supplementary materials


ya2134 scheme

Acta Cryst. (2011). E67, m150-m151    [ doi:10.1107/S1600536810054115 ]

[[mu]2-Bis(diphenylphosphanyl)methane][[mu]3-bis(diphenylphosphanyl)methyl]trichloridotetragold(I) tetrahydrofuran disolvate

H.-H. Wang, Q. Gao, Y. Cui, L. Wang and Y.-B. Xie

Abstract top

The title tetranuclear complex, [Au4(C25H21P2)Cl3(C25H22P2)]·2C4H8O, features two non-equivalent Ph2PCPPh2 fragments, one of which represents the `complete' molecule (with two H atoms at the central C atom); each of the two P atoms of this molecule is coordinated by an Au atom [Au-P = 2.2256 (13) and 2.2710 (13) Å], and these two Au atoms form an Au-Au bond [3.2945 (3) Å], thus closing the five-membered Au2P2C ring. The first of these Au atoms has a terminal chlorido ligand [Au-Cl = 2.2806 (12) Å], whereas the second Au atom forms a covalent bond with the central C atom of the bis(diphenylphosphino)methyl group [Au-C = 2.114 (5) Å]; the latter group in turn coordinates with its P atoms the gold atoms of the Cl-Au-Au-Cl group [Au-P = 2.2356 (13) and 2.2338 (13), Au-Au = 3.3177 (3), Au-Cl = 2.3091 (12) and 2.2950 (13) Å], thus closing the second Au2P2C ring. The two such rings have different chemical functions, but both exhibit envelope conformations. However, the first (with different substituents at the Au atoms) is non-symmetrical with one of the P atoms in the flap position of the envelope; the other one has a conformation with mirror symmetry, and the gold-substituted C atom is displaced by 0.740 (5) Å from the almost exactly planar (r.m.s. deviation = 0.0038 Å) Au2P2 group.

Comment top

The crystal structures of Au compounds with the bis(diphenylphosphanyl)methane ligand have been widely studied (see, for instance, Bruce et al., 2006; Feng et al., 1997; Sevillano et al., 2007). Herein, we report the bis(tetrahydrofurane) solvate of a new tetranuclear complex with this ligand and a rather peculiar non-symmetrical structure.

The molecule of the title compound, (Fig. 1) features two chemically different fragments derived from bis(diphenylphosphanyl)methane, one of which represents neutral molecule coordinated to two gold atoms through each of its P atoms [Au3-P3 2.2710 (13), Au4-P4 2.2256 (13) Å]. These gold atoms are bonded to each other [Au3-Au4 3.2945 (3) Å] thus closing the Au2P2C-ring. The Au4 atom also has a terminal chloro ligand [Au4-Cl4 2.2806 (12) Å], whereas the Au3 atom is bonded to the C13 atom belonging to the bis(diphenylphosphanyl)methyl group [Au3-C13 2.114 (5) Å], which in its turn has each of its phosphorus atoms P1 and P2 bonded to gold atoms of the Cl1-Au1-Au2-Cl2 fragment [Au1-P1 2.2356 (13) Å, Au2-P2 2.2338 (13) Å, Au1-Au2 3.3177 (3) Å, Au1-Cl1 2.3091 (12) Å, Au2-Cl2 2.2950 (13) Å], thus closing the second five-membered ring. Both five-memebered Au2P2C rings have envelope conformations, however the conformation of symmetrically substituted ring with Au1 and Au2 atoms has a mirror symmetry [displacement of the C13 atom from the almost exactly planar Au2P2 group being 0.740 (5) Å], whereas the second five-membered ring is not symmetrical with one of the phosphorus atoms (P3) in the flap position, its displacement from the plane of the rest of the atoms in this ring being 0.889 (1) Å.

Related literature top

For the structures of related gold complexes with bis(diphenylphosphanyl)methane ligands, see: Bruce et al. (2006); Feng et al. (1997); Sevillano et al. (2007).

Experimental top

A solution of AuCl (0.1 mmol, 23.5 mg) in 1 ml of H2O and bis(diphenylphosphanyl)methane (0.2 mmol, 77 mg) in 1 ml of THF were mixed and sealed in a 4 ml glass vial and kept at 333 K for 2 days. Then the mixture was cooled down to room temperature and was allowed to stand. After 5 days, colorless crystals suitable for the X-ray diffraction experiment were collected.

Refinement top

All H atoms were placed geometrically (C-H 0.95 Å and 0.99 Å for aromatic and methylene H atoms respectively) and treated as riding with Uiso(H) = 1.2Ueq(C). There are four residual peaks higher than 1 eÅ-3, each one in the vicinity of each of the Au atom at the distances of 0.881-0.991 Å.

