Preparation and characterisation of a series of cationic monometallated, and neutral and cationic tridentate dimetallated, tri-o-tolyl phosphite iridium(III) complexes
- 1 January 1978
- journal article
- research article
- Published by Royal Society of Chemistry (RSC) in J. Chem. Soc., Dalton Trans.
- No. 8,p. 926-931
- https://doi.org/10.1039/dt9780000926
Abstract
Stoicheiometric additions of P(OC6H4Me-o)3 to [{IrCl(cod)}2](cod = cyclo-octa-1,5-diene) in various solvents have given the internally metallated complexes [Ir(P–C)(cod){P(OC6H4Me-o)3}][P–C = P(OC6H3Me-o)-(OC6H4Me-o)2], [IrCl(P–C)2{P(OC6H4Me-o)3}], and a complex analysing for [Ir2Cl2{P(OC6H4Me-o)3}3]. Chemical attempts to fully characterise the last product afforded the dimers [lr2Cl2(P–C2)2L(L′)][P–C2= P(OC6H3Me-o)2(OC6H4Me-o); L = P(OC6H4Me-o)3, L′= MeCN; L = L′= MeCN, EtOH, PrnOH, CO, or SbPh3]. Bridge fission of [Ir2Cl2(P–C2)2(CO)2] with 4-methylpyridine gives [IrCl(P–C2)(CO)(4Me-py)]. The complex [Ir2Cl2{P(OC6H4Me-o)3)3] is an excellent precursor for the preparation of: (i)[IrCl(P–C2) L2][L = 4Me-py, py, PMePh2, PMe2Ph, AsMe2Ph, P[(OCH2)3CMe], or PEt3; L2= 2,2′-bipyridyl] from ethanol {addition of Na[BPh4] to the mother liquors of these reactions gives the salts [IrCl(P–C)L3][BPh4]}; and (ii) the salts [Ir(P–C2(NCMe)3]A (A = PF6 or BPh4) from EtOH-MeCN mixtures. Further substitution of this salt produces [Ir(P–C2)(NCMe)L2]A (L2= Ph2PCH2CH2PPh2; L = PMePh2 or PMe2Ph). Relevant aspects of the X-ray crystallo-graphic determination of [IrCl(P–C2)(4Me-py)2] are briefly discussed together with i.r. and 1H n.m.r. data for all the complexes prepared.Keywords
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