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Bis[μ-N'-(adamantan-1-ylcarbon-yl)-2-oxidobenzohydrazidato(3-)]tetra-pyridine-trinickel(II) dimethyl-formamide monosolvate monohydrate.
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MedLine Citation:
PMID:  22590119     Owner:  NLM     Status:  In-Data-Review    
Abstract/OtherAbstract:
In the title trinuclear Ni(II) compound, [Ni(3)(C(18)H(19)N(2)O(3))(2)(C(5)H(5)N)(4)]·C(3)H(7)NO·H(2)O, three Ni(II) cations are bridged by two N'-(adamantan-1-ylcarbon-yl)-2-oxidobenzohydrazidate trianions. The central Ni(II) cation has a distorted octa-hedral N(4)O(2) coordination environment where a reverse torsion occurs between the two bridging ligands, whereas the two Ni(II) cations on the sides each adopt an N(2)O(2) square-planar coordination. Weak intra-molecular C-H⋯O and C-H⋯N inter-actions help to stabilize the mol-ecular structure. In the crystal, the lattice water mol-ecule links with the Ni(II) complex and dimethyl-formamide solvent mol-ecule via O-H⋯O hydrogen bonding.
Authors:
Han-Chang Wei; Wan-Yun Huang; Xiang Zhou; Meng Shi; Fu-Pei Liang
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Publication Detail:
Type:  Journal Article     Date:  2012-04-18
Journal Detail:
Title:  Acta crystallographica. Section E, Structure reports online     Volume:  68     ISSN:  1600-5368     ISO Abbreviation:  Acta Crystallogr Sect E Struct Rep Online     Publication Date:  2012 May 
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Created Date:  2012-05-16     Completed Date:  -     Revised Date:  -    
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Nlm Unique ID:  101089178     Medline TA:  Acta Crystallogr Sect E Struct Rep Online     Country:  United States    
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Languages:  eng     Pagination:  m619-20     Citation Subset:  -    
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Journal ID (nlm-ta): Acta Crystallogr Sect E Struct Rep Online
Journal ID (iso-abbrev): Acta Crystallogr Sect E Struct Rep Online
Journal ID (publisher-id): Acta Cryst. E
ISSN: 1600-5368
Publisher: International Union of Crystallography
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A full version of this article is available from Crystallography Journals Online.© Wei et al. 2012
open-access:
Received Day: 11 Month: 3 Year: 2012
Accepted Day: 28 Month: 3 Year: 2012
collection publication date: Day: 01 Month: 5 Year: 2012
Electronic publication date: Day: 18 Month: 4 Year: 2012
pmc-release publication date: Day: 18 Month: 4 Year: 2012
Volume: 68 Issue: Pt 5
First Page: m619 Last Page: m620
ID: 3344353
PubMed Id: 22590119
Publisher Id: xu5481
DOI: 10.1107/S1600536812013396
Coden: ACSEBH
Publisher Item Identifier: S1600536812013396

Bis[μ-N′-(adamantan-1-ylcarbon­yl)-2-oxidobenzohydrazidato(3−)]tetra­pyridine­trinickel(II) dimethyl­formamide monosolvate monohydrate Alternate Title:[Ni3(C18H19N2O3)2(C5H5N)4]·C3H7NO·H2O
Han-Chang Weia
Wan-Yun Huangb
Xiang Zhoub
Meng Shib
Fu-Pei Liangb*
aNanning Prefecture Education College, Nanning, Guangxi 530001, People’s Republic of China
bKey Laboratory for the Chemistry and Molecular Engineering of Medicinal Resources (Ministry of Education of China), School of Chemistry and Chemical Engineering, Guangxi Normal University, Guilin 541004, People’s Republic of China
Correspondence: Correspondence e-mail: xiaoaojianghunn@yahoo.com.cn

Related literature  

For the use of N-acyl­salicylhydrazide in the construction of polynuclear complexes and metallacrown structures, see: Liu et al. (2008); Moon et al. (2006); Qin et al. (2011); Wang et al. (2005). For applications of complexes with N-acyl­salicyl­hydrazide ligands, see: Alexiou et al. (2003); Li et al. (1996); Zeng et al. (2007); Zhou et al. (2010). For related structures, see: Lin et al. (2007); Meng et al. (2007); Xiao & Jin (2008); Yang & Lin (2005). [Chemical Structure ID: scheme1]


Experimental  
Crystal data  

  • [Ni3(C18H19N2O3)2(C5H5N)4]·C3H7NO·H2O
  • Mr = 1206.35
  • Triclinic,
  • a = 14.3496 (8) Å
  • b = 14.8499 (9) Å
  • c = 15.2256 (9) Å
  • α = 62.061 (1)°
  • β = 72.261 (1)°
  • γ = 85.202 (1)°
  • V = 2723.3 (3) Å3
  • Z = 2
  • Mo Kα radiation
  • μ = 1.09 mm−1
  • T = 185 K
  • 0.27 × 0.22 × 0.15 mm

Data collection  

  • Bruker SMART 1000 CCD area-detector diffractometer
  • Absorption correction: multi-scan (SADABS; Bruker, 2001) Tmin = 0.757, Tmax = 0.853
  • 13829 measured reflections
  • 9496 independent reflections
  • 8034 reflections with I > 2σ(I)
  • Rint = 0.016

Refinement  

  • R[F2 > 2σ(F2)] = 0.037
  • wR(F2) = 0.100
  • S = 1.04
  • 9496 reflections
  • 714 parameters
  • H-atom parameters constrained
  • Δρmax = 0.39 e Å−3
  • Δρmin = −0.66 e Å−3

Data collection: SMART (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.


Supplementary Material

Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536812013396/xu5481sup1.cif

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812013396/xu5481Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report


Notes

fnu1Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: XU5481).

This project was supported by the National Natural Science Foundation of China (grant No. 20971029) and the Guangxi Natural Science Foundation of China (No. 2010GXNSFD013018).

supplementary crystallographic information
Comment

Metal complexes of hydrazide and its ramification have been paid much attention to in recent years because of their prodigious applications in magnetism material, optical material, automatic recognition and assembly of molecules, catalysis and biochemistry, and so on (Alexiou et al., 2003; Li et al., 1996; Zeng et al., 2007; Zhou et al., 2010). N-acylsalicylhydrazide ligands, one of this type of ligand, which contain N, O coordination atoms, the great conjugated system and rich hydrogen-bonded donors and accepters, have been widely used to construct polynuclear complexes and coordination polymers with interesting structural motifs, such as the one-dimensional, the two-dimensional, the three-dimensional and the metallacrown(Liu et al., 2008; Moon et al., 2006; Qin et al., 2011; Wang et al., 2005). For nickel(II) complexes with N-acylsalicylhydrazide ligands, we can see that trinuclear complexes is more common from the former reports (Lin et al., 2007); Meng et al., 2007); Xiao & Jin, 2008); Yang & Lin, 2005) and most of them are unstable in air. We report here a new trinuclear nickel(II) complex, [Ni3(C18H19N2O3)2(py)4].DMF.H2O, which is stable at room temperature. Its molecular configuration was illustrated in Fig. 1.

In the molecular structure, the arrangement of three Ni2+ ions and the ligands which were coordinated to the central Ni2+ ion in axial positions are different from the reported trinuclear nickel(II) complexes containing N-acylsalicylhydrazide ligands (Yang & Lin, 2005; Xiao & Jin, 2008). In this complex, three Ni2+ ions are arranged in an arcuate shape. The central Ni2 atom adopts a distorted octahedral geometry and is coordinated by two hydrazide nitrogen atoms (N1, N4) and two salicyl carbonyl oxygen atoms (O2, O5) from two bridge deprotonated N-adamantanecarbonylsalicylichydrazide ligands (abbreviated as (ashz)3-) in the equatorial plane and by two nitrogen atoms (N7, N10) from twopyridine molecules in the axial positions. There is a reverse torsion to be occurred between the two planes of the bridge (ashz)3- ligands because of the steric hindrance effect caused by adamantly. This torsion led the bond angles of O5—Ni2—N10 and O2—Ni2—N10 to be pressed to 85.958 (3)° and 84.284 (3)° respectively from the ideal 90°. Two other Ni2+ ions on two side adopt square-planar coordination environments and are coordinated respectively by a phenolic oxygen atom, a adamantanecarbonyl oxygen atom, a hydrazide nitrogen atom and a pyridine nitrogen atom. By O(8)—H(8 A)···O(7) and O(8)—H(8B)···O(6) hydrogen bonds, two hydrogen atoms of water molecule are respectively connected to the phenolic oxygen atom(O6) and the oxygen atom(O7) of DMF to forming dimethylformamide solvate monohydrate.

