The Electron Diffraction Investigation of the Molecular Structures of Hydrogen Disulfide, Dimethyl Disulfide and Sulfur Dichloride

Stevenson, D. P.; Beach, J. Y.

doi:10.1021/ja01279a011

Cited by 59 publications

(15 citation statements)

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“…Although the C-S bond distance is insignificantly shorter than that of 1.81 /i given in the table of covalent radii (Pauling, 1942, p. 164), our value is the same as that found in the electron-diffraction studies of dimethyl disulfide (Stevenson & Beach, 1938) and dimethyl trisulfide (Donohue & Schomaker, 1948), and is greater than that found in thiophene (Schomaker & Pauhng, 1939). We cannot be sure that the observed C=C distance is really significantly shorter than the 'normal' C =C distance because of our relatively large probable errors.…”

Section: Discussionsupporting

confidence: 61%

The crystal and molecular structure of 1,4-dithiadiene

Howell¹,

Curtis²,

Lipscomb³

1954

Acta Crystallogr

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Section: Discussionsupporting

confidence: 61%

The crystal and molecular structure of 1,4-dithiadiene

Howell¹,

Curtis²,

Lipscomb³

1954

Acta Crystallogr

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“…2.04 A in formamidinium disulphide ion J Foss, Johnsen & Tverdten, 1958) ide and dithiolanecarboxylic acid, 2.09 and 2.10, Foss & Tjmosland, 1958a, b). The mean value of the angles SSC (98°), as could be expected, is intermediate between the angles found in non-cyclic disulphides (dimethyl disulphide, 107 °, Stevenson & Beach, 1938;bistrifluoromethyl disulphide, 105 °, Bowen, 1954; formamidinium disulphide ion, 104 °, Foss et al, 1958) and those in five-membered cyclic disulphides (e.g. 92 ° in thiuret disulphide ion).…”

Section: Conformation and Configurationsupporting

confidence: 52%

The structure of the methylene dibromide adduct of sporidesmin at –150°C

Fridrichsons¹,

Mathieson²

1965

Acta Cryst

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The structure of sporidesmin, the causative agent of facial eczema in sheep, isolated by Synge & White from cultures of the fungus Pithomyces chartarum (previously Sporidesmium bakerii Syd.) has been determined from its CH2Br2 adduct.The compound crystallizes in the orthorhombic space group P212~21 with cell dimensions a = 9.681, b= 10.629, c= 23.358/~ at -150 °C. Data were collected for 0-7 layers about a and the 0-layer about b. The positions of the Br atoms (occupied only 0"65) and also the S atoms were determined from normal and generalized Patterson projections and Harker sections. Two three-dimensional electron-density distributions with two-dimensional e0 and Ae distributions led to the structure (I), corresponding to the formula CI8H2006N3S2CI. 0"65 CH2Br2.FI OH

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“…118.7 1-3 C(4)--C(5)--C(6) 120.9 1.5 C(5)--C(6)--C (7) 120.1 1.4 C(6)--C(7)--C(2) 119-3 1-1 C(8)--C(9)--C(10) 119.7 1-2 C(8)--C(9)--C (14) 122-1 1.2 C(10)-C(9)-- C(14) 117.9 1.2 C(9)--C(10)-C(11) 117-8 1.2 C(10)-C(ll)- C(12) 123-4 1.3 C(11)-C(12)- C(13) 116.9 1-3 C(12)-C(13), C(14) 120.5 1-5 C(13)-C(14)- C(9) 123-3 1-3 calculated by the method of Schomaker, Waser, Marsh & Bergman (1959) and are given in Table 8. The central part of the molecule C(1)--S(1)-S(2)-C(8) adopts a skewed non-planar configuration like that found in hydrogen peroxide (Abrahams, Collin & Lipscomb, 1951), hydrogen disulphide (Stevenson & Beach, 1938;Wilson & Badger, 1949), dimethyl disulphide (Stevenson & Beach, 1938) and diphenyl disulphide (Lee & Bryant, 1969). The observed S-S bond length of 2.02/~ may have 23 % of double bond character if the Pauling (1960) value of 2.08 A is taken as the length of a pure single bond.…”

