配合物[Fe(CTS)2]·5SO4·7H2O的热分解动力学

研究了壳聚糖对Fe2+的吸附行为,并进行了条件优化,得到了较为理想的合成产物.通过红外光谱和紫外光谱进行了表征,进而用化学分析、元素分析确定了配合物的组成,并利用TG-DSC分析,采用常用的22种机理函数,对非等温动力学数据进行了线性回归拟合处理,求得了配合物主要分解阶段热动力学最可机理函数和动力学参数(E和A).     

[Er(C_4H_4O_5)_3]·2NaClO_4·6H_2O晶体中Er~(3+)离子能级的配位场分析

采用点群链R(3)*O*D3*关系标记D3*点群的斯塔克能级。基于双层点电荷配位场(DSCPCF)和经典的简单点电荷配位场(PCF)两种模型,利用自编的计算程序对三角对称(D3)的[Er(C4H4O5)3].2NaC lO4.6H2O晶体中Er3+离子的65个配位场微扰能级进行了理论计算和归属,计算结果与实验能级进行比较,DSCPCF模型得到的均方根偏差(σ)为19.9 cm-1,而PCF模型计算的为25.5 cm-1,表明前者模型更为优越,它是基于实际的配位结构并且仅包含较少的拟合参数。     

配合物[Fe(CTS)_2]·SO_4·7H_2O的热分解动力学

研究了壳聚糖对Fe2 + 的吸附行为 ,并进行了条件优化 ,得到了较为理想的合成产物。通过红外光谱和紫外光谱进行了表征 ,进而用化学分析、元素分析确定了配合物的组成 ,并利用TG DSC分析 ,采用常用的 2 2种机理函数 ,对非等温动力学数据进行了线性回归拟合处理 ,求得了配合物主要分解阶段热动力学最可机理函数和动力学参数 (E和A)。     

[(CH3)2NH2]3[NSiMo12O40]·2DMF·4H2O的合成和晶体结构

电荷转移盐;[(CH3)2NH2]3[NSiMo12O40]·2DMF·4H2O的合成和晶体结构     

[Gd(Gly)3(H2O)2]Cl3·H2O的合成与晶体结构

氯化钆;甘氨酸;固态配合物;[Gd(Gly)3(H2O)2]Cl3·H2O的合成与晶体结构     

Dawson结构多金属氧酸电荷转移化合物[CH3NH2CH3]2[CH3NHCH3]4H4[P2W18O62]·H2O的合成、表征及晶体结构

钨磷酸;二甲胺;Dawson结构多金属氧酸电荷转移化合物[CH3NH2CH3]2[CH3NHCH3]4H4[P2W18O62]·H2O的合成、表征及晶体结构     

[Cu(H_2O)(phen)_2](CIO_4)_2的晶体结构

标题化合物晶体属三斜晶系;空间群为P_1;晶胞参数:a=8.182(2)A,b=10.389(2)A,c=16.261(5)A,α=99.38(2)°,β=89.97(2)°,γ=113.18(2)°;Z=2,两个phen上的四个N原子和一个配位水中的O原子围绕中心体Cu原子形成一个畸变的三角双锥构型,配位水与阴离子ClO_4~-中的O原子形成氢键。     

(NH4)11Gd[Gd4Mo29O100(H2O)16]·33H2O杂多化合物在苯酚羟化反应中的催化活性

对苯二酚;过氧化氢;(NH4)11Gd[Gd4Mo29O100(H2O)16]·33H2O杂多化合物在苯酚羟化反应中的催化活性     

超分子化合物[C6H11NH3]6[P2Mo18O62]·4H2O的水热法合成及结构

超分子化合物[C6H11NH3]6[P2Mo18O62]·4H2O的水热法合成及结构;Wells-Dawson结构;杂多化合物     

NH_4Al(SO_4)_2·12H_2O的热分解动力学研究

采用热分析(TG-DTA/DTG)、X射线衍射(XRD)研究了固态物质NH4Al(SO4)2.12H2O在氩气中的热分解过程。热分析结果表明,NH4Al(SO4)2.12H2O在氩气中分5步分解,其质量变化率与理论计算相吻合。XRD结果表明,NH4Al(SO4)2.12H2O热分解的最终产物为Al2O3。用Friedman法对各步分解过程的活化能Ea进行了计算,依此为初始值,采用多元非线性回归法得到各个分解步骤可能的动力学模型和参数。     

