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The Use of Electron Optical Methods To American Mineralogist, Volume 79, pages 426-437, 1994 The use of electron optical methodsto determinethe crystal structure of a modulatedphyllosilicate: Parsettensite R. A. Eccr.rroN Department of Geology, Australian National University, Canberra,ACT 2601, Australia SrrprrnN GuccnNrrnrvr Department of Geological Sciences,University of Illinois at Chicago, Chicago,Illinois 60680, U.S.A. Ansrucr The crystal structureof parsettensite,approximately Mi5(Mn,Mg)on(Siuo,,Alr r)":rrO,ur- (OH)ro'nHrO where M+ is an exchangeablecation such as K, Na, or Ca, was solved by trial-and-error methods basedon high-resolution transmissionelectron microscopy images and electron diffraction data. A simple tilting experiment was utilized to determine qual- itatively the magnitude of dynamical diffraction effectsfor reflectionsin a diffraction plane. Thus, it was determined that a kinematical approximation could be used, since dynamical diffraction effectswere minimized by using very thin grains and superstructurereflections streakedparallel to c* were not affectedsignificantly by orientation changesnear the (001) plane. Derived structural models of a single layer projected down c were compared with /rk Fourier transforms. The technique was capable of discriminating among models. A distance least-squares(DLS) refinement confirmed that the tetrahedral linkages are di- mensionally reasonable,and DlS-derived atomic coordinates are given. The ideal three- dimensional model conformsto C2/m symmetry with cell parameters,derived from X-ray powdermethods, of a :39.1(l), b : 22.84(5),c : 17.95(6),doo,: 12.56A, and B : 135.6(2y. Parsettensiteis a modulated 2: I layer silicate. It consists of a continuous Mn-rich oc- tahedral sheet coordinated by silicate tetrahedral rings forming islands three tetrahedral rings wide. Pairs ofislands are linked by inverted and partially tilted tetrahedra that form four-membered ring interisland connectors,with junctions of three islands forming also I 2-memberedring connectors.Layers are crosslinked through two setsof four-membered ring connectors(double four-membered rings). Although the tetrahedral island connectors are different from those in stilpnomelane, the tetrahedral islands are similar, which ex- plains the similarities in the diffraction patterns of the two minerals, as noted by earlier workers. INrnooucrroN stractspublished simultaneously by Ozawaet al. (1986) and Guggenheim(1986) showed that parsettensiteis dis- Parsettensiteis a poorly described Mn-rich hydrous tinct from stilpnomelane.Electron diffraction patternsre- phyllosilicatewith doo,equal to about 12.6 A. Irrtiitter vealing differencesbetween parsettensite and stilpnome- (1916)first presentedphysical, chemical, and opticaldata lane were publishedby Guggenheimand Eggleton(1987, for this mineral, but it was Jakob (1923, 1933)who ap- 1988)in papersgiving the systematicsof the modulated parently named parsettensiteand offereddetailed chem- 2:l layersilicates. Guggenheim and Eggleton(1987, 1988) ical and optical data for both parsettensiteand "errite." noted also that parsettensiteis similar to stilpnomelane "Errite" was later shown to be a variety of parsettensite in that both structures are modulated 2:l layer silicates with a light green color instead of brown-red (Geiger, with continuous octahedral sheetsand islandlike regions 1948),possibly caused by mixed oxidation statesofcon- ofideal tetrahedralsheets separated by inverted tetrahe- stituent Mn or Fe. Geiger (1948) presentedadditional dra. The doo,value of 12.6A suggeststhat tetrahedrain analysesand optical information and also provided an the interlayer spaceare joined along c through apical O X-ray study coupledto dehydrationexperiments. Geiger atoms. Mn-dominant stilpnomelane,however, has been reemphasizedthe possibility that parsettensiteis the Mn reported(Dunn et al., 1984, 1992),although the amount end-memberof stilpnomelane,which was suggestedear- of Mn doesnot greatlyexceed about half of the possible lier by Hutton (1938)on the basisof chemistryand poor- octahedralsites in the stilpnomelanestructure. quality Laue X-ray data. Ozawaet al. (1986) reportedthat parsettensitehas an More recently,Eggleton (1972) arguedthat the parset- orthohexagonal-basedcell with a : \/3b : 39.1, b : tensiteanalysis of Jakob (1923)does not conform to his 22.6, and doo,: 12.6A, and they suggestedthat the true proposedstructure of stilpnomelane.Subsequently, ab- symmetry is probably monoclinic. A prominent pseu- 0003-004x/94/0506-0426502.00 426 EGGLETON AND GUGGENHEIM: MODULATED PHYLLOSILICATE STRUCTURE 427 dotrigonalcell was reportedalso, with et : ez: 22.6 A Becausewe combine multiple proceduresto solve a parallel to the orthohexagonal b. From the hkl net, a very complex structure,it