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The molecular structure of the title compound with displacement ellipsoids drawn at the 30% probability level; hydrogen atoms are omitted.
2-Bis(diphenylphosphanyl)methane][µ3-bis(diphenylphosphanyl)methyl]\ trichloridotetragold(I) tetrahydrofuran disolvate top
Crystal data top
[Au4(C25H21P2)Cl3(C25H22P2)]·2C4H8OF(000) = 3400
Mr = 1806.15Dx = 2.088 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 9747 reflections
a = 14.9822 (6) Åθ = 2.3–28.3°
b = 14.6274 (6) ŵ = 10.47 mm1
c = 27.1356 (10) ÅT = 100 K
β = 104.981 (1)°Block, colorless
V = 5744.7 (4) Å30.22 × 0.20 × 0.18 mm
Z = 4
Data collection top
Bruker SMART CCD area-detector
diffractometer
10683 independent reflections
Radiation source: fine-focus sealed tube9041 reflections with I > 2σ(I)
graphiteRint = 0.034
phi and ω scansθmax = 25.5°, θmin = 1.4°
Absorption correction: multi-scan
(SADABS; Bruker, 1998)
h = 1815
Tmin = 0.115, Tmax = 0.152k = 1716
31460 measured reflectionsl = 3232
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.027Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.058H-atom parameters constrained
S = 0.99 w = 1/[σ2(Fo2) + (0.0278P)2]
where P = (Fo2 + 2Fc2)/3
10683 reflections(Δ/σ)max = 0.002
640 parametersΔρmax = 1.32 e Å3
0 restraintsΔρmin = 0.61 e Å3
Crystal data top
[Au4(C25H21P2)Cl3(C25H22P2)]·2C4H8OV = 5744.7 (4) Å3
Mr = 1806.15Z = 4
Monoclinic, P21/nMo Kα radiation
a = 14.9822 (6) ŵ = 10.47 mm1
b = 14.6274 (6) ÅT = 100 K
c = 27.1356 (10) Å0.22 × 0.20 × 0.18 mm
β = 104.981 (1)°
Data collection top
Bruker SMART CCD area-detector
diffractometer
10683 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 1998)
9041 reflections with I > 2σ(I)
Tmin = 0.115, Tmax = 0.152Rint = 0.034
31460 measured reflectionsθmax = 25.5°
Refinement top
R[F2 > 2σ(F2)] = 0.027H-atom parameters constrained
wR(F2) = 0.058Δρmax = 1.32 e Å3
S = 0.99Δρmin = 0.61 e Å3
10683 reflectionsAbsolute structure: ?
640 parametersFlack parameter: ?
0 restraintsRogers parameter: ?
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2sigma(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Au10.821477 (13)0.165214 (13)0.399909 (7)0.01754 (5)
Au20.729665 (13)0.371899 (13)0.398530 (7)0.01955 (5)
Au30.830843 (12)0.267477 (13)0.528113 (7)0.01567 (5)
Au40.821891 (13)0.276224 (13)0.648058 (8)0.01946 (5)
Cl10.92100 (8)0.18934 (9)0.34889 (5)0.0225 (3)
Cl20.80684 (10)0.44543 (10)0.34719 (5)0.0330 (3)
Cl40.70061 (9)0.17746 (9)0.63746 (5)0.0295 (3)
P10.73048 (9)0.12581 (9)0.45001 (5)0.0168 (3)
P20.64608 (9)0.31387 (9)0.44833 (5)0.0175 (3)
P30.97673 (9)0.31433 (9)0.56659 (5)0.0161 (3)
P40.93872 (9)0.37510 (9)0.66646 (5)0.0167 (3)
O10.4371 (3)0.2321 (3)0.54344 (19)0.0568 (13)
O20.4516 (4)0.4614 (3)0.26736 (19)0.0697 (16)
C10.6251 (3)0.0689 (3)0.41479 (18)0.0180 (11)
C20.5989 (4)0.0764 (4)0.3627 (2)0.0346 (15)
H2A0.63670.10850.34540.041*
C30.5162 (4)0.0368 (5)0.3354 (2)0.0451 (18)
H3A0.49680.04390.29940.054*
C40.4635 (4)0.0115 (4)0.3596 (2)0.0356 (15)
H4A0.40770.03900.34060.043*
C50.4906 (4)0.0209 (4)0.4121 (2)0.0335 (14)
H5A0.45410.05560.42910.040*
C60.5703 (4)0.0200 (4)0.4393 (2)0.0277 (13)
H6A0.58820.01470.47540.033*
C70.8515 (4)0.0167 (4)0.4873 (2)0.0282 (13)
