Synthesis Characterization and Crystal Structure of 2-(3,4,5-trimethoxyphenyl)-1-(4-fluorophenyl)-4,5-diphenyl-1H-imidazole

The title compound, C₃₀H₂₅FN₂O₃, was prepared from the four-component one-pot condensation reaction and the product crystallized using dimethylformamide. The structure of the compound was established by elemental analysis, Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), UV-Visible, and single-crystal X-ray diffraction. The compound crystallizes in the triclinic crystal system with the space group Pī, with unit cell parameters a = 10.286(2) Å, b = 11.795(2) Å, c = 21.331(4) Å, α = 100.270(3)°, β = 90.093(3)°, γ = 90.062(3)°, and Z = 4. The crystal and molecular structure of the title molecule is stabilized by intra-molecular interactions of types C–H···N and C–H···O.     

Synthesis,Crystal Structure,and Characterization of New 2,4,5-Triphenyl Imidazole: 4,5-Diphenyl-2-(3,4,5-trimethoxyphenyl)-1H-imidazole

The substituted triarylimidazole, C₂₄H₂₂N₂O₃, was prepared from the three-component one-pot condensation reaction and the product was crystallized by using dimethylformamide. The structure of the compound was confirmed by elemental analysis, FT-IR, thermogravimetric analysis (TGA), UV-Visible and single-crystal X-ray diffraction. The compound crystallizes in the monoclinic crystal system in the space group P2₁/c with unit cell parameters a = 10.509(3) Å, b = 18.748(5) Å, c = 22.016(6) Å, β = 90.844(5)°, and Z = 8. The crystal structure of the compound was stabilized by the inter-molecular interactions of types N–H???N, C–H???O, and C–H???N, and intra-molecular interactions of the type C–H???O. The structure also involves C–H???π interactions.     

Synthesis,Characterization, Crystal Structure,and Thermal Analysis of 4-[(3-acetylphenyl)amino]-2-methylidene-4-oxobutanoic Acid

4-[(3-Acetylphenyl)amino]-2-methylidene-4-oxobutanoic acid (1) is synthesized by a ring opening reaction of itaconic anhydride with 3-aminoacetophenone and characterized by FT-IR, ¹H NMR, UV-Vis, TGA, DTA, and single crystal X-ray diffraction. The crystal of 1 belongs to triclinic unit cell in the P-1 space group with the unit cell dimensions a = 4.9485(3), b = 5.3614(6), c = 22.457(2) Å, α = 88.295(8), β = 89.379(7), γ = 84.495(7), and Z = 2 The crystal structure is solved by direct methods using single-crystal X-ray diffraction data collected at room temperature and refined by full-matrix least-squares procedures to a final R-value of 0.0467 for 1623 observed reflections. Intermolecular N&;sbnd;H?…O and O&;sbnd;H?…O hydrogen bonds links the molecules into chains along [010] direction. In addition the thermal stability of the 1 is determined by using DTA, TGA analysis, and wavelength absorption at λ_max = 297 nm is determined by UV-Vis spectrophotometer.     

Crystal structure and spectroscopic characterization of bis(N-phenylthiourea)

Bis(N-phenylthiourea) (BPTU) has been synthesized and characterized by means of X-ray, IR, Raman, UV-Vis, ¹H NMR, and FAB mass spectra. The BPTU crystal belongs to the monoclinic C2/c space group with the cell constants a = 26.992(8) Å, b = 6.336(3) Å, c = 9.463(3) Å, = = 90°, = 105.97(7)°, Z = 4. The compound has been found to exist in the thione form, with cis configuration of the thiosemicarbazone moiety and skew conformation of the molecule.     

Crystal and molecular structure of triphenyl[2-(p-tolylthio)ethyl]tin

The crystal and molecular structure of Ph₃SnCH₂CH₂SC₆H₄Me-p has been determined by X-ray crystallography. In each of the two independent molecules in the asymmetric unit the tin atom has an irregular tetrahedral geometry, with C–Sn–C valency angles ranging from 104.1(5) to 114.7(5)° in molecule (1) and from 104.6 to 112.7(6)° in molecule (2). The bond lengths, C_alkyl–Sn are 2.18(1) and 2.17(2)Å (in molecules (1) and (2), respectively) while the C_aryl–Sn bond lengths range from 2.11(1) to 2.13(1)Å in molecule (1) and from 2.09(1) to 2.14(1)Å in molecule (2). The Sn–C–C–S torsion angle, 172(1)° is the same for both molecules. NMR spectral data are presented; the¹H NMR spectrum in solution of the central-CH₂–CH₂-unit suggests that each of the protons on each of the CH₂ groups is magnetically distinct and that rotations about the C–C bond are slow on the NMR time scale. Comparisons with similar molecules are made and conformations discussed in terms of steric effects.     

