锌（Ⅱ）配位聚合物[Zn（HCPGA）2（H2O）2]n的合成和晶体结构

以3-(4-氯苯基)戊二酸(H2CPGA)为主要配体采用微波合成法合成了一个锌的新型配位聚合物[Zn(HCPGA)2(H2O)2]n(1),用元素分析仪、荧光光谱仪、红外光谱仪、热重分析仪和单晶衍射仪等对其进行了表征。结果表明该配位聚合物属于单斜晶系,空间群是C2/c。晶胞参数:a=2.9922(12)nm,b=0.7370(3)nm,c=1.0924(4)nm,β=98.008(6)°,F(000)=1200,Dc=1.628 g·cm-3,V=2.3855(16)nm3,Mr=584.68,Z=4,μ=1.309 mm-1,R1=0.0352,wR2=0.1124。     

新型稀土配位聚合物{Ln2（m-bdc）3（H2O）2}n（Ln=Ce,Nd）的合成、结构和动力学分析

以Ln(NO3)3.6H2O[Ln=Ce(1),Nd(2)]、间苯二甲酸(m-H2bdc)为原料,用水-DMF溶剂热合成法合成了两个异质同构的新型三维孔洞稀土金属配位聚合物{Ln2(m-bdc)3(H2O)2}n[Ln=Ce(1),Nd(2)],晶体结构经X射线单晶衍射仪分析确定,两种配合物的晶系均为单斜晶系,P21/c空间群,配位聚合物1:a=1.35428(11)nm,b=1.45987(11)nm,c=1.67101(10)nm,β=127.750(4)°,V=2.6122(3)nm3,Z=4,Dc=2.056 g.cm-3。配位聚合物2:a=1.34364(3)nm,b=1.45406(3)nm,c=1.66669(5)nm,β=127.382(2)°,V=2.5875(11)nm3,Z=4,Dc=2.097 g.cm-3。对配位聚合物1和2进行了元素分析、热重、红外光谱等表征,同时对标题配位聚合物的热稳定性及动力学进行了分析。     

单核Co（Ⅱ）含氮配体配合物[Co（py）3（H2O）3]（1,5-nds）的合成、晶体结构及热稳定性

在去离子水中合成了标题配合物[Co(py)3(H2O)3](1,5-nds)(py=吡啶,1,5-nds=1,5-萘二磺酸根离子),通过红外光谱、X射线单晶衍射、热分析等手段对配合物进行了表征。结果表明,该配合物晶体属于单斜晶系,空间群为C2/c。晶体学参数:a=1.5912(3)nm,b=1.2206(2)nm,c=1.4855(3)nm,α=90°,β=98.18(3)°,γ=90°,V=2.8558(10)nm3,Z=4。每个钴离子与3个吡啶分子及3个水分子配位,1,5-萘二磺酸阴离子起到平衡电荷的作用。     

配位聚合物{[Mn（H2BCPBA）2（H2O）4]}n的合成和表征

采用3,5-bi(4-carboxy-phenoxy)-benzoic acid(H3BCPBA)为配体,以Mn为中心离子采用自组装的方法合成了配位聚合物{[Mn(H2BCPBA)2(H2O)4]}n,采用单晶衍射仪,红外光谱,热重,固体紫外和元素分析对其进行了晶体结构的解析和表征。它属于三斜晶系,P1空间群,晶胞参数分别为a=0.58423(13)nm,b=1.3644(3)nm,c=1.3910(3)nm,α=109.173(2)°,β=98.927(3)°,γ=99.123(3)°,V=1.0082(4)nm,Mr=913.63,Z=1,Dc=1.505 g/cm3,μ=0.414 mm-1,F(000)=471.0。热重分析表明,该配合物在410℃下稳定,UV固体光谱表明,该配合物有很弱的吸收。     

2-甲基4-(4-(吡啶-3-乙炔基)苯基)-3-丁炔-2-醇的合成及晶体结构

由1,4-二碘代苯出发,经过两步Sonogashira偶联反应合成了标题配合物2-甲基4.(4-(吡啶-3-乙炔基)苯基)-3-丁炔-2-醇.通过1H NMR、13C NMR核磁共振、Ⅹ-射线单晶衍射等手段对化合物的结构进行了表征.结果表明,该化合物晶体属于单斜晶系,空间群为P21/c.晶体学参数:a=3.3321 (4) nm,b=1.00539(11) nm,c=0.89158(10) nm,α =90.00°,β=92.442(2)°,y=90.00°,V=2984.2(6) nm3,Z =4.     

