+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008src0131 started at 16:00:41 on 28-Feb-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src0131 in P2(1)/n CELL 0.71073 7.9919 9.1538 17.7888 90.000 98.160 90.000 ZERR 2.00 0.0004 0.0005 0.0007 0.000 0.003 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N S UNIT 56 64 4 8 V = 1288.19 F(000) = 556.0 Mu = 0.39 mm-1 Cell Wt = 1049.59 Rho = 1.353 MERG 2 OMIT -3.00 55.00 TEMP -153 ACTA SIZE 0.25 0.04 0.01 FMAP 2 PLAN 20 BOND WGHT 0.00000 6.40500 L.S. 4 FVAR 0.43533 C1 1 0.482260 -0.038253 -0.078788 11.00000 0.02390 0.02631 = 0.01616 -0.00109 0.00160 -0.00407 AFIX 43 H1 2 0.470746 -0.063973 -0.129840 11.00000 -1.20000 AFIX 0 C2 1 0.425699 0.095703 -0.055899 11.00000 0.01928 0.02789 = 0.01773 0.00279 0.00279 -0.00273 C3 1 0.443244 0.132498 0.022528 11.00000 0.02115 0.02452 = 0.01710 -0.00226 0.00340 -0.00187 C4 1 0.312510 0.317530 -0.066885 11.00000 0.01939 0.02529 = 0.01769 0.00203 0.00239 -0.00505 C5 1 0.236833 0.447135 -0.103066 11.00000 0.02108 0.02416 = 0.01656 0.00300 -0.00088 -0.00067 C6 1 0.122864 0.621461 -0.202774 11.00000 0.03663 0.02870 = 0.02726 0.00156 -0.00285 0.00189 AFIX 43 H6 2 0.083532 0.672543 -0.246952 11.00000 -1.20000 AFIX 0 C7 1 0.125440 0.676430 -0.131683 11.00000 0.03359 0.02252 = 0.02526 -0.00027 0.00155 0.00114 AFIX 43 H7 2 0.088939 0.770323 -0.122380 11.00000 -1.20000 AFIX 0 C8 1 0.188517 0.578267 -0.073097 11.00000 0.01924 0.02789 = 0.02228 -0.00337 0.00306 -0.00393 C9 1 0.202364 0.613018 0.010615 11.00000 0.02200 0.02420 = 0.01955 -0.00137 0.00028 -0.00100 AFIX 23 H9A 2 0.320093 0.605467 0.032857 11.00000 -1.20000 H9B 2 0.139896 0.539827 0.034616 11.00000 -1.20000 AFIX 0 C10 1 0.137054 0.764085 0.028955 11.00000 0.02484 0.02533 = 0.02392 -0.00259 0.00267 -0.00148 AFIX 23 H10A 2 0.016913 0.769756 0.010796 11.00000 -1.20000 H10B 2 0.193474 0.837790 0.002463 11.00000 -1.20000 AFIX 0 C11 1 0.167216 0.796268 0.114229 11.00000 0.02296 0.02809 = 0.02434 0.00138 0.00454 0.00047 AFIX 23 H11A 2 0.115934 0.719809 0.141047 11.00000 -1.20000 H11B 2 0.287750 0.796021 0.131915 11.00000 -1.20000 AFIX 0 C12 1 0.093013 0.944010 0.132399 11.00000 0.03308 0.02567 = 0.02614 0.00217 0.00428 -0.00011 AFIX 23 H12A 2 -0.029093 0.935606 0.127044 11.00000 -1.20000 H12B 2 0.120056 1.015473 0.095699 11.00000 -1.20000 AFIX 0 C13 1 0.158714 0.999328 0.212659 11.00000 0.03569 0.03093 = 0.02924 -0.00199 0.00513 0.00413 AFIX 23 H13A 2 0.279326 1.016548 0.216127 11.00000 -1.20000 H13B 2 0.105296 1.092322 0.220165 11.00000 -1.20000 AFIX 0 C14 1 0.128294 0.898339 0.275417 11.00000 0.07315 0.03943 = 0.03393 0.00372 0.01425 0.01435 AFIX 137 H14A 2 0.011287 0.870607 0.268990 11.00000 -1.50000 H14B 2 0.156896 0.946902 0.323351 11.00000 -1.50000 H14C 2 0.197174 