H7A0.86880.01100.45620.034*
C80.8916 (4)0.0829 (4)0.5219 (2)0.0406 (16)
H8A0.93590.12310.51430.049*
C90.8682 (4)0.0914 (4)0.5676 (2)0.0323 (14)
H9A0.89610.13760.59120.039*
C100.8047 (4)0.0332 (4)0.5790 (2)0.0304 (13)
H10A0.78890.03900.61050.036*
C110.7632 (4)0.0346 (3)0.54457 (19)0.0228 (12)
H11A0.71990.07560.55270.027*
C120.7862 (3)0.0416 (3)0.49766 (18)0.0190 (11)
C130.7005 (3)0.2186 (3)0.48621 (18)0.0150 (10)
H13A0.66280.19670.50940.018*
C140.5300 (3)0.2836 (3)0.4117 (2)0.0230 (12)
C150.4999 (4)0.3097 (4)0.3611 (2)0.0353 (15)
H15A0.53990.34310.34560.042*
C160.4112 (4)0.2871 (5)0.3327 (3)0.0431 (17)
H16A0.39000.30580.29820.052*
C170.3556 (5)0.2382 (5)0.3550 (3)0.0507 (19)
H17A0.29500.22330.33550.061*
C180.3839 (4)0.2096 (4)0.4047 (3)0.0422 (17)
H18A0.34420.17360.41910.051*
C190.4719 (4)0.2338 (4)0.4341 (3)0.0336 (14)
H19A0.49170.21640.46890.040*
C200.6101 (3)0.4881 (3)0.4785 (2)0.0230 (12)
H20A0.60030.50290.44340.028*
C210.6037 (4)0.5561 (4)0.5126 (2)0.0282 (13)
H21A0.58840.61680.50090.034*
C220.6198 (3)0.5354 (4)0.5637 (2)0.0280 (13)
H22A0.61850.58240.58760.034*
C230.6378 (4)0.4463 (4)0.5800 (2)0.0303 (13)
H23A0.64700.43220.61520.036*
C240.6427 (3)0.3773 (4)0.5459 (2)0.0233 (12)
H24A0.65420.31600.55740.028*
C250.6304 (3)0.3988 (3)0.49429 (19)0.0190 (11)
C261.0386 (3)0.3562 (3)0.52206 (19)0.0171 (11)
C271.0185 (4)0.3184 (3)0.47360 (19)0.0215 (12)
H27A0.96940.27570.46380.026*
C281.0685 (4)0.3417 (4)0.4394 (2)0.0246 (12)
H28A1.05380.31520.40630.030*
C291.1403 (3)0.4036 (4)0.4535 (2)0.0236 (12)
H29A1.17670.41830.43060.028*
C301.1587 (4)0.4440 (4)0.5008 (2)0.0287 (13)
H30A1.20640.48830.51000.034*
C311.1088 (4)0.4211 (4)0.5351 (2)0.0271 (13)
H31A1.12220.44960.56770.033*
C321.1373 (4)0.2379 (4)0.6298 (2)0.0248 (12)
H32A1.16350.29730.63070.030*
C331.1891 (4)0.1670 (4)0.6566 (2)0.0280 (13)
H33A1.25020.17800.67650.034*
C341.1521 (4)0.0800 (4)0.6544 (2)0.0280 (13)
H34A1.18830.03150.67250.034*
C351.0638 (4)0.0636 (3)0.6265 (2)0.0266 (13)
H35A1.03880.00370.62510.032*
C361.0102 (4)0.1348 (3)0.59980 (19)0.0207 (11)
H36A0.94860.12350.58050.025*
C371.0472 (3)0.2224 (3)0.60168 (19)0.0186 (11)
C380.9833 (3)0.4068 (3)0.61248 (18)0.0163 (11)
H38A1.04850.42600.62530.020*
H38B0.94780.45980.59490.020*
C390.9083 (3)0.4827 (3)0.69037 (18)0.0182 (11)
C400.9591 (3)0.5624 (3)0.68955 (19)0.0211 (11)
H40A1.01000.56190.67470.025*
C410.9355 (4)0.6418 (4)0.7103 (2)0.0272 (13)
H41A0.97080.69560.71000.033*
C420.8605 (4)0.6442 (4)0.7316 (2)0.0303 (13)
H42A0.84450.69920.74580.036*
C430.8097 (4)0.5655 (4)0.7319 (2)0.0303 (13)
H43A0.75830.56660.74630.036*
C440.8327 (3)0.4859 (4)0.71156 (19)0.0228 (12)
H44A0.79700.43240.71190.027*
C451.0375 (4)0.2417 (4)0.73054 (19)0.0224 (12)
H45A0.98160.20760.72150.027*
C461.1162 (4)0.2022 (4)0.76134 (19)0.0245 (12)
H46A1.11500.14120.77320.029*
C471.1964 (4)0.2527 (3)0.77444 (19)0.0235 (12)
H47A1.25110.22580.79510.028*
C481.1986 (4)0.3414 (4)0.75816 (19)0.0243 (12)
H48A1.25440.37550.76800.029*
C491.1199 (3)0.3813 (4)0.72746 (19)0.0199 (11)
H49A1.12090.44290.71650.024*
C501.0389 (3)0.3297 (3)0.71279 (18)0.0162 (11)
C510.4491 (5)0.2656 (5)0.5949 (3)0.054 (2)
H51A0.48900.32060.60080.065*
H51B0.47800.21820.62000.065*
C520.3534 (5)0.2887 (6)0.5999 (3)0.070 (3)
H52A0.34900.28310.63560.084*
