[Rh(C 13 H 23 ) {(PCC 6 H 5 ) 3 } 2 ]•0,5 C 6 H 6 cristallise dans P1 avec a=12,260, b=13,05, c=15,91 A, α=71,30, β=76,24, γ=67,71 o , τ=2; affinement jusqu'a R=0,043. Les atomes du cycle a 13 chai←nons sont dans une configuration trans. Les distances des 3 atomes de ce cycle lies au metal sont de 2,120; 2,180; 2,231 A, et les angles formes par ces atomes sont de 123,9 et 125,7 o
Crystals of the title sulfur compound are orthorhombic, Cmca, with a=9.872 (1), b=9.594 (1), and c=15.488 (1) Å, V=1467.0 (4) Å3, Z=4, and Dc =1.38 g cm−2. The final refinement using 537 observed reflections for 57 variable gave R=0.025. The non-isomorphous crystals of the selenium analog are also orthorhombic, Cmca, with a=9.300 (1), b=19.724 (1), c=8.064 (1) Å, V=1479.1 (4) Å, Z=4, and Dc =2.21 g cm−2. Refinement with 48 variables using 447 observed reflections gives R=0.041. In both structures the molecules have 2/m symmetry imposed by the lattice symmetry; the S (or Se) atoms of the central 4-membered ring are located on the rotation axis, and the P, exo S (or Se), and two carbon atoms of the t-butyl group lie on the mirror plane. The central rings are not readily hydrolyzed or oxidized by exposure to air, apparently as a result of steric protection provided by the t-butyl groups.
AbstractThe title compounds (II) and (V) prepared as shown in the scheme react with excess of norbornadiene to afford the adducts (III) and (VI) in almost quantitative yield.
The preparation, spectral properties, and crystal structure of a mononuclear copper(II) complex of acetylsalicylate and pyridine are reported. The complex exists as bis(acetylsalicylato)bis(pyridine)copper(II) both in the solid state and in chloroform solution. The crystal is monoclinic, space group P21/n, with a = 17.823(5), b = 10.903(4), c = 6.598(2) Å, β = 95.74(2)°. The final refinement used 1472 observed reflections and gave an R of 0.046. The copper atom is surrounded by four atoms in a trans square planar arrangement with two short CuO distances of 1.949(3) Å and two CuN distances of 2.003(4) Å. Two longer CuO distances of 2.623(3) Å are made with the remaining oxygen atoms of the aspirin carboxylate groups.
Chemischer InformationsdienstVolume 15, Issue 6 Physical Organic Chemistry ChemInform Abstract: CRYSTAL AND MOLECULAR STRUCTURES OF C7H8(S3N)2: SUBSTITUENT EFFECTS ON THE S3N CHROMOPHORE A. W. CORDES, A. W. CORDESSearch for more papers by this authorH. KOENIG, H. KOENIGSearch for more papers by this authorM. C. NOBLE, M. C. NOBLESearch for more papers by this authorR. T. OAKLEY, R. T. OAKLEYSearch for more papers by this author A. W. CORDES, A. W. CORDESSearch for more papers by this authorH. KOENIG, H. KOENIGSearch for more papers by this authorM. C. NOBLE, M. C. NOBLESearch for more papers by this authorR. T. OAKLEY, R. T. OAKLEYSearch for more papers by this author First published: February 7, 1984 https://doi.org/10.1002/chin.198406056Read the full textAboutPDF 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 Share a linkShare onFacebookTwitterLinkedInRedditWechat No abstract is available for this article. Volume15, Issue6February 7, 1984 RelatedInformation
The reaction of tetrasulphur dinitride with norbornadiene produces the 1:1 adduct S4N2•C7H8; X-ray crystallographic analysis of this compound reveals that olefin addition cleaves one of the sulphur–sulphur bonds of S4N2, yielding a novel eight-membered C2S4N2 ring. Crystals of S4N2•C7H8 are monoclinic, space group P21/c, a = 6.127(1), b = 17.369(1), c = 9.580(1) Å, β = 106.74(1)°, V = 1003.8(5) Å3Z = 4. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to R = 0.039. The S—S—N—S—N—S fragment of the C2S4N2 ring is planar to within 0.15 Å. The S—C—C—S unit is folded out of this plane to produce a dihedral angle of 74.5°.
