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Arizona Porphyry Copper Hydrothermal Deposits II: Crystal Structure of Ajoite

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Arizona Porphyry Copper Hydrothermal Deposits II: Crystal Structure of Ajoite Arizona porphyry copper͞hydrothermal deposits II: Crystal structure of ajoite, K ؉ Na)3Cu20Al3Si29O76(OH)16⅐ϳ8H2O) Joseph J. Pluth* and Joseph V. Smith* Department of Geophysical Sciences, Center for Advanced Radiation Sources (CARS) and Materials Research Science and Engineering Center, University of Chicago, 5734 South Ellis Avenue, Chicago, IL 60637-1434 Contributed by Joseph V. Smith, July 2, 2002 A crystal from the type locality Ajo, AZ, yielded just enough Many specimens in several museums were examined, and intensity from streaked diffractions using synchrotron x-rays at the finally the present specimen no. 159940 from the National Advanced Photon Source to solve the crystal structure with com- Museum of Natural History of the Smithsonian Institution was ៮ chosen on the basis of uniform slightly greener color and ؍ position (K ؉ Na)3Cu20Al3Si29O76(OH)16⅐ϳ8H2O; triclinic, P1, a fresher appearance’’ than other slightly bluer specimens. After‘‘ ؍ ␤ ,°(1)110.83 ؍ ␣ ,(7)14.522 ؍ c ,(7)13.687 ؍ Å, b (5)13.634 Electron examining many crystals, one was found that gave streaked .%12.5 ؍ refined to a final R ;(1)105.68 ؍ ␥ ,(1)107.21 microprobe analysis yielded a similar chemical composition that is diffractions with intensity just good enough to solve the main slightly different from the combined chemical and electron micro- features of the structure but with a poor agreement factor probe analyses in the literature. The ajoite structure can be de- (ϳ12.5%). The structure has Si͞Al and Na͞K disorder as well scribed as a zeolitic octahedral-tetrahedral framework that com- as poorly defined water molecules, and the agreement factor bines the alternate stacking of edge-sharing octahedral CuO6 reflects the poor crystal quality and is similar to those for layers and curved aluminosilicate layers and strings. Channels large-pore zeolites. It is likely that the other bluer ajoite crystals bounded by elliptical 12-rings and circular 8-rings of tetrahedra have undergone partial dehydration and rehydration that has contain (K and Na) ions and water. The Al atoms occupy some of damaged the regularity of the crystal structure. the Si tetrahedral sites. Each Cu atom has near-planar bonds to four Materials and Methods oxygen atoms plus two longer distances that generate a distorted ϫ ϫ ␮ 3 octahedron. Valence bond estimates indicate that 8 oxygen atoms A crystal of ajoite, 60 15 5 m , was mounted on the tip of ␮ of 46 are hydroxyl. Only one alkali atom was located in distorted a glass fiber tapered to 1 m. Data sets were collected at the octahedral coordination, and electron microprobe analyses indi- GeoSoilEnviro and ChemMat-Consortium for Advanced Radi- cate K and Na as major substituents. The water from chemical ation Sources (CARS) sectors 13 and 15 at the Advanced Photon analysis presumably occurs as disordered molecules of zeolitic type Source (Argonne, IL). The data set used in the refinement was not giving electron density from diffraction. The high R factor collected using radiation from a diamond (111) crystal at a results from structural disorder and many weak intensities close to wavelength of 0.56954 Å and focused using horizontal and detection level. The crystal chemistry is compared with shattuckite, vertical Rh-coated float glass Kirkpatrick–Baez mirrors to pro- duce a 100 ϫ 100-␮m2 beam. Data were collected using a Bruker Cu5(SiO3)4(OH)2, and planche´ite, Cu8Si8O22(OH)4⅐H2O, both found in oxidized copper deposits of Arizona but only the former directly 6000 SMART charge-coupled device detector at a fixed angle of 28° 2⌰ and frame widths in ␸ of 0.3° with a 2-sec counting time with ajoite. per frame. The charge-coupled device detector was mounted on a Huber 4-circle diffractometer with the ␻ axis of the diffrac- microcrystal ͉ microporous ͉ copper silicates tometer in the plane of the ring. Two full rotations of the ␾ axis yielded 1,200 frames with ␹ ϭ 0° and 1,200 with ␹ ϭ 270°. The ៮ ydrothermal ore deposits supply most of the copper plus symmetry is triclinic: space group P1. Unit-cell dimensions, a ϭ Hsignificant molybdenum, gold, and other metals important 13.634(5) Å, b ϭ 13.687(7) Å, c ϭ 14.522(7) Å, ␣ ϭ 110.833(11)°, for human welfare. Great advances in understanding the differ- ␤ ϭ 107.208(13)°, ␥ ϭ 105.680(10)°, were refined by least squares ent types of hydrothermal ore deposits have occurred over the using 863 reflections. Data were integrated and