+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 17:12:50 on 04-Aug-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 01cce003 in P2(1)/c CELL 0.71073 12.6651 13.6078 12.3362 90 95.807 90 ZERR 4 0.0005 0.0007 0.0005 0 0.003 0 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 88 112 16 8 V = 2115.16 F(000) = 816.0 Mu = 0.08 mm-1 Cell Wt = 1521.94 Rho = 1.195 SHEL 7 0.9 TEMP -123 SIZE 0.2 0.2 0.1 FMAP 2 PLAN 30 L.S. 4 WGHT 0.082800 EXTI 0.013573 FVAR 0.34845 H7 2 0.665470 0.202674 0.346245 11.00000 0.02640 H8 2 0.761422 0.175465 0.194775 11.00000 0.03916 H11 2 0.514182 0.079132 0.764154 11.00000 0.03406 H12 2 0.656443 0.043316 0.658841 11.00000 0.04518 H13 2 0.639260 0.084976 0.467806 11.00000 0.03041 H16A 2 0.276626 0.427284 0.353039 11.00000 0.05343 H16B 2 0.157268 0.431863 0.389082 11.00000 0.04687 H16C 2 0.246291 0.367948 0.461399 11.00000 0.04327 H17A 2 0.203742 0.392255 0.175566 11.00000 0.05046 H17B 2 0.082750 0.372944 0.200815 11.00000 0.06039 H17C 2 0.140914 0.290241 0.142069 11.00000 0.05475 H18A 2 0.131083 0.233226 0.442456 11.00000 0.03866 H18B 2 0.046363 0.290151 0.362367 11.00000 0.04017 H20A 2 -0.061590 0.059773 0.369084 11.00000 0.06345 H20B 2 -0.088188 0.174694 0.378493 11.00000 0.08348 H20C 2 -0.006280 0.119986 0.470532 11.00000 0.07825 H21A 2 0.077806 0.155048 0.147424 11.00000 0.07744 H21B 2 -0.033204 0.204335 0.184581 11.00000 0.06463 H21C 2 -0.023980 0.080385 0.183933 11.00000 0.06416 H22A 2 0.199949 0.071914 0.288841 11.00000 0.07535 H22B 2 0.173599 0.057603 0.416521 11.00000 0.05963 H22C 2 0.108674 -0.005082 0.322991 11.00000 0.06241 C1 1 0.856515 0.099703 -0.072687 11.00000 0.03633 0.07432 = 0.04468 -0.00647 0.02024 -0.00729 C2 1 0.690619 0.109458 -0.003728 11.00000 0.02367 0.03668 = 0.03399 0.00475 0.00125 0.00108 C3 1 0.633306 0.132282 0.092287 11.00000 0.02388 0.02895 = 0.02976 0.00256 0.00355 0.00178 C4 1 0.523634 0.117400 0.084103 11.00000 0.02559 0.03086 = 0.02945 0.00054 -0.00239 0.00360 C5 1 0.468359 0.131151 0.173456 11.00000 0.01928 0.02890 = 0.03640 0.00186 0.00248 0.00341 C6 1 0.520035 0.160901 0.273858 11.00000 0.02054 0.02631 = 0.03441 -0.00150 0.00306 0.00394 C7 1 0.629785 0.178039 0.279908 11.00000 0.02337 0.03856 = 0.03196 -0.00887 0.00068 -0.00245 C8 1 0.685344 0.163327 0.190763 11.00000 0.01970 0.03859 = 0.03971 -0.00343 0.00519 -0.00296 C9 1 0.356533 0.206548 0.376406 11.00000 0.01994 0.03091 = 0.02690 0.00034 0.00196 0.00086 C10 1 0.411900 0.158236 0.537113 11.00000 0.02433 0.02914 = 0.02840 -0.00466 0.00071 -0.00141 C11 1 0.509522 0.095993 0.686056 11.00000 0.03896 0.03222 = 0.03185 -0.00181 -0.00706 0.00166 C12 1 0.594014 0.075069 0.625098 11.00000 0.03196 0.03538 = 0.04072 -0.00308 -0.01045 0.00573 C13 1 0.586026 0.097344 0.517791 11.00000 0.02397 0.03268 = 0.04231 -0.00363 -0.00321 0.00428 C14 1 0.459538 0.172449 0.367444 11.00000 0.02220 0.02900 = 0.02911 -0.00093 0.00047 0.00078 C15 1 0.193119 0.301605 0.310309 11.00000 