| | 2 | Author
| W. Stoeger, A. Rabenau | Requires cookie* | | | Title
| Tl6Ag2Iio9 ein Polyiodid mit Ag2-Paaren Darstellung, Eigenschaften und Kristallstruktur Tl6Ag2Iio, a Polyiodide with Ag2 Pairs Preparation, Properties, and Crystal Structure  | | | | Abstract
| TleAg2Iio forms hexagonal crystals with metallic luster. Under its own I2-pressure the m.p. is 302 °C. In vacuum or under inert gas TleAg2Iio decomposes above 170 °C forming 1 mole of I2. The space group is P62c with the lattice constants a = 10.480 A, c = 13.415 A and Z = 2. TleAg2Iio is built up by a framework of TIöIö with channels parallel to the c-axis. These channels contain Ag2 pairs with an Ag-Ag distance of 2.98 A and I| _ -polyiodide ions, respectively. | | | |
Reference
| Z. Naturforsch. 33b, 740—744 (1978); eingegangen am 21. April 1978 | | | |
Published
| 1978 | | | |
Keywords
| X-ray, Structure Determination, Polyhalides | | | |
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| default:Reihe_B/33/ZNB-1978-33b-0740.pdf | | | | Identifier
| ZNB-1978-33b-0740 | | | | Volume
| 33 | |
| 3 | Author
| G. Struckmeier, J. Engel, U. Thewalt | Requires cookie* | | | Title
| Molekül-und Kristallstruktur des 5.5' -Diethoxycarbonyl-3.3' -diethyl-4.4' -dimethyl-pyrromethen-hydrobromids Crystal and Molecular Structure of 5,5'-Diethoxycarbonyl-3,3'-chethyl-4,4'-cÜmethyl-pyiTomethene Hydrobromide | | | | Abstract
| The crystal and molecular structure of the title compound has been determined by X-ray diffraction. The compound possesses an (almost) planar Z configuration. The ions form ion pairs in the solid state: each bromide anion is connected via two hydrogen bonds with a cation. The crystal data are: space group P2i/n with Z = 4; cell dimensions a = 14.097(2), b = 11.591(2), c = 14.133(3) A, ß = 106,22(2)°. | | | |
Reference
| Z. Naturforsch. 33b, 753—755 (1978); eingegangen am 12. April 1978 | | | |
Published
| 1978 | | | |
Keywords
| Pyrromethenes, X-ray, Molecular Structure | | | |
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| default:Reihe_B/33/ZNB-1978-33b-0753.pdf | | | | Identifier
| ZNB-1978-33b-0753 | | | | Volume
| 33 | |
| 4 | Author
| Dieter Weber | Requires cookie* | | | Title
| CHsNHsSnBraJa-z = 0-3), a Sn(II)-System with Cubic Perovskite Structure | | | | Abstract
| CH3NH3SnBr^l3 -.x [x = 0—3) has the cubic perovskite structure with the unit cell parameters a = 5.89 A {x = 3), a = 6.01 A (x = 2) and a = 6.24 A (x = 0) and Z = 1. The compounds show intense colour and conducting property. The U9 Sn Mössbauer data are consistent with the high symmetry environment of the Sn(II)-ion. A bonding model, using a "p-resonance-bonding", can explain the properties of the cubic system. The synthesis is described. | | | |
Reference
| Z. Naturforsch. 33b, 862—865 (1978); eingegangen am 5. Mai 1978 | | | |
Published
| 1978 | | | |
Keywords
| Synthesis, X-ray, Mössbauer Spectra | | | |
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| default:Reihe_B/33/ZNB-1978-33b-0862.pdf | | | | Identifier
| ZNB-1978-33b-0862 | | | | Volume
| 33 | |
| 5 | 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 | |
| 7 | 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 | |
| 8 | 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 | |
| 9 | 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 | |
| 12 | 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 | |
| 14 | Author
| Markus Wieber, Christian Burschka, Ulrich Baudis | Requires cookie* | | | Title
| Darstellung und Molekülstruktur von 2-Methylthio-l,3,2-benzodithiastibol Preparation and X-ray Structure of 2-Methylthio-l,3,2-benzodithiastibole | | | | Abstract
