共查询到20条相似文献,搜索用时 718 毫秒
1.
Souad Chaouche Rachid Ouarsal Mohammed Lachkar Francesco Capitelli Brahim El Bali 《Journal of chemical crystallography》2010,40(6):486-490
Abstract
A new hybrid phosphate, (C6H5NH3)[ZnCl(HPO3)], has been synthesized and its structure characterized from single-crystal X-ray diffraction. The title compound crystallizes in the orthorhombic space group Pbca (n. 61) with the unit-cell parameters: a = 9.8635(2) ?, b = 9.4516(10) ?, c = 22.2430(4) ?, Z = 8 and V = 2,073.62(6) ?3. The final R factors were R/ωR = 0.0361/0.0924. Its framework might be described as a layered structure with two (010)-parallel cationic and anionic layers. The IR spectrum of this phase shows characteristic bands of phosphite and anilinium groups. 相似文献2.
Abstract
The title complex triaqua (3-hydroxy-5-hydroxymethyl-2-methylpyridine-4-carboxaldehyde-3-methylisothiosemicarbazone-k3,O3,N7,N10)Ni(II) nitrate ([Ni(PLITSC)(H2O)3](NO3)2, 1) represents the second transition metal complex incorporating an isothiosemicarbazide-pyridoxal based Schiff base that has been crystallographically characterized. Complex 1 crystallizes in a P21/n space group, with lattice constants: a = 11.2254(1) ?, b = 12.9941(2) ?, c = 12.8663(2), β = 96,7713(5)°, V = 1863.64(4) ?3, Z = 4, F(000) = 1016, R 1 = 0.0681, wR 2 = 0.1201. The central Ni(II) cation is found in a six-coordinate octahedral geometry formed by the tridentate Schiff base ligand PLITSC and three water molecules. The identity of 1 was further confirmed by elemental analysis, IR spectra, and conductometric and magnetochemical measurements. 相似文献3.
Günseli Turgut Cin Seda Demirel Topel Abban Cakıcı Arzu Özek Yıldırım Ahmet Karadağ 《Journal of chemical crystallography》2012,42(4):372-380
Abstract
Two novel ferrocenyl substituted N-acetyl-2-pyrazolines, N-acetyl-3-(2-furyl)-5-ferrocenyl-2-pyrazoline (3) and N-acetyl-3-(2-thienyl)-5-ferrocenyl-2-pyrazoline (4), have been synthesized and characterized by FTIR, 1H-NMR, 13C-NMR techniques, elemental analysis and X-ray structure analysis. Thermal properties of these compounds have been determined by TGA, DTA and DSC analysis. Compound 3 (C19H18N2O2Fe) crystallizes in the monoclinic space group P21/c and Z = 4, with a = 8.6970(4) ?, b = 18.4725(9) ?, c = 11.0041(5) ?, β = 110.942(3)°. Compound 4 (C19H18N2OSFe) crystallizes in the orthorhombic space group Fdd2 and Z = 16, with a = 84.242(2) ?, b = 13.5416(5) ?, c = 5.9405(2) ?, β = 90°. In terms of crystal packing, each compound shows different molecular arrangement, which are stabilized by C–H···O intermolecular weak hydrogen bonds, and/or C–H···π interactions. 相似文献4.
Jeongho Yeon Sang-Hwan Kim P. Shiv Halasyamani 《Journal of chemical crystallography》2011,41(3):328-331
Abstract
A new quinternary oxide, NaTl3Cu4Te2O12, has been synthesized and characterized by single crystal X-ray diffraction. The reported material was synthesized by hydrothermal techniques using TlNO3, CuO, TeO2, and NaOH as reagents. The material exhibits a two-dimensional layered structure consisting of edge-shared CuO6 and TeO6 polyhedra separated by Na+ and Tl+ cations. NaTl3Cu4Te2O12 crystallizes in space group C2/m with a = 12.9800(17) ?, b = 9.3455(12) ?, c = 5.2335(7) ?, β = 104.276(2)°, V = 615.24(14) ?3, and Z = 2. 相似文献5.
