2D氢键网状Mg(Ⅱ)配合物的合成和晶体结构

The title complex [Mg(H₂O)₆]·(L)·(H₂O) [L=2-formyl-benzenesulfonate-hydrazine] was synthesized by the reaction of magnesium chloride hexahydrate with 2-formyl-benzenesulfonic acid sodium-hydrazine in the CH₃CH₂OH/H₂O. It was characterized by elemental analysis, IR and X-ray single crystal structure analysis. The crystal of the title complex [Mg(H₂O)₆]·(C₁₄H₁₂N₂O₇S₂)·(H₂O) belongs to triclinic, space group P1 with a=0.781 09(12) nm, b=0.781 27(13) nm, c=0.995 68(19) nm, α=102.054(2)°, β=92.331 0(10)°, γ=105.500(2)°, V=0.569 59(17) nm³, Z=1, D_c=1.559 Mg·m^-3, μ=0.334 mm^-1, F(000)=280, and final R₁=0.033 9, wR₂=0.091 6. The complex comprises a six-coordinated magnesium(Ⅱ) center, with a O₆ distorted octahedron coordination environment. The molecules are connected by hydrogen bonds to form two dimensional network structures. CCDC: 716601.     

荧光素/层状钇氢氧化物复合体的发光性能及对Hg2+的识别

合成了层状钇氢氧化物(LYH)复合体FN/OS-LYH(FN为荧光素,OS为1-辛烷磺酸钠),研究了复合体的光致发光性能及剥离态胶体对Hg~(2+)的荧光识别性能。固态下,FN的钠盐不发光,FN/OS-LYH复合体发射黄绿光(564 nm);甲酰胺中,剥离为胶体悬浮液后,复合体发射绿光(540 nm,即剥离后蓝移24 nm),比FN阴离子的发射(572 nm)蓝移32 nm。复合体对高毒性Hg~(2+)具有很好的荧光识别能力,优于其他离子(Mg~(2+),Ni~(2+),Co~(2+),Cu~(2+),Zn~(2+),Pb~(2+)和Cd~(2+))。复合体加入Hg~(2+)后发生荧光淬灭,Hg~(2+)检测限为2.73×10-7mol·L-1,淬灭常数(Ksv)为4.82×102 L·mol-1。     

Synthesis,Crystal Structure and Antibacterial Activity of （2E,3E）-N1,N2-Bis（2,3,4-trimethoxy-6-methylbenzylidene）ethane-1,2-diamine

The title compound （2E,3E）-N1,N2-bis（2,3,4-trimethoxy-6-methylbenzylidene）- ethane-l,2-diamine （C24H32N2O6, Mr = 444.52） was synthesized and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. The crystal belongs to triclinic, space group P2/c, with a = 8.5480（10）, b = 9.3710（12）, c = 15.280（2）A, β = 90.780（2）°, V= 1223.9（3）A3, Z = 2, Dc= 1.206 g/cm3, 2 = 0.71073A,μ（MoKa） = 0.087 mm^-1, F（000） = 476, the final R = 0.0680 and wR = 0.1450 for 2144 observed reflections with I 〉 2σ（I）. X-ray diffraction analysis reveals that the molecule adopts an E configuration about the central C=N functional bond. The phenyl rings of two 2,3,4-trimethoxy-6-methylbenzaldehyde groups are symmetrically parallel. The molecules are linked through C-H…O hydrogen bonding interactions. The title compound possesses moderate antibacterial activity.     

固定化脲酶催化作用下双醛纤维素对尿素氮的吸附平衡和动力学

研究了在固定化脲酶催化作用下双醛纤维素对尿素氮的吸附平衡和动力学. 吸附过程符合Langmuir方程, 为单分子层化学吸附. 考察了双醛纤维素的氧化度、初始尿素氮浓度、双醛纤维素与固定化脲酶的质量比和温度等对双醛纤维素吸附尿素氮的影响, 结果表明上述因素对尿素氮的吸附均有较显著的影响. 实验数据能很好地拟合准二级吸附速率方程, 说明该吸附过程遵从二级动力学模型. 当氧化度为88%的双醛纤维素与固定化脲酶的质量比为10∶1, 尿素氮浓度为638.3 mg•L^－1时, 由Arrhenius方程求得表观吸附活化能为6.0 kJ•mol^－1, 该吸附过程为吸热反应.     

