534 A.

CH2CMe2CH CHdClL (I3C, Io3Rh),SS9 [Rh(Ph2PC6H4CHMeNMe2)(nbd)] = + (31P),MoRh[Ph2PCH(CH20CH2Ph)CH2PPh2](nbd)) { (13C, 3LP)7L Rh(Ph,[ PCH2CHPhPPh&nbd)] (31P),M2 (diolefin)Rh(p-indazolate),Rh(CO)(PPh3) ("P)?' [Rh(cod)(OPPh,),]+ (31P),s64 (Et,P),Rh(p-PPhd,Rh(cod) (31P)?S Cp,Rh,(CO)(PF,NEtd(CF,C= CCF,) (I3C,19F, ' P , Rh2(HC,Ph)(C0)2(dppm), I)= (31P),M7 (q3-C3Hs)Ir(l,5-C8Hl~P(OMe)3 t31P),%* and (COD)fr(Ph,PC,H,COCHCOEt) (31P).sa9 In (34), 'J(13C,IH) ofCHR' is only ca. 70 Hzowing to metal interactions. I'B n.m.r. data were also reported.'7o The 19'Pt n.m.r. spectrum of PtRh4(p-C0),(CSMe,),is a
1:4:6:4:1 quintet due to 'J(19'Pt,'03Rh) 68 Hz. The I3C n.m.r. spectrum was also = recorded.571N.m.r. data have also been reported for Co(CHCHCHCO)(CO), (13C),572 (2-Me-allyl)Rh(chelating diphosphine) (33P),573 Rh[Ph,PC(S)NR], (31P):74 { [C4(OMe)R1 R2R3]C~L(C0)2) (13C, 19F),575 CpCo(C,Ph,)(PPh,) ( 13C):76 C ~ C O [ C , ( S ~ M ~ , ) ~ C M ~ ~ O H ]CpCo(MeNBEtCEtCMeSiMe3('IB, 13C),578 (13C),577 Rh(CSMe5)(C4Ph2HCPhCsPh2H3 (13C),579 IrCl(truns-MeCHCHCHCH2)= (PPh,)* (31P),580 CpCo[CpFeCSH4B(CHCH)BCSH,FeCp] (B:* ")* [CpCo(MkCMeBMeCMeBMe)]- (1)8 C~CO[PO(OM~),]~P(OM~), 1B:2 (13C,
M. Cocivera, A. J. McAlecs, R. McCrindle, and P. Sznecinski,J. Organomet. Chem., 1982, 235, 97. N.C. Payne and D. W. Stephan, Inorg. Chem., 1982,21, 182. M J. P. Amma and J. K. Stille, J. Org. Chem., 1982, 47, 468. I 562 J. M.Brown and B. A. Murrer, J. Chem. Soc., Perkin Trans. 2, 1982, 489. 563 R. U s h , L. A. Oro, M. A. Ciriano, and M. C. Bello, J. Organomet. Chem., 1982,240, 199. 564 R. U s h , L. A. Oro, M. A. Ciriano, F. J. Lahoz, and M. C. Bello, J. Organomet. Chem., 1982,234,205. 565 D. W. Meek, P. E. Kreter, and G. G. Christoph, J. Organomet. Chem., 1982, 231, C53. 566 R. S.Dickson, A. P. Oppenheim, and G. N. Pain, J. Organomet. Chem., 1982, 224, 377. 567C. P. Kubiak, C. Woodcock, and R. Eisenberg, lnorg. Chem., 1982, 21, 2119. 568 E.L. Muetterties, K. D. Tau, J. F. Kirner, T. V. Harris, J. Stark, M. R. Thompson, and V. W. Day, Organometallics, 1982, 1, 1562. 569 D. A. Wrobleski and T. B. Rauchfuss, J. Am. Chem. Soc., 1982, 104, 2314. 5'0 W. Siebert, J. Edwin, and H.Pritzkow, Angew. Chem., Int. Ed. Engl., 1982, 21, 148. S71 M.Green, J. A. K. Howard, G. N. Pain, and F. G. A. Stone, J. Chem. SOC.,Dalton 7+ans., 1982, 1327. 572 W. A. Donaldson and R. P. Hughes, J. Am. Chem. SOC., 1982, 104,4846. 573 M. D. Fryzuk, Inorg. Chem., 1982,21, 2134. S74 D. M. W. Thewissen,J. G. Noltes, J. Willemse, and J. W. Diewveld, lnorg. Chim. Acta, 1982,59, 181. H. S75 W. A. Donaldson, R. P. H g e ,R. E.Davis, and S. M. Gadol, Organometallics, 1982, 1, 812. uhs 576 W. C. Trogler and J. A. Ibers, Organometallics, 1982, 1, 536. 577 J. R. Fritch and K. P. C. Vollhardt, Orgunmtallics, 1982, 1, 590. 57i3 R. Koster, G. Seidel, S. Amirkhalili, R. Boese, and G. Schmid, Chem. Ber., 1982, 115, 738. 5f9 J. Moreto, K. 4 Maruya, P. M.Bailey, and P.M.Maitlis, J. Chem. Soc.,Dalton Dam., 1982, 4. 580 R. B. Osborne and J. A. Ibers, J. Organomet. Chem., 1982,232,267. 5n1 G. E. Herberich and B. Hessner, Chem. Ber., 1982, 115, 31 15. 582 W. Siebert, J. Edwin, H. Wadepohl, and H. Pritzkow, Angew. Chem., Int. Ed. Engl., 1982, 21, 149.

