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Title: Synthesis and crystal structure of (S, S, S, S)-N, N′-bis[N-(P-toluenesulfonamido)-1,2-diphenylethyl]ethylenediamine

Abstract

(S, S, S, S)-N,N′-bis[N-(p-toluenesulfonamido)-1,2-diphenylethyl] ethylenediamine (C{sub 44}H{sub 46}N{sub 4}O{sub 4}S{sub 2}), has been synthesized and structurally characterized by elemental analysis, {sup 1}H-NMR, MS, IR and single-crystal X-ray diffraction. The title compound contains four chiral centers with C atoms in S configuration. Molecules are connected to one another by hydrogen bonds between sulfonamide nitrogen and sulfonyl oxygen to form chains alone a axis.

Authors:
; ; ;  [1]
  1. Hangzhou Normal University, College of Material Chemistry and Chemical Engineering (China)
Publication Date:
OSTI Identifier:
22311405
Resource Type:
Journal Article
Resource Relation:
Journal Name: Crystallography Reports; Journal Volume: 58; Journal Issue: 7; Other Information: Copyright (c) 2013 Pleiades Publishing, Inc.; http://www.springer-ny.com; Country of input: International Atomic Energy Agency (IAEA)
Country of Publication:
United States
Language:
English
Subject:
75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND SUPERFLUIDITY; 36 MATERIALS SCIENCE; AMINES; CARBON; CRYSTAL STRUCTURE; INFRARED SPECTRA; MONOCRYSTALS; NUCLEAR MAGNETIC RESONANCE; STRUCTURAL CHEMICAL ANALYSIS; STYRENE; SULFONAMIDES; TOLUENE; X-RAY DIFFRACTION

