Bis­[μ2-bis­(diphenyl­phosphino)methane]-1:2κ2P:P′;2:3κ2P:P′-dichlorido-1κCl,3κCl-triangulo-trigold(I) hexa­fluoro­phosphate

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

doi:10.1107/S160053680702421X

Bis[μ₂-bis(diphenylphosphino)methane]-1:2κ²P:P′;2:3κ²P:P′-dichlorido-1κCl,3κCl-triangulo-trigold(I) hexafluorophosphate

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

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.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680702421X/bt2371sup1.cif Contains datablocks I, global
	Structure factor file (CIF format) https://doi.org/10.1107/S160053680702421X/bt2371Isup2.hkl Contains datablock I

CCDC reference: 650693

checkCIF report

Key indicators

Single-crystal X-ray study
T = 173 K
Mean (C-C) = 0.015 Å
Disorder in main residue
R factor = 0.036
wR factor = 0.041
Data-to-parameter ratio = 13.0

checkCIF/PLATON results

No syntax errors found



Alert level A
PLAT308_ALERT_2_A Single Bonded Metal Atom (Unusual !) ...........        Au3

Author Response: Atom Au3 is not singly bonded. See bond parameter list.


Alert level B
PLAT220_ALERT_2_B Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       3.64 Ratio
PLAT241_ALERT_2_B Check High      Ueq as Compared to Neighbors for        C18
PLAT241_ALERT_2_B Check High      Ueq as Compared to Neighbors for        C49

Alert level C
PLAT222_ALERT_3_C Large Non-Solvent    H     Ueq(max)/Ueq(min) ...       3.17 Ratio
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for         C5
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for         C9
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for        C22
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        C14
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        C48
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for         P5
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....       2.29
PLAT301_ALERT_3_C Main Residue  Disorder .........................       9.00 Perc.
PLAT342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ...         15

Alert level G
PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints .......        144

   1 ALERT level A = In general: serious problem
   3 ALERT level B = Potentially serious problem
  10 ALERT level C = Check and explain
   1 ALERT level G = General alerts; check

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
  10 ALERT type 2 Indicator that the structure model may be wrong or deficient
   4 ALERT type 3 Indicator that the structure quality may be low
   1 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

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).

Structure description 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).

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

	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.
	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
M_r = 1575.56	F(000) = 1488
Triclinic, P1	D_x = 2.044 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 9.6740 (1) Å	Cell parameters from 12197 reflections
b = 15.4549 (2) Å	θ = 1–28°
c = 18.9003 (3) Å	µ = 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)
Graphite monochromator	R_int = 0.026
φ and ω scans	θ_max = 27.9°, θ_min = 1.2°
Absorption correction: multi-scan DENZO and SCALEPACK (Otwinowski & Minor, 1997)	h = −12→12
T_min = 0.38, T_max = 0.45	k = −20→20
23737 measured reflections	l = −24→24
12197 independent reflections

Refinement top

Refinement on F	Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: full	H-atom parameters constrained
R[F² > 2σ(F²)] = 0.036	Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A₀T₀(x) + A₁T₁(x) ··· + A_n-1]T_n-1(x)] where A_i are the Chebychev coefficients listed below and x = F /Fmax Method = Robust Weighting (Prince, 1982) W = [weight] [1-(deltaF/6sigmaF)²]² A_i 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 = 1.11	Δρ_max = 2.95 e Å⁻³
8452 reflections	Δρ_min = −4.06 e Å⁻³
651 parameters	Extinction correction: Larson (1970), Equation 22
144 restraints	Extinction coefficient: 25 (4)
Primary atom site location: structure-invariant direct methods

Crystal data top

[Au₃Cl₂(C₂₅H₂₂P₂)₂](PF₆)	γ = 101.6696 (8)°
M_r = 1575.56	V = 2559.58 (6) Å³
Triclinic, P1	Z = 2
a = 9.6740 (1) Å	Mo Kα radiation
b = 15.4549 (2) Å	µ = 8.89 mm⁻¹
c = 18.9003 (3) Å	T = 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)
T_min = 0.38, T_max = 0.45	R_int = 0.026
23737 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.036	144 restraints
wR(F²) = 0.041	H-atom parameters constrained
S = 1.11	Δρ_max = 2.95 e Å⁻³
8452 reflections	Δρ_min = −4.06 e Å⁻³
651 parameters

