+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008src1291p21c started at 11:16:39 on 20-Feb-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src1291p21c in P2(1)/c CELL 0.71073 20.4469 5.6971 9.6808 90.000 93.743 90.000 ZERR 4.00 0.0013 0.0003 0.0005 0.000 0.004 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O S UNIT 40 60 12 8 4 V = 1125.29 F(000) = 512.0 Mu = 0.28 mm-1 Cell Wt = 965.24 Rho = 1.424 MERG 2 OMIT -3.00 55.00 SHEL 7 0.84 FMAP 2 PLAN 10 SIZE 0.01 0.03 0.23 ACTA 50 BOND $H WGHT 0.00000 6.16990 L.S. 4 TEMP -153.00 FVAR 0.51927 MOLE 1 C2 1 0.104425 0.339855 -0.151813 11.00000 0.02914 0.04000 = 0.03243 -0.00928 -0.00182 -0.00658 AFIX 43 H2 2 0.100096 0.214337 -0.216366 11.00000 -1.20000 AFIX 0 C3 1 0.055783 0.507212 -0.156267 11.00000 0.02258 0.04297 = 0.03011 0.00090 -0.00456 -0.00150 AFIX 43 H3 2 0.019020 0.498551 -0.221340 11.00000 -1.20000 AFIX 0 C4 1 0.062964 0.688680 -0.061473 11.00000 0.02952 0.04087 = 0.03239 0.00435 -0.00223 0.00893 AFIX 43 H4 2 0.030242 0.806846 -0.059824 11.00000 -1.20000 AFIX 0 C5 1 0.117272 0.699293 0.030640 11.00000 0.02742 0.02985 = 0.01807 -0.00459 -0.00162 0.00705 AFIX 43 H5 2 0.122661 0.825448 0.094543 11.00000 -1.20000 AFIX 0 C6 1 0.164197 0.521479 0.028381 11.00000 0.01704 0.02170 = 0.02069 0.00637 0.00393 -0.00518 C8 1 0.222645 0.649874 0.246066 11.00000 0.01933 0.01527 = 0.02435 -0.00238 0.00214 0.00372 AFIX 23 H8A 2 0.203014 0.549231 0.315736 11.00000 -1.20000 H8B 2 0.195750 0.793925 0.234713 11.00000 -1.20000 AFIX 0 C9 1 0.291703 0.715506 0.297247 11.00000 0.02679 0.01956 = 0.02050 -0.00346 -0.00360 0.00471 AFIX 23 H9A 2 0.310473 0.827394 0.232326 11.00000 -1.20000 H9B 2 0.291490 0.791094 0.389299 11.00000 -1.20000 AFIX 0 C11 1 0.332587 0.380566 0.170354 11.00000 0.02543 0.02204 = 0.01457 -0.00429 -0.00186 0.00561 AFIX 23 H11A 2 0.359910 0.237162 0.178555 11.00000 -1.20000 H11B 2 0.351811 0.487312 0.103220 11.00000 -1.20000 AFIX 0 C12 1 0.263493 0.316897 0.119998 11.00000 0.02844 0.01743 = 0.02260 -0.00539 -0.00381 0.00215 AFIX 23 H12A 2 0.263669 0.245264 0.026851 11.00000 -1.20000 H12B 2 0.245766 0.200044 0.183381 11.00000 -1.20000 AFIX 0 C15 1 0.452899 0.706004 0.321599 11.00000 0.01781 0.02795 = 0.02733 0.00740 -0.00187 -0.00038 AFIX 137 H15A 2 0.496140 0.704385 0.371618 11.00000 -1.50000 H15B 2 0.434533 0.864761 0.323624 11.00000 -1.50000 H15C 2 0.457186 0.658262 0.225356 11.00000 -1.50000 AFIX 0 N1 3 0.157870 0.341490 -0.062156 11.00000 0.03170 0.02892 = 0.02632 -0.00464 -0.00224 -0.00242 N7 3 0.221764 0.524805 0.113851 11.00000 0.01755 0.01957 = 0.02475 -0.00103 -0.00049 0.00476 N10 3 0.331625 0.497032 0.306635 11.00000 0.01727 0.01874 = 0.01582 -0.00204 0.00140 0.00010 O13 4 0.428610 0.279433 0.398939 11.00000 0.02760 0.01826 = 0.02523 0.00187 -0.00137 0.00220 O14 4 0.386192 0.609470 0.531583 11.00000 0.02964 0.02278 = 0.01661 0.00091 -0.00132 0.00064 S1 5 0.400635 0.509954 0.400809 11.00000 0.02279 