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Title: Synthesis, structure, growth and characterization of a novel organic NLO single crystal: Morpholin-4-ium p-aminobenzoate

Abstract

Highlights: ► A new organic NLO crystal morpholin-4-ium p-aminobenzoate has been grown for the first time. ► The structure is reported for the first time in the literature. ► Thermal, optical and SHG studies suggest its suitability for various NLO applications. -- Abstract: The title compound, morpholin-4-ium p-aminobenzoate (MPABA)(C{sub 4}H{sub 10}NO{sup +},C{sub 7}H{sub 6}NO{sub 2}{sup −}), has been synthesized for the first time by the addition of morpholine with 4-aminobenzoic acid in equi-molar ratio and good quality single crystals have been grown by solution growth technique using methanol as a solvent. The molecular structure of the compound was solved and refined by Direct Methods using SHELXS97 and full-matrix least-squares technique using SHELXL97, respectively. MPABA crystallizes in a monoclinic system with unit cell parameters, a = 5.948(5) Å, b = 18.033(4) Å, c = 10.577(5) Å, β = 90.40(1)° and non-centrosymmetric space group Cc. The experimentally measured density and chemical compositions were found to be in good agreement with the theoretical values. The phases and functional groups of MPABA have been identified and confirmed through powder X-ray diffraction and Fourier transform infrared (FTIR) studies, respectively. The thermal stability and decomposition details were studied through TG/DTA thermograms. The UV–visible transmission spectra weremore » recorded for the grown crystal and its NLO characteristic was explored by powder second harmonic generation (SHG) studies.« less

Authors:
 [1]; ;  [2];  [1]
  1. Department of Physics, Anna University of Technology Tiruchirappalli, Tiruchirappalli 620024 (India)
  2. X-ray Crystallography Division, Indian Institute of Chemical Technology, CSIR, Hyderabad 500007 (India)
Publication Date:
OSTI Identifier:
22215724
Resource Type:
Journal Article
Resource Relation:
Journal Name: Materials Research Bulletin; Journal Volume: 47; Journal Issue: 9; Other Information: Copyright (c) 2012 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved.; Country of input: International Atomic Energy Agency (IAEA)
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; CHEMICAL COMPOSITION; CRYSTAL GROWTH; DECOMPOSITION; DIFFERENTIAL THERMAL ANALYSIS; FOURIER TRANSFORMATION; HARMONIC GENERATION; INFRARED SPECTRA; LEAST SQUARE FIT; MOLECULAR STRUCTURE; MONOCLINIC LATTICES; MONOCRYSTALS; OPTICAL PROPERTIES; SPACE GROUPS; SYNTHESIS; X-RAY DIFFRACTION

Citation Formats

Shanmugam, G., Ravi Kumar, K., Sridhar, B., and Brahadeeswaran, S., E-mail: sbrag67@yahoo.com. Synthesis, structure, growth and characterization of a novel organic NLO single crystal: Morpholin-4-ium p-aminobenzoate. United States: N. p., 2012. Web. doi:10.1016/J.MATERRESBULL.2012.05.037.
Shanmugam, G., Ravi Kumar, K., Sridhar, B., & Brahadeeswaran, S., E-mail: sbrag67@yahoo.com. Synthesis, structure, growth and characterization of a novel organic NLO single crystal: Morpholin-4-ium p-aminobenzoate. United States. doi:10.1016/J.MATERRESBULL.2012.05.037.
Shanmugam, G., Ravi Kumar, K., Sridhar, B., and Brahadeeswaran, S., E-mail: sbrag67@yahoo.com. Sat . "Synthesis, structure, growth and characterization of a novel organic NLO single crystal: Morpholin-4-ium p-aminobenzoate". United States. doi:10.1016/J.MATERRESBULL.2012.05.037.
@article{osti_22215724,
title = {Synthesis, structure, growth and characterization of a novel organic NLO single crystal: Morpholin-4-ium p-aminobenzoate},
author = {Shanmugam, G. and Ravi Kumar, K. and Sridhar, B. and Brahadeeswaran, S., E-mail: sbrag67@yahoo.com},
abstractNote = {Highlights: ► A new organic NLO crystal morpholin-4-ium p-aminobenzoate has been grown for the first time. ► The structure is reported for the first time in the literature. ► Thermal, optical and SHG studies suggest its suitability for various NLO applications. -- Abstract: The title compound, morpholin-4-ium p-aminobenzoate (MPABA)(C{sub 4}H{sub 10}NO{sup +},C{sub 7}H{sub 6}NO{sub 2}{sup −}), has been synthesized for the first time by the addition of morpholine with 4-aminobenzoic acid in equi-molar ratio and good quality single crystals have been grown by solution growth technique using methanol as a solvent. The molecular structure of the compound was solved and refined by Direct Methods using SHELXS97 and full-matrix least-squares technique using SHELXL97, respectively. MPABA crystallizes in a monoclinic system with unit cell parameters, a = 5.948(5) Å, b = 18.033(4) Å, c = 10.577(5) Å, β = 90.40(1)° and non-centrosymmetric space group Cc. The experimentally measured density and chemical compositions were found to be in good agreement with the theoretical values. The phases and functional groups of MPABA have been identified and confirmed through powder X-ray diffraction and Fourier transform infrared (FTIR) studies, respectively. The thermal stability and decomposition details were studied through TG/DTA thermograms. The UV–visible transmission spectra were recorded for the grown crystal and its NLO characteristic was explored by powder second harmonic generation (SHG) studies.},
doi = {10.1016/J.MATERRESBULL.2012.05.037},
journal = {Materials Research Bulletin},
number = 9,
volume = 47,
place = {United States},
year = {Sat Sep 15 00:00:00 EDT 2012},
month = {Sat Sep 15 00:00:00 EDT 2012}
}
  • Graphical abstract: 1,3-Dimethylurea dimethylammonium picrate is identified as potential candidate for efficient frequency conversion. Research highlights: {yields} A new organic crystal, 1,3-dimethylurea dimethylammonium picrate, crystal has been grown for the first time and reported. {yields} The structure is reported for the first time in the literature. {yields} The high resolution X-ray diffraction curve (DC) measurements substantiate the good quality of the crystals. {yields} Powder test with Nd:YAG laser radiation shows a high second harmonic generation. {yields} Single shot and multiple shot (50 pulses) surface laser damage thresholds are determined to be 0.42 GW/cm{sup 2} and 0.31 GW/cm{sup 2} at 532more » nm laser radiation, respectively. -- Abstract: A novel noncentrosymmetric crystal was prepared from 1,3-dimethylurea dimethylammonium picrate, C{sub 11}H{sub 18}N{sub 6}O{sub 8} (DMUP), which was designed for second harmonic generation. DMUP crystals exist in noncentro symmetric space group Cmc2{sub 1} with unit cell dimensions a = 14.288(4) A, b = 17.023(5) A, c = 6.8268(13) A, {alpha} = {beta} = {gamma} = 90{sup o} and volume = 1660.5(8) A{sup 3}. The crystal structure of DMUP has been determined using single crystal X-ray diffraction studies. The single crystals of DMUP were successfully grown by the slow evaporation method with dimensions 10 mm x 4 mm x 3 mm using dimethylformamide as solvent. The structural perfection of the grown crystals has been analysed by High-resolution X-ray diffraction (HRXRD) rocking curve measurements. Powder test with Neodymium-doped Yttrium aluminum garnet (Nd:YAG) laser radiation shows a high second harmonic generation (SHG). The laser induced surface damage threshold for the grown crystal was measured using Nd:YAG laser.« less
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