氯化二(羟胺根)·(羟胺—O)·水合氧钒(Ⅴ)[VO·(NH_2O)_2·(NH_3O)·H_2O]Cl的晶体结构

调节硫酸氧钒与盐酸羟胺溶液至pH～4制得的题目晶体属空间群P2_1/n,晶胞参数a=8.201,b=8.597,c=9.947A,β=93.00°,Z=4.结构解出精修后R因子为0.069.结果表明,不对称单位中二个羟胺根以侧接态与VO~(3+)配位,另一羟胺取端接态以O占据V的第五赤道配位位置,配位水处于氧钒基强键反位,Cl~-则在配阳离子界外以平衡电荷,晶体对的化学式确证为[(VO~(3+))(NH_2O~_)_2(NH_3O)(H_2O)][Cl~-]     

Syntheses and structures of p-HOOCC6F4COOH · H2O (H2L · H2O) and luminescent coordination polymers [Tb2(H2O)4(L)3 · 2H2O] n and Tb2(Phen)2(L)3 · 2H2O

Compounds p-HOOCC₆F₄COOH · H₂O (H₂L · H₂O), [Tb₂(H₂O)₄(L)₃ · 2H₂O] _n (I), and Tb₂(Phen)₂(L)₃ · 2H₂O (II) are synthesized. According to the X-ray structure analysis data, the crystal structure of H₂L · H₂O is built of centrosymmetric molecules H₂L and molecules of water of crystallization. The crystal structure of compound I is built of layers of coordination 2D polymer [Tb₂(H₂O)₄(L)₃] _n and molecules of water of crystallization. The ligands are the L^2? anions performing both the tetradentate bridging and pentadentate bridging-chelating functions. The coordination polyhedron TbO₉ is a distorted three-capped trigonal prism. Acid H₂L manifests photoluminescence in the UV region (??_max = 368 nm). Compounds I and II have the green luminescence characteristic of the Tb³⁺ ions, and the band with ??_max = 545 nm (transition ⁵ D ₄?? ⁷ F ₅) is maximum in intensity. The photoluminescence intensity of compound II is higher than that for compound I.     

Thulium(III) trifluoroacetates Tm(CF3COO)3 · 3H2O and Tm2(CF3COO)6 · 2CF3COOH · 3H2O: Synthesis and crystal structure

Thulium trifluoroacetate compounds have been synthesized, Tm(CF₃COO)₃ · 3H₂O (I) and Tm₂(CF₃COO)₆ · 2CF₃COOH · 3H₂O (II). The structure of I has been refined by the Rietveld method on the basis of the structural data for Cd(CF₃COO)₃ · 3H₂O. The structure of II has been solved in a single-crystal X-ray diffraction study. Compound I has been studied by thermal analysis. Crystals of I and II are monoclinic: for I a = 9.062(2) Å, b = 18.678(3) Å, c = 9.687(2) Å, β = 113.93(1)°, Z = 2, space group P2₁/c, R ₁ = 0.062; for II a = 8.560(4) Å, b = 19.866(5) Å, c = 20.813(7) Å, β = 101.69(4)°, Z = 8, space group C2/c, R ₁ = 0.0392. In the molecular structure of I, thulium atoms are bonded in pairs through four bridging trifluoroacetate anions to form dimers. The coordination polyhedron of the thulium atom also includes the three O atoms of the water molecules and the O atom of the monodentate trifluoroacetate group; the coordination number of the thulium atom is eight. In the chain structure of II, there are two crystallographically independent thulium atoms with coordination numbers 8 and 9. The coordination polyhedra of the Tm(1) and Tm(2) atoms are a distorted monocapped tetragonal antiprism and a distorted tetragonal antiprism, respectively. The Tm-O bond lengths are in the range 2.28(1)–2.85(2) Å. The thulium atoms are bound into chains through carboxylate groups. These chains are linked into layers through hydrogen bonds.     

Synthesis,Structure and Characterization of Three Metal Molybdate Hydrates: Fe(H2O)2(MoO4)2·H3O,NaCo2(MoO4)2(H3O2)and Mn2(MoO4)3·2H3O

Three metal molybdate hydrates,Fe(H2O)2(MoO4)2·H3O(FeMo),NaCo2(MoO4)2(H3O2)(CoMo)and Mn2(MoO4)3·2H3O(MnMo),were synthesized by the mixed-solvent-thermal methods and characterized by singlecrystal X-ray...     

