+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0113 started at 17:19:30 on 19-Feb-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0113 in P2(1)/c CELL 0.71073 15.8650 5.6205 16.4742 90.000 106.779 90.000 ZERR 4.00 0.0012 0.0004 0.0012 0.000 0.004 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O F UNIT 64 68 16 4 4 V = 1406.45 F(000) = 632.0 Mu = 0.10 mm-1 Cell Wt = 1201.34 Rho = 1.418 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 EQIV_$1 -x, y+1/2, -z+1/2 HTAB N3 O13_$1 EQIV_$2 x-1, y+1, z HTAB N3 F17_$2 EQIV_$3 -x, -y+1, -z HTAB N3 F17_$3 FMAP 2 PLAN 10 ACTA SIZE 0.43 0.05 0.01 BOND $H WGHT 0.00000 6.58780 L.S. 4 TEMP -153.00 FVAR 0.61579 MOLE 1 C2 1 -0.184336 1.127354 0.121621 11.00000 0.02547 0.01932 = 0.02915 -0.00433 0.00975 0.00373 AFIX 43 H2 2 -0.208892 1.264950 0.139473 11.00000 -1.20000 AFIX 0 C3 1 -0.240903 0.943489 0.085920 11.00000 0.02527 0.03172 = 0.01746 0.00420 0.00886 0.00366 C4 1 -0.203023 0.742856 0.062514 11.00000 0.02800 0.02885 = 0.01969 -0.00524 0.00654 -0.00282 AFIX 43 H4 2 -0.238719 0.610433 0.038411 11.00000 -1.20000 AFIX 0 C5 1 -0.112599 0.735250 0.074314 11.00000 0.02738 0.01536 = 0.02433 -0.00304 0.00814 0.00048 AFIX 43 H5 2 -0.086055 0.597444 0.058979 11.00000 -1.20000 AFIX 0 C6 1 -0.061521 0.932032 0.108864 11.00000 0.02176 0.02385 = 0.01893 0.00198 0.00803 0.00202 C8 1 0.071707 0.737373 0.095640 11.00000 0.02418 0.02406 = 0.02146 -0.00614 0.00491 0.00425 AFIX 23 H8A 2 0.036707 0.681260 0.038970 11.00000 -1.20000 H8B 2 0.073348 0.608117 0.136893 11.00000 -1.20000 AFIX 0 C9 1 0.165193 0.794373 0.093971 11.00000 0.02355 0.03101 = 0.02529 -0.00611 0.00901 0.00461 AFIX 23 H9A 2 0.193933 0.647444 0.082052 11.00000 -1.20000 H9B 2 0.163176 0.909835 0.048066 11.00000 -1.20000 AFIX 0 C11 1 0.174023 1.101528 0.200793 11.00000 0.02479 0.01630 = 0.02843 -0.00309 0.00916 0.00357 AFIX 23 H11A 2 0.172908 1.234417 0.161053 11.00000 -1.20000 H11B 2 0.208849 1.153111 0.258125 11.00000 -1.20000 AFIX 0 C12 1 0.081119 1.045611 0.201486 11.00000 0.02326 0.02079 = 0.02151 -0.00106 0.00716 0.00537 AFIX 23 H12A 2 0.082566 0.929024 0.246914 11.00000 -1.20000 H12B 2 0.052509 1.192433 0.213689 11.00000 -1.20000 AFIX 0 C13 1 0.294430 0.810837 0.222290 11.00000 0.02491 0.01860 = 0.02425 0.00555 0.01094 -0.00037 C14 1 0.343431 0.640218 0.182537 11.00000 0.01243 0.02462 = 0.02484 -0.00123 0.00625 -0.00554 C15 1 0.374478 0.426702 0.222790 11.00000 0.01942 0.02546 = 0.02505 0.00311 0.00808 0.00054 AFIX 43 H15 2 0.360660 0.384031 0.273272 11.00000 -1.20000 AFIX 0 C16 1 0.425574 0.275161 0.189770 11.00000 0.01926 0.02151 = 0.03364 -0.00212 