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Abstract

Meitnerite (IMA2017-065), (NH4)(UO2)(SO4)(OH)·2H2O, is a new mineral from the Green Lizard mine in Red Canyon, San Juan County, Utah, USA, where it occurs as a secondary alteration phase. It occurs on partially recrystallized quartz grains in association with beshtauite and gypsum. Meitnerite occurs as intergrowths of tabular crystals, flattened on {0 1 1}, up to about 80mm in diameter and 30 mm thick. The mineral is slightly greenish yellow and transparent with a vitreous lustre and very pale yellow streak. It exhibits greenish-white fluorescence in 405 nm light. Crystals are brittle with irregular fracture, and a perfect cleavage on {0 1 1}. The Mohs’ hardness is ca. 2. The calculated density is 3.320 g·cm–3. At room temperature, the mineral is slowly soluble in H2O and very rapidly soluble in dilute HCl. Optically, meitnerite is biaxial (–), with alpha = 1.568(2), beta = 1.589(2), gamma = 1.607(2) (white light); 2V = 84(1)°. The dispersion is r > v, moderate, The optical orientation is X ∧ b = 26°, Y ∧ a = 15°, Z ∧ c = 53°. The pleochroism is X nearly colourless, Z pale green yellow, Y light green yellow; X < Z < Y. Electron-microprobe analyses gave the empirical formula (NH4)1.01Na0.07(U0.97O2)(S1.03O4)[(OH)0.93O0.07]·2H2O, based on 9 O apfu. Meitnerite is triclinic, P1, a = 6.7964(2), b = 8.0738(3), c = 9.2997(7) A, alpha = 113.284(8), beta = 99.065(7), gamma = 105.289(7)°, V = 431.96(5) A^3 and Z = 2. The crystal structure, refined to R1 = 0.013 for 1871 observed reflections [I > 2sI], contains uranyl sulfate sheets based on the phosphuranylite anion topology. The interlayer region contains an NH4 group and two H2O groups.

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... The Green Lizard mine is near the head of Low Canyon on the east side of Red Canyon, 2.1 km north of the Blue Lizard mine. The Green Lizard mine is also a type locality for greenlizardite (Kampf et al., 2018b), shumwayite (Kampf et al., 2017b) and meitnerite (Kampf et al., 2018c). The Markey mine is also a type locality for feynmanite (Kampf et al., 2019), leószilárdite (Olds et al., 2017) and markeyite (Kampf et al., 2018a). ...
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Magnesioleydetite and straßmannite, two new uranyl sulfates minerals with sheet structures from Red Canyon, Utah - Anthony R. Kampf, Jakub Plášil, Anatoly V. Kasatkin, Barbara P. Nash, Joe Marty
Article
Chemically induced polytypic phase transitions have been observed during experimental investigations of crystallization in the mixed uranyl sulfate-selenate Mg[(UO2)(TO4)2(H2O)](H2O)4 (T = S, Se) system. Three different structure types form in the system, depending upon the Se:S ratio in the initial aqueous solution. The phases with the Se/(Se + S) ratios (in mol %) in the ranges 0-9, 16-47, and 58-100 crystallize in the space groups P21, Pmn21, and P21/c, respectively. The structures of the phases are based upon the same type of uranyl-based sulfate/selenate chains that, through hydrogen bonds, are linked into pseudolayers of the same topological type. The layers are linked into three-dimensional structures via interlayer Mg-centered octahedra. The three structure types contain the same layers but with different stacking sequences that can be conveniently described as belonging to the 1M, 2O, and 2M polytypic modifications. The Se-for-S substitution demonstrates a strong selectivity with preferential incorporation of Se into less tightly bonded T1 site. The larger ionic radius of Se6+ relative to S6+ induces rotation of (T1O4) tetrahedra in the adjacent layers and reconstruction of the structure types. From the information-theoretic viewpoint, the intermediate Pmn21 structure type is more complex than the monoclinic end-member structure types.
