
Supporting information
![]() | Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803001120/tk6088sup1.cif |
![]() | Structure factor file (CIF format) https://doi.org/10.1107/S1600536803001120/tk6088Isup2.hkl |
CCDC reference: 204660
The title compound was synthesized by a modification of a literature procedure (Porter et al., 1989). The complex was obtained by the reaction between [Au2(µ-dppm)2]Cl2 and AgPF6 in a 1:2 ratio in acetonitrile solution under anaerobic conditions for 12 h. After the white precipitate, AgCl, was filtered off, the solution was evaporated under vacuum affording [Au2(µ-dppm)2](PF6)2 in good yield. Well formed colorless crystals suitable for X-ray diffraction measurements were grown by the slow diffusion of diethyl ether into a mixture of dichloromethane and a minimum of acetonitrile at room temperature.
The positions of the H atoms were generated geometrically (C—H bonds lengths were fixed at 0.96 Å), assigned isotropic displacement parameters and allowed to ride on their respective parent C atoms. The maximum (?) residual electron-density peak was located near the Au atom.
Data collection: SMART (Siemens, 1996); cell refinement: SMART and SAINT (Siemens, 1994); data reduction: XPREP in SHELXTL (Siemens, 1994); program(s) used to solve structure: SHELXTL; program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
![]() | Fig. 1. View of the dication of (I), showing the atomic numbering scheme. Displacement ellipsoids are drawn at the 30% probability level. |
[Au2(C25H22P2)2](PF6)2·2C2H4Cl4 | F(000) = 3136 |
Mr = 1622.46 | Dx = 1.869 Mg m−3 |
Orthorhombic, Pnma | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2n | Cell parameters from 4469 reflections |
a = 20.6825 (10) Å | θ = 1.8–25.1° |
b = 21.0325 (9) Å | µ = 5.51 mm−1 |
c = 13.2577 (6) Å | T = 293 K |
V = 5767.2 (5) Å3 | Block, colorless |
Z = 4 | 0.42 × 0.40 × 0.20 mm |
Siemens SMART CCD diffractometer | 5246 independent reflections |
Radiation source: fine-focus sealed tube | 3249 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.097 |
ω scans | θmax = 25.1°, θmin = 1.8° |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | h = −24→24 |
Tmin = 0.121, Tmax = 0.332 | k = −20→25 |
16736 measured reflections | l = −15→13 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.066 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.160 | H-atom parameters constrained |
S = 1.13 | w = 1[s2(Fo2) + (0.0355P)2 + 11.5869P] where P = (Fo2 + 2Fc2)3 |
5246 reflections | (Δ/σ)max = 0.001 |
361 parameters | Δρmax = 1.79 e Å−3 |
10 restraints | Δρmin = −1.15 e Å−3 |
