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Acta Cryst. (2007). E63, m1698-m1699    [ doi:10.1107/S160053680702421X ]

Bis[[mu]2-bis(diphenylphosphino)methane]-1:2[kappa]2P:P';2:3[kappa]2P:P'-dichlorido-1[kappa]Cl,3[kappa]Cl-triangulo-trigold(I) hexafluorophosphate

E. C. Constable, C. E. Housecroft, M. Neuburger, S. Schaffner and E. J. Shardlow

Abstract top

In the title compound, [Au3Cl2(C25H22P2)2](PF6), the cation possesses a triangular Au3 core [Au-Au distances 3.1525 (4), 3.2770 (4) and 3.1922 (4) Å], two sides of which are bridged by dppm ligands [dppm = bis(diphenylphosphino)methane]. One phenyl group is disordered over two positions in a 0.65:0.35 ratio. The structure of the cation is compared with those in three other salts reported previously.

Comment top

The structure of [I]+ has been determined in several salts (Usón et al., 1983, Lin et al., 1994; Zhang et al., 2005) and exhibits a V-shaped cluster of gold(I) centres. The structure of the cation in [I][PF6] is shown in Fig. 1; with the exception of the bond parameters for the Au3 unit, bond distances and angles are similar to those previously reported. One phenyl ring (atoms C89—C94 and C39—C44) is disordered over two positions with 0.65 (3) and 0.35 (3) occupancies. The three gold atoms in [I][PF6] form a near equilateral triangle with Au—Au—Au bond angles in the range 58.311 (9) to 62.190 (9)o. The two shorter edges are bridged by dppm ligands, one above and one below the triangle. This ligand disposition and the orientation of the two chloro ligands resembles those observed for [I]+ in the chloro (Lin et al., 1994), the perchlorate (Zhang, et al., 2005) and the chlorotris(pentafluorophenyl)gold(III) (Usón et al., 1983) salts. The principal difference between the structures arises in the aurophilic interactions (Pyykkö, 2002; Pyykkö, 2004) in the trigold unit (Table 1). The atom numbering for all structures in Table 1 is as defined in Fig. 1. No e.s.d.'s are available for atom positions in [I][AuCl(C6F5)3]. It has been reported that the strength of an aurophilic interaction is comparable to that of a typical hydrogen bond (Pyykkö, 2004), and the coexistence of gold···gold contacts and hydrogen-bonded interactions and their role in crystal engineering has been discussed (Mendizabal et al., 2003). Hydrogen bonding involving [PF6]- anions in [I][PF6] is extensive (Fig. 2 and Table 2) and we conclude that the geometry of the Au3 cluster in salts containing [I]+ responds to the influence of the hydrogen-bonded interactions in the lattice.

Related literature top

For related literature, see: Lin et al. (1994); Mendizabal et al. (2003); Pyykkö (2002, 2004); Shardlow (2007); Usón et al. (1983); Zhang et al. (2005).

Experimental top

ClAu(µ-dppm)AuCl was prepared by a literature method (Lin et al., 1994). Crystals of [I][PF6] were obtained serendipidously from a crude reaction mixture (CH2Cl2) containing ClAu(µ-dppm)AuCl to which an excess of NH4PF6 had been added (Shardlow, 2007).

Refinement top

All H atoms were treated as riding models, with C—H = 0.96 Å and Uiso(H) = 1.2Ueq(C). Restraints have been used to control the behaviour of the disordered phenyl ring and the PF6. C—C and P—F distances have been restrained to their common means respectively. Moreover U-values of bonded atoms in these two structural fragments have been restrained to be similar.

Computing details top

Data collection: COLLECT (Nonius, 2001); cell refinement: DENZO and SCALEPACK (Otwinowski & Minor, 1997); data reduction: DENZO and SCALEPACK; program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: CRYSTALS (Betteridge et al., 2003); molecular graphics: CAMERON (Watkin et al., 1996); software used to prepare material for publication: CRYSTALS.

