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ISSN: 2056-9890

Crystal structures of two dimeric nickel di­phenyl­acetate com­plexes

aSt Petersburg State Institute of Technology, Moskovsky pr. 26, 190013 St Petersburg, Russian Federation, bInstitute of Macromolecular Compounds, Russian Academy of Sciences, Bolshoy pr. 31, 199004 St Petersburg, Russian Federation, cSt Petersburg State University, University Emb. 7/9, 199034, St Petersburg, Russian Federation, and dPeter the Great St Petersburg Polytechnic University, Polytechnicheskaya 29, 195251 St Petersburg, Russian Federation
*Correspondence e-mail: ha9room@gmail.com

Edited by H. Stoeckli-Evans, University of Neuchâtel, Switzerland (Received 30 September 2019; accepted 15 October 2019; online 29 October 2019)

In the crystal structures of the title com­pounds, namely μ-aqua-κ2O:O-di-μ-di­phenyl­acetato-κ4O:O′-bis­[(di­phenyl­acetato-κO)bis­(pyridine-κN)nickel(II)], [Ni2(C14H11O2)4(C5H5N)4(H2O)] (1) and μ-aqua-κ2O:O-di-μ-di­phenyl­acetato-κ4O:O′-bis­[(2,2′-bi­pyridine-κ2N,N′)(di­phenyl­acetato-κO)nickel(II)]–aceto­nitrile–di­phenyl­acetic acid (1/2.5/1), [Ni2(C14H11O2)4(C10H8N2)2(H2O)]·2.5CH3CN·C14H12O2 (2), the com­plex units are stabilized by a variety of intra- and inter­molecular hydrogen bonds, as well as C—H⋯π and ππ contacts between the aromatic systems of the pyridine, dipyridyl and di­phenyl­acetate ligands. Despite the fact that the di­phenyl­acetate ligand is sterically bulky, this does not inter­fere with the formation of the described aqua-bridged dimeric core, even with a 2,2′-bi­pyridine ligand, which has a strong chelating effect.

1. Chemical context

The title com­pounds, 1 and 2, were synthesized as a part of our ongoing research on catalytically active polynuclear NiII and CoII carboxyl­ate com­plexes with various structures and nuclearity in lactone ring-opening polymerization and ketone hydro­silylation. They belong to the type of aqua-bridged dinickel(II) carboxyl­ates with the general formula [MII2(μ-H2O)(μ-O2CR)2(O2CR)2Ln] (n = 4 in the case of a monodentate ligand or 2 in the case of bidentate coordination), well known since the 1970s (Turpeinen, 1976[Turpeinen, U. (1976). Finn. Chem. Lett. p. 173.]). In this work, it is shown that the reaction of highly reactive synthetic hellyerite, NiCO3·5.5H2O (Bette et al., 2016[Bette, S., Rincke, C., Dinnebier, R. E. & Voigt, W. (2016). Z. Anorg. Allg. Chem. 642, 652-659.]), a stoichiometric amount of di­phenyl­acetic acid and treatment with the N-donor ligand leads to self-assembly of the title com­pounds. The use of sterically bulky ligands and ligands that are prone to the formation of multiple intra- and inter­molecular inter­actions can give unexpected and inter­esting results (Lee et al., 2002[Lee, D., Hung, P.-L., Spingler, B. & Lippard, S. J. (2002). Inorg. Chem. 41, 521-531.]; Nikolaevskii et al., 2016[Nikolaevskii, S. A., Kiskin, M. A., Starikova, A. A., Efimov, N. N., Sidorov, A. A., Novotortsev, V. M. & Eremenko, I. L. (2016). Russ. Chem. Bull. 65, 2812-2819.]).

2. Structural commentary

In the title binuclear com­plexes, 1 and 2, each NiII ion is six-coordinated by two carboxyl­ate O atoms from two bidentate-bridged di­phenyl­acetate ligands, one O atom from a monodentate di­phenyl­acetate ligand, two N atoms from two pyridine (Py) (for 1) or one 2,2′-bi­pyridine (Bipy) ligand (for 2) and one O atom from a bridging aqua ligand in an octa­hedral geometry (Figs. 1[link] and 2[link]). The com­plexes display idealized twofold symmetry, with the axis passing through the bridging water mol­ecule. The Ni⋯Ni distances in the com­plexes are 3.5779 (4) (for 1) and 3.4826 (5) Å (for 2). Each monodentate coordinated di­phenyl­acetate ligand is involved in the formation of an intra­molecular hydrogen bond with a bridging water mol­ecule. Hydrogen-bond geometries are specified in Tables 1[link] and 2[link].

[Scheme 1]

Table 1
Hydrogen-bond geometry (Å, °) for 1[link]

D—H⋯A D—H H⋯A DA D—H⋯A
O9—H9A⋯O2 0.85 (2) 1.79 (2) 2.6201 (15) 165 (2)
O9—H9B⋯O8 0.87 (3) 1.70 (3) 2.5617 (14) 169 (2)
C8—H8⋯O8i 0.93 2.39 3.211 (2) 148
C12—H12⋯O2ii 0.93 2.46 3.302 (2) 151
Symmetry codes: (i) -x+2, -y+1, -z+1; (ii) -x+1, -y+1, -z+1.

Table 2
Hydrogen-bond geometry (Å, °) for 2[link]

D—H⋯A D—H H⋯A DA D—H⋯A
O9—H9A⋯O8 0.91 (3) 1.74 (3) 2.6461 (16) 173 (2)
O9—H9B⋯O2 0.96 (3) 1.53 (3) 2.4777 (15) 169 (3)
O11—H11A⋯O8 0.82 1.76 2.5599 (16) 164
C4—H4⋯O5i 0.93 2.48 3.3253 (19) 152
C17—H17⋯O4ii 0.93 2.48 3.3493 (19) 155
Symmetry codes: (i) -x+1, -y+1, -z+2; (ii) -x+1, -y+2, -z+1.
[Figure 1]
Figure 1
The mol­ecular structure of 1, showing the atom-labelling scheme. Displacement ellipsoids are drawn at the 50% probability level. H atoms have been omitted for clarity.
[Figure 2]
Figure 2
The mol­ecular structure of 2, showing the atom-labelling scheme. Displacement ellipsoids are drawn at the 50% probability level. H atoms and solvent mol­ecules have been omitted for clarity.

3. Supra­molecular features

In the crystal packing of com­pound 1, mol­ecules are combined into pairs connected by a centre of symmetry using offset face-to-face ππ stacking inter­actions, in which coordinated pyridine ligands of each com­plex [the N1/C1–C5⋯N1iii/C1iii–C5iii plane-to-plane distance = 3.342 Å; symmetry code: (iii) −x + 2, −y + 1, −z] are involved. These pairs, which result from the intermolecular hydrogen bonds between Py ligands and O atoms of carbonyl groups of di­phenyl­acetate ligands [C8—H8⋯O8i and C12—H12⋯O2ii; symmetry codes: (i) −x + 1, −y + 1, −z + 1; (ii) −x + 1, −y + 1, −z + 1], form layered structures parallel to the (101) plane. The layers form a 3D supra­molecular structure through inter­molecular C—H⋯π contacts, as well as ππ stacking inter­actions between the phenyl substituents of di­phenyl­acetate ligands [C57—C62⋯Cg1iv, plane-to-centroid distance = 3.231 Å; Cg1 is the centroid of the C57A–C62A ring; symmetry code: (iv) −x + 2, −y + 2, −z].

In the crystal structure of com­pound 2, each mol­ecule of the com­plex is associated with two neighbouring mol­ecules via ππ stacking inter­actions between Bipy ligands [N1—N2⋯N1i—N2i and N3—N4⋯N3ii—N4ii, plane-to-plane distances = 3.342 (2) and 3.310 (1) Å, respectively; symmetry codes: (i) −x + 1, −y + 1, −z + 2; (ii) −x + 1, −y + 2, −z + 1]. As a result, polymer chains are formed along the [01[\overline{1}]] direction, in which every pair of neighbouring mol­ecules is connected by a centre of symmetry. The chains are linked through C—H⋯π inter­actions of phenyl substituents of di­phenyl­acetate ligands and thereby form a three-dimensional supra­molecular framework. Aceto­nitrile solvent mol­ecules are associated with com­plex units via van der Waals inter­actions.

4. Hirshfeld surface analysis

In order to visualize and qu­anti­tatively describe inter­molecular inter­actions in the crystal packing of com­plexes 1 and 2, Hirshfeld surface analysis (Spackman & Jayatilaka, 2009[Spackman, M. A. & Jayatilaka, D. (2009). CrystEngComm, 11, 19-32.]) and two-dimensional fingerprint plots (McKinnon et al., 2007[McKinnon, J. J., Jayatilaka, D. & Spackman, M. A. (2007). Chem. Commun. pp. 3814-3816.]) were carried out and generated using CrystalExplorer (Version 17; Turner et al., 2017[Turner, M. J., McKinnon, J. J., Wolff, S. K., Grimwood, D. J., Spackman, P. R., Jayatilaka, D. & Spackman, M. A. (2017). CrystalExplorer17. University of Western Australia.]). The percentage contributions of the inter­molecular inter­actions to the Hirshfeld surface are shown in Figs. 3[link] (for 1) and 4[link] (for 2).

[Figure 3]
Figure 3
The two-dimensional fingerprint plots for com­pound 1.
[Figure 4]
Figure 4
The two-dimensional fingerprint plots for com­pound 2.

For com­pound 1, the largest bright-red spots on the Hirshfeld surface near the phenyl substituents (C37–C42, C37A–C42A and C43–C48) of the di­phenyl­acetate ligands (Fig. 5[link]a) are indicative of C—H⋯π inter­actions. Such spots are associated with disorder of the aforementioned phenyl substituents. In addition, other bright-red zones correspond to the weak hydrogen bonds C8—H8⋯O8ii and C12—H12⋯O2iii (Fig. 5[link]b and Table 1[link]).

[Figure 5]
Figure 5
The Hirshfeld surface mapped over dnorm for com­pound 1 in the range −0.4078 to 1.4837 a.u.

On the surface over shape index (Fig. 6[link]), areas highlighted by white ellipses and blue and red triangles united along a common vertex are observed, which confirms the presence of close C⋯C inter­planar contacts and, therefore, ππ stacking inter­actions between Py ligands.

[Figure 6]
Figure 6
Hirshfeld surface of com­pound 1 plotted over shape-index.

For com­pound 2, the bright-red spots on the Hirshfeld surface correspond to hydrogen bond O11—H11A⋯O8 with the di­phenyl­acetic acid mol­ecule, as well as weak C4—H4⋯O5i and C17—H17⋯O4ii hydrogen bonds between the O atoms of bridged di­phenyl­acetate ligands and Bipy ligands (Fig. 7[link] and Table 2[link]). Other observed red spots correspond to C—H⋯π inter­actions between the phenyl substituents of di­phenyl­acetate ligands [C67—H67⋯Cg2iii and C61—H61⋯C68iv; Cg2 is the centroid of the C23–C28 ring; symmetry codes: (iii) x + 1, y, z; (iv) −x + 2, −y + 1, −z + 1], as well as N⋯H inter­actions involving aceto­nitrile solvent mol­ecules [C59—H59⋯N7Ai; symmetry code: (i) −x + 1, −y + 1, −z + 2].

[Figure 7]
Figure 7
The Hirshfeld surface mapped over dnorm for com­pound 2 in the range −0.7804 to 1.5753 a.u.

As in the case of com­plex 1, close C⋯C inter­planar contacts, responsible for ππ stacking inter­actions between Bipy ligands, are displayed as patches of combined blue and red triangles on the surface over shape index (Fig. 8[link]).

[Figure 8]
Figure 8
Hirshfeld surface of com­pound 2 plotted over shape-index.

5. Database survey

A search in the Cambridge Structural Database (CSD, Version 5.40, updated February 2019; Groom et al., 2016[Groom, C. R., Bruno, I. J., Lightfoot, M. P. & Ward, S. C. (2016). Acta Cryst. B72, 171-179.]) for di­phenyl­acetate com­plexes of transition metals reveals that 54 original structures have been reported. Ten of them are homonuclear com­plexes of Fe, Co and Ni with nuclearity from 3 to 12 and eight of them include the M2(μ-O2CCHPh2) fragment and no binuclear structures were found. A survey of the CSD reveals 46 related structures of NiII carboxyl­ates with a similar structure fragment.

6. Synthesis and crystallization

6.1. Compound 1

A suspension of synthetic hellyerite, NiCO3·5.5H2O (0.653 g, 3.0 mmol), in aceto­nitrile (40 ml) was added to a solution of di­phenyl­acetic acid (1.274 g, 6.0 mmol) in 10 ml aceto­nitrile. After full conversion of hellyerite, pyridine (0.485 ml, 6.0 mmol) was added and the solution was refluxed for 15 min. The resulting pale-green–blue solution was cooled to room temperature and filtered. After a few days, blue crystals of 1 were collected by filtration (yield ∼70%).

6.2. Compound 2

The synthesis of com­pound 2 was carried out in a similar manner to the synthesis of com­pound 1, but 2,2′-bi­pyridine (0.469 g, 3.0 mmol) was added instead of pyridine. The resulting blue solution was cooled to room temperature and filtered. After a few days, blue crystals of 2 were collected by filtration (yield ∼60%).

7. Refinement

Crystal data, data collection and structure refinement details are summarized in Table 3[link]. The H atoms of the water mol­ecules were located in difference Fourier maps and refined freely. The other H atoms were placed in calculated positions and refined using a riding model, with C—H = 0.98 Å and Uiso(H) = 1.2Ueq(C) for the tertiary C atoms, C—H = 0.93 Å and Uiso(H) = 1.2Ueq(C) for aromatic C atoms, and C—H = 0.96 Å and Uiso(H) = 1.5Ueq(C) for methyl groups.

Table 3
Experimental details

  1 2
Crystal data
Chemical formula [Ni2(C14H11O2)4(C5H5N)4(H2O)] [Ni2(C14H11O2)4(C10H8N2)2(H2O)]·2.5C2H3N·C14H12O2
Mr 1296.74 1607.58
Crystal system, space group Triclinic, P[\overline{1}] Triclinic, P[\overline{1}]
Temperature (K) 100 100
a, b, c (Å) 13.2138 (2), 14.1981 (2), 17.5370 (2) 15.6064 (3), 17.7440 (4), 17.9143 (4)
α, β, γ (°) 82.696 (1), 80.002 (1), 80.784 (1) 70.462 (2), 69.631 (2), 64.726 (2)
V3) 3181.60 (8) 4103.17 (18)
Z 2 2
Radiation type Cu Kα Cu Kα
μ (mm−1) 1.25 1.10
Crystal size (mm) 0.21 × 0.13 × 0.07 0.22 × 0.14 × 0.08
 
Data collection
Diffractometer Rigaku SuperNova, Single source at offset/far, HyPix3000 Rigaku SuperNova, Single source at offset/far, HyPix3000
Absorption correction Multi-scan (CrysAlis PRO; Rigaku OD, 2017[Rigaku OD (2017). CrysAlis PRO. Rigaku Oxford Diffaction, Tokyo, Japan.]) Multi-scan (CrysAlis PRO; Rigaku OD, 2017[Rigaku OD (2017). CrysAlis PRO. Rigaku Oxford Diffaction, Tokyo, Japan.])
Tmin, Tmax 0.815, 1.000 0.809, 1.000
No. of measured, independent and observed [I > 2σ(I)] reflections 35511, 11971, 11154 52698, 15557, 13874
Rint 0.031 0.045
(sin θ/λ)max−1) 0.609 0.609
 
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.034, 0.088, 1.03 0.038, 0.103, 1.06
No. of reflections 11971 15557
No. of parameters 949 1079
No. of restraints 42 1
H-atom treatment H atoms treated by a mixture of independent and constrained refinement H atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å−3) 0.32, −0.44 0.48, −0.57
Computer programs: CrysAlis PRO (Rigaku OD, 2017[Rigaku OD (2017). CrysAlis PRO. Rigaku Oxford Diffaction, Tokyo, Japan.]), SHELXT (Sheldrick, 2015a[Sheldrick, G. M. (2015a). Acta Cryst. A71, 3-8.]), SHELXL (Sheldrick, 2015b[Sheldrick, G. M. (2015b). Acta Cryst. C71, 3-8.]), DIAMOND (Brandenburg, 2012[Brandenburg, K. (2012). DIAMOND. Crystal Impact GbR, Bonn, Germany.]) and OLEX2 (Dolomanov et al., 2009[Dolomanov, O. V., Bourhis, L. J., Gildea, R. J., Howard, J. A. K. & Puschmann, H. (2009). J. Appl. Cryst. 42, 339-341.]).

