Preparation and structural characterization of Ru~(II)-DMSO and Ru~(III)-DMSO-substituted α-Keggin-type phosphotungstates, [PW_(11)O_(39)Ru~(II)DMSO]~(5-) and [PW _(11)O_(39)Ru~(III)DMSO]~(4-), and catalytic activity for water oxidation

Sadakane M.; Rinn N.; Moroi S.; Kitatomi H.; Ozeki T.; Kurasawa M.; Itakura M.; Hayakawa S.; Kato K.; Miyamoto M.; Ogo S.; Ide Y.; Sano T.

首页> 外文期刊>Zeitschrift fur Anorganische und Allgemeine Chemie >Preparation and structural characterization of Ru~(II)-DMSO and Ru~(III)-DMSO-substituted α-Keggin-type phosphotungstates, [PW_(11)O_(39)Ru~(II)DMSO]~(5-) and [PW _(11)O_(39)Ru~(III)DMSO]~(4-), and catalytic activity for water oxidation

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Preparation and structural characterization of Ru~(II)-DMSO and Ru~(III)-DMSO-substituted α-Keggin-type phosphotungstates, [PW_(11)O_(39)Ru~(II)DMSO]~(5-) and [PW _(11)O_(39)Ru~(III)DMSO]~(4-), and catalytic activity for water oxidation

机译：Ru〜（II）-DMSO和Ru〜（III）-DMSO取代的α-Keggin型磷钨酸盐[PW_（11）O_（39）Ru〜（II）DMSO]〜（5-）的制备及结构表征和[PW _（11）O_（39）Ru〜（III）DMSO]〜（4-）以及对水氧化的催化活性

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Ru~(II)-and Ru~(III)-substituted α-Keggin-type phosphotungstates with a dimethyl sulfoxide (DMSO) ligand, [PW _(11)O_(39)Ru~(II)DMSO]~(5-) (1) and [PW _(11)O_(39)Ru~(III)DMSO]~(4-) (2), were synthesized. Compound 1 was prepared by reaction of [PW_(11)O _(39)]~(7-) with [Ru~(II)(DMSO)_4]Cl _2 in water at 125 °C under hydrothermal conditions and was isolated as a cesium salt. Compound 2 was prepared by reaction of 1 with bromine in water at 60 °C and was isolated as a cesium salt. The compounds were characterized by cyclic voltammetry, elemental analysis, UV/Vis, IR, ~(31)P NMR, ~(183)W NMR, ~1H NMR, and XANES (Ru K-edge and L_3-edge)spectroscopic methods. Single crystal structural analysis of 1 revealed that Ru~(II) is incorporated in the α-Keggin framework and coordinated by DMSO through a Ru-S bond. Cyclic voltammetry of 1 indicated that the incorporated Ru~(II)-DMSO is reversibly oxidizable to the Ru~(III)-DMSO derivative 2. Compound 1 showed catalytic activity for water oxidation in the presence of cerium ammonium nitrate as an oxidant.

机译：具有二甲亚砜（DMSO）配体[PW _（11）O_（39）Ru〜（II）DMSO]〜（5-）的Ru〜（II）和Ru〜（III）取代的α-Keggin型磷钨酸盐）（1）和[PW _（11）O_（39）Ru〜（III）DMSO]〜（4-）（2）。在水热条件下，[PW_（11）O _（39）]〜（7-）与[Ru〜（II）（DMSO）_4] Cl _2在水中于125°C的反应制备化合物1，并分离为铯盐。通过使1与溴在60°C的水中反应制备化合物2，并将其分离为铯盐。通过循环伏安法，元素分析，UV / Vis，IR，〜（31）P NMR，〜（183）W NMR，〜1H NMR和XANES（Ru K边和L_3-edge）光谱法对化合物进行表征。 1的单晶结构分析表明，Ru〜（II）结合在α-Keggin骨架中，并通过DMSO通过Ru-S键配位。循环伏安法为1表示掺入的Ru〜（II）-DMSO可逆地氧化为Ru〜（III）-DMSO衍生物2。在硝酸铈铵铵作为氧化剂的存在下，化合物1对水氧化具有催化活性。