Figures top
[Figure 1] Fig. 1. The molecular structure of [I]+ in [I][PF6] with displacement ellipsoids drawn at the 20% probability level. H atoms are omitted for clarity. One phenyl ring is disordered and only the major occupancies C89—C94 are shown.
[Figure 2] Fig. 2. Hydrogen-bonds in [I][PF6] involving [PF6]- anions. Symmetry codes: i = 1 - x, 1 - y, 1 - z; ii = x, 1 + y, z; iii = 1 - x, -y, -z.
Bis[µ2-bis(diphenylphosphino)methane]- 1:2κ2P:P';2:3κ2P:P'- dichlorido-1κCl,3κCl-trigold(I) hexafluorophosphate top
Crystal data top
[Au3Cl2(C25H22P2)2](PF6)Z = 2
Mr = 1575.56F(000) = 1488
Triclinic, P1Dx = 2.044 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.6740 (1) ÅCell parameters from 12197 reflections
b = 15.4549 (2) Åθ = 1–28°
c = 18.9003 (3) ŵ = 8.89 mm−1
α = 105.9872 (8)°T = 173 K
β = 101.5928 (7)°Plate, colourless
γ = 101.6696 (8)°0.11 × 0.09 × 0.09 mm
V = 2559.58 (6) Å3
Data collection top
Nonius KappaCCD
diffractometer		8452 reflections with I > 3σ(I)
graphiteRint = 0.026
φ and ω scansθmax = 27.9°, θmin = 1.2°
Absorption correction: multi-scan
DENZO and SCALEPACK (Otwinowski & Minor, 1997)		h = −12→12
Tmin = 0.38, Tmax = 0.45k = −20→20
23737 measured reflectionsl = −24→24
12197 independent reflections
Refinement top
Refinement on FHydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.036 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A0*T0(x) + A1*T1(x) ··· + An-1]*Tn-1(x)]
where Ai are the Chebychev coefficients listed below and x = F /Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)2]2 Ai are: 0.371 0.154 0.134
Prince, E. (1982). Mathematical Techniques in Crystallography and Materials Science. New York: Springer-Verlag.
Watkin, D. (1994). Acta Cryst. A50, 411–437.
wR(F2) = 0.041(Δ/σ)max = 0.002
S = 1.11Δρmax = 2.95 e Å−3
8452 reflectionsΔρmin = −4.06 e Å−3
651 parametersExtinction correction: Larson (1970), Equation 22
144 restraintsExtinction coefficient: 25 (4)
Primary atom site location: structure-invariant direct methods
Crystal data top
[Au3Cl2(C25H22P2)2](PF6)γ = 101.6696 (8)°
Mr = 1575.56V = 2559.58 (6) Å3
Triclinic, P1Z = 2
a = 9.6740 (1) ÅMo Kα radiation
b = 15.4549 (2) ŵ = 8.89 mm−1
c = 18.9003 (3) ÅT = 173 K
α = 105.9872 (8)°0.11 × 0.09 × 0.09 mm
β = 101.5928 (7)°
Data collection top
Nonius KappaCCD
diffractometer		12197 independent reflections
Absorption correction: multi-scan
DENZO and SCALEPACK (Otwinowski & Minor, 1997)		8452 reflections with I > 3σ(I)
Tmin = 0.38, Tmax = 0.45Rint = 0.026
23737 measured reflectionsθmax = 27.9°
Refinement top
R[F2 > 2σ(F2)] = 0.036H-atom parameters constrained
wR(F2) = 0.041Δρmax = 2.95 e Å−3
S = 1.11Δρmin = −4.06 e Å−3
8452 reflectionsAbsolute structure: ?
651 parametersFlack parameter: ?
144 restraintsRogers parameter: ?
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Au10.53079 (3)0.538005 (18)0.269126 (16)0.0384
Au20.85524 (3)0.612438 (19)0.263223 (16)0.0381
Au30.60667 (3)0.46319 (3)0.110429 (16)0.0481
Cl20.9497 (2)0.48182 (12)0.24667 (14)0.0622
Cl30.67207 (17)0.59597 (13)0.07330 (9)0.0404
P10.47840 (18)0.67473 (12)0.26160 (10)0.0343
P20.80771 (18)0.75229 (12)0.28655 (10)0.0345
P30.54834 (19)0.40221 (12)0.29448 (10)0.0345
P40.5357 (2)0.32487 (17)0.12760 (11)0.0492