Synthesis,spectral, X-ray diffraction and DFT studies on 1-(2-methyl-2-propenyl)-3-(2,3,4,5,6-pentamethylbenzyl)benzimidazolium chloride hydrate

A new benzimidazole based N-heterocyclic carbene (NHC) salt (1) was synthesized by the reaction of benzimidazole precursor with alkyl halide. The structure of 1 was determined by elemental analysis, FT-IR, ¹H NMR and ¹³C NMR spectroscopy tecniques and X-ray crystallography. The compound crystallized in the triclinic space group P-1 with two molecules in the unit cell. The optimization of 1 was firstly performed at B3LYP/6-311G++(d,p) level, then the theoretical spectral studies performed and compared with the experimental values. Besides the frontier molecular orbital energies and chemical reactivity analysis of 1, together with the electrostatic potential and molecular electrostatic potential analyses were performed at the same level of theory.     

Synthesis,characterization, and crystal structure analysis of 2-(2-hydroxy-3-methoxyphenyl)-1-(4-chlorophenyl)-4,5-diphenyl-1h-imidazole

The substituted imidazole C₂₈H₂₁ClN₂O₂, was prepared via multicomponent reactions and the product crystallized using dimethylformamide. The structure of the compound was established by elemental analysis, Fourier transform infrared spectroscopy, thermogravimetric analysis, UV-visible, proton nuclear magnetic resonance spectroscopy, and single-crystal X-ray diffraction. The molecule is crystallized in the tetragonal crystal system with the space group P4₃2₁2 and with unit cell parameters a = 12.246(4) Å, b = 12.246(4) Å, c = 31.781(2) Å, and Z = 8. The molecular and crystal structures of the title molecule are stabilized by the intramolecular interactions, O-H···N and C-H···N, and intermolecular interaction, C-H···O.     

Synthesis,Characterization and Crystal Structure of the Bis(2,4-dinitrobenzoato)tetrabutyldistannoxane(IV) Dimer

Abstract The title compound, bis(2,4-dinitrobenzoato)tetrabutyldistannoxane(IV), was obtained from the reaction of di-n-butyltin(IV) oxide with 2,4-dinitrobenzoic acid. It crystallizes out as the usual dicarboxylatotetrabutyldistannoxane(IV) dimer. In the monoclinic system P2₁/c, a = 12.391(3) ?, b = 19.937(5) ?, c = 15.026(4) ?, α = γ = 90°, β = 102.857(2)°, V = 3618.95(16) ?³ and Z = 2. A crystal structure determination of the title compound reveals the presence of a centrosymmetric planar Sn₂O₂, with two different environments for tin atoms and two distinct carboxylate groups. Two of the carboxylate groups are bonded to the exocyclic tin atom in a bidentate bridging manner and the remaining two carboxylate groups are bonded to the tin atom in a monodentate manner. As a result, both the tin atoms moieties in the complex are five coordinate and exhibit trigonal bipyramid geometry. Index Abstract Synthesis, Characterization and Crystal Structure of the Bis(2,4-dinitrobenzoato)tetrabutyldistannoxane(IV) Dimer Yip Foo Win, Teoh Siang Guan, Lim Eng Khoon, Shea Lin Ng, Hoong Kun Fun A crystal structure determination of the title compound reveals the presence of a centrosymmetric planar Sn₂O₂, with two different environments for tin atoms and two distinct carboxylate groups.      

Synthesis,Characterization and Crystal Structure of a Polymeric Zinc(II) Complex Containing the Antimalarial Quinine as Ligand

