Preparation and characterization of bis[(mu-acetato)halo(mu-bis(diphenylphosphino)amine)molybdenum(II)] complexes

被引:21
作者
Arnold, DI
Cotton, FA
Kuhn, FE
机构
[1] TEXAS A&M UNIV, DEPT CHEM, COLLEGE STN, TX 77843 USA
[2] TEXAS A&M UNIV, MOL STRUCT & BONDING LAB, COLLEGE STN, TX 77843 USA
关键词
D O I
10.1021/ic9514758
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
Molecules of the formula Mo(2)X(2)(OAc)(2)(mu-dppa)(2) (X = Cl (2), Br (3), I (4); dppa = bis(diphenylphosphino)-amine; OAc = CH3COO-) can be synthesized by the reaction of Mo-2(OAc)(4) (1) With dppa and (CH3)(3)SiX. All three compounds were characterized by IR and UV-visible spectroscopy, mass spectrometry, and P-31{H-1} NMR spectroscopy. Single-crystal diffraction studies yield the following pertinent crystal data: for 2 . 2EtOH, orthorhombic Pbca (No. 61), a = 16.830(2) Angstrom, b = 20.310(4) Angstrom, c = 16.751(2) Angstrom, V = 5726(2) Angstrom(3), Z = 4; for 3 . 2(toluene), monoclinic C2/c (No. 15), a = 22.481(2) Angstrom, b = 19.151(9) Angstrom, c = 14.358(2) Angstrom, beta = 95.19(2)degrees, V = 6156(3) Angstrom(3), Z = 4; for 4 . EtOH . CH3CN, monoclinic P2(1)/c (No. 14), a = 20.607(9)Angstrom, b = 16.020(3) Angstrom, c = 17.189(5) Angstrom, beta = 95.81(2)degrees, V = 5645(3) Angstrom(3), Z = 4. The Mo-Mo distances for compounds 2-4 are 2.158(1), 2.176(1), and 2.164(1) Angstrom, respectively. Both crystallographic data and physical measurements indicate that 2 and 3 have nearly identical Mo-X bond distances while those in 3 and 4 differ more significantly; the spectroscopic data bear this out. The Mo-O and Mo-P distances are very similar in all three of the complexes reported.
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页码:4733 / 4737
页数:5
相关论文
共 32 条
[1]   2 BIS(DIPHENYLPHOSPHINOMETHANE) (DPPM) COMPLEXES OF QUADRUPLY BONDED DIMOLYBDENUM(II) - MO2(DPPM)2X4, X = CL, NCS [J].
ABBOTT, EH ;
BOSE, KS ;
COTTON, FA ;
HALL, WT ;
SEKUTOWSKI, JC .
INORGANIC CHEMISTRY, 1978, 17 (11) :3240-3245
[2]  
ARNOLD DI, IN PRESS INORG CHEM
[3]   COMPLEXES OF THE TYPE MO2(O2CR)2X2(L-L) IN WHICH THE BIDENTATE PHOSPHINE-LIGANDS L-L STRADDLE THE MO=MO BOND [J].
BAKIR, M ;
WALTON, RA .
POLYHEDRON, 1988, 7 (14) :1279-1284
[4]   STRUCTURES OF PD[(PPH2)2(NME)]CL2, PT[(PPH2)2(NME)]CL2 AND PT[(PPH2)2(NME)](CN)2 [J].
BROWNING, CS ;
FARRAR, DH ;
FRANKEL, DC .
ACTA CRYSTALLOGRAPHICA SECTION C-CRYSTAL STRUCTURE COMMUNICATIONS, 1992, 48 :806-811
[5]  
BRUGGEMANN R, 1992, 1 JAHR TAG DTSCH GES, P33
[6]   CORRELATION OF MO-MO QUADRUPLE BOND LENGTH WITH ANGLE OF INTERNAL-ROTATION, USING DATA FOR 10 COMPOUNDS [J].
CAMPBELL, FL ;
COTTON, FA ;
POWELL, GL .
INORGANIC CHEMISTRY, 1984, 23 (25) :4222-4226
[7]  
Cotton F.A., 1993, MULTIPLE BONDS METAL
[8]   SYNTHESIS AND CHARACTERIZATION OF MOLYBDENUM SPECIES - DINUCLEAR AND MONONUCLEAR SPECIES OF THE MOLECULAR FORMULAS [MO2(O2CCH3)2(LL)2][BF4]2 AND [MO(O)(F)(LL)2][BF4] WHERE LL = BIS-PHOSPHINE - THE USE OF [MO2(NCCH3)10][BF4]4 AS A SOURCE FOR THE [MO2]4+ CORE [J].
COTTON, FA ;
EGLIN, JL ;
WIESINGER, KJ .
INORGANICA CHIMICA ACTA, 1992, 195 (01) :11-23
[9]   CRYSTAL AND MOLECULAR-STRUCTURES OF MO2CL4(PMEPH2)4 AND RE2CL4(PMEPH2)4 [J].
COTTON, FA ;
CZUCHAJOWSKA, J ;
LUCK, RL .
JOURNAL OF THE CHEMICAL SOCIETY-DALTON TRANSACTIONS, 1991, :579-585
[10]   SYNTHESIS AND MOLECULAR-STRUCTURE OF MO2I4(BIS(DIPHENYPHOSPHINO)METHANE)2.2C7H8 [J].
COTTON, FA ;
DUNBAR, KR ;
POLI, R .
INORGANIC CHEMISTRY, 1986, 25 (20) :3700-3703