Table 1. Crystal data and structure refinement for 1b. Identification code 1b Empirical formula C26 H28 O5 Formula weight 420.48 Temperature 123(2) K Wavelength 0.71073 A Crystal system, space group Orthorhombic, Pna2(1) Unit cell dimensions a = 11.4843(2) A alpha = 90 deg. b = 23.5263(3) A beta = 90 deg. c = 8.04560(10) A gamma = 90 deg. Volume 2173.78(5) A^3 Z, Calculated density 4, 1.285 Mg/m^3 Absorption coefficient 0.088 mm^-1 F(000) 896 Crystal size 0.40 x 0.30 x 0.20 mm Theta range for data collection 2.68 to 28.29 deg. Limiting indices -15<=h<=15, -31<=k<=31, 0<=l<=10 Reflections collected / unique 8443 / 2743 [R(int) = 0.0404] Completeness to theta = 28.29 94.8 % Absorption correction None Max. and min. transmission 0.9826 and 0.9656 Refinement method Full-matrix least-squares on F^2 Data / restraints / parameters 2743 / 1 / 280 Goodness-of-fit on F^2 1.044 Final R indices [I>2sigma(I)] R1 = 0.0528, wR2 = 0.1377 R indices (all data) R1 = 0.0730, wR2 = 0.1497 Absolute structure parameter 0.6(16) Largest diff. peak and hole 0.444 and -0.236 e.A^-3 Table 2. Atomic coordinates ( x 10^4) and equivalent isotropic displacement parameters (A^2 x 10^3) for 1b. U(eq) is defined as one third of the trace of the orthogonalized Uij tensor. ________________________________________________________________ x y z U(eq) ________________________________________________________________ O(2) 5652(2) 4342(1) 7628(3) 35(1) O(1) 6689(2) 2637(1) 10568(3) 39(1) O(3) 7856(2) 4725(1) 8601(3) 41(1) O(5) 10054(2) 3344(1) 13238(3) 43(1) C(14) 7851(3) 2904(1) 13449(4) 32(1) C(13) 8577(3) 2948(1) 14937(4) 32(1) O(4) 9527(2) 4436(1) 11104(3) 45(1) C(16) 5953(3) 3262(1) 14657(4) 33(1) C(15) 6708(3) 3016(1) 13301(4) 28(1) C(2) 5173(3) 3295(1) 11139(4) 28(1) C(1) 6213(3) 2944(1) 11591(4) 30(1) C(24) 10065(3) 2981(1) 17674(5) 37(1) C(23) 10438(3) 3190(1) 16177(5) 36(1) C(6) 6105(3) 4867(1) 6997(5) 40(1) C(18) 4406(3) 3499(1) 12549(4) 32(1) C(17) 5148(3) 3724(1) 13977(4) 34(1) C(4) 4144(3) 3835(1) 8871(4) 33(1) C(12) 9713(3) 3173(1) 14794(5) 34(1) C(26) 8222(3) 2747(1) 16492(4) 35(1) C(22) 3654(3) 4660(1) 7178(4) 37(1) C(3) 5066(3) 3455(1) 9562(4) 31(1) C(21) 2488(3) 4566(2) 7501(5) 42(1) C(20) 2139(3) 4117(2) 8508(5) 39(1) C(7) 7398(3) 4817(2) 6990(5) 42(1) C(9) 8608(3) 4072(2) 10625(5) 42(1) C(5) 4492(3) 4297(1) 