+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008src1283 started at 14:52:24 on 13-Jan-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src1283 in P2(1) CELL 0.71073 8.2919 5.9109 12.4020 90.000 96.272 90.000 ZERR 2.00 0.0003 0.0002 0.0005 0.000 0.002 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N O UNIT 28 30 6 4 V = 604.22 F(000) = 272.0 Mu = 0.10 mm-1 Cell Wt = 514.58 Rho = 1.414 MERG 4 OMIT -3.00 55.00 EXTI 0.07342 SHEL 7 0.77 FMAP 2 PLAN 10 SIZE 0.11 0.18 0.46 ACTA BOND $H WGHT 0.04200 0.13810 L.S. 4 TEMP -153.00 FVAR 1.54571 MOLE 1 C2 1 0.719009 0.601982 1.232528 11.00000 0.02844 0.02335 = 0.02023 -0.00320 0.00226 0.00107 AFIX 43 H2 2 0.745882 0.739147 1.270197 11.00000 -1.20000 AFIX 0 C3 1 0.637156 0.439134 1.284553 11.00000 0.02222 0.02913 = 0.02039 -0.00067 0.00371 0.00257 AFIX 43 H3 2 0.607298 0.463129 1.355469 11.00000 -1.20000 AFIX 0 C4 1 0.600110 0.238450 1.229015 11.00000 0.02146 0.02871 = 0.02561 0.00514 0.00384 -0.00161 AFIX 43 H4 2 0.544364 0.121312 1.262068 11.00000 -1.20000 AFIX 0 C5 1 0.644551 0.209106 1.125238 11.00000 0.02121 0.02160 = 0.02499 -0.00149 0.00467 -0.00251 AFIX 43 H5 2 0.619535 0.072784 1.086400 11.00000 -1.20000 AFIX 0 C6 1 0.727473 0.385661 1.078785 11.00000 0.01341 0.01693 = 0.01922 0.00239 0.00097 0.00113 C8 1 0.695052 0.210924 0.897442 11.00000 0.02022 0.01688 = 0.02392 -0.00267 0.00346 -0.00519 AFIX 23 H8A 2 0.589880 0.280347 0.869965 11.00000 -1.20000 H8B 2 0.672467 0.066518 0.933342 11.00000 -1.20000 AFIX 0 C9 1 0.792531 0.164061 0.802861 11.00000 0.02332 0.01749 = 0.02444 -0.00194 0.00336 -0.00231 AFIX 23 H9A 2 0.890322 0.075048 0.828674 11.00000 -1.20000 H9B 2 0.726246 0.073330 0.747408 11.00000 -1.20000 AFIX 0 C11 1 0.939047 0.515054 0.834772 11.00000 0.01805 0.02084 = 0.01742 0.00116 -0.00031 -0.00265 AFIX 23 H11A 2 0.970977 0.657158 0.800569 11.00000 -1.20000 H11B 2 1.039124 0.432517 0.862109 11.00000 -1.20000 AFIX 0 C12 1 0.842329 0.569762 0.928531 11.00000 0.02057 0.01569 = 0.02044 -0.00095 0.00239 -0.00426 AFIX 23 H12A 2 0.911565 0.655265 0.984522 11.00000 -1.20000 H12B 2 0.748797 0.666612 0.902270 11.00000 -1.20000 AFIX 0 C13 1 0.746258 0.456196 0.665953 11.00000 0.01729 0.02096 = 0.01810 -0.00542 0.00253 0.00150 C14 1 0.790742 0.667209 0.612610 11.00000 0.01672 0.02395 = 0.01611 -0.00356 0.00085 0.00047 C15 1 0.699064 0.790015 0.535974 11.00000 0.02328 0.02543 = 0.01918 -0.00341 0.00000 0.00558 AFIX 43 H15 2 0.589209 0.762169 0.508945 11.00000 -1.20000 AFIX 0 C16 1 0.798830 0.967755 0.504069 11.00000 0.03225 0.02590 = 0.01758 0.00298 0.00333 0.00545 AFIX 43 H16 2 0.768819 1.082474 0.452074 11.00000 -1.20000 AFIX 0 C17 1 0.944966 0.941127 0.562432 11.00000 0.03089 0.02331 = 0.01918 0.00439 0.00398 -0.00114 AFIX 43 H17 2 1.035976 1.036529 0.557170 11.00000 -1.20000 AFIX 0 N1 3 0.763482 0.579505 1.131683 11.00000 0.02359 0.01961 = 0.01966 -0.00136 0.00231 -0.00029 N7 3 0.783454 0.363409 0.976826 11.00000 0.01828 0.01738 = 0.01694 -0.00240 0.00215 -0.00257 N10 3 0.841549 0.375881 0.753975 11.00000 0.02056 0.01748 = 0.01814 -0.00034 0.00020 -0.00251 O18 4 0.944388 0.758233 0.630197 11.00000 0.01901 0.02382 = 0.01977 0.00195 -0.00012 -0.00201 O19 4 0.622808 0.356547 0.626449 11.00000 0.02023 0.02692 = 0.02879 -0.00487 -0.00263 -0.00360 HKLF 4 Covalent radii and connectivity table for 2008src1283 in P2(1) C 0.770 H 0.320 N 0.700 O 0.660 C2 - N1 C3 C3 - C2 C4 C4 - C5 C3 C5 - C4 C6 C6 - N1 N7 C5 C8 - N7 C9 C9 - N10 C8 C11 - N10 C12 C12 - N7 C11 C13 - O19 N10 C14 C14 - C15 O18 C13 C15 - C14 C16 C16 - C17 C15 C17 - C16 O18 N1 - C6 C2 N7 - C6 C12 C8 N10 - C13 C9 C11 O18 - C17 C14 O19 - C13 Floating origin restraints generated 8662 Reflections read, of which 17 rejected -10 =< h =< 10, -7 =< k =< 7, -16 =< l =< 14, Max. 2-theta = 54.95 0 Systematic absence violations 0 Inconsistent equivalents 1522 Unique reflections, of which 0 suppressed R(int) = 0.0512 R(sigma) = 0.0373 Friedel opposites merged Maximum memory for data reduction = 1812 / 14875 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 = 2303 / 215198 wR2 = 0.0868 before cycle 1 for 1522 data and 173 / 173 parameters GooF = S = 1.048; Restrained GooF = 1.048 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0420 * P )^2 + 0.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.54571 0.00443 0.000 OSF 2 0.07342 0.00802 0.000 EXTI Mean shift/su = 0.002 Maximum = -0.005 for U23 O18 Max. shift = 0.000 A for N10 Max. dU = 0.000 for N7 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2303 / 215198 wR2 = 0.0868 before cycle 2 for 1522 data and 173 / 173 parameters GooF = S = 1.048; Restrained GooF = 1.048 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0420 * P )^2 + 0.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.54571 0.00443 0.000 OSF 2 0.07342 0.00802 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.002 for U22 O19 Max. shift = 0.000 A for C4 Max. dU = 0.000 for C2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2303 / 215198 wR2 = 0.0868 before cycle 3 for 1522 data and 173 / 173 parameters GooF = S = 1.048; Restrained GooF = 1.048 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0420 * P )^2 + 0.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.54571 0.00443 0.000 OSF 2 0.07342 0.00802 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.000 for z N1 Max. shift = 0.000 A for C15 Max. dU = 0.000 for C16 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2303 / 215198 wR2 = 0.0868 before cycle 4 for 1522 data and 173 / 173 parameters GooF = S = 1.048; Restrained GooF = 1.048 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0420 * P )^2 + 0.