Mössbauer spectroscopic and X-ray diffraction study of the thermal decomposition of Fe(CH3COO)2 and FeOH(CH3COO)2

Thermal decomposition of iron(II) acetate, Fe(CH₃COO)₂, and iron(III) acetate hydroxide, FeOH(CH₃COO)₂, has been studied using⁵⁷Fe Mössbauer spectroscopy and X-ray diffraction. Samples were thermally treated in air atmosphere between 150°C and 1000°C. The formation of maghemite '-Fe₂O₃, and hematite, -Fe₂O₃, is discussed. Hematite appears as the final decomposition product.     

The structure and spectra of bis(ethylenediamine)nickel(II)-tetracyanopalladate(II), Ni(NH2CH2CH2NH2)2Pd(CN)4

The structure of bis(ethylenediamine)nickel(II)tetracyanopalladate(II), Ni(NH₂CH₂CH₂NH₂)₂Pd(CN)₄, has been determined from three-dimensional X-ray data, using Weissenberg photographs. The compound crystallizes with two molecules in the monoclinic space group P2₁/n with a=7.174(10), b=10.740(15), c=10.135(15) Å, =115.0(5)°. The measured and the calculated density is 1.83 g/cm³. Anisotropic refinement gave a finalR factor of 10.2%. The structure consists of infinite chains, -Pd-C-N-Ni-N-C-, parallel to thec-axis. Two trans-nitrogen atoms of the square Pd(CN) ₄ ^2– are linked to Ni, leading thus to a polynuclear compound with an octahedral [NiN₆] group in agreement with visible and infrared spectra. The trans-Ni(NH₂CH₂CH₂NH₂)₂(NC)₂-group has an asymmetric gauche ()-conformation. Average distances are: Pd-C: 1.96 Å, CN: 1.15 Å, Ni-N: 2.08 Å.

---

Zusammenfassung Die Struktur von Bis(äthylendiamin)nickel(II)-tetracyanopalladat(II), Ni(NH₂CH₂CH₂NH₂)₂Pd(CN)₄, wurde mit Hilfe von Weissenbergaufnahmen ermittelt. Die Substanz kristallisiert mit zwei Formeleinheiten in der monoklinen Raumgruppe P2₁/n mit den Zelldimensionen a=7,174(10), b=10,740(15), c=10,135(15) Å, =115,0(5)°. Die gemessene und die berechnete Dichte betragen beide 1,83 g/cm³. Die, Verfeinerung unter Berücksichtigung anisotroper Temperaturfaktoren führte zu einem. R-Wert von 10,2%. Unendlich lange-Pd-C-N-Ni-N-C-Ketten sind parallel derc-Achse angeordnet. In Übereinstimmung mit den Spektren im sichtbaren und infraroten Bereich handelt es sich um einen polynuklearen Komplex, indem die trans-Cyanidgruppen von Pd(CN) ₄ ^2– als ambidente Liganden zu einer oktaedrischen [NiN₆]-Koordinationseinheit führen. Die trans-Ni(NH₂CH₂CH₂NH₂)₂(NC)₂-Gruppe weist eine asymmetrische gauche ()- Konformation auf. Mittlere Atomabstände betragen: Pd-C=1,96 Å. CN=1,15 Å, Ni-N=2,08 Å.

---

Résumé La structure du tétracyanopalladate (II) de bis (éthylènediamine) nickel (II) a été déterminée à partir de données tri-dimensionnelles aux rayons X, avec des photographies de Weissenberg. Le composé cristallise avec deux molécules dans le groupe spatial monoclinique P2₁/n avec les param ètres a=7.174 (10), b=10.740 (15), c=10.135 (15) Å, =115.0 (5)°. La densité mesurée et calculée est 1,83 g/cm³. L'amélioration anisotrope donne un facteurR final de 10,2%. La structure se présente comme des chaînes infinies -Pd-C-N-Ni-N-C, parallèles à l'axec. Deux atomes d'azote trans du groupe carré Pd(CN) ₄ ^2– sont liés à Ni, conduisant ainsi à un composé polycyclique avec un groupe [NiN₆] octaédrique, ce qui est en accord avec le spectre visible et infra-rouge. Le groupe trans-Ni (NH₂CH₂CH₂NH₂)₂(NC)₂ a une conformation assymétrique gauche (). Les distances moyennes sont Pd-C: 1,96 Å, CN:1,15 Å, Ni-N: 2,08 Å.