Synthesis,Crystal Structure and Antibacterial Activity of （E）-N1,N4-Bis（2,3,4-trimethoxy-6- methylbenzylidene）butane- 1,4-diamine

The title compound （E）-N1,N4-bis（2,3,4-trimethoxy-6-methylbenzylidene） butane- 1,4- diamine （C26H36N2O6, Mr = 472.57） was synthesized and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. The crystal belongs to triclinic, space group C2/c with a = 36.102（4）, b = 5.6620（11）, c = 13.015（2）A,β = 105.491 （2）°, V = 2563.7（7）A3, Z = 4, Dc = 1.224 g/cm3, 2 = 0.71073 A,μ（MoKα） = 0.087 mm^-1, F（000） = 1016, the final R = 0.0456 and wR = 0.1257 for 2255 observed reflections with I 〉 2σ（I）. X-ray diffraction analysis reveals that the molecule adopts an E configuration about the central C=N functional bond. The phenyl rings of two 2,3,4-trimethoxy-6-methylbenzaldehyde groups are parallel by symmetry. The molecules are linked through π-π and C-H…π stacking interactions and C-H…O hydrogen bonding interactions. The title compound possesses moderate antibacterial activity.     

四硫代钼酸根/1-辛烷磺酸根/LEuH复合体发光性能及对Hg~(2+)的识别

采用改进的均匀沉淀法合成了硝酸根插层的稀土铕层状氢氧化物(NO_3-LEuH),通过离子交换法将阴离子型表面活性剂1-辛烷磺酸根(OS-)及无机阴离子MoS2-4共插层于LEu H的层间,通过改变MoS_4~(2-)和OS~-的投料比得到一系列发光强度不同的复合体(MoS_4)_xOS_(1-x)-LEuH(x=0.02,0. 10,0. 20).采用X射线粉末衍射仪(XRD)、傅里叶变换红外光谱仪(FTIR)和荧光分光光度计(PL)等研究了其结构及性质.结果表明,MoS_4~(2-)会明显削弱层板Eu~(3+)的红光发射,且在一定MoS_4~(2-)/OS~-摩尔比范围内发光强度随MoS_4~(2-)含量增加而降低.选择MoS_4~(2-):OS~-摩尔比为0.02∶0. 98的复合体(MoS4)0.02OS0.98-LEu H用于水体系重金属离子Hg~(2+),Cu~(2+),Ag+,Pb~(2+)的荧光识别,发现剥离态复合体对Hg~(2+)具有选择性识别能力,加入含Hg~(2+)水溶液后发光有一定程度增强,可用作off-on型荧光传感器件识别毒性Hg~(2+).     

荧光素-层状双金属氢氧化物复合体的发光性能及对Fe3+的荧光识别

采用离子交换法合成了FLN/OS-LDH复合体(FLN: 荧光素, OS: 1-辛烷磺酸钠, LDH: 镁铝型层状双金属氢氧化物), 并研究了其光致发光和对Fe³⁺的识别性能. 固态时, FLN不发光, 而FLN/OS-LDH复合体呈黄绿色荧光(发射波长为565 nm), 是荧光素(FLN)的特征发射光. 在甲酰胺(FM)中可将该复合体方便剥离为胶状悬浮液, 其发射波长发生蓝移, 为绿光发射(531 nm). 研究了复合体剥离液对金属离子的荧光识别特性, 发现其对Fe³⁺的选择性识别能力很强, 远优于其它离子(Mg²⁺, Ni²⁺, Co²⁺, Cu²⁺, Zn²⁺, Pb²⁺, Cd²⁺和Hg²⁺). 该复合体与Fe³⁺结合发生荧光猝灭现象, 可将其用作检测Fe³⁺的荧光传感器. Fe³⁺检测限为1.27×10^-7 mol/L, 猝灭常数(K_sv)为3.44×10² L/mol.