Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768101010527/bk0091sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768101010527/bk0091tmapyrsup2.hkl |
CCDC reference: 174976
Data collection: Nonius (1997), KappaCCD Collect Program; cell refinement: DENZO-SMN (Otwinowski & Minor 1997); data reduction: HKL DENZO and SCALEPACK (Otwinowski & Minor 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: Molecular Structure Corporation (1999). ORTEP. TEXRAY Structure Analysis Package. MSC, 3200 Research Forest Drive, The Woodlands,TX 77381, USA.; software used to prepare material for publication: SHELXL97 (Sheldrick, 1997), CrystalMaker (Palmer, 1999).
C44H35O14 | Z = 2 |
Mr = 787.72 | F(000) = 822 |
Triclinic, P1 | Dx = 1.393 Mg m−3 |
a = 9.5330 (5) Å | Mo Kα radiation, λ = 0.71070 Å |
b = 13.5400 (7) Å | Cell parameters from 7840 reflections |
c = 14.6440 (9) Å | θ = 2.0–25.0° |
α = 93.880 (2)° | µ = 0.11 mm−1 |
β = 95.020 (2)° | T = 293 K |
γ = 90.140 (3)° | Prism, brown |
V = 1878.57 (18) Å3 | 0.35 × 0.30 × 0.25 mm |
KappaCCD diffractometer | 3827 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.000 |
Graphite monochromator | θmax = 25.0°, θmin = 1.4° |
CCD scans | h = 0→11 |
6639 measured reflections | k = −16→16 |
6639 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)] = 0.058 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.141 | w = 1/[σ2(Fo2) + (0.058P)2 + 0.2978P] where P = (Fo2 + 2Fc2)/3 |
S = 1.02 | (Δ/σ)max = 0.005 |
6639 reflections | Δρmax = 0.24 e Å−3 |
655 parameters | Δρmin = −0.17 e Å−3 |
0 restraints | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.018 (3) |
C44H35O14 | γ = 90.140 (3)° |
Mr = 787.72 | V = 1878.57 (18) Å3 |
Triclinic, P1 | Z = 2 |
a = 9.5330 (5) Å | Mo Kα radiation |
b = 13.5400 (7) Å | µ = 0.11 mm−1 |
c = 14.6440 (9) Å | T = 293 K |
α = 93.880 (2)° | 0.35 × 0.30 × 0.25 mm |
β = 95.020 (2)° |
KappaCCD diffractometer | 3827 reflections with I > 2σ(I) |
6639 measured reflections | Rint = 0.000 |
6639 independent reflections |
R[F2 > 2σ(F2)] = 0.058 | 0 restraints |
wR(F2) = 0.141 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.02 | Δρmax = 0.24 e Å−3 |
6639 reflections | Δρmin = −0.17 e Å−3 |
655 parameters |
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 | ||
C1 | 0.4224 (2) | 0.91240 (17) | 0.24107 (16) | 0.0450 (6) | |
C2 | 0.3746 (3) | 0.94852 (18) | 0.32396 (18) | 0.0478 (6) | |
C3 | 0.4265 (2) | 1.03779 (17) | 0.36599 (16) | 0.0443 (6) | |
C4 | 0.5248 (2) | 1.09116 (18) | 0.32459 (18) | 0.0468 (6) | |
