Literature DB >> 21582104

Bis[dichlorido(5,5'-dimethyl-2,2'-bi-pyridine-κN,N')gold(III)] tetra-chlorido-aurate(III) dichloridooaurate(I).

Selvi Karaca, Mehmet Akkurt, Nasser Safari, Vahid Amani, Orhan Büyükgüngör, Anita Abedi.   

Abstract

The title compound, [Au(III)Cl(2)(C(12)n class="Species">H(12)N(2))](2)[Au(III)Cl(4)][Au(I)Cl(2)], contains three distinct types of Au atom. In the cation, the Au(III) atom is four-coordinated in a distorted square-planar arrangement by an N,N'-bidentate 5,5'-dimethyl-2,2'-bipyridine ligand and two terminal Cl atoms. In the [AuCl(4)](-) anion, the centrosymmetric Au(III) atom has a square-planar coordination. The centrosymmetric [AuCl(2)](-) anion is linear. Intra- and inter-molecular C-H⋯Cl hydrogen bonds help to establish the conformation and packing.

Entities:  

Year:  2009        PMID： 21582104      PMCID： PMC2968657          DOI： 10.1107/S1600536809006436

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


Related literature

For related stuctures, see: Abbate et al. (2000 ▶); Adams & Strähle (1982 ▶); Ahmadi, Amani & Khavasi (2008 ▶); Ahmadi, Dehghan, Amani & Khavasi (2008 ▶); Bjernemose et al. (2004 ▶); Hayoun et al. (2006 ▶); Hollis & Lippard (1983 ▶); McInnes et al. (1995 ▶); Yıldırım et al. (2008 ▶).

Experimental

Crystal data

[AuCl2(n class="CellLine">C12H12N2)]2[AuCl4][AuCl2] M = 1510.86 Triclinic, a = 9.0698 (4) Å b = 10.0886 (4) Å c = 11.1678 (5) Å α = 91.155 (4)° β = 108.148 (4)° γ = 111.344 (3)° V = 894.09 (7) Å3 Z = 1 Mo Kα radiation μ = 17.13 mm−1 T = 295 K 0.41 × 0.28 × 0.08 mm

Data collection

Stoe IPDS-2 diffractometer Absorption correction: integration (X-RED32; Stoe & Cie, 2002 ▶) T min = 0.054, T max = 0.341 9898 measured reflections 3651 independent reflections 3193 reflections with I > 2σ(I) R int = 0.059

