The crystal structure of curite, [Pb6.56(H2O,OH)4] [(UO2)8O8(OH)6]2

Summary The crystal structure of curite, of which until now only the arrangement of the U and Pb atoms was known, has been redetermined with a synthetic crystal using three-dimensional X-ray techniques.R=0.043 for 1270 observed reflections. Curite is orthorhombic, space groupPnam-D _2h ¹⁶ ,a=12.513,b=13.002,c=8.373 ,Z=6.56 PbO·16UO₃·9.44H₂O. The structure consists of a novel type of washboard like puckered layers ² [(UO₂)₈O₈ (OH)₆]^6– formed by tetragonal bipyramidal [(UO₂)O₃(OH)] and pentagonal bipyramidal [(UO₂)O₃ (OH)₂] polyhedra. The layers are parallel to {100} and are directly connected by hydrogen bonds. Lead atoms and oxygen atoms (H₂O+OH) are located in folds between the layers, helping to connect them. The interlayer atomic positions are slightly disordered and one of them is partially occupied. The variable concentrations of the interlayer atoms are responsible for the changes in chemical composition.The structural formula [Pb_8–x (OH)_4–2x (H₂O)_2x ] [(UO₂)₈(OH)₆]₂ is suggested for curite;x=1.44 for the investigated synthetic curite. Within the three different U–O polyhedra the axial U–O distances are 1.81–1.88 , the equatorial 2.14–2.57 . The two different Pb atoms have ionic coordinations, each by ten oxygens with Pb–O distances of 2.46–3.32 , on the average 2.82 .

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Die Kristallstruktur von Curit, [Pb _6,56 (H ₂ O, OH) ₄ ] [(UO ₂)₈ O ₈(OH)₆]₂

Zusammenfassung Die Kristallstruktur von Curit, von der bisher nur die Lagen der Uran- und Bleiatome bekannt waren, wurde anhand eines künstlichen Kristalls mit dreidimensionalen Röntgendaten neu bearbeitet und für 1270 Reflexe aufR=0,043 verfeinert. Curit kristallisiert rhombisch, RaumgruppePnam-D _2h ¹⁶ ,a=12,513,b=13,002,c=8,373 ,Z=6,56 PbO·16 UO₃·9,44 H₂O. Die Struktur enthält gewellte Schichten eines neuen Typs, ² [(UO₂)₈O₈(OH)₆]^6–, die sich aus tetragonal bipyramidalen [(UO₂)O₃(OH)]- und pentagonal-bipyramidalen [(UO₂)O₃(OH)₂]-Polyedern zusammensetzen. Die Schichten verlaufen parallel {100} und sind über Wasserstoffbrücken miteinander unmittelbar verknüpft. Zwischen den Schichten befinden sich Bleiatome und zusätzliche Sauerstoffatome (H₂O+OH). Diese Atome weisen zum Teil Fehlordnung auf; eine der beiden Pb-Lagen ist nur partiell besetzt. Für Schwankungen in der chemischen Zusammensetzung von Curit ist der unterschiedliche Gehalt an Zwischenschichtatomen verantwortlich. Aufgrund dieser Untersuchung wird die Strukturformel [Pb_8–x (OH)_4–2x (H₂O)_2x ] [(UO₂)₈O₈(OH)₆]₂ vorgeschlagen; für den untersuchten Curit istx=1,44. Die drei verschiedenen U–O-Polyeder der Struktur besitzen axiale bzw. äquatoriale U–O-Abstände von 1,81–1,88 bzw. 2,14–2,57 . Die zwei Arten von Bleiatomen besitzen eine ionische Koordination; beide sind von 10 Sauerstoffatomen in Abständen von 2,46–3,32 (Mittelwert 2,82 ) umgeben.