Experimental

Synthesis of ligand H3ashz

Adamantanecarbonyl chloride (6.0 g, 0.03 mol) which was dissolved in tetrahydrofuran(30.0 ml)was dropped slowly into a solution of salicylhydrazide (5.5 g, 0.036 mol) and triethylamine(2.0 ml) dissolved in 60.0 ml of tetrahydrofuran at 0°C. After dropped off, the mixture was slowly warmed up to the room temperature, stirred continually for 24 h and then filtered. The filtrate was recrystallizated by distilled water, and the yellow product was obtained(yield 8.31 g, 87.5%). IR(PE Spectrum One FT—IR Spectrometer, KBr tablet, cm-1): 3352(m), 3243(s), 2915(s), 2851(m), 1665(s), 1637(s), 1608(m), 1531(m), 1515(m), 1495(m), 1456(m). 1278(m), 1236(s), 749(m), 709(m). ESI-Ms: M—H¯ peak at m/z 313.01.

Synthesis of the complex

[Ni3(C18H19N2O3)2(py)4].DMF.H2O Ni(OAc)2.4H2O(0.15 mmol), H3ashz (0.10 mmol) and five drops of pyridine were mixed into the solution of DMF(2 ml) and acetonitrile (10 ml). Stirring for 10 min, the resulting solution was filtered and left to stand at room temperature. Red rhomboid crystals suitable for X-ray analysis were obtained (yield 52.1%) by slowly volatilizing the solvent over a period of two weeks. Carbon, hydrogen and nitrogen were determined by a Perkin-Elmer 2400II CHN element analysis instrument. Analysis, calculated for [Ni3(C18H19N2O3)2(py)4].DMF.H2O: C, 58.74%: H, 5.60%; N, 10.44%. found: C, 58.87%; H, 5.60%; N, 10.53%. IR(KBr tablet, cm-1): 3468(w), 3071(w), 2903(s), 2840(m), 1670(m), 1597(s), 1569(s), 1503(s), 1481(s), 1443(s), 1403(s), 1334(m), 1305(m), 1264(m), 753(s), 693(s).

Refinement

H atoms were placed in geometrically calculated positions and refined as riding atoms, with O—H = 0.85 and C—H = 0.95–1.00 Å and Uiso(H) = 1.5Ueq(C) for methyl H atoms and 1.2Ueq(C,O) for the others.

Figures
Crystal data
Data collection
Refinement
Special details
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)
Atomic displacement parameters (Å2)
Geometric parameters (Å, º)
Hydrogen-bond geometry (Å, º)

Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1, −y+1, −z.


References
Alexiou, M., Tsivikas, I., Dendrinou-Samara, C., Pantazaki, A. A., Trikalitis, P., Lalioti, N., Kyriakidis, D. A. & Kessissoglou, D. P. (2003). J. Inorg. Biochem.93, 256–264.
Bruker. (2001). SADABS Bruker AXS Inc., Madison, Wisconsin, USA.
Bruker. (2007). SMART and SAINT Bruker AXS Inc., Madison, Wisconsin, USA.
Li, S.-X., Hu, S.-Z. & Wu, W.-S. (1996). Chin. J. Struct. Chem.15(2), 134–137.
Lin, S., Yang, M.-X. & Liu, S.-X. (2007). Polyhedron, 26, 4793–4798.
Liu, W. L., Lee, K., Park, M., Jonh, R. P., Moon, D., Zou, Y., Liu, X. F., Ri, H. C., Kim, G. H. & Lah, M. S. (2008). Inorg. Chem.47, 8807–8812.
Meng, X.-G., Lou, W., Sun, X.-Z., Xiao, F.-P., Shen, J.-F., Zhong, Y., Cheng, G.-Z. & Ji, Z.-P. (2007). Inorg. Chem. Commun.10, 1351–1353.
Moon, D., Leek, K., John, R. P., Kim, G. H., Suh, B. J. & Lah, M. S. (2006). Inorg. Chem.45, 7991–8004.
Qin, S.-N., Zu, C., Chen, Z.-L., Huang, W.-Y., Qin, J.-K. & Liang, F.-P. (2011). Inorg. Chem. Commun.11, 1036–1038.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122.
Wang, C.-X., Du, C.-X., Li, Y.-H. & Wu, Y.-J. (2005). Inorg. Chem. Commun.8, 379–381.
Xiao, F.-P. & Jin, L.-F. (2008). Z. Anorg. Allg. Chem.34, 397–402.
Yang, M.-X. & Lin, S. (2005). Acta Cryst. E61, m1095–m1096.
Zeng, M.-H., Yao, M.-X., Liang, H., Zhang, W.-X. & Chen, X.-M. (2007). Angew. Chem. Int. Ed.46, 1832–1835.
Zhou, Y.-L., Zeng, M.-H., Wei, L.-Q., Li, B.-W. & Kurmoo, M. (2010). Chem. Mater.22, 4295–4303.

Figures

[Figure ID: Fap1]
Fig. 1. 

Molecular structure of the title compound. H atoms not involved in hydrogen bonds have been omitted for clarity. Symmetry codes: (i) -1+x, y, z; (ii) x, 1-y, -z; (iii) x, y, -1+z.



Tables
[TableWrap ID: d1e372]
[Ni3(C18H19N2O3)2(C5H5N)4]·C3H7NO·H2O Z = 2
Mr = 1206.35 F(000) = 1264
Triclinic, P1 Dx = 1.471 Mg m3
Hall symbol: -P 1 Mo Kα radiation, λ = 0.71073 Å
a = 14.3496 (8) Å Cell parameters from 6088 reflections
b = 14.8499 (9) Å θ = 2.2–26.0°
c = 15.2256 (9) Å µ = 1.09 mm1
α = 62.061 (1)° T = 185 K
β = 72.261 (1)° Block, red
γ = 85.202 (1)° 0.27 × 0.22 × 0.15 mm
V = 2723.3 (3) Å3

[TableWrap ID: d1e535]
Bruker SMART 1000 CCD area-detector diffractometer 9496 independent reflections
Radiation source: fine-focus sealed tube 8034 reflections with I > 2σ(I)
Graphite monochromator Rint = 0.016
φ and ω scans θmax = 25.1°, θmin = 1.6°
Absorption correction: multi-scan (SADABS; Bruker, 2001) h = −16→17
Tmin = 0.757, Tmax = 0.853 k = −17→17
13829 measured reflections l = −15→18

[TableWrap ID: d1e652]
Refinement on F2 Primary atom site location: structure-invariant direct methods
Least-squares matrix: full Secondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.037 Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.100 H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.0519P)2 + 1.7341P] where P = (Fo2 + 2Fc2)/3
9496 reflections (Δ/σ)max < 0.001
714 parameters Δρmax = 0.39 e Å3
0 restraints Δρmin = −0.66 e Å3

[TableWrap ID: d1e809]
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.

