bluuebunny/crossref_metadata_2025 huggingface dataset:
Lithium-tetrahydroaluminat in Ether: eine NMR-Untersuchung / Lithiumtetrahydroaluminate in Ether: an NMR Study
Authors: Nöth Heinrich
Published: February 2015

Ether solutions of LiAlH4 have been investigated by 27Al and 7Li magnetic resonance in the concentration range 3.75-0.0075 M. The Al-signal shows a fine structure due to Al-H coupling only at concentrations below 0.15 M. The observed chemical shift 27Al is only slightly concentration dependent. The line width of the 27Al signal, which is inversely proportional to T2*, reaches a minimum value at a concentration where the best resolution of the 27Al quintet is observed. This, however, is not matched by the 7Li line width whose minimum value was found at a somewhat higher concentration. The results are consistent with multiple ion formation at the higher concentrations and with an ion pair at low concentrations.
Oligophosphin-Liganden, I. Einfache Synthesen der trimethylenverknüpften Triphosphine RP[(CH2)3PPh2]2 und ihrer Vorstufen Ph2P(CH2)3P(H)R (R = Ph, Me) / Oligophosphine Ligands, I Convenient Syntheses of the Trimethylene-linked TriphosphinesRP[(CH2)3PPh2]2 and their Precursors Ph2P(CH2)3P(H)R (R = Ph, Me)
Authors: Arpac Ertugrul , Dahlenburg Lutz
Published: February 2015

The secondary-tertiary diphosphines Ph2P(CH2)3P(H)Ph (2) and Ph2P(CH2)3P(H)Me (3) have been prepared from Ph2P(CH2)3Cl (1) and NaP(H)Ph or LiP(H)Me, respectively. Metallation of 2 and 3 with n-butyl lithium and further reaction of the lithio-derivatives with one equivalent of 1 yields PhP[(CH2)3PPh2]2 (4) and MeP[(CH2)3PPh2]2 (5). The tritertiary phosphines 4 and 5 have likewise been obtained from RPLi2 (R = Ph, Me) and two equivalents of 1. The synthesis of 4 from PhPCl2 and two equivalents of the Grignard reagent of 1 is also reported. Each of the phosphines 1-5 was characterized by NMR and mass spectroscopy.
Tellurium in Organic Synthesis, VII [1] / Novel Synthesis of Telluroesters
Authors: Bergman Jan , Engman Lars
Published: February 2015

Four substituted tellurobenzoic acid-Te-esters (1 a-1 d) have been synthesized by a phase transfer technique from substituted benzoyl chlorides and sodium telluride.
27-p-Cumaroxy-ursolsäure, ein neuer Inhaltsstoff von Ilex aquifolium L. [1] / 27-p-Cumaroxy Ursolic Acid -a New Constituent of Ilex aquifolium L. [1]
Authors: Budzikiewicz H. , Thomas H.
Published: February 2015

The structure elucidation of 27-p-cumaroxy ursolic acid is described.
NOTIZEN. Weitere Verbindungen vom Typ A3NO3: K3NO3 und Rb3NO3 / Further Compounds Typ A3NO3: K3NO3 and Rb3NO3
Authors: Jansen Martin
Published: February 2015

K3NO3 and RbsNO3 were prepared by solid state reaction of equimolar mixtures of K2O/KNO2 and Rb20/RbN02, respectively. According to X-ray powder photographs their crystal structures are derived from the perovs-kite structure. K3NO3 is isostructural with Na3NO3 (a = 521.7 pm, Z = 1), Rb3NO3 represents a tetragonally distorted variant with a = 770.5, c = 550.8 pm and Z = 2.
Darstellung und Kristallstruktur des Dithallium(I)blei(II)tetrathiogermanats(IV) Tl2PbGeS4 / Preparation and Crystal Structure of Dithallium(I)Lead(II) Tetrathiogermanate (IV)
Authors: Eulenberger Günther
Published: February 2015

Tl2PbGeS4 was synthetized by fusion of a stoichiometric mixture of Tl2S, PbS, and GeS2, and prolonged heating of the reaction product. A single crystal could be isolated for intensity measurements on an automated four-circle single crystal diffractometer. Tl2PbGeS4 is monoclinic, space group P21/a with a = 8.907(2), b= 9.114(2), c = 10.502(3) Å, β = 94.08(2)°, and Z = 4. The crystal structure was determined by means of standard methods and refined to R = 0.065. The structure is composed of tetrahedral [GeS4]4- anions which are held together by Tl1+ and Pb2+ cations. The GeS4 tetrahedra are only slightly deformed (mean distance Ge-S: 2.220 Å). The Tl atoms are surrounded by eight S atoms at distances ranging from 3.085 to 4.055 Å forming irregular coordination polyhedra. The Pb atom is coordinated by six S atoms in a strongly distorted octahedral arrangement at distances varying from 2.803 to 3.256 A. The Pb atoms and the Tl(2) atoms are alternately situated between slabs of GeS4 tetrahedra parallel to the ab plane. The Tl(l) atoms are found within these slabs located between the GeS4 tetrahedra.
A Study of the Bonding and Geometry in Phosphacumulene Ylides
Authors: Albright Thomas A. , Hofmann Peter , Rossi Angelo R.
Published: February 2015

A series of ab initio molecular orbital calculations have been carried out on phosphacumulene ylides of the type H3P = C = C = X where X = S, O, CNH, and (OH)2. The variation in the P-C-C bond angle was examined and compared to the experimentally determined structures of analogs. The dominant factor in setting the P-C-C angle was found to be the relative π-acceptor capability of the C = X fragment in the plane of the bending motion. Quantitative PMO-arguments were constructed for the X = S, O and (OH)2 cases along this line. It is also shown, that P-C σ* character mixes into the highest occupied molecular orbital. The magnitude of this effect is dictated by the amount of bending and this strongly influences the 1JP-C nuclear spin coupling constants. Finally, the bending in H3P = C = PH3 was also investigated in a similar manner.
Zur Kenntnis der Verbindungen CaNi2As2, SrNi2As2 und Ca2,3Ni11,7As7 / On the Compounds CaNi2As2, SrNi2As2, and Ca2,3Ni11,7As7
Authors: Mewis Albrecht , Distler Astrid
Published: February 2015

Investigations of the systems Ca(Sr)-Ni-As resulted in the discovery of three ternary phases. CaNi2As2 and SrNi2As2 are isotypic and crys-tallize in the ThCr2Si2-structure (space group I 4/mmm) with the following constants:

CaNi2As2 a = 406.5(1) pm, c= 994.9(2) pm, SrNi2As2 a = 415.4(1) pm, c = 1029.0(2) pm.

