Sterically encumbered charge-compensated carbaboranes: Synthesis and reactivity - Molecular structures of 7-Ph-11-SMe2-7,8-nido-C2B9H10 and 1-Ph-3,3-(CO2-7-SMe)(2)-3,1,2-closo-RhC2B9H8

被引：27

作者：

Rosair, GM ^{[1
]}

Welch, AJ ^{[1
]}

Weller, AS ^{[1
]}

Zahn, SK ^{[1
]}

机构：

[1] HERIOT WATT UNIV,DEPT CHEM,EDINBURGH EH14 4AS,MIDLOTHIAN,SCOTLAND

来源：

JOURNAL OF ORGANOMETALLIC CHEMISTRY | 1997年 / 536卷 / 1-2期

关键词：

boron; rhodium; carbaboranes; steric effects; crystal structure;

D O I：

10.1016/S0022-328X(96)06740-X

中图分类号：

O61 [无机化学];

学科分类号：

070301 ; 081704 ;

摘要：

Reaction between K[7-Ph-7,8-nido-C2B9H11] and dmso in H2SO4 affords a mixture of the isomers 7-Ph-9-SMe2-7,8-nido-C2B9H10 (1a) and 7-Ph-11-SMe2-7,8-nido-C2B9H10 (1b). Similarly, starting from K[7,8-Ph-2-7,8-nido-C2B9H10], the diphenyl analogue 7,8-Ph-2-9-SMe2-7,8-nido-C2B9H9 (2) was produced. These three new nido carbaboranes have been characterised spectroscopically, including B-11-B-11 COSY and H-1-H-1 NOESY experiments, and by a single crystal diffraction study on 1b. Deprotonation of 1a followed by addition of [RhCl(CO)(2)](2) affords the carbametallaborane 1-Ph-3,3-(CO)(2)-7-SMe2-3,1,2-closo-RhC2B9H9 (3), characterised by R-1 and H-1 and B-11 NMR spectroscopies and by a crystallographic study. (C) 1997 Elsevier Science S.A.

引用

页码：299 / 308

页数：10

共 24 条

[1] STERICALLY-INDUCED LOW-TEMPERATURE POLYHEDRAL REARRANGEMENTS OF CARBAPLATINABORANES - SYNTHESIS AND CRYSTAL-STRUCTURES OF 1-PH-3,3-(PME2PH)2-3,1,2-PTC2B9H10,1-PH-3,3-(PME2PH)2-3,1,11-PTC2B9H10,11-PH-3,3-(PME2PH)2-3,1,11-PTC2B9H10 AND 1,11-PH2-3,3-(PME2PH)2-3,1,11-PTC2B9H9 [J].

BAGHURST, DR ;

COPLEY, RCB ;

FLEISCHER, H ;

MINGOS, DMP ;

KYD, GO ;

YELLOWLEES, LJ ;

WELCH, AJ ;

SPALDING, TR ;

OCONNELL, D .

JOURNAL OF ORGANOMETALLIC CHEMISTRY, 1993, 447 (02) :C14-C17

[2] Synthesis and characterisation of pseudocloso iridium and ruthenium diphenyl carbaboranes. Molecular structures of 1,2-Ph(2)-3-(eta-C6H6)-3,1,2-pseudocloso-RuC2B9H9 and 1,2-Ph(2)-3-(cym)-3,1,2-pseudocloso-RuC2B9H9 (cym equals p-cymene) and individual gauge for localised orbitals calculations on carbametallaboranes [J].

Brain, PT ;

Buhl, M ;

Cowie, J ;

Lewis, ZG ;

Welch, AJ .

JOURNAL OF THE CHEMICAL SOCIETY-DALTON TRANSACTIONS, 1996, (02) :231-237

[3] 1-Phenyl-1,2-dicarba-closo-dodecaborane, 1-Ph-1,2-closo-C2B10H11. Synthesis, characterization, and structure as determined in the gas phase by electron diffraction, in the crystalline phase at 199 K by X-ray diffraction, and by ab initio computations [J].

