Synthesis and crystal structure of a 1D chainlike rare earth coordinated tungstogermenate:[(CH_3)_4N]_(1.50)H_(3.50)[Gd(GeW_(11)O_(39))(H_2O)_2]·2.5H_2O

AID zigzag polyoxometalate [（CH3）4N]1.50H3.50[Gd（GeW11O39）（H2O）2]·2.5H2O （1） was synthesized by reaction of the monova- cant polyanion [α-GeW11O39]^8- with Gd^3＋ ions in aqueous solution and characterized by IR, UV spectra, ICP, and X-ray crystallography. X-ray single-crystal structural analysis indicated that the title compound crystallized in a monoclinic lattice, C2/c space group with α= 2.8201（5）, b=2.2885（3）, c=2.4033（4） nm, β=123.875 （2）°, V=12.878（4） nm3, Z=8, R1=0.0623, wR2=0.1287. The solid-state structure of the title compound displayed an infinite one-dimensional arrangement built up of [α-GeW11O39]^8- polyanions connected by Gd^Ⅲ cations.

Synthesis, Crystal Structure and Characterization of a One-dimensional Supramolecular Rare Earth Complex of N-(6-(4-Methylpyridinyl))ketoacetamide

A one-dimensional （1D） supramolecular rare earth complex [Nd（NO3）2L2-（C3H6O）][NdL（NO3）4]} （L=N-（6-（4-methylpyridinyl））ketoacetamide） has been prepared and characterized by elemental analysis, IR and electronic spectroscopy, and single-crystal X-ray diffraction. The crystal crystallizes in the triclinic system, space group P1^- with a=0.9146（6）, b=1.2581（8）, c=2.2316（14） nm, α=99.352（10）,β=97.209（9）, γ=103.935（9）°, V=2.422（3） nm3, Dc=1.776 g/cm^3, C33H42N12Nd2O25, Mr=1295.27, Z=2, F（000）=1288, μ=2.217 mm-1, R=0.0508and wR=0.1046 for 5173 observed reflections （I 〉 2σ（I））. In the structure of the title complex,one-dimensional supramolecular double-chains are formed by intermolecular hydrogen bonding interactions.

Synthesis and Structures of A Series of Novel Rare Earth Transition Metal Sulfates

Seven new rare earth transition metal sulfates were synthesized by hydrothermal reactions under conditions slightly above the critical point of water. Their crystal structures were determined from single crystal X-ray data. The compositions of the new compounds can be represented by two general formulae ： REM （OH） 3 （SO4） and RE2M （OH） 3 （SO4） 2F （H2O） with RE = Gd, Tb, Dy ; M = Ni, Cu. Three different crystal structure types were found for the formula REM （OH） 3 （SO4）. The structures of the new compounds all feature infinite chains of REOn coordination polyhedra, which are connected to chains of CuO6 or NiO6 octabedra. The limited size range of the rare earth cations observed in these compounds is most likely because of interactions between the octabedral chains and the chains of REOn polyhedra. The new compounds are closely related to the known yttrium transition metal sulfates.

THE CRYSTAL STRUCTURE OF RARE EARTH COMPLEX WITH AMINO ACIDS Ⅱ The Crystal Structure of Gtutamate Comptex of Erbium Perchtorate

The crystat structure of {[Er;（L—Glu）;（H;O）;]（ClO;）;·3H;O);has been studied by X-ray diffraction. The crystal is monoctinic with space group P2;and cell parameters a=19.987（3） , b=16.505（3） , c=11.040（2） , β=104.69（1）;, V=3538（1） , Z=2, Dc=2.29 g. cm;, μ=53.2 cm;, F（000）=2384. The asymmetric unit contains two complex motecules and four centre ions. Each erbium （Ⅲ） is coordinated by five oxygen donors from four different glutamates and four oxygen donors from the aqua ligand to form a nine coordination potyhedron. The mean distances of Er—0 （carboxylate） and Er—Ow are 2.439 and 2.41 respectivety. The finat R and Rw are 0.043 and 0. 058, respectivety.

