+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0462 started at 11:25:01 on 28-Apr-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0462 in P2(1)/n CELL 0.71073 4.9556 15.8959 15.8659 90.000 92.257 90.000 ZERR 4.00 0.0001 0.0004 0.0004 0.000 0.002 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 60 44 12 8 V = 1248.85 F(000) = 552.0 Mu = 0.10 mm-1 Cell Wt = 1061.07 Rho = 1.411 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 FMAP 2 PLAN 10 SIZE 0.04 0.07 0.67 ACTA BOND $H WGHT 0.02110 1.57610 L.S. 4 TEMP -153.00 FVAR 0.44123 MOLE 1 C1 1 -0.231501 0.093730 0.361134 11.00000 0.01910 0.01964 = 0.02668 -0.00258 0.00149 -0.00274 C2 1 -0.274013 0.168661 0.316040 11.00000 0.02111 0.02589 = 0.02467 0.00146 0.00020 -0.00471 AFIX 43 H2 2 -0.174149 0.179947 0.267409 11.00000 -1.20000 AFIX 0 C3 1 -0.461492 0.225917 0.342607 11.00000 0.02259 0.02052 = 0.02966 0.00225 -0.00107 -0.00211 AFIX 43 H3 2 -0.491592 0.276434 0.311652 11.00000 -1.20000 AFIX 0 C4 1 -0.607127 0.210616 0.414194 11.00000 0.01839 0.02106 = 0.02781 -0.00332 -0.00206 -0.00053 C5 1 -0.568837 0.135750 0.459380 11.00000 0.02188 0.02332 = 0.02654 -0.00065 0.00211 -0.00269 AFIX 43 H5 2 -0.670802 0.124198 0.507508 11.00000 -1.20000 AFIX 0 C6 1 -0.378628 0.078682 0.432390 11.00000 0.02301 0.01912 = 0.02703 0.00114 0.00045 -0.00062 AFIX 43 H6 2 -0.348302 0.028171 0.463335 11.00000 -1.20000 AFIX 0 C7 1 -0.038880 0.030764 0.335233 11.00000 0.02038 0.02473 = 0.01942 -0.00047 0.00152 -0.00362 C9 1 0.275926 -0.017843 0.257646 11.00000 0.02104 0.02244 = 0.02437 -0.00376 -0.00070 -0.00022 C10 1 0.209433 -0.076656 0.315813 11.00000 0.02538 0.02441 = 0.02105 -0.00529 -0.00012 0.00147 C13 1 0.501708 0.055936 0.143530 11.00000 0.03247 0.02626 = 0.02609 0.00449 0.00272 0.00256 AFIX 43 H13 2 0.411832 0.108643 0.145566 11.00000 -1.20000 AFIX 0 C14 1 0.699789 0.034594 0.091162 11.00000 0.03385 0.03905 = 0.02454 0.00334 0.00680 0.00061 AFIX 43 H14 2 0.773687 0.070062 0.049755 11.00000 -1.20000 AFIX 0 C15 1 0.778306 -0.049551 0.108517 11.00000 0.02785 0.03409 = 0.02781 -0.00551 0.00581 0.00328 AFIX 43 H15 2 0.914065 -0.080178 0.081059 11.00000 -1.20000 AFIX 0 C16 1 0.625478 -0.078579 0.171199 11.00000 0.02932 0.02611 = 0.03123 -0.00501 0.00402 0.00226 AFIX 43 H16 2 0.633859 -0.133283 0.195272 11.00000 -1.20000 AFIX 0 C17 1 0.312630 -0.159680 0.328611 11.00000 0.02753 0.03062 = 0.02075 -0.00118 0.00181 0.00316 C20 1 -0.943707 0.258328 0.507099 11.00000 0.02436 0.03086 = 0.03114 -0.00689 0.00332 0.00249 AFIX 137 H20A 2 -1.040337 0.204892 0.499628 11.00000 -1.50000 H20B 2 -1.074318 0.304225 0.511743 11.00000 -1.50000 H20C 