Reactions of phenylimidotrichlorobis(triphenyl-phosphine)rhenium(V). Reaction with trimethyl-phosphine and reduction of trimethylphosphine complex to phenylamido complexes of rhenium(I, III). The X-ray crystal structures of phenylamido-(dinitrogen)tetrakis(trimethylphosphine)-rhenium(I) and phenylamido(buta-1,3-diene)-tetrakis-(trimethylphosphine)rhenium(I)

Kwok W. Chiu; Wai Kwok Wong; Geoffrey Wilkinson; Anita M.R. Galas; Michael B. Hursthouse

doi:10.1016/S0277-5387(00)81065-7

Reactions of phenylimidotrichlorobis(triphenyl-phosphine)rhenium(V). Reaction with trimethyl-phosphine and reduction of trimethylphosphine complex to phenylamido complexes of rhenium(I, III). The X-ray crystal structures of phenylamido-(dinitrogen)tetrakis(trimethylphosphine)-rhenium(I) and phenylamido(buta-1,3-diene)-tetrakis-(trimethylphosphine)rhenium(I)

Kwok W. Chiu
, Wai Kwok Wong
, Geoffrey Wilkinson^*
, Anita M.R. Galas
, Michael B. Hursthouse^*

^*Corresponding author for this work

Department of Chemistry

Research output: Contribution to journal › Journal article › peer-review

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Abstract

The interaction of Re(NPh)Cl₃(PPh₃)₂ with PMe₃ gives Re(NPh)Cl₃(PMe₃)(PPh₃) or Re(NPh)Cl₃(PMe₃)₂ depending on conditions. In the presence of excess PMe₃ the phenylimido compounds in tetrahydrofuran are reduced by sodium amalgam giving products whose nature depends on the atmosphere (Ar, N₂, H₂ CO, butadiene) used. The following compounds have been characterised: Re(NHPh)(N₂)(PMe₃)₄, ReH(NHPh)(η′-CH₂PMe₂)(PMe₃)₄, Re(H)₂(NHPh)(PMe₃)₄, Re(NHPh)(CO)₂(PMe₃)₃, Re(NHPh)(CO)₃(PMe₃)₂, Re(NHPh)(η⁴-C₄H₆)(PMe₃)₃ and Re(NPh)Cl₂(PMe₃)₃. The structures of Re(NHPh)(N₂)(PMe₃)₄ (3) and Re(NHPh)(C₄H₆)(PMe₃)₃, (8) have been confirmed by single-crystal X-ray diffraction studies. (3) is monoclinic, space group P2₁/n with a = 9.574(2), b = 19.528(3), c = 14.385(3)Å and β = 99.06(2)°; (8) is orthorhombic, space group Pbc2₁, with a = 12.207(2), b = 13.884(2), c = 14.242(2)Å. The structures were solved via the heavy atom method and refined by least squares to R values of 0.065 and 0.062 for 3249 and 2009 observed diffractometer data, respectively. In the dinitrogen complex the N₂ and NHPh ligands adopt a cis configuration with Re–N bond lengths of 1.955(13) and 2.200(14)Å, respectively. In the butadiene complex, whose structure is not well defined due to disorder and/or pseudo symmetry correlation effects, the Re–N (amido) distance is 2.13(3)Å.

Original language	English
Pages (from-to)	37-44
Number of pages	8
Journal	Polyhedron
Volume	1
Issue number	1
DOIs	https://doi.org/10.1016/S0277-5387(00)81065-7
Publication status	Published - Jan 1982

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Chiu, K. W., Wong, W. K., Wilkinson, G., Galas, A. M. R., & Hursthouse, M. B. (1982). Reactions of phenylimidotrichlorobis(triphenyl-phosphine)rhenium(V). Reaction with trimethyl-phosphine and reduction of trimethylphosphine complex to phenylamido complexes of rhenium(I, III). The X-ray crystal structures of phenylamido-(dinitrogen)tetrakis(trimethylphosphine)-rhenium(I) and phenylamido(buta-1,3-diene)-tetrakis-(trimethylphosphine)rhenium(I). Polyhedron, 1(1), 37-44. https://doi.org/10.1016/S0277-5387(00)81065-7

Chiu, Kwok W. ; Wong, Wai Kwok ; Wilkinson, Geoffrey et al. / Reactions of phenylimidotrichlorobis(triphenyl-phosphine)rhenium(V). Reaction with trimethyl-phosphine and reduction of trimethylphosphine complex to phenylamido complexes of rhenium(I, III). The X-ray crystal structures of phenylamido-(dinitrogen)tetrakis(trimethylphosphine)-rhenium(I) and phenylamido(buta-1,3-diene)-tetrakis-(trimethylphosphine)rhenium(I). In: Polyhedron. 1982 ; Vol. 1, No. 1. pp. 37-44.

