| | 21 | Author
| Frank Borkenhagen, Ion Neda, H. Olger Thönnessen, PeterG. Jones, R. Einhard, Schm Utzler | Requires cookie* | | | Title
| Synthesis and Characterization o f 2-Substituted 5 Darstellung und Charakterisierung von 2-substituierten 5,6-Benzo-l-methyl  | | | | Abstract
| ,6 -B en zo -l-m eth y l-3 -R -l,3 ,2 -diazaphosphorin-4-ones (R = 2-M orpholinoethyl, 1-Adam antyl) C ontaining Phosphorus w ith Coordination N um bers T hree, Four and Five The reaction of N-methylisatoic anhydride with 2-morpholinoethylamine or 1-amino-adamantane furnished N-methyl-N'-(2-morpholinoethyl)anthranilamide 1 and N-methyl-N'-(l-adamantyl)anthranilamide 2, respectively. 1 and 2 are intermediates in the synthesis of the 2-chloro-3-methyl-1,3,2 A'-diazaphosphorinones 3 and 4 by reaction of 1 and 2 with PCI,. The reaction of 3 with bis(2-chloroethyl)amine hydrochloride/triethylamine or (2-chloroethyl)amine hydrochloride/triethylamine formed the 2-substituted diazaphosphorinones 5 and 6. Hydrolysis of 3 led to the 2-oxo-A4P-compound 7. The reaction of 6 with hexafluoroacetone furnished the (A5) phosphorane 8. 5 reacted with C7H8Cr(CO)4 to form complex 9 whereas oxidation of 5 with the H20 2: urea 1:1 adduct yielded the phosphoryl compound 10. The crystal structure of 1 displays two independent molecules that show different chain conformations. Both molecules form chains parallel to the y-axis by intermolecular N (am ide)-H -0(am ide) bonds. The crystal structure of 6 shows a half-boat conformation for the phosphorinone ring; the P atom lies out of the plane. Again the molecules are linked by H-bonds into chains parallel to the y-axis. | | | |
Reference
| Z. Naturforsch. 51b, 1627—1638 (1996); eingegangen am 14. März 1996 | | | |
Published
| 1996 | | | |
Keywords
| Diazaphosphorinones, Oxidative Addition, X-Ray | | | |
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| default:Reihe_B/51/ZNB-1996-51b-1627.pdf | | | | Identifier
| ZNB-1996-51b-1627 | | | | Volume
| 51 | |
| 22 | Author
| M. Onoheteroarylborates [, Norbert Kuhn3, Heike Kotowski3, Dieter Bläserb, Roland Boeseb | Requires cookie* | | | Title
| Monoheteroarylborate [1] | | | | Abstract
| The heteroaryl borates Li[C4Me4NBH3] (6) and Na[C3H 3N2(BMe3)2]* 2 C4HgO (8) are ob tained by treatment of Li[C4Me4N] and Na[C3H3N2] with Me2S • BH3 and BMe3, respectively. The X-ray structure of [Na(C4H 80) 6][C3H 3N 2(BM e3)2] (10) is reported. | | | |
Reference
| Z. Naturforsch. 52b, 351—354 (1997); eingegangen am 28. Oktober 1996 | | | |
Published
| 1997 | | | |
Keywords
| Borates, Pyrroles, Imidazoles, X-Ray | | | |
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| default:Reihe_B/52/ZNB-1997-52b-0351.pdf | | | | Identifier
| ZNB-1997-52b-0351 | | | | Volume
| 52 | |
| 23 | Author
| N. Orbert Kuhn, Riad Faw, M. Anfred, Steim Ann, JörgW. Iethoff, Herrn | Requires cookie* | | | Title
| Zur Reaktion von Derivaten des l,3-Dimethyl-2-iminoimidazolins mit CS2 [1] | | | | Abstract
| 1,3-Dimethyl-2-iminoimidazoline (4, ImNH) reacts with CS2 to give the imidazolium salt [ImNH2][(ImNCS2)2H] (7) in which two dithioformimide fragments are linked by a hydrogen bridge. From the trimethylsilyl derivative ImNSiMe3 (11) and CS2 the adduct ImNSiMe3 • CS2 (12) is obtained which reacts with oxygen to give the disulfide (ImNCS2) (14). The X-ray structures of 7 and 14 were determined. | | | |
Reference
| Z. Naturforsch. 52b, 609—614 (1997); eingegangen am 19. Februar 1997 | | | |
Published
| 1997 | | | |
Keywords
| Imidazoles, Carbon Disulfide, X-Ray | | | |
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| default:Reihe_B/52/ZNB-1997-52b-0609.pdf | | | | Identifier
| ZNB-1997-52b-0609 | | | | Volume
| 52 | |
| 28 | Author
| W. Muschick, Hk Müller-Buschbaum | Requires cookie* | | | Title
| Ein Beitrag zur Kristallchemie dreiwertiger Seltenerdoxide Zur Stabilisierung der m onoklinen B-Form | | | | Abstract
