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Ulexite, Nacabsou(OH)R.Shro:Structure Refinement, Polyanion Configuration, Hydrogen Bonding,And Fiberoptics

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Ulexite, Nacabsou(OH)R.Shro:Structure Refinement, Polyanion Configuration, Hydrogen Bonding,And Fiberoptics American Mineralogist, Volume 63, pages 160-171, 1978 Ulexite, NaCaBsOu(OH)r.sHrO:structure refinement, polyanion configuration, hydrogen bonding,and fiberoptics SuBnnre GHosn, Cun'Nc WnN Department of Geological Sciences, Uniuersity of l(ashington S eatt le, Washington 98I 95 eNoJoeN R. Cmnx U. S. GeologicalSuruey,345 Middlefeld Road Menlo Park, California 94025 Abstract The crystalstructure of ulexite,NaCaBsOe(OH)6.5HrO, triclinic, PT. has been refined to a conventionalR:0.046 usingleast-squares methods, partially block-diagonal, for 49ll reflectionscollected on a single-crystaldiffractometer with graphite-monochromatizedMo radiation.AII l6 hydrogenatoms in theasymmetric unit werelocated, and all form hydrogen bonds.Refinedcellconstantsare:d=8.816(3),b=12.870(7),c=6.678(l)A,a:90.36(2)", B : 109.05(2)',7 = 104.98(4)",V : 688.4(4)A3,2 :2, density(calc) = 1.955g/cm3. The structurecontains isolated pentaborate-type polyanions composed of three tetrahedraand two triangles,plus chainsof Na octahedraand chainsof Ca polyhedra,all cross-linkedby polyanionbonds to thecations and by a networkof hydrogenbonds. Average bond distances (A) are:B-O, tetrahedrall.4T5,triangular 1.367; Na-O,2.421;Ca-O,2.484;hydrogen bonds, O-H 0.80,H . .O 2.08,O. .O 2.852.The octahedraland polyhedral chains are parallel to c, theelongation direction, and causethe fibrous habit of ulexitecrystals that is essentialto the opticalfiber bundles.The hydrogenbonds rangefrom strongwith a minimum O..'O distanceof 2.595(3)A to veryweak and possibly bifurcated with O. .'O distancesof 3.082(a) and3.194(3) A. The watermolecule environments are normal; each contacts at leastoneNa or Ca on its lone-pairside. Bond strengthscalculated using the observedO-H and H.'.O valuesagree fairly well with thoseobtained from an empiricalrelationship. A good cleavage parallelto {120},rather than to {010}as previously suggested, breaks hydrogen and Na-OH(5) bondsonly; a reproduciblefracture surface is parallelto {001}. Introduction by Weichel-Mooreand Potter(1963), who conclude their paper with the sentence"The discoveryand According to Dqna's Systemof Mineralogy(Pa- study of ulexiteshow that it is possibleto find in lacheet al.,195l, p. 345-348),ulexite has been recog- Naturea devicealmost as good as a man-made[opti- nizedas a validspecies since about 1840. Its formula, cal] fibre bundle." NarO'2CaO'5BrOs'16HrO, assignedby chemist Thecrystallography of ulexitewas studied by Mur- George Ludwig Ulex for whom the mineral was doch (1940)and reexaminedby Clark and Christ named,has been associated with the mineralalmost (1959),who alsogave indexed X-ray diffraction pow- as long. Ulexiteoccurs in saltplayas and dry saline der data. Clark and Appleman(1964) solved the lakesand hasalso beenfound associatedwith gyp- structure,but publishedonly a brief reportbecause sum deposits.Frequently it occursin bundlesof fi- the data weretoo