+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + an8809 started at 14:56:35 on 27-Aug-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL AN8809r in P2(1)2(1)2(1) CELL 0.71073 7.2921 8.0475 26.3777 90.000 90.000 90.000 ZERR 4.00 0.0015 0.0016 0.0053 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, - Z SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H O UNIT 72 96 8 V = 1547.93 F(000) = 592.0 Mu = 0.07 mm-1 Cell Wt = 1089.49 Rho = 1.169 MERG 4 HFIX 43 -1.20 C12 HFIX 23 -1.20 C2 C5 C9 C11 C14 C15 C16 C17 HFIX 13 -1.20 C1 C3 C4 C8 HFIX 137 -1.50 C10 FMAP 2 PLAN 25 SIZE 0.28 0.48 0.50 ACTA 55.00 BOND $H WGHT 0.20000 L.S. 10 TEMP 0.00 FVAR 0.29947 C1 1 0.381684 0.012409 0.861710 11.00000 0.05240 0.04755 = 0.04984 -0.00665 -0.00150 -0.01083 C2 1 0.380802 0.246381 0.926127 11.00000 0.06574 0.04393 = 0.06156 -0.00525 0.00671 -0.00212 C3 1 0.492276 0.157193 0.884456 11.00000 0.04742 0.04379 = 0.04864 -0.00345 -0.00832 0.00270 O2 3 0.139475 -0.156292 1.024211 11.00000 0.14484 0.08596 = 0.07379 0.01327 0.03528 -0.02503 C4 1 0.326759 -0.101656 0.904273 11.00000 0.05194 0.03965 = 0.05367 -0.00235 0.00137 -0.00615 C5 1 0.495229 -0.077536 0.821435 11.00000 0.08012 0.06721 = 0.06670 -0.02698 0.01124 -0.01676 C6 1 0.661216 0.185441 0.803227 11.00000 0.07330 0.07729 = 0.05186 0.00029 0.00357 -0.01817 C7 1 0.204314 -0.013393 0.943969 11.00000 0.04691 0.05958 = 0.05383 0.00565 0.00086 0.00207 C8 1 0.565643 0.278267 0.844272 11.00000 0.05317 0.05481 = 0.05770 0.00890 -0.00078 -0.00915 C9 1 0.311724 0.127474 0.967546 11.00000 0.08400 0.05659 = 0.05280 -0.01541 0.01087 -0.01016 O1 3 1.097622 0.385333 0.799725 11.00000 0.07797 0.14311 = 0.17097 0.03190 0.00221 -0.04077 C10 1 0.018342 0.043878 0.923107 11.00000 0.05298 0.09474 = 0.07503 0.00575 0.00516 0.01944 C11 1 0.225331 -0.265153 0.893899 11.00000 0.08721 0.06591 = 0.07968 -0.01884 0.01255 -0.02850 C12 1 0.836657 0.221839 0.790399 11.00000 0.06905 0.09637 = 0.06659 0.00290 0.01379 -0.01345 C13 1 0.161719 -0.161688 0.978453 11.00000 0.06591 0.07328 = 0.06178 0.00676 0.01006 -0.00212 C14 1 0.156292 -0.316701 0.947129 11.00000 0.09254 0.05615 = 0.08676 0.00084 0.01292 -0.01763 C15 1 0.557371 0.041070 0.780644 11.00000 0.10033 0.11287 = 0.05074 -0.02675 0.01753 -0.04585 C16 1 0.819212 0.493632 0.832567 11.00000 0.08528 0.09749 = 0.12336 0.00017 -0.02167 -0.04828 C17 1 0.686585 0.409213 0.871224 11.00000 0.08611 0.06282 = 0.08660 -0.00319 -0.00357 -0.02334 C18 1 0.933801 0.365741 0.808262 11.00000 0.06176 0.12022 = 0.09028 0.03015 -0.00132 -0.02098 HKLF 4 Covalent radii and connectivity table for AN8809r in P2(1)2(1)2(1) C 0.770 H 0.320 O 0.660 C1 - C4 C5 C3 C2 - C9 C3 C3 - C8 C1 C2 O2 - C13 C4 - C1 C11 C7 C5 - C15 C1 C6 - C12 C8 C15 C7 - C9 C13 C10 C4 C8 - C6 C3 C17 C9 - C7 C2 O1 - C18 C10 - C7 C11 - C4 C14 C12 - C6 C18 C13 - O2 C14 C7 C14 - C13 C11 C15 - C5 C6 C16 - C18 C17 C17 - C8 C16 C18 - O1 C12 C16 2077 Reflections read, of which 0 rejected 0 =< h =< 9, 0 =< k =< 10, 0 =< l =< 34, Max. 2-theta = 55.49 0 Systematic absence violations 0 Inconsistent equivalents 2072 Unique reflections, of which 0 suppressed R(int) = 0.0093 R(sigma) = 0.0060 Friedel opposites merged Maximum memory for data reduction = 2263 / 20327 Default effective X-H distances for T = 0.