Hydrothermal Synthesis and Crystal Structure of a New 3-D Open-framework Zincophosphate

An open-framework zincophosphate, [C4N3H16][Zn4.5（PO4）4] 1, has been hydro- thermally synthesized and characterized by single-crystal X-ray diffraction. It crystallizes in the tetragonal space group P4 with a = 14.512（5）, c = 8.914（3）A, V = 1877.3（11）A3, C4H16NaO16P4Zn4.50, Mr = 780 24： Z = 4, Dc = 2.761 g/cm^3,μ= 6.103 mm^-1, F（000） = 1536, T = 298（2） K, R = 0.0416 and wR = 0.0816. In the structure, ZnO4 and PO4 tetrahedra are linked to each other, forming four-membered rings which are connected variably to form two secondary building units （SBUs）. The SBUs are connected so as to generate two chains along the c axis, which are further linked together alternatively via common oxygen atoms （Zn-O-P） giving rise to 8-ring-channels in the [001] direction, and the protonated guest diethylenetriamine （DETA） molecules sit in the middle of these channels. Other characterizations are also described by elemental analysis, thermal analysis and IR and fluorescent spectra.     

Synthesis of a Chain Aluminophosphate Containing Racemic 1,2—Diaminopropane

A one-dimensional chain aluminophosphate C1.5H7.5N1.5Al0.5PO4 containing diprotonated recemic 1,2-diaminopropane cations was synthesized from an alcoholic system. The compound consists of infinite inorganic [AlP2O8] chains of alternately connected AlO4 and PO2(=O)2 tetrahedral units and the racemic template moecules. The macroanionic chains contain corner-shared double four-membered rings.     

Solvothermal Synthesis, Structural Characterization and Properties of Two New Layered Lanthanide Sulfates

Two new layered lanthanide sulfates,[C₁₀H₁₀N₂][Pr₂(SO₄)₄(H₂O)₂](1)and[H₅O₂][Sm(SO₄)₂(H₂O)₃](2)were synthesized via solvothermal reaction and structurally characterized by single-crystal X-ray diffraction(XRD), infrared(IR) spectroscopy, thermal analysis, fluorescent spectra and inductively coupled plasma(ICP). Crystal data for compound 1, triclinic, P space group, a=0.8052(4) nm, b=0.9438(4) nm, c=1.4990(7) nm, α=79.450(5)°, β= 83.703(5)°, γ=74.048(5)°, V=1.0746(9) nm³, Z=2; for compound 2, monoclinic, P2₁/c space group, a=0.6599(11) nm, b=1.8940(3) nm, c=0.8765(14) nm, β=96.596(2)°, V=1.0883(3) nm³, Z=4. Structure analysis indicates that both the compounds exhibit a 2D corrugated layer structure, with protonated 4,4'-bipyridine cations and water dimmers (H₅O₂)⁺ located between the inorganic layers of compounds 1 and 2, respectively. Luminescent properties of compounds 1 and 2 were further investigated.     

Synthesis and crystal structure of a layered cobalt phosphate with a racemic 1,2-Diaminopropane template

A novel layered cobalt phosphate with racemic 1,2-diaminopropane as the templating agent, [CH₂(NH₃)-CH(NH₃)CH₃] [CoPO₄]₂, has been synthesized and structurally characterized by single-crystal X-ray diffraction methods. The compound crystallizes in the monoclinic system, space group P2₁/c with a = 10.457(2), b = 7.849(1), c = 6.692(l)?Å, β = 103.30(1)°, V = 534.5(2)?ų, Z = 2. The interaction of cobalt phosphate anionic layers and doubly protonated 1,2-diaminopropane cations is mainly ionic. The crystal structure is stabilized by a hydrogen bonding network between layers and templating cations.     