corrected for past three decades (1). In general, various granitic bodies intrude Lorentz, polarization, and background effects using Bruker the crust in continental margins and interiors that are composed software (SAINTPLUS). Systematic errors such as beam decay and of volcanic rocks and sediments. Hot brines of many chemical absorption were corrected with the program SADABS on the basis types (2) permeate the existing rocks to generate diverse mineral of the intensities of equivalent reflections. A total of 44,861 assemblages (3). This series of papers concentrates on the reflections was obtained from 3 to 58° 2␪; of the 18,567 unique ϭ porphyry copper deposits of Arizona. Paper I described the reflections (RINT 3.0%), 12,110 were classed as observed ͉ ͉ Ͼ ␴ crystal structures of chenevixite and luethite, two copper Fe͞Al ( Fo 4 F). The crystal structure was refined using SHELXTL 6.12, arsenate hydroxide minerals (4). This paper covers ajoite, a rare, F2, and isotropic temperature factors to a final R of 12.5%. When beautiful, blue-green mineral (5) that has challenged crystallog- scaled to Cu, the largest peak on the final difference Fourier was raphers for four decades. Structural relations in copper oxysalt ϳ3 electrons per Å3. Final atomic coordinates are shown in minerals are reviewed in ref. 6, and static and Jahn–Teller Table 1, and selected bond distances are shown in Table 2. chemical-bonding effects in Cu(II) oxysalts are reviewed in ref. 7. Electron microprobe analysis was done on four crystals with Ajoite occurs rarely in the oxidized zone of porphyry copper 5–8 analyses completed on a polished surface of crystalline deposits in Arizona (3). Type crystals are blue-green laths or fragments mounted in epoxy using standard wavelength- plates originally listed as monoclinic but now are known to be dispersive techniques and standards: K, asbestos microcline; Na, triclinic from x-ray diffraction study (8). The first sample for amelia albite; Si and Al, anorthite; and Cu, metal. The Si, Al, and chemical analysis (5) was believed to be contaminated with quartz, and a new combined chemical and electron microprobe *To whom reprint requests may be addressed. E-mail: [email protected] or analysis (8) is given in reference books. [email protected]. 11002–11005 ͉ PNAS ͉ August 20, 2002 ͉ vol. 99 ͉ no. 17 www.pnas.org͞cgi͞doi͞10.1073͞pnas.132391299 Downloaded by guest on September 29, 2021 Table 1. Atomic coordinates (؋104) and isotropic displacement Cu analyses were equal within experimental error, but the parameters, U,(Å2 ؋ 103) for ajoite average Na and K analyses for each crystal varied. Atoms per 20 xyzUCu atoms: K 0.20, 1.29, 0.23, and 2.15; Na 0.15, 0.65, 0.10, and 1.57; (Na ϩ K) add up to 0.35, 1.94, 0.33, and 3.72 atoms per unit. Cu(1) 905 (1) 2149 (1) 4795 (1) 6 (1) Because of ajoite instability in the electron beam (8), we decided Cu(2) 2917 (1) 1663 (1) 4821 (1) 6 (1) to prefer the conventional bulk analyses for alkalis and not to Cu(3) Ϫ3123 (1) 3137 (1) 4739 (1) 7 (1) Cu(4) Ϫ1117 (1) 2633 (1) 4739 (1) 7 (1) make electron probe analyses of the crystal used for x-ray Cu(5) 6937 (1) 674 (1) 4870 (1) 7 (1) diffraction. Cu(6) Ϫ5122 (1) 3618 (1) 4779 (1) 8 (1) Bearing in mind the evidence for half the bulk water being Cu(7) 4904 (1) 1143 (1) 4814 (1) 5 (1) zeolitic, the formula in ref. 8 was amended to give (K ϩ Cu(8) 8985 (1) 236 (1) 4971 (1) 6 (1) Na)ϳ Cu Al Si O (OH) ⅐ϳ8H O for bulk analysis. This as- Cu(9) 948 (1) 4663 (1) 4917 (1) 8 (1) 3 20 3 29 76 16 2 Cu(10) 2895 (1) 4106 (1) 4811 (1) 8 (1) sumes that one cation, K, fills the atomic site obtained from x-ray Si(1) 6643 (1) 3950 (1) 7006 (1) 5 (1) diffraction, and the remaining K and Na are located in the cavity Si(2) 701 (1) 3064 (1) 7035 (1) 5 (1) associated with water molecules. No doubt the alkali and water Si(3) 4619 (1) 4426 (1) 7031 (1) 7 (1) contents of ajoite vary from spot to spot depending on the salt Si(4) 2748 (1) 2604 (1) 7058 (1) 5 (1) content of hydrothermal brines during original growth and the Si(5) Ϫ713 (1) 4667 (1) 2873 (1) 6 (1) humidity after collection. Possibly ion exchange has occurred Si(6) 1296 (1) 4192 (1) 2741 (1) 8 (1) ϩ ϩ ϩ Si(7) 6719 (1) 1773 (1) 7118 (1) 5 (1) between K ,Na , and H . Si(8) 7100 (1) Ϫ524 (1) 2641 (1) 7 (1) Si(9) 5006 (1) Ϫ103 (1) 2554 (1) 6 (1) Results and Discussion Si(10) 8838 (1) 1424 (1) 7223 (1) 6 (1) The ajoite structure consists of alternating CuO octahedral Si(11) Ϫ2735 (1) 2659 (1) 2552 (1) 7 (1) 6 Si(12) Ϫ2213 (1) 602 (1) 1340 (1) 10 (1) sheets and SiO4 tetrahedral layers composed of chains and Si(13) 8941 (1) 292 (1) 8708 (1) 9 (1) strings.
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