一种新型三维包结物的合成和晶体结构

以六氰合钴酸钾,五水硫酸铜和乙二胺为原料,通过采用不同溶剂、不同配比实验对比,合成了一种新的三维夹心配位包结物 [Cu(en)2]2{K[Co(CN)6]}2[en=乙二胺]晶体,对其进行了元素分析、红外光谱表征和单晶结构测定.X射线单晶衍射测定表明,该配位包结物属单斜晶系,C2/c空间群,晶胞参数为a=0.8406(3)nm,b=1.6906(5)nm,c=1.1803(4)nm,β=98.931(5)°,V=0.16570(9)nm3,Z=2,dc=1.755g/cm3,μ=2.549mm-1,F(000)=884, R1=0.0323,wR2=0.0807.这种新的三维的夹心配位包结物由[Co(CN)6]3-与外界的K+离子通过氰根(-CN-)配位形成三维网络格子,在每个网格中镶嵌着二乙胺合铜(II)配合物.     

Crystal growth,structure and characterization of diglycine zinc dipicrate: Centrosymmetric crystal exhibiting second harmonic generation efficiency

A new cadmium coordination polymer, formulated as [Cd(L)(phen)]_n, were prepared by hydrothermal reactions based on 3,4-dibromothiophene-2,5-dicarboxylic acid (H₂L) and 1,10-phenanthroline (phen) mixed organic linkers. In the complex, adjacent Cd²⁺ ions are linked by L^2? anions to form a one-dimensional (1D) [CdL]_n chain with [Cd₂(COO)₂] as the secondary building unit (SBU). These adjacent chains are further stacked together by direct C?Br···Br halogen bonds interactions, generating a two-dimensional (2D) supramolecular structure. From the viewpoint of topology, the 2D supramolecular network can be rationalized to a 3,4-connected 3,4L13 net with {4.6²}₂{4².6².8²} topology.     

Crystal structure of 2,2,3-trimethyl-3-(2′,4′,5′-tricyanophenyl) cyclopentyl-1-acetic acid, methyl ester, C20H21N3O2

The title compound crystallizes in space group P2₁/n, with a = 14.600(2), b = 7.091(2), c = 18.211(5) Å, and = 103.67(2)°. Owing to the centric space group, both C(1) and C(3) chiral centers are either R or S. The acetate group is equatorial, the H(1) and the methyl group at C(3) are axial and reciprocally trans.     

超分子化合物(C_(12)H_(10)N_4)(C_7H_6O_3)_2的合成、晶体结构及荧光性质

合成了超分子化合物(C_(12)H_(10)N_4)(C_7H_6O_3)_2,并进行了元素分析、红外光谱、紫外光谱表征和单晶X射线衍射分析.构筑单元之间通过多重氢键和π-π堆积作用的协同效应形成超分子化合物,并研究了化合物的固体荧光性能.研究表明:该晶体属于单斜晶系P2_1/c空间群,晶胞参数为:a=0.3974(1) nm,b=2.0330(2) nm,c=1.4343(1) nm, β=94.892(2)°,V=1.15440(19) nm~3,d_c=1.400 g/cm~3,Z = 2,μ= 0.102 mm~(-1),F_((000))=508,R_1=0.0359,wR_2=0.0893 [I>2σ(I)].     

Crystal structure of 9,12-ethano-12a-methoxycarbonyl-5, 8a,9,12,12a,12b-hexahydro-6H-[1,2]dioxino[4′,5′:4,5] isoxazolo[3,2-a]isoquinoline, C17H19NO5

The title compound crystallizes in the space group P2₁/n, with a = 18.423(3), b = 9.628(3), c = 19.243(2) Å, = 116.208(8)°, with two independent molecules in the asymmetric unit, which are not enantiomers. The chiral centers C8a, C9, C12, C12a, C12b are either S,R,S,R,R or R,S,R,S,S, respectively, because of the centric space group.     

X-ray structure analysis of 1-(4-bromophenyl)-3-(4-chlorophenyl)-prop-2-en-1-one

The title compound crystallizes in the monoclinic space group P2₁/c with unit cell parameters a = 15.6239(15) ?, b = 14.0537(14) ?, c = 5.8396(5) ?, β = 92.666(3)°, V = 1280.8 (2) ?³, and Z = 4. The final reliability index is 0.0538 for 2921 observed reflections. Two phenyl rings of the title molecule are not coplanar, with a dihedral angle of 46.3(0)°. The molecular planarity of this substituted chalcone is strongly affected by the 4′-bromo group. The crystal cohesion is accentuated by π···π, C–H···Br interactions and R₃ ¹ (11) hydrogen bond.     

