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The title compound, 7-[(Ph2P)Au(PPh3)]-8-(CH3)-7,8-nido-C2B9H10]·­0.5CH2Cl2 or [Au(C15H23B9P)­(C18H15P)]·­0.5CH2Cl2, is the first reported gold derivative of the ligand [7-­(Ph2P)-8-(CH3)-7,8-nido-C2B9H10]-. It has a mono­nuclear structure with the gold centre in an essentially linear coordination [P-Au-P 174.041 (15)°]. The open C2B3 face contains one H atom that is strongly bonded to the central B atom and semi-bridging to a neighbouring B atom [B-H distances 1.070 (16) and 1.45 (3) Å].

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270199014328/bm1352sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270199014328/bm1352Isup2.hkl
Contains datablock I

CCDC reference: 140936

Comment top

We are interested in closo- and nido-carborane derivatives, and have reported several complexes in which a gold moiety is coordinated to the anionic nido-diphosphine ligand 7,8-bis(diphenylphosphino)-7,8-dicarba-nido-undecaborate(1–) (Crespo, Gimeno, Laguna & Jones, 1996; Crespo et al., 1997, 1998). We report here the structure of the neutral title complex 7-{diphenyl[(triphenylphosphine)aurio]phosphine(1+)-P}-8-methyl-7,8- dicarba-nido-undecaborate(1-) dichloromethane hemisolvate, (I). The synthetic reaction (see Experimental) results in the coordination of an {Au(PPh3)} fragment and partial degradation of the icosahedral carborane diphosphine 1-(Ph2P)-2-(CH3)-1,2-closo-C2B10H10. The product is the first reported gold derivative of the parent carbaborylphosphine and one of the few metallorganic derivatives described with the nido-diphosphine [7-(Ph2P)-8-(CH3)-7,8-nido-C2B9H10] (cf. Viñas et al., 1996). [The `diphosphine' compound above only had one P atom ?]

The structural study of (I) (Fig. 1) reveals for the C2B9 cage a geometry corresponding to an icosahedron from which one vertex has been removed. The C1—C2 distance of 1.588 (2) Å is shorter than that found in the corresponding closo-phosphine 1-(Ph2P)-2-(CH3)-1,2-closo-C2B10H10 [1.702 (6) Å; Kivekäs et al., 1994], but very similar to those observed in the various ruthenium complexes, which range from 1.538 (9) Å in [Ru{7-(PPh2)-8-(CH3)-7,8-C2B9H10}2] (Viñas et al., 1995) to 1.561 (8) Å in [RuCl{7-(PPh2)-8-(CH3)-7,8-C2B9H10}(PPh3)2] (Viñas et al., 1996). The P1—Au—P2 fragment shows the linearity usually associated with two-coordinate gold(I) complexes, with Au—P distances of 2.3060 (5) and 2.3159 (5) Å, and a P—Au—P angle of 174.041 (15)°. A search of the Cambridge Structural Database (Allen & Kennard, 1993) for neutral molecules containing the P—Au—P group yielded 12 hits with a mean Au—P bond length of 2.317 Å.

The `extra' H atom (H2b) in the pentagonal C2B3 open face (atoms C1, C2, B1, B2 and B3; B2 bears two H atoms) is strongly bonded to the central B atom [B2—H2b 1.070 (16) Å], but can be considered as semi-bridging to B1 [B1—H2b 1.45 (3) Å]. This distance is similar to those in related derivatives such as [AuCl2{(PPh2)2C2B9H10}] (1.37 Å; Jones et al., 1997), [Au{(PPh2)2C2B9H10}{(PPh2)2C2B10H10] (1.35 Å; Crespo et al., 1997) or [Au2(C26H30B9C2)(C6F5)].CH2Cl2 [1.50 (8) Å; Crespo et al., 1998]. We attributed the imprecision of these values to the presence of heavy atoms; the current structure is appreciably more precise despite the presence of gold. We have observed a similar arrangement of H atoms in silver complexes of the open-face carborane ligand (Crespo, Gimeno, Jones & Laguna, 1996) and in the light-atom derivative [C2B9H10(SC5H4NH)2)](CF3SO3), in which the H atoms were freely refined, clearly showing the semi-bridging nature of this H atom [B—H distances 1.12 (3) and 1.39 (3) Å; Jones et al., 1997].

