bluuebunny/crossref_metadata_2025_split huggingface dataset:
Synthese des 9,9-DimethyI-9-silaacridans sowie einiger Derivate mit variierter Seitenkette / Synthesis of 9,9-Dimethyl-9-silaacridane and of Some Derivatives with Varied N-Side Chains
Authors: Wannagat Ulrich , Wiese Dietma 
Published: March 2015

Abstract
9,9-Dimethyl-9-silaacridane 3a was synthesized by ringclosing reactions of N-trimethylsilyl-bis(2-halogenophenyl)amines with dichlorodimethylsilane and acid cleavage of the silyl groups (eqs (6-9)). Syntheses of N-organyl-substituted 9,9-dimethyl-9-silaacridanes 13 occurred by ring closure of N-organyl-bis(2-halogenophenyl)amines 12 with dichlorodimethylsilane. organyl groups here being dimethylaminoethyl. pyrrolidinoethyl, piperidinoethyl, 3-dimethylamino-2-methyl-propyl and (1-methylpiperidin-3-yl)methyl. 13 were transformed to their hydrochlorides and methoiodides 14. Structures of 13 are compared with those of analogous compounds bearing aminopropyl-side chains and discussed in the light of psychopharmacological effects of tricyclic ring systems.
Struktur und Reaktivität von isoanellierten heterocyclischen Systemen mit 4nπ- und (4n+2)π-Elektronen, XIV [1]: Tri- und tetracyclische Hetarene mit lokalisierten oder delokalisierten PyrroI-Strukturen / Structure and Reactivity of Isoannellated Heterocyclic Systems with 4nπ- and (4n+2)π-Electrons, XIV [1]: Tri- and Tetracyclic Hetarenes with Localized or Delocalized Pyrrole Units
Authors: Kreher Richard P. , Hildebrand Thomas 
Published: March 2015

Abstract
2,7-Di-tert-butyl-2,7-dihydro-benzo[ 1,2-c:3,4-c′]dipyrrole (2b) and 2,5,8-Tri-tert-butyl-5.8-di-hydro-2H-benzo[1,2-c:3,4-c′:5,6-c″]tripyrrole (3b) have been prepared by acetolysis of the cor-responding tri-and tetracyclic N-oxides, isolated in crystallinic form and characterized by spectroscopic data. The scope of the N-oxide route is documented and the existence of benzoannellated pyrroles is proofed. The stabilizing effect of the tert-butyl group is presumably sup-ported by the vicinal annellated heterocycles.
The Crystal Structure of TlBrI2(4-methylpyridine-N-oxide)2
Authors: Hiller W. , Castiñeiras A. , García- Fernandez M. E. , Bermejo M. R. , Bravo J. , Sanchez A. 
Published: March 2015

Abstract
The unit cell of TlBrI2 (4-methylpyridine-N-oxide) 2 is orthorhombic, space group Pnna. with a = 1126.9(3),b = 919.8(2),c = 1210.4(3) pm.and Z = 4. The structure consists of discrete TlBrI2 (4-methyl-pyridine-N-oxide)2 molecules which have a distorted trigonal-bipyramidal geometry. The thallium atom is coordinated to two iodine atoms and a bromine atom in equatorial positions, and by two 4-methyl-pyridine-N-oxide ligands in the axial positions.
(Ph4P)2 Mn2Br6 und (Ph3PCH2Ph)2Mn2I6 (Ph = C6H5) / (Ph4P)2Mn2Br6 and (Ph 3PCH2Ph)2Mn2I6 (Ph = C6H5
Authors: Pohl Siegfried , Saak Wolfgang , Stolz Peter 
Published: March 2015

