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A triclinic polymorph of bis­­(μ-di-tert-butyl­phosphanido)bis­­[(di-tert-butyl­phosphane)palladium(I)]

aInstitut für Anorganische und Analytische Chemie, Goethe-Universität Frankfurt, Max-von-Laue-Strasse 7, 60438 Frankfurt am Main, Germany
*Correspondence e-mail: bolte@chemie.uni-frankfurt.de

(Received 23 May 2012; accepted 23 May 2012; online 31 May 2012)

A new polymorph of the title compound, [Pd2(C8H18P)2(C8H19P)2], has been found. It belongs to the triclinic P-1 space group, whereas the known form [Leoni, Sommovigo, Pasquali, Sabatino & Braga (1992[Leoni, P., Sommovigo, M., Pasquali, M., Sabatino, P. & Braga, D. (1992). J. Organomet. Chem. 423, 263-270.]), J. Organo­met. Chem. 423, 263–270] crystallizes in the monoclinic C2/c space group. The title compound features a dinuclear palladium complex with a planar central Pd2(μ-P)2 core (r.m.s. deviation = 0.003 Å). The Pd—Pd distance of 2.5988 (5) Å is within the range of a PdI—PdI bond. The mol­ecules of both polymorphs are located on a crystallographic centre of inversion. The mol­ecular conformations of the two polymorphs are essentially identical. The crystal packing patterns, on the other hand, are slightly different.

Related literature

For synthetic background, see: Dornhaus et al. (2006a[Dornhaus, F., Bolte, M., Lerner, H.-W. & Wagner, M. (2006a). Eur. J. Inorg. Chem. pp. 1777-1785.],b[Dornhaus, F., Bolte, M., Lerner, H.-W. & Wagner, M. (2006b). Eur. J. Inorg. Chem. pp. 5138-5147.]); Kückmann et al. (2005[Kückmann, T. I., Hermsen, M., Bolte, M., Wagner, M. & Lerner, H.-W. (2005). Inorg. Chem. 44, 3449-3458.]); Lerner (2005[Lerner, H.-W. (2005). Coord. Chem. Rev. 249, 781-798.]); Sänger et al. (2012[Sänger, I., Kückmann, T. I., Dornhaus, F., Bolte, M., Wagner, M. & Lerner, H.-W. (2012). Dalton Trans. 41, 6671-6676.]). For the monoclinic polymorph of the title compound, see: Leoni et al. (1992[Leoni, P., Sommovigo, M., Pasquali, M., Sabatino, P. & Braga, D. (1992). J. Organomet. Chem. 423, 263-270.]). For the Cambridge Structural Database, see: Allen (2002[Allen, F. H. (2002). Acta Cryst. B58, 380-388.]).

[Scheme 1]

Experimental

Crystal data
  • [Pd2(C8H18P)2(C8H19P)2]

  • Mr = 795.59

  • Triclinic, [P \overline 1]

  • a = 9.0721 (5) Å

  • b = 10.5156 (6) Å

  • c = 11.5351 (6) Å

  • α = 89.064 (5)°

  • β = 67.307 (4)°

  • γ = 75.330 (5)°

  • V = 978.06 (9) Å3

  • Z = 1

  • Mo Kα radiation

  • μ = 1.10 mm−1

  • T = 173 K

  • 0.23 × 0.14 × 0.04 mm

Data collection
  • Stoe IPDS II two-circle diffractometer

  • Absorption correction: multi-scan (MULABS; Spek, 2009[Spek, A. L. (2009). Acta Cryst. D65, 148-155.]; Blessing, 1995[Blessing, R. H. (1995). Acta Cryst. A51, 33-38.]) Tmin = 0.786, Tmax = 0.957

  • 13922 measured reflections

  • 4481 independent reflections

  • 4083 reflections with I > 2σ(I)

  • Rint = 0.066

Refinement
  • R[F2 > 2σ(F2)] = 0.042

  • wR(F2) = 0.111

  • S = 1.05

  • 4481 reflections

  • 176 parameters

  • H atoms treated by a mixture of independent and constrained refinement

  • Δρmax = 2.31 e Å−3

  • Δρmin = −1.34 e Å−3

Data collection: X-AREA (Stoe & Cie, 2001[Stoe & Cie (2001). X-AREA. Stoe & Cie, Darmstadt, Germany.]); cell refinement: X-AREA; data reduction: X-AREA; 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: XP (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXL97.

