SYNTHESES AND CRYSTAL STRUCTURES, REACTION OF α -THIOPI-COLIN-o-TOLUIDIDE AND ITS ORGANOTIN COMPLEX

<正> α-thiopicolin-o-toluidide and its organotin complex have been synthesized, and both crystal structures have been determined by X-ray analysis. The ligand:C13 H12N2S,Mr = 228. 3,monoclinic,P21/n,a=16. 387(1),b = 7. 752(2),c=18. 334(1) A ,β=95. 52(1),V = 2324. 8A3,Z = 8,DC=1. 305g·cm-3,F(000) = 960e. The final R= 0. 053 for 3291 observed unique reflections. There are two molecules in the asymmetric unit,which are confirmed to exist as the keto,cis-N configuration in the solid state. The complex:C17H21N2SClSn,Mr = 439. 6,orthorhombic,P212121,a = 8. 801(3),b = 9. 188 (2),c=24. 087(6) A,V=1947. 9A3,Z = 4,DC=1. 499g·cm-3,F(000) = 880e. The final R = 0. 041 for 1694 observed unique reflections. The tin atom is surrounded by an irregular (5 + 1) coordination geometry with five normal bonds and one weak bond [Sn....C1]. The molecules join each other through the weak bonds to form infinite polymeric chains parallel to the a axis. In addition, the possible reaction mechanism in coordination is discussed.     

STUDIES ON SCHIFF BASE COMPLEXES——Ⅳ. SYNTHESIS AND CRYSTAL STRUCTURE OF Fe (SALDPT) SAL

制备了Fe(saldpt)sal单晶并作了晶体结构分析。晶体数据:单斜,空间群P2₁/C(#14),a=12.486(5),b=18.502(8),c=10.870(5)Å,β=104.23(3)°,V=2434(2)ų,Z=4,D_c=1.40g/cm³.     

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)°.