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1994 (283)
121Author    Bromo, P. Prillwitz, W. PreetzRequires cookie*
 Title    Darstellung, Schwingungsspektren und Normalkoordinatenanalyse der  
 Abstract    The IR and Raman spectra of the ten brom o-iodo-rhenates(IV) [ReBr"I6_"]2 -, n = 0 -6 , including the geometrical isomers for n -2,3,4, have been recorded at 80 K. The vibrational spectra are com pletely assigned according to point groups O h, D 4h, C4v, C3v, and C2v, as supported by normal coordinate analyses based on a general valence force field. Due to the different mms-influences Br < I in asymmetric axes B r '-R e -I ', the R e -I ' bonds are strengthened and the R e -B r ' bonds are weakened, as indicated by valence force constants, for R e -I ' on average 8,5% higher and for O s -B r ' 8,3% lower, as compared with the values calculated for symmetric I -R e -I and B r -R e -B r axes, respectively 
  Reference    Z. Naturforsch. 49b, 753—7 (1994); eingegangen am 7. März 1994 
  Published    1994 
  Keywords    -Iodo-Rhenate(IV), [ReBr, !^, ]2-, n = 0 -6 Brom o-Iodo-Rhenates(IV ), Stereoisomers, rra/is-Influence, Vibrational Spectra, Normal Coordinate Analysis 
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 Identifier    ZNB-1994-49b-0753 
 Volume    49 
122Author    MichaelW. Zenke, Karl HensenRequires cookie*
 Title    Thermodynamische Untersuchungen zur Lewis-Acidität von Trimethylchlorsilan - die Phasendiagramme und Exzeßvolumina der Systeme (CH3)3SiCl/Pyridin und (CH3)3CC1/Pyridin Thermodynamic Examinations on the Lewis Acidity of Trimethylchlorosilane - the Phase Diagrams and Excess Volumes of the Systems (C H 3)3SiCl/Pyridine and (CH3)3CC1/Pyridine  
 Abstract    The isobaric melting and boiling diagrams for the systems: trimethylchlorosilane/pyridine and trimethylchloromethane/pyridine are reproduced. Some measurements of the molar vol­ ume of mixtures between trimethylchlorosilane and pyridine and trimethylchloromethane and pyridine are reported. For both systems the molar excess volume has been calculated as a function of the mole fractions. 
  Reference    Z. Naturforsch. 49b, 759—7 (1994); eingegangen am 7. Februar 1994 
  Published    1994 
  Keywords    Phase Diagrams, Pyridine, Trimethylchlorosilane, Trimethylchloromethane, Excess Volumes 
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 Identifier    ZNB-1994-49b-0759 
 Volume    49 
123Author    M. Onika, Fritz, Johann Hiermeier, FrankH. KöhlerRequires cookie*
 Title    Fusing Nickelocene and Cyclopentadiene by Two Silyl Bridges. Synthesis and *H, 13C, and 29Si NMR Investigation of a Paramagnetic Building Block for High-Nuclear Metallocenes  
 Abstract    Two isomers of tetrahydro-4,4,8,8-tetramethyl-4,8-disila-s-indacene (L H 2) were m onode-protonated and treated with cyclopentadienyl anion and NiBr2(TH F)i 5 to give a 72% yield of the mixed nickelocene CpNi(LH) where a cyclopentadiene is fused to a nickelocene. The analysis of the paramagnetic 'H, 13C, and 29Si NMR spectra demonstrated that the syn and anti isomer of C pNi(LH) formed in a ratio of 5/1. Both isomers could be deprotonated to yield the anion C pNi(L~). According to its 13C NM R spectrum the bridging ligand L is not planar. 
