［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。     

高氯酸四(DL-a-缬氨酸)八水合二钐的合成和结构

α-氨基酸在人体有极为重要的生理作用,近年来人们对其稀土配合物进行了广泛的研究。进一步研究稀土氨基酸配合物的单晶结构对于探讨稀土离子与生物体的作用是很有意义的。将高氯酸钐溶液与生化试剂DL-a-缬氨酸以1:1摩尔比混合,在75℃水浴中反应6小时,加热浓缩后,室温下缓慢挥发,即得到浅黄色透明棱状晶体。 结果与讨论     

Synthesis, structural characterization and properties of a 3D infinitely extended structural rare earth coordination compound of K3{[Sm(H2O)7]2Na[α-SiW11O39Sm(H2O)4]2}·14 H2O

A 3D infinitely extended structural rare earth coordination compound with a formula of K3{[Sm(H2O)7]2Na[α-SiW11O39Sm(H2O)4]2}·14H2O has been synthesized by reaction of Sm2O3, HClO4, NaOH with α-K8SiW11O39·nH2O, and characterized by IR,UV spectra, ICP, TG-DTA, cyclic voltammetry, variable-temperature magnetic susceptibility and X-ray single-crystal diffraction.X-ray single-crystal diffraction indicates that the title compound crystallizes in a triclinic lattice, Pī space group, with a=1.2462(3) nm, b=1.2652(3) nm,c=1.8420(4) nm,α=87.45(3)°,β=79.91(3)°,γ=82.57(3)°,Z=1, R1=0.0778,wR2=0.1610.Structural analysis reveals that Sm3+(1) coordination cation has incorporated into the vacant site of [α-SiW11O39]8- entity,forming the [α-SiW11O39Sm(H2O)4]5- subunit.The two adjacent [α-SiW11O39Sm(H2O)4]5- subunits are combined with each other through two Sm(1)-O-W bridges accompanying the formation of dimmer structural unit [α-SiW11O39Sm(H2O)4]210- of the title compound.The neighboring dimmer structural units [α-SiW11O39Sm(H2O)4]210- are linked to form the 1D chainlike structure by means of two Sm3+(2) and a Na+(1) coordination cations.The K+(1) cations connect the 1D packing chains constructing the 2D netlike structure, and adjacent netlike layers are also grafted by K+(2) cations to build the novel 3D infinitely extended structure.The result of TG-DTA curves manifests that the decomposition temperature of the title polyanionic framework is 554℃.The cyclic voltammetry measurements show that the title polyanion has the two-step redox processes in aqueous solution with pH=3.1.Variable temperature magnetic susceptibility indicates the title compound obeys the Cruie-Weiss Law in the higher temperature range from 110 to 300 K, while in the lower temperature range from 2 to 110 K the comparatively strong antiferromagnetism interactions can be observed.     

Zur Kristallchemie der Kupfer-Lanthanoid-Oxowolframate: (I) triklin-α-CuTbW2O8, (II) monoklin-CuInW2O8 und (III) monoklin-CuYW2O8

The Crystal Chemistry of Copper Rare-Earth Oxotungstates: (I): triclinic-α-CuTbW₂O₈, (II): monoclinic-CuInW₂O₈ and (III): monoclinic-CuYW₂O₈ Single crystals of (I), (II) and (III) were prepared by recrystallisation in closed systems and examined by X-ray technique. (I): space group C? P1 , a = 7.3080, b = 7.8945, c = 7.1476 Å, α = 115.23, β = 116.21, γ = 56.98°, Z = 2; (II): space group C? C2/c, a = 9.6576, b = 11.6496, c = 4.9863 Å, β = 91.17°, Z = 4; (III): space group C? P2/n, a = 10.0504, b = 5.8214, c = 5.0224 Å, β = 94.23°, Z = 2. The crystal structures are discussed with respect to calculations of the coulombterms of lattice energy and possible valence states of Cu²⁺ and Mo⁵⁺.     

