Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806019209/rz2030sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806019209/rz20303sup2.hkl |
CCDC reference: 610878
Key indicators
- Single-crystal X-ray study
- T = 294 K
- Mean (C-C) = 0.006 Å
- R factor = 0.045
- wR factor = 0.126
- Data-to-parameter ratio = 8.8
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.78 Ratio PLAT222_ALERT_3_B Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.68 Ratio PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for O6 PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for O8 PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C19 PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C22
Alert level C PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ? PLAT230_ALERT_2_C Hirshfeld Test Diff for O6 - C18 .. 6.80 su PLAT340_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 6
Alert level G 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 26.55 From the CIF: _reflns_number_total 2644 Count of symmetry unique reflns 2658 Completeness (_total/calc) 99.47% 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 6 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 6 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997) and PLATON (Spek, 2003); software used to prepare material for publication: SHELXTL.
C24H34O8 | F(000) = 484 |
Mr = 450.51 | Dx = 1.240 Mg m−3 |
Monoclinic, P21 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2yb | Cell parameters from 2420 reflections |
a = 10.288 (4) Å | θ = 2.7–23.4° |
b = 9.992 (3) Å | µ = 0.09 mm−1 |
c = 11.983 (4) Å | T = 294 K |
β = 101.552 (6)° | Block, colourless |
V = 1206.9 (7) Å3 | 0.26 × 0.22 × 0.16 mm |
Z = 2 |
Bruker SMART CCD area-detector diffractometer | 2644 independent reflections |
Radiation source: fine-focus sealed tube | 1831 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.031 |
φ and ω scans | θmax = 26.6°, θmin = 1.7° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −12→12 |
Tmin = 0.976, Tmax = 0.985 | k = −12→5 |
6896 measured reflections | l = −15→14 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.045 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.126 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.02 | w = 1/[σ2(Fo2) + (0.066P)2 + 0.1782P] where P = (Fo2 + 2Fc2)/3 |