1,2-二甲基-3-吲哚甲叉(异丙叉)丁二酸酐(1)和1,2-二甲基-3-吲哚乙叉(异丙叉)丁二酸酐(2)的晶体结构

The crystal structures of 1,2-dimethyl-3-indolylmethylidene succinic fulgide anhydride (1) and 1,2-dimethyl-3-indolylethylidene succinic fulgide anhydride(2) were determined by singe crystal X-ray diffraction analysis. The crystal data are C_(18)H_(17)NO_3(1), orthogonal space group Pbca, with a=1.0084(3) nm, b=1.3966(4) nm, c=2.0945(6) nm, V=2.9498(15) nm, Z=8; C_(19)H_(19)NO_3 (2), orthogonal space group Pbca, with a=0.7988(3) nm, b=2.5782(10) nm, c=1.5664(5) nm, V=3.2259(22) nm, Z=8. R values are 0. 047 for (1) and 0.059 for (2) respectively.The photochemical properties of (1) and (2) were reported. Compound (1) is nonphotochromic, compound (2) changed from pale yellow to blue or green on irradiation at 365 nm or on exposure to indoor UV light either in crystal state or in solution (liquid or rigid plastic matrix).The differences in photochromic properties of compound (1) and (2) were discussed.     

1,2-二甲基-3-吲哚甲叉(异丙叉)丁二酸酐(1)和1,2-二甲基-3-吲哚乙叉(异丙叉)丁二酸酐(2)的晶体结构

1.2-二甲基-3-吲哚甲叉(异丙叉)丁二酸酐(1)(C_(18)H_(17)NO_3)与1.2-二甲基-3-吲哚乙叉(异丙叉)丁二酸酐(2)(C_(19)H_(19)NO_3)同属于吲哚俘精酸类化合物,它们的分子结构非常类似,只是(1)中为吲哚甲叉,(2)中为吲哚乙叉.但它们的光色性却差别很大.化合物(1)无光致变色性,化合物(2)则表现为良好的光致变色性.其原因在于结构的不同。     

A new uranyl niobate sheet in the cesium uranyl niobate Cs9[(UO2)8O4(NbO5)(Nb2O8)2]

A new cesium uranyl niobate, Cs₉[(UO₂)₈O₄(NbO₅)(Nb₂O₈)₂] or Cs₉U₈Nb₅O₄₁ has been synthesized by high-temperature solid-state reaction, using a mixture of U₃O₈, Cs₂CO₃ and Nb₂O₅. Single crystals were obtained by incongruent melting of a starting mixture with metallic ratio=Cs/U/Nb=1/1/1. The crystal structure of the title compound was determined from single crystal X-ray diffraction data, and solved in the monoclinic system with the following crystallographic data: a=16.729(2) Å, b=14.933(2) Å, c=20.155(2) Å β=110.59(1)°, P2₁/c space group and Z=4. The crystal structure was refined to agreement factors R₁=0.049 and wR₂=0.089, calculated for 4660 unique observed reflections with I?2σ(I), collected on a BRUKER AXS diffractometer with MoKα radiation and a CCD detector.In this structure the UO₇ uranyl pentagonal bipyramids are connected by sharing edges and corners to form a uranyl layer corresponding to a new anion-sheet topology, and creating triangular, rectangular and square vacant sites. The two last sites are occupied by Nb₂O₈ entities and NbO₅ square pyramids, respectively, to form infinite uranyl niobate sheets stacking along the [010] direction. The Nb₂O₈ entities result from two edge-shared NbO₅ square pyramids. The Cs⁺ cations are localized between layers and ensured the cohesion of the structure.The cesium cation mobility between the uranyl niobate sheets was studied by electrical measurements. The conductivity obeys the Arrhenius law in all the studied temperature domains. The observed low conductivity values with high activation energy may be explained by the strong connection of the Cs⁺ cations to the infinite uranyl niobate layers and by the high density of these cations in the interlayer space without vacant site.Infrared spectroscopy investigated at room temperature in the frequency range 400-4000 cm⁻¹, showed some characteristic bands of uranyl ion and niobium polyhedra.     

