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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
CCDC reference: 236030
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (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
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 = 306.07 | Dx = 1.745 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 25 reflections |
a = 8.627 (5) Å | θ = 15–16° |
b = 13.115 (4) Å | µ = 1.79 mm−1 |
c = 10.299 (2) Å | T = 293 K |
β = 90.38 (2)° | Prism, yellow |
V = 1165.2 (8) Å3 | 0.3 × 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 tube | Rint = 0.051 |
Graphite monochromator | θmax = 28.0°, θmin = 2.5° |
non–profiled ω/2θ scans | h = −11→11 |
Absorption correction: ψ scan (North et al., 1968) | k = 0→17 |
Tmin = 0.536, Tmax = 0.584 | l = 0→13 |
2962 measured reflections | 1 standard reflections every 238 reflections |
2815 independent reflections | intensity decay: 3% |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.041 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.105 | H 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 parameters | Δρmax = 0.99 e Å−3 |
0 restraints | Δρmin = −0.64 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
Pd1 | 0.21099 (3) | 0.52619 (3) | 0.47197 (3) | 0.03913 (14) | |
Cl1 | 0.21991 (14) | 0.50436 (9) | 0.70117 (11) | 0.0499 (3) | |
N1 | 0.1074 (4) | 0.6732 (3) | 0.4809 (3) | 0.0412 (8) | |
C2 | 0.1210 (6) | 0.7335 (4) | 0.5841 (5) | 0.0531 (12) | |
H2 | 0.1796 | 0.7108 | 0.6544 | 0.064* | |
C3 | 0.0522 (7) | 0.8281 (4) | 0.5916 (6) | 0.0649 (14) | |
H3 | 0.0673 | 0.8691 | 0.6643 | 0.078* | |
C4 | −0.0387 (6) | 0.8609 (4) | 0.4902 (5) | 0.0604 (13) | |
H4 | −0.0913 | 0.9227 | 0.4947 | 0.072* | |
C5 | −0.0502 (6) | 0.8006 (4) | 0.3825 (5) | 0.0531 (12) | |
H5 | −0.1074 | 0.8223 | 0.3107 | 0.064* | |
C6 | 0.0227 (5) | 0.7085 (4) | 0.3810 (4) | 0.0467 (10) | |
H6 | 0.0132 | 0.6682 | 0.3071 | 0.056* | |
C7 | 0.2214 (7) | 0.5105 (4) | 0.2670 (5) | 0.0578 (13) | |
H7A | 0.1180 | 0.5010 | 0.2891 | 0.069* | |
H7B | 0.2480 | 0.5596 | 0.2059 | 0.069* | |
C8 | 0.3360 (6) | 0.4514 (4) | 0.3253 (5) | 0.0559 (12) | |
H8 | 0.4396 | 0.4604 | 0.3037 | 0.067* | |
C9 | 0.2937 (5) | 0.3794 (4) | 0.4153 (5) | 0.0500 (11) | |
H9 | 0.1886 | 0.3658 | 0.4249 | 0.060* | |
C10 | 0.4058 (6) | 0.3213 (4) | 0.4991 (5) | 0.0553 (12) | |
H10A | 0.491 | 0.3576 | 0.5113 | 0.066* | |
H10B | 0.3639 | 0.3090 | 0.576 | 0.066* | |
O11 | 0.4414 (5) | 0.2296 (3) | 0.4375 (4) | 0.0688 (10) | |
C12 | 0.5168 (7) | 0.1589 (4) | 0.5201 (6) | 0.0790 (18) | |
H12A | 0.5999 | 0.1924 | 0.5656 | 0.119* | |
H12B | 0.5579 | 0.1040 | 0.4692 | 0.119* | |
H12C | 0.4440 | 0.1324 | 0.5815 | 0.119* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Pd1 | 0.03213 (18) | 0.0440 (2) | 0.0413 (2) | −0.00210 (14) | 0.00199 (12) | −0.00404 (14) |
Cl1 | 0.0516 (6) | 0.0553 (6) | 0.0428 (6) | −0.0009 (5) | −0.0025 (5) | −0.0004 (5) |
