
Acta Cryst. (2008). E64, m99 [ doi:10.1107/S1600536807064458 ]
In the crystal structure of the title compound, [Cu(C18H15As)4]PF6, the Cu atom is coordinated by four As atoms of triphenylarsine ligands in a tetrahedral geometry. The complex cation is located on a crystallographic threefold axis. Both PF6- anions are located on special positions of site symmetry
. The Cu-As bond of the independent arsine ligand is shorter than the Cu-As bonds of the three symmetry-related arsine ligands.
The title compound was isolated as a side-product in the preparation of [(Ph-BIAN)Cu(I)(Ph3As)2][PF6] (Ph-BIAN = Bis(phenyl-imino)acenaphthene). [Cu(NCMe)4]PF6 (50 mg, 0.13 mmol) and Ph3As (93 mg, 0.30 mmol) was stirred in methylene chloride (10 ml) for 2 h. Ph-BIAN (51 mg, 0.15 mmol) was added and stirring was continued for another 2 h. The product was precipitated with pentane. Slow diffusion of diethyl ether into a methylene chloride solution of the product mixture yielded a dark powder and the title compound as colourless crystals. To identify the colourless crystals a single-crystal analysis was performed.
The H-atoms were calculated geometrically and refined using a riding model with C—H = 0.93Å and U(H) = 1.2Ueq(C).
Data collection: IPDS Software (Stoe, 1998); cell refinement: IPDS Software (Stoe, 1998); data reduction: IPDS Software (Stoe, 1998); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 2003); software used to prepare material for publication: PLATON (Spek, 2003).
| Fig. 1. : View of the title compound with the atom numbering scheme. Displacement ellipsoids for non-H atoms are drawn at the 50% probability level. |
| [Cu(C18H15As)4]PF6 | Z = 6 |
| Mr = 1433.40 | F000 = 4332 |
| Trigonal, R3 | Cell parameters were determined by indexing 8000 reflections with I/sigma limit 6.0. |
| Hall symbol: -R 3 | Dx = 1.528 Mg m−3 |
| a = 14.4025 (10) Å | Mo Kα radiation λ = 0.71073 Å |
| b = 14.4025 (10) Å | Cell parameters from 8000 reflections |
| c = 52.015 (4) Å | θ = 2.4–25.9º |
| α = 90º | µ = 2.55 mm−1 |
| β = 90º | T = 296 K |
| γ = 120º | Prism, light yellow, translucent |
| V = 9344.1 (12) Å3 | 0.14 × 0.12 × 0.10 mm |
| Stoe IPDS diffractometer | 4049 independent reflections |
| Radiation source: fine-focus sealed tube | 3118 reflections with I > 2σ(I) |
| Monochromator: graphite | Rint = 0.032 |
| T = 296(1) K | θmax = 25.9º |
| rotation scans | θmin = 2.4º |
| Absorption correction: part of the refinement model (ΔF) refined from delta-F (Walker & Stuart, 1983) | h = −17→17 |
| Tmin = 0.349, Tmax = 0.769 | k = −17→17 |
| 23664 measured reflections | l = −63→61 |