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With 3 Figures     

The crystal structure of sonoraite,Fe3+Te4+O3(OH)·H2O

Summary Sonoraite, FeTeO₃(OH)·H₂O, is monoclinic,P 2₁/c, witha=10.984(2),b=10.268(2),c=7.917(2) Å, =108.49(2)°. For 8 formula units per cell the calculated density is 4.179(2) g/cm³; the observed value is 3.95(1) g/cm³. The Supper-Pace automated diffractometer was used to collect 1884 independent reflections which were corrected for absorption. The structure was determined by an automated symbolic addition procedure. It was refined to a residualR of 6.2% using anisotropic temperature factors for the cations and isotropic temperature factors for the oxygen atoms. Chains of octahedra about Fe extend along [101]; edge-sharing pairs of these octahedra are joined by corner sharing. The Fe–Fe distances across the shared edges are 3.05 and 3.20 Å, short enough to suggest magnetic interactions. All but one H₂O are involved in the chains. The Te⁴⁺ ions have a pseudotetrahedral coordination, with three oxygen ions forming one face of the tetrahedron and the lone electron pair of Te occupying the fourth corner. The O–Te–O average bond angle is 95°. The Fe chains are tied together by Te–O bonds in all three dimensions.

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Die Kristallstruktur von Sonorait, Fe³⁺Te⁴⁺O₃(OH).H₂O

Zusammenfassung Sonorait, FeTeO₃(OH)·H₂O, ist monoklin, P 2₁/c, mit den folgenden Zelldimensionen:a=10,984(2),b=10,268(2),c=7,917(2) Å, =108,49(2)°. Mit 8 Formel-Einheiten errechnet man eine Dichte von 4,179(2) g/cm³; die gemessene Dichte beträgt 3,95(1) g/cm³. Das Supper-Pace automatische Diffraktometer wurde zur Sammlung von 1884 unabhängigen Reflexen benutzt, welche für Absorption korrigiert wurden. Die Struktur wurde mit Hilfe eines vollständig automatischen Programms für symbolische Addition bestimmt. Mit anisotropen Temperaturfaktoren für die Kationen und mit isotropen Temperaturfaktoren für die Sauerstoff-Atome wurde ein Residuum von 6,2% erreicht. Ketten von Eisen-Oktaedern erstrecken sich entlang [101]; Oktaeder-Paare mit gemeinsamen Kanten sind über Eckenverknüpfung verbunden. Die Fe–Fe-Abstände über die gemeinsamen Kanten betragen 3,05 und 3,20 Å, kurz genug, um zu magnetischer Wechselwirkung führen zu können. Nur ein H₂O-Molekül ist nicht Teil einer Kette. Die Te⁴⁺-Ionen befinden sich in pseudotetraedrischer Koordination; drei Sauerstoff-Ionen bilden eine Fläche des Tetraeders, die vierte Ecke wird durch das einsame Elektronenpaar von Te besetzt. Der Mittelwert des O–Te–O-Bindungswinkels beträgt 95° Die Fe-Ketten werden durch Te–O-Bindungen dreidimensional verbunden.

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With 3 Figures     

The crystal structure of trigonite,Pb3Mn(AsO3)2(AsO2OH)

Summary The mineral trigonite crystallizes in the monoclinic space groupPn–C _s ² witha ₀=7.26,b ₀=6.78,c ₀=11.09Å; =91.5°,Z=2. The structure was determined from 1250 X-ray intensities collected on an automatic two circle Weissenberg-type diffractometer. The final residual isR=6.5% using anisotropic temperature factors for Pb, Mn and As, and isotropic temperature factors for O.The structure consists of MnO₆ octahedra, sharing all six oxygens with arsenite groups to form a framework. The Pb atoms are attached to this framework with Pb–O distances2.23Å. One oxygen, bound only to an As atom, is interpreted as the donor for a hydrogen bond of 2.75Å.

