+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 09:06:31 on 01-Feb-2002 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s93 in P2(1) CELL 0.71073 8.1183 5.9280 9.0398 90.000 113.000 90.000 ZERR 1.00 0.0007 0.0005 0.0007 0.000 0.007 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H O UNIT 16 24 8 V = 400.46 F(000) = 184.0 Mu = 0.11 mm-1 Cell Wt = 344.35 Rho = 1.428 SHEL 7 0.84 TEMP -153 SIZE 0.2 0.1 0.1 ACTA FMAP 2 PLAN 20 BOND L.S. 4 WGHT 0.0227 0.0000 EXTI 0.052150 FVAR 0.57325 H2B 2 0.667730 -0.181456 0.944690 11.00000 0.04882 H2C 2 0.492218 -0.061999 0.953334 11.00000 0.03122 H4 2 0.685701 0.511414 0.741160 11.00000 0.02456 H5 2 0.640475 0.267513 0.526808 11.00000 0.01648 H6 2 0.938613 0.019660 0.594983 11.00000 0.02009 H7A 2 0.925482 0.654927 0.692225 11.00000 0.01608 H7B 2 1.124586 0.569447 0.777410 11.00000 0.03510 H8 2 0.998621 0.431756 0.954419 11.00000 0.02518 MOLE 1 C1 1 0.378356 0.186430 0.685435 11.00000 0.01902 0.02856 = 0.02702 -0.00266 0.00944 -0.00105 C2 1 0.548965 -0.116912 0.877814 11.00000 0.02711 0.02699 = 0.02425 -0.00117 0.01325 -0.00217 C3 1 0.557540 0.077931 0.776850 11.00000 0.02061 0.02526 = 0.01672 -0.00540 0.00960 -0.00089 C4 1 0.745262 0.365481 0.775270 11.00000 0.02188 0.01986 = 0.02470 -0.00019 0.01221 0.00047 C5 1 0.717445 0.203405 0.633198 11.00000 0.02250 0.01768 = 0.01878 0.00184 0.00889 -0.00208 C6 1 0.910990 0.165061 0.653788 11.00000 0.02063 0.02239 = 0.01922 0.00292 0.01188 -0.00339 C7 1 1.000420 0.526624 0.732986 11.00000 0.02711 0.01983 = 0.03368 -0.00070 0.01397 -0.00310 C8 1 0.947157 0.388112 0.848209 11.00000 0.02212 0.02114 = 0.01965 -0.00615 0.00796 -0.00113 O1 3 0.680846 0.241081 0.876473 11.00000 0.02151 0.02933 = 0.01886 -0.00534 0.01003 -0.00359 O2 3 0.640579 0.005892 0.669926 11.00000 0.02345 0.02097 = 0.01973 -0.00279 0.01309 -0.00286 O3 3 1.006347 0.165053 0.822484 11.00000 0.02098 0.02190 = 0.01951 0.00018 0.00822 0.00295 O4 3 0.966716 0.369244 0.601236 11.00000 0.02656 0.01975 = 0.02310 0.00278 0.01182 -0.00012 MOLE 0 H1A 2 0.387882 0.311824 0.620431 11.00000 0.03403 H1B 2 0.326882 0.238853 0.770007 11.00000 0.03164 H1C 2 0.298419 0.078323 0.622066 11.00000 0.02812 H2A 2 0.477561 -0.226609 0.810267 11.00000 0.02085 HKLF 4 1.0 0.00 1.00 0.00 1.00 0.00 0.00 0.00 0.00 -1.00 Covalent radii and connectivity table for s93 in P2(1) C 0.770 H 0.320 O 0.660 C1 - C3 C2 - C3 C3 - O1 O2 C2 C1 C4 - O1 C8 C5 C5 - O2 C6 C4 C6 - O3 O4 C5 C7 - O4 C8 C8 - O3 C4 C7 O1 - C4 C3 O2 - C5 C3 O3 - C6 C8 O4 - C6 C7 Floating origin restraints generated 4307 Reflections read, of which 498 rejected -9 =< h =< 9, -6 =< k =< 7, -10 =< l =< 10, Max. 2-theta = 50.02 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -2 -1 4 84.83 2.70 3 16.44 0 -1 5 97.78 0.99 4 31.69 -3 1 8 15.88 0.87 3 7.74 -5 1 9 18.19 1.68 2 