Synthesis,growth, and characterization of a new NLO material 3-(2,3-dimethoxyphenyl)-1-(pyridin-2-yl)prop-2-en-1-one

3-(2,3-Dimethoxyphenyl)-1-(pyridin-2-yl)prop-2-en-1-one (DMPP) a potential second harmonic generating (SHG) has been synthesized and grown as a single crystal by the slow evaporation technique at ambient temperature. The structure determination of the grown crystal was done by single crystal X-ray diffraction study. DMPP crystallizes with orthorhombic system with cell parameters a = 20.3106(8) Å, b = 4.9574(2) Å, c = 13.4863(5) Å, α = 90°, β = 90°, γ = 90° and space group Pca2₁. The crystals were characterized by FT-IR, thermal analysis, UV–vis–NIR spectroscopy and SHG measurements. Various functional groups present in DMPP were ascertained by FTIR analysis. DMPP is thermally stable up to 80 °C and optically transparent in the visible region. The crystal exhibits SHG efficiency comparable to that of KDP.     

Synthesis and crystal structure of methyl 2-(2,4-dichloro-5-fluorobenzoyl)-3-(pyrimidin-2-ylamino)acrylate

Methyl 2-(2,4-dichloro-5-fluorobenzoyl)-3-(pyrimidin-2-ylamino)acrylate has been prepared. Its crystal structure is discussed. The compound crystallizes in the triclinic space group P-1 with a = 11.6259 (7) Å, b = 11.8789 (7) Å, c = 13.9206 (5) Å, α = 68.0250 (10)°, β = 77.5660 (10)°, γ = 62.4950 (10)°, V = 1579.18 (14) ų, Z = 4. There are two independent but chemically identical molecules in the asymmetric unit. The molecules are packed in the crystal structure by weak intermolecular C–H···O and C–H···F interactions.     

Two coordination polymers of manganese(II) isophthalate and their preparation,structures, and magnetic properties

Two manganese coordination polymers, [Mn₂(ip)₂(dmf)]·dmf (1) and [Mn₄(ip)₄(dmf)₆]·2dmf (2) (ip=isophthalate; dmf=N,N-dimethylformamide), have been synthesized and characterized. X-ray crystal structural data reveal that compound 1 crystallizes in triclinic space group P?1, a=9.716(3) Å, b=12.193(3) Å, c=12.576(3) Å, α=62.19(2)°, β=66.423(17)°, γ=72.72(2)°, Z=2, while compound 2 crystallizes in monoclinic space group Cc, a=19.80(3) Å, b=20.20(2) Å, c=18.01(3) Å, β=108.40(4)°, Z=4. Variable-temperature magnetic susceptibilities of compounds 1 and 2 exhibit overall weak antiferromagnetic coupling between the adjacent Mn(II) ions.     

Growth, structure, and characterization of tris(thiourea)silver(I) nitrate

Single crystals of tris(thiourea)silver(I) nitrate have been grown by slow evaporation solution growth technique from an aqueous solution at 25 °C. The single crystal X-ray diffraction study reveals that the crystal belongs to tetragonal system and cell parameters are a = b = 14.2790(4) Å, c = 24.8900(7) Å, and V = 5074.8(2) Å³. The various functional groups present in the molecule are confirmed by Fourier transformed infrared spectroscopy (FT-IR). The structure and the crystallinity of the materials were further confirmed by powder X-ray diffraction analysis. Thermogravimetric and differential thermal analysis reveal the purity of the sample and no decomposition is observed up to the melting point. The crystal is further characterized by UV–Vis and Vickers microhardness analysis.     

Synthesis,growth, structure and characterization of nickel(II)-doped hexaaquacobalt(II) dipotassium tetrahydrogen tetra-o-phthalate tetrahydrate crystals

Single crystals of K₂[Co_(1−x)Ni_x(H₂O)₆] (C₈H₅O₄)₄·4H₂O (x = 0.25) (PCNHP), a semiorganic black colored transparent crystal of size ∼20 × 13 × 4 mm³, are grown from an aqueous solution of potassium hydrogen phthalate enriched with cobalt chloride and nickel chloride by slow evaporation solution growth technique at room temperature. Structural analysis by single crystal X-ray diffraction reveals that the crystal belongs to monoclinic system with space group P2₁/c and the cell parameters are a = 10.41(3) Å, b = 6.84(2) Å, c = 29.46(9) Å, Z = 4. Incorporation of both Co(II) and Ni(II) into the potassium hydrogen phthalate (KHP) crystal lattice is well confirmed by EDS and chemical tests. Powder XRD profiles indicate the crystallinity and FT-IR studies reveal the vibrational patterns. The UV–vis optical absorption spectrum of PCNHP shows the lower optical cut-off at ∼300 nm and the crystal was transparent in the entire visible region. The crystalline perfection of the grown crystal analysed by high-resolution X-ray diffraction (HRXRD) analysis reveals that the diffraction curve (DC) contains multi-peaks with low angular spread indicating the possibility of low angle structural grain boundaries. Scanning electron microscope (SEM) studies indicate the structure defect centers. The dielectric, thermal and mechanical behaviors of the specimen were also investigated.     