| Refinement on F2 | Secondary atom site location: difference Fourier map |
| Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
| R[F2 > 2σ(F2)] = 0.037 | H-atom parameters constrained |
| wR(F2) = 0.097 | w = 1/[σ2(Fo2) + (0.P)2] where P = (Fo2 + 2Fc2)/3 |
| S = 1.04 | (Δ/σ)max = 0.001 |
| 4049 reflections | Δρmax = 1.77 e Å−3 |
| 254 parameters | Δρmin = −0.62 e Å−3 |
| Primary atom site location: structure-invariant direct methods | Extinction correction: none |
| [Cu(C18H15As)4]PF6 | γ = 120º |
| Mr = 1433.40 | V = 9344.1 (12) Å3 |
| Trigonal, R3 | Z = 6 |
| a = 14.4025 (10) Å | Mo Kα |
| b = 14.4025 (10) Å | µ = 2.55 mm−1 |
| c = 52.015 (4) Å | T = 296 K |
| α = 90º | 0.14 × 0.12 × 0.10 mm |
| β = 90º |
| Stoe IPDS diffractometer | 4049 independent reflections |
| Absorption correction: part of the refinement model (ΔF) refined from delta-F (Walker & Stuart, 1983) | 3118 reflections with I > 2σ(I) |
| Tmin = 0.349, Tmax = 0.769 | Rint = 0.032 |
| 23664 measured reflections |
| R[F2 > 2σ(F2)] = 0.037 | 254 parameters |
| wR(F2) = 0.097 | H-atom parameters constrained |
| S = 1.04 | Δρmax = 1.77 e Å−3 |
| 4049 reflections | Δρmin = −0.62 e Å−3 |
Experimental. Data were collected applying an imaging plate system (Stoe) with the following measurement parameters: Detector distance [mm] 70 Phi movement mode Oscillation Phi incr. [degrees] 1.0 Number of exposures 192 Irradiation / exposure [min] 2.50 For a detailed description of the method see: Sheldrick, G.M., Paulus, E. Vertesy, L. & Hahn, F. (1995) Acta Cryst. B51, 89–98. |
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles |
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 | ||
| As1 | 0.47917 (3) | 0.20088 (3) | 0.06525 (1) | 0.0440 (1) | |
| As2 | 0.66667 | 0.33333 | 0.12958 (1) | 0.0398 (1) | |
| Cu1 | 0.66667 | 0.33333 | 0.08144 (1) | 0.0466 (2) | |
| C1 | 0.4361 (3) | 0.0520 (3) | 0.07350 (6) | 0.0448 (10) | |
| C2 | 0.5099 (3) | 0.0188 (3) | 0.06918 (8) | 0.0610 (14) | |
| C3 | 0.4877 (4) | −0.0818 (4) | 0.07706 (10) | 0.0771 (19) | |
| C4 | 0.3929 (4) | −0.1499 (3) | 0.08911 (9) | 0.0730 (16) | |
| C5 | 0.3189 (4) | −0.1186 (3) | 0.09291 (9) | 0.0699 (16) | |
| C6 | 0.3402 (3) | −0.0175 (3) | 0.08519 (7) | 0.0564 (12) | |
| C7 | 0.4540 (3) | 0.1926 (3) | 0.02816 (6) | 0.0491 (11) | |
| C8 | 0.3857 (4) | 0.0974 (4) | 0.01602 (8) | 0.0779 (18) | |
| C9 | 0.3650 (6) | 0.0970 (5) | −0.00996 (10) | 0.106 (3) | |
| C10 | 0.4128 (6) | 0.1912 (5) | −0.02384 (9) | 0.096 (2) | |
| C11 | 0.4819 (5) | 0.2846 (5) | −0.01205 (9) | 0.082 (2) | |
| C12 | 0.5020 (3) | 0.2858 (3) | 0.01399 (7) | 0.0604 (12) | |
