bluuebunny/crossref_metadata_2025_split huggingface dataset:
Chemie des Dicyans: Reaktionen von Diiminosuccinonitril (DISN) mit Sulfenylchloriden und Chlortrimethylsilan sowie Cyclisierung zu Trifluormethyl‐substituierten 2H‐Imidazolen
Authors: Sundermeyer Jörg , Roesky Herbert W. 
Published: July 2007

Chemistry of Cyanogen: Reactions of Diiminosuccinonitrile (DISN) with Sulfenyl Chlorides, Chlorotrimethylsilane and Ring Closure to Trifluoromethyl‐Substituted 2H‐Imidazoles4,5‐Dicyano‐2‐hydroxy‐2‐(trifluoromethyl)‐2H‐imidazole (1) is easily prepared by treating DISN with trifluoroacetic anhydride. In the presence of 4‐(dimethylamino)pyridine, however, the O‐acylated derivative 2 is formed in excellent yield, while the reaction of 1 with chlorotrimethylsilane affords the O‐silylated product 6. A bi‐1,2,5‐thiadiazole of the formula S2(CN)4Cl2 (5) is the final reaction product, when DISN is treated with sulfur dichloride in the presence of “naked” chloride ions. On the other hand the non‐heterocyclic N‐sulfenyl derivative 4 has readily been obtained, when DISN is treated with F3CSCl instead. Finally a procedure is described to convert DISN into the corresponding N‐silylated diimine 3.
Synthese und Strukturen von Imidotitanverbindungen — Steuerung der Bildung monomerer und dimerer Spezies durch Änderung der Basizität des Lösungsmittels
Authors: Roesky Herbert W. , Raubold Thomas , Witt Michael , Bohra Rakesh , Noltemeyer Mathias 
Published: July 2007

Synthesis and Structures of Imidotitanium Compounds — Directing the Monomer‐Dimer Formation by Changing the Basicity of the SolventsThe reaction of (i‐Pr)2PN(SiMe3)2 (1) with elemental sulfur leads to (i‐Pr)2P(S)N(SiMe3)2 (2). Compound 2 reacts with TiCl4 with elimination of chlorotrimethylsilane to yield the adducts [(i‐Pr)2P(S)NTiCl2‐MeCN]2 (3) and (i‐Pr)2P(S)N = TiCl2.3py (4), crystallized from MeCN or pyridine, respectively. Compound 3 crystallises in the space group Pbca, 4 in the space group p&1macr;.
Metallkomplexe mit biologisch wichtigen Liganden, LX. Metallkomplexe von 3′‐Azido‐3′‐desoxythymidin (AZT) und 3′‐Isocyan‐3′‐desoxythymidin
Authors: Pill Thomas , Polborn Kurt , Kleinschmidt Andrea , Erfle Volker , Breu Walter , Wagner Hildebert , Beck Wolfgang 
Published: July 2007

Metal Complexes of Biologically Important Ligands, LX. — Metal Complexes of 3′‐Azido‐3′‐deoxythymidine (AZT) and 3′‐Isocyano‐3′‐deoxythymidineMetal complexes of N‐3‐deprotonated 3′‐azido‐3′‐deoxythymidine (AZT — H+), (AZT — H+)AuPR3 (R = Me, Et, Ph) (2, 3, 4), trans‐(AZT — H+)2Pd(NH3)2 (5), [(n‐Bu3P)(AZT — H+) M(μ‐Cl)2M(AZT — H+)(n‐Bu3P)] (M = Pd, Pt) (6, 7), trans‐(Ph3P)2Pd(AZT — H+)2 (8), cis‐(Ph3P)2Pt(AZT— H+)(Cl) (9), and complexes of 3′‐isocyano‐3′‐deoxythymidine (L), (Et3P)(L)‐ PdCl, (11), magnified image (12), (n‐Bu3P)(L)PtCl2 (13), [(Ph3P)2(L)PtCl](BF4) (14), (η5‐C5Me5)(L)RhCl2 (15), and (η5‐C5Me5)(L)IrCl2 (16) have been prepared and characterized by IR and NMR spectra, 2 by X‐ray crystallography. 2, 4, and 9 show an anti‐HIV activity very similar to AZT; 2 exhibits antiinflammatory activity.
Nitro‐ und Allyloxy‐substituierte helicale [2.2]Metacyclophane: Synthese, Circulardichroismus und Röntgen‐Kristallstrukturanalysen
Authors: Knops Peter , Windscheif Paul‐Michael , Vögtle Fritz , Roloff Albrecht , Jansen Martin , Nieger Martin , Niecke Edgar , Okamoto Yoshio 
Published: July 2007

