SYNTHESIS OF EARLY TRANSITION-METAL PORPHYRIN HALIDE-COMPLEXES - FIRST STRUCTURAL CHARACTERIZATION OF A VANADIUM(III) PORPHYRIN COMPLEX

被引:38
作者
BERREAU, LM [1 ]
HAYS, JA [1 ]
YOUNG, VG [1 ]
WOO, LK [1 ]
机构
[1] IOWA STATE UNIV SCI & TECHNOL,DEPT CHEM,AMES,IA 50011
关键词
D O I
10.1021/ic00079a020
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
A general method for the preparation of early transition metal porphyrin halide complexes using a porphyrin dianion, (THF)(2)Li-2(POR) (POR=OEP, TTP;OEP=octaethylporphyrinato, TTP=meso-tetra-p-tolylporphyrinato), and the appropriate metal halide complex, MX(n) (MX(n) VCl3(THF)(3), TiCl4(THF)(2), TiCl3(THF)(3), MoCl4(CH3CN)(2), WCl4), is described. The structure of (TTP)(VCl)-Cl-III.THF (2.THF) has been determined by single-crystal X-ray diffraction analysis. Complex 2.THF crystallizes in the centrosymmetric space group P2(1)/m with alpha=11.968(2) Angstrom, b=17.072(3) Angstrom, c=12.649(2) Angstrom, beta=98.62(2)degrees, V=2555.2(8) Angstrom(3), Z=2, R=4.6%, and R(w)=6.7%. The V-Cl bond length is 2.272(1) Angstrom, the V-N bond lengths range from 2.040(4) to 2.050(3) Angstrom, and the V-O bond distance is 2.141(3) Angstrom .
引用
收藏
页码:105 / 108
页数:4
相关论文
共 42 条
[1]   A SIMPLIFIED SYNTHESIS FOR MESO-TETRAPHENYLPORPHIN [J].
ADLER, AD ;
LONGO, FR ;
FINARELLI, JD ;
GOLDMACH.J ;
ASSOUR, J ;
KORSAKOF.L .
JOURNAL OF ORGANIC CHEMISTRY, 1967, 32 (02) :476-+
[2]   A METALLOPORPHYRIN CARBORANE SANDWICH COMPOUND - SYNTHESIS AND X-RAY CRYSTAL-STRUCTURE OF (OEP)ZR(ETA-5-1,2-C2B9H11) [J].
ARNOLD, J ;
JOHNSON, SE ;
KNOBLER, CB ;
HAWTHORNE, MF .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1992, 114 (10) :3996-3997
[4]   NOVEL SYNTHETIC ROUTE TO SCANDIUM PORPHYRIN DERIVATIVES AND THE 1ST STRUCTURALLY CHARACTERIZED METALLOPORPHYRIN-ETA-5-CYCLOPENTADIENYL SANDWICH COMPOUND [J].
ARNOLD, J ;
HOFFMAN, CG .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1990, 112 (23) :8620-8621
[5]   DIAMAGNETIC REVERSIBLE PARAMAGNETIC EQUILIBRIA IN SOLUTIONS OF BIS(DIALKYLPHOSPHINO)ETHANE COMPLEXES OF IRON [J].
BAKER, MV ;
FIELD, LD ;
HAMBLEY, TW .
INORGANIC CHEMISTRY, 1988, 27 (16) :2872-2876
[6]   MOLECULAR-STRUCTURE OF METHOXOTITANIUM(III) TETRAPHENYLPORPHYRIN, A SLIGHTLY BENT METHOXO COMPLEX [J].
BOREHAM, CJ ;
BUISSON, G ;
DUEE, E ;
JORDANOV, J ;
LATOUR, JM ;
MARCHON, JC .
INORGANICA CHIMICA ACTA-ARTICLES, 1983, 70 (01) :77-82
[7]   EARLY TRANSITION-METAL PORPHYRINS - SYNTHESIS AND REACTIVITY OF SOME NOVEL ZIRCONIUM DERIVATIVES AND THE X-RAY CRYSTAL-STRUCTURE OF THE 1ST METALLOPORPHYRIN CIS-DIALKYL - (OEP)ZR(CH2SIME3)2 [J].
BRAND, H ;
ARNOLD, J .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1992, 114 (06) :2266-2267
[8]   THE CHEMISTRY OF RHENIUM AND TUNGSTEN PORPHYRIN COMPLEXES IN LOW OXIDATION-STATES - SYNTHESIS AND CHARACTERIZATION OF RHENIUM AND TUNGSTEN PORPHYRIN DIMERS CONTAINING METAL-METAL MULTIPLE BONDS [J].
COLLMAN, JP ;
GARNER, JM ;
WOO, LK .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1989, 111 (21) :8141-8148
[9]   MOLYBDENUM(IV)-PORPHYRIN DERIVATIVES - OXO(5,10,15,20-TETRA-PARA-TOLYLPORPHYRINATO)MOLYBDENUM(IV), MOO(TTP), AND DICHLORO(5,10,15,20-TETRA-PARA-TOLYLPORPHYRINATO)MOLYBDENUM(IV), MO(CL)2(TTP) - SYNTHESES AND STRUCTURES [J].
DIEBOLD, T ;
CHEVRIER, B ;
WEISS, R .
INORGANIC CHEMISTRY, 1979, 18 (05) :1193-1200
[10]   THE SYNTHESIS OF MOLYBDENUM AND TUNGSTEN DINITROGEN COMPLEXES [J].
DILWORTH, JR ;
RICHARDS, RL .
INORGANIC SYNTHESES, 1990, 28 :33-43