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• W2116714853 abstract "Abstract The tripod nickel(0) species [ tripod 4 Ni 3 ] ( 1 ) { tripod = CH 3 C(CH 2 PPPh 2 ) 3 } is shown to undergo oxidative addition with disulfides or diselenides REER (E = S, Se, R = t Bu, Ph) to produce [ tripod Ni(ER)] ( 2 ). Compounds 2 show pseudo tetrahedral coordination. They are paramagnetic with one unpaired electron per molecule. Their magnetic behaviour is almost that of an ideal Curie‐type magnet down to temperatures of 2 K. They undergo reversible one electron oxidation to the 16 valence electron species [ tripod Ni(ER)] + . The isoelectronic pseudo tetrahedral 16 valence electron cobalt species [ tripod Co(ER)] ( 3 ) are obtained by reduction of CoCl 2 with KC 8 in the presence of tripod and subsequent reaction with REER (E = S, Se; R = t Bu, Ph). They are paramagnetic with two unpaired electrons per molecule. They can be reversibly oxidised to the 15 valence electron compounds [ tripod Co(ER)] + while their reduction to the 17 valence electron species [ tripod Co(ER)] – , which would be isoelectronic to the stable compounds 2 , is not observed. Under appropriate conditions the reactions with REER do not result in the formation of 3 but yield [ tripod CoECo tripod ] ( 4 ) by extrusion of sulfur and selenium from the substrate. Compounds 4 show a linear Co–E–Co framework with very short Co–E bonds (E = S: 205 pm; E = Se: 216 pm). They are members of a family of dimetallaheterocumulenic compounds [L n MEML n ] (E = main group element of groups III to VI) with a valence electron count of 36 electrons. Quantum chemistry predicts that the HOMO of such compounds should be a degenerated pair of mainly metal centred orbitals. Electrochemistry of 4a , [ tripod CoSCo tripod ], shows three quasi‐reversible oxidation steps in the range of –700 mV vs. SCE to 570 mV vs. SCE, which can be understood as metal centred oxidations. Three different types of crystals have been obtained for different types of pseudopolymorphs 4a . The geometric parameters of the coordination compounds are almost equal in these pseudopolymorphic crystals. The real difference is the content of solvent molecules and, hence, the packing of the molecules. In the crystals of 4a containing no solvent the coordination compounds form close packed layers stacked on each other in an oblique way. In the crystals containing 4a· DME a layer of solvent molecules separates each pair of layers of close packed molecules. In the crystal of 4a· 3DME a cuboctahedral cage of solvent molecules embedding each coordination compound separates the complex molecules from each other. The different types of crystals observed underpin the globular shape of 4 and the effective shielding power of the tripod ligand. (© Wiley‐VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2008)" @default.
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• W2116714853 date "2008-03-01" @default.
• W2116714853 modified "2023-09-23" @default.
• W2116714853 title "Reductive Activation of <i>tripod</i> Metal Compounds: Preparative Application" @default.
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• W2116714853 doi "https://doi.org/10.1002/ejic.200700874" @default.
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