Synthesis and Crystal Structure of a Complex of Palladium(II) with 2-Hydroxyimino-3-(2-hydrazonopyridyl)-butane

Abstract  

Schiff-base condensation of an equimolar proportion of diacetyl-monoxime and 2-hydrazino pyridine in methanol gives rise to 2-hydroxyimino-3-(2-hydrazonopyridyl)-butane (HL). The ligand has been characterised by FT-IR, ¹H NMR and UV–Vis spectra. Reaction of 1:1 stoichiometric proportion of HL with Na₂[PdCl₄] in methanol affords a mononuclear palladium(II) compound, [PdLCl]·H₂O (1). The compound is characterised by C, H and N analyses, FT-IR, conductivity measurement, UV–Vis spectra, thermal analysis and magnetic susceptibility measurement. The X-ray crystal structure of the title compound (1) has been determined. The compound crystalises in the triclinic space group P[`1] Poverline{1} with a = 7.3033(3), b = 9.4139(4), c = 9.4445(5) ?, α = 79.789(3), β = 68.285(2), γ = 77.978(3)o, V = 586.42(5) ?³ and Z = 2. Pd(II) is in ‘N₃Cl’ coordination chromophore. The geometry around Pd(II) is square-planar. The compound is essentially diamagnetic.     

Synthesis and Crystal Structure Analysis of Acridine Derivatives

Crystallography Reports - The title compounds were synthesised by the reaction of substituted benzaldehyde with dimedone in presence of liquid ammonia in a water–ethanol system. The yields of...     

Synthesis and Crystal Structure Analysis of Thiourea-Pendant Pyridines

Abstract  The crystal structures of pyridine containing thiourea moieties as substituents, (1) and (2), have been determined. The ortho-substituted pyridine (1) crystallized in monoclinic space group P2₁/c with a = 16.091(3) ?, b = 11.368(2) ?, c = 7.4364(14) ?, β = 100.489(4)o, V = 1337.5(4) ?³, z = 4. In this structure an intramolecular N–H···N hydrogen bond forms a pseudo-seven-membered ring. The meta-substituted pyridine (2) crystallized in monoclinic space group P2₁/c with a = 14.5408(15) ?, b = 8.8508(9) ?, c = 10.7959(11) ?, β = 106.435(2)o, V = 1332.6(2) ?³, z = 4. Crystal packing revealed that compounds (1) and (2) can form dimeric structures via intermolecular H-bonding using N–H···S and N–H···N interactions, respectively. Graphical Abstract  Varying the substituent position on the pyridine ring using thiourea moieties gave unique molecular aggregations in solid state structures.      

Microwave Synthesis and Crystal Structure of 2-Hydroxy-3-iodo-benzaldehyde-copper (II)

Abstract  

One new complex, 2-hydroxy-3-iodo-benzaldehyde-copper (II) has been designed and microwave synthesized. The structure was determined by UV, IR and single X-ray crystallography study. The title complex C₁₄H₈CuI₂O₄ crystallizes in the orthorhombic space group Pna2₁ with the cell parameters a = 12.7897(12) ?, b = 6.1132(8) ?, c = 19.5114(18) ?, V = 1525.5(3) ?³ and Z = 4. The central copper (II) is four-coordinated by four oxygen atoms from two 3-iodosalicylaldehyde. The complex is linked into rhombic crystals by weak intermolecular interactions.     