2 -0.828031 0.255876 0.558580 11.00000 -1.50000 AFIX 0 N11 3 0.004763 -0.044005 0.364991 11.00000 0.02442 0.02367 = 0.02333 -0.00118 0.00240 0.00124 N12 3 0.454443 -0.013999 0.193913 11.00000 0.02352 0.02584 = 0.02196 -0.00272 0.00381 0.00226 N18 3 0.392485 -0.226874 0.338700 11.00000 0.04269 0.03057 = 0.02871 -0.00076 0.00058 0.01005 O8 4 0.121996 0.050975 0.268862 11.00000 0.02082 0.02195 = 0.02304 -0.00001 0.00354 0.00024 O19 4 -0.780759 0.272922 0.436038 11.00000 0.02515 0.02373 = 0.03690 0.00002 0.00436 0.00466 HKLF 4 Covalent radii and connectivity table for 2009src0462 in P2(1)/n C 0.770 H 0.320 N 0.700 O 0.660 C1 - C6 C2 C7 C2 - C3 C1 C3 - C2 C4 C4 - O19 C3 C5 C5 - C6 C4 C6 - C5 C1 C7 - N11 O8 C1 C9 - O8 C10 N12 C10 - C9 N11 C17 C13 - C14 N12 C14 - C13 C15 C15 - C16 C14 C16 - C15 N12 C17 - N18 C10 C20 - O19 N11 - C7 C10 N12 - C9 C16 C13 N18 - C17 O8 - C9 C7 O19 - C4 C20 15096 Reflections read, of which 343 rejected -6 =< h =< 6, -20 =< k =< 20, -20 =< l =< 16, Max. 2-theta = 54.95 0 Systematic absence violations 0 Inconsistent equivalents 2865 Unique reflections, of which 0 suppressed R(int) = 0.0588 R(sigma) = 0.0500 Friedel opposites merged Maximum memory for data reduction = 1695 / 28439 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 = 2183 / 226016 wR2 = 0.1322 before cycle 1 for 2865 data and 182 / 182 parameters GooF = S = 1.079; Restrained GooF = 1.079 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0211 * P )^2 + 1.58 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.44103 0.00104 -0.191 OSF Mean shift/su = 0.038 Maximum = -0.191 for OSF Max. shift = 0.001 A for H20C Max. dU = 0.000 for C1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2183 / 226016 wR2 = 0.1322 before cycle 2 for 2865 data and 182 / 182 parameters GooF = S = 1.080; Restrained GooF = 1.080 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0211 * P )^2 + 1.58 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.44096 0.00104 -0.067 OSF Mean shift/su = 0.013 Maximum = -0.067 for OSF Max. shift = 0.000 A for H20C Max. dU = 0.000 for C1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2183 / 226016 wR2 = 0.1322 before cycle 3 for 2865 data and 182 / 182 parameters GooF = S = 1.080; Restrained GooF = 1.080 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0211 * P )^2 + 1.58 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.44096 0.00104 0.001 OSF Mean shift/su = 0.001 Maximum = 0.003 for z C4 Max. shift = 0.000 A for C4 Max. dU = 0.000 for C20 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2183 / 226016 wR2 = 0.1322 before cycle 4 for 2865 data and 