Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768100015184/an0566sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768100015184/an0566xraysup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768100015184/an0566neutronsup3.hkl | |
Portable Document Format (PDF) file https://doi.org/10.1107/S0108768100015184/an0566sup4.pdf |
CCDC references: 166505; 166506
Data collection: CAD-4 EXPRESS88 for xray; RETREAT for neutron. Program(s) used to solve structure: SHELXS86 (Sheldrick, 1990) for xray; SHELXS86? (Sheldrick, 1990) for neutron. Program(s) used to refine structure: SHELXL92 (Sheldrick, 1993) for xray; SHELXL92? (Sheldrick, 1993) for neutron. Molecular graphics: SNOOPI for neutron.
C24H30O6·H2O | F(000) = 928 |
Mr = 432.50 | Dx = 1.258 Mg m−3 |
Monoclinic, P21 | Cu Kα radiation, λ = 1.54180 Å |
Hall symbol: P 2y1 | Cell parameters from 25 reflections |
a = 12.845 (5) Å | θ = 25–30° |
b = 14.575 (3) Å | µ = 0.75 mm−1 |
c = 13.779 (2) Å | T = 293 K |
β = 117.72 (2)° | Plate, colourless |
V = 2283.6 (11) Å3 | 0.35 × 0.25 × 0.20 mm |
Z = 4 |
Nonius CAD-4 diffractometer | 4804 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.046 |
Graphite monochromator | θmax = 72.9°, θmin = 3.6° |
ω/2θ scans | h = −15→15 |
17753 measured reflections | k = −18→18 |
9092 independent reflections | l = −17→17 |
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)] = 0.062 | Calculated w = 1/[σ2(Fo2) + (0.0922P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.169 | (Δ/σ)max = 0.078 |
S = 0.91 | Δρmax = 0.23 e Å−3 |
9092 reflections | Δρmin = −0.26 e Å−3 |
605 parameters | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
217 restraints | Absolute structure parameter: 0.2 (4) |
Primary atom site location: structure-invariant direct methods |
C24H30O6·H2O | V = 2283.6 (11) Å3 |
Mr = 432.50 | Z = 4 |
Monoclinic, P21 | Cu Kα radiation |
a = 12.845 (5) Å | µ = 0.75 mm−1 |
b = 14.575 (3) Å | T = 293 K |
c = 13.779 (2) Å | 0.35 × 0.25 × 0.20 mm |
β = 117.72 (2)° |
Nonius CAD-4 diffractometer | 4804 reflections with I > 2σ(I) |
17753 measured reflections | Rint = 0.046 |
9092 independent reflections |
R[F2 > 2σ(F2)] = 0.062 | 217 restraints |
wR(F2) = 0.169 | Δρmax = 0.23 e Å−3 |
S = 0.91 | Δρmin = −0.26 e Å−3 |
9092 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
605 parameters | Absolute structure parameter: 0.2 (4) |
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 0 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 | ||
O20A | 1.26721 (14) | 1.28501 (15) | 0.26123 (15) | 0.0892 (8) | |
C21A | 1.1736 (2) | 1.3377 (2) | 0.2564 (2) | 0.0919 (12) | |
H21A | 1.2025 (2) | 1.3968 (2) | 0.2910 (2) | 0.128 (9)* | |
H21B | 1.1374 (2) | 1.3067 (2) | 0.2954 (2) | 0.128 (9)* | |
C10A | 0.6746 (2) | 1.0963 (2) | −0.1405 (2) | 0.0625 (8) | |
C23A | 0.6729 (3) | 1.0505 (2) | −0.2406 (2) | 0.0876 (11) | |
H23A | 0.6383 (13) | 0.9906 (5) | −0.2501 (8) | 0.092 (6)* | |
H23B | 0.7518 (3) | 1.0449 (10) | −0.2303 (6) | 0.092 (6)* | |
H23C | 0.6273 (12) | 1.0870 (6) | −0.3045 (3) | 0.092 (6)* | |
C24A | 0.5486 (3) | 1.1187 (2) | −0.1648 (3) | 0.1043 (14) | |
H24A | 0.5473 (4) | 1.1353 (14) | −0.0980 (4) | 0.124 (7)* | |
H24B | 0.4996 (5) | 1.0659 (5) | −0.1961 (16) | 0.124 (7)* | |
H24C | 0.5197 (7) | 1.1689 (10) | −0.2156 (14) | 0.124 (7)* | |
C14A | 0.7499 (2) | 1.1809 (2) | −0.1093 (2) | 0.0636 (8) | |
C4A | 0.7084 (3) | 1.2545 (2) | −0.1814 (2) | 0.0897 (12) | |
H4A | 0.6356 (3) | 1.2506 (2) | −0.2434 (2) | 0.103 (10)* | |
C3A | 0.7747 (2) | 1.3332 (2) | −0.1616 (2) | 0.0846 (11) | |
H3A | 0.7463 (2) | 1.3815 (2) | −0.2113 (2) | 0.077 (8)* | |
C2A | 0.8824 (2) | 1.3418 (2) | −0.0695 (2) | 0.0705 (8) | |
H2A | 0.9256 (2) | 1.3957 (2) | −0.0562 (2) | 0.039 (5)* | |
C1A | 0.9248 (2) | 1.2690 (2) | 0.0025 (2) | 0.0634 (8) | |
C13A | 0.8596 (2) | 1.1871 (2) | −0.0192 (2) | 0.0625 (8) | |
C9A | 0.9154 (2) | 1.1054 (2) | 0.0543 (2) | 0.0588 (7) | |
H9A | 0.9569 (2) | 1.1260 (2) | 0.1307 (2) | 0.087 (9)* | |
O9A | 0.9972 (2) | 1.06641 (13) | 0.02441 (14) | 0.0698 (6) | |
H9A1 | 1.0642 (2) | 1.0783 (14) | 0.0715 (10) | 0.065 (7)* | |
C12A | 0.8338 (2) | 1.0332 (2) | 0.0445 (2) | 0.0644 (9) | |
C8A | 0.8687 (2) | 0.9626 (2) | 0.1222 (2) | 0.0760 (10) | |
C7A | 0.8041 (2) | 0.8866 (2) | 0.1143 (2) | 0.0926 (12) | |
H7A | 0.8319 (2) | 0.8423 (2) | 0.1691 (2) | 0.095 (10)* | |
C6A | 0.6964 (3) | 0.8767 (2) | 0.0229 (2) | 0.1072 (15) | |
H6A | 0.6500 (3) | 0.8252 (2) | 0.0139 (2) | 0.069 (7)* | |
C5A | 0.6594 (3) | 0.9457 (2) | −0.0548 (2) | 0.1020 (14) | |
H5A | 0.5862 (3) | 0.9395 (2) | −0.1160 (2) | 0.168 (16)* | |
C11A | 0.7251 (2) | 1.0238 (2) | −0.0468 (2) | 0.0772 (9) | |
O8A | 0.9745 (2) | 0.98222 (13) | 0.2110 (2) | 0.0821 (6) | |
C15A | 1.0246 (2) | 0.9196 (2) | 0.3019 (2) | 0.0871 (11) | |
H15A | 1.0462 (2) | 0.8631 (2) | 0.2786 (2) | 0.267 (19)* | |
H15B | 0.9664 (2) | 0.9050 (2) | 0.3258 (2) | 0.267 (19)* | |
C16A | 1.1301 (2) | 0.9595 (2) | 0.3950 (2) | 0.0845 (11) | |
H16A | 1.1122 (2) | 1.0208 (2) | 0.4102 (2) | 0.126 (9)* | |
H16B | 1.1518 (2) | 0.9224 (2) | 0.4600 (2) | 0.126 (9)* | |
O16A | 1.22518 (14) | 0.9633 (2) | 0.37032 (14) | 0.0858 (7) | |
C17A | 1.3310 (2) | 0.9833 (2) | 0.4651 (2) | 0.0993 (13) | |
H17A | 1.3963 (2) | 0.9684 (2) | 0.4508 (2) | 0.135 (9)* | |
H17B | 1.3368 (2) | 0.9438 (2) | 0.5241 (2) | 0.135 (9)* | |
C18A | 1.3439 (3) | 1.0807 (2) | 0.5031 (2) | 0.1015 (14) | |
H18A | 1.2781 (3) | 1.0976 (2) | 0.5157 (2) | 0.194 (15)* | |
H18B | 1.4157 (3) | 1.0877 (2) | 0.5715 (2) | 0.194 (15)* | |
O18A | 1.3473 (2) | 1.13845 (13) | 0.4223 (2) | 0.0935 (8) | |
C19A | 1.3602 (4) | 1.2315 (2) | 0.4528 (3) | 0.122 (2) | |
H19A | 1.4308 (4) | 1.2401 (2) | 0.5218 (3) | 0.083 (6)* | |
H19B | 1.2932 (4) | 1.2518 (2) | 0.4616 (3) | 0.083 (6)* | |
C20A | 1.3682 (3) | 1.2850 (3) | 0.3652 (2) | 0.1063 (14) | |
H20A | 1.3864 (3) | 1.3480 (3) | 0.3898 (2) | 0.160 (12)* | |
H20B | 1.4338 (3) | 1.2614 (3) | 0.3562 (2) | 0.160 (12)* | |
C22A | 1.0854 (2) | 1.3511 (2) | 0.1398 (2) | 0.0818 (11) | |
H22A | 1.0289 (2) | 1.3975 (2) | 0.1346 (2) | 0.086 (7)* | |
H22B | 1.1244 (2) | 1.3719 (2) | 0.0980 (2) | 0.086 (7)* | |
O1A | 1.0270 (2) | 1.26735 (11) | 0.0965 (2) | 0.0795 (7) | |
OWA | 1.2217 (2) | 1.0887 (2) | 0.1896 (2) | 0.1034 (9) | |
HWA1 | 1.2253 | 1.0557 | 0.2626 | 0.050* | |
O20B | 1.22322 (15) | 1.1070 (2) | 0.87323 (14) | 0.0851 (7) | |
C21B | 1.1266 (2) | 1.1159 (3) | 0.8959 (2) | 0.0930 (12) | |
H21C | 1.1491 (2) | 1.1553 (3) | 0.9593 (2) | 0.093 (6)* | |
H21D | 1.1076 (2) | 1.0560 (3) | 0.9141 (2) | 0.093 (6)* | |
C10B | 0.6738 (3) | 0.9797 (2) | 0.3641 (3) | 0.0773 (10) | |
C23B | 0.6749 (3) | 1.0198 (2) | 0.2608 (3) | 0.0972 (14) | |
H23D | 0.7523 (5) | 1.0422 (11) | 0.2795 (4) | 0.092 (5)* | |
H23E | 0.6196 (12) | 1.0694 (8) | 0.2327 (9) | 0.092 (5)* | |