0.02333 0.03798 = 0.03395 0.00201 0.00357 0.00941 C16 1 0.223888 0.389289 0.384295 11.00000 0.03540 0.03787 = 0.05644 0.00011 0.00542 0.00256 C17 1 0.152907 0.342112 0.197469 11.00000 0.03007 0.05862 = 0.04625 0.01492 0.00379 0.01550 C18 1 0.107141 0.243203 0.362655 11.00000 0.02174 0.04055 = 0.03224 -0.00191 0.00400 0.00870 C19 1 0.060906 0.143661 0.321242 11.00000 0.02433 0.04498 = 0.04342 -0.00691 0.00036 0.00035 C20 1 -0.030635 0.121531 0.390304 11.00000 0.03743 0.05598 = 0.07814 -0.00444 0.01220 -0.01259 C21 1 0.016402 0.144437 0.201366 11.00000 0.05186 0.06813 = 0.05593 -0.01356 -0.01369 -0.00732 C22 1 0.141880 0.060505 0.338940 11.00000 0.04020 0.04293 = 0.07644 -0.00997 -0.00582 0.00025 N1 3 0.328000 0.197882 0.479553 11.00000 0.01933 0.03619 = 0.02875 0.00107 0.00083 0.00211 N2 3 0.419340 0.135746 0.643353 11.00000 0.03057 0.03472 = 0.02794 -0.00097 -0.00250 0.00094 N3 3 0.495387 0.142162 0.472616 11.00000 0.02010 0.02814 = 0.03086 -0.00380 -0.00184 0.00183 N4 3 0.287722 0.242077 0.292491 11.00000 0.02244 0.04209 = 0.02877 0.00611 0.00580 0.00810 O1 4 0.650961 0.074860 -0.087595 11.00000 0.03145 0.07046 = 0.03072 -0.00408 0.00058 0.00057 O2 4 0.794910 0.129619 0.013593 11.00000 0.02739 0.06094 = 0.04094 -0.00934 0.01377 -0.01085 MOLE 0 H1A 2 0.928260 0.114171 -0.045979 11.00000 0.05653 H1B 2 0.830756 0.134744 -0.140734 11.00000 0.05902 H1C 2 0.843809 0.029249 -0.088985 11.00000 0.08056 H4 2 0.489537 0.096242 0.014570 11.00000 0.02099 H4N 2 0.321714 0.265966 0.238822 11.00000 0.03998 H5 2 0.391790 0.115475 0.168562 11.00000 0.04259 HKLF 4 1.0 0.00 0.00 1.00 0.00 -1.00 0.00 1.00 0.00 0.00 Covalent radii and connectivity table for 01cce003 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 C1 - O2 C2 - O1 O2 C3 C3 - C8 C4 C2 C4 - C5 C3 C5 - C4 C6 C6 - C5 C7 C14 C7 - C8 C6 C8 - C7 C3 C9 - N1 N4 C14 C10 - N1 N2 N3 C11 - N2 C12 C12 - C13 C11 C13 - C12 N3 C14 - N3 C9 C6 C15 - N4 C16 C17 C18 C16 - C15 C17 - C15 C18 - C15 C19 C19 - C22 C21 C20 C18 C20 - C19 C21 - C19 C22 - C19 N1 - C10 C9 N2 - C11 C10 N3 - C13 C14 C10 N4 - C9 C15 O1 - C2 O2 - C2 C1 16865 Reflections read, of which 3671 rejected -14 =< h =< 14, -15 =< k =< 15, -13 =< l =< 13, 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) -2 2 4 43.05 0.95 5 4.85 1 2 5 267.85 1.05 5 57.18 -3 2 6 167.82 1.18 5 27.57 -3 3 6 76.81 0.52 5 13.74 1 4 6 55.51 1.09 5 7.12 -4 3 7 24.35 0.44 2 20.08 1 6 8 18.67 0.64 5 4.71 0 8 9 8.68 0.65 5 3.77 4 3 10 64.26 0.60 6 21.78 4 4 10 21.19 1.02 4 7.88 10 Inconsistent equivalents 3030 Unique reflections, of which 0 suppressed R(int) = 0.0684 R(sigma) = 0.0496 Friedel opposites merged Maximum memory for data reduction = 2227 / 30404 Least-squares cycle 1 Maximum vector length = 511 Memory required = 3097 / 464940 wR2 = 0.1215 before cycle 1 for 3030 data and 366 / 366 parameters GooF = S = 0.968; Restrained GooF = 0.968 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0828 