Ba7Fe6F32 · 2H2O: Original isolated trimers [Fe3F16]7− in a new defective jarlite-type compound

Ba₇Fe₆F₃₂ · 2H₂O was prepared from HF aqueous solution in a teflon bomb (Berghof) at 180°C. A partial exchange F^?/OH^? can be realized in more diluted HF medium and leads to Ba₇Fe₆F_32–x(OH)_x · 2H₂O. The compounds crystallize in the monoclinic system, space group C2/m (Z = 2) with a = 17.023(1) Å, b = 11.482(1) Å, c = 7.624(1) Å, β = 101.13(1)° for x = 0 and a = 17.036(2) Å, b = 11.489(1) Å, c = 7.620(2) Å, β = 101.48(1)° for x ≈? 5.3. The structures were determined from 2 256 and 1 343 independent reflections for x = 0 and x ≈? 5.3 respectively, collected with a Siemens AED2 four-circle diffractometer with the MoKα radiation (R = 0.0235 and R_w = 0.0240 for x = 0 and R = 0.0324 and R_w = 0.0335 for x ≈? 5.3). The structure, closely related to that of the Jarlite-type, is built up from isolated octahedra trimers [Fe₃F₁₆]^7?, connected together by Ba²⁺-cations. The location of anions and water molecules is discussed from bond valence calculations. Magnetic and Mössbauer studies are reported and discussed.     

The Crystal Structure of Pb8FeIIFeF24: an ordered Fluorite-like Compound

Pb₈Fe^IIFeF₂₄ is triclinic: a = 20.118(3) Å, b = 5.597(1) Å, c = 9.440(2) Å, α = 89.75(2)°, β = 105.79(2)°, α = 89.38(2)°, Z = 2. The structure is solved in the unconventional space group C1 , from X-ray single crystal data using 1 641 independent reflections (R = 0.048, R_w = 0.051). It is built up from the stacking of two subnetworks along the a axis: fluorite-like [Pb₈F₁₀]_n⁶ⁿ⁺ layers and infinite dimetallic [Fe^IIFeF₁₄]_n^6n? double-chains of corner-sharing octahedra running along the b axis.     

Preparation and crystal structure of Li6Zr2O7 and Li6Hf2O7

Li₆Zr₂O₇ was obtained by annealing an intimate mixture of LiOH · H₂O and freshly prepared ZrO₂ in a stream of argon. It is monoclinic: C2/c, a = 1 044.5(1), b = 598.9(1), c = 1 020.0(1) pm, β = 100.26(1)°, Z = 4, R = 0.016 for 1 218 F values and 55 variables. The structure is closely related to that of NaCl with an ordered distribution of the metal atoms on the sodium sites while the oxygen atoms occupy seven eighths of the chlorine positions. Li has square pyramidal, Zr octahedral oxygen coordination. The corresponding Hf compound is isotypic: a = 1 040.2(1), b = 596,2(1), c = 1 015.0(1) pm, β = 100.36(1)°. ⁷Li nuclear magnetic resonance spectra of this compound give no indication for a high mobility of the Li⁺ ions.     

Synthesis,Crystal Structure,and Properties of a New Lead Aluminum Fluoride Borate,Pb6AlB2O7F7

A new compound, Pb₆AlB₂O₇F₇, was synthesized from the PbF₂/B₂O₃ flux system, which is the first compound found in the PbF₂/Al₂O₃/B₂O₃ system. It crystallizes in the orthorhombic system, space group Cmca (No. 64) with unit cell parameters a = 11.649(7) Å, b = 18.300(11) Å, c = 6.394(4) Å, Z = 4. The crystal structure of Pb₆AlB₂O₇F₇ contains the group [Pb₆BO₁₁F₁₀] as basal building unit, which connects with each other forming two‐dimensional _∞[Pb₆BO₁₁F₁₀] layers, whereas aluminum atoms are filled in the interlayers. The IR spectrum further confirms the presence of BO₃ groups. The calculated band structures and the density of states of Pb₆AlB₂O₇F₇ suggest that its indirect gap is 2.968 eV. The DSC analysis and X‐ray diffraction technique prove that Pb₆AlB₂O₇F₇ is a congruent‐melting compound.     

4-甲氧基-6-甲基-7a-苯基苯并吡喃并[2,3-b]氮丙啶-7-酮的合成及晶体结构研究

通过5-甲基-7-甲氧基异黄酮与盐酸羟胺的缩合制得中间产物4-苯基-5-（2-羟基-4-甲氧基-6-甲基苯基）异恶唑,然后经过光异构化反应合成了4-甲氧基-6-甲基-7a-苯基苯并吡喃并[2,3-b]氮丙啶-7-酮,并采用IR,NMR,HRMS和单晶X-衍射分析对其结构进行了表征.单晶X-衍射分析结果表明：标题化合物属于单斜晶系,空间群P2（1）/n.在其晶体结构中,存在着氢键及芳香堆积作用,这些作用将标题化合物分子组装成了三维网络结构.     

