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Markascherite, Cu3(Moo4)(OH)4, a New Mineral Species Polymorphic with Szenicsite, from Copper Creek, Pinal County, Arizona, U.S.A

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Markascherite, Cu3(Moo4)(OH)4, a New Mineral Species Polymorphic with Szenicsite, from Copper Creek, Pinal County, Arizona, U.S.A American Mineralogist, Volume 97, pages 197–202, 2012 Markascherite, Cu3(MoO4)(OH)4, a new mineral species polymorphic with szenicsite, from Copper Creek, Pinal County, Arizona, U.S.A. H. YANG,* R.A. JENKINS, R.M. THOMPSON, R.T. DOWNS, S.H. EVANS, AND E.M. BLOCH Department of Geosciences, University of Arizona, 1040 East 4th Street, Tucson, Arizona 85721, U.S.A. ABSTRACT A new mineral species, markascherite (IMA2010-051), ideally Cu3(MoO4)(OH)4, has been found at Copper Creek, Pinal County, Arizona, U.S.A. The mineral is of secondary origin and is associated with brochantite, antlerite, lindgrenite, wulfenite, natrojarosite, and chalcanthite. Markascherite crys- tals are bladed (elongated along the b axis), up to 0.50 × 0.10 × 0.05 mm. The dominant forms are {001}, {100}, and {010}. Twinning is found with the twofold twin axis along [101]. The mineral is green, transparent with green streak and vitreous luster. It is brittle and has a Mohs hardness of 3.5~4; cleavage is perfect on {100} and no parting was observed. The calculated density is 4.216 g/cm3. Optically, markascherite is biaxial (–), with nα >1.8, nβ > 1.8, and nγ >1.8. The dispersion is strong (r > v). It is insoluble in water, acetone, or hydrochloric acid. An electron microprobe analysis yielded an empirical formula Cu2.89(Mo1.04O4)(OH)4. Markascherite, polymorphic with szenicsite, is monoclinic, with space group P21/m and unit-cell parameters a = 9.9904(6), b = 5.9934(4), c = 5.5255(4) Å, β = 97.428(4)°, and V = 328.04(4) Å3. Its 2+ structure is composed of three nonequivalent, markedly distorted Cu (O,OH)6 octahedra and one MoO4 tetrahedron. The Cu1 and Cu2 octahedra share edges to form brucite-type layers parallel to (100), whereas the Cu3 octahedra share edges with one another to form rutile-type chains parallel to the b axis. These layers and chains alternate along [100] and are interlinked together by both MoO4 tetrahedra and hydrogen bonds. Topologically, the structure of markascherite exhibits a remarkable 2+ resemblance to that of deloryite, Cu4(UO2)(MoO4)2(OH)6, given the coupled substitution of [2Cu + 2(OH−)]2+ for [(U6+ + ) + 2O2–]2+. The Raman spectra of markascherite are compared with those of two other copper molybdate minerals szenicsite and lindgrenite. Keywords: Markascherite, szenicsite, molybdate, copper oxysalt, crystal structure, X-ray diffrac- tion, Raman spectra INTRODUCTION sensors, solid-state electrolytes, and energy storage (e.g., Xu et al. 1999; Tian et al. 2004; Pavani and Ramanan 2005; Pavani et A new mineral species, markascherite, ideally Cu3(MoO4)(OH)4, has been found at Copper Creek, Pinal County, Arizona, U.S.A. It is al. 2006, 2009, 2011; Vilminot et al. 2006; Xu and Xue 2007; dimorphic with szenicsite (Francis et al. 1997) and is named after its Montney et al. 2009; Alam and Feldmann 2010; Mitchell et finder, Mark Goldberg Ascher, a mineral collector and engineer in al. 2010). In particular, lindgrenite has been synthesized under Tucson, Arizona. The new mineral and its name have been approved hydrothermal conditions for studies on its morphological archi- by the Commission on New Minerals, Nomenclature and Classifi- tecture, structural, and magnetic properties, thermal behaviors, cation (CNMNC) of the International Mineralogical Association and catalytic effects (Pavani and Ramanan 2005; Bao et al. (IMA2010-051). A part of the cotype sample has been deposited at 2006; Vilminot et al. 2006; Xu and Xue 2007). Furthermore, a the University of Arizona Mineral Museum (catalog 19291) and a triclinic Cu3(MoO4)2(OH)2 phase, dimorphic with lindgrenite, part is in the RRUFF Project (deposition R100030). has also been synthesized hydrothermally (Xu et al. 1999). In Hydroxyl copper molybdates are not common in nature. this paper, we describe the physical and chemical properties of In addition to szenicsite and markascherite, four other min- markascherite and its structural relationships with other hydroxyl erals may be classified into this category, including lindg- copper molybdates based on single-crystal X-ray diffraction and Raman spectroscopic data. renite Cu3(MoO4)2(OH)2, deloryite Cu4(UO2)Mo2O8(OH)6, molybdofornacite CuPb 2MoO4AsO4(OH), and obradovicite AMPLE DESCRIPTION AND EXPERIMENTAL METHODS 3+ S H4KCuFe2 (AsO4)(MoO4)5·12H2O. Despite their relative rarity in nature, hydroxyl copper molybdates have attracted considerable Occurrence, physical, and chemical properties, and attention recently owing to their promising applications in vari- Raman spectra ous fields, such as organic-inorganic hybrid materials, catalysts, Markascherite was found in material collected from the surface of the south adsorption, electrical conductivity, magnetism, photochemistry, glory