A robust voltammetric method has been developed and validated for the determination of Fe（Ⅱ） and Fe（Ⅲ） in pharmaceutical iron polysaccharidic complexes. Undesirable low molecular weight iron complexes, at concen...A robust voltammetric method has been developed and validated for the determination of Fe（Ⅱ） and Fe（Ⅲ） in pharmaceutical iron polysaccharidic complexes. Undesirable low molecular weight iron complexes, at concentration about 3% in the pharmaceutical formulation, can be easily determined with good accuracy and precision. This methodology can be proposed as a viable, environmentally sustainable substitute for the conventional Normal Pulse Polarographic method in US Pharmacopeia, with better analytical figures of merit, and reduced Hg consumption. A deeper insight in Fe（Ⅱ） and Fe（Ⅲ） composition can be gained by the combined use of a new potentiometric technique after chemical decomposition of the complex.展开更多
An iron（Ⅱ） coordination polymer, [Fe（Haip）2（H2O）2]n （1, Haip = 5-ammoniumiso- phthalato）, has been hydro/solvothermally synthesized and characterized by single-crystal X-ray diffraction, elemental analysis, i...An iron（Ⅱ） coordination polymer, [Fe（Haip）2（H2O）2]n （1, Haip = 5-ammoniumiso- phthalato）, has been hydro/solvothermally synthesized and characterized by single-crystal X-ray diffraction, elemental analysis, infrared spectrum and magnetic measurement. Compound 1 crystalizes in monoclinic, space group P2/c with a = 6.9874（14）, b = 9.960（2）, c = 12.894（4） A, β = 117.47（2）°, Fe（C8H6NO4）2（H2O）2, Mr = 452.16, V= 796.2（3） A3, Z = 2, Dc = 1.886 g.cm-3, p = 1.017 mm-1, F（000） = 464.0, 2.71〈0〈28.42°, R = 0.0307, wR = 0.0840 and S = 1.005. Single-crystal X-ray diffraction analysis reveals that 1 features an infinite one-dimensional loop-like chain structure and Haip ligand in 1 is of zwitterionic form. Magnetic measurement results show the dominated ferromagnetic interactions among Fe11 atoms.展开更多
Oxidation of alkybenzenes PhCH_2R(R=H, CH_3, C_2H_5 and n-C_3H_7) under 1 atm. of O_2 or air catalyzed by iron(Ⅱ, Ⅲ)-2,2'-bipyridine and 1,10-phenanthroline complexes, affords the aryl-substituted ketones and al...Oxidation of alkybenzenes PhCH_2R(R=H, CH_3, C_2H_5 and n-C_3H_7) under 1 atm. of O_2 or air catalyzed by iron(Ⅱ, Ⅲ)-2,2'-bipyridine and 1,10-phenanthroline complexes, affords the aryl-substituted ketones and alcohols with the conversion of 15.00％～34.58％ containing of 97.60％～99.80％ ketones and alcohols. The turnover numbers of these catalysts are over 3500 mol-cat. ^(-1)for 3.5 h.展开更多
An unsymmetric 2,6-bis(imino)pyridine iron(II) complex 1' was synthesized. The relationship between catalyststructure and its activity in ethylene polymerization is discussed. The kinetic behavior of ethylene poly...An unsymmetric 2,6-bis(imino)pyridine iron(II) complex 1' was synthesized. The relationship between catalyststructure and its activity in ethylene polymerization is discussed. The kinetic behavior of ethylene polymerization and theeffects of polymerization conditions such as temperature, aluminum/iron molar ratio on the activity of catalyst and thecharacteristics of polyethylene were reported. The unsymmetric catalyst 1' has a good catalytic performance of 3.47×10~6 gPE·mol^(-1)·Fe·h^(-1) at 40℃ with aluminum/iron molar ratio = 2500. A dependence of catalyst activity on themethylaluminoxane (MAO) concentration and reaction temperature was found. The molecular weight (MW) of polyethylenewith broad dispersity is about 10~4-10~5 g/mol. The melting temperature and branching of polyethylenes vary with changingreaction temperature and aluminum/iron molar ratio.展开更多
