Details of the synthesis, physical and spectroscopic characterization, and thermal decomposition of tris(benzylthiolato)bismuth, (BnS)(3)Bi, Bn = CH(2)C(6)H(5), are presented. Results from pyrolysis of (BnS)(3)Bi demonstrate that this compound is a convenient precursor to phase-pure, polycrystalline Bi(2)S(3) with low carbon and hydrogen contamination under mild thermal conditions (ca. 275 degrees C). Flow-tube pyrolysis produces small ( approximately 1 &mgr;m) spherical particles, whereas sealed-tube pyrolysis produces 6-&mgr;m diameter spherical particles composed of radiating acicular crystallites. Bi(2)S(3) was characterized by X-ray powder diffraction and scanning electron microscopy.
The title compound, (Bn2SnTe)3, Bn = CH2C6H5, was prepared in high yield by treating
Bn2SnCl2 with (NH4)2Te. Details of the synthesis and characterization (1H, 13C, 119Sn, and
125Te NMR; IR, single-crystal XRD, and elemental analyses) are presented. (Bn2SnTe)3 serves
as an efficient single-source precursor to phase-pure cubic SnTe under mild conditions
The syntheses and characterization of two types of complexes
having a metal−Salan ligand
stoichiometry of 2:1 (where Salan =
N,N ‘-bis(o-hydroxybenzyl)-1,2-diaminoethane
(SaleanH4),
N,N ‘-bis(o-hydroxybenzyl)-1,2-diaminobenzene
(SalophanH4), and
N,N ‘-bis(o-hydroxybenzyl)-1,2-diamino-(4,5-dimethyl)benzene
(SalomphanH4)) are reported. The first
are
designated type I and are of the general formula
LHAlR(AlR2), where L = Salean [R =
Me
(1), Et (2), iBu
(3)], Salophan [R = Me (4), Et
(5), iBu (6)], and Salomphan
[R = Me (7), Et
(8), iBu (9)]. Formed by
the thermolysis of RH from the type I complexes, the type
II
complexes are of the general formula
[LAl(AlR2)]2, where L = Salophan [R
= Me (10), iBu
(11)] and Salomphan [R = Me (12),
iBu (13)]. The type I complexes can
be converted into
the trimetallic derivatives SalanAlR(AlR2)2
(type III) through the addition of AlR3 while
the
type II cannot. One structurally characterized trimetallic
complex, SalophanAlEt(AlEt2)2
(14), serves as a representative of this successful
transformation.
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