| Starting with SbCl3 and 1,2-benzenedithiol, one can easily obtain heterocyclic 2-chloro-1,3,2-benzodithiastibole [1], which, without iso-lation, can be treated with a solution of sodium methanethiolate to yield 2-methylthio-1,3,2-benzodithiastibole. Yellow crystals were obtain-ed by recrystallization from acetonitrile. The compound was found to be monomeric in ben-zene solution. The crystal structure was solved by means of X-ray diffraction methods and could be refined to an .R-value of 0.03 with 870 independent reflections observed. The monoclinic unit cell contains 4 formula units, the space group is P2i/c. The structure can be compared with that of 2-methoxi-l,3,2-benzodioxastibole, a prelimi-nary report of which has been given [2]. The compounds are, however, not isomorphous. Interactions between neighbouring molecules in the thiastibole seem to be significantly weaker than in the corresponding oxygen compound. Verbindungen des Typs R-M<^j^>R', M = P, As, | | | |
Reference
| Z. Naturforsch. 33b, 1051—1052 (1978); eingegangen am 2. Juni 1978 | | | |
Published
| 1978 | | | |
Keywords
| 2-Methylthio -1, 3, 2 -benzodithiastibole, Preparation, X-ray | | | |
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| default:Reihe_B/33/ZNB-1978-33b-1051_n.pdf | | | | Identifier
| ZNB-1978-33b-1051_n | | | | Volume
| 33 | |
| 16 | Author
| W. S. Sheldrick, J. A. Gibson, G.-V Röschenthaler | Requires cookie* | | | Title
| The Crystal Molecular Structure of the Adduct of 2,2,2-Trifluoro-4,4,5,5-tetrakis(trifluoromethyl)-l,3,2A 5 -dioxaphospholane with Trimethylphosphine. A Strong P —» P Coordinate Bond | | | | Abstract
| The adduct of 2,2,2-trifluoro-4,4,5,5-tetrakis(trifluoromethyl)-1,3,2 A 5 -dioxaphospholane with trimethylphosphine crystallises in the orthorhombic space group Pbcm, Z = 4, with a — 11.018(2), b — 12.978(4), c= 11.607(2) A at —120 °C. The perfluoropinacolyl ring system lies in a crystallographic plane of symmetry. This ring conformation and the very long endocyclic C-C bond and average C-CF3 distances of respectively 1.59(1) and 1.59(1) A are presumably a consequence of very short F---F steric contacts. The P->P bond distance of 2.234(5) is very short for a coordinate bond being only 0.01-0.03 A longer than that typically observed for a a-bond. The tr-bond lengths to the hexacoordinate phosphorus are influenced by the nature of the Zrans-bond in the octahedron. | | | |
Reference
| Z. Naturforsch. 33b, 1102—1 (1978); eingegangen am 22. Juni 1978 | | | |
Published
| 1978 | | | |
Keywords
| X-ray, Hexacoordinate Phosphorus Adduct, Coordinate P-*P Distance Planar Perfluoropinacolyl Ring System, Long Endocyclic C-C Bond | | | |
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| default:Reihe_B/33/ZNB-1978-33b-1102.pdf | | | | Identifier
| ZNB-1978-33b-1102 | | | | Volume
| 33 | |
| 17 | Author
| M. Veith | Requires cookie* | | | Title
| Cyclische Diazastannylene, II 1 Intermolekulare Lewis-Säure-Base-Addukte bei 1.3.2.4A 2 -Diazasilastannetidinen Cyclic Diazastannylenes, II 1 Intermolecular Lewis-Acid-Base Adducts of 1, 3,2,4A 2 -Diazasilastannetidines | | | | Abstract
| -diazasilastannetidines can be prepared as mono-mers (organyl = <erf-butyl) or dimers (organyl = isopropyl) in nonpolar solvents, depending on the organic nitrogen substituent. The formation of the dimer, which is due to an intermolecular Lewis-acid-base interaction of Sn(II) with nitrogen, can be initiated by solidification. When the tertf-butyl compound is cooled below 0 °C two crystalline modi-fications are found: a monoclinic phase (C 2/c; a= 10.655(5); b = 24.75(1); c = 17.334(9) Ä; ß = 106.9(1)°) and a triclinic phase (P I; a = 10.68(1); b = 13.51(1); c = 12.36(1) A; a = 96.2(1); ß = 102.6(1); y = 118.4(1)°). The crystal structures turn out to be built of dimeric and monomeric units in the first case and presumably only dimeric species in the second case. The isopropyl derivative crystallizes in the space group P 2i/b (a = 10.77(1); b= 12.14(2); c = 11.15(2) A; ß = 120.2(2)°) with only dimeric units being present, as in the liquid. Interrelationships between the three structures are discussed. | | | |
Reference
| (Z. Naturforsch. 33b, 1—6 [1978]; eingegangen am 5. September/6. Oktober 1977) | | | |
Published
| 1978 | | | |
Keywords
| Diazastannylenes, Solid State, X-ray, Crystal Structure, NMR l, 3-Diorganyl-2, 2-dimethyl-I, 3, 2, 4A 2 | | | |
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| default:Reihe_B/33/ZNB-1978-33b-0001.pdf | | | | Identifier
| ZNB-1978-33b-0001 | | | | Volume
| 33 | |
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