共查询到20条相似文献,搜索用时 15 毫秒
1.
K. Subramanian S. Lakshmi K. Rajagopalan Thomas Steiner Evgeni B. Starikov 《Journal of chemical crystallography》1998,28(7):581-584
In the X-ray crystal structure of the alkynol 5-hydroxy-5-(prop-2-ynyl)-10-methyl-1(9)-octalin-2-one [C14H18O2, Pca2
1, a = 13.559(1), b = 7.960(2), c = 21.748(3) Å], the hydroxyl and propynyl groups form a hydrogen bond chain C---C-HO-HO which is supposed to be a cooperative arrangement. Quantum chemical calculations estimate cooperativity enhancement within the array to be 0.4 kcal/mol, which is only a small (but recognizable) effect. 相似文献
2.
Cun-Gen Zhang Yong-Jun Leng Zi-Feng Ma De-Yue Yan 《Journal of chemical crystallography》1999,29(10):1081-1084
Preparation of the mononuclear cobalt(II) complex, [Co(bipy)(maleato) (H2O)3]·H2O (1) where bipy = 2,2-bipyridine, were accomplished by reaction of an aqueous solution containing sodium maleate and an ethanolic solution of Co(NO3)2·6H2O and bipy. The crystal structure of complex (1) was determined by X-ray crystallography. The complex crystallizes in the monoclinic space group P21/n with a = 9.477(3), b = 7.660(2), c =23.526 (3) Å, = 97.64(2)°, V = 1692.6(6) Å3, and Z = 4. The structure consists of discrete mononuclear cobalt molecules. The cobalt atom is six-coordinate and presents a slightly distorted octahedral geometry, which consists of the two imine N atoms of bipy, a terminal carboxylate O atom from maleato ligand, and a water O atom in the basal plane with Co—N bond distances of 2.116(2) and 2.124(3) Å and Co—O distances of 2.075(2) and 2.088(2) Å, respectively. The relatively shorter Co—O distances are due to the trans effect of the bipy ligand. The octahedral coordination is completed the other two water molecules. The coordinate and the lattice water molecules were identified by TG study. 相似文献
3.
The title compound is monoclinic,P21/n,Z=4,a=9.934(1),b=18.399(2),c=11.098(2)Å, =111.08(1)°. The molecule can conveniently be visualized as a benzophenone molecule with one of the aromatic rings fused to a 1,3-dioxin ring which adopts a distorted envelope conformation withcis-trichloromethyl groups substituted at positions 2 and 4. An interaction, observed for the first time, involves a hydrogen atom and a chlorine atom from opposite sides of the same aromatic ring to give C-H-(Ar)Cl-C. The parameters are Hring-centroid 2.63 A, Clring centroid 3.41 Å, Hring-centroidCl 167°, C-Hring centroid 159°, C-Clring centroid 150.2°. The (Ar) system is that of the unfused aromatic ring. A second (Ar) Cl-C interaction occurs but this time with the (Ar) system of the fused aromatic ring. The ClCl and ClO(=C) interactions form the familiar zig-zag pattern which has been noted for many chloroaromatic compounds. 相似文献
4.
Wansheng You Zaiming Zhu Enbo Wang Lin Xu Changwen Hu 《Journal of chemical crystallography》2000,30(9):577-581
[(H3O)(C14H20O5)2][Me2NH2]2 [PMo12O40] · 2C14H20O5
1 was synthesized from benzo-15-crown-5 and H3PMo12O40·24H2O in N,N-dimethylformamide for the first time. 1 crystallizes in the monoclinic space group C2/c with a = 18.583(4), b = 25.510(5), c = 19.904(4) Å, = 94.66(3)° D
c = 2.124 mg/m3 for Z = 4. Refinement based on 7358 observed reflections led to a R1(wR2) = 0.0378(0.0761). The complex cation, [(H3O)(C14H20O5)2]+, exhibits a sandwich structure by hydrogen-bonding in the mean distance of 2.955 Å. The anion, PMo12O40
3–, is a -Keggin structure. 相似文献
5.
