μ-Bis(diphenyl­arsino)methane-κ2As:As′-bis­[chloridogold(I)]

Monkowius, U.; Zabel, M.; Yersin, H.

doi:10.1107/S1600536809004802

metal-organic compounds

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ISSN: 2056-9890

Volume 65| Part 3| March 2009| Page m281

doi:10.1107/S1600536809004802

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μ-Bis(diphenylarsino)methane-κ²As:As′-bis[chloridogold(I)]

Uwe Monkowius,^a ^* Manfred Zabel ^b and Hartmut Yersin ^c

^aInstitut für Anorganische Chemie, Johannes Kepler Universität Linz, Altenbergerstrasse 69, 4040 Linz, Austria, ^bRöntgenstrukturanalyse, Zentrale Analytik, Universität Regensburg, Universitätsstrasse 31, 93053 Regensburg, Germany, and ^cInstitut für Physikalische Chemie, Universität Regensburg, Universitätsstrasse 31, 93053 Regensburg, Germany
^*Correspondence e-mail: uwe.monkowius@jku.at

(Received 30 January 2009; accepted 10 February 2009; online 18 February 2009)

The title structure, [Au₂Cl₂(C₂₅H₂₂As₂)], consists of discrete molecules disposed about a crystallographic twofold axis. The Au atom exhibits a nearly linear coordination by As and Cl atoms. Au⋯Au interactions [3.4285Å(4) Å] and a weak intermolecular C—H⋯Cl hydrogen bond are present.

Related literature

For related structures, see: Healy (2003 ); Schmidbaur et al. (1977a ,b ). For the synthesis of related complexes, see: Monkowius et al. (2003a ,b ).

Experimental

Crystal data

[Au₂Cl₂(C₂₅H₂₂As₂)]
M_r = 937.11
Monoclinic, C 2/c
a = 22.7171 (18) Å
b = 7.3151 (6) Å
c = 18.2047 (15) Å
β = 120.342 (8)°
V = 2610.8 (4) Å³
Z = 4
Mo Kα radiation
μ = 13.96 mm⁻¹
T = 173 K
0.24 × 0.20 × 0.18 mm

Data collection

Stoe IPDS diffractometer
Absorption correction: analytical [from crystal shape; X-SHAPE and X-RED in IPDS Software (Stoe & Cie, 1998 )] T_min = 0.051, T_max = 0.083
12353 measured reflections
2790 independent reflections
2431 reflections with I > 2σ(I)
R_int = 0.062

Refinement

R[F² > 2σ(F²)] = 0.023
wR(F²) = 0.055
S = 0.96
2790 reflections
142 parameters
H-atom parameters constrained
Δρ_max = 1.65 e Å⁻³
Δρ_min = −0.70 e Å⁻³

Table 1
Selected geometric parameters (Å, °)

Au1—As1	2.3426 (5)
Au1—Cl1	2.2887 (16)

As1—Au1—Cl1	174.82 (4)
Symmetry code: (i) $[-x, y, -z+{\script{1\over 2}}]$ .

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C1—H1A⋯Cl1ⁱⁱ	0.99	2.70	3.658 (4)	163
Symmetry code: (ii) $[-x, y+1, -z+{\script{1\over 2}}]$ .

Data collection: IPDS Software (Stoe & Cie, 1998); cell refinement: IPDS Software; data reduction: IPDS Software; program(s) used to solve structure: SIR97 (Altomare et al., 1999 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ); molecular graphics: PLATON (Spek, 2009 ); software used to prepare material for publication: PLATON.

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809004802/nc2133sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536809004802/nc2133Isup2.hkl