| C13 | 0.3514 (3) | 0.2028 (3) | 0.07735 (6) | 0.0457 (10) | |
| C14 | 0.2602 (3) | 0.1674 (4) | 0.06245 (8) | 0.0648 (14) | |
| C15 | 0.1694 (4) | 0.1644 (4) | 0.07263 (9) | 0.0786 (19) | |
| C16 | 0.1697 (4) | 0.1970 (4) | 0.09752 (9) | 0.0730 (17) | |
| C17 | 0.2590 (4) | 0.2334 (4) | 0.11206 (8) | 0.0699 (16) | |
| C18 | 0.3503 (3) | 0.2367 (3) | 0.10222 (7) | 0.0584 (12) | |
| C19 | 0.7988 (3) | 0.4342 (3) | 0.14716 (6) | 0.0420 (10) | |
| C20 | 0.8947 (3) | 0.4451 (3) | 0.13850 (7) | 0.0541 (11) | |
| C21 | 0.9898 (3) | 0.5153 (3) | 0.15034 (9) | 0.0653 (16) | |
| C22 | 0.9904 (4) | 0.5749 (4) | 0.17108 (9) | 0.0732 (17) | |
| C23 | 0.8955 (4) | 0.5649 (4) | 0.17971 (9) | 0.0786 (17) | |
| C24 | 0.7999 (3) | 0.4955 (3) | 0.16784 (7) | 0.0620 (14) | |
| P1 | 0.00000 | 0.00000 | 0.00000 | 0.0713 (7) | |
| F1 | 0.0013 (5) | 0.0885 (4) | 0.01719 (9) | 0.185 (3) | |
| P2 | 1.33333 | 0.66667 | 0.16667 | 0.0504 (6) | |
| F2 | 1.2304 (2) | 0.6030 (3) | 0.18418 (6) | 0.0990 (11) | |
| H2 | 0.57430 | 0.06430 | 0.06100 | 0.0730* | |
| H3 | 0.53770 | −0.10360 | 0.07420 | 0.0930* | |
| H4 | 0.37920 | −0.21700 | 0.09470 | 0.0880* | |
| H5 | 0.25380 | −0.16520 | 0.10070 | 0.0830* | |
| H6 | 0.28950 | 0.00340 | 0.08790 | 0.0680* | |
| H8 | 0.35360 | 0.03350 | 0.02530 | 0.0940* | |
| H9 | 0.31860 | 0.03270 | −0.01810 | 0.1270* | |
| H10 | 0.39760 | 0.19070 | −0.04120 | 0.1160* | |
| H11 | 0.51590 | 0.34790 | −0.02150 | 0.0990* | |
| H12 | 0.54850 | 0.35030 | 0.02200 | 0.0730* | |
| H14 | 0.25960 | 0.14560 | 0.04560 | 0.0780* | |
| H15 | 0.10820 | 0.14010 | 0.06260 | 0.0940* | |
| H16 | 0.10850 | 0.19410 | 0.10430 | 0.0870* | |
| H17 | 0.25940 | 0.25630 | 0.12880 | 0.0840* | |
| H18 | 0.41120 | 0.26190 | 0.11240 | 0.0700* | |
| H20 | 0.89480 | 0.40460 | 0.12460 | 0.0650* | |
| H21 | 1.05390 | 0.52250 | 0.14430 | 0.0780* | |
| H22 | 1.05460 | 0.62170 | 0.17920 | 0.0880* | |
| H23 | 0.89590 | 0.60540 | 0.19370 | 0.0950* | |
| H24 | 0.73620 | 0.48980 | 0.17370 | 0.0740* |
| U11 | U22 | U33 | U12 | U13 | U23 | |
| As1 | 0.0427 (2) | 0.0399 (2) | 0.0462 (2) | 0.0183 (2) | −0.0025 (1) | −0.0001 (1) |
| As2 | 0.0426 (2) | 0.0426 (2) | 0.0341 (3) | 0.0213 (1) | 0.0000 | 0.0000 |
| Cu1 | 0.0483 (3) | 0.0483 (3) | 0.0431 (4) | 0.0241 (1) | 0.0000 | 0.0000 |
| C1 | 0.0454 (19) | 0.0368 (17) | 0.0476 (17) | 0.0171 (15) | −0.0056 (14) | −0.0021 (13) |
| C2 | 0.051 (2) | 0.050 (2) | 0.081 (3) | 0.0245 (19) | 0.0029 (19) | 0.0043 (19) |
| C3 | 0.079 (3) | 0.063 (3) | 0.106 (4) | 0.048 (3) | 0.000 (3) | 0.002 (2) |
| C4 | 0.087 (3) | 0.043 (2) | 0.087 (3) | 0.031 (2) | −0.010 (2) | 0.003 (2) |
