L. Dosta´l et al. / Journal of Organometallic Chemistry 692 (2007) 2350–2353
2353
OCH2), 7.20 (2H, d, Ar–H3,5), 7.30 (1H, t, Ar–H4). 13C
3. Supplementary material
NMR (125.76 MHz, CDCl3): 58.60 (s, CH3O), 75.33 (s,
OCH2), 125.30 (s, Ar–C3,5), 129.70 (s, Ar–C4), 145.86 (s,
Ar–C2,6), 151.36 (s, Ar–C1). Data found for 3 (analysis
of collected single crystals): Mp >140 ꢁC decomposition.
Anal. Calc. for C40H52Cl11O8Sb5 (1659.5): C, 28.95; H,
3.16; Found: C, 29.49; H, 3.36%. ESI mass spectra: m/z
451 [L2Sb]+, 100%. Negative-ions ESI mass spectra: m/z
433 [Cl2SbOSbCl3]ꢀ; m/z 261 [SbCl4]ꢀ 100%; m/z 207
[OSbCl2]ꢀ. 1H NMR (500 MHz, CDCl3): 3.28 (6H, s,
CH3O), 4.57 (4H, s, OCH2), 7.20–7.37 (m, Ar–H). 13C
NMR (125.76 MHz, CDCl3): 58.50 (s, CH3O), 76.13
(s, OCH2), 128.09 (s, Ar–C3,5), 129.38 (s, Ar–C4), 144.80
(s, Ar–C2,6), 146.98 (s, Ar–C1).
CCDC 624442 contains the supplementary crystallo-
graphic data for 3. These data can be obtained free of
html, or from the Cambridge Crystallographic Data
Centre, 12 Union Road, Cambridge CB2 1EZ, UK; fax:
(+44) 1223-336-033; or e-mail: deposit@ccdc.cam.ac.uk.
Acknowledgements
The authors thank the Ministry of Education of the
Czech Republic (Projects MSM0021627501, MSM00-
21627502 and LC523) and the Grant Agency of the Czech
Republic Grant – 203/07/P094 for financial support. The
authors would like to thank reviewer 1 for stimulating sug-
gestions as well.
2.2. X-ray structure determination
C40H52Cl11O8Sb5, M = 1659.52, monoclinic, C2/c, a =
˚
˚
˚
36.3170(3) A, b = 13.8660(1) A, c = 28.3610(3) A, b =
3
˚
References
127.8521(5)ꢁ, V = 11276.86(17) A , Z = 8, Dx = 1.955
Mg mꢀ3. A colourless crystal of dimensions 0.3 · 0.15 ·
´
´
ˇ
´
˚
ˇ
´
ˇ
[1] L. Dostal, I. Cısarova, R. Jambor, A. Ruzˇicka, R. Jirasko, J. Holecek,
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˚
ter by monochromatized Mo Ka radiation (k = 0.71073 A)
at 150(2) K. The analytical correction on absorption was
applied (l = 2.931 mmꢀ1), Tmin = 0.499, Tmax = 0.726; a
total of 102435 diffractions were measured in the range
h = ꢀ 37 to 47, k = ꢀ 17 to 18, l = ꢀ 36 to 36 (hmax
=
27.49ꢁ), from which 12926 were unique (Rint = 0.0498) and
10529 observed according to the I > 2r(I) criterion. Cell
parameters from 75629 reflections (h = 1–27.49ꢁ). The
structure was solved by direct methods (SIR92, Altomare,
1994) and refined by full-matrix least squares based on F2
(SHELXL 97). The hydrogen atoms were fixed into idealised
positions (riding model) and assigned temperature factors
either Hiso (H) = 1.2 Ueq (pivot atom) or Hiso(H) = 1.5 Ueq
(pivot atom) for methyl moiety. The final difference map dis-
played no peaks of chemical significance as the highest max-
ima are in close vicinity of antimony (Dqmax = 2.426, Dqmin
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664;
C
56 (2000)
(b) M. Bujak, J. Zaleski, J. Chem. Cryst. 29 (1999) 555.
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ꢀ2.050 e Aꢀ3).
˚
2.3. X-ray powder diffraction
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Sci. 49 (1994) 471.
[8] Joint Committee on Powder Diffraction Standards, International
Centre of Diffraction Data, Swarthmore, PA.
[9] The decomposition of 3 to 2 was performed under argon atmosphere to
avoid the hydrolysis of incipient SbCl3 for several times, unfortunately
in all cases the observed insoluble material was of amorphous nature
thus unsuitable for X-ray powder diffraction method.
Powder X-ray diffraction data were obtained with a D8-
Advance diffractometer (Bruker AXE, Germany) using Cu
Ka radiation with a secondary graphite monochromator.
Diffraction angles were measured from 10ꢁ to 65ꢁ (2H) in
0.02ꢁ steps with a counting time of 10 s per step.