[Au2(C25H22P2)2](PF6)2·2C2H4Cl4 | V = 5767.2 (5) Å3 |
Mr = 1622.46 | Z = 4 |
Orthorhombic, Pnma | Mo Kα radiation |
a = 20.6825 (10) Å | µ = 5.51 mm−1 |
b = 21.0325 (9) Å | T = 293 K |
c = 13.2577 (6) Å | 0.42 × 0.40 × 0.20 mm |
Siemens SMART CCD diffractometer | 5246 independent reflections |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | 3249 reflections with I > 2σ(I) |
Tmin = 0.121, Tmax = 0.332 | Rint = 0.097 |
16736 measured reflections |
R[F2 > 2σ(F2)] = 0.066 | 10 restraints |
wR(F2) = 0.160 | H-atom parameters constrained |
S = 1.13 | w = 1[s2(Fo2) + (0.0355P)2 + 11.5869P] where P = (Fo2 + 2Fc2)3 |
5246 reflections | Δρmax = 1.79 e Å−3 |
361 parameters | Δρmin = −1.15 e Å−3 |
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. |
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. |
x | y | z | Uiso*/Ueq | ||
Au | 0.89681 (2) | 0.17918 (2) | 0.06337 (4) | 0.03926 (18) | |
Cl1 | 1.0149 (6) | 0.0193 (5) | 0.6436 (7) | 0.217 (5) | |
Cl2 | 1.1365 (4) | −0.0067 (4) | 0.7345 (7) | 0.164 (3) | |
P1 | 0.79368 (14) | 0.17692 (18) | −0.0043 (3) | 0.0394 (8) | |
P2 | 0.99966 (14) | 0.17747 (17) | 0.1328 (2) | 0.0349 (7) | |
P3 | 0.7473 (3) | 0.7500 | 0.8759 (5) | 0.0579 (16) | |
P4 | 0.4626 (3) | 0.7500 | 0.2775 (5) | 0.0674 (19) | |
F11 | 0.7454 (6) | 0.8237 (5) | 0.8747 (8) | 0.105 (4) | |
F12 | 0.7942 (6) | 0.7500 | 0.9696 (9) | 0.082 (4) | |
F13 | 0.8062 (6) | 0.7500 | 0.8012 (10) | 0.108 (6) | |
F14 | 0.7022 (5) | 0.7500 | 0.7778 (9) | 0.079 (4) | |
F15 | 0.6863 (6) | 0.7500 | 0.9475 (10) | 0.094 (5) | |
F21 | 0.4632 (11) | 0.6818 (7) | 0.2741 (19) | 0.303 (17) | |
F22 | 0.5104 (8) | 0.7500 | 0.3672 (12) | 0.211 (15) | |
F23 | 0.5215 (7) | 0.7500 | 0.2021 (11) | 0.121 (6) | |
F24 | 0.4179 (8) | 0.7500 | 0.1869 (15) | 0.31 (3) | |
F25 | 0.4039 (6) | 0.7500 | 0.3539 (11) | 0.128 (7) | |
C1 | 0.7496 (8) | 0.2500 | 0.0251 (14) | 0.038 (5) | |
H1A | 0.7093 | 0.2500 | −0.0123 | 0.046* | |
H1B | 0.7390 | 0.2500 | 0.0963 | 0.046* | |
C01 | 1.0786 (15) | 0.0484 (14) | 0.699 (3) | 0.209 (18) | |
H01A | 1.0647 | 0.0712 | 0.7590 | 0.250* | |
H01B | 1.0986 | 0.0790 | 0.6543 | 0.250* | |
C2 | 1.0434 (8) | 0.2500 | 0.1018 (14) | 0.035 (4) | |
H2A | 1.0843 | 0.2500 | 0.1377 | 0.041* | |
H2B | 1.0529 | 0.2500 | 0.0301 | 0.041* | |
C11 | 0.7452 (6) | 0.1135 (6) | 0.0494 (11) | 0.040 (3) | |
C12 | 0.7378 (8) | 0.1131 (8) | 0.1551 (13) | 0.069 (5) | |
H12A | 0.7565 | 0.1451 | 0.1937 | 0.082* | |
C13 | 0.7032 (9) | 0.0658 (8) | 0.2013 (16) | 0.085 (6) | |
H13A | 0.6957 | 0.0674 | 0.2704 | 0.101* | |
C14 | 0.6794 (10) | 0.0158 (10) | 0.145 (2) | 0.107 (9) | |
H14A | 0.6571 | −0.0171 | 0.1767 | 0.128* | |
