Synthesis and Molecular Structure of trans‐[IrCl(coe)(^tBu₂PH)₂] (coe = cis‐cyclooctene)

Abstract

The reaction of [{Ir(µ-Cl)(coe) 2 } 2 ] (1) (coe ϭ cis-cyclooctene) with the secondary phosphane t Bu 2 PH afforded, under defined conditions, the novel complex trans-[IrCl(coe)( t Bu 2 PH) 2 ] (2), which has been characterized by spectroscopic methods as well as by X-ray diffraction. Compound 2 represents the first isolated and structurally characterized type of complex trans-[IrCl(coe)L 2 ] (L ϭ * Priv.-Doz. 913 phosphane). The compound is presumably isolable because of the convenient electronic effects of the chosen phosphane ligands. rent interest in similar reactions using some tertiary phosphanes [4,5].

Towards Rhodium and Iridium Complexes Containing the Secondary Phosphane Ligand tBu2PH

“…Numerous thermolysis studies of 6b using various solvents resulted only in the detection of the starting material in each case, and no hints for the formation of the hypothetical species [{Ir(µ-Cl)( t Bu 2 PH) 2 } 2 ] using similar reaction conditions as reported for the preparation of [{Ir(µ-Cl)( t Bu 2 PCH 2 P t Bu 2 )} 2 ] [14] have been observed. For example, repeated attempts to react [{Ir(µ-Cl)(coe) 2 } 2 ] with t Bu 2 PH (molar ratio 1:4) in refluxing heptane resulted, surprisingly, in the formation of [IrCl( t Bu 2 PH) 3 ] as the main product indicated by agreement of the observed with the previously reported 31 P{ 1 H} NMR data [5]. This observation is consistent with the finding that [IrCl( t Bu 2 PH) 3 ] is also the main product using this molar ratio under room temperature conditions [5].…”

Synthesis and Molecular Structure of trans‐[RhCl(NO)(PtBu2H)2]BF4

“…However, another possible useful precursor for the synthesis of the Ir(NO) species may be the compound trans-[IrCl(coe)(PtBu 2 H) 2 ]. [9] Experimental Section General: All preparative work was carried out in a dry nitrogen atmosphere using standard Schlenk techniques. Chemicals were purchased from Sigma/Aldrich and used as received.…”

Nachrichten des Verbandes Biologie, Biowissenschaften & Biomedizin in Deutschland

“…For the near future a more detailed DNMR study including compound trans ‐[IrCl(NO)(P t Bu 2 H) 2 ]BF 4 , which could still not be prepared to date because of the inaccessibility of the starting complex [{Ir(μ‐Cl)(P t Bu 2 H) 2 } 2 ] is planned. However, another possible useful precursor for the synthesis of the Ir(NO) species may be the compound trans ‐[IrCl(coe)(P t Bu 2 H) 2 ] 9…”