Oxidation-reduction properties of some Fe-S and Mo-Fe-S clusters have been studied by cyclic voltammetric measurement. It is indicated that there are some factors which affect the oxidation- reduction properties of cl...Oxidation-reduction properties of some Fe-S and Mo-Fe-S clusters have been studied by cyclic voltammetric measurement. It is indicated that there are some factors which affect the oxidation- reduction properties of clusters, of which are charge density of metal atom in cluster core, electron effect of ligands, charge and geometric configurations of the reactant particle, etc.展开更多
The characteristic studies, by means of LR, UV-Vis and XPS spectroscopies, of the preparation process of Mo-Co-S and Mo-Fe-S catalysts for HDS and HDN, derived from (NH4)2MoS4-CoCl2 and (NH4)2MoS4-FeCl2 complexes supp...The characteristic studies, by means of LR, UV-Vis and XPS spectroscopies, of the preparation process of Mo-Co-S and Mo-Fe-S catalysts for HDS and HDN, derived from (NH4)2MoS4-CoCl2 and (NH4)2MoS4-FeCl2 complexes supported on γ-Al2O3, respectively, indicate that the catalytically essential moiety on the surface of the catalysts is dominantly some sulfido-bimetallic species with such a structural unit (M' =Co or Fe), and both Co and Fe, served as promoters, can donate electrons to Mo probably via bridging-S. The nature of active-sites and the mechanism of promotion are discussed according to the results.展开更多
Reaction of [Mo3(CO)7(S,O-C6H4-1,2)3]2- with FeCl2 in MeCN at 60℃ affords a new Mo-Fe-S cluster complex containing MoO3S3 unit and mixed-valeut Mo atoms, [Et4N]2[Mo2Fe-(CO)4(O,S-C6H4-1,2)aCl2] (1). 1 is characterized...Reaction of [Mo3(CO)7(S,O-C6H4-1,2)3]2- with FeCl2 in MeCN at 60℃ affords a new Mo-Fe-S cluster complex containing MoO3S3 unit and mixed-valeut Mo atoms, [Et4N]2[Mo2Fe-(CO)4(O,S-C6H4-1,2)aCl2] (1). 1 is characterized by elemental analysis, IR, Mossbauer spectra, X-ray photoelectron spectra and mass spectra. And the structure of 1 is suggested as the structure which contains a [Mo(S,O-C6H4-1,2)3] unit of which the two of three sulfur atoms link to a Mo(CO)4-moiety and the three oxygen atoms are coordinated to a FeCl2 ligand.展开更多
The reaction system of [Et4N]2MoSe4, FeCI2 and R2NCS2Na in DMF-CH3CN at ambient temperature yielded the Mo-Fe-Se cluster compounds MoFe3Se4(μ-R2NCS2)2(R2NCS2)4 (R2=Me2(1), Et2(2), C4H8(3)) with MoFe3Se4 core. X-ray d...The reaction system of [Et4N]2MoSe4, FeCI2 and R2NCS2Na in DMF-CH3CN at ambient temperature yielded the Mo-Fe-Se cluster compounds MoFe3Se4(μ-R2NCS2)2(R2NCS2)4 (R2=Me2(1), Et2(2), C4H8(3)) with MoFe3Se4 core. X-ray diffraction analyses of 2 revealed that the molecular structure contains a distorted cubane like M4Se4 core with two bridged and four chelated Et2NCS2- ligands. The cyclic voltammetric studies of the compounds showed the reversible mul-tielectron-transfer sequence.展开更多
目的通过电感耦合等离子体质谱(inductively coupled plasma mass spectrometry,ICP-MS)法建立加味左金丸中Cd、Pb、As、Hg、Co、V、Ni、Cu、Li、Sb、Ba、Mo、Sn、Cr、Na、Mg、Al、Ca、Ti、Mn、Fe、Zn、Ga、Se、Sr、Tl共计26种无机元素...目的通过电感耦合等离子体质谱(inductively coupled plasma mass spectrometry,ICP-MS)法建立加味左金丸中Cd、Pb、As、Hg、Co、V、Ni、Cu、Li、Sb、Ba、Mo、Sn、Cr、Na、Mg、Al、Ca、Ti、Mn、Fe、Zn、Ga、Se、Sr、Tl共计26种无机元素的测定方法。方法加味左金丸通过微波消解法处理后,根据相对分子质量的大小选择内标物,其中^(7)Li、^(23)Na、^(24)Mg、^(27)Al、^(40)Ca、^(48)Ti、^(51)V、^(52)Cr、^(55)Mn、^(56)Fe、^(58)Ni、^(59)Co、^(63)Cu、^(66)Zn、^(70)Ga、^(75)As、^(77)Se、^(86)Sr以^(72)Ge作为内标;^(95)Mo、^(114)Cd、^(118)Sn、^(121)Sb、^(137)Ba以^(115)In作为内标;^(202)Hg、^(205)Tl、^(208)Pb以^(209)Bi作为内标。对标准品溶液、空白溶液与供试品溶液进行分析,采用标准曲线法进行定量分析。通过ICP-MS法进行测定。结果26种无机元素线性的相关系数r≥0.9996,检出限为0.001~1.500μg/L,定量限为0.01~5.00μg/L,精密度与重复性试验的RSD均小于5%,平均回收率在82.64%~106.44%,RSD均小于5%。对3个厂家的12批样品进行了测定,26种元素的含量差异较大,其中Na、Mg、Ca、Fe 4种元素的含量比较高,均大于500μg/g,Cd、Pb、As、Hg、Co、Li、Sb、Mo、Sn、Cr、Se、Tl的含量比较低,均小于1μg/g。由结果可知,人体的常量元素,如Na、Mg、Ca的含量比较高,Cd、Pb、As、Hg等有害元素含量比较低。根据《中国药典》2020年版一部的要求,本品中Cd、Pb、As、Hg与Cu均符合规定。结论该方法快速、准确,可以用于加味左金丸中无机元素的测定。展开更多
