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1642427476
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note
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In the sublimation vessel, both valentine and senarmontite formed. Diffraction data on valentine (Pccn) was also collected in the same manner as described for senarmontite, but the crystal shape was anomalous and the analytical absorption correction did not model the effect well. Hence multipole refinements reconstructed the electrond density distribution poorly. The revelant structural parameters obtained from a spherical atom refinement are: a = 4.8996(3) Å, b = 12.4490(7) Å, c = 5.4103(3) Å, α = β = γ = 90°. Sb (0.04064, 0.12753, 0.17784), O(1) (1/4, 1/4, 0.0209), O(2) (0.1509, 0.0587, -0.1454). Full crystallographic details are included in the CIF file.
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10
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1642550270
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Bruker, Madison, WI
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teXsan for Windows: Single crystal structure analysis software, Molecular Structure Corporation, The Woodlands, TX, 1997-1998.
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1642427477
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Xtal3.6 System
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1642509361
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note
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32- were refined unconstrained.
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25
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0000914758
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P. J. Becker and P. Coppens, Acta Crystallogr., Sect. A, 1974, 30, 129.
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0003867643
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1642427478
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Towler, M.D.1
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30
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1642468590
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note
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In comparison, Mulliken charges obtained from the CRYSTAL98 calculations are somewhat greater: for senarmontite, +1.76 on Sb, and -1.17 on O, and for valentine, +1.77 on Sb, -1.23 on O(1) and -1.15 on O(2).
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36
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0007720163
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B. Beagly, D. W. J. Cruickshank, T. G. Hewitt and K. H. Jost, Trans. Faraday Soc., 1969, 65, 1219
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0003081431
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F. C. Hill, G. V. Gibbs and M. B. Boisen, Phys. Chem. Mineral., 1997, 24, 582
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G. V. Gibbs, M. B. Boisen, F. C. Hill, O. Tamada and R. T. Downs, Phys. Chem. Mineral., 1998, 25, 574.
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48
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0003422019
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Wavefunction Inc., 18401 Von Karman Ave., Irvine CA 92715, USA. The DN* basis set is slightly larger than the common 6-31G* basis set
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SPARTAN version 5.0, Wavefunction Inc., 18401 Von Karman Ave., Irvine CA 92715, USA. The DN* basis set is slightly larger than the common 6-31G* basis set.
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SPARTAN Version 5.0
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49
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1642468592
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note
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We note that in this study, and most likely other studieds involving heavy atoms, proper treatment of absorption is vital, and in some cases it may be a greater problem than extinction. For senarmontite, if the most heavily extinction-affected reflections were removed from the refinement very little changed, but small optimisations made to the crystal dimensions, subsequently used in the absorption correction, substantially altered the deformation density and derived properties.
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