Two mononuclear tin(IV) complexes, [Sn(pda)2(edt)2] (pda = o-phenylenediamine) (C16H24N4S4Sn, Mr = 519.32) 1 and [Sn(eda)(edt)2] (eda = ethylenediamine) (C6H16N2S4Sn, Mr = 363.14) 2 were synthesized and characterized ...Two mononuclear tin(IV) complexes, [Sn(pda)2(edt)2] (pda = o-phenylenediamine) (C16H24N4S4Sn, Mr = 519.32) 1 and [Sn(eda)(edt)2] (eda = ethylenediamine) (C6H16N2S4Sn, Mr = 363.14) 2 were synthesized and characterized by X-ray structure analysis. 1 belongs to trigonal, space group P-3c1 with a = b = 20.0280(6), c = 8.7679(5) ? V = 3045.8(2) ?, Z = 6, Dc = 1.699 g/cm3, m = 1.677 mm-1, F(000) = 1572, the final R = 0.0418 and wR = 0.1019 for 1805 independent reflections. 2 crystallizes in monoclinic, space group P21/c with a = 10.911(3), b = 9.783(2), c = 11.831(3) ? b = 100.28(2), V = 1242.6(6) ?, Z = 4, Dc = 1.941 g/cm3, m = 2.690 mm-1, F(000) = 720, the final R = 0.0280 and wR = 0.0627 for 2166 independent reflections. Both Sn4+ ions in these two complexes are six-coordinated with a slightly distorted octahedral configu- ration.展开更多
In this paper,a novel diiron ethane-1,2-dithiolate complex[Fe2(CO)4{κ2-(Ph2P)2(1,2-C6H4)}(μ-SCH2CH2S)]has been prepared and structurally characterized.Treatment of the parent complex[Fe2(CO)6(μ-SCH2CH2S)]with 1 equ...In this paper,a novel diiron ethane-1,2-dithiolate complex[Fe2(CO)4{κ2-(Ph2P)2(1,2-C6H4)}(μ-SCH2CH2S)]has been prepared and structurally characterized.Treatment of the parent complex[Fe2(CO)6(μ-SCH2CH2S)]with 1 equivalent of 1,2-bis(diphenylphosphino)benzene and Me3NO?2H2O as the oxidative agent gave the title complex in good yield.The title complex has been characterized by elemental analysis,IR,1H NMR,31P{1H}NMR,13C{1H}NMR spectroscopy,and X-ray crystallography.X-ray crystal structure of the title complex contains a butterfly diiron cluster with a bridging ethane-1,2-dithiolate,four terminal carbonyls,and a chelating 1,2-bis(diphenylphosphino)benzene.In addition,electrochemical studies revealed that the title complex can catalyze the reduction of protons to H2 in the presence of acetic acid.展开更多
The reactions of Co（C1O4）2·6H2O and Co（NO3）2.6H2O with the di-Schiff base ligand N,N＇-bis-（1-benzimidazo-2-yl-ethylidene）-ethane-1,2-diamine （LA） in ethanol have been investigated. The reactions of LA wi...The reactions of Co（C1O4）2·6H2O and Co（NO3）2.6H2O with the di-Schiff base ligand N,N＇-bis-（1-benzimidazo-2-yl-ethylidene）-ethane-1,2-diamine （LA） in ethanol have been investigated. The reactions of LA with excess amount of cobalt salts yield the six-coordinate complexes [CoL2]（ClO4）E·H2O 1 and [CoL2]（NO3）E·H2O 2 as isolatable products （L= N-（1- benzimidazo-2-yl-ethylidene）-ethane-1,2-diamine）, where L is a tri-dentate mono-Schiff base ligand, resulting from the hydrolysis of the precursor di-Schiff base LA. Both complexes were characterized