Bis(μ-acetato)(μ-2,6-bis­{[(2-hydroxy­ethyl)(2-pyridylmeth­yl)amino]meth­yl}-4-methyl­phenolato)dinickel(II) hexa­fluoro­phosphate hemihydrate

The asymmetric unit of the title compound, [Ni₂(C₂₅H₃₁N₄O₃)(C₂H₃O₂)₂]PF₆·0.5H₂O, consists of two dinuclear nickel cations, two hexa­fluoro­phosphate anions and one water mol­ecule of crystallization. Within each cation, the Ni atoms are bridged by two exogenous acetate groups and an endogenous cresol O atom of a phenolate-based `end-off' compartmental ligand that possesses two pendant chelating arms attached to the ortho positions of the phenol ring. Each Ni atom is six-coordinate with a slightly distorted octa­hedral geometry. The two symmetry-independent cations are linked into a dimeric unit through O—H...O hydrogen bonds. Additional O—H...O, C—H...F and C—H...O inter­molecular inter­actions link all of the units in the structure into a three-dimensional framework.

S1. Comment

The hydrolysis of biomolecules by dinuclear metallohydrolases has been a hot subject for bioinorganic chemists for many years (Wilcox, 1996). Dinuclear nickel complexes have long been of great interest because the Ni atom was found to act as the active center of urease (Lippard, 1995), which is an enzyme isolated from various bacteria and plants that can hydrolyze urea to form carbamate and ammonia. To gain an insight into the relationship of the structure and catalytic activity of urease, as well as its hydrolytic mechanism, a number of synthetic functional models containing dinuclear nickel of relevance of the active site of urease has been reported (Barrios & Lippard, 2000; Carlsson et al., 2004; Beddie et al., 2005). We have synthesized previously a symmetrical ligand, 2,6-bis{[(2-pyridylmethyl)(2-hydroxyethyl)amino] methyl}-4-methylphenol, (L), and showed that it can form a dinuclear zinc complex with a phenolate and an acetate bridge (Chen et al., 2005). We report here the crystal structure of the title compound, (I), whose structure is different from that of the previously reported dinuclear zinc complex (discussed later).

The asymmetric unit of (I) (Fig. 1), contains two dinuclear nickel cations, two hexafluorophosphate anions and one water molecule of crystallization. The two symmetry-independent dinuclear cations are linked into a dimeric unit through cooperative O—H···O hydrogen bonds (O9—H9···O7 and O3—-H3···O13; Table 2). The second hydroxy O atom in each cation forms a hydrogen bond with the O atom of a neighbouring water molecule. The water H atoms, in turn, interact with hydroxy O atoms and an acetate O atom in two different but symmetry-related cations. Together, these interactions link the cations into extended chains which run parallel to the [100] direction. Additional weak intermolecular C—H···F and C—H···O interactions (Table 1), link all of the units in the structure into a three-dimensional framework.

Within each cation, the two Ni atoms are bridged by two exogenous acetate groups and an endogenous cresolic O atom of L in a syn–syn mode, providing a (µ-phenolato)bis(µ-acetato)dinickel(II) core. Both nickel centers have an N₂O₄ coordination environment and the geometry around each Ni atom can be regarded as that of a slightly distorted octahedron. The two octahedra in each dinuclear nickel cation are corner-shared via the bridging phenol O atom. The planes defined by each Ni atom and its coordinated N atoms from the imine pendant arm (represented by atoms N1, N2, N5 and N6) and the pyridine ring include the two coordinated O atoms of the acetate bridges and are almost coplanar with the associated pyridine ring. The structure of (I) is different from that of the analogous dinuclear zinc complex (Chen et al., 2005). In the latter complex, the independent Zn atoms have different coordination numbers and geometry. One Zn atom is six-coordinate with an N₂O₄ donor set having a slightly distorted octahedral geometry, whereas the other Zn atom is five-coordinate with an N₂O₃ donor set having a roughly trigonal–bipyramidal geometry. Moreover, the two zinc-bound terminal alcohol hydroxy groups are also different; one is deprotonated but the other is protonated.

The average separation between the two Ni atoms in (I) is 3.399 (1) Å, which is comparable with that in urease (3.5 Å) (Jabri et al., 1995) and also similar to the Ni···Ni distances in most of the `end-off' compartmental ligand-derived dinuclear nickel complexes with additional bridges (Koga et al., 1998; Uozumi et al., 1998; Adams et al., 2003; Carlsson et al., 2004). The average Ni—O_ethanol bond length is 2.136 (3) Å, which is longer than those for Ni—O_cresol [1.992 (3) Å] and Ni—O_acetate [2.048 (2) Å]. The Ni—O distances for the acetate O atom not accepting a hydrogen bond and longer than those where a hydrogen bond is involved. As a result of the two exogenous acetate bridges, the Ni···Ni distance and the Ni—O_cresol—Ni angle [116.37 (14)°] are somewhat smaller than those observed in similar binuclear nickel complexes without additional bridges, e.g. [Ni₂L⁴(OAc)(µ-OAc)(CH₃OH)(OH₂)]⁺ [Ni···Ni = 3.5419 (12) Å and Ni—O_cresol—Ni = 121.40 (19)°; Adams et al., 2003] and [Ni₂(BPPMP)(H₂O)₄]⁺ [Ni···Ni = 3.775 (1) Å and Ni—O_cresol—Ni = 131.8 (1)°; de Brito et al., 2000]. The average Ni—N distance in (I) [2.083 (3) Å] agrees with the values expected for octahedral Ni^II complexes (Buchanan et al., 1989).

Related literature

For related literature, see: Adams et al. (2003); Barrios & Lippard (2000); Beddie et al. (2005); Brito et al. (2000); Buchanan et al. (1989); Carlsson et al. (2004); Chen et al. (2005); Jabri et al. (1995); Koga et al. (1998); Lippard (1995); Uozumi et al. (1998); Wilcox (1996).

S2. Experimental

Nickel acetate trihydrate (230 mg, 1.0 mmol) dissolved in methanol was added dropwise to a stirred solution of 2,6-bis{[(2-pyridylmethyl)(2-hydroxyethyl)amino]methyl}-4-methylphenol (218.3 mg, 0.5 mmol) in 25 ml of methanol and refluxed for 30 min in air. After the mixture was cooled to room temperature, a white precipitate was formed upon addition of potassium hexafluorophosphate (184.2 mg, 0.5 mmol) in portions. The precipitate was filtered off, and washed with cold methanol and diethyl ether. Green needle-shaped single crystals of (I) suitable for a crystal structure determination were obtained after ca 1 week by slow evaporation of the filtrate at room temperature [m.p. 509.6 (5) K].

S3. Refinement

The water and hydroxy H atoms were located in a difference Fourier map and their positions were refined with U_iso(H) = 1.2U_eq(O). The methyl H atoms were constrained to an ideal geometry with C—H = 0.96 Å and U_iso(H) = 1.5U_eq(C), but were allowed to rotate freely about the C—C bonds. All other H atoms were placed in geometrically idealized positions and constrained to ride on their parent C atom at a distance of 0.93 or 0.97 Å for phenyl or methylene groups, respectively, and with U_iso(H) = 1.2U_eq(C).

Computing details

Data collection: SMART (Bruker, 2000); cell refinement: SMART; data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXTL (Bruker, 2000); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Figures

Fig. 1. The two symmetry-independent dinuclear nickel cations of the title compound, showing 30% probability displacement ellipsoids and the atom-labelling scheme. The H atoms, except H9 and H3, have been omitted for clarity.

Bis(µ-acetato)(µ-2,6-bis{[(2-hydroxyethyl)(2-pyridylmethyl)amino]methyl}- 4-methylphenolato)dinickel(II) hexafluorophosphate hemihydrate

Crystal data

[Ni2(C25H31N4O3)(C2H3O2)2]PF6·0.5H2O	F(000) = 3400
Mr = 825.03	Dx = 1.587 Mg m^−3
Monoclinic, P21/c	Melting point: 509.6(5) K
Hall symbol: -P 2ybc	Mo Kα radiation, λ = 0.71073 Å
a = 15.7776 (19) Å	Cell parameters from 804 reflections
b = 17.191 (2) Å	θ = 2.4–15.7°
c = 25.513 (3) Å	µ = 1.22 mm^−1
β = 93.914 (3)°	T = 291 K
V = 6904.0 (14) Å^3	Needle, green
Z = 8	0.28 × 0.24 × 0.22 mm

Data collection

Bruker APEX CCD diffractometer	13513 independent reflections
Radiation source: sealed tube	9603 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.044
ϕ and ω scans	θmax = 26.0°, θmin = 1.8°
Absorption correction: multi-scan (SADABS; Bruker, 2000)	h = −19→16
Tmin = 0.72, Tmax = 0.76	k = −20→21
36723 measured reflections	l = −30→31

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.060	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.102	H atoms treated by a mixture of independent and constrained refinement
S = 1.10	w = 1/[σ^2(Fo^2) + (0.0298P)^2 + 5.0551P] where P = (Fo^2 + 2Fc^2)/3
13513 reflections	(Δ/σ)max = 0.020
916 parameters	Δρmax = 0.48 e Å^−3
3 restraints	Δρmin = −0.42 e Å^−3