| Single crystals of 1 — a'Ho203 : xCaO (x = 0.07), CaHoC>2.5 (A) and Cao.5H 01.5O2.75 (B) were prepared by high temperature reaction and investigated with X-ray single crystal data. It can be shown that small amounts of CaO stabilize the monoclinic B-Typ of rare earth oxides. Phase (A) and (B) cannot be seen as a stabilized B-type crystal because they have an new crystal structure with space group C.7h-P 2 i/m, a = 656.6, b = 356.7, c = 529.4pm , ß = 92.3°; a = 650.2, b = 352.4, c = 584.5, ß = 92.3°. | | | |
Reference
| (Z. Naturforsch. 32b, 495—498 [1977]; eingegangen am 15. Februar 1977) | | | |
Published
| 1977 | | | |
Keywords
| Holmium, Thulium, Calcium, X-ray, Crystal Structure | | | |
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| default:Reihe_B/32/ZNB-1977-32b-0495.pdf | | | | Identifier
| ZNB-1977-32b-0495 | | | | Volume
| 32 | |
| 29 | Author
| Cyclic Diazastannylenes, Iii, M. Veith | Requires cookie* | | | Title
| Cyclische Diazastannylene, DI 1 Die Kristall-und Molekülstruktur der monoklinen Phase von 1.3-Di-feri-butyl-2.2-dimethyl-1.3.2.4A 2 -diazasilastannetidin The Crystal and Molecular Structure of the Monoclinic Phase of l,3-Di-feri-butyl-2,2-dimethyl-l,3,2,4A 2 -diazasilastannetidine | | | | Abstract
| The crystal and molecular structure of the monoclinic phase of l,3-di-£eri-butyl-2,2-dimethyl-l,3,2,4A 2 -diazasilastannetidine has been determined from three-dimensional X-ray data collected on a two-circle diffractometer at —120 °C (MoKa radiation, 2623 re-flexions, R — 0,050). The crystals are monoclinic, space group C 2/c, with cell dimensions a = 10.655(5), b = 25.75(1), c = 17.33(1) A, ß = 106.8(1)° and Z = 12. Four monomeric (crystal site symmetry 2 (C2)) and four dimeric units (crystal site symmetry I (Cj)) are present in the structure interacting over tin-tin (3.68 A). Remarkable are the very short Sn-N bond (2.09 A) in the monomer and the donation bond Sn-N (2.39 Ä) in the dimer. The coordination of the tin atoms in the different units is discussed in detail. | | | |
Reference
| (Z. Naturforsch. 33b, 7—13 [1978]; eingegangen am 5. September/6. Oktober 1977) | | | |
Published
| 1978 | | | |
Keywords
| Diazastannylenes, X-ray, Molecular Structure, Crystal Structure | | | |
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| default:Reihe_B/33/ZNB-1978-33b-0007.pdf | | | | Identifier
| ZNB-1978-33b-0007 | | | | Volume
| 33 | |
| 31 | Author
| Herbert Binder, Dieter Sellmann | Requires cookie* | | | Title
| Röntgen-photoelektronenspektroskopische Untersuchungen an Pentacarbonyl- Chrom-und -Wolfram-Komplexen mit Stickstoffliganden c X-ray Photoelectron Studies of Pentacarbonyl Chromium and Tungsten Complexes with Nitrogen Ligands | | | | Abstract
| The ionization energies of some chromium and tungsten pentacarbonyl complexes of the type [M(CO)5] xL (L = N2H2, N2H4, NH3; x = 1 or 2 for N2H4 or a; = 1 for N2H2) are reported. The results are discussed in terms of the effects of tr-donor and 7r-acceptor bonds on XPS data. Satellite lines, which can be explained in terms of a shake-up process, give information about the nature of the metal-ligand bond. These shake-up processes are, to a large extent, specific to the atoms of the acceptor groups. The spectroscopic and chemical importance of multi-peak structures of XPS bands is emphasised. | | | |
Reference
| Z. Naturforsch. 33b, 173—179 (1978); eingegangen am 21. Dezember 1977 | | | |
Published
| 1978 | | | |
Keywords
| X-ray, PE Spectra, Monosubstituted Pentacarbonyls, Chromium, Tungsten | | | |
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| default:Reihe_B/33/ZNB-1978-33b-0173.pdf | | | | Identifier
| ZNB-1978-33b-0173 | | | | Volume
| 33 | |
| 32 | Author
| HeinzP. Fritz, Helmut Gebauer, Peter Friedrich, Peter Ecker, Reinhold Artes, Ulrich Schubert | Requires cookie* | | | Title
| Elektrochemische Synthesen, XIV [1] Radikalkation-Salze des Naphthalins Electrochemical Syntheses, XIV [1]. Radical Cation Salts of Naphthalene | | | | Abstract
