摘要:

1980 1803Photochemistry of Chloro-, Bromo-, and lodo-pentacarbonylmanganesein Frozen Gas Matrices at 12 K. Infrared Spectroscopic Evidence forTetracarbonylhalogenomanganese Species with a CzV Trigonal-bipyra-midal StructureBy Terence M. McHugh, Antony J. Rest.' and David J. Taylor, Department of Chemistry, The University,Southampton SO9 5NHInfrared spectroscopic evidence, including W O labelling and energy-factored force-field fitting for [ Mn (CO),CI]and [Mn(CO),CI], is presented to show that on photolysis of [Mn(CO),X] (X = CI, Br, or I ) complexes at highdilutions in Ar and CHI matrices at 12 K new species [Mn(CO)QX], with the X ligand occupying an equatorialposition in a trigonal-bipyramidal structure and having Cza symmetry, are produced. The observations of CO ejec-tion, the formation of a co-ordinatively unsaturated species, and the reversibility of the reaction (i) are interpreted ashvhv'[Mn(CO),X] ,7 [Mn(CO),X] + COconfirming the existence of a co-ordinatively unsaturated species as the intermediate in the substitution reactions of[Mn(CO),X] complexes; i.e.the reaction follows the dissociative path proposed from previous kinetic studies.THE CO-exchange and ligand-substitution reactions ofthe Group 7A pentacarbonylhalogenometal complexeshave been extensively studied and it is generally agreedthat the rate-determining step is CO dissociation inboth cases [equation (1)I.l-s Some early work l y 2 has[M(CO),(L)XI (1)M = Mn or Re; X = C1, Br, or I; L = 13C0, ClSO,indicated that the rate constant for dissociation of theradial CO ligands, cis to the halide ligand, is greater thanthat for dissociation of the axial CO ligand, althoughthis difference was found to depend on the nature ofX.3 Experiments with C1*0, however, showed4 thatfor [Mn(CO),Cl] and [Mn(CO),Br] the five CO ligandsexchange at approximately the same rate, in agreementwith the results of Hieber and Wollmann, for thesetwo compounds.Later has clearly demon-strated the preference for labilisation of the radial COligands to form the co-ordinatively unsaturated inter-mediate [Mn(CO),X]. Discussions of the details of thereaction mechanism have assumed that the co-ordin-atively unsaturated intermediate adopts either a square-pyramidal or trigonal-bipyramidal structure and haverecognised that such a species could be fl~xional.~-~Additionally, it has been pointed out that there mightbe a non-dissociative exchange of radial and axial COligands in [M(CO),X] compounds.Of the four possiblestructures (I-IV), it has been proposed7 that theinstantaneous structure is either (I) or (111). General-ised molecular-orbital calculations favoured structures(I) or (11) for [M(CO),X] fragments.l0P1l A more recentcalculation, however, has shown that the lowest energyPR, etc.The matrix-isolation technique lends itself well toestablishing the existence and geometry of unstablemetal carbonyl species,13-15 including those of [Mn-(CO),H] l6 and [Mn(CO),(CH3)].17 In this paper wepresent i.r. spectroscopic evidence for the formation of[Mn(CO),X] species on photolysis of [Mn(CO),X] com-plexes in Ar and CH, matrices and we relate the results0X IICIX I0 - C --MI AP0 0( m 1 ( c,, 1 ( I Y 1 ( c, " 1to previous kinetic studies; 1-8 a preliminary report ofthe results has been made.lsEXPERIMENTALCryogenic temperatures (ca.12 K) were obtained using aDisplex CSA-202 closed-cycle helium refrigeration