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  • 1
    Electronic Resource
    Electronic Resource
    Springer
    Monatshefte für Chemie 127 (1996), S. 461-468 
    ISSN: 1434-4475
    Keywords: Coordination of As(III) and Sb(III) ; Structure ; Enantiomers
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Summary Arsen-tris(2,2-dimethylpropionate) (1) crystallizes monoclinic in the space group P21/n witha=926.2,b=2158.6,c=983.7 pm, β=94.92°, andZ=4. As has a coordination number of 3+3. Antimony tripropionate (2) crystallizes monoclinic in the space group P21/c witha=930.2,b=863.0,c=1575.2 pm, β=90.27, andZ=4. The molecules are bridged to chains; therefore, Sb reaches the coordination number 3+3 (+3).
    Notes: Zusammenfassung Arsen-tris(2,2-dimethylpropionat) (1) kristallisiert monoklin in der Raumgruppe P21/n mita=926.2,b=2158.6,c=983.7 pm, β=94.92° undZ=4. As hat gegenüber O die Koordinationszahl 3+3. Antimontripropionat (2) kristallisiert monoklin in der Raumgruppe P21/c mita=930.2,b=863.0,c=1575.2 pm, β=90.27 undZ=4. Die Moleküle sind intermolekular zu Ketten verknüpft, wodurch Sb die Koordinationszahl 3+3 (+3) erreicht.
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  • 2
    Electronic Resource
    Electronic Resource
    Springer
    Monatshefte für Chemie 127 (1996), S. 1215-1220 
    ISSN: 1434-4475
    Keywords: Coordination of As(III) ; Structure ; Stereoisomeres
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Summary Arsenictris(trifluoroacetate) (1) crystallizes monoclinic in the space group Cc witha=1229.3,b=1697.9,c=1243.5 pm, β=110.01°, andZ=8. The trifluoroacetic acid ions acts as chelating ligands. Additionally they are bridging crystallographic independent molecules. As has a coordination number of 3+3(+2). The unit cell contains two sets of chirameres.
    Notes: Zusammenfassung Arsen-tris(trifluoracetat) (1) kristallisiert monoklin in der Raumgruppe Cc mita=1229.3,b=1697.9,c=1243.5 pm, β=110.01° undZ=8. Die Trifluoracetatanionen fungieren gegenüber As als zweizähnige Liganden und verknüpfen die beiden kristallographisch unabhängigen Moleküle zusätzlich intermolekular. As erreicht dadurch gegenüber O die Koordinationszahl 3+3(+2). Die Elementarzelle enthält zwei Sätze von chirameren Molekülen.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Springer
    Monatshefte für Chemie 126 (1995), S. 1045-1050 
    ISSN: 1434-4475
    Keywords: Coordination of Sb(III) ; Structure ; Enantiomers
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Summary The Δ isomer of (C6H5CO2)3Sb crystallizes rhombohedrally (hexagonal axes) in the space group R3 witha=1944.0 pm,c=422.3 pm, andZ=3. The molecules are stacked parallel to 001; Sb has a coordination number of 3+3 (Sb-O: 208 and 256 pm, resp.).
    Notes: Zusammenfassung Das Δ-Isomer des Antimontribenzoats kristallisiert rhomboedrisch (hexagonale Aufstellung) in der Raumgruppe R3 mita=1944.0 pm,c=422.3 pm undZ=3. Die Moleküle sind parallel zu 001 gestapelt. Sb hat gegenüber O die Koordinationszahl 3+3 (Sb-O: 208 bzw. 256 pm).
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 1799-1804 
    ISSN: 0044-2313
    Keywords: 1,4,2λ5,5λ5-Dioxadiphosphorinane ; NMR spectra ; Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: P,P′-(2,5-Dihydroxy-3,6-dimethyl-2,5-dioxo-2λ5,5λ5-[1,4,2,5]dioxadiphosphinane-2,5-diyl)-bis-phosphonic AcidThe tetrahydrate 1 of the title compound crystallizes in the monoclinic space group P21/c with a = 845.8, b = 1 098, c = 981.7 pm, β = 113.02° and Z = 2. The anions of the oxonium compound (H3O+ · H2O)2(C4H10O12P42-) are layered by hydrogen bridges. The 1H, 13C and 31P NMR spectra (4 and 5 spin systems) are discussed.
