246
M.A. Beckett et al. / Journal of Organometallic Chemistry 595 (2000) 241–247
3.3. Preparation of (PhBO)2(Ph2SiO)2·C6H11NH2 (16)
1258, 1191, 1119, 1070, 1027; 20: 1447, 1429, 1389,
1314, 1279, 1127, 1096, 1039.
At room temperature C6H11NH2 (0.082 g, 0.83
mmol) in Et2O (20 ml) solution was added to a stirred
suspension of (PhBO)2(Ph2SiO)2 (0.5 g, 0.83 mmol) in
Et2O (20 ml). The diboracyclotetrasiloxane dissolved
after a few minutes stirring and the resultant solution
was filtered. The product, a white air-stable analytically
pure solid (0.5 g, 86%), was obtained after evaporation
of the solvent and oven drying (50°C) of the residue.
3.6. X-ray structure of (p-BrC6H4BO)2(Ph2SiO)2 (8)
Crystallographic measurements were made using a
FAST area detector diffractometer and Mo–Ka radia-
tion following previously described procedures [36]. The
data were corrected for absorption (DIFABS) [37].
Crystal data: C36H28B2Br2O4Si2, formula weight=
(
762.20, triclinic, space group P1, a=8.5613(11),
1
3.4. H-NMR data (CDCl3/r.t. 250 MHz)
,
b=10.1141(6), c=10.2200(7) A, a=71.068(12), b=
3
,
81.91(2), k=86.902(9)°, U=828.71(13) A , Z=1,
u(Mo–Ka)=0.71069 A, v=25.58 cm−1, crystal size
2: 0.2 (s, 12H), 7.4 (d, 2H), 7.65 (d, 2H); 3: 0.3 (s,
12H), 3.65 (br s, 2H), 6.8 (d, 1H), 7.25 (m, 3H); 5: 0.55
(s, 6H), 7.2–7.45 (m, 10H), 7.5 (d, 2H), 7.75 (d, 2H); 6:
0.5 (s, 6H), 3.6 (br s, 2H), 6.7 (d, 1H), 7.05–7.4 (m,
11H), 7.7 (m, 2H); 8: 7.3–7.5 (m, 12H), 7.6 (d, 4H),
7.75 (m, 8H), 7.97 (d, 4H); 9: 2.6 (s, 6H), 7.15–7.5 (m,
18H), 7.6 (m, 8H), 8.05 (d, 2H); 10: 3.7 (s, 4H), 6.9 (d,
2H), 7.3 (t, 2H), 7.35 (t, 12H), 7.5 (m, 2H), 7.55 (d,
2H), 7.75 (m, 8H); 11: 7.35–7.55 (m, 12H), 7.6 (t, 2H),
7.75 (m, 8H), 8.4 (m, 4H), 8.85 (s, 2H); 12: 1.0 (t, 6H),
1.15 (m, 4H), 1.45 (m, 4H), 1.6 (q, 4H), 7.35–7.55 (m,
12H), 7.7 (m, 8H); 13: 0.4 (s, 6H), 0.9 (m, 10H), 1.3 (m,
24H), 7.45 (m, 6H), 7.9 (m, 4H); 14: 0.3 (s, 6H), 0.9 (m,
10H), 1.2 (m, 24H), 7.45 (d, 4H), 7.6 (d, 4H); 15: 0.4 (s,
6H), 0.75 (m, 10H), 1.15 (m, 24H), 7.5 (t, 2H), 8.05 (d,
2H), 8.25 (d, 2H), 8.55 (s, 2H); 16: 1.25 (m, 6H),
1.7–1.95 (m, 4H), 2.5 (br s, 2H), 2.9 (m, 1H), 7.15–7.55
(m, 18H), 7.7 (m, 8H), 8.0 (m, 4H); 17: 1.1 (t, 9H), 2.7
(q, 6H), 7.1–7.6 (m, 26H), 7.95 (m, 4H); 18: 1.35 (m,
6H), 2.05 (br s, 1H), 2.75 (t, 4H), 7.05–7.35 (m, 18H),
7.55 (m, 8H), 7.8 (m, 4H); 19: 0.8 (d, 6H), 1.6 (sept,
1H), 2.55 (d, 2H), 2.65 (br s, 2H), 7.15–7.5 (m, 18H),
7.6–7.75 (m, 8H), 8.05 (m, 4H); 20: 1.0 (br s, 1H), 2.65
(s, 6H), 2.8 (t, 4H), 3.5 (t, 4H), 7.3 (m, 18H), 7.6 (m,
8H), 7.9 (m, 2H).
,
0.35×0.30×0.25 mm, colourless prism, T=150 K,
3430 data collected [2.125q524.87°; −85h59,
−115k511, −115l511], 2276 unique with Fo\0
(Rint=0.0739). The structure was solved by direct
methods (SHELXS-86 [38]) and refined on F2 by full-ma-
trix least-squares (SHELXL-96 [39]) using all unique data
to final wR (on F2)=0.0921 (all 2276 data and 208
parameters) and R [on F, Fo\4|(Fo)]=0.0403. The
non-hydrogen atoms were refined anisotropically and
the hydrogen atoms included in calculated positions
(riding model) with Uiso set at 1.2 times the Ueq of the
parent atom.
4. Supplementary material
Crystallographic data for the structure analysis have
been deposited with the Cambridge Crystallographic
Data Centre, CCDC no. 119653. Copies of this infor-
mation may be obtained free of charge from the Direc-
tor, CCDC, 12 Union Road, Cambridge, CB2 1EZ
[fax:
+44-1223-336033
or
e-mail:
deposit
@ccdc.cam.ac.uk or http://www.ccdc.cam.ac.uk].
3.5. Selected IR data (wmax(strong)/cm−1, thin films on
NaCl plates or KBr discsa)
Acknowledgements
We thank Dr D. Apperley at the EPSRC solid state
NMR service centre (Durham University) for spectra.
We also acknowledge the EPSRC X-ray Crystallo-
graphic service at UWC.
1: 1438, 1316, 1261, 1070; 2: 1391, 1315, 1261, 1067;
3: 1439, 1340, 1310, 1260, 1066; 4: 1438, 1429, 1318,
1262, 1190, 1070; 5: 1390, 1361, 1317, 1261, 1124, 1104,
1068; 6: 1440, 1317, 1261, 1123, 1072; 7a: 1441, 1388,
1180, 1132, 1071; 8a: 1390, 1308, 1148, 1130, 1118,
1067; 9a: 1439, 1429, 1352, 1303, 1275, 1150, 1117; 10a:
1440, 1357, 1315, 1255, 1128, 1118; 11a: 1429, 1374,
1340,1300, 1268, 1153, 1129; 12: 1430, 1364, 1283, 1254,
1198, 1128, 1118; 13: 1441, 1363, 1306, 1261, 1142; 14:
1392, 1270, 1342, 1306, 1262,1139, 1012; 15: 1478, 1427,
1387, 1350, 1302, 1270, 1149; 16: 1443, 1429, 1403,
1332, 1285, 1252, 1123, 1028; 17: 1446, 1423, 1297,
1271, 1252, 1118, 1087; 18: 1429, 1283, 1234, 1184,
1149, 1120, 1064, 1028; 19: 1441, 1430, 1400, 1313,
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