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34845 0.00108 0.001 OSF 2 0.01357 0.00208 0.000 EXTI Mean shift/esd = 0.002 Maximum = 0.005 for y H20C Max. shift = 0.000 A for H20C Max. dU = 0.000 for H20C Least-squares cycle 2 Maximum vector length = 511 Memory required = 3097 / 464940 wR2 = 0.1216 before cycle 2 for 3030 data and 366 / 366 parameters GooF = S = 0.968; Restrained GooF = 0.968 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0828 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34845 0.00108 0.000 OSF 2 0.01357 0.00208 0.000 EXTI Mean shift/esd = 0.001 Maximum = 0.003 for y H20C Max. shift = 0.000 A for H20C Max. dU = 0.000 for H20C Least-squares cycle 3 Maximum vector length = 511 Memory required = 3097 / 464940 wR2 = 0.1215 before cycle 3 for 3030 data and 366 / 366 parameters GooF = S = 0.968; Restrained GooF = 0.968 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0828 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34845 0.00108 0.000 OSF 2 0.01357 0.00208 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for y H20C Max. shift = 0.000 A for H20C Max. dU = 0.000 for H20C Least-squares cycle 4 Maximum vector length = 511 Memory required = 3097 / 464940 wR2 = 0.1215 before cycle 4 for 3030 data and 366 / 366 parameters GooF = S = 0.968; Restrained GooF = 0.968 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0828 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34845 0.00108 0.000 OSF 2 0.01357 0.00208 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H20C Max. dU = 0.000 for H20C No correlation matrix elements larger than 0.500 01cce003 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq H7 0.66547 0.20267 0.34624 1.00000 0.02639 0.03556 0.00149 0.00141 0.00141 0.00000 0.00489 H8 0.76143 0.17546 0.19478 1.00000 0.03917 0.03846 0.00182 0.00155 0.00157 0.00000 0.00574 H11 0.51419 0.07913 0.76416 1.00000 0.03407 0.03571 0.00160 0.00146 0.00170 0.00000 0.00542 H12 0.65645 0.04332 0.65884 1.00000 0.04519 0.03832 0.00180 0.00169 0.00160 0.00000 0.00628 H13 0.63926 0.08498 0.46781 1.00000 0.03042 0.03428 0.00167 0.00143 0.00152 0.00000 0.00521 H16A 0.27662 0.42728 0.35303 1.00000 0.05343 0.04334 0.00207 0.00179 0.00178 0.00000 0.00705 H16B 0.15727 0.43186 0.38909 1.00000 0.04687 0.03904 0.00194 0.00168 0.00163 0.00000 0.00622 H16C 0.24629 0.36795 0.46140 1.00000 0.04328 0.03929 0.00178 0.00164 0.00184 0.00000 0.00614 H17A 0.20375 0.39226 0.17557 1.00000 0.05046 0.04307 0.00205 0.00179 0.00174 0.00000 0.00686 H17B 0.08275 0.37294 0.20081 1.00000 0.06040 0.04348 0.00225 0.00182 0.00176 0.00000 0.00744 H17C 0.14091 0.29024 0.14207 1.00000 0.05476 0.04603 0.00187 0.00196 0.00190 0.00000 0.00729 H18A 0.13108 0.23323 0.44246 1.00000 0.03867 0.03682 0.00157 0.00147 0.00167 0.00000 0.00568 H18B 0.04636 0.29015 0.36236 1.00000 0.04015 0.03644 0.00176 0.00168 0.00151 0.00000 0.00569 H20A -0.06159 0.05977 0.36908 1.00000 0.06346 0.04934 0.00207 0.00209 0.00193 