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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