(Ph4P)2Mn2Br6 (1) and (Ph3PCH2Ph)2Mn2I6 (2) were prepared from the reaction of manganese dihalide with the corresponding phosphonium halide in CH2Cl2.
The structures of 1 and 2 were determined from single crystal X-ray diffraction data.
Both compounds crystallize in the triclinic space group P 1 with one formula unit per unit cell.
1:a = 998.1(1), b = 1005.7(1), c = 1313.3(2) pm, α = 108.51(1), β = 94.25(1), γ = 100.36(1)°.
2: a = 1058.6(2), b = 1236.3(2), c = 1248.4(3) pm, α = 63.53(1), β = 74.15(1), γ = 74.65(1)°.
The structures of 1 and 2 exhibit discrete, dimeric anions formed by the fusion of two identical tetrahedral-like units with a common halogen-halogen edge. The mean Mn-Hal bond lengths were found to be 251.8 pm (Mn-Br) and 272.2 pm (Mn-I). The difference between the bridging and terminal Mn-Hal bond lengths is about 12-13 pm in both compounds
1,3,5-Tris(dimethylamino)benzol mit Iod und 1,3,5-Tricyanobenzol: Eine ungewöhnliche Dimerisierung und ein „normaler“ Donor/Akzeptor-Komplex / 1,3,5-Tris(dimethylamino)benzene with Iodine and 1,3,5-Tricyanobenzene: An Unusual Dimerization and a “Normal” Donor/Acceptor-Complex
Authors: Keller H. J. , Niebl R. , Renner G. , Ruhr D. von der , Schweitzer D. 
Published: March 2015

Reaction of 1,3,5-tris(dimethylamino)benzene (TDMAB) with iodine in solution gives dark red needles of a compound (1) with stoichiometry C24H42I6N6, Mr = 1176.07, orthorhombic, Cmca, Z = 4, a = 10.865(2) Å, b = 16.737(6) Å. c = 20.511(9) Å, V = 3730 Å3, dc = 2.1 g·cm-3 measured at room temperature, R = 0.062 for 744 independent reflections and 100 L. S.-parameters. The solid contains bis[tris(dimethylamino)cyclohexadienylium]dications - obtained by dimerization of TDMAB+ radical cations - and triiodide counter anions. The solid is diamagnetic.
Reaction of TDMAB with 1,3,5-tricyanobenzene (TCB) leads to orange platelets of 2 with stoichiometry C21H24N6, Mr = 360.4, orthorhombic, Pna21 Z = 4, a = 11.074(4) Å, b = 11.568(4) Å, c = 16.100(7) Å, V = 2060 Å3, dc = 1.18 g·cm-3, measured at room temperature, R = 0.065 for 921 independent reflections and 156 parameters. The solid consists of donor (TDMAB) - acceptor (TCB) pairs. The compound is diamagnetic at room temperature.
Darstellung und Redoxverhalten aller bindungsisomeren Hexakis(thiocyanato(N)-thiocyanato(S))-osmate(III) und (IV), [Os(NCS)n(SCN)6-n]3-/2-, n = 0—6, einschließlich der Stereoisomeren / Preparation and Electrochemical Behaviour of All Bond-Isomeric Hexakis(thiocyanato(N)-thiocyanato(S))osmates(III) and (IV), [Os(NCS)n(SCN)6-n]3-/2-, n = 0—6, Including Stereoisomers
Authors: Bütje K. , Preetz W. 
Published: March 2015

Abstract
The first two complete series of all 10 possible linkage and geometric isomers of the general formula [Os(NCS)n(SCN)6-n]3-/2- have been obtained. The Os(III) complexes, some of which have been previously known, are prepared from the reactions of K2[OsX6], X = Cl. Br. I, and K2[OsO2(OH)4] with excess aqueous or methanolic KSCN solution and subsequent chromato­graphic separation on DEAE cellulose. Oxidation with Ce(IV) in acetone or methanol yields the corresponding Os(IV) compounds without changes in the ligand sphere except for n = 0, but pure salts of [Os(SCN)6]2“ are isolated by repeated recrystallization. S-bonding is less favoured in Os(IV) than in Os(III), proving that Os(IV) is the harder Lewis acid. Cyclic voltammograms of all isomers show two waves, a mainly irreversible Os(II)/Os(III) couple and a reversible Os(III)/Os(IV) couple. Characteristic shifts of the half-wave potentials of both electron transfer reactions within the series give strong evidence of π-back donation to -NCS.
Pentamethylcyclopentadienyl-, Acetylcyclopentadienyl- und Indenyl-dicarbonyl-AcetylenkompIexe des Vanadiums. Molekülstruktur von C9H7V(CO)2PhC2H / Pentamethylcyclopentadienyl, Acetylcyclopentadienyl and Indenyl Dicarbonyl Acetylene Complexes of Vanadium. Molecular Structure of C9H7V(CO)2PhC2H
Authors: Alt Helmut G. , Engelhardt Heidi E. , Razavi Abbas , Rausch Marvin D. , Rogers Robin D. 
Published: March 2015