Nitro‐ and Allyloxy‐Substituted Helical [2.2]Metacyclophanes: Synthesis, Circular Dichroism and Crystal StructuresThe preparations of the title compound 3a, intraannularly nitro‐functionalized, of the extraannularly substituted reference compound 3b, and of the sulfone 4 are described. Enantiomeric resolution of these helical phanes was accomplished on (+)‐PTrMA and cellulose tris(3,5‐dimethylphenyl)carbamate by HPLC. Racemization of the enantiomers of 3b is faster than that of the previously reported extraannularly substituted phanes. The crystal structure of 3a as well as that of the allyl ether 3d show severe distortions of the benzene rings; the CD spectrum of 3a is pointing at an intramolecular charge‐transfer complex, an effect that cannot be evaluated from the CD spectrum of 3b.
Carbodesilylierung von (Trimethylsilyl)imidazolen und ‐pyrazolen
Authors: Effenberger Franz , Roos Michael , Ahmad Roshan , Krebs Andreas 
Published: July 2007

Carbodesilylation of (Trimethylsilyl)imidazoles and ‐pyrazolesThe preparation of the 1‐methyl(trimethylsilyl) (TMS)‐substituted imidazoles 3a, 4a, 8, 9, and 11a by silylation of the corresponding metallated imidazoles is described. Carbodesilylation of 3 with aldehydes or carboxylic halogenides occurs selectively in 2‐position. In the presence of a strong base (CsF) the reactivity against carbon electrophiles correlates well with the stability of the imidazolyl anions; regioselective carbodesilylation in 2‐, 5‐, or 4‐position of the twofold TMS‐substituted imidazoles 3a and 9 therefore is possible, which allows the synthesis of a great variety of hydroxyalkyl‐substituted imidazoles and of acylimidazoles. By using the dimethylsulfamoyl substituent as an N‐protecting group, the N‐ unsubstituted 5‐benzoylimidazole (26) as well as the comparable 5‐benzoyl‐pyrazole (30b) and 5‐(hydroxyphenylmethyl)‐pyrazole (30a) are accessible.
Medizinisch interessante Metallchelate, VI Synthese eines tripodalen Triisocyanid‐Liganden und seine Reaktion mit Na[99mTcO4]
Authors: Ekkehardt Hahn F. , Tamm Matthias , Dittler‐Klingemann Andreas , Neumeier Reinhard 
Published: July 2007

Metal Chelates of Medical Interest, VI. – Synthesis of a Tripodal Triisocyanide Ligand and its Reaction with Na[99mTcO4]The tripodal triisocyanide ligand tris[3‐(2‐isocyanophenoxy)‐ propyl]amine, TARC (6), is prepared from tris(3‐chloropropyl)‐ amine (1) and the potassium salt of 2‐nitrophenole followed by reduction of the nitro functions and conversion of the primary amines into isocyanide functions by the method of Ugi et al. The structure of the intermediate tris[3‐(2‐nitrophenoxy)‐ propyl]amine (3) has been determined by X‐ray diffraction. Tripode 6 binds 99mTc from nuclide generator‐produced Na[99mTcO4].
(1,1′,3,3′‐Tetra‐tert‐butyl‐5,5′‐pentafulvalen) dithallium – Synthese und Kristallstruktur: Ein Beitrag zur Diskussion von nichtklassischen Thallium‐Thallium‐Wechselwirkungen
Authors: Jutzi Peter , Schnittger Jörg , Hursthouse Mike B. 
Published: July 2007

