Synthesis and coordination chemistry of tripodal dialkyl[1,2-bis(diethylcarbamoyl)ethyl]phosphonates with lanthanide nitrates |
| |
Institution: | 1. Membrane Science and Separation Technology Division, Electro Membrane Processes Laboratory, CSIR-Central Salt and Marine Chemicals Research Institute, Bhavnagar 364002, India;2. Academy of Scientific and Innovative Research (AcSIR), Ghaziabad 201002, India;3. Inorganic Materials and Catalysis Division, CSIR-Central Salt and Marine Chemicals Research Institute, Bhavnagar 364002, India;4. Advanced polymer Design Development Research Laboratory (APDDRL), School for Advanced Research in petrochemicals (SARP), Central Institute of Petrochemical Engineering and Technology (CIPET), Bengaluru, India |
| |
Abstract: | Trifunctional dialkyl 1,2-bis(diethylcarbamoyl)- ethyl] phosphonates, (RO)2P(O)CHC(O)N(C2H5)2]- CH2C(O)N(C2H5)2] R CH3, C2H5, i-C3H7, n-C6H13 were prepared from the respective sodium salts, Na(RO)2P(O)CHC(O)N(C2H5)2] and N,N- diethylchloroacetamide, and they were characterized by elemental analysis, mass, infrared and NMR spectroscopy. The molecular structure of (i-C3H7O)2- P(O)CHC(O)N(C2H5)2]CH2C(O)N(C2H5)2] was determined by single crystal X-ray diffraction analysis and found to crystallize in the monoclinic space group P21/c with a=15.589(6), b=9.783(4), c= 16.283(7) Å, β = 110.90(3)°, Z = 4 and V= 2320(2) Å3. The structure was solved by direct methods and blocked least-squares refinement converged with Rf = 5.7% and RwF= 4.4% on 2266 unique data with F>4σ(F). Important bond distances include PO 1.459(3) Å, CHCO 1.228(3) Å and CHCH2CO 1.223(3) Å. The coordination chemistry of the ligand with several lanthanides was examined, and the structure of the complex Gd(NO3)3{(i-C3H7O)2P(O)CHC(O)N(C2H5)2]CH2C(O)N(C2H5)2]}2·H2O was determined. The complex crystallized in the monoclinic space group P21/n with a = 13.524(5), b = 22.033(4), c = 19.604(4) Å β = 106.22(2)°, Z = 4 and V= 5609(3) Å3. The structure was solved by heavy atom techniques and blocked least-squares refinement converged with RF = 5.9% and RwF = 4.1% on 5275 reflections with F > 4σ(F). Both trifunctional ligands were found to bond to Gd(III) through only the phosphoryl oxygen atoms. The remainder of the Gd coordination sphere was composed of three bidentate nitrate oxygen atoms and an oxygen bonded water molecule. Several important bond distances include GdO(phosphoryl)av = 2.343(5) Å, GdO(nitrate)av = 2.475(7) Å, GdO(water) = 2.354(5) Å, PO(phosphoryl)av = 1.467(6) Å, CHCOav = 1.242(10) Å and CHCH2COav = 1.209(11) Å. |
| |
Keywords: | |
本文献已被 ScienceDirect 等数据库收录! |
|