182 / 182 parameters GooF = S = 1.080; Restrained GooF = 1.080 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0211 * P )^2 + 1.58 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.44096 0.00104 0.001 OSF Mean shift/su = 0.000 Maximum = 0.002 for U22 O19 Max. shift = 0.000 A for C6 Max. dU = 0.000 for C16 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 -0.1742 0.1799 0.2674 43 0.950 0.000 C2 C3 C1 H3 -0.4916 0.2764 0.3116 43 0.950 0.000 C3 C2 C4 H5 -0.6707 0.1242 0.5075 43 0.950 0.000 C5 C6 C4 H6 -0.3484 0.0281 0.4633 43 0.950 0.000 C6 C5 C1 H13 0.4117 0.1086 0.1456 43 0.950 0.000 C13 C14 N12 H14 0.7737 0.0701 0.0498 43 0.950 0.000 C14 C13 C15 H15 0.9141 -0.0802 0.0811 43 0.950 0.000 C15 C16 C14 H16 0.6338 -0.1333 0.1953 43 0.950 0.000 C16 C15 N12 H20A -1.0406 0.2049 0.4996 137 0.980 0.000 C20 O19 H20A H20B -1.0741 0.3043 0.5118 137 0.980 0.000 C20 O19 H20A H20C -0.8280 0.2558 0.5586 137 0.980 0.000 C20 O19 H20A 2009src0462 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.23146 0.09373 0.36113 1.00000 0.01908 0.01953 0.02653 -0.00261 0.00146 -0.00273 0.02170 0.00355 0.00041 0.00013 0.00013 0.00000 0.00101 0.00100 0.00109 0.00086 0.00084 0.00085 0.00045 C2 -0.27402 0.16865 0.31604 1.00000 0.02106 0.02579 0.02458 0.00147 0.00022 -0.00472 0.02383 0.00367 0.00043 0.00014 0.00014 0.00000 0.00104 0.00109 0.00110 0.00090 0.00084 0.00091 0.00047 H2 -0.17417 0.17993 0.26740 1.00000 0.02860 0.00000 0.00000 C3 -0.46152 0.22592 0.34260 1.00000 0.02259 0.02045 0.02956 0.00230 -0.00104 -0.00215 0.02425 0.00373 0.00043 0.00013 0.00014 0.00000 0.00108 0.00104 0.00115 0.00090 0.00090 0.00088 0.00047 H3 -0.49164 0.27643 0.31165 1.00000 0.02910 0.00000 0.00000 C4 -0.60709 0.21060 0.41419 1.00000 0.01833 0.02105 0.02774 -0.00332 -0.00199 -0.00058 0.02245 0.00358 0.00042 0.00013 0.00014 0.00000 0.00100 0.00102 0.00112 0.00087 0.00086 0.00085 0.00046 C5 -0.56880 0.13576 0.45937 1.00000 0.02186 0.02325 0.02649 -0.00065 0.00218 -0.00270 0.02384 0.00369 0.00043 0.00013 0.00014 0.00000 0.00107 0.00105 0.00111 0.00090 0.00087 0.00089 0.00047 H5 -0.67074 0.12422 0.50751 1.00000 0.02861 0.00000 0.00000 C6 -0.37864 0.07867 0.43239 1.00000 0.02299 0.01901 0.02699 0.00115 0.00048 -0.00067 0.02301 0.00367 0.00043 0.00013 0.00014 0.00000 0.00106 0.00100 0.00110 0.00087 0.00086 0.00087 0.00046 H6 -0.34839 0.02815 0.46332 1.00000 0.02761 0.00000 0.00000 C7 -0.03895 0.03077 0.33524 1.00000 0.02033 0.02464 0.01934 -0.00049 0.00151 -0.00363 0.02142 0.00356 0.00042 0.00013 0.00013 0.00000 0.00103 0.00107 0.00101 0.00085 0.00082 0.00087 0.00045 C9 0.27592 -0.01785 0.25765 1.00000 0.02102 