0.00602 0.00001 AFIX 43 H16 2 0.446233 0.127962 0.216501 11.00000 -1.20000 AFIX 0 C17 1 0.445433 0.344676 0.117041 11.00000 0.01443 0.02873 = 0.03010 -0.00849 0.00425 0.00134 C18 1 0.417298 0.555042 0.075960 11.00000 0.02531 0.03334 = 0.02426 -0.00168 0.01221 -0.00189 AFIX 43 H18 2 0.432967 0.599008 0.026542 11.00000 -1.20000 AFIX 0 C19 1 0.364918 0.701735 0.109391 11.00000 0.02576 0.02905 = 0.02224 0.00443 0.00902 0.00043 AFIX 43 H19 2 0.343442 0.846959 0.081547 11.00000 -1.20000 AFIX 0 N1 3 -0.097325 1.124551 0.132723 11.00000 0.02373 0.02054 = 0.02977 0.00130 0.01382 0.00184 N3 3 -0.331907 0.965899 0.072194 11.00000 0.01915 0.03634 = 0.03375 -0.00566 0.00325 0.00418 AFIX 93 H3A 2 -0.353782 1.098216 0.086330 11.00000 -1.20000 H3B 2 -0.367191 0.847658 0.049438 11.00000 -1.20000 AFIX 0 N7 3 0.029669 0.947657 0.119283 11.00000 0.01990 0.02222 = 0.02274 -0.00340 0.00692 0.00147 N10 3 0.216522 0.894039 0.175146 11.00000 0.02176 0.02377 = 0.02546 -0.00217 0.00633 0.00328 O13 4 0.328792 0.879558 0.296335 11.00000 0.02339 0.03208 = 0.02353 -0.00118 0.00745 0.00066 F17 5 0.495358 0.197390 0.083441 11.00000 0.02605 0.03730 = 0.04303 -0.01266 0.01415 0.00379 HKLF 4 Covalent radii and connectivity table for 2009src0113 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 F 0.640 C2 - N1 C3 C3 - C2 C4 N3 C4 - C3 C5 C5 - C4 C6 C6 - N1 C5 N7 C8 - N7 C9 C9 - N10 C8 C11 - N10 C12 C12 - N7 C11 C13 - O13 N10 C14 C14 - C19 C15 C13 C15 - C16 C14 C16 - C17 C15 C17 - F17 C18 C16 C18 - C17 C19 C19 - C14 C18 N1 - C6 C2 N3 - C3 N7 - C6 C8 C12 N10 - C13 C9 C11 O13 - C13 F17 - C17 Operators for generating equivalent atoms: $1 -x, y+1/2, -z+1/2 $2 x-1, y+1, z $3 -x, -y+1, -z 16409 Reflections read, of which 1100 rejected -20 =< h =< 20, -7 =< k =< 6, -20 =< l =< 21, Max. 2-theta = 54.96 0 Systematic absence violations 0 Inconsistent equivalents 3206 Unique reflections, of which 0 suppressed R(int) = 0.1269 R(sigma) = 0.1232 Friedel opposites merged Maximum memory for data reduction = 2184 / 32423 Default effective X-H distances for T = -153.0 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 = 2749 / 247693 wR2 = 0.2138 before cycle 1 for 3206 data and 199 / 199 parameters GooF = S = 1.135; Restrained GooF = 1.135 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 6.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.61580 0.00201 0.003 OSF Mean shift/su = 0.002 Maximum = -0.007 for y C3 Max. shift = 0.000 A for C3 Max. dU = 0.000 for C17 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2749 / 247693 wR2 = 0.2138 before cycle 2 for 3206 data and 199 / 199 parameters GooF = S = 1.135; Restrained GooF = 1.135 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 6.