Abstract
The photo-induced reaction of C5Me5V(CO)4 (1). (C5H4COMe)V(CO)4 (2) and C9H7V(CO)4 (3) with acetylenes R1C2R2 (R1, R2 = H. Me, Ph) yields the substitution products C5Me5V(CO)2R1C2R2 (4), (C5H4COMe)V(CO)2R1C2R2 (6) and C9H7V(CO)2R1C2R2 (7). One CO ligand of complexes 4 can be substituted by PMe3 affording complexes of the type C5Me5V(CO)(PMe3)R1C2R2 (5). The acetylene complexes 4-7 are characterized by their IR. 1H, 13C and 51V NMR as well as their mass spectra. In these compounds the alkyne ligand shows a hindered rotation around the metal alkyne bond axis. The rotation barrier (ΔG≠ = 40-50 kJ/mol) is higher than in the corresponding cyclopentadienyl complexes. An X-ray crystal structure analysis of C9H7V(CO)2PhC2H indicates an orientation of the alkyne-C-C-axis in the symmetry plane of the C9H7V(CO)2 fragment. The phenyl substituent is pointing away from the metal and the indenyl ligand.
Beiträge zur Chemie des Bors, 190 [1] Synthese und Molekülstruktur von 1,2-Dihydroboreten und Azadiboretidinen / Contribution to the Chemistry of Boron, 190 [1] Synthesis and Molecular Structure of 1,2-Dihydrodiboretes and Azadiboretidines
Authors: Glaser Bernhard , Mayer Erwin P. , Nöth Heinrich , Rattay Wilfried , Wietelmann Ulrich 
Published: March 2015

Abstract
[2+2]-Cycloadditions of 9-Fluorenylidentetramethylpiperidinoboranes have been studied with selected olefines, acetylenes and iminoboranes. No reactions with olefines were observed. While propiolic methylester reacts exclusively at the carbonyl bond producing the oxaboretane 5, alkines such as diethylamino-alkines, cyclo-octine and phenylacetylene provide access to the'1,2-dihydroboretenes 6, 3 and 2. Tetramethylpiperidinoiminoboranes make 1.2.4-azadiboretidines 7 available.
6a and 7a contain a folded four-membered ring as shown by X-ray structure analysis. There is only a weak 1,3-intraannular interaction due to BN-;r-bonding of the boron atoms with their exocyclic amino group.
On the Synthesis and Electrochemical Properties of Some New Bipyridinium and Related Compounds
Authors: Bauer Rupert , Nussbaumer Peter , Neumann-Spallart Michael 
Published: March 2015

Abstract
The synthesis of some new bipyridinium salts is described. Their behavior upon reduction is studied by cyclovoltammetry, coulometry and spectroscopically. Halfwave potentials range from -0.28 V to -0.59 V and ε values of the reduced viologens lie around 104 M-1cm -1 . In addition two relay compounds (4,4′-pyridine-2,4-diyl)-bis-(1-methylpyridinium methylsulfate), 4.4′,4″-(pyridine-2,4,6-triyl)-tris-(1-methylpyridiniumchloride) that are not viologens are described. These substances also form a colored radical upon reduction, but with exceptional stability to-wards oxidation with dioxygen. From coulometric measurements it is inferred that three electrons are transferred in one step. Spectral changes observed in the course of the electrochemical reduction are explained by dimer formation.
Molekülstruktur von {[P(C6H5)3]2RhOH}2· 2 C6H6 / The Molecular Structure of {[P(C6H5)3]2RhOH}2· 2 C6H6
Authors: Brune Hans-Albert , Hemmer Reinhard , Unsin Josef , Holl Konrad , Thewalt Ulf 
Published: March 2015

