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The dinuclear AuI complex containing the 4,5-bis­(diphenyl­phosphino)-9,9-dimethylxanthene (xantphos) ligand and trifluoro­acetate anions exists in a solvent-free form, [μ-4,5-bis­(diphenyl­phosphino)-9,9-dimethyl­xanthene]bis­[(trifluoro­acetato)gold(I)], [Au2(C2F3O2)2(C39H32OP2)], (I), and as a dichloro­methane solvate, [Au2(C2F3O2)2(C39H32OP2)]·0.58CH2Cl2, (II). The trifluoro­acetate anions are coordinated to the AuI centres bridged by the xantphos ligand in both compounds. The AuI atoms are in distorted linear coordination environments in both compounds. The phosphine substituents are in a syn arrangement in the xantphos ligand, which facilitates the formation of short aurophilic Au...Au inter­actions of 2.8966 (8) Å in (I) and 2.9439 (6) Å in (II).

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270110013363/fg3162sup1.cif
Contains datablocks global, I, II

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270110013363/fg3162Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270110013363/fg3162IIsup3.hkl
Contains datablock II

CCDC references: 779954; 779955

Comment top

Coordination-directed self-assembly of metal centres and multidentate ligands has become a powerful technique for the preparation of large supramolecular structures of defined shapes and sizes (Levin & Stang, 2000). Among these compounds are the AuI–diphosphine complexes, which have attracted much interest because of their photophysical, catalytic and pharmaceutical applications (Keefe et al., 2000). The 9,9-dimethyl-4,5-bis(diphenylphosphino)xanthene ligand (xantphos) was first structurally characterised by Hillebrand et al. (1995), and in recent years xantphos and its metal complexes have been used as effective catalysts (Kranenburg et al., 1995). The transition metal [rhodium(I), platinum(II), palladium(II), nickel(II)] complexes of the xantphos ligand are essential catalysts in hydroformylation, allylic alkylation, amination and hydrocyanation reactions (Kamer et al., 2001). The AuI complex of xantphos, [AuCl(xantphos)], catalyses the dehydrogenative silylation of alcohols with high chemoselectivity and solvent tolerance (Ito et al., 2005).

The first AuI–xantphos complexes of dinuclear [Au2Cl2(µ-xantphos)] and mononuclear [Au(xantphos)2][SbF6] were synthesised and structurally characterized a few years ago (Pintado-Alba et al., 2004). We recently reported the synthesis and structural characterization of two novel AuI–xantphos complexes, [Au2(NO3)2(µ-xantphos)] [the first example of the crystallization-induced spontaneous resolution of a dinuclear AuI complex] and [Au2(µ-xantphos)2](NO3)2 (Deák et al., 2006). As a continuation of our work on AuI complexes of xanthene-based diphosphine ligands, the dinuclear [Au2(nixantphos)2](NO3)2 [nixantphos = 4,6-bis(diphenylphosphino)phenoxazine] complex was synthesised and X-ray analysis revealed the solvent-assisted spontaneous resolution of the [Au2(nixantphos)2]2+ metallacycle (Tunyogi et al., 2008).

All reported dinuclear AuI complexes with xantphos and nixantphos ligands exhibit short intramolecular aurophilic Au···Au interactions ranging from 2.856 (1) to 2.995 (1) Å (Deák et al., 2006; Pintado-Alba et al., 2004; Tunyogi et al., 2008). The Au···Au bond distance in complexes showing aurophilic interactions ranges from 2.70 to 3.30 Å (Schmidbaur, 2000). The strength of this attraction has been determined to be ca 7–11 kcal mol-1 [1 kcal mol-1 = 4.184 kJ mol-1] and is comparable with that of hydrogen bonding (Schmidbaur et al., 1988). Very recently, the tricoordinate monomeric [AuCl(xantphos)] complex was prepared and structurally characterised (Ito et al., 2009). The mononuclear [Au(xantphos)2][SbF6] and [AuCl(xantphos)] complexes lack any additional aurophilic interactions (Ito et al., 2009; Pintado-Alba et al., 2004).

We report here the structures of a dinuclear AuI complex containing the xantphos ligand and trifluoroacetate anions, in a solvent-free form, [Au2(O2CCF3)2(µ-xantphos)], (I), and as a dichloromethane solvate, [Au2(O2CCF3)2(µ-xantphos)].0.58CH2Cl2, (II). In both (I) and (II) the trifluoroacetate anions are coordinated to the AuI centres bridged by the xantphos ligand (Figs. 1 and 2). In (I), the Au1 atom is disordered over two sites. The AuI atoms are in distorted linear coordination environments in both compounds, with P—Au—O angles of 159.4 (5), 173.29 (15) and 174.1 (2)° in (I), and 168.40 (14) and 174.18 (14)° in (II). The deviation from linearity of the P—Au—O angles could be the result of an intramolecular aurophilic interaction (Mohamed et al., 2003). The AuI atom has little affinity for O-donor ligands, and AuI complexes containing Au—O bonds are generally used as precursors in gold chemistry (Brandys et al., 2000; Deák et al., 2007; Preisenberger et al., 1999).

Gold(I)–phosphine complexes containing the trifluoroacetate anion can be grouped into three broad categories, namely those having no aurophilic interactions, those with intermolecular Au···Au interactions, and those with intramolecular Au···Au interactions. Complexes in the first category, e.g. [Ph3PAu(O2CCF3)], are mononuclear and contain a monophosphine ligand with bulky substituents on P, and the formation of an Au···Au interaction is precluded by steric restraints (Zhang et al., 1988). Gold(I) compounds in the second category contain either monophosphine or diphosphine ligands. Complexes of monophosphine ligands, e.g. [Me3PAu(O2CCF3)], form trimers via intermolecular Au···Au interactions when the substituents on P are not too bulky (Preisenberger et al., 1999). Complexes of diphosphine ligands having phosphine substituents linked by conformationally flexible backbones, e.g. [Au2(O2CCF3)2(µ-dppb)] [dppb = 1,4-bis(diphenylphosphino)butane] (Brandys et al., 2000) and [Au2(O2CCF3)2(µ-dppf)] [dppf = 1,1'-bis(diphenylphosphino)ferrocene] (Low et al., 1997), also exhibit intermolecular Au···Au interactions. In these compounds, the formation of any intramolecular aurophilic interaction is precluded by the anti arrangement of the phosphine substituents. Gold(I) complexes in the third category exhibit intramolecular Au···Au interactions as a result of their rigid phosphine backbone, which preorganizes the AuI centres in a syn configuration. In the [Au2(O2CCF3)2(µ-dppbz)] [dppbz = 1,2-bis(diphenylphosphino)benzene] complex, the rigid backbone of the diphosphine advances the formation of an intramolecular aurophilic interaction of 2.908 (1) Å (Deák et al., 2007). Complexes (I) and (II) also exhibit short aurophilic interactions of 2.8966 (8) Å in (I) and 2.9439 (6) Å (II). In (I) and (II) the xantphos ligand backbone is folded and tilted [by 53.9 (1)° in (I) and 52.8 (1)° in (II)] with respect to the main Au···Au axis, most likely to accommodate the two AuI atoms at a close distance.

The Au–P bond lengths are 2.2208 (19) and 2.2113 (18) Å in (I), and 2.2133 (16) and 2.2202 (17) Å in (II). The observed P1···P2 distances in (I) [4.687 (2) Å] and (II) [4.742 (2) Å] are significantly longer than that in the free ligand [4.045 (1) Å; Hillebrand et al., 1995]. The trifluoroacetate ions in both (I) and (II) coordinate to the AuI atom through only one O atom, with Au—O = 2.060 (5) and 2.100 (7) Å in (I), and 2.071 (5) and 2.094 (5) Å in (II). For comparison, in the acetate structure [Ph3PAu(O2CMe)] (Jones, 1984) the Au—O distance is 2.063 (6) Å.

In (I) and (II), the orientation of the coordinated trifluoroacetate anions can be defined by the values of the O2—Au1—Au2—O4 torsion angles [-74.2 (3) in (I) and -67.6 (2)° (II)]. In both complexes, the CF3 group has high thermal motion consistent, with some unresolved rotational disorder, as is often found in other trifluoroacetate compounds (Kia et al., 2005; Rodrigues et al., 2000, 2001). In (II), the anisotropic displacement parameters of atoms O3 and C17 atoms are also large, however the data quality did not enable to develop an adequate model for this possible disorder of the trifluoroacetate group.

A variety of dinuclear AuI–diphosphine complexes have been reported to be luminescent in solution and in the solid state under ambient conditions (King et al.,1989; Pawlowski et al.,2004; Pintado-Alba et al., 2004). Complex (I) is nonemissive in dichloromethane solution at room temperature. The solid-state emission spectrum of (I) at room temperature exhibits a broad band at 416 nm and two shoulders at 450 and 560 nm, when excited at 340 nm. [Corresponding data for (II)?]

Experimental top

Compound (I) was prepared starting from [Au2Cl2(µ-xantphos)] (Deák et al., 2006). A solution of [Au2Cl2(µ-xantphos)] (1 mmol) in dichloromethane (20 ml) was added to a suspension of silver(I)? trifluoroacetate (2 mmol) in dichloromethane (5 ml). After stirring for 45 min shielded from light, the AgCl precipitate was filtered through Celite. To the colourless filtrate, diethyl ether (10 ml) was added, and shiny crystals of (I) were obtained by slow evaporation of this solution.

Crystals of (II) were obtained by layering the filtrate with n-hexane. Shiny crystals of (I) and (II) were collected by filtration, washed with n-hexane and dried under vacuum. [How were the two compounds separated?] Absorption–emission and excitation data for (I) (Hitachi F-2500 fluorescence spectrophotometer, nm): 280 and 340 (CH2Cl2, 10-5 M at room temperature); λex = 340 nm, λmax (nm) = 416 (br), 450 (sh), 560 (sh); λem = 420 nm, λmax (nm) = 270, 315 (sh) (solid, room temperature).