Rachel C. Severance Adam H. Fox Samuel J. MugaveroIII Mark D. Smith Hans-Conrad zur Loye 《Journal of chemical crystallography》2011,41(4):496-501
Abstract
Two polymorphs of trilanthanum iridium septaoxide, La3IrO7, were prepared as single crystals using a molten cesium hydroxide flux and were structurally characterized using single-crystal X-ray diffraction. Polymorph A crystallizes in the orthorhombic space group Cmcm with unit cell dimensions of a = 11.2103(3) ?, b = 7.4982(2) ?, and c = 7.6110(2) ?. Polymorph B crystallizes into the monoclinic space group P21/n with the unit cell dimensions of a = 8.8512(5) ?, b = 5.7167(3) ?, c = 24.4454(13) ?, and β = 95.542(2)°. The crystal structure of polymorph A is isostructural to the family of compounds with formula Ln3MO7 (M = Nb5+, Mo5+, Ru5+, Ta5+, Re5+, Os5+, and Ir5+) while the crystal structure of polymorph B has no known corollaries. 相似文献6.
K. G. Sanjaya Ranmohotti Wendy L. Queen J. Palmer West Don VanDerveer Shiou-Jyh Hwu 《Journal of chemical crystallography》2009,39(4):303-307
Abstract A new barium chlorovanadate, Ba5(V2O7)2Cl2, was isolated by a high-temperature (850 °C) reaction employing a CsCl/RbCl flux. The structure was determined by single
crystal X-ray diffraction methods. This compound crystallizes in an orthorhombic crystal system, Pmmn (No. 59), with a = 11.558(2) ?, b = 15.164(3) ?, c = 10.023(2) ?, Z = 4 and V = 1756.7(6) ?3. The structure of Ba5(V2O7)2Cl2 was determined by full-matrix, least-squares methods with R
1 = 0.0398, wR
2 = 0.1069 and GOF = 1.048 for all data. This new structure can be described as a composite lattice made up of mixed covalent
and ionic moities. The extended framework is orchestrated by stacked [Ba(V2O7)Cl]3− slabs that are interconnected by Ba2+ cations through Ba–O bonds to the [V2O7] units. The Ba2+ and Cl- ions form BN-type “[BaCl]” sheets with pseudo-hexagonal windows that are centered by [V2O7]4− pyrovanadate units.
Graphical Abstract The structure of a new chlorovanadate, Ba5(V2O7)2Cl2, exhibits an interesting BN-type salt lattice that consists of an extended [BaCl] sheet containing pseudo-hexagonal windows
that are centered by [V2O7] pyrovanadate units.
相似文献
7.
Sridhar Balasubramanian Ravikumar Krishnan Krishnan Harihara 《Journal of chemical crystallography》2010,40(5):461-467
Abstract
The crystal structures of zolmitriptan with pyridine (I) and propiophenone (II) solvates have been determined by single crystal X-ray diffraction studies. Compound (I) crystallizes in the orthorhombic space group P212121 with a = 8.5610(5) ?, b = 12.2709(7) ?, c = 19.6201(12) ?, V = 2061.1(2) ?3, and Z = 4, while compound (II) crystallizes in the monoclinic space group P21 with a = 15.085(1) ?, b = 19.656(12) ?, c = 21.0860(13) ?, β = 92.068(1)°, V = 6248(4) ?3 and Z = 4. The asymmetric unit of (I), C16H21N3O2·C5H5N, contains one zolmitriptan molecule and one pyridine solvate, while the asymmetric unit of (II), 3(C16H21N3O2)·2(C9H10O) comprises six zolmitriptan molecules and four propiophenone solvates. In both structures, the N–H···N hydrogen bonds, form an infinite helical chain and generate a C(11)-type motif in (I) and a D22(13)-type motif in (II). Both the complexes have layer structures, the layers being constructed from rings (cavity) of four zolmitriptan molecules, hydrogen bonded through N–H···N and N–H···O bonds, where the pyridine (I) and propiophenone (II) solvates are included in an R44(33) ring. 相似文献8.
