Kristall- und Molekülstruktur von Arsen-tris(trifluoracetat)

Zusammenfassung Arsen-tris(trifluoracetat) (1) kristallisiert monoklin in der Raumgruppe Cc mita=1229.3,b=1697.9,c=1243.5 pm, =110.01° undZ=8. Die Trifluoracetatanionen fungieren gegenüber As als zweizähnige Liganden und verknüpfen die beiden kristallographisch unabhängigen Moleküle zusätzlich intermolekular. As erreicht dadurch gegenüber O die Koordinationszahl 3+3(+2). Die Elementarzelle enthält zwei Sätze von chirameren Molekülen.

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Crystal and molecular structure of arsenictris(trifluoroacetate)

Summary Arsenictris(trifluoroacetate) (1) crystallizes monoclinic in the space group Cc witha=1229.3,b=1697.9,c=1243.5 pm, =110.01°, andZ=8. The trifluoroacetic acid ions acts as chelating ligands. Additionally they are bridging crystallographic independent molecules. As has a coordination number of 3+3(+2). The unit cell contains two sets of chirameres.

     

Einkristallstrukturanalyse vonBis(trimethylsilyl)peroxid

Zusammenfassung Bis(trimethylsilyl)peroxid wurde aus Trimethylchlorsilan, Wasserstoffperoxid und 1,4-Diazobicyclo[2.2.2]octan dargestellt. Ein Einkristall wurdein situ auf einem Vierkreisdiffraktometer gezüchtet und mittels Einkristallstrukturanalyse charakterisiert (T=193(2) K, 2522 Reflexe, P2₁/c;a=606.7(1) pm,b=1098.5(1) pm,c=858.2(1) pm, =101.88(2)°,Z=2,R=0.045). Die Konformation des Moleküls im Kristall ist durch C-H...O-Brücken bestimmt.

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Crystal structure ofbis(trimethylsilyl)peroxide

Summary Bis(trimethylsilyl)peroxide has been prepared from trimethylchlorsilane, hydrogen peroxide, and 1,4-diazobicyclo[2.2.2]octane. Crystal growth was achievedin situ on a diffractometer and characterized by crystal structure analysis (T=193(2) K, 2522 reflections, P2₁/c;a=606.7(1) pm,b=1098.5(1) pm,c=858.2(1) pm, =101.88(2)°,Z=2,R=0.045). The molecule's conformation in the crystalline solid is determined by C-H...O-bridges.

     

The crystal structures ofbis-{(2-benzotrifluoride)-[(2-oxo-3H-naphth-3-ylidene)-methyl]-aminato} Copper(II) andbis-{(3-benzotrifluoride)-[(2-oxo-3H-naphth-3-ylidene)-methyl]-aminato} Copper(II)

Summary TheSchiff base ligands 3-[(2-benzotrifluoride)-2-hydroxy-3H-naphth-3-ylidene)-methyl] aldamine (1) and 3-[(3-benzotrifluoride)-2-hydroxy-3H-naphth-3-ylidene)-methyl] aldamine (2) and their corresponding Cu(II) complexes (I, II) were synthesized. The crystal structures ofbis-{(2-benzotrifluoride)-[(2-oxo-3H-naphth-3-ylidene)]-methyl]-aminato} Copper(II) (I) andbis-{(3-benzotrifluoride)-[(2-oxo-3H-naphth-3-ylidene)-methyl]-aminato} Copper(II) (II) were determined. CompoundI crystallizes in the triclinic crystal system (a=12.561(3),b=16.211(4),c=8.007(2) Å, =96.29(2), =101.42(2), =97.10(2)°, space group ,Z=2); compoundII crystallizes in the monoclinic crystal system (a=5.064(2),b=19.172(4),c=15.111(3) Å, =95.05(2)°, space group P2₁/c,Z=2). The X-ray diffraction study shows that the geometry around the metal atom is square planar for both copper complexes.

