Synthesis and Crystal Structure of 5,17-Diformyl-11,23-di（tert-butyl）25,26,27,28-tetrapropoxy-calix[4]arene

The title compound 5,17-diformyl-11,23-di（tert-butyl）-25,26,27,28-tetrapropoxycalix[4]arene has been synthesized by selective formylation of 5,11,17,23-tetra（tert-butyl）25,26,27,28-tetrahydroxycalix[4]arene in three steps and characterized by1H NMR and X-ray single-crystal diffraction.The crystal belongs to the monoclinic system,space group C2/c with a = 25.760（3）,b = 10.9952（10）,c = 18.630（2）,β = 119.985（4）°,V = 4570.4（9）3,Z = 4,Dc = 1.106 g/cm3,Mr = 761.01,F（000） = 1648,μ = 0.071 mm-1,MoKa radiation（λ = 0.71073）,R = 0.0710 and wR = 0.2411 for 3234 observed reflections with I 2σ（I）.X-ray analysis reveals that the title compound adopts a pinched cone conformation which leads to an open cavity.Intermolecular C–H O weak interactions link the molecules along the bc plane,which are effective in the stabilization of the crystal structure.     

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Synthesis and Crystal Structure of N,N′,N″- Tris-（2-aminophenyltriphenylphosphium）- benzene- 1,3,5-tricarboxamide

A new tripodal P,N ligand （C63H48N3O3P3） was prepared and characterized by elemental analysis, IR and single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 13.013（3）, b = 28.406（6）, c = 14.911（3） A^°, β= 111.04（3）°, V= 5144.6（18） A^°^3 Z = 4, Dc = 1.276 g/cm^3, Mr = 987.95, λ（MoKa） = 0.71073 A^°,μ = 0.17 mm^-1, F（000） = 2064, R = 0.0786 and wR = 0.1545. A total of 43260 unique reflections were collected, of which 5112 with I 〉 2σ（I） were observed. The title compound has a central benzene ring, which is linked by -NH-CO- bonds to three 2-aminophenyltriphenylphosphium moieties, of which two with P（1） and P（2） centers are pointing to the same face of the central aryl ring, while the third one directs oppositely, forming a pseudo-propeller. In the crystal structure, there exist face-to-face π-π stacking interactions which increase the stability of the crystal structure.     

Synthesis,Crystal Structure and Biological Activities of N-（4-Cyanopyrazole-3-yl）- α-（3,5-difluorophenyl）- O,O-diisopropyl- α-aminophosphonate

The title compound has been synthesized by the addition reaction of N-（4-cyanopyrazole-3-yl）-3,5-difluorophenyl-imine and diisopropyl phosphate. Its structure was confirmed by means of IR, ^1H NMR and elemental analysis. The single-crystal structure of the title compound was determined by X-ray crystallography. The compound crystallizes in monoclinic, space group C2/c with a = 18.9959（14）, b = 9.2212（7）, c = 22.1108（16）A^°, β= 90.1540（10）°, V = 3873.0（5） A^°^3, Dc = 1.366 g/cm^3, Z = 8, μ = 0.185, F（000） = 1664, and the final R = 0.0503 and wR = 0.1539 for 2996 observed reflections （I 〉 2σ（I））. The results demonstrate that the dihedral angle between the pyrazole and benzene rings is 105.5°, and there is a full delocalized pyrazole system with sp^2 hydridization of N（3）. The crystal structure is stabilized by two intermolecular hydrogen bonds of N（1）-H（1）…O（3） and N（3）-H（3A）…N（4）. The preliminary biological test shows that the title compound has a moderate antifungal activity.     

Synthesis,Crystal Structure and Luminescent Property of a 2-D Hybrid Constructed from [Pb_2I_4] Subunits

A novel organic-inorganic hybrid compound, [Pb2I4（bipy）], （bipy = 4,4′-bipyridine）, was synthesized by self-assembly and its structure was determined by X-ray crystallography method The crystal belongs to the monoclinic system, space group P2 1/c with α = 4.4691（9）, b = 15.385（3）, c = 14.136（3） A, β = 93.75（3）°, V= 969.9（3） A^3, Mr = 1078.16, Dc= 3.692 g/cm^3, F（000） = 916, μ = 23.688 mm^-1, Z = 2, the final R = 0.0395 and wR = 0.0887 for 1557 observed reflections with I 〉 2σ（I）. The title compound presents a two-dimensional layer-like structure constructed from [PbI5N] octahedron and bis-bridging ligand 4,4′-bipyridine. The fluorescence of the title compound is also discussed in this communication.     