C5 | 0.5716 (2) | 1.05629 (17) | 0.24158 (17) | 0.0458 (6) | |
C6 | 0.5208 (3) | 0.96617 (18) | 0.19998 (19) | 0.0483 (6) | |
C7 | 0.3674 (3) | 0.81756 (18) | 0.19504 (19) | 0.0524 (7) | |
C8 | 0.3794 (3) | 1.07867 (18) | 0.45520 (18) | 0.0500 (6) | |
C9 | 0.6729 (2) | 1.11616 (17) | 0.19628 (18) | 0.0484 (6) | |
O10 | 0.4170 (2) | 0.78509 (13) | 0.12282 (14) | 0.0722 (6) | |
O11 | 0.2711 (2) | 0.77369 (14) | 0.23194 (14) | 0.0729 (6) | |
O12 | 0.2810 (2) | 1.02586 (14) | 0.48618 (14) | 0.0685 (6) | |
O13 | 0.4304 (2) | 1.15272 (14) | 0.49533 (13) | 0.0705 (6) | |
O14 | 0.71991 (19) | 1.19484 (13) | 0.23637 (13) | 0.0642 (5) | |
O15 | 0.70589 (19) | 1.08326 (14) | 0.11754 (14) | 0.0684 (6) | |
C16 | 0.1915 (2) | 0.46915 (16) | 0.03896 (16) | 0.0437 (6) | |
C17 | 0.0898 (2) | 0.41711 (17) | 0.07887 (18) | 0.0439 (6) | |
C18 | 0.0374 (2) | 0.32817 (16) | 0.03695 (16) | 0.0437 (6) | |
C19 | 0.0879 (3) | 0.29080 (19) | −0.04426 (18) | 0.0482 (6) | |
C20 | 0.1905 (2) | 0.34239 (17) | −0.08451 (17) | 0.0470 (6) | |
C21 | 0.2418 (3) | 0.43170 (18) | −0.04320 (17) | 0.0481 (6) | |
C22 | 0.2436 (3) | 0.56566 (17) | 0.08294 (18) | 0.0477 (6) | |
C23 | −0.0711 (2) | 0.27235 (17) | 0.07904 (18) | 0.0482 (6) | |
C24 | 0.2423 (3) | 0.29838 (19) | −0.17123 (19) | 0.0543 (7) | |
O25 | 0.3396 (2) | 0.61008 (14) | 0.04615 (14) | 0.0746 (6) | |
O26 | 0.19201 (19) | 0.60031 (13) | 0.15391 (13) | 0.0623 (5) | |
O27 | −0.1129 (2) | 0.30864 (13) | 0.15392 (14) | 0.0641 (5) | |
O28 | −0.1180 (2) | 0.19280 (13) | 0.03883 (13) | 0.0681 (6) | |
O29 | 0.2051 (2) | 0.21756 (15) | −0.20487 (14) | 0.0822 (7) | |
O30 | 0.3321 (2) | 0.35434 (14) | −0.20649 (14) | 0.0709 (6) | |
C31 | 0.3055 (4) | 0.1082 (3) | 0.0585 (2) | 0.0851 (10) | |
C32 | 0.3880 (4) | 0.1884 (3) | 0.0657 (2) | 0.0834 (11) | |
C33 | 0.3848 (3) | 0.2630 (2) | 0.1395 (2) | 0.0659 (8) | |
C34 | 0.4688 (4) | 0.3483 (3) | 0.1483 (3) | 0.0891 (11) | |
C35 | 0.4582 (4) | 0.4168 (3) | 0.2189 (4) | 0.0974 (13) | |
C36 | 0.3650 (4) | 0.4057 (3) | 0.2838 (3) | 0.0853 (11) | |
C37 | 0.2783 (3) | 0.3210 (2) | 0.2804 (2) | 0.0611 (7) | |
C38 | 0.1803 (4) | 0.3051 (3) | 0.3458 (2) | 0.0744 (9) | |
C39 | 0.1004 (3) | 0.2242 (3) | 0.3398 (2) | 0.0718 (9) | |
C40 | 0.1074 (3) | 0.1491 (2) | 0.2663 (2) | 0.0592 (7) | |
C41 | 0.0245 (3) | 0.0639 (3) | 0.2594 (3) | 0.0832 (11) | |
C42 | 0.0320 (4) | −0.0041 (3) | 0.1868 (4) | 0.0980 (13) | |
C43 | 0.1213 (4) | 0.0080 (2) | 0.1208 (3) | 0.0881 (11) | |
C44 | 0.2095 (3) | 0.0917 (2) | 0.1249 (2) | 0.0659 (8) | |
