supplementary materials


HTML versionpdf versioncif file3d viewstructure factorssupplementary materialsCIF check reportsimilar papers Open access

gk2195 scheme

Acta Cryst. (2009). E65, m669    [ doi:10.1107/S1600536809018133 ]

Bis[1,3([eta]3)-allyl][[mu]-2([eta]4)-1,3-bis(diphenylphosphino)-2,4-diphenylcyclobuta-1,3-diene-1:3[kappa]2P:P']dichlorido-1[kappa]Cl,3[kappa]Cl-[2([eta]5)-isopropylcyclopentadienyl]-2-cobalt(I)-1,3-dipalladium(II) dichloromethane solvate

C.-P. Chang and F.-E. Hong

Abstract top

In the title complex, [CoPd2(C3H5)2(C8H11)Cl2(C40H30P2)]·CH2Cl2, the CoI atom is sandwiched between the cyclopentadienyl and cyclobutadiene rings. The two diphenylphosphine substituents of the cyclobutadiene ring are situated opposite to each other and bind two PdII atoms, which are additionally coordinated by a chloride ion and the three C atoms of an allyl ligand, forming a distorted planar coordination environment. The Cl atoms of the dichloromethane solvent molecule (equal occupancies) and one C atom and its attached H atom of each of the allyl ligands (occupancies 0.55:0.45) are disordered.

Comment top

Recently, we have synthesized a series of cobalt-containing phosphine-coordinated palladium complexes which have shown high activities in the Suzuki-Miyaura reaction (Chang et al., 2005). We report herein the synthesis and crystal structure of a cobalt-containing phosphine coordinated palladium complex, a potential catalyst for cross-coupling reactions.

The crystal structure of the title compound reveals that it is a CoI sandwich complex (Figure 1) containing two diphenylphosphino-coordinated palladium moieties attached to the cyclobutadiene ring. The two rings sandwiching the Co atom, cyclopentadienyl and cyclobutadiene, are almost parallel to each other [dihedral angle of 8.46 (8)° ]. The cyclopentadienyl ring bears an isopropyl group as a substituent. The palladium atoms are pentacoordinated; they bind to a chloride ion, a phosphorous atom from the diphenylphosphine ligand and three carbon atoms from the disordered allylic group.

Related literature top

For applications of cobalt-containing phosphine-coordinated palladium complexes, see: Chang & Hong (2005).

Experimental top

A 100 ml round-bottomed Schlenk flask equipped with a magnetic stirbar and a rubber septum was charged with allylpalladium(II) chloride dimer (0.05 g, 0.15 mmol), (η5-C5H4iPr)Co(η4-1,3-Ph2-2,4-(PPh2)2C4)(0.11 g, 0.15 mmol) and 10 ml CH2Cl2. After stirring at room temperature for 1 h, the solvent was removed under reduced pressure. The yellow-colored residue was purified by CTLC (Chromatotron, Harrison model 8924) employed EA/CH2Cl2=1:1 mixed solvent. The isolated product was identified as the title compound by spectroscopic methods. 1H NMR (CDCl3, 400 MHz): δ 7.02–8.01 (m, 30H), 5.41 (m, 1H), 4.06 (d, 2H), 2.98 (d, 2H), 0.31 (d, 6H) p.p.m. 13C{1H} NMR (CDCl3, 100 MHz): δ 127.5–132.9, 135.6, 82.0, 80.4, 24.3, 22.0 p.p.m. 31P{1H} NMR (CDCl3, 100 MHz): δ8.6 p.p.m. LRMS: m/s = 1027 [M—Cl]+, [C57H59Cl2CoP2Pd2]. The yield was 53% (0.09 g, 0.08 mmol).

Refinement top

All H atoms were placed in geometrically idealized positions and constrained to ride on their parent atoms with C—H distances in the range 0.93–0.98 Å and Uiso(H) = 1.2Ueq(C). The two allyl groups and the dichloromethane molecule are disordered over two positions with the occupancy factors ratio of 55:45 for the allyl groups and 50:50 for the solvent molecule.

