+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 16:19:50 on 24-Nov-2000 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 00MAU005 in P2(1)/c CELL 0.71073 6.9056 8.6519 12.8184 90.000 94.411 90.000 ZERR 4.00 0.0014 0.0017 0.0026 0.000 0.030 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 24 36 12 12 V = 763.59 F(000) = 360.0 Mu = 0.12 mm-1 Cell Wt = 684.65 Rho = 1.489 MERG 2 OMIT -3.00 55.00 EXTI 0.04082 FMAP 2 PLAN 20 SIZE 0.08 0.12 0.40 ACTA BOND WGHT 0.06140 0.11730 L.S. 4 TEMP -123.00 FVAR 1.00638 MOLE 1 C1 1 0.216567 0.212418 0.536002 11.00000 0.02178 0.02455 = 0.02410 0.00315 0.00289 -0.00144 C2 1 0.212510 0.368726 0.582008 11.00000 0.04200 0.02397 = 0.03668 -0.00088 0.00214 0.00004 AFIX 137 H2A 2 0.151567 0.440770 0.530403 11.00000 -1.50000 H2B 2 0.345545 0.402606 0.602215 11.00000 -1.50000 H2C 2 0.137725 0.366549 0.643942 11.00000 -1.50000 AFIX 0 C3 1 0.370952 0.083234 0.696437 11.00000 0.02789 0.03155 = 0.01807 -0.00251 -0.00491 -0.00099 AFIX 23 H3A 2 0.413143 0.188901 0.717280 11.00000 -1.20000 H3B 2 0.487058 0.015738 0.701664 11.00000 -1.20000 AFIX 0 C4 1 0.227563 0.025345 0.771283 11.00000 0.03668 0.02800 = 0.01986 -0.00085 0.00010 0.00183 AFIX 23 H4A 2 0.188026 -0.081435 0.751770 11.00000 -1.20000 H4B 2 0.291584 0.022647 0.843067 11.00000 -1.20000 AFIX 0 C5 1 0.268473 -0.033130 0.515334 11.00000 0.02007 0.02188 = 0.02066 -0.00120 0.00182 -0.00166 C6 1 0.185857 0.025682 0.424317 11.00000 0.02329 0.02850 = 0.01901 -0.00132 0.00169 -0.00482 AFIX 43 H6 2 0.155693 -0.031165 0.361766 11.00000 -1.20000 AFIX 0 N1 3 0.153382 0.179016 0.437290 11.00000 0.02583 0.02846 = 0.02209 0.00413 0.00080 -0.00137 N2 3 0.288175 0.085872 0.587357 11.00000 0.02185 0.02165 = 0.01849 -0.00059 -0.00016 -0.00078 N3 3 0.322657 -0.189146 0.535107 11.00000 0.02562 0.02563 = 0.02629 -0.00150 0.00289 -0.00004 O1 4 0.060652 0.120014 0.770091 11.00000 0.03204 0.03609 = 0.02360 -0.00839 -0.00025 0.00066 AFIX 147 H1 2 0.074889 0.185398 0.818516 11.00000 -1.50000 AFIX 0 O2 4 0.303616 -0.278322 0.460305 11.00000 0.05652 0.02695 = 0.03411 -0.01052 0.00270 -0.00011 O3 4 0.384869 -0.228448 0.623177 11.00000 0.05195 0.03332 = 0.03096 0.00345 -0.00728 0.01150 HKLF 4 Covalent radii and connectivity table for 00MAU005 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 C1 - N1 N2 C2 C2 - C1 C3 - N2 C4 C4 - O1 C3 C5 - C6 N2 N3 C6 - C5 N1 N1 - C1 C6 N2 - C1 C5 C3 N3 - O3 O2 C5 O1 - C4 O2 - N3 O3 - N3 h k l Fo^2 Sigma Why rejected -2 0 1 1.56 0.24 observed but should be systematically absent -1 0 1 5.18 0.62 observed but should be systematically absent -1 0 1 4.51 0.85 observed but should be systematically absent -1 0 1 6.00 0.37 observed but should be systematically absent 6318 Reflections read, of which 235 rejected -8 =< h =< 8, -11 =< k =< 11, -16 =< l =< 