A new compound [Cu（AFO）2（N3）2]（DMF）（H2O）（AFO=4,5-diazafluorene-9-one）was synthesized.Its structure was determined by single X-ray diffraction.The crystal belongs to monoclinic system,space group C2/c.The cry...A new compound [Cu（AFO）2（N3）2]（DMF）（H2O）（AFO=4,5-diazafluorene-9-one）was synthesized.Its structure was determined by single X-ray diffraction.The crystal belongs to monoclinic system,space group C2/c.The crystallographic data,were determined a=1.2609（2）nm,b=0.8000（1）nm,c=2.6220（4）nm,β=109.964（6）°,V=2.4859（6）nm3,Z=4,F（000）=1236,Mr=603.07,Dc=1.611 Mg/m3,μ=0.937 nm-1,R1=0.0561,and wR2=0.1290.In the crystal Cu（II） atom is coordinated with four nitrogen from two AFO ligands and two nitrogen atoms from two azide ions to form an elonged-octahedron geometry.展开更多
The title complex, [Cu(L)Cl2]n (L = 2,5-di-2-pyridyl-1,3,4-oxodiazole) 1, has been obtained from the reaction of 3,6-di-2-pyridyl-1,2,4,5-tetrazine (bptz) and CuCl2?H2O in a mixture solvent of CH3CN and CH2Cl2 (L is g...The title complex, [Cu(L)Cl2]n (L = 2,5-di-2-pyridyl-1,3,4-oxodiazole) 1, has been obtained from the reaction of 3,6-di-2-pyridyl-1,2,4,5-tetrazine (bptz) and CuCl2?H2O in a mixture solvent of CH3CN and CH2Cl2 (L is generated from the metal-assisted hydrolysis reaction of bptz) and structurally characterized. It crystallizes in space group C2/c of monoclinic system with cell parameters: a = 9.812(2), b = 12.679(3), c = 11.111(2) ? b = 103.92(3)? V = 1341.6(5) 3, Z = 4, Dc = 1.776 g/cm3, Mr = 358.66, F(000) = 716, ?= 2.024 mm1 and S = 1.004. The final R = 0.0346 and wR = 0.0938 for 1011 observed reflections with I > 2(I). The Cu(Ⅱ) ion is six-coordinated by four N atoms of two L ligands and two Cl ions in a distorted octahedral geometry. The ligand L acts as a bis-bidentate ligand to bridge the Cu(Ⅱ) ions, resulting in an infinite chain structure.展开更多
The growth of crystals of the high T c oxide superconductors has been hampe red by the complexities of the materials and their phase diagrams.The most common crys tal growth technique adopted for these oxides is the ...The growth of crystals of the high T c oxide superconductors has been hampe red by the complexities of the materials and their phase diagrams.The most common crys tal growth technique adopted for these oxides is the “flux”method,where the st arting materials are solved in a melt,which is usually formed by excess CuO and BaO or a KCl/NaCl mixture.The crystals are produced by slow cooling of the heate d solvent.This method,however,suffers from several disadvantages: (1) the crystals are contaminated with the crucible material, (2) the crystals are difficult to remove from the crucible, (3) the crystals contain flux inclusions.展开更多
A new one-dimensional mixed-valence Cu（Ⅰ）/Cu（Ⅱ） complex [Cu（bipy）（Me2dtc）CuI2]n 1 （bipy = 2,2′-bipyridine and Me2dtc = N,N-dimethyldithiocarbamate） has been synthesized under solution condition, and chara...A new one-dimensional mixed-valence Cu（Ⅰ）/Cu（Ⅱ） complex [Cu（bipy）（Me2dtc）CuI2]n 1 （bipy = 2,2′-bipyridine and Me2dtc = N,N-dimethyldithiocarbamate） has been synthesized under solution condition, and characterized by elemental analysis, IR spectrum, single-crystal X-ray diffraction and magnetic property. The crystal belongs to the tetragonal system, space group P4122 with a = b = 11.6504（16）, c = 13.466（3） A, V = 1827.8（5） A^3, Z = 4, Dc = 2.389 g/cm^3, Mr = 657.27, λ（MoKa） = 0.71073 , μ = 5.931 mm·1, F（000） = 1236, the final R = 0.0483 and wR = 0.1245. A total of 2102 unique reflections were collected, of which 2009 with I 〉 2σ（I） were observed. 1 consists of polymeric [Cu^II2]nn^- anions and [Cu^II（bipy）（Me2dtc）]^＋ cations. It is interesting that the cations of 1 interact through π-π stacking interactions after rotating 90° to form one-dimensional chains parallel to the anion chains. The magnetic study indicates antiferromagnetic behavior for this complex.展开更多
