A novel anionic organotin(Ⅳ) complex {[(pClCHCH)Sn(HO)(Cl)OCOCH(O)CH(O)COSn(HO)(Cl)(p-ClCHCH)]·2(HNEt)}(1) was synthesized by the reaction of di(p-chlorobenzy)tin dichloride with the D-tartaric acid in 2:1 molar...A novel anionic organotin(Ⅳ) complex {[(pClCHCH)Sn(HO)(Cl)OCOCH(O)CH(O)COSn(HO)(Cl)(p-ClCHCH)]·2(HNEt)}(1) was synthesized by the reaction of di(p-chlorobenzy)tin dichloride with the D-tartaric acid in 2:1 molar in the presence of an organic base triethylamine. The structure was characterized by elemental analysis, IR, TG, XRD and single-crystal X-ray diffraction. It crystallizes in triclinic, P1 space group, with a = 0.7067(1), b = 1.9762(3), c = 2.2383(3) nm, α = 91.544(2)°, β = 90.075(2)°, γ = 90.110(2)°, V = 3.1247(7) nm~3, Z = 3, Dc = 1.621 g/cm~3, m(Mo Kα) = 16.29 cm–1, F(000) = 1530, R = 0.0394, wR = 0.1092,(Δρ)max = 1224 and(Δρ)min = –840 e/nm~3. The stabilities, orbital energies and composition characteristics of some frontier molecular orbitals of 1 have been carefully investigated with quantum chemistry calculation. In addition, the in vitro antitumor activity suggested that 1 had stronger inhibitory activity on H460, MCF7 than on A549.展开更多
Four new five-coordinated anionic tin(Ⅳ) complexes with a form of [R_ n NH_ 4- n ][PhSn( μ 2-SCH_2COO)_2] were synthesized via the reaction of mercaptoacetic acid with phenyltin trichloride in the presence of dif...Four new five-coordinated anionic tin(Ⅳ) complexes with a form of [R_ n NH_ 4- n ][PhSn( μ 2-SCH_2COO)_2] were synthesized via the reaction of mercaptoacetic acid with phenyltin trichloride in the presence of different organic bases and characterized by means of IR, 1H NMR and MS spectroscopies. The crystal structure of [( i -Pr)_2NH_2] [PhSn( μ 2-SCH_2COO)_2] was determined by X-ray diffraction. In the crystal structure,the tin atom is five-coordinated and exists in trigonal bipyramid geometry with cell parameters a =1.1766(11) nm, b =1.3144(14) nm, c =1.3336(15) nm,β =90° and Z =4.展开更多
Hafnium（Ⅳ） bis（perfluorooctanesulfonyl）imide complex is found to be an efficient catalyst for the multicomponent condensation ofβ-naphthol,aromatic aldehydes and urea or amides in perfluorodecalin to afford the ...Hafnium（Ⅳ） bis（perfluorooctanesulfonyl）imide complex is found to be an efficient catalyst for the multicomponent condensation ofβ-naphthol,aromatic aldehydes and urea or amides in perfluorodecalin to afford the corresponding substituted amidomethyl naphthols in good yields.The remarkable features of this new procedure are high yields,shorter reaction times, reusability of catalyst and simple work-up procedures.展开更多
A new isopolyoxovanadate [Ni(1,10′-phen) 3] 2 [V Ⅳ 2V Ⅴ 8O 26] was hydrothermally synthesized and structurally characterized by the single crystal X-ray diffraction. The compound crystallizes in orthorhombic system...A new isopolyoxovanadate [Ni(1,10′-phen) 3] 2 [V Ⅳ 2V Ⅴ 8O 26] was hydrothermally synthesized and structurally characterized by the single crystal X-ray diffraction. The compound crystallizes in orthorhombic system, space group Pbcn with a=1.362 9(3) nm, b=2.215 6(4) nm, c= 2.571 2(4) nm, V=7.764(2) nm 3, Z=4, R=0.040 3, wR 2=0.044 6. The compound exhibits an unusual empty ellipsoidal cage, which is constructed by eight {V ⅤO 4} tetrahedra and two {V ⅣO 5} square pyramids via corner-sharing modes. The chiral [Ni(1,10′-phen) 3] 2+ complexes act as the counter cations.展开更多
