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Refinement of the Crystal Structure of Cuprosklodowskite, Cu[(UO

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Refinement of the Crystal Structure of Cuprosklodowskite, Cu[(UO American Mineralogist, Volume 60, pages 44845i, 1975 Refinementof the Crystal Structureof Cuprosklodowskite, Cu[(UO,),(SiOaOH),]. 6H,o' AsneHe[{ RoseNzwErc, Department of Geology, Oberlin College, Oberlin, Ohio 44074 eNn RorsRr R. RyeN Los Alamos Scientific Laboratory, Uniuersity ol CaliJomia, Los Alamos, New Mexico 87544 Abstract The structureof cuprosklodowskitehas beenrefined using three dimensional X-ray tech- niques.Thespacegroupis PIwith a:7.052(5),b =9.267(8\,c:6.655(5) A,a:109.2J.(5),6 : : : 89.84'(5),r I10.01'(7\,and Z 2.The structureconsists of sheetsof [(UOr),(SiOn)r]a-, formed by edge-sharingpentagonal-bipyramidal Uo, groupsand SiOntetrahedra, separaied by [cu(Hro)a]2+ions and Hro. The coordinationpolyhedron for cu2+ is a tetragonal bipyramidwith axialCu-O distance of 2.48A andan equatorialdistance of 1.97A. In theUO7 polyhedronthe axial distances are 1.77 A with equatorialdistances ranging from 2.29 to 2.43 A. ttre threeoxygen Si-O distancesin the SiOotelrahedron which areshared with UOrr+ions are 1.59,160, and 1.61A whilethe distanceto the unsharedoxygen atom is 1.67A,lending supportto the hypothesisthat the 2 protonsper formula unit, which are necessaryfor charge balance,are attachedto the unsharedsilicate oxygen. The structurewas found to containone watermolecule more than previouslyreported; the formulaCu[(UOr)dSiOrOH;r1 .6HrO is suggested. Introduction methods.Their solutionsupports the composition as given by Novacek,and establishedthe existenceof The mineralcuprosklodowskite was first described the fundamentalstructural unit as a sheetof com- (1933) by Vaes from theoxidized uranium ores ofthe position KUOr)r(SiOn)2lo-,essentially identical to Katangaregion. An occurrenceat Joachimsthalwas that foundin uranophane,CuO .2UOs.2SiOr.6HrO, independentlydescribed by Novacek (1935a)who asdescribed by Smith,Gruner, and Lipscomb (1957). named it jachimovite. The identity of the two The same structural unit was also found for mineralswas recognizedby both Novacek(1935b) sklodowskite,MgO.2UOs.2SiOr.6HrO (Mokeeva, andBillet (1936). Novacek (1935 a, b) determinedthe 1958,1964; Huynen and van Meerssche,1962). Ac- compositionto approximateCuO . 2UOs. 2SiO,. cording to the acceptedempirical formulasof these 6HrO.All of theseaurhors thought cuproklodowskite threeminerals, they are isostoichiometric,and prior to be orthorhombic,but thiswas questioned by Vaes to the deductionof their true symmetriesthey were andGuillemin (1958) and by Frondel(1958). Melon assumedto be isostructural.This early assumption and Dejace(1959) carefully studied the symmetry, may explainthe adherenceto the empiricalformulae morphologyand optical properties of cuprosklodows-eventhough the analysesfor waterare rarely in good kite and establishedthe symmetryas