^31P NMR Studies on the Ligand Dissociation of Trinuclear Molybde-num Cluster Compounds

A series of carboxylate-substituted trinudear molybdenum dus-ter compounds formulated as Mo3S4(DTP)3(RCO2)(L), where RffiH, CH3, C2H5, CH2Cl, CCl3, R^1C6H4(R^1 is the group on the benzene ring of aromatic carboxylate ), L=pyridine,CH3CN, DMF, have been synthesized by the ligand substitu-tion reaction. The dissociation of the loosely-coordinated ligand L from the cluster core was studied by ^31p NMR. The dissocia-tion process of L is related to the solvent, temperature, and acidity of carboxylate groups, so as to affect the solution struc-ture and reactive properties of the duster. The long-distance in-teraction between ligands RCO2 and L is transported by Mo3S4 core.     

水合法合成樟脑副产油中异莰烷的分离和鉴定

水合法合成樟脑副产油中异莰烷的分离和鉴定     

高效液相色谱法测定乙炔催化反应液中丁烯二酸二丁酯的异构体

丁烯二酸二丁酯可作为涂料、粘接剂及多种化工产品的重要原料。本实验是以乙炔和亚硝酸丁酯为原料,在一氧化碳存在下,用钯作催化剂产生丁烯二酸二丁酯,丁烯二酸二丁酯有顺式和反式两种异构体,反应式如下:     

Synthesis,Structure and Photoluminescence of a New Cadmium（Ⅱ） Complex Involving in situ Decarboxylation

A new luminescent dinuclear cluster complex [Cd2（pzc）2（AmTAZ）（HEO）4（NO3）]·NO3 （Hpzc = pyrazine-2-carboxylic acid, AmTAZ = 3-amino-4H-1,2,4-triazole） has been prepared by the assembly of Cdn with pyrazine-2,3-dicarboxylic acid and 3-amino-lH-1,2,4-triazole-5-car- boxylic acid ligands under hydrothermal conditions, in which in situ decarboxylation of H2pzdc and HAmTZC ligands simultaneously occurred, and HEpzdc was transformed into Hpzc while HAmTZC into AmTAZ. The crystal structure is of triclinic, space group P1 with a = 7.096（2）, b = 11.140（4）, c = 14.887（5）А, α= 92.641（4）, β= 91.348（6）, γ= 96.058（6）°, V = 1168.5（7）А^3, C12H18Cd2N10O14, Mr = 751.16, Z = 2, Dc = 2.126 g/cm^3, F（000） = 730,μ=1.910 mm^-1, R = 0.0320 and wR = 0.0998 for 4549 observed reflections （I 〉 2σ（I））. The dinuclear cluster of 1 is extended into a 3D supramolecular architecture through intermolecular hydrogen bonding interactions. Complex I exhibits strong blue photoluminescence at room temperature.     

Identification and Structures of Two Main Unknown Components in the By-product from the Hydration Synthesis of Camphor

Two main unknown components in the by-product of camphor hydration synthesis were separated and identified by fine fractional distillation and spectroscopic analyses. The components with different ratios of unknown components A and B were collected by the further distillation. The combined spectral results of GC, MS,GC-MS and 13C NMR of the collected samples revealed that A is exo-2, 2, 3-trimethylbicyclo[2, 2, 1 ]heptane, and B is endo-2, 2, 3-trimethylbicyclo[2, 2, 1 ]heptane.     

双金属Ni-Cu催化剂用于催化乙醇羰化合成丙酸和丙酸乙酯

研究了Ni-Cu(催化剂的比表面积、原料气含O_2量等对乙醇羰化合成丙酸和丙酸乙醇的影响。在常压和300℃下,Cu_(2+)为2.2％和CO/C_2H_5OH=2.8(摩尔)时,丙酸和丙酸乙酯收率最高。对Cu_(2+)在催化剂中的作用以及催化剂的稳定性进行了讨论。     

A 2-D Copper Coordination Polymer [Cu(4,4''''-bpy)(H_2O)_4](C_4H_2O_4)(H_2O)_4 Integrated by Hydrogen Bonds and VDW Interactions

1 INTRODUCTION A great deal of interest in transition metal com- plex assembly has recently been devoted to the development of rational synthetic routes to novel one-, two- and three-dimensional crystal frameworks, due to their potential applications in…     

Synthesis and Crystal Structure of a Mo-S Cluster Compound Coordinated by Isonicotinate

A cluster compound, Mo3S4(DTP)3(IN)(Py)·EtOH I (DTP = diethyl dithiophospha- te, IN = isonicotinate) has been rationally synthesized and characterized by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1 with a = 13.6345(2), b = 13.7805(2), c = 14.5400(1) , α = 107.078(1), β = 113.380(1), γ = 96.310(1)o, C25H45Mo3- N2O9P3S10, Mr = 1218.96, V = 2315.75(5) 3, Z = 2, Dc = 1.748 g/cm3, μ = 1.399, F(000) = 1224, R = 0.0425 and wR = 0.1144 for 6335 observed reflections (I > 2σ(I)). 31P NMR spectrum has been measured with the resonance 110.050 and 108.783 (2:1).     

溶胶凝胶法制备的Cu/SiO2催化剂及其催化草酸二甲酯加氢反应

采用溶胶凝胶法制备了用于草酸二甲酯加氢合成乙二醇的Cu/SiO2催化剂,在优化的反应条件下,当催化剂中Cu含量为15%～25%时,草酸二甲酯转化率和乙二醇选择性分别达到99.9%和95.0%.通过N2吸附-脱附、透射电镜、X射线衍射、氢气程序升温还原、N2O滴定法和X射线光电子能谱等手段对各Cu/SiO2催化剂进行了表...     

Synthesis, Structure and Topological Analysis of a New Zinc（Ⅱ） Complex [Zn2（bptc）（bpe）（H2O）]n

A novel zinc coordination polymer,[Zn 2 (bptc)(bpe)(H 2 O)] n (1,H 4 bptc=3,3,4,4-benzophenonetetracarboxylate,bpe=1,2-bis(4-pyridyl) ethane),has been prepared under hydrother-mal conditions.The crystal structure is of monoclinic,space group C/2c with a=27.50(2),b=6.207(4),c=16.233(11),β=107.522(14)°,V=2642 (3)3,C 29 H 22 N 2 O 11 Zn 2,M r=705.27,Z=4,D c=1.773 g/cm 3,F(000)=1432,μ=1.887 mm-1,R=0.0421 and wR=0.1049 for 2594 observed reflections (I > 2σ(I)).X-ray single-crystal diffraction analysis shows that 1 features two-dimensional [Zn 2 (bptc)(H 2 O)] layers,which are further linked by the bpe ligands to give rise to a three-dimensional pillar-layered structure.According to the topology analysis,this framework can be simplified into a (4,6)-connected (4 4 ·6 2)(4 4 ·6 10 ·8) network.