[Rh(NH3)5Cl]WO4 crystal structure

At T 150 K the crystal structure of [Rh(NH₃)₅Cl]WO₄ is studied: a = 11.2374(4) Å, b = 8.4857(3) Å, c = 10.5326(3) Å, V = 1004.36(6) ų, space group Pnma, Z= 4, d _x = 3.117 g/cm³. In the structure, complex ions are bound by N—H…O hydrogen bonds, with the shortest ones of 2.85–2.94 Å. Ionic packing is shown to be considered as rhombohedral with a _t ≈ 5.26 Å, α_t ≈ 106°. Thermal properties of the salt are studied in the hydrogen atmosphere. The product of thermal decomposition at 750°C is a mixture of three solid solutions of Rh_x W _1- x based on fcc, bcc, and hcp structures. All the obtained phases are nanocrystalline. The sizes of coherent scattering regions are 10–12 nm.     

Synthese und Kristallstruktur des tetrameren Nitridokomplexes [Cu(CH3CN)4]2[W4N4Cl14(CH3CN)2]

Synthesis and Crystal Structure of the Tetrameric Nitrido Complex [Cu(CH₃CN)₄]₂[W₄N₄Cl₁₄(CH₃CN)₂] . The title compound has been prepared by the reaction of CuCl with WNCl₃ in acetonitrile solution, forming red, moisture sensitive crystals. They were characterized by IR spectroscopy and by an X-ray structure determination. Space group I2/a, Z = 4, 2 027 observed unique reflections, R = 0.049. Lattice dimensions at -80°C: a = 2 527.0, b = 971.9, c = 2 137.5 pm, β = 106.01°. The compound consists of [Cu(CH₃CN)₄]⁺ ions, which are arranged to form strands, and of anions [W₄N₄Cl₁₄(CH₃CN)₂]^2?, in which the tungsten atoms were located at the vertices of a square and are linked with one another via linear W?N? W bridges. Two of the four tungsten atoms have four chlorine atoms as terminal ligands, the other two tungsten atoms have three chlorine atoms and an acetonitrile molecule as terminal ligands.     

Tetramethylammoniumamalgam, [N(CH3)4]Hg8

Tetramethyl Ammonium Amalgam, [N(CH₃)₄]Hg₈ Crystals of tetramethyl ammonium amalgam with the composition [N(CH₃)₄]Hg₈ were prepared by electrolysis. According to temperature‐dependent X‐ray diffraction experiments the compound transforms into an amorphous product above 6 °C; the decomposition is a multi‐stage process as shown by DTA experiments. X‐ray examinations of crystalline aggregates indicate a structure of low symmetry with remarkable similarities to that of α‐Hg.     

Synthesis,structure, and thermal behavior of the complex {Co2[N(CH2CH2OH)3]2Cl2}Cl2

Russian Journal of General Chemistry - Complex {Co2[N(CH2CH2OH)3]2Cl2}Cl2 was obtained for the first time by the reaction of triethanolamine with cobalt chloride. It was characterized by the...     

一个新的二维配位聚合物:{Cu_2[C_(10)H_8Cl_2NO_4]_2[C_(10)H_8N_2]_3}_n的合成及其晶体结构

采用铜(Ⅱ)盐和3,5-二氯水杨醛缩丝氨酸以及4,4′-联吡啶在乙醇水溶液中合成了具有二维层状的配位聚合物.通过元素分析、红外光谱对该配位聚合物进行了表征,并利用X射线单晶衍射仪对其结构进行了鉴定.晶体结构表明,该标题配合物属三斜方晶系,空间群C2/c,晶胞参数为a=2.711(3)nm,b=2.711(3)nm,c=4.977(5)nm;α=90.00°,β=90.00°,γ=120.00°,V=3.167 8 nm3,Z=18,Dc=1.173 g.cm-3,F(000)=11 448,μ=0.807 mm-1,R1=0.078 8,wR2=0.187 2.     

Photogeneration of metastable side-on N2 linkage isomers in [Ru(NH3)5N2]Cl2, [Ru(NH3)5N2]Br2 and [Os(NH3)5N2]Cl2

Photogeneration of side-on N2 linkage isomers in [Ru(NH3)5N2]2+ and [Os(NH3)5N2]2+ is achieved by irradiation with lambda = 325 nm of powder samples at T = 80 K and detected by the downshift of the nu(N-N) vibration and by the heat release at elevated temperature due to the back switching of the side-on configuration to the ground state. The concentration of the transferred molecules is evaluated by the decrease of the area of the nu(N-N) or 2nu(N-N) vibrational bands. All characteristic changes between the linear Ru-N-N and side-on configuration are predicted by DFT calculations: the structure of the anion, shifts of the vibrations, electronic excitation energy, energetic position and sequence of the electronic orbitals, the potentials of the ground and relaxed metastable state with the activation energy, saddle points and energetic position of the minimum.     

Synthesis and crystal structure of the octahedral cluster complex [Th(DMSO)8Cl][Re6Se7Cl7]

A cluster complex of the composition [Th(DMSO)₈Cl][Re₆Se₇Cl₇] has been obtained by interaction of ThCl₄ solution in DMSO with a water solution of K₃[Re₆Se₇Cl₇] and KCl. The compound crystallizes in the rhombic space group Pbcm with unit cell parameters a = 12.262(2) Å, b = 19.653(6) Å, c = 23.603(6) Å, V = 5688(2) ų, Z = 4, d _calc = 3.282 g/cm³. The structure is built from centrosymmetric cluster anions [Re₆Se₇Cl₇]^3? and complex cations [Th(DMSO)₈Cl]³⁺ possessing mirror-plane symmetry, half of the DMSO ligands being doubly disordered.     

