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THE GRYSTAL STRUCTURE of MAWSONITE, Gu.Fe,Sns' J. T

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THE GRYSTAL STRUCTURE of MAWSONITE, Gu.Fe,Sns' J. T Canadian Minerologist Vol. 14 w. 529-535 (1976) THE GRYSTALSTRUCTURE OF MAWSONITE, Gu.Fe,SnS' J. T. SZYMANSKI Mineral Sciences Laboratory, CANMET, Department ol EnergX, Mittes and Resoutces 555 Booth Street, Qtr6tta, Canada A.rsrnecr INtnoPucrroN The crystal structure of mawsonite, Cu6FesSnS6, Mawsonite, CudFeaSnSe,was first described has been determined and refined to an R-value of by Markham & Lawrence (1965)' and idedified 0.049 (all 1426 d^ta) and 0.037 (1004 "observed" by them as being present in the material de- data only) from multiple sets of four-circle diffrac- scribed as "orange bornite" by Murdock (1916). tometer X-ray intensity data. Microprobe analysis The chemical composition has been variously indicates that the fonnula is stoichiometric in terms reported as CuzFeaSnSro(Marlfiam & Lawrence of tlre metals, but with l.SVo of tbe sulfur replaced 1965), 1967)' C\reFea by selenium in the specimen examined. The struc- Cus.urFer.eeSno.ssSe.soS-6vy ture is tetragonal, a 7.603(2), c 5.358(1)4, space SnSa (Springer 1968), and Cu:.aoFeSno.ssSe.oo (Kachalovskaya 1973). The more lecent group P4m2, based ccp sulfur et al, and is on a nearly & matrix with metals filling hall of the tetrahedral analysesof Petruk (1973) and of Yamanaka interstices and an extra interstitial Fe atom at the Kato (1976) are in agreement with the present (Yz,Vz,/z) position. The latter gives rise- to close analyses and with the present structural deter- Fe Fe . Fe contacts (2.679(1)A) in the mination. z direction, but no close Fe . Fe contacts normal Mawsonite powder ,patterns generally have to tbis. The deviations from an ideal ccp structure been indexed on a pseudo-cubic cell, a L0.74! are due to the large Sn atorn at the origin, and r/z,Yz,Yz. .014, but becauseof its anisotropic optical prop- the extra Fe atom at The bond lengths, (Mark- angles and thermal parameters are in close agree- erties, mawsonite cannot be truly cubic ment with those found in stannite, Cug(FeZn)SnSa, ham & Lawrence 1965). Recently, Yamanaka and kesterite, CudZn,Fe)SnSr. & Kato (1976) have indexed the mawsonite P1tr tern usins a tetragonalcell. a 1O.745,c I0.7llA. Sorvrtvrens Structu-ral exiittination' of mawsonite was in our laboratory, to provide ac- La structure cristalline de la mawsonite, undertaken Cu6Fe2SnS6,a 6t6 ddtermin€e et affin6e jusqu I un curate information on a metal-rich coPper-iron- indice R de 0.049 (pour toutes les 1426 donn6es) tin sulfide mineral, for comparison with the et de 0.037 (pour les 1004 donn6es "observ6es", related non metal-rich minerals, stannite and seulement) au moyen de plusieurs s6ries de don- kesterite (Ilall et al, 1975), in the same way n6es d'intensit6 recueillies sur diffractomdtre aux that the chalcopyrite series of minerals was rayons X i quatre cercles. L'analyse i la microsonde investigated (Hall 1975). In the latter series, indique que la formule est stoechiom6trigue en ce two metal-rich copper-iron sulfides, haycockite, qui que concerne les m6taux, mais 1.57o du soufie CuoFesSr,and mooihoekite, CueFee'Sre,w€fe both cotrtenu dans 1'6chantillon 6tudi6 est remplace par iron atoms filling additional du s6l6nium. La structure est t6tragonale, a 7.603(8), believed to have tetrahedral interstices,though it was difficult to c 5.358(1)A, dans le groupe spatial fim2; eTle cot- prove It was hoped that the siste en un assemblage quasi-cubique compact d'a- this unequivocally. tomes de soufre, dont les interstices t6tra6driques present investigation would indicate more clearly sont remplis pour moiti6 par les m6taux tandis the preference of iron over copper to occupy qu'un atome de fer suppldmentaire est interstitiel additional interstitial sites. en position (r/z,Yz,r/z'). Celui-ci donne lieu I de (2.679(l)A) courtes distances Fe . Fe . Fe ExPERTMENTAL dans la direction z, mais non perpendiculairement a cette direction. La structure s'6carte de la struc- Three single-crystal fragments of mawsonite ture id6ale i empilement cubique compact; deux were successively examined by microprobe atomes en sont la cause: le gros atome Sn,i I'origine 1/2,/z analysisand crystal structure determination. The et l'atome Fe en ,r/2. I.es valeurs des longueurs first two fragments proved to be too small for de liaison, angles des parambtres thermiques des et parameter concordent avec celles que I'on observe dans la an accurate refinement, though the stannite Cuz(Fe,Zn)SnSaet la kest6rite Cu{Zn,Fe) structure was solved using these dat4. The re- SnS,. sults of the third crystal structure determination, 529 Downloaded from http://pubs.geoscienceworld.org/canmin/article-pdf/14/4/529/3445798/529.pdf by guest on 25 September 2021 530 THE CANADIAN MINERALOGIST IABLEI. !4ICROPROBEA}IAlYSTs FOR I4AI{SONIIE TABLE2. CRYSTALDATA FoR l4Al,llsol{ITi, Cu6Fe2SnSs Elemt (mlcrtpmbe glven in Tabie l) speciren I Speciren 2 Speclmn 3 conposition: analysjs ldt.l Fomla ldt.