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.61580 0.00201 0.002 OSF Mean shift/su = 0.001 Maximum = -0.003 for y C3 Max. shift = 0.000 A for C3 Max. dU = 0.000 for C17 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2749 / 247693 wR2 = 0.2139 before cycle 3 for 3206 data and 199 / 199 parameters GooF = S = 1.135; Restrained GooF = 1.135 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 6.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.61580 0.00201 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for U13 C18 Max. shift = 0.000 A for C13 Max. dU = 0.000 for C11 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2749 / 247693 wR2 = 0.2138 before cycle 4 for 3206 data and 199 / 199 parameters GooF = S = 1.135; Restrained GooF = 1.135 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 6.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.61580 0.00201 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H3A Max. dU = 0.000 for C19 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 -0.2089 1.2649 0.1395 43 0.950 0.000 C2 N1 C3 H4 -0.2387 0.6104 0.0384 43 0.950 0.000 C4 C3 C5 H5 -0.0861 0.5974 0.0590 43 0.950 0.000 C5 C4 C6 H8A 0.0367 0.6813 0.0390 23 0.990 0.000 C8 N7 C9 H8B 0.0733 0.6081 0.1369 23 0.990 0.000 C8 N7 C9 H9A 0.1939 0.6474 0.0821 23 0.990 0.000 C9 N10 C8 H9B 0.1632 0.9098 0.0481 23 0.990 0.000 C9 N10 C8 H11A 0.1729 1.2344 0.1611 23 0.990 0.000 C11 N10 C12 H11B 0.2088 1.1531 0.2581 23 0.990 0.000 C11 N10 C12 H12A 0.0826 0.9290 0.2469 23 0.990 0.000 C12 N7 C11 H12B 0.0525 1.1924 0.2137 23 0.990 0.000 C12 N7 C11 H15 0.3607 0.3840 0.2733 43 0.950 0.000 C15 C16 C14 H16 0.4462 0.1280 0.2165 43 0.950 0.000 C16 C17 C15 H18 0.4330 0.5990 0.0265 43 0.950 0.000 C18 C17 C19 H19 0.3434 0.8470 0.0815 43 0.950 0.000 C19 C14 C18 H3A -0.3538 1.0982 0.0863 93 0.880 0.000 N3 C3 C2 H3B -0.3672 0.8477 0.0494 93 0.880 0.000 N3 C3 C2 2009src0113 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C2 -0.18434 1.12735 0.12162 1.00000 0.02548 0.01932 0.02915 -0.00433 0.00977 0.00373 0.02425 0.00959 0.00031 0.00091 0.00031 0.00000 0.00264 0.00264 0.00274 0.00220 0.00221 0.00224 0.00111 H2 -0.20889 1.26495 0.13947 1.00000 0.02910 0.00000 0.00000 C3 -0.24090 0.94348 0.08592 1.00000 0.02527 0.03172 0.01747 0.00419 0.00885 0.00365 0.02425 0.01006 0.00032 0.00097 0.00029 0.00000 0.00259 0.00302 0.00247 0.00223 0.00209 0.00235 0.00114 C4 -0.20302 0.74285 0.06251 1.00000 0.02801 0.02885 0.01970 -0.00523 0.00655 -0.00283 0.02559 0.00987 0.00032 0.00096 0.00030 