共查询到20条相似文献,搜索用时 26 毫秒
1.
Daniel A. Ramirez Jianxing Zhang Kevin Klausmeyer Robert R. Kane 《Journal of chemical crystallography》2005,35(3):227-232
The combretastatin A-4 analogue cis-1-(3-N,N-dimethylthiocarbamoyl-4-methoxy)-2-(3,4, 5-trimethoxyphenyl) ethene (1) and its trans stereoisomer (2) were synthesized. The molecular structures of these compounds were obtained by single-crystal X-ray diffraction. Crystallization of 1 occurs in the centrosymmetric monoclinic space group C2/c (No. 15) with a = 21.468(5), b = 7.932(1), c = 23.949(3); and = 100.75(1) and Z = 8. Crystallization of 2 occurs in the centrosymmetric monoclinic space group P21/n (No. 14) with a = 11.7825(7), b = 11.562(1), c = 14.911(1) and = 93.294(6); and Z = 4. Details of the synthesis and the structural characterization of the title compounds are presented and discussed. 相似文献
2.
Savariapichai Martin Chandran Revathi Arunachalam Dayalan 《Journal of chemical crystallography》2009,39(12):908-912
Abstract
The title complex: C4H12N2[Co(C4H7N2O2)2Cl2]2·2H2O, viz., PpH2[Co(dmgH)2Cl2]2·2H2O, where, dmgH− = dimethylglyoximate and Pp = piperazine was synthesized and analyzed by single crystal XRD studies. The complex was grown as brown crystals by the slow evaporation method in ethanol. The complex crystallizes as triclinic with the space group p[`1] p\overline{1} and unit cell parameters a = 8.4521 (10) Å, b = 10.0999 (11) Å, c = 10.8952(13) Å; α = 94.066(6)°, β = 106.047(6)° and γ = 100.901(6)°. There are two complex molecules present in the unit cell. The short intra molecular O–H···O hydrogen bonds link the glyoximate moieties in the crystal. 相似文献3.
Juan Mo Su-Mei Zhang Wen-Zhong Ge Jian-Hua Liu 《Journal of chemical crystallography》2009,39(12):890-893
Abstract
The title complex [Cu2(C10H8N2)(C12H10N4)(C18H15)2(BF4)2] n has been synthesized and characterized by single crystal X-ray analysis. The compound crystallizes in the monoclinic space group P21/c with a = 10.450(4) Å, b = 14.027(5) Å, c = 18.950(6) Å, β = 100.459(5)°, V = 2,731.7(16) Å3. In the title complex, the cation forms a linear chain, which is bridged by 4,4′-bipyridine and pyridine-2-carbaldehyde azine. The crystallographic asymmetry unit could be expanded polymeric structure using symmetry code: x, 1 + y, z; 1 − x, −y, 1 − z. The Cu(I) atom is coordinated by one P atom of PPh3 ligand, two N atoms of pyridine-2-carbaldehyde azine ligand and one N atom of 4,4′-bipyridine ligand. There is a crystallographic centre of symmetry at the mid-point of the C–C bond between two pyridine rings of 4,4′-bipyridine. 相似文献4.
Hai-Yun Zhu 《Journal of chemical crystallography》2011,41(11):1785-1789
Abstract
Two new hydrazone compounds, 3-bromo-N′-(2-methoxybenzylidene)benzohydrazide (1) and N′-(2-methoxybenzylidene)-3,4-methylenedioxybenzohydrazide (2), have been synthesized and characterized by elemental analysis, IR, and single crystal X-ray diffractions. Compound (1) crystallizes in the triclinic space group P1 with unit cell dimensions a = 8.4088(5) ?, b = 8.5398(5) ?, c = 10.6572(6) ?, α = 90.356(3)°, β = 102.868(3)°, γ = 97.987(3)°, V = 738.28(7) Ǻ3, Z = 2, R 1 = 0.0406, and wR 2 = 0.0804. Compound (2) crystallizes in the tetragonal space group P41 with unit cell dimensions a = b = 9.792(4) ?, c = 15.788(6) ?, V = 1513.8(10) Ǻ3, Z = 4, R 1 = 0.0415, and wR 2 = 0.0818. The molecules of both compounds display E configurations with respect to the C=N double bonds. In the crystal structure of (1), molecules are linked through N–H···O hydrogen bonds, forming chains running along the b axis. In the crystal structure of (2), molecules are linked through N–H···O hydrogen bonds, forming chains running along the c axis. 相似文献5.
