Synthesis of Several 2-Azafluorenones and 5H[1]Benzopyrano[3,4-c]Py Riding-Ones

Convenient syntheses of 2-azafluorenones 5a-f and 5H[1]benzopyrano[3,4-c]pyridin-5-ones 6a-b were performed by using intramolecular cyclization of 4-arylnicotinic acids 4a-F. 4a-f were obtained via permanganate oxidation from the corresponding of 4-arylpyridines 3a-f in good yields.     

[WS4Cu2（Py）4]的合成及晶体结构

(NH_4)_2WS_4、CuCl和(n-Bu)_4NBr在Ar气氛中,90℃下反应10 h,所得产物先后经CH_2Cl_2与CH_3OH处理,得一桔红色晶体。该晶体与吡啶反应,即得到桔红色针状晶体[WS_4Cu_2(Py)_4],属单斜晶系,空间群C2/c,晶胞参数:a=14.109(1),b=12.704(1),c=14.071(1);β=96.97(1)°;Z=4。结构用重原子法解出,经最小二乘法修正,偏离因子R=0.027。     

Strukturen von planaren und tetraedrischen TetrafulminatoMetallkomplexen: [N(C3H7)4]2 [Ni(CNO)4], [N(C3H7)4]2 [Pt(CNO)4] und [N(C3H7)4]2 [Zn(CNO)4]

Pseudohalogeno Metal Compounds. LXXVIII. Structures of Planar and Tetrahedral Tetrafulminato Metal Complexes: [N(C₃H₇)₄]₂ [Ni(CNO)₄], [N(C₃H₇)₄]₂ [Pt(CNO)₄], and [N(C₃H₇)₄]₂ [Zn(CNO)₄] The crystals contain the tetrafulminatometallates of an ideal square planar structure ([Ni(CNO)₄]^2–, [Pt(CNO)₄]^2–) with D_4h symmetry at the nickel and platinum atom and a tetrahedron ([Zn(CNO)₄]^2–) with perfect T_d symmetry at the zinc atom and with linear C≡N–O ligands. The metal carbon bonds (Ni–C: 187 pm, Pt–C: 200 pm, Zn–C: 201 pm) of the metal fulminates are very close to those of the corresponding cyano complexes. In the crystals the anions ([Ni(CNO)₄]^2–, [Pt(CNO)₄]^2–, [Zn(CNO)₄]^2–) are separated by the cations ([N(C₃H₇)₄]⁺) which explains the thermal stability of these compounds.     

Pyridinium‐Chlorometallate von Lanthanoid‐Elementen. Die Kristallstrukturen von [HPy]2[LnCl5(Py)] mit Ln = Eu,Er, Yb und von [H(Py)2][YbCl4(Py)2] · Py

Pyridinium Chlorometallates of Lanthanoid Elements. Crystal Structures of [HPy]₂[LnCl₅(Py)] mit Ln = Eu, Er, Yb und von [H(Py)₂][YbCl₄(Py)₂] · Py The pyridinium chlorometallates [HPy]₂[LnCl₅(Py)] with Ln = Eu, Er and Yb, as well as [H(Py)₂][YbCl₄(Py)₂]·Py have been obtained by the reaction of diacetone alcohol with solutions of the corresponding metal trichlorides in pyridine at 100 °C. According to the crystal structure determinations the anions [LnCl₅(Py)]^2— are linked by bifurcated Cl···H···Cl bridges with the protons of the [HPy]⁺ cations forming chains along [001]. The anions of [H(Py)₂][YbCl₄(Py)₂]·Py form discrete octahedrons with trans‐positions of the pyridine ligands. [HPy]₂[EuCl₅(Py)] ( 1a ): Space group Pnma, Z = 4, lattice dimensions at —80 °C: a = 1874.4(2), b = 1490.2(2), c = 741.5(1) pm, R₁ = 0.0466. [HPy]₂[ErCl₅(Py)] ( 1b ): Space group Pnma, Z = 4, lattice dimensions at —80 °C: a = 1864.3(1), b = 1480.7(2), c = 739.7(1) pm, R₁ = 0.0314. [HPy]₂[YbCl₅(Py)] ( 1c ): Space group Pnma, Z = 4, lattice dimensions at —80 °C: a = 1858.9(2), b = 1479.0(1), c = 736.8(1) pm, R₁ = 0.0306. [H(Py)₂][YbCl₄(Py)₂]·Py ( 2 ·Py): Space group Ia, Z = 4, lattice dimensions at —80 °C: a = 1865.5(1), b = 827.5(1), c = 1873.4(1) pm, ß = 103.97(1)°, R₁ = 0.0258.     