0.00000 0.00270 0.00297 0.00253 0.00220 0.00217 0.00235 0.00116 H4 -0.23872 0.61043 0.03841 1.00000 0.03071 0.00000 0.00000 C5 -0.11260 0.73525 0.07431 1.00000 0.02738 0.01537 0.02434 -0.00304 0.00814 0.00048 0.02222 0.00933 0.00032 0.00086 0.00030 0.00000 0.00260 0.00253 0.00260 0.00205 0.00214 0.00212 0.00108 H5 -0.08606 0.59744 0.05898 1.00000 0.02667 0.00000 0.00000 C6 -0.06152 0.93204 0.10886 1.00000 0.02176 0.02384 0.01893 0.00198 0.00804 0.00202 0.02106 0.00938 0.00030 0.00090 0.00029 0.00000 0.00246 0.00270 0.00248 0.00209 0.00205 0.00216 0.00107 C8 0.07171 0.73737 0.09564 1.00000 0.02418 0.02406 0.02147 -0.00614 0.00492 0.00426 0.02359 0.00957 0.00031 0.00090 0.00031 0.00000 0.00255 0.00281 0.00255 0.00215 0.00207 0.00223 0.00112 H8A 0.03671 0.68126 0.03897 1.00000 0.02831 0.00000 0.00000 H8B 0.07335 0.60812 0.13689 1.00000 0.02831 0.00000 0.00000 C9 0.16519 0.79437 0.09397 1.00000 0.02355 0.03101 0.02529 -0.00611 0.00902 0.00461 0.02620 0.00965 0.00031 0.00100 0.00031 0.00000 0.00253 0.00301 0.00267 0.00231 0.00217 0.00233 0.00117 H9A 0.19393 0.64745 0.08205 1.00000 0.03145 0.00000 0.00000 H9B 0.16318 0.90983 0.04807 1.00000 0.03145 0.00000 0.00000 C11 0.17402 1.10153 0.20079 1.00000 0.02479 0.01630 0.02844 -0.00309 0.00916 0.00357 0.02287 0.00966 0.00031 0.00086 0.00032 0.00000 0.00251 0.00251 0.00271 0.00214 0.00212 0.00217 0.00108 H11A 0.17291 1.23442 0.16105 1.00000 0.02744 0.00000 0.00000 H11B 0.20885 1.15311 0.25812 1.00000 0.02744 0.00000 0.00000 C12 0.08112 1.04562 0.20149 1.00000 0.02326 0.02078 0.02152 -0.00106 0.00717 0.00536 0.02170 0.00923 0.00030 0.00089 0.00030 0.00000 0.00247 0.00263 0.00248 0.00212 0.00205 0.00218 0.00107 H12A 0.08257 0.92903 0.24692 1.00000 0.02605 0.00000 0.00000 H12B 0.05251 1.19244 0.21369 1.00000 0.02605 0.00000 0.00000 C13 0.29443 0.81083 0.22229 1.00000 0.02490 0.01860 0.02426 0.00555 0.01093 -0.00037 0.02178 0.00978 0.00031 0.00087 0.00030 0.00000 0.00259 0.00259 0.00266 0.00214 0.00218 0.00215 0.00108 C14 0.34343 0.64021 0.18254 1.00000 0.01244 0.02462 0.02484 -0.00123 0.00625 -0.00553 0.02045 0.00901 0.00029 0.00089 0.00030 0.00000 0.00216 0.00269 0.00254 0.00214 0.00193 0.00205 0.00105 C15 0.37448 0.42671 0.22279 1.00000 0.01942 0.02546 0.02505 0.00312 0.00809 0.00053 0.02296 0.00941 0.00030 0.00091 0.00030 0.00000 0.00244 0.00284 0.00265 0.00220 0.00210 0.00217 0.00111 H15 0.36066 0.38404 0.27327 1.00000 0.02755 0.00000 0.00000 C16 0.42557 0.27517 0.18977 1.00000 0.01926 0.02151 0.03363 -0.00213 0.00602 0.00002 0.02514 0.00946 0.00030 0.00093 0.00031 0.00000 0.00248 0.00273 0.00298 0.00228 0.00222 0.00216 