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The title compound, di-μ-chloro-bis{[(2,3,4-η)-ethyl 6,6-di­methyl-5-oxohept-2-enoato]­palladium(II)}, [Pd2Cl2(C11­H17­O3)2], is a binuclear chloro-bridged palladium allyl complex that was obtained serendipitously From the reaction of 6,6-di­methyl-2-hepten-4-ynoate with Na2PdCl4 in water-containing alcohol. The allyl group is substituted with an ester and a tert-butyl­carboxy group. The dimeric mol­ecules link via C—H...O contacts into a two-dimensional network parallel to the bc plane.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100008799/gg1012sup1.cif
Contains datablocks global, II

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100008799/gg1012IIsup2.hkl
Contains datablock 1

CCDC reference: 150755

Computing details top

Data collection: Locally modified CAD-4 Software (Enraf-Nonius, 1989); cell refinement: SET4 (de Boer & Duisenberg, 1984); data reduction: HELENA (Spek, 1997); program(s) used to solve structure: DIRDIF99 (Beurskens et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 2000); software used to prepare material for publication: PLATON.

Bis(µ2-chloro)-bis-[1,2,3,3-(4-oxo-6,6-dimethyl-1-ethoxycarbonyl)- hexenyl]-palladium (II) top
Crystal data top
[Pd2(C11H17O3)2Cl2]Z = 1
Mr = 678.23F(000) = 340
Triclinic, P1Least Squares Treatment of 25 SET4 setting angles.
Hall symbol: -P 1Dx = 1.734 Mg m3
a = 6.6157 (11) ÅMo Kα radiation, λ = 0.71073 Å
b = 9.654 (4) ÅCell parameters from 25 reflections
c = 10.748 (4) Åθ = 9.6–14.0°
α = 101.96 (3)°µ = 1.62 mm1
β = 90.13 (3)°T = 150 K
γ = 104.29 (3)°Plate, orange
V = 649.7 (4) Å30.50 × 0.42 × 0.13 mm
Data collection top
CAD4T
diffractometer
2903 reflections with I > 2σ(I)
Radiation source: Rotating AnodeRint = 0.034
Graphite monochromatorθmax = 27.5°, θmin = 1.9°
ω–scanh = 88
Absorption correction: analytical
(De Meulenaer & Tompa, 1965)
k = 1212
Tmin = 0.549, Tmax = 0.805l = 1313
6309 measured reflections3 standard reflections every 60 min
2994 independent reflections intensity decay: 3%
Refinement top
Refinement on F2161 parameters
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.018 w = 1/[σ2(Fo2) + (0.0134P)2 + 0.225P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.044(Δ/σ)max < 0.002
S = 1.12Δρmax = 0.45 e Å3
2994 reflectionsΔρmin = 0.68 e Å3
Special details top

