Synthesis and Crystal Structure of Neodymium Complex with Glycine [Nd(Gly)(H_2O)_7]Cl_3

The title complex [Nd(Gly)(H 2O) 7]Cl 3 was synthesized and its crystal structure was determined by X ray diffraction to obtain a final R value of 0 026 0 and a wR value of 0 086 8. The crystal is of monoclinic system with a space groug Pm . Every two neodymium ions in the crystal are connected with a carboxyl group to form a polymeric chain molecule. And each neodymium ion is further coordinated with seven oxygen atoms from water molecules. The counter ion(Cl -) is non coordinated to fill up the space between the polymeric chains. So the Nd 3+ cation is nine coordinated and the coordination polyhedron is a trigonotetradecahedron. In addition, there exists the mirror symmetry in the complex.

SYNTHESIS AND CRYSTAL STRUCTURE OF NEODYMIUM COMPLEX OF 1-METHYL-1,4,7,10-TETRAAZACYCLODODECANE

The complex [Nd(L)(CH_3CN)(CF_3SO_3)_3] has been synthesized, where L=1-methyl-1,4,7,10-tetraazacyclododecane. The crystal structure of the complex has been determined by a fourcircle X-ray diffractometer to a final R value of 0.0370 and Rw value of 0.0385 respectively. The crystal is triclinic system, space group P1 with a=8.738(2), b=12.870(3), c=12.900(3), α=85.63(2), β=87.25(2), γ=78.30(2)°, V=1415.71(60)~3, Z=2, Dc=1.92g/cm^3. The neodymiumion is eight-coordinated, forming a distorted square antiprism.

Synthesis and Crystal Structure of Neodymium Complex [Nd(C_6H_4OHCHNC_2H_4NCHC_6H_4OH)(NO_3)_3(CH_3SOCH_3)]

The title complex was obtained by reaction of hydrated neodymium(Ⅲ) nitrate with N,N-disalicyclideneethylenediamine in DMSO. The complex [Nd(C_6H_4OHCHNC_2H_4NCHC_6H_4OH)(NO_3)_3(CH_3SOCH_3)] crystallizes in monoclinic system, space group- P2_1/n, a=9.663(2), b=16.610(6),c=16.322(5),β=102.77(2)°,V=2555(3),M_r=676.71,Z=4,Dx=1.759 gcm-3. The coordination number of Nd(Ⅲ) is 9 with the geometry of a monocapped square antiprism.All of coordination atoms are oxygen atoms from three bidentate nitrate groups, two dischiff base molecules and one DMSO molecule.

Synthesis and Crystal Structure of Bis(tert-butyl-cyclopentadienyl)Erbium Ethoxide, (t-BuCp)_2ErOEt

The formation of ( t BuCp) 2ErOEt was discussed. Its single crystal structure was determined by X ray diffraction. The crystal is monoclinic, P 2(1)/ c space group, a =1.0191(2), b =1.6203(5), c =1.2118(3) nm, β =102.960(10)°, V =1.9500 (nm 3), Z =2, D c=1.566 mg·m -3 , R =0.0450, R w=0.1363. The complex is monomeric and solvent free in the solid state. The erbium ion is coordinated by two tert butyl cyclopentadienyl rings and one oxygen atom of ethoxy group to form a seven coordinated complex.

Synthesis and Crystal Structure of Neodymium Heteropolymolybdate Complex Na_4(NH_4)_(10)[Nd_4 Mo_(29)O_(100)(H_2O)_(16)]·34H_2O

Single crystals of the title complex Na4 (NH4)10[Nd4Mo29O100(H2O)16]·34H2O obtained from the reaction of (NH4)6Mo7O24 and Nd (NO3)3, crystallize in themonoclinic, space group C2/c, with a= 19. 556(8), b= 43. 22 (2), c= 20. 389 (7) A,β= 117. 43(3)°, V= 15297(10) A3, Z=4, Dc= 1. 331g· cm-3, F(000) =5824, μ=1. 875 mm-1, final R(wR) = 0. 0816 (0. 2039) for 6128 unique intensity data [I≥2σ(I)]. In the molecule, each Nd heteroatom is coordinated by nine oxygen atoms with amono-capped square-antiprism configuration[1], while the Mo (VI) ions have severaldifferent coordination numbers (4, 5 and 6) with different configurations such as tetra-hedron, distorted square pyramid and octahedron respectively.

