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1983 (307)
181Author    Dietmar SchomburgRequires 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 
182Author    CorneliusG. Kreiter, Ulrich KoemmRequires 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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 TEI-XML for    default:Reihe_B/38/ZNB-1983-38b-0943.pdf 
 Identifier    ZNB-1983-38b-0943 
 Volume    38 
183Author    Michael Hesse, Uwe Klingebiel, Jürgen Heinze, John MortensenRequires 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 
184Author    Marianne Baudler, Thomas PontzenRequires 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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 TEI-XML for    default:Reihe_B/38/ZNB-1983-38b-0955.pdf 
 Identifier    ZNB-1983-38b-0955 
 Volume    38 
185Author    Dieter Sellmann+, Günther Lanzrath, Gottfried Huttner, Laszlo Zsolnai, Carl Krüger, K. H. ClausRequires 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 
186Author    W. S. SheldrickRequires 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 
187Author    Hans-Dietrich Stachel, Hermann Poschenrieder, Bruno WiesendRequires 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 
188Author    Hans ZimmerRequires 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 
189Author    Alicia Baldessari, EduardoG. GrosRequires 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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 TEI-XML for    default:Reihe_B/38/ZNB-1983-38b-0997.pdf 
 Identifier    ZNB-1983-38b-0997 
 Volume    38 
190Author    Franz Dallaeker, Johannes Jacobs, Wim CoerverRequires 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 
191Author    Detlef GeffkenRequires 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 
192Author    A. Marston, E. HeckerRequires 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 
193Author    Anders Ljungqvist, Karl FolkersRequires 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 
194Author    Walter Tötsch, Fritz SladkyRequires 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 
195Author    HansH. KarschRequires 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 
196Author    Bernhard Czeska, Kurt Dehnicke, Dieter FenskeRequires 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 
197Author    JeanE. Rockley, LindsayA. SummersRequires 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 
198Author    Ernst-Dieter FranzRequires 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 
199Author    Ali Mahan, Albrecht MewisRequires 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 
200Author    Alfred Koblischek, Hans-Dieter Hausen, Johann Weidlein, Herbert BinderRequires 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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