C15 | 0.6889 (10) | 0.0150 (8) | 0.0449 (19) | 0.097 (7) | |
H15A | 0.6735 | −0.0192 | 0.0075 | 0.116* | |
C16 | 0.7209 (7) | 0.0635 (7) | −0.0037 (14) | 0.066 (5) | |
H16A | 0.7259 | 0.0622 | −0.0734 | 0.079* | |
C21 | 0.7921 (6) | 0.1684 (6) | −0.1397 (10) | 0.045 (4) | |
C22 | 0.7340 (8) | 0.1692 (8) | −0.1926 (15) | 0.077 (5) | |
H22A | 0.6947 | 0.1723 | −0.1588 | 0.093* | |
C23 | 0.7360 (10) | 0.1652 (8) | −0.2969 (14) | 0.075 (5) | |
H23A | 0.6975 | 0.1672 | −0.3330 | 0.091* | |
C24 | 0.7919 (11) | 0.1586 (8) | −0.3474 (13) | 0.081 (6) | |
H24A | 0.7920 | 0.1555 | −0.4174 | 0.097* | |
C25 | 0.8489 (9) | 0.1566 (8) | −0.2944 (15) | 0.073 (5) | |
H25A | 0.8878 | 0.1524 | −0.3288 | 0.087* | |
C26 | 0.8491 (7) | 0.1607 (7) | −0.1901 (12) | 0.059 (4) | |
H26A | 0.8878 | 0.1581 | −0.1547 | 0.071* | |
C31 | 1.0006 (6) | 0.1692 (7) | 0.2668 (10) | 0.046 (4) | |
C32 | 0.9441 (9) | 0.1680 (8) | 0.3219 (13) | 0.076 (5) | |
H32A | 0.9046 | 0.1701 | 0.2886 | 0.092* | |
C33 | 0.9454 (11) | 0.1637 (10) | 0.4269 (13) | 0.093 (7) | |
H33A | 0.9071 | 0.1630 | 0.4636 | 0.112* | |
C34 | 1.0040 (11) | 0.1606 (9) | 0.4753 (13) | 0.083 (6) | |
H34A | 1.0055 | 0.1588 | 0.5453 | 0.100* | |
C35 | 1.0586 (10) | 0.1602 (9) | 0.4223 (13) | 0.079 (6) | |
H35A | 1.0980 | 0.1566 | 0.4556 | 0.095* | |
C36 | 1.0576 (7) | 0.1650 (8) | 0.3203 (12) | 0.063 (5) | |
H36A | 1.0965 | 0.1655 | 0.2853 | 0.075* | |
C41 | 1.0487 (6) | 0.1122 (6) | 0.0869 (9) | 0.036 (3) | |
C42 | 1.1027 (8) | 0.1183 (8) | 0.0261 (15) | 0.084 (6) | |
H42A | 1.1164 | 0.1580 | 0.0041 | 0.101* | |
C43 | 1.1356 (9) | 0.0639 (11) | −0.0012 (19) | 0.107 (8) | |
H43A | 1.1719 | 0.0684 | −0.0420 | 0.128* | |
C44 | 1.1191 (8) | 0.0067 (9) | 0.0265 (15) | 0.077 (5) | |
H44A | 1.1431 | −0.0285 | 0.0063 | 0.092* | |
C45 | 1.0652 (11) | −0.0004 (9) | 0.0863 (18) | 0.110 (8) | |
H45A | 1.0514 | −0.0406 | 0.1059 | 0.132* | |
C46 | 1.0321 (9) | 0.0530 (8) | 0.1166 (16) | 0.093 (7) | |
H46A | 0.9969 | 0.0481 | 0.1594 | 0.112* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Au | 0.0234 (2) | 0.0362 (3) | 0.0581 (3) | −0.0001 (2) | −0.0057 (2) | −0.0006 (3) |
Cl1 | 0.257 (12) | 0.202 (11) | 0.190 (8) | 0.000 (9) | −0.043 (9) | 0.091 (8) |
Cl2 | 0.160 (7) | 0.145 (7) | 0.186 (7) | 0.003 (6) | 0.057 (6) | 0.023 (6) |
P1 | 0.0210 (16) | 0.0395 (19) | 0.058 (2) | 0.0005 (16) | −0.0047 (15) | −0.0070 (19) |
P2 | 0.0224 (15) | 0.0340 (18) | 0.0484 (19) | −0.0004 (15) | −0.0036 (14) | 0.0018 (18) |
P3 | 0.033 (3) | 0.078 (5) | 0.063 (4) | 0.000 | 0.000 (3) | 0.000 |
P4 | 0.042 (3) | 0.090 (6) | 0.071 (4) | 0.000 | 0.004 (3) | 0.000 |