Supporting information


Comment top

Recently, we have made a comparison of cyclopentadienyliron dicarbonyl complexes with two series of isoelectronic and largely isosteric ligands (Sänger et al., 2012), namely phosphanes PR3, phosphanyl borohydrides [PR2BH3]- (Dornhaus et al., 2006a), and silanides [SiR3]- (Lerner, 2005), and the corresponding chalcogene derivatives SPtBu3, [SPtBu2BH3]- (Dornhaus et al., 2006b) and [SSitBu3]- (Kückmann et al., 2005). We have concluded that, with respect to electron donor strength, phosphanyl borohydrides occupy an intermediate position between phosphanes (weakest donors) and silyl ligands (strongest donors). In addition we found that electron-rich tBu-substituted silanides tend to liberate isobutene. In this paper we report the structure of a new polymorph of [(tBu2HP)PdPtBu2]2, (I). The title compound was obtained via photolysis of Pd(PtBu3)2 accompanied by liberation of isobutene and dihydrogen (Fig. 1).

A perspective view of the title compound is shown in Fig. 2. The molecules lie on a crystallographic centre of inversion. In the monoclinic form, the molecules also show Ci symmetry. A least-squares fit of the P and Pd atoms (r.m.s. deviation 0.004 Å) of the two polymorphs shows that the two structures are essentially identical (Fig. 3). The crystal packing patterns, on the other hand, are slightly different (Figs. 4 and 5). The value of the acyclic P—Pd bond [2.2860 (8) Å] agrees well with 2.29 (4) Å, which was found for comparable structures in the Cambridge Structural Database (Version 5.33 of November 2011, plus one update; Allen, 2002). The cyclic P—Pd bonds [2.3374 (9) Å, 2.3405 (8) Å] and the Pd···Pd [2.5988 (5) Å] distance, on the other hand, are slightly longer than the database values [P—Pd = 2.315 (16) Å and Pd···Pd = 2.31 (3) Å].

Related literature top

For synthetic background, see: Dornhaus et al. (2006a, 2006b); Kückmann et al. (2005); Lerner (2005); Sänger et al. (2012). For the monoclinic polymorph of the title compound, see: Leoni et al. (1992). For the Cambridge Structural Database, see: Allen (2002).

Experimental top

All experiments were carried out under an atmosphere of dry nitrogen or argon using Schlenk techniques or in an argon filled glovebox. Solvents ([D6]benzene, benzene) were freshly distilled from sodium/benzophenone prior to use. NMR spectra were recorded on a Bruker Avance 400 (1H, 1H31P-COSY) or a Bruker Avance 300 (31P, 31P{1H}) instrument. Chemical shift values (1H) are reported in p.p.m. relative to SiMe4 and were referenced to residual solvent signals. The 31P{1H} and 31P NMR chemical shift values were referenced to external H3PO4 (85%). Abbreviations: d = doublet, t = triplet, m = multiplet, br = broad. Pd(PtBu3)2 (38 mg, 0.074 mmol) was dissolved in 0.5 ml C6D6 in a vial. The vial was sealed and stored at room temperature under daylight for six weeks. During this period red plate-shaped crystals formed. Those were collected atop a frit and washed with 2 ml of benzene. Drying in vacuo yielded the title compound (8 mg, 0.009 mmol, 24%).

1H (400.13 MHz, [D6]Benzene, 25°C): δ = 1.56 (m, PtBu2), 1.39 (m, HPtBu2); 31P{1H} NMR (121.45 MHz, [D6]Benzene, 25°C): δ = 284.3 (t, 2JPP = 32.2 Hz, PtBu2), 57.9 (t, 2JPP = 32.2 Hz, HPtBu2); 31P NMR (121.45 MHz, [D6]Benzene, 25°C): δ = 284.3 (br, PtBu2), 57.9 (d br, 1JHP = 280 Hz, HPtBu2).

Refinement top

H atoms bonded to C were refined using a riding model, with C—H = 0.98 Å and with Uiso(H) = 1.5Ueq(C). The H atom bonded to P was freely refined.

The final difference Fourier map had a peak and a hole in the vicinity of Pd1.