2644 reflections | (Δ/σ)max = 0.001 |
300 parameters | Δρmax = 0.31 e Å−3 |
14 restraints | Δρmin = −0.26 e Å−3 |
Experimental. 1H NMR (CDCl3): δ 1.38 (s, 9H), 1.42 (s, 12H), 4.01–4.68 (m, 8H), 5.90 (d, J = 3.9 Hz, 1H), 7.41 (d, J = 2.4 Hz, 1H), 7.48 (d, J = 1.8 Hz, 1H), 9.87 (s, 1H), 1.80 (s, 1H). 13C NMR (CDCl3): δ 197.0, 161.0, 138.6, 133.9, 131.0, 128.3, 120.3, 111.9, 109.1, 105.3, 82.6, 81.6, 81.3, 77.7, 76.7, 72.4, 71.8, 67.5, 34.9, 29.1, 26.9, 26.8, 26.7, 26.2. IR (KBr): ν (cm-1) 3423, 2992, 2969, 2936, 2862, 1655, 1617, 1456, 1440, 1384, 1374, 1321, 1265, 1226, 1212, 1167, 1152, 1081, 1024, 847, 771, 759. |
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 | 0.1023 (3) | 0.2965 (3) | 0.9930 (2) | 0.0679 (8) | |
H1 | 0.015 (4) | 0.301 (6) | 1.000 (5) | 0.099 (17)* | |
O2 | −0.1408 (3) | 0.3831 (4) | 0.9716 (3) | 0.0789 (9) | |
O3 | 0.0917 (2) | 0.7819 (2) | 0.64049 (18) | 0.0503 (6) | |
O4 | −0.0362 (2) | 0.8290 (3) | 0.4037 (2) | 0.0589 (7) | |
O5 | −0.2263 (2) | 0.6466 (3) | 0.5789 (2) | 0.0601 (7) | |
O6 | −0.4041 (3) | 0.7580 (4) | 0.4823 (4) | 0.1014 (13) | |
O7 | 0.1763 (3) | 0.5978 (2) | 0.4034 (2) | 0.0568 (7) | |
O8 | 0.0926 (3) | 0.7598 (3) | 0.2764 (2) | 0.0854 (10) | |
C1 | 0.1675 (3) | 0.6256 (4) | 0.7983 (3) | 0.0467 (8) | |
C2 | 0.2667 (3) | 0.5314 (4) | 0.8375 (3) | 0.0490 (9) | |
H2 | 0.3492 | 0.5445 | 0.8186 | 0.059* | |
C3 | 0.2510 (4) | 0.4192 (4) | 0.9029 (3) | 0.0497 (9) | |
C4 | 0.1250 (4) | 0.4025 (4) | 0.9288 (3) | 0.0491 (8) | |
C5 | 0.0224 (3) | 0.4933 (4) | 0.8886 (3) | 0.0474 (8) | |
C6 | 0.0441 (3) | 0.6033 (4) | 0.8241 (3) | 0.0476 (8) | |
H6 | −0.0250 | 0.6627 | 0.7980 | 0.057* | |
C7 | 0.3643 (4) | 0.3190 (5) | 0.9411 (3) | 0.0656 (11) | |
C8 | 0.3204 (6) | 0.1791 (5) | 0.8930 (5) | 0.0896 (16) | |
H8A | 0.3945 | 0.1189 | 0.9085 | 0.134* | |
H8B | 0.2886 | 0.1853 | 0.8122 | 0.134* | |
H8C | 0.2508 | 0.1462 | 0.9283 | 0.134* | |
C9 | 0.3988 (5) | 0.3144 (7) | 1.0736 (4) | 0.0962 (18) | |
H9A | 0.4318 | 0.4001 | 1.1025 | 0.144* | |
H9B | 0.4653 | 0.2474 | 1.0980 | 0.144* | |
H9C | 0.3205 | 0.2929 | 1.1021 | 0.144* | |
C10 | 0.4904 (4) | 0.3583 (6) | 0.9000 (4) | 0.0853 (15) | |