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Au1	0.53079 (3)	0.538005 (18)	0.269126 (16)	0.0384
Au2	0.85524 (3)	0.612438 (19)	0.263223 (16)	0.0381
Au3	0.60667 (3)	0.46319 (3)	0.110429 (16)	0.0481
Cl2	0.9497 (2)	0.48182 (12)	0.24667 (14)	0.0622
Cl3	0.67207 (17)	0.59597 (13)	0.07330 (9)	0.0404
P1	0.47840 (18)	0.67473 (12)	0.26160 (10)	0.0343
P2	0.80771 (18)	0.75229 (12)	0.28655 (10)	0.0345
P3	0.54834 (19)	0.40221 (12)	0.29448 (10)	0.0345
P4	0.5357 (2)	0.32487 (17)	0.12760 (11)	0.0492
P5	0.6289 (3)	0.05910 (16)	0.26952 (18)	0.0699
C1	0.3153 (7)	0.6553 (5)	0.1858 (4)	0.0389
C2	0.3099 (9)	0.6066 (7)	0.1109 (5)	0.0567
C3	0.1877 (10)	0.5902 (8)	0.0515 (5)	0.0658
C4	0.0678 (9)	0.6204 (8)	0.0683 (6)	0.0633
C5	0.0711 (11)	0.6654 (10)	0.1405 (7)	0.0874
C6	0.1937 (10)	0.6830 (8)	0.2002 (6)	0.0708
C7	0.4504 (8)	0.7439 (5)	0.3493 (4)	0.0423
C8	0.4398 (14)	0.7087 (8)	0.4077 (6)	0.0763
C9	0.4172 (17)	0.7641 (11)	0.4753 (7)	0.0966
C10	0.4015 (14)	0.8493 (9)	0.4824 (6)	0.0813
C11	0.4133 (10)	0.8847 (7)	0.4253 (5)	0.0635
C12	0.4375 (9)	0.8335 (6)	0.3588 (4)	0.0482
C13	0.6236 (7)	0.7503 (5)	0.2395 (4)	0.0362
C14	0.8397 (8)	0.8099 (5)	0.3875 (4)	0.0394
C15	0.8084 (8)	0.8944 (5)	0.4164 (5)	0.0474
C16	0.8355 (9)	0.9362 (6)	0.4939 (5)	0.0586
C17	0.8992 (15)	0.8984 (8)	0.5447 (6)	0.0783
C18	0.930 (2)	0.8157 (10)	0.5176 (7)	0.1188
C19	0.9010 (18)	0.7708 (8)	0.4398 (6)	0.0928
C20	0.9235 (8)	0.8334 (5)	0.2544 (4)	0.0394
C21	0.8744 (10)	0.8529 (9)	0.1886 (7)	0.0788
C22	0.9696 (13)	0.9104 (10)	0.1641 (8)	0.0935
C23	1.1131 (11)	0.9483 (7)	0.2048 (7)	0.0700
C24	1.1642 (9)	0.9310 (6)	0.2719 (6)	0.0569
C25	1.0690 (9)	0.8736 (6)	0.2964 (5)	0.0493
C26	0.6729 (8)	0.4262 (5)	0.3875 (4)	0.0445
C27	0.6617 (13)	0.4984 (8)	0.4482 (5)	0.0743
C28	0.7438 (16)	0.5169 (12)	0.5207 (6)	0.1015
C29	0.8367 (15)	0.4635 (12)	0.5355 (6)	0.0980
C30	0.8541 (14)	0.3944 (10)	0.4760 (7)	0.0902
C31	0.7710 (11)	0.3747 (7)	0.4016 (5)	0.0657
C32	0.3757 (8)	0.3331 (5)	0.2981 (4)	0.0377
C33	0.3741 (9)	0.2537 (5)	0.3186 (5)	0.0482
C34	0.2439 (11)	0.1979 (6)	0.3189 (6)	0.0586
C35	0.1145 (10)	0.2204 (6)	0.3007 (6)	0.0607
C36	0.1152 (10)	0.3006 (7)	0.2817 (6)	0.0645
C37	0.2461 (9)	0.3584 (6)	0.2815 (5)	0.0533
C38	0.6086 (8)	0.3223 (5)	0.2235 (4)	0.0405
C45	0.5879 (11)	0.2338 (7)	0.0645 (5)	0.0639
C46	0.6316 (12)	0.1662 (8)	0.0864 (6)	0.0724
C47	0.6587 (16)	0.0918 (8)	0.0301 (9)	0.0979
C48	0.6431 (18)	0.0947 (9)	−0.0425 (8)	0.0984
C49	0.606 (2)	0.1659 (13)	−0.0636 (8)	0.1303
C50	0.5781 (17)	0.2351 (10)	−0.0100 (6)	0.0999
C39	0.344 (4)	0.255 (4)	0.102 (3)	0.0886	0.35 (3)
C40	0.299 (3)	0.165 (3)	0.107 (2)	0.0911	0.35 (3)
C41	0.149 (2)	0.117 (3)	0.085 (2)	0.0986	0.35 (3)
C42	0.045 (3)	0.162 (3)	0.061 (3)	0.1050	0.35 (3)
C43	0.090 (3)	0.252 (3)	0.057 (3)	0.1094	0.35 (3)
C44	0.240 (3)	0.298 (4)	0.076 (3)	0.1023	0.35 (3)
C89	0.3386 (16)	0.2954 (10)	0.1095 (10)	0.0497	0.65 (3)
C90	0.2670 (16)	0.2046 (11)	0.1045 (10)	0.0634	0.65 (3)
C91	0.1153 (16)	0.1797 (14)	0.0948 (11)	0.0816	0.65 (3)
C92	0.0366 (17)	0.2456 (14)	0.0896 (11)	0.0852	0.65 (3)
C93	0.1088 (13)	0.3366 (14)	0.0955 (9)	0.0733	0.65 (3)
C94	0.2601 (13)	0.3617 (13)	0.1047 (8)	0.0579	0.65 (3)
F1	0.5384 (9)	−0.0466 (4)	0.2460 (5)	0.1087
F2	0.7181 (10)	0.1628 (4)	0.2882 (7)	0.1579
F3	0.6891 (10)	0.0284 (6)	0.1969 (5)	0.1189
F4	0.5492 (12)	0.0834 (7)	0.3351 (4)	0.1344
