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1.
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2.
Peng-Cheng Lv Kai-Rui Wang Wen-Jun Mao Rui-Qin Fang Jin Chen Jing Xiong Hai-Liang Zhu 《Journal of chemical crystallography》2009,39(12):927-930
Abstract
A depside derivative, 2-(2-methoxy-2-oxoethyl)phenyl 2-(3,4-dimethoxyphenyl)acetate (3), was synthesized through a facile approach in high yields. Its structure was confirmed by 1H NMR, 13C NMR, ESI mass spectra, elemental analyses and X-ray single crystal diffraction study. Crystal structure analysis revealed that compound 3 crystallized in the monoclinic, space group P21/c with the following unit cell parameters: a = 10.173(2) Å, b = 10.459(2) Å, c = 16.516(3) Å, α = 90°, β = 102.30(3)°, γ = 90°, V = 1717.0(6) Å3, Z = 4. 相似文献3.
Naijue Zhu Danielle Lightsey Jiawang Liu Maryam Foroozesh Kathleen M. Morgan Edwin D. Stevens Cheryl L. Klein Stevens 《Journal of chemical crystallography》2010,40(4):343-352
Abstract
The single-crystal X-ray structures and in vivo activities of three aryl acetylenic inhibitors of cytochromes P450 1A1, 1A2, 2A6, and 2B1 have been determined and are reported herein. These are 1-ethynylpyrene, 1-propynylpyrene, and 4-propynylpyrene. To investigate electronic influences on the mechanism of enzyme inhibition, the experimental electron density distribution of 1-ethynylpyrene has been determined using low-temperature X-ray diffraction measurements, and the resulting net atomic charges compared with various theoretical calculations. A total of 82,390 reflections were measured with Mo Kα radiation to a (sinθ/λ)max = 0.985 Å−1. Averaging symmetry equivalent reflections yielded 8,889 unique reflections. A least squares refinement procedure was used in which multipole parameters were added to describe the distortions of the atomic electron distributions from spherical symmetry. A map of the model electron density distribution of 1-ethynylpyrene was obtained. Net atomic charges calculated from refined monopole population parameters yielded charges that showed that the terminal acetylenic carbon atom (C18) is more negative than the internal carbon (C17). Net atomic charges calculated by ab initio, density functional theory, and semi-empirical methods are consistent with this trend suggesting that the terminal acetylenic carbon atom is more likely to be the site of oxidation. This is consistent with the inhibition mechanism pathway that results in the formation of a reactive ketene intermediate. This is also consistent with assay results that determined that 1-ethynylpyrene acts as a mechanism-based inhibitor of P450s 1A1 and 1A2 and as a reversible inhibitor of P450 2B1. Crystallographic data: 1-ethynylpyrene, C18H10, P21/c, a = 14.571(2) Å, b = 3.9094(5) Å, c = 20.242(3) Å, β = 105.042(2)°, V = 1,113.5(2) Å3; 1-propynylpyrene, C19H12, P21/n, a = 8.970(2) Å, b = 10.136(1) Å, c = 14.080(3) Å, β = 99.77(2)°, V = 1,261.5(4) Å3; 4-propynylpyrene, C19H12, Pbca, a = 9.904(1) Å, b = 13.174(2) Å, c = 19.401(1) Å, V = 2,531.4(5) Å3. 相似文献4.
Wesley H. Monillas Glenn P. A. Yap Klaus H. Theopold 《Journal of chemical crystallography》2009,39(5):380-383
Abstract Addition of one equivalent of CrI2 to two equivalents of lithium cyclohexylamino-pent-2-en-4-onate results in bis[(cyclohexylamino)pent-2-en-4-onato]-chromium(II).
