Krishnaswamy, M

Ratho, T

English

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eiCRYSTALLOGRAPHIC DATA FOR COMPLEX COPPER LUTIDINE CHLORIDET. RATHO AiTD Mrs. M. KRISHNASWAMYK e q io n a ii J^^^rarKiiiniTNa CoiiLErtu, IIoutixeijA {Received A2>ril II, ]0(5G; Resubmitted Jane 1, li)G0) ^ABSTRACT. Dohyo iSdierrer ptiiiom of Ooppoi Lut.idniLi Chloride hns beljjr photo- giiiphod wil-h liho holp of Kig.iku <himoid. at. looin tomperoiiirori I ’lie 3'owdor diftiuoimu daba showed thut. the complex heloiigud to t,ho niutKiclinio Hyistem with o -- 13 7.T A, b -- 11 .70 A, 0 -  10 !JI A and fi — 103“1 1' 1’he number of moloculo.s per unit cell is 4. TJie svatomatio oxbiiicbions observed are ocmsistouti with the space grouii P' j^ Ivh—G s^ji or P'^i- Cz -^I N T R O D U C T I O NCopper Lntitline Clvloridc [Cu(C7//j,Ar)2Cl2l is obtainable in the microcryfllal- lino form, pinli in colour, and the diamagnetic propertic.s of such complexes using Lutidinc a.s ligand is of some interest. As it is not possible to grow large crystal powder method has boon resorted to, to investigate some of its crystallographic properties.K X  P K R I M  E N T A LWhen Cupric Chloride dissolved in Ethanol is treated with ethanolic solulion of Lutidinc, a shinning pink crystalline substance seperates out. This is the micro­crystalline complex compound of Copper Lutidinc Chloride.Filtered CuA„radiation was obtained from a Maohlett A -2 X-ray diffraction tube running at 16 , 30 K.V. and the siiccimen was contained in a Lindmannglass capillary tube of 0.5 mm. diameter, wall thiclmes.s 0.01 mm. The Debye ScheiTcr pattern of the substance was obtained on a photographic film using the Kigaku Camera of 9 cm. diameter. The time of exposure was about 12 hours.The intcrplanar distances were calculated from the measurements on the dif­fraction pattern with great accuracy. Attempts were made to index the powder lines in terms of cubic, tetragonal and hexagonal" systems.Since the observed data did not fit into any one of these systems of higher symmetry, the Lipson’s midhod (Lipson, 1949) was tried and this also did not give Bufiicicnt number of constant differences. This evidently shows that the crystal Iierhaps belongs to the lower symmetry group of monoclinic or triclinic systems Therefore it became necessary to apply either De Wolffe’s method (De Wolffe, 1957) or Ito’s method (Ito, 1950).570CrysUdlagraphic Data for Complex Copper, He. 5 7 7E X P E R I M E N T  A J, 1) A T AThe X-ray data oUaiued are given in Table II ,Si„„,. „]| (j,,, „„|;nonn parametera are to bo determined, the most general metliod of lie (Uo. I9o0) iraa applied.The powder pattern was indexed by Jto’s method (Tto’«, 11)50, A/oi iu’oirniul Buerger, 1958). The mtorplanar spaoings and the ooriespondino Q valiK's — a-ro listed in Table IIIn Ito’s method the expression relating sin2(9(9) to the cell constants of a triclinic cell isQhH =  h^a* -^\-h^h* -^{‘ l^c*--\-27db*c  ^ cos a*+27*?c*^0*008 /}*-\ 2hJca*h* cosy*where a*, /?*, y*  and a*, h* and c* arc the reciprocal angles and axes respectively.The first throe lines in Table II were first taken as andAttempts were made to index the othc»r lines Avith the above assumi)tion Smee it Avas not possible, the first three linos were talam again as andIt can be seen from Table I that the observed <?’s arc m good agroemoixt with the, calculated Q values for the other higlicr orders of reflection.TABLE ISelection of Qo^q, Qo2o> QooaQ, (^ ori'ocl-i»dQhkl Computed Ohsorved Ei'1‘!)1 id QQ'200 0 0227^400 0 0908 0 0891- 0  0017 _  _  40.2043 -Q02O 0.0202Oo40 0.11G8 0 1106, 0 0028 -1— -Qoao 0.2028 —O002 0.03465Oo04 0.1386 0.14181 0 0032 ^Qooa 0.31]8 0 31900.0072 +  ■" 9iVom Table I one gets the reciprocal cell dimensions+  0.0008 0 03545a* ^  0,0747 6* == 0.08648 c* =  0.094125 7 8 T. Eatho and Mrs, M. KrishnaswamyNow considering the Q values for planes hoi and hd with /?