Supporting information


Computing details top

For both structures, data collection: CrysAlis PRO (Rigaku OD, 2017); cell refinement: CrysAlis PRO (Rigaku OD, 2017); data reduction: CrysAlis PRO (Rigaku OD, 2017); program(s) used to solve structure: SHELXT (Sheldrick, 2015a); program(s) used to refine structure: SHELXL (Sheldrick, 2015b); molecular graphics: OLEX2 (Dolomanov et al., 2009) and DIAMOND (Brandenburg, 2012); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009).

µ-Aqua-κ2O:O-di-µ-diphenylacetato-κ4O:O'-bis[(diphenylacetato-κO)bis(pyridine-κN)nickel(II)] (1) top
Crystal data top
[Ni2(C14H11O2)4(C5H5N)4(H2O)]Z = 2
Mr = 1296.74F(000) = 1356
Triclinic, P1Dx = 1.354 Mg m3
a = 13.2138 (2) ÅCu Kα radiation, λ = 1.54184 Å
b = 14.1981 (2) ÅCell parameters from 25598 reflections
c = 17.5370 (2) Åθ = 2.5–72.0°
α = 82.696 (1)°µ = 1.25 mm1
β = 80.002 (1)°T = 100 K
γ = 80.784 (1)°Prism, light green
V = 3181.60 (8) Å30.21 × 0.13 × 0.07 mm
Data collection top
SuperNova, Single source at offset/far, HyPix3000
diffractometer
11971 independent reflections
Radiation source: micro-focus sealed X-ray tube, SuperNova (Cu) X-ray Source11154 reflections with I > 2σ(I)
Mirror monochromatorRint = 0.031
ω scansθmax = 70.0°, θmin = 2.6°
Absorption correction: multi-scan
(CrysAlis PRO; Rigaku OD, 2017)
h = 1516
Tmin = 0.815, Tmax = 1.000k = 1717
35511 measured reflectionsl = 2021
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: mixed
R[F2 > 2σ(F2)] = 0.034H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.088 w = 1/[σ2(Fo2) + (0.0414P)2 + 1.5925P]
where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max < 0.001
11971 reflectionsΔρmax = 0.32 e Å3
949 parametersΔρmin = 0.44 e Å3
42 restraintsExtinction correction: (SHELXL-2018/3; Sheldrick 2015b), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: dualExtinction coefficient: 0.00100 (6)
Special details top