Clyde R. Metz John D. Knight Anna C. Dawsey William T. Pennington Donald G. VanDerveer Jordan B. Brown Kevin J. Bigham Charles F. Beam 《Journal of chemical crystallography》2010,40(4):296-301
Abstract
Dilithiated C(α), N-carbomethoxyhydrazones were condensed with lithiated methyl 2-(aminosulfonyl)benzoate to afford intermediates that were isolated and not characterized but cyclized with acetic anhydride, which also resulted in N-acetylation. The X-ray crystal structure determinations of methyl 2-acetyl-5′-phenyl-2H-spiro[benzo[d]isothiazole-3,3′-pyrazole]-1,1-dioxide-2′(4′H)-carboxylate and methyl 2-acetyl-5′-(2-thienyl)-2H-spiro[benzo[d]isothiazole-3,3′-pyrazole]-1,1-dioxide-2′(4′H)-carboxylate products were a follow up for absorption spectra, and they confirmed their structures. Mechanistic intermediates to describe the reaction may include C-acylated intermediates that cyclize to spiro(N-benzoisothiazole dioxide-pyrazole) instead of N-carbomethoxypyrazole-ortho-benzenesulfonamides. Crystals of C19H17N3O5S 7 are monoclinic, P21/c, a = 11.899(2) ?, b = 17.562(4) ?, c = 9.484(2) ?, β = 111.03(3)°, Z = 4, V = 1849.9(6) ?3, R 1 = 0.0857 and wR 2 = 0.2216 for reflections with I > 2σ(I); crystals of C17H15N3O5S2 8 are orthorhombic, Pbca, a = 16.045(3) ?, b = 10.746(2) ?, c = 20.389(4) ?, Z = 8, V = 3516(1) ?3, R 1 = 0.0841 and wR 2 = 0.2179 for all reflections with I > 2σ(I). 相似文献6.
Z. A. Carlson Bronwyn L. Harrod Daniel Widener William A. Howard Keliang Pang 《Journal of chemical crystallography》2010,40(10):863-866
Abstract
[Zn(H2O)6][{Zn(H2O)}2(ttha)]·4H2O (ttha = triethylenetetraamine-N,N,N′,N″,N‴,N‴-hexaacetate) has been structurally characterized (triclinic, P-1, a = 7.4014(4) ?, b = 8.5521(4) ?, c = 15.0309(7) ?, α = 73.582(1)°, β = 85.173(1)°, γ = 69.935(1)°; V = 857.15(7) ?3; Z = 1). The two Zn2+ ions bound by the [ttha]−6 ligand are in distorted octahedral environments. While there exists a center of symmetry in the [{Zn(H2O)}2(ttha)]2− anion in the crystalline state, 13C{1H} NMR spectroscopy demonstrates the absence of a center of symmetry in aqueous solution. Furthermore, electronic absorption spectroscopy reveals that [Zn(H2O)6][{Zn(H2O)}2(ttha)]·4H2O reacts with vanadyl(IV) acetate in aqueous solution at room temperature to yield [(VO)2(ttha)]2−. This reaction implies that Zn2+ can dissociate from [{Zn(H2O)}2(ttha)]2− in aqueous solution. 相似文献7.
Verica V. Glodjovi Frank W. Heinemann Sreko R. Trifunovi 《Journal of chemical crystallography》2008,38(12):883-889
Abstract The s-cis-[Cr(S,S-eddp)L]− complexes (S,S-eddp = S,S-ethylenediamine-N,N′-di-2-propionate ion; L = oxalate or malonate ions) were prepared. The complexes were purified by ion-exchange chromatography.
The geometry of the complexes has been supposed on the basis of the electronic absorption spectra, and the absolute configurations
of the isolated s-cis-[Cr(S,S-eddp)L]− complexes have been predicted on the basis of their circular dichroism (CD) spectra and confirmed by X-ray analysis of the
crystal structure of the Δ-(–)589-s-cis-K[Cr(S,S-eddp)(ox)] 0.5H2O complex.
Index Abstract The title compound, s-cis-potassium-(ethylenediamine-N,N’-di-S,S-2-propionato) (oxalato)chromate(III) semihydrate was synthesized by passing the corresponding sodium salt through cation
exchange-resin Merck I in potassium form and its crystal structure determined. Single crystal X-ray diffraction analysis reveals
s-cis geometry of the complex cation.