0.00000 0.00808 H20B -0.08819 0.17469 0.37848 1.00000 0.08347 0.05258 0.00252 0.00238 0.00212 0.00000 0.00966 H20C -0.00630 0.12001 0.47053 1.00000 0.07821 0.05372 0.00243 0.00204 0.00237 0.00000 0.00934 H21A 0.07782 0.15504 0.14742 1.00000 0.07743 0.04910 0.00243 0.00205 0.00219 0.00000 0.00875 H21B -0.03320 0.20433 0.18458 1.00000 0.06462 0.04352 0.00214 0.00217 0.00181 0.00000 0.00783 H21C -0.02397 0.08038 0.18393 1.00000 0.06418 0.05028 0.00213 0.00199 0.00188 0.00000 0.00765 H22A 0.19995 0.07191 0.28884 1.00000 0.07534 0.04810 0.00237 0.00204 0.00217 0.00000 0.00881 H22B 0.17359 0.05759 0.41653 1.00000 0.05965 0.04642 0.00196 0.00183 0.00198 0.00000 0.00744 H22C 0.10867 -0.00508 0.32300 1.00000 0.06240 0.04898 0.00197 0.00218 0.00178 0.00000 0.00749 C1 0.85651 0.09970 -0.07269 1.00000 0.03633 0.07432 0.04468 -0.00648 0.02024 -0.00730 0.05068 0.00550 0.00023 0.00025 0.00021 0.00000 0.00162 0.00226 0.00154 0.00140 0.00120 0.00145 0.00071 C2 0.69062 0.10946 -0.00373 1.00000 0.02367 0.03667 0.03400 0.00474 0.00125 0.00108 0.03156 0.00373 0.00016 0.00015 0.00016 0.00000 0.00121 0.00137 0.00120 0.00094 0.00092 0.00095 0.00053 C3 0.63331 0.13228 0.09229 1.00000 0.02388 0.02895 0.02976 0.00256 0.00355 0.00179 0.02747 0.00348 0.00015 0.00015 0.00015 0.00000 0.00115 0.00119 0.00105 0.00084 0.00083 0.00089 0.00049 C4 0.52363 0.11740 0.08410 1.00000 0.02559 0.03086 0.02945 0.00054 -0.00239 0.00360 0.02899 0.00369 0.00016 0.00015 0.00016 0.00000 0.00119 0.00127 0.00114 0.00088 0.00088 0.00094 0.00051 C5 0.46836 0.13115 0.17346 1.00000 0.01928 0.02890 0.03640 0.00186 0.00248 0.00341 0.02822 0.00368 0.00016 0.00015 0.00015 0.00000 0.00114 0.00122 0.00115 0.00087 0.00087 0.00092 0.00049 C6 0.52003 0.16090 0.27386 1.00000 0.02053 0.02631 0.03441 -0.00150 0.00306 0.00394 0.02706 0.00342 0.00015 0.00014 0.00015 0.00000 0.00110 0.00118 0.00111 0.00084 0.00084 0.00088 0.00049 C7 0.62979 0.17804 0.27991 1.00000 0.02337 0.03856 0.03196 -0.00887 0.00068 -0.00245 0.03144 0.00367 0.00016 0.00016 0.00016 0.00000 0.00120 0.00134 0.00113 0.00093 0.00088 0.00097 0.00052 C8 0.68534 0.16333 0.19076 1.00000 0.01970 0.03859 0.03971 -0.00343 0.00519 -0.00296 0.03252 0.00375 0.00017 0.00016 0.00016 0.00000 0.00121 0.00138 0.00121 0.00093 0.00091 0.00097 0.00053 C9 0.35653 0.20655 0.37641 1.00000 0.01994 0.03091 0.02690 0.00034 0.00196 0.00086 0.02595 0.00330 0.00015 0.00015 0.00014 0.00000 0.00106 0.00120 0.00105 0.00083 0.00079 0.00092 0.00048 C10 0.41190 0.15824 0.53711 1.00000 0.02433 0.02914 0.02840 -0.00466 0.00070 -0.00141 0.02742 0.00326 0.00015 0.00015 0.00014 0.00000 0.00116 0.00122 0.00107 0.00084 0.00087 0.00092 0.00049 C11 0.50952 0.09599 0.68606 1.00000 0.03896 0.03222 0.03185 -0.00182 -0.00706 0.00166 0.03507 0.00366 0.00018 0.00016 0.00017 0.00000 0.00140 0.00131 0.00122 0.00093 0.00099 0.00104 0.00055 C12 0.59401 0.07507 0.62510 1.00000 0.03196 0.03538 0.04072 -0.00308 -0.01045 0.00573 0.03698 0.00377 