Experimental top

To a suspension of 1-(Ph2P)-2-(CH3)-7,8-nido-C2B10H10 (0.034 g, 0.1 mmol; Kivekäs et al., 1994) in ethanol (30 ml), [Au(PPh3)(SC4H8)]ClO4 (0.096 g, 0.15 mmol) was added. The mixture was refluxed for 30 min and the complex (a white solid) filtered off and washed with ethanol (10 ml) (yield: 72%). Analysis calculated for C33H38AuB9P2: C 50.05, H 4.08%; found: C 49.65, H 4.6%. NMR data: 31P{1H} (AB system) 17.21 p.p.m., J = 327.5 Hz; 1H −2.25 (m, vr, 1H), 1.41 (s, 3H, CH3), 6.7–7.8 (m, br, 15H, C6H5) p.p.m. Single crystals were obtained from an n-heptane–dichloromethane solution.

Refinement top

The dichloromethane solvate molecule is disordered over an inversion centre; C—Cl bond lengths were restrained to be equal. The high displacement parameters of this molecule may indicate partial occupation. All non-H atoms, except solvent C atoms, were refined anisotropically. H atoms of the carbaborane open face were located in difference syntheses and refined freely, but with B—H distances restrained to be equal. The methyl H atoms were identified from difference syntheses, idealized and refined as a rigid group allowed to rotate but not tip. Other H were included using a riding model. A total of 433 restraints were applied, involving local phenyl-ring symmetry and light-atom displacement parameters, in addition to the B—H restraints. The largest feature of residual electron density (1.07 e Å−3) is 0.79 Å from the Au atom.

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP (Siemens, 1994); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. The molecular structure of the title compound (solvent omitted). Ellipsoids are drawn at the 50% probability level and H-atom radii are arbitrary. The semi-bridging H2b—B1 interaction is indicated by a dashed line (see text).
7-[Triphenylphosphine(diphenylphosphino)gold(I)—P]-8-methyl-7,8- dicarba-nido-undecaborate(−1) Dichloromethane hemisolvate top
Crystal data top
[Au(C15H23B9P)(C18H15P)]·0.5CH2Cl2Z = 2
Mr = 833.29F(000) = 822
Triclinic, P1Dx = 1.481 Mg m3
a = 11.3770 (8) ÅMo Kα radiation, λ = 0.71073 Å
b = 12.518 (1) ÅCell parameters from 8011 reflections
c = 15.4837 (12) Åθ = 2–28°
α = 69.925 (3)°µ = 4.12 mm1
β = 72.338 (3)°T = 143 K
γ = 66.953 (3)°Irregular wedge, colourless
V = 1869.1 (2) Å30.29 × 0.22 × 0.16 mm
Data collection top
Bruker SMART 1000 CCD
diffractometer
10779 independent reflections
Radiation source: fine-focus sealed tube9788 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.017
Detector resolution: 8.192 pixels mm-1θmax = 30°, θmin = 1.4°
ω scansh = 1516
Absorption correction: multi-scan
(SADABS; Bruker, 1998)
k = 1717
Tmin = 0.400, Tmax = 0.518l = 2121
22230 measured reflections
Refinement top
Refinement on F2Primary atom site location: Patterson
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.020Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.048H atoms treated by a mixture of independent and constrained refinement
S = 0.99 w = 1/[σ2(Fo2) + (0.0291P)2]
where P = (Fo2 + 2Fc2)/3
10779 reflections(Δ/σ)max = 0.027
445 parametersΔρmax = 1.07 e Å3
443 restraintsΔρmin = 0.81 e Å3
Crystal data top
[Au(C15H23B9P)(C18H15P)]·0.5CH2Cl2γ = 66.953 (3)°
Mr = 833.29V = 1869.1 (2) Å3
Triclinic, P1Z = 2
a = 11.3770 (8) ÅMo Kα radiation
b = 12.518 (1) ŵ = 4.12 mm1
c = 15.4837 (12) ÅT = 143 K
α = 69.925 (3)°0.29 × 0.22 × 0.16 mm
β = 72.338 (3)°
Data collection top
Bruker SMART 1000 CCD
diffractometer
10779 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 1998)
9788 reflections with I > 2σ(I)
Tmin = 0.400, Tmax = 0.518Rint = 0.017
22230 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.020443 restraints
wR(F2) = 0.048H atoms treated by a mixture of independent and constrained refinement
S = 0.99Δρmax = 1.07 e Å3
10779 reflectionsΔρmin = 0.81 e Å3
445 parameters
Special details top

