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1.
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
2.
The title compound crystallizes in the space group P21/n, with a = 18.423(3), b = 9.628(3), c = 19.243(2) Å, = 116.208(8)°, with two independent molecules in the asymmetric unit, which are not enantiomers. The chiral centers C8a, C9, C12, C12a, C12b are either S,R,S,R,R or R,S,R,S,S, respectively, because of the centric space group. 相似文献
3.
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4.
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5.
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
6.
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.
R. Alan Howie Edward R. T. Tiekink James L. Wardell Solange M. S. V. Wardell 《Journal of chemical crystallography》2009,39(4):293-298
Abstract The central mercury atom in Hg[S2CN(CH2CH2OH)2]2 is asymmetrically chelated by two dithiocarbamate ligands leading to a distorted square planar geometry. Molecules aggregate
into supramolecular chains via Hg···S interactions that are connected into a three dimensional array by extensive hydrogen
bonding interactions. The compound crystallizes in the orthorhombic space group Pna21 with a = 13.8173(7) ?, b = 4.5307(1) ?, c = 26.0261(12) ?, and Z = 4.
Index Abstract Molecules associate into supramolecular chains via Hg···S interactions and these are connected into a three dimensional architecture
by O–H···O hydrogen-bonding interactions.
相似文献
9.
The crystal structure of [C12H14N2O2S]SeO4 · [C12H12N2O2S] was determined by X-ray diffraction on single crystal. Crystals are orthorhombic, space group Pbca, with cell parameters a = 11.545 (1), b = 8.143 (1), c = 55.783(1)Å, V = 5244.2 (8)Å3 and Z = 8. The structure can be described as organic layers built by [C12H14N2O2S]2+ cations and [C12H12N2O2S] molecules, parallel to ab plane, between which the inorganic groups SeO 4 2? are inserted. In this atomic arrangement, H-bonds between the different species play an important role in the three-dimensional network cohesion. 相似文献
10.
Yinxiang Lu 《Journal of chemical crystallography》2011,41(9):1395-1399
Abstract
The title compounds, Methyl N-(4-methoxyphenylmethyl)-N′-cyanocarbamimidothioate, I, and Methyl N-[1-(phenylmethyl)-4-piperidinyl]-N′-cyanocarbamimidothioate, II, have been designed and synthesized for use as new potential organic molecular electronic materials. The crystal structure of I and II were determined with crystal data (I: Monoclinic, P21/c, a = 4.746(2) ?, b = 5.737(3) ?, c = 17.399(7) ?, β = 91.667(7)o, R all = 0.0703; II: Orthorhombic, Pna21, a = 18.209(8) ?, b = 11.463(5) ?, c = 7.539(3) ?, β = 90.00 o, R all = 0.0481). N–H···N hydrogen bonds were responsible for the formation of one-dimensional zigzag molecular chains of I, and trifurcated hydrogen-bonded molecular chains were indicated in structure of II. C–H···π and C–H···N hydrogen bonds were found in both structures. All these types of interaction together form an extended three-dimensional network and stabilize the title crystals. 相似文献11.
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12.
Elin Abraham Stephen G. Davies Paul M. Roberts Amber L. Thompson James E. Thomson 《Journal of chemical crystallography》2011,41(11):1722-1728
Abstract
Crystals of the dimeric β-peptides 13 and 20, derived from (1R,2S)-2-aminocyclopentanecarboxylic acid and (1S,2R,3S)-2-amino-3-methylcyclopentanecarboxylic acid, respectively, were synthesised and studied by X-ray diffraction in order to establish their solid state secondary structural characteristics. Compound 13 crystallises in the monoclinic space group P 2 1 with cell parameters of a = 5.2682(1) ?, b = 9.1211(2) ?, c = 22.4467(6) ?, β = 91.3855(9)°, V = 1078.29(4) ?3 and Z = 2. Compound 20 crystallizes in the orthorhombic space group P 2 1 2 1 2 1 with cell parameters of a = 5.0968(1) ?, b = 11.5546(2) ?, c = 43.5414(8) ?, V = 2564.22(8) ?3 and Z = 4. In both cases adjacent molecules are linked by a series of N–H···O=C hydrogen bonds to form β-sheet like structures. 相似文献13.
Mino R. Caira Ashutosh V. Bedekar Vishwakarma Singh 《Journal of chemical crystallography》1995,25(9):583-587
A single crystal X-ray diffraction study of two annulated bicyclo[2.2.2]octenones has been carried out to establish their precise stereostructures. The compounds, with their crystal data, are:1, 9-hydroxy-9-chloromethyl-endo-tricyclo[5.2.2.02,6]undeca-4,10-diene-3-spiro(1-cyclopropane)-8-one, C14H15O2Cl, space group P21/c,a=10.540(2),b=9.668(1),c=11.841(4)Å, =95.67(2)°,Z=4, and2, 12-hydroxy-12-chloromethyl-endo-tricyclo[8.2.2.02,9]tetradeca-13-en-11-one, C15H21O2Cl, space group C2/c,a=20.747(8),b=6.498(1),c=20.525(3)Å, =93.04(3)°,Z=8. The molecule of1 has endo stereochemistry at the ring junction and the spirocyclopropane ring is proximal to the hydroxyl group. In2, the eight membered ring deviates from a chair conformation and one ring atom is disordered. Crystals of1 and2 contain centrosymmetric dimers formed by C=O...O–H hydrogen bonds. 相似文献
14.