For Part II see Glodjović VV, Trifunović SR (2008) J Serb Chem Soc 73:541. 相似文献
8.
Hossni Ziyat Moulay Youssef Ait Itto Mustapha Ait Ali Abdellah Karim Abdelkhalek Riahi Jean-Claude Daran 《Journal of chemical crystallography》2011,41(3):338-342
Abstract
The title compounds C11H16Cl2O3 (III) and C11H16Br2O3 (IV) have been prepared from (S)-Limonen. Their crystal structure and absolute configuration have been determined by X-ray analysis which confirmed the 1′S absolute configuration at the cyclopropyl moiety, in agreement with the known absolute configuration of the starting material. Both (III) and (IV) are orthorhombic, space group P212121 with a = 7.2558(4) ? (for III) 7.4058(6) ? (for IV), b = 9.7885(5) ? (for III) 9.7459(7) ? (for IV), c = 17.7551(10) ? (for III) 18.0354(14) ? (for IV), α = 90°, β = 90°, γ = 90° and Z = 4. 相似文献9.
O. V. Kovalchukova A. I. Stash S. B. Strashnova E. P. Romashkina B. E. Za?tsev 《Crystallography Reports》2010,55(3):428-431
The complex compounds (H3
L · Cl)[CoCl4] (I) and H2
L[CuBr4] (II), where L is 2,4,6-tri(N,N-dimethylamino)methylphenol, were isolated in the crystalline state and studied by X-ray diffraction. The organic cations
were found to be outer-sphere ligands. All three nitrogen atoms of the tertiary amino groups are protonated. In compound I, the H3
L
3+ cation exists as the cis tautomer. In compound II, the H2
L
2+ dication exists as the trans isomer. In the crystal structure, the dications are arranged in layers via hydrogen bonds. 相似文献
10.
Zhi-Ping Li You-Ji Li Zhao-Xia Li Hui Li Zhu-Ping Xiao 《Journal of chemical crystallography》2011,41(10):1568-1572
Abstract
A new hydrazine ligand N′-3,5-dibromo-2-hydroxybenzylidene)-2-hydroxy-3-methylbenzohydrazide (1) and its oxovanadium(V) complex [N′-(3,5-dibromo-2-oxidobenzylidene-κO)-2-hydroxy-3-methylbenzohydrazidato-κ 2 N′,O](methanol-κO)(methanolato-κO)oxidovanadium(V) (2), were prepared and were structurally characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. Compound 1 crystallizes in the triclinic space group P−1, with unit cell dimensions a = 7.813(2) ?, b = 8.748(2), c = 26.071(6) ?, α = 85.763(2)°, β = 81.521(2)°, γ = 89.358(3)°, V = 1757.6(7) ?3, Z = 4, R 1 = 0.0587, and wR 2 = 0.1054. Compound 2 crystallizes in the triclinic space group P-1, with unit cell dimensions a = 7.777(3) ?, b = 11.594(3), c = 12.363(3) ?, α = 107.965(3)°, β = 103.190(2)°, γ = 96.656(2)°, V = 1011.3(5) ?3, Z = 2, R 1 = 0.0634, and wR 2 = 0.1480. The hydrazine ligand coordinates to the V atom through the phenolic O, imino N, and ethanolic O atoms. The V atom in the complex is in an octahedral coordination, with the three donor atoms of the hydrazine ligand and one methanolato O atom defining the equatorial plane, and with one methanol O and one oxo O atoms occupying the axial positions. The displacement of the V atom from the equatorial plane towards the axial oxo O atom is 0.305(2) ?. 相似文献11.
Sanjay Kapoor Renu Sachar Kuldeep Singh Vivek K. Gupta Rajnikant 《Journal of chemical crystallography》2012,42(5):458-463
Abstract
The [Ni(S2COCH2CH2CH3)2(C6H4N2)2] adduct of 4-cyanopyridine with [Ni(S2COCH2CH2CH3)2] was synthesized and characterized by elemental analysis, magnetic susceptibility measurement, IR, electronic spectral data, Thermogravimetric analysis/DTA techniques and X-ray diffraction analysis. The Ni atom in the title complex is octahedrally coordinated within a trans-N2S4 donor set, with the Ni atom located on a centre of inversion. The title complex crystallizes in the monoclinic space group P2 1 /c with unit cell parameters a = 11.75(4), b = 11.62(3), c = 9.20(2) ?, β = 104.99(3)°. Crystal structure was solved by direct methods and refined by full matrix least squares procedures to a final R-value of 0.0294 for 1895 observed reflections. The packing of layers of molecules is stabilized by weak C–H···N and C–H···π interactions. 相似文献12.
