SYNTHESIS AND CRYSTAL STRUCTURE OF La（NO3）3（16—C—5）

<正> The title complex LaC11H22O14N3 (Mr = 559. 27) crystallizes in the monoclinic space group P21/c with a=14. 452(7) ,b=8. 260(2),c= 16. 641(8) A ,β= 90. 85(4)°, Z = 4, V=1986. 2(1) A3,Dc=1. 87g·cm-3, F(000) = 1112,μ(MoKa) = 22. 7cm-1. The final refinement converged with R=0. 036 and Rw = 0. 038 for 2996 observed independent reflectios. The average La-O(crown) bond length of 2. 683 A (2. 660-2. 701A)is shorter than that in La(NO3)3(15-C-5)(2. 694A).The distances between opposite O atoms (3. 47~4. 68A) indicate that the cavity of 16-C-5 in the complex is elliptic.     

SYNTHESIS AND CRYSTAL STRUCTURE OF （C5H5）2Ti（o—NHPhC6H4CO2）2

<正> Cp2Ti(o-NHPhC6H4CO2)2, Mr = 602. 54, space group C2/c, a = 33. 77(2), b = 12. 611(6), c=14. 486(9) A ,β=103. 28(4)°,V = 6004(5) (?)3,Z = 8, Dc= 1. 33gcm-1, MoKa(λ=0. 71069(?)) radiation, μ = 3. 21cm-1, F(000) = 2512e, R = 0. 066, Rw= 0. 085 for 2511 radiations. The Ti atom in the molecule is coordinated by two C5H5 groups and two monodentate carboxyl ligands in a distorted tetrahedral geometry with the bonds in the range of Ti-C = 2. 334 - 2. 41(?) ; Ti-O = 1. 914(5) and 1. 919(5)(?);and the bond angles O-Ti-O = 91. 7(2)°; (cent-C5H5)-Ti-(cent-C5H5) = 135. 9(6)°.     

SYNTHESIS AND CRYSTAL STRUCTURE OF [C8H8NdCl（THF）2]2

<正> The title complex was prepared from the reaction of NdClLi0.3 and C8H8, its crystal structure was determined by single-crystal X-ray diffraction. It crystallizes in the monoclinic space group P21/c with cell dimensions o = 11. 819(3), 6=12.651(3), c=13. 478(3)A, β=122.99(2)°, Mr = 856. 00, Z = 2, Dc=1. 68g/cm3, F(000) = 636. 89, V = 1690. 33A3. The structure was solved by direct methods and Fourier techniques. Least squares refinement on the basis of 1842 observed reflections led to final R = 0. 038 and Rw = 0. 040. The molecule is a dimer of C3H8NdCl(THF)2 bridged by two Cl atoms with Nd -Cl bond lengths of 2. 832(2) A and 2. 917(3)A.     

SYNTHESIS AND CRYSTAL STRUCTURE OF V ^（v）O[N（CH2Ch2O）3]

<正> Reaction of ammonium metavanadate with triethanolamine in ethanol yields the title compound (2,2' , 2"-nitrilotriethoxy)oxo-vanadium (Ⅴ ). The crystal and molecular structure has been determined crystallographically. The complex V(v) O[N(CH2CH2O)3] crystallzes in the monoclinic system, space group P21, a = 7.140(1), 6 = 7.474(2), c=8.040(2) A ,β=92. 48(2)°, V=428. 7(1) A3, Mr= 213.1, Z = 2, F(000) = 220,μ= 10. 95cm-1, Dc= 1. 65gcm-3, final R= 0. 032 and Rw = 0. 034 based on 758 independant reflections with I>2σ(I). The vanadium center is in a distorted trigonal bipyramidal environment of a quadridentate chelating ligand and a terminal oxygen atom.     

SYNTHESIS AND CRYSTAL STRUCTURE OF Eu[（CH3O）2PO2]3

<正> The title complex has been synthesized and characterized by elementary analysis,FT-IR and Raman spectra. The crystal and molecular structure was determined by X-ray diffraction analysis. The crystal of this complex C6H18O12P3Eu(Mr = 527. 08) is monoclinic with space group P21/c and cell parameters a= 10. 418(2) ,b= 16. 596(6) ,c =10. 766(2) A ,β=111. 67(2)°,V=1729. 8(8) A3 and Z=4. Dimethyl phosphate an-ions coordinate with europium ions through double O-P-O bridges to form a special network of rings-linking-rings. The local coordination geometry of Eu is a slightly distorted octahedron.     

CRYSTAL STRUCTURE OF（η^5—C5H5）GdCl2（THF）3

<正> Compound (η5-C5H5)GdCl2(THF)3 was successfully prepared from action of GdCl3 and NaC5H5 in tetrahydrofuran (THF). X-ray diffraction data were collected at low temperature (about 210K). Its crystal belongs to the monoclinic space group P 21/n with a = 7. 821(2), b = 17.068(1), c=15. 057(1)(?), β=94. 76 (2)°, V = 2003. 2(10)(?)3, Z = 4, Dc=1. 69g/cm3, F(000)=1012, Mr=509. 6. The structure was solved by heavy-atom method. Least-squares refinement converged to a final R value of 0. 050. The coordination number of the Gd atom is 8. The centre of the cyclopentadienyl, the two Cl atoms and the three oxygen atoms of THF molecules form a distorted octahedron about the Gd atom.     

SYNTHESIS AND CRYSTAL STRUCTURE OF Nb3（Se2）6I

<正> Nb3(Se2)6I,Mr = 1353. 1, tetragonal, space group D64h-P4/mnc, a= 9. 45(1), b = 9. 45(1) , c=19. 08(3)(?), V = 1705. 6(9)(?)3, and Z = 4, Dc=5. 27g/cm3. Final R = 0. 045 and Rw = 0. 053 for 881 independent reflections with I> 3σ(I). In the structure of Nb3(Se2)6I, the Nb(Se2)4 units are almost regular rectangular antiprism, which are packed in chain forms along c axis with the I (0) atoms between these chains.