| | 1 | Author
| ManfredL. Ziegler, Klaus Blechschmitt, Harald Bock, Ernst Guggolz, RichardP. Korswagen | Requires cookie* | | | Title
| Über die Reaktivität von [(CH 3 ) 2 N] 6 W 2 (W=W) gegenüber CS 2 /S 8 und CS 2 /Se, Röntgenstrukturanalyse von [(CH 3 ) 2 NCS 2 ] 2 W(S)(S 2 ) Reactivity of [(CH 3 ) 2 N] 6 W 2 (W=W) Towards CS 2 /S 8 and CS 2 /Se 8 . X-Ray Structure Analysis of [(CH 3 ) 2 NCS 2 ] 2 W(S)(S 2 )  | | | | Abstract
| In this paper we report two improved preparation methods for [(CH 3) 2 N] 6 W 2 (W=W) (1), one starting from WC1 4 (yield 51%), and a second one starting from W 2 C1 6 (THF) 4 (ca. 60% yield). We have studied the reactions of 1 with different nucleophiles, among them triphenylalkylidenphos-phoranes (like Ph 3 P=CH 2 and Ph 3 P=CHPh • LiCl; Ph = phenyl), sulfur and CS 2 . 1 reacts with S 8 and CS 2 in hexane to yield the two new compounds (Me 2 NCS 2) 2 WS(S 2) (4) and W(CS 2 H)(Me 2 NCS 2) 2 (5), both containing dithiocarbamato ligands formed by insertion of CS 2 into the W-N bond. The two mononuclear compounds were characterized spectroscopically, in the case of 4 an X-ray diffraction structure analysis was performed. The reaction of 1 with Se and CS 2 , leads to the compounds 4, (Me 2 NCS 2) 2 W 2 S 4 (6) and [(Me 2 N) 2 C]CS 2 (7), which were also characterized spectroscopically. No Se-containing compounds could be isolated. 4 crystallizes monoclinically, C 5 2h -P2Jn, with a = 648.6(3), b = 1346.7(6) and c = 1745.9(7) pm, ß = 91.85(3)°, V = 1524xl0 6 pm 3 , Z = 4. The structure of the seven-coordinate tungsten compound is discussed and compared to complexes with similar ligands and geometry. | | | |
Reference
| Z. Naturforsch. 43b, 590—598 (1988); eingegangen am 28. Dezember 1987 | | | |
Published
| 1988 | | | |
Keywords
| Reactivity, Synthesis, X-Ray | | | |
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| default:Reihe_B/43/ZNB-1988-43b-0590.pdf | | | | Identifier
| ZNB-1988-43b-0590 | | | | Volume
| 43 | |
| 2 | Author
| HerbertW. Roesky, Ulrich Seseke, Mathias Noltemeyer, GeorgeM. Sheldrick | Requires cookie* | | | Title
| Darstellungen und Strukturen viergliedriger Metall-Stickstoff-Ringe Preparations and Structures of Four-Membered Metal-Nitrogen Rings | | | | Abstract
| Ph 3 P=NSiMe 3 (1) reacts with InCl 3 , SnCl, and FeCl, to yield (Ph,P=N) 2 (InCl 2) 2 • 2 DMF (2a), (Ph 3 P=N) 2 Sn 2 Cl 4 • 2 CH 3 CN (3a) and (Ph 3 P=N) 2 (FeCl 2) 2 (4). The X-ray single crystal structures of 2a, 3a and 4 are reported. The compounds form four-membered rings consisting of alternating metal and nitrogen atoms. 2a and 4 are symmetrical, but 3a has both a Sn(II)Cl and a Sn(IV)Cl 3 group in the four-membered ring. | | | |
Reference
| Z. Naturforsch. 43b, 1130—1136 (1988); eingegangen am 29. März 1988 | | | |
Published
| 1988 | | | |
Keywords
| Indium, Tin, Iron, X-Ray | | | |
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| default:Reihe_B/43/ZNB-1988-43b-1130.pdf | | | | Identifier
| ZNB-1988-43b-1130 | | | | Volume
| 43 | |
| 5 | Author
