| | 221 | Author
| Steffen Runge, M. Athias, O. Senge | Requires cookie* | | | Title
| Electron Donor-Acceptor Compounds. Synthesis and Structure of 5-(l,4-Benzoquinone-2-yl)-10,15,20-trialkylporphyrins  | | | | Abstract
| A series of 5-(benzoquinone)-10,15,20-trialkylporphyrins was synthesized via cross conden sation of the respective aldehydes, 2,5-dimethoxybenzaldehyde and pyrrole followed by de-methylation with BBr3 and oxidation with P b 0 2. This method worked reasonably well for compounds bearing the benzoquinone substituent and butyl, isopropyl, 1 -methylpropyl and 2-ethylpropyl residues (2a-d). The free base porphyrin quinones were converted into the zinc(II) complexes (3a-d) all of which showed remarkable stability for porphyrin quinones. The zinc(II) complex 3c bearing isopropyl residues was investigated by X-ray crystallography and showed a supramolecular structure consisting of polymeric chains facilitated by coordina tion of a benzoquinone oxygen to a neighboring zinc(II) center. Attempts to synthesize a 5-(benzoquinone)-10,15,20-tris(terr-butylporphyrin) resulted in the formation of a yellow por-phomethene (4), which could not be oxidized further. A crystal structure analysis of 4, the first for a free base porphomethene, shows an extremely twisted conformation with syn-orientation of the three rm-butyl groups. The results indicate that new methods will have to be developed for the synthesis of nonplanar porphyrin quinones. | | | |
Reference
| Z. Naturforsch. 53b, 1021—1030 (1998); received June 15 1998 | | | |
Published
| 1998 | | | |
Keywords
| Porphyrins, Quinones, Electron Transfer Compounds, Crystal Structure, Conformation | | | |
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| default:Reihe_B/53/ZNB-1998-53b-1021.pdf | | | | Identifier
| ZNB-1998-53b-1021 | | | | Volume
| 53 | |
| 222 | Author
| M. Sm, B. Ern, H. Ard, N. Eum Üller, K. Urt, D. Ehnicke | Requires cookie* | | | Title
| ClPb[N(SiMe3)2]3 C rystal S tructure of C lPb[N (SiM e3 ) 2 ]3 | | | | Abstract
| Pale brown single crystals of the title compound have been obtained by the reaction of Pb[N(SiMe3) 2] 2 with molybdenum pentachloride in ether solution as a result of a redox reaction. ClPb[N(SiMe3) 2] 3 crystallizes in the trigonal space group R3 with three formula units per unit cell. Lattice dimensions at -50 °C: a = b -1828.7(2), c = 854.5(1) pm. The compound forms monomeric molecules with bond lengths P b-C l = 247.9(4) pm and P b -N = 213(2) pm. | | | |
Reference
| Z. Naturforsch. 53b, 1074—1076 (1998); eingegangen am 3. Juli 1998 | | | |
Published
| 1998 | | | |
Keywords
| Lead(IV), Amido Complex, Crystal Structure | | | |
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| default:Reihe_B/53/ZNB-1998-53b-1074_n.pdf | | | | Identifier
| ZNB-1998-53b-1074_n | | | | Volume
| 53 | |
| 223 | Author
| Frank Wendland, Christian Näther, Michael Schur, Wolfgang Bensch | Requires cookie* | | | Title
| Solvothermal Synthesis and Crystal Structure Determination of Tris- (ethyleneamine-ammonium) Tetraselenoantimonat: Non-Centrosymmetry Mediated by an Extended Unusual N-H***N Hydrogen Bonded Network? | | | | Abstract
