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
Reaction of [8-(dimethylamino)-1-naphthyl- C, N]lithium with SnCl 2 affords the new monomeric stannylene bis[8-(dimethylamino)-1-naphthyl- C, N]tin(II) ( 3). The reaction between W(CO) 5(NME 3) and 3 yields {bis[8-(dimethylamino)-1-naphthyl- C, N]tin(II)} tungsten pentacarbonyl ( 4). The crystal str...
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Published in | Journal of organometallic chemistry Vol. 367; no. 1; pp. 55 - 68 |
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Main Authors | , , , , , , |
Format | Journal Article |
Language | English |
Published |
Lausanne
Elsevier B.V
09.05.1989
Elsevier Science |
Subjects | |
Online Access | Get full text |
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Summary: | Reaction of [8-(dimethylamino)-1-naphthyl-
C,
N]lithium with SnCl
2 affords the new monomeric stannylene bis[8-(dimethylamino)-1-naphthyl-
C,
N]tin(II) (
3). The reaction between W(CO)
5(NME
3) 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: C
24H
24N
2Sn, 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: C
29H
24N
2O
5SnW,
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
P
1
,
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. |
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ISSN: | 0022-328X 1872-8561 |
DOI: | 10.1016/0022-328X(89)87205-5 |