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  • Articles  (61)
  • Inorganic Chemistry  (61)
  • 1990-1994  (61)
  • 1935-1939
  • 1991  (61)
  • 1
    Electronic Resource
    Electronic Resource
    Synthesis, Structure, and Reactivity of Chiral Rhenium Cycloalkene Complexes of the Formula ; Facile Vinylic Deprotonation of a Coordinated Alkene (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 729-742 
    Details
    ISSN: 0009-2940
    Keywords: Cycloalkene ligands ; Cyclopentylidene ligands ; Deprotonotion reactions ; Rhenium complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reactions of [(η5-C5H5)Re(NO)(PPh3)(ClC6H5)]+BF-4 and (n = 5, a; 6, b; 7, c; 8, d) give cycloalkene complexes (6a - d, 94 to 79%). A crystal structure of the methylcyclopentadienyl analog of 6a shows the Re - plane and Re - PPh3 bond to be coplanar, with the vinyl protons syn to the cyclopentadienyl ligand. Reaction of 6a and tBuO-K+ leads to the vinyl complex (9a, 90%) instead of expected allyl complex (10a) Analogous reactions of 6b - d give varying mixtures of 9b - d/10b - d. HBF4 · OEt2 and 9a react to form the cyclopentylidene complex (10+ BF-4, 96%), the stability of which precludes any intermediacy in the deprotonation of 6a. A crystal structure of 11+ PF-6 shows the Re=C—C planes to be perpendicular to the Re - P bond. Spectroscopic features of compounds 6 are analyzed in detail, and NMR data show a high barrier to cyclopentylidene ligand rotation in 11+ BF-4 (ΔG≢ (110°C) ≥ 19 kcal/mol).
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19911240410
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  • 2
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    Electronic Resource
    Darstellung und Charakterisierung von [N-(2-Mercaptoacetyl)-N′ -4-(penten-3on-2)ethylen-1,2-diaminato]oxorhenium(V), ReO(MRP 40)Professor Eberhard Hoyer zum 60. Geburtstage am 26. Mai 1991 gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 600 (1991), S. 15-19 
    Details
    ISSN: 0044-2313
    Keywords: Rhenium compounds ; synthesis ; mass spectra ; n.m.r ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Characterization of [N-(2-Mercaptoacetyl)-N′ -4-(penten-3on-2)ethylen-1,2-diaminato]oxorhenium(V), ReO(MRP 40)The title complex is obtained in good yields from the reaction of the triphenylmethyl-protected ligand with (Bu4N)ReOBr4 or ReOCl3(Ph3P)2. The structure of the compound as neutral oxorhenium(V) complex is confirmed by analytical, 1H-, 13C-NMR, IR, UV/Vis as well as mass spectrometric studies.
    Notes: Der Titelkomplex entsteht in guten Ausbeuten bei der Umsetzung von (Bu4N)ReOBr4 oder ReOCl3(Ph3P)2 mit der triphenylmethyl-geschützten Form des vierzähnigen Liganden.Die Struktur des Chelats als neutrale Oxoverbindung des Rheniums (V) wird durch analytische sowie 1H-, 13C-NMR, IR-, UV/Vis- und massenspektrometrische Untersuchungen gestützt.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19916000103
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  • 3
    Electronic Resource
    Electronic Resource
    Zwei- und dreikernige Nickel(II)-chelate bis-bidentater N-AcylselenoharnstoffeProfessor Eberhard Hoyer zum 60. Geburtstage am 26. Mai 1991 gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 600 (1991), S. 73-81 
    Details
    ISSN: 0044-2313
    Keywords: Nickel(II) chelates ; syntheses ; crystal structures ; FAB mass spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Di- and Trinuclear Nickel(II) Chelates of Bis-bidentate N-AcylselenoureasBis-bidentate isophthaloyl-bis(selenoureas) form with nickel(II) ions under deprotonating conditions macrocyclic dinuclear metal chelates. This was confirmed by X-ray crystal structure analysis of the cyclo-di[nickel-μ-[1,1,1′,1′-tetraisobutyl-3,3′-iso-phthaloyl-bis-selenoureato(2-)Se,O:O′, Se′]], 2. The compound 2 crystallizes in the monoclinic space group P 21/c with a = 11.673 (1); b = 19.834 (2); c = 13.606 (1) Å; β = 107.45 (1)° and Z = 2. The final R value was R = 0.081 for 3049 observed reflections.Bis-bidentate terephthaloyl-bis(selenoureas) give under the same conditions macrocyclic trinuclear nickel(II) chelates.Both types of the complexes are characterized by FAB mass spectra.