F5	0.4984 (6)	0.0786 (4)	0.2162 (3)	0.0704
F6	0.7605 (10)	0.0398 (6)	0.3212 (6)	0.1499
H21	0.3915	0.5840	0.1005	0.0717*
H31	0.1854	0.5587	−0.0004	0.0781*
H41	−0.0182	0.6086	0.0276	0.0734*
H51	−0.0123	0.6858	0.1510	0.0966*
H61	0.1944	0.7148	0.2517	0.0782*
H81	0.4473	0.6464	0.4026	0.1033*
H91	0.4133	0.7400	0.5168	0.1262*
H101	0.3823	0.8854	0.5277	0.0960*
H111	0.4046	0.9468	0.4311	0.0695*
H121	0.4454	0.8602	0.3191	0.0552*
H131	0.6143	0.8130	0.2550	0.0470*
H132	0.6105	0.7285	0.1852	0.0470*
H151	0.7677	0.9235	0.3816	0.0551*
H161	0.8085	0.9933	0.5123	0.0658*
H171	0.9218	0.9300	0.5990	0.0930*
H181	0.9746	0.7874	0.5524	0.1198*
H191	0.9218	0.7120	0.4214	0.1026*
H211	0.7735	0.8264	0.1595	0.1034*
H221	0.9342	0.9237	0.1182	0.1285*
H231	1.1790	0.9870	0.1869	0.0929*
H241	1.2648	0.9585	0.3012	0.0704*
H251	1.1041	0.8615	0.3429	0.0615*
H271	0.5956	0.5350	0.4385	0.0862*
H281	0.7372	0.5673	0.5617	0.1114*
H291	0.8896	0.4742	0.5872	0.1084*
H301	0.9237	0.3601	0.4862	0.1109*
H311	0.7811	0.3259	0.3604	0.0810*
H331	0.4640	0.2374	0.3325	0.0622*
H341	0.2438	0.1422	0.3322	0.0754*
H351	0.0245	0.1809	0.3010	0.0743*
H361	0.0249	0.3167	0.2685	0.0813*
H371	0.2466	0.4152	0.2700	0.0702*
H381	0.7138	0.3406	0.2363	0.0511*
H382	0.5750	0.2598	0.2243	0.0511*
H401	0.3690	0.1357	0.1249	0.1098*	0.3500
H411	0.1188	0.0558	0.0867	0.1190*	0.3500
H421	−0.0570	0.1309	0.0480	0.1274*	0.3500
H431	0.0196	0.2815	0.0402	0.1340*	0.3500
H441	0.2707	0.3555	0.0685	0.1281*	0.3500
H901	0.3210	0.1603	0.1076	0.0703*	0.6500
H911	0.0659	0.1184	0.0918	0.0888*	0.6500
H921	−0.0671	0.2282	0.0816	0.0984*	0.6500
H931	0.0546	0.3811	0.0930	0.0949*	0.6500
H941	0.3090	0.4226	0.1073	0.0807*	0.6500
H461	0.6447	0.1671	0.1384	0.0874*
H471	0.6869	0.0411	0.0435	0.1149*
H481	0.6592	0.0444	−0.0801	0.1092*
H491	0.5998	0.1677	−0.1146	0.1489*
H501	0.5512	0.2859	−0.0238	0.1136*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Au1	0.04197 (14)	0.03611 (14)	0.04576 (15)	0.01282 (11)	0.01474 (11)	0.02356 (12)
Au2	0.03584 (14)	0.03875 (15)	0.04292 (15)	0.01733 (11)	0.00944 (11)	0.01406 (11)
Au3	0.04596 (16)	0.0768 (2)	0.03611 (15)	0.02721 (14)	0.01776 (12)	0.02902 (14)
Cl2	0.0510 (10)	0.0267 (8)	0.0873 (15)	0.0177 (7)	−0.0229 (10)	0.0101 (9)
Cl3	0.0341 (7)	0.0638 (11)	0.0259 (7)	0.0151 (7)	0.0100 (6)	0.0163 (7)
P1	0.0354 (8)	0.0359 (9)	0.0400 (9)	0.0127 (7)	0.0165 (7)	0.0189 (7)
P2	0.0349 (8)	0.0363 (9)	0.0409 (9)	0.0138 (7)	0.0151 (7)	0.0195 (7)
P3	0.0400 (9)	0.0353 (9)	0.0338 (8)	0.0126 (7)	0.0107 (7)	0.0178 (7)
P4	0.0406 (10)	0.0726 (14)	0.0350 (9)	0.0115 (9)	0.0119 (8)	0.0203 (9)
P5	0.0814 (16)	0.0422 (12)	0.0975 (19)	0.0271 (11)	0.0226 (14)	0.0346 (12)
C1	0.034 (3)	0.038 (4)	0.048 (4)	0.008 (3)	0.014 (3)	0.018 (3)
C2	0.049 (4)	0.085 (6)	0.045 (4)	0.036 (4)	0.017 (4)	0.021 (4)
C3	0.054 (5)	0.102 (8)	0.039 (4)	0.024 (5)	0.012 (4)	0.019 (5)
C4	0.036 (4)	0.086 (7)	0.061 (5)	0.016 (4)	−0.001 (4)	0.025 (5)
C5	0.047 (5)	0.115 (9)	0.080 (7)	0.032 (6)	0.012 (5)	−0.004 (7)
C6	0.042 (4)	0.089 (7)	0.065 (6)	0.022 (5)	0.011 (4)	−0.001 (5)
C7	0.042 (4)	0.043 (4)	0.045 (4)	0.009 (3)	0.020 (3)	0.015 (3)
C8	0.113 (9)	0.079 (7)	0.066 (6)	0.038 (6)	0.056 (6)	0.039 (5)
C9	0.137 (11)	0.115 (10)	0.063 (7)	0.035 (9)	0.063 (7)	0.043 (7)
C10	0.096 (8)	0.090 (8)	0.054 (6)	0.025 (7)	0.035 (6)	0.008 (6)
C11	0.055 (5)	0.068 (6)	0.050 (5)	0.013 (4)	0.015 (4)	−0.004 (4)