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

Distance B—H

1.0557 (0.0152) B1 - H01 1.0700 (0.0152) B2 - H02A 1.0702 (0.0164) B2 - H02B 1.0736 (0.0148) B3 - H03 1.4497 (0.0271) B1 - H02B

Angle HBH

110.20 (1.84) H02A - B2 - H02B

Angle BHB

93.74 (1.67) B2 - H02B - B1

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 solvate molecule is disordered over an inversion centre; C—Cl bond lengths were restrained to be equal. The high displacement parameters of this molecule may indicate partial occupation. All non-H atoms, except solvent C atoms, were refined anisotropically. H atoms of the carbaborane open face were located in difference syntheses and refined freely, but with B—H distances restrained to be equal. The methyl H atoms were identified from difference syntheses, idealized and refined as a rigid group allowed to rotate but not tip. Other H were included using a riding model. A total of 433 restraints were applied, involving local phenyl-ring symmetry (FLAT/SAME in SHELXL97; Sheldrick, 1997) and light-atom displacement parameters (DELU $C $B) in addition to the B—H restraints. The largest feature of residual electron density (1.07 e Å−3) is 0.79 Å from the Au atom.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Au0.294569 (7)0.514577 (6)0.275580 (5)0.02054 (2)
P10.15542 (4)0.70599 (4)0.28257 (3)0.01615 (8)
P20.43217 (5)0.32997 (4)0.25232 (3)0.02091 (9)
C10.01721 (16)0.75754 (15)0.22595 (11)0.0159 (3)
C20.04506 (17)0.74417 (16)0.12267 (12)0.0183 (3)
C30.18218 (18)0.69612 (19)0.07072 (13)0.0256 (4)
H3A0.23020.75090.06050.031*
H3B0.17950.68960.01010.031*
H3C0.22590.61670.10780.031*
C110.24231 (17)0.81368 (16)0.22694 (12)0.0186 (3)
C120.19030 (19)0.92600 (17)0.16855 (13)0.0241 (4)
H120.10590.94860.15600.029*
C130.2624 (2)1.0051 (2)0.12859 (15)0.0315 (4)
H130.22681.08180.08900.038*
C140.3857 (2)0.9723 (2)0.14645 (15)0.0328 (5)
H140.43491.02610.11870.039*
C150.4373 (2)0.8614 (2)0.20451 (15)0.0315 (4)
H150.52150.83960.21720.038*
C160.36690 (18)0.78184 (18)0.24439 (13)0.0246 (4)
H160.40330.70530.28380.030*
C210.09478 (18)0.71731 (16)0.40300 (12)0.0206 (3)
C220.0685 (2)0.82219 (19)0.42780 (14)0.0344 (5)
H220.08090.89160.38090.041*
C230.0243 (3)0.8256 (2)0.52109 (16)0.0495 (7)
H230.00630.89760.53770.059*
C240.0065 (3)0.7254 (2)0.58978 (16)0.0501 (7)
H240.02410.72850.65350.060*
C250.0331 (3)0.6207 (2)0.56590 (15)0.0456 (6)
H250.02060.55160.61320.055*
