Supplementary Material (ESI) for Dalton Transactions
This journal is © The Royal Society of Chemistry 2005

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Prof Henry Kozlowski'
_publ_contact_author_address     
;
Faculty of Chemistry
University of Wroclaw
F Joliot-Curie 14
Wroclaw
50-383
;

_publ_contact_author_email       HENRYKOZ@WCHUWR.CHEM.UNI.WROC.PL

_publ_section_title              
;
Effect of Metal Ionic Radius and Chelate Rings
Alternation Motif on Stabilization of Trivalent Nickel and Copper in
Binuclear Complexes with Double cis-Oximato Bridges
;
loop_
_publ_author_name
'Henry Kozlowski'
'Agnieszka Dobosz'
'Igor O. Fritsky'
'Olga Kanderal'
'Jolanta Kozlowska'
;
F.Meyer
;

data_7
_database_code_depnum_ccdc_archive 'CCDC 263427'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
(tris(2-aminoethyl)amine)-cobalt(III)(N,N'-bis(2-Hydroxyiminopropionyl)
propane-1,3-diamine)-copper(II) nitrate lithium nitrate pentahydrate methanol
solvate
;
_chemical_name_common            
;
(tris(2-aminoethyl)amine)-cobalt(iii)(N,N'-bis(2-
Hydroxyiminopropionyl) propane-1,3-diamine)-copper(ii) nitrate lithium
nitrate pentahydrate methanol solvate
;
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H42.50 Co Cu Li0.25 N9.25 O14'
_chemical_formula_weight         700.79

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   I4(1)/a

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   19.8716(8)
_cell_length_b                   19.8716(8)
_cell_length_c                   29.6313(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     11700.8(9)
_cell_formula_units_Z            16
_cell_measurement_temperature    190(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5856
_exptl_absorpt_coefficient_mu    1.371
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      190(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       omega-scan
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8943
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_theta_min         2.00
_diffrn_reflns_theta_max         30.51
_reflns_number_total             8943
_reflns_number_gt                6777
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
;
Refinement of 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^)+(0.0448P)^2^+38.1678P] 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         8943
_refine_ls_number_parameters     562
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0454
_refine_ls_wR_factor_ref         0.1268
_refine_ls_wR_factor_gt          0.1118
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_restrained_S_all      1.130
_refine_ls_shift/su_max          0.008
_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
Cu1 Cu 0.522905(16) 0.351959(17) 0.067415(11) 0.02322(9) Uani 1 1 d . . .
Co1 Co 0.649415(17) 0.386222(17) -0.021302(12) 0.01917(8) Uani 1 1 d . . .
N1 N 0.51554(11) 0.34357(11) 0.00063(8) 0.0224(4) Uani 1 1 d . . .
N2 N 0.42689(12) 0.34017(13) 0.06458(9) 0.0290(5) Uani 1 1 d . . .
N3 N 0.52998(13) 0.34519(12) 0.13240(8) 0.0277(5) Uani 1 1 d . . .
N4 N 0.62187(11) 0.35476(11) 0.07171(7) 0.0214(4) Uani 1 1 d . . .
N5 N 0.73689(11) 0.43123(11) -0.02095(8) 0.0237(4) Uani 1 1 d . . .
N6 N 0.61169(12) 0.47207(12) -0.00162(9) 0.0244(5) Uani 1 1 d . . .
N7 N 0.64386(12) 0.41092(13) -0.08505(8) 0.0243(4) Uani 1 1 d . . .
N8 N 0.69825(11) 0.30388(12) -0.03524(9) 0.0226(4) Uani 1 1 d . . .
N9 N 0.52483(12) 0.51653(11) 0.09706(8) 0.0238(4) Uani 1 1 d . . .
O1 O 0.56515(9) 0.34299(10) -0.03062(7) 0.0250(4) Uani 1 1 d . . .
O2 O 0.34318(10) 0.31320(10) 0.01376(8) 0.0326(5) Uani 1 1 d . . .
O3 O 0.60896(12) 0.32004(11) 0.18706(7) 0.0353(5) Uani 1 1 d . . .
O4 O 0.66808(9) 0.36077(10) 0.03917(6) 0.0249(4) Uani 1 1 d . . .
O5 O 0.58697(10) 0.51376(11) 0.10266(7) 0.0314(4) Uani 1 1 d . . .
O6 O 0.49824(10) 0.48481(10) 0.06486(7) 0.0283(4) Uani 1 1 d . . .
O7 O 0.48894(11) 0.54969(11) 0.12353(7) 0.0324(5) Uani 1 1 d . . .
C1 C 0.43604(15) 0.31749(15) -0.06099(11) 0.0282(6) Uani 1 1 d . . .
C2 C 0.45519(13) 0.32974(13) -0.01306(10) 0.0239(5) Uani 1 1 d . . .
C3 C 0.40329(13) 0.32674(13) 0.02414(11) 0.0267(6) Uani 1 1 d . . .
C4 C 0.38101(16) 0.34113(16) 0.10282(12) 0.0327(6) Uani 1 1 d . . .
C5 C 0.47283(17) 0.34080(16) 0.16314(11) 0.0327(6) Uani 1 1 d . . .
C6 C 0.59150(15) 0.33472(14) 0.14745(10) 0.0270(5) Uani 1 1 d . . .
C7 C 0.64480(14) 0.34219(13) 0.11180(9) 0.0245(5) Uani 1 1 d . . .
C8 C 0.71779(17) 0.33500(17) 0.12163(11) 0.0322(6) Uani 1 1 d . . .
C9 C 0.41144(17) 0.37578(15) 0.14374(12) 0.0343(7) Uani 1 1 d . . .
C10 C 0.66553(16) 0.52345(15) 0.00543(11) 0.0305(6) Uani 1 1 d . . .
C11 C 0.73183(15) 0.48698(15) 0.01281(11) 0.0301(6) Uani 1 1 d . . .
C12 C 0.68900(16) 0.46814(16) -0.09455(10) 0.0298(6) Uani 1 1 d . . .
C13 C 0.75262(15) 0.45732(16) -0.06744(10) 0.0285(6) Uani 1 1 d . . .
C14 C 0.77250(14) 0.31490(15) -0.03252(11) 0.0289(6) Uani 1 1 d . . .
C15 C 0.78757(14) 0.37964(15) -0.00694(10) 0.0276(6) Uani 1 1 d . . .
O1W O 0.2256(2) 0.3610(3) 0.0533(2) 0.133(2) Uani 1 1 d . . .
O2W O 0.5594(4) 0.2964(7) 0.2703(3) 0.090(4) Uani 0.50 1 d P . .
O2WA O 0.5288(4) 0.3058(5) 0.2647(2) 0.062(2) Uani 0.50 1 d P . .
O3W O 0.6930(6) 0.2335(5) 0.2296(3) 0.083(4) Uani 0.50 1 d P . .
O3WA O 0.7093(5) 0.2135(4) 0.2107(3) 0.055(2) Uani 0.50 1 d P . .
O4W O 0.4246(14) 0.3418(7) 0.4059(5) 0.268(13) Uani 0.50 1 d P . .
O4WA O 0.3696(5) 0.2768(5) 0.3362(4) 0.105(3) Uani 0.50 1 d P . .
O5W O 0.3977(10) 0.3078(9) 0.3656(8) 0.100(6) Uani 0.25 1 d P . .
O5WA O 0.5193(11) 0.3859(9) 0.3257(7) 0.110(7) Uani 0.25 1 d P . .
O6W O 0.3289(6) 0.3773(5) 0.2745(3) 0.114(3) Uani 0.50 1 d P . .
O6WA O 0.3995(4) 0.3500(3) 0.2716(2) 0.0623(16) Uani 0.50 1 d P . .
O7WN O 0.3803(3) 0.4665(3) 0.40415(19) 0.1181(18) Uani 1 1 d . . .
O22 O 0.3230(6) 0.4738(8) 0.3882(5) 0.073(4) Uani 0.25 1 d P . .
O23 O 0.4270(6) 0.4641(7) 0.3828(4) 0.059(3) Uani 0.25 1 d P . .
O24 O 0.3892(6) 0.4828(7) 0.4480(4) 0.058(3) Uani 0.25 1 d P . .
Li1 Li 0.4835(18) 0.2736(16) 0.3586(10) 0.064(8) Uani 0.25 1 d P . .
H1A H 0.4679(18) 0.3411(18) -0.0797(12) 0.032(9) Uiso 1 1 d . . .
H1B H 0.437(2) 0.273(2) -0.0662(14) 0.051(12) Uiso 1 1 d . . .
H1C H 0.390(2) 0.332(2) -0.0665(13) 0.042(10) Uiso 1 1 d . . .
H4A H 0.3690(16) 0.2938(17) 0.1106(11) 0.023(8) Uiso 1 1 d . . .
H4B H 0.341(2) 0.368(2) 0.0941(13) 0.042(10) Uiso 1 1 d . . .
H5A H 0.4829(18) 0.3592(18) 0.1910(12) 0.032(9) Uiso 1 1 d . . .
H5B H 0.4677(17) 0.2909(18) 0.1710(12) 0.031(9) Uiso 1 1 d . . .
H8A H 0.7403(18) 0.3722(19) 0.1132(12) 0.030(9) Uiso 1 1 d . . .
H8B H 0.717(2) 0.332(2) 0.1520(17) 0.065(14) Uiso 1 1 d . . .
H8C H 0.733(2) 0.301(2) 0.1029(14) 0.045(11) Uiso 1 1 d . . .
H9A H 0.3789(17) 0.3796(16) 0.1671(11) 0.024(8) Uiso 1 1 d . . .
H9B H 0.4216(19) 0.421(2) 0.1344(13) 0.039(10) Uiso 1 1 d . . .
H10A H 0.6712(16) 0.5512(17) -0.0225(11) 0.024(8) Uiso 1 1 d . . .
H10B H 0.656(2) 0.552(2) 0.0284(14) 0.044(11) Uiso 1 1 d . . .
H11A H 0.769(2) 0.515(2) 0.0100(13) 0.041(10) Uiso 1 1 d . . .
H11B H 0.7308(17) 0.4682(17) 0.0417(12) 0.026(8) Uiso 1 1 d . . .
H12A H 0.6976(17) 0.4704(17) -0.1266(12) 0.026(8) Uiso 1 1 d . . .
H12B H 0.6674(16) 0.5049(17) -0.0888(11) 0.019(7) Uiso 1 1 d . . .
H13A H 0.7805(18) 0.4257(18) -0.0800(12) 0.030(9) Uiso 1 1 d . . .
H13B H 0.7741(19) 0.4953(19) -0.0645(12) 0.035(10) Uiso 1 1 d . . .
H14A H 0.7958(18) 0.2767(18) -0.0206(12) 0.031(9) Uiso 1 1 d . . .
H14B H 0.7893(16) 0.3174(16) -0.0618(11) 0.022(8) Uiso 1 1 d . . .
H15A H 0.7799(15) 0.3703(15) 0.0283(10) 0.018(7) Uiso 1 1 d . . .
H15B H 0.8351(18) 0.3980(17) -0.0146(11) 0.030(9) Uiso 1 1 d . . .
H61 H 0.5827(19) 0.4873(18) -0.0197(12) 0.030(9) Uiso 1 1 d . . .
H62 H 0.5931(16) 0.4662(15) 0.0229(11) 0.015(7) Uiso 1 1 d . . .
H71 H 0.6564(17) 0.3781(18) -0.1038(12) 0.027(9) Uiso 1 1 d . . .
H72 H 0.606(2) 0.4203(18) -0.0915(12) 0.032(10) Uiso 1 1 d . . .
H81 H 0.6920(17) 0.2752(18) -0.0159(12) 0.025(9) Uiso 1 1 d . . .
H82 H 0.6917(17) 0.2886(17) -0.0615(12) 0.023(8) Uiso 1 1 d . . .
H1W1 H 0.2644 0.3445 0.0365 0.050 Uiso 1 1 d . . .
H2W1 H 0.2199 0.3155 0.0567 0.050 Uiso 1 1 d . . .
H1W2 H 0.5675 0.3032 0.2421 0.050 Uiso 1 1 d . . .
H2W2 H 0.5377 0.3371 0.2809 0.050 Uiso 1 1 d . . .
H1W3 H 0.6797 0.2568 0.2058 0.050 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
Cu1 0.02058(16) 0.02341(16) 0.02566(17) -0.00138(12) 0.00317(12) -0.00300(12)
Co1 0.01647(16) 0.01925(16) 0.02180(17) -0.00176(12) 0.00123(12) 0.00058(12)
N1 0.0184(10) 0.0202(10) 0.0287(11) -0.0020(8) 0.0026(8) -0.0009(8)
N2 0.0205(11) 0.0308(12) 0.0356(13) -0.0011(10) 0.0064(9) -0.0028(9)
N3 0.0323(12) 0.0245(11) 0.0263(12) -0.0003(9) 0.0068(9) -0.0054(9)
N4 0.0222(10) 0.0193(10) 0.0228(10) -0.0013(8) 0.0022(8) -0.0018(8)
N5 0.0198(10) 0.0229(10) 0.0283(11) -0.0028(9) 0.0030(8) -0.0023(8)
N6 0.0244(11) 0.0218(11) 0.0271(12) -0.0017(9) 0.0031(10) 0.0035(9)
N7 0.0212(11) 0.0281(12) 0.0235(11) -0.0013(9) 0.0010(9) 0.0026(9)
N8 0.0218(10) 0.0209(10) 0.0251(11) -0.0017(9) 0.0022(9) 0.0013(8)
N9 0.0271(11) 0.0206(10) 0.0237(11) -0.0004(8) -0.0023(9) 0.0003(8)
O1 0.0190(9) 0.0289(10) 0.0273(10) -0.0053(8) 0.0025(7) -0.0031(7)
O2 0.0169(9) 0.0265(10) 0.0545(14) -0.0081(9) 0.0010(9) -0.0025(7)
O3 0.0477(13) 0.0330(11) 0.0251(10) 0.0016(8) -0.0016(9) -0.0112(10)
O4 0.0195(9) 0.0311(10) 0.0242(9) 0.0012(8) 0.0018(7) 0.0022(7)
O5 0.0223(9) 0.0356(11) 0.0363(11) -0.0053(9) -0.0049(8) 0.0006(8)
O6 0.0299(10) 0.0289(10) 0.0261(10) -0.0049(8) -0.0069(8) -0.0005(8)
O7 0.0330(11) 0.0361(11) 0.0279(10) -0.0073(9) -0.0007(8) 0.0109(9)
C1 0.0248(13) 0.0248(13) 0.0349(15) 0.0000(11) -0.0053(11) -0.0027(10)
C2 0.0204(11) 0.0175(11) 0.0337(14) -0.0029(10) -0.0010(10) -0.0011(9)
C3 0.0196(12) 0.0156(11) 0.0447(16) -0.0017(11) 0.0032(11) -0.0010(9)
C4 0.0276(14) 0.0265(14) 0.0441(18) 0.0003(12) 0.0124(13) -0.0025(11)
C5 0.0397(17) 0.0264(14) 0.0319(16) -0.0008(12) 0.0120(13) -0.0097(12)
C6 0.0346(14) 0.0204(12) 0.0260(13) -0.0019(10) 0.0014(11) -0.0051(10)
C7 0.0283(13) 0.0189(11) 0.0263(13) -0.0001(10) -0.0016(10) -0.0022(9)
C8 0.0335(15) 0.0346(16) 0.0285(15) 0.0005(12) -0.0063(12) 0.0012(13)
C9 0.0373(16) 0.0242(14) 0.0414(17) -0.0023(12) 0.0189(14) -0.0036(11)
C10 0.0331(15) 0.0218(13) 0.0367(16) -0.0059(12) 0.0042(12) -0.0006(11)
C11 0.0283(14) 0.0281(14) 0.0339(16) -0.0063(12) 0.0017(12) -0.0055(11)
C12 0.0338(15) 0.0279(14) 0.0277(14) 0.0037(11) 0.0043(11) 0.0014(11)
C13 0.0259(13) 0.0281(14) 0.0315(14) 0.0006(11) 0.0063(11) -0.0064(11)
C14 0.0200(12) 0.0305(14) 0.0361(16) -0.0018(12) 0.0035(11) 0.0050(10)
C15 0.0172(12) 0.0336(14) 0.0321(14) -0.0010(11) 0.0008(10) 0.0005(10)
O1W 0.048(2) 0.157(5) 0.195(6) 0.024(4) 0.037(3) 0.033(3)
O2W 0.041(4) 0.188(10) 0.043(4) 0.048(5) 0.010(3) 0.020(5)
O2WA 0.062(5) 0.092(6) 0.032(3) -0.001(3) 0.000(3) -0.020(4)
O3W 0.103(8) 0.056(6) 0.090(8) 0.036(5) -0.064(7) -0.022(5)
O3WA 0.066(4) 0.042(4) 0.056(5) 0.003(3) -0.022(4) -0.003(3)
O4W 0.59(4) 0.117(11) 0.102(10) 0.051(8) -0.066(16) 0.073(17)
O4WA 0.097(7) 0.082(6) 0.136(9) 0.031(6) 0.052(6) 0.024(5)
O5W 0.106(14) 0.063(10) 0.132(17) -0.029(11) -0.034(12) 0.017(9)
O5WA 0.153(19) 0.071(10) 0.106(14) -0.041(10) 0.016(12) 0.024(11)
O6W 0.144(9) 0.088(6) 0.110(8) -0.002(5) -0.023(7) -0.004(6)
O6WA 0.069(4) 0.052(3) 0.065(4) -0.014(3) 0.008(3) -0.006(3)
O7WN 0.132(5) 0.118(4) 0.105(4) 0.014(3) 0.038(4) -0.021(3)
O22 0.039(6) 0.093(10) 0.088(10) 0.039(8) -0.031(6) -0.027(6)
O23 0.035(6) 0.085(9) 0.058(7) 0.026(6) 0.006(5) 0.006(6)
O24 0.059(7) 0.067(8) 0.047(7) 0.001(6) 0.014(5) -0.012(6)
Li1 0.07(2) 0.06(2) 0.056(17) -0.007(13) 0.011(16) -0.018(15)

_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
Cu1 N2 1.924(2) . ?
Cu1 N3 1.935(2) . ?
Cu1 N4 1.971(2) . ?
Cu1 N1 1.991(2) . ?
Cu1 Co1 3.7006(5) . ?
Co1 O4 1.898(2) . ?
Co1 O1 1.9021(19) . ?
Co1 N8 1.947(2) . ?
Co1 N6 1.952(2) . ?
Co1 N7 1.955(2) . ?
Co1 N5 1.955(2) . ?
N1 C2 1.296(3) . ?
N1 O1 1.353(3) . ?
N2 C3 1.314(4) . ?
N2 C4 1.455(4) . ?
N3 C6 1.318(4) . ?
N3 C5 1.458(4) . ?
N4 C7 1.297(3) . ?
N4 O4 1.337(3) . ?
N5 C15 1.496(4) . ?
N5 C11 1.496(4) . ?
N5 C13 1.505(4) . ?
N6 C10 1.494(4) . ?
N6 H61 0.84(4) . ?
N6 H62 0.82(3) . ?
N7 C12 1.476(4) . ?
N7 H71 0.89(4) . ?
N7 H72 0.79(4) . ?
N8 C14 1.494(4) . ?
N8 H81 0.82(4) . ?
N8 H82 0.84(4) . ?
N9 O5 1.247(3) . ?
N9 O7 1.248(3) . ?
N9 O6 1.260(3) . ?
O1 O4 2.930(3) . ?
O2 C3 1.263(3) . ?
O3 C6 1.258(4) . ?
C1 C2 1.490(4) . ?
C1 H1A 0.96(4) . ?
C1 H1B 0.89(4) . ?
C1 H1C 0.97(4) . ?
C2 C3 1.511(4) . ?
C4 C9 1.520(5) . ?
C4 H4A 1.00(3) . ?
C4 H4B 0.99(4) . ?
C5 C9 1.517(5) . ?
C5 H5A 0.93(4) . ?
C5 H5B 1.02(4) . ?
C6 C7 1.503(4) . ?
C7 C8 1.486(4) . ?
C8 H8A 0.90(4) . ?
C8 H8B 0.90(5) . ?
C8 H8C 0.93(4) . ?
C9 H9A 0.95(3) . ?
C9 H9B 0.96(4) . ?
C10 C11 1.519(4) . ?
C10 H10A 1.00(3) . ?
C10 H10B 0.91(4) . ?
C11 H11A 0.93(4) . ?
C11 H11B 0.93(3) . ?
C12 C13 1.513(4) . ?
C12 H12A 0.96(3) . ?
C12 H12B 0.87(3) . ?
C13 H13A 0.92(4) . ?
C13 H13B 0.87(4) . ?
C14 C15 1.523(4) . ?
C14 H14A 0.96(4) . ?
C14 H14B 0.93(3) . ?
C15 H15A 1.07(3) . ?
C15 H15B 1.04(4) . ?
O1W H1W1 0.9742 . ?
O1W H2W1 0.9161 . ?
O2W O2WA 0.658(9) . ?
O2W H1W2 0.8624 . ?
O2W H2W2 0.9694 . ?
O2WA H1W2 1.0213 . ?
O2WA H2W2 0.8050 . ?
O3W O3WA 0.758(12) . ?
O3W H1W3 0.8838 . ?
O3WA H1W3 1.0521 . ?
O4W O5W 1.47(2) . ?
O4W Li1 2.27(4) . ?
O4W Li1 2.43(4) 16_656 ?
O4W Li1 2.51(4) 11_666 ?
O4WA O5W 1.205(19) . ?
O4WA Li1 2.36(4) . ?
O5W Li1 1.85(4) . ?
O5W Li1 2.28(4) 16_656 ?
O5WA Li1 2.54(4) . ?
O6W O6WA 1.508(13) . ?
O7WN O23 1.126(12) . ?
O7WN O22 1.242(12) . ?
O7WN O24 1.351(13) . ?
Li1 Li1 1.14(7) 6_554 ?
Li1 Li1 1.26(6) 11_666 ?
Li1 Li1 1.26(6) 16_656 ?
Li1 O5W 2.28(4) 11_666 ?
Li1 O4W 2.43(4) 11_666 ?
Li1 O4W 2.51(4) 16_656 ?

