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Bis(pyrene)metal complexes of vanadium, niobium and titanium: isolable homoleptic pyrene complexes of transition metals
Author(s) -
Kucera Benjamin E.,
Jilek Robert E.,
Brennessel William W.,
Ellis John E.
Publication year - 2014
Publication title -
acta crystallographica section c
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.304
H-Index - 17
ISSN - 2053-2296
DOI - 10.1107/s2053229614015290
Subject(s) - homoleptic , pyrene , vanadium , niobium , transition metal , titanium , chemistry , metal , inorganic chemistry , organic chemistry , catalysis
Reduction of VCl 3 (THF) 3 (THF is tetrahydrofuran) and NbCl 4 (THF) 2 by alkali metal pyrene radical anion salts in THF affords the paramagnetic sandwich complexes bis[(1,2,3,3a,10a,10b‐η)‐pyrene]vanadium(0), [V(C 16 H 10 ) 2 ], and bis[(1,2,3,3a,10a,10b‐η)‐pyrene]niobium(0), [Nb(C 16 H 10 ) 2 ]. Treatment of tris(naphthalene)titanate(2−) with pyrene provides the isoelectronic titanium species, isolated as an (18‐crown‐6)potassium salt, namely catena ‐poly[[(18‐crown‐6)potassium]‐μ‐[(1,2‐η:1,2,3,3a,10a,10b‐η)‐pyrene]‐titanate(−I)‐μ‐[(1,2,3,3a,10a,10b‐η:6,7‐η)‐pyrene]], {[K(C 12 H 24 O 6 )][Ti(C 16 H 10 ) 2 ]} n . The first two compounds have very similar packing, with neighboring molecules arranged orthogonally to one another, such that aromatic donor–acceptor interactions are likely responsible for the specific arrangement. The asymmetric unit contains a half‐occupancy metal center η 6 ‐coordinated to one pyrene ligand, with the full M (pyrene) 2 molecule generated by a crystallographic inversion center. In the titanium compound, the cations and anions are in alternating contact throughout the crystal structure, in one‐dimensional chains along the [101] direction. As in the other two compounds, the asymmetric unit contains a half‐occupancy Ti atom η 6 ‐coordinated to one pyrene ligand. Additionally, the asymmetric unit contains one half of an (18‐crown‐6)potassium cation, located on a crystallographic inversion center coincident with the K atom. The full formula units are generated by those inversion centers. In all three structures, the pyrene ligands are eclipsed and sandwich the metals in one of two inversion‐related sites. These species are of interest as the first isolable homoleptic pyrene transition metal complexes to be described in the scientific literature.

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