| 1 | Author
| Rüdiger Kniep, Lutz Körte, Dietrich Mootz | Requires cookie* | | Title
| Kristallstrukturell von Verbindungen A2X2 (A = S, Se; X = Cl, Br) Crystal Structures of Compounds A2X2 (A = S, Se; X = Cl, Br)  | | | Abstract
| The crystal structures of compounds A2X2 (A = S, Se; X = Cl, Br) contain molecules X-A-A-X with dihedral angles between 83.9° and 87.4°. Three different types of molecular packing are realized: S2CI2, S2Br2 (a-Se2Br2) and /?-Se2Br2(Se2Cl2). Details of molecular geometries as well as crystal structures are discussed. | | |
Reference
| (Z. Naturforsch. 38b, 1—6 [1983]; eingegangen am 20. August 1982) | | |
Published
| 1983 | | |
Keywords
| Sulfur(I) Halides, Selenium(I) Halides, Crystal Structure | | |
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| default:Reihe_B/38/ZNB-1983-38b-0001.pdf | | | Identifier
| ZNB-1983-38b-0001 | | | Volume
| 38 | |
3 | Author
| PeterG. Jones, GeorgeM. Sheldrick, Einhard Schwarzmann, Andreas Vielmäder | Requires cookie* | | Title
| Darstellung und Kristallstruktur von Di-gold(III)bis(selenit)oxid, Au2(Se03)20 Preparation and Crystal Structure of Di-gold(III) Bis(selenite) Oxide, Au2(Se03)20  | | | Abstract
| Au2(Se0s)20 was prepared from gold and excess selenic acid in a sealed tube at 533 K. The crystal structure [P6a2, a = 659.2(2), b = 1183.7(3), c = 399.8(1) pm, Z = 2,R = 0.087] was determined; gold atoms are bridged by oxide ions (lying on twofold axes) and selenite ions. The extended structure consists of polymeric layers parallel to the ««/-plane. The light atom positions are inaccurate because of the presence of a heavy atom in a polar space group. | | |
Reference
| (Z. Naturforsch. 38b, 10—11 [1983]; eingegangen am 20. September 1982) | | |
Published
| 1983 | | |
Keywords
| Crystal Structure, Sealed-tube Synthesis, Gold(III), Selenite, Oxide | | |
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| default:Reihe_B/38/ZNB-1983-38b-0010.pdf | | | Identifier
| ZNB-1983-38b-0010 | | | Volume
| 38 | |
5 | Author
| W. S. Sheldrick | Requires cookie* | | Title
| Characterisation of a Binary Transition Metal Complex of a Purine 3 -Nucleotide, {[Cua(3 -GMP)2(3 -GMPH)2(H20)5] 7 H20}". [1] Phosphate-only Binding of Copper(II)  | | | Abstract
| Guanosine 3'-Monophosphate, Copper(II) Complex, Phosphate-only Binding, X-ray {[Cu3(3'-GMP)2(3'-GMPH)2(H20)5] • 7 H20}" (1) was isolated from an aqueous solution of Cu(N03)2 and guanosine 3'-monophosphate at a pH of 4.4. 1 is monoclinic space group C 2 with a = 29.140(7), b = 6.865(5), c = 16.980(7)Ä, ß = 90.31(3)°, Z = 2, Dc = 1.81 g -cm-". The structure was refined to R — 0.065 with i?w = 0.060 for 2642 independent reflections. It is disordered about a crystallographic diad axis with one of the copper atoms Cu(2) sited on this axis. This and the other independent copper atom Cu(l) both display square pyramidal geometries. Cu(l) binds N(7) of a guanine base, two phosphate O atoms of nucleotide molecules not symmetry-related to one another and two water oxygens. The guanine base involved in this coordination adopts a syn-conformation relative to the ribose ring with = —118.5°. Cu(2) is coordinated by four phosphate O atoms of different nucleotide molecules and one water oxygen. The second guanine base, which is not involved in metal binding, displays the anZi-conformation relative to the ribose ring. | | |
Reference
| (Z. Naturforsch. 38b, 16—19 [1983]; received September 6 1982) | | |
Published
| 1983 | | |
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| default:Reihe_B/38/ZNB-1983-38b-0016.pdf | | | Identifier
| ZNB-1983-38b-0016 | | | Volume
| 38 | |
6 | Author
