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1.
A new inclusion complex (n-C4H9)4N+C4H3O 4 ?  · C4H4O4 · (NH2)2CS has been prepared and characterized by X-ray crystallography. Crystal data: space group P \( \overline 1 \), a = 8.799(2) Å, b = 9.590(1) Å, c = 18.684(4) Å, α = 89.63(1)°, β = 79.56(1)°, γ = 79.74(1)°, V = 1525.2(5) Å3, Z = 2, R 1 = 0.0562 and wR = 0.1033. In the title compound, thiourea molecules, fumaric acid and fumarate anions are joined together by typical O–H···O, N–H···O and N–H···S, plus weak C–H···O and C–H···S, hydrogen bonds to generate a hydrogen-bonded layer corresponding to the (100) family of planes. The tetra-n-butylammonium cations are orderly arranged in a sandwich-like packing mode between the stacked layers. The simultaneous presence of different varieties of intermolecular hydrogen bonds is an interesting feature of the title compound.  相似文献   

2.
The crystal structure of the title compound has been determined. The compound crystallizes in the monoclinic space group P21/c with a = 5.9885(2) Å, b = 14.7345(4) Å, c = 12.3719(4) Å, β = 96.655(5)°, V = 1084.31(8) Å3, z = 4. An intramolecular N–H···N hydrogen bond forms a pseudo-six-membered ring with graph set S 1 1(6). The crystal structure is stabilized by intermolecular interactions of the type N–H···N and C–H···N. The packing motifs in accordance with Etter’s analysis are R 2 2(8) corresponding to N–H···N dimer and that generated by the chain is C(7).  相似文献   

3.
The title compound, 3′-(4-methoxyphenyl)-2-phenyl-4′-(4-ethoxyphenyl)-1,2-dihydro-4H,4′H-spiro[isoquinoline-3,5′-isoxazol]-4-one was synthesized from the reaction of dipolarophile with p-methoxybenzadoxime in the presence of sodium hypochlorite in chloroform solution. The structure of the synthesized compound was determined by IR, 1H NMR, mass spectroscopic data, 13C NMR spectroscopy, elemental analysis and X-ray crystallography. The structure was solved in monoclinic, space group C2/c with a = 21.941 (4), b = 17.233 (3), c = 15.404 (3) Å, β = 122.193 (2), V = 4928.9 (16) Å3, Z = 8 and with Rint = 0.154. The geometry of the title compound showed that the piperidine ring adopts a half-chair conformation. In the crystal structure, molecules are linked by C–H···O and C–H···N contacts. Weak C–H···π interactions plays an important role in stabilizing the supramolecular structure.  相似文献   

4.
The crystal structure of the compound (C5H7N2O)·(C6H4NO3)·H2O (1) consisting of 2-amino-3-hydroxypyridium, isoniconate-N-oxide and lattice water was characterized by single-crystal X-ray diffraction analysis: monoclinic, P21/c, a = 9.6905(8), b = 6.0040(4), c = 21.039(2) Å, β = 101.062(8)°, V = 1201.34(18) Å3, Z = 4. In 1, the deprotonated isoniconate-N-oxide, the protonated 2-amino-3-hydroxypyridium and the lattice water are linked by a series of classical hydrogen bonds to form 2-D layer. Then, these 2-D sheets assemble to a 3-D network via weak hydrogen bonds.  相似文献   

5.
A novel iron (II) complex of formula [Fe3(2,2′-bipy)6(ox)3]·12.25H2O (2,2′-bipy = 2,2′-bipyridine, ox = oxalate) has been prepared and structurally characterized by X-ray crystallography. In the complex, the metal atoms are six-coordinated in distorted octahedral environment. In the complex [Fe(ox)3]4? anions and water molecules are linked together into 1D chain structure by hydrogen interaction. The red crystal of the complex is monoclinic, space group P21/c, with a = 22.932(6) Å, b = 13.715(4) Å, c = 22.493(6) Å, β = 93.177(5)°, and V = 7063(3) Å3 with Z = 4.  相似文献   

6.
The title compound C19H16N2O crystallize as either triclinic or monoclinic polymorph depending on the solvent used. Polymorph [1] crystallizes from methanol in the space group P \( \mathop 1\limits^ - \) with unit cell dimensions: a = 8.723(2), b = 9.344(2), c = 10.544(2) Å, α = 71.54(2), ß = 78.74(2), γ = 74.15(2)°, and Z = 2. Polymorph [2] crystallizes from benzene with space group P21/n with unit cell dimensions: a = 10.230(3), b = 20.536(7), c = 14.563(4) Å, ß = 97.14(3)°, and Z = 8. The only similarity between molecules of [1] and two independent molecules of [2] can be found in almost co-planar phenyl moiety with chelate ring. Both structures are characterized with strong intramolecular O-H···N hydrogen bond. Whereas the molecular interconnections in [2] are based on van der Waals attractions between discrete molecules, molecules of [1] associate in dimers via intermolecular N-H···O hydrogen bonding by the operation of crystallographic centre of inversion.  相似文献   