The title compound [ClCH2(C7H6N2)]NO3 has been prepared and characterized by elemental analysis and X-ray studies. It crystallizes in the monoclinic system, space group P21/n with a = 7.4189(3), b =15.3064(6), c = 9.2...The title compound [ClCH2(C7H6N2)]NO3 has been prepared and characterized by elemental analysis and X-ray studies. It crystallizes in the monoclinic system, space group P21/n with a = 7.4189(3), b =15.3064(6), c = 9.2657(3) ? b = 102.449(2)? C8H8ClN3O3, Mr = 229.62, V = 1027.44(7) 3, Z = 4, Dc = 1.484 g/cm3, F(000) = 472, = 0.363 mm-1, R = 0.0671 and wR = 0.1546. The crystal structure consists of discrete 2-chloromethyl-1H-benzimidazole cations and NO3- anions. The benzimidazole ring with the conjunction carbon atom C(1) is fairly planar, with the deviation from the least plane through the ring atoms is smaller than 0.010(3) ? The analytical results of crystal structure show that three different non-covalent interactions in the compound, NH…O intermolecular hydrogen bonds, CH…O interaction and p-p stacking interaction, play an important role in the crystal packing.展开更多
Ab initio quantum mechanical method has been applied to nitrogen cages N_ 2n (n=12-18). Full geometry optimization, harmonic vibrational frequency and thermodynamics data for eight structures of nitrogen cages N_ 2n (...Ab initio quantum mechanical method has been applied to nitrogen cages N_ 2n (n=12-18). Full geometry optimization, harmonic vibrational frequency and thermodynamics data for eight structures of nitrogen cages N_ 2n (n=12-18) were performed at the HF/cc-pVDZ level. Cage N_ 24 (D_ 6d ), N_ 24 (O_h), N_ 26 (D_ 6d ), N_ 28 (T_d), N_ 30 (D_ 5h ), N_ 32 (D_ 3d ), N_ 36 (D_ 2d ) and N_ 36 (D_ 6h ) were found to be local minima on the potential energy surfaces. The computational results show that all the bond lengths of the eight structures are close to 0.145 nm and their bond energies E_ N-N are near to the experimental data of N-N single-bond. In addition, the thermochemical data of these nitrogen cages indicated that they are stable. It suggests that they are candidates for high energy density materials.展开更多
The title compound (C10H12N2O7, Mr = 272.22) crystallizes in triclinic, space group P1 with a = 5.532(2), b = 9.760(4), c = 11.731(5) ?, α = 68.107(7), β = 89.179(7), γ = 77.830(7)o, V = 573.1(4) ?3, Z = 2, Dc = 1....The title compound (C10H12N2O7, Mr = 272.22) crystallizes in triclinic, space group P1 with a = 5.532(2), b = 9.760(4), c = 11.731(5) ?, α = 68.107(7), β = 89.179(7), γ = 77.830(7)o, V = 573.1(4) ?3, Z = 2, Dc = 1.578 g/cm3, F(000) = 284 and μ(MoKa) = 0.136 mm-1. The final R = 0.0400 and wR = 0.0951 for 1468 observed reflections with I > 2σ(I). The title compound is a 1:1 adduct of sarcosine and 5-nitrosalicylic acid. The nitrogen atom of sarcosine is protonated, and the proton is from the carboxyl group of sarcosine and 5-nitrosalicylic acid with the probability of 50 percent for each. The 5-nitrosalicylic acid and sarcosine molecule of the title adduct are ABAB arranged along the c axis. There exist a lot of hydrogen bonds in the structure, linking sarcosine and 5-nitrosalicylic acid to form a three-dimensional network.展开更多
Condensation of D-glucose, o-phenylenediamine and N,N-benzylphenylhydrazine hydrochloride (NNBPHH) in a one-pot reaction, or condensation of 2-(D-arabino-tetritol-1-yl) quinoxaline and NNBPHH, gave 3-(D-erythro-glycer...Condensation of D-glucose, o-phenylenediamine and N,N-benzylphenylhydrazine hydrochloride (NNBPHH) in a one-pot reaction, or condensation of 2-(D-arabino-tetritol-1-yl) quinoxaline and NNBPHH, gave 3-(D-erythro-glycerol-1- yl)-1-phenyl-1H-pyrazolo[3,4-b]quinoxaline. The structure of the latter was determined by 1H NMR spectroscopy and by synthesis using phenylhydrazine hydrochloride instead of NNBPHH. Condensation of D-glucose and 4,5-dichloro-o-phenylenediamine gave 6,7-dichloro-2-(D-arabino-tetritol-1-yl)quinoxaline, which upon condensation with NNBPHH gave the corresponding 6,7-dichloro-3-(D-erythro-glycerol-1-yl)-1-phenyl-1H-pyrazolo[3,4-b]quinoxaline. The structure and mechanism of formation of these compounds are discussed.展开更多