ADVERTISEMENT RETURN TO ISSUEPREVArticleNEXTCrystal and molecular structures of C7H8(S3N)2: substituent effects on the S3N chromophoreA. W. Cordes, H. Koenig, M. C. Noble, and R. T. OakleyCite this: Inorg. Chem. 1983, 22, 23, 3375–3378Publication Date (Print):November 1, 1983Publication History Published online1 May 2002Published inissue 1 November 1983https://pubs.acs.org/doi/10.1021/ic00165a004https://doi.org/10.1021/ic00165a004research-articleACS PublicationsRequest reuse permissionsArticle Views21Altmetric-Citations7LEARN ABOUT THESE METRICSArticle Views are the COUNTER-compliant sum of full text article downloads since November 2008 (both PDF and HTML) across all institutions and individuals. These metrics are regularly updated to reflect usage leading up to the last few days.Citations are the number of other articles citing this article, calculated by Crossref and updated daily. Find more information about Crossref citation counts.The Altmetric Attention Score is a quantitative measure of the attention that a research article has received online. Clicking on the donut icon will load a page at altmetric.com with additional details about the score and the social media presence for the given article. Find more information on the Altmetric Attention Score and how the score is calculated. Share Add toView InAdd Full Text with ReferenceAdd Description ExportRISCitationCitation and abstractCitation and referencesMore Options Share onFacebookTwitterWechatLinked InRedditEmail Other access optionsGet e-AlertscloseSupporting Info (1)»Supporting Information Supporting Information Get e-Alerts
The reaction of norbornadiene with (triphenylphosphoranediyl)aminocyclotrithiatriazene produces the cycloadduct Ph3PN—S3N3•C7H8. The crystal and molecular structure of this compound has been determined by X-ray crystallography. Crystals of Ph3PN—S3N3•C7H8 are monoclinic, space group P21/c, a = 9.757(1), b = 15.114(1), c = 16.535(2) Å, β = 100.73(1)°, V = 2395.7(9) Å3, and Z = 4. The structure was solved by direct methods and refined by Fourier and full-matrix least-squares procedures to give a final R of 0.040 and Rw of 0.058 for 2620 observed reflections. The structure reveals that the S3N3 ring adds to norbornadiene in an exo fashion via two sulphur atoms. The S3N3 ring adopts a chair conformation with the three ligands occupying axial positions on the same side of the ring. The relative rates of this and other cycloadditions involving SN substrates and olefins are discussed in terms of the energies of the interacting frontier orbitals. The results suggest that HOMO(olefin)–LUMO(SN substrate) interactions control the kinetics of these reactions.
The reaction of tetrasulfur tetranitride with tetrafluoroboric acid diethyl etherate in methylene chloride solution produces S4N4H+BF4-, the first simple salt of S4N4. the crystal and molecular structure of S4N4H+BF4has been determined by X-ray crystallo raphy. Crystals of the compound are monoclinic, space group P2,/n, a = 6.563 (2) A, b = 11.717 (2) A, c = 11.409 (2) 8, B = 101.63 (2)O, V = 859.3 (6) AS, and 2 = 4. The structure was solved by direct methods and refined by Fourier and full-matrix least-squares procedures to give a final R of 0.042 for 1428 observed reflections. The structure of the S4N4H+ cation consists of a boat-shaped 8-membered ring with approximately coplanar (to within 0.02 A) sulfur atoms. The reasons for the structural rearrangement which the protonation of S4N4 induces are discussed in the light of MNDO molecular orbital calculations on a number of idealized conformations of S4N4H+ unit. In spite of the lack of evidence usually regarded as diagnostic of aromatic behavior, e.g., heats of formation andZ diamagnetic ring currents? the descriptions of the electronic structures of cyclic binary sulfur nitride derivatives often allude to their aromatic character. The empirical rules devised by Banister4 and the symmetry-based molecular orbital arguments of Gleiter5 and of Gimarc and TrinajstiE6 emphasize the preponderance of cyclic .rr systems containing 4n + 2 electrons. However, the need for such a complement vanishes in molecules possessing less than 3-fold ~ y m m e t r y . ~ Recently several cyclic molecules containing 4n T electrons have been reported.*,9 The observed structure of tetrasulfur tetranitride (1) has long
