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Facet section ZfN Section B:Volume 038 [X]

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181	Author	Dietmar Schomburg	Requires cookie*
	Title	Strukturchemie von Verbindungen des penta-koordinierten Siliciums. Quadratisch-pyramidale Geometrie i m Bis (tetramethylethylendioxy)fluorsilan -Anion Structural Chemistry of Penta-coordinated Silicon. Square-Pyramidal Geometry in the Bis(tetramethylethylenedioxy)fluorosilane Anion
	Abstract	The geometry around the penta-coordinated silicon atoms in the two crystallographically independent molecules in tetramethylammonium-bis(tetramethylethylenedioxy)fluoro-silane dichloromethane solvate is distorted from the trigonal bipyramid towards the square pyramid by 69.1 % and 52.3%, resp. [N(CH3)4]+[FSi(0C(CH3)2C(CH3)20)2]- • CH2C12 crystal-lizes in the monoclinic space group P2x/n, Z = 8 with a = 20.926(6), b= 15.117(1), c — 17.008(4) A,ß= 114.88(2)°. The structure was refined to R = 0.084 using 2203 independent reflections.
	Reference	Z. Naturforsch. 38b, 938—942 (1983); eingegangen am 28. März 1983
	Published	1983
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	Identifier	ZNB-1983-38b-0938
	Volume	38

182	Author	CorneliusG. Kreiter, Ulrich Koemm	Requires cookie*
	Title	Gehinderte Ligandbewegungen in Übergangsmetallkomplexen, XIX [1] Oktaedrische Wolfram-Olefin-Komplexe mit Bisphospbinoethan-Liganden Hindered Ligand Motions in Transition Metal Complexes, XIX [I] Octahedral Tungsten Olefin Complexes with Bisphosphinoethane Ligands
	Abstract	(OC-6-32)-W(CO)3[(CH3)2PC2H4P(CH3)2](olefin) complexes (9-14) were prepared photochemicallyfromW(CO)4[(CH3)2PC2H4P(CH3)2](l)viaW(CO)3[(CH3)2PC2H4P(CH3)2]-(THF) (2) and the electron poor olefins dimethyl malonate(3), fumarate (4), methylfuma-rate (5), fiuorofumarate (6), chlorofumarate (7) and bromofumarate (8). The stereoche-mistry of 9-14 was elucidated by IR and NMR spectroscopy. The hindered rotations of the olefin ligands in 9-14 were studied by D-NMR spectroscopy. 11-14 form two diastereomeric isomers when the olefin rotation is freezed. The spectroscopic behaviour of the dimethyl fumarate complex 10 gives unambiguous proof for the rotation of the olefin ligand around the metal-olefin-bond. Alternative motions are ruled out.
	Reference	Z. Naturforsch. 38b, 943—952 (1983); eingegangen am 7. Februar/15. März 1983
	Published	1983
	Keywords	Olefin Complexes, Synthesis, Ligand Rotations
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	Identifier	ZNB-1983-38b-0943
	Volume	38

183	Author	Michael Hesse, Uwe Klingebiel, Jürgen Heinze, John Mortensen	Requires cookie*
	Title	Oxidation of 4-Lithium-diazasilacyclopentene with Transition Metal Halides
	Abstract	4-Lithium-3,3,5-trimethyl-2-ter^-butyl-l,2-diaza-3-sila-5-cyclopentene is oxidized in the reaction with transition metal halides and subsequently dimerizes. Oxidation potentials are given and a reaction mechanism is proposed.
	Reference	Z. Naturforsch. 38b, 953—954 (1983); eingegangen am 2. Mai 1983
	Published	1983
	Keywords	Diazasilacyclopentene, Oxidation Potential, Dimerisation
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	Identifier	ZNB-1983-38b-0953
	Volume	38