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.54571 0.00443 0.000 OSF 2 0.07342 0.00802 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.000 for z C4 Max. shift = 0.000 A for C11 Max. dU = 0.000 for C17 Largest correlation matrix elements 0.554 EXTI / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.7459 0.7391 1.2702 43 0.950 0.000 C2 N1 C3 H3 0.6073 0.4631 1.3555 43 0.950 0.000 C3 C2 C4 H4 0.5444 0.1213 1.2621 43 0.950 0.000 C4 C5 C3 H5 0.6195 0.0728 1.0864 43 0.950 0.000 C5 C4 C6 H8A 0.5899 0.2803 0.8700 23 0.990 0.000 C8 N7 C9 H8B 0.6725 0.0665 0.9333 23 0.990 0.000 C8 N7 C9 H9A 0.8903 0.0750 0.8287 23 0.990 0.000 C9 N10 C8 H9B 0.7262 0.0733 0.7474 23 0.990 0.000 C9 N10 C8 H11A 0.9710 0.6572 0.8006 23 0.990 0.000 C11 N10 C12 H11B 1.0391 0.4325 0.8621 23 0.990 0.000 C11 N10 C12 H12A 0.9116 0.6553 0.9845 23 0.990 0.000 C12 N7 C11 H12B 0.7488 0.6666 0.9023 23 0.990 0.000 C12 N7 C11 H15 0.5892 0.7622 0.5089 43 0.950 0.000 C15 C14 C16 H16 0.7688 1.0825 0.4521 43 0.950 0.000 C16 C17 C15 H17 1.0360 1.0365 0.5572 43 0.950 0.000 C17 C16 O18 2008src1283 in P2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C2 0.71901 0.60198 1.23253 1.00000 0.02844 0.02335 0.02023 -0.00320 0.00226 0.00107 0.02404 0.00421 0.00027 0.00041 0.00018 0.00000 0.00116 0.00119 0.00115 0.00096 0.00090 0.00097 0.00051 H2 0.74588 0.73915 1.27020 1.00000 0.02885 0.00000 0.00000 C3 0.63716 0.43913 1.28455 1.00000 0.02222 0.02913 0.02039 -0.00067 0.00371 0.00257 0.02381 0.00419 0.00026 0.00043 0.00019 0.00000 0.00101 0.00125 0.00112 0.00103 0.00084 0.00101 0.00049 H3 0.60730 0.46313 1.35547 1.00000 0.02857 0.00000 0.00000 C4 0.60011 0.23845 1.22902 1.00000 0.02146 0.02871 0.02561 0.00514 0.00384 -0.00161 0.02517 0.00422 0.00026 0.00042 0.00019 0.00000 0.00103 0.00133 0.00115 0.00107 0.00085 0.00100 0.00052 H4 0.54436 0.12131 1.26207 1.00000 0.03020 0.00000 0.00000 C5 0.64455 0.20911 1.12524 1.00000 0.02121 0.02160 0.02499 -0.00149 0.00467 -0.00251 0.02244 0.00405 0.00025 0.00040 0.00018 0.00000 0.00100 0.00117 0.00115 0.00098 0.00082 0.00091 0.00048 H5 0.61954 0.07278 1.08640 1.00000 0.02693 0.00000 0.00000 C6 0.72747 0.38566 1.07878 1.00000 0.01341 0.01693 0.01922 0.00239 0.00097 0.00113 0.01658 0.00377 0.00023 0.00038 0.00017 0.00000 0.00085 0.00103 0.00104 0.00088 0.00074 0.00080 0.00044 C8 0.69505 0.21092 0.89744 1.00000 0.02022 0.01688 0.02392 -0.00266 0.00346 -0.00519 0.02026 0.00372 0.00024 0.00038 0.00018 0.00000 0.00096 0.00106 0.00110 0.00091 0.00081 0.00085 0.00046 H8A 0.58988 0.28035 0.86996 1.00000 