P50.6289 (3)0.05910 (16)0.26952 (18)0.0699
C10.3153 (7)0.6553 (5)0.1858 (4)0.0389
C20.3099 (9)0.6066 (7)0.1109 (5)0.0567
C30.1877 (10)0.5902 (8)0.0515 (5)0.0658
C40.0678 (9)0.6204 (8)0.0683 (6)0.0633
C50.0711 (11)0.6654 (10)0.1405 (7)0.0874
C60.1937 (10)0.6830 (8)0.2002 (6)0.0708
C70.4504 (8)0.7439 (5)0.3493 (4)0.0423
C80.4398 (14)0.7087 (8)0.4077 (6)0.0763
C90.4172 (17)0.7641 (11)0.4753 (7)0.0966
C100.4015 (14)0.8493 (9)0.4824 (6)0.0813
C110.4133 (10)0.8847 (7)0.4253 (5)0.0635
C120.4375 (9)0.8335 (6)0.3588 (4)0.0482
C130.6236 (7)0.7503 (5)0.2395 (4)0.0362
C140.8397 (8)0.8099 (5)0.3875 (4)0.0394
C150.8084 (8)0.8944 (5)0.4164 (5)0.0474
C160.8355 (9)0.9362 (6)0.4939 (5)0.0586
C170.8992 (15)0.8984 (8)0.5447 (6)0.0783
C180.930 (2)0.8157 (10)0.5176 (7)0.1188
C190.9010 (18)0.7708 (8)0.4398 (6)0.0928
C200.9235 (8)0.8334 (5)0.2544 (4)0.0394
C210.8744 (10)0.8529 (9)0.1886 (7)0.0788
C220.9696 (13)0.9104 (10)0.1641 (8)0.0935
C231.1131 (11)0.9483 (7)0.2048 (7)0.0700
C241.1642 (9)0.9310 (6)0.2719 (6)0.0569
C251.0690 (9)0.8736 (6)0.2964 (5)0.0493
C260.6729 (8)0.4262 (5)0.3875 (4)0.0445
C270.6617 (13)0.4984 (8)0.4482 (5)0.0743
C280.7438 (16)0.5169 (12)0.5207 (6)0.1015
C290.8367 (15)0.4635 (12)0.5355 (6)0.0980
C300.8541 (14)0.3944 (10)0.4760 (7)0.0902
C310.7710 (11)0.3747 (7)0.4016 (5)0.0657
C320.3757 (8)0.3331 (5)0.2981 (4)0.0377
C330.3741 (9)0.2537 (5)0.3186 (5)0.0482
C340.2439 (11)0.1979 (6)0.3189 (6)0.0586
C350.1145 (10)0.2204 (6)0.3007 (6)0.0607
C360.1152 (10)0.3006 (7)0.2817 (6)0.0645
C370.2461 (9)0.3584 (6)0.2815 (5)0.0533
C380.6086 (8)0.3223 (5)0.2235 (4)0.0405
C450.5879 (11)0.2338 (7)0.0645 (5)0.0639
C460.6316 (12)0.1662 (8)0.0864 (6)0.0724
C470.6587 (16)0.0918 (8)0.0301 (9)0.0979
C480.6431 (18)0.0947 (9)−0.0425 (8)0.0984
C490.606 (2)0.1659 (13)−0.0636 (8)0.1303
C500.5781 (17)0.2351 (10)−0.0100 (6)0.0999
C390.344 (4)0.255 (4)0.102 (3)0.08860.35 (3)
C400.299 (3)0.165 (3)0.107 (2)0.09110.35 (3)
C410.149 (2)0.117 (3)0.085 (2)0.09860.35 (3)
C420.045 (3)0.162 (3)0.061 (3)0.10500.35 (3)
C430.090 (3)0.252 (3)0.057 (3)0.10940.35 (3)
C440.240 (3)0.298 (4)0.076 (3)0.10230.35 (3)
C890.3386 (16)0.2954 (10)0.1095 (10)0.04970.65 (3)
C900.2670 (16)0.2046 (11)0.1045 (10)0.06340.65 (3)
C910.1153 (16)0.1797 (14)0.0948 (11)0.08160.65 (3)
C920.0366 (17)0.2456 (14)0.0896 (11)0.08520.65 (3)
C930.1088 (13)0.3366 (14)0.0955 (9)0.07330.65 (3)
C940.2601 (13)0.3617 (13)0.1047 (8)0.05790.65 (3)
F10.5384 (9)−0.0466 (4)0.2460 (5)0.1087
F20.7181 (10)0.1628 (4)0.2882 (7)0.1579
F30.6891 (10)0.0284 (6)0.1969 (5)0.1189
F40.5492 (12)0.0834 (7)0.3351 (4)0.1344
F50.4984 (6)0.0786 (4)0.2162 (3)0.0704
F60.7605 (10)0.0398 (6)0.3212 (6)0.1499
H210.39150.58400.10050.0717*
H310.18540.5587−0.00040.0781*
H41−0.01820.60860.02760.0734*
H51−0.01230.68580.15100.0966*
H610.19440.71480.25170.0782*
H810.44730.64640.40260.1033*
H910.41330.74000.51680.1262*
H1010.38230.88540.52770.0960*
H1110.40460.94680.43110.0695*
H1210.44540.86020.31910.0552*
H1310.61430.81300.25500.0470*
H1320.61050.72850.18520.0470*
H1510.76770.92350.38160.0551*
H1610.80850.99330.51230.0658*
H1710.92180.93000.59900.0930*
H1810.97460.78740.55240.1198*
H1910.92180.71200.42140.1026*
H2110.77350.82640.15950.1034*