0.01894 = 0.01702 0.00051 0.00101 0.00068 HKLF 4 1.0 0.00 0.00 1.00 0.00 -1.00 0.00 1.00 0.00 0.00 Covalent radii and connectivity table for 2008src1291p21c in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 C2 - N1 C3 C3 - C2 C4 C4 - C5 C3 C5 - C4 C6 C6 - N1 N7 C5 C8 - N7 C9 C9 - N10 C8 C11 - N10 C12 C12 - N7 C11 C15 - S1 N1 - C6 C2 N7 - C6 C12 C8 N10 - C11 C9 S1 O13 - S1 O14 - S1 S1 - O13 O14 N10 C15 11224 Reflections read, of which 2339 rejected -24 =< h =< 24, -6 =< k =< 6, -11 =< l =< 11, Max. 2-theta = 50.05 0 Systematic absence violations 0 Inconsistent equivalents 1981 Unique reflections, of which 0 suppressed R(int) = 0.1029 R(sigma) = 0.0894 Friedel opposites merged Maximum memory for data reduction = 1687 / 19743 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 = 2115 / 184252 wR2 = 0.1769 before cycle 1 for 1981 data and 146 / 146 parameters GooF = S = 1.151; Restrained GooF = 1.151 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 6.17 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.51982 0.00195 0.283 OSF Mean shift/su = 0.228 Maximum = -1.007 for U12 C3 Max. shift = 0.003 A for H8A Max. dU = 0.001 for C5 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2115 / 184252 wR2 = 0.1760 before cycle 2 for 1981 data and 146 / 146 parameters GooF = S = 1.144; Restrained GooF = 1.144 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 6.17 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.52016 0.00194 0.178 OSF Mean shift/su = 0.091 Maximum = -0.436 for U12 C3 Max. shift = 0.001 A for H15C Max. dU = 0.000 for C5 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2115 / 184252 wR2 = 0.1760 before cycle 3 for 1981 data and 146 / 146 parameters GooF = S = 1.143; Restrained GooF = 1.143 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 6.17 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.52019 0.00194 0.013 OSF Mean shift/su = 0.010 Maximum = -0.054 for U12 C3 Max. shift = 0.000 A for C2 Max. dU = 0.000 for N7 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2115 / 184252 wR2 = 0.1760 before cycle 4 for 1981 data and 146 / 146 parameters GooF = S = 1.143; Restrained GooF = 1.143 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 6.17 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.52019 0.00194 0.001 OSF Mean shift/su = 0.002 Maximum = -0.012 for y C3 Max. shift = 0.000 A for C3 Max. dU = 0.000 for C6 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 H2 0.1001 0.2143 -0.2163 43 0.950 0.000 C2 N1 C3 H3 0.0189 0.4991 -0.2212 43 0.950 0.000 C3 C2 C4 H4 0.0303 0.8066 -0.0598 43 0.950 0.000 C4 C5 C3 H5 0.1227 0.8258 0.0944 43 0.950 0.000 C5 C4 C6 H8A 0.2031 0.5501 0.3159 23 0.990 0.000 C8 N7 C9 H8B 0.1959 0.7947 0.2348 23 0.990 0.000 C8 N7 C9 H9A 0.3105 0.8271 0.2320 23 0.990 0.000 C9 N10 C8 H9B 0.2916 0.7913 0.3890 23 0.990 0.000 C9 N10 C8 H11A 0.3597 0.2373 0.1781 23 0.990 0.000 C11 N10 C12 H11B 0.3516 0.4876 0.1030 