    Notes: Bis-bidentate Isophthaloyl-bis(selenoharnstoffe) bilden mit Nickel(II)-Ionen unter deprotonierenden Bedingungen makrocyclische Zweikernchelate. Dies wurde durch Röntgenkristallstrukturanalyse des cyclo-Di[nickel-μ-[1,1,1,′,1′-tetraisobutyl-3,3′-iso-phthaloyl-bisselenoureaoto(2-)-Se, O:O′, Se′]], 2, bestätigt. Die Verbindung 2 kristallisiert monoklin in der Raumgruppe P 21/c mit den Gitterkonstanten a = 11,673 (1); b = 19,834 (2); c = 13,606 (1) Å; β = 107,45 (1)° und Z = 2. Der abschließende R-Wert betrug R = 0,081 für 3049 beobachtete Reflexe. Bis-bidentate Terephthaloyl-bis(selenoharnstoffe) ergeben unter den gleichen Bedingungen makrocyclische Dreikernnickel(II)-chelate.Beide Komplextypen wurden durch FAB-Massenspektren charakterisiert.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19916000111
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  • 4
    Electronic Resource
    Electronic Resource
    Ternäre Chloride in den Systemen ACl/GdCl3 (A = Na—Cs)Professor Hans-Georg von Schnering zum 60. Geburtstage gewidmet (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 598 (1991), S. 307-318 
    Details
    ISSN: 0044-2313
    Keywords: Alkali halides/gadolinium halide systems ; phase diagrams ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ternary Chlorides in the Systems ACl/GdCl3 (A = Na—Cs)The phase diagrams of the pseudobinary systems ACl/GdCl3 (A = Na—Cs) were investigated by DTA. Their powder diffractograms were indexed in analogy to known structure families. By solution calorimetry and measurements of e.m.f. = f(T) in galvanic cells for solid electrolytes the enthalpies ΔH0 and free enthalpies ΔG0 for the formation of the ternary chlorides from the compounds adjacent in the systems were determined. The systems with A = K, Rb, Cs are analogous to those with Sm3+ and Eu3+. There exist compounds A3GdCl6, A2GdCl5 and AGd2Cl7. Cs2GdCl5 is crystallysing in the Cs2DyCl5 type; the Rb- and K-compounds and also Na2GdCl5 have the K2PrCl5-structure. In the system NaCl/GdCl3 additionally the compounds NaGdCl4 and Na3GdCl6 were found. L—Na3GdCl6 is metastable compared with (NaCl + Na2GdCl5); above 265°C stable H—Na3GdCl6 is existing (cryolite-structure).
    Notes: Die Zustandsdiagramme der pseudobinären Systeme ACl/GdCl3 (A = Na—Cs) wurden mittels DTA untersucht und soweit noch nicht bekannt die Strukturen der existierenden ternären Chloride aus Röntgenaufnahmen an Kristallpulvern bestimmt. Die Systeme mit A = K, Rb, Cs entsprechen den Systemen des Sm3+ und Eu3+. Es treten die Verbindungen A3GdCl6, A2GdCl5 und AGd2Cl7 auf. Von den 2:1-Verbindungen kristallisiert Cs2GdCl5 im Cs2DyCl5-Typ, die Verbindungen mit Rb und K sowie Na2GdCl5 im K2PrCl5-Typ. Im System NaCl/GdCl3 wurden außerdem die Verbindungen Na3GdCl6 und NaGdCl4 nachgewiesen. T—Na3GdCl6 ist metastabil gegenüber dem Zerfall zu NaCl und Na2GdCl5; oberhalb 265°C existiert stabiles H—Na3GdCl6 mit Kryolith-Struktur.über Messungen der Lösungsenthalpien und EMK-Messungen als Funktion der Temperatur in galvanischen Zellen für feste Elektrolyte wurden die Enthalpien ΔH0 und freien Enthalpien ΔG0 für die Bildung der ternären Chloride aus den im System benachbarten Verbindungen bestimmt. Auch hier entsprechen die Ergebnisse den in den Sm- und Eu-Systemen gefundenen.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915980128
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  • 5
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    Synthesis, structure, and properties of LaSrCuGaO5Dedicated to Professor Hans-Georg von Schnering on his 60th Birthday (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 598 (1991), S. 327-338 
    Details
    ISSN: 0044-2313
    Keywords: Lanthanum strontium copper gallate ; preparation ; crystal structure ; magnetic susceptibility ; electrical resistivity ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Präparation, Struktur und Eigenschaften von LaSrCuGaO5Die neue Brownmillerit-verwandte Verbindung, LaSrCuGaO5, wird dargestellt und charakterisiert. Sie kristallisiert in der orthorhombischen nicht-zentrosymmetrischen Raumgruppe Ima2.Die Gitterparameter sind a = 16,383(1) Å, b = 5,5293(7) Å, c = 5,3275(6) Å. Die Struktur ist der des Perowskits verwandt, enthält aber geordnete Sauerstoffleerstellen in den zweidimensionalen Gallium-Sauerstoff-Schichten, was zur tetraedrischen Koordination der Gallium-Kationen führt. Andere wichtige Strukturmerkmale sind die gewellten Kupfer-Sauerstoff-Ebenen und die statische Verteilung der Lanthan- und Strontium-Kationen über die A-Lage. Genaue Gitterkonstanten-Bestimmungen zeigen eine Dehnung der a-Achse um 0,17 Å bei Dotierung mit Strontium La1-xSr1-xCuGaO5 (xmax = 0,13). Messungen der magnetischen Suszeptibilität zeigen, daß die Verbindung bis zu 4 K paramagnetisch bleibt.