ADVERTISEMENT RETURN TO ISSUEPREVArticleNEXTPreparation and crystal and molecular structure of tetrasulfur tetranitride-tetrafluoroboric acid salt (S4N4H+BF4-). Molecular orbital study of the protonation of tetrasulfur tetranitrideA. W. Cordes, C. G. Marcellus, M. C. Noble, R. T. Oakley, and W. T. PenningtonCite this: J. Am. Chem. Soc. 1983, 105, 19, 6008–6012Publication Date (Print):September 1, 1983Publication History Published online1 May 2002Published inissue 1 September 1983https://pubs.acs.org/doi/10.1021/ja00357a008https://doi.org/10.1021/ja00357a008research-articleACS PublicationsRequest reuse permissionsArticle Views112Altmetric-Citations19LEARN ABOUT THESE METRICSArticle Views are the COUNTER-compliant sum of full text article downloads since November 2008 (both PDF and HTML) across all institutions and individuals. These metrics are regularly updated to reflect usage leading up to the last few days.Citations are the number of other articles citing this article, calculated by Crossref and updated daily. Find more information about Crossref citation counts.The Altmetric Attention Score is a quantitative measure of the attention that a research article has received online. Clicking on the donut icon will load a page at altmetric.com with additional details about the score and the social media presence for the given article. Find more information on the Altmetric Attention Score and how the score is calculated. Share Add toView InAdd Full Text with ReferenceAdd Description ExportRISCitationCitation and abstractCitation and referencesMore Options Share onFacebookTwitterWechatLinked InRedditEmail Other access optionsGet e-AlertscloseSupporting Info (1)»Supporting Information Supporting Information Get e-Alerts
AbstractDie gemäß dem Schema als erstes einfaches Salz des S4N4 dargestellte Titelverbindung (III) kristallisiert in der Raumgruppe P21/n mit Z=4.
ADVERTISEMENT RETURN TO ISSUEPREVArticleNEXTPreparation and molecular and electronic structures of cyclo-1.lambda.5-phospha-3,5-dithia-2,4,6-triazenes and their norbornadiene adductsN. Burford, T. Chivers, A. W. Cordes, W. G. Laidlaw, M. C. Noble, R. T. Oakley, and P. N. SwepstonCite this: J. Am. Chem. Soc. 1982, 104, 5, 1282–1290Publication Date (Print):March 1, 1982Publication History Published online1 May 2002Published inissue 1 March 1982https://pubs.acs.org/doi/10.1021/ja00369a023https://doi.org/10.1021/ja00369a023research-articleACS PublicationsRequest reuse permissionsArticle Views93Altmetric-Citations39LEARN ABOUT THESE METRICSArticle Views are the COUNTER-compliant sum of full text article downloads since November 2008 (both PDF and HTML) across all institutions and individuals. These metrics are regularly updated to reflect usage leading up to the last few days.Citations are the number of other articles citing this article, calculated by Crossref and updated daily. Find more information about Crossref citation counts.The Altmetric Attention Score is a quantitative measure of the attention that a research article has received online. Clicking on the donut icon will load a page at altmetric.com with additional details about the score and the social media presence for the given article. Find more information on the Altmetric Attention Score and how the score is calculated. Share Add toView InAdd Full Text with ReferenceAdd Description ExportRISCitationCitation and abstractCitation and referencesMore Options Share onFacebookTwitterWechatLinked InRedditEmail Other access optionsGet e-AlertscloseSupporting Info (1)»Supporting Information Supporting Information Get e-Alerts
AbstractDie Reaktion der Diphosphine (I) oder des Phosphits (II) mit Tetraschwefeltetranitrid ergibt die cyclischen Titelverbindungen (III), deren Charakterisierung durch ′5 N‐ und "P ‐′ H ‐NMR‐ sowie IR‐ spektroskopische Daten erfolgt.