Ba7(BO3)3F5晶体结构及热分析

采用高温溶液法从BaCO3,BaF2及H3BO3混合体系中生长出了一种氟硼酸钡晶体,Ba7(BO3)3F5晶体属六方晶系,空间群为P63mc,晶胞参数:a=1.11562(15) nm,c=0.72415(14) nm,Z=2,V=0.7805(2) nm3.Ba7(BO3)3F5晶体结构是由Ba(1)O7F3基团,Ba(2)O4F3基团,Ba(3)O6F4基团和独立的BO3基团相互连接形成的三维空间网络结构.Ba7(BO3)3F5的热分析分析结果表明Ba7(BO3)3F5在1070℃同成份熔化.     

Synthesis and crystal structure of 2-anilino-6<Emphasis Type="Italic">H</Emphasis>-5-(1-phenyl-3-methyl-5-pyrazolone-4-ylene)-1,3,4-thiadiazine

A novel pyrazolone derivative 2-anilino-6H-5-(1-phenyl-3-methyl-5-pyrazolone-4-ylene)-1,3,4-thiadiazine (PMCP-PTSC) containing NNS hexa-atomic heterocycle has been obtained and characterized by means of single crystal X-ray diffraction, IR and ¹H NMR spectroscopies. It is interesting that when grown from two different solvents, two different crystalline structures are formed. The monoclinic crystal A belongs to a P2₁/c space group. The unit cell parameters are a = 16.414(4) Å, b = 12.530(3) Å, c = 8.432(1) Å, = 91.75(2) Å, and Z = 4. The triclinic crystal B belongs to a P space group. The unit cell parameters are a = 11.386(2) Å, b = 12.326(2) Å, c = 12.411(3) Å, = 83.07(1)°, = 87.76(2)°, = 86.52(2)°, and Z = 4. The structure analyses show the title compound is the keto-form. Dimers in crystal packing of A and supramolecular one-dimensional (B) concatenate structures were assembled by the intermolecular hydrogen bonds.     

全取代环戊基六元瓜环晶体制备及其晶体结构研究

研究了对全取代环戊基六元瓜环(CyP6Q6)与结构诱导剂ZnCl2在稀盐酸条件下长的晶体进行X-射线单晶衍射分析.通过实验得到一个新的晶体,其结构表明,晶体属于斜方晶系,空间群为P21/n,a=27.599(7)(A),6=17.393(7)(A),c=18.265(5)(A),α=90.00°,β=93.369(6)°,γ=90.00°,Z=4,R=0.046,其中结构中出现了蜂巢效应并且形成了较大的孔道.     

Synthesis and crystal structure of copper(II) complex with 1,9-diamino-5-methyl-5-nitro-3,7-diazanonane

Condensation of bis(ethanediamine)copper(II) perchlorate with formaldehyde and nitroethane in basic methanol was found to generate (1,9-diamino-5-methyl-5-nitro-3,7-diazanonane)copper(II) perchlorate, [Cu(L₁)](ClO₄)₂. The copper(II) complex was characterized by elemental analysis and infrared and electronic spectra studies. The structure of [Cu(L₁)](ClO₄)₂ was determined by X-ray diffraction. The crystal structure revealed that the copper ion is in an elongated octahedral coordination with four nitrogens at the equational position and perchlorate anions at the axial positions and that one of the perchlorate anions bridges two copper ions, leading to a linear polymeric structure in the crystal.     

