+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 16:25:38 on 03-Aug-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 01SOT020 in P2(1)/n CELL 0.71073 11.8390 8.0773 22.6950 90 91.840 90 ZERR 4 0.002 0.001 0.004 0 0.03 0 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H O UNIT 92 104 32 V = 2169.14 F(000) = 912.0 Mu = 0.10 mm-1 Cell Wt = 1721.75 Rho = 1.318 SHEL 7 0.9 TEMP -123 SIZE 0.1 0.1 0.1 FMAP 2 PLAN 20 L.S. 4 WGHT 0.190500 EXTI 0.004857 FVAR 0.09352 MOLE 1 C1 1 0.085884 0.369643 0.060214 11.00000 0.09470 0.06633 = 0.07266 0.01257 -0.02784 -0.01134 AFIX 33 H1A 2 0.023593 0.329293 0.034602 11.00000 -1.50000 H1B 2 0.058054 0.391596 0.099661 11.00000 -1.50000 H1C 2 0.145608 0.285708 0.062810 11.00000 -1.50000 AFIX 0 C2 1 0.177351 0.909542 -0.027213 11.00000 0.15800 0.16919 = 0.26202 0.14399 -0.09910 -0.06028 AFIX 33 H2A 2 0.121393 0.879481 -0.058132 11.00000 -1.50000 H2B 2 0.247043 0.946354 -0.045350 11.00000 -1.50000 H2C 2 0.147431 0.999295 -0.003202 11.00000 -1.50000 AFIX 0 C3 1 0.460680 1.070029 0.076422 11.00000 0.23644 0.11757 = 0.09477 0.00057 0.00064 -0.14354 AFIX 33 H3A 2 0.470392 1.174968 0.055511 11.00000 -1.50000 H3B 2 0.528305 1.001545 0.072323 11.00000 -1.50000 H3C 2 0.449286 1.092179 0.118269 11.00000 -1.50000 AFIX 0 C4 1 0.272934 0.525031 0.114805 11.00000 0.05105 0.04662 = 0.05277 -0.00863 0.01097 -0.00792 AFIX 43 H4 2 0.250921 0.418844 0.128300 11.00000 -1.20000 AFIX 0 C5 1 0.219066 0.596529 0.066783 11.00000 0.07074 0.05733 = 0.04005 0.00537 -0.00699 -0.01847 C6 1 0.249474 0.751405 0.045746 11.00000 0.15336 0.07345 = 0.04348 0.02548 -0.02545 -0.05493 C7 1 0.337349 0.836006 0.075365 11.00000 0.13099 0.06657 = 0.03663 0.01736 -0.00020 -0.02282 C8 1 0.392415 0.769160 0.124500 11.00000 0.05253 0.05128 = 0.06844 -0.01439 0.01918 -0.01820 AFIX 43 H8 2 0.450555 0.828833 0.145024 11.00000 -1.20000 AFIX 0 C9 1 0.360286 0.611192 0.143244 11.00000 0.03814 0.04928 = 0.05891 -0.01053 0.00558 -0.00256 C10 1 0.417119 0.543053 0.200225 11.00000 0.04304 0.03001 = 0.08261 -0.02228 -0.00255 -0.00196 AFIX 13 H10 2 0.486922 0.607860 0.210611 11.00000 -1.20000 AFIX 0 C11 1 0.427087 0.276031 0.238409 11.00000 0.03253 0.04620 = 0.06777 -0.00307 -0.00906 -0.00922 C12 1 0.370391 0.379304 0.285380 11.00000 0.04255 0.05547 = 0.05466 -0.00723 0.00377 0.00336 AFIX 13 H12 2 0.302076 0.321914 0.300225 11.00000 -1.20000 AFIX 0 C13 1 0.450118 0.439298 0.337795 11.00000 0.04261 0.07316 = 0.06130 -0.00749 -0.00754 -0.00163 AFIX 13 H13 2 0.406859 0.432846 0.374853 11.00000 -1.20000 AFIX 0 C14 1 0.371969 0.674540 0.297353 11.00000 0.06651 0.07920 = 0.05794 -0.01492 -0.01337 0.03136 AFIX 23 H14A 2 0.387692 0.780251 0.277119 11.00000 -1.20000 H14B 2 0.311838 0.692773 0.325974 11.00000 -1.20000 AFIX 0 C15 1 0.337972 0.539117 0.252862 11.00000 0.04221 0.06831 = 0.05134 -0.01862 0.00711 0.00718 AFIX 13 H15 2 0.256159 0.543469 0.240557 11.00000 -1.20000 AFIX 0 C16 1 0.557971 0.349997 0.347761 11.00000 0.04588 0.05708 = 0.04640 -0.01436 -0.00844 -0.00112 C17 1 0.573353 0.238882 0.394240 11.00000 0.06292 0.07274 = 0.04738 -0.01415 0.00763 0.00529 AFIX 