Refinement

R[F 2 > 2σ(F 2)] = 0.042 wR(F 2) = 0.112 S = 1.05 3651 reflections 191 parameters H-atom parameters constrained Δρmax = 1.64 e Å−3 Δρmin = −1.91 e Å−3 Data collection: X-AREA (Stoe & Cie, 2002 ▶); cell refinement: X-AREA; data reduction: X-RED32 (Stoe & Cie, 2002 ▶); program(s) used to solve structure: SIR97 (Altomare et al., 1999 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997 ▶); software used to prepare material for publication: WinGX (Farrugia, 1999 ▶). Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809006436/hb2902sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536809006436/hb2902Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[AuCl2(C12H12N2)]2[AuCl4][AuCl2]Z = 1
Mr = 1510.86F(000) = 682
Triclinic, P1Dx = 2.806 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.0698 (4) ÅCell parameters from 16778 reflections
b = 10.0886 (4) Åθ = 1.9–28.0°
c = 11.1678 (5) ŵ = 17.13 mm−1
α = 91.155 (4)°T = 295 K
β = 108.148 (4)°Prism, yellow
γ = 111.344 (3)°0.41 × 0.28 × 0.08 mm
V = 894.09 (7) Å3
Stoe IPDS-2 diffractometer3651 independent reflections
Radiation source: sealed X-ray tube, 12 x 0.4 mm long-fine focus3193 reflections with I > 2σ(I)
plane graphiteRint = 0.059
Detector resolution: 6.67 pixels mm-1θmax = 26.5°, θmin = 1.9°
ω scansh = −10→11
Absorption correction: integration (X-RED32; Stoe & Cie, 2002)k = −12→12
Tmin = 0.054, Tmax = 0.341l = −14→14
9898 measured reflections
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.042H-atom parameters constrained
wR(F2) = 0.112w = 1/[σ2(Fo2) + (0.0703P)2 + 0.309P] where P = (Fo2 + 2Fc2)/3
S = 1.05(Δ/σ)max = 0.001
3651 reflectionsΔρmax = 1.64 e Å−3
191 parametersΔρmin = −1.91 e Å−3
0 restraintsExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=KFc[1+0.001XFc2Λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0042 (5)
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 on F2 for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating -R-factor-obs 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.
xyzUiso*/Ueq
Au11.23403 (3)0.77774 (3)0.26312 (3)0.0544 (1)
Cl11.2859 (3)0.5914 (3)0.1987 (3)0.0790 (9)
Cl21.5117 (3)0.9173 (3)0.3196 (3)0.0782 (9)
N10.9831 (9)0.6658 (8)0.2201 (7)0.060 (2)
N21.1693 (8)0.9371 (7)0.3140 (6)0.0528 (19)
C10.9039 (11)0.5243 (9)0.1758 (9)0.066 (3)
C20.7317 (12)0.4506 (10)0.1500 (9)0.069 (3)
C30.6467 (11)0.5303 (11)0.1758 (10)0.076 (3)
C40.7298 (11)0.6737 (11)0.2244 (10)0.074 (3)
C50.8990 (11)0.7414 (9)0.2443 (8)0.060 (3)
C60.6455 (15)0.2922 (11)0.1035 (13)0.093 (4)
C71.0005 (10)0.8939 (9)0.2956 (8)0.056 (3)
C80.9407 (12)0.9933 (11)0.3240 (10)0.069 (3)
C91.0501 (13)1.1320 (11)0.3714 (11)0.076 (3)
C101.2194 (13)1.1753 (9)0.3894 (10)0.070 (3)
C111.2737 (11)1.0742 (9)0.3607 (8)0.060 (3)
C121.3426 (14)1.3307 (10)0.4439 (12)0.082 (4)
Au20.000000.000000.000000.0681 (2)
Cl30.2497 (5)−0.0056 (5)0.0129 (5)0.1187 (16)
Cl40.1272 (6)0.2391 (3)0.0717 (3)0.1093 (12)
Au31.000000.500000.500000.0654 (2)
Cl51.2288 (4)0.7061 (3)0.5439 (3)0.0836 (7)*
H10.966200.473700.161900.0790*
