DABCO-Catalyzed Multicomponent Reaction for Synthesis of Benzo[a]carbazoles

DABCO (1,4-diazabicyclo[2.2.2]octane) catalyzed a multicomponent reaction using the starting precursor 2,3,4,9-tetrahydro-1H-carbazol-1-one, malononitrile, and aromatic/heteroaromatic aldehyde.     

Synthesis and THF Accompanied Crystal Structure of llH-Naphtho[1＇,2＇：5,6]- pyrano[2,3-d]pyrimidin- 11 （10H）-one

8,9,12-Trihydro-9,9-pentamethylene- 12-（3-nitrophenyl）- 11H-naphtho[ 1＇,25,6]- pyrano[2,3-d]pyfimidin- 11 （10H）-one 1, another conversion product of Ffiedlandler reaction, has been synthesized by the reaction of 2-amino-4-（3-nitrophenyl）-4H-benzo[f]chromene-3-carbonitrile 2 with cyclohexanone in the presence of Lewis acid catalysts. The crystal of the title compound 1 THF solvate, C60H62N6O10, was obtained and determined by X-ray diffraction method. The crystal is of triclinic, space group P1 with a = 11.4633（11）, b = 12.6247（12）, c = 19.658（2）A, α = 72.642（8）, β = 89.045（9）, γ = 68.340（5）°, V = 2509.6（4）, Z = 2, De = 1.359 g/cm^3, F（000） = 1088, Mr = 1027.16, the final R = 0.0674 and wR = 0.1869 with Ⅰ 〉 2σ（Ⅰ） and the goodness-of-fit S = 1.045 on F^2. The pyrimidine ring has an envelope conformation, linked with a six-membered ring through a spiro C atom. The crystal packing of 1 THF solvate is stabilized by N-H…O hydrogen bonds, and π-π stacking interaction occurs between two adjacent nearly planar molecules of 1.     

Synthesis and THF Accompanied Crystal Structure of 11H-Naphtho[1',2':5,6]- pyrano[2,3-d]pyrimidin-11(10H)-one

8,9,12-Trihydro-9,9-pentamethylene-12-(3-nitrophenyl)-11H-naphtho[1',25,6]-pyrano[2,3-d]pyrimidin-11(10H)-one 1,another conversion product of Friedlndler reaction,has been synthesized by the reaction of 2-amino-4-(3-nitrophenyl)-4H-benzo[f]chromene-3-carbo-nitrile 2 with cyclohexanone in the presence of Lewis acid catalysts.The crystal of the title compound 1 THF solvate,C60H62N6O10,was obtained and determined by X-ray diffraction me-thod.The crystal is of triclinic,space group P with a = 11.4633(11),b = 12.6247(12),c = 19.658(2) ,α = 72.642(8),β = 89.045(9),γ = 68.340(5)°,V = 2509.6(4),Z = 2,Dc = 1.359 g/cm3,F(000) = 1088,Mr = 1027.16,the final R = 0.0674 and wR = 0.1869 with Ⅰ > 2σ(Ⅰ) and the goodness-of-fit S = 1.045 on F2.The pyrimidine ring has an envelope conformation,linked with a six-membered ring through a spiro C atom.The crystal packing of 1 THF solvate is stabilized by N-H···O hydrogen bonds,and π-π stacking interaction occurs between two adjacent nearly planar molecules of 1.     

K_(10)[H_2W_(12)O_(42)]·11H_2O的合成及晶体结构分析

在水溶液中反应制得无色透明的标题化合物单晶 ,单晶X -射线结构分析表明 ,属单斜晶系 ,空间群P2 1,晶胞参数 :a=1.15 47(2 )nm ,b =1.430 9(3)nm ,c =1.5 495 (3)nm ,β =10 5 .41(3)° ,V =2 .46 81(9)nm3,Z =2 ,Dc=4.6 39Mg/m3,对 5 45 4个独立衍射点 (I>2δ(I) )进行全矩阵最小二乘法修正后 ,可靠性因子R =0 .0 487     

1,3-Alternate and C-1,2-Alternate Tetrahomodioxacalix[4]crowns. Crystal Structures and Metal Ion Complexation

Two novel tetrahomodioxacalix[4]crowns with crown-5 and crown-6 rings weresynthesized. From X-ray crystal structures, homooxacalix[4]crown-5 (3) andhomooxacalix[4]crown-6 (2) were found to be in the 1,3-alternate and theC-1,2-alternate conformations, respectively. Homooxacalix[4]crown-5 (1)shows a marked selectivity for cesium ion over other metal ions tested.     

