TY - JOUR
T1 - Synthesis and characterization of a stable bis-naphthyltin(II) compound. Bis[8-(dimethylamino)-1-naphthyl-C,N]tin(II) and its W(CO)5 adduct
AU - Jastrzebski, Johann T B H
AU - van der Schaaf, Paul A.
AU - Boersma, Jaap
AU - Koten, Gerard van
AU - Heijdenrijk, Dick
AU - Goubitz, Kees
AU - de Ridder, Dirk J A
PY - 1989/5/9
Y1 - 1989/5/9
N2 - Reaction of [8-(dimethylamino)-1-naphthyl-C,N]lithium with SnCl2 affords the new monomeric stannylene bis[8-(dimethylamino)-1-naphthyl-C,N]tin(II) (3). The reaction between W(CO)5(NME3) and 3 yields {bis[8-(dimethylamino)-1-naphthyl-C,N]tin(II)} tungsten pentacarbonyl (4). The crystal structures of 3 and 4 have been determined by X-ray diffraction methods. 3: C24H24N2Sn, orthorhombic, space group Pbca with a 22.383(4), b 30.865(5), c 12.127(2) Å and Z = 16, final R = 0.067 for 4983 observed reflections. 4: C29H24N2O5SnW, a 12.509(3), b 15.191(1), c 9.780(1) Å, α 98.42(1), β 104.33(1), γ 107.27(1)°, space group P1, Z = 2, triclinic; R = 0.046 for 7116 observed reflections. The geometry about tin in 3 is distorted ψ-trigonal bypyramidal, and that in 4 is distorted trigonal bipyramidal. In both 3 and 4 the 8-(dimethylamino)-1-naphthyl groups are C,N-chelate bonded, with the C(1) atoms at equatorial sites and the nitrogen atoms at axial sites. The Sn lone pair in 3 and the W(CO)5 moiety in 4 occupy the remaining equatorial sites. 1H, 13C, and 119Sn solution NMR spectroscopic studies of 3 and 4 show that at low temperature (≤ - 15°C) they retain the structures found in the solid state. At higher temperatures fluxional processes become operative.
AB - Reaction of [8-(dimethylamino)-1-naphthyl-C,N]lithium with SnCl2 affords the new monomeric stannylene bis[8-(dimethylamino)-1-naphthyl-C,N]tin(II) (3). The reaction between W(CO)5(NME3) and 3 yields {bis[8-(dimethylamino)-1-naphthyl-C,N]tin(II)} tungsten pentacarbonyl (4). The crystal structures of 3 and 4 have been determined by X-ray diffraction methods. 3: C24H24N2Sn, orthorhombic, space group Pbca with a 22.383(4), b 30.865(5), c 12.127(2) Å and Z = 16, final R = 0.067 for 4983 observed reflections. 4: C29H24N2O5SnW, a 12.509(3), b 15.191(1), c 9.780(1) Å, α 98.42(1), β 104.33(1), γ 107.27(1)°, space group P1, Z = 2, triclinic; R = 0.046 for 7116 observed reflections. The geometry about tin in 3 is distorted ψ-trigonal bypyramidal, and that in 4 is distorted trigonal bipyramidal. In both 3 and 4 the 8-(dimethylamino)-1-naphthyl groups are C,N-chelate bonded, with the C(1) atoms at equatorial sites and the nitrogen atoms at axial sites. The Sn lone pair in 3 and the W(CO)5 moiety in 4 occupy the remaining equatorial sites. 1H, 13C, and 119Sn solution NMR spectroscopic studies of 3 and 4 show that at low temperature (≤ - 15°C) they retain the structures found in the solid state. At higher temperatures fluxional processes become operative.
UR - http://www.scopus.com/inward/record.url?scp=0002510441&partnerID=8YFLogxK
U2 - 10.1016/0022-328X(89)87205-5
DO - 10.1016/0022-328X(89)87205-5
M3 - Article
AN - SCOPUS:0002510441
SN - 0022-328X
VL - 367
SP - 55
EP - 68
JO - Journal of Organometallic Chemistry
JF - Journal of Organometallic Chemistry
IS - 1-2
ER -