C260.0782 (2)0.61597 (18)0.47297 (14)0.0314 (4)
H260.09780.54320.45700.038*
C310.60289 (18)0.31324 (16)0.23430 (13)0.0224 (3)
C320.6408 (2)0.41605 (19)0.19330 (17)0.0358 (5)
H320.57710.49260.17850.043*
C330.7712 (2)0.4063 (2)0.17417 (18)0.0395 (5)
H330.79650.47650.14640.047*
C340.8645 (2)0.2957 (2)0.19520 (17)0.0356 (5)
H340.95370.28980.18190.043*
C350.8283 (2)0.19323 (19)0.23569 (17)0.0359 (5)
H350.89270.11700.25000.043*
C360.6976 (2)0.20148 (18)0.25549 (15)0.0298 (4)
H360.67300.13100.28340.036*
C410.39740 (18)0.20412 (17)0.34414 (13)0.0232 (4)
C420.4148 (2)0.09751 (18)0.32435 (14)0.0330 (5)
H420.44850.08920.26200.040*
C430.3829 (3)0.0035 (2)0.39556 (16)0.0399 (5)
H430.39510.06900.38200.048*
C440.3337 (2)0.0158 (2)0.48583 (16)0.0386 (5)
H440.31140.04830.53440.046*
C450.3163 (2)0.1208 (2)0.50647 (15)0.0409 (5)
H450.28320.12830.56900.049*
C460.3475 (2)0.2153 (2)0.43536 (14)0.0325 (4)
H460.33450.28780.44930.039*
C510.40975 (18)0.31485 (16)0.14640 (12)0.0209 (3)
C520.5137 (2)0.27239 (19)0.07808 (14)0.0286 (4)
H520.60060.25030.08560.034*
C530.4899 (2)0.2623 (2)0.00136 (15)0.0344 (5)
H530.56090.23210.04750.041*
C540.3642 (2)0.29575 (19)0.01359 (14)0.0302 (4)
H540.34890.29000.06860.036*
C550.2601 (2)0.3379 (2)0.05440 (16)0.0346 (5)
H550.17340.36040.04620.041*
C560.2827 (2)0.3469 (2)0.13438 (15)0.0317 (4)
H560.21130.37520.18110.038*
B10.0574 (2)0.85634 (19)0.06323 (14)0.0218 (4)
H010.030 (2)0.8906 (19)0.0097 (11)0.027 (6)*
B20.1739 (2)0.94821 (19)0.14447 (15)0.0232 (4)
H02A0.234 (2)1.0398 (14)0.1249 (15)0.028 (6)*
H02B0.0736 (17)0.940 (2)0.1147 (18)0.050 (8)*
B30.10664 (19)0.87126 (18)0.25025 (14)0.0194 (4)
H030.112 (2)0.9149 (18)0.3008 (13)0.021 (5)*
B40.0200 (2)0.64254 (18)0.21094 (13)0.0187 (4)
H40.03180.54370.23290.022*
B50.12371 (19)0.72534 (18)0.29432 (14)0.0191 (4)
H50.14160.67980.37100.023*
B60.2419 (2)0.84704 (19)0.23901 (15)0.0224 (4)
H60.34120.88310.28060.027*
B70.2141 (2)0.8395 (2)0.11944 (15)0.0234 (4)
H70.29360.87100.07930.028*
B80.0780 (2)0.71029 (19)0.10608 (14)0.0220 (4)
H80.06790.65570.05860.026*
B90.1897 (2)0.70441 (19)0.21366 (15)0.0221 (4)
H90.25460.64760.23690.027*
Cl10.5668 (6)0.3554 (6)0.4816 (4)0.217 (2)0.50
Cl20.5633 (6)0.5764 (6)0.4672 (5)0.244 (3)0.50
C990.5917 (9)0.4761 (8)0.4187 (7)0.094 (3)*0.50
H99A0.68410.45620.38630.112*0.50
H99B0.53820.51010.36980.112*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Au0.02145 (4)0.01662 (3)0.02164 (4)0.00004 (2)0.00705 (2)0.00723 (2)
