.9700 . ?
C16B H16D 0.9700 . ?
C17B N4B 1.474(5) . ?
C17B H17C 0.9700 . ?
C17B H17D 0.9700 . ?
N4B C20B 1.497(5) . ?
N4B C18B 1.500(5) . ?
C18B C19B 1.515(7) . ?
C18B H18C 0.9700 . ?
C18B H18D 0.9700 . ?
C19B H19D 0.9600 . ?
C19B H19E 0.9600 . ?
C19B H19F 0.9600 . ?
C20B C21B 1.502(7) . ?
C20B H20C 0.9700 . ?
C20B H20D 0.9700 . ?
C21B H21D 0.9600 . ?
C21B H21E 0.9600 . ?
C21B H21F 0.9600 . ?
O2B H23 0.994(10) . ?
O2B H24 0.995(10) . ?
O3B C22B 1.231(4) . ?
O4B C22B 1.234(4) . ?
C22B C23B 1.525(5) . ?
C23B F2B 1.262(7) . ?
C23B F3B 1.284(6) . ?
C23B F1B 1.293(6) . ?
O5B C24B 1.243(4) . ?
O6B C24B 1.232(4) . ?
C24B C25B 1.528(5) . ?
C25B F6B 1.200(6) . ?
C25B F5B 1.284(6) . ?
C25B F4B 1.339(6) . ?
O7B C26B 1.213(5) . ?
C26B N5B 1.291(5) . ?
C26B H26B 0.9300 . ?
N5B C28B 1.439(10) . ?
N5B C27B 1.479(10) . ?
C27B H27D 0.9600 . ?
C27B H27E 0.9600 . ?
C27B H27F 0.9600 . ?
C28B H28D 0.9600 . ?
C28B H28E 0.9600 . ?
C28B H28F 0.9600 . ?
O8B C29B 1.204(8) . ?
O9B C29B 1.266(8) . ?
C29B C30B 1.482(10) . ?
C30B F9B 1.225(8) . ?
C30B F7B 1.241(9) . ?
C30B F8B 1.424(13) . ?
O10B H103 0.998(10) . ?
O10B H104 0.997(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
N3A Ni1 O3A 172.35(12) . . ?
N3A Ni1 O1A 89.44(11) . . ?
O3A Ni1 O1A 96.62(10) . . ?
N3A Ni1 O5A 90.50(12) . . ?
O3A Ni1 O5A 94.22(12) . . ?
O1A Ni1 O5A 89.32(10) . . ?
N3A Ni1 O2A 87.50(13) . . ?
O3A Ni1 O2A 88.05(13) . . ?
O1A Ni1 O2A 87.99(11) . . ?
O5A Ni1 O2A 176.66(12) . . ?
N3A Ni1 N4A 83.27(12) . . ?
O3A Ni1 N4A 90.69(11) . . ?
O1A Ni1 N4A 172.69(10) . . ?
O5A Ni1 N4A 90.10(11) . . ?
O2A Ni1 N4A 92.31(12) . . ?
N1A Ni2 O6A 172.60(13) . . ?
N1A Ni2 O4A 94.31(13) . . ?
O6A Ni2 O4A 90.94(13) . . ?
N1A Ni2 O1A 87.89(11) . . ?
O6A Ni2 O1A 97.14(10) . . ?
O4A Ni2 O1A 91.98(10) . . ?
N1A Ni2 O7A 88.16(13) . . ?
O6A Ni2 O7A 86.66(13) . . ?
O4A Ni2 O7A 177.40(13) . . ?
O1A Ni2 O7A 87.34(11) . . ?
N1A Ni2 N2A 81.62(14) . . ?
O6A Ni2 N2A 93.43(13) . . ?
O4A Ni2 N2A 87.52(13) . . ?
O1A Ni2 N2A 169.43(12) . . ?
O7A Ni2 N2A 93.62(14) . . ?
C1A O1A Ni1 123.9(2) . . ?
C1A O1A Ni2 121.2(2) . . ?
Ni1 O1A Ni2 114.75(11) . . ?
O1A C1A C2A 121.8(3) . . ?
O1A C1A C6A 122.1(3) . . ?
C2A C1A C6A 116.1(3) . . ?
C3A C2A C1A 120.5(4) . . ?
C3A C2A C8A 115.6(4) . . ?
C1A C2A C8A 123.9(3) . . ?
C4A C3A C2A 122.9(4) . . ?
C4A C3A H3A 118.5 . . ?
C2A C3A H3A 118.5 . . ?
C5A C4A C3A 116.8(3) . . ?
C5A C4A C7A 122.0(4) . . ?
C3A C4A C7A 121.1(4) . . ?
C4A C5A C6A 123.2(4) . . ?
C4A C5A H5A 118.4 . . ?
C6A C5A H5A 118.4 . . ?
C5A C6A C1A 120.2(3) . . ?
C5A C6A C15A 115.5(3) . . ?
C1A C6A C15A 124.3(3) . . ?
C4A C7A H7A1 109.5 . . ?
C4A C7A H7A2 109.5 . . ?
H7A1 C7A H7A2 109.5 . . ?
C4A C7A H7A3 109.5 . . ?
H7A1 C7A H7A3 109.5 . . ?
H7A2 C7A H7A3 109.5 . . ?
N1A C8A C2A 125.6(3) . . ?
N1A C8A H8A 117.2 . . ?
C2A C8A H8A 117.2 . . ?
C8A N1A C9A 119.0(3) . . ?
C8A N1A Ni2 124.4(3) . . ?
C9A N1A Ni2 114.8(3) . . ?
N1A C9A C10A 111.5(4) . . ?
N1A C9A H9A1 109.3 . . ?
C10A C9A H9A1 109.3 . . ?
N1A C9A H9A2 109.3 . . ?
C10A C9A H9A2 109.3 . . ?
H9A1 C9A H9A2 108.0 . . ?
C9A C10A N2A 108.6(5) . . ?
C9A C10A H10A 110.0 . . ?
N2A C10A H10A 110.0 . . ?
C9A C10A H10B 110.0 . . ?
N2A C10A H10B 110.0 . . ?
H10A C10A H10B 108.4 . . ?
C13A N2A C11A 112.5(5) . . ?
C13A N2A C10A 113.8(6) . . ?
C11A N2A C10A 101.7(5) . . ?
C13A N2A Ni2 115.1(4) . . ?
C11A N2A Ni2 112.6(3) . . ?
C10A N2A Ni2 99.7(3) . . ?
N2A C11A C12A 117.6(6) . . ?
N2A C11A H11A 107.9 . . ?
C12A C11A H11A 107.9 . . ?
N2A C11A H11B 107.9 . . ?
C12A C11A H11B 107.9 . . ?
H11A C11A H11B 107.2 . . ?
C11A C12A H12A 109.5 . . ?
C11A C12A H12B 109.5 . . ?
H12A C12A H12B 109.5 . . ?
C11A C12A H12C 109.5 . . ?
H12A C12A H12C 109.5 . . ?
H12B C12A H12C 109.5 . . ?
N2A C13A C14A 116.5(8) . . ?
N2A C13A H13A 108.2 . . ?
C14A C13A H13A 108.2 . . ?
N2A C13A H13B 108.2 . . ?
C14A C13A H13B 108.2 . . ?
H13A C13A H13B 107.3 . . ?
C13A C14A H14A 109.5 . . ?
C13A C14A H14B 109.5 . . ?
H14A C14A H14B 109.5 . . ?
C13A C14A H14C 109.5 . . ?
H14A C14A H14C 109.5 . . ?
H14B C14A H14C 109.5 . . ?
N3A C15A C6A 126.4(3) . . ?
N3A C15A H15A 116.8 . . ?
C6A C15A H15A 116.8 . . ?
C15A N3A C16A 120.0(3) . . ?
C15A N3A Ni1 125.7(2) . . ?
C16A N3A Ni1 113.1(2) . . ?
N3A C16A C17A 107.4(3) . . ?
N3A C16A H16A 110.2 . . ?
C17A C16A H16A 110.2 . . ?
N3A C16A H16B 110.2 . . ?
C17A C16A H16B 110.2 . . ?
H16A C16A H16B 108.5 . . ?
N4A C17A C16A 111.2(4) . . ?
N4A C17A H17A 109.4 . . ?
C16A C17A H17A 109.4 . . ?
N4A C17A H17B 109.4 . . ?
C16A C17A H17B 109.4 . . ?
H17A C17A H17B 108.0 . . ?
C20A N4A C17A 109.6(3) . . ?
C20A N4A C18A 111.4(3) . . ?
C17A N4A C18A 107.2(3) . . ?
C20A N4A Ni1 115.1(3) . . ?
C17A N4A Ni1 101.5(2) . . ?
C18A N4A Ni1 111.3(2) . . ?
C19A C18A N4A 117.1(4) . . ?
C19A C18A H18A 108.0 . . ?
N4A C18A H18A 108.0 . . ?
C19A C18A H18B 108.0 . . ?
N4A C18A H18B 108.0 . . ?
H18A C18A H18B 107.3 . . ?
C18A C19A H19A 109.5 . . ?
C18A C19A H19B 109.5 . . ?
H19A C19A H19B 109.5 . . ?
C18A C19A H19C 109.5 . . ?
H19A C19A H19C 109.5 . . ?
H19B C19A H19C 109.5 . . ?
N4A C20A C21A 114.6(4) . . ?
N4A C20A H20A 108.6 . . ?
C21A C20A H20A 108.6 . . ?
N4A C20A H20B 108.6 . . ?
C21A C20A H20B 108.6 . . ?
H20A C20A H20B 107.6 . . ?
C20A C21A H21A 109.5 . . ?
C20A C21A H21B 109.5 . . ?
H21A C21A H21B 109.5 . . ?
C20A C21A H21C 109.5 . . ?
H21A C21A H21C 109.5 . . ?
H21B C21A H21C 109.5 . . ?
Ni1 O2A H21 127(3) . . ?
Ni1 O2A H22 120(5) . . ?
H21 O2A H22 107(6) . . ?
C22A O3A Ni1 133.0(2) . . ?
C22A O4A Ni2 130.2(2) . . ?
O4A C22A O3A 130.5(3) . . ?
O4A C22A C23A 115.7(3) . . ?
O3A C22A C23A 113.8(3) . . ?
F2A C23A F3A 108.9(5) . . ?
F2A C23A F1A 106.1(5) . . ?
F3A C23A F1A 102.2(5) . . ?
F2A C23A C22A 113.3(4) . . ?
F3A C23A C22A 113.7(4) . . ?
F1A C23A C22A 111.9(4) . . ?
C24A O5A Ni1 131.4(3) . . ?
C24A O6A Ni2 129.8(3) . . ?
O5A C24A O6A 130.2(4) . . ?
O5A C24A C25A 115.4(4) . . ?
O6A C24A C25A 114.4(4) . . ?
F4A C25A F6A 111.2(7) . . ?
F4A C25A F5A 101.8(7) . . ?
F6A C25A F5A 96.0(7) . . ?
F4A C25A C24A 118.3(5) . . ?
F6A C25A C24A 113.8(6) . . ?
F5A C25A C24A 112.8(5) . . ?
C26A O7A Ni2 124.5(3) . . ?
O7A C26A N5A 127.1(6) . . ?
O7A C26A H26A 116.4 . . ?
N5A C26A H26A 116.4 . . ?
C26A N5A C27A 124.5(7) . . ?
C26A N5A C28A 118.7(6) . . ?
C27A N5A C28A 116.5(7) . . ?
N5A C27A H27A 109.5 . . ?
N5A C27A H27B 109.5 . . ?
H27A C27A H27B 109.5 . . ?
N5A C27A H27C 109.5 . . ?
H27A C27A H27C 109.5 . . ?
H27B C27A H27C 109.5 . . ?
N5A C28A H28A 109.5 . . ?
N5A C28A H28B 109.5 . . ?
H28A C28A H28B 109.5 . . ?
N5A C28A H28C 109.5 . . ?
H28A C28A H28C 109.5 . . ?
H28B C28A H28C 109.5 . . ?
O8A C29A O9A 129.4(5) . . ?
O8A C29A C30A 115.2(5) . . ?
O9A C29A C30A 115.3(5) . . ?
F7A C30A F9A 104.3(6) . . ?
F7A C30A F8A 108.7(6) . . ?
F9A C30A F8A 103.2(5) . . ?
F7A C30A C29A 113.6(5) . . ?
F9A C30A C29A 113.4(5) . . ?
F8A C30A C29A 112.8(5) . . ?
H101 O10A H102 110.0(15) . . ?
N3B Ni3 O5B 173.31(11) . . ?
N3B Ni3 O1B 88.67(10) . . ?
O5B Ni3 O1B 96.85(9) . . ?
N3B Ni3 O3B 88.18(11) . . ?
O5B Ni3 O3B 95.69(11) . . ?
O1B Ni3 O3B 88.83(10) . . ?
N3B Ni3 O2B 90.74(12) . . ?
O5B Ni3 O2B 85.59(11) . . ?
O1B Ni3 O2B 89.07(10) . . ?
O3B Ni3 O2B 177.66(11) . . ?
N3B Ni3 N4B 82.68(12) . . ?
O5B Ni3 N4B 91.95(11) . . ?
O1B Ni3 N4B 170.98(10) . . ?
O3B Ni3 N4B 88.33(11) . . ?
O2B Ni3 N4B 93.60(11) . . ?
N1B Ni4 O4B 173.97(13) . . ?
N1B Ni4 O6B 91.73(12) . . ?
O4B Ni4 O6B 92.68(11) . . ?
N1B Ni4 O1B 87.12(12) . . ?
O4B Ni4 O1B 96.83(9) . . ?
O6B Ni4 O1B 92.05(10) . . ?
N1B Ni4 O7B 88.37(12) . . ?
O4B Ni4 O7B 87.10(11) . . ?
O6B Ni4 O7B 178.11(11) . . ?
O1B Ni4 O7B 89.84(10) . . ?
N1B Ni4 N2B 83.15(15) . . ?
O4B Ni4 N2B 92.79(13) . . ?
O6B Ni4 N2B 89.24(12) . . ?
O1B Ni4 N2B 170.22(12) . . ?
O7B Ni4 N2B 88.90(12) . . ?
C1B O1B Ni3 124.5(2) . . ?
C1B O1B Ni4 121.5(2) . . ?
Ni3 O1B Ni4 113.71(10) . . ?
O1B C1B C2B 122.0(3) . . ?
O1B C1B C6B 121.9(3) . . ?
C2B C1B C6B 116.1(3) . . ?
C3B C2B C1B 120.9(4) . . ?
C3B C2B C8B 116.1(3) . . ?
