# 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
#  of the CCDC or of third parties, and may not be copied or further
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data_12003

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H54 N6 Ni2 O6, 4(N O3), 4(H2 O)'
_chemical_formula_sum            'C26 H62 N10 Ni2 O22'
_chemical_formula_weight         984.28

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/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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                   9.233(3)
_cell_length_b                   16.580(5)
_cell_length_c                   14.170(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.545(7)
_cell_angle_gamma                90.00
_cell_volume                     2168.4(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7983
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      28.28

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1040
_exptl_absorpt_coefficient_mu    0.958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7365
_exptl_absorpt_correction_T_max  0.9019
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2001)'

_exptl_special_details           
; 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20070
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_sigmaI/netI    0.0561
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.89
_diffrn_reflns_theta_max         28.34
_reflns_number_total             5351
_reflns_number_gt                4177
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'SMART (Bruker, 2007)'
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'

_refine_special_details          
; 
;

_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^)+(0.0420P)^2^+0.9000P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5351
_refine_ls_number_parameters     308
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0413
_refine_ls_wR_factor_ref         0.0962
_refine_ls_wR_factor_gt          0.0892
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      1.004
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.36911(3) 0.342613(16) 0.75992(2) 0.01140(9) Uani 1 1 d . . .
O1 O 0.55604(18) 0.34324(10) 0.84813(12) 0.0165(3) Uani 1 1 d . . .
H1AO H 0.621(3) 0.3110(16) 0.8534(19) 0.020 Uiso 1 1 d . . .
H1BO H 0.541(3) 0.3609(16) 0.899(2) 0.020 Uiso 1 1 d . . .
O2 O 0.3437(2) 0.45824(10) 0.81016(12) 0.0166(4) Uani 1 1 d . . .
H2AO H 0.275(3) 0.4718(15) 0.8443(19) 0.020 Uiso 1 1 d . . .
H2BO H 0.403(3) 0.4819(16) 0.8276(19) 0.020 Uiso 1 1 d . . .
O3 O 0.26618(19) 0.29646(11) 0.87990(12) 0.0196(4) Uani 1 1 d . . .
H3AO H 0.281(3) 0.3213(16) 0.929(2) 0.024 Uiso 1 1 d . . .
H3BO H 0.190(3) 0.2768(16) 0.8810(19) 0.024 Uiso 1 1 d . . .
N1 N 0.3863(2) 0.22504(10) 0.70282(13) 0.0132(4) Uani 1 1 d . . .
C2 C 0.4769(2) 0.22938(13) 0.61755(16) 0.0149(5) Uani 1 1 d . . .
H2A H 0.4141 0.2387 0.5609 0.018 Uiso 1 1 calc R . .
H2B H 0.5284 0.1776 0.6093 0.018 Uiso 1 1 calc R . .
C3 C 0.5862(2) 0.29751(12) 0.62799(16) 0.0137(4) Uani 1 1 d . . .
H3A H 0.6547 0.2864 0.6814 0.016 Uiso 1 1 calc R . .
H3B H 0.6421 0.3028 0.5697 0.016 Uiso 1 1 calc R . .
N4 N 0.5047(2) 0.37284(11) 0.64563(14) 0.0120(4) Uani 1 1 d . . .
H4 H 0.457(3) 0.3846(14) 0.5967(18) 0.014 Uiso 1 1 d . . .
C5 C 0.5997(2) 0.44348(13) 0.66168(16) 0.0145(5) Uani 1 1 d . . .
H5A H 0.6710 0.4296 0.7125 0.017 Uiso 1 1 calc R . .
H5B H 0.5394 0.4881 0.6854 0.017 Uiso 1 1 calc R . .
C6 C 0.6826(2) 0.47494(12) 0.57839(15) 0.0120(4) Uani 1 1 d . . .
C7 C 0.7836(2) 0.53604(13) 0.59607(16) 0.0146(5) Uani 1 1 d . . .
H7 H 0.8017 0.5537 0.6591 0.017 Uiso 1 1 calc R . .
C8 C 0.8579(2) 0.57145(13) 0.52323(16) 0.0148(5) Uani 1 1 d . . .
H8 H 0.9268 0.6126 0.5370 0.018 Uiso 1 1 calc R . .
C9 C 0.6586(2) 0.44981(12) 0.48548(16) 0.0140(5) Uani 1 1 d . . .
H9 H 0.5906 0.4081 0.4719 0.017 Uiso 1 1 calc R . .
C10 C 0.7336(2) 0.48537(12) 0.41226(16) 0.0140(5) Uani 1 1 d . . .
H10 H 0.7168 0.4671 0.3493 0.017 Uiso 1 1 calc R . .
C11 C 0.8328(2) 0.54735(12) 0.42996(16) 0.0131(4) Uani 1 1 d . . .
C12 C 0.9124(2) 0.58598(13) 0.35010(16) 0.0149(5) Uani 1 1 d . . .
H12A H 1.0102 0.6021 0.3736 0.018 Uiso 1 1 calc R . .
H12B H 0.9250 0.5454 0.2998 0.018 Uiso 1 1 calc R . .
N13 N 0.8380(2) 0.65837(10) 0.30819(14) 0.0124(4) Uani 1 1 d . . .
H13 H 0.886(3) 0.6689(14) 0.2613(18) 0.015 Uiso 1 1 d . . .
C14 C 0.8459(2) 0.72972(12) 0.37092(16) 0.0145(5) Uani 1 1 d . . .
H14A H 0.9484 0.7449 0.3832 0.017 Uiso 1 1 calc R . .
H14B H 0.8018 0.7170 0.4321 0.017 Uiso 1 1 calc R . .
C15 C 0.7651(2) 0.79916(13) 0.32340(17) 0.0152(5) Uani 1 1 d . . .
H15A H 0.7633 0.8459 0.3668 0.018 Uiso 1 1 calc R . .
H15B H 0.8162 0.8157 0.2660 0.018 Uiso 1 1 calc R . .
C16 C 0.4503(3) 0.16535(13) 0.77020(17) 0.0175(5) Uani 1 1 d . . .
H16A H 0.4415 0.1111 0.7432 0.026 Uiso 1 1 calc R . .
H16B H 0.3988 0.1676 0.8297 0.026 Uiso 1 1 calc R . .
H16C H 0.5529 0.1780 0.7821 0.026 Uiso 1 1 calc R . .
N1A N 0.1079(2) 0.74759(11) 0.13875(13) 0.0160(4) Uani 1 1 d . . .
O1A O 0.09953(19) 0.68957(10) 0.19595(13) 0.0236(4) Uani 1 1 d . . .
O2A O -0.00404(17) 0.78539(10) 0.11327(12) 0.0231(4) Uani 1 1 d . . .
O3A O 0.22766(17) 0.76631(10) 0.10649(13) 0.0231(4) Uani 1 1 d . . .
N1B N 0.4135(2) 0.40955(12) 0.07388(14) 0.0196(4) Uani 1 1 d . . .
O1B O 0.40922(19) 0.45370(10) 0.14690(12) 0.0239(4) Uani 1 1 d . . .
O2B O 0.52642(18) 0.40587(10) 0.02831(12) 0.0224(4) Uani 1 1 d . . .
O3B O 0.3027(2) 0.37066(13) 0.04961(14) 0.0400(5) Uani 1 1 d . . .
O1S O 0.1490(2) 0.53705(13) 0.11297(15) 0.0305(5) Uani 1 1 d . . .
H1SA H 0.220(4) 0.5120(18) 0.129(2) 0.037 Uiso 1 1 d . . .
H1SB H 0.160(3) 0.5816(19) 0.135(2) 0.037 Uiso 1 1 d . . .
O2S O 0.1292(2) 0.52023(11) 0.91010(14) 0.0240(4) Uani 1 1 d . . .
H2SA H 0.053(3) 0.5015(17) 0.904(2) 0.029 Uiso 1 1 d . . .
H2SB H 0.140(3) 0.5269(17) 0.968(2) 0.029 Uiso 1 1 d . . .

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 0.00981(15) 0.01338(14) 0.01095(16) -0.00056(11) -0.00085(10) -0.00111(11)
O1 0.0138(9) 0.0215(8) 0.0139(9) -0.0026(7) -0.0037(7) 0.0025(7)
O2 0.0135(9) 0.0184(8) 0.0179(9) -0.0052(7) 0.0014(7) -0.0028(7)
O3 0.0176(9) 0.0284(9) 0.0127(9) -0.0019(7) -0.0012(7) -0.0098(7)
N1 0.0113(9) 0.0146(9) 0.0134(10) 0.0018(7) -0.0023(7) -0.0013(7)
C2 0.0152(11) 0.0151(10) 0.0145(12) -0.0007(8) 0.0012(9) 0.0007(9)
C3 0.0141(11) 0.0134(10) 0.0137(12) -0.0001(8) 0.0020(9) 0.0027(8)
N4 0.0106(10) 0.0129(9) 0.0123(10) -0.0004(7) -0.0020(8) -0.0010(7)
C5 0.0137(11) 0.0156(10) 0.0141(12) -0.0016(8) -0.0005(9) -0.0033(9)
C6 0.0121(11) 0.0104(10) 0.0133(11) 0.0001(8) -0.0014(9) 0.0018(8)
C7 0.0143(12) 0.0167(10) 0.0125(11) -0.0009(8) -0.0035(9) 0.0005(9)
C8 0.0121(11) 0.0133(10) 0.0188(12) 0.0018(8) -0.0040(9) -0.0002(8)
C9 0.0130(11) 0.0122(10) 0.0166(12) 0.0000(8) -0.0016(9) -0.0008(8)
C10 0.0125(11) 0.0149(10) 0.0144(12) -0.0016(8) -0.0013(9) 0.0011(8)
C11 0.0095(11) 0.0129(10) 0.0168(12) 0.0018(8) -0.0007(9) 0.0025(8)
C12 0.0113(11) 0.0153(10) 0.0182(12) 0.0005(9) 0.0001(9) 0.0026(8)
N13 0.0121(10) 0.0141(9) 0.0111(10) -0.0003(7) -0.0001(8) 0.0010(7)
C14 0.0111(11) 0.0161(10) 0.0161(12) -0.0014(8) -0.0036(9) -0.0005(8)
C15 0.0129(11) 0.0144(10) 0.0181(12) -0.0005(9) -0.0024(9) -0.0016(8)
C16 0.0181(12) 0.0150(11) 0.0189(13) 0.0038(9) -0.0044(10) 0.0014(9)
N1A 0.0155(10) 0.0170(9) 0.0155(10) 0.0001(7) -0.0016(8) -0.0015(8)
O1A 0.0192(9) 0.0258(9) 0.0259(10) 0.0109(7) 0.0037(8) 0.0013(7)
O2A 0.0137(9) 0.0249(9) 0.0304(10) 0.0046(7) -0.0039(7) 0.0033(7)
O3A 0.0121(8) 0.0273(9) 0.0300(10) 0.0090(7) 0.0030(7) -0.0017(7)
N1B 0.0212(11) 0.0210(10) 0.0163(11) -0.0011(8) -0.0049(9) -0.0022(8)
O1B 0.0220(9) 0.0296(9) 0.0201(9) -0.0128(7) -0.0010(7) -0.0032(7)
O2B 0.0179(9) 0.0302(9) 0.0192(9) -0.0046(7) 0.0003(7) 0.0048(7)
O3B 0.0342(12) 0.0568(13) 0.0292(12) -0.0205(10) 0.0049(9) -0.0273(10)
O1S 0.0190(10) 0.0350(11) 0.0373(12) -0.0126(9) -0.0057(9) 0.0013(8)
O2S 0.0189(10) 0.0303(10) 0.0230(10) -0.0019(8) 0.0052(8) -0.0019(8)