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Die Kristallstruktur des Trigonits, Pb₃Mn(AsO₃)₂(AsO₂OH)

Zusammenfassung Das Mineral Trigonit kristallisiert monoklin, RaumgruppePn–C _s ² ,a ₀=7,26,b ₀=6,78,c ₀=11,09Å; =91,5°;Z=2. Die Strukturermittlung erfolgte anhand von 1250 Röntgenintensitäten, die auf einem automatischen Zweikreis-Weissenbergdiffraktometer gesammelt wurden. Mit anisotropen Temperaturfaktoren für Pb, Mn und As sowie isotropen für die O-Atome ergibt sich einR-Wert von 6,5%.Die MnO₆-Oktaeder werden über die sechs Sauerstoffe mit Arsenitgruppen zu einem dreidimensionalen Gerüst verknüpft. Über Pb-O-Abstände2,23 Å sind die Pb-Atome in dieses Gerüst eingebaut. Ein Sauerstoff, nur an ein As-Atom gebunden, wird als Donator einer H-Brücke von 2,75 Å interpretiert.

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Synthesis and crystal structure of a triple chain silicate,Na2Mg4Si6O16(OH)2

In the system Na₂CO₃-MgO-SiO₂-H₂O a new sodium magnesium silicate was synthesized under hydrothermal conditions; 450–600 ° C and 300–1000 Kg/cm₂. The structure of the specimen was determined by X-ray powder methods, and its properties were studied by chemical, infrared and TG analyses. The specimen has a triple chain structure (space group, C2/c) with the ideal chemical composition, 4 (Na₂Mg₄Si₆O₁₆(OH)₂) and lattice parameters, a= 10.152(2), b=27.137(4), c=5.276(1) Å, and = 106.97(3) °.The essential feature of the structure is shown by the presence of SiO₄ tetrahedra linked to form chains which have three times the width of those in pyroxene. These triple chains have a periodicity, 5.27 Å, along their lengths, and are bonded to each other laterally by the brucite layer made up by eight Mg cations and sandwiched between two inward pointing bands of tetrahedra. These units are linked back to back by cations (Mg or Na) in the Na(2) site and by a large cation (Na) at the Na(1) site.     

Lunar ilmenite (Refinement of the crystal structure)

The crystal structure of ilmenites from Mare Tranquillitatis and terrestrial basaltic rocks have been refined from X-ray data using least squares methods. The two structures are virtuallly identical both in structural parameters and relative degree of order. Occupation of Fe and Ti sites is highly ordered. The metal ions have low apparent charges (near 0.3) and formal oxidation states of Fe (II) and Ti (IV).     

The crystal structure of arsentsumebite, Pb2Cu[(As, S)O4]2(OH)

Summary The crystal structure of arsentsumebite, ideally, Pb₂Cu[(As, S)O₄]₂(OH), monoclinic, space group P2₁/m, a = 7.804(8), b = 5.890(6), c = 8.964(8) ?, β = 112.29(6)°, V = 381.2 ?³, Z = 2, d_calc. = 6.481 has been refined to R = 0.053 for 898 unique reflections with I> 2σ(I). Arsentsumebite belongs to the brackebuschite group of lead minerals with the general formula Pb₂ Me(XO₄)₂(Z) where Me = Cu²⁺, Mn²⁺, Zn²⁺, Fe²⁺, Fe³⁺; X = S, Cr, V, As, P; Z = OH, H₂O. Members of this group include tsumebite, Pb₂Cu(SO₄)(PO₄)(OH), vauquelinite, Pb₂Cu(CrO₄)(PO₄)(OH), brackebuschite, Pb₂ (Mn, Fe)(VO₄)₂(OH), arsenbracke buschite, Pb₂(Fe, Zn)(AsO₄)₂(OH, H₂O), fornacite, Pb₂Cu(AsO₄)(CrO₄)(OH), and feinglosite, Pb₂(Zn, Fe)[(As, S)O₄]₂(H₂O). Arsentsumebite and all other group members contain M = M–T chains where M = M means edge-sharing between MO₆ octahedra and M–T represents corner sharing between octahedra and XO₄ tetrahedra. A structural relationship exists to tsumcorite, Pb(Zn, Fe)₂(AsO₄)₂ (OH, H₂O)₂ and tsumcorite-group minerals Me(1)Me(2)₂(XO₄)₂(OH, H₂O)₂. Received June 24, 2000; revised version accepted February 8, 2001     

