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Acta Cryst. (2007). E63, m3083    [ doi:10.1107/S1600536807058291 ]

cis-Dichlorido[bis(dicyclohexylphosphino)methane-[kappa]2P,P']palladium(II) dichloromethane solvate

J. T. Mague, D. H. Pool and M. J. Fink

Abstract top

The title compound, [PdCl2(C25H46P2)]·CH2Cl2, exhibits a distorted square-planar coordination about the PdII atom. The major distortion, seen in the P-Pd-P angle, is the result of the small bite angle of the diphosphine ligand. There is also a slight tetrahedral distortion from planarity, as measured by the dihedral angle of 2.26 (3)° between the PdP2 and PdCl2 planes. The dichloromethane solvent molecule is disordered over two sites with approximate occupancies of 0.58 and 0.42.

Comment top

cis-Dichloro(bis(dicyclohexylphosphino)methanepalladium(II), (dcpm)PdCl2 (I), has received brief mention as an intermediate in the synthesis of (dcpm)PdI2 (Zhuravel et al., 2000) but appears not to have been fully characterized. The present sample was obtained following prolonged exposure of a dichloromethane/diethyl ether solution of oxalato(bis(dicyclohexylphosphino)methanepalladium(II) to light in an attempt to grow crystals of the latter. Complex (I) exhibits distorted square planar coordination about the metal, the major distortion being the P1—Pd1—P2 angle of 73.82 (2)° which is the consequence of the small bite angle of the dcpm ligand. Additionally there is a slight tetrahedral distortion from planarity as indicated by a dihedral angle of 2.26 (3)° between the PdP2 and PdCl2 planes. These two metrical parameters are essentially the same as seen in the only other structurally characterized palladium dcpm complex (dcpm)Pd(CH3)2 (Reid et al., 2001) where they are, respectively 73.34 and 2.69°. The Pd—P and Pd—Cl distances differ only slightly in each case and compare favorably with those in the related complexes (RCH(PPh2)2)PdCl2 (R = H (Palenik et al., 1975), CH3 (Lee et al., 1986), CN (Braun et al., 2007)).

Related literature top

For related structures see: Reid et al. (2001); Palenik, et al. (1975); Lee et al. (1986); Braun et al. (2007). For related literature, see: Zhuravel et al. (2000).

Experimental top

Crystals of (dcpm)PdCl2 (dcpm = bis(dicyclohexylphosphino)methane) were obtained from a methylene chloride/diethyl ether solution of (dcpm)PdC2O4 which was exposed to fluorescent lighting for seven days in an attempt to crystallize the latter. The 31P{1H} NMR spectrum of the material remaining after selection of the crystal for x-ray diffraction exhibits a single resonance at −33.3 p.p.m. and no visible carbonyl resonance in the 13C{1H} NMR spectrum·The same −33.3 p.p.m. resonance is observed after treatment of an authentic sample of (dcpm)PdC2O4 with HCl suggesting that the prolonged exposure of (dcpm)PdC2O4 to the chlorinated solvent and light generated sufficient HCl to convert the (dcpm)PdC2O4 to (dcpm)PdCl2. Additional evidence for this proposal comes from the observation of a small peak at −33.3 p.p.m. in the 31P{1H} NMR spectrum of the product initially obtained in the synthesis of (dcpm)PdC2O4 by ligand displacement from (tmeda)PdC2O4 (tmeda = N,N',N",N"'-tetramethylethylenediamine) with dcpm in methylene chloride with stirring over three days. 1H NMR (CD2Cl2): δ 1.2–2.4 (m, 44 H, Cy), 2.85 (t, JPH = 10 Hz, 2 H, PCH2P). 31P{1H} NMR (CD2Cl2): δ −33.3. 13C{1H} NMR (CD2Cl2): δ 19.37 (t, JPC = 21 Hz, PCH2P), 26.18 (s, Cy), 27.13 (t, JPC = 6 Hz Cy), 27.42 (t, JPC = 7 Hz Cy), 28.70 (s, Cy), 29.52 (s, Cy), 35.94 (t, JPC = 10 Hz, –CHP–).