  Reference    Z. Naturforsch. 49b, 763—7 (1994); received March 16 1994 
  Published    1994 
  Keywords    N ickelocenes, Disilylcyclopentadiene Lithium Cyclopentadienide, Paramagnetic NM R Spectra 
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 Identifier    ZNB-1994-49b-0763 
 Volume    49 
124Author    Klaus Schulbert, Rainer MattesRequires cookie*
 Title    Strukturen  
 Abstract    der m ehrkernigen N ickelth iolato-K om p lexe [(//-S M e)2(N i(M e N H C S 2))2] und c^ c/o -[(//-S M e)2N i]6 Structures of Two Polynuclear Nickel-Thiolato-Complexes [(//-SMe)2(Ni(MeNHCS2))2] and cyc/o-[(/*-SMe)2Ni]6 Thiolato Complexes of Nickel The reactions of N-substituted dithiocarbamic acid esters and nickel acetate yield, by par­ tial degradation of the esters, the polynuclear nickel thiolato complexes cyc/o-[(w-SMe)2Ni]6, 
  Reference    Z. Naturforsch. 49b, 770—772 (1994); eingegangen am 26. Januar 1994 
  Published    1994 
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 Identifier    ZNB-1994-49b-0770 
 Volume    49 
125Author    Marianne Baudler, Helmut Tschäbunin, H. Orst Suchomel, Jürgen HasenbachRequires cookie*
 Title    Beiträge zur Chemie des Phosphors, 228 [1] Funktionalisierte Diphosphane als Synthesebausteine: LiH(f-BuP)2, Li2(r-BuP)2, K2(i-PrP)2, (*-PrP)2Cl2 Contributions to the Chemistry of Phosphorus, 228 [1] Functionalized Diphosphanes as Synthetic Building Blocks: LiH(r-BuP)2, Li2(f-BuP)2, K2(/-PrP)2, (/-PrP)2Cl2  
  Reference    Z. Naturforsch. 49b, 773—7 (1994); eingegangen am 28. März 1994 
  Published    1994 
  Keywords    Diphosphanes, 1 -Lithium-2-hydrogen-1, 2-di-rm-butyldiphosphide, 12-Dilithiurn-l, 2-di-rm-butyldiphosphide, l, 2-Dipotassium -l, 2-diisopropyldiphosphide, 12-Dichloro-l, 2-diisopropyldiphosphane 
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 Identifier    ZNB-1994-49b-0773 
 Volume    49 
126Author    A. Lexander Becht, Arnd VoglerRequires cookie*
 Title    Luminescence Quenching and Photooxidation of Trichlorostannate(II) by Oxygen  
 Abstract    Tin(II), Chloro Complexes, Luminescence Quenching, Photooxidation The luminescence of [SnCl3]_ in acetonitrile (r = 1.6 /us) is quenched by oxygen with k = 3.8xl08 L mol-1 s_1. This quenching is associated with an electron transfer from [SnCl3]_ in its 3Pi sp-excited state to 0 2. Secondary processes lead to the formation of SnOCl2(CH3CN)" with an overall quantum yield of cp = 1.5 at Airr = 254 nm. While this Sn(IV) complex is not light sensitive, [SnClf,]2-in CH3CN undergoes a photochemical reductive elimination with the generation of [SnCl3]_ with cp -0.015 at Airr = 254 nm. 
  Reference    Z. Naturforsch. 49b, 778—780 (1994); received February 14 1994 
  Published    1994 
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 Identifier    ZNB-1994-49b-0778 
 Volume    49 
127Author    Peter Lange, Holger Beruda, Wolfgang Hiller, H. Ubert SchmidbaurRequires cookie*
 Title    Polynuclear Gold(I) Complexes of Dendritic Amines: Formation of Terminal Tris[(triphenylphosphine)aurio(I)]ammonium Groups -N(AuPPh3)3,+  
 Abstract    G old(I) Complexes, Dendritic Amines, G old(I) Complexes, Primary Amines The reactions of dendritic amines R N (C H 2CH2CH2N H 2)2 (R = Me, c-Hex, PhCH2) and N (C H 2CH2N H 2)3 with tris[(triphenylphosphine)aurio(I)]oxonium tetrafluoroborate [0(A u P P h 3)3]+BF4_ in TH F yield species with terminal imido cluster groups -N (A u P P h 3)3,+. The compounds have been obtained as stable crystalline solids in high yields and characterized by NM R spectroscopy as well as mass spectrometry and elem ental analysis. The triply charged nonanuclear com plex [N (C H 2CH2N(AuPPh3)3)3]3+ exhibits major changes in the 'H spectroscopic data and in the chemical properties as compared with com ­ pounds with dications [R N (C H 2C H 2CH2N (A uPPh3)3)2]2+ (R = Me, c-Hex, PhCH2). Excess­ ive auration to give hypercoordinated species has not been observed. 
