An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

The title compound, C11H26P2S2, displays crystallographic mirror symmetry. Key bond lengths (Angstrom) are P1-C(methylene) 1.8464 (18), P1-C(butyl) 1.8711 (13), P2-C(methylene) 1.8266 (18), P2-C(methyl) 1.7948 (15), P1=S 1.9631 (8) and P2=S 1.9552 (8), where P1 is the di-tert-butylphosphino P atom and P2 is the dimethylphosphino P atom. The angle P-C-P [124.31 (10)degrees] is wide and S=P-C(methylene) [108.91 (6)degrees] narrow. Steric pressure from the tert-butyl groups may cause some of the molecular dimensions to depart from normal values.

The title compound 3 was formed in the reaction of Cl2PCCl2PCl2 (2) with catechol in the presence of triethylamine. The reaction of 3 with tetrachloro-o-benzoquinone (TOB), 4, led to the sigma(3)P/sigma(5)P-species 5, and the sigma(5)P/sigma(5)P-species 6a/6b. 5 was stable only in solution, and its existence and identity are postulated on the basis of its P-31-NMR spectrum. The structure of 6a/6b could not be assigned unambiguously to one isomer. The reaction of 6a/6b with water yielded the phosphorate 10. The structures of 3 and 10 were determined by single crystal X-ray methods. A wide P-C-P angle (123.2 degrees) was observed in 3. The cation of 10 is a centrosymmetric, protonated DMF dimer with O ... O 241.3 pm.

The title compound 1 was allowed to react with catechol, 2,3-dihydroxynaphthalene, tetrabromocatechol, resorcinol, saligenin, and 3,5-di-tert-butylcatechol in the presence of triethylamine to form compounds 4a–4d and 4f. Whereas the catechol derivative 4a, the naphthol derivative 4b, and the tetrabromocatechol derivative 4c could be readily obtained, the saligenin derivative 4d and the 3,5-di-tert-butylcatechol derivative 4f were found to be stable only in solution. Contrary to expectation, compound 4e was not formed in the reaction of 1 with resorcinol. The reaction of 1 with 1,2,4,5-tetrahydroxybenzene led to the pentacyclic derivative 4g. Reaction of hydroquinone with 1 led to the formation of the dimeric structure 4h. Crystal structure analyses of 4a and 4b show that the nine-membered rings adopt essentially identical “tub” conformations in which the P and O atoms are coplanar. The P-C-P angles (across the CCl2 bridge) are wide (ca. 119°). © 1997 John Wiley & Sons, Inc.

Bis[(di‐tert‐butylphosphanyl)methyl]methylphosphane[1]The synthesis of [(di‐tert‐butylphosphanyl)methyl]dimethyl‐phosphane (3) and of the title compound 5 is described. 5 reacts with sulfur to form the trisulfide 6. Both 3 and 5 behave as bidentate ligands in forming the molybdenum complexes 8 and 10, which are characterized by single crystal X‐ray structure determinations. 10 reacts with sulfur to yield the sulfide 11, which decomposes in solution within 6 h.