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

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#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
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#  fide research purposes only. It may contain copyright material
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data_drag050

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H29 N6 Ni2 O6, N O3, 0.5(H2 O)'
_chemical_formula_sum            'C22 H30 N7 Ni2 O9.50'
_chemical_formula_weight         661.95

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           tetragonal
_symmetry_space_group_name_H-M   'P -4 21 c'

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

_cell_length_a                   18.5183(16)
_cell_length_b                   18.5183(16)
_cell_length_c                   17.4171(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5972.8(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4662
_cell_measurement_theta_min      1.61
_cell_measurement_theta_max      24.00

_exptl_crystal_description       prismatic
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2744
_exptl_absorpt_coefficient_mu    1.320
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.604
_exptl_absorpt_correction_T_max  0.812
_exptl_absorpt_process_details   'SORTAV (Blessing, Acta Cryst., 1995, A51,33)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Brucker APEX II CCD'
_diffrn_measurement_method       '\f scans and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            62694
_diffrn_reflns_av_R_equivalents  0.0981
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.61
_diffrn_reflns_theta_max         24.00
_reflns_number_total             4662
_reflns_number_gt                3728
_reflns_threshold_expression     I>2sigma(I)

_computing_data_collection       Brucker
_computing_cell_refinement       Brucker
_computing_data_reduction        Brucker
_computing_structure_solution    'SHELXS-86(Sheldrick, 1986)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0947P)^2^+7.4446P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_number_reflns         4662
_refine_ls_number_parameters     354
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0525
_refine_ls_wR_factor_ref         0.1597
_refine_ls_wR_factor_gt          0.1378
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.084
_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 0.14868(5) 0.08256(5) 0.88389(6) 0.0331(3) Uani 1 1 d . . .
Ni2 Ni 0.19312(5) 0.11057(5) 1.04758(6) 0.0326(2) Uani 1 1 d . . .
O1 O 0.2020(3) 0.1612(3) 0.9439(3) 0.0363(12) Uani 1 1 d . . .
C1 C 0.1944(4) 0.2312(4) 0.9341(5) 0.0389(19) Uani 1 1 d . . .
C2 C 0.2116(5) 0.2816(4) 0.9914(5) 0.044(2) Uani 1 1 d . . .
C3 C 0.2115(6) 0.3553(5) 0.9737(6) 0.062(3) Uani 1 1 d . . .
H3 H 0.2262 0.3872 1.0118 0.074 Uiso 1 1 calc R A .
C4 C 0.1917(6) 0.3834(5) 0.9061(6) 0.065(3) Uani 1 1 d . . .
C5 C 0.1711(6) 0.3352(5) 0.8501(6) 0.059(3) Uani 1 1 d . . .
H5 H 0.1568 0.3535 0.8027 0.071 Uiso 1 1 calc R A .
C6 C 0.1705(4) 0.2589(4) 0.8603(5) 0.044(2) Uani 1 1 d . . .
C7 C 0.1918(9) 0.4633(5) 0.8866(8) 0.103(5) Uani 1 1 d . . .
H7A H 0.1468 0.4759 0.8627 0.155 Uiso 1 1 calc R A .
H7B H 0.2308 0.4735 0.8520 0.155 Uiso 1 1 calc R . .
H7C H 0.1978 0.4910 0.9328 0.155 Uiso 1 1 calc R . .
C8 C 0.2326(5) 0.2611(5) 1.0700(5) 0.056(2) Uani 1 1 d . . .
H8 H 0.2509 0.2979 1.1006 0.067 Uiso 1 1 calc R A .
N1 N 0.2287(4) 0.2001(4) 1.1004(4) 0.0462(17) Uani 1 1 d . . .
C9 C 0.2602(7) 0.1925(5) 1.1780(5) 0.068(3) Uani 1 1 d . . .
H9A H 0.3072 0.1698 1.1736 0.081 Uiso 1 1 calc R A .
H9B H 0.2673 0.2402 1.1997 0.081 Uiso 1 1 calc R . .
C10 C 0.2158(8) 0.1504(6) 1.2302(7) 0.090(4) Uani 1 1 d . . .
H10A H 0.1669 0.1690 1.2275 0.108 Uiso 1 1 calc R . .
H10B H 0.2332 0.1588 1.2819 0.108 Uiso 1 1 calc R . .
C11 C 0.2125(6) 0.0684(5) 1.2175(5) 0.061(3) Uani 1 1 d . . .