Synthesis and structure of [Cr3O(CH3COO)6(H2O)3][UO2 (CH3COO)3] · 3H2O

Crystals of [Cr₃O(CH₃COO)₆(H₂O)₃][UO₂(CH₃COO)₃]·3H₂O (I) were synthesized for the first time and studied by X-ray crystallography. The crystals of I are orthorhombic: a = 8.3561(3) ?, b = 16.8421(5) ?, c = 25.7448(9) ?, V = 3623.2(2) ?³, space group P2₁2₁2₁, Z = 4, R = 0.0409. The structure is composed of trinuclear [Cr₃O(CH₃COO)₆(H₂O)₃]⁺ complexes and mononuclear [UO₂(CH₃COO)₃]^? complexes classified with crystal-chemical groups A₃M³B ₆ ² M ₃ ¹ (A = Cr³⁺, M³ = O^2?, B² = CH₃COO^?, M¹ = H₂O) and AB ₃ ⁰¹ (A = UO ₂ ²⁺ , B⁰¹ = CH₃COO^?), respectively. The complexes are bound to each other by electrostatic interactions and hydrogen bonds involving outer-sphere water molecules. The results of IR spectroscopic study of I are in good agreement with the structural data for the crystal.     

[Gd(Gly)3(H2O)2]Cl3·H2O的合成与晶体结构

氯化钆;甘氨酸;固态配合物;[Gd(Gly)3(H2O)2]Cl3·H2O的合成与晶体结构     

A Novel Copper Ammonium Diphosphate--Dimorphic Cu 3 (NH 4 ) 2 (P 2 O 7 ) 2 ·3H 2 O

This article deals with the insoluble compounds, formed in CuSO 4 -(NH 4 ) 4 P 2 O 7 -H 2 O system. The solutions were analyzed by means of chemical analysis, the precipitate--by means of x-ray diffraction, chemical and thermal analysis, and FTIR spectroscopy. We have established that at least three poorly soluble compounds can form in the system CuSO 4 -(NH 4 ) 4 P 2 O 7 -H 2 O. Their chemical formulae are Cu 2 P 2 O 7 ;5H 2 O and polymorphic Cu 3 (NH 4 ) 2 (P 2 O 7 ) 2 ;3H 2 O. The first modification is most stable when |Cu + P 2 O 7 | = 0.25 M ( n = 1.0), and, in a matter of days, Dimorph A transforms to Dimorph B, which has not been described in any publications.     

[Co(Phen)2(H2O)2](HL)NO3·3H2O的合成及晶体结构

在水溶液中,以邻菲咯啉、丁二酸与硝酸钴为原料合成了一个新的超分子化合物[Co(Phen)2(H2O)2].(HL).(NO3).3H2O,并经元素分析、IR、X射线单晶衍射分析进行了结构表征.结构分析表明,晶体属三斜晶系,P1-空间群,a=0.968 0(2)nm,b=1.370(3)nm,c=1.394 9(3)nm,α=61.714(3)°,β=71.495(4)°,γ=79.575(4)°,V=1.543 7 nm3,Z=2,ρ=1.481 g/cm3,C28H31CoN5O12,Mr=688.51,F(000)=714 andμ=0.627 mm-1,7 754个独立衍射点中,5 428个可观察点满足I≥2σ(I),R1=0.074 5,wR2=0.210 7.晶体中[Co(Phen)2(H2O)2]2+通过π-π相互作用堆积成二维层状结构,层间通过氢键作用构成三维超分子.     

Crystal structures of Co3(SeO3)3·H2O and Ni3(SeO3)3·H2O,two new isotypic compounds

Summary The crystal structures of the new, hydrothermally synthesized, isotypic compounds Co₃(SeO₃)₃·H₂O and Ni₃(SeO₃)₃·H₂O were determined by direct and Fourier methods and refined toR _w=0.023, 0.032 using single crystal X-ray data up to sin/=0.81 Å^–1 [space group P ,a=8.102 (2), 7.986 (3) Å;b=8.219 (2), 8.133 (3) Å;c=8.572 (2), 8.422 (3) Å, =69.15 (1), 69.50 (1)°; =62.88 (1), 62.50 (1)°; =67.23 (1), 67.64 (1)°;Z=2]. The structures are built up from [Me ₅(SeO₃)₆·2H₂O]^2– sheets containing three crystallographically different types of octahedrally coordinatedMe ²⁺ and trigonal pyramidal coordinated Se⁴⁺ atoms, respectively. These sheets are linked only by a fourth type ofMe ^2+[6] atom. All coordination polyhedra deviate significantly from their ideal shapes, bond lengths within the extremly distortedMe(4)O₆ polyhedra range from 1.983 (2) Å to 2.403 (2) Å in Co₃(SeO₃)₃·H₂O and from 1.987 (4) Å to 2.301 (3) Å in the Ni compound, O-Se-O bond angles were found between 92.8 (2)° and 104.9 (1)°. Hydrogen bond lengths are 2.802 (3)Å and 2.600 (4)Å in the Co compound, and 2.762 (6) Å and 2.561 (6) Å in Ni₃(SeO₃)₃·H₂O. The latter is one of the shortest known hydrogen bonds donated by a water molecule.