Ca2.3Ni11.7As7 (a= 940.4(1) pm, c= 381.6(1)pm) crystallizes in a hexagonal lattice; a Zr2Fe12P7-structure is supposed.
Beiträge zur Chemie des Bors, CX [1]. Synthese und Reaktionen von Sila-und Phosphaborazinen / Contributions to the Chemistry of Boron, CX [1]. Synthesis and Reactions of Sila-and Phosphaborazines
Authors: Barlos Kleomenis , Nöth Heinrich
Published: February 2015

The synthesis of permethylated silaborazines starting from Br(CH3)B-NCH3-Si(CH3)2Br or Br(CH3)B-NSi(CH3)3-Si(CH3)2Br is described. These may in turn be used to prepare phosphaborazines, since phosphorus halides replace selectively the sila group from the silaborazines. The P-Cl bond of P-chloro-pentamethylphosphaborazine is more reactive than the P -N and B-N bonds of the ring and allows selective nucleophilic substitution reactions at phosphorus. The NMR data of the new compounds suggest a nonplanar ring configuration.
A Convenient Preparation Method of Anhydrous Lithium, Potassium, Rubidium and Cesium Dithiocarboxylates
Authors: Kato Shinzi , Yamada Shunji , Goto Hideyuki , Terashima Kiyomitsu , Mizuta Masateru , Katada Tomonori
Published: February 2015

It has been found that a series of anhydrous alkali metal dithiocarboxylates are readily obtained in good yields by the reaction of dithio acid with metal hydride (LiH, NaH, KH), n-butyl lithium, or rubidium or cesium acetates, respectively. Their spectral data were compared.
Reactions with the Arylhydrazones of α-Cyanoketones: Utility of Arylhydrazonomesoxalonitriles for the Synthesis of Azoles and Azolines
Authors: Hafez Ebtisam Abdel Aziz , Khalifa Mohamed Ali Elsayed , Guda Sayed Kamel Ahmed , Elnagdi Mohamed Hilmy
Published: February 2015

The arylhydrazonomesoxalonitriles derivatives 1 a - c were utilised for the synthesis of several new pyrimidine, pyridines, triazine and isoxazole derivatives.

Compound 1 a reacted with alkyl halides to yield the N-alkyl derivatives 12a, b. The latter reacted with hydrazines to yield the amidrazones 13 a, b.
Zur elektrochemischen Untersuchung von 1-Phenyl-5-mercaptotetrazolen / Electrochemical Investigation of 1-Phenyl-5-mercaptotetrazoles
Authors: Gürtler Oswald
Published: February 2015

The reductive and oxidative half-wave potentials of some phenyl-substituted derivatives of 1-phenyl-5-mercaptotetrazole were evaluated in acetonitrile.

Linear relationships between measured half-wave potentials and substituent values given by Hammett as well as influences of substituents on the electrochemical reactivity of 1-phenyl-5-mercaptotetrazoles has been studied. Furthermore, a reduction scheme of these compounds in acetonitrile at the Hg-Elektrode was established.
Spektralreines Bis(phthalocyaninato)protactinium(IV) / Spectroscopically Pure Bis(phthalocyaninato)protactinium(IV)
Authors: Lux Franz , Beck Oskar F. , Krauß Heinz , Brown David , Tso Tze C.
Published: February 2015

Spectroscopically pure PaPc2 has been prepared by reaction between PaI4 · 4 CH3CN and o-phthalic acid dinitrile in 1-chloronaphthalene followed by sublimation at 5 · 10-3 Pa in a temperature profile with three clearly defined zones (520 °C/350 °C/room temperature). This procedure gives a product almost completely free of H2Pc impurity which is known to have been present in previously reported complexes of the type AnPc2. Thus, the trace of H2Pc in the substance could only be detected by derivative spectroscopy. X-ray powder diffraction shows the compound to be isostructural with ThPc2 and UPc2. The ligand spectrum is typical of AnPc2 complexes, f-f Bands observed in a solid state spectrum provide additional proof that the compound is PaIV Pc2.
Reaktion von Imidodiphosphorsäuretetraphenylester mit Quecksilber(II)-oxid und Phenylquecksilberhydroxid / Reaction of Imidodiphosphoric Tetraphenylester with Mercury (II) Oxide and Phenylmercuryhydroxide
Authors: Richter Horst , Fluck Ekkehard , Schwarz Wolfgang
Published: February 2015

Reaction of imidodiphosphoric tetraphenylester with HgO yields the twelve-membered ring system 1, the properties, NMR and X-ray structural data of which are reported. A reaction mechanism is suggested. Reaction product from imidodiphosphoric tetraphenyl-ester and C6H5HgOH is N-phenylmercury-bis(phosphoric diphenylester)-imide (2).
Neue ternäre Phosphor-und Arsenverbindungen mit Zr2Fe12P7-Struktur / New Ternary Compounds of Phosphorus and Arsenic with the Zr2Fe12P7-Structure
Authors: Mewis Albrecht
Published: February 2015

Abstract The ternary compounds Mg2.5Ni11.5P7, Ca2.1Ni11.9P7 and Ca2.3Ni11.7As7 were structurally characterized. They are isotypic and crystallize in the Zr2Fe12P7-type (space group P6̅) with the following constants:

Mg2.5NI11.5P7, a = 907,9(1) pm, c = 355,7(1) pm,

Ca2.1Ni11.9P7, a = 910.3(1) pm, c = 367.6(1) pm,

Ca2.3NI11.7AS7, a = 940.4(1) p m , c = 381.6(1) pm.
Ba2ZnGe2S6O: Ein neues Oxidsulfid mit Tetraedergerüststruktur/On Ba2ZnGe2S6O. A New Oxide Sulfide with Tetrahedral Framework Structure
Authors: Teske Chr. L.
Published: February 2015

Ba2ZnGe2S6O was prepared for the first time and the crystal structure determined by using single crystal X-ray methods. The space group is D3
2d-P4̄21m, tetragonal (No. 113). Lattice constants: a = 963.59 ± 0.22; c = 645.06 ± 0.25 pm. The tetrahedral framework structure is described and discussed. Zn is linked only to sulfur. The oxygen belongs to the coordination sphere of Ge and Ba.
Electronic and Resonance Raman Spectra of Some New Mixed-Valence Compounds of Pt and Pd with a Metal-Halide Chain
Authors: Papavassiliou G. C. , Layek D.
Published: February 2015

The electronic and resonance Raman spectra of new mixed-valence compounds of the type M2ʹ[M(L)X3][M(L)X5], where Mʹ = K, NH4, M = Pt or Pd, L = NH3 or pyridine, and X = Cl, Br or I, have been studied. The single-crystal polarized reflectance spectra indicate the one-dimensional semiconductor behaviour. The polarized resonance Raman spectra confirm the --M(II)--X-M(IV)-X linear chain structure, which is in accordance with the X-ray results. The polarization of M-N bands can be explained by the Snyder's theory (1971).
Perfluormethyl-Element-Liganden, XXIII [1] Darstellung und spektroskopische Untersuchung von Mo(CO)5L-Komplexen (L = R2EER2ʹ , R2EEʹR; R, Rʹ = CH3, CF3; E = P, As; Eʹ = S, Se, Te)/Perfluoromethyl Element Ligands, XXIII [1] Preparation and Spectroscopic Investigation of Mo(CO)5L Complexes (L = R2EER2ʹ, R2EEʹR; R, Rʹ = CH3, CF3; E = P, As; Eʹ = S, Se, Te)
Authors: Grobe Joseph , Le Van Duc
Published: February 2015