C12	0.051 (4)	0.047 (4)	0.039 (4)	0.011 (3)	0.012 (3)	0.005 (3)
C13	0.039 (3)	0.035 (3)	0.043 (4)	0.014 (3)	0.017 (3)	0.020 (3)
C14	0.044 (4)	0.039 (4)	0.045 (4)	0.016 (3)	0.021 (3)	0.020 (3)
C15	0.044 (4)	0.037 (4)	0.055 (5)	0.008 (3)	0.010 (3)	0.010 (3)
C16	0.051 (5)	0.045 (4)	0.065 (6)	0.006 (4)	0.020 (4)	−0.003 (4)
C17	0.122 (9)	0.068 (6)	0.047 (5)	0.021 (6)	0.041 (6)	0.014 (5)
C18	0.25 (2)	0.095 (9)	0.051 (6)	0.098 (11)	0.052 (9)	0.034 (6)
C19	0.180 (13)	0.080 (7)	0.043 (5)	0.079 (8)	0.032 (7)	0.027 (5)
C20	0.038 (3)	0.039 (4)	0.048 (4)	0.014 (3)	0.018 (3)	0.018 (3)
C21	0.049 (5)	0.119 (9)	0.088 (7)	0.011 (5)	0.017 (5)	0.076 (7)
C22	0.066 (6)	0.141 (11)	0.113 (9)	0.023 (7)	0.039 (6)	0.095 (9)
C23	0.059 (5)	0.074 (6)	0.099 (8)	0.012 (5)	0.046 (5)	0.050 (6)
C24	0.050 (4)	0.045 (4)	0.081 (6)	0.011 (4)	0.031 (4)	0.020 (4)
C25	0.048 (4)	0.048 (4)	0.058 (5)	0.017 (3)	0.021 (4)	0.019 (4)
C26	0.049 (4)	0.048 (4)	0.036 (4)	0.006 (3)	0.009 (3)	0.022 (3)
C27	0.089 (7)	0.088 (7)	0.039 (5)	0.026 (6)	0.009 (5)	0.015 (5)
C28	0.096 (9)	0.143 (12)	0.040 (5)	0.009 (9)	0.008 (6)	0.016 (7)
C29	0.088 (8)	0.144 (12)	0.040 (5)	−0.008 (8)	−0.006 (5)	0.041 (7)
C30	0.084 (8)	0.123 (10)	0.070 (7)	0.034 (7)	−0.003 (6)	0.053 (7)
C31	0.067 (6)	0.080 (6)	0.056 (5)	0.023 (5)	0.005 (4)	0.036 (5)
C32	0.047 (4)	0.030 (3)	0.040 (4)	0.009 (3)	0.016 (3)	0.016 (3)
C33	0.058 (5)	0.036 (4)	0.061 (5)	0.018 (3)	0.024 (4)	0.024 (3)
C34	0.080 (6)	0.037 (4)	0.072 (6)	0.016 (4)	0.032 (5)	0.028 (4)
C35	0.060 (5)	0.056 (5)	0.070 (6)	0.005 (4)	0.029 (4)	0.026 (4)
C36	0.048 (5)	0.063 (6)	0.092 (7)	0.019 (4)	0.025 (5)	0.034 (5)
C37	0.047 (4)	0.053 (5)	0.075 (6)	0.020 (4)	0.025 (4)	0.034 (4)
C38	0.042 (4)	0.045 (4)	0.040 (4)	0.015 (3)	0.014 (3)	0.019 (3)
C45	0.070 (6)	0.051 (5)	0.055 (5)	−0.007 (4)	0.028 (4)	0.002 (4)
C46	0.082 (7)	0.069 (6)	0.067 (6)	0.006 (5)	0.047 (5)	0.015 (5)
C47	0.121 (10)	0.050 (6)	0.116 (10)	−0.002 (6)	0.071 (9)	0.007 (6)
C48	0.141 (12)	0.061 (7)	0.073 (8)	0.003 (7)	0.054 (8)	−0.012 (6)
C49	0.204 (19)	0.107 (12)	0.061 (8)	0.023 (12)	0.049 (10)	0.002 (8)
C50	0.139 (12)	0.105 (10)	0.040 (5)	0.023 (8)	0.029 (6)	0.004 (6)
C39	0.048 (13)	0.15 (3)	0.086 (16)	0.002 (14)	0.012 (11)	0.094 (19)
C40	0.045 (12)	0.15 (3)	0.094 (16)	−0.002 (13)	0.012 (11)	0.085 (18)
C41	0.047 (11)	0.16 (3)	0.103 (17)	−0.001 (13)	0.017 (12)	0.082 (19)
C42	0.052 (12)	0.17 (3)	0.109 (18)	0.001 (13)	0.011 (12)	0.091 (19)
C43	0.058 (12)	0.17 (3)	0.114 (19)	0.004 (14)	0.005 (13)	0.10 (2)
C44	0.058 (12)	0.16 (3)	0.106 (18)	0.010 (14)	0.010 (13)	0.10 (2)
C89	0.039 (6)	0.082 (8)	0.037 (6)	0.016 (6)	0.009 (5)	0.034 (7)
C90	0.050 (7)	0.076 (9)	0.048 (7)	−0.002 (7)	0.004 (6)	0.016 (7)
C91	0.055 (8)	0.099 (11)	0.067 (9)	−0.011 (7)	0.012 (7)	0.016 (8)
C92	0.050 (8)	0.132 (13)	0.063 (8)	0.006 (7)	0.013 (7)	0.031 (9)
C93	0.049 (6)	0.132 (13)	0.055 (8)	0.035 (7)	0.013 (6)	0.051 (8)
C94	0.041 (6)	0.123 (11)	0.039 (6)	0.044 (7)	0.019 (5)	0.049 (7)
F1	0.137 (6)	0.053 (3)	0.144 (6)	0.016 (4)	0.046 (5)	0.047 (4)
F2	0.123 (6)	0.054 (4)	0.228 (10)	−0.007 (4)	−0.063 (6)	0.043 (5)
F3	0.121 (6)	0.136 (6)	0.161 (7)	0.074 (5)	0.087 (5)	0.081 (6)
F4	0.206 (9)	0.155 (7)	0.073 (4)	0.103 (7)	0.045 (5)	0.041 (5)
F5	0.076 (3)	0.065 (3)	0.079 (4)	0.023 (3)	0.025 (3)	0.032 (3)
F6	0.141 (7)	0.109 (6)	0.187 (8)	0.051 (5)	−0.030 (6)	0.071 (6)