checkCIF report

Comment top

The title compound was prepared from dpam [dpam = bis(diphenylarsino)methane] and (tht)AuCl (tht = tetrahydrothiophene) in methylene chloride in nearly quantitative yields. It is isomorphous to the crystal structure of the phosphorus congener [dppm(AuCl)₂], which was determined by Schmidbaur et al. (1977b) [a = 22.31 (1) Å, b = 7.215 (7) Å, c = 18.12 (1) Å and β = 120.43 (8)°]. The structure consists of discrete molecules of [dpam(AuCl)₂] disposed about a crystallographic twofold axis, which passes through the C1 atom. The Au atom is in a standard linear coordination [As—Au—Cl 174.82 (4)°] with As—Au and Au—Cl bond lengths of 2.3426 (5) and 2.289 (2) Å, respectively. The Au—As···As—Au torsion angle is 66.78 (2)°, yielding a staggered conformation of both Ph₂AsAuCl moieties and an intramolecular Au···Au distance of 3.4285 (4) Å, indicative of attractive aurophilic interactions. The shortest intermolecular Au···Au distance is 5.863 Å. In its crystal, the complexes are linked to infinite chains via weak C—H···Cl intermolecular hydrogen bonds with C···Cl distance of 3.658 (4) Å and a C1—H1a···Cl1ⁱⁱ angle of 163° (symmetry code: (ii) -x, y + 1, -z + 1/2).

For comparison, the geometrical data of the phosphorus compound are: Au—P 2.238 (5), Au—Cl 2.288 (7), Au···Au 3.351 (2) Å, P—Au—Cl 175 (2), Au—P···P—Au 67 (1)°. It should be noted, that a second polymorph of the phosphorus complex exists: Unlike the herein presented structure, there are no aurophilic bonds between the gold(I) atoms (Healy, 2003).

All attempts to prepare the 1:1 complex [(dpamAuCl)₂] starting from the title compound analogous to the published synthesis of phosphorus complex [(dppmAuCl)₂] (Schmidbaur et al., 1977a) failed.

Related literature top

For related structures, see: Healy (2003); Schmidbaur et al. (1977a,b). For the synthesis of related complexes, see: Monkowius et al. (2003a,b).

Experimental top

The title compound was prepared analogously to a previously published procedure (Monkowius et al., 2003a,b): dpam (0.22 g, 0.47 mmol) and (tht)AuCl (0.30 g, 0.94 mmol, tht = tetrahydrothiophene) were stirred in methylene chloride (20 ml) at room temperature for 2 h. The product was precipitated with n-pentane and isolated by filtration. Recrystallization from methylene chloride/diethyl ether yields colourless crystals suitable for X-ray crystallography. Yield: 0.40 g (0.43 mmol, 91%); ¹H NMR (300 MHz, CDCl₃): 7.55–7.60 (m, Ph—H, 8 H), 7.37–7.51 (m, Ph—H, 12 H), 3.48 p.p.m. (s, CH₂, 2 H); ¹³C NMR (75.5 MHz, CDCl₃): 134.63, 132.93, 130.44, 129.23, 25.08 p.p.m.; MS (ESI): m/z (%) = 1605.3 [L₂Au₃Cl₂]⁺ (5), 1373.3 [L₂Au₃Cl]⁺ (47), 1141.3 [L₂Au]⁺ (76), 901.1 [M—Cl]⁺ (25), 669.2 [LAu]⁺ (100); EA (C₂₅H₂₂As₂Au₂Cl₂) calc.: C 32.04, H 2.37, found: C 32.01, H 2.37.

Computing details top

Data collection: IPDS Software (Stoe & Cie, 1998); cell refinement: IPDS Software (Stoe & Cie, 1998); data reduction: IPDS Software (Stoe & Cie, 1998); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: PLATON (Spek, 2009); software used to prepare material for publication: PLATON (Spek, 2009).

Figures top

	Fig. 1. View of the title compound with the atom numbering scheme (symmetry code: (i) -x, y, -z + 1/2). Displacement ellipsoids for non-H atoms are drawn at the 50% probability level.
	Fig. 2. Crystal structure of the title compound depicting the intermolecular hydrogen bonds between H1A and Cl1ⁱⁱ (symmetry code: (ii) -x, y + 1, -z + 1/2). The H atoms not involved in hydrogen bonding have been omitted.

µ-Bis(diphenylarsino)methane-κ²As:As'-bis[chloridogold(I)] top

Crystal data top

[Au₂Cl₂(C₂₅H₂₂As₂)]	F(000) = 1720
M_r = 937.11	Cell parameters were determined by indexing 8000 reflections with I/sigma limit 6.0.
Monoclinic, C2/c	D_x = 2.384 Mg m⁻³
Hall symbol: -C 2yc	Mo Kα radiation, λ = 0.71073 Å
a = 22.7171 (18) Å	Cell parameters from 8000 reflections
b = 7.3151 (6) Å	θ = 2.1–26.9°
c = 18.2047 (15) Å	µ = 13.96 mm⁻¹
β = 120.342 (8)°	T = 173 K
V = 2610.8 (4) Å³	Prism, colourless
Z = 4	0.24 × 0.20 × 0.18 mm

