四元混合阴离子配合物〔La(C_6H_5COO)_2(NO_3)(bipy)〕_2的合成和晶体结构

合成了新型镧系四元混合阴离子配合物〔Ｌａ（Ｃ６Ｈ５ＣＯＯ）２（ＮＯ３）（ｂｉｐｙ）〕２, 化学经验式为Ｃ２４Ｈ１８Ｎ３Ｏ７Ｌａ,Ｍｒ＝ ５９９．３３,晶体属三斜晶系,Ｐ１ 空间群,晶胞参数：ａ＝１１．０２０（４）, ｂ＝ １１．１８２（２）, ｃ＝ １０．２８５（３） , α＝ １０２．８３（２）, β＝ １０９．１６（２）, γ＝８２．２３（３）°, Ｚ＝ １ , Ｄｃ＝ １．７０９ ｇ／ｃｍ ３, Ｖ＝ １１６４．７（６） ３, μ（ＭｏＫα）＝ １８．７７ｃｍ － １, Ｆ（０００）＝ ５９２．００ ;全矩阵最小二乘法修正至Ｒ＝ ０．０２３,Ｒｗ ＝ ０．０３１,独立可观测衍射点数为３８２８ 个。标题配合物是双核分子,中心离子配位数为９,配位多面体结构为单帽四方反棱柱,四个苯甲酸根呈双齿桥联和三齿桥联二种配位方式,且配合物中存在分子间芳环堆积作用。     

稀土冠醚类配合物的研究(ⅩⅧ)——〔Sc(NO_3)_3(H_2O)_2〕·(15-C-5)配合物的合成、性质和结构

在乙腈介质中培养出由水合硝酸钪与15-冠-5(15C5)组成的配合物(Sc(NO_3)_3(H_2O)_2]·(15C5)单晶。对配合物进行了元素分析、红外光谱、溶解性及摩尔电导测定和X射线结构分析。     

硝酸镧联吡啶冠醚混配合物La（NO3）3（bipy）（H2O）2（B—15—C—5）的合成及晶体结构

本文报道了La(NO3)3(bipy)(2H2O)(B-15-C-5),(Mr=785.46)的合成和晶体结构。晶体属单斜晶系，空间群为P21／n，晶胞参数：a=11.951(6),b=18.181(7),c=14.754(5)A,B=96.19(3),V=3187,0A3,Z=4,Dc=1.637g/cm3，晶体结构由直接法和Fourier合成解出，使用对角块矩阵和全矩阵最小二乘法对原子参数进行修正，最后偏离因子R＝0．035（5261个1＞3σ（I）射衍，单晶结构分析表明，在该配合物中，直接参与位的是联吡啶上的两上氮原子，三个NO3中的六个氧原子以及两个水分子中的氧原子，La^3 的配位数为10，B－15－C－5是通过氢键与2O分子 相连的。     

轻稀土B-15-C-5联吡啶三元配合物

合成了稀土(Ln=La—Eu)硝酸盐与苯并-15-冠-5和2,2’-联吡啶的三元配合物,并培养出La-配合物的单晶,测定了的分子结构和晶体结构。经元素分析确定其化学组成为Ln(NO_3)_3·bipy·2H_2O·B-15-C-5。晶体属单斜晶系,空间群为P2_1/n。晶胞参数:a=11.951(6),b=18.181(7),c=14.754(5);β=96.19(3)°;V=3187.0,Z=4,D_c=1.637g/cm~3。最后偏离因子R=0.035。     

[La(CH_2ClCOO)_2(NO_3)(phen)(H_2O)]_n的合成和晶体结构

合成了混合阴离子配合物［Ｌａ（ＣＨ２ＣｌＣＯＯ）２（ＮＯ３）（ｐｈｅｎ）（Ｈ２Ｏ）］ｎ。配合物经元素分析、ＩＲ、ＤＴＡＴＧ和ＵＶ等表征。用Ｘ射线单晶结构分析解析了标题配合物的晶体结构，三斜，空间群Ｐ１，晶胞参数为ａ＝１０５３３（２），ｂ＝１３１３６（３），ｃ＝７７７６（１），α＝９６５９（１）°，β＝９５７６（１）°，γ＝１０８４２（２）°，Ｖ＝１００３３（３）３，Ｚ＝２，Ｄｃ＝１９４０ｇ／ｃｍ３，Ｆ（０００）＝５７２，μ（ＭｏＫα）＝２４３６ｃｍ－１。     