P10.01644 (19)0.01485 (19)0.01604 (19)0.00315 (15)0.00430 (15)0.00381 (15)
P20.0224 (2)0.0179 (2)0.0202 (2)0.00113 (17)0.00508 (17)0.00756 (17)
C10.0159 (7)0.0174 (7)0.0147 (7)0.0061 (6)0.0025 (6)0.0040 (6)
C20.0199 (8)0.0224 (8)0.0140 (7)0.0088 (6)0.0028 (6)0.0043 (6)
C30.0202 (8)0.0355 (10)0.0202 (8)0.0075 (8)0.0003 (7)0.0111 (8)
C110.0181 (8)0.0222 (8)0.0170 (8)0.0070 (7)0.0032 (6)0.0066 (6)
C120.0263 (9)0.0255 (9)0.0233 (9)0.0133 (8)0.0084 (7)0.0007 (7)
C130.0404 (12)0.0311 (10)0.0273 (10)0.0216 (9)0.0100 (9)0.0021 (8)
C140.0366 (11)0.0443 (12)0.0292 (10)0.0286 (10)0.0020 (9)0.0090 (9)
C150.0220 (9)0.0477 (13)0.0333 (11)0.0167 (9)0.0036 (8)0.0156 (9)
C160.0196 (8)0.0296 (10)0.0258 (9)0.0059 (7)0.0071 (7)0.0086 (7)
C210.0246 (9)0.0205 (8)0.0163 (8)0.0066 (7)0.0045 (7)0.0043 (6)
C220.0565 (14)0.0236 (10)0.0221 (9)0.0135 (10)0.0039 (9)0.0072 (8)
C230.091 (2)0.0349 (12)0.0262 (11)0.0234 (13)0.0047 (12)0.0138 (9)
C240.085 (2)0.0479 (14)0.0186 (10)0.0270 (14)0.0012 (11)0.0108 (10)
C250.0773 (19)0.0391 (13)0.0188 (10)0.0276 (13)0.0037 (11)0.0001 (9)
C260.0496 (13)0.0241 (10)0.0213 (9)0.0152 (9)0.0069 (9)0.0029 (7)
C310.0249 (9)0.0215 (8)0.0224 (8)0.0044 (7)0.0075 (7)0.0087 (7)
C320.0349 (11)0.0214 (9)0.0476 (13)0.0060 (8)0.0125 (10)0.0043 (9)
C330.0371 (12)0.0288 (11)0.0524 (14)0.0140 (9)0.0099 (11)0.0052 (10)
C340.0300 (11)0.0352 (11)0.0442 (13)0.0114 (9)0.0096 (9)0.0104 (10)
C350.0287 (10)0.0241 (10)0.0517 (14)0.0019 (8)0.0136 (10)0.0085 (9)
C360.0309 (10)0.0206 (9)0.0368 (11)0.0057 (8)0.0110 (9)0.0054 (8)
C410.0218 (9)0.0226 (9)0.0208 (8)0.0024 (7)0.0035 (7)0.0064 (7)
C420.0455 (13)0.0259 (10)0.0225 (9)0.0094 (9)0.0005 (9)0.0089 (8)
C430.0540 (15)0.0285 (11)0.0337 (11)0.0162 (10)0.0004 (10)0.0080 (9)
C440.0377 (12)0.0365 (12)0.0296 (11)0.0125 (10)0.0023 (9)0.0011 (9)
C450.0451 (13)0.0441 (13)0.0229 (10)0.0106 (11)0.0046 (9)0.0099 (9)
C460.0364 (11)0.0326 (11)0.0259 (10)0.0065 (9)0.0009 (8)0.0141 (8)
C510.0234 (9)0.0187 (8)0.0190 (8)0.0037 (7)0.0047 (7)0.0060 (6)
C520.0254 (9)0.0372 (11)0.0243 (9)0.0082 (8)0.0033 (7)0.0126 (8)
C530.0346 (11)0.0484 (13)0.0231 (10)0.0160 (10)0.0008 (8)0.0152 (9)
C540.0425 (12)0.0315 (10)0.0239 (9)0.0174 (9)0.0100 (8)0.0062 (8)
C550.0303 (11)0.0386 (12)0.0405 (12)0.0075 (9)0.0133 (9)0.0155 (10)
C560.0245 (10)0.0385 (11)0.0344 (11)0.0053 (8)0.0049 (8)0.0185 (9)
B10.0213 (9)0.0255 (10)0.0190 (9)0.0095 (8)0.0064 (7)0.0017 (7)