Preparation and Crystal Structure of a Rare-earth Salt Based on the Decavanadate (V10O286-):[Y(H2O)8]2[V10O28]·9H2O

The salt, [Y(H2O)8]2[V10O28]·9H2O, contains two discrete water-groups coordinated Y(III) cations, an isopoly complex ion, decavanadate (V10O286-) and nine additional water molecules, which are combined together by static electric forces and hydrogen bonds. The Y3+ is eight-coor- dinated with a square antiprism geometry. The single-crystal X-ray analysis reveals that the crystal crystallizes in triclinic, space group P with a = 9.1454 (18), b = 10.007(2), c = 12.772(3)(A),α = 68.86(3), β = 77.50(3),γ = 89.23(3)°, V = 1061.7(4)(A)3 and Z = 1.     

Syntheses,Crystal Structures and Properties of Three New Complexes [Ni（C9N2O2H7）2（CH3OH）2],[Zn（C9N2O2H7）2（H2O）2] and [Cd（C9N2O2H7）2（CH3OH）2]

Three novel metal-organic complexes with formulas [Ni(C9N2O2H7)2(CH3OH)2](1),[Zn(C9N2O2H7)2(H2O)2](2) and [Cd(C9N2O2H7)2(CH3OH)2](3) were synthesized by the reactions of Ni,Zn and Cd salts with ethyl 2-benzimidazolylacetate under hydrothermal conditions or layering technique,and characterized by single-crystal X-ray diffraction analysis,IR spec-troscopy,solid-state luminescent properties and thermogravimetric(TG) analysis.The crystal data for these three complexes are as follows:for 1,monoclinic,space group P21/c,a = 9.384(3),b = 9.634(3),c = 11.292(3) ,β = 95.787(5)°,V = 1015.7(5) 3,Z = 2,F(000) = 492,Dc = 1.547 Kg/m3,μ = 1.002 mm-1,the final R = 0.0451 and wR = 0.0900 for 1833 observed reflections with Ⅰ 2σ(Ⅰ);for 2,orthorhombic,space group Pbca,a = 10.031(4),b = 10.379(4),c = 17.525(7),V = 1824.6(12) 3,Z = 4,F(000) = 928,Dc = 1.645 Kg/m3,μ = 1.392 mm-1,the final R = 0.0452 and wR = 0.0996 for 1661 observed reflections with Ⅰ 2σ(Ⅰ);for 3,monoclinic,space group P21/c,a = 9.9114(13),b =10.4852(15),c = 10.4120(14) ,β = 108.453(5)°,V = 1026.4(2) 3,Z = 2,F(000) = 532,Dc = 1.705 Kg/m3,μ = 1.110 mm-1,the final R = 0.0322 and wR = 0.0805 for 1822 observed reflections with Ⅰ 2σ(Ⅰ).In the three complexes,the ethyl 2-benzimidazolylacetate shows the same chelating mode,and the adjacent units are interlinked into a two-dimensional layer through hydrogen-bonds(O-H···O,N-H···O).     

Indium-based liquid clathrates. I. The preparation of the first indium liquid inclusion compound and crystal structure of its parent complex, [K · 18-Crown-6]2[InClI2(CH3)][InClI(CH3)2]

The synthesis of the first liquid clathrate derived from an indium precursor is described. The aromatic/anion ratio of the inclusion complex prepared using benzene is 12.4. The use of toluene results in the inclusion of 10.3 guest toluene molecules/anion. The crystal structure of the parent complex, [K·18-Crown-6]₂[InClI₂(CH₃)][InClI(CH₃)₂] was carried out. The compound belongs to the monoclinic space groupP2₁/c, witha=19.508(9),b=8.503(5), andc=29.437(9) Å, =96.55(3)°, andD _calc=1.83 g cm^–3 forZ=4. Least-squares refinement based on 3449 observed reflections led to a finalR=0.099. The structure displays two different environments for the two K⁺ cations in the asymmetric unit. One adopts the near-planar [K·18-crown-6]⁺ configuration while the other K⁺ resides 0.81 Å above the second 18-crown-6 plane. The latter K⁺ is apparently pulled out of the crown by a strong interaction with a Cl^– ion. Supplementary Data related to this article are deposited with the British Library as Supplementary Publication No. SUP 82046 (25 pages).     

一种新颖层状磷酸镓化合物[Ga3(PO4)4](H3NCH2CH2)2NH2的合成与结构表征

晶体结构;水热合成;一种新颖层状磷酸镓化合物[Ga3(PO4)4](H3NCH2CH2)2NH2的合成与结构表征     

ChemInform Abstract: Ab initio Characterization of [H3N×BH3]2, [H3N×AlH3]2, and [H3N×GaH3]2.