| T. Sogo, J. Romero, A. Sousa, A. De Blas, M. L. Durán, E. E. Castellano | Requires cookie* | | | Title
| The Electrochemical Synthesis of Neutral Zinc(II) Complexes of Schiff Base Ligands: The Crystal Structure of Bis[N-(4-methylphenyl)salicylaldiminato]zinc(II) | | | | Abstract
| The electrochemical synthesis and physico-chemical properties of neutral zinc(II) complexes of bidentate Schiff bases derived from salicylaldehydes are presented together with the X-ray struc-ture of bis[N-(4-methylphenyl)salicylaldiminato]zinc(II). The crystal is monoclinic, a = 21.877(3), b = 8.801(2), c = 12.027(5) Ä, ß = 96.55(3)°, space group C2/c. The complex is a monomer, and the zinc atom is tetrahedrally coordinated. | | | |
Reference
| Z. Naturforsch. 43b, 611—615 (1988); received November 5 1987/January 28. 1988 | | | |
Published
| 1988 | | | |
Keywords
| X-Ray, Zinc, Schiff Bases, Electrochemical Synthesis | | | |
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| default:Reihe_B/43/ZNB-1988-43b-0611.pdf | | | | Identifier
| ZNB-1988-43b-0611 | | | | Volume
| 43 | |
| 7 | Author
| Uwe Scholz, Mathias Noltemeyer, HerbertW. Roesky | Requires cookie* | | | Title
| Synthese und Struktur eines ungewöhnlichen Molybdän-Heterocyclus durch Substitution eines Phenylringes in ortho-Stellung Synthesis and Structure of an Unusual Molybdenum Heterocycle by Substitution of a Phenyl Ring in ortho-Position | | | | Abstract
| The new ligand (Me 3 Si) 2 NC(Ph)NP(Ph) 2 N(SiMe 3) (1) reacts with MOOC1 4 to yield the green metallacycle 4. 4 was characterized by X-ray diffraction. Crystals of 4 are monoclinic, space group P2,/n with a = 1061.2(10). b = 1590.5(10), c = 1737.4(20) pm, ß = 104.84(7)° and Z = 4. Mo is coordinated octahedrally by two nitrogens of the bifunctional ligand. by one oxygen and three chlorine atoms. The ligand undergoes cyclization, a bond being formed between N and one phenylic o-position. | | | |
Reference
| Z. Naturforsch. 43b, 937—940 (1988); eingegangen am 23. März 1988 | | | |
Published
| 1988 | | | |
Keywords
| X-Ray, Molybdenum, Heterocycle Phosphorus-Nitrogen Compound | | | |
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| default:Reihe_B/43/ZNB-1988-43b-0937.pdf | | | | Identifier
| ZNB-1988-43b-0937 | | | | Volume
| 43 | |
| 8 | Author
| Gisela Sawitzki, Wolfgang Einholz, Wolfgang Haubold | Requires cookie* | | | Title
| Kristall-und Molekülstruktur von N,N'-Bis(l,3-dimethylbenzo[b]-l,3?2-diazaboroIidin-2-yl)carbodiimid Crystal and Molecular Structure of N,N'-Bis(l,3-dimethylbenzo[b]-l,3,2-diazaborolidin-2-yl)carbodiimide | | | | Abstract
| Crystals of the title compound (2) are monoclinic with a = 905.5(3), b = 593.6(2). c — 3243.5(8) pm, ß = 95.63(2)°, Z = 4, space group P2 x ln. The molecule 2 neither has a C 2 -symmet-rical allene-type nor a D 2d -symmetrical cumulene-type structure, but it has a non-linear B-N = C=N —B arrangement and is nearly planar. The central N = C=N angle has a value of 171.9(3)°, the B —N = C angles are 145.9(2)° and 163.1(3)°. | | | |
Reference
| Z. Naturforsch. 43b, 1179—1183 (1988); eingegangen am 25. Mai 1988 | | | |
