+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + ssg0301 started at 16:51:14 on 25-Oct-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL ssg0301 in P2(1)2(1)2(1) CELL 0.71073 7.7110 8.2850 13.8440 90.000 90.000 90.000 ZERR 4.00 0.0002 0.0004 0.0005 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 N O UNIT 32 40 8 16 V = 884.43 F(000) = 416.0 Mu = 0.12 mm-1 Cell Wt = 792.72 Rho = 1.488 MERG 4 OMIT 2 0 6 SHEL 7 0.77 EQIV_$1 x-1, y, z HTAB O1B O4A_$1 FMAP 2 PLAN 10 SIZE 0.10 0.10 0.14 ACTA BOND $H WGHT 0.06930 1.16260 L.S. 4 TEMP -153.00 FVAR 0.83669 C1 1 -0.434935 0.156478 0.838581 11.00000 0.03500 0.02761 = 0.02573 0.00130 -0.00081 0.00325 C2 1 -0.247348 0.161234 0.804196 11.00000 0.03363 0.02496 = 0.02106 0.00045 -0.00374 0.00154 AFIX 23 H2A 2 -0.223955 0.266568 0.773047 11.00000 -1.20000 H2B 2 -0.228754 0.075516 0.755461 11.00000 -1.20000 AFIX 0 C3 1 -0.121728 0.136964 0.887995 11.00000 0.03465 0.01673 = 0.02033 0.00153 -0.00025 -0.00012 AFIX 13 H3 2 -0.144783 0.222104 0.937559 11.00000 -1.20000 AFIX 0 C4 1 0.066531 0.157058 0.851322 11.00000 0.02797 0.02897 = 0.02054 0.00033 -0.00054 -0.00454 C22 1 -0.151193 -0.162366 0.887108 11.00000 0.03567 0.02188 = 0.02222 -0.00058 0.00551 -0.00238 AFIX 43 H22 2 -0.133349 -0.176988 0.819776 11.00000 -1.20000 AFIX 0 C24 1 -0.181143 -0.049108 1.029335 11.00000 0.06853 0.02198 = 0.02032 -0.00085 0.00452 -0.00598 AFIX 43 H24 2 -0.189275 0.030274 1.078646 11.00000 -1.20000 AFIX 0 C25 1 -0.196807 -0.210108 1.040289 11.00000 0.07241 0.02220 = 0.02065 0.00104 0.00354 -0.00060 AFIX 43 H25 2 -0.215846 -0.265886 1.099300 11.00000 -1.20000 AFIX 0 C26 1 -0.189005 -0.451555 0.927523 11.00000 0.05923 0.01764 = 0.03305 -0.00110 0.00498 0.00036 AFIX 137 H26A 2 -0.310594 -0.485807 0.925454 11.00000 -1.50000 H26B 2 -0.127469 -0.513017 0.977356 11.00000 -1.50000 H26C 2 -0.134870 -0.471240 0.864570 11.00000 -1.50000 AFIX 0 N21 3 -0.180145 -0.278828 0.950257 11.00000 0.03952 0.01708 = 0.02317 -0.00060 0.00601 -0.00129 N23 3 -0.151057 -0.022342 0.932681 11.00000 0.03160 0.01724 = 0.01969 -0.00040 0.00205 -0.00027 O1A 4 -0.476615 0.211346 0.916264 11.00000 0.04026 0.04008 = 0.02945 -0.00404 0.00487 0.00494 O1B 4 -0.539095 0.083505 0.776729 11.00000 0.03420 0.05096 = 0.04044 -0.01073 0.00216 -0.00279 AFIX 147 H1 2 -0.628046 0.050863 0.805802 11.00000 -1.50000 AFIX 0 O4A 4 0.157937 0.032843 0.843259 11.00000 0.03229 0.03172 = 0.04049 0.00295 0.00231 -0.00195 O4B 4 0.106537 0.297617 0.828947 11.00000 0.04098 0.02902 = 0.02663 0.00470 0.00339 -0.00741 HKLF 4 Covalent radii and connectivity table for ssg0301 in P2(1)2(1)2(1) C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1A O1B C2 C2 - C1 C3 C3 - N23 C2 C4 C4 - O4B O4A C3 C22 - N23 N21 C24 - C25 N23 C25 - C24 N21 C26 - N21 N21 - C22 C25 C26 N23 - C22 