0.02235 0.02426 -0.00378 -0.00068 -0.00018 0.02258 0.00360 0.00043 0.00013 0.00013 0.00000 0.00104 0.00105 0.00109 0.00088 0.00085 0.00087 0.00046 C10 0.20946 -0.07666 0.31580 1.00000 0.02531 0.02428 0.02110 -0.00520 -0.00010 0.00145 0.02359 0.00368 0.00044 0.00014 0.00013 0.00000 0.00110 0.00108 0.00104 0.00087 0.00085 0.00091 0.00047 C13 0.50166 0.05593 0.14355 1.00000 0.03244 0.02624 0.02611 0.00444 0.00267 0.00258 0.02822 0.00413 0.00048 0.00015 0.00014 0.00000 0.00124 0.00113 0.00115 0.00095 0.00095 0.00099 0.00051 H13 0.41175 0.10863 0.14559 1.00000 0.03387 0.00000 0.00000 C14 0.69978 0.03460 0.09116 1.00000 0.03375 0.03893 0.02454 0.00333 0.00683 0.00058 0.03226 0.00439 0.00050 0.00016 0.00015 0.00000 0.00129 0.00136 0.00115 0.00103 0.00099 0.00111 0.00055 H14 0.77367 0.07007 0.04976 1.00000 0.03871 0.00000 0.00000 C15 0.77832 -0.04956 0.10851 1.00000 0.02778 0.03404 0.02780 -0.00555 0.00580 0.00319 0.02975 0.00413 0.00047 0.00015 0.00014 0.00000 0.00119 0.00128 0.00117 0.00101 0.00096 0.00101 0.00053 H15 0.91407 -0.08019 0.08105 1.00000 0.03570 0.00000 0.00000 C16 0.62546 -0.07858 0.17120 1.00000 0.02924 0.02603 0.03119 -0.00503 0.00398 0.00228 0.02875 0.00403 0.00047 0.00015 0.00015 0.00000 0.00119 0.00115 0.00121 0.00098 0.00096 0.00098 0.00051 H16 0.63381 -0.13328 0.19528 1.00000 0.03450 0.00000 0.00000 C17 0.31262 -0.15968 0.32862 1.00000 0.02744 0.03060 0.02072 -0.00125 0.00182 0.00307 0.02623 0.00397 0.00046 0.00015 0.00014 0.00000 0.00116 0.00124 0.00107 0.00093 0.00088 0.00098 0.00049 C20 -0.94374 0.25832 0.50710 1.00000 0.02429 0.03087 0.03111 -0.00694 0.00341 0.00258 0.02870 0.00409 0.00046 0.00015 0.00015 0.00000 0.00114 0.00122 0.00123 0.00099 0.00094 0.00098 0.00051 H20A -1.04061 0.20494 0.49958 1.00000 0.04305 0.00000 0.00000 H20B -1.07414 0.30427 0.51181 1.00000 0.04305 0.00000 0.00000 H20C -0.82803 0.25577 0.55857 1.00000 0.04305 0.00000 0.00000 N11 0.00472 -0.04401 0.36501 1.00000 0.02435 0.02362 0.02329 -0.00118 0.00237 0.00119 0.02372 0.00318 0.00037 0.00011 0.00011 0.00000 0.00093 0.00093 0.00092 0.00075 0.00074 0.00077 0.00041 N12 0.45445 -0.01399 0.19391 1.00000 0.02343 0.02577 0.02187 -0.00270 0.00384 0.00224 0.02361 0.00320 0.00037 0.00011 0.00011 0.00000 0.00092 0.00095 0.00092 0.00077 0.00074 0.00078 0.00041 N18 0.39250 -0.22688 0.33870 1.00000 0.04270 0.03055 0.02863 -0.00072 0.00057 0.00994 0.03398 0.00372 0.00044 0.00013 0.00013 0.00000 0.00123 0.00112 0.00108 0.00088 0.00091 0.00096 0.00049 O8 0.12199 0.05098 0.26886 1.00000 0.02081 0.02188 0.02300 -0.00001 0.00360 0.00023 0.02182 0.00252 0.00028 0.00009 0.00009 0.00000 0.00075 0.00074 