by X-ray crystallography. Crystal data for complex 1： monoclinic, space group P21/c, a = 11.9214（10）, b = 23.5828（17）, c = 14.0387（12）A, β = 135.219（4）°, C22H30Cl2CoN8O9, Mr = 680.37, V = 2780.1（4） A^3 ,Z = 4, Dc = 1.625 g/cm^3,μ（MoKa） = 0.876 mm^-1, F（000） = 1404, the final R = 0.0725 and wR = 0.1530 for 5726 observed reflections （I 〉 2σ（I））. Crystal data for complex 2： monoclinic, space group P21/c, a = 18.2162（16）, b = 10.0610（6）, c = 18.593（2）A, β = 130.099（3）°, C22H30CoN10O7, Mr = 605.49, V = 2606.5（4） A3 Z = 4, Dc = 1.543 g/cm^3,μ（MoKa） = 0.722 mm^-1, F（000） = 1260, the final R = 0.0619 and wR = 0.1429 for 5194 observed reflections （I 〉 2σ（I））. X-ray diffraction analysis reveals that each cobalt atom in the two complexes is chelated by six nitrogen atoms from two tridentate iigands L, exhibiting a slightly distorted octahedral coordination sphere. In both complexes, the strong hydrogen-bonding interactions between the lattice waters and N-H groups of the ligands result in 1D chains which are further connected by ClO4^- （or NO3^-） groups to form a 3D framework. In complex 2, the strong π-π interactions increase the stability of the structure.展开更多
A novel carbazole photoinitiator 1-(6-o-chloro-benzoyl-9-ethyl-9H-carbazol-3yl)-ethane-1-one oxime O-ethyrate is synthesized from carbazole by N-alkylation,Friedel-Crafts acylation,oximation and esterification.The str...A novel carbazole photoinitiator 1-(6-o-chloro-benzoyl-9-ethyl-9H-carbazol-3yl)-ethane-1-one oxime O-ethyrate is synthesized from carbazole by N-alkylation,Friedel-Crafts acylation,oximation and esterification.The structure is characterized by 1HNMR,13CNMR,UV and IR.This paper discuss the catalyst,temperature and time of oximation and gain the optimum reaction conditions:CH3COOK is base,temperature is 70℃ and time is 6h.The yield is 89.1%.展开更多
研究了p H以及表面活性剂对邻羟基苯基亚氨基乙二铵氟硼酸盐DJQ-45的光谱,发现p H对DJQ-45的光谱的影响具有可逆性;DJQ-45可以定量检测表面活性剂TX-100,当TX-100的浓度小于0.2 m M时,溶液的荧光强度下降的较为缓慢,当TX-100的浓度大于0...研究了p H以及表面活性剂对邻羟基苯基亚氨基乙二铵氟硼酸盐DJQ-45的光谱,发现p H对DJQ-45的光谱的影响具有可逆性;DJQ-45可以定量检测表面活性剂TX-100,当TX-100的浓度小于0.2 m M时,溶液的荧光强度下降的较为缓慢,当TX-100的浓度大于0.2 m M时,溶液的荧光强度急剧下降,当TX-100的浓度达到16 m M时,溶液的荧光光谱发生蓝移,蓝移了14 nm,强度急剧下降,当TX-100的浓度从25 m M到45 m M时,溶液的荧光强度基本保持不变。邻羟基苯基亚氨基乙二铵氟硼酸盐有希望被用做检测TX-100。展开更多
Reaction of 4,4’-(1,4-phenylene)bis(5-acetyl-6-methyl-2-thioxo-1,2-dihydropyridine-3-carbonitrile) (1) with methyl iodide afforded the 4,4’-(1,4-phenylene)bis(5-acetyl-6-methyl-2-(methylthio)nicotinonitrile) (2). Th...Reaction of 4,4’-(1,4-phenylene)bis(5-acetyl-6-methyl-2-thioxo-1,2-dihydropyridine-3-carbonitrile) (1) with methyl iodide afforded the 4,4’-(1,4-phenylene)bis(5-acetyl-6-methyl-2-(methylthio)nicotinonitrile) (2). The reaction of 2 with hydrazine hydrate followed by diazotization reaction af-forded the 1,1’-(1,4-phenylenebis(3-amino-6-methyl-1H-pyrazolo[3,4-b]pyridine-4,5-diyl))bis(e-than-1-one) (3) and 