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1.
New heteroligand Cu(II) and Zn(II) complexes with the α-naphthylacetic acid anion (NAA) and monoethanolamine (MEA), [M(NAA)2(MEA)2] (M = Cu2+, (I), Zn2+ (II)), are synthesized. The crystal structures of the obtained complexes are determined by X-ray diffraction analysis (CIF files CCDC 984097 (I) and 930946 (II)). The crystals are monoclinic, for I: a = 18.8140(9) Å, b = 4.82500(14) Å, c = 16.0360(7) Å, β = 115.135(6)°, V = 1317.87(11) Å3, space group P21/c, Z = 2; for II: a = 32.9760(14) Å, b = 5.0911(3) Å, c = 15.7994(10) Å, β = 94.418(5)°, V = 2644.6(3) Å3, space group C2/c, Z = 4. In the structure of complex I, the Cu2+ ion arranged in the symmetry center is coordinated at the vertices of the distorted octahedron by the oxygen atoms of two NAA molecules (Cu-O(2) 2.019(4) Å) and two MEA molecules. The latter is the bidentate-chelating ligand and coordinates the metal through the O and N atoms to form the five-membered metallocycle (Cu-O(3) 2.457(5), Cu-N(1) 1.986(5) Å). In complex II, the Zn atom (on axis 2) is coordinated at the vertices of the distorted tetrahedron by the oxygen atoms of two NAA molecules (Zn-O(2) 1.976(4) Å) and the nitrogen atoms of two MEA molecules (Zn-N 2.034(6) Å). The character of the interaction of coordinated NAA and MEA ligands and methods for packing complexes I and II are considered on the basis of the structural data.  相似文献   

2.
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   

3.
The first order rate constants for the tautomerization of the hydrio(alkynyl) clusters Ru3Pt(μ-H){μ42-C ≡ C1Bu}(CO)9(L2);1a: L2 = dppe,1b; L2 = dppet,1c; L2 = dppp and1d; L2 =S,S-dppb to the corresponding vinylidene clusters Ru3Pt{μ42-C = C(H)tBu}(CO)9(L2)2 have been measured, and they follow the orser1d <1a <1b1c. The reactions involving1a and1d exhibit an inverse kinetic deuterium isotope effect. The structures of1b, 2b, 2c, and2d were determined by X-ray crystallography, and are compared with those of1a and2a which have been previously reported. Crystal data for1b, space groupPbca,a = 13.338(4) Å,b = 17.771(6) Å,c = 36.092(8) Å,Z = 8,R(R w) = 0.059(0.058) for 2342 absorption corrected, observed data; for2b, space group P21/n,a = 10.566(2) Å,b = 20.234(5) Å,c = 20.270(3) Å,β = 96.11(1)°,Z = 4,R(R w) = 0.043(0.053) for 5865 absorption corrected, observed data; for2c, space group P21/n,a = 14.211(5) Å,b = 19.534(2) Å,c = 15.870(2) Å,β = 100.81(2)°,Z = 4,R(R w) = 0.055(0.031) for 6566 absorption corrected, observed data: for2d, space group P212121,a = 12.309(4) Å,b = 19.047(6) Å,c = 19.206(4) Å,Z = 4,R(R w) = 0.055(0.053) fpr 2151 absorption corrected, observed data. The fluxional behavior of1d and1e (which consists of two interconverting isomers) has been examined by variable temperature13C NMR spectroscopy and by31P EXSY.  相似文献   