C24 C3 O1A - C1 O1B - C1 O4A - C4 O4B - C4 Operators for generating equivalent atoms: $1 x-1, y, z h k l Fo^2 Sigma Why rejected 3 0 0 4.05 0.73 observed but should be systematically absent 3 0 0 5.26 0.82 observed but should be systematically absent 0 3 0 3.74 0.68 observed but should be systematically absent 0 3 0 2.99 0.66 observed but should be systematically absent 0 3 0 3.43 0.47 observed but should be systematically absent 0 0 3 4.39 0.61 observed but should be systematically absent 0 0 3 3.22 0.61 observed but should be systematically absent 0 0 3 3.94 0.56 observed but should be systematically absent 0 0 5 3.73 0.64 observed but should be systematically absent 0 0 5 2.80 0.63 observed but should be systematically absent 0 0 5 3.15 0.57 observed but should be systematically absent 0 0 7 2.90 0.60 observed but should be systematically absent 9405 Reflections read, of which 1808 rejected -9 =< h =< 10, -10 =< k =< 10, -17 =< l =< 17, Max. 2-theta = 54.97 12 Systematic absence violations 0 Inconsistent equivalents 1145 Unique reflections, of which 0 suppressed R(int) = 0.0556 R(sigma) = 0.0335 Friedel opposites merged Maximum memory for data reduction = 1429 / 11252 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 = 1783 / 163476 wR2 = 0.1730 before cycle 1 for 1145 data and 129 / 129 parameters GooF = S = 1.158; Restrained GooF = 1.158 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0693 * P )^2 + 1.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.83668 0.00532 -0.002 OSF Mean shift/esd = 0.002 Maximum = -0.008 for tors H1 Max. shift = 0.001 A for H1 Max. dU = 0.000 for O1A Least-squares cycle 2 Maximum vector length = 511 Memory required = 1783 / 163476 wR2 = 0.1730 before cycle 2 for 1145 data and 129 / 129 parameters GooF = S = 1.158; Restrained GooF = 1.158 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0693 * P )^2 + 1.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.83666 0.00532 -0.003 OSF Mean shift/esd = 0.001 Maximum = -0.006 for tors H1 Max. shift = 0.000 A for H1 Max. dU = 0.000 for O1A Least-squares cycle 3 Maximum vector length = 511 Memory required = 1783 / 163476 wR2 = 0.1730 before cycle 3 for 1145 data and 129 / 129 parameters GooF = S = 1.158; Restrained GooF = 1.158 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0693 * P )^2 + 1.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.83666 0.00532 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.003 for tors H1 Max. shift = 0.000 A for H1 Max. dU = 0.000 for O1B Least-squares cycle 4 Maximum vector length = 511 Memory required = 1783 / 163476 wR2 = 0.1730 before cycle 4 for 1145 data and 129 / 129 parameters GooF = S = 1.158; Restrained GooF = 1.158 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0693 * P )^2 + 1.