10.1021/ic700945a.s003 Zhi Yang Zhi Yang Xiaoli Ma Xiaoli Ma Herbert W. Roesky Herbert W. Roesky Ying Yang Ying Yang Jörg Magull Jörg Magull Arne Ringe Arne Ringe Synthesis and Characterization of Well-Defined Aluminum-Containing Heterobimetallic Selenides<sup>†</sup> American Chemical Society 2007 THF Ph 2 GeCl 2 novel aluminum heterobimetallic selenides HC aluminum atom Cp 2 TiCl 2 Compound 2 Cp 2 ZrCl 2 NMR LAl 2 GeCl 2 spirocyclic arrangement 2007-08-20 00:00:00 Dataset https://acs.figshare.com/articles/dataset/Synthesis_and_Characterization_of_Well_Defined_Aluminum_Containing_Heterobimetallic_Selenides_sup_sup_/2990332 A series of novel aluminum heterobimetallic selenides were reported. The reaction of LAl(SeH)<sub>2</sub> (<b>1</b>) with LiN(SiMe<sub>3</sub>)<sub>2</sub> resulted in the formation of [LAl(SeLi)<sub>2</sub>(THF)<sub>2</sub>] (<b>2</b>) (L = HC(CMeNAr)<sub>2</sub>, Ar = 2,6-<i>i</i>Pr<sub>2</sub>C<sub>6</sub>H<sub>3</sub>). Compound <b>2</b> reacted with Me<sub>2</sub>GeCl<sub>2</sub>, Ph<sub>2</sub>GeCl<sub>2</sub>, Cp<sub>2</sub>TiCl<sub>2</sub>, and Cp<sub>2</sub>ZrCl<sub>2</sub>, respectively, to produce LAl(μ-Se)<sub>2</sub>GeMe<sub>2</sub> (<b>3</b>), LAl(μ-Se)<sub>2</sub>GePh<sub>2</sub> (<b>4</b>), LAl(μ-Se)<sub>2</sub>TiCp<sub>2</sub> (<b>5</b>), and LAl(μ-Se)<sub>2</sub>ZrCp<sub>2</sub> (<b>6</b>) in moderate yields. Compounds <b>2</b>−<b>6</b> were characterized by elemental analysis, NMR, and electron impact-MS. The X-ray single-crystal structure of <b>3</b> is reported and confirms the spirocyclic arrangement of the aluminum atom within the six-membered AlN<sub>2</sub>C<sub>3</sub> and four-membered AlSe<sub>2</sub>Ge rings.