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Robertsite, Ca2mniii3o2(PO4)3.3H2O

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Robertsite, Ca2mniii3o2(PO4)3.3H2O inorganic compounds Acta Crystallographica Section E Experimental Structure Reports Crystal data Online ˚ 3 Ca2Mn3O2(PO4)3Á3H2O V = 3777.7 (3) A ISSN 1600-5368 Mr = 615.94 Z =12 Monoclinic, Aa Mo K radiation a = 17.3400 (9) A˚ = 4.26 mmÀ1 III ˚ Robertsite, Ca2Mn 3O2(PO4)3Á3H2O b = 19.4464 (10) A T = 293 K c = 11.2787 (6) A˚ 0.07 Â 0.06 Â 0.06 mm = 96.634 (3) Marcelo B. Andrade,a* Shaunna M. Morrison,a Adrien J. Di Domizio,a Mark N. Feinglosb and Robert T. Downsa Data collection Bruker APEXII CCD area-detector 28397 measured reflections aDepartment of Geosciences, University of Arizona, 1040 E. 4th Street, Tucson, diffractometer 12635 independent reflections Arizona 85721-0077, USA, and bDuke University Medical Center, Box 3921, Absorption correction: multi-scan 9678 reflections with I >2(I) Durham, North Carolina 27710, USA (SADABS; Bruker, 2004) Rint = 0.037 T = 0.755, T = 0.784 Correspondence e-mail: [email protected] min max Received 13 August 2012; accepted 30 August 2012 Refinement 2 2 ˚ À3 R[F >2(F )] = 0.045 Ámax = 1.74 e A 2 ˚ À3 Key indicators: single-crystal X-ray study; T = 293 K; mean (P–O) = 0.006 A˚; wR(F ) = 0.107 Ámin = À1.09 e A R factor = 0.045; wR factor = 0.107; data-to-parameter ratio = 18.7. S = 1.02 Absolute structure: Flack (1983), 12635 reflections 5755 Friedel pairs 677 parameters Flack parameter: 0.676 (18) 2 restraints Robertsite, ideally Ca2Mn3O2(PO4)3Á3H2O [calcium manga- nese(III) tris(orthophosphate) trihydrate], can be associated Table 1 with the arseniosiderite structural group characterized by the Hydrogen-bond geometry (A˚ ). general formula Ca2A3O2(TO4)3ÁnH2O, with A =Fe,Mn;T = As, P; and n = 2 or 3. In this study, single-crystal X-ray DÁÁÁADÁÁÁA DÁÁÁADÁÁÁA Ow5ÁÁÁO25iii 2.792 (7) diffraction data were used to determine the robertsite Ow1ÁÁÁO17 2.964 (7) Ow6ÁÁÁO13iv 2.977 (6) Ow1ÁÁÁO33 2.889 (8) structure from a twinned crystal from the type locality, the Ow6ÁÁÁOw9ii 2.651 (7) Ow2ÁÁÁO33 2.815 (7) Ow7ÁÁÁO9v 2.768 (7) Tip Top mine, Custer County, South Dakota, USA, and to Ow2ÁÁÁOw8 2.655 (8) Ow7ÁÁÁOw3vi 2.645 (7) Ow3ÁÁÁO1i 2.957 (4) refine anisotropic displacement parameters for all atoms. The Ow8ÁÁÁO13 2.710 (8) Ow3ÁÁÁO17 2.821 (6) Ow8ÁÁÁOw1 2.635 (7) general structural feature of robertsite resembles that of the Ow4ÁÁÁO29 2.764 (7) Ow9ÁÁÁO12v 2.989 (7) Ow4ÁÁÁOw9 2.631 (8) other two members of the arseniosiderite group, the structures Ow9ÁÁÁO21vii 2.743 (8) Ow5ÁÁÁOw7ii 2.682 (8) of which have previously been reported. It is characterized by 1 1 1 1 Symmetry codes: (i) x þ 2; Ày þ 2; z þ 2; (ii) x; y; z þ 1; (iii) x þ 2; Ày þ 1; z; (iv) 1 1 1 1 1 1 1 sheets of [MnO6] octahedra in the form of nine-membered x; y À 2; z þ 2; (v) x þ 2; Ày þ 2; z À 2; (vi) x; y þ 2; z À 2; (vii) x; y; z À 1. pseudo-trigonal rings. Located at the center of each nine- membered ring is a PO4 tetrahedron, and the other eight PO4 Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT tetrahedra sandwich the Mn–oxide sheets. The six different (Bruker, 2004); data reduction: SAINT; program(s) used to solve Ca2+ ions are seven-coordinated in form of distorted penta- structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: Xtal- gonal bipyramids, [CaO5(H2O)2], if Ca—O distances less than 2.85 A˚ are considered. Along with hydrogen bonding invol- Draw (Downs & Hall-Wallace, 2003); software used to prepare material for publication: publCIF (Westrip, 2010). ving the water molecules, they hold the manganese–phosphate sheets together. All nine [MnO ] octahedra are distorted by 6 We are very grateful to A. R. Kampf and T. A. Loomis for the Jahn–Teller effect. providing the rare pararobertsite samples to the RRUFF project. Support of this study was given by the Arizona Related literature Science Foundation, CNPq 202469/2011-5 from the Brazilian For information on the arseniosiderite group minerals, see: government, and NASA NNX11AN75A, Mars Science Moore & Ito (1974); Moore & Araki (1977); van Kauwen- Laboratory Investigations. Any opinions, findings, and bergh et al. (1988); Voloshin et al. (1982). For details of conclusions or recommendations expressed in this material sailaufite, see: Wildner et al. (2003). For studies on para- are those of the author(s) and do not reflect the views of the robertsite, see: Roberts et al. (1989); Kampf (2000). For National Aeronautics and Space Administration. research involving Mn3+ pairing in phosphate minerals, see: Fransolet (2000). For information on crystalline manganese Supplementary data and figures for this paper are available from the phosphate-based adsorbers, see: Kulprathipanja et al. (2001). IUCr electronic archives (Reference: WM2672). References Bruker (2004). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA. i74 Andrade et al. doi:10.1107/S160053681203735X Acta Cryst. (2012). E68, i74–i75 inorganic compounds Downs, R. T. & Hall-Wallace, M. (2003). Am. Mineral. 88, 247–250. Roberts, A. C., Sturman, B. D., Dunn, P. J. & Roberts, W. L. (1989). Can. Flack, H. D. (1983). Acta Cryst. A39, 876–881. Mineral. 27, 451–455. Fransolet, A. M. (2000). Can. Mineral. 38, 893–898. Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Kampf, A. R. (2000). Am. Mineral. 85, 1302–1306. Voloshin, A. V., Men’shikov, Yu. P., Polezhaeva, L. I. & Lentsi, A. A. (1982). Kauwenbergh, S. J. van, Cooper-Fleck, M. & Williams, M. R. (1988). Mineral. Mineral. Zh. 4, 90–95. Mag. 52, 505–508. Westrip, S. P. (2010). J. Appl. Cryst. 43, 920–925. Kulprathipanja, S., Lewis, G. J. & Willis, R. R. (2001). US Patent No. 6 190 562. Wildner, M., Tillmanns, E., Andrut, M. & Lorenz, J. (2003). Eur. J. Mineral. 15, Moore, P. B. & Araki, T. (1977). Inorg. Chem. 16, 1096–1106. 555–564. Moore, P. B. & Ito, J. (1974). Am. Mineral. 59, 48–59. Acta Cryst. (2012). E68, i74–i75 Andrade et al. Ca2Mn3O2(PO4)3Á3H2O i75 supporting information supporting information Acta Cryst. (2012). E68, i74–i75 [https://doi.org/10.1107/S160053681203735X] III Robertsite, Ca2Mn 3O2(PO4)3·3H2O Marcelo B. Andrade, Shaunna M. Morrison, Adrien J. Di Domizio, Mark N. Feinglos and Robert T. Downs S1. Comment Robertsite is a member of the arseniosiderite-type compounds adopting a sheet structure that is characterized by layers of nine-membered pseudo-trigonal rings of octahedra. They exhibit the general formula Ca2A3O2(TO4)3.nH2O, with A = Fe, Mn; T = As, P; and n = 2 or 3. There are five members of this group in the current list of minerals approved by the 3+ International Mineralogical Association (IMA), including arseniosiderite, [Ca2Fe 3O2(AsO4)3.3H2O], kolfanite, 3+ 3+ 3+ [Ca2Fe 3O2(AsO4)3.2H2O], mitridatite, [Ca2Fe 3O2(PO4)3.3H2O], sailaufite, (Ca,Na)2Mn 3O2(AsO4)2CO3.3H2O, and 3+ robertsite [Ca2Mn 3O2(PO4)3.3H2O]. Because of ubiquitous twinning in this group, only the structures of mitridatite (Moore & Araki, 1977) and sailaufite (Wildner et al., 2003) have previously been reported. Arseniosiderite, mitridatite and robertsite exhibit monoclinic symmetry with space group Aa. Kolfanite can also be assigned in space group Aa, but with weak unindexed reflections (Voloshin et al., 1982). Sailaufite has been reported in space group Cm and a doubled cell presumably due to ordering of the carbonate group that substitutes the tetrahedral group. Robertsite and pararobertsite (Roberts et al., 1989; Kampf, 2000), are dimorphs with composition 3+ 2+ 3+ Ca2Mn 3O2(PO4)3.3H2O, and are the only phosphate minerals known to date with Ca and Mn cations (Fransolet, 2000). They occur in altered pegmatites and sedimentary phosphate ores as typical products of weathering (van Kauwenbergh et al., 1988), and are thus important to our understanding of the alteration processes of primary phosphate minerals. Crystalline manganese phosphates are also of particular interest for technological applications. For example, they have been studied as potential adsorbers of metal contaminants, such as Ag, Hg, and Pd, from industrial waste (Kulprathipanja et al., 2001). Robertsite was previously investigated by Moore & Ito (1974) using powder X-ray diffraction, but its crystal structure was not refined owing to the rarity of suitable single crystals. This study presents the first crystal structure determination of robertsite. The single-crystal data was obtained from a sample from the Tip Top mine. The structure of robertsite is built from sheets of [MnO6] octahedra sandwiched between layers of PO4 tetrahedra. The 3+ [MnO6] octahedra share edges to form nine-membered pseudo-trigonal rings that pack in monolayers (Fig. 1). The Mn cations sit on their own Kagome net, as a result of the repulsion between them (Kampf, 2000). All [MnO6] octahedra are distorted, characteristic of the Jahn-Teller effects for high-spin Mn3+ with d4 electromic configuration. Among the nine [MnO6] octahedra, that of Mn7 is flattened, while the others are elongated. For example, the Mn1 cation is surrounded by four short equatorial O atoms at 1.967 (5), 1.992 (5), 1.956 (4), and 1.862 (4) Å and by two axial O atoms at 2.137 (4) and 2.138 (4) Å. In contrast, the two-axial O atoms, O7 and O23, bonded to Mn7 are at 1.952 (5) and 1.898 (5) Å, respectively, whereas the four equatorial O atoms are at approximately 2.05 Å. Situated at the center of each nine- membered ring is a PO4 tetrahedron. The sheets of [MnO6] octahedra and PO4 tetrahedra are stacked together along the a axis by water molecules and a double layer of Ca2+ cations.
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