Nuclear Magnetic Resonance Spectroscopj.
[Co(NH3),LI2+,and [CoL3I3+has been studied using 'H, 13C, "Co, and IssPt n.m.r. spectroscopy.6I2 "0 n.m.r. spectra of specifically labelled [CO(NH,)@OJ]~' have shown that spontaneous intramolecular 0-0 exchange in the NO2 ligand occurs at a rate comparable to that of the spontaneous 0-N and isomerism.613 structure of ion pairs between ci~-[Co(en)~XJ+ the counterThe anions has been investigated by 'H n.m.r. spectroscopy.614 analysis of 'J('H,'H) An for the chelate rings formed by N-methylethane-12-diamine shown that in Co"' has 5-membered diamine chelate rings the NCCN torsional angle is approximately 510.615 For some trans-diacido(tetramine)cobalt(III) complexes, a(' 3C) is linearly dependent on the ligand-field strength of the axial ligands.616 13C n.m.r. spectra have indicated high conformational mobility of mer-(Co[bis(3-amino6 'H spin-lattice relaxation times have been measured propyl)amine],j3 '" for dicyanocobalamin and dicyanocobinamide.6'8 H and 13C n.m.r. signals of 'H heptamethyl dicyanocobyrinate have been fully a~signed.6'~ and 13C n.m.r. spectroscopy has been used to investigate the biosynthesis of vitamin B12.620.621 13C labelling experiments point to C-17 as the site where the fourth methyl group is introduced in the biosynthesis of vitamin B12.622 Mn2+and Gd3+bind preferentially to the carboxylic acid in cyanocobalamin-monocarboxylic acids according to 13C n.m.r. ~pectroscopy.6~~ n.m.r. spectroscopy has been shown to be an extremely 13C sensitive probe to the stereochemistry of a series of complexes such as uno-cis[Co(2,2,3-tet)val12+ and Co"' complexes of glycine or /3-alanine.6" The high624 frequency shifts of the orcarbon atoms in N-alkylglycines, which are caused by the chelation to Co"', are larger than those in C-alkylglycines.626 co-ordination to On Co"', the 15Nresonance of amino-acids moves 24-42 p.p.m. to higher shielding.627 The products of the reaction of Co(glygly)(NO,)en with acetaldehyde have been The identified by 13Cn.m.r. spectroscopy.628 interaction of Eu(fod), with a series of Co"'(BAE) derivatives has been investigated using H and 13Cn.m.r. spectroscopy. Line broadening due to exchange was found.629 N.m.r. data have also been reported for [ C O ( C N ) , - ~ ~ ( ~ C ~ C ) ,(31P)p30 , L ~ ] ~ - [Co(3,3-dimethyl-l,2-butanediamine),13+

(31P)p8'

trans-PtHC1(PR3), (31P)f80 [HPt(PEt3),(p-H),Pt(PEt3),] PtHX(PBu',), (31P)p79 [Pt,H(CO)(p-dppm),] (31 P)P8, [Pt,H(py)(p-dppm),] (3 1P),683 and [Pt3(PPh3)3(p-PPh2)2(p-H)] (3'P).684 The 400 and 500 MHz 'H n.m.r. spectra of a series of q1,q2-alkenyl and q3cycloalkenyl-$-cyclopentadienylnickel complexes have been analysed with the aid of special n.m.r. techniques such as double resonance and n.0.e. m e a s ~ r e m e n t s. ~ ~ 'J('3C,'3C) has been determined for (q',q*-alkenyl)CpNi complexes. For coordinated double bonds, 'J('3C,13C) between the value for free ethylene and lies cyclopropane.686N.m.r. data have also been reported for poly[trans-bis(tributy1phosphine)platinum 1,4-butadiynediyl] and the Pd, Pt-Pd, and Pt-Ni analogues Li(thf)2Ni(o-C6H,CH,Fbh2)2(3'P),688 and Ni[C6H3(OMe),],(PR1R2Me), (31P)p87 (3' P)Y9 31P n.m.r. spectroscopy has been used to show that when PdCl(CH2CN)(PPh3)2 is irradiated then PdCl,(PPh,), is formed.690 n.m.r. spectroscopy has been used to I5N by determine the mode of metallation of 1-(2-methylnaphthyl)N=NC6H2Me20H PdC12.691 trans-M(SnC13),L2(M = Pd or Pt) 2J('19Sn,117Sn)between and In is n.m.r. spectra were re~orded.6~~N.m.r. have also data Hz. "P, lI9Sn,and 195Pt { (36) been reported for PdX(R)(PPh,), (13C)p93Pkl[P(CMe,dH2)But23), (3'P)f94 ("C)p9' (37) ("C, "P)f% N~(Bu',PCH,CH~CRCH,CH,PBU'JX 31P;M = Pd (13C,

Pt)f97

[Pd{ CH2CH[CH(C02Et),]CH2NMe,)(dppe)]
R. M. Goel, W. 0. Ogini, and R. C. Srivastava, Oryanomrtallics, 1982, 1, 819. A. B. Goel and S. Goel, Inorg. Chim. Acta, 1982, 65, L77. R. S. Paonessa and W. C. Trogler, J. Am. Chrm. Soc., 1982, 104, 3529. 682 J. R. Fisher, A. J. Mills, S. Sumner, M. P. Brown, M. A. Thomson, R. J. Puddephatt, A. A. Frew, L. Manojlovic-Muir. and K. W. Muir, Organometallics, 1982, I, 1421. 683 R. H. Hill, P. de Mayo, and R. J. Puddephatt, Inorg. Chem., 1982, 21, 3642. 684 P. L. Bellon, A. Ceriotti, F. Demartin,G. Longoni, and B. T. Heaton, J. Chem. Soc., Dalton Trans., 1982,
R. Benn, J. Klein, A. Rufinska. and G. Schroth, Z. Naturforsch., Teil B, 1981, 36, 1595. 686 R. Benn and A. Rufiriska, J. Organomet. Chem., 1982,238, C27. 68' S. Takahashi, Y. Takai, H. Morimoto, K. Sonogashira, and N. Hagihara, Mol. Cryst. Liq. Cryst., 1982, 82, 139 (Chem. Abstr., 1982, 97, 154328). 688 H.-P. Abicht, K. Issleib, B. Hipler, and E. Uhlig, Synth. React. Inorg. Met.-Org. Chem., 1982,12, 331. 6g9 M. Wada, K. Nishiwaki, and Y. Kawasaki, J. Chem. SOC., Dalton Trans., 1982, 1443. 690 R. McCrindle, G. Ferguson, A. J. McAlees, M. Parvez, and P. J. Roberts, J. Chem. SOC., Dalton Trans., 1982, 1699. 691 K. Gehrig, M. Hugentobler, A. J. Klaus, and P. Rys, Inorg. Chem., 1982, 21, 2493. b9* K. H. A. Ostoja-Starzewski, P. S. Pregosin, and H. Ruegger, Helu. Chim. Acta, 1982, 65, 785. 693 K. Isobe and S. Kawaguchi, Heterocycles, 1981, 16, 1603. 694 R. G. Goel and W. 0. Ogini, Organometallics, 1982, 1, 654. 695 M.A. Andrew and C.-W. F. Cheng, J. Am. Chem. SOC., 1982, 15,4268. 696 P. Binger, H. M. Buch, R. Benn, and R. Mynott, Angew. Chem., Suppl., 1982, 153. 697 R. J. Errington, W. S. McDonald, and B. L. Shaw, J. Chem. SOC.,Dalton Trans., 1982, 1829. 698 E. L. Weinberg, B. K. Hunter, and M. C. Baird, J. Organomer. Chem., 1982, 240, 95.