---

---

Dedicated to the memory of Professor Hans-Ludwig Schläfer.     

Synthesis and Characterization of [NH3（CH2）2NH2（CH2）2NH3]BiCl6

1 INTRODUCTION During the past decade, a series of organic-inor- ganic hybrid compounds based on metal halide units have been prepared and studied[1]. The combination of organic and inorganic components at the mole- cular level affords us the opportunity to design new hybrid materials and modulate the properties of components[2]. As a result, some interesting proper- ties, such as non-linear optical[3], interesting magne- tic[4], efficient luminescence[2], ideal thermal and mechanical sta…     

[(NH2CH2CH2NH3)2WⅥO2(NHC6H4NH)2]2(NH2CH2CH2NH2)·H2O配合物的合成与晶体结构

Cis-dioxo-tungsten(Ⅵ) complex, (NH₂CH₂CH₂NH₂)[(NH₂CH₂CH₂NH₃)₂W^ⅥO₂(NHC₆H₄NH)₂]₂·H₂O is synthesized at room temperature by the reaction of sodium tungstate with o-phenylenediamine. The crystal structure of complex was determined by X-ray diffraction structural analysis. The results show that complex belongs to monoclinic system with space group P2₁/ c, a=0.712 8(2) nm, b=3.081 1(10) nm, c=0.981 9(3) nm, β=102.615(4)°, V=2.104 4(11) nm³, Z=2, μ=55.26 cm^-1, F(000)=1 176. Compared the complex with its analogous biomimetic complexes of the cofactor of molybdoenzymes and tungstoenzymses, it is found that the variance of the coordination atoms and the metal ions center have no influence on the coordination feature, and exhibits distored octahedral coordination with cis-dioxo o-phenylenediamine. CCDC: 252834.     

[Pd(CH3COO)2]n from X‐ray powder diffraction data

The water‐insoluble title compound, catena‐poly­[palladium(II)‐di‐μ‐acetato‐κ⁴O:O′], [Pd(C₂H₃O₂)₂]_n, was obtained from a nitratopalladium solution and acetic acid as a pale‐pink powder. Ab initio crystal structure determination was carried out using X‐ray powder diffraction techniques. Patterson and Fourier syntheses were used for atom location and the Rietveld technique was applied for the final structure refinement. The structure consists of palladium acetate complexes connected into polymeric chains running along b, in which two Pd atoms are bridged by two acetate groups that are in a cis configuration with respect to one another. The unique Pd atom lies on a site with 2/m symmetry and the acetate moieties have imposed m symmetry; these are joined into infinite chains running along the b direction. The shortest Pd⋯Pd distance in the row is 2.9192 (1) Å. The planes of adjacent palladium complexes are inclined towards each other, the angle between the planes being approximately 30°.     

Struktur und thermische Zersetzung von Bis(triethanolamin)kupfer(II)-acetat [Cu{N(CH2CH2OH)3}2](CH3COO)2

Structure and Thermal Decomposition of Bis(triethanolamine)copper(II) Acetate [Cu{N(CH₂CH₂OH)₃}₂](CH₃COO)₂ Bis(triethanolamine)copper(II) acetate [Cu{N · (CH₂CH₂OH)₃}₂](CH₃COO)₂ was prepared using the basic components; the structure was determined by single crystal X-ray diffraction. The complex crystallizes in the monoclinic space group P2₁/c with a = 9.101 Å, b = 13.136 Å, c = 9.819 Å, β = 111.63°. Details of the synthesis, X-ray data, and the thermal decomposition are reported.     