Mo(CO)5L complexes (L = R2EER2ʹ, R2EEʹR; R, Rʹ = CH3 and/or CF3; E = P, As; Eʹ = S, Se, Te) have been prepared by reaction of Mo(CO)5THF with L at room temperature. The new compounds were characterized by analytical and spectroscopic (IR, NMR, MS) methods.
The Metal Chelates of Heterocyclic β-Diketones and their Derivatives, Part IV New Mixed Ligand Tetrakis Complexes of Lanthanides Derived from tris-Acetylacetonates and Some 4-Acyl Pyrazolones
Authors: Okafor Emmanuel Chukwuemeka
Published: February 2015

Some new mixed ligand tetrakis chelates derived from tris acetylacetonates of La, Ce, Pr, Nd, and Gd with other β-diketones, like 1-phenyl-3-methyl-4-benzoyl-pyrazolone-5 and 1-phenyl-3-methyl-4-acetyl-pyrazolone-5 have been synthesised. The compounds are characterised by elemental analyses and IR data. The UV spectral properties and the conductance in DMF have also been reported.
Übergangsmetallkomplexe von Diazenen, XV [1] Darstellung und Eigenschaften von Heterodimetallkomplexen des Typs LnM-(cis-RN=NR)-MʹLm Transition Metal Complexes of Diazenes, XV [1] Synthesis and Properties of Heterodimetal Complexes LnM-(cis-RN=NR)-MʹLm
Authors: Battaglia R. , Kisch H. , Krüger C. , Liu L.-K.
Published: February 2015

Complexes of type LnM(η2 - pentamethylenediazirine)MʹLm, LnM/MʹLm = (CO)5Cr/Mo(CO)5, (CO)5Cr/Fe(CO)4, (CO)5W/Fe(CO)4 and (CO)5Cr/Mn(CO)2
5η(-MeC5H4) were prepared from [MʹLm(THF)] or Fe2(CO)9 and (η1 -pentamethylenediazirine)MLn. The structure of the Cr/Mo complex was determined by X-ray analysis. The IR and UV-VIS data resemble those of the corresponding homodi-metal complexes.
Notizen: Darstellung, IR-Spektrum und Kristalldaten von [ReNCl3 · POCl3]4 · 2POCl3/Preparation, IR Spectrum and Crystallographic Data of [ReNCL · POCl3]4 · 2 POCl3
Authors: Liese Werner , Dehnicke Kurt , Walker Ingeborg , Strähle Joachim
Published: February 2015

The title compound is prepared by treating ReNCL with excess POCl3. The complex is isotypic with the corresponding tungsten complex [WNCl3 · POCl3]4 · 2 POCl3. The structure consists of Re4N4 eight-membered rings with alternating Re ≡ N-Re bonds. The IR spectrum was recorded and assigned.
Notizen: Regiospecific Synthesis of 1,2-Dialkylthio-7(alkyl-or aryl)thiocycloheptatrienes and 1,2-Dialkylthio-7-alkoxycycloheptatrienes
Authors: Cavazza Marino , Morganti Gioia
Published: February 2015

Hydride abstraction by trityl tetrafluoborate from a mixture of cyeloheptatriene[1,2]-and cycloheptatriene[3,4]-p-dithiine gave tropenylium[1,2]-p-dithiin tetrafluoborate. The latter was found to add either methoxide or various thiolates only at the tropenylium C-3, which constitutes the first entry to regiospecifically trifunctionalized cycloheptatrienes. In contrast, cycloheptatriene[1,7]-p-dithiine or various other cycloheptatrienes substituted at C-7 with either methylthio or t-butylthio groups were found to undergo alkylthiolate abstraction by trityl tetrafluoborate. This limits the usefulness of the above synthetic methods for polyfunctionalized cycloheptatrienes.
Die Kristallstruktur des Dodekamethyl-hexasila-tetraarsa-adamantans (Sime2)6As4 / Crystal Structure of Dodecamethyl-hexasila-tetraarsa-adamantane (Sime2)6As4
Authors: Hönle Wolfgang , Schnering Hans Georg von
Published: February 2015

Dodecamethyl-hexasila-tetraarsa-adamantane (Sime2)6As4 crystallizes in the cubic space group I 4̄3m with a = 1098.2 pm and Z = 2 formula units. The bond lengths are As-Si - 235.1 pm and C-Si - 185.9 pm. The bond angles at the As atoms are 103.2° and the Si atoms 121.0°
Zur Kenntnis der Hydrate des Mangan- und Zinksulfits. Röntgenographische, thermoanaly tische, Raman- und IR-spektroskopische Untersuchungen / Hydrates of Manganese and Zinc Sulfite. X-ray, Thermoanalytical, Raman, and IR Data
Authors: Lutz Heinz Dieter , El-Suradi Saleh M. , Mertins Christiane , Engelen Bernward
Published: February 2015

X-ray, IR and Raman data as well as thermoanalytical measurements (DTA, TG, and DTG) of several new hydrates, viz. MnSO3 · 2 ½ H2O, MnSO3 · 2 H2O, ZnSO3 · 3 H2O, β-ZnSO3 · 2 ½ H2O, and γ-ZnSO3 · 2 ½ H2O, and of previously reported hydrates in the systems MnSO3-H2O, ZnSO3-H2O, and MnSO3-ZnSO3-H2O are presented. Furthermore, the formation of mixed crystals is studied in the system MnSO3-ZnSO3-H2O. The following crystal data have been determined by single crystal measurements: MnSO3 · 2 ½ H2O (P41212) : a = b = 968.4(1), c = 1040.9(1) pm, Z = 8, MnSO3 · 2 H2O (P21/n): a = 650.9(1), b = 873.8(1), c = 774.7(1) pm, β = 99.80(1)°, Z = 4, ZnSO3 · 3 H2O (Pnma): a = 953.6(1), b = 553.0(1), c = 941.9(1) pm, Z = 4, β-ZnSO3 · 2 ½ H2O (P41212): a = b = 952.1(1), c = 1025.4(1) pm, Z = 8, γ-ZnSO3 · 2 ½ H2O (with small amount of Mn2+) (o-rh.): a = 1493(1), b = 1812(2), c = 753(1) pm, Z = 16, ZnSO3 · ½ H2O (mon.): a = 1326.7(5), b = 706.3(2), c = 834.4(1) pm, β = 117.41(3)°, Z = 8. The IR spectra show that, with the exception of γ-ZnSO3 · 2 ½ H2O, both weak and strong hydrogen bonds are present in the sulfite hydrates. Under an SO2 atmosphere the sulfite hydrates can be dehydrated without simultaneous dissociation to the oxide and sulfur dioxide. The isotypic hydrates β-MnSO3 · 3 H2O and ZnSO3 · 3 H2O (β-MnSO3 · 3 H2O type), and MnSO3 · 2 H2O and ZnSO3 · 2 H2O (ZnSeO3 · 2 H2O type) form complete mixed crystal series. Solid solutions are also formed from α-MnSO3 · 3 H2O (α-FeSO3 · 3 H2O type), γ-ZnSO3 · 2 ½ H2O, MnSO3 · 1 H2O, and ZnSO3 · ½ H2O. No incorporation of Mn or Zn could be observed for α-ZnSO3 · 2 ½ H2O and the isotype hydrates MnSO3 · 2 ½ H2O and β-ZnSO3 · 2 ½ H2O (CoSO3 ½ 2 ½ H2O type)
S4N4 und seine Derivate: α-FeCl3 · S4N4, ein Übergangsmetallkomplex mit dem S4N4-Ligand / S4N4 and its Derivatives: α-FeCl3 · S4N4, a Transition Metal Complex with the S4N4 Ligand
Authors: Thewalt Ulf
Published: February 2015