Section: Discussionmentioning

confidence: 94%

The crystal and molecular structure of dibenzyl disulphide. The refinement of a structure with high correlation coefficients

Lee¹,

Bryant²

1969

Acta Crystallogr Sect B

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The crystal structure of dibenzyl disulphide, C6Hs-CH2-S-S-CH2-C6Hs, has been determined from three-dimensional X-ray diffraction data. The crystals are monoclinic and belong to the space group Cc.The unit cell has dimensions a= 13.46, b= 8.23, c= 11.29/~, ~= y= 90 °, fl= 99°30 ', and contains four molecules. Difficulty was exl~erienced because of a very strong tendency to twinning of the crystals, often only detected on high-layer line photographs. Positional and temperature factor parameters for sulphur and carbon atoms have been refined by Fourier, block-diagonal least squares and finally by full-matrix least squares. Refinement was unusually difficult because of large correlation coefficients between parameters, associated with a pseudo twofold axis of symmetry in the molecule. In the final stages, hydrogen atoms were included in fixed positions. The final R value based on 867 independent observed reflexions was 7.9%. The precise chemical nature of the S-S bond is examined. ExperimentalA sample of dibenzyl disulphide was recrystaUized from ethanol and gave colourless plate-like crystals, which showed straight extinction parallel to the plate edges when viewed under the polarizing microscope. The density of the crystals was measured by the method of flotation in aqueous solutions of potassium iodide and found to be 1.28 g.cm -3.Considerable difficulty was experienced in selecting a suitable crystal for X-ray analysis since many crystals which appeared suitable after optical and preliminary X-ray examination proved to be twinned when high layer line Weissenberg photographs were taken. A single crystal of dimensions 0.025 x 0.025 x 0.015 cm was eventually used for X-ray analysis, and threedimensional equi-inclination Weissenberg data were collected for the hkO, hkl...hk8, hOl and hll zones.The intensities of 867 independent reflexions were collected photographically, measured visually and converted to [F] 2 and [FI by applying Lorentz and polarization corrections. In view of the small crystal size and the low absorption coefficient, corrections for absorption were considered unnecessary. No correction was made for extinction. Reflexions too weak to be observed were ignored. Crystal data (C6H5. CH2)2S2, M = 246.3 . Monoclinic, a= 13.46, b = 8.23, c = 11.29A_, all + 0.02~ = ), = 90 °, fl = 99 ° 30' + 30'. U= 1233.5~ 3, Z=4, Din= l'28g.cm -3, De= l'32g.cm -3 F000 = 520, Cu K~, 2 = 1.542 A, ~ = 36 cm -1 .Absent reflexions: hkl when h+k is odd, hOl when l is odd (and when h is odd), 0k0 when k is odd.These absences restrict the space group to Cc or C2/c, but the former was confirmed by the pyroelectric test, the statistical test and by the structure refinement. Structure analysisThere are four molecules in the unit cell, and for the space group Cc these must occupy the general positions (x,y,z); (x,-y,½+z); (½+x,½+y,z) and (½+x, ½-Y, ½+z). Patterson summations were performed with hkO and hOl data, but these were not interpreted in terms of a satisfactory trial structure because of the diffuse nature of the peaks. Th...

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The Electron Diffraction Investigation of the Molecular Structures of Hydrogen Disulfide, Dimethyl Disulfide and Sulfur Dichloride

Cited by 59 publications

References 0 publications

The crystal and molecular structure of 1,4-dithiadiene

The crystal and molecular structure of 1,4-dithiadiene

The structure of the methylene dibromide adduct of sporidesmin at –150°C

The crystal and molecular structure of dibenzyl disulphide. The refinement of a structure with high correlation coefficients

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