Data collection top

Stoe IPDS diffractometer	2790 independent reflections
Radiation source: fine-focus sealed tube	2431 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.062
rotation scans	θ_max = 26.9°, θ_min = 2.1°
Absorption correction: analytical [from crystal shape; X-SHAPE and X-RED in IPDS Software (Stoe & Cie, 1998)]	h = −28→28
T_min = 0.051, T_max = 0.083	k = −9→9
12353 measured reflections	l = −22→22

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.023	H-atom parameters constrained
wR(F²) = 0.055	w = 1/[σ²(F_o²) + (0.0315P)²] where P = (F_o² + 2F_c²)/3
S = 0.96	(Δ/σ)_max = 0.001
2790 reflections	Δρ_max = 1.65 e Å⁻³
142 parameters	Δρ_min = −0.70 e Å⁻³
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001Fc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.00085 (4)

Crystal data top

[Au₂Cl₂(C₂₅H₂₂As₂)]	V = 2610.8 (4) Å³
M_r = 937.11	Z = 4
Monoclinic, C2/c	Mo Kα radiation
a = 22.7171 (18) Å	µ = 13.96 mm⁻¹
b = 7.3151 (6) Å	T = 173 K
c = 18.2047 (15) Å	0.24 × 0.20 × 0.18 mm
β = 120.342 (8)°

Data collection top

Stoe IPDS diffractometer	2790 independent reflections
Absorption correction: analytical [from crystal shape; X-SHAPE and X-RED in IPDS Software (Stoe & Cie, 1998)]	2431 reflections with I > 2σ(I)
T_min = 0.051, T_max = 0.083	R_int = 0.062
12353 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.023	0 restraints
wR(F²) = 0.055	H-atom parameters constrained
S = 0.96	Δρ_max = 1.65 e Å⁻³
2790 reflections	Δρ_min = −0.70 e Å⁻³
142 parameters

Special details top

Experimental. Data were collected applying an imaging plate system (Stoe) with the following measurement parameters:

Detector distance [mm] 65 Phi movement mode Oscillation Phi incr. [degrees] 1.2 Number of exposures 200 Irradiation / exposure [min] 2.00

For a detailed description of the method see: Sheldrick, G. M., Paulus, E., Vertesy, L. & Hahn, F. (1995). Acta Cryst. B51, 89–98.