H23F | 0.6536 (15) | 0.9729 (4) | 0.2060 (6) | 0.092 (5)* | |
C24B | 0.5464 (2) | 0.9498 (3) | 0.3353 (3) | 0.0946 (13) | |
H24D | 0.5181 (8) | 0.9072 (12) | 0.2753 (13) | 0.120 (6)* | |
H24E | 0.4962 (5) | 1.0027 (3) | 0.3149 (18) | 0.120 (6)* | |
H24F | 0.5464 (4) | 0.9210 (14) | 0.3980 (7) | 0.120 (6)* | |
C14B | 0.7177 (2) | 1.0482 (2) | 0.4549 (2) | 0.0638 (9) | |
C4B | 0.6495 (2) | 1.1250 (2) | 0.4450 (3) | 0.0916 (12) | |
H4B | 0.5752 (2) | 1.1324 (2) | 0.3858 (3) | 0.077 (8)* | |
C3B | 0.6967 (3) | 1.1899 (2) | 0.5267 (2) | 0.1023 (14) | |
H3B | 0.6536 (3) | 1.2431 (2) | 0.5186 (2) | 0.202 (19)* | |
C2B | 0.8028 (2) | 1.1817 (2) | 0.6193 (2) | 0.0878 (12) | |
H2B | 0.8286 (2) | 1.2271 (2) | 0.6729 (2) | 0.096 (9)* | |
C1B | 0.8708 (2) | 1.1048 (2) | 0.6314 (2) | 0.0667 (8) | |
C13B | 0.8273 (2) | 1.0391 (2) | 0.5451 (2) | 0.0621 (8) | |
C9B | 0.9127 (2) | 0.9632 (2) | 0.5548 (2) | 0.0571 (8) | |
H9B | 0.9525 (2) | 0.9414 (2) | 0.6308 (2) | 0.044 (6)* | |
O9B | 1.0000 (2) | 1.00306 (14) | 0.5267 (2) | 0.0715 (6) | |
H9B1 | 1.063 (3) | 1.010 (7) | 0.5826 (11) | 0.49 (6)* | |
C12B | 0.8559 (2) | 0.8842 (2) | 0.4808 (2) | 0.0569 (8) | |
C8B | 0.9201 (2) | 0.8019 (2) | 0.5029 (2) | 0.0633 (9) | |
C7B | 0.8799 (2) | 0.7268 (2) | 0.4360 (2) | 0.0777 (10) | |
H7B | 0.9230 (2) | 0.6726 (2) | 0.4534 (2) | 0.156 (14)* | |
C6B | 0.7737 (2) | 0.7336 (2) | 0.3423 (2) | 0.0765 (9) | |
H6B | 0.7462 (2) | 0.6844 (2) | 0.2939 (2) | 0.092 (9)* | |
C5B | 0.7082 (2) | 0.81269 (15) | 0.3200 (2) | 0.0667 (9) | |
H5B | 0.6355 (2) | 0.81508 (15) | 0.2577 (2) | 0.078 (9)* | |
C11B | 0.7476 (2) | 0.8895 (2) | 0.3882 (2) | 0.0665 (9) | |
O8B | 1.0261 (2) | 0.80219 (14) | 0.5980 (2) | 0.0759 (7) | |
C15B | 1.0855 (3) | 0.7176 (2) | 0.6420 (2) | 0.0864 (12) | |
H15C | 1.1248 (3) | 0.6966 (2) | 0.6007 (2) | 0.122 (9)* | |
H15D | 1.0295 (3) | 0.6711 (2) | 0.6378 (2) | 0.122 (9)* | |
C16B | 1.1724 (2) | 0.7340 (2) | 0.7576 (2) | 0.0801 (10) | |
H16C | 1.1344 (2) | 0.7651 (2) | 0.7950 (2) | 0.073 (5)* | |
H16D | 1.2021 (2) | 0.6757 (2) | 0.7939 (2) | 0.073 (5)* | |
O16B | 1.2668 (2) | 0.7879 (2) | 0.7646 (2) | 0.0932 (8) | |
C17B | 1.3691 (3) | 0.7837 (3) | 0.8685 (2) | 0.109 (2) | |
H17C | 1.4362 (3) | 0.8046 (3) | 0.8601 (2) | 0.104 (7)* | |
H17D | 1.3833 (3) | 0.7202 (3) | 0.8924 (2) | 0.104 (7)* | |
C18B | 1.3609 (3) | 0.8397 (2) | 0.9554 (3) | 0.0924 (13) | |
H18C | 1.2937 (3) | 0.8200 (2) | 0.9642 (3) | 0.191 (13)* | |
H18D | 1.4312 (3) | 0.8310 (2) | 1.0247 (3) | 0.191 (13)* | |
O18B | 1.3487 (2) | 0.93327 (15) | 0.9260 (2) | 0.0989 (9) | |
C19B | 1.3442 (3) | 0.9910 (3) | 1.0066 (2) | 0.1053 (14) | |
H19C | 1.4158 (3) | 0.9845 (3) | 1.0753 (2) | 0.089 (6)* | |
H19D | 1.2781 (3) | 0.9741 (3) | 1.0187 (2) | 0.089 (6)* | |
C20B | 1.3312 (2) | 1.0877 (3) | 0.9673 (3) | 0.1019 (14) | |
H20C | 1.3387 (2) | 1.1281 (3) | 1.0262 (3) | 0.117 (9)* | |
H20D | 1.3951 (2) | 1.1018 (3) | 0.9509 (3) | 0.117 (9)* | |
C22B | 1.0205 (3) | 1.1545 (2) | 0.8024 (2) | 0.0891 (12) | |
H22C | 0.9615 (3) | 1.1694 (2) | 0.8251 (2) | 0.069 (5)* | |
H22D | 1.0405 (3) | 1.2100 (2) | 0.7760 (2) | 0.069 (5)* | |
O1B | 0.9771 (2) | 1.08707 (14) | 0.7189 (2) | 0.0767 (7) | |
OWB | 1.2241 (2) | 0.9817 (2) | 0.6897 (2) | 0.1035 (10) | |
HWB1 | 1.2512 | 1.0182 | 0.7744 | 0.050* |
U11 | U22 | U33 | U12 | U13 | U23 | |
O20A | 0.0800 (11) | 0.105 (2) | 0.0771 (11) | 0.0029 (12) | 0.0315 (10) | 0.0112 (11) |
C21A | 0.072 (2) | 0.083 (2) | 0.098 (2) | 0.000 (2) | 0.020 (2) | −0.006 (2) |
C10A | 0.0671 (13) | 0.072 (2) | 0.0450 (11) | 0.0204 (13) | 0.0233 (11) | 0.0127 (12) |
C23A | 0.117 (2) | 0.089 (2) | 0.0533 (14) | 0.009 (2) | 0.0372 (15) | −0.0170 (15) |
C24A | 0.111 (2) | 0.088 (2) | 0.101 (2) | 0.009 (2) | 0.038 (2) | −0.022 (2) |
C14A | 0.0824 (14) | 0.057 (2) | 0.0594 (13) | −0.0075 (13) | 0.0397 (12) | 0.0061 (12) |
C4A | 0.103 (2) | 0.073 (2) | 0.061 (2) | 0.008 (2) | 0.011 (2) | −0.003 (2) |
C3A | 0.106 (2) | 0.085 (2) | 0.0433 (13) | 0.037 (2) | 0.0189 (14) | 0.0174 (14) |
C2A | 0.096 (2) | 0.049 (2) | 0.0796 (15) | −0.0042 (15) | 0.0524 (13) | 0.0071 (13) |
C1A | 0.0769 (14) | 0.058 (2) | 0.0649 (13) | 0.0009 (13) | 0.0406 (12) | 0.0101 (12) |
C13A | 0.0737 (14) | 0.067 (2) | 0.0503 (13) | 0.0158 (14) | 0.0312 (12) | 0.0077 (12) |
C9A | 0.0655 (12) | 0.062 (2) | 0.0570 (12) | 0.0192 (12) | 0.0352 (11) | −0.0039 (11) |
O9A | 0.0707 (9) | 0.0763 (13) | 0.0658 (10) | 0.0039 (10) | 0.0346 (9) | 0.0030 (9) |
C12A | 0.0674 (15) | 0.066 (2) | 0.0492 (13) | 0.0120 (14) | 0.0184 (12) | −0.0018 (12) |
C8A | 0.0581 (14) | 0.094 (2) | 0.0605 (15) | 0.002 (2) | 0.0150 (12) | −0.007 (2) |
C7A | 0.097 (2) | 0.069 (2) | 0.104 (2) | 0.003 (2) | 0.041 (2) | 0.017 (2) |
C6A | 0.105 (2) | 0.070 (2) | 0.124 (3) | −0.024 (2) | 0.034 (2) | 0.023 (2) |
C5A | 0.087 (2) | 0.119 (3) | 0.082 (2) | 0.010 (2) | 0.024 (2) | 0.006 (2) |
C11A | 0.101 (2) | 0.058 (2) | 0.099 (2) | −0.0121 (15) | 0.0684 (14) | −0.0031 (13) |
O8A | 0.1054 (12) | 0.0721 (13) | 0.0806 (10) | 0.0076 (11) | 0.0532 (10) | 0.0273 (10) |
C15A | 0.114 (2) | 0.081 (2) | 0.078 (2) | 0.012 (2) | 0.055 (2) | 0.028 (2) |
C16A | 0.110 (2) | 0.099 (2) | 0.0403 (12) | 0.024 (2) | 0.0321 (13) | 0.0145 (14) |
O16A | 0.0923 (11) | 0.105 (2) | 0.0683 (10) | 0.0249 (12) | 0.0447 (9) | 0.0005 (11) |
C17A | 0.096 (2) | 0.122 (3) | 0.064 (2) | 0.009 (2) | 0.024 (2) | 0.016 (2) |
C18A | 0.100 (2) | 0.114 (3) | 0.053 (2) | 0.013 (2) | 0.004 (2) | −0.008 (2) |
O18A | 0.1085 (13) | 0.109 (2) | 0.0638 (11) | 0.0072 (14) | 0.0409 (10) | −0.0049 (12) |
C19A | 0.119 (3) | 0.111 (3) | 0.079 (2) | −0.001 (3) | −0.001 (2) | −0.018 (2) |
C20A | 0.088 (2) | 0.124 (3) | 0.084 (2) | −0.036 (2) | 0.021 (2) | −0.011 (2) |
C22A | 0.076 (2) | 0.076 (2) | 0.088 (2) | 0.001 (2) | 0.034 (2) | 0.019 (2) |
O1A | 0.0791 (11) | 0.0452 (11) | 0.0969 (14) | −0.0051 (10) | 0.0265 (11) | −0.0014 (10) |
OWA | 0.1239 (15) | 0.125 (2) | 0.0685 (11) | 0.0209 (14) | 0.0512 (11) | −0.0019 (13) |
O20B | 0.0924 (12) | 0.112 (2) | 0.0576 (10) | −0.0031 (13) | 0.0403 (10) | −0.0046 (11) |
C21B | 0.093 (2) | 0.124 (3) | 0.088 (2) | −0.013 (2) | 0.064 (2) | −0.020 (2) |
C10B | 0.077 (2) | 0.066 (2) | 0.083 (2) | 0.018 (2) | 0.032 (2) | 0.026 (2) |
C23B | 0.108 (2) | 0.078 (2) | 0.090 (2) | 0.024 (2) | 0.032 (2) | 0.005 (2) |
C24B | 0.054 (2) | 0.105 (3) | 0.110 (3) | 0.003 (2) | 0.025 (2) | −0.021 (2) |
C14B | 0.0588 (15) | 0.067 (2) | 0.0488 (14) | 0.0030 (14) | 0.0109 (13) | 0.0000 (13) |
C4B | 0.083 (2) | 0.064 (2) | 0.109 (3) | 0.041 (2) | 0.029 (2) | −0.005 (2) |
C3B | 0.100 (2) | 0.093 (3) | 0.115 (3) | 0.027 (2) | 0.051 (2) | 0.007 (2) |
C2B | 0.099 (2) | 0.079 (2) | 0.092 (2) | 0.018 (2) | 0.049 (2) | −0.023 (2) |
C1B | 0.104 (2) | 0.0457 (15) | 0.0698 (14) | 0.0056 (15) | 0.0565 (13) | −0.0105 (12) |
C13B | 0.087 (2) | 0.048 (2) | 0.073 (2) | 0.0112 (14) | 0.0549 (13) | −0.0034 (12) |
