metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

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ISSN: 2056-9890

{Bis[2-(di­phenyl­phosphino)eth­yl]phenyl­phosphine-κ3P,P′,P′′}chloridopalladium(II) hexa­fluoridophosphate

aChemistry Department, Fort Lewis College, 1000 Rim Drive, Durango, CO 81301, USA, and bChemistry Department, Colorado State University, Fort Collins, CO 80523, USA
*Correspondence e-mail: helm_m@fortlewis.edu

(Received 28 May 2009; accepted 11 June 2009; online 20 June 2009)

In the title compound, [PdCl(C34H33P3)]PF6, the PdII atom adopts a distorted PdP3Cl square-planar geometry arising from the P,P′,P′′-tridentate triphos ligand and a chloride ion.

Related literature

For the synthesis, see: King et al. (1971[King, R. B., Kapoor, P. N. & Kapoor, R. N. (1971). Inorg. Chem. 10, 1841-1850.]). The corresponding complex with a PtII metal center is concurently published (Heston et al., 2009[Heston, S. A., Noll, B. C. & Helm, M. L. (2009). Acta Cryst. E65, m793.]). The corresponding PdII complex has been previously reported as a trifluoro­methane­sulfonate salt (Müller et al., 2000[Müller, T. E., Grosche, M., Herdtweck, E., Pleier, A.-K., Walter, E. & Yaw-Kai, Y. (2000). Organometallics, 19, 170-183.]). The corresponding complexes with both PtII and PdII have been previously reported as chloride and diphenyl­tetra­chlorido­stannate(IV) salts (Sevillano et al., 1999a[Sevillano, P., Habtemariam, A., Parsons, S., Castineiras, A., Garcia, M. E. & Sadler, P. J. (1999a). J. Chem. Soc. Dalton Trans. pp. 2861-2870.]; Garcia-Seijo et al., 2001[Garcia-Seijo, M. I., Castineiras, A., Mahieu, B., Janosi, L., Berente, Z., Kollar, L. & Garcia-Fernandez, M. E. (2001). Polyhedron, 20, 855-868.]; Housecroft et al., 1990[Housecroft, C. E., Shaykh, B. A. M., Rheingold, A. L. & Haggerty, B. S. (1990). Acta Cryst. C46, 1549-1551.]). For other group 10–triphos complexes, see: Sevillano et al. (1999b[Sevillano, P., Habtemariam, A., Parsons, S., Castineiras, A., Garcia, M. E. & Sadler, P. J. (1999b). Polyhedron, 18, 383-389.]); Fernadez et al. (2005); Aizawa et al. (2002[Aizawa, S., Sone, Y., Kawamoto, T., Yamada, S. & Nakamura, M. (2002). Inorg. Chim. Acta, 338, 235-239.]); Bertinsson et al. (1983[Bertinsson, G.-I. (1983). Acta Cryst. C39, 563-567.]); Autissier et al. (2005[Autissier, V., Brockman, E., Clegg, W., Harrington, R. W. & Henderson, R. A. (2005). J. Organomet. Chem. 690, 1763-1771.]); Fernandez et al. (2005[Fernandez, D., Garcia-Seijo, M. I., Sevillano, P., Castineiras, A. & Garcia-Fernandez, M. E. (2005). Inorg. Chim. Acta, 358, 2575-2584.]).

[Scheme 1]

Experimental

Crystal data
  • [PdCl(C34H33P3)]PF6

  • Mr = 821.33

  • Triclinic, [P \overline 1]

  • a = 11.2465 (5) Å

  • b = 11.8182 (5) Å

  • c = 15.5093 (7) Å

  • α = 69.029 (2)°

  • β = 70.439 (2)°

  • γ = 69.697 (2)°

  • V = 1752.27 (13) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 0.84 mm−1

  • T = 100 K

  • 0.47 × 0.15 × 0.10 mm

Data collection
  • Bruker APEXII CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2000[Bruker (2000). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.693, Tmax = 0.917

  • 48576 measured reflections

  • 13341 independent reflections

  • 10917 reflections with I > 2σ(I)

  • Rint = 0.030

Refinement
  • R[F2 > 2σ(F2)] = 0.031

  • wR(F2) = 0.067

  • S = 1.03

  • 13341 reflections

  • 415 parameters

  • H-atom parameters constrained

  • Δρmax = 0.71 e Å−3

  • Δρmin = −0.67 e Å−3

Table 1
Selected bond lengths (Å)

Pd1—P1 2.2176 (4)
Pd1—P2 2.3178 (4)
Pd1—P3 2.3329 (4)
Pd1—Cl1 2.3441 (4)

Data collection: APEX2 (Bruker, 2006[Bruker (2006). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2006[Bruker (2006). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXTL.