Simon G. Bott Huafeng Shen Michael G. Richmond 《Journal of chemical crystallography》1998,28(5):385-399
Thermal and Me3NO-assisted activation of the donor–acceptor complex Ru2(CO)6(bpcd) (1) [where bpcd = 4,5-bis(diphenylphosphino)-4-cyclopenten-1,3-dione] with PMe3 or tBuNC affords the mono-substituted complexes Ru2(CO)5L(bpcd), as a result of regiospecific ligand attack at the diphosphine-substituted ruthenium center. Solution NMR measurements (1H and 31P) reveal that the PMe3 derivative exists as a noninterconverting mixture of axial (3a) and equatorial (3e) isomers, with the only the equatorial isomer being observed for Ru2(CO)5(tBuNC)(bpcd) (5). Near-UV irradiation of 1 in the presence of added ligand yields Ru2(CO)5L(bpcd), in addition to the known 2-phosphido complex Ru2(CO)6 [-C=C(PPh2)C(O)CH2C(O)](2-PPh2) (2) and the corresponding phosphido-substituted complexes Ru2(CO)5L[-{C =C(PPh2)C(O)CH2C}(O)]2-PPh2)[4 (L = PMe3); 6 (L = tBuNC)]. As with compounds 3a, 3e, and 5, both 4 and 6 exhibit ligand attachment at the diphosphine-substituted ruthenium center. The molecular structures of 3e, 4, 5, and 6 were determined by X-ray crystallography. 3e, as the 1/2 C6H6 solvate, crystallizes in the monoclinic space group C2/c: a = 40.573(3) Å, b = 10.2663(9) Å, c = 18.347(1) Å, = 95.371(6)°, V = 7609(1) Å3 and Z = 8; 4, crystallizes in the monoclinic space group P21/n: a = 10.8241(8) Å, b = 18.074(1) Å, c = 19.194(1) Å, = 96.968(6)°, V = 3727.3(5) Å3, and Z = 4; 5, as the 1/2CH2Cl2 solvate, crystallizes in the monoclinic space group C2/c: a = 40.955(3) Å, b = 9.7230(6) Å, c = 20.542(1) Å, = 106.596(5)°, V = 7839.2(9) Å3, and Z = 8; 6, as the 1/2C5H12 solvate, crystallizes in the monoclinic space group P21/c: a = 21.773(2) Å, b = 10.907(3) Å, c = 18.744(4) Å, = 114.68(1)°, V = 4045(1) Å3, and Z = 4. The site occupied by the PMe3 and tBuNC ligands in these compounds is discussed relative to the steric size/electronic properties of the ancillary ligand and its interaction with the bpcd ligand. 相似文献
6.
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
7.
Crystallography Reports - The structure and thermal properties of azobenzene derivatives R1–C6H4–N=N–C6H4–R2, where R1/R2 = CH3COO/C2H5O (I), CH2=C(CH3)COO/C2H5 (II), or... 相似文献
8.
Fangfang Jian Kui Jiao Qingxiang Wang Huanxiang Wang 《Journal of chemical crystallography》2004,34(2):147-151
The mononuclear complex, Ni[N3-ImSP(OiPr)2]2[S2P(OiPr)2]2 (Im = imidazole; iPr = isopropyl), was unexpectedly obtained in a reaction of bis(O,O-diisopropyl-dithiophosphato) nickel(II) complex with imidazole ligand, and its structure was determined by X-ray crystallography. It crystallizes in the triclinic system, space group P
, with lattice parameters a = 12.437(3) Å, b = 13.181(3) Å, c = 8.4580(17) Å, = 93.16(3)°, = 101.93(3)°, = 65.26(3)°, and Z = 1. The Ni atom has almost perfect octahedral coordination geometry and is coordinated by two N atoms of imidazole from two O,O-diisopropylthiophosphoryl-1H-imidazole ligands in axial positions and four S atoms from two (O,O-diisopropyldithiophosphato) anions which act as bidentate ligands forming a four-membered chelate ring in the equatorial plane. The Ni—S bond distances are 2.469(1) and 2.507(1) Å, and the Ni—N bond distances are 2.097(2) Å. The IR spectra data are in agreement with the structural data. 相似文献
9.