0.00018 0.00016 0.00017 0.00000 0.00134 0.00137 0.00127 0.00099 0.00101 0.00107 0.00056 C13 0.58603 0.09734 0.51779 1.00000 0.02397 0.03268 0.04232 -0.00363 -0.00321 0.00428 0.03344 0.00362 0.00017 0.00016 0.00017 0.00000 0.00123 0.00130 0.00129 0.00097 0.00098 0.00097 0.00053 C14 0.45954 0.17245 0.36744 1.00000 0.02220 0.02900 0.02911 -0.00093 0.00047 0.00078 0.02692 0.00336 0.00015 0.00015 0.00015 0.00000 0.00113 0.00120 0.00106 0.00081 0.00081 0.00088 0.00049 C15 0.19312 0.30160 0.31031 1.00000 0.02334 0.03798 0.03395 0.00201 0.00357 0.00941 0.03171 0.00365 0.00015 0.00016 0.00015 0.00000 0.00113 0.00133 0.00108 0.00093 0.00083 0.00098 0.00052 C16 0.22389 0.38929 0.38430 1.00000 0.03540 0.03787 0.05644 0.00011 0.00542 0.00256 0.04318 0.00442 0.00021 0.00019 0.00022 0.00000 0.00150 0.00153 0.00161 0.00117 0.00119 0.00123 0.00061 C17 0.15291 0.34211 0.19747 1.00000 0.03007 0.05862 0.04625 0.01492 0.00378 0.01550 0.04499 0.00549 0.00021 0.00023 0.00020 0.00000 0.00143 0.00185 0.00143 0.00131 0.00109 0.00135 0.00065 C18 0.10714 0.24320 0.36266 1.00000 0.02174 0.04055 0.03224 -0.00191 0.00400 0.00870 0.03142 0.00377 0.00017 0.00016 0.00016 0.00000 0.00115 0.00139 0.00116 0.00094 0.00086 0.00101 0.00053 C19 0.06091 0.14366 0.32124 1.00000 0.02433 0.04498 0.04342 -0.00691 0.00036 0.00035 0.03779 0.00371 0.00016 0.00017 0.00016 0.00000 0.00119 0.00146 0.00125 0.00101 0.00093 0.00104 0.00056 C20 -0.03063 0.12153 0.39030 1.00000 0.03743 0.05598 0.07814 -0.00444 0.01221 -0.01259 0.05675 0.00564 0.00023 0.00024 0.00026 0.00000 0.00160 0.00203 0.00209 0.00153 0.00136 0.00150 0.00074 C21 0.01640 0.14444 0.20137 1.00000 0.05185 0.06814 0.05594 -0.01356 -0.01369 -0.00732 0.05995 0.00486 0.00025 0.00027 0.00022 0.00000 0.00181 0.00219 0.00165 0.00142 0.00139 0.00170 0.00078 C22 0.14188 0.06050 0.33894 1.00000 0.04020 0.04293 0.07644 -0.00996 -0.00582 0.00025 0.05399 0.00510 0.00022 0.00022 0.00026 0.00000 0.00159 0.00175 0.00196 0.00137 0.00143 0.00131 0.00070 N1 0.32800 0.19788 0.47955 1.00000 0.01933 0.03619 0.02875 0.00107 0.00083 0.00211 0.02820 0.00273 0.00012 0.00012 0.00011 0.00000 0.00093 0.00106 0.00090 0.00073 0.00069 0.00078 0.00043 N2 0.41934 0.13575 0.64335 1.00000 0.03057 0.03472 0.02794 -0.00097 -0.00250 0.00094 0.03145 0.00286 0.00013 0.00013 0.00012 0.00000 0.00105 0.00106 0.00091 0.00073 0.00073 0.00081 0.00045 N3 0.49539 0.14216 0.47262 1.00000 0.02010 0.02814 0.03086 -0.00380 -0.00184 0.00183 0.02667 0.00268 0.00012 0.00012 0.00012 0.00000 0.00092 0.00098 0.00089 0.00070 0.00070 0.00073 0.00042 N4 0.28772 0.24208 0.29249 1.00000 0.02244 0.04209 0.02877 0.00611 0.00581 0.00810 0.03088 0.00301 0.00013 0.00013 0.00013 0.00000 0.00097 0.00113 0.00092 0.00078 0.00074 0.00080 0.00045 O1 0.65096 0.07486 -0.08759 1.00000 0.03145 0.07047 0.03072 -0.00408 0.00058 0.00057 0.04439 0.00265 0.00011 0.00012 0.00011 0.00000 0.00090 0.00122 0.00083 0.00074 0.00066 0.00080 0.00045 O2 0.79491 0.12962 