Supporting information


Comment top

The crystal structure of the title compound, (I), consists of a [Pd(triphos)Cl]+ cation and PF6- anion (Fig. 1). The cation shows a distorted square planar geometry around the metal center and the charge is balanced by a non-coordinating PF6- anion.

Related literature top

For the synthesis, see: King et al. (1971). The corresponding complex with a Pt(II) metal center is concurently published (Heston et al., 2009). The corresponding PdII complex has been previously reported as a trifluoromethanesulfonate salt (Muller et al., 2000). The corresponding complexes with both Pt(II) and PdII have been previously reported as chloride and diphenyltetrachlorostannate(IV) salts (Sevillano et al., 1999a; Garcia-Seijo et al., 2001; Housecroft et al., 1990). For other group 10–triphos complexes, see: Sevillano et al. (1999b); Fernadez et al. (2005); Aizawa et al. (2002); Bertinsson et al. (1983); Autissier et al. (2005). For related literature, see: Fernandez et al. (2005).

Experimental top

The title compound was prepared by a previously reported proceedure (King, et al., 1971). Colourless rods of (I) were grown by slow solvent evaporation of a saturated dichloromethane solution.

Refinement top

All H atoms were placed in calculated positions (C—H = 0.93–0.97Å) and refined as riding with Uiso(H) = 1.2Ueq(C).

Computing details top

Data collection: APEX2 (Bruker, 2006); cell refinement: SAINT (Bruker, 2006); data reduction: SAINT (Bruker, 2006; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The molecular structure of (I) with 50% probability displacement ellipsoids.
[Figure 2] Fig. 2. The molecular structure of (I), with atom labels and 50% probability displacement ellipsoids. Hydrogen atoms are omitted for clarity.
{Bis[2-(diphenylphosphino)ethyl]phenylphosphine-κ3P,P',P''}chloridopalladium(II) hexafluoridophosphate top
Crystal data top
[PdCl(C34H33P3)]PF6Z = 2
Mr = 821.33F(000) = 828
Triclinic, P1Dx = 1.557 Mg m3
Hall symbol: -P 1Melting point: not measured K
a = 11.2465 (5) ÅMo Kα radiation, λ = 0.71073 Å
b = 11.8182 (5) ÅCell parameters from 9890 reflections
c = 15.5093 (7) Åθ = 2.7–33.3°
α = 69.029 (2)°µ = 0.84 mm1
β = 70.439 (2)°T = 100 K
γ = 69.697 (2)°Rod, colourless
V = 1752.27 (13) Å30.47 × 0.15 × 0.10 mm
Data collection top
Bruker APEXII CCD
diffractometer
13341 independent reflections
Radiation source: fine-focus sealed tube10917 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.030
ϕ and ω scansθmax = 33.4°, θmin = 1.9°
Absorption correction: multi-scan
(SADABS; Bruker, 2000)
h = 1617
Tmin = 0.693, Tmax = 0.917k = 1818
48576 measured reflectionsl = 2321
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)] = 0.031Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.067H-atom parameters constrained
S = 1.03 w = 1/[σ2(Fo2) + (0.0249P)2 + 0.7353P]
where P = (Fo2 + 2Fc2)/3
13341 reflections(Δ/σ)max = 0.002
415 parametersΔρmax = 0.71 e Å3
0 restraintsΔρmin = 0.67 e Å3
Crystal data top
[PdCl(C34H33P3)]PF6γ = 69.697 (2)°
Mr = 821.33V = 1752.27 (13) Å3
Triclinic, P1Z = 2
a = 11.2465 (5) ÅMo Kα radiation
b = 11.8182 (5) ŵ = 0.84 mm1
c = 15.5093 (7) ÅT = 100 K
α = 69.029 (2)°0.47 × 0.15 × 0.10 mm
β = 70.439 (2)°
Data collection top
Bruker APEXII CCD
diffractometer
13341 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2000)
10917 reflections with I > 2σ(I)
Tmin = 0.693, Tmax = 0.917Rint = 0.030
48576 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0310 restraints
wR(F2) = 0.067H-atom parameters constrained
S = 1.03Δρmax = 0.71 e Å3
13341 reflectionsΔρmin = 0.67 e Å3
415 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.