Geometry. 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ni10.86036 (2)0.56693 (2)0.22819 (2)0.01538 (7)
Ni20.63704 (2)0.71634 (2)0.31544 (2)0.01813 (7)
O10.83261 (8)0.42908 (7)0.22669 (6)0.0203 (2)
O20.70924 (8)0.41090 (8)0.33058 (6)0.0261 (2)
O30.75989 (7)0.61255 (7)0.14928 (6)0.0195 (2)
O40.61190 (8)0.69087 (8)0.21025 (6)0.0237 (2)
O50.90084 (8)0.69794 (7)0.22860 (6)0.0207 (2)
O60.75619 (8)0.79440 (8)0.27245 (6)0.0251 (2)
O70.65566 (8)0.75227 (7)0.42278 (6)0.0191 (2)
O80.79419 (8)0.64488 (7)0.44359 (6)0.0229 (2)
O90.74232 (8)0.58900 (8)0.32440 (6)0.0177 (2)
H9A0.7221 (16)0.5342 (16)0.3318 (12)0.038 (6)*
H9B0.7648 (18)0.6012 (17)0.3656 (15)0.051 (6)*
N10.98037 (9)0.54472 (8)0.13464 (7)0.0173 (2)
N20.97001 (9)0.51567 (9)0.30433 (7)0.0204 (3)
N30.51229 (9)0.64273 (10)0.36897 (7)0.0225 (3)
N40.53887 (10)0.84630 (10)0.30576 (7)0.0261 (3)
C11.00564 (12)0.61720 (11)0.08151 (8)0.0211 (3)
H10.9689000.6781700.0870350.025*
C21.08438 (12)0.60480 (12)0.01866 (9)0.0249 (3)
H21.1007830.6568580.0166390.030*
C31.13811 (12)0.51440 (12)0.00909 (9)0.0246 (3)
H31.1895900.5039620.0336280.030*
C41.11372 (12)0.43957 (11)0.06445 (9)0.0246 (3)
H41.1496420.3780690.0601630.029*
C51.03497 (11)0.45756 (10)0.12640 (9)0.0203 (3)
H51.0193960.4071390.1637370.024*
C60.95013 (12)0.45687 (11)0.36959 (9)0.0234 (3)
H60.8868010.4334410.3806250.028*
C71.02039 (14)0.42979 (12)0.42112 (9)0.0293 (4)
H71.0039930.3892700.4660790.035*
C81.11481 (14)0.46336 (12)0.40527 (10)0.0318 (4)
H81.1627270.4463630.4394600.038*
C91.13695 (13)0.52269 (13)0.33768 (10)0.0301 (4)
H91.2003960.5458150.3250840.036*
C101.06261 (12)0.54709 (11)0.28896 (9)0.0243 (3)
H101.0776630.5871410.2434770.029*
C110.46124 (13)0.66469 (14)0.43870 (10)0.0338 (4)
H110.4769100.7171690.4588650.041*
C120.38673 (14)0.61388 (16)0.48233 (11)0.0415 (5)
H120.3540590.6310470.5309780.050*
C130.36170 (14)0.53689 (15)0.45212 (11)0.0389 (4)
H130.3127260.5003770.4804760.047*
C140.41074 (13)0.51523 (13)0.37911 (12)0.0360 (4)
H140.3936210.4651720.3566500.043*
C150.48575 (12)0.56905 (12)0.33978 (10)0.0286 (3)
H150.5192490.5534000.2909080.034*
C160.56963 (14)0.92724 (12)0.32038 (10)0.0312 (4)
H160.6336900.9231540.3366320.037*
C170.50984 (17)1.01630 (14)0.31223 (12)0.0443 (5)
H170.5337111.0709450.3222760.053*
C180.41458 (19)1.02259 (16)0.28903 (12)0.0544 (6)
H180.3726501.0815060.2838040.065*
C190.38216 (18)0.94072 (18)0.27368 (12)0.0568 (7)
H190.3181440.9435280.2576650.068*
C200.44654 (15)0.85328 (15)0.28244 (10)0.0406 (5)
H200.4245390.7980300.2717050.049*
C210.77488 (11)0.38012 (10)0.27535 (8)0.0189 (3)
C220.78915 (11)0.27192 (10)0.26665 (9)0.0210 (3)
H220.7549560.2410030.3153490.025*
C230.73781 (11)0.24837 (11)0.20167 (9)0.0226 (3)
C240.71461 (14)0.15525 (13)0.20423 (10)0.0326 (4)
H240.7311820.1100380.2450430.039*
C250.66754 (16)0.12921 (15)0.14723 (11)0.0440 (5)
H250.6520250.0671010.1502150.053*
C260.64343 (15)0.19529 (16)0.08575 (11)0.0426 (5)
H260.6120920.1776700.0471820.051*
C270.66614 (14)0.28780 (15)0.08184 (10)0.0346 (4)
H270.6500240.3323890.0405240.042*
C280.71314 (12)0.31440 (12)0.13966 (9)0.0267 (3)
H280.7280620.3767140.1366920.032*
C290.90422 (12)0.23236 (10)0.25944 (9)0.0221 (3)
C300.95005 (12)0.21158 (11)0.32657 (10)0.0255 (3)
H300.9095150.2192550.3749260.031*
C311.05549 (13)0.17957 (12)0.32195 (11)0.0318 (4)
H311.0852840.1659480.3671200.038*
C321.11661 (13)0.16781 (12)0.25025 (11)0.0323 (4)
H321.1874110.1466540.2471430.039*
C331.07188 (13)0.18766 (12)0.18344 (11)0.0322 (4)
H331.1126170.1796120.1352170.039*
C340.96625 (13)0.21961 (12)0.18800 (10)0.0290 (3)
H340.9367230.2326060.1426900.035*
C350.66876 (11)0.65485 (10)0.15315 (8)0.0176 (3)
C360.61982 (11)0.66467 (11)0.07811 (8)0.0193 (3)
H360.6643990.6182370.0456420.023*0.540 (5)
H36A0.6535600.6133640.0459600.023*0.460 (5)
C370.5100 (7)0.6270 (4)0.0969 (4)0.0173 (10)0.540 (5)
C37A0.5095 (8)0.6602 (4)0.0965 (6)0.0173 (10)0.460 (5)
C380.4230 (3)0.6850 (3)0.1284 (2)0.0284 (8)0.540 (5)
H380.4272920.7479190.1357410.034*0.540 (5)
C38A0.4336 (3)0.7400 (4)0.1143 (2)0.0291 (10)0.460 (5)
H38A0.4537070.8002080.1120940.035*0.460 (5)
C390.3275 (4)0.6491 (5)0.1496 (4)0.0381 (14)0.540 (5)
H390.2689120.6871490.1724540.046*0.540 (5)
C39A0.3299 (3)0.7294 (5)0.1351 (2)0.0477 (15)0.460 (5)
H39A0.2810060.7822420.1475260.057*0.460 (5)
C400.3223 (4)0.5562 (4)0.1356 (3)0.0387 (11)0.540 (5)
H400.2595730.5318900.1487030.046*0.540 (5)
C40A0.2988 (6)0.6408 (9)0.1373 (5)0.056 (2)0.460 (5)
H40A0.2286150.6346380.1494770.067*0.460 (5)
C410.4082 (3)0.5006 (3)0.1031 (2)0.0404 (10)0.540 (5)
H410.4038930.4386350.0932660.048*0.540 (5)
C41A0.3693 (6)0.5629 (6)0.1219 (4)0.057 (2)0.460 (5)
H41A0.3481260.5030560.1243390.068*0.460 (5)
C420.5024 (4)0.5357 (3)0.0843 (3)0.0270 (8)0.540 (5)
H420.5610660.4966040.0628820.032*0.540 (5)
C42A0.4737 (5)0.5730 (5)0.1025 (3)0.0365 (12)0.460 (5)
H42A0.5216140.5185240.0931570.044*0.460 (5)
C430.62888 (15)0.76136 (12)0.03166 (10)0.0323 (4)
C440.6813 (3)0.8349 (2)0.05213 (19)0.0301 (5)0.517 (2)
H440.7058580.8257550.0994940.036*0.517 (2)
C44A0.5936 (3)0.8448 (2)0.0759 (2)0.0301 (5)0.483 (2)
H44A0.5745330.8375520.1296490.036*0.483 (2)
C450.6961 (3)0.9188 (3)0.0033 (2)0.0398 (9)0.517 (2)
H450.7230960.9672730.0207320.048*0.517 (2)
C45A0.5897 (3)0.9347 (3)0.0343 (2)0.0392 (9)0.483 (2)
H45A0.5757810.9893770.0605860.047*0.483 (2)
C460.6707 (3)0.9300 (3)0.0706 (2)0.0376 (6)0.517 (2)
H460.6819050.9845350.1044650.045*0.517 (2)
C46A0.6067 (3)0.9435 (3)0.0469 (2)0.0376 (6)0.483 (2)
H46A0.6031671.0045330.0736930.045*0.483 (2)
C470.62988 (15)0.85997 (15)0.09120 (11)0.0418 (5)
H470.6465860.8647630.1451620.050*0.483 (2)
H47A0.6036190.8692720.1378910.050*0.517 (2)
C480.62478 (15)0.77339 (13)0.04588 (10)0.0348 (4)
H480.6181640.7203430.0697940.042*
C490.85089 (12)0.77680 (11)0.24726 (8)0.0207 (3)
C500.91418 (13)0.86074 (11)0.23638 (9)0.0265 (3)
H50A0.8633920.9175150.2476320.032*0.493 (6)
H500.8666230.9210260.2404430.032*0.507 (6)
C510.98786 (12)0.85182 (12)0.29505 (10)0.0289 (4)
C521.03369 (14)0.93196 (13)0.30295 (14)0.0455 (5)
H521.0169040.9896730.2732750.055*
C531.10317 (18)0.92623 (16)0.3541 (2)0.0689 (8)
H531.1327160.9801150.3584840.083*
C541.12956 (18)0.84128 (16)0.39892 (18)0.0643 (7)
H541.1774740.8374900.4326570.077*
C551.08389 (16)0.76237 (14)0.39294 (13)0.0441 (5)
H551.1008380.7050220.4230230.053*
C561.01275 (13)0.76792 (12)0.34229 (10)0.0310 (4)
H560.9811770.7145590.3399320.037*
C57A0.9471 (5)0.8709 (4)0.1487 (4)0.0214 (12)0.493 (6)
C580.9364 (4)0.8885 (3)0.0929 (3)0.0252 (9)0.507 (6)
H580.8645860.9043200.1017130.030*0.507 (6)
C58A0.8777 (5)0.8931 (3)0.0952 (2)0.0325 (11)0.493 (6)
H58A0.8069600.9043700.1136440.039*0.493 (6)
C590.9884 (4)0.8883 (4)0.0163 (3)0.0275 (13)0.507 (6)
H590.9522100.9025790.0256710.033*0.507 (6)
C59A0.9106 (6)0.8988 (3)0.0158 (2)0.0488 (16)0.493 (6)
H59A0.8630600.9134800.0187370.059*0.493 (6)
C601.0975 (5)0.8658 (4)0.0048 (3)0.0285 (12)0.507 (6)
H601.1344670.8653680.0454000.034*0.507 (6)
C60A1.0192 (8)0.8818 (4)0.0118 (4)0.053 (2)0.493 (6)
H60A1.0434810.8860060.0650370.064*0.493 (6)
C611.1494 (3)0.8445 (3)0.0678 (2)0.0336 (11)0.507 (6)
H611.2213380.8300620.0597400.040*0.507 (6)
C61A1.0857 (6)0.8598 (4)0.0390 (4)0.047 (2)0.493 (6)
H61A1.1564690.8483240.0205760.056*0.493 (6)
C621.0958 (4)0.8442 (3)0.1427 (3)0.0267 (9)0.507 (6)
H621.1316960.8292210.1848120.032*0.507 (6)
C62A1.0517 (5)0.8536 (3)0.1199 (3)0.0321 (11)0.493 (6)
H62A1.0998070.8377280.1540440.038*0.493 (6)
C630.73115 (11)0.71922 (10)0.45772 (8)0.0169 (3)
C640.74739 (11)0.77306 (10)0.52482 (8)0.0186 (3)
H640.8188370.7515050.5341940.022*
C650.73824 (12)0.88095 (11)0.50243 (8)0.0217 (3)
C660.64628 (13)0.94269 (12)0.51620 (11)0.0337 (4)
H660.5862910.9180120.5403190.040*
C670.64156 (15)1.04079 (13)0.49477 (12)0.0376 (4)
H670.5791331.0810710.5053850.045*
C680.72881 (17)1.07819 (13)0.45802 (12)0.0420 (5)
H680.7256321.1434980.4421530.050*
C690.8211 (2)1.01800 (16)0.44490 (16)0.0665 (8)
H690.8807271.0430630.4205590.080*
C700.82635 (16)0.92010 (14)0.46756 (13)0.0471 (5)
H700.8897060.8805980.4591940.057*
C710.67644 (11)0.74405 (10)0.59961 (8)0.0187 (3)
C720.71774 (12)0.71662 (11)0.66819 (9)0.0223 (3)
H720.7886750.7141070.6674120.027*
C730.65462 (14)0.69292 (12)0.73784 (9)0.0290 (4)
H730.6834110.6755990.7832550.035*
C740.54887 (14)0.69499 (12)0.73991 (10)0.0310 (4)
H740.5064200.6797750.7865500.037*
C750.50733 (13)0.71997 (12)0.67172 (10)0.0281 (3)
H750.4367550.7202530.6723980.034*
C760.57012 (12)0.74460 (11)0.60234 (9)0.0231 (3)
H760.5409930.7617010.5570600.028*
C570.9883 (5)0.8662 (4)0.1552 (4)0.0200 (12)0.507 (6)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.01573 (13)0.01719 (13)0.01225 (12)0.00063 (9)0.00144 (9)0.00258 (9)
Ni20.01713 (13)0.02215 (14)0.01389 (13)0.00304 (10)0.00201 (9)0.00521 (10)
O10.0222 (5)0.0189 (5)0.0175 (5)0.0023 (4)0.0034 (4)0.0022 (4)
O20.0244 (5)0.0299 (6)0.0227 (6)0.0069 (4)0.0078 (4)0.0090 (4)
O30.0177 (5)0.0245 (5)0.0155 (5)0.0017 (4)0.0033 (4)0.0041 (4)
O40.0216 (5)0.0334 (6)0.0146 (5)0.0062 (4)0.0042 (4)0.0074 (4)
O50.0221 (5)0.0202 (5)0.0192 (5)0.0005 (4)0.0004 (4)0.0063 (4)
O60.0244 (6)0.0230 (5)0.0245 (6)0.0018 (4)0.0016 (4)0.0036 (4)
O70.0185 (5)0.0234 (5)0.0153 (5)0.0003 (4)0.0027 (4)0.0056 (4)
O80.0260 (5)0.0243 (5)0.0175 (5)0.0042 (4)0.0055 (4)0.0051 (4)
O90.0188 (5)0.0202 (5)0.0132 (5)0.0005 (4)0.0013 (4)0.0040 (4)
N10.0173 (6)0.0204 (6)0.0144 (6)0.0019 (5)0.0024 (5)0.0033 (5)
N20.0208 (6)0.0225 (6)0.0166 (6)0.0026 (5)0.0032 (5)0.0040 (5)
N30.0168 (6)0.0318 (7)0.0197 (6)0.0012 (5)0.0034 (5)0.0076 (5)
N40.0280 (7)0.0299 (7)0.0155 (6)0.0096 (5)0.0013 (5)0.0041 (5)
C10.0248 (7)0.0211 (7)0.0164 (7)0.0017 (6)0.0020 (6)0.0021 (5)
C20.0273 (8)0.0283 (8)0.0183 (7)0.0070 (6)0.0002 (6)0.0006 (6)
C30.0187 (7)0.0351 (9)0.0195 (8)0.0049 (6)0.0031 (6)0.0078 (6)
C40.0185 (7)0.0246 (8)0.0289 (8)0.0001 (6)0.0020 (6)0.0079 (6)
C50.0190 (7)0.0200 (7)0.0209 (7)0.0023 (6)0.0007 (6)0.0025 (6)
C60.0266 (8)0.0233 (7)0.0178 (7)0.0022 (6)0.0017 (6)0.0023 (6)
C70.0404 (9)0.0252 (8)0.0190 (8)0.0071 (7)0.0073 (7)0.0010 (6)
C80.0343 (9)0.0336 (9)0.0283 (9)0.0098 (7)0.0175 (7)0.0076 (7)
C90.0240 (8)0.0359 (9)0.0314 (9)0.0015 (7)0.0094 (7)0.0073 (7)
C100.0221 (7)0.0283 (8)0.0216 (8)0.0006 (6)0.0041 (6)0.0037 (6)
C110.0251 (8)0.0566 (11)0.0237 (8)0.0136 (8)0.0012 (7)0.0163 (8)
C120.0284 (9)0.0741 (14)0.0252 (9)0.0189 (9)0.0016 (7)0.0102 (9)
C130.0229 (8)0.0519 (11)0.0422 (11)0.0140 (8)0.0042 (8)0.0036 (9)
C140.0234 (8)0.0344 (9)0.0521 (12)0.0053 (7)0.0045 (8)0.0122 (8)
C150.0217 (8)0.0330 (9)0.0318 (9)0.0008 (6)0.0021 (6)0.0131 (7)
C160.0348 (9)0.0230 (8)0.0273 (9)0.0041 (7)0.0091 (7)0.0004 (6)
C170.0524 (12)0.0270 (9)0.0398 (11)0.0091 (8)0.0109 (9)0.0045 (8)