KCaZn2(BO3)2F的固相合成、晶体结构及表征

采用高温固相合成了一种新的类Sr2Be2B2O7族化合物KCaZn2(BO3)2F,利用粉末X射线衍射精修其晶体结构.该晶体同KCdZn2(BO3) 2F同构,为三方晶系,空间群为P31c,单胞参数为a=5.03096(5)A,c=15.3940(2)A,Z=2.晶体基本阴离子基元是平面三角形的BO3和四面体的ZnO3F基元,两个基元通过共顶的O原子相连,在ab平面形成二维的十二元环的(Zn3B3O6 F3)∞结构.(Zn3B3O6F3)∞结构通过F原子连接,形成(Zr6B6O12F3)∞双层单元,双层单元之内的两层BO3基元排列方式基本相反.(Zn6B6O12F3)∞双层单元与同它中心对称的另一个(Zn6B6O12F3)∞双层单元在c方向堆垛成三维的结构,K+和Ca2+分别位于(Zn6B6O12F3)∞双层单元的层内和层间空隙处.紫外可见漫反射光谱表明该晶体在400～2500 nm范围具有高的透过率,晶体的紫外截止波长为235 nm.     

Synthesis and X-ray Crystal Structure Analysis of CU2(CH3CH2COO)4(OP)2

The complex of [CU(CH₃CHCOO)₂(OPph)]₂ has been synthesized and its X-ray crystal structure determined at room temperature, M = 975.96, tetragonal, space group: 14_1/a(#88), Dx = 1.39 g/ cm³, The final R is 0.067 for 2087 independent observed reflections with 1 > 3α(I). The molecule has an inversion center on the middle of the Cu Cu axis. The bond-length of the Cu Cu is 2.61/(2) Å. The coordinate polyhedron of Cu corresponds to a tetragonal bipyramid. The angle of Cu O P is significantly smaller than that of its adducts [Cu(O₂CR)₂L]₂.     

Synthesis and Crystal Structure Analysis of Substituted Diethyl Malonate

Abstract  

As intermediates of light stabilizer malonate, diethyl 3,5-di-t-butyl-4-hydroxybenzyl phenyl malonates (F.W. 454.58) was synthesized, characterized by ¹H NMR, 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 = 9.8218(4) ?, b = 13.5571(5) ?, c = 19.7233(8) ?; β = 102.3530(10)°, and Z = 4. The structure exhibits inter-molecular hydrogen bonds of the type O–H–O, leading to the formation of one dimensional chains.     

Crystal and Molecular Structure Analysis of 2-Methylimidazole

Abstract  

The crystal structure of the title compound, C₄H₆N₂, has been determined using X-ray diffraction at 100 K. The crystal of 2-methylimidazole is in orthorhombic crystal system with space group P2₁2₁2₁ (Z = 4), lattice parameters: a = 5.9957(12) ?, b = 8.1574(16) ? and c = 9.7010(19) ?, V = 474.47(16) ?. The molecule of 2-methylimidazole is approximately planar. The maximum deviation from the least-squares imidazole plane, calculated for all non-H atoms is 0.006(2) ?. N–H···N hydrogen bonds link the molecules together, forming infinite chains of hydrogen bond pattern C(4) defined by the graph-set analysis. Two chains, which are almost antiparallel to each other, pass through each unit cell. The dihedral angle between the mean planes of molecules forming these intersecting chains is 76.90(4)°. No evidence was found for disorder of the hydrogen-bonding proton between the atoms N1 and N3. The significance of this study lies in the analysis of the interactions occurring via hydrogen bonds in this structure, as well as, in the comparison drawn between the molecular structure of 2-methylimidazole and those of several of other imidazole derivatives possessing a hydrogen atom in the N1 position.     

Synthesis and Crystal Structure of Heptyl 3-(3,4-dihydroxyphenyl)-2-propenoate

Abstract  The title compound, C₁₆H₂₂O₄, synthesized by modified Knoevenagel condensation of protocatechualdehyde with monoheptyl-malonate and recrystallized from benzene, was confirmed by single-crystal X-ray diffraction (CCDC 272827). The compound crystallizes in triclinic space group Pī with cell parameters a = 5.296(3) ?, b = 10.711(13) ?, c = 13.870(4) ?, α = 98.84(7)°, β = 90.97(4)°, γ = 96.77(7)° and Z = 2. The structure is the E isomer and its packing is stabilized by intermolecular O–H···O and C–H···O hydrogen bonds. Index Abstract  The title compound, C₁₆H₂₂O₄, synthesized by modified Knoevenagel condensation, was confirmed by single-crystal X-ray diffraction showing its structure is in E isomer and its packing is stabilized by hydrogen bonds.      