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The technogenic mineral phases NH4MgCl3·6H2O and (NH4)2Fe3+Cl5·H2O from the burned dumps of the Chelyabinsk coal basin have been investigated by single-crystal X-ray diffraction, scanning electron microscopy and high-temperature powder X-ray diffraction. The NH4MgCl3·6H2O phase is monoclinic, space group C2/c, unit cell parameters a = 9.3091(9), b = 9.5353(7), c = 13.2941(12) Å, β = 90.089(8)° and V = 1180.05(18) Å3. The crystal structure of NH4MgCl3·6H2O was refined to R1 = 0.078 (wR2 = 0.185) on the basis of 1678 unique reflections. The (NH4)2Fe3+Cl5·H2O phase is orthorhombic, space group Pnma, unit cell parameters a = 13.725(2), b = 9.9365(16), c = 7.0370(11) Å and V = 959.7(3) Å3. The crystal structure of (NH4)2Fe3+Cl5·H2O was refined to R1 = 0.023 (wR2 = 0.066) on the basis of 2256 unique reflections. NH4MgCl3·6H2O is stable up to 90 °C and then transforms to the less hydrated phase isotypic to β-Rb(MnCl3)(H2O)2 (i.e., NH4MgCl3·2H2O), the latter phase being stable up to 150 °C. (NH4)2Fe3+Cl5·H2O is stable up to 120 °C and then transforms to an X-ray amorphous phase. Hydrogen bonds provide an important linkage between the main structural units and play the key role in determining structural stability and physical properties of the studied phases. The mineral phases NH4MgCl3·6H2O and (NH4)2Fe3+Cl5·H2O are isostructural with natural minerals novograblenovite and kremersite, respectively.
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Uranyl sulfates, including those occurring in Nature (∼40 known members), possess particularly interesting structures. They exhibit a great dimensional and topological diversity of structures: from those based upon clusters of polyhedra to layered structures. There is also a great variability in the type of linkages between U and S polyhedra. From the point of view of complexity of those structures (measured as the amount of Shannon information per unit cell), most of the natural uranyl sulfates are intermediate (300–500 bits per cell) to complex (500–1000 bits per cell) with some exceptions, which can be considered as very complex structures (>1000 bits per cell). These exceptions are minerals alwilkinsite-(Y) (1685.95 bits per cell), sejkoraite-(Y) (1859.72 bits per cell), and natrozippeite (2528.63 bits per cell). The complexity of these structures is due to an extensive hydrogen bonding network which is crucial for the stability of these mineral structures. The hydrogen bonds help to propagate the charge from the highly charged interlayer cations (such as Y ³⁺ ) or to link a high number of interlayer sites ( i.e. five independent Na sites in the monoclinic natrozippeite) occupied by monovalent cations (Na ⁺ ). The concept of informational ladder diagrams was applied to the structures of uranyl sulfates in order to quantify the particular contributions to the overall informational complexity and identifying the most contributing sources (topology, real symmetry, interlayer bonding).
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SIR2011, the successor of SIR2004, is the latest program of the SIR suite. It can solve ab initio crystal structures of small- and medium-size molecules, as well as protein structures, using X-ray or electron diffraction data. With respect to the predecessor the program has several new abilities: e. g. a new phasing method (VLD) has been implemented, it is able to exploit prior knowledge of the molecular geometry via simulated annealing techniques, it can use molecular replacement methods for solving proteins, it includes new tools like free lunch and new approaches for electron diffraction data, and it visualizes three-dimensional electron density maps. The graphical interface has been further improved and allows the straightforward use of the program even in difficult cases.