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Kristallstruktur vonbis-{(2-Benzotrifluorid)-[(2-oxo-3H-naphth-3-yliden)-methyl]-aminato}-Kupfer(II) undbis-{(3-Benzotrifluorid)-[(2-oxo-3H-naphth-3-yliden)-methyl]-aminato}-Kupfer(II)

Zusammenfassung DieSchiffschen Basen 3-[(2-Benzotrifluorid)-2-hydroxy-3H-naphth-3-yliden)-methyl]-aldamin (1) und 3-[(3-Benzotrifluorid)-2-hydroxy-3H-naphth-3-yliden)-methyl]-aldamin (2) sowie ihre entsprechenden Cu(II)-Komplexe (I,II) wurden synthetisiert und ihre Struktur im Kristall bestimmt. VerbindungI kristallisiert triklin (a=15.561(3),b=16.211(4),c=8.007(2) Å, =96.29(2), =101.42(2), =97.10(2)°, Raumgruppe ,Z=2); VerbindungII kristallisiert monoklin (a=5.064(2),b=19.172(4),c=15.111(3) Å, =95.05(2)°, Raumgruppe P2₁/c,Z=2). Aus der Röntgenstrukturanalyse ergibt sich eine quadratisch planare Geometrie der Komplexe.

     

Die Kristallstruktur eines polynuklearen Co(II)-Komplexes in Cs2[Co3(N3)8]

Cs₂[Co₃(N₃)₈] crystallizes monoclinic,a=1 123.8 (3),b=568.4 (2),c=1 542.6 (4) pm, =107.37 (2)°, space group P2₁/n,Z=2. The crystal structure was determined by single crystal X-ray diffraction,R _w=0.069. Coatoms are coordinated octahedrally to six azide groups and form polynuclear complexes of composition [Co₃(N₃)₈]^2–. The complex anions share edges and are connected to infinite chains running along theb-axis direction. Cesium is irregularly surrounded by azide groups.

     

Antimontribenzoat

Zusammenfassung Das -Isomer des Antimontribenzoats kristallisiert rhomboedrisch (hexagonale Aufstellung) in der Raumgruppe R3 mita=1944.0 pm,c=422.3 pm undZ=3. Die Moleküle sind parallel zu 001 gestapelt. Sb hat gegenüber O die Koordinationszahl 3+3 (Sb-O: 208 bzw. 256 pm).

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Antimonytribenzoate

Summary The isomer of (C₆H₅CO₂)₃Sb crystallizes rhombohedrally (hexagonal axes) in the space group R3 witha=1944.0 pm,c=422.3 pm, andZ=3. The molecules are stacked parallel to 001; Sb has a coordination number of 3+3 (Sb-O: 208 and 256 pm, resp.).

     

Crystal structure of Ag2TeS3 and Na(Na1−x Ag x )TeS3 (x≈0.5) and the geometry of Te(IV)S3 polyhedra

Summary Structural data determined by single crystal X-ray experiments (T=300 K) are reported for Ag₂TeS₃ (monoclinic, Cc-C _s ⁴ ;a=6.783(1),b=11.567(2),c=7.693(1) Å; =114.44(1)°;Z=4;R=0.044) and for Na(Na_1–x Ag _x )TeS₃ x0.5; monoclinic, P2₁/c-C _2h ⁵ ;a=5.761(9),b=12.171(8),c=8.342(4) Å; =92.26(6)°;Z=4;R=0.030). In both compounds the atomic arrangements are characterized by isolated trigonal pyramidal TeS₃ polyhedra, irregularly coordinated Ag and Na atoms forming AgS₄ and (Na, Ag)S₄ polyhedra, and slightly distorted NaS₆ octahedra. Crystals of both compounds were synthesized under moderate hydrothermal conditions from an equimolar mixture of the elements in concentrated aqueous ammonia and 5N NaOH solution, respectively.

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Kristallstruktur von Ag₂TeS₃ und Na(Na_1–x Ag _x )TeS₃ (x0.5) nebst einem Vergleich der Geometrie von TeS₃-Gruppen