| The title compound has been synthesized under solvothermal conditions by the reaction of elemental chromium, antimony and selenium in a solution of 40% 1,2-ethanediamine (en) in methanol. The crystal structure consists of tetrahedral SbSe,*3 --anions which are connected by monoprotonated 1,2-ethanediamine (enH+) cations via N-H--Se hydrogen bonding. The enH+ cations are joined via strong N-H -N hydrogen bonds between the ammonium hydrogen and the amino nitrogen atom forming four distinct chains, each built up of three crystallographically independent enH+ cations. Two of these chains are running parallel to [100], the other two are parallel to [010]. Based on this arrangement different centrosymmetric or non-centrosymmetric hydrogen bonding patterns are possible, but only in one chain the sequence of NH2 and NH3+ groups was determined by X-ray diffraction. | | | |
Reference
| Z. Naturforsch. 53b, 1144—1148 (1998); received June 15 1998 | | | |
Published
| 1998 | | | |
Keywords
| Selenoantimonates, Solvothermal Synthesis, Crystal Structure, Hydrogen Bonding | | | |
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| default:Reihe_B/53/ZNB-1998-53b-1144.pdf | | | | Identifier
| ZNB-1998-53b-1144 | | | | Volume
| 53 | |
| 224 | Author
| Markus Tampier, Dirk Johrendt | Requires cookie* | | | Title
| B aC u 6G e2S8 -Ein Thiogermanat als Variante der L i3Bi-Struktur BaCu6Ge2S8 -A Thiogermanate as a Variant of the Li3Bi Structure | | | | Abstract
| BaCu6Ge2S8 was synthesized by direct reaction of the elements at 750°C and characteri zed by X-ray single crystal techniques. The thiogermanate crystallizes in a new orthorhombic structure type (a = 6.122(1) A, b = 12.084(3) A , c = 17.614(5) A; Pbcm, Z = 4). Isola ted [GeS4]4_ tetrahedra form a slightly distorted cubic face-centered (fee) arrangement. Ba-and Cu-atoms each occupy half the octahedral gaps (O G) of this " tetrahedra packing" . Fur ther Cu atoms fill the tetrahedral gaps (T G) completely. The compound can be written as Ba2<l/2 0 G,(Cu2)2<l/2<:)G)Cu8<7G)(GeS4)4 . Thus the structure o f BaCu6Ge2S8 can be derived from the Li^Bi type. The sulfur coordination o f the metal atoms (Cu tetrahedral or trigonal, Ba with CN 8) are realized by the spatial orientation of the [GeS4]4~ tetrahedra. Their centers nearly maintain the fcc-arrangement. This structure interpretation of BaCu6 Ge2S8 from the viewpoint o f a " filled tetrahedra packing" is discussed for further known thiogermanate compounds. | | | |
Reference
| Z. Naturforsch. 53b, 1483—1488 (1998); eingegangen am 9. Juli 1998 | | | |
Published
| 1998 | | | |
Keywords
| Chalcogenides, Germanium, Copper, Preparation, Crystal Structure | | | |
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| default:Reihe_B/53/ZNB-1998-53b-1483.pdf | | | | Identifier
| ZNB-1998-53b-1483 | | | | Volume
| 53 | |
| 225 | Author
| Z. Naturforsch | Requires cookie* | | | Title
| The Stereochemistry of Chloro-bis(N-morpholino)phenylsilane | | | | Abstract
| Treatment of phenyltrichlorosilane with an excess of morpholine and N-lithium-morpholide in pentane/toluene affords only the disubstitution product Cl(Ph)Si(M or)2 with Mor = 0 (C H 2C H :)2N-. The third halogen atom is not replaced owing to sterical hindrance. The title compound crystallizes with two independent molecules in the unit cell. These two molecules can be classified as enantiomers, because a disrotatory twist of the two morpholino ligands away from the potential mirror plane induces a chiral conformation. In benzene solution there is racemization owing to completely free rotation, chair/boat interconversion, and nitrogen inversion of the morpholino groups on the NMR time scale, but all CH 2 protons remain anisochronous (diastereotopic). | | | |
Reference
| (Z. Naturforsch. 54b, 18—20 [1999]; received October 15 1998) | | | |
Published