B20.0203 (9)0.0206 (9)0.0261 (10)0.0055 (8)0.0067 (8)0.0022 (8)
B30.0183 (9)0.0174 (9)0.0214 (9)0.0050 (7)0.0041 (7)0.0043 (7)
B40.0223 (9)0.0184 (9)0.0174 (9)0.0081 (7)0.0031 (7)0.0058 (7)
B50.0174 (9)0.0215 (9)0.0183 (9)0.0082 (7)0.0006 (7)0.0049 (7)
B60.0170 (9)0.0243 (10)0.0249 (10)0.0067 (7)0.0020 (7)0.0070 (8)
B70.0194 (9)0.0275 (10)0.0240 (10)0.0088 (8)0.0062 (8)0.0044 (8)
B80.0230 (10)0.0263 (10)0.0204 (9)0.0123 (8)0.0038 (7)0.0054 (8)
B90.0214 (9)0.0252 (10)0.0236 (10)0.0117 (8)0.0028 (7)0.0072 (8)
Cl10.246 (6)0.266 (6)0.152 (4)0.089 (5)0.038 (4)0.062 (4)
Cl20.200 (5)0.286 (7)0.318 (8)0.084 (5)0.058 (5)0.153 (6)
Geometric parameters (Å, º) top
Au—P22.3060 (5)C42—C431.390 (3)
Au—P12.3159 (5)C43—C441.377 (3)
P1—C111.8072 (18)C44—C451.383 (3)
P1—C211.8158 (18)C45—C461.391 (3)
P1—C11.8197 (17)C51—C521.391 (3)
P2—C411.808 (2)C51—C561.393 (3)
P2—C311.8130 (19)C52—C531.392 (3)
P2—C511.8153 (18)C53—C541.377 (3)
C1—C21.588 (2)C54—C551.387 (3)
C1—B31.621 (3)C55—C561.388 (3)
C1—B51.743 (2)B1—B71.791 (3)
C1—B41.753 (2)B1—B81.802 (3)
C2—C31.510 (2)B1—B21.857 (3)
C2—B11.631 (3)B2—B61.776 (3)
C2—B41.722 (3)B2—B71.780 (3)
C2—B81.721 (3)B2—B31.815 (3)
C11—C121.395 (2)B3—B61.748 (3)
C11—C161.399 (2)B3—B51.784 (3)
C12—C131.394 (3)B4—B81.749 (3)
C13—C141.386 (3)B4—B91.770 (3)
C14—C151.380 (3)B4—B51.781 (3)
C15—C161.385 (3)B5—B61.750 (3)
C21—C221.389 (3)B5—B91.772 (3)
C21—C261.392 (3)B6—B91.790 (3)
C22—C231.388 (3)B6—B71.811 (3)
C23—C241.378 (3)B7—B81.769 (3)
C24—C251.379 (3)B7—B91.803 (3)
C25—C261.387 (3)B8—B91.761 (3)
C31—C361.395 (3)B1—H011.056 (15)
C31—C321.397 (3)B2—H02A1.070 (15)
C32—C331.386 (3)B2—H02B1.070 (16)
C33—C341.378 (3)B3—H031.074 (15)
C34—C351.383 (3)B1—H02B1.45 (3)
C35—C361.393 (3)Cl1—C991.571 (9)
C41—C461.387 (3)Cl2—C991.559 (8)
C41—C421.397 (3)
P2—Au—P1174.041 (15)B7—B1—B258.39 (12)
C11—P1—C21104.95 (8)B8—B1—B2107.35 (14)
C11—P1—C1106.93 (8)B6—B2—B761.22 (12)
C21—P1—C1108.63 (8)B6—B2—B358.23 (11)
C11—P1—Au110.30 (6)B7—B2—B3105.49 (14)
C21—P1—Au111.18 (6)B6—B2—B1105.23 (14)
C1—P1—Au114.35 (6)B7—B2—B158.94 (12)
C41—P2—C31109.24 (9)B3—B2—B1101.07 (13)
C41—P2—C51105.28 (9)C1—B3—B6105.46 (14)
C31—P2—C51106.42 (8)C1—B3—B561.34 (11)
C41—P2—Au113.87 (6)B6—B3—B559.39 (11)
C31—P2—Au113.12 (6)C1—B3—B2106.02 (14)
C51—P2—Au108.33 (6)B6—B3—B259.75 (12)
C2—C1—B3115.31 (14)B5—B3—B2109.19 (14)
C2—C1—B5112.04 (13)C2—B4—B859.47 (11)
B3—C1—B563.92 (11)C2—B4—C154.38 (10)