0.02431 0.00000 0.00000 H8B 0.67247 0.06652 0.93334 1.00000 0.02431 0.00000 0.00000 C9 0.79253 0.16406 0.80286 1.00000 0.02332 0.01749 0.02444 -0.00194 0.00336 -0.00231 0.02169 0.00406 0.00026 0.00040 0.00018 0.00000 0.00105 0.00105 0.00118 0.00093 0.00087 0.00092 0.00048 H9A 0.89032 0.07505 0.82867 1.00000 0.02603 0.00000 0.00000 H9B 0.72625 0.07333 0.74741 1.00000 0.02603 0.00000 0.00000 C11 0.93905 0.51505 0.83477 1.00000 0.01805 0.02084 0.01741 0.00116 -0.00031 -0.00265 0.01894 0.00365 0.00024 0.00038 0.00017 0.00000 0.00096 0.00111 0.00105 0.00089 0.00081 0.00085 0.00047 H11A 0.97098 0.65716 0.80057 1.00000 0.02272 0.00000 0.00000 H11B 1.03912 0.43252 0.86211 1.00000 0.02272 0.00000 0.00000 C12 0.84233 0.56976 0.92853 1.00000 0.02057 0.01569 0.02044 -0.00095 0.00239 -0.00426 0.01889 0.00386 0.00026 0.00038 0.00017 0.00000 0.00101 0.00102 0.00110 0.00089 0.00082 0.00086 0.00045 H12A 0.91157 0.65526 0.98452 1.00000 0.02266 0.00000 0.00000 H12B 0.74880 0.66661 0.90227 1.00000 0.02266 0.00000 0.00000 C13 0.74626 0.45620 0.66595 1.00000 0.01729 0.02096 0.01810 -0.00542 0.00253 0.00150 0.01874 0.00381 0.00024 0.00040 0.00017 0.00000 0.00094 0.00105 0.00104 0.00092 0.00078 0.00088 0.00045 C14 0.79074 0.66721 0.61261 1.00000 0.01672 0.02395 0.01611 -0.00356 0.00085 0.00047 0.01900 0.00371 0.00024 0.00040 0.00017 0.00000 0.00091 0.00112 0.00101 0.00092 0.00077 0.00088 0.00045 C15 0.69906 0.79001 0.53597 1.00000 0.02328 0.02543 0.01918 -0.00341 0.00000 0.00558 0.02280 0.00413 0.00027 0.00042 0.00018 0.00000 0.00105 0.00116 0.00105 0.00099 0.00085 0.00093 0.00049 H15 0.58921 0.76217 0.50894 1.00000 0.02736 0.00000 0.00000 C16 0.79883 0.96775 0.50407 1.00000 0.03225 0.02590 0.01758 0.00298 0.00333 0.00545 0.02520 0.00431 0.00028 0.00044 0.00018 0.00000 0.00116 0.00123 0.00108 0.00101 0.00089 0.00104 0.00051 H16 0.76882 1.08247 0.45207 1.00000 0.03024 0.00000 0.00000 C17 0.94497 0.94113 0.56243 1.00000 0.03089 0.02331 0.01918 0.00439 0.00398 -0.00114 0.02437 0.00425 0.00027 0.00042 0.00018 0.00000 0.00114 0.00113 0.00109 0.00097 0.00089 0.00101 0.00049 H17 1.03598 1.03653 0.55717 1.00000 0.02924 0.00000 0.00000 N1 0.76348 0.57950 1.13168 1.00000 0.02359 0.01961 0.01966 -0.00136 0.00231 -0.00029 0.02095 0.00332 0.00022 0.00033 0.00015 0.00000 0.00094 0.00093 0.00095 0.00079 0.00071 0.00079 0.00042 N7 0.78345 0.36341 0.97683 1.00000 0.01828 0.01738 0.01694 -0.00240 0.00215 -0.00257 0.01751 0.00316 0.00019 0.00034 0.00014 0.00000 0.00082 0.00085 0.00088 0.00074 0.00068 0.00077 0.00039 N10 0.84155 0.37588 0.75398 1.00000 0.02056 0.01748 0.01814 -0.00034 0.00020 -0.00251 0.01887 0.00307 0.00020 0.00032 0.00014 0.00000 0.00083 0.00090 0.00091 0.00078 0.00070 0.00078 0.00040 O18 