H10A | 0.5214 | 0.4432 | 0.9322 | 0.128* | |
H10B | 0.4715 | 0.3647 | 0.8184 | 0.128* | |
H10C | 0.5574 | 0.2916 | 0.9236 | 0.128* | |
C11 | −0.1106 (4) | 0.4735 (5) | 0.9127 (3) | 0.0639 (11) | |
H11 | −0.1765 | 0.5338 | 0.8810 | 0.077* | |
C12 | 0.1971 (3) | 0.7468 (4) | 0.7339 (3) | 0.0532 (9) | |
H12A | 0.2142 | 0.8220 | 0.7859 | 0.064* | |
H12B | 0.2771 | 0.7304 | 0.7047 | 0.064* | |
C13 | 0.0707 (3) | 0.6870 (3) | 0.5496 (3) | 0.0413 (8) | |
H13 | 0.0759 | 0.5944 | 0.5772 | 0.050* | |
C14 | −0.0630 (4) | 0.7183 (4) | 0.4720 (3) | 0.0466 (8) | |
H14 | −0.0912 | 0.6412 | 0.4225 | 0.056* | |
C15 | 0.0930 (4) | 0.8160 (4) | 0.3844 (3) | 0.0526 (9) | |
H15 | 0.1391 | 0.9024 | 0.3928 | 0.063* | |
C16 | 0.1659 (4) | 0.7137 (3) | 0.4695 (3) | 0.0458 (8) | |
H16 | 0.2525 | 0.7462 | 0.5098 | 0.055* | |
C17 | −0.1761 (3) | 0.7605 (4) | 0.5285 (3) | 0.0505 (9) | |
H17 | −0.1448 | 0.8279 | 0.5871 | 0.061* | |
C18 | −0.2963 (4) | 0.8138 (5) | 0.4449 (4) | 0.0714 (12) | |
H18A | −0.2994 | 0.9108 | 0.4472 | 0.086* | |
H18B | −0.2946 | 0.7855 | 0.3678 | 0.086* | |
C19 | −0.3644 (4) | 0.6392 (5) | 0.5401 (4) | 0.0697 (12) | |
C20 | −0.3981 (6) | 0.5218 (7) | 0.4613 (7) | 0.134 (3) | |
H20A | −0.3777 | 0.4403 | 0.5035 | 0.201* | |
H20B | −0.3472 | 0.5264 | 0.4025 | 0.201* | |
H20C | −0.4910 | 0.5238 | 0.4277 | 0.201* | |
C21 | −0.4299 (6) | 0.6271 (11) | 0.6403 (6) | 0.156 (3) | |
H21A | −0.4154 | 0.7076 | 0.6847 | 0.234* | |
H21B | −0.3928 | 0.5524 | 0.6863 | 0.234* | |
H21C | −0.5234 | 0.6135 | 0.6142 | 0.234* | |
C22 | 0.1578 (4) | 0.6354 (4) | 0.2863 (3) | 0.0549 (9) | |
C23 | 0.0694 (6) | 0.5346 (6) | 0.2161 (4) | 0.1034 (19) | |
H23A | 0.0504 | 0.5628 | 0.1379 | 0.155* | |
H23B | −0.0119 | 0.5272 | 0.2433 | 0.155* | |
H23C | 0.1131 | 0.4493 | 0.2219 | 0.155* | |
C24 | 0.2892 (5) | 0.6497 (8) | 0.2513 (4) | 0.103 (2) | |
H24A | 0.3421 | 0.7148 | 0.2990 | 0.155* | |
H24B | 0.2753 | 0.6782 | 0.1733 | 0.155* | |
H24C | 0.3343 | 0.5650 | 0.2592 | 0.155* |
U11 | U22 | U33 | U12 | U13 | U23 | |
O1 | 0.078 (2) | 0.0662 (19) | 0.0634 (16) | 0.0010 (17) | 0.0235 (15) | 0.0105 (15) |
O2 | 0.0735 (19) | 0.097 (2) | 0.0728 (19) | −0.0167 (18) | 0.0300 (15) | −0.0030 (19) |
O3 | 0.0585 (14) | 0.0433 (13) | 0.0455 (12) | 0.0015 (12) | 0.0018 (11) | −0.0030 (11) |