43 H17 2 0.513063 0.221824 0.420198 11.00000 -1.20000 AFIX 0 C18 1 0.674297 0.151271 0.404206 11.00000 0.04160 0.05519 = 0.06867 -0.00157 -0.00103 0.00184 AFIX 43 H18 2 0.681896 0.075142 0.435993 11.00000 -1.20000 AFIX 0 C19 1 0.761103 0.177144 0.367597 11.00000 0.03007 0.04405 = 0.08843 0.00265 0.00627 0.01202 C20 1 0.749565 0.289200 0.319730 11.00000 0.04558 0.06167 = 0.05329 0.00239 0.00431 -0.00730 C21 1 0.650554 0.375653 0.311270 11.00000 0.04675 0.04198 = 0.06850 -0.01443 -0.01695 0.00022 AFIX 43 H21 2 0.644277 0.454322 0.280221 11.00000 -1.20000 AFIX 0 C22 1 0.829027 0.396819 0.233318 11.00000 0.05587 0.07884 = 0.10071 0.04403 0.01187 0.00194 AFIX 33 H22A 2 0.898440 0.393292 0.210960 11.00000 -1.50000 H22B 2 0.814029 0.511092 0.245290 11.00000 -1.50000 H22C 2 0.765612 0.356009 0.208581 11.00000 -1.50000 AFIX 0 C23 1 0.881658 0.001429 0.425206 11.00000 0.06883 0.16519 = 0.12897 0.10707 0.03651 0.05168 AFIX 33 H23A 2 0.957392 -0.047451 0.424810 11.00000 -1.50000 H23B 2 0.825064 -0.086947 0.426412 11.00000 -1.50000 H23C 2 0.875542 0.072081 0.460063 11.00000 -1.50000 AFIX 0 O1 3 0.130719 0.520586 0.035977 11.00000 0.09663 0.06552 = 0.03828 0.00776 -0.01933 -0.02111 O2 3 0.194036 0.810076 -0.001400 11.00000 0.40133 0.15853 = 0.10532 0.09921 -0.15337 -0.16478 O3 3 0.365156 0.985134 0.052031 11.00000 0.23941 0.10150 = 0.06023 0.02869 -0.02327 -0.09005 O4 3 0.445379 0.371026 0.189982 11.00000 0.04565 0.06220 = 0.05366 -0.01201 0.00724 0.00087 O5 3 0.444190 0.129732 0.238804 11.00000 0.05365 0.04876 = 0.06562 -0.00701 -0.00343 -0.00302 O6 3 0.472006 0.610089 0.325933 11.00000 0.05116 0.07949 = 0.06364 -0.02571 -0.01795 0.01279 O7 3 0.842299 0.293660 0.285126 11.00000 0.03961 0.06327 = 0.08775 0.03054 0.00520 0.00642 O8 3 0.862598 0.098892 0.373013 11.00000 0.04347 0.08473 = 0.09914 0.04323 0.02218 0.01530 HKLF 4 1.0 0.00 -1.00 0.00 -1.00 0.00 0.00 0.00 0.00 -1.00 Covalent radii and connectivity table for 01SOT020 in P2(1)/n C 0.770 H 0.320 O 0.660 C1 - O1 C2 - O2 C3 - O3 C4 - C5 C9 C5 - C4 O1 C6 C6 - O2 C5 C7 C7 - O3 C8 C6 C8 - C7 C9 C9 - C4 C8 C10 C10 - O4 C9 C15 C11 - O5 O4 C12 C12 - C11 C15 C13 C13 - O6 C16 C12 C14 - O6 C15 C15 - C12 C14 C10 C16 - C17 C21 C13 C17 - C16 C18 C18 - C19 C17 C19 - C18 O8 C20 C20 - O7 C21 C19 C21 - C20 C16 C22 - O7 C23 - O8 O1 - C5 C1 O2 - C2 C6 O3 - C7 C3 O4 - C11 C10 O5 - C11 O6 - C14 C13 O7 - C20 C22 O8 - C19 C23 16091 Reflections read, of which 2135 rejected -13 =< h =< 13, -8 =< k =< 8, -25 =< l =< 25, Max. 2-theta = 46.51 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 3 1 0 1.37 0.14 6 1.05 4 2 0 5.91 0.20 6 1.47 0 1 3 0.44 0.16 6 1.24 3 2 4 15.14 0.22 4 8.96 4 2 7 7.76 0.47 3 3.37 5 Inconsistent equivalents 2999 Unique reflections, of which 0 suppressed R(int) = 0.3615 R(sigma) = 0.2909 Friedel opposites merged Maximum memory for data reduction = 2252 / 30108 Default effective X-H distances for T = -123.