23 0.990 0.000 C11 N10 C12 H12A 0.2637 0.2455 0.0271 23 0.990 0.000 C12 N7 C11 H12B 0.2459 0.2007 0.1837 23 0.990 0.000 C12 N7 C11 H15A 0.4962 0.7044 0.3713 137 0.980 0.000 C15 S1 H15A H15B 0.4346 0.8650 0.3237 137 0.980 0.000 C15 S1 H15A H15C 0.4571 0.6588 0.2251 137 0.980 0.000 C15 S1 H15A 2008src1291p21c in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C2 0.10446 0.33980 -0.15169 1.00000 0.02896 0.03783 0.03321 -0.00921 -0.00156 -0.00558 0.03349 0.01069 0.00029 0.00120 0.00062 0.00000 0.00364 0.00423 0.00340 0.00308 0.00284 0.00316 0.00159 H2 0.10012 0.21430 -0.21626 1.00000 0.04019 0.00000 0.00000 C3 0.05571 0.50756 -0.15620 1.00000 0.02508 0.04205 0.02671 -0.00088 -0.00469 -0.00685 0.03156 0.01050 0.00027 0.00126 0.00056 0.00000 0.00311 0.00395 0.00298 0.00341 0.00247 0.00355 0.00144 H3 0.01893 0.49905 -0.22122 1.00000 0.03787 0.00000 0.00000 C4 0.06304 0.68845 -0.06153 1.00000 0.03098 0.04228 0.03218 0.00597 -0.00273 0.00906 0.03536 0.01149 0.00031 0.00123 0.00061 0.00000 0.00370 0.00430 0.00342 0.00321 0.00283 0.00323 0.00162 H4 0.03032 0.80662 -0.05984 1.00000 0.04243 0.00000 0.00000 C5 0.11732 0.69952 0.03062 1.00000 0.02795 0.03115 0.02020 -0.00522 -0.00073 0.00675 0.02653 0.01036 0.00028 0.00110 0.00056 0.00000 0.00338 0.00363 0.00285 0.00269 0.00252 0.00290 0.00141 H5 0.12272 0.82584 0.09441 1.00000 0.03184 0.00000 0.00000 C6 0.16422 0.52136 0.02837 1.00000 0.01770 0.01996 0.02030 0.00469 0.00570 -0.00549 0.01912 0.00943 0.00024 0.00104 0.00050 0.00000 0.00272 0.00315 0.00259 0.00261 0.00214 0.00273 0.00119 C8 0.22271 0.65047 0.24615 1.00000 0.01969 0.01727 0.02336 -0.00050 0.00073 0.00292 0.02014 0.00927 0.00026 0.00100 0.00053 0.00000 0.00300 0.00318 0.00289 0.00235 0.00229 0.00246 0.00127 H8A 0.20305 0.55010 0.31591 1.00000 0.02416 0.00000 0.00000 H8B 0.19590 0.79471 0.23476 1.00000 0.02416 0.00000 0.00000 C9 0.29172 0.71549 0.29702 1.00000 0.02880 0.01924 0.02141 -0.00273 -0.00177 0.00301 0.02329 0.00976 0.00027 0.00101 0.00057 0.00000 0.00332 0.00324 0.00284 0.00249 0.00242 0.00269 0.00132 H9A 0.31050 0.82715 0.23198 1.00000 0.02795 0.00000 0.00000 H9B 0.29159 0.79129 0.38902 1.00000 0.02795 0.00000 0.00000 C11 0.33242 0.38072 0.17016 1.00000 0.02542 0.02212 0.01571 -0.00293 -0.00107 0.00689 0.02119 0.00940 0.00027 0.00104 0.00051 0.00000 0.00315 0.00317 0.00262 0.00246 0.00227 0.00267 0.00128 H11A 0.35974 0.23729 0.17812 1.00000 0.02543 0.00000 0.00000 H11B 0.35158 0.48760 0.10300 1.00000 0.02543 0.00000 0.00000 C12 0.26354 0.31739 0.12021 1.00000 0.02775 0.01697 0.02496 -0.00664 -0.00463 0.00156 0.02350 0.00941 0.00027 0.00098 0.00058 0.00000 0.00335 0.00317 0.00297 0.00253 0.00248 0.00268 0.00134 H12A 0.26367 0.24552 0.02713 1.00000 0.02821 0.00000 0.00000 H12B 0.24586 0.20067 0.18373 1.00000 0.02821 0.00000 0.00000 C15 0.45293 0.70626 0.32144 1.00000 0.01701 0.02793 0.02846 0.00664 -0.00096 -0.00138 0.02458 0.01003 0.00026 0.00105 0.00057 0.00000 