(1,1′,3,3′‐Tetra‐tert‐butyl‐5,5′‐pentafulvalene)dithallium – Synthesis and Crystal Structure: a Contribution to the Discussion of Nonclassical TI(I)‐TI(I) InteractionsReaction of 1,1′,3,3′‐tetra‐tert‐butyl‐5,5′‐dihydropentafulvalenediyldilithium with stoichiometric amounts of thallium chloride affords the dinuclear complex (η5:(η5‐tBu4C10H4)Tl2 (2). Compound 2 is air‐and moisture‐sensitive, and photolabile. It crystallizes in the space group P•1 and consists of two (cyclopentadienyl)thallium units which are connected by a central C‐C bond and twisted against each other by 70°. The monomeric units of 2 form a two‐dimensional polymer with a zick‐zack chain of T1 atoms and a periphery of substituted cyclopentadienyl ligands. Rather short T1‐T1 contacts of 3.760 and 3.998 Å are formed within a dimeric substructure. The geometry of the cyclopentadienyl ligands around the shortest T1‐T1 bond is similar to that predicted by the theory for weak T1‐T1 interactions.
Structures of Tris(donor)‐Tris(acceptor)‐Substituted Benzenes, 2.Potassium Salts of Trinitrophloroglucinol
Authors: Jens Wolff J. , Nelsen Stephen F. , Powell Douglas R. , Desper John M. 
Published: July 2007

AbstractThe X‐ray crystallographic analysis of the mono‐, di‐, and tri‐potassium salts 2b – d of trinitrophloroglucinol (2a) show their benzene rings to become considerably more distorted on successive deprotonation. A parallel increase in C – C, and a decrease in C – O and C – N bond lengths leading to a radialenetype structure is also observed. For 2b, two chemically different molecules are found in the crystal which differ in their hydrogen‐bond pattern as well as in their average bond lengths and deviation of their benzene rings from planarity. AM1 calculations show that for 2b,d a multitude of structures, differing widely in the deviation of their benzene cores form planarity, can exist within a small energy range ( < 3 kcal/mol). The experimental and computational results are discussed in terms of a model that emphasizes “push‐pull” interactions as the main cause for the distortions of the benzene rings in compounds of type 1 and 2.
Funktionalisierte Octabisvalene
Authors: Trupp BjöRn , Handreck Dirk‐Rainer , Böhm Hans‐Peter , Knothe Lothar , Fritz Hans , Prinzbach Horst 
Published: July 2007

Functionalized OctabisvalenesQuadricyclanone (13) is the starting material for a five‐step synthesis of 3‐cyanooctabisvalene (24, 19% total yield), cyclooctatetraene for a six‐step synthesis of (Z)‐3,7‐dicyanooctabisvalene (58, 7% total yield). By decyanation of 24, the parent octabisvalene (1) is produced. NMR data, including 13C,13C coupling constants, are presented.
Organische Synthesen mit übergangsmetall‐Komplexen, 52 N‐Vinylaminocarben‐ und N‐(2‐Propenyl)aminocarben‐Komplexe durch Addition von Keteniminen an Carben‐Eisenkomplexe
Authors: Aumann Rudolf , Trentmann Beate , Dartmann Mechtild , Krebs Bernt 
Published: July 2007

Organic Syntheses with Transition Metal Complexes, 52 1). ‐ N‐Vinylaminocarbene and N‐(2‐Propenyl)aminocarbene Complexes by Addition of Ketene Imines to Carbene Iron ComplexesKetene imines R(Me)C = C = NPh (2, R = Me, Et, i‐Pr) form 1 : 1 adducts with the carbene iron complex (CO)4,FeC(OEt)Ph (1). The initial step of the reaction involves an attack of the nitrogen atom of 2 at the carbene carbon atom of 1 and a subsequent rearrangement to give N‐vinylaminocarbene complexes (E/Z)‐4. In a parallel process with different regiochemistry the central carbon of the CCN unit is attached to the carbene carbon to yield π‐allyl,σ‐complexes (E/Z)‐3. Alkylation of 3a with [Et3O]BF4 leads to the formation of a cationic N‐(2‐propenyl)‐aminocarbene complex 6a. Protonation of 4 with trifluoroacetic acid results in a ring contraction to give the four‐membered metallacycles 7. X‐ray data are reported for prototypes (Z)‐4c and 6a.
Photo Valence Isomerization of 8,9‐Bis(N‐cyclohexylcarbamoyloxymethyl)‐[6]paracyclophane
Authors: Bockisch Frank , Dreeskamp Herbert , Von Haugwitz Thilo , Tochtermann Werner 
Published: July 2007