Tetra\{\[4\|carboxymethoxyphenyl\]\}porphyrin copper(Ⅱ), nickel(Ⅱ), zinc(Ⅱ) complex and their dibutyltin(Ⅳ) ester derivatives have been synthesized and characterized. The equilibrium constants of the aggregation o...Tetra\{\[4\|carboxymethoxyphenyl\]\}porphyrin copper(Ⅱ), nickel(Ⅱ), zinc(Ⅱ) complex and their dibutyltin(Ⅳ) ester derivatives have been synthesized and characterized. The equilibrium constants of the aggregation of the metal porphyrin and the equilibrium constant of the π\|π coordination with phenothoroline have been measured by using UV\|Vis titration method. The results show that the equilibrium constants decrease in the order of K \-\{CuP\}> K \-\{NiP\}> K \-\{ZnP\}. The vitro anti\|tumor activities of the dibutyltin(Ⅳ) metal porphyrinate has some relation with the ability of aggregation and coordination with ligand of the metal porphyrin.展开更多
A new complex [Ni（en）3]4[HVⅣ12VⅤ6O42（PO4）] has been hydrothermally synthesize d and characterized by X-Ray diffraction,IR and Elemental analysis.Single crystal X-ray analysis indicates that this compoud cry stal...A new complex [Ni（en）3]4[HVⅣ12VⅤ6O42（PO4）] has been hydrothermally synthesize d and characterized by X-Ray diffraction,IR and Elemental analysis.Single crystal X-ray analysis indicates that this compoud cry stallizes in cubic system,space group Im3m with a=17.4081（2）*!,V=5275.38（10）*! 3 ,R=0.0420,w R=0.1055,Z =2,D c =1.663g·cm -3 ,μ=2.297mm -1 ,F（000）=2636.The crystal structure consis ts of[Ni （en） 3 ] 2+ cations and{HV 18 O 42 （PO 4 ）} 8- cluster anion which construct from 18{VO 5 }.square pyramids.The VO 5 pyramids joined each other to form a {V 18 O 42 }cage hosting a tetrahedral{PO 4 } 3- moiety with disordered oxygen atoms .CCDC:185574.展开更多
A convenient and efficient method for the preparation of α-substituted β-amino acids has been developed by reacting compound 2 with various boric acid/borate 3 through Suzuki coupling reaction,which gave multiple st...A convenient and efficient method for the preparation of α-substituted β-amino acids has been developed by reacting compound 2 with various boric acid/borate 3 through Suzuki coupling reaction,which gave multiple structure types of substituted Ni（II） complexes 4 in high yields.Hydrogenation and hydrolysis of complexes 4 led to the corresponding α-substituted β-amino acids.展开更多
The title nickel complex I and cobalt complex II were obtained separately from the direct reaction of D-（＋）-leucinol with Ni（II） chloride and L-（-）-leucinol with Co（II） acetate tetra- hydrate in anhydrous met...The title nickel complex I and cobalt complex II were obtained separately from the direct reaction of D-（＋）-leucinol with Ni（II） chloride and L-（-）-leucinol with Co（II） acetate tetra- hydrate in anhydrous methanol. The crystal structures of I and II were determined by single-crystal X-ray diffraction and further characterized by elemental analysis and IR. For I： [Ni（C18H45N3O3）]Cl2, orthorhombic, P212121, a = 11.2807（9）, b = 14.7115（11）, c = 16.3580（13） A, V = 2714.7（4） A3, Z = 4, Pcalcd = 1.177 Mg/m3, the final R = 0.0407, and 16539 reflections observed with I 〉 2σ（/）; For II： [Co（C45HI08N6015）], trigonal, R3：H, a = 23.981（3）, b =23.981（3）, c = 10.8925（15） A, γ = 120°, V = 5425.1（14） A3, Z = 3, Pcalcd = 1.002 Mg/m3, the final R = 0.0625 for 16556 observed reflections with I 〉 2σ（I）. The complexes were then used to catalyze the Henry reaction and obtained good catalytic results. The catalytic activity of the complexes was determined by IH NMR. And research is going towards the application to other organic reactions such as cyanosilylation reaction.展开更多