文摘A new compound [Cu（AFO）2（N3）2]（DMF）（H2O）（AFO=4,5-diazafluorene-9-one）was synthesized.Its structure was determined by single X-ray diffraction.The crystal belongs to monoclinic system,space group C2/c.The crystallographic data,were determined a=1.2609（2）nm,b=0.8000（1）nm,c=2.6220（4）nm,β=109.964（6）°,V=2.4859（6）nm3,Z=4,F（000）=1236,Mr=603.07,Dc=1.611 Mg/m3,μ=0.937 nm-1,R1=0.0561,and wR2=0.1290.In the crystal Cu（II） atom is coordinated with four nitrogen from two AFO ligands and two nitrogen atoms from two azide ions to form an elonged-octahedron geometry.
基金This work was supported by the National Natural Science Foundation of China (No.20001007 20131020) Natural Science Foundation of the Chinese Academy of Sciences (KJCX2-H3) and Fujian province (2000F006)
文摘The title complex, [Cu(L)Cl2]n (L = 2,5-di-2-pyridyl-1,3,4-oxodiazole) 1, has been obtained from the reaction of 3,6-di-2-pyridyl-1,2,4,5-tetrazine (bptz) and CuCl2?H2O in a mixture solvent of CH3CN and CH2Cl2 (L is generated from the metal-assisted hydrolysis reaction of bptz) and structurally characterized. It crystallizes in space group C2/c of monoclinic system with cell parameters: a = 9.812(2), b = 12.679(3), c = 11.111(2) ? b = 103.92(3)? V = 1341.6(5) 3, Z = 4, Dc = 1.776 g/cm3, Mr = 358.66, F(000) = 716, ?= 2.024 mm1 and S = 1.004. The final R = 0.0346 and wR = 0.0938 for 1011 observed reflections with I > 2(I). The Cu(Ⅱ) ion is six-coordinated by four N atoms of two L ligands and two Cl ions in a distorted octahedral geometry. The ligand L acts as a bis-bidentate ligand to bridge the Cu(Ⅱ) ions, resulting in an infinite chain structure.
文摘The growth of crystals of the high T c oxide superconductors has been hampe red by the complexities of the materials and their phase diagrams.The most common crys tal growth technique adopted for these oxides is the “flux”method,where the st arting materials are solved in a melt,which is usually formed by excess CuO and BaO or a KCl/NaCl mixture.The crystals are produced by slow cooling of the heate d solvent.This method,however,suffers from several disadvantages: (1) the crystals are contaminated with the crucible material, (2) the crystals are difficult to remove from the crucible, (3) the crystals contain flux inclusions.
基金Supported by the National High Technology Research and Development Program of China (863 Program, No. 2009AA03Z217)the National Natural Science Foundation of China (No. 90922028)+1 种基金the Young Talent Program of Fujian Province (No. 2007F3060)the Fund of Fujian Provincial Key Laboratory of Nanomaterials (No. NM10-5)
文摘A new one-dimensional mixed-valence Cu（Ⅰ）/Cu（Ⅱ） complex [Cu（bipy）（Me2dtc）CuI2]n 1 （bipy = 2,2′-bipyridine and Me2dtc = N,N-dimethyldithiocarbamate） has been synthesized under solution condition, and characterized by elemental analysis, IR spectrum, single-crystal X-ray diffraction and magnetic property. The crystal belongs to the tetragonal system, space group P4122 with a = b = 11.6504（16）, c = 13.466（3） A, V = 1827.8（5） A^3, Z = 4, Dc = 2.389 g/cm^3, Mr = 657.27, λ（MoKa） = 0.71073 , μ = 5.931 mm·1, F（000） = 1236, the final R = 0.0483 and wR = 0.1245. A total of 2102 unique reflections were collected, of which 2009 with I 〉 2σ（I） were observed. 1 consists of polymeric [Cu^II2]nn^- anions and [Cu^II（bipy）（Me2dtc）]^＋ cations. It is interesting that the cations of 1 interact through π-π stacking interactions after rotating 90° to form one-dimensional chains parallel to the anion chains. The magnetic study indicates antiferromagnetic behavior for this complex.
