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Synthesis and spectroscopic characterization of tris(O,O '-ditolyl dithiophosphato) arsenic/antimony/bismuth(III) compounds: Crystal structures of [As{S2P(OC6H4Me-m)(2)}(3)]center dot 0.5C(6)H(14), [Sb{S2P(OC6H4Me-m)(2)}(3)] and [Bi{S2P(OC6H4Me-m)(2)}(3)]

Synthesis and spectroscopic characterization of tris(O,O '-ditolyl dithiophosphato) arsenic/antimony/bismuth(III) compounds: Crystal structures of [As{S2P(OC6H4Me-m)(2)}(3)]center dot 0.5C(6)H(14), [Sb{S2P(OC6H4Me-m)(2)}(3)] and [Bi{S2P(OC6H4Me-m)(2)}(3)]
Synthesis and spectroscopic characterization of tris(O,O '-ditolyl dithiophosphato) arsenic/antimony/bismuth(III) compounds: Crystal structures of [As{S2P(OC6H4Me-m)(2)}(3)]center dot 0.5C(6)H(14), [Sb{S2P(OC6H4Me-m)(2)}(3)] and [Bi{S2P(OC6H4Me-m)(2)}(3)]
Arsenic(III), antimony(III) and bismuth(III) compounds of the type, [M{S2P(OR)(2)}(3)] (where M = As, Sb and Bi; R = o-, m-, p-C6H4Me) were obtained by reactions of MCl3 with ammonium salts of the corresponding O,O'-ditolyl dithiophosphate on refluxing in benzene. These compounds were characterized by elemental analysis, IR, H-1 NMR and P-31 NMR spectroscopy. The single crystal X-ray structures of three representative compounds were determined. [As{S2P(OC6H4Me-m)(2)}(3)]center dot 0.5C(6)H(14) crystallizes as triclinic in the space group P (1) over bar with a = 10.9396(1), b = 14.1891(2), c = 17.5359(2) angstrom, alpha = 70.731(1), beta = 84.734(1), gamma = 74.205(1)degrees, Z = 4,V = 2472.37(5) angstrom(3). [Sb{S2P(OC6H4Me-m)(2)}(3)] and [Bi{S2P(OC6H4Me-m)(2)}(3)] both crystallize as monoclinic in the space group P2(1) with a = 12.4520(3), b = 22.8760(5), c = 16.2165(4) angstrom, beta = 93.022(1)degrees, Z = 4, V = 4612.9(2) angstrom(3) and with a = 12.4903(2), b = 22.9554(4), c = 16.1032(3)angstrom, beta = 92.4300(10)degrees, Z = 4, V = 4612.96(14) angstrom(3), respectively. In all three molecules, the central metal atom is surrounded by all six sulfur atoms of the three chelating anisobidentate O,O'-ditolyl dithiophosphate groups in a pseudo trigonally distorted octahedron with a lone pair positioned on one of the triangular octahedral faces. The three metal sulfur bonds adjacent to the lone pair (capped face) are longer than the three furthest from the lone pair (uncapped face). Inter-ligand angles between the longer bonds are greater than those between the shorter bonds. (C) 2008 Elsevier Ltd. All rights reserved.
0277-5387
689-694
Maheshwari, Seema
276fab22-7ef8-421c-9501-ca095456ea7a
Drake, John E.
6de1350f-4eb6-4ca7-b796-947f4fec467d
Kori, Kavita
cc97c9f4-3632-431e-a5c1-7255aa6394d8
Light, Mark Edward
cf57314e-6856-491b-a8d2-2dffc452e161
Ratnani, Raju
0a86c56f-00c6-4c9f-8aa0-52667938ba70
Maheshwari, Seema
276fab22-7ef8-421c-9501-ca095456ea7a
Drake, John E.
6de1350f-4eb6-4ca7-b796-947f4fec467d
Kori, Kavita
cc97c9f4-3632-431e-a5c1-7255aa6394d8
Light, Mark Edward
cf57314e-6856-491b-a8d2-2dffc452e161
Ratnani, Raju
0a86c56f-00c6-4c9f-8aa0-52667938ba70

Maheshwari, Seema, Drake, John E., Kori, Kavita, Light, Mark Edward and Ratnani, Raju (2009) Synthesis and spectroscopic characterization of tris(O,O '-ditolyl dithiophosphato) arsenic/antimony/bismuth(III) compounds: Crystal structures of [As{S2P(OC6H4Me-m)(2)}(3)]center dot 0.5C(6)H(14), [Sb{S2P(OC6H4Me-m)(2)}(3)] and [Bi{S2P(OC6H4Me-m)(2)}(3)]. Polyhedron, 28 (4), 689-694. (doi:10.1016/j.poly.2008.12.017).

Record type: Article

Abstract

Arsenic(III), antimony(III) and bismuth(III) compounds of the type, [M{S2P(OR)(2)}(3)] (where M = As, Sb and Bi; R = o-, m-, p-C6H4Me) were obtained by reactions of MCl3 with ammonium salts of the corresponding O,O'-ditolyl dithiophosphate on refluxing in benzene. These compounds were characterized by elemental analysis, IR, H-1 NMR and P-31 NMR spectroscopy. The single crystal X-ray structures of three representative compounds were determined. [As{S2P(OC6H4Me-m)(2)}(3)]center dot 0.5C(6)H(14) crystallizes as triclinic in the space group P (1) over bar with a = 10.9396(1), b = 14.1891(2), c = 17.5359(2) angstrom, alpha = 70.731(1), beta = 84.734(1), gamma = 74.205(1)degrees, Z = 4,V = 2472.37(5) angstrom(3). [Sb{S2P(OC6H4Me-m)(2)}(3)] and [Bi{S2P(OC6H4Me-m)(2)}(3)] both crystallize as monoclinic in the space group P2(1) with a = 12.4520(3), b = 22.8760(5), c = 16.2165(4) angstrom, beta = 93.022(1)degrees, Z = 4, V = 4612.9(2) angstrom(3) and with a = 12.4903(2), b = 22.9554(4), c = 16.1032(3)angstrom, beta = 92.4300(10)degrees, Z = 4, V = 4612.96(14) angstrom(3), respectively. In all three molecules, the central metal atom is surrounded by all six sulfur atoms of the three chelating anisobidentate O,O'-ditolyl dithiophosphate groups in a pseudo trigonally distorted octahedron with a lone pair positioned on one of the triangular octahedral faces. The three metal sulfur bonds adjacent to the lone pair (capped face) are longer than the three furthest from the lone pair (uncapped face). Inter-ligand angles between the longer bonds are greater than those between the shorter bonds. (C) 2008 Elsevier Ltd. All rights reserved.

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Published date: 12 March 2009

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Local EPrints ID: 67647
URI: http://eprints.soton.ac.uk/id/eprint/67647
ISSN: 0277-5387
PURE UUID: 71676623-ff8e-4d16-bee8-4f16d728e549
ORCID for Mark Edward Light: ORCID iD orcid.org/0000-0002-0585-0843

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Date deposited: 02 Sep 2009
Last modified: 22 Oct 2019 00:49

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Author: Seema Maheshwari
Author: John E. Drake
Author: Kavita Kori
Author: Raju Ratnani

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