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Intercalate of Xenon Tetrafluoride with Graphite

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Intercalate of Xenon Tetrafluoride with Graphite 953 Table I. Average Molybdenum-Oxygen Distances for the pi autodiffractometer using Nb-filtered Mo 6 radiation and 8-28 scans. cu-M0sO26~-ion in ~~-[(~-C~H~)(C~H~),P]~MO~~~~.CH~CN.H~~The four molyWenum atoms of the asymmetric unit were located using direct methods (MULTAN) and the remaining atoms by standard difference Fourier techniques. The resulting structural parameters have been refined TypeU Distance, A to convergence (R= 0.031 for 461 1 independent reflections having 28-n < 43' (the equivalent of 0.50 limiting Cu KE sphere) and I > 38(1)) using 1.696 (3,2, 3) unit-weighted fulknatrix least-squares techniques with anisotropic tfwmal parameters for all nonhydrogen atoms and isotropic thermal parameters 1.904 (3,4,9) for all hydrogen atoms. Refinement is continuing with those reflections 2.425 (3, 19, 56) having 28~< 59'. 1.783 (3, 3, 5) (6) F. A. Schroeder, Acta Crystallogr.. Sect. 6, 31, 2294 (1975). (7) In ref 2a an analogous but far geater variation is noted. In view of the lower 1.708 (3) precision obtained in the study reported in ref 2a, it is difficult to assess the significance of this greater variation. (1 See Figure la for labeling scheme. The first number in paren- (8) K. Matsumoto, A. Kobayashi, and Y. Sasaki, Bull. Chem. SOC.Jpfl., 48, theses following an average value is the root mean squared value of 1009 (1975). (9) KihlborglO in his study of Moos was apparently the first to note that certain the estimated standard deviation for an individual datum. The second molybdate structures containing octahedrally coordinated molybdenum and third numbers, when given, are the mean and maximum deviations with marked offcenter displacement toward an octahedral edge may be from the averaged value, respectively. best viewed as containing tetrahedral units. In the case of MoO3, he de- scribed infinite drains of comer sharing, distorted Moo4 tetrahedra which are only weakly associated to yield six-coordinate molybdenums. formula (M004~-)-)z(M06018)which characterizes the weak (IO) L. Kihlborg. Ark. Kemi, 21, 357 (1963). interactions between the two Mo042- ions and a ring of six (11) J. Berkowitz, M. G. Inghram, and W. A. Chupka, J. Chem. phys., 26,842 distorted Moo4 tetrahedra sharing This represen- (1957). corner^.^ (12) We refer here to the pioneering work of Baker and Tsigdinos on oxygen tation is also in accord with the existence of stable rings and chromium exchange in (Cr(OH)s3-)(Mo6018):L. C. W. Baker in "Ad- (Moo3)*, n = 3,4, and 5, studied in the vapor phase by Ber- vances in the Chemistry of Coordination Compounds", S. Kirchner, Ed., MacMillan. New York, N.Y., 1961, and references therein. kowitz et al. (13) M. Filowitz and W. G. Klemperer, J. Chem. Soc., Chem. Commun., 233 The simple relationship between kinetic lability and low (1976). (14) R. Strandberg, Acta Chem. Scad., 27, 1004 (1973). bond order established here is consistent with previous ex- (15) J. K. Stalick and C. 0. Quicksall, lnorg. Chem., 15, 1577 (1976). change studies12and may be extended in an attempt to predict (16) K. Barkigia, L. M. Rajkovic, M. T. Pope, and C. 0. Quicksall, J. Am. Chem. the kinetic behavior of other polyaxomolybdates. Several Soc., 97,4146 (1975). (17) For approximate bond distances in P-MO~O~~~-,see ref 3a. heteropolyanions may be viewed as structurally related to the (18) Camille and Henry Dreyfus Teacher-Scholar. CY-MO~O~~~-ion and represented as (AsO~~-)~(MO&I~),'~ (CsHsAs032-)2(Mo60~8),'3(P043-)2(Mos0~*),14 V. W. Day,* M. F. Fredricb ( CH3P032-)2( Mo501 =,),I5 and ((CH3)2As02-) (OH-)- Department of Chemistry, University of Nebraska (Mo4012),l6 which in turn implies potential lability with re- Lincoln, Nebraska 68508 spect to dissociation of hod3-, C6H~As03~-,FQ3-, CH3P032-, and (CH3)2As02-, respectively. One may spec- W. G. Klemperer,* W.Shum ulate further into the more general case where a large po- Department of Chemistry, Columbia University lyoxomolybdate cluster may be dissected into smaller clusters New York, New York 10027 by breaking only weak bonds. For example, @-Mo~O~~~-may Received October 18, 1976 be accurately represented by ((02-)(Mo4012)2 since the 8- Mo~O~~~-cluster can be dissected into two (02-)(Mo4012) subunits by breaking only bonds whose lengths exceed 2.22 AI7 and hence have bond orders less than 0.2.6 This fact points Intercalate of Xenon Tetrafluoride with Graphite toward a mechanistic pathway for the reaction of ((02-)- (Mo4012)2 with (CH&As02H to form the ((CH&As02-)- Sir: (OH-)(Mo4012) ion mentioned above. We are currently at- The compounds xenon hexafluoride' and xenon oxide tet- tempting to verify some of these speculations using dynamic rafluoride2 have previously been shown to intercalate in I7O NMR techniques. graphite. While these compounds react directly with graphite, Acknowledgments. V.W.D. and W.G.K. acknowledge the xenon difluoride reacts only in the presence of hydrogen flu- donors of the Petroleum Research Fund, administered by the oride to yield an intercalate of variable compo~ition.