Refinement top

H-atoms were placed in calculated positions (C—H = 0.99 − 1.00 Å) and included as riding contributions with isotropic displacement parameters 1.2 times those of the attached carbon atoms. The solvent dichloromethane molecule is disordered over two sites having one chlorine (Cl3) in common in a 5755 (15):4245 (15) ratio of refined occupancies. Refinement was completed with the disordered model constrained to have C—Cl distances of 1.72 (1) Å.

Computing details top

Data collection: APEX2 (Bruker, 2007); cell refinement: APEX2 (Bruker, 2007); data reduction: SAINT-Plus (Bruker, 2006); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: APEX2 (Bruker, 2007); software used to prepare material for publication: APEX2 (Bruker, 2007).

Figures top
[Figure 1] Fig. 1. The molecular structure with displacement ellipsoids drawn at the 50% probability level and H-atoms are represented by spheres of arbitrary radius. The dichloromethane solvent is not shown.
cis-Dichlorido[bis(dicyclohexylphosphino)methane-κ2P,P']palladium(II) dichloromethane solvate top
Crystal data top
[PdCl2(C25H46P2)]·CH2Cl2F000 = 1392.1
Mr = 670.78Dx = 1.438 Mg m−3
Monoclinic, P21/cMo Kα radiation
λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 9765 reflections
a = 10.6978 (4) Åθ = 2.3–29.3º
b = 20.2154 (7) ŵ = 1.06 mm−1
c = 15.0333 (5) ÅT = 100 (2) K
β = 107.641 (1)ºBlock, colourless
V = 3098.2 (2) Å30.19 × 0.15 × 0.11 mm
Z = 4
Data collection top
Bruker SMART APEX CCD area-detector
diffractometer		7832 independent reflections
Radiation source: fine-focus sealed tube6992 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.033
T = 100(2) Kθmax = 28.5º
φ and ω scansθmin = 2.2º
Absorption correction: multi-scan
(SADABS; Sheldrick, 2007)		h = −14→14
Tmin = 0.803, Tmax = 0.894k = −27→27
54228 measured reflectionsl = −19→20
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.026H-atom parameters constrained
wR(F2) = 0.058  w = 1/[σ2(Fo2) + (0.0171P)2 + 3.7026P]
where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max = 0.001
7832 reflectionsΔρmax = 1.11 e Å−3
305 parametersΔρmin = −1.05 e Å−3
4 restraintsExtinction correction: none
Primary atom site location: structure-invariant direct methods
Crystal data top
[PdCl2(C25H46P2)]·CH2Cl2V = 3098.2 (2) Å3
Mr = 670.78Z = 4
Monoclinic, P21/cMo Kα
a = 10.6978 (4) ŵ = 1.06 mm−1
b = 20.2154 (7) ÅT = 100 (2) K
c = 15.0333 (5) Å0.19 × 0.15 × 0.11 mm
β = 107.641 (1)º
Data collection top
Bruker SMART APEX CCD area-detector
diffractometer		7832 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 2007)		6992 reflections with I > 2σ(I)
Tmin = 0.803, Tmax = 0.894Rint = 0.033
54228 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0264 restraints
wR(F2) = 0.058H-atom parameters constrained
S = 1.04Δρmax = 1.11 e Å−3
7832 reflectionsΔρmin = −1.05 e Å−3
305 parameters
Special details top

Experimental. The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5 °. in omega, colllected at phi = 0.00, 90.00 and 180.00 °. and 2 sets of 800 frames, each of width 0.45 ° in phi, collected at omega = −30.00 and 210.00 °. The scan time was 10 sec/frame.