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 0.98 0.97 0.96 0.93 0.86 0.89 1.10 0.82 0.93 0.86 0.93 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. Difference electron density (eA^-3x100) at 15 degree intervals for AFIX 137 group attached to C10 The center of the range is eclipsed (cis) to C9 and rotation is clockwise looking down C7 to C10 12 24 32 41 45 37 20 6 5 16 22 18 16 14 6 0 1 7 15 27 33 24 7 2 After local symmetry averaging: 6 15 23 29 32 25 11 3 Least-squares cycle 1 Maximum vector length = 511 Memory required = 2829 / 224994 wR2 = 0.4555 before cycle 1 for 2072 data and 182 / 182 parameters GooF = S = 2.465; Restrained GooF = 2.465 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.30131 0.00427 0.430 OSF 167 0.87008 0.00028 -4.142 z C17 Mean shift/su = 0.574 Maximum = -4.142 for z C17 Max. shift = 0.034 A for C17 Max. dU =-0.004 for O1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2829 / 224994 wR2 = 0.4280 before cycle 2 for 2072 data and 182 / 182 parameters GooF = S = 2.286; Restrained GooF = 2.286 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.30230 0.00396 0.250 OSF Mean shift/su = 0.316 Maximum = -1.441 for z C17 Max. shift = 0.032 A for H10A Max. dU = 0.001 for C5 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2829 / 224994 wR2 = 0.4257 before cycle 3 for 2072 data and 182 / 182 parameters GooF = S = 2.268; Restrained GooF = 2.268 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.30248 0.00395 0.047 OSF Mean shift/su = 0.122 Maximum = -0.539 for U22 C16 Max. shift = 0.011 A for H10A Max. dU = 0.001 for O1 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2829 / 224994 wR2 = 0.4259 before cycle 4 for 2072 data and 182 / 182 parameters GooF = S = 2.265; Restrained GooF = 2.265 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.30258 0.00396 0.026 OSF Mean shift/su = 0.047 Maximum = -0.177 for U23 C17 Max. shift = 0.001 A for C17 Max. dU = 0.000 for O1 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2829 / 224994 wR2 = 0.4260 before cycle 5 for 2072 data and 182 / 182 parameters GooF = S = 2.265; Restrained GooF = 2.265 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.30263 0.00396 0.011 OSF Mean shift/su = 0.021 Maximum = 0.091 for y C17 Max. shift = 0.001 A for C17 Max. dU = 0.000 for C16 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2829 / 224994 wR2 = 0.4261 before cycle 6 for 2072 data and 182 / 182 parameters GooF = S = 2.266; Restrained GooF = 2.266 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.30264 0.00396 0.003 OSF Mean shift/su = 0.011 Maximum = 0.059 for U23 C16 Max. shift = 0.000 A for C17 Max. dU = 0.000 for C16 Least-squares cycle 7 Maximum vector length = 511 Memory required = 2829 / 224994 wR2 = 0.4262 before cycle 7 for 2072 data and 182 / 182 parameters GooF = S = 2.266; Restrained GooF = 2.266 