A 1,3,5-triazin derivative: N,N’-bis-(4,6-dichloro——triazin-2-yl)-hexane-1,6-diamine was prepared from cyanuric chloride and hexane-1,6-diamine by nucleophilic substitution reaction.By trying experiments,the molar ...A 1,3,5-triazin derivative: N,N’-bis-(4,6-dichloro——triazin-2-yl)-hexane-1,6-diamine was prepared from cyanuric chloride and hexane-1,6-diamine by nucleophilic substitution reaction.By trying experiments,the molar ratio of cyanuric chloride to hexane-1,6-diamine was 2:1,using sodium hydroxide as base and the mixture of dichlormethane and water as solvent.On the basis of these results,a L9(33) orthogonal layout was designed to investigate the effects of the reaction time,the variety and dosage of base as well as the vomule ratio of dichlormethane and water on the yields of products.Three levels were selected for every factor.The result showed that when the molar ratio of sodium hydroxide to hexane-1,6-diamine was 2:1,the volume ratio of dichloromethane and water was 1:1 and the reaction was carried out at 0-5 ℃ for 6 h,the product yield could reach to 92.8%.The structure of the target product was characterized by elementary analysis,MS,1 H-NMR and FTIR.展开更多
The compound [H2（teta）]2+·2Cl-·3H2O （teta=meso-5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane）was synthesized and characterized by elementary analysis and the structure was determined by sin...The compound [H2（teta）]2+·2Cl-·3H2O （teta=meso-5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane）was synthesized and characterized by elementary analysis and the structure was determined by single-crystal X-ray diffraction.The crystal belongs to triclinic,space group Pī with a=7.8364（16）,b=8.3607（13）,c=9.4762（15）?,α=61.900（12）,β=78.970（16）,γ=80.008（16）°,V=535.06（16）?3,Z=1,ρcalc=1.277g/cm3,F（000）=226.The macrocylic tetraamine cation contains two protonated secondary amine N atoms and two secondary amine N atoms.The water molecules are distinguished by their inequality in structure formation.They are involved in different types of intermolecular hydrogen bonding in the crystal lattice.展开更多
The manganese(Ⅲ) complex [Mn (acacen) {N (CN)2}]n [H2acacen =bis (acetylacetone)ethylenediimine] has been synthesized and the structure has been determined. The complex forms a one-dimensional chain structure via the...The manganese(Ⅲ) complex [Mn (acacen) {N (CN)2}]n [H2acacen =bis (acetylacetone)ethylenediimine] has been synthesized and the structure has been determined. The complex forms a one-dimensional chain structure via the bidentate bridge ligandμ1,5-[N(CN)2]- linking [Mn(acacen)] moiety. The magnetic property of the compound (75～300 K) shows the existence of an antiferromagnetic exchange interaction among paramagnetic centers along the chain. CCDC: 244940.展开更多
The cadmium complex[Cd(PMBP)2(EtOH)2](HPMBP =1-phenyl-3-methyl-4-benzoyl-pyrazolone-5)wassynthesized and characterized by IR and thermogravimetric analysis.The structure was determined by single X-ray diffraction anal...The cadmium complex[Cd(PMBP)2(EtOH)2](HPMBP =1-phenyl-3-methyl-4-benzoyl-pyrazolone-5)wassynthesized and characterized by IR and thermogravimetric analysis.The structure was determined by single X-ray diffraction anal-ysis.The crystal belongs to triclinic system,space group P 1.The crystallographic data are:a =9.121(4),b =10.193(5),c =10.895(5),α=107.085(4),β=108.239(4),γ=104.028(2)°,V=855.0(6) 3,Z =1,F(000) =390,Mr =759.12,Dc=1.474 Mg/m3,μ=0.692 mm-1,R1=0.0312 and wR2=0.0836.In the crystal Cd(Ⅱ)ion is coordinated by four oxygen atomsfrom two PMBP ligands and two oxygen atoms from two solvent EtOHmolecules to form a distorted octahedron geometry.展开更多