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. H-atoms were placed in calculated positions (C—H = 0.99 − 1.00 Å) and included as riding contributions with isotropic displacement parameters 1.2 times those of the attached carbon atoms. The solvent dichloromethane molecule is disordered over two sites having one chlorine (Cl3) in common in a 58:42 ratio. Refinement was completed with the disordered model constrained to have C—Cl distances of 1.72 (1) Å.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Pd10.448118 (12)0.231722 (6)0.766483 (9)0.01362 (4)
Cl10.28057 (4)0.23668 (2)0.62016 (3)0.01973 (9)
Cl20.60824 (4)0.18028 (2)0.70938 (3)0.02113 (9)
P10.32599 (4)0.28077 (2)0.84313 (3)0.01365 (8)
P20.57527 (4)0.24148 (2)0.91426 (3)0.01433 (9)
C10.19916 (16)0.23196 (8)0.87199 (12)0.0150 (3)
H10.16870.25790.91820.018*
C20.25493 (17)0.16610 (9)0.91832 (13)0.0183 (3)
H2A0.28750.13960.87460.022*
H2B0.32980.17490.97470.022*
C30.14985 (19)0.12702 (9)0.94548 (13)0.0224 (4)
H3A0.18680.08420.97310.027*
H3B0.12260.15200.99320.027*
C40.03056 (19)0.11457 (10)0.86100 (14)0.0247 (4)
H4A−0.03790.09140.88110.030*
H4B0.05580.08580.81590.030*
C5−0.02433 (18)0.17960 (10)0.81380 (14)0.0232 (4)
H5A−0.05840.20610.85680.028*
H5B−0.09850.17020.75720.028*
C60.07970 (17)0.21976 (10)0.78645 (13)0.0203 (4)
H6A0.04200.26270.75950.024*
H6B0.10730.19550.73840.024*
C70.25300 (17)0.35974 (9)0.79393 (12)0.0175 (3)
H70.18030.34960.73580.021*
C80.35254 (19)0.40298 (10)0.76581 (14)0.0237 (4)
H8A0.38300.37950.71840.028*
H8B0.42960.41090.82110.028*
C90.2918 (2)0.46947 (10)0.72597 (15)0.0300 (4)
H9A0.35990.49750.71260.036*
H9B0.22170.46180.66650.036*
C100.2346 (2)0.50554 (10)0.79358 (15)0.0291 (4)
H10A0.19300.54720.76470.035*
H10B0.30590.51690.85100.035*
C110.1332 (2)0.46278 (10)0.81885 (16)0.0293 (4)
H11A0.05820.45470.76230.035*
H11B0.10000.48650.86470.035*
C120.19240 (19)0.39641 (9)0.86022 (14)0.0222 (4)
H12A0.12310.36860.87230.027*
H12B0.26080.40420.92050.027*
C130.45996 (16)0.29384 (8)0.95274 (11)0.0147 (3)
H13A0.43990.27611.00830.018*
H13B0.48830.34060.96290.018*
C140.60524 (17)0.16181 (9)0.97685 (12)0.0168 (3)
H140.52880.13310.94480.020*
C150.7263 (2)0.12752 (9)0.96282 (13)0.0231 (4)
H15A0.71890.12680.89560.028*
H15B0.80640.15260.99600.028*
