Dichlorido(4,7-diphenyl-1,10-phenanthroline-κ2 N,N′)gold(III) tetra­chloridoaurate(III)

Roya Ahmadi; Vahid Amani; Hamid Reza Khavasi

doi:10.1107/S1600536808025476

. 2008 Aug 13;64(Pt 9):m1156–m1157. doi: 10.1107/S1600536808025476

Dichlorido(4,7-diphenyl-1,10-phenanthroline-κ² N,N′)gold(III) tetrachloridoaurate(III)

Roya Ahmadi ^a, Vahid Amani ^a,^*, Hamid Reza Khavasi ^b

PMCID: PMC2960497 PMID: 21201607

Abstract

In the cation of the title compound, [AuCl₂(C₂₄H₁₆N₂)][AuCl₄], the Au^III atom is four-coordinated in a distorted square-planar configuration by two N atoms from a 4,7-diphenyl-1,10-phenanthroline ligand and two terminal Cl atoms. In the anion, the Au^III atom has a square-planar coordination. In the crystal structure, intra- and intermolecular C—H⋯Cl hydrogen bonds are found.

Related literature

For related literature, see: Hojjat Kashani et al. (2008 ▶); Mclnnes et al. (1995 ▶); Bjernemose et al. (2004 ▶); Hayoun et al. (2006 ▶); Abbate et al. (2000 ▶); Adams & Strahle (1982 ▶).

Experimental

Crystal data

[AuCl₂(C₂₄H₁₆N₂)][AuCl₄]
M _r = 939.03
Monoclinic,
a = 26.2625 (16) Å
b = 13.7608 (6) Å
c = 14.4292 (9) Å
β = 101.207 (5)°
V = 5115.2 (5) Å³
Z = 8
Mo Kα radiation
μ = 12.10 mm⁻¹
T = 120 (2) K
0.43 × 0.35 × 0.30 mm

Data collection

Bruker SMART CCD area-detector diffractometer
Absorption correction: numerical (X-SHAPE and X-RED; Stoe & Cie, 2005 ▶) T _min = 0.580, T _max = 0.640
18667 measured reflections
6864 independent reflections
6404 reflections with I > 2σ(I)
R _int = 0.090

Refinement

R[F ² > 2σ(F ²)] = 0.068
wR(F ²) = 0.173
S = 1.16
6864 reflections
308 parameters
H-atom parameters constrained
Δρ_max = 1.07 e Å⁻³
Δρ_min = −1.02 e Å⁻³

Data collection: SMART (Bruker, 1998 ▶); cell refinement: SMART; data reduction: SAINT (Bruker, 1998 ▶); program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXTL; molecular graphics: ORTEP-3 for Windows (Farrugia, 1997 ▶); software used to prepare material for publication: WinGX (Farrugia, 1999 ▶).

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808025476/hk2509sup1.cif

e-64-m1156-sup1.cif^{(22.9KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808025476/hk2509Isup2.hkl

e-64-m1156-Isup2.hkl^{(329.2KB, hkl)}

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

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

Au1—N2	2.032 (6)
Au1—N1	2.039 (7)
Au1—Cl2	2.2546 (19)
Au1—Cl1	2.257 (2)
Au2—Cl4	2.281 (2)
Au2—Cl5	2.281 (2)
Au2—Cl6	2.284 (2)
Au2—Cl3	2.285 (2)

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N2—Au1—N1	81.1 (3)
N2—Au1—Cl2	175.42 (19)
N1—Au1—Cl2	94.3 (2)
N2—Au1—Cl1	94.92 (19)
N1—Au1—Cl1	175.95 (19)
Cl2—Au1—Cl1	89.62 (8)
Cl4—Au2—Cl5	90.26 (10)
Cl4—Au2—Cl6	178.77 (8)
Cl5—Au2—Cl6	89.67 (9)
Cl4—Au2—Cl3	89.96 (10)
Cl5—Au2—Cl3	178.75 (7)
Cl6—Au2—Cl3	90.14 (9)

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

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C1—H1⋯Cl2	0.93	2.68	3.244 (9)	120
C1—H1⋯Cl6ⁱ	0.93	2.79	3.668 (8)	159
C18—H18⋯Cl2ⁱⁱ	0.93	2.79	3.653 (8)	155
C22—H22⋯Cl1	0.93	2.66	3.239 (8)	121
C22—H22⋯Cl4ⁱⁱⁱ	0.93	2.76	3.555 (9)	143

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

Acknowledgments

We are grateful to the Islamic Azad University, Shahr-e-Rey Branch, for financial support.

supplementary crystallographic information

Comment

Recently, we reported the synthesis and crystal structure of [H₂DA18C6]- [AuCl₄].2H₂O, (II) (Hojjat Kashani et al., 2008) [where H₂DA18C6 is 1,10-Diazonia-18-crown-6]. There are several Au^III complexes, with formula, [AuCl₂(N—N)], such as [AuCl₂(bipy)][BF₄], (III) (Mclnnes et al., 1995), [AuCl₂(bipy)](NO₃), (IV) (Bjernemose et al., 2004), [AuCl₂(bipy)]- [AuBr₄], (V) (Hayoun et al., 2006) and [AuCl₂(phen)]Cl.H₂O, (VI) (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. There are also two Au^III complexes, with formula, [AuCl₂L₂], such as [AuCl₂(py)₂][AuCl₄], (VII) and [AuCl₂(py)₂]Cl.H₂O, (VIII) (Adams & Strahle, 1982) [where py is pyridine] have been synthesized and characterized by single-crystal X-ray diffraction methods. We report herein the synthesis and crystal structure of the title compound, (I).

The asymmetric unit of (I), (Fig. 1) contains one cation and one anion. In the cation, the Au^III atom is four-coordinated in a distorted square-planar configuration by two N atoms from 4,7-diphenyl-1,10-phenanthroline ligand and two terminal Cl atoms. In the anion, the Au ion has a square-planar coordination. In the cation, the Au-Cl and Au-N bond lengths and angles (Table 1) are in good agreement with the corresponding values in (III) and (IV). In the anion, the Au-Cl bond lengths and angles (Table 1) are within normal ranges.

In the crystal structure, intra- and intermolecular C-H···Cl hydrogen bonds (Table 2) link the molecules, in which they may be effective in the stabilization of the structure.

Experimental

For the preparation of the title compound, a solution of 4,7-diphenyl-1,10- phenanthroline (0.21 g, 0.63 mmol) in EtOH (30 ml) was added to a solution of HAuCl₄.3H₂O, (0.25 g, 0.63 mmol) in acetonitrile (40 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 prismatic crystals were isolated (yield; 0.45 g, 75.8%, m.p. < 573 K).