Hydrothermal synthesis,crystal structure,and properties of a novel magnesium phosphonate with a 1D chain structure

A novel 1D chain magnesium phosphonate with a 1D channel system along the c-axis, [Mg(H₄L)(H₂O)₃]_n (1) (H₄L^2-=HN(CH₂PO₃H)₃)^2-, has been synthesized under hydrothermal condition using triphosphonate ligand. The MgO₆ polyhedra and NC₃ planes are connected by phosphonate groups to form a 1D chain. The chains are interlinked by hydrogen bonds into 2D layers. Adjacent layers are further linked via hydrogen bonds to build a 3D network structure. The luminescent property of complex 1 has been also studied. For the complex 1, a blue fluorescent emission band with a maximum peak at 460 nm was observed.     

Synthesis and Crystal Structure of Diethyl (4,6-diamino-1,3,5-triazine-2-yl) phosphonate

1　INTRODUCTIONSomeoforganophosphoruscompounds,includingmanyheterocycliccompoundscontainingphosphonogroup,havegoodbioactivityinorganism[1].Duetotheirrela-tionwithbiochemical/biological,pharmacologicalandpesticidalresearch,hetero-cycliccompoundscontainingphosphonogrouphavebeensynthesizedbysomeofnewsyntheticmethods,inwhichseveralnewbuildingblockwereused,suchasβ-phos-phonicenemines,[2,3]isocyanomethylphosphonate,[4]β-functionalγ-oxo-alkylphos-phonates,[5]andacetylenicphosphonate.[6]Inourpr…     

三苯基锡2－噻吩甲酸酯的合成、性质和晶体结构

用三苯基氯化锡与2-噻吩甲酸钠反应，合成了三苯基锡2-噻吩甲酸酯，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/n，晶胞参数：a=1.3429(7)nm，b=1.11773(6)nm，c=1.4241(8)nmβ =116.519(6)°，V=2.0146(18)nm^3,Z=4，Dc=1.573g/cm^3，R1=0.0391，Wr2=0. 0943。该化合物的晶体是由孤立的分子所组成，四配位的锡原子呈畸变的四面体构 型，配体噻吩环上的硫原子和锡原子之间存在弱的配位作用。     

Synthesis and Crystal Structure of 5,7-Dimethoxy-2-phenylquinolin-4-yl Phenyloxy （N-L-Alanine ethyl ester） Phosphoramidate

5,7-Dimethoxy-2-phenylquinolin-4-yl phenyloxy （N-L-alanine ethyl ester） phosphoramidate （C28H29N2O7P, Mr = 536.17） has been synthesized by a facial phosphorylated reaction, and its structure was determined by IR, NMR, HR MS and X-ray single-crystal diffraction. The crystal belongs to triclinic, space group P1^-, with a = 11.375（2）, b = 11.591（2）, c = 11.638（2） A^°, α= 109.46（3）, β= 104.58（3）, γ= 100.48（3）°, V = 1339.6（5）A^°^3, Z = 2, Dc = 1.330 g/cm^3,μ = 0.152 mm^-1, F（000） = 564, the final R = 0.0654 and wR = 0.1546. In the crystal structure, the title compound is constructed by a centrosymmetric dimmer unit composed of a pair of π-π stacking diastereoisomers. The compound has a noteworthy feature in the framework, and such units are linked by two equal intermolecular P=O…H-N hydrogen bonds.     

双2-乙酰基二茂铁合汞的合成及其晶体结构

标题化合物(C24H22Fe2HgO2)3是由2 氯汞基 1 乙酰基二茂铁与乙二胺反应得到的,其结构通过单晶X 射线衍射法确定。其晶体属三斜晶系,P 1空间群,Mr=1964 12,a=10 193(2),b=11 504(2),c=14 413(3) ,α=92 21(3),β=104 12(3),γ=102 67(3)°,V=1591 55(5) 3,Z=1,Dc=2 049mg/cm3,μ=8 583mm-1,F(000)=942,最终偏离因子为R=0 0859,wR=0 2617。该晶体中同时含有meso型及dl型分子,各分子中Hg原子的配位情况不一样。meso分子中的两个二茂铁是相互平行的,而另两分子dl型的二茂铁是相互垂直的。Hg原子以桥联形式连接两个二茂铁部分。meso型与dl型分子通过Hg O弱配位作用相连。     

Synthesis and crystal structure of complex of Ce(NO_3)_3 with N-(3-methyl-pyridin-2-yl)-formimidoyl-(3-methyl-pyridin-2-yl) hydrazone

Rare earth complexes with organic ligands have been used as luminescence-material usually. Except their luminescent property, the complexes of trivalent lanthanide ions have low toxicity and powerful para-magnetic properties[1,2], so the lanthanide complexes are associated with important biological uses as diag-nostic tools and medicines[36]. Recently, there are some reports on Ce(III) complexes, some of which show anti-cancer activities[7]. S- tetrazines can be used as poly-dentate chelatin…     