Published
| 1988 | | | |
Keywords
| Boron-Nitrogen Compounds, Borylated Carbodiimides, X-Ray | | | |
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| default:Reihe_B/43/ZNB-1988-43b-1179.pdf | | | | Identifier
| ZNB-1988-43b-1179 | | | | Volume
| 43 | |
| 10 | Author
| Susanne Maier, Wolfgang Hiller, Joachim Strähle, Christina Ergezinger, Kurt Dehnicke | Requires cookie* | | | Title
| | | | | Abstract
| The copper(I)amidinato complex Cu 2 [Ph-C(NSiMe 3) 2 ] ; has been prepared by the reaction of CuCl with N.N,N'-tris(trimethylsilyl)benzamidine in boiling acetonitrile. forming white crystals. The compound was characterized by its IR spectrum as well as by an X-ray structure determina-tion. Crystal data: space group PI, Z = 2 (2851 observed independent reflexions, R = 0.047). Lattice dimensions at 20 °C: a = 1135.0(3); b = 1219.6(4); c = 1372.4(4) pm; a = 106.74(3)°; ß = 107.92(4)°; y = 91.40(4)°. The compound forms dimeric molecules with a short Cu--Cu contact of 242 pm and two chelating amidinato ligands with Cu-N bond lengths of (averaged) 189.0 pm and bond angles N —C—N of 124.1°. | | | |
Reference
| Z. Naturforsch. 43b, 1628—1632 (1988); eingegangen am 11. August/30. September 1988 | | | |
Published
| 1988 | | | |
Keywords
| Synthesis, X-Ray, Copper(I) Amidinato Complex | | | |
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| default:Reihe_B/43/ZNB-1988-43b-1628.pdf | | | | Identifier
| ZNB-1988-43b-1628 | | | | Volume
| 43 | |
| 12 | Author
| St Böck, H. Nöth, P. Rahm | Requires cookie* | | | Title
| Lithium-dimethylamino-hydrido-aluminate: Lösungszustand in Diethylether, Tetrahydrofuran und Dimethyldiglykolether Lithium Dimethylamino Hydrido Aluminates: The Solution State in Diethylether, Tetrahydrofuran and Dimethyldiglycol Ether | | | | Abstract
| The reaction of LiAlH 4 with dimethylamine has been studied in THF, diglyme and diethyl ether solution covering the molar ratios 1:0.5 to 1:4. In all cases the stoichiometric amount of H : is evolved. With the exception of LiAl[N(CH 3) 2 ] 4 all other members of the series LiAlH 4 _"[N(CH 3) 2 ]" cannot be isolated. They are in equilibrium with one another in solution. These equilibria are independent of the solvent used. The structure of compound LiAl[N(CH 3) 2 ] 4 -2(OC 4 H 8) has been determined by X-ray diffrac-tion. The anion acts as a bidentate ligand to Li which is also bonded to the oxygen atoms of two THF molecules. | | | |
Reference
| (Z. Naturforsch. 43b, 53—60 [1988]; eingegangen am 19. August 1987) | | | |
Published
| 1988 | | | |
Keywords
| Lithium Dimethylaminohydrido Aluminates, 27 A1 NMR Spectra, Solution State, X-Ray, 7 Li NMR Spectra | | | |
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| default:Reihe_B/43/ZNB-1988-43b-0053.pdf | | | | Identifier
| ZNB-1988-43b-0053 | | | | Volume
| 43 | |
| 13 | Author
| Frank Edelmann, Claudia Spang, HerbertW. Roesky, PeterG. Jones | Requires cookie* | | | Title