[C5H5Fe(CO)2]LnCl2·nTHF和[C5H5Fe(CO)2][C5H4(SiMe3)]LnCl·nTHF双核配合物的合成

合成了稀土铁双核配合物:(C₅H₅Fe(CO)₂)LnCl₂·nTHF(Ln=Nd,Sm,Gd;n=1,2)和(C₅H₅Fe(CO)₂)(C₅H₄(SiMe₃))·LnCl·nTHF(Ln=Nd,Sm,Gd;n=0,1,2)。元素分析,热分析,红外光谱和质谱分析确认了这两种配合物。红外光谱数据表明铁与稀土原子是以羰基桥连接。晶体结构分析表明((C₅H₅Fe(CO)₂)Na·4THF是(C₅H₅Fe(CO)₂)LnCl₂·nTHF合成的中间体。     

K_6[P_2W_(18)O_(62)]·14H_2O制备及性质表征实验教学研究

Dawson结构多酸化合物K_6[P_2W_(18)O_(62)]·14H_2O的制备及性质表征实验,通过水溶液回流方法制备,利用红外光谱、热重分析和电化学方法表征其性质。该实验中采用了经典的多酸化合物制备方法,不但产物具有良好的电致变色性质,而且将多酸化学研究的方法和思路,化合物制备、测试、数据分析等训练融入到"多酸化学"实验课的教学中,加深了学生对多酸化学相关知识点的理解,探索提升无机化学研究生科研素质的实验教学。     

K2[Mo2O4(C2O4)2(H2O)2]·3H2O

The crystal and molecular structure of dipotassium di‐μ‐oxo‐bis[aqua(oxalato‐O¹,O²)oxomolybdenum(III)] trihydrate, K₂­[Mo₂O₄(C₂O₄)₂(H₂O)₂]·3H₂O, has been determined from X‐ray diffraction data. In the dimeric anion, which has approximate twofold symmetry, each Mo atom is in a distorted octahedral coordination, being bonded to one terminal oxo‐O atom, two bridging O atoms, two O atoms from the oxalato ligand and one from the water mol­ecule. Bond lengths trans to the multiple‐bonded terminal oxo ligand are larger than those in the cis position, confirming the trans influence as a generally valid rule.     

Preparation of57Fe enriched K4[Fe(CN)6] and K3[Fe(CN)6]

A simple method to prepare⁵⁷Fe enriched K₄[Fe(CN)₆] and K₃[Fe(CN)₆] is described. The yields of the products are much better than those reported in the literature so far. The enrichment is essential for⁵⁷Fe Mössbauer investigation in a variety of Prussiate type complexes and other inorganic compounds which are conveniently prepared from K₄[Fe(CN)₆] and K₃[Fe(CN)₆]. K₄[Fe(CN)₆] was obtained by reacting freshly prepared Fe(OH)₃ with glacial acetic acid and treating with iron acetate in boiling aqueous solution of KCN. The novel feature of the procedure to obtain K₃[Fe(CN)₆] is that the oxidation of K₄[Fe(CN)₆] has been carried out in the solid state by passing chlorine gas over the powdered specimen. K₃[Fe(CN)₆] was crystallised from alkaline solution of this oxidised powder. The compounds were characterised by Mössbauer spectroscopy.     

Kristallstruktur von Kaliumtriflat‐Butyrolacton, [K3(O3SCF3)3(O2C4H6)2]

Crystal Structure of Potassium Triflate‐butyrolactone, [K₃(O₃SCF₃)₃(O₂C₄H₆)₂] Single Crystals of [K₃(O₃SCF₃)₃(O₂C₄H₆)₂] ( 1 ) have been obtained as a by‐product from the reaction of KNPPh₃ with Yb(O₃SCF₃)₃ in THF with subsequent addition of butyrolactone. The structure of 1 consists of three symmetry‐independent potassium ions which are linked by the oxygen atoms of the triflate ions and the butyrolactone molecules to give a supramolecular structure with layers normal to the crystallographic b‐axis. The carbonyl oxygen atoms of both butyrolactone molecules show a μ₃‐bridging function between three K⁺ ions, one of them is, in addition, coordinated by the ring O‐atom in a chelate manner. 1 : Space group P2₁/c, Z = 4, lattice dimensions at 193 K: a = 1155.0(1), b = 1537.2(1), c = 1531.1(1) pm, β = 100.623(7)°, R = 0.0484.     

4:2钼、钨过氧配合物的制备、结构及其氧化还原分解行为

本文作者曾在用过钨酸分解法制备钨酸的过程中发现, 溶液中W与O2^2^-之比始终为2:1, 这一事实说明溶液中有2:1金属过氧配合物形成, 2:1铂过氧络合物[Mo4O12(O2)2]^4^-文献上已有记载, 但类似的钨配合物尚未见报道。本文制备了这二种配合物, 对比它们的红外和Raman光谱, 并用循环伏安法, 恒电位电解法探讨它们的氧化还原分解体系。