| 1999 | | | |
Keywords
| Silylamines, Aminosilanes, Symmetry, NMR Data, Crystal Structure | | | |
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| default:Reihe_B/54/ZNB-1999-54b-0018.pdf | | | | Identifier
| ZNB-1999-54b-0018 | | | | Volume
| 54 | |
| 226 | Author
| Z. Naturforsch | Requires cookie* | | | Title
| SrRhIn2, SrPdIn2, Srlrln2, and SrPtIn2 -New Intermetallic Compounds with a Filled Variant of the Caln2 Structure | | | | Abstract
| SrR hlm , SrPdIn2, Srlrln2, and SrPtIn2 have been synthesized by reaction of mixtures of the elements in glassy carbon crucibles in a high-frequency furnace. The new compounds were investigated by X-ray diffraction on powders as well as single crystals; a = 437.3(2), b = 1091.9(5), c = 798.0(2) pm for SrRhln^, a = 453.54(7), b = 1079.8(2), c = 790.4(1) pm for SrPdIn2, a = 434.83(8),b= 1102.6(2) ,c = 798.6(2) pm for Srlrln2, a = 447.5(1) , b = 1091.0(3), c = 787.6(1) pm for SrPtIn2. They adopt the MgCuAl2 structure, a ternary ordered version of Re^B. Chemical bonding analysis leads to the description of a filled S rln2 structure in which the In-in-bonding is modified by the insertion of transition metal atoms into the planar strontium layers, thus favoring strong indium-transition metal | | | |
Reference
| (Z. Naturforsch. 54b, 38—44 [1999]; received August 28 1998) | | | |
Published
| 1999 | | | |
Keywords
| Intermetallic Compounds, Crystal Structure, Chemical Bonding | | | |
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| default:Reihe_B/54/ZNB-1999-54b-0038.pdf | | | | Identifier
| ZNB-1999-54b-0038 | | | | Volume
| 54 | |
| 227 | Author
| MarkusF. Zum, R. Olf-D, Hoffm Ieter, Rainer Ann, Pöttgen | Requires cookie* | | | Title
| The Intermetallic Zirconium Compounds ZrNiAl, ZrRhSn, and ZrPtGa -Structural Distortions and Metal-Metal Bonding in Fe2P Related Compounds | | | | Abstract
| ZrNiAl, ZrPtGa, and ZrRhSn have been prepared by reacting the elements in an arc-melting furnace and subsequent annealing at 970 K. These compounds have previously been investigated only by use of X-ray powder data for ZrPtGa and ZrRhSn and single crystal film data for ZrNiAl. Precise single crystal diffractometer data are reported in the present paper. The structure of ZrNiAl is confirmed. It adopts a substitution variant of the FeiP type: P62m, a = 691.5(2), c = 346.6(1) pm, Z = 3, wR2 = 0.0538, 320 F2 values, 14 parameters. The structure refinement reveals a large displacement parameter U 33 for one nickel position, indicative of a slight nickel dislocation. Weak superstructure reflections could be found on Guinier powder patterns for ZrPtGa and ZrRhSn. These compounds crystallize with the HfRhSn type structure (Z = 6 , space group P62c), a superstructure of the Fe2P type: a = 714.5(1), c = 706.3(2) pm, w/?2 = 0.0651, 594 F2 values, 18 parameters for ZrPtGa and a = 734.2(2), c = 721.8(2) pm, wR2 = 0.0349, 355 F2 values, 18 parameters for ZrRhSn. Structural motifs of these compounds are transition metal centered trigonal prisms formed by the zirconium, aluminium, gallium, and tin atoms. While these trigonal prisms are regular in ZrNiAl, significant distortions occur in the structures of ZrPtGa and ZrRhSn. Due to the distortions of the trigonal prisms in the superstructures, some platinum and rhodium atoms are dislocated from the subcell mirror planes towards Pt-Pt and Rh-Rh pairs with distances o f 310 and 313 pm, respectively. The formation of the superstructure is most likely due to packing reasons. Chemical bonding in ZrRhSn was investigated on the basis of an extended Hückel calculation. | | | |