C160.7371 (2)0.05674 (10)1.00019 (14)0.0300 (5)
H16A0.81850.03630.99470.036*
H16B0.66190.03050.96190.036*
C170.7388 (2)0.05499 (11)1.10233 (14)0.0320 (5)
H17A0.73880.00841.12270.038*
H17B0.82010.07621.14180.038*
C180.6198 (2)0.09083 (9)1.11558 (13)0.0243 (4)
H18A0.62590.09071.18260.029*
H18B0.53890.06691.08110.029*
C190.61176 (19)0.16234 (9)1.08058 (12)0.0195 (4)
H19A0.68980.18741.11740.023*
H19B0.53270.18411.08810.023*
C200.73094 (17)0.28521 (9)0.93334 (12)0.0173 (3)
H200.79510.25210.92370.021*
C210.71984 (19)0.33969 (10)0.86050 (13)0.0220 (4)
H21A0.68560.32070.79700.026*
H21B0.65760.37400.86760.026*
C220.8540 (2)0.37096 (10)0.87262 (14)0.0259 (4)
H22A0.84480.40710.82670.031*
H22B0.91390.33730.86030.031*
C230.91271 (19)0.39850 (10)0.97123 (14)0.0250 (4)
H23A1.00130.41640.97800.030*
H23B0.85730.43530.98130.030*
C240.92213 (19)0.34531 (11)1.04445 (14)0.0281 (4)
H24A0.95430.36541.10740.034*
H24B0.98640.31141.03940.034*
C250.78904 (19)0.31208 (11)1.03284 (13)0.0251 (4)
H25A0.80040.27531.07810.030*
H25B0.72780.34461.04610.030*
Cl30.39612 (6)0.01216 (3)0.56653 (4)0.03819 (13)
C260.3451 (16)0.0691 (4)0.6368 (9)0.0492 (10)0.5755 (15)
H26A0.42320.08160.68900.059*0.5755 (15)
H26B0.31490.10950.59920.059*0.5755 (15)
Cl40.22199 (18)0.04556 (6)0.68461 (10)0.0584 (3)0.5755 (15)
C26A0.350 (2)0.0762 (5)0.6273 (12)0.0492 (10)0.4245 (15)
H26C0.42060.10970.64590.059*0.4245 (15)
H26D0.26950.09790.58730.059*0.4245 (15)
Cl4A0.3214 (3)0.04277 (8)0.72482 (14)0.0584 (3)0.4245 (15)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pd10.01279 (6)0.01723 (7)0.01114 (6)0.00052 (5)0.00407 (5)0.00010 (4)
Cl10.0177 (2)0.0280 (2)0.01247 (18)0.00222 (16)0.00295 (15)0.00058 (15)
Cl20.0178 (2)0.0288 (2)0.0184 (2)0.00419 (16)0.00797 (16)−0.00154 (16)
P10.0119 (2)0.0162 (2)0.01268 (19)0.00027 (15)0.00344 (16)0.00006 (15)
P20.0127 (2)0.0175 (2)0.01261 (19)0.00122 (16)0.00358 (16)0.00073 (15)
C10.0129 (8)0.0169 (8)0.0163 (8)−0.0011 (6)0.0059 (6)−0.0009 (6)
C20.0169 (8)0.0174 (8)0.0208 (9)−0.0003 (6)0.0058 (7)0.0001 (6)
C30.0238 (9)0.0188 (9)0.0259 (10)−0.0035 (7)0.0093 (8)−0.0001 (7)
C40.0233 (10)0.0229 (9)0.0302 (10)−0.0073 (7)0.0117 (8)−0.0055 (8)
C50.0136 (8)0.0283 (10)0.0276 (10)−0.0037 (7)0.0060 (7)−0.0033 (8)
C60.0151 (8)0.0260 (9)0.0185 (9)−0.0020 (7)0.0032 (7)−0.0010 (7)