〔phenH〕〔La(NO_3)_4(H_2O)(phen)〕·H_2O的合成和晶体结构

标题化合物由Ｌａ（ＮＯ３）３·ｎＨ２Ｏ,１,１０－邻菲罗啉（ｐｈｅｎ）和乙酰丙酮等在无水乙醇和水的混合溶剂中合成并用ＩＲ谱和Ｘ射线结构分析进行表征。晶体学数据如下：Ｃ２４ Ｈ２１ＬａＮ８Ｏ１４,Ｍｒ＝ ７８４．４０, 三斜, Ｐ１, ａ＝ ７．１２４（１）, ｂ＝ １１．０４７（２）, ｃ＝ １９．３９３（４）, α＝ ８１．１０（３）, β＝ ８７．７９（３）, γ＝ ７４．３６（３）°, Ｖ＝ １４５２．０（５）３, Ｚ＝ ２, Ｄｃ＝１．７９４ｇ／ｃｍ ３, Ｆ（０００）＝ ７８０, μ（ＭｏＫα）＝ １．５５７ｍ ｍ － １。化合物由阳离子〔ｐｈｅｎＨ〕＋ 和配合阴离子〔Ｌａ（ＮＯ３）４（Ｈ２Ｏ）（ｐｈｅｎ）〕－ 及一个结晶水分子组成。配合阴离子中以Ｌａ原子为中心,周围被２ 个Ｎ原子（来自ｐｈｅｎ）和９ 个Ｏ原子（来自ＮＯ３－ 和Ｈ２Ｏ）所占据,构成较为罕见的１１ 配位。晶胞中两两阳离子〔ｐｈｅｎＨ〕＋ 及两两配体ｐｈｅｎ 平面之间均相互平行堆积,并有多种类型的氢键存在,这些都可以降低能量,有利于化合物在晶体中的堆积。     

[U(CO_3)_3(H_2O)_2]·2H_2O配合物的合成及晶体结构

A uranylcontaining compound [U(CO_3)_3(H_2O)_2]·2H_2O has been synthesized under hydrothermal condition and characterized by X-ray single-crystal analysis. Crystal structural analysis indicates that this compound consists of three CO_3~(2-) molecules, one U~(6+). The results reveal that the title compound presents a 3D frame work built up by O-H……O week hydrogen bonds interactions. The central uranium atom is eight-coordinated through three CO_3~(2-) molecules and two H_2O. The compound shows a coplanar hexagonal network structure, each hexagon containing a hexagonal hole with a water moleculet.     

CRYSTAL STRUCTURES OF La(NO_3)_3 COMPLEXES WITH BENZO-15-C-5 AND CYCLOHEXYL-15-C-5

<正> Complex La(NO3)3(Benzo-15-C-5) (C14H20LaN3O14, Mt= 593. 28) crystallizes in the orthorhombic,space group P212121 with a=8. 393(2),b= 16. 624(5), c = 17. 326(4) A ,V = 2417. 6(6) A3,Z = 4,DC= 1. 63gcm-3,F(000) = 1176, μ= 18. 7cm~1(MoKa). The final refinement converged with R = 0. 060 and Rw=0. 065 for 2223observed independent reflections. Complex La ( NO3 )3 ( Cyclohexyl- 15- C- 5 ) (C14H26LaN3O14,MT = 599. 34) is monoclinic,P21/n space group with a=9. 917(4),b= 13. 667(5),c=16. 763(5)A,β=104. 33(3),V = 2201(1)A3,Z=4,Dc=1.81gcm-3, F(000) = 1200,μ= 20. 4cm-1(MoKa).The final refinement converged with R=0. 048 and Rw=0. 036 for 1495 observed independent reflections. In the two complexes,the La (Ⅲ) ion is 11-coordinate and bonded to six oxygen atoms from three bidentate nitrate groups and five oxygen atoms from the crown ether. The average bond lengths of La -O (crown) and La -O(nitrate)are 2. 68 and 2. 61A for La(NO3)3(Benzo-15-C-5) ,re-snectively and 2. 71 and 2. 62 A for La(NO3)3(Cyclohexyl-15-C-5) re     