C1B C2B C8B 123.0(3) . . ?
C4B C3B C2B 123.1(4) . . ?
C4B C3B H3B 118.4 . . ?
C2B C3B H3B 118.4 . . ?
C5B C4B C3B 116.4(4) . . ?
C5B C4B C7B 122.6(5) . . ?
C3B C4B C7B 121.0(5) . . ?
C4B C5B C6B 124.2(4) . . ?
C4B C5B H5B 117.9 . . ?
C6B C5B H5B 117.9 . . ?
C5B C6B C1B 119.1(3) . . ?
C5B C6B C15B 116.0(3) . . ?
C1B C6B C15B 124.9(3) . . ?
C4B C7B H7B1 109.5 . . ?
C4B C7B H7B2 109.5 . . ?
H7B1 C7B H7B2 109.5 . . ?
C4B C7B H7B3 109.5 . . ?
H7B1 C7B H7B3 109.5 . . ?
H7B2 C7B H7B3 109.5 . . ?
N1B C8B C2B 125.5(3) . . ?
N1B C8B H8B 117.2 . . ?
C2B C8B H8B 117.2 . . ?
C8B N1B C9B 120.0(3) . . ?
C8B N1B Ni4 125.1(2) . . ?
C9B N1B Ni4 113.0(3) . . ?
N1B C9B C10B 106.1(3) . . ?
N1B C9B H9B1 110.5 . . ?
C10B C9B H9B1 110.5 . . ?
N1B C9B H9B2 110.5 . . ?
C10B C9B H9B2 110.5 . . ?
H9B1 C9B H9B2 108.7 . . ?
N2B C10B C9B 112.0(4) . . ?
N2B C10B H10C 109.2 . . ?
C9B C10B H10C 109.2 . . ?
N2B C10B H10D 109.2 . . ?
C9B C10B H10D 109.2 . . ?
H10C C10B H10D 107.9 . . ?
C11B N2B C10B 110.8(4) . . ?
C11B N2B C13B 109.4(4) . . ?
C10B N2B C13B 109.9(4) . . ?
C11B N2B Ni4 114.9(3) . . ?
C10B N2B Ni4 101.7(3) . . ?
C13B N2B Ni4 109.9(3) . . ?
N2B C11B C12B 116.0(4) . . ?
N2B C11B H11C 108.3 . . ?
C12B C11B H11C 108.3 . . ?
N2B C11B H11D 108.3 . . ?
C12B C11B H11D 108.3 . . ?
H11C C11B H11D 107.4 . . ?
C11B C12B H12D 109.5 . . ?
C11B C12B H12E 109.5 . . ?
H12D C12B H12E 109.5 . . ?
C11B C12B H12F 109.5 . . ?
H12D C12B H12F 109.5 . . ?
H12E C12B H12F 109.5 . . ?
N2B C13B C14B 114.8(5) . . ?
N2B C13B H13C 108.6 . . ?
C14B C13B H13C 108.6 . . ?
N2B C13B H13D 108.6 . . ?
C14B C13B H13D 108.6 . . ?
H13C C13B H13D 107.5 . . ?
C13B C14B H14D 109.5 . . ?
C13B C14B H14E 109.5 . . ?
H14D C14B H14E 109.5 . . ?
C13B C14B H14F 109.5 . . ?
H14D C14B H14F 109.5 . . ?
H14E C14B H14F 109.5 . . ?
N3B C15B C6B 125.3(3) . . ?
N3B C15B H15B 117.4 . . ?
C6B C15B H15B 117.4 . . ?
C15B N3B C16B 119.6(3) . . ?
C15B N3B Ni3 127.4(2) . . ?
C16B N3B Ni3 112.9(2) . . ?
N3B C16B C17B 108.3(3) . . ?
N3B C16B H16C 110.0 . . ?
C17B C16B H16C 110.0 . . ?
N3B C16B H16D 110.0 . . ?
C17B C16B H16D 110.0 . . ?
H16C C16B H16D 108.4 . . ?
N4B C17B C16B 111.1(3) . . ?
N4B C17B H17C 109.4 . . ?
C16B C17B H17C 109.4 . . ?
N4B C17B H17D 109.4 . . ?
C16B C17B H17D 109.4 . . ?
H17C C17B H17D 108.0 . . ?
C17B N4B C20B 109.7(3) . . ?
C17B N4B C18B 110.1(4) . . ?
C20B N4B C18B 110.5(3) . . ?
C17B N4B Ni3 101.4(2) . . ?
C20B N4B Ni3 113.4(2) . . ?
C18B N4B Ni3 111.3(2) . . ?
N4B C18B C19B 115.0(4) . . ?
N4B C18B H18C 108.5 . . ?
C19B C18B H18C 108.5 . . ?
N4B C18B H18D 108.5 . . ?
C19B C18B H18D 108.5 . . ?
H18C C18B H18D 107.5 . . ?
C18B C19B H19D 109.5 . . ?
C18B C19B H19E 109.5 . . ?
H19D C19B H19E 109.5 . . ?
C18B C19B H19F 109.5 . . ?
H19D C19B H19F 109.5 . . ?
H19E C19B H19F 109.5 . . ?
N4B C20B C21B 115.1(4) . . ?
N4B C20B H20C 108.5 . . ?
C21B C20B H20C 108.5 . . ?
N4B C20B H20D 108.5 . . ?
C21B C20B H20D 108.5 . . ?
H20C C20B H20D 107.5 . . ?
C20B C21B H21D 109.5 . . ?
C20B C21B H21E 109.5 . . ?
H21D C21B H21E 109.5 . . ?
C20B C21B H21F 109.5 . . ?
H21D C21B H21F 109.5 . . ?
H21E C21B H21F 109.5 . . ?
Ni3 O2B H23 118(4) . . ?
Ni3 O2B H24 119(4) . . ?
H23 O2B H24 110(5) . . ?
C22B O3B Ni3 130.1(2) . . ?
C22B O4B Ni4 127.9(2) . . ?
O3B C22B O4B 130.4(3) . . ?
O3B C22B C23B 114.4(4) . . ?
O4B C22B C23B 115.2(4) . . ?
F2B C23B F3B 108.6(5) . . ?
F2B C23B F1B 104.2(6) . . ?
F3B C23B F1B 103.7(5) . . ?
F2B C23B C22B 114.9(4) . . ?
F3B C23B C22B 114.1(4) . . ?
F1B C23B C22B 110.3(4) . . ?
C24B O5B Ni3 131.0(2) . . ?
C24B O6B Ni4 129.4(2) . . ?
O6B C24B O5B 130.7(3) . . ?
O6B C24B C25B 114.8(3) . . ?
O5B C24B C25B 114.4(3) . . ?
F6B C25B F5B 113.5(6) . . ?
F6B C25B F4B 102.7(6) . . ?
F5B C25B F4B 98.1(5) . . ?
F6B C25B C24B 115.1(4) . . ?
F5B C25B C24B 114.6(4) . . ?
F4B C25B C24B 110.7(4) . . ?
C26B O7B Ni4 125.8(3) . . ?
O7B C26B N5B 124.4(5) . . ?
O7B C26B H26B 117.8 . . ?
N5B C26B H26B 117.8 . . ?
C26B N5B C28B 120.9(5) . . ?
C26B N5B C27B 119.0(6) . . ?
C28B N5B C27B 119.9(6) . . ?
N5B C27B H27D 109.5 . . ?
N5B C27B H27E 109.5 . . ?
H27D C27B H27E 109.5 . . ?
N5B C27B H27F 109.5 . . ?
H27D C27B H27F 109.5 . . ?
H27E C27B H27F 109.5 . . ?
N5B C28B H28D 109.5 . . ?
N5B C28B H28E 109.5 . . ?
H28D C28B H28E 109.5 . . ?
N5B C28B H28F 109.5 . . ?
H28D C28B H28F 109.5 . . ?
H28E C28B H28F 109.5 . . ?
O8B C29B O9B 131.0(7) . . ?
O8B C29B C30B 118.6(6) . . ?
O9B C29B C30B 110.2(7) . . ?
F9B C30B F7B 115.2(9) . . ?
F9B C30B F8B 95.9(8) . . ?
F7B C30B F8B 92.4(9) . . ?
F9B C30B C29B 121.0(8) . . ?
F7B C30B C29B 117.4(6) . . ?
F8B C30B C29B 106.7(10) . . ?
H103 O10B H104 115(7) . . ?

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        28.00
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         1.143
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.075
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_complex_2b
_database_code_depnum_ccdc_archive 'CCDC 1402079'
_audit_update_record             
;
2015-12-10 deposited with the CCDC.
2015-12-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H54 N5 Ni2 O7, Cl O4, C3 H7 N O'
_chemical_formula_sum            'C33 H61 Cl N6 Ni2 O12'
_chemical_formula_weight         886.75

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

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

_cell_length_a                   19.664(3)
_cell_length_b                   11.6297(18)
_cell_length_c                   20.591(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 117.270(4)
_cell_angle_gamma                90.00
_cell_volume                     4185.5(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    295
_cell_measurement_reflns_used    51533
_cell_measurement_theta_min      1.95
_cell_measurement_theta_max      26.37

_exptl_crystal_description       block
_exptl_crystal_colour            'light green'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1880
_exptl_absorpt_coefficient_mu    1.027
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.695
_exptl_absorpt_correction_T_max  0.802
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      295
_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       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            51533
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.95
_diffrn_reflns_theta_max         26.37
_reflns_number_total             8467
_reflns_number_gt                6939
_reflns_threshold_expression     I>2sigma(I)

_computing_data_collection       'Brucker SMART'
_computing_cell_refinement       'Brucker SMART'
_computing_data_reduction        'Brucker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Diamond
_computing_publication_material  
'SHELXL-97 (Sheldrick, 1997),PLATON (Spek, 2009)'

_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)+(0.0495P)²+3.8135P] 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         8467
_refine_ls_number_parameters     497
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0377
_refine_ls_wR_factor_ref         0.1046
_refine_ls_wR_factor_gt          0.0969
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.058
_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 0.253308(18) 0.00691(3) 0.485290(15) 0.02581(10) Uani 1 1 d . . .
Ni2 Ni 0.378335(18) 0.20528(3) 0.596288(16) 0.02769(10) Uani 1 1 d . . .
O1 O 0.28567(9) 0.10448(14) 0.57768(8) 0.0260(4) Uani 1 1 d . . .
C1 C 0.25042(14) 0.0998(2) 0.61890(12) 0.0247(5) Uani 1 1 d . . .
C2 C 0.28956(14) 0.1243(2) 0.69543(12) 0.0265(5) Uani 1 1 d . . .
C3 C 0.25195(15) 0.1104(2) 0.73847(12) 0.0288(5) Uani 1 1 d . . .
H3 H 0.2791 0.1244 0.7884 0.035 Uiso 1 1 calc R . .
C4 C 0.17677(15) 0.0770(2) 0.71024(13) 0.0284(5) Uani 1 1 d . . .
C5 C 0.13726(15) 0.0605(2) 0.63535(13) 0.0276(5) Uani 1 1 d . . .
H5 H 0.0856 0.0418 0.6147 0.033 Uiso 1 1 calc R . .
C6 C 0.17169(14) 0.0710(2) 0.58978(12) 0.0253(5) Uani 1 1 d . . .
C7 C 0.13787(17) 0.0565(3) 0.75834(14) 0.0365(6) Uani 1 1 d . . .
H7A H 0.0836 0.0666 0.7299 0.055 Uiso 1 1 calc R . .
H7B H 0.1571 0.1104 0.7981 0.055 Uiso 1 1 calc R . .
H7C H 0.1483 -0.0204 0.7773 0.055 Uiso 1 1 calc R . .
C8 C 0.12187(15) 0.0502(2) 0.51237(13) 0.0300(6) Uani 1 1 d . . .
H8 H 0.0694 0.0496 0.4966 0.036 Uiso 1 1 calc R . .
N1 N 0.14519(12) 0.0330(2) 0.46483(10) 0.0302(5) Uani 1 1 d . . .
C9 C 0.09061(16) 0.0061(3) 0.38945(14) 0.0422(7) Uani 1 1 d . . .
H9A H 0.0894 0.0676 0.3571 0.051 Uiso 1 1 calc R . .
H9B H 0.0397 -0.0031 0.3851 0.051 Uiso 1 1 calc R . .
C10 C 0.11693(15) -0.1051(3) 0.36954(14) 0.0415(7) Uani 1 1 d . . .
H10A H 0.1133 -0.1672 0.3992 0.050 Uiso 1 1 calc R . .
H10B H 0.0836 -0.1232 0.3187 0.050 Uiso 1 1 calc R . .
N2 N 0.19715(12) -0.0956(2) 0.38122(11) 0.0321(5) Uani 1 1 d . . .
C11 C 0.23278(16) -0.2115(2) 0.39268(14) 0.0352(6) Uani 1 1 d . . .
H11A H 0.2321 -0.2456 0.4354 0.042 Uiso 1 1 calc R . .
H11B H 0.2859 -0.2020 0.4035 0.042 Uiso 1 1 calc R . .
C12 C 0.19562(19) -0.2958(3) 0.32923(17) 0.0483(8) Uani 1 1 d . . .
H12A H 0.2215 -0.3685 0.3429 0.072 Uiso 1 1 calc R . .
H12B H 0.1992 -0.2661 0.2874 0.072 Uiso 1 1 calc R . .
H12C H 0.1428 -0.3058 0.3174 0.072 Uiso 1 1 calc R . .
C13 C 0.19818(17) -0.0368(3) 0.31744(14) 0.0405(7) Uani 1 1 d . . .
H13A H 0.1765 0.0394 0.3129 0.049 Uiso 1 1 calc R . .
H13B H 0.1658 -0.0793 0.2734 0.049 Uiso 1 1 calc R . .
C14 C 0.27680(18) -0.0260(3) 0.32262(16) 0.0445(7) Uani 1 1 d . . .
H14A H 0.2733 0.0125 0.2799 0.067 Uiso 1 1 calc R . .
H14B H 0.2983 -0.1012 0.3259 0.067 Uiso 1 1 calc R . .
H14C H 0.3090 0.0176 0.3654 0.067 Uiso 1 1 calc R . .
C15 C 0.36833(15) 0.1635(2) 0.73352(13) 0.0319(6) Uani 1 1 d . . .
H15 H 0.3908 0.1652 0.7843 0.038 Uiso 1 1 calc R . .
N3 N 0.40942(12) 0.1956(2) 0.70372(11) 0.0322(5) Uani 1 1 d . . .
C16 C 0.48628(16) 0.2420(3) 0.75132(15) 0.0437(7) Uani 1 1 d . . .
