Synthesis and X-ray Crystal Structure of a New Molecular Clip

The synthesis and X-ray crystal structure of a new molecular clip 2 was reported. It （C24H24N4O2, Mr = 400.47） crystallizes in the space group C2/c with a = 15.587（2）, b = 8.5805（12）, c = 15.259（2） A, β = 102.448（3）°, V= 1992.9 （5）A63, Z = 4, Dc = 1.335 g/cm63,μ = 0.087 mm^-1 and F（000） = 848. It remains monomeric in the crystal and a tape-like structure is formed in the crystal structure of molecular clip. The most unusual structural feature of 2 is the boat conformation of its cyclohexyl ring imposed by the ring fusion at C（9）-C（9a）.     

Synthesis,X-ray Molecular Structure,and Semiempirical Calculations of a New Heteroarylpiperazine Derivative

The new piperazine derivative (1) was synthesized by linking a coumarin system to a heteroarylpiperazine via a propyloxy chain. Its molecular structure, as determined by X-ray diffractometry is compared to those computed by three semiempirical methods. PM3 and MNDO give the best accuracy in reproducing the bond distances and angles, respectively. AM1 gives the best agreement with X-ray in reproducing the whole three-dimensional (3D) structure of this molecule. An analysis of these results at the light of other similar previously reported is carried out.     

The Synthesis,Crystal, Molecular and Electronic Structure of [ReCl2(NO)(py)3]

In line with our investigations of rhenium nitrosyl complexes, we have studied the reaction of [ReCl₃(NO)(OPPh₃)(PPh₃)] with pyridine. The [ReCl₂(NO)(py)₃] complex obtained in this reaction has been characterised by IR, electronic spectra and magnetochemical measurements; ligand field parameters and the electronic structure have been determined. The crystal and molecular structure of [ReCl₂(NO)(py)₃] has been solved by the heavy atom method. Crystals of [ReCl₂(NO)(py)₃] contain distorted octahedral molecules with the pyridine ligands in the mer-arrangement. The nitrosyl group is coordinated linearly to the rhenium atom as NO⁺.     

Synthesis,Crystal Structure and Stability Studies of Dithiocarbamate Complexes of Some Transition Elements (M=Co,Ni, Pd)

Single-crystal x-ray structure determinations have been recorded at 295 K for the dithiocarbamate metal compounds [Co(Et₂dtc)₃], [Co(nPr₂dtc)₃], [Pd(iPr₂dtc)₂] and [Pd(Et₂dtc)₂]. The stability constants(K) in EtOH of dialkyldithiocarbamate metal complexes [M(R₂dtc)_n] (M=Co, Ni, Pd. R=Me, Et, iPr, nPr. n=2, 3. dtc=dithiocarbamate) are determined by UV-vis data. The stability of the metal complexes increases in the order: Co<Ni<Pd. The effects of alkyl groups on the stability of [M(R₂dtc)₂] (M=Ni and Pd) increase in the order: Me<Et<nPr<iPr, and [Co(R₂dtc)₃] decrease in the order: Et>iPr>nPr>Me. The results obtained from this study confirm that the stability due to alkyl groups may be partly attributed to changes in the residual positive charge and also partly to steric hindrance of branched alkyl-groups. The comparison between the solid and solution states shows that the [M(R₂dtc)₂] (M=Pd, Ni) complexes have similar changes in M-S distance and stability with change in alkyl group. [M(iPr₂dtc)₂] has the shortest M-S distance and the highest stability in solution.     

一些二茂铁苯基亚胺化合物的合成与表征

通过回流对应的二茂铁苯胺和芳香醛的混合物的同样路径合成了一系列新颖的二茂铁苯基亚胺化合物(5~12)。当暴露于空气时化合物5~12稳定,不发生任何分解。所有化合物均用¹H、¹³C NMR,MS,IR,UV-Vis和元素分析表征。还报导了化合物N-(3-bromo-2-hydroxylbenzylidene)-4-ferrocenylimine(10)的单晶结构,其结晶属单斜晶系P2₁/c空间群。     

一些二茂铁苯基亚胺化合物的合成与表征

通过回流对应的二茂铁苯胺和芳香醛的混合物的同样路径合成了一系列新颖的二茂铁苯基亚胺化合物(5~12)。当暴露于空气时化合物5~12稳定,不发生任何分解。所有化合物均用¹H、¹³C NMR,MS,IR,UV-Vis和元素分析表征。还报导了化合物N-(3-bromo-2-hydroxylbenzylidene)-4-ferrocenylimine(10)的单晶结构,其结晶属单斜晶系P2₁/c空间群。     