0.812690 0.274191 11.00000 -1.50000 AFIX 0 N1 3 0.351973 0.203509 -0.104519 11.00000 0.01956 0.02524 = 0.01789 -0.00071 0.00171 -0.00164 S1 4 0.362270 0.305136 0.032812 11.00000 0.02611 0.02305 = 0.01821 -0.00101 0.00242 0.00178 S2 4 0.200102 0.448102 -0.201446 11.00000 0.03468 0.02635 = 0.01797 -0.00034 0.00042 0.00013 HKLF 4 Covalent radii and connectivity table for 2008src0131 in P2(1)/n C 0.770 H 0.320 N 0.700 S 1.030 C1 - C2 C3_$1 C2 - N1 C1 C3 C3 - C1_$1 C2 S1 C4 - N1 C5 S1 C5 - C8 C4 S2 C6 - C7 S2 C7 - C6 C8 C8 - C5 C7 C9 C9 - C8 C10 C10 - C9 C11 C11 - C12 C10 C12 - C11 C13 C13 - C14 C12 C14 - C13 N1 - C4 C2 S1 - C3 C4 S2 - C6 C5 Operators for generating equivalent atoms: $1 -x+1, -y, -z 11993 Reflections read, of which 485 rejected -10 =< h =< 9, -11 =< k =< 11, -22 =< l =< 23, 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) 2 4 0 54.15 4.10 7 41.00 2 1 7 255.16 13.93 7 72.49 -2 4 9 61.22 5.57 5 32.85 3 Inconsistent equivalents 2926 Unique reflections, of which 0 suppressed R(int) = 0.0865 R(sigma) = 0.0796 Friedel opposites merged Maximum memory for data reduction = 1686 / 29235 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 = 2141 / 193805 wR2 = 0.1853 before cycle 1 for 2926 data and 155 / 155 parameters GooF = S = 1.185; Restrained GooF = 1.185 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 6.41 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43571 0.00141 0.267 OSF Mean shift/esd = 0.024 Maximum = 0.267 for OSF Max. shift = 0.001 A for H14B Max. dU = 0.000 for C10 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2141 / 193805 wR2 = 0.1853 before cycle 2 for 2926 data and 155 / 155 parameters GooF = S = 1.185; Restrained GooF = 1.185 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 6.41 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43579 0.00141 0.061 OSF Mean shift/esd = 0.009 Maximum = 0.061 for OSF Max. shift = 0.001 A for H14B Max. dU = 0.000 for C14 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2141 / 193805 wR2 = 0.1853 before cycle 3 for 2926 data and 155 / 155 parameters GooF = S = 1.185; Restrained GooF = 1.185 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 6.41 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43579 0.00141 0.000 OSF Mean shift/esd = 0.001 Maximum = 0.003 for tors H14A Max. shift = 0.000 A for H14B Max. dU = 0.000 for C14 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2141 / 193805 wR2 = 0.1853 before cycle 4 for 2926 data and 155 / 155 parameters GooF = S = 1.185; Restrained GooF = 1.185 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 6.41 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.43579 0.00141 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for U11 C8 Max. shift = 0.000 A for H14B Max. dU = 0.000 for C14 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 H1 0.4705 -0.0645 -0.1310 43 0.950 0.000 C1 C2 C3_$1 H6 0.0827 0.6736 -0.2479 43 0.950 0.000 C6 C7 S2 H7 0.0881 0.7724 -0.1222 43 0.950 0.000 C7 C6 C8 H9A 0.3225 0.6053 0.0333 23 0.990 0.000 C9 C8 C10 H9B 0.1386 0.5383 0.0351 23 0.990 0.000 C9 C8 C10 H10A 0.0144 0.7699 0.0104 23 0.990 0.000 C10 C9 C11 H10B 0.1947 0.8393 0.0019 23 0.990 0.000 C10 C9 C11 H11A 0.1149 0.7182 0.1416 23 0.990 0.000 C11 C12 C10 H11B 0.2903 0.7960 0.1323 23 0.990 0.000 C11 C12 C10 H12A -0.0316 0.9355 0.1269 23 0.990 0.000 C12 C11 C13 H12B 0.1206 1.0170 0.0949 23 0.990 0.000 C12 C11 C13 H13A 0.2818 1.0169 0.2162 23 0.990 0.000 C13 C14 C12 H13B 0.1042 1.0943 0.2203 23 0.990 0.000 C13 C14 C12 H14A 0.0089 0.8698 0.2688 137 0.980 0.000 C14 C13 H14A H14B 0.1572 0.9479 0.3244 137 0.980 0.000 C14 C13 H14A H14C 0.1988 0.8110 0.2742 137 0.980 0.000 C14 C13 H14A 2008src0131 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.48226 -0.03826 -0.07881 1.00000 0.02392 0.02622 0.01635 -0.00099 0.00164 -0.00411 0.02228 0.00825 0.00058 0.00053 0.00025 0.00000 0.00239 0.00251 0.00205 0.00188 0.00172 0.00193 0.00098 H1 0.47051 -0.06454 -0.13096 1.00000 0.02674 0.00000 0.00000 C2 0.42570 0.09570 -0.05590 1.00000 0.01931 0.02796 0.01783 0.00278 0.00280 -0.00274 0.02168 0.00833 0.00057 0.00054 0.00024 0.00000 0.00227 0.00252 0.00207 0.00188 0.00171 0.00187 0.00097 C3 0.44324 0.13248 0.02253 1.00000 0.02115 0.02458 0.01722 -0.00227 0.00344 -0.00189 0.02091 0.00806 0.00057 0.00052 0.00024 0.00000 0.00236 0.00246 0.00204 0.00184 0.00172 0.00186 0.00096 C4 0.31251 0.31754 -0.06689 1.00000 0.01939 0.02539 0.01774 0.00206 0.00239 -0.00504 0.02086 0.00803 0.00056 0.00052 0.00024 0.00000 0.00228 0.00251 0.00202 0.00188 0.00167 0.00188 0.00095 C5 0.23683 0.44714 -0.10306 1.00000 0.02117 0.02420 0.01659 0.00299 -0.00084 -0.00070 0.02099 0.00810 0.00057 0.00053 0.00024 0.00000 0.00233 0.00241 0.00203 0.00185 0.00171 0.00188 0.00095 C6 0.12286 0.62148 -0.20280 1.00000 0.03651 0.02871 0.02739 0.00143 -0.00278 0.00180 0.03158 0.00934 0.00068 0.00058 0.00028 0.00000 0.00299 0.00288 0.00251 0.00218 0.00214 0.00230 0.00118 H6 0.08269 0.67365 -0.24793 1.00000 0.03789 0.00000 0.00000 C7 0.12542 0.67648 -0.13169 1.00000 0.03354 0.02270 0.02520 -0.00024 0.00154 0.00104 0.02740 0.00887 0.00064 0.00055 0.00026 0.00000 0.00279 0.00258 0.00232 0.00202 0.00199 0.00210 0.00108 H7 0.08812 0.77239 -0.12219 1.00000 0.03288 0.00000 0.00000 C8 0.18853 0.57827 -0.07309 1.00000 0.01929 0.02794 0.02235 -0.00340 0.00302 -0.00391 0.02319 0.00822 0.00057 0.00055 0.00025 0.00000 0.00234 0.00263 0.00224 0.00194 0.00178 0.00190 0.00101 C9 0.20237 0.61299 0.01063 1.00000 0.02224 0.02420 0.01951 -0.00151 0.00032 -0.00088 0.02224 