The crystal structure of sarkinite,Mn2AsO4(OH)

Summary Sarkinite is a basic manganese arsenate, Mn₂AsO₄(OH). The lattice parameters are:a=12.779 (2) Å,b=13.596 (2) Å,c=10.208 (2) Å, =108°53 (6). Space groupP2₁/a,Z=16. The crystal structure has been solved by direct methods from three-dimensional X-ray diffractometer data and refined by least-squares methods toR=0.052 for 3519 independent reflections. The crystal structure is built up by a three-dimensional framework of MnO₄(OH)₂ octahedra, MnO₄(OH) trigonal bipyramids and AsO₄ tetrahedra, as found in wagnerite. Isotypy of sarkinite with triploidite is confirmed.

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Die Kristallstruktur des Sarkinits, Mn₂AsO₄(OH)

Zusammenfassung Die Kristallstruktur des basischen Manganarsenates Sarkinit, Mn₂AsO₄(OH), mit den Gitterkonstantena=12,779 (2) Å,b=13,596 (2) Å,c=10,208 (2) Å, =108°53 (6). RaumgruppeP2₁/a,Z=16, wurde mit dreidimensionalen Röntgendiffraktometermessungen durch direkte Methoden gelöst und nach dem kleinste-Quadrate-Verfahren verfeinert (R=0,052 für 3519 unabhängige Reflexe). Die Struktur besteht aus einem dreidimensionalen Gerüst aus MnO₄(OH)₂-Oktaedern, trigonalen Bipyramiden von MnO₄(OH) und AsO₄-Tetraedern wie in Wagnerit. Die Isotypie von Sarkinit mit Triploidit wurde bestätigt.

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With 1 Figure     

Reversible hydration in synthetic mixite, BiCu6(OH)6(AsO4)3·nH2O (n≤3): hydration kinetics and crystal chemistry

 The presence of zeolitic water, with a reversible hydration behaviour, was determined by structural and kinetic studies on synthetic mixite BiCu₆(OH)₆(AsO₄)₃·nH₂O (n≤3). X-ray diffraction and infrared-spectroscopic investigations were performed on single crystals. Isothermal thermogravimetric experiments were carried out to determine the reaction kinetics of the de- and rehydration processes. The single-crystal structure refinement of a fully hydrated crystal yielded five partially occupied Ow positions (Ow=oxygen atom of a H₂O molecule) within the tube-like channels of the hexagonal [BiCu₆(OH)₆(AsO₄)₃] framework. For the partially dehydrated form, with n≈1, at least two of these sites were found to be occupied significantly. In addition, the structural investigations allowed two different intra-framework hydrogen bonds to be distinguished that are independent of the extra-framework water distribution and are responsible for the stability of the self-supporting framework. The kinetic analysis of the rate data in the 298–343K temperature range shows that the dehydration behaviour obeys a diffusion-controlled reaction mechanism with an empirical activation energy of E _a ^dehyd=54±4 kJ mol^–1. A two-stage process controls rehydration of which the individual steps were attributed to an initial surface-controlled (E _a ^hyd-I=6±1 kJ mol^–1) and subsequent diffusion-controlled reaction mechanism (E _a ^hyd-II=12±1 kJ mol^–1). The estimated hydration enthalpy of 42±5 kJ mol^–1 supports the distribution model of molecular water within the channels based on a purely hydrogen-bonded network. Received June 26, 1996 / Revised, accepted November 11, 1996     

Refinement of the crystal structure of bonshtedtite, Na3Fe(PO4)(CO3)

The crystal structure of bonshtedtite, Na₃Fe(PO₄)(CO₃) (monoclinic, P2₁/m, a = 5.137(4), b = 6.644(4), c = 8.908(6) Å, β = 90.554(14)°, V = 304.0(4) ų, Z = 2) has been refined to R ₁ = 0.041 on the basis of 1314 unique reflections. The structure is similar to that of other minerals of the bradleyite group. It is based on the [Fe(PO₄)(CO₃)]^3? layers oriented parallel to (001). The layers are formed by corner-sharing PO₄ tetrahedra and FeO₄(CO₃) complexes, where FeO₆ tetrahedra and CO₃ triangles are edge-shared. The topology of the octa-tetrahedral layer in bonshtedtite is similar to that of the autunite-group minerals, but it differs from the latter in terms of local topological properties.     

