Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805021847/sj6115sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805021847/sj6115IIsup2.hkl |
CCDC reference: 282635
Key indicators
- Single-crystal X-ray study
- T = 292 K
- Mean (C-C) = 0.003 Å
- R factor = 0.049
- wR factor = 0.149
- Data-to-parameter ratio = 10.6
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT063_ALERT_3_C Crystal Probably too Large for Beam Size ....... 0.72 mm
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 1 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: CAD-4 Software (Enraf–Nonius, 1989); cell refinement: CAD-4 Software; data reduction: modified version of NRC-2/NRC2A (Ahmed et al., 1973); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: enCIFer (Allen et al., 2004).
C32H36O8Si | Dx = 1.315 Mg m−3 |
Mr = 576.70 | Cu Kα radiation, λ = 1.5418 Å |
Tetragonal, I41/a | Cell parameters from 25 reflections |
Hall symbol: -I 4ad | θ = 20.0–22.5° |
a = 17.230 (7) Å | µ = 1.14 mm−1 |
c = 9.812 (4) Å | T = 292 K |
V = 2913 (2) Å3 | Block, colorless |
Z = 4 | 0.72 × 0.15 × 0.12 mm |
F(000) = 1224 |
Enraf–Nonius CAD-4 diffractometer | 1138 reflections with I > 2σ(I) |
Radiation source: X-ray sealed tube | Rint = 0.077 |
Graphite monochromator | θmax = 69.7°, θmin = 5.1° |
ω/2θ scans | h = −21→21 |
Absorption correction: integration (ABSORP in NRCVAX; Gabe et al., 1989) | k = −21→21 |
Tmin = 0.760, Tmax = 0.880 | l = −11→11 |
10945 measured reflections | 5 standard reflections every 60 min |
1377 independent reflections | intensity decay: 0.3% |
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)] = 0.049 | All H-atom parameters refined |
wR(F2) = 0.149 | w = 1/[σ2(Fo2) + (0.1051P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.06 | (Δ/σ)max = 0.001 |
1377 reflections | Δρmax = 0.38 e Å−3 |
130 parameters | Δρmin = −0.36 e Å−3 |
0 restraints | Extinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0013 (3) |
Experimental. X-ray crystallographic data for II were collected from a single-crystal sample, which was mounted on a glass fiber. Data were collected using an Enraf–Nonius CAD4 diffractometer equipped with FR590 generator, a Kappa goniometer, a standard scintillation counter and a locally modified low temperature device. The initial unit-cell parameters were determined by a least-squares fit of the angular setting of 25 strong reflections. The intensity of some selected strong reflections was monitored during the course of the data collection. Data were corrected for absorption, Lorentz and polarization effect |
