+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0067p21c started at 09:15:46 on 02-Feb-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0067p21c in P2(1)/c CELL 0.71073 15.1518 6.1889 11.2790 90.000 109.004 90.000 ZERR 4.00 0.0005 0.0002 0.0003 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 40 56 16 4 V = 1000.02 F(000) = 440.0 Mu = 0.09 mm-1 Cell Wt = 825.01 Rho = 1.370 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 FMAP 2 PLAN 10 SIZE 0.13 0.06 0.04 ACTA HTAB BOND $H WGHT 0.01920 1.28800 L.S. 4 TEMP -153.00 FVAR 0.80432 MOLE 1 C2 1 0.103914 1.712777 0.549733 11.00000 0.02692 0.02101 = 0.02387 -0.00243 0.01061 -0.00001 AFIX 43 H2 2 0.103578 1.789215 0.622626 11.00000 -1.20000 AFIX 0 C3 1 0.030339 1.743860 0.439943 11.00000 0.02270 0.02303 = 0.02878 -0.00054 0.00907 0.00260 AFIX 43 H3 2 -0.020142 1.837864 0.435818 11.00000 -1.20000 AFIX 0 C4 1 0.034700 1.630407 0.337105 11.00000 0.02077 0.02092 = 0.02282 0.00300 0.00232 -0.00051 AFIX 43 H4 2 -0.014852 1.647403 0.260237 11.00000 -1.20000 AFIX 0 C6 1 0.172973 1.478006 0.451784 11.00000 0.02123 0.01485 = 0.01773 0.00269 0.00698 -0.00149 C8 1 0.251213 1.222848 0.349151 11.00000 0.02215 0.02594 = 0.01369 -0.00104 0.00542 0.00511 AFIX 23 H8A 2 0.307429 1.270704 0.329967 11.00000 -1.20000 H8B 2 0.195864 1.253412 0.275132 11.00000 -1.20000 AFIX 0 C9 1 0.257386 0.981457 0.375996 11.00000 0.02291 0.02218 = 0.01802 -0.00268 0.00341 0.00176 AFIX 23 H9A 2 0.197332 0.929558 0.382513 11.00000 -1.20000 H9B 2 0.269237 0.903548 0.306014 11.00000 -1.20000 AFIX 0 C11 1 0.325222 1.056717 0.600336 11.00000 0.02278 0.02258 = 0.01425 -0.00129 0.00493 0.00283 AFIX 23 H11A 2 0.379891 1.025193 0.675078 11.00000 -1.20000 H11B 2 0.268212 1.012396 0.618635 11.00000 -1.20000 AFIX 0 C12 1 0.321188 1.298458 0.571611 11.00000 0.01972 0.02309 = 0.01547 -0.00272 0.00356 0.00253 AFIX 23 H12A 2 0.312284 1.380570 0.642189 11.00000 -1.20000 H12B 2 0.380629 1.345552 0.561055 11.00000 -1.20000 AFIX 0 C13 1 0.402978 0.800636 0.494595 11.00000 0.02371 0.01752 = 0.02051 0.00221 0.00772 -0.00149 C14 1 0.477549 0.759833 0.619122 11.00000 0.02421 0.02150 = 0.02404 0.00135 0.00614 0.00380 AFIX 137 H14A 2 0.516212 0.637276 0.611228 11.00000 -1.50000 H14B 2 0.448108 0.726952 0.682568 11.00000 -1.50000 H14C 2 0.516728 0.888788 0.644397 11.00000 -1.50000 AFIX 0 N1 3 0.175100 1.581103 0.558218 11.00000 0.02419 0.01954 = 0.02082 -0.00151 0.00876 0.00065 N5 3 0.104638 1.497879 0.339339 11.00000 0.02218 0.01871 = 0.01883 0.00054 0.00395 0.00131 N7 3 0.244056 1.341462 0.457191 11.00000 0.02375 0.02298 = 0.01386 -0.00098 0.00351 0.00527 N10 3 0.332468 0.935870 0.492828 11.00000 0.02626 0.02047 = 0.01465 -0.00115 0.00362 0.00353 O15 4 0.406896 