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
Key indicators
- Single-crystal X-ray study
- T = 150 K
- Mean (C-C) = 0.009 Å
- R factor = 0.096
- wR factor = 0.273
- Data-to-parameter ratio = 20.1
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level B:
DIFMX_01 Alert B The maximum difference density is > 0.1*ZMAX*1.00 _refine_diff_density_max given = 1.532 Test value = 1.400
Alert Level C:
DIFMX_02 Alert C The minimum difference density is > 0.1*ZMAX*0.75 The relevant atom site should be identified. RFACR_01 Alert C The value of the weighted R factor is > 0.25 Weighted R factor given 0.273 General Notes
REFLT_03 From the CIF: _diffrn_reflns_theta_max 27.46 From the CIF: _reflns_number_total 3566 Count of symmetry unique reflns 2706 Completeness (_total/calc) 131.78% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 860 Fraction of Friedel pairs measured 0.318 Are heavy atom types Z>Si present yes WARNING: Large fraction of Friedel related reflns may be needed to determine absolute structure
0 Alert Level A = Potentially serious problem
1 Alert Level B = Potential problem
2 Alert Level C = Please check
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 |