_geom_special_details            
; 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O2 2.0606(17) . ?
Ni1 O1 2.1036(17) . ?
Ni1 O3 2.1134(18) . ?
Ni1 N1 2.1182(19) . ?
Ni1 N13 2.119(2) 3_666 ?
Ni1 N4 2.133(2) . ?
O1 H1AO 0.81(3) . ?
O1 H1BO 0.80(3) . ?
O2 H2AO 0.84(3) . ?
O2 H2BO 0.71(3) . ?
O3 H3AO 0.82(3) . ?
O3 H3BO 0.78(3) . ?
N1 C16 1.487(3) . ?
N1 C2 1.490(3) . ?
N1 C15 1.492(3) 3_666 ?
C2 C3 1.519(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N4 1.483(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
N4 C5 1.477(3) . ?
N4 H4 0.83(3) . ?
C5 C6 1.516(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C9 1.393(3) . ?
C6 C7 1.395(3) . ?
C7 C8 1.385(3) . ?
C7 H7 0.9500 . ?
C8 C11 1.394(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.394(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.395(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.508(3) . ?
C12 N13 1.498(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
N13 C14 1.480(3) . ?
N13 Ni1 2.119(2) 3_666 ?
N13 H13 0.83(2) . ?
C14 C15 1.520(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 N1 1.492(3) 3_666 ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
N1A O3A 1.247(2) . ?
N1A O2A 1.254(2) . ?
N1A O1A 1.262(2) . ?
N1B O2B 1.242(3) . ?
N1B O3B 1.249(3) . ?
N1B O1B 1.269(2) . ?
O1S H1SA 0.80(3) . ?
O1S H1SB 0.81(3) . ?
O2S H2SA 0.78(3) . ?
O2S H2SB 0.83(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ni1 O1 83.65(7) . . ?
O2 Ni1 O3 90.06(7) . . ?
O1 Ni1 O3 84.45(7) . . ?
O2 Ni1 N1 176.93(7) . . ?
O1 Ni1 N1 99.36(7) . . ?
O3 Ni1 N1 90.81(7) . . ?
O2 Ni1 N13 93.13(7) . 3_666 ?
O1 Ni1 N13 170.64(7) . 3_666 ?
O3 Ni1 N13 86.77(8) . 3_666 ?
N1 Ni1 N13 83.98(7) . 3_666 ?
O2 Ni1 N4 96.80(7) . . ?
O1 Ni1 N4 87.76(7) . . ?
O3 Ni1 N4 169.00(7) . . ?
N1 Ni1 N4 82.79(7) . . ?
N13 Ni1 N4 101.37(8) 3_666 . ?
Ni1 O1 H1AO 130.4(19) . . ?
Ni1 O1 H1BO 113(2) . . ?
H1AO O1 H1BO 108(3) . . ?
Ni1 O2 H2AO 122.9(18) . . ?
Ni1 O2 H2BO 123(2) . . ?
H2AO O2 H2BO 104(3) . . ?
Ni1 O3 H3AO 116(2) . . ?
Ni1 O3 H3BO 127(2) . . ?
H3AO O3 H3BO 109(3) . . ?
C16 N1 C2 109.33(17) . . ?
C16 N1 C15 109.54(17) . 3_666 ?
C2 N1 C15 110.72(17) . 3_666 ?
C16 N1 Ni1 113.58(14) . . ?
C2 N1 Ni1 108.36(12) . . ?
C15 N1 Ni1 105.25(13) 3_666 . ?
N1 C2 C3 110.04(17) . . ?
N1 C2 H2A 109.7 . . ?
C3 C2 H2A 109.7 . . ?
N1 C2 H2B 109.7 . . ?
C3 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
N4 C3 C2 107.72(18) . . ?
N4 C3 H3A 110.2 . . ?
C2 C3 H3A 110.2 . . ?
N4 C3 H3B 110.2 . . ?
C2 C3 H3B 110.2 . . ?
H3A C3 H3B 108.5 . . ?
C5 N4 C3 113.09(17) . . ?
C5 N4 Ni1 115.32(14) . . ?
C3 N4 Ni1 103.93(13) . . ?
C5 N4 H4 104.0(17) . . ?
C3 N4 H4 108.4(17) . . ?
Ni1 N4 H4 112.1(17) . . ?
N4 C5 C6 117.57(18) . . ?
N4 C5 H5A 107.9 . . ?
C6 C5 H5A 107.9 . . ?
N4 C5 H5B 107.9 . . ?
C6 C5 H5B 107.9 . . ?
H5A C5 H5B 107.2 . . ?
C9 C6 C7 118.4(2) . . ?
C9 C6 C5 124.20(19) . . ?
C7 C6 C5 117.31(19) . . ?
C8 C7 C6 121.1(2) . . ?
C8 C7 H7 119.5 . . ?
C6 C7 H7 119.5 . . ?
C7 C8 C11 120.8(2) . . ?
C7 C8 H8 119.6 . . ?
C11 C8 H8 119.6 . . ?
C6 C9 C10 120.5(2) . . ?
C6 C9 H9 119.7 . . ?
C10 C9 H9 119.7 . . ?
C9 C10 C11 121.0(2) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 H10 119.5 . . ?
C8 C11 C10 118.2(2) . . ?
C8 C11 C12 121.18(19) . . ?
C10 C11 C12 120.6(2) . . ?
N13 C12 C11 114.21(18) . . ?
N13 C12 H12A 108.7 . . ?
C11 C12 H12A 108.7 . . ?
N13 C12 H12B 108.7 . . ?
C11 C12 H12B 108.7 . . ?
H12A C12 H12B 107.6 . . ?
C14 N13 C12 112.81(17) . . ?
C14 N13 Ni1 107.99(13) . 3_666 ?
C12 N13 Ni1 124.97(14) . 3_666 ?
C14 N13 H13 107.1(17) . . ?
C12 N13 H13 103.6(17) . . ?
Ni1 N13 H13 97.8(18) 3_666 . ?
N13 C14 C15 108.89(18) . . ?
N13 C14 H14A 109.9 . . ?
C15 C14 H14A 109.9 . . ?
N13 C14 H14B 109.9 . . ?
C15 C14 H14B 109.9 . . ?
H14A C14 H14B 108.3 . . ?
N1 C15 C14 110.63(17) 3_666 . ?
N1 C15 H15A 109.5 3_666 . ?
C14 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 3_666 . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 108.1 . . ?
N1 C16 H16A 109.5 . . ?
N1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O3A N1A O2A 120.15(18) . . ?
O3A N1A O1A 119.72(19) . . ?
O2A N1A O1A 120.11(19) . . ?
O2B N1B O3B 121.6(2) . . ?
O2B N1B O1B 119.81(19) . . ?
O3B N1B O1B 118.6(2) . . ?
H1SA O1S H1SB 106(3) . . ?
H2SA O2S H2SB 104(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
#O2 Ni1 N1 C16 -156.8(13) . . . . ? 
#O2 Ni1 N1 C2 81.5(14) . . . . ? 
#O2 Ni1 N1 C15 -37.0(14) . . . 3_666 ? 
O1 Ni1 N1 C16 34.08(15) . . . . ?
O3 Ni1 N1 C16 -50.43(15) . . . . ?
N13 Ni1 N1 C16 -137.10(15) 3_666 . . . ?
N4 Ni1 N1 C16 120.60(16) . . . . ?
O1 Ni1 N1 C2 -87.62(14) . . . . ?
O3 Ni1 N1 C2 -172.13(13) . . . . ?
N13 Ni1 N1 C2 101.20(14) 3_666 . . . ?
N4 Ni1 N1 C2 -1.10(13) . . . . ?
O1 Ni1 N1 C15 153.90(13) . . . 3_666 ?
O3 Ni1 N1 C15 69.39(14) . . . 3_666 ?
N13 Ni1 N1 C15 -17.28(13) 3_666 . . 3_666 ?
N4 Ni1 N1 C15 -119.58(14) . . . 3_666 ?
C16 N1 C2 C3 -94.4(2) . . . . ?
C15 N1 C2 C3 144.86(17) 3_666 . . . ?
Ni1 N1 C2 C3 29.9(2) . . . . ?
N1 C2 C3 N4 -56.1(2) . . . . ?
C2 C3 N4 C5 177.26(18) . . . . ?
C2 C3 N4 Ni1 51.47(18) . . . . ?
O2 Ni1 N4 C5 31.08(16) . . . . ?
O1 Ni1 N4 C5 -52.25(15) . . . . ?
O3 Ni1 N4 C5 -97.1(4) . . . . ?
N1 Ni1 N4 C5 -151.98(16) . . . . ?
N13 Ni1 N4 C5 125.67(15) 3_666 . . . ?
O2 Ni1 N4 C3 155.45(13) . . . . ?
O1 Ni1 N4 C3 72.11(13) . . . . ?
O3 Ni1 N4 C3 27.2(4) . . . . ?
N1 Ni1 N4 C3 -27.62(13) . . . . ?
N13 Ni1 N4 C3 -109.96(13) 3_666 . . . ?
C3 N4 C5 C6 69.0(2) . . . . ?
Ni1 N4 C5 C6 -171.54(14) . . . . ?
N4 C5 C6 C9 10.2(3) . . . . ?
N4 C5 C6 C7 -173.37(19) . . . . ?
C9 C6 C7 C8 0.4(3) . . . . ?
C5 C6 C7 C8 -176.3(2) . . . . ?
C6 C7 C8 C11 0.5(3) . . . . ?
C7 C6 C9 C10 -0.3(3) . . . . ?
C5 C6 C9 C10 176.1(2) . . . . ?
C6 C9 C10 C11 -0.7(3) . . . . ?
C7 C8 C11 C10 -1.5(3) . . . . ?
C7 C8 C11 C12 179.53(19) . . . . ?
C9 C10 C11 C8 1.6(3) . . . . ?
C9 C10 C11 C12 -179.43(19) . . . . ?
C8 C11 C12 N13 -89.8(2) . . . . ?
C10 C11 C12 N13 91.3(2) . . . . ?
C11 C12 N13 C14 72.5(2) . . . . ?
C11 C12 N13 Ni1 -62.2(2) . . . 3_666 ?
C12 N13 C14 C15 -178.81(18) . . . . ?
Ni1 N13 C14 C15 -36.6(2) 3_666 . . . ?
N13 C14 C15 N1 54.9(2) . . . 3_666 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1AO O3A 0.81(3) 1.97(3) 2.763(2) 169(3) 3_666
O1 H1BO O2B 0.80(3) 1.98(3) 2.776(2) 174(3) 1_556
O2 H2AO O2S 0.84(3) 1.84(3) 2.671(3) 169(3) .
O2 H2BO O1B 0.71(3) 2.06(3) 2.763(2) 169(3) 3_666
O3 H3AO O3B 0.82(3) 1.90(3) 2.714(3) 174(3) 1_556
O3 H3BO O2A 0.78(3) 2.01(3) 2.779(3) 174(3) 3_566
N13 H13 O1A 0.83(2) 2.22(3) 2.972(3) 150(2) 1_655
N13 H13 O3 0.83(2) 2.48(3) 2.907(3) 113(2) 3_666
O1S H1SA O1B 0.80(3) 2.01(3) 2.802(3) 170(3) .
O1S H1SB O1A 0.81(3) 2.07(3) 2.831(3) 157(3) .
O2S H2SA O1S 0.78(3) 1.98(3) 2.750(3) 175(3) 3_566
O2S H2SB O1S 0.83(3) 2.06(3) 2.889(3) 175(3) 1_556