system(Air Products and Chemicals Inc .) . The [Mn (CO),X]complexes are intermediate between those whichare volatileenough t o give gas mixtures for ' pulsed ' deposition l9 andthose which need high temperatures t o sublime them ontothe cold window. A glass spray-on system was designed 2ot o co-condense the vapour evaporating from the cooledsolid (ca.10 "C) with host matrix gas onto the cold CsI orLiF window. Monomer isolation fca. 1 : 2 000) was ensured form of [Mn(CO),Br] is the Cb structure (IV).I2 1804100C 0 .- 3 80-2.-E ulCca460c cQ, V LQ,R401J.C.S. Dalton---by having a substantially higher gas flow for the hostmatrix gas than for the complex to be isolated. Depositionwas monitored throughout by running i.r. spectra of thematrix and checking that the half-width a t half-heightof the terminal CO stretching bands did not exceed ca. 2cm-l and that there was no tailing of bands to lower wave-numbers.Infrared spectra in the 2 200 to 1850 cm-1 region wererecorded on a Grubb-Parsons Spectromajor grating spectro-meter modified to suppress the grating change to 1 850 cm-1.Calibration in the terminal CO stretching region was carriedout regularly using the gas-phase absorption bands of CO,DCl, and H20.Resolution was better than 1 cm-1 and thereproducibility of measurements was f 0.5 cm-l.The photolysis source was a medium-pressure mercuryarc lamp (Philips HPK 125 W). Wavelength-selectivephotolysis was achieved using the following filters: A,200 < A < 280 nm, quartz gas cell (pathlength 25 mni)containing C1, gas (2 atm *); B, A > 380 nm, quartz gascell containing C1, gas and a soda glass disc (thickness6 mm).Matrix gases (Ar, CH,) were B.O.C. ' Grade X ' purityand WO (95% enriched) was obtained from B.O.C. ProchemLtd. Samples of [Mn(CO),X] (X = C1, Br, and I) wereprepared from freshly sublimed [Mn,(CO) (Strem Chemi-cals Inc.) by standard procedures.2' Samples of WO-enriched [Mn(CO),Cl] were obtained by stirring a solutionof the complex (ca. 20 mg) in CH2C12 (10 cm3; lioch-Light,used after further purification) at 25 "C for 36 h in a closedvessel under a 12CO-13C0 atmosphere of known composition.The solid was obtained by pumping off the gas and solventand was purified by sublimation (50 "C at Torr).100806040RESULTSThe Isotro~ic Spectra of ~n(CO),Cl] .-The Group 7Apentacarbonylhalogenometal complexes all belong to theC,, symmetry point group and are expected to show three(ZA, + E) i.r.-active terminal CO stretching funda-m e n t a l ~ .~ ~ , ~ ~ The i.r. spectrum of [Mn(CO),Cl] is typicalof that for [Mn(CO),X] complexes in Ar or CH, matricesat 12 K [Figure l(a)].As expected, three groups of bandsare observed with splittings arising from matrix effects asdemonstrated by the different patterns for the same funda-mental in Ar and CH, (Table 1). In Figure l(a) the bandmarked with an asterisk is due to [Mn(12CO),(WO)Cl]occurring in natural abundance while those marked with adagger are due to a small amount of [Mn,(CO)In order to assign the structures of photolysis productsarising from [Mn(CO),X] complexes it was necessary todemonstrate the ability of the force-field fitting procedureto analyse the i.r. spectra of TO-enriched [Mn(CO),Cl],e.g. Figure 2(a). The choice of [Mn(CO),Cl] for this exercisewas made on the basis of a faster rate of 14C0 incorporationfor this complex (C1 : Br : I = 200 : 8 : 1).l Use of theenergy-factored CO stretching and interaction force con-stants for [Mn(CO),Cl] in solution 23 allowed the bandpositions and the relative band intensities of all the possiblewn(l2CO) 6-,(13CO),&1] molecules to be calculated.Thisimpurity.