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Studies of the Torbernite Minerals (Ii): the Crystal Structure of Meta-Torbernitei

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Studies of the Torbernite Minerals (Ii): the Crystal Structure of Meta-Torbernitei THE AMERICAN MINERALOGIST, VOL. 49, NOVEMBER_DECEMBER, 1964 STUDIES OF THE TORBERNITE MINERALS (II): THE CRYSTAL STRUCTURE OF META-TORBERNITEI M.q.rcorrrRoss,2 H. T. EveNs,JR. AND D. E. Arereuaw, U. S. GeologicalSurwy, Washi.ngton,D. C. ABSTRAcT The crystal structure of meta-torbernite, Cu(UOrPODz.8HgO, has been determined and refined by three-dimensional least-squares analysis. The structure consists of infinite (UOrPOt""- sheets isostructural rn'ith those of meta-autunite(I) and abernathyite. Be- tween the sheets lie squares of four water molecules. Two of the four squares per unit ceII coordinate the two copper atoms. The other two squares do not coordinate a cation but are hydrogen bonded together in the same manner as those in the abernathyite structure. Each water molecule of the Cu(H:O)a squares is hydrogen bonded to a water molecule of an adjacent (HzO)a square and to a phosphate oxygen atom. Each water molecule of the (H:O)a seuares is hydrogen bonded to two other water molecules within the square, to an adjacent Cu(H:O)r water molecule, and to a phosphate oxygen atom. The copper atoms are also bonded to two uranyl-oxygen atoms; thus the coordination polyhedra about the copper cations is in the form of an asymmetrical tetragonal dipyramid. X-ray powder data for meta-torbemite are given. Unit-cell data for meta-zeunerite, Cu(UOzAsOr)z.SHzO, are also presented. IN'rnonucrroN In the first paper of this three-part series (Ross and Evans, 1964r hereafter referred to as Part I) the crystal structures of three members of the torbernite mineral group were given, namely those of abernathyite, NHa(UO2AsOa)' 3HzO, and K(H3O)(UOzAsOa)z'6HzO. The presentpaper (Part II) presentsthe crystal structure of a fourth member of this group, meta-torbernite, Cu(UOrPOn)r.8H2O.A general discussionof the tor- bernite minerals was given in Part I. In Part III of this series(Ross and Evans, 1965) the crystal chemistry of the torbernite minerals will be discussedin detail. Cnysrer-rocRApHy oF META-roRBERNrrE A sample of meta-torbernitefrom Schneeberg,Germany, (U. S. Na- tional Museum No. 84318) was used in the crystal-structure study. The crystals are clear, transparent, and bright emerald green in color. The optical propertiesare: uniaxial negative,u:I.626*0.002. The value of € was not determined becauseof the small amount of material available. No birefrigenceis evident in the plane of the plate. Spectrographicanaly- sis of this specimen (K. V. Hazel, analyst) showed >107o ll , t-\To P, 1 Publication authorized by the Director, U. S. Geological Survey. 2 Based on a dissertation submitted by M. Ross to the Department of Geological Sci- ences, Harvard University (19621 in partial fulfillment of the requirements of the degree of Doctor of Philosophy. 1603 1604 -41.ROSS, rI. T. EVANS, lR. AND D. E. APPLEMAN Cu, and O.14.57o Mn. No other elementswere detected. X-ray powder patterns (Daphne R. Ross, anaiyst) confirmed that the material is meta- torbernite. X-ray single-crystalstudies were made with the Buerger precession camera using zirconium-filtered molybdenum radiation. The spacegroup was determinedfrom the inspectionof the hkl, hkl, hkz, hk3, hk4, hks, 0fr1,and 1ftl photographs. The condition limiting the possiblereflections is: hk0:h*h:2n The hkl, hk3, and 2ft5 photographsshow distinct 4f m Laue s) mmetry. Thus the spacegroup is P4/n (No. 85). The 4/m Laue symmetry is not apparent inthe hkJ, hh2,hk+,0k1, and 1ft1photographs, and if only these were used for the spacegroup determination it would appear that meta- torbernite possesses4f mmm Laue symmetry and belongs in spacegroup P4/nmm (No. 129). As will be discussedlater, the strong pseudo-s1'm- metry is due to the fact that the uranium, phosphorus,copper, and uranyl oxygen atoms occupy special positions compatible with the higher 4f mmm symmetry. LII *-ray reflectionsare sharp, giving no indication of possible atomic disorder or mechanical distortion in the crystals. The unit-cell and optical data found for meta-torbernite in the present studl', the unit-cell data found for this mineral by Donnay and Donnay (1955), and the data of Makarov and Tobelko (1960) are compared in Table 1. The unit-cell data for the present study were obtained from a least- squaresrefi.nement of the *-ray powder film data listed in Table 2 using a program written by Evans et al. (1963). Donnay and Donnay observed the 4/m Laue symmetry but did not observe the weak 003 and 005 reflections and thus assumedthat meta-torbernite possesseda screw axis parallel to c. As a result they assignedthe space group P42f n. Makarov and Tobelko did not observe the 4/m Laue symmetry and thus assigned the space group PLf nmm to this mineral. The indexed c-ray powder data for meta-torbernite(U.S.N.M. specimenNo. 