Computing details top

Data collection: SMART (Bruker, 1999); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT (Bruker, 1999); 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. A view of the molecular structure of the title compound with displacement ellipsoids shown at the 40% probability level. Hydrogen atoms have been omitted for clarity.
Bis[1,3(η3)-allyl][µ-2(η4)-1,3-bis(diphenylphosphino)-2,4- diphenylcyclobuta-1,3-diene-κ2P:P']dichlorido- 1κCl,3κCl-[2(η5)-isopropylcyclopentadienyl]-2- cobalt(I)-1,3-dipalladium(II) dichloromethane solvate top
Crystal data top
[CoPd2(C3H5)2(C8H11)Cl2(C40H30P2)]·CH2Cl2Z = 2
Mr = 1189.44F000 = 1198
Triclinic, P1Dx = 1.536 Mg m−3
Hall symbol: -P 1Mo Kα radiation
λ = 0.71073 Å
a = 10.889 (4) ÅCell parameters from 4357 reflections
b = 12.499 (4) Åθ = 2.2–25.4º
c = 21.746 (8) ŵ = 1.32 mm−1
α = 94.617 (7)ºT = 298 K
β = 102.136 (7)ºParallelepiped, yellow
γ = 115.166 (7)º0.25 × 0.20 × 0.15 mm
V = 2570.1 (16) Å3
Data collection top
Bruker SMART 1000 CCD
diffractometer		10003 independent reflections
Radiation source: fine-focus sealed tube6379 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.033
Detector resolution: 0 pixels mm-1θmax = 26.1º
T = 298 Kθmin = 2.0º
φ and ω scansh = −13→9
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		k = −15→14
Tmin = 0.734, Tmax = 0.827l = −24→26
14882 measured reflections
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)] = 0.047H-atom parameters constrained
wR(F2) = 0.126  w = 1/[σ2(Fo2) + (0.06P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.98(Δ/σ)max < 0.001
10003 reflectionsΔρmax = 0.60 e Å−3
608 parametersΔρmin = −0.59 e Å−3
Primary atom site location: structure-invariant direct methodsExtinction correction: none
Crystal data top
[CoPd2(C3H5)2(C8H11)Cl2(C40H30P2)]·CH2Cl2γ = 115.166 (7)º
Mr = 1189.44V = 2570.1 (16) Å3
Triclinic, P1Z = 2
a = 10.889 (4) ÅMo Kα
b = 12.499 (4) ŵ = 1.32 mm−1
c = 21.746 (8) ÅT = 298 K
α = 94.617 (7)º0.25 × 0.20 × 0.15 mm
β = 102.136 (7)º
Data collection top
Bruker SMART 1000 CCD
diffractometer		10003 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		6379 reflections with I > 2σ(I)
Tmin = 0.734, Tmax = 0.827Rint = 0.033
14882 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.047608 parameters
wR(F2) = 0.126H-atom parameters constrained
S = 0.98Δρmax = 0.60 e Å−3
10003 reflectionsΔρmin = −0.59 e Å−3
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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*/UeqOcc. (<1)
Pd10.72416 (5)0.71604 (4)0.45564 (2)0.04002 (13)
Co10.45423 (7)0.73312 (6)0.26318 (3)0.03195 (17)
P10.76022 (14)0.84931 (11)0.38561 (6)0.0323 (3)
C10.3718 (7)0.8474 (6)0.2772 (3)0.0563 (17)
H10.42240.93080.28400.068*
Pd20.53088 (5)0.78107 (4)0.06221 (2)0.04233 (13)
P20.51015 (14)0.63486 (11)0.12431 (6)0.0331 (3)