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.30265 0.00397 0.001 OSF Mean shift/su = 0.006 Maximum = 0.037 for U23 C16 Max. shift = 0.000 A for C17 Max. dU = 0.000 for C16 Least-squares cycle 8 Maximum vector length = 511 Memory required = 2829 / 224994 wR2 = 0.4262 before cycle 8 for 2072 data and 182 / 182 parameters GooF = S = 2.266; Restrained GooF = 2.266 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.30265 0.00397 0.000 OSF Mean shift/su = 0.003 Maximum = 0.023 for U23 C16 Max. shift = 0.000 A for C17 Max. dU = 0.000 for C12 Least-squares cycle 9 Maximum vector length = 511 Memory required = 2829 / 224994 wR2 = 0.4262 before cycle 9 for 2072 data and 182 / 182 parameters GooF = S = 2.266; Restrained GooF = 2.266 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.30265 0.00397 0.000 OSF Mean shift/su = 0.002 Maximum = 0.014 for U23 C16 Max. shift = 0.000 A for C17 Max. dU = 0.000 for C12 Least-squares cycle 10 Maximum vector length = 511 Memory required = 2829 / 224994 wR2 = 0.4262 before cycle 10 for 2072 data and 182 / 182 parameters GooF = S = 2.266; Restrained GooF = 2.266 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.30265 0.00397 0.000 OSF Mean shift/su = 0.001 Maximum = 0.009 for U23 C16 Max. shift = 0.000 A for C17 Max. dU = 0.000 for C12 Largest correlation matrix elements -0.569 U12 C16 / U11 C16 -0.547 U23 C5 / U22 C5 -0.550 U12 C16 / U22 C16 -0.509 U12 C15 / U22 C15 Idealized hydrogen atom generation before cycle 11 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.2715 0.0562 0.8455 13 0.980 0.000 C1 C4 C5 C3 H2A 0.4587 0.3294 0.9418 23 0.970 0.000 C2 C9 C3 H2B 0.2777 0.3018 0.9110 23 0.970 0.000 C2 C9 C3 H3 0.5988 0.1076 0.9009 13 0.980 0.000 C3 C8 C1 C2 H4 0.4386 -0.1328 0.9222 13 0.980 0.000 C4 C1 C11 C7 H5A 0.6012 -0.1289 0.8381 23 0.970 0.000 C5 C15 C1 H5B 0.4222 -0.1665 0.8071 23 0.970 0.000 C5 C15 C1 H8 0.4601 0.3356 0.8291 13 0.980 0.000 C8 C6 C3 C17 H9A 0.4139 0.0845 0.9868 23 0.970 0.000 C9 C7 C2 H9B 0.2325 0.1889 0.9908 23 0.970 0.000 C9 C7 C2 H10A -0.0546 0.0875 0.9505 137 0.960 0.000 C10 C7 H10A H10B -0.0450 -0.0520 0.9091 137 0.960 0.000 C10 C7 H10A H10C 0.0350 0.1249 0.8977 137 0.960 0.000 C10 C7 H10A H11A 0.3067 -0.3474 0.8797 23 0.970 0.000 C11 C4 C14 H11B 0.1228 -0.2477 0.8708 23 0.970 0.000 C11 C4 C14 H12 0.8942 0.1508 0.7668 43 0.930 0.000 C12 C6 C18 H14A 0.0325 -0.3609 0.9449 23 0.970 0.000 C14 C13 C11 H14B 0.2358 -0.4014 0.9612 23 0.970 0.000 C14 C13 C11 H15A 0.4524 0.0819 0.7625 23 0.970 0.000 C15 C5 C6 H15B 0.6362 -0.0181 0.7571 23 0.970 0.000 C15 C5 C6 H16A 0.7519 0.5533 0.8081 23 0.970 0.000 C16 C18 C17 H16B 0.8972 0.5676 0.8518 23 0.970 0.000 C16 C18 C17 H17A 0.7540 0.3623 0.8973 23 0.970 0.000 C17 C8 C16 H17B 0.6082 0.4984 0.8838 23 0.970 0.000 C17 C8 C16 AN8809r in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.38209 0.01188 0.86171 1.00000 0.05036 0.04979 0.05060 -0.00909 -0.00096 -0.00993 0.05025 0.00611 0.00057 0.00051 0.00014 0.00000 0.00185 0.00175 0.00163 0.00151 0.00154 0.00167 0.00093 H1 0.27151 0.05621 0.84550 1.00000 