C180.0714 (15)0.0427 (12)0.0328 (11)0.0346 (11)0.0045 (10)0.0012 (9)
C190.0539 (13)0.0746 (16)0.0350 (11)0.0389 (12)0.0232 (10)0.0181 (10)
C200.0398 (10)0.0512 (12)0.0291 (9)0.0206 (9)0.0154 (8)0.0176 (8)
C210.0165 (7)0.0234 (7)0.0167 (7)0.0023 (6)0.0016 (5)0.0032 (6)
C220.0205 (7)0.0216 (7)0.0187 (7)0.0062 (6)0.0041 (6)0.0001 (6)
C230.0178 (7)0.0279 (8)0.0208 (8)0.0072 (6)0.0077 (6)0.0069 (6)
C240.0365 (9)0.0314 (9)0.0289 (9)0.0130 (7)0.0083 (7)0.0081 (7)
C250.0534 (12)0.0477 (11)0.0348 (10)0.0288 (10)0.0141 (9)0.0205 (9)
C260.0399 (10)0.0666 (13)0.0272 (9)0.0264 (10)0.0087 (8)0.0231 (9)
C270.0301 (9)0.0550 (11)0.0188 (8)0.0113 (8)0.0035 (7)0.0079 (7)
C280.0250 (8)0.0333 (9)0.0214 (8)0.0086 (7)0.0039 (6)0.0060 (6)
C290.0219 (7)0.0145 (7)0.0287 (8)0.0052 (6)0.0011 (6)0.0006 (6)
C300.0278 (8)0.0210 (7)0.0291 (8)0.0099 (6)0.0016 (6)0.0034 (6)
C310.0319 (9)0.0257 (8)0.0425 (10)0.0084 (7)0.0133 (8)0.0053 (7)
C320.0215 (8)0.0256 (8)0.0508 (11)0.0039 (6)0.0052 (7)0.0074 (7)
C330.0255 (8)0.0297 (9)0.0366 (10)0.0007 (7)0.0050 (7)0.0033 (7)
C340.0253 (8)0.0303 (8)0.0268 (8)0.0002 (7)0.0017 (6)0.0013 (7)
C350.0196 (7)0.0188 (7)0.0141 (7)0.0016 (5)0.0027 (5)0.0020 (5)
C360.0187 (7)0.0247 (7)0.0141 (7)0.0011 (6)0.0032 (5)0.0055 (6)
C370.0245 (9)0.016 (3)0.0140 (8)0.012 (3)0.0079 (6)0.005 (3)
C37A0.0245 (9)0.016 (3)0.0140 (8)0.012 (3)0.0079 (6)0.005 (3)
C380.0255 (17)0.033 (2)0.0292 (18)0.0031 (15)0.0049 (13)0.0114 (16)
C38A0.0189 (18)0.044 (3)0.026 (2)0.0020 (18)0.0044 (14)0.0091 (19)
C390.030 (3)0.059 (3)0.029 (3)0.010 (2)0.006 (2)0.009 (2)
C39A0.019 (2)0.097 (4)0.026 (2)0.010 (2)0.0017 (15)0.002 (2)
C400.034 (2)0.058 (3)0.027 (2)0.024 (2)0.0055 (19)0.0066 (17)
C40A0.035 (4)0.114 (6)0.025 (3)0.039 (3)0.011 (2)0.014 (3)
C410.051 (2)0.036 (2)0.039 (2)0.0198 (18)0.0113 (17)0.0018 (16)
C41A0.049 (4)0.085 (5)0.043 (3)0.047 (4)0.015 (3)0.027 (3)
C420.033 (2)0.022 (2)0.028 (2)0.0053 (16)0.0092 (15)0.0006 (15)
C42A0.043 (3)0.033 (3)0.037 (3)0.012 (3)0.016 (2)0.007 (2)
C430.0473 (10)0.0255 (8)0.0275 (9)0.0023 (7)0.0195 (8)0.0001 (7)
C440.0386 (12)0.0282 (12)0.0260 (12)0.0098 (11)0.0116 (10)0.0033 (9)
C44A0.0386 (12)0.0282 (12)0.0260 (12)0.0098 (11)0.0116 (10)0.0033 (9)
C450.052 (2)0.0315 (18)0.038 (2)0.0154 (16)0.0127 (17)0.0079 (15)
C45A0.047 (2)0.0240 (18)0.050 (2)0.0102 (16)0.0157 (19)0.0026 (16)
C460.0359 (16)0.0355 (14)0.0366 (16)0.0059 (14)0.0051 (13)0.0149 (12)
C46A0.0359 (16)0.0355 (14)0.0366 (16)0.0059 (14)0.0051 (13)0.0149 (12)
C470.0412 (10)0.0473 (11)0.0311 (10)0.0032 (9)0.0050 (8)0.0129 (8)
C480.0439 (10)0.0362 (9)0.0213 (8)0.0044 (8)0.0008 (7)0.0010 (7)
C490.0266 (8)0.0216 (7)0.0124 (7)0.0001 (6)0.0015 (6)0.0030 (5)
C500.0348 (9)0.0184 (7)0.0222 (8)0.0023 (6)0.0067 (7)0.0040 (6)
C510.0213 (8)0.0241 (8)0.0396 (10)0.0062 (6)0.0055 (7)0.0070 (7)
C520.0275 (9)0.0251 (9)0.0838 (16)0.0099 (7)0.0053 (9)0.0018 (9)
C530.0428 (12)0.0311 (11)0.145 (3)0.0148 (9)0.0387 (15)0.0076 (13)
C540.0492 (13)0.0400 (12)0.118 (2)0.0116 (10)0.0452 (14)0.0104 (13)
C550.0428 (11)0.0332 (10)0.0619 (13)0.0087 (8)0.0200 (10)0.0054 (9)
C560.0306 (9)0.0268 (8)0.0374 (10)0.0106 (7)0.0025 (7)0.0062 (7)
C57A0.019 (3)0.0159 (17)0.026 (3)0.006 (2)0.009 (3)0.0029 (15)
C580.021 (2)0.0274 (18)0.026 (3)0.0064 (16)0.0028 (19)0.0003 (14)
C58A0.043 (3)0.0280 (19)0.028 (2)0.0087 (19)0.007 (2)0.0021 (14)
C590.029 (4)0.027 (2)0.024 (3)0.0072 (18)0.003 (2)0.000 (2)
C59A0.089 (5)0.032 (2)0.031 (2)0.019 (2)0.017 (2)0.0012 (16)
C600.032 (3)0.0290 (19)0.021 (3)0.0107 (17)0.013 (2)0.005 (2)
C60A0.094 (7)0.030 (2)0.030 (4)0.025 (3)0.024 (4)0.008 (2)
C610.026 (2)0.042 (2)0.032 (2)0.0077 (15)0.0047 (17)0.0078 (15)
C61A0.059 (5)0.038 (3)0.036 (4)0.022 (2)0.035 (4)0.014 (3)
C620.017 (2)0.036 (2)0.025 (2)0.0029 (16)0.0049 (16)0.0056 (14)
C62A0.023 (3)0.0269 (19)0.043 (3)0.0038 (17)0.005 (3)0.0043 (17)
C630.0176 (7)0.0209 (7)0.0115 (6)0.0058 (5)0.0021 (5)0.0009 (5)
C640.0168 (7)0.0253 (7)0.0144 (7)0.0061 (6)0.0004 (5)0.0037 (5)
C650.0271 (8)0.0257 (8)0.0141 (7)0.0107 (6)0.0005 (6)0.0036 (6)
C660.0263 (8)0.0284 (9)0.0461 (11)0.0093 (7)0.0049 (7)0.0026 (7)
C670.0372 (10)0.0284 (9)0.0479 (11)0.0052 (7)0.0110 (8)0.0008 (8)
C680.0603 (13)0.0251 (9)0.0394 (11)0.0160 (9)0.0023 (9)0.0003 (8)
C690.0613 (15)0.0348 (11)0.0884 (19)0.0221 (11)0.0407 (13)0.0024 (11)
C700.0402 (11)0.0307 (10)0.0612 (14)0.0127 (8)0.0254 (10)0.0058 (9)
C710.0227 (7)0.0190 (7)0.0152 (7)0.0071 (6)0.0013 (6)0.0059 (5)
C720.0254 (8)0.0251 (8)0.0180 (7)0.0085 (6)0.0012 (6)0.0048 (6)
C730.0399 (9)0.0322 (9)0.0157 (7)0.0110 (7)0.0009 (7)0.0021 (6)
C740.0364 (9)0.0333 (9)0.0211 (8)0.0130 (7)0.0110 (7)0.0061 (7)
C750.0232 (8)0.0330 (9)0.0279 (9)0.0099 (7)0.0070 (6)0.0097 (7)
C760.0227 (7)0.0274 (8)0.0202 (8)0.0056 (6)0.0001 (6)0.0082 (6)
C570.012 (3)0.0188 (17)0.028 (2)0.007 (2)0.008 (3)0.0050 (14)
Geometric parameters (Å, º) top
Ni1—O12.0524 (10)C38—H380.9300
Ni1—O32.0570 (10)C38—C391.409 (7)
Ni1—O52.0174 (10)C38A—H38A0.9300
Ni1—O92.1077 (10)C38A—C39A1.382 (6)
Ni1—N12.0913 (12)C39—H390.9300
Ni1—N22.1211 (12)C39—C401.386 (9)
Ni2—O42.0163 (10)C39A—H39A0.9300
Ni2—O62.0518 (11)C39A—C40A1.379 (12)
Ni2—O72.0759 (10)C40—H400.9300
Ni2—O92.1040 (10)C40—C411.357 (7)
Ni2—N32.1109 (13)C40A—H40A0.9300
Ni2—N42.0849 (13)C40A—C41A1.350 (13)
O1—C211.2595 (17)C41—H410.9300
O2—C211.2553 (18)C41—C421.385 (6)
O3—C351.2512 (17)C41A—H41A0.9300
O4—C351.2548 (17)C41A—C42A1.388 (9)
O5—C491.2561 (18)C42—H420.9300
O6—C491.2488 (18)C42A—H42A0.9300
O7—C631.2569 (17)C43—C441.454 (4)
O8—C631.2579 (17)C43—C44A1.467 (4)
O9—H9A0.85 (2)C43—C481.358 (2)
O9—H9B0.87 (3)C44—H440.9300
N1—C11.3405 (19)C44—C451.395 (4)
N1—C51.3401 (19)C44A—H44A0.9300
N2—C61.3412 (19)C44A—C45A1.386 (5)
N2—C101.341 (2)C45—H450.9300
N3—C111.338 (2)C45—C461.378 (5)
N3—C151.340 (2)C45A—H45A0.9300
N4—C161.346 (2)C45A—C46A1.394 (6)
N4—C201.338 (2)C46—H460.9300
C1—H10.9300C46—C471.319 (4)
C1—C21.386 (2)C46A—H46A0.9300
C2—H20.9300C46A—C471.463 (5)
C2—C31.379 (2)C47—H470.9300
C3—H30.9300C47—H47A0.9300
C3—C41.384 (2)C47—C481.381 (3)
C4—H40.9300C48—H480.9300
C4—C51.386 (2)C49—C501.537 (2)
C5—H50.9300C50—H50A0.9800
C6—H60.9300C50—H500.9800
C6—C71.384 (2)C50—C511.516 (2)
C7—H70.9300C50—C57A1.518 (7)
C7—C81.377 (3)C50—C571.583 (6)
C8—H80.9300C51—C521.404 (2)
C8—C91.380 (3)C51—C561.390 (2)
C9—H90.9300C52—H520.9300
C9—C101.386 (2)C52—C531.377 (3)
C10—H100.9300C53—H530.9300
C11—H110.9300C53—C541.384 (3)
C11—C121.379 (3)C54—H540.9300
C12—H120.9300C54—C551.378 (3)
C12—C131.382 (3)C55—H550.9300
C13—H130.9300C55—C561.388 (3)
C13—C141.379 (3)C56—H560.9300
C14—H140.9300C57A—C58A1.397 (7)
C14—C151.383 (2)C57A—C62A1.381 (6)
C15—H150.9300C58—H580.9300
C16—H160.9300C58—C591.399 (7)
C16—C171.384 (2)C58—C571.366 (7)
C17—H170.9300C58A—H58A0.9300
C17—C181.375 (3)C58A—C59A1.380 (6)
C18—H180.9300C59—H590.9300
C18—C191.373 (4)C59—C601.411 (8)
C19—H190.9300C59A—H59A0.9300
C19—C201.395 (3)C59A—C60A1.424 (9)
C20—H200.9300C60—H600.9300
C21—C221.541 (2)C60—C611.375 (7)
C22—H220.9800C60A—H60A0.9300
C22—C231.519 (2)C60A—C61A1.335 (12)
C22—C291.524 (2)C61—H610.9300
C23—C241.398 (2)C61—C621.380 (5)
C23—C281.391 (2)C61A—H61A0.9300
C24—H240.9300C61A—C62A1.407 (8)
C24—C251.381 (3)C62—H620.9300
C25—H250.9300C62—C571.389 (6)
C25—C261.382 (3)C62A—H62A0.9300
C26—H260.9300C63—C641.5441 (19)
C26—C271.384 (3)C64—H640.9800
C27—H270.9300C64—C651.523 (2)
C27—C281.396 (2)C64—C711.5259 (19)
C28—H280.9300C65—C661.384 (2)
C29—C301.393 (2)C65—C701.383 (2)
C29—C341.388 (2)C66—H660.9300
C30—H300.9300C66—C671.390 (2)
C30—C311.386 (2)C67—H670.9300
C31—H310.9300C67—C681.370 (3)
C31—C321.385 (3)C68—H680.9300
C32—H320.9300C68—C691.374 (3)
C32—C331.380 (3)C69—H690.9300
C33—H330.9300C69—C701.390 (3)
C33—C341.389 (2)C70—H700.9300
C34—H340.9300C71—C721.392 (2)
C35—C361.5457 (18)C71—C761.396 (2)
C36—H360.9800C72—H720.9300
C36—H36A0.9800C72—C731.390 (2)
C36—C371.593 (7)C73—H730.9300
C36—C37A1.447 (11)C73—C741.387 (2)
C36—C431.516 (2)C74—H740.9300
C37—C381.377 (9)C74—C751.384 (2)
C37—C421.365 (5)C75—H750.9300
C37A—C38A1.415 (9)C75—C761.387 (2)
C37A—C42A1.382 (6)C76—H760.9300
O1—Ni1—O389.05 (4)C42A—C37A—C36119.7 (6)
O1—Ni1—O991.80 (4)C42A—C37A—C38A116.1 (8)
O1—Ni1—N188.57 (4)C37—C38—H38120.0
O1—Ni1—N289.66 (5)C37—C38—C39120.0 (4)
O3—Ni1—O992.91 (4)C39—C38—H38120.0
O3—Ni1—N188.54 (4)C37A—C38A—H38A119.6
O3—Ni1—N2176.62 (4)C39A—C38A—C37A120.9 (6)
O5—Ni1—O1175.04 (4)C39A—C38A—H38A119.6
O5—Ni1—O394.32 (4)C38—C39—H39120.6
O5—Ni1—O991.66 (4)C40—C39—C38118.9 (5)
O5—Ni1—N187.87 (4)C40—C39—H39120.6
O5—Ni1—N286.77 (5)C38A—C39A—H39A119.9
O9—Ni1—N290.26 (4)C40A—C39A—C38A120.2 (6)
N1—Ni1—O9178.51 (4)C40A—C39A—H39A119.9
N1—Ni1—N288.30 (5)C39—C40—H40119.8
O4—Ni2—O695.12 (5)C41—C40—C39120.4 (5)
O4—Ni2—O7175.70 (4)C41—C40—H40119.8
O4—Ni2—O991.62 (4)C39A—C40A—H40A119.7
O4—Ni2—N389.72 (5)C41A—C40A—C39A120.5 (7)
O4—Ni2—N489.26 (5)C41A—C40A—H40A119.7
O6—Ni2—O784.55 (4)C40—C41—H41119.9
O6—Ni2—O991.13 (4)C40—C41—C42120.3 (4)
O6—Ni2—N3174.71 (5)C42—C41—H41119.9
O6—Ni2—N486.13 (5)C40A—C41A—H41A120.3
O7—Ni2—O992.67 (4)C40A—C41A—C42A119.4 (7)
O7—Ni2—N390.47 (4)C42A—C41A—H41A120.3
O7—Ni2—N486.44 (5)C37—C42—C41120.8 (5)
O9—Ni2—N390.86 (5)C37—C42—H42119.6
N4—Ni2—O9177.19 (5)C41—C42—H42119.6
N4—Ni2—N391.81 (5)C37A—C42A—C41A122.9 (8)
C21—O1—Ni1129.29 (9)C37A—C42A—H42A118.5
C35—O3—Ni1134.83 (9)C41A—C42A—H42A118.5
C35—O4—Ni2133.74 (9)C44—C43—C36124.90 (17)
C49—O5—Ni1133.34 (10)C44A—C43—C36115.38 (19)
C49—O6—Ni2136.62 (10)C48—C43—C36120.72 (15)
C63—O7—Ni2125.14 (9)C48—C43—C44110.06 (19)
Ni1—O9—H9A99.6 (14)C48—C43—C44A117.98 (19)
Ni1—O9—H9B113.6 (15)C43—C44—H44118.8
Ni2—O9—Ni1116.32 (5)C45—C44—C43122.4 (3)
Ni2—O9—H9A121.7 (14)C45—C44—H44118.8
Ni2—O9—H9B95.8 (15)C43—C44A—H44A121.3
H9A—O9—H9B110 (2)C45A—C44A—C43117.4 (3)
C1—N1—Ni1121.13 (10)C45A—C44A—H44A121.3
C5—N1—Ni1120.90 (10)C44—C45—H45119.9
C5—N1—C1117.97 (13)C46—C45—C44120.2 (3)
C6—N2—Ni1123.53 (10)C46—C45—H45119.9
C10—N2—Ni1118.69 (10)C44A—C45A—H45A119.9
C10—N2—C6117.69 (13)C44A—C45A—C46A120.2 (4)
C11—N3—Ni2119.23 (11)C46A—C45A—H45A119.9
C11—N3—C15117.13 (14)C45—C46—H46121.4
C15—N3—Ni2123.43 (11)C47—C46—C45117.2 (3)
C16—N4—Ni2119.84 (11)C47—C46—H46121.4
C20—N4—Ni2122.14 (13)C45A—C46A—H46A118.9
C20—N4—C16117.97 (15)C45A—C46A—C47122.2 (3)
N1—C1—H1118.7C47—C46A—H46A118.9
N1—C1—C2122.56 (14)C46—C47—H47A118.9
C2—C1—H1118.7C46—C47—C48122.3 (2)
C1—C2—H2120.4C46A—C47—H47122.9
C3—C2—C1119.23 (14)C48—C47—C46A114.1 (2)
C3—C2—H2120.4C48—C47—H47122.9
C2—C3—H3120.7C48—C47—H47A118.9
C2—C3—C4118.51 (14)C43—C48—C47123.68 (18)
C4—C3—H3120.7C43—C48—H48118.2
C3—C4—H4120.5C47—C48—H48118.2
C3—C4—C5119.05 (14)O5—C49—C50115.65 (13)
C5—C4—H4120.5O6—C49—O5127.33 (14)
N1—C5—C4122.63 (14)O6—C49—C50117.02 (13)
N1—C5—H5118.7C49—C50—H50A105.5
C4—C5—H5118.7C49—C50—H50109.3
N2—C6—H6118.8C49—C50—C57112.3 (2)