Crystal structure and packing analysis of the liquid crystal dimer alpha,omega-bis(4-cyanobiphenyl-4-yloxy)octane

The crystal structure of the liquid crystal dimer α,ω-bis(4-cyanobiphenyl-4'-yloxy)octane has been determined from diffraction data obtained with synchrotron radiation. The structure is triclinic, with the space group P-1 with Z = 2 and the unit cell parameters are a= 7.135(5) Å, b= 12.811(5) Å, c= 15.639(5) Å, α= 75.800(5)°, β= 84.690(5)°, γ= 77.930(5)°. The flexible spacer linking the mesogenic groups is in the all-trans-conformation. Although the molecule has a potential centre of symmetry, it occupies a general position in the cell; this unusual behaviour has been investigated with the aid of a theoretical evaluation of the packing energy.     

2,3-二取代-4-(IH-l,2,4-三唑-l-基)-5-苯基氢基噻吩的合成及生物活性研究

合成了九个以噻吩为母体环的含三唑环的化合物——2，3-二取代-4-(1H-1， 2，4．三唑-1-基)-5-苯基氨基噻吩(2a-2i)，并测定了2a的晶体结构．晶体为三斜 晶系，P-1空间群，晶胞参数为：a=0．79816(15)nm，b=1．00259(13)nm，c=1． 4478(4)nm，a=100．326(16)°，β=94．69(2)°，r=106．083(9)°，V=1．0845 (4)nm～3，z=2，D_c=1．396 g／cm～3．初步生物活性表明所有目标化合物杀菌活 性较低，有一定的植物生长调节活性．     

噻吩甲酰三氟丙酮合铕螯合物(TTA)_4Eu(4—MePy)H的分子结构

题目所指化合物分子式为(C_8H_4O_2F_3S)_4·Eu·(C_6H_7N)H,分子量1130.4,晶体空间群PT,晶胞参数a=16.323;b=12.364;c=11.714;α=108.54,β=90.22,Υ=102.36°;晶胞中有两个分子。由重原子法解出铕原子的位置,用加权傅里叶综合解得粗结构。经块对角矩阵最小二乘修正,偏离因子R=0.046。     

Crystal Structure of trans－2－（1－Naphthyl）－1－（p－（4＇，4＇，5＇，5＇－tetramethyl－4＇，5＇－dihydro－1＇H－imidazolyl－1＇－oxy－3＇－oxide）－phenyl）－imine，C_（24）H_（24）N_3O_2

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆｔｒａｎｓ－２－（１－Ｎａｐｈｔｈｙｌ）－１－（ｐ－（４＇，４＇，５＇，５＇－ｔｅｔｒａｍｅｔｈｙｌ－４＇，５＇－ｄｉｈｙｄｒｏ－１＇Ｈ－ｉｍｉｄａｚｏｌｙｌ－１＇－ｏｘｙ－３＇－ｏｘｉｄｅ）－ｐｈｅｎｙｌ）－ｉｍ...     

1-二茂铁基-3-(4-烷氧基-3-溴苯基)-1,3-丙二酮的合成及其结构表征

由乙酰基二茂铁(1)与4-长链烷氧基-3-溴苯甲酸甲酯(2)通过酮酯缩合反应, 合成了1-二茂铁基-3-(4-烷氧基-3-溴苯基)-1,3-丙二酮(3). 标题化合物3为首次合成, 具有复杂的共振结构．通过元素分析、红外光谱、核磁共振氢谱对其结构进行了表征. 用X射线单晶衍射法测定了1-二茂铁基-3-(4-十二烷氧基-3-溴苯基)-1,3-丙二酮(3c)的结构, 结果表明: 晶体属于三斜晶系, P-1空间群, a＝0.8677(5) nm, b＝0.8791(5) nm, c＝2.1444(11) nm, α＝101.489(9)°, β＝94.784(10)°, γ＝102.522(9)°, V＝1.5511(14) nm3, Dc＝1.273 g•cm－3, μ＝1.801 mm－1, F(000)＝618, Z＝2, R1＝0.0597, wR2＝0.1386.     