Geometric parameters (Å, º) top

Au1—Au2	3.1525 (4)	C21—H211	0.960
Au1—Au3	3.1922 (4)	C22—C23	1.363 (16)
Au1—P1	2.3047 (16)	C22—H221	0.959
Au1—P3	2.3083 (16)	C23—C24	1.382 (14)
Au2—Au3	3.2770 (4)	C23—H231	0.961
Au2—Cl2	2.3496 (17)	C24—C25	1.385 (11)
Au2—P2	2.2441 (17)	C24—H241	0.960
Au3—Cl3	2.3560 (18)	C25—H251	0.960
Au3—P4	2.241 (2)	C26—C27	1.403 (13)
P1—C1	1.815 (7)	C26—C31	1.387 (12)
P1—C7	1.812 (7)	C27—C28	1.357 (15)
P1—C13	1.831 (7)	C27—H271	0.959
P2—C13	1.814 (7)	C28—C29	1.38 (2)
P2—C14	1.802 (7)	C28—H281	0.960
P2—C20	1.823 (7)	C29—C30	1.39 (2)
P3—C26	1.814 (7)	C29—H291	0.960
P3—C32	1.817 (7)	C30—C31	1.387 (14)
P3—C38	1.832 (7)	C30—H301	0.960
P4—C38	1.822 (7)	C31—H311	0.960
P4—C45	1.806 (10)	C32—C33	1.382 (9)
P4—C39	1.84 (4)	C32—C37	1.390 (10)
P4—C89	1.806 (15)	C33—C34	1.378 (12)
P5—F1	1.579 (6)	C33—H331	0.960
P5—F2	1.563 (6)	C34—C35	1.369 (13)
P5—F3	1.588 (7)	C34—H341	0.960
P5—F4	1.586 (7)	C35—C36	1.381 (13)
P5—F5	1.584 (5)	C35—H351	0.960
P5—F6	1.574 (6)	C36—C37	1.396 (12)
C1—C2	1.393 (11)	C36—H361	0.960
C1—C6	1.382 (11)	C37—H371	0.960
C2—C3	1.383 (12)	C38—H381	0.960
C2—H21	0.959	C38—H382	0.960
C3—C4	1.395 (13)	C45—C46	1.338 (16)
C3—H31	0.960	C45—C50	1.398 (15)
C4—C5	1.342 (15)	C46—C47	1.443 (15)
C4—H41	0.960	C46—H461	0.960
C5—C6	1.383 (14)	C47—C48	1.36 (2)
C5—H51	0.960	C47—H471	0.960
C6—H61	0.960	C48—C49	1.36 (2)
C7—C8	1.372 (12)	C48—H481	0.960
C7—C12	1.380 (11)	C49—C50	1.37 (2)
C8—C9	1.414 (15)	C49—H491	0.961
C8—H81	0.960	C50—H501	0.960
C9—C10	1.329 (18)	C39—C40	1.403 (10)
C9—H91	0.961	C39—C44	1.402 (10)
C10—C11	1.350 (16)	C40—C41	1.401 (10)
C10—H101	0.960	C40—H401	0.944
C11—C12	1.381 (11)	C41—C42	1.401 (10)
C11—H111	0.959	C41—H411	0.946
C12—H121	0.960	C42—C43	1.401 (10)
C13—H131	0.960	C42—H421	0.958
C13—H132	0.960	C43—C44	1.403 (10)
C14—C15	1.389 (10)	C43—H431	0.946
C14—C19	1.390 (12)	C44—H441	0.937
C15—C16	1.374 (12)	C89—C90	1.401 (9)
C15—H151	0.959	C89—C94	1.404 (9)
C16—C17	1.363 (15)	C90—C91	1.400 (9)
C16—H161	0.964	C90—H901	0.949
C17—C18	1.356 (16)	C91—C92	1.402 (10)
C17—H171	0.965	C91—H911	0.951
C18—C19	1.383 (14)	C92—C93	1.400 (9)
C18—H181	0.964	C92—H921	0.953
C19—H191	0.957	C93—C94	1.399 (9)
C20—C21	1.373 (12)	C93—H931	0.951
C20—C25	1.387 (11)	C94—H941	0.948
C21—C22	1.386 (13)