4.
Four new fluorochromatouranylates, namely, K[UO2(CrO4)F] · 1.5H2O (I), Rb[UO2(CrO4)F] · 1.5H2O (II), Rb[UO2(CrO4)F] · 0.5H2O (III), and Cs[UO2(CrO4)F] · 0.5H2O (IV), have been synthesized, and their crystallographic characteristics have been determined. All the compounds crystallize in monoclinic system, space group P21/c, with the unit cell parameters a = 13.1744(5) Å, b = 9.4598(3) Å, c = 13.0710(4) Å, β = 103.746(1)°, Z = 4, R = 0.0235 (I); a = 13.5902(7) Å, b = 9.5022(4) Å, c = 13.2271(6) Å, β = 102.914(2)°, Z = 4, R = 0.0247 (II); a = 24.7724(8) Å, b = 12.6671(4) Å, c = 9.4464(3) Å, β = 97.661(1)°, Z = 8, R = 0.0448 (III); a = 25.725(1) Å, b = 12.8261(5) Å, c = 9.4929(4) β = 97.208(1)°, Z = 8 (IV). The pairs of compounds I and II and compounds III and IV are isostructural. Crystals of compounds I–III have been subjected to complete X-ray diffraction study. It has been established that the structures of compounds I–III are built of [UO2(CrO4)F] n n? layers, which are parallel to the (100) plane and linked into a framework by alkali-metal cations located between layers, together with water molecules. The effect of topological and geometric isomerism on the structural features of 34 known uranyl compounds of the AT3M2 crystallochemical group, to which the studied compounds I–III also belong, is discussed.  相似文献   

5.
Anhydrous and partially hydrated acid trinuclear trifluoroacetates of divalent transition metals of the composition [M3(CF3COO)6(CF3COOH)6)](CF3COOH) and [M3(CF3COO)6(CF3COOH)2(H2O)4)](CF3COOH)2, respectively, where M = Co (I, III) Ni (II, IV), were synthesized and studied by X-ray diffraction. Complexes I and II were obtained by crystallization from solutions of M(CF3COO)2 · 4H2O in trifluoroacetic anhydride; complexes III and IV were synthesized under the same conditions with the use of 99% trifluoroacetic acid as a solvent. Crystals I are triclinic: space group $P\bar 1$ , a = 13.199(6) Å, b = 14.649(6) Å, c = 15.818(6) Å, α = 90.04(4)°, β = 114.32(4)°, γ = 108.55(4)°, V = 2611.3(19) Å3, Z = 2, R = 0.0480. Crystals II are trigonal: space group $R\bar 3$ , a = 13.307(2) Å, c = 53.13(1) Å, V = 8148(2) Å3, Z = 6, R = 0.1112. Crystals III are triclinic: space group $P\bar 1$ , a = 9.001(8) Å, b = 10.379(9) Å, c = 12.119(9) Å, α = 83.67(5)°, β = 72.33(5)°, γ = 83.44(5)°, V = 1068.3(15) Å3, Z = 1 Å, R = 0.1031. Crystals IV are triclinic: space group $P\bar 1$ , a = 9.121(18) Å, b = 10.379(2) Å, c = 12.109(2) Å, α = 84.59(3)°, β = 72.20(3)°, γ = 82.80(3)°, V = 1080.94(40) Å3, Z = 1, R = 0.0334.  相似文献   

6.
It has been shown that N,N’-diaryldiaza-18-crown-6 ethers with p-dimethylamino-and p-methoxy groups in the benzene ring (aryl is 4-Mc2NC6H4) (I) and 4-MeOC6H4 (II) form complexes with potassium and barium salts. The influence of these salts on the UV and 1H NMR spectra of crown ethers I and II has been studied. The stability constants (logβ) of the complexes increase in the series II · Ba(ClO4)2 (2.0), I · Ba(ClO4)2 (2.3), II · KBr (2.8), I · KBr (3.0). N,N’-bis(4-dimethylphenylamine)diaza-18-crown-6 (L, I) and its complex with barium perchlorate Ba(ClO4)2 · L (III) are characterized by X-ray crystallography. The crystals of I are monoclinic: a = 13.778(2) Å, b = 5.9731(9) Å, c = 17.542(3) Å, β = 106.65(1)°, V = 1383.1(4) Å3, Z = 2, space group P21/n, R = 0.0374 for 990 reflections with I > 2σ(I). The crystals of III are monoclinic: a = 17.275(4) Å, b = 8.017(2) Å, c = 26.935(4) Å, β = 100.47(2)°, V = 3669(1) Å3, Z = 4, space group C2/c, R = 0.0320 for 1897 reflections with I > 2σ(I). The molecules of I and III are centrosymmetric. In III, the Ba atom is in the center of substituted diaza-18-crown-6 (DA18C6). The Ba atom is coordinated by all six donor atoms of diaza-18-crown-6 (av. Ba-O, 2.779(3) Å; Ba-N, 3.004(4) Å) and four oxygen atoms of two asymmetrically bound perchlorate groups (Ba-O, 2.832(4) and 3.031(4) Å) arranged below and above the plane of substituted diaza-18-crown-6. The conformations of the macrocycle in free and coordinated L are different.  相似文献   