C20.2990 (6)0.7701 (6)0.2175 (3)0.0592 (18)
H20.29270.79340.17790.071*
C30.2363 (6)0.6497 (6)0.2280 (3)0.0530 (15)
H30.18430.58070.19630.064*
C40.2667 (5)0.6531 (5)0.2947 (3)0.0430 (13)
C50.3551 (6)0.7764 (5)0.3256 (3)0.0476 (14)
H50.39460.80500.36940.057*
C60.6348 (5)0.8196 (4)0.2430 (2)0.0310 (11)
C70.6545 (5)0.7806 (4)0.3037 (2)0.0301 (11)
C80.5800 (5)0.6533 (4)0.2708 (2)0.0315 (11)
C90.5603 (5)0.6945 (4)0.2091 (2)0.0313 (11)
C100.6979 (6)0.9356 (4)0.2197 (2)0.0351 (12)
C110.8424 (6)0.9924 (5)0.2267 (3)0.0501 (15)
H110.89760.95710.24480.060*
C120.9045 (7)1.1006 (6)0.2071 (3)0.0649 (19)
H121.00141.13800.21240.078*
C130.8247 (8)1.1533 (5)0.1798 (3)0.071 (2)
H130.86691.22570.16620.085*
C140.6823 (7)1.0987 (5)0.1727 (3)0.0618 (18)
H140.62791.13500.15510.074*
C150.6191 (6)0.9894 (5)0.1917 (3)0.0481 (14)
H150.52200.95180.18550.058*
C160.5674 (5)0.5406 (4)0.2916 (2)0.0329 (11)
C170.5024 (6)0.5014 (5)0.3394 (3)0.0457 (14)
H170.46710.54710.35870.055*
C180.4891 (7)0.3958 (6)0.3589 (3)0.0638 (18)
H180.44430.37010.39070.077*
C190.5425 (8)0.3279 (6)0.3310 (4)0.070 (2)
H190.53080.25530.34310.084*
C200.6126 (8)0.3672 (6)0.2853 (3)0.072 (2)
H200.65160.32300.26770.086*
C210.9370 (5)0.9072 (4)0.3733 (2)0.0331 (11)
C220.9643 (6)0.8345 (5)0.3321 (3)0.0444 (13)
H220.89290.75830.31170.053*
C231.0946 (6)0.8727 (5)0.3208 (3)0.0526 (15)
H231.11170.82220.29380.063*
C241.1996 (6)0.9865 (6)0.3500 (3)0.0676 (19)
H241.28691.01410.34130.081*
C251.1763 (6)1.0592 (6)0.3916 (3)0.0650 (19)
H251.24801.13520.41200.078*
C261.0448 (6)1.0188 (5)0.4032 (3)0.0496 (15)
H261.02941.06810.43180.060*
C270.7412 (5)0.9859 (4)0.4061 (2)0.0371 (12)
C280.6891 (6)0.9970 (5)0.4581 (3)0.0567 (17)
H280.66390.93540.48130.068*
C290.6744 (7)1.0980 (6)0.4754 (4)0.070 (2)
H290.63991.10480.51040.084*
C300.7105 (7)1.1895 (6)0.4411 (4)0.069 (2)
H300.69791.25690.45210.083*
C310.7647 (8)1.1807 (6)0.3910 (3)0.0651 (18)
H310.79241.24360.36870.078*
C320.7787 (7)1.0783 (5)0.3731 (3)0.0548 (16)
H320.81411.07240.33830.066*
C330.3390 (5)0.5024 (4)0.1043 (2)0.0382 (12)
C340.2326 (6)0.4928 (5)0.0537 (3)0.0612 (17)
H340.24960.55360.02990.073*
C350.0994 (7)0.3932 (6)0.0373 (4)0.078 (2)
H350.02810.38880.00350.093*
C360.0750 (7)0.3034 (6)0.0711 (3)0.0667 (19)
H36−0.01300.23650.06010.080*
C370.1786 (7)0.3106 (6)0.1209 (3)0.0675 (19)
H370.16060.24890.14420.081*
C380.3102 (6)0.4083 (5)0.1375 (3)0.0559 (16)
H380.38060.41100.17130.067*
C390.6377 (5)0.5762 (5)0.1229 (2)0.0382 (12)
C400.7772 (6)0.6478 (5)0.1557 (3)0.0477 (14)
H400.80410.72490.17750.057*
C410.8782 (6)0.6077 (6)0.1572 (3)0.0610 (17)
H410.97170.65770.17950.073*
C420.8399 (8)0.4940 (7)0.1257 (3)0.070 (2)
H420.90690.46600.12760.084*
C430.7029 (8)0.4219 (6)0.0914 (3)0.070 (2)
H430.67730.34560.06920.084*
C440.6018 (7)0.4626 (5)0.0898 (3)0.0535 (15)