Au2—Au1—Au3	62.191 (9)	C14—C19—C18	120.5 (9)
Au2—Au1—P1	91.42 (4)	C14—C19—H191	119.2
Au3—Au1—P1	101.01 (4)	C18—C19—H191	120.3
Au2—Au1—P3	99.15 (4)	P2—C20—C21	122.8 (6)
Au3—Au1—P3	90.65 (4)	P2—C20—C25	118.3 (6)
P1—Au1—P3	167.01 (6)	C21—C20—C25	118.9 (7)
Au1—Au2—Au3	59.499 (9)	C20—C21—C22	120.4 (9)
Au1—Au2—Cl2	104.90 (6)	C20—C21—H211	119.8
Au3—Au2—Cl2	79.66 (5)	C22—C21—H211	119.8
Au1—Au2—P2	84.86 (4)	C21—C22—C23	120.4 (10)
Au3—Au2—P2	108.81 (5)	C21—C22—H221	119.8
Cl2—Au2—P2	169.64 (7)	C23—C22—H221	119.8
Au1—Au3—Au2	58.311 (9)	C22—C23—C24	120.1 (8)
Au1—Au3—Cl3	105.39 (4)	C22—C23—H231	120.0
Au2—Au3—Cl3	77.12 (4)	C24—C23—H231	119.9
Au1—Au3—P4	82.19 (5)	C23—C24—C25	119.4 (8)
Au2—Au3—P4	110.30 (5)	C23—C24—H241	120.3
Cl3—Au3—P4	171.67 (7)	C25—C24—H241	120.3
Au1—P1—C1	113.1 (2)	C20—C25—C24	120.7 (8)
Au1—P1—C7	112.9 (2)	C20—C25—H251	119.7
C1—P1—C7	106.5 (3)	C24—C25—H251	119.6
Au1—P1—C13	112.6 (2)	P3—C26—C27	116.6 (7)
C1—P1—C13	104.1 (3)	P3—C26—C31	123.8 (7)
C7—P1—C13	106.9 (3)	C27—C26—C31	119.5 (8)
Au2—P2—C13	115.4 (2)	C26—C27—C28	120.5 (11)
Au2—P2—C14	111.4 (2)	C26—C27—H271	119.8
C13—P2—C14	107.5 (3)	C28—C27—H271	119.7
Au2—P2—C20	113.2 (2)	C27—C28—C29	120.2 (13)
C13—P2—C20	103.1 (3)	C27—C28—H281	120.0
C14—P2—C20	105.5 (3)	C29—C28—H281	119.8
Au1—P3—C26	111.9 (3)	C28—C29—C30	120.2 (10)
Au1—P3—C32	113.3 (2)	C28—C29—H291	119.8
C26—P3—C32	104.4 (3)	C30—C29—H291	120.0
Au1—P3—C38	113.9 (2)	C29—C30—C31	120.1 (11)
C26—P3—C38	107.6 (4)	C29—C30—H301	119.9
C32—P3—C38	105.1 (3)	C31—C30—H301	119.9
Au3—P4—C38	115.6 (3)	C30—C31—C26	119.3 (10)
Au3—P4—C45	112.1 (3)	C30—C31—H311	120.4
C38—P4—C45	105.3 (4)	C26—C31—H311	120.3
Au3—P4—C39	124.8 (11)	P3—C32—C33	118.9 (6)
C38—P4—C39	102.2 (12)	P3—C32—C37	121.7 (5)
C45—P4—C39	93.3 (18)	C33—C32—C37	119.4 (7)
Au3—P4—C89	107.3 (5)	C32—C33—C34	120.2 (7)
C38—P4—C89	106.4 (6)	C32—C33—H331	119.9
C45—P4—C89	110.0 (6)	C34—C33—H331	119.9
F1—P5—F2	176.9 (6)	C33—C34—C35	121.1 (7)
F1—P5—F3	87.3 (5)	C33—C34—H341	119.5
F2—P5—F3	90.0 (7)	C35—C34—H341	119.4
F1—P5—F4	88.3 (5)	C34—C35—C36	119.2 (8)
F2—P5—F4	94.3 (7)	C34—C35—H351	120.4
F3—P5—F4	173.0 (6)	C36—C35—H351	120.4
F1—P5—F5	90.2 (4)	C35—C36—C37	120.6 (8)
F2—P5—F5	88.3 (4)	C35—C36—H361	119.8
F3—P5—F5	87.7 (4)	C37—C36—H361	119.7
F4—P5—F5	86.9 (4)	C36—C37—C32	119.4 (7)
F1—P5—F6	90.2 (5)	C36—C37—H371	120.3
F2—P5—F6	91.3 (5)	C32—C37—H371	120.3
