Tris(pyridin-2-yl­methanol)nickel(II) hexa­fluoridophosphate trifluoro­acetate

Tomohiko Hamaguchi; Tomoko Nagata; Satoshi Kawata; Isao Ando

doi:10.1107/S160053681104431X

. 2011 Oct 29;67(Pt 11):m1632. doi: 10.1107/S160053681104431X

Tris(pyridin-2-ylmethanol)nickel(II) hexafluoridophosphate trifluoroacetate

Tomohiko Hamaguchi ^a,^*, Tomoko Nagata ^a, Satoshi Kawata ^a, Isao Ando ^a

PMCID: PMC3247549 PMID: 22219854

Abstract

In the crystal structure of the title complex, [Ni(C₆H₇NO)₃](PF₆)(C₂F₃O₂), the Ni^II ion is in a slightly distorted octahedral NiO₃N₃ coordination geometry with each of the three N and three O atoms in a meridional coordination. In the crystal, the complex molecules and the trifluoroacetate anions are connected via O—H⋯O hydrogen bonding into layers parallel to the ab plane.

Related literature

For related complexes, see: Ito & Onaka (2004 ▶); Kermagoret & Braunstein (2008 ▶).

Experimental

Crystal data

[Ni(C₆H₇NO)₃](PF₆)(C₂F₃O₂)
M _r = 644.08
Triclinic,
a = 9.6381 (2) Å
b = 11.9668 (4) Å
c = 11.9892 (3) Å
α = 109.950 (1)°
β = 95.348 (1)°
γ = 101.411 (1)°
V = 1254.60 (6) Å³
Z = 2
Mo Kα radiation
μ = 0.94 mm⁻¹
T = 200 K
0.40 × 0.30 × 0.20 mm

Data collection

Rigaku R-AXIS RAPID diffractometer
Absorption correction: multi-scan (ABSCOR; Rigaku, 1995 ▶) T _min = 0.813, T _max = 1.000
12517 measured reflections
5736 independent reflections
5234 reflections with I > 2σ(I)
R _int = 0.018

Refinement

R[F ² > 2σ(F ²)] = 0.033
wR(F ²) = 0.088
S = 1.05
5736 reflections
376 parameters
9 restraints
H-atom parameters constrained
Δρ_max = 0.50 e Å⁻³
Δρ_min = −0.45 e Å⁻³

Data collection: RAPID-AUTO (Rigaku, 2002 ▶); cell refinement: RAPID-AUTO; data reduction: RAPID-AUTO; program(s) used to solve structure: SIR2004 (Burla et al., 2005 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: Yadokari-XG (Wakita, 2001 ▶; Kabuto et al., 2009 ▶), ORTEP-3 for Windows (Farrugia, 1997 ▶) and Mercury (Macrae et al., 2008 ▶); software used to prepare material for publication: Yadokari-XG and publCIF (Westrip, 2010 ▶).

Supplementary Material

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S160053681104431X/nc2249sup1.cif

e-67-m1632-sup1.cif^{(31.8KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S160053681104431X/nc2249Isup2.hkl

e-67-m1632-Isup2.hkl^{(280.8KB, hkl)}

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

Table 1. Selected geometric parameters (Å, °).

Ni1—O1	2.0461 (12)
Ni1—N2	2.0601 (14)
Ni1—O2	2.0647 (12)
Ni1—N1	2.0662 (14)
Ni1—O3	2.0714 (12)
Ni1—N3	2.0769 (14)

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O1—Ni1—N1	78.11 (5)
N2—Ni1—O2	78.53 (5)
O3—Ni1—N3	78.09 (5)

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Table 2. Hydrogen-bond geometry (Å, °).

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1⋯O4ⁱ	0.87	1.76	2.6003 (19)	162.5
O2—H2⋯O5ⁱⁱ	0.92	1.77	2.6965 (18)	175.8
O3—H3⋯O5ⁱⁱⁱ	0.98	1.65	2.6267 (18)	173.8

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Symmetry codes: (i) Inline graphic ; (ii) ; (iii) .

Acknowledgments

This work was supported in part by funds (No. 115001) from the Central Research Institute of Fukuoka University.

supplementary crystallographic information

Comment

The crystal structure of the title compound is composed of [Ni^II(C₆H₇ON)₃]²⁺ cations, hexafluorophosphate and trifluoroacetate anions. The Ni^II ion is in a slightly distorted octahedral coordination, comprising three N atoms and three O atoms from three pyridine-2-methanol ligands (Fig. 1 and Table 1). The three N and three O atoms make a meridional NiO₃N₃ coordination and the mean bite angle of the pyridine-2-methanol ligand amount to 78.2 (2) °.

In the crystal structure the complexes are connected via O—H···O hydrogen bonding between the hydroxy H atoms of the pyridine-2-methanol ligand and the O atoms of the trifluoroacetate anion into layers that are parallel to the a/b plane. (Fig. 2 and 3 and Table 2).

Experimental

A solution of NiSO₄.6H₂O (0.5 mmol) in H₂O (1 ml) was added to the solution of pyridine-2-methanol (1.5 mmol) in H₂O (3 ml). Afterwards NH₄PF₆ (6.0 mmol) and CF₃COONa (2.5 mmol) were added to the resulting blue solution. The resulting pale blue precipitate was collected. The crude product was purified by recrystallization from acetone and water. The blue prism-like crystals were obtained a few days later on slow evaporation of the solvent.