H440.50900.41320.06640.064*
C520.2038 (6)0.5526 (5)0.3285 (3)0.0533 (15)
H520.27890.55800.36450.064*
C530.6248 (7)0.4743 (5)0.2656 (3)0.0511 (15)
H530.67210.50120.23470.061*
C540.0937 (8)0.5682 (8)0.3559 (4)0.101 (3)
H54A0.13620.64550.38370.151*
H54B0.05670.50600.37970.151*
H54C0.01860.56300.32150.151*
C550.1415 (8)0.4290 (6)0.2856 (4)0.089 (2)
H55A0.06820.42180.24960.133*
H55B0.10310.36740.30950.133*
H55C0.21410.42000.27050.133*
Cl10.51400 (16)0.70395 (13)0.47871 (7)0.0526 (4)
Cl20.31495 (17)0.79401 (14)0.05176 (8)0.0607 (4)
C480.7290 (7)0.8105 (6)0.0497 (3)0.073 (2)
H48A0.67570.76330.07680.087*
H48B0.82150.81570.05250.087*
C470.7535 (9)0.5996 (7)0.5217 (4)0.090 (3)
H47A0.67870.62370.51400.107*
H47B0.75540.55200.55460.107*
C490.6587 (12)0.8395 (9)−0.0045 (5)0.042 (3)0.55
H49A0.71390.8581−0.03580.050*0.55
C49'0.697 (3)0.886 (2)0.0259 (12)0.105 (9)*0.45
H49B0.78390.94170.01690.126*0.45
C460.8156 (14)0.5940 (10)0.4751 (6)0.052 (3)0.55
H460.85620.53790.48150.063*0.55
C46'0.862 (2)0.6582 (17)0.5070 (10)0.078 (5)*0.45
H46'0.93630.64590.53480.093*0.45
C450.9043 (8)0.6902 (7)0.4564 (4)0.082 (2)
H45A0.99420.69590.45300.099*
H45B0.86740.73630.43150.099*
C500.6146 (9)0.9242 (7)0.0062 (4)0.092 (3)
H50A0.64360.9933−0.01450.110*
H50B0.53290.90450.02260.110*
Cl4'1.3448 (8)1.1123 (8)0.1784 (6)0.137 (3)0.50
Cl3'1.0857 (6)0.9245 (8)0.1500 (5)0.175 (3)0.50
Cl31.0708 (6)0.9902 (5)0.0675 (4)0.160 (3)0.50
Cl41.276 (3)1.067 (2)0.1853 (10)0.376 (15)0.50
C561.2044 (18)0.9887 (15)0.1210 (8)0.181 (7)
H56A1.17091.01750.08410.217*
H56B1.23800.93320.10660.217*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pd10.0423 (3)0.0414 (2)0.0371 (2)0.0195 (2)0.01012 (19)0.00980 (18)
Co10.0251 (3)0.0379 (4)0.0374 (4)0.0164 (3)0.0113 (3)0.0112 (3)
P10.0309 (7)0.0332 (7)0.0332 (7)0.0155 (6)0.0088 (6)0.0039 (6)
C10.050 (4)0.052 (4)0.092 (5)0.034 (3)0.041 (4)0.028 (4)
Pd20.0447 (3)0.0415 (3)0.0407 (3)0.0177 (2)0.0134 (2)0.01344 (19)
P20.0294 (7)0.0344 (7)0.0332 (7)0.0123 (6)0.0085 (6)0.0065 (6)
C20.038 (3)0.098 (5)0.069 (5)0.047 (4)0.025 (3)0.043 (4)
C30.024 (3)0.072 (4)0.056 (4)0.016 (3)0.011 (3)0.010 (3)
C40.026 (3)0.056 (4)0.052 (4)0.019 (3)0.019 (3)0.016 (3)
C50.044 (3)0.060 (4)0.053 (4)0.031 (3)0.026 (3)0.014 (3)
C60.028 (3)0.031 (3)0.038 (3)0.016 (2)0.011 (2)0.006 (2)
C70.026 (3)0.031 (3)0.037 (3)0.015 (2)0.012 (2)0.007 (2)
C80.027 (3)0.036 (3)0.034 (3)0.016 (2)0.009 (2)0.005 (2)
C90.025 (3)0.037 (3)0.032 (3)0.013 (2)0.010 (2)0.006 (2)
C100.042 (3)0.029 (3)0.032 (3)0.013 (2)0.012 (2)0.004 (2)
C110.038 (3)0.048 (3)0.055 (4)0.010 (3)0.014 (3)0.013 (3)
C120.055 (4)0.056 (4)0.066 (4)0.003 (4)0.026 (4)0.024 (3)
C130.078 (5)0.037 (3)0.081 (5)0.007 (4)0.027 (4)0.024 (3)
C140.070 (5)0.048 (4)0.065 (4)0.024 (4)0.014 (4)0.022 (3)
C150.051 (4)0.043 (3)0.055 (4)0.022 (3)0.019 (3)0.020 (3)
