| | 2 | Author
| Karl-Friedrich Tebbe, Roland Fröhlich | Requires cookie* | | | Title
| Beiträge zur Strukturchemie phosphorhaltiger Ketten und Ringe, V [1]  | | | | Abstract
| Die Molekül-und Kristallstruktur des 1.2.3.4-Tetra-ferf-butyl-1.4-bis(trimethylsilyl)tetraphosphans, Me3Si-(«-BuP)4-SiMe3 Structural Chemistry of Phosphorus-Containing Chains and Rings, V [1] Molecular and Crystal Structure of 1,2,3,4-Tetra-ferf-butyl-1,4-bis(trimethylsilyl)tetraphosphane, (H3C)3Si-(f-BuP)4-Si(CH3)3 The compound l,2,3,4-tetra-£er£-butyl-l,4-bis(trimethylsilyl)tetraphosphane, Me3Si-(£-BuP)4-SiMe3, C22H54P4Si2, crystallizes monoclinically in the space group P2i/n (No. 14) with a = 889.9 pm, b = 2292.8 pm, c = 1568.0 pm, ß = 94.14° and Z = 4 formula units. The molecule forms a twisted Si-P4-Si-chain with two kinds of P-P-bonds. The atoms neighbouring the silicium atoms take part in bonds of length d(P-P) = 218.8 pm, whereas the central bond d(P-P) = 221.4 pm is much longer. A special feature of the structure is a short contact d(P-P) = 345.6 pm. Therefore, the inner region of the molecule has the shape of a nearly planar trapezium of the four phosphorus atoms. The periphery of the molecule is as expected. The average bond lengths are d(P-Si) = 228.5 pm, H(P-C) — 190.2 pm, d(Si-C) = 186.6 pm, d(C-C) = 151.8 pm and d(C-H) = 94 pm. | | | |
Reference
| Z. Naturforsch. 37b, 534—541 (1982); eingegangen am 23. Dezember 1981 | | | |
Published
| 1982 | | | |
Keywords
| Tetraphosphane, Phosphorus Chain, Crystal Structure | | | |
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| default:Reihe_B/37/ZNB-1982-37b-0534.pdf | | | | Identifier
| ZNB-1982-37b-0534 | | | | Volume
| 37 | |
| 3 | Author
| M. Pušelj, Z. Ban, A. Drašner | Requires cookie* | | | Title
| On the Crystal Structure of HgZn3 | | | | Abstract
| The crystal structure of the intermetallic phase HgZn3 was determined using X-ray single crystal and powder diffraction methods. The phase belongs to the orthorhombic system, most probable space group being Cmc2i, and appears to be isostructural with /S'-Cu3Ti. Under standard preparative conditions a statistical distribution of both atomic species was observed. | | | |
Reference
| Z. Naturforsch. 37b, 557—559 (1982); received December 14 1981 | | | |
Published
| 1982 | | | |
Keywords
| Crystal Structure, Zinc, Mercury, Amalgam | | | |
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| default:Reihe_B/37/ZNB-1982-37b-0557.pdf | | | | Identifier
| ZNB-1982-37b-0557 | | | | Volume
| 37 | |
| 5 | Author
| Helmut Endres, Nasser Kadkhodai-Elyaderani | Requires cookie* | | | Title
| Malonenamidoxim, Nickelkomplexe und deren ßeaktionsprodukte mit Sauerstoff und Kohlendioxid: Vergleichende Strukturuntersuchungen Malonenamide Oxime, Nickel Complexes, and their Reaction Products with Oxygen and Carbon Dioxide: Comparative Structural Studies | | | | Abstract
| Malonenamide oxime [HONC(NH2)CH2C(NH2)NOH = C3H8N402] (1), its bis-chelate complex with Ni(II) [Ni(C3HyN402)2] (2) and an ethanol solvate of this complex [Ni(C3H7N402)2 • 0.6 C2H5OH] (3) are characterized by X-ray structure analysis, as well as a paramagnetic tris-complex [Ni(C3H7N402)2(C3HsN402)] (4), which forms a catena structure in the crystal. The molecular structures of two reaction products of 2 with air are described: [Ni(C3H5N403)2(H20)2] • 4 H20 (5) has formed by oxidation of the methylene groups and may be taken as a complex of mesoxalamide oxime; [NiCsHieNsOs] • 6 H20 (6) has a macrocyclic ligand which is a derivative of orthocarbonic acid, formed by addition of carbon dioxide to the oxime groups. | | | |
Reference
| Z. Naturforsch. 37b, 1255—1265 (1982); eingegangen am 25. Mai 1982 | | | |
Published