0.00301 0.00346 0.00304 0.00275 0.00244 0.00268 0.00135 H15A 0.49621 0.70442 0.37128 1.00000 0.03686 0.00000 0.00000 H15B 0.43459 0.86505 0.32370 1.00000 0.03686 0.00000 0.00000 H15C 0.45712 0.65879 0.22512 1.00000 0.03686 0.00000 0.00000 N1 0.15785 0.34126 -0.06214 1.00000 0.02966 0.02928 0.02775 -0.00344 -0.00206 -0.00313 0.02907 0.00834 0.00024 0.00091 0.00048 0.00000 0.00291 0.00319 0.00265 0.00233 0.00222 0.00241 0.00124 N7 0.22175 0.52514 0.11395 1.00000 0.01787 0.01803 0.02424 -0.00088 -0.00173 0.00604 0.02018 0.00778 0.00020 0.00084 0.00043 0.00000 0.00229 0.00264 0.00228 0.00216 0.00186 0.00218 0.00104 N10 0.33163 0.49686 0.30651 1.00000 0.01661 0.02024 0.01607 -0.00029 0.00312 0.00086 0.01755 0.00755 0.00019 0.00087 0.00039 0.00000 0.00220 0.00241 0.00203 0.00220 0.00171 0.00231 0.00095 O13 0.42863 0.27918 0.39905 1.00000 0.02718 0.01712 0.02634 0.00135 -0.00061 0.00255 0.02365 0.00665 0.00018 0.00067 0.00037 0.00000 0.00219 0.00222 0.00205 0.00175 0.00172 0.00178 0.00094 O14 0.38620 0.60924 0.53152 1.00000 0.03029 0.02217 0.01676 0.00044 -0.00065 0.00047 0.02317 0.00651 0.00018 0.00068 0.00035 0.00000 0.00229 0.00219 0.00184 0.00168 0.00162 0.00182 0.00093 S1 0.40063 0.50977 0.40080 1.00000 0.02303 0.01921 0.01746 0.00019 0.00104 0.00001 0.01991 0.00249 0.00007 0.00028 0.00013 0.00000 0.00070 0.00073 0.00062 0.00068 0.00050 0.00071 0.00036 Final Structure Factor Calculation for 2008src1291p21c in P2(1)/c Total number of l.s. parameters = 146 Maximum vector length = 511 Memory required = 1969 / 24017 wR2 = 0.1760 before cycle 5 for 1981 data and 0 / 146 parameters GooF = S = 1.143; Restrained GooF = 1.143 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 6.17 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0876 for 1289 Fo > 4sig(Fo) and 0.1461 for all 1981 data wR2 = 0.1760, GooF = S = 1.143, Restrained GooF = 1.143 for all data Occupancy sum of asymmetric unit = 16.00 for non-hydrogen and 15.00 for hydrogen atoms Principal mean square atomic displacements U 0.0452 0.0338 0.0214 C2 0.0447 0.0315 0.0185 C3 0.0478 0.0366 0.0217 C4 0.0385 0.0230 0.0180 C5 0.0251 0.0233 0.0090 C6 0.0238 0.0213 0.0153 C8 0.0316 0.0210 0.0173 C9 0.0320 0.0171 0.0145 C11 0.0351 0.0223 0.0131 C12 0.0354 0.0216 0.0166 C15 0.0331 0.0320 0.0221 N1 0.0273 0.0214 0.0118 N7 0.0204 0.0182 0.0140 N10 0.0294 0.0253 0.0162 O13 0.0308 0.0222 0.0165 O14 0.0231 0.0192 0.0174 S1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.020 0.030 0.040 0.053 0.067 0.086 0.110 0.151 1.000 Number in group 216. 203. 185. 188. 203. 198. 195. 200. 194. 199. GooF 1.248 1.184 1.252 1.324 1.191 1.248 1.005 1.071 0.996 0.819 K 10.406 2.381 1.455 1.122 1.061 1.035 1.014 1.001 0.996 1.008 Resolution(A) 0.84 0.87 0.91 0.95 0.99 1.06 1.14 1.25 1.43 1.81 inf Number in group 199. 200. 203. 190. 205. 194. 196. 197. 200. 