La(NO3)3·bipy·2H2O·(B-15-C-5)电子结构和电化学键

稀土硝酸盐与双啮杂环胺配体α,α′联吡啶(bipy)的配合物研究不多.Hart 等合成了Ln(NO_3)_3(bipy)_2配合物;亦已解析了3个晶体结构:La(NO_3)_3(bipy)_2,Tb(NO_3)_3(bipy)_2,La(NO_3)3·bipy·2H_2O·(B-15-C-5)(B-15-C-5=苯并15-冠-5,).我们对La(NO_3)_3(bipy)_2的电子结构和化学键作过研究.本文利用自旋非限制适于稀土配合物计算的INDO方法研究了La(NO_3)_3·bipy·     

一维链状配合物Cd(SDBA)(H_2O)_2的合成及其晶体结构

用水热法合成了新型的一维配合物Cd(SDBA)(H2O)2(1,H2SDBA=二苯砜-4,4'-二甲酸),其结构经IR,元素分析和X-射线单晶衍射表征.1属于单斜晶系,P2/c空间群,晶胞参数: a=1.330 3(6) nm,b=0.528 2(9) nm,c=1.217 6(6) nm,β=116.143(5)°,V=0.768(6) nm3,Z=2,Mr=452.7 g·mol-1,Dc=1.958 g·cm-3,μ=1.599 mm-1,F(000)=448,R1=0.041 3,wR2=0.098 3,S=0.985. 1中Cd2+与2个SDBA2-配体上的4个O原子和2个配位水上的2个O原子配位,形成一个畸变的八面体.在a轴方向,Cd2+经SDBA2-桥联形成一维波浪状链,链与链之间通过氢键相互作用形成三维超分子结构.     

Synthesis and Crystal Structure of［Lu（NO_3）_3（H_2O）_2（CH_3CN）］（Benzo－15－C－5）·CH_3CN

ＳｙｎｔｈｅｓｉｓａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆ［Ｌｕ（ＮＯ_３）_３（Ｈ_２Ｏ）_２（ＣＨ_３ＣＮ）］（Ｂｅｎｚｏ－１５－Ｃ－５）·ＣＨ_３ＣＮＷａｎｇＲｕｉ－Ｙａｏ；ＪｉｎＺｈｏｎｇ－Ｓｈｅｎｇ；ＮｉＪｉａ－Ｚｕａｎ（Ｌａｂｏｒａｔｏｒｙｏ...     

Synthesis and Crystal Structure of Mn(phen)(CF_3COO)(H_2O)_3·NO_3

1 INTRODUCTION The manganese(II) ion is a biologically essential element. Knowledge of its importance is increasing as more and more enzymes are found to contain manganese ions at the active center[1, 2]. The X-ray crystallographic structures of a consi…     

Synthesis and Crystal Structure of a New Complex （H3IDC）（Prz）0.5（H2O）

The compound （H3IDC）（Prz）0.5（H2O） （H3IDC = imidazole-4,5-dicarboxylate, Prz = piperazine） has been prepared from a hydrothermal approach and was characterized by IR analysis and X-ray diffraction. Its crystal structure consists of discrete 4,5-imidazole-dicarboxylate, H2O and piperazine molecules. The whole structural motif was assembled by three different non-covalent interactions of O-H…O, N-H…O and π-π stacking, which play an important role in packing the molecules. Interestingly, the connections between imidazole-4,5-dicarboxylate molecule and water molecule result in a helical polymeric chain. Crystal data for compound 1： monoclinic system, space group P21/c, a = 6.4600（13）, b = 19.910（4）, c = 6.9123（14） A^°, β = 94.26（3）°, V= 886.6（3） A^°^3, Z= 4, C7H10O5N3, Mr = 216.18.     