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Die Kristallstrukturen von Co₃(SeO₃)₃·H₂O und Ni₃(SeO₃)₃·H₂O, zwei neue isotype Verbindungen

Zusammenfassung Die Kristallstrukturen der neuen, hydrothermal synthetisierten, isotypen Verbindungen Co₃(SeO₃)₃·H₂O und Ni₃(SeO₃)₃·H₂O wurden mit direkten und Fourier-Methoden bestimmt und unter Verwendung von Einkristallröntgendaten bis sin/=0.81 Å^–1 aufR _w-Werte von 0.023, 0.032 verfeinert [Raumgruppe P ,a=8.102 (2), 7.986 (3) Å;b=8.219 (2), 8.133 (3) Å;c=8.572 (2), 8.422 (3) Å, =69.15 (1), 69.50 (1)°; =62.88 (1), 62.50 (1)°; =67.23 (1), 67.64 (1)°;Z=2]. Die Strukturen werden von [Me ₅(SeO₃)₆·2H₂O]^2– Schichten aufgebaut, die je drei kristallographisch unterschiedliche Arten von oktaedrisch koordiniertenMe ²⁺ und trigonal pyramidal koordinierten Se⁴⁺ Atomen enthalten. Diese Schichten sind nur durch eine vierte Art vonMe ^2+[6] Atomen verknüpft. Alle Koordinationspolyeder weichen deutlich von ihren Idealformen ab, Bindungslängen in den extrem verzerrtenMe(4)O₆ Polyedern variieren zwischen 1.983 (2) Å und 2.403 (2) Å in Co₃(SeO₃)₃·H₂O und zwischen 1.987 (4) Å und 2.301 (3) Å in der Ni-Verbindung, O-Se-O-Bindungswinkel liegen zwischen 92.8 (2)° und 104.9 (1)°. Wasserstoffbrückenlängen sind 2.802 (3) Å und 2.600 (4) Å in der Co-Verbindung, und 2.762 (6) Å und 2.561 (6) Å in Ni₃(SeO₃)₃·H₂O. Letztere ist eine der kürzesten bekannten Wasserstoffbrücken eines Wassermoleküls.

     

[La(Phen)2(NO3)2(H2O)2]ClO4·2Phen·H2O的合成与晶体结构

合成了[La(Phen)2(NO3)2(H2O)2]ClO4·2Phen·H2O(1,化学式为C48H38ClN10O13La,Mr=1137.24,Phen=邻菲咯啉),经X-射线单晶衍射测定其晶体结构属于三斜晶系,Pī空间群,a=11.250(4),b=13.364(4),c=16.327(5)(。A),α=103.042(6),β=90.327(6),γ=99.567(6)°,V =2355.8(12)(。A)3,Z = 2,Dc =1.603g·cm-3,F(000)=1148,μ=1.042mm-1,R=0.0569,wR= 0.1064.1由 [La(Phen)2(NO3)2(H2O)2]+ 阳离子,ClO-4阴离子,两个共结晶的Phen分子和1个H2O分子构成.内界的中心金属La(III)离子为十配位的变形的双帽四方反棱柱体,其配位环境分别被6个来自两个双齿配位硝基和两个H2O分子的氧原子和4个来自两个Phen配体的氮原子所包围,形成单核+1价阳离子,外界有1个水分子,1个ClO-4阴离子和两个Phen分子构成.整个分子通过分子间氢键形成3D网络结构.     