锌(Ⅱ)配位聚合物{[Zn(CPGA)(DPPP)]H2O}n的合成和晶体结构

采用水热法合成了一个锌的新型配位聚合物{[Zn(CPGA)(DPPP)]·H2O｝n(1),[CPGA=3-(4-氯苯基)戊二酸根,DPPP=l,3-二(4-吡啶基)丙烷],用元素分析、红外光谱和X-射线单晶结构等进行了表征.结果表明该配位聚合物属于单斜晶系,P21/n空间群.晶胞参数为:a=1.3775(2) nm,b=1.20745(19) nm,c=1.4854(2) nm,F(000)=1080,Dc=1.419 g·cm-3,V=2.4446(7) nm3,Mr=522.28,Z=4,μ=1.151 mm-1,月1=0.0389,ωR2=0.1253.该配位聚合物晶体中,Zn(Ⅱ)与配体3-(4-氯苯基)戊二酸根和DPPP连接形成一维波浪面结构,水分子和3-(4-氯苯基)戊二酸根中未参与配位的氧原子形成的氢键将相邻的两层连接形成双层结构,双层结构没有进一步连接.     

3LiMnPO4·Li3V2（PO4）3正极材料的制备及其电化学性能研究

以五氧化二钒干凝胶、碳酸锰、磷酸二氢铵、碳酸锂、乙炔黑为原料,采用固相法在相对较低的温度条件下合成了x Li Mn PO4·y Li3V2(PO4)3锂离子电池复合正极材料。采用X射线衍射(XRD)、扫描电镜(SEM)对其晶体结构和表面形貌进行表征。结果表明,750℃下烧结15 h合成的3Li Mn PO4·Li3V2(PO4)3为结晶良好的两相结构,颗粒粒径较小且分布比较均匀,其在室温、0.2 C倍率下首次充放电容量分别为144.8 m Ah/g和139.8 m Ah/g,循环50次后容量为130.5 m Ah/g。     

含异主族金属硫属化合物(1,2-dap)2InAsSeS3的溶剂热合成及晶体结构

采用溶剂热合成法合成含有异主族金属的硫属化合物(1,2-dap)2InAsSeS3(1,2-dap:1,2-丙二胺),且该化合物同时含有两种硫族元素.本文对该化合物进行单晶X-射线衍射分析、粉末X射线衍射(XRD)、红外光谱分析(IR)、差热-热重(TG-DSC)分析等表征.单晶X-射线衍射分析表明该化合物属于四方晶系,空间群为P42bc,a=1.41178(12)nm,b=1.41178(12)nm,c=1.6220(4)nm,Z=8.标题化合物为零维簇状结构,是由AsS2(S/Se)2四面体与InS(S/Se)N4八面体通过共边连接形成.     

一种新的非线性光学材料—Na3Sm2（BO3）3

本文采用固相反应法合成了一种新的硼酸盐化合物Na3Sm2(BO3)3,以Na2CO3-H3BO3为助熔剂,用悬挂铂丝法获得了3mm×2mm×0.5mm的透明单晶,X射线粉末衍射分析表明,该化合物属正交晶系,晶胞参数a=0.50585nm,b=1.10421nm,c=0.70316nm.红外光谱测量证实晶体结构中含有BO33-基团,粉末倍频效应测试表明该化合物具有非线性光学效应,粉末倍频信号强度接近KDP.     

具有三维超分子结构的单核锌配合物[Zn(py3（H2O）3]（1,5-nds）的合成与表征

在水和乙醇混合溶剂中合成了具有三维超分子结构的单核Zn(Ⅱ)含氮配体配合物[Zn(py)3(H2O)3](1,5-nds)(py=吡啶,1,5-nds=1,5-萘二磺酸根离子)。采用X射线单晶衍射、红外光谱、元素分析等方法对配合物进行了表征。X射线单晶衍射表征结果表明,该配合物晶体属于单斜晶系,空间群为C2/c。晶体学参数:a=1.58349(14)nm,b=1.21220(11)nm,c=1.45471(16)nm,α和γ=90°,β=98.2800(10)°,V=2.8052(4)nm3,Z=4。     

A Unique Example of a Co-crystal of [Co(AMTTO)2(H2O)2](NO3)2 and [Co(AMTTO)2(CH3CN)2](NO3)2 (AMTTO = 4-amino-5-methyl-1,2,4-triazol-3(2H)-thione)

A co-crystal of cobalt(II) complexes, Co(AMTTO)₂(CH₃CN)₂]²⁺(NO₃)₂. [Co(AMTTO)₂(H₂O)₂]²⁺(NO₃)₂, compound (1) was isolated from the reaction of Co(NO₃)₂?6H₂O and 4-amino-3-mercapto-6-methyl-5-oxo-1,2,4-triazine (AMTTO) in acetonitrile as solvent. Isolated crystals were characterized by elemental analyses, IR spectroscopy as well as X-ray diffraction studies. Crystal data for 1 at 95 K revealed a monoclinic space group P2₁/n, a?=?11.7903(5), b?=?12.1279(5), c?=?14.1443(6) Å, β?=?99.244(4)°, Z?=?2, R₁?=?0.0339. Compound 1 consists of two co-crystallized Co(II) complexes [Co(AMTTO)₂(CH₃CN)₂]²⁺ and [Co(AMTTO)₂(H₂O)₂]²⁺ and four nitrate counter anions In both complexes, cobalt(II) ions are in an octahedral arrangement. Two S, N bidentate AMTTO ligands are coordinated to both Co(II) ions. The coordination sphere of Co1 is completed by two acetonitrile molecules, and these positions are occupied by water molecules for Co2.