C160.030 (3)0.034 (3)0.031 (3)0.014 (2)0.000 (2)0.004 (2)
C170.041 (3)0.053 (3)0.050 (3)0.026 (3)0.014 (3)0.020 (3)
C180.062 (4)0.066 (4)0.067 (4)0.025 (4)0.024 (4)0.032 (4)
C190.081 (5)0.044 (4)0.083 (5)0.032 (4)0.008 (4)0.023 (4)
C200.105 (6)0.061 (4)0.078 (5)0.060 (5)0.028 (5)0.022 (4)
C210.029 (3)0.036 (3)0.034 (3)0.018 (2)0.003 (2)0.003 (2)
C220.031 (3)0.045 (3)0.057 (4)0.019 (3)0.011 (3)0.005 (3)
C230.039 (3)0.059 (4)0.059 (4)0.024 (3)0.013 (3)−0.003 (3)
C240.030 (3)0.087 (5)0.079 (5)0.021 (4)0.018 (3)0.003 (4)
C250.036 (3)0.053 (4)0.082 (5)0.003 (3)0.015 (3)−0.011 (3)
C260.033 (3)0.051 (4)0.053 (4)0.013 (3)0.008 (3)−0.005 (3)
C270.039 (3)0.039 (3)0.037 (3)0.023 (3)0.007 (2)0.003 (2)
C280.062 (4)0.042 (3)0.072 (4)0.022 (3)0.038 (4)0.004 (3)
C290.074 (5)0.064 (4)0.085 (5)0.036 (4)0.041 (4)0.000 (4)
C300.075 (5)0.053 (4)0.087 (5)0.046 (4)0.007 (4)−0.006 (4)
C310.087 (5)0.056 (4)0.065 (4)0.046 (4)0.014 (4)0.017 (3)
C320.077 (5)0.053 (4)0.044 (3)0.040 (4)0.014 (3)0.004 (3)
C330.035 (3)0.034 (3)0.038 (3)0.008 (2)0.012 (2)0.001 (2)
C340.043 (4)0.049 (4)0.071 (4)0.010 (3)0.000 (3)0.013 (3)
C350.047 (4)0.062 (4)0.084 (5)0.005 (4)−0.017 (4)0.008 (4)
C360.039 (4)0.052 (4)0.082 (5)0.002 (3)0.009 (4)0.002 (4)
C370.058 (4)0.053 (4)0.071 (5)0.003 (4)0.021 (4)0.020 (3)
C380.047 (4)0.053 (4)0.057 (4)0.015 (3)0.006 (3)0.017 (3)
C390.036 (3)0.040 (3)0.038 (3)0.015 (3)0.014 (2)0.006 (2)
C400.041 (3)0.054 (4)0.050 (4)0.024 (3)0.014 (3)0.007 (3)
C410.039 (3)0.077 (5)0.069 (4)0.030 (4)0.014 (3)0.002 (4)
C420.067 (5)0.101 (6)0.065 (5)0.061 (5)0.017 (4)0.004 (4)
C430.080 (5)0.072 (5)0.071 (5)0.051 (4)0.015 (4)−0.008 (4)
C440.050 (4)0.058 (4)0.049 (4)0.027 (3)0.003 (3)0.000 (3)
C520.038 (3)0.061 (4)0.062 (4)0.019 (3)0.020 (3)0.025 (3)
C530.068 (4)0.056 (4)0.046 (3)0.039 (3)0.023 (3)0.018 (3)
C540.079 (6)0.121 (7)0.146 (8)0.051 (5)0.085 (6)0.080 (6)
C550.077 (6)0.067 (5)0.097 (6)0.009 (4)0.021 (5)0.024 (4)
Cl10.0488 (9)0.0544 (9)0.0561 (9)0.0202 (8)0.0234 (7)0.0133 (7)
Cl20.0568 (10)0.0636 (10)0.0678 (10)0.0341 (9)0.0130 (8)0.0171 (8)
C480.042 (4)0.103 (6)0.096 (6)0.033 (4)0.049 (4)0.060 (5)
C470.096 (6)0.110 (6)0.110 (7)0.074 (6)0.042 (5)0.079 (5)
C490.050 (7)0.036 (6)0.037 (6)0.006 (5)0.035 (5)0.012 (5)
C460.073 (8)0.045 (7)0.053 (7)0.045 (7)0.004 (7)0.015 (6)
C450.077 (5)0.113 (6)0.111 (6)0.078 (5)0.042 (5)0.065 (5)
C500.099 (6)0.098 (6)0.120 (7)0.049 (5)0.081 (6)0.082 (6)
Cl4'0.096 (4)0.098 (4)0.166 (8)0.042 (3)−0.037 (4)−0.031 (4)
Cl3'0.082 (4)0.233 (8)0.229 (8)0.060 (5)0.078 (5)0.115 (7)
Cl30.067 (3)0.119 (4)0.253 (8)0.008 (3)0.058 (4)−0.015 (5)
Cl40.64 (4)0.56 (3)0.214 (15)0.53 (3)0.08 (2)0.11 (2)
C560.239 (18)0.266 (18)0.162 (14)0.200 (16)0.111 (14)0.064 (13)
Geometric parameters (Å, °) top
Pd1—C46'2.09 (2)C25—H250.9300
Pd1—C452.116 (6)C26—H260.9300
