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The Crvstal Strugture of Ailoclas

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The Crvstal Strugture of Ailoclas Canadian Mineralogist VoL 14, pp. 561-566 (1976) THE CRVSTALSTRUGTURE OF AILOCLAS|TE,GoAs$, AND THE ALLOCI.ASITE.GOBATTITETRANSFORMATIONO J. DOUGLAS SCOTT,8'$ exn W. NOWACKI Abteilung fiir KistaUographie und Strukturlehrq, (Jniversitiit Bern, Sahlistrasse6, CH-3012 Bern, Swilq,erland ABST.lrA-*CT muth as an essential constituent. Tschermak later concluded, however, that alloclasite was Alloclasite, CoAsS, crystallizes in the mono- not after all a distinct species but a bismuthian clinic space group P2r with lattioe constants d of ma- 4.661Q), b 5.602Q), c-3.411(1)1" p go.2(5)" z-2. variety of cobaltite. A re-examination mine, Full-matrix least-squares refinement of 600 ob- terial from the Elizabeth Oravicza, Rou- served reflections with anisotropic temperature fbc- mania (fschermak's type locality for alloclasite) tors and an ordered arrangement of As and S re- was made by Krenner, who concluded that tho sulted in an R factor of 0.029. The systematic ex- mineral was a high-cobalt glaucodot on the tinction of 00/ with / odd has been found to be basis of a new analysis which showed only structural in nature. Decause alloclasite has a 0.1/o Bi.In 1963 Polushkina & Sidorenko de- marcasite-type structure it may be readily trans- scribed a mineral, from an unnamed locality formed to either the ordered orthorhombic or the in the Tuva autonomous region, U.S.S.R., which disordered cubic form of cobaltite. The structure and powder pat- of ordered cobaltite was refined on the basis of an from their reported analysis absorption-corrected version of previously pub- tern is certainly alloclasite. They did not, how- lished data for purposes of comparison. ever, suggest this identification in their paper, feferring to the mineral as a structural variety Souuenr of cobaltite. Although the early literature on alloclasite L'alloclasite CoAsS cristallise dans le groupe casts considerable doubt on its validity as a spatial monoclinique P2r, avec constantes r6ticulai- distinct mineral species,its powder pattern was res: a4.66LQ), b 5.602(2),c3.411(l)4, p90"2(5),, sufficiently unique that Berry & Thompson Z-2. Sa structure cristalline a 6t6 affin6€ sur six (1962) mineral as a valid species cents r6flexions observ€es, par la m6thode des moin- included the dres carr6s i matrice entidre, avec coefficients d,a- in the Peacock Atlas. Subsequent work has gitation tlermique anisotrope et une mise en ordre tended to confirm its validity, although there de As et S, jusqu'i un r6sidu R de 0.029. L'ab- has existed considerable confusion about its senoe syst6matique de 001 avec I impair s'est av6r€e space group and symmetry. Polushkina & Sido- strusturale. Du fait que sa structure est du tylre renko (1963) suggestedunit-cell parameters and 'structural marcasite, falloclasite peut se transformer facile- the space group Pnnm for their menten I'un eou l'autre des formes de la cobaltite; variety of cobaltite' on the basis of a graphical orthorhombique ordonn6e ou cubique d6sordonn6e. indexing of their powder pattern by analogy A titre de comparaison, la structure de la cobaltite made no single- ordonn6e a 6t€, affinee au moyen de donn6es d6ji with that of marcasite, but publi&s, corrig6es oette fois pour les erreurs crystal studies of their material. Borishanskaya d'absorption. et al. (1965) reported an analysis and powder (fraduit par la R6daction) pattern for alloclasite from an iron-ore deposit at South Dashkesan, Azerbaydzhan S.S.R., and INTRoDUcTIoN suggestedthat it was a modification of glau- codot with a distinctive composition, intrinsis According (1929), to Krenner alloclasite was structure and optical properties, although again first named and described in 1866 bv G. no single-crystal work was done. The first re- Tschermak, who believed the new mineial to ported single-crystal study of alloclasite was be very glaucodot similar to but to contain bis- that of Kingston (1971), who used material from the type locality and defined the space group PZZrZt. Petruk et aI. *Contribution as Almost simultaneously, No. 289b. - Part 86 on sulfides and (1971) reported single-crystal data on alloclasite sulfosalts. from the 4th level, Silverfields mine, Cobalt, *'rPresent address: CANMET, 300 Lebreton St., Ontario, giving the space group P22L, More Ottawa KIA 0c1. recently, alloclasite analyses and powder pat- 561 Downloaded from http://pubs.geoscienceworld.org/canmin/article-pdf/14/4/561/3445845/561.pdf by guest on 01 October 2021 562 THE CANADIAN MINERALOGIST terns have been reported for material from lected using CuKcr radiation and the o-scan Bou-Azzer, Morocco (Johan et al. 1972\ and technique, for a crystal in the form of a tetra- from Lautaret, France (Maurel & Picot 1973); gonal prism inounted on a Supper-Pace auto- however, no further single-crystal studies have diffraciometer. The intensities were corrected been reported. for Lorentz and polarization effects and for The present study was undertaken in order to absorption, and then averaged to give 98 in- determine the true space group and crystal dependent observed reflections. structure of alloclasite, and to explain the na- All attempts to solve the structure in space ture of the structural transformation alloclasite- group P222r failed, even for severely disor- cobaltite (both with formula CoAsS). The same dered models. Because of the similarity in their specimen of type material as was used by cell parameters and their analogous composi- Kingston (1971) (USNM 62855, Elizabeth mine, tions, it was decided to investigate a possible Oravicza, Roumania) was borrowed from the relationship between the structures of allo- United States National Museum. As noted by clasite and costibite (CoSbS-Rowlatd et al- Kingston, this specimen consists of compact 1975). This would, require that all atoms of radiatirig bundles of alloslasite crystals in a alloclasite occupy 2(a) special positions in the blocky, white calcite gangue with minor inter- spacegroup Pn2tm. The extinction condition for grown wire gold; this description compares this. 0&/ absent for ft1l odd, was violated by favorably with that given by Krenner (1929) several reflections, which were therefore re- for his material from this locality. All results moved from the data set. Refinement of a given here were obtained from crystal fragments costibite-like model terminated at R-0.15 and selected from a single such bundle. gave unreasonably short Ce'As/S bonds. It was then noted that the well-resolved Patterson map ExPERIMENTAL could also be interpreted in terms of a Co-As/S octahedral structure in the space grolup Pzfim- The results of new microprobe analyses and Reflections of type ft01 with h+l odd were re- density determinations are given in Table 1, moved from the data set and the cell contents together with those reported by Kingston (1971) transformed to the new origin. Refinement of and Petruk et aI. (L97L). Weissenberg photo- a model in which Co was ordered with As plus graphs appeared initially to confirm the ortho- S statistically oceupying the other two sites rhombic space group F22t2t (0&0 absent for ft terminated at R=0.088. Five of the six Co-As/S odd, 00/ absent for / odd). The slight variation bonds. as well as the As/S-As/S bond, fell in occasionally observed befween h*l and hkl was the range 2.322 to 23464. The remaining attributed to absorption, as 4lR=14 for the Co-As/S distance ot 2.I9OA was, however, un- crystal used. Double-radius zero-level Weissen- reasonably short for an octahedral bond. berg photographs, calibrated with superimposed It appeared that this structure must be essen- Si powder lines, were taken in order to refine tially correct, even though it was not crystal- the unit-cell parameters on the basis of meas- lographically satisfactory, being in an obviously ured values of d for high-angle resolved re- incorrect space group. The atomic positions flections (program LAPA, T. Ito, unpublished); were therefore re-examined to determine the results of the final such refinement are given whether there was a possible monoclinic space in Table 1. group which would accept tbLeP2tnrn sites, re- A complete sphere of intensities was col- move the extinction condition imposed, and allow an ordered arrangement of As and S. TAELEI. AMI-YSESAI{D CELLPAMMEIERs REPOR'IED FOR ALLOCLASITE With a suitable origin transformation, the space Present rork Klngston(1971) Petruk at al.(197]), group P2r (second setting) fulfils these condi- and ta.t Ar* Ut.Z Ator6 vt,g Atom tions. The cobalt sites remain unchanged * * the four As/S sites may be split into a pair for Co 1.36 ,5A fr45 zb. a t.aa 6.7 0.38 8.4 0.49 6.0 0.36 each of As and S. The only extinction condi- NI 1.0 0.05 lr loo tion of Pzt (Ok0 with k odd) is already present, As 47.5 '1.98z.02 44.3 49.0 2,20 5 ro o 18.7 17.0 1.80 and therefore the condition of 00/ absent with / I00.2 96.8 9d. t odd must be,structural in nature. a 4.56r(2)1 4.64r 4.658 A second crystal, in the form of a trigonal b 5.6t2(2) 5.606 5.OZ I o 3.411(l ) 3.415 J.lv9 prism elongate [010] and bounded by {101}, ! 9002(5)' Space grlup F?.1 42121 il221 and {010} cleavagefaces z2- {10I}, {401}, {010}- o(reas.) 5.95(2) glfr 5.9I 5.02 (crystal volume O.I26X10* cm)' was se- ulihKo 28 wl lected for the collection of a new data set. In t*p" tt5^) this case monochromatized MoKa radiation Downloaded from http://pubs.geoscienceworld.org/canmin/article-pdf/14/4/561/3445845/561.pdf by guest on 01 October 2021 CRYSTAL STRUCTIJRE OF ALLOCLASITE 563 TABLE2.
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