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. Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 13.3221 (0.0105) x + 6.3407 (0.0132) y + 5.0677 (0.0071) z = 2.0909 (0.0023) * 0.0040 (0.0014) C1 * -0.0073 (0.0014) C2 * 0.0038 (0.0015) C3 * 0.0031 (0.0015) C4 * -0.0066 (0.0014) C5 * 0.0030 (0.0014) C6 0.1277 (0.0027) Si 0.0177 (0.0031) O3 - 0.0480 (0.0029) O5 - 0.0978 (0.0049) C31 - 0.0949 (0.0044) C51 Rms deviation of fitted atoms = 0.0049 |
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 | ||
Si | 0.0000 | 0.2500 | 0.1250 | 0.0331 (3) | |
O3 | 0.15623 (11) | −0.00610 (8) | 0.01301 (19) | 0.0578 (5) | |
O5 | 0.17764 (10) | 0.19154 (9) | −0.30352 (17) | 0.0508 (5) | |
C1 | 0.06290 (11) | 0.18689 (10) | 0.0142 (2) | 0.0359 (5) | |
C2 | 0.08161 (12) | 0.11174 (11) | 0.0568 (2) | 0.0398 (5) | |
H2 | 0.0601 (14) | 0.0918 (14) | 0.144 (3) | 0.048 (6)* | |
C3 | 0.13314 (12) | 0.06695 (11) | −0.0204 (2) | 0.0401 (5) | |
C4 | 0.16448 (12) | 0.09599 (12) | −0.1393 (2) | 0.0418 (5) | |
H4 | 0.1976 (15) | 0.0652 (14) | −0.186 (3) | 0.048 (6)* | |
C5 | 0.14504 (11) | 0.16987 (11) | −0.1825 (2) | 0.0383 (5) | |
C6 | 0.09483 (11) | 0.21584 (11) | −0.1062 (2) | 0.0378 (5) | |
H6 | 0.0841 (14) | 0.2685 (14) | −0.135 (2) | 0.045 (6)* | |
C31 | 0.1215 (2) | −0.04219 (16) | 0.1267 (4) | 0.0673 (8) | |
H31A | 0.1318 (19) | −0.0154 (18) | 0.211 (3) | 0.071 (9)* | |
H31B | 0.1464 (19) | −0.0959 (19) | 0.130 (3) | 0.078 (9)* | |
H31C | 0.0654 (19) | −0.0464 (16) | 0.114 (3) | 0.061 (8)* | |
C51 | 0.15877 (17) | 0.26615 (15) | −0.3565 (3) | 0.0573 (7) | |
H51A | 0.1756 (18) | 0.3049 (18) | −0.290 (3) | 0.070 (9)* | |
H51B | 0.100 (2) | 0.267 (2) | −0.378 (4) | 0.084 (10)* | |
H51C | 0.191 (2) | 0.275 (2) | −0.448 (4) | 0.087 (10)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Si | 0.0285 (4) | 0.0285 (4) | 0.0425 (6) | 0.000 | 0.000 | 0.000 |
O3 | 0.0743 (11) | 0.0314 (8) | 0.0677 (12) | 0.0145 (7) | 0.0131 (8) | 0.0084 (7) |
O5 | 0.0584 (10) | 0.0421 (8) | 0.0519 (10) | 0.0090 (7) | 0.0136 (7) | 0.0051 (7) |
C1 | 0.0313 (9) | 0.0315 (9) | 0.0449 (11) | −0.0007 (7) | −0.0022 (7) | −0.0020 (8) |
C2 | 0.0389 (10) | 0.0323 (9) | 0.0482 (12) | 0.0018 (7) | 0.0027 (9) | 0.0013 (8) |
C3 | 0.0413 (10) | 0.0281 (9) | 0.0509 (12) | 0.0044 (7) | −0.0016 (9) | 0.0007 (8) |
C4 | 0.0393 (10) | 0.0346 (10) | 0.0516 (12) | 0.0066 (8) | 0.0038 (9) | −0.0035 (9) |