C9B | 0.0702 (15) | 0.050 (2) | 0.0514 (13) | 0.0125 (13) | 0.0283 (12) | −0.0051 (12) |
O9B | 0.0890 (11) | 0.0620 (13) | 0.0810 (12) | −0.0092 (11) | 0.0542 (10) | −0.0022 (10) |
C12B | 0.0698 (15) | 0.0487 (15) | 0.0573 (14) | 0.0051 (13) | 0.0339 (12) | 0.0001 (12) |
C8B | 0.071 (2) | 0.057 (2) | 0.0590 (15) | −0.003 (2) | 0.0275 (13) | 0.0028 (14) |
C7B | 0.092 (2) | 0.072 (2) | 0.069 (2) | −0.008 (2) | 0.038 (2) | −0.009 (2) |
C6B | 0.110 (2) | 0.057 (2) | 0.084 (2) | 0.001 (2) | 0.062 (2) | −0.010 (2) |
C5B | 0.077 (2) | 0.076 (2) | 0.0548 (14) | −0.019 (2) | 0.0365 (13) | −0.0137 (14) |
C11B | 0.073 (2) | 0.074 (2) | 0.0488 (14) | −0.018 (2) | 0.0247 (13) | 0.0064 (14) |
O8B | 0.0748 (12) | 0.0716 (14) | 0.0676 (12) | 0.0076 (12) | 0.0214 (10) | −0.0110 (11) |
C15B | 0.101 (2) | 0.051 (2) | 0.101 (2) | 0.025 (2) | 0.041 (2) | 0.021 (2) |
C16B | 0.106 (2) | 0.073 (2) | 0.077 (2) | 0.016 (2) | 0.056 (2) | 0.012 (2) |
O16B | 0.0877 (13) | 0.096 (2) | 0.0912 (14) | −0.0081 (13) | 0.0374 (12) | 0.0225 (13) |
C17B | 0.085 (2) | 0.115 (3) | 0.095 (3) | −0.025 (2) | 0.015 (2) | 0.003 (3) |
C18B | 0.096 (2) | 0.108 (3) | 0.072 (2) | −0.007 (2) | 0.038 (2) | 0.003 (2) |
O18B | 0.101 (2) | 0.107 (2) | 0.0738 (14) | −0.012 (2) | 0.0286 (13) | 0.0056 (14) |
C19B | 0.111 (2) | 0.147 (4) | 0.062 (2) | −0.008 (3) | 0.044 (2) | −0.009 (2) |
C20B | 0.096 (2) | 0.124 (3) | 0.088 (2) | −0.039 (2) | 0.045 (2) | −0.013 (2) |
C22B | 0.097 (2) | 0.092 (3) | 0.065 (2) | −0.002 (2) | 0.026 (2) | −0.027 (2) |
O1B | 0.0792 (13) | 0.0759 (14) | 0.0521 (10) | 0.0028 (11) | 0.0113 (10) | −0.0128 (10) |
OWB | 0.097 (2) | 0.119 (2) | 0.0660 (13) | −0.026 (2) | 0.0140 (12) | 0.0077 (14) |
O20A—C20A | 1.417 (2) | O20B—C21B | 1.420 (3) |
O20A—C21A | 1.402 (3) | O20B—C20B | 1.418 (3) |
C21A—C22A | 1.487 (3) | C21B—C22B | 1.483 (3) |
C21A—H21A | 0.97 | C21B—H21C | 0.97 |
C21A—H21B | 0.97 | C21B—H21D | 0.97 |
C10A—C14A | 1.501 (4) | C10B—C14B | 1.490 (4) |
C10A—C24A | 1.529 (4) | C10B—C11B | 1.564 (4) |
C10A—C23A | 1.522 (4) | C10B—C23B | 1.545 (5) |
C10A—C11A | 1.557 (4) | C10B—C24B | 1.556 (4) |
C23A—H23A | 0.96 | C23B—H23D | 0.96 |
C23A—H23B | 0.96 | C23B—H23E | 0.96 |
C23A—H23C | 0.96 | C23B—H23F | 0.96 |
C24A—H24A | 0.96 | C24B—H24D | 0.96 |
C24A—H24B | 0.96 | C24B—H24E | 0.96 |
C24A—H24C | 0.96 | C24B—H24F | 0.96 |
C14A—C13A | 1.381 (2) | C14B—C4B | 1.389 (3) |
C14A—C4A | 1.389 (2) | C14B—C13B | 1.385 (2) |
C4A—C3A | 1.378 (3) | C4B—C3B | 1.376 (3) |
C4A—H4A | 0.93 | C4B—H4B | 0.93 |
C3A—C2A | 1.381 (2) | C3B—C2B | 1.372 (3) |
C3A—H3A | 0.93 | C3B—H3B | 0.93 |
C2A—C1A | 1.380 (3) | C2B—C1B | 1.383 (3) |
C2A—H2A | 0.93 | C2B—H2B | 0.93 |
C1A—O1A | 1.349 (3) | C1B—O1B | 1.361 (3) |
C1A—C13A | 1.408 (3) | C1B—C13B | 1.423 (3) |
C13A—C9A | 1.511 (3) | C13B—C9B | 1.518 (3) |
C9A—O9A | 1.413 (3) | C9B—O9B | 1.466 (4) |
C9A—C12A | 1.447 (4) | C9B—C12B | 1.486 (3) |
C9A—H9A | 0.98 | C9B—H9B | 0.98 |
O9A—H9A1 | 0.82 | O9B—H9B1 | 0.82 |
C12A—C11A | 1.384 (2) | C12B—C8B | 1.407 (3) |
C12A—C8A | 1.400 (3) | C12B—C11B | 1.384 (2) |
C8A—C7A | 1.357 (4) | C8B—C7B | 1.367 (4) |
C8A—O8A | 1.371 (3) | C8B—O8B | 1.383 (3) |
C7A—C6A | 1.378 (3) | C7B—C6B | 1.378 (3) |
C7A—H7A | 0.93 | C7B—H7B | 0.93 |
C6A—C5A | 1.382 (3) | C6B—C5B | 1.375 (3) |
C6A—H6A | 0.93 | C6B—H6B | 0.93 |
C5A—C11A | 1.391 (3) | C5B—C11B | 1.397 (3) |
C5A—H5A | 0.93 | C5B—H5B | 0.93 |
O8A—C15A | 1.437 (3) | O8B—C15B | 1.427 (3) |
C15A—C16A | 1.484 (3) | C15B—C16B | 1.478 (3) |
C15A—H15A | 0.97 | C15B—H15C | 0.97 |
C15A—H15B | 0.97 | C15B—H15D | 0.97 |
C16A—O16A | 1.413 (3) | C16B—O16B | 1.410 (3) |
C16A—H16A | 0.97 | C16B—H16C | 0.97 |
C16A—H16B | 0.97 | C16B—H16D | 0.97 |
O16A—C17A | 1.410 (2) | O16B—C17B | 1.425 (3) |
C17A—C18A | 1.495 (4) | C17B—C18B | 1.493 (4) |
C17A—H17A | 0.97 | C17B—H17C | 0.97 |
C17A—H17B | 0.97 | C17B—H17D | 0.97 |
C18A—O18A | 1.413 (3) | C18B—O18B | 1.410 (3) |
C18A—H18A | 0.97 | C18B—H18C | 0.97 |
C18A—H18B | 0.97 | C18B—H18D | 0.97 |
O18A—C19A | 1.406 (3) | O18B—C19B | 1.416 (3) |
C19A—C20A | 1.479 (5) | C19B—C20B | 1.491 (5) |
C19A—H19A | 0.97 | C19B—H19C | 0.97 |
C19A—H19B | 0.97 | C19B—H19D | 0.97 |
C20A—H20A | 0.97 | C20B—H20C | 0.97 |
C20A—H20B | 0.97 | C20B—H20D | 0.97 |
C22A—O1A | 1.412 (3) | C22B—O1B | 1.416 (3) |
C22A—H22A | 0.97 | C22B—H22C | 0.97 |
C22A—H22B | 0.97 | C22B—H22D | 0.97 |
OWA—HWA1 | 1.096 (2) | OWB—HWB1 | 1.178 (3) |
C20A—O20A—C21A | 114.2 (2) | C21B—O20B—C20B | 113.6 (2) |
O20A—C21A—C22A | 109.2 (2) | O20B—C21B—C22B | 112.8 (3) |
O20A—C21A—H21A | 109.85 (14) | O20B—C21B—H21C | 109.0 (2) |
C22A—C21A—H21A | 109.9 (2) | C22B—C21B—H21C | 109.0 (2) |
O20A—C21A—H21B | 109.8 (2) | O20B—C21B—H21D | 109.0 (2) |
C22A—C21A—H21B | 109.8 (2) | C22B—C21B—H21D | 109.0 (2) |
H21A—C21A—H21B | 108.3 | H21C—C21B—H21D | 107.8 |
C14A—C10A—C24A | 111.3 (2) | C14B—C10B—C11B | 115.4 (2) |
C14A—C10A—C23A | 110.9 (2) | C14B—C10B—C23B | 111.0 (3) |
C24A—C10A—C23A | 109.1 (2) | C11B—C10B—C23B | 104.4 (3) |
C14A—C10A—C11A | 110.8 (2) | C14B—C10B—C24B | 110.1 (3) |
C24A—C10A—C11A | 108.4 (3) | C11B—C10B—C24B | 106.3 (3) |
C23A—C10A—C11A | 106.2 (2) | C23B—C10B—C24B | 109.3 (3) |
C10A—C23A—H23A | 109.5 (2) | C10B—C23B—H23D | 109.5 (2) |
C10A—C23A—H23B | 109.5 (2) | C10B—C23B—H23E | 109.5 (2) |
H23A—C23A—H23B | 109.5 | H23D—C23B—H23E | 109.5 |
C10A—C23A—H23C | 109.47 (15) | C10B—C23B—H23F | 109.5 (2) |
H23A—C23A—H23C | 109.5 | H23D—C23B—H23F | 109.5 |
H23B—C23A—H23C | 109.5 | H23E—C23B—H23F | 109.5 |
C10A—C24A—H24A | 109.5 (2) | C10B—C24B—H24D | 109.5 (2) |
C10A—C24A—H24B | 109.5 (2) | C10B—C24B—H24E | 109.5 (2) |
H24A—C24A—H24B | 109.5 | H24D—C24B—H24E | 109.5 |
C10A—C24A—H24C | 109.5 (2) | C10B—C24B—H24F | 109.5 (2) |
H24A—C24A—H24C | 109.5 | H24D—C24B—H24F | 109.5 |
H24B—C24A—H24C | 109.5 | H24E—C24B—H24F | 109.5 |
C13A—C14A—C4A | 118.9 (2) | C4B—C14B—C13B | 119.8 (2) |
C13A—C14A—C10A | 124.3 (2) | C4B—C14B—C10B | 118.8 (2) |
C4A—C14A—C10A | 116.6 (2) | C13B—C14B—C10B | 121.3 (2) |
C3A—C4A—C14A | 120.3 (2) | C3B—C4B—C14B | 117.1 (3) |
C3A—C4A—H4A | 119.83 (13) | C3B—C4B—H4B | 121.4 (2) |
C14A—C4A—H4A | 119.83 (14) | C14B—C4B—H4B | 121.45 (14) |
C4A—C3A—C2A | 121.3 (2) | C4B—C3B—C2B | 124.8 (3) |
C4A—C3A—H3A | 119.33 (14) | C4B—C3B—H3B | 117.6 (2) |
C2A—C3A—H3A | 119.3 (2) | C2B—C3B—H3B | 117.6 (2) |
C3A—C2A—C1A | 118.9 (2) | C3B—C2B—C1B | 118.7 (3) |
C3A—C2A—H2A | 120.6 (2) | C3B—C2B—H2B | 120.6 (2) |
C1A—C2A—H2A | 120.57 (14) | C1B—C2B—H2B | 120.6 (2) |
O1A—C1A—C2A | 125.9 (2) | O1B—C1B—C2B | 125.3 (2) |
O1A—C1A—C13A | 113.9 (2) | O1B—C1B—C13B | 117.0 (2) |
C2A—C1A—C13A | 120.1 (2) | C2B—C1B—C13B | 117.7 (2) |
C14A—C13A—C1A | 120.3 (2) | C14B—C13B—C1B | 121.7 (2) |
C14A—C13A—C9A | 121.2 (2) | C14B—C13B—C9B | 122.7 (2) |
C1A—C13A—C9A | 118.4 (2) | C1B—C13B—C9B | 115.5 (2) |
O9A—C9A—C12A | 106.5 (2) | O9B—C9B—C12B | 108.5 (2) |
