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The Structure of H3O -Exchanged Pharmacosiderite

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The Structure of H3O -Exchanged Pharmacosiderite Mineralogical Magazine, June 2010, Vol.74(3), pp.487–492 + The structure of H3O -exchanged pharmacosiderite 1, 2 2 2 1 S. J. MILLS *, S. L. HAGER ,P.LEVERETT ,P.A.WILLIAMS AND M. RAUDSEPP 1 Department of Earthand Ocean Sciences, University of BritishColumbia, Vancouver, BC, Canada V6T 1Z4 2 School of Natural Sciences, University of Western Sydney, Locked Bag 1797, Penrith South DC, NSW 1797, Australia [Received 2 May 2010; Accepted 16 June 2010] ABSTRACT + The crystal structure of H3O -exchanged pharmacosiderite (pharmacosiderite is KFe4(AsO4)3(OH)4· nH2O, sensu stricto) has been determined by single-crystal X-ray diffraction and refined to R1 = + + 0.0418. H3O -exchanged pharmacosiderite, (H3O )Fe4(AsO4)3(OH)4·4.5H2O, is cubic, space group P4¯3m, with a = 7.982(9) A˚ , V = 508.5(9) A˚ 3 and Z = 1. The structure broadly conforms to that of the general pharmacosiderite structure type, with the hydronium ion generated by partial protonation of a site corresponding to a molecule of water of crystallization and its symmetry-related equivalents. In addition, the structure of a ‘‘pharmacosiderite’’ from Cornwall, United Kingdom, in which no alkali + metals could be detected, has been re-evaluated and found to be consistent with that of the H3O - + exchanged structure. Its composition is (H3O )Fe4(AsO4)3(OH)4·4H2O, withthepartially occupied water found for the exchanged structure at (Ý, Ý, Ý) being absent in this case. KEYWORDS: hydronium, pharmacosiderite, crystal structure, exchange, Cornwall. Introduction pharmacosiderite variants. This has seen the THE pharmacosiderite group of minerals and description of bariopharmacosiderite-C and -Q synthetic variants have attracted much interest and natropharmacosiderite-C (Mills et al., 2010). due to a number of factors including ion exchange Alkali pharmacosiderites are usually cubic, space properties, changes in symmetry (Mutter et al., group P4¯3m with a & 8A˚ (Buerger et al., 1967), 1984; Peacor and Dunn, 1985) and their potential or space group I4¯3m with a & 16 A˚ (Mutter et al., use as molecular sieves (Mutter et al., 1984; 1984). However, some members exhibit ordering, Harrison et al., 1995; Dadachov and Harrison, which reduces the cubic symmetry to tetragonal, 1997; Behrens et al., 1998). One of the main space group P4¯2m with a & c & 8A˚ (Mills et al., drives for the latter is the capacity of pharmaco- 2010), or space group I4¯2m with a & c & 16 A˚ siderite to readily exchange alkali or alkaline (Mutter et al., 1984). earthions for heavierions suchas Cs + (Harrison The structure of pharmacosiderite was originally et al., 1995; Xu et al., 2004). Phases structurally reported by Zemann (1947, 1948), but the K+ ion related to pharmacosiderite have also been shown could not be located. Subsequently, Buerger et al. to be useful in the separation of the 90Y from 90Sr (1967) reported the crystal structure of pharmaco- (Sylvester, 2003) and the recovery of 82Sr from siderite from Cornwall, UK. In their structural irradiated targets (Sylvester et al., 2006). description, they pointed out that they too were Recently, there has been interest in developing unable to locate the K+ ion and postulated that the structural models for the various polymorphs of charge imbalance could be accounted for by the presence of a hydronium ion. In this connection, a spectrographic analysis of their crystal found that alkali metals were absent. To evaluate these suggestions, we have re-evaluated the crystal * E-mail: [email protected] structure of Buerger et al. (1967) and here we DOI: 10.1180/minmag.2010.074.3.487 report our findings, together with a description of a # 2010 The Mineralogical Society S. J. MILLS ET AL. + + single-crystal X-ray structure of an H3O - crystals. Similar methods to prepare H3O - exchanged natropharmacosiderite. exchanged pharmacosiderite have been reported by Mutter et al. (1984). The sample used is housed in the collections of Mineral Sciences Experimental Department, Natural History Museum of Los Sample description Angeles County, catalogue number LACMNH For the exchange experiment, several orange– 61590. A complete sample description can be brown, cubic, single crystals of natropharmacosi- found in Mills et al. (2010). derite [(Na0.75,K0.14,Ba0.11)S1.00Fe4(AsO4)3 (OH) O ·4H O; Mills et al. 2010] from the 3.89 0.11 2 Data collection Gold Hill mine, Gold Hill, Tooele County, Utah, 3 + USA, were placed in 10 cm of distilled water, to The single-crystal study of an H3O -exchanged which were added four drops of 10% aqueous crystal was carried out using a Bruker X8 ApexII HCl. Within ~10 s the colour of the crystals single-crystal