Refinement top

In complex (I), the disorder of atom Au1 was refined over two positions using an EADP constraint (SHELXL97; Sheldrick, 2008) [refined site-occupancy factors are 0.834 (8) and 0.166 (8)]. The carboxylic acid atoms O3 and C16 were also determined to be disordered over two positions. Between the disordered components [refined site-occupancy factors are 0.65 (3) and 0.35 (3)], all equivalent C—O and C—C distances were restrained to be equal. The displacement parameters for atoms C161 and C162 atoms were also constrained using EADP constraints. Planarity was also restrained for the disordered C17/C161/O2/O31 and C17/C162/O2/O32 carboxyl systems. The anisotropic displacement parameters of atoms C14 and C15 are large for methyl C atoms, which may be due to large thermal motion and/or disorder.

In (II), the dichloromethane solvent molecule was not sufficiently resolved in the electron-density map, and therefore it could not be modelled with disordered atoms. Accordingly, the residual electron density was removed using the SQUEEZE routine in PLATON (Spek, 2009). The total volume available for solvent molecules was 529 Å3, which is distributed over four voids. The residual electron count was 97 electrons per unit cell, which corresponds to 2.31 dichloromethane molecules per unit cell. This means that 0.58 of a dichloromethane molecule could be accommodated in each void.

The methyl H atoms were constrained to an ideal geometry (C—H = 0.96 Å), with Uiso(H) = 1.5Ueq(C), but were allowed to rotate freely about their C—C bonds. All remaining H atoms were placed in geometrically idealized positions (C—H = 0.93 Å), and constrained to ride on their parent atoms with Uiso(H) = 1.2Ueq(C).

Computing details top

For both compounds, data collection: CrystalClear (Rigaku/MSC, 2005); cell refinement: CrystalClear (Rigaku/MSC, 2005); data reduction: CrystalClear (Rigaku/MSC, 2005); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: PLATON (Spek, 2009); software used to prepare material for publication: WinGX (Farrugia, 1999), PLATON (Spek, 2009), SHELXL97 (Sheldrick, 2008), enCIFer (Allen et al., 2004) and publCIF (Westrip, 2010).