H2210.93420.92370.11820.1285*
H2311.17900.98700.18690.0929*
H2411.26480.95850.30120.0704*
H2511.10410.86150.34290.0615*
H2710.59560.53500.43850.0862*
H2810.73720.56730.56170.1114*
H2910.88960.47420.58720.1084*
H3010.92370.36010.48620.1109*
H3110.78110.32590.36040.0810*
H3310.46400.23740.33250.0622*
H3410.24380.14220.33220.0754*
H3510.02450.18090.30100.0743*
H3610.02490.31670.26850.0813*
H3710.24660.41520.27000.0702*
H3810.71380.34060.23630.0511*
H3820.57500.25980.22430.0511*
H4010.36900.13570.12490.1098*0.3500
H4110.11880.05580.08670.1190*0.3500
H421−0.05700.13090.04800.1274*0.3500
H4310.01960.28150.04020.1340*0.3500
H4410.27070.35550.06850.1281*0.3500
H9010.32100.16030.10760.0703*0.6500
H9110.06590.11840.09180.0888*0.6500
H921−0.06710.22820.08160.0984*0.6500
H9310.05460.38110.09300.0949*0.6500
H9410.30900.42260.10730.0807*0.6500
H4610.64470.16710.13840.0874*
H4710.68690.04110.04350.1149*
H4810.65920.0444−0.08010.1092*
H4910.59980.1677−0.11460.1489*
H5010.55120.2859−0.02380.1136*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Au10.04197 (14)0.03611 (14)0.04576 (15)0.01282 (11)0.01474 (11)0.02356 (12)
Au20.03584 (14)0.03875 (15)0.04292 (15)0.01733 (11)0.00944 (11)0.01406 (11)
Au30.04596 (16)0.0768 (2)0.03611 (15)0.02721 (14)0.01776 (12)0.02902 (14)
Cl20.0510 (10)0.0267 (8)0.0873 (15)0.0177 (7)−0.0229 (10)0.0101 (9)
Cl30.0341 (7)0.0638 (11)0.0259 (7)0.0151 (7)0.0100 (6)0.0163 (7)
P10.0354 (8)0.0359 (9)0.0400 (9)0.0127 (7)0.0165 (7)0.0189 (7)
P20.0349 (8)0.0363 (9)0.0409 (9)0.0138 (7)0.0151 (7)0.0195 (7)
P30.0400 (9)0.0353 (9)0.0338 (8)0.0126 (7)0.0107 (7)0.0178 (7)
P40.0406 (10)0.0726 (14)0.0350 (9)0.0115 (9)0.0119 (8)0.0203 (9)
P50.0814 (16)0.0422 (12)0.0975 (19)0.0271 (11)0.0226 (14)0.0346 (12)
C10.034 (3)0.038 (4)0.048 (4)0.008 (3)0.014 (3)0.018 (3)
C20.049 (4)0.085 (6)0.045 (4)0.036 (4)0.017 (4)0.021 (4)
C30.054 (5)0.102 (8)0.039 (4)0.024 (5)0.012 (4)0.019 (5)
C40.036 (4)0.086 (7)0.061 (5)0.016 (4)−0.001 (4)0.025 (5)
C50.047 (5)0.115 (9)0.080 (7)0.032 (6)0.012 (5)−0.004 (7)
C60.042 (4)0.089 (7)0.065 (6)0.022 (5)0.011 (4)−0.001 (5)
C70.042 (4)0.043 (4)0.045 (4)0.009 (3)0.020 (3)0.015 (3)
C80.113 (9)0.079 (7)0.066 (6)0.038 (6)0.056 (6)0.039 (5)
C90.137 (11)0.115 (10)0.063 (7)0.035 (9)0.063 (7)0.043 (7)
C100.096 (8)0.090 (8)0.054 (6)0.025 (7)0.035 (6)0.008 (6)
C110.055 (5)0.068 (6)0.050 (5)0.013 (4)0.015 (4)−0.004 (4)
C120.051 (4)0.047 (4)0.039 (4)0.011 (3)0.012 (3)0.005 (3)
C130.039 (3)0.035 (3)0.043 (4)0.014 (3)0.017 (3)0.020 (3)
C140.044 (4)0.039 (4)0.045 (4)0.016 (3)0.021 (3)0.020 (3)
C150.044 (4)0.037 (4)0.055 (5)0.008 (3)0.010 (3)0.010 (3)
C160.051 (5)0.045 (4)0.065 (6)0.006 (4)0.020 (4)−0.003 (4)
C170.122 (9)0.068 (6)0.047 (5)0.021 (6)0.041 (6)0.014 (5)
C180.25 (2)0.095 (9)0.051 (6)0.098 (11)0.052 (9)0.034 (6)
C190.180 (13)0.080 (7)0.043 (5)0.079 (8)0.032 (7)0.027 (5)
C200.038 (3)0.039 (4)0.048 (4)0.014 (3)0.018 (3)0.018 (3)
C210.049 (5)0.119 (9)0.088 (7)0.011 (5)0.017 (5)0.076 (7)
C220.066 (6)0.141 (11)0.113 (9)0.023 (7)0.039 (6)0.095 (9)
C230.059 (5)0.074 (6)0.099 (8)0.012 (5)0.046 (5)0.050 (6)
C240.050 (4)0.045 (4)0.081 (6)0.011 (4)0.031 (4)0.020 (4)
C250.048 (4)0.048 (4)0.058 (5)0.017 (3)0.021 (4)0.019 (4)