H16A H 0.5131 0.1909 0.7925 0.052 Uiso 1 1 calc R . .
H16B H 0.4817 0.3166 0.7701 0.052 Uiso 1 1 calc R . .
C17 C 0.53096(17) 0.2536(3) 0.70824(16) 0.0449(7) Uani 1 1 d . . .
H17A H 0.5765 0.2994 0.7359 0.054 Uiso 1 1 calc R . .
H17B H 0.5471 0.1781 0.7008 0.054 Uiso 1 1 calc R . .
N4 N 0.48442(13) 0.3087(2) 0.63635(12) 0.0341(5) Uani 1 1 d . . .
C18 C 0.52374(17) 0.2929(3) 0.58972(17) 0.0441(7) Uani 1 1 d . . .
H18A H 0.4901 0.3208 0.5410 0.053 Uiso 1 1 calc R . .
H18B H 0.5311 0.2112 0.5858 0.053 Uiso 1 1 calc R . .
C19 C 0.60090(19) 0.3527(3) 0.6163(2) 0.0565(9) Uani 1 1 d . . .
H19A H 0.6194 0.3425 0.5809 0.085 Uiso 1 1 calc R . .
H19B H 0.6367 0.3199 0.6621 0.085 Uiso 1 1 calc R . .
H19C H 0.5951 0.4333 0.6226 0.085 Uiso 1 1 calc R . .
C20 C 0.47273(17) 0.4325(3) 0.64644(18) 0.0462(7) Uani 1 1 d . . .
H20A H 0.5219 0.4660 0.6789 0.055 Uiso 1 1 calc R . .
H20B H 0.4404 0.4382 0.6705 0.055 Uiso 1 1 calc R . .
C21 C 0.4373(2) 0.5024(3) 0.5776(2) 0.0549(9) Uani 1 1 d . . .
H21A H 0.4215 0.5755 0.5875 0.082 Uiso 1 1 calc R . .
H21B H 0.3937 0.4624 0.5414 0.082 Uiso 1 1 calc R . .
H21C H 0.4742 0.5139 0.5597 0.082 Uiso 1 1 calc R . .
O2 O 0.30747(10) 0.35137(15) 0.58711(9) 0.0318(4) Uani 1 1 d . . .
C22 C 0.23941(14) 0.3471(2) 0.54066(12) 0.0275(5) Uani 1 1 d . . .
H22 H 0.2185 0.2751 0.5231 0.033 Uiso 1 1 calc R . .
N5 N 0.19441(12) 0.43760(18) 0.51424(11) 0.0288(5) Uani 1 1 d . . .
C23 C 0.11395(16) 0.4239(3) 0.46147(15) 0.0415(7) Uani 1 1 d . . .
H23A H 0.0824 0.4600 0.4799 0.062 Uiso 1 1 calc R . .
H23B H 0.1017 0.3435 0.4537 0.062 Uiso 1 1 calc R . .
H23C H 0.1048 0.4591 0.4160 0.062 Uiso 1 1 calc R . .
C24 C 0.22262(17) 0.5540(2) 0.53526(16) 0.0400(7) Uani 1 1 d . . .
H24A H 0.2102 0.5991 0.4922 0.060 Uiso 1 1 calc R . .
H24B H 0.2771 0.5523 0.5647 0.060 Uiso 1 1 calc R . .
H24C H 0.1992 0.5875 0.5627 0.060 Uiso 1 1 calc R . .
O3 O 0.35884(10) -0.04105(16) 0.50603(9) 0.0306(4) Uani 1 1 d . . .
O4 O 0.44212(10) 0.06531(16) 0.60044(9) 0.0326(4) Uani 1 1 d . . .
C25 C 0.42355(15) -0.0206(2) 0.55890(14) 0.0311(6) Uani 1 1 d . . .
C26 C 0.48558(17) -0.1091(3) 0.57218(17) 0.0467(8) Uani 1 1 d . . .
H26A H 0.4613 -0.1805 0.5485 0.056 Uiso 1 1 calc R . .
H26B H 0.5161 -0.0823 0.5492 0.056 Uiso 1 1 calc R . .
C27 C 0.5366(2) -0.1326(4) 0.6493(2) 0.0758(13) Uani 1 1 d . . .
H27A H 0.5739 -0.1891 0.6531 0.114 Uiso 1 1 calc R . .
H27B H 0.5072 -0.1612 0.6724 0.114 Uiso 1 1 calc R . .
H27C H 0.5622 -0.0630 0.6731 0.114 Uiso 1 1 calc R . .
O5 O 0.24545(11) 0.14875(16) 0.42380(9) 0.0348(4) Uani 1 1 d . . .
O6 O 0.35473(11) 0.24261(16) 0.49189(9) 0.0352(4) Uani 1 1 d . . .
C28 C 0.29553(17) 0.2230(2) 0.43332(14) 0.0342(6) Uani 1 1 d . C .
C29 C 0.2803(2) 0.2962(3) 0.36711(16) 0.0502(8) Uani 1 1 d D . .
H29A H 0.2668 0.2481 0.3248 0.060 Uiso 0.70 1 d P A 1
H29B H 0.3271 0.3380 0.3759 0.060 Uiso 0.70 1 d P B 1
C30 C 0.2177(3) 0.3829(5) 0.3522(3) 0.0612(13) Uiso 0.70 1 d PD C 1
H30A H 0.1723 0.3437 0.3464 0.092 Uiso 0.70 1 calc PR C 1
H30B H 0.2072 0.4246 0.3084 0.092 Uiso 0.70 1 calc PR C 1
H30C H 0.2340 0.4356 0.3925 0.092 Uiso 0.70 1 calc PR C 1
H29C H 0.2286 0.3240 0.3459 0.073 Uiso 0.30 1 d P D 2
H29D H 0.2860 0.2487 0.3313 0.073 Uiso 0.30 1 d P E 2
C30' C 0.3278(7) 0.3956(9) 0.3808(7) 0.061(3) Uiso 0.30 1 d PD C 2
H30D H 0.3128 0.4528 0.4054 0.092 Uiso 0.30 1 calc PR C 2
H30E H 0.3223 0.4260 0.3353 0.092 Uiso 0.30 1 calc PR C 2
H30F H 0.3802 0.3747 0.4110 0.092 Uiso 0.30 1 calc PR C 2
O7 O 0.25395(10) -0.14394(15) 0.54488(9) 0.0295(4) Uani 1 1 d . . .
H7X H 0.2123 -0.1468 0.5484 0.035 Uiso 1 1 d . . .
H7Y H 0.2914 -0.1403 0.5877 0.035 Uiso 1 1 d . . .
O8 O 0.36669(11) -0.15661(18) 0.68170(10) 0.0380(5) Uani 1 1 d . . .
C31 C 0.34121(15) -0.1462(2) 0.72585(13) 0.0304(6) Uani 1 1 d . . .
H31 H 0.2883 -0.1470 0.7076 0.037 Uiso 1 1 calc R . .
N6 N 0.38315(12) -0.1338(2) 0.79742(11) 0.0339(5) Uani 1 1 d . . .
C32 C 0.34928(18) -0.1257(2) 0.84675(15) 0.0402(7) Uani 1 1 d . . .
H32A H 0.3629 -0.0534 0.8720 0.060 Uiso 1 1 calc R . .
H32B H 0.3679 -0.1874 0.8815 0.060 Uiso 1 1 calc R . .
H32C H 0.2946 -0.1309 0.8193 0.060 Uiso 1 1 calc R . .
C33 C 0.46552(18) -0.1279(4) 0.82898(18) 0.0727(12) Uani 1 1 d . . .
H33A H 0.4835 -0.0609 0.8594 0.109 Uiso 1 1 calc R . .
H33B H 0.4804 -0.1234 0.7906 0.109 Uiso 1 1 calc R . .
H33C H 0.4875 -0.1954 0.8578 0.109 Uiso 1 1 calc R . .
Cl1 Cl 0.06920(4) -0.24678(5) 0.55902(3) 0.03073(15) Uani 1 1 d . . .
O9 O 0.14966(11) -0.22120(17) 0.59989(10) 0.0385(4) Uani 1 1 d . . .
O10 O 0.04038(13) -0.1990(2) 0.48713(11) 0.0532(6) Uani 1 1 d . . .
O11 O 0.02894(11) -0.19664(18) 0.59525(11) 0.0428(5) Uani 1 1 d . . .
O12 O 0.05894(13) -0.36854(19) 0.55562(15) 0.0575(6) 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 N1 1.992(2) . ?
Ni1 O3 1.9969(18) . ?
Ni1 O5 2.0417(19) . ?
Ni1 O1 2.0499(16) . ?
Ni1 O7 2.1376(18) . ?
Ni1 N2 2.250(2) . ?
Ni2 N3 2.010(2) . ?
Ni2 O6 2.0274(18) . ?
Ni2 O4 2.0328(18) . ?
Ni2 O1 2.0498(18) . ?
Ni2 O2 2.1500(18) . ?
Ni2 N4 2.214(2) . ?
O1 C1 1.320(3) . ?
C1 C6 1.420(3) . ?
C1 C2 1.430(3) . ?
C2 C3 1.400(4) . ?
C2 C15 1.452(4) . ?
C3 C4 1.374(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.386(3) . ?
C4 C7 1.522(4) . ?
C5 C6 1.391(3) . ?
C5 H5 0.9300 . ?
C6 C8 1.459(3) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 N1 1.273(3) . ?
C8 H8 0.9300 . ?
N1 C9 1.460(3) . ?
C9 C10 1.517(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.487(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
N2 C11 1.487(4) . ?
N2 C13 1.489(3) . ?
C11 C12 1.526(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.506(4) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 N3 1.274(3) . ?
C15 H15 0.9300 . ?
N3 C16 1.476(3) . ?
C16 C17 1.514(4) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 N4 1.482(4) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
N4 C20 1.487(4) . ?
N4 C18 1.495(4) . ?
C18 C19 1.524(4) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 C21 1.501(5) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
O2 C22 1.239(3) . ?
C22 N5 1.321(3) . ?
C22 H22 0.9300 . ?
N5 C24 1.452(4) . ?
N5 C23 1.461(3) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
O3 C25 1.262(3) . ?
O4 C25 1.256(3) . ?
C25 C26 1.522(4) . ?
C26 C27 1.465(5) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
O5 C28 1.256(3) . ?
O6 C28 1.255(3) . ?
C28 C29 1.517(4) . ?
C29 C30' 1.430(8) . ?
C29 C30 1.509(5) . ?
C29 H29A 0.966(3) . ?
C29 H29B 0.981(4) . ?
C29 H29C 0.960(3) . ?
C29 H29D 0.969(3) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C30 H29C 0.747(5) . ?
C30' H29B 0.677(10) . ?
C30' H30D 0.9600 . ?
C30' H30E 0.9600 . ?
C30' H30F 0.9600 . ?
O7 H7X 0.8543(17) . ?
O7 H7Y 0.8528(16) . ?
O8 C31 1.229(3) . ?
C31 N6 1.326(3) . ?
C31 H31 0.9300 . ?
N6 C33 1.444(4) . ?
N6 C32 1.450(4) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
Cl1 O12 1.428(2) . ?
Cl1 O10 1.433(2) . ?
Cl1 O11 1.4370(19) . ?
Cl1 O9 1.442(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
N1 Ni1 O3 172.52(9) . . ?
N1 Ni1 O5 88.60(9) . . ?
O3 Ni1 O5 97.72(8) . . ?
N1 Ni1 O1 87.67(7) . . ?
O3 Ni1 O1 96.07(7) . . ?
O5 Ni1 O1 91.80(7) . . ?
N1 Ni1 O7 88.36(8) . . ?
O3 Ni1 O7 85.17(7) . . ?
O5 Ni1 O7 176.28(7) . . ?
O1 Ni1 O7 90.23(7) . . ?
N1 Ni1 N2 82.46(8) . . ?
O3 Ni1 N2 93.68(7) . . ?
O5 Ni1 N2 88.44(8) . . ?
O1 Ni1 N2 170.12(7) . . ?
O7 Ni1 N2 89.03(8) . . ?
N3 Ni2 O6 170.14(9) . . ?
N3 Ni2 O4 92.20(8) . . ?
O6 Ni2 O4 93.04(7) . . ?
N3 Ni2 O1 88.27(8) . . ?
O6 Ni2 O1 99.92(7) . . ?
O4 Ni2 O1 91.63(7) . . ?
N3 Ni2 O2 89.94(8) . . ?
O6 Ni2 O2 85.03(7) . . ?
O4 Ni2 O2 177.52(7) . . ?
O1 Ni2 O2 87.17(7) . . ?
N3 Ni2 N4 82.00(9) . . ?
O6 Ni2 N4 89.86(8) . . ?
O4 Ni2 N4 87.80(8) . . ?
O1 Ni2 N4 170.22(7) . . ?
O2 Ni2 N4 93.75(8) . . ?
C1 O1 Ni2 125.96(15) . . ?
C1 O1 Ni1 122.84(15) . . ?
Ni2 O1 Ni1 111.19(8) . . ?
O1 C1 C6 122.0(2) . . ?
O1 C1 C2 121.6(2) . . ?
C6 C1 C2 116.4(2) . . ?
C3 C2 C1 120.0(2) . . ?
C3 C2 C15 115.9(2) . . ?
C1 C2 C15 124.1(2) . . ?
C4 C3 C2 122.9(2) . . ?
C4 C3 H3 118.5 . . ?
C2 C3 H3 118.5 . . ?
C3 C4 C5 117.1(2) . . ?
C3 C4 C7 122.2(2) . . ?
C5 C4 C7 120.7(2) . . ?
C4 C5 C6 122.7(2) . . ?
C4 C5 H5 118.6 . . ?
C6 C5 H5 118.6 . . ?
C5 C6 C1 120.6(2) . . ?
C5 C6 C8 115.6(2) . . ?
C1 C6 C8 123.8(2) . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 C6 124.6(2) . . ?
N1 C8 H8 117.7 . . ?
C6 C8 H8 117.7 . . ?
C8 N1 C9 120.2(2) . . ?
C8 N1 Ni1 125.95(17) . . ?
C9 N1 Ni1 112.68(16) . . ?
N1 C9 C10 107.1(2) . . ?
N1 C9 H9A 110.3 . . ?
C10 C9 H9A 110.3 . . ?
N1 C9 H9B 110.3 . . ?
C10 C9 H9B 110.3 . . ?
H9A C9 H9B 108.6 . . ?
N2 C10 C9 111.2(2) . . ?
N2 C10 H10A 109.4 . . ?
C9 C10 H10A 109.4 . . ?