Wesley H. Monillas Glenn P. A. Yap Klaus H. Theopold 《Journal of chemical crystallography》2009,39(7):535-538
Abstract Addition LiNHPh to a [(NacNac)Cr(μ-I)]2 [NacNac = 2,4 pentane-N-N′-bis(2,6-diisopropylphenyl) ketiminato] in THF yields a dimeric anilido complex, 1, that crystallizes in P21/n with unit cell parameters a = 13.390(2) ?, b = 26.298(5) ?, c = 21.326(4) ?, β = 93.905(4)°, V = 7492(2) ?3 and Z = 4. The same reaction in the presence of aniline yields a monomeric anilido complex, 2, with a coordinated aniline molecule. Complex 2 crystallizes in P2
1
/c with unit cell parameters a = 28.530(5) ?, b = 10.8116(18) ?, c = 26.492(5) ?, β = 115.685(3)°, V = 7364(2) ?3 and Z = 8. Addition of aniline to isolated 1 yields 2. Addition of LiNPh2 to [(NacNac)Cr(μ-I)]2 in THF yields a monomeric complex that crystallizes in P21/n with the unit cell parameters a = 11.152(6) ?, b = 23.820(12) ?, c = 17.915(9) ?, β = 106.223(9)°, V = 4569(4) ?3 and Z = 4. All complexes have been spectroscopically and structurally characterized.
Graphical Abstract Addition of LiNHPh or LiNPh2 to [(NacNac)Cr(μ-I)]2 yields a dimeric or a monomeric complex whereas addition of LiNHPh in the presence of aniline yields the monomeric anilido
complex.
相似文献
9.
Wesley H. Monillas Tyler C. Bazzoli Glenn P. A. Yap Klaus H. Theopold 《Journal of chemical crystallography》2010,40(1):67-71
Abstract
The new ligand 2,4-N,N′-bis(napthylamino)-pent-2-ene (Lnapth) (1) has been synthesized and crystallizes in space group P212121 with crystal cell parameters a = 8.196(3) ?, b = 9.119(3) ?, c = 25.746(10) ?, V = 1924.3(12) ?3 and Z = 4. The complexes bis[2,4-pentane-N,N′-bis(napthyl)ketiminato] chromium(II) (2), bis[2,4-pentane-N,N′-bis(isopropylphenyl)ketiminato] chromium(II) (3), and bis[2,4-pentane-N,N′-bis(tertbutylphenyl)ketiminato] chromium(II) (4) were synthesized and structurally characterized. Complex 2, the first complex reported with a bis(napthyl) β-diketiminate ligand, crystallizes in space group P − 1 with crystal cell parameters a = 12.0824(15) ?, b = 12.2462(16) ?, c = 14.8975(19) ?, α = 87.035(2)°, β = 80.615(2)°, γ = 62.756(2)°, V = 1932.9(4) ?3 and Z = 2. Complex 3 crystallizes in space group P21/n with crystal cell parameters a = 13.088(3) ?, b = 22.222(5) ?, c = 14.206(3) ?, β = 102.310(4)°, V = 4036.6(17) ?3 and Z = 4. Complex 4 crystallizes in space group P21/n with crystal cell parameters a = 20.831(6) ?, b = 11.575(4) ?, c = 21.373(7) ?, β = 107.241(5)°, V = 4922(3) ?3 and Z = 4. The degree of twist between the ligand planes is dependent on the steric bulk of the ligand. 相似文献10.
Abstract
New copper(I) complex involving the flexible N2S2 Schiff-base ligand ca2dapte [Cu(ca2dapte)(NCS)], [ca2dapte = N,N′-bis-(cinnamaldehyde)-1,2-di(o-iminophenylthio)ethane], has been synthesized and structurally characterized by X-ray diffraction analysis. The coordination polyhedron around the Cu(I) center is best described as a distorted tetrahedron. The flexible N2S2 Schiff-base ligand ca2dapte acts as a tridentate ligand via two S atoms and one N atom, while the NCS- ligand is coordinated to the metal ion through its nitrogen atom. Crystal data: space group P-1, a = 10.7486(7), b = 12.3737(13), c = 12.7578(11) ?, α = 89.385(7), β = 68.527(7), γ = 66.190(8)°; V = 1425.8(2) ?3, Z = 2, R = 0.0417, wR 2 = 0.0744. 相似文献11.