CRYSTAL STRUCTURE OF [Sm(CCl_3COO)_3(H_2O)_2]·2H_2O

<正> Biaqua-trichloroacetate-samarium dihydrate, [Sm(CCl3COO)3(H2O)2]-2H2O, Mr=707.54, orthorhombic, space group Pnne, with a = 19.158(5), b = 22.176(4), c= 9.798(4)A, Z= 8, V= 4162.7A3.F{000)= 2696,λ(MoKα)=0.71069A, Dx = 2.258 g/cm3, final R=0.061. The title compound has non-molecular structural character, and its structural units Sm(μ-CCl3COO)s/2-(H2O>2 constitute 2-dinensional infinite chains of Sm(μ-CCl3COO)4Sm(μ-CCl3-COO)2Sm.The Sa(Ⅲ) atom in each unit is bound to two O atoms from aqua-molecules and six 0 atoms from six bridging CCl3COO groups (four of which are shared with the SB atom of another unit, two shared with the Sm atom of a third unit) forming a square antiprism.     

The solid-state thermal decomposition of Sr3[La(C2O4)3(H2O)2]2·11H2O

Strontium(II)diaquatris(oxalato)lanthanate(III)unidecahydrate, Sr₃[La(C₂O₄)₃(H₂O)₂]₂·11H₂O, has been synthesized and characterized by elemental, IR and electronic spectral studies. Thermal studies (TG, DTG and DTA) in air showed that all the crystal and coordinated water molecules are removed at ca. 225 °C. The final end product at 1,000 °C was shown to be a mixture of mainly SrCO₃, Sr₃La₄O₉ and La₂Sr₂O₅ along with oxides and carbides of both the metal, through the formation of an intermediate mixture of likely SrC₂O₄ and La₂(C₂O₄)_2.8 at 282 °C, and SrCO₃ and La₂O(CO₃)₂ at 540 °C. The multi-step dehydration and decomposition of the compound has been explored from the DSC study in nitrogen up to 670 °C, and the evaluated kinetic parameters are discussed.     

一维梯状配合物{[Cu2(4,4''-bpy)3(p-Ab)2(H2O)2]·(NO3)2·4H2O}n的晶体结构

合成了一维分子梯状配合物{[Cu2(4,4'-bpy)3(p-Ab)2(H2O)2]·(NO3) 2·4H2O}n(4,4'-bpy=4,4'-联吡啶,p-Ab-=对氨基苯甲酸根离子),该配合物晶体属单斜晶系,P2(1)/c空间群,晶胞参数:a=1.110 7(5) nm,b=1.550 4(3) nm,c=1.450 9(3) nm,β=104.81(3)°,V=2.415 5(12) nm3,Z=2.铜离子周围有3个氧原子和3个氮原子与之配位,其中2个氧原子由对氨基苯甲酸的螯合氧原子提供,另一个氧原子由配位水提供,3个氮原子分别由三个4,4'-联吡啶提供.这六个原子在铜离子周围形成一个畸变的八面体配位环境.配体对氨基苯甲酸只有一种配位形式--双齿螯合,第二配体4,4'-联吡啶的两个氮原子均参与配位,将配合物组装成一维分子梯结构.     

新型无机-有机杂化微孔晶体Cd3(BDC)0.5(BTC)2(DMF)(H2O)·3DMF·H3O·H2O的合成与结构

传统分子筛是以硅氧四面体和铝氧四面体为骨架的微孔晶体材料. 近年来, 以无机-有机结构单元为骨架组成的微孔晶体材料已引起人们的广泛关注[1～19]. 该类材料是由金属离子(或金属氧簇)与有机配体(大多数是芳香多酸和多碱)构成的建筑单元通过共价键或者分子间作用力构成的. 无机-有机杂化晶体材料有多种结构类型, 如1-D, 2-D, 3-D和笼状结构等.     