0.713787 0.397890 11.00000 0.03718 0.03079 = 0.02234 -0.00232 0.01086 0.00829 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 2009src0067p21c in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 C2 - N1 C3 C3 - C4 C2 C4 - N5 C3 C6 - N1 N7 N5 C8 - N7 C9 C9 - N10 C8 C11 - N10 C12 C12 - N7 C11 C13 - O15 N10 C14 C14 - C13 N1 - C2 C6 N5 - C4 C6 N7 - C6 C12 C8 N10 - C13 C11 C9 O15 - C13 12763 Reflections read, of which 790 rejected -19 =< h =< 19, -8 =< k =< 7, -14 =< l =< 14, Max. 2-theta = 54.95 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 9 5 3 3.53 1.07 2 5.43 1 Inconsistent equivalents 2280 Unique reflections, of which 0 suppressed R(int) = 0.0478 R(sigma) = 0.0416 Friedel opposites merged Maximum memory for data reduction = 1582 / 23120 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 = 1983 / 172736 wR2 = 0.1219 before cycle 1 for 2280 data and 137 / 137 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0192 * P )^2 + 1.29 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.80389 0.00191 -0.227 OSF Mean shift/su = 0.162 Maximum = -0.556 for U33 N1 Max. shift = 0.002 A for H14C Max. dU = 0.000 for C9 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1983 / 172736 wR2 = 0.1216 before cycle 2 for 2280 data and 137 / 137 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0192 * P )^2 + 1.29 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.80349 0.00190 -0.209 OSF Mean shift/su = 0.056 Maximum = -0.209 for OSF Max. shift = 0.001 A for H14A Max. dU = 0.000 for N10 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1983 / 172736 wR2 = 0.1216 before cycle 3 for 2280 data and 137 / 137 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0192 * P )^2 + 1.29 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.80349 0.00190 0.001 OSF Mean shift/su = 0.003 Maximum = 0.013 for y C9 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C2 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1983 / 172736 wR2 = 0.1216 before cycle 4 for 2280 data and 137 / 137 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0192 * P )^2 + 1.29 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.80350 0.00190 0.004 OSF Mean shift/su = 0.001 Maximum = 0.005 for U22 C2 Max. shift = 0.000 A for N5 Max. dU = 0.000 for C2 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 0.1036 1.7889 0.6227 43 0.950 0.000 C2 N1 C3 H3 -0.0201 1.8378 0.4359 43 0.950 0.000 C3 C4 C2 H4 -0.0148 1.6474 0.2602 43 0.950 0.000 C4 N5 C3 H8A 0.3074 1.2706 0.3299 23 0.990 0.000 C8 N7 C9 H8B 0.1959 1.2533 0.2751 23 0.990 0.000 C8 N7 C9 H9A 0.1973 0.9297 0.3825 23 0.990 0.000 C9 N10 C8 H9B 0.2693 0.9037 0.3060 23 0.990 0.000 C9 N10 C8 H11A 0.3798 1.0253 0.6751 23 0.990 0.000 C11 N10 