9.16 4 Inconsistent equivalents 1360 Unique reflections, of which 0 suppressed R(int) = 0.0637 R(sigma) = 0.0734 Friedel opposites not merged Maximum memory for data reduction = 1273 / 13552 Least-squares cycle 1 Maximum vector length = 511 Memory required = 1647 / 196326 wR2 = 0.0753 before cycle 1 for 1360 data and 158 / 158 parameters GooF = S = 0.997; Restrained GooF = 0.997 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0227 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.57243 0.00166 -0.495 OSF 2 0.04935 0.00618 -0.452 EXTI Mean shift/esd = 0.128 Maximum = -0.495 for OSF Max. shift = 0.012 A for H7B Max. dU = 0.002 for H2C Least-squares cycle 2 Maximum vector length = 511 Memory required = 1647 / 196326 wR2 = 0.0751 before cycle 2 for 1360 data and 158 / 158 parameters GooF = S = 0.996; Restrained GooF = 0.995 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0227 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.57206 0.00165 -0.223 OSF 2 0.04825 0.00606 -0.182 EXTI Mean shift/esd = 0.042 Maximum = -0.223 for OSF Max. shift = 0.005 A for H7A Max. dU = 0.001 for H2C Least-squares cycle 3 Maximum vector length = 511 Memory required = 1647 / 196326 wR2 = 0.0751 before cycle 3 for 1360 data and 158 / 158 parameters GooF = S = 0.995; Restrained GooF = 0.995 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0227 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.57207 0.00164 0.001 OSF 2 0.04817 0.00601 -0.013 EXTI Mean shift/esd = 0.004 Maximum = 0.025 for U11 H2C Max. shift = 0.001 A for H2C Max. dU = 0.000 for H2C Least-squares cycle 4 Maximum vector length = 511 Memory required = 1647 / 196326 wR2 = 0.0751 before cycle 4 for 1360 data and 158 / 158 parameters GooF = S = 0.995; Restrained GooF = 0.995 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0227 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.57207 0.00164 0.003 OSF 2 0.04816 0.00601 -0.001 EXTI Mean shift/esd = 0.002 Maximum = 0.011 for U11 H1B Max. shift = 0.000 A for H2C Max. dU = 0.000 for H1B Largest correlation matrix elements 0.579 U13 C3 / U11 C3 0.526 EXTI / OSF 0.514 U13 C4 / U11 C4 0.560 U13 C6 / U11 C6 0.525 U13 O3 / U11 O3 0.512 U13 C5 / U11 C5 0.529 U13 C2 / U11 C2 0.521 z C7 / x C7 0.510 U13 O2 / U33 O2 0.527 U13 C7 / U11 C7 0.518 U13 C4 / U33 C4 s93 in P2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq H2B 0.66834 -0.18037 0.94474 1.00000 0.04957 0.06406 0.00445 0.00561 0.00350 0.00000 0.00941 H2C 0.49168 -0.06190 0.95418 1.00000 0.03451 0.05078 0.00357 0.00408 0.00315 0.00000 0.00830 H4 0.68545 0.51197 0.74055 1.00000 0.02588 0.05157 0.00328 0.00485 0.00280 0.00000 0.00734 H5 0.64026 0.26763 0.52689 1.00000 0.01745 0.04690 0.00310 0.00429 0.00254 0.00000 0.00618 H6 0.93934 0.01983 0.59488 1.00000 0.01982 0.04964 0.00300 0.00486 