184	Author	Marianne Baudler, Thomas Pontzen	Requires cookie*
	Title	Beiträge zur Chemie des Phosphors, 132 [1] 31 P-Kernresonanzspektrum und Struktur von Trimethyl-heptaphosphan(3), P7Me3 Contributions to the Chemistry of Phosphorus, 132 [1] 31 P NMR Spectrum and Structure of Trimethylheptaphosphane(3), IVMe3
	Abstract	Trimethy lheptaphosphane (3), 3,5,7 -Triorganotricyclo [ 2.2.1.0 2 -6 ] heptaphosphanes, Polycyclic Phosphanes, 31 P NMR Spectroscopy
	Reference	Z. Naturforsch. 38b, 955—960 (1983); eingegangen am 19. Mai 1983
	Published	1983
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	Identifier	ZNB-1983-38b-0955
	Volume	38

185	Author	Dieter Sellmann+, Günther Lanzrath, Gottfried Huttner, Laszlo Zsolnai, Carl Krüger, K. H. Claus	Requires cookie*
	Title	Übergangsmetall-Komplexe mit Schwefelliganden, V* Synthese, Reaktivität und Struktur von Carbonyl-, Phosphin-und Hydrazin- Eisen(II)-Komplexen mit zwei-und vierzähnigen Schwefelliganden Transition Metal Complexes with Sulfur Ligands, V* Synthesis, Reactivity and Structure of Carbonyl-, Phosphine-, and Hvdrazin-Iron(II) Complexes with Two-and Fourdentate Sulfur Ligands
	Abstract	Iron(II) Sulfur Complexes, Synthesis, Reactions, X-Ray Reaction of FeCl2 • 4 H20 with dttd 2 -, the dianion of 2,3,8,9-dibenzo-l,4,7,10-tetra-thiadecane, leads to the solvated [Fe(dttd)], which coordinates CO, PMe3 and N2H4 yielding [Fe(CO)2dttd], [Fe(PMe3)2dttd], [Fe(CO)PMe3(dttd)], [Fe(N2H4)2dttd] and [Fe(N2H4)CO(dttd)], respectively. With H2S and [Fe(dttd)] the Fe(III) complex (PPN)2[Fe2(S)2(dttd)2] is obtained. PPh3 cannot be coordinated to [Fe(dttd)], whereas the reaction between [Fe(PPh3)(CO)3I2] and LiSC6H4SCH3 yields [Fe(PPh3)CO(CH3SC6H4S)2] besides the major product [Fe(CO)2(CH3SC6H4S)2]-A PPh3 complex can be obtained also with o-benzenedithiolate, CeH4S2 2-: Reacting [Fe(PPh3)(CO)3I2] with Li2S2CeH4 yields the binuclear [Fe(PPh3)(CO)2C6H4S2]2. Oxidation of [Fe(N2H4)CO(dttd)] by various agents leads to [Fe(CO)dttd]2 without evidence of formation of a N2 complex intermediate. Nucleophilic attack of [Fe(CO)2(CH3SCeH4S)2] by lithium organyls as e.g. LiPh leads to the benzoylato complex [Li(THF)3][Fe(CO)(PhCO)(CH3SC6H4S)2]; the structures of the starting complex as well as of the adduct have been elucidated by X-ray structure determination. Nucleophilic attack of the corresponding [Fe(CO)2dttd] by LiPh occurs reversibly at the Fe center; by cleavage of a Fe-S bond [Fe(Ph)(CO)2dttd']" is formed, where dttd' is acting as a tridentate ligand. This result shows how the reactions of formally equivalent complexes like [Fe(CO)2(CH3SCeH4S)2] and [Fe(CO)2dttd] depend strongly upon the denticity of the sulfur ligands. The dependance upon the character of the nucleophilic agent is shown by the reaction of [Fe(CO)2dttd] with Li[BEt3H]; in this case again a CO ligand is attacked reversibly yielding the formyl complex [LiBEt3][Fe(HCO)CO(dttd)J, the structure of which could be elucidated so far only spectroscopically as well as by elemental analysis. [Fe(Ph)(CO)2dttd']-forms salts like e.g. (AsPh4)[Fe(Ph)(CO)2dttd]; in solution they slowly loose CO yielding e.g. binuclear (AsPh4)2[Fe(Ph)dttd]2. Attempts to isolate the anion as [Li(TMED)2]+ salt lead to the loss of CO as well as of phenyl ligands yielding the paramagnetic [Fe(TMED)dttd], which is also obtained directly from [Fe(dttd)] and TMED. The phenyl complex [Fe(Ph)dttd]2 2 -is also formed by reaction of [Fe(dttd)] with LiPh; on reaction with dimethyl-formamide it yields [Fe(DMF)dttd]2. A series of the above described compounds has been investigated by Mößbauer spectroscopy.
	Reference	Z. Naturforsch. 38b, 961—981 (1983); eingegangen am 4. Mai 1983
	Published	1983
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	Identifier	ZNB-1983-38b-0961
	Volume	38