C5 | 0.0356 (9) | 0.0360 (10) | 0.0433 (11) | 0.0003 (7) | 0.0014 (8) | −0.0008 (8) |
C6 | 0.0359 (10) | 0.0297 (9) | 0.0478 (12) | 0.0023 (7) | −0.0016 (8) | 0.0011 (8) |
C31 | 0.087 (2) | 0.0383 (13) | 0.077 (2) | 0.0037 (13) | 0.0108 (16) | 0.0134 (12) |
C51 | 0.0677 (16) | 0.0436 (13) | 0.0605 (16) | 0.0051 (11) | 0.0102 (12) | 0.0122 (11) |
Si—C1i | 1.881 (2) | C3—C4 | 1.379 (3) |
Si—C1ii | 1.881 (2) | C4—C5 | 1.383 (3) |
Si—C1iii | 1.881 (2) | C4—H4 | 0.91 (3) |
Si—C1 | 1.881 (2) | C5—C6 | 1.392 (3) |
O3—C3 | 1.360 (2) | C6—H6 | 0.97 (2) |
O3—C31 | 1.410 (3) | C31—H31A | 0.96 (3) |
O5—C5 | 1.366 (2) | C31—H31B | 1.02 (3) |
O5—C51 | 1.424 (3) | C31—H31C | 0.98 (3) |
C1—C6 | 1.395 (3) | C51—H51A | 0.98 (3) |
C1—C2 | 1.398 (3) | C51—H51B | 1.03 (3) |
C2—C3 | 1.399 (3) | C51—H51C | 1.07 (4) |
C2—H2 | 1.00 (3) | ||
C1iii—Si—C1i | 109.38 (12) | C5—C4—H4 | 122.5 (17) |
C1iii—Si—C1ii | 109.52 (6) | O5—C5—C4 | 114.76 (17) |
C1i—Si—C1ii | 109.52 (6) | O5—C5—C6 | 124.62 (18) |
C1iii—Si—C1 | 109.52 (6) | C4—C5—C6 | 120.62 (19) |
C1i—Si—C1 | 109.52 (6) | C5—C6—C1 | 119.82 (18) |
C1ii—Si—C1 | 109.38 (12) | C5—C6—H6 | 119.7 (13) |
C3—O3—C31 | 118.33 (19) | C1—C6—H6 | 120.5 (13) |
C5—O5—C51 | 118.06 (17) | O3—C31—H31A | 112.9 (19) |
C6—C1—C2 | 119.57 (18) | O3—C31—H31B | 104.3 (17) |
C6—C1—Si | 120.65 (14) | H31A—C31—H31B | 109 (3) |
C2—C1—Si | 119.67 (15) | O3—C31—H31C | 110.6 (17) |
C1—C2—C3 | 119.66 (19) | H31A—C31—H31C | 109 (3) |
C1—C2—H2 | 119.4 (14) | H31B—C31—H31C | 111 (2) |
C3—C2—H2 | 120.8 (14) | O5—C51—H51A | 107.7 (18) |
O3—C3—C4 | 115.16 (18) | O5—C51—H51B | 108 (2) |
O3—C3—C2 | 124.4 (2) | H51A—C51—H51B | 115 (3) |
C4—C3—C2 | 120.41 (18) | O5—C51—H51C | 108.5 (19) |
C3—C4—C5 | 119.90 (18) | H51A—C51—H51C | 108 (2) |
C3—C4—H4 | 117.6 (17) | H51B—C51—H51C | 110 (3) |
C1i—Si—C1—C6 | −81.85 (12) | C1—C2—C3—C4 | −1.1 (3) |
C1ii—Si—C1—C6 | 38.18 (13) | O3—C3—C4—C5 | −179.82 (19) |
C1iii—Si—C1—C6 | 158.20 (16) | C2—C3—C4—C5 | 0.1 (3) |
C1i—Si—C1—C2 | 94.3 (2) | C51—O5—C5—C4 | 178.4 (2) |
C1ii—Si—C1—C2 | −145.63 (18) | C51—O5—C5—C6 | −0.5 (3) |
C1iii—Si—C1—C2 | −25.60 (17) | C3—C4—C5—O5 | −178.07 (18) |
C6—C1—C2—C3 | 1.1 (3) | C3—C4—C5—C6 | 0.9 (3) |
Si—C1—C2—C3 | −175.13 (15) | O5—C5—C6—C1 | 177.98 (18) |
C31—O3—C3—C4 | −174.6 (2) | C4—C5—C6—C1 | −0.9 (3) |
C31—O3—C3—C2 | 5.5 (4) | C2—C1—C6—C5 | −0.1 (3) |
C1—C2—C3—O3 | 178.81 (19) | Si—C1—C6—C5 | 176.07 (14) |
Symmetry codes: (i) −y+1/4, x+1/4, −z+1/4; (ii) −x, −y+1/2, z; (iii) y−1/4, −x+1/4, −z+1/4. |