N. W. Mitzel · Synthesis and Structures of Simple (Silylmethyl)(methyl)ethers
763
◦
◦
◦
−
96 and −196 C. The product was contained in the −96 C 2θmax. = 54 , ω-scan, 4028 scattering intensities collected
trap (5.7 g, 69% yield), while some SiF was received in the of which all were unique, 390 parameters, R = 0.0346 for
4
1
◦
1
96 C trap.
3170 reflections with Fo > 4σ(Fo) and wR = 0.0979 for all
2
1
◦
H NMR (400.05 MHz, C D , 21 C): δ = 2.95 (s, 4028 data. Crystal data F3SiCH2OCH3, C2H5OF3Si, Mr =
broad), 2.99 (s, broad). – C NMR (100.64 MHz, C D , 130.15, crystal system orthorhombic, space group Pna21,
6
6
13
6
6
◦
1
1
˚
2
1
C): δ = 55.31 (t, broad, JCH = 137 Hz), 62.44 Z = 4, a = 14.755(6), b = 7.461(4), c = 4.778(3) A, V =
qt, JCH = 141.7 Hz, 3JSiH = 3.3 Hz, CH ). –
17
O
˚ 3
−1 ◦
(
526.0(5) A at 123(2) K, µ = 0.398 mm . 2θmax. = 54 ,
3
◦
19
NMR (54.26 MHz, C D , 21 C): δ = −53. – F NMR ω-scan, 2818 scattering intensities collected of which 782
6
6
◦
376.54 MHz, C D , 21 C): δ = 65.26. – Si NMR were unique, 84 parameters, R1 = 0.0388 for 760 reflections
6 6
29
(
(
2
1
9
◦
1
1
79.38 MHz, C D , 21 C): δ = −69.4 (q, broad, J
=
with Fo > 4σ(Fo) and wR2 = 0.0979 for all 782 data.
6
6
SiF
−
82 Hz). – IR (ν, cm ) 2976 s, 2950 m, 2876 s, 2791 w,
Structure solutions and refinements were undertaken with
476 w, 1447 w, 1391 w, 1362 w, 1142 ss, 1080 w, 1030 m, the program SHELXTL 5.01 [17]. Crystallographic data (ex-
45 w, 808 ss.
cluding structure factors) have been deposited with the Cam-
Crystal structure determination of H SiCH OCH and bridge Crystallographic Data Centre as supplementary pub-
3
2
3
F SiCH OCH . Single crystals of H SiCH OCH and lication no. CCDC-204076 (H3SiCH2OCH3) and CCDC-
3
2
3
3
2
3
F SiCH OCH were grown in situ on the diffractometer by 204075 (F3SiCH2OCH3). Copies of the data can be obtained
3
2
3
slowly cooling the melt in a sealed capillary below the melt- free of charge on application to CCDC, 12 Union Road,
ing point after generating a suitable seed crystal. Data col- Cambridge CB2 1EZ, UK (e-mail: deposit@ccdc.cam.ac.uk.
lection was undertaken with a Nonius Turbo-CAD4 diffrac-
tometer.
Acknowledgements
Crystal data H SiCH OCH , C H OSi, Mr = 76.17, crys-
tal system triclinic, space group P1, Z = 8, a = 4.524(1),
3
2
3
2 8
This work was supported by Deutsche Forschungs-
gemeinschaft and Fonds der Chemischen Industrie. Ms.
Daniela Arnold is thanked for part of the preparative work.
˚
˚ 3
b = 7.339(1), c = 29.207(5) A, α = 89.98(1), β = 90.02(2),
◦
−1
.
γ =89.93(2) , V = 969.7(3) A at 123(2) K, µ = 0.306 mm
[
[
[
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