AbstractIrradiation in the wavelength range of λ = 270 ‐ 320 nm of 8,9‐bis(N‐cyclohexylcarbamoyloxymethyl)‐[6]paracyclophane(1b) in dilute fluid solutions produces the 1,4‐Dewar isomer 2b in a quantum yield of 2.8% while the quantum yield of the rearomatization is 19% in heptane at room temperature. A photostationary equilibrium may be attained which depends strongly on the wavelength of irradiation. At λ = 290 nm 76% of the [6]paracyclophane isomer 1b is obtained whereas at λ = 310 nm 83% of the Dewar isomer 2b is formed in ethanol. The thermal back reaction 2b → 1b follows the Arrhenius law (Ea = 95.9 ± 4.0 kJ/mol, lg A = 10.6 ± 0.4 in heptane). By irradiating 1b with λ < 270 nm the prismane isomer 3b is formed via the Dewar isomer 2b.
Notizen/Notes Kronenether aus o‐Chinondiaziden und Oxetan
Authors: Kirmse Wolfgang , Lelgemann Rudolf 
Published: July 2007

Crown Ethers from o‐Quinone Diazides and OxetaneThe carbenes 11, generated by photolysis of the di‐ and tetrachloro‐o‐quinone diazides 10, react with oxetane in a 1:3 ratio to give the 15‐membered crown ethers 19. In the presence of methanol, the oxonium ions 12 are trapped with formation of 1‐(aryloxy)‐3‐methoxypropanes (13). In the absence of additional nucleophiles, 12 reacts with oxetane until the chain length is appropriate for inverting intramolecular attack of the aryl oxide at the α‐carbon atom of the oxonium ion (18 → 19).
Tripeldecker‐Komplexe, VIII. Elektrophile Aufstockungsreaktionen von Borataferrocen‐ und Bis(borol)cobaltat‐Ionen mit Tricarbonylmetall‐Fragmenten der Chrom‐ und Mangan‐Gruppe
Authors: Herberich Gerhard E. , Köffer Dieter P. J. , Peters Karl M. 
Published: July 2007

Tripledecker Complexes, VIII. — Electrophilic Stacking Reactions of Borataferrocene and Bis(borole)cobaltate Ions with Tricarbonylmetal Fragments of Chromium and Manganese Group MetalsBis(borole)cobaltate ions [CoL2]‐ (1‐) and borataferrocene ions [CpFeL]‐ (2‐) (a: L = C4H4BMe; b: L = C4H4BPh) readily undergo stacking reactions. When treated with sources of chromium group M(CO)3 fragments, 1b‐ and 2b‐ form 30‐e tripledecked anions [μ‐L(CoL){M(CO)3}]‐ (M = Cr, Mo, W) (3‐ ‐ 5‐) and [μ‐L(FeCp){M(CO)3}]‐ (M = Cr, Mo, W) (6‐‐8‐). These 30‐e anions are very sensitive to nucleophilic degradation by e.g. water, acetonitrile and to a lesser extent acetone. Cyclic voltammetry reveals a reversible oxidation of 6‐ to give the 29‐e neutral tripledecker complex μ‐ L(FeCp)[Cr(CO)3] (6), while the oxidation of the higher homologues is fully irreversible. Protonation of 6‐ ‐8‐ affords hydrido complexes μ‐L(FeCp)[MH(CO)3] (M = Cr, Mo, W) (9–11), and, with PhCH2Br, the benzyl derivate μ‐L(FeCp)‐[W(CO)3(CH2Ph)] (12) is produced. Similar stacking reactions with manganese group M(CO)3 fragments produce neutral tripledecked complexes as e.g. μ‐L(CoL)[Re(CO)3] (14) (L = C4H4BPh). In the case of the reaction of [CpFeL]‐ (2‐) with [Mn(CO)3(NCMe)3]3]PF6 symmetric tripledecker compounds μ‐L[Mn(CO)3]2 (15a,b) and μ‐L(FeCp)2 (16a,b) are formed in a novel dismutation reaction (a: L = C4H4BMe; b: L = C4H4BPh).
Vinyliden‐übergangsmetallkomplexe, XVII. Synthese von trans‐[IrCl(=C=CH2)(PR3)2] (PR3 = PMetBu2, PPh3), [IrHCl(CCPh)(PMe2tBu)3] und einigen Dihydridoiridium(III)‐Komplexen
Authors: Werner Helmut , Dirnberger Thomas , Höhn Arthur 
Published: July 2007