Figures top
[Figure 1] Fig. 1. A view of the molecular structure of complex (I), with the atomic numbering scheme. Displacement ellipsoids are plotted at the 30% probability level and H atoms are shown as small spheres of arbitrary radii. Only the major components of the disordered atoms Au1, O3 and C16 are shown.
[Figure 2] Fig. 2. A view of the molecular structure of complex (II), with the atomic numbering scheme. Displacement ellipsoids are plotted at the 30% probability level and H atoms are shown as small spheres of arbitrary radii.
(I) [µ-4,5-Bis(diphenylphosphino)-9,9- dimethylxanthene]bis[(trifluoroacetato)gold(I)] top
Crystal data top
[Au2(C2F3O2)2(C39H32OP2)]Z = 2
Mr = 1198.56F(000) = 1144
Triclinic, P1Dx = 1.905 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71070 Å
a = 10.2311 (15) ÅCell parameters from 62308 reflections
b = 13.041 (2) Åθ = 3.0–27.5°
c = 17.344 (3) ŵ = 7.16 mm1
α = 73.969 (6)°T = 295 K
β = 88.123 (6)°Block, colourless
γ = 70.353 (6)°0.45 × 0.34 × 0.31 mm
V = 2090.0 (6) Å3
Data collection top
Rigaku R-AXIS RAPID
diffractometer
7370 independent reflections
Radiation source: fine-focus sealed tube6387 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.085
Detector resolution: 10 pixels mm-1θmax = 25.0°, θmin = 3.1°
ϕ and ω scansh = 1212
Absorption correction: multi-scan
CrystalClear (Rigaku/MSC, 2005)
k = 1515
Tmin = 0.067, Tmax = 0.109l = 2020
66358 measured reflections
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)] = 0.041Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.108H-atom parameters constrained
S = 1.03 w = 1/[σ2(Fo2) + (0.0567P)2 + 6.9312P]
where P = (Fo2 + 2Fc2)/3
7370 reflections(Δ/σ)max = 0.001
542 parametersΔρmax = 1.65 e Å3
5 restraintsΔρmin = 1.06 e Å3
Crystal data top
[Au2(C2F3O2)2(C39H32OP2)]γ = 70.353 (6)°
Mr = 1198.56V = 2090.0 (6) Å3
Triclinic, P1Z = 2
a = 10.2311 (15) ÅMo Kα radiation
b = 13.041 (2) ŵ = 7.16 mm1
c = 17.344 (3) ÅT = 295 K
α = 73.969 (6)°0.45 × 0.34 × 0.31 mm
β = 88.123 (6)°
Data collection top
Rigaku R-AXIS RAPID
diffractometer
7370 independent reflections
Absorption correction: multi-scan
CrystalClear (Rigaku/MSC, 2005)
6387 reflections with I > 2σ(I)
Tmin = 0.067, Tmax = 0.109Rint = 0.085
66358 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0415 restraints
wR(F2) = 0.108H-atom parameters constrained
S = 1.03Δρmax = 1.65 e Å3
7370 reflectionsΔρmin = 1.06 e Å3
542 parameters
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 > σ(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*/UeqOcc. (<1)
Au110.91247 (12)0.11920 (7)0.73878 (14)0.0470 (3)0.834 (8)
Au120.8965 (5)0.1126 (3)0.7183 (4)0.0470 (3)0.166 (8)
Au20.64593 (3)0.15526 (2)0.809294 (15)0.04475 (10)
P10.91458 (17)0.28178 (15)0.65507 (11)0.0435 (4)
P20.69139 (17)0.23702 (14)0.89617 (10)0.0406 (4)
C10.7589 (6)0.4057 (6)0.6157 (4)0.0417 (14)
C20.7421 (8)0.4531 (6)0.5320 (4)0.0514 (17)
H20.80210.41620.49910.062*
C30.6369 (9)0.5545 (7)0.4984 (5)0.063 (2)
H30.62470.58430.44280.075*
C40.5505 (7)0.6114 (6)0.5461 (5)0.0528 (18)
H40.48080.67990.52240.063*
C50.5648 (7)0.5690 (6)0.6292 (4)0.0470 (16)
C60.4807 (9)0.6381 (6)0.6822 (5)0.065 (2)
C70.4761 (7)0.5632 (6)0.7649 (4)0.0468 (16)
C80.3800 (8)0.5981 (6)0.8188 (5)0.0552 (18)
H80.31310.67020.80280.066*
C90.3803 (9)0.5301 (7)0.8947 (5)0.068 (2)
H90.31400.55650.92920.081*
C100.4772 (8)0.4239 (7)0.9203 (4)0.0565 (18)
H100.47710.37880.97220.068*
C110.5757 (7)0.3826 (6)0.8695 (4)0.0416 (14)
C120.5750 (6)0.4548 (5)0.7920 (4)0.0404 (14)
O10.6804 (4)0.4119 (4)0.7452 (3)0.0467 (11)
C130.6647 (7)0.4634 (6)0.6626 (4)0.0425 (15)
C140.3315 (12)0.7050 (12)0.6444 (7)0.154 (8)
H14A0.27790.65530.65420.231*
H14B0.33430.73530.58750.231*
H14C0.28930.76600.66780.231*
C150.5564 (18)0.7189 (10)0.6908 (9)0.150 (7)
H15A0.57620.75770.63860.226*
H15B0.64180.67600.72320.226*
H15C0.49830.77340.71610.226*
C210.9931 (8)0.2483 (7)0.5655 (4)0.0532 (18)
C221.0936 (9)0.2906 (9)0.5289 (5)0.073 (2)
H221.12350.33720.55070.088*
C231.1497 (10)0.2647 (12)0.4610 (6)0.098 (4)
H231.21810.29300.43740.118*
C241.1063 (12)0.1986 (12)0.4283 (6)0.095 (4)
H241.14380.18310.38150.114*
C251.0071 (13)0.1534 (9)0.4628 (6)0.092 (3)
H250.97840.10680.44040.111*
C260.9511 (10)0.1791 (8)0.5320 (5)0.073 (2)
H260.88420.14930.55620.088*
C311.0335 (7)0.3338 (7)0.6944 (5)0.0539 (17)
C321.0069 (9)0.4487 (8)0.6837 (6)0.074 (2)
H320.92150.50140.66050.089*
C331.1075 (11)0.4844 (11)0.7076 (8)0.099 (4)
H331.09000.56120.70070.119*
C341.2337 (11)0.4060 (12)0.7415 (7)0.098 (4)
H341.30180.43010.75700.117*
C351.2599 (9)0.2921 (11)0.7527 (6)0.088 (3)
H351.34530.23950.77590.106*
C361.1603 (8)0.2566 (8)0.7296 (5)0.066 (2)
H361.17800.17950.73760.079*
C410.8645 (6)0.2410 (6)0.9063 (4)0.0421 (14)
C420.8876 (8)0.3403 (7)0.9050 (5)0.0583 (19)
H420.81310.40820.89470.070*
C431.0194 (9)0.3392 (9)0.9187 (6)0.074 (2)
H431.03460.40630.91670.089*
C441.1284 (9)0.2387 (10)0.9355 (6)0.081 (3)
H441.21680.23750.94780.097*
C451.1099 (8)0.1412 (9)0.9345 (5)0.070 (2)
H451.18600.07460.94270.085*
C460.9786 (8)0.1408 (7)0.9213 (5)0.0576 (19)
H460.96560.07320.92230.069*
C510.6529 (7)0.1737 (6)0.9986 (4)0.0454 (15)
C520.7298 (8)0.1645 (7)1.0651 (4)0.0539 (17)
H520.80350.19201.05930.065*
C530.6968 (10)0.1142 (7)1.1408 (5)0.066 (2)
H530.75130.10491.18580.080*
C540.5865 (11)0.0783 (7)1.1500 (5)0.071 (2)
H540.56340.04701.20130.085*
C550.5076 (10)0.0878 (8)1.0837 (6)0.070 (2)
H550.43150.06331.09030.084*
C560.5416 (8)0.1335 (7)1.0081 (5)0.0581 (19)
H560.49060.13760.96330.070*
O20.9244 (8)0.0429 (6)0.8103 (4)0.0873 (19)
C1610.971 (2)0.1210 (12)0.7818 (8)0.068 (4)0.65 (3)
O311.043 (3)0.1359 (16)0.7292 (12)0.137 (10)0.65 (3)
C1620.920 (3)0.1056 (16)0.7731 (12)0.068 (4)0.35 (3)
O320.911 (5)0.079 (3)0.7031 (14)0.146 (15)0.35 (3)
C170.9281 (11)0.2272 (8)0.8270 (6)0.075 (2)
F10.8243 (11)0.2148 (9)0.8694 (7)0.183 (4)
F20.9097 (18)0.2816 (9)0.7826 (6)0.223 (7)
F31.0308 (10)0.2921 (8)0.8789 (7)0.182 (5)
O40.5813 (6)0.0815 (5)0.7340 (3)0.0573 (13)
O50.6096 (9)0.2050 (6)0.6236 (4)0.098 (2)
C180.5788 (8)0.1240 (6)0.6589 (4)0.0515 (17)
C190.5296 (12)0.0628 (8)0.6101 (6)0.075 (2)
F40.4027 (11)0.0729 (14)0.6177 (9)0.238 (7)
F50.5323 (19)0.0960 (10)0.5370 (4)0.245 (8)
F60.5832 (12)0.0425 (6)0.6323 (6)0.157 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Au110.0473 (2)0.0442 (2)0.0433 (6)0.01137 (16)0.0093 (3)0.0085 (2)
Au120.0473 (2)0.0442 (2)0.0433 (6)0.01137 (16)0.0093 (3)0.0085 (2)
Au20.04841 (17)0.04397 (17)0.04297 (16)0.01752 (12)0.01020 (11)0.01259 (12)
P10.0388 (9)0.0441 (10)0.0441 (9)0.0118 (7)0.0088 (7)0.0106 (8)
P20.0396 (8)0.0402 (9)0.0383 (8)0.0118 (7)0.0051 (7)0.0078 (7)
C10.039 (3)0.042 (4)0.046 (4)0.020 (3)0.002 (3)0.006 (3)
C20.059 (4)0.049 (4)0.044 (4)0.019 (3)0.004 (3)0.009 (3)
C30.071 (5)0.059 (5)0.046 (4)0.014 (4)0.007 (4)0.004 (4)
C40.048 (4)0.039 (4)0.061 (4)0.012 (3)0.009 (3)0.002 (3)
C50.039 (3)0.038 (4)0.056 (4)0.013 (3)0.005 (3)0.002 (3)
C60.070 (5)0.036 (4)0.071 (5)0.008 (4)0.025 (4)0.005 (4)
C70.043 (4)0.035 (3)0.058 (4)0.011 (3)0.009 (3)0.011 (3)
C80.054 (4)0.039 (4)0.061 (5)0.003 (3)0.011 (4)0.014 (3)
C90.065 (5)0.063 (5)0.062 (5)0.002 (4)0.019 (4)0.025 (4)
C100.064 (5)0.056 (5)0.042 (4)0.014 (4)0.008 (3)0.013 (3)
