Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802001332/cf6142sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536802001332/cf6142Isup2.hkl |
CCDC reference: 180807
Data collection: COLLECT (Nonius, 1998); cell refinement: HKL SCALEPACK (Otwinowski & Minor, 1997); data reduction: HKL SCALEPACK and DENZO (Otwinowski & Minor, 1997); 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) and CAMERON (Watkin et al., 1996); software used to prepare material for publication: SHELXL97.
C10H22 | F(000) = 82 |
Mr = 142.28 | Dx = 0.931 Mg m−3 |
Triclinic, P1 | Melting point: 243 K |
a = 4.1741 (4) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 4.7239 (6) Å | Cell parameters from 3994 reflections |
c = 13.5066 (15) Å | θ = 1.0–27.5° |
α = 85.974 (1)° | µ = 0.05 mm−1 |
β = 81.463 (7)° | T = 150 K |
γ = 74.652 (6)° | Cylinder, colourless |
V = 253.85 (5) Å3 | 0.15 mm (radius) |
Z = 1 |
Nonius KappaCCD diffractometer | 865 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.069 |
Graphite monochromator | θmax = 27.4°, θmin = 4.6° |
Thin–slice ω and φ scans | h = −4→5 |
2851 measured reflections | k = −6→6 |
1122 independent reflections | l = −15→17 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.054 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.181 | All H-atom parameters refined |
S = 1.09 | w = 1/[σ2(Fo2) + (0.0856P)2 + 0.0416P] where P = (Fo2 + 2Fc2)/3 |
1122 reflections | (Δ/σ)max < 0.001 |
90 parameters | Δρmax = 0.22 e Å−3 |
0 restraints | Δρmin = −0.18 e Å−3 |
Experimental. Crystal grown in situ in 0.3 mm glass capillary at 241.5 K |
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 | ||
C1 | 0.8145 (4) | 0.2469 (3) | 0.90220 (10) | 0.0378 (5) | |
H1A | 1.032 (5) | 0.112 (4) | 0.8816 (13) | 0.047 (4)* | |
H1B | 0.659 (4) | 0.132 (4) | 0.9203 (13) | 0.048 (4)* | |
H1C | 0.822 (5) | 0.348 (4) | 0.9652 (15) | 0.058 (5)* | |
C2 | 0.7018 (3) | 0.4660 (3) | 0.81807 (9) | 0.0314 (4) | |
H2A | 0.865 (4) | 0.588 (3) | 0.8014 (11) | 0.041 (4)* | |
H2B | 0.485 (4) | 0.594 (3) | 0.8401 (11) | 0.039 (4)* | |
C3 | 0.6817 (3) | 0.3198 (2) | 0.72290 (8) | 0.0269 (4) | |
H3A | 0.899 (4) | 0.184 (3) | 0.7009 (11) | 0.032 (3)* | |
H3B | 0.523 (4) | 0.199 (3) | 0.7389 (11) | 0.031 (3)* | |
C4 | 0.5746 (3) | 0.5375 (2) | 0.63783 (8) | 0.0269 (4) | |
H4A | 0.737 (4) | 0.654 (3) | 0.6228 (11) | 0.035 (4)* | |
H4B | 0.358 (4) | 0.671 (3) | 0.6601 (11) | 0.032 (3)* | |
C5 | 0.5523 (3) | 0.3915 (2) | 0.54273 (8) | 0.0265 (4) | |
H5A | 0.767 (4) | 0.255 (3) | 0.5210 (11) | 0.031 (3)* | |
H5B | 0.390 (4) | 0.270 (3) | 0.5587 (12) | 0.036 (4)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0419 (8) | 0.0452 (9) | 0.0268 (7) | −0.0105 (7) | −0.0103 (5) | 0.0040 (5) |
C2 | 0.0360 (7) | 0.0327 (7) | 0.0253 (6) | −0.0069 (5) | −0.0073 (5) | −0.0004 (5) |
C3 | 0.0296 (7) | 0.0270 (7) | 0.0234 (7) | −0.0060 (5) | −0.0050 (5) | 0.0012 (5) |
C4 | 0.0304 (7) | 0.0263 (7) | 0.0236 (7) | −0.0058 (5) | −0.0056 (5) | 0.0010 (5) |
C5 | 0.0301 (7) | 0.0259 (7) | 0.0228 (7) | −0.0058 (5) | −0.0053 (5) | 0.0011 (5) |
C1—C2 | 1.5232 (18) | C3—H3A | 0.979 (16) |
C1—H1A | 0.976 (18) | C3—H3B | 0.974 (15) |
C1—H1B | 0.946 (18) | C4—C5 | 1.5257 (15) |
C1—H1C | 1.01 (2) | C4—H4A | 0.972 (15) |
C2—C3 | 1.5242 (15) | C4—H4B | 0.976 (16) |
C2—H2A | 0.994 (16) | C5—C5i | 1.523 (2) |
C2—H2B | 0.963 (16) | C5—H5A | 0.974 (16) |
C3—C4 | 1.5233 (16) | C5—H5B | 0.988 (16) |
C2—C1—H1A | 111.5 (10) | C4—C3—H3B | 109.3 (9) |
C2—C1—H1B | 110.0 (10) | C2—C3—H3B | 108.4 (9) |
H1A—C1—H1B | 107.2 (16) | H3A—C3—H3B | 106.1 (13) |
C2—C1—H1C | 112.0 (10) | C3—C4—C5 | 113.56 (9) |
H1A—C1—H1C | 110.0 (15) | C3—C4—H4A | 107.9 (9) |
H1B—C1—H1C | 105.9 (14) | C5—C4—H4A | 109.1 (9) |
C1—C2—C3 | 113.19 (11) | C3—C4—H4B | 109.4 (9) |
C1—C2—H2A | 108.7 (9) | C5—C4—H4B | 109.2 (9) |
C3—C2—H2A | 108.1 (9) | H4A—C4—H4B | 107.5 (13) |
C1—C2—H2B | 109.7 (9) | C5i—C5—C4 | 113.69 (11) |
C3—C2—H2B | 108.8 (9) | C5i—C5—H5A | 109.7 (9) |
H2A—C2—H2B | 108.3 (13) | C4—C5—H5A | 109.6 (9) |
C4—C3—C2 | 113.50 (10) | C5i—C5—H5B | 109.2 (9) |
C4—C3—H3A | 109.7 (9) | C4—C5—H5B | 108.8 (9) |
C2—C3—H3A | 109.6 (8) | H5A—C5—H5B | 105.5 (13) |
C1—C2—C3—C4 | −179.04 (11) | C3—C4—C5—C5i | −179.59 (12) |
C2—C3—C4—C5 | −179.63 (9) |
Symmetry code: (i) −x+1, −y+1, −z+1. |