H11A H 0.2608 0.0487 1.2120 0.073 Uiso 1 1 calc R A .
H11B H 0.1890 0.0449 1.2605 0.073 Uiso 1 1 calc R . .
O2 O 0.1721(3) 0.0578(3) 1.1489(3) 0.0472(14) Uani 1 1 d . . .
H2 H 0.1340 0.0251 1.1501 0.057 Uiso 1 1 calc R . .
C12 C 0.1455(4) 0.2161(5) 0.7965(5) 0.045(2) Uani 1 1 d . . .
H12 H 0.1339 0.2423 0.7527 0.054 Uiso 1 1 calc R A .
N2 N 0.1367(3) 0.1486(3) 0.7905(3) 0.0367(14) Uani 1 1 d D A .
C13A C 0.1160(11) 0.1184(9) 0.7184(9) 0.060 Uiso 0.70 1 d PD A 1
H13A H 0.1602 0.1085 0.6905 0.072 Uiso 0.70 1 calc PR A 1
H13B H 0.0910 0.1561 0.6904 0.072 Uiso 0.70 1 calc PR A 1
C14A C 0.0706(8) 0.0523(8) 0.7128(9) 0.070 Uiso 0.70 1 d PD A 1
H14A H 0.0670 0.0393 0.6589 0.084 Uiso 0.70 1 calc PR A 1
H14B H 0.0223 0.0647 0.7300 0.084 Uiso 0.70 1 calc PR A 1
C15A C 0.0942(9) -0.0135(8) 0.7561(9) 0.070 Uiso 0.70 1 d PD A 1
H15A H 0.0655 -0.0548 0.7402 0.084 Uiso 0.70 1 calc PR A 1
H15B H 0.1444 -0.0238 0.7449 0.084 Uiso 0.70 1 calc PR A 1
O3A O 0.0850(4) -0.0012(4) 0.8393(4) 0.040 Uiso 0.70 1 d PD A 1
H3OA H 0.0536 -0.0283 0.8694 0.048 Uiso 0.70 1 calc PR A 1
C13B C 0.104(3) 0.130(2) 0.719(2) 0.070 Uiso 0.30 1 d PD A 2
H13C H 0.1017 0.1728 0.6859 0.084 Uiso 0.30 1 calc PR A 2
H13D H 0.0559 0.1121 0.7264 0.084 Uiso 0.30 1 calc PR A 2
C14B C 0.1513(19) 0.0735(19) 0.682(2) 0.080 Uiso 0.30 1 d PD A 2
H14C H 0.1973 0.0946 0.6678 0.096 Uiso 0.30 1 calc PR A 2
H14D H 0.1604 0.0353 0.7188 0.096 Uiso 0.30 1 calc PR A 2
C15B C 0.116(2) 0.0421(17) 0.6118(18) 0.080 Uiso 0.30 1 d PD A 2
H15C H 0.1448 0.0022 0.5930 0.096 Uiso 0.30 1 calc PR A 2
H15D H 0.0688 0.0230 0.6259 0.096 Uiso 0.30 1 calc PR A 2
O3B O 0.1066(13) 0.0961(13) 0.5491(14) 0.080 Uiso 0.30 1 d PD A 2
H3OB H 0.0816 0.1296 0.5645 0.096 Uiso 0.30 1 calc PR A 2
C22 C 0.0393(4) 0.1425(4) 0.9990(5) 0.0359(18) Uani 1 1 d . . .
O4 O 0.0543(3) 0.1301(3) 0.9278(3) 0.0395(13) Uani 1 1 d . A .
O5 O 0.0865(3) 0.1404(3) 1.0525(3) 0.0401(12) Uani 1 1 d . A .
O6 O -0.0248(3) 0.1596(3) 1.0157(3) 0.0388(12) Uani 1 1 d . A .
N4 N 0.2976(3) 0.0722(3) 1.0402(4) 0.0411(15) Uani 1 1 d . A .
C16 C 0.3492(5) 0.1013(5) 0.9999(6) 0.057(2) Uani 1 1 d . . .
H16 H 0.3459 0.1470 0.9780 0.068 Uiso 1 1 calc R A .
N5 N 0.4062(4) 0.0597(5) 0.9932(5) 0.065(2) Uani 1 1 d . A .
H5A H 0.4453 0.0695 0.9688 0.078 Uiso 1 1 calc R . .
C17 C 0.3916(6) -0.0003(6) 1.0315(7) 0.075(3) Uani 1 1 d . . .