O9A—C9A—C13A | 107.9 (2) | O9B—C9B—C13B | 107.4 (2) |
C12A—C9A—C13A | 114.4 (2) | C12B—C9B—C13B | 113.6 (2) |
O9A—C9A—H9A | 109.29 (11) | O9B—C9B—H9B | 109.10 (12) |
C12A—C9A—H9A | 109.29 (14) | C12B—C9B—H9B | 109.10 (14) |
C13A—C9A—H9A | 109.28 (13) | C13B—C9B—H9B | 109.10 (14) |
C9A—O9A—H9A1 | 109.47 (12) | C9B—O9B—H9B1 | 109.47 (13) |
C11A—C12A—C8A | 116.9 (2) | C8B—C12B—C11B | 118.9 (2) |
C11A—C12A—C9A | 122.5 (2) | C8B—C12B—C9B | 117.5 (2) |
C8A—C12A—C9A | 120.2 (2) | C11B—C12B—C9B | 123.4 (2) |
C7A—C8A—O8A | 123.9 (2) | C7B—C8B—O8B | 122.6 (2) |
C7A—C8A—C12A | 124.9 (2) | C7B—C8B—C12B | 122.5 (2) |
O8A—C8A—C12A | 111.2 (2) | O8B—C8B—C12B | 114.9 (2) |
C8A—C7A—C6A | 118.4 (3) | C8B—C7B—C6B | 118.2 (3) |
C8A—C7A—H7A | 120.8 (2) | C8B—C7B—H7B | 120.9 (2) |
C6A—C7A—H7A | 120.8 (2) | C6B—C7B—H7B | 120.9 (2) |
C5A—C6A—C7A | 117.9 (3) | C5B—C6B—C7B | 120.4 (3) |
C5A—C6A—H6A | 121.0 (2) | C5B—C6B—H6B | 119.80 (14) |
C7A—C6A—H6A | 121.0 (2) | C7B—C6B—H6B | 119.8 (2) |
C6A—C5A—C11A | 123.8 (3) | C6B—C5B—C11B | 121.9 (2) |
C6A—C5A—H5A | 118.1 (2) | C6B—C5B—H5B | 119.03 (14) |
C11A—C5A—H5A | 118.07 (15) | C11B—C5B—H5B | 119.03 (14) |
C12A—C11A—C5A | 118.1 (2) | C12B—C11B—C5B | 118.0 (2) |
C12A—C11A—C10A | 122.8 (2) | C12B—C11B—C10B | 119.5 (2) |
C5A—C11A—C10A | 119.1 (2) | C5B—C11B—C10B | 122.5 (2) |
C8A—O8A—C15A | 120.1 (2) | C8B—O8B—C15B | 119.7 (2) |
O8A—C15A—C16A | 111.3 (2) | O8B—C15B—C16B | 107.7 (2) |
O8A—C15A—H15A | 109.4 (2) | O8B—C15B—H15C | 110.2 (2) |
C16A—C15A—H15A | 109.4 (2) | C16B—C15B—H15C | 110.2 (2) |
O8A—C15A—H15B | 109.4 (2) | O8B—C15B—H15D | 110.2 (2) |
C16A—C15A—H15B | 109.4 (2) | C16B—C15B—H15D | 110.2 (2) |
H15A—C15A—H15B | 108.0 | H15C—C15B—H15D | 108.5 |
O16A—C16A—C15A | 110.6 (2) | O16B—C16B—C15B | 111.0 (2) |
O16A—C16A—H16A | 109.5 (2) | O16B—C16B—H16C | 109.4 (2) |
C15A—C16A—H16A | 109.5 (2) | C15B—C16B—H16C | 109.4 (2) |
O16A—C16A—H16B | 109.53 (13) | O16B—C16B—H16D | 109.44 (15) |
C15A—C16A—H16B | 109.5 (2) | C15B—C16B—H16D | 109.4 (2) |
H16A—C16A—H16B | 108.1 | H16C—C16B—H16D | 108.0 |
C17A—O16A—C16A | 110.7 (2) | C16B—O16B—C17B | 114.0 (2) |
O16A—C17A—C18A | 115.0 (2) | O16B—C17B—C18B | 113.9 (3) |
O16A—C17A—H17A | 108.5 (2) | O16B—C17B—H17C | 108.8 (2) |
C18A—C17A—H17A | 108.5 (2) | C18B—C17B—H17C | 108.8 (2) |
O16A—C17A—H17B | 108.5 (2) | O16B—C17B—H17D | 108.8 (2) |
C18A—C17A—H17B | 108.5 (2) | C18B—C17B—H17D | 108.8 (2) |
H17A—C17A—H17B | 107.5 | H17C—C17B—H17D | 107.7 |
O18A—C18A—C17A | 109.2 (3) | O18B—C18B—C17B | 109.8 (3) |
O18A—C18A—H18A | 109.8 (2) | O18B—C18B—H18C | 109.7 (2) |
C17A—C18A—H18A | 109.8 (2) | C17B—C18B—H18C | 109.7 (2) |
O18A—C18A—H18B | 109.85 (14) | O18B—C18B—H18D | 109.71 (15) |
C17A—C18A—H18B | 109.84 (14) | C17B—C18B—H18D | 109.7 (2) |
H18A—C18A—H18B | 108.3 | H18C—C18B—H18D | 108.2 |
C19A—O18A—C18A | 112.4 (2) | C18B—O18B—C19B | 112.9 (3) |
O18A—C19A—C20A | 107.9 (3) | O18B—C19B—C20B | 108.4 (3) |
O18A—C19A—H19A | 110.1 (2) | O18B—C19B—H19C | 110.0 (2) |
C20A—C19A—H19A | 110.1 (2) | C20B—C19B—H19C | 110.0 (2) |
O18A—C19A—H19B | 110.1 (2) | O18B—C19B—H19D | 110.0 (2) |
C20A—C19A—H19B | 110.1 (2) | C20B—C19B—H19D | 110.0 (2) |
H19A—C19A—H19B | 108.4 | H19C—C19B—H19D | 108.4 |
O20A—C20A—C19A | 116.6 (3) | O20B—C20B—C19B | 114.6 (3) |
O20A—C20A—H20A | 108.2 (2) | O20B—C20B—H20C | 108.6 (2) |
C19A—C20A—H20A | 108.2 (2) | C19B—C20B—H20C | 108.6 (2) |
O20A—C20A—H20B | 108.1 (2) | O20B—C20B—H20D | 108.6 (2) |
C19A—C20A—H20B | 108.2 (2) | C19B—C20B—H20D | 108.6 (2) |
H20A—C20A—H20B | 107.3 | H20C—C20B—H20D | 107.6 |
O1A—C22A—C21A | 109.3 (2) | O1B—C22B—C21B | 107.3 (3) |
O1A—C22A—H22A | 109.81 (15) | O1B—C22B—H22C | 110.2 (2) |
C21A—C22A—H22A | 109.8 (2) | C21B—C22B—H22C | 110.3 (2) |
O1A—C22A—H22B | 109.8 (2) | O1B—C22B—H22D | 110.3 (2) |
C21A—C22A—H22B | 109.8 (2) | C21B—C22B—H22D | 110.3 (2) |
H22A—C22A—H22B | 108.3 | H22C—C22B—H22D | 108.5 |
C1A—O1A—C22A | 118.6 (2) | C1B—O1B—C22B | 116.2 (2) |
C20A—O20A—C21A—C22A | 166.5 (3) | C20B—O20B—C21B—C22B | 168.2 (3) |
C24A—C10A—C14A—C13A | 131.7 (3) | C11B—C10B—C14B—C4B | −172.4 (3) |
C23A—C10A—C14A—C13A | −106.7 (3) | C23B—C10B—C14B—C4B | 69.0 (4) |
C11A—C10A—C14A—C13A | 11.0 (4) | C24B—C10B—C14B—C4B | −52.1 (4) |
C24A—C10A—C14A—C4A | −53.2 (4) | C11B—C10B—C14B—C13B | 11.4 (4) |
C23A—C10A—C14A—C4A | 68.4 (3) | C23B—C10B—C14B—C13B | −107.2 (3) |
C11A—C10A—C14A—C4A | −173.9 (3) | C24B—C10B—C14B—C13B | 131.6 (3) |
C13A—C14A—C4A—C3A | −1.6 (5) | C13B—C14B—C4B—C3B | 0.9 (5) |
C10A—C14A—C4A—C3A | −176.9 (3) | C10B—C14B—C4B—C3B | −175.4 (3) |
C14A—C4A—C3A—C2A | −1.1 (5) | C14B—C4B—C3B—C2B | −3.6 (6) |
C4A—C3A—C2A—C1A | 1.3 (5) | C4B—C3B—C2B—C1B | 2.4 (6) |
C3A—C2A—C1A—O1A | −178.7 (3) | C3B—C2B—C1B—O1B | −179.5 (3) |
C3A—C2A—C1A—C13A | 1.0 (5) | C3B—C2B—C1B—C13B | 1.4 (5) |
C4A—C14A—C13A—C1A | 3.9 (4) | C4B—C14B—C13B—C1B | 2.8 (5) |
C10A—C14A—C13A—C1A | 178.9 (3) | C10B—C14B—C13B—C1B | 179.0 (3) |
C4A—C14A—C13A—C9A | −172.5 (3) | C4B—C14B—C13B—C9B | −172.4 (3) |
C10A—C14A—C13A—C9A | 2.5 (4) | C10B—C14B—C13B—C9B | 3.8 (5) |
O1A—C1A—C13A—C14A | 176.1 (3) | O1B—C1B—C13B—C14B | 176.8 (3) |
C2A—C1A—C13A—C14A | −3.6 (4) | C2B—C1B—C13B—C14B | −4.0 (5) |
O1A—C1A—C13A—C9A | −7.4 (4) | O1B—C1B—C13B—C9B | −7.7 (4) |
C2A—C1A—C13A—C9A | 172.9 (3) | C2B—C1B—C13B—C9B | 171.5 (3) |
C14A—C13A—C9A—O9A | 99.8 (3) | C14B—C13B—C9B—O9B | 100.6 (3) |
C1A—C13A—C9A—O9A | −76.7 (3) | C1B—C13B—C9B—O9B | −74.9 (3) |
C14A—C13A—C9A—C12A | −18.6 (4) | C14B—C13B—C9B—C12B | −19.4 (4) |
C1A—C13A—C9A—C12A | 164.9 (3) | C1B—C13B—C9B—C12B | 165.2 (3) |
O9A—C9A—C12A—C11A | −98.2 (3) | O9B—C9B—C12B—C8B | 76.5 (3) |
C13A—C9A—C12A—C11A | 20.9 (4) | C13B—C9B—C12B—C8B | −164.2 (3) |
O9A—C9A—C12A—C8A | 73.7 (3) | O9B—C9B—C12B—C11B | −99.0 (3) |
C13A—C9A—C12A—C8A | −167.2 (3) | C13B—C9B—C12B—C11B | 20.3 (4) |
C11A—C12A—C8A—C7A | 0.0 (5) | C11B—C12B—C8B—C7B | 0.2 (5) |
C9A—C12A—C8A—C7A | −172.3 (3) | C9B—C12B—C8B—C7B | −175.5 (3) |
C11A—C12A—C8A—O8A | −176.6 (3) | C11B—C12B—C8B—O8B | −178.9 (3) |
C9A—C12A—C8A—O8A | 11.0 (4) | C9B—C12B—C8B—O8B | 5.4 (4) |
O8A—C8A—C7A—C6A | 176.9 (3) | O8B—C8B—C7B—C6B | −179.3 (3) |
C12A—C8A—C7A—C6A | 0.6 (6) | C12B—C8B—C7B—C6B | 1.7 (5) |
C8A—C7A—C6A—C5A | −1.0 (6) | C8B—C7B—C6B—C5B | −2.9 (5) |
C7A—C6A—C5A—C11A | 0.8 (6) | C7B—C6B—C5B—C11B | 2.3 (5) |
C8A—C12A—C11A—C5A | −0.3 (4) | C8B—C12B—C11B—C5B | −0.9 (4) |
C9A—C12A—C11A—C5A | 171.9 (3) | C9B—C12B—C11B—C5B | 174.5 (3) |
C8A—C12A—C11A—C10A | −179.6 (3) | C8B—C12B—C11B—C10B | 178.5 (3) |
C9A—C12A—C11A—C10A | −7.4 (5) | C9B—C12B—C11B—C10B | −6.0 (4) |
C6A—C5A—C11A—C12A | −0.1 (5) | C6B—C5B—C11B—C12B | −0.3 (4) |
C6A—C5A—C11A—C10A | 179.2 (3) | C6B—C5B—C11B—C10B | −179.7 (3) |
C14A—C10A—C11A—C12A | −8.8 (4) | C14B—C10B—C11B—C12B | −10.4 (4) |
C24A—C10A—C11A—C12A | −131.2 (3) | C23B—C10B—C11B—C12B | 111.7 (3) |