Vinylidene Transition‐Metal Complexes, XVII. — Synthesis of trans‐[IrCl(=C=CH2)(PR3)2] (PR3 = PMetBu2, PPh3), [IrHCl(CCPh)(PMe2tBu)3], and of some Dihydridoiridium(III) Complexes[IrCl(C8H14)2]2 (1) reacts with PMetBu2 in the presence of H2 to give [IrH2Cl(PMetBu2)2] (2). Treatment of 2 with acetylene yields the vinylidene complex trans‐[IrCl(=C=CH2)‐(PMetBu2)2] (3). The reaction of 1 with PMePh2 or PMe2tBu in the presence of H2 leads to the formation of fac‐[IrH2Cl(PR3)3] (4a, 5a), which on warming to 60°C rearrange to give the more stable mer isomers 4b, 5b. Treatment of 1 with PMePh2 or PMe2tBu and phenylacetylene affords the hydrido(phenyl‐ethynyl)iridium(III) compounds mer‐[IrHCl(CCPh)(PR3)3] (8, 9), which could not be converted by phosphine elimination to the corresponding (phenylvinylidene)iridium complexes. The synthesis of trans‐[IrCl(=C=CH2)(PPh3)2] (11) has been achieved by CO abstraction from [IrHCl(CCH)(CO)(PPh3)2] (13) by using trimethylamine oxide.
Mehrstufige reversible Redoxsysteme, LV. Kristallstruktur des CT‐Komplexes 2,5‐Me2‐DCNQI/TTF aus N,N′‐Dicyan‐2,5‐dimethyl‐1,4‐benzochinondiimin und Tetrathiafulvalen sowie des Acceptors 2,5‐Me2‐DCNQI
Authors: Aumüller Alexander , Erk Peter , Hünig Siegfried , Hädicke Erich , Peters Karl , Schnering Hans Georg Von 
Published: July 2007

Multi‐Step Redox Systems, LV. – Crystal Structure of the CT Complex 2,5‐Me2‐DCNQI/TTF from N,N′‐Dicyano‐2,5‐dimethyl‐1,4‐benzoquinone Diimine and Tetrathiafulvalene and of the Acceptor 2,5‐Me2‐DCNQIThe crystal structure of the title compound is described and discussed in terms of a neutral non‐conducting mixed‐stack CT complex. X‐ray data for the acceptor 2,5‐Me2‐DCNQI are given for comparison.
Halogen – Kohlenstoff – Schwefel‐Verbindungen: Synthese und Reaktionsverhalten von 4,5‐Bis(trifluormethyl)‐1,3‐dithiol‐Derivaten
Authors: Maletzko Christian , Sundermeyer Wolfgang , Pritzkow Hans , Irngartinger Hermann , Huber‐Patz Ursula 
Published: July 2007

Halogen – Carbon – Sulfür Compounds: Synthesis and Modes of Reactions of 4.5‐Bis(trifluoromethyl)‐1,3‐dithiole DerivativesThe chemistry of the bis(trifluoromethyl)‐1,3‐dithiole system is thoroughly investigated starting from the 2‐thione 6. By its oxidation the sulfine 2 and the ketone 7 are obtained. Further oxidation of 2 leads to the spiro compound 3. By chlorination of 6 the 2‐sulfenyl chloride 5 is obtained, which can be desulfurized by PCl3 to the 2,2‐dichloro compound 10. The best method for the preparation of the latter is the reaction of 6 with PCl5. Hydrolysis of 10 yields again the ketone 7. By reaction of 1,2‐ethanedithiol with 10 the spiro compound 11 is obtained, the reaction of which with hexafluoro‐2‐butyne also affords 3. 10 reacts with primary amines to the 2‐imines 9a and 9b, whereas 5 under similar conditions reacts via the thione S‐imides 4a and 4b to 9a (with sulfur extrusion) or in a rearrangement reaction to the 1,2,4‐trithiine 1. The preparation of the tosyl hydrazone 12 does not open an access to the diazo compound 16, neither does the reaction of 10 with hydrazine, which yields the ketazine 14. The homogeneous reaction of disilylhydrazine and 10 produced the tetrazene 17, which is a dimer of 16 and decomposes at its high melting point to the ketazine 14.
Polylithiumorganische Verbindungen, XVI. 1,4‐Disila[6]radialene: Aktivierungsparameter der Sessel‐Twist‐Inversion und analytische Enantiomerentrennung der Twist‐Konformeren
Authors: Maercker Adalbert , Brieden Walter , Kastner Fritz , Mannschreck Albrecht 
Published: July 2007