The Synthesis and Characterization of a New Layered Chlorozincophosphate Zn(HPO4)Cl[C4H10N]

Along a systematic study of open-framework materials aiming at producing new molecular sieves, we characterized a new zincophosphate Zn(HPO₄)Cl[C₄H₁₀N]. It was synthesized under mild conditions (r.t.) in the presence of pyrrolidinium as an organic-structure directing agent. The structure of this compound, determinated by single crystal X-ray diffraction, consists of anionic parallel [Zn(HPO₄)Cl]^? sheets alternating with thick slabs of organic molecules (C₄H₁₀N)⁺. These latters are linked to the anionic sheets through hydrogen bonds. Zn(HPO₄)Cl[C₄H₁₀N] crystallizes in the monoclinic system and the space group C2/c (No. 9) with cell parameters a = 24,83(9), b = 9,258(5), c = 8.778(3), β = 110,45(4), Z = 8, V = 1891.0(14) Åt³, R = 0.045, and R_w = 0.07. Solid state ³¹P and ¹³C MAS NMR spectroscopies are in agreement with the X-ray structure.     

Solvothermal Synthesis of a New Amine-Templated Vanadium Sulfate

A new organic-templated vanadium sulfate with formula [C₄H₁₂N₂][V^III (OH)(SO₄)₂] · H₂O 1 has been prepared under solvothermal conditions by using a mixture of glycol and water as solvent. The structure of this compound was characterized by IR, element analysis, TG and single crystal X-ray diffraction. The title compound crystallizes in the space group monoclinic, P2₁/c, a = 9.290(4) Å, b = 18.264(7) Å, c = 7.132(3) Å, β = 98.149(8)°,V = 1197.88 Å³, Z = 4. Structural analysis indicates that the title compound 1 possesses a 1D chain structure formed by VO₆ octahedra and SO₄ tetrahedra.     

具有十二元环开放结构磷酸锌的非水合成与表征

从非水体系中制备了 Zn2 ( HPO4) 3· H3NCH2 CH2 NH3单晶 ,用 X射线测定了晶体结构 ,用红外光谱 ,DTA-TG等方法对化合物进行了表征 .晶体属三斜晶系 ,P1空间群 .晶胞参数 a=0 .82 1 5( 3 ) nm,b=0 .8557( 3 ) nm,c=0 .9760 ( 3 ) nm,α=93 .8( 3 )°,β=95.3 8( 3 )°,γ=1 0 9.75( 3 )°,V=0 .63 94 nm3,Z=2 ,Dc=2 .50 g·cm- 3.结构中的锌和磷均与氧形成四面体配位 ,Zn O4和 HPO4四面体严格交替排列 ,骨架中的氧分为二桥氧和端氧 ,端氧只向 P原子配位 .三维开放式骨架结构中沿 a轴和 b轴方向有十二元环直孔道 ,质子化的有机胺在 a轴方向的十二元环孔道中     

Synthesis and crystal structure of the A6B5O18 perovskite-like compounds

New members of the A_nB_n−1O_3n perovskite-like family (Ba₅KNb₅O₁₈ and Sr₆Nb₄SnO₁₈ compounds) with n = 6 have been synthesized and studied by the X-ray powder diffraction. Their crystal structures were found to belong to the Ba₆Nb₄TiO₁₈-type with a = 0.57840(7) nm, c = 4.2532(5) nm and a = 0.5661(1) nm, c = 4.186(1) nm for Ba₅KNb₅O₁₈ and Sr₆Nb₄SnO₁₈, respectively. It was shown that Ba and K (A-atoms) are completely disordered in the crystal structure of Ba₅KNb₅O₁₈ compound. But Nb and Sn atoms (B-atoms) in the crystal structure of the Sr₆Nb₄SnO₁₈ compound are quite ordered with the preferred Sn⁺⁴ and Nb⁵⁺ cations localization in the center of perovskite-like block and on the boundaries of these blocks, respectively. Temperature and frequency dependencies of the real components of electric conductivity σ^I and dielectric permeability ɛ^I; specific electric conductivity at the direct current σ_dc have been obtained by the impedance spectroscopy method for Sr₆Nb₄SnO₁₈.     