Special details

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

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Ni1	0.54320 (3)	0.78470 (3)	0.46951 (2)	0.03709 (13)
Ni2	0.33237 (3)	0.77866 (3)	0.490289 (19)	0.03253 (12)
N1	0.61751 (19)	0.68250 (16)	0.47567 (12)	0.0337 (7)
N2	0.24926 (19)	0.7306 (2)	0.43004 (12)	0.0409 (8)
N3	0.56413 (17)	0.76482 (16)	0.39065 (12)	0.0313 (7)
N4	0.29435 (19)	0.68072 (17)	0.52949 (12)	0.0352 (7)
O1	0.43301 (15)	0.72605 (15)	0.46242 (10)	0.0375 (6)
O2	0.66820 (17)	0.83241 (16)	0.48823 (12)	0.0438 (7)
H2	0.666 (3)	0.862 (3)	0.5105 (18)	0.053*
O3	0.21475 (17)	0.83544 (15)	0.50327 (11)	0.0401 (6)
H3	0.199 (3)	0.812 (2)	0.5299 (17)	0.048*
O4	0.49467 (16)	0.88996 (14)	0.45591 (11)	0.0394 (6)
O5	0.35525 (16)	0.88416 (15)	0.45299 (10)	0.0415 (7)
O6	0.53072 (15)	0.79184 (15)	0.54994 (10)	0.0379 (6)
O7	0.39566 (15)	0.82015 (15)	0.55780 (10)	0.0388 (6)
C1	0.4303 (2)	0.6589 (2)	0.44025 (14)	0.0340 (8)
C2	0.3641 (2)	0.6397 (2)	0.40119 (16)	0.0373 (9)
C3	0.3590 (3)	0.5685 (3)	0.37842 (17)	0.0527 (11)
H3A	0.3129	0.5578	0.3548	0.063*
C4	0.4178 (3)	0.5122 (2)	0.38848 (16)	0.0452 (10)
C5	0.4833 (3)	0.5316 (2)	0.42539 (15)	0.0413 (10)
H5	0.5248	0.4942	0.4331	0.050*
C6	0.4915 (3)	0.6006 (2)	0.45106 (16)	0.0410 (9)
C7	0.5603 (2)	0.6191 (2)	0.49181 (16)	0.0385 (9)
H7A	0.5939	0.5727	0.4994	0.046*
H7B	0.5351	0.6345	0.5238	0.046*
C8	0.4171 (3)	0.4362 (2)	0.36068 (16)	0.0495 (11)
H8A	0.3602	0.4162	0.3573	0.074*
H8B	0.4532	0.4001	0.3804	0.074*
H8C	0.4376	0.4432	0.3264	0.074*
C9	0.3009 (2)	0.7031 (2)	0.38678 (15)	0.0370 (9)
H9A	0.3314	0.7473	0.3738	0.044*
H9B	0.2624	0.6846	0.3582	0.044*
C10	0.6551 (2)	0.6641 (2)	0.42515 (14)	0.0455 (10)
H10A	0.7150	0.6773	0.4281	0.055*
H10B	0.6503	0.6087	0.4186	0.055*
C11	0.6140 (2)	0.70582 (19)	0.38106 (13)	0.0357 (9)
C12	0.6310 (3)	0.6866 (3)	0.33271 (16)	0.0559 (12)
H12	0.6689	0.6466	0.3268	0.067*
C13	0.5916 (3)	0.7269 (3)	0.29116 (19)	0.0657 (14)
H13	0.6017	0.7126	0.2570	0.079*
C14	0.5392 (3)	0.7861 (3)	0.29914 (19)	0.0632 (14)
H14	0.5123	0.8139	0.2715	0.076*
C15	0.5275 (3)	0.8035 (2)	0.35027 (16)	0.0415 (10)
H15	0.4918	0.8448	0.3572	0.050*
C16	0.6876 (3)	0.7012 (2)	0.51752 (18)	0.0520 (12)
H16A	0.6640	0.7046	0.5516	0.062*
H16B	0.7297	0.6600	0.5190	0.062*
C17	0.7282 (3)	0.7765 (3)	0.50487 (18)	0.0523 (11)
H17A	0.7610	0.7954	0.5358	0.063*
H17B	0.7669	0.7681	0.4775	0.063*
C18	0.2025 (2)	0.6660 (2)	0.45048 (15)	0.0414 (10)
H18A	0.2030	0.6235	0.4255	0.050*
H18B	0.1438	0.6819	0.4525	0.050*
C19	0.2345 (2)	0.6362 (2)	0.50307 (15)	0.0320 (8)
C20	0.2031 (3)	0.5720 (2)	0.52414 (18)	0.0505 (11)
H20	0.1609	0.5435	0.5056	0.061*
C21	0.2330 (3)	0.5485 (3)	0.5726 (2)	0.0668 (14)
H21	0.2124	0.5033	0.5872	0.080*
C22	0.2934 (3)	0.5915 (3)	0.5997 (2)	0.0673 (15)
H22	0.3141	0.5769	0.6333	0.081*
C23	0.3229 (3)	0.6563 (3)	0.57677 (18)	0.0509 (11)
H23	0.3652	0.6851	0.5951	0.061*
C24	0.1933 (2)	0.7948 (3)	0.41343 (15)	0.0450 (10)
H24A	0.1487	0.7757	0.3887	0.054*
H24B	0.2255	0.8336	0.3956	0.054*
C25	0.1535 (3)	0.8323 (3)	0.46015 (17)	0.0483 (11)
H25A	0.1342	0.8844	0.4509	0.058*
H25B	0.1049	0.8020	0.4695	0.058*
C26	0.4707 (2)	0.8073 (2)	0.57660 (15)	0.0351 (8)
C27	0.4868 (3)	0.8130 (3)	0.63477 (16)	0.0517 (11)
H27A	0.5041	0.7632	0.6487	0.062*
H27C	0.4358	0.8292	0.6501	0.062*
H27B	0.5310	0.8504	0.6430	0.062*
C28	0.4236 (2)	0.9168 (2)	0.44654 (15)	0.0378 (9)
C29	0.4181 (3)	0.9993 (2)	0.42881 (18)	0.0509 (11)
H29A	0.4413	1.0326	0.4564	0.076*
H29B	0.3597	1.0128	0.4204	0.076*
H29C	0.4497	1.0058	0.3983	0.076*
Ni3	0.18799 (3)	0.94476 (3)	0.63169 (2)	0.03748 (12)
Ni4	−0.02340 (3)	0.96572 (3)	0.64428 (2)	0.04316 (14)
O8	0.09418 (16)	0.96703 (14)	0.67716 (10)	0.0372 (6)
O9	0.29492 (18)	0.94084 (16)	0.58567 (11)	0.0426 (7)
H9	0.317 (3)	0.899 (3)	0.5893 (17)	0.051*
O10	−0.15073 (19)	0.94549 (18)	0.61502 (13)	0.0534 (8)
H10	−0.152 (3)	0.926 (3)	0.5861 (19)	0.064*
O11	0.14149 (17)	1.02106 (16)	0.57337 (11)	0.0464 (7)
O12	0.00436 (17)	1.02009 (16)	0.57890 (12)	0.0496 (7)
O13	0.13024 (18)	0.85538 (15)	0.59146 (11)	0.0468 (7)
O14	−0.00036 (18)	0.85345 (17)	0.61917 (13)	0.0547 (8)
N5	0.26711 (19)	1.0279 (2)	0.67245 (13)	0.0448 (8)
N6	−0.0742 (2)	0.9264 (2)	0.71081 (14)	0.0509 (9)
N7	0.2495 (2)	0.8707 (2)	0.68456 (13)	0.0437 (8)
N8	−0.0492 (2)	1.0699 (2)	0.67971 (14)	0.0493 (9)
C30	0.1054 (3)	0.9900 (3)	0.72570 (18)	0.0546 (12)
C31	0.1655 (3)	1.0502 (3)	0.74111 (19)	0.0580 (12)
C32	0.1742 (3)	1.0723 (3)	0.7926 (2)	0.0607 (13)
H32	0.2121	1.1117	0.8029	0.073*
C33	0.1264 (4)	1.0361 (4)	0.8303 (2)	0.0767 (16)
C34	0.0708 (3)	0.9783 (3)	0.81221 (19)	0.0651 (14)
H34	0.0380	0.9547	0.8366	0.078*
C35	0.0605 (3)	0.9544 (3)	0.7641 (2)	0.0602 (13)
C36	0.2133 (3)	1.0869 (2)	0.69908 (19)	0.0527 (12)
H36A	0.2495	1.1277	0.7143	0.063*
H36B	0.1734	1.1105	0.6731	0.063*
C37	0.1388 (4)	1.0651 (4)	0.8866 (2)	0.0847 (18)
H37A	0.0874	1.0574	0.9041	0.127*
H37B	0.1525	1.1195	0.8866	0.127*
H37C	0.1842	1.0368	0.9048	0.127*