Zusammenfassung Es wird über die mittels Röntgenbeugungsexperimenten an Einkristallen bei 300 K bestimmten Strukturen von Ag₂TeS₃ (monoklin Cc-C _s ⁴ ;a=6.783(1),b=11.567(2),c=7.693(1) Å; =114.44(1)°;Z=4;R=0.044) und Na(Na_1–x Ag _x )TeS₃ (x0.5; monoklin, P2₁/c-C _2h ⁵ ;a=5.761(9),b=12.171(8),c=8.342(4)Å; =92.26(6)°;Z=4;R=0.030) berichtet. In beiden Verbindungen ist die Atomanordnung durch isolierte trigonal-pyramidale TeS₃-Polyeder, unregelmäßig koordinierte Ag- und Na-Atome, AgS₄- und (Na, Ag)S₄-Polyeder bildend, sowie leicht verzerrte NaS₆-Oktaeder charakterisiert. Kristalle der beiden Verbindungen wurden unter moderaten Hydrothermalbedingungen aus einem equimolaren Gemenge der Elemente und konzentrierter wäßriger Ammoniaklösung bzw. 5N NaOH-Lösung gezüchtet.

     

The crystal structures ofα,ω-diaminoalkane-cadmium(II) tetracyanonickelate(II) — Aromatic molecule inclusion compounds. VII: Three-dimensional host structures built ofcatena-[cadmium(II) tetra-μ-cyanonickelate(II)] layers and 1,3-diaminopropane, 1,5-diaminopentane or 1,7-diaminoheptane pillar

The crystal structures of four novel Hofmann-diam-type clathrates [Cd(tn)Ni(CN)₄]·1.72(o-MeC₆H₄NH₂),3-o, [Cd(tn)Ni(CN)₄]·0.5(m-ClC₆H₄NH₂),3-m, [Cd(daptn)Ni(CN)₄]·1.5(p-MeC₆H₄NH₂),5-p and [Cd(dahpn)Ni(CN)₄]·1.5(2-MeC₉H₆N),7-q have been determined by single crystal X-ray diffraction method [tn:n=3, daptn:n=5, dahpn:n=7 for NH₂(CH₂) _n NH₂.3-o crystallizes in the monoclinic space groupP2/m,a=7.538(2),b=9.314(5),c=7.670(2) Å, =91.03(2)°,Z=1,R=0.047 for 1252 reflections;3-m: orthorhombicPbam,a=12.1714(7),b=15.798(1),c=7.737(1) Å,Z=4,R=0.044 for 1871;5-p: monoclinicP2₁/a,a=13.736(3),b=22.014(4),c=7.762(3) Å, =91.04(3)°,Z=4,R=0.047 for 5281; and7-q: orthorhombicPbam,a=13.599(2),b=27.938(4),c=7.619(2) Å,Z=4,R=0.054 for 3098. Their host structures are topologically the same to those of the previously reported Hofmann-diam-type clathrates: the two-dimensional [CdNi(CN)₄] networks are spanned by NH₂(CH₂) _n NH₂ at every Cd atom to build up the three-dimensional hosts. The number of cavities available for the guest is regulated by the deformation of the 2D networks and the diamine ligand in the host structure. Supplementary Data relating to this article are deposited with the British Library as Supplementary Publication No. SUP 82192 (37 pages).     

Neutral molecule/crown ether interactions 5. Comparison of the C−H acidic interactions of nitromethane and acetonitrile with 18-crown-6 and dibenzo-18-crown-6. Crystal structures of dibenzo-18-crown-6·2 CH3NO2 and dibenzo-18-crown-6·2 CH3CN

Complete structural characterization of dibenzo-18-crown-6·2 CH₃NO₂ and dibenzo-18-crown-6·2 CH₃CN have been carried out, including location and refinement of the methyl hydrogen atoms. Dibenzo-18-crown-6·2 CH₃NO₂ is monoclinic,P2₁/c, with (at –150°C)a=9.573(2),b=14.636(2),c=33.471(7) Å, =93.77(2)°, andD _calc=1.37 g cm^–3 forZ=8. Interactions between the solvent methyl groups and the crown ethers and other solvent nitro groups associate the 1 : 2 complexes into polymeric chains alongb. The acetonitrile adduct exists as discreet 1 : 2 complexes in the solid state with C–H...O interactions exlusively to the ether. This complex is triclinic,P 1, with (at –150°C)a=9.458(6),b=9.570(5),c=14.404(5) Å, =73.18(4), =79.85(5), =66.82(6)°, andD _calc=1.28 g cm^–3 forZ=2. Supplementary Data relating to this article are deposited with the British Library as Supplementary Publication No. SUP 82070 (22 pages).For part 4, see reference [1].     