186	Author	W. S. Sheldrick	Requires cookie*
	Title	Preparation and Structures of Ternary Copper(II) Complexes of Purine 3',5'-Cyclic Nucleotides [1]
	Abstract	Copper(II Ternary Complexes, X-Ray Ternary copper(II) complexes of 3',5'-cIMP and 3',5'-cGMP with o-phenanthroline have been isolated from aqueous solution at respective pH values of 2.8 and 5.8. Their structures have been established by single crystal X-ray diffraction. The copper atom in [Cu(3',5'-cIMP)(phen)(H20)a][N03].2H20 (1) binds N(7) of the hypoxanthine base and displays a square pyramidal coordination. [Cu(phen)2(H20)] 2+ and 3',5'-cGMP form a 1 : 2 intercalation complex [Cu(phen)2(H20)][3',5'-cGMP]2 • 9H2O (2) in which direct metal-nucleotide binding is absent.
	Reference	Z. Naturforsch. 38b, 982—987 (1983); received March 15 1983
	Published	1983
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	Identifier	ZNB-1983-38b-0982
	Volume	38

187	Author	Hans-Dietrich Stachel, Hermann Poschenrieder, Bruno Wiesend	Requires cookie*
	Title	Ein einfaches Verfahren zur Herstellung der labilen Stereoisomeren von 5-Benzyliden-pyrrolin-2-onen A Simple Procedure to Prepare the Labile Stereoisomers of 5-Benzylidenepyrrolin-2-ones
	Abstract	5-Benzylidenepyrrolin-2-ones, 5-Benzylidenetetramic Acids, cis-trans Isomerisation The known Z-isomers of some N-unsubstituted 5-benzylidenepyrrolin-2-ones (2, 10, 12) change the configuration upon heating with oxalylchloride. Methanolysis of the inter-mediate imides (6, 8, 9) yields the corresponding E-isomers.
	Reference	Z. Naturforsch. 38b, 988—991 (1983); eingegangen am 5. April 1983
	Published	1983
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	Identifier	ZNB-1983-38b-0988
	Volume	38

188	Author	Hans Zimmer	Requires cookie*
	Title	Adel Amer* [3], Montserrat Ventura [4]
	Abstract	3-(l-Halo-2-oxo-2-substitutedethyl)-2(lH)quinoxalinones, Furo[2,3-b]quinoxalines An efficient method for the synthesis of furo[2,3-b]quinoxalines has been devised. Thus, 3-halo-2-arylfuro[2,3-b]quinoxalines, 5a-5c were synthesized by the action of conc. H2SO4 on 3-(l-halo-2-oxo-2-arylethyl)-2(lH)quinoxalinones, 3b, 3c and 3f respectively. When 3-(1 -halo-2-oxo-2-substitutedethyl)-2(1H)quinoxalinones 3d and 3e (substituent = «-butyl, ethoxy) were utilized in this reaction 3-halomethylene-2(lH)quinoxalinone 6 a and 6b were obtained in high yield.
	Reference	Z. Naturforsch. 38b, 992—996 (1983); eingegangen am 14. April 1983
	Published	1983
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	Identifier	ZNB-1983-38b-0992
	Volume	38