[TableWrap ID: d1e908]
x y z Uiso*/Ueq
C1 0.29062 (18) 0.3762 (2) 0.3952 (2) 0.0228 (6)
C2 0.35980 (19) 0.4437 (2) 0.2850 (2) 0.0258 (6)
H2A 0.3704 0.4078 0.2424 0.031*
H2B 0.3294 0.5082 0.2507 0.031*
C3 0.3398 (2) 0.2765 (2) 0.4466 (2) 0.0299 (6)
H3A 0.2965 0.2322 0.5176 0.036*
H3B 0.3501 0.2393 0.4053 0.036*
C4 0.4391 (2) 0.3006 (3) 0.4531 (2) 0.0360 (7)
H4 0.4703 0.2354 0.4863 0.043*
C5 0.5064 (2) 0.3679 (3) 0.3430 (2) 0.0364 (7)
H5A 0.5175 0.3315 0.3008 0.044*
H5B 0.5706 0.3831 0.3466 0.044*
C6 0.4585 (2) 0.4677 (2) 0.2919 (2) 0.0320 (7)
H6 0.5026 0.5116 0.2201 0.038*
C7 0.4238 (2) 0.3567 (3) 0.5181 (3) 0.0439 (8)
H7A 0.4877 0.3716 0.5227 0.053*
H7B 0.3811 0.3132 0.5897 0.053*
C8 0.3763 (2) 0.4563 (3) 0.4670 (3) 0.0404 (8)
H8 0.3661 0.4930 0.5096 0.048*
C9 0.4435 (2) 0.5240 (3) 0.3569 (3) 0.0403 (8)
H9A 0.4135 0.5891 0.3240 0.048*
H9B 0.5076 0.5398 0.3604 0.048*
C10 0.2769 (2) 0.4329 (2) 0.4610 (2) 0.0313 (7)
H10A 0.2457 0.4975 0.4291 0.038*
H10B 0.2331 0.3901 0.5323 0.038*
C11 0.19072 (18) 0.3516 (2) 0.39238 (19) 0.0216 (5)
C12 0.04791 (18) 0.30740 (19) 0.27002 (19) 0.0213 (5)
C13 −0.05672 (18) 0.28752 (19) 0.2881 (2) 0.0223 (5)
C14 −0.0812 (2) 0.2582 (2) 0.2221 (2) 0.0279 (6)
H14 −0.0301 0.2530 0.1681 0.033*
C15 −0.1763 (2) 0.2367 (2) 0.2332 (2) 0.0327 (7)
H15 −0.1907 0.2155 0.1885 0.039*
C16 −0.2518 (2) 0.2463 (2) 0.3109 (2) 0.0345 (7)
H16 −0.3181 0.2333 0.3182 0.041*
C17 −0.23028 (19) 0.2746 (2) 0.3770 (2) 0.0307 (6)
H17 −0.2825 0.2814 0.4292 0.037*
C18 −0.13288 (19) 0.2938 (2) 0.3693 (2) 0.0243 (6)
C19 −0.1626 (2) 0.2900 (2) 0.6377 (2) 0.0325 (7)
H19 −0.1903 0.2518 0.6150 0.039*
C20 −0.2156 (2) 0.2941 (2) 0.7278 (2) 0.0362 (7)
H20 −0.2779 0.2578 0.7673 0.043*
C21 −0.1772 (2) 0.3516 (2) 0.7602 (2) 0.0364 (7)
H21 −0.2131 0.3560 0.8216 0.044*
C22 −0.0864 (2) 0.4021 (2) 0.7018 (2) 0.0324 (7)
H22 −0.0590 0.4433 0.7215 0.039*
C23 −0.0353 (2) 0.3926 (2) 0.6140 (2) 0.0279 (6)
H23 0.0287 0.4253 0.5757 0.033*
C24 0.2374 (2) 0.4137 (2) −0.0965 (2) 0.0319 (6)
H24A 0.2207 0.4227 −0.0331 0.038*
H24B 0.3019 0.4507 −0.1430 0.038*
C25 0.1590 (2) 0.4585 (2) −0.1525 (2) 0.0350 (7)
H25 0.1561 0.5329 −0.1721 0.042*
C26 0.0597 (2) 0.4028 (2) −0.0788 (2) 0.0360 (7)
H26A 0.0083 0.4319 −0.1135 0.043*
H26B 0.0429 0.4117 −0.0154 0.043*
C27 0.0641 (2) 0.2892 (2) −0.0488 (2) 0.0336 (7)
H27 −0.0012 0.2529 −0.0009 0.040*
C28 0.0900 (2) 0.2746 (3) −0.1456 (2) 0.0392 (7)
H28A 0.0385 0.3009 −0.1807 0.047*
H28B 0.0937 0.2010 −0.1257 0.047*
C29 0.1886 (2) 0.3319 (3) −0.2198 (2) 0.0392 (8)
H29 0.2049 0.3230 −0.2839 0.047*
C30 0.2681 (2) 0.2875 (3) −0.1657 (2) 0.0345 (7)
H30A 0.3325 0.3236 −0.2136 0.041*
H30B 0.2722 0.2143 −0.1476 0.041*
C31 0.1426 (2) 0.2434 (2) 0.0066 (2) 0.0289 (6)
H31A 0.1450 0.1698 0.0260 0.035*
H31B 0.1256 0.2502 0.0712 0.035*
C32 0.1844 (2) 0.4455 (3) −0.2508 (2) 0.0413 (8)
H32A 0.1341 0.4748 −0.2869 0.050*
H32B 0.2486 0.4820 −0.2989 0.050*
C33 0.32242 (19) 0.2535 (2) −0.0119 (2) 0.0247 (6)
C34 0.24377 (19) 0.2993 (2) −0.0659 (2) 0.0243 (6)
C35 0.42577 (18) 0.1992 (2) 0.1817 (2) 0.0222 (5)
C36 0.50165 (19) 0.1339 (2) 0.2230 (2) 0.0264 (6)
C37 0.5680 (2) 0.0860 (2) 0.1709 (2) 0.0331 (7)
C38 0.6336 (2) 0.0212 (3) 0.2204 (3) 0.0467 (9)
H38 0.6772 −0.0131 0.1871 0.056*
C39 0.6363 (2) 0.0061 (3) 0.3159 (3) 0.0469 (9)
H39 0.6819 −0.0372 0.3472 0.056*
C40 0.5723 (2) 0.0543 (3) 0.3662 (3) 0.0407 (8)
H40 0.5738 0.0445 0.4320 0.049*
C41 0.5066 (2) 0.1165 (2) 0.3199 (2) 0.0309 (6)
H41 0.4628 0.1490 0.3551 0.037*
C42 0.6283 (2) 0.0585 (2) −0.0914 (3) 0.0362 (7)
H42 0.6447 0.0297 −0.0281 0.043*
C43 0.6803 (2) 0.0324 (3) −0.1681 (3) 0.0433 (8)
H43 0.7317 −0.0124 −0.1578 0.052*
C44 0.6563 (2) 0.0725 (3) −0.2593 (3) 0.0464 (9)
H44 0.6907 0.0555 −0.3130 0.056*
C45 0.5820 (2) 0.1375 (3) −0.2717 (3) 0.0477 (9)
H45 0.5640 0.1662 −0.3341 0.057*
C46 0.5337 (2) 0.1605 (3) −0.1918 (3) 0.0407 (8)
H46 0.4822 0.2054 −0.2009 0.049*
C47 0.37565 (19) 0.4790 (2) 0.0152 (2) 0.0283 (6)
H47 0.4239 0.4310 0.0160 0.034*
C48 0.3986 (2) 0.5787 (2) −0.0627 (2) 0.0339 (7)
H48 0.4616 0.5988 −0.1131 0.041*
C49 0.3285 (2) 0.6488 (2) −0.0661 (2) 0.0358 (7)
H49 0.3420 0.7178 −0.1192 0.043*
C50 0.2380 (2) 0.6164 (2) 0.0096 (2) 0.0330 (7)
H50 0.1880 0.6626 0.0091 0.040*
C51 0.2220 (2) 0.5157 (2) 0.0856 (2) 0.0269 (6)
H51 0.1601 0.4942 0.1380 0.032*
C52 0.1332 (2) 0.0861 (2) 0.2905 (2) 0.0290 (6)
H52 0.1220 0.1183 0.2243 0.035*
C53 0.2090 (2) 0.0869 (2) 0.4018 (2) 0.0327 (7)
H53 0.2526 0.1194 0.4160 0.039*
C54 0.1647 (2) −0.0083 (2) 0.4786 (2) 0.0398 (8)
H54 0.1775 −0.0398 0.5439 0.048*
C55 0.0864 (2) −0.0088 (2) 0.3630 (2) 0.0372 (7)
H55 0.0441 −0.0408 0.3469 0.045*
C59 −0.0459 (3) 0.0942 (4) 0.8286 (4) 0.0659 (11)
H59 −0.0609 0.1617 0.7873 0.079*
C60 0.0721 (4) −0.0299 (4) 0.8530 (5) 0.115 (2)
H60A 0.1205 −0.0217 0.8827 0.172*
H60B 0.1021 −0.0607 0.8073 0.172*
H60C 0.0158 −0.0744 0.9093 0.172*
C61 0.1112 (3) 0.1364 (4) 0.6989 (3) 0.0745 (13)
H61A 0.0816 0.2009 0.6660 0.112*
H61B 0.1313 0.1063 0.6515 0.112*
H61C 0.1686 0.1494 0.7144 0.112*
N1 0.17739 (14) 0.33462 (16) 0.31992 (16) 0.0207 (5)
N2 0.07407 (14) 0.31891 (17) 0.34132 (16) 0.0209 (5)
N3 −0.07305 (16) 0.33827 (18) 0.58081 (17) 0.0264 (5)
N4 0.32325 (15) 0.25005 (17) 0.07580 (17) 0.0224 (5)
N5 0.40790 (15) 0.19873 (17) 0.10142 (17) 0.0238 (5)
N6 0.55583 (16) 0.12256 (19) −0.10201 (19) 0.0311 (5)
N7 0.28944 (15) 0.44640 (17) 0.08939 (16) 0.0217 (5)
N8 0.0404 (2) 0.0667 (2) 0.7946 (3) 0.0532 (8)
C62 0.1021 (2) −0.0562 (2) 0.4588 (2) 0.0390 (7)
H62 0.0701 −0.1211 0.5105 0.047*
N10 0.19352 (16) 0.13518 (17) 0.30863 (17) 0.0255 (5)
Ni1 −0.00220 (2) 0.32886 (3) 0.45606 (3) 0.02189 (10)
Ni2 0.24878 (2) 0.29225 (3) 0.19742 (2) 0.01995 (9)
Ni3 0.48439 (2) 0.15812 (3) 0.00729 (3) 0.02747 (10)
O1 0.11573 (13) 0.34834 (15) 0.46962 (14) 0.0266 (4)
O2 0.11103 (12) 0.31102 (14) 0.18823 (13) 0.0220 (4)
O3 −0.11911 (13) 0.31607 (15) 0.43894 (14) 0.0279 (4)
O4 0.39292 (14) 0.21619 (16) −0.06013 (15) 0.0320 (5)
O5 0.37708 (12) 0.24968 (14) 0.22717 (14) 0.0252 (4)
O6 0.57437 (14) 0.09919 (18) 0.07684 (17) 0.0400 (5)
O7 −0.1092 (2) 0.0409 (3) 0.9089 (3) 0.0913 (11)
O8 0.2154 (3) 0.8318 (3) 0.0105 (3) 0.1010 (12)
H8B 0.2758 0.8522 −0.0146 0.121*
H8A 0.1839 0.8705 0.0345 0.121*