The polyiodide salts: Pyridinium pentaiodide;β-naphthylammonium pentaiodide; andN-methyl-γ-picolinium heptaiodide. Structures with channel inclusion features

The crystal structures of three polyiodode salts are reported (pyridinium pentaiodide, monoclinic,P2 ₁/m,a=9.221(5),b=12.918(5),c=6.026(4) Å, =103.60(7)^o,Z=2,R _F=0.087 for 1187 intensities; -naphthyl-ammonium pentaiodide, triclinic,173-1,a=10.390(5),b=9.502(5),c=4.462(3) Å, =99.19(7), =90.40(7),=108.49(8)^o,Z=2,R _F=0.059 for 1319 intensities;N-methyl--picolinium heptaiodide, monoclinic,C2/c,a=19.315(7),b=12.714(5),c=8.442(4) Å, =107.26(7)^o,Z=4,R _F=0.065 for 1336 intensities). All three structures can be described as having channel inclusion features; the cations are contained in channels in polyiodide frameworks based on different arrangements of I₂ molecules and I ₃ ^– anions. This structural type is the converse of the more widespread kind where polyiodide anions are contained in an organic matrix (e.g., cyclodextrin polyiodides). Supplementary Data relating to this article are deposited with the British Library as Supplementary Publication No. SUP 82016 (30 pages).Part X of Crystal Structures of Polyiodide Salts and Complexes. For Part IX, see F. H. Herbstein, G. M. Reisner, and W. Schwotzer,Acta Crystallogr. C, accepted for publication, 1984     

Kristallstrukturen von drei Addukten des Zinkazides mit Dimethylpyridinen

Summary Three adducts of zinc azide with 2,4-/3,4- and 3,5-dimethylpyridine (DMP), respectively, were prepared and the crystal structures determined by single crystal X-ray diffraction methods. The three compounds crystallize in the monoclinic space group P2₁/c withZ=4:Zn(N₃)₂·2,4-DMP at 300 (2) K:a=1 098.6(4),b=1 600.2(6),c=608.8(3) pm, =102.47(3)°;R=0.071 (R _w =0.056).Zn(N₃)₂·3,4-DMP at 103 (3) K:a=1 102.1(3),b=1 649.0(4),c=611.8(1) pm, =104.54(2)°;R=0.055 (R _w =0.051).Zn(N₃)₂·3,5-DMP at 97 (3) K:a=602.1(2),b=2 037.9(7),c=853.8(3) pm, =90.77(3)°;R=0.069 (R _w =0.055).The molecular geometry is similar for the three adducts, but the packing of theDMP-molecules is different. The zinc atoms are surrounded by five nitrogen atoms, four belonging to the azide groups and one to theDMP-adduct. The trigonal bipyramidal shaped ZnN₅-polyhedra share common edges to form chains.

     

Direct Evidence for Metal Triangle Mobility within a Relatively Rigid Ligand Polytope: Dynamic Disorder in the X-Ray Crystal Structures of Ru3(CO)11(L), L=CN t Bu, PMe3, and Ru3(CO)9{P(OMe)3}3

The disorder in the X-ray crystal structures of Ru₃(CO)₁₁(L), L=CN ^t Bu 1 and PMe₃ 3 has been re-examined. Crystallographic data for 1 at 100 K: C₁₆H₉NO₁₁Ru₃, space group P2₁/n, a=11.796(5), b=11.748(2), c=16.040(7) Å, =109.81(3)°, Z=4, 6077 reflections, R=0.028. For 3 at 223 K: C₁₄H₉O₁₁PRu₃, space group P2₁/n, a=8.5971(15), b=12.391(7), c=40.345(8) Å, =94.43(2)°, Z=8, 7966 reflections, R=0.031. The disorder present in 1 and 3 at room temperature disappears reversibly on cooling, showing that it is dynamic in origin. The ligator atoms of the isonitrile and phosphine ligands move by a maximum of 0.8 Å, indicating that the whole cluster does not rotate intact within the crystal lattice, but rather that the Ru₃ triangle effectively oscillates within a relatively rigid ligand polyhedron. The crystal structure of Ru₃(CO)₉{P(OMe)_{3 3}} 7, which crystallizes in triclinic (7-t) and monoclinic (7-m) modifications is also reported. Both modifications have two independent molecules in the asymmetric unit, and both modifications display dynamic disorder in the metal framework. Crystalllographic data for 7-t at 173 K: C₁₈H₂₇O₁₈P₃Ru₃, space group P-1, a=11.8085(18), b=15.915(2), c=17.350(3) Å, =99.929(14), =101.811(14), =90.630(12)°, Z=4, 11242 reflections, R=0.048. For 7-m at 120 K: C₁₈H₂₇O₁₈P₃Ru₃, space group P2₁/c, a=11.708(8), b=15.922(5), c=33.950(10) Å, =99.29(4), Z=8, 10191 reflections, R=0.027.     