0.01359 1.00000 0.02739 0.06094 0.04094 -0.00934 0.01377 -0.01085 0.04239 0.00254 0.00011 0.00012 0.00011 0.00000 0.00089 0.00112 0.00085 0.00070 0.00066 0.00073 0.00044 H1A 0.92825 0.11417 -0.04598 1.00000 0.05652 0.04783 0.00230 0.00177 0.00185 0.00000 0.00731 H1B 0.83074 0.13473 -0.14075 1.00000 0.05903 0.04456 0.00196 0.00185 0.00204 0.00000 0.00751 H1C 0.84381 0.02924 -0.08898 1.00000 0.08058 0.05499 0.00225 0.00247 0.00209 0.00000 0.00974 H4 0.48954 0.09624 0.01457 1.00000 0.02099 0.03498 0.00150 0.00130 0.00147 0.00000 0.00465 H4N 0.32171 0.26596 0.23882 1.00000 0.03997 0.03702 0.00176 0.00154 0.00169 0.00000 0.00623 H5 0.39178 0.11548 0.16856 1.00000 0.04259 0.03878 0.00192 0.00154 0.00152 0.00000 0.00610 Final Structure Factor Calculation for 01cce003 in P2(1)/c Total number of l.s. parameters = 366 Maximum vector length = 511 Memory required = 2731 / 22995 wR2 = 0.1215 before cycle 5 for 3030 data and 0 / 366 parameters GooF = S = 0.968; Restrained GooF = 0.968 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0828 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0443 for 2264 Fo > 4sig(Fo) and 0.0644 for all 3030 data wR2 = 0.1215, GooF = S = 0.968, Restrained GooF = 0.968 for all data Occupancy sum of asymmetric unit = 28.00 for non-hydrogen and 28.00 for hydrogen atoms Principal mean square atomic displacements U 0.0781 0.0520 0.0220 C1 0.0403 0.0310 0.0233 C2 0.0322 0.0269 0.0233 C3 0.0347 0.0309 0.0214 C4 0.0368 0.0296 0.0182 C5 0.0348 0.0281 0.0183 C6 0.0447 0.0280 0.0216 C7 0.0429 0.0358 0.0189 C8 0.0310 0.0270 0.0199 C9 0.0335 0.0266 0.0221 C10 0.0482 0.0319 0.0251 C11 0.0547 0.0340 0.0222 C12 0.0470 0.0318 0.0215 C13 0.0307 0.0283 0.0218 C14 0.0428 0.0336 0.0187 C15 0.0564 0.0394 0.0337 C16 0.0718 0.0410 0.0222 C17 0.0443 0.0322 0.0178 C18 0.0516 0.0376 0.0241 C19 0.0801 0.0599 0.0302 C20 0.0795 0.0692 0.0312 C21 0.0836 0.0417 0.0367 C22 0.0365 0.0292 0.0189 N1 0.0366 0.0336 0.0241 N2 0.0355 0.0256 0.0189 N3 0.0470 0.0264 0.0192 N4 0.0709 0.0337 0.0286 O1 0.0685 0.0387 0.0200 O2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.007 0.013 0.020 0.027 0.036 0.046 0.059 0.078 0.112 1.000 Number in group 346. 263. 306. 301. 310. 313. 286. 307. 293. 305. GooF 0.806 0.910 0.976 1.060 1.053 0.925 1.062 0.871 0.947 1.051 K 1.575 0.932 0.962 0.987 0.985 0.986 0.981 1.009 1.021 1.032 Resolution(A) 0.90 0.93 0.97 1.02 1.07 1.13 1.22 1.34 1.53 1.94 inf Number in group 314. 294. 317. 286. 304. 304. 309. 295. 305. 302. GooF 0.920 0.877 0.909 0.969 0.928 0.917 0.893 0.935 1.118 1.169 K 0.994 1.024 1.023 1.001 1.018 1.035 1.031 1.046 1.042 1.016 R1 0.145 0.118 0.094 0.072 0.064 0.054 0.054 0.050 0.047 0.042 Recommended weighting scheme: WGHT 0.0721 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) -3 3 5 44.83 26.20 4.21 0.021 1.99 2 2 2 44.69 61.30 3.62 0.032 3.57 5 3 10 109.47 152.19 3.46 0.050 1.03 -7 2 5 267.33 207.17 3.12 0.059 1.49 -6 1 3 327.46 257.40 3.09 0.065 1.93 -6 2 5 483.68 381.04 3.05 0.080 1.63 1 5 10 137.42 185.30 3.00 0.056 1.11 0 11 8 6.73 28.92 3.00 0.022 0.96 -1 3 12 -5.16 8.86 2.98 0.012 1.00 2 3 3 0.70 5.67 2.96 0.010 2.66 8 2 1 1072.61 856.25 2.93 0.119 1.50 -1 3 1 316.45 400.42 2.91 0.082 4.07 -6 1 8 24.11 11.28 2.90 0.014 1.30 -1 5 2 297.95 377.67 2.89 0.079 2.46 6 2 3 97.70 74.14 2.88 0.035 1.74 5 0 4 93.60 66.31 2.87 0.033 1.86 -2 7 6 11.53 0.13 2.87 0.001 1.40 -4 5 8 15.94 32.15 2.87 0.023 1.27 -12 2 4 63.37 99.37 2.87 0.041 1.01 -12 1 8 122.36 79.43 2.85 0.036 0.91 0 1 4 131.26 165.11 2.82 0.052 2.99 -10 4 8 213.93 276.96 2.80 0.068 0.98 0 4 2 2304.54 2878.50 2.79 0.219 2.98 8 9 2 -10.22 15.64 2.78 0.016 1.06 4 5 10 -0.01 13.02 2.76 0.015 1.02 -9 4 6 46.16 26.01 2.76 0.021 1.14 4 2 5 10.19 2.48 2.71 0.006 1.78 -7 3 2 129.44 165.76 2.70 0.053 1.65 -1 8 9 16.36 30.01 2.70 0.022 1.07 -6 7 10 39.15 74.70 2.69 0.035 0.96 0 4 4 47.85 62.31 2.65 0.032 2.28 -9 3 7 65.66 93.00 2.64 0.039 1.12 6 4 11 47.62 20.59 2.61 0.019 0.91 3 5 5 116.86 146.91 2.60 0.049 1.63 -10 4 5 94.91 129.52 2.60 0.046 1.11 -1 1 6 2.71 7.39 2.60 0.011 2.03 8 4 5 12.06 26.41 2.58 0.021 1.19 2 9 1 77.66 106.96 2.54 0.042 1.46 1 2 10 25.59 41.70 2.54 0.026 1.19 -2 1 13 40.45 0.43 2.51 0.003 0.95 7 2 0 71.95 49.57 2.51 0.029 1.74 -2 8 2 57.69 40.30 2.50 0.026 1.60 7 8 7 4.54 26.43 2.50 0.021 0.98 6 8 3 150.23 192.63 2.48 0.057 1.23 8 0 2 1701.90 1390.92 2.47 0.152 1.49 6 13 2 361.70 278.38 2.47 0.068 0.92 4 7 11 178.64 136.40 2.47 0.048 0.90 -2 5 6 36.48 50.22 2.47 0.029 1.61 -1 3 3 402.17 489.36 2.46 0.090 3.01 -11 6 4 113.65 148.60 2.45 0.050 1.00 FMAP and GRID set by program FMAP 2 3 15 GRID -2.083 -2 -2 2.083 2 2 R1 = 0.0643 for 3030 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.18 at 0.0170 0.1280 0.2090 [ 0.24 A from C21 ] Deepest hole -0.23 at 0.7177 0.7189 0.1259 [ 0.95 A from C9 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 2711 / 18615 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3563 0.1225 0.3592 1.00000 0.05 0.17 1.16 C9 1.47 C14 1.87 N1 1.98 N4 Q2 1 0.6511 0.0937 0.1534 1.00000 0.05 0.17 0.93 C3 1.12 C8 1.78 C4 1.82 H8 Q3 1 0.8626 0.1770 0.1019 1.00000 0.05 0.16 1.47 O2 1.63 H21B 1.80 H8 2.13 H21C Q4 1 0.3008 0.1440 0.2735 1.00000 0.05 0.16 1.37 N4 1.63 C9 1.64 H22A 1.74 H4N Q5 1 0.4790 0.1403 0.4217 1.00000 0.05 0.16 0.64 N3 0.82 C14 1.75 C10 1.81 C13 Q6 1 0.6035 0.1408 0.5851 1.00000 0.05 0.15 1.03 C13 1.03 C12 1.71 H12 1.73 H13 Q7 1 0.3320 0.3969 0.2707 1.00000 0.05 0.15 1.36 H16A 1.83 H4N 1.91 H17A 2.06 N2 Q8 1 0.1936 0.3536 0.3215 1.00000 0.05 0.15 0.72 C15 0.96 C16 1.46 H16B 1.48 H16A Q9 1 0.6722 0.1638 -0.0926 1.00000 0.05 0.15 1.24 O1 1.32 C2 1.97 H7 1.98 O2 Q10 1 0.4994 0.0874 0.2303 1.00000 0.05 0.15 0.97 C5 1.15 C6 1.54 H5 1.90 C4 Q11 1 0.2955 0.1079 0.4127 1.00000 0.05 0.14 1.51 N1 1.63 C9 1.69 H22B 1.91 H22A Q12 1 0.6741 0.1449 0.3657 1.00000 0.05 0.14 0.83 H7 1.23 C7 1.60 H13 2.17 C6 Q13 1 0.8629 0.1547 -0.1252 1.00000 0.05 0.14 0.51 H1B 1.00 C1 1.33 H1A 1.79 H1C Q14 1 0.3998 0.1426 0.5688 1.00000 0.05 0.14 0.48 C10 0.93 N2 1.55 N1 1.78 N3 Q15 1 0.7567 0.1137 0.4177 1.00000 0.05 0.13 1.71 H13 1.84 H7 2.23 H20B 2.38 C7 Q16 1 0.2678 0.4183 0.2887 1.00000 0.05 0.13 0.80 H16A 1.41 C16 1.58 H17A 1.88 C15 Q17 1 0.6483 0.1816 0.1173 1.00000 0.05 0.13 0.76 C3 1.01 C8 1.64 H8 1.82 C4 Q18 1 0.8015 0.0843 -0.1685 1.00000 0.05 0.13 0.84 H1B 1.31 H1C 1.33 C1 2.13 H1A Q19 1 0.7990 0.1259 0.5006 1.00000 0.05 0.13 2.10 H13 2.28 H20B 2.53 H20C 2.63 H7 Q20 1 -0.1656 0.0837 0.4547 1.00000 0.05 0.13 1.80 H20A 1.89 H20B 2.02 C20 2.07 H20C Q21 1 0.4484 0.1028 0.3696 1.00000 0.05 0.13 0.96 C14 1.45 N3 1.75 C6 1.84 C9 Q22 1 0.7846 0.1329 0.5197 1.00000 0.05 0.13 2.00 H13 2.55 H20B 2.56 C13 2.67 H7 Q23 1 0.1234 0.3789 0.4772 1.00000 0.05 0.12 1.41 H16B 1.60 H16C 1.80 C16 2.03 H18A Q24 1 0.3073 0.1002 0.5168 1.00000 0.05 0.12 1.44 N1 1.54 C10 2.06 N2 2.08 H22B Q25 1 0.7979 0.1954 0.0211 1.00000 0.05 0.12 0.90 O2 1.80 C2 1.94 C1 2.22 H1A Q26 1 0.1680 0.3401 0.1001 1.00000 0.05 0.12 0.94 H17C 1.22 H17A 1.24 C17 1.78 H17B Q27 1 0.0180 0.3784 0.3283 1.00000 0.05 0.12 1.31 H18B 1.85 H17B 1.98 H16B 2.02 H1A Q28 1 0.9513 0.0920 -0.1469 1.00000 0.05 0.12 1.34 H1A 1.59 C1 1.64 H1B 1.81 H1C Q29 1 0.6468 0.1421 -0.1528 1.00000 0.05 0.12 1.22 O1 1.92 C2 2.06 H11 2.13 H7 Q30 1 1.0019 0.0794 -0.1596 1.00000 0.05 0.12 1.82 H1A 1.87 H18B 2.00 H16B 2.19 H17B Shortest distances between peaks (including symmetry equivalents) 19 22 0.32 27 30 0.63 28 30 0.69 9 29 0.83 5 21 0.88 7 16 0.91 19 20 0.95 27 28 1.01 1 11 1.08 15 19 1.12 15 20 1.12 1 21 1.19 1 4 1.24 12 15 1.24 3 25 1.25 20 22 1.26 2 17 1.28 11 24 1.28 15 22 1.30 13 18 1.31 8 16 1.38 14 24 1.40 13 28 1.45 1 5 1.68 4 11 1.79 18 28 1.89 10 21 1.91 7 8 2.01 9 25 2.06 11 21 2.06 13 30 2.12 1 24 2.12 13 25 2.13 18 29 2.14 13 27 2.15 23 27 2.16 5 14 2.16 4 21 2.18 12 19 2.19 8 23 2.22 2 10 2.23 23 30 2.24 9 18 2.24 12 22 2.25 8 27 2.26 11 14 2.27 24 26 2.28 17 25 2.34 22 25 2.34 5 11 2.36 12 20 2.36 5 6 2.43 19 25 2.44 9 13 2.49 6 17 2.50 5 10 2.51 6 22 2.51 18 30 2.53 23 28 2.56 6 14 2.57 1 10 2.57 1 14 2.60 8 30 2.63 5 24 2.63 5 12 2.63 9 17 2.65 14 21 2.65 9 12 2.65 2 16 2.67 21 24 2.67 2 12 2.70 8 26 2.72 13 29 2.73 4 10 2.73 3 17 2.74 16 26 2.75 10 12 2.75 4 5 2.76 7 14 2.77 10 17 2.77 6 19 2.79 18 25 2.79 18 27 2.79 3 13 2.82 25 29 2.82 2 7 2.84 7 26 2.91 3 22 2.91 15 25 2.92 12 21 2.92 12 29 2.92 6 12 2.94 2 25 2.94 6 15 3.00 Time profile in seconds ----------------------- 0.22: 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 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.50: Structure factors and derivatives 3.08: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.73: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.05: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 17:13:00 Total CPU time: 8.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++