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  • single crystal structure  (9)
  • Organic Chemistry  (4)
  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1969-1972 
    ISSN: 0044-2313
    Keywords: Chromium tetrafluoride ; single crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Structure of Chromium TetrafluorideBy direct fluorination of elemental chromium with a HF/F2-mixture under solvothermal conditions CrF4 has been obtained for the first time in form of single crystal suitable for x-ray investigations. The violet till amethyst coloured CrF4 crystallizes tetragonal, space group P42/mnm-D4h14 (Nr. 136), a = 829.6(1) pm, c = 373.7(1) pm, Z = 4 and is closely related to the NbOCl3-type of structure [1].
    Notes: Durch Druckfluorierung von elementarem Chrom mit einem HF/F2-Gemisch unter Solvothermalbedingungen gelang es erstmals, CrF4 in Form zur Strukturbestimmung geeigneter Einkristalle darzustellen. Das violette bis amethystfarbene, häufig nadelförmige Chromtetrafluorid kristallisiert tetragonal in der Raumgruppe P42/mnm-D4h14 (Nr. 136) mit a = 829,6(1) pm, c = 373,7(1) pm, Z = 4 und ist vom Aufbau her dem NbOCl3-Typ eng verwandt [1].
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1076-1082 
    ISSN: 0044-2313
    Keywords: Dioxygenyl compounds ; single crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Crystal Structure of O2+MF6- (M = Sb, Ru, Pt, Au)O2+MF6- (M = Sb, Ru, Pt, Au) were obtained again, but for the first time investigated by X-ray methods. Colourless O2+SbF6- and the rubyred compounds O2+RuF6- and O2+PtF6- crystallize isostructural in space group Ia3-Th7 (Nr. 206) with a = 1016(1) pm (Sb), a = 1002.6(9) pm (Ru) and a = 1003.6(9) pm (Pt), Z = 8. Yellow O2+AuF6- crystallizes trigonal-rhombohedric in space group R3-D326 (Nr. 148) with a = 775.9(3) pm, c = 711.7(4) pm, Z = 3.
    Notes: Erneut dargestellt, aber erstmals anhand von Einkristallen röntgenographisch untersucht wurden die Fluoride O2+MF6- (M = Sb, Ru, Pt, Au). Farbloses O2+ und die rubinroten Verbindungen O2+RuF6- und O2+PtF6- kristallisieren isotyp in der Raumgruppe Ia3-Th7 (Nr. 206) mit a = 1016(1) pm (Sb), a = 1002,6(9) pm (Ru) und a = 1003,6(9) pm (Pt), Z = 8. Gelbes O2+AuF6- kristallisiert trigonal-rhomboedrisch in der Raumgruppe R3-D326 (Nr. 148) mit a = 775,9(3) pm, c = 711,7(4) pm, Z = 3.
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 597 (1991), S. 9-18 
    ISSN: 0044-2313
    Keywords: Alkali fluoro palladate(II) ; preparation ; single crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Fluoropalladates(II) M2[PdF4] (M = Na, K) and K2RbPdF5For the first time bright yellow single crystals M2[PdF4] (M = Na, K) have been obtained and their structure determined. K2[PdF4] crystallizes monoclinic, space group C2/m-C2h3 (No. 12) with a = 975.2(3) pm, b = 597.6(1) pm, c = 420.2(1) pm, β = 92.17(2)° and Z = 2. Structure related Na2[PdF4] crystallizes monoclinic too, but in space group P21/c-C2h5 (No. 14) with a = 340.88(7) pm, b = 561.1(1) pm, c = 999.2(2) pm, β = 93.97(2)° and Z = 2. K2RbPdF5, yellow, crystallizes tetragonal with a = 724.9(1) pm, c = 627.9(1) pm, Z = 2 and is isotypic with Rb2CsPdF5 (space group P4/mbm-D4h5, No. 127), an ordered structure variant of the Rb3PdF5-type [1].
    Notes: Erstmals konnten leuchtend gelbe Einkristalle M2[PdF4] (M = Na, K) dargestellt und ihre Struktur bestimmt werden. K2[PdF4] kristallisiert monoklin, R.G. C2/m-C32h (Nr. 12) mit a = 975,2(3) pm, b = 597,6(1) pm, c = 420,2(1) pm, β = 92,17(2)° und Z = 2. Strukturverwandtes Na2[PdF4] kristallisiert ebenfalls monoklin, jedoch in der R.G. P21/c-C2h5 (Nr. 14) mit a = 340,88(7) pm, b = 561,1(1) pm, c = 999,2(2) pm, β = 93,97(2)°und Z = 2. K2RbPdF5, gelb, kristallisiert tetragonal mit a = 724,9(1) pm, c = 627,9(1) pm, Z = 2 und ist isotyp zu Rb2CsPdF5 (R.G. P4/mbm-D4h5, Nr. 127), einer geordneten Strukturvarianten des Rb3PdF5-Typs [1].