Crystal structure of an uncomplexed 25-crown-7 comprising one 2,6-pyridino and two 1,4-benzo condensations

Single crystal X-ray analysis of the uncomplexed crown macroring 1 is reported. Crystals are triclinic, , witha=10.809(1),b=10.945(1),c=10.256(1) Å, =107.85(1), =104.15(1), =87.27(1)°,D _c=1.318 g cm^–3,Z=2. Three torsion angles in the macrocycle take upgauche conformations in contrast to the usualanti conformation. The crystal structure is stabilized by intramolecular van der Waals forces and weak C–H...O and C–H...N hydrogen bond attractions. Stacking of pyridine rings is a noticeable packing feature in the crystal lattice. Supplementary Data relating to this article are deposited with the British Library as Supplementary Publication No. SUP 82168 (6 pages).Macroring Uncharged Molecule Complexation. Part 20. For Part 19 of this series see Ref. [1].     

Urea-water-anion Lattices Part 1. Crystal structures of (C2H5)4N+X−·(NH2)2CO·2 H2O (X=Cl,Br, CN), an isomorphous series of layer-type inclusion complexes

The title ternary complexes (1, X=Cl;2, X=Br;3, X=CN) have been prepared and characterized by X-ray crystallography. Crystal data: space groupP2₁/n,Z=4;1,a=7.505(2),b=14.556(4),c=14.453(3) Å, =98.13(2)^o, andR _F=0.088 for 1831 observed MoK data;2,a=7.483(1),b=14.643(6),c=14.443 Å, =98.25(2)^o, andR _F=0.113 for 923 data;3,a=7.490(2),b=14.646(5),c=14.594(5) Å, =98.85(5)^o, andR _F=0.082 for 915 data. In the isomorphous crystal structure of1 and2, ordered (C₂H₅)₄N⁺ cations are sandwiched between puckered layers matching the (020) family of planes, each being constructed from the cross-linking of planar zigzag chains of hydrogen-bonded urea molecules by the water molecules and halide ions. Compound3 has the same structure except that its cyanide group is disordered. Supplementary Data relating to this article are deposited with the British Library as Supplementary Publication No. SUP 82066 (30 pages).Operated under contract DE-AC02-76CH00016 with the U.S. Department of Energy, Office of Basic Energy Science.     

Synthesis and Structure of Complexes Formed in the CuCl2–Cu–N-allylquinolinium Chloride System

The crystals of [C₉H₇N(C₃H₅)]₂Cu^IICl₄(IV) were obtained through ac electrochemical synthesis using CuCl₂· 2H₂O, N-allylquinolinium chloride, and copper electrodes in an ethanol-benzene medium. These crystals transformed with time into crystals of the [C₉H₇N(C₃H₅)][Cu^IICl₃(C₉H₇N)] complex (V). When tin(II) chloride was added to the initial reagents, the [C₉H₇N(C₃H₅)]Cu^I ₂Cl₃complex (VI) was obtained. The X-ray diffraction analysis (DARCh-1 autodiffractometer, MoK radiation, Zr filter) indicated that complexes IVand Vcrystallize in the triclinic system: space group P ; for IV, a= 12.817(4), b= 10.435(3), c= 9.606(3) Å, = 97.94(2)°, = 107.28(2)°, = 95.99(2)°, V= 1200.6(6) ų, Z= 2; for V, a= 16.992(5), b= 8.243(2), c= 7.345(3) Å, = 91.89(3)°, = 91.19(3)°, = 88.18(3)°, V= 1027.5(6) ų, Z= 2. Crystals VIare monoclinic, space group P2₁/n, a= 13.578(5), b= 15.079(4), c= 6.953(4) Å, = 105.08(4)°, V= 1370.6(10) ų, Z= 4. Structures IV–VIconsist of N-allylquinolinium cations and different anions: isolated [CuCl₄]^2–tetrahedrons (IV), [C₉H₇NCuCl₃]^–tetrahedrons (V) containing a quinoline molecule, and a polymer chain |[Cu^I ₄Cl₆]^2–} _n (VI) in which two independent metal atoms have trigonal-pyramidal and planar-trigonal environments. The C=C bond of the allyl group is not involved in cooordination with the Cu(I) atom.     