| 1982 | | | |
Keywords
| a, y-Diondioxime Complexes, Crystal Structure | | | |
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| default:Reihe_B/37/ZNB-1982-37b-1255.pdf | | | | Identifier
| ZNB-1982-37b-1255 | | | | Volume
| 37 | |
| 6 | Author
| Peter Pullmann, Karl Hensen, JanW. Bats | Requires cookie* | | | Title
| Röntgenstrukturbestimmung von A1C13-Pyridin-Addukten: Der strukturelle Aufbau im fra7is-Dichlorotetrakis(pyridin)aluminium(III)- Tetrachloroaluminat(III) und im Trichlorotris(pyridin)aluminium(III) X-ray Diffraction Study of AICI3-Pyridine Adducts: The Crystal Structure of 7ra/?s-Dichlorotetrakis(pyridine)aluminium(III)tetrachloroaluminat(III) and of Trichlorotris(pyridine)aluminium(III) | | | | Abstract
| Crystals of [A1(C5H5N)4C12][A1C14] are orthorhombic, Pna2lf Z = 4, a = 18.522(7), b = 15.141(5), c = 9.593(3) A, V = 2690(2) A 3 , Dc = 1.440 g/cm 3 . The structure has been solved from 5968 diffractometer measured intensities and refined by full-matrix least squares to RW(F) = 0.032. The crystal structure shows the complex to be £ra»s-dichloro-tetrakis(pyridine)aluminium(III) tetrachloroaluminat(III). The mean trans Al-Cl-and trans Al-N-distances in the octahedron are 2.279(3) and 2.070(4) A, respectively. Crystals of Al(C5H5N)3Cl3 are monoclinic, P2i/c, Z = 4, a = 7.261(2), b = 29.961(4), c = 8.624(1) A, ß = 98.12(2)°, V -1857(1) A 3 , D0 = 1.326 g/cm 3 . The structure has been solved from 4707 diffractometer measured intensities and refined to RW(F) = 0.028. The crystal structure shows octahedral complexes AICI3 • 3 (C5H5N) with trans geometry. The Al-N-distance trans to chlorine (2.096(2) A) is significantly longer than the two other Al-N-distances (mean 2.072(2) A). | | | |
Reference
| Z. Naturforsch. 37b, 1312—1315 (1982); eingegangen am 5. Mai 1982 | | | |
Published
| 1982 | | | |
Keywords
| Aluminium Chloride, Pyridine, Crystal Structure | | | |
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| default:Reihe_B/37/ZNB-1982-37b-1312.pdf | | | | Identifier
| ZNB-1982-37b-1312 | | | | Volume
| 37 | |
| 7 | Author
| Bernt Krebs, Andreas Schäffer, Marita Hucke | Requires cookie* | | | Title
| Oxotrihalogenoselenate(IV) | | | | Abstract
| Darstellung, Struktur und Eigenschaften von P(C6H5)4SeOCl3, P(C6H5)4SeOBr3 und As(C6H5)4SeOBr3 Oxotrihalogenoselenates(IV): Preparation, Structure and Properties of P(C6H5)4SeOCl3, P(C6H5)4SeOBr3 and As(C6H5)4SeOBr3 The novel oxotribromosolenate(IV) SeOBr3~ anion was prepared from the reaction of stoichiometric quantities of SeOBi'2 and bromide in acetonitrile solution, and it was isolated as the tetraphenylphosphonium and -arsonium salts in crystalline form. For the synthesis of the analogous SeOCl3 _ as P(C'6H5)4SeOCl3, SeCl4 was reacted in the presence of a small quantity of H«() with P(CeH5)4Cl in acetonitrile. Complete N-ray structural analyses of P(C6H5)4SeOCi3 (space group P I, a = 10.981(3), b = 11.059(3), c = 10.358(3) A, a = 73.77(2)°, ß = 83.33(2)°, -/ = 80.51(2)°, V -1187.9(6) A 3) and of P(C6H5)4SeOBr3 (space group P 2i/c, a = 11.719(4), b = 16.088(4), c = 13.124(4) A, ß = 94.72(3)°, V = 2466(1) A 3) show dimeric centrosymmetric Se202Cl6 2-and Se202Br6 2 -anions being present in the solid. In the anions two square-pyramidal (y-octahedral) SeOHal4 groups are connected through a common Hal-Hal edge. The axial oxygen ligands (Se-O: 1.597(4) and 1.584(6) A) cause a pronounced stereochemical iraws-activation of the inert pairs at the Se atoms. As(C6H5)4So()Br3 is isotypic with P(C6H5)4SeOCl3. | | | |
Reference
| Z. Naturforsch. 37b, 1410—1417 (1982); eingegangen am 13. Mai 1982 | | | |
Published
| 1982 | | | |
Keywords
| Oxohalogenoselenate, Crystal Structure, Selenium | | | |