Synthesis and Crystal Structure of 3-[(Naphthalen-2-yl)methyl]Isocoumarin

Abstract 3-[(Naphthalen-2-yl) methyl]isocoumarin was synthesized by the reaction of homophthalic acid with 2-(naphthalen-2-yl)acetyl chloride at elevated temperature and its crystal structure has been determined (C₂₀H₁₄O₂), Mr = 286.31, a = 13.704(3), b = 7.356(4), c = 7.042(7) ?, β = 99.21(3)°, space group Pc, Z = 2, and V = 700.7(8) ?³. The isocoumarin and the naphthalene ring systems are individually planar and the dihedral angle between the mean planes of these two ring systems is 70.05(8)°. Graphical Abstract Synthesis and crystal structure of 3-[(Naphthalen-2-yl)methyl]isocoumarin Aamer Saeed, Junmei Liang, Masood Parvez The synthesis and crystal structure of a novel isocoumarin, 3-[(naphthalen-2-yl)methyl]isocoumarin has been presented.      

含异主族金属硫属化合物(1,2-dap)2InAsSeS3的溶剂热合成及晶体结构

采用溶剂热合成法合成含有异主族金属的硫属化合物(1,2-dap)2InAsSeS3(1,2-dap:1,2-丙二胺),且该化合物同时含有两种硫族元素.本文对该化合物进行单晶X-射线衍射分析、粉末X射线衍射(XRD)、红外光谱分析(IR)、差热-热重(TG-DSC)分析等表征.单晶X-射线衍射分析表明该化合物属于四方晶系,空间群为P42bc,a=1.41178(12)nm,b=1.41178(12)nm,c=1.6220(4)nm,Z=8.标题化合物为零维簇状结构,是由AsS2(S/Se)2四面体与InS(S/Se)N4八面体通过共边连接形成.     

Synthesis and Novel Crystal Structure Analysis of Anthracene-Based Chalcone Derivatives

Abstract

Four novel anthracene-based chalcone derivatives, (E)-1-(anthracen-9-yl)-3-(4-nitrophenyl)prop-2-en-1-one 1, (E)-1-(anthracen-9-yl)-3-(3-chlorophenyl)prop-2-en-1-one 2, (E)-1-(anthracen-9-yl)-3-(3,4,5-trimethoxyphenyl)prop-2-en-1-one 3, and (E)-1-(anthracen-9-yl)-3-(pyridin-4-yl)prop-2-en-1-one four were synthesized and their structures were solved by single crystal X-ray diffraction methods. The anthracenyl chalcone 1 crystallizes in the centrosymmetric monoclinic P2₁/c space group. The crystal structure analysis shows that the molecules of one form two dimensional (2D) corrugated layer structure. The anthracenyl chalcone 2 crystallizes in the centrosymmetric triclinic P-1 space group and forms one dimensional (1D) tape like structure in the crystal. Compound 3 crystallizes in the centrosymmetric monoclinic P2₁/n space group. Anthracenyl chalcone 4 crystallizes in the centrosymmetric triclinic P-1 space group.     

The Crystal and Molecular Structure of 1α,2α-Methylene Gibberellin A3 Methyl Ester

The three-dimensional structure of the 1α,2α-methylene gibberellin A₃ methyl ester has been determined by single-crystal X-ray diffraction techniques. The crystals are monoclinic, space group P 2₁ with two molecules in the unit cell of dimensions a = 9.236, b = 7.109, c = 14.155 Å and β = 104.61º. The structure was refined to an R-value of 0.0983 for 1359 observed reflections.     

