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1991[X]
1Author    UlrichW. Annagat, Gabriele Bogedain, A. Drian Schervan, HeinrichC M Arsm Ann, DavidJ. Brauer, Hans Bürger, FrankD. Örrenbach, Gottfried Pawelke, Carl Krüger, Karl-Heinz ClausRequires cookie*
 Title    Das Isosterenpaar S iO /P N , I Zur Isosterie von Perchlorcyclosiloxanen und Perchlorcyclophosphazenen. Schwingungsspektren und Röntgenstrukturanalyse von (Cl2SiO )3 und (Cl2SiO )4 The SiO/PN Isoelectronic Pair, I Perchlorocyclosiloxanes and Perchlorocyclophosphazenes. Vibrational Spectra and X-Ray Structure Analysis o f (Cl2SiO) 3 and (Cl2SiO) 4  
 Abstract    Hexachlorocyclotrisiloxane (2) and octachlorocyclotetrasiloxane (4) were prepared by reac­ tion o f SiCl4 with 0 2 at 955 C. Their mass spectra are compared with those o f the isoelectronic cyclophosphazenes. The vibrational spectra o f 2 and 4 are very similar and closely related to that o f (PNC12)3, but clearly different from that o f the puckered (PNCU) 4 molecule. The X-ray examination o f 2 and 4 reveals planarity o f the (SiO)", n = 3 and 4 ring systems, with d (S i-O) on average 1.619(4) and 1.584(3) Ä, respectively. 
  Reference    Z. Naturforsch. 46b, 931—9 (1991); eingegangen am 2. Novem ber 1990 
  Published    1991 
  Keywords    Perchlorocyclosiloxanes, Perchlorocyclophosphazenes, Isoelectronic Relations, X-Ray, Vibrational Spectra 
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 TEI-XML for    default:Reihe_B/46/ZNB-1991-46b-0931.pdf 
 Identifier    ZNB-1991-46b-0931 
 Volume    46 
2Author    H. Erbert, W. Roesky, Birgit Meller-Rehbein, M. Athias NoltemeyerRequires cookie*
 Title    Reactions of M e2NC(S)SN(SiMe3)2 with M etal Halides -Crystal Structure of M e2NCS2ZrCl3 * 3 Pyridine  
 Abstract    M e-,NC(S)SN(SiM e3)2 (1) reacts with TeCl4 and N bC lj to yield M e2N C (S)SN TeC l2 (4) and 
  Reference    Z. Naturforsch. 46b, 1117—1121 (1991); eingegangen am 14. Februar 1991 
  Published    1991 
  Keywords    Tellurium, Niobium, Zirconium, Hafnium, Complexes, X-Ray 
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 TEI-XML for    default:Reihe_B/46/ZNB-1991-46b-1117_n.pdf 
 Identifier    ZNB-1991-46b-1117_n 
 Volume    46 
3Author    Yüniu Bai, M. Athias Noltemeyer, H. Erbert, W. RoeskyRequires cookie*
 Title    Synthese und Strukturen von Monoalkylamiden und -imiden des Titans Synthesis and Structures o f M onoalkylam ides and -imides of Titanium  
 Abstract    A new method for the preparation o f m onoalkylam ides o f com position Cp'TiCl2N H R is reported. M e3SnN H R (R = /Bu l a , CH/Pr-, lb) reacts with Cp'TiCl3 with elimination o f M e3SnCl to yield Cp'TiCLNHR (2) (2a: Cp' = C 5H 5, R = /Bu, 2b: Cp' = M e3SiC5H 4, R = t Bu, 2c: Cp' = (M e3Si)?C 5H 3, R = /Bu, 2d: Cp' = M e4C5H, R = /Bu, 2e: Cp' = M e5C5, R = t Bu, 2f: Cp' = C5H 5, R = CH/Pr2, 2g: Cp' = M e3SiC5H 4, R = CH/Pr2, 2h: Cp' = (M e3Si)2C5H3, R = CH/Pr2, 2i: Cp' = M e4C5H , R = CH/Pr2, 2j: Cp' = M e5C5, R = CH/Pr2). Compounds 2 a -2 j are stable and eliminate HC1 only in the presence o f a strong base to form (C5H 5T iC lN /B u)2 (3a) or (M e3SiC5H4T iC lN /B u)2 (3b) from 2 a and 2b, respectively. In 3a the chlorine atom s are substituted by N H /B u groups in boiling T H F by means o f L iN H /Bu to give (C5H 5T iN H /B uN /B u)2 (4). The reactions o f 2 e and 2b with L iN (SiM e3)2-Et20 in the presence o f pyridine yield M e5C5T iC lN /B u • Py (5 a) (Py = pyridine) and M e3SiC5H4T iC lN /B u P y (5 b), respectively. Com pounds 2 e and 5 a have been characterized by X-ray crystal structural analysis. 