Two complexes[Ni(L)(OAc)](1)and[Co(L)2]Cl·4CH3OH(2)(HL=2-aceto-3-methylpyrazine N-(4-fluorophenyl)thiosemicarbazone)have been synthesized and structurally determined by single-crystal X-ray diffraction,elemental ...Two complexes[Ni(L)(OAc)](1)and[Co(L)2]Cl·4CH3OH(2)(HL=2-aceto-3-methylpyrazine N-(4-fluorophenyl)thiosemicarbazone)have been synthesized and structurally determined by single-crystal X-ray diffraction,elemental analysis and IR spectroscopy.X-ray diffraction analysis results show that the Ni(Ⅱ)ion in complex 1 with a distorted square planar geometry is surrounded by one anionic TSC ligand with NNS donor set and one monodentate acetate.By contrast,Co(Ⅲ)ion coordinates with two tridentate TSC ligands,and thus possessing a distorted octahedron coordination geometry.Moreover,the fluorescence spectra indicate that the interactions of complexes 1 and 2 with DNA are stronger than that of the ligand HL.CCDC:1848437,1;1848438,2.展开更多
The title complex Ni(C4H5NO4)(C7H6N2)31.75(H2O) (C25H26.5N7NiO5.75, Mr = 575.74) has been prepared and its crystal structure was determined by X-ray diffraction method. The crystal of this chiral complex belongs to mo...The title complex Ni(C4H5NO4)(C7H6N2)31.75(H2O) (C25H26.5N7NiO5.75, Mr = 575.74) has been prepared and its crystal structure was determined by X-ray diffraction method. The crystal of this chiral complex belongs to monoclinic, space group P21 with a = 13.208(1), b = 10.741(1), c = 19.398(1) ? b = 104.39(1)o, V = 2665.8(4) 3, Z = 4, Dc = 1.435 g/cm3, m(MoKa) = 0.780 mm-1 and F(000) = 1198. The final R = 0.0504 and wR = 0.1267 for 9159 observed reflections (I > 2s(I)), and R = 0.065 and wR = 0.1299 for 11006 independent reflections. The complex assumes a distorted octa- hedral coordinate geometry formed by one aspartate dianion and three benzimidazole ligands. The aspartate chelates to the Ni atom as a tridentate ligand. The lattice water molecules are hydrogen- bonded to the Ni complex molecule.展开更多
A Ni（Ⅱ） supramolecular complex,[Ni 2 （btec）（3py） 2 （H 2 O） 8 ]（H 2 O） 4 （1）,has been synthesized by Ni（ClO 4） 2 ·6H 2 O,benzene-1,2,4,5-tetracarboxylic acid （H 4 btec） and terminal ligand 3-hydro...A Ni（Ⅱ） supramolecular complex,[Ni 2 （btec）（3py） 2 （H 2 O） 8 ]（H 2 O） 4 （1）,has been synthesized by Ni（ClO 4） 2 ·6H 2 O,benzene-1,2,4,5-tetracarboxylic acid （H 4 btec） and terminal ligand 3-hydroxypyridine （3py） in aqueous solution.The title compound crystallizes in triclinic system,space group P1,with a=8.5637（12）,b=9.4138（13）,c=10.3611（14）,α=67.9540（10）,β=85.1740（10）,γ=76.9890（10）°,V=754.33（18） 3,Z=2,M r=386.96,D c=1.704 Mg/m 3,μ=1.345 mm-1,F（000）=402,the final R=0.0222 and wR=0.0563 for 2675 observed reflections with I 2σ（Ⅰ）.The adjacent discrete molecules are further self-assembled by intermolecular π-π and O-H···O hydrogen bonding interactions to construct a 3D supramolecular framework.Magnetic measurement shows weak ferromagnetic interaction in the range of 2～300 K.展开更多
A new binuclear complex [Ni2（2,2＇-bpy）2（C8H3NO6）2（H2O）4] 1 （2,2＇-bpy = 2,2＇- bipyridine, C8H3NO6 = 4-nitrophthalate） has been synthesized by a hydrothermal reaction and characterized by X-ray single-crystal...A new binuclear complex [Ni2（2,2＇-bpy）2（C8H3NO6）2（H2O）4] 1 （2,2＇-bpy = 2,2＇- bipyridine, C8H3NO6 = 4-nitrophthalate） has been synthesized by a hydrothermal reaction and characterized by X-ray single-crystal diffraction analysis. The complex crystallizes in triclinic, space group P1 with a = 7.206（2）, b = 10.337（4）, c = 12.480（4） , α = 89.887（11）, β = 77.033（9）, γ = 78.349（6）o, V = 886.3（5） 3, Z = 1, C36H30Ni2N6O16, Mr = 920.08, Dc = 1.724 g cm-3, F（000） = 472, μ = 1.152 mm-1, the final R = 0.0458 and wR = 0.1163 for 3372 observed reflections with I 2σ（Ⅰ）. The two Ni（Ⅱ） ions are bridged by two 4-nitrophthalates both in a bis-monodentate mode. Magnetic measurements reveal that the intramolecular exchange couplings in the dimer are ferromagnetic with 2J/k = 2.32 K, D =-1.44 K and g = 2.18.展开更多