Hydrothermal Syntheses and Structural Characterization of One-Dimensional [Cu4Br2I3(C12H8N2)2] n and Molecular Cu3Br3(C12H8N2)2

The hydrothermal reactions of CuBr₂, CuX (X=Br, I), and phen (phen=1,10-phenanthroline, C₁₂H₈N₂) have lead to the syntheses of two novel complexes of one-dimensional [Cu₄Br₂I₃(phen)₂] _n 1 and trinuclear discrete cluster Cu₃Br₃(phen)₂ 2. Both compounds were characterized by singe-crystal X-ray diffraction. Crystal data for 1. Monoclinic, space group P2 ₁/c with a=14.054(3) Å, b=13.700(3) Å, c=15.920(3) Å, =114.16(3)°, Z=2; 2. Monoclinic, space group C2/c with a=10.040(2) Å, b=14.516(3) Å, c=16.319(3) Å, =94.29(3)°, Z=6.     

Crystal structure and vibrational spectra of pyridine-2,6-dithio-carbomethylamide

The crystal structure of Pyridine-2,6-dithio-carbomethylamide (PDTA) is described: C₉H₁₁N₃S₂, monoclinic, P2₁/c,Z=4,a=6.000 (1) Å,b=8.840 (1) Å,c=21.452 (1) Å, =105.47 (1)^o,d _x=1.47 gcm^–3. The structure was solved with direct methods and refined to a conventionalR-factor of 0.047. The molecule is nearly planar in the crystal. There are possibly weak intramolecular H-bonds between the two amide nitrogens and the pyridine nitrogen and intermolecular H-bonds between two amide nitrogens and one thioamide sulfur atom. The IR andRaman spectra ofPDTA and deuteratedPDTA are discussed.

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Kristallstruktur und Schwingungsspektren von Pyridin-2,6-dithiocarbomethylamid

Zusammenfassung Die Kristallstruktur von Pyridin-2,6-dithiocarbomethylamid (PDTA) wurde bestimmt: C₉H₁₁N₃S₂, monoklin, P2₁/c,Z=4,a=6,000 (1) Å,b=8,840 (1) Å,c=21,452 (1) Å, =105,47 (1)^o,d _x=1,47 gcm^–3. Das Phasenproblem wurde mittels direkter Methoden gelöst und die Struktur bis zu einemR-Faktor vonR=0,047 verfeinert. Das Molekül ist im Kristall nahezu planar. Das Vorliegen schwacher intramolekularer Wasserstoffbrücken zwischen den beiden Thioamid-Stickstoffatomen und dem Pyridinstickstoff sowie intermolekularer Wasserstoffbrücken zwischen Thioamid-Stickstoff- und Thioamid-Schwefelatomen wird postuliert. IR- undRaman-Spektren vonPDTA und deuteriertemPDTA werden diskutiert.

     

Crystal structure of K3SbS4·4 1/2 H2O

Summary The crystal structure of K₃SbS₄·4 1/2 H₂O, monoclinic, P2₁/c-C ₅ ^2h ,a=12.732(3),b=7.720(2),c=13.928(4) Å, =90.19(1)°,V=1369.0(5) ų,Z=4, has been determined from X-ray single crystal data and refined by least-squares methods toR=0.031 for 3 024 reflections. The structure is built up from KS_{4 – 5}(H₂O)_{3 – 5} polyhedra and SbS₄ tetrahedra (Sb-S=2.327 Å) which are three-dimensionally linked. The water molecules are bonded to two or three K⁺ ions and form exclusively O-H ... S-type hydrogen bonds. One of the five crystallographically different water molecule sites is due to space limitations only half occupied.