Computing details top

Data collection: X-AREA (Stoe & Cie, 2001); cell refinement: X-AREA (Stoe & Cie, 2001); data reduction: X-AREA (Stoe & Cie, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP (Sheldrick, 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. Reaction scheme for obtaining the title compound.
[Figure 2] Fig. 2. A perspective view of the title compound, showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 50% probability level. H atoms bonded to C are omitted for clarity. Atoms with the suffix A were generated by the symmetry operator -x + 1, -y, -z + 1.
[Figure 3] Fig. 3. Least-squares fit of the two polymorphs of the title compound. The triclinic polymorph is drawn with full bonds, the monoclinic form with open bonds.
[Figure 4] Fig. 4. Packing diagram of the triclinic polymorph of the title compound.
[Figure 5] Fig. 5. Packing diagram of the monoclinic polymorph of the title compound.
bis(µ-di-tert-butylphosphanido)bis[(di-tert- butylphosphane)palladium(I)] top
Crystal data top
[Pd2(C8H18P)2(C8H19P)2]Z = 1
Mr = 795.59F(000) = 418
Triclinic, P1Dx = 1.351 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.0721 (5) ÅCell parameters from 11232 reflections
b = 10.5156 (6) Åθ = 3.5–28.0°
c = 11.5351 (6) ŵ = 1.10 mm1
α = 89.064 (5)°T = 173 K
β = 67.307 (4)°Plate, red
γ = 75.330 (5)°0.23 × 0.14 × 0.04 mm
V = 978.06 (9) Å3
Data collection top
Stoe IPDS II two-circle
diffractometer
4481 independent reflections
Radiation source: fine-focus sealed tube4083 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.066
ω scansθmax = 27.5°, θmin = 3.5°
Absorption correction: multi-scan
(MULABS; Spek, 2009; Blessing, 1995)
h = 1111
Tmin = 0.786, Tmax = 0.957k = 1313
13922 measured reflectionsl = 1414
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)] = 0.042Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.111H atoms treated by a mixture of independent and constrained refinement
S = 1.05 w = 1/[σ2(Fo2) + (0.0669P)2 + 1.1837P]
where P = (Fo2 + 2Fc2)/3
4481 reflections(Δ/σ)max < 0.001
176 parametersΔρmax = 2.31 e Å3
0 restraintsΔρmin = 1.34 e Å3
Crystal data top
[Pd2(C8H18P)2(C8H19P)2]γ = 75.330 (5)°
Mr = 795.59V = 978.06 (9) Å3
Triclinic, P1Z = 1
a = 9.0721 (5) ÅMo Kα radiation
b = 10.5156 (6) ŵ = 1.10 mm1
c = 11.5351 (6) ÅT = 173 K
α = 89.064 (5)°0.23 × 0.14 × 0.04 mm
β = 67.307 (4)°
Data collection top
Stoe IPDS II two-circle
diffractometer
4481 independent reflections
Absorption correction: multi-scan
(MULABS; Spek, 2009; Blessing, 1995)
4083 reflections with I > 2σ(I)
Tmin = 0.786, Tmax = 0.957Rint = 0.066
13922 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0420 restraints
wR(F2) = 0.111H atoms treated by a mixture of independent and constrained refinement
S = 1.05Δρmax = 2.31 e Å3
4481 reflectionsΔρmin = 1.34 e Å3
176 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
Pd10.50058 (3)0.07733 (2)0.41089 (2)0.01892 (10)
P10.46490 (10)0.14997 (8)0.61308 (7)0.02064 (18)
P20.49486 (11)0.23437 (8)0.27214 (8)0.02250 (18)
H20.479 (6)0.345 (5)0.312 (4)0.033 (11)*
C10.2544 (4)0.2667 (4)0.7086 (3)0.0275 (7)
C20.6381 (4)0.2167 (3)0.6181 (3)0.0256 (7)
C30.3122 (5)0.2678 (4)0.2244 (3)0.0305 (7)
C40.6950 (5)0.2228 (4)0.1328 (3)0.0290 (7)
C110.2300 (6)0.4002 (4)0.6554 (5)0.0476 (11)
H11A0.30970.44450.66200.071*
H11B0.11700.45460.70340.071*