% Foru'la I'lt.% Forola Source: (ldd Creek mine, Tinmlns, ontario 868.1 LU 43.2 5.89 4?.8 5.89 44.0 6.02 Fomula welght: '13.8 Sn I .01 13.8 1.01 13.7 l.0l crystal system: tetragonal Fe l3.l 2.02 13.0 2.03 12.9 2.02 systenatlc absences: none 29.8 8.07 29.2 7.95 ?8.8 7.83 Se 1.0 0.lt l.l 0.12 space group: (possibly) P422({891,P4m(*99), PA?rG1I1), P4nZ(#'l'l 51, P4/ m (#123) Total 99.9 100.5 P4nl2.(1115)confimd by structure analysis. Specl@n l. Hotukoveln, Kanaga*I Klnomlne, Hyogo Prefecture, - - Japon(Sol tisonlan Instl tute, SpEfu n rl 22102). Celt dtrensions: a 7.603(2), c 5.358(l)A at zO'Cusing Specluens2r 3: Kldd Creeknlne, Tlmlns, ont8rlo. r(Morol) - 0.709264 Llnear absorptlon coefflcient: lj(t'lorc) ' 160.3 cm-] on a mawsonite specimen from the Kidd Creek Denslty: rcalc - 4.659/cm-3iz' l mine, Timmins, Ontario, are reported here. (Density not rEasured) The microprobe analyses for the three maw- sonite specimens examined are listed in Table L. measured afrter The second and third were found to have a scan time. Three standards were a check on small but significant quantity of selenium re- every 50 reflections to maintain stability. A placing sulfur. This appears to be the first es- crystal alignment and instrument 4Vo of. tablished ocqurence of selenium in mawsonite. uniforrn systematic decrease of about was noted over The third specimen of mawsonite, after ex- the intensity of the standards as the crystal traction from a polished section, was cut with the period of data collection, and at the a knife, to provide more regular "faces" so as alignment was found to be unchanged procedure was applied to to facilitate subsequent absorption corrections. end, a linear scaling The resultant fragment was an irregular hexa- the data to account for this decrease. were applied to the gonal tablet 0.3X0.2X0.005 mm. Gandolfi Absorption corrections integration powder photographs of the single crystal were intensity data using a Gaussian the same as those previously published for maw- procedure, and the five equivalent segments sonite (Markham & Lawrence 1965), and con- were averaged and reduced to a single data intensi- tained no additional lines that could be attri- set which contained 1426 rndependent ob- buted to impurities. ties, of which 1004 can be considered as served at the LO% significance level, i.e. The crystal was mounted on a four-circle 1(net)21.65a(4.'fhe discrepancyfactor Cf,Af/ automatic diffractometer in a general orienta- among the five data sets was 0.031. tion. The cell dimensionswere determined from X4 a least-squares refinement of the 20, 1 and co Srnucrune Sor-urroN AND REFINEMBI{r angles @using 1970) for 90 reflections in tle range 55"q20<93". The parameterswere re- Examination of the cell dimensions suggested fined on a triclinic cell. The difference betweeu that the structure was based on two sphalerite- the a and 6 cell edgeswas less than 0.2cr, and tvpe 5.3A "cubes". with the tetragonal cell di- the maximum deviation from orthogonality was mi:nsion a, representingthe face diagonal of 'ocube". less than It of arc. The errors quoted in the the This reasoning imposed the condi- Table 2 represent 3cr as derived from the least- tion that the nearly ccp sulfur lattice would be squaresmatrix. Long-exposureprecession photo- approximately c-centred and would have Z sym- graphs, and diffractometer traces of weak axial metry about the c-axis (and hence about a line reflections showed that there were no systematic through the mid-point of the c-face). An added absences. Comparison of absorption-corrected condition for limiting the choice of spacegroup intensities of symmetry-related reflections was that, based upon the probable value of showed that the Laue symmetry of the lattice Z=t (i.e. one formula unit per unit cell to as- was 4/mmm and not 4/m. count for a reasonablevalue of D"n"), the space Five Friedel-equivalent segments of data, each group chosenwould have to have a site with an l/L6 of. the Ewald sphere, were collected using equivalent-position multiplicity of 1, where tin monochromatized MoKa radiation to a limit of could be assigned. Examination of the seven 2A=12O". The scan range was 1.9o plus the possible space groups for equivalent position cr-cvz dispersion, and the background counts sites that would yield an approximately ccp were measured on either side of the peak for sulfur lattice with normal S .
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