杂氮三环化合物X射线研究——Ⅲ.1-氯甲基-2,8,9-三氧杂-5-氮杂-1-硅三环[3,3,3,0~(1.5)]十一烷-3-酮的结构测定

题目所指化合物属单斜晶系,P2_1/c空间群,晶胞参数a=6.751(1),b=11.274(3),c=13.134(4),β=100.390(3)°,晶胞含分子数Z=4.用直接法和Fourier综合解得粗结构,取1490个可观测独立反射数据,经最小二乘修正,偏离因子R为0.056。三个五员环(Si,O,C,C,N)中各最大扭角分别为33.2°,23.0°,35.1°,其中最小者(23.0°)属于含羰基的环。     

新型不对称吡喃鎓方酸菁染料的晶体结构

通过缓慢挥发溶剂法得到一种不对称吡喃方酸菁染料的单晶,测定了其晶体结构.其晶系为三斜晶系,空间群为P1,a=0.9228(4),b=1.4122(6),c=0.6124(3)nm,α=93.97(4),β=98.14(5),γ=71.05(4),V=0.7470(6)nm³,Z=1.用晶体结构数据解释了此不对称染料的¹H-NMR谱.     

Crystal structure,Hirshfeld surface analysis,Thermal study and Conduction mechanism of [(C4H9)4P]3Bi2Cl9 compound

A novel tris (tetrabutylphosphonium) nonachlorodibismuthate (III) compound has been synthesized and characterized by a single‐crystal X‐ray diffraction, calorimetric, IR spectroscopy and electrical measurements. X‐ray diffraction analysis at room temperature reveals that the title compound belongs to the monoclinic system with P2₁/c space group. The unit cell dimensions are: a = 19.201(6) Å, b = 16.743 (5) Å, c = 22.396 (8) Å, β = 98.96 (2)° and Z = 4. The crystal structure was solved down to R equal to 0.035 for 5597 independent reflections. The crystal package is provided by electrostatic interactions and hydrogen bonds (C‐H ^…. Cl). Intermolecular interactions present in the grown single crystal were analyzed by Hirshfeld surface and 2‐dimensional fingerprint plot. The differential scanning calorimetry reveals one order–disorder phase transition at 400 ± 5 K.The electrical conductivity were carried out in the frequency range 200 Hz–1 MHz at various temperatures 343–413 K using impedance spectroscopy technique. The obtained results were analyzed by fitting the experimental data to an equivalent circuit model. The temperature dependence of alternating and direct current conductivities confirms the observed phase transition in the calorimetric study; they were described in terms of Arrhenius relation. AC conductivity measurements reveal that the conduction depends on both frequency and temperature, this agrees well with Correlated Barrier Hopping model in phase I and II.     

蝴蝶形原子簇化合物[MoOS3Cu2(PyPPh2)3]的制备、晶体结构 和非线性光学性质 研究

采用固相反应方法以[NH4]2[MoS2O2],CuI.Et4NBr和2-)二苯基膦)吡啶(PyPPh2)为原料制备了标题化合物。其结构用单晶分析法测定。测得化合物的分子式为MoOS3Cu2(PyPPh2)3],该晶体结构属三斜晶系,空间群为P1,所得晶胞参数为a=1.16736(4)nm,b=1.42254(5)nm,c=1.68034(6)nm,α=100.07°,β=103.2450(10)°,γ=105.0650(10)°,V=2.53991(15)nm^3,Z=2,Dc=1.504g·cm^-3,F(000)=1166,μ=13.57cm^-1.偏差因子R1=0.0590,wR2=0.1238。簇合物具有高度弯曲的蝴蝶状核,其中MoOS3^2-基团以三齿配体的形式与两个具有不同构型的Cu原子配位,氧原子不参加配位仅以端基形式存在。通过标题化合物在DMF中非线性光学性质的测定,表明其具有较好的非线性吸收和与以往不同的自散焦效应,算得其非线性吸收系数α2=4.4×10^-11m·W^-1,非线性折射系数n2=—8.225×10^-18m^2·W^-1;从而说明外围配体对非线性光学性质也具有大的影响作用。     

SYNTHESIS AND CRYSTAL STRUCTURE OF 3-(METHYLMER-CAPTO)PHENANTHRO[9,10-e] 1,2,4-TRIAZINE

<正> The title compound was synthesized by a new method and its crystal structure was determined by X-ray diffraction analysis. C16H11N3S, Mr = 277. 34, triclinic system, space group P1, cell parameters: a = 10. 410(4), b = 17. 953(5), c = 7. 468(3)(?), α=101. 47(3)°,β=110. 85(3)°, γ = 81. 53(3)°, V = 1273.8(8) (?)3, Z = 4 and Dc=1. 45gcm-3. Refinements of full-matrix least-squares converged at R = 0. 053 and Kw = 0.065 for 2794 observed reflections. There are two independent molecules in an asymmetric unit. All non-hydrogen atoms of phenanthro[9,10-e]-1,2,4-triazine make up a 18 18 large conjugated plane.     

