Synthesis and Structure of cis-Dioxo(3-Methoxysalicylaldehyde 4-Methylthiosemicarbazonato-N,O,S)(γ-Picoline-N) Molybdenum(VI)

被引:8
作者
Milic, Dalibor [1 ]
Vrdoljak, Visnja [1 ]
Matkovic-Calogovic, Dubravka [1 ]
Cindric, Marina [1 ]
机构
[1] Univ Zagreb, Lab Gen & Inorgan Chem, Dept Chem, Fac Sci, Zagreb 10000, Croatia
关键词
Molybdenum(VI) complex; Thiosemicarbazone; Tridentate ligand; Crystal structure; X-ray analysis; Hydrogen bond; THIOSEMICARBAZIDE-BASED LIGANDS; TRANSITION-METAL-COMPLEXES; OXYGEN-ATOM TRANSFER; SCHIFF-BASE LIGANDS; ONS-DONOR LIGANDS; CRYSTAL-STRUCTURES; DIOXOMOLYBDENUM(VI) COMPLEXES; CIS-DIOXOMOLYBDENUM(VI) COMPLEXES; XANTHINE-OXIDASE; S-METHYLISOTHIOSEMICARBAZONE;
D O I
10.1007/s10870-009-9525-0
中图分类号
O7 [晶体学];
学科分类号
0702 ; 070205 ; 0703 ; 080501 ;
摘要
Red crystals of cis-dioxo(3-methoxysalicylaldehyde 4-methylthiosemicarbazonato-N,O,S)(gamma-picoline-N)-molybdenum(VI), [MoO(2)L(gamma-pic)], [L(2-)=CH(3)OC(6)H(4)(O) CH=NN=C(S)NHCH(3), 3-methoxysalicylaldehyde 4-methylthiosemicarbazonato] were prepared by the reaction of [MoO(2)L](n) with gamma-picoline in dry methanol. The title compound crystallized in the monoclinic space group P2(1)/n, a = 6.7984(7) angstrom, b = 15.9760(12) angstrom, c = 17.1466(14) angstrom, beta = 93.613(8)degrees, V = 1858.6(3) angstrom(3), Z = 4. The coordination geometry around the molybdenum center is distorted octahedral with the tridentate thiosemicarbazonato ligand (L(2-)) bonded meridionally to the [MoO(2)](2+) core. The sixth coordination site is occupied by a weakly bound gamma-picoline molecule. The adjacent molecules are joined by the N-H center dot center dot center dot O hydrogen bonds between their amino and methoxy groups thus forming infinite molecular chains. The three-dimensional solid-state structure is achieved by the additional C-H center dot center dot center dot O, C-H center dot center dot center dot pi and van der Waals interactions.
引用
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页码:553 / 557
页数:5
相关论文
共 44 条
[1]  
[Anonymous], 2006, CRYSALIS SOFTWARE SY
[2]   Transition metal complexes with thiosemicarbazide-based ligands .25. Synthesis and x-ray crystal structure of cis-dioxo [(salicylaldehyde thiosemicarbazonato(1-))] aquomolybdenum (VI) chloride monohydrate, [MoO2(HL)H2O]Cl.H2O [J].
Argay, G ;
Kalman, A ;
Leovac, VM ;
Cesljevic, VI ;
Ribar, B .
JOURNAL OF COORDINATION CHEMISTRY, 1996, 37 (1-4) :165-171
[3]   The wide pharmacological versatility of semicarbazones, thiosemicarbazones and their metal complexes [J].
Beraldo, H ;
Gambino, D .
MINI-REVIEWS IN MEDICINAL CHEMISTRY, 2004, 4 (01) :31-39
[4]   A MODEL FOR THE ACTIVE-SITES OF OXO-TRANSFER MOLYBDOENZYMES - SYNTHESIS, STRUCTURE, AND PROPERTIES [J].
BERG, JM ;
HOLM, RH .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1985, 107 (04) :917-925
[5]   STRUCTURE PROOFS OF LIGATED AND POLYMERIC DIOXOMOLYBDENUM(VI)-TRIDENTATE COMPLEXES - MOO2(C5H3N-2,6-(CH2S)2)(C4H8SO) AND [MOO2(C5H3N-2,6-(CH2O)2)]N [J].
BERG, JM ;
HOLM, RH .
INORGANIC CHEMISTRY, 1983, 22 (12) :1768-1771
[6]   SYNTHESIS, CHARACTERIZATION, AND ELECTROCHEMISTRY OF CIS-DIOXOMOLYBDENUM(VI) COMPLEXES OF SCHIFF-BASES DERIVED FROM CARBOHYDRAZIDE, THIOCARBOHYDRAZIDE, AND SALICYLALDEHYDE - CRYSTAL-STRUCTURES OF [MOO2(O-OC6H4CH=NN=CSNHN=CHC6H4OH-O)ME2SO] AND [(MOO2)2(O-OC6H4CH=NN=CONN=CHC6H4O-O)(ME2SO)2].0.5ME2SO [J].
BUSTOS, C ;
BURCKHARDT, O ;
SCHREBLER, R ;
CARRILLO, D ;
ARIF, AM ;
COWLEY, AH ;
NUNN, CM .
INORGANIC CHEMISTRY, 1990, 29 (20) :3996-4001
[7]   SYNTHESIS OF MO(IV) AND MO(V) COMPLEXES USING OXO ABSTRACTION BY PHOSPHINES - MECHANISTIC IMPLICATIONS [J].
CHEN, GJJ ;
MCDONALD, JW ;
NEWTON, WE .
INORGANIC CHEMISTRY, 1976, 15 (11) :2612-2615
[8]   Synthesis and characterization of some mono- and dinuclear molybdenum(VI) thiosemicarbazonato complexes [J].
Cindric, M ;
Vrdoljak, VN ;
Strukan, N ;
Kamenar, B .
POLYHEDRON, 2005, 24 (02) :369-376
[9]   Synthesis, characterization, and crystal structure of mononuclear and dinuclear dioxomolybdenum(VI) complexes with tridentate Schiff-base ligands. Part 2 [J].
Cindric, M ;
Strukan, N ;
Vrdoljak, V ;
Kamenar, B .
ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE, 2004, 630 (04) :585-590
[10]   OXOMOLYBDENUM(IV,V,VI) COMPLEXES - STRUCTURES, REACTIVITIES, AND CRITERIA OF DETECTION OF BINUCLEAR (MU-OXO)MOLYBDENUM(V) PRODUCTS IN OXYGEN ATOM TRANSFER SYSTEMS [J].
CRAIG, JA ;
HARLAN, EW ;
SNYDER, BS ;
WHITENER, MA ;
HOLM, RH .
INORGANIC CHEMISTRY, 1989, 28 (11) :2082-2091