Crystallization in diethylether reaction solvent forms the hemi-etherate A with the asymmetric unit showing two target compounds and one molecule of cocrystallized diethylether in the P-1 space group with crystal cell parameters a = 12.931(4) Å, b = 13.207(4) Å, c = 16.104(5) Å, α = 66.559(5)°, β = 77.670(5)°, γ = 81.562(5)°, V = 2,459.1(14) Å3 and Z = 4. Drying A in vacuo and recrystallization in pentane yields a nonsolvated crystalline phase B with an asymmetric unit displaying only one molecule of the target compound in the P21/c space group with crystal cell parameters a = 14.290(7) Å, b = 14.082(7) Å, c = 11.246(6) Å, β = 94.807(8)°, V = 2,255.1(19) Å3 and Z = 4.
Graphical Abstract A Cr(II) complex supported by two β-enaminoketiminato ligands, bis[(cyclohexylamino)pent-2-en-4-onato]-chromium(II), has been
synthesized and has been structurally characterized in two different crystal phases.
相似文献
5.
Abstract
Two phosphate salts (2-aminopyrimidine): (phosphoric acid): H2O [HL1+ (H2PO4) − ]·H2O (1), and (4-phenylthiazol-2-amine): (phosphoric acid) [HL2+·(H2PO4)−] (2) based on 2-aminoheterocyclic compounds, 2-aminopyrimidine (L1), and 4-phenylthiazol-2-amine (L2) were prepared and structurally characterized by X-ray crystallography. Compound 1 crystallizes in the triclinic, space group P-1, with a = 6.2201(7) Å, b = 8.6139(9) Å, c = 9.4800(10) Å, α = 109.685(2)°, β = 106.3340(10)°, γ = 95.4450(10)°, V = 448.72(8) Å3, Z = 2. For 1, the cations were linked to each other via intermolecular C–H···N hydrogen bonds to form a 1-D chain structure running along the a-axis direction. The anions and the water molecules were connected alternatively along the a-axis direction through O–H···O hydrogen bonds to form a 1-D chain also. The cationic chains and the anionic chains were alternatively connected along the c-axis direction through N–H···O and C–H···O hydrogen bonds to form a 2D corrugated sheet. Adjacent sheets were combined together through π–π interaction to form double sheet. These double sheets were further joined together by O–H···O and N–H···O hydrogen bonds to produce a 3D network structure. Compound 2 crystallizes in the Orthorhombic, space group Pbca, with a = 10.1929(10) Å, b = 8.4406(9) Å, c = 27.589(2) Å, α = 90°, β = 90°, γ = 90°, V = 2373.6(4) Å3, Z = 8. In 2, the phosphates formed 1D chain along the b-axis through two P–O–H···O = P hydrogen bonds. The cations formed 1D zigzag chain along the b-axis direction under the CH–π interaction. The anionic chains were intercalated between two adjacent cationic chains through N–H···O, O–H···O, C–H···O, and O–S contacts. Such stacking repeated along the c-axis direction to form a 3D network structure. 相似文献6.
Abstract
A new acetyl phosphorylamidate P(O)[NHC(O)C6H4(4-NO2)][N(CH(CH3)2)(CH2C6H5)]2 has been synthesized and characterized by elemental analysis, 1H, 13C and 31P NMR, IR and single crystal X-ray diffraction. Single crystal X-ray analysis shows that it belongs to triclinic system, space group P[`1] P\bar{1} , with a = 10.5868(16) Å, b = 11.8058(18) Å, c = 12.4364(19) Å, α = 65.410(3)°, β = 67.492(4)°, γ = 85.879(3)°, V = 1,298.6(3) Å3, and Z = 2. The intermolecular PO···HN hydrogen bond makes H-bonded dimer of molecule with Ci symmetry. In the crystal network, the dimers are aggregated in the chain arrays through π-stacking between p-NO2–C6H4–C(O)–NH– moieties. Moreover, weak C–H···O and C–H···π interactions exist in the crystal network. 相似文献7.