0.94439 0.75823 0.63020 1.00000 0.01901 0.02382 0.01977 0.00195 -0.00012 -0.00201 0.02103 0.00266 0.00017 0.00028 0.00012 0.00000 0.00071 0.00081 0.00077 0.00068 0.00056 0.00065 0.00036 O19 0.62281 0.35655 0.62645 1.00000 0.02023 0.02693 0.02879 -0.00487 -0.00263 -0.00360 0.02571 0.00275 0.00017 0.00031 0.00013 0.00000 0.00074 0.00083 0.00086 0.00072 0.00064 0.00071 0.00039 Final Structure Factor Calculation for 2008src1283 in P2(1) Total number of l.s. parameters = 173 Maximum vector length = 511 Memory required = 2132 / 25046 wR2 = 0.0868 before cycle 5 for 1522 data and 2 / 173 parameters GooF = S = 1.048; Restrained GooF = 1.048 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0420 * P )^2 + 0.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0357 for 1356 Fo > 4sig(Fo) and 0.0435 for all 1522 data wR2 = 0.0868, GooF = S = 1.048, Restrained GooF = 1.048 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 19.00 for non-hydrogen and 15.00 for hydrogen atoms Principal mean square atomic displacements U 0.0290 0.0250 0.0182 C2 0.0300 0.0224 0.0191 C3 0.0326 0.0236 0.0193 C4 0.0268 0.0218 0.0187 C5 0.0208 0.0161 0.0129 C6 0.0261 0.0216 0.0130 C8 0.0256 0.0230 0.0164 C9 0.0235 0.0178 0.0155 C11 0.0231 0.0204 0.0132 C12 0.0254 0.0177 0.0132 C13 0.0255 0.0169 0.0146 C14 0.0319 0.0190 0.0176 C15 0.0354 0.0235 0.0166 C16 0.0311 0.0261 0.0160 C17 0.0236 0.0210 0.0183 N1 0.0210 0.0173 0.0142 N7 0.0227 0.0182 0.0156 N10 0.0260 0.0198 0.0173 O18 0.0335 0.0278 0.0158 O19 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.026 0.041 0.053 0.064 0.079 0.095 0.117 0.150 0.206 1.000 Number in group 160. 155. 150. 144. 156. 150. 153. 153. 151. 150. GooF 0.882 1.020 1.136 1.093 1.141 1.097 1.053 0.963 1.036 1.046 K 1.005 0.903 0.945 0.958 0.973 0.981 1.008 1.021 1.022 1.010 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.06 1.16 1.34 1.69 inf Number in group 159. 151. 151. 152. 148. 153. 152. 151. 154. 151. GooF 1.093 0.978 1.041 1.048 1.107 1.033 1.065 0.829 1.112 1.141 K 0.999 1.001 1.007 1.005 1.017 1.014 1.020 1.019 1.024 0.998 R1 0.111 0.098 0.076 0.059 0.054 0.037 0.031 0.024 0.027 0.023 Recommended weighting scheme: WGHT 0.0420 0.1381 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) 9 3 4 11.62 24.31 4.22 0.068 0.78 -2 0 1 584.08 702.39 3.84 0.365 4.04 -3 2 12 8.80 17.96 3.62 0.058 0.95 2 4 7 44.22 57.41 3.36 0.104 1.07 -5 5 5 4.53 10.00 3.29 0.044 0.92 -1 0 7 226.31 189.64 3.26 0.189 1.76 0 0 2 30.06 44.04 3.19 0.091 6.16 4 5 7 33.46 44.76 3.16 0.092 0.87 0 0 3 186.96 222.59 3.10 0.205 4.11 -5 3 9 17.65 25.30 2.96 0.069 0.97 0 6 8 30.07 19.24 2.83 0.060 0.83 -3 4 6 53.08 65.14 2.82 0.111 1.13 3 2 14 5.31 12.89 2.77 0.049 0.78 -3 0 11 1.32 6.10 2.76 0.034 