16, Max. 2-theta = 54.97 4 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 4 2 0 405.92 2.20 6 57.30 4 1 2 124.75 0.37 4 66.86 6 3 2 77.11 1.08 3 57.85 6 3 3 10.24 0.65 4 3.92 4 Inconsistent equivalents 1725 Unique reflections, of which 0 suppressed R(int) = 0.0378 R(sigma) = 0.0431 Friedel opposites merged Maximum memory for data reduction = 1164 / 17123 Default effective X-H distances for T = -123.0 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 = 1474 / 144011 wR2 = 0.1099 before cycle 1 for 1725 data and 112 / 112 parameters GooF = S = 1.021; Restrained GooF = 1.021 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0614 * P )^2 + 0.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.00675 0.00352 0.104 OSF 2 0.04157 0.01026 0.073 EXTI Mean shift/esd = 0.030 Maximum = 0.104 for OSF Max. shift = 0.001 A for H1 Max. dU = 0.000 for C3 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1474 / 144011 wR2 = 0.1099 before cycle 2 for 1725 data and 112 / 112 parameters GooF = S = 1.021; Restrained GooF = 1.021 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0614 * P )^2 + 0.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.00669 0.00352 -0.017 OSF 2 0.04175 0.01030 0.017 EXTI Mean shift/esd = 0.011 Maximum = 0.031 for y O3 Max. shift = 0.000 A for H1 Max. dU = 0.000 for C2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1474 / 144011 wR2 = 0.1099 before cycle 3 for 1725 data and 112 / 112 parameters GooF = S = 1.021; Restrained GooF = 1.021 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0614 * P )^2 + 0.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.00667 0.00352 -0.005 OSF 2 0.04173 0.01031 -0.002 EXTI Mean shift/esd = 0.001 Maximum = -0.005 for OSF Max. shift = 0.000 A for H2A Max. dU = 0.000 for O3 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1474 / 144011 wR2 = 0.1099 before cycle 4 for 1725 data and 112 / 112 parameters GooF = S = 1.021; Restrained GooF = 1.021 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0614 * P )^2 + 0.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.00667 0.00352 0.000 OSF 2 0.04171 0.01031 -0.002 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for EXTI Max. shift = 0.000 A for H2A Max. dU = 0.000 for C3 Largest correlation matrix elements 0.543 EXTI / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2A 0.1516 0.4408 0.5304 137 0.980 0.000 C2 C1 H2A H2B 0.3455 0.4026 0.6022 137 0.980 0.000 C2 C1 H2A H2C 0.1377 0.3666 0.6439 137 0.980 0.000 C2 C1 H2A H3A 0.4132 0.1889 0.7173 23 0.990 0.000 C3 N2 C4 H3B 0.4871 0.0157 0.7017 23 0.990 0.000 C3 N2 C4 H4A 0.1880 -0.0814 0.7518 23 0.990 0.000 C4 O1 C3 H4B 0.2916 0.0226 0.8431 23 0.990 0.000 C4 O1 C3 H6 0.1557 -0.0312 0.3618 43 0.950 0.000 C6 C5 N1 H1 0.0748 0.1853 0.8186 147 0.840 0.000 O1 C4 H1 00MAU005 