含有NH2CH2CH2CH2NH2和o-C6H4(NH2)2配体的镍配合物的合成、结构和它们在乙烯聚合中的作用

两种镍的配合物[Ni(NH2CH2CH2CH2NH2)3]Cl2 (1)和[Ni(C6H4N2H4)2Cl2] (2)已经被合成并且通过红外和单晶X射线衍射分析对其进行了表征。在配合物1中,镍原子处于手性假八面体[NiN6]的几何构型中,它与三个1,3-丙二胺分子形成了三个六元环。在配合物2中,镍原子除了与两个o-苯二胺分子通过四个Ni-N键形成两个五元环外,它还与两个Cl原子配位形成了反式Ni-Cl2,这不同于以往报道过的镍的二胺配合物。这两个镍的配合物被MAO, MMAO或Et2AlCl活化后,对乙烯的二聚合或三聚合显示了很好的催化活性[对于配合物2,催化活性达到3.59×106 g mol-1 (Ni) h-1]。     

Blue-luminescent/electroluminescent Zn(II) compounds of 7-azaindole and N-(2-pyridyl)-7-azaindole: Zn(7-azaindole)2(CH3COO)2, Zn(NPA)(CH3COO)2, and Zn(NPA)((S)-(+)-CH3CH2CH(CH3)COO)2 (NPA = N-(2-pyridyl)-7-azaindole)

A new 7-azaindole zinc(II) compound, Zn(7-azaindole)2(CH3COO)2 (1), a new ligand N-(2-pyridyl)-7-azaindole (NPA), and two NPA zinc(II) complexes, Zn(NPA)(CH3COO)2 (2) and Zn(NPA)((S)-(+)-CH3CH2CH(CH3)COO)2 (3), have been synthesized and structurally characterized. Compound 1 has a tetrahedral geometry, whereas compounds 2 and 3 have irregular six-coordinate geometry. The NPA ligand in compounds 2 and 3 functions as a bidentate chelate to the zinc center. Compound 1 has a blue luminescence in the solution and the solid state. Compounds 2 and 3 emit a blue color in the solid state. In solution, compounds 2 and 3 are fluxional, as established by 1H NMR experiments. Compound 1 is thermally stable, whereas compounds 2 and 3 undergo decomposition when heated in the solid state. A blue electroluminescent device using compound 1 as the emitting layer has been fabricated. Crystal data: NPA, monoclinic, P2(1)/c, a = 13.993(5) A, b = 8.456(3) A, c = 16.886(5) A, beta = 104.666(12) degrees, V = 1932.9(11) A3; 1, triclinic, P1, a = 9.5114(18) A, b = 10.460(7) A, c = 11.002(3) A, alpha = 117.18(3) degrees, beta = 103.287(18) degrees, gamma = 90.94(2) degrees, V = 938.3(7) A3; 2, monoclinic, C2/c, a = 13.234(6) A, b = 9.373(3) A, c = 13.956(7) A, beta = 113.24(3) degrees, V = 1590.7(12) A3; 3, monoclinic, P2(1), a = 11.047(7) A, b = 15.343(9) A, c = 13.785(8) A, beta = 100.123(9) degrees, V = 2300(2) A3.     

Crystal structure of one of the strontium hydroacetates,Sr(H2O)2(CH3COO)2[H2(CH3COO)3]

All-Union Scientific-Research Institute for Chemical Reagents and Ultrapure Chemical Substances. Translated from Zhurnal Strukturnoi Khimii, Vol. 29, No. 1, pp. 104–108, January–February, 1988.     

Darstellung und Eigenschaften von W(CH3COO)2

Synthesis and Properties of W(CH₃COO)₂. W(Ac)₂ is reported for the first time. IR- and UV-spectroscopic investigations give indications concerning the structure of the compound. The IR-spectrum shows the bridging function of the acetate group. From the UV-spectrum the presence of a W? W bond is derived. Investigations of vapourization (mass spectrometer) and the behaviour in solution are explained by a polymeric structure     

配合物RuCl2(bdpx)(NHCH2CH2NH2)的合成及其催化活性

合成了一种新的双膦-钌-二胺配合物--RuCl2(bdpx)(NH2CH2CH2NH2)[bdpx=邻-二(二苯基膦)二甲苯](1),并研究了1催化苯乙酮(2)的加氢反应.在1 0.002 mmol,n(2):n(Me3COK):n(1)=10 000:120:1,氢气压力为3 MPa的条件下,于70℃反应4 h,2的转化率达100%.