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.83666 0.00532 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.002 for tors H1 Max. shift = 0.000 A for H1 Max. dU = 0.000 for O1B 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 H2A -0.2240 0.2666 0.7730 23 0.990 0.000 C2 C1 C3 H2B -0.2288 0.0755 0.7555 23 0.990 0.000 C2 C1 C3 H3 -0.1448 0.2221 0.9376 13 1.000 0.000 C3 N23 C2 C4 H22 -0.1333 -0.1770 0.8198 43 0.950 0.000 C22 N23 N21 H24 -0.1893 0.0303 1.0786 43 0.950 0.000 C24 C25 N23 H25 -0.2159 -0.2659 1.0993 43 0.950 0.000 C25 C24 N21 H26A -0.3106 -0.4858 0.9254 137 0.980 0.000 C26 N21 H26A H26B -0.1275 -0.5130 0.9774 137 0.980 0.000 C26 N21 H26A H26C -0.1348 -0.4712 0.8646 137 0.980 0.000 C26 N21 H26A H1 -0.6280 0.0507 0.8058 147 0.840 0.000 O1B C1 H1 ssg0301 in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.43494 0.15648 0.83858 1.00000 0.03498 0.02761 0.02573 0.00130 -0.00081 0.00325 0.02944 0.00757 0.00057 0.00051 0.00029 0.00000 0.00203 0.00183 0.00176 0.00172 0.00163 0.00173 0.00086 C2 -0.24735 0.16123 0.80420 1.00000 0.03363 0.02496 0.02105 0.00046 -0.00374 0.00155 0.02655 0.00701 0.00056 0.00051 0.00027 0.00000 0.00198 0.00175 0.00161 0.00150 0.00146 0.00167 0.00081 H2A -0.22396 0.26657 0.77305 1.00000 0.03186 0.00000 0.00000 H2B -0.22875 0.07551 0.75546 1.00000 0.03186 0.00000 0.00000 C3 -0.12173 0.13696 0.88800 1.00000 0.03464 0.01674 0.02033 0.00153 -0.00024 -0.00012 0.02390 0.00668 0.00054 0.00044 0.00026 0.00000 0.00205 0.00155 0.00157 0.00134 0.00149 0.00153 0.00081 H3 -0.14478 0.22210 0.93756 1.00000 0.02868 0.00000 0.00000 C4 0.06653 0.15706 0.85132 1.00000 0.02797 0.02897 0.02053 0.00034 -0.00053 -0.00454 0.02582 0.00686 0.00052 0.00051 0.00027 0.00000 0.00180 0.00184 0.00162 0.00155 0.00146 0.00164 0.00080 C22 -0.15119 -0.16237 0.88711 1.00000 0.03566 0.02187 0.02222 -0.00058 0.00551 -0.00238 0.02658 0.00683 0.00056 0.00045 0.00026 0.00000 0.00206 0.00166 0.00165 0.00141 0.00159 0.00171 0.00083 H22 -0.13335 -0.17699 0.81978 1.00000 0.03190 0.00000 0.00000 C24 -0.18114 -0.04911 1.02934 1.00000 0.06853 0.02198 0.02032 -0.00084 0.00452 -0.00598 0.03694 0.00805 0.00076 0.00050 0.00029 0.00000 0.00322 0.00184 0.00175 0.00147 0.00207 0.00210 0.00111 H24 -0.18928 0.03028 1.07865 1.00000 0.04433 0.00000 0.00000 C25 -0.19681 -0.21011 1.04029 1.00000 0.07241 0.02220 0.02064 0.00104 0.00354 -0.00060 0.03842 0.00868 0.00078 0.00054 0.00030 0.00000 0.00336 0.00188 0.00177 0.00149 0.00208 0.00225 0.00115 H25 -0.21585 -0.26589 1.09930 1.00000 0.04610 0.00000 0.00000 C26 -0.18901 -0.45155 0.92752 1.00000 0.05922 0.01764 0.03305 -0.00111 0.00498 0.00036 0.03663 0.00839 0.00074 0.00047 0.00033 0.00000 0.00291 0.00176 0.00200 0.00160 0.00219 0.00191 0.00105 H26A -0.31060 -0.48580 0.92543 1.00000 0.05495 0.00000 0.00000 H26B -0.12751 -0.51302 0.97737 1.00000 0.05495 0.00000 0.00000 H26C -0.13483 -0.47125 0.86458 1.00000 0.05495 0.00000 0.00000 N21 -0.18015 -0.27883 0.95026 1.00000 0.03951 0.01708 0.02317 -0.00061 0.00601 -0.00129 0.02659 0.00608 0.00050 0.00040 0.00024 0.00000 0.00183 0.00143 0.00153 0.00117 0.00140 0.00148 0.00075 N23 -0.15106 -0.02234 0.93268 1.00000 0.03160 0.01725 0.01968 -0.00040 0.00205 -0.00027 0.02284 0.00551 0.00046 0.00036 0.00022 0.00000 0.00161 0.00136 0.00137 0.00110 0.00133 0.00132 0.00069 O1A -0.47662 0.21135 0.91626 1.00000 0.04025 0.04008 0.02944 -0.00404 0.00487 0.00494 0.03659 0.00577 0.00044 0.00040 0.00022 0.00000 0.00167 0.00163 0.00145 0.00131 0.00131 0.00152 0.00077 O1B -0.53910 0.08350 0.77673 1.00000 0.03420 0.05094 0.04043 -0.01073 0.00216 -0.00280 0.04186 0.00575 0.00044 0.00045 0.00024 0.00000 0.00174 0.00193 0.00170 0.00159 0.00144 0.00157 0.00087 H1 -0.62797 0.05072 0.80582 1.00000 0.06279 0.00000 0.00000 O4A 0.15794 0.03284 0.84326 1.00000 0.03228 0.03172 0.04049 0.00295 0.00231 -0.00195 0.03483 0.00546 0.00041 0.00037 0.00023 0.00000 0.00151 0.00153 0.00158 0.00131 0.00138 0.00134 0.00074 O4B 0.10654 0.29762 0.82895 1.00000 0.04097 0.02902 0.02663 0.00470 0.00339 -0.00741 0.03221 0.00533 0.00041 0.00036 0.00021 0.00000 0.00167 0.00147 0.00134 0.00117 0.00131 0.00133 0.00075 Final Structure Factor Calculation for ssg0301 in P2(1)2(1)2(1) Total number of l.s. parameters = 129 Maximum vector length = 511 Memory required = 1656 / 25046 wR2 = 0.1730 before cycle 5 for 1145 data and 2 / 129 parameters GooF = S = 1.158; Restrained GooF = 1.158 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0693 * P )^2 + 1.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0627 for 1118 Fo > 4sig(Fo) and 0.0637 for all 1145 data wR2 = 0.1730, GooF = S = 1.158, Restrained GooF = 1.158 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 14.00 for non-hydrogen and 10.00 for hydrogen atoms Principal mean square atomic displacements U 0.0362 0.0276 0.0245 C1 0.0348 0.0249 0.0199 C2 0.0346 0.0209 0.0162 C3 0.0331 0.0239 0.0205 C4 0.0380 0.0216 0.0202 C22 0.0697 0.0213 0.0198 C24 0.0727 0.0227 0.0199 C25 0.0601 0.0322 0.0175 C26 0.0416 0.0212 0.0170 N21 0.0319 0.0194 0.0172 N23 0.0451 0.0392 0.0254 O1A 0.0581 0.0341 0.0334 O1B 0.0417 0.0340 0.0288 O4A 0.0446 0.0317 0.0203 O4B Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.049 0.079 0.107 0.135 0.167 0.200 0.254 0.331 0.462 1.000 Number in group 115. 115. 114. 116. 113. 117. 112. 114. 114. 115. GooF 1.722 1.405 1.095 0.843 0.919 1.062 1.064 1.007 1.079 1.127 K 2.638 1.433 1.169 1.090 1.047 1.033 0.983 1.004 0.989 0.998 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.30 1.58 inf Number in group 117. 113. 114. 117. 111. 117. 114. 113. 114. 115. GooF 0.817 1.126 0.766 0.937 0.819 0.952 1.176 1.474 1.172 1.875 K 1.066 1.071 1.023 1.009 1.009 0.985 0.958 0.984 1.000 1.043 R1 0.092 0.101 0.070 0.074 0.058 0.055 0.052 0.059 0.051 0.068 Recommended weighting scheme: WGHT 0.0693 1.1610 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) 6 0 4 30.63 1.76 5.99 0.037 1.20 3 1 0 73.38 25.15 5.67 0.140 2.45 6 0 1 47.17 12.02 5.28 0.097 1.28 7 0 11 14.45 0.10 4.90 0.009 0.83 6 0 3 31.96 7.14 4.89 0.075 1.24 8 2 8 12.27 0.16 4.66 0.011 0.83 7 2 0 19.46 2.72 4.59 0.046 1.06 0 2 2 19.40 3.34 4.44 0.051 3.55 1 2 1 9.85 39.12 4.33 0.175 3.53 5 4 5 15.51 1.58 4.18 0.035 1.13 4 5 1 36.03 12.43 4.16 0.098 1.25 4 6 5 24.24 6.43 4.06 0.071 1.04 3 0 2 92.67 49.67 3.92 0.197 2.41 4 0 2 219.87 92.71 3.72 0.269 1.86 5 0 7 12.94 0.54 3.67 0.021 1.22 3 0 8 17.18 3.89 3.64 0.055 1.44 8 0 9 10.57 0.55 3.37 0.021 0.82 4 1 3 99.84 60.99 3.30 0.218 1.74 1 2 5 97.47 60.01 3.22 0.216 2.21 0 0 6 38.67 18.53 3.08 0.120 2.31 0 4 4 115.54 74.48 3.07 0.241 1.78 1 4 0 343.90 252.34 2.98 0.443 2.00 7 0 9 15.81 4.85 2.93 0.061 0.90 2 4 6 75.10 46.60 2.86 0.190 1.43 6 7 0 6.39 0.45 2.86 0.019 0.87 0 2 4 222.77 304.16 2.78 0.487 2.66 0 3 3 149.88 211.42 2.78 0.406 2.37 8 5 5 12.07 3.37 2.74 0.051 0.80 5 8 0 9.43 1.24 2.67 0.031 0.86 8 0 3 6.06 0.61 2.67 0.022 0.94 4 6 2 12.10 4.01 2.55 0.056 1.11 0 2 5 235.29 177.47 2.50 0.372 2.30 7 3 2 37.55 21.40 2.46 0.129 1.01 1 3 3 129.49 94.27 2.38 0.271 2.27 4 0 8 17.28 7.58 2.35 0.077 1.29 0 1 10 11.58 4.16 2.35 0.057 1.37 9 1 5 6.29 1.35 2.29 0.032 0.81 6 6 5 12.22 4.80 2.22 0.061 0.89 4 0 3 132.16 98.18 2.21 0.277 1.78 0 1 6 327.19 260.45 2.18 0.450 2.22 2 4 2 68.82 47.60 2.17 0.193 1.76 0 2 7 172.26 131.89 2.17 0.320 1.78 7 1 3 46.70 30.15 2.15 0.153 1.06 2 4 7 219.09 172.07 2.11 0.366 1.34 5 3 1 55.01 78.85 2.10 0.248 1.34 5 0 4 334.08 412.78 2.04 0.567 1.41 2 2 2 167.75 213.72 2.03 0.408 2.61 1 5 2 64.40 45.28 2.02 0.188 1.58 1 5 1 552.28 458.65 2.01 0.598 1.61 2 2 8 36.44 54.50 2.00 0.206 1.48 Bond lengths and angles C1 - Distance Angles O1A 1.2110 (0.0051) O1B 1.3205 (0.0053) 125.90 (0.42) C2 1.5233 (0.0060) 121.32 (0.39) 112.75 (0.34) C1 - O1A O1B C2 - Distance Angles C1 1.5233 (0.0060) C3 1.5247 (0.0052) 111.23 (0.31) H2A 0.9900 109.39 109.39 H2B 0.9900 109.39 109.39 108.01 C2 - C1 C3 H2A C3 - Distance Angles N23 1.4751 (0.0044) C2 1.5247 (0.0052) 109.86 (0.32) C4 1.5469 (0.0055) 112.20 (0.32) 109.41 (0.30) H3 1.0000 108.43 108.43 108.43 C3 - N23 C2 C4 C4 - Distance Angles O4B 1.2439 (0.0050) O4A 1.2523 (0.0052) 127.41 (0.38) C3 1.5469 (0.0055) 114.53 (0.36) 117.97 (0.36) C4 - O4B O4A C22 - Distance Angles N23 1.3206 (0.0046) N21 1.3210 (0.0049) 109.00 (0.32) H22 0.9500 125.50 125.50 C22 - N23 N21 C24 - Distance Angles C25 1.3479 (0.0060) N23 1.3760 (0.0050) 106.50 (0.36) H24 0.9500 