Synthesis and structure of chloro(methoxalyl)bis(triphenylphosphine)palladium

Fayos, J.; Dobrzynski, Edward D.; Angelici, Robert J.; Clardy, Jon

doi:10.1016/s0022-328x(00)95011-3

Cited by 20 publications

(5 citation statements)

References 4 publications

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“…This may result from packing effects: the phenyl groups on atom P(2) are tilted more toward the P(2) and S(2) atoms than are those attached to atom P(l) toward the P(l) and S(l) atoms. In any event, the Pd-P distances are typical of those found in a variety of Pd complexes.11™19 Moreover, the Pd-S distances are close to those found in Pd(CS2)-(PPh3)220 (2.305 (11) A), in Pd2(S2CSCMe3)2(SCMe3)2 (2.313 (3) and 2.330 (3) A), a dimer,21 and in the trimers21, 22 Pd-(S2CPh)2 (2.320 (3)-2.343 (3) A) and Pd3(S2CSEt)3(SEt)3 (2.331 (4)-2.349 (5) A).…”

Section: Discussionsupporting

confidence: 62%

Structure of bis(triphenylphosphine)(N-ethoxycarbonyldithiocarbimato) palladium(II), formed by the reaction of excess ethoxycarbonyl isothiocyanate with palladium(0) in the presence of triphenylphosphine

Ahmed¹,

Itoh²,

Matsuda³

et al. 1977

Inorg. Chem.

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When a large excess of EtOCONCS is added to Pd(0) complexes in the presence of PPh3 (Et = C2HS, Ph = C6H,), a compound of composition Pd(S2CNCOOEt)(PPh3), is isolated. On the basis of an x-ray diffraction study the compound is shown to be bis(triphenylphosphine)(N-ethoxycarbonyldithiocarbimato)palladium(II).The compound crystallizes in space group C,'-P1 of the triclinic system with two molecules in a unit cell of dimensions a = 13.371 (2) A, b = 13.741 (3) A, c = 10.995 (2) A, a = 93.85 (I)", = 113.74 (l)', y = 95.30 (l)", and V = 1829 A3. The structure has been solved by the heavy-atom method and refined by full-matrix least-squares techniques to a final value of the conventional R index on Fo of 0.042 based on 5794 unique reflections having F: 1 3u(FO2) collected by counter methods. The Pd atom is coordinated to two P atoms from the PPh3 groups and to two S atoms of the S,C=NCOOEt dithiocarbimato ligand in approximately a square-planar fashion. The Pd-P distances are 2.306 (1) and 2.333 (1) A, and the Pd-S distances are 2.316 (1) and 2.343 (1) A. The S-Pd-S angle is 75.03 (4)', while the P-Pd-P angle is 98.89 (4)". All five atoms in the inner coordination sphere are within 0.1 8, of the best least-squares plane defined by these atoms. The S-C bond lengths are 1.742 (4) and 1.754 (4) A and the C-N bond length is 1.282 (5) A. The comparable parameters within the inner coordination sphere agree very well with those found in the bis(N-cyanodithiocarbimato)nickelate(II) anion. In addition, these parameters differ but little from those of typical dithiocarbamate complexes.

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Section: Discussionsupporting

confidence: 62%

Structure of bis(triphenylphosphine)(N-ethoxycarbonyldithiocarbimato) palladium(II), formed by the reaction of excess ethoxycarbonyl isothiocyanate with palladium(0) in the presence of triphenylphosphine

Ahmed¹,

Itoh²,

Matsuda³

et al. 1977

Inorg. Chem.

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“…Both the ir and Raman spectra are consistent with the proposed structure; in heptane solution five bands were seen in the metal carbonyl region at 21 18, 2058, 2028, 2022, and 2010 cm-1 as well as three bands in the acyl stretching region at 1682, 1633, and 1620 cm-1.4a The Raman spectrum (powder) has strong bands at 598 and 399 cm-1 which supports our assignment of similar bands in the spectrum of 4a as Mn-C-O bending and Mn-C stretching, respectively. The uv-visible spectrum of 9 (heptane) had a long wavelength band at 438 nm (< 273), responsible for the orange-red color of its solutions, and additional maxima at 208 (e 38 300) and 253 nm (< 19 100).…”

Section: Resultsmentioning

confidence: 99%

“…Benzoylformylpentacarbonylmanganese(I) (9). NaMn(CO)s (12 ml, 1.1 , 13.2 mmol) in THF was added to a stirred solution of 2.95 g (17.5 mmol) of benzoylformyl chloride and 10 ml of THF at 0°.…”

Section: Methodsmentioning

confidence: 99%

Synthesis, crystal structure, and stability of pyruvoylpentacarbonylmanganese(I)

Casey¹,

Bunnell²,

Calabrese³

1976

J. Am. Chem. Soc.

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Sodium pentacarbonylmanganese reacts with pyruvoyl chloride to give pyruvoylpentacarbonylmanganese(I) (4a), which was characterized by spectral means and by x-ray crystallography. 4a reacts with 4-ethyl-2,6,7-trioxa-1 -phosphabicyclo[2.2.2]octane, EXPO, in a first-order reaction to give CH3COCOMn(CO)4(ETPO) (4b). 4a undergoes decarbonylation at 75°to give a mixture of acetylpentacarbonylmanganese(I) (2a) and methylpentacarbonylmanganese(I). Xhe rate of decarbonylation of 4a is 21 times slower than that of 2a at 75°. Less than 0.3% 4a is in equilibrium with 2a at 85°and 110 atm of CO. Ligand substitution of 2a via CH3COMn(CO)4 ( 1) is calculated to be over 77 500 faster than ligand substitution of 2a via CH3COCOMn(CO)4 (3).Table II. Raman Data (powder) CompoundAbsorptions (cm-1) 4a

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“…After vacuum removal of the CH3OH, the orange-brown residue was extracted with 40 ml of pentane. After treatment with activated charcoal and filtration, the pale yellow solution was concentrated under vacuum to about 15 ml. Cooling to -20°g ave white needles of the product (0.13 g, 32%), which was identified by its spectra (Table I).…”

Section: Methodsmentioning

confidence: 99%