0.00819 0.00059 0.00052 0.00024 0.00000 0.00238 0.00249 0.00213 0.00188 0.00175 0.00189 0.00098 H9A 0.32252 0.60528 0.03334 1.00000 0.02669 0.00000 0.00000 H9B 0.13859 0.53830 0.03512 1.00000 0.02669 0.00000 0.00000 C10 0.13705 0.76411 0.02894 1.00000 0.02506 0.02542 0.02384 -0.00266 0.00268 -0.00140 0.02485 0.00855 0.00062 0.00053 0.00026 0.00000 0.00243 0.00254 0.00230 0.00199 0.00185 0.00199 0.00102 H10A 0.01443 0.76992 0.01041 1.00000 0.02981 0.00000 0.00000 H10B 0.19466 0.83933 0.00191 1.00000 0.02981 0.00000 0.00000 C11 0.16725 0.79622 0.11424 1.00000 0.02323 0.02807 0.02427 0.00124 0.00458 0.00053 0.02507 0.00877 0.00061 0.00055 0.00026 0.00000 0.00245 0.00259 0.00229 0.00205 0.00186 0.00205 0.00102 H11A 0.11489 0.71818 0.14160 1.00000 0.03009 0.00000 0.00000 H11B 0.29027 0.79597 0.13229 1.00000 0.03009 0.00000 0.00000 C12 0.09299 0.94403 0.13238 1.00000 0.03323 0.02566 0.02609 0.00203 0.00423 -0.00002 0.02832 0.00913 0.00066 0.00056 0.00027 0.00000 0.00283 0.00258 0.00246 0.00212 0.00207 0.00220 0.00109 H12A -0.03164 0.93545 0.12692 1.00000 0.03399 0.00000 0.00000 H12B 0.12059 1.01695 0.09492 1.00000 0.03399 0.00000 0.00000 C13 0.15873 0.99936 0.21266 1.00000 0.03593 0.03094 0.02908 -0.00195 0.00511 0.00405 0.03193 0.00972 0.00071 0.00060 0.00028 0.00000 0.00301 0.00278 0.00256 0.00221 0.00218 0.00234 0.00117 H13A 0.28183 1.01691 0.21620 1.00000 0.03832 0.00000 0.00000 H13B 0.10423 1.09427 0.22033 1.00000 0.03832 0.00000 0.00000 C14 0.12827 0.89831 0.27543 1.00000 0.07295 0.03940 0.03394 0.00375 0.01425 0.01429 0.04812 0.01285 0.00092 0.00070 0.00033 0.00000 0.00470 0.00347 0.00301 0.00264 0.00295 0.00322 0.00163 H14A 0.00888 0.86982 0.26879 1.00000 0.07218 0.00000 0.00000 H14B 0.15721 0.94795 0.32436 1.00000 0.07218 0.00000 0.00000 H14C 0.19878 0.81098 0.27425 1.00000 0.07218 0.00000 0.00000 N1 0.35197 0.20351 -0.10452 1.00000 0.01961 0.02535 0.01794 -0.00073 0.00171 -0.00165 0.02106 0.00676 0.00048 0.00044 0.00020 0.00000 0.00193 0.00208 0.00175 0.00161 0.00143 0.00162 0.00082 S1 0.36227 0.30513 0.03281 1.00000 0.02620 0.02312 0.01827 -0.00101 0.00242 0.00179 0.02260 0.00212 0.00015 0.00013 0.00006 0.00000 0.00062 0.00060 0.00053 0.00047 0.00043 0.00049 0.00029 S2 0.20010 0.44810 -0.20145 1.00000 0.03475 0.02642 0.01803 -0.00033 0.00042 0.00013 0.02672 0.00227 0.00017 0.00014 0.00006 0.00000 0.00071 0.00064 0.00055 0.00048 0.00046 0.00053 0.00032 Final Structure Factor Calculation for 2008src0131 in P2(1)/n Total number of l.s. parameters = 155 Maximum vector length = 511 Memory required = 1986 / 22995 wR2 = 0.1853 before cycle 5 for 2926 data and 0 / 155 parameters GooF = S = 1.185; Restrained GooF = 1.185 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 6.41 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0916 