| Bernt Krebs, Marita Hucke, Michael Hein, Andreas Schäffer | Requires cookie* | | Title
| Monomere und dimere Oxotrihalogenoselenate(IV): Darstellung, Struktur und Eigenschaften von [As(C6H5)4]SeOCl3 und [N(C2H5)4]SeOCl3 Monomerie and Dimeric Oxotrihalogenoselenates(IV): Preparation, Structure and Properties of [As(C6H5)4]SeOCl3 and [N(C2H5)4] SeOCl3  | | | Abstract
| The monomeric SeOCl3~ ion, which can be prepared as the tetraphenylarsonium salt from SeOCl2 and As(C6Hs)4C1, was structurally characterized by a low-temperature single crystal X-ray diffraction analysis. [As(C6Hs)4]SeOCl3 is monoclinic, space group P2i/c, with a = 9,332(3), b = 13,761(4), c = 18,985(6) A, ß = 110,97(3)° (at —135 °C), Z = 4; it contains a novel type of y>-trigonal bipyramidal oxotrichloroselenate(IV) anion which is not associated to dimers or polymer chains as in known structures. The equatorial positions are occupied by doubly bonded oxygen (Se-O 1,601(3) Ä) and by one Cl (Se-Cl 2,234(1) A), the axial Se-Cl bonds (2,430(1) and 2,475(1) A) being significantly longer. [N(C2H5)4]SeOCl3, which was obtained as crystals by oxidation of trichloroselenate(II), is triclinic, space group P I, with a = 10,607(3), b = 8,950(2), c = 8,862(2) A, a = 119,79(2)°, ß = 101,07(2)°, y = 96,28(2)°, Z = 2. The X-ray structure analysis shows the anions to be present as centrosymmetric dimers Se202Cl6 2 " like in the [P(CeH5)4] + salt, with two tetragonal SeOCU pyramids linked through a C1---C1 edge and the lone pairs trans to the axial Se-0 bonds (1,589(4) A). Se-Cl bond lengths are 2.270(1) and 2,351(2) A (terminal); 2,698(1) and 2,920(1) A (bridging). The results show that the nature of the reaction products of the Lewis acid SeOCl2 with halogenides as bases changes very sensitively with small variations in cations and environment. The vibrational spectra are discussed. | | |
Reference
| (Z. Naturforsch. 38b, 20—29 [1983]; eingegangen am 23. September 1982) | | |
Published
| 1983 | | |
Keywords
| Oxohalogenoselenates, Crystal Structure, Selenium, Inert Electron Pair, Selenium Oxychloride | | |
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| default:Reihe_B/38/ZNB-1983-38b-0020.pdf | | | Identifier
| ZNB-1983-38b-0020 | | | Volume
| 38 | |
8 | Author
| Lutz Rösch, Gerald Altnau, Carl Krüger, Y.-H Tsay | Requires cookie* | | Title
| Röntgenstrukturuntersuchungen an Trimethylsilylaluminiumverbindungen X-Ray Crystal Study of Trimethylsilylaluminium Compounds  | | | Abstract
| Structure, Tris(trimethylsilyl)aluminium, Sodium-tetrakis(trimethylsilyl)aluminate The crystal and molecular structures of three trimethylsilylaluminium compounds -tris(trimethylsilyl)aluminium coordinated to a diethylether molecule (1), sodium-tetrakis-(trimethylsilyl)aluminate coordinated to two toluene molecules (2 b) and unsolvated sodium-tetrakis(trimethylsilyl)aluminate (2 a) -have been determined by X-ray structure analysis. In all three compounds the aluminium is tetrahedrally coordinated, the Al-Si-distances lying between 2.44 and 2.49 A. (1) is monomeric and (2a) and (2b) form linear chains resulting from contact-ion pair interactions. | | |
Reference
| (Z. Naturforsch. 38b, 34—41 [1983]; eingegangen am 14. September 1982) | | |
Published
| 1983 | | |
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| default:Reihe_B/38/ZNB-1983-38b-0034.pdf | | | Identifier
| ZNB-1983-38b-0034 | | | Volume
| 38 | |
10 | Author
| Angelika Sebald, Bernd Wrackmeyer, Wolfgang Beck | Requires cookie* | | Title
| Kernresonanzspektroskopische Untersuchungen OH-, 13 C-, 31 P-, 195 Pt-NMR) an Alkinyl-Komplexen von Pt n , Pd n und Ni" Nuclear Magnetic Resonance ^H-, 13 C-, 31 P-, 195 Pt-NMR)-Studies of Alkynyl Derivatives of Pt 11 , Pd 11 and Ni 11  | | | Abstract
