The addition of Re(CO)(5)(+) [as Re(CO)(5)FBF3] to P(CN)(3) and to P(CN)(2)(-) affords the complexes [Ro(CO)(5)](3)P(CN)(3)(BE4)(3) and Re(CO)(5)P(CN)(2), respectively. The spectroscopic data indicate that Re(CO)(5)(+) is coordinated to each of the three cyano groups of P(CN)(3) to give {P[C equivalent to N-Re(CO)(5)](3)}[BF4](3), whereas the psoudohalido P(CN)(2)(-) is bonded to the rhenium cation through the phosphorus atom.

All accessible NMR shifts δ³¹P of phosphorus surrounded by four nitrogen atoms are compiled systematically. They cover the relatively wide range from -40 to +50 ppm. All shift differences observed correlate well with changes in nitrogen hybridization: in the order p³ → sp³ → sp² → sp for nitrogen δ³¹P (N₄) is shifted to a higher field. In particular, δ³¹P (N₄) is a linear function of the degree of substitution, when phosphazeno groups are substituted by amino groups in open chain or cyclic systems. This is also true of δ³¹P (0₄) in alkoxy or phenoxy/phosphoroxy substitution series

Like the combination of PCl and AsCl with imino units leads to chlorophosphazanes and chloroarsazanes (RNECl)2,3,4, their combination with ylidediyl units results in the oligomeric compounds (PhP3CECl)2,3,4. which tend, however, more to ionic structures.

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Heteroatom ChemistryVolume 12, Issue 4 p. 181-182 Free to Read A tribute to professor Naoki Inamoto on the occasion of his 72nd birthday Juzo Nakayama, Corresponding Author Juzo Nakayama Regional Editor Department of Chemistry, Faculty of Science, Saitama University, Urawa, Saitama 338-8570, JapanDepartment of Chemistry, Faculty of Science, Saitama University, Urawa, Saitama 338-8570, JapanSearch for more papers by this authorWilliam E. McEwen, William E. McEwen Editor-in-Chief Department of Chemistry, University of Massachusetts, Amherst, MA 01003Search for more papers by this authorAlfred Schmidpeter, Alfred Schmidpeter Regional Editor Department Chemie, Ludwig-Maximilians-Universität, Butenandtstrasse 9, D-81377 München, GermanySearch for more papers by this author Juzo Nakayama, Corresponding Author Juzo Nakayama Regional Editor Department of Chemistry, Faculty of Science, Saitama University, Urawa, Saitama 338-8570, JapanDepartment of Chemistry, Faculty of Science, Saitama University, Urawa, Saitama 338-8570, JapanSearch for more papers by this authorWilliam E. McEwen, William E. McEwen Editor-in-Chief Department of Chemistry, University of Massachusetts, Amherst, MA 01003Search for more papers by this authorAlfred Schmidpeter, Alfred Schmidpeter Regional Editor Department Chemie, Ludwig-Maximilians-Universität, Butenandtstrasse 9, D-81377 München, GermanySearch for more papers by this author First published: 30 May 2001 https://doi.org/10.1002/hc.1029AboutPDF ToolsRequest permissionExport citationAdd to favoritesTrack citation ShareShare Give accessShare full text accessShare full-text accessPlease review our Terms and Conditions of Use and check box below to share full-text version of article.I have read and accept the Wiley Online Library Terms and Conditions of UseShareable LinkUse the link below to share a full-text version of this article with your friends and colleagues. Learn more.Copy URL No abstract is available for this article. Volume12, Issue4Special Issue: A Tribute to Professor Naoki Inamoto in Honor of His Outstanding Contributions to Main Group Chemistry, Part 12001Pages 181-182 RelatedInformation

The solid state 13C and 15N CPMAS NMR spectra of 3,5‐di‐tert‐butyl‐1,2,4‐diazaphosphole 4 and 3,5‐diphenyl‐1,2,4‐diazaphosphole 5 have been recorded. The X‐ray structure of the first compound was already known (it is a cyclic dimer with localized N–H protons) while the structure of the second cannot be determined due to the difficulty to grow suitable single crystals. NMR results pointed out that 4 is a “classical” compound while 5 is probably a tetramer showing Intermolecular Solid‐State Proton Transfer (ISSPT). GIAO/ab initio calculations have been carried out to estimate the absolute 1H, 13C and 15N shieldings. The agreement with the experimental chemical shifts is good enough to assign the signals of carbons C‐3 and C‐5.

The solid state C-13 and N-15 CPMAS NMR spectra of 3,5-di-tert-butyl-1,2,4-diazaphosphole 4 and 3,5-diphenyl-1,2,4-diazaphosphole 5 have been recorded. The X-ray structure of the first compound was already known (it is a cyclic dimer with localized N-H protons) while the structure of the second cannot be determined due to the difficulty to grow suitable single crystals. NMR results pointed out that 4 is a "classical" compound while 5 is probably a tetramer showing Intermolecular Solid-State Proton Transfer (ISSPT). GIAO/ab initio calculations have been carried out to estimate the absolute H-1, C-13 and N-15 shieldings. The agreement with the experimental chemical shifts is good enough to assign the signals of carbons C-3 and C-5.

Ylidyl chlorophosphanes 1 and dichlorophosphanes 2 react with trimethylsilyl phosphanes to yield the ylidyl diphosphanes 3, 4,5, 7 and the 2-ylidyl triphosphanes 8. From the reaction of compounds 1 with lithium diphosphanyl amide and diphosphanyl methanide result the ylidyl diphosphonium ylides 11 and ylidyl diphosphinimines 13. The former rearrange to give the ylidyl triphosphanyl methanes 12. The chloromethyl diphosphinimine 13c enters a cyclization to give the 1,2,3,5-azatriphosphole derivative 14, the structure of which has been solved by X-ray analysis. From the reaction of ylidyl bis(chlorophosphanes) 17 and 20 with the same reagents the 1,2,4,5-tetraphosphinine derivative 18 and the 1,2,3,5,6-azatetraphosphinine derivatives 19 and 21 are obtained.