  Reference    Z. Naturforsch. 46b, 1357 (1991); eingegangen am 22. März 1991 
  Published    1991 
  Keywords    X -Ray, Synthesis, Titanium, Amides, Imides 
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 TEI-XML for    default:Reihe_B/46/ZNB-1991-46b-1357.pdf 
 Identifier    ZNB-1991-46b-1357 
 Volume    46 
4Author    Dieter Sellmann+, Bernd Seubert, W. Olfgang Kern, Falk Knoch, M. Atthias, MollRequires cookie*
 Title    Übergangsmetallkomplexe mit Schwefelliganden, LXIX* and X-Ray Structure Analyses  
 Abstract    Chrom-und Wolfram-Nitrosyl-Komplexe mit schwefeldominierten Koordinationssphären: IC r(N O)XS4')]v (x = 1, y = 2; x = 2, y = 1), (NR4)2[W (NO)2(S 2)2] (R = M e, /i-Bu), [W(L)(NO)('S4)] (L = NO , N P M e3, NPEt3) und [//-0 { W (N 0)(S4)} 2] ('S2'2" = l,2-Benzoldithiolat(2-); 'S4'2-= l,2-Bis(2-mercaptophenylthio)ethan(2-)); Synthesen, Eigenschaften und Röntgenstrukturanalysen Transition M etal Complexes with Sulfur Ligands, LXIX* Chromium and Tungsten Nitrosyl Complexes with Sulfur Dom inated C oordination Spheres: [C r(N O)/S 4')]v(* = \ , y = 2 \x = 2 , y = 1), (N R 4)2[W(NO)2('S2')2] (R = Me, «-Bu), [W(L)(NO)('S4')] (L = NO, N PM e3, N P E t3) and [//-0{W (N 0)('s7)}2] ('S2'2-= 1.2-B enzenedithiolate(2-);'S4'2-= 1.2-Bis(2-mercaptophenylthio)ethane(2-)); Syntheses, Properties In order to study the properties o f sulfur coordinated metal centres, the chromium and tung­ sten complexes [Cr(NO)(//-'S4% (4), (N R 4),[W (N O)2('S 0 2] (1) (R = Me (la), «-Bu (lb)), [W (NO)2('S4')] (2), [^ -0 {W (N 0)('S 4')}2] (3) and [W (N PR 3)(N O)('S4')] (5) (R = Me (5a), Et (5b)) were synthesized ('S2'2 = 1,2-benzenedithiolate(2—) ; 'S4'2 = 1,2-bis(2-mercaptophenyl-th io)ethane(2-)). la and lb result from the reductive nitrosylation o f Li2[W('S2')3] which was prepared by reduction o f [W('S2')3] with rc-BuLi. la was also obtained from [W (NO)2(Cl)2]", 'S2'2-and N M e4+. Alkylation o f la or lb by 1.2-dibromoethane yields 2, whose X-ray structure 
  Reference    Z. Naturforsch. 46b, 1435—5 (1991); eingegangen am 8. A pril/ 8. Juli 1991 
  Published    1991 
  Keywords    Chromium, Tungsten, Nitrosyl Complexes, Sulfur Ligands, X-Ray 
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 TEI-XML for    default:Reihe_B/46/ZNB-1991-46b-1435.pdf 
 Identifier    ZNB-1991-46b-1435 
 Volume    46 
5Author    Dieter Sellmann, Peter Lechner, Falk Knoch, M. Atthias, MollRequires cookie*
 Title    Übergangsmetallkomplexe mit Schwefelliganden  
 Abstract    , LXXIII. Diastereospezifische Dichlormethylierung schwefelreicher IRu'^SRR XPPh^yS/j-Komplexe (SRR' = einzähniger Thioether-oder Thiol-Ligand; 'S4'2-= l,2-Bis(2-mercaptophenylthio)ethan(2-))* Transition Metal Complexes with Sulfur Ligands, LXXIII. Diastereospecific Dichlorom ethylation of Sulfur Rich [Run(SR R')(PPh3)'S4'] Complexes (SR R' = M onodentate Thioether or Thiol Ligand; 'S4': ~ = 1,2-Bis(2-m ercaptophenylthio)ethane(2-)) Under exclusion o f air the thioether and thiol complexes [Ru(SRR')(PPh3)'S4'] ('S4'2-= l,2-bis(2-m ercaptophenylthio)ethane (2 -)) easily react with C H C l, yielding [Ru(Cl)(PPh,)('S4'-C H C L)] in which one thiolato atom o f the 'S4' ligand is diastereospecifical-ly dichloromethylated. In the presence o f air, however, [Rum(Cl)(PPh3)'S4'] is formed. The molecular structures o f [Ru(Cl)(PPh3)('S4'-C H C l:)]-2C H C l3 and [Rum(Cl)(PPh3)'buS4'] have been determined by X-ray crystallography. 'buS4'2-(= 1,2-bis(3,5-di(/-butyl)-2-m ercaptophenylthio)ethane(2-)) is the r-butyl derivative o f the 'S4' ligand. Reasons for ob ­ served diastereospecifity o f alkylation are discussed. 