Saeed Ahmad Muhammad Altaf Helen Stoeckli-Evans Anvarhusein A. Isab Muhammam Riaz Malik Saqib Ali Shaukat Shuja 《Journal of chemical crystallography》2011,41(8):1099-1104
Abstract
Cadmium(II) complexes, dibromidobis(N,N′-dimethylthiourea-S)cadmium(II), [Cd(Dmtu)2Br2] (1) and diiodidobis(N,N′-dimethylthiourea-S)cadmium(II), [Cd(Dmtu)2I2] (2), have been prepared and their structures have been determined by X-ray crystal structure analysis. Compound 1 crystallized in the monoclinic space group C2/c, and the metal ion is situated on a twofold rotation axis. Compound 2 also crystallized in a monoclinic space group, P21/c, but here the molecules have no crystallographic symmetry. In both compounds the cadmium atom is bonded to two halide ions and to two dimethylthiourea molecules through the sulfur atoms in a tetrahedral environment. The molecules are linked via N–H⋯Halide hydrogen bonds to form infinite one-dimensional chains in 1 and infinite two dimensional networks in 2. The complexes were also characterized by IR and NMR spectroscopy and the data are consistent with the structures of the compounds. 相似文献13.
M. Akkurt S. Ö. Yıldırım A. Kerbal B. Bennani M. Daoudi Z. H. Chohan V. McKee T. Ben Hadda 《Journal of chemical crystallography》2010,40(3):231-234
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
14.
Abstract
Reactions of 4-chlorobenzohydrazide with 3-bromo-5-chloro-2-hydroxybenzaldehyde and 3,5-dichloro-2-hydroxybenzaldehyde, respectively, afforded two isostructural hydrazone compounds, C14H9BrCl2N2O2·CH3OH (1) and C14H9Cl3N2O2·CH3OH (2). Both compounds were structurally characterized by X-ray determination. Compound 1 crystallizes in the triclinic space group P − 1 with unit cell dimensions a = 7.462(1) ?, b = 9.281(2) ?, c = 12.626(1) ?, α = 98.451(2)°, β = 98.630(2)°, γ = 100.025(2)°, V = 837.8(2) ?3, Z = 2, R 1 = 0.0394 and wR 2 = 0.0967. Compound 2 crystallizes in the monoclinic space group P21/n with unit cell dimensions a = 7.485(1) ?, b = 13.389(2) ?, c = 16.693(2) ?, β = 99.754(2)°, V = 1648.7(4) ?3, Z = 4, R 1 = 0.0375 and wR 2 = 0.0900. X-ray structural determination revealed that each compound consists of a hydrazone molecule and a methanol molecule of crystallization. In the crystal structures of both compounds, the adjacent molecules are linked by methanol molecules through N–H···O and O–H···O hydrogen bonds, forming dimers. 相似文献15.
Ashley R. Head Donna S. Amenta John W. Gilje Glenn P. A. Yap 《Journal of chemical crystallography》2011,41(2):247-250
Abstract
The title compound cis-Cl2Pd [P(Ph)2PCH2P(O)Ph2]2 crystallizes in the monoclinic space group, P21/c with crystal cell parameters a = 13.076(5) ?, b = 12.931(5) ?, c = 27.465(9) ?, β = 92.661(6)o, V = 4639(3) ?3, Z = 4. The bulk of the phenyl groups prohibits the molecule from assuming a conformation that would permit both P=O groups to coordinate another metal ion. 相似文献16.