1,1’-(1,4-phenylenebis(3-(chlorodiazenyl)-6-methyl-1H-pyrazolo[3,4-b]-pyridine-4,5-diyl))bis(ethan-1-one) (4) respectively. On the other hand, reaction of 4 with malononitrile, 2-cyanoethanethioamide, ethyl acetoacetate, acetyl acetone, ethyl benzoylacetate, diethylmalonate, ethyl cyanoacetate and phenacylbromide aiming to build up pyrazolotriazine or pyrazole ring on the ring system of 4. Structures of all newly synthesized heterocyclic compounds in the present study were confirmed by considering the data of IR, 1H NMR, mass spectra as well as that of elemental analyses.展开更多
基金This research was financially supported by the grants from the State Key Laboratory of Structural Chemistry the National Science and Technology of China (001CB1089)+1 种基金 the Chinese Academy of Sciences (CAS) the National Science Foundation of China (20
文摘Two mononuclear tin(IV) complexes, [Sn(pda)2(edt)2] (pda = o-phenylenediamine) (C16H24N4S4Sn, Mr = 519.32) 1 and [Sn(eda)(edt)2] (eda = ethylenediamine) (C6H16N2S4Sn, Mr = 363.14) 2 were synthesized and characterized by X-ray structure analysis. 1 belongs to trigonal, space group P-3c1 with a = b = 20.0280(6), c = 8.7679(5) ? V = 3045.8(2) ?, Z = 6, Dc = 1.699 g/cm3, m = 1.677 mm-1, F(000) = 1572, the final R = 0.0418 and wR = 0.1019 for 1805 independent reflections. 2 crystallizes in monoclinic, space group P21/c with a = 10.911(3), b = 9.783(2), c = 11.831(3) ? b = 100.28(2), V = 1242.6(6) ?, Z = 4, Dc = 1.941 g/cm3, m = 2.690 mm-1, F(000) = 720, the final R = 0.0280 and wR = 0.0627 for 2166 independent reflections. Both Sn4+ ions in these two complexes are six-coordinated with a slightly distorted octahedral configu- ration.
基金supported by the Natural Science Foundation of Zhejiang Province(LY19B020002)National Natural Science Foundation of China(21501124)+2 种基金Science&Technology Department of Sichuan Province(2018JY0235)Education Department of Sichuan Province(18ZA0337)Sichuan University of Science&Engineering(S201910622022)。
文摘In this paper,a novel diiron ethane-1,2-dithiolate complex[Fe2(CO)4{κ2-(Ph2P)2(1,2-C6H4)}(μ-SCH2CH2S)]has been prepared and structurally characterized.Treatment of the parent complex[Fe2(CO)6(μ-SCH2CH2S)]with 1 equivalent of 1,2-bis(diphenylphosphino)benzene and Me3NO?2H2O as the oxidative agent gave the title complex in good yield.The title complex has been characterized by elemental analysis,IR,1H NMR,31P{1H}NMR,13C{1H}NMR spectroscopy,and X-ray crystallography.X-ray crystal structure of the title complex contains a butterfly diiron cluster with a bridging ethane-1,2-dithiolate,four terminal carbonyls,and a chelating 1,2-bis(diphenylphosphino)benzene.In addition,electrochemical studies revealed that the title complex can catalyze the reduction of protons to H2 in the presence of acetic acid.