  Reference    Z. Naturforsch. 49b, 781—7 (1994); received February 22 1994 
  Published    1994 
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 Identifier    ZNB-1994-49b-0781 
 Volume    49 
128Author    Ralf Sonnenburg, Ion Neda, Axel Fischer, PeterG. Jones, Reinhard SchmutzlerRequires cookie*
 Title    Verbindungen mit dem 5,6-Benzo-l,3,2-diazaphosphorinan-4-on-Ringsystem: Synthese von 2-Chlor-, 2-N,N-dimethylamino-und 2-Bis-(2-chlorethyl)amino- substituierten Derivaten mit drei-und vierfach koordiniertem Phosphor Compounds Involving the 5,6-Benzo-l,3,2-diazaphosphorinane-4-one Ring System: Synthesis of 2-Chloro-, 2-N,N-dimethylamino-and 2-Bis-(2-chloroethyl)amino- Substituted Derivatives with Three-and Four-Coordinated Phosphorus  
  Reference    Z. Naturforsch. 49b, 788—8 (1994); eingegangen am 16. D ezem ber 1993 
  Published    1994 
  Keywords    5, 6-Benzo-l, 3, 2-diazaphosphorinan-4-one Derivatives, Dialkylamino Substituents, Bis-(2-chloroethyl)amino Substituents, Platinum Complex, NM R Spectra 
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 Identifier    ZNB-1994-49b-0788 
 Volume    49 
129Author    JensR. Goerlich, Axel Fischer, PeterG. Jones, Reinhard Schmutzler+Requires cookie*
 Title    Organophosphorverbindungen mit tertiären Alkylsubstituenten. III*: Synthese und Reaktionen Di-l-adamantylsubstituierter Phosphorverbindungen; Kristallstruktur von Di-l-Adamantylphosphinsäurechlorid Organophosphorus Compounds with Tertiary Alkyl Substituents. Ill: Synthesis and Reactions of D i-l-adam antyl-Substituted Phosphorus Compounds; Crystal Structure of Di-l-adam antylphosphinic Chloride  
 Abstract    The reaction of adamantane with PC13/A1C13, followed by hydrolysis, gave (l-Ad)2P(: 0)C1 1, which was converted to (l-Ad)2P(:Ö)F 2 and (l-Ad)2P(:S)Cl 3 by standard procedures. The structure of 1 was confirmed by a single crystal X-ray structure determination; despite the bulky substituents the P-C bond lengths are normal (184.0(3), 185.0(3) pm). Whereas chlorine-fluorine exchange in 3 with AsF3 furnished (l-Ad)2P(: S)F 4, desulfuration of 3 with Ph3P to give (l-Ad)2PCl 5 failed. The secondary phosphine oxides R 'R 2P(:0)H (R1, R2 = 1-Ad: 6; R1 = 1-Ad, R2 = 'Bu: 7; R1, R2 = 'Bu: 8) were synthesized by reaction of 1, l-AdP(:0)Cl2 and 'BuP(:0)Cl2 with 'BuLi. 6 and 8 reacted readily with chloral to give the adducts R2P(:0)CH(0H)CC13 (R = 1-Ad: 9; R = 'Bu: 10). Silylation of 6 with Me2NSiMe3 in the presence of dry air led to (l-Ad)2P(:0)0SiM e3 11, which was hydrolyzed to give (l-Ad)2P (:0)0H 12. (l-Ad)2POSiMe3 13 was obtained by the reaction of 6 with /z-BuLi, followed by Me3SiCl. No reaction took place upon heating 6 with Mo(CO)6. (l-Ad)2PCl 5 was synthesized in low yield by the reaction of 6 with PC13. The action of tetrachloro-o-benzoquinone (TOB) upon 6 furnished (l-Ad)2P(: 0)(o-OH)C6Cl4 15, whereas the 'butyl analogue of 15, 16, was synthesized by hydrolysis of the TOB-adduct of di-'butylfluorophos-phine. Analogous 1-adamantyl-and 'butyl-phosphorus compounds are compared with regard to their 31P NMR data. 