    Notes: C4H12O12P4 · 4 H2O (1), das Tetrahydrat der Titelverbindung, kristallsiert monoklin in der Raumgruppe P21/c mit a = 845,8, b = 1 098, c = 981,7 pm, β = 113,02° und Z = 2. 1 liegt als Oxoniumsalz (H3O+ · H2O)2(C4H10O12P42-) vor, in dem die Anionen über H-Brücken zu Schichten verknüpft sind. Die 4- und 5-Spinsysteme der 1H-, 13C- und 31P-NMR-Spektren werden detailliert analysiert.
    Additional Material: 4 Ill.
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1038-1046 
    ISSN: 0044-2313
    Keywords: Binuclear antimony(V) complexes ; structure ; dynamics ; NMR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: d, h-μ-Benzylalkoxophosphonato-e-μ-alkoxo-f-μ-oxo-bis[trichloroantimony(V)] CompoundsThe binuclear antimony(V) complexes Cl3Sb(O)[R3(R1O)PO2](OR2)SbCl3 1 - 6 with R1 = R2 = CH3, C2H5 and R3 = C6H5CH2, (CH3)3C6H2CH2 in solution slowly exchanges the R2 groups between the oxygen atoms of the Sb2O2 ring. The SbOPOSb ringsystem makes rapid pseudorotation. The isomeres are detected by nmr spectroscopy. 1 (R1 = R2 = CH3) crystallizes in the orthorhombic space group Pnma with a = 1247.0, b = 1324.1, c = 1207.9 pm and Z = 4. 2 (R1 = CH3, R2 = C2H5) and 5 (R1 = R2 = CH3, R3 = (CH3)3 · C6H2CH2) crystallizes triclinic in the space group P-1 with a = 984.1, b = 1026.7, c = 1079.9 pm, α = 87.93, β = 75.70, γ = 87.62° and Z = 2 and a = 1164.6, b = 1296.9, c = 1712.9 pm, α = 109.9, β = 96.3, γ = 100.2° and Z = 4 resp., with two crystallographically independent molecules in the asymmetric unit.
    Notes: Die zweikernigen Antimon(V)-Komplexe Cl3Sb(O)[R3(R1O)PO2](OR2)SbCl3 1 bis 6 mit R1 = R2 = CH3, C2H5 und R3 = C6H5CH2, (CH3)3C6H2CH2 tauschen bei RT in Lösung langsam die R2-Gruppen aus. Daneben erfolgt rasches Umklappen des SbOPOSb-quasi-Fünfringes. Die Isomerenbildung wird NMR-spektroskopisch nachgewiesen. 1 (R1 = R2 = CH3) kristallisiert orthorhombisch in der Raumgruppe Pnma mit a = 1247,0, b = 1324,1, c = 1207,9 pm und Z = 4. 2 (R1 = CH3, R2 = C2H5) und 5 (R1 = R2 = CH3, R3 = (CH3)3C6H2CH2) kristallisieren triklin in der Raumgruppe P-1 mit a = 984,1, b = 1026,7, c = 1079,9 pm, α = 87,93, β = 75,70, γ = 87,62° und Z = 2 bzw. a = 1164,6, b = 1296,9, c = 1712,9 pm, α = 109,9, β = 96,3, γ = 100,2° und Z = 4 mit zwei kristallographisch unabhängigen Molekülen in der asymmetrischen Einheit.
    Additional Material: 4 Ill.
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1168-1174 
    ISSN: 0044-2313
    Keywords: Sulfoximide ; Sulfoximidium Salts ; Structure ; Hydrogenbonding ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Sulfoximide and Sulfoximidium Salts - Structures and Hydrogen BondingIn the solid state dimethylsulfoximide (1) (orthorhombic; space group Pbca; a = 577.8, b = 931.2 and c = 1645.6 pm) makes intermolecular N—H ≡ N hydrogen bonds. The hydrogen halide salts (CH3)2S(O)NH2+Hal- ((2), Hal-=Cl-; (4), Hal-=Br-) reacts with metal halides to yield (CH3)2S(O)NH2+MHalyn- with the complex anions ((5), MHalyn-=SbCl4-; (6), MHalyn-=SbCl52-; (7), MHalyn-=SbCl6-; (8), MHalyn-=SbBr52-; (9), MHalyn-=AlCl4-). 2 crystallizes from ethanol (96%) as [(CH3)2S(O)NH2+Cl-]2 · H2O (3). The structures of 3 (monoclinic; space group P21/c; a = 917.0, b = 1344.7, c = 1080.8 pm and β = 103.8°; Z = 10), 4 (orthorhombic; space group Pbcn; a = 1028.9, b = 1132.6, c = 1074.1 pm; Z = 8) and 6 (monoclinic; space group C2/c; a = 2041.1, b = 1101.4, c = 3365.6 pm and β = 153.8°; Z = 8) are determined by X-ray analysis. In 6 Sb is coordinated in a distorted octahedra by 6 Cl in three short (mean 245,5 pm; SbCl3) and three long distances (291 to 299 pm; Cl-). Two of the chloride ions connect the Sb atoms to infinite Sb … Cl … Sb chains. Except for 7 and 9 there are bridges between the NH2 groups and the halide ions. The NH valence vibrations are discussed in view of hydrogen bonding.