Abstract
The dinuclear Rhodium(I) complex Bis(μ-hydroxo)bis(bistriphenylphosphane-rhodium) forms during the HRh(PPh3)2 catalyzed hydrogenation of Schiff bases by isopropanol. It can be isolated from benzene solution as a crystalline solvate of composition {[P(C6H5)3]2RhOH}2·2 C6H6 (1). The complex contains a four-membered ring with bridging hydroxo groups. Crystals of 1 are triclinic, space group P1̄ with a = 12.570(3), b = 12.850(4), c = 13.982(3) Å, α = 116.23(3), β = 115.08(3), γ = 90.89(3)°, and Z = 1.
Stickstoffverbindungen von Elementen der dritten Hauptgruppe mit intra- und intermolekularen Donor-Akzeptor-Bindungen, V [1]. Spezielle Gallium- und Indiumamide mit Alkoxogruppen / Nitrogen Compounds of Elements of the Third Main Group with Intra- and Intermolecular Donor Acceptor Bonds, V [1]. Special Gallium and Indium Amides with Alkoxo Groups
Authors: Veith M. , Pöhlmann J. 
Published: March 2015

Abstract
The lithium alkoxoamidosilane (Me2Si(OtBu)(NtBu)Li)2 (4) and its trimethyltin derivative Me2Si(OtBu)(NtBu)SnMe3 (7) have been used, to introduce the ligand Me2Si(OtBu)(NtBu) = L into molecular compounds of gallium and indium. The following molecules were synthesized: L-M(Me)Cl (M = Ga (5), In (6)), L-InMe2 (8), L-InX2 (X = Cl (9), Br (10)), L2InX (X = Cl (11), Br (12)) and L2Ga2Cl2 (22). The ligand L is assumed to chelate the metal atom on the basis of temperature dependent 1H NMR spectra. The chelating effect is more pronounced in the gallium derivatives than in the indium analogues. Equilibria between L2InX/InX3 and LInX2 have been observed in diethylether solutions. No metal(I) derivatives LGa or LIn could be isolated. L2Ga2Cl2 (22), formally containing gallium(ll), can be sublimed without decomposition at 110 °C in vacuo.
Synthese und Struktur von 1,5-Bis(tolyl)pentaazadienidokomplexen von Eisen(II) und Ruthenium(I): [Fe(tolN5tol)2]2 und [Ru(CO)3(tolN5tol)]2 / Synthesis and Structure of 1,5-Bis(tolyl)pentaazadienido Complexes of Iron(II) and Ruthenium(I): [Fe(tolN5tol)2]2 and [Ru(CO)3(tolN5tol)]2
Authors: Schmid Raimund , Strähle Joachim 
Published: March 2015

The reaction of Fe(CO)4I2 with Ag(tolN5tol) in THF yields dark violet, oxygen sensitive [Fe(tolN5tol)2]2 (1), whereas in the case of Ru(CO)4I2 the reaction with Ag(tolN5tol) occurs under reduction to Ru(I), and brownish, air stable [Ru(CO)3(tolN5tol)]2 (2) is obtained.
1 crystallizes from THF as 1·THF in the monoclinic space group P21/c with a = 1395.7(4), b = 2226.5(9), c = 1973.5(7) pm. β = 105.10(2)°, Z = 4. In the binuclear complex four pentaazadienido anions act as (N1,N3)-η2, (N5)-η1 bridging ligands coordinating the Fe atoms octahedrally. 2 forms triclinic crystals with the space group P1̄ and a = 1368.6(6), b = 1393.7(6), c = 1076.1(5) pm, α = 104.59(4)°, β = 107.36(4)°, γ = 73.90(3)°, Z = 2. Two pentaazadienido ligands bridge two Ru(CO)3
+ units with their atoms N1 and N3. In addition, the Ru atoms are connected by a Ru-Ru single bond of 267.5 pm. In 1 as well as in 2 the pentaazadienido ligands exhibit planar N5 zigzag chains in the all-trans configuration. The N -N-distances are in the range of 124.2 to 137.4 pm.
Zur Chemie und Strukturchemie von Phosphiden und Polyphosphiden, 49 [1]. Bildung und Struktur des Henicosaphosphids [Li(12-Krone-4)2]3P21(THF)2 / Chemistry and Structural Chemistry of Phosphides and Polyphosphides, 49 [1]. Formation and Structure of the Henicosaphosphide [Li(12-Crown-4)2]3P21(THF)2
Authors: Fritz Gerhard , Schneider Hans-Werner , Hönle Wolfgang , Schnering Hans Georg von 
Published: March 2015