[TableWrap ID: d1e2867]
U11 U22 U33 U12 U13 U23
C1 0.0212 (13) 0.0271 (14) 0.0230 (14) 0.0013 (11) −0.0071 (11) −0.0137 (12)
C2 0.0239 (14) 0.0304 (15) 0.0240 (14) 0.0002 (12) −0.0054 (11) −0.0141 (12)
C3 0.0283 (15) 0.0338 (16) 0.0276 (15) 0.0035 (12) −0.0102 (12) −0.0134 (13)
C4 0.0278 (15) 0.0461 (19) 0.0400 (17) 0.0085 (14) −0.0185 (14) −0.0206 (15)
C5 0.0231 (14) 0.052 (2) 0.0422 (18) 0.0041 (14) −0.0113 (13) −0.0275 (16)
C6 0.0217 (14) 0.0419 (18) 0.0324 (16) −0.0059 (13) −0.0032 (12) −0.0190 (14)
C7 0.0322 (17) 0.070 (2) 0.0373 (18) −0.0011 (16) −0.0166 (14) −0.0273 (18)
C8 0.0330 (16) 0.063 (2) 0.0461 (19) −0.0016 (15) −0.0109 (14) −0.0418 (18)
C9 0.0295 (16) 0.050 (2) 0.053 (2) −0.0046 (14) −0.0106 (15) −0.0339 (17)
C10 0.0290 (15) 0.0447 (18) 0.0298 (15) 0.0033 (13) −0.0089 (12) −0.0251 (14)
C11 0.0216 (13) 0.0208 (13) 0.0209 (13) 0.0021 (11) −0.0063 (11) −0.0086 (11)
C12 0.0233 (13) 0.0176 (13) 0.0218 (13) 0.0041 (10) −0.0086 (11) −0.0076 (11)
C13 0.0197 (13) 0.0199 (13) 0.0242 (14) 0.0019 (10) −0.0082 (11) −0.0069 (11)
C14 0.0265 (14) 0.0333 (16) 0.0276 (15) 0.0056 (12) −0.0108 (12) −0.0162 (13)
C15 0.0301 (15) 0.0392 (17) 0.0367 (17) 0.0019 (13) −0.0152 (13) −0.0209 (14)
C16 0.0242 (15) 0.0390 (18) 0.0428 (18) 0.0020 (13) −0.0132 (13) −0.0192 (15)
C17 0.0203 (14) 0.0358 (17) 0.0334 (16) 0.0045 (12) −0.0054 (12) −0.0161 (13)
C18 0.0237 (13) 0.0225 (14) 0.0243 (14) 0.0039 (11) −0.0074 (11) −0.0092 (11)
C19 0.0285 (15) 0.0390 (17) 0.0290 (15) −0.0002 (13) −0.0028 (12) −0.0182 (14)
C20 0.0287 (15) 0.0429 (18) 0.0281 (16) 0.0012 (14) 0.0008 (12) −0.0151 (14)
C21 0.0401 (17) 0.0429 (18) 0.0271 (16) 0.0132 (15) −0.0061 (13) −0.0212 (14)
C22 0.0404 (17) 0.0335 (16) 0.0318 (16) 0.0125 (14) −0.0155 (14) −0.0209 (14)
C23 0.0280 (14) 0.0295 (15) 0.0271 (15) 0.0044 (12) −0.0099 (12) −0.0134 (13)
C24 0.0346 (16) 0.0306 (16) 0.0338 (16) 0.0027 (13) −0.0130 (13) −0.0161 (13)
C25 0.0460 (18) 0.0265 (16) 0.0359 (17) 0.0062 (14) −0.0204 (14) −0.0130 (13)
C26 0.0341 (16) 0.0458 (19) 0.0361 (17) 0.0154 (14) −0.0194 (14) −0.0220 (15)
C27 0.0298 (15) 0.0387 (17) 0.0314 (16) −0.0002 (13) −0.0119 (13) −0.0135 (14)
C28 0.0503 (19) 0.0368 (18) 0.0417 (18) 0.0061 (15) −0.0286 (16) −0.0187 (15)
C29 0.0503 (19) 0.049 (2) 0.0259 (16) 0.0110 (16) −0.0180 (14) −0.0207 (15)
C30 0.0394 (17) 0.0446 (19) 0.0255 (15) 0.0098 (14) −0.0113 (13) −0.0212 (14)
C31 0.0304 (15) 0.0310 (16) 0.0247 (14) 0.0017 (12) −0.0098 (12) −0.0116 (12)
C32 0.0472 (19) 0.0436 (19) 0.0267 (16) 0.0047 (15) −0.0159 (14) −0.0088 (14)
C33 0.0221 (13) 0.0252 (14) 0.0263 (14) 0.0023 (11) −0.0045 (11) −0.0135 (12)
C34 0.0270 (14) 0.0288 (15) 0.0219 (14) 0.0051 (12) −0.0085 (11) −0.0153 (12)
C35 0.0189 (13) 0.0202 (13) 0.0252 (14) 0.0000 (10) −0.0044 (11) −0.0098 (11)
C36 0.0196 (13) 0.0234 (14) 0.0349 (16) 0.0023 (11) −0.0085 (12) −0.0126 (12)
C37 0.0264 (15) 0.0354 (17) 0.0438 (18) 0.0089 (13) −0.0142 (13) −0.0225 (14)
C38 0.0337 (17) 0.054 (2) 0.064 (2) 0.0227 (16) −0.0216 (17) −0.0357 (19)
C39 0.0396 (18) 0.046 (2) 0.060 (2) 0.0202 (16) −0.0303 (17) −0.0215 (18)
C40 0.0344 (17) 0.046 (2) 0.0403 (18) 0.0066 (15) −0.0181 (14) −0.0152 (15)
C41 0.0263 (14) 0.0329 (16) 0.0322 (16) 0.0049 (12) −0.0104 (12) −0.0136 (13)
C42 0.0305 (16) 0.0313 (17) 0.0423 (18) 0.0044 (13) −0.0026 (13) −0.0190 (14)
C43 0.0399 (18) 0.0385 (19) 0.051 (2) 0.0077 (15) −0.0027 (16) −0.0281 (17)
C44 0.0412 (19) 0.052 (2) 0.052 (2) −0.0002 (16) 0.0056 (16) −0.0393 (18)
C45 0.0409 (19) 0.065 (2) 0.045 (2) 0.0048 (17) −0.0049 (16) −0.0367 (19)
C46 0.0296 (16) 0.052 (2) 0.0433 (19) 0.0060 (15) −0.0043 (14) −0.0289 (17)
C47 0.0227 (14) 0.0369 (17) 0.0275 (15) 0.0014 (12) −0.0081 (12) −0.0163 (13)
C48 0.0263 (15) 0.0441 (18) 0.0266 (15) −0.0067 (13) −0.0061 (12) −0.0125 (14)
C49 0.0414 (17) 0.0292 (16) 0.0310 (16) −0.0070 (14) −0.0132 (14) −0.0068 (13)
C50 0.0370 (16) 0.0272 (16) 0.0342 (16) 0.0054 (13) −0.0110 (13) −0.0142 (13)
C51 0.0300 (15) 0.0270 (15) 0.0255 (14) 0.0031 (12) −0.0059 (12) −0.0156 (12)
C52 0.0335 (15) 0.0264 (15) 0.0276 (15) 0.0029 (12) −0.0098 (12) −0.0127 (12)
C53 0.0384 (16) 0.0301 (16) 0.0309 (16) 0.0036 (13) −0.0137 (13) −0.0135 (13)
C54 0.056 (2) 0.0329 (17) 0.0248 (16) 0.0079 (15) −0.0145 (15) −0.0082 (13)
C55 0.0380 (17) 0.0290 (16) 0.0439 (19) −0.0007 (13) −0.0125 (14) −0.0158 (14)
C59 0.054 (2) 0.069 (3) 0.088 (3) 0.014 (2) −0.023 (2) −0.048 (3)
C60 0.072 (3) 0.061 (3) 0.136 (5) 0.023 (3) −0.002 (3) −0.006 (3)
C61 0.080 (3) 0.068 (3) 0.066 (3) 0.001 (2) −0.013 (2) −0.029 (2)
N1 0.0151 (10) 0.0241 (12) 0.0219 (11) 0.0009 (9) −0.0050 (9) −0.0102 (9)
N2 0.0158 (10) 0.0261 (12) 0.0202 (11) 0.0003 (9) −0.0043 (9) −0.0109 (9)
N3 0.0254 (12) 0.0298 (13) 0.0240 (12) 0.0032 (10) −0.0053 (10) −0.0141 (10)
N4 0.0203 (11) 0.0229 (12) 0.0253 (12) 0.0070 (9) −0.0084 (9) −0.0121 (10)
N5 0.0178 (11) 0.0253 (12) 0.0294 (12) 0.0069 (9) −0.0073 (9) −0.0144 (10)
N6 0.0250 (12) 0.0323 (14) 0.0361 (14) 0.0027 (10) −0.0028 (10) −0.0200 (11)
N7 0.0230 (11) 0.0241 (12) 0.0195 (11) 0.0016 (9) −0.0064 (9) −0.0111 (9)
N8 0.0508 (18) 0.0444 (18) 0.072 (2) 0.0105 (15) −0.0221 (16) −0.0325 (17)
C62 0.0445 (18) 0.0221 (15) 0.0374 (18) 0.0008 (13) −0.0065 (14) −0.0068 (13)
N10 0.0253 (12) 0.0252 (12) 0.0243 (12) 0.0058 (10) −0.0068 (10) −0.0114 (10)
Ni1 0.01830 (17) 0.0270 (2) 0.02113 (18) 0.00131 (14) −0.00339 (14) −0.01332 (15)
Ni2 0.01796 (17) 0.02193 (18) 0.02015 (18) 0.00337 (13) −0.00538 (13) −0.01051 (14)
Ni3 0.02173 (18) 0.0325 (2) 0.0326 (2) 0.00796 (15) −0.00624 (15) −0.02078 (17)
O1 0.0220 (9) 0.0373 (11) 0.0223 (10) −0.0003 (8) −0.0033 (8) −0.0171 (9)
O2 0.0203 (9) 0.0279 (10) 0.0191 (9) 0.0030 (8) −0.0062 (7) −0.0122 (8)
O3 0.0195 (9) 0.0387 (12) 0.0287 (10) 0.0031 (8) −0.0049 (8) −0.0199 (9)
O4 0.0289 (10) 0.0426 (12) 0.0322 (11) 0.0137 (9) −0.0097 (9) −0.0252 (10)
O5 0.0221 (9) 0.0299 (10) 0.0289 (10) 0.0070 (8) −0.0092 (8) −0.0178 (9)
O6 0.0298 (11) 0.0536 (14) 0.0497 (14) 0.0211 (10) −0.0163 (10) −0.0348 (12)
O7 0.0562 (19) 0.088 (2) 0.124 (3) 0.0048 (18) −0.004 (2) −0.058 (2)
O8 0.092 (3) 0.090 (3) 0.104 (3) 0.002 (2) −0.002 (2) −0.048 (2)