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*/Ueq
Pd10.543690 (10)0.544468 (10)0.728992 (7)0.01221 (3)
Cl10.66556 (3)0.69224 (3)0.64082 (3)0.01911 (7)
P10.41725 (3)0.41349 (3)0.80705 (3)0.01332 (7)
P20.34703 (3)0.69724 (3)0.73350 (3)0.01374 (7)
P30.71382 (3)0.36524 (3)0.75901 (3)0.01384 (7)
C10.63963 (14)0.23211 (14)0.82230 (11)0.0178 (3)
H1A0.63340.19640.77560.021*
H1B0.69560.16580.86310.021*
C20.50294 (14)0.27458 (14)0.88395 (11)0.0177 (3)
H2A0.50890.29480.93880.021*
H2B0.45660.20770.90820.021*
C30.26481 (14)0.49798 (14)0.87132 (11)0.0182 (3)
H3A0.20090.44650.90030.022*
H3B0.28000.51910.92240.022*
C40.21432 (13)0.61759 (14)0.79763 (11)0.0184 (3)
H4A0.13790.67360.82970.022*
H4B0.18690.59620.75230.022*
C50.32177 (14)0.80673 (14)0.79914 (10)0.0156 (3)
C60.19906 (14)0.89177 (15)0.81373 (11)0.0197 (3)
H6A0.13150.88930.79110.024*
C70.17601 (16)0.97952 (16)0.86117 (12)0.0242 (3)
H7A0.09251.03700.87130.029*
C80.27491 (17)0.98361 (16)0.89391 (12)0.0261 (4)
H8A0.25911.04440.92600.031*
C90.39634 (16)0.89942 (17)0.87998 (12)0.0250 (3)
H9A0.46340.90220.90290.030*
C100.42046 (15)0.81067 (15)0.83243 (11)0.0207 (3)
H10A0.50390.75310.82280.025*
C110.31785 (13)0.79486 (14)0.61900 (10)0.0158 (3)
C120.35593 (15)0.90719 (15)0.57975 (11)0.0193 (3)
H12A0.38970.93380.61560.023*
C130.34469 (16)0.97972 (16)0.48887 (12)0.0259 (4)
H13A0.37101.05570.46250.031*
C140.29516 (17)0.94151 (18)0.43648 (12)0.0305 (4)
H14A0.28720.99130.37420.037*
C150.25735 (19)0.8311 (2)0.47485 (13)0.0337 (4)
H15A0.22280.80550.43890.040*
C160.26919 (17)0.75693 (18)0.56544 (13)0.0271 (4)
H16A0.24410.68030.59090.033*
C170.79995 (13)0.37155 (14)0.83702 (10)0.0156 (3)
C180.81699 (16)0.48626 (15)0.82975 (12)0.0222 (3)
H18A0.77790.56080.78800.027*
C190.89105 (16)0.49210 (16)0.88346 (13)0.0245 (3)
H19A0.90260.57050.87810.029*
C200.94768 (14)0.38410 (15)0.94455 (11)0.0200 (3)
H20A0.99810.38830.98120.024*
C210.93115 (15)0.26977 (16)0.95254 (11)0.0211 (3)
H21A0.97080.19560.99430.025*
C220.85680 (15)0.26298 (15)0.89975 (11)0.0201 (3)
H22A0.84460.18450.90620.024*
C230.84173 (13)0.31713 (15)0.66107 (11)0.0173 (3)
C240.85893 (17)0.40133 (16)0.57143 (12)0.0253 (3)
H24A0.80390.48430.56120.030*
C250.95762 (18)0.36365 (18)0.49618 (13)0.0327 (4)
H25A0.97000.42110.43470.039*
C261.03721 (16)0.24272 (18)0.51127 (14)0.0304 (4)
H26A1.10420.21730.46000.037*
C271.01997 (16)0.15849 (18)0.60052 (13)0.0286 (4)
H27A1.07470.07540.61020.034*
C280.92312 (15)0.19491 (16)0.67579 (12)0.0231 (3)
H28A0.91190.13720.73720.028*
C290.37076 (14)0.36381 (14)0.72824 (11)0.0170 (3)
C300.43949 (16)0.37635 (18)0.63357 (12)0.0264 (4)