Two new coordination polymers,[Ni(Hpdc)(bib)(H_(2)O)]_(n)(1)and{[Ni(bib)_(3)](ClO_(4))_(2)}_(n)(2),were prepared by mixing Ni^(2+),3,5⁃pyrazoledicarboxylic acid(H3pdc)/p⁃nitrobenzoic acid and 1,4⁃bis(imidazol⁃1⁃ylmeth...Two new coordination polymers,[Ni(Hpdc)(bib)(H_(2)O)]_(n)(1)and{[Ni(bib)_(3)](ClO_(4))_(2)}_(n)(2),were prepared by mixing Ni^(2+),3,5⁃pyrazoledicarboxylic acid(H3pdc)/p⁃nitrobenzoic acid and 1,4⁃bis(imidazol⁃1⁃ylmethyl)butane(bib)by a hydrothermal method,respectively.X⁃ray crystallography reveals a 2D network constructed by six⁃coordinated Ni(Ⅱ)centers,bib,and Hpdc2-ligands in complex 1,while a 2D network is built by Ni(Ⅱ)and bib ligands in 2.Furthermore,the quantum⁃chemical calculations have been performed on‘molecular fragments’extracted from the crystal structure of 1 using the PBE0/LANL2DZ method in Gaussian 16 and the VASP program.CCDC:2343794,1;2343798,2.展开更多
One new three-dimensional polymeric PbⅡ complex,[Pb3(CTA)2(H2 O)2]n·nH2O(1),(H3 CTA = cis,cis-1,3,5-cyclohexanetricarboxylic acid), has been synthesized. Single-crystal X-ray diffraction analyses reveal that com...One new three-dimensional polymeric PbⅡ complex,[Pb3(CTA)2(H2 O)2]n·nH2O(1),(H3 CTA = cis,cis-1,3,5-cyclohexanetricarboxylic acid), has been synthesized. Single-crystal X-ray diffraction analyses reveal that complex 1 has a three-dimensional architecture consisting of Pb2O2 dimeric building units, which shows two types of PbⅡ centers(eight-coordinated Pb(1),six-coordinated Pb(2) and Pb(3)). The eight-coordinated Pb(1) center possesses a stereochemically ‘inactive’ electron lone pair, and the coordination sphere is holodirected. However, the arrangement of oxygen atoms around Pb(2) and Pb(3) suggests a gap or hole in the coordination geometry. The stereo-chemically ‘active’ electron lone pairs of Pb(2) and Pb(3) possibly occupy these ‘holes’ and their coordination spheres are hemidirected. Its properties have been determined by FT-IR spectra, elemental analyses and thermogravimetric analyses(TGA). Solid-state luminescent properties of 1 also have been determined, indicating strong fluorescent emissions.展开更多
基金supported by FAR, Fondo Ateneoper la Ricerca Universitá di Pavia,Italy
文摘A robust voltammetric method has been developed and validated for the determination of Fe（Ⅱ） and Fe（Ⅲ） in pharmaceutical iron polysaccharidic complexes. Undesirable low molecular weight iron complexes, at concentration about 3% in the pharmaceutical formulation, can be easily determined with good accuracy and precision. This methodology can be proposed as a viable, environmentally sustainable substitute for the conventional Normal Pulse Polarographic method in US Pharmacopeia, with better analytical figures of merit, and reduced Hg consumption. A deeper insight in Fe（Ⅱ） and Fe（Ⅲ） composition can be gained by the combined use of a new potentiometric technique after chemical decomposition of the complex.
基金supported by the Scientific Research Start-up Funds of Shangrao Normal Universitythe Fourth Characteristic Specialty Foundation of University from Ministry of Education(TS11524)the Natural Science Foundation of Jiangxi Province(No.20122BAB203002)
文摘An iron（Ⅱ） coordination polymer, [Fe（Haip）2（H2O）2]n （1, Haip = 5-ammoniumiso- phthalato）, has been hydro/solvothermally synthesized and characterized by single-crystal X-ray diffraction, elemental analysis, infrared spectrum and magnetic measurement. Compound 1 crystalizes in monoclinic, space group P2/c with a = 6.9874（14）, b = 9.960（2）, c = 12.894（4） A, β = 117.47（2）°, Fe（C8H6NO4）2（H2O）2, Mr = 452.16, V= 796.2（3） A3, Z = 2, Dc = 1.886 g.cm-3, p = 1.017 mm-1, F（000） = 464.0, 2.71〈0〈28.42°, R = 0.0307, wR = 0.0840 and S = 1.005. Single-crystal X-ray diffraction analysis reveals that 1 features an infinite one-dimensional loop-like chain structure and Haip ligand in 1 is of zwitterionic form. Magnetic measurement results show the dominated ferromagnetic interactions among Fe11 atoms.