@article{0c4a19e1f4a7498dbe3b475dc4fc4f67,

title = "Reactions of phenylimidotrichlorobis(triphenyl-phosphine)rhenium(V). Reaction with trimethyl-phosphine and reduction of trimethylphosphine complex to phenylamido complexes of rhenium(I, III). The X-ray crystal structures of phenylamido-(dinitrogen)tetrakis(trimethylphosphine)-rhenium(I) and phenylamido(buta-1,3-diene)-tetrakis-(trimethylphosphine)rhenium(I)",

abstract = "The interaction of Re(NPh)Cl3(PPh3)2 with PMe3 gives Re(NPh)Cl3(PMe3)(PPh3) or Re(NPh)Cl3(PMe3)2 depending on conditions. In the presence of excess PMe3 the phenylimido compounds in tetrahydrofuran are reduced by sodium amalgam giving products whose nature depends on the atmosphere (Ar, N2, H2 CO, butadiene) used. The following compounds have been characterised: Re(NHPh)(N2)(PMe3)4, ReH(NHPh)(η′-CH2PMe2)(PMe3)4, Re(H)2(NHPh)(PMe3)4, Re(NHPh)(CO)2(PMe3)3, Re(NHPh)(CO)3(PMe3)2, Re(NHPh)(η4-C4H6)(PMe3)3 and Re(NPh)Cl2(PMe3)3. The structures of Re(NHPh)(N2)(PMe3)4 (3) and Re(NHPh)(C4H6)(PMe3)3, (8) have been confirmed by single-crystal X-ray diffraction studies. (3) is monoclinic, space group P21/n with a = 9.574(2), b = 19.528(3), c = 14.385(3){\AA} and β = 99.06(2)°; (8) is orthorhombic, space group Pbc21, with a = 12.207(2), b = 13.884(2), c = 14.242(2){\AA}. The structures were solved via the heavy atom method and refined by least squares to R values of 0.065 and 0.062 for 3249 and 2009 observed diffractometer data, respectively. In the dinitrogen complex the N2 and NHPh ligands adopt a cis configuration with Re–N bond lengths of 1.955(13) and 2.200(14){\AA}, respectively. In the butadiene complex, whose structure is not well defined due to disorder and/or pseudo symmetry correlation effects, the Re–N (amido) distance is 2.13(3){\AA}.",

author = "Chiu, \{Kwok W.\} and Wong, \{Wai Kwok\} and Geoffrey Wilkinson and Galas, \{Anita M.R.\} and Hursthouse, \{Michael B.\}",

note = "Publisher copyright: {\textcopyright} 1982 Published by Elsevier Ltd.",

year = "1982",

month = jan,

doi = "10.1016/S0277-5387(00)81065-7",

language = "English",

volume = "1",

pages = "37--44",

journal = "Polyhedron",

issn = "0277-5387",

publisher = "Elsevier Ltd.",

number = "1",

}

Chiu, KW, Wong, WK, Wilkinson, G, Galas, AMR & Hursthouse, MB 1982, 'Reactions of phenylimidotrichlorobis(triphenyl-phosphine)rhenium(V). Reaction with trimethyl-phosphine and reduction of trimethylphosphine complex to phenylamido complexes of rhenium(I, III). The X-ray crystal structures of phenylamido-(dinitrogen)tetrakis(trimethylphosphine)-rhenium(I) and phenylamido(buta-1,3-diene)-tetrakis-(trimethylphosphine)rhenium(I)', Polyhedron, vol. 1, no. 1, pp. 37-44. https://doi.org/10.1016/S0277-5387(00)81065-7

Reactions of phenylimidotrichlorobis(triphenyl-phosphine)rhenium(V). Reaction with trimethyl-phosphine and reduction of trimethylphosphine complex to phenylamido complexes of rhenium(I, III). The X-ray crystal structures of phenylamido-(dinitrogen)tetrakis(trimethylphosphine)-rhenium(I) and phenylamido(buta-1,3-diene)-tetrakis-(trimethylphosphine)rhenium(I). / Chiu, Kwok W.; Wong, Wai Kwok; Wilkinson, Geoffrey et al.
In: Polyhedron, Vol. 1, No. 1, 01.1982, p. 37-44.

Research output: Contribution to journal › Journal article › peer-review

TY - JOUR

T1 - Reactions of phenylimidotrichlorobis(triphenyl-phosphine)rhenium(V). Reaction with trimethyl-phosphine and reduction of trimethylphosphine complex to phenylamido complexes of rhenium(I, III). The X-ray crystal structures of phenylamido-(dinitrogen)tetrakis(trimethylphosphine)-rhenium(I) and phenylamido(buta-1,3-diene)-tetrakis-(trimethylphosphine)rhenium(I)

AU - Chiu, Kwok W.

