Synthesis and Reaction Chemistry of Sb(ECH₂CH₂NMe₂)₃ (E = O, S)

Abstract

The antimony aminoalkoxide and aminothiolates Sb(ECH 2 CH 2 NMe 2 ) 3 [E = O (1), S (2)] were synthesized and their ability to form adducts with other metal moieties investigated. Compound 1 forms 1:1 adducts with NiI 2 (3) and M(acac) 2 [M = Cd (4), Ni (5)], while 2 undergoes ligand exchange with AlMe 3 to afford Me 2-AlSCH 2 CH 2 NMe 2 (6). The structures of 2-4 and 6 were determined. Compound 2 incorporates three S,N-chelating ligands though the inter-1699 action with nitrogen is weaker than in analogous alkoxide complexes. Product 3 reveals one iodine has migrated from nickel to antimony, and all three alkoxide ligands bridge the two metals through μ 2 -O atoms. In contrast, in 4, only one alkoxide links the antimony and cadmium. Compound 6 adopts the same structure, a chelating S,N ligand generating a tetrahedral center at aluminum, as known tBu 2-AlSCH 2 CH 2 NR 2 species (R = Me, Et).

Alternative Precursors for the Synthesis of Binary Sb2E3 and Bi2E3 (E = S, Se, Te) Nanoparticles by the Hot Injection Method

“…The 1 H and 13 C NMR spectroscopic data of 1 correspond to values reported previously and are also similar to those observed for 2 . Compound 1 is a colorless liquid that starts to decompose at 256 °C, while 2 is a light yellow solid, which starts to decompose at 252 °C according to a differential scanning calorimetry (DSC) study (Figure ).…”

“…The O atoms of these ligands are involved in nonclassical hydrogen bonding (C4–H4C ··· O2′ 2.50 Å, 159.9°; C23–H23C ··· O3′ 2.61 Å, 153.7°), which may explain the nonoptimal conformation . The S‐analogue Sb(SCH 2 CH 2 NMe 2 ) 3 , in which the Sb atom adopts a distorted octahedral coordination geometry, shows no hydrogen bonding, and all three ligands have C–S–Sb–S torsion angles larger than 170°. Consequently, nearly equal Sb–S bond lengths [2.8443(18), 2.8481(18), 2.838(2) Å], which are longer than the Sb–O bond lengths in 1 due to the different covalent radii of O and S, and Sb–N bond lengths [2.8443(18), 2.8481(18), 2.838(2) Å] were observed.…”