Aliakbar Dehno Khalaji Karla Fejfarova Michal Dusek 《Journal of chemical crystallography》2012,42(3):263-266
Abstract
New Schiff base compound bis[(2,3,4-trimethoxy-benzylidenepropylideneamino)phenyl]-ether (1) was synthesized and characterized by elemental analyses (CHN), FT-IR and 1H-NMR spectroscopy and single-crystal X-ray diffraction. The title compound 1 crystallizes in triclinic system, space group P-1, with a = 6.8255(4) Å, b = 10.4346(4) Å, c = 19.4166(8) Å, α = 86.588(3)°, β = 85.019(4)°, γ = 89.042(4)°, V = 1375.12(11) Å3 and Z = 2. It displays a trans configuration about the C=N double bonds. 相似文献8.
Xiao-liu Li Xiao-li Zhen Jian-rong Han Shouxin Liu 《Journal of chemical crystallography》2009,39(12):870-873
Abstract
As precursors of α-amino acids, methyl 2-hydroxyimino-3-phenyl-propionate (F.W. 193.20) was synthesized, characterized by 1H NMR, IR, element analysis and confirmed by X-ray crystal structure analysis. This compound crystallizes in monoclinic class under the space group P21/c with cell parameters, a = 8.6435(17) Å, b = 5.4957(11) Å, c = 21.146(4) Å; β = 97.12(3)°, and Z = 4. The structure exhibits inter-molecular hydrogen bonds of the type O–H···N, O–H···O, C–H···O. 相似文献9.
Thapong Teerawatananond Narongsak Chaichit Nongnuj Muangsin 《Journal of chemical crystallography》2010,40(7):591-596
Abstract
A 1:1 co-crystal structure of 11-hydroxy-2,3,9-trimethoxy-6H-chromeno[3,4-b]chromen-12-one and 11-hydroxy-2,3,9-trimethoxy-chromeno[3,4-b]chromene-6,12-dione (stemonone) was crystallized from the reaction mixture of 6-deoxyclitoriacetal and methanesulfonyl chloride, and its structure was characterized by X-ray diffraction. This co-crystal crystallizes in a triclinic crystal system, space group P(−1) with unit cell parameters of a = 8.1317(3) Å, b = 9.8224(4) Å, c = 10.7268(3) Å, α = 78.116(1)°, β = 77.463(1)°, γ = 77.140(1)°, Z = 2 and V = 804.11(3) Å3. The crystal structure was solved by direct methods and refined by full-matrix least-squares on F 2 to final values of R 1 = 0.0501 and wR 2 = 0.1520. 相似文献10.
Max M. Abrahams Gregory W. Cushing Zachary N. Pickett William A. Howard Kraig A. Wheeler 《Journal of chemical crystallography》2010,40(7):583-590
Abstract
Mer-RhBr3(Me2pzH)3 (Me2pzH = 3,5-dimethylpyrazole) (monoclinic, P21/n, a = 8.3300 (5) Å, b = 16.2889 (9) Å, c = 15.9299 (11) Å, α = 90°, β = 100.217 (5)°, γ = 90°; V = 2,127.2 (2) Å3; Z = 4) has been characterized by X-ray diffraction, 1H and 13C nuclear magnetic resonance spectroscopy, infrared spectroscopy, and electronic absorption spectroscopy, and modeled by density functional theory (DFT) and time-dependent density functional theory (TDDFT). Mer-RhBr3(Me2pzH)3 is an octahedral complex with a HOMO → LUMO transition at 486 nm. The DFT and TDDFT calculations predicted mer-RhBr3(Me2pzH)3 to be an octahedral complex with a HOMO → LUMO transition at 540 nm. 相似文献11.