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.21658 0.21241 0.53600 1.00000 0.02180 0.02451 0.02408 0.00312 0.00287 -0.00145 0.02341 0.00229 0.00018 0.00015 0.00010 0.00000 0.00063 0.00073 0.00069 0.00053 0.00046 0.00048 0.00032 C2 0.21251 0.36874 0.58200 1.00000 0.04200 0.02391 0.03665 -0.00092 0.00215 0.00006 0.03423 0.00263 0.00022 0.00017 0.00012 0.00000 0.00083 0.00078 0.00083 0.00064 0.00061 0.00058 0.00037 H2A 0.15160 0.44078 0.53039 1.00000 0.05135 0.00000 0.00000 H2B 0.34554 0.40262 0.60223 1.00000 0.05135 0.00000 0.00000 H2C 0.13770 0.36657 0.64393 1.00000 0.05135 0.00000 0.00000 C3 0.37097 0.08323 0.69644 1.00000 0.02790 0.03149 0.01803 -0.00248 -0.00493 -0.00100 0.02615 0.00224 0.00019 0.00016 0.00010 0.00000 0.00069 0.00080 0.00065 0.00053 0.00049 0.00052 0.00034 H3A 0.41316 0.18890 0.71729 1.00000 0.03138 0.00000 0.00000 H3B 0.48708 0.01574 0.70167 1.00000 0.03138 0.00000 0.00000 C4 0.22757 0.02534 0.77128 1.00000 0.03662 0.02797 0.01989 -0.00085 0.00009 0.00183 0.02827 0.00254 0.00020 0.00017 0.00010 0.00000 0.00076 0.00076 0.00065 0.00056 0.00051 0.00056 0.00034 H4A 0.18804 -0.08143 0.75176 1.00000 0.03392 0.00000 0.00000 H4B 0.29159 0.02264 0.84306 1.00000 0.03392 0.00000 0.00000 C5 0.26849 -0.03314 0.51533 1.00000 0.02008 0.02188 0.02064 -0.00120 0.00183 -0.00163 0.02085 0.00216 0.00017 0.00015 0.00009 0.00000 0.00062 0.00070 0.00062 0.00051 0.00044 0.00046 0.00030 C6 0.18587 0.02567 0.42431 1.00000 0.02329 0.02848 0.01900 -0.00129 0.00169 -0.00480 0.02358 0.00227 0.00018 0.00016 0.00010 0.00000 0.00064 0.00075 0.00064 0.00053 0.00046 0.00050 0.00032 H6 0.15572 -0.03117 0.36175 1.00000 0.02830 0.00000 0.00000 N1 0.15339 0.17903 0.43729 1.00000 0.02581 0.02842 0.02209 0.00413 0.00081 -0.00138 0.02549 0.00197 0.00015 0.00014 0.00008 0.00000 0.00059 0.00065 0.00059 0.00047 0.00042 0.00044 0.00029 N2 0.28819 0.08587 0.58735 1.00000 0.02185 0.02165 0.01848 -0.00062 -0.00018 -0.00079 0.02075 0.00177 0.00014 0.00012 0.00008 0.00000 0.00054 0.00060 0.00056 0.00042 0.00038 0.00040 0.00028 N3 0.32266 -0.18914 0.53511 1.00000 0.02562 0.02557 0.02627 -0.00153 0.00289 -0.00003 0.02577 0.00199 0.00016 0.00013 0.00009 0.00000 0.00057 0.00065 0.00061 0.00049 0.00042 0.00044 0.00029 O1 0.06065 0.12002 0.77009 1.00000 0.03207 0.03605 0.02356 -0.00838 -0.00026 0.00068 0.03068 0.00163 0.00013 0.00012 0.00007 0.00000 0.00055 0.00061 0.00054 0.00041 0.00037 0.00040 0.00028 H1 0.07483 0.18534 0.81856 1.00000 0.04603 0.00000 0.00000 O2 0.30363 -0.27831 0.46030 1.00000 0.05645 0.02696 0.03411 -0.01050 0.00271 -0.00010 0.03921 0.00188 0.00017 0.00012 0.00008 0.00000 0.00071 0.00060 0.00063 0.00047 0.00048 0.00046 0.00031 O3 0.38488 -0.22843 0.62318 1.00000 0.05193 0.03331 0.03096 0.00345 -0.00729 0.01153 0.03927 0.00192 0.00016 0.00012 0.00008 0.00000 0.00068 0.00063 0.00061 0.00046 0.00046 0.00048 0.00032 Final Structure Factor Calculation for 00MAU005 in P2(1)/c Total number of l.s. parameters = 112 Maximum vector length = 511 Memory required = 1362 / 22995 wR2 = 0.1099 before cycle 5 for 1725 data and 0 / 112 parameters GooF = S = 1.021; Restrained GooF = 1.021 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0614 * P )^2 + 0.