Pd1—C462.171 (10)C27—C321.368 (7)
Pd1—C472.195 (6)C27—C281.389 (7)
Pd1—P12.3132 (15)C28—C291.372 (8)
Pd1—Cl12.3901 (17)C28—H280.9300
Co1—C61.964 (5)C29—C301.378 (9)
Co1—C71.973 (5)C29—H290.9300
Co1—C91.976 (5)C30—C311.361 (9)
Co1—C81.998 (5)C30—H300.9300
Co1—C12.018 (5)C31—C321.387 (8)
Co1—C22.022 (5)C31—H310.9300
Co1—C52.072 (5)C32—H320.9300
Co1—C32.075 (5)C33—C341.376 (8)
Co1—C42.146 (5)C33—C381.386 (7)
P1—C71.813 (5)C34—C351.399 (8)
P1—C211.835 (5)C34—H340.9300
P1—C271.837 (5)C35—C361.354 (9)
C1—C21.400 (9)C35—H350.9300
C1—C51.421 (8)C36—C371.355 (9)
C1—H10.9300C36—H360.9300
Pd2—C482.110 (6)C37—C381.378 (8)
Pd2—C49'2.09 (3)C37—H370.9300
Pd2—C492.174 (9)C38—H380.9300
Pd2—C502.223 (6)C39—C401.380 (7)
Pd2—P22.3215 (15)C39—C441.389 (7)
Pd2—Cl22.3897 (18)C40—C411.384 (8)
P2—C91.806 (5)C40—H400.9300
P2—C331.823 (5)C41—C421.372 (9)
P2—C391.830 (5)C41—H410.9300
C2—C31.424 (8)C42—C431.369 (9)
C2—H20.9300C42—H420.9300
C3—C41.412 (8)C43—C441.391 (8)
C3—H30.9300C43—H430.9300
C4—C51.433 (8)C44—H440.9300
C4—C521.489 (7)C52—C541.520 (8)
C5—H50.9300C52—C551.526 (9)
C6—C71.449 (6)C52—H520.9800
C6—C91.460 (6)C53—H530.9300
C6—C101.500 (6)C54—H54A0.9600
C7—C81.475 (6)C54—H54B0.9600
C8—C161.473 (7)C54—H54C0.9600
C8—C91.482 (6)C55—H55A0.9600
C10—C151.377 (7)C55—H55B0.9600
C10—C111.390 (7)C55—H55C0.9600
C11—C121.381 (8)C48—C49'1.25 (3)
C11—H110.9300C48—C491.425 (14)
C12—C131.369 (9)C48—H48A0.9700
C12—H120.9300C48—H48B0.9700
C13—C141.370 (9)C47—C46'1.222 (19)
C13—H130.9300C47—C461.344 (14)
C14—C151.386 (7)C47—H47A0.9700
C14—H140.9300C47—H47B0.9700
C15—H150.9300C49—C49'0.75 (2)
C16—C531.382 (7)C49—C501.358 (13)
C16—C171.386 (7)C49—H49A0.9800
C17—C181.377 (8)C49'—C501.21 (3)
C17—H170.9300C49'—H49B0.9800
C18—C191.382 (9)C46—C46'0.893 (18)
C18—H180.9300C46—C451.342 (13)
C19—C201.374 (9)C46—H460.9800
C19—H190.9300C46'—C451.31 (2)
C20—C531.400 (8)C46'—H46'0.9800
C20—H200.9300C45—H45A0.9700
C21—C261.374 (7)C45—H45B0.9700
C21—C221.387 (7)C50—H50A0.9700
C22—C231.375 (7)C50—H50B0.9700
C22—H220.9300Cl4'—C561.78 (2)
C23—C241.379 (8)Cl3'—C561.502 (14)
C23—H230.9300Cl3—C561.670 (17)
C24—C251.367 (8)Cl4—C561.48 (2)
C24—H240.9300C56—H56A0.9700
C25—C261.387 (8)C56—H56B0.9700
C46'—Pd1—C4536.2 (5)C18—C17—C16121.1 (6)
C46'—Pd1—C4624.1 (5)C18—C17—H17119.5
C45—Pd1—C4636.5 (4)C16—C17—H17119.5
C46'—Pd1—C4733.0 (5)C17—C18—C19119.8 (6)
C45—Pd1—C4766.9 (3)C17—C18—H18120.1
C46—Pd1—C4735.9 (4)C19—C18—H18120.1
C46'—Pd1—P1130.0 (5)C20—C19—C18120.4 (6)
C45—Pd1—P196.36 (19)C20—C19—H19119.8
C46—Pd1—P1129.6 (4)C18—C19—H19119.8
C47—Pd1—P1163.0 (2)C19—C20—C53119.3 (6)
C46'—Pd1—Cl1126.2 (6)C19—C20—H20120.3
C45—Pd1—Cl1161.9 (2)C53—C20—H20120.3
C46—Pd1—Cl1126.6 (4)C26—C21—C22118.1 (5)
C47—Pd1—Cl194.9 (2)C26—C21—P1123.4 (4)
P1—Pd1—Cl1101.77 (5)C22—C21—P1118.6 (4)
C6—Co1—C743.20 (19)C23—C22—C21121.4 (5)