| C5 | 0.064 (3) | 0.047 (2) | 0.083 (3) | 0.016 (2) | 0.012 (2) | 0.012 (2) |
| C6 | 0.050 (2) | 0.045 (2) | 0.070 (2) | 0.0205 (18) | 0.0069 (17) | 0.0076 (17) |
| C7 | 0.049 (2) | 0.053 (2) | 0.0471 (17) | 0.0269 (17) | −0.0011 (14) | −0.0021 (15) |
| C8 | 0.102 (4) | 0.061 (3) | 0.055 (2) | 0.029 (3) | −0.014 (2) | −0.0080 (19) |
| C9 | 0.148 (6) | 0.099 (4) | 0.065 (3) | 0.058 (4) | −0.034 (3) | −0.032 (3) |
| C10 | 0.145 (5) | 0.129 (5) | 0.047 (2) | 0.093 (5) | −0.008 (3) | −0.002 (3) |
| C11 | 0.110 (4) | 0.099 (4) | 0.061 (3) | 0.070 (4) | 0.017 (3) | 0.024 (3) |
| C12 | 0.061 (2) | 0.060 (2) | 0.060 (2) | 0.030 (2) | 0.0038 (18) | 0.0097 (18) |
| C13 | 0.0430 (18) | 0.0395 (18) | 0.0536 (18) | 0.0199 (15) | −0.0032 (14) | 0.0017 (14) |
| C14 | 0.059 (2) | 0.080 (3) | 0.061 (2) | 0.039 (2) | −0.0094 (19) | −0.009 (2) |
| C15 | 0.056 (3) | 0.105 (4) | 0.085 (3) | 0.048 (3) | −0.013 (2) | −0.004 (3) |
| C16 | 0.067 (3) | 0.076 (3) | 0.087 (3) | 0.044 (3) | 0.015 (2) | 0.010 (2) |
| C17 | 0.079 (3) | 0.071 (3) | 0.063 (2) | 0.040 (3) | 0.011 (2) | −0.002 (2) |
| C18 | 0.055 (2) | 0.058 (2) | 0.058 (2) | 0.025 (2) | −0.0021 (17) | −0.0078 (17) |
| C19 | 0.0421 (18) | 0.0405 (17) | 0.0400 (15) | 0.0181 (15) | 0.0002 (13) | 0.0029 (13) |
| C20 | 0.054 (2) | 0.058 (2) | 0.0539 (19) | 0.0306 (19) | −0.0005 (16) | −0.0032 (16) |
| C21 | 0.041 (2) | 0.067 (3) | 0.088 (3) | 0.027 (2) | 0.0015 (19) | 0.005 (2) |
| C22 | 0.054 (3) | 0.065 (3) | 0.093 (3) | 0.024 (2) | −0.020 (2) | −0.014 (2) |
| C23 | 0.067 (3) | 0.080 (3) | 0.081 (3) | 0.031 (3) | −0.020 (2) | −0.039 (2) |
| C24 | 0.051 (2) | 0.069 (3) | 0.062 (2) | 0.027 (2) | −0.0027 (17) | −0.0179 (19) |
| P1 | 0.0817 (12) | 0.0817 (12) | 0.0507 (13) | 0.0409 (6) | 0.0000 | 0.0000 |
| F1 | 0.229 (6) | 0.182 (5) | 0.173 (4) | 0.124 (5) | −0.008 (4) | −0.076 (4) |
| P2 | 0.0409 (7) | 0.0409 (7) | 0.0694 (14) | 0.0205 (4) | 0.0000 | 0.0000 |
| F2 | 0.0655 (17) | 0.101 (2) | 0.117 (2) | 0.0315 (17) | 0.0315 (16) | 0.0196 (18) |
| As1—Cu1 | 2.5472 (5) | C13—C14 | 1.384 (6) |
| As1—C1 | 1.959 (4) | C13—C18 | 1.386 (5) |
| As1—C7 | 1.956 (3) | C14—C15 | 1.391 (8) |
| As1—C13 | 1.958 (5) | C15—C16 | 1.376 (7) |
| As2—Cu1 | 2.5044 (9) | C16—C17 | 1.352 (8) |
| As2—C19 | 1.950 (4) | C17—C18 | 1.390 (8) |
| As2—C19i | 1.950 (5) | C19—C20 | 1.385 (7) |
| As2—C19ii | 1.950 (4) | C19—C24 | 1.387 (5) |
| P1—F1iii | 1.549 (8) | C20—C21 | 1.376 (6) |
| P1—F1iv | 1.549 (5) | C21—C22 | 1.376 (7) |
| P1—F1v | 1.549 (7) | C22—C23 | 1.376 (9) |
| P1—F1vi | 1.549 (8) | C23—C24 | 1.378 (7) |
| P1—F1vii | 1.549 (7) | C2—H2 | 0.9300 |
| P1—F1 | 1.549 (5) | C3—H3 | 0.9300 |
