The trinuclear nickel? complex Ni3(C11H11N2O3)2(C5H5N)4 was prepared by the reaction of Ni(OAc)2· 4H2O with N butylsalicylhydrazide Schiff base ligand and characterized by X ray crystallography. The crystal belon...The trinuclear nickel? complex Ni3(C11H11N2O3)2(C5H5N)4 was prepared by the reaction of Ni(OAc)2· 4H2O with N butylsalicylhydrazide Schiff base ligand and characterized by X ray crystallography. The crystal belongs to triclinic, Mr=930.91, space group with cell parameters a=9.8489(2)? , b=12.3110(2)? , c=18.4035(3)? , α =71.353(2)° , β =76.638(2)° ,γ =84.815(2)° ,V=2056.72(6)? 3,Z=2,Dc=1.503g· cm- 3, μ (MoKα ) =1.417mm- 1, F(000)=964, R=0.0317, wR=0.0868. A total of 5393 independent reflections were collected, of which 4448 reflections with I ≥ 2σ (I) were observed. There are two centrosymmetrical trinuclear molecules in a unit cell, each molecule exhibits a linear trinuclear metal arrangement with the Ni... Ni... Ni angle of 180° . The interatomic distances between the nickel atoms on the two sides are 9.2030(8)? and 9.1876(9)? for the two molecules, respectively. The central nickel atom adopts an axially elongated octahedral geometry whereas the nickel atoms on the two sides have square planar coordination environment. CCDC: 194083.展开更多
A series of novel silica-based hybrid adsorbents were prepared by the crosslinking reaction of N-[3- （trimethoxysilyl）propyl] ethylene diamine （TMSPEDA） with epichlorohydrin （ECH） via a sol-gel process. Fourier ...A series of novel silica-based hybrid adsorbents were prepared by the crosslinking reaction of N-[3- （trimethoxysilyl）propyl] ethylene diamine （TMSPEDA） with epichlorohydrin （ECH） via a sol-gel process. Fourier transform infrared （FTIR） spectra confirmed that the reaction occurred. TGA curves showed that the thermal stability of these hybrid adsorbents reached as high as 180 ℃. As a typical example, the adsorption performance of nickel（U） ions onto an adsorbent （the volume ratio of TMSPEDA and ECH was 4：1 ） was explored. It was found that the adsorption of nickel（Ⅱ） ions onto this adsorbent followed the Lagergren pseudo-second-order kinetic model. The investigation of the adsorption mechanism demonstrated that nickel（Ⅱ） adsorption was chiefly controlled by diffusion-chemisorption, suggesting that more diffusion processes were involved in the adsorption of nickel（Ⅱ） ions onto this type of adsorbents. Desorption experiment indicates that these hybrid adsorbents can be regenerated. These findings reveal that this type of silica-based hybrid adsorbent is promising in the separation and recovery of nickel（Ⅱ） ions from Ni-containing wastewater or contaminated water.展开更多
2,4-Bis(3,5-dimethylpyrazol-1-yl)-6-methoxyl-1,3,5-triazine(bpt) has been synthesized by using a new, simple and general method with high yields. Reactions of bpt with Ni(ClO4)2·6H2O and Zn(ClO4)2·6H2O in me...2,4-Bis(3,5-dimethylpyrazol-1-yl)-6-methoxyl-1,3,5-triazine(bpt) has been synthesized by using a new, simple and general method with high yields. Reactions of bpt with Ni(ClO4)2·6H2O and Zn(ClO4)2·6H2O in methanol gave mononuclear complex [Ni(bpt)2]· (ClO4)2·H2O and ternary complex [Zn(mpt)2(dmp)](ClO4)2 respectively, where mpt (2,4-dimethoxy-6-(3,5-dimethyl- pyrazol-1-yl)-1,3,5-triazine) and dmp(3,5-dimethylpyrazole) are the alcoholysis products of bpt in the presence of Zn2+ ion. A possible mechanism for this catalytic reaction was proposed. X-ray crystal structure for ligand bpt, Ni and Zn complexes are reported. The protonated form of the ligand bpt crystallizes as its perchlorate salt including one molecule of water, [Hbpt·H2O·ClO4]. The proton is located on one pyrazole N-atom. [Hbpt·H2O·ClO4], in which [Hbpt]+ is in cis-cis conformation, are packed in slipped stacks of approximately parallel layers. The Π -Π overlap interactions between the non-protonized pyrazoles of the adjacent layers give a zigzag arrangement of the planar aromatic [Hbpt]+ molecules. In [Ni(bpt)2](ClO4)2·H2O, bpt are meridionally three-coordinated with Ni2+. The coordination sphere around Ni2+ is a slightly distorted square bipyramid, where four pyrazole nitrogen atoms occupy the basal positions and two triazine nitrogen atoms the apical one. In [Zn(mpt)2(dmp)](ClO4)2, the Zn atom is coordinated with a pair of bidentate mpt ligands and one monodentate dmp ligand, forming a distorted trigonal bipyramid, where the two triazine nitrogen atoms of mpt and one nitrogen atom of dmp occupy the basal positions, and the two pyrazole nitrogen atoms of mpt the apical one.展开更多
