+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0037p-1 started at 12:44:35 on 23-Jan-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0037p-1 in P-1 CELL 0.71073 5.8219 7.4643 9.8058 79.046 77.621 81.676 ZERR 1.00 0.0003 0.0006 0.0007 0.003 0.004 0.004 LATT 1 SFAC C H N O UNIT 14 28 2 6 V = 406.22 F(000) = 174.0 Mu = 0.10 mm-1 Cell Wt = 320.38 Rho = 1.310 MERG 2 OMIT -3.00 55.00 OMIT 2 -3 1 OMIT -1 4 1 OMIT 1 -4 2 OMIT 1 3 3 OMIT 2 -3 3 EXTI 0.12518 SHEL 7 0.77 HTAB N21 O1B EQIV_$1 x-1, y, z HTAB N21 O1A_$1 HTAB N21 O1B_$1 EQIV_$2 -x+1, -y-1, -z+1 MPLA C1 O1A O1B MPLA C1_$2 O1A_$2 O1B_$2 FMAP 2 PLAN 10 SIZE 0.04 0.06 0.12 ACTA BOND $H WGHT 0.11980 3.87210 L.S. 4 TEMP -153.00 FVAR 1.63616 MOLE 1 C1 1 0.696313 -0.123135 0.329050 11.00000 0.02251 0.01441 = 0.02125 -0.00294 -0.00345 -0.00466 C2 1 0.512764 -0.239110 0.426319 11.00000 0.01559 0.02012 = 0.02842 0.00174 -0.00427 -0.00435 AFIX 23 H2A 2 0.471927 -0.196948 0.519233 11.00000 -1.20000 H2B 2 0.367429 -0.217854 0.385816 11.00000 -1.20000 AFIX 0 C3 1 0.591022 -0.443526 0.449693 11.00000 0.01570 0.01737 = 0.02190 -0.00274 -0.00287 -0.00120 AFIX 23 H3A 2 0.738900 -0.464843 0.487633 11.00000 -1.20000 H3B 2 0.626822 -0.486829 0.357270 11.00000 -1.20000 AFIX 0 O1A 4 0.909179 -0.170434 0.339643 11.00000 0.01775 0.02369 = 0.03839 0.00795 -0.00770 -0.00604 O1B 4 0.628890 0.013979 0.245095 11.00000 0.02291 0.02039 = 0.02554 0.00265 -0.00217 -0.00353 MOLE 2 C23 1 0.294073 0.329958 0.001068 11.00000 0.02970 0.02417 = 0.02358 -0.00046 -0.00129 -0.00753 AFIX 23 H23A 2 0.463323 0.296183 0.005857 11.00000 -1.20000 H23B 2 0.282584 0.372208 -0.099483 11.00000 -1.20000 AFIX 0 C22 1 0.161251 0.163260 0.058591 11.00000 0.02788 0.01970 = 0.02077 -0.00500 -0.00724 -0.00420 AFIX 23 H22A 2 -0.005808 0.194129 0.047822 11.00000 -1.20000 H22B 2 0.232213 0.063009 0.004434 11.00000 -1.20000 AFIX 0 C26 1 0.081644 0.255445 0.291158 11.00000 0.02659 0.02772 = 0.01883 -0.00572 -0.00427 -0.00394 AFIX 23 H26A 2 0.100518 0.216495 0.390800 11.00000 -1.20000 H26B 2 -0.088821 0.289926 0.290279 11.00000 -1.20000 AFIX 0 C25 1 0.217520 0.419311 0.224537 11.00000 0.03217 0.02328 = 0.02528 -0.00279 -0.01003 -0.00229 AFIX 23 H25A 2 0.153001 0.522909 0.276307 11.00000 -1.20000 H25B 2 0.385739 0.387100 0.232413 11.00000 -1.20000 AFIX 0 N21 3 0.172140 0.101507 0.210739 11.00000 0.01568 0.01904 = 0.02186 -0.00130 -0.00265 -0.00386 AFIX 23 H21A 2 0.082522 0.005292 0.247029 11.00000 -1.20000 H21B 2 0.325954 0.061167 0.219816 11.00000 -1.20000 AFIX 0 O24 4 0.201249 0.474251 0.079027 11.00000 0.03842 0.01929 = 0.03086 0.00249 -0.01464 -0.00575 HKLF 4 Covalent radii and connectivity table for 06skc0037p-1 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1B O1A C2 C2 - C3 C1 C3 - C2 C3_$2 O1A - C1 O1B - C1 C23 - O24 C22 C22 - N21 C23 C26 - N21 C25 C25 - O24 C26 N21 - C26 C22 O24 - C23 C25 Operators for generating equivalent atoms: $1 x-1, y, z $2 -x+1, -y-1, -z+1 7640 Reflections read, of which 64 rejected -7 =< h =< 7, -9 =< k =< 9, -12 =< l =< 12, Max. 2-theta = 54.96 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 3 -4 2 75.72 14.48 2 114.14 2 -1 2 384.57 16.90 5 104.09 0 -3 3 178.71 13.02 5 104.23 3 Inconsistent equivalents 1859 Unique reflections, of which 0 suppressed R(int) = 0.1083 R(sigma) = 0.1023 Friedel opposites merged Maximum memory for data reduction = 1620 / 18498 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 = 1922 / 131570 wR2 = 0.3776 before cycle 1 for 1859 data and 101 / 101 parameters GooF = S = 1.117; Restrained GooF = 1.117 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1198 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.63626 0.01888 0.005 OSF 2 0.12533 0.03806 0.004 EXTI Mean shift/esd = 0.001 Maximum = 0.005 for OSF Max. shift = 0.000 A for C3 Max. dU = 0.000 for O1B Least-squares cycle 2 Maximum vector length = 511 Memory required = 1922 / 131570 wR2 = 0.3776 before cycle 2 for 1859 data and 101 / 101 parameters GooF = S = 1.117; Restrained GooF = 1.117 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1198 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.63629 0.01888 0.001 OSF 2 0.12539 0.03808 0.002 EXTI Mean shift/esd = 0.000 Maximum = 0.002 for EXTI Max. shift = 0.000 A for C3 Max. dU = 0.000 for O1B Least-squares cycle 3 Maximum vector length = 511 Memory required = 1922 / 131570 wR2 = 0.3776 before cycle 3 for 1859 data and 101 / 101 parameters GooF = S = 1.117; Restrained GooF = 1.117 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1198 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.63629 0.01888 0.000 OSF 2 0.12539 0.03809 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for U22 O1B Max. shift = 0.000 A for H25A Max. dU = 0.000 for O1B Least-squares cycle 4 Maximum vector length = 511 Memory required = 1922 / 131570 wR2 = 0.3776 before cycle 4 for 1859 data and 101 / 101 parameters GooF = S = 1.117; Restrained GooF = 1.117 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1198 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.63629 0.01888 0.000 OSF 2 0.12540 0.03809 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for U23 O24 Max. shift = 0.000 A for C2 Max. dU = 0.000 for O1B Largest correlation matrix elements 0.605 EXTI / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2A 0.4719 -0.1969 0.5192 23 0.990 0.000 C2 C3 C1 H2B 0.3674 -0.2179 0.3858 23 0.990 0.000 C2 C3 C1 H3A 0.7389 -0.4648 0.4876 23 0.990 0.000 C3 C2 C3_$2 H3B 0.6268 -0.4868 