| P2—F2viii | 1.584 (5) | C4—H4 | 0.9300 |
| P2—F2 | 1.584 (3) | C5—H5 | 0.9300 |
| P2—F2ix | 1.583 (5) | C6—H6 | 0.9300 |
| P2—F2x | 1.585 (3) | C8—H8 | 0.9300 |
| P2—F2xi | 1.584 (3) | C9—H9 | 0.9300 |
| P2—F2xii | 1.584 (3) | C10—H10 | 0.9300 |
| C1—C2 | 1.385 (7) | C11—H11 | 0.9300 |
| C1—C6 | 1.377 (6) | C12—H12 | 0.9300 |
| C2—C3 | 1.381 (6) | C14—H14 | 0.9300 |
| C3—C4 | 1.371 (8) | C15—H15 | 0.9300 |
| C4—C5 | 1.363 (8) | C16—H16 | 0.9300 |
| C5—C6 | 1.389 (6) | C17—H17 | 0.9300 |
| C7—C8 | 1.378 (6) | C18—H18 | 0.9300 |
| C7—C12 | 1.377 (5) | C20—H20 | 0.9300 |
| C8—C9 | 1.383 (7) | C21—H21 | 0.9300 |
| C9—C10 | 1.379 (8) | C22—H22 | 0.9300 |
| C10—C11 | 1.356 (9) | C23—H23 | 0.9300 |
| C11—C12 | 1.383 (6) | C24—H24 | 0.9300 |
| As1···H2ii | 3.1700 | C14···H9vi | 3.0700 |
| Cu1···H2 | 3.5700 | C19···H24ii | 2.6000 |
| Cu1···H12 | 3.6000 | C19···H18ii | 2.6700 |
| Cu1···H18 | 3.6600 | C20···H24ii | 3.0000 |
| Cu1···H20 | 3.6800 | C20···H18ii | 2.8000 |
| Cu1···H2i | 3.5700 | C21···H22x | 2.9700 |
| Cu1···H12i | 3.6000 | C24···H24ii | 3.0700 |
| Cu1···H18i | 3.6600 | H2···Cu1 | 3.5700 |
| Cu1···H20i | 3.6800 | H2···C13i | 2.9300 |
| Cu1···H2ii | 3.5700 | H2···As1i | 3.1700 |
| Cu1···H12ii | 3.6000 | H3···H10xiii | 2.5600 |
| Cu1···H18ii | 3.6600 | H4···H4xiv | 2.5300 |
| Cu1···H20ii | 3.6800 | H4···H4xv | 2.5300 |
| F2···C22 | 3.343 (7) | H6···C14 | 2.9200 |
| F1···H14vii | 2.7500 | H6···C13 | 2.6000 |
| F1···H15 | 2.7100 | H8···C1 | 2.7300 |
| F2···H22 | 2.6900 | H8···C11v | 3.0300 |
| C6···C14 | 3.590 (7) | H9···C14v | 3.0700 |
| C8···C14 | 3.455 (7) | H10···H3xiii | 2.5600 |
| C14···C8 | 3.455 (7) | H12···Cu1 | 3.6000 |
| C14···C6 | 3.590 (7) | H12···C12ii | 3.0000 |
| C18···C19i | 3.574 (6) | H12···C7ii | 2.8000 |
| C18···C20i | 3.551 (6) | H14···C7 | 2.6900 |
| C19···C18ii | 3.574 (5) | H14···C8 | 2.7200 |
| C20···C24ii | 3.590 (6) | H14···F1iii | 2.7500 |
| C20···C18ii | 3.551 (6) | H15···F1 | 2.7100 |
| C22···F2 | 3.343 (7) | H18···C20i | 2.8000 |
| C24···C20i | 3.590 (7) | H18···Cu1 | 3.6600 |
| C1···H8 | 2.7300 | H18···C19i | 2.6700 |
| C1···H20ii | 2.8200 | H20···C1i | 2.8200 |
| C6···H20ii | 3.0000 | H20···C6i | 3.0000 |
| C7···H12i | 2.8000 | H20···Cu1 | 3.6800 |
| C7···H14 | 2.6900 | H21···H22x | 2.3900 |
| C8···H14 | 2.7200 | H22···F2 | 2.6900 |
| C11···H8vi | 3.0300 | H22···C21ix | 2.9700 |
| C12···H12i | 3.0000 | H22···H21ix | 2.3900 |
| C13···H6 | 2.6000 | H24···C20i | 3.0000 |
| C13···H2ii | 2.9300 | H24···C24i | 3.0700 |
| C14···H6 | 2.9200 | H24···C19i | 2.6000 |
| Cu1—As1—C1 | 112.61 (13) | C8—C9—C10 | 120.5 (5) |
| Cu1—As1—C7 | 117.80 (13) | C9—C10—C11 | 119.8 (5) |
