Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802010875/cf6185sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536802010875/cf6185Isup2.hkl |
CCDC reference: 189910
Data collection: COLLECT (Nonius, 1998); cell refinement: HKL SCALEPACK (Otwinowski & Minor, 1997); data reduction: HKL DENZO and SCALEPACK; program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP (Sheldrick, 1993); software used to prepare material for publication: SHELXL97.
C5H10Si | Dx = 0.912 Mg m−3 |
Mr = 98.22 | Melting point: 265 K |
Monoclinic, P21 | Mo Kα radiation, λ = 0.7107 Å |
a = 10.868 (2) Å | Cell parameters from 16948 reflections |
b = 5.742 (1) Å | θ = 1.0–27.5° |
c = 17.190 (2) Å | µ = 0.21 mm−1 |
β = 91.31 (1)° | T = 150 K |
V = 1072.4 (3) Å3 | Cylinder, colourless |
Z = 6 | 0.15 mm (radius) |
F(000) = 324 |
Nonius KappaCCD diffractometer | 2955 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.069 |
Graphite monochromator | θmax = 27.5°, θmin = 3.6° |
Thin–slice ω and φ scans | h = −13→9 |
5343 measured reflections | k = −5→7 |
3566 independent reflections | l = −21→22 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.096 | H-atom parameters constrained |
wR(F2) = 0.273 | w = 1/[σ2(Fo2) + (0.1617P)2 + 1.4254P] where P = (Fo2 + 2Fc2)/3 |
S = 1.04 | (Δ/σ)max < 0.001 |
3566 reflections | Δρmax = 1.53 e Å−3 |
177 parameters | Δρmin = −0.52 e Å−3 |
25 restraints | Absolute structure: Flack (1983), 860 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.1 (4) |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
Si1A | 0.77397 (12) | 0.2544 (3) | 0.59596 (8) | 0.0386 (4) | |
C1A | 0.6713 (6) | 0.0708 (11) | 0.6558 (4) | 0.0554 (16) | |
H1AA | 0.7212 | −0.0207 | 0.6929 | 0.106 (7)* | |
H1AB | 0.6239 | −0.0346 | 0.6218 | 0.106 (7)* | |
H1AC | 0.6149 | 0.1709 | 0.6843 | 0.106 (7)* | |
C2A | 0.8694 (6) | 0.0753 (12) | 0.5309 (4) | 0.0584 (17) | |
H2AA | 0.9033 | −0.0577 | 0.5599 | 0.106 (7)* | |
H2AB | 0.9369 | 0.1702 | 0.5112 | 0.106 (7)* | |
H2AC | 0.8184 | 0.0188 | 0.4870 | 0.106 (7)* | |
C3A | 0.8712 (7) | 0.4445 (13) | 0.6599 (4) | 0.072 (2) | |
H3AA | 0.9167 | 0.3483 | 0.6978 | 0.106 (7)* | |
H3AB | 0.8186 | 0.5543 | 0.6875 | 0.106 (7)* | |
H3AC | 0.9294 | 0.5311 | 0.6282 | 0.106 (7)* | |
C4A | 0.6767 (5) | 0.4434 (10) | 0.5356 (3) | 0.0428 (13) | |
C5A | 0.6078 (6) | 0.5668 (11) | 0.4989 (4) | 0.0495 (15) | |
H5A | 0.5532 | 0.6646 | 0.4698 | 0.085 (15)* | |
Si1B | 0.27337 (12) | −0.2583 (3) | 0.73718 (8) | 0.0388 (4) | |
C1B | 0.1643 (6) | −0.0761 (12) | 0.6804 (4) | 0.0560 (16) | |
H1BA | 0.2091 | 0.0121 | 0.6413 | 0.106 (7)* | |
H1BB | 0.1231 | 0.0323 | 0.7154 | 0.106 (7)* | |
H1BC | 0.1028 | −0.1758 | 0.6545 | 0.106 (7)* | |
C2B | 0.3760 (6) | −0.0761 (13) | 0.7980 (4) | 0.0606 (18) | |
H2BA | 0.4414 | −0.0122 | 0.7660 | 0.106 (7)* | |
H2BB | 0.4125 | −0.1707 | 0.8400 | 0.106 (7)* | |