C45 | 0.2025 (3) | 0.16312 (18) | 0.19952 (17) | 0.0482 (6) | |
C46 | 0.2882 (3) | 0.24936 (19) | 0.20683 (18) | 0.0506 (6) | |
C47 | 0.7631 (4) | 0.3628 (3) | 0.4108 (4) | 0.0855 (11) | |
C48 | 0.8687 (3) | 0.4360 (2) | 0.4134 (2) | 0.0632 (8) | |
C49 | 0.9461 (2) | 0.46348 (18) | 0.49768 (19) | 0.0513 (6) | |
C50 | 0.9164 (3) | 0.4182 (2) | 0.5787 (2) | 0.0655 (8) | |
C51 | 0.8089 (4) | 0.3467 (3) | 0.5717 (4) | 0.0936 (12) | |
C52 | 0.7353 (4) | 0.3198 (3) | 0.4893 (4) | 0.1012 (14) | |
C53 | 0.9017 (4) | 0.4835 (3) | 0.3339 (3) | 0.0789 (10) | |
C54 | 0.9974 (4) | 0.4486 (3) | 0.6624 (3) | 0.0792 (10) | |
O55 | 0.8316 (2) | 0.89668 (16) | 0.37023 (16) | 0.0750 (6) | |
C56 | 0.9601 (6) | 0.8527 (5) | 0.4014 (4) | 0.1114 (15) | |
O57 | 0.5858 (3) | 0.7016 (2) | 0.36560 (17) | 0.0946 (8) | |
C58 | 0.6061 (6) | 0.6252 (3) | 0.4244 (3) | 0.1074 (13) | |
H58A | 0.7005 | 0.6285 | 0.4533 | 0.30 (4)* | |
H58B | 0.5912 | 0.5627 | 0.3899 | 0.21 (2)* | |
H58C | 0.5406 | 0.6317 | 0.4706 | 0.22 (3)* | |
H2 | 0.302 (3) | 0.9097 (19) | 0.3514 (18) | 0.065 (8)* | |
H4 | 0.559 (3) | 1.155 (2) | 0.3513 (18) | 0.070 (8)* | |
H6 | 0.554 (2) | 0.9401 (17) | 0.1421 (18) | 0.056 (7)* | |
H11 | 0.236 (4) | 0.704 (3) | 0.193 (3) | 0.159 (16)* | |
H12 | 0.248 (3) | 1.056 (2) | 0.540 (2) | 0.093 (11)* | |
H15 | 0.787 (4) | 1.133 (3) | 0.085 (3) | 0.159 (16)* | |
H17 | 0.056 (2) | 0.4431 (16) | 0.1357 (16) | 0.043 (6)* | |
H19 | 0.058 (3) | 0.2310 (19) | −0.0719 (18) | 0.061 (8)* | |
H21 | 0.313 (2) | 0.4710 (16) | −0.0716 (16) | 0.049 (6)* | |
H25 | 0.380 (4) | 0.685 (3) | 0.084 (3) | 0.152 (15)* | |
H27 | −0.184 (5) | 0.255 (4) | 0.192 (3) | 0.189 (19)* | |
H30 | 0.369 (4) | 0.325 (3) | −0.259 (3) | 0.116 (13)* | |
H31 | 0.313 (4) | 0.053 (3) | 0.002 (3) | 0.140 (14)* | |
H32 | 0.450 (3) | 0.195 (2) | 0.022 (2) | 0.078 (9)* | |
H34 | 0.534 (4) | 0.360 (3) | 0.099 (3) | 0.113 (12)* | |
H35 | 0.517 (4) | 0.480 (3) | 0.224 (3) | 0.126 (13)* | |
H36 | 0.351 (3) | 0.450 (3) | 0.334 (2) | 0.096 (12)* | |
H38 | 0.172 (3) | 0.360 (2) | 0.397 (2) | 0.106 (11)* | |
H39 | 0.034 (3) | 0.211 (2) | 0.385 (2) | 0.107 (11)* | |
H41 | −0.040 (4) | 0.051 (2) | 0.307 (3) | 0.110 (12)* | |
H42 | −0.028 (4) | −0.068 (3) | 0.184 (3) | 0.123 (13)* | |
H43 | 0.133 (3) | −0.036 (3) | 0.070 (2) | 0.096 (11)* | |
H47 | 0.713 (4) | 0.348 (3) | 0.352 (3) | 0.117 (14)* | |
H51 | 0.789 (4) | 0.314 (3) | 0.628 (3) | 0.128 (14)* | |
H52 | 0.652 (4) | 0.265 (3) | 0.488 (3) | 0.151 (15)* | |
H53 | 0.847 (3) | 0.460 (2) | 0.276 (2) | 0.092 (11)* | |