Abstract A novel polymeric zinc(II) complex of quinine, [chlorosulphato (2-ethenyl)-4-azabicyclo[2.2.2]oct-5-ylium-(6-methoxyquinolin-4-yl) methanol zinc(II)] has been synthesized and characterized. Single-crystal X-ray diffraction analysis of the complex (C₂₀H₂₅ClN₂O₆SZn) revealed that quinine forms a zigzag coordination polymeric complex with Zn(II) of extended chains –ZnCl–O–SO₂–O–Zn–O–SO₂–O–ZnCl–. The crystals are monoclinic, space group C2 with a = 20.5035(5), b = 9.7943(2), c = 11.7814(4) ?, β = 96.578(2)°, Z = 4, V = 2350.3(1) ?³. The complex exhibits a tetrahedral geometry. Each Zn(II) centre is thus coordinated to an O atom from each of two sulphate bridges, a Cl atom and quinoline atom N(4) of the quinine moiety. The second quinuclidine nitrogen in the quinine is protonated. In the crystal, there is linkage of two polymeric chains related by a twofold rotation axis, resulting in a bilayer. The linking is achieved by hydrogen bonding from the quinine cation which provides two donors (–OH, N⁺–H), to oxygen atoms of sulphate groups which act as acceptors. Graphical Abstract The new polymeric zinc(II) complex of quinine, [chlorosulphato (2-ethenyl)-4-azabicyclo[2.2.2]oct-5-ylium-(6-methoxy quinolin-4-yl) methanol Zinc(II)] has been synthesized and structurally characterized The compound was characterized by IR spectroscopy, elemental analysis and X-ray diffraction. X-ray analysis showed that quinine forms a zigzag coordination polymeric complex with Zn(II) of extended chains –ZnCl–O–SO2–O–Zn–O–SO2–O–ZnCl–.      

Spectroscopic Studies and Crystal Structure of 3-[(2-morpholinoethylimino)methyl]benzene-1,2-diol

Abstract Schiff base 3-[(2-morpholinoethylimino)methyl]benzene-1,2-diol has been synthesized from the reaction of 4-(2-aminoethyl)morpholine with 2,3-dihydroxybenzaldehyde. The title compound has been characterized by elemental analysis, IR, ¹H-NMR, ¹³C-NMR and UV–visible techniques. The structure of the compound also has been examined crystallographically. For the compound exist as dominant form of enol-imines in both the solutions and solid state. The crystal structure has been solved by direct methods and refined by full-matrix least squares. The title compound crystallize in the monoclinic space group P2₁/n with a = 12.085(1), b = 8.256(1), c = 13.650(1) ?, β = 108.56(1)°, V = 1291.1(2) ?³, D _x = 1.288 g cm⁻³, respectively (R ₁ = 0.0336 and wR ₂ = 0.0922 for 2117 reflections [I > 2σ(I)]. Index abstract Intramolecular hydrogen bonding is important on the tautomeric properties and the type of aldehyde plays a vital role of the enol-imine and keto-amine properties of the Schiff base ligand.      

有机锡配合物{[nBu2Sn(OOCC5H3(NO2)2)]2O}2的合成、谱学表征和晶体结构

以3,5-二硝基苯甲酸和二丁基氧化锡为原料,合成了一种新的有机锡配合物{[~nBu_2Sn(OOCC_5H_3(NO_2)_2)]_2O}_2,并对其进行了元素分析、红外光谱表征和X射线单晶衍射.结果表明:该配合物属三斜晶系,P_ī空间群,a=1.0705(2) nm,b=1.3333(3) nm,c=1.4360(3) nm,α=68.892(3) °,β=78.297(3) °,γ=80.285(3) °, V=1.8620(7) nm~3 , Z=1, dc=1.613 g/cm~3 , μ=1.406 mm~(-1), F(000) =908, R_1=0.0408, wR_2=0.0948.该化合物分子是以Sn_2O_2四元环为中心,对称的二聚体结构,内外环锡原子均为五配位的畸变三角双锥构型.     

双核铜配合物[Cu(pht)2(ba)2]2的合成、晶体结构和抑菌活性

由过渡金属Cu(Ⅱ)、苯妥英(Hpht)与苄胺(ba)反应,得到一种新型双核铜配合物[Cu(pht)_2(ba)_2]_2,通过元素分析、摩尔电导、红外光谱、X-射线单晶衍射等对配合物的结构进行了解析和表征.结果表明:该晶体属三斜晶系,空间群为P_1~-,晶胞参数:a=1.0554(15) nm,b=1.201(17) nm,c=1.489(2) nm,α=93.24(2) °,β=102.14(2) °,γ=91.79(2) °,V=1.840(5) nm~3,F(000)=814,Z=1,Dc=1.408 g·cm~(-3),μ=0.648 mm~(-1),R_1=0.0973, wR_2=0.1929.配合物分子中每个Cu(II)离子以N4O1的五配位形式位于变形的三角双锥构型中.利用琼脂扩散法测试了该配合物的抑菌活性,结果表明对4种受试细菌均有一定的活性.     