C38	−0.0110 (3)	0.8959 (3)	0.74590 (16)	0.0562 (12)
H38A	0.0147	0.8517	0.7295	0.067*
H38B	−0.0374	0.8769	0.7767	0.067*
C39	0.3264 (3)	0.9848 (3)	0.7136 (2)	0.0659 (14)
H39A	0.3848	0.9929	0.7052	0.079*
H39B	0.3198	1.0077	0.7478	0.079*
C40	0.3107 (3)	0.9016 (3)	0.71669 (15)	0.0518 (12)
C41	0.3611 (3)	0.8561 (3)	0.75290 (17)	0.0533 (12)
H41	0.4048	0.8769	0.7748	0.064*
C42	0.3403 (4)	0.7799 (3)	0.7530 (2)	0.0659 (14)
H42	0.3704	0.7472	0.7767	0.079*
C43	0.2819 (4)	0.7505 (3)	0.7224 (2)	0.0681 (14)
H43	0.2703	0.6975	0.7235	0.082*
C44	0.2376 (3)	0.7963 (3)	0.68903 (19)	0.0580 (12)
H44	0.1949	0.7736	0.6672	0.070*
C45	0.3141 (3)	1.0641 (3)	0.62974 (18)	0.0521 (11)
H45A	0.2748	1.0934	0.6064	0.063*
H45B	0.3565	1.0999	0.6449	0.063*
C46	0.3562 (3)	1.0028 (3)	0.59936 (17)	0.0531 (12)
H46A	0.3766	1.0251	0.5676	0.064*
H46B	0.4045	0.9817	0.6203	0.064*
C47	−0.1190 (3)	0.9880 (3)	0.7400 (2)	0.0661 (14)
H47A	−0.1793	0.9877	0.7295	0.079*
H47B	−0.1118	0.9787	0.7775	0.079*
C48	−0.0822 (3)	1.0617 (3)	0.7273 (2)	0.0648 (14)
C49	−0.0817 (4)	1.1174 (4)	0.7612 (2)	0.0797 (16)
H49	−0.1062	1.1092	0.7929	0.096*
C50	−0.0450 (5)	1.1900 (4)	0.7515 (3)	0.093 (2)
H50	−0.0447	1.2297	0.7764	0.112*
C51	−0.0097 (4)	1.2008 (3)	0.7043 (2)	0.0797 (17)
H51	0.0154	1.2478	0.6960	0.096*
C52	−0.0129 (3)	1.1392 (3)	0.66983 (17)	0.0534 (11)
H52	0.0114	1.1456	0.6379	0.064*
C53	−0.1375 (3)	0.8616 (3)	0.69253 (18)	0.0573 (12)
H53A	−0.1719	0.8468	0.7210	0.069*
H53B	−0.1071	0.8161	0.6816	0.069*
C54	−0.1956 (3)	0.8950 (3)	0.64500 (17)	0.0528 (12)
H54A	−0.2176	0.8524	0.6232	0.063*
H54B	−0.2436	0.9222	0.6583	0.063*
C55	0.0606 (3)	0.8243 (3)	0.59773 (16)	0.0467 (11)
C56	0.0501 (3)	0.7403 (3)	0.5808 (2)	0.0573 (12)
H56A	0.0821	0.7310	0.5507	0.086*
H56B	−0.0089	0.7297	0.5719	0.086*
H56C	0.0705	0.7068	0.6091	0.086*
C57	0.0706 (3)	1.0425 (3)	0.55888 (15)	0.0446 (10)
C58	0.0618 (3)	1.1012 (3)	0.51513 (16)	0.0495 (11)
H58A	0.0514	1.1516	0.5295	0.074*
H58B	0.0150	1.0868	0.4910	0.074*
H58C	0.1131	1.1024	0.4970	0.074*
P1	0.38834 (10)	0.98382 (9)	0.25655 (6)	0.0690 (4)
F1	0.44570 (18)	1.02820 (16)	0.21986 (11)	0.0721 (8)
F2	0.46706 (18)	0.97125 (16)	0.29585 (11)	0.0716 (8)
F3	0.3359 (2)	0.9371 (2)	0.29229 (12)	0.0861 (9)
F4	0.3094 (2)	0.99697 (18)	0.21814 (13)	0.0842 (9)
F5	0.41148 (18)	0.90714 (16)	0.22714 (11)	0.0710 (8)
F6	0.3649 (2)	1.05971 (18)	0.28480 (12)	0.0849 (9)
P2	0.92703 (10)	0.65001 (9)	0.42341 (6)	0.0701 (4)
F7	0.96839 (18)	0.70076 (15)	0.46255 (12)	0.0700 (8)
F8	0.97736 (18)	0.58069 (16)	0.43800 (11)	0.0697 (8)
F9	0.88030 (19)	0.61357 (17)	0.37770 (12)	0.0737 (8)
F10	0.87439 (19)	0.72389 (17)	0.40607 (12)	0.0762 (8)
F11	0.99782 (18)	0.67458 (16)	0.38628 (12)	0.0731 (8)
F12	0.85898 (19)	0.62638 (18)	0.46113 (12)	0.0797 (8)
O15	0.7575 (2)	0.9793 (2)	0.51634 (14)	0.0543 (8)
H15A	0.758 (3)	1.008 (3)	0.544 (2)	0.065*
H15B	0.733 (3)	1.003 (3)	0.492 (2)	0.065*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ni1	0.0353 (3)	0.0351 (3)	0.0429 (3)	−0.0032 (2)	0.0183 (2)	0.0016 (2)
Ni2	0.0251 (2)	0.0355 (2)	0.0386 (3)	−0.0017 (2)	0.01434 (19)	0.0008 (2)
N1	0.0368 (17)	0.0276 (15)	0.0381 (18)	0.0012 (13)	0.0116 (14)	0.0042 (13)
N2	0.0292 (16)	0.062 (2)	0.0326 (17)	0.0009 (15)	0.0065 (13)	0.0066 (16)
N3	0.0249 (15)	0.0283 (16)	0.0421 (18)	−0.0135 (12)	0.0118 (13)	−0.0027 (14)
N4	0.0321 (16)	0.0355 (17)	0.0401 (19)	−0.0043 (14)	0.0170 (14)	−0.0010 (15)
O1	0.0292 (13)	0.0421 (15)	0.0438 (15)	−0.0043 (11)	0.0220 (11)	−0.0030 (12)
O2	0.0340 (15)	0.0445 (17)	0.0545 (19)	−0.0078 (13)	0.0154 (14)	−0.0037 (13)
O3	0.0354 (15)	0.0409 (16)	0.0452 (17)	0.0011 (12)	0.0116 (13)	−0.0066 (13)
O4	0.0296 (14)	0.0360 (14)	0.0539 (17)	0.0064 (11)	0.0119 (12)	−0.0081 (13)
O5	0.0368 (15)	0.0518 (16)	0.0384 (15)	0.0011 (12)	0.0205 (12)	0.0211 (13)
O6	0.0271 (13)	0.0530 (16)	0.0334 (14)	0.0039 (12)	0.0013 (11)	−0.0103 (12)
O7	0.0280 (14)	0.0500 (16)	0.0402 (15)	−0.0091 (12)	0.0163 (11)	−0.0100 (13)
C1	0.0237 (18)	0.048 (2)	0.032 (2)	−0.0084 (16)	0.0146 (15)	0.0002 (18)
C2	0.0247 (18)	0.041 (2)	0.047 (2)	−0.0001 (16)	0.0118 (17)	0.0166 (19)
C3	0.053 (3)	0.065 (3)	0.041 (3)	0.003 (2)	0.013 (2)	−0.008 (2)
C4	0.055 (3)	0.050 (2)	0.033 (2)	−0.006 (2)	0.023 (2)	0.0097 (19)
C5	0.045 (2)	0.046 (2)	0.036 (2)	0.0023 (19)	0.0201 (18)	0.0200 (19)
C6	0.042 (2)	0.044 (2)	0.038 (2)	0.0002 (18)	0.0096 (18)	0.0108 (19)
C7	0.031 (2)	0.036 (2)	0.051 (2)	0.0002 (16)	0.0152 (17)	0.0193 (18)
C8	0.063 (3)	0.047 (2)	0.038 (2)	−0.016 (2)	0.006 (2)	0.002 (2)
C9	0.0192 (17)	0.056 (2)	0.035 (2)	0.0095 (16)	−0.0010 (15)	−0.0012 (18)
C10	0.044 (2)	0.039 (2)	0.056 (3)	−0.0038 (18)	0.024 (2)	0.002 (2)
C11	0.032 (2)	0.0297 (19)	0.047 (2)	−0.0136 (16)	0.0136 (17)	−0.0078 (17)
C12	0.068 (3)	0.067 (3)	0.033 (2)	0.011 (2)	0.004 (2)	−0.020 (2)
C13	0.073 (3)	0.078 (3)	0.045 (3)	−0.001 (3)	−0.001 (2)	−0.023 (3)
C14	0.060 (3)	0.079 (3)	0.047 (3)	0.014 (3)	−0.023 (2)	−0.014 (3)
C15	0.041 (2)	0.035 (2)	0.051 (3)	−0.0039 (17)	0.0159 (19)	−0.0091 (19)
