The title compound, 1-4-（dimethylamino）benzylidene）-4-（naphthalene-1-yl） thiosemicarbazide （DMABNTS, C20H20N4S, Mr = 348.47）, was synthesized and characterized by elemental analysis, 1R, ^1H NMR and MS. The cry...The title compound, 1-4-（dimethylamino）benzylidene）-4-（naphthalene-1-yl） thiosemicarbazide （DMABNTS, C20H20N4S, Mr = 348.47）, was synthesized and characterized by elemental analysis, 1R, ^1H NMR and MS. The crystal structure of DMABNTS with 1,4-dioxane （Diox, C4H8O2） solvent molecules （DMABNTS·2Diox, C28H36N4O4S, Mr = 524.67） was determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic system, space group P21/c with a = 14.418（4）, b = 7.1702（19）, c = 28.350（7）°A,β= 101.154（6）°, V= 2875.4（13） °A^3, Z= 4, Dc= 1.212 g/cm^3, F（000） = 1120 and μ= 0.151 mm^-1. A total of 6458 reflections were collected, of which 4671 were unique. The structure was solved by direct methods and refined to the final R = 0.0732 and wR = 0.2127 for 3921 observed reflections （I〉 2σ（I））. There exist intermolecular hydrogen bonds （N（2）-H（2B）…S（1A）and N（1）-H（1A）…O（4B）） in the structure. The study of fluorescent properties ＇shows that DMABNTS emits bright solid-state fluorescence in the visible region and exhibits blue photoluminescence.展开更多
The title compound bis（1-（4-（dimethylamino）benzylidene）-4-phenylthiosemicar-bazato）-palladium（Ⅱ）（PdL2） was obtained by reacting 1-（4-（dimethylamino）benzylidene）-4-phenyl-thiosemicarbazide with dichloro...The title compound bis（1-（4-（dimethylamino）benzylidene）-4-phenylthiosemicar-bazato）-palladium（Ⅱ）（PdL2） was obtained by reacting 1-（4-（dimethylamino）benzylidene）-4-phenyl-thiosemicarbazide with dichlorobis（benzonitrile）palladium（Ⅱ） in methanol,and its structure was characterized by single-crystal X-ray diffraction.The crystal of PdL2 was obtained in dimethyl-formamide（DMF） solvent with solvent molecules involved in the cell and crystallizes in the monoclinic system,space group C2 with a = 18.485（15）,b = 7.090（5）,c = 17.595（11） ,β = 121.21（3）o,V = 1972（2） 3,Z = 2,Mr = 847.40,Dc = 1.427 g/cm3,μ = 0.624 mm-1,F（000） = 880,R = 0.0607 and wR = 0.1358.The Pd atom adopts a distorted square planar coordination geometry with two Pd-N and two Pd-S bonds.The ligand loses a proton from its tautomeric thiol form and coordinates to the Pd atom via mercapto sulfur and the imine nitrogen atom,which binds to palladium as bidentate N,S-donors forming five-membered chelate rings.The complex formed hydrogen bonding interaction with solvent DMF molecules from the hydrogen of phenylamine to the oxygen of DMF and several intramolecular hydrogen bonds.Pd（Ⅱ） perturbed ligand π-π＊ transition and metal-to-ligand charge transfer（MLCT） transition are observed in its electronic absorption spectra.The complex exhibits intraligand 1π-π＊（IL） state and MLCT state dual fluorescent emissions in organic solvent at room temperature.展开更多
We report results from the investigation of the nonlinear refractive index and nonlinear absorption coefficient of {(1Z)-[4-(Dimethylamino)phenyl]methylene} 4-nitrobenzocarboxy hydrazone mono-hydrate (DMPM4NBCHM) solu...We report results from the investigation of the nonlinear refractive index and nonlinear absorption coefficient of {(1Z)-[4-(Dimethylamino)phenyl]methylene} 4-nitrobenzocarboxy hydrazone mono-hydrate (DMPM4NBCHM) solution using Z-scan technique with a continuous wave (CW) Argon ion laser. The results show that this type of organic material has a large nonlinear absorption and nonlinear refractive index at 488 nm and 514 nm. The origin of the nonlinear effects was discussed. We demonstrate that the light induced nonlinear refractive index variation, leads to limiting effect. The results indicated that DMPM4NBCHM could be promising candidates for application on nonlinear photonic devices and optical limiters.展开更多
Hinokitiolis frequently added to personal care products as an antibacterial agent. We previously established an HPLC-UV method for determination of hinokitiol in skin lotion after pre-column derivatization with 4-fluo...Hinokitiolis frequently added to personal care products as an antibacterial agent. We previously established an HPLC-UV method for determination of hinokitiol in skin lotion after pre-column derivatization with 4-fluoro-7-nitro-2,1,3-benzoxadiazole. However, the labeling reagent is expensive, and derivatives of degradation products of parabens, which may be added to skin lotion as general preservatives, interfered with the peak of the hinokitiol derivative. In this study, the concentration of hinokitiol in skin lotions was determined by HPLC with a visible light detector (450 nm) after pre-column derivatization with 4-(dimethylamino)azobenzene-4’-sulfonyl chloride (Dabsyl-Cl), a more economical reagent. A standard curve was obtained after derivatization with Dabsyl-Cl in borate buffer (pH 9.5) at 55°C for 10 min. The retention time of Dabsyl-hinokitiol was 6.8 min. The calibration plot was linear in the range of 1.25 to 40 μg/mL with a r2 value of 0.9991, and the lower limit of quantification and detection were 0.60 μg/mL (absolute amount of 0.86 ng/20μL injection, signal-to-noise ratio of 10:1) and 0.18 μg/mL (absolute amount of 0.26 ng/20μL injection, signal-to-noise ratio of 3:1), respectively. The coefficient of variation was less than 8.8%. Seven Dabsyl-paraben derivatives showed little interference with the peak of Dabsyl-hinokitiol. The developed system was used to determine the content of hinokitiol in two skin lotions. Addition-recovery tests gave satisfactory results.展开更多
文摘The title compound, 1-4-（dimethylamino）benzylidene）-4-（naphthalene-1-yl） thiosemicarbazide （DMABNTS, C20H20N4S, Mr = 348.47）, was synthesized and characterized by elemental analysis, 1R, ^1H NMR and MS. The crystal structure of DMABNTS with 1,4-dioxane （Diox, C4H8O2） solvent molecules （DMABNTS·2Diox, C28H36N4O4S, Mr = 524.67） was determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic system, space group P21/c with a = 14.418（4）, b = 7.1702（19）, c = 28.350（7）°A,β= 101.154（6）°, V= 2875.4（13） °A^3, Z= 4, Dc= 1.212 g/cm^3, F（000） = 1120 and μ= 0.151 mm^-1. A total of 6458 reflections were collected, of which 4671 were unique. The structure was solved by direct methods and refined to the final R = 0.0732 and wR = 0.2127 for 3921 observed reflections （I〉 2σ（I））. There exist intermolecular hydrogen bonds （N（2）-H（2B）…S（1A）and N（1）-H（1A）…O（4B）） in the structure. The study of fluorescent properties ＇shows that DMABNTS emits bright solid-state fluorescence in the visible region and exhibits blue photoluminescence.
