Synthesis, crystal structure and properties of [Fe(h5-C5H5)(CO)(μ-SC5H9NCH3)]2

Walter Gaete; Josep Ros; Ramon Yañez; Xavier Solans; Manuel Font-Altaba

doi:10.1016/0022-328X(86)82085-X

Synthesis, crystal structure and properties of [Fe(h⁵-C₅H₅)(CO)(μ-SC₅H₉NCH₃)]₂

Walter Gaete, Josep Ros, Ramon Yañez, Xavier Solans, Manuel Font-Altaba

Department of Chemistry

Research output: Contribution to journal › Article › Research › peer-review

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Abstract

The reaction of Fe2(CO)4(h5-C5H5)2 with 4-N-methylpiperidine-disulphide affords [Fe(h5-C5H5)(μ-SC5H9NCH3]2, the crystal structure of which has been determined. The crystals are monoclinic, space group C2/c with a 18.761(3), b 14.543(2), c 9.556(1) Å, β 103.67(2)°. With Z = 4 the calculated density is 1.46 g cm cm-3; the final weighted R factor was 0.047 for 1645 independent reflections. The two carbonyl groups and the two sulphur-attached piperidine groups in the dimeric structure are both cisoid. Reaction with CH3I leads to methylation that with aqueous HClO4 to protonation of the nitrogen atoms of the piperidine rings, giving formation of the [Fe(h5- C5H5)(CO)(μ-SC5H9N(CH3)2]2I2 · 2H2O salt and [Fe(h5-C5H5)(CO)(μ-SC5- H9NHCH3)]22+ cation, respectively. © 1986.

Original language	English
Pages (from-to)	169-175
Journal	Journal of Organometallic Chemistry
Volume	316
Issue number	1-2
DOIs	https://doi.org/10.1016/0022-328X(86)82085-X
Publication status	Published - 25 Nov 1986

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@article{e815ca31d1304c80a17adde1ab33651b,

title = "Synthesis, crystal structure and properties of [Fe(h5-C5H5)(CO)(μ-SC5H9NCH3)]2",

abstract = "The reaction of Fe2(CO)4(h5-C5H5)2 with 4-N-methylpiperidine-disulphide affords [Fe(h5-C5H5)(μ-SC5H9NCH3]2, the crystal structure of which has been determined. The crystals are monoclinic, space group C2/c with a 18.761(3), b 14.543(2), c 9.556(1) {\AA}, β 103.67(2)°. With Z = 4 the calculated density is 1.46 g cm cm-3; the final weighted R factor was 0.047 for 1645 independent reflections. The two carbonyl groups and the two sulphur-attached piperidine groups in the dimeric structure are both cisoid. Reaction with CH3I leads to methylation that with aqueous HClO4 to protonation of the nitrogen atoms of the piperidine rings, giving formation of the [Fe(h5- C5H5)(CO)(μ-SC5H9N(CH3)2]2I2 · 2H2O salt and [Fe(h5-C5H5)(CO)(μ-SC5- H9NHCH3)]22+ cation, respectively. {\textcopyright} 1986.",

author = "Walter Gaete and Josep Ros and Ramon Ya{\~n}ez and Xavier Solans and Manuel Font-Altaba",

year = "1986",

month = nov,

day = "25",

doi = "10.1016/0022-328X(86)82085-X",

language = "English",

volume = "316",

pages = "169--175",

number = "1-2",

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TY - JOUR

T1 - Synthesis, crystal structure and properties of [Fe(h5-C5H5)(CO)(μ-SC5H9NCH3)]2

AU - Gaete, Walter

AU - Ros, Josep

AU - Yañez, Ramon

AU - Solans, Xavier

AU - Font-Altaba, Manuel

PY - 1986/11/25

Y1 - 1986/11/25

N2 - The reaction of Fe2(CO)4(h5-C5H5)2 with 4-N-methylpiperidine-disulphide affords [Fe(h5-C5H5)(μ-SC5H9NCH3]2, the crystal structure of which has been determined. The crystals are monoclinic, space group C2/c with a 18.761(3), b 14.543(2), c 9.556(1) Å, β 103.67(2)°. With Z = 4 the calculated density is 1.46 g cm cm-3; the final weighted R factor was 0.047 for 1645 independent reflections. The two carbonyl groups and the two sulphur-attached piperidine groups in the dimeric structure are both cisoid. Reaction with CH3I leads to methylation that with aqueous HClO4 to protonation of the nitrogen atoms of the piperidine rings, giving formation of the [Fe(h5- C5H5)(CO)(μ-SC5H9N(CH3)2]2I2 · 2H2O salt and [Fe(h5-C5H5)(CO)(μ-SC5- H9NHCH3)]22+ cation, respectively. © 1986.

AB - The reaction of Fe2(CO)4(h5-C5H5)2 with 4-N-methylpiperidine-disulphide affords [Fe(h5-C5H5)(μ-SC5H9NCH3]2, the crystal structure of which has been determined. The crystals are monoclinic, space group C2/c with a 18.761(3), b 14.543(2), c 9.556(1) Å, β 103.67(2)°. With Z = 4 the calculated density is 1.46 g cm cm-3; the final weighted R factor was 0.047 for 1645 independent reflections. The two carbonyl groups and the two sulphur-attached piperidine groups in the dimeric structure are both cisoid. Reaction with CH3I leads to methylation that with aqueous HClO4 to protonation of the nitrogen atoms of the piperidine rings, giving formation of the [Fe(h5- C5H5)(CO)(μ-SC5H9N(CH3)2]2I2 · 2H2O salt and [Fe(h5-C5H5)(CO)(μ-SC5- H9NHCH3)]22+ cation, respectively. © 1986.

U2 - 10.1016/0022-328X(86)82085-X

DO - 10.1016/0022-328X(86)82085-X

M3 - Article

VL - 316

SP - 169

EP - 175

IS - 1-2

ER -

Synthesis, crystal structure and properties of [Fe(h5-C5H5)(CO)(μ-SC5H9NCH3)]2

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Synthesis, crystal structure and properties of [Fe(h⁵-C₅H₅)(CO)(μ-SC₅H₉NCH₃)]₂