基金the Natural Science Foundation of Shandong province (No. Y2002B06)the Outstanding Adult-Young Scientific Research Encouraging Foundation of Shandong province (No. O1BS18)
文摘The title compound [ClCH2(C7H6N2)]NO3 has been prepared and characterized by elemental analysis and X-ray studies. It crystallizes in the monoclinic system, space group P21/n with a = 7.4189(3), b =15.3064(6), c = 9.2657(3) ? b = 102.449(2)? C8H8ClN3O3, Mr = 229.62, V = 1027.44(7) 3, Z = 4, Dc = 1.484 g/cm3, F(000) = 472, = 0.363 mm-1, R = 0.0671 and wR = 0.1546. The crystal structure consists of discrete 2-chloromethyl-1H-benzimidazole cations and NO3- anions. The benzimidazole ring with the conjunction carbon atom C(1) is fairly planar, with the deviation from the least plane through the ring atoms is smaller than 0.010(3) ? The analytical results of crystal structure show that three different non-covalent interactions in the compound, NH…O intermolecular hydrogen bonds, CH…O interaction and p-p stacking interaction, play an important role in the crystal packing.
文摘Ab initio quantum mechanical method has been applied to nitrogen cages N_ 2n (n=12-18). Full geometry optimization, harmonic vibrational frequency and thermodynamics data for eight structures of nitrogen cages N_ 2n (n=12-18) were performed at the HF/cc-pVDZ level. Cage N_ 24 (D_ 6d ), N_ 24 (O_h), N_ 26 (D_ 6d ), N_ 28 (T_d), N_ 30 (D_ 5h ), N_ 32 (D_ 3d ), N_ 36 (D_ 2d ) and N_ 36 (D_ 6h ) were found to be local minima on the potential energy surfaces. The computational results show that all the bond lengths of the eight structures are close to 0.145 nm and their bond energies E_ N-N are near to the experimental data of N-N single-bond. In addition, the thermochemical data of these nitrogen cages indicated that they are stable. It suggests that they are candidates for high energy density materials.
文摘The title compound (C10H12N2O7, Mr = 272.22) crystallizes in triclinic, space group P1 with a = 5.532(2), b = 9.760(4), c = 11.731(5) ?, α = 68.107(7), β = 89.179(7), γ = 77.830(7)o, V = 573.1(4) ?3, Z = 2, Dc = 1.578 g/cm3, F(000) = 284 and μ(MoKa) = 0.136 mm-1. The final R = 0.0400 and wR = 0.0951 for 1468 observed reflections with I > 2σ(I). The title compound is a 1:1 adduct of sarcosine and 5-nitrosalicylic acid. The nitrogen atom of sarcosine is protonated, and the proton is from the carboxyl group of sarcosine and 5-nitrosalicylic acid with the probability of 50 percent for each. The 5-nitrosalicylic acid and sarcosine molecule of the title adduct are ABAB arranged along the c axis. There exist a lot of hydrogen bonds in the structure, linking sarcosine and 5-nitrosalicylic acid to form a three-dimensional network.
文摘Condensation of D-glucose, o-phenylenediamine and N,N-benzylphenylhydrazine hydrochloride (NNBPHH) in a one-pot reaction, or condensation of 2-(D-arabino-tetritol-1-yl) quinoxaline and NNBPHH, gave 3-(D-erythro-glycerol-1- yl)-1-phenyl-1H-pyrazolo[3,4-b]quinoxaline. The structure of the latter was determined by 1H NMR spectroscopy and by synthesis using phenylhydrazine hydrochloride instead of NNBPHH. Condensation of D-glucose and 4,5-dichloro-o-phenylenediamine gave 6,7-dichloro-2-(D-arabino-tetritol-1-yl)quinoxaline, which upon condensation with NNBPHH gave the corresponding 6,7-dichloro-3-(D-erythro-glycerol-1-yl)-1-phenyl-1H-pyrazolo[3,4-b]quinoxaline. The structure and mechanism of formation of these compounds are discussed.
