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.

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.

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, Structure and Luminescent Properties of Three 1D Chain Rare Earth Complexes

Three 1 D chain coordination polymers [Ln(pydc)2(H2 O)2]n·n Him(Ln = Dy(1), Gd(2), Sm(3), H2 pydc = pyridine-2,5-dicarboxylic acid, Im = imidazole), were solvothermally synthesized by the reaction of pyridine-2,5-dicarboxylic acid(H2 pydc), Ln(Ⅲ) salts and imidazole. They have been characterized by X-ray single-crystal diffraction, IR spectra, TGA analysis and elemental analysis. Structural analyses revealed that complexes 1~3 have similar 1 D chain structures and belong to P1 space group. It is noteworthy that complexes 1~3 exhibited excellent thermal stability and no weightlessness below 117 ℃. Meanwhile, 1 and 3 show characteristic fluorescence of corresponding lanthanide metal ions in solid state at room temperature.

Crystal Structure and Luminescence Property of Lanthanide Complexes with 2-Fluorobenzoic Acid and 2,2′-Bipyridine

The two compounds of [Ln（2-FBA）3·2,2＇-bpy ]2（2-FBA = 2-fluorobenzoato, 2,2＇-bpy = 2,2＇-bipyridine, Ln = Eu（1 ）, Dy（2）） were synthesized and their structures were determined by X-ray diffraction method. Crystallized complexes 1 and 2 are isomorphous, monoelinie system with P21/n space group. The two complexes are binuclear molecule with an inversion center. The two lanthanide ions are linked by four bridged 2-FBA ligands and each lanthanide ion is further bonded to one chelated bidentate 2-FBA ligand and one 2,2＇-bipyridine molecule. The coordination number of metal ion is eight. The europium complex exhibits strong red fluorescence. ^5D0→^7Fj（j = 1 - 4） transition emission of Eu^3＋ ion was observed.

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,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, crystal structure, and fluorescence of two dimeric europium(III) complexes with 2-(trifluoromethyl)benzoate

Two complexes [Eu2（2-TFMBA）6（2,2′-bipy）2]·2H2O （1） and Eu2（2-TFMBA）6（1,10-phen）2 （2） （2-TFMBA=2-（Trifluoromethyl） benzoate; 2,2′-bipy=2,2′-bipyridine; 1,10-phen= 1,10-phenanthroline） were synthesized by solvent method and determined by X-ray diffraction analysis. Complex 1 crystallizes in monoclinic system with space group P21/c, whereas complex 2 crystallizes in triclinic system with space group Pi. Both are binuclear molecules with an inversion center. In complex 1, two center Eu^3＋ ions are linked together by four 2-TFMBA ligands in bidentate-bridging mode. Each Eu^3＋ ion is eight-coordinated with six O atoms from five 2-TFMBA ligands and two N atoms from one 2,2′-bipy molecule. In complex 2, two center Eu^3＋ ions are linked together by four 2-TFMBA ligands in two modes, namely, bidentate-bridging and tridentate-bridging. Each Eu^3＋ ion is nine-coordinated with seven O atoms from five 2-TFMBA ligands and two N atoms from one 1,10-phen molecule. The two complexes both exhibited strong red fluorescence under ultraviolet light, and the ^5D0→^7Fj （j=0-4） transition emissions of Eu^3＋ ion were observed in their emission spectra.

Synthesis,crystal structure and fluorescence property of 1-D europium complex with 2,3-difluorobenzoate

A new chain europium complex [Eu(2,3-DFBA)3·(H2O)2]n(2,3-DFBA=2,3-difluorobenzoate) was synthesized by solvent method.X-ray single-crystal diffraction analysis revealed that Eu3+ ions were linked through 2,3-DFBA groups via alternate bidentate-bridging and tridentate chelating-bridging coordination modes to form a one-dimensional(1-D) polymeric chain.Each Eu3+ ion is eight-coordinated by six O atoms of five 2,3-DFBA ligands and two water molecules.The abundant hydrogen bonds between chains resulted in a two...

