The crystal structure of ammonium β-octamolybdate pentahydrate

X-ray structure analysis (film data, R = 0.080 for 1568 reflections) has confirmed the structure of the anion in (NH₄)₄[Mo₈O₂₆], 5H₂O, deduced by Lindqvist in 1950 from the Mo coordinates alone. The compound is triclinic, P$\text{1}$, a = 9.769(16), b = 9.832(13), c = 7.848(11) Å, α = 99.11(4), β = 101.03(11), γ = 97.40(4)°, Z = 1. Eight MoO₆ octahedra share edges in a compact grouping, with short terminal MoO bonds (1.69 to 1.75 Å), longer bonds (1.88–2.00 Å) to bicoordinate O atoms, and long bonds (2.18–2.39 Å) to multiply-shared interior atoms.     

The crystal structure of tetraphenylphosphonium tetracyanohydroxooxorhenium(V)

Summary The crystal structure of (PPh₄)₂[ReO(OH)(CN)₄]·5H₂O has been determined from three-dimensional x-ray diffraction data. The light brown crystals are monoclinic, space group P2₁/n, with cell dimensionsa=16.753(2),b=19.928(2),c=15.338(2) Å and =101,894(1)°,z=4, D_m=1.45(1) g cm^–3. The anisotropic refinement of the 6088 observed reflections converged to R=0.077.The [ReO(OH)(CN)₄]^2– ion has a distorted octahedral geometry. Bond distances: Re =1.70(1), Re–OH=1.90(1) and ReC_av=2.12(2) Å. The Re atom is displaced by 0.08 Å out of the plane formed by the four carbon atoms towards the terminal oxo ligand.     

溴化四苯基膦合成的研究

研究了以三苯基膦和溴苯为原料用NiCl2为催化剂定向合成溴化四苯基膦的原子经济性绿色合成反应,系统的考察了催化反应过程中催化剂、反应温度、溶剂、反应时间等因素对产物收率的影响,同时敢讨论了催化剂回收和产物提纯的工艺条件,优化结果表明采用无毒害正辛醇溶剂,回流温度为195℃,反应6h,产物收率可达89%以上。在产物收率和有利环境友好方面的结果尚未见文献报道。     

Preparation and crystal structure of tetraphenylphosphonium triiodotetrabromide [PPh4][I3Br4

Tetraphenylphosphonium triiodotetrabromide [PPh4][I3Br4] is obtained by the reaction of tetraphenylphosphonium bromide with iodine monobromide. It is the first example of an iodine rich, seven-membered polybromide. [PPh4][I3Br4] crystallizes triclinic in the space group P1 with a = 10.947(1) A, b = 11.945(1) A, c = 12.896(1) A, alpha = 66.80(1) degrees, beta = 77.21(1) degrees, gamma = 85.73(1) degrees, and two formula units per unit cell. The final R indices [I > 4 sigma(I)] are R1 = 0.0362 and wR2 = 0.0944.     

Synthesis and crystal structure of diferrocenylmethoxyethylamine

The reaction of diethanolamine with diferrocenylmethyl carbonium (2) that was generated by diferrocenylmethanol (1) treated with BF₃ in CH₂Cl₂ provided the synthesis of title compound diferrocenylmethoxyethylamine (3). The structure of 3 was determined by the X-ray diffraction (XRD) with crystal data: monoclinic P2₁/n space group and a=5.8419(14) Å, b=13.572(3) Å, c=23.839(6) Å, α=90°, β=91.827(5)°, γ=90°, V=1889.2(8) Å³, Z=4, D _c =1.558 mg·m^?3, μ=1.548 mm^?1, F(000)=920. The intra- and inter-molecular H bonding modes in 3 were demonstrated both in molecular crystal structure and IR spectral characterization.     

Synthesis and crystal structure of poly-trivinyltinferrocenoate

Binuclear complexes of formula C₅H₁₅FeC₅H₄COOSn(CHCH₂)₃ (I), C₅H₅FeC₅H₄COOSnPh₃ (II) and Ph₃GeCOOSnPh₃ (III) have been prepared and characterized by IR spectra. The polymeric structure of solid C₅H₅FeC₅H₄COOSn(CHCH₂)₃ has been established by X-ray crystallography. The crystals are monoclinic, space group P2₁/a, with a 15.105(5), b 10.030(4), c 11.402(4) Å, and β 104.06(4)°. In this compound the tin atoms are five-coordinate trigonal bipiramidal, with the vinyl groups equatorial and two apical oxygen atoms from bridging carboxylato groups. The resulting structure is a linear polymer with SnO bond lengths of 2.12 and 2.42 Å. The spectra indicate that similar polymeric structure exist also for compounds II and III in the solid state, whereas an equilibrium monomer ? dimer seems to be present in CHCl₃ solution for the compound III.     

Synthesis and crystal structure of azafulgides

Two azafulgides were synthesized and their crystal structures determined by a single crystal X-ray diffraction analysis. The substances crystallized in the following symmetries and cell parameters. C₂₃H₁₉NO₃( 2 ): triclinic space group P&1bar; with a = 7.243(2). b = 10.981(6) and c = 12.672(8)Å, α = 80.40(5)°, β = 75.58(4)° and γ = 77.32(3)° Z = 2; C₁₉H₁₉NO₃( 1 ): orthogonal space group C_2v⁹-Pmc2₁ with a = 8.079(8), b = 12.752(9) and c = 15.752(13)Å, Z=4. The calculated densities are 1.26 and 1.27 g/cm³ respectively for 2 and 1 . The crystal structures were determined by direct methods. The least-squares refinement led to R values of 0.044 and 0.058 for 2 and 1 for 2738 and 952 reflections with I > 3σ-(I) respectively.     