    Notes: The new brownmillerite-related compound, LaSrCuGaO5, has been synthesized and characterized. It crystallizes in the orthorhombic non-centrosymmetric space group Ima2. The unit cell dimensions are a = 16.383(1) Å, b = 5.5293(7) Å, c = 5.3275(6) Å. The structure is related to perovskite but contains ordered oxygen vacancies within the two-dimensional gallium oxygen layers resulting in tetrahedral coordination of the gallium cations. Other important structural features include buckled copper-oxygen planes, and disorder of the lanthanum and strontium cations over the A-site. Accurate lattice constant measurements reveal an a-axis expansion of 0.17 Å when doped with strontium La1-xSr1+xCuGaO5 (xmax = 0.13). Magnetic susceptibility measurements demonstrate that the compound remains paramagnetic to 4 K.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915980130
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  • 6
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    Electronic Resource
    Chemie polyfunktioneller Moleküle. 107. Silber(I)-halogenid-Komplexe des Bis(diphenylphosphino)aminsProfessor Dieter Sellmann zum 50. Geburtstage gewidmet. (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 603 (1991), S. 77-88 
    Details
    ISSN: 0044-2313
    Keywords: Silver(I) halide complexes ; bis(diphenylphosphino) amine ligand ; preparation ; nmr, ir, Raman data ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Chemistry of Polyfunctional Molecules.107. Silver(I) Halide Complexes of Bis(diphenylphosphino)amineBis(diphenylphosphino)amine, [(C6H5)2P]2NH, dppa, (1) reacts with the Silver(I) Halides AgX (X = Cl, Br, I) in methanol to the ionic complexes [Ag3X2(dppa)3]+X- (3a: X = Cl, 3 b: X = Br, 3 c: X = 1). Metathesis with NH4PF6 in methanol yields the complexes [Ag3X2(dppa)3]+PF6- (3 a′: X = Cl, 3b′: X = Br, 3c′: X = I). For spectroscopic comparisons the compounds [Ag3X2(dppm)3]+X- [X = Cl, Br, I; 5a-c; dppm = (C6H52PCH2P(C6H5)2 (4)], in part described earlier, were also synthesized. Besides elemental analyses, conductivity measurements 31P{1H}-NMR, 1H-NMR and infrared spectra the complexes were especially characterized by their Raman spectra. The latter show for the trigonal bipyramidal cations of 3a-c, 3a′-c′ and 5a-c typical vs (XAg3X) bands at 135 (X = Cl), 125 (X = Br) and 105 (X = I) cm-1.