H11C0.24760.38740.56660.071*
C120.2212 (6)0.2872 (5)0.8483 (4)0.0439 (10)
H12A0.23700.20130.88270.066*
H12B0.10700.34040.89430.066*
H12C0.29830.33280.85740.066*
C130.1300 (5)0.1985 (4)0.6982 (4)0.0379 (9)
H13A0.14520.11250.73250.057*
H13B0.14760.18590.60940.057*
H13C0.01710.25330.74610.057*
C210.6472 (6)0.3438 (4)0.5533 (5)0.0418 (10)
H21A0.65340.33000.46760.063*
H21B0.74600.36850.54960.063*
H21C0.54800.41460.60130.063*
C220.6292 (6)0.2379 (6)0.7517 (4)0.0456 (11)
H22A0.62380.15610.79310.068*
H22B0.52990.30850.80000.068*
H22C0.72810.26260.74760.068*
C230.7975 (5)0.1095 (4)0.5433 (4)0.0360 (8)
H23A0.79470.02690.58370.054*
H23B0.89350.13730.54160.054*
H23C0.80630.09560.45680.054*
C310.1604 (5)0.2900 (6)0.3489 (4)0.0508 (13)
H31A0.17100.21250.39630.076*
H31B0.06020.30380.33150.076*
H31C0.15260.36790.39860.076*
C320.2917 (7)0.3882 (6)0.1519 (5)0.0564 (14)
H32A0.28690.46580.20050.085*
H32B0.18890.40240.13820.085*
H32C0.38620.37410.07030.085*
C330.3187 (7)0.1459 (6)0.1504 (6)0.0576 (14)
H33A0.33170.06890.19810.086*
H33B0.41300.13070.06860.086*
H33C0.21570.15990.13700.086*
C410.6962 (6)0.3430 (5)0.0581 (5)0.0507 (12)
H41A0.66560.42230.11480.076*
H41B0.61630.35160.01860.076*
H41C0.80740.33280.00750.076*
C420.8260 (6)0.2088 (6)0.1887 (4)0.0475 (11)
H42A0.79770.28720.24580.071*
H42B0.93490.19980.12040.071*
H42C0.82920.13030.23560.071*
C430.7432 (7)0.0998 (5)0.0447 (4)0.0513 (12)
H43A0.74280.02220.09280.077*
H43B0.85440.08990.02080.077*
H43C0.66350.10810.00510.077*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pd10.02206 (14)0.01645 (14)0.01839 (13)0.00473 (9)0.00844 (9)0.00263 (8)
P10.0242 (4)0.0166 (4)0.0205 (4)0.0051 (3)0.0085 (3)0.0012 (3)
P20.0298 (4)0.0190 (4)0.0194 (4)0.0058 (3)0.0110 (3)0.0036 (3)
C10.0252 (16)0.0240 (17)0.0274 (16)0.0013 (13)0.0072 (13)0.0011 (13)
C20.0277 (16)0.0240 (17)0.0263 (16)0.0077 (13)0.0115 (13)0.0001 (12)
C30.0291 (17)0.0328 (19)0.0302 (17)0.0051 (15)0.0144 (14)0.0069 (14)
C40.0316 (18)0.0306 (19)0.0247 (16)0.0105 (15)0.0098 (14)0.0054 (13)
C110.038 (2)0.026 (2)0.062 (3)0.0038 (17)0.010 (2)0.0070 (19)
C120.038 (2)0.052 (3)0.0302 (19)0.0041 (19)0.0060 (17)0.0134 (18)
C130.0273 (18)0.040 (2)0.042 (2)0.0073 (16)0.0103 (16)0.0037 (17)
C210.046 (2)0.030 (2)0.058 (3)0.0197 (18)0.025 (2)0.0115 (18)
C220.040 (2)0.069 (3)0.035 (2)0.018 (2)0.0187 (18)0.005 (2)
C230.0261 (17)0.034 (2)0.043 (2)0.0082 (15)0.0092 (16)0.0012 (16)
C310.030 (2)0.078 (4)0.038 (2)0.006 (2)0.0127 (18)0.017 (2)
C320.048 (3)0.060 (3)0.066 (3)0.011 (2)0.031 (2)0.038 (3)
C330.061 (3)0.059 (3)0.070 (3)0.010 (3)0.047 (3)0.008 (3)
C410.043 (2)0.052 (3)0.050 (3)0.017 (2)0.009 (2)0.027 (2)
C420.035 (2)0.073 (3)0.037 (2)0.019 (2)0.0144 (18)0.009 (2)
C430.056 (3)0.052 (3)0.033 (2)0.013 (2)0.004 (2)0.0114 (19)
Geometric parameters (Å, º) top
Pd1—P22.2860 (8)C13—H13B0.9800
Pd1—P1i2.3374 (9)C13—H13C0.9800
Pd1—P12.3405 (8)C21—H21A0.9800
Pd1—Pd1i2.5988 (5)C21—H21B0.9800
P1—C21.896 (4)C21—H21C0.9800
P1—C11.898 (4)C22—H22A0.9800
P1—Pd1i2.3373 (9)C22—H22B0.9800
P2—C41.881 (4)C22—H22C0.9800
P2—C31.891 (4)C23—H23A0.9800
P2—H21.21 (5)C23—H23B0.9800
C1—C111.521 (6)C23—H23C0.9800
C1—C131.523 (5)C31—H31A0.9800
C1—C121.529 (5)C31—H31B0.9800
C2—C211.526 (5)C31—H31C0.9800
C2—C221.529 (5)C32—H32A0.9800
C2—C231.533 (5)C32—H32B0.9800
C3—C321.517 (6)C32—H32C0.9800
C3—C331.528 (6)C33—H33A0.9800
C3—C311.528 (6)C33—H33B0.9800