ChemInform is a weekly Abstracting Service, delivering concise information at a glance that was extracted from about 100 leading journals. To access a ChemInform Abstract of an article which was published elsewhere, please select a “Full Text” option. The original article is trackable via the “References” option.     

Synthesis and the crystal structure of the supramolecular complex [Cl3InW3S4(H2O)9]2+ with cucurbituril

The supramolecular complex {[Cl₃InW₃S₄(H₂O)₉]₂(C₃₆H₃₆N₂₄O₁₂)}Cl₄·28H₂O was prepared by mixing solutions of [Cl₃InW₃S₄(H₂O)₉]²⁺ and cucurbituril in hydrochloric acid. The molecular and crystal structure of the resulting complex was established by X-ray diffraction analysis.     

M3+(H2AsO4)(H2As2O7) (M3+ = Al,Ga) and In2(H2AsO4)2(H2As2O7)2: a new layer structure type and a new framework structure type containing the rare H2As2O72− group

The crystal structures of hydrothermally synthesized aluminium dihydrogen arsenate(V) dihydrogen diarsenate(V), Al(H₂AsO₄)(H₂As₂O₇), gallium dihydrogen arsenate(V) dihydrogen diarsenate(V), Ga(H₂AsO₄)(H₂As₂O₇), and diindium bis[dihydrogen arsenate(V)] bis[dihydrogen diarsenate(V)], In₂(H₂AsO₄)₂(H₂As₂O₇)₂, were determined from single‐crystal X‐ray diffraction data collected at room temperature. The first two compounds are representatives of a novel sheet structure type, whereas the third compound crystallizes in a novel framework structure. In all three structures, the basic building units are M ³⁺O₆ octahedra (M = Al, Ga, In) that are connected via one H₂AsO₄⁻ and two H₂As₂O₇²⁻ groups into chains, and further via H₂As₂O₇²⁻ groups into layers. In Al/Ga(H₂AsO₄)(H₂As₂O₇), these layers are interconnected by weak‐to‐medium–strong hydrogen bonds. In In₂(H₂AsO₄)₂(H₂As₂O₇)₂, the H₂As₂O₇²⁻ groups link the chains in three dimensions, thus creating a framework topology, which is reinforced by weak‐to‐medium–strong hydrogen bonds. The three title arsenates represent the first compounds containing both H₂AsO₄⁻ and H₂As₂O₇²⁻ groups.     

Short-step syntheses and complexation properties of Z,Z-tribenzodidehydro- and all-Z-tribenzo[12]annulenes

Syntheses of all-Z-tribenzo[12]annulenes (1a-c) and Z,Z-tribenzodidehydro[12]annulenes (2a-c) by the reduction of the corresponding tribenzohexadehydro[12]annulenes 3a-c were carried out using a low valent titanium complex generated from Ti(O-i-Pr)₄ and i-PrMgCl. The unique structure of the first reduction products 2a-c as well as 1a-c was fully characterized. Complexation of these annulenes with silver(I) ions produces the corresponding silver complexes. Among them, the silver complexes of 2a-c exhibit interesting monomer-dimer equilibrium.     

二维层状结构十钒酸盐[K(H2O)2Ni(H2O)6]2[V10O28]的合成及性质(英)

A novel heteropoly compound, containing two kinds of coordinated cations, [K(H₂O)₂Ni(H₂O)₆]₂[V₁₀O₂₈], has been synthesized through routine process and characterized by elemental analyses, IR, ⁵¹V NMR and single crystal X-ray diffraction. It crystallizes in the triclinic system, space group P1 with a=0.87382(17) nm, b=1.075 4(2) nm, c=1.111 1(2) nm, α=65.10(3)°, β=75.01(3)°, γ=70.63(3)°, V=0.884 8(3) nm³ and Z=1. The X-ray analysis reveals that the two kinds of coordinated cations are linked by three shared coordinated water molecules, and K⁺ cations coordinate with ten oxygen atoms: five of which come from V₁₀O₂₈^6- anion, the other five from water molecules. The title compound exhibits extended 2D array building up of V₁₀O₂₈^6- groups connected by ten-coordinated K⁺ cations. The hexahydrated nickel cations Ni(H₂O)₆²⁺ lie in neat apposition to three adjacent V₁₀O₂₈^6- clusters. CSD: 413271.     