C23A—C10A—C11A—C12A | 111.7 (3) | C24B—C10B—C11B—C12B | −132.8 (3) |
C14A—C10A—C11A—C5A | 171.9 (3) | C14B—C10B—C11B—C5B | 169.0 (3) |
C24A—C10A—C11A—C5A | 49.5 (4) | C23B—C10B—C11B—C5B | −68.9 (3) |
C23A—C10A—C11A—C5A | −67.6 (4) | C24B—C10B—C11B—C5B | 46.6 (4) |
C7A—C8A—O8A—C15A | 1.5 (5) | C7B—C8B—O8B—C15B | −13.5 (5) |
C12A—C8A—O8A—C15A | 178.3 (3) | C12B—C8B—O8B—C15B | 165.5 (3) |
C8A—O8A—C15A—C16A | −172.3 (2) | C8B—O8B—C15B—C16B | −162.3 (3) |
O8A—C15A—C16A—O16A | −71.6 (3) | O8B—C15B—C16B—O16B | −71.0 (3) |
C15A—C16A—O16A—C17A | −168.1 (3) | C15B—C16B—O16B—C17B | −162.0 (3) |
C16A—O16A—C17A—C18A | −74.3 (4) | C16B—O16B—C17B—C18B | −77.2 (4) |
O16A—C17A—C18A—O18A | −64.0 (4) | O16B—C17B—C18B—O18B | −62.7 (4) |
C17A—C18A—O18A—C19A | −179.6 (3) | C17B—C18B—O18B—C19B | −178.1 (3) |
C18A—O18A—C19A—C20A | 177.5 (3) | C18B—O18B—C19B—C20B | −179.9 (3) |
C21A—O20A—C20A—C19A | 73.0 (4) | C21B—O20B—C20B—C19B | 76.2 (4) |
O18A—C19A—C20A—O20A | 64.7 (5) | O18B—C19B—C20B—O20B | 65.9 (4) |
O20A—C21A—C22A—O1A | 71.2 (3) | O20B—C21B—C22B—O1B | 69.9 (4) |
C2A—C1A—O1A—C22A | 14.7 (5) | C2B—C1B—O1B—C22B | −0.9 (5) |
C13A—C1A—O1A—C22A | −165.1 (3) | C13B—C1B—O1B—C22B | 178.2 (3) |
C21A—C22A—O1A—C1A | 163.4 (3) | C21B—C22B—O1B—C1B | 171.7 (3) |
C24H30O6·H2O | F(000) = 928 |
Mr = 432.49 | Dx = 1.303 Mg m−3 |
Monoclinic, P21 | ? radiation, λ = 1.538 and 1.312 Å |
a = 12.605 (5) Å | Cell parameters from 25 reflections |
b = 14.458 (3) Å | θ = 25–30° |
c = 13.588 (2) Å | µ = 0.00 mm−1 |
β = 117.12 (2)° | T = 15 K |
V = 2204.1 (10) Å3 | Plate, colourless |
Z = 4 | 2.5 × 1.6 × 0.2 mm |
D19 ILL ω diffractometer | Rint = 0.000 |
Radiation source: fine-focus sealed tube | θmax = 46.1°, θmin = 3.7° |
Graphite monochromator | h = −10→11 |
1931 measured reflections | k = 0→13 |
1931 independent reflections | l = −9→12 |
1881 reflections with I > 2σ(I) |
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)] = 0.046 | Calculated w = 1/[σ2(Fo2) + (0.1016P)2 + 0.5955P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.132 | (Δ/σ)max = −0.123 |
S = 0.78 | Δρmax = 0.06 e Å−3 |
1881 reflections | Δρmin = −0.06 e Å−3 |
507 parameters | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
1 restraint | Absolute structure parameter: −10.0 (100) |
Primary atom site location: structure-invariant direct methods |
C24H30O6·H2O | V = 2204.1 (10) Å3 |
Mr = 432.49 | Z = 4 |
Monoclinic, P21 | ? radiation, λ = 1.538 and 1.312 Å |
a = 12.605 (5) Å | µ = 0.00 mm−1 |
b = 14.458 (3) Å | T = 15 K |
c = 13.588 (2) Å | 2.5 × 1.6 × 0.2 mm |
β = 117.12 (2)° |
D19 ILL ω diffractometer | 1881 reflections with I > 2σ(I) |
1931 measured reflections | Rint = 0.000 |
1931 independent reflections |
R[F2 > 2σ(F2)] = 0.046 | (Δ/σ)max = −0.123 |
wR(F2) = 0.132 | Δρmax = 0.06 e Å−3 |
S = 0.78 | Δρmin = −0.06 e Å−3 |
1881 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
507 parameters | Absolute structure parameter: −10.0 (100) |
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 50 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 | Occ. (<1) | |
O1A | 1.0310 (9) | 1.2748 (9) | 0.1040 (9) | 0.042 (3)* | 1.06 (5) |
C1A | 0.9244 (8) | 1.2716 (8) | 0.0017 (8) | 0.014 (2)* | 1.06 (5) |
C2A | 0.8861 (7) | 1.3479 (7) | −0.0635 (7) | 0.006 (2)* | 1.06 (5) |
C3A | 0.7772 (8) | 1.3367 (7) | −0.1633 (7) | 0.010 (2)* | 1.06 (5) |
C4A | 0.7108 (8) | 1.2618 (7) | −0.1854 (7) | 0.008 (2)* | 1.06 (5) |
C5A | 0.6499 (8) | 0.9442 (7) | −0.0627 (8) | 0.009 (3)* | 1.06 (5) |
C6A | 0.6938 (8) | 0.8734 (7) | 0.0227 (7) | 0.006 (2)* | 1.06 (5) |
C7A | 0.8037 (8) | 0.8843 (7) | 0.1134 (7) | 0.004 (2)* | 1.06 (5) |
O8A | 0.9789 (9) | 0.9838 (8) | 0.2145 (9) | 0.008 (3)* | 0.83 (4) |
C8A | 0.8701 (8) | 0.9630 (7) | 0.1275 (8) | 0.007 (2)* | 1.06 (5) |
O9A | 1.0110 (12) | 1.0712 (8) | 0.0351 (9) | 0.009 (3)* | 0.83 (4) |
C9A | 0.9144 (8) | 1.1082 (8) | 0.0570 (8) | 0.016 (3)* | 1.06 (5) |
C10A | 0.6738 (8) | 1.0973 (8) | −0.1401 (7) | 0.014 (2)* | 1.06 (5) |
C11A | 0.7175 (8) | 1.0263 (8) | −0.0480 (8) | 0.016 (3)* | 1.06 (5) |
C12A | 0.8295 (7) | 1.0345 (6) | 0.0453 (7) | 0.004 (2)* | 1.06 (5) |
C13A | 0.8575 (7) | 1.1926 (7) | −0.0218 (7) | 0.006 (2)* | 1.06 (5) |
C14A | 0.7501 (7) | 1.1833 (7) | −0.1107 (7) | 0.007 (2)* | 1.06 (5) |
C15A | 1.0213 (8) | 0.9183 (7) | 0.3038 (7) | 0.009 (2)* | 1.06 (5) |
O16A | 1.2297 (9) | 0.9671 (8) | 0.3749 (9) | 0.017 (3)* | 0.83 (4) |
C16A | 1.1303 (9) | 0.9540 (8) | 0.3998 (8) | 0.015 (3)* | 1.06 (5) |
C17A | 1.3347 (8) | 0.9811 (7) | 0.4697 (8) | 0.006 (2)* | 1.06 (5) |
O18A | 1.3513 (10) | 1.1365 (9) | 0.4303 (10) | 0.020 (3)* | 0.83 (4) |
C18A | 1.3469 (9) | 1.0811 (7) | 0.5136 (8) | 0.008 (2)* | 1.06 (5) |
C19A | 1.3678 (10) | 1.2326 (8) | 0.4612 (9) | 0.017 (3)* | 1.06 (5) |
O20A | 1.2752 (8) | 1.2881 (7) | 0.2708 (8) | 0.005 (2)* | 0.83 (4) |
C20A | 1.3758 (8) | 1.2875 (7) | 0.3687 (7) | 0.014 (2)* | 1.06 (5) |
C21A | 1.1768 (7) | 1.3369 (7) | 0.2663 (7) | 0.008 (2)* | 1.06 (5) |
C22A | 1.0850 (7) | 1.3605 (7) | 0.1461 (6) | 0.003 (2)* | 1.06 (5) |
C23A | 0.6799 (10) | 1.0533 (7) | −0.2422 (8) | 0.015 (3)* | 1.06 (5) |
C24A | 0.5420 (8) | 1.1211 (7) | −0.1683 (9) | 0.014 (3)* | 1.06 (5) |
H3A | 0.7506 (16) | 1.3933 (14) | −0.2223 (15) | 0.024 (5)* | 0.94 (4) |
H2A | 0.9420 (13) | 1.4129 (13) | −0.0490 (12) | 0.009 (4)* | 0.94 (4) |
H4A | 0.6225 (12) | 1.2588 (11) | −0.2578 (11) | 0.004 (4)* | 0.94 (4) |
H5A | 0.5656 (16) | 0.9403 (13) | −0.1314 (15) | 0.026 (5)* | 0.94 (4) |
H6A | 0.641 (2) | 0.8176 (19) | 0.010 (2) | 0.055 (7)* | 0.94 (4) |
H7A | 0.8399 (14) | 0.8296 (13) | 0.1840 (13) | 0.017 (4)* | 0.94 (4) |
H9A | 0.9651 (17) | 1.1251 (13) | 0.1416 (16) | 0.028 (5)* | 0.94 (4) |
H9A1 | 1.071 (3) | 1.0774 (16) | 0.081 (2) | 0.037 (6)* | 0.94 (4) |
H15A | 1.0568 (13) | 0.8547 (12) | 0.2701 (12) | 0.011 (4)* | 0.94 (4) |
H15B | 0.9557 (18) | 0.9002 (17) | 0.3340 (16) | 0.039 (6)* | 0.94 (4) |
H16A | 1.1111 (16) | 1.0277 (14) | 0.4158 (15) | 0.032 (5)* | 0.94 (4) |
H16B | 1.1595 (14) | 0.9103 (14) | 0.4738 (14) | 0.016 (4)* | 0.94 (4) |
H17A | 1.4115 (19) | 0.9659 (19) | 0.4500 (18) | 0.045 (6)* | 0.94 (4) |
H17B | 1.3440 (12) | 0.9350 (11) | 0.5390 (12) | 0.000 (4)* | 0.94 (4) |
H18A | 1.2851 (18) | 1.1028 (15) | 0.5339 (16) | 0.035 (6)* | 0.94 (4) |
H18B | 1.428 (2) | 1.0912 (18) | 0.5913 (19) | 0.044 (6)* | 0.94 (4) |
H19A | 1.4414 (18) | 1.2429 (16) | 0.5343 (17) | 0.036 (5)* | 0.94 (4) |
H19B | 1.2888 (16) | 1.2507 (14) | 0.4739 (14) | 0.025 (5)* | 0.94 (4) |
H20A | 1.3919 (13) | 1.3613 (12) | 0.4041 (12) | 0.011 (4)* | 0.94 (4) |
H20B | 1.4432 (14) | 1.2519 (13) | 0.3490 (13) | 0.026 (5)* | 0.94 (4) |
H21A | 1.2101 (17) | 1.4075 (17) | 0.3021 (16) | 0.035 (5)* | 0.94 (4) |
H21B | 1.1324 (19) | 1.3023 (17) | 0.3046 (17) | 0.036 (5)* | 0.94 (4) |
H22A | 1.0322 (14) | 1.4147 (14) | 0.1394 (13) | 0.023 (5)* | 0.94 (4) |
