Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806055498/rz2101sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806055498/rz2101Isup2.hkl |
CCDC reference: 638522
Key indicators
- Single-crystal X-ray study
- T = 291 K
- Mean (C-C) = 0.003 Å
- R factor = 0.027
- wR factor = 0.057
- Data-to-parameter ratio = 9.2
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C12
Alert level G REFLT03_ALERT_1_G ALERT: Expected hkl max differ from CIF values From the CIF: _diffrn_reflns_theta_max 27.45 From the CIF: _reflns_number_total 1271 From the CIF: _diffrn_reflns_limit_ max hkl 14. 10. 21. From the CIF: _diffrn_reflns_limit_ min hkl -14. -9. -21. TEST1: Expected hkl limits for theta max Calculated maximum hkl 15. 15. 21. Calculated minimum hkl -15. -15. -21. REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 27.45 From the CIF: _reflns_number_total 1271 Count of symmetry unique reflns 1278 Completeness (_total/calc) 99.45% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 0 Fraction of Friedel pairs measured 0.000 Are heavy atom types Z>Si present no
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 1 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Data collection: COLLECT (Nonius, 1998); cell refinement: DENZO and SCALEPACK (Otwinowski & Minor, 1997); data reduction: DENZO and SCALEPACK; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL-Plus (Sheldrick, 1991); software used to prepare material for publication: SHELXL97, PARST95 (Nardelli, 1995) and PLATON (Spek, 2003).
C28H26O2 | Dx = 1.205 Mg m−3 |
Mr = 394.49 | Mo Kα radiation, λ = 0.71073 Å |
Tetragonal, I41 | Cell parameters from 14054 reflections |
Hall symbol: I 4bw | θ = 3.5–27.5° |
a = 11.5777 (8) Å | µ = 0.07 mm−1 |
c = 16.2234 (8) Å | T = 291 K |
V = 2174.6 (2) Å3 | Block, colourless |
Z = 4 | 0.25 × 0.20 × 0.20 mm |
F(000) = 840 |
Nonius KappaCCD diffractometer | 707 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.027 |
Graphite monochromator | θmax = 27.5°, θmin = 3.5° |
Detector resolution: 19 vertical, 18 horizontal pixels mm-1 | h = −14→14 |
415 frames via ω–rotation (Δω=1%) and two times 25 s per frame (four sets at different κ–angles) scans | k = −9→10 |
14054 measured reflections | l = −21→21 |
1271 independent reflections |
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)] = 0.027 | H-atom parameters constrained |
wR(F2) = 0.057 | w = 1/[σ2(Fo2) + (0.0252P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.88 | (Δ/σ)max < 0.001 |
1271 reflections | Δρmax = 0.10 e Å−3 |
138 parameters | Δρmin = −0.08 e Å−3 |
1 restraint | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0185 (10) |
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 | ||
O1 | 0.99540 (10) | 0.62800 (12) | 0.98077 (8) | 0.0659 (4) | |