Unique Isle Anion [Cu6Cl10]4- in π-Complex of Cu(I) Chloride with 1-(2-Pyridyl)-4-allyl-piperazinium. Synthesis and crystal structure of [(C5H4NH)NC4H8NH(C3H5]2+[Cu3Cl5]2-

Single crystals of [(C₅H₄NH)NC₄H₈NH(C₃H₅)]²⁺[Cu₃Cl₅]^2? are obtained by ac synthesis in ethanol from 1-(2-pyridyl)-4-allyl-piperazinium and Cu(II) dichlorides and their structure is studied by X-ray diffraction analysis (space group P-1, a = 7.246(7) Å, b = 8.54(1) Å, c = 16.41(1) Å, α = 70.76(8)°, β = 77.24(8)°, λ = 80.42(9)°, V = 30(4) ų, Z = 2, R(F) = 0.0686. In the structure of this π-complex, the Cu and Cl atoms form unusual centrosymmetrical Cu₆Cl₁₀ fragments, each fragment being bonded to two 1-(2-pyridyl)-4-allyl-piper-azinium cations via π-interaction Cu-(C=C). A three-dimensional structure is formed by means of N-H…Cl hydrogen bonds. The trigonal-pyramidal surrounding of the Cu(1) atom includes three Cl atoms and the C=C bond, while the tetrahedral surrounding of Cu(2) and the trigonal surrounding of Cu(3) involve the Cl atoms only.     

Aminoguanidinium cations and the square-bipyramidal hexachlorocuprate(II) anion in the (CH8N4)2[CuCl6] crystal structure

Synthesis and structure of a novel thermochromic complex (CH₈N₄)₂[CuCl₆] are reported. X-ray analysis of the compound was carried out for a single crystal 0.4×0.2×0.05 mm in size (a bright-yellow plate). The monoclinic unit cell parameters are a=7.167(1), b=15.561(3), c=7.328(1) Å, β=118.73(3)°, V=716.7(2) ų, space group P2₁, Z=2 (CH₈N₄)₂[CuCl₆] d_calc=1.99 g/cm³, μ(MoK_α)=2.65 mm^?1, R=0.0264, and R_w=0.0290 for 1411 I_hkl>2σ_I.     

配合物[Fe(OPPh3)4Cl2][FeCl4]的合成和晶体结构

亚砜（R2SO4）是四价有机硫化合物中最重要的一类化合物,它的还原产物R2S可作为配体与过渡金属离子配位,从而得到许多结构新颖的化合物。这类反应一般在金属离子Os^11、Ru^11、Pt^11和Re^Vi等存在下发生,但很少出现在Fe^Ⅲ离子上。本文首次利用FeCl3、PPh3和DMSO反应,得到标题配合物并测定了其晶体结构。     

Crystal structure of the dichlorobis(1-allyltetrazole-N4)copper(II) complex [Cu(1-CH2=CHCH2−N4CH)2Cl4/2]∞∞

The crystal structure of the dichlorobis(1-allyltetrazole-N⁴)copper(II) complex was determined by X-ray diffraction analysis. The crystals are monoclinic, a=14.233(3), b=6.755(1), c=7.273(1) Å, β=104.63(3)°, V_cell=676.6(2), ų, space group P2₁/c, Z=4, d_calc=1.741g/cm³, d_msd=1.69 g/cm³, CAD-4, λMoK_α radiation, R_F=0.0377 for 520 F_hkl>4σ(F_hkl) and 0.0560 for all 872 independent reflections. The structure is layered; the coordination polyhedron of copper is a square bipyramid, in which the equatorial positions are occupied by two chlorine atoms (Cu?Cl 2.27(2)–2.31(2) Å) and two N⁴ atoms of planar tetrazole ligands, whereas the axial positions are occupied by two chlorine atoms of the neighboring molecules of the complex (Cu?Cl 2.97(2)–3.01(2) Å). The sublattice of chlorine atoms is disordered in such a way that the [CuCl_4/2]_∞∞ layer is a superposition of two variants with weights 61(3) and 39(3)% and with similar geometrical characteristics: the equatorial chlorine atoms in variant A are replaced by the axial atoms in variant B and vice versa. The tetrazole ligand has the same position in both variants. In general, the crystal is a polytype with random alternation of A and B type blocks. It is shown that the compound is isostructural to the complex with 1-ethyltetrazole [Cu(ettz)₂Cl₂], in which only variant B is realized.     

铜配合物[Cu(AFO)2(N3)2](DMF)(H2O)的合成和晶体结构(AFO=4,5-二氮芴-9-酮)

近年来,利用晶体工程方法设计裁剪和组装具有一维、二维、三维框架结构的固体化合物材料已成为材料科学和化学学科中最活跃的研究领域之一。研究表明在这些框架内镶嵌活性组分可得到新型功能材料,如磁性材料、非线性光学材料及新型催化剂等[1]。而叠氮根是一个多功能桥联配体,它能形成一维[2],二维[3],三维[4]等配合物,有关叠氮根的磁性研究也成为分子基铁磁体研究的一个重要方面[5]。本文报道了[Cu(AFO)2(N3)2](DMF)(H2O)(DMF=N,N 二甲基甲酰胺)配合物的合成和晶体结构,并进行了元素分析和红外光谱表征。1　实验部分1 1　试剂与…