在Ni70Mn25Co5-C体系中添加含氢化合物Fe(C5H5)2作为新型氢源,利用温度梯度法,在压力为5.5—6.0 GPa、温度为1280—1400°C的条件下,成功合成出氢掺杂的宝石级金刚石大单晶.通过傅里叶显微红外光谱发现,随着Fe(C5H5)2添加量的增加,...在Ni70Mn25Co5-C体系中添加含氢化合物Fe(C5H5)2作为新型氢源,利用温度梯度法,在压力为5.5—6.0 GPa、温度为1280—1400°C的条件下,成功合成出氢掺杂的宝石级金刚石大单晶.通过傅里叶显微红外光谱发现,随着Fe(C5H5)2添加量的增加,合成晶体中与氢相关的对应于sp3杂化C—H键的对称伸缩振动和反对称伸缩振动的红外特征峰2850和2920 cm 1逐渐增强,而晶体中氮含量却逐渐减少.通过合成晶体的拉曼光谱分析发现,金刚石的拉曼峰伴随Fe(C5H5)2的添加向高频偏移,这表明氢的进入在金刚石内部产生了压应力.观察扫描电子显微镜图像发现,在低含量Fe(C5H5)2添加时晶体表面平滑,而高含量添加时晶体表面缺陷增多,且呈现出气孔状.使用新的添加剂Fe(C5H5)2作为氢源,合成出含氢宝石级金刚石单晶,丰富了金刚石单晶中对氢的研究内容,也可为理解天然金刚石的形成机理提供帮助.展开更多
It was proved by ICP, fluorescence spectra and N 2 adsorption that the rare earth complex [C 5H 5NC 16H 33] [Eu(TTA) 4] is in the channel of Si-MCM-41 in the course of assembly. The rare earth complex of 67.9% is in t...It was proved by ICP, fluorescence spectra and N 2 adsorption that the rare earth complex [C 5H 5NC 16H 33] [Eu(TTA) 4] is in the channel of Si-MCM-41 in the course of assembly. The rare earth complex of 67.9% is in the channel, suggesting that the assembly of the complex molecular on the mesoporous MCM-41 was carried out mainly in the channel.展开更多
The novel copper?complex with salicylaldehyde benzoylhydrazone and pyridine ligands, Cu(C14H10N2O2)(C5H5N), has been synthesized and characterized by elemental analysis, IR and thermal analysis. The crystal structure ...The novel copper?complex with salicylaldehyde benzoylhydrazone and pyridine ligands, Cu(C14H10N2O2)(C5H5N), has been synthesized and characterized by elemental analysis, IR and thermal analysis. The crystal structure of the title complex has been determined by single crystal X ray diffraction techniques. The crystal belongs to monoclinic with space group P21/c. The cell parameters are: a=1.6362(9)nm, b=1.7140(9)nm, c=1.2255(7)nm, β=105.168(9)°, V=3.317(3)nm3, Z=8, Dc=1.525g·cm-3, μ(MoKα)=1.334mm-1, F(000)=1560. The structure wasrefined to final R1=0.0376, wR2=0.0909. The copper?ion lies in a distorted square planar environment composed of two oxygen atoms, one nitrogen atom of tridentate acyhydrazone Schiff base ligand and one nitrogen atom of the pyridine ligand. CCDC: 193111.展开更多
A thin film electroluminescence cell with the structure of ITO /PPV /PVK∶Eu（TTA）4C5H5NC16H33∶PBD /Alq 3 /Al has been fabricated.Red emissio n with a very sharp spectral band at 614nm was observed and a maximum lum...A thin film electroluminescence cell with the structure of ITO /PPV /PVK∶Eu（TTA）4C5H5NC16H33∶PBD /Alq 3 /Al has been fabricated.Red emissio n with a very sharp spectral band at 614nm was observed and a maximum luminance of 20cd·m -2 at 36V was obtained from the spin-coated device.The full width at half maximum of lu-minescent spectrum is less than 10nm.展开更多
The Copper(Ⅰ) supramolecular complexes of 4,5-bis(methylthio)-1,3-dithiole-2-thione (C5H6S5), [Cu(C5H6S5)(SCN)]∞ 1 and [Cu(C5H6S5)I]∞ 2, have been prepared and characterized. X-ray structure analysis for complex 1 ...The Copper(Ⅰ) supramolecular complexes of 4,5-bis(methylthio)-1,3-dithiole-2-thione (C5H6S5), [Cu(C5H6S5)(SCN)]∞ 1 and [Cu(C5H6S5)I]∞ 2, have been prepared and characterized. X-ray structure analysis for complex 1 reveals that the infinite chain structure with polymeric stairs of different lengths is formed through the coordination mode (μ3) of the thiocyanate bridges. The shorter interchain S...S contacts give rise to a three-dimensional network structure. CCDC: 215668.展开更多