N2—C6—C7122.41 (15)C51—C50—C49113.04 (13)
C7—C6—H6118.8C51—C50—H50A105.5
C6—C7—H7120.3C51—C50—H50109.3
C8—C7—C6119.45 (15)C51—C50—C57A124.4 (3)
C8—C7—H7120.3C51—C50—C57103.5 (3)
C7—C8—H8120.6C57A—C50—C49101.3 (2)
C7—C8—C9118.74 (15)C57A—C50—H50A105.5
C9—C8—H8120.6C57—C50—H50109.3
C8—C9—H9120.7C52—C51—C50118.99 (16)
C8—C9—C10118.60 (16)C56—C51—C50123.43 (14)
C10—C9—H9120.7C56—C51—C52117.58 (17)
N2—C10—C9123.09 (15)C51—C52—H52119.6
N2—C10—H10118.5C53—C52—C51120.86 (19)
C9—C10—H10118.5C53—C52—H52119.6
N3—C11—H11118.2C52—C53—H53119.6
N3—C11—C12123.68 (17)C52—C53—C54120.79 (18)
C12—C11—H11118.2C54—C53—H53119.6
C11—C12—H12120.8C53—C54—H54120.4
C11—C12—C13118.48 (17)C55—C54—C53119.1 (2)
C13—C12—H12120.8C55—C54—H54120.4
C12—C13—H13120.6C54—C55—H55119.8
C14—C13—C12118.72 (17)C54—C55—C56120.4 (2)
C14—C13—H13120.6C56—C55—H55119.8
C13—C14—H14120.5C51—C56—H56119.4
C13—C14—C15119.02 (17)C55—C56—C51121.16 (16)
C15—C14—H14120.5C55—C56—H56119.4
N3—C15—C14122.91 (16)C58A—C57A—C50124.0 (4)
N3—C15—H15118.5C62A—C57A—C50118.1 (5)
C14—C15—H15118.5C62A—C57A—C58A117.8 (5)
N4—C16—H16118.6C59—C58—H58119.1
N4—C16—C17122.71 (19)C57—C58—H58119.1
C17—C16—H16118.6C57—C58—C59121.8 (4)
C16—C17—H17120.6C57A—C58A—H58A118.9
C18—C17—C16118.9 (2)C59A—C58A—C57A122.3 (6)
C18—C17—H17120.6C59A—C58A—H58A118.9
C17—C18—H18120.4C58—C59—H59121.1
C19—C18—C17119.14 (18)C58—C59—C60117.8 (5)
C19—C18—H18120.4C60—C59—H59121.1
C18—C19—H19120.4C58A—C59A—H59A120.8
C18—C19—C20119.1 (2)C58A—C59A—C60A118.5 (5)
C20—C19—H19120.4C60A—C59A—H59A120.8
N4—C20—C19122.2 (2)C59—C60—H60120.0
N4—C20—H20118.9C61—C60—C59120.1 (5)
C19—C20—H20118.9C61—C60—H60120.0
O1—C21—C22116.15 (12)C59A—C60A—H60A120.2
O2—C21—O1126.15 (14)C61A—C60A—C59A119.6 (6)
O2—C21—C22117.69 (13)C61A—C60A—H60A120.2
C21—C22—H22106.9C60—C61—H61119.6
C23—C22—C21113.29 (12)C60—C61—C62120.8 (4)
C23—C22—H22106.9C62—C61—H61119.6
C23—C22—C29113.40 (12)C60A—C61A—H61A119.1
C29—C22—C21109.11 (11)C60A—C61A—C62A121.8 (7)
C29—C22—H22106.9C62A—C61A—H61A119.1
C24—C23—C22118.21 (14)C61—C62—H62120.0
C28—C23—C22123.48 (14)C61—C62—C57120.0 (5)
C28—C23—C24118.31 (15)C57—C62—H62120.0
C23—C24—H24119.4C57A—C62A—C61A120.2 (6)
C25—C24—C23121.17 (18)C57A—C62A—H62A119.9
C25—C24—H24119.4C61A—C62A—H62A119.9
C24—C25—H25119.9O7—C63—O8125.65 (13)
C24—C25—C26120.12 (17)O7—C63—C64117.57 (12)
C26—C25—H25119.9O8—C63—C64116.77 (12)
C25—C26—H26120.2C63—C64—H64106.8
C25—C26—C27119.70 (17)C65—C64—C63111.78 (11)
C27—C26—H26120.2C65—C64—H64106.8
C26—C27—H27119.9C65—C64—C71113.92 (12)
C26—C27—C28120.25 (18)C71—C64—C63110.41 (11)
C28—C27—H27119.9C71—C64—H64106.8
C23—C28—C27120.45 (16)C66—C65—C64123.43 (13)
C23—C28—H28119.8C70—C65—C64118.73 (15)
C27—C28—H28119.8C70—C65—C66117.83 (16)
C30—C29—C22119.00 (14)C65—C66—H66119.3
C34—C29—C22122.36 (14)C65—C66—C67121.46 (16)
C34—C29—C30118.59 (15)C67—C66—H66119.3
C29—C30—H30119.7C66—C67—H67120.0
C31—C30—C29120.61 (16)C68—C67—C66120.06 (18)
C31—C30—H30119.7C68—C67—H67120.0
C30—C31—H31119.9C67—C68—H68120.4
C32—C31—C30120.20 (16)C67—C68—C69119.17 (17)
C32—C31—H31119.9C69—C68—H68120.4
C31—C32—H32120.2C68—C69—H69119.6
C33—C32—C31119.65 (16)C68—C69—C70120.85 (19)
C33—C32—H32120.2C70—C69—H69119.6
C32—C33—H33119.9C65—C70—C69120.59 (19)
C32—C33—C34120.22 (16)C65—C70—H70119.7
C34—C33—H33119.9C69—C70—H70119.7
C29—C34—C33120.73 (16)C72—C71—C64119.61 (13)
C29—C34—H34119.6C72—C71—C76118.06 (13)
C33—C34—H34119.6C76—C71—C64122.33 (13)
O3—C35—O4128.23 (13)C71—C72—H72119.5
O3—C35—C36116.15 (12)C73—C72—C71121.02 (15)
O4—C35—C36115.62 (12)C73—C72—H72119.5
C35—C36—H36104.8C72—C73—H73119.9
C35—C36—H36A109.7C74—C73—C72120.29 (15)
C35—C36—C37110.0 (3)C74—C73—H73119.9
C37—C36—H36104.8C73—C74—H74120.4
C37A—C36—C35110.8 (4)C75—C74—C73119.18 (15)
C37A—C36—H36A109.7C75—C74—H74120.4
C37A—C36—C43105.1 (3)C74—C75—H75119.7
C43—C36—C35111.71 (12)C74—C75—C76120.54 (15)
C43—C36—H36104.8C76—C75—H75119.7
C43—C36—H36A109.7C71—C76—H76119.6
C43—C36—C37119.3 (3)C75—C76—C71120.88 (15)
C38—C37—C36120.4 (3)C75—C76—H76119.6
C42—C37—C36120.0 (6)C58—C57—C50113.5 (4)
C42—C37—C38119.6 (6)C58—C57—C62119.6 (5)
C38A—C37A—C36124.1 (5)C62—C57—C50126.7 (5)
Ni1—O1—C21—O211.3 (2)C36—C37A—C42A—C41A178.3 (6)
Ni1—O1—C21—C22167.06 (9)C36—C43—C44—C45173.6 (3)
Ni1—O3—C35—O46.9 (2)C36—C43—C44A—C45A173.1 (3)
Ni1—O3—C35—C36173.47 (9)C36—C43—C48—C47178.30 (17)
Ni1—O5—C49—O60.3 (2)C37—C36—C43—C44A79.7 (4)
Ni1—O5—C49—C50178.68 (9)C37—C36—C43—C4872.7 (4)
Ni1—N1—C1—C2179.68 (11)C37—C38—C39—C402.2 (8)
Ni1—N1—C5—C4178.74 (11)C37A—C36—C43—C44123.1 (4)
Ni1—N2—C6—C7175.36 (11)C37A—C36—C43—C4882.6 (4)
Ni1—N2—C10—C9175.80 (12)C37A—C38A—C39A—C40A1.2 (8)
Ni2—O4—C35—O39.4 (2)C38—C37—C42—C410.2 (9)
Ni2—O4—C35—C36170.28 (10)C38—C39—C40—C410.8 (8)
Ni2—O6—C49—O513.1 (2)C38A—C37A—C42A—C41A2.4 (11)
Ni2—O6—C49—C50167.89 (10)C38A—C39A—C40A—C41A2.3 (9)
Ni2—O7—C63—O817.3 (2)C39—C40—C41—C420.9 (7)
Ni2—O7—C63—C64163.81 (9)C39A—C40A—C41A—C42A1.1 (10)
Ni2—N3—C11—C12172.46 (15)C40—C41—C42—C371.2 (7)
Ni2—N3—C15—C14173.33 (13)C40A—C41A—C42A—C37A1.3 (10)
Ni2—N4—C16—C17177.54 (13)C42—C37—C38—C391.9 (9)
Ni2—N4—C20—C19178.02 (15)C42A—C37A—C38A—C39A1.1 (10)
O1—C21—C22—C2378.13 (16)C43—C36—C37—C3850.1 (7)
O1—C21—C22—C2949.23 (17)C43—C36—C37—C42132.1 (5)
O2—C21—C22—C23103.38 (15)C43—C36—C37A—C38A36.6 (8)
O2—C21—C22—C29129.26 (14)C43—C36—C37A—C42A147.8 (7)
O3—C35—C36—C37128.5 (3)C43—C44—C45—C467.0 (6)
O3—C35—C36—C37A146.5 (3)C43—C44A—C45A—C46A7.6 (5)
O3—C35—C36—C4396.69 (16)C44—C43—C48—C4724.0 (3)
O4—C35—C36—C3751.8 (3)C44—C45—C46—C471.9 (6)
O4—C35—C36—C37A33.8 (3)C44A—C43—C48—C4726.6 (3)
O4—C35—C36—C4383.01 (17)C44A—C45A—C46A—C470.6 (6)
O5—C49—C50—C5171.40 (17)C45—C46—C47—C488.5 (5)
O5—C49—C50—C57A64.0 (3)C45A—C46A—C47—C485.1 (5)
O5—C49—C50—C5745.3 (3)C46—C47—C48—C4321.7 (4)
O6—C49—C50—C51109.49 (16)C46A—C47—C48—C4318.7 (3)
O6—C49—C50—C57A115.1 (3)C48—C43—C44—C4517.0 (4)
O6—C49—C50—C57133.8 (3)C48—C43—C44A—C45A19.9 (4)
O7—C63—C64—C6546.07 (17)C49—C50—C51—C52166.44 (15)
O7—C63—C64—C7181.84 (15)C49—C50—C51—C5613.3 (2)
O8—C63—C64—C65134.96 (13)C49—C50—C57A—C58A61.4 (5)
O8—C63—C64—C7197.13 (15)C49—C50—C57A—C62A116.0 (4)
N1—C1—C2—C31.2 (2)C49—C50—C57—C5866.8 (4)
N2—C6—C7—C80.5 (2)C49—C50—C57—C62108.3 (5)
N3—C11—C12—C131.2 (3)C50—C51—C52—C53178.3 (2)
N4—C16—C17—C180.7 (3)C50—C51—C56—C55177.42 (17)
C1—N1—C5—C41.8 (2)C50—C57A—C58A—C59A178.0 (4)
C1—C2—C3—C42.3 (2)C50—C57A—C62A—C61A178.4 (4)
C2—C3—C4—C51.4 (2)C51—C50—C57A—C58A170.2 (3)
C3—C4—C5—N10.7 (2)C51—C50—C57A—C62A12.4 (6)
C5—N1—C1—C20.9 (2)C51—C50—C57—C58171.0 (3)
C6—N2—C10—C90.9 (2)C51—C50—C57—C6214.0 (5)
C6—C7—C8—C90.6 (2)C51—C52—C53—C540.0 (4)
C7—C8—C9—C100.8 (2)C52—C51—C56—C552.8 (3)
C8—C9—C10—N20.1 (3)C52—C53—C54—C551.2 (4)
C10—N2—C6—C71.2 (2)C53—C54—C55—C560.3 (4)
C11—N3—C15—C141.3 (2)C54—C55—C56—C511.7 (3)
C11—C12—C13—C141.2 (3)C56—C51—C52—C532.0 (3)
C12—C13—C14—C152.2 (3)C57A—C50—C51—C5270.2 (3)
C13—C14—C15—N31.0 (3)C57A—C50—C51—C56110.1 (3)
C15—N3—C11—C122.4 (3)C57A—C58A—C59A—C60A0.2 (6)
C16—N4—C20—C190.5 (3)C58—C59—C60—C610.3 (7)
C16—C17—C18—C190.8 (3)C58A—C57A—C62A—C61A0.9 (7)
C17—C18—C19—C200.3 (3)C58A—C59A—C60A—C61A0.8 (8)
C18—C19—C20—N40.4 (3)C59—C58—C57—C50174.3 (4)
C20—N4—C16—C170.0 (2)C59—C58—C57—C621.2 (7)
C21—C22—C23—C24158.79 (13)C59—C60—C61—C620.4 (7)
C21—C22—C23—C2821.5 (2)C59A—C60A—C61A—C62A0.5 (9)
C21—C22—C29—C3079.85 (16)C60—C61—C62—C570.4 (6)
C21—C22—C29—C3497.64 (16)C60A—C61A—C62A—C57A0.4 (8)
C22—C23—C24—C25179.70 (15)C61—C62—C57—C50174.4 (4)
C22—C23—C28—C27179.88 (14)C61—C62—C57—C580.4 (7)
C22—C29—C30—C31177.09 (13)C62A—C57A—C58A—C59A0.6 (7)
C22—C29—C34—C33176.92 (14)C63—C64—C65—C6691.85 (17)
C23—C22—C29—C30152.85 (13)C63—C64—C65—C7089.17 (18)
C23—C22—C29—C3429.7 (2)C63—C64—C71—C72130.31 (14)
C23—C24—C25—C260.7 (3)C63—C64—C71—C7650.22 (18)
C24—C23—C28—C270.2 (2)C64—C65—C66—C67179.97 (16)
C24—C25—C26—C270.4 (3)C64—C65—C70—C69178.8 (2)
C25—C26—C27—C280.0 (3)C64—C71—C72—C73177.80 (14)
C26—C27—C28—C230.1 (3)C64—C71—C76—C75178.47 (14)
C28—C23—C24—C250.6 (2)C65—C64—C71—C72102.95 (16)
C29—C22—C23—C2476.13 (17)C65—C64—C71—C7676.52 (17)
C29—C22—C23—C28103.56 (17)C65—C66—C67—C681.1 (3)
C29—C30—C31—C320.0 (2)C66—C65—C70—C692.1 (3)
C30—C29—C34—C330.6 (2)C66—C67—C68—C691.9 (3)
C30—C31—C32—C330.3 (2)C67—C68—C69—C700.8 (4)
C31—C32—C33—C340.2 (3)C68—C69—C70—C651.3 (4)
C32—C33—C34—C290.2 (3)C70—C65—C66—C671.0 (3)
C34—C29—C30—C310.5 (2)C71—C64—C65—C6634.2 (2)
C35—C36—C37—C3880.8 (6)C71—C64—C65—C70144.81 (16)
C35—C36—C37—C4297.0 (6)C71—C72—C73—C740.9 (2)
C35—C36—C37A—C38A84.2 (7)C72—C71—C76—C751.0 (2)
C35—C36—C37A—C42A91.4 (8)C72—C73—C74—C750.6 (2)
C35—C36—C43—C442.8 (3)C73—C74—C75—C761.3 (2)
C35—C36—C43—C44A50.5 (2)C74—C75—C76—C710.5 (2)
C35—C36—C43—C48157.13 (16)C76—C71—C72—C731.7 (2)
C36—C37—C38—C39175.9 (5)C57—C50—C51—C5271.8 (3)
C36—C37—C42—C41177.6 (4)C57—C50—C51—C56108.5 (3)
C36—C37A—C38A—C39A176.9 (5)C57—C58—C59—C601.1 (7)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O9—H9A···O20.85 (2)1.79 (2)2.6201 (15)165 (2)
O9—H9B···O80.87 (3)1.70 (3)2.5617 (14)169 (2)
O9—H9B···O70.87 (3)2.60 (2)3.0236 (14)111.2 (18)
C1—H1···O50.932.522.9814 (18)111
C5—H5···O10.932.512.9899 (18)112
C11—H11···O70.932.452.9850 (19)117
C8—H8···O8i0.932.393.211 (2)148
C12—H12···O2ii0.932.463.302 (2)151
C15—H15···O40.932.603.089 (2)113
Symmetry codes: (i) x+2, y+1, z+1; (ii) x+1, y+1, z+1.
µ-Aqua-κ2O:O-di-µ-diphenylacetato-κ4O:O'-\ bis[(2,2'-bipyridine-κ2N,N')(diphenylacetato-κO)\ nickel(II)]–acetonitrile–diphenylacetic acid (1/2.5/1) (2) top
Crystal data top
[Ni2(C14H11O2)4(C10H8N2)2(H2O)]·2.5C2H3N·C14H12O2Z = 2
Mr = 1607.58F(000) = 1682
Triclinic, P1Dx = 1.301 Mg m3
a = 15.6064 (3) ÅCu Kα radiation, λ = 1.54184 Å
b = 17.7440 (4) ÅCell parameters from 31385 reflections
c = 17.9143 (4) Åθ = 2.6–71.7°
α = 70.462 (2)°µ = 1.10 mm1
β = 69.631 (2)°T = 100 K
γ = 64.726 (2)°Prism, light green
V = 4103.17 (18) Å30.22 × 0.14 × 0.08 mm
Data collection top
Rigaku SuperNova, Single source at offset/far, HyPix3000
diffractometer
15557 independent reflections
Radiation source: micro-focus sealed X-ray tube, SuperNova (Cu) X-ray Source13874 reflections with I > 2σ(I)
Mirror monochromatorRint = 0.045
ω scansθmax = 70.0°, θmin = 2.7°
Absorption correction: multi-scan
(CrysAlis PRO; Rigaku OD, 2017)
h = 1918
Tmin = 0.809, Tmax = 1.000k = 2121
52698 measured reflectionsl = 2121
Refinement top
Refinement on F2Primary atom site location: dual
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.038Hydrogen site location: mixed
wR(F2) = 0.103H atoms treated by a mixture of independent and constrained refinement
S = 1.06 w = 1/[σ2(Fo2) + (0.0489P)2 + 1.9174P]
where P = (Fo2 + 2Fc2)/3
15557 reflections(Δ/σ)max < 0.001
1079 parametersΔρmax = 0.48 e Å3
1 restraintΔρmin = 0.57 e Å3
Special details top