Abstract
Two lanthanide(III) coordination polymers, namely [Ce(pzdc)1.5(H2O)] n (1), [Er(pzdc)(μ2-OH)(H2O)] n ·nH2O (2) (H2pzdc = pyrazine-2,5-dicarboxylic acid), have been hydrothermally synthesized and characterized by single crystal X-ray diffraction and magnetic measurements. Polymer 1 crystallizes in triclinic space group P-1, with a = 6.2875(6), b = 6.7396(6), c = 13.3858(14) Å, α = 82.858(4), β = 83.118(4), γ = 63.452(4)°, V = 502.16(8) Å3, and Z = 2. Polymer 2 crystallizes in monoclinic space group P2(1)/c, with a = 11.706(4), b = 6.151(2), c = 14.063(5) Å, β = 92.255(3), V = 502.16(8) Å3, and Z = 4. Single-crystal X-ray diffraction studies show that compound 1 possess a 3D framework structure consisted of double chains. Compound 2 features a 3D open framework structure with a dinuclear Er(III) secondary building unit. Magnetic studies for complex 1 show stronger antiferromagnetic coupling between the Ce(III) ions. 相似文献12.
Crystal Structure of 4-Bromo-3,4-Dichloro-1-(1-Morpholinyl)-1-(Decylsulfanyl)-2-Nitro-Buta-1,3-Diene
Cemil Ibis Nahide Gulsah Deniz Amac Fatih Tuyun 《Journal of chemical crystallography》2010,40(4):353-356
Abstract
The compound 4-bromo-3,4-dichloro-1-(1-morpholinyl)-1-(decylsulfanyl)-2-nitro-buta-1,3-diene was synthesized from the reaction of 4-bromo-1,3,4-trichloro-1-(decylsulfanyl)-2-nitro-buta-1,3-diene with morpholine and characterized by elemental analysis, IR spectrum, UV spectra, 1H NMR,13C NMR and X-ray single crystal determination. In the title compound, C18H29BrCl2N2O3S, crystallizes in the monoclinic space group P21/c, a = 15.8326(4) Å, b = 8.9915(10) Å, c = 16.7528(5) Å, β = 100.808(10)°, V = 2,342.6(3) Å3, Z = 4, R 1 = 0.0590 and wR 2 = 0.0940. The morpholine ring adopts a chair conformation. The morpholine ring and the butadiene group are inclined at an angle of 113.4 (1)°. The butadiene unit is not planar as can be expected if the two double bonds are fully conjugated. 相似文献13.
Abstract
Using pyridine-2,5-dicarboxylic acid (2,5-pdcH2) and Gd2O3, a new three-dimensional (3D) polymeric complex, [Gd(2,5-pdc)(nic)·H2O] n (1) was synthesized under hydrothermal conditions, in which nic (nicotinate; also named as pyridine-2-carboxylic acid) might have been formed from the 2,5-pdc ligands through the C–C bond cleavage and release of CO2 molecules. The complex crystallizes in monoclinic system, space group P21/c with unit cell parameters a = 9.221(9) Å, b = 14.179(14) Å, c = 10.516(10) Å, β = 95.658(14)°, V = 1,368(2) Å3 and Z = 2. 2,5-pdc ligands bridge gadolinium centers to form the three-dimensional framework featuring hexagonal channels along the axis a which are occupied by bridging nic anions and mono-coordinated water molecules. Magnetic properties have been investigated in the range of 2–300 K reveal that t there is very weak antiferromagnetic exchange between the Gd(III) ions (J = −0.017 cm−1). 相似文献14.
Synthesis,Characterization and Crystal Structure Determination of a Hepta-coordinated Cadmium(II) Complex with Thiocyanato-bridges 总被引:1,自引:0,他引:1
Dongbin Dang Jide Sun Yan Bai Hui Gao Weili Shang 《Journal of chemical crystallography》2009,39(9):683-687
Abstract A new cadmium(II) complex [(C28H24N6)Cd(SCN)2]2(CH3OH)2 (1) has been synthesized and characterized by IR, UV spectra, TG-DTA technique and single crystal X-ray diffraction analysis.
