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1.
By alternating‐current electrochemical technique crystals of copper(I) π‐complex with 1‐allylpyridinium chloride of [C5H5N(C3H5)][Cu2Cl3] ( 1 ) composition have been obtained and structurally investigated. Compound 1 crystallizes in monoclinic system, space group C2/c a = 24.035(1) Å, b = 11.4870(9) Å, c = 7.8170(5) Å, β = 95.010(5)°, V = 2150.0(2) Å3 (at 100 K), Z = 8, R = 0.028, for 4836 independent reflections. In the structure 1 trigonal‐pyramidal environment of π‐coordinated copper(I) atom is formed by a lengthened to 1.376(2) Å C=C bond of allyl group and by three chlorine atoms. Other two copper atoms are tetrahedrally surrounded by chlorine atoms only. The coordination polyhedra are combined into an original infinite (Cu4Cl62—)n fragment. Structural comparison of 1 and the recently studied copper(I) chloride π‐complexes with 3‐amino‐, 2‐amino‐, 4‐amino‐1‐allylpyridinium chlorides of respective [LCu2Cl3] ( 2 ), [L2Cu2Cl4] ( 3 ), and [LCuCl2] ( 4 ) compositions allowed us to reveal the trend of the inorganic fragment complication which depends on pKa (base) value of the corresponding initial heterocycle. 相似文献
2.
Single crystals of [CuCl0.85Br0.15(C6H4N3CH2=CH2)] (I) were obtained by alternating current electrochemical synthesis; their X-ray structural investigation has been carried
out (DARCh automatic diffractometer, MoK
α radiation, θ/2θ scanning; 1460 reflections with F ≥ 4σ(F), R = 0.0517). The crystals are monoclinic, their space group is P21/c, a = 7.292(3) Å, b = 17.947(8) Å, c = 7.398(4) Å, β = 93.56(4)°, V = 966(1) Å3, Z = 4). Complex I is close in structure to the previously investigated compound [CuCl(C6H4N3CH2=CH2)] (II). In both structures, the trigonal-pyramidal surroundings of the copper atom include two halide atoms (one is apical),
a nitrogen atom, and a C=C group. The Cu2X2 dimers are associated into {[Cu2X2(C6H5N3CH2=CH2)]}n layers due to the bridging function of the 1-allylbenzotriazole molecule. In spite of the similar coordination polyhedra
of the metal atoms and identical bridging function of the ligand molecule in I and II, the differences in the conformation
parameters of the allyl group π-coordinated by the copper(I) atom (trans-like in I and cis-like in II) caused by the presence
of bromine atoms in the coordination sphere predetermine different structures of the organometallic [Cu2X2(C6H5N3CH2=CH2)]4 tetramer subunits in the layers and, as a consequence, formation of different crystal structures.
Original Russian Text Copyright ? 2005 by E. A. Goreshnik, B. M. Mykhalichko, and V. N. Davydov
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Translated from Zhurnal Strukturnoi Khimii, Vol. 46, No. 1, pp. 174–178, January–February, 2005. 相似文献
3.
Jagodič M. Vakulka A. Goreshnik E. Jagličić Z. Trontelj Z. 《Theoretical and Experimental Chemistry》2021,57(5):366-370
Theoretical and Experimental Chemistry - The magnetochemical behavior of the cis-[CuCl2(DMSO)2] complex was analyzed. cis-Complex crystals were found to be perfectly paramagnetic above 50 K and... 相似文献
4.
N2H6(Sb2F11)2 was synthesized by the reaction of N2H6F2 with excess of SbF5 in anhydrous hydrogen fluoride (aHF). It crystallizes in the triclinic space group P$\bar{1}$ (No. 2) with a = 6.6467(3) Å, b = 8.3039(4) Å, c = 8.3600(5) Å, α = 76.394(5) o, β = 70.161(5) o, γ = 70.797(5) o, V = 405.90(4) Å3 at 150 K, Z = 2. When it is redissolved in aHF, it solvolysis with the release of SbF5 yielding N2H6(SbF6)2 which crystallizes in the monoclinic C2/c space group (No. 15) with a = 7.3805(3) Å, b = 12.3248(5) Å, c = 10.4992(4) Å, β = 92.218(4) o, V = 954.33(7) Å3 at 150 K, and Z = 8. No other phases were observed in crystallization products when different molar ratios of N2H6F2/SbF5 (1:1,2:3,1:3) in aHF were used as starting materials. 相似文献
5.
Yu. I. Slyvka N. T. Pokhodylo E. A. Goreshnik M. G. Mys’kiv 《Journal of Structural Chemistry》2014,55(2):368-369
By the AgClO4 interaction with 1-allyl-5-(2-Pyridyl)-1H-tetrazolee (1aPyt) in a methanol solution, an [Ag2(1aPyt)2](ClO4)2 π-complex is obtained, which is studied using single crystal X-ray diffraction. 相似文献
6.
