Synthesis of novel mononuclear and dinuclear ruthenium(II) complexes with terpyridine and acetylacetonate ancillary ligands and cyanamide derivative ligands
Several new mononuclear and dinuclear ruthenium(II) complexes incorporating 2,2′:6′,2″-terpyridine and acetylacetonate as ancillary ligands and phenylcyanamide derivative ligands of the type [Ru(tpy)(acac)(L)] and [{Ru(tpy)(acac)} 2(μ-L′)] (where tpy = 2,2′:6′,2″-terpyridine, acac = acetylacetonate,...
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| Published in: | Inorganica Chimica Acta Vol. 358; no. 7; pp. 2384 - 2394 |
|---|---|
| Main Authors: | , , |
| Format: | Journal Article |
| Language: | English |
| Published: |
Elsevier B.V
15-04-2005
Elsevier |
| Subjects: | |
| Online Access: | Get full text |
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| Summary: | Several new mononuclear and dinuclear ruthenium(II) complexes incorporating 2,2′:6′,2″-terpyridine and acetylacetonate as ancillary ligands and phenylcyanamide derivative ligands of the type [Ru(tpy)(acac)(L)] and [{Ru(tpy)(acac)}
2(μ-L′)] (where tpy
=
2,2′:6′,2″-terpyridine, acac
=
acetylacetonate, L
=
hmbpcyd
=
4-(3-hydroxy-3-methylbutynyl)phenylcyanamide anion and epcyd
=
4-ethynylphenylcyanamide anion and L′
=
bcpda
=
bis(4-cyanamidophenyl)diacetylene dianion and bcpea
=
9,10-bis(4-cyanamidophenylethynyl)anthracene dianion) have been prepared and characterized by spectroscopies and X-ray.
Several new mononuclear and dinuclear ruthenium(II) complexes – incorporating 2,2′:6′,2″-terpyridine and acetylacetonate as ancillary ligands and phenylcyanamide derivative ligands – of the type [Ru(tpy)(acac)(L)] and [{Ru(tpy)(acac)}
2(μ-L′)] (where tpy
=
2,2′:6′,2″-terpyridine, acac
=
acetylacetonate, L
=
hmbpcyd
=
4-(3-hydroxy-3-methylbutynyl)phenylcyanamide anion (
2) and epcyd
=
4-ethynylphenylcyanamide anion (
3) and L′
=
bcpda
=
bis(4-cyanamidophenyl)diacetylene dianion (
4) and bcpea
=
9,10-bis(4-cyanamidophenylethynyl)anthracene dianion (
5)) were synthesized in a stepwise manner starting from [Ru(tpy)(acac)(Ipcyd)] (
1), where Ipcyd
=
4-iodophenylcyanamide anion. Tetraphenylarsonium salts of the phenylcyanamide derivative ligands were also prepared. The four complexes have been characterized by UV–Vis, IR, ES-MS, electrochemistry and
1H NMR. Mononuclear complexes
2 and
3 were further characterized by
13C NMR. The single crystal X-ray structure of
2 was determined, it crystallized with one molecule of water with empirical formula of C
32H
31N
5O
5Ru, in a monoclinic crystal system and space group of
P2
1
/n with
a
=
17.642(5)
Å,
b
=
9.634(2)
Å,
c
=
20.063(7)
Å,
β
=
92.65(3)°,
V
=
3406(2)
Å
3 and
Z
=
4. The structure was refined to a final
R factor of 0.040. The Ru(III/II) couple of
1–
3 appeared around 0.34
V versus the saturated calomel electrode in dimethylformamide and at a slightly higher potential, around 0.36–0.37
V for
4 and
5. Spectroelectrochemical studies were also performed for
4 and
5, no intervalence transition was observed despite all attempts. |
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| ISSN: | 0020-1693 1873-3255 0020-1693 |
| DOI: | 10.1016/j.ica.2005.01.004 |