* ^  90°, we haveQhoi =  a* cos /?*=. /tVi*“+Z^c*2_2Mc*a*oos fi*.It is seen that these quantities are symmetrical with respect to the quantity Uy giving proper values to h and I, the two symmetrically placed linos hoi and hoi were found out. Then /?* was calculated fromCos . {Qhol Qhol)■ 4:C*am \This /J* was found out to be 76° 49'. The other two angles a* and y*  wero derived in the same way and they wei(i found to be a* =  90°, and 7 * — 90° Therefore the six parameters of the reciprocal cells arca* =  0.0747 a* =  90°b* ^  0.08648 /3* =- 76° 49'c* := 0.09412 y*  =  90°The direct cell ilimerisions are therefore a 13.751 a - -  90°& == 11.561 =  103° 11'c =  10 911 7  =  90°.The Biierger’s tost for reduced cell dimensions has been applied and the dimensions are found to be the reduced ones.TABLE II0. of 1IJ0BIntonsily d l Qm -  l/d2 observedQhHcomputedIndiooa1. VH 6 G36 0.0227 0 0223 2002. w 5.852 0 0292 0.0299 0200 0298 210n. vw 5 371 0 034G5 0 03545 0220 0355 1200.0346 1024. vvw 4.504 0.04799 0 0476 1210.0474 1025. w 4 222 0 0561 0.0569 3TT6. niH 3 773 0.0703 0 0706 2027. w 3 538 0.0799 /0.0797 f 003{0,0794 1 321'0 0801 I 32O8. H 3.350 0 0891 0.0892 4000.0896 2309, w 3 181 0.0988 0.0991 4020.0986 321Crystallographic Data for Complex Copper, etc,T A B L E  I I  {conid )5 7 9No.  of Tnl.onnil'y ii A Qm-i Quid lmlioi>K,linen ol>Hervticl r.ominitrcl10. w 2 892 0 1196 0 1 1 96 0400 1 1 92 42011. ms 2 756 0.1316 0 1311 32:r0 1309 14!12 vw 2 654 0 1418 0 MIS 0010.1420 2400 1420 11413. w 2 606 0 1473 0 1470 6100 M71 03314. ms 2 681 0.1.601 0 i5o;i 4020 1.502 2330 1504 51216. vw 2.506 0 1693 0 1688 30316. m 2 433 0 1690 0 1684 2240 1086 3330 1692 :ui0 1694 52017. vw 2.353 0.1806 0 1803 42218. vw 2 290 0 1907 0 1902 2420 190.5 60119. vw 2 261 0 1956 0.1954 1430.1959 05120. vw 2 187 0 2091 0 2091 0340 2090 4400.2093 26021. vw 2 180 0 2106 0.2111 1050.2103 63222. m 2 .104 0 2268 (I 2261 33323. m 1.998 0 2506 0 2603 44324. vw 1 .834 0 2972 0 2972 6230.2979 4510 2977 33426. vw 1 .770 0 3190 0 3191 0.31970063050.3195 3600.3191 3100 3188 3610.3194 55126. vw 1 .693 0 3486 0 3488 0.34900200630 3487 53627 vvw 1 676 0.3660 0 3607 32628. vw 1 642 0.3712 0 370436329. vw 1 .690 0 3966 0.395524630 w w 1 644 0.4194 0.41940.419060446231. w w 1 420 0.4898 0.4B992565 8 0 T. Mcdho and Mrs. M. KrishnaawamyThe crystal therefore belongs to the monoclinic system.Finally all the Qj i^ i^ values were computed using the above general formula. The powder pattern so indexed showed the following conditions. hJcl— n^o condition ; oko— odd absent.This obviously leads to the probable space group orThe observed density of 1.412 gms./cc. indicates 4 molecules per unit cell; calculated density is 1.372 gms./cc.Tt is however not possible to throw light on the complete structure of this substance. Further work on these lines is in progi’ess.A C K N O W L E D G M E N TOur thanks are due to Dr. D. V. Raman Rao, Head of the Department of Chemistry, fur supplying the chemically pure sample used in this work.H E F E 11 E N C JC BAzroff, L. V- and Duergor, M. .T , 10.^ )8, Powder Method, li50Doyo and Wait, 1960, X-ray Powder Photography in Jnorgamc Chemistry,Ito, T , 1950, X-ray studies in Polymorphism, Maruzon Tokyo,Lipaon, 11 . 1919, Acta Cryst, 2, i:i

Crystallographic Data for Complex Copper Lutidine Chloride

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Crystallographic Data for Complex Copper Lutidine Chloride

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