The adduct α-FeCl3 · S4N4 has been prepared from FeCl3 and S4N4 in CCl4. The new compound crystallizes in the monoclinic space group P 21/c with Z = 4 and lattice parameters a = 6.360(2), b = 13.066(4), c = 12.686(5) Å, and β = 99.43(3)°. An X-ray analysis shows that the S4N4 ring is bonded via one of its nitrogen atoms to the iron atom of the FeCl3 group and that the four ligand atoms around the iron atom form a tetrahedron. The structure of the complex is similar to the known structure of BF3 · S4N4
Darstellung und Ligandeneigenschaften eines 1.2.5-Azadiborolen-Derivates [1] / Synthesis and Ligand Properties of an 1,2,5-Azadiborolene Derivative [1]
Authors: Siebert Walter , Schmidt Hans , Full Roland
Published: February 2015

3,4-Diethyl-1,2,5-trimethyl-1,2,5-azadiborolene (3) is obtained from 3,4-diethyl-2,5-dimethyl-1,2,5-thiadiborolene (1) and heptamethyldistannazan. The Lewis-acidic π4 ligand (3) forms the transition metal complexes 5, 6, 7 and 8, when reacted with Fe2(CO)9, (C5H5)CO(CO)2, Ni(CO)4 and Co2(CO)8, respectively. The properties of 5-8 are compared with those of the corresponding thiadiborolene complexes. In contrast to 1 the azadiborolene ligand does not favor the formation of tripledecker complexes
A New Weak Base from Rauwolfia vomitoria Afzuelia
Authors: Malik Abdul , Siddiqui Salimuzzaman , Voelter Wolfgang
Published: February 2015

A new weak base from reserpine family has been isolated from Rauwolfia vomitoria Afzuelia and provisionally named as neonorreserpine. The chemical and spectral evidence established it as a distinct isomer of pseudoreserpine
Rb6In2S6 und Rb4In2S5, zwei neue Thioindate mit isolierten und verknüpften [In2S6]6- Anionen / Rb6In2Se6 and Rb4ln2S5, Two NEW Thioindates with Isolated and Connected [In2S6]6- Anions Respectively
Authors: Deiseroth Hans-Jörg
Published: February 2015

The hitherto unknown title compounds were prepared by a disproportionation reaction starting from elementary rubidium and indium monosulfide. Rb4ln2S5 crystallizes in the triclinic system (P1̄) with the lattice constants a = 931.7(2); b = 1097.6(3);c = 761.2(2)pm; a = 111.32°(2); β = 94.70°(2); γ = 103.70°(2) (Z = 2) and Rb6In2S6 in the monoclinic system (C2/m) with the lattice constants a = 895.3(2); b = 1356.9(2); c = 791.8(2) pm; β = 101.53°(2) (Z = 2). The quasi molecular [In2Se6]6- group which is isoelectronic with the gas phase molecule In2Cl6 consists of two edge sharing InS4 tetrahedra and is the basic unit of Rb6ln2S6 as well as of Rb6In2S6. The formation process, structural relationships between the two compounds and their possible role in the phase diagram of the components Rb2S and In2S3 are discussed.
Darstellung und spektroskopische Untersuchungen von Me3SiOP(S)Cl2, Me3SiOP(S)Br2 sowie Me3SiOP(O)Br2 / Preparation and Spectroscopic Properties of Me3SiOP(S)Cl2, Me3SiOP(S)Br2 and Me3SiOP(O)Br2
Authors: Shihada Abdel-Fattah , Majed Rehab
Published: February 2015

Trimethylsilyl dichlorothiophosphate (Me3SiOP(S)Cl2) and trimethylsilyl dibromothio-phosphate (Me3SiOP(S)Br2) are prepared by reactions of (Me3Si)2S with P0Cl3 and POBr3, respectively. The reaction of POBr3 with Me3SiOCOCH3 in the mol ratio 1:1 gives Me3SiOP(O)Br2, a molar ratio of 1:3 leads to (Me3SiO)3PO. The vibrational spectra have been used to elucidate the structures of the compounds. It was found that -OP(S)Cl2 as well as -OP(S)Br2 are linked to the trimethylsilyl group through the oxygen atom.
Mesoionische 4nπ-Heterocyclen, I Mesoionische 4π-Fünfringheterocyclen und 8π-Heteropentalene. Entwicklung der Systeme und Untersuchungen am 1-Oxo-lH-pyrazolo [1.2-a] pyrazol-4-ium-3-olat-Typ / Mesoionic 4nπ-Heterocycles, I Mesoionic 4π Five-Membered Heterocycles and 8 π-Heteropentalenes. Development of the Systems and Investigations on the 1-Oxo-1H-pyrazolo[1,2-a]pyrazol-4-ium-3-olate Type
Authors: Friedrichsen Willy
Published: February 2015

4n π-Mesoionic heterocycles are -with one exception -a hitherto unknown class of compounds. In this paper the possible 4 π-five-membered mesoionic heterocycles, their ring anellated derivatives and the corresponding heteropentalenes are derived. Reactions of the 1-oxo-1H-pyrazolo[1,2-a]pyrazol-4-ium-3-olate system with tetrachloro-o-benzo-quinone are described.
Reaction of Dihydroxymethyl Radical with Molecular Oxygen in Aqueous Solution
Authors: Bothe Eberhard , Schulte-Frohlinde Dietrich
Published: February 2015

Dihydroxymethyl radical (1) was found to react with oxygen diffusion controlled (k = 4.5 x 109 M-1 s-1). The final products of the reaction are formic acid and 1/2 hydrogen peroxide. The precursor of H2O2 was shown to be O2
·- which is formed with G(O2
·-) = 6.3 (a value which includes the O2
·- formed by H atoms and oxygen (G(H) = 0.55)). If it is assumed that dihydroxymethylperoxyl radicals are formed as intermediates the rate constant of O2
·- formation must be ≥ 106 s-1 . A bimolecular reaction of two dihydroxy-methylperoxyl radicals forming tetroxides does not occur at the dose rates used. The rate constants for the establishment of the equilibrium

have been determined at pH 5.7 and 19 °C to be k3=1.9x 10-2 M-1 s-1 and k-3 = 1.5 X 10-6 M-1 s-1 in aqueous solution.
Inerte Amminkomplexe als mehrwertige Kationsäuren in wäßriger Lösung / Inert Ammine Complexes as Multivalent Cationic Acids in Aqueous Solution
Authors: Kretschmer Matthias , Labouvie Lutwin , Quirin Karl-W. , Wiehn Helmut , Heck Ludwig
Published: February 2015

Acidity constants of ammine complexes of tetravalent platinum in aqueous solutions have been determined by a spectrophotometric method at very low ionic strengths and extrapolated to zero ionic strength. Temperature variations of pK-values (25 °C and 50 °C) yield thermodynamic parameters for two successive deprotonation steps of hexaammineplatinum(IV), pentaamminechloroplatinum(IV), and tris(ethylenediamine)pla- tinum(IV) complexes and for the deprotonation of pentaammineaquacobalt(III) ion.

