Unexpected cis-dioxido uranyl carboxylate compound: Synthesis,characterization and photocatalytic activity of uranyl-succinate complexes

Two new complexes formed by uranyl ions with succinic acid and 4,4′-dipyridine have been investigated. Interestingly, the uranium(VI) coordination polymers possess two types dioxido unit, a cis-dioxido bond angle with 115.421(2)°and a trans-dioxido bond angle with 178.421(2)°, respectively. The complexes were characterized by elemental analysis, IR and UV–vis spectroscopy and X-ray crystal diffraction. In addition, the properties of luminescence and photocatalytic analysis were also investigated. The result revealed that the two complexes show different photocatalytic activity in the decomposition of RhB under visible light and UV light irradiation.     

Synthesis and characterization of polymeric complexes of cobalt(II) with chloro substituted 2-hydroxyacetophenone oximes

Summary The polymeric complexes of cobalt (II) with 5-chloro 2-hydroxyacetophenone oxime and 3,5-dichloro-2-hydroxyacetophenone oxime were synthesised and characterized by elemental analysis, magnetic measurements and spectral studies.     

苯基锗吡啶基羧酸酯的合成及表征

利用二或三苯基氯化锗与吡啶基羧酸钠反应，合成了9种苯基锗吡啶基羧酸酯。通过元素分析，红外光谱和核磁共振氢谱对其结构进行表征。     

Di-2-pyridyl ketone oxime in 3d-metal carboxylate cluster chemistry: a new family of mixed-valence Mn2IIMn2III complexes

Several reaction schemes involving di-2-pyridyl ketone oxime, (py)₂CNOH, Mn sources, RCO₂⁻ ligands and X⁻ in MeCN or MeCN/EtOH lead to the new family of mixed-valence complexes [Mn₂^IIMn₂^III(O₂CR)₂X₂{(py)₂CNO}₂{(py)₂CO₂}₂] (R=Me, Ph; X=Cl, Br; (py)₂CO₂²⁻=the gem-diolate(-2) form of di-2-pyridyl ketone). The products have been characterized by single crystal X-ray crystallography and exhibit the same structural motif. Magnetic studies indicate weak antiferromagnetic exchange interactions in the complexes.     

Synthesis and characterization of telechelic phosphine oxide polyesters and cobalt(II) chloride complexes

A monofunctional phosphine oxide containing endcapping reagent, 4-carboxyphenyl biphenyl phosphine oxide, was synthesized for the preparation of telechelic polyester oligomers. The chemical structure of the endcapping reagent was verified using NMR spectroscopy, mass spectroscopy, and elemental analysis. Phosphine oxide telechelic polyesters were prepared for the first time via copolymerization of a low molar mass polyester oligomer precursor and the phosphine oxide endcapping reagent in the melt state. The quantitative incorporation of telechelic phosphine oxide functionality was confirmed using ¹H NMR spectroscopy and elemental analysis. The corresponding complexes of phosphine oxide terminated polyesters and cobalt(II) chloride were prepared via charging the cobalt salt at the onset of melt polymerization. ³¹P {¹H} NMR spectroscopy, FT-IR spectroscopy, and UV-vis spectroscopy indicated that the cobalt(II) ion preferentially coordinated with the phosphine oxide end groups. The complexes exhibited higher melt viscosity than their salt-free analogues due to the formation of coordinated polymers. The presence of the telechelic phosphine oxide end groups also aided in the homogeneous dispersion of the cobalt salt in a poly(ethylene terephthalate) (PET) matrix.     

两种A2B型咔咯化合物的合成及表征

以5-(3-硝基苯基)二吡咯甲烷与2,4-二氯基苯甲醛或2,4-二甲氧基苯甲醛为原料,在水和甲醇溶剂中采用改进的Lindsey法合成了标题化合物,测定了化合物的紫外-可见及荧光光谱,用红外、核磁共振、质谱等技术对化合物的结构进行了表征,结果表明所得产物即为目标配合物。     

2-羟基-2-二茂铁基丙胺过渡金属配合物的合成与表征

采用2-羟基-2-二茂铁基丙胺与Ni(Ⅱ)、Cu(Ⅱ)、Zn(Ⅱ)、Cd(Ⅱ)、Hg(Ⅱ)反应合成了5个新的配合物,经元素分析、红外光谱、核磁共振氢谱、差热-热重分析和摩尔电导对配合物的结构进行了表征,确定配合物的组成为M(FcA)Cl2.nH2O(M=Ni,Cu,Zn,Hg,n分别为5,2,1,0;Cd为Cd(FcA)2Cl2.2H2O),FcA为2-羟基-2-二茂铁基丙胺。     

A trinuclear platinum–cobalt acetate-bridged complex {PtII(acac)}2CoII(μ-OOCMe)4: Synthesis and structure

Reaction of the platinum(II) acetylacetonate Pt(acac)₂ with Co(OOCMe)₂ · 4H₂O in air produced the Pt^II–Co^II heterodimetallic complex {Pt^II(acac)}₂Co^II(μ-OOCMe)₄ as established by single-crystal X-ray diffraction.     