O4 | 0.0596 (15) | 0.0560 (17) | 0.0617 (15) | 0.0130 (13) | 0.0134 (12) | 0.0235 (14) |
O5 | 0.0444 (13) | 0.0616 (17) | 0.0737 (17) | 0.0050 (13) | 0.0103 (11) | 0.0162 (15) |
O6 | 0.0512 (17) | 0.068 (2) | 0.170 (4) | 0.0052 (16) | −0.014 (2) | 0.028 (2) |
O7 | 0.0780 (17) | 0.0480 (15) | 0.0460 (13) | 0.0135 (13) | 0.0162 (12) | 0.0070 (12) |
O8 | 0.136 (3) | 0.074 (2) | 0.0483 (15) | 0.043 (2) | 0.0234 (17) | 0.0148 (15) |
C1 | 0.0479 (18) | 0.052 (2) | 0.0378 (16) | −0.0008 (17) | 0.0031 (14) | −0.0031 (17) |
C2 | 0.0438 (18) | 0.057 (2) | 0.0450 (19) | −0.0009 (17) | 0.0066 (15) | −0.0060 (17) |
C3 | 0.055 (2) | 0.054 (2) | 0.0405 (17) | 0.0039 (18) | 0.0100 (15) | −0.0040 (16) |
C4 | 0.061 (2) | 0.050 (2) | 0.0368 (17) | 0.0006 (18) | 0.0111 (15) | −0.0017 (16) |
C5 | 0.0485 (19) | 0.057 (2) | 0.0364 (17) | −0.0034 (17) | 0.0076 (14) | −0.0099 (17) |
C6 | 0.0446 (18) | 0.057 (2) | 0.0380 (17) | 0.0052 (17) | 0.0010 (13) | −0.0059 (17) |
C7 | 0.068 (2) | 0.069 (3) | 0.059 (2) | 0.022 (2) | 0.0109 (19) | 0.007 (2) |
C8 | 0.118 (4) | 0.063 (3) | 0.094 (4) | 0.030 (3) | 0.036 (3) | 0.009 (3) |
C9 | 0.096 (3) | 0.119 (5) | 0.066 (3) | 0.042 (4) | 0.000 (2) | 0.016 (3) |
C10 | 0.060 (3) | 0.105 (4) | 0.092 (3) | 0.031 (3) | 0.018 (2) | 0.006 (3) |
C11 | 0.058 (2) | 0.083 (3) | 0.051 (2) | −0.004 (2) | 0.0141 (18) | −0.013 (2) |
C12 | 0.055 (2) | 0.055 (2) | 0.0462 (18) | −0.0019 (18) | 0.0004 (16) | 0.0002 (18) |
C13 | 0.0504 (19) | 0.0310 (16) | 0.0420 (17) | 0.0006 (14) | 0.0084 (14) | −0.0006 (14) |
C14 | 0.054 (2) | 0.0389 (19) | 0.0446 (17) | −0.0008 (15) | 0.0037 (15) | 0.0028 (16) |
C15 | 0.063 (2) | 0.044 (2) | 0.0521 (19) | −0.0033 (18) | 0.0136 (16) | 0.0091 (18) |
C16 | 0.0496 (19) | 0.0393 (19) | 0.0472 (18) | −0.0046 (15) | 0.0065 (15) | 0.0029 (16) |
C17 | 0.0485 (19) | 0.045 (2) | 0.057 (2) | 0.0029 (17) | 0.0081 (16) | −0.0038 (18) |
C18 | 0.057 (2) | 0.065 (3) | 0.090 (3) | 0.011 (2) | 0.009 (2) | 0.013 (3) |
C19 | 0.043 (2) | 0.069 (3) | 0.094 (3) | 0.004 (2) | 0.006 (2) | 0.012 (3) |
C20 | 0.113 (4) | 0.077 (4) | 0.186 (6) | −0.008 (3) | −0.033 (4) | −0.010 (4) |
C21 | 0.100 (4) | 0.232 (8) | 0.153 (5) | 0.019 (5) | 0.066 (4) | 0.026 (6) |