H52B0.33380.35080.58700.084*
C530.2995 (6)0.2156 (7)0.5663 (3)0.077 (3)
H53A0.30360.15700.58510.093*
H53B0.23370.23320.55400.093*
C540.3414 (5)0.2074 (5)0.5243 (3)0.058 (2)
H54A0.33600.14390.51120.069*
H54B0.31060.24880.49610.069*
C550.4912 (7)0.5337 (6)0.3012 (3)0.080 (3)
H55A0.55920.53380.30700.096*
H55B0.47660.52550.33440.096*
C560.4515 (8)0.6222 (6)0.2772 (3)0.112 (4)
H56A0.50110.66500.27440.134*
H56B0.41280.65150.29720.134*
C570.3939 (5)0.5940 (5)0.2249 (3)0.0517 (18)
H57A0.32720.59450.22350.062*
H57B0.40490.63500.19810.062*
C580.4262 (6)0.5006 (5)0.2190 (3)0.058 (2)
H58A0.37630.46450.19630.070*
H58B0.47970.50230.20400.070*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Au10.01512 (11)0.01976 (11)0.01662 (11)0.00144 (8)0.00206 (8)0.00055 (8)
Au20.02057 (11)0.01999 (11)0.01713 (11)0.00422 (8)0.00314 (9)0.00074 (8)
Au30.01249 (10)0.01809 (10)0.01494 (11)0.00262 (7)0.00085 (8)0.00149 (7)
Au40.01640 (11)0.02231 (11)0.01836 (11)0.00511 (8)0.00215 (9)0.00039 (8)
Cl10.0166 (7)0.0295 (7)0.0206 (7)0.0000 (5)0.0035 (5)0.0009 (5)
Cl20.0441 (9)0.0331 (8)0.0253 (8)0.0208 (6)0.0152 (7)0.0065 (6)
Cl40.0243 (7)0.0347 (8)0.0292 (8)0.0154 (6)0.0063 (6)0.0004 (6)
P10.0166 (7)0.0174 (7)0.0146 (7)0.0021 (5)0.0011 (6)0.0001 (5)
P20.0131 (7)0.0199 (7)0.0173 (7)0.0013 (5)0.0003 (6)0.0008 (5)
P30.0141 (7)0.0179 (7)0.0154 (7)0.0029 (5)0.0022 (6)0.0009 (5)
P40.0156 (7)0.0178 (7)0.0151 (7)0.0014 (5)0.0010 (6)0.0008 (5)
O10.053 (3)0.062 (3)0.057 (3)0.003 (2)0.017 (3)0.002 (3)
O20.115 (5)0.045 (3)0.049 (3)0.027 (3)0.019 (3)0.008 (3)
C10.020 (3)0.015 (3)0.016 (3)0.003 (2)0.000 (2)0.001 (2)
C20.034 (4)0.048 (4)0.019 (3)0.026 (3)0.002 (3)0.006 (3)
C30.049 (4)0.063 (5)0.017 (3)0.029 (3)0.003 (3)0.000 (3)
C40.027 (3)0.046 (4)0.028 (3)0.023 (3)0.003 (3)0.001 (3)
C50.033 (4)0.039 (4)0.029 (3)0.018 (3)0.010 (3)0.001 (3)
C60.026 (3)0.037 (3)0.016 (3)0.011 (3)0.002 (2)0.001 (2)
C70.034 (3)0.027 (3)0.022 (3)0.007 (2)0.004 (3)0.001 (2)
C80.039 (4)0.037 (4)0.041 (4)0.019 (3)0.002 (3)0.002 (3)
C90.033 (4)0.023 (3)0.032 (3)0.002 (3)0.008 (3)0.010 (3)
C100.034 (3)0.027 (3)0.026 (3)0.005 (3)0.000 (3)0.005 (2)
C110.021 (3)0.019 (3)0.023 (3)0.004 (2)0.002 (2)0.000 (2)
C120.019 (3)0.020 (3)0.014 (3)0.004 (2)0.002 (2)0.001 (2)
C130.008 (2)0.022 (3)0.013 (3)0.0027 (19)0.001 (2)0.000 (2)
C140.017 (3)0.018 (3)0.031 (3)0.003 (2)0.000 (2)0.002 (2)
C150.026 (3)0.048 (4)0.027 (3)0.006 (3)0.000 (3)0.010 (3)
C160.023 (3)0.058 (5)0.041 (4)0.005 (3)0.005 (3)0.010 (3)
C170.028 (4)0.042 (4)0.065 (5)0.003 (3)0.020 (4)0.010 (4)
C180.027 (4)0.033 (4)0.062 (5)0.012 (3)0.002 (3)0.004 (3)
C190.019 (3)0.025 (3)0.051 (4)0.000 (2)0.000 (3)0.000 (3)
C200.017 (3)0.023 (3)0.029 (3)0.000 (2)0.007 (2)0.000 (2)
C210.021 (3)0.024 (3)0.041 (4)0.002 (2)0.010 (3)0.000 (3)
C220.014 (3)0.034 (3)0.034 (3)0.002 (2)0.003 (3)0.014 (3)
C230.022 (3)0.045 (4)0.023 (3)0.007 (3)0.004 (3)0.006 (3)
C240.017 (3)0.026 (3)0.026 (3)0.003 (2)0.004 (2)0.002 (2)
C250.011 (3)0.022 (3)0.023 (3)0.006 (2)0.003 (2)0.003 (2)
C260.017 (3)0.016 (3)0.017 (3)0.005 (2)0.002 (2)0.004 (2)
C270.022 (3)0.020 (3)0.023 (3)0.004 (2)0.005 (2)0.003 (2)
C280.029 (3)0.024 (3)0.020 (3)0.002 (2)0.005 (3)0.004 (2)
C290.017 (3)0.030 (3)0.025 (3)0.005 (2)0.007 (2)0.006 (2)