William H. Watson Jie Liu Michael G. Richmond 《Journal of chemical crystallography》2005,35(3):249-258
The reaction of the terminal alkyne methyl propiolate with the heterometallic dimers CoRu(CO)7(μ-PPh2) (1) and CoRu(CO)5[(Z)-Ph2PCH=CHPPh2](μ-PPh2) (2) has been investigated at 65°C in toluene. In the reaction of 1, chromatographic purification afforded a minor band, from which the two species RuCo(CO)4(μ-CO)[μ-PPh2C(O)CHC(CO2Me)] and RuCo(CO)4(μ-CO)[μ-PPh2CHC(CO2Me)] were observed by 1H NMR spectroscopy, and one major band, whose 1H NMR spectrum revealed the presence of multiple species. The identity of one of the compounds in the major component has been established as that of CoRu(CO)4(μ-CO)[μ-PPh2C(O)CH(CCO2Me)C(O)CHC(CO2Me)] (3) by X-ray diffraction analysis. The solid-state structure of 3 confirms the double insertion of CO and head-to-head coupling of the methyl propiolate that accompanies the formation of this product. Compound 3 crystallizes in the triclinic space group P-1, a = 8.4035(4), b = 9.6721(5), c = 17.678(1) Å, α = 94.135(2), β = 103.318(2), γ = 101.336(2)°, V = 1360.5(1) Å3, Z = 2, D calc = 1.732 Mg/m3; R = 0.0300, R w = 0.0760 for 8630 reflections with I > 2σ(I). The ruthenium-bound diphosphine ligand in 2 exerts a controlling influence on the reaction with added alkyne insomuch as only the mono-insertion product CoRu(CO)3(μ-CO)[(Z)-Ph2PCH=CHPPh2][μ-PPh2C(O)C(CO2Me)CH] (4) is formed as a single regioisomer. The molecular structure of 4 was established by X-ray diffraction analysis and 4 was found to crystallize in the monoclinic space group P21/c, a = 19.483(7), b = 11.905(4), c = 20.131(7) Å, β = 110.455(6)°, V = 4375(3) Å3, Z = 4, D calc = 1.466 Mg/m3; R = 0.0961, R w = 0.1683 for 6262 reflections with I > 2σ(I). The reactivity of methyl propiolate with 1 and 2 is compared with the known reactivity that has been reported for other alkynes. 相似文献
10.
Abstract
The 2-((E)-3-(2-nitrophenyl)-1-(4-methoxyphenyl)allylidene)malononitrile and 2-((E)-3-(2-chlorophenyl)-1-(4-bromophenyl)allylidene)malononitrile were synthesized and characterized by IR, 1H NMR, and elemental analysis. The molecular structures were further confirmed by X-ray diffraction analysis. The former 1, C19H13N3O3, is triclinic, space group P−1, a = 7.3834(13), b = 10.901(3), c = 11.227(2) ?, α = 88.64(2), β = 71.596(14), γ = 78.186(18), Z = 2, V = 838.5(3) ?3. The unclassical hydrogen bond of C–H⋯N links the molecules forming polymers. The latter 2, C36H20Br2Cl2N4, is orthorhombic, space group Pnma, a = 20.900 (4), b = 7.0710 (11), c = 10.9170 (18) ?, Z = 2, V = 1613.4(5) ?3. The same hydrogen bond of C–H⋯N and another type of C–H⋯Cl hydrogen bond link the adjacent molecules forming polymers along a axis. 相似文献11.