基金the National Natural Science Foundation of China (20425313)the Natural Science Foundation of Fujian Province (2005HZ01-1, 2006L2005, 2006F3135, 2006J0183)
文摘The reactions of Co（C1O4）2·6H2O and Co（NO3）2.6H2O with the di-Schiff base ligand N,N＇-bis-（1-benzimidazo-2-yl-ethylidene）-ethane-1,2-diamine （LA） in ethanol have been investigated. The reactions of LA with excess amount of cobalt salts yield the six-coordinate complexes [CoL2]（ClO4）E·H2O 1 and [CoL2]（NO3）E·H2O 2 as isolatable products （L= N-（1- benzimidazo-2-yl-ethylidene）-ethane-1,2-diamine）, where L is a tri-dentate mono-Schiff base ligand, resulting from the hydrolysis of the precursor di-Schiff base LA. Both complexes were characterized by X-ray crystallography. Crystal data for complex 1： monoclinic, space group P21/c, a = 11.9214（10）, b = 23.5828（17）, c = 14.0387（12）A, β = 135.219（4）°, C22H30Cl2CoN8O9, Mr = 680.37, V = 2780.1（4） A^3 ,Z = 4, Dc = 1.625 g/cm^3,μ（MoKa） = 0.876 mm^-1, F（000） = 1404, the final R = 0.0725 and wR = 0.1530 for 5726 observed reflections （I 〉 2σ（I））. Crystal data for complex 2： monoclinic, space group P21/c, a = 18.2162（16）, b = 10.0610（6）, c = 18.593（2）A, β = 130.099（3）°, C22H30CoN10O7, Mr = 605.49, V = 2606.5（4） A3 Z = 4, Dc = 1.543 g/cm^3,μ（MoKa） = 0.722 mm^-1, F（000） = 1260, the final R = 0.0619 and wR = 0.1429 for 5194 observed reflections （I 〉 2σ（I））. X-ray diffraction analysis reveals that each cobalt atom in the two complexes is chelated by six nitrogen atoms from two tridentate iigands L, exhibiting a slightly distorted octahedral coordination sphere. In both complexes, the strong hydrogen-bonding interactions between the lattice waters and N-H groups of the ligands result in 1D chains which are further connected by ClO4^- （or NO3^-） groups to form a 3D framework. In complex 2, the strong π-π interactions increase the stability of the structure.
文摘A novel carbazole photoinitiator 1-(6-o-chloro-benzoyl-9-ethyl-9H-carbazol-3yl)-ethane-1-one oxime O-ethyrate is synthesized from carbazole by N-alkylation,Friedel-Crafts acylation,oximation and esterification.The structure is characterized by 1HNMR,13CNMR,UV and IR.This paper discuss the catalyst,temperature and time of oximation and gain the optimum reaction conditions:CH3COOK is base,temperature is 70℃ and time is 6h.The yield is 89.1%.
文摘研究了p H以及表面活性剂对邻羟基苯基亚氨基乙二铵氟硼酸盐DJQ-45的光谱,发现p H对DJQ-45的光谱的影响具有可逆性;DJQ-45可以定量检测表面活性剂TX-100,当TX-100的浓度小于0.2 m M时,溶液的荧光强度下降的较为缓慢,当TX-100的浓度大于0.2 m M时,溶液的荧光强度急剧下降,当TX-100的浓度达到16 m M时,溶液的荧光光谱发生蓝移,蓝移了14 nm,强度急剧下降,当TX-100的浓度从25 m M到45 m M时,溶液的荧光强度基本保持不变。邻羟基苯基亚氨基乙二铵氟硼酸盐有希望被用做检测TX-100。
文摘Reaction of 4,4’-(1,4-phenylene)bis(5-acetyl-6-methyl-2-thioxo-1,2-dihydropyridine-3-carbonitrile) (1) with methyl iodide afforded the 4,4’-(1,4-phenylene)bis(5-acetyl-6-methyl-2-(methylthio)nicotinonitrile) (2). The reaction of 2 with hydrazine hydrate followed by diazotization reaction af-forded the 1,1’-(1,4-phenylenebis(3-amino-6-methyl-1H-pyrazolo[3,4-b]pyridine-4,5-diyl))bis(e-than-1-one) (3) and 1,1’-(1,4-phenylenebis(3-(chlorodiazenyl)-6-methyl-1H-pyrazolo[3,4-b]-pyridine-4,5-diyl))bis(ethan-1-one) (4) respectively. On the other hand, reaction of 4 with malononitrile, 2-cyanoethanethioamide, ethyl acetoacetate, acetyl acetone, ethyl benzoylacetate, diethylmalonate, ethyl cyanoacetate and phenacylbromide aiming to build up pyrazolotriazine or pyrazole ring on the ring system of 4. Structures of all newly synthesized heterocyclic compounds in the present study were confirmed by considering the data of IR, 1H NMR, mass spectra as well as that of elemental analyses.