7.
Tetraamminecobalt hydrogen hexamolybdoferrate [Co(NH3)4] · H[FeMo6O18(OH)6] · 6H2O (I) and tetraamminecobalt hydrogen hexamolybdogallate(III) [Co(NH3)4] · H[GaMo6O18(OH)6] · 6H2O (II) were synthesized and studied by mass spectrometry, thermogravimetry, IR spectroscopy, and X-ray diffraction. Crystals of I and II are monoclinic; a = 16.21 Å, b = 5.43 Å, c = 12.32 Å, β = 119.63°, V = 1092.11 Å3, ρcalcd = 2.21 g/cm3, and Z = 1 for I; a = 16.24 Å, b = 5.59 Å, c = 12.29 Å, β = 119.79°, V = 1064.05 Å3, ρcalcd = 2.15 g/cm3, and Z = 1 for II. Compounds I and II were used as catalysts for soft oxidation of natural gas.  相似文献   

8.
Two compounds of 2-ferrocenylmethylidenehydrazono-1,3-dithiane (1) and 2-ferrocenylmethylidenehydrazono-1,3-dithiepane (2) are synthesized and their single crystal structures are determined by the X-ray diffraction method. Compound 1 belongs to the orthorhombic Pca21 space group with the cell parameters: a = 13.989(4) Å, b = 5.785(2) Å, c = 18.231(5) Å, V = 1475.4(7) Å3; while compound 2 crystallizes in a monoclinic symmetry, P21/c space group with a = 15.320(2) Å, b = 5.8028(6) Å, c = 36.584(4) Å, β = 91.932(1)° and V = 3250.4(6) Å3.  相似文献   

9.
ZnPhen(EtOCS2)2 (I) and Zn(2,2′-Bipy)(n-BuOCS2)2 (II) mixed-ligand complexes have been synthesized. The structures were solved from X-ray diffraction data (CAD-4 and X8-APEX diffractometers, MoK α radiation, 1879 and 3637 F hkl , R = 0.0374 and 0.0315). Crystals I are monoclinic with parameters a = 11.678(3) Å, b = 19.215(3) Å, c = 9.655(1) Å; β = 101.23(1)°; V = 2125.0(7) Å3; Z = 4, space group P21/c; crystals II are triclinic with parameters a = 8.7875(3) Å, b = 11.833(1) Å, c = 13.3454(6) Å; α = 112.154(2)°, β = 108.503(1)°, γ = 92.787(2)°; V = 1196.2(1) Å3; Z = 2, space group 1 $P\bar 1$ . The structures are composed of discrete mononuclear molecules. The polyhedra of the Zn atoms are distorted trigonal bipyramids N2S3 formed by coordination of the N atoms of Phen or 2,2′-Bipy molecules and sulfur atoms of the monodentate and cyclic bidentate xanthogenate ligand. In structures I and II, dimer assemblies are formed by π-π interactions of Phen or 2,2′-Bipy molecules.  相似文献   