C110.042 (3)0.042 (4)0.042 (3)0.013 (3)0.004 (3)0.015 (3)
C120.034 (3)0.039 (3)0.047 (4)0.012 (3)0.006 (3)0.012 (3)
O10.037 (2)0.042 (3)0.049 (3)0.006 (2)0.012 (2)0.004 (2)
C130.039 (3)0.039 (3)0.043 (4)0.015 (3)0.007 (3)0.001 (3)
C140.085 (8)0.157 (12)0.084 (8)0.064 (8)0.029 (6)0.045 (8)
C150.263 (18)0.098 (9)0.168 (13)0.133 (11)0.152 (13)0.087 (9)
C210.051 (4)0.057 (4)0.044 (4)0.013 (3)0.013 (3)0.009 (3)
C220.064 (5)0.099 (7)0.050 (5)0.030 (5)0.017 (4)0.010 (4)
C230.062 (6)0.158 (12)0.055 (6)0.028 (7)0.023 (4)0.011 (7)
C240.080 (7)0.134 (10)0.046 (5)0.006 (7)0.020 (5)0.025 (6)
C250.117 (9)0.081 (7)0.071 (6)0.013 (6)0.002 (6)0.033 (5)
C260.083 (6)0.074 (6)0.069 (5)0.028 (5)0.027 (5)0.033 (5)
C310.043 (4)0.061 (5)0.060 (4)0.018 (3)0.007 (3)0.022 (4)
C320.051 (5)0.080 (6)0.102 (7)0.024 (4)0.006 (4)0.041 (5)
C330.077 (7)0.097 (8)0.147 (11)0.043 (6)0.003 (7)0.055 (8)
C340.075 (7)0.137 (11)0.114 (9)0.060 (7)0.005 (6)0.058 (8)
C350.043 (5)0.130 (10)0.088 (7)0.018 (5)0.002 (4)0.041 (7)
C360.050 (4)0.070 (5)0.073 (5)0.014 (4)0.007 (4)0.020 (4)
C410.039 (3)0.049 (4)0.038 (3)0.015 (3)0.005 (3)0.011 (3)
C420.047 (4)0.063 (5)0.059 (5)0.015 (4)0.001 (3)0.011 (4)
C430.057 (5)0.090 (7)0.086 (6)0.035 (5)0.003 (4)0.029 (5)
C440.049 (5)0.113 (9)0.079 (6)0.023 (5)0.001 (4)0.028 (6)
C450.047 (4)0.085 (6)0.071 (6)0.010 (4)0.003 (4)0.024 (5)
C460.051 (4)0.059 (5)0.052 (4)0.010 (4)0.004 (3)0.010 (4)
C510.049 (4)0.039 (4)0.043 (4)0.012 (3)0.009 (3)0.007 (3)
C520.063 (4)0.059 (5)0.043 (4)0.026 (4)0.007 (3)0.015 (3)
C530.090 (6)0.067 (5)0.042 (4)0.027 (5)0.010 (4)0.016 (4)
C540.101 (7)0.061 (5)0.052 (5)0.036 (5)0.034 (5)0.013 (4)
C550.071 (5)0.071 (6)0.074 (6)0.034 (5)0.033 (5)0.020 (5)
C560.054 (4)0.063 (5)0.061 (5)0.028 (4)0.015 (4)0.016 (4)
O20.105 (5)0.063 (4)0.078 (4)0.015 (4)0.020 (4)0.014 (3)
C1610.056 (12)0.107 (9)0.061 (6)0.036 (8)0.012 (7)0.048 (7)
O310.19 (2)0.114 (13)0.145 (14)0.077 (15)0.108 (15)0.085 (11)
C1620.056 (12)0.107 (9)0.061 (6)0.036 (8)0.012 (7)0.048 (7)
O320.15 (4)0.14 (3)0.12 (2)0.03 (2)0.05 (2)0.011 (19)
C170.090 (7)0.058 (5)0.074 (6)0.023 (5)0.017 (5)0.018 (5)
F10.173 (9)0.146 (8)0.225 (11)0.079 (7)0.103 (8)0.024 (7)
F20.47 (2)0.175 (9)0.122 (7)0.213 (12)0.055 (10)0.070 (7)
F30.138 (7)0.133 (7)0.203 (10)0.023 (6)0.023 (7)0.040 (7)
O40.079 (4)0.063 (3)0.042 (3)0.040 (3)0.012 (2)0.015 (2)
O50.148 (7)0.093 (5)0.066 (4)0.083 (5)0.020 (4)0.011 (4)
C180.059 (4)0.052 (4)0.048 (4)0.025 (4)0.003 (3)0.012 (3)
C190.105 (8)0.063 (6)0.062 (6)0.037 (5)0.013 (5)0.018 (4)
F40.125 (8)0.376 (19)0.314 (16)0.085 (10)0.014 (9)0.251 (16)
F50.58 (3)0.215 (10)0.055 (4)0.280 (15)0.025 (8)0.035 (5)
F60.238 (11)0.071 (5)0.173 (8)0.053 (6)0.038 (7)0.046 (5)
Geometric parameters (Å, º) top
Au11—O22.100 (7)C25—C261.389 (13)
Au11—P12.2208 (19)C25—H250.9300
Au11—Au22.8966 (8)C26—H260.9300
Au12—O22.143 (8)C31—C361.379 (11)
Au12—P12.243 (4)C31—C321.389 (12)
Au12—Au22.938 (4)C32—C331.380 (13)
Au2—O42.060 (5)C32—H320.9300
Au2—P22.2113 (18)C33—C341.374 (16)
P1—C311.809 (8)C33—H330.9300
P1—C211.819 (7)C34—C351.375 (17)
P1—C11.829 (7)C34—H340.9300
P2—C411.805 (6)C35—C361.364 (13)
P2—C111.806 (7)C35—H350.9300
P2—C511.832 (7)C36—H360.9300
C1—C131.399 (9)C41—C421.386 (10)
C1—C21.403 (9)C41—C461.394 (10)
C2—C31.380 (11)C42—C431.371 (11)
C2—H20.9300C42—H420.9300
C3—C41.367 (11)C43—C441.369 (14)
C3—H30.9300C43—H430.9300
C4—C51.387 (10)C44—C451.351 (14)
C4—H40.9300C44—H440.9300
C5—C131.388 (9)C45—C461.372 (11)
C5—C61.511 (11)C45—H450.9300
C6—C71.506 (10)C46—H460.9300
C6—C151.541 (14)C51—C521.373 (10)
C6—C141.541 (14)C51—C561.393 (10)
C7—C81.386 (10)C52—C531.382 (10)
C7—C121.395 (9)C52—H520.9300
C8—C91.370 (11)C53—C541.349 (13)
C8—H80.9300C53—H530.9300
C9—C101.366 (11)C54—C551.380 (13)
C9—H90.9300C54—H540.9300
C10—C111.385 (10)C55—C561.367 (11)
C10—H100.9300C55—H550.9300
C11—C121.410 (9)C56—H560.9300
C12—O11.387 (8)O2—C1621.184 (17)
O1—C131.392 (8)O2—C1611.201 (13)
C14—H14A0.9600C161—O311.173 (14)
C14—H14B0.9600C161—C171.583 (16)
C14—H14C0.9600C162—O321.16 (2)
C15—H15A0.9600C162—C171.58 (2)
C15—H15B0.9600C17—F21.238 (12)
C15—H15C0.9600C17—F11.263 (12)
C21—C261.378 (12)C17—F31.295 (13)
C21—C221.382 (11)O4—C181.265 (8)
C22—C231.370 (13)O5—C181.202 (9)
C22—H220.9300C18—C191.509 (12)
C23—C241.344 (17)C19—F51.223 (11)
C23—H230.9300C19—F61.246 (12)
C24—C251.381 (17)C19—F41.267 (14)
C24—H240.9300
O2—Au11—P1174.1 (2)C23—C24—H24119.4
O2—Au11—Au275.83 (19)C25—C24—H24119.4
P1—Au11—Au2109.24 (5)C24—C25—C26118.4 (11)
O2—Au12—P1159.4 (5)C24—C25—H25120.8
O2—Au12—Au274.3 (2)C26—C25—H25120.8
P1—Au12—Au2107.21 (16)C21—C26—C25121.0 (9)
O4—Au2—P2173.29 (15)C21—C26—H26119.5
O4—Au2—Au1191.23 (16)C25—C26—H26119.5
P2—Au2—Au1195.48 (7)C36—C31—C32119.3 (7)
O4—Au2—Au1283.0 (2)C36—C31—P1118.0 (6)
P2—Au2—Au12103.72 (17)C32—C31—P1122.3 (6)
Au11—Au2—Au128.54 (11)C33—C32—C31119.9 (9)
C31—P1—C21104.0 (4)C33—C32—H32120.1
C31—P1—C1105.7 (3)C31—C32—H32120.1
C21—P1—C1104.0 (3)C34—C33—C32119.7 (11)
C31—P1—Au11110.6 (3)C34—C33—H33120.1
C21—P1—Au11106.4 (3)C32—C33—H33120.1
C1—P1—Au11124.3 (2)C33—C34—C35120.5 (9)
C31—P1—Au12121.0 (3)C33—C34—H34119.7
C21—P1—Au1298.5 (3)C35—C34—H34119.7
C1—P1—Au12120.6 (2)C36—C35—C34119.8 (9)
C41—P2—C11106.3 (3)C36—C35—H35120.1
C41—P2—C51104.8 (3)C34—C35—H35120.1
C11—P2—C51105.3 (3)C35—C36—C31120.7 (9)
C41—P2—Au2119.2 (2)C35—C36—H36119.7
C11—P2—Au2108.1 (2)C31—C36—H36119.7
C51—P2—Au2112.2 (2)C42—C41—C46118.2 (7)
C13—C1—C2117.8 (6)C42—C41—P2121.8 (5)
C13—C1—P1125.1 (5)C46—C41—P2119.8 (6)
C2—C1—P1116.7 (5)C43—C42—C41120.6 (8)
C3—C2—C1120.2 (7)C43—C42—H42119.7
C3—C2—H2119.9C41—C42—H42119.7
C1—C2—H2119.9C44—C43—C42119.6 (9)
C4—C3—C2120.5 (7)C44—C43—H43120.2
C4—C3—H3119.7C42—C43—H43120.2
C2—C3—H3119.7C45—C44—C43121.2 (9)
C3—C4—C5121.3 (7)C45—C44—H44119.4
C3—C4—H4119.3C43—C44—H44119.4
C5—C4—H4119.3C44—C45—C46119.8 (9)
C4—C5—C13117.9 (7)C44—C45—H45120.1
C4—C5—C6121.2 (6)C46—C45—H45120.1
C13—C5—C6120.7 (6)C45—C46—C41120.5 (8)
C7—C6—C5110.9 (6)C45—C46—H46119.7
C7—C6—C15107.8 (9)C41—C46—H46119.7
C5—C6—C15106.8 (7)C52—C51—C56119.7 (7)
C7—C6—C14109.7 (7)C52—C51—P2122.3 (5)
C5—C6—C14110.4 (9)C56—C51—P2118.0 (6)
C15—C6—C14111.1 (11)C51—C52—C53119.5 (7)
C8—C7—C12116.6 (6)C51—C52—H52120.2
C8—C7—C6123.0 (6)C53—C52—H52120.2
C12—C7—C6120.3 (6)C54—C53—C52120.7 (8)
C9—C8—C7122.3 (7)C54—C53—H53119.7
C9—C8—H8118.9C52—C53—H53119.7
C7—C8—H8118.9C53—C54—C55120.3 (7)
C10—C9—C8120.4 (7)C53—C54—H54119.8
C10—C9—H9119.8C55—C54—H54119.8
C8—C9—H9119.8C56—C55—C54119.9 (8)
C9—C10—C11120.6 (7)C56—C55—H55120.0
C9—C10—H10119.7C54—C55—H55120.0
C11—C10—H10119.7C55—C56—C51119.8 (8)
C10—C11—C12118.0 (6)C55—C56—H56120.1
C10—C11—P2122.0 (5)C51—C56—H56120.1
C12—C11—P2119.8 (5)C162—O2—Au11114.0 (10)
O1—C12—C7122.2 (6)C161—O2—Au11117.7 (8)
O1—C12—C11115.7 (5)C162—O2—Au12102.7 (11)
C7—C12—C11122.1 (6)C161—O2—Au12109.0 (8)
C12—O1—C13118.2 (5)O31—C161—O2133.7 (14)
C5—C13—O1121.6 (6)O31—C161—C17113.7 (12)
C5—C13—C1121.9 (6)O2—C161—C17112.6 (10)
O1—C13—C1116.5 (6)O32—C162—O2123 (2)
C6—C14—H14A109.5O32—C162—C17123 (2)
C6—C14—H14B109.5O2—C162—C17113.9 (15)
H14A—C14—H14B109.5F2—C17—F1104.6 (12)
C6—C14—H14C109.5F2—C17—F3108.8 (12)
H14A—C14—H14C109.5F1—C17—F3103.0 (10)