Brain, PT ;

Cowie, J ;

Donohoe, DJ ;

Hnyk, D ;

Rankin, DWH ;

Reed, D ;

Reid, BD ;

Robertson, HE ;

Welch, AJ ;

Hofmann, M ;

Schleyer, PV .

INORGANIC CHEMISTRY, 1996, 35 (06) :1701-1708

[4] CARBABORANE DERIVATIVES OF THE LATE-TRANSITION AND POST-TRANSITION ELEMENTS .3. STRUCTURAL CONSEQUENCES OF LIGAND SUBSTITUTION IN PALLADADICARBADODECABORANES 3-L2-3,1,2-PDC2B9H11 - THE CRYSTAL AND MOLECULAR-STRUCTURES OF 3-[ME2N(CH2)2NME2]-3,1,2-PDC2B9H11 AND 3-(PME3)2-3,1,2-PDC2B9H11 [J].

COLQUHOUN, HM ;

GREENHOUGH, TJ ;

WALLBRIDGE, MGH .

JOURNAL OF THE CHEMICAL SOCIETY-DALTON TRANSACTIONS, 1985, (04) :761-769

[5] STERIC EFFECTS IN HETEROBORANES .7. THE SYNTHESIS AND CHARACTERIZATION OF ARENE-RUTHENIUM COMPLEXES OF C-SUBSTITUTED CARBABORANES - MOLECULAR-STRUCTURES OF 1-PH-3-(MES)-3,1,2-CLOSO-RUC2B9H10 (MES=C6H3-1,3,5) AND 1-PH-2-ME-3-(P-CYM)-3,1,2-CLOSO-RUC2B9H9 (P-CYM=C(6)H(4)ME-1-PR-I-4), THE LATTER SHOWING AN INCIPIENT DEFORMATION [J].

COWIE, J ;

REID, BD ;

WATMOUGH, JMS ;

WELCH, AJ .

JOURNAL OF ORGANOMETALLIC CHEMISTRY, 1994, 481 (02) :283-293

[6] STRUCTURE OF 10,11-MU-HYDRO-9-DIMETHYLSULFIDO-7,8-DICARBA-NIDO-UNDECABORANE(11) [J].

COWIE, J ;

HAMILTON, EJM ;

LAURIE, JCV ;

WELCH, AJ .

ACTA CRYSTALLOGRAPHICA SECTION C-CRYSTAL STRUCTURE COMMUNICATIONS, 1988, 44 :1648-1650

[7] THE CHEMISTRY OF MONOANIONIC CARBABORANE LIGANDS - SYNTHESIS, AND MOLECULAR AND ELECTRONIC-STRUCTURE OF [3,3,3-(CO)3-4-SME2-3,1,2-MNC2B9H10], AND ORDER-OF-MAGNITUDE IMPROVED STRUCTURE OF (ETA-C5H5)MN(CO)3 [J].

COWIE, J ;

HAMILTON, EJM ;

LAURIE, JCV ;

WELCH, AJ .

JOURNAL OF ORGANOMETALLIC CHEMISTRY, 1990, 394 (1-3) :1-13

[8]

CRAMER R, 1974, INORG SYNTH, V15, P17

[9] THE CHEMISTRY OF MONOANIONIC CARBABORANE LIGANDS - SYNTHESIS AND STRUCTURE OF COMPOUNDS WITH CARBONYL AND CYCLOOCTA-1,5-DIENE LIGANDS ADDITIONALLY BOUND TO METAL ATOMS, INCLUDING A CATIONIC CARBAMETALLABORANE [J].

DOUEK, NL ;

WELCH, AJ .

JOURNAL OF THE CHEMICAL SOCIETY-DALTON TRANSACTIONS, 1993, (13) :1917-1925

[10] Reactions of nido-7,8-C2B9H13 with pentacarbonyl(methyl)manganese: Crystal structure of the charge-compensated complex [Mn(CO)(3){eta(5)-7,8-C2B9H10-10-O(CH2)(4)}] [J].

GomezSaso, M ;

Mullica, DF ;

Sappenfield, E ;

Stone, FGA .

POLYHEDRON, 1996, 15 (5-6) :793-801

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