Krishnaswamy, M

Ratho, T

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102ON THE DETERMINATION OF UNIT CELL DIMENSIONS FROM POWDER DIFFRACTION DATA OF COMPLEX SILVER LUTIDINE NITRATET. RATHO AND Mrs. M. KRISHNASWAMYBBGIOKAli ENOINBEBINOi COLLEGE ROUBKELLA“8.iNuikA.(Eeoeived M ay  25, 1967; E e ^ m iU e d  Deoemher 26, 1967).ABSTRAGT. Debye Scherrer pattern of fiilvor Lutidine Nitrate has been photographed using a Rigaku camera at room temperature. .The analysis showed that the crystal belongs to the orthorhombic system with 13.7 A ; 5=* 16.8 A and 7.12 A ; The unit coll contained four molecules. The spa<!e group P222 or Pmm2 can bo assigned to the crystal.I N T R O D U C T I O NSilver Lutidine Nitrate, Ag(C7H9N)2NOs is a white microorystatlline subs- tance whose dia-magnetic properties are of special interest. The crystallographic data was obtained from powder diffraction data.E X P E R I M E N T A LA Machlett A-2 X^-ay diffraction tube with copper target running at 30 K.V. and 20m.A. supplied the X-rays. The radiation was made monochroinatic by usme .  Ni filter. The epecimon. finely powdered, wu  eontoined m .  ghus onpillMy tube of 0.6 mm dimeter and of 0.01mm waU ftiokne®. The Debye Soherrer pattern was obtained in four hour, over a pbotographio film in a Bigakn oamera of 9 cm diameter.The interplanar distances were calculated accurately after measurements on the diffraction pattern and attempts were made to index the of cubic, tetragonal and hexagonal systems. Smee the data did not fit m with any of these systems, Lipson’s method (Lipson, 1949) was tried.Tba yatae. of Si.*d for the ring. In the powdar pattern aro m t ^ ^With tbteo valne. the differonoamethod. The firequently occurring values 0.00315, 0.00fatfeflw as the constants A, B and C respectively.( A A» . I f l* ’ A* .46*’871= ^  ) 4c* /872 T. Baiho and Mrs. M. Krishnaswam/yUsing the equation Sin®  ^=  Ah^+Bk^+Cl* and the above values ot A, B  and Cy all the rings were indexed quite satisfactorily.The axial lengths calculated from the values oi A ^  By G are a =  IS.tA, h =16.81 c =  7.I2I .The values of Sin®0, calculated with these axial lengths, the intensities of the lines on the Debye Scherrer pattern and the corresponding d spacing values are given in the table.As there have been no systematic absences the space group P222 or Pmm2 can be assigned to the crystal. I t  contains four molecules per unit cell. The observed density 1.5645gms./c.c. is in good agreement with the calculated density of 1.5535gms/c.c.TABLiG INo. of linesInton aity dA observed Values of Sin *6 IndicesObserved Calculated1. w 14.188 0.00295 0.00315 1002. s 7.384 0.01090 0.01139 1203. R 7.018 0.01207 0 01175 0010.01260 2004. 8 6.510 0.01402 0 01381 on5. V8 6.010 0.01645 0 01696 111C. WW 5.409 0.0203J 0.01999 0210.02084 2207. W 4.273 0.03255 0.03269 2210.03296 0408. m 4.088 0.03556 0.03611 1409. w 4.004 0.03709 0.03659 32010. ms 3.806 0.03998 0.04010 30111. 8 3.702 0.04334 0.04289 23112. vs 3.537 0.04749 0.04700 0020.04786 1410.04689 33013. w 3.387 0.05174 0.05160 0500.05221 11214. vw 3.222 0.05726 0.06731 24115. vw 3.083 0.06263 0.06215 40116. vw 2.969 0.06742 0.06784 22217. vw 2.896 0.07086 0.07039 42118. w 2.744 0.07817 0.07875 5000.07741 3120.07814 232Unit Gdl Dimension of Silver I/tdidine NitrateTable l —(contd).873No. of linesIntensity dA observedValues of Sin*^Obaorvoil Calculated Indices0.08124 0.08081 5100.08069 4310.08570 0.08591 0610.08922 0.08906 1610 0981.8 0.09850 0520.09851 2610.09874 6210.1079 0.10781 0130.1083 342o.m o 0.11714 1230.1248 0.12456 4600.12415 6010.12429 0330.12431 1620.1359 0.1363 4610.1362 3130.1425 0.1420 5510.1423 3230.1484 0.1489 4520.1625 0.1625 6120.1704 0.1699 2530.1785 0.1789 6320.18.54 0.1856 3530.1939 0.1934 6420.2000 0.2006 2040.1999 5620.2033 0.2030 5330.2161 0.2164 3040.2269 0.2274 6230.2363 0.2360 5530.2431 0.2427 1540.2516 0.2521 2540.2521 6430.2618 0.2622 0640.2755 0.2750 6240.2840 0.2863 6340.2909 0.2905 3640.3047 0.3061 1250.3238 0.3242 3150.3349 0.3344 6440.3480 0.3484 1660.3683 0.3579 25519.20. 21.35.36.37.38.39.40.41.42.43.44.45.46.47.48.49.vwrvwwvwvwvwvvwvwwwww2.7052.6452.58122. ms 2.46123. ms 2.34724. w 2.25426. ms 2.18220. w 2.09127. vw 2.04228. w 2.00129. w 1.91330. vw 1.86731. vw 1.82332. w 1.79033. vw 1.75034. vw 1.7241.70981.6581.6181.5841.5641.5401.5071.4691.4441.4291.3961.3551.3321.3071.288874 T. Batho and Mrs. M. Krishnasv)amyA C K N O W L E D G M E N T SThe authors wish to express their sincere thanks to the Education Ministry, Oovemment of India for awarding a Research Scholarship to one of them (Mrs. M. Krishnaswamy). Their thanks are also due to Dr. D. V. Ramana Rao and Mr. R. N. Patel of the department of Chemistry for making the pure substance available to them.B t E F E B E N C E SLipson, H. 1949, A ct. Ory»t. 2» 43.Azroff and Buerger—TAe Powder Method.

On the Determination of Unit Cell Dimensions from Powder Diffraction Data of Complex Silver Lutidine Nitrate

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On the Determination of Unit Cell Dimensions from Powder Diffraction Data of Complex Silver Lutidine Nitrate

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