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Magnesioleydetite and straßmannite, two new uranyl sulfates minerals with sheet structures from Red Canyon, Utah - Anthony R. Kampf, Jakub Plášil, Anatoly V. Kasatkin, Barbara P. Nash, Joe Marty
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The new mineral greenlizardite (IMA2017-001), (NH 4 )Na(UO 2 ) 2 (SO 4 ) 2 (OH) 2 ·4H 2 O, was found in the Green Lizard mine, Red Canyon, San Juan County, Utah, USA, where it occurs as a secondary alteration phase. It is associated with ammoniozippeite, boussingaultite and dickite. It forms as light green-yellow blades up to ~0.3 mm long. The mineral is vitreous and transparent with a white streak. It fluoresces greenish blue in 405 nm light. Mohs hardness is ~2. Crystals are brittle with irregular fracture and two cleavages: perfect {001} and good {2 $\bar 1$ 0}. Greenlizardite is easily soluble in room-temperature H 2 O. The calculated density is 3.469 g cm –3 . Optically, it is biaxial (+) with α = 1.559(1), β = 1.582(1) and γ = 1.608(1) (measured in white light). The measured 2V is 88(1)°; the calculated 2V is 87.8°. Dispersion is moderate, r < v . Pleochroism is X = very pale yellow green, Y = pale yellow green and Z = light yellow green; X < Y < Z . The optical orientation is X ≈ c , Y ≈ a and Z ≈ b* . The Raman spectrum exhibits bands attributable to both sulfate and uranyl groups. Electron probe microanalyses (with H 2 O based on the crystal structure) yielded (NH 4 ) 0.98 Na 1.00 U 1.96 S 2.04 O 18.00 H 10.02 . Greenlizardite is triclinic, P$\bar 1$ , a = 6.83617(17), b = 9.5127(3), c = 13.8979(10) Å, α = 98.636(7), β = 93.713(7), γ = 110.102(8)°, V = 832.49(8) Å ³ and Z = 2. The crystal structure ( R1 = 2.39% for 2542 I > 2σ I ) contains edge-sharing dimers of UO 7 pentagonal bipyramids. The dimers link by sharing corners with SO 4 groups to form a [(UO 2 ) 2 (SO 4 ) 2 (OH) 2 ] 2– sheet based on the phosphuranylite anion topology. Zig-zag edge-sharing chains of NaO 6 octahedra link adjacent [(UO 2 ) 2 (SO 4 ) 2 (OH) 2 ] 2– sheets, forming thick slabs. NH 4 bonds to O atoms in adjacent slabs linking them together. H 2 O groups occupy channels in the slabs and space between the slabs.
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This chapter demonstrates a wide structural diversity of actinyl compounds containing hexavalent cations of S, Cr, Se, Mo, and W. Several factors control such diversity: (i) coordination of cations: both actinide and hexavalent cations may have different coordinations; (ii) mode of linkage of coordination polyhedra: all combinations of corner and edge sharing among polyhedra are allowed; of special interest is the high frequency of edge sharing between UO7 pentagonal bipyramids and SO4 tetrahedra; actinyl polyhedra polymerize by sharing either equatorial anions or even apical anions; (iii)high flexibility of structural units consisting of actinyl polyhedral and TO4 tetrahedra that are analysed by means of statistical investigations of U-Obr-T bond angles; among different units, uranyl molybdates show the widest variation of the angular characteristics, in agreement with their strong tendency to formation framework structures.
Article
A new mineral beshtauite, (NH4)2(UO2)(SO4)2·2H2O, was found in the oxidation zone of the Beshtau uranium deposit, Mount Beshtau, Stavropol region, Northern Caucasus, Russia, and named after the locality. It is associated with rozenite, gypsum, lermontovite, and older marcasite, pyrite, halloysite, and opal. Beshtauite occurs as well-shaped short-prismatic crystals up to 0.1 × 0.15 × 0.2 mm, their clusters and crusts up to 0.5 mm across growing on marcasite. Beshtauite is transparent, light green. The luster is vitreous. The mineral fluoresces strongly yellow-green under both short- and long-wave UV irradiation. It is brittle. The Mohs hardness is ca. 2. Cleavage was not observed. Dcalc is 3.046 g/cm3. Beshtauite is optically biaxial (+), α = 1.566(3), β = 1.566(3), γ = 1.592(3), 2Vmeas < 10°. The chemical composition (wt%, electron microprobe data, H2O by difference) is: (NH4)2O 10.33, UO3 53.21, SO3 29.40, H2Ocalc 7.06, total 100.00. Content of (NH4)2O was calculated from measured nitrogen content: 5.56 wt% N. The empirical formula, calculated on the basis of 12 O apfu, is (NH4)2.12U0.99S1.96O9.91(H2O)2.09. Beshtauite is monoclinic, P21/c, a = 7.7360(8), b = 7.3712(5), c = 20.856(2) Å, β = 102.123(8)°, V = 1162.76(19) Å3, Z = 4 (from single-crystal X-ray diffraction data). The strongest reflections of the X-ray powder pattern [d (Å), I(hkl)] are: 6.86, 100(011, 102̄); 5.997, 19(012); 5.558, 15(102); 5.307, 36(111̄,110); 5.005, 35(013,112̄); 3.410, 38(114,204̄,106̄); 3.081, 24(016); 2.881, 20(106,123). The crystal structure was solved by direct methods and refined on the basis of 2677 independent reflections with I > 4σ(I) to R1 = 0.093. The structure is based upon [UO2(SO4)2(H2O)]2− layers consisting of corner-sharing UO6(H2O) pentagonal bipyramids and SO4 tetrahedra. The layers are coplanar to (1̄02) and are linked via hydrogen bonding that involve interlayer NH4+ ions and H2O molecules. Beshtauite is important indicator mineral: its presence can be considered as an evidence of transportation of U6+ in nature in forms of mobile complexes of uranyl cation with ammonia or polyamines.
