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

doi:10.1016/j.inoche.2004.07.006

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

Department of Chemistry

Research output: Contribution to journal › Article › peer-review

135 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 language	English (US)
Pages (from-to)	1023-1026
Number of pages	4
Journal	Inorganic Chemistry Communications
Volume	7
Issue number	9
DOIs	https://doi.org/10.1016/j.inoche.2004.07.006
State	Published - Sep 2004

Keywords

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

ASJC Scopus subject areas

Physical and Theoretical Chemistry
Inorganic Chemistry
Materials Chemistry

Access to Document

10.1016/j.inoche.2004.07.006

Cite this

@article{8db5bbc2690a4d3ca47180a47a5188ff,

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",

author = "Neva Lazarova and Shelly James and John Babich and Jon Zubieta",

year = "2004",

month = sep,

doi = "10.1016/j.inoche.2004.07.006",

language = "English (US)",

volume = "7",

pages = "1023--1026",

journal = "Inorganic Chemistry Communications",

issn = "1387-7003",

publisher = "Elsevier",

number = "9",

}

TY - JOUR

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]

AU - Lazarova, Neva

AU - James, Shelly

AU - Babich, John

AU - Zubieta, Jon

PY - 2004/9

Y1 - 2004/9

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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U2 - 10.1016/j.inoche.2004.07.006

DO - 10.1016/j.inoche.2004.07.006

M3 - Article

AN - SCOPUS:4544281766

SN - 1387-7003

VL - 7

SP - 1023

EP - 1026

JO - Inorganic Chemistry Communications

JF - Inorganic Chemistry Communications

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