N2 C10 H10B 109.4 . . ?
C9 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
C10 N2 C11 110.3(2) . . ?
C10 N2 C13 109.5(2) . . ?
C11 N2 C13 111.1(2) . . ?
C10 N2 Ni1 102.39(14) . . ?
C11 N2 Ni1 109.82(15) . . ?
C13 N2 Ni1 113.44(18) . . ?
N2 C11 C12 116.1(2) . . ?
N2 C11 H11A 108.3 . . ?
C12 C11 H11A 108.3 . . ?
N2 C11 H11B 108.3 . . ?
C12 C11 H11B 108.3 . . ?
H11A C11 H11B 107.4 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N2 C13 C14 113.9(2) . . ?
N2 C13 H13A 108.8 . . ?
C14 C13 H13A 108.8 . . ?
N2 C13 H13B 108.8 . . ?
C14 C13 H13B 108.8 . . ?
H13A C13 H13B 107.7 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N3 C15 C2 125.9(2) . . ?
N3 C15 H15 117.0 . . ?
C2 C15 H15 117.0 . . ?
C15 N3 C16 118.0(2) . . ?
C15 N3 Ni2 127.31(18) . . ?
C16 N3 Ni2 114.39(18) . . ?
N3 C16 C17 109.6(2) . . ?
N3 C16 H16A 109.7 . . ?
C17 C16 H16A 109.7 . . ?
N3 C16 H16B 109.7 . . ?
C17 C16 H16B 109.7 . . ?
H16A C16 H16B 108.2 . . ?
N4 C17 C16 111.4(2) . . ?
N4 C17 H17A 109.3 . . ?
C16 C17 H17A 109.3 . . ?
N4 C17 H17B 109.3 . . ?
C16 C17 H17B 109.3 . . ?
H17A C17 H17B 108.0 . . ?
C17 N4 C20 110.1(2) . . ?
C17 N4 C18 108.9(2) . . ?
C20 N4 C18 111.5(2) . . ?
C17 N4 Ni2 100.51(18) . . ?
C20 N4 Ni2 113.48(17) . . ?
C18 N4 Ni2 111.74(17) . . ?
N4 C18 C19 115.9(3) . . ?
N4 C18 H18A 108.3 . . ?
C19 C18 H18A 108.3 . . ?
N4 C18 H18B 108.3 . . ?
C19 C18 H18B 108.3 . . ?
H18A C18 H18B 107.4 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N4 C20 C21 115.3(3) . . ?
N4 C20 H20A 108.5 . . ?
C21 C20 H20A 108.5 . . ?
N4 C20 H20B 108.5 . . ?
C21 C20 H20B 108.5 . . ?
H20A C20 H20B 107.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C22 O2 Ni2 117.61(16) . . ?
O2 C22 N5 124.6(2) . . ?
O2 C22 H22 117.7 . . ?
N5 C22 H22 117.7 . . ?
C22 N5 C24 121.9(2) . . ?
C22 N5 C23 120.8(2) . . ?
C24 N5 C23 117.3(2) . . ?
N5 C23 H23A 109.5 . . ?
N5 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N5 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N5 C24 H24A 109.5 . . ?
N5 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N5 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C25 O3 Ni1 132.11(16) . . ?
C25 O4 Ni2 128.85(16) . . ?
O4 C25 O3 126.9(2) . . ?
O4 C25 C26 117.2(2) . . ?
O3 C25 C26 115.9(2) . . ?
C27 C26 C25 114.6(3) . . ?
C27 C26 H26A 108.6 . . ?
C25 C26 H26A 108.6 . . ?
C27 C26 H26B 108.6 . . ?
C25 C26 H26B 108.6 . . ?
H26A C26 H26B 107.6 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C28 O5 Ni1 128.86(16) . . ?
C28 O6 Ni2 129.84(19) . . ?
O6 C28 O5 126.2(2) . . ?
O6 C28 C29 118.4(3) . . ?
O5 C28 C29 115.3(2) . . ?
C30' C29 C30 84.2(6) . . ?
C30' C29 C28 115.7(6) . . ?
C30 C29 C28 111.4(3) . . ?
C30' C29 H29A 122.1(6) . . ?
C30 C29 H29A 110.1(3) . . ?
C28 C29 H29A 110.2(3) . . ?
C30' C29 H29B 24.7(5) . . ?
C30 C29 H29B 108.4(3) . . ?
C28 C29 H29B 109.2(3) . . ?
H29A C29 H29B 107.5(3) . . ?
C30' C29 H29C 106.1(6) . . ?
C30 C29 H29C 24.3(2) . . ?
C28 C29 H29C 109.3(3) . . ?
H29A C29 H29C 89.3(3) . . ?
H29B C29 H29C 128.8(3) . . ?
C30' C29 H29D 108.5(6) . . ?
C30 C29 H29D 126.5(3) . . ?
C28 C29 H29D 108.7(3) . . ?
H29A C29 H29D 20.16(7) . . ?
H29B C29 H29D 89.8(3) . . ?
H29C C29 H29D 108.3(3) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
C29 C30 H29C 31.9(3) . . ?
H30A C30 H29C 82.3 . . ?
H30B C30 H29C 104.8 . . ?
H30C C30 H29C 136.7 . . ?
C29 C30' H29B 37.3(6) . . ?
C29 C30' H30D 109.5 . . ?
C29 C30' H30E 109.5 . . ?
H30D C30' H30E 109.5 . . ?
C29 C30' H30F 109.5 . . ?
H30D C30' H30F 109.5 . . ?
H30E C30' H30F 109.5 . . ?
Ni1 O7 H7X 109.04(14) . . ?
Ni1 O7 H7Y 109.13(15) . . ?
H7X O7 H7Y 108.79(18) . . ?
O8 C31 N6 125.2(2) . . ?
O8 C31 H31 117.4 . . ?
N6 C31 H31 117.4 . . ?
C31 N6 C33 120.2(3) . . ?
C31 N6 C32 122.3(2) . . ?
C33 N6 C32 117.5(2) . . ?
N6 C32 H32A 109.5 . . ?
N6 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N6 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N6 C33 H33A 109.5 . . ?
N6 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N6 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O12 Cl1 O10 110.74(15) . . ?
O12 Cl1 O11 109.20(14) . . ?
O10 Cl1 O11 109.13(13) . . ?
O12 Cl1 O9 109.02(13) . . ?
O10 Cl1 O9 109.37(13) . . ?
O11 Cl1 O9 109.36(12) . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.929
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.069
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_complex_3a
_database_code_depnum_ccdc_archive 'CCDC 1402080'
_audit_update_record             
;
2015-11-03 deposited with the CCDC.
2015-12-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H45 N7 Ni2 O4 S2'
_chemical_formula_sum            'C28 H45 N7 Ni2 O4 S2'
_chemical_formula_weight         725.25

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'
S S 0.1246 0.1234 '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   Fdd2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   17.461(3)
_cell_length_b                   67.604(9)
_cell_length_c                   12.0678(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     14246(3)
_cell_formula_units_Z            16
_cell_measurement_temperature    295
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            'light green'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6112
_exptl_absorpt_coefficient_mu    1.215
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.615
_exptl_absorpt_correction_T_max  0.750
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      295
_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       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            36794
_diffrn_reflns_av_R_equivalents  0.1302
_diffrn_reflns_av_sigmaI/netI    0.0930
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -78
_diffrn_reflns_limit_k_max       80
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.07
_diffrn_reflns_theta_max         25.25
_reflns_number_total             6317
_reflns_number_gt                3474
_reflns_threshold_expression     I>2sigma(I)

_computing_data_collection       'Brucker SMART'
_computing_cell_refinement       'Brucker SMART'
_computing_data_reduction        'Brucker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Diamond
_computing_publication_material  
'SHELXL-97 (Sheldrick, 1997), PLATON (Spek, 2009)'
_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)+(0.0001P)²+170.0925P] 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   0.00
_refine_ls_number_reflns         6317
_refine_ls_number_parameters     392
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.1745
_refine_ls_R_factor_gt           0.0874
_refine_ls_wR_factor_ref         0.1526
_refine_ls_wR_factor_gt          0.1206
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_restrained_S_all      1.130
_refine_ls_shift/su_max          0.002
_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 -0.04711(8) 0.16813(2) 0.48827(12) 0.0669(4) Uani 1 1 d . A .
Ni2 Ni 0.07165(9) 0.19788(2) 0.57541(15) 0.0804(5) Uani 1 1 d . A .
O1 O 0.0689(4) 0.17251(10) 0.4863(8) 0.075(2) Uani 1 1 d . . .
C1 C 0.1228(7) 0.15964(17) 0.4636(9) 0.064(3) Uani 1 1 d . . .
C2 C 0.2024(7) 0.16451(16) 0.4857(11) 0.073(3) Uani 1 1 d . . .
C3 C 0.2592(8) 0.1516(2) 0.4500(10) 0.086(4) Uani 1 1 d . . .
H3 H 0.3099 0.1555 0.4581 0.103 Uiso 1 1 calc R . .
C4 C 0.2452(8) 0.1335(2) 0.4037(11) 0.080(3) Uani 1 1 d . . .
C5 C 0.1699(8) 0.1281(2) 0.3922(9) 0.084(4) Uani 1 1 d . . .
H5 H 0.1589 0.1159 0.3605 0.100 Uiso 1 1 calc R . .
C6 C 0.1072(7) 0.14043(18) 0.4271(10) 0.072(3) Uani 1 1 d . . .
C7 C 0.3098(8) 0.1203(2) 0.3646(10) 0.111(5) Uani 1 1 d . . .
H7A H 0.3509 0.1207 0.4175 0.167 Uiso 1 1 calc R . .
H7B H 0.3280 0.1248 0.2941 0.167 Uiso 1 1 calc R . .
H7C H 0.2915 0.1069 0.3576 0.167 Uiso 1 1 calc R . .
C8 C 0.0330(8) 0.13172(18) 0.4223(9) 0.075(3) Uani 1 1 d . . .
H8 H 0.0303 0.1189 0.3940 0.090 Uiso 1 1 calc R . .
N1 N -0.0302(6) 0.13953(15) 0.4525(7) 0.072(3) Uani 1 1 d . . .
C9 C -0.1002(7) 0.12799(18) 0.4570(11) 0.089(4) Uani 1 1 d . . .
H9A H -0.1075 0.1229 0.5314 0.107 Uiso 1 1 calc R . .
H9B H -0.0963 0.1168 0.4068 0.107 Uiso 1 1 calc R . .
C10 C -0.1672(8) 0.1407(2) 0.4252(13) 0.112(5) Uani 1 1 d . . .
H10A H -0.1641 0.1439 0.3469 0.135 Uiso 1 1 calc R . .
H10B H -0.2143 0.1334 0.4374 0.135 Uiso 1 1 calc R . .
N2 N -0.1689(5) 0.15935(14) 0.4912(9) 0.073(3) Uani 1 1 d . . .
C11 C -0.1993(8) 0.1562(2) 0.6013(12) 0.108(5) Uani 1 1 d . . .
H11A H -0.1656 0.1471 0.6398 0.130 Uiso 1 1 calc R . .
H11B H -0.2488 0.1498 0.5943 0.130 Uiso 1 1 calc R . .
C12 C -0.2089(9) 0.1741(2) 0.6716(13) 0.133(6) Uani 1 1 d . . .
H12A H -0.2549 0.1729 0.7148 0.200 Uiso 1 1 calc R . .
H12B H -0.2125 0.1856 0.6252 0.200 Uiso 1 1 calc R . .
H12C H -0.1657 0.1754 0.7202 0.200 Uiso 1 1 calc R . .
C13 C -0.2201(7) 0.1731(2) 0.4271(12) 0.109(5) Uani 1 1 d . . .
H13A H -0.2177 0.1860 0.4623 0.130 Uiso 1 1 calc R . .
H13B H -0.1985 0.1746 0.3534 0.130 Uiso 1 1 calc R . .
C14 C -0.3023(8) 0.1678(2) 0.4142(13) 0.137(6) Uani 1 1 d . . .
H14A H -0.3264 0.1769 0.3640 0.206 Uiso 1 1 calc R . .
H14B H -0.3273 0.1684 0.4850 0.206 Uiso 1 1 calc R . .
H14C H -0.3064 0.1546 0.3854 0.206 Uiso 1 1 calc R . .
C15 C 0.2282(8) 0.1818(2) 0.5497(13) 0.100(5) Uani 1 1 d . A .
H15 H 0.2807 0.1838 0.5568 0.120 Uiso 1 1 calc R . .
N5 N 0.1838(5) 0.19404(15) 0.5958(10) 0.095(4) Uani 1 1 d D . .
C16 C 0.2107(13) 0.2082(3) 0.6788(16) 0.105(5) Uiso 0.60 1 d PD A 1
H16A H 0.2660 0.2094 0.6794 0.125 Uiso 0.60 1 calc PR A 1
H16B H 0.1924 0.2050 0.7526 0.125 Uiso 0.60 1 calc PR A 1
C17 C 0.1713(10) 0.2268(4) 0.630(3) 0.105(5) Uiso 0.40 1 d PD A 1
H17A H 0.1942 0.2388 0.6594 0.125 Uiso 0.40 1 calc PR A 1
H17B H 0.1744 0.2270 0.5502 0.125 Uiso 0.40 1 calc PR A 1
C16' C 0.2263(12) 0.2107(3) 0.640(3) 0.105(5) Uiso 0.40 1 d PD A 2
H16C H 0.2583 0.2162 0.5814 0.125 Uiso 0.40 1 calc PR A 2
H16D H 0.2597 0.2061 0.6985 0.125 Uiso 0.40 1 calc PR A 2
C17' C 0.1735(8) 0.2268(3) 0.6845(19) 0.105(5) Uiso 0.60 1 d PD A 2
H17C H 0.1825 0.2279 0.7636 0.125 Uiso 0.60 1 calc PR A 2
H17D H 0.1893 0.2393 0.6517 0.125 Uiso 0.60 1 calc PR A 2
N6 N 0.0916(7) 0.22478(16) 0.6676(12) 0.103(4) Uani 1 1 d D . .
C18 C 0.0677(12) 0.2237(2) 0.7818(16) 0.143(7) Uani 1 1 d . A .
H18A H 0.0880 0.2354 0.8188 0.172 Uiso 1 1 calc R . .
H18B H 0.0928 0.2124 0.8144 0.172 Uiso 1 1 calc R . .
C19 C -0.0164(11) 0.2224(2) 0.8111(17) 0.156(7) Uani 1 1 d . . .
H19A H -0.0222 0.2154 0.8799 0.234 Uiso 1 1 calc R A .