H30A0.51370.40950.61000.032*
C310.40025 (19)0.3407 (2)0.57341 (13)0.0337 (4)
H31A0.44830.34840.50910.040*
C320.29116 (19)0.29404 (19)0.60692 (13)0.0313 (4)
H32A0.26420.27020.56550.038*
C330.2214 (2)0.2821 (2)0.70068 (14)0.0359 (5)
H33A0.14590.25110.72330.043*
C340.26129 (17)0.31525 (18)0.76138 (12)0.0289 (4)
H34A0.21420.30500.82600.035*
P40.21871 (4)0.13320 (4)1.11479 (3)0.01765 (8)
F10.14268 (9)0.04474 (9)1.10733 (7)0.0233 (2)
F20.23404 (11)0.04420 (10)1.21717 (7)0.0334 (2)
F30.35426 (8)0.05090 (9)1.06650 (7)0.0241 (2)
F40.29314 (10)0.22256 (10)1.12031 (9)0.0334 (3)
F50.20332 (10)0.22185 (10)1.01037 (8)0.0341 (3)
F60.08134 (9)0.21610 (10)1.16043 (9)0.0359 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pd10.01063 (5)0.00951 (5)0.01375 (5)0.00185 (3)0.00232 (3)0.00135 (4)
Cl10.01759 (15)0.01486 (17)0.02136 (17)0.00688 (13)0.00301 (13)0.00013 (13)
P10.01253 (15)0.01079 (17)0.01399 (16)0.00290 (13)0.00164 (12)0.00189 (13)
P20.01197 (15)0.01054 (17)0.01684 (17)0.00140 (12)0.00385 (13)0.00272 (13)
P30.01189 (15)0.01076 (17)0.01771 (17)0.00135 (13)0.00379 (13)0.00387 (14)
C10.0156 (6)0.0118 (7)0.0239 (7)0.0031 (5)0.0050 (5)0.0026 (6)
C20.0174 (6)0.0135 (7)0.0188 (7)0.0043 (5)0.0045 (5)0.0001 (5)
C30.0151 (6)0.0159 (7)0.0193 (7)0.0039 (5)0.0005 (5)0.0044 (6)
C40.0133 (6)0.0129 (7)0.0255 (7)0.0031 (5)0.0019 (5)0.0041 (6)
C50.0170 (6)0.0122 (7)0.0156 (6)0.0024 (5)0.0044 (5)0.0025 (5)
C60.0180 (6)0.0178 (7)0.0232 (7)0.0020 (6)0.0060 (6)0.0072 (6)
C70.0242 (7)0.0193 (8)0.0272 (8)0.0009 (6)0.0040 (6)0.0107 (7)
C80.0322 (8)0.0220 (8)0.0270 (8)0.0052 (7)0.0079 (7)0.0112 (7)
C90.0268 (8)0.0274 (9)0.0263 (8)0.0076 (7)0.0105 (6)0.0092 (7)
C100.0198 (7)0.0208 (8)0.0218 (7)0.0023 (6)0.0081 (6)0.0059 (6)
C110.0137 (6)0.0138 (7)0.0189 (7)0.0003 (5)0.0066 (5)0.0040 (5)
C120.0211 (7)0.0158 (7)0.0201 (7)0.0033 (6)0.0065 (6)0.0038 (6)
C130.0264 (8)0.0199 (8)0.0229 (8)0.0027 (6)0.0062 (6)0.0010 (6)
C140.0279 (8)0.0363 (10)0.0194 (8)0.0009 (7)0.0116 (7)0.0002 (7)
C150.0347 (9)0.0471 (12)0.0274 (9)0.0119 (9)0.0166 (8)0.0099 (9)
C160.0310 (8)0.0294 (9)0.0278 (9)0.0122 (7)0.0122 (7)0.0067 (7)
C170.0130 (6)0.0133 (7)0.0179 (7)0.0010 (5)0.0030 (5)0.0043 (5)
C180.0245 (7)0.0138 (7)0.0293 (8)0.0023 (6)0.0129 (6)0.0037 (6)
C190.0258 (8)0.0186 (8)0.0347 (9)0.0047 (6)0.0128 (7)0.0094 (7)
C200.0162 (6)0.0237 (8)0.0213 (7)0.0029 (6)0.0053 (5)0.0091 (6)
C210.0212 (7)0.0205 (8)0.0199 (7)0.0038 (6)0.0082 (6)0.0022 (6)
C220.0227 (7)0.0145 (7)0.0229 (7)0.0045 (6)0.0080 (6)0.0029 (6)
C230.0136 (6)0.0197 (7)0.0224 (7)0.0052 (5)0.0033 (5)0.0100 (6)
C240.0296 (8)0.0197 (8)0.0252 (8)0.0102 (7)0.0011 (6)0.0080 (7)