Two new Ni（ Ⅱ） coordination polymers, {[Ni（tbip）（bipy）（H2O）]-0.5H2O}n 1 and [Ni（tbip）（phen）（H2O）]n 2 （Hatbip = 5-tert-butyl isophthalic acid, bipy = 2,2＇-bipyridine, phen = 1,10-phenanthroline）, have...Two new Ni（ Ⅱ） coordination polymers, {[Ni（tbip）（bipy）（H2O）]-0.5H2O}n 1 and [Ni（tbip）（phen）（H2O）]n 2 （Hatbip = 5-tert-butyl isophthalic acid, bipy = 2,2＇-bipyridine, phen = 1,10-phenanthroline）, have been synthesized under hydrothermal conditions and characterized by elemental analysis, X-ray diffraction, and IR spectroscopy. In the two polymers, H2tbip acts as a tridentate ligand. Compound 1 has a tbip bridged 1-D linear chain which is extended by hydrogen bonds into a 1-D double chain, while compound 2 exhibits a 1-D zigzag chain.展开更多
A new kind of Schiff base HL（HL= 1-phenyl-3-methyl-4-（p-methylbenzoyl）-5-pyrazolone with L-Leucine methyl ester） and complexes Ni L′_2·0.75C_2H_5OH·0.25H_2O,Cu L′′2（L′ = 1-phenyl-3-methyl-4-（p-meth...A new kind of Schiff base HL（HL= 1-phenyl-3-methyl-4-（p-methylbenzoyl）-5-pyrazolone with L-Leucine methyl ester） and complexes Ni L′_2·0.75C_2H_5OH·0.25H_2O,Cu L′′2（L′ = 1-phenyl-3-methyl-4-（p-methylbenzoyl）-5-pyrazolone with L-leucine ethyl,L′′ = 1-phenyl-3-methyl-4-（p-methylbenzoyl）-5-pyrazolone with L-leucine） have been synthesized and structurally determined by X-ray diffraction. For HL： crystal structure determination indicates that there are two independent HLs with different conformations in one asymmetric unit. For complex 1： the Ni（Ⅱ） ion is six-coordinated by two carbonyl oxygen atoms from pyrazolone ring,two nitrogen atoms from different HL′ and two oxygen atoms from L-Leucine ethyl ester to form a distorted octahedral geometry. For complex 2： the Cu（Ⅱ） ion is four-coordinated by one carbonyl oxygen atom from the pyrazolone ring,one nitrogen atom from HL′′,and two different carboxylic oxygen atoms from L-leucine with the same conformation to form a distorted quadrilateral geometry.展开更多
基金Supported by the Open Fund Project innovation platform of Key Laboratory of Higher Educational Institutions of Hunan Province(GN16K01)Scientific&Technological Projects of Hengyang(2016KL03)+1 种基金Aid programs for Science and Technology Innovative Research Team in Higher Educational Institutions of Hunan Provincethe Key Discipline of Hunan Province,Project funding for research and innovation experiment of university students in Hunan Province
文摘A novel anionic organotin(Ⅳ) complex {[(pClCHCH)Sn(HO)(Cl)OCOCH(O)CH(O)COSn(HO)(Cl)(p-ClCHCH)]·2(HNEt)}(1) was synthesized by the reaction of di(p-chlorobenzy)tin dichloride with the D-tartaric acid in 2:1 molar in the presence of an organic base triethylamine. The structure was characterized by elemental analysis, IR, TG, XRD and single-crystal X-ray diffraction. It crystallizes in triclinic, P1 space group, with a = 0.7067(1), b = 1.9762(3), c = 2.2383(3) nm, α = 91.544(2)°, β = 90.075(2)°, γ = 90.110(2)°, V = 3.1247(7) nm~3, Z = 3, Dc = 1.621 g/cm~3, m(Mo Kα) = 16.29 cm–1, F(000) = 1530, R = 0.0394, wR = 0.1092,(Δρ)max = 1224 and(Δρ)min = –840 e/nm~3. The stabilities, orbital energies and composition characteristics of some frontier molecular orbitals of 1 have been carefully investigated with quantum chemistry calculation. In addition, the in vitro antitumor activity suggested that 1 had stronger inhibitory activity on H460, MCF7 than on A549.