Citation Formats

Liu, X.-G., Zhang, T., Hu, Y.-Y., and Shen, L., E-mail: shenchem@hotmail.com. Synthesis and crystal structure of (S, S, S, S)-N, N′-bis[N-(P-toluenesulfonamido)-1,2-diphenylethyl]ethylenediamine. United States: N. p., 2013. Web. doi:10.1134/S1063774513080063.
Liu, X.-G., Zhang, T., Hu, Y.-Y., & Shen, L., E-mail: shenchem@hotmail.com. Synthesis and crystal structure of (S, S, S, S)-N, N′-bis[N-(P-toluenesulfonamido)-1,2-diphenylethyl]ethylenediamine. United States. doi:10.1134/S1063774513080063.
Liu, X.-G., Zhang, T., Hu, Y.-Y., and Shen, L., E-mail: shenchem@hotmail.com. 2013. "Synthesis and crystal structure of (S, S, S, S)-N, N′-bis[N-(P-toluenesulfonamido)-1,2-diphenylethyl]ethylenediamine". United States. doi:10.1134/S1063774513080063.
@article{osti_22311405,
title = {Synthesis and crystal structure of (S, S, S, S)-N, N′-bis[N-(P-toluenesulfonamido)-1,2-diphenylethyl]ethylenediamine},
author = {Liu, X.-G. and Zhang, T. and Hu, Y.-Y. and Shen, L., E-mail: shenchem@hotmail.com},
abstractNote = {(S, S, S, S)-N,N′-bis[N-(p-toluenesulfonamido)-1,2-diphenylethyl] ethylenediamine (C{sub 44}H{sub 46}N{sub 4}O{sub 4}S{sub 2}), has been synthesized and structurally characterized by elemental analysis, {sup 1}H-NMR, MS, IR and single-crystal X-ray diffraction. The title compound contains four chiral centers with C atoms in S configuration. Molecules are connected to one another by hydrogen bonds between sulfonamide nitrogen and sulfonyl oxygen to form chains alone a axis.},
doi = {10.1134/S1063774513080063},
journal = {Crystallography Reports},
number = 7,
volume = 58,
place = {United States},
year = 2013,
month =
}
  • A new manganese(II) phosphate templated by ethylenediamine, (C{sub 2}H{sub 10}N{sub 2})[Mn{sub 2}(HPO{sub 4}){sub 3}(H{sub 2}O)], has been prepared by hydrothermal synthesis and characterized by single-crystal diffraction data and spectroscopic and magnetic techniques. The compound crystallizes in the monoclinic space group P2{sub 1}/n with a = 21.961(7), b = 9.345(1), c = 6.639(2) {angstrom}; {beta} = 91.06(2){degree}; V = 1362.3(6) {angstrom}{sup 3}; and Z = 4. The structure consists of anionic sheets of formula [Mn{sub 2}(HPO{sub 4}){sub 3}]{sup 2-}, being the charge compensated by ethylendiammonium cations. The sheets are constructed by edge-sharing MnO{sub 6} octahedra, MnO{sub 5} trigonal bipyramids, and hydrogenmore » phosphate tetrahedra. Within a layer, the edge-sharing octahedra and the trigonal bipyramids are linked in an alternating way, forming zigzag chains along the [001] direction. The ethylenediammonium cations and the water molecules are located in the interlayer space. The compound has been characterized by IR spectroscopy. A study of the compound by luminescence and diffuse reflectance spectroscopies is carried out. The Dq and Racah parameters have been calculated for Mn(II) ions in octahedral sites. The EST spectra at different temperatures of the compound show isotropic signals, with a g value that remains unchanged with variation in temperature. The intensity and the line width of the ESR signals increase continuously from room temperature to 4.2 K. Magnetic measurements from room temperature to 1.8 K indicate the presence of antiferromagnetic interactions. A value of J/k = {minus}0.75 K for the exchange parameter has been calculated by fitting the experimental magnetic data to a triangular lattice antiferromagnet of S = 5/2 spins.« less
  • A novel intercalated borate compound (NH{sub 3}CH{sub 2}CH{sub 2}NH{sub 3})B{sub 6}O{sub 9}(OH){sub 2}, has been solvothermally synthesized, and structurally characterized by single crystal X-ray diffraction. Compound crystallizes in the monoclinic, space group P2(1)/c, a=8.6200(17)A, b=15.656(3)A, c=8.8386(18)A, {beta}=93.32(3){sup o}, V=1190.8(4)A{sup 3}, Z=4. Its oxoborate structure is built up from 1-D polyborate chains with 3, 11-membered boron rings bonded diamine molecules through electrostatic attraction and hydrogen bond interactions to construct 2-D layered compound. Other characterizations by IR, element analysis, thermal analysis and specific surface area are also discussed.
  • The crystal structures of two new complexes of hexavalent actinides have been solved, and the uranyl and neptunyl complexes have been compared. The bond lengths in the equatorial plane have been found to decrease in the transition from uranium to neptunium.
  • An x-ray structural investigation of (Cu(H/sub 2/EDDIPH)H/sub 2/O) x H/sub 2/O, where H/sub 2/EDDIPH/sup 2 -/ denotes an acidic ethylenediaminedi(isopropylphosphonate) anion, has been carried out (lambda Mo K..cap alpha.., 1506 reflections, direct method, anisotropic least-squares method to R = 0.036). The crystals are orthorhombic: a = 6.685(1), b = 15.605(4), c = 15.159(4) A, Z = 4, space group Pbc2/sub 1/. The Cu atom has tetragonal-pyramidal coordination with two O atoms and two N atoms of the tetradentate ligand in the base and with the O atom of a water molecule at the apex. The bond lengths in the polyhedronmore » are as follows: Cu-O = 1.912(5) and 1.968(5) A, Cu-O/sub w1/ = 2.302(5), and Cu-N = 2.014(6) and 2.059(6) A. The molecules exist in a meso form. Each of the two terminal ionized oxygen atoms of the monoprotonated phosphonate groups serves as an acceptor in three H bonds of the O...H-O, O...H-N, and O...H/sub w1/-O/sub w1/ types (w1 denotes a coordinated water molecule) with an adjacent molecule, one of the H bonds being weakened. Two H rings are formed as a result. One is six-membered and is similar to the ring discovered in the structure of ethylenediaminetetramethylphosphonic acid. A comparison with the structure of the complex compound of H/sub 4/EDDIPH with oxonium cations has been made.« less