Polylithiumorganic Compounds, XVI. – 1,4‐Disila[6]radialenes: Activation. Parameters of the Chair‐Twist Inversion and Analytical Separation of the Enantiomers of the Twist ConformersKinetic measurements of the chair‐twist inversion of the 1,4‐disila[6]radialenes 2 – 4 have been performed at four different temperatures, respectively. The entropies of activation are found to be negative. While the chair conformers of the radialenes are achiral as expected, the enantiomers of the three twist conformers could be separated by HPLC on an optically active stationary phase.
Bestimmung der Singulett‐Triplett‐Aufspaltung von Diradikalen mit Hilfe der Sauerstoff‐Abfang‐Technik
Authors: Roth Wolfgang R. , Ruhkamp Joerg , Lennartz Hans‐Werner 
Published: July 2007

Determination of the Singlet‐Triplet Splitting of Diradicals by Oxygen‐TrappingThe diradical 2, generated by thermolysis of 7‐methylenebi‐cyclo[3.2.0]hept‐1‐ene (1), can be trapped by oxygen in the gasphase. From the different trapping rates with and without added SF6 the intersystem crossing rates of the diradical have been deduced. From their temperature dependance the singlet‐triplet splitting is calculated to be 7.4 kcal mol‐1 with the triplet being the ground state. The triplet is protected by an enthalpy barrier of 13.0 kcal mol‐1 against recombination of the unpaired electrons (2‐tr→1). From the heat of hydrogenation of 1 the heat of formation of 1, 2‐s and 2‐tr is derived.
Photochemistry of Tetrabenzo[c,e,i,k] [1,2,7,8]tetraazacyclododecine in 2‐Propanol
Authors: Tauer Erich , Grellmann Karl‐Heinz , Heinrich Angelika 
Published: July 2007

AbstractThe photochemical properties of the tetraazacyclododecine 1 were investigated. The trans,trans isomer 1tt can be photoisomerized yielding the stable cis,cis isomer 1ee. The isomerization requires two photons and proceeds via the unstable trans,cis isomer 1tc. In nitrogen‐purged 2‐propanol as solvent 1 yields five stable photoproducts as a result of a number of consecutive photoreduction reactions. Our attempts to convert 1 by light into the tetraazetidine 4 were not successful.
Schwefelverbindungen, 143 Synthese und Charakterisierung der neuen bicyclischen Schwefel‐Kohlenstoff‐Verbindungen C6H8S8, C4H4S7 und C4H4S82)
Authors: Westphal Ursula , Steudel Ralf 
Published: July 2007

Sulfur Compounds, 143. — Synthesis and Characterisation of the New Bicyclic Sulfur‐Carbon Compounds C6H8S8, C4H4S7, and C4H4S8The reaction of Cp4Ti2C2S4 (1) with two equivalents of the bissulfenyl chloride 1,2‐C2H4(SCl)2 affords the new bicyclic compound C6H8S8 (2). Treatment of 1 with one equivalent of SxCl2 (x = 1, 2) results in Cp2TiC2S5 (3) and Cp2TiC2S6 (4), respectively, which on reaction with 1,2‐C2H4(SCl)2 give the asymmetric bicyclic polysulfides C4H4S7 (5) and C4H4S8 (6), respectively.
Thiolatokomplexe des einwertigen Golds. Synthese und Struktur von [(2,4,6‐iPr3C6H2S)Au]6 und (NH4)[(2,4,6‐iPr3C6H2S)2Au]
Authors: Schröter Ingrid , Strähle Joachim 
Published: July 2007