Geometry. 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ni10.48008 (2)0.65582 (2)0.79941 (2)0.01430 (7)
Ni20.53556 (2)0.83920 (2)0.69046 (2)0.01383 (7)
O10.49052 (8)0.60373 (7)0.70516 (7)0.0185 (2)
O20.63673 (8)0.61134 (7)0.62971 (7)0.0198 (2)
O30.36089 (8)0.75365 (7)0.76627 (7)0.0175 (2)
O40.41490 (8)0.84939 (7)0.66178 (7)0.0179 (2)
O50.46560 (8)0.71448 (7)0.88737 (6)0.0175 (2)
O60.46012 (8)0.84528 (7)0.80835 (6)0.0183 (2)
O70.65406 (8)0.83659 (7)0.71911 (7)0.0194 (2)
O80.73202 (8)0.70008 (7)0.77037 (7)0.0223 (2)
O90.58547 (8)0.70752 (7)0.72274 (7)0.0152 (2)
H9A0.6353 (19)0.7009 (16)0.7424 (15)0.048 (7)*
H9B0.612 (2)0.6715 (17)0.6843 (17)0.056 (8)*
N10.58608 (10)0.53971 (8)0.84176 (8)0.0165 (3)
N20.39298 (10)0.58745 (8)0.87998 (8)0.0172 (3)
N30.50578 (9)0.96934 (8)0.65646 (8)0.0155 (3)
N40.61480 (9)0.85119 (8)0.56857 (8)0.0160 (3)
C10.68338 (12)0.51896 (10)0.81861 (10)0.0190 (3)
H10.7089890.5593890.7807610.023*
C20.74780 (12)0.43986 (11)0.84850 (10)0.0226 (3)
H20.8149570.4270650.8302640.027*
C30.70891 (13)0.38054 (10)0.90639 (11)0.0239 (4)
H30.7499500.3274870.9284230.029*
C40.60855 (13)0.40093 (10)0.93110 (10)0.0213 (3)
H40.5814490.3619850.9700440.026*
C50.54871 (12)0.48098 (10)0.89654 (9)0.0179 (3)
C60.44044 (12)0.50713 (10)0.91752 (9)0.0175 (3)
C70.39047 (13)0.45370 (11)0.97104 (10)0.0225 (3)
H70.4243020.3987640.9962370.027*
C80.28924 (13)0.48339 (11)0.98648 (11)0.0250 (4)
H80.2543860.4486141.0220420.030*
C90.24107 (13)0.56570 (11)0.94800 (10)0.0247 (4)
H90.1734100.5869460.9571380.030*
C100.29551 (12)0.61580 (11)0.89564 (10)0.0209 (3)
H100.2629970.6712300.8704540.025*
C110.45404 (12)1.02389 (10)0.70602 (10)0.0197 (3)
H110.4223181.0040610.7588710.024*
C120.44597 (12)1.10901 (11)0.68143 (11)0.0227 (3)
H120.4095811.1455970.7172140.027*
C130.49305 (12)1.13866 (10)0.60261 (11)0.0228 (3)
H130.4883821.1955750.5846500.027*
C140.54719 (12)1.08241 (10)0.55088 (10)0.0198 (3)
H140.5792081.1009770.4977040.024*
C150.55274 (11)0.99750 (10)0.58005 (10)0.0165 (3)
C160.61181 (11)0.93211 (10)0.53012 (9)0.0158 (3)
C170.66203 (12)0.95145 (10)0.44910 (10)0.0194 (3)
H170.6563951.0076950.4228630.023*
C180.72045 (12)0.88599 (11)0.40804 (10)0.0219 (3)
H180.7559480.8974840.3544730.026*
C190.72511 (12)0.80302 (11)0.44818 (10)0.0220 (3)
H190.7644800.7578180.4223200.026*
C200.66994 (12)0.78890 (10)0.52753 (10)0.0194 (3)
H200.6712500.7335650.5535280.023*
C210.35006 (11)0.81917 (10)0.70956 (9)0.0157 (3)
C220.24624 (11)0.87016 (10)0.69508 (10)0.0175 (3)
H220.2322610.9297630.6941770.021*
C230.24589 (11)0.86855 (10)0.61060 (10)0.0174 (3)
C240.29523 (12)0.79379 (10)0.58092 (10)0.0206 (3)
H240.3290780.7439030.6130170.025*
C250.29421 (12)0.79327 (11)0.50377 (11)0.0241 (4)
H250.3260120.7428550.4850380.029*
C260.24560 (12)0.86817 (12)0.45449 (10)0.0245 (4)
H260.2454330.8679040.4027200.029*
C270.19759 (12)0.94294 (11)0.48275 (10)0.0233 (3)
H270.1656350.9931170.4497450.028*
C280.19710 (11)0.94312 (10)0.56054 (10)0.0193 (3)
H280.1639300.9934130.5794470.023*
C290.16779 (11)0.84258 (10)0.76417 (10)0.0198 (3)
C300.12384 (15)0.88219 (14)0.82986 (12)0.0346 (4)
H300.1424740.9251500.8306290.042*
C310.05241 (18)0.85864 (17)0.89449 (13)0.0486 (6)
H310.0232420.8862680.9377090.058*
C320.02449 (15)0.79395 (15)0.89470 (12)0.0364 (5)
H320.0232190.7780660.9379050.044*
C330.06808 (13)0.75360 (13)0.83038 (12)0.0305 (4)
H330.0502440.7098870.8302710.037*
C340.13897 (13)0.77814 (11)0.76533 (11)0.0262 (4)
H340.1674650.7508070.7219270.031*
C350.44896 (11)0.79360 (10)0.87518 (9)0.0164 (3)
C360.41004 (12)0.82922 (10)0.95331 (9)0.0185 (3)
H360.3540800.8116230.9864190.022*
C370.48648 (12)0.78748 (10)1.00317 (10)0.0190 (3)
C380.45875 (14)0.76057 (11)1.08758 (10)0.0243 (4)
H380.3936790.7670591.1129330.029*
C390.52729 (15)0.72404 (12)1.13450 (11)0.0308 (4)
H390.5078690.7064611.1908340.037*
C400.62440 (15)0.71393 (11)1.09719 (12)0.0295 (4)
H400.6700040.6904491.1285800.035*
C410.65370 (14)0.73885 (11)1.01294 (12)0.0279 (4)
H410.7191220.7309310.9877480.033*
C420.58490 (13)0.77572 (11)0.96624 (10)0.0232 (3)
H420.6046970.7926970.9098700.028*
C430.37201 (13)0.92683 (10)0.93423 (10)0.0218 (3)
C440.27937 (14)0.97071 (12)0.91935 (11)0.0289 (4)
H440.2414710.9401560.9235690.035*
C450.24237 (16)1.05974 (13)0.89821 (12)0.0372 (5)
H450.1804041.0880700.8882340.045*
C460.29814 (17)1.10600 (12)0.89207 (12)0.0366 (5)
H460.2736871.1653720.8780820.044*
C470.39007 (16)1.06340 (12)0.90685 (12)0.0329 (4)
H470.4275761.0942120.9028990.039*
C480.42706 (14)0.97426 (11)0.92772 (11)0.0262 (4)
H480.4891870.9462020.9373820.031*
C490.56412 (11)0.58864 (10)0.64647 (9)0.0174 (3)
C500.57011 (12)0.53499 (10)0.59164 (10)0.0192 (3)
H500.5083870.5247390.6091620.023*
C510.58260 (12)0.58163 (10)0.50230 (10)0.0195 (3)
C520.51097 (13)0.60167 (10)0.46238 (11)0.0225 (3)
H520.4556300.5873780.4909970.027*
C530.52074 (14)0.64282 (11)0.38019 (11)0.0260 (4)
H530.4718090.6563020.3545920.031*
C540.60332 (14)0.66364 (11)0.33663 (11)0.0273 (4)
H540.6105020.6901680.2815560.033*
C550.67510 (13)0.64478 (11)0.37547 (11)0.0262 (4)
H550.7304550.6589280.3464370.031*
C560.66473 (12)0.60474 (11)0.45774 (10)0.0231 (3)
H560.7128370.5931730.4834970.028*
C570.65133 (13)0.44844 (10)0.60972 (10)0.0225 (3)
C580.64922 (15)0.40498 (11)0.69087 (11)0.0293 (4)
H580.5980610.4279820.7322120.035*
C590.72236 (18)0.32799 (12)0.71066 (13)0.0394 (5)
H590.7200990.2999030.7650390.047*
C600.79861 (19)0.29282 (13)0.64989 (14)0.0468 (6)
H600.8484410.2417500.6631160.056*
C610.80003 (19)0.33431 (14)0.56931 (14)0.0488 (6)
H610.8504760.3104220.5280700.059*
C620.72678 (16)0.41137 (12)0.54935 (12)0.0350 (4)
H620.7284040.4383900.4948090.042*
C630.72383 (11)0.77861 (10)0.74597 (9)0.0169 (3)
C640.80523 (11)0.80416 (10)0.74729 (10)0.0182 (3)
H640.8429300.7580170.7846320.022*
C650.87439 (11)0.81350 (10)0.66271 (10)0.0180 (3)
C660.95957 (13)0.82589 (12)0.65567 (11)0.0263 (4)
H660.9728670.8263100.7022320.032*
C671.02485 (13)0.83759 (12)0.58085 (12)0.0299 (4)
H671.0811180.8458640.5775990.036*
C681.00631 (12)0.83695 (11)0.51108 (11)0.0247 (4)
H681.0492630.8457780.4605900.030*
C690.92303 (13)0.82302 (12)0.51719 (11)0.0285 (4)
H690.9108040.8213420.4706380.034*
C700.85750 (12)0.81150 (12)0.59241 (11)0.0261 (4)
H700.8017980.8023740.5955750.031*
C710.76376 (11)0.88550 (11)0.77937 (10)0.0197 (3)
C720.70963 (12)0.96398 (11)0.73765 (11)0.0228 (3)
H720.7001130.9679200.6878360.027*
C730.66983 (14)1.03629 (12)0.77002 (13)0.0310 (4)
H730.6328631.0880710.7423320.037*
C740.68524 (15)1.03124 (14)0.84358 (13)0.0379 (5)
H740.6583011.0795530.8653270.045*
C750.74056 (16)0.95449 (14)0.88447 (12)0.0378 (5)
H750.7519260.9513820.9332290.045*
C760.77938 (14)0.88169 (13)0.85280 (11)0.0276 (4)
H760.8160690.8300490.8808980.033*
O100.89816 (10)0.61438 (9)0.89341 (9)0.0355 (3)
O110.88935 (9)0.57424 (8)0.79119 (8)0.0289 (3)
H11A0.8389380.6161860.7923390.043*
C770.93148 (12)0.56702 (11)0.84692 (11)0.0237 (4)
C781.02974 (12)0.49329 (11)0.84603 (11)0.0235 (3)
H781.0395390.4764040.9012720.028*
C791.03147 (12)0.41411 (11)0.82837 (11)0.0237 (4)
C801.05206 (13)0.40451 (11)0.74937 (11)0.0264 (4)
H801.0668500.4467790.7052430.032*
C811.05078 (14)0.33216 (12)0.73555 (12)0.0305 (4)
H811.0648990.3264810.6823820.037*
C821.02850 (16)0.26856 (12)0.80082 (13)0.0359 (4)
H821.0274160.2204420.7916120.043*
C831.00797 (17)0.27756 (13)0.87961 (13)0.0401 (5)
H830.9928340.2353360.9236060.048*
C841.00983 (15)0.34950 (12)0.89346 (12)0.0319 (4)
H840.9965050.3545610.9467200.038*
C851.11269 (12)0.52450 (11)0.78942 (11)0.0242 (4)
C861.10475 (14)0.58408 (12)0.71570 (11)0.0292 (4)
H861.0464940.6073580.6994660.035*
C871.18377 (15)0.60882 (13)0.66634 (13)0.0350 (4)
H871.1776940.6489580.6175030.042*
C881.27130 (15)0.57424 (13)0.68924 (14)0.0386 (5)
H881.3241120.5904090.6556470.046*
C891.27958 (14)0.51551 (13)0.76243 (15)0.0385 (5)
H891.3380450.4922160.7783480.046*
C901.20077 (13)0.49130 (12)0.81212 (13)0.0302 (4)
H901.2068470.4521850.8615030.036*
N60.89316 (15)0.60085 (15)0.47738 (14)0.0648 (7)
C930.88350 (15)0.55719 (16)0.54003 (14)0.0442 (5)
C940.87032 (16)0.50006 (17)0.62001 (14)0.0516 (6)
H94A0.9165050.4435050.6168800.077*
H94B0.8052270.4990290.6371000.077*
H94C0.8805350.5200180.6587350.077*
N70.0085 (7)0.9325 (6)1.0732 (5)0.048 (2)0.25
N7A0.2022 (7)0.8257 (6)1.1303 (6)0.054 (2)0.25
C950.0792 (9)0.9005 (6)1.0992 (6)0.029 (2)0.25
C95A0.1436 (11)0.8766 (8)1.1074 (6)0.032 (3)0.25
C960.1568 (13)0.8685 (14)1.1297 (10)0.077 (5)0.25
H96A0.2111750.8337621.0954440.116*0.25
H96B0.1430950.8343271.1836260.116*0.25
H96C0.1723170.9143381.1322230.116*0.25
C96A0.0590 (11)0.9333 (12)1.0781 (9)0.077 (5)0.25
H96D0.0777310.9538741.0201920.116*0.25
H96E0.0269540.9807301.1044140.116*0.25
H96F0.0152040.9036201.0899380.116*0.25
N50.03424 (17)1.10131 (13)0.70838 (13)0.0529 (5)
C910.00598 (16)1.06094 (13)0.70844 (14)0.0394 (5)
C920.05605 (17)1.00871 (16)0.70753 (17)0.0521 (6)
H92A0.0339380.9949420.6549510.078*
H92B0.1251331.0396430.7183380.078*
H92C0.0421910.9569980.7487000.078*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.01608 (13)0.01387 (13)0.01361 (13)0.00694 (10)0.00404 (10)0.00111 (10)
Ni20.01495 (13)0.01422 (13)0.01300 (13)0.00682 (10)0.00418 (10)0.00069 (10)
O10.0194 (5)0.0220 (6)0.0164 (5)0.0093 (5)0.0027 (4)0.0058 (4)
O20.0202 (6)0.0225 (6)0.0201 (6)0.0103 (5)0.0023 (4)0.0077 (5)
O30.0173 (5)0.0165 (5)0.0179 (5)0.0074 (4)0.0050 (4)0.0000 (4)
O40.0169 (5)0.0210 (5)0.0171 (5)0.0103 (4)0.0056 (4)0.0006 (4)
O50.0235 (6)0.0160 (5)0.0147 (5)0.0089 (4)0.0053 (4)0.0020 (4)
O60.0230 (6)0.0167 (5)0.0144 (5)0.0089 (4)0.0027 (4)0.0019 (4)
O70.0190 (5)0.0175 (5)0.0244 (6)0.0077 (4)0.0106 (5)0.0006 (4)
O80.0207 (6)0.0166 (5)0.0318 (7)0.0083 (5)0.0115 (5)0.0004 (5)
O90.0169 (5)0.0147 (5)0.0155 (5)0.0070 (4)0.0048 (4)0.0025 (4)
N10.0202 (7)0.0165 (6)0.0151 (6)0.0082 (5)0.0053 (5)0.0029 (5)
N20.0213 (7)0.0181 (6)0.0140 (6)0.0100 (5)0.0032 (5)0.0028 (5)
N30.0157 (6)0.0159 (6)0.0157 (6)0.0069 (5)0.0061 (5)0.0001 (5)
N40.0159 (6)0.0173 (6)0.0158 (6)0.0075 (5)0.0055 (5)0.0009 (5)
C10.0210 (8)0.0186 (8)0.0189 (8)0.0089 (6)0.0060 (6)0.0021 (6)
C20.0214 (8)0.0225 (8)0.0241 (9)0.0069 (7)0.0073 (7)0.0045 (7)
C30.0275 (9)0.0163 (8)0.0264 (9)0.0039 (7)0.0119 (7)0.0022 (7)
C40.0285 (9)0.0174 (8)0.0179 (8)0.0098 (7)0.0064 (7)0.0005 (6)
C50.0241 (8)0.0171 (7)0.0150 (7)0.0099 (6)0.0041 (6)0.0037 (6)
C60.0231 (8)0.0162 (7)0.0149 (7)0.0087 (6)0.0032 (6)0.0042 (6)
C70.0283 (9)0.0186 (8)0.0194 (8)0.0116 (7)0.0015 (7)0.0028 (6)
C80.0291 (9)0.0249 (8)0.0222 (8)0.0180 (7)0.0026 (7)0.0047 (7)
C90.0226 (8)0.0287 (9)0.0227 (9)0.0127 (7)0.0006 (7)0.0058 (7)
C100.0205 (8)0.0219 (8)0.0200 (8)0.0088 (7)0.0036 (6)0.0040 (6)
C110.0200 (8)0.0196 (8)0.0192 (8)0.0070 (6)0.0051 (6)0.0035 (6)
C120.0243 (8)0.0192 (8)0.0242 (9)0.0070 (7)0.0055 (7)0.0054 (7)
C130.0238 (8)0.0155 (7)0.0288 (9)0.0080 (6)0.0088 (7)0.0006 (7)
C140.0188 (8)0.0197 (8)0.0207 (8)0.0096 (6)0.0051 (6)0.0001 (6)
C150.0144 (7)0.0177 (7)0.0188 (8)0.0075 (6)0.0074 (6)0.0005 (6)
C160.0148 (7)0.0180 (7)0.0167 (7)0.0079 (6)0.0069 (6)0.0002 (6)