In recent years,the organometallic ehemistry of the lanthanide metals in low oxidation states has beenactively investigated.The synthesis of the low一valent lanthanide eomPlexes has the signifieant meanings ontheory a...In recent years,the organometallic ehemistry of the lanthanide metals in low oxidation states has beenactively investigated.The synthesis of the low一valent lanthanide eomPlexes has the signifieant meanings ontheory and praeti展开更多
The LB film of the title complex was prepared by dropping a benzene solution of the title complex on the surfaceof water subphase at 25±1℃.The film was deposited in Z type on various hydrophilic pretreated subst...The LB film of the title complex was prepared by dropping a benzene solution of the title complex on the surfaceof water subphase at 25±1℃.The film was deposited in Z type on various hydrophilic pretreated substrates ofquartz,CaF;and electronic conductive glass for different purposes.The π-A curve of the film shows that thecross section per molecule is 125;,which indicates that the alkyl chain of the molecule is basically perpendiculalto the surface of the substrate.UV,IR spectra and transmission electronic microscopy of the film were also obtained.展开更多
利用水热合成法合成了分子组成为(C6H11NH3)5H(P2Mo5O23)4H2O的杂多化合物, 用单晶X-ray衍射方法测定了它的结构,该晶体属于单斜晶系,空间群P21/c, a = 12.830(3), b = 14.848(3), c = 25.258(5) ? b = 92.95(3), Mr = 1483.62, V = 48...利用水热合成法合成了分子组成为(C6H11NH3)5H(P2Mo5O23)4H2O的杂多化合物, 用单晶X-ray衍射方法测定了它的结构,该晶体属于单斜晶系,空间群P21/c, a = 12.830(3), b = 14.848(3), c = 25.258(5) ? b = 92.95(3), Mr = 1483.62, V = 4805.1(17) 3, Z = 4, Dc = 2.051 g/cm3, m = 1.431 mm-1, F(000) = 3000, I >2s(I) 的可观察衍射点4426个, 最终结构偏差因子R = 0.0464, wR = 0.0801, S = 0.731。在[P2Mo5O23]6-杂多阴离子中5个MoO6八面体通过共边和共角相连, 形成1个近似的五角平面骨架, 2个PO4四面体加在五角平面的两侧。热性质研究表明杂多阴离子骨架在547.4 ℃左右分解。展开更多
The novel polyoxometalate, 32[Mo8ⅣMo4ⅤV2ⅣO38(PO4)], was synthesized and characterized by elementary analysis, EPR, IR spectra and X ray diffraction. The compoundcrystallizes in triclinic system, space group with a=...The novel polyoxometalate, 32[Mo8ⅣMo4ⅤV2ⅣO38(PO4)], was synthesized and characterized by elementary analysis, EPR, IR spectra and X ray diffraction. The compoundcrystallizes in triclinic system, space group with a= 1.41999(2)nm, b=1.43467(2)nm, c=1.694610(10)nm, α=95.7250(10)°, β=92.2110(10)°, γ=92.6060(10)°, V=3.42829(7)nm3, Z=2, Dc=2.388g·cm-3, Mr=2465.10g·mol-1, μ=2.489mm-1, F(000)=2388, R1=0.0584, wR2=0.1461, S=1.164. The heteropolyanion is a bi capped pseudo Keggin complex. CCDC: 186645.展开更多
The title complex Cu[C5H3N(CCH3=N-C6H5)2]2(PF6)2 has been synthesized by r eaction of Schiff base C5H3N(CCH3=N-C6H5)2 and cupric sulfate in toluene solut ion. The crystal structure was determined by X-ray diffraction ...The title complex Cu[C5H3N(CCH3=N-C6H5)2]2(PF6)2 has been synthesized by r eaction of Schiff base C5H3N(CCH3=N-C6H5)2 and cupric sulfate in toluene solut ion. The crystal structure was determined by X-ray diffraction method and the chemical formula weight of the complex is 1041.85. The crystal structure belongs to triclinic system with spacegroup and cell parameters: a=12.6470(10) , b=14. 