8431&)are given in'I'able 2. Cnvsrar Srnucrunn DerpnurNarrou A small tabular crystal measuring0.02 X 0.30X 0.42 mm, mounted with the thin direction parallel to the precessionaxis, was used to collect the hk}, hht, hkz, hk3, hk4, and 2ft5 intensity data. The thinness of the crystal in the c-direction minimizes the absorption error for these net planes (Donnay and Donnay, 1955). To collect the 0kl, lkl, and 2kl data, a pyramidal-shapedcrystal measuring0.05X0.06X0.10 mm was used. The hkl, hk3, and hkS photographs were made with unfiltered molyb- denum radiation; all others with zirconium-filtered molybdenum radi- M ETA-TORB ERN I T I] ST RU CT U RE Tenrr 1. X-nev nxo Oprrcer, Pnopnnrms ol MnrA-rcxeERNrrE. Cu(UOzPOr)g.8H:O Donnay and Makarov and Present studyl Donnay,1955 | Tobelko,1960 System Tetragonal Tetragonal Tetragonal o (A) 6.969+ 0.001 6.98 6.95 d (A) 17.306 + 0.005 17.4r tl.zo V (49 840.5 848.2 833.7 Z 2 2 2 LaueGroup 4/m 4/m 4/mmtn Space Group P4/n P$r/n P4/nmm Density, g,/cm3 (Obs) 3.40 3.79 Density, g/cm3 (calc) 3.70 J.O/ 3.73 c @ 1.626 Forms [100],[001] Locality Schneeberg, Cornwall, Germany England (u.s.N.M.84318) 1 The unit-cell edges were obtained from a least-squares refinement of the X-ray powder film data listed in Table 2. These values are in excellent asreement with the values o:6.963+0.00? A and c: 17.2g7+o.or8 A obtained from single-crystal patterns taken with a quartz-calibrated Buerger precessioncamera. ation. Lorentz and polarization corrections were applied to the observed intensities by means of a computer program based on the relations given by Waser (1951).No absorptioncorrections were made. The assumptionwas made at first that the structureof the (UOzpOn).^- sheetsof meta-torberniteis identical to that of the (UOzAsOs)^"-sheets of abernathyite(Part I). The four uranium atomswere placed tentatively in two 2c positions;two U at z:0.051, and two U at a:0.551 cyclesof space group P4/n. The four phosphorus atoms were placed in positions 2b and 2a. The 16 water molecules and the 16 phosphate oxygen atoms were placed in four eight-fold positions (8g) at coordinates equivalent to those given the water molecules and arsenate oxygens in abernathyite. The two copperatoms were placedin position 2c at z:0.815. This posi- tioning permits each copper atom to be coordinated by four water mole- culesso as to form squareplanar Cu(H:O)a groups.Thus, with the excep- tion of copper,the tentative structure was given atomic coordinatesiden- tical to those of abernathyite. Instead of first preparing Fourier projections, as was done with the previous compounds (Part I), it was decided to subject the proposed 1606 11. ROSS,H. T. EVANS, IR. AND D. E. APPLEMAN T.mln 2. X-nev Powoen Dera lon Met.q-toneenNrlrl I2 d(meas.) d(calc.)a hkl 12 d(meas.) d(calc.)s hkl 17.3r 001 1.940 r.937 2t7 20 8 71* 8.65 002 1.929 305 8 6.48 6.46 101 1.923 009 5 J./J J.ll 003 1.921 32r 5.44* 5.43 102 1 888* 1.886 322 15 4.93+ 4.93 110 |.873 226 4 1.70 4.74 111 1 859 315 4.M 103 1.854 109 IJ 4 .3t* 4.33 004 10 1.838t 1.839 208 4.28 tt2 1.833 323 3.747 113 10 1.809* 1.809 306 20 3.678+ 3.676 104 1.791 119 l6 3.480* 3.48+ 200 9 1.778 r.777 218 3.461 005 12 1.766* 1.765 \)L 3.416 201 t.751 3t6 3 25r lt4 10 1.743* 1.742 400 t6 3.232* 3.232 202 8 r.732 3.100 105 10 1.710+ 1.708 402 8 3.063 3.067 2lr 5 1.658+ 1.659 4t2 3 2.979 2.982 203 .5 1.642 t4 2.93t* 2.932 212 10 1.634* 1.633 11,1,0 2.884 006 6 1.616 2 2.84A 2.832 I l.) 9 1.605* 1.606 326 2.742 2r3 7 1.585 1.583 308 8 2.7t4* 2.7t4 204 10 1.575+ |.574 414 t4 2.667* 2.665 106 10 1.560 1.558 420 t4 2.529+ 2.529 214 12 1.544" 1.544 318 o 2.488* 2.489 1t6 o 1.535 2.472 007 6 1.459* 1.458 416 t2 2 462+ 2.464 220 6 l.M3 2.456 205 11 t.414 2.439 22r I 1 386 13 2.368* 2.370 222 6 l.J/o 2.330 to7 11 1.361 2.316 215 3 1.351* I .350 512 2.304 2.302 301 5 I.JJJ l CuKo raciiation, Ni filter (\:1.5413 A) Ca*e.a diameter: 114.59 mm.
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