Synthesis and Structure of the Double Oxide Pb6Re6O19

Pb₆Re₆O₁₉ oxide has been synthesized in a sealed evacuted silica tube and by high-pressure high-temperature technique. Its crystal structure, refined from X-ray powder data (a = 9.3162(1) Å, space group Pn3, R_I = 0.021, R_p = 0.067), is based on a three-dimensional network of Re₂O₁₀ groups linked together by corner sharing. The short Re–Re separation inside the Re₂O₁₀ groups (2.45 Å) indicates the presence of a metal-metal bonding.     

Pb3Al2F12: Crystal structure of a cyclo-fluoroaluminate related to Ba3Al2F12

Pb₃Al₂F₁₂ is a fluorometalate obtained in single-crystal form by hydrothermal synthesis. It crystallizes in the monoclinic system, space group P 2₁/n, with a = 9.435(6) Å, b = 9.610(5) Å, c = 10.100(9) Å, β = 90.59(5)°, V = 915.7(2) ų, Z = 4. The structure was solved from single crystal using 3 044 unique reflections (MoKα, λ = 0.71073 Å), R = 0.0463, R_w = 0.0465. The structure exhibits isolated tetrameric groups of octahedra encaged in a subnetwork of independent fluoride polyhedra and is related to that of Ba₃Al₂F₁₂. A discussion about the existence and the structure of A₃M₂F₁₂ compounds is given.     

The new structure type Gd3Ni7Al14

The crystal structure of Gd₃Ni₇Al₁₄ (trigadolinium heptanickel tetradecaaluminide) belongs to a family of two‐layer structures and can be described as an assembly of interpenetrating centred straight prisms. For the Ni atoms, trigonal prisms (Al₄Gd₂ and Al₆) are observed, the Al atoms are inside tetragonal (Ni₂Al₂Gd₄, Ni₂Al₄Gd₂, Al₄Gd₄, Ni₄Al₄ and Al₈) and pentagonal (Ni₄Al₆ and Al₁₀) prisms, while the Gd atoms are at the centres of pentagonal (Ni₄Al₆) and hexagonal (Ni₄Al₈) prisms. In each case, the true coordination polyhedron is a capped prism, also including atoms from the same layer. The structural features of Gd₃Ni₇Al₁₄ are similar to those of the intermetallides PrNi₂Al₃ and ZrNiAl. In all these structures, Ni‐centred trigonal prisms form infinite columns via common triangular faces. The columns share prism edges and form a three‐dimensional framework with six‐membered rings in the (001) plane in the case of the PrNi₂Al₃ and ZrNiAl types. In the case of Gd₃Ni₇Al₁₄, six‐membered rings are also observed, but only two‐thirds of the rings are interconnected via prism edges.     

A rare octacoordinated mononuclear iron(III) spin‐crossover compound: synthesis,crystal structure and magnetic properties

The chemistry of transition‐metal complexes with unusually high coordination numbers has been of interest because of their application in catalytic and biological systems. Deprotonation of the ionogenic tetradentate ligand 6,6′‐bis(1H‐tetrazol‐5‐yl)‐2,2′‐bipyridine [H₂bipy(ttr)₂] in the presence of iron(III) and tetra‐n‐butylammonium bromide, [n‐Bu₄N]Br, in solution resulted in the synthesis of a rare octacoordinated anionic mononuclear complex, tetra‐n‐butylammonium bis[6,6′‐bis(tetrazol‐1‐id‐5‐yl)‐2,2′‐bipyridine]iron(III) methanol hemisolvate dihydrate, (C₁₆H₃₆N)[Fe(C₁₂H₆N₁₀)₂]·0.5CH₃OH·2H₂O or [n‐Bu₄N][Fe{bipy(ttr)₂}₂]·0.5CH₃OH·2H₂O ( 1 ), which has been structurally characterized by elemental analysis, powder X‐ray diffraction (PXRD) and single‐crystal X‐ray diffraction. In 1 , the coordination sphere of the iron(III) ion is a distorted bis‐disphenoid dodecahedron, in which the eight coordination positions are occupied by eight N atoms from two independent tetradentate [bipy(ttr)₂]^2? anionic ligands, therefore forming the anionic [Fe{bipy(ttr)₂}₂]^? unit, with the negative charge balanced by a free [n‐Bu₄N]⁺ cation. An investigation of the magnetic properties of 1 revealed a gradual incomplete spin‐crossover behaviour below 150 K.     