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 Cu1 N3 96.15(11) . . ?
N2 Cu1 N4 174.50(10) . . ?
N3 Cu1 N4 82.26(10) . . ?
N2 Cu1 N1 82.73(10) . . ?
N3 Cu1 N1 171.21(9) . . ?
N4 Cu1 N1 98.04(9) . . ?
N2 Cu1 Co1 131.68(8) . . ?
N3 Cu1 Co1 132.09(7) . . ?
N4 Cu1 Co1 50.43(7) . . ?
N1 Cu1 Co1 50.16(6) . . ?
O4 Co1 O1 100.88(9) . . ?
O4 Co1 N8 83.05(10) . . ?
O1 Co1 N8 91.63(9) . . ?
O4 Co1 N6 91.48(10) . . ?
O1 Co1 N6 95.74(9) . . ?
N8 Co1 N6 171.55(11) . . ?
O4 Co1 N7 171.89(9) . . ?
O1 Co1 N7 85.60(9) . . ?
N8 Co1 N7 91.96(11) . . ?
N6 Co1 N7 92.73(11) . . ?
O4 Co1 N5 86.74(9) . . ?
O1 Co1 N5 171.96(9) . . ?
N8 Co1 N5 86.70(10) . . ?
N6 Co1 N5 86.56(10) . . ?
N7 Co1 N5 86.59(10) . . ?
O4 Co1 Cu1 54.07(6) . . ?
O1 Co1 Cu1 54.69(6) . . ?
N8 Co1 Cu1 109.55(7) . . ?
N6 Co1 Cu1 71.81(7) . . ?
N7 Co1 Cu1 133.97(7) . . ?
N5 Co1 Cu1 133.19(7) . . ?
C2 N1 O1 117.3(2) . . ?
C2 N1 Cu1 113.39(19) . . ?
O1 N1 Cu1 128.87(17) . . ?
C3 N2 C4 119.3(2) . . ?
C3 N2 Cu1 114.74(19) . . ?
C4 N2 Cu1 125.9(2) . . ?
C6 N3 C5 120.1(3) . . ?
C6 N3 Cu1 114.51(19) . . ?
C5 N3 Cu1 124.7(2) . . ?
C7 N4 O4 115.9(2) . . ?
C7 N4 Cu1 113.84(18) . . ?
O4 N4 Cu1 129.87(17) . . ?
C15 N5 C11 111.5(2) . . ?
C15 N5 C13 110.5(2) . . ?
C11 N5 C13 111.8(2) . . ?
C15 N5 Co1 106.65(17) . . ?
C11 N5 Co1 106.42(17) . . ?
C13 N5 Co1 109.71(17) . . ?
C10 N6 Co1 111.35(18) . . ?
C10 N6 H61 109(2) . . ?
Co1 N6 H61 113(2) . . ?
C10 N6 H62 107(2) . . ?
Co1 N6 H62 108(2) . . ?
H61 N6 H62 108(3) . . ?
C12 N7 Co1 110.09(18) . . ?
C12 N7 H71 106(2) . . ?
Co1 N7 H71 114(2) . . ?
C12 N7 H72 110(3) . . ?
Co1 N7 H72 110(3) . . ?
H71 N7 H72 107(3) . . ?
C14 N8 Co1 110.96(17) . . ?
C14 N8 H81 102(2) . . ?
Co1 N8 H81 111(2) . . ?
C14 N8 H82 105(2) . . ?
Co1 N8 H82 115(2) . . ?
H81 N8 H82 112(3) . . ?
O5 N9 O7 120.4(2) . . ?
O5 N9 O6 119.6(2) . . ?
O7 N9 O6 120.0(2) . . ?
N1 O1 Co1 122.57(15) . . ?
N1 O1 O4 91.40(14) . . ?
Co1 O1 O4 39.51(5) . . ?
N4 O4 Co1 124.78(16) . . ?
N4 O4 O1 91.08(14) . . ?
Co1 O4 O1 39.61(5) . . ?
C2 C1 H1A 108(2) . . ?
C2 C1 H1B 109(3) . . ?
H1A C1 H1B 111(3) . . ?
C2 C1 H1C 111(2) . . ?
H1A C1 H1C 112(3) . . ?
H1B C1 H1C 107(3) . . ?
N1 C2 C1 124.7(3) . . ?
N1 C2 C3 114.3(2) . . ?
C1 C2 C3 121.0(2) . . ?
O2 C3 N2 127.1(3) . . ?
O2 C3 C2 118.5(3) . . ?
N2 C3 C2 114.4(2) . . ?
N2 C4 C9 112.2(2) . . ?
N2 C4 H4A 108.5(19) . . ?
C9 C4 H4A 109.8(19) . . ?
N2 C4 H4B 108(2) . . ?
C9 C4 H4B 107(2) . . ?
H4A C4 H4B 112(3) . . ?
N3 C5 C9 111.2(3) . . ?
N3 C5 H5A 111(2) . . ?
C9 C5 H5A 109(2) . . ?
N3 C5 H5B 106(2) . . ?
C9 C5 H5B 117(2) . . ?
H5A C5 H5B 102(3) . . ?
O3 C6 N3 127.4(3) . . ?
O3 C6 C7 119.0(3) . . ?
N3 C6 C7 113.6(2) . . ?
N4 C7 C8 122.8(3) . . ?
N4 C7 C6 114.5(2) . . ?
C8 C7 C6 122.7(3) . . ?
C7 C8 H8A 111(2) . . ?
C7 C8 H8B 101(3) . . ?
H8A C8 H8B 110(4) . . ?
C7 C8 H8C 106(3) . . ?
H8A C8 H8C 106(3) . . ?
H8B C8 H8C 123(4) . . ?
C5 C9 C4 114.5(3) . . ?
C5 C9 H9A 108(2) . . ?
C4 C9 H9A 110(2) . . ?
C5 C9 H9B 112(2) . . ?
C4 C9 H9B 106(2) . . ?
H9A C9 H9B 106(3) . . ?
N6 C10 C11 108.4(2) . . ?
N6 C10 H10A 109.9(19) . . ?
C11 C10 H10A 106.5(19) . . ?
N6 C10 H10B 113(3) . . ?
C11 C10 H10B 112(3) . . ?
H10A C10 H10B 107(3) . . ?
N5 C11 C10 108.4(2) . . ?
N5 C11 H11A 109(2) . . ?
C10 C11 H11A 113(2) . . ?
N5 C11 H11B 109(2) . . ?
C10 C11 H11B 108(2) . . ?
H11A C11 H11B 110(3) . . ?
N7 C12 C13 107.3(2) . . ?
N7 C12 H12A 109(2) . . ?
C13 C12 H12A 112(2) . . ?
N7 C12 H12B 108(2) . . ?
C13 C12 H12B 116(2) . . ?
H12A C12 H12B 104(3) . . ?
N5 C13 C12 111.2(2) . . ?
N5 C13 H13A 105(2) . . ?
C12 C13 H13A 113(2) . . ?
N5 C13 H13B 108(2) . . ?
C12 C13 H13B 110(2) . . ?
H13A C13 H13B 110(3) . . ?
N8 C14 C15 110.2(2) . . ?
N8 C14 H14A 112(2) . . ?
C15 C14 H14A 113(2) . . ?
N8 C14 H14B 108(2) . . ?
C15 C14 H14B 110(2) . . ?
H14A C14 H14B 102(3) . . ?
N5 C15 C14 108.0(2) . . ?
N5 C15 H15A 107.1(16) . . ?
C14 C15 H15A 108.1(16) . . ?
N5 C15 H15B 108.1(19) . . ?
C14 C15 H15B 111.6(19) . . ?
H15A C15 H15B 114(2) . . ?
H1W1 O1W H2W1 79.8 . . ?
O2WA O2W H1W2 83.3 . . ?
O2WA O2W H2W2 55.4 . . ?
H1W2 O2W H2W2 105.4 . . ?
O2W O2WA H1W2 57.0 . . ?
O2W O2WA H2W2 82.3 . . ?
H1W2 O2WA H2W2 105.4 . . ?
O3WA O3W H1W3 79.3 . . ?
O3W O3WA H1W3 55.6 . . ?
O5W O4W Li1 54.1(13) . . ?
O5W O4W Li1 66.6(12) . 16_656 ?
Li1 O4W Li1 31.0(15) . 16_656 ?
O5W O4W Li1 82.6(13) . 11_666 ?
Li1 O4W Li1 30.1(15) . 11_666 ?
Li1 O4W Li1 26.7(15) 16_656 11_666 ?
O5W O4WA Li1 50.6(13) . . ?
O4WA O5W O4W 172(2) . . ?
O4WA O5W Li1 99.1(16) . . ?
O4W O5W Li1 85.8(17) . . ?
O4WA O5W Li1 103.2(14) . 16_656 ?
O4W O5W Li1 77.1(13) . 16_656 ?
Li1 O5W Li1 33.6(18) . 16_656 ?
O23 O7WN O22 123.2(11) . . ?
O23 O7WN O24 116.3(10) . . ?
O22 O7WN O24 117.4(11) . . ?
Li1 Li1 Li1 63.1(14) 6_554 11_666 ?
Li1 Li1 Li1 63.1(14) 6_554 16_656 ?
Li1 Li1 Li1 54(3) 11_666 16_656 ?
Li1 Li1 O5W 146(4) 6_554 . ?
Li1 Li1 O5W 122(3) 11_666 . ?
Li1 Li1 O5W 92(3) 16_656 . ?
Li1 Li1 O4W 141.6(10) 6_554 . ?
Li1 Li1 O4W 85(3) 11_666 . ?
Li1 Li1 O4W 81(3) 16_656 . ?
O5W Li1 O4W 40.2(10) . . ?
Li1 Li1 O5W 101(4) 6_554 11_666 ?
Li1 Li1 O5W 54(2) 11_666 11_666 ?
Li1 Li1 O5W 104(3) 16_656 11_666 ?
O5W Li1 O5W 107.9(14) . 11_666 ?
O4W Li1 O5W 73.6(12) . 11_666 ?
Li1 Li1 O4WA 125(4) 6_554 . ?
Li1 Li1 O4WA 145(3) 11_666 . ?
Li1 Li1 O4WA 97(3) 16_656 . ?
O5W Li1 O4WA 30.3(8) . . ?
O4W Li1 O4WA 70.3(12) . . ?
O5W Li1 O4WA 134.1(16) 11_666 . ?
Li1 Li1 O4W 81(3) 6_554 11_666 ?
Li1 Li1 O4W 68(2) 11_666 11_666 ?
Li1 Li1 O4W 120(2) 16_656 11_666 ?
O5W Li1 O4W 133.0(18) . 11_666 ?
O4W Li1 O4W 108.2(13) . 11_666 ?
O5W Li1 O4W 36.3(8) 11_666 11_666 ?
O4WA Li1 O4W 142.2(15) . 11_666 ?
Li1 Li1 O4W 73(3) 6_554 16_656 ?
Li1 Li1 O4W 115(2) 11_666 16_656 ?
Li1 Li1 O4W 65(2) 16_656 16_656 ?
O5W Li1 O4W 76.0(14) . 16_656 ?
O4W Li1 O4W 105.4(13) . 16_656 ?
O5W Li1 O4W 168.6(17) 11_666 16_656 ?
O4WA Li1 O4W 53.2(9) . 16_656 ?
O4W Li1 O4W 146.4(15) 11_666 16_656 ?
Li1 Li1 O5WA 124(4) 6_554 . ?
Li1 Li1 O5WA 102(3) 11_666 . ?
Li1 Li1 O5WA 152(3) 16_656 . ?
O5W Li1 O5WA 88.7(15) . . ?
O4W Li1 O5WA 81.7(12) . . ?
O5W Li1 O5WA 49.0(10) 11_666 . ?
O4WA Li1 O5WA 97.9(13) . . ?
O4W Li1 O5WA 46.3(10) 11_666 . ?
O4W Li1 O5WA 142.3(15) 16_656 . ?

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
N2 Cu1 Co1 O4 -168.57(13) . . . . ?
N3 Cu1 Co1 O4 15.71(12) . . . . ?
N4 Cu1 Co1 O4 4.74(11) . . . . ?
N1 Cu1 Co1 O4 -153.03(11) . . . . ?
N2 Cu1 Co1 O1 -25.55(13) . . . . ?
N3 Cu1 Co1 O1 158.73(12) . . . . ?
N4 Cu1 Co1 O1 147.76(11) . . . . ?
N1 Cu1 Co1 O1 -10.01(11) . . . . ?
N2 Cu1 Co1 N8 -103.15(13) . . . . ?
N3 Cu1 Co1 N8 81.12(12) . . . . ?
N4 Cu1 Co1 N8 70.15(11) . . . . ?
N1 Cu1 Co1 N8 -87.61(11) . . . . ?
N2 Cu1 Co1 N6 85.66(13) . . . . ?
N3 Cu1 Co1 N6 -90.07(13) . . . . ?
N4 Cu1 Co1 N6 -101.04(11) . . . . ?
N1 Cu1 Co1 N6 101.20(12) . . . . ?
N2 Cu1 Co1 N7 9.99(15) . . . . ?
N3 Cu1 Co1 N7 -165.74(14) . . . . ?
N4 Cu1 Co1 N7 -176.71(13) . . . . ?
N1 Cu1 Co1 N7 25.53(13) . . . . ?
N2 Cu1 Co1 N5 152.39(14) . . . . ?
N3 Cu1 Co1 N5 -23.34(14) . . . . ?
N4 Cu1 Co1 N5 -34.31(13) . . . . ?
N1 Cu1 Co1 N5 167.93(13) . . . . ?
N2 Cu1 N1 C2 -4.82(19) . . . . ?
N3 Cu1 N1 C2 78.4(7) . . . . ?
N4 Cu1 N1 C2 169.68(19) . . . . ?
Co1 Cu1 N1 C2 -173.2(2) . . . . ?
N2 Cu1 N1 O1 -176.8(2) . . . . ?
N3 Cu1 N1 O1 -93.6(7) . . . . ?
N4 Cu1 N1 O1 -2.3(2) . . . . ?
Co1 Cu1 N1 O1 14.84(16) . . . . ?
N3 Cu1 N2 C3 -165.5(2) . . . . ?
N4 Cu1 N2 C3 -92.7(11) . . . . ?
N1 Cu1 N2 C3 5.7(2) . . . . ?
Co1 Cu1 N2 C3 17.7(3) . . . . ?
N3 Cu1 N2 C4 10.8(3) . . . . ?
N4 Cu1 N2 C4 83.6(11) . . . . ?
N1 Cu1 N2 C4 -178.0(2) . . . . ?
Co1 Cu1 N2 C4 -165.99(19) . . . . ?
N2 Cu1 N3 C6 164.4(2) . . . . ?
N4 Cu1 N3 C6 -10.3(2) . . . . ?
N1 Cu1 N3 C6 82.2(7) . . . . ?
Co1 Cu1 N3 C6 -18.9(2) . . . . ?
N2 Cu1 N3 C5 -6.1(2) . . . . ?
N4 Cu1 N3 C5 179.2(2) . . . . ?
N1 Cu1 N3 C5 -88.2(7) . . . . ?
Co1 Cu1 N3 C5 170.72(18) . . . . ?
N2 Cu1 N4 C7 -64.8(11) . . . . ?
N3 Cu1 N4 C7 8.65(19) . . . . ?
N1 Cu1 N4 C7 -162.48(19) . . . . ?
Co1 Cu1 N4 C7 -179.5(2) . . . . ?
N2 Cu1 N4 O4 107.6(11) . . . . ?
N3 Cu1 N4 O4 -178.9(2) . . . . ?
N1 Cu1 N4 O4 10.0(2) . . . . ?
Co1 Cu1 N4 O4 -7.11(17) . . . . ?
O4 Co1 N5 C15 54.19(18) . . . . ?
O1 Co1 N5 C15 -107.2(7) . . . . ?
N8 Co1 N5 C15 -29.03(18) . . . . ?
N6 Co1 N5 C15 145.87(19) . . . . ?
N7 Co1 N5 C15 -121.19(18) . . . . ?
Cu1 Co1 N5 C15 84.91(18) . . . . ?
O4 Co1 N5 C11 -65.01(19) . . . . ?
O1 Co1 N5 C11 133.6(6) . . . . ?
N8 Co1 N5 C11 -148.2(2) . . . . ?
N6 Co1 N5 C11 26.68(19) . . . . ?
N7 Co1 N5 C11 119.62(19) . . . . ?
Cu1 Co1 N5 C11 -34.3(2) . . . . ?
O4 Co1 N5 C13 173.90(19) . . . . ?
O1 Co1 N5 C13 12.5(7) . . . . ?
N8 Co1 N5 C13 90.68(19) . . . . ?
N6 Co1 N5 C13 -94.42(19) . . . . ?
N7 Co1 N5 C13 -1.48(19) . . . . ?
Cu1 Co1 N5 C13 -155.38(14) . . . . ?
O4 Co1 N6 C10 83.9(2) . . . . ?
O1 Co1 N6 C10 -175.0(2) . . . . ?
N8 Co1 N6 C10 34.4(8) . . . . ?
N7 Co1 N6 C10 -89.2(2) . . . . ?
N5 Co1 N6 C10 -2.8(2) . . . . ?
Cu1 Co1 N6 C10 135.1(2) . . . . ?
O4 Co1 N7 C12 -56.4(8) . . . . ?
O1 Co1 N7 C12 160.4(2) . . . . ?
N8 Co1 N7 C12 -108.2(2) . . . . ?
N6 Co1 N7 C12 64.8(2) . . . . ?
N5 Co1 N7 C12 -21.58(19) . . . . ?
Cu1 Co1 N7 C12 131.95(16) . . . . ?
O4 Co1 N8 C14 -80.0(2) . . . . ?
O1 Co1 N8 C14 179.3(2) . . . . ?
N6 Co1 N8 C14 -30.0(8) . . . . ?
N7 Co1 N8 C14 93.6(2) . . . . ?
N5 Co1 N8 C14 7.1(2) . . . . ?
Cu1 Co1 N8 C14 -127.84(18) . . . . ?
C2 N1 O1 Co1 161.29(19) . . . . ?
Cu1 N1 O1 Co1 -27.0(3) . . . . ?
C2 N1 O1 O4 -172.9(2) . . . . ?
Cu1 N1 O1 O4 -1.2(2) . . . . ?
O4 Co1 O1 N1 43.2(2) . . . . ?
N8 Co1 O1 N1 126.4(2) . . . . ?
N6 Co1 O1 N1 -49.4(2) . . . . ?
N7 Co1 O1 N1 -141.7(2) . . . . ?
N5 Co1 O1 N1 -155.7(6) . . . . ?
Cu1 Co1 O1 N1 13.48(15) . . . . ?
N8 Co1 O1 O4 83.23(10) . . . . ?
N6 Co1 O1 O4 -92.62(10) . . . . ?
N7 Co1 O1 O4 175.07(10) . . . . ?
N5 Co1 O1 O4 161.1(7) . . . . ?
Cu1 Co1 O1 O4 -29.73(8) . . . . ?
C7 N4 O4 Co1 -174.60(18) . . . . ?
Cu1 N4 O4 Co1 13.1(3) . . . . ?
C7 N4 O4 O1 163.1(2) . . . . ?
Cu1 N4 O4 O1 -9.2(2) . . . . ?
O1 Co1 O4 N4 -36.6(2) . . . . ?
N8 Co1 O4 N4 -126.9(2) . . . . ?
N6 Co1 O4 N4 59.6(2) . . . . ?
N7 Co1 O4 N4 -179(25) . . . . ?
N5 Co1 O4 N4 146.0(2) . . . . ?
Cu1 Co1 O4 N4 -6.57(15) . . . . ?
N8 Co1 O4 O1 -90.33(9) . . . . ?
N6 Co1 O4 O1 96.13(9) . . . . ?
N7 Co1 O4 O1 -142.6(7) . . . . ?
N5 Co1 O4 O1 -177.40(9) . . . . ?
Cu1 Co1 O4 O1 29.99(8) . . . . ?
N1 O1 O4 N4 5.96(18) . . . . ?
Co1 O1 O4 N4 150.71(17) . . . . ?
N1 O1 O4 Co1 -144.75(16) . . . . ?
O1 N1 C2 C1 -4.0(4) . . . . ?
Cu1 N1 C2 C1 -176.9(2) . . . . ?
O1 N1 C2 C3 176.1(2) . . . . ?
Cu1 N1 C2 C3 3.1(3) . . . . ?
C4 N2 C3 O2 -0.8(4) . . . . ?
Cu1 N2 C3 O2 175.7(2) . . . . ?
C4 N2 C3 C2 177.8(2) . . . . ?
Cu1 N2 C3 C2 -5.6(3) . . . . ?
N1 C2 C3 O2 -179.6(2) . . . . ?
C1 C2 C3 O2 0.4(4) . . . . ?
N1 C2 C3 N2 1.6(3) . . . . ?
C1 C2 C3 N2 -178.4(3) . . . . ?
C3 N2 C4 C9 -164.1(3) . . . . ?
Cu1 N2 C4 C9 19.8(4) . . . . ?
C6 N3 C5 C9 161.5(3) . . . . ?
Cu1 N3 C5 C9 -28.6(3) . . . . ?
C5 N3 C6 O3 0.6(4) . . . . ?
Cu1 N3 C6 O3 -170.3(2) . . . . ?
C5 N3 C6 C7 -179.1(2) . . . . ?
Cu1 N3 C6 C7 10.0(3) . . . . ?
O4 N4 C7 C8 0.2(4) . . . . ?
Cu1 N4 C7 C8 173.8(2) . . . . ?
O4 N4 C7 C6 -179.1(2) . . . . ?
Cu1 N4 C7 C6 -5.6(3) . . . . ?
O3 C6 C7 N4 177.4(2) . . . . ?
N3 C6 C7 N4 -2.9(3) . . . . ?
O3 C6 C7 C8 -1.9(4) . . . . ?
N3 C6 C7 C8 177.8(3) . . . . ?
N3 C5 C9 C4 68.5(3) . . . . ?
N2 C4 C9 C5 -63.8(3) . . . . ?
Co1 N6 C10 C11 -21.7(3) . . . . ?
C15 N5 C11 C10 -161.0(2) . . . . ?
C13 N5 C11 C10 74.7(3) . . . . ?
Co1 N5 C11 C10 -45.1(3) . . . . ?
N6 C10 C11 N5 43.7(3) . . . . ?
Co1 N7 C12 C13 38.9(3) . . . . ?
C15 N5 C13 C12 141.2(2) . . . . ?
C11 N5 C13 C12 -93.9(3) . . . . ?
Co1 N5 C13 C12 23.9(3) . . . . ?
N7 C12 C13 N5 -40.8(3) . . . . ?
Co1 N8 C14 C15 16.4(3) . . . . ?
C11 N5 C15 C14 160.1(2) . . . . ?
C13 N5 C15 C14 -74.9(3) . . . . ?
Co1 N5 C15 C14 44.3(2) . . . . ?
N8 C14 C15 N5 -39.8(3) . . . . ?
Li1 O4WA O5W O4W -126(13) . . . . ?
Li1 O4WA O5W Li1 -34.0(18) . . . 16_656 ?
Li1 O4W O5W O4WA 126(13) . . . . ?
Li1 O4W O5W O4WA 94(12) 16_656 . . . ?
Li1 O4W O5W O4WA 116(12) 11_666 . . . ?
Li1 O4W O5W Li1 -32.9(17) 16_656 . . . ?
Li1 O4W O5W Li1 -10.6(14) 11_666 . . . ?
Li1 O4W O5W Li1 32.9(17) . . . 16_656 ?
Li1 O4W O5W Li1 22.3(14) 11_666 . . 16_656 ?
O4WA O5W Li1 Li1 -59(3) . . . 6_554 ?
O4W O5W Li1 Li1 115(2) . . . 6_554 ?
Li1 O5W Li1 Li1 41(2) 16_656 . . 6_554 ?
O4WA O5W Li1 Li1 -148(3) . . . 11_666 ?
O4W O5W Li1 Li1 25(3) . . . 11_666 ?
Li1 O5W Li1 Li1 -48(4) 16_656 . . 11_666 ?
O4WA O5W Li1 Li1 -100(3) . . . 16_656 ?
O4W O5W Li1 Li1 73(3) . . . 16_656 ?
O4WA O5W Li1 O4W -173(2) . . . . ?
Li1 O5W Li1 O4W -73(3) 16_656 . . . ?
O4WA O5W Li1 O5W 153.9(19) . . . 11_666 ?
O4W O5W Li1 O5W -32.8(14) . . . 11_666 ?
Li1 O5W Li1 O5W -106(3) 16_656 . . 11_666 ?
O4W O5W Li1 O4WA 173(2) . . . . ?
Li1 O5W Li1 O4WA 100(3) 16_656 . . . ?
O4WA O5W Li1 O4W 123(2) . . . 11_666 ?
O4W O5W Li1 O4W -64(2) . . . 11_666 ?
Li1 O5W Li1 O4W -137(4) 16_656 . . 11_666 ?
O4WA O5W Li1 O4W -37.2(13) . . . 16_656 ?
O4W O5W Li1 O4W 136.1(13) . . . 16_656 ?
Li1 O5W Li1 O4W 63(2) 16_656 . . 16_656 ?
O4WA O5W Li1 O5WA 108.1(15) . . . . ?
O4W O5W Li1 O5WA -78.6(13) . . . . ?
Li1 O5W Li1 O5WA -152(3) 16_656 . . . ?
O5W O4W Li1 Li1 -125(7) . . . 6_554 ?
Li1 O4W Li1 Li1 -21(5) 16_656 . . 6_554 ?
Li1 O4W Li1 Li1 33(5) 11_666 . . 6_554 ?
O5W O4W Li1 Li1 -159(3) . . . 11_666 ?
Li1 O4W Li1 Li1 -54(3) 16_656 . . 11_666 ?
O5W O4W Li1 Li1 -105(3) . . . 16_656 ?
Li1 O4W Li1 Li1 54(3) 11_666 . . 16_656 ?
Li1 O4W Li1 O5W 105(3) 16_656 . . . ?
Li1 O4W Li1 O5W 159(3) 11_666 . . . ?
O5W O4W Li1 O5W 147.5(13) . . . 11_666 ?
Li1 O4W Li1 O5W -108(2) 16_656 . . 11_666 ?
Li1 O4W Li1 O5W -54(2) 11_666 . . 11_666 ?
O5W O4W Li1 O4WA -3.6(11) . . . . ?
Li1 O4W Li1 O4WA 101(2) 16_656 . . . ?
Li1 O4W Li1 O4WA 155(3) 11_666 . . . ?
O5W O4W Li1 O4W 136(2) . . . 11_666 ?
Li1 O4W Li1 O4W -119(3) 16_656 . . 11_666 ?
Li1 O4W Li1 O4W -65(3) 11_666 . . 11_666 ?
O5W O4W Li1 O4W -44.2(15) . . . 16_656 ?
Li1 O4W Li1 O4W 60(2) 16_656 . . 16_656 ?
Li1 O4W Li1 O4W 114(2) 11_666 . . 16_656 ?
O5W O4W Li1 O5WA 97.9(15) . . . . ?
Li1 O4W Li1 O5WA -157(3) 16_656 . . . ?
Li1 O4W Li1 O5WA -103(3) 11_666 . . . ?
O5W O4WA Li1 Li1 145(3) . . . 6_554 ?
O5W O4WA Li1 Li1 52(5) . . . 11_666 ?
O5W O4WA Li1 Li1 82(3) . . . 16_656 ?
O5W O4WA Li1 O4W 4.6(15) . . . . ?
O5W O4WA Li1 O5W -36(2) . . . 11_666 ?
O5W O4WA Li1 O4W -90(3) . . . 11_666 ?
O5W O4WA Li1 O4W 132.9(18) . . . 16_656 ?
O5W O4WA Li1 O5WA -73.7(17) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        30.51
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.754
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.091


data_2b
_database_code_depnum_ccdc_archive 'CCDC 263428'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
tetraphenylphosphonium (N,N'-bis(2-Hydroxyiminopropionyl)propane-1,3-diamine)
-nickelate(II) monohydrate
;
_chemical_name_common            
;
tetraphenylphosphonium (N,N'-bis(2-
Hydroxyiminopropionyl)propane-1,3-diamine) -nickelate(ii) monohydrate
;
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H35 N4 Ni O5 P'
_chemical_formula_weight         657.33