C170.0204 (8)0.0215 (8)0.0188 (8)0.0117 (6)0.0070 (6)0.0011 (6)
C180.0216 (8)0.0286 (9)0.0160 (8)0.0128 (7)0.0030 (6)0.0020 (7)
C190.0230 (8)0.0241 (8)0.0189 (8)0.0093 (7)0.0034 (6)0.0053 (6)
C200.0220 (8)0.0179 (7)0.0194 (8)0.0080 (6)0.0062 (6)0.0026 (6)
C210.0179 (7)0.0169 (7)0.0155 (7)0.0079 (6)0.0055 (6)0.0036 (6)
C220.0176 (7)0.0166 (7)0.0196 (8)0.0075 (6)0.0063 (6)0.0017 (6)
C230.0147 (7)0.0211 (8)0.0188 (8)0.0101 (6)0.0054 (6)0.0008 (6)
C240.0189 (8)0.0208 (8)0.0231 (8)0.0094 (6)0.0057 (6)0.0020 (6)
C250.0209 (8)0.0283 (9)0.0267 (9)0.0115 (7)0.0022 (7)0.0102 (7)
C260.0230 (8)0.0376 (10)0.0178 (8)0.0162 (7)0.0046 (7)0.0049 (7)
C270.0202 (8)0.0291 (9)0.0207 (8)0.0118 (7)0.0084 (7)0.0024 (7)
C280.0158 (7)0.0210 (8)0.0218 (8)0.0087 (6)0.0051 (6)0.0019 (6)
C290.0170 (7)0.0224 (8)0.0180 (8)0.0075 (6)0.0080 (6)0.0027 (6)
C300.0400 (11)0.0499 (12)0.0236 (9)0.0289 (10)0.0012 (8)0.0089 (8)
C310.0562 (14)0.0766 (17)0.0221 (10)0.0419 (13)0.0076 (10)0.0149 (11)
C320.0318 (10)0.0579 (13)0.0207 (9)0.0283 (10)0.0051 (8)0.0050 (9)
C330.0267 (9)0.0360 (10)0.0311 (10)0.0200 (8)0.0110 (8)0.0060 (8)
C340.0239 (9)0.0279 (9)0.0284 (9)0.0135 (7)0.0043 (7)0.0042 (7)
C350.0157 (7)0.0183 (7)0.0167 (8)0.0075 (6)0.0042 (6)0.0032 (6)
C360.0221 (8)0.0180 (8)0.0151 (8)0.0088 (6)0.0027 (6)0.0027 (6)
C370.0274 (8)0.0145 (7)0.0171 (8)0.0077 (6)0.0066 (6)0.0041 (6)
C380.0321 (9)0.0227 (8)0.0178 (8)0.0092 (7)0.0056 (7)0.0051 (7)
C390.0463 (11)0.0283 (9)0.0184 (9)0.0110 (8)0.0134 (8)0.0027 (7)
C400.0412 (11)0.0225 (9)0.0305 (10)0.0076 (8)0.0209 (8)0.0045 (7)
C410.0293 (9)0.0250 (9)0.0337 (10)0.0099 (7)0.0120 (8)0.0065 (7)
C420.0287 (9)0.0227 (8)0.0199 (8)0.0114 (7)0.0058 (7)0.0036 (7)
C430.0292 (9)0.0203 (8)0.0131 (7)0.0076 (7)0.0014 (6)0.0055 (6)
C440.0304 (9)0.0270 (9)0.0265 (9)0.0061 (8)0.0075 (7)0.0072 (7)
C450.0365 (11)0.0292 (10)0.0337 (11)0.0026 (8)0.0115 (9)0.0080 (8)
C460.0537 (13)0.0176 (8)0.0282 (10)0.0048 (8)0.0068 (9)0.0060 (7)
C470.0486 (12)0.0230 (9)0.0270 (10)0.0150 (8)0.0038 (8)0.0076 (7)
C480.0345 (10)0.0221 (8)0.0218 (9)0.0100 (7)0.0055 (7)0.0058 (7)
C490.0199 (8)0.0156 (7)0.0167 (8)0.0060 (6)0.0061 (6)0.0018 (6)
C500.0211 (8)0.0206 (8)0.0196 (8)0.0099 (6)0.0040 (6)0.0064 (6)
C510.0234 (8)0.0178 (7)0.0198 (8)0.0064 (6)0.0048 (6)0.0085 (6)
C520.0263 (8)0.0196 (8)0.0253 (9)0.0082 (7)0.0076 (7)0.0075 (7)
C530.0362 (10)0.0219 (8)0.0260 (9)0.0092 (7)0.0159 (8)0.0051 (7)
C540.0429 (11)0.0242 (8)0.0179 (8)0.0143 (8)0.0076 (7)0.0047 (7)
C550.0302 (9)0.0287 (9)0.0211 (9)0.0141 (7)0.0003 (7)0.0088 (7)
C560.0233 (8)0.0263 (8)0.0223 (8)0.0090 (7)0.0051 (7)0.0085 (7)
C570.0306 (9)0.0183 (8)0.0236 (8)0.0098 (7)0.0087 (7)0.0069 (7)
C580.0405 (10)0.0224 (9)0.0243 (9)0.0118 (8)0.0053 (8)0.0062 (7)
C590.0626 (14)0.0239 (9)0.0276 (10)0.0103 (9)0.0167 (10)0.0014 (8)
C600.0593 (14)0.0245 (10)0.0405 (12)0.0073 (10)0.0213 (11)0.0075 (9)
C610.0553 (14)0.0349 (11)0.0337 (11)0.0081 (10)0.0089 (10)0.0141 (9)
C620.0437 (11)0.0268 (9)0.0247 (9)0.0006 (8)0.0091 (8)0.0085 (8)
C630.0168 (7)0.0193 (8)0.0151 (7)0.0072 (6)0.0029 (6)0.0041 (6)
C640.0181 (7)0.0189 (7)0.0197 (8)0.0082 (6)0.0079 (6)0.0010 (6)
C650.0156 (7)0.0150 (7)0.0233 (8)0.0050 (6)0.0058 (6)0.0034 (6)
C660.0229 (8)0.0374 (10)0.0250 (9)0.0161 (8)0.0045 (7)0.0086 (7)
C670.0209 (8)0.0395 (10)0.0348 (10)0.0173 (8)0.0011 (7)0.0116 (8)
C680.0203 (8)0.0233 (8)0.0249 (9)0.0067 (7)0.0005 (7)0.0058 (7)
C690.0234 (9)0.0392 (10)0.0231 (9)0.0093 (8)0.0050 (7)0.0101 (8)
C700.0189 (8)0.0379 (10)0.0262 (9)0.0131 (7)0.0043 (7)0.0095 (8)
C710.0172 (7)0.0248 (8)0.0213 (8)0.0132 (7)0.0014 (6)0.0058 (7)
C720.0223 (8)0.0245 (8)0.0254 (9)0.0124 (7)0.0050 (7)0.0054 (7)
C730.0256 (9)0.0264 (9)0.0425 (11)0.0101 (7)0.0034 (8)0.0132 (8)
C740.0390 (11)0.0393 (11)0.0407 (12)0.0188 (9)0.0053 (9)0.0242 (9)
C750.0474 (12)0.0535 (13)0.0244 (10)0.0271 (10)0.0008 (9)0.0185 (9)
C760.0306 (9)0.0375 (10)0.0214 (9)0.0193 (8)0.0051 (7)0.0058 (7)
O100.0316 (7)0.0343 (7)0.0369 (8)0.0010 (6)0.0093 (6)0.0161 (6)
O110.0232 (6)0.0235 (6)0.0415 (8)0.0022 (5)0.0148 (6)0.0095 (5)
C770.0214 (8)0.0222 (8)0.0261 (9)0.0084 (7)0.0054 (7)0.0028 (7)
C780.0211 (8)0.0244 (8)0.0237 (9)0.0051 (7)0.0075 (7)0.0053 (7)
C790.0181 (8)0.0222 (8)0.0269 (9)0.0037 (7)0.0068 (7)0.0037 (7)
C800.0241 (9)0.0255 (9)0.0262 (9)0.0077 (7)0.0059 (7)0.0030 (7)
C810.0299 (9)0.0303 (9)0.0299 (10)0.0069 (8)0.0082 (8)0.0090 (8)
C820.0430 (11)0.0239 (9)0.0410 (11)0.0087 (8)0.0137 (9)0.0078 (8)
C830.0562 (13)0.0251 (10)0.0330 (11)0.0148 (9)0.0115 (10)0.0021 (8)
C840.0378 (10)0.0256 (9)0.0252 (9)0.0064 (8)0.0075 (8)0.0034 (7)
C850.0215 (8)0.0240 (8)0.0281 (9)0.0059 (7)0.0047 (7)0.0108 (7)
C860.0277 (9)0.0304 (9)0.0288 (10)0.0099 (8)0.0060 (7)0.0069 (8)
C870.0390 (11)0.0306 (10)0.0333 (11)0.0157 (9)0.0014 (8)0.0106 (8)
C880.0282 (10)0.0348 (11)0.0564 (14)0.0157 (8)0.0062 (9)0.0251 (10)
C890.0232 (9)0.0371 (11)0.0619 (14)0.0066 (8)0.0102 (9)0.0245 (10)
C900.0260 (9)0.0281 (9)0.0392 (11)0.0047 (7)0.0120 (8)0.0127 (8)
N60.0373 (11)0.0650 (14)0.0478 (13)0.0032 (10)0.0042 (9)0.0065 (11)
C930.0235 (10)0.0553 (14)0.0355 (12)0.0000 (9)0.0057 (8)0.0077 (11)
C940.0267 (10)0.0723 (17)0.0331 (12)0.0060 (11)0.0043 (9)0.0024 (11)
N70.044 (5)0.063 (6)0.050 (5)0.022 (5)0.013 (4)0.021 (4)
N7A0.043 (5)0.047 (5)0.051 (5)0.016 (4)0.017 (4)0.020 (4)
C950.039 (7)0.026 (4)0.026 (5)0.018 (5)0.003 (5)0.013 (4)
C95A0.036 (7)0.037 (6)0.023 (6)0.021 (6)0.007 (5)0.011 (5)
C960.031 (5)0.096 (9)0.036 (6)0.022 (6)0.005 (4)0.003 (5)
C96A0.031 (5)0.096 (9)0.036 (6)0.022 (6)0.005 (4)0.003 (5)
N50.0647 (14)0.0425 (11)0.0501 (12)0.0274 (10)0.0012 (10)0.0129 (9)
C910.0335 (11)0.0296 (10)0.0421 (12)0.0068 (9)0.0036 (9)0.0036 (9)
C920.0388 (12)0.0487 (13)0.0655 (16)0.0221 (11)0.0200 (11)0.0082 (12)
Geometric parameters (Å, º) top
Ni1—O12.1107 (11)C45—H450.9300
Ni1—O32.0367 (11)C45—C461.388 (3)
Ni1—O52.0654 (11)C46—H460.9300
Ni1—O92.0752 (11)C46—C471.380 (3)
Ni1—N12.1154 (13)C47—H470.9300
Ni1—N22.0672 (13)C47—C481.396 (3)
Ni2—O42.0403 (11)C48—H480.9300
Ni2—O62.0423 (11)C49—C501.538 (2)
Ni2—O72.0633 (11)C50—H500.9800
Ni2—O92.0630 (11)C50—C511.523 (2)
Ni2—N32.0639 (13)C50—C571.536 (2)
Ni2—N42.0921 (13)C51—C521.391 (2)
O1—C491.2575 (19)C51—C561.402 (2)
O2—C491.2683 (19)C52—H520.9300
O3—C211.2546 (19)C52—C531.394 (2)
O4—C211.2640 (19)C53—H530.9300
O5—C351.2685 (19)C53—C541.386 (3)
O6—C351.2497 (19)C54—H540.9300
O7—C631.2461 (19)C54—C551.385 (3)
O8—C631.2762 (19)C55—H550.9300
O9—H9A0.91 (3)C55—C561.391 (2)
O9—H9B0.96 (3)C56—H560.9300
N1—C11.342 (2)C57—C581.396 (2)
N1—C51.351 (2)C57—C621.385 (3)
N2—C61.355 (2)C58—H580.9300
N2—C101.338 (2)C58—C591.386 (3)
N3—C111.336 (2)C59—H590.9300
N3—C151.348 (2)C59—C601.382 (3)
N4—C161.357 (2)C60—H600.9300
N4—C201.339 (2)C60—C611.381 (3)
C1—H10.9300C61—H610.9300
C1—C21.391 (2)C61—C621.388 (3)
C2—H20.9300C62—H620.9300
C2—C31.389 (2)C63—C641.529 (2)
C3—H30.9300C64—H640.9800
C3—C41.386 (2)C64—C651.528 (2)
C4—H40.9300C64—C711.527 (2)
C4—C51.398 (2)C65—C661.395 (2)
C5—C61.489 (2)C65—C701.388 (2)
C6—C71.389 (2)C66—H660.9300
C7—H70.9300C66—C671.386 (3)
C7—C81.390 (3)C67—H670.9300
C8—H80.9300C67—C681.382 (3)
C8—C91.387 (3)C68—H680.9300
C9—H90.9300C68—C691.385 (3)
C9—C101.387 (2)C69—H690.9300
C10—H100.9300C69—C701.392 (2)
C11—H110.9300C70—H700.9300
C11—C121.387 (2)C71—C721.396 (2)
C12—H120.9300C71—C761.394 (2)
C12—C131.386 (2)C72—H720.9300
C13—H130.9300C72—C731.391 (2)
C13—C141.387 (2)C73—H730.9300
C14—H140.9300C73—C741.388 (3)
C14—C151.394 (2)C74—H740.9300
C15—C161.484 (2)C74—C751.380 (3)
C16—C171.394 (2)C75—H750.9300
C17—H170.9300C75—C761.393 (3)
C17—C181.386 (2)C76—H760.9300
C18—H180.9300O10—C771.210 (2)
C18—C191.388 (2)O11—H11A0.8200
C19—H190.9300O11—C771.321 (2)
C19—C201.385 (2)C77—C781.532 (2)
C20—H200.9300C78—H780.9800
C21—C221.547 (2)C78—C791.528 (2)
C22—H220.9800C78—C851.528 (2)
C22—C231.525 (2)C79—C801.390 (3)
C22—C291.524 (2)C79—C841.397 (3)
C23—C241.396 (2)C80—H800.9300
C23—C281.399 (2)C80—C811.396 (3)
C24—H240.9300C81—H810.9300
C24—C251.391 (2)C81—C821.390 (3)
C25—H250.9300C82—H820.9300
C25—C261.393 (3)C82—C831.383 (3)
C26—H260.9300C83—H830.9300
C26—C271.384 (3)C83—C841.393 (3)
C27—H270.9300C84—H840.9300
C27—C281.392 (2)C85—C861.395 (3)
C28—H280.9300C85—C901.393 (3)
C29—C301.389 (3)C86—H860.9300
C29—C341.388 (2)C86—C871.392 (3)
C30—H300.9300C87—H870.9300
C30—C311.391 (3)C87—C881.385 (3)
C31—H310.9300C88—H880.9300
C31—C321.390 (3)C88—C891.382 (3)
C32—H320.9300C89—H890.9300
C32—C331.376 (3)C89—C901.387 (3)
C33—H330.9300C90—H900.9300
C33—C341.395 (2)N6—C931.133 (3)
C34—H340.9300C93—C941.458 (3)
C35—C361.549 (2)C94—H94A0.9600
C36—H360.9800C94—H94B0.9600
C36—C371.521 (2)C94—H94C0.9600
C36—C431.529 (2)N7—C951.184 (15)
C37—C381.393 (2)N7A—C95A1.062 (15)
C37—C421.397 (2)C95—C961.324 (19)
C38—H380.9300C95A—C96A1.424 (17)
C38—C391.393 (3)C96—H96A0.9600
C39—H390.9300C96—H96B0.9600
C39—C401.385 (3)C96—H96C0.9600
C40—H400.9300C96A—H96D0.9600
C40—C411.389 (3)C96A—H96E0.9600
C41—H410.9300C96A—H96F0.9600
C41—C421.393 (2)N5—C911.136 (3)
C42—H420.9300C91—C921.452 (3)
C43—C441.391 (3)C92—H92A0.9600
C43—C481.393 (3)C92—H92B0.9600
C44—H440.9300C92—H92C0.9600
C44—C451.395 (3)
O1—Ni1—N188.76 (5)C41—C42—C37120.72 (16)
O3—Ni1—O187.17 (4)C41—C42—H42119.6
O3—Ni1—O589.56 (4)C44—C43—C36118.50 (16)
O3—Ni1—O998.04 (4)C44—C43—C48118.20 (16)
O3—Ni1—N1168.74 (5)C48—C43—C36123.25 (16)
O3—Ni1—N290.73 (5)C43—C44—H44119.4
O5—Ni1—O1176.31 (4)C43—C44—C45121.14 (19)
O5—Ni1—O988.97 (4)C45—C44—H44119.4
O5—Ni1—N194.77 (5)C44—C45—H45120.0
O5—Ni1—N292.21 (5)C46—C45—C44119.92 (19)
O9—Ni1—O189.79 (4)C46—C45—H45120.0
O9—Ni1—N192.44 (5)C45—C46—H46120.2
N2—Ni1—O189.55 (5)C47—C46—C45119.63 (17)
N2—Ni1—O9171.17 (5)C47—C46—H46120.2
N2—Ni1—N178.74 (5)C46—C47—H47119.8
O4—Ni2—O691.24 (5)C46—C47—C48120.32 (19)
O4—Ni2—O7176.60 (4)C48—C47—H47119.8
O4—Ni2—O994.49 (4)C43—C48—C47120.80 (18)
O4—Ni2—N393.24 (5)C43—C48—H48119.6
O4—Ni2—N492.72 (5)C47—C48—H48119.6
O6—Ni2—O788.03 (5)O1—C49—O2125.58 (14)
O6—Ni2—O990.43 (4)O1—C49—C50118.18 (14)
O6—Ni2—N392.11 (5)O2—C49—C50116.19 (14)
O6—Ni2—N4170.92 (5)C49—C50—H50107.7
O7—Ni2—N383.47 (5)C51—C50—C49111.94 (13)
O7—Ni2—N487.53 (5)C51—C50—H50107.7
O9—Ni2—O788.84 (4)C51—C50—C57115.15 (13)
O9—Ni2—N3171.81 (5)C57—C50—C49106.33 (13)
O9—Ni2—N497.39 (5)C57—C50—H50107.7
N3—Ni2—N479.52 (5)C52—C51—C50119.45 (15)
C49—O1—Ni1123.88 (10)C52—C51—C56118.11 (15)
C21—O3—Ni1133.52 (10)C56—C51—C50122.44 (15)
C21—O4—Ni2125.18 (10)C51—C52—H52119.4
C35—O5—Ni1123.96 (10)C51—C52—C53121.11 (17)
C35—O6—Ni2136.92 (10)C53—C52—H52119.4
C63—O7—Ni2134.27 (10)C52—C53—H53120.0
Ni1—O9—H9A118.5 (16)C54—C53—C52120.02 (17)
Ni1—O9—H9B97.3 (16)C54—C53—H53120.0
Ni2—O9—Ni1114.61 (5)C53—C54—H54120.1
Ni2—O9—H9A96.8 (16)C55—C54—C53119.70 (16)
Ni2—O9—H9B123.8 (16)C55—C54—H54120.1
H9A—O9—H9B107 (2)C54—C55—H55119.9
C1—N1—Ni1127.18 (11)C54—C55—C56120.25 (17)
C1—N1—C5118.55 (14)C56—C55—H55119.9
C5—N1—Ni1114.25 (10)C51—C56—H56119.6
C6—N2—Ni1116.03 (11)C55—C56—C51120.78 (16)
C10—N2—Ni1125.10 (11)C55—C56—H56119.6