Phase Behavior and Crystal Structure of Perovskite-Type Rare Earth Complex Oxides

Several compounds of rare earth complex oxides containing manganese and titanium were synthesized in Ar, and their crystal structures were analyzed by powder X-ray diffraction data and Rietveld method. Structures of A0.67Ln0.33 Mn0.33Ti0.6703（A = Ca or Sr and Ln = rare earth） were found to have orthorhombic symmetry with the space group Pnrna, and their interatomic distances and bond angles were obtained. This space group was also derived from electron microscopic study. Electrical conductivity of Cao.67Ln0.33Mn0.33Ti0.6703 for several rare earth elements showed a semiconducting property with the activation energy of 0.4 eV. Some of these compounds of the strontium system show the antiferromagnetic properties below 10 K.

Syntheses,Crystal Structures and Kinetic Mechanisms of Thermal Decomposition of Rare Earth Complexes with Schiff Base Derived from o-Vanillin and p-Toluidine

Three complexes, [Pr（NO3）3（HL）2] （1）, [Nd（NO3）3（HL）2] （2） and [Er（NO3）3（HL）2] ·0.5H2O （3）, were synthesized from the reaction of a Schiff base ligand 2-[ （4-methylphenylimino）methyl ]-6-methoxyphenol （C15 H15 NO2, HL） with Ln（NO3）3·6H2O （Ln = Pr, Nd, Er）. Characterization by single-crystal X-ray diffraction technique, elemental analysis, molar conductance, FT-IR, UV-Vis, ^1H NMR and thermal analysis shows the title complexes are neutral molecules where the central Ln（ Ⅲ） ion is ten-coordinated in biapical anti-hexahedron prism geometry, with four oxygen atoms of the phenolic hydroxy and methoxy groups in the two bidentate Schiff base ligands and six oxygen atoms provided by the three bidentate NO3 - anions. Additionally, the kinetic mechanism of thermal decomposition of complex 3 was determined with a TG-DTG curves by both integral and differential methods. The functions of thermal decomposition reaction mechanism and the equation of kinetic compensation effect were obtained.

Syntheses and crystal structures of rare earth (Nd, Gd) 1-D chain com-plexes with N-p-tolylsulfonyl-β-alanine

Two rare earth complexes of Ts-β-AlaH with the formula of [Ln2（H2O）4（Ts-β-AlaH）6]n·4nH2O （where Ln = Nd（1）, Gd（2）; Ts-β-AlaH = N-p-tolylsulfonyl-β-Alanine） have been synthesized and characterized by elemental analysis, IR and X-ray diffraction. The results show that the two complexes are isostructural. They crystallize in a monoclinic system with P21/n space group. Crystal data for 1： a = 0.95149（19） nm, b = 1.9012（4） nm, c = 2.2863（5） nm, β= 100.37（3）°, Z= 4, De= 1.509 mg/cm^3, F（000） = 1880, R1= 0.0560, wR2= 0.1564 [I 〉 2σ（/）]; for 2： a = 0.9495（2） nm, b = 1.9037（4） nm, c = 2.2987（5） nm, β= 99.87（3）°, Z = 4, Dc= 1.541 mg/cm^3, F（000） = 1916, R1= 0.0515, wR2= 0.1566 [I〉2σ（I）]. The two complexes are one-dimensional chains and the coordination number of the Nd^3＋ or Gd^3＋ ion is nine.

Syntheses aod Crystal Structures of Rare Earth Complexes with Adamantanecarboxylic Acid, [LnL_3(HL)(H_2O)]_2·2EtOH·2H_2O (Ln=Nd (1), La (2))

The title complexes （LnL3 （HL） （H2O） ]2· 2EtOH·2H2O （Ln= Nd （1）, La （2）, HL=adamantanecarboxylic acid） were prepared and determined by single-crystal X-ray diffraction. Both complexes crystallize in triclinic system with space group P 1^-, cell parameters are： complex （1） a = 1.0556（2） nm, b =1.4913（3） nm, c = 1.4920（3） nm, a = 106.26 （3）°, β=93.51（3）°, γ=97.23（3）°, V=2.2253 （5） nm^3, Dcal=1.409 g · cm^-3, Z = I , F （ 000 ） = 990, μ（Mo Kα） = 1. 225 mm^-1, M, = 1884.50; complex （2） a = 1.0453（2） nm, b = 1.4971（3）nm, c = 1.5052（3） nm, α = 106.07（3）°, β =93.58 （3）°, γ=97.56（3）°, V=2.2391（5）nm^3, Dcal= 1.397 g·cm^-3, Z = 1, F（000） =984, μ（Mo Kα） = 1.015 mm^-1, Mr= 1877.88. The final R and wR are 0. 0396 and 0. 1062 for 8589 （1 ≥ 2σ （I）） observed reflections for complex （1）, 0.0505 and 0. 1344 for 8417 （ 1 ≥ 2σ （1） ） observed reflections for complex （2）, respectively. The crystals are consisted of a binuelear molecule. The coordination geometry of the Ln（ Ⅲ ） ion can be described as trieapped trigonal prism.