Synthesis and Crystal Structure of Neodymium Complex[Nd (C_(18)H_(20)N_2O_4) (NO_3)_3]

The title complex (Nd (C18H20N2O4) (NO3)3] was prepared and char-acterized by X-ray diffraction. The complex crystallizes in monociinic system, spacegroup P21/n, a= 14. 220(5) A, b= 11. 777(3) A, c= 14. 812(4) A, β= 105. 28(3)°, V= 2393(2) A3, Mr= 658. 63, Z=4, Dx= 1. 828 g/cm3, F(000) = 1308, thefinal R= 0. 053, Rw= 0. 065. In the complex the coordination number of Nd(Ⅲ) is 10with the geometry of a bicapped square antiprism. All of the coordination atoms areoxygen atoms.

Synthesis and Crystal Structure of a Cyano-bridged Bimetallic Complex:[NdFe(CN)_6(DMF)_4(H_2O)_3]H_2O

A new bimetallic cyano-bridged complex, [NdFe(CN)6(DMF)4(H2O)3]H2O (DMF = N,N-dimethylformamide) 1, has been obtained by the reaction of hexacyanoferrate potassium with neodymium (Ⅲ) chloride in H2O/EtOH/DMF (volume ratio: 2:2:1), and its structure was determined by means of single-crystal X-ray diffraction. The compound crystallizes in space group P21/n of monoclinic system with cell parameters: a = 17.646(1), b = 8.9011(3), c = 19.945(1) ? b = 95.835(2)? V = 3116.6(3) ?, Z = 4, Dc = 1.536 g/cm3, Mr = 720.66, F(000) = 1456, m = 2.166 mm-1, R = 0.0386, wR = 0.1120 and S = 1.061. The central Nd (Ⅲ) ion is coordinated by seven oxygen atoms of four DMF molecules and three water molecules and one nitrogen atom of the bridging cyanide in a slightly distorted square-antiprism arrangement, and the Fe (Ⅲ) ion is in an almost octahedral environment coordinated to six cyano-ligands, of which one cyanide ligand bridges the Nd (Ⅲ) ion to form a bimetallic complex. Molecules of complexes in the crystal lattice are held together by hydrogen bonding, forming a three-dimensional framework.

Synthesis, Crystal Structure and Optical Properties of a New Nd(III) Nitronyl Nitroxide Complex [Nd(NIT2Py)_2(NO_3)_3]

A new Nd（Ⅲ） nitronyl nitroxide complex [Nd（NIT2Py）2（NO3）3] （NIT2Py = 2-（2＇-pyridyl）-4,4,5,5-tetramethylimidazoline-l-oxyl-3-oxide） has been synthesized and structurally characterized by X-ray diffraction. It crystallizes in monoclinic, space group P21/n with a = 12.396（4）, b =11.134（4）, c = 23.360（7） A°, β = 98.178（6）°, V= 3191.2（18） A°^3, C24H32N9NdO13, Mr = 798.83, Dc =1.663 g/cm^3, μ（MoKa） = 1.704 mm^-1, F（000） = 1612, Z = 4, the final R = 0.0425 and wR = 0.0957 for 6532 independentreflections with Rint = 0.0642 and 4552 observed reflections （I 〉 2σ（I））. The complex exists as discrete mononuclear molecules and the neodymium（Ⅲ） ion is ten-coordinated with three bidentate nitrate anions and two radical ligands （NIT2Py） via bidentate chelating mode.The optical properties of the complex are discussed.

Studies on Organolanthanide Complexes(L)——Syntheses and Crystal Structures of(CH_3OCH_2CH_2C_5H_4)_2 SmI and(CH_3OCH_2CH_2C_5H_4)SmI_2·2THF

Reactions of samarium triiodides with 2 equivalents of potassium 2-methoxyethyl- cyelopentadienyl or 1 equivalent of potassium 2-methoxyethylcyclopentadienyl in tetrehydrofuran afford bis- (2-methoxyethylcyclopentadienyl) samarium iodide complex Cp′_2 SmI 1 (Cp′=MeOCH_2CH_2C_5H_4),and (2- methoxyethylcyclopentadienyl) samarium diioidide complex Cp′SmI_2·2THF 2.Compound 1 crystallizes from THF/hexane in orthorhombic space group P2_12_12_1 with cell dimensions a= 11.074(4),b= 12.929(9), c=12.269(4) ,V=1756.9 ~3 and D_(cacld)=1.978 g/cm^3 for Z=4.The central metal Sm is coordinated with two Cp′ ring centroids,one iodine atom and two oxygen atoms of Cp′ forming a distorted trigonal bipyramid.The coordination number of Sm (Ⅲ) in 1 is 9.The crysal of 2 belongs to the monoclinie crystal system,space group P2_1/c with a=16.304(6),b=8.335(2),c=16.527(5) ,β=111.8 (1)°,V= 2085.3 ~3 D_(cacld)=2.138 g/cm^3 and Z=4.The central metal Sm is coordinated by one Cp′ ring centroid, two iodine atoms,one oxygen atom of Cp′ and two oxygen atoms of THF forming a distorted octahedron. The coordination number of Sm (Ⅲ) in 2 is 8.