189	Author	Alicia Baldessari, EduardoG. Gros	Requires cookie*
	Title	Synthesis of Some N-Alkylamino-N-vanillylpropionamides
	Reference	Z. Naturforsch. 38b, 997—999 (1983); received April 11 1983
	Published	1983
	Keywords	N-Alkylamino-N-vanillylpropionamides, Synthesis, X H NMR Spectra, 13 C NMR Spectra
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	Identifier	ZNB-1983-38b-0997
	Volume	38

190	Author	Franz Dallaeker, Johannes Jacobs, Wim Coerver	Requires cookie*
	Title	Über Naphtho[1.8-de]-1.3-dioxiiie Naphtho[l ,8-de]-1,3-dioxines
	Abstract	6-Brom-naphtho[l,8-de]-l,3-dioxine, 6-Nitro-naphtho[l,8-de]-l,3-dioxine, 4-Methyl-naphtho[l,8-de;4,5-d'e']bis-l,3-dioxine-9-carboxylic Acid Treatment of 1,8-Dihydroxy-naphthaline with bromochloromethane/K3C03 in DMF gives Naphtho[l,8-de]-l,3-dioxine (la) in good yield. The bromo (lb) and nitro compound (lc) can be obtained free of isomerics by electrophilic substitution of la. Bromolithium exchange of lb leads to a lithium organic compound, which possibles the synthesis of alkyl-, olefinic-, and carboxylic derivatives of the substrate la. In a similar way the treatment of 2,3-dihydroxynaphthazarin with chlorobromo-methane/K2C03 gives the naphtho[l,8-de;4,5-d'e']-bis-l,3-dioxine (3a). The substrate 3a can be subjected to electrophilic aromatic substitutions.
	Reference	Z. Naturforsch. 38b, 1000—1007 (1983); eingegangen am 11. April/9. Juni 1983
	Published	1983
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	Identifier	ZNB-1983-38b-1000
	Volume	38

191	Author	Detlef Geffken	Requires cookie*
	Title	3-Hydroxy-, 3-Alkoxy-und 3-Amino-2-thioxooxazolidin-4-one aus 6 -Thioxoperhydro -1.5.2-dioxazin -3 -onen 3-Hydroxy-, 3-Alkoxy-and 3-Amino-2-thioxooxazolidine-4-ones from 6-Thioxoperhydro-1,5,2-dioxazine-3-ones
	Reference	Z. Naturforsch. 38b, 1008—1014 (1983); eingegangen am 5. Mai 1983
	Published	1983
	Keywords	Glycolohydroxamic Acids, l, l'-Thiocarbonyldiimidazole, 6-Thioxoperhydro-1, 5, 2-dioxazine-3-ones, Ring Transformation
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	Identifier	ZNB-1983-38b-1008
	Volume	38

192	Author	A. Marston, E. Hecker	Requires cookie*
	Title	Structure-Activity Relationships of Polyfunctional Diterpenes of the Tigliane Type, V* Preparation and Irritant Activities of Amino Acid and Peptide Esters of Phorbol
	Abstract	The synthesis of a series of 12-O-amino acyl-and 12-0-peptidyl-13-acetate and -13,20-diacetate esters of the tetracyclic diterpene alcohol phorbol is described. These esters, which include amino acid moieties with both N-protected and free amino functions, were all tested for irritant activity on mouse ear. The highest activities were observed for esters with N-9-fluorenylmethyloxycarbonyl-protected leucine and 11-aminoundecanoic acid.
	Reference	Z. Naturforsch. 38b, 1015—1021 (1983); received March 28 1983
	Published	1983
	Keywords	Amino Acids, Peptides, Phorbol Esters, Irritants, Tumour Promoters
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	Identifier	ZNB-1983-38b-1015
	Volume	38