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.078

_iucr_refine_instruction_details 
; 
TITL 12003 in P2(1)/n 
CELL 0.71073   9.233   16.580   14.170   90.000  91.545  90.000 
ZERR    2.00   0.003    0.005    0.004    0.000   0.007   0.000 
LATT  1 
SYMM 0.5-X, 0.5+Y, 0.5-Z 
SFAC C  H   N  O  Ni 
UNIT 52 124 20 44 4 
TEMP -173 
SIZE 0.11 0.30 0.34 
acta 50.5 
conf 
wpdb -2 
eqiv $1 -x+1, -y+1, -z+1 
eqiv $2 x, y, z+1 
eqiv $3 -x, -y+1, -z+1 
eqiv $4 x+1, y, z 
htab o1 o3a_$1 
htab o1 o2b_$2 
htab o2 o2s 
htab o2 o1b_$1 
htab o3 o3b_$2 
htab o3 o2a_$3 
htab n13 o1a_$4 
htab n13 o3_$1 
htab o1s o1b 
htab o1s o1a 
htab o2s o1s_$3 
htab o2s o1s_$2 
htab 
  
L.S. 4 
BOND $h 
FMAP 2 
PLAN 20 
  
WGHT    0.042000    0.900000 
FVAR       0.50749 
NI1   5    0.369112    0.342613    0.759920    11.00000    0.00981    0.01338 = 
         0.01095   -0.00056   -0.00085   -0.00111 
O1    4    0.556042    0.343245    0.848134    11.00000    0.01384    0.02146 = 
         0.01385   -0.00255   -0.00366    0.00248 
H1AO  2    0.620929    0.310975    0.853427    11.00000   -1.20000 
H1BO  2    0.541248    0.360947    0.899345    11.00000   -1.20000 
O2    4    0.343672    0.458237    0.810163    11.00000    0.01347    0.01839 = 
         0.01789   -0.00518    0.00142   -0.00282 
H2AO  2    0.274720    0.471837    0.844329    11.00000   -1.20000 
H2BO  2    0.403074    0.481941    0.827612    11.00000   -1.20000 
O3    4    0.266183    0.296457    0.879902    11.00000    0.01763    0.02843 = 
         0.01269   -0.00191   -0.00125   -0.00981 
H3AO  2    0.281174    0.321301    0.928985    11.00000   -1.20000 
H3BO  2    0.189937    0.276799    0.880991    11.00000   -1.20000 
N1    3    0.386346    0.225043    0.702822    11.00000    0.01134    0.01461 = 
         0.01337    0.00181   -0.00234   -0.00128 
C2    1    0.476894    0.229381    0.617548    11.00000    0.01523    0.01508 = 
         0.01450   -0.00068    0.00124    0.00071 
AFIX  23 
H2A   2    0.414079    0.238674    0.560866    11.00000   -1.20000 
H2B   2    0.528421    0.177603    0.609267    11.00000   -1.20000 
AFIX   0 
C3    1    0.586166    0.297508    0.627991    11.00000    0.01410    0.01342 = 
         0.01371   -0.00012    0.00200    0.00268 
AFIX  23 
H3A   2    0.654665    0.286375    0.681357    11.00000   -1.20000 
H3B   2    0.642134    0.302788    0.569694    11.00000   -1.20000 
AFIX   0 
N4    3    0.504741    0.372841    0.645635    11.00000    0.01061    0.01295 = 
         0.01233   -0.00038   -0.00199   -0.00104 
H4    2    0.456853    0.384582    0.596724    11.00000   -1.20000 
C5    1    0.599740    0.443480    0.661680    11.00000    0.01373    0.01560 = 
         0.01414   -0.00159   -0.00051   -0.00327 
AFIX  23 
H5A   2    0.671005    0.429565    0.712546    11.00000   -1.20000 
H5B   2    0.539437    0.488087    0.685406    11.00000   -1.20000 
AFIX   0 
C6    1    0.682585    0.474935    0.578393    11.00000    0.01214    0.01045 = 
         0.01335    0.00005   -0.00135    0.00178 
C7    1    0.783579    0.536041    0.596073    11.00000    0.01425    0.01669 = 
         0.01255   -0.00090   -0.00355    0.00048 
AFIX  43 
H7    2    0.801663    0.553662    0.659088    11.00000   -1.20000 
AFIX   0 
C8    1    0.857937    0.571449    0.523232    11.00000    0.01207    0.01331 = 
         0.01876    0.00181   -0.00397   -0.00024 
AFIX  43 
H8    2    0.926839    0.612637    0.537010    11.00000   -1.20000 
AFIX   0 
C9    1    0.658575    0.449812    0.485477    11.00000    0.01299    0.01219 = 
         0.01658    0.00001   -0.00158   -0.00082 
AFIX  43 
H9    2    0.590564    0.408122    0.471920    11.00000   -1.20000 
AFIX   0 
C10   1    0.733559    0.485368    0.412257    11.00000    0.01255    0.01489 = 
         0.01439   -0.00162   -0.00128    0.00110 
AFIX  43 
H10   2    0.716827    0.467131    0.349348    11.00000   -1.20000 
AFIX   0 
C11   1    0.832849    0.547354    0.429956    11.00000    0.00948    0.01294 = 
         0.01680    0.00182   -0.00065    0.00252 
C12   1    0.912439    0.585978    0.350100    11.00000    0.01127    0.01530 = 
         0.01824    0.00048    0.00010    0.00261 
AFIX  23 
H12A  2    1.010152    0.602125    0.373578    11.00000   -1.20000 
H12B  2    0.924991    0.545368    0.299757    11.00000   -1.20000 
AFIX   0 
N13   3    0.838027    0.658367    0.308192    11.00000    0.01213    0.01412 = 
         0.01107   -0.00025   -0.00006    0.00096 
H13   2    0.886370    0.668886    0.261275    11.00000   -1.20000 
C14   1    0.845930    0.729722    0.370924    11.00000    0.01113    0.01607 = 
         0.01613   -0.00138   -0.00364   -0.00047 
AFIX  23 
H14A  2    0.948399    0.744933    0.383205    11.00000   -1.20000 
H14B  2    0.801815    0.717005    0.432070    11.00000   -1.20000 
AFIX   0 
C15   1    0.765097    0.799163    0.323396    11.00000    0.01294    0.01439 = 
         0.01814   -0.00052   -0.00240   -0.00158 
AFIX  23 
H15A  2    0.763315    0.845921    0.366801    11.00000   -1.20000 
H15B  2    0.816224    0.815661    0.265988    11.00000   -1.20000 
AFIX   0 
C16   1    0.450347    0.165348    0.770201    11.00000    0.01811    0.01504 = 
         0.01894    0.00375   -0.00438    0.00136 
AFIX 137 
H16A  2    0.441510    0.111085    0.743235    11.00000   -1.50000 
H16B  2    0.398816    0.167608    0.829707    11.00000   -1.50000 
H16C  2    0.552907    0.177997    0.782078    11.00000   -1.50000 
AFIX   0 
N1A   3    0.107923    0.747586    0.138747    11.00000    0.01551    0.01700 = 
         0.01547    0.00013   -0.00164   -0.00148 
O1A   4    0.099528    0.689568    0.195949    11.00000    0.01920    0.02578 = 
         0.02593    0.01092    0.00374    0.00134 
O2A   4   -0.004042    0.785388    0.113266    11.00000    0.01367    0.02493 = 
         0.03036    0.00462   -0.00390    0.00334 
O3A   4    0.227658    0.766311    0.106493    11.00000    0.01207    0.02725 = 
         0.03003    0.00905    0.00295   -0.00173 
N1B   3    0.413513    0.409552    0.073877    11.00000    0.02122    0.02096 = 
         0.01630   -0.00110   -0.00487   -0.00217 
O1B   4    0.409220    0.453703    0.146897    11.00000    0.02203    0.02959 = 
         0.02013   -0.01281   -0.00097   -0.00319 
O2B   4    0.526423    0.405872    0.028308    11.00000    0.01793    0.03020 = 
         0.01918   -0.00461    0.00033    0.00482 
O3B   4    0.302745    0.370665    0.049614    11.00000    0.03425    0.05680 = 
         0.02918   -0.02045    0.00490   -0.02733 
O1S   4    0.148973    0.537053    0.112968    11.00000    0.01898    0.03498 = 
         0.03725   -0.01264   -0.00566    0.00132 
H1SA  2    0.219920    0.512040    0.129197    11.00000   -1.20000 
H1SB  2    0.159873    0.581615    0.134785    11.00000   -1.20000 
O2S   4    0.129244    0.520231    0.910098    11.00000    0.01895    0.03030 = 
         0.02303   -0.00186    0.00516   -0.00187 
H2SA  2    0.052624    0.501487    0.903963    11.00000   -1.20000 
H2SB  2    0.139819    0.526908    0.968003    11.00000   -1.20000 
  