C260.049 (4)0.048 (4)0.036 (4)0.006 (3)0.009 (3)0.022 (3)
C270.089 (7)0.088 (7)0.039 (5)0.026 (6)0.009 (5)0.015 (5)
C280.096 (9)0.143 (12)0.040 (5)0.009 (9)0.008 (6)0.016 (7)
C290.088 (8)0.144 (12)0.040 (5)−0.008 (8)−0.006 (5)0.041 (7)
C300.084 (8)0.123 (10)0.070 (7)0.034 (7)−0.003 (6)0.053 (7)
C310.067 (6)0.080 (6)0.056 (5)0.023 (5)0.005 (4)0.036 (5)
C320.047 (4)0.030 (3)0.040 (4)0.009 (3)0.016 (3)0.016 (3)
C330.058 (5)0.036 (4)0.061 (5)0.018 (3)0.024 (4)0.024 (3)
C340.080 (6)0.037 (4)0.072 (6)0.016 (4)0.032 (5)0.028 (4)
C350.060 (5)0.056 (5)0.070 (6)0.005 (4)0.029 (4)0.026 (4)
C360.048 (5)0.063 (6)0.092 (7)0.019 (4)0.025 (5)0.034 (5)
C370.047 (4)0.053 (5)0.075 (6)0.020 (4)0.025 (4)0.034 (4)
C380.042 (4)0.045 (4)0.040 (4)0.015 (3)0.014 (3)0.019 (3)
C450.070 (6)0.051 (5)0.055 (5)−0.007 (4)0.028 (4)0.002 (4)
C460.082 (7)0.069 (6)0.067 (6)0.006 (5)0.047 (5)0.015 (5)
C470.121 (10)0.050 (6)0.116 (10)−0.002 (6)0.071 (9)0.007 (6)
C480.141 (12)0.061 (7)0.073 (8)0.003 (7)0.054 (8)−0.012 (6)
C490.204 (19)0.107 (12)0.061 (8)0.023 (12)0.049 (10)0.002 (8)
C500.139 (12)0.105 (10)0.040 (5)0.023 (8)0.029 (6)0.004 (6)
C390.048 (13)0.15 (3)0.086 (16)0.002 (14)0.012 (11)0.094 (19)
C400.045 (12)0.15 (3)0.094 (16)−0.002 (13)0.012 (11)0.085 (18)
C410.047 (11)0.16 (3)0.103 (17)−0.001 (13)0.017 (12)0.082 (19)
C420.052 (12)0.17 (3)0.109 (18)0.001 (13)0.011 (12)0.091 (19)
C430.058 (12)0.17 (3)0.114 (19)0.004 (14)0.005 (13)0.10 (2)
C440.058 (12)0.16 (3)0.106 (18)0.010 (14)0.010 (13)0.10 (2)
C890.039 (6)0.082 (8)0.037 (6)0.016 (6)0.009 (5)0.034 (7)
C900.050 (7)0.076 (9)0.048 (7)−0.002 (7)0.004 (6)0.016 (7)
C910.055 (8)0.099 (11)0.067 (9)−0.011 (7)0.012 (7)0.016 (8)
C920.050 (8)0.132 (13)0.063 (8)0.006 (7)0.013 (7)0.031 (9)
C930.049 (6)0.132 (13)0.055 (8)0.035 (7)0.013 (6)0.051 (8)
C940.041 (6)0.123 (11)0.039 (6)0.044 (7)0.019 (5)0.049 (7)
F10.137 (6)0.053 (3)0.144 (6)0.016 (4)0.046 (5)0.047 (4)
F20.123 (6)0.054 (4)0.228 (10)−0.007 (4)−0.063 (6)0.043 (5)
F30.121 (6)0.136 (6)0.161 (7)0.074 (5)0.087 (5)0.081 (6)
F40.206 (9)0.155 (7)0.073 (4)0.103 (7)0.045 (5)0.041 (5)
F50.076 (3)0.065 (3)0.079 (4)0.023 (3)0.025 (3)0.032 (3)
F60.141 (7)0.109 (6)0.187 (8)0.051 (5)−0.030 (6)0.071 (6)
Geometric parameters (Å, °) top
Au1—Au23.1525 (4)C21—H2110.960
Au1—Au33.1922 (4)C22—C231.363 (16)
Au1—P12.3047 (16)C22—H2210.959
Au1—P32.3083 (16)C23—C241.382 (14)
Au2—Au33.2770 (4)C23—H2310.961
Au2—Cl22.3496 (17)C24—C251.385 (11)
Au2—P22.2441 (17)C24—H2410.960
Au3—Cl32.3560 (18)C25—H2510.960
Au3—P42.241 (2)C26—C271.403 (13)
P1—C11.815 (7)C26—C311.387 (12)
P1—C71.812 (7)C27—C281.357 (15)
P1—C131.831 (7)C27—H2710.959
P2—C131.814 (7)C28—C291.38 (2)
P2—C141.802 (7)C28—H2810.960
P2—C201.823 (7)C29—C301.39 (2)
P3—C261.814 (7)C29—H2910.960
P3—C321.817 (7)C30—C311.387 (14)
P3—C381.832 (7)C30—H3010.960
P4—C381.822 (7)C31—H3110.960
P4—C451.806 (10)C32—C331.382 (9)
P4—C391.84 (4)C32—C371.390 (10)
P4—C891.806 (15)C33—C341.378 (12)
P5—F11.579 (6)C33—H3310.960
P5—F21.563 (6)C34—C351.369 (13)
P5—F31.588 (7)C34—H3410.960
P5—F41.586 (7)C35—C361.381 (13)
P5—F51.584 (5)C35—H3510.960
P5—F61.574 (6)C36—C371.396 (12)
C1—C21.393 (11)C36—H3610.960
C1—C61.382 (11)C37—H3710.960
C2—C31.383 (12)C38—H3810.960