~We have American Chemical Society, for partial support of this re- now found that xenon tetrafluoride also forms intercalates with search. Also, W.G.K. acknowledges the National Science graphite. Foundation for financial support and V. W.D. acknowledges Weighed quantities of graphite and excess XeF4 were al- a generous grant of computing time from the University of lowed to react in preweighed Kel-F reaction vessels for periods Nebraska Computing center. W.G.K. and W.S. are grateful of up to 3 weeks at room temperature. Reactions were gener- to Mr. I. Miura for obtaining NMR spectra. ally complete after about 10 days, their slowness probably due to the low vapor pressure of XeF4. The excess XeF4 was then References and Notes pumped off until the reactor attained constant weight or did (1) W. G. Klemperer and W. Shum, J. Am. Chem. Soc.,98,8291 (1976). not lose weight at rates exceeding 2 mg/h. Stoichiometries (2) For the structure of (r-M08O~6~-see: (a) J. Fuchs and H. Hartl, Angsw. were calculated on the assumption that total weight gains were Chem.. lnt. Ed. €fig/., 15, 375 (1976); (b) M. F. Fredrich. V. W. Day, W. Shum, and W. G. Klemperer, Am. Cryst. Assoc. Summer Meeting, 1976, due to XeF4. The latter were extrapolated back to zero paper M5. pumping time. (3) For the structure of P-Mo8026'- see (a) L. 0. Atovmyan and 0. N. Krase The graphite used was either BDH powder or GTA grade chka, J. Struct. Chem. (USSR).13,319 (1972); (b) I. Linqvist. Ark. Kemi, 2, 349 (1950). Grafoil from Union Carbide Co. Considerable variations in (4) M. Filowitz, W. G. Klemperer. L. Messerle, and W. Shum, J. Am. Chem. stoichiometry were observed. The results with powder based Soc., 98, 2345 (1976). Although this reference considers complexes containing only octahedrally coordinated molybdenum, assignments of on nine different reactions were C28.3*2.4XeF4, while those resonances to 0, and OC in the present work are made using anal- with Grafoil were C41*1XeF4 based on four experiments. In reasoning. (5) Compound 3 crystallizes in the centrosymmetric "clinic space goup, one case, however, a stoichiometry of C17.8XeF4was obtained CZI (No. 15) with a = 28.096 (6) A, b = 14.313 (2) A, c = 27.1 16 even after pumping for 27 h. Neither xenon nor carbon fluo- (5) 1, P = 121.32 (1)'. and Z= 4 (fmhmits as given above). Diffracted rides were liberated during the course of the reaction, and intensities were measured on a spherical crystal having pr = 0.28 for 12 892 independent reflections having 28- < 59' (the equivalent of samples showed no visible changes. Fluorine analyses (Table 1.2 limiting Cu KE spheres) on a computer-controlled fourcircle Syntex I) correspond roughly to stoichiometries obtained from weight Communications to the Editor 954 dled outside the vacuum line, although part of the intercalated fluoride is slowly hydrolyzed, releasing HF. The residue is neither shock-sensitive nor exhibits appreciable oxidizing power. Preliminary investigations show that the intercalate may also be useful as a moderate fluorinating agent in organic chemistry. Experiments with aromatic systems gave the fol- lowing results: With benzene, the products were monofluoro- benzene (26%), p-difluorobenzene (1 l%), and starting mate- rial (63%). Phenanthrene6 yielded mainly 9-fluorophenan- threne (22%) and 9,9,1O-trifluoro-9,1O-dihydrophenanthrene ,W IW rW, , m Iwm, , ,W, (19%). As in the case of XeF2' fluorination of benzene proceeds Ilm*.lu-.c,L, only in the presence of HF catalyst. Figure 1. Thermogravimetric analysis of C26.7XeFd: sample weight, 25.7 mg; heating rate, 4O/min; atmosphere argon. Dashed line corresponds to References and Notes calculated final weight after complete decomposition. (1) H. Selig, M. Rabinovitz, I. Aganat, C. H. Lin. and L. EM,J. Am. Cbm. Soc., 98, 1601 (1976). (2) H. Selig and 0. Gani, lnorg. Nucl. Chem. Lett., 11, 75 (1975). (3) M. Rabinovitz, H. Selig, I. Agranat, C. H. Lin, and L. Ebert, unpublished ob- servations. Table I. Analysis of C,XeF4 (4) H. D. Frame, Chem. Phys. Lett., 3, 182 (1969). (5) W. Riidorff and U. Hofman, Z. Anorg. Allg. Chem., 238, 1 (1938). mequiv mequiv of I (6) (a)M. Zupan and A. Pollak, <I.Org. Chem., 25, 3794 (1975); (b) I. Agranat, M. Rabinovitz, H. Selig, and C. H. Lin, Chem. Lett., 1271 (1975). mmol of I per mmolof % F % F (7) M. J. Shaw, H. H. Hyman, and R. Filler, J. Am. Chem. Soc., 92, 6498 Material taken titrated intercalate found calcd (1970). C40XeF4 0.182 0.355 1.95 H.
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