Synthesis and crystal structure of CuZrTiO5—A new crystal structure type

A new compound, CuZrTiO₅, was synthesized as strongly pleochroic green crystals from the oxides between 995 and 1010 °C, 1 atm. Its crystal structure was determined by single crystal XRD, resulting in R (F²>2σ(F²))=0.032 and wR (all data)=0.079). CuZrTiO₅ is orthorhombic, space group P2₁2₁2₁, a=3.5871(3) Å, b=6.6968(4) Å, c=14.6679(9) Å, V=352.35(4) Å³, Z=4. The structure is topologically similar to In₂TiO₅ but differs in space group and cation coordination. CuZrTiO₅ has relatively regular TiO₆ polyhedra, but coordination is 7+1 for Zr, and 4+2 for Cu due to the Jahn-Teller effect. Ordering of the long Cu-O bonds causes reduction in symmetry relative to In₂TiO₅. Layers of Cu alternate with Ti+Zr on (001), giving rise to a distinct cleavage. Bond valence sums on Ti and Zr are far from ideal, which appears due to the limited ability of this structural topology to avoid close next-nearest neighbour distances.     

Synthesis and crystal structure of EuBi2

The new hypervalent binary phase EuBi₂ was obtained from high temperature solid-state reactions of the pure metal elements in welded Ta tubes under argon atmosphere. Its structure was established by single-crystal X-ray diffraction. The title compound crystallizes in the tetragonal space group I4₁/amd (No. 141) with cell parameters of , and Z=8. The structure of EuBi₂ is isotypic with HfGa₂ and features 1D Bi⁻ zigzag anionic chains along both a- and b-axes and 2D Bi⁻ square sheets normal to c-axis. It can be formulated as Eu²⁺(Bi)_chain⁻(Bi)_square⁻.     

Synthesis and crystal structure of MgB12

Single crystals of MgB₁₂ were synthesized from the elements in a Mg/Cu melt at 1600 °C. MgB₁₂ crystallizes orthorhombic in space group Pnma with , and . The crystal structure (Z=30, 5796 reflections, 510 variables, R₁(F)=0.049, wR₂(I)=0.134) consists of a three dimensional net of B₁₂ icosahedra and B₂₁ units in a ratio 2:1. The B₂₁ units are observed for the first time in a solid compound. Mg is on positions with partial occupation. The summation reveals the composition MgB_12.35 or Mg_0.97B₁₂ , respectively. This is in good agreement with the value of MgB_11.25 as expected by electronic reasons to stabilize the boron polyhedra and .     

Synthesis and crystal structure of SnSbBiS4

The quaternary compound SnSbBiS₄ formed in the SnSb₂S₄-SnBi₂S₄ system at the ratio SnSb₂S₄: SnBi₂S₄ = 1: 1 was studied for the first time by various physicochemical methods over a wide temperature interval. Single crystals of SnSbBiS₄ were prepared by chemical transport. The unit cell parameters of SnSbBiS₄, which crystallized in the hexagonal system (a = 15.52 ?, c = 3.81 ?), were determined.     

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.     

Synthesis, crystal structure, and electronic structure of RbVSe2

RbVSe₂ has been synthesized at 773 K through the reaction of V and Se with a Rb₂Se₃ reactive flux. The compound crystallizes in the orthorhombic space group D_2h²⁴-Fddd with 16 formula units in a cell of dimensions , , and at . The structure possesses infinite one-dimensional chains of edge-sharing VSe₄ tetrahedra separated from the Rb⁺ ions. These chains distort slightly to chains. The V-V distance within these chains is 2.8362(4) Å. First-principles total energy calculations indicate that a non-magnetic configuration for the V³⁺ cations is the most stable.     

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.     

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.     

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。     

Synthesis of cis-3,4-dibromopyrrolidine and its crystal and molecular structure

Synthesis and structural studies of 3,4-dibromopyrrolidine hydrochloride are reported. The conformation of the dibromopyrrolidine ring is a slightly deformed envelope with ΔC_s(3–4) = 4.03°. The Br atoms have cis conformation. Short Cl?H—N hydrogen bonds link the 3,4-dibromopyrrolidine cations and Cl^? anions along the a-axis.     

三苯基锡4－吡啶甲酸酯的合成、性质和晶体结构

用三苯基氯化锡与4-吡啶甲酸钠反应，合成了三苯基锡4-吡啶甲酸酯，并进行 了红外光谱、核磁共振氢谱及质谱表征。X射线单晶衍射表明，化合物属单斜晶系 ，空间群P21，晶胞参数：a=1.6629（3）nm，b=104987(4)nm，c=2.4318(7)nm，β =90.040（5）°，Z=8,Dc=1.1529g/cm^3，R1=0.0543，wR2=0.1086。化合物的晶体 是由两个结构相似但键长和键角不同的独立分子所组成，且每个分子含有两种化学 环境不同的锡原子。它们通过4-吡啶甲酸配体的氮原子桥联，形成五配位三角双锥 构型的一维无限链聚合物。     

一种具有Keggin结构的固体杂多酸的合成及其晶体结构

以钨酸钠、氯化钴、醋酸钴及1,3-丙二胺为原料,利用水热合成法制备了一种具有Keggin结构的杂多酸H6[CoW12O40].2.5H2O;利用单晶X射线衍射分析了产物的晶体结构.结果表明,产物中的过渡金属Co2+离子作为中心原子与4个氧原子形成CoO4四面体;CoO4四面体被4个W3O13金属簇包围,与每个W3O13金属簇之间通过共顶点连接而形成[CoW12O40]6-阴离子;六个氢离子作为抗衡阳离子,最终形成固体杂多酸分子.     

Synthesis and crystal structure of dimeric 2,4,6-triphenylphenylbismuthdichloride

Reaction of BiCl₃ with one equivalent of 2,4,6-triphenylphenyllithium in toluene results in the formation of crystalline 2,4,6-triphenyl-phenylbismuthdichloride toluene disolvate (1). The crystal structure of 1 has been determined by X-ray diffraction. In spite of the extremely bulky substituents at the bismuth atom, complex 1 is dimeric in the solid state with intramolecular Bi-Cl bond lengths of 2.530(1) Å and bridging Bi-Cl of 3.074(1) Å.     

Synthesis and Catalytic Activities of Porphyrin‐Based PCP Pincer Complexes

2,18‐Bis(diphenylphosphino)porphyrins undergo peripheral cyclometalation with group 10 transition‐metal salts to afford the corresponding porphyrin‐based PCP pincer complexes. The porphyrinic plane and the PCP‐pincer unit are apparently coplanar, with small strain. The catalytic activities of the porphyrin‐based pincer complexes at the periphery were investigated in the allylation of benzaldehyde with allylstannane and in the 1,4‐reduction of chalcone to discover the electronic interplay between the inner metal and the outer metal in catalysis.