Synthesis and Crystal Structure of the First Diaza-spirobifluorene：2-（Spirobifluorene-2-yl）-3,4-diaza-spirobifluorene

The title compound 2-(spirobifluorene-2-yl)-3,4-diaza-spirobifluorene(C48H28N2,Mr = 632.72) has been synthesized and characterized by 1H NMR,13C NMR and single-crystal X-ray diffraction.The crystal crystallizes in the monoclinic system,space group Cc with a = 13.8523(6),b = 29.3297(13),c = 8.6397(4) ,β = 111.8760(10)°,V = 3257.4(3) 3,Z = 4,Dc = 1.290 mg/m3,μ = 0.075 mm-1,F(000) = 1320,the final R = 0.0425 and wR = 0.1110 for 5288 observed reflections(Ⅰ 2σ(Ⅰ)).     

N-[(1-甲基-2-咪唑基)-1-亚甲基]-β-丙氨酸锌配合物的合成及晶体结构

金属离子Zn(Ⅱ)是生物体的必需元素,多年来其配位化学受到广泛的关注,含咪唑基团的Zn(Ⅱ)配合物更是受到人们的青睐[1]。本文报道了锌配合物[Zn(MIMHA)Cl2]2(MIMHA=1 [(1 甲基 2 咪唑基) 1 亚甲基] β 丙氨酸)的合成和晶体结构。1　实验部分将0 89g(10mmol)β 丙氨酸及适量的NaOH固体加入到20ml无水甲醇溶液中,待完全溶解后过滤,滤液滴加到10ml含有1 11g(10mmol)1 甲基 2 咪唑醛的无水甲醇溶液中,回流2h,回流过程中,溶液逐渐变为黄色。冰水浴下,分多次加入NaBH4(0 46g)固体,加完再搅拌2h,用浓HCl调溶液pH为2～3后,再搅拌2h,过…     

Hydrothermal synthesis,crystal structure and magnetic properties of a copper(II) phosphonate

The treatment of 3-ammonium-1-hydroxypropylidene-1,1′-bisphosphonate (H₇ahdp) and 4,4′-bipy with CuCl₂?·?2H₂O resulted in a metal phosphonate [Cu(H₅ahdp)?·?H₂O] _n . Its crystal structure has been characterized by single X-ray crystallography. Although there is no 4,4′-bipy in the lattice structure, it plays a very important role in forming the one-dimensional chain of the polymer. Hydrogen bonds link the chains into a 3D network. The dinuclear secondary building units are observed in the compound. The determination of variable-temperature magnetic susceptibilities (5?～?300?K) shows weak intrachain antiferromagnetic coupling between copper(II) centers. The magnetic data were fitted to the appropriate equations derived from the Hamiltonian H?=??2JS ₁ S ₂, giving the parameter J?=??25.78?cm^?1. Its thermal properties were also investigated.     

1,2-二[3-(6,8-二叔丁基-3,4-二氢-1,3-苯并嗪)基]乙烷的合成及晶体结构

~~1,2-二[3-(6,8-二叔丁基-3,4-二氢-1,3-苯并噁嗪)基]乙烷的合成及晶体结构@徐小平$苏州大学化学化工学院!江苏省有机合成重点实验室,江苏苏州215006 @姚英明$苏州大学化学化工学院!江苏省有机合成重点实验室,江苏苏州215006 @赵艺萍$江阴市长泾中学!江苏江阴214411 @张勇$苏州大学化学化工学院!江苏省有机合成重点实验室,江苏苏州215006 @沈琪$苏州大学化学化工学院!江苏省有机合成重点实验室,江苏苏州2150061,2-二[3-(6,8-二叔丁基.3,4-二氢-1,3-苯并噁嗪)基]乙烷;;合成;;晶体结构[1] Neuvonen K,Pihlaja K. J. Chan. Soc…     

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.     

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 and crystal structure of complex of Ce(NO<Subscript>3</Subscript>)<Subscript>3</Subscript> with N-(3-methyl-pyridin-2-yl)-formimidoyl-(3-methyl-pyridin-2-yl) hydrazone

The reaction of 3,6-di-(3-methyl-pyridin-2-yI)-s-tetrazine (DMPTZ, II) with Ce^III salt [Ce(NO₃)₃ · 6H₂O] generates a new ligand, N-(3-methyl-pyridin-2-yl)-formimidoyl-(3-methyl-pyridin-2-yl) hydrazone (L), and forms a new complex: a mononuclear complex [Ce(L)(NO₃)₂ (H₂O)₃] · NO₃ (III). Crystal data for III: space group P-1, with a = 0.7133(4) nm, b = 1.1139(2) nm, c = 1.4572(3) nm, α= 102.13(2)°, β= 99.81(3)°, γ= 91.10(3)°, Z = 2, V = 1113.6(7) nm³, μ = 2.123 mm⁻¹ and F(000) = 630. L acts as a tri-dentate chelating ligand in III. There are 10 coordination sites around Ce³⁺ of III, which are respectively occupied by seven oxygen atoms (four from two nitrate anions and three from three H₂O molecules) and three nitrogen atoms (all from L). The cerium atom and three chelating nitrogen atoms are coplanar. The mechanism of the metal assisted decomposition is discussed briefly.     