C16	0.040 (2)	0.054 (3)	0.060 (3)	0.011 (2)	−0.017 (2)	−0.005 (2)
C17	0.034 (2)	0.066 (3)	0.057 (3)	−0.001 (2)	−0.0065 (19)	−0.011 (2)
C18	0.0226 (19)	0.061 (3)	0.041 (2)	−0.0036 (18)	0.0027 (16)	−0.002 (2)
C19	0.0224 (17)	0.0296 (18)	0.046 (2)	0.0013 (14)	0.0163 (16)	−0.0122 (17)
C20	0.058 (3)	0.044 (2)	0.051 (3)	−0.015 (2)	0.016 (2)	−0.003 (2)
C21	0.059 (3)	0.058 (3)	0.085 (4)	−0.015 (2)	0.007 (3)	0.015 (3)
C22	0.076 (4)	0.065 (3)	0.060 (3)	−0.013 (3)	0.002 (3)	0.040 (3)
C23	0.047 (3)	0.055 (3)	0.050 (3)	−0.014 (2)	−0.001 (2)	0.012 (2)
C24	0.030 (2)	0.076 (3)	0.030 (2)	0.013 (2)	0.0094 (16)	−0.005 (2)
C25	0.042 (2)	0.054 (3)	0.051 (3)	0.015 (2)	0.012 (2)	−0.005 (2)
C26	0.040 (2)	0.0264 (18)	0.040 (2)	−0.0004 (16)	0.0127 (18)	0.0046 (16)
C27	0.037 (2)	0.079 (3)	0.040 (2)	−0.017 (2)	0.0059 (18)	−0.008 (2)
C28	0.034 (2)	0.043 (2)	0.039 (2)	−0.0005 (17)	0.0243 (17)	−0.0032 (18)
C29	0.050 (3)	0.046 (2)	0.059 (3)	0.016 (2)	0.015 (2)	−0.003 (2)
Ni3	0.0335 (3)	0.0340 (3)	0.0456 (3)	−0.0043 (2)	0.0069 (2)	0.0019 (2)
Ni4	0.0294 (3)	0.0509 (3)	0.0511 (3)	−0.0032 (2)	0.0173 (2)	−0.0115 (3)
O8	0.0359 (14)	0.0377 (14)	0.0383 (15)	0.0033 (11)	0.0052 (11)	−0.0036 (12)
O9	0.0437 (16)	0.0360 (15)	0.0503 (17)	0.0019 (13)	0.0194 (13)	0.0021 (14)
O10	0.0497 (18)	0.0543 (18)	0.057 (2)	−0.0305 (15)	0.0082 (16)	−0.0069 (16)
O11	0.0414 (17)	0.0552 (17)	0.0451 (17)	0.0124 (14)	0.0217 (13)	0.0100 (14)
O12	0.0415 (16)	0.0510 (17)	0.0579 (19)	0.0091 (13)	0.0152 (14)	0.0106 (15)
O13	0.0463 (17)	0.0450 (16)	0.0499 (18)	−0.0125 (13)	0.0076 (14)	−0.0159 (14)
O14	0.0446 (18)	0.0504 (18)	0.071 (2)	−0.0164 (14)	0.0152 (16)	−0.0178 (16)
N5	0.0303 (17)	0.060 (2)	0.045 (2)	−0.0073 (16)	0.0112 (15)	−0.0149 (17)
N6	0.045 (2)	0.056 (2)	0.053 (2)	−0.0097 (17)	0.0205 (18)	0.0015 (18)
N7	0.0311 (18)	0.058 (2)	0.042 (2)	0.0075 (16)	0.0018 (15)	0.0064 (17)
N8	0.042 (2)	0.053 (2)	0.053 (2)	0.0136 (17)	0.0080 (17)	−0.0054 (18)
C30	0.043 (3)	0.077 (3)	0.044 (3)	0.012 (2)	0.001 (2)	−0.019 (2)
C31	0.040 (3)	0.079 (3)	0.053 (3)	0.009 (2)	−0.007 (2)	−0.004 (3)
C32	0.049 (3)	0.058 (3)	0.073 (4)	−0.005 (2)	−0.005 (2)	−0.020 (3)
C33	0.084 (4)	0.096 (4)	0.049 (3)	0.021 (4)	−0.001 (3)	−0.009 (3)
C34	0.065 (3)	0.092 (4)	0.037 (3)	0.009 (3)	0.004 (2)	0.020 (3)
C35	0.041 (3)	0.082 (4)	0.055 (3)	0.014 (2)	−0.010 (2)	0.001 (3)
C36	0.041 (2)	0.045 (2)	0.071 (3)	−0.007 (2)	0.001 (2)	−0.016 (2)
C37	0.101 (5)	0.091 (4)	0.062 (4)	0.018 (4)	0.004 (3)	−0.010 (3)
C38	0.072 (3)	0.072 (3)	0.025 (2)	−0.014 (3)	0.004 (2)	0.013 (2)
C39	0.057 (3)	0.077 (4)	0.061 (3)	−0.010 (3)	−0.016 (2)	−0.024 (3)
C40	0.046 (3)	0.087 (3)	0.023 (2)	0.012 (2)	0.0042 (18)	−0.014 (2)
C41	0.032 (2)	0.090 (4)	0.037 (2)	0.018 (2)	0.0001 (18)	−0.012 (2)
C42	0.070 (3)	0.075 (4)	0.053 (3)	0.021 (3)	0.004 (3)	0.010 (3)
C43	0.087 (4)	0.051 (3)	0.066 (3)	0.025 (3)	0.006 (3)	0.014 (3)
C44	0.053 (3)	0.064 (3)	0.059 (3)	0.013 (2)	0.020 (2)	0.014 (2)
C45	0.048 (3)	0.050 (2)	0.058 (3)	−0.032 (2)	0.003 (2)	−0.001 (2)
C46	0.040 (2)	0.080 (3)	0.041 (2)	−0.026 (2)	0.0096 (19)	0.011 (2)
C47	0.062 (3)	0.088 (4)	0.050 (3)	−0.007 (3)	0.015 (2)	−0.017 (3)
C48	0.041 (3)	0.090 (4)	0.064 (3)	−0.002 (3)	0.013 (2)	−0.024 (3)
C49	0.091 (4)	0.082 (4)	0.069 (4)	0.005 (3)	0.028 (3)	−0.006 (3)
C50	0.134 (6)	0.068 (4)	0.081 (4)	0.032 (4)	0.032 (4)	−0.001 (3)
C51	0.110 (5)	0.054 (3)	0.078 (4)	−0.006 (3)	0.028 (4)	−0.003 (3)
C52	0.059 (3)	0.065 (3)	0.036 (2)	0.009 (2)	0.004 (2)	0.007 (2)
C53	0.064 (3)	0.063 (3)	0.047 (3)	−0.018 (2)	0.022 (2)	−0.009 (2)
C54	0.050 (3)	0.057 (3)	0.053 (3)	−0.028 (2)	0.009 (2)	−0.009 (2)
C55	0.041 (2)	0.057 (3)	0.041 (2)	−0.019 (2)	−0.0053 (19)	−0.017 (2)
C56	0.050 (3)	0.053 (3)	0.068 (3)	−0.016 (2)	−0.002 (2)	−0.012 (2)
C57	0.046 (3)	0.063 (3)	0.026 (2)	0.001 (2)	0.0130 (18)	−0.0054 (19)
C58	0.048 (2)	0.061 (3)	0.039 (2)	0.013 (2)	0.0017 (19)	−0.002 (2)
P1	0.0680 (9)	0.0725 (9)	0.0688 (10)	−0.0008 (7)	0.0213 (8)	0.0039 (8)
F1	0.075 (2)	0.0724 (18)	0.0715 (19)	−0.0003 (15)	0.0237 (15)	0.0032 (15)
F2	0.0698 (19)	0.0741 (19)	0.0734 (19)	−0.0010 (15)	0.0223 (15)	0.0030 (15)
F3	0.080 (2)	0.102 (2)	0.079 (2)	−0.0078 (18)	0.0234 (17)	0.0141 (18)
F4	0.089 (2)	0.084 (2)	0.081 (2)	0.0103 (18)	0.0168 (18)	−0.0191 (17)
F5	0.0715 (19)	0.0727 (18)	0.0714 (19)	−0.0006 (15)	0.0235 (15)	0.0042 (15)
F6	0.093 (2)	0.082 (2)	0.081 (2)	0.0101 (18)	0.0171 (18)	−0.0185 (18)
P2	0.0721 (9)	0.0658 (9)	0.0754 (10)	−0.0031 (7)	0.0265 (7)	0.0042 (8)
F7	0.0732 (19)	0.0573 (16)	0.081 (2)	−0.0028 (14)	0.0179 (16)	0.0122 (15)
F8	0.0707 (18)	0.0629 (17)	0.080 (2)	−0.0019 (14)	0.0353 (15)	0.0085 (15)
F9	0.076 (2)	0.0715 (19)	0.0745 (19)	0.0003 (15)	0.0094 (15)	0.0019 (15)
F10	0.077 (2)	0.0761 (19)	0.077 (2)	0.0134 (16)	0.0151 (16)	0.0132 (16)
F11	0.073 (2)	0.0682 (18)	0.081 (2)	−0.0015 (15)	0.0317 (16)	0.0081 (15)
F12	0.074 (2)	0.089 (2)	0.078 (2)	−0.0045 (16)	0.0223 (14)	0.0058 (17)
O15	0.0472 (18)	0.067 (2)	0.049 (2)	0.0031 (16)	0.0061 (15)	0.0046 (16)