dppm),MeL] (31P),723Pt[CH,CH,C(OH)RH,]Cl,(py), (31P),724 (Ph,P),PiCH,CH,CH, (13C, 31P),725 (Pr',P),Pt(CH,),CMe, (31P),726 Pi(CH2C6H4dH2)(cod) ('3C),727 [MePt,(p-dppm),(p-CHJL]' (31P),728 [Ph3PCH2PtC1(PPh3)]+[Pt(CH,PR,)(PR,),X]+ (31P),730 Pt(PPh,),(CH,Cl)I [AlCl,]- (*'Al, "P, 19sPt),729 (31P),731 (Ph3P),Pt(CH,CF3)(00But) (19F, 31P):32 (PR'R2,)C1PtNMe,CH,CHCHCH,NMe,Pt(PR' R2,)C1 ( )c, 31P, 195pt):33

712 '13

M. C. Grossel. R. P. Moulding, and K. R. Seddon, Inorg. Chim. Acta, 1982, 64, L275. K. A. 0. Starzewski and P. S. Pregosin. A t k. Chrm. Srr., 1982, 196, 23. 714 J. H. Nelson and N. W. Alcock, Inorg. C17rm. 1982, 21, 1196. 715 S. Carr, R. Colton. and D. Dakternieks, J. Orgunomrt. Chem. 1982, 240, 143. 71b P. G. Pringle and B. L. Shaw, J. Chem. Soc. Chrm. Commun., 1982, 1313. 7 S. S. Moore and G. M. Whitesides, J. Org. Chem. 1982, 47, 1489. 718 P. K. Monaghan and R. J. Puddephatt. Inorg. Chini. Acra, 1982, 65, L59. A. R. Middleton, G. Wilkinson, M. B. Hursthouse, and N. P. Walker,J. Chem. Soc., Dalton Trans., 1982, 663. 7?o D. W. Meek, R. Waid. K. D. Tau, and R. M. Kirchner, Inorg. Chim. Acta, 1982, 64, L221. 721 A. B. Goel and S. Goel, Inorg. Chim. Acra, 1982. 59. 237. 722 N. C. Payne and D. W. Stephan, J. Organomet. Chrm., 1982, 228, 203. '23 K. A. Azam, R. J. Puddephatt, M. P. Brown, and A. Yavari, J. Organomet. Chem., 1982, 234, C31. 724 J. T. Burton and R. J. Puddephatt, J. Am. Chem. Soc., 1982, 104, 4242. 7?5 R. J. Klinger, J. C. Huffman. and J. K. Kochi. J. A m. Chem. SOC., 1982, 104, 2147. ' Z h R. DiCosimo and G. M. Whitesides, J. Am. Chrm. Soc., 1982, 104. 3601. 727 M. F. Lappert,T. R. Martin, C. L. Raston. B. W. Skelton, and A. H. White, J. Chem. SOC.,Dalton Trans., 1982, 1959. 728 K. A. Azam, A. A. Frew. B. R. Lloyd, L. Manojlovic-Muir. K. W. Muir. and R. J. Puddephatt,J. Chem. SOC.,Chem. Commun., 1982, 614. 729 0. J. Scherer and H. Jungmann, J. Organomer. Chem. 1982, 228, C61. 730 N. J. Kermode, M. F. Lappert, B. W. Skelton, A. H. White, and J. Holton, J. Organornet. Chem., 1982, 228, C 7 1. 731 C. Engelter, J. R. Moss, M. L. Niven, L. R. Nassimbeni, and G. Reid, J. Organomet. Chem., 1982, 232, C78. :32G. Strukul, R. Ros, and R. A. Michelin. Inorg. Chem., 1982, 21, 495. 733 J. R. Briggs, C. Crocker, W. S. McDonald, and B. L. Shaw, J. Chem. SOC., Dalton Trans., 1982, 457.

Me-Pt-P

P-Pt -Me U P h ,

35 cis-PtR R2(PR3,),

[d(Bu'2CH2CH2 CHCH2CH,PBut2)Y]

(,' P),7,,

(31P),735

Cobalt. Enantiomerization of [Co,(CO),CCHR]
has been investigated and
AG*22, determined as 10.5
0.1 kcal r n ~ l - '. ' ' ~ ~
Rhodium. 'H n.m.r. spectra of [PtRh2(p-H)(p-CO)2(CO)2(q5-C5Me5)J show hydride exchange with coupling to one rhodium at low temperature and two at high temperature. 13C and ,'P n.m.r. spectra were given for [PtRh,(p-H)(pC0)2(CO)(PPh3)(q-CsMe5)2] Dynamic 13C n.m.r. spectroscopy has been used to investigate olefin rotation in (acac)Rh(RCH=CH)2.'03SN.m.r. studies have established that (q3-CH2c6Me,)Rh[P(OPri),], is highly fluxional, and the transition state was proposed to be an q'-benzyl complex rather than [1.5]sigmatropic shifts.'036 Variable-temperature 13C n.m.r. spectra have shown fluxional behaviour of the cyclo-octadiene moiety in p[NN'-(0-phenylene)bis(slicylaldiminato)] bis(q-l,5-~od)Rh,.'~~~ Exchange between pyrazolyl groups in B(pz),Rh(cod) has been investigated,lo3*The fluxionality of Rh,(p-CO),(CO)(C,has been investigated using 13Cn.m.r. spectr~scopy.''~~ "P n.m.r. specThe trum of { Rh(C,Me,)Cl[ R2N(CH3,PPh2],} shows the presence of four rotamers
M. A. Bennett, I. J. McMahon,andT. W. Turney, Angew. Chem.,lnt. Ed. Engl., 1982,21,378; Suppl. 853.
1024 P. Bischofberger and H.-H. Hansen, Helu. Chim. Acta, 1982, 65, 721. 1025 P. Hachett, B. F. G. Johnson, and J. Lewis. J. Chem. SOC., Dalton Trans., 1982, 939. 1026 K. J. Karel, T. A. Albright, and M. Brookhart, Organomerallics (Washington, D.C.), 1982, 1, 102' C. lo28 H. 1029 G.
E. Johnson and W. C. Trogler, Inorg. Chem., 1982, 21, 427. Patin, G. Mignani, A. Benoit, J.-Y. Le Marouille, and D. Grandjean, Inorg. Chem., 1981,20,4351. Jaouen, A. Marinetti, B. Mentzen, R. Mutin, J. Y. Saillard, B. G. Sayer, and M. J. McGlinchey, Organometallics, 1982, 1, 753. D. A. Roberts, A. D. Harley, and G. L. Geoffroy, Organometallics, 1982, 1, 1050. 1031 G. Suess-Fink, U. Thewalt, and H. P. Klein, J. Organomet. Chem., 1982, 224, 59. 1032 S. C. Grocott and S. B. Wild, Inorg. Chem., 1982, 21, 3535. 1033 R. T. Edidin, J. R. Norton, and K. Mislow, Organomerallics (Washingron, D.C.), 1982, 1, 561. 1034 M. Green, R. M. Mills,G. N. Pain, F. G. A. Stone, and P. Woodward, J. Chem. SOC.,Dalton Trans., 1982,
D. Parker, J. Organomet. Chem., 1982, 240, 83. 10% R. R. Burch, E.L. Muetterties, and V.W. Day, Organometallics (Washington, D.C.), 1982,1, 188, 1016. 1037 R. Bonnaire, J. M. Manoli, C. Potvin, N. Platzer, N. Goasdoue, and D. Davoust, Inorg. Chem., 1982,21,