Disordered crystal structure of 4,7,13,16,21,24-hexaoxa-1-aza-10-azoniabicyclo[8.8.8]hexacosane isocyanurate

X-ray spectral analysis has been applied to study the crystal structure of 4,7,13,16,21,24-hexaoxa-1-aza-10-azoniabicyclo[8.8.8]hexacosane isocyanurate of an unusual composition: [H_1.2(Crypt-222)]^1,2+ · [H_0.8(Crypt-222)]^0.8+·2(C₃H₂N₃O₃)^? (I). The structure of I (space group C2/c, a = 37.840 Å, b = 13.760 Å, c = 19.456 Å, β = 91.21°, Z = 8) was solved by a direct method and refined by the full-matrix least-squares technique in the anysotropic approximation up to R = 0.119 over 6500 independent reflections measured (autodiffractometer CAD-4, λ-MoK _α). The structure of I has two independent cations of 2.2.2-cryptand linked by the proximate pseudo-center of inversion and they have a rare conformation of exo-exo type, in which H atom or lone pair at both their node atoms N are directed outward their cavity. In the structure of I, all H atoms at N atoms of cations and half of H atoms of isocyanurate anions are disordered and have the populations of positions 0.7, 0.5, and 0.3. There is a developed system of interionic hydrogen bonds in the crystal structure of I.     

Synthesis and N-methylation of tetrabutylammonium isocyanurate

A simple and efficient method for the synthesis of ammonium salt of isocyanuric acid is set out. This process is based on the direct addition of the corresponding hydroxide to isocyanuric acid. This salt exhibits several interesting properties. Its alkylation by iodomethane in various solvents is demonstrated and leads to various substituted isocyanurate derivatives.     

Synthesis and crystal structure of maleopimaric acid

The title compound maleopimaric acid was synthesized by a Diels-Alder reaction between maleic anhydride and Pinus elliottii engelm oleoresin at room temperature and it was characterized by single crystal X-ray diffraction. The white crystals crystallized in the orthorhombic system, space group P2(12121) with cell dimensions: a = 7.6960 (15) A, b = 11.851 (2) A, c = 24.577 (5) A, alpha = 90 degrees, beta = 90 degrees, gamma = 90 degrees, V = 2241.6(8) A(3), and R(1) = 0.0716, wR(2) = 0.1975. The two fused and unbridged cyclohexane rings form a trans ring junction with chair conformation with two methyl groups in axis positions, the anhydride ring is planar. Crystal water existed in the molecular and stabilized the structure through intermolecular hydrogen bonds.     

Synthesis and crystal structure of AgInO2

Single crystals of AgInO₂ were obtained by hydrothermal reaction of Ag₂O and In₂O₃ in NaOH at elevated temperature and O₂ pressure. The delafossite type crystal structure was refined using single crystal X-ray diffractometer data (R3m; a_hex = 327.68(7), c_hex = 1887.8(7) pm; Z = 3; R_w = 0.022; 171 independent structure factors). InO and AgO bond distances are 217.4(4) and 207.6(8) pm, respectively. Structure and bond characteristics are discussed.     

Synthesis and crystal structure of methylammonium dicitratoborate

Methylammonium dicitratoborate CH₃NH₃[(C₆H₆O₇)₂B] (I) was synthesized for the first time. The crystal structure of the compound was studied by X-ray crystallography. Crystals of I are triclinic, space group P \(\bar 1\), a = 8.9726(3) Å, b = 10.1039(3) Å, c = 10.7231(4) Å, α = 66.894(1)°, β = 85.347(1)°, γ = 84.991(2)°, V = 889.57(5) ų, Z = 2, ρ_calcd = 1.580 g/cm³. Crystals of I are built up from large dicitratoborate anions with a spiran structure and methylammonium cations. The crystals have a layered structure. A hydrogen-bond system is formed by seven independent contacts O(N)-H?O.     

Synthesis and crystal structure of 29,30-dibromoallobetulin

The bromination of betulin with bromine was descibed. The reaction in chloroform proceeded smoothly to form 29,30-dibromoallobetulin in 80% yield. __________ Translated from Khimiya Prirodnykh Soedinenii, No. 2, pp. 153–155, March–April, 2006.     

N-二茂铁甲基乙酰胺的合成及其晶体结构

标题化合物(C13H15FeNO)由二茂铁甲酰肟与乙酸乙酯经一锅煮方法制得,其结构通过元素分析,1HNMR,13CNMR,IR和单晶X-射线衍射法确定,化合物具有一维无限链状结构。其晶体属正交晶系,Pbca空间群,M r:257.11,a=9.6101(19),b=9.2313(18),c=25.869(5),v=2295.0(8)3,z=8,D c=1.488Mg.m-3,u=0.71073,F(000)=1072,最终偏离因子为R=0.0517,wR=0.0877。