The crystal of zinc complex with salicylaldehyde salicylhydrazone(SHSH ) was obtained in DMF and pyridine. It has been characterized by IR, UV, element analysis and X-ray diffraction analysis. The crystallographic dat...The crystal of zinc complex with salicylaldehyde salicylhydrazone(SHSH ) was obtained in DMF and pyridine. It has been characterized by IR, UV, element analysis and X-ray diffraction analysis. The crystallographic data were as foll ows: monoclinic system, space group Pn, a=1.094 6 nm, b=0.884 0 nm, c=1.161 0 nm , 穋m-3, ≥2 The X-ray crystal structure analysis revealed that the center zinc(Ⅱ) is bonded to two oxygen atoms and one nitrogen atoms from a tridentate ligand(SHSH) and two nitrogen atoms from two solvent pyridine molecules to form a five-coord inate distorted trigonal bipyramid. The full-optimized molecular geometries of t itle complex was calculated at B3LYP/6-31G and HF/6-31G levels with Guassian 98W program. CCDC: 252832.展开更多
The crystal of binuclear zinc complex Zn2(dhaash)2(py)4 was obtained in DMF and pyridine, where H2dhaash is 2,4-dihydroxy-5-acetylacetophenone-N-salicylhydrazone. It has been characterized by IR, UV, element analysis ...The crystal of binuclear zinc complex Zn2(dhaash)2(py)4 was obtained in DMF and pyridine, where H2dhaash is 2,4-dihydroxy-5-acetylacetophenone-N-salicylhydrazone. It has been characterized by IR, UV, element analysis and X-ray single crystal diffraction. The crystallographic data were as follows: monoclinic system, space group P21 / c, a=1.108 98(11) nm, b=1.640 84(16) nm, c=1.445 14(14) nm, β=108.617(2)°, Z=2, V=2.492 1(4) nm3, Dc=1.466 g·cm-3, Mr=1 099.74, μ=1.031 mm-1, F(000)=1 136 and the final R=0.044 8 and wR=0.105 8 for 4 143 observed reflections with I≥2σ(I), respectively. The X-ray crystal structure analysis revealed that, in the centrosymmetric binuclear complex molecule, two zinc髤 centers are linked by two oxygen atoms (O(3) and O(3A)), respectively. Zn(1)...Zn(1A) distance is 0.314 81(6) nm, O(3)...O(3A) distance is 0.270 4(2) nm. Every zinc髤 ion has an elongated octahedral coordination. For example, the two pyridine nitrogen atoms, one oxygen atom and one nitrogen atom from salicylhydrazone, one oxygen atom from 2,4-dihydroxy-5-acetylacetophenone in one dhaash2- ligand and one oxygen atom from 2,4-dihydroxy-5-acetylacetophenone in another dhaash2- ligand coordinated to zinc髤 ion, respectively. Two zinc髤 ions and all the 72 non-hydrogen atoms in the two dhaash2- ligands are in the same plane. CCDC: 261929.展开更多
The title complex, C24H18Br2N4ZnO3, has been prepared and characterized by X- ray diffraction analysis. It crystallizes in the triclinic system, space group PI^- with α = 0.89000（11）, b = 1.22172（14）, c= 1.31342...The title complex, C24H18Br2N4ZnO3, has been prepared and characterized by X- ray diffraction analysis. It crystallizes in the triclinic system, space group PI^- with α = 0.89000（11）, b = 1.22172（14）, c= 1.31342（16）nm, a = 101.696（2）, β = 103.519（2）, γ = 110.744（2）°, V= 1.2329（3） nm^3, Z = 2, Mr = 635.61, F（000） = 628, Dc= 1.712 g/cm^3 and μ（MoKa） = 4.270 mm^-1. The structure was refined to the final R = 0.0524 and wR = 0.1239 for 2763 observed reflections with I 〉 2σ（ I）. The X-ray crystal structure analysis revealed that the center zinc（Ⅱ） is bonded with two oxygen and one nitrogen atoms from a tridentate ligand 3,5-dibromo-salicylaldehyde salicyloylhydrazone （DBSHSH） and two nitrogen atoms from two solvent pyridine molecules to form a distorted five-coordinate trigonal bipyramid. The intramolecular hydrogen bonds in the crystal structure play an important role in the title complex＇s thermostability.展开更多