0.00282 0.00000 0.00633 H7A 0.92446 0.65748 0.69194 1.00000 0.01771 0.04721 0.00330 0.00487 0.00253 0.00000 0.00672 H7B 1.12327 0.56785 0.77623 1.00000 0.03475 0.05648 0.00401 0.00478 0.00273 0.00000 0.00827 H8 0.99910 0.43173 0.95521 1.00000 0.02401 0.05191 0.00325 0.00400 0.00310 0.00000 0.00781 C1 0.37833 0.18646 0.68549 1.00000 0.01836 0.02878 0.02690 -0.00297 0.00902 -0.00113 0.02463 0.00626 0.00039 0.00057 0.00033 0.00000 0.00155 0.00189 0.00147 0.00155 0.00120 0.00144 0.00068 C2 0.54901 -0.11681 0.87799 1.00000 0.02694 0.02681 0.02384 -0.00114 0.01285 -0.00237 0.02496 0.00661 0.00043 0.00054 0.00035 0.00000 0.00178 0.00172 0.00147 0.00142 0.00130 0.00152 0.00066 C3 0.55749 0.07808 0.77694 1.00000 0.02039 0.02464 0.01674 -0.00512 0.00961 -0.00071 0.01987 0.00479 0.00032 0.00043 0.00026 0.00000 0.00151 0.00170 0.00125 0.00110 0.00109 0.00124 0.00064 C4 0.74529 0.36552 0.77528 1.00000 0.02178 0.01949 0.02466 -0.00001 0.01230 0.00036 0.02098 0.00538 0.00035 0.00049 0.00028 0.00000 0.00150 0.00162 0.00138 0.00121 0.00113 0.00137 0.00061 C5 0.71752 0.20342 0.63321 1.00000 0.02203 0.01729 0.01864 0.00187 0.00875 -0.00204 0.01907 0.00505 0.00034 0.00043 0.00029 0.00000 0.00153 0.00170 0.00128 0.00116 0.00109 0.00129 0.00063 C6 0.91096 0.16492 0.65375 1.00000 0.02052 0.02209 0.01901 0.00298 0.01185 -0.00301 0.01927 0.00510 0.00033 0.00048 0.00027 0.00000 0.00160 0.00157 0.00128 0.00121 0.00105 0.00126 0.00061 C7 1.00033 0.52687 0.73295 1.00000 0.02694 0.01969 0.03333 -0.00072 0.01382 -0.00351 0.02603 0.00620 0.00044 0.00053 0.00033 0.00000 0.00180 0.00176 0.00161 0.00136 0.00133 0.00150 0.00067 C8 0.94711 0.38810 0.84821 1.00000 0.02137 0.02094 0.01946 -0.00618 0.00777 -0.00128 0.02065 0.00536 0.00035 0.00045 0.00031 0.00000 0.00154 0.00160 0.00144 0.00124 0.00112 0.00128 0.00062 O1 0.68083 0.24105 0.87644 1.00000 0.02131 0.02890 0.01844 -0.00533 0.00981 -0.00371 0.02226 0.00331 0.00022 0.00030 0.00018 0.00000 0.00100 0.00126 0.00086 0.00081 0.00074 0.00089 0.00050 O2 0.64058 0.00583 0.66996 1.00000 0.02312 0.02070 0.01938 -0.00284 0.01302 -0.00280 0.01962 0.00341 0.00021 0.00030 0.00019 0.00000 0.00097 0.00102 0.00090 0.00077 0.00073 0.00086 0.00046 O3 1.00638 0.16505 0.82253 1.00000 0.02056 0.02185 0.01941 0.00013 0.00802 0.00322 0.02054 0.00333 0.00022 0.00028 0.00018 0.00000 0.00103 0.00110 0.00086 0.00077 0.00071 0.00085 0.00046 O4 0.96675 0.36918 0.60124 1.00000 0.02630 0.01972 0.02251 0.00279 0.01160 -0.00015 0.02221 0.00346 0.00022 0.00029 0.00018 0.00000 0.00103 0.00107 0.00096 0.00080 0.00074 0.00091 0.00046 H1A 0.38794 0.31202 0.62064 1.00000 0.03595 0.05640 0.00367 0.00584 0.00307 0.00000 0.00833 H1B 0.32617 0.23788 0.77100 1.00000 0.03072 0.04931 0.00337 0.00472 0.00300 0.00000 0.00713 H1C 0.29891 0.07862 0.62277 1.00000 0.02750 0.05866 0.00348 