F11 | 0.132 (10) | 0.091 (9) | 0.092 (8) | −0.014 (8) | −0.022 (7) | 0.002 (7) |
F12 | 0.048 (7) | 0.142 (14) | 0.056 (8) | 0.000 | −0.022 (6) | 0.000 |
F13 | 0.044 (8) | 0.206 (19) | 0.072 (9) | 0.000 | 0.010 (7) | 0.000 |
F14 | 0.045 (7) | 0.123 (12) | 0.070 (9) | 0.000 | −0.018 (7) | 0.000 |
F15 | 0.075 (9) | 0.125 (13) | 0.083 (10) | 0.000 | 0.007 (8) | 0.000 |
F21 | 0.40 (4) | 0.083 (12) | 0.43 (4) | −0.077 (17) | 0.21 (3) | −0.053 (17) |
F22 | 0.077 (13) | 0.49 (5) | 0.069 (11) | 0.000 | −0.007 (10) | 0.000 |
F23 | 0.070 (10) | 0.20 (2) | 0.088 (11) | 0.000 | 0.018 (9) | 0.000 |
F24 | 0.060 (13) | 0.77 (9) | 0.106 (16) | 0.000 | 0.005 (12) | 0.000 |
F25 | 0.054 (9) | 0.24 (2) | 0.093 (11) | 0.000 | 0.012 (9) | 0.000 |
C1 | 0.026 (9) | 0.039 (11) | 0.050 (11) | 0.000 | −0.006 (8) | 0.000 |
C01 | 0.16 (3) | 0.10 (2) | 0.36 (6) | −0.04 (2) | 0.09 (3) | 0.02 (3) |
C2 | 0.020 (9) | 0.029 (10) | 0.055 (12) | 0.000 | 0.008 (8) | 0.000 |
C11 | 0.024 (6) | 0.025 (7) | 0.069 (10) | 0.000 (5) | 0.004 (7) | 0.006 (7) |
C12 | 0.073 (12) | 0.060 (12) | 0.073 (12) | −0.015 (9) | 0.004 (9) | 0.006 (9) |
C13 | 0.096 (14) | 0.052 (11) | 0.106 (15) | −0.007 (11) | 0.025 (12) | 0.024 (11) |
C14 | 0.077 (14) | 0.064 (14) | 0.18 (2) | −0.018 (11) | 0.052 (16) | 0.036 (16) |
C15 | 0.081 (14) | 0.040 (10) | 0.17 (2) | −0.025 (10) | 0.008 (15) | 0.016 (13) |
C16 | 0.067 (11) | 0.041 (10) | 0.089 (12) | −0.016 (8) | −0.005 (10) | −0.012 (9) |
C21 | 0.043 (8) | 0.041 (9) | 0.051 (8) | −0.011 (7) | −0.007 (7) | 0.000 (7) |
C22 | 0.046 (9) | 0.089 (14) | 0.097 (14) | 0.012 (9) | −0.026 (9) | −0.018 (12) |
C23 | 0.096 (14) | 0.070 (13) | 0.061 (12) | 0.014 (11) | −0.032 (11) | −0.004 (10) |
C24 | 0.131 (19) | 0.062 (12) | 0.050 (11) | 0.013 (12) | 0.007 (12) | 0.004 (9) |
C25 | 0.073 (12) | 0.063 (12) | 0.083 (13) | −0.008 (9) | 0.003 (11) | 0.001 (10) |
C26 | 0.050 (9) | 0.070 (12) | 0.058 (10) | −0.010 (8) | 0.011 (8) | −0.006 (9) |
C31 | 0.033 (7) | 0.057 (10) | 0.049 (8) | −0.002 (7) | 0.007 (6) | −0.004 (7) |
C32 | 0.068 (11) | 0.086 (14) | 0.075 (12) | 0.024 (10) | 0.020 (10) | 0.014 (11) |
C33 | 0.098 (15) | 0.123 (19) | 0.059 (12) | 0.046 (13) | 0.022 (11) | 0.018 (12) |
C34 | 0.114 (17) | 0.080 (14) | 0.055 (11) | 0.038 (12) | 0.003 (12) | 0.011 (10) |
C35 | 0.075 (13) | 0.105 (16) | 0.057 (11) | −0.006 (11) | −0.023 (10) | 0.009 (10) |
C36 | 0.039 (8) | 0.094 (14) | 0.055 (10) | −0.002 (8) | −0.006 (7) | 0.005 (9) |
C41 | 0.035 (7) | 0.028 (8) | 0.043 (8) | 0.001 (5) | −0.006 (6) | 0.001 (6) |
C42 | 0.077 (12) | 0.038 (9) | 0.138 (17) | 0.007 (9) | 0.047 (13) | −0.002 (10) |
