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M. M. Monchak A. V. Pavlyuk V. V. Kinzhibalo M. G. Mys’kiv 《Russian Journal of Coordination Chemistry》2009,35(6):405-410
The alkylation of ethylenediamine with allyl bromide in the presence of a fourfold (with respect to ethylenediamine) molar
amount of NaHCO3 in acetone with an ethanol admixture (15: 1) affords LBr2 · 2H2O (I), where L2+ is the N,N,N,N′,N′,N′-hexaallylethylenediaminium cation. Single crystals of complexes L[CuII(Br0.45Cl3.55)] (II), L[Cu4I(Br4.55Cl1.45)] (III), and L[Cu4IBr6] (IV) are prepared by ac electrochemical synthesis from an ethanolic solution of LBr2 · 2H2O, CuCl2 · 2H2O (or CuBr2) at copper wire electrodes. The crystal structures of compounds I–IV are determined by X-ray diffraction analysis. The crystals of complex I are monoclinic: space group P21/n, a = 8.544(3), b = 10.404(3), c = 13.350(4) ?, β = 97.29(3)°, V = 1177.2(6) ?3, Z = 2. The bromine anions in compound I are bonded to the L2+ cations and water molecules through hydrogen contacts (E)H…Br (E = O, C) of 2.57(3)–2.86(3) ?. The crystals of compounds
II–IV are triclinic: space group P
. For II: a = 8.762(4), b = 9.163(4), c = 16.500(6) ?, α = 95.62(4)°, β = 96.39(4)°, γ = 111.46(4)°, V = 1211.4(9) ?3, Z = 2; for III: a = 9.074(4), b = 9.435(4), c = 9.829(5) ?, α = 116.12(4)°, β = 104.14(4)°, γ = 100.22(4)°, V = 692.3(6) ?3, Z = 1; for IV isostructural III: a = 9.084(4), b = 9.404(4), c = 9.869(4) ?, α = 116.31(3)°, β = 104.00(3)°, γ = 100.37(3)°, V = 692.1(5) ?3, Z = 1. Unlike the isolated tetrahedral CuX42− anion in structure II, an original chain anion (Cu4X62−)
n
is observed in the structures of π complexes III and IV.
Original Russian Text ? M.M. Monchak, A.V. Pavlyuk, V.V. Kinzhibalo, M.G. Mys’kiv, 2009, published in Koordinatsionnaya Khimiya,
2009, Vol. 35, No. 6, pp. 414–419. 相似文献
2.
Yu. I. Slyvka V. V. Kinzhibalo T. Lis B. M. Mykhalichko M. G. Mys’kiv 《Russian Journal of Coordination Chemistry》2009,35(4):307-311
A reaction of but-2-yne-1,4-diol with CuCl in a concentrated aqueous solution of piperazinium dichloride gave the π-complex
(PipH2)[CuCl2(HOCH2C≡CCH2OH)]2 · H2O ((PipH2)2+ is the piperazinium cation). The complex was examined by X-ray diffraction analysis (space group P
, a = 7.355(1) ?, b = 10.3572(8) ?, c = 13.632(2) ?, α = 101.055(9)°, β = 95.350(1)°, γ = 101.875(9)°, Z = 2). The complex consists of two crystallographically independent anions [CuCl2(HOCH2C≡CCH2OH)]− and the biprotonated piperazinium cation. The trigonal environment of the Cu(I) atom in either complex anion includes is
made up of two Cl atoms and the C≡C bond. Apart from the hydrogen bonds N-H⋯O that imparts a directed character to the ionic
interaction Cat+⋯An−, the piperazinium cation with molecules of crystallization water with bridging function form the cross-linking hydrogen bonds
N-H⋯OH2 and OH-H⋯Cl.
Original Russian Text ? Yu.I. Slyvka, V.V. Kinzhibalo, T. Lis, B.M. Mykhalichko, M.G. Mys’kiv, 2009, published in Koordinatsionnaya
Khimiya, 2009, Vol. 35, No. 4, pp. 311–315. 相似文献
3.