7869(4) 34(1) C(19) 2961(3) 3750(2) 9171(4) 37(1) C(25) 8946(3) 2759(1) 17854(5) 39(1) C(8) 8301(4) 4167(2) 8837(5) 46(1) C(11) 10697(4) 3879(2) 13105(6) 53(1) C(10) 9885(4) 4372(2) 12788(6) 54(1) ________________________________________________________________ Table 3. Bond lengths [A] and angles [deg] for 1b. _____________________________________________________________ O(2)-C(5) 1.351(4) O(2)-C(6) 1.432(4) O(1)-C(1) 1.225(4) O(3)-C(7) 1.416(5) O(3)-C(8) 1.420(4) O(5)-C(12) 1.372(5) O(5)-C(11) 1.464(5) C(14)-C(15) 1.344(5) C(14)-C(13) 1.463(5) C(13)-C(26) 1.398(5) C(13)-C(12) 1.412(5) O(4)-C(9) 1.413(4) O(4)-C(10) 1.424(6) C(16)-C(15) 1.509(5) C(16)-C(17) 1.529(4) C(15)-C(1) 1.497(4) C(2)-C(3) 1.330(5) C(2)-C(1) 1.496(4) C(2)-C(18) 1.515(5) C(24)-C(23) 1.370(6) C(24)-C(25) 1.396(5) C(23)-C(12) 1.390(5) C(6)-C(7) 1.490(5) C(18)-C(17) 1.526(5) C(4)-C(19) 1.394(5) C(4)-C(5) 1.411(5) C(4)-C(3) 1.493(5) C(26)-C(25) 1.376(5) C(22)-C(21) 1.382(5) C(22)-C(5) 1.402(5) C(21)-C(20) 1.389(5) C(20)-C(19) 1.386(5) C(9)-C(8) 1.498(5) C(11)-C(10) 1.508(6) C(5)-O(2)-C(6) 118.5(3) C(7)-O(3)-C(8) 113.4(3) C(12)-O(5)-C(11) 117.6(3) C(15)-C(14)-C(13) 128.0(3) C(26)-C(13)-C(12) 118.0(3) C(26)-C(13)-C(14) 122.8(3) C(12)-C(13)-C(14) 119.1(3) C(9)-O(4)-C(10) 114.3(3) C(15)-C(16)-C(17) 111.2(3) C(14)-C(15)-C(1) 115.5(3) C(14)-C(15)-C(16) 124.9(3) C(1)-C(15)-C(16) 119.3(3) C(3)-C(2)-C(1) 117.5(3) C(3)-C(2)-C(18) 124.8(3) C(1)-C(2)-C(18) 117.2(3) O(1)-C(1)-C(2) 121.2(3) O(1)-C(1)-C(15) 121.0(3) C(2)-C(1)-C(15) 117.7(3) C(23)-C(24)-C(25) 120.9(3) C(24)-C(23)-C(12) 120.4(3) O(2)-C(6)-C(7) 107.1(3) C(2)-C(18)-C(17) 110.5(3) C(18)-C(17)-C(16) 111.1(3) C(19)-C(4)-C(5) 119.0(3) C(19)-C(4)-C(3) 122.8(3) C(5)-C(4)-C(3) 118.2(3) O(5)-C(12)-C(23) 123.4(3) O(5)-C(12)-C(13) 116.6(3) C(23)-C(12)-C(13) 119.9(3) C(25)-C(26)-C(13) 122.0(3) C(21)-C(22)-C(5) 119.5(3) C(2)-C(3)-C(4) 126.2(3) C(22)-C(21)-C(20) 120.8(3) C(19)-C(20)-C(21) 120.1(3) O(3)-C(7)-C(6) 112.3(3) O(4)-C(9)-C(8) 110.3(3) O(2)-C(5)-C(22) 124.9(3) O(2)-C(5)-C(4) 115.0(3) C(22)-C(5)-C(4) 120.1(3) C(20)-C(19)-C(4) 120.5(3) C(26)-C(25)-C(24) 118.8(3) O(3)-C(8)-C(9) 110.6(3) O(5)-C(11)-C(10) 111.2(3) O(4)-C(10)-C(11) 114.9(4) _____________________________________________________________ Symmetry transformations used to generate equivalent atoms: Table 4. Anisotropic