雷公藤内脂四醇的晶体结构

雷公藤系卫矛科植物( Tripterygium wlfordii Hook. f) , 1972) 年,Kupechan从分得三种环二萜内酯类化合物,显示出较强的抗白血压病活性。为了寻找低毒有效的类似物,本文从雷公藤根皮乙醇提取物的氯仿溶出部分,反复经硅胶柱层析分理,得到一种新的环氧二萜酯;雷共藤内酯四醇(Tripletraolide)。在乙酸乙酯重结晶,得无色长极状晶体,m.p.258~260℃。经高分辩质谱确定其分子为C~0H~26O~8,M~r=394.2。     

新马兜铃内酯的晶体结构

从绵毛马兜铃的根茎中分离出一种新的倍半萜内酯, 它的分子式由高分辨质谱数据确定为C~1~5H~2~0O~2, 它的结构用单晶X射线衍射法测定, 晶体属三斜晶系, 空间群为P1, a=0.6275(3)nm, b=0.8057(4)nm, c=1.3622(6)nm; α=88.78(4)°,β=91.44(4)°, γ=105.20(4)°; Z=2.3107。     

Molecular and crystal structure of an ethanol solvate of 6-O-Methylerythromycin A

6-O-Methylerythromycin A (clarithromycin) ethanol solvate, C₃₈H₆₉NO₁₃·0.5(C₂H₅OH), crystallizes in orthorhombic space group P2₁2₁2₁ with a = 8.8459(14) ?, b = 14.616(2)?, c = 38.787(8) ?, V = 5014.9(15) ?³, Z = 4. The conformation of clarithromycin in the title compound is essentially the same as that in previously studied clarithromycin unsolvated crystal and its methanol solvate. However, the crystal structure of the title compound differs from the previously studied structures due to differences in hydrogen bonding which lead to different molecular packing arrangements. The lactone carbonyl oxygen atom is not involved in hydrogen bonding, which is consistent with IR data. Original Russian Text Copyright ? 2009 by Z. M. Jin, L. L. Ma, W. X. Wei, C. S. Lin, and W. Z. Li The text was submitted by the authors in English. Zhurnal Strukturnoi Khimii, Vol. 50, No. 1, pp. 192–196, January–February, 2009.     

异雷公藤内酯四醇的晶体结构

在Rigakui AFC5R四圆衍射仪上测定了异雷藤内酯四醇的晶体结构.晶体属单斜晶系的空间群P2~1,晶胞参数为:a=1.021(1),b=1,126(1),c=1.8209(9)nm,β=98.84(5)°V~c=2.09(3)nm^3,Z=4.表2     

The crystal structure of Solid Perrhenic Acid Monohydrate

Solid perrhenic acid monohydrate has been characterized by X-ray single crystal structure analysis (300 K). HReO₄ · H₂O, M_r = 269.23, tetragonal, I4₁/a, Scheelite-type (CaWO₄), a = 5.8320(2) Å, c = 12.9384(6) Å, V = 440.06(5) ų, Z = 4, D_x = 4.063 g cm^?3, X-ray wavelength λ (MoKα) = 0.71069 Å The structure consists of [ReO₄]^?-tetrahedra and oxonium ions linked by hydrogen bridges to form a three-dimensional network.     

C3N6H6(H3BO3)2的合成及晶体结构

以三聚氰胺和硼酸为原料在水溶液中反应合成出了一种新的BCN化合物先驱体C3N6H6(H3BO3)2。XRD表征结果表明三聚氰胺和硼酸的最佳配比为1∶3(物质的量比)。用单晶X-射线衍射分析法测定了该化合物的晶体结构。该化合物属单斜晶系,空间群为P21/C,晶胞参数为a=0.3597(7)nm,b=2.0105(4)nm,c=1.4112(3)nm,α=90,°β=92.07(3),°γ=90,°V=1.0199(3)nm3,Z=4,D c=1.627g.cm-3,μ(MoKα)=0.144mm-1,F(000)=520。晶体结构经全矩阵最小二乘法修正,最终可靠因子R1=0.0519,wR2=0.1361。该化合物是由C3N6H6分子和H3BO3分子通过氢键加合组装形成的三维超分子结构化合物。     

Zwei neue Sulfidchloride der Lanthanide: Synthese und Kristallstruktur von Pr7S6Cl9 und Nd7S6Cl9