C2—H210.959C38—H3820.960
C3—C41.395 (13)C45—C461.338 (16)
C3—H310.960C45—C501.398 (15)
C4—C51.342 (15)C46—C471.443 (15)
C4—H410.960C46—H4610.960
C5—C61.383 (14)C47—C481.36 (2)
C5—H510.960C47—H4710.960
C6—H610.960C48—C491.36 (2)
C7—C81.372 (12)C48—H4810.960
C7—C121.380 (11)C49—C501.37 (2)
C8—C91.414 (15)C49—H4910.961
C8—H810.960C50—H5010.960
C9—C101.329 (18)C39—C401.403 (10)
C9—H910.961C39—C441.402 (10)
C10—C111.350 (16)C40—C411.401 (10)
C10—H1010.960C40—H4010.944
C11—C121.381 (11)C41—C421.401 (10)
C11—H1110.959C41—H4110.946
C12—H1210.960C42—C431.401 (10)
C13—H1310.960C42—H4210.958
C13—H1320.960C43—C441.403 (10)
C14—C151.389 (10)C43—H4310.946
C14—C191.390 (12)C44—H4410.937
C15—C161.374 (12)C89—C901.401 (9)
C15—H1510.959C89—C941.404 (9)
C16—C171.363 (15)C90—C911.400 (9)
C16—H1610.964C90—H9010.949
C17—C181.356 (16)C91—C921.402 (10)
C17—H1710.965C91—H9110.951
C18—C191.383 (14)C92—C931.400 (9)
C18—H1810.964C92—H9210.953
C19—H1910.957C93—C941.399 (9)
C20—C211.373 (12)C93—H9310.951
C20—C251.387 (11)C94—H9410.948
C21—C221.386 (13)
Au2—Au1—Au362.191 (9)C14—C19—C18120.5 (9)
Au2—Au1—P191.42 (4)C14—C19—H191119.2
Au3—Au1—P1101.01 (4)C18—C19—H191120.3
Au2—Au1—P399.15 (4)P2—C20—C21122.8 (6)
Au3—Au1—P390.65 (4)P2—C20—C25118.3 (6)
P1—Au1—P3167.01 (6)C21—C20—C25118.9 (7)
Au1—Au2—Au359.499 (9)C20—C21—C22120.4 (9)
Au1—Au2—Cl2104.90 (6)C20—C21—H211119.8
Au3—Au2—Cl279.66 (5)C22—C21—H211119.8
Au1—Au2—P284.86 (4)C21—C22—C23120.4 (10)
Au3—Au2—P2108.81 (5)C21—C22—H221119.8
Cl2—Au2—P2169.64 (7)C23—C22—H221119.8
Au1—Au3—Au258.311 (9)C22—C23—C24120.1 (8)
Au1—Au3—Cl3105.39 (4)C22—C23—H231120.0
Au2—Au3—Cl377.12 (4)C24—C23—H231119.9
Au1—Au3—P482.19 (5)C23—C24—C25119.4 (8)
Au2—Au3—P4110.30 (5)C23—C24—H241120.3
Cl3—Au3—P4171.67 (7)C25—C24—H241120.3
Au1—P1—C1113.1 (2)C20—C25—C24120.7 (8)
Au1—P1—C7112.9 (2)C20—C25—H251119.7
C1—P1—C7106.5 (3)C24—C25—H251119.6
Au1—P1—C13112.6 (2)P3—C26—C27116.6 (7)
C1—P1—C13104.1 (3)P3—C26—C31123.8 (7)
C7—P1—C13106.9 (3)C27—C26—C31119.5 (8)
Au2—P2—C13115.4 (2)C26—C27—C28120.5 (11)
Au2—P2—C14111.4 (2)C26—C27—H271119.8
C13—P2—C14107.5 (3)C28—C27—H271119.7
Au2—P2—C20113.2 (2)C27—C28—C29120.2 (13)
C13—P2—C20103.1 (3)C27—C28—H281120.0
C14—P2—C20105.5 (3)C29—C28—H281119.8
Au1—P3—C26111.9 (3)C28—C29—C30120.2 (10)
Au1—P3—C32113.3 (2)C28—C29—H291119.8
C26—P3—C32104.4 (3)C30—C29—H291120.0
Au1—P3—C38113.9 (2)C29—C30—C31120.1 (11)
C26—P3—C38107.6 (4)C29—C30—H301119.9
C32—P3—C38105.1 (3)C31—C30—H301119.9
Au3—P4—C38115.6 (3)C30—C31—C26119.3 (10)
Au3—P4—C45112.1 (3)C30—C31—H311120.4
C38—P4—C45105.3 (4)C26—C31—H311120.3
Au3—P4—C39124.8 (11)P3—C32—C33118.9 (6)
C38—P4—C39102.2 (12)P3—C32—C37121.7 (5)
C45—P4—C3993.3 (18)C33—C32—C37119.4 (7)
Au3—P4—C89107.3 (5)C32—C33—C34120.2 (7)
C38—P4—C89106.4 (6)C32—C33—H331119.9
C45—P4—C89110.0 (6)C34—C33—H331119.9
F1—P5—F2176.9 (6)C33—C34—C35121.1 (7)
F1—P5—F387.3 (5)C33—C34—H341119.5
F2—P5—F390.0 (7)C35—C34—H341119.4
F1—P5—F488.3 (5)C34—C35—C36119.2 (8)
F2—P5—F494.3 (7)C34—C35—H351120.4
F3—P5—F4173.0 (6)C36—C35—H351120.4
F1—P5—F590.2 (4)C35—C36—C37120.6 (8)
F2—P5—F588.3 (4)C35—C36—H361119.8
F3—P5—F587.7 (4)C37—C36—H361119.7
F4—P5—F586.9 (4)C36—C37—C32119.4 (7)
F1—P5—F690.2 (5)C36—C37—H371120.3
F2—P5—F691.3 (5)C32—C37—H371120.3
