Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768101013234/an0583sup1.cif | |
Portable Document Format (PDF) file https://doi.org/10.1107/S0108768101013234/an0583sup2.pdf |
CCDC references: 174982; 174983
For both compounds, data collection: MSC/AFC, Diffractometer Control Software (Molecular Structure Corporation, 1992); cell refinement: MSC/AFC, Diffractometer Control Software (Molecular Structure Corporation, 1992); data reduction: TEXSAN, (Molecular Structure Corporation, 1992); program(s) used to solve structure: SIR92 (Altomare et al. 1994); program(s) used to refine structure: SHELXL93 (Sheldrick, 1993); molecular graphics: SHELXTL (Siemens, 1994); software used to prepare material for publication: SHELXL93 (Sheldrick, 1993).
C26H45NO2·C2H3N | Dx = 1.091 Mg m−3 |
Mr = 444.68 | Mo Kα radiation, λ = 0.71069 Å |
Orthorhombic, P212121 | Cell parameters from 21 reflections |
a = 13.384 (2) Å | θ = 17–20° |
b = 17.452 (3) Å | µ = 0.07 mm−1 |
c = 11.596 (3) Å | T = 293 K |
V = 2708.4 (10) Å3 | Irregular block, colorless |
Z = 4 | 0.75 × 0.60 × 0.55 mm |
F(000) = 984 |
Rigaku AFC-7S diffractometer | 1881 reflections with I > 2σ(I) |
Radiation source: normal focus sealed tube | Rint = 0.000 |
Graphite monochromator | θmax = 25.0°, θmin = 2.1° |
ω–2θ scans | h = 0→15 |
Absorption correction: ψ scan (North, Phillips & Mathews, 1968)' | k = 0→20 |
Tmin = 0.943, Tmax = 0.971 | l = 0→13 |
2689 measured reflections | 3 standard reflections every 150 reflections |
2689 independent reflections | intensity decay: 4% |
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)] = 0.055 | See text |
wR(F2) = 0.141 | w = 1/[σ2(Fo2) + (0.1144P)2] P = (Fo2 + 2Fc2)/3 |
S = 0.96 | (Δ/σ)max = 0.025 |
2468 reflections | Δρmax = 0.35 e Å−3 |
290 parameters | Δρmin = −0.18 e Å−3 |
0 restraints | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −3.61 (318) |
C26H45NO2·C2H3N | V = 2708.4 (10) Å3 |
Mr = 444.68 | Z = 4 |
Orthorhombic, P212121 | Mo Kα radiation |
a = 13.384 (2) Å | µ = 0.07 mm−1 |
b = 17.452 (3) Å | T = 293 K |
c = 11.596 (3) Å | 0.75 × 0.60 × 0.55 mm |
Rigaku AFC-7S diffractometer | 1881 reflections with I > 2σ(I) |
Absorption correction: ψ scan (North, Phillips & Mathews, 1968)' | Rint = 0.000 |
Tmin = 0.943, Tmax = 0.971 | 3 standard reflections every 150 reflections |
2689 measured reflections | intensity decay: 4% |
2689 independent reflections |
R[F2 > 2σ(F2)] = 0.055 | See text |
wR(F2) = 0.141 | Δρmax = 0.35 e Å−3 |
S = 0.96 | Δρmin = −0.18 e Å−3 |
2468 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
290 parameters | Absolute structure parameter: −3.61 (318) |
0 restraints |
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 on F2 for ALL reflections except for 221 with very negative F2 or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating -R-factor_obs 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 | 0.1475 (2) | 0.0600 (2) | −0.4845 (3) | 0.0590 (8) | |
H1O | 0.1398 (2) | 0.0881 (2) | −0.5609 (3) | 0.068 (2)* | |
O2 | −0.7357 (2) | −0.0792 (2) | −0.4732 (2) | 0.0547 (8) | |
H2O | −0.7786 (2) | −0.0333 (2) | −0.4765 (2) | 0.068 (2)* | |
N1 | −0.6684 (3) | −0.1572 (2) | −0.1848 (3) | 0.0504 (9) | |
H1N | −0.6007 (3) | −0.1645 (2) | −0.2021 (3) | 0.068 (2)* | |
N2 | −0.4487 (6) | −0.2587 (4) | −0.2113 (6) | 0.127 (2) | |
C1 | −0.1291 (3) | 0.0774 (3) | −0.4100 (4) | 0.0496 (10) | |
H1A | −0.1717 (3) | 0.1220 (3) | −0.4015 (4) | 0.068 (2)* | |
H1B | −0.1286 (3) | 0.0505 (3) | −0.3368 (4) | 0.068 (2)* | |
C2 | −0.0221 (3) | 0.1043 (3) | −0.4373 (4) | 0.0546 (11) | |
H2A | −0.0230 (3) | 0.1366 (3) | −0.5054 (4) | 0.068 (2)* | |
H2B | 0.0029 (3) | 0.1347 (3) | −0.3734 (4) | 0.068 (2)* | |