[TableWrap ID: d1e4438]
C1—C11 1.526 (3) C32—H32B 0.9900
C1—C3 1.542 (4) C33—O4 1.306 (3)
C1—C2 1.544 (4) C33—N4 1.315 (3)
C1—C10 1.548 (4) C33—C34 1.525 (4)
C2—C6 1.535 (4) C35—O5 1.278 (3)
C2—H2A 0.9900 C35—N5 1.326 (3)
C2—H2B 0.9900 C35—C36 1.480 (3)
C3—C4 1.540 (4) C36—C41 1.397 (4)
C3—H3A 0.9900 C36—C37 1.413 (4)
C3—H3B 0.9900 C37—O6 1.326 (4)
C4—C7 1.528 (4) C37—C38 1.409 (4)
C4—C5 1.531 (4) C38—C39 1.375 (5)
C4—H4 1.0000 C38—H38 0.9500
C5—C6 1.532 (4) C39—C40 1.385 (5)
C5—H5A 0.9900 C39—H39 0.9500
C5—H5B 0.9900 C40—C41 1.374 (4)
C6—C9 1.529 (4) C40—H40 0.9500
C6—H6 1.0000 C41—H41 0.9500
C7—C8 1.528 (5) C42—N6 1.343 (4)
C7—H7A 0.9900 C42—C43 1.384 (4)
C7—H7B 0.9900 C42—H42 0.9500
C8—C9 1.533 (5) C43—C44 1.373 (5)
C8—C10 1.535 (4) C43—H43 0.9500
C8—H8 1.0000 C44—C45 1.374 (5)
C9—H9A 0.9900 C44—H44 0.9500
C9—H9B 0.9900 C45—C46 1.383 (4)
C10—H10A 0.9900 C45—H45 0.9500
C10—H10B 0.9900 C46—N6 1.342 (4)
C11—N1 1.310 (3) C46—H46 0.9500
C11—O1 1.314 (3) C47—N7 1.333 (3)
C12—O2 1.278 (3) C47—C48 1.381 (4)
C12—N2 1.335 (3) C47—H47 0.9500
C12—C13 1.471 (3) C48—C49 1.380 (4)
C13—C14 1.404 (4) C48—H48 0.9500
C13—C18 1.414 (4) C49—C50 1.385 (4)
C14—C15 1.369 (4) C49—H49 0.9500
C14—H14 0.9500 C50—C51 1.379 (4)
C15—C16 1.394 (4) C50—H50 0.9500
C15—H15 0.9500 C51—N7 1.346 (3)
C16—C17 1.375 (4) C51—H51 0.9500
C16—H16 0.9500 C52—N10 1.341 (4)
C17—C18 1.408 (4) C52—C55 1.380 (4)
C17—H17 0.9500 C52—H52 0.9500
C18—O3 1.320 (3) C53—N10 1.338 (4)
C19—N3 1.346 (4) C53—C54 1.384 (4)
C19—C20 1.378 (4) C53—H53 0.9500
C19—H19 0.9500 C54—C62 1.370 (5)
C20—C21 1.382 (4) C54—H54 0.9500
C20—H20 0.9500 C55—C62 1.374 (4)
C21—C22 1.373 (4) C55—H55 0.9500
C21—H21 0.9500 C59—O7 1.217 (5)
C22—C23 1.380 (4) C59—N8 1.301 (5)
C22—H22 0.9500 C59—H59 0.9500
C23—N3 1.350 (3) C60—N8 1.413 (5)
C23—H23 0.9500 C60—H60A 0.9800
C24—C25 1.537 (4) C60—H60B 0.9800
C24—C34 1.540 (4) C60—H60C 0.9800
C24—H24A 0.9900 C61—N8 1.445 (5)
C24—H24B 0.9900 C61—H61A 0.9800
C25—C26 1.526 (4) C61—H61B 0.9800
C25—C32 1.529 (4) C61—H61C 0.9800
C25—H25 1.0000 N1—N2 1.432 (3)
C26—C27 1.528 (4) N1—Ni2 2.180 (2)
C26—H26A 0.9900 N2—Ni1 1.822 (2)
C26—H26B 0.9900 N3—Ni1 1.926 (2)
C27—C28 1.520 (4) N4—N5 1.437 (3)
C27—C31 1.535 (4) N4—Ni2 2.176 (2)
C27—H27 1.0000 N5—Ni3 1.834 (2)
C28—C29 1.526 (5) N6—Ni3 1.947 (2)
C28—H28A 0.9900 N7—Ni2 2.097 (2)
C28—H28B 0.9900 C62—H62 0.9500
C29—C32 1.525 (5) N10—Ni2 2.174 (2)
C29—C30 1.535 (4) Ni1—O3 1.8124 (18)
C29—H29 1.0000 Ni1—O1 1.8277 (18)
C30—C34 1.542 (4) Ni2—O5 2.0099 (17)
C30—H30A 0.9900 Ni2—O2 2.0109 (17)
C30—H30B 0.9900 Ni3—O4 1.8226 (19)
C31—C34 1.543 (4) Ni3—O6 1.825 (2)
C31—H31A 0.9900 O8—H8B 0.8500
C31—H31B 0.9900 O8—H8A 0.8500
C32—H32A 0.9900
C11—C1—C3 110.0 (2) H32A—C32—H32B 108.3
C11—C1—C2 111.9 (2) O4—C33—N4 120.3 (2)
C3—C1—C2 108.5 (2) O4—C33—C34 114.5 (2)
C11—C1—C10 109.4 (2) N4—C33—C34 125.3 (2)
C3—C1—C10 108.2 (2) C33—C34—C24 111.4 (2)
C2—C1—C10 108.7 (2) C33—C34—C30 109.7 (2)
C6—C2—C1 110.0 (2) C24—C34—C30 108.4 (2)
C6—C2—H2A 109.7 C33—C34—C31 110.3 (2)
C1—C2—H2A 109.7 C24—C34—C31 108.6 (2)
C6—C2—H2B 109.7 C30—C34—C31 108.4 (2)
C1—C2—H2B 109.7 O5—C35—N5 122.6 (2)
H2A—C2—H2B 108.2 O5—C35—C36 119.3 (2)
C4—C3—C1 110.3 (2) N5—C35—C36 118.0 (2)
C4—C3—H3A 109.6 C41—C36—C37 118.1 (2)
C1—C3—H3A 109.6 C41—C36—C35 118.4 (2)
C4—C3—H3B 109.6 C37—C36—C35 123.5 (2)
C1—C3—H3B 109.6 O6—C37—C38 117.0 (3)
H3A—C3—H3B 108.1 O6—C37—C36 124.5 (3)
C7—C4—C5 109.4 (3) C38—C37—C36 118.5 (3)
C7—C4—C3 109.9 (2) C39—C38—C37 121.7 (3)
C5—C4—C3 109.4 (2) C39—C38—H38 119.2
C7—C4—H4 109.4 C37—C38—H38 119.2
C5—C4—H4 109.4 C38—C39—C40 119.8 (3)
C3—C4—H4 109.4 C38—C39—H39 120.1
C4—C5—C6 109.4 (2) C40—C39—H39 120.1
C4—C5—H5A 109.8 C41—C40—C39 119.3 (3)
C6—C5—H5A 109.8 C41—C40—H40 120.3
C4—C5—H5B 109.8 C39—C40—H40 120.3
C6—C5—H5B 109.8 C40—C41—C36 122.6 (3)