Synthesis and Crystal Structure of a 3-D Hydrogen-bonded Supramolecular Decavanadate Compound [Habo]6[V10O28]·2C3H7OH·2H2O

A new inorganic-organic hybrid supramolecular compound [Habo]6[V10O28]·solvents and its crystal structure was reported as follows: monoclinic, space group P21/n, a =11.419(9), b = 16.811(16), c = 15.521(12) (A), β= 102.98(2)°, V= 2903(4) (A)3, Z = 4, C15H46N3O19V5,Mr = 827.25, Dc = 1.893 g/cm3, λ(MoKα) = 0.71073 A,μ = 1.636 mm-1, F(000) = 1696, the final R =0.0696 and wR = 0.1361 for 4641 observed reflections with I ＞ 2σ(I). The compound is based on decavanadate clusters [V 1oO28]6-. The hydrogen bonding interactions among Habo+ cations, solvents and decavanadate clusters extend 1 into a three-dimensional supramolecular architecture.     

螺［异苯并呋喃－1（3H），9＇－（9H）－2＇－N，N－二苄胺基－6＇－二乙胺基占吨］－酮－3的合成及晶体结构研究

合成了螺［异苯并呋喃－１（３Ｈ），９＇－（９Ｈ）－２＇－Ｎ，Ｎ－二苄胺基－６＇－二乙胺基占吨］－酮－３，Ｃ＿（３７）Ｈ＿（３４）Ｎ＿２Ｏ＿３，单斜晶系，空间群Ｃｃ，晶体学参数为ａ＝１６．８２６（４），ｂ＝１０．６４８（４），ｃ＝１７．６１８（７），β＝９２．２５（２）°，Ｖ＝３１５４（２），Ｚ＝４，Ｍ＿ｒ＝５６６．７，Ｄ＿ｘ＝１．１９ｇ／ｃｍ３，Ｆ（０００）＝１２００。结构由直接法解出，偏离因子Ｒ＝０．０８０。分子由占吨和异苯并呋喃两部分组成Ｙ形结构，占吨部分相连的苄基的两个苯环位于占吨部分的两侧。     

Crystal Structure of 1 －Acetyl －2－［O－methylphenyl） phenyl－ thiophosphonyl］ Hydrazine

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅＯｆ１－Ａｃｅｔｙｌ－２－［Ｏ－ｍｅｔｈｙｌｐｈｅｎｙｌ）ｐｈｅｎｙｌ－ｔｈｉｏｐｈｏｓｐｈｏｎｙｌ］Ｈｙｄｒａｚｉｎｅ￥ＺｈａｎｇＬｉ－Ｊｕａｎ；ＬｉｕＸｉａｏ－Ｌａｎ；ＭｉａｏＦａｎｇ－Ｍｉｎｇ（Ｉｎｓｔｉｔｕｔｅ...     

Properties of a Tetrahomodioxacalix[6]arene Derivative

The synthesis and X-ray crystalstructure of a novel tetrahomodioxacalix[6]arenehexamethylester 2 arepresented. Preliminary investigations of alkali metal ioncomplexation showed that 2 is apoor extractant with selectivity for lithium.     

Synthesis and Crystal Structure of 8-methyl-5-phenyl-4-thia-6-aza-spiro [2.5] oct-5-en-7-ol

1 INTRODUCTION bacterical and so on[3]. Recently, we have reported a novel way to synthesize cyclopropane-annuated sul- Cyclopropane-containing compounds attract the fer or selenium heterocycles[4]. Herein we report the organic chemists for a long time because many of molecule structure of the title compound syhthesized them have biological activities in natural systems[1], by the tandem Michael-nucleophilic addition of thio- including cyclopropyl-amine, cyclopropylmethanols, benzamide an…     

(C_2H_(10)N_2)[H_3As_3O_(10)]的水热合成与晶体结构

采用中温水热方法合成了新化合物(C2H10N2)[H3As3O10].利用X射线粉末衍射仪、红外光谱仪、热重分析仪及X射线单晶衍射仪表征了产物的结构.结果表明:该化合物属于单斜晶系,P2(1)/n空间群;晶胞参数为a=0.808 3(6)nm,b=1.446 9(9)nm,c=0.892 0(8)nm,β=98.16°,V=1.032 7(14)nm3,Z=4,F(000)=864,R1=0.025 3,wR2=0.093 4.其化学式为C2H13As3N2O10,分子量Mr=449.90.该化合物是由有机胺阳离子支撑的第一个具有一维链状结构的砷酸盐化合物,相邻的砷酸盐链通过AAAA堆积方式形成三维拓扑扩展结构.