Thiolato Complexes of Monovalent Gold. Synthesis and Structure of [(2,4,6‐iPr3C6H2S)Au]6 and (NH4)[(2,4,6‐iPr3C6H2S)2Au]Reaction of Au(CO)Cl with 2,4,6‐tri(isopropyl)thiophenol affords hexameric gold(I) thiolate [(2,4,6‐iPr3C6H2S)Au]6 (1). According to an X‐ray analysis 1 forms a centrosymmetrical twelve‐membered Au – S ring in the chair conformation with the linearly coordinated Au atoms at the mid‐edges and the S atoms at the corners of the heterocycle. When the reaction of 2,4,6‐tri(isopropyl)thiophenol is carried out with AuI in liquid ammonia the thiolato complex [(2,4,6‐iPr3C6H2S)2Au]– ‐NH+4 (2) is obtained. It crystallizes as NH4 · 2 · 3 NH3. The gold atom in 2 is linearly coordinated by two thiolato S atoms. The ammonium cation forms hydrogen bonds with three NH3 solvate molecules.
Kristallisiertes Natrium‐triethylhydroborat — Bildung und Charakterisierung
Authors: Köster Roland , Schüßler Wilhelm , Boese Roland , Bläser Dieter 
Published: July 2007

Crystalline Sodium Triethylhydroborate — Formation and CharacterizationTwo equiv. of NaHBEt3 (1) and one equiv. of mesitylene form a crystalline compound, which is characterized by DSC and by a single‐crystal X‐ray structure analysis at 190 K as the solid phase 2.
Enantiomerenreine 3,7‐Dioxa‐2‐azabicylo[3.3.0]octane durch intramolekulare 1,3‐dipolare Cycloaddition von Nitronen
Authors: Güinter Aurich Hans , Biesemeie Frank , Boutahar Mostafa 
Published: July 2007

Enantiomerically Pure 3,7‐Dioxa‐2‐azabicyclo[3.3.0]octanes by Intramolecular 1,3‐Dipolar Cycloaddition of NitronesStarting with chiral non‐racemic esters of lactic acid 7 and mandelic acid 8, respectively, chiral nitrones 4 have been prepared. They spontaneously undergo an intramolecular cycloaddition which proceeds with asymmetric induction by the chiral center yielding exclusively the bicyclic compounds 5 in enantimerically pure form. Reductive opening of the isoxazolidine ring affords tetrahydrofuran derivatives 13 with an γ‐amino alcohol group. Reaction of 13 with (‐)‐camphanoyl chloride gives the esters 14. Their 1H‐NMR spectra reveal a diastereomeric purity of at least 98%.
Synthese von 6,6,7,7,13,13,14,14‐Octamethyl‐6,7,13,14‐tetrasiladispiro[4.2.4.2]‐ tetradeca‐1,3,9,11‐tetraen und sein Einsatz in der π‐Komplexchemie von p‐ und d‐Block‐Elementen
Authors: Jutzi Peter , Krallmann Ralf , Wolf Gerald , Neumann Beate , Stammler Hans‐Georg 
Published: July 2007

Synthesis of 6,6,7,7,13,13,14,14‐Octamethyl‐6,7,13,14‐tetrasiladispiro[4.2.4.2] tetradeca‐1,3,9,11‐tetraene and Its Application in the Chemistry of π Complexes of p‐ and d‐Block ElementsThe title compound 2 can be synthesized either by reaction of ([C5H5SiMe2SiMe2C5H5]2‐ 2 Li+) with XSiMe2SiMe2X or by an intermolecular nucleophilic substitution reaction between two molecules of ([XSiMe2SiMe2C5H5]‐ Li+). Isomers of 2 with allylic hydrogen atoms arise from silatropic rearrangements and therefore show “cyclopentadiene reactivity”. Reaction of the monoanion of 2 with FeCl2 yields the ferrocene 4. From the reaction of the dianion of 2 with Me5C5RuCl, the binuclear ruthenium complex 7 with Si – Si bridges in 1,2‐position can be isolated; reactions with FeCl2 or Me5C5Fe(acac), with Me5C5GeCl, with SnCl2, and with PbCl2, lead to the metallocenes 6, 7, 8, and 9; in all these complexes the disilane bridges are in 1,2‐position. The binuclear cobalt complex 10, in which the cyclopentadienyl rings are connected with each other by disilane bridges in 1,3‐position, can be synthesized by the reaction of 2 with CO2(CO)8. The results of single‐crystal X‐ray structure analyses of 6 and 10 are presented. The possible conformations of the dianion of 2 are discussed.