共查询到20条相似文献,搜索用时 31 毫秒
1.
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2.
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3.
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4.
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5.
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6.
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7.
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
8.
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
9.
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10.
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
11.
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
12.
Miguel A. Harvey María E. Díaz de Vivar María T. Garland Sergio Baggio 《Journal of chemical crystallography》2011,41(2):155-158
Abstract
The title compound is monomeric with a Ni(II) hexacoordinated center. The coordination sphere is formed with four nitrogens from two neocuproine molecules and two oxygens from a sulfate ion that acts as a bidentate ligand. A water molecule completes the formula with an important role in the stabilization of the structure through the formation of OW–H···OS bridges, in which it acts as a donor and interactions of the type Car–H···OW and CMet–H···OW, where it is an acceptor group (W: water; S: sulfate; ar: arene; Met: methyl). The compound is monoclinic, space group P21 /c with a = 14.4829(4) ?, b = 14.4563(4) ?, c = 12.1559(3) ?, β = 94.407(1)°, V = 2,537.55(12) ?3 and Z = 4. The structure was solved by direct methods with a conventional R (on F) = 0.0359 for 4841 reflexions with Fo > 4σ(Fo). Three levels of super-structural hierarchy can be identified in the crystal construction: (1) the primary structure corresponding to the molecular skeletons of their building blocks, the isolated complex itself and the water molecule, (2) an 1D supramolecular array that form chains through a non-covalent polymerization via interactions OW–H···OS, Car–H···OW, Car–H···OS and CMet–H···OW and (3) finally the 3D macroscopic conglomerate formed through inter-chains interactions Car–H···OW, Car–H···OS, CMet–H···ar and offset stacked arene–arene. 相似文献13.
Zuzana Bujdo?ová Katarína Gy?ryová Milan Melník Marian Koman Jana Ková?ová 《Journal of chemical crystallography》2011,41(4):443-448
Abstract
Two ligand isomers [Zn{4-ClC6H3-2-(OH)COO}2(Menia)2(H2O)2] (I) and [Zn{5-ClC6H3-2-(OH)COO}2(Menia)2(H2O)2] (II) (Menia = N-methylnicotinamide) were prepared and characterized by elemental analysis, IR spectroscopy and thermal analysis. The X-ray crystal structures of complexes (I) and (II) were determined. Compound (I) crystallizes in the triclinic space group P[`1] P\bar{1} with a = 8.105(1) ?, b = 10.036(2) ?, c = 10.545(2) ?, α = 109.088(9)°, β = 91.416(8)°, γ = 102.757(9)°, V = 786.2(2) ?3, Z = 1. Compound (II) crystallizes in the triclinic space group P[`1] P\bar{1} . Its cell parameters are: a = 8.133(1) ?, b = 10.119(2) ?, c = 10.428(1) ?, α = 66.44(1)°, β = 74.32(1)°, γ = 80.16(1)°, V = 755.5(2) ?3, Z = 1. The molecular structure of both isomers is monomeric. Each Zn(II) atom is hexacoordinated by three pairs of unidentate ligands in trans-positions (ZnO4N2). The 5-Clsal complex is somewhat less distorted than 4-Clsal complex (Cl-sal = chlorosalicylate). The structural data are compared with those found in similar [Zn(RCOO)2(NL)2(H2O)2]. 相似文献14.
Shu-Lin Ma Shi Ren Yue Ma Shi-Ping Yan Dai-Zheng Liao 《Journal of chemical crystallography》2010,40(11):1011-1015
Abstract
A mononuclear fragment [Cu(L)Cl]ClO4 (1) and a cyano-bridged CuII–NiII binuclear complex [CuL][Ni(CN)4]·0.25H2O (2) (L = 1,3,6,8,11,14-hexaazatricyclo[12.2.1.18,11]-octadecane), have been prepared and characterized. X-ray single crystal analyses indicate that the both complexes crystallize in the monoclinic crystalline system. The complex of 1 in P1n1 space group with unit cell constants a = 6.1176(6) ?, b = 11.9147(10) ?, c = 12.2041(12) ?, β = 98.816(5)° and 2 in the P21/n space group with unit cell constants a = 8.1419(13) ?, b = 14.695(2) ?, c = 16.863(3) ?, β = 98.375(2)° have been revealed. The complex 2 assumes a binuclear structure in which the nickel(II) ion is in a square planar environment and the copper(II) is in a square-prism geometry environment. 相似文献15.