C70.0155 (8)0.0176 (8)0.0177 (8)0.0011 (6)0.0024 (7)0.0023 (6)
C80.0232 (10)0.0227 (9)0.0268 (10)0.0001 (7)0.0099 (8)0.0062 (7)
C90.0315 (11)0.0263 (10)0.0304 (11)−0.0001 (8)0.0066 (9)0.0112 (8)
C100.0264 (10)0.0190 (9)0.0371 (11)0.0027 (8)0.0025 (9)0.0082 (8)
C110.0220 (10)0.0201 (9)0.0449 (13)0.0049 (7)0.0087 (9)0.0034 (8)
C120.0192 (9)0.0196 (9)0.0300 (10)0.0019 (7)0.0107 (8)0.0015 (7)
C130.0129 (8)0.0157 (8)0.0151 (8)0.0006 (6)0.0039 (6)−0.0014 (6)
C140.0174 (8)0.0173 (8)0.0156 (8)0.0023 (6)0.0047 (7)0.0021 (6)
C150.0274 (10)0.0239 (9)0.0205 (9)0.0095 (7)0.0109 (8)0.0041 (7)
C160.0436 (13)0.0243 (10)0.0266 (10)0.0147 (9)0.0172 (9)0.0045 (8)
C170.0474 (13)0.0262 (10)0.0242 (10)0.0160 (9)0.0137 (9)0.0083 (8)
C180.0362 (11)0.0212 (9)0.0174 (9)0.0039 (8)0.0109 (8)0.0021 (7)
C190.0226 (9)0.0205 (9)0.0160 (8)0.0032 (7)0.0070 (7)0.0009 (6)
C200.0119 (8)0.0218 (9)0.0184 (8)0.0009 (6)0.0048 (7)0.0016 (6)
C210.0213 (9)0.0251 (9)0.0177 (9)−0.0048 (7)0.0034 (7)0.0022 (7)
C220.0259 (10)0.0312 (11)0.0226 (9)−0.0083 (8)0.0104 (8)0.0006 (8)
C230.0187 (9)0.0304 (10)0.0243 (10)−0.0052 (8)0.0042 (8)0.0015 (8)
C240.0172 (9)0.0378 (12)0.0246 (10)−0.0061 (8)−0.0007 (8)0.0042 (8)
C250.0200 (9)0.0364 (11)0.0161 (9)−0.0070 (8)0.0015 (7)0.0035 (8)
Cl30.0340 (3)0.0310 (3)0.0464 (3)0.0093 (2)0.0075 (2)0.0033 (2)
C260.053 (2)0.0254 (19)0.078 (3)−0.0104 (18)0.0321 (18)−0.0084 (19)
Cl40.1019 (10)0.0379 (4)0.0566 (7)−0.0043 (7)0.0557 (7)0.0007 (5)
C26A0.053 (2)0.0254 (19)0.078 (3)−0.0104 (18)0.0321 (18)−0.0084 (19)
Cl4A0.1019 (10)0.0379 (4)0.0566 (7)−0.0043 (7)0.0557 (7)0.0007 (5)
Geometric parameters (Å, °) top
Pd1—P12.2205 (4)C13—H13A0.9900
Pd1—P22.2345 (5)C13—H13B0.9900
Pd1—Cl22.3756 (4)C14—C151.539 (2)
Pd1—Cl12.3815 (4)C14—C191.540 (2)
P1—C71.8316 (18)C14—H141.0000
P1—C11.8330 (17)C15—C161.529 (3)
P1—C131.8459 (17)C15—H15A0.9900
P2—C201.8297 (18)C15—H15B0.9900
P2—C141.8435 (18)C16—C171.531 (3)
P2—C131.8464 (17)C16—H16A0.9900
C1—C61.534 (2)C16—H16B0.9900
C1—C21.537 (2)C17—C181.529 (3)
C1—H11.0000C17—H17A0.9900
C2—C31.527 (2)C17—H17B0.9900
C2—H2A0.9900C18—C191.532 (3)
C2—H2B0.9900C18—H18A0.9900
C3—C41.524 (3)C18—H18B0.9900
C3—H3A0.9900C19—H19A0.9900
C3—H3B0.9900C19—H19B0.9900
C4—C51.525 (3)C20—C211.532 (2)
C4—H4A0.9900C20—C251.535 (3)
C4—H4B0.9900C20—H201.0000