Reference
| (Z. Naturforsch. 54b, 45—53 [1999]; received August 20 1998) | | | |
Published
| 1999 | | | |
Keywords
| Intermetallic Compounds, Crystal Structure, Superstructure, Chemical Bonding | | | |
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| default:Reihe_B/54/ZNB-1999-54b-0045.pdf | | | | Identifier
| ZNB-1999-54b-0045 | | | | Volume
| 54 | |
| 228 | Author
| Z. Naturforsch | Requires cookie* | | | Title
| U ntersuchungen an Polyhalogeniden, X X X IX | | | | Abstract
| [1] [(H 30)(1 8 -K r o n e -6)]I7, eine Struktur-Neubestim m ung Studies on Polyhalides, X X X IX [1] S tructure R efinem ent of [(H 30)(1 8 -cro w n -6)]I7 Sawsan A bd El K halika, M ervat El Essaw ia, Ingo D om brow skih, K arl-Friedrich T ebbeb * The structure analysis of the compound [(H30)(18-Krone-6)]I7 has been repeated. The al ready known structure could now be described with improved precision. The unique polyiodide chain i [ (I _'2I2) I2] may be derived from the regu lar three dimensional iodide-iodine lattice c»[U 3I2] by separation. | | | |
Reference
| Z. Naturforsch. 54b, 136—139 (1999); eingegangen am 6. Oktober 1998 | | | |
Published
| 1999 | | | |
Keywords
| Polyhalogenide, Heptaiodide, Crown Ether, Oxonium Compound, Crystal Structure | | | |
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| default:Reihe_B/54/ZNB-1999-54b-0136_n.pdf | | | | Identifier
| ZNB-1999-54b-0136_n | | | | Volume
| 54 | |
| 229 | Author
| Rainer Mattes, Ulrich Voet | Requires cookie* | | | Title
| Komplexe zweier vierzehngliedriger Tetraazadibenzo-Makrocyclen. Strukturen eines freien Liganden und von Nickel(II)-, Kupfer(II)-und Zink(II)-Komplexen Complexes o f Two 14-Membered N4 Dibenzo Macrocycles. Crystal Structures o f a Free Ligand and o f Nickel(II), Copper(II) and Zinc(II) Complexes | | | | Abstract
| The syntheses and structural characterizations of complexes of two 14-membered macrocy clic trans-N4 dibenzo ligands, 5,7,8,9,14,16,17,18-octahydrodibenzo[e,l]-[l,4,8,l ll-tetraaza-cyclotetradecine-6,15-dimethyl (L3) resp. -6,15-diacetamide (L4), are presented. The crystal structures of five compounds have been determined by single crystal X-ray diffraction. The free ligand L3 has a saddle-shaped structure with intramolecular hydrogen bonds. This conformation of the ligand exists also in the Zn(II) complex in which the metal ion is five-coordinated with the metal center outside the cavity. The coordination polyhedron is intermediate between a trigonal bipyramid and a square pyramid. In c/5-[Ni(L3)(NCS)2] the ligand is folded along an N- • N axis. The nickel ion in this complex shows an approximate octahedral geometry. For Ni(II) and Cu(II) complexes of ligand L the overall geometry is also distorted octahedral. The folding of the ligand causes a d s-N 40 2 coordination. | | | |
Reference
| Z. Naturforsch. 54b, 321—328 (1999); eingegangen am 6. Oktober 1998 | | | |
Published
| 1999 | | | |
Keywords
| Macrocyclic N4-Donor Ligands, Transition Metal Complexes, Crystal Structure | | | |
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| default:Reihe_B/54/ZNB-1999-54b-0321.pdf | | | | Identifier
| ZNB-1999-54b-0321 | | | | Volume
| 54 | |
| 232 | Author
| B. Wedelb, K. Sugiyama3, K. Hiraga3, K. Itagakib | Requires cookie* | | | Title
| Zur Kristallchemie des ersten Blei-Zink-Silicium-Telluroxids: PbZn4SiTeOio On the Crystal Chemistry o f the First Lead Zinc Silicon Tellurium Oxyde PbZn4SiTeO 10 | | | | Abstract