Three new cyclohexaphosphates with general formula M0.5((C6H5CH2)2NH2)5P6O18·H2O (M=Co, Cu, Cd) are reported. They crystallize with monoclinic unit-cells and are isotropic. We have determined their structure from the salt M=Co. This later exhibits the following unit-cell parameters: a = 22.739(5), b = 17.682(3), c = 18.342(3) Å, = 91.22(1)°, Z = 4,P21/n, V = 7373 Å3, and Dx = 1.373 g cm–3. The atomic arrangement can be described as layers containing P6O18 ring anions and CoO6 octahedra spreading in the (101) planes and intercalated by the dibenzylammonium groups and the water molecules. Synthesis and characterization by X-ray diffraction, IR absorption, and TA are described. 相似文献
12.
L. B. Serezhkina E. V. Peresypkina A. V. Virovets N. A. Neklyudova D. V. Pushkin 《Crystallography Reports》2008,53(4):651-654
Synthesis and X-ray diffraction study of {NH2C(NHC6H5)2}3[UO2(C2O4)2(NCS)] · 1.25H2O single crystals have been performed. This compound is crystallized in the orthorhombic system, with the unit-cell parameters a = 45.2646(8) Å, b = 57.7359(11) Å, c = 7.9244(3) Å, sp. gr. Fdd2, Z = 16, V = 20 709.6(10) Å3, and R = 0.0477. The uranium-containing structural units of the crystals are one-core groups of the [UO2(C2O4)2(NCS)]3? composition, belonging to the crystallochemical group AB 2 01 M 1 (A = UO 2 +2 , B 01 = C2O 4 2? , M 1 = NCS?) of uranyl complexes. The uranium-containing complexes are connected into a three-dimensional framework owing to the electrostatic interactions with the outer-sphere cations and a system of hydrogen bonds. 相似文献
13.
In aqueous solution, [M(chelate)Cl2]x (chelate = 2,2-bipyridine, 1,10-phenanthroline) complexes can disproportionate to produce M(chelate)2
n+ species that contain two chelating ligands. After extraction with organic solvent,Co(phen)2(-Cl)2CoCl2(1) has been characterized by X-ray diffraction (monoclinic, C2/c, a = 10.278(2)Å, b = 22.026(5)Å, c = 12.941(3)Å, = 103.959(4)°, Z = 4, 2414 reflections [I 2 (I)], R
1 = 0.0321, wR
2 = 0.0864). However, addition of [M(chelate)Cl2]x starting materials to dimethyl sulfoxide produces complexes that retain a single chelate ligand. The pentacoordinate complex Co(bpy)Cl2DMSO (2) has been structurally characterized (triclinic, P
, a = 7.824(2)Å, b = 9.570(4)Å, c = 10.025(2)Å, = 83.24(3)°, = 87.14(2)°, = 83.35(3)°, Z = 2, 2455 reflections [I 2 (I)], R
1 = 0.0278, wR
2 = 0.0747). In the case of nickel, two different geometric isomers are observed, depending on the chelate identity: trans-(DMSO)2Ni(bpy)Cl2 DMSO (3) (monoclinic, P21/c, a = 10.9149(8)Å, b = 12.1287(9)Å, c = 17.0044(13)Å, = 98.610(1)°, Z = 4,3519 reflections [I 2 (I)], R
1 = 0.0209, wR
2 = 0.0560) and cis-(DMSO)2Ni(phen)Cl2 (4) (monoclinic, P21/c, a = 8.404(2)Å, b = 14.051(4)Å, c = 16.710(4)Å, = 92.44(3)°, Z = 4, 3069 reflections [I 2 (I)], R
1 = 0.0691, wR
2 = 0.1782). 相似文献
14.