hole of the Childs Aldwinkle mine in the Galiuro Mountains, Bunker Hill District, Copper Creek, Pinal County, Arizona, U.S.A. (lat. 32°45′07″ N and long. 110°28′55″). The south glory hole is the top of a breccia pipe. Associated minerals include brochantite, Cu4SO4(OH)6, on a brecciated quartz matrix. The * E-mail: [email protected] mineral is of secondary origin from the breakdown of primary molybdenite 0003-004X/12/0001–197$05.00/DOI: http://dx.doi.org/10.2138/am.2012.3895 197 198 YANG ET AL.: NEW MINERAL MARKASCHERITE –1 MoS2, bornite Cu5FeS4, chalcocite Cu2S, and chalcopyrite CuFeS2, all of which cooled CCD detector. The laser is partially polarized with 4 cm resolution are present in the south glory hole. Other minerals found in the south glory and a spot size of 1 µm. hole include antlerite Cu3(SO4)(OH)4, lindgrenite Cu3(MoO4)2(OH)2, wulfenite 3+ PbMoO4, natrojarosite NaFe3 (SO4)2(OH)6, and chalcanthite CuSO4·5H2O. X‑ray crystallography Markascherite crystals are bladed (elongated along the b axis), up to 0.50 × Because of the limited amount of available material, no powder X-ray diffrac- 0.10 × 0.05 mm (Fig. 1). The dominant forms are {001}, {100}, and {010}. tion data were measured for markascherite. Listed in Table 1 are the powder X-ray Twinning is found with the twofold twin axis along [101]. The mineral is green, diffraction data calculated from the determined structure using the program XPOW transparent with green streak and subadamantine luster. It is brittle and has (Downs et al. 1993). Single-crystal X-ray diffraction data of markascherite were a Mohs hardness of 3.5~4; cleavage is perfect on {100} and no parting was collected from a nearly equi-dimensional, untwinned crystal (0.04 × 0.05 × 0.05 observed. The calculated density is 4.216 g/cm3 using the empirical formula, mm) on a Bruker X8 APEX2 CCD X-ray diffractometer equipped with graphite- which is less than that calculated for szenicsite (~4.280 cm3) using data from monochromatized MoKα radiation with frame widths of 0.5° in ω and 30 s counting Burns (1998) and Stolz and Armbruster (1998). Optically, markascherite is time per frame. All reflections were indexed on the basis of a monoclinic unit cell biaxial (–), with nα >1.8, nβ > 1.8, and nγ >1.8. The dispersion is strong (r > (Table 2). The intensity data were corrected for X-ray absorption using the Bruker v). It is insoluble in water, acetone, or hydrochloric acid. program SADABS. The systematic absences of reflections suggest possible space The chemical composition was determined with a CAMECA SX50 electron group P21 (no. 4) or P21/m (no. 11). The crystal structure was solved from the direct microprobe at 15 kV and 20 nA. The standards used include chalcopyrite for method and refined using SHELX97 (Sheldrick 2008) based on the space group Cu and CaMoO4 for Mo, yielding an average composition (wt%) (13 points) of P21/m, because it yielded the better refinement statistics in terms of bond lengths CuO 54.99(47), MoO3 35.17(43), and total = 90.16(64). The theoretical content and angles, atomic displacement parameters, and R factors. The detailed structure of H2O is 8.61% from the ideal formula (see below). The resultant chemical refinement procedures were similar to those described by Yang et al. (2011). The formula, calculated on the basis of 8 O atoms (from the structure determina- positions of all atoms were refined with anisotropic displacement parameters, except tion), is Cu2.89(Mo1.04O4)(OH)4, which can be simplified as Cu3(MoO4)(OH)4. for H atoms, which were refined with a fixed isotropic displacement parameter (Ueq The Raman spectra of markascherite, along with those of szenicsite and = 0.03). The ideal chemistry, Cu3(MoO4)(OH)4, was assumed during the structure lindgrenite (RRUFF deposition R050146 and R060241, respectively) for refinements, because an exploratory refinement showed that all Cu sites were nearly comparison, were collected on a randomly oriented crystal from 9 scans at fully occupied, contrasting the slightly low Cu total from the electron microprobe 30 s and 200 mW power per scan on a Thermo Almega microRaman system, analysis. Final coordinates and displacement parameters of atoms in markascherite using a solid-state laser with a frequency of 532 nm and a thermoelectrically are listed in Table 3, and selected bond distances in Table 4. TABLE 1. Calculated powder X-ray diffraction data for markascherite Intensity dcalc h k l Intensity dcalc h k l 22 9.896 0 0 1 2 1.876 1 3 0 5 5.472 1 0 0 1 1.870 2 1 4 65 5.124 0 1 1 11 1.861 1 2 4 100 4.948 0 0 2 2 1.852 0 3 2 10 4.040 1 1 0 4 1.850 1 1 5 21 3.938 1 0 2 5 1.828 1 3 1 15 3.875 1 1 1 18 1.810 2 2 2 24 3.815 0 1 2 10 1.803 2 2 3 34 3.619 1 1 1 4 1.781 1 3 2 54 3.450 1 0 2 5 1.753 3 0 1 51 3.299 0 0 3 2 1.745 3 1 0 31 3.290 1 1 2 17 1.725 2 0 4 53 3.006 1 0 3 4 1.715 3 1 2 2 2.995 0 2 0 2 1.694 3 0 3 4 2.990 1 1 2 1 1.682 3 1 1 2 2.890 0 1 3 1 1.658 2 1 4 55 2.736 2 0 0 9 1.649 0 0 6 2 2.731 2 0 1 2 1.649 2 1 5 11 2.673 1 0 3 6 1.645 2 2 4 88 2.580 1 2 1 1 1.643 3 0 2 FIGURE 1.
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