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Au1	0.00458 (1)	0.59917 (2)	0.15885 (1)	0.0364 (1)
As1	−0.05684 (2)	0.86199 (5)	0.15224 (2)	0.0286 (1)
Cl1	0.07339 (7)	0.35726 (17)	0.17281 (11)	0.0617 (5)
C1	0.00000	1.0152 (8)	0.25000	0.0335 (16)
C2	−0.08392 (19)	1.0208 (6)	0.0560 (3)	0.0345 (11)
C3	−0.0783 (2)	0.9600 (7)	−0.0115 (3)	0.0430 (14)
C4	−0.0981 (2)	1.0716 (9)	−0.0818 (3)	0.0553 (18)
C5	−0.1228 (2)	1.2445 (8)	−0.0834 (3)	0.0583 (17)
C6	−0.1289 (3)	1.3050 (8)	−0.0165 (4)	0.074 (2)
C7	−0.1091 (3)	1.1941 (7)	0.0543 (3)	0.0640 (19)
C8	−0.13949 (18)	0.8231 (6)	0.1565 (2)	0.0330 (10)
C9	−0.1733 (3)	0.6586 (8)	0.1285 (4)	0.0591 (19)
C10	−0.2351 (3)	0.6299 (9)	0.1269 (5)	0.078 (2)
C11	−0.2608 (2)	0.7632 (10)	0.1543 (4)	0.0641 (18)
C12	−0.2273 (3)	0.9248 (9)	0.1831 (4)	0.064 (2)
C13	−0.1665 (2)	0.9580 (8)	0.1839 (3)	0.0515 (16)
H1A	−0.02910	1.09450	0.26260	0.0400*
H3A	−0.06070	0.84140	−0.01000	0.0520*
H4A	−0.09480	1.02880	−0.12880	0.0660*
H5A	−0.13560	1.32180	−0.13100	0.0700*
H6A	−0.14670	1.42340	−0.01840	0.0890*
H7A	−0.11280	1.23700	0.10110	0.0770*
H9A	−0.15470	0.56450	0.11040	0.0720*
H10A	−0.25880	0.51740	0.10660	0.0930*
H11A	−0.30250	0.74360	0.15340	0.0760*
H12A	−0.24560	1.01640	0.20300	0.0770*
H13A	−0.14390	1.07230	0.20310	0.0620*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Au1	0.0406 (1)	0.0289 (1)	0.0443 (1)	0.0048 (1)	0.0248 (1)	0.0023 (1)
As1	0.0285 (2)	0.0273 (2)	0.0273 (2)	0.0012 (1)	0.0121 (1)	−0.0007 (2)
Cl1	0.0723 (8)	0.0355 (6)	0.1015 (11)	0.0191 (6)	0.0618 (8)	0.0183 (7)
C1	0.026 (2)	0.032 (3)	0.034 (3)	0.0000	0.009 (2)	0.0000
C2	0.0340 (18)	0.032 (2)	0.0292 (19)	−0.0015 (16)	0.0098 (15)	0.0020 (16)
C3	0.0330 (19)	0.057 (3)	0.037 (2)	0.0046 (19)	0.0163 (17)	0.004 (2)
C4	0.041 (2)	0.087 (4)	0.041 (3)	0.004 (2)	0.023 (2)	0.014 (3)
C5	0.054 (3)	0.065 (3)	0.044 (3)	−0.007 (3)	0.016 (2)	0.017 (3)
C6	0.107 (5)	0.036 (3)	0.058 (3)	0.010 (3)	0.026 (3)	0.011 (3)
C7	0.106 (4)	0.038 (3)	0.038 (3)	0.010 (3)	0.029 (3)	0.001 (2)
C8	0.0248 (16)	0.041 (2)	0.0267 (18)	−0.0002 (16)	0.0082 (14)	−0.0010 (17)
C9	0.051 (3)	0.049 (3)	0.084 (4)	−0.013 (2)	0.039 (3)	−0.021 (3)
C10	0.058 (3)	0.071 (4)	0.108 (5)	−0.028 (3)	0.045 (4)	−0.019 (4)
C11	0.035 (2)	0.092 (4)	0.065 (3)	−0.008 (3)	0.025 (2)	0.001 (3)
C12	0.043 (3)	0.087 (4)	0.065 (4)	0.006 (3)	0.029 (2)	−0.015 (3)
C13	0.040 (2)	0.054 (3)	0.057 (3)	−0.006 (2)	0.022 (2)	−0.017 (2)

Geometric parameters (Å, º) top

Au1—As1	2.3426 (5)	C11—C12	1.360 (10)
Au1—Cl1	2.2887 (16)	C12—C13	1.395 (9)
As1—C1	1.941 (3)	C1—H1A	0.9900
As1—C2	1.926 (5)	C1—H1Aⁱ	0.9900
As1—C8	1.939 (5)	C3—H3A	0.9500
C2—C3	1.372 (7)	C4—H4A	0.9500
C2—C7	1.385 (7)	C5—H5A	0.9500
C3—C4	1.388 (7)	C6—H6A	0.9500
C4—C5	1.378 (9)	C7—H7A	0.9500
C5—C6	1.367 (8)	C9—H9A	0.9500
C6—C7	1.391 (8)	C10—H10A	0.9500
C8—C9	1.379 (8)	C11—H11A	0.9500
C8—C13	1.381 (7)	C12—H12A	0.9500
C9—C10	1.405 (11)	C13—H13A	0.9500
C10—C11	1.355 (10)