C5—C61.531 (3)C21—C221.527 (3)
C5—H5A0.9900C21—H21A0.9900
C5—H5B0.9900C21—H21B0.9900
C6—H6A0.9900C22—C231.529 (3)
C6—H6B0.9900C22—H22A0.9900
C7—C81.533 (2)C22—H22B0.9900
C7—C121.535 (3)C23—C241.520 (3)
C7—H71.0000C23—H23A0.9900
C8—C91.533 (3)C23—H23B0.9900
C8—H8A0.9900C24—C251.536 (3)
C8—H8B0.9900C24—H24A0.9900
C9—C101.522 (3)C24—H24B0.9900
C9—H9A0.9900C25—H25A0.9900
C9—H9B0.9900C25—H25B0.9900
C10—C111.523 (3)Cl3—C26A1.740 (9)
C10—H10A0.9900Cl3—C261.757 (6)
C10—H10B0.9900C26—Cl41.747 (9)
C11—C121.533 (3)C26—H26A0.9900
C11—H11A0.9900C26—H26B0.9900
C11—H11B0.9900C26A—Cl4A1.724 (9)
C12—H12A0.9900C26A—H26C0.9900
C12—H12B0.9900C26A—H26D0.9900
P1—Pd1—P273.816 (16)P1—C13—P292.87 (8)
P1—Pd1—Cl2170.092 (17)P1—C13—H13A113.1
P2—Pd1—Cl296.291 (16)P2—C13—H13A113.1
P1—Pd1—Cl193.670 (16)P1—C13—H13B113.1
P2—Pd1—Cl1167.313 (16)P2—C13—H13B113.1
Cl2—Pd1—Cl196.195 (16)H13A—C13—H13B110.5
C7—P1—C1108.02 (8)C15—C14—C19111.11 (14)
C7—P1—C13110.87 (8)C15—C14—P2110.30 (12)
C1—P1—C13107.22 (8)C19—C14—P2117.28 (12)
C7—P1—Pd1115.18 (6)C15—C14—H14105.8
C1—P1—Pd1118.46 (6)C19—C14—H14105.8
C13—P1—Pd196.16 (5)P2—C14—H14105.8
C20—P2—C14109.44 (8)C16—C15—C14110.13 (16)
C20—P2—C13109.67 (8)C16—C15—H15A109.6
C14—P2—C13111.74 (8)C14—C15—H15A109.6
C20—P2—Pd1116.70 (6)C16—C15—H15B109.6
C14—P2—Pd1112.93 (6)C14—C15—H15B109.6
C13—P2—Pd195.67 (5)H15A—C15—H15B108.1
C6—C1—C2110.56 (14)C15—C16—C17111.53 (17)
C6—C1—P1112.12 (12)C15—C16—H16A109.3
C2—C1—P1111.10 (12)C17—C16—H16A109.3
C6—C1—H1107.6C15—C16—H16B109.3
C2—C1—H1107.6C17—C16—H16B109.3
P1—C1—H1107.6H16A—C16—H16B108.0
C3—C2—C1110.67 (15)C18—C17—C16111.26 (17)
C3—C2—H2A109.5C18—C17—H17A109.4
C1—C2—H2A109.5C16—C17—H17A109.4
C3—C2—H2B109.5C18—C17—H17B109.4
C1—C2—H2B109.5C16—C17—H17B109.4
H2A—C2—H2B108.1H17A—C17—H17B108.0
C4—C3—C2111.16 (16)C17—C18—C19111.40 (17)
C4—C3—H3A109.4C17—C18—H18A109.3
C2—C3—H3A109.4C19—C18—H18A109.3
C4—C3—H3B109.4C17—C18—H18B109.3
C2—C3—H3B109.4C19—C18—H18B109.3
H3A—C3—H3B108.0H18A—C18—H18B108.0
C3—C4—C5110.65 (16)C18—C19—C14108.78 (15)
C3—C4—H4A109.5C18—C19—H19A109.9
C5—C4—H4A109.5C14—C19—H19A109.9
C3—C4—H4B109.5C18—C19—H19B109.9
C5—C4—H4B109.5C14—C19—H19B109.9
H4A—C4—H4B108.1H19A—C19—H19B108.3
C4—C5—C6111.93 (15)C21—C20—C25111.28 (15)
C4—C5—H5A109.2C21—C20—P2111.44 (12)
C6—C5—H5A109.2C25—C20—P2113.85 (12)
