Syntheses and crystal structures of new naphthalene – and anthracene – vanadate salts and an unprecedented dimetallabis(anthracene) sandwich complex: [Na(tetrahydrofuran)3][V2(anthracene)2]

Reduction of bis(naphthalene)vanadium(0) by potassium naphthalene (KNp) in tetrahydrofuran (THF) provides a highly reactive, thermolabile, and so far unisolable brown substance, which affords the first reported derivatives of bis(naphthalene)vanadates. From these solutions, thermally stable (298   K) and structurally characterized compounds have been obtained, including dark-red rods of catena-poly[bis( μ 3- η 4: η 6: η 4-naphthalene)tetrakis(tetrahydrofuran)dipotassiumvanadium], [K2V(C4H8O)4(C10H8)2]n or [K(THF)2]2[V(C10H8)2] (3), and red plates of (4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane)potassium [1,2-bis(dimethylphosphanyl)ethane]bis( η 4-naphthalene)vanadium tetrahydrofuran monosolvate, [K(C18H36N2O6)][V(C10H8)2(C6H16P2)] · C4H8O or [K([2.2.2]cryptand)][V(C10H8)2(dmpe)] · THF [dmpe is 1,2-bis(dimethylphosphanyl)ethane] (4b). Notably, [V(C10H8)2]2 − is the only example of a structurally authenticated homoleptic bis(arene)metallate dianion and was obtained by further reduction of the brown material by KNp in THF, in the presence of trimethylphosphane (PMe3). Addition of anthracene (An) to the brown material in THF afforded deep-violet and paramagnetic crystalline (1,4,7,10,13,16-hexaoxacyclooctadecane)bis(tetrahydrofuran)potassium [( η 4-anthracene)(tetrahydrofuran)vanadium]- μ - η 4: η 2-anthracene-[(1,4,7,10,13,16-hexaoxacyclooctadecane)potassium]- μ - η 2: η 4-anthracene-[( η 4-anthracene)(tetrahydrofuran)vanadium] tetrahydrofuran d...

Source: Acta Crystallographica Section C - February 9, 2022 Category: Chemistry Authors: Kucera, B.E. Young, V.G. Brennessel, W.W. Ellis, J.E. Tags: naphthalene anthracene bis(polyarene)vanadates dimetallabis(anthracene) sandwich complex crystal structure research papers Source Type: research