The complexes of four ferrocenylaldehyde aroylhydrazones with lead(Ⅱ) were synthesized and characterized. Their compositions, bonding forms and properties were researched by means of elemental analysis, IR, UV Vis,...The complexes of four ferrocenylaldehyde aroylhydrazones with lead(Ⅱ) were synthesized and characterized. Their compositions, bonding forms and properties were researched by means of elemental analysis, IR, UV Vis, 1H NMR spectra, thermal analysis and molar conductance. The free ligands which existed in the keto form coordinated to lead(Ⅱ) in the enol form to form neutral complexes. The molar ratio of the ligand to lead(Ⅱ) is 2∶1 and the thermal stability of the complex is higher than that of the corresponding ligand because of the formation of the stable chelate ring. The ligands and the complexes are all non electrolytes.展开更多
A 3-D coordination polymer [PbNH(CH2COO)2] 1 has been prepared under hydrothermal conditions and its crystal structure was studied by single-crystal X-ray diffraction. The compound belongs to orthorhombic system, spac...A 3-D coordination polymer [PbNH(CH2COO)2] 1 has been prepared under hydrothermal conditions and its crystal structure was studied by single-crystal X-ray diffraction. The compound belongs to orthorhombic system, space group Fdd2 with unit cell parameters: a = 13.6304(6), b = 36.295(1), c = 5.0821(2) ? V = 2514.19(17) 3, Z = 16, Mr = 338.28, Dc = 3.575 g/cm3, F(000) = 2400 and m(MoKa) = 2.679 cm-1. The final R and wR are 0.0290 and 0.0685, respectively, for 874 observed reflections with I > 2s(I). The lead has a distorted tetragonal pyramid environment with four oxygen donors in the basal plane and one nitrogen donor in the axial site. Micro-channels are observed in the neutral 3-D network of 1.展开更多
[Pb（TPT）（μ-I）2PbI2（μ-I）2Pb（TPT）] 1 （TPT is the abbreviation of 3,5,6-tris（2- pyridyl）-1,2,4-triazine ligand） has been synthesized and characterized by elemental analysis, IR, J H- NMR spectroscopy and st...[Pb（TPT）（μ-I）2PbI2（μ-I）2Pb（TPT）] 1 （TPT is the abbreviation of 3,5,6-tris（2- pyridyl）-1,2,4-triazine ligand） has been synthesized and characterized by elemental analysis, IR, J H- NMR spectroscopy and studied by thermal and electrochemical properties as well as X-ray crystallography. The single-crystal X-ray data show two different kinds of Pb2＋ ions in 1 with coordination numbers of six, Pbl = PbI6, and five, Pb2 = PbN312, with holodirected and hemidirected coordination spheres, respectively. The supramolecular features in 1 are negotiated through the weak but directional Pb...I, C-H...N and C-H...I interactions and aromatic π-π stacking interactions.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
The self-assembly of 1,10-phenanthroline（phen） and 1,3-benzenedicarboxylic acid（H2bdc） with Pb（NO3）2 under solvothermal conditions in N,N-dimethylacetamide（DMA） gives rise to a one-dimensional chain coordinati...The self-assembly of 1,10-phenanthroline（phen） and 1,3-benzenedicarboxylic acid（H2bdc） with Pb（NO3）2 under solvothermal conditions in N,N-dimethylacetamide（DMA） gives rise to a one-dimensional chain coordination polymer, [Pb（phen）（bdc）]（1）, which was characterized by elemental analysis, FT-IR and single-crystal X-ray diffraction. This complex crystallizes in triclinic, space group P1 with a = 7.5595（6）, b = 9.8199（8）, c = 13.1663（11） , α = 69.7590（10）, β = 80.6000（10）, γ = 71.3180（10）o, Z = 2, C20H12N2O4Pb, Mr = 551.51, Dc = 2.112 g/cm3, F（000） = 520 and μ = 9.757 mm-1. The final R = 0.0304 and wR = 0.0763 for 3427 observed reflections with I 〉 2σ（I） and R = 0.0365 and wR = 0.0894 for all data. The structure contains one crystallographic unique Pb（Ⅱ） atom, one phen molecule chelating with a Pb（Ⅱ） atom, and one bdc2- anion, acting as a bidentate bridging ligand linking the Pb（Ⅱ） atoms to form a one-dimensional structure. The two-dimensional layer and three-dimensional stacking structures are formed by C–H···O hydrogen bonding interactions. The thermal stable and fluorescent properties of 1 were investigated. PbO micro-crystal particles are produced by calcination of powder sample of complex 1. The obtained PbO is characterized and observed by XRD and SEM analyses.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
The indirect voltammetric determination of trace sulfate (2.0×10^(-6)～4.0×10^(-5) mol/L ) with the adsorptive complex wave of lead(Ⅱ)-tetrakis (4-trimethylammonium phenyl) porphyrin (PbTTMAPP) is reported....The indirect voltammetric determination of trace sulfate (2.0×10^(-6)～4.0×10^(-5) mol/L ) with the adsorptive complex wave of lead(Ⅱ)-tetrakis (4-trimethylammonium phenyl) porphyrin (PbTTMAPP) is reported.This method has been used for the analysis of natural waters with satisfactory results.展开更多
文摘The complexes of four ferrocenylaldehyde aroylhydrazones with lead(Ⅱ) were synthesized and characterized. Their compositions, bonding forms and properties were researched by means of elemental analysis, IR, UV Vis, 1H NMR spectra, thermal analysis and molar conductance. The free ligands which existed in the keto form coordinated to lead(Ⅱ) in the enol form to form neutral complexes. The molar ratio of the ligand to lead(Ⅱ) is 2∶1 and the thermal stability of the complex is higher than that of the corresponding ligand because of the formation of the stable chelate ring. The ligands and the complexes are all non electrolytes.