7.
3-(2,4-Dimethylphenyloxymethyl)-3,4-dihydroisocoumarin (C18H18O3) was prepared by the alkylation of o-lithio N-methyl benzamide with 2-(2,4-dimethylphenoxy)methyl oxirane, followed by alkaline hydrolysis. The compound crystallizes in the orthorhombic space group Pbca with unit cell parameters : a = 8.239(2) Å, b = 14.918(5) Å, c = 24.831(9) Å, Z = 8. The crystal structure was solved by direct methods and refined to R = 0.0514 for 1564 observed reflections. The heterocyclic ring adopts a distorted half-chair conformation. Molecules are connected by π–π interactions between phenyl rings of the isocoumarin nucleus forming dimers. Dimers are connected via C–H...O hydrogen bonds forming chains. Further intermolecular C–H...π hydrogen bonds link the dimer chains to form supramolecular structure.  相似文献   

8.
Tert-butyl 2-((phenylthio)carbonyl)pyrrolidine-1-carboxylate, was synthesized by using iso-butoxycarbonyl chloride (i-BuOCOCl) via mixed anhydride method. The obtained product was characterized spectroscopically and finally confirmed by X-ray diffraction studies. The title compound C16 H21 N O3 S crystallizes in the triclinic space group P1 with the cell parameters a = 6.0250(7) Å, b = 8.2820(13) Å, c = 8.7700(14) Å, α = 102.352(4)°, β = 102.993(11)°, γ = 90.279(8)°, V = 415.89(10) Å3 and Z = 1. The proline ring in the structure is in a envelope conformation. The structure exhibits intermolecular hydrogen bonds of the type C–H...O.  相似文献   

9.
The crystal structure of 4-aminopyridinium 3,5-dinitrobenzoate, C12H10O6N4, has been determined by single-crystal X-ray diffraction technique. The title compound crystallizes in the monoclinic sp. gr. P21/n with the unit cell parameters: a = 7.4726(3) Å, b = 23.0898(9) Å, c = 8.0744(4) Å, V = 1338.64(10) Å3, Z = 4. The asymmetric unit of the compound consists of one 3,5-dinitrobenzoate anion and 4-aminopyridine cation. The adjacent anions and cations are linked through two N?H···O hydrogen bonds, N2?H2A···O5 and N2?H2B···O6, to form an infinite chain of anions and cations, extended along the [010] direction.  相似文献   

10.
Exposure of dichloromethane solution of [OEOPFe(BF4)], where OEOP is the monoanion of octaethyloxoporphyrin, to dioxygen results in its transformation into the μ-oxo bridged compound, [(OEOPFe)2O)](BF4)2. The molecular structure of the title compound, [(OEOPFe)2O](BF4)2, was determined by single-crystal X-ray diffraction. It contains a binuclear centrosymmetric [(OEOPFe)2O]2+ cation (the bridging O atom lies on an inversion centre) and two tetrafluoroborate anions. The Fe atom is five-coordinate to four N atoms of the porphyrin ring and to one bridging O atom. The compound is characterized by an average Fe–N bond length of 2.064 Å. The Fe–O bond distance is 1.7665(11) Å and the Fe–O–Fe bond angle is 180.0° and the two porphyrin rings are parallel. Crystal data: crystal system, monoclinic, a = 8.867(3), b = 26.104(9), c = 15.748(6) Å, β = 105.40(3)°, space group, P21/c, V = 3514(2) Å3, Z = 2.  相似文献   

