The title compd. was prepd. from a mixt. of Re(CO)3(bpy)Cl and AgPF6 in CH2Cl2 and MeOH which was stirred for 18 h at room temp. After filtration and solvent removal, the yellow residue was redissolved in CH2Cl2 and treated with a soln. of TCNQ in the same solvent. After pptn. with n-pentane and recrystn., dark blue rods of (m4-TCNQ)fac-Re(CO)3(bpy)4(PF6)4 were isolated which were used for a single-crystal x-ray structure detn. The compd. is monoclinic, space group P21/n, a 10.3137(4), b 22.0360(5), c 20.6476(6) \AA, b 97.2520(1)°, Z = 2, dc = 1.776, R = 0.0603, and Rw = 0.1564 for 6048 obsd. reflections with I0 \textgreater 2s(Io). The structure of the complex cation is described and discussed and bonding lengths are given. The complex was characterized by elemental anal., 1H-NMR spectroscopy, measurements of the redn. potential, and UV-vis and IR spectroelectrochem. measurements. on SciFinder(R)
%0 Journal Article
%1 Hartmann.2001
%A Hartmann, Heiko
%A Kaim, Wolfgang
%A Hartenbach, Ingo
%A Schleid, Thomas
%A Wanner, Matthias
%A Fiedler, Jan.
%D 2001
%J Angewandte Chemie, International Edition
%K bipyridyl carbonyl complex crystal cyanoquinodimethane fluorophosphate mol potential rhenium structure;redn synthesis
%N 15
%P 2842--2844
%R 10.1002/1521-3773(20010803)40:15\textless2842::AID-ANIE2842\textgreater3.0.CO;2-R
%T A fully characterized complex ion with unreduced TCNQ as fourfold bridging ligand. (m4-TCNQ)fac-Re(CO)3(bpy)44+
%V 40
%X The title compd. was prepd. from a mixt. of Re(CO)3(bpy)Cl and AgPF6 in CH2Cl2 and MeOH which was stirred for 18 h at room temp. After filtration and solvent removal, the yellow residue was redissolved in CH2Cl2 and treated with a soln. of TCNQ in the same solvent. After pptn. with n-pentane and recrystn., dark blue rods of (m4-TCNQ)fac-Re(CO)3(bpy)4(PF6)4 were isolated which were used for a single-crystal x-ray structure detn. The compd. is monoclinic, space group P21/n, a 10.3137(4), b 22.0360(5), c 20.6476(6) \AA, b 97.2520(1)°, Z = 2, dc = 1.776, R = 0.0603, and Rw = 0.1564 for 6048 obsd. reflections with I0 \textgreater 2s(Io). The structure of the complex cation is described and discussed and bonding lengths are given. The complex was characterized by elemental anal., 1H-NMR spectroscopy, measurements of the redn. potential, and UV-vis and IR spectroelectrochem. measurements. on SciFinder(R)
@article{Hartmann.2001,
abstract = {The title compd. was prepd. from a mixt. of [Re(CO)3(bpy)Cl] and AgPF6 in CH2Cl2 and MeOH which was stirred for 18 h at room temp. After filtration and solvent removal, the yellow residue was redissolved in CH2Cl2 and treated with a soln. of TCNQ in the same solvent. After pptn. with n-pentane and recrystn., dark blue rods of [(\textgreek{m}4-TCNQ){fac-Re(CO)3(bpy)}4](PF6)4 were isolated which were used for a single-crystal x-ray structure detn. The compd. is monoclinic, space group P21/n, a 10.3137(4), b 22.0360(5), c 20.6476(6) {\AA}, \textgreek{b} 97.2520(1)°, Z = 2, dc = 1.776, R = 0.0603, and Rw = 0.1564 for 6048 obsd. reflections with I0 {\textgreater} 2\textgreek{s}(Io). The structure of the complex cation is described and discussed and bonding lengths are given. The complex was characterized by elemental anal., 1H-NMR spectroscopy, measurements of the redn. potential, and UV-vis and IR spectroelectrochem. measurements. [on SciFinder(R)]},
added-at = {2019-07-15T13:41:23.000+0200},
author = {Hartmann, Heiko and Kaim, Wolfgang and Hartenbach, Ingo and Schleid, Thomas and Wanner, Matthias and Fiedler, Jan.},
biburl = {https://puma.ub.uni-stuttgart.de/bibtex/2d12ada7de5d66c8dc7682b7766cc2005/b_schwederski},
doi = {10.1002/1521-3773(20010803)40:15{\textless}2842::AID-ANIE2842{\textgreater}3.0.CO;2-R},
interhash = {47856c56bfaecd51079f622f20d617b5},
intrahash = {d12ada7de5d66c8dc7682b7766cc2005},
issn = {1433-7851},
journal = {Angewandte Chemie, International Edition},
keywords = {bipyridyl carbonyl complex crystal cyanoquinodimethane fluorophosphate mol potential rhenium structure;redn synthesis},
number = 15,
pages = {2842--2844},
timestamp = {2019-07-15T11:42:10.000+0200},
title = {A fully characterized complex ion with unreduced TCNQ as fourfold bridging ligand. [(\textgreek{m}4-TCNQ){fac-Re(CO)3(bpy)}4]4+},
volume = 40,
year = 2001
}