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| default:Reihe_B/37/ZNB-1982-37b-1410.pdf | | | | Identifier
| ZNB-1982-37b-1410 | | | | Volume
| 37 | |
| 8 | Author
| Ursula Frank-Cordier, Gerhard Cordier, Herbert Schäfer | Requires cookie* | | | Title
| Die Struktur des Na7Ga13-I und ein Konzept zur bindungsmäßigen Deutung The Structure of NavGai3-I and its Characterization by a Bonding Scheme | | | | Abstract
| The new compound NayGa^-I crystallizes in the trigonal-rhombohedral system, space group R 3 m, with the constants a = 1496.5(3) pm, c = 3893(1) pm, c/o = 2.60. The Ga atoms form Gai2 icosahedra and Gais clusters, connected to a threedimensional net. The arrangement of these clusters is related to the MgCu2 structure. The Na content of this compound correlates with the number of electrons necessary for a stable electron configuration in the Ga partial structure. The BaAl4 type structure of NaGa4 has been confirmed by single crystal data. | | | |
Reference
| (Z. Naturforsch. 37b, 119—126 [1982]; eingegangen am 5. Oktober 1981) | | | |
Published
| 1982 | | | |
Keywords
| Natrium Gallides, Crystal Structure, Bonding Scheme | | | |
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| default:Reihe_B/37/ZNB-1982-37b-0119.pdf | | | | Identifier
| ZNB-1982-37b-0119 | | | | Volume
| 37 | |
| 10 | Author
| Doris Bodenstein, Axel Brehm, PeterG. Jones, Einhard Schwarzmann, GeorgeM. Sheldrick | Requires cookie* | | | Title
| Darstellung und Kristallstruktur vom Arsen(III)arsen(V)oxidhydroxid As305(0H) Preparation and Crystal Structure of the Arsenic(III) Arsenic(V) Oxide Hydroxide As305(0H) | | | | Abstract
| The title compound was prepared by heating the hydrolysis products of AS2O4 in a sealed tube. The crystal structure was determined and refined to R = 0.058 [P2j./c, a = 1250.4(6), b = 459.3(2), c = 1097.6(6) pm, ß = 118.08(5)°, Z = 4]. The structure consists of infinite layers, containing pyramidal As(III)03 and tetrahedral As(V)04 groups, and stabilised by hydrogen bonding. | | | |
Reference
| Z. Naturforsch. 37b, 138—140 (1982); eingegangen am 7. Oktober 1981 | | | |
Published
| 1982 | | | |
Keywords
| Sealed-Tube Synthesis, Crystal Structure, Arsenic, Oxide | | | |
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| default:Reihe_B/37/ZNB-1982-37b-0138.pdf | | | | Identifier
| ZNB-1982-37b-0138 | | | | Volume
| 37 | |
| 12 | Author
| William Clegg, Uwe Klingebiel, GeorgeM. Sheldrick | Requires cookie* | | | Title
| Cyclisierungsreaktionen lithiierter Fluorsilanole und Aminofluorsiloxane - Kreuzdimerisierung eines Silicenium-Ylids Cyclisation Reactions of Lithiated Fluorosilanols and Aminofluorosiloxanes - Cross-dimerisation of a Silicenium-Ylid | | | | Abstract
| KOH reacts with bis(isopropyl-trimethylsilyl)-amino-difluorosilane to give the fluoro-silanol 1. An aminofluorosiloxane 2 is obtained in the reaction of [(Me3Si)2N]2SiF2 with KOH via a 1,3-silyl-group migration. The four-membered SiOSiN ring 5 can be prepared in several steps from 1. Six-membered SiO rings 8-10 are formed in the reaction of 1,3-fluorosilanols 6 and 7 with butyllithium. Lithiated 2 reacts with PCI3 to give a four-membered P2N2 ring 11, and with 2-methyl-2-propenal to give two isomeric (2 + 4) cycloadducts 12 and 13. The silicenium ylid formed initially by thermal elimation of LiF from lithiated 2 in PE/THF cross-dimerises to give a Si2N2 ring 14. If the reaction is carried out in n-heptane, the product after recrystallisation from acetone, 16, is an isomer of 14. The crystal structures of 14 and 16 have been determined. | | | |
Reference
| Z. Naturforsch. 37b, 423—431 (1982); eingegangen am 14. Dezember 1981 | | | |
Published
| 1982 | | | |
Keywords