0.3573 23 0.990 0.000 C3 C2 C3_$2 H23A 0.4633 0.2962 0.0059 23 0.990 0.000 C23 O24 C22 H23B 0.2826 0.3722 -0.0995 23 0.990 0.000 C23 O24 C22 H22A -0.0058 0.1941 0.0478 23 0.990 0.000 C22 N21 C23 H22B 0.2322 0.0630 0.0044 23 0.990 0.000 C22 N21 C23 H26A 0.1005 0.2165 0.3908 23 0.990 0.000 C26 N21 C25 H26B -0.0888 0.2899 0.2903 23 0.990 0.000 C26 N21 C25 H25A 0.1530 0.5229 0.2763 23 0.990 0.000 C25 O24 C26 H25B 0.3857 0.3871 0.2324 23 0.990 0.000 C25 O24 C26 H21A 0.0825 0.0053 0.2470 23 0.920 0.000 N21 C26 C22 H21B 0.3260 0.0612 0.2198 23 0.920 0.000 N21 C26 C22 06skc0037p-1 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.69631 -0.12313 0.32905 1.00000 0.02251 0.01442 0.02126 -0.00294 -0.00345 -0.00467 0.01924 0.00843 0.00103 0.00078 0.00062 0.00000 0.00279 0.00267 0.00284 0.00219 0.00222 0.00214 0.00124 C2 0.51276 -0.23911 0.42632 1.00000 0.01559 0.02012 0.02843 0.00174 -0.00427 -0.00435 0.02190 0.00911 0.00099 0.00081 0.00067 0.00000 0.00258 0.00296 0.00320 0.00240 0.00225 0.00217 0.00133 H2A 0.47193 -0.19695 0.51923 1.00000 0.02628 0.00000 0.00000 H2B 0.36743 -0.21785 0.38582 1.00000 0.02628 0.00000 0.00000 C3 0.59102 -0.44353 0.44969 1.00000 0.01569 0.01738 0.02191 -0.00275 -0.00287 -0.00120 0.01857 0.00852 0.00095 0.00077 0.00061 0.00000 0.00255 0.00279 0.00289 0.00226 0.00217 0.00213 0.00125 H3A 0.73890 -0.46485 0.48763 1.00000 0.02228 0.00000 0.00000 H3B 0.62682 -0.48683 0.35727 1.00000 0.02228 0.00000 0.00000 O1A 0.90918 -0.17043 0.33964 1.00000 0.01775 0.02369 0.03839 0.00796 -0.00770 -0.00604 0.02763 0.00689 0.00073 0.00061 0.00050 0.00000 0.00208 0.00232 0.00264 0.00190 0.00182 0.00168 0.00116 O1B 0.62889 0.01398 0.24509 1.00000 0.02292 0.02040 0.02554 0.00265 -0.00217 -0.00353 0.02408 0.00659 0.00074 0.00058 0.00046 0.00000 0.00215 0.00223 0.00230 0.00175 0.00170 0.00169 0.00110 C23 0.29407 0.32996 0.00107 1.00000 0.02970 0.02418 0.02358 -0.00046 -0.00129 -0.00752 0.02640 0.00975 0.00116 0.00087 0.00068 0.00000 0.00320 0.00324 0.00309 0.00250 0.00249 0.00257 0.00143 H23A 0.46332 0.29618 0.00586 1.00000 0.03168 0.00000 0.00000 H23B 0.28258 0.37221 -0.09948 1.00000 0.03168 0.00000 0.00000 C22 0.16125 0.16326 0.05859 1.00000 0.02788 0.01970 0.02078 -0.00500 -0.00724 -0.00420 0.02201 0.00856 0.00110 0.00083 0.00063 0.00000 0.00301 0.00291 0.00295 0.00230 0.00236 0.00235 0.00131 H22A -0.00581 0.19413 0.04782 1.00000 0.02641 0.00000 0.00000 H22B 0.23221 0.06301 0.00443 1.00000 0.02641 0.00000 0.00000 C26 0.08164 0.25545 0.29116 1.00000 0.02659 0.02773 0.01883 -0.00571 -0.00427 -0.00394 0.02405 0.00903 0.00110 0.00089 0.00064 0.00000 0.00306 0.00327 0.00287 0.00237 0.00234 0.00247 0.00135 H26A 0.10052 0.21650 0.39080 1.00000 0.02885 0.00000 0.00000 H26B -0.08882 0.28993 