H19B H -0.0432 0.2154 0.7536 0.234 Uiso 1 1 calc R . .
H19C H -0.0373 0.2355 0.8185 0.234 Uiso 1 1 calc R . .
C20 C 0.0552(8) 0.24274(16) 0.6187(13) 0.121(6) Uani 1 1 d . A .
H20A H 0.0003 0.2407 0.6178 0.146 Uiso 1 1 calc R . .
H20B H 0.0719 0.2438 0.5422 0.146 Uiso 1 1 calc R . .
C21 C 0.0706(10) 0.26249(18) 0.6750(19) 0.188(10) Uani 1 1 d . . .
H21A H 0.0848 0.2721 0.6202 0.282 Uiso 1 1 calc R A .
H21B H 0.1116 0.2610 0.7274 0.282 Uiso 1 1 calc R . .
H21C H 0.0253 0.2668 0.7128 0.282 Uiso 1 1 calc R . .
N3 N -0.0558(6) 0.17514(16) 0.3239(9) 0.089(3) Uani 1 1 d . . .
C22 C -0.0582(6) 0.17750(16) 0.2314(11) 0.068(3) Uani 1 1 d . . .
S1 S -0.0612(2) 0.18057(5) 0.0966(3) 0.0946(11) Uani 1 1 d . . .
N4 N -0.0448(6) 0.19905(15) 0.5298(8) 0.079(3) Uani 1 1 d . . .
C23 C -0.0908(7) 0.21109(18) 0.5158(10) 0.075(4) Uani 1 1 d . A .
S2 S -0.1566(2) 0.22858(5) 0.4999(4) 0.1225(15) Uani 1 1 d . . .
O2 O -0.0364(4) 0.16043(11) 0.6510(6) 0.072(2) Uani 1 1 d . . .
O3 O 0.0482(5) 0.18203(11) 0.7141(7) 0.082(2) Uani 1 1 d . . .
C24 C 0.0042(7) 0.16790(18) 0.7260(11) 0.073(3) Uani 1 1 d . A .
C25 C -0.0032(8) 0.1584(2) 0.8377(10) 0.108(5) Uani 1 1 d . . .
H25A H -0.0514 0.1516 0.8423 0.162 Uiso 1 1 calc R A .
H25B H -0.0009 0.1684 0.8942 0.162 Uiso 1 1 calc R . .
H25C H 0.0378 0.1491 0.8482 0.162 Uiso 1 1 calc R . .
O4 O 0.1030(6) 0.21421(14) 0.4319(10) 0.111(3) Uani 1 1 d . . .
C26 C 0.0935(8) 0.2093(2) 0.3319(16) 0.108(5) Uani 1 1 d . A .
H26 H 0.0566 0.1998 0.3157 0.129 Uiso 1 1 calc R . .
N7 N 0.1321(7) 0.21681(17) 0.2509(12) 0.103(4) Uani 1 1 d . . .
C27 C 0.1200(9) 0.2124(3) 0.1355(15) 0.144(7) Uani 1 1 d . A .
H27A H 0.1668 0.2077 0.1035 0.217 Uiso 1 1 calc R . .
H27B H 0.1041 0.2242 0.0976 0.217 Uiso 1 1 calc R . .
H27C H 0.0810 0.2025 0.1285 0.217 Uiso 1 1 calc R . .
C28 C 0.1899(10) 0.2320(3) 0.2721(17) 0.228(18) Uani 1 1 d . A .
H28A H 0.208(12) 0.236(3) 0.212(11) 0.343 Uiso 1 1 calc R . .
H28B H 0.225(10) 0.2272(15) 0.31(2) 0.343 Uiso 1 1 calc R . .
H28C H 0.170(5) 0.241(2) 0.31(2) 0.343 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 2.003(10) . ?
Ni1 O2 2.041(8) . ?
Ni1 N3 2.045(11) . ?
Ni1 O1 2.047(7) . ?
Ni1 N4 2.150(10) . ?
Ni1 N2 2.209(9) . ?
Ni2 N5 1.990(9) . ?
Ni2 O1 2.025(8) . ?
Ni2 O3 2.029(8) . ?
Ni2 N4 2.108(10) . ?
Ni2 O4 2.126(11) . ?
Ni2 N6 2.161(11) . ?
O1 C1 1.311(12) . ?
C1 C6 1.398(15) . ?
C1 C2 1.453(14) . ?
C2 C3 1.390(15) . ?
C2 C15 1.470(17) . ?
C3 C4 1.367(16) . ?
C3 H3 0.9300 . ?
C4 C5 1.371(16) . ?
C4 C7 1.515(16) . ?
C5 C6 1.441(16) . ?
C5 H5 0.9300 . ?
C6 C8 1.424(16) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 N1 1.276(13) . ?
C8 H8 0.9300 . ?
N1 C9 1.451(13) . ?
C9 C10 1.501(16) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.494(15) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
N2 C11 1.447(15) . ?
N2 C13 1.504(14) . ?
C11 C12 1.488(17) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.489(16) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 N5 1.265(15) . ?
C15 H15 0.9300 . ?
N5 C16' 1.447(10) . ?
N5 C16 1.463(10) . ?
C16 C17 1.548(10) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 N6 1.467(10) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C16' C17' 1.530(10) . ?
C16' H16C 0.9700 . ?
C16' H16D 0.9700 . ?
C17' N6 1.451(10) . ?
C17' H17C 0.9700 . ?
C17' H17D 0.9700 . ?
N6 C18 1.441(19) . ?
N6 C20 1.492(15) . ?
C18 C19 1.51(2) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 C21 1.522(16) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
N3 C22 1.128(13) . ?
C22 S1 1.641(14) . ?
N4 C23 1.156(12) . ?
C23 S2 1.660(13) . ?
O2 C24 1.255(12) . ?
O3 C24 1.234(13) . ?
C24 C25 1.499(16) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
O4 C26 1.262(17) . ?
C26 N7 1.290(17) . ?
C26 H26 0.9300 . ?
N7 C27 1.439(18) . ?
N7 C28 1.462(17) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.8297 . ?
C28 H28B 0.8297 . ?
C28 H28C 0.8297 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 O2 87.0(3) . . ?
N1 Ni1 N3 91.5(4) . . ?
O2 Ni1 N3 178.3(5) . . ?
N1 Ni1 O1 89.5(4) . . ?
O2 Ni1 O1 87.5(3) . . ?
N3 Ni1 O1 91.6(4) . . ?
N1 Ni1 N4 170.4(4) . . ?
O2 Ni1 N4 91.3(3) . . ?
N3 Ni1 N4 90.1(4) . . ?
O1 Ni1 N4 81.0(3) . . ?
N1 Ni1 N2 83.5(4) . . ?
O2 Ni1 N2 90.3(4) . . ?
N3 Ni1 N2 90.4(4) . . ?
O1 Ni1 N2 172.7(3) . . ?
N4 Ni1 N2 106.0(4) . . ?
N5 Ni2 O1 88.8(4) . . ?
N5 Ni2 O3 91.6(4) . . ?
O1 Ni2 O3 89.2(3) . . ?
N5 Ni2 N4 170.4(5) . . ?
O1 Ni2 N4 82.5(3) . . ?
O3 Ni2 N4 92.3(3) . . ?
N5 Ni2 O4 85.1(5) . . ?
O1 Ni2 O4 90.8(4) . . ?
O3 Ni2 O4 176.7(4) . . ?
N4 Ni2 O4 90.9(4) . . ?
N5 Ni2 N6 83.5(4) . . ?
O1 Ni2 N6 172.0(4) . . ?
O3 Ni2 N6 93.0(4) . . ?
N4 Ni2 N6 105.0(4) . . ?
O4 Ni2 N6 86.6(5) . . ?
C1 O1 Ni2 131.0(7) . . ?
C1 O1 Ni1 128.1(6) . . ?
Ni2 O1 Ni1 98.0(3) . . ?
O1 C1 C6 122.8(10) . . ?
O1 C1 C2 119.9(10) . . ?
C6 C1 C2 117.1(11) . . ?
C3 C2 C1 118.9(11) . . ?
C3 C2 C15 116.3(11) . . ?
C1 C2 C15 124.7(12) . . ?
C4 C3 C2 124.1(13) . . ?
C4 C3 H3 117.9 . . ?
C2 C3 H3 117.9 . . ?
C3 C4 C5 116.9(13) . . ?
C3 C4 C7 121.5(13) . . ?
C5 C4 C7 121.6(13) . . ?
C4 C5 C6 123.0(12) . . ?
C4 C5 H5 118.5 . . ?
C6 C5 H5 118.5 . . ?
C1 C6 C8 125.1(12) . . ?
C1 C6 C5 118.8(11) . . ?
C8 C6 C5 116.1(12) . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 C6 127.1(12) . . ?
N1 C8 H8 116.5 . . ?
C6 C8 H8 116.5 . . ?
C8 N1 C9 121.1(11) . . ?
C8 N1 Ni1 126.1(8) . . ?
C9 N1 Ni1 112.7(8) . . ?
N1 C9 C10 109.9(10) . . ?
N1 C9 H9A 109.7 . . ?
C10 C9 H9A 109.7 . . ?
N1 C9 H9B 109.7 . . ?
C10 C9 H9B 109.7 . . ?
H9A C9 H9B 108.2 . . ?
N2 C10 C9 111.2(10) . . ?
N2 C10 H10A 109.4 . . ?
C9 C10 H10A 109.4 . . ?
N2 C10 H10B 109.4 . . ?
C9 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
C11 N2 C10 111.8(11) . . ?
C11 N2 C13 110.3(11) . . ?
C10 N2 C13 105.1(10) . . ?
C11 N2 Ni1 114.1(8) . . ?
C10 N2 Ni1 101.5(7) . . ?
C13 N2 Ni1 113.4(7) . . ?
N2 C11 C12 116.3(13) . . ?
N2 C11 H11A 108.2 . . ?
C12 C11 H11A 108.2 . . ?
N2 C11 H11B 108.2 . . ?
C12 C11 H11B 108.2 . . ?
H11A C11 H11B 107.4 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 N2 118.5(11) . . ?
C14 C13 H13A 107.7 . . ?
N2 C13 H13A 107.7 . . ?
C14 C13 H13B 107.7 . . ?
N2 C13 H13B 107.7 . . ?
H13A C13 H13B 107.1 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N5 C15 C2 124.3(13) . . ?
N5 C15 H15 117.9 . . ?
C2 C15 H15 117.9 . . ?
C15 N5 C16' 110.7(13) . . ?
C15 N5 C16 122.2(14) . . ?
C16' N5 C16 22.7(18) . . ?
C15 N5 Ni2 129.4(10) . . ?
C16' N5 Ni2 116.7(12) . . ?
C16 N5 Ni2 108.4(11) . . ?
N5 C16 C17 97.5(19) . . ?
N5 C16 H16A 112.3 . . ?
C17 C16 H16A 112.3 . . ?
N5 C16 H16B 112.3 . . ?
C17 C16 H16B 112.3 . . ?
H16A C16 H16B 109.9 . . ?
N6 C17 C16 103.3(16) . . ?
N6 C17 H17A 111.1 . . ?
C16 C17 H17A 111.1 . . ?
N6 C17 H17B 111.1 . . ?
C16 C17 H17B 111.1 . . ?
H17A C17 H17B 109.1 . . ?
N5 C16' C17' 112.0(17) . . ?
N5 C16' H16C 109.2 . . ?
C17' C16' H16C 109.2 . . ?
N5 C16' H16D 109.2 . . ?
C17' C16' H16D 109.2 . . ?
H16C C16' H16D 107.9 . . ?
N6 C17' C16' 118.4(18) . . ?
N6 C17' H17C 107.7 . . ?
C16' C17' H17C 107.7 . . ?
N6 C17' H17D 107.7 . . ?
C16' C17' H17D 107.7 . . ?
H17C C17' H17D 107.1 . . ?
C18 N6 C17' 99.0(15) . . ?
C18 N6 C17 125(2) . . ?
C17' N6 C17 25.9(16) . . ?
C18 N6 C20 107.1(13) . . ?
C17' N6 C20 113.5(14) . . ?
C17 N6 C20 101.9(13) . . ?
C18 N6 Ni2 113.9(9) . . ?
C17' N6 Ni2 108.2(11) . . ?
C17 N6 Ni2 94.3(16) . . ?
C20 N6 Ni2 114.4(9) . . ?
N6 C18 C19 120.5(16) . . ?
N6 C18 H18A 107.2 . . ?
C19 C18 H18A 107.2 . . ?
N6 C18 H18B 107.2 . . ?
C19 C18 H18B 107.2 . . ?
H18A C18 H18B 106.8 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N6 C20 C21 117.5(12) . . ?
N6 C20 H20A 107.9 . . ?
C21 C20 H20A 107.9 . . ?
N6 C20 H20B 107.9 . . ?
C21 C20 H20B 107.9 . . ?
H20A C20 H20B 107.2 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C22 N3 Ni1 174.3(12) . . ?
N3 C22 S1 179.1(13) . . ?
C23 N4 Ni2 137.3(9) . . ?
C23 N4 Ni1 129.6(9) . . ?
Ni2 N4 Ni1 92.4(4) . . ?
N4 C23 S2 178.2(12) . . ?
C24 O2 Ni1 130.0(8) . . ?
C24 O3 Ni2 129.1(8) . . ?
O3 C24 O2 125.3(13) . . ?
O3 C24 C25 119.4(11) . . ?
O2 C24 C25 115.3(11) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C26 O4 Ni2 127.6(10) . . ?
O4 C26 N7 123.6(15) . . ?
O4 C26 H26 118.2 . . ?
N7 C26 H26 118.2 . . ?
C26 N7 C27 125.2(14) . . ?
C26 N7 C28 120.2(15) . . ?
C27 N7 C28 114.5(14) . . ?
N7 C27 H27A 109.5 . . ?
N7 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N7 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N7 C28 H28A 109.5 . . ?
N7 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
N7 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.075
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_complex_3b
_database_code_depnum_ccdc_archive 'CCDC 1402081'
_audit_update_record             
;
2015-11-03 deposited with the CCDC.