Synthesis,structures, and magnetic properties of tetranuclear nickel and cobalt complexes with 2-mercaptobenzoxazole

The synthesis and magnetic properties of two tetranuclear Ni complex Ni₄(L)₄(CH₃CN)₄(OCH₃)₄ 1 and Co complex Co₄(L)₄(CH₃CN)₄(OCH₃)₄ 2 (HL = 2-mercaptobenzoxazole) are reported. The X-ray structures reveal that 1 and 2 are isostructural with [Ni₄O₄] 1 and [Co₄O₄] 2 cubane-like cores. Analysis of the temperature dependent magnetic measurements data shows that both complexes are paramagnetic with weak antiferromagnetic coupling. One-J model and two-J model are both applied to fit the experimental magnetic data of 1 and the results indicate the exchange coupling between the type A Ni(II) ions affected by NCS three atoms bridge in 2-mercaptobenzoxazole ligand.     

两种甲氧基苯基咔咯配合物的合成与表征

以吡咯和甲氧基苯甲醛为反应起始物,在水和甲醇溶剂中采用改进的Lindsey法合成了4-甲氧基苯基咔咯(a)和2,4-二甲氧基苯基咔咯(b)两种无金属甲氧基苯基咔咯配合物.测定了配合物在二氯甲烷溶剂中的紫外-可见及荧光光谱.发现配合物a和b的Soret分别位于418和420 nm,Q吸收峰则分别位于570、608、645...     

二（2—苯并咪唑亚甲基）胺过渡金属配合物的合成及表征

合成了二（２－苯并咪唑亚甲基）胺及其四种全新的过渡金属的双核配合物。通过元素分析,红外光谱和紫外光谱对配体及配合物进行了结构表征。     

Synthesis and characterization of aspartate polymer complexes

Oligomeric polyester, namely poly(tetramethylene asparate) (PTMA), was synthesized From D ,L ‐aspartic acid and 1,4‐butanediol by a melt codensation technique. Polyester–metal complexes were synthesized by the reaction of PTMA with hydrated acetates of Fe(III), Pd(IV), and UO₂(II) in DMSO. The polyester–metal complexes were characterized by elemental analysis, UV–Vis, IR spectral studies, magnetic susceptibility measurements and ¹H‐NMR. Mossbauer spectra of mixed samples of Pd‐PTMA and Fe(II)‐PTMA with a ratio of 1 : 2 mol showed the iron(III) oxide formed in early stages of the decomposition at 250°C is mainly fine‐grained and as the temperature is increased, well‐crystalline hematic is formed. Above 250°C, the Mossbauer spectrum showed the typical six‐line pattern of magnetically oriented Fe(III) oxide, but at 800°C, the spectrum showed quadrupole interaction characteristic of PdFe₂O₄ spinel. The metal ions were found to be six—coordinated with two water molecules as additional ligands besides oxygen and nitrogen atoms of polyester repeating units. Thermogravimetric analysis (DTA‐TG) showed that co‐ordination polymers are thermally more stable than polyester; the activation parameters for both decomposition steps were calculated and discussed. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 93: 942–947, 2004     

Self-assembly of neutral dinuclear and trinuclear zinc-benzoate complexes

A structurally important self-assembly of dinuclear and trinuclear zinc-benzoate complexes having formula [Zn₃(μ-OBz)₆(py)₂] · [Zn₂(OBz)₄(py)₂] (A) (where OBz is benzoate and py is pyridine ligand) is reported. The dinuclear and trinuclear complexes present in the crystal lattice of the self-assembly are held together by weak C–Hπ and C–HO interactions.     

Synthesis, characterization and catalytic activity of ruthenium-doped cobalt catalysts

Cobalt-based catalysts doped with different amounts of ruthenium supported on Zr-MSU type materials were studied in the hydrogenation and hydrogenolysis/hydrocracking of tetralin at different temperatures. The catalytic tests were carried out in a high-pressure fixed-bed continuous-flow stainless steel catalytic reactor operating at a pressure of 6.0 MPa. Textural, structural, acidic and metallic properties were studied by XRD, XPS, H₂-TPR, NH₃-TPD and Elemental Chemical Analysis. Five catalysts were prepared with 10 wt% of cobalt and a ruthenium loading ranging from 0.5 to 5 wt%, along with a monometallic ruthenium catalyst with 3 wt% of metal, for comparison. From catalysts characterization, no interaction between cobalt and ruthenium can be established, however, the presence of ruthenium influences the reducibility of cobalt.