C250.0392 (10)0.0307 (10)0.0258 (9)0.0207 (8)0.0096 (7)0.0098 (8)
C260.0206 (7)0.0380 (11)0.0365 (10)0.0127 (7)0.0074 (7)0.0228 (8)
C270.0181 (7)0.0313 (10)0.0370 (10)0.0007 (7)0.0048 (7)0.0188 (8)
C280.0186 (7)0.0244 (8)0.0251 (8)0.0008 (6)0.0076 (6)0.0093 (7)
C290.0179 (6)0.0135 (7)0.0188 (7)0.0043 (5)0.0056 (5)0.0022 (5)
C300.0228 (7)0.0368 (10)0.0224 (8)0.0134 (7)0.0001 (6)0.0107 (7)
C310.0355 (9)0.0511 (13)0.0214 (8)0.0196 (9)0.0027 (7)0.0136 (8)
C320.0380 (10)0.0370 (11)0.0283 (9)0.0175 (8)0.0132 (7)0.0071 (8)
C330.0402 (10)0.0468 (12)0.0322 (10)0.0302 (9)0.0076 (8)0.0065 (9)
C340.0325 (9)0.0381 (11)0.0220 (8)0.0231 (8)0.0022 (7)0.0055 (7)
P40.01521 (16)0.01243 (18)0.0248 (2)0.00147 (14)0.00703 (14)0.00449 (15)
F10.0217 (4)0.0182 (5)0.0329 (5)0.0076 (4)0.0095 (4)0.0054 (4)
F20.0469 (6)0.0305 (6)0.0226 (5)0.0058 (5)0.0139 (5)0.0061 (4)
F30.0169 (4)0.0213 (5)0.0338 (5)0.0021 (4)0.0041 (4)0.0118 (4)
F40.0237 (5)0.0232 (5)0.0630 (8)0.0036 (4)0.0147 (5)0.0214 (5)
F50.0362 (6)0.0240 (5)0.0363 (6)0.0103 (5)0.0185 (5)0.0098 (5)
F60.0185 (4)0.0226 (5)0.0633 (8)0.0007 (4)0.0014 (5)0.0216 (5)
Geometric parameters (Å, º) top
Pd1—P12.2176 (4)C15—C161.387 (3)
Pd1—P22.3178 (4)C15—H15A0.9500
Pd1—P32.3329 (4)C16—H16A0.9500
Pd1—Cl12.3441 (4)C17—C181.394 (2)
P1—C291.8073 (16)C17—C221.398 (2)
P1—C31.8193 (14)C18—C191.392 (2)
P1—C21.8211 (15)C18—H18A0.9500
P2—C111.8037 (15)C19—C201.381 (2)
P2—C51.8126 (15)C19—H19A0.9500
P2—C41.8476 (15)C20—C211.384 (2)
P3—C231.8132 (15)C20—H20A0.9500
P3—C171.8185 (16)C21—C221.389 (2)
P3—C11.8418 (15)C21—H21A0.9500
C1—C21.534 (2)C22—H22A0.9500
C1—H1A0.9900C23—C241.387 (2)
C1—H1B0.9900C23—C281.401 (2)
C2—H2A0.9900C24—C251.398 (2)
C2—H2B0.9900C24—H24A0.9500
C3—C41.532 (2)C25—C261.383 (3)
C3—H3A0.9900C25—H25A0.9500
C3—H3B0.9900C26—C271.383 (3)
C4—H4A0.9900C26—H26A0.9500
C4—H4B0.9900C27—C281.385 (2)
C5—C101.392 (2)C27—H27A0.9500
C5—C61.399 (2)C28—H28A0.9500
C6—C71.384 (2)C29—C301.393 (2)
C6—H6A0.9500C29—C341.402 (2)
C7—C81.389 (2)C30—C311.388 (3)
C7—H7A0.9500C30—H30A0.9500
C8—C91.384 (2)C31—C321.385 (3)
C8—H8A0.9500C31—H31A0.9500
C9—C101.393 (2)C32—C331.384 (3)
C9—H9A0.9500C32—H32A0.9500
C10—H10A0.9500C33—C341.382 (3)
C11—C161.390 (2)C33—H33A0.9500
C11—C121.399 (2)C34—H34A0.9500
C12—C131.384 (2)P4—F11.6158 (10)
C12—H12A0.9500P4—F21.5872 (11)
C13—C141.384 (3)P4—F31.5997 (10)
C13—H13A0.9500P4—F41.5967 (11)
C14—C151.378 (3)P4—F61.6005 (10)
C14—H14A0.9500P4—F51.6117 (11)
P1—Pd1—P283.905 (14)C14—C15—H15A120.1
P1—Pd1—P384.262 (14)C16—C15—H15A120.1
P2—Pd1—P3166.221 (13)C15—C16—C11119.90 (17)
P1—Pd1—Cl1175.897 (14)C15—C16—H16A120.1