An Expansion of Crystalline Sponge X-ray Analysis to Elucidate the Molecular Structure of Reactive Compounds via Ion Pair Formation

The crystalline sponge (CS) method allows structural elucidation of a target compound (guest) in solution by single crystal X-ray diffraction through trapping the guest into the CS framework. In principle, the CS method is inapplicable to reactive compounds that break the CS framework, such as acidic, basic, or nucleophilic ones. Here, a solution to this problem is disclosed wherein an ion pair of the guest compound is formed during the guest-soaking step by adding a suitable reagent. The ion pair can be observed and does not damage the CS framework. Using the developed method, amino, guanidino, and amidino compounds have been successfully analyzed as ion pairs with sulfonic acids. Practical utility has been shown because the absolute configurations of optically resolved amine derivatives were revealed with only a few micrograms. This demonstrates that the ion-pair-soaking method is simple and expands the range of compounds applicable to the CS method.     

Synthesis，X－ray Structure and Spectral Propertiesofa Tetra－component Heteropoly Compound

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Solution of the Crystal and Molecular Structure of Complex Low-Symmetry Organic Compounds with Powder Diffraction Techniques: Fluorescein Diacetate

Without any prior knowledge of the molecular structure , all 31 carbon and oxygen atoms of fluorescein diacetate were accurately located based on a high-resolution powder diffraction experiment. Direct methods and Fourier recycling were used. This represents a considerable advance with respect to the size of an organic molecule whose structure can be solved by ab initio methods from measurements on a powder.     

Synthesis of 1,2,4-substituted hexahydropyridazines and X-ray structural investigation of 4-hydroxyimino-2-methyl-1-phenethylhexahydropyridazine

A series of new 1,2,4-substituted hexahydropyridazines was prepared in order to evaluate qualitatively and quantitatively the role and influence of substituents on the biological activity of this system. An X-ray structural investigation of 4-hydroxyimino-2-methyl-1-phenethylhexahydropyridazine was performed. The compounds considered exhibit moderate local anesthetic, antihistaminic, and anticonvulsive activity.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 3, pp. 539–541, March, 1993.     

Synthesis,Molecular Structure,Optical Properties and Electrical Conductivity of Zwitterionic Ferrocenyldithiophosphonates

Ferrocenyldithiodiphosphetane [FcPS(μ‐S)]₂ [Fc = Fe(η⁵‐C₅H₄)(η⁵‐C₅H₅)] reacts with the aminoethanol derivatives 1‐ethyl‐3‐pyrrolidinol and 2‐(piperazin‐1‐yl)ethanol to give the zwitterionic (O‐ethylammonium)ferrocenyldithiophosphonates ( 2 ) and ( 3 ), which were fully characterized by elemental analysis, IR and NMR spectroscopy and mass spectrometry. The optical and electrical properties of 2 and 3 as well as those of the previously reported [FcP(S)S(OC₂H₄NHEt₂)] ( 1 ) were studied. A molecular structure determination of 1 is also reported.     

Synthesis and Crystal Structure of Some Macrocyclic Ring Compounds

A bola-shaped diester–dicarboxylic acid (L1H₂) synthesized with ethanediol spacer and phthalic anhydride head group is demonstrated to form various macrocyclic ring compounds such as M₁, M₂, and M₃. Compound M₁, containing both lactam [-C(=O)-N-H)] and lactone [-C(=O)-O-] functional groups, has a [16]-membered macrocyclic ring, while compound M₂, composed of only lactones [-C(=O)-O-], exists with a [19]-membered macrocyclic ring. Similarly, compound M₃, composed of Cu(II) metal ions, exists with a macrocycle-like [15]-membered chelate ring. In addition to the ¹H NMR spectra, the single crystals obtained for M₁ and M₃ thoroughly established, the formation of the ring structures. This article demonstrates the versatile capability of diester-dicarboxylic acid for forming various types of ring compounds, such as bis-chelate rings in M₃ and lactam cum lactone-type macrocyclic rings in M₁ and M_2.

The Molecular and Electronic Structure of [ReOX3(AsPh3)(OAsPh3)] Complexes (X = Cl,Br)

New rhenium oxo-complexes [ReOX₃(OAsPh₃)(AsPh₃)] (X = Cl and Br) have been synthesised and characterised by X-ray diffraction, IR, electronic and magnetochemical measurements. They were obtained in high yield in reactions between [ReOX₃(AsPh₃)₂] and acetonitrile in air.     