文摘The trinuclear nickel? complex Ni3(C11H11N2O3)2(C5H5N)4 was prepared by the reaction of Ni(OAc)2· 4H2O with N butylsalicylhydrazide Schiff base ligand and characterized by X ray crystallography. The crystal belongs to triclinic, Mr=930.91, space group with cell parameters a=9.8489(2)? , b=12.3110(2)? , c=18.4035(3)? , α =71.353(2)° , β =76.638(2)° ,γ =84.815(2)° ,V=2056.72(6)? 3,Z=2,Dc=1.503g· cm- 3, μ (MoKα ) =1.417mm- 1, F(000)=964, R=0.0317, wR=0.0868. A total of 5393 independent reflections were collected, of which 4448 reflections with I ≥ 2σ (I) were observed. There are two centrosymmetrical trinuclear molecules in a unit cell, each molecule exhibits a linear trinuclear metal arrangement with the Ni... Ni... Ni angle of 180° . The interatomic distances between the nickel atoms on the two sides are 9.2030(8)? and 9.1876(9)? for the two molecules, respectively. The central nickel atom adopts an axially elongated octahedral geometry whereas the nickel atoms on the two sides have square planar coordination environment. CCDC: 194083.
基金Supported by the National Natural Science Foundation of China(21376059)the Key Discipline of Hefei University(2014xk01)
文摘A series of novel silica-based hybrid adsorbents were prepared by the crosslinking reaction of N-[3- （trimethoxysilyl）propyl] ethylene diamine （TMSPEDA） with epichlorohydrin （ECH） via a sol-gel process. Fourier transform infrared （FTIR） spectra confirmed that the reaction occurred. TGA curves showed that the thermal stability of these hybrid adsorbents reached as high as 180 ℃. As a typical example, the adsorption performance of nickel（U） ions onto an adsorbent （the volume ratio of TMSPEDA and ECH was 4：1 ） was explored. It was found that the adsorption of nickel（Ⅱ） ions onto this adsorbent followed the Lagergren pseudo-second-order kinetic model. The investigation of the adsorption mechanism demonstrated that nickel（Ⅱ） adsorption was chiefly controlled by diffusion-chemisorption, suggesting that more diffusion processes were involved in the adsorption of nickel（Ⅱ） ions onto this type of adsorbents. Desorption experiment indicates that these hybrid adsorbents can be regenerated. These findings reveal that this type of silica-based hybrid adsorbent is promising in the separation and recovery of nickel（Ⅱ） ions from Ni-containing wastewater or contaminated water.
基金the National Natural Science Foundation of China (Grant No. 29671034) and Natural Science Foundation of Guangdong Province (Grant Nos. 990128,974174).
文摘2,4-Bis(3,5-dimethylpyrazol-1-yl)-6-methoxyl-1,3,5-triazine(bpt) has been synthesized by using a new, simple and general method with high yields. Reactions of bpt with Ni(ClO4)2·6H2O and Zn(ClO4)2·6H2O in methanol gave mononuclear complex [Ni(bpt)2]· (ClO4)2·H2O and ternary complex [Zn(mpt)2(dmp)](ClO4)2 respectively, where mpt (2,4-dimethoxy-6-(3,5-dimethyl- pyrazol-1-yl)-1,3,5-triazine) and dmp(3,5-dimethylpyrazole) are the alcoholysis products of bpt in the presence of Zn2+ ion. A possible mechanism for this catalytic reaction was proposed. X-ray crystal structure for ligand bpt, Ni and Zn complexes are reported. The protonated form of the ligand bpt crystallizes as its perchlorate salt including one molecule of water, [Hbpt·H2O·ClO4]. The proton is located on one pyrazole N-atom. [Hbpt·H2O·ClO4], in which [Hbpt]+ is in cis-cis conformation, are packed in slipped stacks of approximately parallel layers. The Π -Π overlap interactions between the non-protonized pyrazoles of the adjacent layers give a zigzag arrangement of the planar aromatic [Hbpt]+ molecules. In [Ni(bpt)2](ClO4)2·H2O, bpt are meridionally three-coordinated with Ni2+. The coordination sphere around Ni2+ is a slightly distorted square bipyramid, where four pyrazole nitrogen atoms occupy the basal positions and two triazine nitrogen atoms the apical one. In [Zn(mpt)2(dmp)](ClO4)2, the Zn atom is coordinated with a pair of bidentate mpt ligands and one monodentate dmp ligand, forming a distorted trigonal bipyramid, where the two triazine nitrogen atoms of mpt and one nitrogen atom of dmp occupy the basal positions, and the two pyrazole nitrogen atoms of mpt the apical one.