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   11.539(2)
_cell_length_b                   12.188(2)
_cell_length_c                   12.527(3)
_cell_angle_alpha                61.69(3)
_cell_angle_beta                 75.10(3)
_cell_angle_gamma                76.22(3)
_cell_volume                     1484.8(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             688
_exptl_absorpt_coefficient_mu    0.757
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10292
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.45
_diffrn_reflns_theta_max         28.34
_reflns_number_total             6536
_reflns_number_gt                5592
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
;
Refinement of 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^)+(0.0540P)^2^+0.8613P] 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         6536
_refine_ls_number_parameters     403
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0365
_refine_ls_wR_factor_ref         0.1019
_refine_ls_wR_factor_gt          0.0979
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.040
_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 0.61794(2) 0.84885(2) 0.57896(2) 0.01459(8) Uani 1 1 d . . .
P1 P 0.88073(4) 0.42757(4) 0.85226(4) 0.01388(11) Uani 1 1 d . . .
O1 O 0.48326(13) 0.72855(13) 0.51233(14) 0.0203(3) Uani 1 1 d . . .
O2 O 0.88908(13) 0.77683(14) 0.34434(13) 0.0235(3) Uani 1 1 d . . .
O3 O 0.54286(15) 1.02066(15) 0.79275(15) 0.0283(3) Uani 1 1 d . . .
O4 O 0.37963(13) 0.78098(13) 0.68243(14) 0.0213(3) Uani 1 1 d . . .
O1W O 0.3844(3) 1.0596(3) 0.9800(3) 0.0949(10) Uani 1 1 d . . .
N1 N 0.59104(15) 0.76503(14) 0.49642(15) 0.0156(3) Uani 1 1 d . . .
N2 N 0.77409(15) 0.84376(15) 0.48966(16) 0.0175(3) Uani 1 1 d . . .
N3 N 0.64145(15) 0.94287(15) 0.65188(15) 0.0177(3) Uani 1 1 d . . .
N4 N 0.46467(15) 0.84425(15) 0.67697(15) 0.0171(3) Uani 1 1 d . . .
C1 C 0.6761(2) 0.6908(2) 0.3356(2) 0.0231(4) Uani 1 1 d . . .
H1A H 0.6276 0.6235 0.3804 0.035 Uiso 1 1 calc R . .
H1B H 0.7567 0.6586 0.3090 0.035 Uiso 1 1 calc R . .
H1C H 0.6412 0.7538 0.2653 0.035 Uiso 1 1 calc R . .
C2 C 0.68021(18) 0.74753(17) 0.41661(18) 0.0169(4) Uani 1 1 d . . .
C3 C 0.79316(18) 0.79157(18) 0.41288(18) 0.0173(4) Uani 1 1 d . . .
C4 C 0.87293(18) 0.89550(19) 0.49474(19) 0.0194(4) Uani 1 1 d . . .
H4A H 0.9332 0.9102 0.4210 0.023 Uiso 1 1 calc R . .
H4B H 0.9112 0.8354 0.5650 0.023 Uiso 1 1 calc R . .
C5 C 0.74869(19) 0.9999(2) 0.6290(2) 0.0223(4) Uani 1 1 d . . .
H5A H 0.7963 0.9463 0.6937 0.027 Uiso 1 1 calc R . .
H5B H 0.7236 1.0805 0.6316 0.027 Uiso 1 1 calc R . .
C6 C 0.54838(19) 0.96196(18) 0.73154(18) 0.0193(4) Uani 1 1 d . . .
C7 C 0.44165(18) 0.90228(18) 0.74496(18) 0.0185(4) Uani 1 1 d . . .
C8 C 0.3256(2) 0.9120(2) 0.8275(2) 0.0261(5) Uani 1 1 d . . .
H8A H 0.2596 0.9390 0.7831 0.039 Uiso 1 1 calc R . .
H8B H 0.3262 0.9721 0.8564 0.039 Uiso 1 1 calc R . .
H8C H 0.3159 0.8314 0.8964 0.039 Uiso 1 1 calc R . .
C9 C 0.82673(19) 1.01885(19) 0.5053(2) 0.0204(4) Uani 1 1 d . . .
H9A H 0.8954 1.0589 0.4933 0.024 Uiso 1 1 calc R . .
H9B H 0.7799 1.0748 0.4405 0.024 Uiso 1 1 calc R . .
C11 C 0.78627(18) 0.38243(18) 0.79021(17) 0.0159(4) Uani 1 1 d . . .
C12 C 0.70694(18) 0.47615(18) 0.71370(18) 0.0187(4) Uani 1 1 d . . .
H12 H 0.7067 0.5604 0.6923 0.022 Uiso 1 1 calc R . .
C13 C 0.62896(18) 0.4417(2) 0.67043(19) 0.0204(4) Uani 1 1 d . . .
H13 H 0.5774 0.5032 0.6184 0.024 Uiso 1 1 calc R . .
C14 C 0.62770(18) 0.3152(2) 0.70469(18) 0.0197(4) Uani 1 1 d . . .
H14 H 0.5753 0.2927 0.6753 0.024 Uiso 1 1 calc R . .
C15 C 0.70433(18) 0.22230(19) 0.78247(18) 0.0193(4) Uani 1 1 d . . .
H15 H 0.7018 0.1380 0.8062 0.023 Uiso 1 1 calc R . .
C16 C 0.78456(18) 0.25517(18) 0.82474(18) 0.0179(4) Uani 1 1 d . . .
H16 H 0.8368 0.1932 0.8756 0.021 Uiso 1 1 calc R . .
C21 C 0.78211(18) 0.52474(18) 0.92032(17) 0.0162(4) Uani 1 1 d . . .
C22 C 0.8039(2) 0.64527(19) 0.88828(19) 0.0215(4) Uani 1 1 d . . .
H22 H 0.8709 0.6776 0.8305 0.026 Uiso 1 1 calc R . .
C23 C 0.7248(2) 0.7169(2) 0.9432(2) 0.0286(5) Uani 1 1 d . . .
H23 H 0.7388 0.7974 0.9219 0.034 Uiso 1 1 calc R . .
C24 C 0.6251(2) 0.6683(2) 1.0299(2) 0.0279(5) Uani 1 1 d . . .
H24 H 0.5731 0.7159 1.0674 0.033 Uiso 1 1 calc R . .
C25 C 0.6026(2) 0.5490(2) 1.0608(2) 0.0281(5) Uani 1 1 d . . .
H25 H 0.5353 0.5172 1.1185 0.034 Uiso 1 1 calc R . .
C26 C 0.6800(2) 0.4768(2) 1.0062(2) 0.0238(4) Uani 1 1 d . . .
H26 H 0.6644 0.3973 1.0263 0.029 Uiso 1 1 calc R . .
C31 C 0.95170(17) 0.28863(17) 0.96717(17) 0.0153(4) Uani 1 1 d . . .
C32 C 0.91851(18) 0.25882(18) 1.09190(18) 0.0175(4) Uani 1 1 d . . .
H32 H 0.8618 0.3136 1.1176 0.021 Uiso 1 1 calc R . .
C33 C 0.9707(2) 0.14633(19) 1.17817(19) 0.0216(4) Uani 1 1 d . . .
H33 H 0.9498 0.1266 1.2615 0.026 Uiso 1 1 calc R . .
C34 C 1.0538(2) 0.06407(19) 1.1396(2) 0.0233(4) Uani 1 1 d . . .
H34 H 1.0862 -0.0123 1.1974 0.028 Uiso 1 1 calc R . .
C35 C 1.0889(2) 0.09498(19) 1.01535(19) 0.0221(4) Uani 1 1 d . . .
H35 H 1.1465 0.0402 0.9904 0.027 Uiso 1 1 calc R . .
C36 C 1.03872(18) 0.20716(18) 0.92760(18) 0.0187(4) Uani 1 1 d . . .
H36 H 1.0624 0.2278 0.8442 0.022 Uiso 1 1 calc R . .
C41 C 0.99920(17) 0.51177(17) 0.73855(17) 0.0148(4) Uani 1 1 d . . .
C42 C 1.09293(19) 0.52597(18) 0.78128(18) 0.0190(4) Uani 1 1 d . . .
H42 H 1.0939 0.4900 0.8652 0.023 Uiso 1 1 calc R . .
C43 C 1.18453(19) 0.59433(19) 0.69724(19) 0.0204(4) Uani 1 1 d . . .
H43 H 1.2469 0.6045 0.7249 0.025 Uiso 1 1 calc R . .
C44 C 1.18268(19) 0.64734(18) 0.57224(19) 0.0199(4) Uani 1 1 d . . .
H44 H 1.2437 0.6936 0.5164 0.024 Uiso 1 1 calc R . .
C45 C 1.09064(19) 0.63214(18) 0.52945(18) 0.0205(4) Uani 1 1 d . . .
H45 H 1.0910 0.6670 0.4453 0.025 Uiso 1 1 calc R . .
C46 C 0.99779(18) 0.56463(18) 0.61253(18) 0.0178(4) Uani 1 1 d . . .
H46 H 0.9356 0.5549 0.5844 0.021 Uiso 1 1 calc R . .
H1O1 H 0.420(4) 0.758(4) 0.602(4) 0.079(12) Uiso 1 1 d . . .
H1W1 H 0.4595 1.0318 0.9072 0.050 Uiso 0.50 1 d P . .
H2W1 H 0.4220 1.0142 1.0718 0.050 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 0.01447(14) 0.01459(13) 0.01760(14) -0.00814(10) -0.00394(9) -0.00338(9)
P1 0.0167(2) 0.0132(2) 0.0125(2) -0.00475(18) -0.00303(18) -0.00460(18)
O1 0.0158(7) 0.0222(7) 0.0302(8) -0.0150(6) -0.0068(6) -0.0045(5)
O2 0.0206(7) 0.0316(8) 0.0210(7) -0.0142(6) -0.0019(6) -0.0046(6)
O3 0.0331(9) 0.0353(9) 0.0269(8) -0.0219(7) 0.0023(7) -0.0129(7)
O4 0.0168(7) 0.0236(7) 0.0291(8) -0.0142(6) -0.0023(6) -0.0084(6)
O1W 0.133(3) 0.089(2) 0.075(2) -0.0481(17) 0.0003(19) -0.030(2)
N1 0.0152(8) 0.0134(7) 0.0202(8) -0.0066(6) -0.0075(6) -0.0023(6)
N2 0.0165(8) 0.0178(8) 0.0216(9) -0.0101(7) -0.0042(6) -0.0042(6)
N3 0.0174(8) 0.0190(8) 0.0203(8) -0.0096(7) -0.0040(6) -0.0061(6)
N4 0.0178(8) 0.0152(8) 0.0191(8) -0.0060(6) -0.0065(6) -0.0038(6)
C1 0.0218(10) 0.0276(11) 0.0276(11) -0.0173(9) -0.0061(8) -0.0032(8)
C2 0.0192(10) 0.0142(8) 0.0189(9) -0.0075(7) -0.0076(7) 0.0000(7)
C3 0.0187(10) 0.0159(9) 0.0159(9) -0.0054(7) -0.0057(7) -0.0006(7)
C4 0.0162(9) 0.0208(9) 0.0240(10) -0.0104(8) -0.0036(8) -0.0058(7)
C5 0.0215(10) 0.0252(10) 0.0274(11) -0.0144(9) -0.0048(8) -0.0089(8)
C6 0.0246(10) 0.0180(9) 0.0164(9) -0.0072(8) -0.0044(8) -0.0047(8)
C7 0.0198(10) 0.0173(9) 0.0180(10) -0.0072(8) -0.0014(7) -0.0046(7)
C8 0.0251(11) 0.0293(11) 0.0274(11) -0.0166(9) 0.0026(9) -0.0085(9)
C9 0.0183(10) 0.0197(10) 0.0266(11) -0.0106(8) -0.0047(8) -0.0064(8)
C11 0.0178(9) 0.0184(9) 0.0128(9) -0.0072(7) -0.0015(7) -0.0055(7)
C12 0.0199(10) 0.0171(9) 0.0189(10) -0.0071(8) -0.0044(8) -0.0027(7)
C13 0.0169(9) 0.0258(10) 0.0193(10) -0.0103(8) -0.0060(8) -0.0002(8)
C14 0.0150(9) 0.0293(11) 0.0196(10) -0.0143(8) -0.0014(7) -0.0052(8)
C15 0.0213(10) 0.0184(9) 0.0205(10) -0.0095(8) -0.0015(8) -0.0070(8)
C16 0.0205(10) 0.0161(9) 0.0165(9) -0.0058(7) -0.0033(7) -0.0045(7)
C21 0.0167(9) 0.0179(9) 0.0142(9) -0.0070(7) -0.0029(7) -0.0028(7)
C22 0.0242(10) 0.0233(10) 0.0200(10) -0.0116(8) 0.0013(8) -0.0097(8)
C23 0.0342(13) 0.0266(11) 0.0319(12) -0.0188(10) 0.0020(10) -0.0113(9)
C24 0.0256(11) 0.0342(12) 0.0301(12) -0.0217(10) 0.0009(9) -0.0045(9)
C25 0.0195(10) 0.0360(12) 0.0289(12) -0.0164(10) 0.0042(9) -0.0081(9)
C26 0.0219(10) 0.0204(10) 0.0274(11) -0.0097(8) 0.0008(8) -0.0073(8)
C31 0.0169(9) 0.0146(8) 0.0151(9) -0.0047(7) -0.0046(7) -0.0053(7)
C32 0.0207(10) 0.0173(9) 0.0156(9) -0.0067(7) -0.0033(7) -0.0056(7)
C33 0.0290(11) 0.0214(10) 0.0132(9) -0.0044(8) -0.0041(8) -0.0078(8)
C34 0.0291(11) 0.0174(9) 0.0214(10) -0.0040(8) -0.0109(8) -0.0023(8)
C35 0.0244(11) 0.0196(10) 0.0218(10) -0.0099(8) -0.0055(8) 0.0017(8)
C36 0.0204(10) 0.0198(9) 0.0162(9) -0.0071(8) -0.0031(7) -0.0052(8)
C41 0.0176(9) 0.0122(8) 0.0143(9) -0.0055(7) -0.0015(7) -0.0037(7)
C42 0.0243(10) 0.0203(9) 0.0140(9) -0.0071(8) -0.0026(8) -0.0075(8)
C43 0.0220(10) 0.0217(10) 0.0219(10) -0.0118(8) -0.0015(8) -0.0080(8)
C44 0.0223(10) 0.0166(9) 0.0205(10) -0.0090(8) 0.0023(8) -0.0068(8)
C45 0.0248(10) 0.0182(9) 0.0145(9) -0.0050(7) -0.0009(8) -0.0032(8)
C46 0.0200(10) 0.0172(9) 0.0172(9) -0.0080(8) -0.0037(7) -0.0030(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 1.8649(18) . ?
Ni1 N3 1.8680(17) . ?
Ni1 N4 1.8718(18) . ?
Ni1 N1 1.8781(17) . ?
P1 C11 1.795(2) . ?
P1 C41 1.798(2) . ?
P1 C21 1.800(2) . ?
P1 C31 1.801(2) . ?
O1 N1 1.355(2) . ?
O1 H1O1 1.33(4) . ?
O2 C3 1.248(2) . ?
O3 C6 1.256(2) . ?
O4 N4 1.356(2) . ?
O4 H1O1 1.13(4) . ?
O1W H1W1 1.2023 . ?
O1W H2W1 1.1642 . ?
N1 C2 1.293(3) . ?
N2 C3 1.335(3) . ?
N2 C4 1.456(2) . ?
N3 C6 1.324(3) . ?
N3 C5 1.461(3) . ?
N4 C7 1.289(3) . ?
C1 C2 1.488(3) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.506(3) . ?
C4 C9 1.527(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C9 1.520(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C7 1.509(3) . ?
C7 C8 1.485(3) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C11 C16 1.403(3) . ?
C11 C12 1.406(3) . ?
C12 C13 1.388(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.393(3) . ?
C13 H13 0.9300 . ?
C14 C15 1.390(3) . ?
C14 H14 0.9300 . ?
C15 C16 1.388(3) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C21 C22 1.395(3) . ?
C21 C26 1.402(3) . ?
C22 C23 1.391(3) . ?
C22 H22 0.9300 . ?
C23 C24 1.388(3) . ?
C23 H23 0.9300 . ?
C24 C25 1.387(3) . ?
C24 H24 0.9300 . ?
C25 C26 1.387(3) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C31 C32 1.393(3) . ?
C31 C36 1.406(3) . ?
C32 C33 1.395(3) . ?
C32 H32 0.9300 . ?
C33 C34 1.386(3) . ?
C33 H33 0.9300 . ?
C34 C35 1.386(3) . ?
C34 H34 0.9300 . ?
C35 C36 1.392(3) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
C41 C46 1.397(3) . ?
C41 C42 1.400(3) . ?
C42 C43 1.391(3) . ?
C42 H42 0.9300 . ?
C43 C44 1.386(3) . ?
C43 H43 0.9300 . ?
C44 C45 1.389(3) . ?
C44 H44 0.9300 . ?
C45 C46 1.394(3) . ?
C45 H45 0.9300 . ?
C46 H46 0.9300 . ?

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 N3 96.69(8) . . ?
N2 Ni1 N4 176.28(7) . . ?
N3 Ni1 N4 83.36(8) . . ?
N2 Ni1 N1 83.29(8) . . ?
N3 Ni1 N1 175.98(7) . . ?
N4 Ni1 N1 96.92(8) . . ?
C11 P1 C41 113.25(9) . . ?
C11 P1 C21 106.22(9) . . ?
C41 P1 C21 110.17(9) . . ?
C11 P1 C31 109.26(9) . . ?
C41 P1 C31 107.42(9) . . ?
C21 P1 C31 110.55(9) . . ?
N1 O1 H1O1 100.9(17) . . ?
N4 O4 H1O1 101(2) . . ?
H1W1 O1W H2W1 107.7 . . ?
C2 N1 O1 119.65(16) . . ?
C2 N1 Ni1 116.74(14) . . ?
O1 N1 Ni1 123.54(13) . . ?
C3 N2 C4 118.79(17) . . ?
C3 N2 Ni1 116.02(14) . . ?
C4 N2 Ni1 125.15(13) . . ?
C6 N3 C5 116.67(17) . . ?
C6 N3 Ni1 115.61(14) . . ?
C5 N3 Ni1 127.70(14) . . ?
C7 N4 O4 119.14(17) . . ?
C7 N4 Ni1 117.11(14) . . ?
O4 N4 Ni1 123.73(13) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C1 125.56(19) . . ?
N1 C2 C3 112.38(17) . . ?
C1 C2 C3 122.05(18) . . ?
O2 C3 N2 127.97(19) . . ?
O2 C3 C2 120.59(18) . . ?
N2 C3 C2 111.44(17) . . ?
N2 C4 C9 110.86(16) . . ?
N2 C4 H4A 109.5 . . ?
C9 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
C9 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
N3 C5 C9 112.07(17) . . ?
N3 C5 H5A 109.2 . . ?
C9 C5 H5A 109.2 . . ?
N3 C5 H5B 109.2 . . ?
C9 C5 H5B 109.2 . . ?
H5A C5 H5B 107.9 . . ?
O3 C6 N3 127.3(2) . . ?
O3 C6 C7 120.60(19) . . ?
N3 C6 C7 112.07(17) . . ?
N4 C7 C8 125.74(19) . . ?
N4 C7 C6 111.85(18) . . ?
C8 C7 C6 122.41(18) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C5 C9 C4 112.60(17) . . ?
C5 C9 H9A 109.1 . . ?
C4 C9 H9A 109.1 . . ?
C5 C9 H9B 109.1 . . ?
C4 C9 H9B 109.1 . . ?
H9A C9 H9B 107.8 . . ?
C16 C11 C12 120.24(18) . . ?
C16 C11 P1 120.70(15) . . ?
C12 C11 P1 118.87(15) . . ?
C13 C12 C11 119.37(18) . . ?
C13 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?
C12 C13 C14 120.22(19) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C15 C14 C13 120.42(19) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C16 C15 C14 120.13(19) . . ?
C16 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
C15 C16 C11 119.59(18) . . ?
C15 C16 H16 120.2 . . ?
C11 C16 H16 120.2 . . ?
C22 C21 C26 120.10(19) . . ?
C22 C21 P1 121.85(15) . . ?
C26 C21 P1 118.04(15) . . ?
C23 C22 C21 119.7(2) . . ?
C23 C22 H22 120.2 . . ?
C21 C22 H22 120.2 . . ?
C24 C23 C22 120.1(2) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C25 C24 C23 120.3(2) . . ?
C25 C24 H24 119.9 . . ?
C23 C24 H24 119.9 . . ?
C26 C25 C24 120.4(2) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C25 C26 C21 119.5(2) . . ?
C25 C26 H26 120.3 . . ?
C21 C26 H26 120.3 . . ?
C32 C31 C36 120.47(18) . . ?
C32 C31 P1 121.71(15) . . ?
C36 C31 P1 117.76(15) . . ?
C31 C32 C33 119.68(19) . . ?
C31 C32 H32 120.2 . . ?
C33 C32 H32 120.2 . . ?
C34 C33 C32 119.92(19) . . ?
C34 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
C35 C34 C33 120.39(19) . . ?
C35 C34 H34 119.8 . . ?
C33 C34 H34 119.8 . . ?
C34 C35 C36 120.6(2) . . ?
C34 C35 H35 119.7 . . ?
C36 C35 H35 119.7 . . ?
C35 C36 C31 118.84(19) . . ?
C35 C36 H36 120.6 . . ?
C31 C36 H36 120.6 . . ?
C46 C41 C42 120.51(18) . . ?
C46 C41 P1 122.28(15) . . ?
C42 C41 P1 117.19(15) . . ?
C43 C42 C41 119.53(18) . . ?
C43 C42 H42 120.2 . . ?
C41 C42 H42 120.2 . . ?
C44 C43 C42 119.92(19) . . ?
C44 C43 H43 120.0 . . ?
C42 C43 H43 120.0 . . ?
C43 C44 C45 120.72(19) . . ?
C43 C44 H44 119.6 . . ?
C45 C44 H44 119.6 . . ?
C44 C45 C46 120.03(19) . . ?
C44 C45 H45 120.0 . . ?
C46 C45 H45 120.0 . . ?
C45 C46 C41 119.29(19) . . ?
C45 C46 H46 120.4 . . ?
C41 C46 H46 120.4 . . ?

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
N2 Ni1 N1 C2 -3.35(14) . . . . ?
N3 Ni1 N1 C2 86.6(10) . . . . ?
N4 Ni1 N1 C2 -179.61(14) . . . . ?
N2 Ni1 N1 O1 179.85(15) . . . . ?
N3 Ni1 N1 O1 -90.2(10) . . . . ?
N4 Ni1 N1 O1 3.59(15) . . . . ?
N3 Ni1 N2 C3 -174.26(14) . . . . ?
N4 Ni1 N2 C3 95.1(11) . . . . ?
N1 Ni1 N2 C3 1.69(14) . . . . ?
N3 Ni1 N2 C4 3.52(17) . . . . ?
N4 Ni1 N2 C4 -87.1(11) . . . . ?
N1 Ni1 N2 C4 179.47(16) . . . . ?
N2 Ni1 N3 C6 -176.40(15) . . . . ?
N4 Ni1 N3 C6 -0.14(15) . . . . ?
N1 Ni1 N3 C6 94.1(10) . . . . ?
N2 Ni1 N3 C5 5.25(18) . . . . ?
N4 Ni1 N3 C5 -178.50(18) . . . . ?
N1 Ni1 N3 C5 -84.2(10) . . . . ?
N2 Ni1 N4 C7 91.7(11) . . . . ?
N3 Ni1 N4 C7 0.63(15) . . . . ?
N1 Ni1 N4 C7 -175.32(15) . . . . ?
N2 Ni1 N4 O4 -86.4(11) . . . . ?
N3 Ni1 N4 O4 -177.42(15) . . . . ?
N1 Ni1 N4 O4 6.62(15) . . . . ?
O1 N1 C2 C1 1.0(3) . . . . ?
Ni1 N1 C2 C1 -175.91(15) . . . . ?
O1 N1 C2 C3 -179.00(15) . . . . ?
Ni1 N1 C2 C3 4.1(2) . . . . ?
C4 N2 C3 O2 2.4(3) . . . . ?
Ni1 N2 C3 O2 -179.65(16) . . . . ?
C4 N2 C3 C2 -177.95(16) . . . . ?
Ni1 N2 C3 C2 0.0(2) . . . . ?
N1 C2 C3 O2 177.07(17) . . . . ?
C1 C2 C3 O2 -3.0(3) . . . . ?
N1 C2 C3 N2 -2.6(2) . . . . ?
C1 C2 C3 N2 177.39(17) . . . . ?
C3 N2 C4 C9 139.92(18) . . . . ?
Ni1 N2 C4 C9 -37.8(2) . . . . ?
C6 N3 C5 C9 -156.90(18) . . . . ?
Ni1 N3 C5 C9 21.4(3) . . . . ?
C5 N3 C6 O3 -2.3(3) . . . . ?
Ni1 N3 C6 O3 179.20(17) . . . . ?
C5 N3 C6 C7 178.26(16) . . . . ?
Ni1 N3 C6 C7 -0.3(2) . . . . ?
O4 N4 C7 C8 -2.9(3) . . . . ?
Ni1 N4 C7 C8 178.91(16) . . . . ?
O4 N4 C7 C6 177.23(15) . . . . ?
Ni1 N4 C7 C6 -0.9(2) . . . . ?
O3 C6 C7 N4 -178.75(18) . . . . ?
N3 C6 C7 N4 0.8(2) . . . . ?
O3 C6 C7 C8 1.4(3) . . . . ?
N3 C6 C7 C8 -179.06(18) . . . . ?
N3 C5 C9 C4 -60.3(2) . . . . ?
N2 C4 C9 C5 69.2(2) . . . . ?
C41 P1 C11 C16 114.28(17) . . . . ?
C21 P1 C11 C16 -124.67(17) . . . . ?
C31 P1 C11 C16 -5.40(19) . . . . ?
C41 P1 C11 C12 -70.58(18) . . . . ?
C21 P1 C11 C12 50.47(18) . . . . ?
C31 P1 C11 C12 169.74(15) . . . . ?
C16 C11 C12 C13 -1.5(3) . . . . ?
P1 C11 C12 C13 -176.65(16) . . . . ?
C11 C12 C13 C14 1.3(3) . . . . ?
C12 C13 C14 C15 0.0(3) . . . . ?
C13 C14 C15 C16 -1.3(3) . . . . ?
C14 C15 C16 C11 1.1(3) . . . . ?
C12 C11 C16 C15 0.3(3) . . . . ?
P1 C11 C16 C15 175.34(15) . . . . ?
C11 P1 C21 C22 -125.61(17) . . . . ?
C41 P1 C21 C22 -2.6(2) . . . . ?
C31 P1 C21 C22 115.97(18) . . . . ?
C11 P1 C21 C26 53.30(18) . . . . ?
C41 P1 C21 C26 176.32(16) . . . . ?
C31 P1 C21 C26 -65.11(18) . . . . ?
C26 C21 C22 C23 0.9(3) . . . . ?
P1 C21 C22 C23 179.83(17) . . . . ?
C21 C22 C23 C24 0.3(3) . . . . ?
C22 C23 C24 C25 -1.0(4) . . . . ?
C23 C24 C25 C26 0.5(4) . . . . ?
C24 C25 C26 C21 0.8(3) . . . . ?
C22 C21 C26 C25 -1.4(3) . . . . ?
P1 C21 C26 C25 179.62(17) . . . . ?
C11 P1 C31 C32 -109.02(17) . . . . ?
C41 P1 C31 C32 127.76(16) . . . . ?
C21 P1 C31 C32 7.53(19) . . . . ?
C11 P1 C31 C36 68.15(17) . . . . ?
C41 P1 C31 C36 -55.07(17) . . . . ?
C21 P1 C31 C36 -175.30(15) . . . . ?
C36 C31 C32 C33 -1.0(3) . . . . ?
P1 C31 C32 C33 176.10(15) . . . . ?
C31 C32 C33 C34 -1.0(3) . . . . ?
C32 C33 C34 C35 2.4(3) . . . . ?
C33 C34 C35 C36 -1.9(3) . . . . ?
C34 C35 C36 C31 0.0(3) . . . . ?
C32 C31 C36 C35 1.5(3) . . . . ?
P1 C31 C36 C35 -175.71(16) . . . . ?
C11 P1 C41 C46 15.82(19) . . . . ?
C21 P1 C41 C46 -102.98(17) . . . . ?
C31 P1 C41 C46 136.55(16) . . . . ?
C11 P1 C41 C42 -165.98(15) . . . . ?
C21 P1 C41 C42 75.22(17) . . . . ?
C31 P1 C41 C42 -45.25(17) . . . . ?
C46 C41 C42 C43 0.6(3) . . . . ?
P1 C41 C42 C43 -177.63(15) . . . . ?
C41 C42 C43 C44 -0.2(3) . . . . ?
C42 C43 C44 C45 -0.6(3) . . . . ?
C43 C44 C45 C46 1.0(3) . . . . ?
C44 C45 C46 C41 -0.6(3) . . . . ?
C42 C41 C46 C45 -0.2(3) . . . . ?
P1 C41 C46 C45 177.97(15) . . . . ?