193	Author	Anders Ljungqvist, Karl Folkers	Requires cookie*
	Title	Study of Hydrogenolytic Cleavage of Peptide-Resin Benzyl Ester Bonds for Synthesis of Protected Fragments of the Human Leukocyte Interferon
	Abstract	Three Boc-protected fragments of the human leukocyte interferon, LeIFA, have been synthesized: I, BOC LeIFA (99-105) (BOC-Val-Ile-Gln-Gly-Val-Gly-Val); II, BOC LeIFA (116-119) (BOC-Ile-Leu-Ala-Val); III, BOC LeIFA (123-126) (BOC-Phe-Gln-Arg(Tos)-Ile). The presence of the Boc-group was desired so that these peptides could serve as intermediates in fragment condensation toward larger segments of interferon. To achieve these intermediates, a study was desirable on three methods of cleavage of the benzyl ester-polymer bonds. It was found that hydrogenolysis with hydrogen and palla-dium generated in situ was distinctly superior to transfer hydrogenation with ammonium formate or cyclohexene. An effective swelling of the peptide-resin to allow penetration of palladium acetate into the matrix and mobility of the peptide chains on the resin to expose the benzyl ester bond to hydrogenolysis appear to be essential conditions for the best cleavage.
	Reference	Z. Naturforsch. 38b, 1022—1024 (1983); received May 2 1983
	Published	1983
	Keywords	Interferon, Peptide Synthesis, Hydrogenation, Palladium Black, Conformation
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	Identifier	ZNB-1983-38b-1022
	Volume	38

194	Author	Walter Tötsch, Fritz Sladky	Requires cookie*
	Title	The Hydrolysis of TeF6
	Abstract	The stereochemistry of the hydrolysis of tellurium hexafluoride has been followed up by 125 Te NMR spectroscopy for each individual step of replacement of fluorine by a hydroxy group.
	Reference	Z. Naturforsch. 38b, 1025—1026 (1983); eingegangen am 18. März 1983
	Published	1983
	Keywords	Tellurium Hexafluoride, Hydrolysis, Stereochemistry, 125 Te NMR Spectra
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	Identifier	ZNB-1983-38b-1025_n
	Volume	38

195	Author	HansH. Karsch	Requires cookie*
	Title	Alkyl Substituted Diphosphinomethanes: Mixed Cl/«-Bu and Me/CH2SiMe3 Derivatives [1]
	Abstract	The syntheses of (£-Bu)2PCH2P(£-Bu)2 and (PhO)2PCH2P(Oph)2 and an improvement of the synthesis of Me2PCH2PMe2 are described. Mixed Me/CH2SiMe3 and Cl/i-Bu diphosphinomethane derivatives are characterized by means of NMR spectroscopy.
	Reference	Z. Naturforsch. 38b, 1027—1030 (1983); eingegangen am 25. April 1983
	Published	1983
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	Identifier	ZNB-1983-38b-1027_n
	Volume	38

196	Author	Bernhard Czeska, Kurt Dehnicke, Dieter Fenske	Requires cookie*
	Title	PPh3Me[Os(NO)Cl4]; a Penta Coordinate Osmium Nitrosyl Complex
	Abstract	Preparation, IR-Spectrum, X-Ray, Methyltri-phenylphosphonium-nitrosyltetrachloroosmate PPh3Me[Os(NO)Cl4] is prepared by the reac-tion of (NO)2[Os(NO)Cl5] with methyltriphenyl-phosphonium chloride in CH2CI2 solution. The complex forms brown, air stable crystals, which are characterized by the IR spectrum as well as by an X-ray structure determination (space group Pi, two formula units per unit cell, a = 906, b = 1172, c = 1198 pm, a = 76.4, ß = 84.8, y = 82.4°, 3254 independent reflexi-ons, i?w — 8.6%). The structure consists of [P(C6H5)3CH3]® ' cations and disordered [Os-(NO)C14] g anions; the latter have approximate C4v symmetry with a linearly coordinated nitrosyl ligand in the axial position.
	Reference	Z. Naturforsch. 38b, 1031—1033 (1983); eingegangen am 5. April 1983
	Published	1983
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	Identifier	ZNB-1983-38b-1031_n
	Volume	38