| Fluorosüanols, Aminofluorosiloxanes, Cyclisation, Cross-dimerisation, Crystal Structure | | | |
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| default:Reihe_B/37/ZNB-1982-37b-0423.pdf | | | | Identifier
| ZNB-1982-37b-0423 | | | | Volume
| 37 | |
| 14 | Author
| PeterG. Jones | Requires cookie* | | | Title
| | | | | Abstract
| The crystal structure of (OC)AuCl has been determined and refined to R 0.037 (space group Cmem, a = 407.1(1), b = 1042.2(4), c —532.1(3) pm, Z =4). The structure consists of discrete, exactly linear molecules; all atoms lie on the special positions 0, y, 1/4. The bond lengths involving the light atoms are affected by libration. The shortest Au — Au contacts between molecules are 338 pm. | | | |
Reference
| Z. Naturforsch. 37b, 823—824 (1982); received March 8 1982 | | | |
Published
| 1982 | | | |
Keywords
| Crystal Structure, Carbonyl, Gold(I) | | | |
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| default:Reihe_B/37/ZNB-1982-37b-0823.pdf | | | | Identifier
| ZNB-1982-37b-0823 | | | | Volume
| 37 | |
| 15 | Author
| HeinzW. Rotter, Gerhard Thiele | Requires cookie* | | | Title
| Fehlordnung von Kationen und Kristallwasser bei kubischen Alkalitetrabromo-und -iodothallaten(III) Disorder of Cations and Water Molecules in Cubic Tetrabromo-and -iodothallates | | | | Abstract
| Tetrabromo-and -iodothallates(III) of the alkali cations crystallise from aqueous solutions as cubic hydrates MTlX4-nH20 (M = Li, Na, K, Rb, Cs, NH4; X — Br, I; n — 1-2). The tetraiodothallates retain their cubic structure on dehydratisation, while the tetrabromothallates undergo structural changes. The X-ray structure analyses of RbTlBr4 • H20, NH4TlBr4 • 2HoO and KTlBr4 • 2H20 (—50 °C) showed that these com-pounds consist of a three-dimensional framework of TlBr4 tetrahedra and MBrjo ikosahedra which reminds of zeolites. In cavities of this framework 2/3 of the alkali cations and the crystal water molecules are accommodated in a disordered manner. | | | |
Reference
| Z. Naturforsch. 37b, 995—1004 (1982); eingegangen am 3. März 1982 | | | |
Published
| 1982 | | | |
Keywords
| Thallium, Tetrabromothallate, Disorder, Tetraiodothallate, Crystal Structure | | | |
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| default:Reihe_B/37/ZNB-1982-37b-0995.pdf | | | | Identifier
| ZNB-1982-37b-0995 | | | | Volume
| 37 | |
| 16 | Author
| Ulrich Müller, ChristinaNorbert Mronga, Kurt Schumacher, Dehnicke | Requires cookie* | | | Title
| Die Kristallstrukturen von PPh4[SnCl3] und PPh4[SnBr3] The Crystal Structures of PPh4[SnCl3] and PPh4[SnBr3] | | | | Abstract
| PPh4[SnCl3] and PPh4[SnBr3] were prepared by reaction of PPh4X with SnX2 in CH2X2 solutions (X — Cl, Br). The vibrational spectra of the [SnX3] e ions show three SnX3 stretching frequencies, which is caused by deviations from the ideal C3v symmetry. In the crystal structure determinations these deviations show up by slightly different Sn-X bond lengths which are explained by differing hydrogen bridges to phenyl-H atoms. The isotypic crystal structures of both compounds were determined and refined from X-ray diffraction data (R values: 0.042 and 0.034). Although triclinic (space group Pi), the structures are closely related to the tetragonal AsPh4[RuNCl4] structure type. Very pure SnBr2 is prepared by the reaction of PPh4[SnBr3] with AlBr3 in CH2Br2 solution. | | | |
Reference
| Z. Naturforsch. 37b, 1122—1126 (1982); eingegangen am 19. Mai 1982 | | | |
Published
| 1982 | | | |
Keywords
| Preparation, Tetraphenylphosphonium Trihalo Stannates, Vibrational Spectra, Crystal Structures | | | |
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| default:Reihe_B/37/ZNB-1982-37b-1122.pdf | | | | Identifier
