Synthesis and Crystal Structure of Mixed-Ligand Ni(II) Complex of N-(1-Phenyl-3-methyl-4-benzylidene-5-pyrazolone) p-Nitrobezoylhydrazide and Pyridine

A novel mixed-ligand nickel complex, [Ni(PMBP—PNH) (Py)₃], [PMBP—PNH=N-(1-phenyl-3-methyl-4-benzylidene-5-pyrazolone) p-nitrobezoylhydrazide; Py = pyridine], has been synthesized by the hydrothermal method and characterized by elemental analysis, IR spectrum, thermal analysis, and single-crystal X-ray diffraction. The X-ray diffraction reveals that the nickel (II) ion in the title complex is in a slightly distorted octahedral arrangement of the ONO donor atoms of primary ligand PMBP-PNH and three N-donor atoms in the secondary ligand pyridine.     

水热法制备高纯超细CeO2-ZrO2复合氧化物

Superfine composite powders of CeO₂-ZrO₂ (CZ) and CeO₂-ZrO₂-La₂O₃ (CZL) were prepared by hydrothermal method. The effects of pH、temperature and time for hydrothermal process on the performance of the resulting powders were studied. The optimized reaction parameters were on follows: the precursor′s pH≈9.0, hydrothermal temperature of 200 ℃ holding for 2 h. Thermal stable powders with average particle size smaller than 10 nm and specific surface area of 171 m²·g^-1 were obtained. A BET specific surface area was still at 44 m²·g^-1 after calcination at 1 000 ℃ for 6 hours.     

二维配位聚合物[Zn(PDC)(phen)]n的合成、晶体结构及荧光性质

合成了锌(II)与3,4-吡啶二羧酸和1,10-邻菲啰啉形成的配位聚合物[Zn(PDC)(phen)]_n (1) (H₂PDC＝3,4-吡啶二羧酸, phen＝1,10-邻菲啰啉), 对其进行了元素分析、红外光谱和X射线单晶衍射表征, 测定了晶体结构. 该聚合物属单斜晶系, P2(1)/n空间群, a＝0.77136 nm, b＝1.9757(4) nm, c＝1.0680(2) nm, β＝95.36(3)°, V＝1.6205(6) nm³, Z＝4, D_c＝1.683 Mg/m³, M_r＝410.68, F(000)＝832, μ＝1.55 mm^－1, 最终偏离因子R₁＝0.0608, wR₂＝0.0967. 该化合物中Zn原子与来自两个PDC的三个羧基氧原子, 另外一个PDC的吡啶氮原子, 以及phen的两个氮原子配位, 形成的ZnN₃O₃八面体通过PDC桥联形成二维层状网络结构. 此外还研究了该聚合物的热性质和荧光性质.     

十八元环多钒硼酸盐的水热合成及其氧化还原性质研究

在水热条件下合成了[Ni(en)2]6[(VO)12O6B18O39(OH)3].6H2O多钒硼酸盐,X射线衍射分析表明,该晶体属三方晶系,R-3空间群.测试了晶体的IR光谱和TG曲线,用循环伏安法详细研究了合成化合物的氧化还原性质及电子转移机理,结果表明该化合物具有两对氧化还原峰,其电子转移数分别为单电子和三电子.     

选相原位法合成立方氮化硼的关键影响因素

利用选相原位法在水溶液中成功制备出了立方氮化硼晶体，对反应条件进行了优化。结果表明，利用选相原位法合成立方氮化硼的最佳实验条件是：反应压力为10.0 MPa，在氯离子加入下利用混合氮源进行反应。在该条件下得到了纯相的立方氮化硼晶体。     

Hydrothermal Synthesis and Structural Characterization of a Novel Organic—Inorganic Hybrid Compound {[Cu（2,2′—bpy）2]2—Mo8O26}