E. M. Vázquez-López A. Castiñeiras A. Sánchez J. S. Casas J. Sordo 《Journal of chemical crystallography》1992,22(4):403-409
The phenylmercury(II) derivatives PhHgS2P(OR)2 (R=C2H5, C6H11 and C6H5) have been synthesized. (O,O-diethyldithiophosphate) phenylmercury(II), C10H15HgO2PS2, crystallizes in the monoclinic space groupP21/c (n° 14) witha=7.330(5),b=18.085(2),c=11.552(4)Å,=105.96(5)°,V=1472.3(6)Å3,Z=4,D=2.088 g.cm–3. The mercury atom is coordinated to the phenyl carbon atom and to a ligand sulphur atom in an almost linear arrangement (C-Hg-S angle, 176.0(2)°. The ligand is almost monodentate, its second sulphur atom only being involved in a weak secondary intermolecular bond.IR and Raman studies of the other two compounds suggest the same coordination scheme. Positive ion FAB and13C,31P and199Hg NMR spectra are also discussed. 相似文献
16.
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
17.
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18.
L. S. Smirnov K. Wozniak P. Dominiak A. Loose I. Natkaniec M. V. Frontasyeva E. V. Pomyakushina A. I. Baranov V. V. Dolbinina 《Crystallography Reports》2008,53(3):418-427
The crystal structure of a mixed [Rb0.11(NH4)0.89]3H(SO4)2 crystal was refined using single-crystal X-ray and neutron diffraction at 300 K. The refinement confirmed that the phase
II of the crystal belongs to the monoclinic crystal system (space group C2/c). It was shown that, according to the single-crystal neutron diffraction data, ammonium ions can be represented as regular
tetrahedra. The analysis of the constructed difference Fourier maps of the electron and nuclear densities of ammonium ions
revealed the presence of additional peaks, which can indicate the dynamic disorder of ammonium ions in the phase II. The results
obtained con-firmed that the phase transition to the orientational-glass state can occur in the mixed [Rb0.11(NH4)0.89]3H(SO4)2 crystal with a decrease in the temperature.
Original Russian Text ? L.S. Smirnov, K. Wozniak, P. Dominiak, A. Loose, I. Natkaniec, M.V. Frontasyeva, E.V. Pomyakushina,
A.I. Baranov, V.V. Dolbinina, 2008, published in Kristallografiya, 2008, Vol. 53, No. 3, pp. 450–459. 相似文献
19.
G. Jovanovski A. Hergold-Brundić O. Grupče D. Matković-Čalogović 《Journal of chemical crystallography》1999,29(2):233-237
The structure of (2,2-bipyridine)lead(II) saccharinate monohydrate has been investigated by X-ray diffraction. The compound crystallizes in the monoclinic space group P2
1/n with a = 22.903(7), b = 12.608(3), c = 8.682(2) Å, = 96.76(3)°, and Z = 4. The structure consists of Pb2+ cations, 2,2-bipyridine ligands, saccharinato anions and water molecules. The Pb2+ cation is surrounded by two O atoms and four N atoms. The two saccharinato ions are nonequivalent. The water molecule forms hydrogen bonds of OW···OCO [2.810(16) Å] and OW···OSO2 [2.893(16) Å] type. 相似文献
20.
A. V. Shlyakhtina A. E. Sokolov V. A. Ul’yanov V. A. Trunov M. V. Boguslavski? A. V. Levchenko L. G. Shcherbakova 《Crystallography Reports》2009,54(1):25-30
The crystal structure of pyrochlore-like solid solutions (Yb1 − x
Ca
x
)2Ti2O7 (x = 0, 0.05, 0.10) synthesized by high-temperature annealing of mechanically activated initial oxides at temperatures of 1300–1500°C
is studied using neutron diffraction. It is found that the Ca2+ cations are located in the ytterbium sublattice, which apparently favors the splitting of one of the oxygen sublattices [O(2)
(48f)] of the pyrochlore structure: the decrease in the occupancy of this sublattice is accompanied by the formation of a new
sublattice O(3) (8b), whereas the other oxygen sublattice O(1) (8a) remains unchanged. This rearrangement of the anions in the oxygen subsystem due to the incorporation of an alkaline-earth
cation explains the high ionic conductance (∼0.2 S/cm at 1000°C) for (Yb0.9Ca0.1)2Ti2O7 ∼ 0.2, which is the maximum value observed to date for pyrochlores of the A
2
B
2O7 type, where A = Ln and B is a Subgroup IVA element of the periodic system. The bulk and grain-boundary components of the conductivity of (Yb0.95Ca0.05)2Ti2O7 synthesized at temperatures of 1300, 1400, and 1500°C are studied using impedance spectroscopy. It is found that the (Yb0.95Ca0.05)2Ti2O7 sample synthesized at 1500°C has the highest total conductivity due to the increased grain-boundary component. The bulk component
of the ionic conductivity of (Yb0.95Ca0.05)2Ti2O7 is hardly affected by the synthesis temperature and depends mainly on the degree of heterovalent substitution.
Original Russian Text ? A.V. Shlyakhtina, A.E. Sokolov, V.A. Ul’yanov, V.A. Trunov, M.V. Boguslavskiĭ, A.V. Levchenko, L.G.
Shcherbakova, 2009, published in Kristallografiya, 2009, Vol. 54, No. 1, pp. 31–36. 相似文献