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(1932) Has Described the Crystal Structure of Covellite As THE CRYSTAL STRUCTURE OF COVELLITE, CUSE AND KLOCKMANNITE, CUSC L. G. BBnnv, Q'ueen'sUniaers'ity, Kingston, Ontorio, Canada ABSTRACT The crystal structure proposed by Oftedal (1932) for covellite, CuS, is confirmed and found to hold also for klockmannite, CuSe. They are hexagonal with space group Dora- P6zfmmc; covellite with-a:3.796, c:16.36 A and cell content 6[CuS]; klockmannite, with o:3.938, c:17.25 A, and cell content 6[CuSe]. The atoms are in the following posi- tions: 2Cu in (d) t, 3, *; 25 or 2Se in (c) i,3, f ; 4Cu in (J) +,3, z, with z:0.107 in CuS and a:0.102 in CuSe; 45 or 4Se in (e) 002,with zs:0.064 and zse:0.066. Covpr,r,rrn Oftedal (1932)has describedthe crystal structureof covelliteas Hexagonal,D6f-P63fmmc; o:3.80, c: 16.4kX 2Cuin (d) i, 3, i; acr ir (fl *, l, z, with z : 0.107 25in (c) *, 3, i; aSin (e)0, 0, z,with z : 1! The lattice dimensions were taken from the earlier work of Roberts & Ksanda (1929)and Gossner& Mussgnug (1927). In order to check this structure in connection with the study of klock- mannite, a small cleavageflake (0.05X0.5X2 mm.) from the Leonard mine, Butte, Montana was mounted for single crystal study. Unfor- tunately it was not possible to obtain an equidimensional fragment be- causeof the perfect basal cleavageof covellite. Rotation and Weissenberg films with CuK (Ka:1.5418 A) and MoKa (0.7107A) radiation yietded the cell dimensions a : 3.796, c :16.36A Three sets of zero layer Weissenbergfilms, using three films in each set separated by brass foil, yielded intensity data for about ninety h}hl re- flections with MoKa radiation. The intensities, estimated by visual comparison with a standard seriesof graded exposures,were converted to lp,l values using the Lp factor and a scale factor (Table 1). The signs of the structure factors were calculated assuming Oftedal's struc- ture for covellite, and a two dimensional Fourier serieswas summed in a plane perpendicular to an a axis, using Patterson-Tunell strips. The resulting Fourier map showed high peaks at (?, -, ]) and (+, -, -b'f ) and moderate peaks at (+, -, t) and (0, -, -*&) The positions of these peaks correspond closely to the atomic positions given by Oftedal, the high peaks representing copper atoms and the moderate peaks sulphur atoms. 5o1 CRYSTAL STRUCTURE OF COVELLITE AND KLOCKMANNITE 505 Tesr,o 1. Cornr,r,rrn: Srnucrunn Fecron Dera lon xun h\hl, ZoNn h0.t h0.t 00.0 270 270 10.26 00 30.26 0 -5 00.2 t2 -r9 t0.27 74 30.28 11 11 00.4 IJ - IO 10.28 a -l 00.6 115 -148 r0.29 8 -3 40.0 0-9 00.8 49 63 40.1 t2 -8 00.10 0 -10 20.0 33 -23 40.2 14 t4 00.t2 24 30 20.t 24 19 40.3 22 -23 00.14 20.2 35 36 40.4 01 00.16 4t 36 20.3 64 58 40.5 69 00.18 29 13 20.+ 43 40.6 06 00.20 33 31 20.5 24 -22 407 16 14 00.22 43 -33 20.6 t7 16 40.8 27 -24 o0.24 24 -9 20.7 35 -33 40.9 o7 00.26 10 -9 20.8 58 -57 40.10 15 -8 00.28 2l 17 20.9 r7 -18 40 tl ro -lo 20.10 40.12 0-3 10.0 31 -35 20.11 37 38 40.13 7 -4, 10.1 28 -29 20.12 0-8 40.t4 20 19 10.2 46 54 20.r3 18 12 40.15 74 10.3 103 -88 20.14 37 40 40.t6 /J 10.4 85 20.15 t4 -9 40.r7 7tl 10.5 31 32 20.16 13 -24 10.6 24 23 20.r7 14 -24 50.0 0-5 r0.7 46 44 20.18 U5 50.1 04 10.8 69 -75 20 t9 07 502 08 10.9 23 25 20.20 8 -14 50.3 IJ IJ 10.10 27 -22 20.21 15 11 50.4 01 10.11 40 -49 50..5 n -q r0.t2 4 -10 30.0 9+ 89 50.6 04 10.13 18 -15 30.2 0-6 50.7 10 -8 10.14 34 50 304 t4 -6 50.8 t6 -r4 10.15 1a 1n 30.6 05 -oz 50.9 0-4 10.16 139 30.8 2+ 27 50.10 0-4 10.17 26 29 30.10 0 -5 50 11 10 10 10.18 06 30.12 t1 15 50.12 0-2 10.19 6-9 30.14 24 -30 50.13 03 10.20 18 -18 30 16 20 20 50.14 15 11 lo.2l 22 -13 30.18 157 'tn 'r7 04 30.20 917 60.0 r7 16 10.23 0-6 30 22 14 -t9 60.2 0 -1 r0.24 , -5 30.24 10 -5 60.4 