C300.022 (3)0.034 (3)0.030 (3)0.009 (2)0.006 (3)0.005 (3)
C310.019 (3)0.040 (3)0.021 (3)0.011 (2)0.003 (2)0.007 (3)
C320.020 (3)0.026 (3)0.026 (3)0.004 (2)0.001 (2)0.006 (2)
C330.015 (3)0.034 (3)0.030 (3)0.005 (2)0.003 (3)0.003 (3)
C340.032 (3)0.027 (3)0.025 (3)0.011 (2)0.008 (3)0.003 (2)
C350.037 (4)0.014 (3)0.029 (3)0.000 (2)0.008 (3)0.002 (2)
C360.024 (3)0.019 (3)0.019 (3)0.002 (2)0.005 (2)0.003 (2)
C370.017 (3)0.020 (3)0.017 (3)0.002 (2)0.001 (2)0.002 (2)
C380.015 (3)0.016 (3)0.018 (3)0.002 (2)0.004 (2)0.002 (2)
C390.019 (3)0.019 (3)0.015 (3)0.004 (2)0.001 (2)0.002 (2)
C400.021 (3)0.023 (3)0.019 (3)0.002 (2)0.004 (2)0.003 (2)
C410.027 (3)0.019 (3)0.033 (3)0.004 (2)0.005 (3)0.001 (2)
C420.030 (3)0.032 (3)0.029 (3)0.007 (3)0.008 (3)0.005 (3)
C430.031 (3)0.036 (4)0.025 (3)0.006 (3)0.009 (3)0.000 (3)
C440.018 (3)0.029 (3)0.021 (3)0.002 (2)0.005 (2)0.001 (2)
C450.025 (3)0.026 (3)0.016 (3)0.004 (2)0.007 (2)0.001 (2)
C460.030 (3)0.024 (3)0.017 (3)0.005 (2)0.001 (2)0.005 (2)
C470.027 (3)0.024 (3)0.015 (3)0.005 (2)0.002 (2)0.001 (2)
C480.020 (3)0.031 (3)0.018 (3)0.005 (2)0.001 (2)0.003 (2)
C490.019 (3)0.022 (3)0.016 (3)0.005 (2)0.001 (2)0.001 (2)
C500.017 (3)0.021 (3)0.009 (2)0.001 (2)0.000 (2)0.000 (2)
C510.050 (5)0.074 (6)0.043 (4)0.007 (4)0.017 (4)0.006 (4)
C520.051 (5)0.098 (7)0.073 (6)0.031 (4)0.037 (5)0.020 (5)
C530.077 (6)0.105 (8)0.061 (6)0.028 (5)0.036 (5)0.040 (5)
C540.048 (5)0.053 (5)0.075 (6)0.017 (4)0.022 (4)0.008 (4)
C550.115 (8)0.070 (6)0.045 (5)0.032 (5)0.002 (5)0.000 (4)
C560.195 (12)0.051 (6)0.057 (6)0.022 (6)0.025 (7)0.005 (4)
C570.062 (5)0.041 (4)0.050 (5)0.001 (3)0.011 (4)0.009 (3)
C580.078 (6)0.055 (5)0.043 (5)0.014 (4)0.019 (4)0.003 (4)
Geometric parameters (Å, °) top
Au1—P12.2356 (13)C24—H24A0.9500
Au1—Cl12.3091 (12)C26—C271.386 (7)
Au1—Au23.3177 (3)C26—C311.393 (7)
Au2—P22.2338 (13)C27—C281.378 (7)
Au2—Cl22.2950 (13)C27—H27A0.9500
Au3—C132.114 (5)C28—C291.382 (7)
Au3—P32.2710 (13)C28—H28A0.9500
Au3—Au43.2945 (3)C29—C301.375 (7)
Au4—P42.2256 (13)C29—H29A0.9500
Au4—Cl42.2806 (12)C30—C311.377 (7)
P1—C131.800 (5)C30—H30A0.9500
P1—C11.822 (5)C31—H31A0.9500
P1—C121.825 (5)C32—C331.384 (7)
P2—C131.797 (5)C32—C371.387 (7)
P2—C251.818 (5)C32—H32A0.9500
P2—C141.820 (5)C33—C341.382 (8)
P3—C261.809 (5)C33—H33A0.9500
P3—C371.819 (5)C34—C351.366 (7)
P3—C381.823 (5)C34—H34A0.9500
P4—C391.805 (5)C35—C361.397 (7)
P4—C501.816 (5)C35—H35A0.9500
P4—C381.820 (5)C36—C371.393 (7)
O1—C541.439 (8)C36—H36A0.9500
O1—C511.447 (8)C38—H38A0.9900
O2—C581.391 (8)C38—H38B0.9900
O2—C551.424 (9)C39—C401.396 (7)
C1—C21.369 (7)C39—C441.397 (7)
C1—C61.381 (7)C40—C411.376 (7)
C2—C31.394 (8)C40—H40A0.9500
C2—H2A0.9500C41—C421.391 (8)
C3—C41.351 (8)C41—H41A0.9500
C3—H3A0.9500C42—C431.381 (8)
C4—C51.382 (8)C42—H42A0.9500
C4—H4A0.9500C43—C441.371 (7)
C5—C61.369 (7)C43—H43A0.9500
C5—H5A0.9500C44—H44A0.9500
C6—H6A0.9500C45—C501.377 (7)
C7—C81.374 (8)C45—C461.384 (7)
C7—C121.379 (7)C45—H45A0.9500
C7—H7A0.9500C46—C471.377 (7)
C8—C91.379 (8)C46—H46A0.9500
C8—H8A0.9500C47—C481.373 (7)
C9—C101.370 (8)C47—H47A0.9500
C9—H9A0.9500C48—C491.385 (7)
C10—C111.393 (7)C48—H48A0.9500
C10—H10A0.9500C49—C501.396 (7)
C11—C121.405 (7)C49—H49A0.9500
C11—H11A0.9500C51—C521.513 (9)
C13—H13A1.0000C51—H51A0.9900