0.00115 H16 0.44623 0.12797 0.21650 1.00000 0.03016 0.00000 0.00000 C17 0.44543 0.34467 0.11704 1.00000 0.01444 0.02874 0.03011 -0.00850 0.00426 0.00135 0.02489 0.00933 0.00030 0.00094 0.00032 0.00000 0.00229 0.00294 0.00281 0.00232 0.00210 0.00218 0.00115 C18 0.41730 0.55504 0.07596 1.00000 0.02532 0.03335 0.02427 -0.00168 0.01221 -0.00190 0.02658 0.00981 0.00032 0.00096 0.00031 0.00000 0.00264 0.00310 0.00266 0.00235 0.00221 0.00240 0.00118 H18 0.43297 0.59901 0.02655 1.00000 0.03190 0.00000 0.00000 C19 0.36492 0.70173 0.10939 1.00000 0.02576 0.02904 0.02226 0.00443 0.00901 0.00043 0.02525 0.00985 0.00031 0.00097 0.00030 0.00000 0.00264 0.00292 0.00260 0.00227 0.00217 0.00233 0.00115 H19 0.34344 0.84696 0.08155 1.00000 0.03030 0.00000 0.00000 N1 -0.09733 1.12455 0.13272 1.00000 0.02372 0.02054 0.02979 0.00130 0.01381 0.00183 0.02340 0.00803 0.00025 0.00074 0.00025 0.00000 0.00219 0.00229 0.00232 0.00185 0.00186 0.00187 0.00095 N3 -0.33191 0.96590 0.07219 1.00000 0.01914 0.03632 0.03376 -0.00567 0.00325 0.00416 0.03066 0.00841 0.00026 0.00086 0.00026 0.00000 0.00218 0.00279 0.00256 0.00213 0.00191 0.00201 0.00109 H3A -0.35378 1.09822 0.08633 1.00000 0.03680 0.00000 0.00000 H3B -0.36719 0.84766 0.04944 1.00000 0.03680 0.00000 0.00000 N7 0.02967 0.94766 0.11928 1.00000 0.01991 0.02223 0.02274 -0.00340 0.00693 0.00147 0.02147 0.00767 0.00025 0.00073 0.00025 0.00000 0.00201 0.00227 0.00211 0.00181 0.00171 0.00181 0.00091 N10 0.21652 0.89404 0.17514 1.00000 0.02176 0.02377 0.02546 -0.00216 0.00633 0.00327 0.02376 0.00792 0.00025 0.00076 0.00025 0.00000 0.00210 0.00233 0.00222 0.00186 0.00177 0.00186 0.00094 O13 0.32879 0.87956 0.29634 1.00000 0.02339 0.03208 0.02354 -0.00119 0.00746 0.00065 0.02619 0.00662 0.00021 0.00064 0.00021 0.00000 0.00177 0.00210 0.00189 0.00161 0.00148 0.00164 0.00082 F17 0.49536 0.19739 0.08344 1.00000 0.02605 0.03731 0.04304 -0.01265 0.01415 0.00380 0.03459 0.00581 0.00018 0.00057 0.00019 0.00000 0.00159 0.00188 0.00186 0.00154 0.00141 0.00144 0.00079 Final Structure Factor Calculation for 2009src0113 in P2(1)/c Total number of l.s. parameters = 199 Maximum vector length = 511 Memory required = 2550 / 24017 wR2 = 0.2139 before cycle 5 for 3206 data and 0 / 199 parameters GooF = S = 1.135; Restrained GooF = 1.135 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 6.