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 1.00 0.99 0.98 0.95 0.88 0.91 1.12 0.84 0.95 0.88 0.95 Note that these distances are chosen to give the best fit to the X-ray data and so avoid the introduction of systematic error. The true internuclear distances are longer and do not vary with temperature ! The apparent variation with temperature is caused by libration. Least-squares cycle 1 Maximum vector length = 511 Memory required = 3061 / 349338 wR2 = 0.3345 before cycle 1 for 2999 data and 281 / 281 parameters GooF = S = 0.811; Restrained GooF = 0.811 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1905 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.09352 0.00075 -0.006 OSF 2 0.00486 0.00288 0.000 EXTI Mean shift/esd = 0.001 Maximum = -0.006 for OSF Max. shift = 0.000 A for H2A Max. dU = 0.000 for O3 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3061 / 349338 wR2 = 0.3345 before cycle 2 for 2999 data and 281 / 281 parameters GooF = S = 0.811; Restrained GooF = 0.811 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1905 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.09351 0.00075 -0.001 OSF 2 0.00486 0.00288 0.000 EXTI Mean shift/esd = 0.001 Maximum = -0.005 for x C2 Max. shift = 0.000 A for C2 Max. dU = 0.000 for O3 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3061 / 349338 wR2 = 0.3345 before cycle 3 for 2999 data and 281 / 281 parameters GooF = S = 0.811; Restrained GooF = 0.811 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1905 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.09351 0.00075 -0.001 OSF 2 0.00485 0.00288 0.000 EXTI Mean shift/esd = 0.001 Maximum = -0.003 for x C2 Max. shift = 0.000 A for C2 Max. dU = 0.000 for O3 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3061 / 349338 wR2 = 0.3345 before cycle 4 for 2999 data and 281 / 281 parameters GooF = S = 0.811; Restrained GooF = 0.811 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1905 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.09351 0.00075 0.000 OSF 2 0.00485 0.00288 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for x C2 Max. shift = 0.000 A for H2A Max. dU = 0.000 for O3 Largest correlation matrix elements -0.650 U12 C3 / U22 C3 -0.531 U12 O2 / U23 O2 0.513 U23 O2 / U22 O2 -0.580 U12 O2 / U11 O2 -0.529 U12 O2 / U22 O2 -0.504 U13 O2 / U33 O2 -0.566 U13 O2 / U23 O2 0.528 y O5 / y C11 0.502 U23 C2 / U22 C2 -0.555 U13 O2 / U11 O2 0.523 U23 C23 / U22 C23 -0.532 U12 C3 / U11 C3 0.515 EXTI / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.0236 0.3293 0.0346 33 0.980 0.000 C1 O1 H1A H1B 0.0581 0.3916 0.0997 33 0.980 0.000 C1 O1 H1A H1C 0.1456 0.2857 0.0628 33 0.980 0.000 C1 O1 H1A H2A 0.1214 0.8795 -0.0581 33 0.980 0.000 C2 O2 H2A H2B 0.2470 0.9464 -0.0453 33 0.980 0.000 C2 O2 H2A H2C 0.1474 0.9993 -0.0032 33 0.980 0.000 C2 O2 H2A H3A 0.4704 1.1750 0.0555 33 0.980 0.000 C3 O3 H3A H3B 0.5283 1.0016 0.0723 33 0.980 0.000 C3 O3 H3A H3C 0.4493 1.0922 0.1183 33 0.980 0.000 C3 O3 H3A H4 0.2509 0.4188 0.1283 43 0.950 0.000 C4 C5 C9 H8 0.4506 0.8288 0.1450 43 0.950 0.000 C8 C7 C9 H10 0.4869 0.6079 0.2106 13 1.000 0.000 C10 O4 C9 C15 H12 0.3021 0.3219 0.3002 13 1.000 0.000 C12 C11 C15 C13 H13 0.4069 0.4329 0.3749 13 1.000 0.000 C13 O6 C16 C12 H14A 0.3877 0.7803 0.2771 23 0.990 0.000 C14 O6 