_diffrn_measured_fraction_theta_max 0.881
_diffrn_reflns_theta_full        28.34
_diffrn_measured_fraction_theta_full 0.881
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.069

data_3b
_database_code_depnum_ccdc_archive 'CCDC 263429'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
tetraphenylarsonium (N,N'-bis(2-Hydroxyiminopropionyl)buthane-1,4-diamine)
-nickelate(II) trihydrate
;
_chemical_name_common            
;
tetraphenylarsonium (N,N'-bis(2-Hydroxyiminopropionyl)buthane-
1,4-diamine) -nickelate(ii) trihydrate
;
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H42 As N4 Ni O7.50'
_chemical_formula_weight         760.35

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   22.274(4)
_cell_length_b                   20.539(4)
_cell_length_c                   15.231(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.18(3)
_cell_angle_gamma                90.00
_cell_volume                     6913(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3160
_exptl_absorpt_coefficient_mu    1.566
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23778
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0526
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.35
_diffrn_reflns_theta_max         28.44
_reflns_number_total             8079
_reflns_number_gt                6289
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
;
Refinement of 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^)+(0.0505P)^2^+0.0000P] 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         8079
_refine_ls_number_parameters     571
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0419
_refine_ls_wR_factor_ref         0.0982
_refine_ls_wR_factor_gt          0.0902
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.071
_refine_ls_shift/su_mean         0.002

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.332523(12) 0.231642(12) 0.680624(17) 0.01536(8) Uani 1 1 d . . .
Ni1 Ni 0.260064(15) 0.466301(15) 0.81694(2) 0.01380(9) Uani 1 1 d . . .
O1 O 0.29173(9) 0.55122(9) 0.68013(12) 0.0204(4) Uani 1 1 d . . .
O2 O 0.43821(8) 0.46088(9) 0.88736(12) 0.0188(4) Uani 1 1 d . . .
O4 O 0.18513(9) 0.52791(9) 0.67335(12) 0.0208(4) Uani 1 1 d . . .
O3 O 0.10432(9) 0.40945(9) 0.89103(13) 0.0251(4) Uani 1 1 d . . .
O1W O 0.48060(10) 0.57092(11) 0.56227(14) 0.0285(5) Uani 1 1 d . . .
O2W O 0.00664(11) 0.32679(12) 0.84338(18) 0.0314(5) Uani 1 1 d . . .
O3W O 0.48572(15) 0.69027(13) 0.6588(2) 0.0508(8) Uani 1 1 d . . .
O4W O 0.5000 0.40248(15) 0.7500 0.0351(8) Uani 1 2 d S . .
N1 N 0.31104(10) 0.51360(10) 0.75093(14) 0.0164(5) Uani 1 1 d . . .
N2 N 0.33521(10) 0.43764(10) 0.87890(14) 0.0156(4) Uani 1 1 d . . .
N3 N 0.20658(10) 0.42788(10) 0.88773(14) 0.0168(5) Uani 1 1 d . . .
N4 N 0.18761(10) 0.49090(10) 0.74798(14) 0.0168(5) Uani 1 1 d . . .
C1 C 0.41383(12) 0.55671(14) 0.7450(2) 0.0242(6) Uani 1 1 d . . .
H1A H 0.4096 0.5530 0.6817 0.036 Uiso 1 1 calc R . .
H1B H 0.4536 0.5428 0.7693 0.036 Uiso 1 1 calc R . .
H1C H 0.4080 0.6012 0.7611 0.036 Uiso 1 1 calc R . .
C2 C 0.36760(12) 0.51486(12) 0.78077(17) 0.0169(5) Uani 1 1 d . . .
C3 C 0.38300(12) 0.46792(12) 0.85539(17) 0.0151(5) Uani 1 1 d . . .
C4 C 0.34784(13) 0.38336(13) 0.94289(18) 0.0188(6) Uani 1 1 d . . .
C9 C 0.30220(13) 0.32801(13) 0.92601(19) 0.0198(6) Uani 1 1 d . . .
C10 C 0.24769(13) 0.33327(13) 0.97719(19) 0.0211(6) Uani 1 1 d . . .
C5 C 0.22236(14) 0.40221(13) 0.97723(18) 0.0203(6) Uani 1 1 d . . .
C6 C 0.14819(12) 0.43044(12) 0.85586(17) 0.0186(6) Uani 1 1 d . . .
C7 C 0.13825(12) 0.46749(13) 0.77009(18) 0.0181(5) Uani 1 1 d . . .
C8 C 0.07699(13) 0.47772(15) 0.7208(2) 0.0285(7) Uani 1 1 d . . .
H8A H 0.0768 0.5170 0.6866 0.043 Uiso 1 1 calc R . .
H8B H 0.0479 0.4813 0.7620 0.043 Uiso 1 1 calc R . .
H8C H 0.0668 0.4415 0.6820 0.043 Uiso 1 1 calc R . .
C21 C 0.25070(12) 0.24327(13) 0.70405(17) 0.0181(5) Uani 1 1 d . . .
C24 C 0.13412(14) 0.26358(15) 0.7430(2) 0.0280(7) Uani 1 1 d . . .
C41 C 0.38845(12) 0.22784(12) 0.78715(17) 0.0171(5) Uani 1 1 d . . .
C45 C 0.47065(13) 0.27428(14) 0.88243(19) 0.0236(6) Uani 1 1 d . . .
C13 C 0.40872(15) 0.07637(15) 0.5612(2) 0.0290(7) Uani 1 1 d . . .
C46 C 0.43070(13) 0.27718(13) 0.80537(18) 0.0195(6) Uani 1 1 d . . .
C22 C 0.22726(13) 0.20275(14) 0.76443(19) 0.0231(6) Uani 1 1 d . . .
C31 C 0.35213(12) 0.30282(12) 0.60906(16) 0.0164(5) Uani 1 1 d . . .
C44 C 0.46830(13) 0.22262(15) 0.94047(19) 0.0241(6) Uani 1 1 d . . .
C36 C 0.37127(13) 0.29018(14) 0.52655(18) 0.0197(6) Uani 1 1 d . . .
C11 C 0.34163(12) 0.15346(12) 0.61608(17) 0.0175(5) Uani 1 1 d . . .
C43 C 0.42659(13) 0.17278(15) 0.92132(19) 0.0249(6) Uani 1 1 d . . .
C12 C 0.39961(14) 0.12907(14) 0.61595(19) 0.0242(6) Uani 1 1 d . . .
C16 C 0.29224(14) 0.12575(13) 0.56400(19) 0.0219(6) Uani 1 1 d . . .
C32 C 0.34728(13) 0.36694(13) 0.63869(18) 0.0212(6) Uani 1 1 d . . .
C26 C 0.21593(14) 0.29352(14) 0.66240(19) 0.0239(6) Uani 1 1 d . . .
C35 C 0.38603(14) 0.34154(15) 0.4743(2) 0.0256(6) Uani 1 1 d . . .
C25 C 0.15802(14) 0.30321(15) 0.6819(2) 0.0286(7) Uani 1 1 d . . .
C33 C 0.36183(14) 0.41766(14) 0.58559(19) 0.0244(6) Uani 1 1 d . . .
C42 C 0.38628(13) 0.17458(13) 0.84403(18) 0.0209(6) Uani 1 1 d . . .
C34 C 0.38126(14) 0.40482(15) 0.5044(2) 0.0277(7) Uani 1 1 d . . .
C23 C 0.16871(14) 0.21350(16) 0.7845(2) 0.0307(7) Uani 1 1 d . . .
C14 C 0.36040(15) 0.04916(14) 0.5086(2) 0.0283(7) Uani 1 1 d . . .
C15 C 0.30241(16) 0.07320(14) 0.5101(2) 0.0287(7) Uani 1 1 d . . .
H1O1 H 0.2397(17) 0.5458(17) 0.676(2) 0.051(11) Uiso 1 1 d . . .
H2 H 0.2316(13) 0.3211(14) 0.6222(19) 0.020(7) Uiso 1 1 d . . .
H3 H 0.2528(14) 0.1403(13) 0.5666(18) 0.020(8) Uiso 1 1 d . . .
H4 H 0.2519(11) 0.4328(12) 1.0087(16) 0.004(6) Uiso 1 1 d . . .
H5 H 0.2499(12) 0.1673(14) 0.7897(18) 0.017(7) Uiso 1 1 d . . .
H6 H 0.3550(14) 0.4628(16) 0.603(2) 0.033(9) Uiso 1 1 d . . .
H8 H 0.3664(13) 0.0124(14) 0.4699(19) 0.021(7) Uiso 1 1 d . . .
H9 H 0.0952(14) 0.2704(13) 0.7556(19) 0.018(7) Uiso 1 1 d . . .
H10 H 0.3350(11) 0.3739(12) 0.6954(18) 0.011(7) Uiso 1 1 d . . .
H14 H 0.2599(12) 0.3214(13) 1.0400(19) 0.016(7) Uiso 1 1 d . . .
H15 H 0.4348(13) 0.1507(14) 0.6517(19) 0.023(8) Uiso 1 1 d . . .
H16 H 0.2881(12) 0.3273(13) 0.864(2) 0.019(7) Uiso 1 1 d . . .
H17 H 0.3871(13) 0.3671(13) 0.9404(18) 0.017(7) Uiso 1 1 d . . .
H18 H 0.4322(14) 0.3135(15) 0.767(2) 0.034(9) Uiso 1 1 d . . .
H19 H 0.3238(14) 0.2858(15) 0.938(2) 0.031(8) Uiso 1 1 d . . .
H20 H 0.4929(12) 0.2204(12) 0.9948(19) 0.013(7) Uiso 1 1 d . . .
H21 H 0.4504(15) 0.0579(15) 0.563(2) 0.034(9) Uiso 1 1 d . . .
H22 H 0.1884(13) 0.4059(13) 1.0078(19) 0.019(7) Uiso 1 1 d . . .
H23 H 0.3761(13) 0.2494(14) 0.5070(19) 0.021(8) Uiso 1 1 d . . .
H24 H 0.2157(13) 0.2995(13) 0.9515(18) 0.016(7) Uiso 1 1 d . . .
H25 H 0.4254(13) 0.1369(15) 0.960(2) 0.027(8) Uiso 1 1 d . . .
H27 H 0.3503(13) 0.3990(14) 1.006(2) 0.024(8) Uiso 1 1 d . . .
H28 H 0.3919(16) 0.4440(18) 0.469(2) 0.051(11) Uiso 1 1 d . . .
H30 H 0.3575(13) 0.1380(14) 0.8308(18) 0.023(8) Uiso 1 1 d . . .
H31 H 0.5017(14) 0.3070(14) 0.895(2) 0.028(8) Uiso 1 1 d . . .
H33 H 0.3995(16) 0.3300(16) 0.418(2) 0.044(10) Uiso 1 1 d . . .
H1W4 H 0.4862(17) 0.4257(17) 0.790(2) 0.048(11) Uiso 1 1 d . . .
H1W1 H 0.4668(19) 0.561(2) 0.500(3) 0.076(14) Uiso 1 1 d . . .
H37 H 0.2704(14) 0.0553(15) 0.474(2) 0.030(9) Uiso 1 1 d . . .
H39 H 0.1315(15) 0.3337(16) 0.650(2) 0.038(9) Uiso 1 1 d . . .
H2W1 H 0.5010(17) 0.5376(18) 0.578(2) 0.047(12) Uiso 1 1 d . . .
H1W3 H 0.4829(15) 0.6676(15) 0.633(2) 0.016(10) Uiso 1 1 d . . .
H1W2 H 0.0349(19) 0.347(2) 0.861(3) 0.060(14) Uiso 1 1 d . . .
H45 H 0.1555(14) 0.1838(16) 0.828(2) 0.035(9) Uiso 1 1 d . . .
H2W2 H 0.001(3) 0.333(3) 0.796(4) 0.011(17) 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
As1 0.01948(15) 0.01298(14) 0.01372(14) 0.00043(10) 0.00240(10) -0.00163(10)
Ni1 0.01580(18) 0.01277(16) 0.01300(17) 0.00069(13) 0.00249(12) -0.00026(13)
O1 0.0220(11) 0.0217(10) 0.0170(10) 0.0081(8) 0.0003(8) 0.0004(8)
O2 0.0163(10) 0.0200(10) 0.0197(10) -0.0009(8) 0.0007(7) -0.0008(8)
O4 0.0223(11) 0.0241(10) 0.0158(10) 0.0063(8) 0.0010(7) 0.0022(8)
O3 0.0194(10) 0.0305(11) 0.0270(11) -0.0001(9) 0.0087(8) -0.0075(9)
O1W 0.0356(13) 0.0296(12) 0.0195(11) -0.0045(9) 0.0000(9) 0.0103(10)
O2W 0.0284(13) 0.0325(13) 0.0326(15) -0.0067(11) 0.0012(11) -0.0048(10)
O3W 0.073(2) 0.0310(15) 0.0487(18) -0.0198(14) 0.0098(15) -0.0018(14)
O4W 0.048(2) 0.0213(16) 0.041(2) 0.000 0.0254(17) 0.000
N1 0.0197(12) 0.0148(11) 0.0144(11) 0.0013(9) 0.0015(8) 0.0016(9)
N2 0.0187(12) 0.0143(10) 0.0138(11) 0.0009(8) 0.0018(8) 0.0000(9)
N3 0.0202(12) 0.0162(11) 0.0143(11) 0.0014(9) 0.0030(9) 0.0007(9)
N4 0.0206(12) 0.0159(11) 0.0139(11) -0.0010(9) 0.0020(8) 0.0009(9)
C1 0.0166(14) 0.0270(15) 0.0297(16) 0.0082(12) 0.0061(11) -0.0024(12)
C2 0.0207(14) 0.0149(12) 0.0161(13) -0.0011(10) 0.0058(10) -0.0021(10)
C3 0.0191(14) 0.0125(12) 0.0143(13) -0.0063(10) 0.0037(10) 0.0014(10)
C4 0.0192(15) 0.0194(14) 0.0175(14) 0.0022(11) 0.0019(11) 0.0037(11)
C9 0.0269(16) 0.0127(13) 0.0202(15) 0.0018(11) 0.0047(11) 0.0006(11)
C10 0.0280(16) 0.0177(13) 0.0177(14) 0.0047(11) 0.0026(11) -0.0016(12)
C5 0.0248(16) 0.0200(14) 0.0171(14) 0.0019(11) 0.0069(11) 0.0003(12)
C6 0.0239(15) 0.0150(13) 0.0177(14) -0.0028(11) 0.0054(11) -0.0032(11)
C7 0.0141(13) 0.0198(13) 0.0208(14) -0.0025(11) 0.0034(10) -0.0002(11)
C8 0.0174(15) 0.0399(18) 0.0278(16) 0.0028(14) 0.0017(12) -0.0015(13)
C21 0.0201(14) 0.0185(13) 0.0154(13) -0.0029(10) 0.0017(10) -0.0017(11)
C24 0.0167(15) 0.0372(18) 0.0309(17) -0.0099(14) 0.0064(12) -0.0015(13)
C41 0.0188(14) 0.0180(13) 0.0150(13) 0.0014(10) 0.0044(10) 0.0002(11)
C45 0.0235(16) 0.0234(15) 0.0234(15) -0.0034(12) 0.0008(11) -0.0033(12)
C13 0.0304(18) 0.0247(15) 0.0330(18) -0.0029(13) 0.0085(13) 0.0044(13)
C46 0.0208(14) 0.0199(14) 0.0181(14) 0.0002(11) 0.0037(11) 0.0001(11)
C22 0.0241(15) 0.0215(14) 0.0237(15) 0.0058(12) 0.0025(11) -0.0028(12)
C31 0.0191(14) 0.0160(13) 0.0136(13) 0.0016(10) 0.0000(10) -0.0016(10)
C44 0.0251(16) 0.0326(16) 0.0142(14) 0.0006(12) 0.0006(11) 0.0043(13)
C36 0.0221(15) 0.0180(14) 0.0193(14) 0.0004(11) 0.0035(11) 0.0013(11)
C11 0.0231(14) 0.0115(12) 0.0180(13) 0.0012(10) 0.0034(10) -0.0011(10)
C43 0.0264(16) 0.0272(15) 0.0213(15) 0.0089(13) 0.0030(12) 0.0019(13)
C12 0.0279(16) 0.0227(14) 0.0218(15) -0.0043(12) 0.0023(12) -0.0006(12)
C16 0.0264(16) 0.0161(13) 0.0227(15) 0.0010(11) 0.0001(11) -0.0024(12)
C32 0.0289(16) 0.0183(14) 0.0165(14) 0.0008(11) 0.0025(11) -0.0011(12)
C26 0.0295(17) 0.0194(14) 0.0225(15) 0.0012(12) 0.0024(12) -0.0013(12)
C35 0.0292(17) 0.0294(16) 0.0196(15) 0.0069(12) 0.0084(12) 0.0008(13)
C25 0.0247(16) 0.0262(16) 0.0344(18) -0.0017(14) 0.0018(13) 0.0029(13)
C33 0.0318(17) 0.0148(14) 0.0261(16) 0.0029(12) 0.0015(12) 0.0000(12)
C42 0.0233(15) 0.0190(14) 0.0200(14) 0.0029(11) 0.0013(11) -0.0008(11)
C34 0.0310(17) 0.0260(15) 0.0264(16) 0.0124(13) 0.0047(13) -0.0036(13)
C23 0.0232(16) 0.0362(18) 0.0332(18) 0.0026(15) 0.0054(13) -0.0070(14)
C14 0.046(2) 0.0170(14) 0.0217(16) -0.0040(12) 0.0045(13) -0.0007(13)
C15 0.043(2) 0.0188(15) 0.0220(16) 0.0017(12) -0.0070(13) -0.0046(14)

_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
As1 C11 1.907(3) . ?
As1 C31 1.907(3) . ?
As1 C21 1.915(3) . ?
As1 C41 1.920(3) . ?
Ni1 N3 1.878(2) . ?
Ni1 N1 1.879(2) . ?
Ni1 N4 1.881(2) . ?
Ni1 N2 1.909(2) . ?
O1 N1 1.352(3) . ?
O1 H1O1 1.16(4) . ?
O2 C3 1.273(3) . ?
O4 N4 1.363(3) . ?
O4 H1O1 1.27(4) . ?
O3 C6 1.248(3) . ?
O1W H1W1 0.98(5) . ?
O1W H2W1 0.84(4) . ?
O2W H1W2 0.78(4) . ?
O2W H2W2 0.73(5) . ?
O3W H1W3 0.61(3) . ?
O4W H1W4 0.86(3) . ?
N1 C2 1.285(3) . ?
N2 C3 1.320(3) . ?
N2 C4 1.484(3) . ?
N3 C6 1.331(3) . ?
N3 C5 1.463(3) . ?
N4 C7 1.283(3) . ?
C1 C2 1.495(4) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.497(4) . ?
C4 C9 1.525(4) . ?
C4 H17 0.94(3) . ?
C4 H27 1.00(3) . ?
C9 C10 1.527(4) . ?
C9 H16 0.95(3) . ?
C9 H19 1.00(3) . ?
C10 C5 1.524(4) . ?
C10 H14 0.99(3) . ?
C10 H24 1.04(3) . ?
C5 H4 0.99(2) . ?
C5 H22 0.94(3) . ?
C6 C7 1.504(4) . ?
C7 C8 1.488(4) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C21 C22 1.390(4) . ?
C21 C26 1.394(4) . ?
C24 C23 1.389(4) . ?
C24 C25 1.391(4) . ?
C24 H9 0.92(3) . ?
C41 C46 1.387(4) . ?
C41 C42 1.400(4) . ?
C45 C46 1.383(4) . ?
C45 C44 1.386(4) . ?
C45 H31 0.97(3) . ?
C13 C14 1.378(4) . ?
C13 C12 1.396(4) . ?
C13 H21 1.00(3) . ?
C46 H18 0.95(3) . ?
C22 C23 1.394(4) . ?
C22 H5 0.94(3) . ?
C31 C36 1.401(4) . ?
C31 C32 1.401(4) . ?
C44 C43 1.389(4) . ?
C44 H20 0.94(3) . ?
C36 C35 1.385(4) . ?
C36 H23 0.90(3) . ?
C11 C12 1.385(4) . ?
C11 C16 1.395(4) . ?
C43 C42 1.389(4) . ?
C43 H25 0.95(3) . ?
C12 H15 1.00(3) . ?
C16 C15 1.392(4) . ?
C16 H3 0.93(3) . ?
C32 C33 1.382(4) . ?
C32 H10 0.95(3) . ?
C26 C25 1.374(4) . ?
C26 H2 0.93(3) . ?
C35 C34 1.386(4) . ?
C35 H33 0.98(4) . ?
C25 H39 0.95(3) . ?
C33 C34 1.385(4) . ?
C33 H6 0.98(3) . ?
C42 H30 0.99(3) . ?
C34 H28 1.01(4) . ?
C23 H45 0.97(3) . ?
C14 C15 1.386(5) . ?
C14 H8 0.98(3) . ?
C15 H37 0.92(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
C11 As1 C31 107.71(11) . . ?
C11 As1 C21 111.47(11) . . ?
C31 As1 C21 107.59(11) . . ?
C11 As1 C41 107.57(11) . . ?
C31 As1 C41 110.09(11) . . ?
C21 As1 C41 112.31(11) . . ?
N3 Ni1 N1 173.70(9) . . ?
N3 Ni1 N4 82.64(10) . . ?
N1 Ni1 N4 95.51(9) . . ?
N3 Ni1 N2 99.58(9) . . ?
N1 Ni1 N2 82.69(9) . . ?
N4 Ni1 N2 175.44(9) . . ?
N1 O1 H1O1 102.0(18) . . ?
N4 O4 H1O1 101.5(16) . . ?
H1W1 O1W H2W1 102(3) . . ?
H1W2 O2W H2W2 106(6) . . ?
C2 N1 O1 118.1(2) . . ?
C2 N1 Ni1 116.91(18) . . ?
O1 N1 Ni1 124.67(17) . . ?
C3 N2 C4 116.0(2) . . ?
C3 N2 Ni1 114.04(17) . . ?
C4 N2 Ni1 129.70(17) . . ?
C6 N3 C5 117.6(2) . . ?
C6 N3 Ni1 115.79(17) . . ?
C5 N3 Ni1 126.21(18) . . ?
C7 N4 O4 118.8(2) . . ?
C7 N4 Ni1 117.15(19) . . ?
O4 N4 Ni1 123.91(17) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C1 124.9(2) . . ?
N1 C2 C3 112.1(2) . . ?
C1 C2 C3 122.9(2) . . ?
O2 C3 N2 128.0(2) . . ?
O2 C3 C2 118.8(2) . . ?
N2 C3 C2 113.2(2) . . ?
N2 C4 C9 112.4(2) . . ?
N2 C4 H17 109.9(17) . . ?
C9 C4 H17 109.3(17) . . ?
N2 C4 H27 111.6(17) . . ?
C9 C4 H27 110.8(17) . . ?
H17 C4 H27 102(2) . . ?
C4 C9 C10 114.7(2) . . ?
C4 C9 H16 108.0(17) . . ?
C10 C9 H16 108.6(17) . . ?
C4 C9 H19 108.7(18) . . ?
C10 C9 H19 111.6(18) . . ?
H16 C9 H19 105(2) . . ?
C5 C10 C9 112.6(2) . . ?
C5 C10 H14 106.6(15) . . ?
C9 C10 H14 109.5(16) . . ?
C5 C10 H24 112.6(15) . . ?
C9 C10 H24 108.3(15) . . ?
H14 C10 H24 107(2) . . ?
N3 C5 C10 112.3(2) . . ?
N3 C5 H4 106.9(14) . . ?
C10 C5 H4 111.5(14) . . ?
N3 C5 H22 108.5(17) . . ?
C10 C5 H22 113.4(17) . . ?
H4 C5 H22 104(2) . . ?
O3 C6 N3 127.7(3) . . ?
O3 C6 C7 120.6(2) . . ?
N3 C6 C7 111.6(2) . . ?
N4 C7 C8 125.2(3) . . ?
N4 C7 C6 112.3(2) . . ?
C8 C7 C6 122.4(2) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C22 C21 C26 120.7(3) . . ?
C22 C21 As1 119.6(2) . . ?
C26 C21 As1 119.7(2) . . ?
C23 C24 C25 120.1(3) . . ?
C23 C24 H9 120.0(18) . . ?
C25 C24 H9 119.9(18) . . ?
C46 C41 C42 121.5(3) . . ?
C46 C41 As1 119.5(2) . . ?
C42 C41 As1 119.1(2) . . ?
C46 C45 C44 120.2(3) . . ?
C46 C45 H31 120.5(18) . . ?
C44 C45 H31 119.2(18) . . ?
C14 C13 C12 120.0(3) . . ?
C14 C13 H21 121.1(19) . . ?
C12 C13 H21 118.8(19) . . ?
C45 C46 C41 119.1(3) . . ?
C45 C46 H18 119.3(19) . . ?
C41 C46 H18 121.6(19) . . ?
C21 C22 C23 119.3(3) . . ?
C21 C22 H5 120.6(17) . . ?
C23 C22 H5 120.1(17) . . ?
C36 C31 C32 120.5(2) . . ?
C36 C31 As1 119.21(19) . . ?
C32 C31 As1 120.3(2) . . ?
C45 C44 C43 120.5(3) . . ?
C45 C44 H20 122.5(17) . . ?
C43 C44 H20 116.9(16) . . ?
C35 C36 C31 119.6(3) . . ?
C35 C36 H23 118.2(19) . . ?
C31 C36 H23 122.1(19) . . ?
C12 C11 C16 121.4(3) . . ?
C12 C11 As1 117.7(2) . . ?
C16 C11 As1 120.6(2) . . ?
C44 C43 C42 120.2(3) . . ?
C44 C43 H25 120.9(19) . . ?
C42 C43 H25 118.8(19) . . ?
C11 C12 C13 119.1(3) . . ?
C11 C12 H15 120.4(16) . . ?
C13 C12 H15 120.4(17) . . ?
C15 C16 C11 118.5(3) . . ?
C15 C16 H3 119.8(18) . . ?
C11 C16 H3 121.6(18) . . ?
C33 C32 C31 119.2(3) . . ?
C33 C32 H10 122.3(16) . . ?
C31 C32 H10 118.6(16) . . ?
C25 C26 C21 119.5(3) . . ?
C25 C26 H2 119.4(18) . . ?
C21 C26 H2 121.1(18) . . ?
C36 C35 C34 119.4(3) . . ?
C36 C35 H33 116(2) . . ?
C34 C35 H33 124(2) . . ?
C26 C25 C24 120.5(3) . . ?
C26 C25 H39 122(2) . . ?
C24 C25 H39 118(2) . . ?
C32 C33 C34 120.1(3) . . ?
C32 C33 H6 120.0(19) . . ?
C34 C33 H6 119.7(19) . . ?
C43 C42 C41 118.5(3) . . ?
C43 C42 H30 119.1(16) . . ?
C41 C42 H30 122.5(17) . . ?
C33 C34 C35 121.2(3) . . ?
C33 C34 H28 116(2) . . ?
C35 C34 H28 123(2) . . ?
C24 C23 C22 119.9(3) . . ?
C24 C23 H45 125.2(19) . . ?
C22 C23 H45 114.9(19) . . ?
C13 C14 C15 120.5(3) . . ?
C13 C14 H8 120.6(17) . . ?
C15 C14 H8 118.9(17) . . ?
C14 C15 C16 120.5(3) . . ?
C14 C15 H37 120(2) . . ?
C16 C15 H37 119(2) . . ?