基金supported by the National Basic Research Program of China (973 Program,2007CB815301)NSF (No. 20721001)the Science & Technology Innovation Project of Xiamen University (No. K70025)
文摘The title compound bis（1-（4-（dimethylamino）benzylidene）-4-phenylthiosemicar-bazato）-palladium（Ⅱ）（PdL2） was obtained by reacting 1-（4-（dimethylamino）benzylidene）-4-phenyl-thiosemicarbazide with dichlorobis（benzonitrile）palladium（Ⅱ） in methanol,and its structure was characterized by single-crystal X-ray diffraction.The crystal of PdL2 was obtained in dimethyl-formamide（DMF） solvent with solvent molecules involved in the cell and crystallizes in the monoclinic system,space group C2 with a = 18.485（15）,b = 7.090（5）,c = 17.595（11） ,β = 121.21（3）o,V = 1972（2） 3,Z = 2,Mr = 847.40,Dc = 1.427 g/cm3,μ = 0.624 mm-1,F（000） = 880,R = 0.0607 and wR = 0.1358.The Pd atom adopts a distorted square planar coordination geometry with two Pd-N and two Pd-S bonds.The ligand loses a proton from its tautomeric thiol form and coordinates to the Pd atom via mercapto sulfur and the imine nitrogen atom,which binds to palladium as bidentate N,S-donors forming five-membered chelate rings.The complex formed hydrogen bonding interaction with solvent DMF molecules from the hydrogen of phenylamine to the oxygen of DMF and several intramolecular hydrogen bonds.Pd（Ⅱ） perturbed ligand π-π＊ transition and metal-to-ligand charge transfer（MLCT） transition are observed in its electronic absorption spectra.The complex exhibits intraligand 1π-π＊（IL） state and MLCT state dual fluorescent emissions in organic solvent at room temperature.
文摘We report results from the investigation of the nonlinear refractive index and nonlinear absorption coefficient of {(1Z)-[4-(Dimethylamino)phenyl]methylene} 4-nitrobenzocarboxy hydrazone mono-hydrate (DMPM4NBCHM) solution using Z-scan technique with a continuous wave (CW) Argon ion laser. The results show that this type of organic material has a large nonlinear absorption and nonlinear refractive index at 488 nm and 514 nm. The origin of the nonlinear effects was discussed. We demonstrate that the light induced nonlinear refractive index variation, leads to limiting effect. The results indicated that DMPM4NBCHM could be promising candidates for application on nonlinear photonic devices and optical limiters.
文摘Hinokitiolis frequently added to personal care products as an antibacterial agent. We previously established an HPLC-UV method for determination of hinokitiol in skin lotion after pre-column derivatization with 4-fluoro-7-nitro-2,1,3-benzoxadiazole. However, the labeling reagent is expensive, and derivatives of degradation products of parabens, which may be added to skin lotion as general preservatives, interfered with the peak of the hinokitiol derivative. In this study, the concentration of hinokitiol in skin lotions was determined by HPLC with a visible light detector (450 nm) after pre-column derivatization with 4-(dimethylamino)azobenzene-4’-sulfonyl chloride (Dabsyl-Cl), a more economical reagent. A standard curve was obtained after derivatization with Dabsyl-Cl in borate buffer (pH 9.5) at 55°C for 10 min. The retention time of Dabsyl-hinokitiol was 6.8 min. The calibration plot was linear in the range of 1.25 to 40 μg/mL with a r2 value of 0.9991, and the lower limit of quantification and detection were 0.60 μg/mL (absolute amount of 0.86 ng/20μL injection, signal-to-noise ratio of 10:1) and 0.18 μg/mL (absolute amount of 0.26 ng/20μL injection, signal-to-noise ratio of 3:1), respectively. The coefficient of variation was less than 8.8%. Seven Dabsyl-paraben derivatives showed little interference with the peak of Dabsyl-hinokitiol. The developed system was used to determine the content of hinokitiol in two skin lotions. Addition-recovery tests gave satisfactory results.