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《Zeitschrift fur Anorganische und Allgemeine Chemie》 |2011年第11期|共8页
作者
Sadakane M.; Rinn N.; Moroi S.; Kitatomi H.; Ozeki T.; Kurasawa M.; Itakura M.; Hayakawa S.; Kato K.; Miyamoto M.; Ogo S.; Ide Y.; Sano T.;
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正文语种 eng
中图分类化学;
关键词
Oxidation; Polyoxometalates; Redox chemistry; Ruthenium; S ligands;

机译：氧化;多金属氧酸盐;氧化还原化学;钌;S配体;

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1. Preparation and structural characterization of Ru~(II)-DMSO and Ru~(III)-DMSO-substituted α-Keggin-type phosphotungstates, [PW_(11)O_(39)Ru~(II)DMSO]~(5-) and [PW _(11)O_(39)Ru~(III)DMSO]~(4-), and catalytic activity for water oxidation [J] . Sadakane M., Rinn N., Moroi S., Zeitschrift fur Anorganische und Allgemeine Chemie . 2011,第11期

机译：Ru〜（II）-DMSO和Ru〜（III）-DMSO取代的α-Keggin型磷钨酸盐[PW_（11）O_（39）Ru〜（II）DMSO]〜（5-）的制备及结构表征和[PW _（11）O_（39）Ru〜（III）DMSO]〜（4-）以及对水氧化的催化活性
2. Determination of α-Keggin structure of [GeW_(11)O_(39)Ru~(III)(H_2O)]~(5-). Reaction of [GeW_(11)O_(39)Ru_(III)(H_2O)]~(5-) with dimethyl sulfoxide to form [GeW_(11)O_(39)Ru~(III)(dmso)]~(5-) and their structural characterization [J] . Ogo S., Shimizu N., Ozeki T., Dalton transactions: An international journal of inorganic chemistry . 2013,第7期

机译：[GeW_（11）O_（39）Ru〜（III）（H_2O）]〜（5-）的α-Keggin结构的确定。 [GeW_（11）O_（39）Ru_（III）（H_2O）]〜（5-）与二甲亚砜反应形成[GeW_（11）O_（39）Ru〜（III）（dmso）]〜（5 -）及其结构表征
3. Microwave-Assisted Rapid Incorporation of Ruthenium into Lacunary Keggin-Type Polyoxotungstates: One-Step Synthesis, ~(99)Ru, ~(183)W NMR Characterization and Catalytic Activity of [PW_(11)O_(39)Ru~(II)(DMSO)]~(5-) [J] . Alessandro Bagno, Marcella Bonchio, Andrea Sartorel, European journal of inorganic chemistry . 2000,第1期

机译：微波辅助将钌快速掺入La的Keggin型多氧钨酸盐中：[PW_（11）O_（39）Ru〜（II）的一步合成，〜（99）Ru，〜（183）W NMR表征和催化活性（DMSO）]〜（5-）
4. Preparation and Characterization of New Lanthanide materials: Layered Double Hydroxide Intercalated by Luminescent Polyoxometalate Anions with Dawson-likeEu(H_2O)_3(α_2-P_2W_(17)O_(61))~(7-) and Keggin-likeEu(H_2O)_2(PW_(11)O_(39))~(4-) [C] . Nanotechnology conference and trade show . 2003

机译：新型镧系元素材料的制备与表征：用Dawsh样液嵌入的分层双氢氧化液相传，具有Dawson样液Eu（H_2O）_3（α_2-P_2W_（17）O_（61））〜（7-）和Keggin样欧盟（H_2O）_2（PW_（11）O_（39））〜（4-）
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6. A Series of Supramolecular Complexes for Solar Energy Conversion via Water Reduction to Produce Hydrogen: An Excited State Kinetic Analysis of Ru(II)Rh(III)Ru(II) Photoinitiated Electron Collectors [O] . Travis A. White, Jessica D. Knoll, Shamindri M. Arachchige, 2012

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Preparation and structural characterization of Ru~(II)-DMSO and Ru~(III)-DMSO-substituted α-Keggin-type phosphotungstates, [PW_(11)O_(39)Ru~(II)DMSO]~(5-) and [PW _(11)O_(39)Ru~(III)DMSO]~(4-), and catalytic activity for water oxidation

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