C15 H14B 0.3118 0.6928 0.3260 23 0.990 0.000 C14 O6 C15 H15 0.2562 0.5435 0.2406 13 1.000 0.000 C15 C12 C14 C10 H17 0.5131 0.2218 0.4202 43 0.950 0.000 C17 C16 C18 H18 0.6819 0.0751 0.4360 43 0.950 0.000 C18 C19 C17 H21 0.6443 0.4543 0.2802 43 0.950 0.000 C21 C20 C16 H22A 0.8984 0.3933 0.2110 33 0.980 0.000 C22 O7 H22A H22B 0.8140 0.5111 0.2453 33 0.980 0.000 C22 O7 H22A H22C 0.7656 0.3560 0.2086 33 0.980 0.000 C22 O7 H22A H23A 0.9574 -0.0475 0.4248 33 0.980 0.000 C23 O8 H23A H23B 0.8250 -0.0869 0.4264 33 0.980 0.000 C23 O8 H23A H23C 0.8755 0.0721 0.4601 33 0.980 0.000 C23 O8 H23A 01SOT020 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.08590 0.36964 0.06021 1.00000 0.09472 0.06633 0.07264 0.01257 -0.02785 -0.01134 0.07855 0.01765 0.00093 0.00129 0.00047 0.00000 0.00836 0.00831 0.00846 0.00694 0.00648 0.00701 0.00348 H1A 0.02360 0.32929 0.03460 1.00000 0.11783 0.00000 0.00000 H1B 0.05807 0.39159 0.09966 1.00000 0.11783 0.00000 0.00000 H1C 0.14562 0.28571 0.06281 1.00000 0.11783 0.00000 0.00000 C2 0.17733 0.90955 -0.02720 1.00000 0.15804 0.16912 0.26209 0.14396 -0.09913 -0.06031 0.19868 0.03200 0.00146 0.00215 0.00096 0.00000 0.01524 0.01956 0.02705 0.01761 0.01525 0.01370 0.01065 H2A 0.12137 0.87949 -0.05812 1.00000 0.29803 0.00000 0.00000 H2B 0.24701 0.94640 -0.04534 1.00000 0.29803 0.00000 0.00000 H2C 0.14740 0.99927 -0.00318 1.00000 0.29803 0.00000 0.00000 C3 0.46066 1.07004 0.07642 1.00000 0.23637 0.11754 0.09480 0.00057 0.00065 -0.14350 0.14967 0.02051 0.00135 0.00162 0.00056 0.00000 0.01732 0.01270 0.01119 0.00888 0.01090 0.01286 0.00709 H3A 0.47037 1.17497 0.05551 1.00000 0.22451 0.00000 0.00000 H3B 0.52830 1.00156 0.07233 1.00000 0.22451 0.00000 0.00000 H3C 0.44926 1.09219 0.11827 1.00000 0.22451 0.00000 0.00000 C4 0.27293 0.52503 0.11480 1.00000 0.05109 0.04661 0.05277 -0.00863 0.01096 -0.00792 0.04996 0.01613 0.00073 0.00121 0.00042 0.00000 0.00607 0.00647 0.00712 0.00556 0.00520 0.00531 0.00262 H4 0.25091 0.41885 0.12830 1.00000 0.05995 0.00000 0.00000 C5 0.21906 0.59653 0.06678 1.00000 0.07074 0.05733 0.04005 0.00538 -0.00700 -0.01848 0.05623 0.01718 0.00083 0.00127 0.00044 0.00000 0.00717 0.00774 0.00658 0.00573 0.00561 0.00588 0.00284 C6 0.24947 0.75140 0.04575 1.00000 0.15345 0.07345 0.04346 0.02549 -0.02547 -0.05494 0.09073 0.02059 0.00112 0.00152 0.00050 0.00000 0.01186 0.00906 0.00750 0.00670 0.00759 0.00852 0.00427 C7 0.33736 0.83600 0.07536 1.00000 0.13104 0.06657 0.03662 0.01736 -0.00020 -0.02283 0.07814 0.02157 0.00111 0.00147 0.00048 0.00000 0.01066 0.00902 0.00729 0.00652 0.00721 0.00777 0.00368 C8 0.39242 0.76916 0.12450 1.00000 0.05252 0.05127 0.06844 -0.01439 0.01920 -0.01820 0.05704 0.01718 0.00077 0.00127 0.00046 0.00000 0.00642 0.00743 0.00814 0.00602 0.00570 0.00544 0.00297 H8 0.45056 0.82884 0.14503 1.00000 0.06845 0.00000 0.00000 C9 0.36029 0.61119 0.14324 1.00000 0.03814 0.04929 0.05891 -0.01053 0.00558 -0.00256 0.04869 0.01703 0.00074 0.00124 0.00043 0.00000 0.00553 0.00704 0.00715 0.00566 0.00506 0.00540 0.00260 C10 0.41713 0.54305 0.20022 1.00000 0.04305 0.03001 0.08261 -0.02228 -0.00255 -0.00197 