C6—Co1—C943.51 (19)C23—C22—H22119.3
C7—Co1—C963.05 (19)C21—C22—H22119.3
C6—Co1—C863.45 (19)C22—C23—C24119.3 (5)
C7—Co1—C843.60 (19)C22—C23—H23120.3
C9—Co1—C843.78 (19)C24—C23—H23120.3
C6—Co1—C1109.4 (2)C25—C24—C23120.4 (6)
C7—Co1—C1120.6 (2)C25—C24—H24119.8
C9—Co1—C1141.4 (2)C23—C24—H24119.8
C8—Co1—C1163.6 (3)C24—C25—C26119.6 (6)
C6—Co1—C2114.4 (2)C24—C25—H25120.2
C7—Co1—C2151.5 (2)C26—C25—H25120.2
C9—Co1—C2116.0 (2)C21—C26—C25121.2 (5)
C8—Co1—C2155.2 (3)C21—C26—H26119.4
C1—Co1—C240.5 (3)C25—C26—H26119.4
C6—Co1—C5134.4 (2)C32—C27—C28118.5 (5)
C7—Co1—C5112.9 (2)C32—C27—P1122.7 (4)
C9—Co1—C5175.9 (2)C28—C27—P1118.7 (4)
C8—Co1—C5132.9 (2)C29—C28—C27120.6 (6)
C1—Co1—C540.6 (2)C29—C28—H28119.7
C2—Co1—C567.9 (2)C27—C28—H28119.7
C6—Co1—C3145.7 (2)C28—C29—C30120.2 (6)
C7—Co1—C3167.8 (2)C28—C29—H29119.9
C9—Co1—C3116.7 (2)C30—C29—H29119.9
C8—Co1—C3126.7 (2)C31—C30—C29119.6 (6)
C1—Co1—C368.0 (3)C31—C30—H30120.2
C2—Co1—C340.7 (2)C29—C30—H30120.2
C5—Co1—C367.1 (2)C30—C31—C32120.2 (6)
C6—Co1—C4173.7 (2)C30—C31—H31119.9
C7—Co1—C4133.2 (2)C32—C31—H31119.9
C9—Co1—C4142.2 (2)C27—C32—C31120.8 (6)
C8—Co1—C4118.2 (2)C27—C32—H32119.6
C1—Co1—C467.2 (2)C31—C32—H32119.6
C2—Co1—C466.9 (2)C34—C33—C38117.5 (5)
C5—Co1—C439.7 (2)C34—C33—P2119.6 (4)
C3—Co1—C439.0 (2)C38—C33—P2123.0 (5)
C7—P1—C2199.7 (2)C33—C34—C35121.2 (6)
C7—P1—C27106.7 (2)C33—C34—H34119.4
C21—P1—C27103.7 (2)C35—C34—H34119.4
C7—P1—Pd1113.91 (16)C36—C35—C34119.6 (7)
C21—P1—Pd1112.87 (16)C36—C35—H35120.2
C27—P1—Pd1117.94 (17)C34—C35—H35120.2
C2—C1—C5108.2 (6)C37—C36—C35120.2 (6)
C2—C1—Co169.9 (3)C37—C36—H36119.9
C5—C1—Co171.7 (3)C35—C36—H36119.9
C2—C1—H1125.9C36—C37—C38120.8 (6)
C5—C1—H1125.9C36—C37—H37119.6
Co1—C1—H1124.2C38—C37—H37119.6
C48—Pd2—C49'34.6 (7)C37—C38—C33120.7 (6)
C48—Pd2—C4938.8 (4)C37—C38—H38119.6
C49'—Pd2—C4920.1 (6)C33—C38—H38119.6
C48—Pd2—C5066.8 (3)C40—C39—C44117.7 (5)
C49'—Pd2—C5032.3 (7)C40—C39—P2119.0 (4)
C49—Pd2—C5036.0 (3)C44—C39—P2123.4 (4)
C48—Pd2—P296.09 (19)C39—C40—C41121.6 (6)
C49'—Pd2—P2130.5 (8)C39—C40—H40119.2
C49—Pd2—P2129.5 (3)C41—C40—H40119.2
C50—Pd2—P2162.7 (2)C42—C41—C40119.8 (6)
C48—Pd2—Cl2160.51 (19)C42—C41—H41120.1
C49'—Pd2—Cl2126.2 (8)C40—C41—H41120.1
C49—Pd2—Cl2122.7 (3)C43—C42—C41120.0 (6)
C50—Pd2—Cl293.9 (2)C43—C42—H42120.0
P2—Pd2—Cl2103.31 (5)C41—C42—H42120.0
C9—P2—C33108.3 (2)C42—C43—C44120.1 (6)
C9—P2—C3999.4 (2)C42—C43—H43120.0
C33—P2—C39105.3 (2)C44—C43—H43120.0
C9—P2—Pd2112.77 (16)C39—C44—C43120.9 (6)
C33—P2—Pd2116.33 (18)C39—C44—H44119.6
C39—P2—Pd2113.17 (17)C43—C44—H44119.6
C1—C2—C3108.2 (6)C4—C52—C54109.3 (5)
C1—C2—Co169.6 (3)C4—C52—C55112.6 (5)
C3—C2—Co171.7 (3)C54—C52—C55111.2 (6)
C1—C2—H2125.9C4—C52—H52107.9
C3—C2—H2125.9C54—C52—H52107.9
Co1—C2—H2124.5C55—C52—H52107.9
C4—C3—C2108.3 (6)C16—C53—C20120.8 (6)
C4—C3—Co173.2 (3)C16—C53—H53119.6
C2—C3—Co167.7 (3)C20—C53—H53119.6
