Crystal and Molecular Structures of the Sulfur-Rich Organic Polysulfanes Heptathiacyclononane (C₂H₄S₇) and Bis(triphenylmethyl)pentaand hexasulfane

Abstract

C 12 H 22 CdN4O14, triclinic, P¯ (no. 2), a = 7.188(2) Å, b = 8.895(3) Å, c = 9.771(3) Å, α = 63.148(3)°, β = 76.750(3)°, γ = 66.225(3)°, V = 509.2(3) Å 3 , Z = 1, Rgt(F) = 0.0253, wR ref (F 2 ) = 0.0676, T = 296(2) K. CCDC no.: 1484775The crystal structure is shown in the gure. Tables 1 and 2 contain details of the measurement method and a list of the atoms including atomic coordinates and displacement parameters. Source of materialThe title compound was synthesized by a hydrothermal method under autogenous pressure. A mixture of CdCl 2 ·H 2 O

Preparation of Organic Polysulfanes R2Sn (n = 5, 7, 8, 9) from Sulfenyl Chlorides, RSCl, and Transition Metal Polysulfido Complexes

“…In a similar fashion, bifunctional organic sulfenyl chlorides and chlorodisulfanes have been treated with titanocene pentasulfide or similar complexes, thereby generating cyclic sulfur-rich polysulfanes with up to 11 sulfur atoms (Equation 5 and 6): [9,10,11] 1,2-C 2 H 4 (SCl) 2 [12] which reacts with sulfenyl chlorides as an S 3 group transfer reagent (Equation 7 and 8; CpЈ ϭ CH 3 C 5 H 4 ): [13] C 10 In this work, we report the synthesis of five chain-like and three cyclic organic polysulfanes with between 5 and 9 sulfur atoms. In the case of the chain-like species, we used alkyl as well as aryl substituents.…”

Synthesis and Structure of the Sulfur-Rich Macrocycle (1,2-C6H4S8)2

“…This sulfane was isolated in 6% yield and characterized by single crystal X-ray crystallography as 5,6,7,8,9,10,11,12,17,18,19,20,21,22,23,24-hexadecathiadibenzo[a,k]cycloeicosene (C 6 H 4 S 8 ) 2 3. This macrocyclic product is obtained from carbon disulfide solutions as yellow crystals that contain one mol of CS 2 per mol of 3.…”

“…[1] Such compounds are often thermally unstable and subject to decomposition by nucleophilic attack, and therefore not easy to prepare by conventional synthetic methods such as those described in Methodicum Chimicum [2] and HoubenWeyl. [3] The most important metal polysulfido complexes used in this context are the titanocene derivatives [(C 5 H 5 ) 2 TiS 5 ], [4Ϫ7] [(C 5 H 5 ) 2 ClTi] 2 S 3 [8] and [(C 5 H 5 ) 2 TiS 2 ] 2 [6] as well as the zinc complex [(TMEDA)ZnS 6 ] 1 (TMEDA: tetramethylethylenediamine). [9] These neutral complexes are soluble in organic solvents and react with organic sulfenyl chlorides almost quantitatively to give the corresponding polysulfanes containing between 5 and 11 cumulated sulfur atoms.…”

“…The centrosymmetric unit cell of (C6 H 4 S 8 ) 2 ·CS 2 and numbering of atoms; selected internuclear distances [pm] and bond angles [°] as well as torsions angles [°]: C(1Ј)Ϫ(C(2Ј) 139.7)ϪS(9) 153.7(2); C(2Ј)ϪC(1Ј)ϪS(1) 117.2(2), C(1Ј)ϪS(1)ϪS(2) 104.97(10), S(1)ϪS(2)ϪS(3) 108.35(5), S(2)ϪS(3)ϪS(4) 106.09(6), S(3)ϪS(4)ϪS(5) 108.22(5), S(4)ϪS(5)ϪS(6) 106.56(5), S(5)ϪS(6)Ϫ S(7) 106.40(4), S(6)ϪS(7)ϪS(8) 105.66(5), S(7)ϪS(8)ϪC(2) 102.09; C(2Ј)ϪC(1Ј)ϪS(1)ϪS(2) Ϫ165.1(2), C(1Ј)ϪS(1)ϪS(2)ϪS(3) Ϫ80.15(10), S(1)ϪS(2)ϪS(3)ϪS(4) Ϫ88.70(6), S(2)ϪS(3)ϪS(4)Ϫ S(5) 105.91(6), S(3)ϪS(4)ϪS(5)ϪS(6) Ϫ90.65(6), S(4)ϪS(5)Ϫ S(6)ϪS(7) 108.95(5), S(5)ϪS(6)ϪS(7)ϪS(8) 88.70(5), S(6)ϪS(7)ϪS(8)ϪC(2) 82.50(10), S(7)ϪS(8)ϪC(2)ϪC(1) Ϫ108.1(1)…”

Principles of crystal packing and intermolecular motifs for Ph3XSnXPh3, X⊕=⊕C, Si, Ge, Sn

“…These, together with the new crystal structure for Ph 3 CS 3 CPh 3 reported here, are listed with cell dimensions and space groups in Table 1. Only one crystal (refcode YAVDAA, Ph 3 CS 5 CPh 3 ?CHCl 3 16 ) includes solvent, and the general nonoccurrence of solvent in this set of 12 crystals is an indication of efficient crystal packing.…”