  Reference    Z. Naturforsch. 49b, 801—811 (1994); eingegangen am 17. Dezember 1993 
  Published    1994 
  Keywords    Di-l-adamantyl Phosphorus Compounds, Secondary Phosphine Oxides, Di-l-adamantyl Phosphinic Acid, NMR Spectra, X-Ray 
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 Identifier    ZNB-1994-49b-0801 
 Volume    49 
130Author    Seltenen, MohsenSafarpour Haghighi, Andreas Franken, H. Einer, HomborgRequires cookie*
 Title    Kristallchemische Analyse der Stereochemie des Kations und Anions in Bis(triphenylphosphin)iminium-di(phthalocyaninato)metallaten der  
 Abstract    Erden, (PNP)[Ln(Pc2_)2] *xH20 (Ln = La, Gd, Tm; x < 0,5) Crystalchemical Analysis of the Stereochemistry of the Cations and Anions in Bis(triphenylphosphine)iminium Di(phthalocyaninato)m etalates of the Rare Earth Elements, (PNP)[Ln(Pc2~)2] jcH20 (Ln = La, Gd, Tm; x < 0.5) Di(phthalocyaninato)metalates, Rare Earth Metal Complexes, Bis(triphenylphosphine)iminium Cation, Crystal Structure, IR Spectra Of the isostructural series of monoclinic (PNP)[Ln(Pc)2] jcH20 compounds (Ln = La — Tm) the crystal structures of the complex salts of tervalent La (1), Gd (2) and Tm (3) have been determined by single crystal X-ray diffraction analysis. Unit cell data for 2: space group P2j/c; a = 15.172(8), b = 20.826(2), c = 25.876(3) Ä, ß = 95.19(3)°, V -8143(4) Ä3, Z = 4; 1 and 3 are isostructural with 2. The lanthanide ion occupies the center of a nearly ideal square antiprism, although the two staggered phthalocyanine rings are severely distorted in an unsymmetrical funnel-shaped fashion due to electronic, steric, and packing influences in the crystal lattice. Steric effects dictate also the geometry of the PNP cation, which adopts a hybrid conformation whose structural characteristics are between the common linear and bent conformers with medium short P -N distances (1.562 A) and large P -N -P angles in the range 165.6° (1) > 158.3° (2) > 156.1° (3). The strong IR bands at ca. 1375 cm"' assigned to the asym. (P-N) stretch are diagnostic for this hybrid conformation. The presence of water of crystallization in the periphery of the diphthalocyanine anion is confirmed. The shortest contact distance is observed to one of the bridging nitrogen atoms of the Pc2_ ligand (3.02 A) indicating a weak (H O -H -N) hydrogen bond. 
  Reference    Z. Naturforsch. 49b, 812—820 (1994); eingegangen am 22. Februar 1994 
  Published    1994 
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 Identifier    ZNB-1994-49b-0812 
 Volume    49 
131Author    D. Ieter Sellmann, Thomas Hofmann, Falk KnochRequires cookie*
 Title    Ni(II)-und Ni(III)-Komplexe mit dem fünfzähnigen Thioether- Thiolat-Amin-Liganden 'NMeS4'2_ ('NMeS4'2_ = Dianion von 2,2'-Bis(2-mercaptophenylthio)diethylmethylamin) Transition Metal Complexes with Sulfur Ligands, CV* Ni(II) and Ni(III) Complexes with the Pentadentate Thioether- Thiolate-Amine-Ligand 'N MeS4'2_ ('N MeS4'2-= Dianion of 2.2'-Bis(2-m ercaptophenylthio)diethylmethylamine)  
 Abstract    Paramagnetic [N i('N MeS4')]2 1 ('N MeS4'2_ = 2.2'-Bis(2-m ercaptophenylthio)diethylm ethyl-a m in e(2 -)) was synthesized from N i(ac)2 and N a2-'N MeS4' and characterized by X-ray structure analysis. In solid state, 1 contains two pseudo-octahedral [N i('N MeS4')] fragments bridged via thiolate donors. In contrast to the parent com plex [N i('N HS4')]2, the thiolate and thioether donors coordinate cis to the Ni center forming m eso [N i('N MeS4')] fragments of Cs symmetry. 1 readily dissociates in solution to give mononuclear [N i('N MeS4')]. Reaction of [N i('N MeS4')]2 1 with PM e3 yielded [N i(PM e3)('N MeS4')] 2, oxidation by io­ dine gave the Ni(III) complex [N i(I)('N MeS4')] 3. Ubergangsmetallkomplexe mit Schwefel-Liganden, CY* 