2015-12-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H45 N11 Ni2 O4'
_chemical_formula_sum            'C26 H45 N11 Ni2 O4'
_chemical_formula_weight         693.15

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   10.3693(9)
_cell_length_b                   35.460(3)
_cell_length_c                   18.8761(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.288(2)
_cell_angle_gamma                90.00
_cell_volume                     6726.0(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    295
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            'light green'
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2928
_exptl_absorpt_coefficient_mu    1.167
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.650
_exptl_absorpt_correction_T_max  0.765
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      295
_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       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            69063
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.25
_diffrn_reflns_theta_max         26.68
_reflns_number_total             13925
_reflns_number_gt                8672
_reflns_threshold_expression     I>2sigma(I)

_computing_data_collection       'Brucker SMART'
_computing_cell_refinement       'Brucker SMART'
_computing_data_reduction        'Brucker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Diamond
_computing_publication_material  
'SHELXL-97 (Sheldrick, 1997), PLATON (Spek, 2009)'
_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)+(0.0625P)²+11.2732P] 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         13925
_refine_ls_number_parameters     776
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.1014
_refine_ls_R_factor_gt           0.0578
_refine_ls_wR_factor_ref         0.1679
_refine_ls_wR_factor_gt          0.1386
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.002
_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 0.48661(5) 0.392672(15) 0.34052(3) 0.04174(15) Uani 1 1 d . A .
Ni2 Ni 0.55354(5) 0.368583(15) 0.19936(3) 0.04161(15) Uani 1 1 d . A .
O1 O 0.5564(3) 0.34570(8) 0.29960(14) 0.0424(6) Uani 1 1 d . . .
C1 C 0.6361(4) 0.31965(12) 0.3356(2) 0.0462(10) Uani 1 1 d . . .
C2 C 0.7068(4) 0.29482(13) 0.2987(3) 0.0536(11) Uani 1 1 d . . .
C3 C 0.7806(5) 0.26512(15) 0.3375(3) 0.0692(14) Uani 1 1 d . . .
H3 H 0.8232 0.2487 0.3123 0.083 Uiso 1 1 calc R . .
C4 C 0.7938(6) 0.25891(17) 0.4103(3) 0.0781(16) Uani 1 1 d . . .
C5 C 0.7314(5) 0.28384(16) 0.4468(3) 0.0701(15) Uani 1 1 d . . .
H5 H 0.7405 0.2804 0.4966 0.084 Uiso 1 1 calc R . .
C6 C 0.6546(4) 0.31434(13) 0.4121(2) 0.0524(11) Uani 1 1 d . . .
C7 C 0.8761(8) 0.2259(2) 0.4505(4) 0.124(3) Uani 1 1 d . . .
H7A H 0.8883 0.2290 0.5022 0.186 Uiso 1 1 calc R . .
H7B H 0.9612 0.2253 0.4390 0.186 Uiso 1 1 calc R . .
H7C H 0.8301 0.2026 0.4353 0.186 Uiso 1 1 calc R . .
C8 C 0.6036(5) 0.33922(15) 0.4589(2) 0.0578(12) Uani 1 1 d . A .
H8 H 0.6180 0.3322 0.5077 0.069 Uiso 1 1 calc R . .
N1 N 0.5407(4) 0.36998(11) 0.44023(19) 0.0547(10) Uani 1 1 d D . .
C9 C 0.5231(9) 0.3975(3) 0.4955(5) 0.0635(14) Uiso 0.50 1 d PD A 1
H9A H 0.5986 0.4145 0.5077 0.076 Uiso 0.50 1 calc PR A 1
H9B H 0.5158 0.3846 0.5397 0.076 Uiso 0.50 1 calc PR A 1
C10 C 0.3947(9) 0.4196(3) 0.4623(5) 0.0635(14) Uiso 0.50 1 d PD A 1
H10A H 0.3199 0.4025 0.4471 0.076 Uiso 0.50 1 calc PR A 1
H10B H 0.3756 0.4373 0.4975 0.076 Uiso 0.50 1 calc PR A 1
C9' C 0.4803(11) 0.3877(2) 0.4947(5) 0.0635(14) Uiso 0.50 1 d PD A 2
H9'1 H 0.5330 0.3828 0.5440 0.076 Uiso 0.50 1 calc PR A 2
H9'2 H 0.3907 0.3784 0.4902 0.076 Uiso 0.50 1 calc PR A 2
C10' C 0.4790(11) 0.4294(2) 0.4772(4) 0.0635(14) Uiso 0.50 1 d PD A 2
H10C H 0.4298 0.4424 0.5073 0.076 Uiso 0.50 1 calc PR A 2
H10D H 0.5699 0.4386 0.4909 0.076 Uiso 0.50 1 calc PR A 2
N2 N 0.4199(4) 0.43976(11) 0.3987(2) 0.0587(10) Uani 1 1 d D . .
C11 C 0.5025(6) 0.47390(17) 0.4035(4) 0.091(2) Uani 1 1 d . A .
H11A H 0.4774 0.4910 0.4378 0.109 Uiso 1 1 calc R . .
H11B H 0.5944 0.4667 0.4241 0.109 Uiso 1 1 calc R . .
C12 C 0.4965(11) 0.4945(2) 0.3363(6) 0.164(5) Uani 1 1 d . . .
H12A H 0.5628 0.5140 0.3453 0.247 Uiso 1 1 calc R A .
H12B H 0.4099 0.5056 0.3193 0.247 Uiso 1 1 calc R . .
H12C H 0.5129 0.4775 0.2999 0.247 Uiso 1 1 calc R . .
C13 C 0.2811(6) 0.45006(19) 0.3661(5) 0.116(3) Uani 1 1 d . A .
H13A H 0.2271 0.4275 0.3638 0.139 Uiso 1 1 calc R . .
H13B H 0.2744 0.4581 0.3162 0.139 Uiso 1 1 calc R . .
C14 C 0.2203(7) 0.48085(18) 0.4042(5) 0.122(3) Uani 1 1 d . . .
H14A H 0.1281 0.4839 0.3797 0.183 Uiso 1 1 calc R A .
H14B H 0.2667 0.5042 0.4026 0.183 Uiso 1 1 calc R . .
H14C H 0.2280 0.4738 0.4542 0.183 Uiso 1 1 calc R . .
C15 C 0.7124(4) 0.29894(14) 0.2229(3) 0.0560(12) Uani 1 1 d . B .
H15 H 0.7516 0.2794 0.2030 0.067 Uiso 1 1 calc R . .
N3 N 0.6690(4) 0.32661(11) 0.18140(19) 0.0527(9) Uani 1 1 d D . .
C16 C 0.7008(12) 0.3329(4) 0.1092(5) 0.0718(15) Uiso 0.50 1 d PD B 1
H16A H 0.7262 0.3094 0.0902 0.086 Uiso 0.50 1 calc PR B 1
H16B H 0.7736 0.3507 0.1142 0.086 Uiso 0.50 1 calc PR B 1
C17 C 0.5730(10) 0.3488(2) 0.0578(6) 0.0718(15) Uiso 0.50 1 d PD B 1
H17A H 0.5808 0.3504 0.0077 0.086 Uiso 0.50 1 calc PR B 1
H17B H 0.4956 0.3339 0.0595 0.086 Uiso 0.50 1 calc PR B 1
C16' C 0.6903(14) 0.3230(3) 0.1088(5) 0.0718(15) Uiso 0.50 1 d PD B 2
H16C H 0.6559 0.2989 0.0881 0.086 Uiso 0.50 1 calc PR B 2
H16D H 0.7849 0.3237 0.1117 0.086 Uiso 0.50 1 calc PR B 2
C17' C 0.6217(11) 0.3544(3) 0.0597(6) 0.0718(15) Uiso 0.50 1 d PD B 2
H17C H 0.6844 0.3639 0.0334 0.086 Uiso 0.50 1 calc PR B 2
H17D H 0.5486 0.3432 0.0237 0.086 Uiso 0.50 1 calc PR B 2
N4 N 0.5677(4) 0.38746(11) 0.0906(2) 0.0585(10) Uani 1 1 d D . .
C18 C 0.6678(6) 0.4155(2) 0.0898(3) 0.094(2) Uani 1 1 d . B .
H18A H 0.6826 0.4165 0.0411 0.113 Uiso 1 1 calc R . .
H18B H 0.7505 0.4076 0.1230 0.113 Uiso 1 1 calc R . .
C19 C 0.6348(8) 0.4534(2) 0.1105(4) 0.123(3) Uani 1 1 d . . .
H19A H 0.6633 0.4716 0.0800 0.185 Uiso 1 1 calc R B .
H19B H 0.6790 0.4580 0.1607 0.185 Uiso 1 1 calc R . .
H19C H 0.5403 0.4553 0.1042 0.185 Uiso 1 1 calc R . .
C20 C 0.4339(7) 0.3998(2) 0.0460(3) 0.103(2) Uani 1 1 d . B .
H20A H 0.3707 0.3799 0.0480 0.124 Uiso 1 1 calc R . .
H20B H 0.4072 0.4218 0.0695 0.124 Uiso 1 1 calc R . .
C21 C 0.4212(8) 0.4092(3) -0.0323(4) 0.145(4) Uani 1 1 d . . .
H21A H 0.3298 0.4145 -0.0556 0.218 Uiso 1 1 calc R B .
H21B H 0.4511 0.3883 -0.0563 0.218 Uiso 1 1 calc R . .
H21C H 0.4746 0.4310 -0.0356 0.218 Uiso 1 1 calc R . .
O4 O 0.2949(3) 0.36833(9) 0.32865(17) 0.0563(8) Uani 1 1 d . . .
C22 C 0.2514(4) 0.34262(13) 0.2872(3) 0.0527(11) Uani 1 1 d . A .
H22 H 0.3139 0.3270 0.2742 0.063 Uiso 1 1 calc R . .
N11 N 0.1275(4) 0.33453(12) 0.2592(3) 0.0751(13) Uani 1 1 d . . .
C23 C 0.0256(7) 0.3623(3) 0.2635(5) 0.155(4) Uani 1 1 d . A .
H23A H -0.0437 0.3503 0.2808 0.232 Uiso 1 1 calc R . .
H23B H -0.0111 0.3727 0.2158 0.232 Uiso 1 1 calc R . .
H23C H 0.0648 0.3821 0.2965 0.232 Uiso 1 1 calc R . .
C24 C 0.0824(6) 0.30511(19) 0.2063(4) 0.117(3) Uani 1 1 d . A .
H24A H 0.0295 0.2874 0.2253 0.176 Uiso 1 1 calc R . .
H24B H 0.1579 0.2924 0.1965 0.176 Uiso 1 1 calc R . .
H24C H 0.0298 0.3159 0.1619 0.176 Uiso 1 1 calc R . .
C25 C 0.7354(4) 0.41924(14) 0.3065(3) 0.0549(11) Uani 1 1 d . A .
O2 O 0.6670(3) 0.41801(9) 0.35233(18) 0.0600(8) Uani 1 1 d . . .
O3 O 0.7179(3) 0.40083(9) 0.24894(17) 0.0547(8) Uani 1 1 d . . .
C26 C 0.8510(5) 0.44684(16) 0.3223(3) 0.0810(17) Uani 1 1 d . . .
H26A H 0.8784 0.4516 0.3739 0.121 Uiso 1 1 calc R A .
H26B H 0.8237 0.4701 0.2969 0.121 Uiso 1 1 calc R . .
H26C H 0.9240 0.4363 0.3061 0.121 Uiso 1 1 calc R . .
N5 N 0.4310(3) 0.40904(10) 0.23066(18) 0.0443(8) Uani 1 1 d . . .
N6 N 0.3162(4) 0.41347(10) 0.1975(2) 0.0497(9) Uani 1 1 d . A .
N7 N 0.2080(4) 0.41820(14) 0.1659(2) 0.0747(13) Uani 1 1 d . . .
N8 N 0.3838(4) 0.33604(11) 0.1484(2) 0.0533(9) Uani 1 1 d . . .
N9 N 0.3871(4) 0.30329(13) 0.1594(2) 0.0568(10) Uani 1 1 d . A .
N10 N 0.3896(5) 0.27075(14) 0.1692(3) 0.0961(17) Uani 1 1 d . . .
Ni3 Ni 0.97973(5) 0.397026(15) -0.16634(3) 0.04469(15) Uani 1 1 d . C .
Ni4 Ni 1.04026(5) 0.363209(16) -0.30443(3) 0.04637(16) Uani 1 1 d . C .
O5 O 1.0519(3) 0.34760(8) -0.19686(15) 0.0464(7) Uani 1 1 d . . .
C27 C 1.1351(4) 0.32416(12) -0.1561(2) 0.0445(10) Uani 1 1 d . . .
C28 C 1.2051(4) 0.29660(12) -0.1868(3) 0.0517(11) Uani 1 1 d . . .
C29 C 1.2824(5) 0.26953(15) -0.1421(3) 0.0666(14) Uani 1 1 d . . .
H29 H 1.3240 0.2512 -0.1640 0.080 Uiso 1 1 calc R . .
C30 C 1.3005(6) 0.26841(17) -0.0677(3) 0.0765(16) Uani 1 1 d . . .
C31 C 1.2408(5) 0.29649(16) -0.0372(3) 0.0673(14) Uani 1 1 d . . .
H31 H 1.2535 0.2968 0.0134 0.081 Uiso 1 1 calc R . .
C32 C 1.1618(4) 0.32469(13) -0.0781(3) 0.0527(11) Uani 1 1 d . . .
C33 C 1.3847(8) 0.2378(2) -0.0208(4) 0.127(3) Uani 1 1 d . . .
H33A H 1.3520 0.2134 -0.0388 0.191 Uiso 1 1 calc R . .
H33B H 1.3792 0.2404 0.0290 0.191 Uiso 1 1 calc R . .
H33C H 1.4757 0.2403 -0.0232 0.191 Uiso 1 1 calc R . .
C34 C 1.1115(5) 0.35297(16) -0.0366(3) 0.0617(13) Uani 1 1 d . C .
H34 H 1.1279 0.3491 0.0136 0.074 Uiso 1 1 calc R . .
N12 N 1.0468(4) 0.38270(13) -0.0620(2) 0.0622(11) Uani 1 1 d D . .
C35 C 1.0007(12) 0.4035(3) -0.0075(5) 0.0748(16) Uiso 0.50 1 d PD C 1
H35A H 1.0755 0.4106 0.0322 0.090 Uiso 0.50 1 calc PR C 1
H35B H 0.9408 0.3880 0.0123 0.090 Uiso 0.50 1 calc PR C 1
C36 C 0.9306(12) 0.4376(3) -0.0419(5) 0.0748(16) Uiso 0.50 1 d PD C 1
H36A H 0.8447 0.4374 -0.0301 0.090 Uiso 0.50 1 calc PR C 1
H36B H 0.9792 0.4588 -0.0157 0.090 Uiso 0.50 1 calc PR C 1
C35' C 1.0273(10) 0.4159(3) -0.0164(6) 0.0748(16) Uiso 0.50 1 d PD C 2
H35C H 1.0924 0.4354 -0.0176 0.090 Uiso 0.50 1 calc PR C 2
H35D H 1.0362 0.4083 0.0340 0.090 Uiso 0.50 1 calc PR C 2
C36' C 0.8845(10) 0.4305(3) -0.0506(5) 0.0748(16) Uiso 0.50 1 d PD C 2
H36C H 0.8201 0.4101 -0.0601 0.090 Uiso 0.50 1 calc PR C 2
H36D H 0.8572 0.4493 -0.0199 0.090 Uiso 0.50 1 calc PR C 2
N13 N 0.9041(4) 0.44717(11) -0.1193(2) 0.0572(10) Uani 1 1 d D . .