C1 | 0.91135 (16) | 0.60295 (17) | 0.92374 (11) | 0.0519 (5) | |
C2 | 0.80159 (17) | 0.65405 (18) | 0.92741 (13) | 0.0602 (5) | |
H2 | 0.7837 | 0.7055 | 0.9695 | 0.072* | |
C3 | 0.72153 (16) | 0.62798 (17) | 0.86910 (12) | 0.0594 (5) | |
H3 | 0.6488 | 0.6618 | 0.8720 | 0.071* | |
C4 | 0.74614 (15) | 0.55129 (17) | 0.80456 (12) | 0.0500 (5) | |
C5 | 0.66338 (18) | 0.52285 (18) | 0.74414 (13) | 0.0646 (6) | |
H5 | 0.5905 | 0.5563 | 0.7466 | 0.078* | |
C6 | 0.6880 (2) | 0.4474 (2) | 0.68236 (15) | 0.0725 (6) | |
H6 | 0.6322 | 0.4294 | 0.6432 | 0.087* | |
C7 | 0.79769 (19) | 0.39708 (17) | 0.67800 (13) | 0.0655 (6) | |
H7 | 0.8147 | 0.3459 | 0.6355 | 0.079* | |
C8 | 0.87975 (18) | 0.42224 (16) | 0.73527 (11) | 0.0552 (5) | |
H8 | 0.9520 | 0.3874 | 0.7315 | 0.066* | |
C9 | 0.85755 (16) | 0.50019 (15) | 0.80043 (10) | 0.0465 (5) | |
C10 | 0.94154 (14) | 0.52736 (15) | 0.86183 (11) | 0.0453 (4) | |
C11 | 0.96027 (19) | 0.66652 (19) | 1.05994 (11) | 0.0636 (6) | |
H11A | 0.8942 | 0.6219 | 1.0784 | 0.076* | |
H11B | 0.9375 | 0.7471 | 1.0571 | 0.076* | |
C12 | 1.0571 (2) | 0.65283 (18) | 1.11950 (12) | 0.0651 (6) | |
C13 | 1.0244 (2) | 0.6738 (3) | 1.20661 (13) | 0.1052 (10) | |
H13A | 1.0911 | 0.6644 | 1.2412 | 0.158* | |
H13B | 0.9659 | 0.6196 | 1.2228 | 0.158* | |
H13C | 0.9952 | 0.7510 | 1.2123 | 0.158* | |
C14 | 1.1616 (2) | 0.6250 (2) | 1.09709 (16) | 0.0866 (8) | |
H14A | 1.1783 | 0.6127 | 1.0417 | 0.104* | |
H14B | 1.2195 | 0.6174 | 1.1365 | 0.104* |
U11 | U22 | U33 | U12 | U13 | U23 | |
O1 | 0.0535 (8) | 0.0948 (11) | 0.0495 (8) | 0.0020 (7) | 0.0008 (7) | −0.0181 (8) |
C1 | 0.0478 (12) | 0.0619 (12) | 0.0459 (11) | −0.0004 (10) | 0.0024 (10) | −0.0004 (10) |
C2 | 0.0555 (13) | 0.0668 (13) | 0.0583 (12) | 0.0080 (10) | 0.0087 (11) | −0.0062 (11) |
C3 | 0.0451 (12) | 0.0661 (14) | 0.0671 (13) | 0.0097 (10) | 0.0074 (11) | 0.0081 (12) |
C4 | 0.0406 (12) | 0.0575 (12) | 0.0519 (11) | −0.0019 (10) | −0.0008 (10) | 0.0108 (10) |
C5 | 0.0474 (13) | 0.0759 (15) | 0.0705 (16) | −0.0034 (11) | −0.0062 (11) | 0.0146 (13) |
C6 | 0.0600 (16) | 0.0917 (17) | 0.0658 (14) | −0.0192 (13) | −0.0184 (12) | 0.0093 (14) |
C7 | 0.0681 (16) | 0.0711 (15) | 0.0573 (12) | −0.0111 (12) | −0.0063 (12) | −0.0026 (12) |
C8 | 0.0532 (13) | 0.0583 (13) | 0.0542 (12) | −0.0034 (10) | −0.0029 (10) | 0.0013 (11) |
C9 | 0.0470 (12) | 0.0488 (12) | 0.0436 (11) | −0.0014 (9) | 0.0009 (9) | 0.0072 (9) |
C10 | 0.0410 (10) | 0.0543 (11) | 0.0405 (10) | 0.0015 (9) | 0.0020 (9) | 0.0027 (10) |
C11 | 0.0737 (14) | 0.0683 (14) | 0.0490 (12) | 0.0021 (11) | 0.0092 (12) | −0.0136 (11) |
C12 | 0.0778 (16) | 0.0647 (14) | 0.0529 (15) | −0.0068 (12) | −0.0041 (12) | −0.0089 (11) |
C13 | 0.134 (2) | 0.125 (2) | 0.0558 (16) | −0.0090 (18) | −0.0028 (15) | −0.0144 (14) |
