Krishnaswamy, M

Ratho, T

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ON THE STRUCTURE OF COMPLEX SILVER QUINOLINE PERCHLORATET. RATHO ANn MRS. M. KRISHNASWAMYHK(JI0NAL F.NGINKKJUJSICi COLRK(;i:. J I ni'RR Kl.A {lUcc.hi'd iJacv.mbor H», I ‘.Mill)ABSTRACT. Tl»o Dobvo S clier ier p u tterii o f  Njivrr Q>mnnlim' ( Lav hcuaisUuliocl uMil a n a ly se d . T he unit d im o ii-in n s are fnund l,o lx- i f  -= ir> A , b  I I.IH A ,i:LOS A and p -= 07\47L There anj I’oui mnlecule^  n> the uml cell. 4’hc .-])are gnm}) a^ s^igiicd to the crx t^al.1 T K () \ y \  V  T 1 o  i\Silver Quinoline perchlorate Ag[C5jH,K|oCl()4 crystals ai*(‘ obtaina])lc in a inicrocrystalline form, white in coloui*. The study of crystal structure of these coniplex ligants throws light on their diamagnetic beliaviour. Tt is also possible  ^to know something about th(j stretching fori‘e constants betwt t^m tlu‘ various croups of atoms in th(*se‘ molecules. As it is not possil>lc to grow largt‘ (Tystals v(‘ hav(' tried to aiialyse tlu  ^ crystal by the wellknown powder nudliods.E X R 1 :\T E N T A('opper radiation from a Machlett A-2 X-ray diffraction tube vas made monochromatic by using a Ni fdttT. The a})])aratus was running at 20 m.A. and .‘$0 K.\". The finely powdid’ed speeimen was contained in a Lindtunann glass capillary of O.Ol mn\. wall thickness and of 0.5 nun diameter. The Debye Sciudrer pliotograph was obtairu’d in a Rigaku earncTa of 9 cm. diameter. Tin* time of (‘X]Kisur(’! was 4 hours. In the usual manner the intej’planar distances wt'ic cal- (ulated accurately. IVhdhods aj)plicabh‘ to the cubic, tc'tragonal and hexagonal systems were applied and the experimental data did not fit into any one of them. 'riuT(ifore the crystal does not belong to the higher symmetry class. Th(‘ J^ipson's method (1949), when tried, did not give a good number of constant diffei’ences. Therefore the most general method of Ito (1950) applicable to crystals of lower symmetry, namely, the monoclinic and th(  ^ triclinic Avas applied.The experimental data relating to the d values and the corresponding Q values Qhki) a-lso given in the table. All the six parameters werefound by using the Ito ’s method and tlie powder pattern was indexed after AzarolT and Bourgor (1958).We have after the above method of Ito,Qhki =  cos a * + 2AZc*a* cos/^*-f 2Aia *6* cosy*625116where a * * " , y *  and and c* arc the rcciproca] angles and axes res­pectively.The first two reflections of very weak intensity, aftta* some trials, could Ik taken as Qqoi seventh rt‘fleciion was taken as losing the aboveformula it was possible to find out the reciprocal cell dimensions. They area* =  0.066646* =  0.08397c* == 0.07714It then became necessary to examine the { h k o ) ,  (/?o/) and { o k l )  reflections lo select the reciprocal cell angles a*, /?* and y*. If a* and y ' weje taken to be 90 then { h k o )  and { o h l )  reflections could be detected. Th(a-(4’ore /y* was calculatro after studying pairs of { h o i )  and ( h d )  reflections after the equation612 T. Ratho and Mrs. M. Krishnaswamycos /y* j^hol~QhofThe value of/?