Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801007176/ci6025sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536801007176/ci6025Isup2.hkl |
CCDC reference: 170288
Key indicators
- Single-crystal X-ray study
- T = 296 K
- Mean (C-C) = 0.003 Å
- R factor = 0.040
- wR factor = 0.137
- Data-to-parameter ratio = 10.7
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level A:
ABSTM_02 Alert A Test not performed as the _exptl_absorpt_correction_type has not been identified. See test ABSTY_01. ABSTY_01 Alert A The absorption correction should be one of the following * none * analytical * integration * numerical * gaussian * empirical * psi-scan * multi-scan * refdelf * sphere * cylinder
Alert Level C:
REFLT_03 From the CIF: _diffrn_reflns_theta_max 70.58 From the CIF: _reflns_number_total 2117 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 2237 Completeness (_total/calc) 94.64% Alert C: < 95% complete General Notes
REFLT_03 From the CIF: _diffrn_reflns_theta_max 70.58 From the CIF: _reflns_number_total 2117 Count of symmetry unique reflns 2237 Completeness (_total/calc) 94.64% 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 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.
2 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check
Data collection: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1992); cell refinement: MSC/AFC Diffractometer Control Software; data reduction: TEXSAN (Molecular Structure Corporation, 2000); program(s) used to solve structure: SAPI91 (Fan, 1991); program(s) used to refine structure: TEXSAN; software used to prepare material for publication: TEXSAN.
C19H40O2 | Dx = 1.034 Mg m−3 |
Mr = 300.52 | Cu Kα radiation, λ = 1.5418 Å |
Orthorhombic, P212121 | Cell parameters from 22 reflections |
a = 7.213 (5) Å | θ = 9.1–15.2° |
b = 52.870 (3) Å | µ = 0.49 mm−1 |
c = 5.061 (3) Å | T = 296 K |
V = 1930 (1) Å3 | Plate, colorless |
Z = 4 | 0.6 × 0.3 × 0.04 mm |
Rigaku AFC-5R diffractometer | Rint = 0.014 |
ω scans | θmax = 70.6° |
Absorption correction: ψ (North et al., 1968) | h = −2→8 |
Tmin = 0.757, Tmax = 1.000 | k = 0→64 |
3390 measured reflections | l = −1→5 |
2117 independent reflections | 3 standard reflections every 150 reflections |
1367 reflections with F2 > 2σ(F2) | intensity decay: 3.0% |
Refinement on F2 | w = 1/[σ2(Fo2) + {0.05[Max(Fo2,0) + 2Fc2]/3}2] |
R[F2 > 2σ(F2)] = 0.040 | (Δ/σ)max = 0.001 |
wR(F2) = 0.137 | Δρmax = 0.09 e Å−3 |
S = 1.42 | Δρmin = −0.11 e Å−3 |
2110 reflections | Extinction correction: Zachariasen (1967), type 2, Gaussian isotropic |
197 parameters | Extinction coefficient: 0.043 (5) |
H atoms treated by a mixture of independent and constrained refinement |
Geometry. none |
Refinement. Refinement using reflections with F2 > -3.0 σ(F2). The weighted R-factor (wR) and goodness of fit (S) are based on F2. R-factor (gt) are based on F. The threshold expression of F2 > 2.0 σ(F2) is used only for calculating R-factor (gt). |