文摘Four new five-coordinated anionic tin(Ⅳ) complexes with a form of [R_ n NH_ 4- n ][PhSn( μ 2-SCH_2COO)_2] were synthesized via the reaction of mercaptoacetic acid with phenyltin trichloride in the presence of different organic bases and characterized by means of IR, 1H NMR and MS spectroscopies. The crystal structure of [( i -Pr)_2NH_2] [PhSn( μ 2-SCH_2COO)_2] was determined by X-ray diffraction. In the crystal structure,the tin atom is five-coordinated and exists in trigonal bipyramid geometry with cell parameters a =1.1766(11) nm, b =1.3144(14) nm, c =1.3336(15) nm,β =90° and Z =4.
基金the project of"Excellence Initiative"and"Zijin Star"in NJUST for financial support
文摘Hafnium（Ⅳ） bis（perfluorooctanesulfonyl）imide complex is found to be an efficient catalyst for the multicomponent condensation ofβ-naphthol,aromatic aldehydes and urea or amides in perfluorodecalin to afford the corresponding substituted amidomethyl naphthols in good yields.The remarkable features of this new procedure are high yields,shorter reaction times, reusability of catalyst and simple work-up procedures.
文摘A new isopolyoxovanadate [Ni(1,10′-phen) 3] 2 [V Ⅳ 2V Ⅴ 8O 26] was hydrothermally synthesized and structurally characterized by the single crystal X-ray diffraction. The compound crystallizes in orthorhombic system, space group Pbcn with a=1.362 9(3) nm, b=2.215 6(4) nm, c= 2.571 2(4) nm, V=7.764(2) nm 3, Z=4, R=0.040 3, wR 2=0.044 6. The compound exhibits an unusual empty ellipsoidal cage, which is constructed by eight {V ⅤO 4} tetrahedra and two {V ⅣO 5} square pyramids via corner-sharing modes. The chiral [Ni(1,10′-phen) 3] 2+ complexes act as the counter cations.
文摘Tetra\{\[4\|carboxymethoxyphenyl\]\}porphyrin copper(Ⅱ), nickel(Ⅱ), zinc(Ⅱ) complex and their dibutyltin(Ⅳ) ester derivatives have been synthesized and characterized. The equilibrium constants of the aggregation of the metal porphyrin and the equilibrium constant of the π\|π coordination with phenothoroline have been measured by using UV\|Vis titration method. The results show that the equilibrium constants decrease in the order of K \-\{CuP\}> K \-\{NiP\}> K \-\{ZnP\}. The vitro anti\|tumor activities of the dibutyltin(Ⅳ) metal porphyrinate has some relation with the ability of aggregation and coordination with ligand of the metal porphyrin.
文摘A new complex [Ni（en）3]4[HVⅣ12VⅤ6O42（PO4）] has been hydrothermally synthesize d and characterized by X-Ray diffraction,IR and Elemental analysis.Single crystal X-ray analysis indicates that this compoud cry stallizes in cubic system,space group Im3m with a=17.4081（2）*!,V=5275.38（10）*! 3 ,R=0.0420,w R=0.1055,Z =2,D c =1.663g·cm -3 ,μ=2.297mm -1 ,F（000）=2636.The crystal structure consis ts of[Ni （en） 3 ] 2+ cations and{HV 18 O 42 （PO 4 ）} 8- cluster anion which construct from 18{VO 5 }.square pyramids.The VO 5 pyramids joined each other to form a {V 18 O 42 }cage hosting a tetrahedral{PO 4 } 3- moiety with disordered oxygen atoms .CCDC:185574.