diffractometer at the Department of changed from orange-brown to pale green, then Chemistry, University of British Columbia more slowly to a pale greenishgrey. Thecrystals (Table 1). A cubic crystal of dimensions were kept in the solution for four days before 0.15 mm60.15 mm60.15 mm was used for being examined by single-crystal X-ray diffrac- collection of intensity data at 293 K. The data tion methods. Chemical analysis confirmed the were processed withtheBruker Apex program absence of Na, K and Ba in the final exchanged suite (Bruker, 2003), withdata reduction using the TABLE 1. Crystal data and structure-refinement details. + H3O -exchanged pharmacosiderite ‘‘pharmacosiderite’’ (Buerger et al., 1967) + + Empirical formula (H3O )Fe4(AsO4)3(OH)4·4.5H2O(H3O )Fe4(AsO4)3(OH)4·4H2O M 808.29 799.28 Temperature 296(2) K Room temperature Wavelength0.71073 A ˚ 1.5418 A˚ Crystal system Cubic Cubic Space group P4¯3mP4¯3m Unit-cell dimensions a = 7.982(9) A˚ a = 7.980(10) A˚ Volume 508.5(9) A˚ 3 508.2(11) A˚ 3 Z 11 À3 À3 Dcalc. 2.639 mg m 2.612 mg m Absorption coefficient 7.73 mmÀ1 28.78 mmÀ1 F(000) 391 386 Crystal size 0.15 mm60.15 mm60.15 mm 0.17 mm60.17 mm60.17 mm y range for data collection 2.55 to 27.28o 7.65 to 69.49o Index ranges À5 4 h 4 9, À8 4 k 4 1, 1 4 h 4 9, 0 4 k 4 6, 0 4 l 4 5 À7 4 l 4 6 Reflections collected, Rint 329, 0.021 128 Independent reflections 171 128 Refinement method Full-matrix least-squares on F2 Full-matrix least-squares on F2 Goodness-of-fit on F2 1.33 1.31 Final R indices [I >2s(I)] R1 = 0.0418, wR2 = 0.1119 R1 = 0.0539, wR2 = 0.1482 R indices (all data)* R1 = 0.0431, wR2 = 0.1122 R1 = 0.0539, wR2 = 0.1482 Extinction coefficient 0.020(6) 0.004(2) Largest diffraction peak and hole 1.62 and À0.57 e.A˚ À3 1.34 and À0.69 e.A˚ À3 * The weighting schemes used were: 2 2 2 + w = 1/[s (Fo) + (0.051P) + 3.19P] for H3O -exchanged pharmacosiderite and; 2 2 2 w = 1/[s (Fo) + (0.071P) + 7.54P] for ‘‘pharmacosiderite’’ of Buerger et al. (1967), 2 2 where P = [Max(Fo) +2(Fc) ]/3 as defined by SHELX-97 488 + THE STRUCTURE OF H3O -EXCHANGED PHARMACOSIDERITE SAINT program and absorption correction by the respectively, and it was noted that they were in multi-scan method using SADABS (Bruker, 2003). similar positions to those reported by Buerger et Lists of observed and calculated structure factors al. (1967) for the general pharmacosiderite are deposited at http://www.minersoc.org/pages/ structure. Withthermalparameters for O3 and e_journals/dep_mat_mm.html#2010. O4 constrained to be isotropic, due to the partial (50%) occupancy of these atoms, an anisotropic refinement converged to R = 0.050. The resulting Description and discussion of the 1 + difference map and the thermal parameter for O3 H3O -exchanged pharmacosiderite structure clearly indicated that this atom was more The structure was solved in space group P4¯3m by appropriately positioned at (Ý, ~0.05, Ý), i.e. direct methods using SHELXS-97 and subsequent statistically distributed across the centre of the difference Fourier syntheses followed by full- cell face. Further, there was a significant residual matrix least-squares refinement on F2 using in the difference map at (Ý, Ý, Ý) which could be SHELXL-97 (Sheldrick, 2008). The initial loca- attributed to another partially occupied (50%) O tion of the framework ions Fe, As, O1 and O2 atom, O5. This final model (Figure 1) converged revealed that they were located in similar to R1 = 0.0418, where acceptable isotropic positions to those reported by Buerger et al. thermal parameters resulted for O3, O4 and O5 (1967) for the general pharmacosiderite structure when each of these atoms was assigned a and a subsequent isotropic refinement converged population parameter of 50%. to R1 = 0.079 at this stage. Inspection of a Inspection of the final difference map revealed difference Fourier map showed two significant no evidence of the expected hydroxyl H atom on residues at (Ý, 0, Ý) and (0.685, 0.685, 0.685) O2, as found in bariopharmacosiderite and which could be attributed to fractionally occupied natropharmacosiderite (Mills et al., 2010), O atoms (water or hydronium ion), O3 and O4 despite O2 having a close contact of 2.70 A˚ FIG. 1. Crystal structure of H3O-exchanged pharmacosiderite. AsO4 tetrahedra (yellow), FeO6 octahedra (orange) and oxygen atoms of water molecules (grey). 489 2 TABLE 2. Final atom coordinates, site occupancies and atom displacement parameters (A˚ ). x/ay/bz/c Occ. Ueq or Uiso U11 U22 U33 U23 U13 U12 + H3O -exchanged pharmacosiderite Fe 0.1433(3) 0.1433(3) 0.1433(3) 1 0.0097(9) 0.0099(9) 0.0099(9) 0.0099(9) À0.0004(8) À0.0004(8) À0.0004(8) As Ý 0 0 1 0.0123(8) 0.0065(15) 0.0153(11) 0.0153(11) 0 0 0 O1 0.1239(9) 0.1239(9) 0.3842(12) 1 0.019(2) 0.022(4) 0.022(4) 0.015(6) 0.001(3) 0.001(3) À0.007(4) S.
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