C10—N2—C6118.84 (14)C58—C57—C50118.56 (15)
C11—N3—Ni2125.40 (11)C62—C57—C50123.18 (16)
C11—N3—C15119.12 (13)C62—C57—C58118.26 (17)
C15—N3—Ni2115.04 (10)C57—C58—H58119.6
C16—N4—Ni2113.83 (10)C59—C58—C57120.88 (18)
C20—N4—Ni2127.69 (11)C59—C58—H58119.6
C20—N4—C16118.39 (13)C58—C59—H59119.9
N1—C1—H1118.4C60—C59—C58120.23 (19)
N1—C1—C2123.13 (15)C60—C59—H59119.9
C2—C1—H1118.4C59—C60—H60120.4
C1—C2—H2121.0C61—C60—C59119.29 (19)
C3—C2—C1118.07 (15)C61—C60—H60120.4
C3—C2—H2121.0C60—C61—H61119.7
C2—C3—H3120.2C60—C61—C62120.6 (2)
C4—C3—C2119.57 (15)C62—C61—H61119.7
C4—C3—H3120.2C57—C62—C61120.74 (18)
C3—C4—H4120.5C57—C62—H62119.6
C3—C4—C5118.93 (15)C61—C62—H62119.6
C5—C4—H4120.5O7—C63—O8124.10 (14)
N1—C5—C4121.70 (15)O7—C63—C64117.08 (14)
N1—C5—C6115.78 (14)O8—C63—C64118.80 (14)
C4—C5—C6122.52 (14)C63—C64—H64107.8
N2—C6—C5115.18 (14)C65—C64—C63110.54 (13)
N2—C6—C7121.64 (15)C65—C64—H64107.8
C7—C6—C5123.17 (15)C71—C64—C63111.36 (13)
C6—C7—H7120.4C71—C64—H64107.8
C6—C7—C8119.16 (16)C71—C64—C65111.45 (13)
C8—C7—H7120.4C66—C65—C64117.71 (15)
C7—C8—H8120.5C70—C65—C64124.37 (14)
C9—C8—C7118.93 (16)C70—C65—C66117.92 (15)
C9—C8—H8120.5C65—C66—H66119.3
C8—C9—H9120.6C67—C66—C65121.50 (17)
C8—C9—C10118.88 (16)C67—C66—H66119.3
C10—C9—H9120.6C66—C67—H67120.0
N2—C10—C9122.54 (16)C68—C67—C66119.99 (16)
N2—C10—H10118.7C68—C67—H67120.0
C9—C10—H10118.7C67—C68—H68120.4
N3—C11—H11118.8C67—C68—C69119.28 (16)
N3—C11—C12122.32 (15)C69—C68—H68120.4
C12—C11—H11118.8C68—C69—H69119.7
C11—C12—H12120.6C68—C69—C70120.57 (17)
C13—C12—C11118.87 (16)C70—C69—H69119.7
C13—C12—H12120.6C65—C70—C69120.72 (16)
C12—C13—H13120.4C65—C70—H70119.6
C12—C13—C14119.18 (15)C69—C70—H70119.6
C14—C13—H13120.4C72—C71—C64121.94 (15)
C13—C14—H14120.6C76—C71—C64119.37 (15)
C13—C14—C15118.77 (15)C76—C71—C72118.69 (16)
C15—C14—H14120.6C71—C72—H72119.7
N3—C15—C14121.73 (15)C73—C72—C71120.51 (17)
N3—C15—C16115.72 (13)C73—C72—H72119.7
C14—C15—C16122.54 (14)C72—C73—H73120.0
N4—C16—C15115.70 (13)C74—C73—C72120.07 (19)
N4—C16—C17121.52 (14)C74—C73—H73120.0
C17—C16—C15122.78 (14)C73—C74—H74120.0
C16—C17—H17120.3C75—C74—C73119.97 (18)
C18—C17—C16119.34 (15)C75—C74—H74120.0
C18—C17—H17120.3C74—C75—H75119.9
C17—C18—H18120.5C74—C75—C76120.10 (18)
C17—C18—C19118.92 (15)C76—C75—H75119.9
C19—C18—H18120.5C71—C76—H76119.7
C18—C19—H19120.7C75—C76—C71120.62 (18)
C20—C19—C18118.66 (15)C75—C76—H76119.7
C20—C19—H19120.7C77—O11—H11A109.5
N4—C20—C19123.08 (15)O10—C77—O11124.32 (16)
N4—C20—H20118.5O10—C77—C78122.31 (16)
C19—C20—H20118.5O11—C77—C78113.35 (15)
O3—C21—O4127.39 (14)C77—C78—H78106.5
O3—C21—C22117.61 (13)C79—C78—C77113.32 (14)
O4—C21—C22115.00 (13)C79—C78—H78106.5
C21—C22—H22106.5C85—C78—C77110.22 (14)
C23—C22—C21109.61 (13)C85—C78—H78106.5
C23—C22—H22106.5C85—C78—C79113.39 (14)
C29—C22—C21112.83 (13)C80—C79—C78122.31 (16)
C29—C22—H22106.5C80—C79—C84118.39 (17)
C29—C22—C23114.34 (13)C84—C79—C78119.29 (16)
C24—C23—C22121.23 (14)C79—C80—H80119.6
C24—C23—C28118.61 (15)C79—C80—C81120.74 (17)
C28—C23—C22120.16 (14)C81—C80—H80119.6
C23—C24—H24119.7C80—C81—H81119.8
C25—C24—C23120.58 (15)C82—C81—C80120.34 (18)
C25—C24—H24119.7C82—C81—H81119.8
C24—C25—H25119.9C81—C82—H82120.3
C24—C25—C26120.11 (16)C83—C82—C81119.31 (19)
C26—C25—H25119.9C83—C82—H82120.3
C25—C26—H26120.1C82—C83—H83119.8
C27—C26—C25119.86 (16)C82—C83—C84120.39 (19)
C27—C26—H26120.1C84—C83—H83119.8
C26—C27—H27120.0C79—C84—H84119.6
C26—C27—C28120.03 (16)C83—C84—C79120.83 (18)
C28—C27—H27120.0C83—C84—H84119.6
C23—C28—H28119.6C86—C85—C78123.14 (16)
C27—C28—C23120.79 (16)C90—C85—C78118.46 (16)
C27—C28—H28119.6C90—C85—C86118.40 (17)
C30—C29—C22119.11 (15)C85—C86—H86119.9
C34—C29—C22122.88 (15)C87—C86—C85120.21 (18)
C34—C29—C30118.00 (16)C87—C86—H86119.9
C29—C30—H30119.5C86—C87—H87119.7
C29—C30—C31121.05 (19)C88—C87—C86120.6 (2)
C31—C30—H30119.5C88—C87—H87119.7
C30—C31—H31119.9C87—C88—H88120.3
C32—C31—C30120.2 (2)C89—C88—C87119.49 (19)
C32—C31—H31119.9C89—C88—H88120.3
C31—C32—H32120.3C88—C89—H89120.0
C33—C32—C31119.38 (18)C88—C89—C90120.04 (19)
C33—C32—H32120.3C90—C89—H89120.0
C32—C33—H33119.9C85—C90—H90119.4
C32—C33—C34120.13 (18)C89—C90—C85121.20 (19)
C34—C33—H33119.9C89—C90—H90119.4
C29—C34—C33121.24 (17)N6—C93—C94178.8 (3)
C29—C34—H34119.4C93—C94—H94A109.5
C33—C34—H34119.4C93—C94—H94B109.5
O5—C35—C36115.18 (13)C93—C94—H94C109.5
O6—C35—O5127.83 (14)H94A—C94—H94B109.5
O6—C35—C36116.99 (13)H94A—C94—H94C109.5
C35—C36—H36106.7H94B—C94—H94C109.5
C37—C36—C35110.00 (13)N7—C95—C96176.9 (13)
C37—C36—H36106.7N7A—C95A—C96A169.9 (14)
C37—C36—C43114.12 (13)C95—C96—H96A109.5
C43—C36—C35112.06 (13)C95—C96—H96B109.5
C43—C36—H36106.7C95—C96—H96C109.5
C38—C37—C36119.95 (15)H96A—C96—H96B109.5
C38—C37—C42118.61 (16)H96A—C96—H96C109.5
C42—C37—C36121.44 (14)H96B—C96—H96C109.5
C37—C38—H38119.6C95A—C96A—H96D109.5
C37—C38—C39120.81 (17)C95A—C96A—H96E109.5
C39—C38—H38119.6C95A—C96A—H96F109.5
C38—C39—H39120.0H96D—C96A—H96E109.5
C40—C39—C38119.95 (17)H96D—C96A—H96F109.5
C40—C39—H39120.0H96E—C96A—H96F109.5
C39—C40—H40120.0N5—C91—C92179.1 (3)
C39—C40—C41120.03 (17)C91—C92—H92A109.5
C41—C40—H40120.0C91—C92—H92B109.5
C40—C41—H41120.1C91—C92—H92C109.5
C40—C41—C42119.85 (18)H92A—C92—H92B109.5
C42—C41—H41120.1H92A—C92—H92C109.5
C37—C42—H42119.6H92B—C92—H92C109.5
Ni1—O1—C49—O29.0 (2)C32—C33—C34—C290.6 (3)
Ni1—O1—C49—C50168.31 (10)C34—C29—C30—C310.6 (3)
Ni1—O3—C21—O411.4 (2)C35—C36—C37—C38136.86 (15)
Ni1—O3—C21—C22168.64 (10)C35—C36—C37—C4243.5 (2)
Ni1—O5—C35—O617.7 (2)C35—C36—C43—C4479.46 (19)
Ni1—O5—C35—C36162.19 (10)C35—C36—C43—C4897.84 (18)
Ni1—N1—C1—C2178.37 (12)C36—C37—C38—C39178.49 (15)
Ni1—N1—C5—C4179.59 (12)C36—C37—C42—C41178.79 (15)
Ni1—N1—C5—C60.31 (17)C36—C43—C44—C45177.24 (16)
Ni1—N2—C6—C51.56 (17)C36—C43—C48—C47177.35 (16)
Ni1—N2—C6—C7177.95 (12)C37—C36—C43—C44154.68 (15)
Ni1—N2—C10—C9177.38 (12)C37—C36—C43—C4828.0 (2)
Ni2—O4—C21—O330.4 (2)C37—C38—C39—C400.2 (3)
Ni2—O4—C21—C22149.50 (10)C38—C37—C42—C410.8 (2)
Ni2—O6—C35—O519.0 (3)C38—C39—C40—C411.1 (3)
Ni2—O6—C35—C36161.12 (11)C39—C40—C41—C421.4 (3)
Ni2—O7—C63—O86.9 (2)C40—C41—C42—C370.4 (3)
Ni2—O7—C63—C64171.48 (10)C42—C37—C38—C391.1 (2)
Ni2—N3—C11—C12172.60 (12)C43—C36—C37—C3896.21 (18)
Ni2—N3—C15—C14174.00 (12)C43—C36—C37—C4283.38 (18)
Ni2—N3—C15—C164.83 (17)C43—C44—C45—C460.3 (3)
Ni2—N4—C16—C150.71 (16)C44—C43—C48—C470.0 (3)
Ni2—N4—C16—C17178.80 (11)C44—C45—C46—C470.1 (3)
Ni2—N4—C20—C19175.35 (12)C45—C46—C47—C480.1 (3)
O1—C49—C50—C51123.84 (15)C46—C47—C48—C430.2 (3)
O1—C49—C50—C57109.61 (16)C48—C43—C44—C450.2 (3)
O2—C49—C50—C5158.63 (18)C49—C50—C51—C52117.76 (16)
O2—C49—C50—C5767.92 (17)C49—C50—C51—C5662.9 (2)
O3—C21—C22—C23116.76 (15)C49—C50—C57—C5850.4 (2)
O3—C21—C22—C2911.9 (2)C49—C50—C57—C62129.54 (18)
O4—C21—C22—C2363.30 (17)C50—C51—C52—C53178.72 (15)
O4—C21—C22—C29168.04 (13)C50—C51—C56—C55177.84 (15)
O5—C35—C36—C3763.75 (18)C50—C57—C58—C59177.98 (17)
O5—C35—C36—C43168.18 (14)C50—C57—C62—C61177.9 (2)
O6—C35—C36—C37116.34 (15)C51—C50—C57—C58174.98 (15)
O6—C35—C36—C4311.7 (2)C51—C50—C57—C625.0 (2)
O7—C63—C64—C6580.18 (17)C51—C52—C53—C540.7 (3)
O7—C63—C64—C7144.29 (19)C52—C51—C56—C551.5 (2)
O8—C63—C64—C6598.32 (16)C52—C53—C54—C551.2 (3)
O8—C63—C64—C71137.21 (15)C53—C54—C55—C560.3 (3)
N1—C1—C2—C31.4 (3)C54—C55—C56—C511.0 (3)
N1—C5—C6—N21.2 (2)C56—C51—C52—C530.6 (2)
N1—C5—C6—C7178.27 (15)C57—C50—C51—C52120.64 (16)
N2—C6—C7—C80.0 (2)C57—C50—C51—C5658.7 (2)
N3—C11—C12—C130.1 (3)C57—C58—C59—C600.3 (3)
N3—C15—C16—N42.7 (2)C58—C57—C62—C612.0 (3)
N3—C15—C16—C17177.77 (14)C58—C59—C60—C611.3 (4)
N4—C16—C17—C183.4 (2)C59—C60—C61—C621.2 (4)
C1—N1—C5—C42.0 (2)C60—C61—C62—C570.5 (4)
C1—N1—C5—C6178.09 (13)C62—C57—C58—C592.0 (3)
C1—C2—C3—C41.3 (3)C63—C64—C65—C66172.01 (14)
C2—C3—C4—C50.4 (2)C63—C64—C65—C708.8 (2)
C3—C4—C5—N12.1 (2)C63—C64—C71—C7264.78 (19)
C3—C4—C5—C6177.99 (15)C63—C64—C71—C76114.66 (16)
C4—C5—C6—N2178.67 (14)C64—C65—C66—C67177.99 (16)
C4—C5—C6—C71.8 (2)C64—C65—C70—C69178.10 (16)
C5—N1—C1—C20.2 (2)C64—C71—C72—C73177.64 (15)
C5—C6—C7—C8179.47 (15)C64—C71—C76—C75178.55 (16)
C6—N2—C10—C91.0 (2)C65—C64—C71—C7259.17 (19)
C6—C7—C8—C90.1 (3)C65—C64—C71—C76121.40 (16)
C7—C8—C9—C100.3 (3)C65—C66—C67—C680.1 (3)
C8—C9—C10—N20.8 (3)C66—C65—C70—C691.1 (3)
C10—N2—C6—C5179.97 (14)C66—C67—C68—C691.1 (3)
C10—N2—C6—C70.5 (2)C67—C68—C69—C701.3 (3)
C11—N3—C15—C141.3 (2)C68—C69—C70—C650.2 (3)
C11—N3—C15—C16177.58 (13)C70—C65—C66—C671.2 (3)
C11—C12—C13—C140.4 (2)C71—C64—C65—C6663.58 (19)
C12—C13—C14—C150.2 (2)C71—C64—C65—C70115.60 (18)
C13—C14—C15—N31.0 (2)C71—C72—C73—C741.2 (3)
C13—C14—C15—C16177.73 (15)C72—C71—C76—C750.9 (3)
C14—C15—C16—N4176.09 (14)C72—C73—C74—C750.4 (3)
C14—C15—C16—C173.4 (2)C73—C74—C75—C761.2 (3)
C15—N3—C11—C120.7 (2)C74—C75—C76—C710.6 (3)
C15—C16—C17—C18176.08 (15)C76—C71—C72—C731.8 (2)
C16—N4—C20—C191.0 (2)O10—C77—C78—C79144.02 (18)
C16—C17—C18—C191.8 (2)O10—C77—C78—C8587.7 (2)
C17—C18—C19—C201.0 (2)O11—C77—C78—C7937.5 (2)
C18—C19—C20—N42.5 (3)O11—C77—C78—C8590.73 (18)
C20—N4—C16—C15177.53 (13)C77—C78—C79—C8085.1 (2)
C20—N4—C16—C172.0 (2)C77—C78—C79—C8493.60 (19)
C21—C22—C23—C2442.37 (19)C77—C78—C85—C8637.8 (2)
C21—C22—C23—C28136.44 (14)C77—C78—C85—C90142.80 (16)
C21—C22—C29—C3089.29 (19)C78—C79—C80—C81178.50 (16)
C21—C22—C29—C3489.59 (19)C78—C79—C84—C83178.14 (18)
C22—C23—C24—C25179.96 (15)C78—C85—C86—C87179.00 (17)
C22—C23—C28—C27178.87 (14)C78—C85—C90—C89178.42 (17)
C22—C29—C30—C31179.56 (19)C79—C78—C85—C8690.4 (2)
C22—C29—C34—C33178.85 (16)C79—C78—C85—C9088.97 (19)
C23—C22—C29—C30144.56 (16)C79—C80—C81—C820.2 (3)
C23—C22—C29—C3436.6 (2)C80—C79—C84—C830.6 (3)
C23—C24—C25—C261.5 (2)C80—C81—C82—C830.2 (3)
C24—C23—C28—C270.0 (2)C81—C82—C83—C840.2 (3)
C24—C25—C26—C270.6 (2)C82—C83—C84—C790.6 (3)
C25—C26—C27—C280.6 (2)C84—C79—C80—C810.2 (3)
C26—C27—C28—C230.9 (2)C85—C78—C79—C8041.5 (2)
C28—C23—C24—C251.2 (2)C85—C78—C79—C84139.79 (17)
C29—C22—C23—C2485.45 (18)C85—C86—C87—C880.6 (3)
C29—C22—C23—C2895.74 (17)C86—C85—C90—C891.0 (3)
C29—C30—C31—C320.7 (4)C86—C87—C88—C890.9 (3)
C30—C29—C34—C330.0 (3)C87—C88—C89—C900.3 (3)
C30—C31—C32—C330.1 (4)C88—C89—C90—C850.7 (3)
C31—C32—C33—C340.6 (3)C90—C85—C86—C870.4 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O9—H9A···O80.91 (3)1.74 (3)2.6461 (16)173 (2)
O9—H9B···O20.96 (3)1.53 (3)2.4777 (15)169 (3)
O11—H11A···O80.821.762.5599 (16)164
C4—H4···O5i0.932.483.3253 (19)152
C17—H17···O4ii0.932.483.3493 (19)155
C10—H10···O30.932.463.015 (2)118
C11—H11···O60.932.523.0646 (19)118
C20—H20···O20.932.323.2283 (19)167
C94—H94B···O20.962.553.295 (2)135
Symmetry codes: (i) x+1, y+1, z+2; (ii) x+1, y+2, z+1.
 

Footnotes

Additional correspondence author, e-mail: vladgeo17@mail.ru

Acknowledgements

We thank the X-ray Diffraction Centre of the St Petersburg State University for the X-ray data collections.

Funding information

This research was executed as part of a government assignment (16-116071450050-6), and supported by Russian Ministry of Science and Higher Education (4.4697.2017/6.7) and RFBR (19-08-01232).

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