| 1 | Author
| F. Fehér, B. Engelen | Requires cookie* | | Title
| Beiträge zur Chemie des Schwefels, 116 [1] Kristall-und Molekülstrukturen von 1.2.4.5-Benzotetrathiepin und 3-Methyl-1.2.4.5-benzotetrathiepin Contributions to the Chemistry of Sulfur, 116 [1] Crystal and Molecular Structures of 1,2,4,5-Benzotetrathiepine and 3-Methyl-1,2,4,5-benzotetrathi  | | | Abstract
| The structures of 1,2,4,5-benzotetrathiepine and 3-methyl-l,2,4,5-benzotetrathiepine were determined by X-ray structure analysis. The constitution of the molecules, which was proposed by way of spectroscopic data, could be verified. The conformation of the seven-membered rings is the chair form. The position of the methyl group in 3-methyl-1,2,4,5-benzotetrathiepine is equatorial with respect to the seven-membered ring. Details of the conformations are discussed. Bond distances and angles are compared with those in other molecules, which have similar structures. | | |
Reference
| Z. Naturforsch. 34b, 426—430 (1979); eingegangen am 18. Oktober 1978 | | |
Published
| 1979 | | |
Keywords
| X-ray, Cyclosulfanes, Conformation | | |
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| default:Reihe_B/34/ZNB-1979-34b-0426.pdf | | | Identifier
| ZNB-1979-34b-0426 | | | Volume
| 34 | |
2 | Author
| Paul Binger, MichaelJ. Doyle, Carl Krüger, Yi-Hung Tsay | Requires cookie* | | Title
| Metallacycloalkane, III [1] Darstellung und Charakterisierung von a.a'-Dipyridyl-Nickelacyclopentan Preparation and Characterisation of a,a'-Bipyridyl-nickelacyclopentane  | | | Abstract
| The title compound was synthesised from bis-l,5-cyclooctadienenickel, a,a'-bipyridyl and 1,4-dibromobutane in 83% yield and its structure determined by X-ray diffraction (a = 16.600, b = 10.837, c = 14.815 Ä; ß = 153.05°; C2/c, Z = 4; symmetry: C2 with square planar coordinated nickel; Ni-C: 1.949 A). a,a'-Bipyridylnickelcyclopentane reacts with maleic anhydride or methylacrylate under reductive elimination to give cyclobutane in 75 and 57% yield; considerable amounts of butenes are formed, in addition to cyclobutane, upon reaction with borontrifluoride-dibutylether or on thermolysis. | | |
Reference
| Z. Naturforsch. 34b, 1289—1292 (1979); eingegangen am 16. Mai 1979 | | |
Published
| 1979 | | |
Keywords
| Nickelacyclopentane, Preparation, Metallacycloalkane, X-ray | | |
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| default:Reihe_B/34/ZNB-1979-34b-1289.pdf | | | Identifier
| ZNB-1979-34b-1289 | | | Volume
| 34 | |
3 | Author
| B. Engelen, C. Freiburg | Requires cookie* | | Title
| Kristallstruktur von Mangan(II)sulfit-Trihydrat, a-MnS03 * 3 H20 Crystal Structure of Manganese(II)sulfite Trihydrate, a-MnS03 * 3 H2O  | | | Abstract
| The structure of a-MnS03 • 3 H20, space group P2i/n, Z = 4, Dm = 2.42, Dx = 2.425gcm-3, a = 6.6501(3), b = 8.9065(4), c = 8.7925(4) Ä, ß=* 96.105(3)°, was solved by the Patterson method and refined by Fourier and least-squares methods. All H atoms were located. The final R's are 2.1/3.2% for the 1749 observed/2280 measured reflexions. Coordination of Mn is octahedral involving O atoms from three water molecules and three different sulfite groups. MnOß octahedra are linked through sulfite sulfur. The Mn-0 distances range from 2.149(2) to 2.314(2) A. The S-0 distances of the sulfite group are 1.529(2), 1.529(2) and 1.544(2) A. The first two are elongated by one, the latter by two H bonds. The O-S-O angles are 103.25(9), 104.18(9) and 104.35(9)°. | | |
Reference
| Z. Naturforsch. 34b, 1495—1499 (1979); eingegangen am 9. Juli 1979 | | |
Published
| 1979 | | |
Keywords
| X-ray, Sulfites, Sulfite Hydrates | | |
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| default:Reihe_B/34/ZNB-1979-34b-1495.pdf | | | Identifier
| ZNB-1979-34b-1495 | | | Volume
| 34 | |
5 | Author
| Joachim Fuchs, Ernst-Peter Flindt | Requires cookie* | | Title