0.06030 0.00000 0.00000 C2 0.38147 0.24551 0.92630 1.00000 0.06690 0.04373 0.06221 -0.00349 0.00248 -0.00245 0.05761 0.00794 0.00073 0.00052 0.00017 0.00000 0.00240 0.00176 0.00206 0.00150 0.00194 0.00183 0.00106 H2A 0.45875 0.32938 0.94183 1.00000 0.06914 0.00000 0.00000 H2B 0.27770 0.30179 0.91098 1.00000 0.06914 0.00000 0.00000 C3 0.49144 0.15672 0.88436 1.00000 0.04634 0.04489 0.04907 -0.00313 -0.00708 0.00036 0.04677 0.00611 0.00055 0.00047 0.00014 0.00000 0.00171 0.00175 0.00167 0.00131 0.00139 0.00141 0.00089 H3 0.59885 0.10761 0.90092 1.00000 0.05612 0.00000 0.00000 O2 0.13988 -0.15664 1.02390 1.00000 0.14697 0.09435 0.06926 0.00901 0.03121 -0.03054 0.10352 0.01050 0.00106 0.00069 0.00016 0.00000 0.00523 0.00346 0.00212 0.00206 0.00313 0.00382 0.00202 C4 0.32522 -0.10200 0.90463 1.00000 0.05210 0.04070 0.05552 -0.00385 0.00175 -0.00501 0.04944 0.00680 0.00059 0.00049 0.00015 0.00000 0.00191 0.00166 0.00174 0.00132 0.00148 0.00161 0.00093 H4 0.43857 -0.13280 0.92224 1.00000 0.05933 0.00000 0.00000 C5 0.49513 -0.07854 0.82211 1.00000 0.08175 0.07212 0.07274 -0.03460 0.01954 -0.02387 0.07554 0.00865 0.00090 0.00077 0.00022 0.00000 0.00321 0.00291 0.00254 0.00240 0.00263 0.00274 0.00159 H5A 0.60121 -0.12886 0.83813 1.00000 0.09065 0.00000 0.00000 H5B 0.42224 -0.16653 0.80709 1.00000 0.09065 0.00000 0.00000 C6 0.66271 0.18516 0.80349 1.00000 0.06843 0.07677 0.05366 0.00014 0.00482 -0.01638 0.06629 0.00903 0.00078 0.00078 0.00017 0.00000 0.00286 0.00281 0.00198 0.00194 0.00199 0.00264 0.00130 C7 0.20524 -0.01336 0.94413 1.00000 0.04716 0.05707 0.05528 0.00335 0.00127 0.00309 0.05317 0.00764 0.00059 0.00057 0.00015 0.00000 0.00191 0.00206 0.00179 0.00165 0.00143 0.00169 0.00100 C8 0.56538 0.27925 0.84454 1.00000 0.05793 0.05717 0.05690 0.00657 -0.00166 -0.01271 0.05733 0.00804 0.00068 0.00059 0.00017 0.00000 0.00217 0.00235 0.00203 0.00162 0.00165 0.00195 0.00111 H8 0.46007 0.33560 0.82914 1.00000 0.06880 0.00000 0.00000 C9 0.31115 0.12821 0.96761 1.00000 0.08118 0.05725 0.05485 -0.01519 0.01194 -0.00991 0.06443 0.00846 0.00084 0.00063 0.00017 0.00000 0.00290 0.00233 0.00187 0.00174 0.00202 0.00231 0.00123 H9A 0.41393 0.08454 0.98678 1.00000 0.07731 0.00000 0.00000 H9B 0.23246 0.18893 0.99076 1.00000 0.07731 0.00000 0.00000 O1 1.09826 0.38433 0.80031 1.00000 0.07626 0.14422 0.16269 0.03296 0.00520 -0.03549 0.12773 0.01436 0.00081 0.00118 0.00032 0.00000 0.00292 0.00628 0.00549 0.00517 0.00366 0.00377 0.00265 C10 0.01750 0.04199 0.92343 1.00000 0.05111 0.09729 0.08068 0.00908 0.00446 0.01584 0.07636 0.01233 0.00073 0.00094 0.00023 0.00000 0.00231 0.00410 0.00276 0.00292 0.00215 0.00269 0.00154 H10A -0.05460 0.08753 0.95053 1.00000 0.11453 0.00000 0.00000 H10B -0.04497 -0.05198 0.90913 1.00000 0.11453 0.00000 0.00000 H10C 0.03502 0.12494 0.89772 1.00000 0.11453 0.00000 0.00000 C11 0.22447 -0.26482 0.89390 1.00000 0.08164 0.06256 0.08295 -0.01713 0.01001 -0.02230 0.07571 0.00982 0.00097 0.00074 0.00023 0.00000 0.00324 0.00279 0.00298 0.00229 0.00270 0.00267 0.00151 H11A 0.30666 -0.34742 0.87973 1.00000 