Ruthenium-doped catalysts not only improve the catalytic activity of monometallic cobalt and ruthenium ones, but also ruthenium acts as a trap for sulphur organic molecules, preserving cobalt particles from sulphur poisoning and thus maintaining their high hydrogenation activity. The catalyst with a ruthenium loading of 3 wt% is found to be the most active, both, with or without sulphur in the feed. The most striking improvement of ruthenium-doped catalyst properties is their greater resistance to sulphur molecules than in the case of monometallic cobalt catalysts, which are otherwise rapidly deactivated under the same experimental conditions.     

Synthesis and characterization of 2-imino-indole nickel complexes and their ethylene oligomerization study

A series of 2-imino-indole derivatives and their neutral nickel complexes were synthesized and characterized. A single-crystal X-ray analysis of [Ni(C₁₀H₇)(C₁₈H₁₆ClN₂)(PPh₃)] shows the nickel center adopted a square-planar coordination geometry. The nickel complexes act solely as effective catalysts for ethylene oligomerization with the activity up to 2.05 × 10⁴ g ethylene mol⁻¹ h⁻¹.     

水溶性二茂钛配合物的合成及表征

二氯二茂钛是一种具有抗肿瘤活性的金属有机化合物。通过二氯二茂钛和水杨酸或甲硫氨酸反应合成了两种二茂钛配合物,经元素分析、红外光谱、核磁共振氢谱和紫外-可见吸收光谱等方法表征了它们的结构。其结果表明:水杨酸配合物为单分子双齿配位的二茂钛配合物,而甲硫氨酸配合物为双分子单齿配位的二茂钛配合物。甲硫氨酸配合物的离子性结构使其具有很好的水溶性,有利于其在生物体系和临床上的使用,同时甲硫氨酸配合物的两个亲脂性的茂环对其渗透进入细胞膜也具有重要作用,因而,它具有较好的临床应用前景。     

Synthesis and spectroscopic characterization of N-substituted thiosemicarbazone complexes

Complexation between Co(II), Ni(II), and Cu(II) with some 3,4-hexanedione bis[N-substituted thiosemicarbazones] has been investigated. The ligands release the two hydrazine hydrogens during the complex formation and act as binegative tetradentate (N₂S₂) except [Cu(H₂Hx4M)Cl₂] and [Cu(H₂Hx4Et)Cl₂]2H₂O in which the ligands behave as neutral tetradentate. The magnetic moments and electronic spectra provide information about the geometry of the complexes, which is supported by calculating the ligand field parameters for the Co(II) complexes. Most Ni(II) complexes are diamagnetic, indicative of a square-planar structure. The bands observed in Nujol are shifted to higher energies in dimethylformamide (DMF) solution, suggesting a weak interaction with the solvent. The ESR spectra of the complexes in solid and DMF solution exhibit axial symmetric g-tensor parameters with g _|>g _⊥>2.0023. The molecular parameters of [Ni(Hx4M)] have been calculated theoretically by semiempirical PM3 method. Also, the electronic transitions were calculated theoretically and found approximately similar to those recorded experimentally.     

纳米四氧化三钴的合成表征及各自在电化学性能的研究

以六水合硝酸钴(Ⅱ)、六水合氯化钴(Ⅱ)为原料制备纳米级别的棒状四氧化三钴、管状四氧化三钴及片状四氧化三钴。利用XRD对制备的产物与原料、中间体进行对比研究,利用SEM观察产物形貌,并利用电化学工作站对不同产物的电化学性能进行研究。经研究发现,在以2 mol/L KOH溶液为电解液的条件下,四氧化三钴纳米棒的电化学性能最为优异。     

两个新型联吡啶类化合物的合成以及表征

我们利用固相合成法,氢氧化钠存在的情况下,分别研磨4-乙酰吡啶和对甲基苯甲醛,对甲基苯乙酮和4-吡啶甲醛,然后再利用醋酸铵合环,高锰酸钾氧化,分别得到了两个新型刚性配体名称4'-(4-羧苯基)-2,4':6',4-三联吡啶(L<,1>)和2,6-二(4-羧苯基)-4,4'-二联吡啶(L<,2>),产率分别为:35.8...