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    Acta Chemica Scandinavica

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    Acta Chemica Scandinavica

    Copyright:

    © All Rights Reserved
    Download as PDF or read online from Scribd
    Flag for inappropriate content
    6 views9 pages

    Acta Vol 53 p0015-0023

    Uploaded by

    Igor Vasiljevic
    Acta Chemica Scandinavica

    Copyright:

    © All Rights Reserved
    Download as PDF or read online from Scribd
    Flag for inappropriate content
    of 9
    Smale tare md a iin © Ate Chemis Semin 188 ACR EMICA SCANDINAVICA Crystal Structure and Spectroscopic Characterization of a Green V'Y Compound, Nag(VO)2(SO4)¢ Kurt Nielsen,* Soghomon Boghosian,® Rasmus Fehrmann’ and Rolf Willestofte Berg”* “Department of Chemistry, Technical University of Denmark, DK-2800 Lyngby, Denmark and YInstitute of Chemical Engineering and High Temperature Chemical Processes, (ICE/HT-FORTH) and Department of Chemical Engineering, University of Patras, Gr-26500 Patras, Greece Nielsen, K., Boghosian, S., Fehrmann, R. and Berg, R. W.,, 1999. Crystal Structure and Specicoscopic Characterization of a Green. V" Compound, Nas(VO)s(SO,je. Acta Chem, Seand, 33° 15-23. © Acta Chemie Scandinavica 1999, [A mixture of green crystals was precipitated at 467°C from around 1.5 mL of a melt, consisting of Na,S,0, and VO, in the molar ratio Na/V=4. The melt tras in contact with a 10/2 SO, 90% N, mixed gas atmosphere, A minor amount Of the product consisted of the green V! compound NaV(SO,)., previously fnvestigated, The majority consisted of another kind of erystal, whose X-tay structure is reported here. The obtained formula was Na,('VO)s(SOq)q, crystal {ng in the monoclinic space group P2,/c, with a=8,6454(2), b= 16:0027(4), c= 15:5074(4) A and B=90.017(1)" at 22°C and Z=4. Surprisingly the erystals sere not blue as would be expected from the +4 oxidation state ofthe vanadium. “The structure consists of two kinds of octahedrally coordinated vanadium atoms, ach closely bound to an O*~ (forming the vanadyl group VO") and five sulfato [roups, the one trans to oxide ata longer distance. A complicated 3. cannot be identified in the spectra, X-Ray single crystal investigation The crystal symmetry and space group were determined from Weissenberg photographs. Crystal data and other experimental results are given in Table I. Intensity data were collected at room temperature on a. Siemens SMART diffractometer with graphite monochromated Mo Ka radiation (0.71073 A). The unit-cell dimensions were determined by least-squares refinements based on the complete data set. The intensities were corrected for Lorentz and polarization effects, but not for absorption. ‘The structure was solved and refined in the space group P2/c. The calculations were done using Sheldrick’s programs," and included full-matrix least-squares F? refinements of positional and anisotropic thermal para- meters, Anomalous dispersion corrections and atomic scattering factors given in Ref. 14 were used. Three of the 5494 reflections having very negative F? were omitted from the refinement. The crystal was twinned with coin- ciding (hk) and (hk —1) reflections; the twin scale factor for the second component was 0.566(1). Atomic coordinates, equivalent isotropic thermal parameters, ‘bond lengths and bond angles are listed in Tables 2 and 3. R-and R,-values are given in Table I. An approximate (isotropic) ireatment of cell esd. is used for estimating esd. involving least-square planes. A list of observed and calculated structure factors as well as anisotropic thermal parameters (U;,) is obtainable from the authors. Visualisations of the structure are shown in Figs. | and 2 Description and discussion of the structure. The asymmet- ric unit contains eight sodium ions, two vanadium(IV) 16 Table 1. Crystal data for NagIVOIsISO4} Formula NaglVOl,{S0e)y ‘Maig mol” 894.16 Crystal systern Monoclinic Space group P2,/¢(No. 14) oA 8.685412) bia v6.002714) A 1550744) r 90.01711) via 215.06 D.igem-? 2.768 TK 29312), Zand F100) and 1752 Mo Kem 1748 Extinction expression = kF,{14+-0.001F229)sin(20))-™ refined Extinction parameter 0.002012 Total no. of reflections 14783 (5494 independent) Fey=0.088 Min, max in 20)" 2.54, 59.33 ‘Min, max in hk fh: 9, 12; ks ~22, 18; 1: ~20, 21 Reflections with />2oil) 4450 No. of parameters 281 Crystal size/mm 0.15008 0.03 Weight function wr '=s8(F2)+(0.0071PF + 7.3562, with P= tf? 26.21/3 10.0732 for al reflections: 0.0479 for reflections with F,>2af,) 0.0854 for ail reflections: (0.0810 for refections with Fe> 2a 41.189 for al rections: 1.134 for reflections with F,>2otfe) 078

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