一个新型层状化合物[Ni(C10H8N2)2V3O8.5]的水热合成与晶体结构

多金属氧酸盐因其在医药临床、工业催化和功能材料等方面的广泛应用而引起人们的关注[1～7]. 由于钒化合物具有令人感兴趣的结构以及在材料领域中的重要的应用而倍受关注. 在以往的合成中, 常压溶液合成是主要手段, 利用水热合成方法制备多金属氧酸盐配合物晶体是近几年来国际上刚刚兴起的一项研究工作, 通过该方法已合成出一批具有新颖结构的层状、链状、多孔、高聚合度化合物[8～11], 一些已用于药物和催化剂的研究工作中. V-O体系化合物的合成与表征近来已引起人们的极大兴趣, 如: [VⅣVⅤ2O7(phen)]n[12]是一含有混合价钒的层状结构; Ni(en)3(VO3)2[13], Cu(dien)V2O6*H2O[14]是一维链状结构. 为了探究水热条件下钒物种的反应特性及生成规律, 制备新的钒配合物晶体, 目前我们正在积极开展这方面的研究并取得了一定成果.     

A bright blue emission material based on anthracene： Synthesis, characterization and luminescent properties

A blue light-emitting material,2-(N-ethyl-anthraceneyl-9) imidazo[4,5-f]1,10-phenanthroline(EAIP),has been synthesized and characterized by ~1H NMR,IR,elemental and single crystal X-ray diffraction analysis.The results of theoretical calculations indicate that the HOMO and LUMO distributions mainly locate at the anthracene fragment.It displays bright blue emission in both solid state and dichloromethane solution.The emission quantum yield calculated is 0.76.     

粉末衍射技术解析青蒿素晶体结构方法学比对研究

以粉末X射线衍射技术(PXRD)表征有机物晶体结构为目的,选取我国第1个全新药物青蒿素(Artemisinin)验证粉晶解析有机物晶体结构方法的合理性。粉晶解析结果为正交晶系,P212121空间群,a=23.98223±0.01624,b=9.42480±0.00645,c=6.34589±0.00439,α=β=γ=90°,Z=4,V=1434.693;单晶解析结果为正交晶系,P212121空间群,a=23.9564(9),b=9.3224(5),c=6.3205(3),α=β=γ=90°,P212121,Z=4,V=1411.55(17)3;两者所确定分子非氢结构键长、键角、二面角的相关系数分别为0.9921、0.9833和0.9997,晶胞参数基本吻合,分子构型相似。结果表明,粉晶X射线衍射技术可以求得较为准确的青蒿素晶胞参数及晶胞内分子构型。     

rac-11-t-Butoxy-1,4-dihydro-1,4-methanoanthracene:A two-dimensional framework structure built from C-H…O and C-H…πhydrogen bonds

The title compound rac-11-t-butoxy-l,4-dihydro-l,4-methanoanthracene(C₁₉H₂₀O,M_r = 264.35) has been synthesized and characterized by FT-IR,’H NMR,HRMS spectra and single-crystal X-ray diffraction.The crystal belongs to monoclinic,space group P2₁/n,with a = 13.5240（10）,b = 8.3453（6）,c = 13.9604（9） ,β= 100.0190（10）°.The structure of the title compound comprises a norbomene unit with a t-butoxy group,having a naphthalene ring fused on one side.The naphthalene is essentially planar with a maximum deviation of 0.032（2） for atom C（3）.In the crystal,inversion-related molecules are linked by pairs of C-H…O hydrogen bonds,forming a cyclic dimer with R₂²（16） graph-set motif.The C-H…πinteractions are also observed,linking the molecules into a continuous two-dimensional framework structure.     