The enthalpy changes for the first and second steps are similar and range from 50 to 75 kJ/mole while for the aqua ligand of Co(III) 33 kJ/mole are found. The very large dif­ference in the entropy changes (about 70 to 80 J/K mole for the first step and -10 to + 20 J/K mole for the second step) is interpreted by a model of solvation change. The primary hydration sphere of strongly oriented and immobilized water dipoles around the highly charged complex cation is transformed to a hydrogen-bonded solvation sheath when the electric field of the complex is weakened upon release of the first proton.
Darstellung und Eigenschaften von und Reaktionen mit metallhaltigen Heterocyclen, VII [1]. Heterolytische Spaltung der Re-Re-Bindung in den Zweikern-Anionen [(OC)4ReP(R2 )O]2
2- mit Elektrophilen - ein Weg zu Heterocyclen mit Re-σ-Bindung / Preparation and Properties of, and Reactions with, Metal-Containing Heterocycles, VII [1]. Heterolytic Cleavage of the Re-Re Bond in the Binuclear Anions [(OC)4ReP(R2)O]2
2- with Electrophiles -a Pathway to Heterocycles with Re-C-σ-Bonds
Authors: Lindner Ekkehard , Au Günter von
Published: February 2015

The preparation of the six-membered rhenacyclohexanes

(1a, b) [R = CH3 (a), C6H5 (b)] is accomplished by heterolytic cleavage of the Re-Re bond in the binuclear anions [(OC)4ReP(R2)O]2
2- with strong electrophiles like the alkanediylbis(triflate) (CH3

)2C(CH2Y)2 (Y = OSO2CF3). followed by an attack of the co-positioned carbenium-like C atom on the phosphinite oxygejn of the anion. 1 a, b insert SO2 under ring expansion yielding the seven-memberod heterocyeles

(2a, b). 1b crystallizes triclinic in the space group P1̄ with Z = 2. Some characteristic IR and NMR data are discussed.
Die Oxidation von aminosubstituierten Cyclotri(λ3-phosphazanen) mit Schwefel / Sulfur Oxidation of Amino Substituted Cyclotri(λ3 -phosphazanes)
Authors: Zeiß Werner , Klehr Hubert
Published: February 2015

Without being able to stop the reaction on the first or second stage, trisamino substituted cyclotri(λ3 -phosphazanes) (2) can be shown to add always three mole equivalents of sulfur under very mild reaction conditions to give cyclotri(λ5 -phosphazanes) (3). Suggesting the reaction to be stereospecific, 3 shows the same 31P NMR pattern as the starting materials 2. From this result and from molecular models, 3a-c as well as 2a-c are assumed to have diequatorial axial-substitution, whereas the bicyclic 2d and 3d are likely to have their phosphorus substituents in a diaxial-equatorial position.
Some Observation on Nickel(IV) Periodate
Authors: Chaudhury M. , Roy A. , Ghosh B. P. , Nag K.
Published: February 2015

Variable temperature EPR spectra of KNiIO6 · 0.5 H2O have established that the paramagnetic behavior of this compound (~ 1 BM) is due to the presence of nickel(III) atoms which have occupied some nickel(IV) sites in the crystal lattices. Change of spectral pattern from rhombic (77 K) to isotropic (300 K) is due to a dynamic Jahn-Teller effect. Electrical conductivity measurement has shown it to be a poor semiconductor. KNiIO6 · 0.5 H2O on heating at 300 °C forms K2Ni2I2O9 which is stable in the temperature range 300-400 °C. Chemical reactivities and reflectance spectrum of this compound have indicated it to be K2Ni2
III2
VIO9.
Beiträge zur Chemie des Bors, 112 [1]Zur Kenntnis von 1.3.2-Dithiaborolen [2] / Contributions to the Chemistry of Boron, 112 [1]1,3,2-Dithiaboroles [2]
Authors: Goetze Richard , Nöth Heinrich
Published: February 2015

The NMR data of this new class of compounds indicate in comparison to 1,3,2-dithia-borolanes, that the heterocycle can be looked at as a 6 π-electron system. A high degree of analogy in the mass spectrometric fragmentation of dithiaborolanes and dithiaborols exists, however, the parent ion of 2-methyl dithiaborol is more stable than that of the saturated analogon.
Compounds of Complex Halo and Pseudohalo Acids of the Group II B Metals, Part HI [1]Spectral Studies of the Hgl-
3 Ion
Authors: Perlepes S. P. , Zafiropoulos Th. F. , Kouinis J. K. , Galinos A. G.
Published: February 2015

A study has been made of the Far-IR spectra (250-30 cm-1) of the complexes HHgI3 · 2 Py and HHgI3 · 2 An (Py = pyridine and An = aniline), in the solid state. Associated anionic structures are present in the two complexes.

The UV spectrum of the aniline complex, in three solvents, shows that the HgI3
- ion is the predominant anionic species in solution.
Synthesis of Some Pyrazolo [Diazepine, Pyrazole, Isoxazole and Pyrimidine] Derivatives and Related Compounds
Authors: Afsah El-Sayed , Amer Fathy A. , Soafan Momdouh
Published: February 2015

4-Arylidene-3-methyl-1-phenyl-2-pyrazolin-5-ones (1a-d) undergoes condensation with diethylmalonate, p-nitroacetophenone and/or 3-acetyl-pyridine under Michael condition to give compounds 2, 3 and 4, respectively. Treatment of 3 and 4 with hydrazine afforded the pyrazolodiazepines 7 and 8, respectively. Interaction of la with diethyl phenyl-malonate gave the Michael product 9, which undergoes hydrolysis, decarboxylation and cyclisation to give the indanone derivative (11). Condensation of 1c with hydrazine, hydroxylamine and urea gives compounds 12, 13 and 14, respectively. Cyclisation of the Michael compound 15 gives the benzopyranopyrazole (14). When 1c was subjected to Riemer-Tiemann reaction gives compounds 17 and 18. Acetic anhydride treatment of 18 gives the acetyl cresotic acid derivative (19).
AB2X2-Verbindungen im CaAl2Si2-Typ, VIII [1] / AB2X2 Compounds with the CaAl2Si2 Structure, VIII [1]
Authors: Klüfers Peter , Neumann Hermann , Mewis Albrecht , Schuster Hans-Uwe
Published: February 2015

Thirteen new compounds were synthesized. They are supposed to crystallize with the CaAl2Si2 type of structure (space group P3̅m1) with the following constants:

SrZn2P2 a = 410.0(0) pm, c = 710.1(1) pm,

SrCd2P2 a = 433.8(0) pm, c = 726.9(1) pm,

BaCd2P2 a = 440.2(0) pm, c = 755.7(1) pm,

BaCd2As2 a = 451.6(0) pm, c = 769.3(1) pm,

BaMg2P2 a = 436.7(1) pm, c = 758.0(3) pm,

EuZn2P2 a = 408.7(1) pm, c = 701.0(1) pm,

EuZn2As2 a = 421.1(1) pm, c = 718.1(1) pm,

EuZn2Sb2 a = 448.9(1) pm, c = 760.9(1) pm,

YbZn2As2 a = 416.0(1) pm, c = 696.1(1) pm,

YbZn2Sb2 a = 444.4(1) pm, c = 742.4(1) pm,

LuZnCuAs2 a = 407.1(1) pm, c = 663.4(1) pm,

YZnCuP2 a = 398.3(1) pm, c = 652.3(1) pm,

YZnCuAs2 a = 410.4(1) pm, c = 669.2(1)pm.
Über zwei Modifikationen von "Tl2Cl3"-valenzgemischten Thallium(I)-hexahalogenothallaten(III) Tl3 [TlCl6] / On Two Modifications of "Tl2Cl3"-Mixed Valence Thallium(I)-hexahalogenothallates(III)
Authors: Böhme Reinhild , Rath Jörg , Grunwald Bernd , Thiele Gerhard
Published: February 2015

The mixed valence thallium chloride "Tl2Cl3" is polymorphous. Raman spectra and comparable lattice translations suggest similar structures of both modifications.