C37 C 0.9858(5) 0.48109(15) -0.1176(3) 0.0749(16) Uani 1 1 d . C .
H37A H 1.0778 0.4747 -0.0952 0.090 Uiso 1 1 calc R . .
H37B H 0.9582 0.4997 -0.0867 0.090 Uiso 1 1 calc R . .
C38 C 0.9789(8) 0.49823(19) -0.1895(5) 0.116(3) Uani 1 1 d . . .
H38A H 1.0451 0.5176 -0.1845 0.174 Uiso 1 1 calc R C .
H38B H 0.8922 0.5090 -0.2084 0.174 Uiso 1 1 calc R . .
H38C H 0.9948 0.4792 -0.2226 0.174 Uiso 1 1 calc R . .
C39 C 0.7625(5) 0.45554(17) -0.1564(4) 0.093(2) Uani 1 1 d . C .
H39A H 0.7112 0.4326 -0.1571 0.112 Uiso 1 1 calc R . .
H39B H 0.7580 0.4623 -0.2068 0.112 Uiso 1 1 calc R . .
C40 C 0.6959(6) 0.48682(18) -0.1227(5) 0.111(3) Uani 1 1 d . . .
H40A H 0.6032 0.4880 -0.1473 0.167 Uiso 1 1 calc R C .
H40B H 0.7374 0.5105 -0.1280 0.167 Uiso 1 1 calc R . .
H40C H 0.7053 0.4816 -0.0718 0.167 Uiso 1 1 calc R . .
C41 C 1.2065(5) 0.29517(13) -0.2639(3) 0.0550(11) Uani 1 1 d . . .
H41 H 1.2505 0.2748 -0.2785 0.066 Uiso 1 1 calc R . .
N14 N 1.1542(4) 0.31868(11) -0.3129(2) 0.0528(9) Uani 1 1 d . . .
C42 C 1.1731(6) 0.31353(16) -0.3863(3) 0.0691(14) Uani 1 1 d . . .
H42A H 1.0987 0.2997 -0.4162 0.083 Uiso 1 1 calc R . .
H42B H 1.2539 0.2993 -0.3842 0.083 Uiso 1 1 calc R . .
C43 C 1.1825(6) 0.35092(18) -0.4184(3) 0.0842(17) Uani 1 1 d . . .
H43A H 1.1877 0.3477 -0.4687 0.101 Uiso 1 1 calc R . .
H43B H 1.2644 0.3629 -0.3920 0.101 Uiso 1 1 calc R . .
N15 N 1.0689(4) 0.37640(12) -0.4172(2) 0.0592(10) Uani 1 1 d . . .
C44 C 1.1181(8) 0.41497(19) -0.4266(4) 0.101(2) Uani 1 1 d . . .
H44A H 1.1435 0.4163 -0.4727 0.121 Uiso 1 1 calc R . .
H44B H 1.1966 0.4200 -0.3876 0.121 Uiso 1 1 calc R . .
C45 C 1.0142(12) 0.4448(2) -0.4257(5) 0.184(5) Uani 1 1 d . . .
H45A H 1.0554 0.4692 -0.4198 0.276 Uiso 1 1 calc R . .
H45B H 0.9742 0.4400 -0.3858 0.276 Uiso 1 1 calc R . .
H45C H 0.9469 0.4440 -0.4709 0.276 Uiso 1 1 calc R . .
C46 C 0.9538(6) 0.3659(2) -0.4770(3) 0.104(2) Uani 1 1 d . . .
H46A H 0.8812 0.3828 -0.4751 0.125 Uiso 1 1 calc R . .
H46B H 0.9263 0.3407 -0.4671 0.125 Uiso 1 1 calc R . .
C47 C 0.9706(8) 0.3664(3) -0.5544(4) 0.166(5) Uani 1 1 d . . .
H47A H 0.8865 0.3612 -0.5879 0.248 Uiso 1 1 calc R . .
H47B H 1.0338 0.3474 -0.5594 0.248 Uiso 1 1 calc R . .
H47C H 1.0020 0.3907 -0.5649 0.248 Uiso 1 1 calc R . .
O8 O 0.7959(3) 0.37043(9) -0.16363(18) 0.0571(8) Uani 1 1 d . . .
C48 C 0.7434(4) 0.34746(13) -0.2097(3) 0.0546(11) Uani 1 1 d . C .
H48 H 0.7927 0.3395 -0.2419 0.066 Uiso 1 1 calc R . .
N22 N 0.6254(4) 0.33301(13) -0.2184(3) 0.0762(13) Uani 1 1 d . . .
C49 C 0.5427(9) 0.3443(3) -0.1714(7) 0.219(7) Uani 1 1 d . C .
H49A H 0.4959 0.3228 -0.1596 0.328 Uiso 1 1 calc R . .
H49B H 0.4797 0.3629 -0.1958 0.328 Uiso 1 1 calc R . .
H49C H 0.5971 0.3549 -0.1273 0.328 Uiso 1 1 calc R . .
C50 C 0.5673(6) 0.30710(19) -0.2777(4) 0.111(3) Uani 1 1 d . C .
H50A H 0.4943 0.3192 -0.3112 0.166 Uiso 1 1 calc R . .
H50B H 0.5360 0.2849 -0.2580 0.166 Uiso 1 1 calc R . .
H50C H 0.6335 0.3001 -0.3030 0.166 Uiso 1 1 calc R . .
O6 O 1.1540(3) 0.42380(9) -0.16823(18) 0.0603(8) Uani 1 1 d . . .
O7 O 1.2027(3) 0.39673(10) -0.26529(19) 0.0636(9) Uani 1 1 d . . .
C51 C 1.2218(5) 0.41999(15) -0.2143(3) 0.0608(13) Uani 1 1 d . C .
C52 C 1.3381(6) 0.44645(18) -0.2084(4) 0.093(2) Uani 1 1 d . . .
H52A H 1.3741 0.4530 -0.1580 0.139 Uiso 1 1 calc R C .
H52B H 1.3087 0.4689 -0.2362 0.139 Uiso 1 1 calc R . .
H52C H 1.4055 0.4343 -0.2271 0.139 Uiso 1 1 calc R . .
N16 N 0.9172(3) 0.40559(10) -0.27841(19) 0.0459(8) Uani 1 1 d . . .
N17 N 0.8047(4) 0.41166(11) -0.3119(2) 0.0569(10) Uani 1 1 d . C .
N18 N 0.6984(5) 0.41785(16) -0.3438(3) 0.0951(17) Uani 1 1 d . . .
N19 N 0.8689(4) 0.33116(12) -0.3487(2) 0.0574(10) Uani 1 1 d . . .
N20 N 0.8702(4) 0.29807(13) -0.3523(2) 0.0567(10) Uani 1 1 d . C .
N21 N 0.8684(6) 0.26540(14) -0.3586(3) 0.0986(18) 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 N1 1.996(4) . ?
Ni1 O2 2.037(3) . ?
Ni1 O1 2.042(3) . ?
Ni1 N5 2.093(3) . ?
Ni1 O4 2.128(3) . ?
Ni1 N2 2.202(4) . ?
Ni2 N3 1.991(4) . ?
Ni2 O1 2.052(3) . ?
Ni2 O3 2.074(3) . ?
Ni2 N5 2.096(3) . ?
Ni2 N8 2.126(4) . ?
Ni2 N4 2.199(4) . ?
O1 C1 1.312(5) . ?
C1 C6 1.422(6) . ?
C1 C2 1.431(6) . ?
C2 C3 1.398(6) . ?
C2 C15 1.453(7) . ?
C3 C4 1.365(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.376(8) . ?
C4 C7 1.535(7) . ?
C5 C6 1.405(6) . ?
C5 H5 0.9300 . ?
C6 C8 1.439(7) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 N1 1.275(6) . ?
C8 H8 0.9300 . ?
N1 C9' 1.471(8) . ?
N1 C9 1.473(8) . ?
C9 C10 1.538(8) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.475(7) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C9' C10' 1.514(8) . ?
C9' H9'1 0.9700 . ?
C9' H9'2 0.9700 . ?
C10' N2 1.503(7) . ?
C10' H10C 0.9700 . ?
C10' H10D 0.9700 . ?
N2 C13 1.465(7) . ?
N2 C11 1.473(7) . ?
C11 C12 1.451(10) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.526(8) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 N3 1.267(6) . ?
C15 H15 0.9300 . ?
N3 C16' 1.447(8) . ?
N3 C16 1.496(8) . ?
C16 C17 1.543(9) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 N4 1.510(8) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C16' C17' 1.511(9) . ?
C16' H16C 0.9700 . ?
C16' H16D 0.9700 . ?
C17' N4 1.478(8) . ?
C17' H17C 0.9700 . ?
C17' H17D 0.9700 . ?
N4 C18 1.439(7) . ?
N4 C20 1.499(7) . ?
C18 C19 1.463(9) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 C21 1.490(8) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
O4 C22 1.213(5) . ?
C22 N11 1.295(5) . ?
C22 H22 0.9300 . ?
N11 C24 1.440(7) . ?
N11 C23 1.461(8) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 O3 1.242(5) . ?
C25 O2 1.247(5) . ?
C25 C26 1.519(6) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
N5 N6 1.210(5) . ?
N6 N7 1.146(5) . ?
N8 N9 1.179(5) . ?
N9 N10 1.168(6) . ?
Ni3 N12 1.986(4) . ?
Ni3 O5 2.043(3) . ?
Ni3 O6 2.049(3) . ?
Ni3 N16 2.076(3) . ?
Ni3 O8 2.138(3) . ?
Ni3 N13 2.216(4) . ?
Ni4 N14 2.002(4) . ?
Ni4 O7 2.045(3) . ?
Ni4 O5 2.079(3) . ?
Ni4 N19 2.101(4) . ?
Ni4 N16 2.107(4) . ?
Ni4 N15 2.269(4) . ?
O5 C27 1.304(5) . ?
C27 C28 1.423(6) . ?
C27 C32 1.429(6) . ?
C28 C29 1.393(6) . ?
C28 C41 1.460(6) . ?
C29 C30 1.371(7) . ?
C29 H29 0.9300 . ?
C30 C31 1.373(8) . ?
C30 C33 1.531(8) . ?
C31 C32 1.399(6) . ?
C31 H31 0.9300 . ?
C32 C34 1.446(7) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 N12 1.278(6) . ?
C34 H34 0.9300 . ?
N12 C35 1.440(8) . ?
N12 C35' 1.502(8) . ?
C35 C36 1.475(9) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 N13 1.460(8) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C35' C36' 1.551(9) . ?
C35' H35C 0.9700 . ?
C35' H35D 0.9700 . ?
C36' N13 1.485(8) . ?
C36' H36C 0.9700 . ?
C36' H36D 0.9700 . ?
N13 C37 1.467(6) . ?
N13 C39 1.492(7) . ?
C37 C38 1.473(9) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 C40 1.525(7) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 N14 1.264(6) . ?
C41 H41 0.9300 . ?
N14 C42 1.459(6) . ?
C42 C43 1.471(8) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 N15 1.490(7) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
N15 C46 1.474(7) . ?
N15 C44 1.486(7) . ?
C44 C45 1.513(10) . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C46 C47 1.512(9) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
O8 C48 1.218(5) . ?
C48 N22 1.299(6) . ?
C48 H48 0.9300 . ?
N22 C49 1.436(8) . ?
N22 C50 1.458(7) . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
O6 C51 1.255(6) . ?
O7 C51 1.245(6) . ?
C51 C52 1.510(7) . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
N16 N17 1.201(5) . ?
N17 N18 1.139(6) . ?
N19 N20 1.176(5) . ?
N20 N21 1.164(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 O2 92.17(15) . . ?
N1 Ni1 O1 89.11(13) . . ?
O2 Ni1 O1 89.99(12) . . ?
N1 Ni1 N5 172.25(15) . . ?
O2 Ni1 N5 90.39(14) . . ?
O1 Ni1 N5 83.57(12) . . ?
N1 Ni1 O4 88.49(14) . . ?
O2 Ni1 O4 177.73(13) . . ?
O1 Ni1 O4 92.19(11) . . ?
N5 Ni1 O4 89.23(13) . . ?
N1 Ni1 N2 83.41(15) . . ?
O2 Ni1 N2 90.24(14) . . ?
O1 Ni1 N2 172.53(13) . . ?
N5 Ni1 N2 103.90(14) . . ?
O4 Ni1 N2 87.68(13) . . ?
N3 Ni2 O1 89.38(13) . . ?
N3 Ni2 O3 91.56(14) . . ?
O1 Ni2 O3 88.79(12) . . ?
N3 Ni2 N5 172.58(14) . . ?
O1 Ni2 N5 83.25(12) . . ?
O3 Ni2 N5 89.03(13) . . ?
N3 Ni2 N8 89.01(15) . . ?
O1 Ni2 N8 91.41(13) . . ?
O3 Ni2 N8 179.40(14) . . ?
N5 Ni2 N8 90.43(14) . . ?
N3 Ni2 N4 83.51(15) . . ?
O1 Ni2 N4 172.87(13) . . ?
O3 Ni2 N4 90.95(14) . . ?
N5 Ni2 N4 103.87(14) . . ?
N8 Ni2 N4 88.93(15) . . ?
C1 O1 Ni1 128.0(3) . . ?
C1 O1 Ni2 128.2(3) . . ?
Ni1 O1 Ni2 95.77(11) . . ?
O1 C1 C6 121.9(4) . . ?
O1 C1 C2 121.0(4) . . ?
C6 C1 C2 117.1(4) . . ?
C3 C2 C1 119.3(5) . . ?
C3 C2 C15 116.2(4) . . ?
C1 C2 C15 124.5(4) . . ?
C4 C3 C2 123.7(5) . . ?
C4 C3 H3 118.2 . . ?
C2 C3 H3 118.2 . . ?
C3 C4 C5 117.2(5) . . ?
C3 C4 C7 121.7(6) . . ?
C5 C4 C7 121.1(6) . . ?
C4 C5 C6 122.9(5) . . ?
C4 C5 H5 118.5 . . ?