Abstract
In order to investigate the intramolecular [4 + 2] cycloaddition, we prepared some new tertiary N-(5-substituted-2-furfuryl)-N-prop-2-ynyl-p-toluidines [Hergold-Brundić et al., Acta Cryst C56:e520, 2000; Mance and Jakopčić, Mol Divers 9:229, 2005; Mance, “unpublished results”] by the alkylation of secondary N-(5-substituted-2-furfuryl)-p-toluidines with the propargyl-bromide [Mance and Šindler-Kulyk, Synth Commun 26:923, 1996]. In the course of preparation of N-(5-methoxy-2-furfuryl)-N-prop-2-ynyl-p-toluidine [Mance, “unpublished results”], besides the main product (compound 1) (Scheme 1) we obtained N,N-di(prop-2-ynyl)-p-toluidine (compound 2) as the colourless crystals. The title compound 2, N,N-di(prop-2-ynyl)-p-toluidine, C13H13N, crystallizes in monoclinic C 2/c space group with unit cell parameters: a = 19.5319(9) ?, b = 7.5230(3) ?, c = 15.9000(7) ?, β = 112.554(5)°, V = 2157.64(18) ?3, Z = 8. The crystal structure is dominated by van der Waals forces only. The bond distances around amine N atom correspond to σ dominated bonds (1.467(2), 1.462(2) and 1.419(2) ?). The angles sum around amine N atom is in accord with sp3 hybridization (343°). 相似文献12.
Shu-Ni Li Quan-Guo Zhai Man-Cheng Hu Yu-Cheng Jiang 《Journal of chemical crystallography》2011,41(1):12-16
Abstract
Two novel complexes constructed from the sulfonamide Schiff base ligand H 2 L, N-[2-(5-bromo-2-hydroxybenzylideneamino)ethyl]-4-methylbenzene-sulfonamide, [Cu(HL)2] (1) and [CuL(H2O)] (2) are synthesized and characterized via X-ray single-crystal diffraction, elemental analysis, FT-IR and UV–Vis. 1 and 2 both form 1-D supramolecular architectures by π–π stacking interactions. 1 and 2 both crystallize in monoclinic, with space group C2/c and P2/c for 1 and 2, with unit cell parameters a = 27.640(18) ?, b = 7.907(5) ?, c = 17.945(14) ?, β = 118.27(2)°, V = 3454(4) ?3, Z = 4 for 1, and a = 16.758(5) ?, b = 7.272(2) ?, c = 15.080(4) ?, β = 106.334(5)°, V = 1763.6(9) ?3, Z = 4 for 2. 相似文献13.
Brian E. Zaugg Torsten Kolb Atta M. Arif Richard D. Ernst 《Journal of chemical crystallography》2010,40(9):778-782
Abstract
The structure of the previously reported (py)3ZnFe(CO)4 (py = pyridine) has been determined, confirming the monomeric nature of this species. The complex has average Zn–N and Zn–Fe bond lengths of 2.0970(7) and 2.4017(3) ?, and features a coordination geometry about Fe which is intermediate between trigonal bipyramidal and face monocapped tetrahedral. The space group is P21/c, with a = 8.22080(10) ?, b = 16.1668(3) ?, c = 15.4669(3) ?, β = 102.5869(11)°, V = 2006.21(6) ?3, Dcalc. = 1.558 g/cm3 at 150(1) K. A monomeric cadmium analogue, (pyridine)(neocuproin)CdFe(CO)4, has also been synthesized, and found to possess a similar geometry, with average Cd–N and Cd–Fe bond lengths of 2.352(2) and 2.5380(5) ?. The space group is P[`1] P\overline{1} with a = 10.8900(2) ?, b = 11.3042(3) ?, c = 15.5488(4) ?, α = 85.1251(10)°, β = 84.3468(14)°, γ = 72.0377(15)°, V = 1808.93(7) ?3, Dcalc. = 1.478 g/cm3 at 150(1) K. 相似文献14.