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, crystal structure and luminescence of a europium complex with phenylmalonic acid and 1, 10-phenanthroline

A new complex Eu2（PA）6（phen）2 was prepared with hydrothermal reaction using EuCl3.6H2O, phenylmalonic acid （H2phma）, and 1, 10-phenanthroline （phen）, where PA was the decarboxylated product of HEphma, phenylacetate. The crystal structure of the title complex was determined with the X-ray diffraction. The title complex was a binuclear molecule with an inversion center. Each Eu^3＋ ion was nine-coordinated with two nitrogen atoms from one phen molecule and seven oxygen atoms from five PA ligands. The carboxylic groups were bonded to the Eu^3＋ ion in three modes, the chelating bidentate, the bridging bidentate, and the bridging-chelating tridentate. The complex emits intense red fluorescence under ultraviolet light. The luminescence peaks correspond to the characteristic emission 5D0→7FJ （J=0-4） transitions of the Eu^3＋ ion.

Nitrilotriacetate Bridged 3d-4f Heteronuclear Complex: Synthesis and Crystal Structure of ｛[GdCu(NTA)(H_2O)_6Cl]ClO_4·H_2O｝_n

The heteronuclear gadolinium copper complex was synthesized. Its crystal structure was determined by single crystal diffraction. The crystal crystallizes in triclinic, space group P 1, a=0 8483(1) nm, b =0 9642(2) nm, c =1 2838(2) nm, α =111 17(1)°, β = 93 52(1)°, γ =100 89(1)°, Z =2, D c=2 335 g·cm -3 . The complex appears as a zigzag 1D chain. Each gadolinium ion is coordinated by three carboxylic oxygen atoms and six oxygen atoms from H 2O. Each copper ion is chelated by NTA with its nitrogen atom and three oxygen atoms of three carboxyl groups, and coordinated by a chlorine ion. The ClO 4 - is located between the chains as a counter ion.

Synthesis and Crystal Structure of Heteronuclear Complex of Copper and Yttrium with Glycine

The title complex [CuY(Gly) 5(H 2O) 2](ClO 4) 5H 2O was synthesized in aqueous solution and its crystal structure was determined by X ray diffraction method. The crystal is triclinic, space group P 1 with a =1 1751(3) nm, b =1 2410(3) nm, c =1 4448(3) nm, α =72 97(2)°, β =71 82(2)°, γ =60 96(2)°, V =1 7244(6) nm 3, Z =2, d c=2 08 g/cm 3. The crystal is composed of one dimensional chain of infinite length.

Synthesis Crystal Structureof Quaternary Mixed AnionComplex of Lanthanides[Ln(CCl_3COO)_2 (CH_3COO)(phen) (H_2O)]_2

Three new quaternary mixed anion complexes of lanthanides were prepared from thewater-ethanol solution under slightacidity condition and characterizedby elemental analysis, IR, UVspectrum and single crystal X-raydiffraction analysis. The crystal ofLa(CCl3COO)2 (CH3COO) (phen)(H2O)·DMF]2 belongs to tricliniccrystal system, space group P1with a=1 .2510 (4) nm, b=1.3460(5) nm, c=1.0343 (3)nm, α=102.47(3)°, β=102.34(2)°, γ=113.82 (2)°, μ(MoKa) = 20.47 cm-1, Z= 1, Dc=1. 800 g·cm-3, F (000) =780. 00. The acetate tends to coordinate with the center ion as abridge and trichloroacetate has fourkinds of coordination modes, somany coordination modes were observed in their co-ligand system.

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

Reaction of hydrated ytterbium nitrate and copper nitrate with diglycolic acid at pH= 7 produced a new Yb-Cu mixed metal complex, Yb2Cu3L6. 6H2O(L= O(CH2COO)2). Complex Yb2Cu3O36C2H36 (Mr= 1437. 23) crystallized in hexagonalP6/mcc (No. 192) with cell parameters of a= 14. 344 (3), c= 15. 470(7) A,V= 2757(2) A 3; Z= 2; F(000) = 1390; Dcalc.= 1- 731 g/cm3 μ(MoKa) =45. 8 cm-1. The final agreernent factors are R= 0. 077 and Rw = 0.089 for 867 observed reflections with I>3δ(I). It has been characterized by elemental analysis, IR spectrum, magnetic measurement and X-ray crystallography. In the complex, the Yb3+ ion is 9-coordinated tothree ether oxygen and six carboxylate oxygen atoms from three ligands, the copper ionis coordinated to four oxygen atoms from four carboxylate groups of four ligands andtwo water molecules. The Yb3+ ions and the Cu2+ ions are connected by the carboxylate groups of the ligands, thus resulting in the formation of the complicated networkstructure.

Spectroscopy Study on Crystal Structure of Ce(NO_3)_3(phen)_2 and Interactions of Ce(NO_3)_3(phen)_2 with DNA

The absorption, fluorescence and Raman spectra of Ce(NO3)(3)(phen)(2) complex were assigned and the crystal structure of the complex was studied. Meanwhile the interactions between Cc (NO3)(3) (phen)(2) and DNA were studied by spectrum methods. As DNA was added, it is found that both the UV absorption bands of Ce(NO3)(3)(phen)(2) and the SERS bands of Ce(NO3)(3)(phen)(2) weaken evidently, while the fluorescence intensity of Ce(NO3)(3)(phen)(2) enhance dramatically. The complex compete against EB on the reaction with DNA. It is indicated by this spectrum methods that there are strong interactions between Ce(NO3)(3)(phen)(2) and DNA, and the bond mode is intercalation. The bond constant of the complex with DNA is determined to be 1.7 x 10(5).

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.

Synthesis and Crystal Structure of [Yb(NTO)_3(H_2O)_4]·6H_2O

Yb(NTO) 3(H 2O) 4]·6H 2O was synthesized by mixing an aqueous solution of lithium 3 nitro 1,2,4 triazol 5 onate(LiNTO) and the dilute nitric acid solution of ytterbium oxide. The crystal structure has been determined by a four circle X ray diffractometer. The crystal is monoclinic, space group C2/c with crystal parameters a= 3 6931(5) nm, b =0 6683(10) nm, c =2 5656(3) nm, β =130 974(5)°, V =4 7811(11) nm 3, Z =8, d c=2 013 g·cm -3 , μ =4 017 mm -1 , F (000)=2850. The final R is 0 0258, the coordination number of Yb 3+ is seven and the geometry of the ytterbium complex is pentagonal bipyramid.

Synthesis, Crystal Structure of [(MeC_5H_4)_2Ln(μ-OCH_2CH_2NMe_2)]_2 (Ln=Sm, Y, Nd) and Their Catalytic Activity for Ring-Opening Polymerization of ε-Caprolactone

Reaction of (MeC 5H 4) 3Ln with HOCH 2CH 2NMe 2 in tetrahydrofuran(THF) gives the new complexes [(MeC 5H 4) 2Ln(μ OCH 2CH 2NMe 2)] 2 (Ln=Sm, Y, Nd) with nitrogen functionalized μ alkoxide ligand. The complexes were characterized by elemental analysis and IR, and [(MeC 5H 4) 2Sm(μ OCH 2CH 2NMe 2)] 2 was structurally characterized by the X ray diffraction to be a dimer formed by two unsymmetric oxygen bridges. The complex has a tricyclic skeleton with the additional two Sm-N bonds via intramolecular coordination of OCH 2CH 2NMe 2. The coordination number of the central metal Sm is nine. The title complexes show good catalytic activity for ring opening polymerization of ε caprolactone.

Reaction of (C_5H_5)_2NdCl·2LiCl with n-Butyllithium: Formation and Crystal Structure of [Li(DME)_3][(C_5H_5)_3Nd(μ-H)Nd(C_5H_5)_3]

The reaction of the THF solution of （C5H5）2NdCl· 2LiCl with n-butyllithium was studied and the neodymium hydride complex, [ Li （ DME ）3 ] [ （C5H5）3Nd （μ-H） Nd （ C5H5 ）3 ] 1 was isolated from the reaction solution. Complex 1 was crystallized from a mixture solvent of THF-DME and structurally characterized by single crystal X-ray diffraction method at - 80 ℃. The crystal is monoclinic, space group P21/c with unit cell dimensions a = 0.9670（2） nm, b =2.1001（5） nm, c=2.1279（7） nm, β=9.089（2）°, Z = 4. The structure was solved by heavy atom method and refined by the least-squares method to a final R = 0.094. The complex consists of disconnected ion pairs of [ Li （ DME ）3 ]^＋ and [ （ C5H5 ）3Nd （μ-H） Nd （C5H5）3]^-. The neodymium atom is coordinated by three η5-cyclopentadienyls, and two （C5H5）3Nd species are connected by one hydrogen bridge to form the anion with Nd-H 0.218（1） nm.