Geometric parameters (Å, º)

Ni1—O4	1.986 (3)	Ni4—O12	1.987 (3)
Ni1—O1	2.007 (2)	Ni4—N6	2.041 (3)
Ni1—O6	2.078 (3)	Ni4—N8	2.060 (3)
Ni1—N3	2.089 (3)	Ni4—O14	2.074 (3)
Ni1—N1	2.112 (3)	Ni4—O10	2.124 (3)
Ni1—O2	2.159 (3)	O8—C30	1.300 (5)
Ni2—O1	2.000 (2)	O9—C46	1.464 (5)
Ni2—O7	2.058 (3)	O9—H9	0.80 (4)
Ni2—N4	2.068 (3)	O10—C54	1.383 (5)
Ni2—O5	2.091 (2)	O10—H10	0.81 (5)
Ni2—N2	2.119 (3)	O11—C57	1.210 (5)
Ni2—O3	2.142 (3)	O12—C57	1.255 (5)
N1—C10	1.489 (5)	O13—C55	1.242 (5)
N1—C7	1.490 (4)	O14—C55	1.244 (5)
N1—C16	1.518 (5)	N5—C45	1.495 (5)
N2—C18	1.450 (5)	N5—C36	1.513 (5)
N2—C24	1.458 (5)	N5—C39	1.547 (6)
N2—C9	1.492 (5)	N6—C38	1.396 (6)
N3—C11	1.317 (4)	N6—C47	1.500 (6)
N3—C15	1.325 (5)	N6—C53	1.546 (5)
N4—C23	1.326 (5)	N7—C44	1.299 (6)
N4—C19	1.358 (5)	N7—C40	1.334 (5)
O1—C1	1.285 (4)	N8—C52	1.354 (6)
O2—C17	1.395 (5)	N8—C48	1.361 (6)
O2—H2	0.76 (4)	C30—C35	1.388 (7)
O3—C25	1.415 (5)	C30—C31	1.439 (7)
O3—H3	0.84 (4)	C31—C32	1.366 (7)
O4—C28	1.221 (4)	C31—C36	1.493 (7)
O5—C28	1.238 (4)	C32—C33	1.407 (8)
O6—C26	1.233 (4)	C32—H32	0.9300
O7—C26	1.266 (4)	C33—C34	1.382 (8)
C1—C6	1.406 (5)	C33—C37	1.521 (7)
C1—C2	1.432 (5)	C34—C35	1.295 (7)
C2—C3	1.355 (6)	C34—H34	0.9300
C2—C9	1.506 (5)	C35—C38	1.559 (7)
C3—C4	1.353 (6)	C36—H36A	0.9700
C3—H3A	0.9300	C36—H36B	0.9700
C4—C5	1.390 (6)	C37—H37A	0.9600
C4—C8	1.486 (6)	C37—H37B	0.9600
C5—C6	1.357 (6)	C37—H37C	0.9600
C5—H5	0.9300	C38—H38A	0.9700
C6—C7	1.486 (6)	C38—H38B	0.9700
C7—H7A	0.9700	C39—C40	1.454 (7)
C7—H7B	0.9700	C39—H39A	0.9700
C8—H8A	0.9600	C39—H39B	0.9700
C8—H8B	0.9600	C40—C41	1.413 (6)
C8—H8C	0.9600	C41—C42	1.351 (7)
C9—H9A	0.9700	C41—H41	0.9300
C9—H9B	0.9700	C42—C43	1.272 (7)
C10—C11	1.449 (5)	C42—H42	0.9300
C10—H10A	0.9700	C43—C44	1.324 (6)
C10—H10B	0.9700	C43—H43	0.9300
C11—C12	1.322 (5)	C44—H44	0.9300
C12—C13	1.378 (7)	C45—C46	1.491 (6)
C12—H12	0.9300	C45—H45A	0.9700
C13—C14	1.336 (7)	C45—H45B	0.9700
C13—H13	0.9300	C46—H46A	0.9700
C14—C15	1.363 (6)	C46—H46B	0.9700
C14—H14	0.9300	C47—C48	1.440 (7)
C15—H15	0.9300	C47—H47A	0.9700
C16—C17	1.489 (6)	C47—H47B	0.9700
C16—H16A	0.9700	C48—C49	1.290 (7)
C16—H16B	0.9700	C49—C50	1.405 (8)
C17—H17A	0.9700	C49—H49	0.9300
C17—H17B	0.9700	C50—C51	1.375 (8)
C18—C19	1.492 (5)	C50—H50	0.9300
C18—H18A	0.9700	C51—C52	1.375 (7)
C18—H18B	0.9700	C51—H51	0.9300
C19—C20	1.338 (5)	C52—H52	0.9300
C20—C21	1.354 (7)	C53—C54	1.578 (6)
C20—H20	0.9300	C53—H53A	0.9700
C21—C22	1.357 (7)	C53—H53B	0.9700
C21—H21	0.9300	C54—H54A	0.9700
C22—C23	1.355 (6)	C54—H54B	0.9700
C22—H22	0.9300	C55—C56	1.513 (6)
C23—H23	0.9300	C56—H56A	0.9600
C24—C25	1.527 (5)	C56—H56B	0.9600
C24—H24A	0.9700	C56—H56C	0.9600
C24—H24B	0.9700	C57—C58	1.504 (6)
C25—H25A	0.9700	C58—H58A	0.9600
C25—H25B	0.9700	C58—H58B	0.9600
C26—C27	1.492 (5)	C58—H58C	0.9600
C27—H27A	0.9600	P1—F3	1.505 (3)
C27—H27C	0.9600	P1—F1	1.547 (3)
C27—H27B	0.9600	P1—F6	1.547 (3)
C28—C29	1.489 (5)	P1—F4	1.547 (4)
C29—H29A	0.9600	P1—F2	1.557 (3)
C29—H29B	0.9600	P1—F5	1.572 (3)
C29—H29C	0.9600	P2—F7	1.447 (3)
Ni3—O8	1.979 (3)	P2—F8	1.466 (3)
Ni3—O13	2.029 (3)	P2—F9	1.476 (3)
Ni3—N7	2.051 (3)	P2—F12	1.544 (3)
Ni3—O11	2.079 (3)	P2—F10	1.565 (3)
Ni3—O9	2.121 (3)	P2—F11	1.571 (3)
Ni3—N5	2.123 (3)	O15—H15A	0.85 (5)
Ni4—O8	1.983 (3)	O15—H15B	0.82 (5)
O4—Ni1—O1	96.93 (11)	O8—Ni4—N6	93.50 (13)
O4—Ni1—O6	93.29 (11)	O12—Ni4—N6	167.31 (14)
O1—Ni1—O6	88.79 (10)	O8—Ni4—N8	90.69 (12)
O4—Ni1—N3	93.73 (11)	O12—Ni4—N8	91.20 (14)
O1—Ni1—N3	91.37 (10)	N6—Ni4—N8	79.77 (15)
O6—Ni1—N3	172.90 (11)	O8—Ni4—O14	87.86 (11)
O4—Ni1—N1	167.49 (11)	O12—Ni4—O14	97.18 (12)
O1—Ni1—N1	93.54 (11)	N6—Ni4—O14	92.04 (14)
O6—Ni1—N1	93.74 (11)	N8—Ni4—O14	171.59 (14)
N3—Ni1—N1	79.17 (12)	O8—Ni4—O10	170.31 (11)
O4—Ni1—O2	91.60 (11)	O12—Ni4—O10	92.25 (12)
O1—Ni1—O2	169.49 (11)	N6—Ni4—O10	79.77 (14)
O6—Ni1—O2	84.60 (11)	N8—Ni4—O10	94.92 (14)
N3—Ni1—O2	94.19 (11)	O14—Ni4—O10	85.44 (12)
N1—Ni1—O2	78.78 (11)	C30—O8—Ni3	123.9 (3)
O1—Ni2—O7	95.89 (10)	C30—O8—Ni4	118.0 (2)
O1—Ni2—N4	93.86 (11)	Ni3—O8—Ni4	117.73 (13)
O7—Ni2—N4	91.00 (12)	C46—O9—Ni3	112.5 (2)
O1—Ni2—O5	93.70 (10)	C46—O9—H9	111 (3)
O7—Ni2—O5	89.50 (11)	Ni3—O9—H9	108 (3)
N4—Ni2—O5	172.33 (11)	C54—O10—Ni4	114.6 (3)
O1—Ni2—N2	91.87 (11)	C54—O10—H10	105 (4)
O7—Ni2—N2	169.39 (11)	Ni4—O10—H10	111 (4)
N4—Ni2—N2	81.24 (13)	C57—O11—Ni3	133.1 (3)
O5—Ni2—N2	97.23 (12)	C57—O12—Ni4	136.3 (3)
O1—Ni2—O3	168.01 (11)	C55—O13—Ni3	129.1 (3)
O7—Ni2—O3	95.08 (10)	C55—O14—Ni4	131.9 (3)
N4—Ni2—O3	90.76 (11)	C45—N5—C36	111.7 (3)
O5—Ni2—O3	81.57 (10)	C45—N5—C39	112.8 (3)
N2—Ni2—O3	77.90 (11)	C36—N5—C39	110.4 (3)
C10—N1—C7	111.6 (3)	C45—N5—Ni3	103.1 (2)
C10—N1—C16	109.9 (3)	C36—N5—Ni3	110.0 (2)
C7—N1—C16	112.7 (3)	C39—N5—Ni3	108.5 (3)
C10—N1—Ni1	111.3 (2)	C38—N6—C47	106.7 (4)
C7—N1—Ni1	106.6 (2)	C38—N6—C53	110.0 (4)
C16—N1—Ni1	104.5 (2)	C47—N6—C53	110.0 (3)
C18—N2—C24	111.8 (3)	C38—N6—Ni4	110.7 (3)
C18—N2—C9	109.9 (3)	C47—N6—Ni4	113.8 (3)
C24—N2—C9	112.0 (3)	C53—N6—Ni4	105.7 (3)
C18—N2—Ni2	110.0 (2)	C44—N7—C40	116.2 (4)
C24—N2—Ni2	104.3 (2)	C44—N7—Ni3	127.2 (3)
C9—N2—Ni2	108.5 (2)	C40—N7—Ni3	116.6 (3)
C11—N3—C15	118.4 (3)	C52—N8—C48	116.8 (4)
C11—N3—Ni1	116.2 (2)	C52—N8—Ni4	125.8 (3)