Co[(C6H11O)2PS2]2·2Py的合成和晶体结构

二烃基二硫代磷酸酯及其过渡金属配合物能阻止烃类自动氧化,是一种很重要的抗氧、抗磨广泛应用于石油的添加剂、高分子材料的稳定剂和人造橡胶的硫化促进剂[1,2].在生物学上也具有十分重要的地位,具有杀虫、抗菌、抗癌和抑制酶水解等特性[3].因此,对该领域的研究也十分活跃.对二烃基二硫代磷酸酯合过渡金属配合物及其加合物的研究,游效曾等已作过多次报导[4-16].     

Schwingungs-Resonanz-Raman-Spektren von [n-(C4H9)4N]2[OsBr6] bei 77 K

Vibrational Resonance Raman Spectra of [n-(C₄H₉)₄N]₂[OsBr₆] at 77 K A rotating Raman cell in the 180° scattering geometry is described. It permits the measurement of Raman spectra of deeply coloured solids and liquids at the temperature of liquid nitrogen. Meaningful polarization measurements on solid samples are obtained by the use of optically isotropic pellets of tetraalkylammonium complex salts. In the solid state [n-(C₄H₉)₄N]₂[OsBr₆] displays a rigorous resonance Raman effect. Especially the excitation at 454.4 and 457.9 nm coincides with an intense electric dipole allowed charge-transfer transition of the anion, so that as far as nine overtones of the totally symmetric stretching vibration A_1g and many combination tones of this vibration with the other ra-active fundamentals are to be observed. The determination of the spectroscopic constants ω₁ and x₁₁ demonstrates, that the deviations from the harmonic oscillator are within the limit of error.     

Two New Modifications of [P(C6H5)4]2[Cu2I4]

Single crystals of two new modifications of [P(C₆H₅)₄]₂[Cu₂I₄] were obtained by reaction of granulated copper with iodine and [P(C₆H₅)₄]I in dry acetone under nitrogen atmosphere. They crystallise monoclinically, space group P2₁/n (No. 14), a = 11.550(6), b = 7.236(2), c = 27.232(13) Å, β = 98.13(3)°, V = 2253(2) ų, and Z = 2 ([P(C₆H₅)₄]₂[Cu₂I₄]-C), and space group Cc (No. 9), a = 17.133(5), b = 15.941(5), c = 18.762 (6) Å, β = 114.02(1)°, V = 4681(3) ų, and Z = 4 ([P(C₆H₅)₄]₂[Cu₂I₄]-D), respectively. In these compounds the [CuI₂]^? anions form dimers di-μ-iodo-diiodocuprate(I), which are either planar ( C ) or folded ( D ).     

Synthesis and Crystal Structure of Dinuclear Copper Complex[Cu（CH2O（C6H4）N=C（C6H4）O）（Py]2

1 INTRODUCTION Synthesis of transition metal complexes with Schiff-base has been a subject of considerable importance [1,2]. They are not only good complexing agents for Schiff-base, but also good bactericide and antitumour agent [3,4]. At present, there is a spectacular growth in this field. Recently, some bridged binuclear complexes have received much attention on account of their biological relevance and condensed-phase magnetic properties[5,6]. Especially, the complexes containin…     

Characterization of [Ni(Py)4]Br2 and its thermal decomposition

The stepwise thermal decomposition of [Ni(Py)₄]Br₂ was studied by means of a derivatograph. By the introduction of a larger halide atom than Cl the degradation mechanism became simpler. The solid intermediates and the starting material was also analysed with X-ray powder diffraction methods and the unit-cell dimensions were calculated.

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Zusammenfassung Mittels eines Derivatographen wurde die stufenweise thermische Zersetzung von [Ni(Py)₄]Br₂ untersucht. Mit Einbringung eines größeren Halogenidatomes als Cl gestaltet sich der Abbaumechanismus einfacherer. Feste Zwischenprodukte und Ausgangsmaterialien wurden ebenfalls mittels Röntgenpulverdiffraktionsmethoden untersucht und die Gitterzellenkonstanten berechnet.

     

[C4N2H12]1.5[Zn2(PO4)(HPO4)2]·H2O晶体的合成与表征

由于在电学、磁学、光学、吸附、离子交换和催化等领域具有潜在的应用价值,具有开放骨架结构的金属磷酸盐的合成一直受到人们的广泛关注。在这些磷酸盐微孔化合物中,磷酸锌晶体是拓扑结构最为丰富的一种犤1犦。自从Stucky等犤2犦报道具有SOD、Li-ABW、FAU等已知结构磷酸锌的合成以来,已经有近百种具有0-D犤3,4犦,1-D犤5,6犦,2-D犤7～9犦,3-D犤10～13犦结构的磷酸锌被成功地合成出来。其中令人瞩目的是具有螺旋孔道的手性磷酸锌犤14犦以及具有二十四元环孔道的两种微孔磷酸锌化合物犤15,16犦的合成。这些化合物大多是采用水热技术以有…