A first example of polyoxotungstate-based giant molecule. Synthesis and molecular structure of a tetrapod-shaped Ti-O-Ti bridged anhydride form of Dawson tri-titanium(iv)-substituted polyoxotungstate

Yoshitaka Sakai; Kenji Yoza; Chika Nozaki Kato; Kenji Nomiya

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A first example of polyoxotungstate-based giant molecule. Synthesis and molecular structure of a tetrapod-shaped Ti-O-Ti bridged anhydride form of Dawson tri-titanium(iv)-substituted polyoxotungstate

机译：基于聚氧钨酸盐的大分子的第一个例子。 Dawson三钛（iv）取代的聚氧钨酸盐的四脚形Ti-O-Ti桥接酸酐形式的合成和分子结构

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The preparation and structural characterization of a giant "tetrapod"-shaped inorganic molecule, [(α-1,2,3-P_2W_(15)Ti_3O_(60.5)_4Cl]~(37-), la (abbreviated to {TiO_6}_(12); FW ～15700), consisting of four tri-Ti~(iv)-1,2,3-substituted α-Dawson substructures and one encapsulated Cl~- ion, are described. A water-soluble, all-inorganic composition compound of the tetrameric Ti-O-Ti bridged anhydride form, Na_xH_(33-X)K_4[1a]·yH_2O, 1 (x = 21-26, y = 60-70), being afforded by a stoichiometric reaction in aqueous solution of tri-lacunary Dawson polyoxotungstate Na_(12)-[B-α-P_2W_(15)O_(56)]·19H_2O with 3 equiv of Ti(SO_4)_2·4H_2O in HCl-acidic aqueous solution followed by exchanging the countercation, was obtained as analytically pure, homogeneous colorless plate crystals. Single-crystal X-ray structure analysis revealed that the polyoxoanion 1a was an inorganic, giant "tetrapod"-shaped molecule (described as a sphere with a diameter of ～31.2 A) with approximately T_d symmetry. Characterization of 1 was also accomplished by complete elemental analysis, TG/DTA, FTIR, UV-vis absorption and solution (~(31)P and (183)W) NMR spectroscopy.

机译：[[α-1,2,3-P_2W_（15）Ti_3O_（60.5）_4Cl]〜（37-），la（缩写为{TiO_6} _）的巨型“四脚”形无机分子的制备与结构表征（12）; FW〜15700），由四个三-Ti〜（iv）-1、2,3-取代的α-道森亚结构和一个包封的Cl〜-离子组成，是一种水溶性，全无机的通过在水溶液中的化学计量反应得到的四聚体Ti-O-Ti桥接酸酐形式的组成化合物Na_xH_（33-X）K_4 [1a]·yH_2O，1（x = 21-26，y = 60-70）含三当量的Ti（SO_4）_2·4H_2O的三酸性道森聚氧钨酸盐Na_（12）-[B-α-P_2W_（15）O_（56）]·19H_2O在HCl酸性水溶液中的溶液，然后交换抗衡阳离子通过分析获得纯净，均匀，无色的板状晶体，单晶X射线结构分析表明，聚氧阴离子1a是无机的巨型“四脚”形分子（描述为直径约为31.2 A的球形），具有近似T_d对称。还可以通过完整的元素分析，TG / DTA，FTIR，UV-vis吸收和溶液（〜（31）P和（183）W）NMR光谱完成1的测定。

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《Dalton transactions: An international journal of inorganic chemistry》 |2003年第18期|共6页
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Yoshitaka Sakai; Kenji Yoza; Chika Nozaki Kato; Kenji Nomiya;
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1. A first example of polyoxotungstate-based giant molecule. Synthesis and molecular structure of a tetrapod-shaped Ti-O-Ti bridged anhydride form of Dawson tri-titanium(iv)-substituted polyoxotungstate [J] . Yoshitaka Sakai, Kenji Yoza, Chika Nozaki Kato, Dalton transactions: An international journal of inorganic chemistry . 2003,第18期

机译：基于聚氧钨酸盐的大分子的第一个例子。 Dawson三钛（iv）取代的聚氧钨酸盐的四脚形Ti-O-Ti桥接酸酐形式的合成和分子结构
2. Synthesis and pH-variable ultracentrifugation molecular weight measurements of the dimeric, Ti-O-Ti bridged anhydride form of a novel di-Ti-IV-1,2-substituted alpha-Keggin polyoxotungstate. Molecular structure of the [(alpha-1,2-PW10Ti2O39)(2)](10-) [J] . Nomiya K., Takahashi M., Widegren JA., Journal of the Chemical Society. Dalton Transactions . 2002,第19期

机译：新型二-Ti-IV-1,2-取代的α-Keggin多氧钨酸盐的二聚体，Ti-O-Ti桥接酸酐形式的合成及pH值可变的超速离心分子量测量。 [（α-1,2-PW10Ti2O39）（2）]（10-）的分子结构
3. Synthesis and characterization of the tetrameric, tri-titanium(IV)-substituted Wells-Dawson-substructure polyoxotungstate, [(P2W15Ti3O60.5)(4)](36-) : the significance of ultracentrifugation molecular weight measurements in detecting aggregated, anhy [J] . Nomiya K., Shimizu Y., Takahashi M., Inorganica Chimica Acta . 2000,第0期

机译：四聚体，三钛（IV）取代的Wells-Dawson亚结构聚氧钨酸盐的合成与表征，[（P2W15Ti3O60.5）（4）]（36-）：超速离心分子量测量在检测聚集的无水硫酸盐中的重要性
4. Catalytic Performance of Copper-Substituted Polyoxotungstate Materials and X-ray Structure of a New Sandwich-Type Compound [C] . Salete S. Balula, Luis Cunha-Silva, Isabel C.M.S. Santos, Advanced Materials Forum IV . 2008

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6. Transformation of Tri-Titanium(IV)-Substituted α-Keggin Polyoxometalate (POM) into Tetra-Titanium(IV)-Substituted POMs : Reaction Products of Titanium(IV) Sulfate with the Dimeric Keggin POM Precursor under Acidic Conditions [O] . Yuki Mouri, Yoshitaka Sakai, Yoshitaka Kobayashi, 2010

机译：三钛（IV）取代的α-Keggin多金属氧酸盐（POM）转变为四钛（IV）取代的POM：酸性条件下硫酸钛（IV）与二聚Keggin POM前体的反应产物
7. Novel Ti-O-Ti Bonding Species Constructed in a Metal-Oxide Cluster: Reaction Products of Bis(oxalato)oxotitanate(IV) with the Dimeric, 1, 2-Dititanium(IV)-Substituted Keggin Polyoxotungstate [O] . -1

机译：在金属氧化物簇中构建的新型Ti-O-Ti粘合物种：双层（oxalato）的反应产物与二聚体，1,2-二硝酸盐（IV） - 二酮 - 取代的Keggin聚氧钨酸盐

A first example of polyoxotungstate-based giant molecule. Synthesis and molecular structure of a tetrapod-shaped Ti-O-Ti bridged anhydride form of Dawson tri-titanium(iv)-substituted polyoxotungstate

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