Gemischtligandenkomplexe mit N-Acyl-thioharnstoffen: Die Struktur des [N-(Morpholinothiocarbonyl)-benzamidato] (3-amino-2-cyano-n-butyl-dithiocrotonato)nickel(II)

Mixed Ligand Complexes of N-Acyl-thioureas: The Structure of [N-(Morpholinothiocarbonyl)-benzamidato] (3-amino-2-cyano-n-butyl-dithiocrotonato)nickel(II) The reaction of a solution of N-(morpholinothiocarbonyl)benzamide and 3-amino-2-cyano-n-butyl-dithiocrotonate with nickel(II)-acetate tetrahydrate yields the first mixed ligand complex of N-acyl-thioureas. Its structure has been determined by an X-ray structure analysis. The coordination geometry is square planar. Bond lengths and angles are in good agreement with those of other bis and tris N-acyl-thiourea chelates.     

Kristall- und Molekülstruktur von Bis[N-(diethylaminothiocarbonyl)-N′-phenylbenzamidinato]nickel(II)

Crystal and Molecular Structure of Bis[N-(diethylaminothiocarbonyl)-N′-phenyl-benz-amidinato]nickel(II) The structure of bis[N-(diethylaminothiocarbonyl)-N′-phenyl-benzamidinato]-nickel(II) has been determined by X-ray structure analysis. The compound crystallizes in orthorhombic space group P2₁2₁2₁ with a = 16.36, b = 16.94, c = 12.96 Å and Z = 4. The solution of the structure was performed by heavy atom technique and gave a final R value of R = 0.055 for 1764 observed reflections. The coordination polyhedron has a tetrahedrally distorted shape. The ligator atoms are arranged in cis position. The chelate rings deviate clearly from planarity. Against the chelate rings the phenyl rings are appreciably twisted. The title compound is compared regarding its structure with the analogous copper chelate.     

Kristall- und Molekülstruktur von Bis[N-(diethylaminothiocarbonyl)-N′-phenylbenzamidinato]kupfer(II)

Crystal and Molecular Structure of Bis[N-(diethylaminothiocarbonyl)-N′-phenyl-benzamidinato]copper(II) The structure of bis[N-(diethylaminothiocarbonyl)-N′-phenyl-benzamidinato]-copper(II) has been determined by X-ray structure analysis. The compound crystallizes in the orthorhombic space group Pbca with a = 27.792, b = 19.197, c = 12.325 Å and 8 formula units per unit cell. The structure was solved by heavy atom technique. The final R value was R = 0.06 for 1589 observed symmetry independent reflections. The coordination polyhedron is a distorted tetrahedron. In spite of the bulky phenyl groups the ligator atoms are arranged in cis position. The chelate rings deviate clearly from planarity. The phenyl rings are appreciably twisted against the chelate rings.     

Synthese und Struktur eines Molybdän–Gadolinium-Heterometall-Komplexes Die Struktur von [Li(thf)4]2[Cp2MoSGdBr4(thf)]2

Synthesis and structure of a Molybdenum–Gadolinium Heterometallic Complex. The Structure of [Li(thf)₄]₂[Cp₂MoSGdBr₄(thf)]₂ [Cp₂MoHLi] reacts in THF with S and GdBr₃ to yield the tetranuclear heterobimetallic complex [Li(thf)₄]₂[Cp₂MoSGdBr₄(thf)]₂. The bonding situation and the structure of this compound were characterized by X-ray structure analysis (space group P1 (No. 2), Z = 1, a = 10.845(2) Å, b = 12.166(2) Å, c = 15.881(2) Å, α = 101.74(2)°, β = 97.62(2)°, γ = 103.97(2)°). Each S atom of the central Mo₂S₂-ring is coordinated by a GdBr₄(thf) fragment. Additionally each Mo atom is connected to two Cp ligands. This leads to a tetrahedral coordination of the Mo atoms and a octahedral coordination of the Gd ions.     

Struktur des Hydrazinolyseproduktes von N-(3-Oxo-1-isoindolinyliden)-alanin-äthylester

Hydrazinolysis of N-(3-Oxo-1-isoindolinyliden)alanin Ethyl Ester, Structure of the Product Treatment of N-(3-oxo-1-isoindolinyliden)alanin ethyl ester (6) with hydrazine hydrate leads to 4-methyl-2,3,4,6-tetrahydro[1,2,4]triazino[3,4-a]isoindole-3, 6-dione ( 8 , Scheme 3) and not to the previously postulated 6-hydroxy-2-methyl-2,3-dihydro-imidazo [2,1-a]phthalazin-3-one ( 7 , cf. [2]). The structure of 8 has been established by an independent synthesis as well as by the X-ray analysis of the reaction product 11 from 8 and 3-dimethylamino-2,2-dimethyl-2 H-azirine ( 1 , Scheme 4). A reaction mechanism for the formation of 8 from 6 is suggested in Scheme 5.     