0.00489 0.00291 0.00000 0.00785 H2A 0.47774 -0.22542 0.81016 1.00000 0.01955 0.05848 0.00339 0.00495 0.00291 0.00000 0.00688 Final Structure Factor Calculation for s93 in P2(1) Total number of l.s. parameters = 158 Maximum vector length = 511 Memory required = 1491 / 24024 wR2 = 0.0751 before cycle 5 for 1360 data and 2 / 158 parameters GooF = S = 0.995; Restrained GooF = 0.995 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0227 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0374 for 1063 Fo > 4sig(Fo) and 0.0609 for all 1360 data wR2 = 0.0751, GooF = S = 0.995, Restrained GooF = 0.995 for all data Flack x parameter = 2.3451 with esd 1.3204 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 12.00 for non-hydrogen and 12.00 for hydrogen atoms Principal mean square atomic displacements U 0.0310 0.0250 0.0179 C1 0.0297 0.0250 0.0201 C2 0.0272 0.0203 0.0121 C3 0.0259 0.0196 0.0175 C4 0.0230 0.0199 0.0143 C5 0.0247 0.0227 0.0104 C6 0.0335 0.0266 0.0180 C7 0.0266 0.0215 0.0139 C8 0.0318 0.0198 0.0152 O1 0.0268 0.0189 0.0131 O2 0.0247 0.0194 0.0175 O3 0.0267 0.0230 0.0169 O4 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.032 0.045 0.061 0.076 0.097 0.118 0.140 0.167 0.230 1.000 Number in group 148. 133. 129. 134. 143. 134. 133. 138. 134. 134. GooF 0.851 0.930 1.047 0.962 1.025 0.993 1.035 0.940 0.941 1.205 K 1.025 0.859 0.915 0.978 0.951 0.977 0.979 1.002 1.008 1.009 Resolution(A) 0.84 0.88 0.91 0.96 1.00 1.08 1.15 1.26 1.45 1.82 inf Number in group 138. 135. 137. 137. 137. 136. 132. 137. 137. 134. GooF 0.954 0.973 0.929 1.008 0.945 0.968 1.020 0.980 1.115 1.049 K 0.927 0.970 0.989 0.972 0.994 1.015 1.012 1.016 1.021 0.991 R1 0.230 0.163 0.103 0.092 0.049 0.040 0.037 0.035 0.029 0.020 Recommended weighting scheme: WGHT 0.0188 0.0000 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) -4 4 4 52.61 68.80 3.60 0.134 1.14 0 -4 7 9.11 0.15 3.13 0.006 0.93 -6 1 9 12.23 21.13 3.08 0.075 0.93 0 -6 3 30.30 56.74 3.08 0.122 0.93 0 1 5 457.55 415.38 2.87 0.330 1.60 0 -1 2 82.93 89.88 2.86 0.154 3.41 -1 -1 1 984.72 1107.64 2.86 0.540 4.55 -6 1 8 23.15 29.19 2.84 0.088 1.00 -4 4 6 69.43 85.24 2.81 0.150 1.02 -9 -2 4 33.44 51.55 2.79 0.116 0.86 0 -2 8 18.40 34.39 2.76 0.095 0.98 0 1 1 4102.15 3804.04 2.76 1.000 4.83 -8 -1 2 14.43 25.88 2.72 0.082 0.98 -2 -1 6 45.77 53.29 2.71 0.118 1.46 0 6 1 19.98 36.59 2.70 0.098 0.98 4 0 5 405.28 364.98 2.69 0.310 1.05 1 -1 0 764.32 839.15 2.67 0.470 4.64 -1 2 5 107.47 97.21 2.66 0.160 1.53 -2 0 2 893.36 974.61 2.61 0.506 3.55 -3 -3 1 -1.02 3.69 2.61 0.031 1.59 1 -3 5 7.18 11.96 2.61 0.056 1.20 1 -1 8 94.20 111.30 2.59 0.171 0.97 1 -2 8 6.14 13.63 2.58 0.060 0.93 -1 1 1 1016.58 1107.94 2.55 0.540 4.55 8 2 0 -3.06 11.60 2.55 0.055 0.89 -2 4 1 283.70 242.54 2.53 0.253 1.39 3 1 5 88.86 76.62 2.51 0.142 1.16 5 -1 2 