STUDY ON SYNTHESIS,CHARACTERIZATION AND STRUCTURE OF A NEW RARE EARTH COORDINATION COMPOUND WITH BENZOIC ACID

In this paper,a new rare earth benzoate coordination compound,[TbL_3(HL)(H_2O)]_2 (HL=C_7H_6O_2=benzoic acid) is synthesized and characterized by elemental analysis DTA,TG,DTC,and IR spectra.The title compound crystallizes in triclinic,space.group P with a=9.148(1),b=11.460(2), c=13.506(2);α=112.76(1),β=91.83(1),γ=91.99(1)°;Z=1;V=1303.3.The final R factor is 0.0235.The rare earth ion is nine-coordinated to form a distorted monocapped square antiprism.

Hydrothermal synthesis and crystal structure study of two novel 3-D mellitates {Nd_2[C_6(COO)_6](H_2O)_6} and {Ho_2[C_6(COO)_6](H_2O)_6}

Two novel 3-D coordination compounds, Nd2[C6（COO）6]（H2O）6 （1）and Ho2[C6（COO）6]（H2O）6 （2）, were hydrothermaily synthesized from mellitic acid and neodymium perchlorate （or holmium perchlorate） in the alkaline aqueous solution and characterized with elemental analysis, TG, IR spectrum, and single crystal X-ray diffraction. The two compounds were isostructural and crystallized in the orthorhombic system, space group Pnnm, with a=1.3531 （4） nm, b=0.6687 （2） nm, c=1.0224（3） nm, V=0.92523（5） nm^3, Z=4, D=2.630 g/cm^3, F（000）=696.0, Goof=1.052. Final R indices [1 〉2∑（Ⅰ）]： R1=0.0195, wR2=0.0382 for 1; a=1.3411 （2） nm, b=0.6586（1） nm, c=1.0116（2） nm, V=0.8935（3） nm^3, Z=4, D=2.877 g/cm^3, F（000）=724.0, Goof=1.061. Final R indices [1 〉2∑（Ⅰ）]： R1=0.0200, wR2=0.0479 for 2. In the two compounds 1 and 2, the mellitic acid ligand, in which all the carboxylate groups were deprotonated, had only one kind of coordination mode to bridge metal ions to form four-connected three-dimensional diamondiod networks.

Synthesis and Crystal Structure of Binuclear Ytterbium Complex with Isonicotinoyl Hydrazone

The ytterbium complex of isonicotinoyl hydrazone was synthesized and the structure was determined by X-ray diffraction analysis. The crystal and molecular structure of the title complex [Yb-2(L)(3)](OH)(3) shows that the complex has two identical nine-coordinated ytterbium ions with each surrounded by N3O6 donor set, Two ytterbium ions are bridged by three phenolate oxygen atoms, The geometry around each ytterbium ions can be considered as a three-capped trigonal prism.

Hydrothermal Synthesis and Crystal Structure of Lanthanum Orotate Supermolecule with A Honeycomb Structure Constructed from Mononuclear Molecules via Hydrogen Bonds

A new complex of lanthanum orotate [La（C5H3N2O4）2（OH）（H2O）6 ]·2（C5H4N2O4）·9H2O was synthesized using a hydrothermal method. The crystal structure was determined with help of single crystal X-ray diffraction analysis. The complex crystallized in orthorhombic system, Cmc2（1） space group. In the complex, the center lanthanum （Ⅲ） ion was nine-coordinated with coordination geometry of a distorted monocapped square antiprism, in which two of the nine coordinated oxygen atoms were from two orotate ligands in a monodentate mode, one oxygen atom from a hydroxyl, and the others from six coordinated water molecules. The mononuclear complex [La（C5H3N2O4）2（OH）（H2O）6 ]·2（C5H4N2O4）·9H2O was linked through the hydrogen bonds into an infinite supermolecular honeycomb structure.