H17 H 0.4220 -0.0399 1.0375 0.090 Uiso 1 1 calc R A .
C18 C 0.3256(6) 0.0066(6) 1.0597(6) 0.068(3) Uani 1 1 d . A .
H18 H 0.3017 -0.0282 1.0887 0.081 Uiso 1 1 calc R . .
N6 N 0.2466(4) 0.0400(4) 0.8427(4) 0.0421(16) Uani 1 1 d . A .
C19 C 0.2986(4) 0.0815(5) 0.8073(5) 0.052(2) Uani 1 1 d . . .
H19 H 0.2926 0.1284 0.7893 0.062 Uiso 1 1 calc R A .
C20 C 0.3583(5) 0.0428(6) 0.8036(6) 0.067(3) Uani 1 1 d . A .
H20 H 0.4023 0.0579 0.7835 0.081 Uiso 1 1 calc R . .
N7 N 0.3443(4) -0.0223(5) 0.8338(5) 0.069(2) Uani 1 1 d . . .
H7 H 0.3738 -0.0579 0.8372 0.083 Uiso 1 1 calc R A .
C21 C 0.2774(5) -0.0215(5) 0.8571(5) 0.054(2) Uani 1 1 d . A .
H21 H 0.2546 -0.0601 0.8811 0.065 Uiso 1 1 calc R . .
N8 N 0.5233(5) 0.1553(5) 0.8719(6) 0.074(3) Uani 1 1 d . . .
O7 O 0.5711(6) 0.1789(7) 0.8358(6) 0.139(4) Uani 1 1 d . . .
O8 O 0.5240(4) 0.0923(5) 0.8903(6) 0.101(3) Uani 1 1 d . . .
O9 O 0.4732(6) 0.1932(5) 0.8940(7) 0.126(4) Uani 1 1 d . . .
O1W O -0.0245(10) 0.1536(10) 0.5784(11) 0.103(6) Uiso 0.50 1 d P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.0358(5) 0.0368(5) 0.0267(5) 0.0018(4) 0.0016(4) 0.0000(4)
Ni2 0.0335(5) 0.0342(5) 0.0300(5) 0.0003(4) -0.0032(4) -0.0020(4)
O1 0.041(3) 0.035(3) 0.033(3) 0.003(2) -0.001(2) -0.001(2)
C1 0.037(4) 0.036(4) 0.044(5) 0.009(3) 0.008(4) 0.002(3)
C2 0.055(5) 0.037(4) 0.038(5) 0.006(4) -0.003(4) -0.006(4)
C3 0.086(7) 0.049(5) 0.051(6) -0.012(5) 0.009(5) -0.005(5)
C4 0.088(7) 0.040(5) 0.066(7) 0.008(5) 0.011(6) -0.008(5)
C5 0.082(7) 0.041(5) 0.055(6) 0.018(4) 0.011(5) 0.009(4)
C6 0.049(5) 0.043(5) 0.040(5) 0.004(4) 0.005(4) 0.000(4)
C7 0.183(14) 0.039(5) 0.087(9) 0.007(6) 0.011(10) -0.015(7)
C8 0.069(6) 0.047(5) 0.052(6) -0.010(5) -0.025(5) -0.008(4)
N1 0.065(5) 0.035(4) 0.039(4) -0.009(3) -0.014(3) -0.004(3)
C9 0.125(9) 0.044(5) 0.035(5) 0.001(4) -0.035(6) -0.013(6)
C10 0.130(11) 0.081(8) 0.058(7) -0.003(6) -0.024(7) -0.033(8)
C11 0.083(7) 0.062(6) 0.038(5) 0.005(4) -0.022(5) -0.012(5)
O2 0.060(4) 0.050(3) 0.032(3) 0.004(3) -0.003(3) -0.012(3)
C12 0.045(5) 0.056(5) 0.033(4) 0.018(4) 0.002(4) 0.002(4)
N2 0.042(3) 0.041(4) 0.027(3) 0.003(3) -0.001(3) -0.002(3)
C22 0.038(4) 0.030(4) 0.040(5) 0.002(4) 0.006(4) 0.001(3)
O4 0.039(3) 0.060(4) 0.020(3) -0.005(2) -0.001(2) 0.007(2)
O5 0.036(3) 0.060(3) 0.024(3) 0.001(3) -0.007(2) 0.007(3)
O6 0.036(3) 0.046(3) 0.034(3) 0.001(2) 0.007(2) 0.005(2)
N4 0.037(3) 0.045(4) 0.041(4) 0.007(3) 0.007(3) 0.001(3)
C16 0.046(5) 0.057(6) 0.067(6) 0.006(5) -0.006(5) 0.000(4)