    Notes: Im festen Dimethylsulfoximid (1) (orthorhombisch; Raumgruppe Pbca; a = 577,8, b = 931,2 und c = 1645,6 pm) sind zwischen den Imidgruppen N—H … N-Brückenbindungen ausgebildet. Die mit HHal darstellbaren Salze (CH3)2S(O)NH2+Hal- ((2), Hal-=Cl-; (4), Hal-=Br-) reagieren mit MHalx zu (CH3)2S(O)NH2+MHalyn- ((5), MHalyn-=SbCl4-; (6), MHalyn-=SbCl52-; (7), MHalyn-=SbCl6-; (8), MHalyn-=SbBr52-; (9), MHalyn-=AlCl4-). 2 kristallisiert aus 96% Ethanol als [(CH3)2S(O)NH2+Cl-]2 · H2O (3). Die Strukturen von 3 (monoklin; Raumgruppe P21/c; a = 917,0, b = 1344,7, c = 1080,8 pm und β = 103,8°; Z = 10), 4 (orthorhombisch; Raumgruppe Pbcn; a = 1028,9, b = 1132,6, c = 1074,1 pm; Z = 8) und 6 (monoklin; Raumgruppe C2/c; a = 2041,1, b = 1101,4, c = 3365.6 pm und β = 153,8°; Z = 8) wurden bestimmt. In 6 ist Sb verzerrt oktaedrisch von 6 Cl in drei kurzen (im Mittel 245,5 pm; SbCl3) und drei langen Abständen (291 bis 299 pm; Cl-) umgeben. Zwei der lang gebundenen Cl-Ionen verknüpfen die Sb-Atome zu unendlichen Sb … Cl … Sb-Ketten. Die NH2-Gruppen der Kationen bilden außer in 7 und in 9 H—Brückenbindungen zu den Halogenidionen. Die NH-Valenzschwingungen werden im Hinblick auf die Wasserstoffbrückenbindungen diskutiert.
    Additional Material: 7 Ill.
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 617 (1992), S. 72-78 
    ISSN: 0044-2313
    Keywords: Ionic antimony(III)-dithiocarbamates ; syntheses ; structure ; vibrational and mass spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: DimethylaminodithiocarbamatostibanesThe Halogeno-bis(dimethylaminodithiocarbamato)stibanes (dtc)2SbCl 2 and (dtc)2SbBr 3 are prepared from (dtc)3Sb 1. Reaction of 2 and 3 resp. with CF3SO3SiMe3 yields the ionic compounds (dtc)2Sb+CF3SO3-4 and (dtc)2Sb+]2Br-(CF3SO3-) CH2Cl2 5 by elimination of Me3SiHal. The molecular structure of 4 is determined by X-ray analysis. The vibrational and mass spectra of 1-5 are reported and briefly discussed.
    Notes: Die Synthese der Halogeno-bis(dismethylaminodithiocarbamato)stibane (dtc)2SbCl 2 und (dtc)2SbBr 3 aus (dtc)1 wird beschrieben. Umsetzungen von 2 bzw. 3 mit CF3SO3SiMe3 führen unter Me3SiHal-Abspaltung zu den salzartigen Verbindungen (dtc)2Sb+CF3SO- 3 4 bzw. [(dtc)2Sb+]2Br-(CF3SO3-). CH2Cl2 5. 4 wird röntgenstrukturanalytisch charakterisiert. Die Schwingungs- und Massenspektren von 1-5 werden diskutiert.
    Additional Material: 1 Ill.
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  • 8
    ISSN: 0044-2313
    Keywords: 1,4,2λ5,5λ5-Dioxadiphosphorinane ; NMR-Spectra ; Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: P,P′-(2,5-Dimethoxy-3,6-dimethyl-2,5-dioxo-2λ5,5λ5-[1,4,2,5]dioxadiphosphinane-2,5-diyl)-bis-phosphonic acid tetramethylesterThe title compound 1 is formed by reaction of the corresponding phosphonic acid 2 and orthoformicacidmethylester as a mixture of four stereoisomeres. The RRSS isomer was separated. It crystallizes in the triclinic space group P -1 with a = 649.2 pm, b = 976.1 pm, c = 1 571.7 pm, α = 80.9°, β = 88.1°, γ = 78.6° and Z = 2. The 31P and 13C NMR spectra (4 and 5 spin systems) are discussed.