吡嗪席夫碱银配位聚合物的晶体结构、发光性质和抗菌活性

利用2-乙酰基吡嗪和异烟肼在无水乙醇中反应得到席夫碱化合物N-[(1-吡嗪基)-1-亚甲基]异烟酰肼(L).以L和硝酸银为原料,通过扩散法合成了配位聚合物{[Ag3L2(NO3)2]CH3CN}n,并通过X-射线单晶衍射、元素分析、红外光谱、荧光光谱对其进行结构解析和性质表征.单晶衍射分析结果表明,该配位聚合物属单斜晶...     

Synthesis,Characterization and Crystal Structure of Iridium(III)bis(2-<Emphasis Type="Italic">p</Emphasis>-tolyl-benzothiazolato-N,C<Superscript>2</Superscript>)(acetylacetonate)

Abstract  A novel thiazole-based iridium (III) complex (iridium(III)bis(2-p-tolyl-benzothiazolato-N,C²)(acetylacetonate)) has been prepared and fully characterized by EA, IR, ¹H-NMR and MS. The molecular structure of the complex has been determined by single crystal X-ray diffraction analysis. The iridium (III) center adopts a distorted octahedral geometry with cis-O–O, cis-C–C, and trans-N–N chelate disposition. The complex crystallizes in the orthorhombic Pbca space group with cell parameters a = 10.1388(7) ?, b = 18.3565(12) ?, c = 31.021(2) ?, α = β = γ = 90 ° and Z = 8. The electronic absorption and emission spectra of this complex have been investigated. Index Abstract  A novel thiazole-based phosphorescent iridium (III) complex (iridium(III) bis (2-p-tolyl-benzothiazolato-N,C²)(acetylacetonate)) has been prepared and fully characterized by EA, IR, ¹H-NMR, MS and X-ray diffraction analysis.     

硼酸锶钡(Ba0.87Sr3.13B14O25)晶体的生长、结构和性质研究

本文报道了一种新的硼酸盐化合物-Ba0.87Sr3.13B14O25,采用泡生法已生长出尺寸为35mm×25mm×5mm的晶体.该晶体为单斜晶系,C2/m空间群,a=1.6425(3)nr,b=0.77739(16)nm,c=1.6665(3)nm,β=119.22(3)°,Z=4.结构中B3O8六元环通过O原子和BO3三角形相互连接,构成三维的硼氧阴离子骨架,金属阳离子占据多面体间的空隙.测量了BSBO晶体的透过谱,该晶体的显微硬度为578kg/mm2.     

5-溴-2-(4-甲基哌啶-1-基)嘧啶的晶体结构及密度泛函理论研究

嘧啶类衍生物在医药、化工和功能材料等领域有着重要应用。在药物研发,特别是抗癌药物研发领域中,5-溴-2-(4-甲基哌啶-1-基)嘧啶是一种含嘧啶环的重要中间体。本文通过一步芳香亲核取代反应合成了5-溴-2-(4-甲基哌啶-1-基)嘧啶,经溶液结晶法获得其单晶体,并进行了晶体学分析(晶系:正交晶系,空间群:P2₁2₁2₁,晶胞:a=10.181 42(6) nm, b=17.620 0(8) nm, c=10.179 02(5) nm,Z=4,ρ_c＝1.478 g·cm^-3,R=0.056 6,wR=0.168 8)。标题化合物的最优结构和前线轨道能量在B3LYP/6-311G(d, p)模式下使用密度泛函理论(DFT)计算得到,经DFT优化的结果与实验确定的数据相近。此外,为进一步揭示标题化合物的物理化学性质,通过DFT进一步研究了分子的静电式和前线分子轨道。     

新型配位聚合物[Co(pda)2(H2O)2]n的水热合成和晶体结构

以CoCl2·6H2O和3-(3-吡啶基)丙烯酸(pda)为原料,在中温水热反应条件下,合成了一种新型配位聚合物[Co(pda)2(H2O)2]n单晶体,并对其进行了元素分析、红外光谱表征、TGA-GTA分析和X射线单晶衍射测定.该配位聚合物属单斜晶系,P2(1)/c空间群,晶胞参数为a=1.6958(8)nm;b=0.5466(3)nm;c=1.8034(8)nm;α=90°;β=106.209(7)°;γ=90°;Mr=391.24;V=1.6051(13)nm3;Z=4;dc=1.619g/cm3;μ=1.106mm-1;F(000)=804;R1=0.0367;wR2=0.0711.该晶体通过配位键的连接形成二维结构,又通过分子间氢键和π-π相互作用形成三维的网状结构.     