H54 | 0.977 (3) | 0.416 (2) | 0.717 (2) | 0.099 (11)* | |
H55 | 0.787 (5) | 0.863 (4) | 0.312 (4) | 0.18 (2)* | |
H56A | 1.012 (5) | 0.840 (4) | 0.356 (4) | 0.17 (2)* | |
H56B | 0.938 (6) | 0.788 (5) | 0.425 (4) | 0.22 (3)* | |
H56C | 1.008 (7) | 0.891 (5) | 0.452 (5) | 0.24 (3)* | |
H57 | 0.594 (5) | 0.758 (4) | 0.403 (3) | 0.153 (18)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0526 (14) | 0.0406 (13) | 0.0418 (15) | −0.0113 (11) | 0.0102 (12) | −0.0043 (11) |
C2 | 0.0535 (15) | 0.0436 (14) | 0.0471 (16) | −0.0100 (12) | 0.0139 (12) | −0.0022 (12) |
C3 | 0.0492 (14) | 0.0410 (13) | 0.0427 (15) | −0.0038 (11) | 0.0086 (11) | −0.0035 (11) |
C4 | 0.0493 (14) | 0.0393 (14) | 0.0517 (17) | −0.0083 (12) | 0.0083 (12) | −0.0027 (12) |
C5 | 0.0481 (14) | 0.0407 (13) | 0.0491 (16) | −0.0077 (11) | 0.0110 (12) | −0.0020 (12) |
C6 | 0.0548 (15) | 0.0443 (14) | 0.0465 (16) | −0.0122 (12) | 0.0155 (13) | −0.0056 (12) |
C7 | 0.0628 (16) | 0.0454 (14) | 0.0502 (17) | −0.0192 (13) | 0.0173 (14) | −0.0020 (13) |
C8 | 0.0572 (15) | 0.0431 (14) | 0.0501 (17) | −0.0035 (13) | 0.0125 (13) | −0.0032 (13) |
C9 | 0.0494 (14) | 0.0416 (14) | 0.0546 (18) | −0.0114 (12) | 0.0142 (13) | −0.0063 (13) |
O10 | 0.0922 (14) | 0.0616 (12) | 0.0640 (13) | −0.0361 (10) | 0.0377 (11) | −0.0240 (10) |
O11 | 0.0982 (15) | 0.0569 (11) | 0.0662 (14) | −0.0397 (11) | 0.0367 (12) | −0.0141 (10) |
O12 | 0.0833 (13) | 0.0672 (12) | 0.0570 (13) | −0.0223 (10) | 0.0322 (11) | −0.0139 (10) |
O13 | 0.0851 (13) | 0.0612 (12) | 0.0651 (13) | −0.0198 (10) | 0.0260 (11) | −0.0218 (10) |
O14 | 0.0691 (12) | 0.0487 (10) | 0.0753 (14) | −0.0252 (9) | 0.0253 (10) | −0.0159 (9) |
O15 | 0.0749 (12) | 0.0677 (12) | 0.0641 (14) | −0.0311 (10) | 0.0319 (10) | −0.0164 (10) |
C16 | 0.0525 (14) | 0.0368 (13) | 0.0417 (15) | −0.0095 (11) | 0.0040 (12) | 0.0026 (11) |
C17 | 0.0498 (14) | 0.0391 (13) | 0.0430 (16) | −0.0066 (11) | 0.0068 (12) | 0.0005 (12) |
C18 | 0.0487 (14) | 0.0388 (13) | 0.0428 (15) | −0.0083 (11) | 0.0027 (11) | −0.0006 (11) |
C19 | 0.0578 (16) | 0.0376 (14) | 0.0481 (17) | −0.0105 (12) | 0.0030 (13) | −0.0020 (12) |
C20 | 0.0544 (15) | 0.0427 (14) | 0.0434 (16) | −0.0112 (12) | 0.0061 (12) | −0.0019 (12) |
C21 | 0.0574 (15) | 0.0441 (14) | 0.0432 (16) | −0.0111 (12) | 0.0090 (13) | 0.0011 (12) |
C22 | 0.0548 (15) | 0.0411 (13) | 0.0472 (16) | −0.0130 (12) | 0.0087 (13) | −0.0018 (12) |
C23 | 0.0524 (14) | 0.0421 (14) | 0.0498 (17) | −0.0149 (12) | 0.0078 (13) | −0.0026 (13) |
C24 | 0.0601 (16) | 0.0525 (16) | 0.0499 (17) | −0.0125 (13) | 0.0097 (13) | −0.0064 (13) |