Synthesis and Crystal Structure of Co(C_6NO_2H_4)_3. H_2O

1INTRoDUCTIONAlotofresultsoncobaltcomplexstructureshavebeenreportedforseveraldecades.Theinterestofresearchinthisfieldhasneverbeenreducedbecausethecobaltcomplexesplayaveryimportantroleinthelifescienceandcatalysis,etc[1-6).WereportherethesynthesisandstructureofcomplexCo(C,NO,H'),.H,O.2EXPERIMENTALAllreagentsandsolventsusedareofARgradefromcommericalsourceswithoutfurtherpurification.ThetitlecompoundCo(C,NO,H,),.H,Owassynthesizedbythefollowingmethod.When2.4g(ca.1mmol)ofCoCl2.6H2Ow…     

Synthesis, Crystal Structure and Spectral Properties of [Ce(NO_3)_5(H_2O)_2]·2(Hphen)·(H_2O)

1 INTRODUCTION Recently, the ternary or quaternary mixed anion complexes of cerium(III) containing 1,10-phenanthroline (phen) have attracted considerable attention due to their rich structural chemistry and appealing magnetic properties[1]. Panagiotopou…     

Supramolecular Terbium-SIP Complex Pillared by 4,4'-Bipyridyl,{[Tb(SIP)(H_2O)_5]_2(bpy)_3(H_2O)}n:Synthesis,Crystal Structure and Photoluminescence

The supramolecular terbium complex, {[Tb(SIP)(H2O)5]2(bpy)3(H2O)}n (NaH2SIP= 5-sulfoisophthalic acid monosodium salt and bpy=4,4'-bipyridyl), has been synthesized by the hydrothermal reaction of Tb4O7 with NaH2SIP and bpy at 165 ℃, and characterized by single-crystal X-ray diffraction, elemental analysis, IR spectrum, powder X-ray diffraction and photoluminescence spectrum. It crystallizes in a monoclinic system, space group C2/c, with a= 30.6840(1), b=10.9206(2), c=17.4967(3), β=111.931(1)o, V=5438.65(14)3, Z=4, C46H52N6O25S2Tb2, Mr=1470.90, Dc=1.796 g/cm3, μ=2.747 mm-1, F(000)=2928, the final R= 0.0654 and wR=0.1322 for 3806 observed reflections with I > 2σ(I). In the neutral [Tb(SIP)(H2O)5]2 motif, the Tb(III) ions are linked by the SIP ligands to form a one-dimensional zigzag chain propagating along the c axis. The zigzag chains are linked together by hydrogen bonds and π-π stacking interactions to form a two-dimensional supramolecular framework. The uncoordinated bpy molecules act as pillars to extend the two-dimensional sheets into a distinctive pillared three-dimensional supramolecular structure through O-H···N hydrogen bonds. The photoluminescence of the complex was investigated at room temperature in the solid state.     

［La（EO_3）_3（H_2O）］（ClO_4）_3·H_2O的晶体结构

稀土高氯酸盐开环冠醚三缩乙二醇（ＥＯ_３）［Ｌａ（Ｃ_６Ｈ_（１４）Ｏ_４）_３（Ｈ_２Ｏ）］（ＣｌＯ_４）_３·Ｈ_２Ｏ，单斜晶系，Ｐ２_１／ｃ空间群。晶胞参数为：ａ＝１５．４７４（２），ｂ＝１１．３８６（１），ｃ＝２０．８４１（４），β＝９９．８２（１）°，Ｖ＝３６１８（１），ＭｏＫα，Ｚ＝４，Ｄ_ｃ＝１．７１８ｇ／ｃｍ３，μ＝１．４９９ｍｍ￣（－１）。全矩阵最小二乘精细修正，结构因子Ｒ＝０．０５６，Ｒ_ｗ＝０．０８３。中心原子Ｌａ与开环冠醚醚链上的Ｏ（１）～Ｏ（９）及一个水分子形成１０配位双帽四方反棱柱结构。弱配体高氯酸根不参加配位。     

Synthesis and Crystal Structure of [{Cd(hmbdc)(H_2O)_3}·2H_2O]_n

A novel coordination polymer [{Cd(hmbdc)(H2O)3}·2H2O]n (hmbdc = 5-hydroxy- isophthalic acid) has been synthesized and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/c, with a = 9.599(3), b = 18.699(5), c = 7.557(2) , β = 108.198(4)°, V = 1288.6(6) 3, Z = 4, Mr = 382.60, Dc = 1.972 g/cm3, F(000) = 760, μ = 1.740, the final R = 0.0555 and wR = 0.0995 for 1732 observed reflections with I > 2σ(I). The structural analysis shows that the intermolecular hydrogen bonds and π-π interactions result in a three-dimensional supramolecular framework.