----* Throughout this paper: 1 atm = 101 326 Pa; 1 Torr =(101 325/700) Pa. t It is difficult to get the reaction of [Mn,(CO),,,] with C1, to goto completion and, since [Mn(CO),Cl] and [Mn,(CO),,] have similarsolubilities in organic solvents and also similar volatilities, i t wasimpossible to remove the last traces of [Mn,(CO),,] (ca. 2%) fromthe sample of [Mn(CO),Cl].2150 21001 1 I2075 2025 1975ti /cm-1FIGURE 1 Infrared spectra from an experiment with [Mn(CO),Cl]isoIated a t high dilution in a CH, matrix a t 12 I<: (a) afterdeposition, ( b ) alter 4 min photolysis using filter A, and (c)after another 15 min photolysis using filter B.See text for anexplanation of the bands marked * and 1805calculation * gave predicted bands and relative band inten-sities which were sufficiently similar to the observed spectrawith varying degrees of 13C0 enrichment to enable theobserved bands t o be assigned. Refinement of the energy-factored force field gave calculated wavenumbers whichcompare well with the observed wavenumbers t as shownin Table 2. The refined force constants obtained in thiswork agree well with those for a cyclohexane solution 23TABLE 1Band positions (an-')* for [Mn(CO) 5X] complexes andtheir photoproducts in the terminal CO stretchingregion for argon and methane matrices a t 12 KAr2 018.9mw1977.4s2 1 3 9 .5 ~ ~2 1 1 8 . 3 ~ ~2 046.7s2 018.9mw2 0 1 6 . 8 ~1979.5ms { 1977.7mw2 1 3 2 . 7 ~2 1 3 0 . 0 ~2 056.9mw2 053.3s2 050.7m{2 1 0 6 . 6 ~2 036.7s2 035.7s2 016.6mw1978.9s* Helati\.c intcnsitics: vw = vcrv wcak.CH,2 1 4 1 . 8 ~ ~2 014.Smw1973.1s2 1 3 7 . 8 ~ ~2 017.7mw1980.9mw1978.8ms1974.9ms2 1 2 9 . 9 ~2 1 2 7 . 6 ~2 049.6s2 046.7m2 045.4s2 002.4s2 1 0 8 . 4 ~2 1 0 6 . 7 ~ ~1975.0sinw = mediumweak, w~ = wcak, m = medium, ins = niediuni strong, s =strong. Bands bracketed together arisc from a single funda-mental with matrix splitting.(Table 2).Once accurately established, the energy-factored force field allowed relative band intensities t o becalculated via dipole moment derivatives (see Appendix),and these were compared 'with the observed relative band* In order to refine calculated and observed spectra inter-actively on the University of Southampton PDP-11 computer itwas necessary to re-cast equations and condense procedures usedpreviously 24-29 to reduce the core store required. Details aregiven in an Appendix which can be obtained in SupplementaryPublication No. SUP 22890 ( G pp.). Sec Notices to Authors No.7, J.C.S. Dalton, 1979, Index issue. t In the event of matrix-split fundamentals, a weightedaverage of wavenumbers was used in the calculations.intensities.The ' in-phase ' solution gave a OC,,.-Mn-COrad. bond angle of 87 f2' which compares reasonably wellwith the value of 89.8' obtained previously.22Photolysis of [Mn(CO),Cl] in Ar and CH, .Watvices.