| Synthese und Struktur des ersten dreigliedrigen Arsen—Phosphor—Platin-Ringes Synthesis and Structure of the First Three-Membered Ring Containing Arsenic, Phosphorus and Platinum | | | | Abstract
| -butylphenylphosphane reacts with CpFe(C,H4AsCl2) in the presence of DBU to yield CpFe[C5H4As=PC6H2(f-Bu)?l. The reaction of this arsaphosphene with (Ph3P)2PtC2H4 yields CpFe[C5H4As—P[C6H2(r-Bu)3]Pt(PPh3)2], a compound with a three-membered ring containing arsenic, phosphorus and platinum. | | | |
Reference
| Z. Naturforsch. 43b, 517—520 (1988); eingegangen am 5. Januar 1988 | | | |
Published
| 1988 | | | |
Keywords
| X-Ray, NMR Spectra, Phosphorus, Arsenic, Platinum 2, 4, 6-Tri | | | |
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| default:Reihe_B/43/ZNB-1988-43b-0517.pdf | | | | Identifier
| ZNB-1988-43b-0517 | | | | Volume
| 43 | |
| 14 | Author
| Astrid Görge, Kurt Dehnicke, Dieter Fenske | Requires cookie* | | | Title
| N-Chlornitrenokomplexe des Wolframs: WC1 4 (NC1) und [CH 3 CN-WC1 4 (NC1)] N-Chloro-Nitrene Complexes of Tungsten: WC1 4 (NC1) and [CH 3 CN-WC1 4 (NC1)] | | | | Abstract
| WC1 4 (NC1) has been prepared as a red-brown crystal powder by the reaction of tungsten hexacarbonyl with excess nitrogen trichloride in boiling CC1 4 . The complex is associated via chloro bridges, forming dimeric units, according to the IR spectrum. Thermal decomposition at 200 °C leads to tungsten nitride trichloride, WNC1,. With acetonitrile, WC1 4 (NC1) reacts with formation of the monomeric complex [CH,CN-WC1 4 (NC1)], which was characterized by its IR spectrum as well as by an X-ray structure determination. Crystal data: space group P2,/m, Z = 2 (1387 independent observed reflexions, R — 0.07). Lattice dimensions at 20 °C: a = 590.4(3), b = 729.0(3), c = 1124.6(4) pm, ß = 100.63(2)°. The complex forms monomeric molecules, in which the tungsten atom has a distorted octahedral environment of four chlorine atoms in equatorial positions, and the acetonitrile molecule in fram-position to the W=N —Cl group. Bond lengths WN = 172 and NCI -161 pm; bond angle WNC1 = 175.5°. | | | |
Reference
| Z. Naturforsch. 43b, 677—681 (1988); eingegangen am 26. Januar 1988 | | | |
Published
| 1988 | | | |
Keywords
| Synthesis, IR Spectra, X-Ray, N-Chloro-Nitrene-Tungsten Tetrachloride, Acetonitrile Adduct | | | |
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| default:Reihe_B/43/ZNB-1988-43b-0677.pdf | | | | Identifier
| ZNB-1988-43b-0677 | | | | Volume
| 43 | |
| 15 | Author
| Fritz Preuss, Harald Becker, Jürgen Kaub, WilliamS. Sheldrick | Requires cookie* | | | Title
| Darstellung und Struktur der zweikernigen tert-Butyliminovanadium(IV)-Komplexe: [('C 4 H 9 N) 2 V 2 Cp 2 X 2 ] (X = 0'C 4 H 9 , Cl) Synthesis and Molecular Structure of the Binuclear terf-Butyliminovanadium(IV) Complexes: [('C 4 H9N) 2 V 2 Cp 2 X 2 ] (X = O f C 4 H 9 , Cl) | | | |
Reference
| Z. Naturforsch. 43b, 1195—1200 (1988); eingegangen am 18. Februar 1988 | | | |
Published
| 1988 | | | |
Keywords
| ferr-Butylimino-cyclopentadienylvanadium(IV) Complexes, Preparation, X-Ray, NMR Spectra, ESR Spectra | | | |