The Crystal Structures of Some 1-Aryl-5-methyl-1,2,3-triazole Derivatives

Abstract  The two 1-aryl-5-methyl-1,2,3-triazole derivatives were prepared by the 1-aryl-5-methyl-1,2,3-triazol-4-carboxylic acids 3. The yielded products 4a–b were confirmed by NMR, MS, IR spectra. We investigated the crystalline structure of compounds 4a and 4b. Compound 4a, C₉H₈BrN₃, Mr = 238.09, crystallizes in the monoclinic space group P2(1)/n with unit cell parameters a = 11.660(2), b = 7.668(2), c = 11.818(2) ?, α = 90.00, β = 116.01(3), γ = 90.00o. V = 949.6(3) ?³, Z = 4, Dx = 1.665 Mg m⁻³. The final R was 0.0477. Compound 4b, C₁₃H₁₁N₃, Mr = 209.25, crystallized in the orthorhombic space group Pbca with unit cell parameters a = 10.373(2) ?, b = 11.691(2) ?, c = 17.579(4) ?, α = 90.00o, β = 90.00o, γ = 90.00o, V = 2131.8(7) ?³, Z = 8, D _m = 1.304 Mg m⁻³. The final R was 0.0565. Index Abstract  The two 1-aryl-5-methyl-1,2,3-triazole derivatives were prepared by the 1-aryl-5-methyl-1,2,3-triazol-4-carboxylic acids 3. The yielded products 4a–b were confirmed by NMR, MS, IR spectra. We investigated the crystalline structure of compounds 4a and 4b. Compound 4a, C9H8BrN3, Mr = 238.09, crystallizes in the monoclinic space group P2(1)/n with unit cell parameters a = 11.660(2), b = 7.668(2), c = 11.818(2)  ?, α = 90.00, β = 116.01(3), γ =90.00o. V = 949.6(3) ?³, Z = 4, Dx = 1.665 Mg m⁻³. The final R was 0.0477. Compound 4b, C13H11N3, Mr = 209.25, crystallized in the orthorhombic space group Pbca with unit cell parameters a = 10.373(2) ?, b = 11.691(2) ?, c = 17.579(4) ?, α = 90.00o, β = 90.00o, γ = 90.00o, V = 2131.8(7) ?³, Z = 8, D _m = 1.304 Mg m⁻³. The final R was 0.0565.      

Na5[B2P3O13]晶体双晶结构的研究

采用泡生法和b向籽晶生长出尺寸为22mm×24mm×20mm的透明Na5[B2P3O13]晶体.晶体定向中发现(100)和(001)晶面的一级衍射出现双峰;正交偏光显微镜下观察晶体的(010)切片,看到清晰的明暗条纹;当一束激光正入射(010)切片时,产生衍射现象;用同步辐射白光X射线形貌术拍摄了(100)、(010)和(001)切片的Laue像,观察到了晶体的孪晶结构,再借助(010)切片的化学腐蚀研究,推出该晶体为规则的聚片双晶,其结合面为(001).     

Crystal structure of pyrazole derivatives. IV. 5-chloro-4-chlorosulfonyl-3-methyl-1-phenylpyrazole

The title compound crystallizes in space groupP2 ₁/a witha=17.063(1),b=13.208(1),c=21.260(2) Å, =99.51(1)°,V=4726(1) ų,Z=16, there are four independent molecules in the asymmetric unit. The phenyl and pyrazole rings are planar, to within experimental accuracy, making different dihedral angles in the independent molecules: 42.2(1), 129.5(1), 52.5(1), and 46.2(1)°.     

Formation and crystal structure of 1-methyl-2-phenylindolizine-3-acetonitrile

1-Methyl-2-phenylindolizine-3-acetonitrile was unexpectedly obtained in the reaction of 1-methyl-2-phenylindolizine-3-thioaldehyde with cyanide ions. Its structure was determined by IR, ¹H NMR, MS, elemental analyses, and X-ray crystallography. Colorless regular prism shaped crystals of C₁₇H₁₄N₂ crystallize in the space group C2/c with cell dimensions a = 12.956(3) Å, b =10.516(2) Å, c = 20.429(4) Å, and = 90°, = 104.98(3)°, = 90°, V =2688.7(9) ų, D _calc =1.217 Mg/m³, and Z = 8.     

非线性光学晶体BaBPO5的生长、结构研究

本文采用顶部籽晶高温溶液法,以Li4P2O7为助熔剂,生长了大尺寸BaBPO5单晶.进行了BaBPO5晶体的结构测定,结果表明该晶体属三方晶系,空间群:P3221,晶胞参数为a=b=0.71329(10)nm,c=0.70368(14)nm,α=β=90°,γ=120°, Z=3.该晶体结构中沿[001]方向存在BO4四面体链,每一个硼氧四面体用它的两个顶点分别与两个PO4四面体相连组成螺旋状的链.硼氧四面体、磷氧四面体和钡氧多面体结合在一起形成一个三维网络结构.同时,对BaBPO5的粉末倍频效应进行了研究.     

Synthesis and structure of 4-methyl-1-N-(p-tolyl)imidazole as organic corrosion inhibitor

Heterocyclic organic compounds containing nitrogen, sulfur or oxygen atoms are often used to protect metals from corrosion acting as organic corrosion inhibitors. Their inhibiting role is based on excellent ligand abilities and formation of stabile metal complex. Two requirements are essential for using selected class of organic inhibitors: (a) ligand capacity in the conditions of corrosion such as atmospheric conditions, acid or neutral corrosion, etc., and (b) nontoxicity, i.e., environmentally friendly inhibitors. Imidazole derivatives are capable to fulfil both requirements and they are, from that point of view, very promising and profound class of ligands. Synthesis and X-ray diffraction molecular and crystal structure of 4-methyl-1-N-(p-tolyl)imidazole has been reported, since it exhibits the most prominent corrosion inhibiting role. The synthesis, starting from 4-methylimidazole and 4-bromotoluene, is based on Ullmann-type coupling reaction by applying modifications of N-arylation by arylhalogenides and Cu₂O as an efficient catalyst.