C22 | 0.066 (2) | 0.053 (2) | 0.0466 (19) | 0.006 (2) | 0.0151 (17) | 0.0085 (19) |
C23 | 0.143 (5) | 0.102 (4) | 0.059 (3) | −0.027 (4) | 0.006 (3) | −0.004 (3) |
C24 | 0.084 (3) | 0.146 (6) | 0.090 (3) | 0.015 (4) | 0.044 (3) | 0.036 (4) |
O1—C4 | 1.357 (4) | C10—H10A | 0.9600 |
O1—H1 | 0.92 (4) | C10—H10B | 0.9600 |
O2—C11 | 1.224 (5) | C10—H10C | 0.9600 |
O3—C13 | 1.428 (4) | C11—H11 | 0.9300 |
O3—C12 | 1.437 (4) | C12—H12A | 0.9700 |
O4—C15 | 1.401 (4) | C12—H12B | 0.9700 |
O4—C14 | 1.435 (4) | C13—C16 | 1.525 (5) |
O5—C19 | 1.406 (4) | C13—C14 | 1.530 (4) |
O5—C17 | 1.432 (4) | C13—H13 | 0.9800 |
O6—C19 | 1.393 (6) | C14—C17 | 1.519 (5) |
O6—C18 | 1.394 (5) | C14—H14 | 0.9800 |
O7—C16 | 1.420 (4) | C15—C16 | 1.530 (5) |
O7—C22 | 1.428 (4) | C15—H15 | 0.9800 |
O8—C22 | 1.407 (5) | C16—H16 | 0.9800 |
O8—C15 | 1.410 (5) | C17—C18 | 1.523 (5) |
C1—C6 | 1.384 (5) | C17—H17 | 0.9800 |
C1—C2 | 1.399 (5) | C18—H18A | 0.9700 |
C1—C12 | 1.499 (5) | C18—H18B | 0.9700 |
C2—C3 | 1.396 (5) | C19—C21 | 1.495 (7) |
C2—H2 | 0.9300 | C19—C20 | 1.502 (8) |
C3—C4 | 1.402 (5) | C20—H20A | 0.9600 |
C3—C7 | 1.535 (5) | C20—H20B | 0.9600 |
C4—C5 | 1.402 (5) | C20—H20C | 0.9600 |
C5—C6 | 1.388 (5) | C21—H21A | 0.9600 |
C5—C11 | 1.467 (5) | C21—H21B | 0.9600 |
C6—H6 | 0.9300 | C21—H21C | 0.9600 |
C7—C10 | 1.527 (6) | C22—C23 | 1.498 (7) |
C7—C8 | 1.544 (7) | C22—C24 | 1.500 (6) |
C7—C9 | 1.557 (6) | C23—H23A | 0.9600 |
C8—H8A | 0.9600 | C23—H23B | 0.9600 |
C8—H8B | 0.9600 | C23—H23C | 0.9600 |
C8—H8C | 0.9600 | C24—H24A | 0.9600 |
C9—H9A | 0.9600 | C24—H24B | 0.9600 |
C9—H9B | 0.9600 | C24—H24C | 0.9600 |
C9—H9C | 0.9600 | ||
C4—O1—H1 | 107 (4) | O4—C14—C13 | 104.6 (3) |
C13—O3—C12 | 114.0 (3) | C17—C14—C13 | 117.5 (3) |
C15—O4—C14 | 108.7 (3) | O4—C14—H14 | 109.1 |
C19—O5—C17 | 109.1 (3) | C17—C14—H14 | 109.1 |
C19—O6—C18 | 109.1 (3) | C13—C14—H14 | 109.1 |
C16—O7—C22 | 108.9 (3) | O4—C15—O8 | 111.1 (3) |
C22—O8—C15 | 111.1 (3) | O4—C15—C16 | 107.8 (3) |
C6—C1—C2 | 117.2 (3) | O8—C15—C16 | 104.9 (3) |
C6—C1—C12 | 122.3 (3) | O4—C15—H15 | 111.0 |
C2—C1—C12 | 120.4 (3) | O8—C15—H15 | 111.0 |
C3—C2—C1 | 124.8 (3) | C16—C15—H15 | 111.0 |
C3—C2—H2 | 117.6 | O7—C16—C13 | 109.8 (3) |
C1—C2—H2 | 117.6 | O7—C16—C15 | 104.8 (3) |