  Reference    Z. Naturforsch. 49b, 821 (1994); eingegangen am 15. Februar 1994 
  Published    1994 
  Keywords    Nickel Complexes, Thioether-Thiolate-Amine-Ligands, X-Ray 
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 Identifier    ZNB-1994-49b-0821 
 Volume    49 
132Author    Felora Heshmatpour, Sigrid Wocadlo, W. Erner Massa, Kurt Dehnicke, Frank Bottomley, R. Obert, W. DayRequires cookie*
 Title    Organometallische Oxide: Die Kristallstruktur von [(f7-C5H5)Ti]8(//-0)i2 Organometallic Oxides: The Crystal Structure of [(77-C5H5)Ti]8(w -0 )|2  
 Abstract    The structure of the complex [(j7-C5H 5)Ti]8(M-:0) 12 has been determined in a crystal of [(?/-C-sHs)Ti]8(/< -0)p -6 CH^CN (space group P I, Z = 1, lattice dimensions at -4 0 °C: a = 1083.9(3). b = 1292.9(1), c = 1304.0(2) pm, a = 61.18(1)°, ß = 71.73(2)°, y = 70.35(2)°, structure solved using 2164 observed unique reflections, R = 0.043). The Ti atoms occupy the corners of an approximate cube. The 12 oxygen atoms are at the mid point of the edges connecting the Ti atoms. Two pairs of the 12 T i-O -T i bridge angles are 147.9(3)° and 148.6(3)°, the remaining eight bridge angles are between 162.4(3)° and 163.9(3)°. The T i-O distances are between 179.5(5) and 181.8(5) pm with an average of 180.5(5) pm. Each Ti atom is capped bv an //''-cyclopentadienyl ligand. The same subane-like unit has been found in [(//-C5Hs)Ti]4C«2-S e),0^ -S e)3-[(?;-C sH ,)fi]s(jW 2-O)12 Et3N THF. 
  Reference    Z. Naturforsch. 49b, 827 (1994); eingegangen am 21. Februar 1994 
  Published    1994 
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 Identifier    ZNB-1994-49b-0827 
 Volume    49 
133Author    Norbert Auner, Carola Wagner, Wolfgang ZieheRequires cookie*
 Title    Silaheterocyclen, XXVII. Substituenteneffekte zur Steuerung des Cycloadditionsverhaltens von Silaethenen [1] Silaheterocycles, XXVII. Controlling the Cycloaddition Behavior of Silenes by Substituent Effects [1]  
 Abstract    The silene Cl2Si=C(Ph)CH2Bu' (2) is formed by the reaction o f l,l,l-trichloro-2-phenyl-l-silaprop-2-ene (1) with LiBu' in n-pentane in the temperature range from -1 5 to 0 °C. TTie reaction initially leads to the corresponding a-lithio adduct A (addition o f LiBu' to the vinyl group of 1); subsequent LiCl elimination yields 2 as an intermediate. 2 can be trapped by Me3SiOMe (3) and dienes which add across the Si=C bond. In the absence of trapping agents but in the presence of the Lewis base N E t3 the mixture 1/LiBu' reacts to give the disilacyclobutane 4. Due to its electronic and steric properties, Cl2Si=C(Ph)C H 2Bu' (2) and butadienes yield mainly the D iels-A lder adducts (5, 7, 9) while with styrene and 1,3-cyclo-hexadiene the [2 + 2] and [4 + 2] products are formed in competition. With 2-norbornene, 2,5-norbornadiene and quadricyclan the [2 + 2] and [2 + 2 + 2] products are formed selectively but only in low yields. In all reactions except with quadricyclan an ene-reaction com petes with the cycloaddition leading to ene-com pounds as by-products. 