O25 | 0.0998 (15) | 0.0601 (12) | 0.0660 (14) | −0.0446 (11) | 0.0378 (11) | −0.0184 (10) |
O26 | 0.0785 (12) | 0.0514 (11) | 0.0582 (12) | −0.0219 (9) | 0.0268 (10) | −0.0149 (9) |
O27 | 0.0789 (12) | 0.0519 (11) | 0.0632 (13) | −0.0224 (9) | 0.0274 (10) | −0.0093 (9) |
O28 | 0.0823 (13) | 0.0553 (11) | 0.0673 (13) | −0.0333 (10) | 0.0248 (10) | −0.0148 (10) |
O29 | 0.1092 (16) | 0.0673 (13) | 0.0703 (15) | −0.0345 (12) | 0.0352 (12) | −0.0286 (11) |
O30 | 0.0929 (14) | 0.0602 (12) | 0.0623 (14) | −0.0254 (11) | 0.0354 (12) | −0.0122 (10) |
C31 | 0.108 (3) | 0.091 (3) | 0.059 (2) | 0.024 (2) | 0.018 (2) | 0.003 (2) |
C32 | 0.087 (2) | 0.107 (3) | 0.063 (2) | 0.026 (2) | 0.035 (2) | 0.023 (2) |
C33 | 0.0597 (17) | 0.074 (2) | 0.068 (2) | 0.0035 (15) | 0.0112 (15) | 0.0273 (17) |
C34 | 0.069 (2) | 0.096 (3) | 0.107 (3) | −0.009 (2) | 0.006 (2) | 0.044 (3) |
C35 | 0.079 (3) | 0.082 (3) | 0.130 (4) | −0.027 (2) | −0.016 (3) | 0.033 (3) |
C36 | 0.092 (3) | 0.066 (2) | 0.091 (3) | −0.004 (2) | −0.023 (2) | −0.004 (2) |
C37 | 0.0608 (17) | 0.0546 (17) | 0.065 (2) | 0.0019 (14) | −0.0112 (15) | 0.0014 (15) |
C38 | 0.082 (2) | 0.085 (2) | 0.053 (2) | 0.020 (2) | 0.0050 (17) | −0.0094 (18) |
C39 | 0.071 (2) | 0.091 (3) | 0.058 (2) | 0.0123 (19) | 0.0197 (17) | 0.0154 (19) |
C40 | 0.0570 (16) | 0.0605 (17) | 0.063 (2) | 0.0010 (14) | 0.0085 (14) | 0.0177 (15) |
C41 | 0.067 (2) | 0.079 (3) | 0.107 (3) | −0.0076 (18) | 0.011 (2) | 0.033 (2) |
C42 | 0.085 (3) | 0.072 (3) | 0.136 (4) | −0.018 (2) | −0.003 (3) | 0.017 (3) |
C43 | 0.109 (3) | 0.053 (2) | 0.096 (3) | 0.001 (2) | −0.011 (2) | −0.015 (2) |
C44 | 0.079 (2) | 0.0565 (17) | 0.061 (2) | 0.0092 (15) | 0.0005 (16) | −0.0024 (15) |
C45 | 0.0539 (15) | 0.0465 (14) | 0.0451 (16) | 0.0031 (12) | 0.0049 (12) | 0.0079 (12) |
C46 | 0.0530 (15) | 0.0509 (15) | 0.0488 (17) | 0.0040 (12) | 0.0032 (12) | 0.0113 (13) |
C47 | 0.069 (2) | 0.080 (2) | 0.102 (3) | −0.0017 (19) | 0.006 (2) | −0.035 (2) |
C48 | 0.0599 (17) | 0.0583 (17) | 0.070 (2) | 0.0032 (14) | 0.0102 (16) | −0.0122 (16) |
C49 | 0.0542 (15) | 0.0478 (14) | 0.0524 (17) | 0.0013 (11) | 0.0172 (13) | −0.0086 (13) |
C50 | 0.0724 (19) | 0.0557 (17) | 0.072 (2) | 0.0017 (15) | 0.0310 (17) | −0.0005 (15) |
C51 | 0.104 (3) | 0.069 (2) | 0.116 (4) | −0.012 (2) | 0.058 (3) | 0.008 (2) |
C52 | 0.088 (3) | 0.080 (3) | 0.137 (4) | −0.024 (2) | 0.042 (3) | −0.026 (3) |
C53 | 0.087 (2) | 0.089 (3) | 0.058 (2) | 0.017 (2) | 0.001 (2) | −0.015 (2) |