基金National Basic Research Program of China (Grants No. 2009CB940903 and 2009CB918502)the National Natural Science Foundation of China (Grant No. 20721003 and 81025017)National S&T Major Projects (Grant No. 2012ZX09103-101-072).
文摘A convenient and efficient method for the preparation of α-substituted β-amino acids has been developed by reacting compound 2 with various boric acid/borate 3 through Suzuki coupling reaction,which gave multiple structure types of substituted Ni（II） complexes 4 in high yields.Hydrogenation and hydrolysis of complexes 4 led to the corresponding α-substituted β-amino acids.
文摘The title nickel complex I and cobalt complex II were obtained separately from the direct reaction of D-（＋）-leucinol with Ni（II） chloride and L-（-）-leucinol with Co（II） acetate tetra- hydrate in anhydrous methanol. The crystal structures of I and II were determined by single-crystal X-ray diffraction and further characterized by elemental analysis and IR. For I： [Ni（C18H45N3O3）]Cl2, orthorhombic, P212121, a = 11.2807（9）, b = 14.7115（11）, c = 16.3580（13） A, V = 2714.7（4） A3, Z = 4, Pcalcd = 1.177 Mg/m3, the final R = 0.0407, and 16539 reflections observed with I 〉 2σ（/）; For II： [Co（C45HI08N6015）], trigonal, R3：H, a = 23.981（3）, b =23.981（3）, c = 10.8925（15） A, γ = 120°, V = 5425.1（14） A3, Z = 3, Pcalcd = 1.002 Mg/m3, the final R = 0.0625 for 16556 observed reflections with I 〉 2σ（I）. The complexes were then used to catalyze the Henry reaction and obtained good catalytic results. The catalytic activity of the complexes was determined by IH NMR. And research is going towards the application to other organic reactions such as cyanosilylation reaction.
文摘Two complexes[Ni(L)(OAc)](1)and[Co(L)2]Cl·4CH3OH(2)(HL=2-aceto-3-methylpyrazine N-(4-fluorophenyl)thiosemicarbazone)have been synthesized and structurally determined by single-crystal X-ray diffraction,elemental analysis and IR spectroscopy.X-ray diffraction analysis results show that the Ni(Ⅱ)ion in complex 1 with a distorted square planar geometry is surrounded by one anionic TSC ligand with NNS donor set and one monodentate acetate.By contrast,Co(Ⅲ)ion coordinates with two tridentate TSC ligands,and thus possessing a distorted octahedron coordination geometry.Moreover,the fluorescence spectra indicate that the interactions of complexes 1 and 2 with DNA are stronger than that of the ligand HL.CCDC:1848437,1;1848438,2.
文摘The title complex Ni(C4H5NO4)(C7H6N2)31.75(H2O) (C25H26.5N7NiO5.75, Mr = 575.74) has been prepared and its crystal structure was determined by X-ray diffraction method. The crystal of this chiral complex belongs to monoclinic, space group P21 with a = 13.208(1), b = 10.741(1), c = 19.398(1) ? b = 104.39(1)o, V = 2665.8(4) 3, Z = 4, Dc = 1.435 g/cm3, m(MoKa) = 0.780 mm-1 and F(000) = 1198. The final R = 0.0504 and wR = 0.1267 for 9159 observed reflections (I > 2s(I)), and R = 0.065 and wR = 0.1299 for 11006 independent reflections. The complex assumes a distorted octa- hedral coordinate geometry formed by one aspartate dianion and three benzimidazole ligands. The aspartate chelates to the Ni atom as a tridentate ligand. The lattice water molecules are hydrogen- bonded to the Ni complex molecule.
