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The structure of the novel title π-allyl palladium complex, [PdCl(C5H9O)(C5H5N)], has been determined. The allyl­ fragment is slightly skewed.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804001631/na6284sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804001631/na6284Isup2.hkl
Contains datablock I

CCDC reference: 236030

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.007 Å
  • R factor = 0.041
  • wR factor = 0.105
  • Data-to-parameter ratio = 21.7

checkCIF/PLATON results

No syntax errors found


No errors found in this datablock

Computing details top

Data collection: CAD-4 Software (Enraf–Nonius, 1994); cell refinement: CAD-4 Software; data reduction: PROFIT (Streltsov & Zavodnik, 1989); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 2003); software used to prepare material for publication: WinGX (Farrugia, 1999).

Chloro(1-methoxymethyl-π-allyl)(pyridine-κN)palladium top
Crystal data top
[PdCl(C5H9O)(C5H5N)]F(000) = 608
Mr = 306.07Dx = 1.745 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 25 reflections
a = 8.627 (5) Åθ = 15–16°
b = 13.115 (4) ŵ = 1.79 mm1
c = 10.299 (2) ÅT = 293 K
β = 90.38 (2)°Prism, yellow
V = 1165.2 (8) Å30.3 × 0.3 × 0.3 mm
Z = 4
Data collection top
Enraf–Nonius CAD-4
diffractometer
2177 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.051
Graphite monochromatorθmax = 28.0°, θmin = 2.5°
non–profiled ω/2θ scansh = 1111
Absorption correction: ψ scan
(North et al., 1968)
k = 017
Tmin = 0.536, Tmax = 0.584l = 013
2962 measured reflections1 standard reflections every 238 reflections
2815 independent reflections intensity decay: 3%
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)] = 0.041Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.105H atoms treated by a mixture of independent and constrained refinement
S = 1.06 w = 1/[σ2(Fo2) + (0.0551P)2 + 0.091P]
where P = (Fo2 + 2Fc2)/3
2815 reflections(Δ/σ)max = 0.001
130 parametersΔρmax = 0.99 e Å3
0 restraintsΔρmin = 0.64 e Å3
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
Pd10.21099 (3)0.52619 (3)0.47197 (3)0.03913 (14)
Cl10.21991 (14)0.50436 (9)0.70117 (11)0.0499 (3)
N10.1074 (4)0.6732 (3)0.4809 (3)0.0412 (8)
C20.1210 (6)0.7335 (4)0.5841 (5)0.0531 (12)
H20.17960.71080.65440.064*
C30.0522 (7)0.8281 (4)0.5916 (6)0.0649 (14)
H30.06730.86910.66430.078*
C40.0387 (6)0.8609 (4)0.4902 (5)0.0604 (13)
H40.09130.92270.49470.072*
C50.0502 (6)0.8006 (4)0.3825 (5)0.0531 (12)
H50.10740.82230.31070.064*
C60.0227 (5)0.7085 (4)0.3810 (4)0.0467 (10)
H60.01320.66820.30710.056*
C70.2214 (7)0.5105 (4)0.2670 (5)0.0578 (13)
H7A0.11800.50100.28910.069*
H7B0.24800.55960.20590.069*
C80.3360 (6)0.4514 (4)0.3253 (5)0.0559 (12)
H80.43960.46040.30370.067*