| ZNB-1982-37b-1122 | | | | Volume
| 37 | |
| 17 | Author
| Brigitte Eisenmann, Hanna Jordan, Herbert Schäfer | Requires cookie* | | | Title
| Neuartige Ge2P4 8 ~-bzw. Ge2As4 8 -Anionen in Ba2GeP2 und Ba2GeAs2 New Ge2P4 8 ~ and Ge2As4 8_ Anions in Ba^GeP? and Ba 2 GeAs2 | | | | Abstract
| The new compounds Ba2GeP2 and Ba2GeAs2 crystallize in the monoclinic system (space group P2i/c) with lattice constants: Ba2GeP2: a = 855.3 ± 0.5 pm, b = 951.5 ± 0.5 pm, c = 748.1 ± 0.5 pm, ß = 105.95 ± 0.08°. Ba2GeAso: a = 875.7 ± 0.5 pm, b = 970.0 ± 0.5 pm, c = 700.7 ± 0.5 pm, ß = 100.03 ± 0.08'. There are characteristic isolated Ge2P4 8_ and Ge2As4 8 ~ anions, which are arranged in sheets. | | | |
Reference
| Z. Naturforsch. 37b, 1221—1224 (1982); eingegangen am 19. April 1982 | | | |
Published
| 1982 | | | |
Keywords
| Intermetallic Compounds, Zintl Phases, Crystal Structure | | | |
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| default:Reihe_B/37/ZNB-1982-37b-1221.pdf | | | | Identifier
| ZNB-1982-37b-1221 | | | | Volume
| 37 | |
| 18 | Author
| Rainer Mattes, Kurt-Ludwig Richter | Requires cookie* | | | Title
| Darstellung und Struktur des Polyvanadato-periodates Na6 [H2V2I2016] * 10 H20 Preparation and Crystal Structure of the Heteropoly Periodate Na6[H2V2I20i6] * 10 H2O | | | | Abstract
| The structure of the heteropoly periodate ion [H2V2I20i6] 6 ~ has been determined in its Na salt at —150 °C by single crystal X-ray diffraction with 1909 reflections and refined to F = 0.022 (R'= 0.028). Na6[H2V2I2Oi6] • 10 HaO crystallizes in the triclinic space group PI with a = 11.407(5), b = 8.865(3), c = 6.105(3)1, a = 82.07(3)°, /? = 84.24(4)° y = 70.23(3)°, V = 574.5 A 3 , Z = 1. The [H2V2I2Oi6] 6 ~ anion consists of edge and corner sharing 106 octahedra and VO5 square pyramids. The vibrational spectra clearly indicate the presence of VO(terminal)2 groups. | | | |
Reference
| Z. Naturforsch. 37b, 1241—1244 (1982); eingegangen am 17. Mai 1982 | | | |
Published
| 1982 | | | |
Keywords
| Heteropoly Periodate, Vanadato Periodate, Crystal Structure | | | |
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| default:Reihe_B/37/ZNB-1982-37b-1241.pdf | | | | Identifier
| ZNB-1982-37b-1241 | | | | Volume
| 37 | |
| 20 | Author
| D. Babel | Requires cookie* | | | Title
| Die Kristallstruktur des Cyano-Elpasoliths [N(CH3)4]2CsFe(CN)6 The Crystal Structure of the Cyano Elpasolite [N(CH3)4]2CsFe(CN)6 | | | | Abstract
| The crystal structure of the cubic compound [N(CH3)4]2CsFe(CN)6 was determined by X-ray methods: a = 2527.4(6) pm, space group Fd3c, Z = 32, Rg = 0.028 (260 independent single crystal reflections). The resulting distances within the practically undistorted Fe (CN) 6 3 ~ -octahedron are Fe-C = 193.4(6) and C-N = 115.7(7) pm. Compared to the ideal elpasolite structure of space group Fm3m, Z = 4, the octahedra are rotated by 7.4° through their 3 axis. This is discussed as caused by steric requirements of the tetramethyl-ammonium groups (N-C = 148.4(10) and 149.1(38) pm, resp.). Three quarters of them, of which also the hydrogen positions could bo located, are well oriented. The remaining quarter shows orientational disorder to approach similar contact distances as the other N(CH3)4+ ion exhibits between the methyl groups and the nitrogen ends of the anions. | | | |
Reference
| Z. Naturforsch. 37b, 1534—1539 (1982); eingegangen am 11. August 1982 | | | |
Published
| 1982 | | | |
Keywords
| Crystal Structure, Elpasolite, Hexacyanoferrate(III) | | | |
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| default:Reihe_B/37/ZNB-1982-37b-1534.pdf | | | | Identifier
| ZNB-1982-37b-1534 | | | | Volume
| 37 | |
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