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1116 for 1796 Fo > 4sig(Fo) and 0.1999 for all 3206 data wR2 = 0.2139, GooF = S = 1.135, Restrained GooF = 1.135 for all data Occupancy sum of asymmetric unit = 22.00 for non-hydrogen and 17.00 for hydrogen atoms Principal mean square atomic displacements U 0.0308 0.0272 0.0147 C2 0.0341 0.0236 0.0150 C3 0.0319 0.0275 0.0173 C4 0.0274 0.0251 0.0142 C5 0.0257 0.0207 0.0168 C6 0.0334 0.0221 0.0153 C8 0.0366 0.0258 0.0162 C9 0.0292 0.0260 0.0134 C11 0.0278 0.0219 0.0154 C12 0.0288 0.0231 0.0134 C13 0.0269 0.0246 0.0098 C14 0.0284 0.0223 0.0181 C15 0.0350 0.0211 0.0192 C16 0.0395 0.0209 0.0142 C17 0.0343 0.0278 0.0177 C18 0.0313 0.0258 0.0187 C19 0.0325 0.0205 0.0172 N1 0.0444 0.0294 0.0182 N3 0.0262 0.0212 0.0170 N7 0.0288 0.0238 0.0187 N10 0.0323 0.0240 0.0223 O13 0.0536 0.0326 0.0177 F17 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.016 0.024 0.034 0.044 0.056 0.072 0.098 0.143 1.000 Number in group 326. 336. 318. 320. 309. 325. 316. 324. 312. 320. GooF 1.209 1.144 1.215 1.201 1.258 1.216 1.091 1.037 0.968 0.963 K 26.492 3.927 2.143 1.659 1.289 1.070 1.044 0.996 0.989 1.008 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.66 inf Number in group 329. 321. 316. 321. 318. 317. 323. 320. 319. 322. GooF 1.223 1.193 1.226 1.229 1.150 1.158 1.079 1.004 1.016 1.042 K 1.347 1.286 1.246 1.141 1.049 1.040 1.010 1.018 1.023 1.002 R1 0.455 0.448 0.398 0.323 0.245 0.167 0.131 0.105 0.098 0.048 Recommended weighting scheme: WGHT 0.0000 6.5757 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) -19 2 4 270.72 26.20 4.59 0.032 0.80 -1 1 20 243.51 0.23 4.13 0.003 0.79 0 4 4 76.38 0.04 3.68 0.001 1.32 -1 3 12 101.33 8.69 3.42 0.018 1.09 -10 5 4 161.63 8.04 3.29 0.018 0.92 5 5 11 234.65 68.20 3.19 0.051 0.81 -11 4 5 87.73 219.32 3.18 0.092 1.00 15 2 5 190.86 28.35 3.15 0.033 0.85 -6 3 17 111.55 7.99 3.07 0.018 0.86 -5 1 18 89.54 0.51 3.07 0.004 0.90 -16 1 14 120.80 4.90 3.07 0.014 0.85 -9 0 18 215.71 15.08 3.03 0.024 0.89 -6 0 18 186.77 42.61 2.98 0.040 0.91 -4 0 10 125.04 274.45 2.97 0.103 1.63 9 2 4 150.81 41.05 2.93 0.040 1.26 -13 3 14 145.38 5.71 2.93 0.015 0.86 2 3 12 127.38 6.68 2.92 0.016 1.03 -6 6 3 92.80 0.74 2.89 0.005 0.88 3 5 10 93.18 0.09 2.88 0.002 0.88 -11 5 1 137.84 0.11 2.87 0.002 0.88 -14 4 2 103.37 0.01 2.85 0.001 0.88 -1 4 12 217.98 84.17 2.83 0.057 0.97 17 1 6 236.60 56.68 2.80 0.047 0.77 14 4 2 -21.90 70.40 2.76 0.052 0.83 0 0 10 6073.54 5166.98 2.74 0.446 1.58 -13 4 13 -60.14 71.61 2.73 0.053 0.81 8 5 5 105.45 3.42 2.73 0.011 0.89 7 1 13 167.00 31.92 2.72 0.035 0.94 12 1 9 -21.31 64.30 2.72 0.050 0.90 -14 3 3 -8.29 55.69 2.70 0.046 0.97 5 0 10 131.32 48.92 2.68 0.043 1.26 -16 2 7 127.61 5.03 2.67 0.014 0.93 6 6 7 139.47 16.48 2.66 0.025 0.79 -3 5 14 222.12 0.47 2.65 0.004 0.81 -6 3 3 58.04 4.22 2.62 0.013 1.52 1 2 15 39.96 152.20 2.60 0.077 0.97 1 3 12 74.26 8.34 2.59 