for 2153 Fo > 4sig(Fo) and 0.1282 for all 2926 data wR2 = 0.1853, GooF = S = 1.185, Restrained GooF = 1.185 for all data Occupancy sum of asymmetric unit = 17.00 for non-hydrogen and 16.00 for hydrogen atoms Principal mean square atomic displacements U 0.0294 0.0214 0.0161 C1 0.0296 0.0189 0.0166 C2 0.0259 0.0204 0.0165 C3 0.0289 0.0179 0.0158 C4 0.0265 0.0219 0.0146 C5 0.0418 0.0294 0.0235 C6 0.0348 0.0248 0.0226 C7 0.0304 0.0215 0.0176 C8 0.0247 0.0243 0.0178 C9 0.0275 0.0256 0.0215 C10 0.0285 0.0245 0.0222 C11 0.0333 0.0279 0.0238 C12 0.0384 0.0309 0.0265 C13 0.0786 0.0342 0.0316 C14 0.0258 0.0200 0.0174 N1 0.0273 0.0224 0.0181 S1 0.0360 0.0264 0.0178 S2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.019 0.029 0.040 0.052 0.065 0.083 0.106 0.150 1.000 Number in group 321. 283. 286. 287. 303. 285. 288. 287. 292. 294. GooF 1.479 1.410 1.287 1.186 1.238 1.092 1.125 1.017 0.937 0.915 K 13.134 3.808 1.586 1.183 1.147 1.011 1.032 1.026 1.017 1.007 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.31 1.66 inf Number in group 294. 305. 285. 297. 286. 287. 294. 292. 292. 294. GooF 1.244 1.272 1.095 1.205 1.118 1.036 1.151 1.105 1.326 1.258 K 1.142 1.137 1.103 1.047 1.023 1.034 1.025 1.006 1.025 1.023 R1 0.257 0.226 0.199 0.184 0.150 0.116 0.099 0.075 0.085 0.055 Recommended weighting scheme: WGHT 0.0000 6.3448 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 2 4 615.06 1.61 6.23 0.007 1.61 0 6 6 208.26 6.73 6.09 0.013 1.35 -6 1 4 394.73 0.72 5.59 0.004 1.30 -5 1 3 1436.52 744.28 5.35 0.140 1.56 -3 2 2 273.19 29.15 5.31 0.028 2.28 4 4 10 135.26 3.03 5.29 0.009 1.08 4 1 4 194.24 10.31 5.08 0.016 1.69 6 3 4 322.95 83.25 4.87 0.047 1.13 -5 3 3 248.40 13.21 4.45 0.019 1.41 -2 5 1 354.11 76.79 4.36 0.045 1.66 -1 6 1 2283.45 9.87 4.22 0.016 1.50 -6 7 4 281.78 0.18 4.16 0.002 0.93 -3 5 2 1640.78 1011.25 4.06 0.163 1.50 3 1 14 251.80 0.05 4.06 0.001 1.07 -5 1 4 149.59 14.89 4.05 0.020 1.54 0 5 8 243.29 1.19 3.84 0.006 1.41 3 5 6 323.69 30.28 3.69 0.028 1.30 3 8 4 537.34 101.66 3.40 0.052 1.01 -5 2 3 358.13 183.70 3.27 0.070 1.50 -3 3 2 805.73 525.00 3.27 0.118 1.99 -7 7 8 379.90 161.25 3.20 0.065 0.83 4 5 16 95.54 0.95 3.17 0.005 0.81 0 2 7 702.55 165.97 3.15 0.066 2.20 -5 9 4 140.82 2.17 3.13 0.008 0.85 -7 7 6 228.68 52.94 3.10 0.037 0.85 0 3 7 171.26 19.00 3.05 0.022 1.94 -5 6 12 62.67 170.39 3.00 0.067 0.92 -5 6 16 277.91 97.18 3.00 0.051 0.82 6 6 6 25.31 127.23 2.96 0.058 0.92 3 5 13 59.48 0.44 2.92 0.003 0.97 -4 9 3 567.74 302.33 2.87 0.089 0.90 0 3 16 336.22 60.84 2.81 0.040 1.04 0 6 15 148.59 10.44 2.80 0.017 0.93 -3 10 10 231.74 49.21 2.80 0.036 0.79 0 6 18 231.95 11.60 2.79 0.017 0.82 -1 5 1 992.41 649.06 2.79 0.131 1.78 -6 1 11 161.80 42.37 2.78 0.033 1.09 -5 3 4 146.10 2.42 2.76 