Journal
INORGANIC CHEMISTRY
Volume 60, Issue 19, Pages 14697-14705Publisher
AMER CHEMICAL SOC
DOI: 10.1021/acs.inorgchem.1c01799
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Funding
- Office of Naval Research [MURI-N00014-15-1-2681]
- FONDECYT [1180683]
- Division of Chemistry (CHE)
- Division of Materials Research (DMR)
- National Science Foundation [NSF/CHE-1834750]
- U.S. DOE [DE-AC02-06CH11357]
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The reaction of [Nb(eta(6)-C6H3Me3)(2)] with ethylenediamine and K4Ge9 in the presence of 18-crown-6 yielded two cluster ions, 1 and 2, with distinct [Ge-6] motifs. These crystalline solids are dark brown, air-sensitive, and sparingly soluble or insoluble in most solvents. Characterization of cluster ions 1 and 2 was done through various techniques, revealing the presence of an electron-deficient carborane-like subunit in 1 and a two-center, two-electron cyclohexane-like subunit in 2.
[Nb(eta(6)-C6H3Me3)(2)] reacts with ethylenediamine (en) solutions of K4Ge9 in the presence of 18-crown-6 to give [(eta(6)-C6H3Me3)NbHGe6](2-) (1) and [(eta(6)-C6H3Me3)NbGe6Nb(eta(C6H3Me3)-C-6)](2-) (2) as their corresponding [K(18-crown-6)](+) salts. The crystalline solids are dark brown, air-sensitive, and sparingly soluble or insoluble in most solvents. The [K(18-crown-6)](+) salts of cluster ions 1 and 2 have been characterized by energydispersive X-ray (EDX) analysis, NMR studies, single-crystal X-ray diffraction, and electrospray ionization time-of-flight (ESI-TOF) mass spectrometry studies. Cluster ions 1 and 2 have markedly different [Ge-6] moieties: an electron-deficient carborane-like subunit in 1 and a two-center, two-electron cyclohexane-like subunit in 2.
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