197	Author	JeanE. Rockley, LindsayA. Summers	Requires cookie*
	Title
	Abstract	Diquaternary Salt of 4,4'-Oxybispyridine, Polarography The diquaternary salt of 4,4'-oxybispyridine, l,l'-dimethyl-4,4'-oxybispyridinediium bis-(fluorosulfonate), is reduced polarographically by a one electron transfer not involving hydro-gen to an unstable radical cation at a potential (E0) of —0.80 V in the pH range 5.1-10.4.
	Reference	Z. Naturforsch. 38b, 1034 (1983); received April 6 1983
	Published	1983
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	Identifier	ZNB-1983-38b-1034_n
	Volume	38

198	Author	Ernst-Dieter Franz	Requires cookie*
	Title	Fluorapatit Ca5F(P04)3 - Ein Modell zur Synthese der Zahnhartsubstanz im System CaF2-Ca3(P04)2 Fluorapatite -A Model for the Synthesis of Dental Enamel in the System CaF2-Ca3(P04)2
	Abstract	Fluorapatite Ca5F(PC>4)3 can be synthesized by melting of CaF2 together with Ca3(P04)2 at 1660 °C in the molar ratio CaF2 • 3 Ca3(PÜ4)2. Fluorapatite is more resistant against acids than hydroxylapatite Cas0H(P04)3 and can activate the remineralisation in dental enamel. The apatite of dental enamel is more resistant against mechanical stress than synthetic apatite due to a different microstructure of the crystal grains.
	Reference	Z. Naturforsch. 38b, 1037—1040 (1983); eingegangen am 25. Mai 1983
	Published	1983
	Keywords	Fluorapatite, Hydroxylapatite, Dental Enamel, Synthesis, Phase Equilibria
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	Identifier	ZNB-1983-38b-1037
	Volume	38

199	Author	Ali Mahan, Albrecht Mewis	Requires cookie*
	Title	A B2X2 -Verbindungen mit CaAl2Si2-Struktur, IX [1] Compounds with the CaAl2Si2 Structure, IX [1]
	Abstract	The compounds ZrCu2P2, YZnCuP2, LaZnCuP2, and CeZnCuP2 have been prepared and their structures have been determined. They are isotypic and crystallize trigonally in the CaAl2Si2-type structure (space group P3m 1) with the lattice constants: ZrCu2P2 a = 381,2(1) pm, c = 617,1(2) pm, YZnCuP2 a = 398,3(1) pm, c = 652,3(2) pm, LaZnCuP2 a = 408,2(1) pm, c = 674,2(2) pm, CeZnCuP2 a = 406,4(1) pm, c = 669,7(2) pm.
	Reference	Z. Naturforsch. 38b, 1041—1045 (1983); eingegangen am 13. Mai 1983
	Published	1983
	Keywords	Ternary and Quaternary Phosphides, Copper, Zinc, Crystal Structure
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	Identifier	ZNB-1983-38b-1041
	Volume	38

200	Author	Alfred Koblischek, Hans-Dieter Hausen, Johann Weidlein, Herbert Binder	Requires cookie*
	Title	Tetrathio -spiro -phosphonia -tetrachloroborate
	Abstract	Die Struktur von 1.4.6.9-Tetrathio-5-phosphonia-spiro(4.4)nonan-tetrachloroborat Tetrathio-spiro-phosphonia Tetrachloroborates The X-Ray Crystal Structure of l,4,6,9-Tetrathio-5-phosphonia-spiro(4.4)nonan Tetrachloroborate Tetrathio-spiro-phosphonia Tetrachloroborates A series of tetrathio-spiro-phosphonia tetrachloroborates have been synthesized by the reaction of PCLj+BCLr with 1,2-ethane-, 1,2-propane-and 1,3-propane dithiole. The crystal structure of l,4,6,9-tetrathio-5-phosphonia-spiro(4,4)nonane tetrachloroborate, 3a, was determined from diffractometer data and refined to R — 0.056 for 4003 independent reflex-ions. 3a, orthorhombic, Pbcn, a = 1493.0(3), b = 1515.6(3), c = 1213.3(4) pm. The unit cell containes eight formula units.
	Reference	Z. Naturforsch. 38b, 1046—1053 (1983); eingegangen am 6. Mai 1983
	Published	1983
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	Identifier	ZNB-1983-38b-1046
	Volume	38

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