0.00075 0.00060 0.00059 0.00061 0.00034 O19 -0.78073 0.27293 0.43602 1.00000 0.02507 0.02370 0.03678 0.00006 0.00440 0.00465 0.02843 0.00282 0.00031 0.00009 0.00010 0.00000 0.00081 0.00081 0.00092 0.00069 0.00069 0.00066 0.00038 Final Structure Factor Calculation for 2009src0462 in P2(1)/n Total number of l.s. parameters = 182 Maximum vector length = 511 Memory required = 2001 / 22995 wR2 = 0.1322 before cycle 5 for 2865 data and 0 / 182 parameters GooF = S = 1.080; Restrained GooF = 1.080 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0211 * P )^2 + 1.58 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0617 for 2147 Fo > 4sig(Fo) and 0.0895 for all 2865 data wR2 = 0.1322, GooF = S = 1.080, Restrained GooF = 1.080 for all data Occupancy sum of asymmetric unit = 20.00 for non-hydrogen and 11.00 for hydrogen atoms Principal mean square atomic displacements U 0.0276 0.0211 0.0164 C1 0.0293 0.0240 0.0181 C2 0.0310 0.0228 0.0190 C3 0.0298 0.0206 0.0170 C4 0.0273 0.0246 0.0197 C5 0.0273 0.0230 0.0187 C6 0.0268 0.0194 0.0181 C7 0.0275 0.0214 0.0189 C9 0.0291 0.0244 0.0172 C10 0.0345 0.0285 0.0217 C13 0.0402 0.0354 0.0212 C14 0.0373 0.0319 0.0200 C15 0.0345 0.0304 0.0213 C16 0.0325 0.0259 0.0203 C17 0.0379 0.0276 0.0205 C20 0.0254 0.0246 0.0211 N11 0.0274 0.0256 0.0179 N12 0.0484 0.0286 0.0249 N18 0.0248 0.0219 0.0188 O8 0.0376 0.0284 0.0194 O19 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.005 0.010 0.015 0.021 0.027 0.035 0.044 0.058 0.087 1.000 Number in group 306. 282. 284. 322. 271. 275. 277. 276. 284. 288. GooF 1.122 1.166 1.156 1.096 1.028 1.112 1.019 1.010 0.932 1.121 K 4.354 1.558 1.188 1.044 1.016 1.033 1.001 1.002 1.005 0.987 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.32 1.63 inf Number in group 293. 285. 292. 276. 290. 289. 279. 289. 285. 287. GooF 1.177 1.188 1.186 1.109 1.009 1.067 0.872 0.985 0.948 1.193 K 1.140 1.057 1.040 1.018 0.998 0.993 0.995 1.000 1.028 0.978 R1 0.245 0.200 0.175 0.141 0.102 0.085 0.046 0.057 0.046 0.035 Recommended weighting scheme: WGHT 0.0201 1.5771 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 1 2 16.85 0.03 3.44 0.001 1.23 3 11 14 40.23 1.09 3.39 0.004 0.77 3 10 9 33.31 4.86 3.31 0.010 0.95 3 8 15 27.70 69.01 3.24 0.036 0.80 1 16 10 5.37 28.73 3.21 0.023 0.83 1 11 12 35.25 10.70 3.16 0.014 0.95 0 2 2 7684.49 8510.92 3.16 0.398 5.61 4 1 15 22.14 1.68 3.12 0.006 0.79 -1 15 11 12.53 49.17 3.11 0.030 0.84 -2 2 19 34.35 11.37 3.08 0.015 0.80 3 16 7 72.88 35.70 3.04 0.026 0.79 4 5 10 56.49 26.06 3.01 0.022 0.92 -5 3 8 2.91 21.47 2.99 0.020 0.89 -2 1 5 3611.30 3239.56 2.98 0.245 1.97 -2 18 7 32.65 7.63 