The crystal structure of the rhombic α-Tl2Cl3 crystallizing in yellow, needle-shaped crystals, has been determined from three-dimensional X-ray diffraction data. The unit cell with cell parameters a= 1474.8(5) pm, b - 2508.7(6) pm and c = 1267.6(2) pm contains 16 formula units distributed on 24 independent atom positions. The compound is a mixed valence thallium(I)-hexachlorothallate(III) Tl3[TlCl6] because three of the nine independent Tl atoms are surrounded octahedrally by CI atoms in distances of 250-265 pm, while the other Tl atoms have seven, eight or nine CI neighbours variing between 306 and 383 pm.

β-Tl3[TlCl6] forms pale yellow thin platelets and crystallizes monoclinic with cell parameters a = 2549.4(13) pm, 6 = 1469.9(8) pm, c = 1308.5(12) pm and β = 108.58°.
Synthesis of Some Diazepinones, Oxazepinones, Pyrimidoquinazolinones and Related Compounds from 1,4-Bis(ethoxycarbonyl)-2,5-diamino-1,4-cyclohexadiene
Authors: Amer Fathy A. , Afsah El-Sayed , Metwally Mohamed A. , El-Zimaity Mohamed T.
Published: February 2015

Interaction of o-phenylenediamine with 1,4-Bis-(ethoxycarbonyl)-2,5-diamino-1,4-cyclo-hexadiene (1) gave 2, which cyclised to the hexahydrobenzodiazepinone (3). On the other hand, interaction of 1 with o-aminophenol, gave compound 4 which on treatment with polyphosphoric acid gave the tetrahydrobis-benzooxazepinone (11). Treatment of 1 with phenylisothiocyanate and formamide afforded the dithiopyrimidoquinazolinone (8) and the tetrahydropyrimidoquinazolinone (9), while the interaction of 1 with benzenesulphonyl-chloride gave dibenzenesulphonamido-cyclohexadiene dicarboxylate (10). The structure of these compounds was established by chemical and spectroscopic methods.
Studies on Vitamin B12 and Related Compounds, 51 [1] Direct Syntheses of Alkylcobalamins from Alkanes and Vitamin B12r under "Oxidizing-Reducing" Conditions
Authors: Maihub Abdussalam , Xu Hui Bi , Schrauzer Gerhard N.
Published: February 2015

Syntheses of methylcobalamin from methane, and of n-alkylcobalamins from n-alkanes (C2→C10) and vitamin B12r are described. The compounds are formed under "oxidizing-reducing" conditions: Oxygen radicals (O2-, HOO·, and HO·) are generated from the reaction of O2 with reducing metal ions, notably V+3 (aq) and abstract hydrogen from the alkane substrates. The resulting alkyl radicals are captured by vitamin Bj2r with high efficiency to yield alkylcobalamins. The reactions take place at room temperature in mildly alkaline or acidic solutions. In addition to n-alkylcobalamins, the preparation of neopentylcobalamin from neopentane, of isobutylcobalamin from isobutane, and of several cycloalkylcobalamins from cycloalkanes, is also reported. Methyl radicals generated in D2O from CH4 under "oxidizing-reducing" conditions are reduced to yield CH3D.
Molekül- und Kristallstruktur des 1.5-Dichlor-3.7-bis(trifluormethyl)-4.8-bis(2′.6′-dimethylphenyl)-2.6.9-trioxa- 4.8-diaza-1.5-diborabicyclo [3.3.1] nonadiens / Molecular and Crystal Structure of 1,5-Dichloro-3,7-bis(trifluoromethyl)-4,8-bis(2′,6′-dimethylphenyl)-2,6,9-trioxa-4,8-diaza- 1,5-diborabicyclo[3,3,1 ]nonadiene
Authors: Clegg William , Noltemeyer Mathias , Sheldrick George M. , Maringgele Walter , Meller Anton
Published: February 2015

The structure of the title compound (a = 1185.4, b = 1197.7, c = 1764.8 pm, β = 73.96°, space group P21/c) has been determined from X-ray diffractometer data. The molecule is structurally analogous to the tetraborate ion [B4O7]2-. The eight-membered ring is folded by 104° about the B - B vector. The boron atoms are more strongly bonded to the bridging oxygen [B-O(B) 139 pm] than to the other atoms [B-O(C) 155 pm, B-N 160 pm, B-Cl 182 pm].
Kristallstruktur von NH4CuS4 / The Crystal Structure of NH4CuS4
Authors: Burschka Christian
Published: February 2015

NH4CuS4 was prepared according to syntheses reported in the literature. Orthorhombic crystals could be grown (P212121, a = 5.249(1), b = 8.444(2), c = 12.782(2) Å , Z = 4), the structure of which was solved from X-ray diffractometer data (R = 0.031 for 767 obs. reflections). In the solid state (CuS4)--chelate rings are linked via additional Cu-S-bonds to form one-dimensional polymeric anions.
Die Kristallstruktur des 1:1-Komplexes von Antimontrichlorid und 2.2′-Bipyridin / The Crystal Structure of the 1:1 Complex of Antimony Trichloride and 2,2′-Bipyridine
Authors: Lipka Annegret , Wunderlich Hartmut
Published: February 2015

The crystal structure of the complex compound of SbCl3 with a chelating bipyridyl group was determined. Sb(C10H8N2)Cl3 crystallizes in the space group P21/c with a = 818.9(4), b = 695.8(7), c = 2331.3(12) pm, β = 103.59(4)° and Z = 4 molecules per unit cell. The SbCl3 fragment is T-shaped with  at 254.7 pm. Taking into account also the N atoms of the chelating 2,2′-bipyridyl group ( = 228.1 pm) and an intermolecular Sb···Cl contact at 334.0 pm the Sb coordination is distorted octahedral.
Studies on Unstabilized π-Sulfuranes: Synthesis of trans-1,2-Disubstituted Epoxides
Authors: Tewari R. S. , Awasthi A. K. , Chaturvedi S. C.
Published: February 2015