C2—C3—C4 | 115.8 (3) | C13—C16—C15 | 104.3 (3) |
C2—C3—C7 | 121.7 (3) | O7—C16—H16 | 112.5 |
C4—C3—C7 | 122.5 (3) | C13—C16—H16 | 112.5 |
O1—C4—C3 | 119.4 (3) | C15—C16—H16 | 112.5 |
O1—C4—C5 | 119.7 (3) | O5—C17—C14 | 109.9 (3) |
C3—C4—C5 | 120.9 (3) | O5—C17—C18 | 104.0 (3) |
C6—C5—C4 | 120.6 (3) | C14—C17—C18 | 113.5 (3) |
C6—C5—C11 | 118.5 (3) | O5—C17—H17 | 109.8 |
C4—C5—C11 | 120.9 (4) | C14—C17—H17 | 109.8 |
C1—C6—C5 | 120.6 (3) | C18—C17—H17 | 109.8 |
C1—C6—H6 | 119.7 | O6—C18—C17 | 104.0 (3) |
C5—C6—H6 | 119.7 | O6—C18—H18A | 111.0 |
C10—C7—C3 | 112.3 (4) | C17—C18—H18A | 111.0 |
C10—C7—C8 | 108.4 (4) | O6—C18—H18B | 111.0 |
C3—C7—C8 | 109.3 (4) | C17—C18—H18B | 111.0 |
C10—C7—C9 | 107.6 (4) | H18A—C18—H18B | 109.0 |
C3—C7—C9 | 109.1 (3) | O6—C19—O5 | 107.2 (3) |
C8—C7—C9 | 110.1 (4) | O6—C19—C21 | 109.5 (5) |
C7—C8—H8A | 109.5 | O5—C19—C21 | 109.1 (4) |
C7—C8—H8B | 109.5 | O6—C19—C20 | 110.2 (4) |
H8A—C8—H8B | 109.5 | O5—C19—C20 | 109.9 (4) |
C7—C8—H8C | 109.5 | C21—C19—C20 | 110.9 (6) |
H8A—C8—H8C | 109.5 | C19—C20—H20A | 109.5 |
H8B—C8—H8C | 109.5 | C19—C20—H20B | 109.5 |
C7—C9—H9A | 109.5 | H20A—C20—H20B | 109.5 |
C7—C9—H9B | 109.5 | C19—C20—H20C | 109.5 |
H9A—C9—H9B | 109.5 | H20A—C20—H20C | 109.5 |
C7—C9—H9C | 109.5 | H20B—C20—H20C | 109.5 |
H9A—C9—H9C | 109.5 | C19—C21—H21A | 109.5 |
H9B—C9—H9C | 109.5 | C19—C21—H21B | 109.5 |
C7—C10—H10A | 109.5 | H21A—C21—H21B | 109.5 |
C7—C10—H10B | 109.5 | C19—C21—H21C | 109.5 |
H10A—C10—H10B | 109.5 | H21A—C21—H21C | 109.5 |
C7—C10—H10C | 109.5 | H21B—C21—H21C | 109.5 |
H10A—C10—H10C | 109.5 | O8—C22—O7 | 106.5 (3) |
H10B—C10—H10C | 109.5 | O8—C22—C23 | 108.7 (4) |
O2—C11—C5 | 124.6 (4) | O7—C22—C23 | 108.8 (3) |
O2—C11—H11 | 117.7 | O8—C22—C24 | 109.5 (4) |
C5—C11—H11 | 117.7 | O7—C22—C24 | 110.4 (3) |
O3—C12—C1 | 113.5 (3) | C23—C22—C24 | 112.7 (4) |
O3—C12—H12A | 108.9 | C22—C23—H23A | 109.5 |
C1—C12—H12A | 108.9 | C22—C23—H23B | 109.5 |
O3—C12—H12B | 108.9 | H23A—C23—H23B | 109.5 |
C1—C12—H12B | 108.9 | C22—C23—H23C | 109.5 |
H12A—C12—H12B | 107.7 | H23A—C23—H23C | 109.5 |
O3—C13—C16 | 110.2 (3) | H23B—C23—H23C | 109.5 |
O3—C13—C14 | 107.9 (3) | C22—C24—H24A | 109.5 |
C16—C13—C14 | 101.2 (3) | C22—C24—H24B | 109.5 |
O3—C13—H13 | 112.3 | H24A—C24—H24B | 109.5 |