HKLF 4 
  
REM  12003 in P2(1)/n 
REM R1 =  0.0413 for   4177 Fo > 4sig(Fo)  and  0.0593 for all   5351 data 
REM    308 parameters refined using      0 restraints 
  
END 
  
WGHT      0.0340      0.8739 
REM Highest difference peak  0.477,  deepest hole -0.464,  1-sigma level  0.078 
Q1    1   0.3562  0.4025  0.7861  11.00000  0.05    0.48 
Q2    1   0.3651  0.2899  0.7943  11.00000  0.05    0.46 
Q3    1   0.8625  0.5468  0.4750  11.00000  0.05    0.43 
Q4    1   0.8541  0.5691  0.3960  11.00000  0.05    0.41 
Q5    1   0.3864  0.2842  0.7270  11.00000  0.05    0.40 
Q6    1   0.7424  0.4990  0.5828  11.00000  0.05    0.39 
Q7    1   0.6583  0.4609  0.6182  11.00000  0.05    0.36 
Q8    1   0.6894  0.4475  0.5415  11.00000  0.05    0.35 
Q9    1   0.4461  0.3552  0.6977  11.00000  0.05    0.33 
Q10   1   0.7836  0.5184  0.4338  11.00000  0.05    0.32 
Q11   1   0.5436  0.3314  0.6456  11.00000  0.05    0.32 
Q12   1   0.5449  0.4149  0.6574  11.00000  0.05    0.31 
Q13   1   0.4387  0.2328  0.6644  11.00000  0.05    0.30 
Q14   1   0.4203  0.3951  0.6631  11.00000  0.05    0.30 
Q15   1   0.6439  0.4850  0.5607  11.00000  0.05    0.30 
Q16   1   0.7876  0.5458  0.6201  11.00000  0.05    0.30 
Q17   1   0.3220  0.3457  0.8325  11.00000  0.05    0.29 
Q18   1   0.4682  0.2099  0.5788  11.00000  0.05    0.29 
Q19   1   0.6902  0.4829  0.4581  11.00000  0.05    0.28 
Q20   1   0.8359  0.6969  0.3348  11.00000  0.05    0.28 
  
;

#===END 
_database_code_depnum_ccdc_archive 'CCDC 970398'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_NiMePEA_Oxalate

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H46 N6 Ni2 O10, 6.85(H2 O)'
_chemical_formula_sum            'C30 H59.43 N6 Ni2 O16.85'
_chemical_formula_weight         891.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_Hall  '-P 1 '
_symmetry_space_group_name_H-M   'P -1   '

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

_cell_length_a                   8.9574(10)
_cell_length_b                   15.128(2)
_cell_length_c                   15.402(2)
_cell_angle_alpha                94.199(9)
_cell_angle_beta                 103.866(9)
_cell_angle_gamma                106.950(10)
_cell_volume                     1915.1(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    90.0(5)
_cell_measurement_reflns_used    4572
_cell_measurement_theta_min      3.96
_cell_measurement_theta_max      63.66