H22B | 1.1379 (15) | 1.3773 (13) | 0.0982 (13) | 0.019 (5)* | 0.94 (4) |
H23A | 0.6141 (15) | 0.9877 (13) | −0.2659 (14) | 0.024 (5)* | 0.94 (4) |
H23B | 0.761 (2) | 1.0395 (18) | −0.230 (2) | 0.053 (7)* | 0.94 (4) |
H23C | 0.6311 (15) | 1.0976 (14) | −0.3194 (15) | 0.030 (5)* | 0.94 (4) |
H24A | 0.5348 (18) | 1.1520 (17) | −0.0984 (19) | 0.045 (6)* | 0.94 (4) |
H24B | 0.4868 (16) | 1.0636 (15) | −0.1914 (14) | 0.023 (5)* | 0.94 (4) |
H24C | 0.5045 (13) | 1.1675 (14) | −0.2422 (14) | 0.023 (5)* | 0.94 (4) |
OWA | 1.2233 (9) | 1.0882 (9) | 0.1936 (9) | 0.017 (3)* | 0.83 (4) |
HWA1 | 1.2353 (16) | 1.1577 (14) | 0.2101 (16) | 0.026 (5)* | 0.94 (4) |
HWA2 | 1.2411 | 1.0636 | 0.2599 | 0.023 (5)* | 0.94 (4) |
O1B | 0.9734 (9) | 1.0879 (8) | 0.7188 (9) | 0.012 (3)* | 0.83 (4) |
C1B | 0.8698 (8) | 1.1051 (7) | 0.6283 (8) | 0.010 (2)* | 1.06 (5) |
C2B | 0.8031 (9) | 1.1869 (8) | 0.6180 (8) | 0.017 (3)* | 1.06 (5) |
C3B | 0.6934 (9) | 1.1942 (8) | 0.5191 (9) | 0.018 (3)* | 1.06 (5) |
C4B | 0.6506 (9) | 1.1274 (8) | 0.4418 (9) | 0.016 (3)* | 1.06 (5) |
C5B | 0.7085 (9) | 0.8125 (8) | 0.3163 (8) | 0.012 (2)* | 1.06 (5) |
C6B | 0.7784 (7) | 0.7261 (7) | 0.3416 (7) | 0.003 (2)* | 1.06 (5) |
C7B | 0.8873 (9) | 0.7214 (9) | 0.4337 (8) | 0.016 (3)* | 1.06 (5) |
O8B | 1.0294 (8) | 0.8019 (8) | 0.6002 (7) | 0.006 (3)* | 0.83 (4) |
C8B | 0.9271 (7) | 0.7975 (7) | 0.5094 (7) | 0.002 (2)* | 1.06 (5) |
O9B | 1.0000 (9) | 1.0033 (8) | 0.5245 (7) | 0.009 (3)* | 0.83 (4) |
C9B | 0.9169 (7) | 0.9626 (7) | 0.5562 (7) | 0.003 (2)* | 1.06 (5) |
C10B | 0.6715 (7) | 0.9755 (7) | 0.3573 (6) | 0.002 (2)* | 1.06 (5) |
C11B | 0.7488 (8) | 0.8868 (7) | 0.3854 (7) | 0.009 (2)* | 1.06 (5) |
C12B | 0.8613 (8) | 0.8831 (7) | 0.4857 (7) | 0.010 (2)* | 1.06 (5) |
C13B | 0.8294 (8) | 1.0388 (7) | 0.5426 (8) | 0.013 (3)* | 1.06 (5) |
C14B | 0.7211 (7) | 1.0496 (6) | 0.4515 (7) | 0.001 (2)* | 1.06 (5) |
C15B | 1.0925 (8) | 0.7181 (8) | 0.6450 (8) | 0.017 (2)* | 1.06 (5) |
O16B | 1.2731 (10) | 0.7867 (8) | 0.7657 (9) | 0.019 (3)* | 0.83 (4) |
C16B | 1.1778 (8) | 0.7292 (7) | 0.7636 (7) | 0.012 (2)* | 1.06 (5) |
C17B | 1.3786 (8) | 0.7797 (7) | 0.8757 (7) | 0.009 (2)* | 1.06 (5) |
O18B | 1.3555 (9) | 0.9309 (8) | 0.9324 (8) | 0.010 (3)* | 0.83 (4) |
C18B | 1.3669 (9) | 0.8383 (7) | 0.9646 (8) | 0.008 (2)* | 1.06 (5) |
C19B | 1.3509 (9) | 0.9916 (8) | 1.0128 (9) | 0.019 (3)* | 1.06 (5) |
O20B | 1.2316 (8) | 1.1126 (7) | 0.8767 (8) | 0.006 (3)* | 0.83 (4) |
C20B | 1.3403 (9) | 1.0906 (8) | 0.9756 (9) | 0.016 (3)* | 1.06 (5) |
C21B | 1.1318 (8) | 1.1146 (7) | 0.8986 (8) | 0.010 (2)* | 1.06 (5) |
C22B | 1.0256 (8) | 1.1579 (7) | 0.7996 (8) | 0.010 (2)* | 1.06 (5) |
C23B | 0.6718 (8) | 1.0206 (7) | 0.2541 (7) | 0.006 (2)* | 1.06 (5) |
C24B | 0.5472 (8) | 0.9471 (7) | 0.3330 (8) | 0.007 (2)* | 1.06 (5) |
H4B | 0.5696 (18) | 1.1413 (15) | 0.3726 (17) | 0.039 (6)* | 0.94 (4) |
H3B | 0.6450 (14) | 1.2614 (11) | 0.5116 (13) | 0.010 (4)* | 0.94 (4) |
H2B | 0.8243 (15) | 1.2366 (16) | 0.6713 (16) | 0.031 (5)* | 0.94 (4) |
H6B | 0.7459 (16) | 0.6684 (16) | 0.2889 (17) | 0.030 (5)* | 0.94 (4) |
H5B | 0.636 (2) | 0.8165 (18) | 0.2401 (19) | 0.049 (6)* | 0.94 (4) |
H7B | 0.9317 (19) | 0.6637 (19) | 0.4523 (18) | 0.038 (6)* | 0.94 (4) |
H9B | 0.9553 (13) | 0.9325 (11) | 0.6423 (12) | 0.009 (4)* | 0.94 (4) |
H15C | 1.1305 (16) | 0.6806 (14) | 0.5991 (15) | 0.030 (5)* | 0.94 (4) |
H15D | 1.0165 (13) | 0.6661 (12) | 0.6469 (13) | 0.018 (4)* | 0.94 (4) |
H16C | 1.1334 (15) | 0.7673 (14) | 0.8086 (15) | 0.021 (4)* | 0.94 (4) |
H16D | 1.2112 (14) | 0.6672 (14) | 0.8121 (14) | 0.019 (4)* | 0.94 (4) |
H17C | 1.4541 (13) | 0.8028 (11) | 0.8647 (11) | 0.014 (4)* | 0.94 (4) |
H17D | 1.4063 (19) | 0.7119 (18) | 0.8970 (17) | 0.047 (6)* | 0.94 (4) |
H18C | 1.2963 (15) | 0.8103 (13) | 0.9810 (13) | 0.019 (5)* | 0.94 (4) |
H18D | 1.4551 (15) | 0.8286 (14) | 1.0456 (14) | 0.026 (5)* | 0.94 (4) |
H19C | 1.4296 (15) | 0.9860 (13) | 1.0900 (15) | 0.017 (5)* | 0.94 (4) |
H19D | 1.2667 (13) | 0.9754 (11) | 1.0266 (12) | 0.012 (4)* | 0.94 (4) |
H20C | 1.348 (2) | 1.137 (2) | 1.044 (2) | 0.066 (8)* | 0.94 (4) |
H20D | 1.4092 (14) | 1.1034 (13) | 0.9510 (13) | 0.016 (4)* | 0.94 (4) |
H21C | 1.1056 (14) | 1.0536 (12) | 0.9267 (12) | 0.016 (4)* | 0.94 (4) |
H21D | 1.1499 (19) | 1.1637 (19) | 0.9662 (19) | 0.045 (6)* | 0.94 (4) |
H22C | 0.9596 (14) | 1.1767 (13) | 0.8278 (12) | 0.015 (4)* | 0.94 (4) |
H22D | 1.0378 (17) | 1.2195 (17) | 0.7669 (16) | 0.037 (5)* | 0.94 (4) |
H23D | 0.7698 (15) | 1.0413 (12) | 0.2734 (14) | 0.015 (4)* | 0.94 (4) |
H23E | 0.6298 (17) | 1.0817 (17) | 0.2301 (16) | 0.035 (5)* | 0.94 (4) |
H23F | 0.6521 (14) | 0.9706 (14) | 0.1916 (14) | 0.022 (4)* | 0.94 (4) |
H24D | 0.5086 (14) | 0.8944 (15) | 0.2705 (16) | 0.028 (5)* | 0.94 (4) |
H24E | 0.4833 (19) | 1.0078 (17) | 0.3096 (17) | 0.039 (5)* | 0.94 (4) |
H24F | 0.5480 (14) | 0.9120 (14) | 0.4046 (14) | 0.022 (5)* | 0.94 (4) |
H9B1 | 1.0850 (14) | 0.9887 (11) | 0.5922 (12) | 0.009 (4)* | 0.94 (4) |
OWB | 1.2310 (9) | 0.9760 (9) | 0.6960 (9) | 0.013 (3)* | 0.83 (4) |
HWB1 | 1.2264 (16) | 1.0171 (14) | 0.7547 (15) | 0.047 (6)* | 0.94 (4) |
HWB2 | 1.2508 (17) | 0.9192 (17) | 0.7269 (17) | 0.034 (5)* | 0.94 (4) |
C10A—C14A | 1.51 (2) | C10B—C24B | 1.503 (13) |
C10A—C11A | 1.514 (15) | C10B—C23B | 1.549 (13) |
C10A—C24A | 1.563 (14) | C10B—C14B | 1.564 (13) |
C10A—C23A | 1.560 (15) | C10B—C11B | 1.549 (15) |
C23A—H23A | 1.20 (2) | C23B—H23D | 1.18 (2) |
C23A—H23B | 0.97 (3) | C23B—H23E | 1.00 (3) |
C23A—H23C | 1.14 (2) | C23B—H23F | 1.06 (2) |
C24A—H24A | 1.09 (3) | C24B—H24D | 1.08 (3) |
C24A—H24B | 1.04 (3) | C24B—H24E | 1.13 (3) |
C24A—H24C | 1.12 (2) | C24B—H24F | 1.09 (2) |
C14A—C13A | 1.349 (12) | C14B—C13B | 1.371 (13) |
C14A—C4A | 1.450 (14) | C14B—C4B | 1.402 (15) |
C4A—C3A | 1.317 (14) | C4B—C3B | 1.35 (2) |
C4A—H4A | 1.10 (2) | C4B—H4B | 1.04 (3) |
C3A—C2A | 1.432 (13) | C3B—C2B | 1.426 (15) |
C3A—H3A | 1.09 (2) | C3B—H3B | 1.13 (2) |
C2A—C1A | 1.358 (14) | C2B—C1B | 1.42 (2) |
C2A—H2A | 1.14 (2) | C2B—H2B | 0.97 (3) |
C1A—C13A | 1.368 (14) | C1B—O1B | 1.347 (14) |
C1A—O1A | 1.427 (14) | C1B—C13B | 1.412 (15) |
C13A—C9A | 1.565 (14) | C13B—C9B | 1.511 (14) |
C9A—C12A | 1.466 (14) | C9B—O9B | 1.428 (14) |
C9A—O9A | 1.48 (2) | C9B—C12B | 1.455 (14) |
C9A—H9A | 1.06 (2) | C9B—H9B | 1.13 (2) |
O9A—H9A1 | 0.73 (4) | O9B—H9B1 | 1.07 (2) |
C12A—C11A | 1.408 (14) | C12B—C8B | 1.442 (14) |
C12A—C8A | 1.435 (13) | C12B—C11B | 1.453 (12) |
C8A—C7A | 1.373 (14) | C8B—O8B | 1.319 (12) |
C8A—O8A | 1.375 (14) | C8B—C7B | 1.432 (14) |
C7A—C6A | 1.380 (13) | C7B—C6B | 1.374 (13) |
C7A—H7A | 1.16 (2) | C7B—H7B | 0.97 (3) |
C6A—C5A | 1.455 (14) | C6B—C5B | 1.475 (15) |
C6A—H6A | 1.01 (3) | C6B—H6B | 1.05 (3) |
C5A—C11A | 1.42 (2) | C5B—C11B | 1.363 (15) |
C5A—H5A | 1.05 (2) | C5B—H5B | 1.02 (3) |
O8A—C15A | 1.44 (2) | O8B—C15B | 1.43 (2) |