Ionic Equilibria The anionic contribution to 'H chemical shifts of aqueous acid solutions does not affect the dissociation constants derived from the measured chemical shifts."7631P n.m.r. data have been used to show that divalent cations bind to tRNA phosphate 'H n.m.r. spectra have been used to determine stability constants between Mg2+,Ca2+,Mn2+,Cu2+,Zn2+,Cd2+,or Ag+ and dbiotin, tetrahydrothiophene, and Me2S.lt7'The qpclear quadrupolar relaxation of 'Li, 23Na,and 63Cuin ionic melts has been e ~ p l a i n e d. " ~ ~ complex stability of The
Derouault, P. Granger, and S. Chapelle, Inorg. Chem., 1982, 21, 1040. M. Dalibart, J. Derouault, and P. Granger, Inorg. Chem., 1982, 21, 2241. 1165 J. W. Akitt, J. Chem. Soc., Faraday Trans. 2, 1982, 78, 289. 'IM V. I. M.ikhaibv and V. I. Chizhik, Veshr. Lmingr. Uniu., Fiz., Khim, 1982.81 (Chem. Abstr., 1982.97,

1163 M.Dalibart, J.

1982,23, 269 (Chem. Abstr., 1982,97, 151 478). V. P. Tarasov, G. A. Kirakosyan, S. B. Randarevich, and Yu. A. Buslaev, Koord. Khim., 1982,8, 1087 (Chem. Abstr., 1982,97, 189014). 1169 T. Matsumoto and K. Ichikawa, Nippon Kagaku Kaishi, 1982, 1100 (Chem. Abstr., 1982,97,65 288). 1170 N.N.Shapek'ko, Yu. S. Bogachev, V. G. Khutsishvili, and N. P. Bulatova, Zh. Obshch. Khim., 1982,52, 740 (Chem. Abstr., 1982, %, 206 327). 1171 N. A. Kostromina, N. S. Anikina, and I. D. Vdovenko, Ukr. Khim. Zh. (Russ. Ed.), 1982,48,230 (Chem. Abstr., 1982, % 169 670). , 1172 A. Laaksonen, J. Kowalewski,and B. Jonsson, Chem. Phys. Lett., 1982,89,412. 1173 T. Sugawara, M. Yudasaka, K. Takahashi, R. Tamamushi, H. Iwamura, and T. Fujiyama, Bull. Chem. Soc.Jpn., 1982, 55, 1959. 1174 M. Y u h k a , T. Supwara, H. Iwamura, and T. Fujiyama, Bull. Chem. Soc. Jpn., 1982.55, 311. 1175 N. Soffer and Y. Marcus, Ber. Bunsenges. Phys. Chem., 1982,86, 72. 1176 J. W. Akitt, J. Chem. SOC., Faraday 7bans. I , 1982, 78, 607. 1177 M. Gueron and J. L. Leroy, Biophys. J., 1982,38,231 (Chem. Abstr., 1982,97, 34870). 1178 H.Sigel and K. H. Scheller, J. Inorg. Biochem., 1982, 16, 297. 1179 K. Ichikawa and T. Matsumoto, Nippon Kagaku Kaishi, 1982, 887 (Chem. Abstr., 1982, 97,79 341).

L. C. Damude. P. A. W. Dean. M. D. Sefcik, and J. Schaefer, J. Orgunomet. Chem., 1982, 226, 105. P. F. Barron, J. Organomer. Cheni. 1982, 236. 157. 1736 I. D. Vagner, T. Maniv, and E. Ehrenfreund. Solid Stare Conimun. 1982,44,635 (Chem. Abstr., 1982,97, 1). 1737 A. Lotz, E. Palangie, and J. Voitlander. J. Muyn. Reson., 1982, 50, 417. 1738 C. A. Fyfe,G. C. Gobbi, J. S. Hartman, R. E. Lenkinski.J. H. OBrien, E. R. Beange,and M. A. R. Smith, J. Magn. Reson., 1982. 47, 168. 1739 R. E. J. Sears, J. Chem. Phys., 1982, 76, 5651. 1740 W. J. Dell and P. J. Bray, Phys. Chem. Glasses, 1982, 23, 126 (Chem. Abstr., 1982, 97, 221 570). 1741 S. Simon,V. Simon, and A. Nicula, Stud. Unit. Babes-Bolyai, Ser. Phys. 1981,26,50 (Chem. Abstr., 1982, 97, 27 538). 1742 S. Simon, V. Simon, and A. Nicula, Stud. Unir. Babes-Bolyai, Ser. Phys., 1981,26, (Chem.Abstr., 1982, 97, 10). 1743 I. Ardelean, M. Coldea, and 0.Cozar, Nucl. lirsrrum. Methods Phys. Res., 1982,199, 189 (Chem. Abstr., 1982, 97, 119 397). I744 0. V. Falaleev and E. P. Zeer, J. Mol. Srruct., 1982, 83, 257. 1745 S. A. Feller, W. J. Del1,and P. J. Bray, J. Non-Crysr. Solids, 1982,51,21 (Chem. Abstr., 1982,97,206 973). 1746 P. W. France and M. Wadsworth, J. Magn. Reson., 1982, 49,48. 1747 S. Schramm and E. Oldfield, J. Chem. Soc., Chem. Cornmun., 1982,980. '748 R. Goering, H. Buerger, H. Nass, and B. Schnabel, Phys. Status Solidi A , 1981, 68, K29. 1749 W. Schiller, D. Mueller, and G. Scheler, Z. Chem., 1982, 22, 44 (Chem. Abstr., 1982, 96,222067). 1'50 R. J. Araujo and J. W. H. Schreurs, Phys. Chem. Glasses, 1982,23,108 (Chem. Abstr., 1982,97, 132 152). 1751 H. J. Behrens and B. Schnabel, Physica B + C (Amsterdam), 1982, 114, 185 (Chem. Abstr., 1982, 97, 173 742). 1752 F. Von Lampe, D. Miiller, W. Gessner, A. R. Grimmer,and G. Scheler, Z. Anorg. AIIg. Chem., 1982,489, 16.

