NDLI: Novel access to carbodiphosphoranes in the coordination sphere of group 10 metals: template synthesis and protonation of PCP pincer carbodiphosphorane complexes of $C(dppm)

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Novel access to carbodiphosphoranes in the coordination sphere of group 10 metals: template synthesis and protonation of PCP pincer carbodiphosphorane complexes of $C(dppm)_{2}$

Content Provider	World Health Organization (WHO)-Global Index Medicus
Author	Schuh, Walter Obendorf, Dagmar Wurst, Klaus Peringer, Paul Reitsamer, Christian Stallinger, Silvia Kopacka, Holger
Description	Author Affiliation: Reitsamer C ( Institut für Allgemeine, Anorganische und Theoretische Chemie der Universität Innsbruck, Innrain 52a, A-6020 Innsbruck, Austria.)
Abstract	In a novel template synthesis of carbodiphosphoranes (CDPs), the phosphine functionalized CDP ligand $C(dppm)_{2}$ (dppm = $Ph_{2}PCH_{2}PPh_{2})$ is formed in the coordination sphere of group 10 metals from $CS_{2}$ and 4 equivalents of dppm. The products are the PCP pincer complexes $[M(Cl)(C(dppm)_{2}-κ3P,C,P)]Cl$ (M = Ni, Pd, Pt) and 2 equivalents of dppmS. The compound $C(dppm)_{2},$ which is composed of a divalent carbon atom and two dppm subunits, represents a new PCP-type pincer ligand with the formally neutral carbon Lewis base of the CDP functionality as the central carbon. Treatment of $[M(Cl)(C(dppm)_{2}-κ3P,C,P)]Cl$ (M = Pd, Pt) with hydrochloric acid results in protonation at the CDP carbon atom and the formation of the PCP pincer complexes $[M(Cl)(CH(dppm)_{2}-κ3P,C,P)]Cl_{2}$ (M = Pd, Pt). The PCP pincer ligand $[CH(dppm)_{2}]^{+}$ involves a formally cationic central carbon donor. The reaction of $[Ni(Cl)(C(dppm)_{2}-κ3P,C,P)]Cl$ with HCl leads to the extrusion of $NiCl_{2}$ and formation of the diprotonated CDP compound $[CH_{2}(dppm)_{2}]Cl_{2},$ from which the monoprotonated conjugate base $[CH(dppm)_{2}]Cl$ is obtained upon addition of bases, such as NH $_{3}$ . The crystal structures of $[M(Cl)(C(dppm)_{2}-κ3P,C,P)]Cl$ (M = Ni, Pd, Pt), $[Ni(Cl)(C(dppm)_{2}-κ3P,C,P)]_{2}[NiCl_{4}],$ $[M(Cl)(CH(dppm)_{2}-κ3P,C,P)]Cl_{2}$ (M = Pd, Pt) as well as $[CH_{2}(dppm)_{2}]Cl_{2}$ and $[CH(dppm)_{2}]Cl$ are presented. A comparison of the solid state structures reveals interesting features, e.g. infinite supramolecular networks mediated by C–H⋯Cl hydrogen bond interactions and an unexpected loss of molecular symmetry upon protonation in the complexes $[M(CH(dppm)_{2}-κ3P,C,P)(Cl)]Cl_{2}$ (M = Pd, Pt) as a result of the flexible ligand backbone. Additionally the new compounds were characterized comprehensively in solution by multinuclear $^{31}P,$ $^{13}C$ and $^{1}H$ NMR spectroscopy : Several spectroscopic parameters show a striking variability in particular regarding the carbodiphosphorane functionality. Furthermore the compound $[Ni(Cl)(C(dppm)_{2}-κ3P,C,P)]Cl$ was examined by cyclic voltammetry ( CV ) and could be shown to display quasi-reversible oxidative as well as reductive behaviour.
ISSN	14779226
Issue Number	12
Journal	Dalton Trans.
Volume Number	41
e-ISSN	13645447
Language	English
Publisher	Royal Society of Chemistry
Publisher Date	2012-03-28
Publisher Place	Great Britain (UK)
Access Restriction	Subscribed
Subject Keyword	Chemistry
Content Type	Text
Resource Type	Article
Subject	Inorganic Chemistry

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