C14 | 0.0786 (17) | 0.108 (2) | 0.0734 (15) | 0.0016 (15) | −0.0198 (14) | −0.0125 (14) |
O1—C1 | 1.374 (2) | C7—H7 | 0.9300 |
O1—C11 | 1.419 (2) | C8—C9 | 1.413 (2) |
C1—C10 | 1.377 (2) | C8—H8 | 0.9300 |
C1—C2 | 1.403 (2) | C9—C10 | 1.427 (2) |
C2—C3 | 1.358 (3) | C10—C10i | 1.495 (3) |
C2—H2 | 0.9300 | C11—C12 | 1.489 (3) |
C3—C4 | 1.402 (2) | C11—H11A | 0.9700 |
C3—H3 | 0.9300 | C11—H11B | 0.9700 |
C4—C5 | 1.410 (3) | C12—C14 | 1.304 (3) |
C4—C9 | 1.421 (2) | C12—C13 | 1.483 (3) |
C5—C6 | 1.359 (3) | C13—H13A | 0.9600 |
C5—H5 | 0.9300 | C13—H13B | 0.9600 |
C6—C7 | 1.399 (3) | C13—H13C | 0.9600 |
C6—H6 | 0.9300 | C14—H14A | 0.9300 |
C7—C8 | 1.360 (3) | C14—H14B | 0.9300 |
C1—O1—C11 | 118.22 (14) | C8—C9—C4 | 117.79 (17) |
O1—C1—C10 | 116.47 (15) | C8—C9—C10 | 122.60 (16) |
O1—C1—C2 | 121.60 (18) | C4—C9—C10 | 119.61 (16) |
C10—C1—C2 | 121.92 (18) | C1—C10—C9 | 118.43 (15) |
C3—C2—C1 | 119.7 (2) | C1—C10—C10i | 119.94 (13) |
C3—C2—H2 | 120.2 | C9—C10—C10i | 121.58 (14) |
C1—C2—H2 | 120.2 | O1—C11—C12 | 109.76 (17) |
C2—C3—C4 | 121.48 (17) | O1—C11—H11A | 109.7 |
C2—C3—H3 | 119.3 | C12—C11—H11A | 109.7 |
C4—C3—H3 | 119.3 | O1—C11—H11B | 109.7 |
C3—C4—C5 | 121.94 (18) | C12—C11—H11B | 109.7 |
C3—C4—C9 | 118.91 (16) | H11A—C11—H11B | 108.2 |
C5—C4—C9 | 119.15 (19) | C14—C12—C11 | 123.0 (2) |
C6—C5—C4 | 121.3 (2) | C14—C12—C13 | 122.9 (2) |
C6—C5—H5 | 119.3 | C11—C12—C13 | 114.1 (2) |
C4—C5—H5 | 119.3 | C12—C13—H13A | 109.5 |
C5—C6—C7 | 119.7 (2) | C12—C13—H13B | 109.5 |
C5—C6—H6 | 120.2 | H13A—C13—H13B | 109.5 |
C7—C6—H6 | 120.2 | C12—C13—H13C | 109.5 |
C8—C7—C6 | 120.7 (2) | H13A—C13—H13C | 109.5 |
C8—C7—H7 | 119.7 | H13B—C13—H13C | 109.5 |
C6—C7—H7 | 119.7 | C12—C14—H14A | 120.0 |
C7—C8—C9 | 121.36 (19) | C12—C14—H14B | 120.0 |
C7—C8—H8 | 119.3 | H14A—C14—H14B | 120.0 |
C9—C8—H8 | 119.3 | ||
C11—O1—C1—C10 | −156.20 (17) | C5—C4—C9—C8 | −0.2 (2) |
C11—O1—C1—C2 | 25.3 (3) | C3—C4—C9—C10 | 0.3 (2) |
O1—C1—C2—C3 | 179.12 (17) | C5—C4—C9—C10 | −179.28 (17) |
C10—C1—C2—C3 | 0.7 (3) | O1—C1—C10—C9 | −179.03 (15) |
C1—C2—C3—C4 | −0.4 (3) | C2—C1—C10—C9 | −0.6 (3) |
C2—C3—C4—C5 | 179.43 (18) | O1—C1—C10—C10i | 3.2 (3) |
C2—C3—C4—C9 | −0.1 (3) | C2—C1—C10—C10i | −178.34 (18) |
C3—C4—C5—C6 | −179.33 (18) | C8—C9—C10—C1 | −178.97 (16) |
C9—C4—C5—C6 | 0.2 (3) | C4—C9—C10—C1 | 0.1 (2) |
C4—C5—C6—C7 | −0.3 (3) | C8—C9—C10—C10i | −1.2 (3) |
C5—C6—C7—C8 | 0.4 (3) | C4—C9—C10—C10i | 177.80 (18) |
C6—C7—C8—C9 | −0.4 (3) | C1—O1—C11—C12 | 161.93 (16) |
C7—C8—C9—C4 | 0.3 (2) | O1—C11—C12—C14 | 8.8 (3) |
C7—C8—C9—C10 | 179.37 (17) | O1—C11—C12—C13 | −171.2 (2) |
C3—C4—C9—C8 | 179.34 (16) |
Symmetry code: (i) −x+2, −y+1, z. |
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