H14B—C14—H14C109.5F2—C17—C162108.4 (11)
C6—C15—H15A109.5F1—C17—C162107.8 (11)
C6—C15—H15B109.5F3—C17—C162122.7 (12)
H15A—C15—H15B109.5F2—C17—C161114.1 (9)
C6—C15—H15C109.5F1—C17—C161120.1 (10)
H15A—C15—H15C109.5F3—C17—C161105.3 (11)
H15B—C15—H15C109.5C18—O4—Au2118.5 (5)
C26—C21—C22118.4 (8)O5—C18—O4128.2 (7)
C26—C21—P1119.5 (6)O5—C18—C19118.2 (7)
C22—C21—P1122.1 (7)O4—C18—C19113.7 (7)
C23—C22—C21120.7 (10)F5—C19—F6109.0 (11)
C23—C22—H22119.6F5—C19—F4101.5 (13)
C21—C22—H22119.6F6—C19—F499.7 (11)
C24—C23—C22120.3 (10)F5—C19—C18116.8 (8)
C24—C23—H23119.8F6—C19—C18115.0 (9)
C22—C23—H23119.8F4—C19—C18112.7 (9)
C23—C24—C25121.2 (9)
O2—Au11—Au2—O474.2 (3)C21—C22—C23—C240.8 (16)
P1—Au11—Au2—O4102.74 (18)C22—C23—C24—C251.4 (18)
O2—Au11—Au2—P2105.7 (2)C23—C24—C25—C260.9 (17)
P1—Au11—Au2—P277.35 (12)C22—C21—C26—C250.7 (14)
O2—Au11—Au2—Au1289.4 (6)P1—C21—C26—C25178.9 (8)
P1—Au11—Au2—Au1287.5 (6)C24—C25—C26—C210.1 (15)
O2—Au12—Au2—O484.0 (3)C21—P1—C31—C3672.0 (7)
P1—Au12—Au2—O4117.4 (3)C1—P1—C31—C36178.9 (6)
O2—Au12—Au2—P296.2 (3)Au11—P1—C31—C3641.9 (7)
P1—Au12—Au2—P262.4 (3)Au12—P1—C31—C3637.1 (8)
O2—Au12—Au2—Au1180.7 (6)C21—P1—C31—C32101.9 (7)
P1—Au12—Au2—Au1177.9 (6)C1—P1—C31—C327.3 (8)
Au2—Au11—P1—C31111.3 (3)Au11—P1—C31—C32144.3 (7)
Au2—Au11—P1—C21136.4 (3)Au12—P1—C31—C32149.0 (7)
Au2—Au11—P1—C116.1 (3)C36—C31—C32—C330.6 (14)
Au2—Au11—P1—Au1290.3 (6)P1—C31—C32—C33173.2 (8)
O2—Au12—P1—C319.5 (9)C31—C32—C33—C340.3 (17)
Au2—Au12—P1—C31100.7 (3)C32—C33—C34—C350.7 (19)
O2—Au12—P1—C21121.5 (8)C33—C34—C35—C360.3 (18)
Au2—Au12—P1—C21147.3 (3)C34—C35—C36—C310.5 (15)
O2—Au12—P1—C1126.7 (8)C32—C31—C36—C350.9 (13)
Au2—Au12—P1—C135.5 (4)P1—C31—C36—C35173.1 (7)
O2—Au12—P1—Au1114.2 (6)C11—P2—C41—C428.9 (7)
Au2—Au12—P1—Au1177.0 (6)C51—P2—C41—C42102.3 (6)
Au11—Au2—P2—C417.0 (3)Au2—P2—C41—C42131.2 (5)
Au12—Au2—P2—C419.3 (3)C11—P2—C41—C46175.6 (5)
Au11—Au2—P2—C11114.4 (2)C51—P2—C41—C4673.2 (6)
Au12—Au2—P2—C11112.1 (2)Au2—P2—C41—C4653.3 (6)
Au11—Au2—P2—C51129.9 (2)C46—C41—C42—C430.4 (11)
Au12—Au2—P2—C51132.2 (3)P2—C41—C42—C43175.1 (7)
C31—P1—C1—C1370.1 (6)C41—C42—C43—C441.4 (14)
C21—P1—C1—C13179.2 (6)C42—C43—C44—C453.6 (15)
Au11—P1—C1—C1359.3 (6)C43—C44—C45—C464.0 (15)
Au12—P1—C1—C1371.9 (7)C44—C45—C46—C412.1 (13)
C31—P1—C1—C2102.5 (6)C42—C41—C46—C450.1 (11)
C21—P1—C1—C26.6 (6)P2—C41—C46—C45175.6 (6)
Au11—P1—C1—C2128.1 (5)C41—P2—C51—C5215.4 (7)
Au12—P1—C1—C2115.5 (5)C11—P2—C51—C5296.5 (6)
C13—C1—C2—C31.1 (10)Au2—P2—C51—C52146.2 (6)
P1—C1—C2—C3172.1 (6)C41—P2—C51—C56164.3 (6)
C1—C2—C3—C41.9 (12)C11—P2—C51—C5683.7 (6)
C2—C3—C4—C50.6 (12)Au2—P2—C51—C5633.5 (6)
C3—C4—C5—C133.6 (11)C56—C51—C52—C530.8 (11)
C3—C4—C5—C6172.7 (8)P2—C51—C52—C53178.9 (6)
C4—C5—C6—C7160.4 (7)C51—C52—C53—C542.8 (13)
C13—C5—C6—C723.3 (10)C52—C53—C54—C552.3 (14)
C4—C5—C6—C1582.3 (11)C53—C54—C55—C560.2 (14)
C13—C5—C6—C1593.9 (10)C54—C55—C56—C512.2 (13)
C4—C5—C6—C1438.6 (11)C52—C51—C56—C551.7 (12)
C13—C5—C6—C14145.1 (9)P2—C51—C56—C55178.6 (6)
C5—C6—C7—C8163.3 (7)Au2—Au11—O2—C162108.5 (14)
C15—C6—C7—C880.0 (10)Au2—Au11—O2—C161135.0 (12)
C14—C6—C7—C841.0 (13)Au2—Au11—O2—Au1291.3 (6)
C5—C6—C7—C1219.6 (10)P1—Au12—O2—C162149.6 (14)
C15—C6—C7—C1297.1 (9)Au2—Au12—O2—C162113.1 (13)
C14—C6—C7—C12141.9 (10)P1—Au12—O2—C161125.5 (12)
C12—C7—C8—C90.6 (12)Au2—Au12—O2—C161137.3 (11)
C6—C7—C8—C9177.8 (8)P1—Au12—O2—Au1114.3 (6)
C7—C8—C9—C100.1 (14)Au2—Au12—O2—Au1183.0 (6)
C8—C9—C10—C110.8 (13)C162—O2—C161—O31109 (3)
C9—C10—C11—C121.8 (11)Au11—O2—C161—O3122 (2)
C9—C10—C11—P2172.1 (7)Au12—O2—C161—O3130 (2)
C41—P2—C11—C10114.5 (6)C162—O2—C161—C1773 (2)
C51—P2—C11—C103.6 (7)Au11—O2—C161—C17160.3 (9)
Au2—P2—C11—C10116.4 (6)Au12—O2—C161—C17151.8 (10)
C41—P2—C11—C1271.7 (6)C161—O2—C162—O32105 (3)
C51—P2—C11—C12177.5 (5)Au11—O2—C162—O320 (3)
Au2—P2—C11—C1257.4 (6)Au12—O2—C162—O323 (2)
C8—C7—C12—O1177.1 (6)C161—O2—C162—C1776 (2)
C6—C7—C12—O10.2 (10)Au11—O2—C162—C17179.5 (11)
C8—C7—C12—C111.7 (10)Au12—O2—C162—C17176.0 (14)
C6—C7—C12—C11179.0 (7)O32—C162—C17—F26 (3)
C10—C11—C12—O1176.5 (6)O2—C162—C17—F2173.6 (18)
P2—C11—C12—O19.4 (8)O32—C162—C17—F1118 (2)
C10—C11—C12—C72.3 (10)O2—C162—C17—F161 (2)
P2—C11—C12—C7171.7 (5)O32—C162—C17—F3122 (2)
C7—C12—O1—C1318.5 (9)O2—C162—C17—F358 (2)
C11—C12—O1—C13162.7 (6)O32—C162—C17—C161106 (3)
C4—C5—C13—O1176.3 (6)O2—C162—C17—C16175 (2)
C6—C5—C13—O17.3 (10)O31—C161—C17—F236.1 (19)
C4—C5—C13—C16.8 (10)O2—C161—C17—F2145.7 (15)
C6—C5—C13—C1169.6 (7)O31—C161—C17—F1161.4 (16)
C12—O1—C13—C514.6 (9)O2—C161—C17—F120 (2)
C12—O1—C13—C1168.3 (6)O31—C161—C17—F383.2 (16)
C2—C1—C13—C55.5 (10)O2—C161—C17—F395.0 (16)
P1—C1—C13—C5167.0 (5)O31—C161—C17—C162111 (3)
C2—C1—C13—O1177.4 (6)O2—C161—C17—C16270 (2)
P1—C1—C13—O110.1 (9)Au11—Au2—O4—C1858.5 (6)
C31—P1—C21—C26162.9 (7)Au12—Au2—O4—C1856.2 (6)
C1—P1—C21—C2686.7 (7)Au2—O4—C18—O50.4 (12)
Au11—P1—C21—C2646.0 (7)Au2—O4—C18—C19180.0 (6)
Au12—P1—C21—C2637.8 (7)O5—C18—C19—F54.3 (17)
C31—P1—C21—C2217.6 (8)O4—C18—C19—F5176.0 (13)
C1—P1—C21—C2292.8 (7)O5—C18—C19—F6134.0 (11)
Au11—P1—C21—C22134.5 (7)O4—C18—C19—F646.4 (13)
Au12—P1—C21—C22142.6 (7)O5—C18—C19—F4112.7 (13)
C26—C21—C22—C230.2 (13)O4—C18—C19—F466.9 (13)
P1—C21—C22—C23179.3 (8)
(II) [µ-4,5-Bis(diphenylphosphino)-9,9- dimethylxanthene]bis[(trifluoroacetato)gold(I)] dichloromethane 0.58-solvate top
Crystal data top
[Au2(C2F3O2)2(C39H32OP2)]·0.58CH2Cl2F(000) = 2385
Mr = 1247.60Dx = 1.896 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71070 Å
Hall symbol: -P 2ybcCell parameters from 92961 reflections
a = 10.548 (3) Åθ = 3.0–27.5°
b = 17.028 (4) ŵ = 6.92 mm1
c = 24.724 (7) ÅT = 295 K
β = 100.253 (11)°Block, colourless
V = 4370 (2) Å30.64 × 0.50 × 0.43 mm
Z = 4
Data collection top
Rigaku R-AXIS RAPID
diffractometer
7703 independent reflections
Radiation source: fine-focus sealed tube6972 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.081
Detector resolution: 10 pixels mm-1θmax = 25.0°, θmin = 3.0°
ϕ and ω scansh = 1212
Absorption correction: multi-scan
CrystalClear (Rigaku/MSC, 2005)
k = 2020
Tmin = 0.021, Tmax = 0.050l = 2929
99529 measured reflections
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)] = 0.037Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.092H-atom parameters constrained
S = 1.08 w = 1/[σ2(Fo2) + (0.0263P)2 + 15.3298P]
where P = (Fo2 + 2Fc2)/3
7703 reflections(Δ/σ)max = 0.001
526 parametersΔρmax = 1.04 e Å3
0 restraintsΔρmin = 1.26 e Å3
Crystal data top
[Au2(C2F3O2)2(C39H32OP2)]·0.58CH2Cl2V = 4370 (2) Å3
Mr = 1247.60Z = 4
Monoclinic, P21/cMo Kα radiation
a = 10.548 (3) ŵ = 6.92 mm1
b = 17.028 (4) ÅT = 295 K
c = 24.724 (7) Å0.64 × 0.50 × 0.43 mm
β = 100.253 (11)°
Data collection top
Rigaku R-AXIS RAPID
diffractometer
7703 independent reflections
Absorption correction: multi-scan
CrystalClear (Rigaku/MSC, 2005)
6972 reflections with I > 2σ(I)
Tmin = 0.021, Tmax = 0.050Rint = 0.081
99529 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0370 restraints
wR(F2) = 0.092H-atom parameters constrained
S = 1.08 w = 1/[σ2(Fo2) + (0.0263P)2 + 15.3298P]
where P = (Fo2 + 2Fc2)/3
7703 reflectionsΔρmax = 1.04 e Å3
526 parametersΔρmin = 1.26 e Å3
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 > σ(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.