0.09086 0.00000 0.00000 H11B 0.12276 -0.24766 0.87079 1.00000 0.09086 0.00000 0.00000 C12 0.83558 0.22147 0.78946 1.00000 0.07422 0.09252 0.06590 0.00482 0.01758 -0.01278 0.07755 0.01183 0.00090 0.00096 0.00020 0.00000 0.00323 0.00432 0.00247 0.00246 0.00245 0.00329 0.00168 H12 0.89422 0.15077 0.76676 1.00000 0.09306 0.00000 0.00000 C13 0.16101 -0.16052 0.97858 1.00000 0.06929 0.07313 0.06609 0.00619 0.01011 -0.00505 0.06950 0.01061 0.00086 0.00075 0.00020 0.00000 0.00283 0.00303 0.00230 0.00214 0.00226 0.00250 0.00135 C14 0.15626 -0.31709 0.94683 1.00000 0.08749 0.05757 0.08632 0.00054 0.01128 -0.01569 0.07713 0.01135 0.00111 0.00072 0.00023 0.00000 0.00376 0.00238 0.00325 0.00238 0.00308 0.00273 0.00156 H14A 0.03254 -0.36090 0.94493 1.00000 0.09255 0.00000 0.00000 H14B 0.23576 -0.40144 0.96122 1.00000 0.09255 0.00000 0.00000 C15 0.55813 0.04053 0.78090 1.00000 0.09719 0.11086 0.05156 -0.02472 0.01843 -0.04293 0.08653 0.01016 0.00109 0.00102 0.00017 0.00000 0.00401 0.00488 0.00204 0.00254 0.00228 0.00389 0.00214 H15A 0.45235 0.08190 0.76252 1.00000 0.10384 0.00000 0.00000 H15B 0.63617 -0.01813 0.75710 1.00000 0.10384 0.00000 0.00000 C16 0.81917 0.49064 0.83347 1.00000 0.08509 0.09410 0.11776 0.00286 -0.01762 -0.04427 0.09898 0.01168 0.00113 0.00106 0.00031 0.00000 0.00440 0.00447 0.00478 0.00416 0.00394 0.00417 0.00235 H16A 0.75191 0.55331 0.80815 1.00000 0.11878 0.00000 0.00000 H16B 0.89718 0.56760 0.85180 1.00000 0.11878 0.00000 0.00000 C17 0.68632 0.41253 0.86964 1.00000 0.08232 0.06506 0.08303 -0.01076 0.00116 -0.02205 0.07681 0.00963 0.00095 0.00078 0.00023 0.00000 0.00348 0.00275 0.00298 0.00238 0.00264 0.00290 0.00153 H17A 0.75400 0.36234 0.89735 1.00000 0.09217 0.00000 0.00000 H17B 0.60824 0.49840 0.88378 1.00000 0.09217 0.00000 0.00000 C18 0.93477 0.36490 0.80789 1.00000 0.06226 0.11017 0.09056 0.03054 -0.00775 -0.02386 0.08766 0.01309 0.00089 0.00115 0.00026 0.00000 0.00274 0.00529 0.00369 0.00371 0.00262 0.00332 0.00210 Final Structure Factor Calculation for AN8809r in P2(1)2(1)2(1) Total number of l.s. parameters = 182 Maximum vector length = 511 Memory required = 2649 / 24024 wR2 = 0.4262 before cycle 11 for 2072 data and 2 / 182 parameters GooF = S = 2.266; Restrained GooF = 2.266 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0967 for 1957 Fo > 4sig(Fo) and 0.1015 for all 2072 data wR2 = 0.4262, GooF = S = 2.266, Restrained GooF = 2.266 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 20.00 for non-hydrogen and 24.00 for hydrogen atoms Principal mean square atomic displacements U 0.0631 0.0514 0.0362 C1 0.0685 0.0614 0.0429 C2 0.0556 0.0449 0.0398 C3 0.1675 0.0938 0.0493 O2 0.0581 0.0519 0.0383 C4 0.1276 0.0615 0.0375 C5 0.0897 0.0586 0.0505 C6 0.0604 0.0528 0.0463 C7 0.0725 0.0558 0.0438 C8 0.0925 0.0601 0.0407 C9 0.1907 0.1346 0.0579 O1 0.1061 0.0768 0.0461 C10 0.1091 0.0727 0.0454 C11 0.0997 0.0842 0.0488 C12 0.0779 0.0765 0.0541 C13 0.1013 0.0799 0.0501 C14 0.1565 0.0608 0.0423 C15 0.1424 0.1112 0.0434 C16 0.1004 0.0820 0.0480 C17 0.1399 0.0715 0.0516 C18 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.007 0.010 0.014 0.018 0.023 0.031 0.043 0.061 0.098 1.000 Number in group 238. 