Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680702421X/bt2371sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680702421X/bt2371Isup2.hkl |
CCDC reference: 650693
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
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).
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).
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.
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.
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).
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.
[Au3Cl2(C25H22P2)2](PF6) | Z = 2 |
Mr = 1575.56 | F(000) = 1488 |
Triclinic, P1 | Dx = 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 |
Nonius KappaCCD diffractometer | 8452 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.026 |
φ and ω scans | θmax = 27.9°, θmin = 1.2° |
Absorption correction: multi-scan DENZO and SCALEPACK (Otwinowski & Minor, 1997) | h = −12→12 |
Tmin = 0.38, Tmax = 0.45 | k = −20→20 |
23737 measured reflections | l = −24→24 |
12197 independent reflections |
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/[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 = 1.11 | Δρmax = 2.95 e Å−3 |
8452 reflections | Δρmin = −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 |
[Au3Cl2(C25H22P2)2](PF6) | γ = 101.6696 (8)° |
Mr = 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)° |
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 = 0.45 | Rint = 0.026 |
23737 measured reflections |
R[F2 > 2σ(F2)] = 0.036 | 144 restraints |
wR(F2) = 0.041 | H-atom parameters constrained |
S = 1.11 | Δρmax = 2.95 e Å−3 |
8452 reflections | Δρmin = −4.06 e Å−3 |
651 parameters |
x | y | z | Uiso*/Ueq | 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* |
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) |
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) |
Mr | 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) |
Tmin, Tmax | 0.38, 0.45 |
No. of measured, independent and observed [I > 3σ(I)] reflections | 23737, 12197, 8452 |
Rint | 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 |
Δρmax, Δρmin (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.
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 |
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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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.