34.57 43.28 2.50 0.107 1.23 -1 -3 5 193.93 217.15 2.50 0.239 1.32 -1 -2 9 45.93 67.57 2.48 0.133 0.92 1 1 0 778.45 839.47 2.48 0.470 4.64 -2 4 2 13.42 18.10 2.41 0.069 1.37 3 -3 4 20.82 27.42 2.39 0.085 1.12 -6 -4 7 20.06 10.43 2.36 0.052 0.88 -6 -2 1 1.22 6.31 2.35 0.041 1.20 2 1 0 410.68 442.93 2.33 0.341 3.16 7 3 1 46.46 70.35 2.33 0.136 0.90 -1 0 3 15.44 22.18 2.31 0.076 3.01 0 -3 2 92.57 107.48 2.30 0.168 1.78 -8 3 1 -2.05 9.74 2.29 0.051 0.87 5 2 2 143.84 125.60 2.26 0.182 1.16 2 3 6 28.65 35.77 2.25 0.097 1.00 -8 0 1 29.44 43.07 2.23 0.106 0.97 -2 0 6 24.46 30.97 2.23 0.090 1.51 4 -2 4 35.71 42.44 2.22 0.106 1.10 5 -1 6 -0.76 5.23 2.21 0.037 0.85 -6 -1 6 18.49 12.10 2.20 0.056 1.16 1 1 5 50.84 45.56 2.20 0.109 1.46 1 -1 2 22.41 18.68 2.20 0.070 2.78 -2 -6 4 0.00 12.32 2.19 0.057 0.90 Bond lengths and angles C1 - Distance Angles C3 1.5073 (0.0037) C1 - C2 - Distance Angles C3 1.4910 (0.0036) C2 - C3 - Distance Angles O1 1.4287 (0.0029) O2 1.4434 (0.0027) 103.08 (0.19) C2 1.4910 (0.0036) 109.09 (0.20) 109.03 (0.21) C1 1.5073 (0.0037) 110.23 (0.22) 111.25 (0.19) 113.62 (0.24) C3 - O1 O2 C2 C4 - Distance Angles O1 1.4242 (0.0029) C8 1.5143 (0.0036) 111.89 (0.20) C5 1.5484 (0.0034) 103.89 (0.21) 101.42 (0.19) C4 - O1 C8 C5 - Distance Angles O2 1.4263 (0.0031) C6 1.5248 (0.0035) 111.88 (0.22) C4 1.5484 (0.0034) 104.57 (0.18) 100.52 (0.19) C5 - O2 C6 C6 - Distance Angles O3 1.4158 (0.0027) O4 1.4369 (0.0030) 104.19 (0.19) C5 1.5248 (0.0035) 103.59 (0.17) 106.04 (0.22) C6 - O3 O4 C7 - Distance Angles O4 1.4533 (0.0031) C8 1.5168 (0.0037) 101.61 (0.22) C7 - O4 C8 - Distance Angles O3 1.4564 (0.0031) C4 1.5143 (0.0036) 102.65 (0.21) C7 1.5168 (0.0037) 100.51 (0.20) 107.40 (0.22) C8 - O3 C4 O1 - Distance Angles C4 1.4242 (0.0029) C3 1.4287 (0.0029) 106.80 (0.18) O1 - C4 O2 - Distance Angles C5 1.4263 (0.0031) C3 1.4434 (0.0027) 105.91 (0.19) O2 - C5 O3 - Distance Angles C6 1.4158 (0.0027) C8 1.4564 (0.0032) 95.54 (0.18) O3 - C6 O4 - Distance Angles C6 1.4369 (0.0030) C7 1.4533 (0.0031) 104.70 (0.17) O4 - C6 FMAP and GRID set by program FMAP 2 2 17 GRID -3.571 -2 -2 3.571 2 2 R1 = 0.0510 for 771 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.18 at 0.2367 0.2676 0.8284 [ 1.06 A from H1B ] Deepest hole -0.18 at 0.0005 0.1392 0.3198 [ 0.67 A from H7A ] Mean = 0.00, Rms deviation from mean = 0.04 e/A^3, Highest memory used = 1507 / 13633 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2367 0.2676 0.8284 1.00000 0.05 0.18 1.06 H1B 1.91 H2B 1.95 O3 1.97 H7B Q2 1 0.4066 0.3841 0.8564 1.00000 0.05 0.17 1.17 H1B 1.62 H2C 1.88 C1 2.12 H1A Q3 1 0.4022 0.1870 0.8801 1.00000 0.05 0.16 0.98 H1B 1.67 H2C 1.69 C1 1.95 C3 Q4 1 0.2828 0.0076 0.8473 1.00000 0.05 0.15 1.63 H1B 1.64 H2C 2.13 H1C 2.18 C1 Q5 1 0.3208 0.3326 0.7247 1.00000 0.05 0.15 0.69 H1B 1.11 C1 1.26 