  Reference    Z. Naturforsch. 46b, 1585 (1991); eingegangen am 3. Mai 1991 
  Published    1991 
  Keywords    Transition Metal Sulfur Complexes, Diastereospecifity, Alkylation, X-Ray 
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 TEI-XML for    default:Reihe_B/46/ZNB-1991-46b-1585.pdf 
 Identifier    ZNB-1991-46b-1585 
 Volume    46 
6Author    Dieter Sellmann, Stefan Fünfgelder, Falk KnochRequires cookie*
 Title    Übergangsmetallkomplexe mit Schwefelliganden, LXXV  
 Abstract    Synthese und Struktur von INi('NHS4)|2 und |N i(Py)2('S2')| * Py; Radikalische Templatalkylierungen von |Ni('S2')2l2~** Transition Metal Complexes with Sulfur Ligands, LXXV* Syntheses and Structure of [Ni('NHS4')]2 and [Ni(Py)2('S2')] • Py; Radical Alkylations of [Ni('S2')2]: ** [N i('N HS4')]2 ('N nS4'2~ = 2,2'-bis(2-m ercaptophenylthio)diethylam ine(2-)) was synthesized from Ni(ac)-, and N a2-' N HS4' and characterized by X-ray structure analysis. In the solid state [N i('N HS4')]2 contains two pseudooctahedral [N i('N HS4')] fragments bridged via thiolate d o ­ nors, in D M F solution at 110 C it dissociates into mononuclear entities. The product o f the template reaction between [Ni('S2')2]2~ ('S2'2-= 1,2-benzenedithiolate) and (BrC\H4)2NH was shown to contain an as yet unidentified by-product in addition to [Ni('NnS4')]2. Pure [N i('N HS4')]2 does not react with pyridine, but the template product forms [N i(Py)2('S2')] which has a square planar coordination geometry with the pyridine rings perpendicular to the N iS2N 2 plane. Investigation o f the template formation o f [N i('N HS4')]2 provided evidence that the reaction o f [Ni('S,')J--with (BrC2H4)^NH involves radicals, suggesting a radical chain reaction m echa­ nism. 
  Reference    Z. Naturforsch. 46b, 1593—1600 (1991); eingegangen am 13. Mai 1991 
  Published    1991 
  Keywords    Nickel Sulfur Complexes, X -Ray, Template Reaction 
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 TEI-XML for    default:Reihe_B/46/ZNB-1991-46b-1593.pdf 
 Identifier    ZNB-1991-46b-1593 
 Volume    46 
7Author    N. Orbert, K. Uhna, Michael Schulten3, Roland Boeseb, Dieter BläserbRequires cookie*
 Title    Synthese und Struktur von l,3?6,8-Tetra-terf-butylcarbazol  
 Abstract    The synthesis o f 1,3,6,8-tetra-/er/-butylcarbazole (2) by the reaction o f carbazole with tert-butyl chloride in the presence o f aluminium chloride is reported. The X-ray structures o f 2 and its diethyl ether adduct are compared. The gap formed by the ter/-butyl groups in 1,8-position has been calculated and compared with that o f the supermesithyl substituent. 
