H. Miyamae

Cluster chemistry: LXXXI. Reactions of Ru3(μ-dppm)(CO)10 with C2(CO2Me)2. X-ray structures of Ru3{μ3-C4(CO2Me)4}(μ-dppm)(CO)6, Ru3(μ-H)2{μ3-C2(CO2Me)2}(μ-dppm)(CO)7 and Ru4(μ3-H){μ-C2(CO2Me)2}{μ-PPh2CH2PPh(C6H4)}(CO)9☆

Abstract Several complexes have been obtained from reactions between Ru 3 (μ-dppm)(CO) 10 and C 2 (CO 2 Me) 2 , including Ru 3 {μ 3 -C 2 (CO 2 Me) 2 }(μ-dppm)(μ-CO)(CO) 7 (7), Ru 3 {μ 3 -C 4 (CO 2 Me) 4 }(μ-dppm)(CO) 6 , ( 8 ), Ru 4 (μ 4 -C 2 )(CO 2 Me) 2 }(μ-dppm)(CO) 10 ( 11 ) and Ru 4 (μ 3 -H){μ 4 -C 2 (CO 2 Me) 2 }{μ-PPh 2 CH 2 PPh(C 6 H 4 )}(CO) 9 ( 10 ). A complex related to 10 , containing a C 4 (CO 2 Me) 4 ligand, was obtained directly from Ru 3 (μ 3 -PPhCH 2 PPh(C 6 H 4 )}(CO) 9 and the alkyne. Ready replacement of CO by 2H occurred in the reaction of 7 with H 2 , which afforded Ru 3 (μ-H) 2 {μ 3 -C 2 (CO 2 Me) 2 }(μ-dppm)(CO) 7 ( 9 ). Complexes 8 , 9 and 10 were characterised by single-crystal X-ray studies: in 8 , the C 4 (CO 2 Me) 4 ligand forms a ruthenacyclopentadiene system which interacts in the η 4 mode with the second Ru atom, and via an ester CO group with the third Ru atom. In 9 , the alkyne is attached to the Ru 3 cluster in the μ 3 -η 2 -|| mode, while in 10 , it is incorporated into an octahedral C 2 Ru 4 cluster; the metallated dppm ligand bridges an edge of one of the wings of the Ru 4 butterfly. Complexes 10 and 11 were obtained in only 1% and 2% yield, respectively.

Lewis-Base Adducts of Lead(II) Compounds. XXI. Revisitations: Synthesis and Structure of the Hydrated 1 : 2 Adduct of Lead(II) Bis(perchlorate) and 2,4,6-Tris(2-pyridyl)-1,3,5-triazine and a Low-Temperature Redetermination of the Structure of Bis(2-aminLewis-Base Adducts of Lead(II) Compounds

Lead(II) perchlorate crystallizes from aqueous ethanol with 2,4,6-tris(2-pyridyl)-1,3,5-triazine (trz) as a 1 : 2 trihydrate adduct, [(trz)2Pb(OH2)(O2ClO2)](ClO4)·2H2O, as has been confirmed by a low temperature (ca .153 K) single crystal X-ray structure determination. The lead(II) environment is derivative of that of the previously recorded hydrated (rather than the methanol solvated) nitrate complex, comprising a pair of tridentate trz ligands, and, in place of the pair of bidentate nitrates, a unidentate water and an unsymmetrically bidentate perchlorate ion. A redetermination of the structure of bis(2-aminomethylpyridine)lead(II) bis(perchlorate) has resulted in a non-disordered model, still based upon the [Pb(amp)2(OClO3)2] entity, where amp = 2-aminomethylpyridine, but with eight independent molecules, devoid of any crystallographic symmetry, comprising the asymmetric unit of the structure, which is described in a larger unit cell of lower symmetry.