C12 H11B 0.2681 1.0125 0.6186 23 0.990 0.000 C11 N10 C12 H12A 0.3122 1.3805 0.6422 23 0.990 0.000 C12 N7 C11 H12B 0.3806 1.3454 0.5611 23 0.990 0.000 C12 N7 C11 H14A 0.5160 0.6370 0.6112 137 0.980 0.000 C14 C13 H14A H14B 0.4481 0.7274 0.6826 137 0.980 0.000 C14 C13 H14A H14C 0.5168 0.8886 0.6442 137 0.980 0.000 C14 C13 H14A 2009src0067p21c in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C2 0.10393 1.71264 0.54979 1.00000 0.02691 0.02081 0.02411 -0.00254 0.01097 -0.00013 0.02330 0.00388 0.00013 0.00032 0.00018 0.00000 0.00098 0.00100 0.00094 0.00081 0.00080 0.00082 0.00042 H2 0.10355 1.78893 0.62271 1.00000 0.02796 0.00000 0.00000 C3 0.03039 1.74381 0.44001 1.00000 0.02243 0.02238 0.02906 -0.00038 0.00922 0.00270 0.02442 0.00391 0.00013 0.00033 0.00018 0.00000 0.00096 0.00103 0.00100 0.00083 0.00081 0.00080 0.00044 H3 -0.02008 1.83785 0.43589 1.00000 0.02930 0.00000 0.00000 C4 0.03474 1.63040 0.33710 1.00000 0.02069 0.02057 0.02295 0.00309 0.00227 -0.00037 0.02258 0.00378 0.00013 0.00032 0.00018 0.00000 0.00091 0.00098 0.00093 0.00078 0.00074 0.00078 0.00042 H4 -0.01481 1.64744 0.26023 1.00000 0.02709 0.00000 0.00000 C6 0.17298 1.47796 0.45175 1.00000 0.02118 0.01451 0.01773 0.00269 0.00702 -0.00173 0.01764 0.00352 0.00012 0.00029 0.00016 0.00000 0.00088 0.00088 0.00086 0.00071 0.00071 0.00074 0.00038 C8 0.25121 1.22277 0.34911 1.00000 0.02206 0.02551 0.01340 -0.00111 0.00529 0.00458 0.02044 0.00373 0.00013 0.00032 0.00016 0.00000 0.00090 0.00103 0.00081 0.00076 0.00070 0.00079 0.00041 H8A 0.30742 1.27064 0.32992 1.00000 0.02453 0.00000 0.00000 H8B 0.19586 1.25328 0.27509 1.00000 0.02453 0.00000 0.00000 C9 0.25741 0.98165 0.37598 1.00000 0.02242 0.02249 0.01739 -0.00253 0.00324 0.00173 0.02155 0.00367 0.00013 0.00032 0.00017 0.00000 0.00093 0.00101 0.00088 0.00076 0.00073 0.00079 0.00042 H9A 0.19735 0.92974 0.38247 1.00000 0.02586 0.00000 0.00000 H9B 0.26927 0.90374 0.30600 1.00000 0.02586 0.00000 0.00000 C11 0.32516 1.05682 0.60035 1.00000 0.02298 0.02250 0.01402 -0.00137 0.00495 0.00275 0.02009 0.00364 0.00013 0.00031 0.00016 0.00000 0.00092 0.00100 0.00082 0.00075 0.00069 0.00079 0.00040 H11A 0.37979 1.02528 0.67513 1.00000 0.02411 0.00000 0.00000 H11B 0.26812 1.01250 0.61858 1.00000 0.02411 0.00000 0.00000 C12 0.32115 1.29837 0.57166 1.00000 0.01956 0.02286 0.01554 -0.00260 0.00348 0.00238 0.01986 0.00359 0.00013 0.00031 0.00016 0.00000 0.00089 0.00099 0.00084 0.00075 0.00071 0.00077 0.00040 H12A 0.31223 1.38047 0.64223 1.00000 0.02384 0.00000 0.00000 H12B 0.38060 1.34544 0.56114 1.00000 0.02384 0.00000 0.00000 C13 0.40296 0.80060 0.49468 1.00000 0.02355 0.01745 0.02050 0.00223 0.00775 -0.00163 0.02036 0.00368 0.00013 0.00031 0.00017 0.00000 0.00093 