The title complex was prepared from self-assembly reaction of La（NO3）3(6H2O, Zn（NO3）2(6H2O, m-cyanobenzoic acid （m-CNC6H4COOH） and pyridine （Py） in refluxing ethanol and its structure was determined by single-...The title complex was prepared from self-assembly reaction of La（NO3）3(6H2O, Zn（NO3）2(6H2O, m-cyanobenzoic acid （m-CNC6H4COOH） and pyridine （Py） in refluxing ethanol and its structure was determined by single-crystal X-ray diffraction. Crystallographic data: C94H62N12La2O22Zn2, Mr = 2120.12, triclinic space group P, a = 13.2219（5）, b = 13.2713（5）, c = 14.1987（6） ?, (???69.156（1）, ( = 84.034（1）, ( = 89.400（1） (, V = 2314.9（2） ?3, Z = 1, Dc = 1.521 g/cm3, F（000） = 1060, ( (MoK（） = 14.94 cm－1, the final R = 0.043 and wR = 0.117 for 6381 unique reflections with I > 2(（I）. Crystal structure determination shows that the neighboring lanthanum（III） and zinc（II） ions are bridged by three bidentate m-cyanobenzonate ligands in the syn-syn fashion to form a pair of dinuclear [LaZn（m-CNC6H4COO）3（Py）（C2H5OH）] subunits, being linked together by two bidentate and two tridentate m-cyanobenzonate groups in the syn-syn and syn-anti modes, respectively, to construct a tetranuclear La-Zn complex [La2Zn2（m-CNC6H4COO）10（Py）2（C2H5OH）2].展开更多
A new dicopper(II) compound with oxalate and reduced imino nitroxide radicals [Cu2(m-C2O4)(Him2-py)2(H2O)2](NO3)2 (Him2-py=1-hydroxy-2-(2-pyridyl)-4,4,5,5-tetramethyli- midazoline) has been synthesized and its crystal...A new dicopper(II) compound with oxalate and reduced imino nitroxide radicals [Cu2(m-C2O4)(Him2-py)2(H2O)2](NO3)2 (Him2-py=1-hydroxy-2-(2-pyridyl)-4,4,5,5-tetramethyli- midazoline) has been synthesized and its crystal structure was determined by X-ray diffraction method. The complex crystallizes in monoclinic, space group P21/n with a = 9.913(4), b = 19.057(8), c = 10.169(4) ? b = 114.292(7), V = 1751(1) 3, C26H38Cu2N8O14, Mr = 813.72, Dc = 1.543 g/cm3, m(MoKa) = 1.290 mm-1, F(000) = 840, Z = 2, the final R = 0.0398 and wR = 0.0986 for 1878 observed reflections (I>2s(I)). The imino nitroxide 2-(2-pyridyl)-4,4,5,5-tetramethyl- imidazoline-1-oxyl (im2-py) is reduced in the reaction to yield Him2-py which consists of oxalato-bridged centrosymmetric [Cu2(m-C2O4)(Him2-py)2(H2O)2]2+ ions and noncoordinated NO3- anions. Each copper(II) ion is in a distorted tetragonal pyramid environment: two nitrogen atoms from Him2-py and two oxygen atoms from the oxalate group are in the basal plane, and one water molecule at the axial position.展开更多
利用热裂解-气相色谱质谱联用(pyrolysis gas chromatography mass spectrometry,Py-GC/MS)分析技术测定黑木耳新品种‘农黑2号’黑色素裂解产物组分的种类及含量,为解析黑色素的结构奠定理论基础。本研究通过碱溶酸沉法提取黑色素,并...利用热裂解-气相色谱质谱联用(pyrolysis gas chromatography mass spectrometry,Py-GC/MS)分析技术测定黑木耳新品种‘农黑2号’黑色素裂解产物组分的种类及含量,为解析黑色素的结构奠定理论基础。本研究通过碱溶酸沉法提取黑色素,并用紫外可见吸收光谱、傅立叶红外光谱、有机元素分析鉴定黑色素,采用Py-GC/MS技术分析其热裂解产物。结果表明,‘农黑2号’黑色素的最大吸收峰值在波长220 nm处,傅立叶红外光谱符合典型的黑色素特征;经有机元素分析,C、H、N、O元素的含量分别为43.47%、5.24%、11.71%和39.58%,不含硫元素,为真黑色素;检出的热裂解产物主要有苯类、苯酚类、吲哚类、苯基腈类、烃类、酸类等物质,其中苯、苯酚、吲哚等化合物为真黑色素的裂解产物。综上所述,‘农黑2号’黑色素为真黑色素,其基本骨架为苯环和吲哚,本研究为精准解析黑木耳黑色素结构提供科学依据。展开更多
