fac-Bis(acetonitrile-κN)tricarbonyl­(trifluoro­acetato-κO)rhenium(I)

Reza Kia; Hoong-Kun Fun

doi:10.1107/S1600536808029966

. 2008 Sep 24;64(Pt 10):m1314. doi: 10.1107/S1600536808029966

fac-Bis(acetonitrile-κN)tricarbonyl(trifluoroacetato-κO)rhenium(I)

Reza Kia ^a, Hoong-Kun Fun ^a,^*

PMCID: PMC2959409 PMID: 21201050

Abstract

In the title compound, [Re(CF₃COO)(CH₃CN)₂(CO)₃], the Re atom has a distorted octahedral configuration. The two acetonitrile molecules and two of the three carbonyl groups occupy the equatorial plane of the complex, with the third carbonyl ligand and the trifluoroacetato ligand in the axial positions. The three carbonyl ligands are arranged in a fac configuration around the Re atom. The CF₃ segment of the trifluoroacetato ligand shows rotational disorder and the refined site-occupancy factors of the disordered parts are ca 0.5/0.5. The crystal structure is stabilized by C—H⋯O and C—H⋯F hydrogen bonds.

Related literature

For values of standard bond lengths, see: Allen et al. (1987 ▶). For related structures, see, for example: Chan et al. (1977 ▶); Lazarova et al. (2004 ▶). For background on the applications, see, for example: Davies & Hartely (1981 ▶); Collin & Sauvage (1989 ▶); Balzani et al. (1996 ▶); Meyer (1989 ▶).

Experimental

Crystal data

[Re(C₂F₃O₂)(C₂H₃N)₂(CO)₃]
M _r = 465.36
Monoclinic,
a = 10.8243 (2) Å
b = 10.4745 (2) Å
c = 14.4772 (3) Å
β = 125.584 (1)°
V = 1334.90 (4) Å³
Z = 4
Mo Kα radiation
μ = 9.16 mm⁻¹
T = 100.1 (1) K
0.32 × 0.23 × 0.19 mm

Data collection

Bruker SMART APEXII CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2005 ▶) T _min = 0.098, T _max = 0.175
24096 measured reflections
5819 independent reflections
5087 reflections with I > 2σ(I)
R _int = 0.037

Refinement

R[F ² > 2σ(F ²)] = 0.031
wR(F ²) = 0.078
S = 1.06
5819 reflections
211 parameters
H-atom parameters constrained
Δρ_max = 2.80 e Å⁻³
Δρ_min = −1.27 e Å⁻³

Data collection: APEX2 (Bruker, 2005 ▶); cell refinement: APEX2; data reduction: SAINT (Bruker, 2005 ▶); 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 and PLATON (Spek, 2003 ▶).

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808029966/at2632sup1.cif

e-64-m1314-sup1.cif^{(17.3KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808029966/at2632Isup2.hkl

e-64-m1314-Isup2.hkl^{(284.9KB, hkl)}

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

Table 1. Hydrogen-bond geometry (Å, °).

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C4—H4B⋯O5ⁱ	0.98	2.42	3.113 (5)	127
C6—H6A⋯F1Aⁱⁱ	0.98	2.35	3.237 (8)	150
C6—H6B⋯O5ⁱⁱⁱ	0.98	2.46	3.075 (5)	121

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

Acknowledgments

H-KF and RK thank the Malaysian Government and Universiti Sains Malaysia for the Science Fund grant No. 305/PFIZIK/613312. RK thanks Universiti Sains Malaysia for a postdoctoral research fellowship.

supplementary crystallographic information

Comment

The synthesis of solvent-coordinated complexes is a matter of considerable interest since they are useful sources for synthesis of new species resulting from the substitution of the coordinated solvent by a more basic ligand (Davies & Hartely, 1981). The lability of the solvent ligand easily gives rise to a highly reactive 16e^- electrophilic fragment able to activate small molecules thus providing an important step in many chemical processes. On the other hand, Rhenium tricarbonyl complexes have been the subject of much attention, mainly because of their photophysical (Meyer 1989) and photochemical properties (Collin & Sauvage 1989) and in supramolecular chemistry (Balzani et al., 1996).

In the title compound (I) (Fig. 1), the Re atom adopts a distorted octahedral geometry. The bond lengths (Allen et al., 1987) and angles are within the normal ranges and are comparable to the related structures (Chan et al., 1977; Lazarova et al., 2004). The two acetonitriles and two carbonyl groups occupy the equatorial plane of the complex, with the third carbonyl ligands and the trifluoroacetate in the axial positions. The three carbonyl ligands at Re atom are arranged in a fac configuration. The cis-equatorial angle of N1–Re1–N2 is 81.88 (13) °. The deviation of the Re atom from the C1/C2/N1/N2 plane is -0.048 (1) Å.

The crystal structure is stabilized by C—H···O and C—H···F hydrogen bonds (Table 1, Fig. 2).

Experimental

The synthetic method has been described earlier (Chan et al., 1977). Single crystals suitable for X-ray diffraction were obtained by evaporation of an acetonitrile solution at room temperature.