1734 1735

in KAl(S04)2 12H20has been described.'753The effect of uniaxial pressure on 27Al n.m.r. spectra of ruby has been i n ~ e s t i g a t e d.The ~ ' ~ ~ possible use of 27Al n.m.r. spectroscopy with CPMAS has been investigated for various a l u r n i n a ~. ' ~ ~ ~ CPMAS I3C n.m.r. spectroscopy has been used to study the structure and position of [Pr,N] in ZSM-5-type zeolites.'756Broad-line 23Na n.m.r. spectroscopy has been used to investigate the existence and growth of a nucleation centre with a faujasite-type s t r u c t ~ r e. ' ~The " mechanism of dealumination~~ ~~~ ultrastabilization of faujasite zeolite catalysts has been studied by 27Al and 29Si n.m.r. s p e c t r o s ~ o p y. High-resolution solid-state 27Al n.m.r. spectra of a number '~~~ of zeolites with different framework structureshave been recorded at 104.2 M H Z. ' ~ ~ The structure of silicate catalysts has been studied by 27Al and BSi magic-anglespinning n.m.r. spectro~copy.'~~' n.m.r. spectra have been obtained for a series of BSi , 14 synthetic faujasite zeolites, and chemical shifts fall in the range -80 to 1 - 110 ~. p. m.27Aln.m.r. spectroscopy has been used to study ZSM-5-type zeolite '~~~ t aluminosilicate precursor species.'763High-resolution 29Si n.m.r. spectroscopy is valuable in determining the environment of silicon in zeolites'764--* and 772 t~bermorites.'~~~ In crystals of alkali feldspars, 27Al n.m.r. has provided more exact quantitative information on order and twinning balance than did X-ray powder diffractometry

G. Greenbaum, W. E. Carlos, and P. C. Taylor, Solid State Commun., 1982, 43, 663 (Chem. Abstr., 1982,97, 137484). 1794 W. L. Earl and D. L. Van der Hart, J. Magn. Reson., 1982,48, 35. I795 L. E. Gorsh, A. A. Shubin, V. M. Nekipelov, and A. N. Kanev, Zh. Strukt. Khim., 1982,23, 26 (Chem. Abstr., 1982, 97, 144910). 17% L. Bemi, H. C. Clark, J. A. Davies, D. Drexler,C. A. Fyfe, and R. Wasylishen,J. Organomer. Chem., 1982, 224, c 5. 1797 A. R. Grimmer, P. Starke, and W. Wieker, Z.Chem., 1982, 22,44 (Chem. Abstr., 1982,%, 149 735). 1798 E. Lippmaa, M. Magi, M. Tarmak, W. Wieker, and A. R. Grimmer, Cem. Concr. Res., 1982,12, 597 (Chem. Abstr., 1982, 97, 173 937). 1799 E. Lippmaa, A. Samoson, M. Magi, R. Teeaar, J. Schraml, and J. Koetz, J. Non-Cryst. Solids, 1982,50, 215 (Chem. Abstr., 1982,97, 221 556). M. Le Floch-Durand, U.Haeberlen,and C. Mueller, J. Phys. (Les Ulis, Fr.), 1982,43,107 (Chem. Abstr., 1982, %, 61 994). 1801 D. I. Vainshtein, V. D. Schchepkin, V. A. Safin, V. M. Vinokurov, and A. V. Chadvik, Fiz. Tverd, Tela (Leningrad), 1982, 24, 1904 (Chem. Abstr., 1982, 97, 82922). 1802 B. K. Hunter and R. J. C. Brown, J. Magn. Reson., 1982,46, 227. 1803 P. N. Tutunjian and J. S. Waugh, J. Chem. Phys., 1982, 76, 1223. 1804 L. W. Dennis, V. J. Bartuska, and G. E. Maciel, J. Am. Chem. Soc., 1982, 104, 230. 1805 J. P. Dutasta, J. B. Robert, and L. Wiesenfeld, Am. Chem. Soc., Symp. Ser., 1981,171,581 (Chem. Abstr., 1982, %, 27619). T. Weller, U. Franck,G. Klose,and R. Lochmann,Z. Chem., 1982,22,62(Chem. Abstr., 1982,97,92 396). I8O7 P. N. Tutunjian and J. S. Waugh, J. Magn. Reson., 1982, 49, 155.

1793 S.

or Te).I8O8 "P n.m.r. spectra of glassy semiconductor selenides have been determined.'8w The effect of vibrations on water molecules in crystals on n.m.r. spectra has been measured.'810 77Se high-resolution n.m.r. spectra of CsH3(Se03)2'811.'8'2 and NH4HSe04'813*'814 have been reported. High-resolution solid-state I3C n.m.r. spectra have been obtained for several tellurium co-ordination complexes including Te(S2CNEt2),.'8'5 The '29Xe nuclear shielding and shielding anisotropy of Xe trapped in quinol chlathrates have been obtained by 'H-enhanced MAS '29Xen.m.r. spect roscopy.'816 MoleculesSorbed Onto Solids.-This section is divided into two subsections: 'Water Sorbed Onto Solids' and 'Atoms and Other Molecules Sorbed Onto Solids'. Water Sorbed Onto Solids. The specific surface of cements and hydrates has been studied by nuclear spin-lattice r e l a ~ a t i o n. ' ~ ' ~. ' ~ nature of water on titanium The ' ~ hydroxide films has been in~estigated.'~'~ adsorbed on porous glass has been Water studied.'820The behaviour of water in suspensions of swelling smectites or kaolinite has been studied using 'H and 2H relaxation measurements.'82' The pressure dependence of in H and D molecules near the kaolinite surface does not show a major change in the hydrogen-bonded structure as is observed in bulk H or D20.1822 n.m.r. spectroscopy has been used to study the microdynamic and 'H thermodynamic behaviour of water in clay suspensions.'823 The n.m.r. pulsed-fieldgradient technique has been applied to self-diffusion studies of water and light