C4—C5—H5B109.2C21—C20—H20106.6
C6—C5—H5B109.2C25—C20—H20106.6
H5A—C5—H5B107.9P2—C20—H20106.6
C5—C6—C1110.42 (15)C22—C21—C20110.22 (15)
C5—C6—H6A109.6C22—C21—H21A109.6
C1—C6—H6A109.6C20—C21—H21A109.6
C5—C6—H6B109.6C22—C21—H21B109.6
C1—C6—H6B109.6C20—C21—H21B109.6
H6A—C6—H6B108.1H21A—C21—H21B108.1
C8—C7—C12111.66 (15)C21—C22—C23111.20 (16)
C8—C7—P1111.21 (12)C21—C22—H22A109.4
C12—C7—P1111.78 (12)C23—C22—H22A109.4
C8—C7—H7107.3C21—C22—H22B109.4
C12—C7—H7107.3C23—C22—H22B109.4
P1—C7—H7107.3H22A—C22—H22B108.0
C7—C8—C9111.12 (16)C24—C23—C22111.22 (17)
C7—C8—H8A109.4C24—C23—H23A109.4
C9—C8—H8A109.4C22—C23—H23A109.4
C7—C8—H8B109.4C24—C23—H23B109.4
C9—C8—H8B109.4C22—C23—H23B109.4
H8A—C8—H8B108.0H23A—C23—H23B108.0
C10—C9—C8111.56 (17)C23—C24—C25111.80 (16)
C10—C9—H9A109.3C23—C24—H24A109.3
C8—C9—H9A109.3C25—C24—H24A109.3
C10—C9—H9B109.3C23—C24—H24B109.3
C8—C9—H9B109.3C25—C24—H24B109.3
H9A—C9—H9B108.0H24A—C24—H24B107.9
C9—C10—C11110.84 (18)C20—C25—C24110.69 (16)
C9—C10—H10A109.5C20—C25—H25A109.5
C11—C10—H10A109.5C24—C25—H25A109.5
C9—C10—H10B109.5C20—C25—H25B109.5
C11—C10—H10B109.5C24—C25—H25B109.5
H10A—C10—H10B108.1H25A—C25—H25B108.1
C10—C11—C12111.10 (16)Cl4—C26—Cl3118.6 (6)
C10—C11—H11A109.4Cl4—C26—H26A107.7
C12—C11—H11A109.4Cl3—C26—H26A107.7
C10—C11—H11B109.4Cl4—C26—H26B107.7
C12—C11—H11B109.4Cl3—C26—H26B107.7
H11A—C11—H11B108.0H26A—C26—H26B107.1
C11—C12—C7111.31 (16)Cl4A—C26A—Cl3107.8 (6)
C11—C12—H12A109.4Cl4A—C26A—H26C110.1
C7—C12—H12A109.4Cl3—C26A—H26C110.1
C11—C12—H12B109.4Cl4A—C26A—H26D110.1
C7—C12—H12B109.4Cl3—C26A—H26D110.1
H12A—C12—H12B108.0H26C—C26A—H26D108.5
Table 1
Selected geometric parameters (Å, °) top
Pd1—P12.2205 (4)Pd1—Cl22.3756 (4)
Pd1—P22.2345 (5)Pd1—Cl12.3815 (4)
P1—Pd1—P273.816 (16)P1—Pd1—Cl193.670 (16)
P1—Pd1—Cl2170.092 (17)P2—Pd1—Cl1167.313 (16)
P2—Pd1—Cl296.291 (16)Cl2—Pd1—Cl196.195 (16)
Acknowledgements top

We thank the Chemistry Department of Tulane University for support of the X-ray laboratory and the Louisiana Board of Regents, through the Louisiana Educational Quality Support Fund (Grant LEQSF (2003–2003)-ENH –TR-67), for the purchase of the APEX diffractometer. This work was also partially supported by DOE/EPSCOR Grant DE—FG02–03ER4646 (to MJF).

references
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