The crystal structure of meta-uranocircite II,Ba(UO2)2(PO4)2·6H2O

Summary The crystal structure of meta-uranocircite II, Ba(UO₂)₂(PO₄)₂·6H₂O, has been determined with a synthetic crystal using three-dimensional X-ray techniques.R=0.071 andR _w =0.064 were obtained for 1743 observed reflections. Ba(UO₂)₂(PO₄)₂·6H₂O is monoclinic, space groupP112₁/a, a=9.789,b=9.822,c=16.868 Å, =89.95° andZ=4. The structure consists of slightly corrugated UO₂PO₄ layers parallel (001). The layers are connected by Ba atoms and H₂O molecules. Uranium exhibits a (2+4)-coordination with mean U-O bond lengths of 1.78 Å for the uranyl oxygens and 2.28 Å for the phosphate oxygens. The average P-O bond length is 1.52 Å. Barium is coordinated by two uranyl oxygens. two phosphate oxygens and five water molecules. The Ba–O bond lengths vary from 2.74 to 3.11 Å. Two of the six water molecules of the formula are not bonded to barium.

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Die Kristallstruktur des Meta-Uranocircits II, Ba(UO₂)₂(PO₄)₂·6H₂O

Zusammenfassung Die Kristallstruktur des Meta-Uranocircits II, Ba(UO₂)₂(PO₄)₂·6H₂O, wurde anhand eines künstlichen Kristalls mit dreidimensionalen Röntgendaten bearbeitet und für 1743 Reflexe aufR=0,071 undR _w =0,064 verfeinert. Ba(UO₂)₂(PO₄)₂·6H₂O kristallisiert monoklin in der RaumgruppeP112₁/a, a=9,789,b=9,882,c=16,868 Å, =89,95° und einem Zellinhalt von vier Formeleinheiten. Die Struktur besteht aus schwach gewellten UO₂PO₄-Schichten parallel (001), die durch Ba-Atome und H₂O-Moleküle miteinander verknüpft sind. Uran besitzt oktaedrische (2+4)-Koordination mit mittleren U-O-Abständen von 1,78 Å für die Uranylsauerstoffatome und 2,28 Å für die Phosphatsauerstoffatome. Die P-O-Abstände der Phosphattetraeder messen im Mittel 1.52 Å. Barium ist von je zwei Uranyl- und Phosphatsauerstoffatomen sowie von fünf Wassermolekülen koordiniert. Die Ba-O-Abstände betragen 2,74–3,11 Å. Von den sechs H₂O-Molekülen der Formel sind zwei nicht an Barium gebunden.

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With 3 Figures     

The crystal structure of Liebigite,Ca2UO2(CO3)3·∼11H2O

Summary The crystal structure of liebigite, previously only incompletely known from a short note, has been determined from X-ray 4-circle diffractometer data and refined toR=0.030 for 3005 observed reflections. Liebigite from Joachimsthal, Böhmen, was used. It was found to crystallize in the polar orthorhombic space groupBba2–C _2v ¹⁷ witha=16.699(3),b=17.557(3),c=13.697(3) Å,V=4016 ų and a cell content of 8 Ca₂UO₂(CO₃)₃·11H₂O. The structure contains UO₂(CO₃)₃ units which are linked by two kinds of CaO₄(H₂O)₄ polyhedra and one kind of CaO₃(H₂O)₄ polyhedron to form puckered Ca₂UO₂(CO₃)₃·8H₂O layers parallel to (010). These layers are interconnected only by hydrogen bonds, both directly as well as via three additional interlayer H₂O molecules, two of which show positional disorder.