that the process of ethylene addition on the Zr-H and Zr-C bonds is preceded by a reversible adsorption of ethylene on the Zr ion.1840 The 13C n.m.r. spectrum of pyridine adsorbed on y-A1203 has been obtained using CPMAS n.m.r. spectroscopy.'841N.m.r. spectroscopy has been used to study the adsorption of polyvinyl alcohol on the surface of A1203.1842 desorption kinetics of dodecane and The dodecene from porous glasses have been studied by n.m.r. spectroscopy.'843 N.m.r. pulsed-field-gradient and n.m.r. tracer-desorption techniques have been used in search of surface barriers on zeolite crystallites and applied to the C2H2NaCaA system.1844 High-resolution 13C n.m.r. spectroscopy has been used to identify carbonaceous residues on H-ZSM-5 and H-mordenite catalysts used in the conversion of MeOH and ethylene to higher hydrocarbon^.'^^^ 13C, 170,and 27Al n.m.r. shielding tensors have been calculated using coupled Hartree-Fock calculations for the A13+/C0system and compared with a 13Cn.m.r. investigation of CO adsorbed on decationated zeolites.1846 Highly resolved I3Cand "N n.m.r. spectra of MeCN adsorbed in zeolites X have been measured and depend on the exchangeable cation.1847 n.m.r. spectroscopy has been used to investigate the adsorption of "N NH,, Me3N, pyridine, and acetonitrile on zeolites.'848 The intermolecular interactions of Et3N with the sulpho-cation-exchange KU-2 and different solvents have been studied by 'H and 13Cn.m.r. ~ p e c t r o s c o p y.High-resolution 13Cn.m.r. '~~~ spectra have been obtained for benzoate, acetate, formate, [HC03]-, [C0,l2-, and [C20412- inside anion-exchange resins.1850Using 27Al n.m.r. spectroscopy, the electric-field gradient of aluminium positions in decationated zeolites has been studied.1851 n.m.r. spectroscopy has been used to identify surface intermediates 13C in the reaction of methanol of HY ze01ite.l~~~ n.m.r. spectroscopy has been '29Xe used to study xenon adsorbed on zeolite^.'^^^-'^^' The dynamics of methane monolayers adsorbed on graphite have been studied.1856 31P n.m.r. spectroscopy has been used to identify Rh(acac)(CO)bound to a phosphinated p ~ l y p r o p y l e n e. ' ~ ~ ~ The power of solid-state 13C n.m.r. spectroscopy for the characterization of

l x W G. A. Nesterov,

V. M. Mastihkin, 0.B. Lapina. and V. A. Zakharov, React. Kinet. Catal. Lett., 1982,19, 175 (Chem. Abstr., 1982, 97, 56301). IX41W. H. Dawson, S. W. Kaiser, P. D. Ellis, and R. R. Inners, J. Phys. Chem., 1982, 86, 867. 1842 B. E. Platonov, A. G. Bratunets, F. D. Ovcharenko, and T. A. Polishchuk, Kolloidn. Zh., 1982,44, 360 (Chem. Abstr., 1982, 97, 12371). 1843 W. Heyer, F. Janowski, J. Kaerger, J. Lenzner, H. Pfeifer, and F. Wolf, Z. Chem., 1982,22, 152 (Chem. Abstr., 1982, 96,206024). 4 J. Kaerger, W. Heink, H. Pfeifer, M. Rauscher, and J. Hoffmann, Zeolites, 1982,2,275 (Chem. Abstr., 1982,97, 223 582). I X E. G. Derouane, J. P. Gilson. and J. B. Nagy, Zeolites, 1982, 2, 42 (Chem. Abstr., 1982, 97, 1 582). 1846 Th. Weller, W. Meiler, A. Michael, H. J. Kohler, H. Lischka, and R. Holler, Chem. Phys., 1982,72, 155. 1847 I. Juenger, W. Meiler, and H. Pfeifer, Zeolites, 1982 2, 310 (Chem. Abstr., 1982, 97. 223 652). 1848 D. Michel, A. Germanus, and H. Pfeifer, J. Chem. SOC., Faraday Trans. I , 1982, 78, 237. 1849 A. A. Samoilenko, G. A. Grifor'eva, N. N. Shapet'ko, and N. I. Nikolaev, Teor. Prakt. Sorbtsjonnykh Protsessou, 1981, 14. 35 (Chem. Abstr., 1982, %, 110755). W. B. Smith, E. T. Strom, and D. E. Woessner, J. Magn. Reson., 1982,46, 172. 1851 V. Bosacek, D. Freude, T. Froehlich, H. Pfeifer,and H. Schmiedel,J. Colloid Interface Sci., 1982,85,502. ISs2 T. Kotanigawa, K. Shimokawa, and T. Yoshida, J. Chem. SOC., Chem. Comrnun., 1982, 1185. 1853 T. Ito and J. Fraissard, J. Chem. Phys., 1982.76, 5225. Igs4 L. C. De Menorval, J. P. Fraissard, and T. Ito, J. Chem. SOC.,Faraday Trans. I , 1982, 78, 403. 1855 J. Fraissard,T. Ito, L. C. De Menorval, and M. A. Springuel-Huet, Stud. Su$ Sci. Catal., 1982,12, 179 (Chem. Abstr., 1982, 97, 223 583). J. H. Quateman and M. Bretz, Phys. Rec. Lett., 1982, 49, 1503 (Chem. Abstr., 1982, 97, 223587). Ig5' F. R. Hartley, S. G. Murray, and P. N. Nicholson, J. Mol. Catal., 1982, 16, 363.

Nucleur Magnetic. Resonance Sprc.rr-oscop~
1-ClB5H7 ["B; M = CpFe(CO),, Co(CO),. Mn(CO),, Re(CO)S, or IrX2(CO)(PMe3)J,1894 B,H,L (11B),1895 l-(Cl,B)B,H, (11B),18%(2,3-Et2C2B4H4)-2("B, 4-Et,P-1,7Co(B5HIO) ("B),18974,6-(Et,P),-1,7-R,-1,4,7-CPtCB,H, J1P),ld98 M ~ , - C L ~. ~ - [ C ~ H ( P E ~ , ) ~ - ~ - H - ~ - ( P E ~ , ) ] - ~ , ~ , ("B, C O C B , H , bu tenyl ~ - C 31P),1899 derivatives of C2B5H7 (11B),1900 Me3N-5-C1-cfoso-2,4-C2B5H6 ( 'lB),1901 6-(C5Me,)CoB,H,, (I*B),1Y02 C,Me,CoB,H,, (l'B),1903HIrB,H,,(PMe3), ("B, 3'P),1904 10-Br-1,2,3-CpCoC2B,H, (11B),1905 3,1,2-(C,H,)RuC,B,Hl, (11B),19M halogenation products of [(C2B,H,,),Co](11B),1907 (C,B,H,,)(Ph,P)RhCPh= CHC(PPh3)=dPh ("B, 31P),1908 closo-2,2-(PPh3),-2-H-2,1,12-RhC2B9Hl I (11B),1909(PPh3)2RhC2B,H I R2 ( 31P),1910-( 1'-C3Hs)-l ,2-C,Bl0H ,,R 1 ( l1B),I9' 1-n-pentyl-o-carbaborane (I3C),l9'* and CoFe(Me,C,B,H,)(PEt,), (I'B, 31P).1913
Other Compounds of Boron.-In [(PhC=C),B] and (PhCrC),BX3_,,,'J(13C,*'B) c o m p n d s roughly with 1J(13C,'3C).The chemical shifts, S(I3C), reveal B-C (pp) nbonding, which is rather weak when compared with Ct-C ( p p ) n - b ~ n d i n g. 'In' ~ ~ ([(mesityl),B],CH) -, ',C n.m.r. spectroscopy shows that the negative charge is d e l o c a l i ~ e d. ' ~ ' ~ data have also been reported for [Me,B(SiMe,),_,]- ("B, N.m.r. 29si)1'9'6 (C9H,,)BPr' (13C),'9'7 (menthyl)( EtCHMe)(C,H, I)B(11B),1918 (norbornyl),B ( l l ~ 13c),1919 C8H14BCH , =CMeHex" (13C),1920 PhEkH,CH=CHCH, (11B),1921
1894M. B. Fischer, D. F. Gaines, and J. A. Ulman, J. Orpriomrr. C'krm., 1982, 231. 55. 1R95N. W. Alcock. H. M. Co1quhoun.G. Haran. J. F. Sawyer.and M. G. H. Wallbridge,J. Chem. SOC.Dalton

Trans., 1982. 2243.