Abstract
Yellow crystals of [Zn(N,N′-bis (5-bromosalicylidene) 2,3-diaminopyridine)] Pyridine, [Zn(C19H11Br2N3O2)]C5H5N, have been obtained and characterized by elemental analysis, FT-IR, UV–Vis, 1H NMR spectroscopy and MALDI-TOF mass spectrometry. The structure has been determined by single crystal X-ray crystallography. The complex crystallizes in the triclinic space group P-1 with two molecules in the asymmetric unit and with unit cell dimensions a = 8.0103(3) ?, b = 12.8340(5) ?, c = 22.3682(11) ?, α = 91.715(2)°, β = 93.918(2)°, γ = 103.708(2)°. V = 2226.30(16) ?3, Z = 4, R 1 = 0.0780 and wR 2 = 0.1192. X-ray structure determination revealed that the complex consists of a [Zn(C19H11Br2N3O2)] moiety with a coordinated pyridine molecule on the metallic centre. The zinc atom adopts a distorted square pyramidal geometry as it is shown in the crystal structure. 相似文献17.
The title compound 1-(1,3-dimethyl-5-chloropyrazol-4-carbonyl)-3-(2-chlorophenyl)-5-amino-4-cyanopyrazole (C16H12Cl2N6O) has been synthesized and characterized by X-ray diffraction: Triclinic, space group P1, with a = 8.6712(8) Å, b = 9.5091(10) Å, c = 11.2170(11) Å = 71.531(2)°, = 84.683(2)°, = 74.099(2)° Z = 2; V = 843.7(14) Å3. C(10), O(1), C(11), and N(2) atoms are coplanar with the average deviation of 0.0071 Å, which form 11.03° and 43.93° dihedral angles with pyrazole planes (I) and (II), respectively. 相似文献
18.
Wesley H. Monillas Glenn P. A. Yap Klaus H. Theopold 《Journal of chemical crystallography》2009,39(5):377-379
Abstract Addition of CrI2 to the lithium salt of N-N′-bis(2,6-diisopropylphenyl)-2,4-diketiminate in diethylether yields a Cr(II) iodide complex with a coordinated, solvated
LiI salt. This complex is the intermediate in the synthesis of a bridging iodide complex that is itself a precursor to a side-on
bridging dinitrogen complex. This complex crystallizes in the P21/n space group with the crystal cell parameters a = 12.3160(19) ?, b = 21.067(3) ?, c = 15.837(3)?, β = 96.767°, V = 4080.6(11) ?3 and Z = 4.
Graphical Abstract Addition CrI2 to the lithium salt of N-N′-bis(2,6- diisopropylphenyl)-2,4-diketiminate in diethylether yields a Cr(II) iodide complex with a coordinated, solvated
LiI salt. Herein we report the spectroscopic and structural characterization.
An erratum to this article can be found at 相似文献
19.
Dalibor Mili? Vi?nja Vrdoljak Dubravka Matkovi?-?alogovi? Marina Cindri? 《Journal of chemical crystallography》2009,39(8):553-557
Abstract Red crystals of cis-dioxo(3-methoxysalicylaldehyde 4-methylthiosemicarbazonato-N,O,S)(γ-picoline-N)molybdenum(VI), [MoO2L(γ-pic)], [L2−=CH3OC6H4(O)CH=NN=C(S)NHCH3, 3-methoxysalicylaldehyde 4-methylthiosemicarbazonato] were prepared by the reaction of [MoO2L]
n
with γ-picoline in dry methanol. The title compound crystallized in the monoclinic space group P21/n, a = 6.7984(7) ?, b = 15.9760(12) ?, c = 17.1466(14) ?, β = 93.613(8)°, V = 1858.6(3) ?3, Z = 4. The coordination geometry around the molybdenum center is distorted octahedral with the tridentate thiosemicarbazonato
ligand (L2−) bonded meridionally to the [MoO2]2+ core. The sixth coordination site is occupied by a weakly bound γ-picoline molecule. The adjacent molecules are joined by
the N–H···O hydrogen bonds between their amino and methoxy groups thus forming infinite molecular chains. The three-dimensional
solid-state structure is achieved by the additional C–H···O, C–H···π and van der Waals interactions.
Graphical Abstract In the title compound, [MoO2L(γ-pic)], the tridentate thiosemicarbazonato ligand (L2−) is meridionally bound to the [MoO2]2+ core, while a molecule of γ-picoline completes the distorted octahedral coordination around the metal atom.
相似文献
20.
Oscar F. Vázquez-Vuelvas David Morales-Morales Juan M. Germán-Acacio Mikhail Tlenkopatchev Armando Pineda-Contreras 《Journal of chemical crystallography》2011,41(3):419-424