0.00093 0.00091 0.00076 0.00076 0.00077 0.00040 C14 0.47751 0.75982 0.61905 1.00000 0.02377 0.02161 0.02408 0.00102 0.00632 0.00359 0.02351 0.00385 0.00013 0.00033 0.00018 0.00000 0.00096 0.00101 0.00096 0.00081 0.00080 0.00081 0.00043 H14A 0.51603 0.63697 0.61118 1.00000 0.03527 0.00000 0.00000 H14B 0.44810 0.72739 0.68259 1.00000 0.03527 0.00000 0.00000 H14C 0.51681 0.88861 0.64417 1.00000 0.03527 0.00000 0.00000 N1 0.17515 1.58108 0.55828 1.00000 0.02408 0.01949 0.02025 -0.00126 0.00876 0.00080 0.02090 0.00311 0.00011 0.00026 0.00014 0.00000 0.00080 0.00083 0.00077 0.00066 0.00063 0.00066 0.00036 N5 0.10466 1.49794 0.33933 1.00000 0.02167 0.01887 0.01862 0.00075 0.00380 0.00137 0.02039 0.00302 0.00011 0.00026 0.00014 0.00000 0.00079 0.00083 0.00076 0.00065 0.00062 0.00065 0.00036 N7 0.24404 1.34148 0.45721 1.00000 0.02363 0.02283 0.01353 -0.00100 0.00344 0.00544 0.02063 0.00307 0.00011 0.00027 0.00014 0.00000 0.00081 0.00085 0.00072 0.00063 0.00062 0.00068 0.00036 N10 0.33247 0.93597 0.49282 1.00000 0.02589 0.02031 0.01437 -0.00119 0.00358 0.00354 0.02091 0.00305 0.00011 0.00026 0.00014 0.00000 0.00083 0.00084 0.00072 0.00064 0.00061 0.00068 0.00036 O15 0.40688 0.71374 0.39782 1.00000 0.03704 0.03064 0.02220 -0.00243 0.01095 0.00835 0.02964 0.00292 0.00010 0.00024 0.00013 0.00000 0.00082 0.00084 0.00071 0.00063 0.00062 0.00068 0.00036 Final Structure Factor Calculation for 2009src0067p21c in P2(1)/c Total number of l.s. parameters = 137 Maximum vector length = 511 Memory required = 1846 / 22995 wR2 = 0.1216 before cycle 5 for 2280 data and 0 / 137 parameters GooF = S = 1.049; Restrained GooF = 1.049 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0192 * P )^2 + 1.29 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0564 for 1793 Fo > 4sig(Fo) and 0.0780 for all 2280 data wR2 = 0.1216, GooF = S = 1.049, Restrained GooF = 1.049 for all data Occupancy sum of asymmetric unit = 15.00 for non-hydrogen and 14.00 for hydrogen atoms Principal mean square atomic displacements U 0.0281 0.0233 0.0185 C2 0.0291 0.0250 0.0191 C3 0.0302 0.0203 0.0173 C4 0.0218 0.0192 0.0119 C6 0.0294 0.0189 0.0130 C8 0.0278 0.0208 0.0161 C9 0.0266 0.0200 0.0137 C11 0.0264 0.0185 0.0147 C12 0.0241 0.0217 0.0153 C13 0.0273 0.0244 0.0188 C14 0.0243 0.0209 0.0175 N1 0.0247 0.0195 0.0170 N5 0.0305 0.0179 0.0134 N7 0.0300 0.0186 0.0141 N10 0.0435 0.0270 0.0183 O15 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.017 0.024 0.033 0.044 0.057 0.076 0.101 0.148 1.000 Number in group 232. 249. 203. 229. 235. 226. 225. 234. 218. 229. GooF 1.037 1.060 1.171 1.118 1.000 1.074 1.082 0.964 0.964 1.018 K 5.817 1.324 1.052 1.093 0.982 1.015 0.997 0.998 1.004 0.998 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.65 inf Number in group 230. 