H5A—C5—H5B 108.2 C40—C41—H41 118.7
C9—C6—C5 109.2 (2) C36—C41—H41 118.7
C9—C6—C2 110.3 (2) N6—C42—C43 123.3 (3)
C5—C6—C2 109.5 (2) N6—C42—H42 118.3
C9—C6—H6 109.3 C43—C42—H42 118.3
C5—C6—H6 109.3 C44—C43—C42 118.8 (3)
C2—C6—H6 109.3 C44—C43—H43 120.6
C4—C7—C8 109.1 (2) C42—C43—H43 120.6
C4—C7—H7A 109.9 C43—C44—C45 119.0 (3)
C8—C7—H7A 109.9 C43—C44—H44 120.5
C4—C7—H7B 109.9 C45—C44—H44 120.5
C8—C7—H7B 109.9 C44—C45—C46 118.9 (3)
H7A—C7—H7B 108.3 C44—C45—H45 120.6
C7—C8—C9 109.7 (3) C46—C45—H45 120.6
C7—C8—C10 109.8 (3) N6—C46—C45 123.3 (3)
C9—C8—C10 109.6 (2) N6—C46—H46 118.3
C7—C8—H8 109.3 C45—C46—H46 118.3
C9—C8—H8 109.3 N7—C47—C48 123.6 (3)
C10—C8—H8 109.3 N7—C47—H47 118.2
C6—C9—C8 109.1 (3) C48—C47—H47 118.2
C6—C9—H9A 109.9 C49—C48—C47 118.9 (3)
C8—C9—H9A 109.9 C49—C48—H48 120.6
C6—C9—H9B 109.9 C47—C48—H48 120.6
C8—C9—H9B 109.9 C48—C49—C50 118.6 (3)
H9A—C9—H9B 108.3 C48—C49—H49 120.7
C8—C10—C1 110.3 (2) C50—C49—H49 120.7
C8—C10—H10A 109.6 C51—C50—C49 118.7 (3)
C1—C10—H10A 109.6 C51—C50—H50 120.7
C8—C10—H10B 109.6 C49—C50—H50 120.7
C1—C10—H10B 109.6 N7—C51—C50 123.3 (3)
H10A—C10—H10B 108.1 N7—C51—H51 118.3
N1—C11—O1 120.6 (2) C50—C51—H51 118.3
N1—C11—C1 124.4 (2) N10—C52—C55 123.3 (3)
O1—C11—C1 115.0 (2) N10—C52—H52 118.3
O2—C12—N2 122.0 (2) C55—C52—H52 118.3
O2—C12—C13 119.4 (2) N10—C53—C54 123.2 (3)
N2—C12—C13 118.6 (2) N10—C53—H53 118.4
C14—C13—C18 118.7 (2) C54—C53—H53 118.4
C14—C13—C12 117.6 (2) C62—C54—C53 118.9 (3)
C18—C13—C12 123.7 (2) C62—C54—H54 120.5
C15—C14—C13 122.1 (3) C53—C54—H54 120.5
C15—C14—H14 118.9 C62—C55—C52 118.9 (3)
C13—C14—H14 118.9 C62—C55—H55 120.6
C14—C15—C16 119.2 (3) C52—C55—H55 120.6
C14—C15—H15 120.4 O7—C59—N8 125.6 (5)
C16—C15—H15 120.4 O7—C59—H59 117.2
C17—C16—C15 120.1 (3) N8—C59—H59 117.2
C17—C16—H16 120.0 N8—C60—H60A 109.5
C15—C16—H16 120.0 N8—C60—H60B 109.5
C16—C17—C18 121.7 (3) H60A—C60—H60B 109.5
C16—C17—H17 119.1 N8—C60—H60C 109.5
C18—C17—H17 119.1 H60A—C60—H60C 109.5
O3—C18—C17 117.5 (2) H60B—C60—H60C 109.5
O3—C18—C13 124.5 (2) N8—C61—H61A 109.5
C17—C18—C13 118.0 (2) N8—C61—H61B 109.5
N3—C19—C20 122.1 (3) H61A—C61—H61B 109.5
N3—C19—H19 118.9 N8—C61—H61C 109.5
C20—C19—H19 118.9 H61A—C61—H61C 109.5
C19—C20—C21 119.5 (3) H61B—C61—H61C 109.5
C19—C20—H20 120.2 C11—N1—N2 108.00 (19)
C21—C20—H20 120.2 C11—N1—Ni2 144.34 (17)
C22—C21—C20 118.7 (3) N2—N1—Ni2 106.17 (14)
C22—C21—H21 120.7 C12—N2—N1 115.3 (2)
C20—C21—H21 120.7 C12—N2—Ni1 129.67 (17)
C21—C22—C23 119.3 (3) N1—N2—Ni1 114.78 (15)
C21—C22—H22 120.3 C19—N3—C23 118.0 (2)
C23—C22—H22 120.3 C19—N3—Ni1 120.22 (19)
N3—C23—C22 122.3 (3) C23—N3—Ni1 121.75 (19)
N3—C23—H23 118.8 C33—N4—N5 107.8 (2)
C22—C23—H23 118.8 C33—N4—Ni2 145.27 (17)
C25—C24—C34 110.4 (2) N5—N4—Ni2 106.93 (14)
C25—C24—H24A 109.6 C35—N5—N4 115.3 (2)
C34—C24—H24A 109.6 C35—N5—Ni3 129.29 (17)
C25—C24—H24B 109.6 N4—N5—Ni3 114.77 (15)
C34—C24—H24B 109.6 C46—N6—C42 116.7 (3)
H24A—C24—H24B 108.1 C46—N6—Ni3 121.03 (19)
C26—C25—C32 109.7 (3) C42—N6—Ni3 122.3 (2)
C26—C25—C24 108.9 (2) C47—N7—C51 117.0 (2)
C32—C25—C24 110.0 (2) C47—N7—Ni2 123.50 (18)
C26—C25—H25 109.4 C51—N7—Ni2 119.06 (18)
C32—C25—H25 109.4 C59—N8—C60 121.8 (4)
C24—C25—H25 109.4 C59—N8—C61 121.4 (4)
C25—C26—C27 109.4 (2) C60—N8—C61 116.7 (3)
C25—C26—H26A 109.8 C54—C62—C55 118.9 (3)
C27—C26—H26A 109.8 C54—C62—H62 120.6
C25—C26—H26B 109.8 C55—C62—H62 120.6
C27—C26—H26B 109.8 C53—N10—C52 116.8 (2)
H26A—C26—H26B 108.2 C53—N10—Ni2 122.35 (19)
C28—C27—C26 110.2 (2) C52—N10—Ni2 120.49 (18)
C28—C27—C31 108.6 (2) O3—Ni1—N2 96.43 (8)
C26—C27—C31 110.0 (2) O3—Ni1—O1 177.27 (9)
C28—C27—H27 109.3 N2—Ni1—O1 83.60 (8)
C26—C27—H27 109.3 O3—Ni1—N3 88.29 (9)
C31—C27—H27 109.3 N2—Ni1—N3 175.20 (9)
C27—C28—C29 109.4 (2) O1—Ni1—N3 91.73 (9)
C27—C28—H28A 109.8 O5—Ni2—O2 170.13 (8)
C29—C28—H28A 109.8 O5—Ni2—N7 99.08 (8)