N5 0.031(4) 0.093(6) 0.071(5) 0.026(5) 0.009(4) 0.007(4)
C17 0.062(6) 0.072(7) 0.090(8) 0.021(6) 0.019(6) 0.025(5)
C18 0.064(6) 0.068(7) 0.071(7) 0.016(6) 0.009(6) 0.012(5)
N6 0.041(4) 0.051(4) 0.035(4) 0.002(3) 0.005(3) 0.010(3)
C19 0.044(5) 0.060(5) 0.053(6) 0.006(5) 0.009(4) -0.008(4)
C20 0.039(5) 0.103(8) 0.059(6) 0.009(6) 0.013(5) 0.005(5)
N7 0.055(5) 0.087(6) 0.064(6) 0.011(5) 0.013(4) 0.026(5)
C21 0.061(6) 0.046(5) 0.056(6) -0.007(4) 0.006(5) 0.012(4)
N8 0.064(6) 0.073(6) 0.085(7) 0.020(6) 0.002(5) 0.003(5)
O7 0.138(9) 0.160(10) 0.119(8) 0.058(7) 0.056(7) -0.026(8)
O8 0.065(5) 0.084(6) 0.153(8) 0.031(6) 0.036(5) 0.019(4)
O9 0.145(9) 0.096(7) 0.137(9) 0.016(7) 0.018(8) 0.040(7)

_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 N2 2.047(6) . ?
Ni1 O1 2.047(5) . ?
Ni1 O6 2.060(5) 8_557 ?
Ni1 O3A 2.098(8) . ?
Ni1 O4 2.101(5) . ?
Ni1 N6 2.103(6) . ?
Ni2 N1 2.007(6) . ?
Ni2 O6 2.030(5) 8_557 ?
Ni2 O1 2.041(5) . ?
Ni2 O5 2.052(5) . ?
Ni2 O2 2.055(5) . ?
Ni2 N4 2.066(6) . ?
O1 C1 1.314(9) . ?
C1 C2 1.404(12) . ?
C1 C6 1.452(11) . ?
C2 C3 1.398(12) . ?
C2 C8 1.472(12) . ?
C3 C4 1.338(14) . ?
C3 H3 0.9300 . ?
C4 C5 1.376(14) . ?
C4 C7 1.518(13) . ?
C5 C6 1.425(12) . ?
C5 H5 0.9300 . ?
C6 C12 1.442(12) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 N1 1.250(11) . ?
C8 H8 0.9300 . ?
N1 C9 1.479(10) . ?
C9 C10 1.453(15) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.534(14) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 O2 1.423(10) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
O2 H2 0.9300 . ?
C12 N2 1.264(10) . ?
C12 H12 0.9300 . ?
N2 C13A 1.427(12) . ?
N2 C13B 1.429(19) . ?
C13A C14A 1.49(2) . ?
C13A H13A 0.9700 . ?
C13A H13B 0.9700 . ?
C14A C15A 1.50(2) . ?
C14A H14A 0.9700 . ?
C14A H14B 0.9700 . ?
C15A O3A 1.478(17) . ?
C15A H15A 0.9700 . ?
C15A H15B 0.9700 . ?
O3A H3OA 0.9300 . ?
C13B C14B 1.51(3) . ?
C13B H13C 0.9700 . ?
C13B H13D 0.9700 . ?
C14B C15B 1.50(3) . ?
C14B H14C 0.9700 . ?
C14B H14D 0.9700 . ?
C15B O3B 1.49(2) . ?
C15B H15C 0.9700 . ?
C15B H15D 0.9700 . ?
O3B H3OB 0.8200 . ?
C22 O6 1.263(9) . ?
C22 O5 1.278(9) . ?
C22 O4 1.291(9) . ?
O6 Ni2 2.030(5) 7_557 ?
O6 Ni1 2.060(5) 7_557 ?
N4 C16 1.303(11) . ?
N4 C18 1.362(12) . ?
C16 N5 1.312(11) . ?
C16 H16 0.9300 . ?
N5 C17 1.325(13) . ?
N5 H5A 0.8600 . ?
C17 C18 1.324(14) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
N6 C21 1.298(11) . ?
N6 C19 1.378(10) . ?
C19 C20 1.320(13) . ?
C19 H19 0.9300 . ?
C20 N7 1.341(13) . ?
