Synthesis and structure of palladium complexes [Ph3PMe]+[PdBr3(DMSO)]- and [Ph3P(CH2)6PPh3]2+[PdBr3(Et2SO)]-2
Автор: Jarygina D.M., Batalov A.Е., Senchurin V.S.
Журнал: Вестник Южно-Уральского государственного университета. Серия: Химия @vestnik-susu-chemistry
Рубрика: Химия элементоорганических соединений
Статья в выпуске: 3 т.10, 2018 года.
Бесплатный доступ
[Ph3PMe]+[PdBr3(dmso- S )]- (1) and [Ph3P(CH2)6PPh3]2+[PdBr3(Et2SO- 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 Кα-emission, λ = 0.71073 Å, graphite monochromator) red-brown crystals 1 [C42H48O2P2S2Br6Pd2, M 1403.12, crystal system moclinic, space group P21, a 8.91(2), b 24.88(4), c 22.34(5) Å, V 4954(18) Å3, Z 4, µ 5.747 mm-1, independent reflections 6306, Rint 0,0525, refinement variables 1022, GOOF 1,069, R 1 = 0,0580, wR 2 = 0.1429] and preliminary data X-rayred-brown crystals 2 [C50H62P2S2Br6Pd2O2, M 1513.32, crystal system triclinic, space group P21, a 13.046(13), b 13.065(14), c 17.784(18) Å, V 2885(5) Å3, Z 2, independent reflections 6831, Rint 0.0647, refinement variables 582, GOOF 1.086, R1 = 0.1422, wR2 = 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).
Palladium dibromide, phosphonium bromide, dimethylsulfoxide, diethylsulfoxide, synthesis, structure, x-ray analysis
Короткий адрес: https://sciup.org/147233103
IDR: 147233103 | DOI: 10.14529/chem180306