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
N3 Ni1 N1 C2 101.7(9) . . . . ?
N4 Ni1 N1 C2 174.33(19) . . . . ?
N2 Ni1 N1 C2 -9.89(19) . . . . ?
N3 Ni1 N1 O1 -71.4(9) . . . . ?
N4 Ni1 N1 O1 1.3(2) . . . . ?
N2 Ni1 N1 O1 177.0(2) . . . . ?
N3 Ni1 N2 C3 -166.81(17) . . . . ?
N1 Ni1 N2 C3 7.25(18) . . . . ?
N4 Ni1 N2 C3 74.3(12) . . . . ?
N3 Ni1 N2 C4 19.0(2) . . . . ?
N1 Ni1 N2 C4 -166.9(2) . . . . ?
N4 Ni1 N2 C4 -99.9(12) . . . . ?
N1 Ni1 N3 C6 78.5(9) . . . . ?
N4 Ni1 N3 C6 5.20(19) . . . . ?
N2 Ni1 N3 C6 -170.77(19) . . . . ?
N1 Ni1 N3 C5 -94.5(9) . . . . ?
N4 Ni1 N3 C5 -167.8(2) . . . . ?
N2 Ni1 N3 C5 16.2(2) . . . . ?
N3 Ni1 N4 C7 -7.0(2) . . . . ?
N1 Ni1 N4 C7 179.0(2) . . . . ?
N2 Ni1 N4 C7 112.4(12) . . . . ?
N3 Ni1 N4 O4 177.7(2) . . . . ?
N1 Ni1 N4 O4 3.8(2) . . . . ?
N2 Ni1 N4 O4 -62.8(12) . . . . ?
O1 N1 C2 C1 2.2(4) . . . . ?
Ni1 N1 C2 C1 -171.3(2) . . . . ?
O1 N1 C2 C3 -176.46(19) . . . . ?
Ni1 N1 C2 C3 10.0(3) . . . . ?
C4 N2 C3 O2 -7.9(4) . . . . ?
Ni1 N2 C3 O2 177.1(2) . . . . ?
C4 N2 C3 C2 171.1(2) . . . . ?
Ni1 N2 C3 C2 -3.9(3) . . . . ?
N1 C2 C3 O2 175.3(2) . . . . ?
C1 C2 C3 O2 -3.4(4) . . . . ?
N1 C2 C3 N2 -3.8(3) . . . . ?
C1 C2 C3 N2 177.6(2) . . . . ?
C3 N2 C4 C9 -145.1(2) . . . . ?
Ni1 N2 C4 C9 29.0(3) . . . . ?
N2 C4 C9 C10 -91.7(3) . . . . ?
C4 C9 C10 C5 43.0(3) . . . . ?
C6 N3 C5 C10 104.5(3) . . . . ?
Ni1 N3 C5 C10 -82.6(3) . . . . ?
C9 C10 C5 N3 55.6(3) . . . . ?
C5 N3 C6 O3 -5.1(4) . . . . ?
Ni1 N3 C6 O3 -178.8(2) . . . . ?
C5 N3 C6 C7 170.8(2) . . . . ?
Ni1 N3 C6 C7 -2.8(3) . . . . ?
O4 N4 C7 C8 -0.5(4) . . . . ?
Ni1 N4 C7 C8 -175.9(2) . . . . ?
O4 N4 C7 C6 -177.4(2) . . . . ?
Ni1 N4 C7 C6 7.1(3) . . . . ?
O3 C6 C7 N4 173.5(2) . . . . ?
N3 C6 C7 N4 -2.7(3) . . . . ?
O3 C6 C7 C8 -3.5(4) . . . . ?
N3 C6 C7 C8 -179.8(2) . . . . ?
C11 As1 C21 C22 70.4(2) . . . . ?
C31 As1 C21 C22 -171.7(2) . . . . ?
C41 As1 C21 C22 -50.4(2) . . . . ?
C11 As1 C21 C26 -111.5(2) . . . . ?
C31 As1 C21 C26 6.4(3) . . . . ?
C41 As1 C21 C26 127.7(2) . . . . ?
C11 As1 C41 C46 123.4(2) . . . . ?
C31 As1 C41 C46 6.3(2) . . . . ?
C21 As1 C41 C46 -113.6(2) . . . . ?
C11 As1 C41 C42 -55.5(2) . . . . ?
C31 As1 C41 C42 -172.6(2) . . . . ?
C21 As1 C41 C42 67.5(2) . . . . ?
C44 C45 C46 C41 0.0(4) . . . . ?
C42 C41 C46 C45 -1.4(4) . . . . ?
As1 C41 C46 C45 179.7(2) . . . . ?
C26 C21 C22 C23 -1.2(4) . . . . ?
As1 C21 C22 C23 176.8(2) . . . . ?
C11 As1 C31 C36 -2.1(2) . . . . ?
C21 As1 C31 C36 -122.4(2) . . . . ?
C41 As1 C31 C36 114.9(2) . . . . ?
C11 As1 C31 C32 177.7(2) . . . . ?
C21 As1 C31 C32 57.4(2) . . . . ?
C41 As1 C31 C32 -65.3(2) . . . . ?
C46 C45 C44 C43 1.1(4) . . . . ?
C32 C31 C36 C35 0.6(4) . . . . ?
As1 C31 C36 C35 -179.6(2) . . . . ?
C31 As1 C11 C12 80.1(2) . . . . ?
C21 As1 C11 C12 -162.1(2) . . . . ?
C41 As1 C11 C12 -38.6(2) . . . . ?
C31 As1 C11 C16 -93.7(2) . . . . ?
C21 As1 C11 C16 24.1(3) . . . . ?
C41 As1 C11 C16 147.6(2) . . . . ?
C45 C44 C43 C42 -0.7(4) . . . . ?
C16 C11 C12 C13 1.2(4) . . . . ?
As1 C11 C12 C13 -172.6(2) . . . . ?
C14 C13 C12 C11 -0.2(4) . . . . ?
C12 C11 C16 C15 -1.1(4) . . . . ?
As1 C11 C16 C15 172.5(2) . . . . ?
C36 C31 C32 C33 -0.2(4) . . . . ?
As1 C31 C32 C33 179.9(2) . . . . ?
C22 C21 C26 C25 0.4(4) . . . . ?
As1 C21 C26 C25 -177.6(2) . . . . ?
C31 C36 C35 C34 -0.4(4) . . . . ?
C21 C26 C25 C24 0.3(5) . . . . ?
C23 C24 C25 C26 -0.4(5) . . . . ?
C31 C32 C33 C34 -0.4(4) . . . . ?
C44 C43 C42 C41 -0.7(4) . . . . ?
C46 C41 C42 C43 1.8(4) . . . . ?
As1 C41 C42 C43 -179.3(2) . . . . ?
C32 C33 C34 C35 0.6(5) . . . . ?
C36 C35 C34 C33 -0.2(5) . . . . ?
C25 C24 C23 C22 -0.4(5) . . . . ?
C21 C22 C23 C24 1.2(5) . . . . ?
C12 C13 C14 C15 -0.7(5) . . . . ?
C13 C14 C15 C16 0.8(5) . . . . ?
C11 C16 C15 C14 0.1(4) . . . . ?

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 H1O1 O4 1.16(4) 1.27(4) 2.412(3) 169(3) .

_diffrn_measured_fraction_theta_max 0.927
_diffrn_reflns_theta_full        28.44
_diffrn_measured_fraction_theta_full 0.927
_refine_diff_density_max         0.800
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.087

data_5
_database_code_depnum_ccdc_archive 'CCDC 263430'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
(tris(2-aminoethyl)amine)-nickel(II)(N,N'-bis(2-Hydroxyiminopropionyl)
ethane-1,2-diamine)-nickel(II) dihydrate
;
_chemical_name_common            
;
(tris(2-aminoethyl)amine)-nickel(ii)(N,N'-bis(2-
Hydroxyiminopropionyl) ethane-1,2-diamine)-nickel(ii) dihydrate
;
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H32 N8 Ni2 O6'
_chemical_formula_weight         525.90

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/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                   7.743(2)
_cell_length_b                   14.627(3)
_cell_length_c                   19.177(4)
_cell_angle_alpha                90.00(3)
_cell_angle_beta                 96.77(3)
_cell_angle_gamma                90.00(3)
_cell_volume                     2156.8(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1104
_exptl_absorpt_coefficient_mu    1.794
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13666
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_sigmaI/netI    0.0172
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.99
_diffrn_reflns_theta_max         28.99
_reflns_number_total             5260
_reflns_number_gt                4839
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
;
Refinement of 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^)+(0.0656P)^2^+2.7719P] 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     SHELXL
_refine_ls_extinction_coef       0.0017(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         5260
_refine_ls_number_parameters     274
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0477
_refine_ls_wR_factor_ref         0.1314
_refine_ls_wR_factor_gt          0.1262
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_restrained_S_all      1.130
_refine_ls_shift/su_max          0.004
_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 0.16419(4) 0.41696(2) 0.354077(17) 0.02958(12) Uani 1 1 d . . .
Ni2 Ni -0.14603(4) 0.24495(2) 0.373229(16) 0.02815(12) Uani 1 1 d . . .
O1 O 0.0572(3) 0.27792(15) 0.44583(11) 0.0393(4) Uani 1 1 d . . .
O2 O 0.3085(4) 0.55393(18) 0.52558(13) 0.0543(6) Uani 1 1 d . . .
O3 O 0.2576(4) 0.48589(16) 0.16613(12) 0.0506(6) Uani 1 1 d . . .
O4 O -0.0020(3) 0.25684(13) 0.28775(11) 0.0357(4) Uani 1 1 d . . .
O5 O 0.1358(6) 0.1273(2) 0.53308(19) 0.0917(12) Uani 1 1 d . . .
O6 O 0.2733(9) 0.4560(4) 0.0295(2) 0.148(3) Uani 1 1 d . . .
N1 N 0.1276(3) 0.36062(16) 0.43937(12) 0.0331(5) Uani 1 1 d . . .
N2 N 0.2566(3) 0.50800(18) 0.41108(13) 0.0406(5) Uani 1 1 d . . .
N3 N 0.2236(3) 0.48926(16) 0.28281(13) 0.0362(5) Uani 1 1 d . . .
N4 N 0.0784(3) 0.33610(15) 0.28122(12) 0.0297(4) Uani 1 1 d . . .
N5 N -0.3743(3) 0.19695(19) 0.31272(14) 0.0411(5) Uani 1 1 d . . .
N6 N -0.0759(4) 0.10517(18) 0.37419(15) 0.0448(6) Uani 1 1 d . . .
H6A H 0.0188 0.0974 0.3518 0.054 Uiso 1 1 calc R . .
H6B H -0.0505 0.0857 0.4187 0.054 Uiso 1 1 calc R . .
N7 N -0.3028(4) 0.23535(19) 0.45534(14) 0.0403(5) Uani 1 1 d . . .
H7A H -0.2793 0.1830 0.4792 0.048 Uiso 1 1 calc R . .
H7B H -0.2797 0.2824 0.4853 0.048 Uiso 1 1 calc R . .
N8 N -0.2549(3) 0.37406(17) 0.34175(14) 0.0384(5) Uani 1 1 d . . .
H8A H -0.2801 0.4053 0.3797 0.046 Uiso 1 1 calc R . .
H8B H -0.1774 0.4068 0.3207 0.046 Uiso 1 1 calc R . .
C1 C 0.1691(5) 0.3762(3) 0.56846(16) 0.0509(8) Uani 1 1 d . . .
H1C H 0.0488 0.3705 0.5754 0.076 Uiso 1 1 calc R . .
H1D H 0.2244 0.4202 0.6009 0.076 Uiso 1 1 calc R . .
H1E H 0.2256 0.3180 0.5762 0.076 Uiso 1 1 calc R . .
C2 C 0.1825(4) 0.4069(2) 0.49541(15) 0.0355(6) Uani 1 1 d . . .
C3 C 0.2573(4) 0.4976(2) 0.47949(15) 0.0372(6) Uani 1 1 d . . .
C4 C 0.3111(5) 0.5908(2) 0.37849(18) 0.0469(7) Uani 1 1 d . . .
H4A H 0.4193 0.6130 0.4034 0.056 Uiso 1 1 calc R . .
H4B H 0.2234 0.6380 0.3796 0.056 Uiso 1 1 calc R . .
C5 C 0.3357(4) 0.5678(2) 0.30295(18) 0.0435(7) Uani 1 1 d . . .
H5A H 0.3031 0.6194 0.2725 0.052 Uiso 1 1 calc R . .
H5B H 0.4563 0.5526 0.2993 0.052 Uiso 1 1 calc R . .
C6 C 0.2019(4) 0.45362(19) 0.21948(15) 0.0337(5) Uani 1 1 d . . .
C7 C 0.1040(3) 0.36516(19) 0.21868(14) 0.0333(5) Uani 1 1 d . . .
C8 C 0.0426(5) 0.3166(2) 0.15251(17) 0.0493(8) Uani 1 1 d . . .
H8C H 0.1363 0.3117 0.1241 0.074 Uiso 1 1 calc R . .
H8D H -0.0516 0.3501 0.1274 0.074 Uiso 1 1 calc R . .
H8E H 0.0033 0.2565 0.1632 0.074 Uiso 1 1 calc R . .
C9 C -0.3203(5) 0.1101(3) 0.2825(2) 0.0555(9) Uani 1 1 d . . .
H9A H -0.2470 0.1227 0.2460 0.067 Uiso 1 1 calc R . .
H9B H -0.4222 0.0771 0.2615 0.067 Uiso 1 1 calc R . .
C10 C -0.2222(6) 0.0524(2) 0.3389(2) 0.0592(10) Uani 1 1 d . . .
H10A H -0.2992 0.0341 0.3728 0.071 Uiso 1 1 calc R . .
H10B H -0.1791 -0.0024 0.3183 0.071 Uiso 1 1 calc R . .
C11 C -0.5157(4) 0.1843(3) 0.3580(2) 0.0523(8) Uani 1 1 d . . .
H11A H -0.5259 0.1197 0.3684 0.063 Uiso 1 1 calc R . .
H11B H -0.6249 0.2040 0.3324 0.063 Uiso 1 1 calc R . .
C12 C -0.4847(4) 0.2372(3) 0.4267(2) 0.0510(8) Uani 1 1 d . . .
H12A H -0.5214 0.3001 0.4186 0.061 Uiso 1 1 calc R . .
H12B H -0.5544 0.2108 0.4605 0.061 Uiso 1 1 calc R . .
C13 C -0.4153(5) 0.2671(3) 0.25825(19) 0.0566(9) Uani 1 1 d . . .
H13A H -0.5289 0.2553 0.2328 0.068 Uiso 1 1 calc R . .
H13B H -0.3299 0.2654 0.2251 0.068 Uiso 1 1 calc R . .
C14 C -0.4140(4) 0.3607(3) 0.2928(2) 0.0544(9) Uani 1 1 d . . .
H14A H -0.4214 0.4078 0.2570 0.065 Uiso 1 1 calc R . .
H14B H -0.5148 0.3665 0.3181 0.065 Uiso 1 1 calc R . .
H1 H 0.1223 0.1800 0.5022 0.050 Uiso 1 1 d . . .
H2 H 0.1668 0.0720 0.5008 0.050 Uiso 1 1 d . . .
H3 H 0.2711 0.4600 0.0785 0.050 Uiso 1 1 d . . .
H4 H 0.3877 0.4303 0.0296 0.050 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 0.02750(19) 0.0305(2) 0.03047(19) -0.00020(12) 0.00216(13) -0.00372(12)
Ni2 0.02717(19) 0.02647(19) 0.03066(19) -0.00177(11) 0.00274(13) -0.00126(11)
O1 0.0395(10) 0.0370(10) 0.0390(10) 0.0073(8) -0.0053(8) -0.0085(8)
O2 0.0689(16) 0.0505(13) 0.0440(12) -0.0174(10) 0.0083(11) -0.0144(12)
O3 0.0714(16) 0.0440(12) 0.0392(11) 0.0055(9) 0.0177(11) -0.0070(11)
O4 0.0390(10) 0.0288(9) 0.0408(10) -0.0061(7) 0.0110(8) -0.0069(7)
O5 0.131(3) 0.064(2) 0.074(2) 0.0172(16) -0.012(2) 0.012(2)
O6 0.232(6) 0.140(4) 0.086(3) -0.063(3) 0.085(4) -0.091(4)
N1 0.0278(10) 0.0341(11) 0.0369(11) 0.0014(9) 0.0019(8) -0.0012(8)
N2 0.0435(13) 0.0391(13) 0.0385(12) -0.0032(10) 0.0018(10) -0.0131(10)
N3 0.0380(12) 0.0328(11) 0.0375(12) 0.0028(9) 0.0037(9) -0.0044(9)
N4 0.0261(9) 0.0284(10) 0.0351(10) -0.0010(8) 0.0061(8) 0.0004(8)
N5 0.0350(12) 0.0447(14) 0.0431(13) -0.0078(11) 0.0025(10) -0.0093(10)
N6 0.0514(15) 0.0339(12) 0.0514(15) 0.0015(11) 0.0147(12) 0.0078(11)
N7 0.0428(13) 0.0409(13) 0.0387(13) -0.0007(10) 0.0111(10) 0.0001(10)
N8 0.0374(12) 0.0347(12) 0.0446(13) 0.0026(10) 0.0111(10) 0.0056(10)
C1 0.0546(19) 0.062(2) 0.0356(15) 0.0013(14) 0.0028(13) -0.0066(16)
C2 0.0308(12) 0.0411(14) 0.0334(13) -0.0046(11) -0.0010(10) -0.0004(10)
C3 0.0337(13) 0.0400(14) 0.0375(13) -0.0068(11) 0.0019(10) -0.0009(11)
C4 0.0518(18) 0.0382(16) 0.0511(18) -0.0054(13) 0.0075(14) -0.0150(13)
C5 0.0468(16) 0.0351(14) 0.0493(17) 0.0006(12) 0.0083(13) -0.0105(12)
C6 0.0330(12) 0.0300(12) 0.0387(13) 0.0031(10) 0.0064(10) 0.0036(10)
C7 0.0317(12) 0.0325(12) 0.0361(13) -0.0002(10) 0.0054(10) 0.0042(10)
C8 0.070(2) 0.0412(16) 0.0375(15) -0.0074(12) 0.0078(14) -0.0055(15)
C9 0.056(2) 0.056(2) 0.0552(19) -0.0261(16) 0.0101(16) -0.0194(17)
C10 0.074(2) 0.0309(15) 0.077(3) -0.0131(15) 0.026(2) -0.0089(16)
C11 0.0364(15) 0.058(2) 0.064(2) -0.0109(16) 0.0128(14) -0.0157(14)
C12 0.0381(16) 0.060(2) 0.058(2) -0.0037(16) 0.0191(14) 0.0002(14)
C13 0.0434(17) 0.079(3) 0.0435(17) 0.0043(17) -0.0099(14) -0.0050(17)
C14 0.0399(16) 0.060(2) 0.062(2) 0.0212(17) 0.0006(14) 0.0118(15)

_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 1.816(3) . ?
Ni1 N3 1.829(2) . ?
Ni1 N1 1.883(2) . ?
Ni1 N4 1.890(2) . ?
Ni1 Ni2 3.5273(12) . ?
Ni2 O1 2.033(2) . ?
Ni2 O4 2.096(2) . ?
Ni2 N7 2.103(3) . ?
Ni2 N6 2.115(3) . ?
Ni2 N5 2.117(3) . ?
Ni2 N8 2.126(3) . ?
O1 N1 1.338(3) . ?
O1 O4 3.028(3) . ?
O2 C3 1.239(4) . ?
O3 C6 1.248(3) . ?
O4 N4 1.329(3) . ?
O5 H1 0.9697 . ?
O5 H2 1.0637 . ?
O6 H3 0.9431 . ?
O6 H4 0.9615 . ?
N1 C2 1.299(4) . ?
N2 C3 1.320(4) . ?
N2 C4 1.448(4) . ?
N3 C6 1.314(4) . ?
N3 C5 1.463(4) . ?
N4 C7 1.309(3) . ?
N5 C13 1.472(5) . ?
N5 C9 1.477(4) . ?
N5 C11 1.487(4) . ?
N6 C10 1.468(5) . ?
N6 H6A 0.9000 . ?
N6 H6B 0.9000 . ?
N7 C12 1.451(4) . ?
N7 H7A 0.9000 . ?
N7 H7B 0.9000 . ?
N8 C14 1.471(4) . ?
N8 H8A 0.9000 . ?
N8 H8B 0.9000 . ?
C1 C2 1.486(4) . ?
C1 H1C 0.9600 . ?
C1 H1D 0.9600 . ?
C1 H1E 0.9600 . ?
C2 C3 1.493(4) . ?
C4 C5 1.521(5) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C7 1.499(4) . ?
C7 C8 1.483(4) . ?
C8 H8C 0.9600 . ?
C8 H8D 0.9600 . ?
C8 H8E 0.9600 . ?
C9 C10 1.505(6) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.523(5) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.521(6) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?