| Darstellung und Strukturuntersuchung von Polywolframaten Ein Beitrag zur Aufklärung des Parawolframations A A Contribution to the Paratungstate A Problem  | | | Abstract
| Polytungstates are obtained by the reaction of hydrated tungsten (VI) oxide with bases or salts after occasional addition of organic solvents. With liquid ammonia the as yet unknown ditungstate, (NH4)2W2Ü7, is produced. Its IR spectrum has few absorption bands suggesting a very simple constitution. Piperidine yields 5 compounds according to varied experimental conditions, which all exhibit approximately paratungstate composi-tions but different crystal habits, lattice parameters, solubility and IR spectra. Structure determinations indicate that two of these compounds are heptatungstates, the anion of which, W7024 6-, has the same structure as the heptamolybdate ion, Mo7024 6 ~. From a comparison of their Raman spectra with the spectrum of a freshly acidified sodium tungstate solution (designated as Paratungstate A) it may be concluded that the heptatungstate ion is the predominant species in such a solution. The anion structure of the previously described tributylammonium(5:24):tungstate [(GiHg^NHJsHaW^C^o was elucidated by X-ray methods. Here the tungsten atoms show the same arrangement as in the a-dodecatungstatophosphate ion (Keggin structure). | | |
Reference
| Z. Naturforsch. 34b, 412—422 (1979); eingegangen am 28. November 1978 | | |
Published
| 1979 | | |
Keywords
| Properties, X-ray, Heptatungstate, Paratungstate A, Metatungstate | | |
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| default:Reihe_B/34/ZNB-1979-34b-0412.pdf | | | Identifier
| ZNB-1979-34b-0412 | | | Volume
| 34 | |
6 | Author
| M. Schweizer, Hk Müller-Buschbaum | Requires cookie* | | Title
| Zur Verbindungsbildung von MeO : M203, Teil III Zur Kenntnis von BeGa204 Compound Formation Me0:M203, Part III BeGa2C>4  | | | Abstract
| A new compound, BeGa204, was prepared by high temperature reaction between BeO and Ga203. X-ray single crystal investigations show a hitherto unknown structure type of M2+M23+04 compounds. BeGa204 crystallizes with hexagonal symmetry a = 775.0 and c = 298.0 pm, space group C£h-P63/m. Be 2+ and Ga 3+ are statistically distributed and are surrounded by 0 2--tetrahedra. | | |
Reference
| Z. Naturforsch. 34b, 1067—1069 (1979); eingegangen am 10. Mai 1979 | | |
Published
| 1979 | | |
Keywords
| Beryllium, Gallium, Oxide, X-ray, Crystal Structure | | |
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| default:Reihe_B/34/ZNB-1979-34b-1067.pdf | | | Identifier
| ZNB-1979-34b-1067 | | | Volume
| 34 | |
7 | Author
| Beate Zimmer-Gasser, Dietmar Neugebauer, Ulrich Schubert, HansH. Karsch | Requires cookie* | | Title
| Funktionelle Trimethylphosphinderivate, XIII [1] Stabilisierte Carbanionen: Die Molekülstruktur von {[(CHa^PJgCjla Functional Derivatives of Trimethylphosphine, XIII [1] Stabilized Carbanions: The Molecular Structure of {[(CH3)3P]3C}l2  | | | Abstract
| The title compound crystallizes in the space group Cmc2i with a = 1086(1), b = 1333(1) and c — 1264(1) (Z = 4). The cation exhibits C8-symmetry with a crystallographic mirror plane perpendicular to the plane of the cation. Thus only two of the three phosphonium groups are stereochemically equivalent. In the planar P3C-moiety the P-C distances are 175 pm, the P-C-P angles 126.5° and 116.7°, respectively. | | |
Reference
| Z. Naturforsch. 34b, 1267—1269 (1979); eingegangen am 11. Juni 1979 | | |
Published
| 1979 | | |
Keywords
| Stabilized Phosphorous Ylid, Charge Derealization, X-ray | | |
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| default:Reihe_B/34/ZNB-1979-34b-1267.pdf | | | Identifier
| ZNB-1979-34b-1267 | | | Volume
| 34 | |
9 | Author
| Ingrid Pilz, K. Arin Goral, FriedrichV D Haar | Requires cookie* | | Title
| Phenylalanyl-tRNA Synthetase from Baker'Yeast: Structural Organization of the Enzyme and Its Complex with tRNAPhe as Determined by X-Ray Small-Angle Scattering  | | | Abstract