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)°.     

Crystal and molecular structure of iso-grayanotoxin II

The crystal and molecular structure of a grayanotoxin derivative, iso-grayanotoxin II, is presented. The crystal is orthorhombic, space group . The molecule is based on a tetracyclic structure consisting of two five-membered, one six-membered, and one seven-membered rings with various conformations.     

Crystal structure of 4-(6-chloro-purin-9-yl)-3-phenyl-4,5,6,6a-tetrahydro-3a H-cyclopenta[d]isoxazol-6-ol, C17H14N5O2Cl

The title compound crystallizes in the space group Pna2₁, with a = 10.124(5), b = 14.335(3), c = 11.113(2) Å. There is no conjugation between the purine moiety and the cyclopentane ring, whereas there is some conjugation between the isoxazoline and the phenyl rings. The chiral centers C3a, C4, C6a, C6 are either S, S, R, R or R, R, S, S respectively, because of the glide planes. The molecules are linked by intermolecular hydrogen bonds and van der Waal’s forces.     

Zn1-x HfxO的电子结构和光学性质的第一性原理计算

基于第一性原理密度泛函理论,计算分析了Zn1-xHfxO(x=0,0.0312,0.0417,0.0625和0.1250)体系的晶格结构、电子结构,Mulliken电荷布居和光学性质.计算结果表明,随着Hf掺杂摩尔百分比的增大,晶体体积膨胀,费米能级进入导带,其附近的导带部分主要由杂质原子Hf的5d态贡献,Hf-O离子键成分作用凸显,故Hf的掺杂引入施主能级进而形成n型ZnO材料的可能性较大.且通过比较吸收谱、反射谱和折射谱,发现适量掺入Hf原子可使ZnO体系在高能区的透过率增加,能量损失谱出现红移.这些性质均与实验中Hf掺杂有类似结果,由此可知适量掺杂Hf的ZnO体系有望在制备光电子器件等领域发挥作用.     

The Crystal and Molecular Structure of tert‐Butoxycarbonyl ‐ α‐aminoisobutyryl ‐ isoleucyl ‐methylester

The crystal structure of the synthetic peptide Boc — Aib — Ile ‐ OMe (C₁₆ H₃ 0 N₂ O₅ ) has been determined from three‐dimensional X — ray diffraction data. The peptide crystallizes in triclinic space group P1 with a = 9.570(9), b = 10.261(7), c = 10.610(2) Å , α = 101.9(0), β = 91.7(0), γ = 98.6(0)° V = 1006.1(12) ų, Z = 2, D_calc = 1.09 Mg m^‐3. The structure was solved by direct methods and refined by full‐matrix least‐squares method to an R value of 0.072 (λ = 1.5418Å). The conformation of Aib residue in molecule A is αL and in molecule B is αR. The Ile residue in molecule A adopts folded conformation, while in molecule B it is in the extended region. The peptide units are trans and show significant deviations from planarity.     

Synthesis and crystal structure of 3,5,9,11-tetraacetyl-14-oxo-1,3,5,7,9,11-hexaazapentacyclo[5.5.3.02,6.04,10.08,12]pentadecane

Crystals of 3,5,9,11-tetraacetyl-14-oxo-1,3,5,7,9,11-hexaazapentacyclo[5.5.3.0^2,6.0^4,10 .0^8,12]pentadecane, a new hexaazaisowurtzitane derivative, were obtained from a condensation reaction of 2,6,8,12-tetraacetyl-2,4,6,8,10,12-hexaazatetracyclo[5.5.0.0^5,9.0^3,11] dodecane with aqueous formaldehyde and subsequent crystallization of the product from aqueous acetone. X-ray diffraction analysis at room temperature indicates that the compound crystallizes in monoclinic system, space group P2₁/n with a = 9.4564(15), b = 14.184(2), c = 13.334(2) ?, β = 107.671(4)°, V = 1704.1(5) ?³, Z = 4, D _calc = 1.475 g/cm³, F(000) = 800, μ(MoK) = 0.112 mm⁻¹, and final R ₁ = 0.0505, wR ₂ = 0.1215 for observed reflections 2641 (I > 2σ(I)). The ether link (C–O–C) forms two heptacyclic rings with the N, C atoms in the cage respectively. The results of elemental analysis, IR and NMR spectroscopy are included.     