| Single crystals of the new lead zinc silicon tellurium oxide PbZn4SiTeO10 have been prepared by solid state reaction in air. The compound is colourless and crystallizes in orthorhombic symmetryj space group Dih Pnma, with the cell parameters: a = 6.542 (5), b = 15.624(4), c = 8.280(4) A, Z = 4. The structure has been determined from a single crystal X-ray study and refined to the conventional values R = 0.032 and wR(F2) = 0.050. Zn~+ and Si4+ show tetrahedral and Te6+ octahedral coordination by 0 2~.The crystal structure is dominated by a ^ [Zn4O l0]12-framework with isolated Te066+ and Si044+ polyhedra. Pb2+ ions are incorporated in the network. The centres of negative charge of the lone of the Coulomb term of the lattice energy. | | | |
Reference
| Z. Naturforsch. 54b, 469—472 (1999); eingegangen am 3. Dezember 1998 | | | |
Published
| 1999 | | | |
Keywords
| Lead, Zinc, Silicon, Tellurium, Crystal Structure | | | |
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| default:Reihe_B/54/ZNB-1999-54b-0469.pdf | | | | Identifier
| ZNB-1999-54b-0469 | | | | Volume
| 54 | |
| 233 | Author
| Markus Häp, TheoG. Illes, Thomas Kruck, Karl-Friedrich Tebbe | Requires cookie* | | | Title
| Dichloro | | | | Abstract
| [bis(775-2,4-cyclopentadien-l-yl)aIkylphosphan]zirconium: PR(C5H4)2 ZrCl2 ; R = Me, Et, 'Pr, 'Bu Dichloro[bis(/7r'-2 ,4 -cyclopentadien-l-yl)alkylphosphine]zirconium: PR(C5H4)7ZrCL; R = Me, Et, 'Pr, ?Bu A series of new ansa-zirconocene dichloride compounds [PR(C5H4)2ZrCl2: R = Me (5), Et (6), 'Pr (7), ?Bu (8)] with phosphorus as bridging atom between the cyclopentadienyl rings have been prepared, isolated, and characterised by 'H, i3C, 31P NMR spectroscopy, mass spectrometry and elemental analysis. The X-ray structure of 5 is reported. | | | |
Reference
| Z. Naturforsch. 54b, 482—486 (1999); eingegangen am 22. Dezember 1998 | | | |
Published
| 1999 | | | |
Keywords
| Zirconium Ansa-Metallocene, Cyclopentadienyl, Phosphine, Crystal Structure | | | |
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| default:Reihe_B/54/ZNB-1999-54b-0482.pdf | | | | Identifier
| ZNB-1999-54b-0482 | | | | Volume
| 54 | |
| 234 | Author
| MikeR. Kopp, Thomas Kräuter, Anahita Dashti-Mommertz, Bernhard Neumüller | Requires cookie* | | | Title
| Organogallitimamide: Synthese und Kristallstrukturen von [IPr2GaN(H/Bu]2 und [Mes(Cl)GaN(H)'Bu]2 Organogallium Amides: Synthesis and Crystal Structures o f ['Pr-,GaN(H)'Bu]-, and [Mes(Cl)GaN(H)'Bu]2 | | | | Abstract
| ['Pr2GaN(H)'Bu]2 (1) and [Mes(Cl)GaN(H)'Bu]2 (2) can be synthesized by the metathesis reaction of 'Pr2GaCl and MesGaCl2 with one equivalent of LiN(H)'Bu, respectively. 1 and 2 were characterized by NMR, IR and MS techniques as well as by X-ray structure analyses. 1 and 2 consist of centrosymmetric dimeric molecules with a G a2N2 skeleton. According to cryoscopic measurements in benzene, both amides | | | |
Reference
| Z. Naturforsch. 54b, 627—631 (1999); eingegangen am 8. Januar 1999 | | | |
Published
| 1999 | | | |
Keywords
| Gallium Compounds, Organogallium Amides, Crystal Structure | | | |
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| default:Reihe_B/54/ZNB-1999-54b-0627.pdf | | | | Identifier
| ZNB-1999-54b-0627 | | | | Volume
| 54 | |
| 235 | Author
| Steffen Runge3, MathiasO. Senge3, Karin Ruhlandt-Sengeb | Requires cookie* | | | Title
| 5,10,15,20-Tetrakis(diphenylmethyl)porphyrin -A Nonplanar Porphyrin with Intermediate Degree of Ruffling | | | | Abstract