AU - Wong, Wai Kwok

AU - Wilkinson, Geoffrey

AU - Galas, Anita M.R.

AU - Hursthouse, Michael B.

PY - 1982/1

Y1 - 1982/1

N2 - The interaction of Re(NPh)Cl3(PPh3)2 with PMe3 gives Re(NPh)Cl3(PMe3)(PPh3) or Re(NPh)Cl3(PMe3)2 depending on conditions. In the presence of excess PMe3 the phenylimido compounds in tetrahydrofuran are reduced by sodium amalgam giving products whose nature depends on the atmosphere (Ar, N2, H2 CO, butadiene) used. The following compounds have been characterised: Re(NHPh)(N2)(PMe3)4, ReH(NHPh)(η′-CH2PMe2)(PMe3)4, Re(H)2(NHPh)(PMe3)4, Re(NHPh)(CO)2(PMe3)3, Re(NHPh)(CO)3(PMe3)2, Re(NHPh)(η4-C4H6)(PMe3)3 and Re(NPh)Cl2(PMe3)3. The structures of Re(NHPh)(N2)(PMe3)4 (3) and Re(NHPh)(C4H6)(PMe3)3, (8) have been confirmed by single-crystal X-ray diffraction studies. (3) is monoclinic, space group P21/n with a = 9.574(2), b = 19.528(3), c = 14.385(3)Å and β = 99.06(2)°; (8) is orthorhombic, space group Pbc21, with a = 12.207(2), b = 13.884(2), c = 14.242(2)Å. The structures were solved via the heavy atom method and refined by least squares to R values of 0.065 and 0.062 for 3249 and 2009 observed diffractometer data, respectively. In the dinitrogen complex the N2 and NHPh ligands adopt a cis configuration with Re–N bond lengths of 1.955(13) and 2.200(14)Å, respectively. In the butadiene complex, whose structure is not well defined due to disorder and/or pseudo symmetry correlation effects, the Re–N (amido) distance is 2.13(3)Å.

AB - The interaction of Re(NPh)Cl3(PPh3)2 with PMe3 gives Re(NPh)Cl3(PMe3)(PPh3) or Re(NPh)Cl3(PMe3)2 depending on conditions. In the presence of excess PMe3 the phenylimido compounds in tetrahydrofuran are reduced by sodium amalgam giving products whose nature depends on the atmosphere (Ar, N2, H2 CO, butadiene) used. The following compounds have been characterised: Re(NHPh)(N2)(PMe3)4, ReH(NHPh)(η′-CH2PMe2)(PMe3)4, Re(H)2(NHPh)(PMe3)4, Re(NHPh)(CO)2(PMe3)3, Re(NHPh)(CO)3(PMe3)2, Re(NHPh)(η4-C4H6)(PMe3)3 and Re(NPh)Cl2(PMe3)3. The structures of Re(NHPh)(N2)(PMe3)4 (3) and Re(NHPh)(C4H6)(PMe3)3, (8) have been confirmed by single-crystal X-ray diffraction studies. (3) is monoclinic, space group P21/n with a = 9.574(2), b = 19.528(3), c = 14.385(3)Å and β = 99.06(2)°; (8) is orthorhombic, space group Pbc21, with a = 12.207(2), b = 13.884(2), c = 14.242(2)Å. The structures were solved via the heavy atom method and refined by least squares to R values of 0.065 and 0.062 for 3249 and 2009 observed diffractometer data, respectively. In the dinitrogen complex the N2 and NHPh ligands adopt a cis configuration with Re–N bond lengths of 1.955(13) and 2.200(14)Å, respectively. In the butadiene complex, whose structure is not well defined due to disorder and/or pseudo symmetry correlation effects, the Re–N (amido) distance is 2.13(3)Å.

UR - https://www.scopus.com/pages/publications/0006627570

U2 - 10.1016/S0277-5387(00)81065-7

DO - 10.1016/S0277-5387(00)81065-7

M3 - Journal article

AN - SCOPUS:0006627570

SN - 0277-5387

VL - 1

SP - 37

EP - 44

JO - Polyhedron

JF - Polyhedron

IS - 1

ER -

Chiu KW, Wong WK, Wilkinson G, Galas AMR, Hursthouse MB. Reactions of phenylimidotrichlorobis(triphenyl-phosphine)rhenium(V). Reaction with trimethyl-phosphine and reduction of trimethylphosphine complex to phenylamido complexes of rhenium(I, III). The X-ray crystal structures of phenylamido-(dinitrogen)tetrakis(trimethylphosphine)-rhenium(I) and phenylamido(buta-1,3-diene)-tetrakis-(trimethylphosphine)rhenium(I). Polyhedron. 1982 Jan;1(1):37-44. doi: 10.1016/S0277-5387(00)81065-7

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