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Titolo:
SELENOETHER MACROCYCLIC CHEMISTRY - SYNTHESES, NMR-STUDIES, REDOX PROPERTIES, AND SINGLE-CRYSTAL STRUCTURES OF [M([16]ANESE(4))](PF6)(2)CENTER-DOT-2MECN (M=PD, PT, [16]ANESE(4)=1,5,9,13-TETRASELENACYCLOHEXADECANE)
Autore:
CHAMPNESS NR; KELLY PF; LEVASON W; REID G; SLAWIN AMZ; WILLIAMS DJ;
Indirizzi:
UNIV SOUTHAMPTON,DEPT CHEM SOUTHAMPTON SO9 5NH HANTS ENGLAND UNIV SOUTHAMPTON,DEPT CHEM SOUTHAMPTON SO9 5NH HANTS ENGLAND UNIV LONDON IMPERIAL COLL SCI TECHNOL & MED LONDON SW7 2AY ENGLAND
Titolo Testata:
Inorganic chemistry
fascicolo: 3, volume: 34, anno: 1995,
pagine: 651 - 657
SICI:
0020-1669(1995)34:3<651:SMC-SN>2.0.ZU;2-X
Fonte:
ISI
Lingua:
ENG
Soggetto:
NUCLEAR MAGNETIC-RESONANCE; CROWN THIOETHER CHEMISTRY; METAL-COMPLEXES; SE-77; 1,5,9,13-TETRASELENACYCLOHEXADECANE; PLATINUM; DICATION; LIGANDS; SULFUR;
Tipo documento:
Article
Natura:
Periodico
Settore Disciplinare:
Science Citation Index Expanded
Citazioni:
28
Recensione:
Indirizzi per estratti:
Citazione:
N.R. Champness et al., "SELENOETHER MACROCYCLIC CHEMISTRY - SYNTHESES, NMR-STUDIES, REDOX PROPERTIES, AND SINGLE-CRYSTAL STRUCTURES OF [M([16]ANESE(4))](PF6)(2)CENTER-DOT-2MECN (M=PD, PT, [16]ANESE(4)=1,5,9,13-TETRASELENACYCLOHEXADECANE)", Inorganic chemistry, 34(3), 1995, pp. 651-657

Abstract

Reaction of MCl(2) (M = Pd, Pt) with 1 molar equiv of [16]aneSe(4) inrefluxing MeCN solution in the presence of TLPF(6) affords the complexes [M([16]aneSe(4))](PF6)(2) in high yield. [Pd([16]aneSe(4))](PF6)(2).2MeCN crystallizes in the monoclinic space group P2(1)/c with a = 10.184(4) Angstrom, b = 10.673(4) Angstrom, c = 13.960(7) Angstrom, beta= 98.01(4)degrees, V = 1502.6 Angstrom(3), Z = 2, and F(000) = 917. The structure shows the Pd-II ion on a center of symmetry at (0, 0, 0),coordinated to a precisely square planar arrangement of the four selenoether donor atoms, with the macrocycle adopting an up,up,down,down configuration, Pd-Se = 2.435(2), 2.428(1) Angstrom. [Pt([16]aneSe(4))](PF6)(2).2MeCN is isomorphous with its Pd-II analogue, giving a = 10.200(7) Angstrom, b = 10.609(6) Angstrom, c = 14.045(8) Angstrom, beta = 98.90(2)degrees, V = 1501.6 Angstrom(3), Z = 2, F(000) = 984, and Pt-Se = 2.420(3), 2.417(3) Angstrom. Variable-temperature Se-77 and Pt-195NMR studies are described which reveal the occurrence of a dynamic process in solution for [M([16]aneSe(4))](2+), involving interconversionof invertomers. The bis-bidentate model complexes [M(MeSeCH(2)CH(2)CH(2)SeMe)2]- (PF6)(2) have also been prepared by reaction MCl(2) with 2molar equiv of MeSeCH(2)CH(2)CH(2)SeMe in refluxing MeCN in the presence of TlPF6. Variable-temperature Se-77 and Pt-195 NMR spectroscopic studies on these complexes are compared with those of the macrocyclic tetraselenoether complexes. Cyclic voltammetry of [M([16]aneSe(4))](PF6)(2) in MeCN solution shows no oxidative activity. An irreversible reduction is seen for each complex at E(pc) = -0.90 V for M = Pd and E(pc) = -1.64 V vs Fc/Fc(+) for M = Pt, at a scan rate of 200 mV s(-1).

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Documento generato il 24/11/20 alle ore 13:36:17