F3—P5—F691.1 (6)P3—C38—P4111.3 (4)
F4—P5—F694.3 (6)P3—C38—H381109.0
F5—P5—F6178.8 (6)P4—C38—H381109.0
P1—C1—C2118.7 (5)P3—C38—H382109.0
P1—C1—C6122.4 (6)P4—C38—H382109.0
C2—C1—C6118.8 (7)H381—C38—H382109.5
C1—C2—C3120.6 (7)P4—C45—C46122.4 (7)
C1—C2—H21119.7P4—C45—C50117.2 (10)
C3—C2—H21119.7C46—C45—C50120.4 (10)
C2—C3—C4118.7 (8)C45—C46—C47118.4 (11)
C2—C3—H31120.6C45—C46—H461120.8
C4—C3—H31120.7C47—C46—H461120.8
C3—C4—C5120.9 (8)C46—C47—C48118.8 (13)
C3—C4—H41119.5C46—C47—H471120.6
C5—C4—H41119.6C48—C47—H471120.6
C4—C5—C6120.6 (9)C47—C48—C49122.7 (11)
C4—C5—H51119.7C47—C48—H481118.6
C6—C5—H51119.6C49—C48—H481118.7
C5—C6—C1120.2 (9)C48—C49—C50117.8 (13)
C5—C6—H61119.9C48—C49—H491121.1
C1—C6—H61119.8C50—C49—H491121.1
P1—C7—C8121.1 (7)C45—C50—C49121.8 (15)
P1—C7—C12120.8 (6)C45—C50—H501119.1
C8—C7—C12118.0 (8)C49—C50—H501119.1
C7—C8—C9119.9 (10)P4—C39—C40125 (2)
C7—C8—H81120.0P4—C39—C44114 (2)
C9—C8—H81120.1C40—C39—C44120 (3)
C8—C9—C10120.9 (10)C39—C40—C41120 (3)
C8—C9—H91119.6C39—C40—H401120.0
C10—C9—H91119.5C41—C40—H401119.6
C9—C10—C11119.4 (9)C40—C41—C42119 (3)
C9—C10—H101120.3C40—C41—H411120.3
C11—C10—H101120.3C42—C41—H411120.5
C10—C11—C12121.6 (10)C41—C42—C43121 (3)
C10—C11—H111119.2C41—C42—H421119.7
C12—C11—H111119.2C43—C42—H421119.8
C11—C12—C7120.2 (8)C42—C43—C44120 (3)
C11—C12—H121120.0C42—C43—H431120.0
C7—C12—H121119.9C44—C43—H431119.7
P1—C13—P2114.0 (3)C43—C44—C39119 (3)
P1—C13—H131108.4C43—C44—H441120.4
P2—C13—H131108.3C39—C44—H441120.2
P1—C13—H132108.4P4—C89—C90117.3 (9)
P2—C13—H132108.3P4—C89—C94121.7 (10)
H131—C13—H132109.5C90—C89—C94120.9 (13)
P2—C14—C15122.5 (6)C89—C90—C91119.7 (14)
P2—C14—C19119.9 (6)C89—C90—H901120.2
C15—C14—C19117.6 (7)C91—C90—H901120.2
C14—C15—C16120.5 (8)C90—C91—C92119.6 (15)
C14—C15—H151119.3C90—C91—H911120.2
C16—C15—H151120.2C92—C91—H911120.2
C15—C16—C17121.3 (8)C91—C92—C93120.6 (15)
C15—C16—H161118.8C91—C92—H921119.7
C17—C16—H161119.8C93—C92—H921119.7
C16—C17—C18119.0 (9)C92—C93—C94120.0 (14)
C16—C17—H171120.4C92—C93—H931119.9
C18—C17—H171120.6C94—C93—H931120.1
C17—C18—C19121.0 (11)C89—C94—C93119.2 (14)
C17—C18—H181120.4C89—C94—H941120.5
C19—C18—H181118.5C93—C94—H941120.3
Table 1
Bond parameters (Å, °) for the trigold unit of (I)+ in different salts top
Compound(I)[PF6](I)[AuCl(C6F5)3](I)Cl.EtOH(I)[ClO4]
Au1-Au23.1525 (4)3.16453.076 (1)3.0883 (8)
Au2-Au33.2770 (4)3.06633.076 (1)3.1738 (6)
Au1-Au33.1922 (4)3.67843.729 (1)3.4500 (8)
Au2-Au1-Au362.190 (9)72.3574.61 (3)66.85 (2)
Au1-Au2-Au359.499 (9)52.5952.70 (2)57.76 (1)
Au1-Au3-Au258.311 (9)55.0652.70 (2)55.39 (1)
ReferenceThis workUsón et al., 1983Lin et al., 1994Zhang et al., 2005
Table 2
Hydrogen bonds (Å, °) in (I)[PF6] involving [PF6]- anions. Symmetry codes are defined in Fig. 2 top
InteractionD—HH···AD···AD—H···A
C10-H101···F4i0.962.433.22 (1)140
C12-H121···F1ii0.962.423.35 (1)162
C13-H131···F1ii0.962.473.38 (1)159
C15-H151···F6ii0.962.383.29 (1)157
C49-H491···F1iii0.962.563.28 (2)132
C48-H481···F5iii0.962.673.42 (2)136
C46-H461···F30.962.743.42 (2)128
C46-H461···F50.962.683.45 (1)137
C38-H382···F20.962.603.30 (1)129
C31-H311···F20.962.403.26 (1)149
C38-H382···F50.962.703.66 (1)174
C33-H331···F40.962.683.46 (1)135
Acknowledgements top