Graphic Abstract

A co-crystal of cobalt(II) compound was isolated from the reaction of Co(NO₃)₂?6H₂O and 4-amino-3-mercapto-6-methyl-5-oxo-1,2,4-triazine in acetonitrile as solvent.

     

Crystal structure investigation of [Mn(3-CH3C5H4N)2(N3)2(H2O)2]

The crystal structure of the title compound has been determined by single crystal X-ray diffraction methods. [Mn(3-CH₃C₅H₄N)₂(N₃)₂(H₂O)₂] crystallizes in the space group P 1 with a = 7.444(2) Å, b = 7.691(2) Å, c = 8.926(3) Å, α = 99.82(3)°, β = 108.80(2)°, γ = 114.99(2)° and Z = 1. Least squares refinement gave a R value of R_w = 0.046 for 1414 observed reflections. The manganese atom in the title complex is octahedrally coordinated by two oxygen atoms of the water molecules and four nitrogen atoms; two N-atoms are the end atoms of azide groups and the other two nitrogen atoms belong to the 3-methylpyridine molecules. The polyhedra are linked via hydrogen bonds between the water molecules and the azide groups.     

Electrical Conductivity of Phenoxazine-Iodine (2:3) and Phenothiazine-Iodine (2:3) Crystals

Abstract

Single crystals of phenoxazine-iodine (2 : 3) and phenothiazine-iodine (2 : 3) salts are found to be highly conducting ([sgrave] _R.T. = 5–20 ohm^?1 cm^?1). The observed deviation from the exponential temperature dependence of the conductivities is ascribed to the degenerate semiconducting phases or alternatively to the metallic phases with impurities. However, phenoxazine-iodine and phenothiazine-iodine are perfect semiconductors below 220° K with activation energies of 0.12 eV and 0.14 eV, respectively. The absorption features related with (phenoxazine)⁺ ₂ and (phenothiazine); cations are observed in the infrared spectra of the salts.     

X-Ray diffraction and IR-spectroscopic studies of UO2(n-C3H7COO)2(H2O)2 and Mg(H2O)6[UO2(n-C3H7COO)3]2

Single crystals of UO₂(n-C₃H₇COO)₂(H₂O)₂ (I) and Mg(H₂O)₆[UO₂(n-C₃H₇COO)₃]₂ (II) are synthesized. Their IR-spectroscopic and X-ray diffraction studies are performed. Crystals I are monoclinic, a = 9.8124(7) Å, b = 19.2394(14) Å, c = 12.9251(11) Å, β = 122.423(1)°, space group P2₁/c, Z = 6, and R = 0.0268. Crystals II are cubic, a = 15.6935(6) Å, space group $Pa\bar 3$ , Z = 4, and R = 0.0173. The main structural units of I and II are [UO₂(C₃H₇COO)₂(H₂O)₂] molecules and [UO₂(C₃H₇COO)₃]^? anionic complexes, respectively, which belong to AB ₂ ⁰¹ M ₂ ¹ (I) and AB ₃ ⁰¹ (II) crystal chemical groups of uranyl complexes (A = UO ₂ ²⁺ , B ⁰¹ = C₃H₇COO^?, and M ¹ = H₂O). A crystal chemical analysis of UO₂ L ₂ · nH₂O compounds, where L is a carboxylate ion, is performed.     

Crystal structures of [WI2(CO)3{Ph2P(CH2) n PPh2}] (n = 2 or 3)

[WI₂(CO)₃{Ph₂P(CH₂)₂PPh₂}] (1) crystallizes out in the monoclinic space group P2₁/n, with a = 13.852(7) Å, b = 14.789(19) Å, c = 14.915(19) Å, = 102.86(1)°, Z = 4. [WI₂(CO)₃{Ph₂P(CH₂)₃PPh₂}] (2) crystallizes out in the monoclinic space group P2₁/n, with a = 10.499(15) Å, b = 14.58(2) Å, c = 20.75(3) Å, = 103.59(1)°, Z = 4. Both structures show the metal in a seven-coordinate environment with a carbonyl in the unique capping position, two further carbonyls and a phosphorus in the capped face, and two iodides and the second phosphorus in the uncapped face.     