C3 | 0.0469 (3) | 0.0368 (3) | −0.4576 (4) | 0.0553 (11) | |
H3 | 0.0504 (3) | 0.0085 (3) | −0.3857 (4) | 0.068 (2)* | |
C4 | 0.0048 (3) | −0.0172 (2) | −0.5465 (4) | 0.0527 (11) | |
H4A | 0.0480 (3) | −0.0616 (2) | −0.5524 (4) | 0.068 (2)* | |
H4B | 0.0043 (3) | 0.0082 (2) | −0.6209 (4) | 0.068 (2)* | |
C5 | −0.1007 (3) | −0.0436 (2) | −0.5180 (4) | 0.0479 (10) | |
H5 | −0.0965 (3) | −0.0688 (2) | −0.4436 (4) | 0.068 (2)* | |
C6 | −0.1392 (3) | −0.1031 (2) | −0.6018 (5) | 0.0602 (13) | |
H6A | −0.0908 (3) | −0.1442 (2) | −0.6088 (5) | 0.068 (2)* | |
H6B | −0.1480 (3) | −0.0801 (2) | −0.6773 (5) | 0.068 (2)* | |
C7 | −0.2383 (3) | −0.1355 (2) | −0.5591 (4) | 0.0598 (12) | |
H7A | −0.2638 (3) | −0.1709 (2) | −0.6164 (4) | 0.068 (2)* | |
H7B | −0.2274 (3) | −0.1639 (2) | −0.4883 (4) | 0.068 (2)* | |
C8 | −0.3166 (3) | −0.0735 (2) | −0.5382 (3) | 0.0444 (10) | |
H8 | −0.3361 (3) | −0.0523 (2) | −0.6121 (3) | 0.068 (2)* | |
C9 | −0.2754 (3) | −0.0080 (2) | −0.4623 (3) | 0.0404 (9) | |
H9 | −0.2631 (3) | −0.0305 (2) | −0.3871 (3) | 0.068 (2)* | |
C10 | −0.1744 (3) | 0.0246 (2) | −0.5022 (3) | 0.0413 (9) | |
C11 | −0.3575 (3) | 0.0517 (2) | −0.4435 (4) | 0.0469 (10) | |
H11A | −0.3735 (3) | 0.0755 (2) | −0.5168 (4) | 0.068 (2)* | |
H11B | −0.3321 (3) | 0.0913 (2) | −0.3926 (4) | 0.068 (2)* | |
C12 | −0.4533 (3) | 0.0187 (2) | −0.3918 (4) | 0.0452 (10) | |
H12A | −0.4395 (3) | 0.0010 (2) | −0.3141 (4) | 0.068 (2)* | |
H12B | −0.5033 (3) | 0.0588 (2) | −0.3869 (4) | 0.068 (2)* | |
C13 | −0.4958 (3) | −0.0484 (2) | −0.4622 (3) | 0.0392 (9) | |
C14 | −0.4093 (3) | −0.1057 (2) | −0.4802 (3) | 0.0411 (9) | |
H14 | −0.3884 (3) | −0.1204 (2) | −0.4032 (3) | 0.068 (2)* | |
C15 | −0.4610 (3) | −0.1766 (2) | −0.5301 (4) | 0.0546 (11) | |
H15A | −0.4226 (3) | −0.2227 (2) | −0.5153 (4) | 0.068 (2)* | |
H15B | −0.4710 (3) | −0.1713 (2) | −0.6125 (4) | 0.068 (2)* | |
C16 | −0.5619 (3) | −0.1786 (2) | −0.4660 (4) | 0.0527 (11) | |
H16A | −0.5643 (3) | −0.2221 (2) | −0.4139 (4) | 0.068 (2)* | |
H16B | −0.6167 (3) | −0.1827 (2) | −0.5203 (4) | 0.068 (2)* | |
C17 | −0.5690 (3) | −0.1025 (2) | −0.3977 (3) | 0.0393 (9) | |
H17 | −0.5372 (3) | −0.1130 (2) | −0.3242 (3) | 0.068 (2)* | |
C18 | −0.5394 (4) | −0.0190 (3) | −0.5754 (4) | 0.0570 (12) | |
H18A | −0.5656 (4) | −0.0618 (3) | −0.6193 (4) | 0.068 (2)* | |
H18B | −0.4875 (4) | 0.0064 (3) | −0.6195 (4) | 0.068 (2)* | |
H18C | −0.5928 (4) | 0.0171 (3) | −0.5595 (4) | 0.068 (2)* | |
C19 | −0.1878 (3) | 0.0704 (2) | −0.6148 (4) | 0.0527 (11) | |
H19A | −0.1237 (3) | 0.0906 (2) | −0.6392 (4) | 0.068 (2)* | |
H19B | −0.2339 (3) | 0.1124 (2) | −0.6015 (4) | 0.068 (2)* | |
H19C | −0.2143 (3) | 0.0371 (2) | −0.6745 (4) | 0.068 (2)* | |
C20 | −0.6774 (3) | −0.0803 (2) | −0.3680 (3) | 0.0423 (9) | |
C21 | −0.6838 (3) | −0.0023 (2) | −0.3088 (4) | 0.0474 (10) | |
H21A | −0.7531 (3) | 0.0093 (2) | −0.2915 (4) | 0.068 (2)* | |
H21B | −0.6569 (3) | 0.0368 (2) | −0.3596 (4) | 0.068 (2)* | |
H21C | −0.6455 (3) | −0.0034 (2) | −0.2378 (4) | 0.068 (2)* | |
C22 | −0.7247 (3) | −0.1440 (2) | −0.2918 (4) | 0.0476 (10) | |
H22 | −0.7230 (3) | −0.1911 (2) | −0.3361 (4) | 0.068 (2)* | |
C23 | −0.8346 (3) | −0.1280 (3) | −0.2627 (4) | 0.0616 (13) | |
H23A | −0.8729 (3) | −0.1236 (3) | −0.3334 (4) | 0.068 (2)* | |
H23B | −0.8389 (3) | −0.0794 (3) | −0.2223 (4) | 0.068 (2)* | |
C24 | −0.8802 (4) | −0.1911 (3) | −0.1865 (5) | 0.0716 (15) | |
H24A | −0.9467 (4) | −0.1760 (3) | −0.1623 (5) | 0.068 (2)* | |
H24B | −0.8856 (4) | −0.2382 (3) | −0.2304 (5) | 0.068 (2)* | |
C25 | −0.8152 (4) | −0.2038 (3) | −0.0807 (5) | 0.0718 (15) | |
H25A | −0.8160 (4) | −0.1584 (3) | −0.0324 (5) | 0.068 (2)* | |
H25B | −0.8417 (4) | −0.2462 (3) | −0.0360 (5) | 0.068 (2)* | |
C26 | −0.7076 (4) | −0.2214 (3) | −0.1162 (4) | 0.0662 (13) | |
H26A | −0.6667 (4) | −0.2293 (3) | −0.0482 (4) | 0.068 (2)* | |
H26B | −0.7062 (4) | −0.2680 (3) | −0.1617 (4) | 0.068 (2)* | |
C27 | −0.3754 (6) | −0.2792 (4) | −0.2413 (6) | 0.085 (2) | |
C28 | −0.2775 (7) | −0.3019 (4) | −0.2731 (8) | 0.147 (4) | |
H28A | −0.2797 (7) | −0.3297 (4) | −0.3455 (8) | 0.068 (2)* | |
H28B | −0.2508 (7) | −0.3348 (4) | −0.2132 (8) | 0.068 (2)* | |
H28C | −0.2350 (7) | −0.2572 (4) | −0.2816 (8) | 0.068 (2)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
O1 | 0.044 (2) | 0.073 (2) | 0.061 (2) | 0.0032 (15) | −0.0048 (14) | 0.010 (2) |
O2 | 0.053 (2) | 0.062 (2) | 0.049 (2) | 0.0080 (15) | −0.0137 (14) | −0.0088 (15) |
N1 | 0.050 (2) | 0.049 (2) | 0.052 (2) | −0.002 (2) | 0.008 (2) | 0.003 (2) |
N2 | 0.142 (6) | 0.135 (5) | 0.104 (4) | 0.022 (5) | −0.028 (5) | −0.012 (4) |
C1 | 0.050 (2) | 0.048 (2) | 0.050 (2) | 0.000 (2) | 0.003 (2) | −0.006 (2) |
C2 | 0.048 (3) | 0.057 (3) | 0.058 (3) | −0.004 (2) | 0.006 (2) | −0.008 (2) |
C3 | 0.050 (2) | 0.062 (3) | 0.054 (3) | 0.003 (2) | 0.002 (2) | 0.014 (2) |
C4 | 0.048 (2) | 0.051 (2) | 0.059 (3) | 0.011 (2) | 0.014 (2) | 0.010 (2) |
C5 | 0.050 (2) | 0.043 (2) | 0.051 (2) | 0.004 (2) | 0.009 (2) | 0.004 (2) |
C6 | 0.059 (3) | 0.043 (2) | 0.079 (3) | 0.002 (2) | 0.023 (3) | −0.009 (2) |
C7 | 0.067 (3) | 0.036 (2) | 0.076 (3) | 0.000 (2) | 0.019 (3) | −0.013 (2) |
C8 | 0.055 (2) | 0.038 (2) | 0.040 (2) | −0.001 (2) | 0.011 (2) | −0.004 (2) |
C9 | 0.049 (2) | 0.036 (2) | 0.037 (2) | 0.004 (2) | 0.003 (2) | 0.003 (2) |
C10 | 0.048 (2) | 0.038 (2) | 0.038 (2) | 0.003 (2) | 0.007 (2) | 0.002 (2) |
C11 | 0.052 (2) | 0.033 (2) | 0.056 (3) | −0.002 (2) | 0.007 (2) | −0.005 (2) |
C12 | 0.046 (2) | 0.036 (2) | 0.054 (2) | 0.002 (2) | 0.006 (2) | −0.008 (2) |
C13 | 0.047 (2) | 0.037 (2) | 0.034 (2) | 0.006 (2) | 0.002 (2) | 0.001 (2) |
C14 | 0.050 (2) | 0.033 (2) | 0.039 (2) | −0.001 (2) | 0.007 (2) | −0.001 (2) |
C15 | 0.063 (3) | 0.042 (2) | 0.059 (3) | −0.001 (2) | 0.006 (2) | −0.013 (2) |
C16 | 0.050 (2) | 0.044 (2) | 0.065 (3) | −0.004 (2) | 0.001 (2) | −0.015 (2) |
C17 | 0.045 (2) | 0.035 (2) | 0.038 (2) | −0.002 (2) | −0.003 (2) | −0.003 (2) |
C18 | 0.062 (3) | 0.062 (3) | 0.047 (2) | 0.004 (2) | −0.004 (2) | 0.013 (2) |
C19 | 0.055 (2) | 0.053 (2) | 0.051 (2) | 0.000 (2) | 0.005 (2) | 0.008 (2) |
C20 | 0.038 (2) | 0.044 (2) | 0.046 (2) | 0.003 (2) | −0.004 (2) | −0.007 (2) |
C21 | 0.047 (2) | 0.043 (2) | 0.052 (2) | 0.006 (2) | −0.005 (2) | −0.002 (2) |
C22 | 0.046 (2) | 0.044 (2) | 0.052 (2) | 0.000 (2) | 0.003 (2) | −0.011 (2) |
C23 | 0.044 (2) | 0.073 (3) | 0.069 (3) | −0.001 (2) | 0.007 (2) | −0.010 (3) |
C24 | 0.056 (3) | 0.069 (3) | 0.091 (4) | −0.016 (3) | 0.021 (3) | −0.009 (3) |
C25 | 0.089 (4) | 0.055 (3) | 0.071 (3) | −0.020 (3) | 0.029 (3) | −0.005 (3) |
C26 | 0.091 (4) | 0.047 (2) | 0.061 (3) | −0.009 (3) | 0.012 (3) | 0.002 (2) |
C27 | 0.106 (5) | 0.081 (4) | 0.067 (4) | 0.019 (4) | 0.007 (4) | 0.008 (3) |
C28 | 0.209 (10) | 0.090 (5) | 0.144 (7) | −0.003 (6) | 0.065 (7) | 0.022 (5) |
O1—C3 | 1.439 (5) | C10—C19 | 1.542 (5) |
O2—C20 | 1.448 (5) | C11—C12 | 1.528 (5) |
N1—C22 | 1.470 (6) | C12—C13 | 1.537 (5) |
N1—C26 | 1.471 (5) | C13—C18 | 1.526 (5) |
N2—C27 | 1.101 (9) | C13—C14 | 1.543 (5) |
C1—C2 | 1.540 (6) | C13—C17 | 1.554 (5) |
C1—C10 | 1.536 (6) | C14—C15 | 1.531 (5) |
C2—C3 | 1.516 (6) | C15—C16 | 1.541 (6) |
C3—C4 | 1.506 (6) | C16—C17 | 1.548 (5) |
C4—C5 | 1.522 (6) | C17—C20 | 1.541 (5) |
C5—C6 | 1.512 (6) | C20—C21 | 1.526 (5) |
C5—C10 | 1.556 (5) | C20—C22 | 1.554 (6) |
C6—C7 | 1.524 (6) | C22—C23 | 1.534 (6) |
C7—C8 | 1.525 (6) | C23—C24 | 1.538 (7) |
C8—C14 | 1.519 (5) | C24—C25 | 1.520 (7) |
C8—C9 | 1.545 (5) | C25—C26 | 1.529 (7) |
C9—C11 | 1.529 (5) | C27—C28 | 1.418 (11) |
C9—C10 | 1.538 (6) | ||
C22—N1—C26 | 113.1 (4) | C18—C13—C14 | 112.9 (3) |
C2—C1—C10 | 114.0 (4) | C12—C13—C14 | 106.8 (3) |
C3—C2—C1 | 111.2 (4) | C18—C13—C17 | 112.2 (3) |
O1—C3—C4 | 112.2 (4) | C12—C13—C17 | 116.1 (3) |
O1—C3—C2 | 112.6 (4) | C14—C13—C17 | 98.3 (3) |
C4—C3—C2 | 111.4 (4) | C8—C14—C15 | 120.0 (3) |
C3—C4—C5 | 112.9 (4) | C8—C14—C13 | 115.7 (3) |
C6—C5—C4 | 112.7 (3) | C15—C14—C13 | 103.6 (3) |
C6—C5—C10 | 112.6 (3) | C14—C15—C16 | 103.4 (3) |
C4—C5—C10 | 112.4 (3) | C15—C16—C17 | 106.3 (3) |
C5—C6—C7 | 110.0 (4) | C20—C17—C16 | 112.9 (3) |
C8—C7—C6 | 112.7 (3) | C20—C17—C13 | 123.3 (3) |
C7—C8—C14 | 111.7 (3) | C16—C17—C13 | 103.6 (3) |
C7—C8—C9 | 111.8 (3) | O2—C20—C21 | 109.7 (3) |
C14—C8—C9 | 108.2 (3) | O2—C20—C17 | 108.8 (3) |
C11—C9—C8 | 109.2 (3) | C21—C20—C17 | 112.2 (3) |
C11—C9—C10 | 115.0 (3) | O2—C20—C22 | 105.6 (3) |
C8—C9—C10 | 114.5 (3) | C21—C20—C22 | 111.0 (3) |
C9—C10—C1 | 111.0 (3) | C17—C20—C22 | 109.3 (3) |
C9—C10—C19 | 110.1 (3) | N1—C22—C23 | 109.5 (4) |
C1—C10—C19 | 108.9 (3) | N1—C22—C20 | 112.5 (3) |
C9—C10—C5 | 108.1 (3) | C23—C22—C20 | 112.7 (4) |
C1—C10—C5 | 106.9 (3) | C22—C23—C24 | 112.2 (4) |
C19—C10—C5 | 111.7 (3) | C25—C24—C23 | 110.0 (4) |
C9—C11—C12 | 113.7 (3) | C26—C25—C24 | 110.5 (4) |
C11—C12—C13 | 112.9 (3) | N1—C26—C25 | 109.3 (4) |
C18—C13—C12 | 110.0 (3) | N2—C27—C28 | 175.4 (9) |
C27H47NO2 | F(000) = 464 |
Mr = 417.66 | Dx = 1.136 Mg m−3 |
Monoclinic, P21 | Mo Kα radiation, λ = 0.71069 Å |
a = 10.478 (3) Å | Cell parameters from 25 reflections |
b = 7.213 (2) Å | θ = 16–20° |
c = 16.384 (2) Å | µ = 0.07 mm−1 |
β = 99.58 (2)° | T = 293 K |
V = 1220.9 (6) Å3 | Needle, colorless |
Z = 2 | 0.67 × 0.30 × 0.12 mm |
Rigaku AFC-7S diffractometer | 3385 reflections with I > 2σ(I) |
Radiation source: normal focus sealed tube | Rint = 0.022 |
Graphite monochromator | θmax = 25.0°, θmin = 2.2° |
ω–2θ scans | h = 0→12 |
Absorption correction: ψ scan (North, Phillips & Mathews, 1968)' | k = −8→8 |
Tmin = 0.96, Tmax = 1.00 | l = −19→19 |
4569 measured reflections | 3 standard reflections every 150 reflections |
4306 independent reflections | intensity decay: 0.7% |
Refinement on F2 | Hydrogen site location: inferred from neighbouring sites |
Least-squares matrix: full | See text |
R[F2 > 2σ(F2)] = 0.047 | w = 1/[σ2(Fo2) + (0.0737P)2 + 0.1251P] P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.116 | (Δ/σ)max = 0.031 |
S = 0.99 | Δρmax = 0.13 e Å−3 |
4078 reflections | Δρmin = −0.14 e Å−3 |
274 parameters | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
1 restraint | Extinction coefficient: 0.0233 (39) |
Primary atom site location: structure-invariant direct methods | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
Secondary atom site location: difference Fourier map | Absolute structure parameter: 0.16 (205) |
C27H47NO2 | V = 1220.9 (6) Å3 |
Mr = 417.66 | Z = 2 |
Monoclinic, P21 | Mo Kα radiation |
a = 10.478 (3) Å | µ = 0.07 mm−1 |
b = 7.213 (2) Å | T = 293 K |
c = 16.384 (2) Å | 0.67 × 0.30 × 0.12 mm |
β = 99.58 (2)° |
Rigaku AFC-7S diffractometer | 3385 reflections with I > 2σ(I) |
Absorption correction: ψ scan (North, Phillips & Mathews, 1968)' | Rint = 0.022 |
Tmin = 0.96, Tmax = 1.00 | 3 standard reflections every 150 reflections |
4569 measured reflections | intensity decay: 0.7% |
4306 independent reflections |
R[F2 > 2σ(F2)] = 0.047 | See text |
wR(F2) = 0.116 | Δρmax = 0.13 e Å−3 |
S = 0.99 | Δρmin = −0.14 e Å−3 |
4078 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
274 parameters | Absolute structure parameter: 0.16 (205) |
1 restraint |
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 on F2 for ALL reflections except for 228 with very negative F2 or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating -R-factor_obs 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 | 0.8422 (2) | 0.0229 (4) | 0.30124 (13) | 0.0908 (8) | |
H1 | 0.814 (3) | −0.061 (4) | 0.2694 (16) | 0.136* | |
O2 | 0.4859 (2) | 0.0978 (5) | 0.96198 (11) | 0.1007 (9) | |
H2 | 0.529 (3) | 0.002 (3) | 0.9678 (16) | 0.151* | |
N1 | 0.1765 (2) | 0.2471 (3) | 0.83192 (12) | 0.0553 (6) | |
C1 | 0.6823 (2) | −0.1231 (3) | 0.48184 (14) | 0.0467 (6) | |
H1A | 0.6794 (2) | −0.2419 (3) | 0.50926 (14) | 0.056* | |
H1B | 0.5941 (2) | −0.0878 (3) | 0.45948 (14) | 0.056* | |
C2 | 0.7585 (2) | −0.1445 (4) | 0.4108 (2) | 0.0570 (7) | |
H2A | 0.8450 (2) | −0.1884 (4) | 0.4324 (2) | 0.068* | |
H2B | 0.7166 (2) | −0.2365 (4) | 0.3721 (2) | 0.068* | |
C3 | 0.7672 (3) | 0.0349 (4) | 0.36631 (15) | 0.0608 (7) | |
H3 | 0.6794 (3) | 0.0750 (4) | 0.34266 (15) | 0.073* | |
C4 | 0.8286 (3) | 0.1817 (4) | 0.4259 (2) | 0.0561 (7) | |
H4A | 0.8288 (3) | 0.2989 (4) | 0.3969 (2) | 0.067* | |
H4B | 0.9177 (3) | 0.1479 (4) | 0.4464 (2) | 0.067* | |
C5 | 0.7564 (2) | 0.2053 (3) | 0.49912 (15) | 0.0446 (6) | |
H5 | 0.6686 (2) | 0.2446 (3) | 0.47528 (15) | 0.054* | |
C6 | 0.8111 (2) | 0.3583 (4) | 0.5578 (2) | 0.0530 (6) | |
H6A | 0.8186 (2) | 0.4709 (4) | 0.5266 (2) | 0.064* | |
H6B | 0.8972 (2) | 0.3238 (4) | 0.5851 (2) | 0.064* | |
C7 | 0.7253 (2) | 0.3956 (3) | 0.6232 (2) | 0.0534 (6) | |
H7A | 0.7685 (2) | 0.4838 (3) | 0.6632 (2) | 0.064* | |
H7B | 0.6448 (2) | 0.4513 (3) | 0.5966 (2) | 0.064* | |
C8 | 0.6948 (2) | 0.2213 (3) | 0.66856 (14) | 0.0419 (5) | |
H8 | 0.7739 (2) | 0.1811 (3) | 0.70490 (14) | 0.050* | |
C9 | 0.6477 (2) | 0.0613 (3) | 0.60816 (13) | 0.0376 (5) | |
H9 | 0.5671 (2) | 0.1054 (3) | 0.57476 (13) | 0.045* | |
C10 | 0.7406 (2) | 0.0219 (3) | 0.54581 (14) | 0.0380 (5) | |
C11 | 0.6101 (2) | −0.1084 (3) | 0.6548 (2) | 0.0484 (6) | |
H11A | 0.6873 (2) | −0.1588 (3) | 0.6884 (2) | 0.058* | |
H11B | 0.5752 (2) | −0.2026 (3) | 0.6150 (2) | 0.058* | |
C12 | 0.5103 (2) | −0.0653 (3) | 0.71061 (15) | 0.0470 (6) | |
H12A | 0.4293 (2) | −0.0294 (3) | 0.67654 (15) | 0.056* | |
H12B | 0.4946 (2) | −0.1762 (3) | 0.74090 (15) | 0.056* | |
C13 | 0.5559 (2) | 0.0906 (3) | 0.77214 (13) | 0.0427 (6) | |
C14 | 0.5907 (2) | 0.2568 (3) | 0.72159 (14) | 0.0423 (5) | |
H14 | 0.5118 (2) | 0.2856 (3) | 0.68248 (14) | 0.051* | |
C15 | 0.6071 (3) | 0.4156 (4) | 0.7842 (2) | 0.0595 (7) | |
H15A | 0.5968 (3) | 0.5349 (4) | 0.7565 (2) | 0.071* | |
H15B | 0.6913 (3) | 0.4108 (4) | 0.8192 (2) | 0.071* | |
C16 | 0.4982 (3) | 0.3809 (4) | 0.8344 (2) | 0.0636 (7) | |
H16A | 0.4290 (3) | 0.4701 (4) | 0.8193 (2) | 0.076* | |
H16B | 0.5309 (3) | 0.3930 (4) | 0.8931 (2) | 0.076* | |
C17 | 0.4477 (2) | 0.1821 (3) | 0.81437 (14) | 0.0441 (5) | |
H17 | 0.3732 (2) | 0.1965 (3) | 0.76996 (14) | 0.053* | |
C18 | 0.6714 (3) | 0.0263 (5) | 0.8361 (2) | 0.0686 (8) | |
H18A | 0.6987 (3) | 0.1255 (5) | 0.8741 (2) | 0.103* | |
H18B | 0.7416 (3) | −0.0084 (5) | 0.8083 (2) | 0.103* | |
H18C | 0.6463 (3) | −0.0784 (5) | 0.8660 (2) | 0.103* | |
C19 | 0.8720 (2) | −0.0501 (4) | 0.5909 (2) | 0.0524 (6) | |
H19A | 0.9095 (2) | 0.0395 (4) | 0.6312 (2) | 0.079* | |
H19B | 0.9290 (2) | −0.0698 (4) | 0.5514 (2) | 0.079* | |
H19C | 0.8595 (2) | −0.1650 (4) | 0.6181 (2) | 0.079* | |
C20 | 0.3935 (3) | 0.0879 (4) | 0.88575 (14) | 0.0567 (7) | |
C21 | 0.3672 (3) | −0.1179 (5) | 0.8711 (2) | 0.0785 (9) | |
H21A | 0.3336 (3) | −0.1693 (5) | 0.9173 (2) | 0.118* | |
H21B | 0.4463 (3) | −0.1799 (5) | 0.8653 (2) | 0.118* | |
H21C | 0.3051 (3) | −0.1343 (5) | 0.8215 (2) | 0.118* | |
C22 | 0.2735 (2) | 0.1989 (4) | 0.90441 (14) | 0.0528 (6) | |
H22 | 0.3091 (2) | 0.3185 (4) | 0.92555 (14) | 0.063* | |
C23 | 0.2118 (3) | 0.1187 (5) | 0.9751 (2) | 0.0754 (9) | |
H23A | 0.1711 (3) | 0.0010 (5) | 0.9581 (2) | 0.090* | |
H23B | 0.2784 (3) | 0.0965 (5) | 1.0228 (2) | 0.090* | |
C24 | 0.1113 (3) | 0.2511 (5) | 0.9990 (2) | 0.0815 (10) | |
H24A | 0.0701 (3) | 0.1955 (5) | 1.0418 (2) | 0.098* | |
H24B | 0.1530 (3) | 0.3650 (5) | 1.0206 (2) | 0.098* | |
C25 | 0.0117 (3) | 0.2930 (6) | 0.9249 (2) | 0.0858 (11) | |
H25A | −0.0506 (3) | 0.3814 (6) | 0.9395 (2) | 0.103* | |
H25B | −0.0343 (3) | 0.1805 (6) | 0.9053 (2) | 0.103* | |
C26 | 0.0792 (3) | 0.3738 (5) | 0.8566 (2) | 0.0811 (10) | |
H26A | 0.0146 (3) | 0.4014 (5) | 0.8085 (2) | 0.097* | |
H26B | 0.1211 (3) | 0.4892 (5) | 0.8760 (2) | 0.097* | |
C27 | 0.1140 (3) | 0.0935 (6) | 0.7846 (2) | 0.0887 (11) | |
H27A | 0.0529 (3) | 0.1400 (6) | 0.7390 (2) | 0.133* | |
H27B | 0.0696 (3) | 0.0186 (6) | 0.8195 (2) | 0.133* | |
H27C | 0.1779 (3) | 0.0197 (6) | 0.7640 (2) | 0.133* |
U11 | U22 | U33 | U12 | U13 | U23 | |
O1 | 0.095 (2) | 0.122 (2) | 0.0656 (13) | −0.0443 (15) | 0.0427 (12) | −0.0312 (13) |
O2 | 0.0622 (13) | 0.198 (3) | 0.0380 (10) | 0.019 (2) | −0.0024 (9) | 0.0213 (15) |
N1 | 0.0483 (12) | 0.0739 (15) | 0.0458 (11) | 0.0053 (11) | 0.0139 (9) | −0.0047 (11) |
C1 | 0.0434 (12) | 0.0478 (14) | 0.0498 (13) | −0.0058 (11) | 0.0100 (10) | −0.0068 (12) |
C2 | 0.0467 (14) | 0.067 (2) | 0.058 (2) | −0.0087 (13) | 0.0104 (12) | −0.0242 (14) |
C3 | 0.0537 (15) | 0.082 (2) | 0.0479 (14) | −0.0125 (14) | 0.0133 (12) | −0.0049 (14) |
C4 | 0.0505 (14) | 0.065 (2) | 0.056 (2) | −0.0115 (13) | 0.0172 (12) | −0.0028 (13) |
C5 | 0.0342 (11) | 0.0467 (14) | 0.0528 (13) | 0.0012 (10) | 0.0070 (10) | 0.0030 (11) |
C6 | 0.0508 (14) | 0.0453 (14) | 0.068 (2) | −0.0101 (12) | 0.0255 (13) | −0.0054 (13) |
C7 | 0.0509 (14) | 0.0449 (15) | 0.068 (2) | −0.0084 (12) | 0.0201 (12) | −0.0105 (13) |
C8 | 0.0350 (11) | 0.0451 (14) | 0.0460 (13) | −0.0009 (10) | 0.0075 (10) | −0.0038 (10) |
C9 | 0.0319 (11) | 0.0366 (12) | 0.0438 (12) | 0.0037 (9) | 0.0049 (9) | 0.0005 (10) |
C10 | 0.0298 (10) | 0.0410 (12) | 0.0427 (11) | 0.0014 (9) | 0.0042 (9) | −0.0036 (10) |
C11 | 0.0515 (13) | 0.0401 (13) | 0.0562 (14) | 0.0042 (11) | 0.0158 (12) | −0.0011 (12) |
C12 | 0.0538 (14) | 0.0393 (13) | 0.0502 (14) | −0.0002 (11) | 0.0155 (11) | 0.0028 (11) |
C13 | 0.0348 (12) | 0.0535 (14) | 0.0388 (11) | 0.0035 (11) | 0.0031 (10) | 0.0037 (11) |
C14 | 0.0363 (12) | 0.0433 (13) | 0.0469 (12) | −0.0003 (10) | 0.0051 (10) | −0.0076 (11) |
C15 | 0.059 (2) | 0.061 (2) | 0.062 (2) | −0.0114 (13) | 0.0203 (13) | −0.0189 (14) |
C16 | 0.062 (2) | 0.074 (2) | 0.058 (2) | −0.0138 (15) | 0.0211 (13) | −0.0231 (14) |
C17 | 0.0422 (12) | 0.0536 (14) | 0.0357 (11) | 0.0012 (11) | 0.0043 (10) | −0.0011 (11) |
C18 | 0.0510 (15) | 0.095 (2) | 0.057 (2) | 0.0168 (15) | −0.0008 (13) | 0.017 (2) |
C19 | 0.0363 (12) | 0.062 (2) | 0.0579 (15) | 0.0116 (11) | 0.0036 (11) | −0.0086 (13) |
C20 | 0.0573 (15) | 0.083 (2) | 0.0294 (11) | 0.0073 (14) | 0.0059 (11) | 0.0108 (13) |
C21 | 0.094 (2) | 0.068 (2) | 0.082 (2) | 0.018 (2) | 0.042 (2) | 0.031 (2) |
C22 | 0.0539 (14) | 0.070 (2) | 0.0360 (12) | −0.0091 (13) | 0.0131 (11) | −0.0091 (12) |
C23 | 0.084 (2) | 0.102 (2) | 0.0465 (15) | −0.006 (2) | 0.0296 (15) | 0.001 (2) |
C24 | 0.093 (2) | 0.098 (2) | 0.066 (2) | −0.021 (2) | 0.048 (2) | −0.022 (2) |
C25 | 0.074 (2) | 0.101 (3) | 0.095 (2) | −0.003 (2) | 0.048 (2) | −0.019 (2) |
C26 | 0.071 (2) | 0.101 (3) | 0.080 (2) | 0.019 (2) | 0.037 (2) | 0.003 (2) |
C27 | 0.066 (2) | 0.130 (3) | 0.068 (2) | −0.015 (2) | 0.004 (2) | −0.035 (2) |