Crystal and molecular structure of the symmetrical bidentate ligand 3,3-di(1-pyrazolyl)pentane, CH3CH2C(C3H3N2)2CH2CH3

The title compound crystallizes in the centrosymmetric space group C2/c with a = 14.4005(23), b = 7.0494(12), c = 11.2462(20) Å, = 101.572(13)° and Z = 4; the molecule lies on a crystallographic C ₂ axis. Hydrogen atoms were both located and refined.     

Crystal Structure of Diethyl 2‐[2,2,2‐ trifluoro‐1‐(indole‐3‐yl)‐ethyl]‐2‐acetamidomalonate

The title compound (C₁₉H₂₁F₃N₂O₅) has been determined from three dimensional X‐ray diffraction data. The crystals are monoclinic, a = 7.626(4)Å, b = 17.515(4)Å, c = 15.066(3)Å, β = 101.02(3)°, V = 1975(1)ų, Z = 4, D_calc = 1.393g cm^‐3, space group P2₁/c. The structure was solved by direct methods and refined by full‐matrix least‐squares method (R = 0.039).     

Structure of 2-(1-phenylimidiazolidin-2-ylidene)- malononitrile and 2-(hexahydropyrimidinyl-2-ylidene)- malononitrile

The crystal structure of 2-(1-phenylimidazolidin-2-ylidene)-malononitrile, I, and 2-(hexahydropyrimidin-2-ylidene)-malononitrile, II, were determined with crystal data (I: Monoclinic, P2₁/n, a=8.116(3) ?, b=7.650(3) ?, c=17.399(7) ?, β=93.065(6)°, R _all=0.0980; II: Monoclinic, P2₁/n, a=9.169(2) ?, b=8.103(2) ?, c=10.337(3) ?, β=99.853(4)°, R _all=0.0877). N−H···N hydrogen bonds were responsible for the formation of centrosymmetric dimers of I and one-dimensional zigzag molecular chains of II.     

Crystal Structure Analysis of a New Coumarin Derivative

The title compound (6,6‐dimethyl‐cis‐6H,6aH,7H,12bH,13H‐bis[1]benzopyrano[4,3‐b:4',3'‐d]pyran‐13‐one) crystallizes in monoclinic space group P2₁ /c with Z = 4. The unit cell dimensions are a = 8.6231(2) Å, b =10.0260(2) Å, c = 19.8376(2) Å, and β = 102.1(1)°, V = 1674.51(5) ų , D_cal = 1.326 Mg/m³. The coumarin moiety is in the planar conformation, the dioxadecalin moiety is cis fused and within the dioxadecalin moiety both the rings are in half cahir/sofa conformations. The structure has many C‐H … O type interactions.     

晶体结构控制晶体形态的理论及应用

本文对比分析了研究晶体宏观形貌与内部结构关系的3种主要理论,即布拉维法则、周期键链理论和负离子配位多面体生长基元理论.提出利用布拉维法则,结合晶胞形状及结构中螺旋轴、滑移面的影响,可以更准确地分析晶体的习性,并据此对晶体习性进行了分类.     

1-(Ethoxymethyl)-6-(phenylselenyl)-5-ethyl uracil: a nucleoside analog

The compound, 1-(ethoxymethyl)-6-(phenylselenyl)-5-ethyl uracil, crystallizes in the monoclinic space group P2₁/n with unit cell parameters a = 5.304(1), b = 21.261(4), c = 13.996(4) Å, = 94.30(2)°, and Z = 4. The acyclic chain C1, O4, C4, C5 is in fully extended form and nearly perpendicular to the uracil base. The molecules are held together by van der Waal's forces.     

Crystal Structure Analysis of 1′,2′,3′,4′‐tetrahydro‐1,3‐diphenyl‐4‐chlorospiro[2‐pyrazoline‐5,2‐napthalen]1′one

The crystal structure of the title compound “1′,2′,3′,4′‐tetrahydro‐1,3‐diphenyl‐4‐chlorospiro[2‐pyrazoline‐5,2‐napthalen] 1′one” has been determined. The structure consists of a pyrazoline ring, three aromatic rings and a tetralone moiety. All the aromatic rings are planar while the cyclohexonone ring of the tetralone moiety is in the distorted sofa conformation. The molecular packing is stabilized by C‐H…O and C‐H…π type inter molecular interactions.