Tridentate coordination by a tripodal ligand system: Synthesis and crystal and molecular structure of (diisopropyl (1,2-bis(diethylcarbamoyl)ethyl)phosphonate)erbium(III) nitrate

Journal Article · Wed Apr 06 00:00:00 EDT 1988 · Inorg. Chem.; (United States)

DOI:https://doi.org/10.1021/ic00280a025· OSTI ID:5614963

McCabe, D J; Duesler, E N; Paine, R T

Combination of Er(NO/sub 3/)/sub 3/ /times/ 5H/sub 2/O with mixtures of (C/sub 2/H/sub 5/O)/sub 3/P(O) and the trifunctional ligand (i-C/sub 3/H/sub 7/O)/sub 2/P(O)CH(C(O)N(C/sub 2/H/sub 5/)/sub 2/)(CH/sub 2/C(O)N(C/sub 2/H/sub 5/)/sub 2/) leads to the formation of a crystalline complex, Er(NO/sub 3/)/sub 3/((i-C/sub 3/H/sub 7/O)/sub 2/P(O)CH(C(O)N(C/sub 2/H/sub 5/)/sub 2/)(CH/sub 2/C(O)N(C/sub 2/H/sub 5/)/sub 2/)). The complex was characterized by elemental analysis, infrared and NMR spectroscopy, and single-crystal x-ray diffraction analysis. The complex was found to crystallize in the monoclinic space group P2/sub 1//n with a = 13.994 (3) /angstrom/, b = 14.914 (4) /angstrom/, c = 15.104 (3) /angstrom/, /beta/ = 103.74 (2)/degree/, Z = 4, and V = 3062 (1) /angstrom//sup 3/. The structure was solved by heavy-atom techniques, and blocked least-squares refinement converged with R/sub F/ = 6.5% and R/sub wF/ = 5.7% on 352 parameters and 3563 reflections with F > 4/sigma/(F). The Er ion is nine-coordinate by bonding with six oxygen atoms contributed by three bidentate nitrate ions and three oxygen atoms provided by one tripodal ligand. The important internal coordination sphere bond distances are Er-O(1) = 2.298 (6) /angstrom/, Er-O(4) = 2.326 (7) /angstrom/, and Er-O(5) = 2.267 (8) /angstrom/, which involve the ligand coordination sites, and Er-O(nitrate)/sub av/ = 2.407 (9) /angstrom/. 12 refs., 1 figs., 3 tabs.

• Research Organization: Univ. of New Mexico, Albuquerque (USA)
• DOE Contract Number: AC04-79ER10465
• OSTI ID: 5614963
• Journal Information: Inorg. Chem.; (United States), Vol. 27:7
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
ERBIUM COMPLEXES
CHEMICAL PREPARATION
CRYSTAL STRUCTURE
ORGANIC PHOSPHORUS COMPOUNDS
ORGANOMETALLIC COMPOUNDS
EXPERIMENTAL DATA
INFRARED SPECTRA
X-RAY DIFFRACTION
COHERENT SCATTERING
COMPLEXES
DATA
DIFFRACTION
INFORMATION
NUMERICAL DATA
ORGANIC COMPOUNDS
RARE EARTH COMPLEXES
SCATTERING
SPECTRA
SYNTHESIS
400201* - Chemical & Physicochemical Properties