C2—C1—B461.82 (11)B8—B4—C1102.37 (13)
B3—C1—B4115.66 (13)C2—B4—B9104.70 (14)
B5—C1—B461.25 (11)B8—B4—B960.05 (12)
C2—C1—P1117.94 (12)C1—B4—B9103.06 (13)
B3—C1—P1118.82 (12)C2—B4—B5104.16 (13)
B5—C1—P1117.28 (11)B8—B4—B5108.28 (14)
B4—C1—P1114.54 (11)C1—B4—B559.10 (10)
C3—C2—C1121.35 (15)B9—B4—B559.88 (11)
C3—C2—B1117.57 (15)C1—B5—B6100.35 (13)
C1—C2—B1109.81 (14)C1—B5—B9103.38 (13)
C3—C2—B4117.37 (15)B6—B5—B961.09 (12)
C1—C2—B463.81 (11)C1—B5—B459.65 (10)
B1—C2—B4115.85 (14)B6—B5—B4107.97 (14)
C3—C2—B8119.04 (15)B9—B5—B459.78 (11)
C1—C2—B8111.00 (13)C1—B5—B354.73 (10)
B1—C2—B864.95 (12)B6—B5—B359.27 (11)
B4—C2—B861.05 (11)B9—B5—B3107.85 (14)
C12—C11—C16119.27 (17)B4—B5—B3106.56 (13)
C12—C11—P1122.95 (13)B3—B6—B561.33 (11)
C16—C11—P1117.78 (14)B3—B6—B262.02 (12)
C13—C12—C11119.89 (18)B5—B6—B2112.63 (14)
C14—C13—C12120.17 (19)B3—B6—B9108.67 (14)
C15—C14—C13120.12 (18)B5—B6—B960.08 (12)
C14—C15—C16120.29 (18)B2—B6—B9110.31 (15)
C15—C16—C11120.26 (18)B3—B6—B7107.08 (14)
C22—C21—C26119.11 (17)B5—B6—B7108.16 (15)
C22—C21—P1122.26 (14)B2—B6—B759.52 (12)
C26—C21—P1118.60 (14)B9—B6—B760.08 (12)
C23—C22—C21120.0 (2)B8—B7—B2112.31 (15)
C24—C23—C22120.5 (2)B8—B7—B160.80 (12)
C23—C24—C25119.9 (2)B2—B7—B162.67 (12)
C24—C25—C26120.1 (2)B8—B7—B959.06 (12)
C25—C26—C21120.33 (19)B2—B7—B9109.52 (14)
C36—C31—C32119.26 (18)B1—B7—B9107.36 (14)
C36—C31—P2122.40 (15)B8—B7—B6106.55 (14)
C32—C31—P2118.26 (15)B2—B7—B659.26 (12)
C33—C32—C31120.0 (2)B1—B7—B6106.57 (14)
C34—C33—C32120.5 (2)B9—B7—B659.40 (12)
C33—C34—C35120.0 (2)C2—B8—B459.48 (11)
C34—C35—C36120.2 (2)C2—B8—B9105.12 (14)
C35—C36—C31120.00 (19)B4—B8—B960.59 (12)
C46—C41—C42119.31 (19)C2—B8—B7102.51 (14)
C46—C41—P2119.40 (15)B4—B8—B7108.98 (15)
C42—C41—P2121.24 (14)B9—B8—B761.41 (12)
C43—C42—C41120.22 (19)C2—B8—B155.09 (11)
C44—C43—C42119.8 (2)B4—B8—B1106.30 (14)
C43—C44—C45120.6 (2)B9—B8—B1108.72 (15)
C44—C45—C46119.8 (2)B7—B8—B160.19 (12)
C41—C46—C45120.3 (2)B8—B9—B459.37 (11)
C52—C51—C56119.47 (17)B8—B9—B5108.11 (14)
C52—C51—P2122.62 (14)B4—B9—B560.34 (11)
C56—C51—P2117.91 (14)B8—B9—B6107.82 (14)
C51—C52—C53119.81 (19)B4—B9—B6106.65 (14)
C54—C53—C52120.5 (2)B5—B9—B658.83 (11)
C53—C54—C55119.97 (19)B8—B9—B759.53 (12)
C54—C55—C56119.9 (2)B4—B9—B7106.54 (14)
C55—C56—C51120.27 (19)B5—B9—B7107.53 (14)
C2—B1—B7105.35 (14)B6—B9—B760.53 (12)
C2—B1—B859.95 (11)H02A—B2—H02B110.2 (18)
B7—B1—B859.01 (12)B2—H02B—B193.7 (17)
C2—B1—B2107.61 (14)Cl2—C99—Cl1118.1 (7)

