Preparation, X-ray structure, and spectroscopic characterization of 1,5-Se2S2N4

被引:20
|
作者
Maaninen, A
Laitinen, RS
Chivers, T
Pakkanen, TA
机构
[1] Univ Oulu, Dept Chem, FIN-90570 Oulu, Finland
[2] Univ Calgary, Dept Chem, Calgary, AB T2N 1N4, Canada
[3] Univ Joensuu, Dept Chem, FIN-80101 Joensuu, Finland
关键词
D O I
10.1021/ic990179i
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
The reaction of [(Me3Si)(2)N](2)S with equimolar amounts of SCl2 and SO2Cl2 produces S4N4 in a good yield. The new chalcogen nitride 1,5-Se2S2N4 has been prepared in high yield by two different reactions: (a) from [(Me3Si)(2)N](2)S and SeCl4 and (b) from [(Me3Si)(2)N](2)Se with equimolar amounts of SCl2 and SO2Cl2. 1,5-Se2S2N4 has a cage structure similar to those of S4N4 and Se4N4. The crystal structure is disordered with site occupation factors ca. 50% for selenium in each chalcogen atom position. The 12 eV EI mass spectrum shows Se2SN2+ as the fragment with highest mass. Both the N-14 and Se-77 NMR spectra show a single resonance (-238 and 1418 ppm, respectively). These data rule out the possibility that the crystalline sample is a solid solution of S4N4 and Se4N4 and imply the presence of 1,5-Se2S2N4. This deduction was further verified by Raman spectroscopy and vibrational analysis.
引用
收藏
页码:3450 / 3454
页数:5
相关论文
共 50 条
  • [41] PREPARATION, SPECTROSCOPIC CHARACTERIZATION AND X-RAY STRUCTURE OF [DICYCLOHEXYLPHOSPHINYL-N-METHYL(THIOFORMAMIDE)]GOLD(I) CHLORIDE - AU[CY(2)P(O)C(S)N(H)ME]CL
    SIASIOS, G
    TIEKINK, ERT
    AUSTRALIAN JOURNAL OF CHEMISTRY, 1995, 48 (04) : 757 - 762
  • [42] High pressure X-ray diffraction study of CdAl2Se4 and Raman study of AAl2Se4 (A = Hg, Zn) and CdAl2X4 (X = Se, S)
    Meenakshi, S.
    Vijyakumar, V.
    Godwal, B. K.
    Eifler, A.
    Orgzall, I.
    Tkachev, S.
    Hochheimer, H. D.
    JOURNAL OF PHYSICS AND CHEMISTRY OF SOLIDS, 2006, 67 (08) : 1660 - 1667
  • [43] X-RAY INVESTIGATION OF SOLID-SOLUTION CD1-XCUXCR2SE4 WITH SPINEL STRUCTURE
    ELISEEV, AA
    AMINOV, TG
    SHABUNINA, GG
    RUSANOVA, TA
    INORGANIC MATERIALS, 1978, 14 (04) : 507 - 511
  • [44] X-ray spectroscopic study of the electronic structure of CuCrO2
    Arnold, T.
    Payne, D. J.
    Bourlange, A.
    Hu, J. P.
    Egdell, R. G.
    Piper, L. F. J.
    Colakerol, L.
    De Masi, A.
    Glans, P. -A.
    Learmonth, T.
    Smith, K. E.
    Guo, J.
    Scanlon, D. O.
    Walsh, A.
    Morgan, B. J.
    Watson, G. W.
    PHYSICAL REVIEW B, 2009, 79 (07)
  • [45] The preparation and X-ray structure of [M{(SePPh2)(2)N}(2)], M=Ni, Pd, Pt
    Papadimitriou, C
    Veltsistas, P
    Novosad, J
    CeaOlivares, R
    Toscano, A
    Garcia, PGY
    LopezCardosa, M
    Slawin, AMZ
    Woollins, JD
    POLYHEDRON, 1997, 16 (16) : 2727 - 2729
  • [46] FORMATION, X-RAY STRUCTURE, AND DEPROTONATION OF AN S,S'-METHYLENE-BRIDGED P2N4S2 RING
    CHIVERS, T
    COWIE, M
    EDWARDS, M
    HILTS, RW
    INORGANIC CHEMISTRY, 1992, 31 (16) : 3349 - 3350
  • [47] Electronic structure and X-ray spectroscopic properties of YbNi2P2
    Shcherba, I. D.
    Bekenov, L. V.
    Antonov, V. N.
    Noga, H.
    Uskokovic, D.
    Zhak, O.
    Kovalska, M. V.
    JOURNAL OF ELECTRON SPECTROSCOPY AND RELATED PHENOMENA, 2016, 212 : 5 - 10
  • [48] Preparation and characterization of bis[4-dimethylamino-2-pyrimidyl] dichalcogenides (S, Se, Te): X-ray crystal structure of bis[4-dimethylamino-2-pyrimidyl] diselenide and its physicochemical behavior in microemulsion media
    Bhasin, K. K.
    Arora, Ekta
    Kaur, Khushwinder
    Kang, Sung-Kyu
    Gobel, Michael
    Klapoetke, T. M.
    Mehta, S. K.
    TETRAHEDRON, 2009, 65 (01) : 247 - 252
  • [49] Electrochemical and Chemical Reduction of Disulfur Dinitride: Formation of [S4N4]-•, EPR Spectroscopic Characterization of the [S2N2H]• Radical, and X-ray Structure of [Na(15-crown-5)][S3N3]
    Roemmele, Tracey L.
    Konu, Jari
    Boere, Rene T.
    Chivers, Tristram
    INORGANIC CHEMISTRY, 2009, 48 (19) : 9454 - 9462
  • [50] μ-1,2,4,5-tetrazine-N1:N4-bis(pentaammineruthenium) tetracation:: Synthesis and X-ray structure
    Tampucci, Silvia
    Ferrari, Marisa Belicchi
    Calucci, Lucia
    Pelosi, Giorgio
    Denti, Gianfranco
    INORGANICA CHIMICA ACTA, 2007, 360 (08) : 2814 - 2818