The crystallographic data for compound 1: triclinic P1ˉ, a = 9.630(2) Å, b = 11.123(3) Å, c = 15.396(4) Å, α = 106.93(1)°, β = 91.60(1)°, γ = 99.99(1)°, V = 1,548.5(6) Å3, Z = 1, Dc = 1.512 mg/m3, F(000) = 716, R
1 = 0.0332, wR
2 = 0.0907. The molecule contains a symmetrical dinuclear unit in which two Cd(II) ions are double bridged by two di-μ-1,3-SCN− anoins with a cadmium–cadmium separation of 6.48 Å. Each Cd(II) ion is seven-coordinated with six nitrogen atoms and a sulfur
atom to form a monocapped trigonal prism coordination geometry. In addition, the molecule is further connected by multiform
intermolecular C–H···π, π···π interactions and hydrogen bonds to form a three-dimensional supramolecular structure.
Graphical Abstract A hepta-coordinated Cd(II) complex which exhibits a distorted a monocapped trigonal prism coordination geometry has been achieved
by using bisbidentate Schiff-base ligand and thiocyanate anion.
相似文献
15.
Frankline K. Keter Bernard Omondi James Darkwa 《Journal of chemical crystallography》2009,39(7):510-514
Abstract Two new palladium(II) complexes, dichloro-{bis(3,5-dimethylpyrazol-1-yl)acetic acid}palladium(II)PdCl2(3,5-Me2bpza)], (1) (3,5-Me2bpza = 3,5-dimethylpyrazol-1-yl)acetic acid) and dichloro-{bis(3,5-ditertbutylpyrazol-1-yl)acetic acid}palladium(II), [PdCl2(3,5-tBu2bpza)], (2a) [3,5-
t
Bu2bpza = 3,5-ditertiarybutylpyrazol-1-yl)acetic acid] complexes, were synthesized from the reactions of pyrazol-1-yl ligands
with palladium salts. Attempts to crystallize 2a led to a hydrolyzed product, dichloro-{3,5-ditertbutylpyrazol-1-yl}palladium(II) (2b), in which the acetic acid moiety in the ligand backbone of 1 is lost. Both complexes 1 and 2b have been characterized by single-crystal X-ray crystallography. Both complexes crystallized in triclinic system (P − 1 space group). The cell parameters are: complex 1 (a = 8.7960(14) Å, b = 16.238(2) Å, c = 16.430(2) Å, α = 78.038(10)°, β = 77.817(11)°, γ = 89.970(10)°) and complex 2b (a = 10.1492(2) Å, b = 12.4001(2) Å, c = 13.108(3) Å, α = 103.0690(10)°, β = 97.4120(10)°, γ = 107.2450(10)°). The asymmetric unit of 1 contains two crystallographic independent monomeric units of 1 and three molecules of DMSO solvent, whilst that of 2b has got one monomeric unit with one molecule of chloroform solvent.
Index Abstract Two palladium complexes, dichloro-{bis(3,5-dimethylpyrazol-1-yl)acetic acid}palladium(II), PdCl2(3,5-Me2bpza)], (1) (3,5-Me2bpza = 3,5-dimethylpyrazol-1-yl)acetic acid) and dichloro-{bis(3,5-ditertbutylpyrazol-1-yl)acetic acid}palladium(II), [PdCl2(3,5-
t
Bu2bpza)], (3,5-
t
Bu2bpza = 3,5-ditertiarybutylpyrazol-1-yl)acetic acid) complexes, were synthesized from the reactions of pyrazol-1-yl ligands
with palladium salts. Attempt to obtain crystals of tertiarybutylpyrazolyl analogue led to hydrolysis, the crystal structure
of the hydrolysis product was established by single crystal X-ray crystallography.
相似文献
16.
Louise G. Edwards Mark Lautens Alan J. Lough 《Journal of chemical crystallography》1997,27(8):471-474
The X-ray diffraction study confirms the Rc,Ss strereochemistry of the title compound. Molecules are linked by relatively close intermolecular contacts through 21 screw axes (C…O[1−x, 0.5+y, 0.5−z] 3.305 Å) to form weakly bonded chains along they-direction. The tetracylononane group is highly strained with Csp
3-Csp
3 bonds ranging from 1.482(5) to 1.535(5) Å. C16H18OS,I2,a=7.049(2),b=9.807(2),c=20.274 Å, β=96.15(2)°. 相似文献
17.