11.
The crystal structures of four new diphosphinated chromium Fischer amino carbenes with the compositions fac-[(P-P)(CO)3Cr=C(NR2′)(R)] (R = Me, NR2′ = pyrrolidino, P-P = dppe, 1; R = Me, NR2′ = pyrrolidino, P-P = dppp, 2; R = Me, R′ = Me, P-P = dppe, 3; R = Me, R′ = Me, P-P = dppp, 4) have been determined at 243 K. Compound 1 crystallizes in the monoclinic system, space group P21 /n with a = 12.1597(11) Å, b = 20.1556(17) Å, c = 14.0557(12) Å, β = 114.163(3)°, V = 3143.0(5) Å3, and Z = 4. Compound 2 crystallizes in the triclinic system, space group ? 1 with a = 7.4424(3) Å, b = 10.8830(5) Å, c = 20.6040(9) Å, α = 100.9880(10)°, β = 91.7650(10)°, γ = 97.6610(10)°, V = 1620.90(12) Å3, and Z = 2. Compound 3 crystallizes in the monoclinic system as a mono-solvate of d5-pyridine, space group P21 /c with a = 11.485(2) Å, b = 22.825(5) Å, c = 14.092(3) Å, β = 108.53(3)°, V = 3502.7(12) Å3, and Z = 4. Compound 4 crystallizes in the orthorhombic system, space group P2 1 2 1 2 1 with a = 8.359(3) Å, b = 15.364(6) Å, c = 23.784(9) Å, V = 3055(2) Å3, and Z = 4. Steric repulsions with the diphosphine ligand favor a conformation with the amino moiety directed away from the diphosphine backbone in 14.  相似文献   

12.
The crystal structure of a pure natrolite sample, Na2(Al2Si3O10)·2H2O, coming from Asheken, Ethiopia, has been analysed by single crystal X-ray diffraction. It crystallizes within the orthorhombic space group Fdd2, with the following cell constants: a = 18.2930(2) Å; b = 18.6430(5) Å; c = 6.5860(5) Å; V = 2246.07(18) Å3. The three-dimensional framework of this hydrated aluminosilicate zeolite is made up by chains of corner-sharing SiO4 and AlO4 tetrahedra down c; the chains are held together by sharing the external vertices of tetrahedra; water molecules and Na+ extra-framework cations fill up the resulting cavities, the latter forming irregular NaO6 octahedra. Hydrogen bonds complete the array.  相似文献   

13.
The crystal structure of p-carboxyphenylhydrazone benzoylacetone is determined. The crystals are monoclinic, a = 13.614(4) Å, b = 11.388(2) Å, c = 20.029(6) Å, β = 104.82(2)°, V = 2339(9) Å3, Z = 8, space group C2/c, and R = 0.038 for 1622 reflections with I > 2σ(I). The crystal is built of C17H14N2O4 neutral molecules that are linked by O-H?O hydrogen bonds between the carboxyl groups into centrosymmetric pseudodimers. The effect of carboxylation of the phenylhydrazone fragment and the position of the carboxyl group on the molecular packing in the crystal is determined. The N(1)-H(1N)?O(1) intramolecular hydrogen bond (N-H, 0.94 Å; H?O, 1.87 Å; N?O, 2.59 Å; and the N-H?O angle, 133°) is formed in the molecule.  相似文献   

14.
Photochemical activation of the triosmium cluster Os3(CO)12 in CH2Cl2 solvent and ethylene, followed by treatment with the diphosphine ligand 4,5-bis(diphenylphosphino)-4-cyclopenten-1,3-dione (bpcd), furnishes the new octahedral compound cis(CO)–ClOs(CO)2(bpcd)[C(O)Et] in low yield. The title compound has been isolated and characterized in solution by IR and 1H NMR spectroscopies, with the solid-state structure of cis(CO)–ClOs(CO)2(bpcd)[C(O)Et] determined by X-ray diffraction analysis. cis(CO)–ClOs(CO)2(bpcd)[C(O)Et] crystallizes in the triclinic space group P-1, a = 10.043(2), b = 11.455(2), c = 16.221(3) Å, α = 74.900(3)°, β = 76.150(3)°, γ = 76.221(2)°, V = 1718.2(5) Å3, Z = 2, D cacl = 1.717 Mg/m3; R = 0.0453, R w = 0.0778 for 6703 observed reflections with I > 2σ(I). The presence of the chlorine and propanioyl groups in cis(CO)–ClOs(CO)2(bpcd)[C(O)Et] is structurally confirmed, and the origin of the these groups from the reaction solvent and ethylene is discussed.  相似文献   

15.
Khayanone was isolated from the stem bark of African mahogany, Khaya senegalensis (Meliaceae), and characterized as 6S,8α-dihydroxy-14,15-dihydrocarapin on the basis of spectral analysis and single crystal X-ray diffraction study. The compound crystallizes in the tetragonal space group P4 1 2 1 2 with unit cell parameters: a = 13.2315(19) Å, c = 29.118(6) Å, Z = 8. The crystal structure has been solved by direct methods and refined to R = 0.0375 for 4552 unique reflections. The six-membered rings A and B exist in boat conformations, rings C and D in chair conformations, and the furan ring is planar. The crystal structure is stabilized by O-H···O and C-H···O interactions. This is the first report about 6S configuration of mexicanolide revealed by X-ray diffraction analysis. The configuration of oxygenated C-6 in mexicanolide-group limonoids is discussed.  相似文献   

