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The reaction of TiCl 4  with (Me 3 Si) 2 S in dichloromethane yields black, insoluble, impure TiSCl 2 . In the presence of oxygen, additionally Ti 3 O(S 2 )3Cl 4  and Ti 4 O(S 2 ) 4 Cl 6  are formed. By reactions of TiSCl 2  with NEt 4 Cl and PPh 4 Cl in dichloromethane (NEt 4 ) 2 [TiSCl 2 ] and (PPh 4 ) 2 [TiSCl 4 ] · 2 CH 2 Cl 2  are formed, respectively. They were characterized by their IR spectra and by X-ray crystal structure determinations. They contain the square-pyramidal [TiSCl 4 ] 2-  ion. which has a rather short Ti = S bond of 211.1(2) pm. Crystal data: (NEt 4 ) 2 [TiSCl 4 ]: tetragonal. P4/n, a = 923.9(3). c = 1406.7(2) pm. Z = 2. 966 unique observed reflexions. R = 0.053; positionally disordered ethyl groups. (PPh 4 )2[TiSCl 4 ] · 2CH 2 Cl 2 : triclinic, P1, a = 1009.7(4), b = 1115.1(3). c = 1242.1(5) pm, α = 70.27(3), β = 79.06(3), γ = 81.37(3)°, Z = 1, 1504 reflexions, β-(AsPh 4 ) 2 UCl 6 ·2CH 2 Cl 2  structure type, high R = 0.107 due to positional disorder of the anion. Addition of NEt 4 Cl or PPh 4 Cl in CH 2 Cl 2  to the primary reaction product in presence of O 2  yields (NEt 4 ) 2 [Ti 3 O(S 2 ) 3 Cl 6 ] and (PPh 4 ) 2 [Ti,O(S 2 ) 3 Cl 6 ] · CH 2 Cl 2 , respectively. Upon recrystallization of the latter from acetonitrile, (PPh 4 ) 2 [Ti 3 O(S 2 ) 3 Cl 6 ] · CH 3 CN is obtained which forms triclinic crystals with a = 1138.8(3). b = 1268.8(4), c = 2166.4(6) pm, α = 101.26(3). β = 97.21(2). γ = 109.24(2)°, Z = 2, P1 (3053 reflexions, R = 0.070). The [Ti 3 O(S 2 ) 3 Cl 6 ] 2-  ion has a cluster-like structure with Ti atoms at the vertices of a triangle, with a μ 3 -O bridging atom and with tree bridging disulfide groups. Crystal data for Ti 4 O(S 2 ) 4 Cl 6 : monoclinic, C2/c, a - 917.3(2), b - 1632.5(2), c = 1268.5(2) pm, β - 108.35(2)°, Z = 4. 1009 reflexions. R = 0.027. In the Ti 4 O(S 2 ) 4 Cl 6  molecule, four Ti atoms form a distorted tetrahedron around an μ 4 -O atom; two edges of the tetrahedron are spanned by chloro bridges, four edges by disulfide bridges.

zeitschrift für naturforschung b

Reaktionen von Titantetrachlorid mit Bistrimethylsilylsulfid. Die Kristallstrukturen von (NEt 4 ) 2 [TiSCl 4 ], (PPh 4 ) 2 [TiSCl 4 ]·2CH 2 Cl 2 , (PPh 4 ) 2 [Ti 3 O(S 2 ) 3 Cl 6 ]CH 3 CN und Ti 4 O(S 2 ) 4 Cl 6  / Reactions of Titanium Tetrachloride with Bistrimethylsilyl Sulfide. Crystal Structures of (NEt 4 ) 2 [TiSCl 4 ], (PPh 4 ) 2 [TiSCl 4 ]·2CH 2 Cl 2 , (PPh 4 ) 2 [Ti 3 O(S 2 ) 3 Cl 6 ]CH 3 CN and Ti 4 O(S 2 ) 4 Cl 6