Synthese und Struktur von Silber(II)-tetrafluoroaurat(III) Ag[AuF4]2

Synthesis and Structure of Silver(II) Tetrafluoroaurate(III) Ag[AuF₄]₂ Intensive green single crystals of Ag[AuF₄]₂ can be obtained by heating up micro crystalline Ag[AuF₄]₂ in autoclaves (p(F₂) ～ 200 bar, T ～ 400°C, t ～ 14 d). It crystallizes monoclinic, space group P2₁/n ? C; (No. 14) with a = 522.3(1), b = 1101.3(3), c = 550.5(2) pm, β = 94.98(3), Z = 2 and is isotypic with Pd[AuF₄]₂.     

Kristall- und Molekülstruktur von Bis[N-(diethylaminothiocarbonyl)-benzamidin]silber(l)-nitrat

Crystal and Molecular Structure of Bis[N-(diethylaminothiocarbonyl)-benzamidine]-silver(I) Nitrate The crystal structure of bis[N-(diethylaminothiocarbonyl)-benzamidine]silver(I) nitrate has been determined by X-ray structure analysis on a single crystal. The compound is monoclinic, space group P2₁/n with a = 12.541, b = 43.470, c = 11.096 Å, β = 106.27° and 8 formula units per unit cell. The structure was solved by application of direct methods to difference structure factors (DIRDIF) and refined for 5242 observed reflections to a final R value of R = 0.070. There are two symmetrically independent molecules of the title compound in the asymmetric unit. The central Ag ion is coordinated by the S atoms of two ligands. The nitrate ions do not coordinate. The coordination geometry is slightly bent.     

Metallierung von Triisopropylsilylarsan durch Bis(tetrahydrofuran)calcium‐bis[tris(trimethylsilylmethyl)zinkat]

Metalation of Triisopropylsilylarsane with Bis(tetrahydrofuran)calcium‐bis[tris(trimethylsilylmethyl)zincate] The transmetalation of bis(trimethylsilylmethyl)zinc with distilled calcium in THF yields bis(tetrahydrofuran)calcium bis[tris‐(trimethylsilylmethyl)zincate] ( 1 ). The trialkylzincate anion appears as a bidentate ligand with Ca‐C‐Zn three‐center‐bonds. The CaC bond lengths show values of 265.5(2) and 271.7(2) pm. The metalation of triisopropylsilylarsane gives tetrakis(tetrahydrofuran)calcium [1, 3‐bis(triisopropylsilylarsanyl)‐2, 4‐bis(triisopropylsilyl)‐1, 3‐dizinca‐2, 4‐diarsacyclobutane‐2, 4‐diide] ( 2 ). The central moiety is a sligthly distorted trigonal As₂CaZn₂ bipyramid with the arsenic atoms in apical positions. The mean Ca‐As bond lengths lie with a mean value of 291.4 pm in the charakteristic region for calcium bis‐(arsanides).     

Beiträge zur Chemie der Silicium-Schwefel-Verbindungen. 50 [1] Bis(triorganoxysilyl)polysulfide und die Struktur des Bis(tri-t-butoxysilyl)disulfids

Contributions to the Chemistry of Silicon-Sulfur Compounds. 50. Bis(triorganoxysilyl)-polysulfides and the Structure of Bis(tri-tert-butoxysilyl)disulfide Disilylated polysulfides (RO)₃SiS_nSi(OR)₃, R = i-Pr, tert-Bu, 2,6-Me₂C₆H₃, n = 2–5, were obtained by reaction of (RO)₃SiSNa with I₂ or S_nCl₂, respectively. The reaction of [(t-BuO)₃Si]₂S₂ with Ph₃SiH yielded the mixed sulfide (t-BuO)₃SiSSiPh₃ and with Ph₃P or Bu₃P, by extrusion of one sulfur atom, the [(t-BuO)₃Si]₂S. The X-ray crystal structure of [(t-BuO)₃Si]₂S₂ was determined. The S? S bond length is 209,2 pm, Si? S 213,2 pm. The mean value of the Si? S? S angle is 100,7°, and the torsion angle Si? S? S? Si ?127,6°.     

Die Kristallstruktur von CsTcO4 [1]

The Crystal Structure of CsTcO₄ CsTcO₄ crystallizes orthorhombic with a = 5.72₇, b = 5.92₁ and c = 14.34 Å. Z = 4, space group Pnma (Nr. 62, I.T.). The metal positions were refined by single crystal data, the oxygen positions first determined: the CsTcO₄ structure is a slight distortion of the scheelite arrangement (parameters: see text). The MADELUNG Part of Lattice Energy, MAPLE, ?Mean Effective Ionic Radii”?, MEIR, and Effective Coordination Numbers, ECoN, are calculated and discussed.     

Die Ableitung der Stereochemie von 1-Isopropyl-4-methyl-bicyclo[3.1.0]hexan (cis-und trans-Thujan) durch Protonenresonanz-Spektroskopie

100 Mc/s proton NMR. spectra of the two diastereoisomeric thujanes obtained by reduction natural thujone have been measured and are given a detailed analysis. The relative configurations of the two hydrocarbons are deduced. Together with the known R-configuration at C(1) the absolute configurations can be derived, (?)-cis-thujane having the (1R:4S:5R)- and (+)-trans-thujane the (1R:4R:5R)-configuration. It can be shown that the trans-isomer adopts a boat-like conformation of the bicyclohexane ring system whereas cis-thujane prefers a half-chair conformation with a flattened cyclopentane ring.