C27—C28—H28B 109.8 O2—Ni2—N7 90.67 (8)
C29—C28—H28B 109.8 O5—Ni2—N10 85.96 (8)
H28A—C28—H28B 108.2 O2—Ni2—N10 84.28 (8)
C28—C29—C32 110.5 (3) N7—Ni2—N10 174.94 (8)
C28—C29—C30 109.0 (3) O5—Ni2—N4 78.18 (7)
C32—C29—C30 109.6 (3) O2—Ni2—N4 103.63 (7)
C28—C29—H29 109.2 N7—Ni2—N4 89.49 (8)
C32—C29—H29 109.2 N10—Ni2—N4 91.97 (8)
C30—C29—H29 109.2 O5—Ni2—N1 100.54 (7)
C29—C30—C34 110.1 (2) O2—Ni2—N1 77.70 (7)
C29—C30—H30A 109.6 N7—Ni2—N1 90.38 (8)
C34—C30—H30A 109.6 N10—Ni2—N1 88.28 (8)
C29—C30—H30B 109.6 N4—Ni2—N1 178.67 (8)
C34—C30—H30B 109.6 O4—Ni3—O6 179.06 (9)
H30A—C30—H30B 108.2 O4—Ni3—N5 83.07 (9)
C27—C31—C34 110.0 (2) O6—Ni3—N5 96.18 (9)
C27—C31—H31A 109.7 O4—Ni3—N6 90.55 (9)
C34—C31—H31A 109.7 O6—Ni3—N6 90.20 (9)
C27—C31—H31B 109.7 N5—Ni3—N6 173.61 (10)
C34—C31—H31B 109.7 C11—O1—Ni1 112.84 (16)
H31A—C31—H31B 108.2 C12—O2—Ni2 113.97 (15)
C29—C32—C25 108.9 (2) C18—O3—Ni1 126.21 (16)
C29—C32—H32A 109.9 C33—O4—Ni3 114.06 (17)
C25—C32—H32A 109.9 C35—O5—Ni2 114.09 (15)
C29—C32—H32B 109.9 C37—O6—Ni3 125.48 (17)
C25—C32—H32B 109.9 H8B—O8—H8A 108.4
C11—C1—C2—C6 179.1 (2) O4—C33—N4—N5 −1.7 (3)
C3—C1—C2—C6 −59.3 (3) C34—C33—N4—N5 178.5 (2)
C10—C1—C2—C6 58.1 (3) O4—C33—N4—Ni2 177.3 (2)
C11—C1—C3—C4 −178.1 (2) C34—C33—N4—Ni2 −2.5 (5)
C2—C1—C3—C4 59.1 (3) O5—C35—N5—N4 −6.4 (4)
C10—C1—C3—C4 −58.6 (3) C36—C35—N5—N4 170.3 (2)
C1—C3—C4—C7 60.1 (3) O5—C35—N5—Ni3 164.11 (19)
C1—C3—C4—C5 −60.0 (3) C36—C35—N5—Ni3 −19.2 (4)
C7—C4—C5—C6 −60.5 (3) C33—N4—N5—C35 172.6 (2)
C3—C4—C5—C6 60.0 (3) Ni2—N4—N5—C35 −6.8 (3)
C4—C5—C6—C9 60.5 (3) C33—N4—N5—Ni3 0.7 (3)
C4—C5—C6—C2 −60.4 (3) Ni2—N4—N5—Ni3 −178.72 (10)
C1—C2—C6—C9 −59.7 (3) C45—C46—N6—C42 −0.6 (5)
C1—C2—C6—C5 60.5 (3) C45—C46—N6—Ni3 −179.9 (3)
C5—C4—C7—C8 60.2 (3) C43—C42—N6—C46 1.0 (4)
C3—C4—C7—C8 −59.9 (3) C43—C42—N6—Ni3 −179.8 (2)
C4—C7—C8—C9 −60.4 (3) C48—C47—N7—C51 0.9 (4)
C4—C7—C8—C10 60.1 (3) C48—C47—N7—Ni2 172.9 (2)
C5—C6—C9—C8 −60.3 (3) C50—C51—N7—C47 0.3 (4)
C2—C6—C9—C8 60.1 (3) C50—C51—N7—Ni2 −172.0 (2)
C7—C8—C9—C6 60.5 (3) O7—C59—N8—C60 −3.6 (7)
C10—C8—C9—C6 −60.1 (3) O7—C59—N8—C61 −178.9 (4)
C7—C8—C10—C1 −60.3 (3) C53—C54—C62—C55 0.8 (5)
C9—C8—C10—C1 60.2 (3) C52—C55—C62—C54 −0.9 (4)
C11—C1—C10—C8 178.7 (2) C54—C53—N10—C52 −1.3 (4)
C3—C1—C10—C8 58.9 (3) C54—C53—N10—Ni2 171.8 (2)
C2—C1—C10—C8 −58.7 (3) C55—C52—N10—C53 1.2 (4)
C3—C1—C11—N1 −84.0 (3) C55—C52—N10—Ni2 −172.0 (2)
C2—C1—C11—N1 36.7 (3) C12—N2—Ni1—O3 0.8 (2)
C10—C1—C11—N1 157.3 (2) N1—N2—Ni1—O3 174.76 (17)
C3—C1—C11—O1 96.0 (3) C12—N2—Ni1—O1 −176.5 (2)
C2—C1—C11—O1 −143.3 (2) N1—N2—Ni1—O1 −2.50 (17)
C10—C1—C11—O1 −22.7 (3) C12—N2—Ni1—N3 170.0 (11)
O2—C12—C13—C14 9.4 (4) N1—N2—Ni1—N3 −16.0 (13)
N2—C12—C13—C14 −169.2 (2) C19—N3—Ni1—O3 30.2 (2)
O2—C12—C13—C18 −172.4 (2) C23—N3—Ni1—O3 −149.9 (2)
N2—C12—C13—C18 9.1 (4) C19—N3—Ni1—N2 −139.1 (11)
C18—C13—C14—C15 0.8 (4) C23—N3—Ni1—N2 40.8 (13)
C12—C13—C14—C15 179.2 (3) C19—N3—Ni1—O1 −152.6 (2)
C13—C14—C15—C16 1.4 (5) C23—N3—Ni1—O1 27.3 (2)
C14—C15—C16—C17 −1.6 (5) C47—N7—Ni2—O5 40.5 (2)
C15—C16—C17—C18 −0.5 (5) C51—N7—Ni2—O5 −147.63 (19)
C16—C17—C18—O3 −177.1 (3) C47—N7—Ni2—O2 −141.0 (2)
C16—C17—C18—C13 2.7 (4) C51—N7—Ni2—O2 30.81 (19)
C14—C13—C18—O3 176.9 (2) C47—N7—Ni2—N10 −144.3 (9)
C12—C13—C18—O3 −1.3 (4) C51—N7—Ni2—N10 27.6 (10)
C14—C13—C18—C17 −2.8 (4) C47—N7—Ni2—N4 −37.4 (2)
C12—C13—C18—C17 178.9 (2) C51—N7—Ni2—N4 134.43 (19)
N3—C19—C20—C21 1.6 (5) C47—N7—Ni2—N1 141.3 (2)
C19—C20—C21—C22 −0.8 (4) C51—N7—Ni2—N1 −46.89 (19)
C20—C21—C22—C23 −1.3 (4) C53—N10—Ni2—O5 47.3 (2)
C21—C22—C23—N3 2.7 (4) C52—N10—Ni2—O5 −139.8 (2)
C34—C24—C25—C26 60.8 (3) C53—N10—Ni2—O2 −131.2 (2)
C34—C24—C25—C32 −59.5 (3) C52—N10—Ni2—O2 41.68 (19)
C32—C25—C26—C27 60.0 (3) C53—N10—Ni2—N7 −128.0 (9)
C24—C25—C26—C27 −60.5 (3) C52—N10—Ni2—N7 44.9 (10)
