A Series of the Twelve-Vertex Ferratricarbollides [2-(eta(5)-C(5)H(5))-9-X-closo-2,1,7,9-FeC(3)B(8)H(10)] (Where X = H(2)N, MeHN, Me(2)N, Bu(t)()HN, Bu(t)()(Me)N). A Highly Stable Metallatricarbaborane System with Amine Functions in the Para Position to the Metal Center

Josef Holub; Bohumír Grüner; Ivana Císarová I; Jirí Fusek; Zbynek Plzák; Francesc Teixidor; Clara Viñas; Bohumil Stíbr

doi:10.1021/ic981400e

A Series of the Twelve-Vertex Ferratricarbollides [2-(eta(5)-C(5)H(5))-9-X-closo-2,1,7,9-FeC(3)B(8)H(10)] (Where X = H(2)N, MeHN, Me(2)N, Bu(t)()HN, Bu(t)()(Me)N). A Highly Stable Metallatricarbaborane System with Amine Functions in the Para Position to the Metal Center

Inorg Chem. 1999 Jun 14;38(12):2775-2780. doi: 10.1021/ic981400e.

Authors

Josef Holub¹, Bohumír Grüner, Ivana Císarová I, Jirí Fusek, Zbynek Plzák, Francesc Teixidor, Clara Viñas, Bohumil Stíbr

Affiliation

¹ Institute of Inorganic Chemistry, Academy of Sciences of the Czech Republic, 250 68 Rez, Czech Republic, Faculty of Natural Sciences of Charles University, Hlavova 2030, 128 42 Prague 2, Czech Republic, and Institute of Material Sciences, CSIC, Campus UAB, 08193 Bellaterra, Spain.

PMID: 11671021
DOI: 10.1021/ic981400e

Abstract

Treatment of the zwitterionic amine tricarbollides of general formula 7-XH-nido-7,8,9-C(3)B(8)H(10) (1) [X = H(2)N (1a), Me(2)N (1b), Bu(t)()HN (1c), Bu(t)()(Me)N (1d)] with [(eta(5)-C(5)H(5))Fe(CO)(2)](2) in refluxing xylene for 24 h resulted in the formation of a series of new mixed-sandwich metallatricarbollides [2-(eta(5)-C(5)H(5))-9-X-closo-2,1,7,9-FeC(3)B(8)H(10)] (2) [X = H(2)N (2a), Me(2)N (2b), Bu(t)()HN (2c), Bu(t)()(Me)N (2d)] in yields 16-54%. The reaction of 1d is associated with partial loss of isobutylene and formation of the 9-MeHN-derivative 2e. Derivatives 2a and 2c were also isolated from reactions between the thallium salts Tl(+)[7-X-nido-7,8,9-C(3)B(8)H(10)](-) (Tl(+)1(-)) [X = H(2)N (Tl(+)1a(-)), BuH(t)()N (Tl(+)1c(-))] and [(eta(5)-C(5)H(5))Fe(CO)( 2)I] in refluxing toluene (yields 38 and 55%, respectively). All complexes of type 2 contain amine functionalities in para-positions with respect to the metal center, the complexation being in all cases associated with an extensive rearrangement of the cluster carbons into positions of maximum separation. The structures of all compounds were established by high-field NMR spectroscopy and mass spectrometry, and that of 2c was determined by an X-ray diffraction study.