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0397 for 1368 Fo > 4sig(Fo) and 0.0547 for all 1725 data wR2 = 0.1099, GooF = S = 1.021, Restrained GooF = 1.021 for all data Occupancy sum of asymmetric unit = 12.00 for non-hydrogen and 9.00 for hydrogen atoms Principal mean square atomic displacements U 0.0275 0.0233 0.0195 C1 0.0422 0.0366 0.0238 C2 0.0322 0.0316 0.0147 C3 0.0375 0.0276 0.0197 C4 0.0233 0.0202 0.0190 C5 0.0314 0.0206 0.0188 C6 0.0312 0.0253 0.0201 N1 0.0229 0.0216 0.0177 N2 0.0277 0.0256 0.0241 N3 0.0408 0.0320 0.0192 O1 0.0566 0.0416 0.0194 O2 0.0606 0.0355 0.0217 O3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.014 0.027 0.044 0.058 0.080 0.099 0.125 0.166 0.240 1.000 Number in group 176. 170. 177. 167. 176. 176. 165. 173. 174. 171. GooF 0.867 1.045 1.091 1.054 1.106 1.024 1.019 1.004 0.981 1.002 K 0.870 0.928 0.955 0.966 0.937 0.990 0.992 1.020 1.024 1.018 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.63 inf Number in group 175. 172. 173. 175. 170. 172. 172. 172. 171. 173. GooF 0.911 0.854 0.764 0.996 0.983 1.005 0.889 0.988 1.208 1.447 K 0.973 0.993 1.030 1.031 1.006 1.021 1.032 1.038 1.037 0.997 R1 0.137 0.132 0.081 0.080 0.057 0.050 0.035 0.035 0.037 0.034 Recommended weighting scheme: WGHT 0.0605 0.1205 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) -3 0 2 3.37 1.16 4.22 0.016 2.21 1 0 0 1.58 4.28 3.87 0.030 6.89 0 3 3 3.74 7.85 3.84 0.041 2.39 1 0 6 118.68 91.03 3.44 0.138 1.99 0 8 5 38.01 52.32 3.34 0.105 1.00 -1 0 2 305.17 382.21 3.23 0.283 4.87 3 3 2 2.48 0.65 3.17 0.012 1.70 -1 5 3 28.55 38.53 3.15 0.090 1.57 3 3 12 23.36 14.98 3.13 0.056 0.89 -2 2 4 34.59 45.29 3.06 0.098 2.12 2 3 5 14.56 21.47 3.05 0.067 1.63 -2 3 1 4.94 2.47 3.04 0.023 2.20 1 2 2 416.62 508.35 2.99 0.327 3.12 1 1 8 60.55 46.80 2.97 0.099 1.51 -2 1 8 -0.81 1.25 2.91 0.016 1.47 0 10 7 9.50 0.37 2.91 0.009 0.78 2 6 2 9.35 5.35 2.84 0.034 1.29 -1 1 4 133.73 163.14 2.78 0.185 2.82 2 1 12 87.66 110.36 2.76 0.152 0.99 3 4 11 2.94 7.90 2.74 0.041 0.91 -1 2 1 4.06 6.58 2.71 0.037 3.56 2 2 7 286.26 240.05 2.69 0.225 1.47 -1 5 12 8.12 17.24 2.62 0.060 0.91 -1 2 7 49.05 39.43 2.62 0.091 1.66 -4 2 4 105.61 87.49 2.58 0.136 1.47 -1 4 1 14.45 19.76 2.58 0.064 2.04 1 5 1 57.39 46.54 2.57 0.099 1.66 2 2 11 23.89 31.73 2.57 0.082 1.04 -1 9 1 8.19 14.63 2.56 0.055 0.95 3 4 6 24.96 32.38 2.56 0.083 1.24 -5 0 2 51.68 66.65 2.54 0.118 1.37 3 1 7 30.00 