C15A—C16A | 1.490 (14) | C15B—C16B | 1.483 (14) |
C15A—H15A | 1.20 (2) | C15B—H15C | 1.09 (2) |
C15A—H15B | 1.11 (3) | C15B—H15D | 1.23 (2) |
C16A—O16A | 1.451 (15) | C16B—O16B | 1.451 (15) |
C16A—H16A | 1.14 (2) | C16B—H16C | 1.14 (2) |
C16A—H16B | 1.10 (2) | C16B—H16D | 1.08 (2) |
O16A—C17A | 1.378 (14) | O16B—C17B | 1.483 (14) |
C17A—C18A | 1.54 (2) | C17B—C18B | 1.536 (15) |
C17A—H17A | 1.14 (3) | C17B—H17C | 1.08 (2) |
C17A—H17B | 1.12 (2) | C17B—H17D | 1.04 (3) |
C18A—O18A | 1.41 (2) | C18B—O18B | 1.40 (2) |
C18A—H18A | 0.99 (3) | C18B—H18C | 1.09 (2) |
C18A—H18B | 1.09 (3) | C18B—H18D | 1.16 (2) |
O18A—C19A | 1.44 (2) | O18B—C19B | 1.42 (2) |
C19A—C20A | 1.53 (2) | C19B—C20B | 1.50 (2) |
C19A—H19A | 1.02 (3) | C19B—H19C | 1.07 (2) |
C19A—H19B | 1.12 (2) | C19B—H19D | 1.18 (2) |
C20A—O20A | 1.356 (13) | C20B—O20B | 1.450 (14) |
C20A—H20A | 1.15 (2) | C20B—H20C | 1.12 (4) |
C20A—H20B | 1.13 (2) | C20B—H20D | 1.08 (2) |
O20A—C21A | 1.404 (14) | O20B—C21B | 1.419 (13) |
C21A—C22A | 1.549 (12) | C21B—C22B | 1.534 (14) |
C21A—H21A | 1.13 (3) | C21B—H21C | 1.07 (2) |
C21A—H21B | 1.05 (3) | C21B—H21D | 1.10 (3) |
C22A—O1A | 1.40 (2) | C22B—O1B | 1.42 (2) |
C22A—H22A | 1.00 (2) | C22B—H22C | 1.10 (2) |
C22A—H22B | 1.15 (2) | C22B—H22D | 1.04 (3) |
OWA—HWA1 | 1.03 (3) | OWB—HWB1 | 1.02 (3) |
OWA—HWA2 | 0.897 (11) | OWB—HWB2 | 0.91 (3) |
C14A—C10A—C11A | 113.1 (7) | C24B—C10B—C23B | 110.4 (7) |
C14A—C10A—C24A | 111.1 (9) | C24B—C10B—C14B | 110.8 (7) |
C11A—C10A—C24A | 107.3 (7) | C23B—C10B—C14B | 106.7 (8) |
C14A—C10A—C23A | 106.7 (7) | C24B—C10B—C11B | 107.6 (8) |
C11A—C10A—C23A | 108.2 (9) | C23B—C10B—C11B | 108.1 (7) |
C24A—C10A—C23A | 110.4 (8) | C14B—C10B—C11B | 113.2 (6) |
C10A—C23A—H23A | 104.6 (11) | C10B—C23B—H23D | 109.9 (11) |
C10A—C23A—H23B | 113.8 (17) | C10B—C23B—H23E | 116.5 (12) |
H23A—C23A—H23B | 115 (2) | H23D—C23B—H23E | 101.2 (17) |
C10A—C23A—H23C | 111.4 (14) | C10B—C23B—H23F | 110.0 (13) |
H23A—C23A—H23C | 100.3 (15) | H23D—C23B—H23F | 101.1 (14) |
H23B—C23A—H23C | 110.8 (19) | H23E—C23B—H23F | 116.5 (17) |
C10A—C24A—H24A | 112.2 (14) | C10B—C24B—H24D | 114.7 (11) |
C10A—C24A—H24B | 113.0 (14) | C10B—C24B—H24E | 112.7 (14) |
H24A—C24A—H24B | 106.3 (18) | H24D—C24B—H24E | 108.6 (17) |
C10A—C24A—H24C | 108.6 (10) | C10B—C24B—H24F | 110.2 (12) |
H24A—C24A—H24C | 111.5 (18) | H24D—C24B—H24F | 101.0 (17) |
H24B—C24A—H24C | 105.0 (16) | H24E—C24B—H24F | 109.0 (17) |
C13A—C14A—C4A | 115.6 (8) | C13B—C14B—C4B | 120.2 (9) |
C13A—C14A—C10A | 125.2 (9) | C13B—C14B—C10B | 121.5 (8) |
C4A—C14A—C10A | 119.1 (7) | C4B—C14B—C10B | 118.3 (7) |
C3A—C4A—C14A | 120.3 (8) | C3B—C4B—C14B | 119.4 (9) |
C3A—C4A—H4A | 120.9 (12) | C3B—C4B—H4B | 116.4 (16) |
C14A—C4A—H4A | 118.7 (12) | C14B—C4B—H4B | 123.7 (15) |
C4A—C3A—C2A | 122.9 (9) | C4B—C3B—C2B | 123.7 (10) |
C4A—C3A—H3A | 120.1 (13) | C4B—C3B—H3B | 122.7 (13) |
C2A—C3A—H3A | 117.0 (13) | C2B—C3B—H3B | 113.6 (12) |
C1A—C2A—C3A | 115.4 (9) | C3B—C2B—C1B | 115.5 (10) |
C1A—C2A—H2A | 123.4 (11) | C3B—C2B—H2B | 118.0 (15) |
C3A—C2A—H2A | 120.5 (11) | C1B—C2B—H2B | 126.5 (14) |
C2A—C1A—C13A | 121.8 (7) | O1B—C1B—C13B | 117.6 (10) |
C2A—C1A—O1A | 120.4 (9) | O1B—C1B—C2B | 121.8 (10) |
C13A—C1A—O1A | 117.5 (9) | C13B—C1B—C2B | 120.6 (8) |
C14A—C13A—C1A | 123.5 (8) | C14B—C13B—C1B | 120.3 (9) |
C14A—C13A—C9A | 119.6 (8) | C14B—C13B—C9B | 124.4 (9) |
C1A—C13A—C9A | 116.8 (7) | C1B—C13B—C9B | 115.2 (8) |
C12A—C9A—O9A | 110.1 (9) | O9B—C9B—C12B | 109.1 (8) |
C12A—C9A—C13A | 114.1 (8) | O9B—C9B—C13B | 104.9 (8) |
O9A—C9A—C13A | 107.9 (8) | C12B—C9B—C13B | 112.9 (7) |
C12A—C9A—H9A | 109.6 (13) | O9B—C9B—H9B | 116.4 (11) |
O9A—C9A—H9A | 99.0 (12) | C12B—C9B—H9B | 103.2 (11) |
C13A—C9A—H9A | 115.1 (14) | C13B—C9B—H9B | 110.6 (11) |
C9A—O9A—H9A1 | 114.0 (17) | C9B—O9B—H9B1 | 104.1 (11) |
C11A—C12A—C8A | 119.7 (8) | C8B—C12B—C11B | 117.2 (8) |
C11A—C12A—C9A | 122.8 (8) | C8B—C12B—C9B | 118.4 (7) |
C8A—C12A—C9A | 117.1 (8) | C11B—C12B—C9B | 124.1 (8) |
C7A—C8A—O8A | 127.4 (9) | O8B—C8B—C12B | 112.6 (8) |
C7A—C8A—C12A | 120.7 (8) | O8B—C8B—C7B | 125.6 (9) |
O8A—C8A—C12A | 111.9 (9) | C12B—C8B—C7B | 121.5 (7) |
C8A—C7A—C6A | 121.2 (9) | C6B—C7B—C8B | 119.5 (10) |
C8A—C7A—H7A | 117.5 (11) | C6B—C7B—H7B | 119.8 (16) |
C6A—C7A—H7A | 121.0 (11) | C8B—C7B—H7B | 120.2 (15) |
C7A—C6A—C5A | 119.6 (9) | C7B—C6B—C5B | 119.8 (9) |
C7A—C6A—H6A | 123.8 (16) | C7B—C6B—H6B | 119.8 (14) |
C5A—C6A—H6A | 116.6 (16) | C5B—C6B—H6B | 120.4 (13) |
C11A—C5A—C6A | 119.3 (9) | C11B—C5B—C6B | 120.7 (8) |
C11A—C5A—H5A | 118.0 (14) | C11B—C5B—H5B | 122.1 (17) |
C6A—C5A—H5A | 122.4 (13) | C6B—C5B—H5B | 116.6 (16) |
C12A—C11A—C5A | 119.2 (9) | C5B—C11B—C12B | 121.0 (9) |
C12A—C11A—C10A | 121.6 (9) | C5B—C11B—C10B | 119.2 (7) |
C5A—C11A—C10A | 118.7 (8) | C12B—C11B—C10B | 119.8 (8) |
C8A—O8A—C15A | 115.1 (9) | C8B—O8B—C15B | 118.4 (9) |
O8A—C15A—C16A | 110.5 (9) | O8B—C15B—C16B | 111.0 (9) |
O8A—C15A—H15A | 104.0 (11) | O8B—C15B—H15C | 119.0 (13) |
C16A—C15A—H15A | 104.1 (10) | C16B—C15B—H15C | 112.8 (12) |
O8A—C15A—H15B | 114.6 (14) | O8B—C15B—H15D | 103.9 (11) |
C16A—C15A—H15B | 107.7 (12) | C16B—C15B—H15D | 103.3 (10) |
H15A—C15A—H15B | 115.4 (17) | H15C—C15B—H15D | 105.0 (16) |
O16A—C16A—C15A | 113.0 (8) | C15B—C16B—O16B | 105.5 (8) |
O16A—C16A—H16A | 101.8 (13) | C15B—C16B—H16C | 110.2 (11) |
C15A—C16A—H16A | 107.5 (11) | O16B—C16B—H16C | 108.5 (13) |
O16A—C16A—H16B | 108.8 (12) | C15B—C16B—H16D | 117.5 (13) |
C15A—C16A—H16B | 113.1 (13) | O16B—C16B—H16D | 112.0 (12) |
H16A—C16A—H16B | 112.1 (15) | H16C—C16B—H16D | 103.0 (15) |
C17A—O16A—C16A | 111.4 (9) | C17B—O16B—C16B | 109.5 (9) |
O16A—C17A—C18A | 112.5 (9) | O16B—C17B—C18B | 113.1 (8) |
O16A—C17A—H17A | 108.1 (13) | O16B—C17B—H17C | 106.3 (11) |
C18A—C17A—H17A | 109.0 (16) | C18B—C17B—H17C | 110.2 (12) |
O16A—C17A—H17B | 112.8 (12) | O16B—C17B—H17D | 112.2 (15) |
C18A—C17A—H17B | 106.2 (11) | C18B—C17B—H17D | 116.3 (13) |
H17A—C17A—H17B | 108.0 (16) | H17C—C17B—H17D | 97.1 (16) |
O18A—C18A—C17A | 104.8 (9) | O18B—C18B—C17B | 108.4 (8) |
O18A—C18A—H18A | 111.6 (14) | O18B—C18B—H18C | 116.4 (13) |
C17A—C18A—H18A | 116.9 (15) | C17B—C18B—H18C | 109.6 (13) |
O18A—C18A—H18B | 109.8 (16) | O18B—C18B—H18D | 109.3 (13) |
C17A—C18A—H18B | 112.6 (16) | C17B—C18B—H18D | 106.6 (12) |
H18A—C18A—H18B | 101.2 (19) | H18C—C18B—H18D | 106.2 (14) |
C19A—O18A—C18A | 111.6 (10) | C19B—O18B—C18B | 112.7 (9) |
O18A—C19A—C20A | 108.5 (9) | O18B—C19B—C20B | 110.9 (10) |
O18A—C19A—H19A | 111.9 (16) | O18B—C19B—H19C | 111.2 (14) |
C20A—C19A—H19A | 110.8 (15) | C20B—C19B—H19C | 107.7 (14) |
O18A—C19A—H19B | 104.6 (14) | O18B—C19B—H19D | 110.6 (12) |
C20A—C19A—H19B | 113.8 (13) | C20B—C19B—H19D | 107.1 (12) |
H19A—C19A—H19B | 107.2 (16) | H19C—C19B—H19D | 109.1 (15) |
O20A—C20A—C19A | 115.2 (8) | O20B—C20B—C19B | 115.0 (10) |
O20A—C20A—H20A | 108.3 (11) | O20B—C20B—H20C | 109.1 (17) |
