Synthesis of mononuclear and dinuclear ruthenium(II)tris(heteroleptic)complexes via photosubstitution in bis(carbonyl)precursors

Declan Mulhern; Sally Brooker; Helmar Gorls; Sven Rau; Johannes G.Vos

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Synthesis of mononuclear and dinuclear ruthenium(II)tris(heteroleptic)complexes via photosubstitution in bis(carbonyl)precursors

机译：在双（羰基）前体中光解合成单核和双核三（杂）钌（II）配合物

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A novel,and quite general,approach for the preparation of tris(heteroleptic)ruthenium(II)complexes is reported.Using this method,which is based on photosubstitution of carbonyl ligands in precursors such as [Ru(bpy)(CO)_2Cl_2] and [Ru(bpy)(Me_2bpy)(CO)_2](PF_6)_2,mononuclear and dinuclear Ru(II)tris(heteroleptic)polypyridyl complexes containing the bridging ligands 3,5-bis(pyridin-2-yl)-1,2,4-triazole(Hbpt)and 3,5-bis(pyrazin-2-yl)-1,2,4-triazole(Hbpzt)have been prepared.The complexes obtained were purified by column chromatography and characterized by HPLC,mass spectrometry,~1H NMR,absorption and emission spectroscopy and by electrochemical methods.The X-ray structures of the compounds [Ru(bpy)(Me_2bpy)(bpt)](PF_6)centre dot 0.5C_4H_(10)O [1 centre dot 0.5C_4H_(10)O],[Ru(bpy)(Me_2bpy)(bpzt)]-(PF_6)centre dot H_2O(2 centre dot H_2O)and [Ru(bpy)(Me_2bpy)(CH_3CN)_2](PF_6)_2 centre dot C_4H_(10)O(6 centre dot C_4H_(10)O)are reported.The synthesis and characterisation of the dinuclear analogues of 1 and 2,[{Ru(bpy)(Me_2bpy)}_2bpt](PF_6)_3 centre dot 2H_2O(3)and [{Ru(bpy)(Me_2bpy)}_2bpzt](PF_6)_3(4),are also described.

机译：报道了一种新颖的，非常通用的制备三（杂）钌（II）配合物的方法。使用这种方法是基于前体如[Ru（bpy）（CO）_2Cl_2]中羰基配体的光解。和[Ru（bpy）（Me_2bpy）（CO）_2]（PF_6）_2，单核和双核Ru（II）三（杂多）多吡啶基配合物，它们包含桥联配体3,5-双（吡啶-2-基）-1制备了2,2,4-三唑（Hbpt）和3,5-双（吡嗪-2-基）-1,2,4-三唑（Hbpzt）。得到的配合物经柱色谱纯化，HPLC鉴定，质谱，〜1H NMR，吸收和发射光谱以及电化学方法。化合物[Ru（bpy）（Me_2bpy）（bpt）]（PF_6）中心点0.5C_4H_（10）O的X射线结构[1中心点0.5C_4H_（10）O]，[Ru（bpy）（Me_2bpy）（bpzt）]-（PF_6）中心点H_2O（2中心点H_2O）和[Ru（bpy）（Me_2bpy）（CH_3CN）_2] [PF_6 ）_2中心点C_4H_（10）O（6个中心点C_4H_（10）O）的报道。双核肛门的合成与表征1和2的对数，[{Ru（bpy）（Me_2bpy）} _ 2bpt]（PF_6）_3中心点2H_2O（3）和[{Ru（bpy）（Me_2bpy）} _ 2bpzt]（PF_6）_3（4）也有描述。

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《Dalton transactions: An international journal of inorganic chemistry》 |2006年第1期|共7页
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Declan Mulhern; Sally Brooker; Helmar Gorls; Sven Rau; Johannes G.Vos;
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1. Synthesis of mononuclear and dinuclear ruthenium(II)tris(heteroleptic)complexes via photosubstitution in bis(carbonyl)precursors [J] . Declan Mulhern, Sally Brooker, Helmar Gorls, Dalton transactions: An international journal of inorganic chemistry . 2006,第1期

机译：在双（羰基）前体中光解合成单核和双核三（杂）钌（II）配合物
2. Synthesis and photophysics of one mononuclear Mn(III) and one dinuclear Mn(III,III) complex covalently linked to a ruthenium(II) tris(bipyridyl) complex [J] . Johansson A., Abrahamsson M., Magnuson A., Inorganic Chemistry: A Research Journal that Includes Bioinorganic, Catalytic, Organometallic, Solid-State, and Synthetic Chemistry and Reaction Dynamics . 2003,第23期

机译：一种单核Mn（III）和一种双核Mn（III，III）配合物与钌（II）三（联吡啶）配合物共价连接的合成及光物理
3. Synthesis, spectroscopic and electrochemical properties of mononuclear and dinuclear bis(bipy)ruthenium(II) complexes containing dimethoxyphenyl(pyridin-2-yl)-1,2,4-triazole ligands [J] . Passaniti P., Browne WR., Lynch FC., Journal of the Chemical Society, Dalton Transactions. Inorganic Chemistry . 2002,第8期

机译：含二甲氧基苯基（吡啶-2-基）-1,2,4-三唑配体的单核和双核双（联吡啶）钌（II）配合物的合成，光谱和电化学性质
4. SERR, FT-Raman, and FT-IR Spectroscopies of Mono- and Dinuclear Ruthenium(II) Bipyridine Complexes with 1,4-Bis ([1,10]Phenanthroline-[5,6-D]Imidazol-2-Yl)Benzene Ligand [C] . Xiao-Yuan Li International conference on Raman spectroscopy;ICORS 2000 . 2000

机译：具有1,4-双（[1,10] Phenanthroline- [5,6-D] Imidazol-2-Yl）苯的单核和双核钌（II）联吡啶配合物的SERR，FT-Raman和FT-IR光谱配体
5. Parallel synthesis, biological evaluation, and stereochemical control of tris-heteroleptic ruthenium(II) complexes. [D] . Mulcahy, Seann Patrick. 2009

机译：Tris-heteroleptic钌（II）配合物的平行合成，生物学评估和立体化学控制。
6. Rhenium(I) Carbonyl Complexes of 246-Tris(2-pyridyl)-135-triazine (TPT). Rhenium(I)-Promoted Methoxylation of the Triazine Ring Carbon Atom in Dinuclear Rhenium Complexes [O] . Xiaoyuan Chen, Frank J. Femia, John W. Babich, -1

机译：246-三（2-吡啶基）-135-三嗪（TPT）的Carbon（I）羰基配合物。 nu（I）促进双核R配合物中三嗪环碳原子的甲氧基化
7. Synthesis, spectroscopic and electrochemical properties of mononuclear and dinuclear bis(bipy)ruthenium(II) complexes containing dimethoxyphenyl(pyridin-2-yl)-1,2,4-triazole ligands [O] . Passaniti Paolo, Browne Wesley R., Lynch Fiona C., 2002

机译：含二甲氧基苯基（吡啶-2-基）-1,2,4-三唑配体的单核和双核双（联吡啶）钌（II）配合物的合成，光谱和电化学性质

Synthesis of mononuclear and dinuclear ruthenium(II)tris(heteroleptic)complexes via photosubstitution in bis(carbonyl)precursors

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