197. GooF 1.357 1.211 1.262 1.172 1.294 1.141 1.040 0.956 0.924 0.971 K 1.161 1.158 1.080 1.075 1.043 0.994 0.999 0.994 1.018 1.002 R1 0.303 0.283 0.287 0.180 0.189 0.127 0.094 0.078 0.068 0.040 Recommended weighting scheme: WGHT 0.0000 5.1503 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)/su Fc/Fc(max) Resolution(A) 8 5 5 215.77 36.23 3.53 0.032 0.91 -18 2 7 316.17 100.54 3.52 0.053 0.86 -16 3 3 268.89 78.44 3.34 0.047 1.02 -2 5 5 164.07 352.66 3.20 0.100 0.98 -4 4 5 186.63 8.25 3.14 0.015 1.13 -9 2 10 149.59 46.49 3.14 0.036 0.87 -17 1 4 114.40 10.99 3.03 0.018 1.08 3 0 10 291.57 20.03 3.02 0.024 0.95 0 2 9 141.67 0.56 2.98 0.004 1.00 6 5 5 285.19 497.80 2.94 0.119 0.93 1 3 8 87.97 0.03 2.92 0.001 1.01 -3 2 10 80.32 0.97 2.91 0.005 0.91 -14 3 8 157.75 22.25 2.87 0.025 0.86 14 2 4 107.12 22.00 2.86 0.025 1.12 11 3 4 106.05 1.85 2.83 0.007 1.14 -2 1 2 111.05 32.73 2.82 0.031 3.52 16 1 6 94.73 0.01 2.77 0.001 0.96 -18 1 2 89.91 0.75 2.72 0.005 1.10 -22 2 2 410.96 233.19 2.70 0.081 0.88 -4 1 11 173.03 47.30 2.65 0.037 0.86 -19 4 2 159.87 29.99 2.64 0.029 0.85 3 3 8 128.60 3.92 2.59 0.011 1.00 17 3 4 31.86 131.38 2.53 0.061 0.92 1 3 4 132.16 18.58 2.53 0.023 1.48 8 2 9 316.46 114.18 2.53 0.057 0.92 -13 2 9 1.86 77.53 2.50 0.047 0.87 9 2 8 107.90 21.25 2.46 0.025 0.98 -3 2 6 63.99 144.63 2.46 0.064 1.39 10 5 0 141.88 42.65 2.45 0.035 0.99 -5 5 7 194.26 82.90 2.44 0.049 0.87 12 3 8 80.03 1.81 2.43 0.007 0.85 4 3 10 165.76 38.77 2.42 0.033 0.84 -14 4 2 357.49 553.83 2.42 0.126 1.01 -8 6 4 394.07 586.76 2.41 0.129 0.84 -16 3 6 124.00 0.39 2.41 0.003 0.91 13 4 6 147.90 29.81 2.41 0.029 0.87 4 3 8 187.57 81.13 2.34 0.048 0.99 7 6 1 102.09 14.98 2.34 0.021 0.90 8 5 0 218.13 106.48 2.32 0.055 1.04 2 6 3 116.69 15.71 2.29 0.021 0.91 8 4 1 61.60 0.08 2.26 0.001 1.23 -18 2 3 -25.84 43.07 2.25 0.035 1.02 -4 4 6 365.00 9.18 2.24 0.016 1.05 19 2 1 77.64 7.70 2.21 0.015 0.99 -2 3 6 -27.15 22.70 2.21 0.025 1.23 -3 1 10 100.48 30.24 2.20 0.029 0.95 -13 4 7 152.52 8.91 2.19 0.016 0.86 7 3 7 337.72 487.84 2.18 0.118 1.02 -15 5 2 199.71 75.75 2.18 0.046 0.87 5 3 6 106.56 7.30 2.18 0.014 1.16 Bond lengths and angles C2 - Distance Angles N1 1.3490 (0.0073) C3 1.3796 (0.0088) 124.66 (0.58) H2 0.9500 117.67 117.67 C2 - N1 C3 C3 - Distance Angles C2 1.3796 (0.0088) C4 1.3807 (0.0088) 116.70 (0.53) H3 0.9500 121.65 121.65 C3 - C2 C4 C4 - Distance Angles C5 1.3793 (0.0080) C3 1.3807 (0.0088) 120.75 (0.60) H4 0.9500 119.62 119.63 C4 - C5 C3 C5 - Distance Angles C4 1.3793 (0.0080) C6 1.3975 (0.0079) 118.73 (0.55) H5 0.9500 120.64 120.63 C5 - C4 C6 C6 - Distance Angles N1 1.3501 (0.0071) N7 1.3940 (0.0064) 116.06 (0.49) C5 1.3975 (0.0079) 121.66 (0.48) 122.19 (0.51) C6 - N1 N7 C8 - Distance Angles N7 1.4646 (0.0065) C9 1.5100 (0.0074) 111.32 (0.43) H8A 0.9900 109.37 109.37 H8B 0.9900 109.37 109.37 107.99 C8 - N7 C9 H8A C9 - Distance Angles N10 1.4886 (0.0070) C8 1.5100 (0.0074) 108.16 (0.45) H9A 0.9900 110.07 110.07 H9B 0.9900 110.07 110.07 108.41 C9 - N10 C8 H9A C11 - Distance Angles N10 