38.17 2.54 0.090 1.36 0 8 1 1.01 4.38 2.54 0.030 1.08 -4 5 10 5.07 10.17 2.53 0.046 0.91 1 0 4 60.46 48.43 2.53 0.101 2.82 1 7 5 53.95 67.36 2.51 0.119 1.09 2 0 10 64.31 50.38 2.50 0.103 1.17 -1 4 2 101.33 84.55 2.49 0.133 1.98 5 3 1 -0.23 0.94 2.48 0.014 1.23 -1 4 3 208.03 176.56 2.45 0.193 1.87 -5 1 11 23.62 31.71 2.45 0.082 0.92 1 4 5 305.97 260.50 2.45 0.234 1.59 0 5 5 6.35 9.71 2.44 0.045 1.43 1 1 7 20.54 15.69 2.39 0.057 1.70 -2 3 4 88.00 104.58 2.33 0.148 1.86 2 8 5 20.37 27.29 2.33 0.076 0.95 -5 6 1 20.41 26.30 2.29 0.074 1.00 -2 8 1 20.48 26.97 2.27 0.075 1.03 1 5 5 11.76 15.91 2.27 0.058 1.39 4 1 12 16.44 21.97 2.27 0.068 0.87 Bond lengths and angles C1 - Distance Angles N1 1.3378 (0.0017) N2 1.3514 (0.0016) 111.49 (0.11) C2 1.4767 (0.0020) 124.10 (0.12) 124.40 (0.12) C1 - N1 N2 C2 - Distance Angles C1 1.4767 (0.0020) C2 - C3 - Distance Angles N2 1.4696 (0.0016) C4 1.5159 (0.0019) 112.46 (0.10) C3 - N2 C4 - Distance Angles O1 1.4133 (0.0017) C3 1.5159 (0.0019) 111.94 (0.11) C4 - O1 C5 - Distance Angles C6 1.3577 (0.0018) N2 1.3826 (0.0016) 107.93 (0.12) N3 1.4181 (0.0018) 126.72 (0.12) 125.34 (0.11) C5 - C6 N2 C6 - Distance Angles C5 1.3577 (0.0018) N1 1.3580 (0.0019) 108.86 (0.11) C6 - C5 N1 - Distance Angles C1 1.3378 (0.0017) C6 1.3580 (0.0019) 106.37 (0.11) N1 - C1 N2 - Distance Angles C1 1.3514 (0.0016) C5 1.3826 (0.0016) 105.34 (0.10) C3 1.4696 (0.0016) 125.24 (0.11) 129.41 (0.10) N2 - C1 C5 N3 - Distance Angles O3 1.2248 (0.0015) O2 1.2300 (0.0015) 123.60 (0.12) C5 1.4181 (0.0018) 119.87 (0.11) 116.53 (0.11) N3 - O3 O2 O1 - Distance Angles C4 1.4133 (0.0017) O1 - O2 - Distance Angles N3 1.2300 (0.0015) O2 - O3 - Distance Angles N3 1.2248 (0.0015) O3 - FMAP and GRID set by program FMAP 2 2 13 GRID -2.500 -2 -2 2.500 2 2 R1 = 0.0547 for 1725 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.20 at 0.1524 0.1985 0.4252 [ 0.23 A from N1 ] Deepest hole -0.24 at 0.6448 0.2403 0.9540 [ 0.66 A from N3 ] Mean = 0.00, Rms deviation from mean = 0.04 e/A^3, Highest memory used = 1479 / 14496 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2818 -0.0695 0.5161 1.00000 0.05 0.17 0.33 C5 1.10 N3 1.54 C6 1.62 N2 Q2 1 0.1701 -0.0292 0.4866 1.00000 0.05 0.17 0.75 C5 0.94 C6 1.60 H6 1.78 N2 Q3 1 0.1322 0.2494 0.8766 1.00000 0.05 0.16 0.99 H1 1.00 N1 1.81 O1 2.06 C6 Q4 1 0.3132 0.0690 0.7371 1.00000 0.05 0.16 0.69 C3 0.85 C4 1.28 H3A 1.39 H3B Q5 1 0.3163 0.0759 0.6415 1.00000 0.05 0.16 0.71 N2 0.78 C3 1.46 H3B 1.50 H3A Q6 1 0.2735 0.0064 0.4578 1.00000 0.05 0.16 0.73 C6 0.82 C5 1.46 H6 1.72 N1 Q7 1 0.2617 0.3757 0.6582 1.00000 0.05 0.15 0.87 H2C 0.98 H2B 1.01 C2 1.84 H2A Q8 1 0.2836 0.0227 0.5614 1.00000 0.05 0.15 0.64 N2 0.76 C5 1.73 C1 1.83 C6 Q9 1 0.2165 -0.3517 0.3731 1.00000 0.05 0.14 1.38 O2 1.62 H4B 1.66 H4A 1.99 C4 Q10 1 0.1517 0.1999 