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The Crystal Structure of Kiittigite

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The Crystal Structure of Kiittigite American M ineralogist., Volume 64, pages 376-382 , I979 The crystalstructure of kiittigite RonBRrcrJ. Hrrr' Department of GeoIogicalSciences Virginia PolytechnicInstitute and Slate Uniuersity B lac ks burg, Vi rgi nia 2406 I Abstract Kdttigite,(Zn2ooCoorrNio,n)(AsOn)r.8HrO, from the typelocality (Schneeberg, East Ger- many)crystallizesinspacegroupC2/mwitha:10.241(3),b:13.405(3),c:4.151(2)A,$: 105.21(2)",and Z :2. Isotypywith vivianiteis confirmed:the hydrogenatoms have been locatedand the crystalstructure refined using 812 Zr-filLered MoKa datato an R valueof 0.054(R. : 0.057).The transitionmetals are randomlydistributed over insular single and double(edge-sharing) octahedral groups of O atomsand HzOmolecules connected by AsO' tetrahedrato form complexslabs parallel to (010).These sheets are held together by hydrogen bondingalone, thereby accounting for theperfect {010} cleavage of themineral. Shortening of the sharededge relative to the unsharededges within the octahedraldimer (0. l39A) is well within the ratherwide rangeof valuesobserved in otherZn compoundscontaining shared octahedraledges. Introduction part of a continuing study of Zn stereochemistryand, in particular, of the characteristicsof Zn octahedron The mineral k6ttigite, ideally Znr(AsOn)r.SHrO, shared-edgeshortening. Material from the type local- has long been recognizedas a member of the vivian- ity in Schneeberg,East Germany, was kindly made ite group of minerals with the general formula available for study by B. D. Sturman of the Royal M,(TO4)2-8H,O. The monoclinic members of this Ontario Museum(ROM specimennumber M15537). family include the phosphatesvivianite (M : Fe), bobierrite (Mg), and bari6ite (Mg,Fe), and the arse- Experimental nateskcittigite, parasymplesite (Fe), hoernesite(Mg), The crystal selectedfor data collection was a pale annabergite (Ni), and erythrite (Co). In addition, red transparent platelet displaying well-developed both vivianite and parasymplesitehave been ob- faces,and having the dimensions0.098 X 0.093 servedin a closely-relatedtriclinic modification asthe {010} X 0.037mm. Detailed morphological,optical, chem- minerafs metavivianite and symplesite (Ritz et al., r974). ical and X-ray data for the material have been re- ported by (1976);the The topology of the monoclinic structuretype was Sturman chemicalcomposition determined in that study has been included in shown by Mori and Ito (1950)'zto consistof octahe- the abstract. The crystal was oriented with the axis dral edge-sharingdimers, MrO"(HrO)n, and insular c* slightly displacedfrom the axis of a Picker Fecs I octahedra, MO2(H.O)4, linked by ZOn tetrahedra @ four-circle diffractometer.Unit-cell parameterswere into complex sheetsparallel to (010). However, the refined by least-squaresmethods to give the best fit atomic coordinateswere not refined, and the details betweencalculated and observedangles 20, y, and of this interesting structure remain in doubt. The Q, measured at 25t2"C with MoKal radiation (tr : structure of the triclinic dimorph is still unknown. 0.70926A), for 30 automatically centered reflections The structural analysisof krittigite was initiated as in the range 20 : 30-45". The resultant cell dimen- : : : I Presentaddress: CSIRO Division of Mineral Chemistrv.P.O. sionsc 10.241(3)3,b 13.405(3),c 4.757(2)A,0 Box 124, Port Melbourne, Victoria 3207, Australia. : 105.21(2)' [unit-cell volume : 630.2(2)As]agree 'zNote that monoclinic FedAsO.),.8HrO is (incorrectly) re- well with valuesreported by Sturman (1976). ferred to as symplesite rather than parasymplesiteby Mori and Ito ' fl950). E.s.d.'s, given in parentheses,refer to the last decimal place. 0003-004x / 79 / 0304-0376$02.00 376 HILL: CRYSTAL STRUCTURE OF KOTTIGITE 377 Table 2. Fractionalatomic coordinates and temperaturefactor coelficientsfor kdttigite Aton 811or B Bzz Bgs Btz 8rg Bzt zn(t) 0.0 0.0 0.0 r-8(2) r_4(1) 102(8) 0 -2(3) 0 zn(2) 0.0 0.38521(9) 0.0 2L(L) 13(1) 1ls (6) 0 5(2) 0 As 0.31s41(9) 0,0 o.37 44 (2) 11(1) 11(r) 67(s) 0 -3(r) 0 o(1) o. 1498(6) 0.0 0.37 54 (L4) 15(6) 2L(4) 24(26) 0 -1(10) 0 o(2) 0.4049(7) 0.0 0.7226(L6) 32(7) 13(4) ro2(32) 0 -2(L2) o o(3) 0. 3432( 5) 0.1066(4) 0. 2135(t_2) 25(4) 11(3) r33(2L) 2(3) 10(7) s (6) o(4) 0.0975(5) 0.1144(4) 0.8081(12) 23(4) 22(3) 146(23) 0(3) 11(8) -2(7) o(s) 0,4000(5) 0,2262(s) 0. 717e(13 ) 42(5) 22(3) L4s (26) 3(4) 6(10) 7(8) H(41) 0. 384(10) 0. 42s(8) 0.364 (22) 2.1 (19) H(43) 0.340 0.37L 0.119 4.0 H(53) 0. 121(10) 0.30s(8) 0.436(24) L.7 (2o) n(s4) 0.044(8) o.236(6) 0. 