C43 | 0.073 (13) | 0.082 (16) | 0.17 (2) | 0.004 (12) | 0.051 (14) | −0.017 (15) |
C44 | 0.059 (11) | 0.055 (12) | 0.116 (15) | 0.012 (9) | 0.013 (10) | −0.025 (11) |
C45 | 0.109 (17) | 0.040 (11) | 0.18 (2) | 0.014 (11) | 0.037 (17) | 0.005 (13) |
C46 | 0.095 (14) | 0.045 (11) | 0.139 (17) | 0.015 (10) | 0.056 (13) | 0.001 (11) |
Au—P1 | 2.314 (3) | C14—H14A | 0.9300 |
Au—P2 | 2.318 (3) | C15—C16 | 1.38 (2) |
Au—Aui | 2.9792 (10) | C15—H15A | 0.9300 |
Cl1—C01 | 1.63 (3) | C16—H16A | 0.9300 |
Cl2—C01 | 1.73 (3) | C21—C26 | 1.365 (19) |
P1—C21 | 1.804 (14) | C21—C22 | 1.392 (19) |
P1—C11 | 1.815 (13) | C22—C23 | 1.39 (2) |
P1—C1 | 1.829 (10) | C22—H22A | 0.9300 |
P2—C31 | 1.786 (13) | C23—C24 | 1.34 (2) |
P2—C41 | 1.811 (13) | C23—H23A | 0.9300 |
P2—C2 | 1.821 (9) | C24—C25 | 1.37 (2) |
P3—F11 | 1.551 (11) | C24—H24A | 0.9300 |
P3—F11ii | 1.551 (11) | C25—C26 | 1.38 (2) |
P3—F13 | 1.570 (13) | C25—H25A | 0.9300 |
P3—F12 | 1.577 (12) | C26—H26A | 0.9300 |
P3—F15 | 1.579 (14) | C31—C32 | 1.377 (19) |
P3—F14 | 1.599 (12) | C31—C36 | 1.378 (18) |
P4—F21 | 1.435 (15) | C32—C33 | 1.40 (2) |
P4—F21ii | 1.435 (15) | C32—H32A | 0.9300 |
P4—F24 | 1.516 (19) | C33—C34 | 1.37 (3) |
P4—F22 | 1.547 (16) | C33—H33A | 0.9300 |
P4—F23 | 1.576 (14) | C34—C35 | 1.33 (2) |
P4—F25 | 1.581 (14) | C34—H34A | 0.9300 |
C1—P1i | 1.829 (10) | C35—C36 | 1.36 (2) |
C1—H1A | 0.9700 | C35—H35A | 0.9300 |
C1—H1B | 0.9700 | C36—H36A | 0.9300 |
C01—H01A | 0.9700 | C41—C46 | 1.35 (2) |
C01—H01B | 0.9700 | C41—C42 | 1.383 (19) |
C2—P2i | 1.821 (9) | C42—C43 | 1.38 (2) |
C2—H2A | 0.9700 | C42—H42A | 0.9300 |
C2—H2B | 0.9700 | C43—C44 | 1.30 (3) |
C11—C16 | 1.360 (19) | C43—H43A | 0.9300 |
C11—C12 | 1.41 (2) | C44—C45 | 1.38 (3) |
C12—C13 | 1.37 (2) | C44—H44A | 0.9300 |
C12—H12A | 0.9300 | C45—C46 | 1.37 (2) |
C13—C14 | 1.38 (3) | C45—H45A | 0.9300 |
C13—H13A | 0.9300 | C46—H46A | 0.9300 |
C14—C15 | 1.35 (3) | ||
P1—Au—P2 | 177.85 (13) | C11—C12—H12A | 119.8 |
P1—Au—Aui | 91.18 (10) | C12—C13—C14 | 120.0 (19) |
P2—Au—Aui | 90.89 (9) | C12—C13—H13A | 120.0 |
C21—P1—C11 | 107.9 (7) | C14—C13—H13A | 120.0 |
C21—P1—C1 | 106.6 (8) | C15—C14—C13 | 119.4 (18) |
C11—P1—C1 | 105.0 (6) | C15—C14—H14A | 120.3 |
C21—P1—Au | 113.9 (5) | C13—C14—H14A | 120.3 |
C11—P1—Au | 111.9 (4) | C14—C15—C16 | 122 (2) |
C1—P1—Au | 111.1 (5) | C14—C15—H15A | 119.2 |
C31—P2—C41 | 104.7 (6) | C16—C15—H15A | 119.2 |
C31—P2—C2 | 107.5 (8) | C11—C16—C15 | 120.5 (18) |
C41—P2—C2 | 106.3 (6) | C11—C16—H16A | 119.8 |
C31—P2—Au | 114.0 (4) | C15—C16—H16A | 119.8 |
C41—P2—Au | 113.1 (4) | C26—C21—C22 | 120.0 (14) |