M. M. Monchak A. V. Pavlyuk V. V. Kinzhibalo V. V. Glukhyi M. G. Mys’kiv 《Russian Journal of Coordination Chemistry》2010,36(3):198-203
Alkylation of ethylenediamine with allyl bromide in the presence of NaHCO3 in benzene-ethanol and acetone-ethanol gave N,N,N′,N′-tetraallylethylenediamine L4 and N,N,N,N′,N′-pentaallylethylenediaminium bromide (L5(H+)Br2), respectively. The ac electrochemical synthesis at copper wire electrodes in solutions of copper(II) halide and an appropriate ligand yielded single crystals of Cu(I) complexes with ethylenediaminium ([L0(H+)2]0.5CuCl2 (I) and [L0(H+)2]0.5CuBr1.67Cl0.33 (II)) and its N-allyl derivatives N,N,N′,N′-tetraallylethylenediaminium ([{L4(H+)2}0.5Cu2Cl3] (III)) and N,N,N,N′,N′-pentaallylethylenediaminium ([L5(H+)Cu4Br6] (IV)). The crystal structures of complexes I–IV were determined by X-ray diffraction. The isostructural crystals of complexes I and II are triclinic, space group P $ \bar 1 $ , Z = 2. For I: a = 5.936(3), b = 6.387(3), c = 7.126(4) Å, α = 67.82(4)°, β = 72.98(4)°, γ = 67.55(4)°, V = 227.7(2) Å3. For II a = 6.110(3), b = 6.657(3), c = 7.309(3) Å, α = 68.40(3)°, β = 72.38(3)°, γ = 67.23(3)°, V = 250.4(2) Å3. In structures I and II, the organic cations are between infinite anionic chains (Cu 2 ? ) n . The crystals of π-complex III are triclinic, space group P $ \bar 1 $ , a = 6.851(4), b = 8.729(4), c = 9.960(4) Å, α = 98.25(3)°, β = 102.29(3)°, γ = 107.30(3)°, V = 541.8(5) Å3, Z = 2. In structure III, all the four allyl groups are π-coordinated by the metal atoms of four discrete anions Cu4Cl 6 2? . The crystals of π-complex IV are monoclinic, space group C2/c, a = 15.228(5), b = 17.095(6), c = 20.182(6) Å, β = 92.43(4)°, V = 5249(3) Å3, Z = 8. Only two of five allyl groups at the same N atom are coordinated by copper(I) atoms. Structure IV contains a complex inorganic fragment of the formula (Cu4Br 6 2? ) n . 相似文献
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A. V. Pavlyuk V. V. Kinzhibalo T. Lis M. G. Mys’kiv 《Russian Journal of Coordination Chemistry》2007,33(7):501-508
Crystals of the copper bromide complexes with N-allylisoquinolinium halides of the composition [C9H7N(C3H5)]2CuIICl2.86Br1.14 (I), [C9H7N(C3H5)]CuIBr2 · H2O (II), and [C9H7N(C3H5)]CuIBr2 (III) are prepared by ac electrochemical synthesis, and their structures are studied by X-ray diffraction analysis (DARCh-1 (for I) and KUMA/CCD (for II and III) diffractometers). The crystals of compound I are monoclinic: space group P21/n, a = 15.053(5) Å, b = 10.486(4) Å, c = 17.179(10) Å, γ = 109.77(3)°, V = 2552(4) Å3, Z = 4. The crystals of complex II are triclinic: space group P $\overline 1 $ , a = 7.040(1) Å, b = 7.610(2) Å, c = 12.460(2) Å, α = 79.54(3)°, β = 86.73(3)°, γ = 89.51(1)°, V = 655.4(2) Å3, Z = 2. The crystals of complex III are monoclinic: space group P21/n, a = 12.799(1) Å, b = 7.692(1) Å, c = 13.491(1) Å, β = 111.08(1)°, V = 1239.3(2) Å3, Z = 4. The structure of compound I is built of the CuIIX 4 2? tetrahedra and N-allylisoquinolinium cations united by the C-H···X contacts into corrugated layers. The crystal structure of π-complex II is formed of dimers of the composition [C9H7(C3H5)]2 Cu 2 I Br4 forming layers in the direction of the z axis due to the C-H···X contacts. An important role in structure formation belongs to water molecules that cross-link the organometallic layers through the O-H···X contacts into a three-dimensional framework. When kept in the mother liquor for 6 months, the crystals of compound II transformed into crystals of compound III, whose structure consists of {[C9H7(C3H5)]2Cu 2 I Br4} n columns united through the C-H···Br contacts (H···Br 2.84(3)?2.92(4) Å) into a three-dimensional framework. 相似文献
5.
Kinzhibalo V. V. Mys'kiv M. G. Davydov V. N. 《Russian Journal of Coordination Chemistry》2002,28(12):867-873
The crystals of [(CH2)6N4(C3H5)]Cu2Cl3 (I), [(CH2)6N4(C3H5)]Cu2Cl3 (II), and [(CH2)6N4(C3H5)]CuCl2 (III) complexes were electrochemically synthesized (ac) from CuCl2 · 2H2O and N-allylhexamethylenetetraminium chloride in ethanol solutions at pH 6, 4.5, and 3. Their structures were determined using X-ray diffraction analysis (DARCh diffractometer, MoK
radiation, /2 scan mode). Complex Icrystallizes in the monoclinic system: space group A2/a, a = 24.812(6) Å, b = 8.855(3) Å, c = 12.080(2) Å, = 89.21(3)°, and Z = 8. Complex II crystallizes in the triclinic system: space group P
, a = 7.618(2) Å, b = 7.048(2) Å, c = 13.150(3) Å, = 97.50(2)°, = 92.70(2)°, = 100.74(2)°, and Z = 2. The crystals of complex III are orthorhombic: space group Pmn21, a = 7.478(2) Å, b = 8.827(2) Å, c = 9.662(3) Å, Z = 2. The organic cation in complex I acts as a tridentate ,,-ligand; that in complex II, as a bidentate ,-ligand. In complex III, the organic cation is involved in coordination with the copper(I) atom only through one nitrogen atom. 相似文献
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