289(19 ) 0.3(ls) * Thezrnal pazdneteys x LO+ for Zt, As mtd o. Pay,enthesized fifu?es here and in aLL subseqtent tables repreaent the e.s.d. in teyns of the Least significant figure to the Left. The H dtons ote identified bg tuo di'gits indicating the danor and. aceeptor o atons respectiueltJ. X-ray intensitydata for the structureanalysls were signed to Zn alone. Least-squares minimization of - collectedat25"C usingZr-filtered MoKa radiation (tr the function Zw(lF"l lnl;'zwhere F' and F. are : 0.71069A) and a 20 scan rate of lo per minute. the observedand calculatedstructure factors, and w Backgrounds were determined from l0-second sta- : l/o2, resultedin convergenceat a conventionalR tionary counts at both ends of each dispersion-cor- value of 0.069.At this point it was observedthat the rected(Alexander and Smith, 1964)scan range (mini- isotropic temperaturefactors of the isolated and di- mum width = 3.0o in 20). All reflectionsconsistent meric octahedralatoms were 0.98(4) and 1.05(3)re- with a C-face-centered lattice were collected to a spectively,indicating that there may be little if any maximum 20 value of 60o, using three reflections to difference in the chemistry of the two sites. Refine- monitor instrument and crystal stability at frequent ment with anisotropictemperature factorsa, incorpo- intervals: these showed no significant change. The rating the symmetry restrictionsof Levy (1956),fur- resultant 4045 reflections were corrected for back- ther reducedR to 0.059.The site multiplicitiesof the ground, Lorentz, polarization and absorption effects octahedralatoms were then released(R : 0.057)in a using a p value of 107.7cm-l (the transmissionfac- crude attempt to account for the presenceof Co and tors ranged from 0.402to 0.680).Multiply-measured Ni. The resultant occupancies of 0.951(9) and and symmetry-equivalent reflections (consistent with 0.947(8) are consistentwith the observedchemistry point group 2/m)werc averaged(using weights based and, furthermore, suggestagain that the three transi- on counting statistics)to yield a set of 962 unique tion metalsare distributedrandomly over the octahe- structure factors, each with a standard deviation esti- dral sites. The inclusion of an isotropic extinction mated from the equation o : [o1 + (0.02/')']o'u/2P", parameter as defined by Coppens and Hamilton where 1 is the corrected raw intensity and o 1is derived (1970)produced a value statisticallyidentical to zero, from counting and averagingstatistics. Of thesedata and the parameter was therefore removed from fur- only those 812 observationswith I ) 2o1 were in- ther consideration. cluded in the subsequentleast-squares refinement. A Fourier differencesynthesis utilizing only those data with sind/tr < 0.4A-' was computed,and peaks Location of the hydrogen atoms and refinement ranging from 0.45 to 0.62eA-3 were found for the Refinement of the heavy-atom positions and iso- four hydrogen atoms in the asymmetric unit. There tropic temperature factors was initiated in space were also a small number of other peaks with maxi- group C2/m, using the atomic coordinates deter- mum density l.06eA-s (less than 10 percent of the mined for parasymplesiteby Mori and Ito (1950). magnitude of an O atom peak), but these were all Although significant amounts of Co and Ni sub- located well within the coordination spheresof Zn stitute for Zn in type kdttigite from Schneeberg(Stur- and As and were interpreted as regions of charge man, 1976), the rather small differences in X-ray scattering abilities of the three atoms were ignored in n The form of the anisotropic thermal ellipsoid the initial refinements and octahedral sites were as- expl-(0,,hz + P22k2+ Bssl" + 20,2hk + z7,shl + 2l3,xkl)1. 378 HILL: CRYSTAL STRUCTURE OF KOTTIGITE Table 3. Magnitudes and orientations of the principal axes of atoms) were obtained from Internationql Tablesfor thermal ellipsoids in kdttigite X-ray Crystallography (1974) and were corrected for R.n.s. dlsDlace- Angle in degrees EO both real and imaginary anomalous dispersioncom- Atm Axis nent (i) +a t'b ft ponents. For H, the spherical scattering factor sug- 0.085(4) 44(5) e0 61(5) gestedby Stewart et al. (1965) was used. Programs 90 zn(l) 2 0.111(4) 90 180 utilized for solution, refinement,and geometrycalcu- J 0. r.19(5) 46(5) 90 151(5) lations were local modifications of Da.re.lrB,DATA- I 0.098(3) 39(6) 90 67(6) zt(2) 2 0.109(3) 90 180 90 soRT,FouRrER, ORXFLS3, ORrrr3 and ORrrp2?. J 0.118(4) 51(6) 90 ls7 (6) 1 0.067(3) 44(4) eo 62(4) Discussionof the structure As2 0. 098(3) 134(4) 90 28<4) 90 J 0.100(3) 900 Kdttigite crystallizes with the topology displayed 1 0.049(26) 81(23) 90 24(23) in Figure I and the bonding dimensionssummarized o(1) Z 0.091(r.9) 171(23) 90 66(23) 0.
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