Molecular and crystal structure of quinoline-2-aldehyde thiosemicarbazone

The molecular and crystal structure of quinoline-2-aldehyde thiosemicarbazone is determined. The thiosemicarbazide fragment has cis-arrangement of terminal nitrogen atoms relative to the central N-C bond. The structure is based on a centrosymmetric dimer formed by hydrogen bonds between NH groups and sulfur atoms of thiosemicarbazide fragments of the neighboring molecules. In the crystal, the dimers are joined with each other through a system of hydrogen bonds and intermolecular π-π interactions.     

N-[(1-甲基-2-咪唑基)-1-亚甲基]-β-丙氨酸铜配合物的合成及晶体结构

含咪唑基团的氨基酸型Ｓｃｈｉｆｆ碱铜配合物有助于了解生物体内金属离子 -蛋白质间的键合作用[1～ 3] ,揭示铜在蛋白中的生物化学功能及其与咪唑和氨基酸等其它基团相互键合作用的本质。本文报道配合物 [Ｃｕ(ＭＩＭＨＡ) ]ＣｌＯ4 (ＭＩＭＨＡ =Ｎ [1 甲基 2 咪唑基 ) 1 亚甲基 ] β 丙氨酸 )的合成和晶体结构。单斜晶系 ,Ｃ2 /ｃ空间群 ,ａ =2 4 68(2 ) ,ｂ =7 60 1 (3 ) ,ｃ=1 4 1 3 7(1 0 ) ,β =1 0 2 8(1 ) ,Ｖ =2 5 86(3 ) 3,Ｚ =8.Ｃｕ(Ⅱ )处于平面四方形配位环境 ,四个配位原子中的三个为配体的二个氮原子和一个氧原子 ,…     

三苄基锡哌啶氨荒酸酯和二苄基锡双哌啶氨荒酸酯合成及晶体结构

利用三苄基氯化锡，二苄基二氯化锡和哌啶氨荒酸钠反应，合成了三苄基锡哌 啶氨荒酸酯（1）和二苄基锡双哌啶氨荒酸酯（2）。通过元素分析、红外光谱、核 磁共振氢谱和质谱对其结构进行了表征。用X-射线单晶衍射测定了这两个化合物的 晶体结构。化合物1为三斜晶系，空间群P-1，a=1.0271(2)nm,b=1.1131(2)nm,c=1. 2096(2)nm,α=75.56(3)°，β=81.09(3)°，γ=89.81(3)°，Z=2。化合物2为单 斜晶系，空间群P21/c,a=0.9710(3),b=2.436(1),c=1.2393(3)nm,β=90.28(2)°， Z=4。在1的晶体中， 锡原子呈五配位畸变三角双锥构型；2的晶体则是六配位的畸 变八面体构型。     

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。     

2-氨基对苯二甲酸双核铜配合物的合成与晶体结构

合成了一种新的铜配合物[Cu2(μ-2-atp)(phen)4].2ClO4(2-atp为2-氨基对苯二甲酸,phen为邻菲咯啉),利用红外光谱和X射线单晶衍射表征了产物的结构,利用元素分析测定了其元素组成,利用热重分析考察了其热分解行为.结果表明,标题化合物属于三斜晶系,P-1空间群,晶胞参数为:a=0.971 0(9)nm,b=1.187 8(1)nm,c=1.234 9(1)nm,α=70.104 0(1)°,β=68.699 0(1)°,γ=86.719 0(1)°,V=1.244 1(2)nm3,Z=1,Dc=1.635g/cm3,μ=1.041mm-1,F(000)=623,R1=0.058 4,wR2=0.129 3.该化合物具有双核铜结构,通过强烈的π-π堆积作用形成二维超分子结构.     

氟芳胺基、氟磺酰胺基磷酸酯的合成

首次合成了氟芳胺基磷酸酯和氟磺酰胺基磷酸酯.对氟苯胺、α-氯-4-三氟甲基吡啶胺、α-氯-4-三氟甲基氧化吡啶胺与二乙氧基磷酰氯在乙腈或DMF中反应,得到氟芳胺基磷酸酯.氟烷基磺酰甲胺与二乙氧基磷酰氯反应,以金属钠处理,相应钠盐在乙腈或DMF中,于室温下反应将得到氟烷磺酰胺基磷酸酯.