186. 222. 189. 219. 196. 207. 201. 208. 206. GooF 2.519 3.388 3.077 2.688 2.309 1.929 1.990 1.193 1.053 1.194 K 2.700 1.261 1.190 1.366 1.306 1.160 1.021 1.034 1.039 1.096 Resolution(A) 0.76 0.80 0.83 0.87 0.92 0.98 1.06 1.17 1.34 1.73 inf Number in group 211. 212. 204. 208. 204. 205. 207. 206. 207. 208. GooF 3.014 2.797 2.805 2.400 2.760 2.089 1.706 1.300 1.595 1.272 K 1.266 1.341 1.275 1.107 1.187 1.074 0.987 1.022 1.433 1.058 R1 0.250 0.238 0.202 0.175 0.183 0.122 0.095 0.061 0.102 0.061 Recommended weighting scheme: WGHT 0.2000 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)/su Fc/Fc(max) Resolution(A) 4 7 5 151.97 4.72 6.32 0.017 0.96 4 7 6 157.21 7.59 6.01 0.021 0.95 8 0 13 69.87 4.72 5.69 0.017 0.83 4 2 8 7850.78 614.95 5.52 0.191 1.48 7 1 11 84.50 8.20 5.24 0.022 0.95 7 1 2 78.82 8.01 5.17 0.022 1.03 7 1 18 82.65 9.23 5.03 0.023 0.84 3 7 3 235.93 30.29 4.77 0.042 1.03 0 6 25 84.50 12.39 4.57 0.027 0.83 4 7 9 3.17 0.40 4.47 0.005 0.92 9 3 2 4.37 0.61 4.47 0.006 0.77 6 4 21 4.80 0.93 3.92 0.007 0.80 1 2 33 1.31 0.08 3.90 0.002 0.78 0 2 32 3.49 0.69 3.78 0.006 0.81 5 4 24 6.33 1.36 3.74 0.009 0.80 3 6 25 5.79 1.25 3.73 0.009 0.78 1 9 7 1.86 0.30 3.66 0.004 0.86 4 8 11 2.84 0.57 3.64 0.006 0.83 2 5 22 4.37 0.98 3.59 0.008 0.93 4 4 23 2.51 0.53 3.48 0.006 0.87 1 4 28 1.53 0.24 3.44 0.004 0.85 7 1 14 0.00 26.14 3.42 0.039 0.91 8 5 8 3.49 0.85 3.36 0.007 0.77 3 5 20 2.84 0.67 3.36 0.006 0.94 2 9 5 7.97 2.07 3.35 0.011 0.86 2 6 26 5.24 1.34 3.34 0.009 0.79 3 2 28 6.33 1.66 3.31 0.010 0.86 0 4 27 2.18 0.49 3.31 0.005 0.88 4 5 13 1.31 28.08 3.23 0.041 1.04 4 4 15 1.31 27.33 3.22 0.040 1.07 8 5 6 28.39 8.02 3.16 0.022 0.78 7 6 3 3.49 0.95 3.14 0.007 0.82 7 3 8 1.86 30.81 3.14 0.043 0.93 0 6 26 2.18 0.54 3.13 0.006 0.81 7 3 15 4.37 1.25 3.07 0.009 0.85 2 8 0 1.31 18.34 3.06 0.033 0.97 4 4 14 3.17 39.88 3.05 0.049 1.10 1 4 15 5.79 69.36 3.04 0.064 1.30 5 4 6 2.18 25.17 3.03 0.039 1.14 5 0 14 3.49 41.44 3.03 0.049 1.15 4 8 8 1.53 0.33 3.02 0.004 0.85 5 6 12 3.17 0.90 3.01 0.007 0.90 0 3 14 7.42 74.83 2.96 0.066 1.54 7 2 6 2.84 27.83 2.96 0.041 0.98 3 7 6 2.18 22.88 2.95 0.037 1.01 9 2 7 0.00 1.31 2.94 0.009 0.78 1 5 25 1.53 0.36 2.92 0.005 0.88 4 6 10 3.49 0.89 2.91 0.007 1.00 4 2 30 2.51 0.73 2.88 0.007 0.78 2 4 29 30.68 9.77 2.87 0.024 0.81 Bond lengths and angles C1 - Distance Angles C4 1.5144 (0.0054) C5 1.5166 (0.0056) 111.92 (0.39) C3 1.5334 (0.0048) 108.13 (0.29) 110.51 (0.35) H1 0.9800 108.74 108.74 108.74 C1 - C4 C5 C3 C2 - Distance Angles C9 1.5302 (0.0061) C3 1.5420 (0.0055) 113.54 (0.34) H2A 0.9700 108.86 108.86 H2B 0.9700 108.86 108.86 107.71 C2 - C9 C3 H2A C3 - Distance Angles C8 1.5382 (0.0054) C1 1.5334 (0.0048) 113.80 (0.32) C2 1.5420 (0.0055) 112.03 (0.32) 111.18 (0.35) H3 0.9800 106.42 106.42 106.42 C3 - C8 C1 C2 O2 - Distance Angles C13 1.2057 (0.0071) O2 - C4 - Distance Angles C1 1.5144 (0.0054) C11 1.5286 (0.0062) 120.80 (0.37) C7 1.5362 (0.0054) 112.45 (0.32) 104.47 (0.37) H4 