0.05199 0.01550 0.00075 0.00111 0.00045 0.00000 0.00580 0.00607 0.00828 0.00546 0.00560 0.00500 0.00275 H10 0.48693 0.60786 0.21061 1.00000 0.06238 0.00000 0.00000 C11 0.42709 0.27603 0.23841 1.00000 0.03252 0.04621 0.06776 -0.00308 -0.00906 -0.00922 0.04906 0.01603 0.00073 0.00145 0.00048 0.00000 0.00554 0.00698 0.00809 0.00685 0.00500 0.00549 0.00264 C12 0.37039 0.37930 0.28538 1.00000 0.04258 0.05547 0.05465 -0.00723 0.00374 0.00336 0.05085 0.01588 0.00072 0.00124 0.00041 0.00000 0.00568 0.00708 0.00689 0.00564 0.00498 0.00526 0.00267 H12 0.30208 0.32191 0.30023 1.00000 0.06102 0.00000 0.00000 C13 0.45012 0.43930 0.33779 1.00000 0.04263 0.07316 0.06130 -0.00749 -0.00755 -0.00164 0.05923 0.01670 0.00076 0.00136 0.00045 0.00000 0.00639 0.00872 0.00752 0.00608 0.00508 0.00619 0.00297 H13 0.40686 0.43285 0.37485 1.00000 0.07107 0.00000 0.00000 C14 0.37196 0.67454 0.29735 1.00000 0.06657 0.07917 0.05794 -0.01494 -0.01340 0.03138 0.06822 0.01708 0.00080 0.00133 0.00044 0.00000 0.00712 0.00862 0.00734 0.00609 0.00559 0.00624 0.00327 H14A 0.38768 0.78025 0.27712 1.00000 0.08187 0.00000 0.00000 H14B 0.31183 0.69276 0.32598 1.00000 0.08187 0.00000 0.00000 C15 0.33797 0.53912 0.25286 1.00000 0.04224 0.06830 0.05134 -0.01861 0.00711 0.00718 0.05384 0.01618 0.00075 0.00125 0.00042 0.00000 0.00562 0.00767 0.00692 0.00608 0.00503 0.00550 0.00275 H15 0.25615 0.54347 0.24056 1.00000 0.06460 0.00000 0.00000 C16 0.55797 0.35000 0.34776 1.00000 0.04582 0.05710 0.04641 -0.01435 -0.00842 -0.00112 0.04999 0.01510 0.00077 0.00122 0.00044 0.00000 0.00648 0.00727 0.00677 0.00559 0.00528 0.00564 0.00267 C17 0.57336 0.23888 0.39424 1.00000 0.06286 0.07276 0.04738 -0.01414 0.00763 0.00530 0.06087 0.01624 0.00086 0.00131 0.00044 0.00000 0.00727 0.00793 0.00696 0.00644 0.00547 0.00621 0.00294 H17 0.51307 0.22183 0.42020 1.00000 0.07305 0.00000 0.00000 C18 0.67429 0.15127 0.40421 1.00000 0.04163 0.05517 0.06865 -0.00157 -0.00105 0.00183 0.05521 0.01574 0.00077 0.00118 0.00045 0.00000 0.00596 0.00702 0.00751 0.00560 0.00541 0.00557 0.00275 H18 0.68189 0.07514 0.43599 1.00000 0.06625 0.00000 0.00000 C19 0.76111 0.17714 0.36760 1.00000 0.03007 0.04407 0.08842 0.00266 0.00628 0.01201 0.05409 0.01645 0.00074 0.00117 0.00048 0.00000 0.00583 0.00673 0.00862 0.00582 0.00566 0.00504 0.00285 C20 0.74957 0.28920 0.31973 1.00000 0.04555 0.06169 0.05329 0.00240 0.00433 -0.00729 0.05345 0.01582 0.00082 0.00130 0.00042 0.00000 0.00648 0.00746 0.00708 0.00602 0.00548 0.00600 0.00270 C21 0.65055 0.37565 0.31127 1.00000 0.04679 0.04195 0.06851 -0.01444 -0.01699 0.00020 0.05282 0.01433 0.00080 0.00115 0.00044 0.00000 0.00602 0.00624 0.00772 0.00550 0.00557 0.00551 0.00274 H21 0.64427 0.45432 0.28022 1.00000 0.06338 0.00000 0.00000 C22 0.82902 0.39682 0.23332 1.00000 0.05589 0.07882 0.10071 0.04402 0.01187 0.00194 0.07827 0.01993 0.00081 0.00130 0.00049 0.00000 0.00661 0.00871 0.00974 0.00742 0.00629 0.00595 0.00366 H22A 0.89843 0.39330 0.21096 1.00000 0.11741 0.00000 0.00000 H22B 0.81402 0.51109 0.24529 1.00000 0.11741 0.00000 0.00000 H22C 0.76560 0.35601 0.20858 1.00000 0.11741 0.00000 