* so found was 82""13'. Th(' dir(*ct cell dimensions are tlKTcfoiv obtained from th(\se six n^ciprocal parameters asa  == 15.15 A.U.b == 11.91 A.U.e 13.08 A. n. a  90"/y ^  97"’47' y -= 90"The above dimensions were found to b(^  tlu‘ nnluet'd omss after appljong the Buerger test (1958). The above data speaks about the monoclinic strueturc' oi the crystal. After indexing all the powder lines in the light of th(‘ above formula the following conditions for the appearance of the liiu's wen*, found.hkl—no conditionhoi—no conditionoko—k ~  2nThe possible space group, therefore, is P2]/w — (72/i^ * The observed density is 1.383 gms/cc. and the calculated density comes out to be 1.323 gms/cc. This gives four molecules per unit cell.TA BLEOn the Structure o f Complex Silver Quinoline^ etc. 13No. o f  linou In ten si ty ci A observed Q n k iconiputod Indioos1. vw 1 4 .99 0 .00444 0.00444 iOOo v w 12 .07 0 .00595 0.00595 001.3. R 8 .024 0 .0155 0 .0 16 0 1114. m 7.46:1 0 .0 18 0 0 .0178 2000 .0188 1115. s 6 .9 7 7 0 .0 20 6 0 .0209 2oT6. vv w 6. 511 0 .0 22 6 0 .0228 0027. vvw 5 .0 7 0 0 .0 28 0 0 .0282 0200 .0 28 0 2 nu s 5 .5 37 0 .0226 0 .0226 1200 .0225 112s .5.241 0.0264 0 .0260 2020.0272 127UK in 5.021 0 .0207 0 .0299 200i f . - 4 .8 0 0 0 .0422 0 .0420 212! l>. vvw 4 .6o:i 0 .0472 0 .0470 2100.0471 202J.i. vw 4 .2  i 4 0 .0527 0 .0526 0020 .0538 1020 .0527 1220.0541 21214. s 4 . i : u 0 .0 58 6 0 .0592 122ir>. 111 :i . 018 0.0651 0 .0612 222Hi, vw 3 .6 4 0 0.0751 0 .0754 1210 .0752 22217. w 3 .4 5 7 0 .0827 0.(»827 4020.0812 2270 .0826 222IS. m 3 .3 1S 0 .0 90 8 0 .0904 1230 .0912 2220 .0 90 8 41210. w 3 .2 37 0 .0954 0 .0952 004514 T .  R a i h o  a n d  M r s .  M .  K r i s h n a s w a m yT A B L E —contd .No. of linos Intensity -------7 1 ------- observed Qhklcom puted Indices20. m 3.077 0.1057 0.1052 1040.1060 3030.1062 4020.1062 33l21, w 2.975 0.1130 0.1128 0400.1123 1140. M.35 3310.1131 3130.1 130 41222. m 2.799 0.1276 0.1279 6l 222. v\v 2,663 0. 14 10 0.1413 40324 vvw 2.581 0.1501 0.1507 5130.1510 41425. vw 2.519 0.1576 0.1574 6oT0.1575 13426. m 2.436 0.1685 0.1678 305O 1687 1340.1682 34227. m 2.322 0 185 1 0.1854 5030 1852 15F0 1849 3420.1855 5140.1856 62128. w 2 214 0 2041 0.2047 43320. w 2.142 0.21H0 0.2180 1440.2180 35 l0.2188 3430 2187 44230. in 2.087 0.2295 0 2298 0630.2291 30631. w 2.034 0.2418 0.2424 0260.2411 5140.2419 63'4“32. w 1.962 0.2597 0.2598 0610.2600 4520.2689 41633. w 1.909 0.2746 0.2747 2610.2749 615TABLE—oont<l.0% the Structure of Complex Silver Quinoline, etc. 515tfo. of Intonsity d X <?/>«= 1/rf* Qhkl Indiceslinos observed (‘omputdHi34. vw 1.844 0.2942 0.2938 3600.2946 5050.2948 35435. vw 1.791 0.3118 n 3121 2360 3111 4350.3116 52036. vw 1.729 0.3.342 0.3335 2630 334S 3630.3,337 65l0.3344 64437 w 1.676 0.3.562 0.35,56 2640,3567 25538. vw 1.628 0.3775 0.3779 2640 3777 56 K 56239. 1.589 0 3958 0.3951 4630.3952 5260 3962 54640. w ] .5.59 0.4116 0 4112 66T41. vw 1.513 0 4372 0 4367 64642. V'W 1.469 0.4633 0.4634 3650,4632 045A f  K N O W I. E I) n M E N T SThe autliors wisli to express their indebtedness to the Lduealion Ministry, Govcrnnient o f India, for awarding a Research scholarsliij* to one of us (Mrs. M. Krishnaswamy). They are also thankful to Dr. D . \ . Raniana Rao and Mr. R. N . Patel o f the Dei)artnieiit o f Chemistry, for supplying us the pure sample used in this work.R E F E R E N r  E SAztiroff, L. V. aiid Buerger, M. .T., 1958,1‘ow:kr method. Me GrawHill, p. 100.It.<), T., 1950, X-ray studies in Polymorphinm. ^luiu/.c'ii, 'I’okyo.Lip.son, II., 1949, Act. Vryst., 2, 43.

On the Structure of Complex Silver Quinoline Perchlorate

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On the Structure of Complex Silver Quinoline Perchlorate

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