Synthesis and X-ray crystal structure of oxamido-bridged heterobinuclear Ni(Ⅱ)-Cu(Ⅱ) complexes

The two complexes [Ni(oxen)Cu(L)2](ClO4)2.xH2O (L=2,2'-bipyridyl(bpy), 1,10-phenanthroline(phen)) have been synthesized, where oxen is N,N'-bis(2-aminoethyl)oxamido di-anion. The crystal structure of [Ni(oxen)Cu(bpy)2](ClO4)2.CH3OH has been determined by X-ray diffraction method. The crystal is triclinic system, space group P1 with a=12.179(1),b=12.298(2), c=11.476(2) A, a=97.57(1), B=97.52(1), 7=80.29(2), V=1669.04(67) A3, Z=2, Dcalcd=1.667 g/cm3. The structure has been refined to final R of 0.076 and Rw of 0.080, respectively. The complexes have an extended oxamido-bridged structure and consist of Ni(Ⅱ) ion in a square planar environment and Cu(Ⅱ) ion in a distorted octahedral environment.     

Two polymorphic modifications of 1-(N-morpholiniomethyl)spirobi- (3-oxo-2,5-dioxa-1-silacyclopentan)- ate hydrate

The compound 1-(N-morpholiniomethyl)spirobi(3-oxo-2,5-dioxa-1-silacyclopentan)ate crystallizes from aqueous solution of γ-butyrolactone in the form of two crystal hydrate modifications: monoclinic (with D = 1.53 g/cm³, space group P 2₁/n) and triclinic (D = 1.45 g/cm³, space group P1^-). For the monoclinic form, an X-ray structural study at -100°C has been performed. For both structures the coordination polyhedron of the silicon atom is a trigonal bipyramid. In the crystal structures there are strong intermolecular hydrogen bonds of NH···O and OH···O types.     

Serendipitous syntheses of the series Cs3Ln7Te12 (Ln = Sm,Gd, Tb): Compounds with large tunnels

Single crystals of Cs₃Ln₇Te₁₂ (Ln = Sm, Gd, Tb) have been grown accidentally through the reaction of Ln and Te with a CsCl or Cs₂Te₃ flux at elevated temperatures. The crystal structures have been determined from single crystal X-ray diffraction data. These compounds, which are isostructural with Rb₃Yb₇Se₁₂, crystallize in space group Pnnm of the orthorhombic system with two molecules in the following cells: Cs₃Sm₇Te₁₂, a=13.750(6), b=28.332(7), c=4.473(3) Å, T=293 K; Cs₃Gd₇Te₁₂, a=13.6064(13), b=28.209(3), c=4.4324(4) Å, T=153 K; Cs₃Tb₇Te₁₂, a=13.5708(16), b=28.116(3), c=4.4147(5) Å, T=153 K.     

Crystal structure and thermal chemical properties of 2-(2,4-dimethylanilino)-3-methyl-6-diethylaminofluorane

The crystal structure of 2-(2,4-dimethylanilino)-3-methyl-6-diethylaminofluorane has been determined by single crystal X-ray diffraction method. The crystal belongs to triclinic system, space group P-1 with unit cell constants a = 11.2877(9) Å, b = 11.9539(9) Å, c = 12.2365(9) Å, α = 97.2580(10)°, β = 116.2850(10)°, γ = 106.3710(10)°, V = 1358.48(18) Å ³, Z = 2, D _c = 1.234 g/cm³, μ = 0.079 mm^?1, F(000) = 536, R and w(R) are 0.0718 and 0.2055, respectively, for 5239 unique reflections with 3745 observed reflections (I > 2σ(I)).     

N-[2-(4-甲基)嘧啶基]-N′-2-硝基苯磺酰脲的合成、晶体结构、生物活性及其与酵母AHAS的分子对接

合成了磺酰脲化合物N-[2-(4-甲基)嘧啶基]-N′-2-硝基苯磺酰脲, 用元素分析、红外、核磁共振氢谱对产物进行了表征, 培养并测定了其晶体结构. 晶体属三斜晶系, 空间群, 晶胞参数a＝0.54159(1) nm, b＝1.1533(3) nm, c＝1.1857(4) nm, α＝83.907(6)°, β＝81.048(5)°, γ＝77.637(4)°, V＝0.7126(4) nm³, D_c＝1.572 g/cm³, Z＝2, F(000)＝348, R＝0.0659, wR＝0.1217. 在晶体结构中, 杂环上的一个N原子与脲桥上邻近的N原子上的H构成分子内氢键. 测定了对酵母AHAS的离体抑制活性, 其抑制常数K_i为(2.48±0.35)×10^－7 mol/L. 用分子对接方法, 将目标化合物晶体结构对接到靶酶酵母AHAS的活性位点, 发现对接完毕目标化合物的构象与复合物晶体中的磺酰脲分子构象接近, 并得到了合理的生物活性预测值. 该研究为进一步理解磺酰脲类的分子结构、药物活性并设计新的分子提供了帮助和指导.