| The title compound was prepared by condensation of pyrrole and diphenylacetaldehyde in 16% yield. Based on spectroscopic data, the free base porphyrin exhibits a nonplanar macrocycle in solution with a degree of distortion between that of 5,10,15,20-tetracyclohexyl-porphyrin and 5,10,15,20-tetra(r-butyl)porphyrin. A crystal structure determination of the cobalt(II) complex reveals a ruffled macrocycle conformation with an average out-of-plane displacement of the m eso carbon atoms by 0.55 A. | | | |
Reference
| Z. Naturforsch. 54b, 662 (1999); received February 17 1999 | | | |
Published
| 1999 | | | |
Keywords
| Porphyrins, Steric Strain, Cobalt Porphyrins, Crystal Structure, Conformation | | | |
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| default:Reihe_B/54/ZNB-1999-54b-0662.pdf | | | | Identifier
| ZNB-1999-54b-0662 | | | | Volume
| 54 | |
| 236 | Author
| Axel Lifferth3, IsabelB. Ahnera, Ut Helm, Lackner, M. Artina Schäferb | Requires cookie* | | | Title
| Synthese und Struktur von Prolinring-modifizierten Actinomycinen des X-Typs Synthesis and Structure of Proline Ring Modified Actinomycins of the X-Type | | | | Abstract
| The first total synthesis o f actinomycins containing L-4-hydroxyproline (1) and the separa tion and NM R spectroscopic assignment o f the regioisomers X (V* and iso-X0/i (lc, le) are described. The synthetic X 0/j proves, that the oxidized proline ring of the natural actinomycins | | | |
Reference
| Z. Naturforsch. 54b, 681—6 (1999); eingegangen am 15. Januar 1999 | | | |
Published
| 1999 | | | |
Keywords
| Antibiotics, Actinomycins, Synthesis, Crystal Structure, NM R Data | | | |
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| default:Reihe_B/54/ZNB-1999-54b-0681.pdf | | | | Identifier
| ZNB-1999-54b-0681 | | | | Volume
| 54 | |
| 237 | Author
| Joachim Pickardt, Pirka Wischlinski | Requires cookie* | | | Title
| Kristallstruktur des "supramolekularen" Komplexes [K(Benzo-18-krone-6)][Zn(CN)3]*H20 mit einem polymeren kettenförmigen Tricyanozincat-Anion Crystal Structure of the "Supramolecular" Complex [K(benzo-18-crown-6)][Zn(CN)3] *H20 with a Polymeric Tricyano Zincate Anion with Chain Structure | | | | Abstract
| Crystals o f the com plex [K (benzo-18-crown-6][Zn(CN)3] H20 were obtained from a solution o f Z n(C N)2, KCN, and b en zo-18-crown-6 in water/methanol. The compound crystallizes in the triclinic space group PI (no. 2),: Z = 2, a = 818,6(5), b = 1236,7(8), c = 1359,6(6) pm, a = 67,02(4), ß = 87,38(4), 7 = 75,46(5). Each Zn atom is bonded to one bridging cyanide ion to give chains -Z n (C N)Z n -, and to two terminal CN groups. The N atom o f one o f the terminal CN groups interacts with a potassium ion o f the [K (benzo-18-crow n-6)]+ unit. The coordination spheres o f the K ions are completed by water molecules, which in turn form hydrogen bonds to N atoms o f terminal CN groups o f neighbouring chains, whereby puckered sheets are formed. | | | |
Reference
| Z. Naturforsch. 54b, 747 (1999); eingegangen am 10. Februar 1999 | | | |
Published
| 1999 | | | |
Keywords
| Zinc Cyanide C om plex, Crown Ether Complex, Crystal Structure | | | |
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| default:Reihe_B/54/ZNB-1999-54b-0747.pdf | | | | Identifier
| ZNB-1999-54b-0747 | | | | Volume
| 54 | |
| 238 | Author
| Christiane Leben, Martin Jansen | Requires cookie* | | | Title
| Darstellung und Kristallstruktur von Triammonium-trisulfimid (NH4)3(N S02)3 Preparation and Crystal Structure of Triammonium-trisulfimid (NH4)3(N S 0 2)3 | | | | Abstract