A novel organic-inorganic hybrid compound {[Cu(2,2′-bpy)2]2Mo8O26} has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction. The compound crystallizes in the orthorhombic space group, Pna21,with a=2.4164(5),b=1.8281(4),c=1.1877(2)nm,V=5.247(2)nm^3,Z=4,and final R1=0.0331,wR2=0.0727.The structure consists of discrete {[Cu(2,2′-bpy)2]2Mo8O26} clusters,constructed from a β-octamolybdate subunit[Mo8O26]^4- covalently bonded to two [Cu(2,2′-bpy)2]^2 coordination complex cations via bridging oxo groups.In addition,the spectroscopic properties and thernal behavior of this compound have been investigated by spectroscopic techniques (UV-vis,IR,Raman and EPR spectra) and TG analysis.     

Hydrothermal Synthesis,Crystal Structure and Thermal Analyses of Pyrazine-2,3-dicarboxylic Acid Bridged Co(II) Coordination Polymer of _∞~2[Co(phen)(μ-L)_(3/3)]·H_2O (H_2L = Pyrazine-2,3-dicarboxylic Acid)

1 INTRODUCTION Molecular assembly and supramolecular che-mistry are young and rapidly growing subjects andhave attracted great attention. Microporous materialsbuilt up by organic ligands and metal ions have po-tential applications in catalysis, chemical absorption,magnetism and electronic conductivity[1～3]. Multi-dentate organic ligands are good building blocks,such as 1,2,4,5-benzene tetracarboxylic acid (BT-CA), 1,3,5-benzene tricarboxylic acid, terephthalicacid, 1,10-phenanthrol…     

Ni(phen)(H2O)(V2O6)的水热合成和晶体结构（英）

A novel compound Ni(phen)(H₂O)(V₂O₆) has been hydrothermally synthesized and structurally determined to be a two-dimensional compound, which contains {V₂O₆}_n^2n- chains interconnected by nickel(Ⅱ) complexes via oxygen atoms. The crystallographic data measured by single-crystal X-ray diffraction analysis are as follows: C₁₂H₁₀N₂NiO₇V₂, M_r=454.81, monoclinic, space group P2₁/c, a=0.784 6(3), b=2.103 6(8), c=0.942 3(4) nm, β=112.872(5)°, V=1.433 0(10) nm³, Z=4, D_c=2.104 Mg·m^-3, μ(Mo Kα)=2.615 mm^-1, F(000)=904, T=298(2) K, 4 480 reflections collected, 2 470 independent (R_int=0.032 2), the final R=0.058 4 and wR₂=0.145 7 for 2 303 observed reflections with I>2σ(I). CCDC: 192520.     

Cu/SO42-/La2O3-ZrO2-Al2O3催化剂的制备及其对C3H6选择还原NO的催化性能

以Al₂O₃为基质，添加ZrO₂和La₂O₃，制成La₂O₃-ZrO₂-Al₂O₃复合载体，然后采用SO₄^2-进行改性，再负载上Cu²⁺，制备了铜基SO₄^2-改性的复合载体催化剂(Cu/SO₄^2-/La₂O₃-ZrO₂-Al₂O₃)。考察了它在富氧条件下对丙烯选择还原NO的催化性能，并借助XRD、SEM、TG、Py-IR、NH₃-TPD、FTIR和TPR等方法研究了Cu/SO₄^2-/La₂O₃-ZrO₂-Al₂O₃的结构和性能的关系。结果表明，ZrO₂的加入主要有利于提高催化剂的低温活性；La₂O₃的加入则主要有利于提高催化剂的热稳定性和还原性能；SO₄^2-能够与Zr形成螯合双配位结构，大幅度促使催化剂表面酸量增加并且酸性增强；因此，有效地提高了Cu/SO₄^2-/La₂O₃-ZrO₂-Al₂O₃在富氧条件下对丙烯选择还原NO的催化活性和水热稳定性。在无水条件下，Cu/SO₄^2-/La₂O₃-ZrO₂-Al₂O₃能使NO的最大转化率高达84.3%，即使在275 ℃ 10%水蒸气存在的情况下，仍能使NO的转化率高达81.2%。