文摘The crystal of zinc complex with salicylaldehyde salicylhydrazone(SHSH ) was obtained in DMF and pyridine. It has been characterized by IR, UV, element analysis and X-ray diffraction analysis. The crystallographic data were as foll ows: monoclinic system, space group Pn, a=1.094 6 nm, b=0.884 0 nm, c=1.161 0 nm , 穋m-3, ≥2 The X-ray crystal structure analysis revealed that the center zinc(Ⅱ) is bonded to two oxygen atoms and one nitrogen atoms from a tridentate ligand(SHSH) and two nitrogen atoms from two solvent pyridine molecules to form a five-coord inate distorted trigonal bipyramid. The full-optimized molecular geometries of t itle complex was calculated at B3LYP/6-31G and HF/6-31G levels with Guassian 98W program. CCDC: 252832.
文摘The crystal of binuclear zinc complex Zn2(dhaash)2(py)4 was obtained in DMF and pyridine, where H2dhaash is 2,4-dihydroxy-5-acetylacetophenone-N-salicylhydrazone. It has been characterized by IR, UV, element analysis and X-ray single crystal diffraction. The crystallographic data were as follows: monoclinic system, space group P21 / c, a=1.108 98(11) nm, b=1.640 84(16) nm, c=1.445 14(14) nm, β=108.617(2)°, Z=2, V=2.492 1(4) nm3, Dc=1.466 g·cm-3, Mr=1 099.74, μ=1.031 mm-1, F(000)=1 136 and the final R=0.044 8 and wR=0.105 8 for 4 143 observed reflections with I≥2σ(I), respectively. The X-ray crystal structure analysis revealed that, in the centrosymmetric binuclear complex molecule, two zinc髤 centers are linked by two oxygen atoms (O(3) and O(3A)), respectively. Zn(1)...Zn(1A) distance is 0.314 81(6) nm, O(3)...O(3A) distance is 0.270 4(2) nm. Every zinc髤 ion has an elongated octahedral coordination. For example, the two pyridine nitrogen atoms, one oxygen atom and one nitrogen atom from salicylhydrazone, one oxygen atom from 2,4-dihydroxy-5-acetylacetophenone in one dhaash2- ligand and one oxygen atom from 2,4-dihydroxy-5-acetylacetophenone in another dhaash2- ligand coordinated to zinc髤 ion, respectively. Two zinc髤 ions and all the 72 non-hydrogen atoms in the two dhaash2- ligands are in the same plane. CCDC: 261929.
基金The project was supported by the Natural Science Education of Hubei Province (No. 2001A27006)
文摘The title complex, C24H18Br2N4ZnO3, has been prepared and characterized by X- ray diffraction analysis. It crystallizes in the triclinic system, space group PI^- with α = 0.89000（11）, b = 1.22172（14）, c= 1.31342（16）nm, a = 101.696（2）, β = 103.519（2）, γ = 110.744（2）°, V= 1.2329（3） nm^3, Z = 2, Mr = 635.61, F（000） = 628, Dc= 1.712 g/cm^3 and μ（MoKa） = 4.270 mm^-1. The structure was refined to the final R = 0.0524 and wR = 0.1239 for 2763 observed reflections with I 〉 2σ（ I）. The X-ray crystal structure analysis revealed that the center zinc（Ⅱ） is bonded with two oxygen and one nitrogen atoms from a tridentate ligand 3,5-dibromo-salicylaldehyde salicyloylhydrazone （DBSHSH） and two nitrogen atoms from two solvent pyridine molecules to form a distorted five-coordinate trigonal bipyramid. The intramolecular hydrogen bonds in the crystal structure play an important role in the title complex＇s thermostability.