displacement parameters (A^2 x 10^3) for 1b. The anisotropic displacement factor exponent takes the form: -2 pi^2 [ h^2 a*^2 U11 + ... + 2 h k a* b* U12 ] _______________________________________________________________________ U11 U22 U33 U23 U13 U12 _______________________________________________________________________ O(2) 40(1) 28(1) 36(1) 2(1) 2(1) -1(1) O(1) 37(1) 44(1) 35(1) -15(1) -6(1) 6(1) O(3) 47(2) 34(1) 41(1) 2(1) -3(1) -2(1) O(5) 35(1) 62(2) 32(1) 0(1) -3(1) -1(1) C(14) 35(2) 30(1) 32(2) -4(1) -3(1) 3(1) C(13) 32(2) 28(2) 36(2) -3(1) -5(1) 7(1) O(4) 44(2) 51(1) 42(2) 4(1) -3(1) -7(1) C(16) 38(2) 33(2) 27(2) -3(1) -6(1) 4(1) C(15) 33(2) 25(1) 28(2) 1(1) -5(1) -2(1) C(2) 32(2) 22(1) 28(2) -4(1) -3(1) -2(1) C(1) 32(2) 28(2) 30(2) -4(1) -4(1) -1(1) C(24) 41(2) 29(2) 41(2) -2(2) -17(2) 8(1) C(23) 32(2) 35(2) 42(2) -3(2) -7(1) 5(1) C(6) 51(2) 32(2) 37(2) 5(1) -4(2) 1(2) C(18) 33(2) 30(1) 32(2) -1(1) -2(1) 5(1) C(17) 37(2) 36(2) 28(2) -7(1) -3(1) 10(1) C(4) 47(2) 26(1) 28(2) -4(1) -3(1) 0(1) C(12) 33(2) 37(2) 33(2) -5(1) -5(1) 6(1) C(26) 35(2) 29(2) 42(2) 3(1) -5(2) 5(1) C(22) 48(2) 31(2) 32(2) -3(1) -5(1) 6(2) C(3) 38(2) 26(1) 30(2) -2(1) -2(1) 0(1) C(21) 42(2) 44(2) 39(2) -8(2) -9(2) 7(2) C(20) 35(2) 41(2) 42(2) -9(2) -6(1) 1(1) C(7) 46(2) 41(2) 37(2) 7(2) -1(2) -5(2) C(9) 44(2) 36(2) 44(2) 3(2) -5(2) -2(2) C(5) 40(2) 34(2) 28(2) -6(1) -4(1) 3(1) C(19) 41(2) 38(2) 31(2) -4(1) -7(1) 2(1) C(25) 45(2) 33(2) 39(2) 3(2) -7(2) 5(2) C(8) 49(2) 37(2) 51(2) -4(2) -6(2) 7(2) C(11) 39(2) 72(3) 48(2) 15(2) -1(2) -10(2) C(10) 56(3) 59(2) 46(2) -7(2) 1(2) -15(2) _______________________________________________________________________ Table 5. Hydrogen coordinates ( x 10^4) and isotropic displacement parameters (A^2 x 10^3) for 1b. ________________________________________________________________ x y z U(eq) ________________________________________________________________ H(14) 8234 2780 12466 39 H(16A) 6454 3424 15538 39 H(16B) 5478 2955 15159 39 H(24) 10576 2988 18603 45 H(23) 11196 3348 16083 43 H(6A) 5859 5187 7713 48 H(6B) 5813 4936 5857 48 H(18A) 3915 3182 12950 38 H(18B) 3885 3804 12143 38 H(17A) 4634 3863 14879 40 H(17B) 5622 4049 13582 40 H(26) 7459 2597 16612 42 H(22) 3886 4969 6494 45 H(3) 5630 3315 8802 37 H(21) 1919 4810 7028 50 H(20) 1336 4062 8742 47 H(7A) 7627 4497 6260 50 