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The Modular Structure of the Novel Uranyl Sulfate Sheet in [Co(H O) ] [(UO ) (SO ) (H O)](H O)

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The Modular Structure of the Novel Uranyl Sulfate Sheet in [Co(H O) ] [(UO ) (SO ) (H O)](H O) Journal of Geosciences, 59 (2014), 135–143 DOI: 10.3190/jgeosci.164 Original paper The modular structure of the novel uranyl sulfate sheet in [Co(H2O)6]3[(UO2)5(SO4)8(H2O)](H2O)5 Sergey V. KrIVOVIcheV1 and Peter c. BurnS2* 1 Department of Crystallography, St. Petersburg State University, University Emb. 7/9, 199034 St. Petersburg, Russia 2 Department of Civil and Environmental Engineering and Earth Sciences, University of Notre Dame, 156 Fitzpatrick Hall, Notre Dame, Indiana 46556–0767, USA; [email protected] * Corresponding author A new uranyl sulfate, [Co(H2O)6]3[(UO2)5(SO4)8(H2O)](H2O)5, has been synthesized using mild hydrothermal methods. 3 The structure (monoclinic, P21/c, a = 27.1597(14), b = 9.9858(5), c = 22.7803(12) Å, β = 106.520(1)°, V = 5923.2(5) Å , 2 Z = 4) has been solved by direct methods and refined on the basis ofF for all unique reflections toR 1 = 0.056, calculated for the 9124 unique observed reflections (|Fo| ≥ 4σF). It contains five symmetrically distinct uranyl pentagonal bipyra- mids and eight sulfate tetrahedra that link via the sharing of vertices between uranyl polyhedra and sulfate tetrahedra, 2+ resulting in sheets parallel to (001). Adjacent sheets are linked by hydrogen bonds to Co (H2O)6 octahedra and H2O groups located in the interlayer. The uranyl sulfate sheet contains four- and five-connected uranyl pentagonal bipyramids and three- and four-connected sulfate tetrahedra. The sheet may be constructed using modules from related structures involving pentagonal bipyramids and tetrahedra, and is readily described using a nodal representation. In general, the uranyl sulfate sheets in [Co(H2O)6]3[(UO2)5(SO4)8(H2O)](H2O)5 are more rigid than the structural units typically found in comparable uranyl molybdates, which involve the sharing of vertices between uranyl pentagonal bipyramids and molybdate tetrahedra. Keywords: uranyl sulfate, crystal structure, hydrothermal methods, structure topology Received: 28 December 2013; accepted: 19 March 2014; handling editor: J. Plášil 1. Introduction structures involving edge-sharing between uranyl and sulfate polyhedra have also been described (Mikhailov Uranyl sulfate hydrates are environmentally important et al. 1977; Hayden and Burns 2002a, b). phases that form in oxidation zones of uranium mineral We report the crystal structure of a cobalt uranyl sul- deposits and possibly as alteration products of nuclear fate in which UrO5 bipyramids do not polymerize with waste (Finch and Murakami 1999). Uranyl sulfates were each other, but share their equatorial vertices with SO4 also found in oxidized zones of the Bangombé and Oké- tetrahedra, resulting in a topologically and geometrically lobondo natural fission reactors in southeastern Gabon, complex uranyl sulfate sheet. This topology may be Africa (Janeczek 1999; Jensen and Ewing 2001). Uranyl described using a nodal approach that we developed for sulfate hydrates of divalent metals (Cu, Mg, Co, Ni, and the description of uranyl molybdate and uranyl chromate Zn) are especially abundant in nature (Frondel et al. units (Krivovichev et al. 2002a, b, 2005; Krivovichev and 1976; Finch and Murakami 1999) and several synthetic Burns 2003a, b, c, d, e). phases are also known (Gil and Gil 1977; Tabachenko et al. 1979; Serezhkin et al. 1981; Serezhkin and Serezhkina 1982). The structures of the most abundant uranyl sul- 2. Experimental fates are based upon structural units consisting of uranyl pentagonal bipyramids (Urφ ; Ur = UO 2+, uranyl ion, φ 5 2 2.1. Synthesis = unspecified ligand) and SO4 tetrahedra (Burns 2005). Urφ bipyramids may polymerize by sharing equatorial 5 A mixture of CoSO4 (0.123 g), CrO3 (0.147 g), UO3 edges as in the structures of zippeite-group minerals (0.110 g) and 5 ml of ultrapure H2O was placed in a (Vochten et al. 1995; Brugger et al. 2003; Burns et al. Teflon-lined 23 ml Parr reaction vessel and heated to 2003; Brugger et al. 2006; Peeters et al. 2008; Plášil et 120 °C for 14 days, followed by cooling to ambient al. 2011a, b, 2012, 2013a), uranopilite (Burns 2001), temperature. No crystals or precipitates had formed, so johannite (Mereiter 1982) and deliensite (Plášil et al. the solution was placed in a fume hood to evaporate. 