C4—C411.519 (6)C33—H33C0.9800
C4—C431.520 (6)C41—H41A0.9800
C4—C421.532 (6)C41—H41B0.9800
C11—H11A0.9800C41—H41C0.9800
C11—H11B0.9800C42—H42A0.9800
C11—H11C0.9800C42—H42B0.9800
C12—H12A0.9800C42—H42C0.9800
C12—H12B0.9800C43—H43A0.9800
C12—H12C0.9800C43—H43B0.9800
C13—H13A0.9800C43—H43C0.9800
P2—Pd1—P1i130.80 (3)C1—C13—H13C109.5
P2—Pd1—P1116.70 (3)H13A—C13—H13C109.5
P1i—Pd1—P1112.50 (2)H13B—C13—H13C109.5
P2—Pd1—Pd1i172.88 (3)C2—C21—H21A109.5
P1i—Pd1—Pd1i56.31 (2)C2—C21—H21B109.5
P1—Pd1—Pd1i56.19 (2)H21A—C21—H21B109.5
C2—P1—C1110.95 (16)C2—C21—H21C109.5
C2—P1—Pd1i120.70 (11)H21A—C21—H21C109.5
C1—P1—Pd1i121.18 (12)H21B—C21—H21C109.5
C2—P1—Pd1114.53 (11)C2—C22—H22A109.5
C1—P1—Pd1114.77 (12)C2—C22—H22B109.5
Pd1i—P1—Pd167.50 (2)H22A—C22—H22B109.5
C4—P2—C3111.79 (16)C2—C22—H22C109.5
C4—P2—Pd1116.35 (12)H22A—C22—H22C109.5
C3—P2—Pd1115.50 (12)H22B—C22—H22C109.5
C4—P2—H296 (2)C2—C23—H23A109.5
C3—P2—H299 (2)C2—C23—H23B109.5
Pd1—P2—H2115 (2)H23A—C23—H23B109.5
C11—C1—C13109.2 (3)C2—C23—H23C109.5
C11—C1—C12109.4 (4)H23A—C23—H23C109.5
C13—C1—C12108.0 (3)H23B—C23—H23C109.5
C11—C1—P1112.3 (3)C3—C31—H31A109.5
C13—C1—P1104.7 (3)C3—C31—H31B109.5
C12—C1—P1113.1 (3)H31A—C31—H31B109.5
C21—C2—C22109.5 (3)C3—C31—H31C109.5
C21—C2—C23108.1 (3)H31A—C31—H31C109.5
C22—C2—C23108.3 (3)H31B—C31—H31C109.5
C21—C2—P1112.6 (3)C3—C32—H32A109.5
C22—C2—P1113.2 (3)C3—C32—H32B109.5
C23—C2—P1104.7 (2)H32A—C32—H32B109.5
C32—C3—C33110.2 (4)C3—C32—H32C109.5
C32—C3—C31108.5 (4)H32A—C32—H32C109.5
C33—C3—C31107.5 (4)H32B—C32—H32C109.5
C32—C3—P2115.2 (3)C3—C33—H33A109.5
C33—C3—P2110.3 (3)C3—C33—H33B109.5
C31—C3—P2104.7 (3)H33A—C33—H33B109.5
C41—C4—C43109.4 (4)C3—C33—H33C109.5
C41—C4—C42108.2 (4)H33A—C33—H33C109.5
C43—C4—C42108.0 (4)H33B—C33—H33C109.5
C41—C4—P2114.6 (3)C4—C41—H41A109.5
C43—C4—P2111.1 (3)C4—C41—H41B109.5
C42—C4—P2105.1 (3)H41A—C41—H41B109.5
C1—C11—H11A109.5C4—C41—H41C109.5
C1—C11—H11B109.5H41A—C41—H41C109.5
H11A—C11—H11B109.5H41B—C41—H41C109.5
C1—C11—H11C109.5C4—C42—H42A109.5
H11A—C11—H11C109.5C4—C42—H42B109.5
H11B—C11—H11C109.5H42A—C42—H42B109.5
C1—C12—H12A109.5C4—C42—H42C109.5
C1—C12—H12B109.5H42A—C42—H42C109.5
H12A—C12—H12B109.5H42B—C42—H42C109.5
C1—C12—H12C109.5C4—C43—H43A109.5
H12A—C12—H12C109.5C4—C43—H43B109.5
H12B—C12—H12C109.5H43A—C43—H43B109.5
C1—C13—H13A109.5C4—C43—H43C109.5
C1—C13—H13B109.5H43A—C43—H43C109.5
H13A—C13—H13B109.5H43B—C43—H43C109.5
P2—Pd1—P1—C265.64 (13)C1—P1—C2—C2165.6 (3)
P1i—Pd1—P1—C2114.74 (13)Pd1i—P1—C2—C21143.7 (3)
Pd1i—Pd1—P1—C2114.74 (13)Pd1—P1—C2—C2166.4 (3)
P2—Pd1—P1—C164.42 (13)C1—P1—C2—C2259.4 (3)
P1i—Pd1—P1—C1115.21 (13)Pd1i—P1—C2—C2291.3 (3)
Pd1i—Pd1—P1—C1115.21 (13)Pd1—P1—C2—C22168.7 (3)
P2—Pd1—P1—Pd1i179.63 (3)C1—P1—C2—C23177.2 (2)
P1i—Pd1—P1—Pd1i0.0Pd1i—P1—C2—C2326.5 (3)
P1i—Pd1—P2—C467.41 (14)Pd1—P1—C2—C2350.9 (3)
P1—Pd1—P2—C4113.05 (14)C4—P2—C3—C3254.6 (4)
P1i—Pd1—P2—C366.64 (15)Pd1—P2—C3—C32169.3 (3)
P1—Pd1—P2—C3112.90 (14)C4—P2—C3—C3371.0 (4)
C2—P1—C1—C1163.1 (3)Pd1—P2—C3—C3365.1 (4)
Pd1i—P1—C1—C11146.4 (3)C4—P2—C3—C31173.6 (3)
Pd1—P1—C1—C1168.7 (3)Pd1—P2—C3—C3150.3 (3)
C2—P1—C1—C13178.6 (2)C3—P2—C4—C4156.2 (4)
Pd1i—P1—C1—C1328.1 (3)Pd1—P2—C4—C41168.2 (3)
Pd1—P1—C1—C1349.6 (3)C3—P2—C4—C4368.6 (4)
C2—P1—C1—C1261.3 (3)Pd1—P2—C4—C4367.1 (3)
Pd1i—P1—C1—C1289.3 (3)C3—P2—C4—C42174.9 (3)
Pd1—P1—C1—C12167.0 (3)Pd1—P2—C4—C4249.5 (3)
Symmetry code: (i) x+1, y, z+1.

