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The Crystal Structure of Bobfergusonite T. Scott

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The Crystal Structure of Bobfergusonite T. Scott Canadion Mineralogist Yol.24, pp. 605-614(1986) THE CRYSTAL STRUCTURE OF BOBFERGUSONITE T. SCOTT ERCITI, FRANK C. HAWTHORNE ENOPETRIERNV Depafimentof GeologicalSciences, University of Manitoba, Winnipeg,Manitoba R3T 2N2 ABSTRAcT dant, Al et Fd+ sont ordonndsentre les chaines,ce qui donnedeux chaines distinctes en composition. Le deuxidme Bobfergusonite Na2Mn5Fe3+Al@O/6 is monoclipic, feuillet,identique d sonanalogue dans la wyllieite,contient F2r/n, witb, a 12.776(2),b 12.488(2),c 11.035(2)A, B deuxtypes de chainede polyddresd cationsX (Na,Mn) 97.21(l)", V 1746J(4) 13, Z:4. The crystal structure,a parallblesi X. Unechaine contient une alternance de poly- more highly ordered derivative of the wyllieite structure, tdresd Na et Mn d facespartagdes; I'autre contientexclu- was refined on the basis of a transformed wyllieite struc- sivementdes polyidres i Na d ar€tespartag4s. Ces deux ture, resulting in an R index of 3.8 Vo for 2889 observed sortesde chaine,qui ne sont pasentreJi6es dans le feuil- (3o) reflections measuredon a single crystal of red-brown let, lient les feuilletsde polybdresi cationsM aux tdtra€- holotype material. The structure of bobfergusohiteis topo- dresPO4. logicaly identical to tlat of wyllieite and alluaudite, but differs from both these structure types in terms of its M- (Traduit par Ia Rddaction) cation ordering. It is a layo structure, and has alternations of two types of layer along L One type of layer consists Mots<l6s:bobfergusonite, structure cristalline, phosphate, of M-cation (Mn,Fd+, Al) octahedral chains cross-linked wyllieite, alluaudite,mise en ordre descations. by phosphate tetrahedra. Each chain has intrachain AIt+ -IuIz+ ordering similar to that of the wyllieite struc- ItrnooucrIoN ture; however,unlike both the wyllieite and alluaudite struc- Ivre,s,ifiterchain ordering of Al and Fd+ occurs,result- BobfergusoniteNa2MnrFe3*Al(POr6 was disco- ing in two compositions of chain. The secondlayer of the ql. (L986) granitic pegmatitesof structure is identical to its counterpaxtin the wylliete struc- vered by Ercit et in ture, and consistsof two types of chains of X<ation (Na, the CrossLake area, Manitoba. The mineral is close- Mn) polyhedra that run parallel to X. One chain consists ly related to wyllieite-group and alluaudite-group of alternating, face-sharingNa and Mn polyhedra;the other minerals, yet differs from all known members of consists exclusively of edge-sharingNa polyhedra. These these groups both in chemistry and structure. The two types of chains are not cross-linked within the layer, chemistry, X-ray crystallography and optical and and serve to link tle layers of M-catiorl chains and POa physicalproperties of the mineral are describedin tetrahedra. Ercitet al. (1986).Because ofthe closerelationship of bobfergusonite to the wyllieite-group and Keywords: bobfergusonite, phosphate, crystal stnrcture, was necessaryto deter- wyllieite, alluaudite, cation ordering. alluaudite-group minerals, it mine the structureof the mineral as part of its charac- terization as a new species. SoMMAIRE ExpsmN4eNrAL La bobfergusoniteNa2Mn5Fd+AI@Of5 est monoqlini- que, P21/n, a 12.776Q\,b 12.488(2),c 11.035(2)A, P A cleavagefragment measuring0.18 x 0.29 x 97.21(l)", V 1746.7(4\ixt, Z:q. C'est un d6riv6 mieux 0.29 mm along its edgeswas used for data collec- ordonne du type structural de la wyllieite que l'on a affin6 tion. The fragment was selectedfrom red-brown sur un modele transformd de cette structure. L'affinernent holotype material of Ercit et al. 1986).Preces- pour @-1 a donn6un rdsiduR de 3.890 2889rdflexions obser- sion photographs confirmed the identity ofthe frag- v6es (3o) sur cristal unique du holotype rouge-brun. La ment as bobfergusonite and indicated it to be well structure est topologiquement identique i celles de la wyllieite et de l'alluaudite, mais diffbre de i celles-cidans crystallizedand single.Intensity data werecollected le degr€ d'ordre des cations M. La structure contient deux v/ith a Nicolet R3m automated four-circle diffrac- softes de feuillets en alternance le long de l. Dans un des tometer operating at 50 kV and 35 mA, using feuillets,des chalnes d'octaddres de cationsM (Mn,Fe3+, graphite-monochromatedMoKa radiation. Unit-cell Al) sont entre-lidespar dest6traddres de phosphate.A I'int€- paramelers for the crystal (Table l) were refined rieur d'une chalne, la mise en ordre des cp;liorlrslvF+ -luP+ from a subsetof 25 inteusediffraction-maxima used ressembleA ce que l'on trouve dans la wyllieite; contraire- in centring the crystal. A 20:Ascanning mode was ment alrx structuresde la wyllieite et de l'alluaudite, cepen- usedto collect the intensity data. Each scancovered a range of 2 20 plus the cv1-cv2separation, in 96 lPresenl address: Mineral Sciences Division, National steps.Scanning speeds were variable, ranging from Museum of Natural Sciences,Ottawa, Ontario KIA 0M8. 