4-Nitrobenzylidenedimethylsulfurane, a semi-stabilized sulfonium ylide has been generated by the attack of methylsulfinyl carbanion in dimethyl sulfoxide and reacted with a series of substituted benzaldehydes, furfural and benzylideneacetophenone to afford trans-1,2-disubstituted epoxides in fair to good yields. The structural assignments of the products are based on IR and NMR spectral evidences.
8-Hydroxy-4-methoxy-monothiochinaldinsäure - eine weitere Thiosäure aus Pseudomonas [1]. / 8-Hydroxy-4-methoxymonothioquinaldic Acid - a Further Thioacid from Pseudomonas
Authors: Neuenhaus W. , Budzikiewicz H. , Korth H. , Pulverer G.
Published: February 2015

The structure elucidation of 8-hydroxy-4-methoxy monothioquinaldic acid -a meta-bolite from Pseudomonas fluorescens -is described.
Hochauflösungs-13C-NMR-Spektroskopie, VI [1]. Strukturabhängigkeit der 13C,H-Kopplungskonstanten in 6.6-disubstituierten Fulvenen / High Resolution 13C NMR Spectroscopy, VI [1]. Structure Dependence of the 13C,H Coupling Constants in 6,6-Disubstituted Fulvenes
Authors: Braun Siegmar , Eiehenauer Ulrich
Published: February 2015

In order to study the structure dependence of the 13C,H couplings in the fulvene system the 1H-coupled 13C NMR spectra of 6,6-disubstituted fulvenes (R = R′ = C6H5, CH3, cyclopropyl and N(CH3)2) were recorded and the interesting couplings determined with high accuracy by complete analysis. They have values typical for unsaturated five membered rings with vastly localised double bonds like cyclopentadiene-1,3 and spiro[2.4]heptadiene- 4,6 and show characteristic correlations with structure parameters.
Synthesis of 3β-Acetoxy-7a-aza-B-homo-22a-spirost-5(6)-en-7-one
Authors: Singh Anil K. , Dhar Durga N.
Published: February 2015

Chromic acid oxidation of diosgenin acetate yielded 7-ketodiosgeninacetate. Oximation of the ketone followed by Beckmann rearrangement of oxime afforded the title compound.
4.4.4-Trichlor-⊿2-1-butenyl-dichlorphosphat und -diehlorphosphit, zwei Reagentien für die Synthese von Oligonukleotiden / 4,4,4-Trichloro-⊿2-1-butenyl-dichlorophosphate and -dichlorophosphite, two Reagents for the Synthesis of Oligonucleotides
Authors: Seidel Peter , Ugi Ivar
Published: February 2015

The preparation of 4,4,4-Trichloro-⊿2-l-butenyl-dichlorophosphate and -dichlorophosphite from the corresponding P(V) and P(III) compounds is described.
Notizen: Darstellung und IR-Spektrum von OsO4 · 2 SbCl5 / Preparation and IR Spectrum of OsO4 · 2 SbCl5
Authors: Dehnicke Kurt , Lößberg Rainer
Published: February 2015

Osmiumtetroxide and antimony pentachloride form a donor acceptor complex, OsO4 · 2 SbCl5. According to the IR spectrum the complex contains OsOSb bridges. With VCl4, TiCl4, MOCl5 and osmiumtetroxide rapid ligand exchange reactions occur, forming VOCl3, TiOCl2 and several oxochlorides of molybdenum and OsCl4, respectively.
Notizen: Nachweis eines doppelt verbrückenden MoS4
2- -Liganden zwischen Fe-Zentren mit dem Resonanz-Raman-Effekt und einfache Darstellung von [(C6H5)4P]2[Cl2FeS2MoS2FeCl2] / Identification of a Doubly Bridging MoS4
2- Ligand between Fe-Centers by the Resonance Raman Effect and a Simple Preparation of [(C6H5)4P]2[Cl2FeS2MoS2FeCl2]
Authors: Müller Achim , Sarkar Sabyasachi , Dommröse Anne-Marie , Filgueira Roberto
Published: February 2015

A very simple preparation method for the complex [Cl2FeS2MoS2FeCl2]2- is described and Fe2+/MoS4
2- interactions are discussed. The Resonance Raman Effect is a sensitive probe for the doubly bridging MoS4
2- ligand.
Stoßaktivierungs-Massenspektren von C6H6M+ -und C7H7M+ - Fragment-Ionen aus Übergangsmetall-π-Komplexen /Collisional Activation Mass Spectra of C6H6M+ and C7H7M+ Fragment Ions from Transition Metal π-Complexes
Authors: Müller Jörn , Lüdemann Frerk
Published: February 2015

Comparative structure investigations of simple gaseous ions formed by electron impact of organometallic π-complexes have been carried out by use of the collisional activation (CA) technique. The CA mass spectra of C6H6M+ ions (M = V, Cr, Fe) arising either from benzene or from methylcyclopentadienyl metal compounds show significant differences indicating different structures of these fragments. Similar observations were made with C7H7M+ ions produced from benzyl or cycloheptatrienyl chromium tricarbonyl derivatives, although the metal-free ligand ions exhibit identical CA mass spectra. The C6H6V+ -ion arising from C5H5VC7H7 by a rearrangement fragmentation was shown to have the π-benzene vanadium structure.
Some New 1-D Compounds with Metal-Halide Chain
Authors: Layek D. , Papavassiliou G. C.
Published: February 2015

Some new mixed valence compounds of the type [M(L-L)2M(L-L)2X2]Y4 (where M = Pt or Pd, L-L = 2NH3 or ethylenediamine, X = Cl, Br or I and Y = HSO4, 1/2 SO4, ClO4 or 1/2 PtCl4) have been synthesized. The polarized Raman spectra of single crystals show the anisotropic character and the presence of ---M(II)---X-M(IV)-X chains. The method of preparation and the chemical behaviour correspond to the mechanism of the formation of Magnus green salt oxidized product.
Non Deprotonated Metal Complexes of the Bis-amide Tetradentate Ligand N,N′ -(Dipicolyl) -1,8-naphthylenediamine
Authors: Zafiropoulos Th. F. , Perlepes S. P. , Ioannou P. V. , Tsangaris J. M. , Galinos A. G.
Published: February 2015

Complexes of the general formula M(LH2)Cl2 · 2 H2O, where LH2 = N,N′-(dipicolyl)-1,8-naphthylenediamine and M = Mn, Ni and Cu, have been prepared. None of the metal ions used promote amide deprotonation on coordination: LH2 acts as a tetradentate ligand.