C54 | 0.106 (3) | 0.080 (2) | 0.057 (2) | 0.015 (2) | 0.029 (2) | 0.010 (2) |
O55 | 0.0800 (15) | 0.0840 (15) | 0.0612 (14) | −0.0085 (12) | 0.0255 (12) | −0.0170 (12) |
C56 | 0.115 (4) | 0.135 (4) | 0.086 (3) | 0.027 (3) | 0.017 (3) | 0.006 (3) |
O57 | 0.143 (2) | 0.0753 (16) | 0.0687 (17) | −0.0128 (15) | 0.0480 (15) | −0.0187 (14) |
C58 | 0.152 (4) | 0.084 (3) | 0.088 (3) | 0.024 (2) | 0.028 (3) | −0.004 (2) |
C1—C6 | 1.388 (3) | C31—C44 | 1.420 (4) |
C1—C2 | 1.392 (3) | C32—C33 | 1.430 (5) |
C1—C7 | 1.482 (3) | C33—C34 | 1.396 (5) |
C2—C3 | 1.388 (3) | C33—C46 | 1.427 (4) |
C3—C4 | 1.387 (3) | C34—C35 | 1.353 (6) |
C3—C8 | 1.490 (3) | C35—C36 | 1.372 (6) |
C4—C5 | 1.385 (3) | C36—C37 | 1.407 (4) |
C5—C6 | 1.393 (3) | C37—C46 | 1.410 (4) |
C5—C9 | 1.487 (3) | C37—C38 | 1.421 (4) |
C7—O10 | 1.249 (3) | C38—C39 | 1.326 (4) |
C7—O11 | 1.271 (3) | C39—C40 | 1.436 (4) |
C8—O13 | 1.206 (3) | C40—C41 | 1.390 (4) |
C8—O12 | 1.308 (3) | C40—C45 | 1.412 (3) |
C9—O14 | 1.244 (3) | C41—C42 | 1.365 (5) |
C9—O15 | 1.274 (3) | C42—C43 | 1.360 (5) |
C16—C17 | 1.389 (3) | C43—C44 | 1.405 (5) |
C16—C21 | 1.398 (3) | C44—C45 | 1.415 (4) |
C16—C22 | 1.482 (3) | C45—C46 | 1.416 (3) |
C17—C18 | 1.386 (3) | C47—C52 | 1.368 (6) |
C18—C19 | 1.387 (3) | C47—C48 | 1.407 (4) |
C18—C23 | 1.480 (3) | C48—C49 | 1.408 (4) |
C19—C20 | 1.395 (3) | C48—C53 | 1.425 (5) |
C20—C21 | 1.383 (3) | C49—C49i | 1.419 (5) |
C20—C24 | 1.490 (3) | C49—C50 | 1.422 (4) |
C22—O26 | 1.252 (3) | C50—C51 | 1.400 (5) |
C22—O25 | 1.272 (3) | C50—C54 | 1.426 (5) |
C23—O28 | 1.254 (3) | C51—C52 | 1.369 (6) |
C23—O27 | 1.268 (3) | C53—C54i | 1.324 (5) |
C24—O29 | 1.209 (3) | C54—C53i | 1.324 (5) |
C24—O30 | 1.304 (3) | O55—C56 | 1.416 (5) |
C31—C32 | 1.333 (5) | O57—C58 | 1.394 (4) |
C6—C1—C2 | 120.0 (2) | C32—C31—C44 | 121.3 (3) |
C6—C1—C7 | 119.4 (2) | C31—C32—C33 | 122.5 (3) |
C2—C1—C7 | 120.7 (2) | C34—C33—C46 | 118.6 (3) |
C3—C2—C1 | 120.0 (2) | C34—C33—C32 | 123.8 (3) |
C4—C3—C2 | 119.7 (2) | C46—C33—C32 | 117.6 (3) |
C4—C3—C8 | 118.5 (2) | C35—C34—C33 | 120.6 (4) |
C2—C3—C8 | 121.8 (2) | C34—C35—C36 | 121.7 (4) |
C5—C4—C3 | 120.6 (2) | C35—C36—C37 | 121.0 (4) |
C4—C5—C6 | 119.6 (2) | C36—C37—C46 | 117.7 (3) |
C4—C5—C9 | 120.0 (2) | C36—C37—C38 | 123.6 (3) |
C6—C5—C9 | 120.4 (2) | C46—C37—C38 | 118.7 (3) |
C1—C6—C5 | 120.0 (2) | C39—C38—C37 | 121.5 (3) |
O10—C7—O11 | 123.6 (2) | C38—C39—C40 | 121.7 (3) |
O10—C7—C1 | 119.0 (2) | C41—C40—C45 | 119.6 (3) |
O11—C7—C1 | 117.4 (2) | C41—C40—C39 | 122.2 (3) |
O13—C8—O12 | 123.7 (2) | C45—C40—C39 | 118.2 (3) |