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 N3 84.82(11) . . ?
N2 Ni1 N1 83.52(11) . . ?
N3 Ni1 N1 168.26(11) . . ?
N2 Ni1 N4 169.47(11) . . ?
N3 Ni1 N4 84.66(10) . . ?
N1 Ni1 N4 107.01(10) . . ?
N2 Ni1 Ni2 133.27(8) . . ?
N3 Ni1 Ni2 136.43(8) . . ?
N1 Ni1 Ni2 54.77(7) . . ?
N4 Ni1 Ni2 56.39(7) . . ?
O1 Ni2 O4 94.34(9) . . ?
O1 Ni2 N7 88.37(10) . . ?
O4 Ni2 N7 176.83(10) . . ?
O1 Ni2 N6 92.64(11) . . ?
O4 Ni2 N6 85.82(10) . . ?
N7 Ni2 N6 95.70(11) . . ?
O1 Ni2 N5 169.53(9) . . ?
O4 Ni2 N5 94.91(9) . . ?
N7 Ni2 N5 82.53(11) . . ?
N6 Ni2 N5 83.17(12) . . ?
O1 Ni2 N8 103.46(10) . . ?
O4 Ni2 N8 86.21(9) . . ?
N7 Ni2 N8 91.57(10) . . ?
N6 Ni2 N8 162.52(11) . . ?
N5 Ni2 N8 82.04(11) . . ?
O1 Ni2 Ni1 54.57(6) . . ?
O4 Ni2 Ni1 55.09(6) . . ?
N7 Ni2 Ni1 125.86(8) . . ?
N6 Ni2 Ni1 120.87(8) . . ?
N5 Ni2 Ni1 135.59(8) . . ?
N8 Ni2 Ni1 65.73(7) . . ?
N1 O1 Ni2 116.21(16) . . ?
N1 O1 O4 90.83(15) . . ?
Ni2 O1 O4 43.64(6) . . ?
N4 O4 Ni2 116.39(15) . . ?
N4 O4 O1 89.32(14) . . ?
Ni2 O4 O1 42.02(6) . . ?
H1 O5 H2 105.3 . . ?
H3 O6 H4 98.5 . . ?
C2 N1 O1 119.5(2) . . ?
C2 N1 Ni1 115.0(2) . . ?
O1 N1 Ni1 125.50(18) . . ?
C3 N2 C4 124.0(3) . . ?
C3 N2 Ni1 117.9(2) . . ?
C4 N2 Ni1 117.9(2) . . ?
C6 N3 C5 124.2(2) . . ?
C6 N3 Ni1 116.44(19) . . ?
C5 N3 Ni1 116.7(2) . . ?
C7 N4 O4 119.5(2) . . ?
C7 N4 Ni1 113.33(18) . . ?
O4 N4 Ni1 127.14(17) . . ?
C13 N5 C9 111.6(3) . . ?
C13 N5 C11 112.9(3) . . ?
C9 N5 C11 112.5(3) . . ?
C13 N5 Ni2 104.7(2) . . ?
C9 N5 Ni2 104.1(2) . . ?
C11 N5 Ni2 110.2(2) . . ?
C10 N6 Ni2 108.7(2) . . ?
C10 N6 H6A 110.0 . . ?
Ni2 N6 H6A 110.0 . . ?
C10 N6 H6B 110.0 . . ?
Ni2 N6 H6B 110.0 . . ?
H6A N6 H6B 108.3 . . ?
C12 N7 Ni2 109.6(2) . . ?
C12 N7 H7A 109.7 . . ?
Ni2 N7 H7A 109.7 . . ?
C12 N7 H7B 109.7 . . ?
Ni2 N7 H7B 109.7 . . ?
H7A N7 H7B 108.2 . . ?
C14 N8 Ni2 109.7(2) . . ?
C14 N8 H8A 109.7 . . ?
Ni2 N8 H8A 109.7 . . ?
C14 N8 H8B 109.7 . . ?
Ni2 N8 H8B 109.7 . . ?
H8A N8 H8B 108.2 . . ?
C2 C1 H1C 109.5 . . ?
C2 C1 H1D 109.5 . . ?
H1C C1 H1D 109.5 . . ?
C2 C1 H1E 109.5 . . ?
H1C C1 H1E 109.5 . . ?
H1D C1 H1E 109.5 . . ?
N1 C2 C1 124.7(3) . . ?
N1 C2 C3 113.0(3) . . ?
C1 C2 C3 122.2(3) . . ?
O2 C3 N2 126.5(3) . . ?
O2 C3 C2 123.0(3) . . ?
N2 C3 C2 110.5(2) . . ?
N2 C4 C5 107.5(2) . . ?
N2 C4 H4A 110.2 . . ?
C5 C4 H4A 110.2 . . ?
N2 C4 H4B 110.2 . . ?
C5 C4 H4B 110.2 . . ?
H4A C4 H4B 108.5 . . ?
N3 C5 C4 106.7(2) . . ?
N3 C5 H5A 110.4 . . ?
C4 C5 H5A 110.4 . . ?
N3 C5 H5B 110.4 . . ?
C4 C5 H5B 110.4 . . ?
H5A C5 H5B 108.6 . . ?
O3 C6 N3 126.1(3) . . ?
O3 C6 C7 122.7(3) . . ?
N3 C6 C7 111.2(2) . . ?
N4 C7 C8 124.1(3) . . ?
N4 C7 C6 113.7(2) . . ?
C8 C7 C6 122.2(3) . . ?
C7 C8 H8C 109.5 . . ?
C7 C8 H8D 109.5 . . ?
H8C C8 H8D 109.5 . . ?
C7 C8 H8E 109.5 . . ?
H8C C8 H8E 109.5 . . ?
H8D C8 H8E 109.5 . . ?
N5 C9 C10 110.0(3) . . ?
N5 C9 H9A 109.7 . . ?
C10 C9 H9A 109.7 . . ?
N5 C9 H9B 109.7 . . ?
C10 C9 H9B 109.7 . . ?
H9A C9 H9B 108.2 . . ?
N6 C10 C9 109.5(3) . . ?
N6 C10 H10A 109.8 . . ?
C9 C10 H10A 109.8 . . ?
N6 C10 H10B 109.8 . . ?
C9 C10 H10B 109.8 . . ?
H10A C10 H10B 108.2 . . ?
N5 C11 C12 113.0(3) . . ?
N5 C11 H11A 109.0 . . ?
C12 C11 H11A 109.0 . . ?
N5 C11 H11B 109.0 . . ?
C12 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
N7 C12 C11 111.4(3) . . ?
N7 C12 H12A 109.4 . . ?
C11 C12 H12A 109.4 . . ?
N7 C12 H12B 109.4 . . ?
C11 C12 H12B 109.4 . . ?
H12A C12 H12B 108.0 . . ?
N5 C13 C14 109.2(3) . . ?
N5 C13 H13A 109.8 . . ?
C14 C13 H13A 109.8 . . ?
N5 C13 H13B 109.8 . . ?
C14 C13 H13B 109.8 . . ?
H13A C13 H13B 108.3 . . ?
N8 C14 C13 111.1(3) . . ?
N8 C14 H14A 109.4 . . ?
C13 C14 H14A 109.4 . . ?
N8 C14 H14B 109.4 . . ?
C13 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?

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
N2 Ni1 Ni2 O1 -46.61(15) . . . . ?
N3 Ni1 Ni2 O1 169.33(14) . . . . ?
N1 Ni1 Ni2 O1 -15.34(12) . . . . ?
N4 Ni1 Ni2 O1 138.74(11) . . . . ?
N2 Ni1 Ni2 O4 -174.18(14) . . . . ?
N3 Ni1 Ni2 O4 41.76(14) . . . . ?
N1 Ni1 Ni2 O4 -142.91(12) . . . . ?
N4 Ni1 Ni2 O4 11.17(11) . . . . ?
N2 Ni1 Ni2 N7 9.53(16) . . . . ?
N3 Ni1 Ni2 N7 -134.53(15) . . . . ?
N1 Ni1 Ni2 N7 40.80(13) . . . . ?
N4 Ni1 Ni2 N7 -165.13(12) . . . . ?
N2 Ni1 Ni2 N6 -115.55(16) . . . . ?
N3 Ni1 Ni2 N6 100.39(15) . . . . ?
N1 Ni1 Ni2 N6 -84.28(13) . . . . ?
N4 Ni1 Ni2 N6 69.80(12) . . . . ?
N2 Ni1 Ni2 N5 130.11(16) . . . . ?
N3 Ni1 Ni2 N5 -13.96(16) . . . . ?
N1 Ni1 Ni2 N5 161.38(14) . . . . ?
N4 Ni1 Ni2 N5 -44.55(13) . . . . ?
N2 Ni1 Ni2 N8 82.74(15) . . . . ?
N3 Ni1 Ni2 N8 -61.32(14) . . . . ?
N1 Ni1 Ni2 N8 114.01(12) . . . . ?
N4 Ni1 Ni2 N8 -91.91(11) . . . . ?
O4 Ni2 O1 N1 60.48(19) . . . . ?
N7 Ni2 O1 N1 -117.9(2) . . . . ?
N6 Ni2 O1 N1 146.5(2) . . . . ?
N5 Ni2 O1 N1 -147.4(5) . . . . ?
N8 Ni2 O1 N1 -26.7(2) . . . . ?
Ni1 Ni2 O1 N1 19.80(15) . . . . ?
N7 Ni2 O1 O4 -178.36(9) . . . . ?
N6 Ni2 O1 O4 86.01(10) . . . . ?
N5 Ni2 O1 O4 152.1(5) . . . . ?
N8 Ni2 O1 O4 -87.14(9) . . . . ?
Ni1 Ni2 O1 O4 -40.68(8) . . . . ?
O1 Ni2 O4 N4 -55.21(19) . . . . ?
N7 Ni2 O4 N4 93.7(16) . . . . ?
N6 Ni2 O4 N4 -147.55(19) . . . . ?
N5 Ni2 O4 N4 129.69(19) . . . . ?
N8 Ni2 O4 N4 48.02(18) . . . . ?
Ni1 Ni2 O4 N4 -14.84(14) . . . . ?
N7 Ni2 O4 O1 148.9(16) . . . . ?
N6 Ni2 O4 O1 -92.34(11) . . . . ?
N5 Ni2 O4 O1 -175.10(10) . . . . ?
N8 Ni2 O4 O1 103.23(10) . . . . ?
Ni1 Ni2 O4 O1 40.37(8) . . . . ?
N1 O1 O4 N4 3.97(18) . . . . ?
Ni2 O1 O4 N4 132.63(16) . . . . ?
N1 O1 O4 Ni2 -128.66(17) . . . . ?
Ni2 O1 N1 C2 143.1(2) . . . . ?
O4 O1 N1 C2 -180.0(2) . . . . ?
Ni2 O1 N1 Ni1 -39.4(3) . . . . ?
O4 O1 N1 Ni1 -2.53(19) . . . . ?
N2 Ni1 N1 C2 -1.1(2) . . . . ?
N3 Ni1 N1 C2 5.2(6) . . . . ?
N4 Ni1 N1 C2 178.86(19) . . . . ?
Ni2 Ni1 N1 C2 -158.8(2) . . . . ?
N2 Ni1 N1 O1 -178.6(2) . . . . ?
N3 Ni1 N1 O1 -172.3(4) . . . . ?
N4 Ni1 N1 O1 1.3(2) . . . . ?
Ni2 Ni1 N1 O1 23.71(17) . . . . ?
N3 Ni1 N2 C3 -179.2(3) . . . . ?
N1 Ni1 N2 C3 -0.5(2) . . . . ?
N4 Ni1 N2 C3 179.6(5) . . . . ?
Ni2 Ni1 N2 C3 24.7(3) . . . . ?
N3 Ni1 N2 C4 6.1(3) . . . . ?
N1 Ni1 N2 C4 -175.2(3) . . . . ?
N4 Ni1 N2 C4 4.9(8) . . . . ?
Ni2 Ni1 N2 C4 -150.0(2) . . . . ?
N2 Ni1 N3 C6 173.4(2) . . . . ?
N1 Ni1 N3 C6 167.1(4) . . . . ?
N4 Ni1 N3 C6 -6.8(2) . . . . ?
Ni2 Ni1 N3 C6 -32.0(3) . . . . ?
N2 Ni1 N3 C5 10.9(2) . . . . ?
N1 Ni1 N3 C5 4.6(7) . . . . ?
N4 Ni1 N3 C5 -169.3(2) . . . . ?
Ni2 Ni1 N3 C5 165.53(17) . . . . ?
Ni2 O4 N4 C7 -150.20(19) . . . . ?
O1 O4 N4 C7 176.5(2) . . . . ?
Ni2 O4 N4 Ni1 29.5(3) . . . . ?
O1 O4 N4 Ni1 -3.90(19) . . . . ?
N2 Ni1 N4 C7 3.1(7) . . . . ?
N3 Ni1 N4 C7 1.98(19) . . . . ?
N1 Ni1 N4 C7 -176.71(18) . . . . ?
Ni2 Ni1 N4 C7 161.4(2) . . . . ?
N2 Ni1 N4 O4 -176.5(5) . . . . ?
N3 Ni1 N4 O4 -177.7(2) . . . . ?
N1 Ni1 N4 O4 3.6(2) . . . . ?
Ni2 Ni1 N4 O4 -18.31(17) . . . . ?
O1 Ni2 N5 C13 152.3(5) . . . . ?
O4 Ni2 N5 C13 -55.6(2) . . . . ?
N7 Ni2 N5 C13 122.5(2) . . . . ?
N6 Ni2 N5 C13 -140.8(2) . . . . ?
N8 Ni2 N5 C13 29.9(2) . . . . ?
Ni1 Ni2 N5 C13 -12.8(3) . . . . ?
O1 Ni2 N5 C9 -90.3(6) . . . . ?
O4 Ni2 N5 C9 61.7(2) . . . . ?
N7 Ni2 N5 C9 -120.1(2) . . . . ?
N6 Ni2 N5 C9 -23.5(2) . . . . ?
N8 Ni2 N5 C9 147.2(2) . . . . ?
Ni1 Ni2 N5 C9 104.6(2) . . . . ?
O1 Ni2 N5 C11 30.6(7) . . . . ?
O4 Ni2 N5 C11 -177.3(2) . . . . ?
N7 Ni2 N5 C11 0.8(2) . . . . ?
N6 Ni2 N5 C11 97.5(2) . . . . ?
N8 Ni2 N5 C11 -91.9(2) . . . . ?
Ni1 Ni2 N5 C11 -134.5(2) . . . . ?
O1 Ni2 N6 C10 166.1(2) . . . . ?
O4 Ni2 N6 C10 -99.7(2) . . . . ?
N7 Ni2 N6 C10 77.5(2) . . . . ?
N5 Ni2 N6 C10 -4.3(2) . . . . ?
N8 Ni2 N6 C10 -36.6(5) . . . . ?
Ni1 Ni2 N6 C10 -144.3(2) . . . . ?
O1 Ni2 N7 C12 163.6(2) . . . . ?
O4 Ni2 N7 C12 14.6(17) . . . . ?
N6 Ni2 N7 C12 -103.9(2) . . . . ?
N5 Ni2 N7 C12 -21.6(2) . . . . ?
N8 Ni2 N7 C12 60.2(2) . . . . ?
Ni1 Ni2 N7 C12 121.0(2) . . . . ?
O1 Ni2 N8 C14 -175.4(2) . . . . ?
O4 Ni2 N8 C14 91.1(2) . . . . ?
N7 Ni2 N8 C14 -86.7(2) . . . . ?
N6 Ni2 N8 C14 28.0(4) . . . . ?
N5 Ni2 N8 C14 -4.4(2) . . . . ?
Ni1 Ni2 N8 C14 144.3(2) . . . . ?
O1 N1 C2 C1 -1.8(4) . . . . ?
Ni1 N1 C2 C1 -179.5(3) . . . . ?
O1 N1 C2 C3 180.0(2) . . . . ?
Ni1 N1 C2 C3 2.3(3) . . . . ?
C4 N2 C3 O2 -2.6(5) . . . . ?
Ni1 N2 C3 O2 -177.0(3) . . . . ?
C4 N2 C3 C2 176.2(3) . . . . ?
Ni1 N2 C3 C2 1.8(3) . . . . ?
N1 C2 C3 O2 176.2(3) . . . . ?
C1 C2 C3 O2 -2.0(5) . . . . ?
N1 C2 C3 N2 -2.6(4) . . . . ?
C1 C2 C3 N2 179.2(3) . . . . ?
C3 N2 C4 C5 165.6(3) . . . . ?
Ni1 N2 C4 C5 -20.0(4) . . . . ?
C6 N3 C5 C4 175.5(3) . . . . ?
Ni1 N3 C5 C4 -23.5(3) . . . . ?
N2 C4 C5 N3 25.7(4) . . . . ?
C5 N3 C6 O3 -7.8(5) . . . . ?
Ni1 N3 C6 O3 -168.8(2) . . . . ?
C5 N3 C6 C7 170.4(3) . . . . ?
Ni1 N3 C6 C7 9.4(3) . . . . ?
O4 N4 C7 C8 2.4(4) . . . . ?
Ni1 N4 C7 C8 -177.3(2) . . . . ?
O4 N4 C7 C6 -177.8(2) . . . . ?
Ni1 N4 C7 C6 2.5(3) . . . . ?
O3 C6 C7 N4 170.7(3) . . . . ?
N3 C6 C7 N4 -7.6(3) . . . . ?
O3 C6 C7 C8 -9.6(4) . . . . ?
N3 C6 C7 C8 172.1(3) . . . . ?
C13 N5 C9 C10 160.4(3) . . . . ?
C11 N5 C9 C10 -71.4(4) . . . . ?
Ni2 N5 C9 C10 48.0(3) . . . . ?
Ni2 N6 C10 C9 31.4(3) . . . . ?
N5 C9 C10 N6 -55.0(4) . . . . ?
C13 N5 C11 C12 -97.2(4) . . . . ?
C9 N5 C11 C12 135.3(3) . . . . ?
Ni2 N5 C11 C12 19.5(4) . . . . ?
Ni2 N7 C12 C11 38.1(4) . . . . ?
N5 C11 C12 N7 -38.8(4) . . . . ?
C9 N5 C13 C14 -162.4(3) . . . . ?
C11 N5 C13 C14 69.6(3) . . . . ?
Ni2 N5 C13 C14 -50.3(3) . . . . ?
Ni2 N8 C14 C13 -21.9(3) . . . . ?
N5 C13 C14 N8 49.5(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.917
_diffrn_reflns_theta_full        28.99
_diffrn_measured_fraction_theta_full 0.917
_refine_diff_density_max         0.928
_refine_diff_density_min         -0.869
_refine_diff_density_rms         0.095

data_6
_database_code_depnum_ccdc_archive 'CCDC 263431'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
(tris(2-aminoethyl)amine)-cobalt(III)(N,N'-bis(2-Hydroxyiminopropionyl)
ethane-1,2-diamine)-nickel(II) perchlorate monohydrate
;
_chemical_name_common            
;
(tris(2-aminoethyl)amine)-cobalt(iii)(N,N'-bis(2-
Hydroxyiminopropionyl) ethane-1,2-diamine)-nickel(ii) perchlorate
monohydrate
;
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H30 Cl Co N8 Ni O9'
_chemical_formula_weight         607.55

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   7.979(2)
_cell_length_b                   11.528(2)
_cell_length_c                   12.454(2)
_cell_angle_alpha                85.93(3)
_cell_angle_beta                 81.40(3)
_cell_angle_gamma                80.95(3)
_cell_volume                     1117.2(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             628
_exptl_absorpt_coefficient_mu    1.770
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5822
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.66
_diffrn_reflns_theta_max         32.10
_reflns_number_total             5822
_reflns_number_gt                5235
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
;
Refinement of 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^)+(0.0358P)^2^+0.8643P] 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         5822
_refine_ls_number_parameters     317
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0282
_refine_ls_wR_factor_ref         0.0746
_refine_ls_wR_factor_gt          0.0716
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.053
_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 0.21124(2) 0.216314(16) 0.46535(2) 0.01206(7) Uani 1 1 d . . .
Co1 Co 0.26484(2) 0.249024(17) 0.73378(2) 0.01031(7) Uani 1 1 d . . .
Cl1 Cl 0.33665(5) 0.70409(3) -0.12578(4) 0.01735(10) Uani 1 1 d . . .
O1 O 0.33018(15) 0.35222(10) 0.61358(11) 0.0163(3) Uani 1 1 d . . .
O2 O 0.13186(16) 0.50994(10) 0.28967(12) 0.0190(3) Uani 1 1 d . . .
O3 O 0.20804(15) -0.10108(10) 0.37691(11) 0.0168(3) Uani 1 1 d . . .
O4 O 0.32042(14) 0.10215(10) 0.66344(11) 0.0143(3) Uani 1 1 d . . .
O5 O 0.35273(18) 0.65880(12) -0.23122(13) 0.0245(3) Uani 1 1 d . . .
O6 O 0.27120(19) 0.61889(12) -0.04473(13) 0.0282(3) Uani 1 1 d . . .
O7 O 0.21558(19) 0.81216(12) -0.11841(14) 0.0303(4) Uani 1 1 d . . .
O8 O 0.50018(19) 0.72581(17) -0.10380(15) 0.0386(4) Uani 1 1 d . . .
O1W O 0.42049(17) 0.57909(11) 0.15370(16) 0.0227(3) Uani 1 1 d . . .
N1 N 0.25805(16) 0.35084(12) 0.52278(13) 0.0138(3) Uani 1 1 d . . .
N2 N 0.15104(18) 0.31643(12) 0.35337(14) 0.0162(3) Uani 1 1 d . . .
N3 N 0.16831(18) 0.10137(12) 0.38482(14) 0.0156(3) Uani 1 1 d . . .
N4 N 0.26617(16) 0.09368(11) 0.56694(13) 0.0122(3) Uani 1 1 d . . .
N5 N 0.20778(15) 0.16402(11) 0.87285(13) 0.0114(3) Uani 1 1 d . . .
N6 N 0.50187(16) 0.21528(11) 0.76279(13) 0.0130(3) Uani 1 1 d . . .
H6A H 0.5689 0.1838 0.7042 0.016 Uiso 1 1 calc R . .
H6B H 0.5380 0.2828 0.7745 0.016 Uiso 1 1 calc R . .
N7 N 0.21674(17) 0.39272(11) 0.81387(13) 0.0152(3) Uani 1 1 d . . .
H7A H 0.3161 0.4171 0.8210 0.018 Uiso 1 1 calc R . .
H7B H 0.1557 0.4495 0.7763 0.018 Uiso 1 1 calc R . .
N8 N 0.02374(16) 0.25638(11) 0.71475(13) 0.0131(3) Uani 1 1 d . . .
H8A H -0.0240 0.3319 0.7060 0.016 Uiso 1 1 calc R . .
H8B H 0.0170 0.2193 0.6547 0.016 Uiso 1 1 calc R . .
C1 C 0.2727(2) 0.56448(15) 0.48715(18) 0.0187(4) Uani 1 1 d . . .
H1A H 0.2849 0.5638 0.5627 0.028 Uiso 1 1 calc R . .
H1B H 0.1802 0.6244 0.4717 0.028 Uiso 1 1 calc R . .
H1C H 0.3771 0.5805 0.4436 0.028 Uiso 1 1 calc R . .
C2 C 0.23541(19) 0.44802(14) 0.46142(16) 0.0154(4) Uani 1 1 d . . .
C3 C 0.16719(19) 0.42750(13) 0.35936(16) 0.0155(4) Uani 1 1 d . . .
C4 C 0.0837(2) 0.26852(15) 0.26639(17) 0.0197(4) Uani 1 1 d . . .
H4A H 0.1265 0.3033 0.1964 0.024 Uiso 1 1 calc R . .
H4B H -0.0405 0.2845 0.2767 0.024 Uiso 1 1 calc R . .
C5 C 0.1453(2) 0.13542(15) 0.27162(17) 0.0194(4) Uani 1 1 d . . .
H5A H 0.0611 0.0936 0.2490 0.023 Uiso 1 1 calc R . .
H5B H 0.2527 0.1168 0.2240 0.023 Uiso 1 1 calc R . .
C6 C 0.20853(18) -0.00831(13) 0.42343(16) 0.0133(4) Uani 1 1 d . . .
C7 C 0.26246(19) -0.01080(13) 0.53457(16) 0.0133(4) Uani 1 1 d . . .
C8 C 0.3135(2) -0.12195(14) 0.59700(17) 0.0188(4) Uani 1 1 d . . .
H8C H 0.4345 -0.1323 0.5997 0.028 Uiso 1 1 calc R . .
H8D H 0.2861 -0.1868 0.5621 0.028 Uiso 1 1 calc R . .
H8E H 0.2527 -0.1186 0.6696 0.028 Uiso 1 1 calc R . .
C9 C 0.35967(18) 0.07304(13) 0.88668(16) 0.0142(4) Uani 1 1 d . . .
H9A H 0.3653 0.0096 0.8385 0.017 Uiso 1 1 calc R . .
H9B H 0.3508 0.0405 0.9609 0.017 Uiso 1 1 calc R . .
C10 C 0.51911(18) 0.13210(14) 0.85957(16) 0.0153(4) Uani 1 1 d . . .
H10A H 0.5337 0.1746 0.9212 0.018 Uiso 1 1 calc R . .
H10B H 0.6193 0.0731 0.8441 0.018 Uiso 1 1 calc R . .
C11 C 0.1753(2) 0.24744(14) 0.96373(16) 0.0154(4) Uani 1 1 d . . .
H11A H 0.2789 0.2438 0.9966 0.018 Uiso 1 1 calc R . .
H11B H 0.0865 0.2238 1.0191 0.018 Uiso 1 1 calc R . .
C12 C 0.1201(2) 0.37320(15) 0.92230(18) 0.0199(4) Uani 1 1 d . . .
H12A H -0.0019 0.3858 0.9180 0.024 Uiso 1 1 calc R . .
H12B H 0.1426 0.4282 0.9719 0.024 Uiso 1 1 calc R . .
C13 C 0.05384(19) 0.10904(14) 0.86347(16) 0.0148(4) Uani 1 1 d . . .
H13A H 0.0019 0.0835 0.9349 0.018 Uiso 1 1 calc R . .
H13B H 0.0863 0.0410 0.8192 0.018 Uiso 1 1 calc R . .
C14 C -0.07179(18) 0.19984(14) 0.81147(16) 0.0151(4) Uani 1 1 d . . .
H14A H -0.1612 0.1625 0.7894 0.018 Uiso 1 1 calc R . .
H14B H -0.1249 0.2586 0.8630 0.018 Uiso 1 1 calc R . .
H1W1 H 0.353(3) 0.543(2) 0.194(2) 0.022(6) Uiso 1 1 d . . .
H2W1 H 0.392(5) 0.578(3) 0.092(3) 0.066(12) 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 0.01594(9) 0.00837(9) 0.01231(17) -0.00194(7) -0.00338(8) -0.00117(6)
Co1 0.01164(8) 0.00833(9) 0.01063(17) -0.00046(8) -0.00209(8) 0.00005(6)
Cl1 0.01858(15) 0.01734(17) 0.0169(3) -0.00079(15) -0.00264(15) -0.00491(12)
O1 0.0200(5) 0.0159(5) 0.0144(9) 0.0013(5) -0.0054(5) -0.0052(4)
O2 0.0274(6) 0.0118(5) 0.0167(9) 0.0017(5) -0.0047(5) 0.0009(4)
O3 0.0214(5) 0.0123(5) 0.0172(9) -0.0063(5) -0.0019(5) -0.0022(4)
O4 0.0190(5) 0.0119(5) 0.0126(9) -0.0029(4) -0.0072(5) 0.0015(4)
O5 0.0347(7) 0.0225(6) 0.0165(10) -0.0033(6) -0.0079(6) 0.0001(5)
O6 0.0352(7) 0.0244(7) 0.0230(10) 0.0055(6) 0.0023(6) -0.0071(5)
O7 0.0362(7) 0.0163(6) 0.0352(11) -0.0033(6) 0.0004(6) 0.0011(5)
O8 0.0240(6) 0.0611(11) 0.0368(12) -0.0132(9) -0.0065(6) -0.0184(7)
O1W 0.0222(6) 0.0174(6) 0.0300(11) -0.0010(6) -0.0060(6) -0.0049(4)
N1 0.0157(5) 0.0139(6) 0.0119(10) -0.0015(5) -0.0024(5) -0.0014(4)
N2 0.0233(6) 0.0120(6) 0.0133(10) -0.0004(5) -0.0046(6) -0.0008(5)
N3 0.0229(6) 0.0117(6) 0.0131(11) -0.0018(5) -0.0059(6) -0.0017(5)
N4 0.0134(5) 0.0131(6) 0.0103(10) -0.0029(5) -0.0028(5) -0.0001(4)
N5 0.0117(5) 0.0112(5) 0.0114(10) -0.0005(5) -0.0031(5) -0.0011(4)
N6 0.0133(5) 0.0109(5) 0.0143(10) -0.0011(5) -0.0011(5) -0.0013(4)
N7 0.0176(5) 0.0108(6) 0.0170(10) -0.0019(5) -0.0020(5) -0.0013(4)
N8 0.0150(5) 0.0118(6) 0.0124(10) -0.0015(5) -0.0042(5) 0.0005(4)
C1 0.0238(7) 0.0153(7) 0.0185(13) -0.0009(6) -0.0057(7) -0.0051(5)
C2 0.0160(6) 0.0136(7) 0.0150(12) 0.0014(6) -0.0002(6) -0.0005(5)
C3 0.0175(6) 0.0118(6) 0.0155(12) -0.0005(6) 0.0002(6) 0.0009(5)
C4 0.0298(8) 0.0155(7) 0.0142(13) -0.0013(6) -0.0078(7) 0.0004(6)
C5 0.0290(8) 0.0149(7) 0.0147(13) -0.0032(6) -0.0063(7) 0.0002(6)
C6 0.0138(6) 0.0126(6) 0.0133(12) -0.0029(6) -0.0002(6) -0.0018(5)
C7 0.0147(6) 0.0112(6) 0.0133(12) -0.0020(6) -0.0001(6) -0.0004(5)
C8 0.0256(7) 0.0118(7) 0.0180(13) 0.0005(6) -0.0040(7) 0.0005(5)
C9 0.0132(6) 0.0132(6) 0.0156(12) 0.0027(6) -0.0040(6) -0.0001(5)
C10 0.0126(6) 0.0172(7) 0.0161(12) 0.0011(6) -0.0041(6) -0.0010(5)
C11 0.0174(6) 0.0183(7) 0.0109(12) -0.0039(6) -0.0029(6) -0.0018(5)
C12 0.0199(7) 0.0163(7) 0.0235(13) -0.0069(7) -0.0004(7) -0.0022(5)
C13 0.0146(6) 0.0139(7) 0.0172(12) 0.0008(6) -0.0037(6) -0.0052(5)
C14 0.0122(6) 0.0155(7) 0.0183(12) -0.0009(6) -0.0036(6) -0.0022(5)