C20 H20 0.9300 . ?
N7 C21 1.303(12) . ?
N7 H7 0.8600 . ?
C21 H21 0.9300 . ?
N8 O7 1.170(12) . ?
N8 O8 1.211(11) . ?
N8 O9 1.225(12) . ?

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
N2 Ni1 O1 91.9(2) . . ?
N2 Ni1 O6 174.5(2) . 8_557 ?
O1 Ni1 O6 83.6(2) . 8_557 ?
N2 Ni1 O3A 95.0(3) . . ?
O1 Ni1 O3A 170.6(3) . . ?
O6 Ni1 O3A 89.2(3) 8_557 . ?
N2 Ni1 O4 87.0(2) . . ?
O1 Ni1 O4 85.2(2) . . ?
O6 Ni1 O4 89.4(2) 8_557 . ?
O3A Ni1 O4 88.7(3) . . ?
N2 Ni1 N6 92.7(3) . . ?
O1 Ni1 N6 91.5(2) . . ?
O6 Ni1 N6 90.6(2) 8_557 . ?
O3A Ni1 N6 94.7(3) . . ?
O4 Ni1 N6 176.6(2) . . ?
N1 Ni2 O6 174.4(3) . 8_557 ?
N1 Ni2 O1 90.0(2) . . ?
O6 Ni2 O1 84.5(2) 8_557 . ?
N1 Ni2 O5 94.2(3) . . ?
O6 Ni2 O5 86.5(2) 8_557 . ?
O1 Ni2 O5 89.4(2) . . ?
N1 Ni2 O2 93.5(3) . . ?
O6 Ni2 O2 92.1(2) 8_557 . ?
O1 Ni2 O2 173.5(2) . . ?
O5 Ni2 O2 84.8(2) . . ?
N1 Ni2 N4 90.3(3) . . ?
O6 Ni2 N4 89.1(2) 8_557 . ?
O1 Ni2 N4 91.6(2) . . ?
O5 Ni2 N4 175.3(2) . . ?
O2 Ni2 N4 93.8(2) . . ?
C1 O1 Ni2 124.0(5) . . ?
C1 O1 Ni1 125.7(5) . . ?
Ni2 O1 Ni1 94.9(2) . . ?
O1 C1 C2 122.7(7) . . ?
O1 C1 C6 119.7(7) . . ?
C2 C1 C6 117.6(7) . . ?
C3 C2 C1 119.5(8) . . ?
C3 C2 C8 117.2(8) . . ?
C1 C2 C8 123.3(7) . . ?
C4 C3 C2 125.0(9) . . ?
C4 C3 H3 117.5 . . ?
C2 C3 H3 117.5 . . ?
C3 C4 C5 116.6(8) . . ?
C3 C4 C7 125.1(10) . . ?
C5 C4 C7 118.3(10) . . ?
C4 C5 C6 123.8(9) . . ?
C4 C5 H5 118.1 . . ?
C6 C5 H5 118.1 . . ?
C5 C6 C12 116.8(8) . . ?
C5 C6 C1 117.3(8) . . ?
C12 C6 C1 125.9(7) . . ?
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 C2 127.8(8) . . ?
N1 C8 H8 116.1 . . ?
C2 C8 H8 116.1 . . ?
C8 N1 C9 116.8(7) . . ?
C8 N1 Ni2 124.8(6) . . ?
C9 N1 Ni2 118.0(6) . . ?
C10 C9 N1 113.5(9) . . ?
C10 C9 H9A 108.9 . . ?
N1 C9 H9A 108.9 . . ?
C10 C9 H9B 108.9 . . ?
N1 C9 H9B 108.9 . . ?
H9A C9 H9B 107.7 . . ?
C9 C10 C11 117.7(10) . . ?
C9 C10 H10A 107.9 . . ?
C11 C10 H10A 107.9 . . ?
C9 C10 H10B 107.9 . . ?
C11 C10 H10B 107.9 . . ?
H10A C10 H10B 107.2 . . ?
O2 C11 C10 106.2(8) . . ?
O2 C11 H11A 110.5 . . ?
C10 C11 H11A 110.5 . . ?
O2 C11 H11B 110.5 . . ?
C10 C11 H11B 110.5 . . ?
H11A C11 H11B 108.7 . . ?
C11 O2 Ni2 123.8(5) . . ?
C11 O2 H2 118.1 . . ?
Ni2 O2 H2 118.1 . . ?
N2 C12 C6 130.4(7) . . ?
N2 C12 H12 114.8 . . ?