文摘Oxidation of alkybenzenes PhCH_2R(R=H, CH_3, C_2H_5 and n-C_3H_7) under 1 atm. of O_2 or air catalyzed by iron(Ⅱ, Ⅲ)-2,2'-bipyridine and 1,10-phenanthroline complexes, affords the aryl-substituted ketones and alcohols with the conversion of 15.00％～34.58％ containing of 97.60％～99.80％ ketones and alcohols. The turnover numbers of these catalysts are over 3500 mol-cat. ^(-1)for 3.5 h.
基金This work was financially supported by the National Natural Science Foundation of China (No. 29734141, 50103012) Core Research for Engineering Innovation KGCX2-203, the Foundation of "One Hundred Talents" program for W-H Sun, Chinese Academy of Sciences
文摘An unsymmetric 2,6-bis(imino)pyridine iron(II) complex 1' was synthesized. The relationship between catalyststructure and its activity in ethylene polymerization is discussed. The kinetic behavior of ethylene polymerization and theeffects of polymerization conditions such as temperature, aluminum/iron molar ratio on the activity of catalyst and thecharacteristics of polyethylene were reported. The unsymmetric catalyst 1' has a good catalytic performance of 3.47×10~6 gPE·mol^(-1)·Fe·h^(-1) at 40℃ with aluminum/iron molar ratio = 2500. A dependence of catalyst activity on themethylaluminoxane (MAO) concentration and reaction temperature was found. The molecular weight (MW) of polyethylenewith broad dispersity is about 10~4-10~5 g/mol. The melting temperature and branching of polyethylenes vary with changingreaction temperature and aluminum/iron molar ratio.
文摘Two new coordination polymers,[Ni(Hpdc)(bib)(H_(2)O)]_(n)(1)and{[Ni(bib)_(3)](ClO_(4))_(2)}_(n)(2),were prepared by mixing Ni^(2+),3,5⁃pyrazoledicarboxylic acid(H3pdc)/p⁃nitrobenzoic acid and 1,4⁃bis(imidazol⁃1⁃ylmethyl)butane(bib)by a hydrothermal method,respectively.X⁃ray crystallography reveals a 2D network constructed by six⁃coordinated Ni(Ⅱ)centers,bib,and Hpdc2-ligands in complex 1,while a 2D network is built by Ni(Ⅱ)and bib ligands in 2.Furthermore,the quantum⁃chemical calculations have been performed on‘molecular fragments’extracted from the crystal structure of 1 using the PBE0/LANL2DZ method in Gaussian 16 and the VASP program.CCDC:2343794,1;2343798,2.
基金supported by the Fundamental Research Funds for the Central Universities(No.3122017071)Training Program of Innovation and Entrepreneurship for Undergraduates(No.201710059010)+1 种基金Open Project of Tianjin Key Lab Struct.&Performance Funct Mol(Tianjin Normal Univ.)National Natural Science Foundation of China(No.21501196)
文摘One new three-dimensional polymeric PbⅡ complex,[Pb3(CTA)2(H2 O)2]n·nH2O(1),(H3 CTA = cis,cis-1,3,5-cyclohexanetricarboxylic acid), has been synthesized. Single-crystal X-ray diffraction analyses reveal that complex 1 has a three-dimensional architecture consisting of Pb2O2 dimeric building units, which shows two types of PbⅡ centers(eight-coordinated Pb(1),six-coordinated Pb(2) and Pb(3)). The eight-coordinated Pb(1) center possesses a stereochemically ‘inactive’ electron lone pair, and the coordination sphere is holodirected. However, the arrangement of oxygen atoms around Pb(2) and Pb(3) suggests a gap or hole in the coordination geometry. The stereo-chemically ‘active’ electron lone pairs of Pb(2) and Pb(3) possibly occupy these ‘holes’ and their coordination spheres are hemidirected. Its properties have been determined by FT-IR spectra, elemental analyses and thermogravimetric analyses(TGA). Solid-state luminescent properties of 1 also have been determined, indicating strong fluorescent emissions.
基金supported by the National Natural Science Foundation of China(No.21973086,No.22203083)the Ministry of Science and Technology of China(No.2021YFA1200103)the Fundamental Research Funds for the Central Universities(No.WK2060000018)。