The molecular and crystal structure of prepared N-substituted imidazole derivative reveals non-planar molecular conformation and the supramolecular assembling of the molecules via C-H···N intermolecular hydrogen bonds between C_sp2-H proton donor groups and basic imidazole nitrogen atom. The molecules are related by a 2₁ screw axis parallel to [0 1 0] in the form of infinite C(4) zig-zag 1D chains via C-H···N intermolecular hydrogen bonds. Such alignment produces additional weak stacking interaction between imidazole and phenyl ring of related chains.     

Crystal structures of two isomeric oximes. (EE)-2-methyl-3-phenyl-3-thiocyanatopropenaldoxime and (Z)-5-methyl-6-phenyl-1,3-thiazin-2-one oxime

The crystal structure of two isomeric oximes, C₁₁N₁₀N₂OS have been studied by X-ray diffraction. The open-chain thiocyanato derivative is somewhat'less dense and crystallizes with the orthorhombic space group Pbcn;a,b,c=18.718(1), 10.601(3), 11.528(1) Å,Z=8. The heterocyclic isomer occurs as pseudo-orthorhombic (Cmma)twinned crystals of space group P2₁/n, a, b, c, =12.11(1), 7.46(1), 12.12(1) Å, 100.09(1)^o,Z=4. Twinning occurs as a result of the near-equality of the monoclinica andc cell constants.     

Structure of (Z)-1-p-methoxyphenyltelluro-1,4-diphenyl but-1-en-3-yne

C₂₃H₁₈TeO,M _r=437.97, ,a=9.940(2),b=13.664(3),c=7.895(2) Å, =80.60(1), =69.71(2), =75.95(1)°,V=972.0(4) ų,Z=2,R=0.041 for 2668 observed reflections. The Te–C bond distances are 2.109(5)Å and the C–Te–C angle is 96.0(2)°. The phenyl rings are planar to within experimental accuracy, making dihedral angles of 64.6(2), 65.3(2) and 31.1(3)°.     

具有非对称中心结构的硼酸盐Bi2ZnB2O7的合成、晶体结构和光学性质

具有非对称中心结构的硼酸盐Bi2ZnB2O7由固相反应法在低于700℃下制备得到.X射线单晶结构分析表明,该化合物以正交空间群Pba2结晶,晶体学参数为:a=1.0819(2)nm,b=1.1023(2)nm,c=0.4890(1)nm,Z=4.其晶体结构中包含分别由[BO3]3-和[BO4]5-组成的[B2O5]4-和[B2O7]8-基团,它们被[ZnO4]四面体通过共用O原子的方式连接成二维2∞[ZnB2O7]6-层,这些层由Bi3+离子进一步结合形成三维网.红外光谱证实了[BO3]3-和[BO4]5-基团的存在,粉末倍频效应测试表明,其强度为KDP(KH2PO4)的4倍,UV漫反射光谱表明该物质吸收边约为360 nm.     

Structure of ultraphosphate glasses with small rare-earth ions by X-ray diffraction

Rare-earth ultraphosphate glasses with nominal R₂O₃ fractions of 10 and 15 mol% and small ionic radius (large atomic number) R³⁺ ions (R = Tb, Tm, Lu) are measured by X-ray diffraction at a synchrotron with photons of 119 keV (maximum scattering vector 260 nm^− 1). The total correlation functions T(r) show well-resolved R-O and O-O first-neighbor peaks. In contrast to all ultraphosphate RP₅O₁₄ crystals and the ultraphosphate glasses of larger R³⁺ ions, where RO₈ polyhedra (mean R-O coordination numbers of ~ 8 for the glasses) are observed, the R³⁺ ions in glasses with R = Lu, Tm, Tb have mean R-O coordination numbers of ~ 7.5. The R-O first-neighbor peaks extracted from the T(r) functions are compared with those obtained from atomic coordinates of related RP₅O₁₄ and RP₃O₉ crystals. The R-O distances of the ultraphosphate glasses studied are found to fall between those of the two crystals but with tails to the side of longer bonds.     