Crystal structure of NH3(CH2)2NH3(BiI4)2·4H2O

The ethylenediammonium bis tetraiodobismuthate(III) tetrahydrate salt is monoclinic with the following unit cell dimensions:a=7.476(3)Å,b=13.194(3)Å,c=13.916(9)Å, β=95.22(6)°, space groupP2₁ lc withZ=2. The structure consists of disordered ethylenediammonium cations, water molecules and polynuclear anions in which slightly distored [BiI₆]^3? octahedra sharingcis edges are interconnected into chains. The [BiI₄]^? anions are connected through O(W2)?H...I hydrogen bonds, so that infinite two dimensional chains parallel to thea axis with anionic period [BiI₄(H₂O)]^? are formed in the structure. These chains are themselves interconnected by means of the O?H...I and N...O(I) bonds originating respectively from the water molecules and the ethylenediammonium entities, forming a three-dimensional network.     

Crystal structure ofcis-diaqua bis(2,2′-bipyridyl)chromium(III) nitrate, [Cr(bipy)2(H2O)2] (NO3)3

cis-Diaquabis(2,2-bipyridyl)chromium(III) nitrate crystallizes in the mono-clinic system, space groupP2₁/c, witha=16.102(6),b=10.792(5),c=15.076(6) Å,=112.90(5)°, andZ=4. The saltlike structure was determined from X-ray crystallography and refined toR=7.5% for 3342 observed reflections. The Cr atom is octahedrally surrounded by twocis water molecules and by two chelated 2,2-bypiridyl ligands forming two nearly orthogonal planes. Selected bond distances are: Cr-O, 2.00(1) and 1.98(1) Å, Cr-N, 2.04 Å (mean).     

Crystal and molecular structures of 1-(2-carboxypropan-2-ylamino)-3-(1-naphthyloxy) propan-2-ol (1) (C17H21NO4) and 1-(2-carbamoyl propan-2-ylamino)-3-(1-naphthyloxy) propan-2-ol (2) (C17H22N2O3)

The crystal structures of two new-adrenergic antagonists, derivatives of propranolol containing 2-methylalanine fragment are described in this paper. The space groups and unit-cell parameters are: compound1 (C₁₇H₂₁NO₄): monoclinic, space groupP2₁/n,a=5.787(1),b=18.703(4),c=23.526(5)Å,=96.49(2)°; compound2 (C₁₇H₂₂N₂O₃): triclinic, space groupP¯1,a=8.321(1),b=10.121(1),c=10.368(1)Å,=109.49(1)°,=90.49(1)°, =103.48(1)°. The structures were solved by direct methods and refined with full matrix least-squares techniques toR indices of 0.055 and 0.049, respectively. The molecules of compound1 exist in the crystal as dual ions. The molecules of compound2 are compact and their external chain is twisted in a characteristic way (similar to that found in peptides).     

Crystal structure of [WI2(CO)3{P(OMe)3}2]

[WI₂(CO)₃{P(OMe)₃}₂]crystallizes in the orthorhombic space group Pca2₁, with a = 26.924(5), b = 10.726(2), c = 14.136(3) Å, and Z = 8. There are two molecules in the asymmetric unit, the metal atoms in each case being seven-coordinate with a capped fac-(CO)₃ octahedral geometry. The molecular dimensions in the two molecules are nearly identical. The W–P distance to the capping atom 2.397 Å (average) is significantly shorter than the other W–P distance, 2.525 Å (average).     

Crystal structure of pentakis ethylenediammonium bis undecachlorodiantimonate(III) tetrahydrate, (NH3(CH2)2NH3)5(Sb2Cl11)2·4H2O

The pentakis ethylenediammonium bis undecachlorodiantimonate(III) tetrahydrate salt is monoclinic with the following unit cell dimensions:a=16.271(5) Å,b=13.004(4) Å,c=13.932(4) Å, β=111.72(2)°, space groupP2₁/c withZ=2. The structure was solved by Patterson methods and refined to a finalR value of 0.023 for 4435 reflections withF ₀>4σ(F ₀). The structure shows a layer arrangement perpendicular to thea axis: planes of the [Sb₂Cl₁₁]⁵⁻ bioctahedra alternate with planes of [NH₃(CH₂)₂NH₃]²⁺ dications. The [Sb₂Cl₁₁]⁵⁻ bioctahedra are connected through O−H...Cl hydrogen bonds, such that infinite chains of composition [Sb₂Cl₁₁(H₂O]_n ⁵ⁿ⁻ are formed in the structure, parallel to the twofold axis. These chains are themselves interconnected by means of N−H...Cl and O−H...Cl bonds originating from the [NH₃(CH₂)₂NH₃]²⁺ entities and the water molecules, respectively, and form a threedimensional network.