Abstract
The reaction of Li3P7(DME)3 with crown ether 12-crown-4 and (CHT)Cr(CO)3 yields a reddish oil, from which red crystals of [Li(12-crown-4)2]3P21(THF)2 (1), red crystals of Li2P16(12-crown-4)x(THF)2 as well as a not yet identified yellow substance separates. From this mixture crystals of 1 could be isolated. [Li(12-crown-4)2]3P21(THF)2 (1) crystallizes in the space group P21/a with a = 3021.1(6) pm, b = 1901.5(4) pm, c = 1603.0(4) pm, β = 95.98(3)° and Z = 4 formula units in the unit cell. The structure is characterized by isolated 1
∞[P21
3-] trianions and Li(12-crown-4)2 cations. The trianion has approximately the symmetry mm2. The bond distances d(P-P) range from 213.9 pm to 226.8 pm and are differentiated by their function in the skeleton. The bond angles β(P-P-P) are in the range 86.1° to 107.7° and image clearly the influence of the repulsion of the non-bonded electron pairs of the strained anion. The curvature of the trianion is approx. 0.8 nm-1 and is three times larger than the curvature evaluated from structural models.
1,1-Disilylethan, CH3CH(SiH3)2 / 1,1-Disilylethane, CH3CH(SiH3)2
Authors: Schmidbaur Hubert , Hager Rudolf 
Published: March 2015

Abstract
1,1-Bis(trichlorosilyl)ethane, CH3CH(SiCl3)2 (1) is readily available through catalytic hydrosilylation of vinyltrichlorosilane and silicochloroform (90% yield), or through the base-induced reduction of acetyl chloride using again silicochloroform (60%). 1 can be converted into the title compound 2 in 80% yield by lithium aluminium hydride in di-n-butylether. Compound 2 is a highly volatile liquid (bp. 40-42 °C), not spontaneously inflamable in air. which is of interest as a precursor for chemical vapour deposition of hydrogen-containing silicon/carbon alloys (a-Si, C:H) and silicon carbide. Based on thermodynamical data, it is the least stable isomer of the composition C2Si2H10.
Notizen: Das Infrarotspektrum des Tetraselentetranitrids, Se4N4 / The Infrared Spectrum of Tetraseleniumtetranitride, Se4N4
Authors: Adel Jörg , Ergezinger Christina , Figge Reiner , Dehnicke Kurt 
Published: March 2015

Abstract
The IR spectrum of solid Se4N4 has been recorded in the region of 100- 4000 cm-1 . The assignment has been made on the basis of slightly deformed D2d symmetry, which is in agreement with the X-ray structure determination.
Dreikernkomplexe mit Ferrocen-1,1'-dithiolat-Brücke / Trinuclear Complexes Containing a Ferrocene-1,1'-dithiolato Bridge
Authors: Herberhold Max , Ott Jutta 
Published: March 2015

Abstract
Trimetallic complexes Fe(C5H4-SMLn)2 (MLn = M(NO)2Cp (M = Cr. Mo, W) and M(CO)3 Cp (M = Mo, W)) containing a ferrocene-1.1'-dithiolato bridge between two group VI metals were prepared and spectroscopically characterized. The mixed species Fe(C5H4-SCr(NO)2Cp)(C5H4-SW(CO)3Cp) and the bimetallic precursors Fe(C5H4-SMLn)(C5H4-SH), (MLn=M(NO)2Cp(M=Cr,Mo), M(CO),Cp(M=Mo,W)). were also obtained. The ferrocene-thiolato ligands are stronger electron-donors than phenyl-and methyl-thiolato ligands.
Übergangsmetall-substituierte Diphosphene, XIV. Zur Reaktivität des Diphosphenylkomplexes (μ5-C5Me5)(CO)2Fe—P=P—Ar (Ar = 2,4,6-t-Bu3C6H2) gegenüber Schwefel, Selen und Tellur. Synthese und Struktur des ersten Thioxo-λ5-diphosphenyl-Komplexes (μ5-C5Me5)(CO)2Fe-P(=S)(=P-Ar) / Transition Metal Substituted Diphosphenes. On the Reactivity of the Diphosphenyl Complex (μ5-C5Me5)(CO)2Fe-P=P-Ar (Ar = 2,4,6-t-Bu3C6H2) towards Sulfur, Selenium, and Tellurium. Synthesis and X-Ray Structure Analysis of the First Thioxo-λ5-diphosphenyl Complex (μ5-C5Me5) (CO)2Fe - P(=S)(=P - Ar)
Authors: Weber Lothar , Meine Georg , Boese Roland , Niederprüm Norbert 
Published: March 2015