C6 C5 H5 118.5 . . ?
C5 C6 C1 119.6(4) . . ?
C5 C6 C8 115.9(4) . . ?
C1 C6 C8 124.4(4) . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 C6 126.5(4) . . ?
N1 C8 H8 116.8 . . ?
C6 C8 H8 116.8 . . ?
C8 N1 C9' 116.6(5) . . ?
C8 N1 C9 121.0(5) . . ?
C9' N1 C9 22.0(5) . . ?
C8 N1 Ni1 127.7(3) . . ?
C9' N1 Ni1 114.7(5) . . ?
C9 N1 Ni1 110.2(5) . . ?
N1 C9 C10 107.1(7) . . ?
N1 C9 H9A 110.3 . . ?
C10 C9 H9A 110.3 . . ?
N1 C9 H9B 110.3 . . ?
C10 C9 H9B 110.3 . . ?
H9A C9 H9B 108.5 . . ?
N2 C10 C9 105.6(7) . . ?
N2 C10 H10A 110.6 . . ?
C9 C10 H10A 110.6 . . ?
N2 C10 H10B 110.6 . . ?
C9 C10 H10B 110.6 . . ?
H10A C10 H10B 108.7 . . ?
N1 C9' C10' 104.2(7) . . ?
N1 C9' H9'1 110.9 . . ?
C10' C9' H9'1 110.9 . . ?
N1 C9' H9'2 110.9 . . ?
C10' C9' H9'2 110.9 . . ?
H9'1 C9' H9'2 108.9 . . ?
N2 C10' C9' 115.8(7) . . ?
N2 C10' H10C 108.3 . . ?
C9' C10' H10C 108.3 . . ?
N2 C10' H10D 108.3 . . ?
C9' C10' H10D 108.3 . . ?
H10C C10' H10D 107.4 . . ?
C13 N2 C11 108.5(5) . . ?
C13 N2 C10 96.3(5) . . ?
C11 N2 C10 124.5(6) . . ?
C13 N2 C10' 126.5(6) . . ?
C11 N2 C10' 93.0(5) . . ?
C10 N2 C10' 35.9(5) . . ?
C13 N2 Ni1 112.1(3) . . ?
C11 N2 Ni1 113.8(3) . . ?
C10 N2 Ni1 100.3(4) . . ?
C10' N2 Ni1 101.7(4) . . ?
C12 C11 N2 117.5(6) . . ?
C12 C11 H11A 107.9 . . ?
N2 C11 H11A 107.9 . . ?
C12 C11 H11B 107.9 . . ?
N2 C11 H11B 107.9 . . ?
H11A C11 H11B 107.2 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N2 C13 C14 117.2(6) . . ?
N2 C13 H13A 108.0 . . ?
C14 C13 H13A 108.0 . . ?
N2 C13 H13B 108.0 . . ?
C14 C13 H13B 108.0 . . ?
H13A C13 H13B 107.2 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N3 C15 C2 126.3(4) . . ?
N3 C15 H15 116.8 . . ?
C2 C15 H15 116.8 . . ?
C15 N3 C16' 113.8(5) . . ?
C15 N3 C16 123.7(6) . . ?
C16' N3 C16 14.3(9) . . ?
C15 N3 Ni2 127.6(3) . . ?
C16' N3 Ni2 117.8(5) . . ?
C16 N3 Ni2 108.7(5) . . ?
N3 C16 C17 106.2(8) . . ?
N3 C16 H16A 110.5 . . ?
C17 C16 H16A 110.5 . . ?
N3 C16 H16B 110.5 . . ?
C17 C16 H16B 110.5 . . ?
H16A C16 H16B 108.7 . . ?
N4 C17 C16 100.7(8) . . ?
N4 C17 H17A 111.6 . . ?
C16 C17 H17A 111.6 . . ?
N4 C17 H17B 111.6 . . ?
C16 C17 H17B 111.6 . . ?
H17A C17 H17B 109.4 . . ?
N3 C16' C17' 110.9(8) . . ?
N3 C16' H16C 109.5 . . ?
C17' C16' H16C 109.5 . . ?
N3 C16' H16D 109.5 . . ?
C17' C16' H16D 109.5 . . ?
H16C C16' H16D 108.0 . . ?
N4 C17' C16' 120.6(8) . . ?
N4 C17' H17C 107.2 . . ?
C16' C17' H17C 107.2 . . ?
N4 C17' H17D 107.2 . . ?
C16' C17' H17D 107.2 . . ?
H17C C17' H17D 106.8 . . ?
C18 N4 C17' 101.4(6) . . ?
C18 N4 C20 111.3(4) . . ?
C17' N4 C20 113.4(6) . . ?
C18 N4 C17 121.5(6) . . ?
C17' N4 C17 20.6(6) . . ?
C20 N4 C17 99.0(5) . . ?
C18 N4 Ni2 115.7(3) . . ?
C17' N4 Ni2 104.3(5) . . ?
C20 N4 Ni2 110.3(3) . . ?
C17 N4 Ni2 97.1(5) . . ?
N4 C18 C19 114.5(6) . . ?
N4 C18 H18A 108.6 . . ?
C19 C18 H18A 108.6 . . ?
N4 C18 H18B 108.6 . . ?
C19 C18 H18B 108.6 . . ?
H18A C18 H18B 107.6 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 N4 117.8(6) . . ?
C21 C20 H20A 107.9 . . ?
N4 C20 H20A 107.9 . . ?
C21 C20 H20B 107.9 . . ?
N4 C20 H20B 107.9 . . ?
H20A C20 H20B 107.2 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C22 O4 Ni1 124.2(3) . . ?
O4 C22 N11 127.1(4) . . ?
O4 C22 H22 116.5 . . ?
N11 C22 H22 116.5 . . ?
C22 N11 C24 124.3(5) . . ?
C22 N11 C23 119.1(5) . . ?
C24 N11 C23 114.3(5) . . ?
N11 C23 H23A 109.5 . . ?
N11 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N11 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N11 C24 H24A 109.5 . . ?
N11 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N11 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O3 C25 O2 127.1(4) . . ?
O3 C25 C26 116.6(5) . . ?
O2 C25 C26 116.3(5) . . ?
C25 O2 Ni1 127.1(3) . . ?
C25 O3 Ni2 127.6(3) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N6 N5 Ni1 122.9(3) . . ?
N6 N5 Ni2 122.0(3) . . ?
Ni1 N5 Ni2 92.96(14) . . ?
N7 N6 N5 179.0(5) . . ?
N9 N8 Ni2 118.0(3) . . ?
N10 N9 N8 178.9(6) . . ?
N12 Ni3 O5 89.85(14) . . ?
N12 Ni3 O6 92.37(16) . . ?
O5 Ni3 O6 90.39(12) . . ?
N12 Ni3 N16 173.06(16) . . ?
O5 Ni3 N16 83.23(12) . . ?
O6 Ni3 N16 88.25(13) . . ?
N12 Ni3 O8 87.68(15) . . ?
O5 Ni3 O8 91.08(12) . . ?
O6 Ni3 O8 178.53(13) . . ?
N16 Ni3 O8 91.87(13) . . ?
N12 Ni3 N13 83.11(16) . . ?
O5 Ni3 N13 172.63(13) . . ?
O6 Ni3 N13 92.06(14) . . ?
N16 Ni3 N13 103.78(14) . . ?
O8 Ni3 N13 86.48(13) . . ?
N14 Ni4 O7 92.15(14) . . ?
N14 Ni4 O5 88.55(14) . . ?
O7 Ni4 O5 87.58(13) . . ?
N14 Ni4 N19 89.97(15) . . ?
O7 Ni4 N19 176.83(16) . . ?
O5 Ni4 N19 94.83(14) . . ?
N14 Ni4 N16 169.95(15) . . ?
O7 Ni4 N16 89.63(14) . . ?
O5 Ni4 N16 81.64(12) . . ?
N19 Ni4 N16 88.69(15) . . ?
N14 Ni4 N15 82.62(15) . . ?
O7 Ni4 N15 86.12(14) . . ?
O5 Ni4 N15 168.94(13) . . ?
N19 Ni4 N15 91.82(15) . . ?
N16 Ni4 N15 107.38(14) . . ?
C27 O5 Ni3 128.0(3) . . ?
C27 O5 Ni4 128.0(3) . . ?
Ni3 O5 Ni4 96.32(12) . . ?
O5 C27 C28 121.8(4) . . ?
O5 C27 C32 122.0(4) . . ?
C28 C27 C32 116.1(4) . . ?
C29 C28 C27 120.1(4) . . ?
C29 C28 C41 115.7(4) . . ?
C27 C28 C41 124.2(4) . . ?
C30 C29 C28 123.5(5) . . ?
C30 C29 H29 118.2 . . ?
C28 C29 H29 118.2 . . ?
C29 C30 C31 116.6(5) . . ?
C29 C30 C33 121.8(6) . . ?
C31 C30 C33 121.6(6) . . ?
C30 C31 C32 123.3(5) . . ?
C30 C31 H31 118.3 . . ?
C32 C31 H31 118.3 . . ?
C31 C32 C27 119.9(4) . . ?
C31 C32 C34 115.9(4) . . ?
C27 C32 C34 124.3(4) . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N12 C34 C32 126.5(4) . . ?
N12 C34 H34 116.7 . . ?
C32 C34 H34 116.7 . . ?
C34 N12 C35 113.0(5) . . ?
C34 N12 C35' 124.4(6) . . ?
C35 N12 C35' 22.0(6) . . ?
C34 N12 Ni3 127.3(3) . . ?
C35 N12 Ni3 118.7(5) . . ?
C35' N12 Ni3 107.7(5) . . ?
N12 C35 C36 108.7(8) . . ?
N12 C35 H35A 110.0 . . ?
C36 C35 H35A 110.0 . . ?
N12 C35 H35B 110.0 . . ?
C36 C35 H35B 110.0 . . ?
H35A C35 H35B 108.3 . . ?
N13 C36 C35 125.6(9) . . ?
N13 C36 H36A 105.9 . . ?
C35 C36 H36A 105.9 . . ?
N13 C36 H36B 105.9 . . ?
C35 C36 H36B 105.9 . . ?
H36A C36 H36B 106.2 . . ?
N12 C35' C36' 105.8(8) . . ?
N12 C35' H35C 110.6 . . ?
C36' C35' H35C 110.6 . . ?
N12 C35' H35D 110.6 . . ?
C36' C35' H35D 110.6 . . ?
H35C C35' H35D 108.7 . . ?
N13 C36' C35' 100.1(7) . . ?
N13 C36' H36C 111.8 . . ?
C35' C36' H36C 111.8 . . ?
N13 C36' H36D 111.8 . . ?
C35' C36' H36D 111.8 . . ?
H36C C36' H36D 109.5 . . ?
C36 N13 C37 101.7(6) . . ?
C36 N13 C36' 20.7(7) . . ?
C37 N13 C36' 120.6(6) . . ?
C36 N13 C39 115.9(6) . . ?
C37 N13 C39 110.1(4) . . ?
C36' N13 C39 99.1(5) . . ?
C36 N13 Ni3 102.5(5) . . ?
C37 N13 Ni3 114.0(3) . . ?
C36' N13 Ni3 99.7(5) . . ?
C39 N13 Ni3 112.1(3) . . ?
N13 C37 C38 114.9(5) . . ?
N13 C37 H37A 108.5 . . ?
C38 C37 H37A 108.5 . . ?
N13 C37 H37B 108.5 . . ?
C38 C37 H37B 108.5 . . ?
H37A C37 H37B 107.5 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N13 C39 C40 116.3(5) . . ?
N13 C39 H39A 108.2 . . ?
C40 C39 H39A 108.2 . . ?
N13 C39 H39B 108.2 . . ?
C40 C39 H39B 108.2 . . ?
H39A C39 H39B 107.4 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
N14 C41 C28 126.7(4) . . ?
N14 C41 H41 116.6 . . ?
C28 C41 H41 116.6 . . ?
C41 N14 C42 118.6(4) . . ?
C41 N14 Ni4 128.1(3) . . ?
C42 N14 Ni4 113.2(3) . . ?
N14 C42 C43 108.5(4) . . ?
N14 C42 H42A 110.0 . . ?
C43 C42 H42A 110.0 . . ?
N14 C42 H42B 110.0 . . ?
C43 C42 H42B 110.0 . . ?
H42A C42 H42B 108.4 . . ?
C42 C43 N15 114.0(5) . . ?
C42 C43 H43A 108.7 . . ?
N15 C43 H43A 108.7 . . ?
C42 C43 H43B 108.7 . . ?
N15 C43 H43B 108.7 . . ?
H43A C43 H43B 107.6 . . ?
C46 N15 C44 112.1(5) . . ?
C46 N15 C43 109.2(5) . . ?
C44 N15 C43 105.1(5) . . ?
C46 N15 Ni4 113.5(3) . . ?
C44 N15 Ni4 115.5(3) . . ?
C43 N15 Ni4 100.2(3) . . ?
N15 C44 C45 112.1(6) . . ?
N15 C44 H44A 109.2 . . ?
C45 C44 H44A 109.2 . . ?
N15 C44 H44B 109.2 . . ?
C45 C44 H44B 109.2 . . ?
H44A C44 H44B 107.9 . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
N15 C46 C47 118.3(5) . . ?
N15 C46 H46A 107.7 . . ?
C47 C46 H46A 107.7 . . ?
N15 C46 H46B 107.7 . . ?
C47 C46 H46B 107.7 . . ?
H46A C46 H46B 107.1 . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C48 O8 Ni3 121.5(3) . . ?
O8 C48 N22 126.6(5) . . ?
O8 C48 H48 116.7 . . ?
N22 C48 H48 116.7 . . ?
C48 N22 C49 119.9(5) . . ?
C48 N22 C50 123.0(5) . . ?
C49 N22 C50 117.0(5) . . ?
N22 C49 H49A 109.5 . . ?
N22 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
N22 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
N22 C50 H50A 109.5 . . ?
N22 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
N22 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C51 O6 Ni3 127.6(3) . . ?
C51 O7 Ni4 128.6(3) . . ?
O7 C51 O6 126.7(4) . . ?
O7 C51 C52 116.2(5) . . ?
O6 C51 C52 117.1(5) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
N17 N16 Ni3 125.5(3) . . ?
N17 N16 Ni4 124.8(3) . . ?
Ni3 N16 Ni4 94.49(14) . . ?
N18 N17 N16 179.2(6) . . ?
N20 N19 Ni4 122.8(3) . . ?
N21 N20 N19 177.3(6) . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        26.68
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.886
_refine_diff_density_min         -0.745
_refine_diff_density_rms         0.071