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| default:Reihe_B/43/ZNB-1988-43b-1195.pdf | | | | Identifier
| ZNB-1988-43b-1195 | | | | Volume
| 43 | |
| 16 | Author
| PaulG. Maué, Dieter Fenske | Requires cookie* | | | Title
| Zur Reaktion von [Cp 2 TiCl 2 ] und [CpTiC! 3 ] mit E(SiMe 3 ) 2 (E = S, Se) Die Kristallstrukturen von [Cp 3 Ti 2 S 2 Cl], [Cp 4 Ti 2 S 2 Cl 2 ], [Cp 3 Ti 2 Se 2 CI] und [Cp4Ti 4 Se 7 0] Reaction of [Cp 2 TiCl 2 ] and [CpTiCl 3 ] with E(SiMe 3 ) 2 (E = S. Se) The Crystal Structures of [Cp 3 Ti 2 S 2 Cl], [Cp 3 Ti 2 S 2 Cl 2 ], [Cp 3 Ti 2 Se 2 Cl] and [Cp 4 Ti 4 Se 7 0] | | | | Abstract
| The reaction of [Cp 2 TiCl 2 ] with E(SiMe 3) 2 leads to dinuclear Ti complexes. In [Cp 3 Ti 2 S 2 Cl] (1) and [Cp 3 Ti 2 Se 2 Cl] (3) two // 2 -S(Se) ligands bridge the Cp 2 Ti and CpTiCl units, respectively in contrast to these, [Cp 4 Ti 2 S 2 Cl 2 ] (2) contains a // 2 V-S 2 bridge connecting two Cp : TiCl fragments. A similar reaction of [CpTiCl 3 ] with Se(SiMe 3) 2 leads to the tetranuclear cluster [Cp 4 Ti 4 Se 7 0] (4). 4 consists of a Ti 4 -tetrahedron which encloses an oxygen atom. | | | |
Reference
| Z. Naturforsch. 43b, 1213—1218 (1988); eingegangen am 11. Mai 1988 | | | |
Published
| 1988 | | | |
Keywords
| X-Ray, Crystal Structure Dinuclear Ti-S and Ti-Se Complexes, Tetranuclear Ti Cluster | | | |
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| default:Reihe_B/43/ZNB-1988-43b-1213.pdf | | | | Identifier
| ZNB-1988-43b-1213 | | | | Volume
| 43 | |
| 18 | Author
| Bernhard Glaser, ErwinP. Mayer, Heinrich Nöth, Wilfried Rattay, Ulrich Wietelmann | Requires cookie* | | | Title
| Beiträge zur Chemie des Bors, 190 [1] Synthese und Molekülstruktur von 1,2-Dihydroboreten und Azadiboretidinen Contribution to the Chemistry of Boron, 190 [1] Synthesis and Molecular Structure of 1,2-Dihydrodiboretes and Azadiboretidines | | | | Abstract
| [2+2]-Cycloadditions of 9-Fluorenylidentetramethylpiperidinoboranes have been studied with selected olefines, acetylenes and iminoboranes. No reactions with olefines were observed. While propiolic methylester reacts exclusively at the carbonyl bond producing the oxaboretane 5, alkines such as diethylamino-alkines, cyclo-octine and phenylacetylene provide access to the'1,2-dihy-droboretenes 6, 3 and 2. Tetramethylpiperidinoiminoboranes make 1.2.4-azadiboretidines 7 available. 6a and 7a contain a folded four-membered ring as shown by X-ray structure analysis. There is only a weak 1,3-intraannular interaction due to BN-;r-bonding of the boron atoms with their exocyclic amino group. | | | |
Reference
| Z. Naturforsch. 43b, 449—456 (1988); eingegangen am 10. Dezember 1987 | | | |
Published
| 1988 | | | |
Keywords
| Reactivity of Aminomethyleneboranes, Transannular Interaction, X-Ray, 1, 2-Dihydroboret Derivatives, 1, 24-Azadiboretidine Derivatives | | | |
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| default:Reihe_B/43/ZNB-1988-43b-0449.pdf | | | | Identifier
| ZNB-1988-43b-0449 | | | | Volume
| 43 | |
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