0.29028 1.00000 0.02885 0.00000 0.00000 C25 0.21752 0.41931 0.22454 1.00000 0.03217 0.02328 0.02529 -0.00279 -0.01004 -0.00229 0.02646 0.00943 0.00118 0.00089 0.00067 0.00000 0.00332 0.00319 0.00322 0.00252 0.00260 0.00256 0.00143 H25A 0.15300 0.52291 0.27631 1.00000 0.03175 0.00000 0.00000 H25B 0.38574 0.38710 0.23241 1.00000 0.03175 0.00000 0.00000 N21 0.17214 0.10151 0.21074 1.00000 0.01568 0.01905 0.02186 -0.00130 -0.00265 -0.00386 0.01909 0.00718 0.00083 0.00068 0.00052 0.00000 0.00223 0.00245 0.00251 0.00192 0.00184 0.00181 0.00112 H21A 0.08252 0.00529 0.24703 1.00000 0.02290 0.00000 0.00000 H21B 0.32595 0.06117 0.21982 1.00000 0.02290 0.00000 0.00000 O24 0.20125 0.47425 0.07903 1.00000 0.03843 0.01929 0.03087 0.00249 -0.01464 -0.00575 0.02893 0.00662 0.00084 0.00060 0.00049 0.00000 0.00262 0.00227 0.00253 0.00183 0.00203 0.00187 0.00118 Final Structure Factor Calculation for 06skc0037p-1 in P-1 Total number of l.s. parameters = 101 Maximum vector length = 511 Memory required = 1821 / 22995 wR2 = 0.3776 before cycle 5 for 1859 data and 0 / 101 parameters GooF = S = 1.117; Restrained GooF = 1.117 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1198 * P )^2 + 3.87 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1403 for 1325 Fo > 4sig(Fo) and 0.1755 for all 1859 data wR2 = 0.3776, GooF = S = 1.117, Restrained GooF = 1.117 for all data Occupancy sum of asymmetric unit = 11.00 for non-hydrogen and 14.00 for hydrogen atoms Principal mean square atomic displacements U 0.0234 0.0212 0.0131 C1 0.0326 0.0189 0.0142 C2 0.0225 0.0176 0.0156 C3 0.0486 0.0189 0.0154 O1A 0.0326 0.0233 0.0164 O1B 0.0327 0.0280 0.0185 C23 0.0284 0.0216 0.0160 C22 0.0284 0.0259 0.0178 C26 0.0337 0.0241 0.0216 C25 0.0235 0.0193 0.0145 N21 0.0435 0.0261 0.0172 O24 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.012 0.023 0.033 0.044 0.058 0.072 0.093 0.119 0.167 1.000 Number in group 200. 189. 189. 168. 187. 182. 189. 182. 187. 186. GooF 1.488 1.191 1.136 0.972 0.994 0.984 0.985 0.944 1.280 1.016 K 40.334 3.616 2.811 1.449 1.414 1.338 1.143 1.067 1.108 1.012 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.64 inf Number in group 191. 188. 179. 187. 184. 186. 189. 185. 185. 185. GooF 0.770 0.990 1.039 0.850 0.917 0.986 1.390 1.313 1.296 1.401 K 1.002 1.284 1.249 1.101 1.086 1.076 1.127 1.122 1.122 1.052 R1 0.281 0.290 0.294 0.203 0.188 0.167 0.156 0.138 0.137 0.111 Recommended weighting scheme: WGHT 0.1198 3.8690 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) 2 4 2 130.01 12.83 6.29 0.053 1.66 -1 -1 2 506.67 87.57 6.17 0.140 2.97 1 1 5 421.45 81.28 5.88 0.134 1.94 4 1 5 177.30 36.34 5.81 0.090 1.28 0 7 1 62.31 0.94 5.25 0.014 1.05 -3 -5 3 86.89 0.31 5.22 0.008 1.05 -3 7 0 83.42 