0.008 1.39 -4 2 3 5287.94 4425.22 2.76 0.341 1.80 -3 7 13 116.55 26.44 2.74 0.026 0.92 -3 2 1 1421.80 379.87 2.72 0.100 2.30 -4 9 7 117.78 6.51 2.70 0.013 0.87 7 6 10 87.00 2.56 2.68 0.008 0.77 1 6 19 562.20 252.95 2.68 0.082 0.78 7 4 7 78.52 184.12 2.66 0.070 0.90 6 7 3 195.63 80.63 2.65 0.046 0.90 3 1 6 1864.59 1504.01 2.65 0.199 1.80 1 10 0 213.41 52.63 2.65 0.037 0.91 -10 2 7 154.54 10.54 2.64 0.017 0.78 -6 4 4 479.07 307.66 2.60 0.090 1.14 Bond lengths and angles C1 - Distance Angles C2 1.3880 (0.0068) C3_$1 1.3897 (0.0064) 117.44 (0.40) C1 - C2 C2 - Distance Angles N1 1.3873 (0.0059) C1 1.3880 (0.0068) 124.94 (0.40) C3 1.4227 (0.0060) 114.65 (0.42) 120.41 (0.42) C2 - N1 C1 C3 - Distance Angles C1_$1 1.3897 (0.0064) C2 1.4227 (0.0060) 122.15 (0.43) S1 1.7273 (0.0048) 128.33 (0.35) 109.52 (0.34) C3 - C1_$1 C2 C4 - Distance Angles N1 1.3027 (0.0061) C5 1.4411 (0.0063) 123.16 (0.39) S1 1.7652 (0.0044) 115.36 (0.35) 121.46 (0.34) C4 - N1 C5 C5 - Distance Angles C8 1.3901 (0.0067) C4 1.4411 (0.0064) 131.41 (0.40) S2 1.7331 (0.0043) 111.50 (0.34) 117.08 (0.34) C5 - C8 C4 C6 - Distance Angles C7 1.3589 (0.0069) S2 1.7018 (0.0054) 112.02 (0.39) C6 - C7 C7 - Distance Angles C6 1.3589 (0.0069) C8 1.4142 (0.0067) 114.03 (0.46) C7 - C6 C8 - Distance Angles C5 1.3901 (0.0067) C7 1.4142 (0.0067) 110.83 (0.40) C9 1.5115 (0.0060) 125.03 (0.42) 124.14 (0.44) C8 - C5 C7 C9 - Distance Angles C8 1.5115 (0.0060) C10 1.5299 (0.0065) 114.87 (0.39) C9 - C8 C10 - Distance Angles C9 1.5299 (0.0065) C11 1.5307 (0.0063) 111.97 (0.39) C10 - C9 C11 - Distance Angles C12 1.5302 (0.0068) C10 1.5307 (0.0063) 111.57 (0.39) C11 - C12 C12 - Distance Angles C11 1.5302 (0.0069) C13 1.5359 (0.0067) 113.32 (0.41) C12 - C11 C13 - Distance Angles C14 1.4962 (0.0076) C12 1.5359 (0.0067) 114.81 (0.48) C13 - C14 C14 - Distance Angles C13 1.4962 (0.0076) C14 - N1 - Distance Angles C4 1.3027 (0.0061) C2 1.3873 (0.0060) 111.22 (0.37) N1 - C4 S1 - Distance Angles C3 1.7273 (0.0048) C4 1.7652 (0.0044) 89.25 (0.22) S1 - C3 S2 - Distance Angles C6 1.7018 (0.0054) C5 1.7331 (0.0043) 91.61 (0.24) S2 - C6 FMAP and GRID set by program FMAP 2 3 22 GRID -1.316 -2 -2 1.316 2 2 R1 = 0.1276 for 2926 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.44 at 0.8241 0.5363 0.1594 [ 0.81 A from S2 ] Deepest hole -0.45 at 0.5463 0.7124 0.0274 [ 1.27 A from C4 ] Mean = 0.00, Rms deviation from mean = 0.10 e/A^3, Highest memory used = 1962 / 16974 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1759 0.4637 -0.1594 1.00000 0.05 0.44 0.81 S2 1.06 C5 1.66 C6 1.85 C8 Q2 1 0.3661 0.3369 -0.0235 1.00000 0.05 0.42 0.85 C4 1.05 S1 1.88 N1 1.92 C5 Q3 1 0.4447 -0.1946 -0.1447 1.00000 0.05 0.42 1.23 H1 1.85 C1 2.30 C3 2.33 H14A Q4 1 0.0372 0.7893 0.3313 1.00000 0.05 0.41 1.33 H14A 