The complex[Ni（teta）（NCS）2]（teta=meso-5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane）was synthesized and characterized by elementary analysis,IR and UV and the structure was determined by single-cry...The complex[Ni（teta）（NCS）2]（teta=meso-5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane）was synthesized and characterized by elementary analysis,IR and UV and the structure was determined by single-crystal X-ray diffraction analysis.The result showed the crystal belonged to triclinic,space group P（1） with a=8.0261（17）,b=9.1174（19）,c=15.485（3）（A）?,a=94.438（5）,β=97.497（6）,γ=92.948（5）o,V=1117.9（4）（A）?3,Z=2,Dcalc=1.365g/cm3,F（000）=492.In the crystal there were two independent Ni（Ⅱ）centres.Each Ni（Ⅱ）ion was coordinated by four nitrogen atoms from one teta ligand and two nitrogen atoms from NCS-anions to form a distorted octahedron geometry.展开更多
A silver(Ⅰ) complex has been obtained from reaction of silver salt and 4-Hpytz(4-Hpytz=3,5-di(4-pyridyl)-1,2,4-triazole) by hydrothermal method.Single crystal structure reveals that it consists of a 2D coordination p...A silver(Ⅰ) complex has been obtained from reaction of silver salt and 4-Hpytz(4-Hpytz=3,5-di(4-pyridyl)-1,2,4-triazole) by hydrothermal method.Single crystal structure reveals that it consists of a 2D coordination polymer [Ag(4-pytz)]∞(1)(4-pytz=3,5-di(4-pyridyl)-1,2,4-triazolate),which was crystallized in monoclinic crystal system and space group of P21/c,with a=0.753 64(1) nm,b=1.135 55(2) nm,c=1.291 7(2) nm,β=104.015(4)°,V=1.072 5(3) nm3,Z=4.Each Ag(Ⅰ) ion has a trigonal coordination geometry which three N atoms from two bridging pytz ligands.4-pytz shows-1 valence which lost its proton located at a triazole ring in final product.The title complex exhibits high thermal stability and decomposed at 472 ℃.Furthermore,complex 1 shows obvious luminescence with λem at 547 nm,which is ascribed to MLCT.展开更多
Two bis（guanidinate）titaium complexes were synthesized by the metathesis reaction of TiCl4（THF）2with 2equivalent of lithium guanidinate,which formed in situ by the reaction of carbodiimide and lithium amide.These ...Two bis（guanidinate）titaium complexes were synthesized by the metathesis reaction of TiCl4（THF）2with 2equivalent of lithium guanidinate,which formed in situ by the reaction of carbodiimide and lithium amide.These complexes were well characterized by （）1H NMR,elemental analysis and IR spectroscopy.Their catalytic activity was also studied under the presence of MMAO.展开更多
The uranyl complex [UO2（PMBP）2（DMDBU）]（HPMBP=1-phenyl-3-methy1-4-benzoyl-pyrazolone-5,DMDBU=N,N′-dimethyl-N,N′-dibenzenyl-urea）was synthesized and characterized.The structure was determined by single X-ray dif...The uranyl complex [UO2（PMBP）2（DMDBU）]（HPMBP=1-phenyl-3-methy1-4-benzoyl-pyrazolone-5,DMDBU=N,N′-dimethyl-N,N′-dibenzenyl-urea）was synthesized and characterized.The structure was determined by single X-ray diffraction analysis.The crystal belongs to triclinic system,space group P（1）-.The crystallographic data are:a=9.5947（10）,b=12.0531（11）,c=20.002（2）,α=77.167（7）,β=80.090（8）,γ=75.870（7）°,V=2170.1（4）3,Z=2,F（000）=1052,Mr=164.92,Dc=1.630 Mg/m3,μ=3.800mm-1,R1=0.0409,wR2=0.0770.In the crystal,the uranyl ion is coordinated by four oxygen atoms from two PMBP ligands and one oxygen atoms from one DMDBU to form a distorted pentagonal-bipyramid geometry.展开更多
A homoleptic lanthanide guanidinate complex [（CH2）5NC（NiPr）2]3Yb was synthesized by the metathesis reaction of lithium guanidinate with anhydrous YbCl3 in 3∶1 molar ratio in THF.Its crystal structure was determin...A homoleptic lanthanide guanidinate complex [（CH2）5NC（NiPr）2]3Yb was synthesized by the metathesis reaction of lithium guanidinate with anhydrous YbCl3 in 3∶1 molar ratio in THF.Its crystal structure was determined by X-ray diffraction.The crystallographic data:C36H72N9Yb,Mr=804.07,orthorhombic,space group P212121（#19）,a=10.3168（7）,b=11.443（7）,c=35.5649（2）?,V=4199.1（5）?3,Z=4,Dc=1.272 g/cm3,F（000）=1684.00,T=193.1K,λ（MoKα）=0.7107?,μ=22.61 cm-1,R=0.040,wR=0.126 for 8653 observed reflections with（I>3.00 σ（I））.The ytterbium is six-coordinate by six nitrogen atoms of three chelation bidentate guanidinate ligands.展开更多