0.00000 C23 0.88165 0.00142 0.42521 1.00000 0.06877 0.16523 0.12900 0.10711 0.03650 0.05168 0.12028 0.02591 0.00090 0.00165 0.00056 0.00000 0.00785 0.01359 0.01206 0.01076 0.00763 0.00830 0.00579 H23A 0.95738 -0.04746 0.42481 1.00000 0.18043 0.00000 0.00000 H23B 0.82505 -0.08695 0.42641 1.00000 0.18043 0.00000 0.00000 H23C 0.87553 0.07208 0.46006 1.00000 0.18043 0.00000 0.00000 O1 0.13072 0.52059 0.03598 1.00000 0.09659 0.06552 0.03829 0.00775 -0.01931 -0.02110 0.06726 0.01108 0.00059 0.00085 0.00027 0.00000 0.00536 0.00511 0.00434 0.00374 0.00370 0.00431 0.00214 O2 0.19403 0.81007 -0.00140 1.00000 0.40139 0.15850 0.10536 0.09921 -0.15341 -0.16476 0.22521 0.01748 0.00142 0.00163 0.00050 0.00000 0.02062 0.01169 0.00898 0.00864 0.01141 0.01293 0.00885 O3 0.36517 0.98513 0.05203 1.00000 0.23932 0.10150 0.06023 0.02868 -0.02326 -0.09005 0.13429 0.01486 0.00092 0.00113 0.00034 0.00000 0.01132 0.00725 0.00599 0.00534 0.00634 0.00768 0.00403 O4 0.44538 0.37103 0.18998 1.00000 0.04564 0.06221 0.05366 -0.01201 0.00724 0.00087 0.05371 0.01005 0.00045 0.00086 0.00028 0.00000 0.00390 0.00507 0.00479 0.00395 0.00328 0.00346 0.00187 O5 0.44419 0.12973 0.23880 1.00000 0.05366 0.04875 0.06561 -0.00701 -0.00343 -0.00303 0.05612 0.01070 0.00049 0.00088 0.00028 0.00000 0.00428 0.00468 0.00484 0.00403 0.00327 0.00371 0.00188 O6 0.47201 0.61009 0.32593 1.00000 0.05116 0.07949 0.06364 -0.02572 -0.01795 0.01278 0.06519 0.01101 0.00051 0.00094 0.00028 0.00000 0.00426 0.00560 0.00493 0.00422 0.00350 0.00418 0.00208 O7 0.84229 0.29366 0.28513 1.00000 0.03962 0.06326 0.08775 0.03053 0.00519 0.00642 0.06347 0.01132 0.00049 0.00080 0.00030 0.00000 0.00381 0.00482 0.00551 0.00419 0.00376 0.00347 0.00207 O8 0.86259 0.09889 0.37301 1.00000 0.04345 0.08474 0.09915 0.04322 0.02219 0.01529 0.07535 0.01293 0.00050 0.00084 0.00032 0.00000 0.00415 0.00563 0.00606 0.00482 0.00376 0.00395 0.00240 Final Structure Factor Calculation for 01SOT020 in P2(1)/n Total number of l.s. parameters = 281 Maximum vector length = 511 Memory required = 2780 / 21973 wR2 = 0.3345 before cycle 5 for 2999 data and 0 / 281 parameters GooF = S = 0.811; Restrained GooF = 0.811 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1905 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0864 for 947 Fo > 4sig(Fo) and 0.2721 for all 2999 data wR2 = 0.3345, GooF = S = 0.811, Restrained GooF = 0.811 for all data Occupancy sum of asymmetric unit = 31.00 for non-hydrogen and 26.00 for hydrogen atoms Principal mean square atomic displacements U 0.1222 0.0626 0.0509 C1 0.4268 0.1072 0.0620 C2 may be split into 0.1682 0.9278 -0.0179 and 0.1865 0.8913 -0.0366 0.3326 0.0948 0.0216 C3 may be split into 0.4778 1.0533 0.0760 and 0.4436 1.0868 0.0768 0.0674 0.0423 0.0402 C4 0.0863 0.0444 0.0379 C5 0.1921 0.0515 0.0286 C6 0.1393 0.0673 0.0279 C7 0.0910 0.0467 0.0334 C8 0.0663 0.0425 0.0372 C9 0.0912 0.0433 0.0214 C10 0.0711 0.0507 0.0254 C11 0.0624 0.0498 0.0403 C12 0.0771 0.0620 0.0386 C13 0.1138 0.0503 0.0405 C14 0.0806 0.0493 0.0316 C15 0.0684 0.0502 0.0314 C16 0.0796 0.0646 0.0384 C17 0.0693 0.0551 0.0412 C18 0.0889 