Synthesis and Molecular Structure of Tris[(trimethylsilyl)silyl](diisopropylamino)(diphenylphosphino)borane
References
Table 1 Crystal data for 3.
[1] Contribution to the Chemistry of Boron, 262. For part 261:
see K. Knabel, H. Nöth. R. T. Paine, Z. Naturforsch., in print.
[2] R. T. Paine, H. Nöth, Chem. Rev. 1995, 95, 343.
[3] M. S. Lube, R. L. Wells, P. S. White, Inorg. Chem. 1996, 35,
5007.
[4] J. D. Watts, L. C. Van Zant, Chem. Phys. Lett. 1996, 251, 119.
[5] B. Riegel, H. D. Hausen, W. Schwarz, G. Heckmann, H.
Binder, E. Fluck, A. Dransfeld, P. v. Schleyer, Z. Anorg. Allg.
Chem. 1996, 622, 1472.
[6] S. Grundei, H. Nöth, R. T. Paine, Chem. Ber. 1996, 129, 1233.
[7] D. Dou, G. W. Linti, T. Q. Chen, E. N. Duesler, R. T. Paine,
H. Nöth, Inorg. Chem. 1996, 35, 3626.
[8] M. Sigl, A. Schier, H. Schmidbaur, Chem. Ber. 1997, 130, 951.
[9] M. Sigl, A. Schier, H. Schmidbaur, Chem. Ber. 1997, 130,
1411.
[10] E. Herdtweck, F. Jäkle, M. Wagner, Organometallics 1997,
16, 4737.
[11] T. L. Breen, D. W. Stephan, Organometallics 1997, 16, 365.
[12] D. A. Hoic, M. DiMare, G. C. Fu, J. Am. Chem. Soc. 1997,
119, 7155.
[13] T. Q. Chen, E. N. Duesler, R. T. Paine, H. Nöth, Inorg. Chem.
1997, 36, 1070.
[14] T. Q. Chen, E. N. Duesler, R. T. Paine, H. Nöth, Chem. Ber.
1997, 130, 933.
Chem. formula
Form. wt.
C27H51BNPSi4
543.8
0.28 x 0.35 x 0.46
monoclinic
P21/n
10.170(2)
17.327(3)
19.580(4)
96.58(3)
3427.5(11)
4
1.054
0.236
1184
Ϫ10 Յ h Յ 10
Ϫ18 Յ k Յ 18
Ϫ21 Յ l Յ 21
3 to 45
9988
4479
Cryst. size /mm
Cryst. system
Space group
˚
a /A
˚
b /A
˚
c /A
β /°
3
˚
V /A
Z
ρ(calcd.)/(Mg/m3)
µ /mmϪ1
F (000)
Index range
2θ /°
Refl. collected
Refl. unique
Refl. observed (1.5σ)
R(int.)
3214
1.92
307
No. variables
Weighting scheme
GOOF
Final R (1.5σ)
Final wR2
wϪ1 ϭ σ2(F) ϩ 0.0003F2
0.93
0.0576
0.0430
0.26/Ϫ0.25
3
˚
Larg. res. peak /(e/A )
[15] T. Q. Chen, R. T. Paine, E. N. Duesler, H. Nöth, Phosphorus
Sulfur and Silicon and the Related Elements 1997, 125, 1.
[16] T. Q. Chen, E. N. Duesler, R. T. Paine, H. Nöth, Inorg. Chem.
1997, 36, 1534.
127.24 127.61, 128.00, 128.38, 128.59, 128.68, 134.27, 134.53 ppm.
Ϫ
[17] M. Ohff, J. Holz, M. Quirmbach, A. Borner, Synthesis 1998,
1391.
[18] T. Q. Chen, E. N. Duesler, R. T. Paine, H. Nöth, Inorg. Chem.
1998, 37, 490.
11B{1H}-NMR: δ ϭ 55 ppm (h1/2 ϭ 380 Hz). Ϫ 31-P{1H}-NMR: δ ϭ
Ϫ31.7 ppm. IR /cmϪ1: ν ϭ 3050 (w), 2967 (m), 2947 (m), 2888 (m), 1582 (2),
1464 (w), 1429 (m), 1366 (w), 1319 (w), 1242 (m), 1182 (m), 1123 (w), 831
(vs), 743 (m), 696 (m), 623 (w).