H(7B) 7738 5169 6523 50 H(9A) 7918 4146 11330 50 H(9B) 8845 3671 10788 50 H(19) 2716 3439 9836 44 H(25) 8688 2619 18899 47 H(8A) 9002 4114 8138 55 H(8B) 7710 3885 8486 55 H(11A) 11267 3852 12185 64 H(11B) 11133 3947 14148 64 H(10A) 9183 4323 13487 64 H(10B) 10275 4726 13146 64 ________________________________________________________________ Table 6. Torsion angles [deg] for 1b. ________________________________________________________________ C(15)-C(14)-C(13)-C(26) 44.5(5) C(15)-C(14)-C(13)-C(12) -139.2(3) C(13)-C(14)-C(15)-C(1) 178.4(3) C(13)-C(14)-C(15)-C(16) 5.3(5) C(17)-C(16)-C(15)-C(14) 136.5(3) C(17)-C(16)-C(15)-C(1) -36.4(4) C(3)-C(2)-C(1)-O(1) -27.6(4) C(18)-C(2)-C(1)-O(1) 159.8(3) C(3)-C(2)-C(1)-C(15) 147.9(3) C(18)-C(2)-C(1)-C(15) -24.7(4) C(14)-C(15)-C(1)-O(1) 22.9(4) C(16)-C(15)-C(1)-O(1) -163.6(3) C(14)-C(15)-C(1)-C(2) -152.6(3) C(16)-C(15)-C(1)-C(2) 20.9(4) C(25)-C(24)-C(23)-C(12) -1.5(5) C(5)-O(2)-C(6)-C(7) 175.3(3) C(3)-C(2)-C(18)-C(17) -127.9(3) C(1)-C(2)-C(18)-C(17) 44.1(4) C(2)-C(18)-C(17)-C(16) -60.1(4) C(15)-C(16)-C(17)-C(18) 56.0(4) C(11)-O(5)-C(12)-C(23) -44.9(5) C(11)-O(5)-C(12)-C(13) 137.8(3) C(24)-C(23)-C(12)-O(5) -176.1(3) C(24)-C(23)-C(12)-C(13) 1.2(5) C(26)-C(13)-C(12)-O(5) 177.3(3) C(14)-C(13)-C(12)-O(5) 0.8(4) C(26)-C(13)-C(12)-C(23) -0.2(5) C(14)-C(13)-C(12)-C(23) -176.6(3) C(12)-C(13)-C(26)-C(25) -0.6(5) C(14)-C(13)-C(26)-C(25) 175.8(3) C(1)-C(2)-C(3)-C(4) -175.7(3) C(18)-C(2)-C(3)-C(4) -3.8(5) C(19)-C(4)-C(3)-C(2) -50.0(5) C(5)-C(4)-C(3)-C(2) 130.2(4) C(5)-C(22)-C(21)-C(20) 0.4(5) C(22)-C(21)-C(20)-C(19) -1.5(5) C(8)-O(3)-C(7)-C(6) 109.3(3) O(2)-C(6)-C(7)-O(3) -60.7(4) C(10)-O(4)-C(9)-C(8) -179.6(3) C(6)-O(2)-C(5)-C(22) 16.9(5) C(6)-O(2)-C(5)-C(4) -164.5(3) C(21)-C(22)-C(5)-O(2) 179.2(3) C(21)-C(22)-C(5)-C(4) 0.6(5) C(19)-C(4)-C(5)-O(2) -179.3(3) C(3)-C(4)-C(5)-O(2) 0.6(4) C(19)-C(4)-C(5)-C(22) -0.6(5) C(3)-C(4)-C(5)-C(22) 179.3(3) C(21)-C(20)-C(19)-C(4) 1.6(5) C(5)-C(4)-C(19)-C(20) -0.6(5) C(3)-C(4)-C(19)-C(20) 179.6(3) C(13)-C(26)-C(25)-C(24) 0.3(5) C(23)-C(24)-C(25)-C(26) 0.8(5) C(7)-O(3)-C(8)-C(9) -171.7(3) O(4)-C(9)-C(8)-O(3) -64.6(4) C(12)-O(5)-C(11)-C(10) -92.5(4) C(9)-O(4)-C(10)-C(11) 80.9(4) O(5)-C(11)-C(10)-O(4) -80.7(4) ________________________________________________________________ Symmetry transformations used to generate equivalent atoms: