Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100011288/gg1020sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270100011288/gg1020Isup2.hkl |
CCDC reference: 153917
Data collection: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1992); data reduction: TEXSAN (Molecular Structure Corporation, 1995); program(s) used to solve structure: SAPI91 (Fan, 1991); program(s) used to refine structure: TEXSAN; molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: TEXSAN.
C21H44O2 | Dx = 1.029 Mg m−3 |
Mr = 328.58 | Cu Kα radiation, λ = 1.5418 Å |
Orthorhombic, P212121 | Cell parameters from 24 reflections |
a = 7.247 (4) Å | θ = 9.2–13.9° |
b = 57.940 (3) Å | µ = 0.48 mm−1 |
c = 5.048 (4) Å | T = 296 K |
V = 2119 (1) Å3 | Plate, colourless |
Z = 4 | 0.50 × 0.50 × 0.05 mm |
F(000) = 744 |
Rigaku AFC-5R diffractometer | 1583 reflections with I > 2σ(I) |
Radiation source: Rigaku rotating anode | Rint = 0.022 |
Graphite monochromator | θmax = 70.6°, θmin = 3.1° |
ω scans | h = −2→8 |
Absorption correction: ψ scans (North et al., 1968) | k = 0→70 |
Tmin = 0.825, Tmax = 0.999 | l = −1→6 |
3723 measured reflections | 3 standard reflections every 150 reflections |
2355 independent reflections | intensity decay: 4% |
Refinement on F | 0 restraints |
Least-squares matrix: full | 0 constraints |
R[F2 > 2σ(F2)] = 0.051 | H-atom parameters constrained |
wR(F2) = 0.083 | w = 1/[σ2(Fo) + 0.00106|Fo|2] |
S = 1.67 | (Δ/σ)max < 0.001 |
1583 reflections | Δρmax = 0.11 e Å−3 |
208 parameters | Δρmin = −0.22 e Å−3 |
Experimental. none |
Geometry. none # O···O details from PLATON (Spek, 1998) # O1···O2i 2.778 (5) Å i = -5/2 - x,-y,1/2 + z # O2···O1ii 2.717 (4) Å ii= -2 - x,1/2 + y,-3/2 - z |
Refinement. None |
x | y | z | Uiso*/Ueq | ||
O1 | −1.0589 (4) | −0.23208 (3) | −0.6415 (4) | 0.0747 (6) | |
O2 | −1.0627 (4) | 0.22760 (3) | −1.0705 (5) | 0.0836 (7) | |
C1 | −0.9982 (6) | −0.22978 (4) | −0.9085 (7) | 0.083 (1) | |
C2 | −1.0545 (6) | −0.20709 (4) | −1.0268 (6) | 0.0715 (9) | |
C3 | −0.9661 (5) | −0.18604 (4) | −0.8983 (6) | 0.0595 (8) | |
C4 | −1.0384 (5) | −0.16364 (4) | −1.0119 (6) | 0.0584 (8) | |
C5 | −0.9575 (5) | −0.14210 (4) | −0.8880 (6) | 0.0549 (7) | |
C6 | −1.0361 (5) | −0.11986 (4) | −0.9999 (6) | 0.0559 (8) | |
C7 | −0.9568 (5) | −0.09813 (4) | −0.8779 (6) | 0.0553 (7) | |
C8 | −1.0377 (5) | −0.07600 (4) | −0.9907 (6) | 0.0550 (7) | |
C9 | −0.9586 (4) | −0.05416 (4) | −0.8718 (6) | 0.0537 (7) | |
C10 | −1.0396 (5) | −0.03217 (4) | −0.9865 (6) | 0.0558 (7) | |
C11 | −0.9597 (4) | −0.01026 (4) | −0.8692 (6) | 0.0546 (7) | |
C12 | −1.0395 (4) | 0.01170 (4) | −0.9854 (6) | 0.0541 (7) | |
C13 | −0.9600 (4) | 0.03370 (4) | −0.8694 (6) | 0.0550 (7) | |
C14 | −1.0403 (5) | 0.05562 (4) | −0.9876 (6) | 0.0548 (7) | |
C15 | −0.9608 (5) | 0.07764 (4) | −0.8736 (6) | 0.0555 (7) | |
C16 | −1.0401 (5) | 0.09944 (4) | −0.9947 (6) | 0.0545 (7) | |
C17 | −0.9596 (5) | 0.12167 (4) | −0.8839 (6) | 0.0556 (7) | |
C18 | −1.0404 (5) | 0.14326 (4) | −1.0082 (6) | 0.0564 (7) | |
C19 | −0.9612 (5) | 0.16574 (4) | −0.9042 (6) | 0.0574 (8) | |
C20 | −1.0465 (5) | 0.18680 (4) | −1.0349 (6) | 0.0598 (8) | |
C21 | −0.9723 (5) | 0.20936 (4) | −0.9359 (6) | 0.0653 (9) | |
H1A | −0.8715 | −0.2311 | −0.9209 | 0.0903* | |
H1B | −1.0560 | −0.2417 | −1.0173 | 0.0903* | |
H1O | −1.1937 | −0.2308 | −0.6318 | 0.0898* | |
H2A | −1.0255 | −0.2070 | −1.2098 | 0.0847* | |
H2B | −1.1875 | −0.2056 | −1.0095 | 0.0847* | |
H2O | −1.0137 | 0.2420 | −1.0100 | 0.0948* | |
H3A | −0.9945 | −0.1862 | −0.7134 | 0.0679* | |
H3B | −0.8387 | −0.1867 | −0.9240 | 0.0679* | |
H4A | −1.0101 | −0.1634 | −1.1957 | 0.0701* | |
H4B | −1.1693 | −0.1633 | −0.9902 | 0.0701* | |
H5A | −0.9851 | −0.1424 | −0.7020 | 0.0648* | |
H5B | −0.8296 | −0.1420 | −0.9131 | 0.0648* | |
H6A | −1.0114 | −0.1196 | −1.1843 | 0.0675* | |
H6B | −1.1669 | −0.1199 | −0.9732 | 0.0675* | |
H7A | −0.9847 | −0.0984 | −0.6920 | 0.0650* | |
H7B | −0.8291 | −0.0980 | −0.9031 | 0.0650* | |
H8A | −1.0115 | −0.0758 | −1.1750 | 0.0648* | |
H8B | −1.1667 | −0.0761 | −0.9634 | 0.0648* | |
H9A | −0.9861 | −0.0542 | −0.6867 | 0.0631* | |
H9B | −0.8310 | −0.0539 | −0.8985 | 0.0631* | |
H10A | −1.0156 | −0.0320 | −1.1708 | 0.0658* | |
H10B | −1.1689 | −0.0321 | −0.9565 | 0.0658* | |
H11A | −0.9855 | −0.0101 | −0.6835 | 0.0644* | |
H11B | −0.8311 | −0.0102 | −0.8962 | 0.0644* | |
H12A | −1.0141 | 0.0117 | −1.1698 | 0.0628* | |
H12B | −1.1682 | 0.0117 | −0.9566 | 0.0628* | |
H13A | −0.9843 | 0.0338 | −0.6832 | 0.0658* | |
H13B | −0.8302 | 0.0337 | −0.8965 | 0.0658* | |
H14A | −1.0151 | 0.0555 | −1.1716 | 0.0639* | |
H14B | −1.1684 | 0.0556 | −0.9573 | 0.0639* | |
H15A | −0.9851 | 0.0780 | −0.6874 | 0.0663* | |
H15B | −0.8304 | 0.0777 | −0.8998 | 0.0663* | |
H16A | −1.0151 | 0.0991 | −1.1790 | 0.0642* | |
H16B | −1.1683 | 0.0996 | −0.9644 | 0.0642* | |
H17A | −0.9824 | 0.1223 | −0.6969 | 0.0666* | |
H17B | −0.8287 | 0.1218 | −0.9107 | 0.0666* | |
H18A | −1.0158 | 0.1426 | −1.1934 | 0.0654* | |
H18B | −1.1685 | 0.1433 | −0.9783 | 0.0654* | |
H19A | −0.9837 | 0.1666 | −0.7168 | 0.0704* | |
H19B | −0.8309 | 0.1660 | −0.9318 | 0.0704* | |
H20A | −1.0242 | 0.1857 | −1.2213 | 0.0706* | |
H20B | −1.1756 | 0.1865 | −1.0043 | 0.0706* | |
H21A | −0.8405 | 0.2101 | −0.9723 | 0.0802* | |
H21B | −0.9891 | 0.2107 | −0.7512 | 0.0802* |
U11 | U22 | U33 | U12 | U13 | U23 | |
O1 | 0.110 (2) | 0.0454 (8) | 0.068 (1) | 0.005 (1) | 0.005 (2) | 0.0058 (9) |
O2 | 0.114 (2) | 0.0375 (8) | 0.099 (2) | −0.002 (1) | −0.026 (2) | 0.0017 (9) |
C1 | 0.138 (4) | 0.042 (1) | 0.070 (2) | 0.002 (2) | 0.012 (2) | −0.008 (1) |
C2 | 0.113 (3) | 0.046 (1) | 0.056 (1) | −0.005 (2) | −0.004 (2) | −0.002 (1) |
C3 | 0.080 (2) | 0.040 (1) | 0.059 (1) | −0.001 (1) | 0.001 (2) | 0.000 (1) |
C4 | 0.077 (2) | 0.042 (1) | 0.056 (1) | 0.000 (1) | −0.003 (2) | 0.003 (1) |
C5 | 0.064 (2) | 0.040 (1) | 0.061 (1) | −0.001 (1) | 0.000 (2) | 0.001 (1) |
C6 | 0.068 (2) | 0.041 (1) | 0.059 (1) | 0.000 (1) | −0.001 (2) | 0.003 (1) |
C7 | 0.067 (2) | 0.039 (1) | 0.060 (1) | −0.002 (1) | 0.000 (2) | 0.001 (1) |
C8 | 0.065 (2) | 0.040 (1) | 0.060 (1) | 0.001 (1) | −0.003 (2) | 0.003 (1) |
C9 | 0.062 (2) | 0.039 (1) | 0.060 (1) | −0.002 (1) | −0.002 (2) | 0.002 (1) |
C10 | 0.068 (2) | 0.039 (1) | 0.061 (1) | 0.001 (1) | −0.002 (2) | 0.002 (1) |
C11 | 0.064 (2) | 0.039 (1) | 0.061 (1) | −0.002 (1) | −0.002 (2) | 0.001 (1) |
C12 | 0.064 (2) | 0.038 (1) | 0.060 (1) | 0.001 (1) | −0.003 (2) | 0.001 (1) |
C13 | 0.065 (2) | 0.040 (1) | 0.061 (1) | −0.002 (1) | −0.001 (2) | 0.001 (1) |
C14 | 0.065 (2) | 0.038 (1) | 0.060 (1) | 0.000 (1) | 0.000 (2) | 0.001 (1) |
C15 | 0.066 (2) | 0.039 (1) | 0.061 (1) | −0.001 (1) | −0.002 (2) | −0.001 (1) |
C16 | 0.064 (2) | 0.040 (1) | 0.060 (2) | 0.001 (1) | −0.002 (2) | −0.002 (1) |
C17 | 0.067 (2) | 0.040 (1) | 0.060 (1) | 0.000 (1) | −0.003 (2) | −0.003 (1) |
C18 | 0.069 (2) | 0.039 (1) | 0.061 (1) | 0.003 (1) | −0.003 (2) | −0.001 (1) |
C19 | 0.069 (2) | 0.041 (1) | 0.062 (2) | 0.000 (1) | −0.003 (2) | −0.003 (1) |
C20 | 0.073 (2) | 0.040 (1) | 0.067 (2) | 0.001 (1) | −0.002 (2) | −0.001 (1) |
C21 | 0.082 (3) | 0.039 (1) | 0.075 (2) | 0.002 (1) | −0.001 (2) | 0.000 (1) |
O1—C1 | 1.424 (4) | C10—C11 | 1.516 (4) |
O2—C21 | 1.417 (3) | C11—C12 | 1.516 (3) |
C1—C2 | 1.501 (4) | C12—C13 | 1.516 (3) |
C2—C3 | 1.523 (4) | C13—C14 | 1.519 (3) |
C3—C4 | 1.513 (3) | C14—C15 | 1.513 (3) |
C4—C5 | 1.514 (4) | C15—C16 | 1.516 (3) |
C5—C6 | 1.518 (3) | C16—C17 | 1.520 (3) |
C6—C7 | 1.515 (3) | C17—C18 | 1.517 (3) |
C7—C8 | 1.521 (3) | C18—C19 | 1.517 (3) |
C8—C9 | 1.513 (3) | C19—C20 | 1.519 (4) |
C9—C10 | 1.518 (3) | C20—C21 | 1.499 (3) |
O1—C1—C2 | 112.0 (3) | C11—C12—C13 | 114.2 (2) |
C1—C2—C3 | 114.7 (3) | C12—C13—C14 | 113.9 (2) |
C2—C3—C4 | 112.3 (3) | C13—C14—C15 | 114.2 (3) |
C3—C4—C5 | 114.6 (3) | C14—C15—C16 | 113.9 (3) |
C4—C5—C6 | 113.6 (3) | C15—C16—C17 | 114.3 (3) |
C5—C6—C7 | 114.3 (3) | C16—C17—C18 | 113.5 (3) |
C6—C7—C8 | 113.7 (3) | C17—C18—C19 | 114.8 (3) |
C7—C8—C9 | 114.2 (3) | C18—C19—C20 | 112.7 (3) |
C8—C9—C10 | 113.8 (3) | C19—C20—C21 | 114.2 (3) |
C9—C10—C11 | 113.9 (2) | O2—C21—C20 | 108.9 (3) |
C10—C11—C12 | 113.9 (2) | ||
O1—C1—C2—C3 | 65.1 (5) | O2—C21—C20—C19 | −179.6 (3) |