10.
The results of syntheses and X-ray diffraction analyses of mononuclear complexes [ML2(H2O)4] (M = Co2+(I), Cu2+(II), and Zn2+(III)) containing water molecules and anions of acetic acid α-(N-benzoxazolin-2-one) (L = C9H6O4) are presented. The crystals of complexes I–III are isostructural (space group P21/n, Z = 2) and are built of discrete neutral complex molecules. The crystallographic data are as follows: for complex I, a = 6.1470(5), b = 5.3310(3), c = 30.5894(17) Å, β = 95.056(6)°, V = 998.50(11) Å3; for complex II, a = 5.9661(6) Å, b = 5.1414(4) Å, c = 32.672(2) Å, β = 92.395(6)°, V = 1001.33(14) Å3; and for complex III, a = 6.1404(3) Å, b = 5.3476(2) Å, c = 30.5865(12) Å, β = 94.708(4)°, V = 1000.96(7) Å3. The metal atoms (M) of the complexing agents are localized in the crystallographic symmetry centers and have a distorted octahedral environment due to two oxygen atoms of the carboxy groups of two monodentate ligands (L) and four water molecules. The M-O(1w)(H2O) and M-O(2w)(H2O) bond lengths for the indicated complexes are 2.088(3) and 2.118(3), 2.446(3) and 1.971(3), and 2.113(4) and 2.093(3) Å for M = Co2+, Cu2+, and Zn2+, respectively. The crystal structures are formed due to packing of chains built of inter-molecular hydrogen bonds O-H…O.  相似文献   

11.
Mixed-ligand complexes of asymmetric gadolinium β-diketonates with 2,2′-bipyridyl (Bipy)—[Gd(Pa)3(Bipy)] (HPa is pivaloylacetone) (I) and [Gd(Pta)3(Bipy)] (HPta is pivaloyltrifluoroacetone) (II)-have been obtained by direct interaction of initial reagents and their structures have been studied by X-ray crystallography. Crystals of I are monoclinic: a = 9.536(1) Å, b = 15.037(1) Å, c = 13.280(1) Å, β = 109.56(1)°, V = 1798.7(3) Å3, Z = 2, space group P21. Crystals of II are triclinic: a = 9.6696(17) Å, b = 12.1348(9) Å, c = 18.243(3) Å, α = 100.257(12)°, β = 103.997(2)°, γ = 101.438(11)°, V = 1977.4(5), Z = 2, space group P $\bar 1$ . The coordination polyhedron of the central gadolinium atom in I and II is a distorted square antiprism formed by six oxygen atoms of the three β-diketonate ligands (av. Gd-O, 2.35(2) and 2.351(5) Å in I and II, respectively) and two nitrogen atoms of the Bipy ligand (av. Gd-N, 2.47(2) and 2.584(7) Å in I and II, respectively). Although the molecular structures of these complexes are similar, they have different crystal packings. In II, the planes of the Bipy ligands of neighboring molecules related by an inversion center are bound by stacking interaction (the distance between the Bipy planes is 3.45 Å). The structure and properties of these mixed-ligand complexes have been discussed based on the results of quantum-chemical density functional theory calculations (DFT/B3PW91). The nature of the substituents in the β-diketonate ligand has an effect on the structure and properties of the complexes. The correlation between the Gd-Dik and Gd (Dik)3-Bipy bond energies has been studied.  相似文献   

12.
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   

13.
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   

14.
[[UO2(L)(OH)] (I), (CN3H6)2[(UO2)2CrO4(L)4] · 2H2O (II), and [UO2(H2O)5][(UO2)2Cr2O7(L)4] (III) crystals, where L is picolinate ion C5H4NCOO?, have been synthesized and studied by X-ray diffraction and IR spectroscopy. Complex I crystallizes in triclinic system with the unit cell parameters a = 6.2858(5) Å, b = 7.9522(5) Å, c = 8.3598(6) Å, α = 79.527(6)°, β = 87.760(6)°, γ = 79.126(6)°, space group P $\bar 1$ , Z = 2, R = 0.0306, and complexes II and III crystalize in monoclinic system with a = 8.8630(9) Å, b = 13.4540(13) Å, c = 31.266(3) Å, β = 93.118(3)°, space group C2/c, Z = 4, R = 0.0187 (II), and a = 7.3172(4) Å, b = 15.4719(8) Å, c = 16.6534(10) Å, β = 98.943(4)°, space group P21/m, Z = 2, R = 0.0588 (III). The structure of complex I is built of electronegative [UO2(L)(OH)] chains, which belong to the AT11M2 crystallochemical group (A = UO 2 2+ , T11 = L, M2 = OH?) of uranyl complexes. The structure of complexes II and III contains [(UO2)2(L′)(L)4]2? dimers (L′ = CrO 4 2? or Cr2O 7 2? ), which belong to the A2B2B 4 01 group (A = UO 2 2+ ,B2 = L′, B01 = L). The specifics of intermolecular interactions in the structures of complexes I–III and some their analogues have been considered using molecular Voronoi-Dirichlet polyhedra.  相似文献   