    Notes: Die Titelverbindung 1 entsteht aus der zugrundeliegenden Phosphonsäure 2 und Orthoameisensäuremethylester als Gemisch aus vier Stereoisomeren, von denen das RRSS-Isomer präparativ abgetrennt werden konnte. Dieses kristallisiert triklin in der Raumgruppe P -1 mit a = 649,2 pm, b = 976,1 pm, c = 1 571,7 pm, α = 80,9°, β = 88,1°, γ = 78,6° und Z = 2. Die 4- und 5-Spinsysteme der 31P- und 13CNMR-Spektren werden analysiert.
    Additional Material: 2 Ill.
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  • 9
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1633-1638 
    ISSN: 0044-2313
    Keywords: (CH3)2S derivatives ; Structure ; Spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: (CH3)2SBr2 - Reactions and Structures(CH3)2SBr2 (1) is a donor acceptor complex (8-S-3 + 10-Br-2) which reacts with (CH3)2S(=O)NSi(CH3)3 to yield [(CH3)2S(O)=N—S(CH3)2]+Br- (2). With SbBr3 (CH3)2SBr+SbBr4- (3) can be isolated. 1 crystallizes monoclinic in the space group P21/c with a = 733.8, b = 734.2, c = 1132.7 pm, β = 92.8° and Z = 4. 2 crystallizes in the orthorhombic space group Pnma with a = 967.2, b = 793.3, c = 1168.3 pm and Z = 4. The SBr and BrBr force constants of 1 are compared with those of S2Br2, 3 and Br2 resp. The nmr and mass spectra of 1 and 2 are communicated.
    Notes: (CH3)2SBr2 (1) ist ein (8-S-3 + 10-Br-2) Donor-Akzeptor-Komplex(8-S-3 + 10-Br-2) bedeutet: acht Valenzelektronen am S-Atom, das von drei Bindungspartnern umgeben ist, und zehn Valenzelektronen am Br-Atom, das zwei Bindungspartner hat; s.: S. W. Perkins, J. C. Martin, A. J. Arduengeo III, W. Lau, A. Alegria, J. K. Kochi, J. Am. Chem. Soc. 1980, 102, 7753. und reagiert mit (CH3)2S(=O)NSi(CH3)3 zu [(CH3)2S(O)=N—S(CH3)2]+Br- (2), mit SbBr3 zu (CH3)2SBr+SbBr4- (3). 1 kristallisiert monoklin (P21/c) mit a = 733,8, b = 734,2, c = 1132,7 pm, β = 92,8° und Z = 4. 2 kristallisiert orthorhombisch in der Raumgruppe Pnma mit a = 967,2, b = 793,3, c = 1168,3 pm und Z = 4. Die SBr- und BrBr-Kraftkonstanten von 1 werden mit denen von S2Br2 und 3 bzw. Br2 verglichen. Die NMR- und Massenspektren von 1 und 2 werden kurz diskutiert.
    Additional Material: 2 Ill.
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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 2029-2033 
    ISSN: 0044-2313
    Keywords: Tetranuclear antimony(V) complex ; structure ; NMR, IR, Raman, mass spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Trichloroantimony(V) MethylphosphonateThe tetrameric trichloroantimony(V) methylphosphonate (1) is synthezised by reaction of antimony(V) chloride and methanephosphonic acid. It crystallizes monoclinic in the space group P21/a with a = 1 813.6 pm, b = 1 024.0 pm, c = 1 831.1 pm, β = 100.5° and Z = 4. In the unit cell there are chiral molecules which lose their chirality in solution. In solution they are dynamical and have an other conformation as in the solid state. The NMR, vibrational and mass spectra are discussed.
    Notes: Tetrameres Trichloroantimon(V)-methylphosphonat (1) entsteht aus Antimon(V)chlorid und Methanphosphonsäure. Es kristallisiert monoklin in der Raumgruppe P21/a mit a = 1 813,6 pm, b = 1 024,0 pm, c = 1 831,1 pm, β = 100,5° und Z = 4. In der Einheitszelle liegt 1 in Form spiegelbildlicher Moleküle vor, die in Lösung ihre Chiralität verlieren und eine andere Konformation als im Feststoff haben. Die NMR-, Schwingungs- und Massenspektren werden diskutiert.
    Additional Material: 2 Ill.
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