F3—P5—F6	91.1 (6)	P3—C38—P4	111.3 (4)
F4—P5—F6	94.3 (6)	P3—C38—H381	109.0
F5—P5—F6	178.8 (6)	P4—C38—H381	109.0
P1—C1—C2	118.7 (5)	P3—C38—H382	109.0
P1—C1—C6	122.4 (6)	P4—C38—H382	109.0
C2—C1—C6	118.8 (7)	H381—C38—H382	109.5
C1—C2—C3	120.6 (7)	P4—C45—C46	122.4 (7)
C1—C2—H21	119.7	P4—C45—C50	117.2 (10)
C3—C2—H21	119.7	C46—C45—C50	120.4 (10)
C2—C3—C4	118.7 (8)	C45—C46—C47	118.4 (11)
C2—C3—H31	120.6	C45—C46—H461	120.8
C4—C3—H31	120.7	C47—C46—H461	120.8
C3—C4—C5	120.9 (8)	C46—C47—C48	118.8 (13)
C3—C4—H41	119.5	C46—C47—H471	120.6
C5—C4—H41	119.6	C48—C47—H471	120.6
C4—C5—C6	120.6 (9)	C47—C48—C49	122.7 (11)
C4—C5—H51	119.7	C47—C48—H481	118.6
C6—C5—H51	119.6	C49—C48—H481	118.7
C5—C6—C1	120.2 (9)	C48—C49—C50	117.8 (13)
C5—C6—H61	119.9	C48—C49—H491	121.1
C1—C6—H61	119.8	C50—C49—H491	121.1
P1—C7—C8	121.1 (7)	C45—C50—C49	121.8 (15)
P1—C7—C12	120.8 (6)	C45—C50—H501	119.1
C8—C7—C12	118.0 (8)	C49—C50—H501	119.1
C7—C8—C9	119.9 (10)	P4—C39—C40	125 (2)
C7—C8—H81	120.0	P4—C39—C44	114 (2)
C9—C8—H81	120.1	C40—C39—C44	120 (3)
C8—C9—C10	120.9 (10)	C39—C40—C41	120 (3)
C8—C9—H91	119.6	C39—C40—H401	120.0
C10—C9—H91	119.5	C41—C40—H401	119.6
C9—C10—C11	119.4 (9)	C40—C41—C42	119 (3)
C9—C10—H101	120.3	C40—C41—H411	120.3
C11—C10—H101	120.3	C42—C41—H411	120.5
C10—C11—C12	121.6 (10)	C41—C42—C43	121 (3)
C10—C11—H111	119.2	C41—C42—H421	119.7
C12—C11—H111	119.2	C43—C42—H421	119.8
C11—C12—C7	120.2 (8)	C42—C43—C44	120 (3)
C11—C12—H121	120.0	C42—C43—H431	120.0
C7—C12—H121	119.9	C44—C43—H431	119.7
P1—C13—P2	114.0 (3)	C43—C44—C39	119 (3)
P1—C13—H131	108.4	C43—C44—H441	120.4
P2—C13—H131	108.3	C39—C44—H441	120.2
P1—C13—H132	108.4	P4—C89—C90	117.3 (9)
P2—C13—H132	108.3	P4—C89—C94	121.7 (10)
H131—C13—H132	109.5	C90—C89—C94	120.9 (13)
P2—C14—C15	122.5 (6)	C89—C90—C91	119.7 (14)
P2—C14—C19	119.9 (6)	C89—C90—H901	120.2
C15—C14—C19	117.6 (7)	C91—C90—H901	120.2
C14—C15—C16	120.5 (8)	C90—C91—C92	119.6 (15)
C14—C15—H151	119.3	C90—C91—H911	120.2
C16—C15—H151	120.2	C92—C91—H911	120.2
C15—C16—C17	121.3 (8)	C91—C92—C93	120.6 (15)
C15—C16—H161	118.8	C91—C92—H921	119.7
C17—C16—H161	119.8	C93—C92—H921	119.7
C16—C17—C18	119.0 (9)	C92—C93—C94	120.0 (14)
C16—C17—H171	120.4	C92—C93—H931	119.9
C18—C17—H171	120.6	C94—C93—H931	120.1
C17—C18—C19	121.0 (11)	C89—C94—C93	119.2 (14)
C17—C18—H181	120.4	C89—C94—H941	120.5
C19—C18—H181	118.5	C93—C94—H941	120.3