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The photoluminescence spectra of hydrated and anhydrous uranyl sulfates have been studied under conditions of high resolution at cryogenic temperatures. All uranyl sulfate systems were found to yield nonequivalent spectra: the energies for the electronic and vibronic origins were found to vary with the system, and certain uranyl vibrational frequencies exhibited a dependence on environment. These differences must reflect the various ways in which the uranyl centers are linked by the bridging sulfate groups, as this linking is the main difference between the various structures.
Article
A study of the low frequency vibrational spectra of compounds of the type L2UO2(NO3)2 (L = mono-dentate ligand), MUO2(NO3)3 (M = monovalent cation), and CS2UO2X4 (X = Cl or Br) has shown that the deformation frequency of the uranyl group occurs in the region 274–245 cm−1 but detailed assignments of the U—O (nitrate) frequencies are not given since it is shown that structurally related complexes do not necessarily give similar low frequency infrared (i.r.) and Raman spectra.
The i.r. spectra of UO2(NO3)2·6H2O, UO2(NO3)2(NH3)2, K2UO2(NO3)2F2 and K2UO2(NO3)2(CN)2 have been measured in the region from 4000 to 30 cm−1. The vibrational assignments of their skeletal vibrations have been made on the basis of a normal coordinate analysis in which a modified valence force field is assumed. Approximate force constants associated with the UO, UNO3 and UL (LH2O, NH3, F, CN) bonds have been obtained for the respective complexes.The ligation effects on the UO bonds in the complexes have been investigated through the calculations of overlap integrals of 1πu-molecular orbitals in the uranyl bonding. It has been suggested that the UO stretching force constant, which is a good measure for the UO bond strength, is closely related to the overlap integrals of the 1πu-molecular orbitals.
Article
Vibrational (Raman and infrared) spectra of nine alkali metal (lithium, sodium and potassium) uranates have been measured in the infrared range of 4000–250 cm−1 and the Raman shift range of 1100–50 cm−1. The Raman spectra of sodium and potassium uranates, and lithium polyuranates are reported for the first time. From these spectra the site symmetries of intrinsic uranate groups are deduced by comparing the number of observed and resolved bands with the number predicted by the various site symmetries subgroups possible for each uranate crystal symmetry. The following could then be assigned: C2h for Li2UO4; D2h for α-Na2UO4; D4h for K2UO4; D2 for Na2U2O7 and C2h for K2U2O7. For the lithium polyuranates, Li2O·1.6UO3, Li2O·1.75UO3, Li2U2O7 and Li2U3O10, as their crystal symmetries are not fully known, no definite conclusions concerning uranate site symmetry could be drawn, except that primitive monoclinic symmetry point groups must be excluded.