2.94 0.012 0.78 3 15 3 33.35 7.17 2.88 0.012 0.88 2 4 5 -1.03 11.88 2.87 0.015 1.73 -2 3 7 484.28 396.93 2.84 0.086 1.62 -1 3 5 452.56 547.91 2.80 0.101 2.42 -4 3 15 -9.96 13.45 2.78 0.016 0.81 3 14 8 93.40 54.65 2.78 0.032 0.84 -1 0 9 621.48 512.23 2.76 0.098 1.68 -2 11 16 45.52 6.00 2.73 0.011 0.78 0 12 15 52.92 2.42 2.71 0.007 0.83 0 16 7 6.22 26.64 2.69 0.022 0.91 -4 10 1 15.28 37.57 2.66 0.026 0.98 -2 6 14 21.26 3.97 2.64 0.009 0.97 -2 2 18 80.63 47.46 2.64 0.030 0.84 -1 17 10 -9.52 22.68 2.64 0.021 0.80 5 8 7 76.26 35.74 2.64 0.026 0.82 4 8 10 23.66 51.08 2.63 0.031 0.86 1 3 19 34.07 2.10 2.60 0.006 0.81 1 1 3 15036.52 16379.54 2.58 0.552 3.46 -1 1 7 1260.95 1114.62 2.57 0.144 2.07 -1 0 1 39.82 16.99 2.55 0.018 4.78 -4 13 3 63.26 118.83 2.55 0.047 0.86 -1 8 3 -1.48 5.85 2.54 0.010 1.75 -4 9 10 108.07 64.72 2.53 0.035 0.87 3 15 8 55.02 27.03 2.52 0.022 0.81 -5 9 4 -10.05 9.19 2.49 0.013 0.85 -6 6 3 128.88 43.86 2.49 0.029 0.78 1 7 11 4.65 18.17 2.48 0.018 1.17 -3 9 6 61.16 94.04 2.46 0.042 1.11 0 19 1 17.40 0.28 2.45 0.002 0.84 2 15 11 104.81 59.23 2.45 0.033 0.80 -4 11 12 172.66 110.19 2.44 0.045 0.78 -3 17 3 -8.59 7.64 2.43 0.012 0.81 -2 11 15 80.74 39.94 2.43 0.027 0.81 5 3 2 13.66 1.16 2.41 0.005 0.96 6 0 4 209.62 150.92 2.39 0.053 0.80 Bond lengths and angles C1 - Distance Angles C6 1.3900 (0.0030) C2 1.4010 (0.0030) 119.24 (0.20) C7 1.4530 (0.0030) 118.86 (0.19) 121.90 (0.19) C1 - C6 C2 C2 - Distance Angles C3 1.3787 (0.0031) C1 1.4010 (0.0030) 119.66 (0.20) H2 0.9500 120.17 120.17 C2 - C3 C1 C3 - Distance Angles C2 1.3787 (0.0031) C4 1.3908 (0.0031) 120.77 (0.20) H3 0.9500 119.62 119.62 C3 - C2 C4 C4 - Distance Angles O19 1.3659 (0.0026) C3 1.3908 (0.0031) 115.61 (0.19) C5 1.3979 (0.0030) 124.16 (0.20) 120.23 (0.20) C4 - O19 C3 C5 - Distance Angles C6 1.3880 (0.0030) C4 1.3979 (0.0030) 118.58 (0.20) H5 0.9500 120.71 120.71 C5 - C6 C4 C6 - Distance Angles C5 1.3880 (0.0030) C1 1.3900 (0.0030) 121.51 (0.20) H6 0.9500 119.25 119.25 C6 - C5 C1 C7 - Distance Angles N11 1.2942 (0.0028) O8 1.3838 (0.0025) 113.44 (0.18) C1 1.4530 (0.0030) 129.17 (0.20) 117.38 (0.18) C7 - N11 O8 C9 - Distance Angles O8 1.3495 (0.0025) C10 1.3629 (0.0031) 108.30 (0.19) N12 1.3711 (0.0028) 116.45 (0.19) 135.25 (0.20) C9 - O8 C10 C10 - Distance Angles C9 1.3629 (0.0031) N11 1.4038 (0.0028) 108.79 (0.19) C17 1.4270 (0.0031) 129.50 (0.21) 121.70 (0.20) C10 - C9 N11 C13 - Distance Angles C14 1.3543 (0.0033) N12 1.3940 (0.0029) 107.11 (0.20) H13 0.9500 126.44 126.44 C13 - C14 N12 C14 - Distance Angles C13 1.3543 (0.0033) C15 1.4172 (0.0034) 108.50 (0.21) H14 0.9500 125.75 125.75 C14 - C13 