A convenient synthesis, chemical characterization and reactivity of [Re(CO) 3(H 2O) 3]Br: The crystal and molecular structure of [Re(CO) 3(CH 3CN) 2Br]

Neva Lazarova, Shelly James, John Babich, Jon Zubieta

Research output: Contribution to journalArticle

122 Scopus citations

Abstract

The useful synthetic precursor [Re(CO) 3(H 2O) 3]Br (1) may be prepared in nearly quantitative yield by refluxing [Re(CO) 5]Br in H 2O for 24 h. Upon concentrating the solution, compound 1 is isolated as a microcrystalline light green powder, which is soluble in water and polar organic solvents. Recrystallization from methanol affords [Re(CO) 3(MeOH) 2Br] (2), while recrystallization from acetonitrile provides the crystalline [Re(CO) 3(CH 3CN) 2Br] (3). The lability of the aqua ligands of 1 is also manifested upon recrystallization from ethyl acetate/hexane, which yields [Re(CO) 3(OH)] 4·4H 2O (4·4H 2O). The reaction chemistry of 1 with dipyridylamine has been compared to that of the conventional starting material [NEt 4] 2[Re(CO) 3Br 3] and shown to produce a monophasic compound, free of contamination with NEt 4Br. Crystal data: C 7H 6BrN 2O 3Re (3): orthorhombic Pnma, a = 6.2289(3) Å, b = 13.1323(7) Å, c = 13.1700(7) Å, V = 1077.3(1) Å 3, D calc = 2.665 g/cm 3. C 3H 3O 5Re (4·4H 2O): tetragonal I-4, a = 11.5964(3) Å, c = 8.8764(4) Å, V = 1193.67(7) Å 3, D calc = 3.397 g/cm 3.

Original languageEnglish (US)
Pages (from-to)1023-1026
Number of pages4
JournalInorganic Chemistry Communications
Volume7
Issue number9
DOIs
StatePublished - Sep 1 2004

Keywords

  • 'Aqua ion' {Re(CO) (H O) }
  • Radiopharmaceuticals
  • {Re(CO) } core

ASJC Scopus subject areas

  • Physical and Theoretical Chemistry
  • Inorganic Chemistry
  • Materials Chemistry

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