C14—C151.385 (8)C51—H51B0.9900
C14—C191.389 (7)C52—C531.499 (10)
C15—C161.392 (8)C52—H52A0.9900
C15—H15A0.9500C52—H52B0.9900
C16—C171.352 (9)C53—C541.443 (9)
C16—H16A0.9500C53—H53A0.9900
C17—C181.371 (9)C53—H53B0.9900
C17—H17A0.9500C54—H54A0.9900
C18—C191.399 (8)C54—H54B0.9900
C18—H18A0.9500C55—C561.501 (11)
C19—H19A0.9500C55—H55A0.9900
C20—C211.378 (7)C55—H55B0.9900
C20—C251.384 (7)C56—C571.514 (10)
C20—H20A0.9500C56—H56A0.9900
C21—C221.378 (8)C56—H56B0.9900
C21—H21A0.9500C57—C581.472 (9)
C22—C231.380 (8)C57—H57A0.9900
C22—H22A0.9500C57—H57B0.9900
C23—C241.385 (7)C58—H58A0.9900
C23—H23A0.9500C58—H58B0.9900
C24—C251.401 (7)
P1—Au1—Cl1173.66 (5)C26—C27—H27A119.4
P1—Au1—Au285.73 (3)C27—C28—C29119.6 (5)
Cl1—Au1—Au2100.61 (3)C27—C28—H28A120.2
P2—Au2—Cl2173.98 (5)C29—C28—H28A120.2
P2—Au2—Au186.70 (3)C30—C29—C28119.6 (5)
Cl2—Au2—Au199.29 (4)C30—C29—H29A120.2
C13—Au3—P3174.14 (13)C28—C29—H29A120.2
C13—Au3—Au4106.05 (13)C29—C30—C31121.0 (5)
P3—Au3—Au479.29 (3)C29—C30—H30A119.5
P4—Au4—Cl4174.11 (5)C31—C30—H30A119.5
P4—Au4—Au390.94 (3)C30—C31—C26120.0 (5)
Cl4—Au4—Au394.90 (3)C30—C31—H31A120.0
C13—P1—C1109.0 (2)C26—C31—H31A120.0
C13—P1—C12104.8 (2)C33—C32—C37120.0 (5)
C1—P1—C12103.8 (2)C33—C32—H32A120.0
C13—P1—Au1114.53 (16)C37—C32—H32A120.0
C1—P1—Au1112.38 (16)C34—C33—C32120.3 (5)
C12—P1—Au1111.48 (17)C34—C33—H33A119.9
C13—P2—C25104.9 (2)C32—C33—H33A119.9
C13—P2—C14110.6 (2)C35—C34—C33120.3 (5)
C25—P2—C14105.4 (2)C35—C34—H34A119.8
C13—P2—Au2113.49 (16)C33—C34—H34A119.8
C25—P2—Au2110.31 (16)C34—C35—C36120.1 (5)
C14—P2—Au2111.61 (18)C34—C35—H35A120.0
C26—P3—C37105.7 (2)C36—C35—H35A120.0
C26—P3—C38105.0 (2)C37—C36—C35119.8 (5)
C37—P3—C38105.6 (2)C37—C36—H36A120.1
C26—P3—Au3113.18 (17)C35—C36—H36A120.1
C37—P3—Au3112.17 (17)C32—C37—C36119.5 (5)
C38—P3—Au3114.40 (16)C32—C37—P3121.2 (4)
C39—P4—C50108.1 (2)C36—C37—P3119.3 (4)
C39—P4—C38104.3 (2)P4—C38—P3113.3 (3)
C50—P4—C38104.0 (2)P4—C38—H38A108.9
C39—P4—Au4112.97 (17)P3—C38—H38A108.9
C50—P4—Au4112.27 (16)P4—C38—H38B108.9
C38—P4—Au4114.55 (16)P3—C38—H38B108.9
C54—O1—C51107.4 (5)H38A—C38—H38B107.7
C58—O2—C55105.6 (6)C40—C39—C44118.8 (5)
C2—C1—C6119.4 (5)C40—C39—P4122.2 (4)
C2—C1—P1118.9 (4)C44—C39—P4119.0 (4)
C6—C1—P1121.7 (4)C41—C40—C39119.9 (5)
C1—C2—C3119.6 (5)C41—C40—H40A120.0
C1—C2—H2A120.2C39—C40—H40A120.0
C3—C2—H2A120.2C40—C41—C42120.9 (5)
C4—C3—C2120.6 (6)C40—C41—H41A119.6
C4—C3—H3A119.7C42—C41—H41A119.6
C2—C3—H3A119.7C43—C42—C41119.1 (5)
C3—C4—C5120.0 (5)C43—C42—H42A120.4
C3—C4—H4A120.0C41—C42—H42A120.4
C5—C4—H4A120.0C44—C43—C42120.6 (5)
C6—C5—C4119.7 (5)C44—C43—H43A119.7
C6—C5—H5A120.1C42—C43—H43A119.7
C4—C5—H5A120.1C43—C44—C39120.7 (5)
C5—C6—C1120.7 (5)C43—C44—H44A119.7
C5—C6—H6A119.7C39—C44—H44A119.7
C1—C6—H6A119.7C50—C45—C46120.9 (5)
C8—C7—C12120.3 (5)C50—C45—H45A119.5
C8—C7—H7A119.9C46—C45—H45A119.5
C12—C7—H7A119.9C47—C46—C45118.9 (5)
C7—C8—C9120.7 (6)C47—C46—H46A120.6
C7—C8—H8A119.7C45—C46—H46A120.6
C9—C8—H8A119.7C48—C47—C46121.0 (5)
C10—C9—C8119.9 (5)C48—C47—H47A119.5
C10—C9—H9A120.1C46—C47—H47A119.5
C8—C9—H9A120.1C47—C48—C49120.3 (5)
C9—C10—C11120.5 (5)C47—C48—H48A119.9
C9—C10—H10A119.7C49—C48—H48A119.9
C11—C10—H10A119.7C48—C49—C50119.1 (5)
C10—C11—C12119.1 (5)C48—C49—H49A120.4
C10—C11—H11A120.4C50—C49—H49A120.4