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Die Kristallstruktur von K₃SbS₄·4 1/2 H₂O

Zusammenfassung Die Kristallstruktur von K₃SbS₄·4 1/2 H₂O, monoklin, P2₁/c-C ₅ ^2h ,a=12.732(3),b=7.720(2),c=13.928(4) Å, =90.19(1)°,V=1369.0(5) ų,Z=4, wurde mit Röntgen-Einkristalldaten bestimmt und für 3 024 Reflexe aufR=0.031 verfeinert. Die Kristallstruktur ist aus dreidimensional verknüpften KS_{4 – 5}(H₂O)_{3 – 5}-Polyedern und SbS₄-Tetraedern (Sb-S=2.327 Å) aufgebaut. Die Wassermoleküle sind an zwei bis drei Kaliumionen gebunden und bilden ausschließlich Wasserstoffbrücken des Typs O-H...S aus. Eine der fünf kristallographisch verschiedenen H₂O-Lagen ist aus Platzmangel nur zur Hälfte besetzt.

     

Über die Darstellung der 7R-Oxirane von 5Z- und 5E-10-Oxo-19-norcholecalciferol

Summary The two title compounds12b and13b have been prepared by direct oxidation of the corresponding 10-oxo-19-norcolcalciferol derivatives3c and4c withMCPBA. The generation of12b and13b by treatment of the ⁷ epoxidized ethylisoxazolin adducts of 5Z- and 5E-cholecalciferol8a,8b and9a,9b with Mo(CO)₆ failed, since besides the retroaldol cleavage of the heterocycle a deoxygenation of the oxirane with retention of configuration to the ⁷ double bond occurs.

     

Kristallstruktur und thermisches Verhalten von Tetrakaliumcyclo-tetraphosphat(V)-Dihydrat, (KPO3)4·2H2O

The crystal structure of (KPO₃)₄ · 2H₂O was solved by direct methods andFourier-syntheses (triclinic; P ;a=1 114.9 (2),b=821.9 (2),c=815.7 (3) pm; =88,88 (2), =84.51 (2), =82.70 (2)°;Z=2; 5910 unique reflections;R=0.052). The cyclic anions exhibit point symmetry S₄ with four terminal oxygens in axial and four in equatorial position. Thermal investigations (DTA, TGA, X-Ray-methods) show that the dehydration occurs in two steps. The anhydrous form of (KPO₃)₄ is stable above 230 °C and undergoes a second order phase transition which is complete at 515±5 °C.

     

Cu2O(SO4), dolerophanite: Refinement of the crystal structure,with a comparison of [O Cu(II)4] tetrahedra in inorganic compounds

The refinement of the crystal structure of Cu₂O(SO₄), dolerophanite, [a=9.370 (1) Å,b=6.319 (1) Å,c=7.639 (1) Å, =122.34 (1)°; space group C 2/m;Z=4;R=0.035] confirmed the trigonal dipyramidal coordination of one Cu(II) atom (mean distance Cu-O=2.025 Å). One O atom is tetrahedrally surrounded by four Cu(II) atoms; the mean Cu(II)-O distance of 1.918 Å compares well to [O Cu(II)₄] tetrahedra found in inorganic crystal structures.de|Die Verfeinerung der Kristallstruktur von Cu₂O(SO₄), Dolerophanit, [a=9.370 (1) Å,b=6.319 (1) Å,c=7.639 (1) Å, =122.34 (1)°; Raumgruppe C 2/m;Z=4;R=0.035] bestätigte die trigonal dipyramidale Koordination des einen Cu(II)-Atoms (mittlerer Cu-O-Abstand=2.025 Å). Ein O-Atom ist tetraedrisch von vier Cu(II)-Atomen umgeben; der mittlere Cu(II)-O-Abstand von 1.918 Å entspricht den in ähnlichen [O Cu(II)₄]-Tetraedern von anorganischen Kristallstrukturen gefundenen Werten.

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Cu₂O(SO₄), Dolerophanit: Verfeinerung der Kristallstruktur mit einem Vergleich von [O Cu(II)₄]-Tetraedern in anorganischen Verbindungen