C15—N3—Ni1	125.3 (3)	C48—N8—Ni4	113.6 (3)
C23—N4—C19	117.0 (3)	O8—C30—C35	119.7 (4)
C23—N4—Ni2	127.3 (3)	O8—C30—C31	121.5 (4)
C19—N4—Ni2	115.7 (3)	C35—C30—C31	118.8 (4)
C1—O1—Ni2	124.0 (2)	C32—C31—C30	118.9 (5)
C1—O1—Ni1	119.6 (2)	C32—C31—C36	123.4 (5)
Ni2—O1—Ni1	116.40 (12)	C30—C31—C36	117.6 (4)
C17—O2—Ni1	113.3 (2)	C31—C32—C33	120.7 (5)
C17—O2—H2	107 (4)	C31—C32—H32	119.6
Ni1—O2—H2	109 (4)	C33—C32—H32	119.6
C25—O3—Ni2	114.5 (2)	C34—C33—C32	116.5 (5)
C25—O3—H3	113 (3)	C34—C33—C37	126.1 (6)
Ni2—O3—H3	102 (3)	C32—C33—C37	117.4 (6)
C28—O4—Ni1	135.8 (3)	C35—C34—C33	125.5 (5)
C28—O5—Ni2	129.3 (3)	C35—C34—H34	117.3
C26—O6—Ni1	133.3 (3)	C33—C34—H34	117.3
C26—O7—Ni2	130.1 (2)	C34—C35—C30	119.5 (5)
O1—C1—C6	123.5 (4)	C34—C35—C38	121.9 (5)
O1—C1—C2	120.9 (3)	C30—C35—C38	117.9 (4)
C6—C1—C2	115.5 (4)	C31—C36—N5	111.4 (4)
C3—C2—C1	121.7 (4)	C31—C36—H36A	109.3
C3—C2—C9	122.1 (4)	N5—C36—H36A	109.3
C1—C2—C9	116.3 (3)	C31—C36—H36B	109.3
C2—C3—C4	123.0 (4)	N5—C36—H36B	109.3
C2—C3—H3A	118.5	H36A—C36—H36B	108.0
C4—C3—H3A	118.5	C33—C37—H37A	109.5
C3—C4—C5	115.2 (4)	C33—C37—H37B	109.5
C3—C4—C8	123.8 (4)	H37A—C37—H37B	109.5
C5—C4—C8	121.0 (4)	C33—C37—H37C	109.5
C6—C5—C4	125.4 (4)	H37A—C37—H37C	109.5
C6—C5—H5	117.3	H37B—C37—H37C	109.5
C4—C5—H5	117.3	N6—C38—C35	114.8 (4)
C5—C6—C1	119.1 (4)	N6—C38—H38A	108.6
C5—C6—C7	124.5 (4)	C35—C38—H38A	108.6
C1—C6—C7	116.3 (4)	N6—C38—H38B	108.6
C6—C7—N1	113.0 (3)	C35—C38—H38B	108.6
C6—C7—H7A	109.0	H38A—C38—H38B	107.5
N1—C7—H7A	109.0	C40—C39—N5	114.3 (4)
C6—C7—H7B	109.0	C40—C39—H39A	108.7
N1—C7—H7B	109.0	N5—C39—H39A	108.7
H7A—C7—H7B	107.8	C40—C39—H39B	108.7
C4—C8—H8A	109.5	N5—C39—H39B	108.7
C4—C8—H8B	109.5	H39A—C39—H39B	107.6
H8A—C8—H8B	109.5	N7—C40—C41	122.1 (5)
C4—C8—H8C	109.5	N7—C40—C39	118.5 (4)
H8A—C8—H8C	109.5	C41—C40—C39	119.3 (4)
H8B—C8—H8C	109.5	C42—C41—C40	114.4 (4)
N2—C9—C2	115.7 (3)	C42—C41—H41	122.8
N2—C9—H9A	108.3	C40—C41—H41	122.8
C2—C9—H9A	108.3	C43—C42—C41	123.3 (5)
N2—C9—H9B	108.4	C43—C42—H42	118.3
C2—C9—H9B	108.4	C41—C42—H42	118.3
H9A—C9—H9B	107.4	C42—C43—C44	119.2 (6)
C11—C10—N1	112.6 (3)	C42—C43—H43	120.4
C11—C10—H10A	109.1	C44—C43—H43	120.4
N1—C10—H10A	109.1	N7—C44—C43	124.7 (5)
C11—C10—H10B	109.1	N7—C44—H44	117.7
N1—C10—H10B	109.1	C43—C44—H44	117.7
H10A—C10—H10B	107.8	C46—C45—N5	110.2 (3)
N3—C11—C12	121.8 (3)	C46—C45—H45A	109.6
N3—C11—C10	118.6 (3)	N5—C45—H45A	109.6
C12—C11—C10	119.5 (4)	C46—C45—H45B	109.6
C11—C12—C13	118.9 (4)	N5—C45—H45B	109.6
C11—C12—H12	120.5	H45A—C45—H45B	108.1
C13—C12—H12	120.5	O9—C46—C45	109.1 (3)
C14—C13—C12	121.1 (5)	O9—C46—H46A	109.9
C14—C13—H13	119.4	C45—C46—H46A	109.9
C12—C13—H13	119.4	O9—C46—H46B	109.9
C13—C14—C15	116.0 (4)	C45—C46—H46B	109.9
C13—C14—H14	122.0	H46A—C46—H46B	108.3
C15—C14—H14	122.0	C48—C47—N6	107.4 (4)
N3—C15—C14	123.6 (4)	C48—C47—H47A	110.2
N3—C15—H15	118.2	N6—C47—H47A	110.2
C14—C15—H15	118.2	C48—C47—H47B	110.2
C17—C16—N1	109.6 (3)	N6—C47—H47B	110.2
C17—C16—H16A	109.8	H47A—C47—H47B	108.5
N1—C16—H16A	109.8	C49—C48—N8	122.4 (5)
C17—C16—H16B	109.8	C49—C48—C47	119.1 (5)
N1—C16—H16B	109.8	N8—C48—C47	118.5 (4)
H16A—C16—H16B	108.2	C48—C49—C50	121.7 (6)
O2—C17—C16	111.9 (3)	C48—C49—H49	119.1
O2—C17—H17A	109.2	C50—C49—H49	119.1
C16—C17—H17A	109.2	C51—C50—C49	118.1 (6)
O2—C17—H17B	109.2	C51—C50—H50	121.0
C16—C17—H17B	109.2	C49—C50—H50	121.0
H17A—C17—H17B	107.9	C52—C51—C50	117.2 (5)
N2—C18—C19	115.9 (3)	C52—C51—H51	121.4
N2—C18—H18A	108.3	C50—C51—H51	121.4
C19—C18—H18A	108.3	N8—C52—C51	123.8 (4)
N2—C18—H18B	108.3	N8—C52—H52	118.1
C19—C18—H18B	108.3	C51—C52—H52	118.1
H18A—C18—H18B	107.4	N6—C53—C54	107.4 (3)
C20—C19—N4	122.0 (4)	N6—C53—H53A	110.2
C20—C19—C18	122.2 (4)	C54—C53—H53A	110.2
N4—C19—C18	115.7 (3)	N6—C53—H53B	110.2
C19—C20—C21	119.8 (4)	C54—C53—H53B	110.2
C19—C20—H20	120.1	H53A—C53—H53B	108.5
C21—C20—H20	120.1	O10—C54—C53	111.1 (3)
C20—C21—C22	119.4 (4)	O10—C54—H54A	109.4
C20—C21—H21	120.3	C53—C54—H54A	109.4
C22—C21—H21	120.3	O10—C54—H54B	109.4
C23—C22—C21	118.5 (5)	C53—C54—H54B	109.4
C23—C22—H22	120.7	H54A—C54—H54B	108.0
C21—C22—H22	120.7	O13—C55—O14	126.9 (4)
N4—C23—C22	123.2 (4)	O13—C55—C56	117.0 (4)
N4—C23—H23	118.4	O14—C55—C56	115.9 (4)
C22—C23—H23	118.4	C55—C56—H56A	109.5
N2—C24—C25	111.4 (3)	C55—C56—H56B	109.5
N2—C24—H24A	109.3	H56A—C56—H56B	109.5
C25—C24—H24A	109.3	C55—C56—H56C	109.5
N2—C24—H24B	109.3	H56A—C56—H56C	109.5
C25—C24—H24B	109.3	H56B—C56—H56C	109.5
H24A—C24—H24B	108.0	O11—C57—O12	124.1 (4)
O3—C25—C24	109.1 (3)	O11—C57—C58	117.9 (4)
O3—C25—H25A	109.9	O12—C57—C58	118.0 (4)
C24—C25—H25A	109.9	C57—C58—H58A	109.5
O3—C25—H25B	109.9	C57—C58—H58B	109.5
C24—C25—H25B	109.9	H58A—C58—H58B	109.5
H25A—C25—H25B	108.3	C57—C58—H58C	109.5
O6—C26—O7	124.2 (4)	H58A—C58—H58C	109.5
O6—C26—C27	118.5 (4)	H58B—C58—H58C	109.5
O7—C26—C27	117.2 (3)	F3—P1—F1	176.9 (2)
C26—C27—H27A	109.5	F3—P1—F6	90.5 (2)
C26—C27—H27C	109.5	F1—P1—F6	91.95 (18)
H27A—C27—H27C	109.5	F3—P1—F4	90.5 (2)
C26—C27—H27B	109.5	F1—P1—F4	91.35 (19)
H27A—C27—H27B	109.5	F6—P1—F4	87.96 (18)
H27C—C27—H27B	109.5	F3—P1—F2	89.04 (18)
O4—C28—O5	126.8 (4)	F1—P1—F2	89.10 (17)
O4—C28—C29	117.0 (3)	F6—P1—F2	91.28 (18)
O5—C28—C29	116.0 (4)	F4—P1—F2	179.1 (2)