C12—C11—H11A120.4C45—C50—C49119.7 (5)
C7—C12—C11119.5 (5)C45—C50—P4120.0 (4)
C7—C12—P1119.4 (4)C49—C50—P4120.1 (4)
C11—C12—P1121.1 (4)O1—C51—C52106.1 (6)
P2—C13—P1114.4 (3)O1—C51—H51A110.5
P2—C13—Au3105.4 (2)C52—C51—H51A110.5
P1—C13—Au3102.8 (2)O1—C51—H51B110.5
P2—C13—H13A111.3C52—C51—H51B110.5
P1—C13—H13A111.3H51A—C51—H51B108.7
Au3—C13—H13A111.3C53—C52—C5199.2 (7)
C15—C14—C19119.8 (5)C53—C52—H52A111.9
C15—C14—P2119.7 (4)C51—C52—H52A111.9
C19—C14—P2120.5 (4)C53—C52—H52B111.9
C14—C15—C16120.2 (6)C51—C52—H52B111.9
C14—C15—H15A119.9H52A—C52—H52B109.6
C16—C15—H15A119.9C54—C53—C52105.3 (6)
C17—C16—C15119.3 (7)C54—C53—H53A110.7
C17—C16—H16A120.3C52—C53—H53A110.7
C15—C16—H16A120.3C54—C53—H53B110.7
C16—C17—C18122.1 (6)C52—C53—H53B110.7
C16—C17—H17A119.0H53A—C53—H53B108.8
C18—C17—H17A119.0O1—C54—C53106.8 (6)
C17—C18—C19119.3 (6)O1—C54—H54A110.4
C17—C18—H18A120.3C53—C54—H54A110.4
C19—C18—H18A120.3O1—C54—H54B110.4
C14—C19—C18119.3 (6)C53—C54—H54B110.4
C14—C19—H19A120.3H54A—C54—H54B108.6
C18—C19—H19A120.3O2—C55—C56108.0 (7)
C21—C20—C25121.5 (5)O2—C55—H55A110.1
C21—C20—H20A119.3C56—C55—H55A110.1
C25—C20—H20A119.3O2—C55—H55B110.1
C20—C21—C22119.4 (5)C56—C55—H55B110.1
C20—C21—H21A120.3H55A—C55—H55B108.4
C22—C21—H21A120.3C55—C56—C57103.7 (7)
C21—C22—C23120.0 (5)C55—C56—H56A111.0
C21—C22—H22A120.0C57—C56—H56A111.0
C23—C22—H22A120.0C55—C56—H56B111.0
C22—C23—C24120.8 (5)C57—C56—H56B111.0
C22—C23—H23A119.6H56A—C56—H56B109.0
C24—C23—H23A119.6C58—C57—C56103.3 (6)
C23—C24—C25119.2 (5)C58—C57—H57A111.1
C23—C24—H24A120.4C56—C57—H57A111.1
C25—C24—H24A120.4C58—C57—H57B111.1
C20—C25—C24118.9 (5)C56—C57—H57B111.1
C20—C25—P2119.3 (4)H57A—C57—H57B109.1
C24—C25—P2121.7 (4)O2—C58—C57107.3 (6)
C27—C26—C31118.6 (5)O2—C58—H58A110.3
C27—C26—P3118.4 (4)C57—C58—H58A110.3
C31—C26—P3123.0 (4)O2—C58—H58B110.3
C28—C27—C26121.2 (5)C57—C58—H58B110.3
C28—C27—H27A119.4H58A—C58—H58B108.5
P1—Au1—Au2—P20.37 (5)C21—C20—C25—P2175.6 (4)
Cl1—Au1—Au2—P2179.53 (5)C23—C24—C25—C202.6 (7)
P1—Au1—Au2—Cl2179.83 (5)C23—C24—C25—P2174.4 (4)
Cl1—Au1—Au2—Cl20.08 (5)C13—P2—C25—C20165.0 (4)
C13—Au3—Au4—P4159.40 (14)C14—P2—C25—C2078.2 (4)
P3—Au3—Au4—P423.07 (5)Au2—P2—C25—C2042.5 (4)
C13—Au3—Au4—Cl419.84 (14)C13—P2—C25—C2411.9 (5)
P3—Au3—Au4—Cl4157.70 (5)C14—P2—C25—C24104.9 (4)
Au2—Au1—P1—C1326.52 (17)Au2—P2—C25—C24134.5 (4)
Au2—Au1—P1—C198.65 (17)C37—P3—C26—C2791.9 (4)
Au2—Au1—P1—C12145.32 (17)C38—P3—C26—C27156.7 (4)
Au1—Au2—P2—C1327.05 (17)Au3—P3—C26—C2731.3 (4)
Au1—Au2—P2—C25144.44 (18)C37—P3—C26—C3184.7 (5)
Au1—Au2—P2—C1498.71 (18)C38—P3—C26—C3126.7 (5)
Au4—Au3—P3—C26166.56 (17)Au3—P3—C26—C31152.1 (4)
Au4—Au3—P3—C3773.93 (17)C31—C26—C27—C282.3 (8)
Au4—Au3—P3—C3846.32 (17)P3—C26—C27—C28174.5 (4)
Au3—Au4—P4—C39120.06 (17)C26—C27—C28—C290.1 (8)
Au3—Au4—P4—C50117.43 (17)C27—C28—C29—C302.5 (8)
Au3—Au4—P4—C380.83 (18)C28—C29—C30—C312.4 (8)
C13—P1—C1—C2111.2 (5)C29—C30—C31—C260.1 (9)
C12—P1—C1—C2137.5 (5)C27—C26—C31—C302.4 (8)
Au1—P1—C1—C217.0 (5)P3—C26—C31—C30174.2 (4)
C13—P1—C1—C667.5 (5)C37—C32—C33—C341.5 (8)
C12—P1—C1—C643.8 (5)C32—C33—C34—C350.8 (8)
Au1—P1—C1—C6164.4 (4)C33—C34—C35—C360.1 (8)
C6—C1—C2—C31.6 (9)C34—C35—C36—C370.3 (8)
P1—C1—C2—C3177.0 (5)C33—C32—C37—C361.2 (8)
C1—C2—C3—C42.3 (11)C33—C32—C37—P3179.3 (4)
C2—C3—C4—C51.0 (11)C35—C36—C37—C320.3 (7)