基金the Natural Science Foundation of China, Fujian Province and Chinese Academy of Sciences.
文摘The title complex was prepared from self-assembly reaction of La（NO3）3(6H2O, Zn（NO3）2(6H2O, m-cyanobenzoic acid （m-CNC6H4COOH） and pyridine （Py） in refluxing ethanol and its structure was determined by single-crystal X-ray diffraction. Crystallographic data: C94H62N12La2O22Zn2, Mr = 2120.12, triclinic space group P, a = 13.2219（5）, b = 13.2713（5）, c = 14.1987（6） ?, (???69.156（1）, ( = 84.034（1）, ( = 89.400（1） (, V = 2314.9（2） ?3, Z = 1, Dc = 1.521 g/cm3, F（000） = 1060, ( (MoK（） = 14.94 cm－1, the final R = 0.043 and wR = 0.117 for 6381 unique reflections with I > 2(（I）. Crystal structure determination shows that the neighboring lanthanum（III） and zinc（II） ions are bridged by three bidentate m-cyanobenzonate ligands in the syn-syn fashion to form a pair of dinuclear [LaZn（m-CNC6H4COO）3（Py）（C2H5OH）] subunits, being linked together by two bidentate and two tridentate m-cyanobenzonate groups in the syn-syn and syn-anti modes, respectively, to construct a tetranuclear La-Zn complex [La2Zn2（m-CNC6H4COO）10（Py）2（C2H5OH）2].
基金This work was supported by the National Natural Science Foundation of China (No. 20271029)
文摘A new dicopper(II) compound with oxalate and reduced imino nitroxide radicals [Cu2(m-C2O4)(Him2-py)2(H2O)2](NO3)2 (Him2-py=1-hydroxy-2-(2-pyridyl)-4,4,5,5-tetramethyli- midazoline) has been synthesized and its crystal structure was determined by X-ray diffraction method. The complex crystallizes in monoclinic, space group P21/n with a = 9.913(4), b = 19.057(8), c = 10.169(4) ? b = 114.292(7), V = 1751(1) 3, C26H38Cu2N8O14, Mr = 813.72, Dc = 1.543 g/cm3, m(MoKa) = 1.290 mm-1, F(000) = 840, Z = 2, the final R = 0.0398 and wR = 0.0986 for 1878 observed reflections (I>2s(I)). The imino nitroxide 2-(2-pyridyl)-4,4,5,5-tetramethyl- imidazoline-1-oxyl (im2-py) is reduced in the reaction to yield Him2-py which consists of oxalato-bridged centrosymmetric [Cu2(m-C2O4)(Him2-py)2(H2O)2]2+ ions and noncoordinated NO3- anions. Each copper(II) ion is in a distorted tetragonal pyramid environment: two nitrogen atoms from Him2-py and two oxygen atoms from the oxalate group are in the basal plane, and one water molecule at the axial position.
文摘利用热裂解-气相色谱质谱联用(pyrolysis gas chromatography mass spectrometry,Py-GC/MS)分析技术测定黑木耳新品种‘农黑2号’黑色素裂解产物组分的种类及含量,为解析黑色素的结构奠定理论基础。本研究通过碱溶酸沉法提取黑色素,并用紫外可见吸收光谱、傅立叶红外光谱、有机元素分析鉴定黑色素,采用Py-GC/MS技术分析其热裂解产物。结果表明,‘农黑2号’黑色素的最大吸收峰值在波长220 nm处,傅立叶红外光谱符合典型的黑色素特征;经有机元素分析,C、H、N、O元素的含量分别为43.47%、5.24%、11.71%和39.58%,不含硫元素,为真黑色素;检出的热裂解产物主要有苯类、苯酚类、吲哚类、苯基腈类、烃类、酸类等物质,其中苯、苯酚、吲哚等化合物为真黑色素的裂解产物。综上所述,‘农黑2号’黑色素为真黑色素,其基本骨架为苯环和吲哚,本研究为精准解析黑木耳黑色素结构提供科学依据。