_exptl_crystal_description       needle
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             945
_exptl_absorpt_coefficient_mu    1.923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6991
_exptl_absorpt_correction_T_max  0.9625
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      90.0(5)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'I\mS microfocus'
_diffrn_radiation_monochromator  'QUAZAR multilayer optics'
_diffrn_measurement_device_type  'Bruker Kappa APEX-II DUO'
_diffrn_measurement_method       '\f 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            19621
_diffrn_reflns_av_R_equivalents  0.0699
_diffrn_reflns_av_sigmaI/netI    0.0584
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.96
_diffrn_reflns_theta_max         63.77
_reflns_number_total             6208
_reflns_number_gt                4672
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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^)+(0.0628P)^2^+1.1514P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6208
_refine_ls_number_parameters     574
_refine_ls_number_restraints     104
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0471
_refine_ls_wR_factor_ref         0.1211
_refine_ls_wR_factor_gt          0.1097
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.014
_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 0.25975(7) 0.92620(4) 0.26971(4) 0.02130(17) Uani 1 1 d . . .
O1 O 0.4057(3) 0.86772(17) 0.35728(16) 0.0253(6) Uani 1 1 d . . .
O2 O 0.3961(3) 0.89978(17) 0.18854(16) 0.0234(5) Uani 1 1 d . . .
O3 O 0.5859(3) 0.8338(2) 0.18406(18) 0.0383(7) Uani 1 1 d . . .
O4 O 0.5972(3) 0.80013(18) 0.35933(17) 0.0314(6) Uani 1 1 d . . .
O5 O 0.4405(3) 1.05716(19) 0.31920(17) 0.0283(6) Uani 1 1 d D . .
H51 H 0.512(5) 1.076(3) 0.290(3) 0.042 Uiso 1 1 d D . .
H52 H 0.472(5) 1.086(3) 0.3735(19) 0.042 Uiso 1 1 d D . .
N1 N 0.1112(4) 0.9413(2) 0.35398(19) 0.0245(7) Uani 1 1 d . . .
N2 N 0.1315(4) 1.0045(2) 0.1868(2) 0.0243(7) Uani 1 1 d . . .
H2N H 0.040(5) 0.960(3) 0.146(3) 0.029 Uiso 1 1 d . . .
N3 N 0.0903(3) 0.7882(2) 0.2310(2) 0.0214(6) Uani 1 1 d . . .
H3N H 0.137(5) 0.757(3) 0.262(3) 0.026 Uiso 1 1 d . . .
C1 C 0.0010(4) 0.9922(3) 0.3095(2) 0.0270(8) Uani 1 1 d . . .
H1A H -0.0269 1.0279 0.3562 0.032 Uiso 1 1 calc R . .
H1B H -0.1007 0.9466 0.2702 0.032 Uiso 1 1 calc R . .
C2 C 0.0825(5) 1.0583(3) 0.2534(2) 0.0253(8) Uani 1 1 d . . .
H2A H 0.0068 1.0891 0.2214 0.030 Uiso 1 1 calc R . .
H2B H 0.1793 1.1073 0.2932 0.030 Uiso 1 1 calc R . .
C3 C 0.2307(4) 1.0627(2) 0.1359(2) 0.0219(7) Uani 1 1 d . . .
H3A H 0.2746 1.0220 0.1032 0.026 Uiso 1 1 calc R . .
H3B H 0.3244 1.1094 0.1804 0.026 Uiso 1 1 calc R . .
C4 C 0.1524(4) 1.1151(2) 0.0677(2) 0.0235(8) Uani 1 1 d . . .
C5 C -0.0107(4) 1.1095(2) 0.0452(2) 0.0217(7) Uani 1 1 d . . .
H5A H -0.0815 1.0715 0.0747 0.026 Uiso 1 1 calc R . .
C6 C -0.0714(4) 1.1588(2) -0.0196(2) 0.0220(7) Uani 1 1 d . . .
H6 H -0.1826 1.1546 -0.0331 0.026 Uiso 1 1 calc R . .
C7 C 0.0284(4) 1.2144(2) -0.0654(2) 0.0215(7) Uani 1 1 d . . .
C8 C 0.1923(4) 1.2205(2) -0.0420(2) 0.0216(7) Uani 1 1 d . . .
H8 H 0.2637 1.2587 -0.0710 0.026 Uiso 1 1 calc R . .
C9 C 0.2519(4) 1.1715(2) 0.0231(2) 0.0222(7) Uani 1 1 d . . .
H9 H 0.3636 1.1766 0.0375 0.027 Uiso 1 1 calc R . .
C10 C 0.0417(4) 0.7355(3) 0.1381(2) 0.0224(7) Uani 1 1 d . . .
H10A H -0.0399 0.6742 0.1355 0.027 Uiso 1 1 calc R . .
H10B H 0.1377 0.7235 0.1253 0.027 Uiso 1 1 calc R . .
C11 C -0.0496(4) 0.7846(3) 0.2680(2) 0.0252(8) Uani 1 1 d . . .
H11A H -0.1065 0.7194 0.2734 0.030 Uiso 1 1 calc R . .
H11B H -0.1274 0.8085 0.2272 0.030 Uiso 1 1 calc R . .
C12 C 0.0156(4) 0.8449(3) 0.3603(2) 0.0265(8) Uani 1 1 d . . .
H12A H -0.0759 0.8469 0.3850 0.032 Uiso 1 1 calc R . .
H12B H 0.0852 0.8171 0.4021 0.032 Uiso 1 1 calc R . .
C13 C 0.2087(5) 0.9927(3) 0.4452(2) 0.0283(8) Uani 1 1 d . . .
H13A H 0.1375 0.9900 0.4851 0.042 Uiso 1 1 calc R . .
H13B H 0.2617 1.0581 0.4408 0.042 Uiso 1 1 calc R . .
H13C H 0.2913 0.9639 0.4702 0.042 Uiso 1 1 calc R . .
C14 C 0.5016(4) 0.8397(2) 0.3220(2) 0.0233(8) Uani 1 1 d . . .
C15 C 0.4959(4) 0.8580(3) 0.2227(2) 0.0245(8) Uani 1 1 d . . .
Ni2 Ni 0.38121(7) 0.51030(4) 0.27575(4) 0.01920(16) Uani 1 1 d . . .
O6 O 0.2568(3) 0.60477(17) 0.27729(15) 0.0230(5) Uani 1 1 d . . .
O7 O 0.3943(3) 0.52598(17) 0.41211(16) 0.0259(6) Uani 1 1 d . . .
O8 O 0.3802(3) 0.63481(19) 0.51260(16) 0.0335(6) Uani 1 1 d . . .
O9 O 0.1464(3) 0.66496(18) 0.37269(16) 0.0278(6) Uani 1 1 d . . .
O10 O 0.5976(3) 0.62206(18) 0.30139(17) 0.0242(5) Uani 1 1 d D . .
H101 H 0.587(5) 0.677(2) 0.310(3) 0.036 Uiso 1 1 d D . .
H102 H 0.649(5) 0.618(3) 0.354(2) 0.036 Uiso 1 1 d D . .
N4 N 0.1720(3) 0.3891(2) 0.24621(18) 0.0209(6) Uani 1 1 d . . .
N5 N 0.5092(3) 0.4114(2) 0.3026(2) 0.0193(6) Uani 1 1 d . . .
H5N H 0.523(5) 0.414(3) 0.358(3) 0.023 Uiso 1 1 d . . .
N6 N 0.3209(3) 0.5011(2) 0.13316(19) 0.0190(6) Uani 1 1 d . . .
H6N H 0.372(5) 0.468(3) 0.116(3) 0.023 Uiso 1 1 d . . .
C16 C 0.2305(4) 0.3160(3) 0.2869(2) 0.0218(7) Uani 1 1 d . . .
H16A H 0.1485 0.2540 0.2611 0.026 Uiso 1 1 calc R . .
H16B H 0.2437 0.3258 0.3529 0.026 Uiso 1 1 calc R . .
C17 C 0.3906(4) 0.3167(2) 0.2702(2) 0.0205(7) Uani 1 1 d . . .
H17A H 0.4310 0.2706 0.3027 0.025 Uiso 1 1 calc R . .
H17B H 0.3756 0.2993 0.2047 0.025 Uiso 1 1 calc R . .
C18 C 0.6685(4) 0.4174(3) 0.2855(2) 0.0216(7) Uani 1 1 d . . .
H18A H 0.7023 0.3645 0.3076 0.026 Uiso 1 1 calc R . .
H18B H 0.7509 0.4761 0.3205 0.026 Uiso 1 1 calc R . .
C19 C 0.6643(4) 0.4153(2) 0.1867(2) 0.0191(7) Uani 1 1 d . . .
C20 C 0.6432(4) 0.3331(3) 0.1311(2) 0.0217(7) Uani 1 1 d . . .
H20 H 0.6324 0.2765 0.1557 0.026 Uiso 1 1 calc R . .
C21 C 0.6379(4) 0.3330(3) 0.0402(2) 0.0210(7) Uani 1 1 d . . .
H21 H 0.6238 0.2763 0.0036 0.025 Uiso 1 1 calc R . .
C22 C 0.6529(4) 0.4151(2) 0.0016(2) 0.0189(7) Uani 1 1 d . . .
C23 C 0.6797(4) 0.4973(3) 0.0581(2) 0.0205(7) Uani 1 1 d . . .
H23 H 0.6941 0.5544 0.0341 0.025 Uiso 1 1 calc R . .
C24 C 0.6858(4) 0.4975(2) 0.1492(2) 0.0205(7) Uani 1 1 d . . .
H24 H 0.7050 0.5548 0.1865 0.025 Uiso 1 1 calc R . .
C25 C 0.3689(4) 0.5913(3) 0.0996(2) 0.0231(8) Uani 1 1 d . . .
H25A H 0.4845 0.6247 0.1308 0.028 Uiso 1 1 calc R . .
H25B H 0.3048 0.6296 0.1167 0.028 Uiso 1 1 calc R . .
C26 C 0.1430(4) 0.4528(2) 0.1037(2) 0.0213(7) Uani 1 1 d . . .
H26A H 0.1050 0.4369 0.0369 0.026 Uiso 1 1 calc R . .
H26B H 0.0853 0.4939 0.1234 0.026 Uiso 1 1 calc R . .
C27 C 0.1093(4) 0.3644(3) 0.1467(2) 0.0227(8) Uani 1 1 d . . .
H27A H -0.0090 0.3314 0.1298 0.027 Uiso 1 1 calc R . .
H27B H 0.1625 0.3222 0.1242 0.027 Uiso 1 1 calc R . .
C28 C 0.0415(4) 0.4016(3) 0.2844(2) 0.0236(8) Uani 1 1 d . . .
H28A H -0.0463 0.3419 0.2729 0.035 Uiso 1 1 calc R . .
H28B H -0.0007 0.4484 0.2558 0.035 Uiso 1 1 calc R . .
H28C H 0.0851 0.4227 0.3498 0.035 Uiso 1 1 calc R . .
C29 C 0.2407(4) 0.6252(2) 0.3549(2) 0.0230(8) Uani 1 1 d . . .
C30 C 0.3486(4) 0.5939(3) 0.4347(2) 0.0260(8) Uani 1 1 d . . .
O11 O 0.6609(3) 1.1320(2) 0.22301(19) 0.0347(6) Uani 1 1 d D . .
H111 H 0.748(4) 1.144(3) 0.269(2) 0.052 Uiso 1 1 d D . .
H112 H 0.674(5) 1.093(3) 0.183(2) 0.052 Uiso 1 1 d D . .
O12 O 0.6164(3) 1.17853(19) 0.47315(16) 0.0285(6) Uani 1 1 d D . .
H121 H 0.609(6) 1.166(3) 0.5264(18) 0.043 Uiso 1 1 d D . .
H122 H 0.624(6) 1.2375(14) 0.474(3) 0.043 Uiso 1 1 d D . .
O13 O 0.7946(4) 0.7882(2) 0.52828(19) 0.0411(7) Uani 1 1 d D . .
H131 H 0.772(6) 0.7275(14) 0.512(3) 0.062 Uiso 1 1 d D . .
H132 H 0.737(5) 0.806(3) 0.483(2) 0.062 Uiso 1 1 d D . .
O14 O 0.7319(4) 0.6031(2) 0.4718(2) 0.0307(9) Uani 0.859(7) 1 d PD . .
H141 H 0.826(3) 0.595(4) 0.478(4) 0.046 Uiso 0.859(7) 1 d PD . .
H142 H 0.674(5) 0.562(3) 0.497(3) 0.046 Uiso 0.859(7) 1 d PD . .
O14A O 0.877(3) 0.6116(15) 0.4365(13) 0.038(6) Uani 0.141(7) 1 d P . .
O15 O 0.8781(4) 1.1813(3) 0.3918(2) 0.0508(8) Uani 1 1 d D . .
H151 H 0.975(3) 1.193(4) 0.427(3) 0.076 Uiso 1 1 d D . .
H152 H 0.815(5) 1.180(4) 0.427(3) 0.076 Uiso 1 1 d D . .
O16 O 0.6147(8) 0.9890(3) 0.0809(3) 0.0891(17) Uani 1 1 d D . .
H161 H 0.526(6) 0.972(5) 0.099(6) 0.134 Uiso 1 1 d D . .
H162 H 0.630(9) 0.936(3) 0.066(6) 0.134 Uiso 1 1 d D . .
O17 O 0.0248(6) 0.5906(6) 0.5097(3) 0.108(3) Uani 0.859(7) 1 d PD . .
H171 H 0.048(14) 0.621(7) 0.466(6) 0.163 Uiso 0.859(7) 1 d PD . .
H172 H 0.080(13) 0.552(6) 0.515(8) 0.163 Uiso 0.859(7) 1 d PD . .