209Bi NQR in Mixed Oxides 2Bi2O3· B2O3, 3Bi2O3· 5B2O3, and Bi2O3· 3B2O3

It was earlier found from nuclear quadrupole resonance (NQR) measurements and computer modeling that -Bi₂O₃, Bi₃O₄Br and mixed oxides Bi₂O₃· 2Al₂O₃, Bi₂O₃· 2Ga₂O₃, Bi₂O₃· 3GeO₂, and 2Bi₂O₃· 3GeO₂exhibit local ordered magnetic fields from 30 to 200 G. It thus follows that these compounds are not diamagnets in a conventional sence of the word. With the aim of revealing previously unknown magnetic properties in bismuth(III) oxide-based Main Group element compounds, the mixed bismuth–boron oxides 2Bi₂O₃· B₂O₃, 3Bi₂O₃· 5B₂O₃, and Bi₂O₃· 3B₂O₃were prepared and studied using ²⁰⁹Bi NQR. The quadrupole interactions of the ²⁰⁹Bi nuclei and their electronic environment were studied, the crystallochemical features of the compounds were discussed, and the conformity of the ²⁰⁹Bi results to the X-ray structure data was verified. The preliminary tests in the field of a permanent magnet showed that the resonance intensities increase in external magnetic fields, indicating that a magnetism of unknown nature develops in the titled compounds. It was found reasonable to continue studies of the magnetic properties of these compounds using single-crystal ²⁰⁹Bi NQR in external magnetic fields.     

Crystal structure of Na6[(UO2)3O(OH)3(SeO4)2]2 · 10H2O

The complex Na₆[(UO₂)₃O(OH)₃(SeO₄)₂]₂ · 10H₂O (I) is synthesized and studied by X-ray diffraction. The compound crystallizes in the orthorhombic crystal system with the unit cell parameters: a = 14.2225(7) Å, b = 18.3601(7) Å, c = 16.5406(6) Å, V = 4319.2(3) ų, Z = 4, space group Cmcm, R ₁ = 0.0406. Compound I is found to be a representative of the crystal-chemical group A₃M³M² ₃T³ ₂ (A = UO²⁺ ₂, M³ = O^2?, M² = OH^?, T³ = SeO^2? ₄) of the uranyl complexes; it contains layer uranium-containing groups [(UO₂)₃O(OH)₃(SeO₄)₂]^3?. These layers linked to form a three-dimensional cage through bonds formed by the sodium atoms with the oxygen atoms of the uranyl ions and SeO₄ groups that belong to different layers.     

Structure of (C3H5NH3)2H2P2O7·H2O

The bis(cyclopropylammonium)dihydrogenodiphosphate monohydrate is a new diphosphate associated with the organic molecule C₃H₅NH₂. We report the chemical preparation and the crystal structure of this organic cation diphosphate. (C₃H₅NH₃)₂H₂P₂O₇.H₂O is orthorhombic (S.G. : P2₁2₁2₁), with Z = 4 and the following unit-cell parameters : a = 4.828(1) Å, b = 11.011(1) Å, c = 25.645(2) Å. The P₂O₇ groups and H₂O water molecules form a succession of bidimensional layers perpendicular to the c axis. The organic cations ensure the three-dimensional cohesion by NH-O hydrogen bonds.     

Synthesis and Structural Characterization of Adduct Cu_2(phen)_2·3(FCA)·(ClO_4)·2H_2O

Differentkindsofcopper(II)carboxylateadductshavebeensynthesizedandalsodinuclearcopper(Il)complexeshavebeenearlystUdiedasusefulmodelstoestablishmagneto-structUra1correlationsforspinexchangebetWeenmetalions.CostaIshowedthestructureof[Cu,(ll-OOCFc),(bpy),(ClO')(CH,Oand[Cu,(n-OOCFc),(bpy)(CH,OH),]' .Asfarasweknow,thecopper(II)compoundscontainingFCAandphenhavenotbeenreported.TheligandofFCAwassynthesizedaccordingtothefoIlowingscheme2.3:Asolutioncontainingl98mg(lmmol)ofphenandl5mLofmet…     

Ga2O3-La2O3-Yb2O3-Er2O3(HO2O3)体系光谱性质的研究

根据稀土离子能级的特点,对Ga2O3-La2O3-Yb2O3-Er2O3(HO2O3)体系的光谱性质进行了探讨,发现它们有二类发光性质:Stokes发光和反Stokes发光,研究了发光强度和发射波长与掺杂离子的依赖关系,观察到由能量的共振转移引起的荧光浓度猝灭现象,并取得了最大发光强度时的掺杂离子浓度和一些规律性结果.     

Syntheses,Crystal Structures and Characterization of Two Zeotype Crystals of K_4Cr_3O(H_2O)_3(OOCH)_6]_2[P_2W_(18)O_(62)]·9.5H_2O and K_4[Cr_3O(H_2O)_3(OOCH)_6]· [H_3P_2W_(17) Co(H_2O)O_(61)·20H_2O

IntroductionPolyoxometalates are used as the versatile inorga-nic building blocks for the construction of molecular-based materials[1—7]. Nanosized polyoxometalates aresuitable building blocks for the construction of crystal-line microporous structural m…