123(2) , c=15.613(2);á=66.150(10)a=79.470(10)?=78.290(10)穖-3 and F(000)=1064. The final R:R1=0.0668, wR 2=0.1927; R(all data): R1=0.1133, wR2=0.2357. The Cu was coordinated by six nitrogen, at the same time the Cu formed a distorted octahedron, besides the angles and pl anes of this compound were discussed . The result of kinetics of the thermal dec omposition indicated that the first step of it is 2 series chemical reactions, t he function of machanism is f(a)=(1-a)2, and the activation energy is 144.64E/ kJ. CCDC: 180872.展开更多
S A new cyclomercurated ferrocenylketimine containing pyridyl ring ([HgCl(5- C5H3C(CH3)=N-3-C5H4N)Fe(5-C5H5)]紺H2Cl2, Mr = 581.66) was synthesized and its molecular structure has been confirmed by IR, elemental analys...S A new cyclomercurated ferrocenylketimine containing pyridyl ring ([HgCl(5- C5H3C(CH3)=N-3-C5H4N)Fe(5-C5H5)]紺H2Cl2, Mr = 581.66) was synthesized and its molecular structure has been confirmed by IR, elemental analysis, 1H-NMR and X-ray crystal structure analysis. It is of monoclinic system, space group P21/c with a = 9.213(2), b = 17.479(4), c = 11.510(2) ? b = 100.32(3)o, V = 1823.7(6) 3, Z = 4, C17.5H16Cl2FeHgN2, Dc = 2.119 g/cm3, m = 9.497 mm-1, F(000) = 1100, R = 0.0436 and wR = 0.0987. The independent reflections are 3527, of which 3153 with I ≥ 2s(I) were observed. The compound contains a five-membered metallocycle. The mercury atom is bonded with the 2-position of substituted cyclopentadienyl ring (Cp), and coordinated weakly to the N atom of imino group. The pyridyl ring is almost perpendicular to the substituted Cp which is nearly coplanar with the metallocycle. The Hg(1)C(1) and Hg(1)Cl(1) bond lengths are 2.050(8) and 2.321(2) ? respectively.展开更多
文摘在Ni70Mn25Co5-C体系中添加含氢化合物Fe(C5H5)2作为新型氢源,利用温度梯度法,在压力为5.5—6.0 GPa、温度为1280—1400°C的条件下,成功合成出氢掺杂的宝石级金刚石大单晶.通过傅里叶显微红外光谱发现,随着Fe(C5H5)2添加量的增加,合成晶体中与氢相关的对应于sp3杂化C—H键的对称伸缩振动和反对称伸缩振动的红外特征峰2850和2920 cm 1逐渐增强,而晶体中氮含量却逐渐减少.通过合成晶体的拉曼光谱分析发现,金刚石的拉曼峰伴随Fe(C5H5)2的添加向高频偏移,这表明氢的进入在金刚石内部产生了压应力.观察扫描电子显微镜图像发现,在低含量Fe(C5H5)2添加时晶体表面平滑,而高含量添加时晶体表面缺陷增多,且呈现出气孔状.使用新的添加剂Fe(C5H5)2作为氢源,合成出含氢宝石级金刚石单晶,丰富了金刚石单晶中对氢的研究内容,也可为理解天然金刚石的形成机理提供帮助.
文摘It was proved by ICP, fluorescence spectra and N 2 adsorption that the rare earth complex [C 5H 5NC 16H 33] [Eu(TTA) 4] is in the channel of Si-MCM-41 in the course of assembly. The rare earth complex of 67.9% is in the channel, suggesting that the assembly of the complex molecular on the mesoporous MCM-41 was carried out mainly in the channel.
文摘The novel copper?complex with salicylaldehyde benzoylhydrazone and pyridine ligands, Cu(C14H10N2O2)(C5H5N), has been synthesized and characterized by elemental analysis, IR and thermal analysis. The crystal structure of the title complex has been determined by single crystal X ray diffraction techniques. The crystal belongs to monoclinic with space group P21/c. The cell parameters are: a=1.6362(9)nm, b=1.7140(9)nm, c=1.2255(7)nm, β=105.168(9)°, V=3.317(3)nm3, Z=8, Dc=1.525g·cm-3, μ(MoKα)=1.334mm-1, F(000)=1560. The structure wasrefined to final R1=0.0376, wR2=0.0909. The copper?ion lies in a distorted square planar environment composed of two oxygen atoms, one nitrogen atom of tridentate acyhydrazone Schiff base ligand and one nitrogen atom of the pyridine ligand. CCDC: 193111.