-Irradiation of [Mn(CO),Cl] isolated a t high dilution inCH, matrices with U.V. light (filter A) produced new bands[Figure l(b)] at 2 138.0 crn-', due to ' free ' CO, and a t2 123.7vw, 2 054.5 and 2 050.6s (doublet), 2 014.5mw, and1 973.1ms cm-1 (Table 1). Subsequent irradiation withlong-wavelength light (filter B) regenerated the parentbands [Figure l(c)] at the expense of the new ones. More-over, the relative intensities of the new bands remainedconstant on varying the forward and reverse photolysistimes and this behaviour indicates that one species isresponsible for the four new bands.Since ' free ' CO wasproduced in the forward photolysis step, the experimentswere carried out at high dilutions, and the primary step wasreversible, which might not have been the case if C1 atomshad been produced, the likely identity of the primary photo-product is the mononuclear species [Mn(CO),Cl] .Two of the simple structures [(II)(C8) and (IV)(C,,)] cangive rise to four i.r.-active fundamentals, one of which isexpected to be very weak and to occur above 2 100 cm-'because it is a symmetric CO stretching mode of a pair ofapproximately co-linear CO ligands. In order to distin-guish between the two possibilities it was necessary toproduce I3CO enriched [Mn(CO),Cl] with various levels ofW O incorporation.Photolysis (filter A) of WO-enriched[Mn(CO),Cl] in a CH, matrix produced a large number ofbands [Figure 2(b)]. Attempts were made to fit theobserved patterns using the C,(II) and C2,(IV) modelgeometries for the 13CO-enriched [Mn(CO),Cl] species.The C, model, although allowing considerable flexibilitythrough having seven force constants, failed to predict thepositions of all the observed bands for the various 13CO-enriched isomers. It also consistently predicted bands,with relatively high intensities, which were not observed.Additionally, the relative band-intensity pattern expectedfor a C , [Mn(WO),Cl] species, e.g. [Cr(CO),(CS)] [2 0 7 0 . 4 ~and 2 0 6 9 . 3 ~ (A'), 2 011.3s (A'), 1 977.7~s and 1 975.6~s(A"), and 1949.3s (A') cm-1],30 is very different fromthat observed (Table 1).In contrast, the Czv modelrefined satisfactorily although the fit of the band positions(Table 3) was not quite as good as for [Mn(CO),ClJ (Table2), the mean errors being f0.4 and f0.2 respectively.The relative band intensities predicted (see Appendix) for[Mn(12CO),C1] using this model [ A , (0.025), B , (0.93),A , (0.20), and B , (0.66)] correlate well with observed relativeintensities [ A , (0.028), B , (0.86), A , (0.20), and B , (0.66);CH, matrix a t 12 K] and also with those of other matrix-isolated C,, species: e.g. [Mn(CO),(NO)][A, (0.08), B ,(0.88), A , (0.20), and B, (0.78); N, matrix a t 12 K] 31 and[Fe(CO), CH,][A, (0.041, B , (0.70), A , (0.20), and B,(0.90) : CH, matrix at 10 Kl.28 It seems probable, there-fore, that [Mn(CO),Cl] adopts structure (IV).For such astructure the bond dipole-moment derivatives gave valuesfor the OCeq.-Mn-COeq. and OC,,~-Mn-CO,,. angles of119f2 and 179+2" respectively on the basis of the ' out-of-phase ' solution, cf. [Fe(CO),] and [Fe(CO), * * * CH,].2*Analogous results were obtained on photolysis of [Mn-(CO),Cl] in Ar matrices (Table I), although the matrixsplittings were different and the overall yield of the [Mn-(CO),Cl] product species was lower.$ Mean errors calculated as (c2/lna)1806ments [Mn(CO),ClJ (n < 4), which will be the subjects offurther work.TABLE 2Observed and calculated a wavenumbers (cm-l) of terminalCO stretching bands of 13CO-enriched [Mn(CO),Cl] ina CH, matrix at 12 K80Point[Mn( lZCO) ,C1] C,, A, 2 141.8 2 142.0Ba b 2 087.9E 2 057.1 2 057.2A, 1999.2 1999.7[Mn ( l2C0) (I3C0) Cl] C , A' 2 134.5 2 134.5(rad.13CO) A' 2081.5 2081.3A" 2067.3 2057.2A' 2025.9 2025.8 40A' 1998.8 1998.8B, b 2 087.9E 2 057.3 2 057.3[Mn (l2CO),( 13C0) aC1 J C, A' 2124.9 2 124.9A' 2029.5 2029.4A' 1998.1(tvans rad. lSCO, rad. I3CO) C,, A, d 2 127.6Complex group v(C0) Observed Calculated60(ax. laC0) c40 c 2 140.8A , 1956.3 1956.3 20(czs rad. 13C0, rad. laC0) A" 2077.1 2077.1 5A" 2021.4 2021.9 --C i 0-J.C.S. Dalton----(ax. K O , rad. 