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1431-1440 
    ISSN: 0044-2313
    Keywords: Fluoroplatinates(IV) ; preparation ; single crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Fluoroplatinates(IV) of the Lanthanides LnF[PtF6] (Ln = Pr, Sm, Gd, Tb, Dy, Ho, Er)For the first time fluorides LnF[PtF6] (Ln = Pr, Sm, Gd, Tb, Dy, Ho, Er), all yellow have been obtained. From single crystal data they crystallize monoclinic, space group P21/n-C2h5 (No. 14), Z = 4, Pr: a = 1 125.77(19) pm, b = 559.04(7) pm, c = 910.27(17) pm, β = 107.29(1)°; Sm: a = 1 114.63(31) pm, b = 552.70(12) pm, c = 898.02(20) pm, β = 107.24(2)°; Gd: a = 1 112.12(15) pm, b = 551.22(7) pm, c = 891.99(11) pm, β = 107.09(1)°; Tb (Powder data): a = 1 108.88(20) pm, b = 552.71(9) pm, c = 889.56(16) pm, β = 107.30(1)°; Dy: a = 1 100.28(23) pm, b = 547.77(8) pm, c = 882.41(13) pm, β = 107.32(1); Ho: a = 1 099.11(16) pm, b = 546.16(7) pm, c = 879.45(15) pm, β = 107.34(1)°; Er: a = 1 095.10(16) pm, b = 544.82(10) pm, c = 874.85(14) pm, β = 107.37(1)°.
    Notes: Erstmals dargestellt wurden Fluoride LnF[PtF6] (Ln = Pr, Sm, Gd, Tb, Dy, Ho, Er), alle gelb. Nach Einkristalluntersuchungen kristallisieren diese monoklin in der Raumgruppe P21/n-C2h5 (Nr. 14), Z = 4, Pr: a = 1 125,77(19) pm, b = 559,04(7) pm, c = 910,27(17) pm, β = 107,29(1)°; Sm: a = 1 114,63(31) pm, b = 552,70(12) pm, c = 898,02(20) pm, β = 107,24(2)°; Gd: a = 1 112,12(15) pm, b = 551,22(7) pm, c = 891,99(11) pm, β = 107,09(1)°; Tb (Pulverdaten): a = 1 108,88(20) pm, b = 552,71(9) pm, c = 889,56(16) pm, β = 107,30(1)°; Dy: 1 100,28(23) pm, b = 547,77(8) pm, c = 882,41(13) pm, β = 107,32(1)°; Ho: a = 1 099,11(16) pm, b = 546,16(7) pm, c = 879,45(15) pm, β = 107,34(1)°; Er: a = 1 095,10(16) pm, b = 544,82(10) pm, c = 874,85(14) pm, β = 107,37(1)°. Im Gegensatz zu älteren Befunden liegt die Raumgruppe P21/n-C2h5 (Nr. 14) mit einem verdoppelten Zellvolumen vor.
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  • 5
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Helvetica Chimica Acta 56 (1973), S. 310-320 
    ISSN: 0018-019X
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: New preparative routes to the isomeric damascones (2, 4 and 9) and β-damascenone (1) starting from the readily accessible ionone isoxazoles [11] are described. γ-Damascone (9) was prepared from 10 following the Büchi-Vederas transformation [11], while α- and β-damascone (4 and 2) were obtained as the end products of the reaction sequence: β-aminodamascones [11]→β-ketodihydrodamascones (20 and 21) → β-hydroxydihydrodamascones (24 and 25). β-Damas cenone (1), however, is formed from the epoxides of β-ionone isoxazole (14) by Birch reduction followed by treatment with acid.The unusual behaviour towards metal hydrides of the crotonyl group in the damascones and damascenones is described.
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  • 6
    ISSN: 0018-019X
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: (-)-cis-Pulegol (1) and (+)-pulegone (2) readily add one mole of oxygen on dyesensitized photo-oxygenation in solution, forming almost exclusively allyl hydroperoxides.The product distributions and structures of the peroxides (B-E) have been derived from analysis of their reduction products. Compound 1 yielded only the diols 4, 5 and 6, besides the epoxyketones 7 and 8 formed directly from the hydroperoxide C (proportions of 4-8, ∼21:56:13:4:6), while 2 gave the keto-alcohols 9,10 and 11 (∼80:6:14) as the sole products.The course of addition of O2(1Δg) on 1 and 2 was found in all cases to be independent of solvent and photosensitizer.
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  • 7
    ISSN: 0018-019X
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The oxirane derivative 2a of β-damascone which appears as the main product in the photo-oxygenation of β-damascol (1a), besides the α-hydroxy-hydroperoxides B and C, can easily be transformed into β-damascenone (8) [1] by a sequence of acid catalyzed reactions.The structure and stereochemistry of the photo-oxygenation products of 1 a and its derivatives 1 b and 1 c are determined. The epoxyketone 2 is a secondary product of the unstable allylhydroperoxide A, while ketones 12 and 13 result from an α-hydroxy-hydroperoxide fragmentation of B and C, respectively.