配合物Cu_2（C_（21）H_（20）N_2O_3）（CH_3COO）_2的EXAFS研究

用延伸Ｘ射线吸收精细结构（ＥＸＡＦＳ），测定了标题化合物中两个铜原子的配位结构。两个铜原子有相同的配位，确认每个铜原子均与一个氮原子，三个氧原子形成四配位结构。一氧一氮源于ＨＳＢ，而另两个氧由乙酸提供。     

Synthesis and Crystal Structure of Squarate Complex ［CuLaSm（C_4O_4）_4（H_2O）_（16）］·2H_2O

ＳｙｎｔｈｅｓｉｓａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆＳｑｕａｒａｔｅＣｏｍｐｌｅｘ［ＣｕＬａＳｍ（Ｃ_４Ｏ_４）_４（Ｈ_２Ｏ）_（１６）］·２Ｈ_２Ｏ￥ＳｈｉＪｉｎｇ－Ｍｉｎ；ＹａｎＳｈｉ－Ｐｉｎｇ；ＬｉａｏＤａｉ－Ｚｈｅｎｇ；ＪｉａｎｇＺｏｎｇ...     

Synthesis，Crystal Structure and Infrared Spectrum of Lanthanum Dinuclear Coordination Compound with Alanine：〔La_2（ala）_4（H_2O）_8〕·（ClO_4）_6

Ｓｙｎｔｈｅｓｉｓ，ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅａｎｄＩｎｆｒａｒｅｄＳｐｅｃｔｒｕｍｏｆＬａｎｔｈａｎｕｍＤｉｎｕｃｌｅａｒＣｏｏｒｄｉｎａｔｉｏｎＣｏｍｐｏｕｎｄｗｉｔｈＡｌａｎｉｎｅ：〔Ｌａ_２（ａｌａ）_４（Ｈ_２Ｏ）_８〕·（ＣｌＯ_４）_６...     

[(C_5H_4CH_3)_2HoN_4CPh]_2·[(C_5H_4CH_3)(C_5H_5)HoN_4CPh]_2的合成和晶体结构

（C5H4CH3）3Ho和（C5H4CH3）2Ho（C5H5）与5-苯基四唑（HN4CPh）在THF中反应，得到复合产物[（C5H4CH3）2HoN4CPh]2·[（C5H4CH3）（C5H5）HoN4CPh]2，该晶体属三斜晶系，P1空间群，晶胞参数为a=9．386（3），b=13．071（3），c=16.571（2）A，a=86．90（1），β=74．61（2），γ=77.30（2）°，V=1912．2（8）A3，Z=1，Dc=1.602g／cm3，Mr=922．61，μ=41．92cm－1，F（000）=896，最终偏离因子R=0．041，Rw=0．056．晶体数据显示，在同一个晶胞里有两个组成不同的分子，每一个分子都是具有对称中心的四唑基桥二聚体结构，其桥环单元-HoN3HoN3-是平面型的。每个钬原子分别被两个茂基和3个四唑基氮原子配位，形成1个边桥变形四面体构型。     

K8[ZnMg(H2O)W11O39]·15H2O的合成、表征及化学热扩渗

利用直接法合成未见文献报道的K8[ZnMg(H2O)W11O39]·15H2O,通过ICP,IR和XRD等方法对其结构进行表征,结果表明所合成的配合物具有Keggin结构.采用化学热扩渗法对合成配合物进行稀土扩渗实验,经XPS测试表明,有微量的钆渗进配合物的体相,并与组成元素存在键合作用,导电性测试结果表明,扩渗后试样的导电率提高105倍,是一种优良的固体电解质,有望成为具有实用价值的功能材料.     

