RT info:eu-repo/semantics/article
T1 Reactions of monocyclopentadienylniobium(III) complexes with α-diketones. Crystal-structure of the phosphonium salt [P{C(OH)MeC(O)Me}Me2Ph]Cl
A1 Jalón Sotés, Félix Ángel
A1 Gómez Sal, Pilar
A1 Otero Montero, Antonio
A1 Royo Gracia, Pascual
A1 García Blanco, S.
A1 Martínez Carrera, Sagrario
K1 Niobium
K1 Crystal structure
K1 Ciencia
K1 Química inorgánica
K1 Science
K1 Chemistry, inorganic
AB The reactions of Nb(η5-C5H5)Cl2(CO)L2 (= PMe3, PMe2Ph) with α-diketones RCOCOR (R = Me, Ph) and 3,5-di-t-butyl-o-quinone have been studied. When L = PMe2Ph and R = Ph the reaction in a molar ratio 1/1 gives Nb(η5-C5H5)Cl2(O2C2Ph2)(PMe2Ph)2 (I) whereas the same reaction for R = Me gives the phosphonium salt [P{C(OH)MeC(O)Me}Me2Ph]Cl (VII). When L = PMe3 only the phosphonium salts [P{C(OH)RC(O)R}Me3]Cl are obtained for R = Me (V) and Ph (VI), but the complex Nb(η5-C5H5)Cl2(O2C2Ph2)PMe3 (II) can be isolated by previous addition of MeI. Similar reactions with 3,5-di-t-butyl-o-quinone give Nb(η5-C5H5)Cl2(o-O2C6H2But)L, L = PMe3 (III), PMe2Ph (IV). All the compounds have been characterized by IR, 1H, 13C, 31P NMR spectroscopy and the crystal structure of VII has been determined by X-ray diffraction. VII crystallizes in the monoclinic space group P21/c with a 7.440(2), b 10.377(3), c 17.644(4) Å, β 96.94(2)° and Dcal 1.039 g cm−3 for Z = 4. A final R value of 0.046 (Rw = 0.049) based on 2309 observed reflections was obtained. The geometry around the P atom is tetrahedral.
PB Elsevier
SN 0022-328X
YR 1987
FD 1987
LK http://hdl.handle.net/10017/4660
UL http://hdl.handle.net/10017/4660
LA eng
DS MINDS@UW
RD 20-abr-2024