15.
Two complexes are synthesized: diaquabromo(18-crown-6)rubidium [RbBr(18-crown-6)(H2O)2] (I) and triaqua(18-crown-6)barium dibromide monohydrate [Ba(18-crown-6)(H2O)3]2+ 2Br? · H2O (II). The orthorhombic structure of compound I (space group Pnma, a = 10.124 Å, b = 15.205 Å, c = 12.544 Å, Z = 4) and the monoclinic structure of compound II (space group C 2/c, a = 17.910 Å, b = 10.315 Å, c = 14.879 Å, β = 123.23°, Z = 4) are determined by a direct method and refined by the full-matrix least-squares method in the anisotropic approximation to R = 0.063 (I) and 0.042 (II) for all 2293 (I) and 3363 (II) independent measured reflections (CAD-4 automated diffractometer, λMoK α). The complex molecule [RbBr(18-crown-6)(H2O)2] in compound I and the randomly disordered cation [Ba(18-crown-6)(H2O)3]2+ in compound II are of the host-guest type: their Rb+ or Ba2+ cation (its coordination number is nine) is located in the cavity of the 18-crown-6 ligand and coordinated by all six O atoms. In structure I, the coordination polyhedron of Rb+ is a distorted hexagonal pyramid with a triple apex at the Br? ligand and two O atoms of the water molecules. In structure II, the Ba2+ polyhedron is a distorted hexagonal bipyramid with one apex at the O atom of the water molecule and the other split apex at two O atoms of water molecules.  相似文献   

16.
Reactions of a solution of AgNO3 in aqueous methanol with solutions of 1,4-diallylpiperazine (acidified with HNO3 to pH = 4) and 1-allyloxybenzotriazole in ethanol gave the crystalline silver(I) π-complexes [Ag2(C4H8N2(C3H5)2(H+)2)(H2O)2(NO3)2](NO3)2 (I) and [Ag(C6H4N3(OC3H5)(NO3))] (II). Their crystal structures were determined by X-ray diffraction. Crystals of complexes I and II are monoclinic, space group P21/c; for I: a = 7.053(3)Å, b = 9.389(3)Å, c = 15.488(4)Å, β = 91.60°, V = 1025.3(6)Å3, Z = 4; for II: a = 10.650(4)Å, b = 15.062(5)Å, c = 7.412(4)Å, β = 104.20(3)°, V = 1152.6(8)Å3, Z = 4. In both structures, the organic components act as bidentate ligands forming with AgNO3 34- and 14-membered topological rings, respectively. In complex I, the nearly tetrahedral environment of the Ag(I) atom is made up of the olefinic C=C bond, the O atoms of the nitrate anions, and the water molecule. 1-Allyloxybenzotriazole in structure II causes the deformation of the coordination polyhedron of Ag into a trigonal pyramid via inclusion of the ligand N atom in its coordination sphere. The topological units of the complexes form infinite polymer layers linked by anionic NO 3 ? bridges. In structure I, these layers are united through a system of hydrogen bonds into a three-dimensional framework.  相似文献   

17.
Two 4-phenylbenzophenones (I) and (II) are synthesized via Friedel-Crafts reactions. There are four crystallographically independent molecules with different conformations in the crystal structure of [1,1′-biphenyl]-4-yl(2-chlorophenyl)methanone (I). Crystals are orthorhombic, Pca21, C19H13ClO, a = 13.699(3) Å, b = 8.9385(17) Å, c = 46.836(9) Å; V = 5735(2) Å3, Z = 16, d x = 1.356 g/cm3. Torsion angles between the biphenyl rings are between 28.5° and 30.8°. Several C-H…O and C-H…Cl hydrogen bonds and weak π-π stacking contacts consolidate the crystal. Crystals of [1,1′-biphenyl]-4-yl(3-methoxyphenyl)methanone (II) are orthorhombic, Pbca, C20H16O2, a = 7.8179(15) Å, b = 16.003(3) Å, c = 23.345(5) Å; V = 2920.7(10) Å3, Z = 8, d x = 1.311 g/cm3. The torsion angle between the biphenyl rings is 28.1° and C-H…O hydrogen bonds are observed in compound (II).  相似文献   