O1—C3 | 1.429 (3) | C13—C18 | 1.535 (3) |
O1—H1 | 0.82 | C13—C14 | 1.535 (3) |
O2—C20 | 1.449 (3) | C13—C17 | 1.568 (3) |
O2—H2 | 0.82 | C14—C15 | 1.528 (3) |
N1—C27 | 1.445 (4) | C14—H14 | 0.98 |
N1—C22 | 1.471 (3) | C15—C16 | 1.533 (4) |
N1—C26 | 1.475 (4) | C15—H15A | 0.97 |
C1—C2 | 1.525 (3) | C15—H15B | 0.97 |
C1—C10 | 1.534 (3) | C16—C17 | 1.544 (4) |
C1—H1A | 0.97 | C16—H16A | 0.97 |
C1—H1B | 0.97 | C16—H16B | 0.97 |
C2—C3 | 1.495 (4) | C17—C20 | 1.540 (3) |
C2—H2A | 0.97 | C17—H17 | 0.98 |
C2—H2B | 0.97 | C18—H18A | 0.96 |
C3—C4 | 1.510 (4) | C18—H18B | 0.96 |
C3—H3 | 0.98 | C18—H18C | 0.96 |
C4—C5 | 1.529 (3) | C19—H19A | 0.96 |
C4—H4A | 0.97 | C19—H19B | 0.96 |
C4—H4B | 0.97 | C19—H19C | 0.96 |
C5—C6 | 1.513 (3) | C20—C21 | 1.522 (5) |
C5—C10 | 1.551 (3) | C20—C22 | 1.563 (4) |
C5—H5 | 0.98 | C21—H21A | 0.96 |
C6—C7 | 1.533 (3) | C21—H21B | 0.96 |
C6—H6A | 0.97 | C21—H21C | 0.96 |
C6—H6B | 0.97 | C22—C23 | 1.532 (4) |
C7—C8 | 1.521 (3) | C22—H22 | 0.98 |
C7—H7A | 0.97 | C23—C24 | 1.520 (5) |
C7—H7B | 0.97 | C23—H23A | 0.97 |
C8—C14 | 1.525 (3) | C23—H23B | 0.97 |
C8—C9 | 1.546 (3) | C24—C25 | 1.494 (5) |
C8—H8 | 0.98 | C24—H24A | 0.97 |
C9—C11 | 1.529 (3) | C24—H24B | 0.97 |
C9—C10 | 1.550 (3) | C25—C26 | 1.535 (5) |
C9—H9 | 0.98 | C25—H25A | 0.97 |
C10—C19 | 1.540 (3) | C25—H25B | 0.97 |
C11—C12 | 1.531 (3) | C26—H26A | 0.97 |
C11—H11A | 0.97 | C26—H26B | 0.97 |
C11—H11B | 0.97 | C27—H27A | 0.96 |
C12—C13 | 1.533 (3) | C27—H27B | 0.96 |
C12—H12A | 0.97 | C27—H27C | 0.96 |
C12—H12B | 0.97 | ||
C3—O1—H1 | 109.47 (14) | C15—C14—C13 | 103.5 (2) |
C20—O2—H2 | 109.5 (2) | C8—C14—C13 | 115.7 (2) |
C27—N1—C22 | 116.3 (2) | C15—C14—H14 | 105.56 (14) |
C27—N1—C26 | 110.5 (2) | C8—C14—H14 | 105.56 (12) |
C22—N1—C26 | 110.0 (2) | C13—C14—H14 | 105.56 (12) |
C2—C1—C10 | 113.0 (2) | C14—C15—C16 | 103.1 (2) |
C2—C1—H1A | 108.98 (15) | C14—C15—H15A | 111.14 (14) |
C10—C1—H1A | 108.98 (13) | C16—C15—H15A | 111.1 (2) |
C2—C1—H1B | 108.98 (13) | C14—C15—H15B | 111.14 (14) |
C10—C1—H1B | 108.98 (12) | C16—C15—H15B | 111.1 (2) |
H1A—C1—H1B | 107.8 | H15A—C15—H15B | 109.1 |
C3—C2—C1 | 111.5 (2) | C15—C16—C17 | 107.3 (2) |
C3—C2—H2A | 109.32 (15) | C15—C16—H16A | 110.3 (2) |
C1—C2—H2A | 109.32 (14) | C17—C16—H16A | 110.26 (14) |
C3—C2—H2B | 109.32 (14) | C15—C16—H16B | 110.26 (14) |
C1—C2—H2B | 109.32 (13) | C17—C16—H16B | 110.26 (14) |
H2A—C2—H2B | 108.0 | H16A—C16—H16B | 108.5 |
O1—C3—C2 | 113.4 (3) | C20—C17—C16 | 113.9 (2) |
O1—C3—C4 | 107.3 (2) | C20—C17—C13 | 122.3 (2) |
C2—C3—C4 | 110.2 (2) | C16—C17—C13 | 103.7 (2) |
O1—C3—H3 | 108.6 (2) | C20—C17—H17 | 105.18 (13) |
C2—C3—H3 | 108.61 (15) | C16—C17—H17 | 105.18 (15) |
C4—C3—H3 | 108.6 (2) | C13—C17—H17 | 105.18 (11) |
C3—C4—C5 | 111.8 (2) | C13—C18—H18A | 109.5 (2) |
C3—C4—H4A | 109.25 (15) | C13—C18—H18B | 109.47 (14) |
C5—C4—H4A | 109.25 (14) | H18A—C18—H18B | 109.5 |
C3—C4—H4B | 109.2 (2) | C13—C18—H18C | 109.47 (15) |
C5—C4—H4B | 109.25 (13) | H18A—C18—H18C | 109.5 |
H4A—C4—H4B | 107.9 | H18B—C18—H18C | 109.5 |
C6—C5—C4 | 113.3 (2) | C10—C19—H19A | 109.47 (13) |
C6—C5—C10 | 111.7 (2) | C10—C19—H19B | 109.47 (12) |
C4—C5—C10 | 113.5 (2) | H19A—C19—H19B | 109.5 |
C6—C5—H5 | 105.86 (13) | C10—C19—H19C | 109.47 (13) |
C4—C5—H5 | 105.86 (13) | H19A—C19—H19C | 109.5 |
C10—C5—H5 | 105.86 (11) | H19B—C19—H19C | 109.5 |
C5—C6—C7 | 111.6 (2) | O2—C20—C21 | 105.1 (3) |
C5—C6—H6A | 109.30 (14) | O2—C20—C17 | 110.8 (2) |
C7—C6—H6A | 109.30 (14) | C21—C20—C17 | 113.0 (2) |
C5—C6—H6B | 109.30 (13) | O2—C20—C22 | 104.5 (2) |
C7—C6—H6B | 109.30 (14) | C21—C20—C22 | 113.6 (2) |
H6A—C6—H6B | 108.0 | C17—C20—C22 | 109.4 (2) |
C8—C7—C6 | 113.1 (2) | C20—C21—H21A | 109.47 (14) |
C8—C7—H7A | 108.97 (13) | C20—C21—H21B | 109.5 (2) |