C19A—C20A—H20A | 101.7 (10) | C19B—C20B—H20C | 109.5 (18) |
O20A—C20A—H20B | 103.8 (11) | O20B—C20B—H20D | 103.3 (12) |
C19A—C20A—H20B | 107.3 (12) | C19B—C20B—H20D | 107.9 (14) |
H20A—C20A—H20B | 121.1 (14) | H20C—C20B—H20D | 112 (2) |
C20A—O20A—C21A | 117.3 (9) | C21B—O20B—C20B | 111.4 (8) |
O20A—C21A—C22A | 112.2 (7) | O20B—C21B—C22B | 109.1 (8) |
O20A—C21A—H21A | 106.8 (12) | O20B—C21B—H21C | 120.3 (13) |
C22A—C21A—H21A | 102.0 (13) | C22B—C21B—H21C | 111.2 (11) |
O20A—C21A—H21B | 113.6 (15) | O20B—C21B—H21D | 108.8 (14) |
C22A—C21A—H21B | 108.5 (13) | C22B—C21B—H21D | 103.7 (15) |
H21A—C21A—H21B | 113.3 (17) | H21C—C21B—H21D | 102.3 (17) |
O1A—C22A—C21A | 103.0 (8) | O1B—C22B—C21B | 107.4 (9) |
O1A—C22A—H22A | 118.3 (12) | O1B—C22B—H22C | 106.8 (12) |
C21A—C22A—H22A | 114.5 (11) | C21B—C22B—H22C | 107.0 (11) |
O1A—C22A—H22B | 104.7 (12) | O1B—C22B—H22D | 112.9 (15) |
C21A—C22A—H22B | 107.2 (10) | C21B—C22B—H22D | 119.0 (13) |
H22A—C22A—H22B | 108.3 (15) | H22C—C22B—H22D | 102.9 (17) |
C22A—O1A—C1A | 119.5 (10) | C1B—O1B—C22B | 119.3 (10) |
HWA1—OWA—HWA2 | 102.9 (14) | HWB1—OWB—HWB2 | 105.6 (18) |
C11A—C10A—C14A—C13A | 11.4 (13) | C24B—C10B—C14B—C13B | 128.0 (9) |
C24A—C10A—C14A—C13A | 132.1 (9) | C23B—C10B—C14B—C13B | −111.8 (9) |
C23A—C10A—C14A—C13A | −107.5 (10) | C11B—C10B—C14B—C13B | 7.0 (11) |
C11A—C10A—C14A—C4A | −172.4 (7) | C24B—C10B—C14B—C4B | −50.7 (10) |
C24A—C10A—C14A—C4A | −51.7 (10) | C23B—C10B—C14B—C4B | 69.5 (9) |
C23A—C10A—C14A—C4A | 68.7 (10) | C11B—C10B—C14B—C4B | −171.7 (8) |
C13A—C14A—C4A—C3A | −1.5 (13) | C13B—C14B—C4B—C3B | 4.2 (14) |
C10A—C14A—C4A—C3A | −178.1 (8) | C10B—C14B—C4B—C3B | −177.1 (8) |
C14A—C4A—C3A—C2A | −3.9 (14) | C14B—C4B—C3B—C2B | −6.5 (16) |
C4A—C3A—C2A—C1A | 7.5 (13) | C4B—C3B—C2B—C1B | 3.1 (15) |
C3A—C2A—C1A—C13A | −5.8 (13) | C3B—C2B—C1B—O1B | −178.0 (9) |
C3A—C2A—C1A—O1A | −179.2 (8) | C3B—C2B—C1B—C13B | 2.4 (14) |
C4A—C14A—C13A—C1A | 3.2 (12) | C4B—C14B—C13B—C1B | 1.1 (13) |
C10A—C14A—C13A—C1A | 179.5 (9) | C10B—C14B—C13B—C1B | −177.6 (8) |
C4A—C14A—C13A—C9A | −173.3 (8) | C4B—C14B—C13B—C9B | −174.0 (9) |
C10A—C14A—C13A—C9A | 3.0 (13) | C10B—C14B—C13B—C9B | 7.3 (13) |
C2A—C1A—C13A—C14A | 0.6 (15) | O1B—C1B—C13B—C14B | 176.0 (9) |
O1A—C1A—C13A—C14A | 174.2 (9) | C2B—C1B—C13B—C14B | −4.4 (14) |
C2A—C1A—C13A—C9A | 177.3 (7) | O1B—C1B—C13B—C9B | −8.5 (12) |
O1A—C1A—C13A—C9A | −9.2 (13) | C2B—C1B—C13B—C9B | 171.2 (8) |
C14A—C13A—C9A—C12A | −17.6 (13) | C14B—C13B—C9B—O9B | 97.2 (10) |
C1A—C13A—C9A—C12A | 165.6 (7) | C1B—C13B—C9B—O9B | −78.2 (10) |
C14A—C13A—C9A—O9A | 105.1 (10) | C14B—C13B—C9B—C12B | −21.5 (13) |
C1A—C13A—C9A—O9A | −71.7 (12) | C1B—C13B—C9B—C12B | 163.1 (8) |
O9A—C9A—C12A—C11A | −103.4 (10) | O9B—C9B—C12B—C8B | 78.9 (11) |
C13A—C9A—C12A—C11A | 18.1 (13) | C13B—C9B—C12B—C8B | −164.9 (7) |
O9A—C9A—C12A—C8A | 69.3 (11) | O9B—C9B—C12B—C11B | −94.0 (10) |
C13A—C9A—C12A—C8A | −169.2 (8) | C13B—C9B—C12B—C11B | 22.3 (12) |
C11A—C12A—C8A—C7A | 3.4 (13) | C11B—C12B—C8B—O8B | 178.1 (8) |
C9A—C12A—C8A—C7A | −169.5 (9) | C9B—C12B—C8B—O8B | 4.8 (12) |
C11A—C12A—C8A—O8A | −177.8 (8) | C11B—C12B—C8B—C7B | 3.9 (13) |
C9A—C12A—C8A—O8A | 9.3 (11) | C9B—C12B—C8B—C7B | −169.4 (7) |
O8A—C8A—C7A—C6A | 178.4 (9) | O8B—C8B—C7B—C6B | −179.7 (9) |
C12A—C8A—C7A—C6A | −3.0 (14) | C12B—C8B—C7B—C6B | −6.4 (14) |
C8A—C7A—C6A—C5A | 3.3 (13) | C8B—C7B—C6B—C5B | 5.4 (14) |
C7A—C6A—C5A—C11A | −4.1 (13) | C7B—C6B—C5B—C11B | −2.3 (14) |
C8A—C12A—C11A—C5A | −4.2 (13) | C6B—C5B—C11B—C12B | −0.1 (14) |
C9A—C12A—C11A—C5A | 168.3 (9) | C6B—C5B—C11B—C10B | −178.6 (7) |
C8A—C12A—C11A—C10A | −176.4 (8) | C8B—C12B—C11B—C5B | −0.7 (13) |
C9A—C12A—C11A—C10A | −3.9 (14) | C9B—C12B—C11B—C5B | 172.2 (9) |
C6A—C5A—C11A—C12A | 4.5 (13) | C8B—C12B—C11B—C10B | 177.8 (8) |
C6A—C5A—C11A—C10A | 177.0 (8) | C9B—C12B—C11B—C10B | −9.3 (13) |
C14A—C10A—C11A—C12A | −11.0 (13) | C24B—C10B—C11B—C5B | 49.7 (10) |
C24A—C10A—C11A—C12A | −133.9 (10) | C23B—C10B—C11B—C5B | −69.6 (11) |
C23A—C10A—C11A—C12A | 106.9 (10) | C14B—C10B—C11B—C5B | 172.5 (7) |
C14A—C10A—C11A—C5A | 176.7 (8) | C24B—C10B—C11B—C12B | −128.9 (8) |
C24A—C10A—C11A—C5A | 53.8 (11) | C23B—C10B—C11B—C12B | 111.9 (9) |
C23A—C10A—C11A—C5A | −65.4 (11) | C14B—C10B—C11B—C12B | −6.1 (11) |
C7A—C8A—O8A—C15A | −5.6 (14) | C12B—C8B—O8B—C15B | 168.1 (8) |
C12A—C8A—O8A—C15A | 175.7 (8) | C7B—C8B—O8B—C15B | −18.1 (13) |
C8A—O8A—C15A—C16A | −171.9 (8) | C8B—O8B—C15B—C16B | −159.1 (8) |
O8A—C15A—C16A—O16A | −63.0 (12) | O8B—C15B—C16B—O16B | −72.0 (9) |
C15A—C16A—O16A—C17A | −167.3 (9) | C15B—C16B—O16B—C17B | −163.6 (8) |
C16A—O16A—C17A—C18A | −79.0 (12) | C16B—O16B—C17B—C18B | −78.3 (11) |
O16A—C17A—C18A—O18A | −63.9 (11) | O16B—C17B—C18B—O18B | −61.1 (12) |
C17A—C18A—O18A—C19A | −177.6 (9) | C17B—C18B—O18B—C19B | −176.6 (7) |
C18A—O18A—C19A—C20A | 178.1 (8) | C18B—O18B—C19B—C20B | 179.3 (9) |
O18A—C19A—C20A—O20A | 65.1 (13) | O18B—C19B—C20B—O20B | 63.7 (12) |
C19A—C20A—O20A—C21A | 69.1 (12) | C19B—C20B—O20B—C21B | 72.5 (12) |
C20A—O20A—C21A—C22A | 160.8 (8) | C20B—O20B—C21B—C22B | 168.0 (9) |
O20A—C21A—C22A—O1A | 73.4 (10) | O20B—C21B—C22B—O1B | 81.6 (11) |
C21A—C22A—O1A—C1A | 167.4 (8) | C13B—C1B—O1B—C22B | 171.2 (9) |
C2A—C1A—O1A—C22A | 11.0 (14) | C2B—C1B—O1B—C22B | −8.4 (15) |
C13A—C1A—O1A—C22A | −162.7 (9) | C21B—C22B—O1B—C1B | 172.5 (8) |
Experimental details
(xray) | (neutron) | |
Crystal data | ||
Chemical formula | C24H30O6·H2O | C24H30O6·H2O |
Mr | 432.50 | 432.49 |
Crystal system, space group | Monoclinic, P21 | Monoclinic, P21 |
Temperature (K) | 293 | 15 |
a, b, c (Å) | 12.845 (5), 14.575 (3), 13.779 (2) | 12.605 (5), 14.458 (3), 13.588 (2) |
β (°) | 117.72 (2) | 117.12 (2) |
V (Å3) | 2283.6 (11) | 2204.1 (10) |
Z | 4 | 4 |
Radiation type | Cu Kα | ?, λ = 1.538 and 1.312 Å |
µ (mm−1) | 0.75 | 0.00 |
Crystal size (mm) | 0.35 × 0.25 × 0.20 | 2.5 × 1.6 × 0.2 |
Data collection | ||
Diffractometer | Nonius CAD-4 diffractometer | D19 ILL ω diffractometer |
Absorption correction | – | – |
No. of measured, independent and observed [I > 2σ(I)] reflections | 17753, 9092, 4804 | 1931, 1931, 1881 |
Rint | 0.046 | 0.000 |
(sin θ/λ)max (Å−1) | 0.620 | – |
Distance from specimen to detector (mm) | – | h = −10→11, k = 0→13, l = −9→12 |
Refinement | ||
R[F2 > 2σ(F2)], wR(F2), S | 0.062, 0.169, 0.91 | 0.046, 0.132, 0.78 |
No. of reflections | 9092 | 1881 |
No. of parameters | 605 | 507 |
No. of restraints | 217 | 1 |
(Δ/σ)max | 0.078 | −0.123 |
Δρmax, Δρmin (e Å−3) | 0.23, −0.26 | 0.06, −0.06 |
Absolute structure | Flack H D (1983), Acta Cryst. A39, 876-881 | Flack H D (1983), Acta Cryst. A39, 876-881 |
Absolute structure parameter | 0.2 (4) | −10.0 (100) |
Computer programs: CAD-4 EXPRESS88, RETREAT, SHELXS86 (Sheldrick, 1990), SHELXS86? (Sheldrick, 1990), SHELXL92 (Sheldrick, 1993), SHELXL92? (Sheldrick, 1993), SNOOPI.