Advanced

Dppm-substituted ruthenium clusters with capping sulfido and selenido ligands derived from thiourea, tetramethylthiourea and elemental selenium

Ahmed, SJ ; Hyder, MI ; Kabir, SE ; Miah, MA ; Deeming, AJ and Nordlander, Ebbe LU (2006) In Journal of Organometallic Chemistry 691(3). p.309-322
Abstract
Treatment of [Ru-3(CO)(10)(mu-dppm)] (4) [dppm = bis(diphenylphosphido)methane] with tetramethylthiourea at 66 degrees C gave the previously reported dihydrido triruthenium cluster [Ru-3(mu-H)(2)(mu(3)-S)(CO)(7)(mu-dppm)] (5) and the new compounds [Ru-3(mu(3)-S)(2)(CO)(7)(mu-dppm)] (6), [Ru-3(mu(3)-S)(CO)(7)(mu(3)-CO)(mu-dppm)] (7) and [Ru-3(mu 3-S)eta(I)-C(NMe2)(2)}(CO)(6)(mu(3)-CO)(mu-dppm)] (8) in 6%, 10%, 32% and 9% yields, respectively. Treatment of 4 with thiourea at the same temperature gave 5 and 7 in 30% and 10% yields, respectively. Compound 7 reacts further with tetramethylthiourea at 66 degrees C to yield 6 (30%) and a new compound [Ru-3(mu(3)-S)(2){mu(3)-C(NMe2)(2)}(CO)(6)(mu-dppm)] (9) (8%). Thermolysis of 8 in refluxing THF... (More)
Treatment of [Ru-3(CO)(10)(mu-dppm)] (4) [dppm = bis(diphenylphosphido)methane] with tetramethylthiourea at 66 degrees C gave the previously reported dihydrido triruthenium cluster [Ru-3(mu-H)(2)(mu(3)-S)(CO)(7)(mu-dppm)] (5) and the new compounds [Ru-3(mu(3)-S)(2)(CO)(7)(mu-dppm)] (6), [Ru-3(mu(3)-S)(CO)(7)(mu(3)-CO)(mu-dppm)] (7) and [Ru-3(mu 3-S)eta(I)-C(NMe2)(2)}(CO)(6)(mu(3)-CO)(mu-dppm)] (8) in 6%, 10%, 32% and 9% yields, respectively. Treatment of 4 with thiourea at the same temperature gave 5 and 7 in 30% and 10% yields, respectively. Compound 7 reacts further with tetramethylthiourea at 66 degrees C to yield 6 (30%) and a new compound [Ru-3(mu(3)-S)(2){mu(3)-C(NMe2)(2)}(CO)(6)(mu-dppm)] (9) (8%). Thermolysis of 8 in refluxing THF yields 7 in 55% yield. The reaction of 4 with selenium at 66 degrees C yields the new compounds [Ru-3(mu(3)-Se)(CO)(7)(mu(3)-CO)(mu-dppm)] (12) and [Ru-4(mu(3)-Se)(mu(3)-eta(3)-PhPCH2PPh(C6H4)(CO)(6)(mu-CO)] (11) and the known compounds [Ru-3(mu-H)(2)(mu(3)-Se)(CO)(7)(mu-dppm)] (12) and [Ru-4(mu(3)-Se)(4)(CO)(6)(mu-dppm)] (13) in 29%, 5%, 2% and 5% yields, respectively. Treatment of 10 with tetramethylthiourea at 66 degrees C gives the mixed sulfur-selenium compounds [Ru-3(mu(3)-S)([mu(3)-Se)(CO)(7)(mu-dppm)] (14) and [Ru-3(mu(3)-S)(mu(3)-Se){eta(1)-C(NMe2)(2)}(CO)(6)(mu-dppm)] (15) in 38% and 10% yields, respectively. The single-crystal XRD structures of 6, 7, 8, 10, 14 and 15 are reported. (Less)
Please use this url to cite or link to this publication:
author
; ; ; ; and
organization
publishing date
type
Contribution to journal
publication status
published
subject
keywords
carbene, selenium, sulfur, triruthenium clusters, tetramethylthiourea, alkylidene, x-ray structures
in
Journal of Organometallic Chemistry
volume
691
issue
3
pages
309 - 322
publisher
Elsevier
external identifiers
  • wos:000234614500006
  • scopus:29344473517
ISSN
0022-328X
DOI
10.1016/j.jorganchem.2005.08.017
language
English
LU publication?