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 0.0185(3) 0.0252(3) 0.0186(3) 0.0014(2) 0.0037(2) 0.0061(3)
O1 0.0206(13) 0.0301(14) 0.0217(13) 0.0016(10) 0.0031(10) 0.0055(11)
O2 0.0184(12) 0.0301(14) 0.0225(12) 0.0045(10) 0.0059(10) 0.0085(11)
O3 0.0281(15) 0.0600(19) 0.0324(15) 0.0024(13) 0.0121(12) 0.0206(14)
O4 0.0287(14) 0.0301(14) 0.0306(14) 0.0033(11) -0.0026(11) 0.0110(12)
O5 0.0267(14) 0.0332(15) 0.0211(13) 0.0006(11) 0.0063(11) 0.0048(12)
N1 0.0258(16) 0.0292(17) 0.0194(15) 0.0023(12) 0.0075(12) 0.0097(14)
N2 0.0251(16) 0.0251(16) 0.0206(15) 0.0004(13) 0.0051(13) 0.0064(14)
N3 0.0188(15) 0.0256(16) 0.0197(15) 0.0052(12) 0.0033(12) 0.0078(13)
C1 0.0240(19) 0.033(2) 0.0269(19) 0.0038(16) 0.0084(16) 0.0131(17)
C2 0.0261(19) 0.029(2) 0.0221(18) 0.0025(15) 0.0058(15) 0.0111(16)
C3 0.0160(17) 0.0229(18) 0.0252(18) 0.0021(15) 0.0048(14) 0.0048(14)
C4 0.0253(19) 0.0220(18) 0.0180(17) -0.0036(14) 0.0015(14) 0.0049(15)
C5 0.0202(18) 0.0240(19) 0.0195(17) -0.0001(14) 0.0064(14) 0.0051(15)
C6 0.0174(17) 0.0260(19) 0.0191(17) -0.0036(14) 0.0021(14) 0.0059(15)
C7 0.0229(18) 0.0206(18) 0.0167(17) -0.0030(14) 0.0018(14) 0.0050(15)
C8 0.0165(17) 0.0237(19) 0.0214(18) 0.0019(14) 0.0052(14) 0.0020(15)
C9 0.0190(17) 0.0235(19) 0.0195(17) -0.0015(14) 0.0037(14) 0.0026(15)
C10 0.0202(17) 0.0254(19) 0.0204(17) 0.0001(14) 0.0044(14) 0.0072(15)
C11 0.0218(18) 0.028(2) 0.0238(18) 0.0035(15) 0.0063(15) 0.0049(16)
C12 0.0251(19) 0.032(2) 0.0236(19) 0.0062(16) 0.0094(15) 0.0080(17)
C13 0.035(2) 0.029(2) 0.0213(18) -0.0007(15) 0.0091(16) 0.0107(17)
C14 0.0178(18) 0.0225(19) 0.0221(18) 0.0006(15) -0.0017(15) 0.0015(15)
C15 0.0161(17) 0.029(2) 0.0222(18) -0.0015(15) 0.0035(15) 0.0004(16)
Ni2 0.0189(3) 0.0245(3) 0.0139(3) 0.0025(2) 0.0047(2) 0.0065(2)
O6 0.0247(13) 0.0308(14) 0.0150(12) 0.0035(10) 0.0064(10) 0.0101(11)
O7 0.0336(14) 0.0263(14) 0.0181(12) 0.0031(10) 0.0054(11) 0.0116(12)
O8 0.0495(17) 0.0345(15) 0.0172(13) 0.0023(11) 0.0057(12) 0.0176(13)
O9 0.0297(14) 0.0326(14) 0.0236(13) 0.0028(11) 0.0101(11) 0.0116(12)
O10 0.0231(13) 0.0263(14) 0.0206(12) 0.0035(11) 0.0034(10) 0.0060(11)
N4 0.0199(15) 0.0296(16) 0.0171(14) 0.0067(12) 0.0082(12) 0.0106(13)
N5 0.0169(14) 0.0269(16) 0.0129(14) 0.0024(12) 0.0056(12) 0.0042(12)
N6 0.0163(15) 0.0225(16) 0.0184(14) 0.0029(12) 0.0049(12) 0.0066(12)
C16 0.0203(18) 0.0254(19) 0.0193(17) 0.0039(14) 0.0063(14) 0.0058(15)
C17 0.0197(17) 0.0237(18) 0.0196(17) 0.0047(14) 0.0058(14) 0.0084(15)
C18 0.0180(17) 0.031(2) 0.0179(17) 0.0068(15) 0.0070(14) 0.0088(15)
C19 0.0086(15) 0.030(2) 0.0179(17) 0.0032(14) 0.0025(13) 0.0053(14)
C20 0.0141(16) 0.029(2) 0.0245(18) 0.0098(15) 0.0065(14) 0.0083(15)
C21 0.0180(17) 0.0256(19) 0.0195(17) 0.0014(14) 0.0049(14) 0.0080(15)
C22 0.0119(16) 0.0259(19) 0.0195(17) 0.0017(14) 0.0053(13) 0.0067(14)
C23 0.0174(17) 0.0262(19) 0.0192(17) 0.0048(14) 0.0053(14) 0.0082(15)
C24 0.0159(17) 0.0246(19) 0.0187(17) -0.0002(14) 0.0019(13) 0.0061(14)
C25 0.0216(18) 0.028(2) 0.0188(18) 0.0022(15) 0.0056(14) 0.0060(15)
C26 0.0159(17) 0.029(2) 0.0176(17) 0.0023(14) 0.0040(14) 0.0056(15)
C27 0.0157(17) 0.029(2) 0.0204(17) 0.0016(15) 0.0038(14) 0.0045(15)
C28 0.0198(18) 0.031(2) 0.0214(18) 0.0042(15) 0.0093(14) 0.0077(16)
C29 0.0196(18) 0.0238(19) 0.0219(18) 0.0039(15) 0.0055(15) 0.0013(15)
C30 0.028(2) 0.029(2) 0.0190(19) 0.0039(16) 0.0072(15) 0.0053(17)
O11 0.0310(15) 0.0365(16) 0.0316(15) 0.0033(12) 0.0040(12) 0.0073(13)
O12 0.0328(15) 0.0295(14) 0.0194(13) -0.0006(11) 0.0033(11) 0.0083(12)
O13 0.0398(17) 0.056(2) 0.0307(15) 0.0143(14) 0.0086(13) 0.0197(16)
O14 0.0269(18) 0.0353(19) 0.0221(16) 0.0081(13) 0.0038(13) 0.0000(14)
O14A 0.041(13) 0.045(13) 0.030(11) -0.001(9) 0.020(9) 0.013(10)
O15 0.0329(17) 0.085(3) 0.0311(16) 0.0080(16) 0.0039(13) 0.0172(18)
O16 0.193(6) 0.057(2) 0.060(2) 0.027(2) 0.080(3) 0.064(3)
O17 0.044(3) 0.263(9) 0.043(3) 0.064(4) 0.028(2) 0.063(4)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O2 2.039(2) . ?
Ni1 O1 2.077(2) . ?
Ni1 O5 2.108(3) . ?
Ni1 N1 2.114(3) . ?
Ni1 N3 2.135(3) . ?
Ni1 N2 2.160(3) . ?
O1 C14 1.271(4) . ?
O2 C15 1.275(4) . ?
O3 C15 1.229(4) . ?
O4 C14 1.239(4) . ?
O5 H51 0.87(3) . ?
O5 H52 0.85(3) . ?
N1 C13 1.483(5) . ?
N1 C12 1.484(5) . ?
N1 C1 1.494(5) . ?
N2 C3 1.470(5) . ?
N2 C2 1.485(5) . ?
N2 H2N 0.94(4) . ?
N3 C10 1.483(5) . ?
N3 C11 1.485(5) . ?
N3 H3N 0.83(4) . ?
C1 C2 1.510(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.522(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C9 1.389(5) . ?
C4 C5 1.394(5) . ?
C5 C6 1.391(5) . ?
C5 H5A 0.9500 . ?
C6 C7 1.398(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.399(5) . ?
C7 C10 1.513(5) 2_575 ?
C8 C9 1.385(5) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C7 1.513(5) 2_575 ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.515(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.566(5) . ?
Ni2 O6 2.055(2) . ?
Ni2 O7 2.067(2) . ?
Ni2 O10 2.097(3) . ?
Ni2 N6 2.116(3) . ?
Ni2 N4 2.132(3) . ?
Ni2 N5 2.142(3) . ?
O6 C29 1.265(4) . ?
O7 C30 1.267(5) . ?
O8 C30 1.236(4) . ?
O9 C29 1.238(4) . ?
O10 H101 0.86(3) . ?
O10 H102 0.85(3) . ?
N4 C16 1.474(4) . ?
N4 C27 1.479(4) . ?
N4 C28 1.480(4) . ?
N5 C17 1.477(4) . ?
N5 C18 1.491(4) . ?
N5 H5N 0.83(4) . ?
N6 C25 1.477(5) . ?
N6 C26 1.485(4) . ?
N6 H6N 0.84(4) . ?
C16 C17 1.514(5) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.510(5) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C24 1.392(5) . ?
C19 C20 1.395(5) . ?
C20 C21 1.389(5) . ?
C20 H20 0.9500 . ?
C21 C22 1.401(5) . ?
C21 H21 0.9500 . ?
C22 C23 1.388(5) . ?
C22 C25 1.516(5) 2_665 ?
C23 C24 1.391(5) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C22 1.516(5) 2_665 ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.519(5) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.565(5) . ?
O11 H111 0.877(17) . ?
O11 H112 0.882(17) . ?
O12 H121 0.871(16) . ?
O12 H122 0.874(16) . ?
O13 H131 0.883(17) . ?