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Die Kristallstruktur des Liebigits, Ca₂UO₂(CO₃)₃·11H₂O

Zusammenfassung Die Kristallstruktur des Minerals Liebigit, die bis jetzt nur unzureichend bekannt war, wurde mit Röntgen-Vierkreisdiffraktometer-Daten bestimmt und für 3005 beobachtete Reflexe aufR=0,030 verfeinert. Der untersuchte, von Joachimsthal, Böhmen, stammende Liebigit kristallisiert in der polaren rhombischen RaumgruppeBba2–C _2v ¹⁷ mita=16,699(3),b=17,557(3),c=13,697(3) Å,V=4016 ų und einem Zellinhalt von 8 Ca₂UO₂(CO₃)₃·11H₂O. Die Struktur enthält UO₂(CO₃)₃-Gruppen, die durch zwei Arten von CaO₄(H₂O)₄-Polyedern und eine Art von CaO₃(H₂O)₄-Polyedern zu buckeligen Ca₂UO₂(CO₃)₃·8H₂O-Schichten parallel (010) verknüpft sind. Diese Schichten sind nur durch Wasserstoffbrücken verbunden, und zwar sowohl direkt als auch mittels dreier zusätzlicher freier Wassermoleküle, von denen zwei eine Lagenfehlordnung aufweisen.

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With 3 Figures     

Refinement of the mangan-neptunite crystal structure

The crystal structure of mangan-neptunite, a manganese analogue of neptunite, has been refined in two space groups (Cc and C2/c). The mineral is monoclinic, with the correct space group Cc; the unit-cell dimensions are: a = 16.4821(6), b = 12.5195(4), c = 10.0292(3) Å, β = 115.474(1)°, and V = 1868.31 ų. The crystal structure has been refined to R ₁ = 0.0307 (wR ₂ = 0.0901) on the basis of 4892 observed reflections with |F _hkl | ≥ 4σ|F _hkl |. The most plausible acentric model is caused by the Ti- and (Fe, Mn, Mg)-ordering in the structure. Ti-octahedrons are strongly distorted and consist of short bond Ti-O (1.7 Å), one long bond (2.2 Å), and four equal bonds (2.0 Å). Fe-octahedrons are regularly shaped, with all Fe-O bonds being approximately identical.     

Stabilization of complex ions by the crystal field: CO 3 2− , NO 3 − , O 3 − , [(OH)4]4−, [(OH)3F]4−, [(OH)2F2]4−

According to Koopmans' theorem, only the electrons associated with molecular levels of negative energy are stable. Many ions which cannot exist in the isolated state because certain occupied levels are positive, become stable in crystals under the stabilization effect arising from the crystal field. As examples, we have studied CO ₃ ^2? in calcite, NO ₃ ^? in NaNO₃, and several natural limpurities: O ₃ ^? in fluorite, [(OH)₄]^4?, [(OH)₃F]^4? and [(OH)₂F₂]^4? in zircon and thorite, by means of the molecular self-consistent field, the crystal field being simulated by point charges. As expected, all the energies corresponding to the occupied levels are negative within the crystal field, contrary to what occurs in the isolated state. Informations concerning the structure and the size of the critical germ are obtained for CaCO₃ and NaNO₃.     

The crystal structure of walpurgite, (UO2)Bi4O4(AsO4)2·2H2O

Summary The crystal structure of walpurgite has been determined from three-dimensional X-ray single crystal data and has been refined toR=0.041 for 1381 independent reflections using a crystal from Schneeberg, Sachsen. Walpurgite crystallizes triclinic, space group , witha=7.135 (2),b=10.426 (4),c=5.494 (1) Å, =101 47 (2), =110.82 (2), =88.20 (2)^o andV-374 A³. Cell content and chemical formula are (UO₂)Bi₄O₄(AsO₄)₂·2H₂O, which is one H₂O less than previously known. The structure consists of complex layers Bi₄O₄(AsO₄)₂·2H₂O extending parallel to (010). Each layer is built up from a network of bismuth and oxygen atoms, to both sides of which AsO₄ groups and water molecules are attached. (UO₂)O₄ octahedra link the layers parallel tob via the AsO₄ groups and thus simultaneously from UO₂(AsO₄)₂ chains parallel toc. The two independent Bi atoms are trivalent and form pronounced one-sided BiO polyhedra: 4–5 oxygens are at distances of 2.11–2.48 Å, 4 additional oxygens are at distances of 2.63–3.35 Å.