The authors thank the Swiss National Science Foundation and the University of Basel for financial support.

references
References top

Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435–?.

Betteridge, P. W., Carruthers, J. R., Cooper, R. I., Prout, K. & Watkin, D. J. (2003). J. Appl. Cryst. 36, 1487–?.

Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565–?. [Not cited - may it be removed?]

Larson, A. C. (1970). Crystallographic Computing, edited by F. R. Ahmed, S. R. Hall & C. P. Huber, pp. 291–294. Copenhagen: Munksgaard.

Lin, I. V. B., Hwang, J. M., Feng, D.-F., Cheng, M. C. & Wang, Y. (1994). Inorg. Chem. 33, 3467–3472.

Mendizabal, F., Pyykkö, P. & Runeberg, N. (2003). Chem. Phys. Lett. 370, 733–740.

Nonius (2001). COLLECT. Nonius BV, Delft, The Netherlands.

Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307–326. New York: Academic Press.

Pyykkö, P. (2002). Angew. Chem. Int. Ed. 41, 3573–3578.

Pyykkö, P. (2004). Angew. Chem. Int. Ed. 43, 4412–4456.

Shardlow, E. J. (2007). PhD Thesis, University of Basel.

Usón, R., Laguna, A., Laguna, M., Fernandez, E., Villacampa, M. D., Jones, P. G. & Sheldrick, G. M. (1983). J. Chem. Soc. Dalton Trans. pp. 1679–1685.

Watkin, D. J., Prout, C. K. & Pearce, L. J. (1996). CAMERON. Chemical Crystallography Laboratory, University of Oxford, England.

Zhang, T.-L., Qin, Y. & Meng, X.-G. (2005). Acta Cryst. E61, m2588–m2589.