1.08 7 5 3 5.67 13.28 2.73 0.050 0.81 -5 2 10 13.59 19.67 2.64 0.061 0.98 0 4 8 8.51 5.18 2.64 0.031 1.07 -2 6 2 5.55 9.66 2.63 0.043 0.95 3 3 12 133.52 111.31 2.58 0.145 0.84 6 0 1 25.27 32.68 2.56 0.079 1.35 2 6 6 40.77 54.45 2.55 0.102 0.86 0 1 7 9.07 5.77 2.55 0.033 1.69 -4 1 11 34.05 43.20 2.54 0.090 1.02 7 3 9 -3.79 3.65 2.54 0.026 0.78 -4 4 11 9.11 15.49 2.50 0.054 0.85 -10 1 6 8.33 16.91 2.48 0.057 0.79 7 3 7 17.18 24.25 2.47 0.068 0.84 -4 4 4 29.68 23.20 2.45 0.066 1.14 4 4 5 11.30 15.27 2.43 0.054 1.05 3 1 7 17.69 13.41 2.41 0.050 1.38 1 6 5 15.62 22.12 2.37 0.065 0.91 3 0 2 39.38 31.61 2.35 0.077 2.41 -3 1 11 41.02 49.97 2.34 0.097 1.06 -1 4 11 5.32 0.98 2.29 0.014 0.90 -5 4 10 42.27 32.60 2.29 0.079 0.85 -3 3 2 17.55 13.44 2.28 0.050 1.57 3 0 0 314.85 352.55 2.28 0.258 2.75 -3 0 13 24.15 34.48 2.28 0.081 0.93 0 4 4 53.99 45.49 2.27 0.093 1.33 4 0 9 5.28 8.49 2.26 0.040 1.09 4 6 5 8.39 16.17 2.26 0.055 0.82 2 4 1 44.25 52.44 2.26 0.100 1.38 4 1 11 0.53 2.36 2.25 0.021 0.93 3 0 6 19.45 24.82 2.25 0.069 1.57 -1 2 1 177.57 199.59 2.23 0.194 2.74 -2 3 11 35.22 43.55 2.22 0.091 0.97 -6 0 9 5.52 9.77 2.20 0.043 1.03 4 2 3 4.28 6.79 2.19 0.036 1.52 9 2 5 19.51 27.96 2.18 0.073 0.80 4 4 3 18.35 14.27 2.16 0.052 1.13 Bond lengths and angles C2 - Distance Angles N1 1.3486 (0.0029) C3 1.3781 (0.0034) 124.33 (0.23) H2 0.9500 117.84 117.84 C2 - N1 C3 C3 - Distance Angles C2 1.3781 (0.0034) C4 1.3891 (0.0034) 117.25 (0.21) H3 0.9500 121.38 121.38 C3 - C2 C4 C4 - Distance Angles C5 1.3878 (0.0032) C3 1.3891 (0.0034) 119.99 (0.22) H4 0.9500 120.01 120.01 C4 - C5 C3 C5 - Distance Angles C4 1.3878 (0.0032) C6 1.4072 (0.0030) 118.56 (0.22) H5 0.9500 120.72 120.72 C5 - C4 C6 C6 - Distance Angles N1 1.3378 (0.0029) N7 1.4000 (0.0026) 116.43 (0.18) C5 1.4072 (0.0030) 121.82 (0.19) 121.68 (0.20) C6 - N1 N7 C8 - Distance Angles N7 1.4701 (0.0027) C9 1.5209 (0.0030) 111.10 (0.16) H8A 0.9900 109.41 109.41 H8B 0.9900 109.41 109.41 108.02 C8 - N7 C9 H8A C9 - Distance Angles N10 1.4677 (0.0030) C8 1.5209 (0.0030) 110.96 (0.19) H9A 0.9900 109.45 109.45 H9B 0.9900 109.45 109.45 108.04 C9 - N10 C8 H9A C11 - Distance Angles N10 1.4688 (0.0027) C12 1.5178 (0.0029) 110.15 (0.16) H11A 0.9900 109.63 109.63 H11B 0.9900 109.63 109.63 108.15 C11 - N10 C12 H11A C12 - Distance Angles N7 1.4658 (0.0028) C11 1.5178 (0.0029) 111.30 (0.18) H12A 0.9900 109.37 109.37 H12B 0.9900 109.37 109.37 108.00 C12 - N7 C11 H12A C13 - Distance Angles O19 1.2350 (0.0026) N10 1.3612 (0.0027) 122.35 (0.22) C14 1.4774 (0.0032) 117.50 (0.19) 120.14 (0.19) C13 - O19 N10 C14 - Distance Angles C15 1.3602 (0.0031) O18 1.3782 (0.0025) 109.79 (0.20) C13 1.4774 (0.0032) 127.99 (0.20) 122.03 (0.18) C14 - C15 O18 C15 - Distance