Synthesis and Crystal Structure of 5,7-Dimethoxy-2-phenylquinolin-4-yl Phenyloxy （N-L-Alanine ethyl ester） Phosphoramidate

5,7-Dimethoxy-2-phenylquinolin-4-yl phenyloxy （N-L-alanine ethyl ester） phosphoramidate （C28H29N2O7P, Mr = 536.17） has been synthesized by a facial phosphorylated reaction, and its structure was determined by IR, NMR, HR MS and X-ray single-crystal diffraction. The crystal belongs to triclinic, space group P1^-, with a = 11.375（2）, b = 11.591（2）, c = 11.638（2） A^°, α= 109.46（3）, β= 104.58（3）, γ= 100.48（3）°, V = 1339.6（5）A^°^3, Z = 2, Dc = 1.330 g/cm^3,μ = 0.152 mm^-1, F（000） = 564, the final R = 0.0654 and wR = 0.1546. In the crystal structure, the title compound is constructed by a centrosymmetric dimmer unit composed of a pair of π-π stacking diastereoisomers. The compound has a noteworthy feature in the framework, and such units are linked by two equal intermolecular P=O…H-N hydrogen bonds.     

Synthesis,Crystal Structure and Luminescent Properties of [Ag（bzdmpymt）]6·2MeOH （bzdmpymtH = 5-Benzyl-4,6-dimethylpyrimidine-2-thione）

Reaction of AgAc with bzdmpymtH in MeOH resulted in the title compound [Ag（bzdmpymt）]6-2MeOH （1.2MeOH）, which was structurally characterized by elemental analysis, IR, and single-crystal X-ray diffraction analysis. 1.2MeOH belongs to the triclinic system, space group Pi, with a = 10.930（2）, b = 11.646（2）, c = 16.794（3）A, a = 103.97（3）, β = 97.07（3）, γ = 97.94（3）°, V = 2027.2（7） A3, Z = 1, μ = 1.629 mm^-1, Dc = 1.710 mg/m3, T = 193（2） K, CsoH86Ag6N12O2S6, Mr = 2087.25, F（000） = 1044, S = 1.034, R = 0.0355 and wR = 0.0709. In 1.2MeOH, six silver（I） atoms are held together by six bzdmpymt ligands through N and S atoms to form a water-wheel-shaped structure. Each Ag atom is coordinated by two S atoms from two bzdmpymt ligands and one N atom from the third bzdmpymt ligand, giving a trigonal planar coordination geometry. Interactions between the CH3 group of bzdmpymt ligand and one pyrimidyl nitrogen atom in an adjacent molecule afford a one-dimensional hydrogen-bonding chain running along the b axis. The luminescent property of 1.2MeOH was also investigated.     

Synthesis and Crystal Structure of a Ni（Ⅱ） Complex of 2＇-[4-N,N＇-（Dimethylaminobenzyl- idene）]-3,5-dihydroxybenzoylhydrazide and Its Spectral Properties

A new nickel（II） complex [NiL2]（DMF）4 （HL = 2＇-[4-N,N＇-（dimethylamino- benzylidene）]-3,5-dihydroxybenzoylhydrazide） has been synthesized and its structure was characterized by IR,UV-Vis,1H NMR and elemental analysis. The fluorescence emission mechanism of the complex was discussed by fluorimetric spectra. The single-crystal structure was determined by X-ray diffraction analysis. The crystal belongs to the triclinic system,space group P1 with a = 0.9918（4）,b = 1.1297（4）,c = 1.1331（4） nm,α = 76.860（7）,β = 75.105（6）,γ = 89.022（7）°,V = 1.1936（8） nm^3,Z = 1,μ = 0.472 mm^-1,Dc = 1.319 g/cm^3,F（000） = 502 and Rint = 0.0913. In the title compound,the nickel（II） atom is four-coordinated with two nitrogen atoms from amide and two oxygen atoms from keto group. The complex is centrosymmetric with nickel located at the center.     

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