基金This work was supported by the State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter+1 种基金 Chinese Academy of Sciences (CAS) the Ministry of Science and Technology of China (001CB1089)
文摘A 3-D coordination polymer [PbNH(CH2COO)2] 1 has been prepared under hydrothermal conditions and its crystal structure was studied by single-crystal X-ray diffraction. The compound belongs to orthorhombic system, space group Fdd2 with unit cell parameters: a = 13.6304(6), b = 36.295(1), c = 5.0821(2) ? V = 2514.19(17) 3, Z = 16, Mr = 338.28, Dc = 3.575 g/cm3, F(000) = 2400 and m(MoKa) = 2.679 cm-1. The final R and wR are 0.0290 and 0.0685, respectively, for 874 observed reflections with I > 2s(I). The lead has a distorted tetragonal pyramid environment with four oxygen donors in the basal plane and one nitrogen donor in the axial site. Micro-channels are observed in the neutral 3-D network of 1.
基金Support of this investigation by Payame Noor University
文摘[Pb（TPT）（μ-I）2PbI2（μ-I）2Pb（TPT）] 1 （TPT is the abbreviation of 3,5,6-tris（2- pyridyl）-1,2,4-triazine ligand） has been synthesized and characterized by elemental analysis, IR, J H- NMR spectroscopy and studied by thermal and electrochemical properties as well as X-ray crystallography. The single-crystal X-ray data show two different kinds of Pb2＋ ions in 1 with coordination numbers of six, Pbl = PbI6, and five, Pb2 = PbN312, with holodirected and hemidirected coordination spheres, respectively. The supramolecular features in 1 are negotiated through the weak but directional Pb...I, C-H...N and C-H...I interactions and aromatic π-π stacking interactions.
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 Natural Science Foundation of Anhui Province(1208085MB31)University Student Creative Project of China(201310377022)
文摘The self-assembly of 1,10-phenanthroline（phen） and 1,3-benzenedicarboxylic acid（H2bdc） with Pb（NO3）2 under solvothermal conditions in N,N-dimethylacetamide（DMA） gives rise to a one-dimensional chain coordination polymer, [Pb（phen）（bdc）]（1）, which was characterized by elemental analysis, FT-IR and single-crystal X-ray diffraction. This complex crystallizes in triclinic, space group P1 with a = 7.5595（6）, b = 9.8199（8）, c = 13.1663（11） , α = 69.7590（10）, β = 80.6000（10）, γ = 71.3180（10）o, Z = 2, C20H12N2O4Pb, Mr = 551.51, Dc = 2.112 g/cm3, F（000） = 520 and μ = 9.757 mm-1. The final R = 0.0304 and wR = 0.0763 for 3427 observed reflections with I 〉 2σ（I） and R = 0.0365 and wR = 0.0894 for all data. The structure contains one crystallographic unique Pb（Ⅱ） atom, one phen molecule chelating with a Pb（Ⅱ） atom, and one bdc2- anion, acting as a bidentate bridging ligand linking the Pb（Ⅱ） atoms to form a one-dimensional structure. The two-dimensional layer and three-dimensional stacking structures are formed by C–H···O hydrogen bonding interactions. The thermal stable and fluorescent properties of 1 were investigated. PbO micro-crystal particles are produced by calcination of powder sample of complex 1. The obtained PbO is characterized and observed by XRD and SEM analyses.
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 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)。
文摘The indirect voltammetric determination of trace sulfate (2.0×10^(-6)～4.0×10^(-5) mol/L ) with the adsorptive complex wave of lead(Ⅱ)-tetrakis (4-trimethylammonium phenyl) porphyrin (PbTTMAPP) is reported.This method has been used for the analysis of natural waters with satisfactory results.