H1A 1.74 H1C Q6 1 0.9586 -0.0065 0.8559 1.00000 0.05 0.15 1.17 O3 1.65 H8 1.99 C6 2.31 H6 Q7 1 0.3250 -0.1260 0.5955 1.00000 0.05 0.14 1.27 H1C 1.39 H5 1.94 H2A 2.00 C1 Q8 1 0.6512 0.3298 0.9021 1.00000 0.05 0.14 0.66 O1 1.62 C4 1.85 C3 1.92 H4 Q9 1 0.7461 0.0122 0.8434 1.00000 0.05 0.14 1.46 C3 1.46 O2 1.53 O1 1.73 H2B Q10 1 0.6165 0.1742 0.8253 1.00000 0.05 0.14 0.67 O1 0.76 C3 1.72 C4 1.79 O2 Q11 1 0.6540 0.3954 0.6472 1.00000 0.05 0.14 1.04 H4 1.12 C4 1.28 C5 1.29 H5 Q12 1 0.8201 -0.0870 0.7599 1.00000 0.05 0.14 1.47 O2 1.95 H7A 2.04 O3 2.06 C5 Q13 1 0.1942 0.2882 0.6974 1.00000 0.05 0.14 1.06 H1B 1.65 C1 1.77 O4 1.78 H1C Q14 1 0.4643 -0.1788 1.0506 1.00000 0.05 0.14 1.20 H2C 1.63 O1 1.90 H1B 1.97 C2 Q15 1 0.7403 0.1263 0.8209 1.00000 0.05 0.14 1.07 O1 1.41 C3 1.47 O2 1.48 C4 Q16 1 0.7923 0.5769 0.7086 1.00000 0.05 0.13 1.09 H4 1.24 H7A 1.50 C4 1.64 C7 Q17 1 0.8588 0.4010 0.8391 1.00000 0.05 0.13 0.69 C8 0.90 C4 1.22 H8 1.49 H4 Q18 1 0.6898 0.5516 0.6331 1.00000 0.05 0.13 1.01 H4 1.62 C4 1.87 H7A 1.90 H5 Q19 1 0.4976 0.2832 0.8396 1.00000 0.05 0.13 1.31 H1B 1.41 O1 1.47 C1 1.50 C3 Q20 1 1.1036 -0.0200 0.9184 1.00000 0.05 0.13 1.43 O3 1.68 H8 2.37 C8 2.44 O1 Shortest distances between peaks (including symmetry equivalents) 9 15 0.70 16 18 0.86 14 19 0.94 5 13 0.99 11 18 0.99 2 19 1.01 10 15 1.06 6 20 1.09 1 13 1.10 2 14 1.12 8 10 1.12 3 19 1.13 2 5 1.16 8 14 1.17 8 19 1.18 2 3 1.19 10 19 1.21 6 12 1.22 9 12 1.28 3 14 1.29 1 3 1.33 9 10 1.39 3 4 1.39 1 5 1.41 5 19 1.43 1 2 1.47 11 16 1.50 16 17 1.51 3 5 1.56 1 4 1.58 12 15 1.61 6 9 1.69 8 15 1.71 10 14 1.74 4 20 1.81 6 15 1.85 2 13 1.85 15 17 1.86 11 17 1.88 2 8 1.89 3 13 1.94 3 10 1.99 8 17 2.02 17 18 2.04 12 16 2.04 1 19 2.08 4 13 2.09 5 14 2.10 3 8 2.13 17 20 2.14 11 15 2.15 4 14 2.16 8 9 2.18 10 11 2.19 8 20 2.21 2 10 2.22 12 20 2.22 15 19 2.24 1 14 2.26 7 11 2.27 7 18 2.28 13 19 2.29 4 5 2.30 1 20 2.33 10 17 2.34 8 11 2.35 4 8 2.36 5 10 2.40 4 19 2.41 2 4 2.44 12 18 2.46 9 17 2.48 10 12 2.50 5 8 2.53 6 17 2.53 4 7 2.56 9 19 2.57 3 14 2.59 11 19 2.61 6 17 2.63 14 15 2.64 4 14 2.65 4 6 2.66 9 20 2.72 9 11 2.80 7 16 2.80 13 14 2.82 8 16 2.84 14 20 2.86 3 20 2.86 15 20 2.86 1 6 2.87 6 16 2.88 6 10 2.89 8 18 2.89 2 3 2.90 9 14 2.91 9 16 2.94 15 16 2.95 7 13 2.96 4 10 2.96 5 7 2.96 2 4 2.96 12 17 2.97 15 18 2.98 Time profile in seconds ----------------------- 0.11: 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. 0.11: 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 0.33: Structure factors and derivatives 0.11: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.05: Apply other restraints 0.06: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.00: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 09:06:31 Total elapsed time: 0.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++