Synthesis,Spectra, Thermal Analysis and Crystal Structure of Trans-Bis(2-Pyridinepropanol)Bis (Saccharinato)Cobalt(II)

The title complex, [Co(pypr)₂(sac)₂] (pypr = 2-pyridinepropanol and sac = saccharinate), has been prepared and characterized by elemental analysis, electronic and FTIR spectra, magnetic susceptibility measurements, thermal analysis and X-ray diffractometry. The complex crystallizes in triclinic space group PI with a = 8.1836(2), b = 10.0062(2), c = 10.4989(3) Å, α = 90.474(1), β = 107.989(1) and γ = 110.923(1)°. The cobalt(II) ion sits on a center of symmetry and is octahedrally coordinated by two pypr and two sac ligands. Both pypr and sac ligands occupy the trans positions of the coordination octahedron. The two pypr ligands are neutral and act as bidentate N- and O-donor ligands forming two symmetry-related seven-membered chelate rings around the cobalt(II) ion, while both sac ligands are O-coordinated through the carbonyl oxygen atoms. On heating the endothermic removal of two pypr ligands occurs in the first stages of decomposition and at higher temperatures the Co/sac intermediate decomposes to Co₃O₄ and finally to CoO.     

Synthesis,Crystal and Molecular Structure of Tetrapyrrolidinyl PNP-lariat Ether Complex with Ki(H2O)2 Monohydrate

The crystal and molecular structure of the title compound, C₂₄H₅₀N₇O₈IKP₃ crystallizing in P2₁/c space group has been determined. The oxygen atoms of the crown ether exist in an almost ideal envelope conformation. The inorganic cyclophosphazene ring P₃N₃ is slightly deviated from planarity. All endocyclic P-N bond lengths are equal within experimental error with the mean value 1.585(5) Å. The K⁺ ion is coordinated by oxygen atoms from the crown ether and two water molecules but not by the cyclophosphazene nitrogen atom.     

3,1-苯并噁嗪化合物的合成及晶体结构

报道了一种用5-硝基-2-胺基苯甲腈为原料, 在二氯化锌催化下与环酮反应环化合成3,1-苯并噁嗪类化合物的新方法, 并用此方法合成了6-硝基-1,2-二氢-2,2-(1,5-亚戊基)-4-亚胺-4H-3,1-苯并噁嗪(4a). 产物经元素分析、红外光谱、核磁共振氢谱和碳谱进行了表征, 用X射线单晶衍射法测定了其晶体结构. 晶体属单斜晶系, P2₁/c空间群, a＝0.66339(13) nm, b＝2.5329(5) nm, c＝0.73756(15) nm, β＝91.85(3)°, V＝1.2387(4) nm³, Z＝4, D_c＝1.401 g/cm³, F(000)＝552, µ＝0.102 mm^－1, R＝0.0994, wR＝0.3001.     

Pyridazine Derivatives and Related Compounds,Part 221: Synthesis,Reactions, and Insecticidal Activity of 3-Amino-5,6-diaryl-1H-pyrazolo[3,4-c]pyridazines

Starting with 3-amino-5,6-diaryl-1H-pyrazolo[3,4-c]pyridazine, the syntheses of thiourea derivatives, dithiocarbamates, ethyl carbamate, phosphoranylidene amino, and substituted acetamido derivatives are described. The products were screened for their insecticidal activity against Mucsa, domestica, and Aphid, Macrosiphum pisi.

Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file.     

磷酸锰铝分子筛MnAPO-5的合成、结构与性能研究

在磷酸锰铝分子筛MnAPO-5纯相合成的基础上,研究了它的结构和物化性能。晶胞参数和红外光谱的测定结果表明它具有AlPO₄-5型分子筛的结构;顺磁共振和电子探针能谱分析及组成分析表明Mn(Ⅱ)结合到分子筛的骨架上。同时对其吸附性能,热稳定性表面酸性进行了研究。     

对-(二甲氨基)苯基锗倍半氧化物的合成、结构及其对体外培养癌细胞的作用

在常压下,由N,N′-二甲基苯胺和GeCl_4合成了对-(二甲氨基)苯基锗倍半氧化物,研究了它的红外光谱、光电子能谱及热分析性质,讨论了化合物的结构.用体外细胞培养法,观察了它对人乳腺癌细胞分裂的抑制作用。