_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 1.8180(17) . ?
Ni1 N3 1.8201(16) . ?
Ni1 N1 1.8644(15) . ?
Ni1 N4 1.8731(16) . ?
Ni1 Co1 3.4869(7) . ?
Co1 O1 1.9070(14) . ?
Co1 O4 1.9207(13) . ?
Co1 N7 1.9510(15) . ?
Co1 N6 1.9524(14) . ?
Co1 N5 1.9573(16) . ?
Co1 N8 1.9612(14) . ?
Cl1 O5 1.4281(17) . ?
Cl1 O8 1.4351(15) . ?
Cl1 O7 1.4507(15) . ?
Cl1 O6 1.4558(15) . ?
O1 N1 1.345(2) . ?
O1 O4 2.9162(17) . ?
O2 C3 1.268(2) . ?
O3 C6 1.253(2) . ?
O4 N4 1.352(2) . ?
N1 C2 1.314(2) . ?
N2 C3 1.315(2) . ?
N2 C4 1.456(3) . ?
N3 C6 1.329(2) . ?
N3 C5 1.467(3) . ?
N4 C7 1.303(2) . ?
N5 C13 1.4908(19) . ?
N5 C9 1.4951(19) . ?
N5 C11 1.504(2) . ?
N6 C10 1.495(2) . ?
N7 C12 1.473(3) . ?
N8 C14 1.492(2) . ?
C1 C2 1.486(2) . ?
C2 C3 1.503(3) . ?
C4 C5 1.536(2) . ?
C6 C7 1.507(3) . ?
C7 C8 1.484(2) . ?
C9 C10 1.519(2) . ?
C11 C12 1.524(2) . ?
C13 C14 1.513(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
N2 Ni1 N3 85.42(7) . . ?
N2 Ni1 N1 84.25(7) . . ?
N3 Ni1 N1 169.08(7) . . ?
N2 Ni1 N4 170.54(7) . . ?
N3 Ni1 N4 85.12(7) . . ?
N1 Ni1 N4 105.19(7) . . ?
N2 Ni1 Co1 134.92(5) . . ?
N3 Ni1 Co1 137.57(5) . . ?
N1 Ni1 Co1 53.33(5) . . ?
N4 Ni1 Co1 54.28(5) . . ?
O1 Co1 O4 99.26(6) . . ?
O1 Co1 N7 83.62(6) . . ?
O4 Co1 N7 175.86(6) . . ?
O1 Co1 N6 90.29(6) . . ?
O4 Co1 N6 83.77(6) . . ?
N7 Co1 N6 93.27(7) . . ?
O1 Co1 N5 169.84(6) . . ?
O4 Co1 N5 89.69(6) . . ?
N7 Co1 N5 87.20(6) . . ?
N6 Co1 N5 85.88(6) . . ?
O1 Co1 N8 97.95(6) . . ?
O4 Co1 N8 90.17(6) . . ?
N7 Co1 N8 92.38(6) . . ?
N6 Co1 N8 170.48(6) . . ?
N5 Co1 N8 86.75(6) . . ?
O1 Co1 Ni1 54.99(4) . . ?
O4 Co1 Ni1 56.21(5) . . ?
N7 Co1 Ni1 127.86(5) . . ?
N6 Co1 Ni1 114.67(6) . . ?
N5 Co1 Ni1 135.05(4) . . ?
N8 Co1 Ni1 67.16(6) . . ?
O5 Cl1 O8 110.25(10) . . ?
O5 Cl1 O7 110.30(10) . . ?
O8 Cl1 O7 109.69(10) . . ?
O5 Cl1 O6 109.11(9) . . ?
O8 Cl1 O6 109.54(11) . . ?
O7 Cl1 O6 107.91(9) . . ?
N1 O1 Co1 118.18(9) . . ?
N1 O1 O4 92.34(9) . . ?
Co1 O1 O4 40.55(4) . . ?
N4 O4 Co1 119.09(9) . . ?
N4 O4 O1 89.73(9) . . ?
Co1 O4 O1 40.20(4) . . ?
C2 N1 O1 118.98(14) . . ?
C2 N1 Ni1 115.52(13) . . ?
O1 N1 Ni1 125.03(11) . . ?
C3 N2 C4 125.24(16) . . ?
C3 N2 Ni1 117.00(14) . . ?
C4 N2 Ni1 117.72(11) . . ?
C6 N3 C5 125.00(16) . . ?
C6 N3 Ni1 115.91(13) . . ?
C5 N3 Ni1 116.18(11) . . ?
C7 N4 O4 118.28(14) . . ?
C7 N4 Ni1 114.28(13) . . ?
O4 N4 Ni1 127.23(10) . . ?
C13 N5 C9 111.42(12) . . ?
C13 N5 C11 112.17(13) . . ?
C9 N5 C11 110.18(14) . . ?
C13 N5 Co1 106.58(11) . . ?
C9 N5 Co1 106.35(11) . . ?
C11 N5 Co1 109.91(10) . . ?
C10 N6 Co1 111.41(10) . . ?
C12 N7 Co1 111.07(10) . . ?
C14 N8 Co1 110.22(11) . . ?
N1 C2 C1 125.33(18) . . ?
N1 C2 C3 111.49(15) . . ?
C1 C2 C3 123.18(15) . . ?
O2 C3 N2 126.18(18) . . ?
O2 C3 C2 122.15(15) . . ?
N2 C3 C2 111.67(16) . . ?
N2 C4 C5 106.39(15) . . ?
N3 C5 C4 107.03(16) . . ?
O3 C6 N3 127.22(18) . . ?
O3 C6 C7 121.53(15) . . ?
N3 C6 C7 111.24(15) . . ?
N4 C7 C8 124.29(17) . . ?
N4 C7 C6 113.00(15) . . ?
C8 C7 C6 122.66(15) . . ?
N5 C9 C10 107.81(12) . . ?
N6 C10 C9 109.51(13) . . ?
N5 C11 C12 111.10(16) . . ?
N7 C12 C11 108.87(14) . . ?
N5 C13 C14 108.03(12) . . ?
N8 C14 C13 108.29(13) . . ?

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
N2 Ni1 Co1 O1 -38.71(8) . . . . ?
N3 Ni1 Co1 O1 163.78(8) . . . . ?
N1 Ni1 Co1 O1 -15.44(7) . . . . ?
N4 Ni1 Co1 O1 144.23(7) . . . . ?
N2 Ni1 Co1 O4 -173.54(8) . . . . ?
N3 Ni1 Co1 O4 28.95(8) . . . . ?
N1 Ni1 Co1 O4 -150.26(7) . . . . ?
N4 Ni1 Co1 O4 9.40(6) . . . . ?
N2 Ni1 Co1 N7 5.53(8) . . . . ?
N3 Ni1 Co1 N7 -151.97(8) . . . . ?
N1 Ni1 Co1 N7 28.81(7) . . . . ?
N4 Ni1 Co1 N7 -171.53(7) . . . . ?
N2 Ni1 Co1 N6 -110.36(8) . . . . ?
N3 Ni1 Co1 N6 92.13(8) . . . . ?
N1 Ni1 Co1 N6 -87.08(7) . . . . ?
N4 Ni1 Co1 N6 72.58(7) . . . . ?
N2 Ni1 Co1 N5 139.26(8) . . . . ?
N3 Ni1 Co1 N5 -18.25(8) . . . . ?
N1 Ni1 Co1 N5 162.54(7) . . . . ?
N4 Ni1 Co1 N5 -37.80(7) . . . . ?
N2 Ni1 Co1 N8 79.85(8) . . . . ?
N3 Ni1 Co1 N8 -77.65(8) . . . . ?
N1 Ni1 Co1 N8 103.13(7) . . . . ?
N4 Ni1 Co1 N8 -97.21(7) . . . . ?
O4 Co1 O1 N1 56.28(11) . . . . ?
N7 Co1 O1 N1 -126.73(11) . . . . ?
N6 Co1 O1 N1 140.02(11) . . . . ?
N5 Co1 O1 N1 -152.2(3) . . . . ?
N8 Co1 O1 N1 -35.20(11) . . . . ?
Ni1 Co1 O1 N1 19.61(8) . . . . ?
N7 Co1 O1 O4 176.99(5) . . . . ?
N6 Co1 O1 O4 83.73(6) . . . . ?
N5 Co1 O1 O4 151.5(3) . . . . ?
N8 Co1 O1 O4 -91.48(6) . . . . ?
Ni1 Co1 O1 O4 -36.67(5) . . . . ?
O1 Co1 O4 N4 -48.19(11) . . . . ?
N7 Co1 O4 N4 178.0(7) . . . . ?
N6 Co1 O4 N4 -137.47(11) . . . . ?
N5 Co1 O4 N4 136.64(11) . . . . ?
N8 Co1 O4 N4 49.89(11) . . . . ?
Ni1 Co1 O4 N4 -12.14(8) . . . . ?
N7 Co1 O4 O1 -133.8(8) . . . . ?
N6 Co1 O4 O1 -89.28(6) . . . . ?
N5 Co1 O4 O1 -175.17(5) . . . . ?
N8 Co1 O4 O1 98.08(6) . . . . ?
Ni1 Co1 O4 O1 36.06(5) . . . . ?
N1 O1 O4 N4 6.56(11) . . . . ?
Co1 O1 O4 N4 139.35(9) . . . . ?
N1 O1 O4 Co1 -132.79(10) . . . . ?
Co1 O1 N1 C2 149.44(12) . . . . ?
O4 O1 N1 C2 -177.80(13) . . . . ?
Co1 O1 N1 Ni1 -38.89(15) . . . . ?
O4 O1 N1 Ni1 -6.13(11) . . . . ?
N2 Ni1 N1 C2 -2.24(12) . . . . ?
N3 Ni1 N1 C2 16.9(4) . . . . ?
N4 Ni1 N1 C2 177.10(11) . . . . ?
Co1 Ni1 N1 C2 -165.90(14) . . . . ?
N2 Ni1 N1 O1 -174.17(13) . . . . ?
N3 Ni1 N1 O1 -155.0(3) . . . . ?
N4 Ni1 N1 O1 5.17(13) . . . . ?
Co1 Ni1 N1 O1 22.17(10) . . . . ?
N3 Ni1 N2 C3 -175.43(13) . . . . ?
N1 Ni1 N2 C3 0.99(13) . . . . ?
N4 Ni1 N2 C3 -175.1(3) . . . . ?
Co1 Ni1 N2 C3 19.57(16) . . . . ?
N3 Ni1 N2 C4 6.57(13) . . . . ?
N1 Ni1 N2 C4 -177.01(13) . . . . ?
N4 Ni1 N2 C4 6.9(4) . . . . ?
Co1 Ni1 N2 C4 -158.43(10) . . . . ?
N2 Ni1 N3 C6 173.42(13) . . . . ?
N1 Ni1 N3 C6 154.3(3) . . . . ?
N4 Ni1 N3 C6 -6.52(12) . . . . ?
Co1 Ni1 N3 C6 -22.35(16) . . . . ?
N2 Ni1 N3 C5 11.72(12) . . . . ?
N1 Ni1 N3 C5 -7.4(4) . . . . ?
N4 Ni1 N3 C5 -168.23(12) . . . . ?
Co1 Ni1 N3 C5 175.95(9) . . . . ?
Co1 O4 N4 C7 -161.58(11) . . . . ?
O1 O4 N4 C7 169.66(12) . . . . ?
Co1 O4 N4 Ni1 24.11(16) . . . . ?
O1 O4 N4 Ni1 -4.64(11) . . . . ?
N2 Ni1 N4 C7 4.2(4) . . . . ?
N3 Ni1 N4 C7 4.58(11) . . . . ?
N1 Ni1 N4 C7 -171.73(11) . . . . ?
Co1 Ni1 N4 C7 171.48(13) . . . . ?
N2 Ni1 N4 O4 178.7(3) . . . . ?
N3 Ni1 N4 O4 179.08(12) . . . . ?
N1 Ni1 N4 O4 2.77(13) . . . . ?
Co1 Ni1 N4 O4 -14.02(9) . . . . ?
O1 Co1 N5 C13 142.1(3) . . . . ?
O4 Co1 N5 C13 -66.00(10) . . . . ?
N7 Co1 N5 C13 116.74(10) . . . . ?
N6 Co1 N5 C13 -149.78(10) . . . . ?
N8 Co1 N5 C13 24.19(10) . . . . ?
Ni1 Co1 N5 C13 -28.43(12) . . . . ?
O1 Co1 N5 C9 -98.9(3) . . . . ?
O4 Co1 N5 C9 52.97(10) . . . . ?
N7 Co1 N5 C9 -124.29(11) . . . . ?
N6 Co1 N5 C9 -30.80(10) . . . . ?
N8 Co1 N5 C9 143.16(11) . . . . ?
Ni1 Co1 N5 C9 90.55(10) . . . . ?
O1 Co1 N5 C11 20.3(3) . . . . ?
O4 Co1 N5 C11 172.22(9) . . . . ?
N7 Co1 N5 C11 -5.03(10) . . . . ?
N6 Co1 N5 C11 88.45(10) . . . . ?
N8 Co1 N5 C11 -97.58(10) . . . . ?
Ni1 Co1 N5 C11 -150.20(8) . . . . ?
O1 Co1 N6 C10 179.12(11) . . . . ?
O4 Co1 N6 C10 -81.60(12) . . . . ?
N7 Co1 N6 C10 95.49(12) . . . . ?
N5 Co1 N6 C10 8.54(11) . . . . ?
N8 Co1 N6 C10 -30.9(5) . . . . ?
Ni1 Co1 N6 C10 -129.86(10) . . . . ?
O1 Co1 N7 C12 168.29(12) . . . . ?
O4 Co1 N7 C12 -57.5(8) . . . . ?
N6 Co1 N7 C12 -101.78(12) . . . . ?
N5 Co1 N7 C12 -16.07(11) . . . . ?
N8 Co1 N7 C12 70.56(12) . . . . ?
Ni1 Co1 N7 C12 133.19(10) . . . . ?
O1 Co1 N8 C14 -169.49(10) . . . . ?
O4 Co1 N8 C14 91.14(11) . . . . ?
N7 Co1 N8 C14 -85.60(11) . . . . ?
N6 Co1 N8 C14 40.8(4) . . . . ?
N5 Co1 N8 C14 1.46(11) . . . . ?
Ni1 Co1 N8 C14 143.93(11) . . . . ?
O1 N1 C2 C1 -4.3(2) . . . . ?
Ni1 N1 C2 C1 -176.71(13) . . . . ?
O1 N1 C2 C3 175.28(12) . . . . ?
Ni1 N1 C2 C3 2.83(17) . . . . ?
C4 N2 C3 O2 -2.1(3) . . . . ?
Ni1 N2 C3 O2 -179.96(13) . . . . ?
C4 N2 C3 C2 178.10(15) . . . . ?
Ni1 N2 C3 C2 0.27(18) . . . . ?
N1 C2 C3 O2 178.21(15) . . . . ?
C1 C2 C3 O2 -2.2(2) . . . . ?
N1 C2 C3 N2 -2.01(19) . . . . ?
C1 C2 C3 N2 177.55(15) . . . . ?
C3 N2 C4 C5 160.88(16) . . . . ?
Ni1 N2 C4 C5 -21.30(19) . . . . ?
C6 N3 C5 C4 174.81(15) . . . . ?
Ni1 N3 C5 C4 -25.36(18) . . . . ?
N2 C4 C5 N3 27.57(19) . . . . ?
C5 N3 C6 O3 -11.8(3) . . . . ?
Ni1 N3 C6 O3 -171.69(13) . . . . ?
C5 N3 C6 C7 166.71(15) . . . . ?
Ni1 N3 C6 C7 6.83(17) . . . . ?
O4 N4 C7 C8 0.2(2) . . . . ?
Ni1 N4 C7 C8 175.27(12) . . . . ?
O4 N4 C7 C6 -176.99(12) . . . . ?
Ni1 N4 C7 C6 -1.96(16) . . . . ?
O3 C6 C7 N4 175.58(14) . . . . ?
N3 C6 C7 N4 -3.03(19) . . . . ?
O3 C6 C7 C8 -1.7(2) . . . . ?
N3 C6 C7 C8 179.68(14) . . . . ?
C13 N5 C9 C10 162.18(15) . . . . ?
C11 N5 C9 C10 -72.65(18) . . . . ?
Co1 N5 C9 C10 46.43(16) . . . . ?
Co1 N6 C10 C9 15.71(17) . . . . ?
N5 C9 C10 N6 -40.60(19) . . . . ?
C13 N5 C11 C12 -93.83(16) . . . . ?
C9 N5 C11 C12 141.42(13) . . . . ?
Co1 N5 C11 C12 24.54(14) . . . . ?
Co1 N7 C12 C11 32.87(16) . . . . ?
N5 C11 C12 N7 -37.39(18) . . . . ?
C9 N5 C13 C14 -160.40(15) . . . . ?
C11 N5 C13 C14 75.54(18) . . . . ?
Co1 N5 C13 C14 -44.79(16) . . . . ?
Co1 N8 C14 C13 -26.64(16) . . . . ?
N5 C13 C14 N8 47.00(19) . . . . ?

_diffrn_measured_fraction_theta_max 0.744
_diffrn_reflns_theta_full        32.10
_diffrn_measured_fraction_theta_full 0.744
_refine_diff_density_max         0.960
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.077

data_2a
_database_code_depnum_ccdc_archive 'CCDC 263432'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
tetraphenylphosphonium (N,N'-bis(2-Hydroxyiminopropionyl)propane-1,3-diamine)
-nickelate(II) monohydrate
;
_chemical_name_common            
;
tetraphenylphosphonium (N,N'-bis(2-
Hydroxyiminopropionyl)propane-1,3-diamine) -nickelate(ii) monohydrate
;
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H35 N4 Ni O5 P'
_chemical_formula_weight         657.33