4.51 5.17 0.032 0.87 2 2 3 177.62 0.00 5.07 0.000 2.19 -1 4 2 64.27 0.26 4.86 0.008 1.63 -3 2 4 89.91 7.31 4.76 0.040 1.27 3 0 10 99.75 1.76 4.68 0.020 0.92 2 -3 7 186.21 45.52 4.60 0.101 1.07 2 4 4 206.20 68.29 4.47 0.123 1.53 1 3 9 344.32 125.13 4.42 0.167 1.05 2 4 8 47.59 3.77 4.42 0.029 1.10 2 4 3 370.14 166.25 4.20 0.192 1.61 1 6 4 322.93 112.04 4.06 0.158 1.18 4 8 4 54.03 0.01 4.06 0.001 0.83 5 2 3 37.38 0.93 4.05 0.014 1.14 -1 -3 6 41.69 0.20 3.95 0.007 1.18 -1 6 6 68.49 5.04 3.91 0.033 0.99 1 3 7 142.72 30.12 3.85 0.082 1.31 -1 -3 3 87.94 15.56 3.82 0.059 1.69 -2 3 6 99.97 25.04 3.78 0.075 1.17 -1 4 7 271.44 123.07 3.77 0.165 1.10 5 2 5 51.47 3.01 3.73 0.026 1.08 1 -6 1 53.62 2.57 3.73 0.024 1.14 3 3 3 275.86 0.17 3.73 0.006 1.59 -2 1 5 203.24 17.66 3.66 0.063 1.44 5 -3 4 41.27 3.99 3.65 0.030 0.94 -3 0 4 160.13 55.56 3.56 0.111 1.35 -1 -1 3 35.89 1.80 3.49 0.020 2.35 3 0 3 338.70 169.33 3.43 0.194 1.77 -4 1 5 57.31 0.53 3.42 0.011 1.03 2 9 4 87.65 0.59 3.41 0.011 0.81 -4 4 0 67.11 14.11 3.39 0.056 1.06 4 1 6 107.09 41.74 3.33 0.096 1.20 3 -2 1 26.10 1.53 3.26 0.018 1.61 -4 4 1 446.38 217.55 3.24 0.220 1.05 4 -6 3 35.16 0.27 3.09 0.008 0.84 6 5 2 24.96 1.10 3.09 0.016 0.86 5 2 4 196.89 11.08 3.08 0.050 1.12 3 7 2 27.10 0.78 3.01 0.013 0.99 3 -2 2 27.62 0.62 2.98 0.012 1.56 4 3 5 52.15 0.64 2.97 0.012 1.22 -1 6 0 148.78 71.89 2.95 0.126 1.16 1 8 3 69.93 21.04 2.89 0.068 0.93 0 7 7 20.93 0.10 2.88 0.005 0.90 0 5 1 611.00 370.91 2.87 0.287 1.48 1 -4 9 22.14 0.37 2.83 0.009 0.85 Bond lengths and angles C1 - Distance Angles O1B 1.2575 (0.0071) O1A 1.2593 (0.0073) 123.83 (0.53) C2 1.5225 (0.0077) 119.12 (0.50) 117.04 (0.50) C1 - O1B O1A C2 - Distance Angles C3 1.5162 (0.0081) C1 1.5225 (0.0077) 114.52 (0.49) H2A 0.9900 108.63 108.63 H2B 0.9900 108.63 108.63 107.58 C2 - C3 C1 H2A C3 - Distance Angles C2 1.5162 (0.0081) C3_$2 1.5171 (0.0108) 113.84 (0.59) H3A 0.9900 108.79 108.79 H3B 0.9900 108.79 108.79 107.67 C3 - C2 C3_$2 H3A O1A - Distance Angles C1 1.2593 (0.0073) O1A - O1B - Distance Angles C1 1.2575 (0.0071) O1B - C23 - Distance Angles O24 1.4155 (0.0081) C22 1.5130 (0.0084) 111.12 (0.51) H23A 0.9900 109.41 109.41 H23B 0.9900 109.41 109.41 108.02 C23 - O24 C22 H23A C22 - Distance Angles N21 1.4876 (0.0075) C23 1.5130 (0.0084) 109.85 (0.47) H22A 0.9900 109.69 109.69 H22B 0.9900 109.69 109.69 108.19 C22 - N21 C23 H22A C26 - Distance Angles N21 1.4868 (0.0080) C25 1.5177 (0.0088) 109.68 (0.49) H26A 0.9900 109.73 109.73 H26B 0.9900 109.73 109.73 108.21 C26 - N21 C25 H26A C25 - Distance Angles O24 1.4274 (0.0075) C26 1.5177 (0.0088) 111.04 (0.50) H25A 0.9900 109.43 109.43 H25B 0.9900 109.43 109.43 108.03 C25 - O24 C26 H25A N21 - Distance Angles C26 1.4868 (0.0080) C22 1.4876 (0.0075) 110.04 (0.46) H21A 0.9200 109.65 109.65 H21B 0.9200 109.65 109.65 108.16 N21 - C26 C22 H21A O24 - Distance Angles C23 1.4155 (0.0081) C25 1.4274 (0.0075) 111.10 (0.47) O24 - C23 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.92 1.81 2.722(6) 171.6 N21-H21B...O1B 0.92 1.76 2.675(6) 172.0 N21-H21A...O1A_$1 0.92 2.64 3.256(6) 125.3 N21-H21A...O1B_$1 Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 0.7778 (0.0471) x + 5.2983 (0.0479) y + 8.0284 (0.0407) z = 2.5309 (0.0235) * 0.0000 (0.0000) C1 * 0.0000 (0.0000) O1A * 0.0000 (0.0000) O1B Rms deviation of fitted atoms = 0.0000 0.7778 (0.0471) x + 5.2983 (0.0480) y + 8.0284 (0.0405) z = 0.9770 (0.0622) Angle to previous plane (with approximate esd) = 0.00 ( 1.11 ) * 0.0000 (0.0000) C1_$2 * 0.0000 (0.0000) O1A_$2 * 0.0000 (0.0000) O1B_$2 Rms deviation of fitted atoms = 0.0000 FMAP and GRID set by program FMAP 2 1 16 GRID -3.846 -2 -2 3.846 2 2 R1 = 0.1754 for 1859 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.68 at 0.4483 0.7403 0.6572 [ 1.33 A from H2A ] Deepest hole -0.44 at 0.1645 0.8945 0.5931 [ 1.66 A from H26B ] Mean = 0.00, Rms deviation from mean = 0.13 e/A^3, Highest memory used = 1877 / 14614 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4483 -0.2597 0.6572 1.00000 0.05 0.68 1.33 H2A 1.67 H25B 2.04 H3B 2.08 H26B Q2 1 0.7283 -0.3296 0.2973 1.00000 0.05 0.60 1.36 H3B 1.61 C1 1.67 C3 1.74 C2 Q3 1 0.4751 0.3399 -0.2154 1.00000 0.05 0.56 1.44 H23B 1.75 H3B 2.04 H2B 2.12 H23A Q4 1 0.2121 0.4275 -0.0754 1.00000 0.05 0.55 0.58 H23B 1.08 C23 1.60 O24 1.88 H23A Q5 1 0.3569 0.0783 0.0073 1.00000 0.05 0.53 0.76 H22B 1.27 C22 1.82 H23A 1.85 C23 Q6 1 0.4372 -0.1718 0.3013 1.00000 0.05 0.52 0.87 H2B 1.37 C2 1.69 C1 1.83 O1B Q7 1 0.0370 0.5431 -0.0111 1.00000 0.05 0.51 1.42 O24 1.69 O24 1.91 H22A 1.95 H23B Q8 1 0.2597 0.4076 0.3384 1.00000 0.05 0.50 1.14 H25A 1.16 H25B 1.18 C25 1.75 H26A Q9 1 0.0000 0.5000 0.0000 0.50000 0.05 0.49 1.51 O24 1.94 H23B 1.98 C23 2.25 H22A Q10 1 0.2024 0.4689 -0.2204 1.00000 0.05 0.48 1.40 H23B 1.49 H3B 1.88 H26B 2.24 H25A Shortest distances between peaks (including symmetry equivalents) 7 9 0.40 7 7 0.80 4 7 1.36 2 10 1.36 4 9 1.39 4 10 1.41 4 7 1.52 2 3 1.58 3 6 1.60 3 10 1.74 5 5 1.89 1 8 1.89 2 6 1.92 3 4 1.95 7 10 2.21 9 10 2.27 2 4 2.37 7 10 2.39 3 8 2.56 1 10 2.60 4 5 2.65 3 5 2.68 4 4 2.78 6 10 2.93 5 6 2.99 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 0.17: Structure factors and derivatives 0.17: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.05: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.00: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0037p-1 finished at 12:44:36 Total CPU time: 1.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++