18% D. F. Gaines, J. A. 1897 L. Borodinsky and
Heppert, D. E. Coons. and M. W. Jorgenson. lirory. C'hein. 1982, 21, 3662. R. N. Grimes, Inory. Chem. 1981. 21. G. K. Barker. M. P. Garcia. M. Green. F. G. A. Stone. and A. J. Welch.I. Chew. SO^,. Ch4171. Cornmun.,

1982, 46.

G.K. Barker, M. P.Garcia, M.Green, F. G.A. Stone, H. E. Parge. and A. J. Welch,J. Chem. SOC.,them.

Cornmun., 1982. 688.

R. Wilczynski and L. G. Sneddon. f n o r y. Chem., 1982, 21. 506.
1901 G. Siwapinyoyos and T. Onak. fnorg. Chem., 1982, 21, 156. I9O2 T. L. Venable, E. Sinn. and R. N. Grimes. fnory. C'hern. 1982. 21. 895. T. L. Venable and R. N. Grimes. Inorg. Chem. 1982. 21. 887. I9O4 S. K. Boocock, J. Bould, N. N. Greenwood, J. D. Kennedy, and W. S. McDonald. J. Clirm. Soc.

M. E. Glogowski, N. Zumbulyadis, and J. L. R. Williams, J. Organomet. Chem., 1982, 231, 97, H. Klusik and A. Berndt, J. Orgunomet. Chem., 1982, 234, C17. S. Amirkhalili, R. Boese, U. Hohner, D. Kampmann, G. Schmid, and P. Rademacher, Chem. Ber., 1982, 115. 732. I9xS. Amirkhalili, U. Hohner, and G. Schmid, Angeu. Chem., f n t. Ed. Engl., 1982, 21, 68; Suppl., 50. 1926 E. Hohaus, Z. Anorg. Allg. Chem., 1982, 484, 41. 1927 S. U. Kulkarni, D. Basavalah, M. Zaldlewicz, and H. C. Brown, Organonietallics, 1982, 1, 212. 192* H. C. Brown and S. Narasimhan, Organometullics, 1982, 1, 762. 1929 K. Hennemuth, A. Meller, and M. Wojnowska, Z. Anorg. Allg. Chem. 1982, 489, 47. 1930 R. Csuk, H. Honig, and C. Romanin, Monatshefte, 1982, 113, 1025. 1931 B. Wrackmeyer and R. Koester, Chem. Ber., 1982, 115, 2022. 1932 W. Biffar and H. Noth, Z. Natur$orsch., Teil B, 1981,36, 1509 (Chem. Abstr., 1982,96, 162800). 1933 P. Paetzold and C. v. Plotho, Chem. Eer., 1982, 115, 2819. 1934 W. Maringgele, Chem. Ber., 1982, 115, 3271. 1935 H. Noth, R. Staudigl, and H. U. Wagner, Inorg. Chem., 1982, 21, 706. 1936 U. Sicker, A. Meller, and W. Maringgele, J. Organornet. Chem., 1982, 231, 191. 193' R. H. Cragg and T. J. Miller, J. Organomet. Chem., 1982, 232, 201. 1938 R. H. Cragg and T. 1 Miller, J. Organomet. Chem., 1982,235, 143. 193y P. G. M.Wuts and P. A. Thompson, J. Organomet. Chem., 1982,234, 137. 1940 C. Eaborn, N. Retta, J. D. Smith, and P. B. Hitchcock, J. Organornet. Chem., 1982, 235, 265. 1941 A. Fox, J. S. Hartman, and R. E. Humphries, J. Chem. SOC.,Dalton Trans., 1982, 1275. 1942 R. F. Childs, D. L. Mulholland, and A. Nixon, Can. J. Chem., 1982, 60,801. 1943 J. M. Walker, R. J. Starks, G. A. Gray, and J. N. Schoolery, Appl. Spectrosc., 1981,35,607 (Chem. Abstr., 1982, %, 62 256). 1944 F. Alam and K. Niedenzu, J. Organomet. Chem., 1982,240, 107. 1945 K. Niedenzu, S. S. Seelig, and W. Weber, Z. Anorg. Allg. Chem., 1981, 483, 51. 1946 J. Higashi, A. D. Eastrnan, and R. W. Parry, Inorg. Chem., 1982,21, 716.

(Z;B-pJR

1-BF2-1,2,3,4-tetrahydro-l,10-phenanthroline I5N, 19F),'947 (13C, Me,SihBXSSdX 29si),1948 Bus2NBXNHSiMe, ('1B),1949 bis(oxa1ato)borates ( '1B),'9s0(70) (11B).1954 (1'B),1951 ("B, 13C),'952 (71) X m (11B),1953 and

( l l ~ ,I ~ F ,

Complexes of Other Group IIIB Elements.-A 27A1 n.m.r. study has shown the Low-temperature 'H formation of NaAlH(NR,), in THF solutions of R2NH.'955 n.m.r. data of Et2AICH2AIEt2OEt, indicate that the ether 0 is simultaneously coordinated to both aluminium atoms.1956 N.m.r. data have also been reported for [(C,e ) R] (13C),1957 (13C),'958 M , AICI (72) and [2- Me,NCH(SMe)C, H 4 ] h Me,