| By anodic oxidation of naphthalene in H2CCI2/O.O2 m Bu4NPF6 at —45 °C dark red-violet crystals of (CioHshPFö can be obtained by electrocrystallisation. They are stable at low temperatures, however, decompose on warming. In solution and in the poly-crystalline state these radical cation salts show only narrow e.p.r. signals without h.f.s. The specific conductivity of a polycrystalline pellet at room temperature was determined to be 0.12 ±0.046 Ohm -1 cm -1 . The structure determination of (CioHs^PFe yielded the tetragonal space group P42/n, Z = 2, a = b = 1156(2), c = 640(1) pm. Patterson synthesis and difference Fourier analyses showed the compound to have a columnar stacking of CioHg units the long molecular axes of which are twisted alternately by 90° around a screw axis in c-direction, and the molecular planes of which are 320 pm apart. The PFß -ions have four nearest CioHs neighbours lying in pairs in parallel planes 63 pm above and below that plane of PF6~ perpendicular to the c-axis and containing a PF4 group. This is the first established case for a columnar structure of a pure hydrocarbon radical cation. (CIOH8)2AsF6 is isomorphous. | | | |
Reference
| Z. Naturforsch. 33b, 498—506 (1978); eingegangen am 21. Februar 1978 | | | |
Published
| 1978 | | | |
Keywords
| Naphthalene Radical Cation, X-ray, Columnar Structure, Conductivity | | | |
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| default:Reihe_B/33/ZNB-1978-33b-0498.pdf | | | | Identifier
| ZNB-1978-33b-0498 | | | | Volume
| 33 | |
| 33 | Author
| Tetraphenylphosphonium-Isopolymolybdates, Roger Grase, Joachim Fuchs | Requires cookie* | | | Title
| Über Tetraphenylphosphonium-Isopolymolybdate | | | | Abstract
| From acidified sodium molybdate solutions mixtures of two polymolybdates are precipitated by addition of tetraphenylphosphonium ions. The pure compounds obtainable by separation with selective organic solvents were identified analytically and by their vibrational spectra as octamolybdate, [P(C6Hs)4]4Mo8026, with "Lindqvist structure" and as hexamolybdate, [P(C6Hs)4Mo60i9. They are characterized by their UV-VIS spectra and X-ray powder patterns. The precipitation of the hexamolybdate from strong acidic solution can be used analytically for the determination of molybdenum. | | | |
Reference
| Z. Naturforsch. 33b, 533—536 (1978); eingegangen am 20. Januar 1978 | | | |
Published
| 1978 | | | |
Keywords
| Isopolymolybdates, Preparation, Vibrational Spectra, X-ray, UV | | | |
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| default:Reihe_B/33/ZNB-1978-33b-0533.pdf | | | | Identifier
| ZNB-1978-33b-0533 | | | | Volume
| 33 | |
| 36 | Author
| R. Hansel, J. Schulz, A. Pelter, M. T. Ayoub, R. Reinhardt | Requires cookie* | | | Title
| Über das Verhalten von 5-Hydroxy-Kawainen gegen Alkali Behaviour of 5-Hydroxykawain Derivatives under Mild Alkaline Conditions | | | | Abstract
| Treatment of cis-dihydroxykawainol = rel (5R, 6R)-(±)-5-hydroxy-4-methoxy-6-phenylethyl-5,6-dihydro-2H-pyran-2-on (eis-3) with potassium hydroxide in methanol (2.5%, 1 h, room temp.) leads to a 1:1 mixture of the corresponding erythro-butenolide 7 and threo-butenolide 8 by a ring contraction process that may have analogies with the biosynthesis of the piperolides 15. Trans-3 gives the same yields (about 70%) of the same mixture (7 and S), which can be separated by silica-gel columns. Starting from mixtures of cis-5-hydroxykawain (C?Ö'-4) and Zrans-5-hydroxykawain (trans-4), there were prepared and described the two epimeric dehydro-butenolides 9 and 10 and their O-methyl-derivatives 11 and 12. The threo-and erythro-series show consistant differences between ,75,6 and the X H NMR spectra. The constitution and configuration of (±)-erythro-5-(l-methoxy-3-phenylallyl)-4-methoxy-2(5H)-furanone (11) were established by X-ray analysis. | | | |
Reference
| Z. Naturforsch. 33b, 1020—1025 (1978); eingegangen am 5. Juni 1978 | | | |
Published
| 1978 | | | |
Keywords
| 5-Hydroxykawain Derivatives, Erythrobutenolides, Threobutenolides, X-ray, Piperolides | | | |
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| default:Reihe_B/33/ZNB-1978-33b-1020.pdf | | | | Identifier
| ZNB-1978-33b-1020 | | | | Volume
| 33 | |
| 38 | 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 | |
| 39 | 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 | |
| 40 | 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 | |
|
