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Synthesis, Crystal structure, Crystal growth and Characterization of 2-Amino-4-picolinium-4-chlorobenzoate

Subramaniyan Raja Ramakrishnan ,  Anandha Babu Govindan ,  Ramasamy Perumalsamy 

Centre for Crystal Growth,SSN College of Engineering,Kalavakkam,Chennai, Chennai 603110, India


2-Amino-4-picolinium-4-chlorobenzoate (2A4P4CB) has been synthesized by dissolving 2-amino-4-picoline (2-amino-4-methyl pyridine) and 4-chlorobenzoic acid in methanol in 1:1 molar ratio. Solubility studies were carried out in various solvents such as acetone, methanol, ethanol and mixed solvents to choose a suitable solvent for crystal growth. It is observed that 2A4P4CB has maximum solubility in acetone-methanol (1:1) solvent mixture when compared to other solvents. Single crystals of  2A4P4CB were successfully grown from the saturated solution by slow evaporation solution growth technique at the room temperature. Single crystal X-ray diffraction studies were carried out on the grown crystal to determine the crystal structure. 2A4P4CB crystallizes in monoclinic system with space group P21/c. The unit cell parameters are a = 9.520(5)Å , b = 11.499(5)Å, c = 11.445(5)Å, α = γ = 90º, β = 98.788º(5) and V = 1238.2(10)Å3 . Fourier transform infrared (FTIR) spectrum of 2A4P4CB was recorded in the region 400-4000 cm-1 to identify the functional groups. The optical transmittance and the lower cut off wavelength of 2A4P4CB have been identified by UV-Vis-NIR spectral analysis. These studies were carried out without any antireflection coatings. The lower cut off wavelength is found to be 367 nm. The thermal properties of 2A4P4CB have been identified from the TG/DTA studies. Microhardness studies were carried out on the grown crystal to measure the load dependant hardness. Indentation time is 5s. It is observed that the hardness number increases with the load which indicates that the reverse indentation size effect occurs in 2A4P4CB crystals   


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Related papers

Presentation: Poster at 17th International Conference on Crystal Growth and Epitaxy - ICCGE-17, Topical Session 7, by Subramaniyan Raja Ramakrishnan
See On-line Journal of 17th International Conference on Crystal Growth and Epitaxy - ICCGE-17

Submitted: 2013-04-15 10:44
Revised:   2013-04-15 11:55