0.0504 0.0230 C19 0.0647 0.0541 0.0416 C20 0.0840 0.0439 0.0306 C21 0.1358 0.0566 0.0424 C22 0.2720 0.0530 0.0358 C23 may be split into 0.8878 0.0229 0.4315 and 0.8755 -0.0200 0.4190 0.1148 0.0551 0.0318 O1 0.5692 0.0808 0.0256 O2 may be split into 0.2176 0.7916 -0.0075 and 0.1704 0.8285 0.0047 0.2914 0.0701 0.0413 O3 may be split into 0.3825 0.9722 0.0502 and 0.3479 0.9981 0.0539 0.0709 0.0503 0.0399 O4 0.0694 0.0550 0.0440 O5 0.1080 0.0512 0.0363 O6 0.1088 0.0445 0.0372 O7 0.1413 0.0483 0.0364 O8 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.006 0.013 0.020 0.028 0.037 0.048 0.065 0.087 0.130 1.000 Number in group 300. 327. 295. 311. 270. 308. 300. 290. 299. 299. GooF 0.700 0.747 0.767 0.809 0.823 0.868 0.850 0.976 0.831 0.708 K -6.552 0.851 1.054 0.744 1.082 1.124 0.931 1.038 1.022 1.024 Resolution(A) 0.90 0.94 0.97 1.02 1.08 1.14 1.24 1.36 1.55 1.95 inf Number in group 312. 292. 299. 301. 296. 305. 299. 293. 302. 300. GooF 0.788 0.786 0.772 0.795 0.799 0.847 0.810 0.880 0.841 0.784 K 0.907 1.257 0.862 0.986 1.063 1.033 1.018 1.073 1.055 1.008 R1 0.632 0.550 0.478 0.360 0.345 0.243 0.256 0.191 0.113 0.064 Recommended weighting scheme: WGHT 0.1025 0.0000 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 5 4 1 -24.02 144.90 5.48 0.067 1.53 -5 3 8 492.75 223.48 3.97 0.083 1.52 8 1 18 720.11 302.22 3.74 0.096 0.94 -8 2 10 190.81 19.87 3.58 0.025 1.20 5 5 8 68.17 280.77 3.45 0.093 1.20 -6 1 12 -2.51 131.72 3.29 0.064 1.37 13 0 1 334.54 61.72 3.14 0.044 0.91 -3 3 3 753.57 466.13 3.13 0.120 2.14 -1 1 1 51.03 21.46 2.99 0.026 6.43 -9 0 17 687.06 225.03 2.96 0.083 0.95 -7 4 18 310.91 1.54 2.95 0.007 0.91 6 6 4 217.27 6.42 2.91 0.014 1.09 11 0 3 262.07 70.43 2.88 0.046 1.06 -1 3 2 339.24 551.43 2.80 0.130 2.56 2 2 19 255.82 73.43 2.79 0.047 1.12 -8 6 5 86.51 274.67 2.77 0.092 0.98 2 1 0 15.16 38.81 2.77 0.035 4.77 -4 6 4 193.16 9.82 2.74 0.017 1.20 -2 3 5 199.46 101.94 2.74 0.056 2.17 -5 1 10 281.15 155.85 2.69 0.069 1.63 1 4 13 -54.10 58.73 2.68 0.042 1.31 5 3 2 49.16 140.70 2.65 0.066 1.75 -5 3 7 104.30 234.18 2.65 0.085 1.57 -1 1 13 18.11 178.58 2.64 0.074 1.70 -9 2 5 181.71 73.42 2.62 0.047 1.21 2 1 19 193.65 0.80 2.62 0.005 1.15 -2 4 5 79.80 192.55 2.62 0.077 1.77 0 5 17 -98.21 97.27 2.56 0.055 1.03 -10 0 2 4073.60 2697.12 2.55 0.288 1.18 -3 5 10 116.52 260.65 2.55 0.089 1.26 -1 6 13 175.01 3.35 2.51 0.010 1.06 -9 3 8 -50.46 66.99 2.50 0.045 1.10 -5 1 9 313.34 185.60 2.50 0.075 1.71 8 0 8 132.16 20.43 2.49 0.025 1.29 2 2 24 461.28 153.69 2.47 0.069 0.91 -8 4 13 -51.85 131.57 2.45 0.064 1.00 -5 3 5 1837.25 1190.57 2.43 0.191 1.67 -7 4 2 10.37 76.29 2.40 0.048 1.29 -7 0 13 209.93 11.39 2.39 0.019 1.23 -10 5 9 254.92 7.17 2.39 0.015 0.90 -11 0 7 -15.10 161.69 2.39 0.070 1.03 7 2 16 144.40 0.14 2.38 0.002 1.03 -7 3 2 -27.07 23.01 2.38 0.027 1.43 -5 1 12 96.76 11.65 2.38 0.019 1.48 -8 6 7 277.86 88.50 2.37 0.052 0.96 -8 3 14 178.19 9.06 2.37 0.017 1.03 -6 5 6 188.32 61.97 2.32 0.044 1.19 4 6 14 156.24 34.76 2.31 0.033 0.97 -9 3 6 58.63 170.15 2.31 0.072 1.14 12 3 5 -105.25 82.60 2.30 0.050 0.90 FMAP and GRID set by program FMAP 2 3 24 