| Cu1—As1—C13 | 122.35 (11) | C10—C11—C12 | 120.0 (5) |
| C1—As1—C7 | 101.64 (15) | C7—C12—C11 | 120.8 (4) |
| C1—As1—C13 | 99.19 (17) | As1—C13—C18 | 118.8 (3) |
| C7—As1—C13 | 99.85 (17) | C14—C13—C18 | 118.5 (4) |
| Cu1—As2—C19 | 117.96 (10) | As1—C13—C14 | 122.7 (3) |
| Cu1—As2—C19i | 117.96 (11) | C13—C14—C15 | 120.2 (4) |
| Cu1—As2—C19ii | 117.96 (10) | C14—C15—C16 | 120.3 (5) |
| C19—As2—C19i | 99.81 (18) | C15—C16—C17 | 119.9 (6) |
| C19—As2—C19ii | 99.81 (18) | C16—C17—C18 | 120.5 (4) |
| C19i—As2—C19ii | 99.8 (2) | C13—C18—C17 | 120.6 (4) |
| As1—Cu1—As2 | 109.30 (2) | As2—C19—C24 | 122.3 (4) |
| As1—Cu1—As1i | 109.65 (2) | C20—C19—C24 | 119.1 (4) |
| As1—Cu1—As1ii | 109.65 (2) | As2—C19—C20 | 118.6 (3) |
| As1i—Cu1—As2 | 109.30 (2) | C19—C20—C21 | 120.5 (4) |
| As1ii—Cu1—As2 | 109.30 (2) | C20—C21—C22 | 120.2 (5) |
| As1i—Cu1—As1ii | 109.65 (2) | C21—C22—C23 | 119.6 (5) |
| F1vii—P1—F1iv | 90.0 (3) | C22—C23—C24 | 120.6 (4) |
| F1vii—P1—F1v | 180.00 | C19—C24—C23 | 119.9 (5) |
| F1vii—P1—F1vi | 90.0 (3) | C1—C2—H2 | 120.00 |
| F1iii—P1—F1iv | 90.0 (3) | C3—C2—H2 | 120.00 |
| F1iii—P1—F1v | 90.0 (3) | C4—C3—H3 | 120.00 |
| F1iii—P1—F1vi | 180.00 | C2—C3—H3 | 120.00 |
| F1iv—P1—F1v | 90.0 (3) | C3—C4—H4 | 120.00 |
| F1iv—P1—F1vi | 90.0 (3) | C5—C4—H4 | 120.00 |
| F1v—P1—F1vi | 90.0 (3) | C4—C5—H5 | 120.00 |
| F1—P1—F1vii | 90.0 (3) | C6—C5—H5 | 120.00 |
| F1—P1—F1iii | 90.0 (3) | C1—C6—H6 | 120.00 |
| F1—P1—F1iv | 180.00 | C5—C6—H6 | 120.00 |
| F1—P1—F1v | 90.0 (3) | C9—C8—H8 | 120.00 |
| F1—P1—F1vi | 90.0 (3) | C7—C8—H8 | 120.00 |
| F1vii—P1—F1iii | 90.0 (3) | C8—C9—H9 | 120.00 |
| F2viii—P2—F2ix | 180.00 | C10—C9—H9 | 120.00 |
| F2viii—P2—F2x | 89.8 (2) | C11—C10—H10 | 120.00 |
| F2xi—P2—F2xii | 89.8 (2) | C9—C10—H10 | 120.00 |
| F2xi—P2—F2ix | 89.8 (2) | C10—C11—H11 | 120.00 |
| F2xi—P2—F2x | 180.00 | C12—C11—H11 | 120.00 |
| F2xii—P2—F2ix | 90.2 (2) | C7—C12—H12 | 120.00 |
| F2xii—P2—F2x | 90.2 (2) | C11—C12—H12 | 120.00 |
| F2ix—P2—F2x | 90.2 (2) | C15—C14—H14 | 120.00 |
| F2viii—P2—F2xii | 89.8 (2) | C13—C14—H14 | 120.00 |
| F2—P2—F2viii | 90.2 (2) | C16—C15—H15 | 120.00 |
| F2—P2—F2xi | 90.2 (2) | C14—C15—H15 | 120.00 |
| F2—P2—F2xii | 180.00 | C15—C16—H16 | 120.00 |
| F2—P2—F2ix | 89.8 (2) | C17—C16—H16 | 120.00 |
| F2—P2—F2x | 89.8 (2) | C16—C17—H17 | 120.00 |
| F2viii—P2—F2xi | 90.2 (2) | C18—C17—H17 | 120.00 |
| C2—C1—C6 | 119.0 (4) | C17—C18—H18 | 120.00 |
| As1—C1—C2 | 117.7 (3) | C13—C18—H18 | 120.00 |
| As1—C1—C6 | 123.1 (3) | C19—C20—H20 | 120.00 |
| C1—C2—C3 | 120.0 (4) | C21—C20—H20 | 120.00 |
| C2—C3—C4 | 120.8 (5) | C22—C21—H21 | 120.00 |