Hydrothermal Synthesis and Crystal Structure of a New Dimeric Lanthanum (Ⅲ) Complex

A new dimeric lanthanum (Ⅲ) complex [La_2(phen)_2(C_7H_3N_2O_6)_6] (phen=1, 10-phenanthroline) was synthesized by the hydrothermal method and determined by single crystal X-ray diffraction analysis. The La(Ⅲ) ion is coordinated to seven oxygen atoms from five carboxylate groups and two nitrogen atoms from a phen ligand, forming a monocapped square antiprismatic geometry. Six carboxylate groups coordinate to two La(Ⅲ) ions in three modes which are chelating bidentate, bridging bidentate and bridging tridentate. The crystal is triclinic with space group P-1, a=1.2030(4) nm, b=1.2962(5) nm, c=1.3330(5) nm, α=104.410(5)°, β=114.048(4)°, γ=100.054 (4)°, V=1.7467 (10) nm^3, M_r=952.46, Z=2, D_c=1.811 g·cm^(-3), F(000)=944, S=1.017, μ=1.320 mm^(-1), with R1=0.0298 and wR2=0.0625.

Synthesis and crystal structure of a novel double 1:11 series arsenotungstate: [Cu^I(phen)_2]_5H_6[Sm(AsW_(11)O_(39))_2]·6H_2O

A novel double 1：11 series arsenotungstate, [Cu^I（phen）2]5H6[Sm（AsW11O39）2]·6H2O （phen=1, 10-phenanthroline） was synthesized by the hydrothermal method and characterized by elemental analysis, 1R spectra, and single-crystal X-ray diffraction. The title compound was monoclinic, space group P2 1/c, a=3.75710（2） nm, b=1.39776（8） nm, c=-3.33735（18） nm, β=96.967（10）°, V=17.3969（17） nm^3, Z=4. Single crystal X-ray structural analyses revealed that the dimeric polyanion, [SmAs2W22O78]^1-, consisted of one central Sm^3＋ ion and two tetradentate heteropoly ligands [ASW11O39]^7-. The Sm^3＋ ion and two tetradentate defective [AsW11O39]^7- anions were joined together by the sharing of four oxygen atoms from each heteropoly ligand. The bond valence sum （BVS） calculations of the title compound suggested that all four Cu atoms were in the ＋1 oxidation sate.

Synthesis, Crystal Structure and Fluorescent Properties of a New One-Dimensional Polymer [Sm(sal)_4(phen)_2Na]_n

The title complex, [Sm(sal)_4(phen)_2Na]_n (Ⅰ), where Hsal=salicylic acid, phen=1, 10-phenanthroline, was synthesized by the reaction of samarium chloride with phen and Hsal in ethanol solution and its crystal structure was determined by X-ray diffraction. The crystal is monoclinic, space group C2/c with cell dimensions of a=2 84989 (7) nm, b=0 93347 (2) nm, c=2.27954 (5) nm, β=132.4010 (8)°, V=4.4781 (2) nm^3, Z=4, μ (Mo Kα)=13.97 cm^(-1), D_c=1.605 g·cm^(-3). The title complex is a compound, with centre of the Sm and Na atoms which are bridged by two carboxylate ligands. The structure of the complex demonstrates one-dimensional chain bridged by carboxyl groups. The fluorescence spectrum of the complex indicates that the second ligand phen shows enhancement effect on the fluorescence of the complex.

Synthesis,crystal structure and fluorescence of a new europium complex with 2-bromobenzoate and 2,2'-bipyridine

A new complex of {[Eu2(2-BrBA)6(2,2’-bpy)2]2·CH3CH2OH·H2O} (2-BrBA=2-bromobenzoate; 2,2’-bpy=2,2’-bipyridine) was prepared by solvent method and characterized with X-ray single-crystal diffraction, IR spectroscopy, UV spectroscopy, and fluorescence spectroscopy. The complex crystallized in triclinic crystal system, Pī space group, with a=1.17196(4) nm, b=2.36142(9) nm, c=2.59151(9) nm, α=113.266(2)°, β=101.100(2)°, and γ=94.400(2)°. Two independent dinuclear molecules were contained in the asymmetric unit. The two molecules were similar to each other. Each Eu(Ⅲ) ion was nine-coordinated with seven oxygen atoms from five 2-BrBA ligands and two nitrogen atoms from 2,2’-bpy molecule. The carboxylate groups acted as bidentate-chelating, bidentate-bridging and chelating-bridging coordination modes. The complex adopted a distorted monocapped square-antiprism coordination geometry. Five peaks at 579, 591, 613, 652, and 697 nm appeared in the fluorescence spectrum, corresponding to 5D0→7F0, 5D0→7F1, 5D0→7F2, 5D0→7F3, and 5D0→7F4 transition emissions of the Eu(Ⅲ) ion, respectively.