2013b). The Urφ5 bipyramids and SO4 tetrahedra are After two days, transparent light yellow crystals of usually linked by corner-sharing only, although several [Co(H2O)6]3[(UO2)5(SO4)8(H2O)](H2O)5 were recovered. www.jgeosci.org Sergey V. Krivovichev, Peter C. Burns 2.2. Data collection distance of 2.45 Å. The site occupancy factors and isotro- pic displacement parameters for the Co(4) positions were The crystal selected for data collection was mounted fixed at 0.50 and 0.10 Å2, respectively. Isotropic displace- on a Bruker three-circle diffractometer equipped with a ment parameters for several H2O groups were fixed at 0.15 SMART APEX CCD (charge-coupled device) detector Å2. The final model included anisotropic displacement with a crystal-to-detector distance of 4.67 cm. Data were parameters for U, S, and non-disordered Co and S atoms, collected using monochromated MoKα X-rays and frame and isotropic displacement parameters for the anions. The widths of 0.3° in ω. The unit-cell dimensions (Tab. 1) final atomic positional and displacement parameters are in were refined on the basis of 8117 intense reflections using Tab. 2, selected interatomic distances are in Tab. 3. least-squares techniques. More than a hemisphere of data was collected and the three-dimensional data set was re- duced and filtered for statistical outliers using the Bruker 3. Results program SAINT. The data were corrected for Lorentz, polarization and background effects. An empirical absorp- On the basis of the structure determination, the composition tion correction was done on the basis of 1500 reflections of the crystal studied is [Co(H2O)6]3[(UO2)5(SO4)8(H2O)] by modeling the crystal as an ellipsoid; this resulted in a (H2O)5. We note that the synthesis reaction included CrO3 decrease of Rint from 0.113 to 0.049. Additional informa- and it is possible that Cr substitutes at the Co site in the tion pertinent to the data collection is given in Tab. 1. crystal structure. Such substitution, especially at a minor level, would be difficult to discern on the basis of X-ray Tab. 1 Crystallographic data and refinement parameters for diffraction. [Co(H2O)6]3[(UO2)5(SO4)8(H2O)](H2O)5 a (Å) 27.1597(14) 3.1. Cation coordination polyhedra b (Å) 9.9858(5) c (Å) 22.7803(12) There are five independent U6+ cations in the structure β (o) 106.520(1) and each is part of an approximately linear UO 2+ uranyl 3 2 V (Å ) 5923.2(5) ion (Ur). The U(1)O 2+, U(2)O 2+, U(3)O 2+ and U(4) Space group P2 /c 2 2 2 1 O 2+ cations are each coordinated by five O atoms that F 4972 2 000 are arranged at the equatorial vertices of UrO pentago- µ (cm–1) 148.54 5 nal bipyramids. The U(5)O 2+ cation is coordinated by Z 4 2 3 four O atoms and one H2O group, giving a UrO4(H2O) Dcalc (g/cm ) 3.06 Crystal size (mm) 0.08 × 0.04 × 0.01 pentagonal bipyramid. The <U–OUr> and <U–Oeq> (Oeq: equatorial O atom) bond lengths are in the range of 1.75 Radiation MoKα Total Ref. 64514 to 1.77 and 2.37 to 2.42 Å, respectively. The U(5)–H2O Unique Ref. 24282 bond length is 2.43 Å, which is typical for equatorial U6+–H O bonds (Burns et al. 1997). Unique |Fo| ≥ 4σF 9124 2 6+ R1 0.056 Eight symmetrically independent S cations are each wR2 0.124 tetrahedrally coordinated by four O atoms. The <S–O> S 0.778 bond lengths range from 1.46 to 1.47 Å, in good agree- Note: R1 = Σ||Fo| – |Fc||/Σ|Fo|; ment with the average <S–O> bond length of 1.473 Å wR2 = {Σ[w(F 2 – F 2)2]/Σ[w(F 2)2]}1/2; o c o reported for sulfates (Hawthorne et al. 2000). 2 2 2 2 2 w =1/[σ (Fo )+(aP) + bP] where P = (Fo + 2Fc )/3; 2+ 2 2 1/2 There are four symmetrically independent Co cat- s = {Σ[w(Fo – Fc )]/(n – p)} where n is the number of reflections and p is the number of refined parameters ions in the structure, each of which is coordinated by six H2O groups. The Co(1), Co(2) and Co(3) sites are fully occupied and are in slightly distorted octahedral 2.3. Structure solution and refinement coordination. In contrast, the coordination environment Scattering curves for neutral atoms, together with anom- around the half-occupied Co(4) site is a strongly distorted alous-dispersion corrections, were taken from Ibers and octahedron. The <Co–O> bond lengths are in the range Hamilton (1974). The Bruker SHELXTL Version 5 system of 2.03 to 2.12 Å. of programs was used for the determination and refine- ment of the structure. The positions of U, Co and S atoms 3.2. Bond-valence analysis and h O groups were determined by direct methods and other atoms were 2 located in the difference-Fourier maps calculated follow- The bond-valence sums were calculated using parameters ing refinement of the partial-structure model. The Co(4) given for U6+–O bonds (Burns et al. 1997) and for S6+– atom is disordered over two sites, with a Co(4)–Co(4) O and Co2+–O bonds (Brown and Altermatt 1985).
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