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 A Zubieta

Research output: Contribution to journalArticle

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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 2004

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Carbon Monoxide
Molecular Structure
Hexane
Acetonitrile
Organic solvents
Molecular structure
Methanol
Contamination
molecular structure
reactivity
Crystal structure
Crystallization
Ligands
methylidyne
Crystalline materials
Powders
Crystals
crystal structure
synthesis
Water

Keywords

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

ASJC Scopus subject areas

  • Biochemistry
  • Inorganic Chemistry
  • Physical and Theoretical Chemistry
  • Materials Chemistry

Cite this

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]. / Lazarova, Neva; James, Shelly; Babich, John; Zubieta, Jon A.

In: Inorganic Chemistry Communications, Vol. 7, No. 9, 09.2004, p. 1023-1026.

Research output: Contribution to journalArticle

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title = "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]",
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) {\AA}, b = 13.1323(7) {\AA}, c = 13.1700(7) {\AA}, V = 1077.3(1) {\AA} 3, D calc = 2.665 g/cm 3. C 3H 3O 5Re (4·4H 2O): tetragonal I-4, a = 11.5964(3) {\AA}, c = 8.8764(4) {\AA}, V = 1193.67(7) {\AA} 3, D calc = 3.397 g/cm 3.",
keywords = "'Aqua ion' {Re(CO) (H O) }, Radiopharmaceuticals, {Re(CO) } core",
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T1 - A convenient synthesis, chemical characterization and reactivity of [Re(CO) 3(H 2O) 3]Br

T2 - The crystal and molecular structure of [Re(CO) 3(CH 3CN) 2Br]

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AU - James, Shelly

AU - Babich, John

AU - Zubieta, Jon A

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N2 - 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.

AB - 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.

KW - 'Aqua ion' {Re(CO) (H O) }

KW - Radiopharmaceuticals

KW - {Re(CO) } core

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