| The quaternary structure of the phenylalanyl-tRNA synthetase and its complex with tRNAPhe was studied in dilute solutions by small angle X-ray scattering. For the free synthetase the radius of gyration was determ ined as 5.5 nm, the volume 523 nm 3, the maximum diam eter 17.5 nm and the m olecular weight as 260 000 using an isopotential specific volume of 0.735. The overall shape could be best approxim ated by a flat cylinder with dimensions 18.2 n m X l l .5 n m X 4 nm ; the loose structure was approxim ated by building up the cylinder by spheres (diam eter 4.2 n m). The corresponding param eters of the enzyme tRN A complex were the following: radius of gyration 5.9 nm, volume 543 nm 3, maximum diam eter 21 nm and m olecular weight 290 000. These param eters suggest an 1:1 complex, whereby it m ust be assumed that the tRN A m olecule is attached in the extension of the longer axis. From the difference in the distance distribution functions of the free enzyme and the complex it is evident that we have to assume a change of conform ation (contraction) of the enzyme upon the binding of the specific tRNA. | | |
Reference
| Z. Naturforsch. 34c, 20 (1979); received November 20 1978 | | |
Published
| 1979 | | |
Keywords
| X-Ray, Small-Angle, Scattering, Enzyme, Complex | | |
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| default:Reihe_C/34/ZNC-1979-34c-0020.pdf | | | Identifier
| ZNC-1979-34c-0020 | | | Volume
| 34 | |
10 | Author
| Axel Thiele, Joachim Fuchs | Requires cookie* | | Title
| Struktur und Schwingungsspektren von Monomolybdaten und Monowolframaten organischer Kationen Structure and Vibrational Spectra of Monomolybdates and Monotungstates with Organic Cations  | | | Abstract
| The crystal structures of dicyclohexylammonium-monomolybdate dihydrate [(C6Hh)2NH2]2MO04 • 2 H2O, (I), cyclohexylammonium-monomolybdate, (C6HHNH3)2MO04, (II) and terf-butylammonium-monotungstate, (C4HgNH3)2W04, (III), were elucidated. In I the anion has nearly tetrahedral structure, in II one Mo-0 distance is significantly shorter than the other three, and in III all four W-0 distances are different. In spite of the variety of structures the following basic principles are recognizable: 1) Each hydrogen atom of the cationic amino groups as well as of the water of crystallization forms hydrogen bridges. 2) Never are oxygen atoms of the same M0O4 connected by these bridges, but always oxygen atoms of neighbouring M0O4 units. 3) From an oxygen atom emanate either two or no hydrogen bridge. For the investigated molybdates (tungstates) there are in all instances isomorphous tungstates (molybdates). The number and position of the vibrational bands is in good agreement with the observed anion symmetry Td, C3V and Ci, respectively. | | |
Reference
| Z. Naturforsch. 34b, 145—154 (1979); eingegangen am 23. Oktober 1978 | | |
Published
| 1979 | | |
Keywords
| Monomolybdates, Monotungstates, Organic Cations, Properties, X-ray, Vibrational Spectra | | |
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| default:Reihe_B/34/ZNB-1979-34b-0145.pdf | | | Identifier
| ZNB-1979-34b-0145 | | | Volume
| 34 | |
11 | Author
| W. Stoeger, A. Rabenau | Requires cookie* | | Title
| Darstellung, Eigenschaften und Kristallstruktur von TlgAu^j 0 Preparation, Properties, and Crystal Structure of TI6AU2I10  | | | Abstract
| TI6AU2I10 forms black crystals with a golden luster. In a closed system the temperature of decomposition is 276 °C. In vacuum or under inert gas TlßA^Iio decomposes above 65 °C forming 1 mol I2. Above 180 °C a second mol I2 is formed giving Til and gold. The space group is P 62c with the lattice constants a = 10.569 and c = 13.431 A and Z = 2. TI6AU2I10 is built up by a framework of Tlßlß with channels parallel to the c-axis. These channels contain Au + mainly with a trigonal planar coordination or linear IJj-polyiodide ions and I -ions, resp. | | |
Reference