C2—P2—Au | 110.7 (5) | C26—C21—P1 | 118.9 (11) |
F11—P3—F11ii | 176.9 (10) | C22—C21—P1 | 121.1 (12) |
F11—P3—F13 | 90.8 (5) | C23—C22—C21 | 118.5 (17) |
F11ii—P3—F13 | 90.8 (5) | C23—C22—H22A | 120.8 |
F11—P3—F12 | 91.3 (5) | C21—C22—H22A | 120.8 |
F11ii—P3—F12 | 91.3 (5) | C24—C23—C22 | 122.0 (17) |
F13—P3—F12 | 91.0 (7) | C24—C23—H23A | 119.0 |
F11—P3—F15 | 89.2 (5) | C22—C23—H23A | 119.0 |
F11ii—P3—F15 | 89.2 (5) | C23—C24—C25 | 119.1 (17) |
F13—P3—F15 | 177.9 (8) | C23—C24—H24A | 120.4 |
F12—P3—F15 | 91.0 (7) | C25—C24—H24A | 120.4 |
F11—P3—F14 | 88.7 (5) | C24—C25—C26 | 120.8 (18) |
F11ii—P3—F14 | 88.7 (5) | C24—C25—H25A | 119.6 |
F13—P3—F14 | 86.5 (7) | C26—C25—H25A | 119.6 |
F12—P3—F14 | 177.6 (7) | C21—C26—C25 | 119.6 (16) |
F15—P3—F14 | 91.4 (7) | C21—C26—H26A | 120.2 |
F21—P4—F21ii | 176.3 (19) | C25—C26—H26A | 120.2 |
F21—P4—F24 | 88.9 (12) | C32—C31—C36 | 116.9 (14) |
F21ii—P4—F24 | 88.9 (12) | C32—C31—P2 | 121.4 (12) |
F21—P4—F22 | 91.1 (12) | C36—C31—P2 | 121.8 (10) |
F21ii—P4—F22 | 91.1 (12) | C31—C32—C33 | 120.9 (18) |
F24—P4—F22 | 177.8 (10) | C31—C32—H32A | 119.5 |
F21—P4—F23 | 88.5 (8) | C33—C32—H32A | 119.5 |
F21ii—P4—F23 | 88.5 (8) | C34—C33—C32 | 119.1 (18) |
F24—P4—F23 | 88.2 (9) | C34—C33—H33A | 120.5 |
F22—P4—F23 | 89.6 (9) | C32—C33—H33A | 120.5 |
F21—P4—F25 | 91.5 (8) | C35—C34—C33 | 120.2 (16) |
F21ii—P4—F25 | 91.5 (8) | C35—C34—H34A | 119.9 |
F24—P4—F25 | 92.2 (9) | C33—C34—H34A | 119.9 |
F22—P4—F25 | 89.9 (8) | C34—C35—C36 | 120.9 (17) |
F23—P4—F25 | 179.6 (9) | C34—C35—H35A | 119.6 |
P1i—C1—P1 | 114.4 (9) | C36—C35—H35A | 119.6 |
P1i—C1—H1A | 108.7 | C35—C36—C31 | 122.0 (16) |
P1—C1—H1A | 108.7 | C35—C36—H36A | 119.0 |
P1i—C1—H1B | 108.7 | C31—C36—H36A | 119.0 |
P1—C1—H1B | 108.7 | C46—C41—C42 | 117.3 (13) |
H1A—C1—H1B | 107.6 | C46—C41—P2 | 117.3 (11) |
Cl1—C01—Cl2 | 115.5 (18) | C42—C41—P2 | 125.3 (11) |
Cl1—C01—H01A | 108.4 | C43—C42—C41 | 118.4 (16) |
Cl2—C01—H01A | 108.4 | C43—C42—H42A | 120.8 |
Cl1—C01—H01B | 108.4 | C41—C42—H42A | 120.8 |
Cl2—C01—H01B | 108.4 | C44—C43—C42 | 124.2 (19) |
H01A—C01—H01B | 107.5 | C44—C43—H43A | 117.9 |
P2i—C2—P2 | 113.8 (9) | C42—C43—H43A | 117.9 |
P2i—C2—H2A | 108.8 | C43—C44—C45 | 118.3 (17) |
P2—C2—H2A | 108.8 | C43—C44—H44A | 120.8 |
P2i—C2—H2B | 108.8 | C45—C44—H44A | 120.8 |
P2—C2—H2B | 108.8 | C46—C45—C44 | 119.0 (18) |
H2A—C2—H2B | 107.7 | C46—C45—H45A | 120.5 |
C16—C11—C12 | 118.0 (14) | C44—C45—H45A | 120.5 |
C16—C11—P1 | 124.6 (13) | C41—C46—C45 | 122.8 (17) |
C12—C11—P1 | 117.0 (11) | C41—C46—H46A | 118.6 |
C13—C12—C11 | 120.3 (17) | C45—C46—H46A | 118.6 |
C13—C12—H12A | 119.8 |