Synthesis and Crystal Structure of Lutetium Complex withTriethylenetetraaminehexaacetic Acid (H_6ttha):{[Lu_2 (ttha) (H_2O)_6Lu_2 (ttha) (H_2O)_4]·21H_2O}_n

The title complex was synthesized in an aqueous solution and its crystal structure was determined by X-raydiffraction method. It crystalizes in triclinic crystal system, space group P1, formula C36H110N8O55Lu4, Mr=2235.2,a=1.09787(7) nm, b=1.27603(10) nm, c=1.45903(10) nm; α=75.769(6)°, β=85.288(5)°, γ=71.577(6)°, V=1.8797(2) nm3,Z=1, Dc= 1.975 g·cm-3, F(000)=1106, μ=5.312 mm-1; R1=0.0239, wR2=0.0527 for 7156 reflections with I>2σ (I). In the complex, the lutetium ion is coordinated by two nitrogen atoms andsix oxygen atoms and the coordination number is 8. Its coordination polyhedron can be described as a distorted squareantiprism. The complex is of an infinite chain structure. The complex was characterized by elemental analysis, IR spectra and thermal analysis.

Synthesis and crystal structure of sodium praseodymium polyphosphate, NaPr(PO_3)_4

Reaction of Na2CO3, Pr6O11 and H3PO4 gave the sodium praseodymium polyphosphate NaPr（PO3）4.The title compound crystallized in the monoclinic P21/n space group with a=0.9965（4） nm, b=1.31437（4） nm, c=0.72271（3） nm, β=90.429（3）°, V=0.9465（4） nm3, Z=4, R=0.0493 and wR=0.1266 for 1855 independent reflections.The structure of NaPr（PO3）4 consisted of PrO8 polyhedra sharing oxygen atoms with phosphoric group PO4 to form a three-dimensional framework, delimiting intersecting tunnels in which the sodium ion was located.Each Na＋ ion was bonded to seven oxygen atoms.

Synthesis,crystal structure and characterization of one-dimension complex constructed by terbium(Ⅲ) and 2-iodobenzoate

The complex of [Tb（2-IBA）3（H2O）2]n （2-IBA=2-iodobenzoate） was prepared by solvent method from TbCl3-6H2O and 2-iodobenzoic acid. The crystal structure was determined with X-ray single-crystal diffraction. The X-ray diffraction analysis indicated that the title complex crystallized in triclinic crystal system and Pi space group. The Tb^3＋ ion was coordinated by six oxygen atoms from five 2-IBA ligands and two oxygen atoms from two water molecules, giving a distorted square-antiprism polyhedral geometry. The carboxyl groups were bonded to the Tb^3＋ ions with bidentate-bridging and bidentate-chelating coordination modes. The adjacent Tb^3＋ ions were linked by two bidentate-bridging 2-IBA ligands, forming 1-D chain structure. The fluorescence spectrum of the complex showed four main peaks at 489, 543, 587, and 618 nm, corresponding to ^5D4→^7Fj（J=6-3） transition emissions of the Tb^3＋ ion, respectively.

Synthesis, Characterization and Crystal Structure of Neutral Homoleptic Lanthanide Amide Yb(NPh_2)_3(THF)

A neutral homoleptic lanthanide amide Yb(NPh 2) 3(THF) 2 was obtained by reaction of anhydrous YbCl 3 with LiNPh 2 in THF. The product was characterized by elemental analysis, infrared spectrum and X-ray crystallographic analysis. The crystal data are monoclinic, P2 1/n space group, a=1.2052(2) nm, b=1.9369(3) nm, c=1.6523(2) nm, β=92.79(1)°, V=3.8524(9) nm 3, Z=4, D c=1.417 g·cm -3, μ=24.67 cm -1 (Mo Kα), F(000)=1668, R=0.036, R w=0.039. The central metal ytterbium is coordinated by three terminal NPh 2 groups and two THF molecules to form a five-coordinate distorted trigonal bipyramid. The mean Yb-N bond length is 0.2219(6) nm.