O13 H132 0.875(17) . ?
O14 O14A 1.50(2) . ?
O14 H141 0.869(17) . ?
O14 H142 0.862(17) . ?
O15 H151 0.867(17) . ?
O15 H152 0.874(17) . ?
O16 H161 0.876(18) . ?
O16 H162 0.877(18) . ?
O17 H171 0.875(18) . ?
O17 H172 0.869(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ni1 O1 80.67(10) . . ?
O2 Ni1 O5 87.58(10) . . ?
O1 Ni1 O5 88.09(10) . . ?
O2 Ni1 N1 175.16(11) . . ?
O1 Ni1 N1 97.01(11) . . ?
O5 Ni1 N1 96.61(11) . . ?
O2 Ni1 N3 92.58(11) . . ?
O1 Ni1 N3 86.01(11) . . ?
O5 Ni1 N3 174.00(11) . . ?
N1 Ni1 N3 83.00(12) . . ?
O2 Ni1 N2 99.63(11) . . ?
O1 Ni1 N2 172.48(11) . . ?
O5 Ni1 N2 84.42(11) . . ?
N1 Ni1 N2 83.23(11) . . ?
N3 Ni1 N2 101.46(12) . . ?
C14 O1 Ni1 113.4(2) . . ?
C15 O2 Ni1 114.7(2) . . ?
Ni1 O5 H51 118(3) . . ?
Ni1 O5 H52 126(3) . . ?
H51 O5 H52 112(4) . . ?
C13 N1 C12 110.4(3) . . ?
C13 N1 C1 110.2(3) . . ?
C12 N1 C1 110.3(3) . . ?
C13 N1 Ni1 111.8(2) . . ?
C12 N1 Ni1 105.9(2) . . ?
C1 N1 Ni1 108.3(2) . . ?
C3 N2 C2 114.3(3) . . ?
C3 N2 Ni1 112.5(2) . . ?
C2 N2 Ni1 102.9(2) . . ?
C3 N2 H2N 109(2) . . ?
C2 N2 H2N 111(2) . . ?
Ni1 N2 H2N 107(2) . . ?
C10 N3 C11 113.2(3) . . ?
C10 N3 Ni1 123.0(2) . . ?
C11 N3 Ni1 108.4(2) . . ?
C10 N3 H3N 103(3) . . ?
C11 N3 H3N 103(3) . . ?
Ni1 N3 H3N 103(3) . . ?
N1 C1 C2 110.2(3) . . ?
N1 C1 H1A 109.6 . . ?
C2 C1 H1A 109.6 . . ?
N1 C1 H1B 109.6 . . ?
C2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
N2 C2 C1 109.0(3) . . ?
N2 C2 H2A 109.9 . . ?
C1 C2 H2A 109.9 . . ?
N2 C2 H2B 109.9 . . ?
C1 C2 H2B 109.9 . . ?
H2A C2 H2B 108.3 . . ?
N2 C3 C4 118.8(3) . . ?
N2 C3 H3A 107.6 . . ?
C4 C3 H3A 107.6 . . ?
N2 C3 H3B 107.6 . . ?
C4 C3 H3B 107.6 . . ?
H3A C3 H3B 107.0 . . ?
C9 C4 C5 117.7(3) . . ?
C9 C4 C3 116.9(3) . . ?
C5 C4 C3 125.4(3) . . ?
C6 C5 C4 121.0(3) . . ?
C6 C5 H5A 119.5 . . ?
C4 C5 H5A 119.5 . . ?
C5 C6 C7 121.2(3) . . ?
C5 C6 H6 119.4 . . ?
C7 C6 H6 119.4 . . ?
C6 C7 C8 117.6(3) . . ?
C6 C7 C10 120.2(3) . 2_575 ?
C8 C7 C10 122.2(3) . 2_575 ?
C9 C8 C7 120.9(3) . . ?
C9 C8 H8 119.6 . . ?
C7 C8 H8 119.6 . . ?
C8 C9 C4 121.7(3) . . ?
C8 C9 H9 119.2 . . ?
C4 C9 H9 119.2 . . ?
N3 C10 C7 113.8(3) . 2_575 ?
N3 C10 H10A 108.8 . . ?
C7 C10 H10A 108.8 2_575 . ?
N3 C10 H10B 108.8 . . ?
C7 C10 H10B 108.8 2_575 . ?
H10A C10 H10B 107.7 . . ?
N3 C11 C12 107.8(3) . . ?
N3 C11 H11A 110.2 . . ?
C12 C11 H11A 110.2 . . ?
N3 C11 H11B 110.2 . . ?
C12 C11 H11B 110.2 . . ?
H11A C11 H11B 108.5 . . ?
N1 C12 C11 110.6(3) . . ?
N1 C12 H12A 109.5 . . ?
C11 C12 H12A 109.5 . . ?
N1 C12 H12B 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
N1 C13 H13A 109.5 . . ?
N1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O4 C14 O1 125.7(3) . . ?
O4 C14 C15 118.5(3) . . ?
O1 C14 C15 115.8(3) . . ?
O3 C15 O2 124.8(3) . . ?
O3 C15 C14 119.8(3) . . ?
O2 C15 C14 115.4(3) . . ?
O6 Ni2 O7 81.51(9) . . ?
O6 Ni2 O10 89.25(10) . . ?
O7 Ni2 O10 89.84(10) . . ?
O6 Ni2 N6 87.64(10) . . ?
O7 Ni2 N6 167.66(11) . . ?
O10 Ni2 N6 95.92(10) . . ?
O6 Ni2 N4 95.46(10) . . ?
O7 Ni2 N4 92.23(11) . . ?
O10 Ni2 N4 175.09(11) . . ?
N6 Ni2 N4 82.91(11) . . ?
O6 Ni2 N5 168.14(10) . . ?
O7 Ni2 N5 86.72(11) . . ?
O10 Ni2 N5 92.20(11) . . ?
N6 Ni2 N5 103.90(12) . . ?
N4 Ni2 N5 83.48(11) . . ?
C29 O6 Ni2 112.3(2) . . ?
C30 O7 Ni2 111.3(2) . . ?
Ni2 O10 H101 115(3) . . ?
Ni2 O10 H102 103(3) . . ?
H101 O10 H102 102(4) . . ?
C16 N4 C27 111.4(3) . . ?
C16 N4 C28 109.2(3) . . ?
C27 N4 C28 109.3(3) . . ?
C16 N4 Ni2 105.2(2) . . ?
C27 N4 Ni2 107.8(2) . . ?
C28 N4 Ni2 113.9(2) . . ?
C17 N5 C18 111.6(3) . . ?
C17 N5 Ni2 107.7(2) . . ?
C18 N5 Ni2 126.1(2) . . ?
C17 N5 H5N 100(3) . . ?
C18 N5 H5N 107(3) . . ?
Ni2 N5 H5N 101(3) . . ?
C25 N6 C26 112.9(3) . . ?
C25 N6 Ni2 115.0(2) . . ?
C26 N6 Ni2 104.0(2) . . ?
C25 N6 H6N 108(3) . . ?
C26 N6 H6N 112(3) . . ?
Ni2 N6 H6N 105(3) . . ?
N4 C16 C17 111.9(3) . . ?
N4 C16 H16A 109.2 . . ?
C17 C16 H16A 109.2 . . ?
N4 C16 H16B 109.2 . . ?
C17 C16 H16B 109.2 . . ?
H16A C16 H16B 107.9 . . ?
N5 C17 C16 109.1(3) . . ?
N5 C17 H17A 109.9 . . ?
C16 C17 H17A 109.9 . . ?
N5 C17 H17B 109.9 . . ?
C16 C17 H17B 109.9 . . ?
H17A C17 H17B 108.3 . . ?
N5 C18 C19 113.2(3) . . ?
N5 C18 H18A 108.9 . . ?
C19 C18 H18A 108.9 . . ?
N5 C18 H18B 108.9 . . ?
C19 C18 H18B 108.9 . . ?
H18A C18 H18B 107.8 . . ?
C24 C19 C20 118.0(3) . . ?
C24 C19 C18 120.0(3) . . ?
C20 C19 C18 122.0(3) . . ?
C21 C20 C19 120.8(3) . . ?
C21 C20 H20 119.6 . . ?
C19 C20 H20 119.6 . . ?
C20 C21 C22 121.2(3) . . ?
C20 C21 H21 119.4 . . ?
C22 C21 H21 119.4 . . ?
C23 C22 C21 117.8(3) . . ?
C23 C22 C25 123.7(3) . 2_665 ?
C21 C22 C25 118.5(3) . 2_665 ?
C22 C23 C24 121.1(3) . . ?
C22 C23 H23 119.5 . . ?
C24 C23 H23 119.5 . . ?
C23 C24 C19 121.2(3) . . ?
C23 C24 H24 119.4 . . ?
C19 C24 H24 119.4 . . ?
N6 C25 C22 115.6(3) . 2_665 ?
N6 C25 H25A 108.4 . . ?
C22 C25 H25A 108.4 2_665 . ?
N6 C25 H25B 108.4 . . ?
C22 C25 H25B 108.4 2_665 . ?
H25A C25 H25B 107.4 . . ?
N6 C26 C27 107.7(3) . . ?
N6 C26 H26A 110.2 . . ?
C27 C26 H26A 110.2 . . ?
N6 C26 H26B 110.2 . . ?
C27 C26 H26B 110.2 . . ?
H26A C26 H26B 108.5 . . ?
N4 C27 C26 109.5(3) . . ?
N4 C27 H27A 109.8 . . ?
C26 C27 H27A 109.8 . . ?
N4 C27 H27B 109.8 . . ?
C26 C27 H27B 109.8 . . ?
H27A C27 H27B 108.2 . . ?
N4 C28 H28A 109.5 . . ?
N4 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
N4 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O9 C29 O6 126.3(3) . . ?
O9 C29 C30 118.0(3) . . ?
O6 C29 C30 115.6(3) . . ?
O8 C30 O7 125.7(3) . . ?
O8 C30 C29 119.2(3) . . ?
O7 C30 C29 115.1(3) . . ?
H111 O11 H112 104(3) . . ?
H121 O12 H122 106(3) . . ?
H131 O13 H132 105(3) . . ?
H141 O14 H142 109(3) . . ?
H151 O15 H152 107(3) . . ?
H161 O16 H162 104(3) . . ?
H171 O17 H172 106(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Ni1 O1 C14 -3.0(2) . . . . ?
O5 Ni1 O1 C14 -90.9(2) . . . . ?
N1 Ni1 O1 C14 172.7(2) . . . . ?
N3 Ni1 O1 C14 90.2(2) . . . . ?
O1 Ni1 O2 C15 3.4(2) . . . . ?
O5 Ni1 O2 C15 91.8(2) . . . . ?
N3 Ni1 O2 C15 -82.2(2) . . . . ?