| C3—C4—C5 | 119.6 (4) | C20—C21—H21 | 120.00 |
| C4—C5—C6 | 120.4 (4) | C21—C22—H22 | 120.00 |
| C1—C6—C5 | 120.3 (5) | C23—C22—H22 | 120.00 |
| As1—C7—C8 | 122.1 (3) | C24—C23—H23 | 120.00 |
| C8—C7—C12 | 119.1 (3) | C22—C23—H23 | 120.00 |
| As1—C7—C12 | 118.8 (3) | C23—C24—H24 | 120.00 |
| C7—C8—C9 | 119.8 (5) | C19—C24—H24 | 120.00 |
| C1—As1—Cu1—As2 | −66.60 (12) | Cu1—As2—C19—C24 | 134.7 (3) |
| C7—As1—Cu1—As2 | 175.59 (14) | C19i—As2—C19—C24 | 5.6 (3) |
| C13—As1—Cu1—As2 | 51.33 (12) | C19ii—As2—C19—C24 | −96.2 (3) |
| C1—As1—Cu1—As1i | 53.18 (12) | As1—C1—C2—C3 | 173.5 (3) |
| C7—As1—Cu1—As1i | −64.63 (15) | As1—C1—C6—C5 | −173.4 (3) |
| C13—As1—Cu1—As1i | 171.12 (12) | C2—C1—C6—C5 | 1.1 (6) |
| C1—As1—Cu1—As1ii | 173.61 (12) | C6—C1—C2—C3 | −1.4 (6) |
| C7—As1—Cu1—As1ii | 55.80 (15) | C1—C2—C3—C4 | 0.2 (7) |
| C13—As1—Cu1—As1ii | −68.45 (13) | C2—C3—C4—C5 | 1.3 (7) |
| C13—As1—C1—C2 | −176.1 (3) | C3—C4—C5—C6 | −1.5 (7) |
| Cu1—As1—C1—C6 | 129.4 (3) | C4—C5—C6—C1 | 0.3 (6) |
| Cu1—As1—C13—C14 | 151.9 (3) | C12—C7—C8—C9 | −1.1 (9) |
| C1—As1—C13—C14 | −83.8 (4) | As1—C7—C8—C9 | 175.6 (6) |
| C7—As1—C13—C14 | 19.8 (4) | C8—C7—C12—C11 | 0.3 (8) |
| Cu1—As1—C1—C2 | −45.2 (3) | As1—C7—C12—C11 | −176.5 (5) |
| C7—As1—C1—C2 | 81.8 (3) | C7—C8—C9—C10 | 0.4 (12) |
| C13—As1—C7—C8 | −80.5 (5) | C8—C9—C10—C11 | 1.1 (13) |
| Cu1—As1—C7—C12 | −38.7 (4) | C9—C10—C11—C12 | −1.8 (13) |
| C7—As1—C1—C6 | −103.6 (3) | C10—C11—C12—C7 | 1.2 (10) |
| C13—As1—C1—C6 | −1.5 (3) | As1—C13—C14—C15 | 176.0 (4) |
| C13—As1—C7—C12 | 96.2 (4) | C14—C13—C18—C17 | 1.1 (6) |
| Cu1—As1—C7—C8 | 144.6 (4) | C18—C13—C14—C15 | −1.2 (7) |
| C1—As1—C7—C8 | 21.1 (5) | As1—C13—C18—C17 | −176.2 (3) |
| C1—As1—C13—C18 | 93.4 (3) | C13—C14—C15—C16 | 0.3 (7) |
| Cu1—As1—C13—C18 | −30.9 (3) | C14—C15—C16—C17 | 0.8 (8) |
| C1—As1—C7—C12 | −162.2 (4) | C15—C16—C17—C18 | −1.0 (7) |
| C7—As1—C13—C18 | −163.0 (3) | C16—C17—C18—C13 | 0.0 (7) |
| C19ii—As2—C19—C20 | 84.2 (3) | As2—C19—C20—C21 | −180.0 (3) |
| C19ii—As2—Cu1—As1 | 63.5 (2) | C24—C19—C20—C21 | 0.4 (6) |
| C19—As2—Cu1—As1 | −176.49 (15) | As2—C19—C24—C23 | 179.4 (3) |
| C19—As2—Cu1—As1ii | −56.49 (15) | C20—C19—C24—C23 | −1.0 (6) |
| C19i—As2—Cu1—As1 | −56.49 (17) | C19—C20—C21—C22 | 0.5 (6) |
| C19—As2—Cu1—As1i | 63.51 (15) | C20—C21—C22—C23 | −0.8 (7) |
| Cu1—As2—C19—C20 | −44.9 (3) | C21—C22—C23—C24 | 0.2 (7) |
| C19i—As2—C19—C20 | −174.0 (3) | C22—C23—C24—C19 | 0.7 (7) |
| Symmetry codes: (i) −y+1, x−y, z; (ii) −x+y+1, −x+1, z; (iii) −x+y, −x, z; (iv) −x, −y, −z; (v) y, −x+y, −z; (vi) x−y, x, −z; (vii) −y, x−y, z; (viii) −y+2, x−y, z; (ix) y+2/3, −x+y+4/3, −z+1/3; (x) x−y+2/3, x−2/3, −z+1/3; (xi) −x+y+2, −x+2, z; (xii) −x+8/3, −y+4/3, −z+1/3; (xiii) −x+1, −y, −z; (xiv) −y, x−y−1, z; (xv) −x+y+1, −x, z. |