H30.531500.486100.160100.0910*
H40.671600.725400.243800.0880*
H6A0.621700.242300.171900.1400*
H6B0.717500.259900.074300.1400*
H6C0.542100.272800.034600.1400*
H80.826600.966000.311000.0820*
H91.009901.198800.392000.0910*
H111.387801.101000.374000.0730*
H12A1.384401.341200.535200.1240*
H12B1.285701.394600.417900.1240*
H12C1.435101.354000.412700.1240*
U11U22U33U12U13U23
Au10.0476 (2)0.0555 (2)0.0651 (2)0.0246 (1)0.0206 (1)0.0069 (1)
Cl10.0748 (14)0.0681 (12)0.1089 (19)0.0387 (10)0.0390 (13)0.0006 (12)
Cl20.0476 (10)0.0728 (13)0.113 (2)0.0220 (9)0.0284 (11)0.0031 (13)
N10.053 (3)0.062 (4)0.059 (4)0.019 (3)0.017 (3)0.002 (3)
N20.051 (3)0.060 (3)0.053 (4)0.025 (3)0.021 (3)0.009 (3)
C10.062 (5)0.057 (4)0.074 (6)0.015 (4)0.027 (4)0.002 (4)
C20.067 (5)0.066 (5)0.062 (5)0.015 (4)0.022 (4)0.000 (4)
C30.051 (5)0.080 (6)0.079 (6)0.007 (4)0.023 (4)0.003 (5)
C40.043 (4)0.072 (5)0.091 (7)0.007 (4)0.021 (4)0.005 (5)
C50.057 (4)0.066 (5)0.061 (5)0.025 (4)0.025 (4)0.011 (4)
C60.077 (7)0.072 (6)0.107 (9)0.005 (5)0.031 (6)−0.010 (6)
C70.050 (4)0.062 (4)0.060 (5)0.028 (3)0.018 (3)0.006 (4)
C80.061 (5)0.078 (5)0.079 (6)0.036 (4)0.030 (4)0.012 (5)
C90.085 (6)0.071 (5)0.094 (7)0.047 (5)0.040 (5)0.009 (5)
C100.084 (6)0.054 (4)0.071 (6)0.027 (4)0.026 (5)0.011 (4)
C110.060 (5)0.060 (4)0.062 (5)0.031 (4)0.014 (4)0.006 (4)
C120.087 (7)0.057 (5)0.103 (8)0.031 (4)0.029 (6)0.007 (5)
Au20.0810 (3)0.0527 (3)0.0547 (3)0.0170 (2)0.0130 (2)0.0067 (2)
Cl30.098 (2)0.133 (3)0.127 (3)0.052 (2)0.033 (2)0.018 (2)
Cl40.160 (3)0.0549 (12)0.0797 (18)0.0144 (15)0.0305 (19)0.0013 (11)
Au30.0724 (3)0.0670 (3)0.0672 (3)0.0335 (2)0.0296 (2)0.0161 (2)
Au1—N12.028 (9)C5—C71.466 (12)
Au1—N22.027 (7)C7—C81.375 (15)
Au1—Cl12.252 (3)C8—C91.362 (15)
Au1—Cl22.262 (3)C9—C101.380 (18)
Au2—Cl4i2.261 (3)C10—C111.355 (15)
Au2—Cl3i2.246 (5)C10—C121.530 (14)
Au2—Cl32.246 (5)C1—H10.9300
Au2—Cl42.261 (3)C3—H30.9300
Au3—Cl5ii2.248 (3)C4—H40.9300
Au3—Cl52.248 (3)C6—H6B0.9600
N1—C11.343 (12)C6—H6A0.9600
N1—C51.334 (13)C6—H6C0.9600
N2—C71.375 (13)C8—H80.9300
N2—C111.339 (11)C9—H90.9300
C1—C21.393 (15)C11—H110.9300
C2—C31.380 (16)C12—H12C0.9600
C2—C61.496 (14)C12—H12A0.9600
C3—C41.369 (15)C12—H12B0.9600
C4—C51.375 (15)
Au1···Cl3iii3.588 (5)N1···C72.368 (12)
Au1···Cl53.243 (3)N1···Cl13.173 (9)
Au2···C7iv3.490 (8)N2···Cl23.165 (9)
Au2···C7v3.490 (8)N2···N12.619 (10)
Au3···C13.486 (9)N2···C52.396 (12)
Au3···C1ii3.486 (9)C1···Au33.486 (9)
Cl1···Cl4vi3.394 (4)C1···Au33.486 (9)
Cl1···N13.173 (9)C3···Cl1viii3.625 (12)
Cl1···C13.203 (11)C5···Cl4iv3.477 (9)
Cl1···Cl23.166 (4)C6···Cl33.564 (14)
Cl1···C3vi3.625 (12)C7···Au2iv3.490 (8)
Cl2···N23.165 (9)C7···Au2iii3.490 (8)
Cl2···C113.233 (11)C8···Cl3iv3.644 (12)
Cl2···Cl13.166 (4)C10···Cl4iii3.513 (11)
Cl2···C11vii3.476 (9)C11···Cl2vii3.476 (9)
Cl2···Cl5vii3.650 (4)C12···C12xi3.448 (15)
Cl3···C63.564 (14)C4···H82.8100
Cl3···C8iv3.644 (12)C8···H42.7900
Cl3···Cl43.185 (7)H1···Cl12.5900
Cl3···Au1v3.588 (5)H1···H6B2.3900
Cl3···Cl4i3.188 (7)H3···Cl1viii2.9300
Cl4···Cl3i3.188 (7)H3···H6C2.5900
Cl4···C10v3.513 (11)H4···C82.7900
