| Abstract: | Acyl- and Alkylidenephosphines. XXIII. Synthesis and Structure of Bis(trimethylsilylsulfano)methylidene]phosphines Analogous to the phenyl derivative 1a 2] tert-butyl- 1b , mesityl- 1c and methylbis-(trimethylsilyl)phosphine 1 d react with carbon disulfide to give the corresponding bis(trimethylsilylsulfano)methylidene]phosphines 4 . Only in case of the mesitylphosphine 1 c the intermediate compounds 2 and 3 could be detected by n.m.r. spectroscopic methods; thermally unstable bis(trimethylsilylsulfano)methylidene]methylphosphine 4 d dimerizes rapidly 1]. Bis(trimethylsilylsulfano)methylidene]phenylphosphine 4 a crystallizes in the monoclinic centrosymmetric space group P21/c with following dimensions of the unit cell determined at ?95 ± 3°C: a = 1386.4(8); b = 1036.0(7); c = 1281.7(8) pm; ß = 101.23(4)°; Z = 4. An X-ray structure determination (R = 0.032) proves the constitution of this compound as already derived from its nmr spectra. Characteristic bond lengths and angles are: P?C 170; P? C(phenyl) 183; C? S 176; S? Si 219 pm; C? P?C 107; P?C? S 124 and 120; S? C? S 116 and C? S? Si 111°. |