| As1—Cu1 | 2.5472 (5) | As2—Cu1 | 2.5044 (9) |
| As1—C1 | 1.959 (4) | As2—C19 | 1.950 (4) |
| As1—C7 | 1.956 (3) | P1—F1 | 1.549 (5) |
| As1—C13 | 1.958 (5) | P2—F2 | 1.584 (3) |
| Cu1—As1—C1 | 112.61 (13) | As1—Cu1—As1i | 109.65 (2) |
| Cu1—As1—C7 | 117.80 (13) | F1ii—P1—F1iii | 90.0 (3) |
| Cu1—As1—C13 | 122.35 (11) | F2iv—P2—F2v | 180.00 |
| C1—As1—C7 | 101.64 (15) | As1—C1—C2 | 117.7 (3) |
| C1—As1—C13 | 99.19 (17) | As1—C7—C8 | 122.1 (3) |
| C7—As1—C13 | 99.85 (17) | As1—C13—C18 | 118.8 (3) |
| Cu1—As2—C19 | 117.96 (10) | As2—C19—C24 | 122.3 (4) |
| C19—As2—C19i | 99.81 (18) | As2—C19—C20 | 118.6 (3) |
| As1—Cu1—As2 | 109.30 (2) |
| Symmetry codes: (i) −y+1, x−y, z; (ii) −y, x−y, z; (iii) −x, −y, −z; (iv) −x+y+2, −x+2, z; (v) x−y+2/3, x−2/3, −z+1/3. |
Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115–119.
Bowmaker, G. A., Healy, P. C., Engelhardt, L. M., Kildea, J. D., Skelton, B. W. & White, A. H. (1990). Aust. J. Chem. 43, 1697–1705.
Engelhardt, L. M., Pakawatchai, C., White, A. H. & Healy, P. C. (1985). J. Chem. Soc. Dalton Trans. pp. 125–133.
Sheldrick, G. M. (1997). SHELXL97. University of Göttingen, Germany.
Spek, A. L. (2003). J. Appl. Cryst. 36, 7–13.
Stoe (1998). IPDS Software. Version 2.89. Stoe & Cie GmbH, Darmstadt, Germany.
Walker, N. & Stuart, D. (1983). Acta Cryst. A39, 158–166.
Crystals of the title compound were obtained as a side-product in the preparation of [(Ph-BIAN)Cu(I)(Ph3As)2][PF6] (Ph-BIAN = Bis(phenyl-imino)acenaphthene) in methylene chloride solution. To identify this compound a single-crystal structure analysis was performed.
The title compound contains [(Ph3As)4Cu]+ ions which are disposed about crystallographic threefold axes, the metal atom lying on a special position of symmetry 3 is coordinated by two independent ligands. One of it is totally independent, whereas the other three are symmetry-related completing the nearly regular tetrahedral environment of the copper atom. The bond angles are 109.30 (2) and 109.65 (2) ° for As1—Cu1—As2 and As1—Cu1—As1', respectively. Two independent phosphorus and fluorine atoms are found. The Cu—As2 bond of the independent (axial) arsine ligand is significantly shorter than the value for the off-axis Cu—As1 bonds (2.5044 (9) versus 2.5472 (5) Å). A similar distortion was previously found for the analogous salts [(Ph3P)4Cu]+ (with ClO4- or PF6- as anions), which also crystallize in the same space group (Bowmaker et al., 1990, Engelhardt et al., 1985).