Experimental details

Crystal data
Chemical formula[Au(C15H23B9P)(C18H15P)]·0.5CH2Cl2
Mr833.29
Crystal system, space groupTriclinic, P1
Temperature (K)143
a, b, c (Å)11.3770 (8), 12.518 (1), 15.4837 (12)
α, β, γ (°)69.925 (3), 72.338 (3), 66.953 (3)
V3)1869.1 (2)
Z2
Radiation typeMo Kα
µ (mm1)4.12
Crystal size (mm)0.29 × 0.22 × 0.16
Data collection
DiffractometerBruker SMART 1000 CCD
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 1998)
Tmin, Tmax0.400, 0.518
No. of measured, independent and
observed [I > 2σ(I)] reflections
22230, 10779, 9788
Rint0.017
(sin θ/λ)max1)0.703
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.020, 0.048, 0.99
No. of reflections10779
No. of parameters445
No. of restraints443
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)1.07, 0.81

Computer programs: SMART (Bruker, 1998), SAINT (Bruker, 1998), SAINT, SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), XP (Siemens, 1994), SHELXL97.

Selected geometric parameters (Å, º) top
Au—P22.3060 (5)C1—C21.588 (2)
Au—P12.3159 (5)C2—C31.510 (2)
P1—C111.8072 (18)B1—H011.056 (15)
P1—C211.8158 (18)B2—H02A1.070 (15)
P1—C11.8197 (17)B2—H02B1.070 (16)
P2—C411.808 (2)B3—H031.074 (15)
P2—C311.8130 (19)B1—H02B1.45 (3)
P2—C511.8153 (18)
P2—Au—P1174.041 (15)C41—P2—C51105.28 (9)
C11—P1—C21104.95 (8)C31—P2—C51106.42 (8)
C11—P1—C1106.93 (8)C41—P2—Au113.87 (6)
C21—P1—C1108.63 (8)C31—P2—Au113.12 (6)
C11—P1—Au110.30 (6)C51—P2—Au108.33 (6)
C21—P1—Au111.18 (6)H02A—B2—H02B110.2 (18)
C1—P1—Au114.35 (6)B2—H02B—B193.7 (17)
C41—P2—C31109.24 (9)
 

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