126.75 126.75 C24 - C25 N23 C25 - Distance Angles C24 1.3479 (0.0060) N21 1.3763 (0.0046) 107.40 (0.35) H25 0.9500 126.30 126.30 C25 - C24 N21 C26 - Distance Angles N21 1.4668 (0.0049) H26A 0.9800 109.47 H26B 0.9800 109.47 109.47 H26C 0.9800 109.47 109.47 109.47 C26 - N21 H26A H26B N21 - Distance Angles C22 1.3210 (0.0049) C25 1.3763 (0.0046) 108.24 (0.31) C26 1.4668 (0.0049) 125.34 (0.35) 126.41 (0.33) N21 - C22 C25 N23 - Distance Angles C22 1.3206 (0.0046) C24 1.3760 (0.0050) 108.84 (0.31) C3 1.4751 (0.0044) 125.86 (0.29) 125.30 (0.31) N23 - C22 C24 O1A - Distance Angles C1 1.2110 (0.0051) O1A - O1B - Distance Angles C1 1.3205 (0.0053) H1 0.8400 109.47 O1B - C1 O4A - Distance Angles C4 1.2523 (0.0053) O4A - O4B - Distance Angles C4 1.2439 (0.0050) O4B - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.74 2.546(5) 161.1 O1B-H1...O4A_$1 FMAP and GRID set by program FMAP 2 1 12 GRID -2.778 -2 -2 2.778 2 2 R1 = 0.0637 for 1145 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.43 at 0.0206 0.7875 0.2648 [ 1.09 A from O1B ] Deepest hole -0.23 at 0.1435 0.1457 0.7999 [ 0.93 A from C4 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 1828 / 15699 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.5206 0.2125 0.7648 1.00000 0.05 0.43 1.09 O1B 1.30 C1 1.67 H1 2.12 O1A Q2 1 -0.0876 -0.4882 0.9210 1.00000 0.05 0.32 0.84 C26 0.86 H26B 0.87 H26C 1.72 H26A Q3 1 0.2140 0.2809 0.8317 1.00000 0.05 0.31 0.84 O4B 1.56 C4 2.11 O4A 2.13 H24 Q4 1 -0.0766 -0.2816 0.9509 1.00000 0.05 0.25 0.80 N21 1.44 C22 1.66 C25 1.68 C26 Q5 1 -0.0875 -0.2265 1.0423 1.00000 0.05 0.23 0.85 C25 1.31 H25 1.52 N21 1.65 C24 Q6 1 -0.5968 0.1663 0.8726 1.00000 0.05 0.23 1.17 O1A 1.34 C1 1.35 H1 1.56 O1B Q7 1 -0.1685 -0.0372 0.9749 1.00000 0.05 0.22 0.61 N23 0.77 C24 1.55 H24 1.60 C22 Q8 1 -0.2310 0.1264 0.6591 1.00000 0.05 0.21 1.40 H2B 1.48 H25 1.82 H24 1.87 C25 Q9 1 0.0504 -0.0163 0.8497 1.00000 0.05 0.21 0.93 O4A 1.44 C4 1.91 C3 1.93 N23 Q10 1 -0.4485 0.3622 0.8065 1.00000 0.05 0.21 1.76 C1 1.96 H2A 1.98 O1A 2.17 O1B Shortest distances between peaks (including symmetry equivalents) 4 5 1.35 1 10 1.48 1 6 1.65 2 4 1.76 3 6 1.83 5 7 1.93 4 7 2.17 6 10 2.19 5 8 2.29 1 3 2.32 7 9 2.43 3 10 2.71 2 5 2.74 1 8 2.76 7 8 2.77 3 9 2.78 4 9 2.78 2 8 2.86 3 8 2.87 4 8 2.92 Time profile in seconds ----------------------- 0.08: 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. 0.44: 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 0.30: Structure factors and derivatives 0.11: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.06: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.02: Analysis of variance 0.00: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + ssg0301 finished at 16:51:15 Total CPU time: 1.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++