Abstract
The aryl functionalized diquinolyl amine MesN(quin)2 (1) and the pyridyl-quinolyl amine (2,6-iPr2C6H3)N(py)quin (2) have been prepared via palladium catalyzed cross-coupling of substituted anilines with 2-chloroquinoline. The HBF4 acid salts of (2,6-iPr2C6H3)N(quin)2 (3) and MesN(py)quin (4), as well as the copper complex [Cu{PhN(py)quin}Cl2] (5) have been prepared in order to probe the effect that ligand coordination has on its geometry. The molecular structures of each have been determined by X-ray crystallography. The free ligands 1 and 2 crystallize in three-bladed propellar conformations, having smaller degrees of “pitch” between the two heterocycles than either has with the aryl “blade”, allowing for greater heterocycle π-system overlap with the amine lone pair. Acid confinement of similar ligands in 3 and 4 results in forced coplanarity of the two heterocycles, which coordinate the HBF4 proton in an asymmetric fashion. The copper complex 5 crystallizes with both monomeric and dimeric forms present in the asymmetric unit. Crystal data: (1) Space group P21/c, a = 14.058(3), b = 12.202(2), c = 12.831(3) ?, β = 104.61(3)°, V = 2129.8(8) ?3, Z = 4, R = 0.0596, wR2 = 0.1453. (2) Space group P21/c, a = 22.250(4), b = 8.628(2), c = 23.031(5) ?, β = 92.88(3)°, V = 4370(2) ?3, Z = 8, R = 0.0514, wR2 = 0.1323. (3) Space group Pbca, a = 13.886(3), b = 18.016(4), c = 21.347(4) ?, V = 5340(2) ?3, Z = 8, R = 0.0722, wR2 = 0.1635. (4) Space group P21/c, a = 10.629(2), b = 18.489(4), c = 10.907(2) ?, β = 92.88(3), V = 2140.6(7) ?3, Z = 4, R = 0.0551, wR2 = 0.1531. (5) Space group \text P[`1]{\text P}\bar{1}, a = 9.706(2), b = 11.325(2), c = 17.322(4) ?, α = 98.28(3), β = 94.85(3), γ = 91.83(3)°, V = 1875.6(7) ?3, Z = 1, R = 0.0481, wR2 = 0.0946. 相似文献15.
Annamária Krajníková Róbert Gyepes Katarína Győryová 《Journal of chemical crystallography》2010,40(8):650-655
Abstract
The syntheses and structural characterizations of two novel 2-bromobenzoatozinc(II) complexes—[Zn(2-BrC6H4COO)2] n (I) and [Zn(2-BrC6H4COO)2(mnad)]2 (II), where mnad is N-methylnicotinamide are reported. Compound (I) crystallized with a monoclinic lattice (space group P21/c) and is polymeric in solid state. Its cell parameters are: a = 7.37220(10) Å, b = 19.9639(3) Å, c = 30.2756(5) Å, β = 94.7510(7)°, V = 4440.59(12) Å3, Z = 4. The coordination environments of all zinc atoms are distorted tetrahedra built from four carboxylate oxygen atoms coming from four 2-bromobenzoato ligands. Compound (II) crystallized with a monoclinic lattice (space group P21/c) with a = 11.7488(2) Å, b = 20.3683(3) Å, c = 9.30130(10) Å, β = 100.3941(11)°, V = 2189.30(5) Å3, Z = 2. This dimeric molecule features a paddle-wheel [Zn2O8] cage in solid state; the coordination environment of the central atom is square pyramidal consisting of four carboxylate oxygen atoms and the pyridine N atom of the mnad ligand. 相似文献16.