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'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 on F2 for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating -R-factor-obs 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
Pd10.09560 (2)1.03703 (1)0.36047 (1)0.0190 (1)
Cl10.09406 (8)0.85197 (4)0.47707 (4)0.0299 (1)
O10.2290 (2)1.17828 (14)0.18198 (15)0.0346 (4)
O20.0129 (2)1.38560 (13)0.29216 (14)0.0339 (4)
O30.0620 (2)0.73743 (15)0.11137 (15)0.0377 (4)
C10.0609 (3)1.24567 (17)0.23201 (17)0.0254 (4)
C20.1227 (3)1.18370 (18)0.23709 (17)0.0241 (4)
C30.1127 (3)1.04112 (17)0.16695 (15)0.0219 (4)
C40.2662 (3)0.97428 (18)0.19883 (16)0.0227 (4)
C50.2334 (2)0.81170 (17)0.15246 (16)0.0232 (4)
C60.4227 (3)0.74894 (18)0.15565 (16)0.0245 (4)
C70.5484 (3)0.8076 (2)0.28382 (19)0.0377 (6)
C80.5590 (3)0.79659 (19)0.04958 (17)0.0274 (4)
C90.3500 (3)0.5822 (2)0.1306 (2)0.0392 (6)
C100.1768 (3)1.4613 (2)0.2914 (2)0.0437 (7)
C110.3061 (4)1.4465 (3)0.3992 (3)0.0587 (9)
H20.259 (4)1.248 (3)0.259 (2)0.046 (7)*
H30.012 (4)0.987 (2)0.120 (2)0.025 (5)*
H40.397 (4)1.032 (2)0.220 (2)0.030 (5)*
H7A0.600000.914200.297700.0570*
H7B0.667100.763600.283200.0570*
H7C0.458700.782600.352400.0570*
H8A0.603500.903700.066300.0410*
H8B0.478500.759600.032400.0410*
H8C0.682200.757000.046900.0410*
H9A0.471800.540900.121500.0590*
H9B0.260300.545800.052100.0590*
H9C0.271400.552900.202100.0590*
H10A0.264901.420300.211300.0530*
H10B0.113401.566300.294600.0530*
H11A0.372001.342800.394800.0880*
H11B0.414501.499400.396900.0880*
H11C0.219201.487500.478500.0880*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pd10.0222 (1)0.0175 (1)0.0186 (1)0.0070 (1)0.0014 (1)0.0046 (1)
Cl10.0489 (3)0.0253 (2)0.0240 (2)0.0218 (2)0.0111 (2)0.0092 (2)
O10.0302 (7)0.0286 (6)0.0463 (8)0.0097 (5)0.0093 (6)0.0083 (6)
O20.0301 (6)0.0204 (5)0.0518 (8)0.0066 (5)0.0010 (6)0.0086 (5)
O30.0219 (6)0.0327 (6)0.0526 (9)0.0076 (5)0.0032 (6)0.0051 (6)
C10.0279 (8)0.0209 (7)0.0302 (8)0.0060 (6)0.0013 (7)0.0118 (6)
C20.0215 (7)0.0238 (7)0.0296 (8)0.0049 (6)0.0026 (6)0.0127 (6)
C30.0218 (7)0.0269 (7)0.0193 (7)0.0060 (6)0.0059 (6)0.0101 (6)
C40.0180 (7)0.0256 (7)0.0241 (7)0.0052 (6)0.0047 (6)0.0049 (6)
C50.0193 (7)0.0261 (7)0.0239 (7)0.0068 (6)0.0045 (6)0.0037 (6)
C60.0204 (7)0.0260 (7)0.0288 (8)0.0083 (6)0.0041 (6)0.0070 (6)
C70.0342 (10)0.0532 (11)0.0311 (9)0.0222 (9)0.0023 (8)0.0077 (8)
C80.0199 (7)0.0319 (8)0.0308 (8)0.0080 (6)0.0046 (6)0.0056 (7)
C90.0338 (9)0.0273 (8)0.0604 (13)0.0119 (7)0.0110 (9)0.0128 (9)
C100.0414 (11)0.0263 (8)0.0662 (14)0.0155 (8)0.0035 (10)0.0077 (9)
C110.0480 (14)0.0668 (16)0.0653 (16)0.0260 (12)0.0008 (12)0.0092 (13)
Geometric parameters (Å, º) top
Pd1—Cl12.3836 (11)C2—H20.96 (3)