C4—C3—H3125.8C52—C54—H54A109.5
C2—C3—H3125.8C52—C54—H54B109.5
Co1—C3—H3124.9H54A—C54—H54B109.5
C3—C4—C5107.2 (5)C52—C54—H54C109.5
C3—C4—C52127.5 (5)H54A—C54—H54C109.5
C5—C4—C52124.7 (5)H54B—C54—H54C109.5
C3—C4—Co167.8 (3)C52—C55—H55A109.5
C5—C4—Co167.4 (3)C52—C55—H55B109.5
C52—C4—Co1136.6 (4)H55A—C55—H55B109.5
C1—C5—C4107.8 (5)C52—C55—H55C109.5
C1—C5—Co167.7 (3)H55A—C55—H55C109.5
C4—C5—Co172.9 (3)H55B—C55—H55C109.5
C1—C5—H5126.1C49—C48—Pd273.0 (5)
C4—C5—H5126.1C49—C48—H48A119.8
Co1—C5—H5124.9Pd2—C48—H48A49.5
C7—C6—C990.4 (4)C49—C48—H48B119.8
C7—C6—C10135.9 (4)Pd2—C48—H48B167.0
C9—C6—C10131.5 (4)H48A—C48—H48B117.7
C7—C6—Co168.7 (3)C46—C47—Pd171.1 (5)
C9—C6—Co168.7 (3)C46—C47—H47A119.4
C10—C6—Co1132.3 (3)Pd1—C47—H47A53.1
C6—C7—C890.9 (4)C46—C47—H47B119.4
C6—C7—P1136.9 (4)Pd1—C47—H47B169.5
C8—C7—P1130.8 (4)H47A—C47—H47B117.0
C6—C7—Co168.1 (3)C50—C49—C48117.9 (9)
C8—C7—Co169.1 (3)C50—C49—Pd274.0 (5)
P1—C7—Co1130.6 (2)C48—C49—Pd268.1 (4)
C16—C8—C7133.0 (4)C50—C49—H49A110.6
C16—C8—C9136.7 (4)C48—C49—H49A110.6
C7—C8—C988.6 (4)Pd2—C49—H49A174.8
C16—C8—Co1132.3 (3)C47—C46—C45124.6 (10)
C7—C8—Co167.3 (3)C47—C46—Pd173.1 (5)
C9—C8—Co167.3 (3)C45—C46—Pd169.6 (5)
C6—C9—C890.2 (4)C47—C46—H46109.4
C6—C9—P2129.4 (4)C45—C46—H46109.4
C8—C9—P2138.9 (4)Pd1—C46—H46177.1
C6—C9—Co167.8 (3)Pd1—C46'—H46'169.9
C8—C9—Co168.9 (3)C46—C45—Pd174.0 (5)
P2—C9—Co1130.6 (3)C46—C45—H45A119.4
C15—C10—C11118.1 (5)Pd1—C45—H45A166.6
C15—C10—C6122.9 (5)C46—C45—H45B119.4
C11—C10—C6119.0 (5)Pd1—C45—H45B50.4
C12—C11—C10120.6 (6)H45A—C45—H45B117.1
C12—C11—H11119.7C49—C50—Pd270.0 (5)
C10—C11—H11119.7C49—C50—H50A119.8
C13—C12—C11120.5 (6)Pd2—C50—H50A170.2
C13—C12—H12119.7C49—C50—H50B119.8
C11—C12—H12119.7Pd2—C50—H50B53.5
C12—C13—C14119.6 (6)H50A—C50—H50B117.6
C12—C13—H13120.2Cl4—C56—Cl3125.4 (11)
C14—C13—H13120.2Cl3'—C56—Cl4'110.1 (11)
C13—C14—C15120.1 (6)Cl4—C56—H56A121.9
C13—C14—H14120.0Cl3'—C56—H56A109.6
C15—C14—H14120.0Cl4'—C56—H56A109.6
C10—C15—C14121.1 (6)Cl4—C56—H56B119.6
C10—C15—H15119.5Cl3'—C56—H56B109.6
C14—C15—H15119.5Cl3—C56—H56B115.0
C53—C16—C17118.6 (5)Cl4'—C56—H56B109.6
C53—C16—C8120.8 (5)H56A—C56—H56B108.2
C17—C16—C8120.6 (5)
Table 1
Selected geometric parameters (Å) top
Pd1—C452.116 (6)Pd2—C482.110 (6)
Pd1—C462.171 (10)Pd2—C492.174 (9)
Pd1—C472.195 (6)Pd2—C502.223 (6)
Pd1—P12.3132 (15)Pd2—P22.3215 (15)
Pd1—Cl12.3901 (17)Pd2—Cl22.3897 (18)
Acknowledgements top

Financial support from the National Science Council of the Republic of China (NSC-95–2113-M-005–015-MY3) is gratefully appreciated.

references
References top

Bruker (1999). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.

Chang, Y.-C. & Hong, F.-E. (2005). Organometallics, 24, 5686–5695.

Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.

Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122.