Souad Chaouche Rachid Ouarsal Brahim El Bali Mohammed Lachkar Michael Bolte Michal Dusek 《Journal of chemical crystallography》2010,40(6):526-530
Abstract
Crystal structure of Li2HPO3,H2O was determined by single-crystal X-Ray diffraction analysis at 173(2) K. It crystallizes in the monoclinic system (P21/c) with the parameters: a = 5.0322(9) ?, b = 8.9795(17) ?, c = 17.088(4) ?, β = 92.672(16)° and Z = 8. The structure was refined to R = 0.0237 and ωR = 0.0650 for 1449 reflexions. The framework of Li2HPO3, H2O can be described as layers perpendicular to the crystallographic c axis. The structure contains two types of Li-tetrahedrons. In one kind each O atom belongs to one HPO3 group, while in the second kind one apex is an O from water. A network of hydrogen bonds interactions insures the connection between the layers. 相似文献17.
Wesley H. Monillas Glenn P. A. Yap Klaus H. Theopold 《Journal of chemical crystallography》2009,39(11):849-852
Abstract
The complexes (bis(2,6-diisopropylphenyl)pentane-2,4-ketiminato)(μ2-diisopropylacetamidinato) chromium(II) (1) and (bis(2,6-diisopropylphenyl)pentane-2,4-ketiminato)(μ2-dicyclohexylacetamidinato) chromium(II) (2) have been synthesized and structurally characterized. Complex 1 crystallizes in space group Pbcn with crystal cell parameters a = 10.7183(13) ?, b = 16.4093(19) ?, c = 20.687(2) ?, V = 3,638.3(7) ?3 and Z = 4. Complex 2 crystallizes in triclinic space group P-1 with crystal cell parameters a = 10.750(3) ?, b = 12.174(3) ?, c = 16.308(4) ?, α = 75.903(4)°, β = 82.137(4)°, γ = 85.511(4), V = 2,048.4(8) ?3 and Z = 2. The complexes adopt a spiro distorted square planar geometry and have similar structural parameters. 相似文献18.
Jin-Xiu Wang Xiao-Zeng Li Li-Na Zhu Ji-Yao Wang Hao Qu 《Journal of chemical crystallography》2010,40(9):726-730
Abstract
A new complex [Fe(N-isonicotinamidosalicylaldimine)Cl2] has been synthesized by template reaction at room temperature and structurally characterized by X-ray single-crystal analysis. The complex crystallizes in triclinic crystal system, Pī space group, a = 7.273(6) ?, b = 10.015(8) ?, c = 10.479(8) ?, α = 71.067(10)°, β = 89.964(11)°, γ = 75.528(10)°, V = 696.4(9) ?3 and Z = 2. The coordination geometry around the Fe(III) ion is a distorted trigonal bipyramid with a O2N1Cl2 donor set. In the crystal structure, N–H···Cl, C–H···O and C–H···Cl hydrogen bonds and π···π stacking interactions involving aromatic and unclosed π-systems link the molecules to form supramolecular double layers. 相似文献19.
Abstract
The synthesis and crystal structure are given for the bis(3-dimethylammonium-1-propyne)pentachlorobismuthate(III) salt. An X-ray investigation has shown that the title compound crystallizes at 298 K in a centrosymmetric monoclinic system, space group C2/c with the following lattice parameters a = 12.6215(4) ?, b = 18.9228(5) ?, c = 8.3134(2) ?, β = 104.100(2)°, V = 1925.70(9) ?3. The structure was solved from 7,716 independent reflections with R 1 = 0.0457 and wR 2 = 0.0906, and refined with 85 parameters. The structure consists of disordered 3-dimethylammonium-1-propyne, C5H9NH+ cations and polynuclear anions in which slightly distorted (BiCl5)2− anions, sharing an apex are interconnected in chains. These chains are themselves interconnected by means of N–H···Cl originating from the C5H9NH+ entities, forming a three-dimensional network. 相似文献20.
Michael Findlater Nicholas J. Hill Alan H. Cowley 《Journal of chemical crystallography》2010,40(1):64-66