numerousto be refinedeconomi- bers matted togetherto resemblea cotton ball, and cally at that time. Eventoday the dimensionsof the this habit is knownas "cottonballulexite." Less fre- structurerefinement are too large to be treatedeco- quentlythe fibers are oriented in parallelbundles that nomically by the usual [ull-matrix least-squares transmitan optical image with remarkableclarity method.In the presentwork with newdata, we have and resolution.This phenomenonwas investigated beenable to determineall the hydrogenpositions and 0003-004x/78l0 l 02-0 l 60$02.00 I 60 GHOSE ET AL.: ULEXITE Table L Crystallographic and optical data for ulexite below3o (/), whereo (/) is the standarddeviation of the intensity(1) as calculatedfrom the countingsta- Ctn1 e fnL Lo gr aphi c da t a, Optical data tistics.The intensitydata were corrected for Lorentz and polarizationfactors. No correctionswere made Triclinic, Pl Biaxial positive (+) for absorption(p : 29.73crn-t, MoKa) or extinction = (oH)6.5H2o1 Z 2 [NaCaBso6 effects.At the end of the refinement(see below) no = a 8.816(3)i a = r.asl ) seriousdiscrepancies between strong observedand b =I2.e1o(7) B=1.506>** c = 6.67A(Ll 'r = I.s2e I calculatedstructure factors with low 2d valueswere a:b:c = O.6850tl:0.5189 2V' caLc. = 79o found, indicating that there were no seriousex- o = 90.36(2). tinction effects. B = I09.05(2) . y = r04.98 (4) . 9p v = 688.4(4) i3 Hydrogenlocations and refinementof the structure Y 11 <o A10 I Constants for Cartesia Y 1000 2L.50 The structure-factorcalculation using the positions mtrices (Evils, 1948): z Lo7" 700 ul = -o.27564 I of non-hydrogenatoms, namely, one calcium,one = qo u2 0.96L23 vA. ,1 sodium,five boron, and seventeenoxygen atoms as Density: carc.=r.y)5gm- givenby Clark and Appleman(1964) yielded an R obs., Murdoch (1940), Theseatomic posilionswere refined = 1.9ss(1) factor of 0.18. with anisotropictemperature factors for Na and Ca *Nmber for B and O atoms in puentheses Ls-one stand4nd deoi,ati,m; fon and isotropictemperature factors 8.816(3) A, read 8.816!0.003 A, etc, to R : 0.088,using the full-matrixleast-squares pro- **1,1. T. Sehaller, u,S. ceoLogical Surnsey, mpubli,sled data, aterage of seua detezrmmtim. gramRnrNr (Finger, 1969). At thisstage the positions (1940) (1951). tlhudoeh ae gi.ua by PaTnche et aL. of sixteenhydrogen atoms were determined from a three-dimensionaldifference Fourier synthesis on the basis of peak heightsand reasonablestereochem- refinethe structuresuccessfully using partial block- istry. The positionaland isotropicthermal parame- diagonalleast-squares methods. We describehere the tersof the hydrogenatoms were refined next, keeping resultsof this refinement,interpreting the physical the positionaland thermal parameters of non-hydro- propertiesof the mineralin termsof its structure. genatoms constant, and the R factorwas reduced to 0.07.Unfortunately, due to the largedimensions of Experimentaldata the problem, further refinement-usinganisotropic The ulexite crystal used for the X-ray diffraction temperaturefactors could not be carriedout using experimentswas selectedfrom a specimenprovided the full-matrixleast-squares program. Hence, sub- by the late WaldemarT. Schaller,U.S. Geological