The transmetalation of bis[(trimethylsilyl)methyl]zinc in THF with distilled strontium and barium yielded bis(tetrahydrofuran)strontium and tetrakis(tetrahydrofuran)barium bis-{tris[(trimethylsilyl)methyl]zincates} (1 and 2, respectively). The reaction of barium with Zn(CH 2 SiMe 3 ) 2 in toluene gave bis(η 6 -toluene)barium bis{tris[(trimethylsilyl)methyl]zincate} (3) with rather short Ba-C bond lengths of 3.028(5) and 3.055(5) Å. All of these trialkylzincate anions coordinate as bidentate ligands with M-C-Zn three-center two-electron bonds. When carried out in the nondonor solvent heptane, the transmetalation reaction yielded barium bis{tris[(trimethylsilyl)methyl]zincate} (4), which reacts with THF to give the complex 2 and a small amount of [(THF) 3 Ba] 2 (µ 4 -O) 2 [(Me 3 SiCH 2 ZnCH 2 ) 2 SiMe 2 ] 2 (5). The central moiety is a centrosymmetric Ba 2 O 2 cycle with Ba-O distances of 2.514(2) and 2.570(3) Å. The oxygen dianion is surrounded, distorted tetrahedrally by two barium and two zinc atoms.
The reaction of bis(cyclopentadienyl) zircona-2,3,4,5-tetraethylcyclopentadiene (1) with antimony trichloride yields 1-chloro-2,3,4,5-tetraethyl-1-stibole (2). The reduction with potassium gives semi(tetrahydrofuran-O)bispotassium bis (2,3,4,5-tetraethylstibolide) (3). The potassium stibolide columns are linked via K-Sb contacts of 3.618 Å, thus forming a wavelike layer structure. The molecular structure shows three crystallographically different metal cations. One potassium atom is located between two stibolide anions, whereas the other ones show additional K-O and K-Sb contacts of 2. 681 and 3.618 Å, respectively.
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