Synthesis and Crystal Structure of 3,5-Dichloro-6-morpholinopyridin-2-ol

Abstract  

A new compound having potential bioactivities 3,5-dichloro-6-morpholinopyridin-2-ol (1) was synthesized and characterized by single crystal X-diffraction. The crystal is monoclinic, space group P2₁/c with a = 10.3609 (6), b = 10.5711 (7), c = 10.3190 (5) ?, β = 108.9433 (15)°, V = 1068.99 (11) ?³, Z = 4, C₉H₁₀Cl₂N₂O₂, D _c  = 1.548 g/cm³, μ (MoKα) = 0.71075 ?, S = 1.01, F (000) = 512.00, R = 0.0397 and wR = 0.1364. In the unit cell, there are two independent molecules linked by intermolecular O–H···O (2.693(2) ?) hydrogen bonds forming onedimensional expanded structure.     

Synthesis and X-Ray Crystal Structure of 1- and 2-Cinnamoyaloxy Acetonaphthones

Abstract  

The synthesis of titled compounds were achieved in one step using hydroxyl naphthones and substituted cinnamic acids in the presence of a catalytic amount of phosphorus oxychloride. X-ray crystal studies were undertaken for three compounds and the results are presented. Compounds 1 (C₂₂H₁₅F₃O₃) and 3 (C₂₁H₁₅BrO₃) formed a monoclinic crystals while compound 2 (C₂₂H₁₅F₃O₃) formed a triclinic crystals. The observed space group of these compounds is P2₁/c and P[`1] \bar{1} respectively. The 2-substituted compounds showed identical space group and showed a perpendicular arrangements of each of the substituents to the plane of the naphthyl ring. On the contrary, the 1-substituted cinnamoyal compound showed an orthogonal arrangement to naphthyl ring but the acetyl group was almost planar relative to the naphthyl moiety. The characterization of the structures of the compounds was also accomplished using high-resolution NMR spectroscopic techniques.     

Synthesis and Crystal Structure of NdCaGaO4

The crystal structure of the NdCaGaO₄ compound was investigated by means of X-ray structure analysis (powder diffractometer HZG-4, CuK_α): structure type LaCuO₄, space group Cmca, a = 5.3700(2) Å, b = 12.1058(3) Å, c = 5.3937(2) Å, Z = 4, R_I = 0.126. The shortest interatomic distances are: Nd(Ca)—O — 2.240(14) Å; Ga—O — 1.913(2) Å, O—O — 2.6852(2) Å, Nd(Ca)—Nd(Ca) — 3.442(3) Å, Nd(Ca)—Ga — 3.154(4) Å, Ga—Ga — 3.8056(2) Å. Atoms have the following coordination numbers: Nd(Ca) — 8; Ga — 6; O1 — 14(6); O2 — 9(5).     

五核簇{Dy2Ni3}配合物的合成、晶体结构及磁学性质

利用2-[(2-羟基-3-甲氧基)苄亚甲基氨基]苯甲酸(H2L)作为配体,以Dy(NO3)3·6H2O和Ni(CH3COO)2·4H2O为金属盐,通过水热法,合成了一种新的异金属五核簇[Dy2Ni3(C15H11NO4)2(NO3)4(Ac)2(OH)2(CH3CN)4(CH3OH)2]配合物1.单晶X射线衍射结果表明,配合物1属于三斜晶系,P-1空间群,晶胞参数a=1.0978(6)nm,b=1.2057(7)nm,c=1.2144(7)nm,α=103.571(7)°,β=90.062(7)°,γ=103.439(8)°,V=1.5171(14)nm3,Z=1.通过元素分析等方法对配合物1进行结构表征,并对其进行磁性测试.直流磁化率(DC)研究结果表明,配合物1具有微弱的铁磁性质,而交流磁化率(AC)并没有出现依赖于外场频率变化极值的现象表明该配合物在零场下不具有较为明显的单分子磁行为.