Zur Kristallchemie der Blei-Lanthanoid-Oxoaluminate. Zur Kenntnis von Pb2HoAl3O8 und Pb2LuAl3O8

Crystal Chemistry of the Lead Lanthanide Oxoaluminates. On Pb₂HoAl₃O₈ and Pb₂LuAl₃O₈ . Single crystals of (I) Pb₂HoAl₃O₈ and (II) Pb₂LuAl₃O₈ were prepared by flux technique and investigated by X-ray methods. It crystallizes with cubic symmetry, space group O–P4₂/n 3 2/m, (I): a = 9.4164(13) Å, (II): a = 9.3486(8) Å, Z = 4. The new structure type shows AlO₄ tetrahedra, LnO₈ hexagonal bipyramids and one sided coordinated Pb²⁺ within heterocubane units. The crystal chemical relationships to other lead oxides containing heterocubane Pb₄O₄ units are discussed.     

A Novel 3D Extended Network Cobalt Paradodecatungstate:Synthesis,Characterization and Crystal Structure of [Co(H_2O)_5]_2[Co(H_2O)_4]_3[H_2W_(12)O_(42)]·11H_2O

1 INTRODUCTION Polyoxometalates are the unique metal-oxygen clusters composed of transition metals in groups V and VI (Mo, W, V, Nb, Ta) in a high oxidation state showing a large structural varieties as well as inte- resting physical and chemical properties in diverse fields including catalysis, analytical chemistry, nanotechnology, chemical sensing, biochemical and geochemical processes, medicine and materials science[1～5]. Recently, there has been increasing interest in the synthesis…     

Synthesis,Magnetic Property and Crystal Structure of a Ytterbium-Copper Mixed Metal Complex:Yb_2Cu_3L_6·6H_2O (L=O(CH_2COO)_2)

1INTRODUCTIONThesynthesisofpolynuc1earmixedcopper-lanthanoidcomplexesisofinterestforseveralreasons[l-4i.Thesecomplexesareimportanttotheunderstandingofthenature0fthemagneticexchangeinteractionsbetweenrareearthandtransiti0n-metalions,andtheycanpossib1ybeusedasmagneticmaterialst2'33andhightemperaturesuperconductors"'.Itwasbelievedthatthemultidentatepoly-carboxylateacidsisgoodligandsforthepreparationoftheLn-Cumixedmetalcomplexesasthemetalionscanbebridgedbythebidentatecarboxylategroups.Thedig…     

CRYSTAL STRUCTURE OF ERBIUM (HI) COMPLEX WITH 5-SUL-FOSALICYLIC ACID[Er (SO_3C_8H_3(OH)CO_2) (H_2O)_7] [Er (SO_3C_6H_3-(OH)CO_2)_2(H_2O)_6]·8H_2O

<正> [Er(SSA)(H2O)7][Er(SSA)2(H2O)6]·8H2O (H2SSA = 5-sul-fosalicylic acid), Mr=1361.3, monoclinic,P21/c, a = 21.459(7), b = 10.125(2), c = 22. 033(5)(?), β=109. 07(2)°, V = 4524(2)(?)3, Z = 4, D,= 1. 998g/cm3, μ (MoKa) = 40. 6cm-1, F(000)=2704, R = 0. 038 for 5805 observed reflections. The Er(Ⅲ) ions in-both complex cation and anion are coordinated by unidentate SSA ligand(s) and water molecules in a trigondodecahedral geometry. The coordination polyhedra are connected with each other by hydrogen bonds involving the uncoordinated carboxylato oxygen atoms and the coordinated water molecules. Stacking interactions between the phenyl rings further stabilize the structure.     

含稀土超强酸催化剂S2O8^2-/ZrO2-SiO2-Sm2O3的结构表征

目前有很多关于硫酸促进性固体超强酸催化剂的研究报道[1],其中硫酸浸渍氧化锆这类催化剂易制备,对于骨架异构、酯化和其他反应具有很高的活性.近年来,关于这类催化剂的制备、表征和应用的报道很多[2,3].     