Three types of unit combinations, FeS2Fe + FeS2Fe, FeS2Fe + MoS2Fe and MoS2Mo + MoS2Mo, lead to Fe4S4, MoFe3S4 and Mo2Fe2S4 cubane-like clusters, respectively. A new doubly bridged single cubane cluster [Mo2Fe2S4(C4H8...Three types of unit combinations, FeS2Fe + FeS2Fe, FeS2Fe + MoS2Fe and MoS2Mo + MoS2Mo, lead to Fe4S4, MoFe3S4 and Mo2Fe2S4 cubane-like clusters, respectively. A new doubly bridged single cubane cluster [Mo2Fe2S4(C4H8dtc)6]·3.5C2H2Cl4 has been obtained and its structure is discussed.展开更多
文摘Oxidation-reduction properties of some Fe-S and Mo-Fe-S clusters have been studied by cyclic voltammetric measurement. It is indicated that there are some factors which affect the oxidation- reduction properties of clusters, of which are charge density of metal atom in cluster core, electron effect of ligands, charge and geometric configurations of the reactant particle, etc.
基金Supported by the National Natural Science Foundation of China
文摘The characteristic studies, by means of LR, UV-Vis and XPS spectroscopies, of the preparation process of Mo-Co-S and Mo-Fe-S catalysts for HDS and HDN, derived from (NH4)2MoS4-CoCl2 and (NH4)2MoS4-FeCl2 complexes supported on γ-Al2O3, respectively, indicate that the catalytically essential moiety on the surface of the catalysts is dominantly some sulfido-bimetallic species with such a structural unit (M' =Co or Fe), and both Co and Fe, served as promoters, can donate electrons to Mo probably via bridging-S. The nature of active-sites and the mechanism of promotion are discussed according to the results.
基金Project supported by the National Natural Science Foundation of China.
文摘Reaction of [Mo3(CO)7(S,O-C6H4-1,2)3]2- with FeCl2 in MeCN at 60℃ affords a new Mo-Fe-S cluster complex containing MoO3S3 unit and mixed-valeut Mo atoms, [Et4N]2[Mo2Fe-(CO)4(O,S-C6H4-1,2)aCl2] (1). 1 is characterized by elemental analysis, IR, Mossbauer spectra, X-ray photoelectron spectra and mass spectra. And the structure of 1 is suggested as the structure which contains a [Mo(S,O-C6H4-1,2)3] unit of which the two of three sulfur atoms link to a Mo(CO)4-moiety and the three oxygen atoms are coordinated to a FeCl2 ligand.
文摘The reaction system of [Et4N]2MoSe4, FeCI2 and R2NCS2Na in DMF-CH3CN at ambient temperature yielded the Mo-Fe-Se cluster compounds MoFe3Se4(μ-R2NCS2)2(R2NCS2)4 (R2=Me2(1), Et2(2), C4H8(3)) with MoFe3Se4 core. X-ray diffraction analyses of 2 revealed that the molecular structure contains a distorted cubane like M4Se4 core with two bridged and four chelated Et2NCS2- ligands. The cyclic voltammetric studies of the compounds showed the reversible mul-tielectron-transfer sequence.
基金Project supported by the National Natural Science Foundation of Chinathe Science Foundation of Chinese Academy of Sciences.
文摘Three types of unit combinations, FeS2Fe + FeS2Fe, FeS2Fe + MoS2Fe and MoS2Mo + MoS2Mo, lead to Fe4S4, MoFe3S4 and Mo2Fe2S4 cubane-like clusters, respectively. A new doubly bridged single cubane cluster [Mo2Fe2S4(C4H8dtc)6]·3.5C2H2Cl4 has been obtained and its structure is discussed.