Abstract
The molecular structure of the complex bis-(2-pyridyl)amine(η2-styrene)silver(I) tetrafluoroborate has been determined. The geometry about the Ag+ ion is pseudo-trigonal planar, with coordination sites occupied by the two pyridyl nitrogen atoms and the midpoint of the alkene double bond. Crystal packing of the molecule is influenced by hydrogen bonding of the amine with the tetrafluoroborate anion, in addition to intermolecular Ag+···aromatic contacts. 1H NMR confirms crystallographic data that suggest weak metal to olefin π-backbonding. Crystal data: space group P21/n, a = 12.764(3), b = 10.590(2), c = 13.624(3) Å, β = 91.17(3)°, V = 1841.3(7) Å3, Z = 4, R = 0.0453, wR 2 = 0.1098. 相似文献18.
Wen-Xiang Chai Li Song Kang-Ying Shu Hong-Sheng Shi Lai-Shun Qin 《Journal of chemical crystallography》2010,40(5):448-452
Abstract
The reaction of isonicotinic acid (IN), sodium hydroxide, 1,10-phenanthroline (phen) and neodymium nitrate leads to the formation of a novel complex [Nd(phen)(IN)2(NO3)(H2O)2]2 1, which has been characterized by single crystal X-ray diffraction analysis: monoclinic, space group C2/c, with a = 24.93(2) Å, b = 9.452(3) Å, c = 21.406(5) Å, β = 97.87(2)°, and Z = 4. Complex 1 consists of a centrosymmetric dinclear molecule, and neodymium atoms are bridged by two carboxyl groups of two IN ligands. The dinuclear clusters of 1 are connected each other into a three-dimensional (3D) supramolecular framework, which is stabilized by O–H···O, O–H···N hydrogen bonds as well as π–π stacking interactions. Its electronic absorption and luminescence properties have also been investigated. 相似文献19.
Evgeny Yu. Bulatov Tatiana G. Chulkova Matti Haukka Vadim Yu. Kukushkin 《Journal of chemical crystallography》2012,42(4):352-355
Abstract
A 1:1 co-crystal of trans-[PtBr2(acetoxime)2] and 18-crown-6 has been obtained by a slow-evaporation of the equimolar mixture of trans-[PtBr2(acetoxime)2] and the crown ether. The compound crystallizes in the triclinic space group P [`1] P\,\bar{1} , with unit cell parameters a = 7.4765(2) Å, b = 9.5044(2) Å, c = 10.1591(3) Å, α = 83.687(1)°, β = 70.847(1)°, γ = 79.773(1)°, Z = 1. trans-[PtBr2(acetoxime)2] is assembled with 18-crown-6 into a 2D network structure by interactions between the oxygen atoms of 18-crown-6 and the hydroxylic and methyl hydrogen atoms of the oxime ligands. 相似文献20.
Liyan Na Ruinian Hua Liying Zhang Wei Zhang Guiling Ning 《Journal of chemical crystallography》2009,39(9):688-691
Abstract A three-dimensional lanthanide metal-organic coordination polymer Yb3(BDC)4.5(DMF)2(H2O)3 · (DMF)2 has been synthesized by the reaction of the lanthanide metal ion (Yb3+) with 1,4-benzenedicarboxylic acid (H2BDC) under mild condition. The compound crystallizes in the triclinic system, space group PI with unit cell parameters a = 10.7428(9) Å, b = 11.2786(9) Å, c = 26.172(2) Å, α = 85.060(2)°, β = 88.1060(10)°, γ = 62.3670(10)°, V = 2798.9 (4) Å3, Z = 2. The crystal structure exhibits one-dimensional channels along the [011] direction. The fluorescent results showed that
there were two emission peaks at 375 and 420 nm when the compound was excited by a 235 nm excitation.
Graphical Abstract The preparation, X-ray structure and luminescent property are presented for a new lanthanide metal-organic coordination polymer
Yb3(BDC)4.5(DMF)2(H2O)3 · (DMF)2.
相似文献