Synthesis and characterization of a pentadentate Schiff base N[sub 3]O[sub 2] ligand and its neutral technetium(V) complex. X-ray structure of (N,N[prime]-3-azapentane-1,5-diylbis(3-(1-iminoethyl)-6-methyl-2H-pyran-2,4(3H)-dionato)(3-)-O,O[prime],N,N[prime],N[double prime])oxotechnetium(V)
- Univ. of British Columbia, Vancouver (Canada)
Preparations of a potentially pentadentate ligand, N,N[prime]-3-azapentane-1,5-diylbis(3-(1-iminoethyl)-6-methyl-2H-pyran-2,4-(3H)-dione) (H[sub 3]apa), and its neutral technetium(V) complex, [TcO(apa)], are described. The [sup 13]C and [sup 1]H NMR, infrared, optical, and mass spectra of the pentadentate ligand and its technetium(V) complex are reported. The X-ray structure of [TcO(apa)] has been determined. Crystals are orthorhombic, space group Pbca, with a = 12.833 (2) [angstrom], b = 33.320 (5) [angstrom], c = 9.942(4) [angstrom], V = 4251 (2) [angstrom], and Z = 8. The structure was solved by Patterson and Fourier methods and was refined by full-matrix least-squares procedures to R = 0.028 and R[sub W] = 0.032 for 4054 reflections with I [ge] 3[sigma](I). The technetium(V) complex has a highly distorted octahedral coordination geometry comprising a [TcO][sup 3+] core and the triply deprotonated pentadentate ligand wrapping around the metal center. One of the two oxygen donor atoms of the pentadentate ligand is located trans to the Tc[double bond]O bond while the remaining four donor atoms, N[sub 3]O, occupy the equatorial sites. The distance between the deprotonated N(1) atom to the Tc center is significantly shorter than a normal Tc-N single bond length of 2.10 angstroms, but longer than that for a Tc-N triple bond. [sup 1]H NMR spectral data reveal a rigid solution structure for the complex, which undergoes no conformational and configurational exchange at temperatures up to 50C.
- OSTI ID:
- 6837251
- Journal Information:
- Inorganic Chemistry; (United States), Vol. 30:26; ISSN 0020-1669
- Country of Publication:
- United States
- Language:
- English
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Related Subjects
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
TECHNETIUM COMPLEXES
CHEMICAL PREPARATION
CRYSTAL STRUCTURE
CARBON 13
LATTICE PARAMETERS
NITROGEN OXIDES
NUCLEAR MAGNETIC RESONANCE
ORTHORHOMBIC LATTICES
SCHIFF BASES
X-RAY DIFFRACTION
CARBON ISOTOPES
CHALCOGENIDES
COHERENT SCATTERING
COMPLEXES
CRYSTAL LATTICES
DIFFRACTION
EVEN-ODD NUCLEI
IMINES
ISOTOPES
LIGHT NUCLEI
MAGNETIC RESONANCE
NITROGEN COMPOUNDS
NUCLEI
ORGANIC COMPOUNDS
ORGANIC NITROGEN COMPOUNDS
OXIDES
OXYGEN COMPOUNDS
RESONANCE
SCATTERING
STABLE ISOTOPES
SYNTHESIS
TRANSITION ELEMENT COMPLEXES
400201* - Chemical & Physicochemical Properties