Two Novel Sulfide Chlorides of the Lanthanides: Synthesis and Crystal Structure of Pr₇S₆Cl₉ and Nd₇S₆Cl₉ The reactions of the elemental lanthanides (M = Pr and Nd, resp.) with sulfur and the respective trichlorides (MCl₃) in evacuated silica tubes (850 °C, 7 d) yield single-phase sulfide chlorides of the composition M₇S₆Cl₉ when appropriate molar ratios (4 : 6 : 3) of the reactants (M : S : MCl₃) are used. A slight excess of trichloride as a flux promotes the formation of lath-shaped transparent single crystals (Pr₇S₆Cl₉: pale green, Nd₇S₆Cl₉: pale violet) which prove to be water soluble and sensitive to hydrolysis. The crystal structure was determined from X-ray single-crystal data taking Nd₇S₆Cl₉ (monoclinic, P2/c (no. 13); a = 2425.0(9), b = 664.2(2), c = 691.8(2) pm, β = 97.43(3)°, Z = 2; R = 0.060, R_w = 0.048) as an example. According to Guinier powder data, Pr₇S₆Cl₉ crystallizes isotypically with a = 2441.6(9), b = 669.1(2), c = 696.3(2) pm, and β = 97.74(3)°. Thus four crystallographically independent cations (M³⁺) are present, each except for M2 coordinated by four S^2– but differing in the number of their next Cl^– neighbors. The figures of coordination are completed by four Cl^– about M1 (square antiprism, CN = 8) and by three Cl^– each about M3 and M4 (monocapped trigonal prisms, CN = 7, 2 Ç ). In contrast, M2 is coordinated by only two S^2– but five (plus one) Cl^– as bicapped trigonal prism (CN = 7 + 1). Eight crystallographically different anions, although indistinguishable by X-ray diffraction, exhibit coordination numbers of four (3 Ç S^2– and 1 Ç Cl^–) and three (4 Ç Cl^–) with respect to the cations. So PbO-analogous layers of the composition ²_∞{[(S6/7Cl_1/7)M_4/4]₇}⁸⁺ parallel (010) are formed, consisting of 6/7 of S^2– and only 1/7 of Cl^– as centering anions for the edge-shared (M³⁺)₄ tetrahedra for reasons of charge neutrality. These cationic layers are held together by alternatingly sheathed layers of Cl^– with only threefold coordinated anions.     

A new CoII complex of diniconazole: synthesis,crystal structure and antifungal activity

A new Co^II complex of diniconazole, namely diaqua[(E)‐(RS)‐1‐(2,4‐dichlorophenyl)‐4,4‐dimethyl‐2‐(1H‐1,2,4‐triazol‐1‐yl‐κN⁴)pent‐1‐en‐3‐ol]cobalt(II) dinitrate dihydrate, [Co(C₁₅H₁₇Cl₂N₃O)₃(H₂O)₂](NO₃)₂·2H₂O, was synthesized and characterized by elemental analysis, IR spectroscopy and single‐crystal X‐ray diffraction. Crystal structural analysis shows that the centrosymmetric Co^II cation is coordinated by four diniconazole ligands and two water molecules, forming a six‐coordinated octahedral structure. There are also two free nitrate counter‐anions and two additional solvent water molecules in the structure. Intermolecular O—H...O hydrogen bonds link the complex cations into a one‐dimensional chain. In addition, the antifungal activity of the complex against Botryosphaeria ribis, Gibberella nicotiancola, Botryosphaeria berengriana and Alternariasolani was studied. The results indicate that the complex shows a higher antifungal activity for Botryosphaeria ribis and Botryosphaeria berengriana than diniconazole, but a lower antifungal activity for Gibberella nicotiancola and Alternariasolani.     

Rheniumselenidtelluride Re2SexTe5–x: Die Struktur von Re6Se8Te7

Rhenium Selenidetellurides Re₂Se_xTe_5–x: The Structure of Re₆Se₈Te₇ Well-crystallized rhenium selenidetellurides of the Re₂Te₅-type structure were prepared from the elements in evacuated sealed quartz glas tubes at 1 130 K within 14 d. The orthorhombic lattice parameters of the phases shrink with increasing selenium content from a = 1 304.9(1) ? 1 255.8(2) pm, b = 1 297.5(1) ? 1 260.0(2) pm, and c = 1 425.1(1) ? 1 408.2(1) pm. The phase width ends at composition Re₂Se_2.7Te_2.3. An X-ray structure analysis of a crystal of composition Re₆Se₈Te₇ was performed. Selenium and tellurium atoms differ structurally completely: Whereas the selenium atoms are separated within distorted octahedral [Re₆Se₈] clusters, the tellurium atoms form homonuclear bonded bicyclic [Te(Te₃)₂] units. They also link the clusters which are arranged according to the motif of a cubic closest packing.