The crystal and molecular structure of bis[2-(N,N-dimethylamino)ethyl]disulfide dihydrochloride

Abstract

The crystal and molecular structure of bis- [2-(N,N-dimethylamino)ethyl]disulfide dihydrochloride [alternatively named 2,2"-dithiobis-(N,N-dimethyl)ethylamine dihydrochloride] has been determined crystallographically using the 1972 unique and significant reflections for which 20< 52 °, and refined to an R index of 0.043. Counter methods with graphite monochromatized Mo K~ radiation were employed. All hydrogen atoms were located on a difference Fourier function. Crystals form in the monoclinic space group P21/c with cell dimensions a = 11"646 (2), b = 11"065 (2), c = 12.370 (3) ,~ and/~ = 112.40 (2) °.Estimated standard deviations in non-hydrogen bond lengths range from 0.001 to 0.005 A and, in angles, from 0.11 to 0-26 °. The sulfur-sulfur bond length is found to be 2.037 (1) A with a dihedral angle of 82.4 (2) °. A short intermolecular contact (3.55 A) between a sulfur atom and a chloride ion is observed.

Assembly of a New Family of Mercury(II) Zwitterionic Thiolate Complexes from a Preformed Compound [Hg(Tab)2](PF6)2 [Tab = 4-(Trimethylammonio)benzenethiolate]

“…On the other hand, the Tab−Tab dication has positive charges located on the NMe 3 groups. The S1−S2 bond length and the C1−S1−S2−C10 torsion angle of 9 are 2.034(3) Å and 81.5(3)°, respectively, which are similar to those in [C 8 H 22 N 2 S 2 ]Cl 2 {2.075(5) Å and 82.39(2)°; C 8 H 22 N 2 S 2 = bis[2-( N , N -dimethylamino)ethyl]disulfide dihydrochloride} and {[C 10 H 10 N 2 S 2 ][Cu 2 Cl 6 ][BF 4 ] 2 } n [2.034(3) Å and 81.5(3)°; C 10 H 10 N 2 S 2 = bis(4-pyridinium)disulfide] . In the crystal of 9 , the H-bonding interactions are also abundant.…”

“…Intriguingly, when compound 1 reacted with HAuCl 4 , it only produced an unexpected disulfide compound 9 (Scheme ). The result may be due to the fact that the thiol-to-disulfide conversion could also be completed via oxygen in the presence of certain metal ions. , In our case, the formation of the Tab−Tab dication in 9 may be due to the protonation and dissociation of Tab from 1 in the presence of HAuCl 4 and the subsequent oxidation of TabH + via Au 3+ and/or oxygen in open air. We also carried out the reaction of 1 with a mixture of HAuCl 4 and excessive Tab (1:1:4) in MeOH/MeCN.…”

Crystal and molecular structure of an organic disulfide complex. Chloro[bis[2-[2-(2-pyridylmethyl)imino]phenyl]disulfide]nickel(II) perchloroate

“…The N(12)-C(27) bond is 1.487 (23) A in length (Table IV) and is nearly a pure N(sp2)-C(sp2) a bond. In contrast, the N(10)-C(15) bond length, which would be equivalent in the uncoordinated ligand, is 1.430 (14) A and has appreciable character. The adjacent bonds at the imine nitrogen atoms are also not equivalent and are altered in the opposite sense: N(10)-C(20) is longer (1.27 (2) A) than N(12)-C (32) (1.23 (2) A).…”