| The NMR parameters (X H, 13 C, 31 P, 195 Pt) of compounds of the type eis-and trans-[M(C=C-R)2(PR'3)2] (M = Ni, Pd, Pt) are reported. The chemical shifts <5 13 C (M-C=C; R) and <5 195 Pt (together with UV data) indicate the presence of jz-backbonding from the metal into the orbitals. This also explains some unusual features of the coupling constants J(= 13 C 1 H), J(i 3 C= 13 C) and J(195 Pt 13 C=). The NMR parameters reflect an increase in the amount of yr-backbonding for Pt < Pd < Ni. | | |
Reference
| (Z. Naturforsch. 38b, 45—56 [1983]; eingegangen am 1. Oktober 1982) | | |
Published
| 1983 | | |
Keywords
| Alkynyl Ptn, Pdn-, Nin-complexes, Multinuclear NMR | | |
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| default:Reihe_B/38/ZNB-1983-38b-0045.pdf | | | Identifier
| ZNB-1983-38b-0045 | | | Volume
| 38 | |
11 | Author
| Hans Hartl, Irene Brüdgam, Farbod Mahdjour-Hassan-Abadi | Requires cookie* | | Title
| Synthese und Strukturuntersuchungen von Iodocupraten(I): II. Diiodocuprate(I) RCuI2 mit isoherten Ketten ^ [Cul4 2~] * R 1 = N-Methylpyridinium, R 2 = Dimethyl ( 3 -dimethylamino -2 -aza -2 -propenyliden ) ammonium [1] Syntheses and Structure Analyses of Iodocuprates(I): II. Diiodocuprates(I) RCUL2 with Isolated Chains [CULI/2~]; R 1 = N-Methylpyridinium, R 2 = Dimethyl(3-dimethylamino-2-aza-2-propenyliden) Ammonium  | | | Abstract
| N-Methylpyridinium-diiodocuprate(I), CßHgNCuI^ and dimethyl(3-dimethylamino-2-aza-2-propenyliden)ammonium-diiodocuprate(I), C6H14N3CUI2, are obtained by reacting Cu with C6H8NI3 or C6H14N3I3 in acetone. Both compounds are built up by the organic cations and chains of edge sharing tetrahedra<jo[Cul4/2-]. The iodocuprate(I) anions are in intimate contact with the cations via intermolecular I • • • C interactions. Though nearly the same average Cu-I distance of 267.2 or 268.2 pm was found for both iodocuprate(I) anions there are different Cu-Cu distances (301-354 pm). | | |
Reference
| (Z. Naturforsch. 38b, 57—61 [1983]; eingegangen am 30. September 1982) | | |
Published
| 1983 | | |
Keywords
| Diiodocuprates(I), Synthesis, Crystal Structure | | |
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| default:Reihe_B/38/ZNB-1983-38b-0057.pdf | | | Identifier
| ZNB-1983-38b-0057 | | | Volume
| 38 | |
12 | Author
| Hubert Schmidbaur, Stefan Schnatterer, KailashC. Dash, ArefA M Aly | Requires cookie* | | Title
| Gold(I)-Bis(  | | | Abstract
| diphenylphosphino)amid und einige Gold(I)-Bis(diarylphosphino)methanide mit sterisch anspruchsvollen Arylsubstituenten Gold(I)-bis(diphenylphosphino)amide and Some Gold(I)-bis(diarylphosphino)methanides with Bulkyl Aryl Substituents Intensely yellow coloured, insoluble gold(I)-bis(diarylphosphino)amides, [(CeH^P^NAu, 1, is obtained from lithiated bis(diphenylphosphino)amine and AuCl complexes of tertiary phosphines. 1 is assigned a dimeric eightmembered ring structure on the basis of its 197 Au-Mößbauer spectrum and of a direct analogy with the corresponding bis(phosphino)methanide complexes, whose structure has recently been confirmed by X-ray diffraction. | | |
Reference
| (Z. Naturforsch. 38b, 62—66 [1983]; eingegangen am 16. September 1982) | | |
Published
| 1983 | | |
Keywords
| Gold Compounds, Metallocycles, Phosphino-amides, Phosphino-methanides, Steric Effects | | |
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| default:Reihe_B/38/ZNB-1983-38b-0062.pdf | | | Identifier
| ZNB-1983-38b-0062 | | | Volume
| 38 | |
14 | Author
| Walter Maringgele | Requires cookie* | | Title
| Neue Synthesewege zu cyclischen N-Silylharnstoffen und thioharnstoffen Reactions of Metal and Metalloid Compounds with Polyfunctional Molecules, XXXVII [1] New Syntheses of Cyclic N-Silylureas and -thioureas  | | | Abstract