0.9800 106.04 106.04 106.04 C4 - C1 C11 C7 C5 - Distance Angles C15 1.5201 (0.0092) C1 1.5166 (0.0056) 110.75 (0.55) H5A 0.9700 109.49 109.49 H5B 0.9700 109.49 109.49 108.07 C5 - C15 C1 H5A C6 - Distance Angles C12 1.3459 (0.0077) C8 1.5000 (0.0070) 122.15 (0.55) C15 1.5136 (0.0079) 122.05 (0.59) 115.72 (0.46) C6 - C12 C8 C7 - Distance Angles C9 1.5094 (0.0061) C13 1.5272 (0.0066) 116.69 (0.37) C10 1.5397 (0.0064) 112.47 (0.46) 104.34 (0.41) C4 1.5362 (0.0054) 109.72 (0.37) 99.42 (0.35) 113.59 (0.36) C7 - C9 C13 C10 C8 - Distance Angles C6 1.5000 (0.0070) C3 1.5382 (0.0053) 109.58 (0.38) C17 1.5383 (0.0069) 113.04 (0.46) 110.74 (0.38) H8 0.9800 107.76 107.76 107.76 C8 - C6 C3 C17 C9 - Distance Angles C7 1.5094 (0.0061) C2 1.5302 (0.0061) 110.17 (0.34) H9A 0.9700 109.62 109.62 H9B 0.9700 109.62 109.62 108.14 C9 - C7 C2 H9A O1 - Distance Angles C18 1.2189 (0.0088) O1 - C10 - Distance Angles C7 1.5397 (0.0064) H10A 0.9600 109.47 H10B 0.9600 109.47 109.47 H10C 0.9600 109.47 109.47 109.47 C10 - C7 H10A H10B C11 - Distance Angles C4 1.5286 (0.0061) C14 1.5406 (0.0085) 102.79 (0.44) H11A 0.9700 111.21 111.21 H11B 0.9700 111.21 111.21 109.13 C11 - C4 C14 H11A C12 - Distance Angles C6 1.3459 (0.0077) C18 1.4463 (0.0105) 123.31 (0.65) H12 0.9300 118.34 118.34 C12 - C6 C18 C13 - Distance Angles O2 1.2057 (0.0071) C14 1.5133 (0.0081) 124.56 (0.59) C7 1.5272 (0.0066) 126.64 (0.58) 108.74 (0.39) C13 - O2 C14 C14 - Distance Angles C13 1.5133 (0.0081) C11 1.5406 (0.0085) 105.47 (0.44) H14A 0.9700 110.65 110.65 H14B 0.9700 110.65 110.65 108.77 C14 - C13 C11 H14A C15 - Distance Angles C5 1.5201 (0.0092) C6 1.5136 (0.0078) 110.83 (0.38) H15A 0.9700 109.48 109.48 H15B 0.9700 109.48 109.48 108.06 C15 - C5 C6 H15A C16 - Distance Angles C18 1.4798 (0.0126) C17 1.4980 (0.0092) 111.82 (0.61) H16A 0.9700 109.25 109.25 H16B 0.9700 109.25 109.25 107.93 C16 - C18 C17 H16A C17 - Distance Angles C8 1.5383 (0.0069) C16 1.4980 (0.0093) 112.91 (0.47) H17A 0.9700 109.00 109.00 H17B 0.9700 109.00 109.01 107.79 C17 - C8 C16 H17A C18 - Distance Angles O1 1.2189 (0.0088) C12 1.4463 (0.0105) 122.43 (0.99) C16 1.4798 (0.0126) 122.97 (0.94) 114.47 (0.54) C18 - O1 C12 FMAP and GRID set by program FMAP 2 3 31 GRID -0.893 -2 -2 0.893 2 2 R1 = 0.1015 for 2072 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.58 at 0.1165 0.2667 0.1801 [ 0.67 A from C6 ] Deepest hole -0.48 at 0.7488 0.2581 0.0643 [ 0.84 A from H2B ] Mean = 0.00, Rms deviation from mean = 0.14 e/A^3, Highest memory used = 2497 / 18355 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.6165 0.2333 0.8199 1.00000 0.05 0.58 0.67 C6 0.84 C8 1.43 H8 1.79 C12 Q2 1 0.8552 0.4429 0.8683 1.00000 0.05 0.54 1.03 C16 1.14 H16B 1.25 H17A 1.26 C17 Q3 1 0.5049 0.2093 0.8762 1.00000 0.05 0.53 0.48 C3 1.10 C8 1.25 H3 1.63 C2 Q4 1 0.3604 -0.0338 0.8808 1.00000 0.05 0.53 0.64 C1 0.87 C4 1.35 H1 1.47 H4 Q5 1 0.5222 -0.0461 0.8124 1.00000 0.05 0.48 0.42 C5 1.11 H5A 1.11 C15 1.22 H5B Q6 1 0.4970 0.5042 0.8122 1.00000 0.05 0.47 1.45 H8 1.90 H16A 2.06 H17B 2.06 C8 Q7 1 0.6214 -0.0150 0.8778 1.00000 