sequentrefinement was carriedout by the Cnvmq Survey,who found the beautifulspecimen with a programincorporated in the X-nnv Svsrru (Stewart clusterof radiatingulexite needles at theBoron Mine, et al., 1972).The positionalparameters of all atoms, U.S. BoraxCorporation, Boron, California. A pris- anisotropicthermal parametersfor non-hydrogen matic crystal(0.12 X 0.20 X 0.28 mm) elongated atoms,and isotropicthermal parameters for hydro- parallelto c wasmounted parallel to the@-axis of the gen atoms (280parameters for 40 atoms)were di- single-crystal,automatic diffractometer for the deter- videdinto 24 blocks.Blocks I throughl3 contained mination of unit-celldimensions and collectionof Na, Ca, and O atomswith anisotropicthermal pa- intensitydata. MoKa radiation,monochromatized rameters,whereas each of the blocks 14 through 24 by reflectionfrom a graphite"single" crystal,and a consistedof an oxygenatom and the hydrogen(s) solid-statedetection system were used for the mea- associatedwith it, i.e., oneblock eachfor six (OH) surements.The cell dimensionswere refined by the groupsand five HzO molecules. methodof leastsquares, based on l5 reflectionswith The atomicscattering factors for Ca, Na, B, and O 2d valuesbetween 35o and 45omeasured on the dif- weretaken from Cromerand Waber (1965) and for H fractometer(Table 1). All reportedcell dimensions from Stewartet al. (1965).Anomalous dispersion for ulexiteare in reasonableagreement. The intensity correctionswere appliedaccording to Cromer and data werecollected by the 20-0 methodusing a vari- Liberman(1970). The observedstructure factors (F,) ablescan rate, the minimum being2" /minute (50 kV, were weightedby the formula l/o'(F"). The final ( - l5mA). All reflectionswith 2d 65owere measured, conventionalRfactor, R : >l l4l lF"ll/>lF"l, is yieldinga total of49l I reflections;ofthese, 1246were 0.045for all49ll reftections.0.041 for the 3665ob- t62 GHOSE ET AL ULEXITE Table2. Atomiccoordinates and thermalDarameters for ulexite a (iz)t C+m'at'n-1 Coordinatee* ThemaL ptrmet.r" roTe* a -eq, uzz utz uzg Ca 0,I422(L) 0. 0256(1) 0.3042 ( 1)l L.59 O.O2O20.0115(2) 0.0103(2) o.u-zs(2) 0.0020(2) 0.0017(2) -0.0003(1) Na 0.4774(I) 0. 501s(1) 0.2438(2)] 4.06 0.0514 0.0316(6) 0.023s(6) o.0266(5) 0.0100(s) 0.0096(5) 0.0012(4) B(1) central T 0.0506(3) o.2oo2(2) 0.668s (4 )l r.9r o.0242 0.012(1) 0. 012(1 ) 0.015(1) 0.00s6(9) 0.0016(9) 0.0009(9) B(2) r 0.3464(3) o.27OO(2) 0.8ee5(4)l 1.90 0.0241 0.013(1) 0,0r3(1 ) 0.013(1) 0.004(1) 0.0027(9) 0.0007(9) B(3) ^ -0.1891(3) o.2240(2) 0.782r(4)12.25 O.O28s 0.015(1) 0.015(r) 0.016(1) 0.007(r) 0.004(1) -0.0009(9) B(4) T 0,2344(3) o.0737 (2) 0.7834(4)j L.92 O.0243 0.013(1) 0. 01r(1) 0.01s(1) 0.0050(9) 0.0037(9) 0.0021(9) B(s) A -0.1737(3) o.2697(2) 0.4276<4)l2.10 O.0266 0.015(1) 0. 01s(1 ) 0.013(r) 0.006(1) 0.0021(9) -0.000s(9) o(1) T-A 0.1985(2) 0.2890(1) 0.7929 G)11 2.2L 0.0280 0. 0r23(8) 0. 0107(8) 0.0219(9) 0. 0043(6 ) -0.000s ( 7) -0. 0012( 6) o(2) T-I 0.1024(2) 0. 1066(r) 0.6208(2)lt.72 0,0218 0. 01rl (7) 0.0121(7) 0.0118(7) 0.00si (6) 0.00r1 (6) -0. 0008( 6) o(3) T-A -o.0289(2) o.2424(t) 0.4664(3 )l 2.4r 0.0305 0. 0r-38(8) 0.0180(8) 0.0141(8 ) 0.0087(7) 0.0039 (6) 0.
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