新型磷-钒-氧层状化合物[H2en]2[H3O]6[Co(H2O)2(VO)8(OH)4(PO4)8]的水热合成与晶体结构

金属磷酸盐材料在吸附、离子交换、离子传导和催化剂方面有潜在的应用前景[1～5]. 近年来, 通过水热反应合成了一些A-V-P-O化合物. 在这些化合物中, A一般为碱金属或有机阳离子, 如层状结构的[H2N(C4H8)2NH2][(VO)4(OH)4(PO4)2][6] 和[H2N(C2H4)3NH2][(VO)8(HPO4)3(PO4)4*(OH)2]*2H2O[6], 一维链状结构的 [H2NCH2CH2NH3(VO)(PO4)][7], 手性双螺旋结构的 [(CH3)2NH2]K4[(VO)10(H2O)2(OH)4(PO4)7]*H2O[8]以及具有三维骨架结构的化合物 [H3N(CH2)3NH3K(VO)3(PO4)3][9], [H3N(CH2)3NH3]2[V(H2O)2(VO)6(OH)2(HPO4)3(PO4)5]*3H2O[10]和[H3N(CH2)2NH3][(VO)3(H2O)2(PO4)2(HPO4)4][11].     

In[NC5H3(CO2)2](OH2)F: A new layered indium-organic framework material (NC5H3(CO2)2=2,6-pyridinedicarboxylate)

A new layered indium-organic framework material, In[NC₅H₃(CO₂)₂](OH₂)F has been synthesized by a hydrothermal reaction using In₂O₃, NH₄F, 2,6-NC₅H₃(CO₂H)₂ (2,6-pyridinedicarboxylic acid), HF, and water at 200 °C. Single-crystal X-ray diffraction was used to determine the structure of the reported material. In[NC₅H₃(CO₂)₂](OH₂)F has a novel layered structure consisting of InO₅NF polyhedra and the pyridinedicarboxylate organic linker. Detailed structural analyses with full characterization including infrared spectrum, thermogravimetric analysis, elemental analysis, exchange reactions for the coordinated water molecule, and gas adsorption experiments are reported.     

Hydrothermal synthesis and structural characterization of a novel cadmium-organic framework

A three-dimensional diamondoid cadmium-organic framework, formulated as [Cd(NDC)(H₂O)] (I) (where NDC²⁻=2,6-naphtalenedicarboxylate), has been hydrothermally synthesized and structurally characterized using single-crystal X-ray diffraction. The hydrothermal synthesis of I has been optimized by modifying the composition of the reactive mixture and the temperature programme, so that a highly crystalline and pure homogeneous phase could be obtained. A novel layered structure, formulated as [Cd₂(NDC)(OH)₂], was isolated when the molar ratio of triethylamine exceeds ca. 0.7. Both products have been characterized using powder X-ray diffraction, IR and Raman spectroscopies, and elemental and thermal analyses.     

Structural change in a series of protonated layered perovskite compounds, HLnTiO4 (Ln=La, Nd and Y)

A deuterated n=1 Ruddlesden-Popper compound, DLnTiO₄ (HLnTiO₄, Ln=La, Nd and Y), was prepared by an ion-exchange reaction of Na⁺ ions in NaLnTiO₄ with D⁺ ions, and its structure was analyzed by Rietveld method using powder neutron diffraction data. The structure analyses showed that DLaTiO₄ and DNdTiO₄ crystallized in the space group P4/nmm with a=3.7232(1) and c=12.3088(1) Å, and a=3.7039(1) and c=12.0883(1) Å, respectively. On the other hand, DYTiO₄ crystallized in the space group P2₁/c with a=11.460(1), b=5.2920(4), c=5.3628(5) Å and β=90.441(9)°. The loaded protons were found to statistically occupy the sites around an apical oxygen of TiO₆ octahedron in the interlayer of these compounds, rather than Na atom sites in NaLnTiO₄.