Ph2P(CH2)20(CH2),O(CH2)2PPh2 (13C),222" (F,C6),PCH2CH2P(C6F,), ("F),ZZ2' Ph2P(0)R (I3C, 31P),2222--2224&F Ph$'C (I3c,31P),2225P(C&X), (l3C, 31P),2226 2-HOC6H4PPh2 (I9F, 31P),2227 PhP= C[NPh(SiMe,)]PPhPPhCand [NPh(SiMe,)] = PPh (31P).2228 The 'H n.m.r. spectra of stibabenzenes and bismabenzenes show very highfrequency signals for the a-protons. 13Cn.m.r. spectra were also re~orded.2,~~ (oFor C6H4D),Bi it is possible to assign the o-hydrogen.22M n.m.r. data have been 13C reported for (CH,=CH),M (M = As or Sb).223' 31Pn.m.r. chemical shifts of R'R2R3P=NX have been correlated with the substituent constants.2232 N.m.r. data have also been reported for R' R2C=NN=PPh3 (13C),2233 Me,PPMe,=C(PMe,), (I3C, 31 P)?'" [*= PPh,CH,CH, PPh,]' (31P),2235 PMeR'R20 (3'P),2236 PR1,R2(0) (13C, 31P),2237 Ph(O)PCH&HOCHCH, (31P),2238 ( 13C),2239 (99) Ph3P(OC6H3CI-3,4)2 (13C, 31P),2240P(C&R)2(C6H&H= CHPhKO) (31P),2241 (10o) t 3 C ,
W. E. Hill, J. G. Taylor, C. A. McAuliffe, K. W. Muir, and L. Manojlovic-Muir, J. Chem. SOC.,Dalton Trans., 1982, 833. 2221 R. L. Cook and J. G. Morse, Inorg. Chem., 1982, 21, 4103. 2222 M. Dankowski and K. Praefcke, Phosphorus Sulfur, 1982, 12, 131. 222) E. Lindner, M. Steinwand, and S. Hoehne, Angew. Chem., Int. Ed. Engl., 1982, 21, 355; Suppl., 913. 2224 E. Lindner, M. Steinwand, and S. Hoehne, Chem. Ber., 1982, 115, 2181. 2225 H. B. Stegmann, H.-M. Kuhne, G. Wax, and K. Schemer, Phosphorus Sulfur, 1982,13, 331. 2226 T. Allman and R. G. Goel, Can. J. Chem., 1982,60,716. z2'J. Heinze-Sauer, Report, 1980, Order No.PB82-1160%, pp. avail. NTIS -from Gov. Rep. Announce. 97 Index (US.), 82, 272 (Chem. Abstr., 1982, W,162837). 1982, 2228 R. Appel, V. Barth, and M. Halstenberg, Chem. Ber., 1982, 115, 1617. 2229 A. J. Ashe, tert., T. R. Diephouse, and M.Y. EISheikh, J. Am. Chem. Soc., 1982, 104, 5693. 2230 U. Praeckel and F. Huber, J. Organomet. Chem., 1982,240, C45. 2231 K. Sille, J. Weidlein, and A. Haaland, Spectrochim. Acta, Part A, 1982, 3 ,475. Yu. P. Egorov, A. A. Kudryavtsev, A. M.Pinchuk, A. P. Marchenko. and V.A. Kovenya, Dor. Eksp. Khim., 1982, 18, 58 (Chem.Abstr., 1982, 96, 198948). 2233 N. Suzuki, K. Sano, S. Wakatsuki, and Y.Izawa, Bull. Chem. Soc. Jpn., 1982, 55, 842. 22% H.H.Karsch, Chem. Ber., 1982, 115, 1956. 2235 A. Schmidpeter, S. Lockschmidt, and W. S. Sheldrick, Angew. Chem., Int. Ed. Engl., 1982, 21. 63. 2 M C. Laurenp, L. Villien, and G. Kaufrnann, J. Chem. Res. ( S ) , 1982, 12. M.Savignac, P. Cadiot, and F. Mathey, Can. J. Chem., 1982,60, 840. 2238 R. Bodalski, T. Janecki, Z. Galdecki, and M.GTbwka, Phosphorus Suyur, 1982,14, 15. 2239 L.D. Quin, K. A. Mesch, R. Bodalski, and K. M. Pietruskwkz, Org. Magn. Reson., 1982,20, 83. 2240 E. Grochowski, B. D.Hilton, R. J. Kupper, and C. Michejda, J. Am. Chem. Soc., 1982,104,6876. J. 2241 T. Butters, I. Haller-Pauls, and W. Winter, Chem. Ber., 1982, 115, 578. 2242 J.-M. Alcarez, A. Braque, and F. Mathey, Tetrahedron Lett., 1982, 23, 1565. 2243 E. F. Landvatter and T. B. Rauchfuss, J. Chem. Soc.,Chem. Commun., 1982, 11 70.

1947. E. 1. Smirnova, A. I. Zavalishina, A. A. Borisenko, M.N. Rybina, and E. E. Nifant'ev,Zh. Obshch. Khim., 1981,51, 1956 (Chem. Absrr., 1982,%, 68950). 2379 G. Zon, S. M. Ludeman, E. M. Sweet, W. Egan, and L. R. Phillips, J. Pharm. Sci., 1982,71,443 (Chem. Abstr., 1982, 97, 16494). 2380 F. P. Tsui, F. A. Robey, T. W. Engle, S. M. Ludeman, and G. Zon, J. Med. Chem., 1982,25,1106 (Chem. Absrr., 1982, 97, 65 934). 2381 Z. Wang, S. Yang, Y. Yang, and Y. Bi. Huaxue Tongbao, 1981,647 (Chem. Abstr., 1982,%, 122092). 2382 T. Miyajima, Y. Miyahara, and S. Ohashi, Polyhedron, 1982, 1, 425.
assigned based on J(31P,'3C) J(3'P,14N).2383 and N.m.r. data have also been reported for PhOP(O)(NMeN H &N HNH Me) (3' P),2384 (PhO),P(O)N = PC1, (31P):385 (RO),P(O)NHSCF, (I9F, 31P),2386 Me,$JPOCHMeCHMed (31P),2387 (RO),(O)PNCS (31P)?388 (107) (13C, 31P),2389 (MeS)(O)$OCH,CH,CH,NH (13C,
31P):3w (MeNH)(S)POC(CH&H,O (31P),2391 EtOP(S)(NHCHMe,)OC,H4R-4 (I~c, 31p),2392 R1R2NP(OR3)2S (31P),2393 Cl,P= NPC1,O (31P)?394and dCH2CH20AkP(0)(OR)2 (31P).2395 "P n.m.r. reference standards have been examined, and the external reference correction has been given for H3P04 and [(HOCH,),P] +?396 Polyphosphate n.m.r. spectroscopy.2397 chemical shifts and 13C species have been identified using 31P J(31P,'3C) for (PhO)3P0 and 13 alkyl derivatives have been determined and discussed in terms of low-frequency y-shielding effect.2398 labelling has provided l8O evidence against a hexa-co-ordinate phosphorus intermediate during alkaline A hydrolysis of OCH,CH,O $(0Et)(0).2399 number of optimization techniques 7 n.m.r. spectra at natural abundance for a variety of have been used to obtain inorganic and organic phosphates and polyphosphates?m*240L n.m.r. spectros"P copy with i70/'80 labelling has been used to investigate the stereochemistry and
R. Murari, M. M. A. A. El-Rahman, Y.Wedmid,S. Parthasarathy, and W. J. Baumann, J. Org. Chem.,

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2384 T.Buenger
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