'TO)A , 2056.7 W1Oo-B, 2 0 i l . 6 2011.6C, A' c 2 133.3 uA' 2081.5 2081.3A" 2057.3 2057.2 ' A' c 2 025.3A' 1966.3 1966.0[Mn ('CO) a( W O ) &1] C, A' 2114.8 2 114.7(ax.W O , rad. 'XO) A' G 2 056.7A' c 2 024.2 60A" 2011.6 2011.6A' c 1997.8A" 2077.1 2077.1A' t 2 028.6 40A" 2021.4 2021.9A' c 1 965.7(tvans rad. W O , rad. "CO) C,, A, d 2 126.3B, 2057.3 2057.2A1 c 1998.4 $(cis rad. WO, rad. W O ) C, A' G 2 123.5A1 c 2 056.0B , 2011.6 2011.6 20A, c 1955.7[Mn(WO) (laCO),C1] C , A, 2097.5 2096.6(ax. W O ) b 2 041.62011.6 2011.6--1807conclude, on the basis of similarity to [Mn(CO)&I], that thespecies formed are [Mn(CO),Br] and [Mn(CO),IJ, both withstructures of type (IV).DISCUSSIONThe photoreactions of [Mn(CO),X] complexes in Arand CH, matrices can be summarised as in equation (2).hv[Mn(CO)JI [Mn(CO),XI 4- CO (2)The observation of CO ejection, the formation of a co-ordinatively unsaturated species, and the reversibilityof the reaction are consistent with the dissociativemechanism and the co-ordinatively unsaturated inter-mediate proposed in kinetic studies.l-8 It should benoted, however, that in the 13C0 exchange in [Mn(CO),-Br] no site preference was found for the photochemicalreaction, in contrast to the thermal reaction, and thisled the authors6 to propose that there were differentintermediates for the two reactions (see below).Unfortunately the proposed fluxionality 4-7p9 of the[Mn(CO),X] species could not be tested directly becausespecifically labelled TO-enriched [Mn(CO),Cl] couldnot be prepared.However, in a separate study of thephotolysis of [Mn(CO),(CH,)] in frozen gas matrices at12 K it was found32 that, after a cycle of forward andreverse photolysis, an appreciable amount of trans-[Mn(12C0),(13CO) (CH,) ] had been produced in an experi-ment which started with exclusively the cis isomer.This result is analogous to the detection of cis-[Cr(12CO),-(YO)(CS)] in a frozen gas matrix after a photolysiscycle starting with the trans isomer and where fluxional-ity of the five-co-ordinate intermediate was proposed.30It seems probable, therefore, that the [Mn(CO),X]species are also fluxional.It is interesting to note thatthe trigonal-bipyramidal structure (IV) proposed for[Mn(CO),X] species is in accordance with the molecular-orbital study l2 for the lowest-energy configuration of[Mn(CO),Br].A square-pyramidal geometry of type(11) was found to be the next lowest-energy configur-ation,12 but the energy separation between (IV) and (11)was not so large as to prevent Berry-type intercon-version33 between the two structures. The otherpossibility for fluxionality is intramolecular rearrange-ment of the [Mn(CO),X] comple~es.~ This possibilityhas recently been demonstrated for 13C1sO-enriched[ W (CO) ,{ P (OCH,) 3}], where st ereochemical non-rigidi t ywas found to occur by a process which did not involveloss of either CO or P(OCH,), ligands. This resulttogether with the fluxionality of [Mn(CO),X] speciessuggests that the stereochemical aspects of CO exchangeand replacement mechanisms will need to be reinvesti-gated.The CzV structure of [Mn(CO),X] in this work is incontrast with earlier matrix-isolation studies of [Mn-(CO),H] l6 and [Mn(CO),(CH,)]; l7 structures of type(111) were assigned to these species on the basis of theobservation of three i.r.