C28—C29—H29A	109.5	F3—P1—F5	89.84 (18)
C28—C29—H29B	109.5	F1—P1—F5	87.73 (16)
H29A—C29—H29B	109.5	F6—P1—F5	179.2 (2)
C28—C29—H29C	109.5	F4—P1—F5	91.34 (17)
H29A—C29—H29C	109.5	F2—P1—F5	89.43 (17)
H29B—C29—H29C	109.5	F7—P2—F8	95.96 (19)
O8—Ni3—O13	96.61 (11)	F7—P2—F9	168.0 (2)
O8—Ni3—N7	94.24 (12)	F8—P2—F9	95.06 (19)
O13—Ni3—N7	92.22 (13)	F7—P2—F12	91.63 (19)
O8—Ni3—O11	93.21 (10)	F8—P2—F12	90.89 (18)
O13—Ni3—O11	89.51 (12)	F9—P2—F12	92.84 (19)
N7—Ni3—O11	172.11 (12)	F7—P2—F10	84.92 (18)
O8—Ni3—O9	170.19 (11)	F8—P2—F10	178.2 (2)
O13—Ni3—O9	92.44 (11)	F9—P2—F10	83.93 (18)
N7—Ni3—O9	89.18 (12)	F12—P2—F10	90.66 (18)
O11—Ni3—O9	83.06 (11)	F7—P2—F11	87.04 (18)
O8—Ni3—N5	91.19 (11)	F8—P2—F11	88.65 (17)
O13—Ni3—N5	170.59 (12)	F9—P2—F11	88.58 (18)
N7—Ni3—N5	81.93 (14)	F12—P2—F11	178.5 (2)
O11—Ni3—N5	95.32 (13)	F10—P2—F11	89.82 (17)
O9—Ni3—N5	80.17 (12)	H15A—O15—H15B	108 (5)
O8—Ni4—O12	95.53 (11)
O4—Ni1—N1—C10	−45.4 (7)	Ni2—O7—C26—C27	−152.0 (3)
O1—Ni1—N1—C10	101.6 (2)	Ni1—O4—C28—O5	15.7 (6)
O6—Ni1—N1—C10	−169.4 (2)	Ni1—O4—C28—C29	−168.7 (3)
N3—Ni1—N1—C10	10.9 (2)	Ni2—O5—C28—O4	8.6 (6)
O2—Ni1—N1—C10	−85.7 (2)	Ni2—O5—C28—C29	−167.1 (3)
O4—Ni1—N1—C7	−167.3 (5)	O13—Ni3—O8—C30	144.9 (3)
O1—Ni1—N1—C7	−20.4 (2)	N7—Ni3—O8—C30	52.2 (4)
O6—Ni1—N1—C7	68.7 (2)	O11—Ni3—O8—C30	−125.2 (3)
N3—Ni1—N1—C7	−111.1 (2)	N5—Ni3—O8—C30	−29.8 (3)
O2—Ni1—N1—C7	152.4 (2)	O13—Ni3—O8—Ni4	−42.25 (15)
O4—Ni1—N1—C16	73.2 (6)	N7—Ni3—O8—Ni4	−134.98 (15)
O1—Ni1—N1—C16	−139.9 (2)	O11—Ni3—O8—Ni4	47.62 (15)
O6—Ni1—N1—C16	−50.9 (3)	N5—Ni3—O8—Ni4	143.02 (15)
N3—Ni1—N1—C16	129.4 (3)	O12—Ni4—O8—C30	132.0 (3)
O2—Ni1—N1—C16	32.9 (2)	N6—Ni4—O8—C30	−39.1 (3)
O1—Ni2—N2—C18	102.7 (2)	N8—Ni4—O8—C30	40.7 (3)
O7—Ni2—N2—C18	−34.3 (8)	O14—Ni4—O8—C30	−131.0 (3)
N4—Ni2—N2—C18	9.1 (2)	O12—Ni4—O8—Ni3	−41.25 (15)
O5—Ni2—N2—C18	−163.3 (2)	N6—Ni4—O8—Ni3	147.68 (16)
O3—Ni2—N2—C18	−83.6 (2)	N8—Ni4—O8—Ni3	−132.53 (16)
O1—Ni2—N2—C24	−137.2 (2)	O14—Ni4—O8—Ni3	55.76 (15)
O7—Ni2—N2—C24	85.8 (7)	O13—Ni3—O9—C46	176.3 (3)
N4—Ni2—N2—C24	129.2 (2)	N7—Ni3—O9—C46	−91.5 (3)
O5—Ni2—N2—C24	−43.2 (2)	O11—Ni3—O9—C46	87.1 (3)
O3—Ni2—N2—C24	36.5 (2)	N5—Ni3—O9—C46	−9.6 (3)
O1—Ni2—N2—C9	−17.6 (2)	O12—Ni4—O10—C54	169.5 (3)
O7—Ni2—N2—C9	−154.7 (6)	N6—Ni4—O10—C54	−20.4 (3)
N4—Ni2—N2—C9	−111.3 (2)	N8—Ni4—O10—C54	−99.1 (3)
O5—Ni2—N2—C9	76.3 (2)	O14—Ni4—O10—C54	72.5 (3)
O3—Ni2—N2—C9	156.1 (3)	O8—Ni3—O11—C57	−30.1 (4)
O4—Ni1—N3—C11	165.9 (2)	O13—Ni3—O11—C57	66.4 (4)
O1—Ni1—N3—C11	−97.1 (2)	O9—Ni3—O11—C57	159.0 (4)
N1—Ni1—N3—C11	−3.7 (2)	N5—Ni3—O11—C57	−121.6 (4)
O2—Ni1—N3—C11	74.0 (2)	O8—Ni4—O12—C57	6.9 (4)
O4—Ni1—N3—C15	−18.4 (3)	N6—Ni4—O12—C57	142.0 (6)
O1—Ni1—N3—C15	78.6 (3)	N8—Ni4—O12—C57	97.7 (4)
N1—Ni1—N3—C15	172.0 (3)	O14—Ni4—O12—C57	−81.7 (4)
O2—Ni1—N3—C15	−110.3 (3)	O10—Ni4—O12—C57	−167.4 (4)
O1—Ni2—N4—C23	83.6 (3)	O8—Ni3—O13—C55	−4.0 (4)
O7—Ni2—N4—C23	−12.4 (3)	N7—Ni3—O13—C55	90.5 (4)
N2—Ni2—N4—C23	174.9 (4)	O11—Ni3—O13—C55	−97.2 (4)
O3—Ni2—N4—C23	−107.5 (3)	O9—Ni3—O13—C55	179.8 (4)
O1—Ni2—N4—C19	−95.2 (2)	O8—Ni4—O14—C55	−46.3 (4)
O7—Ni2—N4—C19	168.8 (2)	O12—Ni4—O14—C55	49.0 (4)
N2—Ni2—N4—C19	−3.9 (2)	N6—Ni4—O14—C55	−139.7 (4)
O3—Ni2—N4—C19	73.7 (2)	O10—Ni4—O14—C55	140.7 (4)
O7—Ni2—O1—C1	138.9 (3)	O8—Ni3—N5—C45	−142.3 (3)
N4—Ni2—O1—C1	47.5 (3)	N7—Ni3—N5—C45	123.6 (3)
O5—Ni2—O1—C1	−131.2 (3)	O11—Ni3—N5—C45	−48.9 (3)
N2—Ni2—O1—C1	−33.8 (3)	O9—Ni3—N5—C45	33.1 (3)
O3—Ni2—O1—C1	−64.9 (6)	O8—Ni3—N5—C36	−23.0 (3)
O7—Ni2—O1—Ni1	−41.94 (15)	N7—Ni3—N5—C36	−117.1 (3)
N4—Ni2—O1—Ni1	−133.35 (15)	O11—Ni3—N5—C36	70.4 (3)
O5—Ni2—O1—Ni1	47.94 (15)	O9—Ni3—N5—C36	152.3 (3)
N2—Ni2—O1—Ni1	145.31 (15)	O8—Ni3—N5—C39	97.9 (3)
O3—Ni2—O1—Ni1	114.2 (5)	N7—Ni3—N5—C39	3.8 (3)
O4—Ni1—O1—C1	142.1 (3)	O11—Ni3—N5—C39	−168.8 (3)
O6—Ni1—O1—C1	−124.7 (3)	O9—Ni3—N5—C39	−86.8 (3)
N3—Ni1—O1—C1	48.2 (3)	O8—Ni4—N6—C38	−16.5 (3)
N1—Ni1—O1—C1	−31.1 (3)	O12—Ni4—N6—C38	−151.8 (6)
O2—Ni1—O1—C1	−73.8 (7)	N8—Ni4—N6—C38	−106.5 (3)
O4—Ni1—O1—Ni2	−37.06 (15)	O14—Ni4—N6—C38	71.5 (3)
O6—Ni1—O1—Ni2	56.11 (14)	O10—Ni4—N6—C38	156.5 (3)
N3—Ni1—O1—Ni2	−130.99 (15)	O8—Ni4—N6—C47	103.7 (3)
N1—Ni1—O1—Ni2	149.78 (14)	O12—Ni4—N6—C47	−31.6 (8)
O2—Ni1—O1—Ni2	107.1 (6)	N8—Ni4—N6—C47	13.6 (3)
O4—Ni1—O2—C17	176.0 (3)	O14—Ni4—N6—C47	−168.3 (3)
O1—Ni1—O2—C17	31.6 (7)	O10—Ni4—N6—C47	−83.3 (3)
O6—Ni1—O2—C17	82.8 (3)	O8—Ni4—N6—C53	−135.5 (3)
N3—Ni1—O2—C17	−90.2 (3)	O12—Ni4—N6—C53	89.2 (7)
N1—Ni1—O2—C17	−12.1 (3)	N8—Ni4—N6—C53	134.4 (3)
O1—Ni2—O3—C25	14.3 (6)	O14—Ni4—N6—C53	−47.5 (3)
O7—Ni2—O3—C25	170.5 (3)	O10—Ni4—N6—C53	37.5 (3)
N4—Ni2—O3—C25	−98.5 (3)	O8—Ni3—N7—C44	88.3 (4)
O5—Ni2—O3—C25	81.7 (3)	O13—Ni3—N7—C44	−8.5 (4)
N2—Ni2—O3—C25	−17.6 (3)	O9—Ni3—N7—C44	−100.9 (4)
O1—Ni1—O4—C28	0.6 (4)	N5—Ni3—N7—C44	178.9 (4)
O6—Ni1—O4—C28	−88.5 (4)	O8—Ni3—N7—C40	−94.4 (3)
N3—Ni1—O4—C28	92.5 (4)	O13—Ni3—N7—C40	168.8 (3)
N1—Ni1—O4—C28	147.4 (5)	O9—Ni3—N7—C40	76.4 (3)
O2—Ni1—O4—C28	−173.2 (4)	N5—Ni3—N7—C40	−3.8 (3)
O1—Ni2—O5—C28	−38.6 (3)	O8—Ni4—N8—C52	65.7 (4)
O7—Ni2—O5—C28	57.3 (3)	O12—Ni4—N8—C52	−29.9 (4)
N2—Ni2—O5—C28	−130.9 (3)	N6—Ni4—N8—C52	159.1 (4)
O3—Ni2—O5—C28	152.5 (3)	O10—Ni4—N8—C52	−122.3 (4)
O4—Ni1—O6—C26	52.6 (3)	O8—Ni4—N8—C48	−91.4 (3)