Distorted octahedral stereochemistries for the complexes in the solid state have been proposed utilising microanalyses, magnetic susceptibilities, molar conductance measurements and IR and visible spectral data. The Ni(II) complex exhibits evidence of a polymeric structure.
Cyclische Diazastannylene, X [1] Die Kristall-und Molekülstruktur eines Moleküls mit verzerrt-würfelförmigem Sn4N3O-Käfig / Cyclic Diazastannylenes, X [1] The Crystal and Molecular Structure of a Molecule with a Distorted Cube-Shaped Sn4N3O-Cage
Authors: Veith M. , Recktenwald
Published: February 2015

The crystal and molecular structure of (me3CN)3(me3A1O)Sn4 has been determined from three-dimensional X-ray data (4-circle diffractometer, R - 0.048). The crystals are mono-clinic, space group P2i/c, with cell dimensions a = 1017.4(5), b - 1488.5(7), c = 1748(1) pm, β-91.5(1)° and Z - 4. The molecules approach 3m point-symmetry and include a Sn4N3O-cage, the atoms occupying the corners of a distorted cube formed by two, differently sized, interpenetrating concentric tetrahedra of tin and nitrogen/oxygen atoms. The nitrogen atoms are attached to tert-butyl groups, whereas the oxygen atom of the cage acts as a base towards the aluminiumtrimethyl group. Typical bond distances and angles (mean values) are: Sn-N = 219.9, Sn-0 = 220.3 pm; N-Sn-N = 81.2°; N-Sn-0 = 79.0°; Sn-N-Sn = 98.8° and Sn-O-Sn -100.2°.
Diazaborolidyl - ein stabiler Substituent an Schwefel-Stickstoff-Verbindungen / Diazaborolidyl - a Stable Substituent at Sulfur Nitrogen Compounds
Authors: Haubold Wolfgang , Günter Hans , Frey Gerhard
Published: February 2015

2-Chlor-diazaborolidine, [CH2-N(CH3)]2BC1 (5) and N-silylated sulfur nitrogen compounds with sulfur in the oxidation state + 4 or + 6 react to form the boranes 7-11 which are thermally stable compounds. Reactions with other chlorboranes like [(CH3)2N]2BC1,

(6), (C6H5)2BCl or C6H5BCl2 as starting materials lead to less stable or unstable compounds. Spectroscopic data of the new compounds are given.
Pt(II)-, Pd(II)-und Cu(II)-Komplexe mit dem 4.4.5.5-Tetramethylimidazolin-1-oxyl-2-m-pyridyl-3-oxid-Liganden / Pt(II), Pd(II) and Cu(II) Complexes with the Ligand 4,4,5,5-Tetramethylimidazohne-1-oxyl-2-m-pyridyl-3-oxide
Authors: Schwarzhans Karl E. , Stuefer Alfons
Published: February 2015

The stable free radical 4,4,5,5-tetramethylimidazoline-1-oxyl-2-m-pyridyl-3-oxide has been prepared and used as a ligand in platinum(II), palladium(II) and copper(II) complexes. The magnetic moments and the EPR spectra of the complexes and the free radical have been investigated. The complexes show a considerable interaction between the nitroxyl radicals of the ligands.
The Metal Complexes of Heterocyclic β-Diketones and their Derivatives, Part VIII Synthesis, Structure, Proton NMR and Infrared Spectral Studies of the Complexes of Al(III), Fe(III), Co(III), Rh(III), In(III), and Zr(IV) with l-Phenyl-3-methyl-4-trifluoroacetyl-pyrazolone-5 (HPMTFP)
Authors: Okafor Emmanuel Chukwuemeka
Published: February 2015

New complexes of Al(III), Fe(III), Co(III), Rh(III), In(III) and Zr(IV) with 1-phenyl- 3-methyl-4-trifluoroacetyl-pyrazolone-5, (HPMTFP), have been synthesized and characterized by means of elemental analyses, conductivity and magnetic moment measurements, proton NMR and infrared spectroscopy. It is concluded that the ligand, HPMTFP, reacts as a bidentate enol forming neutral metal chelates. The PMR spectra of chelates sufficiently soluble in deuterated NMR solvents were recorded and studied. The IR spectra are measured between 4000-200 cm-1 and assignments are proposed for the observed frequencies. The M-O stretching frequency follows the order: AI > Rh > Fe = Co = Zr > In.
Die Darstellung von 1.3-Dunethyl-6-hydroxy-dihychothymin durch photochemische Wasser-Addition an 1.3-Dimethyl-thymin+ / Preparation of 1,3-Dimethyl-6-hydroxy-dihydrothymine by Photochemical Addition of Water to 1,3-Dimethyl-thymine+
Authors: Fahr Egon , Fecher Peter
Published: February 2015

UV irradiation of aqueous solutions of 1,3-dimethyl-thymine with wavelength > 280 nm yields the eis-and trans-form of water addition product 1,3-dimethyl-6-hydroxy-dihydro-thymine (2/3).
Aktivierung von Steroidsystemen zu alkylierenden Agenzien / Activation of Steroid Systems to Alkylating Agents
Authors: Wilk Manfred , Schmitt Karlheinz
Published: February 2015

7-Dehydrocholesterol and ergosterol are oxidised by iodine and FeCl3 under "physiologically similar" conditions to highly reactive alkylating species. These can be trapped by nucleophiles, such as 1-methylimidazole.

The oxidation of the sterols to those alkylating species is discussed as a model-reaction for the first step in chemical carcinogenesis by endogene substrates.
Beiträge zur Chemie des Phosphors, 89 [1] Cyclisierung eines 1.3-DihaIogen-1.2.3- triorganyltriphosphans zum entsprechenden Triorganyl-cyclotriphosphan / Contributions to the Chemistry of Phosphorus, 89 [1] Cyclization of a 1,3-Dihalogen-1,2,3- triorganyltriphosphane to the Corresponding Triorganyl-cyclotriphosphane
Authors: Baudler Marianne , Hellmann Jochen
Published: February 2015

Tri-tert-butyl-cyclotriphosphane is obtained by the dehalogenation of 1,3-diiodo-1,2,3-tri-tert-butyl-triphosphane with lithiumhydride. This reaction represents a so far unknown type of ring-closure leading to cyclotriphosphanes, which corresponds to the classical synthesis of cyclopropanes starting from 1,3-dichloropropanes.
Darstellung von Antimon(V)tetrafluoridpentafluorotellurat(VI), SbF4OTeF5 und Antimon(V)trifluorid-bis[pentafluorotellurat(VI)], SbF3(OTeF5)2 / Preparation of Antimony(V)tetrafluoridepentafluorotellurate( VI), SbF4OTeF5 and Antimony(V)trifluoride-bis[pentafluorotellurate( VI)], SbF3(OTeF5)2
Authors: Leitzke Ortwin , Sladky Fritz
Published: February 2015

The interaction of SbF5 with B(OTeF5)3 yields SbF4OTeF5 and SbF3(OTeF5)2.
Isolation of a New Natural Quinone, 2-Hydroxy-6-methoxy-3,5-dimethyl-1,4-benzoquinone, from the Potato Culture Solation of Phoma wasabiae Yokogi
Authors: Soga Osamu , Iwamoto Hidetoshi
Published: February 2015

2-Hydroxy-6-methoxy-3,5-dimethyl-1,4- benzoquinone was found in the blackish potato culture solution of Phoma wasabiae.
Über die Reaktion von [(C0)4FeC(O)NMe2]-[C(NMe2)3]+ mit einigen Diorganylbromboranen / On the Reaction of [(C0)4FeC(O)NMe2]-[C(NMe2)3]+ with Some Diorganoboron Bromides
Authors: Petz W.
Published: February 2015

The carbamoyl complex [(CO)4FeC(O)NMe2][C(NMe2)3] (1) reacts with boron halides of the type BrBR2 (R = Me, Ph, NMe2) at low temperature to give the boroxycarben complexes 2, which decompose at ambient temperature to the aminoboranes 3 and Fe(CO)5. The 1NMR and IR spectra of the new compounds 2 are reported.