N1 | 0.0345 (17) | 0.0439 (19) | 0.0451 (19) | −0.0019 (15) | 0.0002 (15) | −0.0016 (16) |
C2 | 0.051 (3) | 0.055 (3) | 0.053 (3) | 0.004 (2) | −0.015 (2) | −0.007 (2) |
C3 | 0.070 (3) | 0.054 (3) | 0.071 (4) | 0.004 (3) | −0.011 (3) | −0.020 (3) |
C4 | 0.057 (3) | 0.046 (3) | 0.078 (4) | 0.005 (2) | −0.001 (3) | 0.003 (3) |
C5 | 0.050 (3) | 0.052 (3) | 0.058 (3) | −0.007 (2) | −0.007 (2) | 0.010 (2) |
C6 | 0.046 (2) | 0.050 (3) | 0.044 (2) | −0.003 (2) | −0.0045 (19) | 0.002 (2) |
C7 | 0.065 (3) | 0.068 (3) | 0.041 (3) | 0.005 (3) | 0.016 (2) | −0.003 (2) |
C8 | 0.052 (3) | 0.063 (3) | 0.053 (3) | 0.003 (2) | 0.016 (2) | −0.013 (2) |
C9 | 0.040 (2) | 0.049 (3) | 0.061 (3) | −0.0004 (19) | 0.009 (2) | −0.011 (2) |
C10 | 0.047 (3) | 0.055 (3) | 0.064 (3) | 0.000 (2) | 0.003 (2) | −0.006 (2) |
O11 | 0.097 (3) | 0.051 (2) | 0.058 (2) | 0.021 (2) | 0.006 (2) | 0.0005 (18) |
C12 | 0.086 (4) | 0.059 (3) | 0.093 (5) | 0.017 (3) | 0.016 (4) | 0.017 (3) |
Geometric parameters (Å, º) top
Pd1—C8 | 2.105 (5) | C6—H6 | 0.9300 |
Pd1—C7 | 2.124 (5) | C7—C8 | 1.390 (7) |
Pd1—N1 | 2.128 (4) | C7—H7A | 0.9300 |
Pd1—C9 | 2.136 (5) | C7—H7B | 0.9300 |
Pd1—Cl1 | 2.3787 (13) | C8—C9 | 1.374 (7) |
N1—C2 | 1.329 (5) | C8—H8 | 0.9300 |
N1—C6 | 1.341 (5) | C9—C10 | 1.499 (7) |
C2—C3 | 1.377 (7) | C9—H9 | 0.9300 |
C2—H2 | 0.9300 | C10—O11 | 1.395 (6) |
C3—C4 | 1.371 (7) | C10—H10A | 0.8866 |
C3—H3 | 0.9300 | C10—H10B | 0.8866 |
C4—C5 | 1.366 (7) | O11—C12 | 1.413 (6) |
C4—H4 | 0.9300 | C12—H12A | 0.9600 |
C5—C6 | 1.362 (7) | C12—H12B | 0.9600 |
C5—H5 | 0.9300 | C12—H12C | 0.9600 |
| | | |
C8—Pd1—C7 | 38.4 (2) | Pd1—C7—H7A | 73.9 |
C8—Pd1—N1 | 132.14 (18) | C8—C7—H7B | 120.0 |
C7—Pd1—N1 | 98.69 (17) | Pd1—C7—H7B | 128.2 |
C8—Pd1—C9 | 37.81 (19) | H7A—C7—H7B | 120.0 |
C7—Pd1—C9 | 68.0 (2) | C9—C8—C7 | 118.9 (5) |
N1—Pd1—C9 | 165.92 (16) | C9—C8—Pd1 | 72.3 (3) |
C8—Pd1—Cl1 | 130.00 (15) | C7—C8—Pd1 | 71.5 (3) |
C7—Pd1—Cl1 | 166.82 (15) | C9—C8—H8 | 120.5 |
N1—Pd1—Cl1 | 94.42 (10) | C7—C8—H8 | 120.5 |
C9—Pd1—Cl1 | 98.85 (14) | Pd1—C8—H8 | 127.6 |
C2—N1—C6 | 116.9 (4) | C8—C9—C10 | 124.4 (4) |
C2—N1—Pd1 | 122.6 (3) | C8—C9—Pd1 | 69.9 (3) |
C6—N1—Pd1 | 120.5 (3) | C10—C9—Pd1 | 121.1 (3) |
N1—C2—C3 | 123.0 (5) | C8—C9—H9 | 117.8 |
N1—C2—H2 | 118.5 | C10—C9—H9 | 117.8 |
C3—C2—H2 | 118.5 | Pd1—C9—H9 | 79.4 |
C4—C3—C2 | 118.9 (5) | O11—C10—C9 | 108.6 (4) |
C4—C3—H3 | 120.5 | O11—C10—H10A | 110.0 |
C2—C3—H3 | 120.5 | C9—C10—H10A | 110.0 |
C5—C4—C3 | 118.4 (5) | O11—C10—H10B | 110.0 |
C5—C4—H4 | 120.8 | C9—C10—H10B | 110.0 |
C3—C4—H4 | 120.8 | H10A—C10—H10B | 108.3 |
C6—C5—C4 | 119.5 (5) | C10—O11—C12 | 113.2 (4) |
C6—C5—H5 | 120.3 | O11—C12—H12A | 109.5 |
C4—C5—H5 | 120.3 | O11—C12—H12B | 109.5 |
N1—C6—C5 | 123.1 (4) | H12A—C12—H12B | 109.5 |
N1—C6—H6 | 118.4 | O11—C12—H12C | 109.5 |
C5—C6—H6 | 118.4 | H12A—C12—H12C | 109.5 |
C8—C7—Pd1 | 70.1 (3) | H12B—C12—H12C | 109.5 |
C8—C7—H7A | 120.0 | | |
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