yes
additional info
The information about affiliations in this record was updated in December 2015. The record was previously connected to the following departments: Chemical Physics (S) (011001060)
id
773b9f3a-0302-4ff4-a261-b00913846f35 (old id 421282)
date added to LUP
2016-04-01 16:53:15
date last changed
2020-05-06 04:04:19
@article{773b9f3a-0302-4ff4-a261-b00913846f35,
  abstract     = {Treatment of [Ru-3(CO)(10)(mu-dppm)] (4) [dppm = bis(diphenylphosphido)methane] with tetramethylthiourea at 66 degrees C gave the previously reported dihydrido triruthenium cluster [Ru-3(mu-H)(2)(mu(3)-S)(CO)(7)(mu-dppm)] (5) and the new compounds [Ru-3(mu(3)-S)(2)(CO)(7)(mu-dppm)] (6), [Ru-3(mu(3)-S)(CO)(7)(mu(3)-CO)(mu-dppm)] (7) and [Ru-3(mu 3-S)eta(I)-C(NMe2)(2)}(CO)(6)(mu(3)-CO)(mu-dppm)] (8) in 6%, 10%, 32% and 9% yields, respectively. Treatment of 4 with thiourea at the same temperature gave 5 and 7 in 30% and 10% yields, respectively. Compound 7 reacts further with tetramethylthiourea at 66 degrees C to yield 6 (30%) and a new compound [Ru-3(mu(3)-S)(2){mu(3)-C(NMe2)(2)}(CO)(6)(mu-dppm)] (9) (8%). Thermolysis of 8 in refluxing THF yields 7 in 55% yield. The reaction of 4 with selenium at 66 degrees C yields the new compounds [Ru-3(mu(3)-Se)(CO)(7)(mu(3)-CO)(mu-dppm)] (12) and [Ru-4(mu(3)-Se)(mu(3)-eta(3)-PhPCH2PPh(C6H4)(CO)(6)(mu-CO)] (11) and the known compounds [Ru-3(mu-H)(2)(mu(3)-Se)(CO)(7)(mu-dppm)] (12) and [Ru-4(mu(3)-Se)(4)(CO)(6)(mu-dppm)] (13) in 29%, 5%, 2% and 5% yields, respectively. Treatment of 10 with tetramethylthiourea at 66 degrees C gives the mixed sulfur-selenium compounds [Ru-3(mu(3)-S)([mu(3)-Se)(CO)(7)(mu-dppm)] (14) and [Ru-3(mu(3)-S)(mu(3)-Se){eta(1)-C(NMe2)(2)}(CO)(6)(mu-dppm)] (15) in 38% and 10% yields, respectively. The single-crystal XRD structures of 6, 7, 8, 10, 14 and 15 are reported.},
  author       = {Ahmed, SJ and Hyder, MI and Kabir, SE and Miah, MA and Deeming, AJ and Nordlander, Ebbe},
  issn         = {0022-328X},
  language     = {eng},
  number       = {3},
  pages        = {309--322},
  publisher    = {Elsevier},
  series       = {Journal of Organometallic Chemistry},
  title        = {Dppm-substituted ruthenium clusters with capping sulfido and selenido ligands derived from thiourea, tetramethylthiourea and elemental selenium},
  url          = {http://dx.doi.org/10.1016/j.jorganchem.2005.08.017},
  doi          = {10.1016/j.jorganchem.2005.08.017},
  volume       = {691},
  year         = {2006},
}