triclinicwith a agreementwith that stoichiometry. singleempirical formula in the unit cell. In all threestructures there is a questionofhow the The structureof cuprosklodowskitewas deter- formal chargebalance is to be accomplished.The minedby Piret-Meunierand van Meerssche(1963) to structuralunit, [(UOr)r(SiO4)r]n-,is balanced by only an R value of 0.14 by two-dimensionalprojection one divalentcation, thus requiringthe presenceof two additional positive charges in the form of I Work performed under the auspices of the U S. Atomic hydrogen ions as suggestedin the case of Energy Commission. cuprosklodowskite(Piret-Meunier and van Meers- CRYSTAL STRUCTURE OF CUPROSKLODOWSKITE 449 sche,1963) or hydroniumions (Smith et al, 1957; Tlsl-e l. Unit Cell Constants for Cuprosklodowskite Huynen and van Meerssche,1962), or by replacing eitheruranyl or silicateoxygen by hydroxyl(Huynen l4elcn & Dejace (1959) Pressrt $Iork and van Meerssche,1962; Mokeeva, 1958; Smith and Stohl, 1972).It was in the hope of illuminating a 7.04A 7.0s2(s)i thisproblem that therefinement of cuprosklodowskite b 9.18 9.257(8) c 6.66 6.655(s) was undertaken. 109. 23(5) ' The material used in this study was from the o r09.23" ' a 90.00" 89.84(5) Musonoi Mine, Kolwezi,Katanga, Zaire (formerly r L08.37" 110.01(7)" BelgianCongo), and was kindly supplied by William W. Pinch. Of these,I 143were considered observed according to the criterionI > 3o(I) where1 is the intensitycor- StructureRefinement rectedfor background,and o(1) : lT + B + [0.015(Z The crystal chosen for data collection was a - B)fzltpwhere 7 is the total countand B is the es- lathe-shapedcleavage fragment-I00 X 47 X 36 timatedbackground. Six boundingplanes were used microns-elongatedparallel to [00] andflattened on to define the crystal shape,and absorptioncorrec- the (010)face. tions were calculatedwith a linear absorption Lattice parametersand intensitieswere measured coefficientof p : 336 cm-' (Larson,Cromer, and usinggraphite monochromatized MoKa radiation(tr Roof, 1964). :0.70930 A) and a PickerFlcs-t diffractometer'The The positional parametersreported by Piret- lattice parametersobtained by refinementof twelve Meunierand van Meerssche (1963) were used directly high 20 reflectionsare in good agreementwith those in a least-squaresrefinement of thenew data. In their (Table l) of Melon and Dejace(1959) except for interpretation,all atomsare in generalpositions, ex- significantdifferences in the b-axis length and the cept for Cu2+and one oxygen-presumedto be a valueof 7. water molecule-which lie on centersof symmetry' A total of 1307unique reflectionswith 20 < 50o Sincethe originalstructure data included no thermal were measuredin a hemisphereof reciprocalspace. parameters,reasonable isotropic thermal parameters Tlst-r 2. Fractional Coordinates and Thermal Parameters (X l0') -12 R. Atom IJ LJ 27(1\ te(t) 3e(t) U 0.2589(r) 0.210(l ) 0.6397(l) 4t(1) 61(l) 57(t) 't78(6) At foI 45(lr) oola\ LU u.ctu/ o.s(o) 0(0) 158(7) 7e(4) 63(r2) 30(t3) 43(r1) Si 0.7735(s) 0.0s26(4)0.8573(4) 6e(8) 68(6) 3e(8) (16) (21 77(34) 23(37) 123(31) 0(1) 0.353(l) 0.235(1) o.6es(1) e5(24) lol rol ) 'l03(21 (1 l30(35) 45(36) l3l (33) o(2) 0.838(1) 0.1e3(l) 0.4r6(r) 73(23) 135 8) ) I47(33) 66(33) 8e(2s) 0(3) 0.s88(t) 0.024(1) 0.6e2( r ) e8(23) 125(16) 26(rB) l04(30) 41(32) 78(28) o(4) 0.s32(r) 0.018(l) 0.6e0(l) 60(2r) r08(15) 36(re) (2r l 18(36) 4l(41 ) 60(30) 0(5)(0H)? 