  Reference    Z. Naturforsch. 46b, 1503—1508 (1991); eingegangen am 4. April 1991 
  Published    1991 
  Keywords    l, 3, 6, 8-Tetra-?m -butylcarbazole, Synthesis, X-Ray 
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 TEI-XML for    default:Reihe_B/46/ZNB-1991-46b-1503.pdf 
 Identifier    ZNB-1991-46b-1503 
 Volume    46 
8Author    Dieter Sellmann, Stefan Fünfgelder, Falk Knoch, M. Atthias, MollRequires cookie*
 Title    Übergangsmetallkomplexe mit Schwefelliganden, LXXVI* Redox-und Additionsreaktionen von Nickelkomplexen mehrzähniger Thioether-Thiolat-Liganden. Röntgenstrukturanalysen von (N M e4)2 [Ni('S2')2 l und INi('S4-C 3 /)(PM e3)]** Transition M etal Complexes with Sulfur Ligands, LXXVI* Redox and Addition Reactions of Nickel Complexes with M ultidentate Thioether-Thiolato Ligands. X-Ray Structure Determinations of (N M e ^ fN ^ 'S ^ j] and [Ni('S4-C 3')(PM e3)]*  
 Abstract    In order to elucidate specific properties o f nickel sulfur com plexes, redox and addition-elim-ination reactions o f [Ni('OS4')]2, [N i('N HS4')]2, [Ni('S5')], [Ni('S4-C 5')]2 and [Ni('S4-C 3')] were investigated ('OS4'2-= 2,2'-bis(2-m ercaptophenylthio)diethylether(2-), 'N HS4'2~ = 2,2'-bis(2-m ercaptophenylthio)diethylam ine(2-), 'S5'2-= 2,2'-bis(2-mercaptophenylthio)diethylsul-fid e (2 -), 'S4-C 5'2-= 1,5-bis(2-m ercaptophenylthio)pentane(2-), 'S4-C 3'2-= l,3-bis(2-m er-captophenylthio)propane(2-)). Cyclovoltammetry proves the complexes to be redox inactive between -1 .4 and +0.8 V vs. N H E. A bove +0.8 V the complexes are irreversibly oxidized, below -1 , 4 V desalkylation takes place and [Ni('S2')2]2" is formed. An X-ray structure analysis was carried out o f (N M e4)2[Ni('S2'):>], which shows a planar anion with the Ni center in a nearly perfect square planar coordination. Distances and angles are practically identical to those in the [Ni('S2')2] m onoanion. The complexes coordinate only phosphines as coligands, but thioether donors simulta­ neously decoordinate and, dependant o f reaction temperature, m ono-or trisphosphine com ­ plexes are formed. [Ni('S4-C 3')(PM e3)] was characterized by X-ray structure analysis and ex­ hibits a square pyramidal coordination geometry. 
  Reference    Z. Naturforsch. 46b, 1601—1608 (1991); eingegangen am 13. Mai 1991 
  Published    1991 
  Keywords    Nickel Sulfur Complexes, Redox and Addition Reactions, X-Ray 
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 Identifier    ZNB-1991-46b-1601 
 Volume    46 
9Author    Pilar Souza, Luisa Sanz, Vicente Fernández, Agueda Arquero, Enrique Gutierrez, AngelesM. OngeRequires cookie*
 Title    Complexes of Zn, Cd and Hg Halides with S and N Polydentate Schiff-Base. Metal Template Effect in the Synthesis o f Analogous Oxygenated Base. Crystal Structure of [Zn(btsc)2Cl2l and [Cd(btsc)2Br2] M ontegancedo s/n, E-28660-Boadilla del M onte (Madrid), Spain  
 Abstract    Zinc, cadmiun and mercury dihalide react with 4-acetylpyridinthiosemicarbazone (4-aptsc) to give complexes with 1:1 and 2:1 ligand/m etal stoichiom etric ratios. These metals are effec­ tive templates for the Schiff-base condensation o f 4-acetylpyridine with semicarbazide to give the complexes [M (4-apsc)XJ and [M (4-apsc)2X 2] where M = Zn, Cd or Hg and X = Cl, Br or I. These com pounds were characterized by elemental analyses, conductivities measurements, IR and l3C, 'H N M R spectra. The zinc chloride and bromide com plexes o f benzalthiosem icarbazone (btsc) have been pre­ pared and characterized by X-ray measurements. The com pounds Zn(btsc)2Cl2 and Cd(btsc)2Br2 are isostructural and crystallize in the space group P 2j/«. The crystal structure o f the chlorine derivative has been resolved by single-crystal X-ray diffraction. The zinc centre is in a slightly distorted tetrahedral environment. There are intra and intermolecular hydrogen bonds. 