M. M. Monchak E. A. Goreshnik M. G. Mys’kiv 《Russian Journal of Coordination Chemistry》2011,37(2):143-148
The Eschweiler-Clarke reaction of ethylenediamine with formaldehyde and formic acid yielded N,N,N′,N′-tetramethylethylenediamine, which was alkylated with allyl chloride or allyl bromide to give the corresponding N,N′-diallyl-N,N,N′,N′-tetramethylethylenediaminium (L2+) dihalides. In methanolic solutions of copper(II) halide and an appropriate ligand, ac electrochemical synthesis with copper wire electrodes afforded single crystals of Cu(I) complexes with L2+: [L0.5CuCl2] (I), [L0.5CuCl0.72Br1.28] (II), and [L0.5CuBr2] (III). The crystal structures of complexes I–III were determined by X-ray diffraction study. The isostructural crystals of I and II are monoclinic, space group P21/n, Z = 4. For I: a = 7.632(4) Å, b = 11.318(5) Å, c = 10.635(5) Å, β = 98.551(7)°, V = 908.4(7) Å3. For II: a = 7.7415(7) Å, b = 11.4652(9) Å, c = 10.7267(10) Å, β = 98.351(4)°, V = 942.0(2) Å3. The organic cation L2+ acts as a bridge linking a pair of separate cuprous halide fragments Cu2X4. Although being isostoichiometric with I and II, complex III has a different structure. The crystals of III are monoclinic, space group P21/c, a = 6.519(2) Å, b = 9.060(3) Å, c = 16.284(6) Å, β = 97.219(4)°, V = 954.2(6) Å3, Z = 4. In structure III, the inorganic fragment forms infinite polymer chains (CuBr 2 ? ) n . The organic and inorganic parts are held together only by electrostatic interactions. Structures I–III are stabilized by hydrogen bonds (C)H…X (2.6–2.9 Å). 相似文献
7.
Pure [Cu(XeF2)2](SbF6)2 was prepared by the reaction of Cu(SbF 6) 2 with a stoichiometric amount of XeF2 in anhydrous hydrogen fluoride (aHF) at ambient temperature. The reaction between Cu(SbF6)2 and XeF2 (1:4 molar ratio) in aHF yielded [Cu(XeF2)4](SbF6)2 contaminated with traces of Xe 2F 3SbF6 and CuF2. The 6-fold coordination of Cu(2+) in [Cu(XeF2)2](SbF6)2 includes two fluorine atoms from two XeF2 ligands and four fluorine atoms provided by four [SbF6](-) anions. The neighboring [Cu(XeF 2)2](2+) moieties are connected via two [SbF6] units, with the bridging fluorine atoms in cis positions, into infinite [Cu(eta(1)-XeF2)2](cis-eta(2)-SbF 6)2[Cu(eta(1)-XeF 2)2] chains. Because of the high electron affinity of Cu(2+), coordinated XeF2 shows the highest distortion (Xe-Fb=210.2(5) pm, Xe-Ft=190.6(5) pm) observed so far among all known [M(x+)(XeF2)n](A)x (A=BF4, PF6, etc.) complexes. The four equatorial coordination sites of the Cu(2+) ion in [Cu(XeF 2) 4](SbF6)2 are occupied by four XeF 2 ligands. Two fluorine atoms belonging to two [SbF6] units complete the Cu (2+) coordination environment. The neighboring [Cu(XeF2)4](2+) species are linked via one [SbF6] unit, with bridging fluorine atoms in trans positions, into linear infinite [Cu(eta(1)-XeF2)4](trans-eta(2)-SbF6)[Cu(eta(1)-XeF2)4] chains. To compensate for the remaining positive charge, crystallographically independent [SbF6](-) anions are located between the chains and are fixed in the crystal space by weak Xe...F(Sb) interactions. 相似文献
8.
Crystal growth from anhydrous hydrogen fluoride solutions of M2+ (M=Cu, Ag) and [AuF6]− gave M(AuF6)2 salts (M=Cu, Ag). Similar attempts to prepare single crystals of the corresponding nickel, zinc and magnesium salts failed. The crystal structure of Cu(AuF6)2 consists of layers of Cu2+ cations connected by [AuF6]− anions, thus forming slabs. Only van der Waals interactions exist between adjacent slabs. The crystal structure of Ag(AuF6)2 consists of a three-dimensional framework in which Ag+ cations are linked by [AuF6]− anions. Both structures are members of the MII(XVF6)2 family, in which seven different structure types have been observed to date. In the crystal structure of O2(CuF)3(AuF6)4 ⋅ HF, the bridging AuF6 units connect [−Cu−F−Cu−F−]∞ chains to form stacks between which O2+ cations and HF molecules are located. 相似文献
9.
The structure of ammonium hexafluoroarsenate, NH4AsF6, has been determined by X‐ray diffraction using a single crystal grown from saturated solution in anhydrous HF. NH4AsF6 crystallizes rhombohedral with the KOsF6 structure type, with a = 7.459(3) Å, c = 7.543(3) Å (at 200 K), Z = 3, space group (No. 148). No phase transition was observed in the 100 K–296 K temperature range. The structure is dominated by regular AsF6 octahedra and disordered NH4+ cations. Raman spectrum of a single crystal of NH4AsF6 shows the bands at 372 cm?1, 572 cm?1, 687 cm?1 (AsF6?) and at 3240 cm?1 and 3360 cm?1 (NH4+). 相似文献
10.
Sergiy Minko Denys Usov Evgenij Goreshnik Manfred Stamm 《Macromolecular rapid communications》2001,22(3):206-211
Two‐component polymer brushes (polystyrene and poly(2‐vinylpyridine)) were synthesized by grafting from the surface of Si‐wafers. The brushes are sensitive to the surrounding medium, and their morphology and composition of the top of a brush can be switched upon exposure to different solvents. Thus surface energetic states and roughness of the film can be precisely tuned. 相似文献