Abstract
The diphosphenyl complex (μ5-C5Me5)(CO)2Fe-P=P-Ar (1a) (Ar = 2,4,6-tert-Bu3C6H2) reacts with an equimolar amount of sulfur to yield the first thioxo- λ5 -diphosphenyl complex (μ5-C5Me5)(CO)2Fe-P(=S)=P-Ar (2). Heating of 2 in boiling benzene affords the metal functionalized thiadiphosphirane 3. Similarily the selenoxo-λ5 -diphosphenyl complex (μ5-C5Me5)(CO)2Fe-P(=Se)=P-Ar (5) and selena-diphosphirane 6 are synthesized. The products have been characterized by elemental analysis as well as by spectroscopic data (IR, 1H, 13C, 31P NMR, MS). The molecular structure of 2 has been elucidated by single crystal X-ray analysis.
Komplexe mit substituierten 2,5-Dihydroxy-p-benzochinonen: Die Schichtverbindung Ca[C6(i-C3H7)2O4H]2·2/3H2O / Complexes with Substituted 2,5-Dihydroxy-p-benzoquinones: The Layer Compound Ca[C6(i-C3H7)2O4H]2·2/3H2O
Authors: Robl Christian , Sheldrick George M. 
Published: March 2015

Abstract
Dark, hydrophobic single crystals of Ca[C6(i-C3H7)2O4H]2·2/3H2O were grown in aqueous silica gel. Infinite layers parallel to (001) formed by Ca2+ and [C6(i-C3H7)2O4H]- are the main feature of the crystal structure. Ca2+ is coordinated in two different manners. Ca(1) has CN7: the coordination polyhedron is a slightly distorted capped trigonal antiprism made up by one water molecule and six oxygen atoms (O(1), O(2)) of the anions which chelate Ca(1). The mean Ca(1)-O distance is 238.9 pm. The coordination polyhedron of Ca(2) is a distorted octahedron formed by six anions acting as monodentate ligands via O(3): Ca(2)-O(3) 227.3 pm. In one half of the [C6(/-C3H7)204H] anion the bonding geometry resembles that of the corresponding dianions, but in the other half the bond lengths are very similar to those observed in free 2,5-dihydroxy-p-benzoquinones. The remaining H atom of the anion is involved in strong intramolecular hydrogen bonding as well as in an intermolecular hydrogen bond.
Synthesis of Quaternary Salts from 3,3′ -Bipyridine and Dibromoalkanes
Authors: Singh Shyam K. , Summers Lindsay A. , Hick Larry A. 
Published: March 2015

Abstract
Reaction of 3,3'-bipyridine with 1,3-dibromopropane, 1,4-dibromobutane, 1.5-dibromo-pentane, 1,6-dibromohexane. 1,7-dibromoheptane and 1.8-dibromooctane affords the corresponding bridged diquaternary salts, the structures of which were confirmed by fast atom bombardment mass spectrometry. Reaction with 1,2-bromoethane gives instead 1.1"-(1,2-ethanediyl)-bis-3.3'-bipyridinium dibromide.
Synthesis of 2-Acetoacetyl- and 2-OxaIoacetyl-1,3-indandiones and Related Compounds
Authors: Hamama W. S. , Hammouda M. , Afsah E. M. 
Published: March 2015

Abstract
Claisen condensation of 2-acetyl-1,3-indandione (1) with ethyl acetate afforded the 2-acetoacetyl-1,3-indandione (2) which upon treatment with benzylamine and paraformaldehyde in a molar ratio of (1:1:2) and (1:2:4) afforded the piperidinone and the diazabicyclic derivative (4) and (5) respectively. On the other hand, Claisen condensation of 1 with diethyl oxalate yielded two products (6) and (9). The behaviour of 6 towards phenyl hydrazine, and of 9 towards selenium dioxide and double Mannich reaction were also investigated.
Synthesis and X-Ray Analysis of the (S) Enantiomer of Methyl 5-Hydroxy-3,11-di-2-pyridyl-4,5-dihydro-1H,3H-2,6-methano- 6-benz[c]azocinecarboxylate C24H23N3O3 and of the Corresponding Camphanic Acid Ester C34H35N3O6
Authors: Hesse K.-F. , Holzgrabe Ulrike , Piening Barthold 
Published: March 2015

