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  • 1
    ISSN: 0044-2313
    Keywords: N,N-Dichloromethylsulfonammonium salts ; crystal structure of CH3S(O)2NCl2 ; vibrational spectra ; 1H ; 13C ; 19F NMR ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New N,N-Dichloromethylsulfonammonium Salts CH3S(O)2NCl2X+MF6- (X = CH3, Cl, F; M = As, Sb) and Crystal Structure of CH3S(O)2NCl2The preparations of new dichlorammonium salts CH3S(O)2NCl2X+MF6- (X = CH3, Cl, F; M = As, Sb) and of CH3S(O)2NCl2 by oxidative halogenation respectively methylation are reported. The thermolabil compounds are characterized by IR, Raman, 1H, 13C, 19F NMR spectroscopy. N,N-Dichlormethylsulfonamid CH3S(O)2NCl2 crystallizes at 173(1) K in the orthorhombic space group Pnma with a = 615.1(3) pm, b = 937.3(5) pm, c = 970.3(5) pm and Z = 4.
    Notes: Die Darstellung einer Reihe von Dichlor ammoniumsalzen des Typs CH3S(O)2NCl2X+MF6- (X = CH3, Cl, F; M = As, Sb) wird angegeben. Die Salze werden durch oxidative Halogenierung bzw. Methylierung von CH3S(O)2NCl2 erhalten. Die Charakterisierung der thermolabilen Verbindungen erfolgte mittels IR-, Raman-sowie Multikern-NMR-Spektroskopie. Die Einkristallröntgenstrukturanalyse von N,N-Dichlormethylsulfonamid CH3S(O)2NCl2 bei 173(1) K ergab: orthorhombische Raum gruppe Pnma mit a = 615,1(3) pm, b = 937,3(5) pm, c = 970,3(5) pm und Z = 4.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 0268-2605
    Keywords: Organotin ; 2-mercaptopyridine ; pyridine-2-thiolato complexes ; Mössbauer ; IR ; NMR ; crystal structure ; Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Diorganotin(IV) derivatives of 2-mercaptopyridine (HSPy), R2Sn(SPy)2, R2SnCl(SPy) (R = Me, iPr, nBu, tBu, Cy, Ph) and Cy2SnBr(SPy), were obtained from R2SnX2 (X = Cl, Br) and NaSPy.Ph2SnCl(SPy) crystals, as determined by singlecrystal X-ray diffraction, are monoclinic in the space group P21/n. Tin forms with the bidentate SPy ligand a four-membered chelate ring with a short NSnS bite angle of 64.8(1)° leading to a heavily distorted trigonal-bipyramidal environment about tin. Apical Cl-Sn-N angle = 156.1(1)° equatorial C-Sn-C angle = 121.9(2)°. From 119Sn Mössbauer and IR data, analogous structures are inferred for the other solid compounds R2SnX(SPy), and distorted octahedral molecular structures for the solid compounds R2Sn(SPy)2 with R in the trans position, and sulfur atoms and nitrogen-donor atoms each in cis positions. According to IR and 1H, 13C and 119Sn NMR data, the solid-state molecular structures are retained in chloroform solution.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 3
    ISSN: 0268-2605
    Keywords: Organotin ; dipeptides ; structures ; X-ray diffraction ; NMR ; Mössbauer ; infrared ; Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The dipeptide complexes R2SnL listed below have been synthesized: (a) Me2SnL; H2L = glycylalanine (H2GlyAla), glycylvaline (H2GlyVal), glycylmethionine (H2GlyMet), glycyltryptophan (H2GlyTrp), glycyltyrosine (H2GlyTyr); (b) nBu2SnL; H2L = H2GlyAla, H2GlyVal; (c) nBu2SnL.H2O; H2L = glycylglycine (H2GlyGly), H2GlyAla; (d) tBu2SnL; H2L = H2GlyAla, H2GlyVal; (e) tBu2SnGlyGly. H2O; (f) Ph2SnL; H2L = H2GlyAla, H2GlyVal, H2GlyTyr, H2GlyTrp; (g) Ph2Sn(HGlyVal)2. The crystal and molecular structures of nBu2SnGl Val have been determined by single-crystal X-ray diffraction. The polyhedron around tin is a distorted trigonal bipyramid, analogous to that of Et2SnGlyTyr (see Vornefeld et al., Appl. Organomet. Chem., 1992, 6: 75). According to infrared and 119Sn (ΔE parameters) Mössbauer spectroscopic data the R2SnL derivatives can be classified by their solid-state structure into two types which are distinguished by the nature of the axial carboxylate [(i) monodentate, as in nBu2SnGlyVal; (ii) bidentate]. Bonding in R2SnL.H2O and Ph2Sn(HGlyVal)2 has been discussed on the basis of vibrational data. Rationalization of the 119Sn Mössbauer parameters has been attempted by ‘literal’ point-charge model, calculations of ΔE in the structural context described above. According to 13C NMR spectra, compounds Me2SnL are undissociated in methanol solutions, whilst dissociation is inferred for aqueous solutions, probably concerning the carboxyl and amino groups only. Five-coordination in methanol and aqueous solutions has been assumed for Me2Snl from 119Sn NMR chemical shifts. Values of coupling constants |2J(119Sn, 1H)|, determined from 1H NMR spectra, gave estimates of C—Sn—C angles in Me2SnL in the range 128-136° in methanol and aqueous solutions, which correspond to values from 119Sn Mössbauer ΔE parameters (129.6-133.8°). The structural relationship of R2SnL molecules in the solid state and in solution phase has been discussed.
    Additional Material: 2 Ill.
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