| The preparation and crystal structure o f (N H 4N S 0 2)3 (a = 11.720(2), b = 6.156(6), c = 14.030(2) A ,ß = 96.69(8)°) is reported. The structure reveals a chair-conformation o f the anions, which are arranged to form a hexagonal rod stacking. Compared to cyclometatriphosphates the cations are coordinated differently due to the different basicities o f the bridging nitrogen and oxygen atoms, respectively. | | | |
Reference
| Z. Naturforsch. 54b, 757 (1999); eingegangen am 24. Februar 1999 | | | |
Published
| 1999 | | | |
Keywords
| Sulfimide, Ammonium, Preparation, Single-Crystal Structure Determination | | | |
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| default:Reihe_B/54/ZNB-1999-54b-0757.pdf | | | | Identifier
| ZNB-1999-54b-0757 | | | | Volume
| 54 | |
| 239 | Author
| Petra Prokop, Rainer Richter, Lothar Beyer | Requires cookie* | | | Title
| Zur Reaktion von 2,4-Dioxo-4-ferrocenyl-butansäureethylester mit primären aromatischen Aminen On the Reaction of Ethyl 2,4-Dioxo-4-ferrocenyl-butanoate with Primary Aromatic Amines | | | | Abstract
| Starting from ethyl 2,4-dioxo-4-ferrocenyl-butanoate (1) a series of new ferrocene derivatives has been prepared. While the reaction with o-phenylene diamine leads to two ferrocene-con taining heterocyclic compounds, 4-ferrocenyl-3//-l,5-benzodiazepine-2-carbonic acid ethyl ester (3) and 3-(2-ferrocenyl-2-oxo-ethylidene)-3,4-dihydro-l//-quinoxalin-2-one • H20 (4), reactions with m-and /?-phenylene diamine give both the mono-and disubstituted products 5 -8, respectively. The conversion of 4 by Lawesson's reagent results in 2-ferrocenvl-thieno[2,3-b]quinoxaline (9). The new compounds have been characterized by their 'H , 1 C NMR, and mass spectra. The molecular structures of 4-ferrocenyl-4-oxo-2-phenylamino-but-2-enoic acid ethyl ester 2, and of 4 and 9 have been determined by X-ray crystal structure analysis. | | | |
Reference
| Z. Naturforsch. 54b, 849—857 (1999); eingegangen am 12. März 1999 | | | |
Published
| 1999 | | | |
Keywords
| Ferrocene, /3-Diketones, Enaminoketones, NMR Data, Crystal Structure | | | |
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| default:Reihe_B/54/ZNB-1999-54b-0849.pdf | | | | Identifier
| ZNB-1999-54b-0849 | | | | Volume
| 54 | |
| 240 | Author
| Max Herberhold, Silke Köppl, Wolfgang Milius | Requires cookie* | | | Title
| Mixed-Sandwich rflry Vanadium Complexes. The Molecular Structure of (?75-2-Methyl-indenyl)-(777-cycloheptatrienyl)-vanadium | | | | Abstract
| The diamagnetic halfsandwich complexes [V(?^7-C7H7)(CO)3] and [V(7/5-L5)(CO)4] have been used as intermediates in the conversion of hexcarbonylvanadium, V(CO)6, to the para magnetic trovacene derivatives, [V(775-L5)(r77-C7H7)] [L^ = cyclopentadienyl ligand, C5H4-R (R = H (1), Me (la), 'Bu (lb)) and CsMes (lc); indenyl (2) and 2-methylindenyl (2a)]. The molecular structure of 2a has been determined: the distances between vanadium and the center Z of the (nearly parallel) ring ligands are 193.0 pm | | | |
Reference
| Z. Naturforsch. 54b, 899—903 (1999); received April 8 1999 | | | |
Published
| 1999 | | | |
Keywords
| Sandwich Compounds, Cycloheptatrienyl Complexes, Vanadium, Crystal Structure | | | |
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| default:Reihe_B/54/ZNB-1999-54b-0899.pdf | | | | Identifier
| ZNB-1999-54b-0899 | | | | Volume
| 54 | |
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