    Notes: Bis(diphenylphosphino)amin, [(C6H5)2P]2NH, dppa, (1) reagiert mit den Silber(I)halogeniden AgX (X = Cl, Br, I) in Methanol zu den ionischen Komplexen [Ag3X2(dppa)3]+X- (3a: X = Cl, 3b: X = Br, 3c: X = I). Metathese mit NH4PF6 in Methanol liefert die Komplexe [Ag3X2(dppa)3]+PF6- (3a′: X = Cl, 3b′: X = Br, 3c′: X = I). Zu spektroskopischen Vergleichszwecken werden auch die teilweise bekannten Verbindungen [Ag3X2(dppm)3]+X-[X = Cl, Br, I; 5a-c; dppm = (C6H5)2PCH2P(C6H5)2 (4)] dargestellt. Neben Elementaranalysen, Leitfähigkeitsmessungen, 31P{1H}-NMR, 1H-NMR- und IR-Spektren werden die Komplexe insbesondere durch ihre Raman-Spektren charakterisiert. Letztere zeigen für die trigonal-bipyramidalen Kationen von 3a-c, 3a′-c′ und 5a-c typische vs (XAg3X)-Banden bei etwa 135 (X = Cl), 125 (X = Br) und 105 (X = I) cm-1.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19916030111
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  • 7
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    Electronic Resource
    Synthese und Strukturuntersuchungen von Ba2H[α-FeO4W12O36] · 26 H2O (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 594 (1991), S. 191-201 
    Details
    ISSN: 0044-2313
    Keywords: Dibarium-α-dodecawolframatoferrate(III)-26-hydrate ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure Studies of Ba2H[α-FeO4W12O36] · 26 H2OThe heteropolyanion compound Ba2H[α-FeO4W12O36] · 26 H2O (I) crystallizes in the tetragonal space group P4n2 with the lattice parameters a = 12.398(6), c = 18.721(6) Å; Z = 2; Dx = 4.128 g · cm-3. The structure was solved on a twinned crystal from 1029 observed reflections and refined to an index R of 7.6%. The calculations were done by means of a modified ORFLS-programme by Eitel and Bärnighausen. The heteropolyanion [α-FeO4W12O36]5- has the well known α-Keggin structure. The average distance of the four central oxygen atoms to the FeIII position (0, 0, 0) is 1.84 Å. The angles ∢ O—Fe—O are 112.3° (4X) and 103.9 (2X), respectively, which leads to an disphenoidal distortion of the FeO4 tetrahedron.The powder and single crystal ESR spectra of I show the anisotropy of the FeIII fine structure transition 1/2 ↔ -1/2. The Mößbauer spectra confirm the tetragonal distortion of the central FeO4 tetrahedron (quadrupole splitting Δ ≈ 0.50 mm · s-1).
    Notes: Die erstmalig in einkristalliner Form dargestellte Heteropolyanionenverbindung Dibarium-α-dodekawolframatoferrat(III)-26-Hydrat, Ba2H[α-FeO4W12O36] · 26 H2O (I), kristallisiert tetragonal mit den Gitterkonstanten a = 12,398(6), c = 18,721(6) Å; Z = 2; Dx = 4,128 g α cm-3. Für den vorliegenden Inversionszwilling mit einem Heteropolyanion vom α-Keggin-Typ wurde zur Verfeinerung der Kristallstruktur in der Raumgruppe P4n2 ein von Eitel und Bärnighausen modifiziertes ORFLS-Programm benutzt (R-Wert 7,6%). Der mittlere Abstand der vier zentralen Sauerstoffatome zur FeIII-Position (0, 0, 0) beträgt 1,84 Å. Die Winkel ∢ O—Fe—O weichen mit 112,3(4X) bzw. 103,9°(2X) deutlich von 109,5° ab, wodurch das Tetraeder zu einem tetragonalen Disphenoid verzerrt wird.Die Mößbauer-Spektren von I weisen eine deutliche Quadrupolaufspaltung von Δ; ≈ 0,50 mm · s-1 auf, die durch die Asymmetrie in der Umgebung von FeIII hervorgerufen wird. Damit in Übereinstimmung zeigen die EPR-Spektren sowohl für Pulver als auch für einen Einkristall von I ein Signal bei g ≃ 2, das im wesentlichen aus dem Feinstrukturübergang 1/2 ↔ - 1/2 des FeIII-Ions herrührt und eine deutliche Anisotropie aufweist.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19915940122
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  • 8
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    Clusteraufbau durch Photolyse von R3PAuN3. V. Synthese und Struktur von [(Ph3PAu)4Co(CO)3]PF6 Bindungsverhältnisse in Clustern [(Ph3PAu)xM(CO)y]+Professor Josef Goubeau in memoriam (1991)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 593 (1991), S. 35-45 
    Details
    ISSN: 0044-2313
    Keywords: Tetragold Cobalt Cluster ; Synthesis ; Crystal Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Cluster Synthesis by Photolysis of R3PAuN3. V. Synthesis and Structure of [(Ph3PAu)4Co(CO)3]PF6. Bonding in Clusters [(Ph3PAu)xM(CO)y]+[(Ph3PAu)4Co(CO)3]+ (1) is formed by photolysis of Ph3PAu—Co(CO)4 and subsequent addition of Ph3PAu+ to the photolysis product. It crystallizes as 1 · PF6 in the triclinic space group P1 with a = 1646,7(6), b = 1915,3(3), c = 1288,0(7) pm, α = 91,35(3), β = 112,02(3), γ = 74,42(2)°; Z = 2. The inner skeleton of the cluster has the form of a trigonal bipyramid with the Co atom in equatorial position and distances Co—Au between 258 and 265 pm. The distances Au—Au range from 278 to 293 pm. The structure and bonding of 1 and related transition metal-gold clusters [(R3PAu)xM(CO)y]+ are discussed.