基金supported by the Natural Science Foundation of Henan Province (Nos. 092102310075 and 0511022600)
文摘A Ni（Ⅱ） supramolecular complex,[Ni 2 （btec）（3py） 2 （H 2 O） 8 ]（H 2 O） 4 （1）,has been synthesized by Ni（ClO 4） 2 ·6H 2 O,benzene-1,2,4,5-tetracarboxylic acid （H 4 btec） and terminal ligand 3-hydroxypyridine （3py） in aqueous solution.The title compound crystallizes in triclinic system,space group P1,with a=8.5637（12）,b=9.4138（13）,c=10.3611（14）,α=67.9540（10）,β=85.1740（10）,γ=76.9890（10）°,V=754.33（18） 3,Z=2,M r=386.96,D c=1.704 Mg/m 3,μ=1.345 mm-1,F（000）=402,the final R=0.0222 and wR=0.0563 for 2675 observed reflections with I 2σ（Ⅰ）.The adjacent discrete molecules are further self-assembled by intermolecular π-π and O-H···O hydrogen bonding interactions to construct a 3D supramolecular framework.Magnetic measurement shows weak ferromagnetic interaction in the range of 2～300 K.
基金supported by the Science and Technology Foundation of Guizhou Province (No.[2008]2216)
文摘A new binuclear complex [Ni2（2,2＇-bpy）2（C8H3NO6）2（H2O）4] 1 （2,2＇-bpy = 2,2＇- bipyridine, C8H3NO6 = 4-nitrophthalate） has been synthesized by a hydrothermal reaction and characterized by X-ray single-crystal diffraction analysis. The complex crystallizes in triclinic, space group P1 with a = 7.206（2）, b = 10.337（4）, c = 12.480（4） , α = 89.887（11）, β = 77.033（9）, γ = 78.349（6）o, V = 886.3（5） 3, Z = 1, C36H30Ni2N6O16, Mr = 920.08, Dc = 1.724 g cm-3, F（000） = 472, μ = 1.152 mm-1, the final R = 0.0458 and wR = 0.1163 for 3372 observed reflections with I 2σ（Ⅰ）. The two Ni（Ⅱ） ions are bridged by two 4-nitrophthalates both in a bis-monodentate mode. Magnetic measurements reveal that the intramolecular exchange couplings in the dimer are ferromagnetic with 2J/k = 2.32 K, D =-1.44 K and g = 2.18.
基金supported by the National Natural Science Foundation of China (Nos.20771026 and 20771054)the Henan Tackle Key Problem of Science and Technology (Nos.072102270030 and 072102270034)the Foundation of Education Committee of Henan Province (2006150017 and 2008A150018)
文摘Two new Ni（ Ⅱ） coordination polymers, {[Ni（tbip）（bipy）（H2O）]-0.5H2O}n 1 and [Ni（tbip）（phen）（H2O）]n 2 （Hatbip = 5-tert-butyl isophthalic acid, bipy = 2,2＇-bipyridine, phen = 1,10-phenanthroline）, have been synthesized under hydrothermal conditions and characterized by elemental analysis, X-ray diffraction, and IR spectroscopy. In the two polymers, H2tbip acts as a tridentate ligand. Compound 1 has a tbip bridged 1-D linear chain which is extended by hydrogen bonds into a 1-D double chain, while compound 2 exhibits a 1-D zigzag chain.
文摘A new kind of Schiff base HL（HL= 1-phenyl-3-methyl-4-（p-methylbenzoyl）-5-pyrazolone with L-Leucine methyl ester） and complexes Ni L′_2·0.75C_2H_5OH·0.25H_2O,Cu L′′2（L′ = 1-phenyl-3-methyl-4-（p-methylbenzoyl）-5-pyrazolone with L-leucine ethyl,L′′ = 1-phenyl-3-methyl-4-（p-methylbenzoyl）-5-pyrazolone with L-leucine） have been synthesized and structurally determined by X-ray diffraction. For HL： crystal structure determination indicates that there are two independent HLs with different conformations in one asymmetric unit. For complex 1： the Ni（Ⅱ） ion is six-coordinated by two carbonyl oxygen atoms from pyrazolone ring,two nitrogen atoms from different HL′ and two oxygen atoms from L-Leucine ethyl ester to form a distorted octahedral geometry. For complex 2： the Cu（Ⅱ） ion is four-coordinated by one carbonyl oxygen atom from the pyrazolone ring,one nitrogen atom from HL′′,and two different carboxylic oxygen atoms from L-leucine with the same conformation to form a distorted quadrilateral geometry.