O1—Ni1—O6—C26	−44.2 (3)	O12—Ni4—N8—C48	173.0 (3)
N1—Ni1—O6—C26	−137.7 (3)	N6—Ni4—N8—C48	2.0 (3)
O2—Ni1—O6—C26	143.9 (3)	O10—Ni4—N8—C48	80.7 (3)
O1—Ni2—O7—C26	−7.2 (3)	Ni3—O8—C30—C35	−132.8 (4)
N4—Ni2—O7—C26	86.8 (3)	Ni4—O8—C30—C35	54.4 (5)
O5—Ni2—O7—C26	−100.8 (3)	Ni3—O8—C30—C31	45.4 (6)
N2—Ni2—O7—C26	129.6 (6)	Ni4—O8—C30—C31	−127.4 (4)
O3—Ni2—O7—C26	177.7 (3)	O8—C30—C31—C32	179.5 (4)
Ni2—O1—C1—C6	−135.8 (3)	C35—C30—C31—C32	−2.3 (7)
Ni1—O1—C1—C6	45.1 (4)	O8—C30—C31—C36	1.4 (6)
Ni2—O1—C1—C2	45.9 (4)	C35—C30—C31—C36	179.6 (4)
Ni1—O1—C1—C2	−133.2 (3)	C30—C31—C32—C33	1.0 (7)
O1—C1—C2—C3	−178.3 (4)	C36—C31—C32—C33	179.1 (5)
C6—C1—C2—C3	3.3 (5)	C31—C32—C33—C34	−0.5 (8)
O1—C1—C2—C9	2.0 (5)	C31—C32—C33—C37	−179.0 (5)
C6—C1—C2—C9	−176.5 (3)	C32—C33—C34—C35	1.3 (8)
C1—C2—C3—C4	−3.8 (6)	C37—C33—C34—C35	179.6 (5)
C9—C2—C3—C4	176.0 (4)	C33—C34—C35—C30	−2.6 (8)
C2—C3—C4—C5	1.9 (6)	C33—C34—C35—C38	−172.7 (5)
C2—C3—C4—C8	−174.7 (4)	O8—C30—C35—C34	−178.8 (4)
C3—C4—C5—C6	0.2 (6)	C31—C30—C35—C34	3.0 (7)
C8—C4—C5—C6	176.9 (4)	O8—C30—C35—C38	−8.3 (7)
C4—C5—C6—C1	−0.4 (6)	C31—C30—C35—C38	173.5 (4)
C4—C5—C6—C7	177.7 (4)	C32—C31—C36—N5	120.5 (5)
O1—C1—C6—C5	−179.7 (3)	C30—C31—C36—N5	−61.4 (5)
C2—C1—C6—C5	−1.3 (5)	C45—N5—C36—C31	179.1 (3)
O1—C1—C6—C7	2.1 (5)	C39—N5—C36—C31	−54.6 (4)
C2—C1—C6—C7	−179.5 (3)	Ni3—N5—C36—C31	65.2 (4)
C5—C6—C7—N1	115.3 (4)	C47—N6—C38—C35	−65.0 (5)
C1—C6—C7—N1	−66.6 (4)	C53—N6—C38—C35	175.8 (4)
C10—N1—C7—C6	−55.9 (4)	Ni4—N6—C38—C35	59.4 (5)
C16—N1—C7—C6	179.9 (3)	C34—C35—C38—N6	113.3 (5)
Ni1—N1—C7—C6	65.9 (3)	C30—C35—C38—N6	−57.0 (6)
C18—N2—C9—C2	−58.2 (4)	C45—N5—C39—C40	−117.2 (4)
C24—N2—C9—C2	176.8 (3)	C36—N5—C39—C40	117.1 (4)
Ni2—N2—C9—C2	62.2 (4)	Ni3—N5—C39—C40	−3.6 (5)
C3—C2—C9—N2	117.5 (4)	C44—N7—C40—C41	1.2 (6)
C1—C2—C9—N2	−62.7 (4)	Ni3—N7—C40—C41	−176.4 (3)
C7—N1—C10—C11	102.6 (4)	C44—N7—C40—C39	−179.6 (4)
C16—N1—C10—C11	−131.6 (3)	Ni3—N7—C40—C39	2.8 (5)
Ni1—N1—C10—C11	−16.3 (4)	N5—C39—C40—N7	0.7 (6)
C15—N3—C11—C12	2.9 (5)	N5—C39—C40—C41	179.9 (4)
Ni1—N3—C11—C12	178.9 (3)	N7—C40—C41—C42	−1.7 (6)
C15—N3—C11—C10	179.1 (3)	C39—C40—C41—C42	179.1 (5)
Ni1—N3—C11—C10	−4.8 (4)	C40—C41—C42—C43	1.6 (8)
N1—C10—C11—N3	14.3 (5)	C41—C42—C43—C44	−1.0 (9)
N1—C10—C11—C12	−169.4 (4)	C40—N7—C44—C43	−0.5 (7)
N3—C11—C12—C13	−3.6 (7)	Ni3—N7—C44—C43	176.8 (4)
C10—C11—C12—C13	−179.9 (4)	C42—C43—C44—N7	0.4 (8)
C11—C12—C13—C14	2.2 (8)	C36—N5—C45—C46	−171.8 (3)
C12—C13—C14—C15	−0.1 (8)	C39—N5—C45—C46	63.2 (4)
C11—N3—C15—C14	−0.7 (6)	Ni3—N5—C45—C46	−53.7 (4)
Ni1—N3—C15—C14	−176.3 (3)	Ni3—O9—C46—C45	−17.1 (4)
C13—C14—C15—N3	−0.6 (7)	N5—C45—C46—O9	47.9 (5)
C10—N1—C16—C17	68.8 (4)	C38—N6—C47—C48	96.8 (5)
C7—N1—C16—C17	−166.0 (3)	C53—N6—C47—C48	−144.0 (4)
Ni1—N1—C16—C17	−50.7 (4)	Ni4—N6—C47—C48	−25.7 (5)
Ni1—O2—C17—C16	−13.3 (4)	C52—N8—C48—C49	2.0 (7)
N1—C16—C17—O2	43.1 (5)	Ni4—N8—C48—C49	161.3 (5)
C24—N2—C18—C19	−128.5 (3)	C52—N8—C48—C47	−178.0 (4)
C9—N2—C18—C19	106.4 (4)	Ni4—N8—C48—C47	−18.7 (6)
Ni2—N2—C18—C19	−13.1 (4)	N6—C47—C48—C49	−151.1 (5)
C23—N4—C19—C20	2.3 (5)	N6—C47—C48—N8	28.9 (6)
Ni2—N4—C19—C20	−178.8 (3)	N8—C48—C49—C50	−1.4 (9)
C23—N4—C19—C18	178.9 (3)	C47—C48—C49—C50	178.6 (6)
Ni2—N4—C19—C18	−2.2 (4)	C48—C49—C50—C51	0.4 (10)
N2—C18—C19—C20	−172.8 (4)	C49—C50—C51—C52	0.0 (9)
N2—C18—C19—N4	10.6 (5)	C48—N8—C52—C51	−1.6 (7)
N4—C19—C20—C21	−2.0 (6)	Ni4—N8—C52—C51	−158.1 (4)
C18—C19—C20—C21	−178.4 (4)	C50—C51—C52—N8	0.7 (9)
C19—C20—C21—C22	1.4 (8)	C38—N6—C53—C54	−168.8 (4)
C20—C21—C22—C23	−1.1 (8)	C47—N6—C53—C54	74.0 (4)
C19—N4—C23—C22	−2.0 (6)	Ni4—N6—C53—C54	−49.2 (4)
Ni2—N4—C23—C22	179.2 (4)	Ni4—O10—C54—C53	−3.1 (4)
C21—C22—C23—N4	1.5 (8)	N6—C53—C54—O10	34.1 (5)
C18—N2—C24—C25	66.8 (4)	Ni3—O13—C55—O14	22.5 (7)
C9—N2—C24—C25	−169.3 (3)	Ni3—O13—C55—C56	−153.2 (3)
Ni2—N2—C24—C25	−52.1 (4)	Ni4—O14—C55—O13	9.5 (7)
Ni2—O3—C25—C24	−5.6 (4)	Ni4—O14—C55—C56	−174.7 (3)
N2—C24—C25—O3	38.9 (5)	Ni3—O11—C57—O12	0.3 (7)
Ni1—O6—C26—O7	3.4 (6)	Ni3—O11—C57—C58	178.6 (3)
Ni1—O6—C26—C27	−175.3 (3)	Ni4—O12—C57—O11	14.9 (7)
Ni2—O7—C26—O6	29.3 (5)	Ni4—O12—C57—C58	−163.4 (3)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O2—H2···O15	0.76 (4)	2.48 (5)	2.956 (4)	122 (4)
O3—H3···O13	0.84 (4)	2.11 (4)	2.714 (4)	129 (4)
O9—H9···O7	0.80 (4)	2.04 (4)	2.737 (4)	145 (4)
O10—H10···O15^i	0.81 (5)	2.39 (5)	2.876 (5)	120 (4)
O15—H15A···O10^ii	0.85 (5)	2.48 (5)	2.876 (5)	109 (4)
O15—H15A···O5^iii	0.85 (5)	2.58 (5)	3.079 (4)	118 (4)
O15—H15B···O9^iii	0.82 (5)	2.22 (5)	3.009 (4)	162 (5)
C8—H8C···F1^iv	0.96	2.69	3.466 (5)	139
C10—H10A···F12	0.97	2.52	3.348 (5)	143
C14—H14···F5	0.93	2.48	3.355 (6)	158
C22—H22···F4^v	0.93	2.52	3.377 (5)	154
C29—H29B···O15^iii	0.96	2.54	3.209 (5)	127
C34—H34···F11^vi	0.93	2.66	3.479 (6)	148
C39—H39A···F2^iii	0.97	2.42	3.370 (6)	166
C46—H46A···O4^iii	0.97	2.61	3.373 (5)	136
C47—H47A···F4^vii	0.97	2.54	3.267 (6)	132
C54—H54B···F6^vii	0.97	2.50	3.406 (6)	155
C58—H58A···F7^iii	0.96	2.57	3.491 (5)	162
C58—H58B···O12^vii	0.96	2.56	3.293 (5)	133

Symmetry codes: (i) x−1, y, z; (ii) x+1, y, z; (iii) −x+1, −y+2, −z+1; (iv) −x+1, y−1/2, −z+1/2; (v) x, −y+3/2, z+1/2; (vi) x−1, −y+3/2, z+1/2; (vii) −x, −y+2, −z+1.