C15 C15 - Distance Angles C16 1.3548 (0.0033) C14 1.4172 (0.0034) 107.87 (0.21) H15 0.9500 126.07 126.07 C15 - C16 C14 C16 - Distance Angles C15 1.3548 (0.0033) N12 1.3878 (0.0028) 107.67 (0.21) H16 0.9500 126.17 126.17 C16 - C15 N12 C17 - Distance Angles N18 1.1482 (0.0029) C10 1.4270 (0.0031) 179.15 (0.26) C17 - N18 C20 - Distance Angles O19 1.4318 (0.0027) H20A 0.9800 109.47 H20B 0.9800 109.47 109.47 H20C 0.9800 109.47 109.47 109.47 C20 - O19 H20A H20B N11 - Distance Angles C7 1.2942 (0.0028) C10 1.4038 (0.0028) 104.52 (0.18) N11 - C7 N12 - Distance Angles C9 1.3711 (0.0028) C16 1.3878 (0.0028) 125.22 (0.19) C13 1.3940 (0.0029) 125.89 (0.19) 108.85 (0.18) N12 - C9 C16 N18 - Distance Angles C17 1.1482 (0.0029) N18 - O8 - Distance Angles C9 1.3495 (0.0025) C7 1.3838 (0.0025) 104.94 (0.16) O8 - C9 O19 - Distance Angles C4 1.3659 (0.0026) C20 1.4318 (0.0027) 117.56 (0.17) O19 - C4 FMAP and GRID set by program FMAP 2 1 9 GRID -4.167 -2 -2 4.167 2 2 R1 = 0.0895 for 2865 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.24 at 0.1636 0.9293 0.2607 [ 0.90 A from C10 ] Deepest hole -0.24 at 0.0465 -0.0040 0.3193 [ 0.75 A from C7 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 2570 / 20598 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1636 -0.0707 0.2607 1.00000 0.05 0.24 0.90 C10 1.01 C9 1.91 N11 1.91 C17 Q2 1 -0.5389 0.2987 0.2923 1.00000 0.05 0.22 0.52 H3 1.45 C3 2.28 H16 2.40 C17 Q3 1 0.3406 0.1004 0.1609 1.00000 0.05 0.22 0.46 H13 1.11 C13 1.97 N12 2.21 O8 Q4 1 -0.3382 0.0740 0.3815 1.00000 0.05 0.21 0.70 C1 0.84 C6 1.49 H6 1.82 C7 Q5 1 -0.1579 0.0642 0.3373 1.00000 0.05 0.21 0.71 C1 0.80 C7 1.78 C2 1.81 O8 Q6 1 -0.2787 0.1182 0.3367 1.00000 0.05 0.21 0.59 C1 0.87 C2 1.58 H2 1.73 C6 Q7 1 0.1940 0.0016 0.1195 1.00000 0.05 0.20 1.73 N12 1.78 C13 1.98 H15 2.05 H13 Q8 1 0.4791 0.2038 0.1749 1.00000 0.05 0.20 1.61 H13 2.15 N18 2.21 H20C 2.25 H2 Q9 1 -0.9614 0.1805 0.5805 1.00000 0.05 0.20 1.38 H20A 1.42 H20C 1.70 C20 2.09 H5 Q10 1 0.0593 -0.0408 0.4126 1.00000 0.05 0.19 0.79 N11 1.73 C7 1.82 C10 2.40 H6 Shortest distances between peaks (including symmetry equivalents) 5 6 1.05 4 6 1.05 4 5 1.17 3 8 1.79 3 7 1.84 9 10 2.27 5 10 2.30 1 2 2.31 8 9 2.40 2 8 2.40 1 7 2.53 1 10 2.53 4 10 2.72 1 5 2.96 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. 0.69: 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 0.50: Structure factors and derivatives 0.64: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.09: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0462 finished at 11:25:03 Total CPU time: 2.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++