  Reference    Z. Naturforsch. 49b, 831 (1994); eingegangen am 18. Februar 1994 
  Published    1994 
  Keywords    Silaheterocycles, l, l, l-Trichloro-2-phenyl-l-silaprop-2-ene, Substituent Effects, Formation of Silenes, Cycloaddition Reactions 
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 Identifier    ZNB-1994-49b-0831 
 Volume    49 
134Author    A. Mcfarlane, J. R. Lusty, H. E., U.K J J A Fiol, Terrón, E. Molins, C. Miravitlles, V. MorenoRequires cookie*
 Title    Pd(II) and Pt(II) Complexes of l,2-Bis(pyridin-2-yl)ethane-Ar ,./V  
 Abstract    Pyridine Pt(II) Compounds, Complexes of Pt(II) and Pd(II) X-ray crystal structures and properties of the two Pd(II) and Pt(II) complexes [bpeH2][PdCl4] and [Pt(bpe)Cl2], [bpe = l,2-bis(pyridin-2-yl)ethane] are described and corre­ lated with the IR and 'H N M R /13C NM R spectroscopic data. In the case of the Pt(II) com ­ plex, the l,2-bis(pyridin-2-yl)ethane is bound to the metal by the heterocycle nitrogen atoms but no direct bond is found in the case of the Pd(II) complex. The ligand exhibits low energy geom etries in both compounds: the c/s-conformation in the Pt(II) complex, and the trans-conformation in the Pd(II) complex. 
  Reference    Z. Naturforsch. 49b, 844 (1994); received January 27 1994 
  Published    1994 
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 Identifier    ZNB-1994-49b-0844 
 Volume    49 
135Author    G. C. Papavassiliou, I. B. KoutselasRequires cookie*
 Title    Excitonic Bands in the Optical Absorption Spectra of A 3M X6 and A 3M2X9 (A = M eNH 3, M e2NH?, M e3NH , Me4N; M = Bi, Sb; X = Cl, Br, I)  
 Abstract    The title compounds (natural low-dimensional semiconductors) show strong excitonic optical ab­ sorption bands in the UV-visible spectral region, because of the dielectric confinement of excitons. as in the cases of other similar systems based on PbX5 ~, SnX^-. P t ' -X -P t IV-X , C d,Sv-clusters etc. 
  Reference    Z. Naturforsch. 49b, 849—851 (1994); received March 28 1994 
  Published    1994 
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 Identifier    ZNB-1994-49b-0849_n 
 Volume    49 
136Author    PeterG. Jones, Oliver Hiemisch, Blaschette ArmRequires cookie*
 Title    Formation and Crystal Structure of the Complex [(18-Crown-6)(CH2Cl2)2]  
 Abstract    (18-Crown-6)-2 Dichlorom ethane. Formation. Crystal Structure Single crystals of the title complex were fortuitously grown from a dichloromethane solu­ tion containing 18-crown-6 and sulfur trioxide. Crystallographic data (at -1 3 0 °C): triclinic, space group P I, a = 819.1(7). b = 860.6(7), c = 905.8(7) pm. a = 63.98(3), ß = 66.56(3), y = 74.95(3)°, V = 0.5236 nm3, Z = 1, D , = 1.377 M g irr3. In the centrosymmetric formula unit, the two CH2C12 m olecules are situated one above and one below the plane of the ether oxy­ gen atoms. They are C -H — O hydrogen-bonded to two opposing oxygen atoms (H —O 237.1 and 270.6 pm, C — O 335.5 and 365.9 pm, C -H — O 171.7 and 161.8°). The crown ether molecule has approximate D?(/ symmetry. 
  Reference    Z. Naturforsch. 49b, 852 (1994); eingegangen am 7. Januar 1994 
  Published    1994 
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 Identifier    ZNB-1994-49b-0852_n 
 Volume    49 
137Author    Z. NaturforschRequires cookie*
 Title    Tris [ (trimethylsilyl)oxy ] antimony  
 Abstract    Heterosiloxanes, Stibiosiloxanes, Antimonites Tris[(trimethylsilyl)oxy]antimony (Sb(OSiMe3)3, 1) has been prepared from SbCl3 and 3 equiv. of LiOSiMe3 in diethylether. According to mass spectrometric and NMR spectroscopic data, 1 appears to be a monomer in solution and in the gas phase. Dimerisation occurs, however, in the solid state as verified by an X-ray crystal structure determination. The unit cell contains three crystallographically independent monomers, two of which form one type of dimer, while the other is part of a centrosymmetrical dimer. In both types of dimers two Sb atoms are connected via two OSiMe3 groups to form distorted Sb20 2-squares. Together with the remaining 4 OSiMe3 groups and the two stereochemically active lone pairs, each Sb exhibits a trigonal bipyramidal coordination. 