| N-Silylated Ureas and Thioureas, Silicon Tetrachloride, Bis(dimethylamino)dimethylsilane N,N'-Diorganylureas react with silicon tetrachloride to give the l,3,5-triaza-2-silacyclo-hexan-4,6-diones 1-4, in case of N,N'-dicyclohexylurea to give dicyclohexylcarbodiimide. By reacting bis(diethylamino)dimethylsilane with N,N'-diorganylureas and thioureas, resp., one obtains l,3,5-triaza-2,4-disilacyclohexan-6-ones 6, 10, 13-15, l-oxa-3,5-diaza-6-silacyclohexan-4-ones 5, 9, l,3,5-triaza-2-silacyclohexan-4,6-diones 7, 11, 1,3-dioxa-5-aza-2,6-trisilacyclohexanes 8,12, l,3,5-triaza-2,4-disilacyclohexan-6-thiones 16-25 or the organylamino-diethylamino-dimethylsilanes 26-28. The compounds were characterized analytically and spectroscopically. | | |
Reference
| (Z. Naturforsch. 38b, 71—80 [1983]; eingegangen am 30. August 1982) | | |
Published
| 1983 | | |
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| default:Reihe_B/38/ZNB-1983-38b-0071.pdf | | | Identifier
| ZNB-1983-38b-0071 | | | Volume
| 38 | |
15 | Author
| Karl Wieghardt, Ursula Bossek, Martina Guttmann, Johannes Weiss | Requires cookie* | | Title
| Metallkomplexe der Liganden  | | | Abstract
| 1.4.7-Triazacyclononan-N.N .N -tris-2-ethansulfonat (TES) und 1.4.7-Triazacyclononan-N.N' .N'' -trisethylacetat (TEA). Die Kristallstrukturen von Na[Ni(TES)(H20)] • 5 H20 und Na[Cu(TES)] • 3 H20 Transition Metal Complexes Containing the Ligands 1,4,7-Triazacyclononane-N,N',N"-tris-2-ethanesulfonate (TES) and l,4,7-Triazacyclononane-N,N , ,N"-tris-ethylacetate (TEA). The Crystal Structures of Na[Ni(TES) (H20)] • 5H20 and of Na[Cu(TES)] • 3H20 The syntheses of two new, potentially hexadentate ligands with an N3O3 donor set is reported: l,4,7-triazacyclononane-N,N , ,N"-tris-2-ethanesulfonate (TES) and 1,4,7-tria-zacyclononane-N,N',N"-tris-ethylacetate (TEA). Complexes of the divalent transition metals Co(II), Ni(II), Cu(II) containing these ligands have been prepared. The kinetics of the reactions of [Co n (TEA)H20] 2 + and [Co II (TCTA)]-(TCTA= 1,4,7-triazacyclononane-N^^N'^tris-acetate) with [Fe m (CN)6] 3 ~, respectively, have been measured. A stable binuclear [Co(TEA)(CN)6Fe]~ species has been characterized in solution whereas the reaction of [Co(TCTA)]-with [Fe(CN)6] 3 -yields [Co in TCTA] and [Fe(CN)6] 4 -via an outer-sphere electron transfer reaction (k = 5,9 x 10 3 1 mol -1 sec -1 ; 25 °C, I = 0,26 M). Na[Ni(TES)H20] • 5H20 crystallizes in the triclinic space group P I (C^-No 2) with cell constants a = 806,7(4), b = 1468,4(8), c = 2317,9(8) pm, a = 72,36(4)°, ß = 83,48 (3)°, y = 81,99(4)°, and Z = 4. The nickel(II) center is in a distorted octahedral environment of a pentadentate TES ligand (N3Ü2)_and a coordinated H20. Na[Cu(TES)] 3H20 crystal-lizes in the triclinic space group P I (C^-No 2) w T ith cell constants a = 747,3(3), b — 1082,6(5), c = 1459,3(9) pm, a = 81,13(5)°, ß = 84,75(4)°, y = 79,39(3)°, and Z = 2. The copper(II) center is in a distorted quadratic pyramidal environment of a pentadentate TES ligand. Each of the complex anions contains one uncomplexed CH2-CH2-SC>3 _ group. | | |
Reference
| (Z. Naturforsch. 38b, 81—89 [1983]; eingegangen am 27. September 1982) | | |
Published
| 1983 | | |
Keywords
| Crystal Structure, O-Coordinated R-S03-group, Metal Complexes | | |
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| default:Reihe_B/38/ZNB-1983-38b-0081.pdf | | | Identifier
| ZNB-1983-38b-0081 | | | Volume
| 38 | |
16 | Author
| Monomeres, Helmut Endres, Nihat Gene, Dietrich Nöthe | Requires cookie* | | Title
| Oxamidoximkomplexe des Kupfers: Structures and EPR Spectroscopic Properties  | | | Abstract