The dichloromethane solvent molecule was not sufficiently resolved in the electron density map, therefore it could not be modelled with disordered atoms. Accordingly, the residual electron density was modelled using the SQUEEZE routine in PLATON (Spek, 2009). The total volume available for solvent molecules is 529 Å3, distributed over four voids. The residual electron count was 97 e/unit cell, which corresponds to 2.31 of dichloromethane / unit cell, which means that 0.58 of dichloromethane molecule could be accommodated in each void.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Au10.24156 (2)0.147441 (14)0.207456 (10)0.04753 (9)
Au20.16507 (2)0.004702 (14)0.260655 (10)0.04694 (9)
P10.20030 (15)0.24986 (9)0.25665 (6)0.0406 (3)
P20.33771 (16)0.00126 (9)0.32663 (7)0.0417 (4)
C10.0907 (6)0.2495 (3)0.3052 (2)0.0422 (13)
C20.0031 (6)0.3084 (4)0.3018 (3)0.0519 (16)
H20.02030.33970.27060.062*
C30.0708 (6)0.3206 (4)0.3444 (3)0.0577 (18)
H30.13270.35990.34170.069*
C40.0454 (7)0.2740 (4)0.3906 (3)0.0553 (17)
H40.09020.28320.41920.066*
C50.0444 (6)0.2139 (4)0.3961 (2)0.0435 (14)
C60.0728 (6)0.1680 (4)0.4480 (2)0.0486 (15)
C70.1753 (6)0.1063 (4)0.4457 (2)0.0445 (14)
C80.2182 (7)0.0579 (4)0.4903 (2)0.0558 (17)
H80.18990.06760.52320.067*
C90.3004 (8)0.0035 (4)0.4877 (3)0.064 (2)
H90.32900.03410.51860.077*
C100.3401 (7)0.0195 (4)0.4392 (3)0.0550 (16)
H100.39350.06230.43680.066*
C110.3016 (6)0.0277 (4)0.3934 (2)0.0433 (13)
C120.2234 (6)0.0922 (3)0.3986 (2)0.0415 (13)
O10.1981 (4)0.1408 (2)0.35332 (16)0.0439 (9)
C130.1090 (6)0.2004 (3)0.3527 (2)0.0425 (13)
C140.0504 (7)0.1255 (5)0.4581 (3)0.0638 (19)
H14A0.07510.08670.43010.096*
H14B0.11880.16300.45710.096*
H14C0.03380.10050.49350.096*
C150.1181 (9)0.2249 (5)0.4963 (3)0.079 (2)
H15A0.14520.19520.52940.118*
H15B0.04830.25890.50100.118*
H15C0.18880.25580.48860.118*
C210.1285 (6)0.3216 (3)0.2046 (2)0.0419 (13)
C220.1637 (7)0.3998 (4)0.2066 (3)0.0590 (18)
H220.22670.41840.23490.071*
C230.1038 (8)0.4498 (4)0.1661 (3)0.069 (2)
H230.12600.50270.16780.083*
C240.0131 (7)0.4239 (4)0.1237 (3)0.0607 (18)
H240.02480.45870.09650.073*
C250.0223 (7)0.3454 (4)0.1212 (3)0.0573 (17)
H250.08490.32720.09260.069*
C260.0359 (6)0.2948 (4)0.1614 (2)0.0515 (15)
H260.01300.24190.15960.062*
C310.3417 (6)0.2975 (4)0.2945 (2)0.0435 (14)
C320.3354 (7)0.3511 (5)0.3346 (3)0.069 (2)
H320.25770.35930.34650.083*
C330.4429 (8)0.3935 (5)0.3580 (4)0.082 (3)
H330.43720.42990.38550.099*
C340.5574 (8)0.3821 (5)0.3407 (4)0.075 (2)
H340.62920.41170.35560.090*
C350.5660 (7)0.3268 (5)0.3015 (3)0.072 (2)
H350.64480.31760.29080.086*
C360.4591 (6)0.2846 (4)0.2777 (3)0.0555 (16)
H360.46530.24780.25050.067*
C410.4751 (6)0.0564 (3)0.3148 (2)0.0433 (13)
C420.5432 (7)0.1029 (4)0.3552 (3)0.0582 (17)
H420.51590.10870.38880.070*
C430.6544 (8)0.1414 (5)0.3454 (4)0.075 (2)
H430.70050.17390.37210.090*
C440.6946 (8)0.1312 (5)0.2964 (4)0.078 (2)
H440.77010.15540.29050.093*
C450.6267 (8)0.0865 (5)0.2562 (4)0.071 (2)
H450.65460.08170.22280.085*
C460.5156 (7)0.0478 (4)0.2644 (3)0.0547 (16)
H460.46930.01680.23680.066*
C510.3990 (6)0.1010 (4)0.3370 (3)0.0483 (15)
C520.5279 (7)0.1167 (4)0.3563 (3)0.0593 (18)
H520.58780.07610.36240.071*
C530.5664 (8)0.1944 (5)0.3665 (3)0.072 (2)
H530.65250.20570.37990.087*
C540.4784 (10)0.2542 (5)0.3570 (3)0.075 (2)
H540.50510.30570.36470.090*
C550.3529 (9)0.2392 (4)0.3364 (3)0.072 (2)
H550.29490.28060.32900.086*
C560.3104 (7)0.1630 (4)0.3262 (3)0.0587 (17)
H560.22410.15290.31240.070*
O20.2740 (6)0.0665 (3)0.14759 (19)0.0745 (15)
O30.2109 (14)0.1561 (5)0.0886 (3)0.186 (5)
C160.2440 (9)0.0916 (5)0.1013 (3)0.076 (2)
C170.247 (2)0.0358 (9)0.0545 (5)0.148 (6)
F10.1950 (13)0.0335 (5)0.0638 (4)0.205 (5)
F20.1972 (16)0.0613 (6)0.0084 (3)0.298 (9)
F30.3596 (16)0.0156 (9)0.0506 (5)0.259 (8)
O40.0107 (5)0.0001 (3)0.1960 (2)0.0654 (14)
O50.0791 (5)0.1143 (4)0.2119 (3)0.0835 (17)
C180.0635 (6)0.0570 (4)0.1852 (3)0.0531 (16)
C190.1423 (9)0.0513 (6)0.1270 (3)0.076 (2)
F40.1472 (8)0.0152 (4)0.1042 (3)0.149 (3)
F50.2637 (6)0.0691 (5)0.1246 (3)0.157 (3)
F60.1022 (9)0.0976 (6)0.0941 (3)0.205 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Au10.06201 (17)0.03656 (15)0.04579 (15)0.00474 (11)0.01438 (11)0.00357 (10)
Au20.05860 (17)0.03718 (15)0.04311 (15)0.00149 (11)0.00382 (11)0.00079 (9)
P10.0478 (8)0.0353 (8)0.0393 (8)0.0010 (7)0.0095 (6)0.0040 (6)
P20.0490 (9)0.0356 (8)0.0410 (8)0.0013 (7)0.0094 (7)0.0034 (6)
C10.050 (3)0.033 (3)0.046 (3)0.001 (3)0.013 (3)0.000 (2)
C20.054 (4)0.043 (4)0.061 (4)0.010 (3)0.017 (3)0.010 (3)
C30.049 (4)0.044 (4)0.086 (5)0.010 (3)0.028 (3)0.005 (3)
C40.064 (4)0.048 (4)0.061 (4)0.007 (3)0.031 (3)0.006 (3)
C50.054 (4)0.042 (3)0.037 (3)0.002 (3)0.014 (3)0.003 (3)
C60.058 (4)0.051 (4)0.039 (3)0.005 (3)0.015 (3)0.009 (3)
C70.054 (4)0.046 (4)0.034 (3)0.005 (3)0.010 (3)0.003 (3)
C80.069 (4)0.068 (5)0.033 (3)0.002 (4)0.013 (3)0.001 (3)
C90.078 (5)0.069 (5)0.043 (4)0.004 (4)0.008 (3)0.014 (3)
C100.063 (4)0.055 (4)0.046 (4)0.009 (3)0.007 (3)0.010 (3)
C110.050 (3)0.043 (3)0.039 (3)0.001 (3)0.011 (3)0.000 (3)
C120.049 (3)0.039 (3)0.035 (3)0.003 (3)0.004 (2)0.002 (2)
O10.056 (2)0.040 (2)0.037 (2)0.0083 (19)0.0118 (18)0.0029 (17)
C130.045 (3)0.037 (3)0.046 (3)0.001 (3)0.009 (3)0.004 (3)
C140.063 (4)0.070 (5)0.063 (4)0.005 (4)0.023 (3)0.010 (4)
C150.100 (6)0.071 (5)0.061 (5)0.005 (5)0.003 (4)0.029 (4)
C210.046 (3)0.035 (3)0.045 (3)0.005 (3)0.009 (3)0.006 (2)
C220.074 (5)0.043 (4)0.057 (4)0.003 (3)0.003 (3)0.007 (3)
C230.085 (5)0.037 (4)0.084 (5)0.003 (4)0.012 (4)0.017 (4)
C240.071 (5)0.058 (5)0.055 (4)0.021 (4)0.016 (4)0.021 (3)
C250.058 (4)0.066 (5)0.046 (4)0.009 (4)0.006 (3)0.005 (3)
C260.066 (4)0.039 (4)0.048 (4)0.002 (3)0.007 (3)0.004 (3)
C310.049 (3)0.040 (3)0.042 (3)0.001 (3)0.009 (3)0.005 (3)
C320.055 (4)0.081 (6)0.070 (5)0.011 (4)0.009 (4)0.021 (4)
C330.071 (5)0.078 (6)0.094 (6)0.001 (5)0.002 (4)0.031 (5)
C340.058 (5)0.073 (6)0.086 (6)0.010 (4)0.007 (4)0.000 (4)
C350.048 (4)0.083 (6)0.083 (6)0.012 (4)0.006 (4)0.004 (5)
C360.053 (4)0.059 (4)0.054 (4)0.004 (3)0.011 (3)0.003 (3)
C410.048 (3)0.036 (3)0.046 (3)0.004 (3)0.010 (3)0.005 (3)
C420.064 (4)0.061 (4)0.049 (4)0.007 (4)0.006 (3)0.004 (3)
C430.066 (5)0.070 (5)0.084 (6)0.018 (4)0.003 (4)0.008 (4)
C440.055 (5)0.070 (6)0.109 (7)0.005 (4)0.019 (5)0.023 (5)
C450.077 (5)0.069 (5)0.077 (5)0.013 (4)0.038 (4)0.016 (4)
C460.066 (4)0.048 (4)0.053 (4)0.005 (3)0.020 (3)0.003 (3)
C510.063 (4)0.036 (3)0.048 (4)0.006 (3)0.015 (3)0.007 (3)
C520.064 (4)0.053 (4)0.061 (4)0.010 (4)0.013 (3)0.004 (3)
C530.082 (5)0.070 (5)0.066 (5)0.035 (5)0.017 (4)0.012 (4)
C540.116 (7)0.043 (4)0.072 (5)0.015 (5)0.033 (5)0.010 (4)
C550.096 (6)0.034 (4)0.092 (6)0.005 (4)0.033 (5)0.007 (4)
C560.069 (5)0.042 (4)0.068 (5)0.000 (3)0.020 (4)0.004 (3)
O20.127 (5)0.053 (3)0.043 (3)0.028 (3)0.016 (3)0.002 (2)
O30.380 (17)0.093 (6)0.066 (5)0.055 (8)0.013 (7)0.006 (4)
C160.114 (7)0.053 (5)0.056 (5)0.012 (5)0.003 (4)0.003 (4)
C170.27 (2)0.095 (10)0.073 (7)0.075 (12)0.009 (10)0.003 (6)
F10.352 (16)0.095 (6)0.139 (7)0.036 (7)0.037 (8)0.047 (5)
F20.62 (2)0.167 (8)0.057 (4)0.169 (12)0.069 (8)0.031 (4)
F30.354 (18)0.261 (14)0.197 (11)0.142 (15)0.143 (12)0.011 (9)
O40.082 (4)0.045 (3)0.060 (3)0.003 (3)0.014 (3)0.006 (2)
O50.078 (4)0.074 (4)0.093 (4)0.008 (3)0.001 (3)0.024 (3)
C180.050 (4)0.043 (4)0.065 (4)0.011 (3)0.008 (3)0.001 (3)
C190.085 (6)0.078 (6)0.059 (5)0.007 (5)0.000 (4)0.008 (4)
F40.204 (8)0.137 (6)0.081 (4)0.032 (5)0.044 (4)0.037 (4)
F50.089 (4)0.234 (9)0.130 (5)0.030 (5)0.032 (4)0.040 (6)
F60.235 (9)0.276 (11)0.082 (4)0.132 (8)0.029 (5)0.083 (6)
Geometric parameters (Å, º) top
Au1—O22.094 (5)C25—C261.375 (9)
Au1—P12.2133 (16)C25—H250.9300