Angles C14 1.3602 (0.0031) C16 1.4199 (0.0033) 106.94 (0.19) H15 0.9500 126.53 126.53 C15 - C14 C16 C16 - Distance Angles C17 1.3511 (0.0031) C15 1.4199 (0.0033) 106.27 (0.21) H16 0.9500 126.86 126.86 C16 - C17 C15 C17 - Distance Angles C16 1.3511 (0.0031) O18 1.3696 (0.0028) 110.95 (0.21) H17 0.9500 124.52 124.52 C17 - C16 O18 N1 - Distance Angles C6 1.3378 (0.0029) C2 1.3486 (0.0029) 118.05 (0.20) N1 - C6 N7 - Distance Angles C6 1.4000 (0.0026) C12 1.4658 (0.0028) 116.68 (0.17) C8 1.4701 (0.0027) 118.18 (0.16) 113.61 (0.16) N7 - C6 C12 N10 - Distance Angles C13 1.3612 (0.0027) C9 1.4677 (0.0030) 117.78 (0.18) C11 1.4688 (0.0027) 125.44 (0.19) 110.65 (0.16) N10 - C13 C9 O18 - Distance Angles C17 1.3696 (0.0028) C14 1.3782 (0.0025) 106.03 (0.17) O18 - C17 O19 - Distance Angles C13 1.2350 (0.0026) O19 - FMAP and GRID set by program FMAP 2 2 16 GRID -3.846 -2 -2 3.846 2 2 R1 = 0.0435 for 1522 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.17 at 0.7266 0.3790 0.0169 [ 0.73 A from N7 ] Deepest hole -0.19 at 0.1214 0.1720 0.0996 [ 0.77 A from C12 ] Mean = 0.00, Rms deviation from mean = 0.04 e/A^3, Highest memory used = 2193 / 17265 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.7266 0.3790 1.0169 1.00000 0.05 0.17 0.73 N7 0.77 C6 1.78 C8 1.85 N1 Q2 1 0.7435 0.8889 0.5211 1.00000 0.05 0.16 0.70 C16 0.73 C15 1.46 H16 1.48 H15 Q3 1 0.8399 0.6181 1.3210 1.00000 0.05 0.15 1.19 H2 1.41 C2 1.80 H17 2.00 C3 Q4 1 0.7166 0.6871 0.8661 1.00000 0.05 0.15 0.51 H12B 1.41 C12 2.07 H12A 2.18 C11 Q5 1 0.8364 0.2035 1.1158 1.00000 0.05 0.15 1.45 C6 1.61 C5 1.83 H11A 1.91 H11B Q6 1 1.0433 1.0107 0.6024 1.00000 0.05 0.15 0.58 H17 1.00 C17 1.76 O18 2.26 C16 Q7 1 0.8385 0.9674 0.5601 1.00000 0.05 0.14 0.74 C16 0.89 C17 1.56 H16 1.57 C15 Q8 1 1.0605 0.3360 0.8656 1.00000 0.05 0.14 0.60 H11B 1.48 C11 2.10 N1 2.11 H9A Q9 1 0.5579 0.4612 0.5383 1.00000 0.05 0.14 1.32 O19 1.75 H15 1.84 H15 2.10 C13 Q10 1 0.8039 0.4611 0.9546 1.00000 0.05 0.14 0.67 N7 0.80 C12 1.43 H12B 1.48 H12A Shortest distances between peaks (including symmetry equivalents) 2 7 0.99 1 10 1.16 3 6 1.43 6 7 1.74 1 5 1.78 4 10 1.83 5 8 2.34 5 10 2.50 2 9 2.56 1 4 2.61 8 10 2.61 2 6 2.68 3 8 2.85 2 9 2.98 Time profile in seconds ----------------------- 0.00: 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 0.02: Analyse other restraints etc. 0.38: 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 0.31: Structure factors and derivatives 0.30: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.08: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.02: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008src1283 finished at 14:52:25 Total CPU time: 1.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++