16.
A four-coordinated complex, L2Co(NCO)2, (L = 1-methylbenzimidazole) has been synthesized and characterized by IR spectroscopy, elemental analyses, and single crystal X-ray diffraction. The crystal is monoclinic, a = 14.522(2) Å, b = 14.610(2) Å, c = 8.6850(13) Å, β = 92.037(3)°, Z = 4, sp. gr. P21/c. Bond lengths Co–N(L) are equal to 2.0165(16) and 2.0174(15) Å, Co–O(NCO) are 1.944(2) and 1.945(2) Å. Intermolecular C–H···O, C–H···N, and C–H···π interactions link the molecules into three-dimensional networks in the crystal.  相似文献   

17.
The X-ray diffraction study of Ba[Ni(Cdta)] · 10H2O is performed (R1 = 0.0441 for 5136 observed reflections). The crystals are triclinic, a = 8.833(2) Å, b = 9.025(2) Å, c = 16.922(3) Å, α = 80.56(3)°, β = 82.77(3)°, γ = 76.98(3)°, Z = 2, and space group \(P\bar 1\). The crystal is built of the [Ni(Cdta)]2? anionic complexes, the [Ba(H2O)6]2+ hydrated cations, and crystallization water molecules. The distorted octahedral coordination of the Ni atom includes two N and four O atoms of the Cdta4? ligand (mean Ni-N, Ni-OG, and Ni-OR re 2.080, 2.082, and 2.036 Å, respectively). The irregular nine-fold coordination of the Ba atom consists of six O atoms of water molecules and three O(Cdta) atoms from three anionic complexes (Ba—O, 2.715–3.090 Å). With consideration for the bonds with three Ba atoms, the Cdta4? ligand is octadentate (2N + 6O) and fulfills the pentadentate μ4-bridging function. The structural units are linked through an extended network of hydrogen bonds.  相似文献   

18.
An oxamido-bridged binuclear copper(II) complex, Cu2(oxen)(NCS)2(DMF)2 (1) (H2oxen = N,N′-bis(2-aminoethyl)oxamide, DMF = dimethylformamide), has been synthesized by the reaction of Cu(oxen) · 2H2O with CuCl2 · 2H2O and KSCN in DMF/CH3OH solution, and characterized by elementary analysis, FT-IR spectra and X-ray single-crystal diffraction. Structural analysis reveals that complex 1 forms a centrosymmetric binuclear molecule in which an oxamido group in the trans conformation bridges two crystallographically equivalent five-coordinate copper(II) ions with Cu–Cu distance of 5.279(2) Å. The complex molecules are assembled into a novel 2D layer through weak Cu?S interactions (d Cu–S = 3.341(4) Å) and intermolecular hydrogen bonds. Viewed along the crystallographic b axis, layers display an interesting hydrophobic–hydrophilic–hydrophobic sandwich arrangement, with the hydrophobic layers dominated by dipole interaction of DMF molecules.  相似文献   

19.
The title compound, 2-(thiophen-2-yl)-1-(5-thioxo-4,5-dihydro-1,3,4-oxadiazol-2-yl)ethenyl] benzamide:N,N-dimethylformamide (1: 1), (C15H11N3O2S2 · C3H7NO), was synthesized, and its structure was established by spectral analysis and X-ray diffraction studies. The compound crystallizes in the monoclinic space group P21/n with a = 10.8714(7), b = 9.0497(5), c = 19.8347(13) Å, β = 91.093(5)°, Z = 4. The crystal structure is stabilized by N–H···S, C–H···O and N–H···O hydrogen bonds. The π···π interactions are also observed between the rings.  相似文献   

20.
1-Benzhydryl-4-phenylmethane sulfonyl piperazine was synthesized from 1-benzhydryl piperazine with phenylmethane sulfonyl chloride. The product obtained was characterized by 1H NMR, MS and IR techniques and finally confirmed by X-ray crystallography. The title compound C24H26N2O2S, M r   =   406.53, crystallizes in the orthorhombic crystal class in the space group Pbca with unit cell parameters a  =  11.1240(10)Å, b  =   9.4940(15)Å, c  =  40.239(4)Å, Z  =  8 and V = 4249.7(9)Å3. The structure was solved by direct methods and refined to R 1=0.0561 for 2,445 reflections with [I > 2 σ(I)]. The piperazine ring adopts a chair conformation. The sulfonyl moiety is in a distorted tetrahedral configuration.  相似文献   

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