C25—C26—C27—C28 −59.4 (3) C53—N10—Ni2—N4 125.3 (2)
C25—C26—C27—C31 60.4 (3) C52—N10—Ni2—N4 −61.8 (2)
C26—C27—C28—C29 58.6 (3) C53—N10—Ni2—N1 −53.4 (2)
C31—C27—C28—C29 −62.0 (3) C52—N10—Ni2—N1 119.5 (2)
C27—C28—C29—C32 −59.0 (3) C33—N4—Ni2—O5 −167.6 (3)
C27—C28—C29—C30 61.6 (3) N5—N4—Ni2—O5 11.41 (15)
C28—C29—C30—C34 −60.1 (3) C33—N4—Ni2—O2 22.4 (3)
C32—C29—C30—C34 61.0 (3) N5—N4—Ni2—O2 −158.64 (15)
C28—C27—C31—C34 61.3 (3) C33—N4—Ni2—N7 −68.2 (3)
C26—C27—C31—C34 −59.5 (3) N5—N4—Ni2—N7 110.80 (16)
C28—C29—C32—C25 59.6 (3) C33—N4—Ni2—N10 107.0 (3)
C30—C29—C32—C25 −60.6 (3) N5—N4—Ni2—N10 −74.04 (16)
C26—C25—C32—C29 −59.9 (3) C33—N4—Ni2—N1 −152 (3)
C24—C25—C32—C29 59.9 (3) N5—N4—Ni2—N1 27 (4)
O4—C33—C34—C24 −119.0 (3) C11—N1—Ni2—O5 10.3 (3)
N4—C33—C34—C24 60.7 (3) N2—N1—Ni2—O5 −152.61 (14)
O4—C33—C34—C30 1.0 (3) C11—N1—Ni2—O2 −179.6 (3)
N4—C33—C34—C30 −179.3 (3) N2—N1—Ni2—O2 17.47 (14)
O4—C33—C34—C31 120.3 (3) C11—N1—Ni2—N7 −89.0 (3)
N4—C33—C34—C31 −59.9 (3) N2—N1—Ni2—N7 108.08 (15)
C25—C24—C34—C33 179.0 (2) C11—N1—Ni2—N10 95.9 (3)
C25—C24—C34—C30 58.3 (3) N2—N1—Ni2—N10 −67.05 (15)
C25—C24—C34—C31 −59.4 (3) C11—N1—Ni2—N4 −5 (4)
C29—C30—C34—C33 179.2 (2) N2—N1—Ni2—N4 −168 (4)
C29—C30—C34—C24 −59.0 (3) C35—N5—Ni3—O4 −170.3 (2)
C29—C30—C34—C31 58.7 (3) N4—N5—Ni3—O4 0.24 (17)
C27—C31—C34—C33 −179.4 (2) C35—N5—Ni3—O6 10.3 (3)
C27—C31—C34—C24 58.3 (3) N4—N5—Ni3—O6 −179.17 (18)
C27—C31—C34—C30 −59.3 (3) C35—N5—Ni3—N6 −166.5 (8)
O5—C35—C36—C41 10.3 (4) N4—N5—Ni3—N6 4.0 (10)
N5—C35—C36—C41 −166.4 (3) C46—N6—Ni3—O4 11.1 (2)
O5—C35—C36—C37 −171.3 (3) C42—N6—Ni3—O4 −168.1 (2)
N5—C35—C36—C37 11.9 (4) C46—N6—Ni3—O6 −169.5 (2)
C41—C36—C37—O6 −177.0 (3) C42—N6—Ni3—O6 11.3 (2)
C35—C36—C37—O6 4.7 (5) C46—N6—Ni3—N5 7.4 (10)
C41—C36—C37—C38 1.8 (4) C42—N6—Ni3—N5 −171.8 (8)
C35—C36—C37—C38 −176.6 (3) N1—C11—O1—Ni1 −4.6 (3)
O6—C37—C38—C39 176.9 (3) C1—C11—O1—Ni1 175.37 (17)
C36—C37—C38—C39 −1.9 (5) O3—Ni1—O1—C11 −87.1 (16)
C37—C38—C39—C40 1.0 (6) N2—Ni1—O1—C11 3.74 (18)
C38—C39—C40—C41 0.2 (5) N3—Ni1—O1—C11 −177.38 (18)
C39—C40—C41—C36 −0.3 (5) N2—C12—O2—Ni2 17.6 (3)
C37—C36—C41—C40 −0.7 (4) C13—C12—O2—Ni2 −160.86 (18)
C35—C36—C41—C40 177.8 (3) O5—Ni2—O2—C12 61.6 (5)
N6—C42—C43—C44 −0.9 (5) N7—Ni2—O2—C12 −109.35 (18)
C42—C43—C44—C45 0.3 (5) N10—Ni2—O2—C12 70.37 (18)
C43—C44—C45—C46 0.0 (5) N4—Ni2—O2—C12 161.02 (17)
C44—C45—C46—N6 0.1 (5) N1—Ni2—O2—C12 −19.11 (17)
N7—C47—C48—C49 −1.4 (4) C17—C18—O3—Ni1 172.16 (19)
C47—C48—C49—C50 0.6 (4) C13—C18—O3—Ni1 −7.6 (4)
C48—C49—C50—C51 0.5 (4) N2—Ni1—O3—C18 7.2 (2)
C49—C50—C51—N7 −1.0 (4) O1—Ni1—O3—C18 97.7 (16)
N10—C53—C54—C62 0.3 (5) N3—Ni1—O3—C18 −171.9 (2)
N10—C52—C55—C62 −0.1 (4) N4—C33—O4—Ni3 2.1 (3)
O1—C11—N1—N2 2.5 (3) C34—C33—O4—Ni3 −178.19 (18)
C1—C11—N1—N2 −177.5 (2) O6—Ni3—O4—C33 37 (6)
O1—C11—N1—Ni2 −160.2 (2) N5—Ni3—O4—C33 −1.17 (19)
C1—C11—N1—Ni2 19.8 (5) N6—Ni3—O4—C33 179.2 (2)
O2—C12—N2—N1 −0.5 (3) N5—C35—O5—Ni2 17.5 (3)
C13—C12—N2—N1 178.0 (2) C36—C35—O5—Ni2 −159.12 (19)
O2—C12—N2—Ni1 173.44 (18) O2—Ni2—O5—C35 86.3 (4)
C13—C12—N2—Ni1 −8.0 (4) N7—Ni2—O5—C35 −102.88 (18)
C11—N1—N2—C12 175.6 (2) N10—Ni2—O5—C35 77.54 (18)
Ni2—N1—N2—C12 −14.7 (2) N4—Ni2—O5—C35 −15.33 (18)
C11—N1—N2—Ni1 0.8 (2) N1—Ni2—O5—C35 165.03 (18)
Ni2—N1—N2—Ni1 170.38 (10) C38—C37—O6—Ni3 167.5 (2)
C20—C19—N3—C23 −0.3 (4) C36—C37—O6—Ni3 −13.8 (4)
C20—C19—N3—Ni1 179.6 (2) O4—Ni3—O6—C37 −31 (6)
C22—C23—N3—C19 −1.8 (4) N5—Ni3—O6—C37 6.7 (3)
C22—C23—N3—Ni1 178.2 (2) N6—Ni3—O6—C37 −173.6 (3)

[TableWrap ID: d1e7971]
D—H···A D—H H···A D···A D—H···A
O8—H8A···O7i 0.85 1.97 2.821 (5) 179
O8—H8B···O6ii 0.85 2.10 2.952 (4) 179
C2—H2A···O5 0.99 2.46 3.356 (4) 151
C3—H3B···O5 0.99 2.55 3.425 (3) 147
C24—H24A···N7 0.99 2.52 3.382 (4) 145
C31—H31B···O2 0.99 2.30 3.259 (4) 163


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