C6 C12 H12 114.8 . . ?
C12 N2 C13A 119.6(10) . . ?
C12 N2 C13B 111(2) . . ?
C13A N2 C13B 12.5(15) . . ?
C12 N2 Ni1 120.7(6) . . ?
C13A N2 Ni1 119.6(9) . . ?
C13B N2 Ni1 127(2) . . ?
N2 C13A C14A 122.1(16) . . ?
N2 C13A H13A 106.8 . . ?
C14A C13A H13A 106.8 . . ?
N2 C13A H13B 106.8 . . ?
C14A C13A H13B 106.8 . . ?
H13A C13A H13B 106.6 . . ?
C13A C14A C15A 118.1(13) . . ?
C13A C14A H14A 107.8 . . ?
C15A C14A H14A 107.8 . . ?
C13A C14A H14B 107.8 . . ?
C15A C14A H14B 107.8 . . ?
H14A C14A H14B 107.1 . . ?
O3A C15A C14A 109.5(12) . . ?
O3A C15A H15A 109.8 . . ?
C14A C15A H15A 109.8 . . ?
O3A C15A H15B 109.8 . . ?
C14A C15A H15B 109.8 . . ?
H15A C15A H15B 108.2 . . ?
C15A O3A Ni1 114.4(7) . . ?
C15A O3A H3OA 122.8 . . ?
Ni1 O3A H3OA 122.8 . . ?
N2 C13B C14B 107(2) . . ?
N2 C13B H13C 110.3 . . ?
C14B C13B H13C 110.3 . . ?
N2 C13B H13D 110.3 . . ?
C14B C13B H13D 110.3 . . ?
H13C C13B H13D 108.5 . . ?
C15B C14B C13B 111(3) . . ?
C15B C14B H14C 109.4 . . ?
C13B C14B H14C 109.4 . . ?
C15B C14B H14D 109.4 . . ?
C13B C14B H14D 109.4 . . ?
H14C C14B H14D 108.0 . . ?
O3B C15B C14B 113(3) . . ?
O3B C15B H15C 109.1 . . ?
C14B C15B H15C 109.1 . . ?
O3B C15B H15D 109.1 . . ?
C14B C15B H15D 109.1 . . ?
H15C C15B H15D 107.8 . . ?
C15B O3B H3OB 109.5 . . ?
O6 C22 O5 118.8(7) . . ?
O6 C22 O4 118.0(7) . . ?
O5 C22 O4 123.2(7) . . ?
C22 O4 Ni1 127.1(5) . . ?
C22 O5 Ni2 129.5(5) . . ?
C22 O6 Ni2 133.4(5) . 7_557 ?
C22 O6 Ni1 131.3(5) . 7_557 ?
Ni2 O6 Ni1 94.9(2) 7_557 7_557 ?
C16 N4 C18 103.0(7) . . ?
C16 N4 Ni2 125.3(6) . . ?
C18 N4 Ni2 130.3(6) . . ?
N4 C16 N5 113.2(8) . . ?
N4 C16 H16 123.4 . . ?
N5 C16 H16 123.4 . . ?
C16 N5 C17 106.5(8) . . ?
C16 N5 H5A 126.7 . . ?
C17 N5 H5A 126.7 . . ?
C18 C17 N5 107.1(9) . . ?
C18 C17 H17 126.5 . . ?
N5 C17 H17 126.5 . . ?
C17 C18 N4 110.2(9) . . ?
C17 C18 H18 124.9 . . ?
N4 C18 H18 124.9 . . ?
C21 N6 C19 105.6(7) . . ?
C21 N6 Ni1 130.0(6) . . ?
C19 N6 Ni1 123.1(5) . . ?
C20 C19 N6 107.8(8) . . ?
C20 C19 H19 126.1 . . ?
N6 C19 H19 126.1 . . ?
C19 C20 N7 107.8(9) . . ?
C19 C20 H20 126.1 . . ?
N7 C20 H20 126.1 . . ?
C21 N7 C20 107.3(8) . . ?
C21 N7 H7 126.4 . . ?
C20 N7 H7 126.4 . . ?
N6 C21 N7 111.6(9) . . ?
N6 C21 H21 124.2 . . ?
N7 C21 H21 124.2 . . ?
O7 N8 O8 119.6(11) . . ?
O7 N8 O9 121.8(12) . . ?
O8 N8 O9 118.5(10) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        24.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.293
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.110
_database_code_depnum_ccdc_archive 'CCDC 869968'