0.05 0.45 1.17 H3 1.40 H5A 1.68 C3 1.81 C5 Q8 1 0.6361 0.4624 0.8495 1.00000 0.05 0.44 0.76 C17 0.97 H17B 1.42 C16 1.56 H16A Q9 1 0.7577 0.4967 0.9361 1.00000 0.05 0.44 1.49 H17A 1.76 H17B 1.87 O2 1.95 C17 Q10 1 -0.1159 0.0242 0.9978 1.00000 0.05 0.44 1.42 H10A 1.82 H14B 2.05 H2A 2.19 C10 Q11 1 0.6175 -0.2464 0.8116 1.00000 0.05 0.43 1.18 H5A 1.57 H5B 1.64 C5 1.89 H16A Q12 1 -0.1126 -0.0158 0.8693 1.00000 0.05 0.43 1.20 H10B 1.73 H10C 1.78 C10 2.34 H10A Q13 1 0.6300 0.2342 0.9383 1.00000 0.05 0.43 1.44 H3 1.47 H2A 1.75 H17A 1.84 C2 Q14 1 0.9849 -0.0096 0.8044 1.00000 0.05 0.41 1.76 H12 2.19 C12 2.41 H1 2.71 H10C Q15 1 0.0071 -0.2602 0.8691 1.00000 0.05 0.41 0.85 H11B 1.66 H16B 1.72 C11 2.02 H10B Q16 1 0.2578 0.2323 0.9998 1.00000 0.05 0.40 0.46 H9B 1.25 C9 1.68 H9A 2.14 C2 Q17 1 -0.2423 0.0198 0.9325 1.00000 0.05 0.39 1.55 H10A 1.59 H3 1.67 H10B 1.92 C10 Q18 1 0.1353 -0.2411 0.8118 1.00000 0.05 0.39 1.56 H11B 2.18 H5B 2.26 H12 2.27 C11 Q19 1 0.5185 0.4734 0.9360 1.00000 0.05 0.39 1.25 H2A 1.54 H17B 2.02 O2 2.10 C2 Q20 1 -0.0019 0.0147 0.9345 1.00000 0.05 0.38 0.39 C10 0.82 H10A 0.91 H10B 1.34 H10C Q21 1 0.6222 0.0423 0.9913 1.00000 0.05 0.38 1.56 H9A 1.88 H14B 2.32 H14A 2.36 H9B Q22 1 0.7577 0.2811 0.8827 1.00000 0.05 0.38 0.76 H17A 1.23 C17 1.73 C8 1.88 H3 Q23 1 0.8579 0.2171 0.8028 1.00000 0.05 0.38 0.39 C12 1.12 H12 1.32 C18 1.45 C6 Q24 1 0.3685 -0.2660 0.8050 1.00000 0.05 0.37 0.89 H5B 1.83 C5 2.13 H11A 2.21 H5A Q25 1 0.2451 -0.1979 1.0108 1.00000 0.05 0.37 0.91 O2 1.09 C13 2.05 C14 2.10 H14B Shortest distances between peaks (including symmetry equivalents) 6 8 1.45 2 22 1.53 2 8 1.68 1 3 1.70 18 24 1.72 9 19 1.75 17 20 1.75 5 11 1.75 7 17 1.77 13 22 1.78 15 18 1.78 1 23 1.82 11 24 1.83 17 21 1.85 12 14 1.85 10 20 1.87 3 13 1.89 5 7 1.89 13 16 1.90 4 7 1.91 12 20 1.92 8 22 1.92 10 21 1.92 3 22 1.94 12 17 1.94 7 12 1.95 10 17 1.95 13 17 1.97 2 9 1.97 1 22 1.99 3 7 1.99 10 19 2.00 1 8 2.01 14 23 2.05 16 21 2.08 6 24 2.08 13 21 2.08 13 19 2.09 5 24 2.10 9 25 2.14 12 15 2.15 4 5 2.16 10 16 2.17 14 18 2.17 6 11 2.19 3 4 2.22 9 22 2.23 22 23 2.29 9 13 2.31 1 6 2.36 3 8 2.36 1 5 2.36 8 19 2.44 8 9 2.46 17 22 2.48 9 16 2.50 2 23 2.51 1 7 2.52 8 11 2.55 7 11 2.55 7 13 2.56 12 23 2.58 7 22 2.58 12 22 2.59 2 15 2.63 14 15 2.65 3 19 2.65 3 5 2.66 16 17 2.68 19 22 2.72 4 24 2.74 1 2 2.74 15 20 2.81 3 17 2.82 19 25 2.82 10 25 2.82 8 23 2.83 3 6 2.91 21 25 2.91 16 19 2.94 10 13 2.96 4 18 2.96 12 18 2.97 8 13 2.98 2 13 2.99 17 25 2.99 Time profile in seconds ----------------------- 0.02: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: 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. 0.09: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.08: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.33: Structure factors and derivatives 0.92: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.20: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.00: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + an8809 finished at 14:56:37 Total CPU time: 2.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++