Au1—Au22.9439 (6)C26—H260.9300
Au2—O42.071 (5)C31—C321.357 (9)
Au2—P22.2202 (17)C31—C361.393 (9)
P1—C311.806 (6)C32—C331.382 (10)
P1—C11.809 (6)C32—H320.9300
P1—C211.837 (6)C33—C341.364 (11)
P2—C411.817 (6)C33—H330.9300
P2—C511.818 (6)C34—C351.366 (12)
P2—C111.828 (6)C34—H340.9300
C1—C21.400 (8)C35—C361.378 (10)
C1—C131.426 (8)C35—H350.9300
C2—C31.389 (9)C36—H360.9300
C2—H20.9300C41—C421.373 (9)
C3—C41.377 (9)C41—C461.397 (8)
C3—H30.9300C42—C431.403 (10)
C4—C51.385 (9)C42—H420.9300
C4—H40.9300C43—C441.364 (12)
C5—C131.388 (8)C43—H430.9300
C5—C61.486 (8)C44—C451.350 (12)
C6—C71.516 (9)C44—H440.9300
C6—C151.546 (9)C45—C461.390 (10)
C6—C141.547 (9)C45—H450.9300
C7—C121.372 (8)C46—H460.9300
C7—C81.386 (9)C51—C521.385 (9)
C8—C91.368 (10)C51—C561.405 (9)
C8—H80.9300C52—C531.393 (10)
C9—C101.366 (10)C52—H520.9300
C9—H90.9300C53—C541.370 (12)
C10—C111.387 (9)C53—H530.9300
C10—H100.9300C54—C551.355 (12)
C11—C121.394 (8)C54—H540.9300
C12—O11.379 (7)C55—C561.381 (10)
O1—C131.382 (7)C55—H550.9300
C14—H14A0.9600C56—H560.9300
C14—H14B0.9600O2—C161.210 (9)
C14—H14C0.9600O3—C161.178 (10)
C15—H15A0.9600C16—C171.501 (14)
C15—H15B0.9600C17—F21.248 (13)
C15—H15C0.9600C17—F31.25 (2)
C21—C221.381 (9)C17—F11.34 (2)
C21—C261.391 (8)O4—C181.247 (8)
C22—C231.380 (9)O5—C181.205 (8)
C22—H220.9300C18—C191.532 (10)
C23—C241.361 (11)C19—F61.257 (10)
C23—H230.9300C19—F41.262 (10)
C24—C251.387 (10)C19—F51.308 (10)
C24—H240.9300
O2—Au1—P1168.40 (14)C23—C24—H24120.2
O2—Au1—Au282.24 (15)C25—C24—H24120.2
P1—Au1—Au2107.98 (4)C26—C25—C24119.4 (7)
O4—Au2—P2174.18 (14)C26—C25—H25120.3
O4—Au2—Au185.89 (14)C24—C25—H25120.3
P2—Au2—Au196.42 (4)C25—C26—C21120.8 (6)
C31—P1—C1102.9 (3)C25—C26—H26119.6
C31—P1—C21105.3 (3)C21—C26—H26119.6
C1—P1—C21103.6 (3)C32—C31—C36119.0 (6)
C31—P1—Au1114.5 (2)C32—C31—P1122.5 (5)
C1—P1—Au1125.0 (2)C36—C31—P1118.1 (5)
C21—P1—Au1103.6 (2)C31—C32—C33121.0 (7)
C41—P2—C51104.7 (3)C31—C32—H32119.5
C41—P2—C11107.5 (3)C33—C32—H32119.5
C51—P2—C11104.5 (3)C34—C33—C32120.0 (8)
C41—P2—Au2115.5 (2)C34—C33—H33120.0
C51—P2—Au2111.8 (2)C32—C33—H33120.0
C11—P2—Au2112.1 (2)C33—C34—C35119.7 (7)
C2—C1—C13117.4 (5)C33—C34—H34120.2
C2—C1—P1119.1 (4)C35—C34—H34120.2
C13—C1—P1122.7 (4)C34—C35—C36120.7 (7)
C3—C2—C1121.0 (6)C34—C35—H35119.7
C3—C2—H2119.5C36—C35—H35119.7
C1—C2—H2119.5C35—C36—C31119.6 (7)
C4—C3—C2119.5 (6)C35—C36—H36120.2
C4—C3—H3120.3C31—C36—H36120.2
C2—C3—H3120.3C42—C41—C46120.5 (6)
C3—C4—C5122.4 (6)C42—C41—P2121.6 (5)
C3—C4—H4118.8C46—C41—P2117.8 (5)
C5—C4—H4118.8C41—C42—C43119.2 (7)
C4—C5—C13117.9 (6)C41—C42—H42120.4
C4—C5—C6120.1 (5)C43—C42—H42120.4
C13—C5—C6121.9 (6)C44—C43—C42119.8 (8)
C5—C6—C7111.6 (5)C44—C43—H43120.1
C5—C6—C15109.0 (6)C42—C43—H43120.1
C7—C6—C15109.8 (6)C45—C44—C43121.1 (8)
C5—C6—C14109.9 (5)C45—C44—H44119.4
C7—C6—C14107.9 (5)C43—C44—H44119.4
C15—C6—C14108.7 (6)C44—C45—C46120.8 (7)
C12—C7—C8117.0 (6)C44—C45—H45119.6
C12—C7—C6121.8 (5)C46—C45—H45119.6
C8—C7—C6121.1 (5)C45—C46—C41118.6 (7)
C9—C8—C7122.5 (6)C45—C46—H46120.7
C9—C8—H8118.8C41—C46—H46120.7
C7—C8—H8118.8C52—C51—C56119.9 (6)
C10—C9—C8119.3 (6)C52—C51—P2122.1 (5)
C10—C9—H9120.3C56—C51—P2117.9 (5)
C8—C9—H9120.3C51—C52—C53118.9 (7)
C9—C10—C11120.6 (7)C51—C52—H52120.6
C9—C10—H10119.7C53—C52—H52120.6
C11—C10—H10119.7C54—C53—C52120.5 (8)
C10—C11—C12118.3 (6)C54—C53—H53119.7
C10—C11—P2120.2 (5)C52—C53—H53119.7
C12—C11—P2121.2 (4)C55—C54—C53120.8 (7)
C7—C12—O1122.5 (5)C55—C54—H54119.6
C7—C12—C11122.0 (5)C53—C54—H54119.6
O1—C12—C11115.5 (5)C54—C55—C56120.6 (8)
C12—O1—C13118.8 (4)C54—C55—H55119.7
O1—C13—C5122.7 (5)C56—C55—H55119.7
O1—C13—C1115.6 (5)C55—C56—C51119.3 (7)
C5—C13—C1121.7 (5)C55—C56—H56120.4
C6—C14—H14A109.5C51—C56—H56120.4
C6—C14—H14B109.5C16—O2—Au1112.8 (5)
H14A—C14—H14B109.5O3—C16—O2126.6 (8)
C6—C14—H14C109.5O3—C16—C17115.6 (9)
H14A—C14—H14C109.5O2—C16—C17117.8 (8)
H14B—C14—H14C109.5F2—C17—F3106.1 (17)
C6—C15—H15A109.5F2—C17—F1109.9 (17)
C6—C15—H15B109.5F3—C17—F1101.3 (12)
H15A—C15—H15B109.5F2—C17—C16114.8 (10)
C6—C15—H15C109.5F3—C17—C16112.7 (17)
H15A—C15—H15C109.5F1—C17—C16111.1 (14)
H15B—C15—H15C109.5C18—O4—Au2120.7 (4)
C22—C21—C26119.5 (6)O5—C18—O4131.0 (7)
C22—C21—P1122.8 (5)O5—C18—C19117.5 (7)
C26—C21—P1117.8 (5)O4—C18—C19111.5 (6)
C23—C22—C21118.9 (7)F6—C19—F4105.4 (9)
C23—C22—H22120.5F6—C19—F5105.4 (9)
C21—C22—H22120.5F4—C19—F5103.1 (9)
C24—C23—C22121.9 (7)F6—C19—C18112.3 (8)
C24—C23—H23119.1F4—C19—C18116.7 (7)
C22—C23—H23119.1F5—C19—C18113.0 (7)
C23—C24—C25119.6 (6)
O2—Au1—Au2—O467.6 (2)C31—P1—C21—C26165.2 (5)
P1—Au1—Au2—O4106.74 (16)C1—P1—C21—C2687.0 (5)
O2—Au1—Au2—P2107.03 (17)Au1—P1—C21—C2644.7 (5)
P1—Au1—Au2—P278.62 (6)C26—C21—C22—C231.3 (10)
O2—Au1—P1—C31100.3 (9)P1—C21—C22—C23179.3 (6)
Au2—Au1—P1—C31108.7 (2)C21—C22—C23—C241.4 (12)
O2—Au1—P1—C1131.5 (9)C22—C23—C24—C251.1 (12)
Au2—Au1—P1—C119.4 (3)C23—C24—C25—C260.7 (11)
O2—Au1—P1—C2113.9 (9)C24—C25—C26—C210.7 (10)
Au2—Au1—P1—C21137.1 (2)C22—C21—C26—C251.0 (10)
Au1—Au2—P2—C4117.3 (2)P1—C21—C26—C25179.6 (5)
Au1—Au2—P2—C51136.9 (2)C1—P1—C31—C3228.4 (7)
Au1—Au2—P2—C11106.2 (2)C21—P1—C31—C3279.8 (6)
C31—P1—C1—C297.4 (5)Au1—P1—C31—C32167.1 (5)
C21—P1—C1—C212.1 (6)C1—P1—C31—C36158.5 (5)
Au1—P1—C1—C2129.8 (5)C21—P1—C31—C3693.3 (5)
C31—P1—C1—C1371.3 (5)Au1—P1—C31—C3619.8 (6)
C21—P1—C1—C13179.2 (5)C36—C31—C32—C331.2 (12)
Au1—P1—C1—C1361.4 (6)P1—C31—C32—C33171.8 (7)
C13—C1—C2—C33.0 (9)C31—C32—C33—C340.1 (14)
P1—C1—C2—C3166.3 (5)C32—C33—C34—C352.0 (14)
C1—C2—C3—C40.1 (11)C33—C34—C35—C362.5 (13)
C2—C3—C4—C51.1 (11)C34—C35—C36—C311.2 (12)
C3—C4—C5—C130.8 (10)C32—C31—C36—C350.6 (10)
C3—C4—C5—C6176.9 (6)P1—C31—C36—C35172.7 (6)
C4—C5—C6—C7178.9 (6)C51—P2—C41—C42102.3 (6)
C13—C5—C6—C71.4 (8)C11—P2—C41—C428.4 (6)
C4—C5—C6—C1557.6 (8)Au2—P2—C41—C42134.3 (5)
C13—C5—C6—C15120.0 (7)C51—P2—C41—C4673.2 (5)
C4—C5—C6—C1461.4 (8)C11—P2—C41—C46176.1 (5)
C13—C5—C6—C14121.0 (7)Au2—P2—C41—C4650.2 (5)
C5—C6—C7—C125.7 (8)C46—C41—C42—C430.2 (10)
C15—C6—C7—C12126.7 (7)P2—C41—C42—C43175.1 (6)
C14—C6—C7—C12115.1 (6)C41—C42—C43—C441.2 (12)
C5—C6—C7—C8178.7 (6)C42—C43—C44—C452.3 (13)
C15—C6—C7—C857.8 (8)C43—C44—C45—C461.9 (13)
C14—C6—C7—C860.5 (8)C44—C45—C46—C410.4 (11)
C12—C7—C8—C92.7 (10)C42—C41—C46—C450.6 (10)
C6—C7—C8—C9173.1 (6)P2—C41—C46—C45174.9 (5)
C7—C8—C9—C101.6 (11)C41—P2—C51—C5225.8 (6)
C8—C9—C10—C112.4 (11)C11—P2—C51—C5287.0 (6)
C9—C10—C11—C121.0 (10)Au2—P2—C51—C52151.6 (5)
C9—C10—C11—P2172.0 (6)C41—P2—C51—C56155.9 (5)
C41—P2—C11—C10101.7 (6)C11—P2—C51—C5691.3 (6)
C51—P2—C11—C109.2 (6)Au2—P2—C51—C5630.2 (6)
Au2—P2—C11—C10130.4 (5)C56—C51—C52—C532.2 (10)
C41—P2—C11—C1285.5 (5)P2—C51—C52—C53176.1 (5)
C51—P2—C11—C12163.7 (5)C51—C52—C53—C540.7 (11)
Au2—P2—C11—C1242.5 (5)C52—C53—C54—C551.4 (12)
C8—C7—C12—O1173.6 (6)C53—C54—C55—C562.1 (13)
C6—C7—C12—O110.7 (9)C54—C55—C56—C510.6 (12)
C8—C7—C12—C116.3 (9)C52—C51—C56—C551.6 (10)
C6—C7—C12—C11169.4 (6)P2—C51—C56—C55176.7 (6)
C10—C11—C12—C75.5 (9)P1—Au1—O2—C1610.2 (14)
P2—C11—C12—C7167.4 (5)Au2—Au1—O2—C16142.0 (7)
C10—C11—C12—O1174.3 (6)Au1—O2—C16—O36.8 (16)
P2—C11—C12—O112.7 (7)Au1—O2—C16—C17172.7 (12)
C7—C12—O1—C137.9 (8)O3—C16—C17—F210 (3)
C11—C12—O1—C13172.3 (5)O2—C16—C17—F2169.6 (16)
C12—O1—C13—C50.4 (8)O3—C16—C17—F3111.7 (16)
C12—O1—C13—C1178.3 (5)O2—C16—C17—F369 (2)
C4—C5—C13—O1178.3 (6)O3—C16—C17—F1135.5 (14)
C6—C5—C13—O14.0 (9)O2—C16—C17—F144 (2)
C4—C5—C13—C13.9 (9)Au1—Au2—O4—C1855.0 (5)
C6—C5—C13—C1173.7 (6)Au2—O4—C18—O515.6 (11)
C2—C1—C13—O1177.1 (5)Au2—O4—C18—C19162.2 (5)
P1—C1—C13—O114.0 (7)O5—C18—C19—F673.5 (11)
C2—C1—C13—C55.0 (9)O4—C18—C19—F6104.6 (10)
P1—C1—C13—C5163.9 (5)O5—C18—C19—F4164.8 (9)
C31—P1—C21—C2214.1 (6)O4—C18—C19—F417.1 (11)
C1—P1—C21—C2293.6 (6)O5—C18—C19—F545.5 (11)
Au1—P1—C21—C22134.6 (5)O4—C18—C19—F5136.3 (8)