0.4922 1.00000 0.05 0.14 0.70 C1 0.73 N1 1.77 C6 1.78 N2 Q11 1 0.2407 -0.2629 0.3770 1.00000 0.05 0.14 1.13 O2 2.09 H6 2.11 H4A 2.16 N3 Q12 1 0.1699 0.0019 0.4050 1.00000 0.05 0.13 0.33 C6 0.63 H6 1.55 C5 1.59 N1 Q13 1 0.2640 -0.2329 0.3231 1.00000 0.05 0.13 1.80 O2 1.90 H4A 1.98 H6 2.36 H3A Q14 1 0.2510 -0.1934 0.3800 1.00000 0.05 0.13 1.29 O2 1.56 H6 2.01 N3 2.04 C6 Q15 1 0.0812 0.0046 0.3618 1.00000 0.05 0.13 0.60 H6 1.05 C6 1.84 N1 2.17 O1 Q16 1 0.2764 0.1535 0.5639 1.00000 0.05 0.13 0.66 N2 0.73 C1 1.73 C5 1.79 N1 Q17 1 0.0383 0.4217 0.6044 1.00000 0.05 0.12 0.95 H2C 1.29 H2A 1.34 C2 2.13 H2B Q18 1 0.0638 -0.0224 0.3418 1.00000 0.05 0.11 0.67 H6 1.37 C6 1.82 O1 2.19 N1 Q19 1 0.1375 0.0018 0.3154 1.00000 0.05 0.11 0.66 H6 1.43 C6 1.99 O1 2.19 N1 Q20 1 0.3928 0.0213 0.4459 1.00000 0.05 0.11 1.37 C5 1.43 C6 1.94 H6 2.08 N2 Shortest distances between peaks (including symmetry equivalents) 15 18 0.36 11 14 0.61 18 19 0.67 15 19 0.73 11 13 0.77 9 11 0.79 12 15 0.79 13 14 0.82 6 20 0.86 2 6 0.88 1 2 0.90 6 12 0.95 1 8 0.99 1 6 0.99 12 18 1.07 2 12 1.08 5 8 1.13 8 16 1.13 12 19 1.15 5 16 1.21 4 5 1.23 9 13 1.27 2 8 1.27 10 16 1.27 6 8 1.33 9 14 1.39 1 20 1.46 3 10 1.54 12 20 1.60 1 12 1.68 7 17 1.69 2 15 1.69 8 20 1.71 2 20 1.72 6 15 1.74 12 14 1.82 6 16 1.86 9 17 1.90 6 10 1.94 2 18 1.94 8 10 1.96 2 16 1.98 20 20 1.98 2 10 1.99 6 19 1.99 6 14 2.00 14 18 2.00 6 18 2.01 14 19 2.01 1 16 2.03 1 5 2.04 1 14 2.04 10 12 2.05 2 14 2.08 14 15 2.08 8 12 2.10 16 20 2.10 3 15 2.16 3 12 2.19 2 19 2.21 13 19 2.21 14 20 2.23 8 20 2.28 7 16 2.28 4 8 2.28 3 19 2.29 1 20 2.30 13 18 2.31 4 16 2.33 15 20 2.34 2 5 2.34 19 20 2.34 11 12 2.38 10 20 2.38 11 17 2.39 10 15 2.40 12 13 2.40 5 10 2.40 1 15 2.41 5 6 2.43 11 18 2.44 3 18 2.44 1 11 2.45 2 2 2.45 13 15 2.48 12 16 2.49 7 19 2.49 1 10 2.51 11 19 2.51 3 6 2.52 5 20 2.52 2 11 2.53 6 20 2.54 6 11 2.55 10 17 2.56 11 15 2.56 18 20 2.57 1 18 2.63 5 7 2.63 5 20 2.64 3 16 2.66 7 10 2.68 4 9 2.68 5 18 2.69 6 13 2.69 2 10 2.70 2 15 2.71 3 4 2.75 4 18 2.75 16 20 2.75 1 19 2.76 10 18 2.76 3 20 2.78 8 18 2.78 8 15 2.78 11 20 2.79 2 3 2.80 13 20 2.81 17 19 2.82 8 15 2.82 14 17 2.83 2 12 2.83 5 15 2.83 10 19 2.84 1 13 2.84 2 13 2.85 4 7 2.85 13 17 2.86 2 18 2.86 16 17 2.91 16 18 2.95 8 14 2.98 4 15 2.98 Time profile in seconds ----------------------- 0.16: 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. 1.59: 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 1.81: Structure factors and derivatives 1.02: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.23: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.22: Analysis of variance 0.11: Merge reflections for Fourier and .fcf 0.16: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 16:19:55 Total CPU time: 5.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++