Au1···C6ⁱⁱ	3.773 (6)	C1···H13Aⁱ	2.9600
Au1···C7ⁱⁱ	3.756 (6)	C1···H13A	2.9600
Au1···C4ⁱⁱⁱ	3.910 (6)	C1···H7A	3.0900
Au1···C5ⁱⁱⁱ	3.759 (5)	C3···H11A^viii	3.0300
Au1···C8ⁱ	3.601 (4)	C4···H11A^viii	3.0200
Au1···C9ⁱ	3.857 (7)	C13···H1A	2.8800
Au1···Au1ⁱ	3.4286 (4)	C13···H4A^ix	2.9500
Au1···H7Aⁱⁱ	3.5200	H1A···C13	2.8800
Au1···H9A	3.2700	H1A···H13A	2.2700
Au1···H3A	3.1900	H1A···Cl1^x	2.7000
Au1···H6Aⁱⁱ	3.5600	H3A···Au1	3.1900
Au1···H4Aⁱⁱⁱ	3.6100	H4A···Au1ⁱⁱⁱ	3.6100
Au1···H5Aⁱⁱⁱ	3.3100	H4A···Cl1^v	3.0400
Cl1···H1A^iv	2.7000	H4A···C13^xi	2.9500
Cl1···H13A^iv	2.8900	H5A···Au1ⁱⁱⁱ	3.3100
Cl1···H4A^v	3.0400	H5A···Cl1ⁱⁱⁱ	3.0300
Cl1···H5Aⁱⁱⁱ	3.0300	H6A···Au1^vii	3.5600
Cl1···H11A^vi	3.1300	H7A···Au1^vii	3.5200
C3···C3ⁱⁱⁱ	3.416 (8)	H7A···C1	3.0900
C3···C4ⁱⁱⁱ	3.481 (7)	H7A···H13A	2.5900
C4···Au1ⁱⁱⁱ	3.910 (6)	H9A···Au1	3.2700
C4···C3ⁱⁱⁱ	3.481 (7)	H11A···Cl1^xii	3.1300
C5···Au1ⁱⁱⁱ	3.759 (5)	H11A···C3^viii	3.0300
C6···Au1^vii	3.773 (6)	H11A···C4^viii	3.0200
C7···Au1^vii	3.756 (6)	H13A···C1	2.9600
C8···Au1ⁱ	3.601 (4)	H13A···H1A	2.2700
C9···Au1ⁱ	3.857 (7)	H13A···H7A	2.5900
C1···H7Aⁱ	3.0900	H13A···Cl1^x	2.8900

As1—Au1—Cl1	174.82 (4)	As1—C1—H1Aⁱ	110.00
Au1—As1—C1	108.88 (12)	As1ⁱ—C1—H1A	110.00
Au1—As1—C2	116.75 (14)	H1A—C1—H1Aⁱ	108.00
Au1—As1—C8	116.18 (13)	As1ⁱ—C1—H1Aⁱ	110.00
C1—As1—C2	104.16 (19)	C2—C3—H3A	120.00
C1—As1—C8	104.90 (11)	C4—C3—H3A	120.00
C2—As1—C8	104.72 (19)	C3—C4—H4A	120.00
As1—C1—As1ⁱ	109.5 (3)	C5—C4—H4A	120.00
As1—C2—C3	119.2 (3)	C4—C5—H5A	120.00
As1—C2—C7	120.7 (4)	C6—C5—H5A	120.00
C3—C2—C7	120.1 (4)	C5—C6—H6A	120.00
C2—C3—C4	120.1 (5)	C7—C6—H6A	120.00
C3—C4—C5	119.9 (5)	C2—C7—H7A	120.00
C4—C5—C6	120.1 (5)	C6—C7—H7A	120.00
C5—C6—C7	120.4 (6)	C8—C9—H9A	120.00
C2—C7—C6	119.4 (5)	C10—C9—H9A	120.00
As1—C8—C9	118.9 (4)	C9—C10—H10A	120.00
As1—C8—C13	121.7 (4)	C11—C10—H10A	120.00
C9—C8—C13	119.4 (5)	C10—C11—H11A	120.00
C8—C9—C10	120.1 (6)	C12—C11—H11A	120.00
C9—C10—C11	119.8 (6)	C11—C12—H12A	119.00
C10—C11—C12	120.4 (6)	C13—C12—H12A	120.00
C11—C12—C13	120.9 (6)	C8—C13—H13A	120.00
C8—C13—C12	119.3 (5)	C12—C13—H13A	120.00
As1—C1—H1A	110.00