-active terminal CO stretchingbands.Experience with [Mn(CO),(NO)], which alsohas ‘ apparently ’ three i.r.-active terminal CO stretchingbands in solution, consistent with structure (111), butfour such bands in a N, matrix, has shown that there canbe band overlaps which lead to incorrect conclusions.The CzV structure of [Mn(CO),(NO)] in the N, matrixwas established 31 by 13C0 substitution together withTABLE 3Observed and calculated a wavenumbers (cm-l) of terminalCO stretching bands of lTO-enriched [Mn(CO),Cl]in a CH, matrix at 12 KComplex[Mn(lBCO),C1][Mn( WO) 3( l3CO) Cl](eq.WO)(ax. ‘TO)[Mn(1zCO),(13CO)aC1](eq. 13C0, eq. 13CO)[Mn(’WO),( 13CO),C1](ax. ‘TO, ax. 13CO)[Mn( l2C0) a( 13CO)2Ci](ax. WO, eq. 13CO)[Mn(12CO)(1aCO)3C1](ax. WO)(en. WO)[Mn(13CO) ,C1]v(C0)A,B,A1B aA’A‘A‘A ”A’A’A’A ”A1A1BlBaA1A1BlBaAAAAA’A’A‘A‘’A’A‘A‘A”A1BlA1BaObserved2 123.72 052.32 014.51973.1b2 052.3b1942.12 108.92 030.22 006.01973.1e2 052.31974.01929.3b2 007.02 006.01973.12 106.5bb1942.12 104.5b1 971.01929.3b2 007.0b1942.1b2 007.01 976.01929.3Calculated2 123.62 052.62 014.61973.12 121.42 052.62 003.01942.32 109.22 029.12 006.01973.32 119.32 052.51973.81929.32 085.42 006.92 005.81973.12 106.62 026.11998.21 942.12 104.12 023.91971.31929.32 080.82 006.91997.11942.02 076.42 006.91 969.71929.3a Refined energy-factored force constants : KSx.= 1 750.4,Keq. = 1817.7, kt = 48.5, k, = 30.3, and k, = 44.9 N m-1.Band obscured by others including those of the [Mn(CO),CI]parent. Band partially obscured by other bands, estimatedposition given. Estimated position of unresolved band.6 Band predicted to have very low intensity.energy-factored force-field fitting of the observed andcalculated spectra and is consistent with the X-raycrystallographic study of the compound.A T O -labelling study 32 of [Mn(CO),(CH,)] has also shown thatenergy-factored force-field fitting of observed and cal-culated spectra is only possible for the Czpl structureof type (IV). It seems possible, therefore, that [Mn-(CO),H] also has a structure of type (IV) rather than oftype (111); l6 i.e. the [Mn(CO),X] (X = C1, Br, I, H, orCH,) series of species has a common structure of type(IV) J.C.S. DaltonWe thank Dr. J. S. Ogden for helpful advice concerningthe energy-factored force-field calculations and computerprograms, and the S.R.C. for support (to A. J. R.) and forResearch Studentships (to T. M. M. and D. J. T.). 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Wilt, Mathematical Methods forDigital Computers,’ Wiley, New York, 1960.26 P. Gans, ‘ Vibrating Molecules,’ Chapman and Hall, London,1971.2’ P. S. Braterman, ‘Metal Carbonyl Spectra,’ AcademicPress, London, 1975.z8 M. Poliakoff and J. J. Turner, J.C.S. Dalton, 1974, 2276.R. N. Perutz and J. J. Turner, Inorg. Chem., 1975, 14, 262.30 M. Poliakoff, Inorg. Chem., 1976, 15, 2022, 2892.3 l A. J . Rest and D. J. Taylor, J.C.S. Chem. Comm., 1977, 717.32 T. M. McHugh and A. J . Rest, J.C.S. Dalton, in the33 R. S. Berry, J . Chem. Pltys., 1960, 32, 933.34 D. J. Darensbourg and B. J. Baldwin, J . Amer. Chem. SOC.,Pure Appl. Chem., 1977, 49, 271.press.1979,101, 6447

ISSN:1477-9226    

DOI:10.1039/DT9800001803

出版商:RSC    

年代:1980

数据来源: RSC