Article ID | Journal | Published Year | Pages | File Type |
---|---|---|---|---|
1323260 | Journal of Organometallic Chemistry | 2015 | 5 Pages |
•Tetraphenylantimony carborane carboxylate (1) was obtained in high yield.•The synthesis of tetraphenylantimony carborane carboxylate proceeds with CO2 elimination.•Bis(tetraphenylantimony) carborane bis(carboxylate) (2) was obtained in high yield.•There are no intramolecular contacts in 1 between Sb and О atom of CO group.•Crystal structures are characterized by weak intermolecular hydrogen bonds H⋯O.
The reaction of equimolar amounts of pentaphenylantimony with carboranedicarboxylic acid in toluene lead to tetraphenylantimony carborane carboxylate (1) in high yield. When using 2:1 M ratio of initial reagents, bis(tetraphenylantimony) carborane bis(carboxylate) (2) was obtained in 94% yield. Sb atoms in 1 and 2 form the distorted trigonal-bipyramidal coordination with carboxylate and phenyl ligands in axial positions (CaxialSbO are 174.06(12)° and 175.74(13)°, 176.77(13)° respectively). The Sb–O и Sb–C bond distances are 2.469(3) Å and 2.095(4)−2.136(4) Å in 1 and 2.275(3), 2.364(3) and 2.112(4)−2.173(4) Å in 2. There are no intramolecular contacts in 1 between Sb and О atom of CO group. In 2 the bond distances Sb⋯O(=C) (3.203(4) и 3.213(4) Å) are much less than a sum of van der Vaals radii of Sb and O atoms. Crystal structures of 1 and 2 are characterized by weak intermolecular hydrogen bonds H⋯O (2.25–2.53 and 2.54 Å, respectively).
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