Experimental details

Crystal data
Chemical formula	[Au₃Cl₂(C₂₅H₂₂P₂)₂](PF₆)
M_r	1575.56
Crystal system, space group	Triclinic, P1
Temperature (K)	173
a, b, c (Å)	9.6740 (1), 15.4549 (2), 18.9003 (3)
α, β, γ (°)	105.9872 (8), 101.5928 (7), 101.6696 (8)
V (Å³)	2559.58 (6)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	8.89
Crystal size (mm)	0.11 × 0.09 × 0.09

Data collection
Diffractometer	Nonius KappaCCD
Absorption correction	Multi-scan DENZO and SCALEPACK (Otwinowski & Minor, 1997)
T_min, T_max	0.38, 0.45
No. of measured, independent and observed [I > 3σ(I)] reflections	23737, 12197, 8452
R_int	0.026
(sin θ/λ)_max (Å⁻¹)	0.658

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.036, 0.041, 1.11
No. of reflections	8452
No. of parameters	651
No. of restraints	144
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	2.95, −4.06

Computer programs: COLLECT (Nonius, 2001), DENZO and SCALEPACK (Otwinowski & Minor, 1997), DENZO and SCALEPACK, SIR92 (Altomare et al., 1994), CRYSTALS (Betteridge et al., 2003), CAMERON (Watkin et al., 1996), CRYSTALS.

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-Au2	3.1525 (4)	3.1645	3.076 (1)	3.0883 (8)
Au2-Au3	3.2770 (4)	3.0663	3.076 (1)	3.1738 (6)
Au1-Au3	3.1922 (4)	3.6784	3.729 (1)	3.4500 (8)
Au2-Au1-Au3	62.190 (9)	72.35	74.61 (3)	66.85 (2)
Au1-Au2-Au3	59.499 (9)	52.59	52.70 (2)	57.76 (1)
Au1-Au3-Au2	58.311 (9)	55.06	52.70 (2)	55.39 (1)
Reference	This work	Usón et al., 1983	Lin et al., 1994	Zhang et al., 2005

Hydrogen bonds (Å, °) in (I)[PF₆] involving [PF₆]^- anions. Symmetry codes are defined in Fig. 2 top

Interaction	D—H	H···A	D···A	D—H···A
C10-H101···F4ⁱ	0.96	2.43	3.22 (1)	140
C12-H121···F1ⁱⁱ	0.96	2.42	3.35 (1)	162
C13-H131···F1ⁱⁱ	0.96	2.47	3.38 (1)	159
C15-H151···F6ⁱⁱ	0.96	2.38	3.29 (1)	157
C49-H491···F1ⁱⁱⁱ	0.96	2.56	3.28 (2)	132
C48-H481···F5ⁱⁱⁱ	0.96	2.67	3.42 (2)	136
C46-H461···F3	0.96	2.74	3.42 (2)	128
C46-H461···F5	0.96	2.68	3.45 (1)	137
C38-H382···F2	0.96	2.60	3.30 (1)	129
C31-H311···F2	0.96	2.40	3.26 (1)	149
C38-H382···F5	0.96	2.70	3.66 (1)	174
C33-H331···F4	0.96	2.68	3.46 (1)	135

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Bis­[μ2-bis­(diphenyl­phosphino)methane]-1:2κ2P:P′;2:3κ2P:P′-dichlorido-1κCl,3κCl-triangulo-trigold(I) hexa­fluoro­phosphate

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Bis[μ₂-bis(diphenylphosphino)methane]-1:2κ²P:P′;2:3κ²P:P′-dichlorido-1κCl,3κCl-triangulo-trigold(I) hexafluorophosphate