4"/min for weak diffractions to 29.3'lmin for in- 605 606 THE CANADIAN MINERALOGIST TABLE1. MISCELLANE0USINFoRIIArI0N FoR BoBFERGUS0NITE SfnUCfUnf ANALYSIS a 12.776(2)A Spacegroup P2\/n it was evident that the b r2.488(2) Crysial size 0.18x0.29x0.29m From the precessionstudy, . 1r nlqf2l ll, Radiatjon 44.5 cm-r, MoKo bobfergusonite structure is a more highly ordered B 97.21(1\ : Total Fo, obs. Fo 4204,2889 v r746.7(4)[3 Final R, wR 3.8,3.4g derivative of the wyllieite structure. The bobfer- from the wyllieite struc- 6"116e11qn15.(Z=4):. gusonite structure differs Naz.cllnq.aFe2', orFe3'. zgAl r.oCar gMg.oZn.oPo0z g.a0H.z* ture in having a doubled a period and the spacegroup R = t(lFol-lFcl)/tlFol P2/n, whereasthe wyllieite structure obeysP21/c = B=l wn Irw(liol-lFcl)'z/trlFol'?l'' @icit et at. L986).Comparison of the symmetry of a P2/c cell doubled along Xto the symmetryof a * for charge balance 0H:0 calculated P21/n cell of equivalentdimensions givestwo pos- sibilities for the origin of the bobfergusonitecell with reference to a wyllieite subcell: (0,0,0)ra and tensediffractions, and were adjusted automatical- (12,0,0,)w,where w refers to wyllieite. ly. Backgrounds were measured for half the scan Structure analysis was done with the program X time at the beginningand end of eachscan. Three in the STIELXTL package.Scattering curves for neu- standard reflections were monitored every 45 reflec- tral atoms from Cromer & Mann (1968) and tions for changesin beam intensity or crystal orien- anomalous-dispersioncoefficients from Cromer & tation. All such changes were insignificant. Data Liberman (1970)were used. A direct-methodssolu- were collected over I asylnmetric unit of reciprocal tion of the structure uniquely gave the origin as space,initially to sina/)r= 0.7035,but later only to (0,0,0)w, so that refinementwas initiated with this sin0/r: 0.5946,to reducethe mrmber of data. In all' setting. Co-ordinates for the wyllieite $tructure 4204reflections were collected, of which 2889were (Moore & Molin-Case 1974),transformed to com- consideredobserved (I>3o). ply with its P2r/c setting (Ercit et al. 1986),_were Subsequentto the collection of the main data-set, used as starting values for the refinement. For a additional intensity-data were collected on I I strong (0,0,0)w origin, the suppressionof certain symmetry- diffraction-maxima evenly dispersedover a range of ilements by the doubled'F21/cto P21/n transfor- 6to 53"?1.These data were collectedevery 10" while mation splitseachM-, P- and O-site,X(la) andXQ) rotating each reflection 360' about its diffraction of the parental wyllieite structure into two non- vector (ry'),using the sameset of scan parametersas equivalent sites;X(lb) remains unsplit but degener- the main collection of data. Thesery'-scan data were atis from a specialto a generalposition [seeMoore used as a calibration data-set by an empirical & Molin-Case (1974)for site nomenclatureof the absorption-correction routine in the SHELXTL wyllieite structurel. This resultsin 6Msites, 5 Xsites, packageof programs, a modification of the proce- 6 P sites arLd?llO sitesin bobfergusonite.The site dure of North e/ al. (1968).Absorption correction nomenclature adopted for bobfergusonite and its was done by assuminga pseudo-ellipsoidalshape for relation to the system used for wyllieite- and the crystal, and by refining the lengths and orienta- alluaudite-groupminerals (Moore & Ito 1979,Moore tions of the ellipsoid semi-axe$while holding p'R > L91l) are given in Table 3. constant.Absorption correctionreduced the merg- For early stagesof the refinement, a wyllieite-like iqg R of the ry'-scandata-set from 3.2 to l.6t/o. Data ordering schemewas assumed,and by using the non- reduction was done with a SIIELXTL program, and geneticmethod of Moore & Ito (1979)for the calcu- included background and L.P corrections, and scal- lation of the formula of wyllieite-groupminerals, ini- ing on the standard reflection-data. tial site-populations were assigned (Table 4). Becauseof the variable composition of bobfer- Subsequently,the total occupancyof eachM andX gusonite,the crystalused in the data collectionwas site was refined using mean scattering-curvesbased embeddedin an epoxy mount and was analyzedwith on the wyllieite-like model, while constraining the the electronmicrbprobe, using the sameanalytical temperaturefactors of the membersof eachsplit site techniquesas in Ercit et ul. (1986). The composition to be equal. is given in Table 2; the resulting formula given in Several cycles of refinement of the scale factor, Table I was used for the structure refinement. all positional and isotropic thermal parameterqand th; X- ard M-site occupanciesgave R indices of 9.0' weightedR 8.090.A differenceFourier map at this TABLE2. ELECTON-IIICROPROBEDATA ON BOBFERGUSONITT CRYSTAL stage showed two large loci of residual electron- sites,suggesting Naro Mgo cao l,4n! Feo zno Fe203 A1203 Pros H20 Total densityon oppositesides of the Xl strong anisotropic vibration for atoms of the site.
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