H2BC | 0.3287 | 0.0519 | 0.8203 | 0.106 (7)* | |
C3B | 0.3628 (7) | −0.4493 (13) | 0.6718 (4) | 0.072 (2) | |
H3BA | 0.4060 | −0.3532 | 0.6341 | 0.106 (7)* | |
H3BB | 0.3066 | −0.5559 | 0.6442 | 0.106 (7)* | |
H3BC | 0.4228 | −0.5393 | 0.7028 | 0.106 (7)* | |
C4B | 0.1828 (5) | −0.4429 (10) | 0.8016 (3) | 0.0420 (13) | |
C5B | 0.1204 (6) | −0.5687 (12) | 0.8398 (4) | 0.0606 (17) | |
H5B | 0.0709 | −0.6686 | 0.8700 | 0.085 (15)* | |
Si1C | 0.73769 (14) | 0.2579 (3) | 0.92845 (8) | 0.0456 (4) | |
C1C | 0.6347 (7) | 0.0704 (13) | 0.9848 (4) | 0.0638 (19) | |
H1CA | 0.5789 | 0.1678 | 1.0148 | 0.106 (7)* | |
H1CB | 0.6839 | −0.0275 | 1.0203 | 0.106 (7)* | |
H1CC | 0.5865 | −0.0288 | 0.9491 | 0.106 (7)* | |
C2C | 0.8319 (7) | 0.4425 (13) | 0.9946 (4) | 0.0652 (19) | |
H2CA | 0.7780 | 0.5276 | 1.0296 | 0.106 (7)* | |
H2CB | 0.8792 | 0.5536 | 0.9641 | 0.106 (7)* | |
H2CC | 0.8885 | 0.3442 | 1.0254 | 0.106 (7)* | |
C3C | 0.6474 (7) | 0.4375 (14) | 0.8580 (4) | 0.067 (2) | |
H3CA | 0.5876 | 0.5317 | 0.8860 | 0.106 (7)* | |
H3CB | 0.6038 | 0.3355 | 0.8209 | 0.106 (7)* | |
H3CC | 0.7030 | 0.5402 | 0.8299 | 0.106 (7)* | |
C4C | 0.8390 (6) | 0.0638 (11) | 0.8740 (4) | 0.0522 (16) | |
C5C | 0.9011 (7) | −0.0681 (13) | 0.8393 (4) | 0.0643 (19) | |
H5C | 0.9508 | −0.1738 | 0.8114 | 0.085 (15)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Si1A | 0.0366 (8) | 0.0334 (8) | 0.0456 (7) | −0.0001 (12) | −0.0055 (5) | 0.0035 (9) |
C1A | 0.064 (4) | 0.047 (4) | 0.056 (3) | −0.004 (3) | 0.009 (3) | 0.001 (3) |
C2A | 0.046 (4) | 0.051 (4) | 0.078 (4) | 0.008 (3) | 0.010 (3) | 0.012 (4) |
C3A | 0.076 (5) | 0.054 (4) | 0.085 (5) | −0.012 (4) | −0.035 (4) | 0.012 (4) |
C4A | 0.033 (3) | 0.043 (3) | 0.052 (3) | −0.006 (3) | −0.003 (2) | −0.008 (3) |
C5A | 0.044 (3) | 0.039 (3) | 0.064 (3) | 0.006 (3) | −0.016 (3) | 0.003 (3) |
Si1B | 0.0314 (7) | 0.0350 (9) | 0.0500 (7) | −0.0001 (11) | 0.0011 (5) | 0.0012 (9) |
C1B | 0.051 (4) | 0.059 (4) | 0.058 (4) | −0.002 (3) | −0.012 (3) | 0.003 (3) |
C2B | 0.052 (4) | 0.060 (4) | 0.070 (4) | −0.007 (4) | −0.006 (3) | 0.004 (4) |
C3B | 0.088 (6) | 0.048 (4) | 0.081 (5) | 0.015 (4) | 0.042 (4) | 0.007 (4) |
C4B | 0.034 (3) | 0.039 (3) | 0.053 (3) | 0.001 (3) | 0.001 (2) | −0.003 (3) |
C5B | 0.054 (4) | 0.050 (4) | 0.078 (4) | 0.000 (3) | 0.011 (3) | 0.003 (3) |
Si1C | 0.0543 (10) | 0.0375 (9) | 0.0449 (7) | 0.0076 (10) | 0.0018 (6) | −0.0007 (9) |
C1C | 0.061 (5) | 0.060 (4) | 0.071 (4) | −0.004 (4) | 0.019 (4) | −0.002 (4) |
C2C | 0.065 (5) | 0.057 (4) | 0.073 (4) | −0.003 (4) | −0.014 (4) | −0.006 (4) |
C3C | 0.069 (5) | 0.079 (5) | 0.052 (3) | 0.026 (4) | −0.008 (3) | −0.010 (4) |
C4C | 0.052 (4) | 0.052 (4) | 0.052 (3) | 0.009 (3) | 0.009 (3) | 0.007 (3) |
C5C | 0.058 (4) | 0.058 (4) | 0.077 (4) | 0.011 (4) | 0.008 (4) | 0.003 (4) |
