Dichlorido(4,4′-di-tert-butyl-2,2′-bi­pyridine-κ2 N,N′)gold(III) tetrachlorido­aurate(III) acetonitrile solvate

Sema Öztürk Yıldırım; Mehmet Akkurt; Nasser Safari; Vahid Amani; Vickie McKee; Anita Abedi; Hamid Reza Khavasi

doi:10.1107/S1600536808025646

. 2008 Aug 20;64(Pt 9):m1189–m1190. doi: 10.1107/S1600536808025646

Dichlorido(4,4′-di-tert-butyl-2,2′-bipyridine-κ² N,N′)gold(III) tetrachloridoaurate(III) acetonitrile solvate

Sema Öztürk Yıldırım ^a, Mehmet Akkurt ^a,^*, Nasser Safari ^b, Vahid Amani ^b, Vickie McKee ^c, Anita Abedi ^d, Hamid Reza Khavasi ^b

PMCID: PMC2960475 PMID: 21201629

Abstract

In the title compound, [AuCl₂(C₉H₁₂N)₂][AuCl₄]·C₂H₃N, there is a mirror plane passing through Au and the central C—C bond of the bipyridyl ligand in the cation, and through Au and two Cl atoms of the anion. A cis-AuCl₂N₂ square-planar geometry for the cation and a square-planar AuCl₄ geometry for the anion result. The two C atoms and the N atom of the acetonitrile molecule all have m site symmetries. In the crystal structure, weak C—H⋯Cl interactions may help to establish the packing.

Related literature

For related structures, see: Abbate et al. (2000 ▶); Adams & Strähle (1982 ▶); Bjernemose et al. (2004 ▶); Hayoun et al. (2006 ▶); McInnes et al. (1995 ▶).

Experimental

Crystal data

[AuCl₂(C₉H₁₂N)₂][AuCl₄]·C₂H₃N
M _r = 916.09
Monoclinic,
a = 6.7880 (9) Å
b = 14.2270 (19) Å
c = 14.1330 (19) Å
β = 97.151 (2)°
V = 1354.3 (3) Å³
Z = 2
Mo Kα radiation
μ = 11.43 mm⁻¹
T = 150 (2) K
0.14 × 0.10 × 0.01 mm

Data collection

Bruker APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 2003 ▶) T _min = 0.298, T _max = 0.894
14949 measured reflections
3888 independent reflections
2860 reflections with I > 2σ(I)
R _int = 0.060

Refinement

R[F ² > 2σ(F ²)] = 0.036
wR(F ²) = 0.079
S = 1.01
3888 reflections
155 parameters
H-atom parameters constrained
Δρ_max = 1.59 e Å⁻³
Δρ_min = −1.24 e Å⁻³

Data collection: APEX2 (Bruker, 2005 ▶); cell refinement: APEX2; data reduction: SAINT (Bruker, 2005 ▶); program(s) used to solve structure: SIR92 (Altomare et al., 1993 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 (Farrugia, 1997 ▶); software used to prepare material for publication: WinGX (Farrugia, 1999 ▶).

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808025646/hb2776sup1.cif

e-64-m1189-sup1.cif^{(19.2KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808025646/hb2776Isup2.hkl

e-64-m1189-Isup2.hkl^{(186.7KB, hkl)}

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

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

Au1—Cl1	2.2590 (17)
Au1—N1	2.020 (4)
Au2—Cl2	2.271 (2)
Au2—Cl3	2.2675 (16)
Au2—Cl4	2.311 (2)

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N2—C11—C10

179.5 (14)

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

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C3—H3⋯Cl3ⁱ	0.93	2.66	3.561 (6)	162
C3—H3⋯Cl1ⁱⁱ	0.93	2.64	3.231 (6)	122

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

Acknowledgments

We are grateful to Shahid Beheshti University and Islamic Azad University, North Tehran Branch, for financial support.

supplementary crystallographic information

Comment

Several Au^III complexes, with formula, [AuCl₂(N—N)], such as [AuCl₂(bipy)][BF₄], (II), (McInnes et al., 1995), [AuCl₂(bipy)](NO₃), (III), (Bjernemose et al., 2004), [AuCl₂(bipy)][AuBr₄], (IV), (Hayoun et al., 2006) and [AuCl₂(phen)]Cl.H₂O, (V), (Abbate et al., 2000) [where bipy is 2,2'-bipyridine and phen is 1,10-phenanthroline] have been synthesized and characterized by single-crystal X-ray diffraction methods.

Other Au^III complexes, with formula, [AuCl₂L₂], such as [AuCl₂(py)₂][AuCl₄], (VI) and [AuCl₂(py)₂]Cl.H₂O, (VII), (Adams & Strähle 1982) [where py is pyridine] have also bee prepared and characterized. We report herein the synthesis and crystal structure of the title compound, (I).

The asymmetric unit of (I) (Fig. 1) contains one half-cation, one half-anion and one half-acetonitrile molecule; the whole assemblage is symmetric according to a mirror plane. Both Au ions have square-planar coordination (Table 1) and the individual bond lengths and angles are in good agreement with the corresponding values in (II), (III), (IV), (V), (VI) and (VII).

In the crystal of (I), weak intermolecular C—H···Cl hydrogen bonds (Table 2) link the molecules to form a supramolecular structure (Fig. 2 and Fig. 3).

Experimental

A solution of 4,4'-di-tert-butyl-2,2'-bipyridine (0.15 g, 0.56 mmol) in acetonitrile (40 ml) was added to a solution of HAuCl₄.3H₂O, (0.22 g, 0.56 mmol) in EtOH (50 ml) and the resulting yellow solution was stirred for 10 min at 313 K. Then, it was left to evaporate slowly at room temperature. After one week, yellow laths and prisms of (I) were isolated (yield 0.38 g; 74.0%).