1.65 C14 1.75 H14B 1.76 H14C Q5 1 0.0403 0.8126 0.3145 1.00000 0.05 0.41 0.97 H14A 1.32 C14 1.54 H14C 1.55 H14B Q6 1 0.2159 0.3111 -0.2147 1.00000 0.05 0.40 1.29 S2 2.22 H6 2.32 N1 2.33 C5 Q7 1 0.1817 0.2154 0.0440 1.00000 0.05 0.40 1.70 S1 1.73 H10A 2.12 H12B 2.31 C3 Q8 1 0.3174 -0.1944 -0.1690 1.00000 0.05 0.39 1.77 H1 2.12 C7 2.14 H7 2.31 C6 Q9 1 0.0714 0.4603 -0.0674 1.00000 0.05 0.38 1.44 C8 1.55 C5 1.85 H9B 1.96 H9B Q10 1 0.3859 -0.0611 -0.1505 1.00000 0.05 0.37 0.72 H1 1.41 C1 2.20 C2 2.57 C3 Q11 1 0.2328 0.2433 -0.1516 1.00000 0.05 0.36 1.23 N1 1.69 C4 2.05 C5 2.07 S2 Q12 1 0.1686 1.0474 0.0805 1.00000 0.05 0.35 0.56 H12B 1.51 C12 2.16 H12A 2.38 C11 Q13 1 0.4836 0.0445 -0.0721 1.00000 0.05 0.35 0.75 C2 0.77 C1 1.44 H1 1.84 N1 Q14 1 0.0487 0.9441 0.2074 1.00000 0.05 0.34 1.01 C13 1.35 C14 1.36 H14A 1.43 C12 Q15 1 0.4382 0.1217 -0.0183 1.00000 0.05 0.34 0.70 C2 0.73 C3 1.76 N1 1.88 C1 Q16 1 -0.0476 0.8184 0.2135 1.00000 0.05 0.33 1.13 H14A 1.81 C14 1.90 H12A 2.11 H14C Q17 1 0.2125 0.5572 -0.1793 1.00000 0.05 0.32 0.97 C6 1.07 S2 1.60 C7 1.68 C5 Q18 1 -0.0363 0.6364 -0.1313 1.00000 0.05 0.32 1.34 C7 1.59 H7 1.93 C6 2.01 C8 Q19 1 0.3151 0.5612 -0.2092 1.00000 0.05 0.32 1.40 S2 1.65 C6 1.77 H14A 2.15 H6 Q20 1 0.4538 0.3994 -0.1040 1.00000 0.05 0.32 1.58 C4 1.79 C5 1.97 N1 2.03 H9A Shortest distances between peaks (including symmetry equivalents) 4 5 0.37 1 17 0.99 17 19 1.04 3 8 1.05 3 4 1.25 6 11 1.27 13 15 1.28 3 10 1.31 8 10 1.36 14 16 1.40 3 5 1.56 7 12 1.68 1 19 1.76 1 6 1.76 2 20 1.78 10 13 1.78 6 16 1.79 11 16 1.81 5 16 1.83 1 9 1.94 4 8 1.96 6 8 2.05 2 15 2.05 1 11 2.07 9 18 2.09 4 16 2.12 5 19 2.13 5 8 2.14 16 19 2.18 13 15 2.24 5 14 2.26 4 19 2.28 2 7 2.31 11 20 2.34 6 17 2.34 8 19 2.35 1 20 2.37 17 18 2.39 6 19 2.42 8 17 2.42 1 18 2.42 4 10 2.46 7 18 2.47 15 15 2.49 19 20 2.52 2 11 2.52 3 13 2.54 14 19 2.54 9 17 2.58 7 15 2.61 17 20 2.62 2 9 2.63 4 14 2.63 3 6 2.65 6 19 2.65 3 19 2.65 6 20 2.66 13 13 2.67 6 10 2.69 5 10 2.72 8 16 2.73 12 14 2.74 5 6 2.76 3 16 2.77 4 6 2.84 10 15 2.87 9 9 2.89 11 14 2.89 1 16 2.89 5 17 2.89 9 11 2.90 11 15 2.91 1 2 2.91 11 17 2.92 11 13 2.92 12 13 2.93 4 17 2.93 3 17 2.94 11 19 2.96 15 20 2.98 8 13 2.98 10 19 2.99 3 15 2.99 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 0.02: Analyse other restraints etc. 2.28: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.48: Structure factors and derivatives 0.53: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.05: Apply other restraints 0.22: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.08: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.08: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008src0131 finished at 16:00:45 Total CPU time: 4.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++