O13—C8—C3 | 122.4 (2) | C42—C41—C40 | 120.0 (4) |
O12—C8—C3 | 113.9 (2) | C43—C42—C41 | 121.7 (4) |
O14—C9—O15 | 123.8 (2) | C42—C43—C44 | 120.9 (4) |
O14—C9—C5 | 119.0 (2) | C43—C44—C45 | 118.1 (3) |
O15—C9—C5 | 117.3 (2) | C43—C44—C31 | 123.5 (3) |
C17—C16—C21 | 120.1 (2) | C45—C44—C31 | 118.4 (3) |
C17—C16—C22 | 119.5 (2) | C40—C45—C44 | 119.7 (3) |
C21—C16—C22 | 120.4 (2) | C40—C45—C46 | 119.7 (2) |
C18—C17—C16 | 120.0 (2) | C44—C45—C46 | 120.6 (2) |
C17—C18—C19 | 119.8 (2) | C37—C46—C45 | 120.1 (2) |
C17—C18—C23 | 120.3 (2) | C37—C46—C33 | 120.4 (3) |
C19—C18—C23 | 119.9 (2) | C45—C46—C33 | 119.6 (3) |
C18—C19—C20 | 120.5 (2) | C52—C47—C48 | 120.4 (4) |
C21—C20—C19 | 119.7 (2) | C47—C48—C49 | 119.0 (3) |
C21—C20—C24 | 122.0 (2) | C47—C48—C53 | 122.8 (4) |
C19—C20—C24 | 118.3 (2) | C49—C48—C53 | 118.2 (3) |
C20—C21—C16 | 119.9 (2) | C48—C49—C49i | 120.3 (3) |
O26—C22—O25 | 122.7 (2) | C48—C49—C50 | 120.1 (3) |
O26—C22—C16 | 119.4 (2) | C49i—C49—C50 | 119.6 (3) |
O25—C22—C16 | 117.9 (2) | C51—C50—C49 | 118.1 (3) |
O28—C23—O27 | 123.4 (2) | C51—C50—C54 | 123.9 (4) |
O28—C23—C18 | 118.8 (2) | C49—C50—C54 | 118.0 (3) |
O27—C23—C18 | 117.8 (2) | C52—C51—C50 | 121.3 (4) |
O29—C24—O30 | 123.4 (2) | C47—C52—C51 | 121.1 (4) |
O29—C24—C20 | 122.6 (2) | C54i—C53—C48 | 121.9 (4) |
O30—C24—C20 | 114.0 (2) | C53i—C54—C50 | 122.0 (3) |
Symmetry code: (i) −x+2, −y+1, −z+1. |
Experimental details
Crystal data | |
Chemical formula | C44H35O14 |
Mr | 787.72 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 293 |
a, b, c (Å) | 9.5330 (5), 13.5400 (7), 14.6440 (9) |
α, β, γ (°) | 93.880 (2), 95.020 (2), 90.140 (3) |
V (Å3) | 1878.57 (18) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 0.11 |
Crystal size (mm) | 0.35 × 0.30 × 0.25 |
Data collection | |
Diffractometer | KappaCCD diffractometer |
Absorption correction | – |
No. of measured, independent and observed [I > 2σ(I)] reflections | 6639, 6639, 3827 |
Rint | 0.000 |
(sin θ/λ)max (Å−1) | 0.596 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.058, 0.141, 1.02 |
No. of reflections | 6639 |
No. of parameters | 655 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.24, −0.17 |
Computer programs: Nonius (1997), KappaCCD Collect Program, DENZO-SMN (Otwinowski & Minor 1997), HKL DENZO and SCALEPACK (Otwinowski & Minor 1997), SHELXS97 (Sheldrick, 1990), Molecular Structure Corporation (1999). ORTEP. TEXRAY Structure Analysis Package. MSC, 3200 Research Forest Drive, The Woodlands,TX 77381, USA., SHELXL97 (Sheldrick, 1997), CrystalMaker (Palmer, 1999).