0.018 1.06 -12 4 15 285.51 70.95 2.59 0.052 0.79 3 3 12 161.55 43.39 2.58 0.041 1.01 -7 2 15 114.41 32.67 2.58 0.035 1.00 8 0 16 926.93 497.70 2.57 0.138 0.79 3 5 0 72.91 6.56 2.57 0.016 1.10 1 7 3 184.12 20.95 2.55 0.028 0.79 -18 3 8 210.09 4.14 2.54 0.013 0.79 -10 2 6 137.34 38.48 2.52 0.038 1.34 4 3 1 -1.16 48.77 2.51 0.043 1.65 -4 5 10 0.23 97.65 2.50 0.061 0.93 -17 1 2 94.36 21.44 2.49 0.029 0.91 -3 1 16 72.60 10.12 2.49 0.020 1.01 11 3 5 115.72 32.78 2.49 0.036 0.98 Bond lengths and angles C2 - Distance Angles N1 1.3392 (0.0060) C3 1.3837 (0.0070) 124.46 (0.46) H2 0.9500 117.77 117.77 C2 - N1 C3 C3 - Distance Angles C2 1.3837 (0.0070) C4 1.3839 (0.0071) 116.52 (0.44) N3 1.4011 (0.0062) 120.87 (0.48) 122.58 (0.50) C3 - C2 C4 C4 - Distance Angles C3 1.3839 (0.0071) C5 1.3916 (0.0068) 119.95 (0.49) H4 0.9500 120.03 120.03 C4 - C3 C5 C5 - Distance Angles C4 1.3916 (0.0068) C6 1.3920 (0.0067) 119.19 (0.45) H5 0.9500 120.41 120.41 C5 - C4 C6 C6 - Distance Angles N1 1.3330 (0.0062) C5 1.3920 (0.0067) 121.21 (0.42) N7 1.4096 (0.0059) 115.04 (0.43) 123.72 (0.44) C6 - N1 C5 C8 - Distance Angles N7 1.4640 (0.0060) C9 1.5254 (0.0064) 110.81 (0.41) H8A 0.9900 109.48 109.48 H8B 0.9900 109.48 109.48 108.06 C8 - N7 C9 H8A C9 - Distance Angles N10 1.4617 (0.0062) C8 1.5254 (0.0064) 110.60 (0.38) H9A 0.9900 109.53 109.53 H9B 0.9900 109.53 109.53 108.09 C9 - N10 C8 H9A C11 - Distance Angles N10 1.4689 (0.0059) C12 1.5103 (0.0064) 111.53 (0.40) H11A 0.9900 109.32 109.32 H11B 0.9900 109.32 109.32 107.97 C11 - N10 C12 H11A C12 - Distance Angles N7 1.4714 (0.0060) C11 1.5103 (0.0064) 110.74 (0.38) H12A 0.9900 109.50 109.50 H12B 0.9900 109.50 109.50 108.07 C12 - N7 C11 H12A C13 - Distance Angles O13 1.2452 (0.0057) N10 1.3400 (0.0061) 121.96 (0.44) C14 1.4989 (0.0067) 119.40 (0.43) 118.55 (0.43) C13 - O13 N10 C14 - Distance Angles C19 1.3875 (0.0064) C15 1.3906 (0.0068) 119.16 (0.45) C13 1.4989 (0.0067) 120.56 (0.45) 120.05 (0.42) C14 - C19 C15 C15 - Distance Angles C16 1.3904 (0.0067) C14 1.3906 (0.0068) 120.55 (0.45) H15 0.9500 119.72 119.72 C15 - C16 C14 C16 - Distance Angles C17 1.3803 (0.0069) C15 1.3904 (0.0067) 118.11 (0.48) H16 0.9500 120.94 120.94 C16 - C17 C15 C17 - Distance Angles F17 1.3683 (0.0054) C18 1.3714 (0.0073) 117.77 (0.45) C16 1.3803 (0.0068) 118.93 (0.46) 123.30 (0.46) C17 - F17 C18 C18 - Distance Angles C17 1.3714 (0.0073) C19 1.3921 (0.0069) 117.50 (0.45) H18 0.9500 121.25 121.25 C18 - C17 C19 C19 - Distance Angles C14 1.3875 (0.0064) C18 1.3921 (0.0069) 121.36 (0.49) H19 0.9500 119.32 119.32 C19 - C14 C18 N1 - Distance Angles C6 1.3330 (0.0062) C2 1.3392 (0.0060) 118.65 (0.44) N1 - C6 N3 - Distance Angles C3 1.4011 (0.0062) H3A 0.8800 120.00 H3B 0.8800 120.00 120.00 N3 - C3 H3A N7 - Distance Angles C6 1.4096 (0.0059) C8 1.4640 (0.0060) 116.60 (0.40) C12 1.4714 (0.0060) 114.37 (0.37) 111.88 (0.37) N7 - C6 C8 N10 - Distance Angles C13 1.3400 (0.0061) C9 1.4617 (0.0062) 125.00 (0.42) C11 1.4689 (0.0059) 122.25 (0.42) 112.75 (0.39) N10 - C13 C9 O13 - Distance Angles C13 1.2452 (0.0057) O13 - F17 - Distance Angles C17 1.3683 (0.0054) F17 - Specified hydrogen bonds (with su's except fixed and riding H) D-H H...A D...A <(DHA) 0.88 2.44 3.168(6) 140.5 N3-H3A...O13_$1 0.88 2.44 3.087(5) 130.3 N3-H3A...F17_$2 0.88 2.53 3.210(5) 134.2 N3-H3B...F17_$3 FMAP and GRID set by program FMAP 2 2 29 GRID -3.846 -1 -1 3.846 1 1 R1 = 0.1999 for 3206 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.40 at 0.2155 0.8768 0.3508 [ 0.66 A from H2 ] Deepest hole -0.37 at 0.2817 0.6646 0.3548 [ 1.31 A from H2 ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 3100 / 46476 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.2155 1.3768 0.1492 1.00000 0.05 0.40 0.66 H2 1.60 C2 2.16 H11B 2.19 H4 Q2 1 -0.0758 1.3018 0.1153 1.00000 0.05 0.33 1.12 N1 1.89 H5 2.01 C2 2.10 C6 Q3 1 -0.1529 0.7352 0.0972 1.00000 0.05 0.33 0.83 C5 0.84 C4 1.58 H5 1.59 H4 Q4 1 -0.1171 0.5456 0.0623 1.00000 0.05 0.32 0.59 H5 1.08 C5 1.76 C4 1.89 H4 Q5 1 0.4721 0.7336 0.1007 1.00000 0.05 0.32 1.31 C18 1.42 H18 1.76 C19 2.07 H19 Q6 1 -0.3461 0.8141 0.0996 1.00000 0.05 0.32 0.82 H3B 1.02 N3 1.61 H3A 1.89 C3 Q7 1 0.4839 0.3871 0.1713 1.00000 0.05 0.32 0.96 C17 1.23 C16 1.81 H16 1.85 F17 Q8 1 0.5115 0.1831 0.2641 1.00000 0.05 0.31 1.15 H16 1.63 C16 2.23 C14 2.27 C15 Q9 1 0.0185 1.3242 0.1338 1.00000 0.05 0.31 1.47 H12B 1.81 H8B 2.01 C12 2.14 N7 Q10 1 -0.2803 0.9103 0.1017 1.00000 0.05 0.31 0.77 C3 0.88 N3 1.44 H3B 1.54 H3A Shortest distances between peaks (including symmetry equivalents) 6 10 1.17 3 4 1.41 2 9 1.44 2 4 1.65 7 8 1.86 7 8 1.96 5 8 2.19 5 7 2.25 3 10 2.27 4 9 2.47 1 2 2.47 1 3 2.50 1 4 2.58 2 3 2.70 1 10 2.84 8 8 2.85 5 6 2.92 Time profile in seconds ----------------------- 0.03: 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. 0.75: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.70: Structure factors and derivatives 0.84: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.13: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.09: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.03: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0113 finished at 17:19:33 Total CPU time: 2.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++