C90.2937 (5)0.3794 (4)0.4153 (5)0.0500 (11)
H90.18860.36580.42490.060*
C100.4058 (6)0.3213 (4)0.4991 (5)0.0553 (12)
H10A0.4910.35760.51130.066*
H10B0.36390.30900.5760.066*
O110.4414 (5)0.2296 (3)0.4375 (4)0.0688 (10)
C120.5168 (7)0.1589 (4)0.5201 (6)0.0790 (18)
H12A0.59990.19240.56560.119*
H12B0.55790.10400.46920.119*
H12C0.44400.13240.58150.119*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pd10.03213 (18)0.0440 (2)0.0413 (2)0.00210 (14)0.00199 (12)0.00404 (14)
Cl10.0516 (6)0.0553 (6)0.0428 (6)0.0009 (5)0.0025 (5)0.0004 (5)
N10.0345 (17)0.0439 (19)0.0451 (19)0.0019 (15)0.0002 (15)0.0016 (16)
C20.051 (3)0.055 (3)0.053 (3)0.004 (2)0.015 (2)0.007 (2)
C30.070 (3)0.054 (3)0.071 (4)0.004 (3)0.011 (3)0.020 (3)
C40.057 (3)0.046 (3)0.078 (4)0.005 (2)0.001 (3)0.003 (3)
C50.050 (3)0.052 (3)0.058 (3)0.007 (2)0.007 (2)0.010 (2)
C60.046 (2)0.050 (3)0.044 (2)0.003 (2)0.0045 (19)0.002 (2)
C70.065 (3)0.068 (3)0.041 (3)0.005 (3)0.016 (2)0.003 (2)
C80.052 (3)0.063 (3)0.053 (3)0.003 (2)0.016 (2)0.013 (2)
C90.040 (2)0.049 (3)0.061 (3)0.0004 (19)0.009 (2)0.011 (2)
C100.047 (3)0.055 (3)0.064 (3)0.000 (2)0.003 (2)0.006 (2)
O110.097 (3)0.051 (2)0.058 (2)0.021 (2)0.006 (2)0.0005 (18)
C120.086 (4)0.059 (3)0.093 (5)0.017 (3)0.016 (4)0.017 (3)
Geometric parameters (Å, º) top
Pd1—C82.105 (5)C6—H60.9300
Pd1—C72.124 (5)C7—C81.390 (7)
Pd1—N12.128 (4)C7—H7A0.9300
Pd1—C92.136 (5)C7—H7B0.9300
Pd1—Cl12.3787 (13)C8—C91.374 (7)
N1—C21.329 (5)C8—H80.9300
N1—C61.341 (5)C9—C101.499 (7)
C2—C31.377 (7)C9—H90.9300
C2—H20.9300C10—O111.395 (6)
C3—C41.371 (7)C10—H10A0.8866
C3—H30.9300C10—H10B0.8866
C4—C51.366 (7)O11—C121.413 (6)
C4—H40.9300C12—H12A0.9600
C5—C61.362 (7)C12—H12B0.9600
C5—H50.9300C12—H12C0.9600
C8—Pd1—C738.4 (2)Pd1—C7—H7A73.9
C8—Pd1—N1132.14 (18)C8—C7—H7B120.0
C7—Pd1—N198.69 (17)Pd1—C7—H7B128.2
C8—Pd1—C937.81 (19)H7A—C7—H7B120.0
C7—Pd1—C968.0 (2)C9—C8—C7118.9 (5)
N1—Pd1—C9165.92 (16)C9—C8—Pd172.3 (3)
C8—Pd1—Cl1130.00 (15)C7—C8—Pd171.5 (3)
C7—Pd1—Cl1166.82 (15)C9—C8—H8120.5
N1—Pd1—Cl194.42 (10)C7—C8—H8120.5
C9—Pd1—Cl198.85 (14)Pd1—C8—H8127.6
C2—N1—C6116.9 (4)C8—C9—C10124.4 (4)
C2—N1—Pd1122.6 (3)C8—C9—Pd169.9 (3)
C6—N1—Pd1120.5 (3)C10—C9—Pd1121.1 (3)
N1—C2—C3123.0 (5)C8—C9—H9117.8
N1—C2—H2118.5C10—C9—H9117.8
C3—C2—H2118.5Pd1—C9—H979.4
C4—C3—C2118.9 (5)O11—C10—C9108.6 (4)
C4—C3—H3120.5O11—C10—H10A110.0
C2—C3—H3120.5C9—C10—H10A110.0
C5—C4—C3118.4 (5)O11—C10—H10B110.0
C5—C4—H4120.8C9—C10—H10B110.0
C3—C4—H4120.8H10A—C10—H10B108.3
C6—C5—C4119.5 (5)C10—O11—C12113.2 (4)
C6—C5—H5120.3O11—C12—H12A109.5
C4—C5—H5120.3O11—C12—H12B109.5
N1—C6—C5123.1 (4)H12A—C12—H12B109.5
N1—C6—H6118.4O11—C12—H12C109.5
C5—C6—H6118.4H12A—C12—H12C109.5
C8—C7—Pd170.1 (3)H12B—C12—H12C109.5
C8—C7—H7A120.0
 

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