[19] H. Dorn, R. A. Singh, J. A. Massey, A. J. Lough, I. Manners,
Angew. Chem. 1999, 111, 3540; Angew. Chem. Int. Ed. Engl.
1999, 38, 3321.
[20] T. Q. Chen, E. N. Duesler, R. T. Paine, H. Nöth, Inorg. Chem.
1999, 38, 4993.
X-Ray Structure
A single crystal of 3 was lodged inside a glass capillary, sealed
under N2 and mounted on the diffractometer (Siemens R3 m/V).
Determinations of the crystal class, orientation matrix and unit cell
dimensions were performed in a standard manner. Data were col-
lected at 20 °C using the ω scan mode with monochromated MoKα
[21] T. Q. Chen, J. Jackson, S. A. Jasper, E. N. Duesler, H. Nöth,
R. T. Paine, J. Organomet. Chem. 1999, 582, 25.
[22] H. Dorn, R. A. Singh, J. A. Massey, J. M. Nelson, C. A. Jaska,
A. J. Lough, I. Manners, J. Am. Chem. Soc. 2000, 122, 6669.
[23] L. Nyulaszi, Tetrahedron 2000, 56, 79.
[24] W. Keller, G. Sawitzki, W. Haubold, Inorg. Chem. 2000, 39,
1282.
[25] T. Q. Chen, E. N. Duesler, H. Nöth, R. T. Paine, J. Organome-
tal. Chem. 2000, 614, 99.
˚
radiation (λ ϭ 0.71073 A), a scintillation counter and pulse height
analyzer. Crystal data are summarized in Table 1. A small
semi-empirical absorption correction based upon psi-scans was
applied.
[26] W. Köstler, G. Linti, Eur. J. Inorg. Chem. 2001, 1841.
[27] K. Miquen, J. M. Sotiropoulos, G. Pfister-Guillouzo, A. C.
Gaumont, J. M. Denis, Organometallics 2001, 20, 143.
[28] H. Dorn, J. M. Rudezno, B. Brunnhofer, E. Rivard, J. A.
Massey, I. Manners, Macromolecules 2003, 36, 291.
[29] U. Vogel, P. Hoemensch, K. C. Schwan, A. Y. Timoshkin, M.
Scheer, Chem. Eur. J. 2003, 9, 515.
[30] K. Kubo, I. Kanemitsu, E. Murakami, T. Mizuta, H.
Nakazawa, K. Miyoshi, J. Organomet. Chem. 2004, 689, 2425.
[31] K. Knabel, T. M. Klapötke, H. Nöth, R. T. Paine, I. Schwab,
Eur. J. Inorg. Chem. 2005, 1099.
All calculations were performed on a Siemens SHELXTL PLUS
(VMS version) structure determination system [48]. Structure
solution used direct methods and full-matrix refinements were
employed [49].Neutral atom scattering factors and anomalous dis-
persion terms were used for all non-hydrogen atoms during the
refinements.The function minimized was Σw(ΗFoΗ-ΗFcΗ)2. The refine-
ment was well behaved.All non-hydrogen atoms were refined aniso-
tropically and H-atoms on the carbon atoms were included in ideal-
ized positions (riding model) with Uiso ϭ 1.25 Uequiv of the parent
carbon atom.Additional data are deposited with the Cambridge
Crystallographic Data Center as publication number CCDC-
612617 and can be obtained free of charge from CCDC, 12 Union
Road, Cambridge CB2 1EZ, UK Fax ϩ44-1223-336033; email:
[32] U. Vogel, K. C. Schwan, P. Hoemensch, M. Scheer, Eur. J.
Inorg. Chem. 2005, 1453.
[33] K. Knabel, H. Nöth, R. T. Paine, Z. Naturforsch. 2006, 61b,
265.
Z. Anorg. Allg. Chem. 2006, 2443Ϫ2446
2006 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
2445