GRID -1.190 -2 -2 1.190 2 2 R1 = 0.2721 for 2999 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.40 at 0.7430 0.2120 0.0039 [ 0.77 A from O2 ] Deepest hole -0.28 at 0.7119 0.3008 0.0323 [ 1.38 A from H23B ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 2516 / 17334 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2570 0.7880 -0.0039 1.00000 0.05 0.40 0.77 O2 1.17 C6 1.45 C2 1.59 H2B Q2 1 0.1571 0.9025 0.0131 1.00000 0.05 0.29 0.87 H2C 0.93 O2 0.95 C2 1.67 H2A Q3 1 0.0842 1.0211 -0.0844 1.00000 0.05 0.24 1.36 H2A 1.88 C16 1.90 C2 1.97 H2C Q4 1 0.4142 1.2002 0.0233 1.00000 0.05 0.22 0.99 H3A 1.68 C3 1.95 O3 2.35 H3C Q5 1 0.2368 0.9914 -0.0004 1.00000 0.05 0.20 1.06 H2C 1.09 H2B 1.13 C2 1.55 O2 Q6 1 -0.0003 0.3963 0.0362 1.00000 0.05 0.20 0.61 H1A 1.16 C1 1.58 H1B 1.85 O1 Q7 1 0.1435 0.5343 0.0007 1.00000 0.05 0.19 0.83 O1 1.79 H18 1.79 C5 2.03 C1 Q8 1 0.5720 0.0664 0.3626 1.00000 0.05 0.19 1.57 C17 1.66 C18 1.96 H17 2.08 H18 Q9 1 0.7147 0.3326 0.1661 1.00000 0.05 0.19 1.14 H22C 2.07 C22 2.23 H23B 2.42 H22A Q10 1 0.2344 0.7285 0.3071 1.00000 0.05 0.19 1.04 H14B 1.71 C14 2.00 H14A 2.13 H4 Q11 1 0.5470 0.8821 0.1848 1.00000 0.05 0.19 1.50 H8 1.62 O7 2.33 C22 2.40 H10 Q12 1 0.3261 0.7888 0.1434 1.00000 0.05 0.19 0.92 C8 1.49 C9 1.51 H8 1.60 C7 Q13 1 0.3960 1.2315 -0.0090 1.00000 0.05 0.19 1.74 H3A 1.75 H23C 2.44 C3 2.46 O3 Q14 1 -0.0656 0.3566 0.0042 1.00000 0.05 0.18 1.26 H1A 1.54 O1 2.03 O2 2.17 C1 Q15 1 0.3056 0.2591 0.1375 1.00000 0.05 0.18 1.46 H4 1.73 H14B 2.20 O4 2.22 H3C Q16 1 0.1817 0.9859 -0.0386 1.00000 0.05 0.18 0.67 C2 0.85 H2B 0.92 H2C 1.19 H2A Q17 1 0.0258 0.5727 0.0197 1.00000 0.05 0.18 1.35 O1 1.56 H1A 1.89 H17 2.00 H1A Q18 1 0.3171 1.2203 0.0539 1.00000 0.05 0.18 1.85 H3A 1.98 O3 2.11 H1C 2.14 C3 Q19 1 0.5694 0.6778 0.3706 1.00000 0.05 0.18 1.61 O6 1.77 H2A 2.40 H1B 2.49 C13 Q20 1 0.1955 1.1319 -0.0452 1.00000 0.05 0.18 1.55 H2C 1.62 H2B 1.86 C2 2.11 C18 Shortest distances between peaks (including symmetry equivalents) 4 13 0.80 14 17 0.93 5 16 1.07 6 14 1.09 16 20 1.20 2 5 1.23 7 14 1.28 6 17 1.32 4 18 1.37 10 15 1.38 2 16 1.39 7 17 1.50 6 17 1.51 3 16 1.55 1 2 1.56 17 17 1.59 5 20 1.59 1 5 1.66 13 18 1.73 3 20 1.80 3 19 1.91 15 18 1.93 6 7 1.95 1 16 1.98 14 17 2.08 6 7 2.21 7 17 2.22 2 20 2.33 6 14 2.34 6 6 2.35 2 14 2.38 5 18 2.40 1 7 2.45 2 3 2.54 1 14 2.55 3 5 2.59 13 20 2.61 5 13 2.72 18 20 2.73 4 5 2.73 16 19 2.76 14 14 2.80 6 8 2.83 11 12 2.85 7 14 2.86 6 19 2.89 8 17 2.95 4 15 2.97 9 19 2.99 2 7 2.99 Time profile in seconds ----------------------- 0.16: Read and process instructions 0.00: Fit rigid groups 0.02: Interpret restraints etc. 0.00: Generate connectivity array 0.02: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 2.28: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.02: Generate idealized H-atoms 1.33: Structure factors and derivatives 1.84: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.44: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.08: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 16:25:44 Total CPU time: 6.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++