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.

Reaction of Bis(Methylcyclopentadienyl) Lanthanide Amido Complex with n-Hexyl isocyanate-Synthesis and Characterization of {(MeC_5H_4)_2YbOC(NPh_2)N(n-hexyl)}_2

Bis （methylcyclopentadienyl） lanthanide amido complex （MeCp） 2YbNPh2 （THF） reacted with n-hexyl isocyanate （n-nexylNCO） in 1：1 molar ratio to give {（MeC5H4）2Yb[OC（NPh2）N（n-hexyl）] }2（1）. Complex 1 was characterized by elemental analyses and X-ray diffraction. The title complex belongs to trigonal system and R-3 space group. Its unit cell parameters are a =2.9533（11） nm, b =2.9533（11） nm, c = 1.5873（6） nm, V= 11.9896（80） nm^3, Z =9, Dc= 1.562 mg·m^-3, μ = 3.536 mm^-1（Mo Kα）, F（000） =5670, R =0.034, Rw =0.064. It is a dimeric structure with two symmetrical bridged oxygen atoms. Nitrogen atom is coordinated to the ytterbium atom to form a tricyclic backbone. The coordination number of ytterbium is 9. The whole molecule shows central symmetry.

Crystal Structure of{[(μ_2-Cl)(C_5H_5)Sm(μ_2-Cl)]_2(μ_3-Cl)(μ_4-O)Sm(μ_2-Cl)·THF}_2^(2-)·[Li(DME)_2·Li(THF)_2·DME]^(2+)·DME

The crystal structure of title complex has been determined by the method of X-ray single crystal diffraction.The crystal belongs to monoclinic space group C_(2/c)with the unit parameters a=2.8907(7), b=2.0431(5),c=1.5723(3)nm;β=115.67(2)°.The unit volume V is 8.36924(348)nm^3;Z=8, Dc=1,82g·cm^(-3),μ(MoK_α)=46.4cn^(-1); F(000)=4416.The final R is 0.083,Rw 0.088.The title complex con- sists of two univalent cations and one divalent anion.The anion has a cluster structure including six Sm^(3+). Coordination numbers of all six Sm^(3+)are eight,but their surroundings are different from each other.Two of them are decahedral array,and the others are octahedral array f the centroid of each pentacyclodienyl ring is taken as one point.

Solvothermal Synthesis,Crystal Structure and Properties of a 3D Organically Amine Templated Lanthanide Sulfate

A new sulfate inorganic framework, {（C2H8N）9[Nds（SO4）12]·2H2O}n （1） templated by organic amine, has been solvothermally synthesized and characterized by TGA, PXRD and single-crystal X-ray diffraction. Compound 1 crystalizes in monoclinic, space group C2/c with a = 20.570（5）, b = 35.815（8）, c = 10.106（2） A, C108H72NgNd5050S12, Mr = 2315.73, V= 6765（3） A3, Z = 4, Dc = 2.274 g·cm-3, μ = 4.253 mm-1, F（000 = 4520, 2.52〈θ〈25°, λ（MoKa） = 0.71073 A, T= 273（2） K, the final R =0.0401, wR = 0.1022 and S = 1.042. X-ray diffraction analysis reveals that complex 1 possesses a 3D inorganic sulfate framework with large 20-membered ring （20 MR） and 10-membered ring （10 MR） channels constructed by two kinds of SBUs. Moreover, the UV-vis and luminescent properties of comolex I were also investigated

Synthesis and Crystal Structure of[C_6H_5CH_2C_5H_4ErCl_2(THF)_3]·THF

C_6H_5CH_2C_5H_4ErCl_2(THF)_3]·THF, Mr=681.9, monoclinic,space group P2_1/n, with a=11. 622(5), b=10. 281(4), c=26. 040(5),β=86. 65 (4)°,V=3106 (3), Z=4, Dc=1. 46 gcm￣(-3),μ=30. 0 cm￣(-1), F (000)=1380. The final R value is 0. 040 for 1911 independent observed reflections (I>3σ(I)). The geometry around the erbium ion is described as an approximate octahedron with the centroid of the benzylcyclopentadienyl rings, the oxygens of three THF's and two chlorine atoms forming the apices of the octahedron. The average distance of Er-C(Cp'ring) is 2. 66A.

Crystal Structure and Raman Spectrum of Neodymium（Ⅲ） Complex of p－Aminobenzoic Acid and 1，10－Phenanthroline

Crystal structure of tetra(1,10-Phenanthroline)neodymium (Ⅲ) tetra(4-aminobenzoate)-hydrate, [Nd(p-ABA)4·2Phen]H+3O·2Phen (p-ABA:p-aminobenzoate,Phen:1,10-phenanthroline) has been determined by X-ray diffraction.The complex crystallizes in monoclinic, space group C2/c.The cell dimensions are a=1.9067 (5) nm,b=1.9192 (3) nm,c=2.0190 (4) nm,β=117.25 (2) °.V=6.568 (3) nm3, Mr= 1428.63,Z=4 and Dx= 1.45 g·cm-3.The coordination number of Nd atom is 10, and the coordinated polyhedron around the Nd atom is distorted trigonal prism.

Synthesis and Characterization of Ethylthioethylcyclopenta-dienyl Organolanthanide Complexes:Cp_2^(Th)LnCl(Ln=Gd,Dy),Cp_2LnCp^(Th)(Ln=Yb,Sm,Dy,Y) and Cp^(Th)ErCl_2·2THF

Six new ethylthioethylcyclopentadienyl-containing organolanthanide complexes CpTh 2LnCl [Ln=Gd (1), Dy (2)] and Cp2LnCpTh [Cp=C5H5, Ln=Yb (3), Sm (4), Dy (5), Y (6)] were synthesized by the reaction of ethylthioethyl-cyclopentadienyl (CpTh) sodium salt with LnCl3 or Cp2LnCl in THF. Complexes 16 were characterized by ele-mental analyses, infrared and mass spectroscopies. The molecular structures of complexes 13 were also deter-mined by the X-ray single crystal diffraction. The results show that the side-chain sulfur atom on the ethylthio-ethylcyclopentadienyl ring can form intramolecular chelating coordination to the central lanthanide ion, improving the stability of organolanthanide complexes and reducing the number of coordinated THF molecules.

Synthesis and Structural Characterization of a Cyano-bridged Dinuclear Neodymium(III)-iron(III) Complex [Nd(DMSO)_5(H_2O)_2](μ-CN)[Fe(CN)_5]

A new neodymiumIII-ironIII complex [Nd(DMSO)5(H2O)2](μ-CN)[Fe(CN)5] (DMSO = dimethyl sulfoxide) has been synthesized by the grinding reaction method. The crystal belongs to monoclinic, space group P21/m with a = 8.859(4), b = 13.684(5), c = 12.290(4) ?, ?= 91.85(2)o, C16H34FeN6NdO7S5, Mr= 782.88, V = 1489(1) ?3, Z = 2, Dc = 1.746 g/cm3, S = 0.906, μ(MoKa) = 2.606 mm-1, F(000) = 788, R = 0.0646 and wR = 0.1654. The slightly distorted square-antiprism eightfold-coordinated Nd(III) and approximately oriented octahedrally sixfold- coordinated Fe(III) are linked by a cyano-bridge group to construct a dinuclear compound. The [Nd(DMSO)5(H2O)2](μ-CN)[Fe(CN)5] species are held together via hydrogen bonds to form a three-dimensional framework.

Structural Studies of Complexes of 1－phenyl－3－methyl－4－benzoyl－5－pyrazolone with Metal Ions（Ⅲ）（Ⅱ） Crystal Structure of 〔Nd(C17H13N2O2)3（H2O）2〕

Nd(C17H13N2O2)3(H2O)2], Mr= 1012. 2, monoclinic, space group C2/c, a=24. 587(5) , b=16. 200(6) , c=25. 804(5) A ,β= 105. 14(3)°, V =9921(2) A3, Z=8, Dx=1. 355 g/cm-3, μ=11. 04 cm-1, F(000) =4120, R=0. 048 , Rw= 0. 058. The Nd(Ⅲ) ion is coordinated by eight oxygen atoms to form a distorted dodecahedral configuration with mean bond length Nd-O of 2. 43 1 (4)A .

Synthesis, Structure and Reactivity of Lanthanocene Complexes

A variety of lanthanocene complexes, e.g. chlorides, hydrocarbyls, amides, hydrides and divalent derivatives, were synthesized by using a series of designed cyclopentadienyl, indenyl and fluorenyl ligands with ring bridges or dornor functionalized sidearms. X Ray crystallographic analyses reveal the formation of intramolecular coordination bonds between central metals and heteroatoms (O, N) in sidearms or bridging chains. Some applications of these complexes are also discussed in this account.