Article
The crystal structures of uranyl minerals and inorganic uranyl compounds are important for understanding the genesis of U deposits, the interaction of U mine and mill tailings with the environment, transport of actinides in soils and the vadose zone, the performance of geological repositories for nuclear waste, and for the development of advanced materials with novel applications. Over the past decade, the number of inorganic uranyl compounds (including minerals) with known structures has more than doubled, and reconsideration of the structural hierarchy of uranyl compounds is warranted. Here, 368 inorganic crystal structures that contain essential U 6+ are considered (of which 89 are minerals). They are arranged on the basis of the topological details of their structural units, which are formed by the polymerization of polyhedra containing higher-valence cations. Overarching structural categories correspond to those based upon isolated polyhedra (8), fi nite clusters (43), chains (57), sheets (204), and frameworks (56) of polyhedra. Within these categories, structures are organized and compared upon the basis of either their graphical representations, or in the case of sheets involving sharing of edges of polyhedra, upon the topological arrangement of anions within the sheets.
Article
The uranyl sulphate mineral zippeite was studied by Raman spectroscopy. The phase purity of the sample was initially checked by X-ray powder diffraction and its chemical composition was defined by electron microprobe (wavelength dispersive spectroscopy, WDS) analysis. The Raman spectroscopy research focused on the low wavenumber and uranyl stretching vibration regions. Vibration bands down to 50 cm(-1) were tentatively assigned. The U-O bond lengths were calculated based on empirical relations. Inferred values are consistent with those obtained from the crystal structure analysis of synthetic zippeite. Number of bands was interpreted on the basis of factor group analysis.
The Geology and Production History of the Uranium Deposits in the White Canyon Mining District
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Chenoweth, W.L. (1993): The Geology and Production History of the Uranium Deposits in the White Canyon Mining District, San Juan County, Utah. Utah Geol. Surv. Misc. Publ., 93, 3.
Fermiite, Na 4 (UO 2 )(SO 4 ) 3 ·3H 2 O, and oppenheimerite, Na 2 (UO 2 )(SO 4 ) 2 ·3H 2 O, two new uranyl sulfate minerals from the Blue Lizard mine
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Kampf, A.R., Plá sil, J., Kasatkin, A.V., Marty, J., Čejka, J. (2015c): Fermiite, Na 4 (UO 2 )(SO 4 ) 3 ·3H 2 O, and oppenheimerite, Na 2 (UO 2 )(SO 4 ) 2 ·3H 2 O, two new uranyl sulfate minerals from the Blue Lizard mine, San Juan County, Utah, USA. Mineral. Mag., 79, 1123-1142.
H 2 O) 2 ] 2 ·H 2 O, a new uranyl sulfate mineral from Red Canyon
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Kampf, A.R., Plá sil, J., Kasatkin, A.V., Marty, J., Čejka, J., Lapčák, L. (2017): Shumwayite, [(UO 2 )(SO 4 )(H 2 O) 2 ] 2 ·H 2 O, a new uranyl sulfate mineral from Red Canyon, San Juan County, Utah, USA. Mineral. Mag., 81, 273-285.
Ammoniozippeite, a new uranyl sulfate from the Blue Lizard mine
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  • J Marty
Kampf, A.R., Plá sil, J., Olds, T.A., Nash, B.P., Marty, J. (2018a): Ammoniozippeite, a new uranyl sulfate from the Blue Lizard mine, San Juan County, Utah, and the Burro mine, San Miguel County, Colorado, USA. Can. Mineral., 56, (in press).
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Plá sil, J., Hauser, J., Petříček, V., Meisser, N., Mills, S.J., Škoda, R., Fejfarová, K., Čejka, J., Sejkora, J., Hlou sek, J., Johannet, J.-M., Machovič, V., Lapčák. L. (2012): Crystal structure and formula revision of deliensite, Fe[(UO 2 ) 2 (SO 4 ) 2 (OH) 2 ](H 2 O) 7. Mineral. Mag., 76, 2837-2860.
O) 4 : X-ray & Raman spectroscopy study
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Plá sil, J., Meisser, N., Čejka, J. (2016): The crystal structure of Na 6 [(UO 2 )(SO 4 ) 4 ](H 2 O) 4 : X-ray & Raman spectroscopy study. Can. Mineral., 54, 5-20.
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Sheldrick, G.M. (2015): Crystal structure refinement with SHELXL. Acta Crystallogr., C71, 3-8.