Synthesis and crystal structure of 4,4′-bis(4-pyridylethyl)biphenyl, noncovalently hydrogen bonded two-dimensional networks

A new pyridine containing compound, 4,4-bis(4-pyridylethyl)biphenyl 1, was synthesized and its structure was determined by X-ray crystallography. Two kinds of two-dimensional networks linked by hydrogen bonds were obtained with different crystal solvents: 1·2H₂O, monoclinic, space group P2₁/n with a = 8.3280(10), b = 5.5990(10), c = 24.054(4) Å, = 98.79(2)°, V = 1108.4(3) ų, Z = 2, Dc = 1.200 g cm^–3, R1 = 0.0558; 1·CH₃OH·2H₂O, triclinic, space group P-1 with a = 8.3310(10), b = 12.861(2), c = 13.111(2) Å, = 64.110(10), = 75.000(10), = 83.750(10)°, V = 1220.7(3) ų, Z = 2, Dc = 1.177 g cm^–3, R1 = 0.0529. It is interesting that in the hydrate the host molecule of 1 contains an essentially flat biphenyl section, while in the methanol complex the host molecule of 1 contains a substantial twist in the center of the biphenyl section. The compounds were also characterized by NMR and FTIR spectroscopies. The ¹H and ¹³C NMR assignments for 1 were carried out by 2D NMR spectral measurements in acetonitrile-d ₃.     

无机-有机杂化晶体[C12H11N2O2][Cd(SCN)3]的合成和晶体结构

合成了无机-有机杂化晶体[C12H11N2O2][Cd(SCN)3],并采用元素分析、红外光谱表征和单晶X射线衍射分析和热重分析研究.红外光谱分析表明SCN-采用1,3-μ模式.结构分析表明,相邻的Cd(II)原子通过三个1,3-μ-SCN- 阴离子桥连形成无限的[Cd(SCN)-3]∞之字链结构,固体结构中[C12H11N2O2]+阳离子和[Cd(SCN)-3]∞配阴离子形成了分离柱状堆积.该晶体属于单斜晶系P2(1)/c空间群,晶胞参数分别为:a = 1.1260(3) nm, b = 1.5080(4) nm, c =1.1070(3) nm, β= 105.410(10) °, V = 1.8121(8) nm3, Z = 4, dc = 1.840 g·cm3 , T = 293(2) K, μ = 1.571 mm-1, F(000) = 992, R1 = 0.0343, wR2 = 0.0750 [I>2σ(I)]. 热分析结果在180-305 ℃化合物失去一个有机分子,305 ℃以上伴随着镉升华失去三个SCN-阴离子.     

Crystal Structures of (2-oxo-2H-Quinaxalin-1-yl)-acetic Acid and its Cobalt and Nickel Complexes and Their Comparison with (1,3-Dioxo-1,3-dihydro-isoindol-2-yl)-acetic Acid

Abstract The crystal structures of (2-oxo-2H-quinaxalin-1-yl)-acetic acid and its cobalt and nickel complexes are determined. The (2-oxo-2H-quinaxalin-1-yl)-acetic acid (1) crystallizes in orthorhombic, Pbca, a = 12.8571(11) ?, b = 9.4267(8) ?, c = 15.0095(13) ?, the cobalt complex of (2-oxo-2H-quinaxalin-1-yl)-acetic acid (2) crystallizes as dihydrate in triclinic, P-1 space group with a = 4.81150(10) ?, b = 11.8631(2) ?, c = 12.4867(3) ?, α = 71.7800(10)°, β = 79.2490(10)°, γ = 84.9020(10)° whereas the nickel complex of (2-oxo-2H-quinaxalin-1-yl)-acetic acid (3) crystallizes in monoclinic, P2₁/c space group with a = 14.9210(5) ?, b = 4.81730(10) ?, c = 15.7672(5) ?. and β = 99.823(2)°. The crystal structure of the ligand and the complexes are compared with structures of (1,3-dioxo-1,3-dihydro-isoindol-2-yl)-acetic acid and its cobalt and nickel complexes. Index Abstract The crystal structures of (2-oxo-2H-quinaxalin-1-yl)-acetic acid and its nickel and cobalt complexes are compared with (1,3-dioxo-1,3-dihydro-isoindol-2-yl)-acetic acid and its corresponding complexes with nickel(II) and cobalt(II).