C6—C7—H7A | 108.97 (13) | H21A—C21—H21B | 109.5 |
C8—C7—H7B | 108.97 (13) | C20—C21—H21C | 109.5 (2) |
C6—C7—H7B | 108.97 (14) | H21A—C21—H21C | 109.5 |
H7A—C7—H7B | 107.8 | H21B—C21—H21C | 109.5 |
C7—C8—C14 | 111.6 (2) | N1—C22—C23 | 112.2 (2) |
C7—C8—C9 | 112.0 (2) | N1—C22—C20 | 115.7 (2) |
C14—C8—C9 | 107.9 (2) | C23—C22—C20 | 114.2 (2) |
C7—C8—H8 | 108.42 (13) | N1—C22—H22 | 104.40 (14) |
C14—C8—H8 | 108.42 (12) | C23—C22—H22 | 104.4 (2) |
C9—C8—H8 | 108.42 (11) | C20—C22—H22 | 104.40 (15) |
C11—C9—C8 | 111.0 (2) | C24—C23—C22 | 110.8 (3) |
C11—C9—C10 | 115.1 (2) | C24—C23—H23A | 109.5 (2) |
C8—C9—C10 | 113.0 (2) | C22—C23—H23A | 109.5 (2) |
C11—C9—H9 | 105.60 (12) | C24—C23—H23B | 109.5 (2) |
C8—C9—H9 | 105.60 (11) | C22—C23—H23B | 109.5 (2) |
C10—C9—H9 | 105.60 (11) | H23A—C23—H23B | 108.1 |
C1—C10—C19 | 108.7 (2) | C25—C24—C23 | 109.8 (3) |
C1—C10—C9 | 110.7 (2) | C25—C24—H24A | 109.7 (2) |
C19—C10—C9 | 110.8 (2) | C23—C24—H24A | 109.7 (2) |
C1—C10—C5 | 107.9 (2) | C25—C24—H24B | 109.7 (2) |
C19—C10—C5 | 111.3 (2) | C23—C24—H24B | 109.7 (2) |
C9—C10—C5 | 107.4 (2) | H24A—C24—H24B | 108.2 |
C9—C11—C12 | 113.2 (2) | C24—C25—C26 | 108.9 (3) |
C9—C11—H11A | 108.93 (12) | C24—C25—H25A | 109.9 (2) |
C12—C11—H11A | 108.93 (13) | C26—C25—H25A | 109.9 (2) |
C9—C11—H11B | 108.93 (12) | C24—C25—H25B | 109.9 (2) |
C12—C11—H11B | 108.93 (13) | C26—C25—H25B | 109.9 (2) |
H11A—C11—H11B | 107.7 | H25A—C25—H25B | 108.3 |
C13—C12—C11 | 111.9 (2) | N1—C26—C25 | 112.8 (3) |
C13—C12—H12A | 109.24 (12) | N1—C26—H26A | 109.0 (2) |
C11—C12—H12A | 109.24 (13) | C25—C26—H26A | 109.0 (2) |
C13—C12—H12B | 109.24 (12) | N1—C26—H26B | 109.0 (2) |
C11—C12—H12B | 109.24 (13) | C25—C26—H26B | 109.0 (2) |
H12A—C12—H12B | 107.9 | H26A—C26—H26B | 107.8 |
C12—C13—C18 | 110.6 (2) | N1—C27—H27A | 109.5 (2) |
C12—C13—C14 | 107.1 (2) | N1—C27—H27B | 109.5 (2) |
C18—C13—C14 | 111.9 (2) | H27A—C27—H27B | 109.5 |
C12—C13—C17 | 115.5 (2) | N1—C27—H27C | 109.5 (2) |
C18—C13—C17 | 111.8 (2) | H27A—C27—H27C | 109.5 |
C14—C13—C17 | 99.4 (2) | H27B—C27—H27C | 109.5 |
C15—C14—C8 | 119.8 (2) |
Experimental details
(1) | (2) | |
Crystal data | ||
Chemical formula | C26H45NO2·C2H3N | C27H47NO2 |
Mr | 444.68 | 417.66 |
Crystal system, space group | Orthorhombic, P212121 | Monoclinic, P21 |
Temperature (K) | 293 | 293 |
a, b, c (Å) | 13.384 (2), 17.452 (3), 11.596 (3) | 10.478 (3), 7.213 (2), 16.384 (2) |
α, β, γ (°) | 90, 90, 90 | 90, 99.58 (2), 90 |
V (Å3) | 2708.4 (10) | 1220.9 (6) |
Z | 4 | 2 |
Radiation type | Mo Kα | Mo Kα |
µ (mm−1) | 0.07 | 0.07 |
Crystal size (mm) | 0.75 × 0.60 × 0.55 | 0.67 × 0.30 × 0.12 |
Data collection | ||
Diffractometer | Rigaku AFC-7S diffractometer | Rigaku AFC-7S diffractometer |
Absorption correction | ψ scan (North, Phillips & Mathews, 1968)' | ψ scan (North, Phillips & Mathews, 1968)' |
Tmin, Tmax | 0.943, 0.971 | 0.96, 1.00 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 2689, 2689, 1881 | 4569, 4306, 3385 |
Rint | 0.000 | 0.022 |
(sin θ/λ)max (Å−1) | 0.595 | 0.595 |
Refinement | ||
R[F2 > 2σ(F2)], wR(F2), S | 0.055, 0.141, 0.96 | 0.047, 0.116, 0.99 |
No. of reflections | 2468 | 4078 |
No. of parameters | 290 | 274 |
No. of restraints | 0 | 1 |
H-atom treatment | See text | See text |
Δρmax, Δρmin (e Å−3) | 0.35, −0.18 | 0.13, −0.14 |
Absolute structure | Flack H D (1983), Acta Cryst. A39, 876-881 | Flack H D (1983), Acta Cryst. A39, 876-881 |
Absolute structure parameter | −3.61 (318) | 0.16 (205) |
Computer programs: MSC/AFC, Diffractometer Control Software (Molecular Structure Corporation, 1992), TEXSAN, (Molecular Structure Corporation, 1992), SIR92 (Altomare et al. 1994), SHELXL93 (Sheldrick, 1993), SHELXTL (Siemens, 1994).