Abstract
Methyl 5-hydroxy-3,11-di-2-pyridyl-4,5-dihydro-1H,3H-2,6-methano-6-benz[c]azocinecarb-oxylate (-)-3 is synthesized by oxidative cyclization of an N-benzyl-4-piperidone, reduction and resolution with (-)-camphanic acid chloride.
The structures of C24H23N3O3 (-)-3 and of the corresponding camphanic acid ester C34H35N3O6 (-)-5 are orthorhombic and monoclinic with space groups P212121 ((-)-3) and P21 ((-)-5). The respective cell parameters are a = 9.758(3), b = 12.815(2), c = 16.584(4) Å, Z = 4 and Dx = 1.29 g cm-3 ((-)-3) and a = 11.189(1), b = 10.591(1), c -12.84(1) Å, β = 92.53(1)°, Z = 2, Dx = 1.27 g cm-3 ((-)-5). They were refined to R (unweighed) -0.037 ((-)-3), 0.069 ((-)-5) and R (weighed) = 0.035 ((-)-3), 0.061 ((-)-5) using 965, 1722 non-equivalent reflections, respectively. The absolute configuration of (-)-3 was determined as 2S, 3R. 5R, 6R, 11 R.
Durch Trichloracetat ausgelöste Alkylierungen von Trichlormethylketonen und eine komplexe Folgereaktion [1] / Alkylations of Trichloromethylketones Effected by Trichloroacetate and a Complex Consecutive Reaction [1]
Authors: Dehmlow Eckehard V. , Raths Hans-Christian 
Published: March 2015

Abstract
A phase transfer reaction between the title ketones, sodium trichloroacetate, and an alkyl halide leads to 2a, b, 4, or 5. Whereas these com-pounds are fragmented by NaOH, sodium meth-oxide/methylmalonate/methanol give compound 8 from 5 in a complex series of consecutive rearrange-ments.
Über die Reaktion von Dicyan mit Cd(II)-Ionen Röntgenstrukturanalyse von [Cd{(CN)2}2SO2 ][AsF6]2/ The Reaction of Cyanogen with Cd(II) Ions X-Ray Structure Analysis of [Cd{(CN)2}2SO2][AsF6]2
Authors: Roesky Herbert W. , Schimkowiak Jürgen , Noltemeyer Mathias , Sheldrick George M. 
Published: March 2015

Abstract
Cd[AsF6]2 (1) reacts with cyanogen to yield [Cd{(CN)2}2SO2][AsF6]2 (2). 2 crystallizes in the space group Pnma with cell constants a = 1475.2(3); b = 821.7(3); c = 1321.2(9) pm. The coordination sphere of cadmium consists of nine atoms (one oxygen, four fluorines and four nitrogens). Cyanogen forms polymeric links.
Aluminiumbromid-Pyridiniumbromid-Verbindung: Kristallstruktur Kristallstrukturbestimmung von [Tris(pyridinium)bromid]bis(tetrabromoaluminat(III))/ Aluminiumbromide-Pyridiniumbromide Compounds: Crystal Structure Crystal Structure Determination of [Tris(pyridinium)bromide]bis(tetrabromoaluminate(III))
Authors: Burger Harald , Hensen Karl , Pickel Peter 
Published: March 2015

Abstract
The compound [(PyH)3Br][AlBr4]2 is formed by melting stoichiometric amounts of AlBr/PyHBr in a ratio of 2:3. It crystallizes in the orthorhombic space group Pbca with lattice constants a = 1365.5(2), b = 1616.0(2), c = 2783.7(3) pm, Z = 8, Dc = 2.21 g/cm3. The structure was solved from 2810 diffractometer measured intensities (Cu -Kα radiation) and refined to Rw (F) = 0.071. The cation shows three pyridinium ions attached via N - H - Br hydrogen bonds to a central bromide ion. The N - Br distances are 321(1), 321(2) and 332(2) pm.