Au1—As1—C1—As1ⁱ	−34.87 (4)	C3—C2—C7—C6	0.4 (9)
C2—As1—C1—As1ⁱ	−160.10 (16)	C7—C2—C3—C4	−0.3 (8)
C8—As1—C1—As1ⁱ	90.12 (13)	As1—C2—C7—C6	−179.4 (5)
Au1—As1—C2—C3	12.2 (5)	C2—C3—C4—C5	0.7 (8)
C1—As1—C2—C3	132.3 (4)	C3—C4—C5—C6	−1.1 (8)
C8—As1—C2—C3	−117.9 (4)	C4—C5—C6—C7	1.2 (10)
Au1—As1—C2—C7	−168.1 (4)	C5—C6—C7—C2	−0.8 (10)
C1—As1—C2—C7	−48.1 (5)	As1—C8—C9—C10	−176.9 (5)
C8—As1—C2—C7	61.9 (5)	C13—C8—C9—C10	0.8 (8)
C2—As1—C8—C9	104.0 (4)	As1—C8—C13—C12	177.9 (4)
Au1—As1—C8—C9	−26.4 (4)	C9—C8—C13—C12	0.3 (7)
C1—As1—C8—C9	−146.6 (4)	C8—C9—C10—C11	−1.1 (10)
C2—As1—C8—C13	−73.6 (4)	C9—C10—C11—C12	0.2 (11)
Au1—As1—C8—C13	156.0 (3)	C10—C11—C12—C13	1.0 (10)
C1—As1—C8—C13	35.7 (4)	C11—C12—C13—C8	−1.2 (8)
As1—C2—C3—C4	179.4 (4)

Symmetry codes: (i) −x, y, −z+1/2; (ii) x, y−1, z; (iii) −x, −y+2, −z; (iv) −x, y−1, −z+1/2; (v) −x, −y+1, −z; (vi) x+1/2, y−1/2, z; (vii) x, y+1, z; (viii) −x−1/2, −y+3/2, −z; (ix) x, −y+2, z+1/2; (x) −x, y+1, −z+1/2; (xi) x, −y+2, z−1/2; (xii) x−1/2, y+1/2, z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C1—H1A···Cl1^x	0.99	2.70	3.658 (4)	163

Symmetry code: (x) −x, y+1, −z+1/2.

Experimental details

Crystal data
Chemical formula	[Au₂Cl₂(C₂₅H₂₂As₂)]
M_r	937.11
Crystal system, space group	Monoclinic, C2/c
Temperature (K)	173
a, b, c (Å)	22.7171 (18), 7.3151 (6), 18.2047 (15)
β (°)	120.342 (8)
V (Å³)	2610.8 (4)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	13.96
Crystal size (mm)	0.24 × 0.20 × 0.18

Data collection
Diffractometer	Stoe IPDS diffractometer
Absorption correction	Analytical [from crystal shape; X-SHAPE and X-RED in IPDS Software (Stoe & Cie, 1998)]
T_min, T_max	0.051, 0.083
No. of measured, independent and observed [I > 2σ(I)] reflections	12353, 2790, 2431
R_int	0.062
(sin θ/λ)_max (Å⁻¹)	0.635

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.023, 0.055, 0.96
No. of reflections	2790
No. of parameters	142
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	1.65, −0.70

Computer programs: IPDS Software (Stoe & Cie, 1998), SIR97 (Altomare et al., 1999), SHELXL97 (Sheldrick, 2008), PLATON (Spek, 2009).

Selected geometric parameters (Å, º) top

Au1—As1	2.3426 (5)	As1—C2	1.926 (5)
Au1—Cl1	2.2887 (16)	As1—C8	1.939 (5)
As1—C1	1.941 (3)

As1—Au1—Cl1	174.82 (4)	C2—As1—C8	104.72 (19)
Au1—As1—C1	108.88 (12)	As1—C1—As1ⁱ	109.5 (3)
Au1—As1—C2	116.75 (14)	As1—C2—C3	119.2 (3)
Au1—As1—C8	116.18 (13)	As1—C2—C7	120.7 (4)
C1—As1—C2	104.16 (19)	As1—C8—C9	118.9 (4)
C1—As1—C8	104.90 (11)	As1—C8—C13	121.7 (4)

Symmetry code: (i) −x, y, −z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C1—H1A···Cl1ⁱⁱ	0.9900	2.7000	3.658 (4)	163.00

Symmetry code: (ii) −x, y+1, −z+1/2.

Acknowledgements

This work was supported by the Bundesministerium für Bildung und Forschung (BMBF).

References

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