Cl4···C5iv3.477 (9)H4···Cl1viii3.1200
Cl4···Cl33.185 (7)H4···Cl2viii3.0500
Cl4···Cl1viii3.394 (4)H4···H82.2800
Cl4···N1iv3.367 (8)H6A···Cl5ii2.9900
Cl5···Au13.243 (3)H6B···H12.3900
Cl5···Cl2vii3.650 (4)H6B···Cl3ix2.8700
Cl1···H4vi3.1200H6C···H32.5900
Cl1···H12.5900H6C···Cl33.0200
Cl1···H3vi2.9300H8···H42.2800
Cl2···H8vi2.7500H8···C42.8100
Cl2···H112.6400H8···Cl2viii2.7500
Cl2···H4vi3.0500H9···H12B2.4800
Cl3···H6C3.0200H9···Cl5x2.9300
Cl3···H6Bix2.8700H11···Cl22.6400
Cl5···H11vii3.1200H11···H12C2.4300
Cl5···H6Aii2.9900H11···Cl5vii3.1200
Cl5···H9x2.9300H12B···H92.4800
N1···Cl4iv3.367 (8)H12C···H112.4300
N1···N22.619 (10)
Cl1—Au1—Cl289.07 (11)C7—C8—C9119.4 (11)
Cl1—Au1—N195.5 (2)C8—C9—C10121.3 (11)
Cl1—Au1—N2175.8 (2)C11—C10—C12121.1 (11)
Cl2—Au1—N1175.3 (2)C9—C10—C11117.6 (9)
Cl2—Au1—N295.0 (2)C9—C10—C12121.3 (10)
N1—Au1—N280.5 (3)N2—C11—C10122.5 (10)
Cl3i—Au2—Cl4i89.95 (19)C2—C1—H1119.00
Cl3—Au2—Cl4i90.05 (19)N1—C1—H1119.00
Cl3—Au2—Cl489.95 (19)C2—C3—H3120.00
Cl3—Au2—Cl3i180.00C4—C3—H3120.00
Cl3i—Au2—Cl490.05 (19)C3—C4—H4120.00
Cl4—Au2—Cl4i180.00C5—C4—H4120.00
Cl5—Au3—Cl5ii180.00C2—C6—H6A109.00
Au1—N1—C1124.0 (7)C2—C6—H6B109.00
Au1—N1—C5115.3 (6)C2—C6—H6C109.00
C1—N1—C5120.7 (9)H6B—C6—H6C109.00
Au1—N2—C11126.2 (7)H6A—C6—H6B109.00
Au1—N2—C7113.9 (5)H6A—C6—H6C109.00
C7—N2—C11120.0 (8)C7—C8—H8120.00
N1—C1—C2122.3 (10)C9—C8—H8120.00
C3—C2—C6121.8 (11)C10—C9—H9119.00
C1—C2—C3116.3 (9)C8—C9—H9119.00
C1—C2—C6121.8 (10)N2—C11—H11119.00
C2—C3—C4120.9 (10)C10—C11—H11119.00
C3—C4—C5120.1 (10)C10—C12—H12A110.00
N1—C5—C4119.7 (8)C10—C12—H12B109.00
N1—C5—C7115.4 (9)C10—C12—H12C109.00
C4—C5—C7124.8 (9)H12A—C12—H12B109.00
N2—C7—C5115.0 (8)H12A—C12—H12C109.00
N2—C7—C8119.3 (8)H12B—C12—H12C109.00
C5—C7—C8125.8 (9)
Cl1—Au1—N1—C13.4 (7)C11—N2—C7—C80.9 (12)
N2—Au1—N1—C1−177.7 (8)N1—C1—C2—C3−1.7 (14)
Cl1—Au1—N1—C5−179.5 (6)N1—C1—C2—C6−178.6 (10)
N2—Au1—N1—C5−0.7 (6)C6—C2—C3—C4176.7 (10)
Cl2—Au1—N2—C7−179.0 (5)C1—C2—C3—C4−0.2 (15)
N1—Au1—N2—C70.0 (6)C2—C3—C4—C52.1 (16)
Cl2—Au1—N2—C111.5 (7)C3—C4—C5—C7180.0 (9)
N1—Au1—N2—C11−179.5 (7)C3—C4—C5—N1−2.2 (14)
Au1—N1—C1—C2178.6 (7)C4—C5—C7—N2176.7 (8)
C5—N1—C1—C21.7 (14)C4—C5—C7—C8−4.2 (15)
Au1—N1—C5—C4−176.8 (7)N1—C5—C7—N2−1.2 (11)
C1—N1—C5—C40.4 (13)N1—C5—C7—C8177.9 (9)
Au1—N1—C5—C71.2 (10)C5—C7—C8—C9180.0 (9)
C1—N1—C5—C7178.4 (8)N2—C7—C8—C9−0.9 (14)
Au1—N2—C11—C10178.3 (7)C7—C8—C9—C101.1 (16)
C7—N2—C11—C10−1.1 (13)C8—C9—C10—C11−1.3 (16)
Au1—N2—C7—C8−178.6 (7)C8—C9—C10—C12−179.4 (10)
Au1—N2—C7—C50.6 (9)C12—C10—C11—N2179.4 (9)
C11—N2—C7—C5−179.9 (7)C9—C10—C11—N21.3 (14)
D—H···AD—HH···AD···AD—H···A
C1—H1···Cl10.932.593.203 (11)124
C8—H8···Cl2viii0.932.753.666 (12)169
C11—H11···Cl20.932.643.233 (11)122
Table 1

Selected bond lengths (Å)

Au1—N12.028 (9)
Au1—N22.027 (7)
Au1—Cl12.252 (3)
Au1—Cl22.262 (3)
Au2—Cl32.246 (5)
Au2—Cl42.261 (3)
Au3—Cl52.248 (3)
Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
C1—H1⋯Cl10.932.593.203 (11)124
C8—H8⋯Cl2i0.932.753.666 (12)169
C11—H11⋯Cl20.932.643.233 (11)122

Symmetry code: (i) .

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