A Novel Ni-capped Silverton-type Complex: H_4{[Ni(H_2O)_3]_2[CeMo_(12)O_(42)]}·13.5H_2O

1 INTRODUCTION Polyoxometalates are metal-oxygen clusters with almost unrivaled versatility, which results from their enormous structural variety, range of sizes, tunable redox properties and fascinating catalytic activi- ties[1~7]. Therein, an important progress in transition metal oxide cluster chemistry has been the study of polyoxoanion-substituted and supported inorganic or organometallic complexes[8, 9]. However, modified polyoxoanions with divalent first-row transition me- tal as c…     

十一钼硅钴杂多蓝H_8[SiMo_(11)Co(H_2O)O_(39)]·20H_2O的合成与晶体结构

采用电解法制备了未见文献报道的杂多蓝H8[SiMo11Co（H2O）O39]·20H2O，通过X-射线衍射测定了其晶体结构，该晶体属单斜晶系，空间群P21；。晶胞参数全矩阵最小二乘法修正至中心原子Si与4个氧形成四面体结构，配原子M（M＝11／12Mo＋1／12Co）与O形成12个MO6八面体结构3个MO6共边形成4个M3O13三金属簇，4个三金属簇与SiO4四面体共角相连形成阴离子结构。     

Hydrothermal Synthesis and Structure of [Mn(C_8H_5NO_4)·H_2O]_n·2nH_2O

1 INTRODUCTION The self-assembly of organic-inorganic hybrid ma- terials is an intriguing area, which is yielding new generations of supramolecular architectures[1, 2]. Coor- dination by transition metals with multifunctional ligands is one of the main design principles. As a rigid multi-dentate ligand, 5-aminoisophthalic acid (AIP) has received considerable attention owing to the variety of bridging abilities[3~8]. It can engage in three types of intermolecular interactions: (1) M-L b…     

Synthesis and Structure of anti-Configuration Complex [Cu(tssb)_2]·2[(H_3O)Cl]·4H_2O

1 INTRODUCTION The complexes of amino acid Schiff base have attracted considerable attention because of their bio- activities[1, 2]. Taurine is a special amino acid in be- ings, and recently the complexes of taurine conden- sation salicylaldehyde Schiff …     

含硫、氮Schiff碱配合物—二水二分之一二甲基亚砜醋酸四邻香草醛缩胺基硫脲合镉（Ⅱ）的合成及晶体结构

Ｘ射线单晶衍射结果表明，三核镉配合物Ｃｄ３［ＣＨ３Ｏ（Ｏ）Ｃ６Ｈ３ＣＨ＝ＮＮＨＣ（Ｓ）ＮＨ２］４·［ＣＨ３ＣＯＯ］２·１／２［ＣＨ３Ｓ（Ｏ）ＣＨ３］·２Ｈ２Ｏ为单斜晶系，空间群为Ｃ２／ｃ，ａ＝３．４２１４（４），ｂ＝１．１５８１（２），ｃ＝１．７９３２（５）ｎｍ，β＝１１９．７６（１）°，Ｖ＝６．１６８ｎｍ３，Ｍｒ＝１４２７．４３，Ｚ＝４，Ｄｃ＝１．５４ｇ／ｃｍ３，μ＝１２．４８ｃｍ（－１），Ｆ（０００）＝２８６０，最后偏离因子Ｒ＝０．０６６．     

希土季铵盐配合物的研究——Ⅴ.[(n-C_4H_9)_4N]_3Nd(NCS)_6的晶体结构研究

合成了硫氰酸合希土酸四丁基季铵盐配合物,测定了它们的远红外光谱及部分配合物的中红外光谱,结果表明,配合物中的NCS~-是以氮原子与Ln~(3+)配位。用X射线单晶衍射法测定了[(n-C_4H_9)_4N]_3Nd(NCS)_6晶体的结构,结果表明,该晶体属单斜晶系,C_c空间群,晶胞参数为:a=25.188(8)(?),b=13.320(6)(?),c=25.322(8)(?),β=121.30(2)°,晶胞体积V=7258.9(?)~3,每一晶胞中有四个配合物分子,中心离子Nd~(3+)与六个来自NCS~-的氮原子配位,这六个氮位于配位正八面体的六个顶角上,构成配阴离子Nd(NCS)_6~(3-),它与三个[(n-C_4H_9)_4N]~+以静电引力结合成中心分子,所以晶体为离子型晶体。