Experimental details

Crystal data
Chemical formula[Pd2(C8H18P)2(C8H19P)2]
Mr795.59
Crystal system, space groupTriclinic, P1
Temperature (K)173
a, b, c (Å)9.0721 (5), 10.5156 (6), 11.5351 (6)
α, β, γ (°)89.064 (5), 67.307 (4), 75.330 (5)
V3)978.06 (9)
Z1
Radiation typeMo Kα
µ (mm1)1.10
Crystal size (mm)0.23 × 0.14 × 0.04
Data collection
DiffractometerStoe IPDS II two-circle
diffractometer
Absorption correctionMulti-scan
(MULABS; Spek, 2009; Blessing, 1995)
Tmin, Tmax0.786, 0.957
No. of measured, independent and
observed [I > 2σ(I)] reflections
13922, 4481, 4083
Rint0.066
(sin θ/λ)max1)0.651
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.042, 0.111, 1.05
No. of reflections4481
No. of parameters176
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)2.31, 1.34

Computer programs: X-AREA (Stoe & Cie, 2001), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), XP (Sheldrick, 2008).

 

References

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First citationBlessing, R. H. (1995). Acta Cryst. A51, 33–38.  CrossRef CAS Web of Science IUCr Journals Google Scholar
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First citationSänger, I., Kückmann, T. I., Dornhaus, F., Bolte, M., Wagner, M. & Lerner, H.-W. (2012). Dalton Trans. 41, 6671–6676.  Web of Science PubMed Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationSpek, A. L. (2009). Acta Cryst. D65, 148–155.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationStoe & Cie (2001). X-AREA. Stoe & Cie, Darmstadt, Germany.  Google Scholar

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