0 -1 10.25 712 60.6 16 -r2 Structure factors, calculated for 0001and 1011reflections over a small range of the a parameters(a6o 0.107 to 0.110 and zs 0.0625and 0.064), L G, BERRY gave the best agreementwith lF,l in terms of the reliability index, R:ttl F,l- |e"ll/>l tr',1, when zcu: O.lO7 and ss : 0.064. Structure factors for all h\frl reflections within the range of observation, calculated with these parameters, were then corrected by a temperature factor. The temperature factor (8:1.84) was found by plotting log given lnl/l4"l as a function of (sin0/X)'z.The resulting F" values are in Table 1. The reliability index, R:0.22, indicates fairly satisfactory agreement between observed and calculated structure factors, consider- ing the unsuitable shapeof the cleavagefragment used for obtaining the intensity data. The data here confi.rm Oftedal's structure but indicate that a slight changein zg parameter is desirable. KrocruewwlrB The lattice dimensions and possible spacegroup of artificial CuSe are given by Earley (1949) Hexagonal,DsnLP6zf mmc; a : 3.938, c : 17.25A who also found that the x-ray powder patterns of klockmannite and artificial CuSe are identical. The natural material is unsuitable for single crystal study. The similarity of lattice dimensions and symmetry suggest that covellite and klockmannite are possibly isostructural. Earley's films show evidenceof the existenceof a superstructure in CuSe. A heavily exposedrotation film about the o axis shows weak difiuse rows requiring a twelve-fold a axis and the rotation about the c axis shows a few weak Iines of nearly continuous diffraction parallel to the Bernal curves. No further information about the nature of the superstructure could be obtained. In 1951 several students cooperated in calculating intensities for the 0001 reflections of klockmannite, using oftedal's atomic positions for covellite, over a range of values for the two variable z parameters. The observed intensities were estimated visually on Earley's original zero layer Weissenbergfilm, h\hl (.usingCuK radiation and a small thin hexag- onal plate of CuSe). On a graph of zcu against zseareas were eliminated in which the relation between each pair of calculated intensities is op- posed to the relation between the correspondingpair of observed inten- sities. This procedure leavesa small area in which the order of calculated intensities in decreasingmagnitude is the same as the order of observed intensities,here the parametervalues a:te'zcs: 0' 109and zse:0'068' The work was laid aside at that time when it was found that theseparameters result in rather poor agreement between calculated and observed in- tensities for 1011reflections. CRYSTALSTRUCTURE OF COVELLITE AND KLOCKMANNITE 507 Tear,E2. Kr,ocrurnrurrn:Srnucrunr FacronDere lor rw hjhl ZoNn h0.t h0-t h0.t I4l F" 00.0 378 378 10.9 20.8 74 -103 00.2 11 -8 10.10 36 -31 20.9 20 -5 00.4 0 8 10.11 34 -37 20.t0 33 -25 00.6 > 67 -235 lo.l2 36 -6 20.r1 21 29 00.8 40 40 10.13 37 -29 20.t2 30 -5 00.10 46 -53 10.14 86 90 20.t3 27 24 00.12 55 65 10.15 48 25 20.r4 59 73 00.14 28 -47 10.16 35 26 20.15 32 -20 00.16 81 78 l0.t7 023 20.t6 35 2l 00.18 0 8 10.18 017 00.20 20 33 10.19 0-2 30.0 o/ t37 00.32 61 -64 10.20 50 -36 30.2 4l -3 t0.2r 34 -22 30.4 42 A 10.0 46 t2 30.6 JO - 101 10.1 59 -56 20.0 469 30.8 2l 19 10.2 >69 110 20.1 50 39 10.3 M -62 20.2 51 77 40.0 24 4 10.4 0 -17 20.3 29 42 40.1 0 _17 10.5 13 8 20.4 16 -12 40.2 23 33 10.6 39 -6 20.5 0-6 40.3 19 -18 r0.7 54 67 206 37 -5 40.4 0 -5 10.8 70 -135 20.7 56 -50 40.5 0 2 40.6 13 The crystalline CuSe, made by Earley in 1946, now consists of sub- parallel aggregatesof tiny six-sidedplates. It is not possible to segregate a single plate large enough to mount.
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