Jin-Min Li 《Journal of chemical crystallography》2009,39(2):143-146
Abstract Hydrated cadmium perchlorate reacted with sodium azide and 2,2′-bypyridine-3,3′-diol (H2L) in ethanol solution and resulted in the formation of a two-dimensional coordination polymer: [Cd(μ-N3)(μ-HL)(H2O)]n. The complex has been characterized by elemental analysis and IR spectrum, and its crystal structure determined by X-ray
crystallography and the complex crystallizes in the monoclinic system with space group P21/c and a = 7.2849(14), b = 9.9568(19), c = 17.058(3) Ǻ, β = 102.254(2)°. In the complex both azide anion and monodepronated 2,2′-bypyridine-3,3′-diol anion (HL) act as bridge ligands
and led to the formation of a two-dimensional sheet structure on (100) plane, and the O–H⋯N hydrogen bond made the sheets
pile up along [100] direction, which forms a supramolecular three-dimensional structure.
Graphical Abstract The title two-dimensional Cd(II) coordination polymer was synthesized by cadmium perchlorate, sodium azide and 2,2′-bypyridine-3,3′-diol
and its crystal structure determined. Single crystal X-ray diffraction analysis reveals that the two-dimensional coordination
polymer was fabricated with azide anion and monodeprotonated 2,2′-bypyridine-3,3′-diol as mixed bridge ligands.
相似文献
15.
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16.
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17.
George D. Bennett Lauren R. Bringman Elise M. Wildman Kraig A. Wheeler 《Journal of chemical crystallography》2010,40(1):76-79
Abstract
The title compounds, C10H12O4 and C12H14O5, were prepared as part of an ongoing study to explore the practical aspects of solventless reaction methods. As confirmed by the crystal structures, treatment of maleic anhydride with (2E,4E)-hexa-2,4-dien-1-ol or its acetate counterpart resulted in cis bicyclo [4.3.0] molecular frameworks. The racemic product derived from the dienol synthon crystallized in chiral space group P212121 via a pasteurian resolution process with molecules organized by carboxyl⋯carboxyl and C–H⋯O contacts. The acetate derivative crystallizes in space group Cc. 相似文献18.
Junqing Chen Min Sun Jin Cai Meng Cao Wen Zhou Min Ji 《Journal of chemical crystallography》2011,41(4):519-522
Abstract
(4α,8β,13β,16β)-13-methyl-16,18-diol-17-norkaurane was synthesized by esterification and reduction of isosteviol, respectively. The structure of the title compound was established by spectral analysis and X-ray diffraction studies. The compound crystallizes in the orthorhombic space group P212121 with unit cell parameters: a = 7.3705 (14) ?, b = 13.508 (3) ?, c = 20.139 (4) ?, V = 2005.1 (7) ?3, Z = 4. The conformation of rings A and B is chair, whereas the conformation of ring C is unsymmetrical distorted chair. The stereochemistry of the A/B and B/C ring junctions is trans, while the five-membered ring D adopts an envelope conformation. 相似文献19.
A. P. Polishchuk N. N. Makarova T. V. Astapova É. B. Rusanov 《Crystallography Reports》2001,46(6):953-958
The crystal structures of two organosilicon compounds are studied by X-ray diffraction at 200 K. Crystals of 2,2′,4,4′,6,8,8′,10,10′,12-decamethylbicyclo[5.5.1]hexasiloxane (C10H30O7Si6) are monoclinic, a = 12.260(1) Å, b = 11.716(1) Å, c = 32.169(2) Å, β = 92.802(2)°, space group C2/c, Z = 8, wR2 = 0.132, and R1 = 0.053 for 3989 reflections with F > 4σ(F). Crystals of 2,2′,4,4′,6,8,8′,10,10′, 12-decamethylbicyclo[5.5.1]-9-carbahexasiloxane (C11H32O6Si6) are triclinic, a = 10.709(1) Å, b = 11.046(1) Å, c = 12.111(1) Å, α = 117.059(1)°, β = 95.566(1)°, γ = 108.088(1)°, space group $P\bar 1$ , Z = 2, wR2 = 0.115, and R1 = 0.048 for 3948 reflections with F > 4σ(F). It is found that the substitution of the methylene group for the oxygen atom is accompanied by a minor conformational change in the bicyclic fragment and the SiCSi angle changes from the tetrahedral angle to 121.0(1)°. The high variability of the SiOSi bond angles is confirmed. 相似文献