Bifunctional Single Amino Acid Chelates for Labeling of Biomolecules with the {Tc(CO)3}+ and {Re(CO)3}+ Cores. Crystal and Molecular Structures of [ReBr(CO)
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- 作者：Sangeeta Ray Banerjee ; Murali K. Levadala ; Neva Lazarova ; Lihui Wei ; John F. Valliant ; Karin A. Stephenson ; John W. Babich ; Kevin P. Maresca ; and Jon Zubieta
- 刊名：Inorganic Chemistry
- 出版年：2002
- 出版时间：December 2, 2002
- 年：2002
- 卷：41
- 期：24
- 页码：6417 - 6425
- 全文大小：183K
- 年卷期：v.41,no.24(December 2, 2002)
- ISSN：1520-510X
文摘
The reactions of a series of potentially tridentate ligands, derived from single amino acids or amino acid analogues, with[NEt4]2[ReBr3(CO)3] have been investigated. The model compounds [Re(CO)3Br{(2-pyridylmethyl)NH2}] (1) and [Re(CO)3{(2-pyridylmethyl)2NH}]Br (2) were also prepared and structurally characterized. With ligands possessing two pyridylappendages, (2-pyridylmethyl)2NX (X = -CH2CO2H, -CH2CO2Et, -CH2CH2CO2H, -CH2CH2CO2Et, -CH2CH2CH2CH2CH(NHCO2tBu)CO2H), complexes of the type [Re(CO)3(ligand)]Br (3-6) were isolated. All possess the fac-{Re(CO)3N3}coordination geometry in the cationic molecular unit. Similarly, the ligands with the imidazolyl arms (2-pyridylmethyl){2-(1-methylimidazolyl)methyl}NCH2CO2Et and {2-(1-methylimidazolyl)methyl}2NCH2CO2Et, complexes 7 and 8 of the same[Re(CO)3(ligand)]Br type, were prepared. Replacement of one pyridyl arm with a thiophene group yielded the complex[Re(CO)3{(2-pyridylmethyl)N(CH2CO2)(2-thiophenemethyl)}] (9), while additional substitution of X = -H for -CH2CO2Hyielded [Re(CO)3Br{(2-pyridylmethyl)NH(2-thiophenemethyl)}] (10). In both 9 and 10, the thiophene is uncoordinatedand pendant, and the derivatives display fac-{Re(CO)3N2O} and fac-{Re(CO)3N2Br} coordination geometries, respectively.Crystal data: C9H8BrN2O3Re (1), triclinic P
, a = 8.156(1) Å, b = 12.077(1) Å, c = 12.945(2) Å, 
= 92.183(3)
, 
= 107.848(3), 
= 100.955(7), V = 1185.1(3) Å, Z = 4; C15H13BrN3O3Re (2), tetragonal P41, a = 8.6095(3) Å, c =22.228(1) Å, V = 1646.9(1) Å3, Z = 4; C17H14BrN3O5Re·CH3OH (3), monoclinic P21/m, a = 7.4425(3) Å, b = 9.7596(4)Å, c = 14.0646(6) Å, = 97.753(1), V = 1012.26(7) Å3, Z = 2; C19H19BrN3O5Re (4), tetragonal P
21c, a = 16.895(3)Å, c = 15.042(3) Å, V = 4293.7(13) Å3, Z = 8; C18H20BrN4O5Re·CH3OH·H2O (7), monoclinic P21/c, a = 10.2816(4) Å,b = 30.386(1) Å, c = 14.5810(6) Å, = 99.868(1), V = 4488.03(3) Å3, Z = 8; C17H21BrN5O5Re·0.5CH2Cl2·0.5H2O(8), triclinic P, a = 11.5363(6) Å, b = 13.1898(6) Å, c = 16.4933(8) Å, = 89.356(1), = 74.907(1), =76.216(1), V = 2349.8(2) Å3, Z = 4; C16H13N2O5ReS (9), monoclinic P21/c, a = 17.2072(7) Å, b = 8.5853(4) Å, c =11.5607(5) Å, = 101.73(1), V = 1672.2(1) Å3, Z = 4; and C14H12N2O3BrReS (10), triclinic P, a = 7.5585(3) Å, b= 9.7713(4) Å, c = 11.7103(4) Å, = 109.566(1), = 98.298(1), = 100.925(1), V = 779.73(5) Å3, Z = 2.
, a = 8.156(1) Å, b = 12.077(1) Å, c = 12.945(2) Å, = 92.183(3), = 107.848(3), = 100.955(7), V = 1185.1(3) Å, Z = 4; C15H13BrN3O3Re (2), tetragonal P41, a = 8.6095(3) Å, c =22.228(1) Å, V = 1646.9(1) Å3, Z = 4; C17H14BrN3O5Re·CH3OH (3), monoclinic P21/m, a = 7.4425(3) Å, b = 9.7596(4)Å, c = 14.0646(6) Å, = 97.753(1), V = 1012.26(7) Å3, Z = 2; C19H19BrN3O5Re (4), tetragonal P21c, a = 16.895(3)Å, c = 15.042(3) Å, V = 4293.7(13) Å3, Z = 8; C18H20BrN4O5Re·CH3OH·H2O (7), monoclinic P21/c, a = 10.2816(4) Å,b = 30.386(1) Å, c = 14.5810(6) Å, = 99.868(1), V = 4488.03(3) Å3, Z = 8; C17H21BrN5O5Re·0.5CH2Cl2·0.5H2O(8), triclinic P, a = 11.5363(6) Å, b = 13.1898(6) Å, c = 16.4933(8) Å, = 89.356(1), = 74.907(1), =76.216(1), V = 2349.8(2) Å3, Z = 4; C16H13N2O5ReS (9), monoclinic P21/c, a = 17.2072(7) Å, b = 8.5853(4) Å, c =11.5607(5) Å, = 101.73(1), V = 1672.2(1) Å3, Z = 4; and C14H12N2O3BrReS (10), triclinic P, a = 7.5585(3) Å, b= 9.7713(4) Å, c = 11.7103(4) Å, = 109.566(1), = 98.298(1), = 100.925(1), V = 779.73(5) Å3, Z = 2.