is important to understandthat sublattice was defined on the basis of the trigonal cell, the goal of this study is to outline the structure of par- wilh a,/7 and ar/1, and the superstructurecontains the settensite.Data werenot of sufrcient quality to refinethe ratio of 72 Si atomsto 49 octahedralatoms. Ozawa et al. structure. After obtaining chemical data, we proceeded noted also considerable stacking disorder. Guggenheim with a one-dimensionalpowder X-ray study to provide and Eggleton(1988, p. 723) presentedan indexedpowder initial information about the interlayer connectors.Such pattern based on lattice parametersof a : 39.47, b : information was enhancedby examining Cs-exchanged 22.18,c : 14.63A, B : 120.8". material also. This information and the electron diffrac- Parsettensiteoccurs at Val d'Err, Oberhalbstein,Grau- tion and high-resolutionTEM imagesallowed the devel- biinden, Switzerland,in metasedimentarymanganese ore opment of several models. These models were tested depositswith manganesesilicates and carbonates(Geiger, against limited electron diffraction data by using Fourier 1948)under low-gradeto very low-gradeconditions. Shear techniques.The best model, which consistedof crudely zonesshow evidenceoffluid circulation,with parsetten- determined atomic coordinates,was refined using dis- site commonly occurring in veins. In addition, similar tanceleast-squares (DLS) techniques.This techniqueuses material obtained for this study occursnear Chiavari and the topologyofthe proposedstructure and adjustsatomic Gambatesa,Italy. An abundant phase(White, 1987)from coordinateson the basisof assignedweighted interatomic the Foote mine, Kings Mountain, North Carolina, was distances;the proceduredid not involve any data from subsequentlyidentified as parsettensite(Guggenheim and parsettensitedirectly. The purpose of this step was to White, unpublished manuscript). In this occurrence,par- checkthat the topology was reasonableand to obtain more settensiteforms "spherical clustersof well-defined platy" realistic atomic coordinatesfor further testing of the best crystals(White, 1987)on surfacesof pegmatite,suggest- model. Using thesecoordinates, we calculatedhigh-res- ing either a hydrothermal or pneumatalytic origin. Par- olution TEM imagesand comparedthem in detail to the settensitewas describedalso by Sameshimaand Kawachi observed images.A companion paper (Guggenheimand (1991),in associationwith the Mn-rich zussmanitemin- Eggleton, 1994) provides further DLS calculationsfor eral, coombsite,from a Mn-rich siliceouslens in a very parsettensiteand stilpnomelane,since both structuresap- low-grade (pumpellyite-prehnite facies) metagraywacke pear to be related. and argillite sequencenear Otago, South Island, New Zealand.Sameshima and Kawachi (1991) indexeda cell Crmurclr, ANALYSTS usinga B angleof 95.6"and other cell parameterssimilar to thoseof Ozawaet al. (1986). Sampleswere analyzed(Table l) using a JEOL JSM- The purposeof this study is to determinethe crystal 6400 scanningelectron microscope (SEM) with an ener- structure of parsettensite,which has a complex super- gy-dispersive spectrometer (EDS). Operating conditions structure. Traditional structural analysis,however, is not included a l5-kV beam,a 40" take-offangle to the S(Li) possiblebecause samples are fine-grainedand impure. In detector,and a 90'incidence angleto the sample.A 20- addition, extensivestacking disorder makes the use of pm squareraster was used with a l-nA beam current. certain powder methods, such as the Rietveld method, Unlike sampleswith volatiles and some other cations inadvisable.Therefore, high-resolutiontransmission where heating by the electron beam produces a loss of electron microscopy (TEM) is used, along with other elemental concentration, a single spot beam showed in- powder X-ray diffraction techniques. creasingK concentrationswith time, indicating K move- It is generally recognizedthat electron dynamical dif- ment toward the beam. This is also consistentwith the fraction effectspreclude the possibility ofobtaining useful behavior of stilpnomelane.With further analysison a electron diffraction data for Fourier analysis, although singlespot, a loss of Si, Al, and Mn occurred.The rapid work by Soviet researchersusing only kinematical ap- deterioration of the sample using a single spot analysisor proximations(for a summary, seeDrits, 1987)appeared raster mode at sufficient beam current precluded the ac- successfulfor structural refinement procedures.We show curateuse of a wavelength-dispersivespectrometer (WDS). in this study a rapid procedureto determineexperimen- Table I presentscalculated formulae on the basis of 72 tally if dynamical effectsare insignificant, so that a struc- tetrahedral sites. All samplesshow a significant presence tural determination
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