  Reference    Z. Naturforsch. 46b, 767 (1991); received June 27/O ctob er 22 1990 
  Published    1991 
  Keywords    4-Acetylpyridinthiosemicarbazone, 4-Acetylpyridinsemicarbazone, Benzalthiosemicarbazone, II-b-Metal Complexes, Crystal Structure, X -Ray 
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 Identifier    ZNB-1991-46b-0767 
 Volume    46 
10Author    Ulrike Holzgrabe, Willy Friedrichsen, Rl-FH. EsseRequires cookie*
 Title    Keto-Enol-Tautomerism and Configurational Isomerism of 2,6-Disubstituted 4-Piperidone-3,5-dicarboxylates [1]  
 Abstract    The dialkyl 2,6-dialkylsubstituted 4-piperidone-3,5-dicarboxylates were synthesized by a M annich procedure. Depending on the substitution at the nitrogen keto-enol-tautomerism and a configurational isomerism at C 2 is observed. The structure o f the N-substituted piperi-done 24 E (C 18H 29N 0 5) has been determined by X-ray analysis: it is characterized by an enol structure o f the /?-ketoester and an axial position o f the alkyl group at C 2 and an equatorial one o f the alkyl group at C 6. The O -H -O hydrogen bond shows characteristic values o f a strong hydrogen bond. The N-unsubstituted piperidones adopt a ketone structure with the all-equatorial position o f all substituents. This stereochemistry is confirmed for other enolic and ketone analogues by N M R spectroscopic methods. To work out the reason for the different thermodynamic stabilities o f the different stereochemical structures o f N-substituted and N-unsubstituted piperidones, various semiempirical calculations were done for series o f simple pairs o f carbonyl/enol tautomers, substituted acetoacetates, oxoglutarate as well as o f syste­ matically varied substituted cyclohexanone, 4-oxacyclohexanone and 4-piperidone deriva­ tives. 
  Reference    Z. Naturforsch. 46b, 1237—1250 (1991); received Novem ber 2 1990 
  Published    1991 
  Keywords    2, 6-Disubstituted 4-Piperidone-3, 5-dicarboxylates, High-resolution N M R, X-Ray, Theoretical Calculations 
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 TEI-XML for    default:Reihe_B/46/ZNB-1991-46b-1237.pdf 
 Identifier    ZNB-1991-46b-1237 
 Volume    46 
11Author    R. Benn, P. Betz, R. G. Oddard, P. W. Jolly, N. Kokel, C. Krüger, I. TopalovićRequires cookie*
 Title    Intermediates in the Palladium-Catalyzed Reaction of 1,3-Dienes, Part 6 [1] A Solid-State NM R Spectroscopic Investigation of Butadiene Complexes of Nickel, Palladium and Platinum  
 Abstract    The structure of the (l,3-butadiene)M (R2PC 2H 4P R 2) com pounds (M = Ni, Pd, Pt; R = Pr', Bu', Cy) in the solid-state have been investigated by 13C and 31P CP/MAS N M R spectroscopy. The bonding mode adopted by the diene is dependent upon the nature o f the metal: the palla­ dium com pounds contain an ^2-diene molecule, the nickel compound where R is cyclohexyl contains an ^4-diene molecule whereas the PKPC2H4PPH-stabilized platinum compound con­ tains a platinacyclopentene ring. The crystal structures of (//2-l,3-C4H6)Pd(Cy2PC2H4PCy2) and (/74-l,3-C4H 6)Ni(Cy2PC2H 4PCy2) have been confirmed by X-ray diffraction. 
  Reference    Z. Naturforsch. 46b, 1395—1405 (1991); received M arch 28 1991 
  Published    1991 
  Keywords    Palladium-Organo Complex, Nickel-Organo Complex, Platinum-Organo Complex, Butadiene Complex, X-Ray 
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 TEI-XML for    default:Reihe_B/46/ZNB-1991-46b-1395.pdf 
 Identifier    ZNB-1991-46b-1395 
 Volume    46