P2—Pd1—Cl192.644 (14)C11—C16—H16A120.1
P3—Pd1—Cl199.430 (14)C18—C17—C22119.14 (15)
C29—P1—C3105.15 (7)C18—C17—P3119.17 (12)
C29—P1—C2108.28 (7)C22—C17—P3121.56 (12)
C3—P1—C2113.38 (7)C19—C18—C17120.29 (15)
C29—P1—Pd1112.53 (5)C19—C18—H18A120.1
C3—P1—Pd1107.87 (5)C17—C18—H18A120.1
C2—P1—Pd1109.64 (5)C20—C19—C18120.05 (15)
C11—P2—C5104.67 (7)C20—C19—H19A120.1
C11—P2—C4108.65 (7)C18—C19—H19A120.1
C5—P2—C4104.60 (7)C19—C20—C21120.16 (15)
C11—P2—Pd1115.24 (5)C19—C20—H20A120.1
C5—P2—Pd1115.29 (5)C21—C20—H20A120.1
C4—P2—Pd1107.76 (5)C20—C21—C22120.26 (15)
C23—P3—C17104.71 (7)C20—C21—H21A120.1
C23—P3—C1105.01 (7)C22—C21—H21A120.1
C17—P3—C1106.71 (7)C21—C22—C17120.09 (15)
C23—P3—Pd1120.12 (5)C21—C22—H22A120.1
C17—P3—Pd1112.42 (5)C17—C22—H22A120.1
C1—P3—Pd1106.97 (5)C24—C23—C28119.94 (14)
C1—C2—H2A109.7C24—C23—P3119.98 (12)
P1—C2—H2A111.0C28—C23—P3120.07 (12)
C1—C2—H2B109.7C23—C24—C25119.72 (16)
P1—C2—H2B111.0C23—C24—H24A120.1
C2—C1—P3110.54 (10)C25—C24—H24A120.1
C2—C1—H1A109.7C26—C25—C24119.95 (17)
P3—C1—H1A109.7C26—C25—H25A120.1
C2—C1—H1B109.7C24—C25—H25A120.1
P3—C1—H1B109.7C25—C26—C27120.43 (15)
C1—C2—P1106.09 (10)C25—C26—H26A120.1
C4—C3—P1106.05 (10)C27—C26—H26A120.1
C4—C3—H3A109.7C26—C27—C28120.18 (17)
P1—C3—H3A111.0C26—C27—H27A120.1
C4—C3—H3B109.7C28—C27—H27A120.1
P1—C3—H3B111.0C27—C28—C23119.77 (16)
C3—C4—P2108.46 (10)C27—C28—H28A120.1
C3—C4—H4A109.7C23—C28—H28A120.1
P2—C4—H4A111.0C30—C29—C34118.84 (15)
C3—C4—H4B109.7C30—C29—P1121.20 (12)
P3—C4—H4B103.0C34—C29—P1119.94 (12)
C10—C5—C6119.82 (14)C31—C30—C29120.39 (15)
C10—C5—P2122.34 (11)C31—C30—H30A120.1
C6—C5—P2117.82 (12)C29—C30—H30A120.1
C7—C6—C5120.02 (15)C32—C31—C30120.12 (16)
C7—C6—H6A120.1C32—C31—H31A120.1
C5—C6—H6A120.1C30—C31—H31A120.1
C6—C7—C8120.02 (15)C33—C32—C31120.01 (17)
C6—C7—H7A120.1C33—C32—H32A120.1
C8—C7—H7A120.1C31—C32—H32A120.1
C9—C8—C7120.21 (16)C34—C33—C32120.17 (16)
C9—C8—H8A120.1C34—C33—H33A120.1
C7—C8—H8A120.1C32—C33—H33A120.1
C8—C9—C10120.21 (16)C33—C34—C29120.46 (16)
C8—C9—H9A120.1C33—C34—H34A120.1
C10—C9—H9A120.1C29—C34—H34A120.1
C5—C10—C9119.72 (15)F2—P4—F491.25 (6)
C5—C10—H10A120.1F2—P4—F390.49 (6)
C9—C10—H10A120.1F4—P4—F390.41 (5)
C16—C11—C12119.14 (14)F2—P4—F690.92 (6)
C16—C11—P2121.99 (12)F4—P4—F690.63 (6)
C12—C11—P2118.63 (12)F3—P4—F6178.24 (6)
C13—C12—C11120.33 (15)F2—P4—F5179.18 (6)
C13—C12—H12A120.1F4—P4—F589.44 (6)
C11—C12—H12A120.1F3—P4—F589.06 (6)
C14—C13—C12120.02 (16)F6—P4—F589.53 (6)
C14—C13—H13A120.1F2—P4—F189.86 (6)
C12—C13—H13A120.1F4—P4—F1178.88 (6)
C15—C14—C13119.87 (16)F3—P4—F189.74 (5)
C15—C14—H14A120.1F6—P4—F189.19 (5)
C13—C14—H14A120.1F5—P4—F189.45 (6)
C14—C15—C16120.72 (17)

