In:
Dalton Transactions, Royal Society of Chemistry (RSC), Vol. 52, No. 28 ( 2023), p. 9582-9589
Abstract:
The new Ge( ii ) cluster [Ge 6 (μ 3 -O) 4 (μ 2 -OC 6 H 2 -2,4,6-Cy 3 ) 4 ](NH 3 ) 0.5 (1) and three divalent Group 14 aryloxide derivatives [Ge(OC 6 H 2 -2,4,6-Cy 3 ) 2 ] 2 (2), [Sn(OC 6 H 2 -2,4,6-Cy 3 ) 2 ] 2 (3), and [Pb(OC 6 H 2 -2,4,6-Cy 3 ) 2 ] 2 (4) of the new tricyclohexylphenyloxo ligand, [(–OC 6 H 2 -2,4,6-Cy 3 ) 2 ] 2 (Cy = cyclohexyl), were synthesized and characterized. Complexes 1–4 were obtained by reaction of the metal bissilylamides M(N(SiMe 3 ) 2 ) 2 (M = Ge, Sn, Pb) with 2,4,6-tricyclohexylphenol in hexane at room temperature. If the freshly generated reaction mixture for the synthesis of 2 is stirred in solution for 12 h at room temperature, the cluster [Ge 6 (μ 3 -O) 4 (μ 2 -OC 6 H 2 -2,4,6-Cy 3 ) 4 ](NH 3 ) 0.5 (1), which features a rare Ge 6 O 8 core that includes ammonia molecules in non-coordinating positions, is formed. Complexes 3 and 4 were also characterized via 119 Sn{ 1 H} NMR and 207 Pb NMR spectroscopy and feature signals at −280.3 ppm ( 119 Sn{ 1 H}, 25 °C) and 1541.0 ppm ( 207 Pb, 37 °C), respectively. The spectroscopic characterization of 3 and 4 extends known 119 Sn parameters for dimeric Sn( ii ) aryloxides, but data for 207 Pb NMR spectra for Pb( ii ) aryloxides are rare. We present also a rare VT-NMR study of a homoleptic 3-coordinate Pb( ii ) aryloxide. The crystal structures of 2, 3, and 4 feature interligand H⋯H contacts that are similar in number to those of related transition metal derivatives despite the larger size of the group 14 elements.
Type of Medium:
Online Resource
ISSN:
1477-9226
,
1477-9234
Language:
English
Publisher:
Royal Society of Chemistry (RSC)
Publication Date:
2023
detail.hit.zdb_id:
1472887-4
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