L. B. Serezhkina E. V. Peresypkina A. V. Virovets Ya. A. Medvedkov V. N. Serezhkin 《Crystallography Reports》2014,59(1):48-52
Malonate-thiocyanate complex (NH4)3[UO2(C3H2O4)2(NCS)] · 2H2O is synthesized and studied by X-ray diffraction. The compound crystallizes in the monoclinic system: a = 13.9983(4) Å, b = 8.1947(2) Å, c = 16.4678(4) Å, β = 100.846(1)°, space group Cc, Z = 4, and R = 0.0158. The main structural units of the crystal are mononuclear [UO2(C3H2O4)2(NCS)]3? groups belonging to the AB 2 01 M 1 crystal chemical group of uranyl complexes (A = UO 2 2+ , B 01 = C3H2O 4 2? , M 1 = NCS?). Discrete uranium-containing groups are connected by electrostatic interactions with ammonium ions and by hydrogen bonds. Some specific structural features of crystals containing [UO2(L)2(NCS)]3? complexes, where L is the oxalate or malonate ion, are discussed. 相似文献
15.
Yue-Qing Zheng Jian-Li Lin Zu-Ping Kong Bao-Ya Chen 《Journal of chemical crystallography》2002,32(10):399-408
The complex [Ni(H2O)3(phen)(C4H2O4)] H2O (1), which was obtained by reaction of phenanthroline, Ni(NO3)2 6H2O, and maleic acid in CH3OH/H2O at pH = 7.05, crystallized in the monoclinic space group P21 (no. 4) with cell dimensions: a = 9.350(1) Å, b = 7.631(1) Å, c = 12.821(1) Å, = 106.25(1), and D
calc = 1.607 g/cm3 for Z = 2. The Ni atoms are each octahe drally coordinated by one chelating phen ligand, three H2O molecules and one monodentate maleato ligand to form [Ni(H2O)3(phen)(C4H2O4)] complex molecules with d(Ni–O) = 2.038–2.090 Å, d(Ni–N) = 2.066, 2.089 Å. The formed complex molecules are, via the intermolecular hydrogen bonds, assembled into columnar 1D chains. Interdigitation of the chelating phen ligands of the neighboring chains leads to 2D layers and the crystal H2O molecules are hydrogen bonded to the oxygen atoms of the maleate not coordinated to the Ni atom. However, reaction of NiCO3, phen, and maleic acid in CH3OH/H2O at pH = 6.33 afforded [Ni(H2O)2(phen)(C4H2O4)] 2H2O (2), which crystallized in the triclinic space group
(no. 2) with cell dimensions: a = 7.971(1) Å, b = 8.237(1) Å, c = 13.304(1) Å, = 81.005(6)°, = 87.877(8)°, = 78.322(8)°, and D
calc = 1.671 g/cm3 for Z = 2. The Ni atoms are each octahedrally coordinated by two N atoms of one phen ligand and four O atoms of two H2O molecules and two bis–monodentate maleato ligands with d(Ni–O) = 2.041–2.120 Å and d(Ni–N) = 2.095 Å. The Ni atoms are bridged by the maleato ligands to generate 1D
1
[Ni(H2O)2(phen)(C4H2O4)2/2] chains along [100]. The supramolecular assemblies of the 1D chains via – stacking inter- actions result in thick 2D layers parallel to (001), between which the noncoordinating H2O molecules are sandwiched. The paramagnetic [Ni(H2O)2(phen)(C4H2O4)2/2] 2H2O (2) obeys the Curie–Weiss law m(T-) = 1.139cm3 mol–1 K with the Weiss constant = –0.95 K. 相似文献
16.
The crystal structure of a cadmium complex of trimethoprim ([CdBr2(TMP)2(H2O)2] · H2O, TMP = trimethoprim) has been determined from X-ray diffraction data using MoK radiation. The crystals are monoclinic, C2/c, with a = 7.7811(11), b = 15.439(3) c = 29.645(6)Å, = 97.23(2)° and Z = 4. Trimethoprim (2,3-diamino(3,4,5trimethoxybenzyl)pyrimidine) acts as a monodentate ligand. Cadmium is coordinated to N(1) atoms of two trimethoprim moieties. The octahetral coordination geometry around cadmium is completed by two Br-ions and two water molecules. The complex has a two-fold axis coinciding with a crystallographic two-fold axis. There is an interligand hydrogen bond between the bromide ion and the 2-amino group of the pyrimidine. 相似文献
17.