1.4776 (0.0063) C12 1.5028 (0.0076) 109.28 (0.44) H11A 0.9900 109.82 109.82 H11B 0.9900 109.82 109.82 108.26 C11 - N10 C12 H11A C12 - Distance Angles N7 1.4587 (0.0069) C11 1.5028 (0.0076) 110.66 (0.45) H12A 0.9900 109.52 109.51 H12B 0.9900 109.52 109.52 108.08 C12 - N7 C11 H12A C15 - Distance Angles S1 1.7591 (0.0055) H15A 0.9800 109.47 H15B 0.9800 109.47 109.47 H15C 0.9800 109.47 109.47 109.47 C15 - S1 H15A H15B N1 - Distance Angles C6 1.3501 (0.0071) C2 1.3490 (0.0073) 117.48 (0.52) N1 - C6 N7 - Distance Angles C6 1.3940 (0.0064) C12 1.4587 (0.0069) 118.78 (0.46) C8 1.4646 (0.0065) 119.31 (0.43) 112.63 (0.41) N7 - C6 C12 N10 - Distance Angles C11 1.4776 (0.0063) C9 1.4886 (0.0070) 110.94 (0.40) S1 1.6312 (0.0041) 117.43 (0.34) 116.58 (0.36) N10 - C11 C9 O13 - Distance Angles S1 1.4336 (0.0040) O13 - O14 - Distance Angles S1 1.4346 (0.0037) O14 - S1 - Distance Angles O13 1.4336 (0.0040) O14 1.4346 (0.0037) 118.53 (0.23) N10 1.6312 (0.0041) 106.47 (0.24) 106.93 (0.22) C15 1.7591 (0.0055) 108.86 (0.26) 107.44 (0.26) 108.21 (0.25) S1 - O13 O14 N10 FMAP and GRID set by program FMAP 2 2 15 GRID 20.833 -2 -1 4.167 2 1 R1 = 0.1455 for 1981 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.39 at 0.4102 0.4968 0.0624 [ 1.29 A from H11B ] Deepest hole -0.40 at 0.2576 0.5687 0.6809 [ 1.30 A from H9A ] Mean = 0.00, Rms deviation from mean = 0.10 e/A^3, Highest memory used = 2285 / 21540 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4102 0.4968 0.0624 1.00000 0.05 0.39 1.29 H11B 2.01 H15C 2.07 C11 2.16 H11A Q2 1 0.4062 0.5337 0.6160 1.00000 0.05 0.37 0.99 O14 1.93 H11A 2.08 S1 2.14 H15B Q3 1 0.3380 0.8024 0.5011 1.00000 0.05 0.37 1.39 H9B 1.49 O14 1.56 H11B 2.19 C9 Q4 1 0.2878 0.7579 0.4229 1.00000 0.05 0.36 0.39 H9B 1.25 C9 1.98 H9A 2.10 N10 Q5 1 0.4404 0.5954 0.3600 1.00000 0.05 0.35 0.79 C15 1.05 S1 1.30 H15A 1.42 H15C Q6 1 0.2867 0.5297 0.4350 1.00000 0.05 0.35 1.56 H9B 1.60 N10 1.71 C9 1.88 H12A Q7 1 0.1692 0.2345 0.0408 1.00000 0.05 0.34 1.18 N1 1.64 C6 1.95 H12A 2.03 H12B Q8 1 0.0870 0.7842 0.1958 1.00000 0.05 0.33 1.28 H5 1.82 C5 2.00 C3 2.06 H3 Q9 1 0.0499 0.9963 0.0387 1.00000 0.05 0.33 1.48 H4 1.83 H5 2.01 H4 2.03 C4 Q10 1 0.5452 0.5864 0.4417 1.00000 0.05 0.32 1.35 H15A 1.77 O13 1.80 O14 1.90 S1 Shortest distances between peaks (including symmetry equivalents) 3 4 1.26 4 6 1.31 2 10 1.36 1 3 1.93 3 6 1.96 8 9 2.05 9 9 2.13 5 10 2.18 5 10 2.24 2 3 2.31 10 10 2.44 1 10 2.51 2 5 2.64 1 2 2.73 7 9 2.79 3 5 2.83 2 6 2.91 1 5 2.96 Time profile in seconds ----------------------- 0.02: 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. 0.50: 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 0.31: 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 0.00: Other dependent quantities, CIF, tables 0.08: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008src1291p21c finished at 11:16:41 Total CPU time: 1.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++