Synthesis and crystal and molecular structure of a (diethyl(N,N-diethylcarbamyl)methylenephosphonate)thorium nitrate complex

Journal Article · Fri Jan 01 04:00:00 EST 1982 · Inorg. Chem.; (United States)

DOI:https://doi.org/10.1021/ic00131a048· OSTI ID:5589093

Bowen, S M; Duesler, E N; Paine, R T

(Diethyl (N,N-diethylcarbamyl)methylenephosphonate)thorium (IV) nitrate, Th((C/sub 2/H/sub 5/O)/sub 2/P(O)CH/sub 2/C(O)N(C/sub 2/H/sub 5/)/sub 2/)/sub 2/(NO/sub 3/)/sub 4/(1),has been prepared from the combination of an acidic solution of Th(NO/sub 3/)/sub 4/ and a benzene solution of the carbamyl phosphonate ligand. The resulting complex has been characterized by infrared and /sup 1/H, /sup 13/C(/sup 1/H), and /sup 31/P(/sup 1/H) NMR spectroscopies. A single-crystal x-ray analysis of 1 has been completed, and the complex was found to crystallize in the monoclinic space group C2/c with a = 20.754 (6) A, b = 8.470 (1) A, c = 21.183 (5) A, ..beta.. = 101.69 (2)/sup 0/, Z = 4, V = 3646.6 A/sup 3/, and rho/sub calcd/ = 1.79 g cm/sup -3/. The structure was solved by standard heavy-atom techniques. Full-matrix least-squares refinement of the structure has led to final discrepancy indices of R/sub F/ = 4.0% and R/sub sF/ = 5.0% on the basis of 4385 independent reflections. The crystal contains monomeric units of 1 that have crystallographic C/sub 2/ symmetry. The thorium atom is bonded to both carbonyl and phosphoryl oxygen atoms of two carbamyl phosphonate ligands and two oxygen atoms of each of four nitrate groups. The resulting coordination number for the thorium atom is 12. Several important bond distances include Th-O(carbonyl) 2.453 (4) A, Th-O(phosphoryl) 2.482 (4) A, and Th-O(nitrate) 2.638 (3) A (average).

• Research Organization: Univ. of New Mexico, Albuquerque
• OSTI ID: 5589093
• Journal Information: Inorg. Chem.; (United States), Journal Name: Inorg. Chem.; (United States) Vol. 21:1; ISSN INOCA
• Country of Publication: United States
• Language: English

Related Subjects

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEAR CHEMISTRY
400702* -- Radiochemistry & Nuclear Chemistry-- Properties of Radioactive Materials
ACTINIDE COMPLEXES
BOND ANGLE
CARBON 13
CARBON ISOTOPES
CARBOXYLIC ACID ESTERS
COHERENT SCATTERING
COMPLEXES
CRYSTAL LATTICES
CRYSTAL STRUCTURE
DATA
DIFFRACTION
DISTANCE
ESTERS
EVEN-ODD NUCLEI
EXPERIMENTAL DATA
HYDROGEN 1
HYDROGEN ISOTOPES
INFORMATION
INFRARED SPECTRA
INTERATOMIC DISTANCES
ISOTOPES
LIGANDS
LIGHT NUCLEI
MOLECULAR STRUCTURE
MONOCLINIC LATTICES
NITRATES
NITROGEN COMPOUNDS
NMR SPECTRA
NUCLEI
NUMERICAL DATA
ODD-EVEN NUCLEI
ORGANIC COMPOUNDS
ORGANIC NITROGEN COMPOUNDS
ORGANIC PHOSPHORUS COMPOUNDS
OXYGEN COMPOUNDS
PHOSPHONIC ACID ESTERS
PHOSPHORUS 31
PHOSPHORUS ISOTOPES
SCATTERING
SPECTRA
STABLE ISOTOPES
SYNTHESIS
THORIUM COMPLEXES
X-RAY DIFFRACTION