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Chondroudis K, Kanatzidis MG, Sayettat J, et al. Palladium Chemistry in Molten Alkali Metal Polychalcophosphate Fluxes. Synthesis and Characterization of K(4)Pd(PS(4))(2), Cs(4)Pd(PSe(4))(2), Cs(10)Pd(PSe(4))(4), KPdPS(4), K(2)PdP(2)S(6), and Cs(2)PdP(2)Se(6). Inorg Chem. 1997;36(25):5859-5868doi: 10.1021/ic970593n.
Chondroudis, K., Kanatzidis, M. G., Sayettat, J., Jobic, S., & Brec, R. (1997). Palladium Chemistry in Molten Alkali Metal Polychalcophosphate Fluxes. Synthesis and Characterization of K(4)Pd(PS(4))(2), Cs(4)Pd(PSe(4))(2), Cs(10)Pd(PSe(4))(4), KPdPS(4), K(2)PdP(2)S(6), and Cs(2)PdP(2)Se(6). Inorganic chemistry, 36(25), 5859-5868. https://doi.org/10.1021/ic970593n
Chondroudis, Konstantinos, et al. "Palladium Chemistry in Molten Alkali Metal Polychalcophosphate Fluxes. Synthesis and Characterization of K(4)Pd(PS(4))(2), Cs(4)Pd(PSe(4))(2), Cs(10)Pd(PSe(4))(4), KPdPS(4), K(2)PdP(2)S(6), and Cs(2)PdP(2)Se(6)." Inorganic chemistry vol. 36,25 (1997): 5859-5868. doi: https://doi.org/10.1021/ic970593n
Chondroudis K, Kanatzidis MG, Sayettat J, Jobic S, Brec R. Palladium Chemistry in Molten Alkali Metal Polychalcophosphate Fluxes. Synthesis and Characterization of K(4)Pd(PS(4))(2), Cs(4)Pd(PSe(4))(2), Cs(10)Pd(PSe(4))(4), KPdPS(4), K(2)PdP(2)S(6), and Cs(2)PdP(2)Se(6). Inorg Chem. 1997 Dec 03;36(25):5859-5868. doi: 10.1021/ic970593n. PMID: 11670209.
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Inorg Chem. 1997 Dec 03;36(25):5859-5868. doi: 10.1021/ic970593n.

Palladium Chemistry in Molten Alkali Metal Polychalcophosphate Fluxes. Synthesis and Characterization of K(4)Pd(PS(4))(2), Cs(4)Pd(PSe(4))(2), Cs(10)Pd(PSe(4))(4), KPdPS(4), K(2)PdP(2)S(6), and Cs(2)PdP(2)Se(6).

Inorganic chemistry

Konstantinos Chondroudis, Mercouri G. Kanatzidis, Julien Sayettat, Stéphane Jobic, Raymond Brec

Affiliations

  1. Institut des Matériaux de Nantes, B.P. 32229, 44322 Nantes Cedex 03, France.

PMID: 11670209 DOI: 10.1021/ic970593n

Abstract

The reaction of Pd with a molten mixture of A(2)Q(x)()/P(2)Q(5)/Q (A = K, Q = S, x = 3; A = Cs, Q = Se, x = 1) produced the molecular compounds K(4)Pd(PS(4))(2) (I), Cs(4)Pd(PSe(4))(2) (II), and Cs(10)Pd(PSe(4))(4) (III) and the solid-state KPdPS(4) (IV), K(2)PdP(2)S(6) (V), and Cs(2)PdP(2)Se(6) (VI). Compounds I-III are air and water sensitive, while IV-VI are air and water stable. All crystals are red or dark red except those of VI, which are black. All of them exhibit a rodlike shape. Compound I crystallizes in the triclinic space group P&onemacr; (No. 2) with a = 6.380(1) Å, b = 6.897(1) Å, c = 8.999(1) Å, alpha = 87.777(8) degrees, beta = 81.581(8) degrees, gamma = 84.429(9) degrees, and Z = 1. Compound II crystallizes in the monoclinic space group P2(1)/c (No. 14) with a = 7.491(2) Å, b = 13.340(2) Å, c = 10.030(3) Å, beta = 92.21(2) degrees, and Z = 2. Compound III crystallizes in the tetragonal space group P&fourmacr;2c (No. 112) with a = b = 13.949(2) Å, c = 11.527(2) Å, and Z = 4. Compound IV crystallizes in the tetragonal space group P4(2)/mnm (No. 136) with a = b = 8.5337(2) Å, c = 10.5595(5) Å, and Z = 4. Compound V crystallizes in the orthorombic space group Pnma (No. 62) with a = 15.612(2) Å, b = 7.0724(7) Å, c = 10.080(1) Å, and Z = 4. Compound VI crystallizes in the monoclinic space group C2/c (No. 15) with a = 12.9750(4) Å, b = 8.3282(2) Å, c = 13.0568(1) Å, beta = 102.940(2) degrees, and Z = 4. Compounds I-III contain the discrete complexes [Pd(PQ(4))(2)](4)(-) (Q = S, Se). The mixed salt III contains additional noncoordinating [PSe(4)](3)(-) units. The structure of IV consists of Pd(II) in square planar sulfur coordination linked by edge-sharing [PS(4)](3)(-) tetrahedral groups to produce one-dimensional chains. The structures of V andVI feature the [P(2)Q(6)](4)(-) (Q = S, Se) group coordinated to the square planar Pd(2+) atoms, yielding [PdP(2)Q(6)](n)()(2)(n)()(-) chains. Physical characterization was performed with DTA, far-IR spectroscopy, solid-state UV/vis diffuse reflectance spectroscopy, and single-crystal optical transmission.

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