C3—C4—C5—C60.9 (10)C35—C36—C37—P3179.8 (4)
C4—C5—C6—C11.5 (9)C26—P3—C37—C3259.2 (5)
C2—C1—C6—C50.2 (9)C38—P3—C37—C3251.8 (5)
P1—C1—C6—C5178.9 (5)Au3—P3—C37—C32177.0 (4)
C12—C7—C8—C90.8 (9)C26—P3—C37—C36120.2 (4)
C7—C8—C9—C100.4 (9)C38—P3—C37—C36128.8 (4)
C8—C9—C10—C110.2 (9)Au3—P3—C37—C363.5 (5)
C9—C10—C11—C121.0 (8)C39—P4—C38—P3157.2 (3)
C8—C7—C12—C112.1 (8)C50—P4—C38—P389.7 (3)
C8—C7—C12—P1177.5 (5)Au4—P4—C38—P333.2 (3)
C10—C11—C12—C72.2 (7)C26—P3—C38—P4172.3 (3)
C10—C11—C12—P1177.4 (4)C37—P3—C38—P460.8 (3)
C13—P1—C12—C7151.7 (4)Au3—P3—C38—P463.0 (3)
C1—P1—C12—C793.9 (4)C50—P4—C39—C4075.2 (5)
Au1—P1—C12—C727.3 (5)C38—P4—C39—C4034.9 (5)
C13—P1—C12—C1128.7 (5)Au4—P4—C39—C40159.9 (4)
C1—P1—C12—C1185.7 (4)C50—P4—C39—C44103.2 (4)
Au1—P1—C12—C11153.1 (4)C38—P4—C39—C44146.6 (4)
C25—P2—C13—P1176.5 (2)Au4—P4—C39—C4421.6 (5)
C14—P2—C13—P170.3 (3)C44—C39—C40—C411.3 (8)
Au2—P2—C13—P156.1 (3)P4—C39—C40—C41177.1 (4)
C25—P2—C13—Au364.4 (3)C39—C40—C41—C420.9 (8)
C14—P2—C13—Au3177.6 (2)C40—C41—C42—C430.1 (9)
Au2—P2—C13—Au356.1 (2)C41—C42—C43—C440.1 (9)
C1—P1—C13—P270.8 (3)C42—C43—C44—C390.3 (8)
C12—P1—C13—P2178.6 (2)C40—C39—C44—C431.0 (8)
Au1—P1—C13—P256.1 (3)P4—C39—C44—C43177.4 (4)
C1—P1—C13—Au3175.6 (2)C50—C45—C46—C470.5 (8)
C12—P1—C13—Au364.9 (3)C45—C46—C47—C481.1 (8)
Au1—P1—C13—Au357.5 (2)C46—C47—C48—C490.9 (8)
Au4—Au3—C13—P2111.11 (19)C47—C48—C49—C500.9 (8)
Au4—Au3—C13—P1128.78 (17)C46—C45—C50—C492.3 (7)
C13—P2—C14—C15136.6 (4)C46—C45—C50—P4172.7 (4)
C25—P2—C14—C15110.6 (5)C48—C49—C50—C452.5 (7)
Au2—P2—C14—C159.2 (5)C48—C49—C50—P4172.5 (4)
C13—P2—C14—C1942.7 (5)C39—P4—C50—C45128.0 (4)
C25—P2—C14—C1970.1 (5)C38—P4—C50—C45121.6 (4)
Au2—P2—C14—C19170.1 (4)Au4—P4—C50—C452.7 (4)
C19—C14—C15—C160.8 (8)C39—P4—C50—C4957.1 (4)
P2—C14—C15—C16179.9 (4)C38—P4—C50—C4953.3 (4)
C14—C15—C16—C171.1 (9)Au4—P4—C50—C49177.7 (3)
C15—C16—C17—C180.4 (10)C54—O1—C51—C5217.8 (8)
C16—C17—C18—C192.1 (10)O1—C51—C52—C5333.9 (8)
C15—C14—C19—C180.9 (8)C51—C52—C53—C5438.2 (10)
P2—C14—C19—C18178.4 (4)C51—O1—C54—C536.9 (8)
C17—C18—C19—C142.3 (9)C52—C53—C54—O129.2 (10)
C25—C20—C21—C221.4 (8)C58—O2—C55—C5625.4 (10)
C20—C21—C22—C233.0 (8)O2—C55—C56—C575.4 (11)
C21—C22—C23—C241.9 (8)C55—C56—C57—C5815.1 (10)
C22—C23—C24—C250.9 (8)C55—O2—C58—C5735.9 (8)
C21—C20—C25—C241.4 (7)C56—C57—C58—O231.8 (9)
Acknowledgements top

This work was supported by the Eighth Technology Fund for Postgraduates of Beijing University of Technology (ykj-2010-3399), the National Natural Science Foundation of China (No. 21075114), the Science and Technology Development Project of Beijing Education Committee (KM200910005025) and the Special Environmental Protection Fund for Public Welfare Projects (201009015).

references
References top

Bruce, M. I., Jevric, M., Skelton, B. W., Smith, M. E., White, A. H. & Zaitseva, N. N. (2006). J. Organomet. Chem. 691, 361–370.

Bruker (1998). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.

Feng, D. F., Tang, S. S., Liu, C. W., Lin, I. J. B., Wen, Y. S. & Liu, L. K. (1997). Organometallics, 16, 901–909.

Sevillano, P., Fuhr, O., Hampe, O., Lebedkin, S., Matern, E., Fenske, D. & Kappes, M. M. (2007). Inorg.Chem. 46, 7294–7298.

Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122.