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/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                   10.812(2)
_cell_length_b                   21.043(4)
_cell_length_c                   14.031(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.89(3)
_cell_angle_gamma                90.00
_cell_volume                     3001.9(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1376
_exptl_absorpt_coefficient_mu    0.749
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20588
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.50
_diffrn_reflns_theta_max         28.59
_reflns_number_total             7014
_reflns_number_gt                5810
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
;
Refinement of 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^)+(0.0416P)^2^+0.0000P] 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         7014
_refine_ls_number_parameters     537
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0355
_refine_ls_wR_factor_ref         0.0818
_refine_ls_wR_factor_gt          0.0765
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_restrained_S_all      1.090
_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 0.03351(2) 0.289013(10) 0.186471(16) 0.01158(7) Uani 1 1 d . . .
P1 P 0.16296(5) 0.51282(2) 0.38012(3) 0.01289(10) Uani 1 1 d . . .
O1 O -0.09630(13) 0.20726(6) 0.28598(10) 0.0177(3) Uani 1 1 d . . .
O2 O -0.32385(12) 0.33450(6) 0.00984(9) 0.0189(3) Uani 1 1 d . . .
O3 O 0.40236(12) 0.31569(6) 0.20438(10) 0.0192(3) Uani 1 1 d . . .
O4 O 0.14240(13) 0.20076(6) 0.34845(10) 0.0183(3) Uani 1 1 d . . .
O1W O -0.52889(15) 0.39475(7) 0.05298(13) 0.0265(3) Uani 1 1 d . . .
N1 N -0.10951(15) 0.25107(7) 0.21183(11) 0.0136(3) Uani 1 1 d . . .
N2 N -0.09788(14) 0.33331(7) 0.08725(11) 0.0140(3) Uani 1 1 d . . .
N3 N 0.17595(14) 0.32579(7) 0.16023(11) 0.0132(3) Uani 1 1 d . . .
N4 N 0.16569(15) 0.24309(7) 0.28343(11) 0.0144(3) Uani 1 1 d . . .
C1 C -0.3519(2) 0.24158(10) 0.15713(17) 0.0203(4) Uani 1 1 d . . .
C2 C -0.22531(17) 0.26699(8) 0.15324(13) 0.0140(4) Uani 1 1 d . . .
C3 C -0.22024(17) 0.31550(8) 0.07551(13) 0.0138(4) Uani 1 1 d . . .
C4 C -0.08078(18) 0.38151(9) 0.01770(14) 0.0152(4) Uani 1 1 d . . .
C9 C 0.04991(18) 0.41563(9) 0.06198(14) 0.0151(4) Uani 1 1 d . . .
C5 C 0.16827(18) 0.37276(8) 0.08125(14) 0.0146(4) Uani 1 1 d . . .
C6 C 0.29344(18) 0.30187(8) 0.21240(13) 0.0140(4) Uani 1 1 d . . .
C7 C 0.28543(17) 0.25249(8) 0.28745(13) 0.0146(4) Uani 1 1 d . . .
C8 C 0.4017(2) 0.21812(10) 0.35603(16) 0.0200(4) Uani 1 1 d . . .
C11 C 0.21063(17) 0.44598(8) 0.46510(13) 0.0141(4) Uani 1 1 d . . .
C12 C 0.20562(19) 0.38440(9) 0.42570(14) 0.0172(4) Uani 1 1 d . . .
C13 C 0.25188(19) 0.33359(9) 0.49101(15) 0.0196(4) Uani 1 1 d . . .
C14 C 0.3041(2) 0.34366(9) 0.59504(15) 0.0204(4) Uani 1 1 d . . .
C15 C 0.30527(19) 0.40419(9) 0.63455(14) 0.0191(4) Uani 1 1 d . . .
C16 C 0.25909(18) 0.45556(9) 0.57004(14) 0.0164(4) Uani 1 1 d . . .
C21 C 0.27400(17) 0.51856(8) 0.30941(13) 0.0143(4) Uani 1 1 d . . .
C22 C 0.26992(18) 0.57440(9) 0.25379(14) 0.0174(4) Uani 1 1 d . . .
C23 C 0.34504(18) 0.57916(10) 0.19128(14) 0.0195(4) Uani 1 1 d . . .
C24 C 0.42438(19) 0.52892(10) 0.18424(15) 0.0208(4) Uani 1 1 d . . .
C25 C 0.43241(19) 0.47472(10) 0.24174(15) 0.0219(4) Uani 1 1 d . . .
C26 C 0.35732(18) 0.46909(9) 0.30413(14) 0.0183(4) Uani 1 1 d . . .
C31 C -0.00320(17) 0.50286(8) 0.29484(13) 0.0140(4) Uani 1 1 d . . .
C32 C -0.07800(18) 0.44980(9) 0.30086(14) 0.0158(4) Uani 1 1 d . . .
C33 C -0.20281(18) 0.44144(9) 0.23026(14) 0.0181(4) Uani 1 1 d . . .
C34 C -0.25518(19) 0.48633(9) 0.15450(15) 0.0185(4) Uani 1 1 d . . .
C35 C -0.18359(19) 0.54018(9) 0.15052(14) 0.0186(4) Uani 1 1 d . . .
C36 C -0.05813(18) 0.54874(9) 0.21946(14) 0.0171(4) Uani 1 1 d . . .
C41 C 0.17800(18) 0.58510(8) 0.45208(13) 0.0151(4) Uani 1 1 d . . .
C42 C 0.3037(2) 0.60391(9) 0.51346(15) 0.0192(4) Uani 1 1 d . . .
C43 C 0.3192(2) 0.65736(9) 0.57481(15) 0.0230(4) Uani 1 1 d . . .
C44 C 0.2103(2) 0.69317(9) 0.57190(15) 0.0224(4) Uani 1 1 d . . .
C45 C 0.0852(2) 0.67530(9) 0.50890(15) 0.0199(4) Uani 1 1 d . . .
C46 C 0.06822(19) 0.62085(9) 0.44961(14) 0.0166(4) Uani 1 1 d . . .
H1 H -0.1511(19) 0.4125(9) 0.0043(14) 0.015(5) Uiso 1 1 d . . .
H2 H 0.1729(18) 0.3778(8) 0.3556(15) 0.010(5) Uiso 1 1 d . . .
H3 H -0.017(2) 0.6087(9) 0.4068(15) 0.015(5) Uiso 1 1 d . . .
H4 H -0.0910(18) 0.3626(8) -0.0485(15) 0.011(5) Uiso 1 1 d . . .
H5 H 0.010(2) 0.6992(10) 0.5054(16) 0.026(6) Uiso 1 1 d . . .
H6 H 0.054(2) 0.4485(11) 0.0138(17) 0.034(6) Uiso 1 1 d . . .
H7 H 0.364(2) 0.4313(10) 0.3405(15) 0.021(5) Uiso 1 1 d . . .
H8 H -0.0092(19) 0.5853(9) 0.2176(14) 0.014(5) Uiso 1 1 d . . .
H9 H -0.044(2) 0.4204(10) 0.3524(16) 0.021(5) Uiso 1 1 d . . .
H10 H 0.2473(19) 0.2934(9) 0.4632(15) 0.015(5) Uiso 1 1 d . . .
H11 H 0.3361(19) 0.3075(9) 0.6395(15) 0.018(5) Uiso 1 1 d . . .
H12 H 0.334(2) 0.4103(9) 0.7052(16) 0.020(5) Uiso 1 1 d . . .
H13 H 0.2148(19) 0.6079(9) 0.2573(15) 0.018(5) Uiso 1 1 d . . .
H14 H 0.473(2) 0.5317(10) 0.1418(16) 0.021(5) Uiso 1 1 d . . .
H15 H -0.340(2) 0.4794(9) 0.1074(16) 0.025(6) Uiso 1 1 d . . .
H16 H 0.0556(18) 0.4361(9) 0.1259(15) 0.014(5) Uiso 1 1 d . . .
H17 H 0.403(2) 0.6686(9) 0.6133(15) 0.015(5) Uiso 1 1 d . . .
H18 H 0.340(2) 0.6160(10) 0.1523(16) 0.027(6) Uiso 1 1 d . . .
H19 H 0.379(2) 0.5806(10) 0.5153(15) 0.023(6) Uiso 1 1 d . . .
H20 H 0.439(2) 0.2396(11) 0.421(2) 0.041(7) Uiso 1 1 d . . .
H21 H 0.2220(19) 0.7294(10) 0.6118(15) 0.019(5) Uiso 1 1 d . . .
H22 H -0.253(2) 0.4036(10) 0.2341(15) 0.021(5) Uiso 1 1 d . . .
H23 H 0.248(2) 0.3980(9) 0.1017(14) 0.016(5) Uiso 1 1 d . . .
H24 H 0.2614(19) 0.4966(9) 0.5997(15) 0.018(5) Uiso 1 1 d . . .
H25 H -0.215(2) 0.5706(9) 0.1061(15) 0.018(5) Uiso 1 1 d . . .
H26 H 0.163(2) 0.3505(9) 0.0191(16) 0.022(5) Uiso 1 1 d . . .
H27 H 0.487(2) 0.4397(10) 0.2387(16) 0.030(6) Uiso 1 1 d . . .
H28 H 0.474(2) 0.2171(11) 0.3272(18) 0.041(7) Uiso 1 1 d . . .
H29 H 0.380(2) 0.1738(12) 0.3675(18) 0.042(7) Uiso 1 1 d . . .
H30 H -0.470(3) 0.3735(12) 0.037(2) 0.049(8) Uiso 1 1 d . . .
H31 H -0.342(3) 0.2100(13) 0.205(2) 0.055(8) Uiso 1 1 d . . .
H32 H -0.410(3) 0.2256(13) 0.093(2) 0.059(9) Uiso 1 1 d . . .
H33 H -0.549(3) 0.3701(13) 0.089(2) 0.048(9) Uiso 1 1 d . . .
H34 H -0.404(3) 0.2738(14) 0.172(2) 0.059(8) Uiso 1 1 d . . .
H1O1 H 0.021(4) 0.2046(14) 0.322(2) 0.086(11) 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 0.01100(12) 0.01162(12) 0.01139(12) 0.00099(9) 0.00286(9) 0.00030(9)
P1 0.0153(2) 0.0105(2) 0.0127(2) -0.00077(17) 0.00454(19) 0.00015(18)
O1 0.0193(7) 0.0173(7) 0.0165(6) 0.0062(5) 0.0061(6) -0.0011(5)
O2 0.0141(6) 0.0253(7) 0.0160(6) 0.0019(5) 0.0032(5) 0.0022(5)
O3 0.0131(6) 0.0222(7) 0.0227(7) 0.0021(6) 0.0067(6) 0.0019(5)
O4 0.0197(7) 0.0160(7) 0.0178(7) 0.0067(5) 0.0044(6) -0.0004(5)
O1W 0.0251(8) 0.0234(8) 0.0363(9) -0.0027(7) 0.0174(7) 0.0010(6)
N1 0.0176(8) 0.0116(7) 0.0118(7) -0.0006(6) 0.0052(6) -0.0013(6)
N2 0.0147(8) 0.0139(7) 0.0135(7) 0.0006(6) 0.0049(6) 0.0003(6)
N3 0.0130(7) 0.0131(7) 0.0128(7) 0.0015(6) 0.0035(6) 0.0010(6)
N4 0.0183(8) 0.0116(7) 0.0129(8) 0.0013(6) 0.0049(6) -0.0017(6)
C1 0.0155(10) 0.0230(11) 0.0236(11) 0.0023(9) 0.0080(9) -0.0018(8)
C2 0.0144(9) 0.0147(8) 0.0140(9) -0.0034(7) 0.0062(7) 0.0001(7)
C3 0.0141(9) 0.0146(9) 0.0127(8) -0.0035(7) 0.0045(7) 0.0024(7)
C4 0.0149(9) 0.0180(9) 0.0121(9) 0.0031(7) 0.0038(7) 0.0035(7)
C9 0.0173(9) 0.0129(9) 0.0156(9) 0.0030(7) 0.0062(8) 0.0011(7)
C5 0.0134(9) 0.0144(9) 0.0158(9) 0.0007(7) 0.0047(8) -0.0004(7)
C6 0.0154(9) 0.0132(9) 0.0132(8) -0.0029(7) 0.0046(7) 0.0008(7)
C7 0.0157(9) 0.0131(9) 0.0131(9) -0.0023(7) 0.0026(7) 0.0016(7)
C8 0.0158(10) 0.0203(10) 0.0198(10) 0.0034(8) 0.0007(8) 0.0029(8)
C11 0.0160(9) 0.0122(9) 0.0137(9) 0.0001(7) 0.0046(7) 0.0004(7)
C12 0.0220(10) 0.0162(9) 0.0127(9) -0.0018(7) 0.0048(8) -0.0010(7)
C13 0.0261(11) 0.0115(9) 0.0215(10) -0.0004(7) 0.0087(9) 0.0001(8)
C14 0.0241(10) 0.0179(10) 0.0188(10) 0.0050(8) 0.0068(8) -0.0005(8)
C15 0.0214(10) 0.0216(10) 0.0128(9) 0.0004(7) 0.0039(8) -0.0033(8)
C16 0.0184(9) 0.0159(9) 0.0158(9) -0.0021(7) 0.0067(8) -0.0028(7)
C21 0.0126(9) 0.0157(9) 0.0127(9) -0.0026(7) 0.0019(7) -0.0012(7)
C22 0.0145(9) 0.0174(9) 0.0182(9) 0.0026(7) 0.0030(8) 0.0022(8)
C23 0.0147(9) 0.0258(10) 0.0157(9) 0.0045(8) 0.0021(8) -0.0028(8)
C24 0.0146(9) 0.0313(11) 0.0168(10) -0.0056(8) 0.0057(8) -0.0042(8)
C25 0.0191(10) 0.0208(10) 0.0258(11) -0.0093(8) 0.0075(9) -0.0007(8)
C26 0.0186(10) 0.0147(9) 0.0198(10) -0.0013(8) 0.0043(8) -0.0004(7)
C31 0.0144(9) 0.0143(9) 0.0134(9) -0.0030(7) 0.0048(7) -0.0001(7)
C32 0.0197(9) 0.0145(9) 0.0153(9) -0.0008(7) 0.0087(8) 0.0002(7)
C33 0.0188(9) 0.0173(10) 0.0203(10) -0.0058(7) 0.0094(8) -0.0039(8)
C34 0.0146(9) 0.0234(10) 0.0176(9) -0.0075(8) 0.0054(8) 0.0004(8)
C35 0.0198(10) 0.0215(10) 0.0153(9) 0.0025(8) 0.0069(8) 0.0046(8)
C36 0.0183(9) 0.0143(9) 0.0191(10) 0.0001(7) 0.0072(8) -0.0019(7)
C41 0.0219(10) 0.0118(8) 0.0127(8) 0.0002(7) 0.0074(8) -0.0019(7)
C42 0.0200(10) 0.0157(9) 0.0209(10) -0.0002(7) 0.0057(8) -0.0005(8)
C43 0.0294(12) 0.0181(10) 0.0191(10) -0.0030(8) 0.0051(9) -0.0080(8)
C44 0.0409(13) 0.0117(9) 0.0187(10) -0.0019(7) 0.0155(9) -0.0049(9)
C45 0.0302(11) 0.0139(9) 0.0209(10) 0.0010(8) 0.0155(9) 0.0021(8)
C46 0.0196(10) 0.0155(9) 0.0159(9) 0.0012(7) 0.0078(8) -0.0020(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 1.8653(16) . ?
Ni1 N3 1.8688(15) . ?
Ni1 N4 1.8720(16) . ?
Ni1 N1 1.8787(15) . ?
P1 C31 1.8002(19) . ?
P1 C41 1.8021(18) . ?
P1 C11 1.8021(18) . ?
P1 C21 1.8030(19) . ?
O1 N1 1.3608(18) . ?
O1 O4 2.4307(19) . ?
O1 H1O1 1.20(4) . ?
O2 C3 1.250(2) . ?
O3 C6 1.255(2) . ?
O4 N4 1.3585(19) . ?
O4 H1O1 1.24(4) . ?
O1W H30 0.87(3) . ?
O1W H33 0.80(3) . ?
N1 C2 1.287(2) . ?
N2 C3 1.330(2) . ?
N2 C4 1.462(2) . ?
N3 C6 1.331(2) . ?
N3 C5 1.466(2) . ?
N4 C7 1.292(2) . ?
C1 C2 1.487(2) . ?
C1 H31 0.92(3) . ?
C1 H32 0.97(3) . ?
C1 H34 0.95(3) . ?
C2 C3 1.508(2) . ?
C4 C9 1.517(3) . ?
C4 H1 0.97(2) . ?
C4 H4 0.981(19) . ?
C9 C5 1.513(2) . ?
C9 H6 0.98(2) . ?
C9 H16 0.978(19) . ?
C5 H23 0.97(2) . ?
C5 H26 0.97(2) . ?
C6 C7 1.503(2) . ?
C7 C8 1.486(3) . ?
C8 H20 0.97(3) . ?
C8 H28 0.99(2) . ?
C8 H29 0.99(3) . ?
C11 C16 1.399(2) . ?
C11 C12 1.403(2) . ?
C12 C13 1.386(3) . ?
C12 H2 0.936(19) . ?
C13 C14 1.390(3) . ?
C13 H10 0.926(19) . ?
C14 C15 1.388(3) . ?
C14 H11 0.97(2) . ?
C15 C16 1.389(3) . ?
C15 H12 0.94(2) . ?
C16 H24 0.956(19) . ?
C21 C26 1.395(3) . ?
C21 C22 1.403(2) . ?
C22 C23 1.387(3) . ?
C22 H13 0.94(2) . ?
C23 C24 1.386(3) . ?
C23 H18 0.94(2) . ?
C24 C25 1.383(3) . ?
C24 H14 0.92(2) . ?
C25 C26 1.387(3) . ?
C25 H27 0.95(2) . ?
C26 H7 0.93(2) . ?
C31 C32 1.398(3) . ?
C31 C36 1.406(2) . ?
C32 C33 1.387(3) . ?
C32 H9 0.93(2) . ?
C33 C34 1.390(3) . ?
C33 H22 0.97(2) . ?
C34 C35 1.384(3) . ?
C34 H15 0.94(2) . ?
C35 C36 1.384(3) . ?
C35 H25 0.88(2) . ?
C36 H8 0.94(2) . ?
C41 C46 1.396(3) . ?
C41 C42 1.396(3) . ?
C42 C43 1.391(3) . ?
C42 H19 0.94(2) . ?
C43 C44 1.387(3) . ?
C43 H17 0.92(2) . ?
C44 C45 1.392(3) . ?
C44 H21 0.93(2) . ?
C45 C46 1.391(3) . ?
C45 H5 0.94(2) . ?
C46 H3 0.95(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
N2 Ni1 N3 96.62(7) . . ?
N2 Ni1 N4 178.50(7) . . ?
N3 Ni1 N4 83.13(7) . . ?
N2 Ni1 N1 83.50(7) . . ?
N3 Ni1 N1 179.23(6) . . ?
N4 Ni1 N1 96.72(7) . . ?
C31 P1 C41 110.49(8) . . ?
C31 P1 C11 110.18(9) . . ?
C41 P1 C11 109.70(8) . . ?
C31 P1 C21 110.05(8) . . ?
C41 P1 C21 107.56(8) . . ?
C11 P1 C21 108.80(8) . . ?
N1 O1 O4 97.83(10) . . ?
N1 O1 H1O1 100.1(15) . . ?
O4 O1 H1O1 3.6(16) . . ?
N4 O4 O1 97.91(10) . . ?
N4 O4 H1O1 100.2(15) . . ?
O1 O4 H1O1 3.5(15) . . ?
H30 O1W H33 102(2) . . ?
C2 N1 O1 119.42(15) . . ?
C2 N1 Ni1 116.94(12) . . ?
O1 N1 Ni1 123.62(11) . . ?
C3 N2 C4 117.32(15) . . ?
C3 N2 Ni1 115.11(12) . . ?
C4 N2 Ni1 127.42(12) . . ?
C6 N3 C5 117.97(15) . . ?
C6 N3 Ni1 115.56(12) . . ?
C5 N3 Ni1 126.13(11) . . ?
C7 N4 O4 118.89(15) . . ?
C7 N4 Ni1 117.30(12) . . ?
O4 N4 Ni1 123.81(11) . . ?
C2 C1 H31 114.1(18) . . ?
C2 C1 H32 113.7(17) . . ?
H31 C1 H32 108(2) . . ?
C2 C1 H34 112.2(17) . . ?
H31 C1 H34 106(2) . . ?
H32 C1 H34 102(2) . . ?
N1 C2 C1 126.18(17) . . ?
N1 C2 C3 111.80(15) . . ?
C1 C2 C3 122.01(16) . . ?
O2 C3 N2 127.27(17) . . ?
O2 C3 C2 120.38(16) . . ?
N2 C3 C2 112.36(15) . . ?
N2 C4 C9 111.51(15) . . ?
N2 C4 H1 109.1(11) . . ?
C9 C4 H1 108.7(11) . . ?
N2 C4 H4 110.5(11) . . ?
C9 C4 H4 111.7(11) . . ?
H1 C4 H4 105.1(15) . . ?
C5 C9 C4 113.86(15) . . ?
C5 C9 H6 108.2(13) . . ?
C4 C9 H6 107.8(13) . . ?
C5 C9 H16 108.2(11) . . ?
C4 C9 H16 110.1(11) . . ?
H6 C9 H16 108.5(17) . . ?
N3 C5 C9 111.35(15) . . ?
N3 C5 H23 109.2(11) . . ?
C9 C5 H23 110.0(11) . . ?
N3 C5 H26 108.9(12) . . ?
C9 C5 H26 109.6(12) . . ?
H23 C5 H26 107.7(17) . . ?
O3 C6 N3 127.77(17) . . ?
O3 C6 C7 120.18(16) . . ?
N3 C6 C7 112.05(15) . . ?
N4 C7 C8 124.66(17) . . ?
N4 C7 C6 111.78(15) . . ?
C8 C7 C6 123.54(16) . . ?
C7 C8 H20 111.9(14) . . ?
C7 C8 H28 110.8(14) . . ?
H20 C8 H28 104.6(19) . . ?
C7 C8 H29 111.5(14) . . ?
H20 C8 H29 109.6(19) . . ?
H28 C8 H29 108.1(19) . . ?
C16 C11 C12 119.89(16) . . ?
C16 C11 P1 120.27(13) . . ?
C12 C11 P1 119.76(13) . . ?
C13 C12 C11 119.69(17) . . ?
C13 C12 H2 120.3(11) . . ?
C11 C12 H2 120.0(11) . . ?
C12 C13 C14 120.18(18) . . ?
C12 C13 H10 118.1(12) . . ?
C14 C13 H10 121.8(12) . . ?
C15 C14 C13 120.31(18) . . ?
C15 C14 H11 120.7(12) . . ?
C13 C14 H11 119.0(12) . . ?
C14 C15 C16 120.10(17) . . ?
C14 C15 H12 120.0(12) . . ?
C16 C15 H12 119.8(12) . . ?
C15 C16 C11 119.76(17) . . ?
C15 C16 H24 118.0(12) . . ?
C11 C16 H24 122.2(12) . . ?
C26 C21 C22 119.61(17) . . ?
C26 C21 P1 122.83(14) . . ?
C22 C21 P1 117.47(14) . . ?
C23 C22 C21 119.86(18) . . ?
C23 C22 H13 119.9(12) . . ?
C21 C22 H13 120.2(12) . . ?
C24 C23 C22 119.98(18) . . ?
C24 C23 H18 120.0(13) . . ?
C22 C23 H18 120.0(13) . . ?
C25 C24 C23 120.34(19) . . ?
C25 C24 H14 119.5(13) . . ?
C23 C24 H14 120.1(13) . . ?
C24 C25 C26 120.32(19) . . ?
C24 C25 H27 122.0(13) . . ?
C26 C25 H27 117.7(13) . . ?
C25 C26 C21 119.81(18) . . ?
C25 C26 H7 117.7(13) . . ?
C21 C26 H7 122.5(13) . . ?
C32 C31 C36 119.27(17) . . ?
C32 C31 P1 121.32(14) . . ?
C36 C31 P1 119.39(14) . . ?
C33 C32 C31 120.03(17) . . ?
C33 C32 H9 120.4(13) . . ?
C31 C32 H9 119.6(13) . . ?
C32 C33 C34 120.27(18) . . ?
C32 C33 H22 119.2(12) . . ?
C34 C33 H22 120.5(12) . . ?
C35 C34 C33 119.95(18) . . ?
C35 C34 H15 121.5(13) . . ?
C33 C34 H15 118.5(13) . . ?
C36 C35 C34 120.47(18) . . ?
C36 C35 H25 117.1(13) . . ?
C34 C35 H25 122.4(13) . . ?
C35 C36 C31 119.95(17) . . ?
C35 C36 H8 121.0(11) . . ?
C31 C36 H8 119.1(12) . . ?
C46 C41 C42 120.24(17) . . ?
C46 C41 P1 121.81(14) . . ?
C42 C41 P1 117.92(14) . . ?
C43 C42 C41 119.87(19) . . ?
C43 C42 H19 118.8(13) . . ?
C41 C42 H19 121.3(13) . . ?
C44 C43 C42 119.9(2) . . ?
C44 C43 H17 122.6(12) . . ?
C42 C43 H17 117.4(12) . . ?
C43 C44 C45 120.23(18) . . ?
C43 C44 H21 119.2(13) . . ?
C45 C44 H21 120.6(13) . . ?
C46 C45 C44 120.32(19) . . ?
C46 C45 H5 118.2(14) . . ?
C44 C45 H5 121.5(13) . . ?
C45 C46 C41 119.39(18) . . ?
C45 C46 H3 120.3(12) . . ?
C41 C46 H3 120.3(12) . . ?

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
N1 O1 O4 N4 -0.50(12) . . . . ?
O4 O1 N1 C2 176.35(14) . . . . ?
O4 O1 N1 Ni1 -1.83(13) . . . . ?
N2 Ni1 N1 C2 3.38(13) . . . . ?
N3 Ni1 N1 C2 -96(5) . . . . ?
N4 Ni1 N1 C2 -175.12(13) . . . . ?
N2 Ni1 N1 O1 -178.40(13) . . . . ?
N3 Ni1 N1 O1 82(5) . . . . ?
N4 Ni1 N1 O1 3.09(13) . . . . ?
N3 Ni1 N2 C3 174.23(12) . . . . ?
N4 Ni1 N2 C3 94(3) . . . . ?
N1 Ni1 N2 C3 -5.01(12) . . . . ?
N3 Ni1 N2 C4 -1.28(15) . . . . ?
N4 Ni1 N2 C4 -82(3) . . . . ?
N1 Ni1 N2 C4 179.49(15) . . . . ?
N2 Ni1 N3 C6 -174.56(13) . . . . ?
N4 Ni1 N3 C6 3.95(13) . . . . ?
N1 Ni1 N3 C6 -75(5) . . . . ?
N2 Ni1 N3 C5 -1.47(15) . . . . ?
N4 Ni1 N3 C5 177.04(15) . . . . ?
N1 Ni1 N3 C5 98(5) . . . . ?
O1 O4 N4 C7 -176.96(14) . . . . ?
O1 O4 N4 Ni1 2.67(13) . . . . ?
N2 Ni1 N4 C7 78(3) . . . . ?
N3 Ni1 N4 C7 -3.21(13) . . . . ?
N1 Ni1 N4 C7 176.02(13) . . . . ?
N2 Ni1 N4 O4 -102(3) . . . . ?
N3 Ni1 N4 O4 177.15(14) . . . . ?
N1 Ni1 N4 O4 -3.61(14) . . . . ?
O1 N1 C2 C1 -0.4(3) . . . . ?
Ni1 N1 C2 C1 177.90(15) . . . . ?
O1 N1 C2 C3 -179.50(13) . . . . ?
Ni1 N1 C2 C3 -1.21(19) . . . . ?
C4 N2 C3 O2 1.5(3) . . . . ?
Ni1 N2 C3 O2 -174.51(14) . . . . ?
C4 N2 C3 C2 -178.47(14) . . . . ?
Ni1 N2 C3 C2 5.54(19) . . . . ?
N1 C2 C3 O2 177.23(16) . . . . ?
C1 C2 C3 O2 -1.9(3) . . . . ?
N1 C2 C3 N2 -2.8(2) . . . . ?
C1 C2 C3 N2 178.03(16) . . . . ?
C3 N2 C4 C9 157.64(16) . . . . ?
Ni1 N2 C4 C9 -26.9(2) . . . . ?
N2 C4 C9 C5 62.7(2) . . . . ?
C6 N3 C5 C9 -154.81(16) . . . . ?
Ni1 N3 C5 C9 32.3(2) . . . . ?
C4 C9 C5 N3 -65.6(2) . . . . ?
C5 N3 C6 O3 1.9(3) . . . . ?
Ni1 N3 C6 O3 175.56(15) . . . . ?
C5 N3 C6 C7 -177.59(14) . . . . ?
Ni1 N3 C6 C7 -3.91(19) . . . . ?
O4 N4 C7 C8 2.7(3) . . . . ?
Ni1 N4 C7 C8 -176.99(14) . . . . ?
O4 N4 C7 C6 -178.48(14) . . . . ?
Ni1 N4 C7 C6 1.86(19) . . . . ?
O3 C6 C7 N4 -178.18(16) . . . . ?
N3 C6 C7 N4 1.3(2) . . . . ?
O3 C6 C7 C8 0.7(3) . . . . ?
N3 C6 C7 C8 -179.79(17) . . . . ?
C31 P1 C11 C16 -125.79(15) . . . . ?
C41 P1 C11 C16 -3.93(17) . . . . ?
C21 P1 C11 C16 113.48(15) . . . . ?
C31 P1 C11 C12 57.59(17) . . . . ?
C41 P1 C11 C12 179.44(15) . . . . ?
C21 P1 C11 C12 -63.14(17) . . . . ?
C16 C11 C12 C13 -1.6(3) . . . . ?
P1 C11 C12 C13 175.01(15) . . . . ?
C11 C12 C13 C14 -0.6(3) . . . . ?
C12 C13 C14 C15 2.7(3) . . . . ?
C13 C14 C15 C16 -2.6(3) . . . . ?
C14 C15 C16 C11 0.4(3) . . . . ?
C12 C11 C16 C15 1.7(3) . . . . ?
P1 C11 C16 C15 -174.91(14) . . . . ?
C31 P1 C21 C26 -105.31(16) . . . . ?
C41 P1 C21 C26 134.27(16) . . . . ?
C11 P1 C21 C26 15.50(18) . . . . ?
C31 P1 C21 C22 71.40(16) . . . . ?
C41 P1 C21 C22 -49.02(16) . . . . ?
C11 P1 C21 C22 -167.78(14) . . . . ?
C26 C21 C22 C23 2.3(3) . . . . ?
P1 C21 C22 C23 -174.53(14) . . . . ?
C21 C22 C23 C24 -0.3(3) . . . . ?
C22 C23 C24 C25 -2.1(3) . . . . ?
C23 C24 C25 C26 2.5(3) . . . . ?
C24 C25 C26 C21 -0.5(3) . . . . ?
C22 C21 C26 C25 -1.9(3) . . . . ?
P1 C21 C26 C25 174.73(14) . . . . ?
C41 P1 C31 C32 -120.16(15) . . . . ?
C11 P1 C31 C32 1.23(17) . . . . ?
C21 P1 C31 C32 121.20(15) . . . . ?
C41 P1 C31 C36 61.02(16) . . . . ?
C11 P1 C31 C36 -177.60(14) . . . . ?
C21 P1 C31 C36 -57.62(17) . . . . ?
C36 C31 C32 C33 2.8(3) . . . . ?
P1 C31 C32 C33 -176.05(14) . . . . ?
C31 C32 C33 C34 -1.3(3) . . . . ?
C32 C33 C34 C35 -1.2(3) . . . . ?
C33 C34 C35 C36 2.2(3) . . . . ?
C34 C35 C36 C31 -0.7(3) . . . . ?
C32 C31 C36 C35 -1.8(3) . . . . ?
P1 C31 C36 C35 177.05(14) . . . . ?
C31 P1 C41 C46 8.97(18) . . . . ?
C11 P1 C41 C46 -112.71(16) . . . . ?
C21 P1 C41 C46 129.11(15) . . . . ?
C31 P1 C41 C42 -172.75(14) . . . . ?
C11 P1 C41 C42 65.58(17) . . . . ?
C21 P1 C41 C42 -52.61(16) . . . . ?
C46 C41 C42 C43 2.0(3) . . . . ?
P1 C41 C42 C43 -176.28(14) . . . . ?
C41 C42 C43 C44 -2.5(3) . . . . ?
C42 C43 C44 C45 0.9(3) . . . . ?
C43 C44 C45 C46 1.1(3) . . . . ?
C44 C45 C46 C41 -1.5(3) . . . . ?
C42 C41 C46 C45 -0.1(3) . . . . ?
P1 C41 C46 C45 178.18(14) . . . . ?

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 H1O1 O4 1.20(4) 1.24(4) 2.4307(19) 173(3) .

_diffrn_measured_fraction_theta_max 0.913
_diffrn_reflns_theta_full        28.59
_diffrn_measured_fraction_theta_full 0.913
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.061