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  • 8
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Journal für Praktische Chemie/Chemiker-Zeitung 311 (1969), S. 912-918 
    ISSN: 0021-8383
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reaktion von 3β-Acetoxy-16α, 17α-epoxy-Δ5-pregnenon-(20) 1 mit Natriumazid und Schwefelsäure in Dimethylsulfoxid führt zu 3β-Acetoxy-16β-azido-17α-hydroxy-17β-methyl-D-homo-Δ5-androstenon-(17a) 2a. Die Strukturaufklärung der Verbindung 2a wird beschrieben. Durch Reduktion der Azidogruppe mit Hydrazinhydrat/RANEY-Nickel werden Aminoverbindungen erhalten. Die Überführung der 3β-Acetoxy-Δ5-16β-azido- und -aminoverbindungen in die entsprechenden 3-Keto-Δ4-Derivate wird beschrieben.
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  • 9
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 616 (1992), S. 7-13 
    ISSN: 0044-2313
    Keywords: Alkali fluoro palladates(II) ; preparation ; single crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On Complex Fluorides of Divalent PalladiumFor the first time single crystals of the new compounds RbPdPdF5, KPdPdF5, and K2CsPdF5 have been obtained. Orange brown RbPdPdF5 crystallizes orthorhombic, space group Imma-D2h28 (No. 74) with a = 633.6(1) pm, b = 765.5.(1) pm, c = 1067.5(1) pm and Z = 4 and is isotypic with CsPdPdF5 [1]. Structure related KPdPdF5 (also orange brown) crystallizes orthorhombic too, but in space group Pnma-D2h16 (No. 62) with a 614.12(9) pm, b = 748.7(1) pm, c = 1065.0(2) pm and Z = 4. K2CsPdF5, light yellow, crystallizes tetragonal with a = 736.3(1) pm, c = 628.0(1) pm, Z = 2, and is isotypic with Rb2CsPdF5 (space group P4/mbm—D4h5 Nr. 127), an ordered structure variant of the Rb3PdF5-Type [1].
    Notes: Neu dargestellt wurden RbPdPdF5, KPdPdF5 und K2CsPdF5, alle in Form von Einkristallen. Orangebraunes RbPdPdF5 kristallisiert orthorhombisch, R. G. Imma-D2h28 (Nr. 74) mit a = 633,6(1) pm, b = 765,5(1) pm, c = 1067,5(1) pm und Z = 4 und ist isotyp zu CsPdPdF5 [1]. Strukturverwandtes KPdPdF5 (ebenfalls orange-braun) kristallisiert gleichfalls orthorhombisch, jedoch in der R. G. Pma—D2h16 (Nr. 62) mit a = 614,12(9) pm, b = 748,7(1) pm, c = 1065,0(2) pm und Z = 4. K2CsPdF5, hellgelb, kristallisiert tetragonal mit a = 736,3(1) pm, c = 628,0(1) pm Z = 2, ist isotyp zu Rb2CsPdF5 (R. G. P4/mbm—D4h5) (Nr. 127) und somit ein weiterer Vertreter der geordneten Strukturvariante des Rb3PdF5-Typs [1].
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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 189-192 
    ISSN: 0044-2313
    Keywords: Fluoropalladates(II) ; preparation ; single crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of LiPdAlF6 and PdZrF6.For the first time single crystals of the new compounds LiPdAlF6 and PdZrF6 have been obtained. LiPdAlF6 (blue) crystallizes trigonal, space group P31c - D3d2 (No. 163; LiCaAlF6-type [2]), in an ordered structure variant of the Li2[ZrF6]-structure [3], with a=497.21(9) pm, c=914.0(9) pm and Z=2. PdZrF6 (also blue) is isotypic with LiSbF6 [4] and crystallizes trigonal-rhomboedric with a=552,3(1) pm, c=1 447,5(4) pm, space group R 3 - C3i2 (No. 148) and Z=3.
    Notes: Neu dargestellt wurden LiPdAlF6 und PdZrF6, beide in Form von Einkristallen. Blaues LiPdAlF6 kristallisiert trigonal im LiCaAlF6-Typ [2], einer Ordnungsvariante der Li2[ZrF6]-Struktur [3], in der Raumgruppe P31c - D3d2 (Nr. 163) mit a=497,21(9) pm, c=914,0(9) pm und Z=2. PdZrF6 (hellblau) kristallisiert trigonal-rhomboedrisch in der Raumgruppe R 3 - C3i2(Nr. 148) mit a=552,3(1) pm, c=1 447,5(4) pm und Z=3 (isotyp zu LiSbF6 [4]).
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