18.
The synthesis and X-ray single crystal study of two mixed-ligand Cu(II) complexes are performed: (CH3C(NCH3)CHC(O)CH3)(CF3C(O)CHC(O)CF3)Cu (1) (space group P21/c, a = 7.0848(12) Å, b = 17.854(3) Å, c = 11.837(2) Å, β = 100.495(6)°, V = 1472.4(4) Å3, Z = 4), (CH3C(NC6H5)CHC(O)CH3)· (CF3C(O)CHC(O)CF3)Cu (2) (space group P-1, a = 9.1119(4) Å, b = 9.6954(4) Å, c = 11.1447(6) Å, α = 113.784(2)°, β = 92.383(2)°, γ = 95.402(2)°, V = 893.52(7) Å3, Z = 2). The structures are molecular, formed from neutral mixed-ligand copper complexes. The central copper atom has the (3O+N) coordination environment with average Cu-O distances of 1.948 Å and Cu-N of 1.932 Å; the chelate O-Cu-N angle (average) is 94.0°. In the structures, the complexes are linked into dimeric associates with Cu…Cu distances of 3.197 Å (for 1) and 3.246 Å (for 2). The volatility of mixed-ligand complexes 1 and 2 is in between of that of the starting homo-ligand complexes.  相似文献   

19.
Two new aroylhydrazones 3-bromo-N′-(2-hydroxy-5-methoxybenzylidene)benzohydrazide (1) and 4-hydroxy-3-methoxy-N′-(2-hydroxy-5-methoxybenzylidene)benzohydrazide (2), derived from 5-methoxysalicylaldehyde, are prepared and determined by means of infrared and 1H NMR spectroscopy and single crystal X-ray diffraction. Compound 1 crystallizes in the monoclinic space group P21/n with a = 5.9406(7) Å, b = 31.833(3) Å, c = 7.6460(8) Å, β = 94.522(4)°, V = 1441.4(3) Å3, Z = 4. Compound 2 crystallizes in the monoclinic space group P21/c with a = 14.3471(9) Å, b = 11.3893(7) Å, c = 9.6853(6) Å, β = 94.063(2)°, V = 1578.6(2) Å3, Z = 4. Both molecules have very similar bond lengths and angles. The crystal structures of both compounds are stabilized by N-H...O and O-H...O hydrogen bonds as well as π...π interactions.  相似文献   

20.
Two complexes, namely, (18-crown-6)bis(perchlorato-O,O′)strontium (I) and (18-crown-6)bis(perchlorato-O,O′)barium (II), are synthesized. Their crystal structures are determined by X-ray diffraction analysis. The structures of I (space group P21/c, a = 15.266 Å, b = 11.080 Å, c = 13.235 Å, β = 109.20°, Z = 4) and II (space group P21/n, a = 8.330 Å, b = 11.202 Å, c = 11.752 Å, β = 98.38°, Z = 2) are solved by a direct method and refined by the full-matrix least-squares method in the anisotropic approximation to R = 0.077 (I) and 0.041 (II) against 3714 (I) and 2478 (II) independent reflections (CAD-4 diffractometer, λMoK α radiation). Complex molecules [Sr(18C6)(ClO4)2] in the structure of I and [Ba(18C6)(ClO4)2] in II (in the inversion center)—are of the host-guest type. The Sr2+ or Ba2+ cation is localized in the center of a cavity of the 18-crown-6 ligand and coordinated by its all six O atoms. In compounds I and II, the coordination polyhedron of the Sr2+ and Ba2+ cations (coordination number 10) can be described as a distorted hexagonal bipyramid with two bifurcated vertices at two O atoms of two ClO 4 ? ligands, which are disordered in I and II and each of them has two orientations.  相似文献   

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