C16—C13—H13 | 112.3 | C22—C24—H24C | 109.5 |
C14—C13—H13 | 112.3 | H24A—C24—H24C | 109.5 |
O4—C14—C17 | 107.0 (3) | H24B—C24—H24C | 109.5 |
C6—C1—C2—C3 | −1.8 (5) | C14—O4—C15—O8 | 98.8 (3) |
C12—C1—C2—C3 | 176.6 (3) | C14—O4—C15—C16 | −15.6 (4) |
C1—C2—C3—C4 | 0.5 (5) | C22—O8—C15—O4 | −116.7 (3) |
C1—C2—C3—C7 | 179.0 (3) | C22—O8—C15—C16 | −0.5 (4) |
C2—C3—C4—O1 | −179.3 (3) | C22—O7—C16—C13 | 130.5 (3) |
C7—C3—C4—O1 | 2.1 (5) | C22—O7—C16—C15 | 19.1 (4) |
C2—C3—C4—C5 | 1.1 (5) | O3—C13—C16—O7 | 160.8 (3) |
C7—C3—C4—C5 | −177.4 (3) | C14—C13—C16—O7 | −85.1 (3) |
O1—C4—C5—C6 | 179.1 (3) | O3—C13—C16—C15 | −87.4 (3) |
C3—C4—C5—C6 | −1.3 (5) | C14—C13—C16—C15 | 26.6 (3) |
O1—C4—C5—C11 | −1.5 (5) | O4—C15—C16—O7 | 107.1 (3) |
C3—C4—C5—C11 | 178.1 (3) | O8—C15—C16—O7 | −11.4 (4) |
C2—C1—C6—C5 | 1.5 (5) | O4—C15—C16—C13 | −8.3 (4) |
C12—C1—C6—C5 | −176.9 (3) | O8—C15—C16—C13 | −126.7 (3) |
C4—C5—C6—C1 | 0.0 (5) | C19—O5—C17—C14 | −127.5 (3) |
C11—C5—C6—C1 | −179.4 (3) | C19—O5—C17—C18 | −5.7 (4) |
C2—C3—C7—C10 | 0.4 (5) | O4—C14—C17—O5 | 168.1 (3) |
C4—C3—C7—C10 | 178.8 (4) | C13—C14—C17—O5 | −74.7 (4) |
C2—C3—C7—C8 | −120.0 (4) | O4—C14—C17—C18 | 52.2 (4) |
C4—C3—C7—C8 | 58.4 (5) | C13—C14—C17—C18 | 169.3 (3) |
C2—C3—C7—C9 | 119.5 (4) | C19—O6—C18—C17 | −26.2 (5) |
C4—C3—C7—C9 | −62.0 (5) | O5—C17—C18—O6 | 19.1 (4) |
C6—C5—C11—O2 | −177.4 (4) | C14—C17—C18—O6 | 138.5 (4) |
C4—C5—C11—O2 | 3.2 (6) | C18—O6—C19—O5 | 23.4 (5) |
C13—O3—C12—C1 | −67.5 (4) | C18—O6—C19—C21 | 141.6 (5) |
C6—C1—C12—O3 | −41.2 (5) | C18—O6—C19—C20 | −96.2 (5) |
C2—C1—C12—O3 | 140.5 (3) | C17—O5—C19—O6 | −9.9 (5) |
C12—O3—C13—C16 | −84.1 (3) | C17—O5—C19—C21 | −128.4 (5) |
C12—O3—C13—C14 | 166.2 (3) | C17—O5—C19—C20 | 109.8 (5) |
C15—O4—C14—C17 | 158.6 (3) | C15—O8—C22—O7 | 12.1 (4) |
C15—O4—C14—C13 | 33.2 (3) | C15—O8—C22—C23 | 129.2 (4) |
O3—C13—C14—O4 | 79.3 (3) | C15—O8—C22—C24 | −107.3 (4) |
C16—C13—C14—O4 | −36.5 (3) | C16—O7—C22—O8 | −19.8 (4) |
O3—C13—C14—C17 | −39.1 (4) | C16—O7—C22—C23 | −136.8 (4) |
C16—C13—C14—C17 | −154.9 (3) | C16—O7—C22—C24 | 99.0 (4) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1···O2 | 0.92 (4) | 1.77 (5) | 2.609 (4) | 150 (6) |
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