    Notes: [(Ph3PAu)4Co(CO)3]+ (1) entsteht durch Photolyse von Ph3PAu—Co(CO)4 und anschließende Zugabe von Ph3PAu+ zum Photolyseprodukt. Es kristallisiert als 1 · PF6 in der triklinen Raumgruppe P1 mit a = 1646,7(6), b = 1915,3(3), c = 1288,0(7) pm, α = 91,35(3), β = 112,02(3), γ = 74,42(2)°; Z = 2. Das innere Clustergerüst Au4Co bildet eine trigonale Bipyramide mit dem Co-Atom in äquatorialer Position und Au—Co-Abständen zwischen 258 und 265 pm, sowie Au—Au-Abständen zwischen 278 und 293 pm. Struktur und Bindungsverhältnisse von 1 und verwandten Übergangsmetall-Gold-Clustern [(R3PAu)xM(CO)y]+ werden diskutiert.
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    URL: http://dx.doi.org/10.1002/zaac.19915930105
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  • 9
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    Metallatome in der Synthese von Metallclustern, II1) Reaktionen von substituierten Cyclopentadienen und Nickelocen mit Nickel- und Eisenatomen (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 301-308 
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    ISSN: 0009-2940
    Keywords: Metal atom synthesis ; Clusters ; Electrochemistry ; Cyclic voltammetry ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Metal Atoms in the Synthesis of Metal Clusters, II1). - Reactions of Substituted Cyclopentadienes and Nickelocene with Nickel and Iron AtomsBy vaporizing nickel atoms into solutions of tert-butyl-substituted cyclopentadienes in methylcyclohexane mononuclear sandwich compounds (1, 4, and 6 as main products) as well as tri- and tetranuclear clusters are prepared. With mono- and di-tert-butyl-substituted cyclopentadienes as ligands the new clusters 2 and 5 are obtained. In the reaction with 1,2,4-tri-tert-butylcyclopentadiene 6 is the only observed product. Hindered rotation around the metal-ligand bond vector is observed for 4 even at room temperature. When treating 1 with nickel atoms cluster 2 is formed, indicating some importance of 1 during the formation of 2 in the above reaction. Clusters 2 and 5 contain hydrido ligands, which could be identified in the case of tris(1,3-di-tert-butyl-η5-cyclopentadienyl)trinickel dihydride (5) by a single crystal structure determination as μ3-H bridges. A tetrahedral structure is found for the cluster 2 by X-ray crystallography. With the aid of MS, IR, magnetic measurements, and cyclovoltammetric investigations 2 is identified as a mixture of 2a and 2b bearing one or three bridging hydrogens, respectively. In general 2a, 2b, and 5 show a rich redox chemistry with reversible redox couples between -2 and +2. Reaction of iron atoms, nickelocene, and mesitylene in methylcyclohexane at -120°C leads unexpectedly to cluster 3, tetrakis(η5-cyclopentadienyl)tetranickel trihydride and a not yet identified (η5-cyclopentadienyl)mesityleneiron complex. Possible formation routes for 1-6 are discussed.
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    URL: http://dx.doi.org/10.1002/cber.19911240210
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  • 10
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    The Conformational Behaviour of 10-Substituted Spiro[4.5]decanes (1991)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 124 (1991), S. 551-561 
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    ISSN: 0009-2940
    Keywords: Conformational analysis ; Spiro[4.5]decanes ; Allylboration, transition state models ; Ketals, chiral, cleavage by Lewis acids ; Calculations, MNDO and SYBYL ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The conformational behaviour of 10-X-substituted 1,4-dioxa-and 1,4,6-trioxaspiro[4.5]decanes 1 - 4 has been studied by 13C-, 19F- and 1H-NMR spectroscopy. Two X-ray analyses (of 2a,e) are presented, and their implications to cleavage reactions of chiral acetals are discussed. Participation of twist boat forms in the conformeric equilibrium of at least 1c has been made plausible by observing 13C,19F-NMR coupling constants. The ratios of axial to equatorial conformer in 1 - 4 have been calculated by molecular mechanics.
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    URL: http://dx.doi.org/10.1002/cber.19911240322
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