17α-acetoxy-17β-methyl-16β-phenyl-D-homo-4,6-pregnadiene-3,17a-dione: synthesis and crystal structure determination of a new rearranged pregnane derivative

The title compound is C₂₉H₃₄O₄, tetragonal, P4₃, a = b = 10.310(1), c = 23.871(2)Å. The A, B, C, and D rings adopt envelope, half-chair, chair, and distorted chair conformations, respectively. The phenyl ring is planar. The methyl substituents at the A/B, C/D, and at C(17) are axial; and the –OCOCH₃ group at C(17) and phenyl ring at C(16) are equatorial. The molecules in the crystal are held together by van der Waals forces and several C–H···O hydrogen bond interactions.     

Synthesis and crystal structure of 1-acetyl-3,6-diphenyl-1,4-dihydro-1,2,4,5-tetrazine

1-Acetyl-3,6-diphenyl-1,4-dihydro-1,2,4,5-tetrazine (1) was prepared and its structure was determined by X-ray diffraction. Crystallization of 1 occurs in the monoclinic space group P2₁/c with a =15.180(5) Å, b = 9.216(4) Å, c =10.129(7) Å; = 101.99(5)°; and Z =4. The structure was solved by direct methods and refined to an R value of 0.0414. The central six-membered ring of the compound of 1 has a boat conformation and is not homoaromatic.     

Crystal structure of 4-methyl-2-phenylbenzo[de]cyclobut[i] isoquinoline-3,5(2H)-dione

4-Methyl-2-phenylbenzo[de]cyclobut[i]isoquinoline-3,5(2H)-dione, C₂₁H₁₅NO₂, resulted from the photochemical reaction of N-methyl-1,8-naphthalenedicarboximide with phenylacetylene, has been characterized by ¹H NMR, IR, and MS spectra and established by single-crystal X-ray crystallography. The crystal structure belongs to the monoclinic space group P2₁/n with cell parameters a = 12.530(2) Å, b = 9.324(2) Å, c = 13.296(2) Å, = 96.85(1), V = 1542.3(4) ų, and Z = 4.     

Crystal structure and conformation of the antimalarial drug 5,7-methoxy-8-(3-methyl-1-buten-3-ol)-coumarin

The crystal and molecular structure of the antimalarial compound 5,7-methoxy-8-(3-methyl-1-buten-3-ol)-coumarin, C₁₆H₁₈O₅, M _r = 290.3 Da, has been determined from X-ray diffraction data. The material crystallizes in the monoclinic space group P2₁/c with 4 molecules per unit cell of dimensions a = 8.9044(9), b = 17.623(1), c = 10.175(1) Å, = 113.97(1)°, crystal density D _c = 1.322 g/cm³. The structure was determined using direct methods and refined by full-matrix least squares to a conventional R index of 0.066 for 2416 measured reflections and 206 parameters.The coumarin ring system is almost planar with the methoxy C atoms rotated slightly out of the coumarin mean plane. Apart from the terminal CH₃ groups C(12) and C(13), which are 1.184(3) Å above and –1.315(3) Å below the plane, the 3-methyl-1-buten-3-ol substituent is planar (rms deviation 0.009 Å) making an angle of 6.31(7)° with the phenyl ring. One intermolecular hydrogen bond is present in the crystal structure between O(5)–HO(5) and the symmetry related O(2) oxygen, generated by the symmetry operation (x, 1/2 – y, –1/2 + z).     

Structure of 2-{2-[3-methyl-3-(2,4,6-trimethylphenyl) cyclobutyl]-2-oxoethyl}isoindole-1,3-dione

2-{2-[3-Methyl-3-(2,4,6-trimethylphenyl)cyclobutyl]-2-oxoethyl}isoindole-1,3-dione (C₂₄ H₂₅NO₃) was synthesized, and its crystal structure was determined by X-ray crystallographic techniques. The compound crystallizes in the triclinic space group P-1, with unit cell parameters: a = 14.109(9) Å, b = 14.130(8) Å, c = 12.152(6) Å, = 105.62(5)°, = 113.75(4)°, = 98.78(5)°, V = 2039.8(19) ų, D _c= 1.223 g/cm³, and Z = 4. The crystal structure has two crystallographically independent molecules, I and II. These molecules are held together by weak intermolecular C—H···O interactions, forming a continuous chain. The dihedral angles between the N-substituted phthalimide moiety and cyclobutane ring in molecules I and II are 60.37(14) and 68.18(18)°, respectively.     

Structural characterization of a series of cyclohexaphosphates: M0.5((C6H5CH2)2NH2)5P6O18·H2O (M = Co, Cu, Cd)

Three new cyclohexaphosphates with general formula M_0.5((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 ų, 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.