Bis-triphenylphosphonio-isophosphindolide cations 1 react with triflic acid to give C-protonated products 4, 5 which show an enhanced reactivity to undergo addition of H2O or MeOH to the cyclic π-system. This reaction is the first step of the hydrolytic decomposition of the heterocycle which was monitored by NMR spectroscopic studies. No evidence for direct P-protonation or P-alkylation (which had been postulated in a previous study) was obtained. Addition of H2O or H2S to the cyclic π-system of 1 is also promoted by oxidizing agents such as I3− or sulfur and affords novel zwitterionic (thio)-phosphinates 11, 13.

From the reaction of trimethylsilyl ylides with AsCl3 the dichloroarsanyl ylides 2b and 5b are obtained. As shown by X-ray structure determination, their AsCl2 groups deviate systematically from the symmetric orientation. This conformation enables an effective charge transfer from the ylide moiety to one of the As-Cl bonds, which as a consequence is up to 15 pm longer than the other. At the same time the length of the As-C bonds in 2b and 5b indicates a partial double bond. The effects observed here are of the same type as those observed for the corresponding dichlorophosphanyl ylides; they are, however, more pronounced. The 1:1 condensation of the bis(trimethylsilyl) ylide 3 and AsCl3 yields the oligomers (Ph3PCAsCl)2,3,4. The dimer 7b has a diarsetane structure. HCl adds readily to one of its As-C bonds without opening it. The trimer and the tetramer are ionic. The cation of the trimer forms a six-membered ring with a delocalized arsenium/phosphonium charge, the cation of the tetramer forms a barrelane cage with a phosphonio substituent, and the anion is AsCl4- in both cases (10, 13). An arsa-phosphocyanine cation as in 10 is also part of the diphosphonio isoarsindolide tetrachloroarsenate(III) 12. The structures of 7b.HCl, 10, and 13 reflect again an ylide to As-Cl charge transfer. The As-Cl bonds of 13 are by far the longest ones known for a chloroarsine (average 249 pm).

AbstractChemInform is a weekly Abstracting Service, delivering concise information at a glance that was extracted from about 100 leading journals. To access a ChemInform Abstract of an article which was published elsewhere, please select a “Full Text” option. The original article is trackable via the “References” option.

Ylidyl chlorophosphanes 1 and dichlorophosphanes 2 react with trimethylsilyl phosphanes to yield the ylidyl diphosphanes 3, 4, 5, 7 and the 2-ylidyl triphosphanes 8. From the reaction of compounds 1 with lithium diphosphanyl amide and diphosphanyl methanide result the ylidyl diphosphonium ylides 11 and ylidyl diphosphinimines 13. The former rearrange to give the ylidyl triphosphanyl methanes 12. The chloromethyl diphosphinimine 13c enters a cyclization to give the 1,2,3,5 -azatriphosphole derivative 14, the structure of which has been solved by X-ray analysis. From the reaction of ylidyl bis(chlorophosphanes) 17 and 20 with the same reagents the 1,7,3,5-tetraphosphinine derivative 18 and the 1,2,3,5,6-azatetraphosphinine derivatives 19 and 21 are obtained.

AbstractChemInform is a weekly Abstracting Service, delivering concise information at a glance that was extracted from about 100 leading journals. To access a ChemInform Abstract of an article which was published elsewhere, please select a “Full Text” option. The original article is trackable via the “References” option.

Heteroatom ChemistryVolume 10, Issue 7 p. 529-537 Free to Read Molecules that we made: An essay on phosphorus chemistry Alfred Schmidpeter, Corresponding Author Alfred Schmidpeter Institut für Anorganische Chemie, Ludwig-Maximilians-Universität Müchen, Butenandstrasse 9, D-81377, MünchenInstitut für Anorganische Chemie, Ludwig-Maximilians-Universität Müchen, Butenandstrasse 9, D-81377, MünchenSearch for more papers by this author Alfred Schmidpeter, Corresponding Author Alfred Schmidpeter Institut für Anorganische Chemie, Ludwig-Maximilians-Universität Müchen, Butenandstrasse 9, D-81377, MünchenInstitut für Anorganische Chemie, Ludwig-Maximilians-Universität Müchen, Butenandstrasse 9, D-81377, MünchenSearch for more papers by this author First published: 24 November 1999 https://doi.org/10.1002/(SICI)1098-1071(1999)10:7<529::AID-HC2>3.0.CO;2-FCitations: 33AboutPDF ToolsRequest permissionExport citationAdd to favoritesTrack citation ShareShare Give accessShare full text accessShare full-text accessPlease review our Terms and Conditions of Use and check box below to share full-text version of article.I have read and accept the Wiley Online Library Terms and Conditions of UseShareable LinkUse the link below to share a full-text version of this article with your friends and colleagues. 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Diphenylnitrilimine adds to the phosphazene bond of the azaphosphole 1. A single-crystal X-ray investigation of the cycloadduct 3 shows a planar bicyclo[3.3.0]octane skeleton meridional to the trigonal bipyramidal phosphorus. The structural data are compared to those of the starting compound 1, to those of the trifluoroacetone adduct 2, and to the change from ideal tetrahedral to ideal tbp geometry.© 1999 John Wiley & Sons, Inc. Heteroatom Chem 10:243–245, 1999