Symmetry codes: (i) x, −y+1/2, z; (ii) x, −y+3/2, z. |
Experimental details
Crystal data | |
Chemical formula | [Au2(C25H22P2)2](PF6)2·2C2H4Cl4 |
Mr | 1622.46 |
Crystal system, space group | Orthorhombic, Pnma |
Temperature (K) | 293 |
a, b, c (Å) | 20.6825 (10), 21.0325 (9), 13.2577 (6) |
V (Å3) | 5767.2 (5) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 5.51 |
Crystal size (mm) | 0.42 × 0.40 × 0.20 |
Data collection | |
Diffractometer | Siemens SMART CCD diffractometer |
Absorption correction | Empirical (using intensity measurements) (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.121, 0.332 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 16736, 5246, 3249 |
Rint | 0.097 |
(sin θ/λ)max (Å−1) | 0.597 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.066, 0.160, 1.13 |
No. of reflections | 5246 |
No. of parameters | 361 |
No. of restraints | 10 |
H-atom treatment | H-atom parameters constrained |
w = 1[s2(Fo2) + (0.0355P)2 + 11.5869P] where P = (Fo2 + 2Fc2)3 | |
Δρmax, Δρmin (e Å−3) | 1.79, −1.15 |
Computer programs: SMART (Siemens, 1996), SMART and SAINT (Siemens, 1994), XPREP in SHELXTL (Siemens, 1994), SHELXTL.
Au—P1 | 2.314 (3) | P1—C21 | 1.804 (14) |
Au—Aui | 2.9792 (10) | P2—C2 | 1.821 (9) |
P1—Au—P2 | 177.85 (13) | C1—P1—Au | 111.1 (5) |
P1—Au—Aui | 91.18 (10) | C31—P2—C2 | 107.5 (8) |
P2—Au—Aui | 90.89 (9) | C31—P2—Au | 114.0 (4) |
C21—P1—C1 | 106.6 (8) | C41—P2—Au | 113.1 (4) |
C21—P1—Au | 113.9 (5) | C2—P2—Au | 110.7 (5) |
Symmetry code: (i) x, −y+1/2, z. |
Binuclear complexes of gold with certain bidentate ligands are of interest owing to their rich luminescence and bonding properties (Jaw et al., 1989; Khan et al., 1988; King et al., 1989). In this context, several compounds of binuclear [Au2(µ-dppm)2]2+ have been characterized previously (Jaw et al., 1989; Khan et al., 1989; Porter et al., 1989; Liou et al., 1994; Wang et al., 1994; Bauer et al., 1997) counterbalanced by various anionic species. Herein, we described another crystal structure determination of the dication but isolated as the hexafluorophosphate salt, i.e. [Au2(µ-dppm)2](PF6)2·2CH2Cl2, (I) (Fig. 1 and Table 1).
The asymmetric unit of (I) comprises half a dication, [Au2(µ-dppm)2]2+, situated about a twofold axis of symmetry, two independent PF6− anions, each lying on Au gold atoms are doubly bridged by two dppm ligands. The Au center exists in the expected linear geometry with the P1—Au—P2 angle being 177.85 (13)°. The intramolecular Au···Au separation is 2.9792 (10) Å. The overall molecular geometry is in essential agreement with the previously determined structures cited above.