x | y | z | Uiso*/Ueq | ||
O1 | 1.0560 (3) | −0.23030 (3) | 0.8589 (4) | 0.0673 (5) | |
O2 | 1.0635 (3) | 0.22552 (3) | 0.4290 (4) | 0.0753 (6) | |
C1 | 0.9980 (5) | −0.22781 (4) | 0.5912 (6) | 0.0716 (9) | |
C2 | 1.0529 (4) | −0.20292 (4) | 0.4731 (5) | 0.0614 (7) | |
C3 | 0.9668 (4) | −0.17984 (4) | 0.6013 (5) | 0.0528 (6) | |
C4 | 1.0383 (4) | −0.15524 (4) | 0.4877 (5) | 0.0532 (6) | |
C5 | 0.9582 (4) | −0.13159 (4) | 0.6122 (5) | 0.0514 (6) | |
C6 | 1.0362 (3) | −0.10725 (4) | 0.4999 (5) | 0.0516 (6) | |
C7 | 0.9584 (4) | −0.08339 (4) | 0.6226 (5) | 0.0519 (6) | |
C8 | 1.0380 (3) | −0.05920 (4) | 0.5089 (5) | 0.0516 (6) | |
C9 | 0.9591 (3) | −0.03524 (4) | 0.6290 (5) | 0.0522 (6) | |
C10 | 1.0394 (3) | −0.01113 (4) | 0.5130 (5) | 0.0509 (6) | |
C11 | 0.9597 (3) | 0.01295 (4) | 0.6297 (5) | 0.0509 (6) | |
C12 | 1.0398 (3) | 0.03697 (4) | 0.5114 (5) | 0.0506 (6) | |
C13 | 0.9594 (3) | 0.06115 (3) | 0.6264 (5) | 0.0512 (6) | |
C14 | 1.0396 (4) | 0.08501 (4) | 0.5060 (5) | 0.0511 (6) | |
C15 | 0.9590 (3) | 0.10942 (4) | 0.6160 (5) | 0.0516 (6) | |
C16 | 1.0399 (4) | 0.13306 (4) | 0.4919 (5) | 0.0519 (6) | |
C17 | 0.9605 (3) | 0.15773 (4) | 0.5962 (5) | 0.0533 (6) | |
C18 | 1.0466 (4) | 0.18074 (4) | 0.4654 (5) | 0.0555 (6) | |
C19 | 0.9709 (4) | 0.20556 (4) | 0.5639 (6) | 0.0595 (7) | |
H1a | 1.0528 | −0.2410 | 0.4904 | 0.0859* | |
H1b | 0.8668 | −0.2293 | 0.5841 | 0.0859* | |
H1o | 1.179 (4) | −0.2287 (5) | 0.857 (6) | 0.0809* | |
H2a | 1.1838 | −0.2014 | 0.4864 | 0.0737* | |
H2b | 1.0179 | −0.2030 | 0.2922 | 0.0737* | |
H2o | 1.008 (4) | 0.2390 (5) | 0.484 (7) | 0.0904* | |
H3a | 0.8363 | −0.1805 | 0.5763 | 0.0634* | |
H3b | 0.9939 | −0.1802 | 0.7850 | 0.0634* | |
H4a | 1.1690 | −0.1549 | 0.5105 | 0.0639* | |
H4b | 1.0097 | −0.1550 | 0.3045 | 0.0639* | |
H5a | 0.8279 | −0.1316 | 0.5850 | 0.0617* | |
H5b | 0.9837 | −0.1320 | 0.7963 | 0.0617* | |
H6a | 1.1666 | −0.1073 | 0.5265 | 0.0619* | |
H6b | 1.0104 | −0.1069 | 0.3159 | 0.0619* | |
H7a | 0.8280 | −0.0833 | 0.5956 | 0.0623* | |
H7b | 0.9839 | −0.0837 | 0.8067 | 0.0623* | |
H8a | 1.1682 | −0.0593 | 0.5375 | 0.0619* | |
H8b | 1.0136 | −0.0590 | 0.3245 | 0.0619* | |
H9a | 0.8289 | −0.0351 | 0.6010 | 0.0627* | |
H9b | 0.9840 | −0.0354 | 0.8133 | 0.0627* | |
H10a | 1.1694 | −0.0112 | 0.5428 | 0.0611* | |
H10b | 1.0158 | −0.0111 | 0.3283 | 0.0611* | |
H11a | 0.8296 | 0.0130 | 0.6009 | 0.0611* | |
H11b | 0.9840 | 0.0130 | 0.8142 | 0.0611* | |
H12a | 1.1698 | 0.0370 | 0.5412 | 0.0607* | |
H12b | 1.0162 | 0.0369 | 0.3267 | 0.0607* | |
H13a | 0.8293 | 0.0611 | 0.5973 | 0.0614* | |
H13b | 0.9835 | 0.0614 | 0.8109 | 0.0614* | |
H14a | 1.1695 | 0.0851 | 0.5372 | 0.0614* | |
H14b | 1.0170 | 0.0846 | 0.3211 | 0.0614* | |
H15a | 0.8290 | 0.1094 | 0.5859 | 0.0619* | |
H15b | 0.9823 | 0.1099 | 0.8007 | 0.0619* | |
H16a | 1.1697 | 0.1331 | 0.5236 | 0.0623* | |
H16b | 1.0176 | 0.1324 | 0.3071 | 0.0623* | |
