palladium dibromide; phosphonium bromide; dimethylsulfoxide; diethylsulfoxide; synthesis; structure; X-ray analysis

Authors

  • D. M. Jarygina South Ural State University, Chelyabinsk, Russian Federation
  • A. Е. Batalov South Ural State University, Chelyabinsk, Russian Federation
  • V. S. Senchurin South Ural State University, Chelyabinsk, Russian Federation

DOI:

https://doi.org/10.14529/chem180306

Keywords:

дибромид палладия, бромид фосфония, диметилсульфоксид, диэтилсульфоксид, синтез, строение, рентгеноструктурный анализ

Abstract

[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, R1 = 0,0580,
wR2 = 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).

Author Biographies

D. M. Jarygina, South Ural State University, Chelyabinsk, Russian Federation

студент химического факультета

A. Е. Batalov, South Ural State University, Chelyabinsk, Russian Federation

студент химического факультета

V. S. Senchurin, South Ural State University, Chelyabinsk, Russian Federation

кандидат химических наук, доцент, кафедра теоретической и прикладной химии

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Published

2018-10-19

Issue

Vol. 10 No. 3 (2018): Вестник Южно-Уральского государственного университета. Серия "Химия"

Section

Химия элементоорганических соединений