Experimental details

(I)(II)
Crystal data
Chemical formula[Au2(C2F3O2)2(C39H32OP2)][Au2(C2F3O2)2(C39H32OP2)]·0.58CH2Cl2
Mr1198.561247.60
Crystal system, space groupTriclinic, P1Monoclinic, P21/c
Temperature (K)295295
a, b, c (Å)10.2311 (15), 13.041 (2), 17.344 (3)10.548 (3), 17.028 (4), 24.724 (7)
α, β, γ (°)73.969 (6), 88.123 (6), 70.353 (6)90, 100.253 (11), 90
V3)2090.0 (6)4370 (2)
Z24
Radiation typeMo KαMo Kα
µ (mm1)7.166.92
Crystal size (mm)0.45 × 0.34 × 0.310.64 × 0.50 × 0.43
Data collection
DiffractometerRigaku R-AXIS RAPID
diffractometer
Rigaku R-AXIS RAPID
diffractometer
Absorption correctionMulti-scan
CrystalClear (Rigaku/MSC, 2005)
Multi-scan
CrystalClear (Rigaku/MSC, 2005)
Tmin, Tmax0.067, 0.1090.021, 0.050
No. of measured, independent and
observed [I > 2σ(I)] reflections
66358, 7370, 6387 99529, 7703, 6972
Rint0.0850.081
(sin θ/λ)max1)0.5950.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.041, 0.108, 1.03 0.037, 0.092, 1.08
No. of reflections73707703
No. of parameters542526
No. of restraints50
H-atom treatmentH-atom parameters constrainedH-atom parameters constrained
w = 1/[σ2(Fo2) + (0.0567P)2 + 6.9312P]
where P = (Fo2 + 2Fc2)/3
w = 1/[σ2(Fo2) + (0.0263P)2 + 15.3298P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)1.65, 1.061.04, 1.26

Computer programs: CrystalClear (Rigaku/MSC, 2005), SIR92 (Altomare et al., 1994), WinGX (Farrugia, 1999), PLATON (Spek, 2009), SHELXL97 (Sheldrick, 2008), enCIFer (Allen et al., 2004) and publCIF (Westrip, 2010).

 

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