Experimental details

Crystal data
Chemical formula[PdCl(C34H33P3)]PF6
Mr821.33
Crystal system, space groupTriclinic, P1
Temperature (K)100
a, b, c (Å)11.2465 (5), 11.8182 (5), 15.5093 (7)
α, β, γ (°)69.029 (2), 70.439 (2), 69.697 (2)
V3)1752.27 (13)
Z2
Radiation typeMo Kα
µ (mm1)0.84
Crystal size (mm)0.47 × 0.15 × 0.10
Data collection
DiffractometerBruker APEXII CCD
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2000)
Tmin, Tmax0.693, 0.917
No. of measured, independent and
observed [I > 2σ(I)] reflections
48576, 13341, 10917
Rint0.030
(sin θ/λ)max1)0.773
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.031, 0.067, 1.03
No. of reflections13341
No. of parameters415
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.71, 0.67

Computer programs: APEX2 (Bruker, 2006), SAINT (Bruker, 2006), SAINT (Bruker, 2006, SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Selected bond lengths (Å) top
Pd1—P12.2176 (4)Pd1—P32.3329 (4)
Pd1—P22.3178 (4)Pd1—Cl12.3441 (4)
 

Acknowledgements

We thank Research Corporation Cottrell Science Award (No. 7293) for funding supporting this study.

References

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