+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 07ch0001 started at 14:41:36 on 31-Jul-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 07ch0001 in P2(1)/c CELL 0.71073 3.9766 16.1062 11.5115 90.000 90.407 90.000 ZERR 4.00 0.0003 0.0013 0.0009 0.000 0.005 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H O UNIT 32 32 16 V = 737.27 F(000) = 352.0 Mu = 0.12 mm-1 Cell Wt = 672.58 Rho = 1.515 MERG 2 OMIT -3.00 55.00 OMIT 1 0 2 EQIV $1 -X, -Y, -Z+1 HTAB O1 O2_$1 hTAB O3 O2 FMAP 2 PLAN 5 SIZE 0.06 0.12 0.26 ACTA BOND $H WGHT 0.06350 0.24050 L.S. 7 TEMP -153.00 FVAR 1.01782 C1 1 0.269458 0.157283 0.326946 11.00000 0.02131 0.01685 = 0.02163 -0.00053 -0.00279 -0.00215 C2 1 0.453277 0.140169 0.226244 11.00000 0.02269 0.01845 = 0.02446 -0.00257 -0.00048 -0.00086 C3 1 0.545330 0.205999 0.153690 11.00000 0.02498 0.02682 = 0.02164 -0.00094 0.00226 -0.00143 AFIX 43 H3 2 0.669013 0.195122 0.085047 11.00000 -1.20000 AFIX 0 C4 1 0.458658 0.285909 0.180802 11.00000 0.02543 0.02138 = 0.02241 0.00405 -0.00003 -0.00215 AFIX 43 H4 2 0.523874 0.329877 0.130776 11.00000 -1.20000 AFIX 0 C5 1 0.276170 0.303749 0.280695 11.00000 0.02121 0.01655 = 0.02654 0.00109 -0.00171 -0.00016 C6 1 0.182343 0.240056 0.353728 11.00000 0.02091 0.01995 = 0.02349 -0.00103 0.00123 -0.00114 AFIX 43 H6 2 0.058966 0.251894 0.422127 11.00000 -1.20000 AFIX 0 C7 1 0.162904 0.089062 0.402294 11.00000 0.02219 0.01837 = 0.02355 -0.00127 -0.00071 -0.00178 C8 1 0.026860 0.407961 0.400065 11.00000 0.03103 0.02149 = 0.02940 -0.00060 0.00391 0.00012 AFIX 137 H8A 2 -0.193041 0.380492 0.399883 11.00000 -1.50000 H8B 2 -0.004634 0.468274 0.402852 11.00000 -1.50000 H8C 2 0.156687 0.389986 0.468235 11.00000 -1.50000 AFIX 0 O1 3 -0.026376 0.111113 0.490804 11.00000 0.03555 0.01807 = 0.02735 0.00305 0.01024 0.00138 AFIX 147 H1 2 -0.088163 0.068527 0.526969 11.00000 -1.50000 AFIX 0 O2 3 0.242050 0.015621 0.384595 11.00000 0.03266 0.01726 = 0.02916 0.00055 0.00660 0.00049 O3 3 0.554496 0.063202 0.193604 11.00000 0.04090 0.01802 = 0.03151 -0.00130 0.01007 0.00213 AFIX 147 H3A 2 0.494670 0.028401 0.243723 11.00000 -1.50000 AFIX 0 O4 3 0.203788 0.386323 0.297062 11.00000 0.03569 0.01554 = 0.02946 0.00242 0.00669 0.00122 HKLF 4 Covalent radii and connectivity table for 07ch0001 in P2(1)/c C 0.770 H 0.320 O 0.660 C1 - C2 C6 C7 C2 - O3 C3 C1 C3 - C4 C2 C4 - C3 C5 C5 - O4 C6 C4 C6 - C5 C1 C7 - O2 O1 C1 C8 - O4 O1 - C7 O2 - C7 O3 - C2 O4 - C5 C8 Operators for generating equivalent atoms: $1 -x, -y, -z+1 8296 Reflections read, of which 208 rejected -5 =< h =< 5, -20 =< k =< 20, -14 =< l =< 14, Max. 2-theta = 55.00 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -4 8 6 -1.05 4.14 2 23.84 -3 6 10 -0.55 0.67 4 3.51 2 Inconsistent equivalents 1690 Unique reflections, of which 0 suppressed R(int) = 0.0567 R(sigma) = 0.0561 Friedel opposites merged Maximum memory for data reduction = 1240 / 16837 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 = 1541 / 142989 wR2 = 0.1333 before cycle 1 for 1690 data and 112 / 112 parameters GooF = S = 1.022; Restrained GooF = 1.022 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0635 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.01779 0.00346 -0.009 OSF Mean shift/esd = 0.005 Maximum = -0.017 for U22 O1 Max. shift = 0.000 A for H3A Max. dU = 0.000 for C1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1541 / 142989 wR2 = 0.1333 before cycle 2 for 1690 data and 112 / 112 parameters GooF = S = 1.022; Restrained GooF = 1.022 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0635 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.01776 0.00346 -0.009 OSF Mean shift/esd = 0.002 Maximum = -0.009 for OSF Max. shift = 0.000 A for H3A Max. dU = 0.000 for C1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1541 / 142989 wR2 = 0.1333 before cycle 3 for 1690 data and 112 / 112 parameters GooF = S = 1.022; Restrained GooF = 1.022 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0635 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.01776 0.00346 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H3A Max. dU = 0.000 for C2 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1541 / 142989 wR2 = 0.1333 before cycle 4 for 1690 data and 112 / 112 parameters GooF = S = 1.022; Restrained GooF = 1.022 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0635 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.01776 0.00346 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y O4 Max. shift = 0.000 A for H3A Max. dU = 0.000 for C7 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1541 / 142989 wR2 = 0.1333 before cycle 5 for 1690 data and 112 / 112 parameters GooF = S = 1.022; Restrained GooF = 1.022 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0635 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.01776 0.00346 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O4 Max. shift = 0.000 A for O4 Max. dU = 0.000 for C3 Least-squares cycle 6 Maximum vector length = 511 Memory required = 1541 / 142989 wR2 = 0.1333 before cycle 6 for 1690 data and 112 / 112 parameters GooF = S = 1.022; Restrained GooF = 1.022 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0635 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.01776 0.00346 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y O4 Max. shift = 0.000 A for O4 Max. dU = 0.000 for O3 Least-squares cycle 7 Maximum vector length = 511 Memory required = 1541 / 142989 wR2 = 0.1333 before cycle 7 for 1690 data and 112 / 112 parameters GooF = S = 1.022; Restrained GooF = 1.022 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0635 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.01776 0.00346 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O1 Max. shift = 0.000 A for H8A Max. dU = 0.000 for O3 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 8 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 0.6690 0.1951 0.0850 43 0.950 0.000 C3 C4 C2 H4 0.5239 0.3299 0.1308 43 0.950 0.000 C4 C3 C5 H6 0.0590 0.2519 0.4221 43 0.950 0.000 C6 C5 C1 H8A -0.1930 0.3805 0.3999 137 0.980 0.000 C8 O4 H8A H8B -0.0046 0.4683 0.4029 137 0.980 0.000 C8 O4 H8A H8C 0.1567 0.3900 0.4682 137 0.980 0.000 C8 O4 H8A H1 -0.0882 0.0685 0.5270 147 0.840 0.000 O1 C7 H1 H3A 0.4946 0.0284 0.2437 147 0.840 0.000 O3 C2 H3A 07ch0001 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.26946 0.15728 0.32695 1.00000 0.02130 0.01684 0.02162 -0.00054 -0.00279 -0.00214 0.01993 0.00312 0.00046 0.00011 0.00016 0.00000 0.00095 0.00090 0.00095 0.00073 0.00075 0.00074 0.00042 C2 0.45328 0.14017 0.22624 1.00000 0.02267 0.01844 0.02445 -0.00257 -0.00047 -0.00085 0.02186 0.00325 0.00048 0.00011 0.00016 0.00000 0.00098 0.00096 0.00100 0.00075 0.00079 0.00077 0.00044 C3 0.54533 0.20600 0.15369 1.00000 0.02497 0.02681 0.02163 -0.00095 0.00226 -0.00142 0.02446 0.00337 0.00048 0.00012 0.00016 0.00000 0.00099 0.00105 0.00099 0.00079 0.00077 0.00081 0.00045 H3 0.66901 0.19512 0.08505 1.00000 0.02935 0.00000 0.00000 C4 0.45866 0.28591 0.18080 1.00000 0.02542 0.02138 0.02240 0.00404 -0.00003 -0.00214 0.02307 0.00334 0.00048 0.00012 0.00016 0.00000 0.00099 0.00096 0.00098 0.00076 0.00078 0.00080 0.00044 H4 0.52388 0.32988 0.13078 1.00000 0.02768 0.00000 0.00000 C5 0.27617 0.30375 0.28070 1.00000 0.02120 0.01654 0.02653 0.00109 -0.00171 -0.00016 0.02143 0.00322 0.00046 0.00011 0.00016 0.00000 0.00092 0.00093 0.00102 0.00076 0.00076 0.00076 0.00043 C6 0.18234 0.24006 0.35373 1.00000 0.02090 0.01994 0.02348 -0.00103 0.00123 -0.00114 0.02143 0.00325 0.00046 0.00011 0.00016 0.00000 0.00090 0.00096 0.00099 0.00074 0.00076 0.00075 0.00043 H6 0.05897 0.25189 0.42213 1.00000 0.02572 0.00000 0.00000 C7 0.16290 0.08906 0.40229 1.00000 0.02218 0.01837 0.02354 -0.00128 -0.00072 -0.00178 0.02137 0.00320 0.00046 0.00011 0.00016 0.00000 0.00096 0.00095 0.00102 0.00075 0.00078 0.00079 0.00043 C8 0.02686 0.40796 0.40007 1.00000 0.03101 0.02149 0.02939 -0.00060 0.00391 0.00012 0.02728 0.00372 0.00053 0.00012 0.00018 0.00000 0.00108 0.00100 0.00112 0.00081 0.00088 0.00083 0.00048 H8A -0.19304 0.38049 0.39989 1.00000 0.04092 0.00000 0.00000 H8B -0.00465 0.46827 0.40285 1.00000 0.04092 0.00000 0.00000 H8C 0.15669 0.38999 0.46824 1.00000 0.04092 0.00000 0.00000 O1 -0.02637 0.11111 0.49080 1.00000 0.03554 0.01805 0.02735 0.00305 0.01024 0.00138 0.02693 0.00251 0.00035 0.00008 0.00011 0.00000 0.00082 0.00069 0.00078 0.00056 0.00063 0.00058 0.00037 H1 -0.08816 0.06853 0.52697 1.00000 0.04040 0.00000 0.00000 O2 0.24205 0.01562 0.38459 1.00000 0.03265 0.01725 0.02915 0.00055 0.00660 0.00048 0.02632 0.00236 0.00034 0.00008 0.00012 0.00000 0.00082 0.00070 0.00078 0.00056 0.00060 0.00056 0.00036 O3 0.55450 0.06320 0.19360 1.00000 0.04089 0.01801 0.03150 -0.00130 0.01007 0.00213 0.03009 0.00255 0.00036 0.00008 0.00012 0.00000 0.00090 0.00072 0.00083 0.00058 0.00066 0.00060 0.00039 H3A 0.49460 0.02840 0.24371 1.00000 0.04513 0.00000 0.00000 O4 0.20379 0.38632 0.29706 1.00000 0.03568 0.01554 0.02945 0.00242 0.00669 0.00122 0.02686 0.00247 0.00035 0.00008 0.00012 0.00000 0.00082 0.00070 0.00077 0.00055 0.00062 0.00056 0.00037 Final Structure Factor Calculation for 07ch0001 in P2(1)/c Total number of l.s. parameters = 112 Maximum vector length = 511 Memory required = 1429 / 21973 wR2 = 0.1333 before cycle 8 for 1690 data and 0 / 112 parameters GooF = S = 1.022; Restrained GooF = 1.022 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0635 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0511 for 1165 Fo > 4sig(Fo) and 0.0840 for all 1690 data wR2 = 0.1333, GooF = S = 1.022, Restrained GooF = 1.022 for all data Occupancy sum of asymmetric unit = 12.00 for non-hydrogen and 8.00 for hydrogen atoms Principal mean square atomic displacements U 0.0246 0.0197 0.0155 C1 0.0254 0.0228 0.0173 C2 0.0281 0.0247 0.0206 C3 0.0274 0.0243 0.0175 C4 0.0272 0.0206 0.0164 C5 0.0243 0.0208 0.0192 C6 0.0240 0.0228 0.0173 C7 0.0340 0.0265 0.0214 C8 0.0425 0.0214 0.0169 O1 0.0375 0.0242 0.0172 O2 0.0470 0.0259 0.0173 O3 0.0399 0.0255 0.0151 O4 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.017 0.025 0.036 0.049 0.064 0.085 0.117 0.176 1.000 Number in group 172. 186. 150. 180. 168. 159. 169. 169. 167. 170. GooF 0.929 0.935 1.003 1.106 1.081 1.084 1.021 1.032 0.986 1.036 K 1.764 1.354 0.903 0.996 0.966 0.957 0.986 1.005 1.027 1.001 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.64 inf Number in group 176. 164. 168. 168. 169. 169. 170. 171. 166. 169. GooF 0.886 1.055 0.987 1.093 1.031 0.992 0.977 0.944 0.959 1.260 K 0.987 1.061 1.028 1.034 0.995 1.015 1.036 1.034 1.038 0.969 R1 0.231 0.215 0.171 0.151 0.102 0.080 0.052 0.045 0.037 0.037 Recommended weighting scheme: WGHT 0.0632 0.2426 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) -1 1 6 156.23 113.62 4.14 0.105 1.72 0 5 1 16.94 9.17 3.66 0.030 3.10 -1 2 2 18.78 11.79 3.22 0.034 3.04 -1 0 6 180.76 139.78 3.19 0.117 1.73 1 13 8 21.92 41.70 3.19 0.064 0.91 1 2 14 25.53 52.49 3.18 0.072 0.80 -2 15 1 22.67 11.04 2.94 0.033 0.94 4 2 7 48.51 86.50 2.90 0.092 0.84 -1 2 9 3.39 8.90 2.84 0.029 1.21 -2 13 6 23.75 37.22 2.82 0.060 0.92 -1 14 8 12.83 1.31 2.81 0.011 0.88 -1 2 10 9.65 3.39 2.80 0.018 1.10 -2 2 9 31.72 44.40 2.75 0.066 1.07 -3 2 4 15.59 26.81 2.72 0.051 1.19 0 20 2 -0.04 13.92 2.69 0.037 0.80 -1 3 5 53.66 41.19 2.64 0.063 1.87 -3 6 11 12.63 1.16 2.62 0.011 0.79 -3 11 6 10.69 0.21 2.61 0.005 0.88 0 4 1 360.39 436.40 2.61 0.206 3.80 -2 2 7 78.07 61.94 2.54 0.078 1.26 -3 14 1 151.30 113.93 2.53 0.105 0.87 -1 5 9 27.32 18.47 2.51 0.042 1.14 -3 10 9 305.00 225.49 2.49 0.148 0.80 -3 3 10 11.68 22.83 2.45 0.047 0.86 -2 16 5 34.09 9.70 2.45 0.031 0.84 2 1 13 53.23 23.77 2.44 0.048 0.81 -2 11 7 3.25 17.43 2.43 0.041 0.96 -3 14 6 -5.70 15.87 2.42 0.039 0.79 -3 5 8 29.78 44.73 2.41 0.066 0.94 1 2 2 145.72 176.20 2.41 0.131 3.02 -1 13 2 -0.56 4.51 2.39 0.021 1.16 -4 0 6 21.13 2.43 2.39 0.015 0.89 -1 14 7 0.63 5.60 2.38 0.023 0.92 -3 0 12 2.99 19.31 2.38 0.043 0.78 0 4 0 1266.87 1495.41 2.36 0.382 4.03 -1 3 4 1.61 4.44 2.36 0.021 2.14 -2 16 2 16.10 30.31 2.36 0.054 0.89 2 2 10 13.63 2.54 2.35 0.016 0.99 -2 13 3 39.14 54.11 2.35 0.073 1.02 0 16 6 -4.24 4.52 2.33 0.021 0.89 4 4 1 13.11 6.80 2.33 0.026 0.96 -2 12 8 16.12 6.48 2.33 0.025 0.88 0 2 4 13.37 8.85 2.31 0.029 2.71 2 5 9 6.38 13.99 2.31 0.037 1.02 -1 4 6 76.34 93.70 2.29 0.096 1.59 0 16 9 1.10 11.98 2.28 0.034 0.79 -3 2 7 25.31 33.67 2.28 0.057 1.03 3 8 3 25.22 35.21 2.25 0.059 1.06 0 13 6 12.51 6.28 2.25 0.025 1.04 3 12 7 103.70 67.27 2.24 0.081 0.82 Bond lengths and angles C1 - Distance Angles C2 1.4022 (0.0026) C6 1.4121 (0.0026) 119.75 (0.16) C7 1.4644 (0.0025) 119.80 (0.16) 120.44 (0.16) C1 - C2 C6 C2 - Distance Angles O3 1.3572 (0.0022) C3 1.4000 (0.0027) 116.57 (0.16) C1 1.4022 (0.0026) 124.46 (0.17) 118.97 (0.17) C2 - O3 C3 C3 - Distance Angles C4 1.3690 (0.0028) C2 1.4000 (0.0027) 120.57 (0.17) H3 0.9500 119.71 119.71 C3 - C4 C2 C4 - Distance Angles C3 1.3690 (0.0028) C5 1.3941 (0.0026) 121.01 (0.17) H4 0.9500 119.50 119.50 C4 - C3 C5 C5 - Distance Angles O4 1.3740 (0.0022) C6 1.3794 (0.0026) 125.34 (0.16) C4 1.3941 (0.0026) 115.05 (0.16) 119.61 (0.17) C5 - O4 C6 C6 - Distance Angles C5 1.3794 (0.0026) C1 1.4121 (0.0026) 120.08 (0.17) H6 0.9500 119.96 119.96 C6 - C5 C1 C7 - Distance Angles O2 1.2412 (0.0022) O1 1.3197 (0.0021) 122.00 (0.16) C1 1.4644 (0.0025) 122.89 (0.16) 115.11 (0.15) C7 - O2 O1 C8 - Distance Angles O4 1.4263 (0.0023) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - O4 H8A H8B O1 - Distance Angles C7 1.3197 (0.0021) H1 0.8400 109.47 O1 - C7 O2 - Distance Angles C7 1.2412 (0.0022) O2 - O3 - Distance Angles C2 1.3572 (0.0022) H3A 0.8400 109.47 O3 - C2 O4 - Distance Angles C5 1.3740 (0.0022) C8 1.4263 (0.0023) 117.10 (0.15) O4 - C5 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.80 2.6414(18) 173.9 O1-H1...O2_$1 0.84 1.92 2.6464(18) 143.3 O3-H3A...O2 FMAP and GRID set by program FMAP 2 1 12 GRID -5.556 24 -2 5.556 1 2 R1 = 0.0840 for 1690 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.23 at -0.0061 0.2571 0.4599 [ 0.51 A from H6 ] Deepest hole -0.25 at 0.3554 0.3479 0.2539 [ 0.84 A from C5 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 1866 / 20055 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.0061 0.2571 0.4599 1.00000 0.05 0.23 0.51 H6 1.46 C6 2.09 H3 2.23 H8A Q2 1 0.5701 0.1738 0.2009 1.00000 0.05 0.23 0.76 C3 0.77 C2 1.43 H3 1.78 O3 Q3 1 0.5470 -0.0556 0.3807 1.00000 0.05 0.22 1.67 O2 1.87 H4 2.09 H3A 2.13 H1 Q4 1 0.3187 -0.0664 0.3329 1.00000 0.05 0.21 1.48 O2 1.83 H4 1.86 H1 1.97 H3A Q5 1 0.4005 0.1732 0.1664 1.00000 0.05 0.20 0.80 C3 0.89 C2 1.47 H3 1.84 C4 Shortest distances between peaks (including symmetry equivalents) 2 5 0.78 3 4 1.07 Time profile in seconds ----------------------- 0.05: 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. 0.39: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.01: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.36: Structure factors and derivatives 0.39: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.04: Apply other restraints 0.09: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.01: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 07ch0001 finished at 14:41:42 Total CPU time: 1.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++