Синтез и строение комплексов палладия [Ph3PMe]+[PdBr3(DMSO)]– и [Ph3P(CH2)6PPh3]2+[PdBr3(Et2SO)]–2

Abstract

[Ph 3 PMe] + [PdBr 3 (dmso- S )] – ( 1 ) and [Ph 3 P(CH 2 ) 6 PPh 3 ] 2+ [PdBr 3 (Et 2 SO- S )] – 2 ( 2 ) was obtained by the reaction of palladium dibromide with methyltriphenylphosphonium bromide (1:1 mol.) in the dimethylsulfoxide and hexamethylene- bis -triphenylphosphonium dibromidein the diethylsulfoxide. According to X-ray analysis was performed on a Bruker D8 QUEST automatic four-circle diffractometer (Mo К α -emission, λ = 0.71073 Å, graphite monochromator) red-brown crystals 1 [C 42 H 48 O 2 P 2 S 2 Br 6 Pd 2 , M 1403.12, crystal system moclinic, space group P2 1 , a 8.91(2), b 24.88(4), c 22.34(5) Å, V 4954(18) Å 3 , Z 4, µ 5.747 mm -1 , independent reflections 6306, R int 0,0525, refinement variables 1022, GOOF 1,069, R 1 = 0,0580, wR 2 = 0.1429] and preliminary data X-rayred-brown crystals 2 [C 50 H 62 P 2 S 2 Br 6 Pd 2 O 2 , M 1513.32, crystal system triclinic, space group P2 1 , a 13.046(13), b 13.065(14), c 17.784(18) Å, V 2885(5) Å 3 , Z 2, independent reflections 6831, R int 0.0647, refinement variables 582, GOOF 1.086, R 1 = 0.1422, wR 2 = 0.3876] atoms P in 1 and 2 have distorted tetrahedral coordination (CPC angles 107.3(14)–111.1(14)°, 107.2(18)–110.9(16)°), bond lengths P–С 1.78(2)–1.84(3) Å and 1,77(4)–1,82(3) Å. In mononuclear planar square anions (angles SPdBr- cis 87,1(3)°, 92.8(3)° ( 1 ), 90.3(3)°, 91.0(3)° ( 2 ), BrPdBr- trance and SPdBr- trance 174.37(14)°, 177.4(2)° ( 1 ), 173.4(2)°, 178.5(3)° ( 2 ), BrPdBr- cis 89.72(19)°–90.43(19)° ( 1 ), 89.2(2)°–89.6(2)° ( 2 )), dimethyl- and diethylsulfoxide ligands coordinated to the Pd by sulfur atoms (Pd–S 2.275(8) and 2.266(13) Å), distances Pd-Br for 1 and 2 vary in the range 2.426(5)–2.450(5) Å and 2.426(5)– 2.451(6) Å. The full tables of atomic coordinates, bond lengths, and bond angles were deposited with the Cambridge Crystallographic Data Centre (CCDC 1833574 for compound 1 deposit@ccdc.cam.ac.uk; http://www.ccdc.cam.ac.uk).