Reaction of a preformed cluster [｛(η5-C5Me5)WS3｝3Cu7(MeCN)9](PF6)4 (1) in MeCN with LiCl and PPh3 gave rise to a tetranuclear cationic cluster [(η5-C5Me5)WS3｛Cu(PPh3)｝3Cl](PF6) (2). The title compound 2 was char...Reaction of a preformed cluster [｛(η5-C5Me5)WS3｝3Cu7(MeCN)9](PF6)4 (1) in MeCN with LiCl and PPh3 gave rise to a tetranuclear cationic cluster [(η5-C5Me5)WS3｛Cu(PPh3)｝3Cl](PF6) (2). The title compound 2 was char- acterized by elementary analysis, IR, UV-Vis, 1H NMR, and its crystal structure was determined by X-ray single crystal diffraction. It belongs to monoclinic, space group P21/c with a=1.7998(4) nm, b=2.0836(4) nm, c=1.9135(4) nm, β=113.63(3)°, V=6.574(3) nm3, Z=4. The cluster cation [(η5-C5Me5)WS3｛Cu(PPh3)｝3Cl]+ of 2 contains a strongly distorted, cubane-like structure [WS3Cu3Cl] in which one Cl weakly fills into the void of the nido-like [WS3Cu3] fragment with three relatively long Cu-Cl distances. CCDC: 270415.展开更多
文摘A 1,3,5-triazin derivative: N,N’-bis-(4,6-dichloro——triazin-2-yl)-hexane-1,6-diamine was prepared from cyanuric chloride and hexane-1,6-diamine by nucleophilic substitution reaction.By trying experiments,the molar ratio of cyanuric chloride to hexane-1,6-diamine was 2:1,using sodium hydroxide as base and the mixture of dichlormethane and water as solvent.On the basis of these results,a L9(33) orthogonal layout was designed to investigate the effects of the reaction time,the variety and dosage of base as well as the vomule ratio of dichlormethane and water on the yields of products.Three levels were selected for every factor.The result showed that when the molar ratio of sodium hydroxide to hexane-1,6-diamine was 2:1,the volume ratio of dichloromethane and water was 1:1 and the reaction was carried out at 0-5 ℃ for 6 h,the product yield could reach to 92.8%.The structure of the target product was characterized by elementary analysis,MS,1 H-NMR and FTIR.
文摘The compound [H2（teta）]2+·2Cl-·3H2O （teta=meso-5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane）was synthesized and characterized by elementary analysis and the structure was determined by single-crystal X-ray diffraction.The crystal belongs to triclinic,space group Pī with a=7.8364（16）,b=8.3607（13）,c=9.4762（15）?,α=61.900（12）,β=78.970（16）,γ=80.008（16）°,V=535.06（16）?3,Z=1,ρcalc=1.277g/cm3,F（000）=226.The macrocylic tetraamine cation contains two protonated secondary amine N atoms and two secondary amine N atoms.The water molecules are distinguished by their inequality in structure formation.They are involved in different types of intermolecular hydrogen bonding in the crystal lattice.
文摘The manganese(Ⅲ) complex [Mn (acacen) {N (CN)2}]n [H2acacen =bis (acetylacetone)ethylenediimine] has been synthesized and the structure has been determined. The complex forms a one-dimensional chain structure via the bidentate bridge ligandμ1,5-[N(CN)2]- linking [Mn(acacen)] moiety. The magnetic property of the compound (75～300 K) shows the existence of an antiferromagnetic exchange interaction among paramagnetic centers along the chain. CCDC: 244940.
文摘The cadmium complex[Cd(PMBP)2(EtOH)2](HPMBP =1-phenyl-3-methyl-4-benzoyl-pyrazolone-5)wassynthesized and characterized by IR and thermogravimetric analysis.The structure was determined by single X-ray diffraction anal-ysis.The crystal belongs to triclinic system,space group P 1.The crystallographic data are:a =9.121(4),b =10.193(5),c =10.895(5),α=107.085(4),β=108.239(4),γ=104.028(2)°,V=855.0(6) 3,Z =1,F(000) =390,Mr =759.12,Dc=1.474 Mg/m3,μ=0.692 mm-1,R1=0.0312 and wR2=0.0836.In the crystal Cd(Ⅱ)ion is coordinated by four oxygen atomsfrom two PMBP ligands and two oxygen atoms from two solvent EtOHmolecules to form a distorted octahedron geometry.