H17a | 0.8307 | 0.1579 | 0.5643 | 0.0639* | |
H17b | 0.9827 | 0.1586 | 0.7810 | 0.0639* | |
H18a | 1.1763 | 0.1804 | 0.4976 | 0.0666* | |
H18b | 1.0245 | 0.1797 | 0.2807 | 0.0666* | |
H19a | 0.9920 | 0.2070 | 0.7486 | 0.0715* | |
H19b | 0.8416 | 0.2064 | 0.5296 | 0.0715* |
U11 | U22 | U33 | U12 | U13 | U23 | |
O1 | 0.089 (1) | 0.0447 (8) | 0.068 (1) | −0.0057 (10) | −0.005 (1) | 0.0044 (8) |
O2 | 0.092 (1) | 0.0371 (7) | 0.097 (1) | 0.0021 (9) | 0.022 (1) | 0.0010 (8) |
C1 | 0.102 (2) | 0.044 (1) | 0.069 (2) | −0.004 (1) | −0.010 (2) | −0.008 (1) |
C2 | 0.086 (2) | 0.044 (1) | 0.054 (1) | 0.005 (1) | 0.005 (2) | −0.0027 (10) |
C3 | 0.060 (1) | 0.0402 (9) | 0.059 (1) | 0.002 (1) | −0.001 (2) | −0.001 (1) |
C4 | 0.057 (1) | 0.043 (1) | 0.060 (1) | 0.002 (1) | 0.003 (2) | 0.0021 (10) |
C5 | 0.055 (1) | 0.0394 (9) | 0.060 (1) | 0.002 (1) | 0.000 (2) | 0.001 (1) |
C6 | 0.053 (1) | 0.0409 (10) | 0.061 (1) | 0.000 (1) | 0.003 (2) | 0.0032 (9) |
C7 | 0.053 (1) | 0.0402 (10) | 0.062 (1) | 0.002 (1) | 0.000 (2) | 0.002 (1) |
C8 | 0.052 (1) | 0.0389 (10) | 0.064 (1) | 0.002 (1) | 0.004 (2) | 0.0025 (9) |
C9 | 0.053 (1) | 0.0408 (10) | 0.063 (1) | 0.002 (1) | 0.002 (2) | 0.001 (1) |
C10 | 0.053 (1) | 0.0382 (9) | 0.062 (1) | 0.002 (1) | 0.002 (1) | 0.0003 (10) |
C11 | 0.052 (1) | 0.0399 (9) | 0.061 (1) | 0.003 (1) | 0.002 (1) | 0.001 (1) |
C12 | 0.052 (1) | 0.0391 (9) | 0.061 (1) | 0.001 (1) | 0.001 (2) | 0.0016 (9) |
C13 | 0.052 (1) | 0.0391 (9) | 0.062 (1) | 0.002 (1) | 0.003 (2) | −0.001 (1) |
C14 | 0.054 (1) | 0.0383 (10) | 0.061 (1) | −0.001 (1) | 0.001 (2) | 0.0011 (9) |
C15 | 0.053 (1) | 0.0403 (10) | 0.062 (1) | 0.002 (1) | 0.004 (2) | −0.001 (1) |
C16 | 0.055 (1) | 0.0385 (9) | 0.063 (1) | −0.002 (1) | 0.002 (2) | −0.0008 (9) |
C17 | 0.056 (1) | 0.0398 (9) | 0.064 (1) | 0.003 (1) | 0.001 (2) | −0.003 (1) |
C18 | 0.060 (1) | 0.0379 (9) | 0.068 (2) | 0.001 (1) | 0.004 (2) | −0.0013 (10) |
C19 | 0.064 (2) | 0.0375 (9) | 0.077 (2) | 0.000 (1) | 0.005 (2) | 0.001 (1) |
O1—C1 | 1.424 (3) | C9—C10 | 1.518 (3) |
O2—C19 | 1.423 (3) | C10—C11 | 1.516 (3) |
C1—C2 | 1.498 (3) | C11—C12 | 1.518 (3) |
C2—C3 | 1.515 (3) | C12—C13 | 1.520 (3) |
C3—C4 | 1.513 (3) | C13—C14 | 1.516 (3) |
C4—C5 | 1.514 (3) | C14—C15 | 1.521 (3) |
C5—C6 | 1.515 (3) | C15—C16 | 1.516 (3) |
C6—C7 | 1.514 (3) | C16—C17 | 1.519 (3) |
C7—C8 | 1.516 (3) | C17—C18 | 1.518 (3) |
C8—C9 | 1.516 (3) | C18—C19 | 1.506 (3) |
O1—C1—C2 | 112.5 (2) | C10—C11—C12 | 113.8 (2) |
C1—C2—C3 | 115.3 (2) | C11—C12—C13 | 114.0 (2) |
C2—C3—C4 | 112.9 (2) | C12—C13—C14 | 113.6 (2) |
C3—C4—C5 | 114.9 (2) | C13—C14—C15 | 114.4 (2) |
C4—C5—C6 | 113.8 (2) | C14—C15—C16 | 113.6 (2) |
C5—C6—C7 | 114.6 (2) | C15—C16—C17 | 114.8 (2) |
C6—C7—C8 | 114.0 (2) | C16—C17—C18 | 112.5 (2) |
C7—C8—C9 | 114.2 (2) | C17—C18—C19 | 113.9 (2) |
C8—C9—C10 | 113.8 (2) | O2—C19—C18 | 108.5 (2) |
C9—C10—C11 | 114.2 (2) | ||
O1—C1—C2—C3 | −63.2 (4) | O2—C19—C18—C17 | 179.4 (2) |