| Chloro(oxamidoximato)(oxamidoxim)kupfer(II) und polymeres Dichloro(oxamidoxim)kupfer(II). Strukturen und EPR spektroskopische Eigenschaften Oxamide Oxime Complexes of Copper(II): Monomeric Chloro(oxamidoximato)(oxamidoxim)copper(II) and Polymerie Dichloro(oxamidoxim)copper(II). CU(C2H6N402)(C2HSN402)C1 (1) crystallizes in the monoclinic space group P2i/c, a = 8.191(4), b = 10.746(3), c = 13.340(7) Ä, ß = 104.94(4)°, V = 1134.5 A 3 , Z = 4, dc = 1.96 gem -3 , final Rw = 0.029 for 1785 reflections. In the monomeric complex molecules Cu is coordinated in the shape of a square pyramid with Cl at the apex. In the basal plane only one intramolecular H bridge exists. Cu(C2HeN402)Cl2 (2), crystallizes in the monoclinic space group Pc, a = 7.708(7), b = 3.751(1), c= 13.377(12) Ä, ß = 105.97(4)°, V = 371.8Ä 3 , Z = 2, dc = 2.25 gem" 3 , final Rw — 0.070 for 903 reflections. The stacking of the nearly planar complex units along b leads to a polymeric structure where Cu is additionally coordinated by a Cl atom, and shows a loose interaction with an oxime N atom of an adjacent monomer. The EPR signal intensity shows Curie-Weiss behaviour in the temperature range 110 K-420 K. | | |
Reference
| (Z. Naturforsch. 38b, 90—95 [1983]; eingegangen am 4. Oktober 1982 1) | | |
Published
| 1983 | | |
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| default:Reihe_B/38/ZNB-1983-38b-0090.pdf | | | Identifier
| ZNB-1983-38b-0090 | | | Volume
| 38 | |
19 | Author
| Jürgen Schallenberg, Eckart Meyer | Requires cookie* | | Title
| Simple Syntheses of 3-Substituted Indoles and their Application for High Yield 14 C-Labelling  | | | Abstract
| Methods are described which allow the synthesis of several plant indole alkaloids and their metabolites at different scales. Compounds synthesized include gramine (1) (3-di-methylaminomethylindole) which is directly derived from indole, while its biosynthetic precursors 3-aminomethylindole (3) and 3-methylaminomethylindole (2) as well as indole-3-carboxylic acid (7) are synthesized via indole-3-aldehyde (6). Slight changes of the experimental conditions allow syntheses with high yields not only at the molar but also at the /imolar level. This is extremely useful when isotope labelled compounds of high specific radioactivity are required for studies of plant metabolism. | | |
Reference
| (Z. Naturforsch. 38b, 108—112 [1983]; received July 22 1982) | | |
Published
| 1983 | | |
Keywords
| 3-Substituted Indoles, Indole Alkaloids, UV Spectra, MS Spectra, 1 H NMR spectra | | |
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| default:Reihe_B/38/ZNB-1983-38b-0108.pdf | | | Identifier
| ZNB-1983-38b-0108 | | | Volume
| 38 | |
20 | Author
| Wolf-Walther Du Mont, Mario Grenz | Requires cookie* | | Title
| Bis(trimethylsiloxy)tin(II): A Heterosiloxane as Soft Ligand  | | | Abstract
| Contrary to earlier reports the reaction of sodium trimethylsilanolate with stannous chlo-ride does not yield bis(trimethylsiloxy)tin(II) (1) but a polynuclear compound of the type Sn20(0SiMe3)2 (2). 1 is obtained from the reac-tion of stannocene with trimethylsilanole. The compound is a dimer that gives rapid exchange reactions of terminal and bridging trimethylsil-oxy groups in inert organic solvents. | | |
Reference
| (Z. Naturforsch. 38b, 113—114 [1983]; eingegangen am 10. September 1982) | | |
Published
| 1983 | | |
Keywords
| Oxastannylenes, Heterosiloxanes, NMR Spectra | | |
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| default:Reihe_B/38/ZNB-1983-38b-0113_n.pdf | | | Identifier
| ZNB-1983-38b-0113_n | | | Volume
| 38 | |
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