Si1A—C4A | 1.823 (5) | C2B—H2BB | 0.980 |
Si1A—C2A | 1.854 (6) | C2B—H2BC | 0.980 |
Si1A—C3A | 1.861 (6) | C3B—H3BA | 0.980 |
Si1A—C1A | 1.862 (6) | C3B—H3BB | 0.980 |
C1A—H1AA | 0.980 | C3B—H3BC | 0.980 |
C1A—H1AB | 0.980 | C4B—C5B | 1.197 (8) |
C1A—H1AC | 0.980 | C5B—H5B | 0.950 |
C2A—H2AA | 0.980 | Si1C—C4C | 1.837 (6) |
C2A—H2AB | 0.980 | Si1C—C1C | 1.844 (6) |
C2A—H2AC | 0.980 | Si1C—C2C | 1.848 (6) |
C3A—H3AA | 0.980 | Si1C—C3C | 1.854 (6) |
C3A—H3AB | 0.980 | C1C—H1CA | 0.980 |
C3A—H3AC | 0.980 | C1C—H1CB | 0.980 |
C4A—C5A | 1.200 (7) | C1C—H1CC | 0.980 |
C5A—H5A | 0.950 | C2C—H2CA | 0.980 |
Si1B—C4B | 1.836 (6) | C2C—H2CB | 0.980 |
Si1B—C2B | 1.838 (6) | C2C—H2CC | 0.980 |
Si1B—C1B | 1.843 (6) | C3C—H3CA | 0.980 |
Si1B—C3B | 1.860 (6) | C3C—H3CB | 0.980 |
C1B—H1BA | 0.980 | C3C—H3CC | 0.980 |
C1B—H1BB | 0.980 | C4C—C5C | 1.185 (8) |
C1B—H1BC | 0.980 | C5C—H5C | 0.950 |
C2B—H2BA | 0.980 | ||
C4A—Si1A—C2A | 108.1 (3) | Si1B—C2B—H2BB | 109.5 |
C4A—Si1A—C3A | 107.5 (3) | H2BA—C2B—H2BB | 109.5 |
C2A—Si1A—C3A | 111.4 (3) | Si1B—C2B—H2BC | 109.5 |
C4A—Si1A—C1A | 107.8 (3) | H2BA—C2B—H2BC | 109.5 |
C2A—Si1A—C1A | 111.7 (3) | H2BB—C2B—H2BC | 109.5 |
C3A—Si1A—C1A | 110.2 (3) | Si1B—C3B—H3BA | 109.5 |
Si1A—C1A—H1AA | 109.5 | Si1B—C3B—H3BB | 109.5 |
Si1A—C1A—H1AB | 109.5 | H3BA—C3B—H3BB | 109.5 |
H1AA—C1A—H1AB | 109.5 | Si1B—C3B—H3BC | 109.5 |
Si1A—C1A—H1AC | 109.5 | H3BA—C3B—H3BC | 109.5 |
H1AA—C1A—H1AC | 109.5 | H3BB—C3B—H3BC | 109.5 |
H1AB—C1A—H1AC | 109.5 | C5B—C4B—Si1B | 176.1 (6) |
Si1A—C2A—H2AA | 109.5 | C4B—C5B—H5B | 180.0 |
Si1A—C2A—H2AB | 109.5 | C4C—Si1C—C1C | 106.9 (4) |
H2AA—C2A—H2AB | 109.5 | C4C—Si1C—C2C | 109.4 (3) |
Si1A—C2A—H2AC | 109.5 | C1C—Si1C—C2C | 110.3 (3) |
H2AA—C2A—H2AC | 109.5 | C4C—Si1C—C3C | 108.6 (3) |
H2AB—C2A—H2AC | 109.5 | C1C—Si1C—C3C | 110.4 (4) |
Si1A—C3A—H3AA | 109.5 | C2C—Si1C—C3C | 111.1 (4) |
Si1A—C3A—H3AB | 109.5 | Si1C—C1C—H1CA | 109.5 |
H3AA—C3A—H3AB | 109.5 | Si1C—C1C—H1CB | 109.5 |
Si1A—C3A—H3AC | 109.5 | H1CA—C1C—H1CB | 109.5 |
H3AA—C3A—H3AC | 109.5 | Si1C—C1C—H1CC | 109.5 |
H3AB—C3A—H3AC | 109.5 | H1CA—C1C—H1CC | 109.5 |
C5A—C4A—Si1A | 176.4 (6) | H1CB—C1C—H1CC | 109.5 |
C4A—C5A—H5A | 180.0 | Si1C—C2C—H2CA | 109.5 |
C4B—Si1B—C2B | 108.2 (3) | Si1C—C2C—H2CB | 109.5 |
C4B—Si1B—C1B | 107.4 (3) | H2CA—C2C—H2CB | 109.5 |
C2B—Si1B—C1B | 110.6 (3) | Si1C—C2C—H2CC | 109.5 |
C4B—Si1B—C3B | 108.6 (3) | H2CA—C2C—H2CC | 109.5 |
C2B—Si1B—C3B | 111.1 (4) | H2CB—C2C—H2CC | 109.5 |
C1B—Si1B—C3B | 110.7 (3) | Si1C—C3C—H3CA | 109.5 |
Si1B—C1B—H1BA | 109.5 | Si1C—C3C—H3CB | 109.5 |
Si1B—C1B—H1BB | 109.5 | H3CA—C3C—H3CB | 109.5 |
H1BA—C1B—H1BB | 109.5 | Si1C—C3C—H3CC | 109.5 |
Si1B—C1B—H1BC | 109.5 | H3CA—C3C—H3CC | 109.5 |
H1BA—C1B—H1BC | 109.5 | H3CB—C3C—H3CC | 109.5 |
H1BB—C1B—H1BC | 109.5 | C5C—C4C—Si1C | 177.5 (7) |
Si1B—C2B—H2BA | 109.5 | C4C—C5C—H5C | 180.0 |