0.863( l ) 0.248(1) 0.02r(r) 2OO(28) 84(15) 81 ) eo(2e) 23(31) 40(27) o(6) o.i2o(l) o.e4o(r) 0.002(l) 75(21) 88(14) 2e(1s) 18(37) -40(46) s3(32) 0(i) (H20) 0.465(1) 0.374(r) 0.te3(l) 248(31) 74(15) 144(?4) 'l78(33) I50(46) 206(68) 288(s5) 0(8) (Hzo) 0.231(l) 0.513(1)0.0s2(l) 131(20)574(48) 314(32) 94(48) 52(se) 124(4?) 0(e) (Hzo) o.zot(l ) 0.482(1) 0.4ee(1) 256(36) 173(22) Extinction paraneter = 2.3(5) x 10-o B's are defineduy expt-(hzBr,+ u2\r2* 02833+ Zhklrr+ 2ke'Brr+zh!'Brr)l 450 A. ROSENZWEIG.AND R. R. RYAN Tenlr 3. Observedand CalculatedScatterins Factors -6 -I2 -7 -6 -2 h=o l=-1 h=o t=o -:3.13 64 6C 52 s3 -1 \7 4? 3 79 79 tto IO9 4 3I St 2 24 25 -, s3so -e -r! , i :!,il,:! :i iA;; t:,:;,i: :;3;: ;i:iil3 : ff:: i:3:; -B c2 co -3 2i 2s -quzru -3;;;; ;;; s 9I6062-7I7Ia-iseso.3565?-29596-39gto2n=et=-si'iilii :::: li;;iff r 75 7s s s6 46 -? - h=\ L=3 : :1 :: 19 12 -r 50 s3 -2 ll4 rl{ -l 61 62 -z rqo rr2 3 ro4 ros -6 33 30 -5 7572 ; i!;; -it;T; -s6s66 _;;;;; I 9t9: -4 ;;i;; :ii;;;il-; ;ilil;-;;'i] _ro-re-l; : :: :: rs7 r58 i us oo o r1B r]8 , ;; ;i i;; i;; -; ;; ;; ; _; ;; ;; -i; -3 -3 : :: 2 66 61 I 38 39 2 9t 9t 5 c9 52 6q 55 6 68 68 8? 36 -8-16 ::::: "': -2re5res ;;i;; ;;;;; ;;;;i ;l;r; -,;);a ;il;: -;;;;; _;-i; -l -I1I2I10 3 2S 27 4 6A 69 ? 31 32 51 6q . -;;;; -6 52 h=o r= "? h'3 z=2 h=o 1.4 9 113lll ; ;; ;; ,--. ,-. s -r+ 7 o s2 ; ; -s 2q r 147 146 _7 56 52 5 t9 15 t 58 se _rt 33 28 I to2 ro2 -c b6 -: ::9] 3 toslo5 -s s? se 7 zq r7 3 \2 \2 3 os 84 -] q q6 :::: l55tss -4 4c s-t! 2 -r 1e <, 4 s? 5? -R !r !r 4 63 65 _, s 73 72 9 9: ]: -3 67 oe s 23 23 -6 62 63 _o s? 88 s 33 33 -7 94 9j 5 62 6t o sl 6 10 72 -2 1 :l :: 62 65 _s 88 ES _? 83 83 6 32 3r -6 3o 3l 6 33 32 f 7s 1 -r7 -r -ro : l" :: Ia s9 62 -q 80 79 -6 I29 I3o ? l0 -s li6 l2o 7 \2 36 2 9l 3 2c 25 o 42 40 o q6 50 -ro 39 39 -3 -5 -4 g5 102-ez ro2 a7 B7 h=3 Lr''u s6 h=4 z=-3 3 59 t: e -lr s r s9 so -e 60 s? -i-2 -4 -r-3 : :: -8 87 ee89 ee99 -ii102 -? rssls3 rbl16f -8 4 64 :il-l: r-o z=r! h=L L'-1t.-' 36 rs -r eo ii -s ii so sr -z rse isi 58 s? i I h=1 -7-t 51;i ;a -z-2 gq -6-b 44 {s -r -? s8 60 h=\ t-4 : ": -10 63 i6 os og ec siss ioo160 rsors6 -l -19 ? -6 38 39 7{ -r -s 6q 6s o e9 9? -6 09 eo -ro 23 I; -tOi; 19i: -9 :-, 19 r ?r 44 43 2s Eo 7! -I8 13 -5 61 61 2 4l q? O J3 j2 -4 4q 44 rt23129 -5 30 79 -9 5g 57 9 4t 3? -6- 6q 6q I 39 3e -q [5 43 s qi ce 5-r? ; -3 61 62 2 so oo -4 g9 Bs -s 56 5s -7 -2 -3 h=O t= -5 lI0 I09 2 37 40 -3 50 5t 1 -I9 29 44cq 45 3 87 39B9 69 66 -? a+ as -: -: i:i ,:: i ;3 ;; -3 'i i ',i Zi -i ;: ;: :: :: -1 li i: :,=',,'=,: h=2.' .,n.
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