文摘The complex[Ni（teta）（NCS）2]（teta=meso-5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane）was synthesized and characterized by elementary analysis,IR and UV and the structure was determined by single-crystal X-ray diffraction analysis.The result showed the crystal belonged to triclinic,space group P（1） with a=8.0261（17）,b=9.1174（19）,c=15.485（3）（A）?,a=94.438（5）,β=97.497（6）,γ=92.948（5）o,V=1117.9（4）（A）?3,Z=2,Dcalc=1.365g/cm3,F（000）=492.In the crystal there were two independent Ni（Ⅱ）centres.Each Ni（Ⅱ）ion was coordinated by four nitrogen atoms from one teta ligand and two nitrogen atoms from NCS-anions to form a distorted octahedron geometry.
文摘A silver(Ⅰ) complex has been obtained from reaction of silver salt and 4-Hpytz(4-Hpytz=3,5-di(4-pyridyl)-1,2,4-triazole) by hydrothermal method.Single crystal structure reveals that it consists of a 2D coordination polymer [Ag(4-pytz)]∞(1)(4-pytz=3,5-di(4-pyridyl)-1,2,4-triazolate),which was crystallized in monoclinic crystal system and space group of P21/c,with a=0.753 64(1) nm,b=1.135 55(2) nm,c=1.291 7(2) nm,β=104.015(4)°,V=1.072 5(3) nm3,Z=4.Each Ag(Ⅰ) ion has a trigonal coordination geometry which three N atoms from two bridging pytz ligands.4-pytz shows-1 valence which lost its proton located at a triazole ring in final product.The title complex exhibits high thermal stability and decomposed at 472 ℃.Furthermore,complex 1 shows obvious luminescence with λem at 547 nm,which is ascribed to MLCT.
文摘Two bis（guanidinate）titaium complexes were synthesized by the metathesis reaction of TiCl4（THF）2with 2equivalent of lithium guanidinate,which formed in situ by the reaction of carbodiimide and lithium amide.These complexes were well characterized by （）1H NMR,elemental analysis and IR spectroscopy.Their catalytic activity was also studied under the presence of MMAO.
文摘The uranyl complex [UO2（PMBP）2（DMDBU）]（HPMBP=1-phenyl-3-methy1-4-benzoyl-pyrazolone-5,DMDBU=N,N′-dimethyl-N,N′-dibenzenyl-urea）was synthesized and characterized.The structure was determined by single X-ray diffraction analysis.The crystal belongs to triclinic system,space group P（1）-.The crystallographic data are:a=9.5947（10）,b=12.0531（11）,c=20.002（2）,α=77.167（7）,β=80.090（8）,γ=75.870（7）°,V=2170.1（4）3,Z=2,F（000）=1052,Mr=164.92,Dc=1.630 Mg/m3,μ=3.800mm-1,R1=0.0409,wR2=0.0770.In the crystal,the uranyl ion is coordinated by four oxygen atoms from two PMBP ligands and one oxygen atoms from one DMDBU to form a distorted pentagonal-bipyramid geometry.
文摘A homoleptic lanthanide guanidinate complex [（CH2）5NC（NiPr）2]3Yb was synthesized by the metathesis reaction of lithium guanidinate with anhydrous YbCl3 in 3∶1 molar ratio in THF.Its crystal structure was determined by X-ray diffraction.The crystallographic data:C36H72N9Yb,Mr=804.07,orthorhombic,space group P212121（#19）,a=10.3168（7）,b=11.443（7）,c=35.5649（2）?,V=4199.1（5）?3,Z=4,Dc=1.272 g/cm3,F（000）=1684.00,T=193.1K,λ（MoKα）=0.7107?,μ=22.61 cm-1,R=0.040,wR=0.126 for 8653 observed reflections with（I>3.00 σ（I））.The ytterbium is six-coordinate by six nitrogen atoms of three chelation bidentate guanidinate ligands.
文摘Reaction of a preformed cluster [｛(η5-C5Me5)WS3｝3Cu7(MeCN)9](PF6)4 (1) in MeCN with LiCl and PPh3 gave rise to a tetranuclear cationic cluster [(η5-C5Me5)WS3｛Cu(PPh3)｝3Cl](PF6) (2). The title compound 2 was char- acterized by elementary analysis, IR, UV-Vis, 1H NMR, and its crystal structure was determined by X-ray single crystal diffraction. It belongs to monoclinic, space group P21/c with a=1.7998(4) nm, b=2.0836(4) nm, c=1.9135(4) nm, β=113.63(3)°, V=6.574(3) nm3, Z=4. The cluster cation [(η5-C5Me5)WS3｛Cu(PPh3)｝3Cl]+ of 2 contains a strongly distorted, cubane-like structure [WS3Cu3Cl] in which one Cl weakly fills into the void of the nido-like [WS3Cu3] fragment with three relatively long Cu-Cl distances. CCDC: 270415.