N2 Ni1 O2 C15 175.8(2) . . . . ?
O1 Ni1 N1 C13 53.0(2) . . . . ?
O5 Ni1 N1 C13 -35.9(2) . . . . ?
N3 Ni1 N1 C13 138.0(2) . . . . ?
N2 Ni1 N1 C13 -119.5(2) . . . . ?
O1 Ni1 N1 C12 -67.3(2) . . . . ?
O5 Ni1 N1 C12 -156.2(2) . . . . ?
N3 Ni1 N1 C12 17.8(2) . . . . ?
N2 Ni1 N1 C12 120.3(2) . . . . ?
O1 Ni1 N1 C1 174.5(2) . . . . ?
O5 Ni1 N1 C1 85.6(2) . . . . ?
N3 Ni1 N1 C1 -100.4(2) . . . . ?
N2 Ni1 N1 C1 2.0(2) . . . . ?
O2 Ni1 N2 C3 -34.4(2) . . . . ?
O5 Ni1 N2 C3 52.2(2) . . . . ?
N1 Ni1 N2 C3 149.5(2) . . . . ?
N3 Ni1 N2 C3 -129.1(2) . . . . ?
O2 Ni1 N2 C2 -157.9(2) . . . . ?
O5 Ni1 N2 C2 -71.3(2) . . . . ?
N1 Ni1 N2 C2 26.0(2) . . . . ?
N3 Ni1 N2 C2 107.4(2) . . . . ?
O2 Ni1 N3 C10 -35.9(3) . . . . ?
O1 Ni1 N3 C10 -116.3(3) . . . . ?
N1 Ni1 N3 C10 146.1(3) . . . . ?
N2 Ni1 N3 C10 64.5(3) . . . . ?
O2 Ni1 N3 C11 -171.1(2) . . . . ?
O1 Ni1 N3 C11 108.4(2) . . . . ?
N1 Ni1 N3 C11 10.9(2) . . . . ?
N2 Ni1 N3 C11 -70.7(2) . . . . ?
C13 N1 C1 C2 92.1(3) . . . . ?
C12 N1 C1 C2 -145.8(3) . . . . ?
Ni1 N1 C1 C2 -30.4(3) . . . . ?
C3 N2 C2 C1 -172.6(3) . . . . ?
Ni1 N2 C2 C1 -50.2(3) . . . . ?
N1 C1 C2 N2 56.3(4) . . . . ?
C2 N2 C3 C4 -68.7(4) . . . . ?
Ni1 N2 C3 C4 174.4(2) . . . . ?
N2 C3 C4 C9 178.1(3) . . . . ?
N2 C3 C4 C5 -3.3(5) . . . . ?
C9 C4 C5 C6 0.0(5) . . . . ?
C3 C4 C5 C6 -178.5(3) . . . . ?
C4 C5 C6 C7 1.0(5) . . . . ?
C5 C6 C7 C8 -1.5(5) . . . . ?
C5 C6 C7 C10 177.8(3) . . . 2_575 ?
C6 C7 C8 C9 1.2(5) . . . . ?
C10 C7 C8 C9 -178.0(3) 2_575 . . . ?
C7 C8 C9 C4 -0.3(5) . . . . ?
C5 C4 C9 C8 -0.3(5) . . . . ?
C3 C4 C9 C8 178.4(3) . . . . ?
C11 N3 C10 C7 76.4(4) . . . 2_575 ?
Ni1 N3 C10 C7 -56.9(4) . . . 2_575 ?
C10 N3 C11 C12 -177.0(3) . . . . ?
Ni1 N3 C11 C12 -37.0(3) . . . . ?
C13 N1 C12 C11 -165.5(3) . . . . ?
C1 N1 C12 C11 72.5(4) . . . . ?
Ni1 N1 C12 C11 -44.4(3) . . . . ?
N3 C11 C12 N1 55.8(4) . . . . ?
Ni1 O1 C14 O4 -177.9(3) . . . . ?
Ni1 O1 C14 C15 2.3(4) . . . . ?
Ni1 O2 C15 O3 178.1(3) . . . . ?
Ni1 O2 C15 C14 -3.1(4) . . . . ?
O4 C14 C15 O3 -0.5(5) . . . . ?
O1 C14 C15 O3 179.3(3) . . . . ?
O4 C14 C15 O2 -179.3(3) . . . . ?
O1 C14 C15 O2 0.5(4) . . . . ?
O7 Ni2 O6 C29 -2.4(2) . . . . ?
O10 Ni2 O6 C29 -92.3(2) . . . . ?
N6 Ni2 O6 C29 171.7(2) . . . . ?
N4 Ni2 O6 C29 89.1(2) . . . . ?
N5 Ni2 O6 C29 4.8(6) . . . . ?
O6 Ni2 O7 C30 -11.0(2) . . . . ?
O10 Ni2 O7 C30 78.2(2) . . . . ?
N6 Ni2 O7 C30 -39.8(6) . . . . ?
N4 Ni2 O7 C30 -106.2(2) . . . . ?
N5 Ni2 O7 C30 170.4(2) . . . . ?
O6 Ni2 N4 C16 -151.25(19) . . . . ?
O7 Ni2 N4 C16 -69.6(2) . . . . ?
N6 Ni2 N4 C16 121.8(2) . . . . ?
N5 Ni2 N4 C16 16.9(2) . . . . ?
O6 Ni2 N4 C27 89.7(2) . . . . ?
O7 Ni2 N4 C27 171.4(2) . . . . ?
N6 Ni2 N4 C27 2.8(2) . . . . ?
N5 Ni2 N4 C27 -102.1(2) . . . . ?
O6 Ni2 N4 C28 -31.7(2) . . . . ?
O7 Ni2 N4 C28 50.0(2) . . . . ?
N6 Ni2 N4 C28 -118.7(2) . . . . ?
N5 Ni2 N4 C28 136.4(2) . . . . ?
O6 Ni2 N5 C17 96.2(5) . . . . ?
O7 Ni2 N5 C17 103.3(2) . . . . ?
O10 Ni2 N5 C17 -167.0(2) . . . . ?
N6 Ni2 N5 C17 -70.4(2) . . . . ?
N4 Ni2 N5 C17 10.6(2) . . . . ?
O6 Ni2 N5 C18 -128.4(5) . . . . ?
O7 Ni2 N5 C18 -121.3(3) . . . . ?
O10 Ni2 N5 C18 -31.6(3) . . . . ?
N6 Ni2 N5 C18 65.1(3) . . . . ?
N4 Ni2 N5 C18 146.1(3) . . . . ?
O6 Ni2 N6 C25 54.9(2) . . . . ?
O7 Ni2 N6 C25 83.3(6) . . . . ?
O10 Ni2 N6 C25 -34.1(2) . . . . ?
N4 Ni2 N6 C25 150.7(2) . . . . ?
N5 Ni2 N6 C25 -127.8(2) . . . . ?
O6 Ni2 N6 C26 -69.1(2) . . . . ?
O7 Ni2 N6 C26 -40.7(6) . . . . ?
O10 Ni2 N6 C26 -158.1(2) . . . . ?
N4 Ni2 N6 C26 26.7(2) . . . . ?
N5 Ni2 N6 C26 108.1(2) . . . . ?
C27 N4 C16 C17 74.0(3) . . . . ?
C28 N4 C16 C17 -165.2(3) . . . . ?
Ni2 N4 C16 C17 -42.6(3) . . . . ?
C18 N5 C17 C16 -178.3(3) . . . . ?
Ni2 N5 C17 C16 -35.9(3) . . . . ?
N4 C16 C17 N5 54.7(4) . . . . ?
C17 N5 C18 C19 72.0(4) . . . . ?
Ni2 N5 C18 C19 -62.1(4) . . . . ?
N5 C18 C19 C24 84.7(4) . . . . ?
N5 C18 C19 C20 -96.9(4) . . . . ?
C24 C19 C20 C21 -2.3(5) . . . . ?
C18 C19 C20 C21 179.2(3) . . . . ?
C19 C20 C21 C22 -0.2(5) . . . . ?
C20 C21 C22 C23 2.5(5) . . . . ?
C20 C21 C22 C25 -174.6(3) . . . 2_665 ?
C21 C22 C23 C24 -2.2(5) . . . . ?
C25 C22 C23 C24 174.8(3) 2_665 . . . ?
C22 C23 C24 C19 -0.4(5) . . . . ?
C20 C19 C24 C23 2.7(5) . . . . ?
C18 C19 C24 C23 -178.9(3) . . . . ?
C26 N6 C25 C22 -68.7(4) . . . 2_665 ?
Ni2 N6 C25 C22 172.1(2) . . . 2_665 ?
C25 N6 C26 C27 -177.0(3) . . . . ?
Ni2 N6 C26 C27 -51.6(3) . . . . ?
C16 N4 C27 C26 -147.0(3) . . . . ?
C28 N4 C27 C26 92.3(3) . . . . ?
Ni2 N4 C27 C26 -32.0(3) . . . . ?
N6 C26 C27 N4 57.7(4) . . . . ?
Ni2 O6 C29 O9 -165.1(3) . . . . ?
Ni2 O6 C29 C30 13.2(4) . . . . ?
Ni2 O7 C30 O8 -160.7(3) . . . . ?
Ni2 O7 C30 C29 20.4(4) . . . . ?
O9 C29 C30 O8 -24.4(5) . . . . ?
O6 C29 C30 O8 157.1(3) . . . . ?
O9 C29 C30 O7 154.6(3) . . . . ?
O6 C29 C30 O7 -23.9(5) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H51 O11 0.87(3) 1.91(3) 2.778(4) 173(5) .
O5 H52 O12 0.85(3) 1.92(3) 2.713(4) 155(4) .
N3 H3N O9 0.83(4) 2.27(4) 3.018(4) 150(4) .
O10 H101 O4 0.86(3) 1.93(3) 2.776(4) 166(4) .
O10 H102 O14 0.85(3) 1.84(3) 2.687(4) 172(4) .
N5 H5N O8 0.83(4) 2.24(4) 2.986(4) 150(4) 2_666
O11 H111 O15 0.877(17) 1.92(2) 2.747(4) 157(4) .
O11 H112 O16 0.882(17) 1.99(2) 2.828(5) 159(4) .
O12 H121 O1 0.871(16) 1.919(16) 2.790(3) 178(4) 2_676
O12 H122 O8 0.874(16) 1.939(19) 2.807(4) 172(4) 2_676
O13 H131 O14 0.883(17) 1.840(18) 2.722(5) 176(5) .
O13 H132 O4 0.875(17) 1.99(3) 2.825(4) 159(4) .
O14 H141 O17 0.869(17) 1.75(2) 2.614(5) 170(6) 1_655
O14 H142 O7 0.862(17) 2.08(3) 2.912(4) 162(5) 2_666
O15 H151 O13 0.867(17) 1.937(19) 2.779(4) 163(5) 2_776
O15 H152 O12 0.874(17) 2.06(2) 2.903(4) 162(5) .
O16 H161 O2 0.876(18) 2.17(5) 2.957(5) 149(8) .
O17 H171 O9 0.875(18) 1.92(4) 2.764(5) 161(10) .
O17 H172 O8 0.869(18) 2.63(11) 3.044(5) 111(9) .

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        63.77
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.074

# END OF CIF
_database_code_depnum_ccdc_archive 'CCDC 970399'