文摘A thin film electroluminescence cell with the structure of ITO /PPV /PVK∶Eu（TTA）4C5H5NC16H33∶PBD /Alq 3 /Al has been fabricated.Red emissio n with a very sharp spectral band at 614nm was observed and a maximum luminance of 20cd·m -2 at 36V was obtained from the spin-coated device.The full width at half maximum of lu-minescent spectrum is less than 10nm.
文摘The Copper(Ⅰ) supramolecular complexes of 4,5-bis(methylthio)-1,3-dithiole-2-thione (C5H6S5), [Cu(C5H6S5)(SCN)]∞ 1 and [Cu(C5H6S5)I]∞ 2, have been prepared and characterized. X-ray structure analysis for complex 1 reveals that the infinite chain structure with polymeric stairs of different lengths is formed through the coordination mode (μ3) of the thiocyanate bridges. The shorter interchain S...S contacts give rise to a three-dimensional network structure. CCDC: 215668.
文摘In recent years,the organometallic ehemistry of the lanthanide metals in low oxidation states has beenactively investigated.The synthesis of the low一valent lanthanide eomPlexes has the signifieant meanings ontheory and praeti
文摘The LB film of the title complex was prepared by dropping a benzene solution of the title complex on the surfaceof water subphase at 25±1℃.The film was deposited in Z type on various hydrophilic pretreated substrates ofquartz,CaF;and electronic conductive glass for different purposes.The π-A curve of the film shows that thecross section per molecule is 125;,which indicates that the alkyl chain of the molecule is basically perpendiculalto the surface of the substrate.UV,IR spectra and transmission electronic microscopy of the film were also obtained.
文摘The novel polyoxometalate, 32[Mo8ⅣMo4ⅤV2ⅣO38(PO4)], was synthesized and characterized by elementary analysis, EPR, IR spectra and X ray diffraction. The compoundcrystallizes in triclinic system, space group with a= 1.41999(2)nm, b=1.43467(2)nm, c=1.694610(10)nm, α=95.7250(10)°, β=92.2110(10)°, γ=92.6060(10)°, V=3.42829(7)nm3, Z=2, Dc=2.388g·cm-3, Mr=2465.10g·mol-1, μ=2.489mm-1, F(000)=2388, R1=0.0584, wR2=0.1461, S=1.164. The heteropolyanion is a bi capped pseudo Keggin complex. CCDC: 186645.
文摘The title complex Cu[C5H3N(CCH3=N-C6H5)2]2(PF6)2 has been synthesized by r eaction of Schiff base C5H3N(CCH3=N-C6H5)2 and cupric sulfate in toluene solut ion. The crystal structure was determined by X-ray diffraction method and the chemical formula weight of the complex is 1041.85. The crystal structure belongs to triclinic system with spacegroup and cell parameters: a=12.6470(10) , b=14. 123(2) , c=15.613(2);á=66.150(10)a=79.470(10)?=78.290(10)穖-3 and F(000)=1064. The final R:R1=0.0668, wR 2=0.1927; R(all data): R1=0.1133, wR2=0.2357. The Cu was coordinated by six nitrogen, at the same time the Cu formed a distorted octahedron, besides the angles and pl anes of this compound were discussed . The result of kinetics of the thermal dec omposition indicated that the first step of it is 2 series chemical reactions, t he function of machanism is f(a)=(1-a)2, and the activation energy is 144.64E/ kJ. CCDC: 180872.
基金This work was supported by NNSFC (No. 20072034) and NSF of Henan province
文摘S A new cyclomercurated ferrocenylketimine containing pyridyl ring ([HgCl(5- C5H3C(CH3)=N-3-C5H4N)Fe(5-C5H5)]紺H2Cl2, Mr = 581.66) was synthesized and its molecular structure has been confirmed by IR, elemental analysis, 1H-NMR and X-ray crystal structure analysis. It is of monoclinic system, space group P21/c with a = 9.213(2), b = 17.479(4), c = 11.510(2) ? b = 100.32(3)o, V = 1823.7(6) 3, Z = 4, C17.5H16Cl2FeHgN2, Dc = 2.119 g/cm3, m = 9.497 mm-1, F(000) = 1100, R = 0.0436 and wR = 0.0987. The independent reflections are 3527, of which 3153 with I ≥ 2s(I) were observed. The compound contains a five-membered metallocycle. The mercury atom is bonded with the 2-position of substituted cyclopentadienyl ring (Cp), and coordinated weakly to the N atom of imino group. The pyridyl ring is almost perpendicular to the substituted Cp which is nearly coplanar with the metallocycle. The Hg(1)C(1) and Hg(1)Cl(1) bond lengths are 2.050(8) and 2.321(2) ? respectively.