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Die Kristallstruktur des Walpurgins, (UO₂)Bi₄O₄(AsO₄)₂·2H₂O

Zusammenfassung Die Kristallstruktur des Walpurgins wurde anhand eines Kristalls von Schneeberg, Sachsen, mit dreidimensionalen Röntgen-Einkristalldaten bestimmt und für 1381 Reflexe aufR=0,041 verfeinert. Walpurgin kristallisiert triklin, Raumgruppe ,a=7,135 (2),b=10,426 (4),c=5,494 (1) Å, =101,47 (2), =110,82 (2), =88,20 (2)^o undV=374 ų. Zellinhalt und chemische Formel lauten (UO₂)Bi₄O₄(AsO₄)₂·2H₂O, das ist um ein H₂O-Molekül weniger als bislang bekannt. Die Struktur enthält kompliziert gebaute Bi₄O₄(AsO₄)₂·2H₂O-Schichten, die sich parallel (010) erstrecken. Jede Schicht besteht aus einem Netz von Wismut- und Sauerstoffatomen, an das zu beiden Seiten AsO₄-Gruppen und H₂O-Moleküle anknüpfen. (UO₂)O₄-Oktaeder verbinden die Schichten über die AsO₄-Gruppen parallel zub und bilden so gleichzeitig (UO₂)(AsO₄)₂-Ketten parallel zuc aus. Die zwei unabhängigen, dreiwertigen Wismutatome des Walpurgins sind von 4–5 Sauerstoffatomen in Abständen von 2,11–2,48Å einseitig koordiniert und darüber hinaus noch von vier weiteren Sauerstoffatomen in Abständen von 2,63–3,35 Å umgeben.

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With 4 Figures     

Refinement of the crystal structure of beryllonite,NaBePO4

Summary The refined lattice parameters of beryllonite are:a=8.178 (3) Å,b=7.818 (2) Å,c=14.114 (6) Å, =90.00° (2); space groupP2₁/n,Z=12. Integrated Weissenberg photographs were taken by using CuK radiation and multiple film packs. The anisotropic refinement of the crystal structure by means of least-square methods gave a finalR value of 0.063 for the 1388 observed reflections. In the crystal structure PO₄ and BeO₄ tetrahedra, linked by shared oxygen atoms in a three-dimensional network, form pseudo-ditrigonal rings perpendicular to theb axis. The independent Na atoms lying in the channels formed by the rings are coordinated as an irregular nine-cornered polyhedron and as distorted octahedra.

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Verfeinerung der Kristallstruktur des Beryllonits,NaBePO ₄

Zusammenfassung Verfeinerte Gitterkonstanten des Beryllonits lauten:a=8,178 (3) Å,b=7,818 (2) Å,c=14,114 (6) Å, =90,00 (2)°; Raumgruppe:P2₁/n,Z=12. Integrierte Weissenbergaufnahmen wurden mit CuK-Strahlung und multiplen Filmpaketen aufgenommen. Die anisotrope Verfeinerung der Kristallstruktur nach der Methode der kleinsten Quadrate ergab für 1388 beob. Reflexe einen abschließendenR-Wert von 0,063. In der Kristallstruktur bilden PO₄-und BeO₄-Tetraeder, die über gemeinsame Sauerstoffe zu einem dreidimensionalen Gerüst verknüpft sind, pseudo-ditrigonale Ringe senkrecht zurb-Achse. Die kristallographisch unabhängigen Arten von Na-Atomen, welche in den aus Ringen gebildeten Kanälen liegen, sind in der Form eines unregelmäßigen neuneckigen Polyeders bzw. in der Form verzerrter Oktaeder koordiniert.

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With 2 Figures