  Reference    Z. Naturforsch. 49b, 855—858 (1994); received February 22 1994 
  Published    1994 
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 Identifier    ZNB-1994-49b-0855 
 Volume    49 
138Author    Herrn Prof, R. DrRequires cookie*
 Title    Synthese von Alkin-, Alkinyl-und Vinyliden-Rhodium-Komplexen ausgehend von Alkinyltriphenylsilanen [1] Rhodium(I) and Rhodium(III) Complexes. Alkyne, Alkynyl and Vinylidene Ligands, Isomerisation Reactions, Alkynyltriphenylsilanes as Substrates  
  Reference    Z. Naturforsch. 49b, 859—869 (1994); eingegangen am 4. März 1994 
  Published    1994 
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 Identifier    ZNB-1994-49b-0859 
 Volume    49 
139Author    IrinaB. Ecker, M. Arcus, W. Indhaus, R. Ainer, M. AttesRequires cookie*
 Title    Synthesen, 121Sb-Mößbauer-Spektren und  
 Abstract    Strukturen von [SbF3(18-Krone-6)], [SbF3(18-Krone-6)]*CH3CN und [(SbF3)2(12-Krone-4)] Synthesis, 121Sb-M ößbauer Spectra and S tructures of [SbF3(18-Crown-6)], [SbF3(18-Crown-6)] C H 3CN, and [(SbF3)2(12-Crow n-4)] The crown ether complexes SbF3(18-crown-6) (1), SbF3(18-crown-6) • CH3CN (2) and (SbF3)2(12-crown-4) (3), have been prepared by reactions of SbF3 and the corresponding crown ether. They have been characterized by IR. Raman and 121Sb-Mößbauer spectroscopy, and by X-ray structure determinations. The s electron density at the Sb atom is diminished in these complexes. 1 and 2 show a symmetrical half-sandwich structure, with coplanar O atoms and S b -O distances ranging from 298 to 321 pm. 3 has a band-like structure. The two metal centers adopt different stereochemistries. The S b -O distances are in the range from 269 to 325 pm. One oxygen atom of 12-crown-4 has a bridging function. Crystal data for 1: space group P 21212i, a = 823,1(1), b = 1146,1(2), c = 1807,0(3) pm, Z = 4; 2: space group P2,/c. a = 1257,7(3), b = 828,9(2), c -1895,5(5) pm, ß = 93,68(2). Z = 4; 3: space group P2j/c, a = 805,6(1), b = 2143,1(4), c = 836,4(2) pm, ß = 90,98(1), Z = 4. 
  Reference    Z. Naturforsch. 49b, 870—876 (1994); eingegangen am 30. Dezember 1993 
  Published    1994 
  Keywords    Crown Ether Complexes of SbF3, 121Sb-Mößbauer Spectra, Crystal Structure 
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 Identifier    ZNB-1994-49b-0870 
 Volume    49 
140Author    H. Ans, Joachim Breunig, M. Oham, EdA M Oham, M. Ed, KlausH E, ErtRequires cookie*
 Title    A Cyclic  
 Abstract    O rgan o an tim o n y (III) O xide, (R S b O)4 [R = (M e3Si)2CH] The cyclic organostibane oxide [(Me3Si)2CHSbO]4 (1) has been prepared by reaction of RSbCl2 with KOH in water/diethylether and crystallization as 1 H 20 from petroleum ether. The crystal structure of 1 H20 consists of a boat shaped 8-membered Sb40 4 heterocycle with the substituents in trans positions (distances S b -O 197.0(3) pm, S b -C 217.2(4) pm, angles O -S b -O 93.2(1)°, S b -O -S b 122.3(2)°, O -S b -C 96.2(1)°) and disordered water molecules. Crystal data: tetragonal, space group 14; a = 16.091(2), c = 11.057(2) A; Z = 2. 
  Reference    Z. Naturforsch. 49b, 877—880 (1994); eingegangen am 28. Januar 1994 
  Published    1994 
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 Identifier    ZNB-1994-49b-0877 
 Volume    49 
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