Pd1—C22.109 (2)C3—H30.94 (2)
Pd1—C32.0913 (18)C4—H40.91 (2)
Pd1—C42.138 (2)C7—H7A0.9801
Pd1—Cl1i2.3811 (11)C7—H7B0.9801
O1—C11.202 (2)C7—H7C0.9791
O2—C11.330 (2)C8—H8A0.9801
O2—C101.450 (2)C8—H8B0.9804
O3—C51.208 (2)C8—H8C0.9801
C1—C21.486 (3)C9—H9A0.9801
C2—C31.411 (2)C9—H9B0.9795
C3—C41.407 (3)C9—H9C0.9799
C4—C51.505 (2)C10—H10A0.9900
C5—C61.523 (3)C10—H10B0.9901
C6—C71.533 (3)C11—H11A0.9795
C6—C81.530 (3)C11—H11B0.9806
C6—C91.527 (3)C11—H11C0.9794
C10—C111.452 (4)
Cl1—Pd1—C2171.29 (6)C3—C2—H2116.8 (16)
Cl1—Pd1—C3133.15 (6)Pd1—C3—H3111.9 (13)
Cl1—Pd1—C4102.46 (6)C2—C3—H3118.7 (14)
Cl1—Pd1—Cl1i88.91 (3)C4—C3—H3122.1 (13)
C2—Pd1—C339.26 (7)Pd1—C4—H4103.4 (14)
C2—Pd1—C468.83 (8)C3—C4—H4117.3 (14)
Cl1i—Pd1—C299.80 (6)C5—C4—H4119.8 (14)
C3—Pd1—C438.84 (8)C6—C7—H7A109.47
Cl1i—Pd1—C3131.63 (6)C6—C7—H7B109.46
Cl1i—Pd1—C4168.60 (6)C6—C7—H7C109.49
Pd1—Cl1—Pd1i91.09 (3)H7A—C7—H7B109.42
C1—O2—C10116.07 (15)H7A—C7—H7C109.48
O1—C1—O2125.06 (18)H7B—C7—H7C109.52
O1—C1—C2124.74 (16)C6—C8—H8A109.48
O2—C1—C2110.19 (16)C6—C8—H8B109.47
Pd1—C2—C1114.03 (13)C6—C8—H8C109.44
Pd1—C2—C369.68 (10)H8A—C8—H8B109.43
C1—C2—C3119.38 (17)H8A—C8—H8C109.50
Pd1—C3—C271.06 (10)H8B—C8—H8C109.51
Pd1—C3—C472.36 (10)C6—C9—H9A109.47
C2—C3—C4116.82 (16)C6—C9—H9B109.46
Pd1—C4—C368.80 (10)C6—C9—H9C109.49
Pd1—C4—C5114.79 (12)H9A—C9—H9B109.44
C3—C4—C5119.00 (16)H9A—C9—H9C109.47
O3—C5—C4119.46 (15)H9B—C9—H9C109.50
O3—C5—C6122.83 (16)O2—C10—H10A109.38
C4—C5—C6117.67 (14)O2—C10—H10B109.44
C5—C6—C7111.61 (15)C11—C10—H10A109.39
C5—C6—C8106.47 (15)C11—C10—H10B109.44
C5—C6—C9109.27 (16)H10A—C10—H10B108.07
C7—C6—C8109.39 (16)C10—C11—H11A109.49
C7—C6—C9109.77 (15)C10—C11—H11B109.40
C8—C6—C9110.27 (15)C10—C11—H11C109.45
O2—C10—C11111.07 (18)H11A—C11—H11B109.46
Pd1—C2—H2104.0 (15)H11A—C11—H11C109.55
C1—C2—H2119.7 (17)H11B—C11—H11C109.49
C3—Pd1—Cl1—Pd1i153.24 (8)C1—C2—C3—C4164.67 (16)
C4—Pd1—Cl1—Pd1i179.17 (5)C2—C3—C4—Pd157.15 (14)
Cl1i—Pd1—Cl1—Pd1i0.00 (3)C2—C3—C4—C5164.56 (16)
Cl1—Pd1—Cl1i—Pd1i0.02 (3)Pd1—C3—C4—C5107.41 (15)
C2—Pd1—Cl1i—Pd1i179.93 (6)Pd1—C4—C5—O363.9 (2)
C3—Pd1—Cl1i—Pd1i153.93 (7)C3—C4—C5—O314.6 (3)
C10—O2—C1—O12.5 (3)C3—C4—C5—C6163.37 (16)
C1—O2—C10—C1189.0 (2)Pd1—C4—C5—C6118.13 (15)
C10—O2—C1—C2178.28 (15)O3—C5—C6—C913.3 (2)
O2—C1—C2—Pd1107.66 (15)C4—C5—C6—C747.2 (2)
O1—C1—C2—C37.8 (3)C4—C5—C6—C9168.83 (15)
O1—C1—C2—Pd171.5 (2)O3—C5—C6—C8105.8 (2)
O2—C1—C2—C3173.02 (16)C4—C5—C6—C872.09 (18)
Pd1—C2—C3—C457.82 (14)O3—C5—C6—C7134.89 (18)
C1—C2—C3—Pd1106.85 (16)
Symmetry code: (i) x, y+2, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C8—H8B···O1ii0.982.5583.392 (3)142.9
C9—H9C···O2iii0.982.4983.394 (3)151.9
Symmetry codes: (ii) x, y+2, z; (iii) x, y1, z.
 

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