A water soluble flavonoid sulfate, [Ni(H2O)6](C19H17O9S)2·2H2O was synthesized and its structure was determined by single-crystal X-ray diffraction analysis. The crystal of it belongs to triclinic crystal system, space group P–1. The results show that the title compound consists of [Ni(H2O)6]2+, C19H17O6SO3
− and H2O. Ni(II) is located on the symmetry center and octahedrally coordinated by six water molecules. A variety of hydrogen bonds among [Ni(H2O)6]2+, C19H17O6SO3
− and the lattice water molecules build a hydrophilic region. Aromatic π–π stacking interactions assemble isoflavone skeletons into a column and the columns form a hydrophobic region of the title compound. The sulfo-groups bridge the hydrophilic regions and the hydrophobic regions as well as the inorganic components and organic components. Hydrogen bonds, stacking interactions and the electrostatic interactions between cation [Ni(H2O)6]2+ and anion sulfonate C19H17O6SO3
− lead the moieties to a three-dimensional structure. 相似文献
18.
Graciela Díaz de Delgado Pedro P. Parra Alexander Briceño José Miguel Delgado 《Journal of chemical crystallography》1995,25(5):241-244
[Sr(C4H2O4)(OH2)3]·H2O is monoclinic, P21/n, witha=11.476(2),b=7.027(1),c=12.344(2) Å, =115.74(3)°,V=896.67 Å3,Z=4. The Sr atom is surrounded by nine oxygen atoms which come from four different maleate anions and three water molecules. The Sr–O distances range from 2.546(2) to 2.808(2) Å. The C–O distances are equal within the standard deviation 1.263(3) to 1.258(3) Å). In the maleate anion, the planes that contain the carboxylate groups form an angle of 74.44(9)°. Both carboxylate groups deviate significantly from planarity. The different coordination modes of the carboxylate group and the extensive hydrogen bonding present are responsible for the polymeric nature of the structure. 相似文献
19.
The crystal and molecular structures of the complex of [Ni{(iPrO)2dtp}2(py)2] and [Cd{(iPrO)2dtp}2(py)2] (dtp = dithiophosphate, py = pyridine) have been determined by X-ray crystallography. They are isomorphous. The crystal structures are very similar and consist of discrete molecules of [Ni{(iPrO)2dtp}2(py)2] and [Cd{(iPrO)2dtp}2(py)2], respectively. They both crystallize in the monoclinic system, space group P21/c, the former with lattice parameters a = 6.489(1) Å, b = 14.830(3) Å, c = 16.386(3) Å, = 99.74(3), and Z = 2; the latter with a = 6.461(3) Å, b = 14.583(4) Å, c = 17.433(4) Å, = 99.55(3)°, and Z = 2. They all display distorted octahedral geometry around the central metal atom. In the complexes, two O,O-diisopropyl dithiophosphate ions act as bidentate ligands with their S atoms coordinated to metal. Each forms a four-membered chelate ring in the equatorial plane. The N atoms from two pyridine ligands are axially coordinated to the metal atom. The Ni–S bond distances are 2.5137(10) and 2.5386(9) Å, and the Ni–N bond distances are 2.127(3) Å. The Cd–S(1) and Cd–S(2) bond distance are 2.694(1) and 2.704(1) Å, respectively, and the Cd–N bond distances are 2.399(3) Å. The IR spectra data is in agreement with the structural data. 相似文献
20.
N. I. Sorokin 《Crystallography Reports》2012,57(6):808-810
The ionic conductivity of nonstoichiometric Bi12(V0.89Bi0.03)O20.27 single crystal with a sillenite-type structure has been investigated by impedance spectroscopy; its conductivity at 673 K is 2 × 10?3 S/cm, which is about two orders of magnitude higher than the conductivity of oxide superionic conductor single crystal Zr0.88Y0.12O1.94. As follows from crystallochemical analysis, ion transport in Bi12(V0.89Bi0.03)O20.27 is due to additional O2? ions, which arise due to oxygen nonstoichiometry. 相似文献