| Z. Naturforsch. 34b, 685—692 (1979); eingegangen am 24. Januar 1979 | | |
Published
| 1979 | | |
Keywords
| X-ray, Structure Determination, Polyhalides, T1 Halides, Au Halides | | |
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| default:Reihe_B/34/ZNB-1979-34b-0685.pdf | | | Identifier
| ZNB-1979-34b-0685 | | | Volume
| 34 | |
12 | Author
| Alfred Schmidpeter, Heinz Eiletz, Joachim Von Seyerl, Gottfried Huttner, @bulletH N Jr, Ph 2%, ^. Pph, N. Ph, P. ^pph, Ch, N. N. | Requires cookie* | | Title
| Struktur eines Spirobi(cyclophosphazens) [1] Structure of a Spirobi(cyclophosphazene) [1] Ph2p" *PPh2 N N0 N N I II Ph2P^ PPh2 Ph,P^ x PPh, 11 | 2 N^ ^NH N^N  | | | Abstract
| Proton addition to the spirobi(cyclotriphosphazene) anion 1 gives the neutral species 2. An X-ray structure determination shows the proton to be located at a nitrogen atom next to the spirocenter. The structural consequences of this protonation can be demonstrated by comparisons of intramolecular bond distances and angles and can be understood in terms of structure-determining repulsive N/N interactions in the central PN4 unit. Die alternierende Verknüpfung von tetrakoordi-niertem Phosphoniumphosphor und zweifach ko-ordiniertem Amidstickstoff _p® -N-führt mit m = n—1 zu kationischen offenkettigen, mit m = n zu neutralen monocyclischen und mit m = n -f 1 zu anionischen bicyclischen Phosphage-nen [2]. Die beiden erstgenannten Fälle sind mit n^ 2 bzw. n ^ 3 zahlreich verwirklicht, für den dritten Fall ist das Spirophosphazen-Anion 1 mit n = 5 das bislang einzige Beispiel [2], Protonierung bzw. Methylierung überführen 1 in die Neutral-verbindungen 2 und 3. Für 3 zeigt das 31 P-NMR-Spektrum, daß die Methylgruppe an einen dem Spirozentrum benachbarten Stickstoff gebunden ist. Dagegen läßt sich die Stellung des Protons in 2 wegen seiner Beweglichkeit in Lösung nicht in glei-cher Weise bestimmen [3]. Die angegebene Stellung ist jedoch aufgrund einer Abschätzung der Basizi-tätsverteilung und in Analogie zu 3 wahrscheinlich [2], Sie wird jetzt durch die Strukturbestimmung bestätigt und anhand der Strukturdiskussion auch plausibel. Cyclotriphosphazenringe [4] stellen ziemlich regel-mäßige Sechsecke dar. Sie weichen allgemein nur geringfügig von der Planarität ab, und die Summe Ph,P^ ^pph 2 3 der Innenwinkel beträgt fast oder genau 720°. Die Winkel am Stickstoff sind dabei etwas größer, die am Phosphor etwas kleiner als 120°. So wurden bei dem für einen Vergleich mit 2 am besten geeigneten (Ph2PN)3 122,1 bzw. 117,8° (Summe 719,7°) gefun-den. Der große Innenwinkel bedeutet eine erhebliche Verzerrung der tetraedrischen Phosphorkoordina-tion. Ihm muß ein entsprechend verengter Winkel zwischen den exocyclischen Substituenten gegen-übertreten. Er liegt allgemein bei 100°, bei (Ph2PN)3 beträgt er 103,8°. In 2 stehen nun am Spirozentrum einander zwei endocyclische NPN-Winkel gegen-über, und es stellt sich die Frage nach den struk-turellen Konsequenzen dieser Situation. Strukturbestimmung Die zur Strukturbestimmung verwendeten Kri-stalle von 2 wurden aus Acetonitril gewonnen und enthalten je Molekül 2 ein Lösungsmittelmolekül. Zellkonstanten und Intensitäten wurden auf einem P3-Diffraktometer bestimmt (A-MoKa = 71,069 pm, 912 A. Schmidpeter et al. • Struktur eines Spirobi(cyclophosphazens) Graphit-Monochromator, T = 200 K, co-scan, Aco = | | |
Reference
| Z. Naturforsch. 34b, 911—914 (1979); eingegangen am 2. März 1979 | | |
Published
| 1979 | | |
Keywords
| Spirocyclic Phosphazene, Basicity Distribution, Coulombic Repulsion of Adjacent N, X-ray | | |
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| default:Reihe_B/34/ZNB-1979-34b-0911.pdf | | | Identifier
| ZNB-1979-34b-0911 | | | Volume
| 34 | |
13 | Author
| Ekkehard Lindner, Sadek Trad, Sigurd Hoehne, Hans-Henning Oetjen | Requires cookie* | | Title
| Präparative, spektroskopische und kristallographische Untersuchungen an Phosphinato-Komplexen des Rheniums mit verschiedenen einzähnigen Liganden Preparative, Spectroscopic and Crystallographic Investigations on Phosphinato Complexes of Rhenium with Various Unidentate Ligands  | | | Abstract
| The stable phosphinato complexes [^-R2P02Re(C0)3L]" (1, 2b-f) [L = THF (a), py (b), NH3 (c), P(C6H5)3 (d), AS(C6H5)3 (e), P(C6Hn)3 (f), 0(C2H5)2 (g)] are obtained by addition of the ligands L to the compounds 0-R2P02Re(C0)3]M (1, 2) [R = CH3 (1), C6H5 (2)] at 20-40 °C (1, 2c: —35 °C). 1, 2b, d, e are also formed when THF in 1, 2a is substituted by the ligands b, d, and e. The unstable ether adducts 1, 2g which result photochemically from Re2(CO)io and the acids R2P02H, are transformed to 1, 2 by elimination of ether. At 20 °C 1, 2 a react with liquid ammonia to give the ionic complexes [(0C)3Re(NH3)3][02PR2] (1, 2h). On the basis of their mass and vibrational spectra, and a crystallographic in-vestigation, the methyl [la-f] and phenyl compounds [2 a-f] are dimeric and oligomeric, respectively. The rhenium atoms are bridged via R2P02~ ligands (phosphinato-0,0'). la crystallizes monoclinic in the space group C2/m with Z = 2. Stabile, monomere Chelatkomplexe des Mangans und Rheniums mit zweizähnigen Carboxylat-oder Phosphinat-Liganden des Typs RCE2M(CO)3L bzw. | | |
Reference
| Z. Naturforsch. 34b, 1203—1212 (1979); eingegangen am 28. Mai 1979 | | |
Published
| 1979 | | |
Keywords
| Phosphinato Complexes, Rhenium(I), MS, IR, Raman, X-Ray | | |
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| default:Reihe_B/34/ZNB-1979-34b-1203.pdf | | | Identifier
| ZNB-1979-34b-1203 | | | Volume
| 34 | |
14 | Author
| Josef Ernst, WilliamS. Sheldrick, Jürgen-Hinrich Fuhrhop | Requires cookie* | | Title
| Die Strukturen der essentiellen ungesättigten Fettsäuren, Kristallstruktur der Linolsäure sowie Hinweise auf die Kristallstrukturen der a-Linolensäure und der Arachidonsäure The Structures of the Essential Unsaturated Fatty Acids. Crystal Structure of Linoleic Acid and Evidence for the Crystal Structures of a-Linolenic Acid and Arachidonic Acid  | | | Abstract
| The essential fatty acids linoleic, a-linolenic and arachidonic acid have been crystallized for the first time. The crystal and molecular structures have been elucidated by X-ray analysis. Linoleic acid crystallizes monoclinic P2ijc with a = 4298(3), b — 463.2(3), c = 937.7(6) pm, ß = 109.38(8)°, Z = 4. The closely packed molecules are stretched with a ttttttsCssCstt conformation a . By comparison of the unit-cell constants and calculated densities of the unsaturated fatty acids it may be shown that both a-linolenic acid and arachidonic acid also possess stretched structures in the crystal lattice, a-linolenic acid must display a ttttttsCssCssCs and arachidonic acid a ttsCssCssCssCsttt conformation. Einleitung | | |
Reference
| Z. Naturforsch. 34b, 706—711 (1979); eingegangen am 15. Januar 1979 | | |
Published
| 1979 | | |
Keywords
| Linoleic Acid, a-Linolenic Acid, Arachidonic Acid, Stretched Molecular Geometries, X-ray | | |
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| default:Reihe_B/34/ZNB-1979-34b-0706.pdf | | | Identifier
| ZNB-1979-34b-0706 | | | Volume
| 34 | |
17 | Author
| Borislav Bogdanović, Richard Goddard, Peter Göttsch, Carl Krüger, Klaus Schlichte, Yi-Hung Tsay | Requires cookie* | | Title
| 7) 3 -Allylmetall-Schwefel-Cluster des Nickels, Palladiums und Platins r/ 3 -Allyl Metal Sulfur Cluster Compounds of Nickel, Palladium, and Platinum  | | |
Reference
| Z. Naturforsch. 34b, 609—613 (1979); eingegangen am 14. Dezember 1978 | | |
Published
| 1979 | | |
Keywords
| Trigonal Prismatic Metal Sulfur Cluster, -Allyl Compounds of Ni, Pt, Pd, l, 6, 6a-Trithiapentalene, X-ray | | |
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| default:Reihe_B/34/ZNB-1979-34b-0609.pdf | | | Identifier
| ZNB-1979-34b-0609 | | | Volume
| 34 | |
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