229. 226. 232. 226. 228. 224. 229. 226. 230. GooF 1.170 1.212 1.076 1.110 1.008 0.935 0.914 0.819 0.952 1.209 K 1.055 1.080 1.079 0.996 1.012 0.990 1.003 0.999 1.022 0.988 R1 0.203 0.188 0.153 0.123 0.090 0.068 0.049 0.042 0.042 0.033 Recommended weighting scheme: WGHT 0.0134 1.2857 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) 0 0 6 26.19 4.98 4.03 0.018 1.78 -10 6 6 52.66 112.88 3.66 0.084 0.82 -3 0 2 241.88 322.39 3.64 0.142 4.33 -4 3 9 136.09 193.19 3.42 0.110 1.07 4 6 5 7.83 33.91 3.30 0.046 0.87 10 4 7 96.52 55.56 3.11 0.059 0.78 6 6 5 27.04 59.37 3.06 0.061 0.83 -10 2 2 17.66 5.36 2.97 0.018 1.36 -3 7 4 210.87 141.92 2.95 0.094 0.84 13 2 6 -3.87 11.14 2.88 0.026 0.80 0 5 8 35.56 64.26 2.88 0.063 0.91 -4 6 5 34.59 60.92 2.84 0.062 0.93 11 0 6 16.55 4.18 2.84 0.016 0.92 -4 2 14 83.40 49.89 2.81 0.056 0.77 5 0 0 21.36 7.80 2.80 0.022 2.87 -1 1 2 352.02 423.58 2.80 0.163 4.17 0 0 2 14246.42 15605.96 2.74 0.989 5.33 -9 1 3 609.70 523.00 2.72 0.181 1.61 -11 6 5 34.17 64.99 2.68 0.064 0.81 2 2 5 61.69 91.31 2.67 0.076 1.61 3 0 2 105.92 76.09 2.63 0.069 3.09 -18 3 3 20.78 3.80 2.63 0.015 0.78 8 1 7 35.90 58.38 2.62 0.060 1.00 -5 2 7 69.32 45.90 2.61 0.054 1.40 3 1 5 1192.42 1064.45 2.61 0.258 1.68 10 3 8 82.83 47.13 2.61 0.054 0.78 4 3 11 -5.02 8.27 2.60 0.023 0.80 -18 0 6 38.00 13.72 2.59 0.029 0.83 2 0 12 11.59 0.60 2.56 0.006 0.85 -1 1 1 2187.40 2402.27 2.52 0.388 5.31 2 1 4 199.41 159.13 2.52 0.100 2.13 -2 1 3 1060.40 1183.12 2.49 0.272 3.18 5 5 7 78.32 49.57 2.48 0.056 0.86 -17 3 1 175.21 129.36 2.47 0.090 0.80 13 0 6 13.31 32.13 2.46 0.045 0.82 -15 4 7 254.66 188.15 2.45 0.109 0.82 10 5 5 121.55 173.89 2.42 0.104 0.80 7 1 0 53.29 34.48 2.41 0.046 1.94 6 6 4 15.91 2.20 2.39 0.012 0.86 -6 6 8 40.18 11.68 2.39 0.027 0.82 -2 2 5 986.14 880.16 2.38 0.235 1.82 14 4 2 17.82 4.28 2.38 0.016 0.81 -15 4 9 42.07 11.28 2.37 0.027 0.78 3 0 0 875.57 983.11 2.35 0.248 4.78 3 4 10 13.20 1.05 2.34 0.008 0.83 -17 2 4 -0.33 6.66 2.32 0.020 0.86 -11 4 11 63.05 35.60 2.32 0.047 0.80 4 5 9 35.19 62.60 2.31 0.063 0.79 1 3 12 29.68 11.10 2.30 0.026 0.80 -3 5 9 38.21 13.06 2.30 0.029 0.88 Bond lengths and angles C2 - Distance Angles N1 1.3302 (0.0025) C3 1.3833 (0.0027) 123.23 (0.18) H2 0.9500 118.39 118.39 C2 - N1 C3 C3 - Distance Angles C4 1.3763 (0.0028) C2 1.3833 (0.0027) 115.97 (0.18) H3 0.9500 122.01 122.01 C3 - C4 C2 C4 - Distance Angles N5 1.3333 (0.0025) C3 1.3763 (0.0028) 123.62 (0.17) H4 0.9500 118.19 118.19 C4 - N5 C3 C6 - Distance Angles N1 1.3514 (0.0024) N7 1.3540 (0.0024) 117.73 (0.16) N5 1.3564 (0.0023) 125.34 (0.17) 116.93 (0.16) C6 - N1 N7 C8 - Distance Angles N7 1.4575 (0.0023) C9 1.5195 (0.0027) 110.17 (0.15) H8A 0.9900 109.62 109.62 H8B 0.9900 109.62 109.62 108.14 C8 - N7 C9 H8A C9 - Distance Angles N10 1.4608 (0.0023) C8 1.5195 (0.0027) 110.44 (0.15) H9A 0.9900 109.56 109.56 H9B 0.9900 109.56 109.56 108.11 C9 - N10 C8 H9A C11 - Distance Angles N10 1.4595 (0.0023) C12 1.5265 (0.0027) 109.53 (0.15) H11A 0.9900 109.77 109.77 H11B 0.9900 109.77 109.77 108.23 C11 - N10 C12 H11A C12 - Distance Angles N7 1.4562 (0.0022) C11 1.5265 (0.0027) 109.42 (0.15) H12A 0.9900 109.79 109.79 H12B 0.9900 109.79 109.79 108.24 C12 - N7 C11 H12A C13 - Distance Angles O15 1.2362 (0.0023) N10 1.3522 (0.0024) 121.38 (0.17) C14 1.5085 (0.0025) 120.81 (0.17) 117.81 (0.16) C13 - O15 N10 C14 - Distance Angles C13 1.5085 (0.0025) H14A 0.9800 109.47 H14B 0.9800 109.47 109.47 H14C 0.9800 109.47 109.47 109.47 C14 - C13 H14A H14B N1 - Distance Angles C2 1.3302 (0.0025) C6 1.3514 (0.0024) 116.15 (0.16) N1 - C2 N5 - Distance Angles C4 1.3333 (0.0025) C6 1.3564 (0.0023) 115.69 (0.16) N5 - C4 N7 - Distance Angles C6 1.3540 (0.0024) C12 1.4562 (0.0022) 123.45 (0.15) C8 1.4575 (0.0023) 123.45 (0.15) 113.10 (0.15) N7 - C6 C12 N10 - Distance Angles C13 1.3522 (0.0024) C11 1.4595 (0.0023) 125.31 (0.15) C9 1.4608 (0.0023) 120.85 (0.15) 113.77 (0.15) N10 - C13 C11 O15 - Distance Angles C13 1.2362 (0.0023) O15 - FMAP and GRID set by program FMAP 2 2 18 GRID 21.667 -2 -1 3.333 2 1 R1 = 0.0780 for 2280 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.24 at 0.4369 0.7341 0.0592 [ 0.75 A from C14 ] Deepest hole -0.28 at 0.0612 0.7443 0.0537 [ 0.72 A from C2 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 2182 / 23850 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4369 0.7659 0.5592 1.00000 0.05 0.24 0.75 C14 0.77 C13 1.37 H14B 1.40 H14A Q2 1 0.3078 0.9147 0.6631 1.00000 0.05 0.20 0.89 H11B 1.21 C11 1.26 H11A 2.08 N10 Q3 1 0.2403 1.5285 0.6541 1.00000 0.05 0.19 1.25 N1 1.46 H12A 1.68 H9B 2.20 C6 Q4 1 0.2436 1.4879 0.4542 1.00000 0.05 0.19 0.91 N7 1.06 C6 1.87 C12 1.89 N1 Q5 1 0.2778 1.0852 0.6198 1.00000 0.05 0.18 0.47 H11B 0.83 C11 1.51 H11A 1.64 C12 Q6 1 0.3715 0.8760 0.4989 1.00000 0.05 0.18 0.68 C13 0.68 N10 1.73 O15 1.88 C14 Q7 1 0.4103 1.0439 0.4557 1.00000 0.05 0.18 1.53 N10 1.58 C13 1.86 H14C 2.14 O15 Q8 1 0.3206 1.1795 0.5796 1.00000 0.05 0.17 0.74 C12 0.79 C11 1.43 H12B 1.46 H12A Q9 1 -0.0917 1.7065 0.4812 1.00000 0.05 0.17 1.57 H3 2.00 C6 2.06 C3 2.14 N1 Q10 1 0.1132 1.7284 0.6768 1.00000 0.05 0.17 0.69 H2 1.40 C2 2.08 N1 2.46 H9A Shortest distances between peaks (including symmetry equivalents) 5 8 1.08 2 5 1.19 1 6 1.21 6 7 1.36 2 8 1.93 1 7 2.04 3 4 2.29 6 8 2.33 2 6 2.36 3 10 2.37 7 8 2.40 4 8 2.44 2 3 2.59 5 6 2.61 7 7 2.63 1 7 2.65 3 9 2.70 3 8 2.74 1 2 2.75 3 5 2.85 4 9 2.89 5 9 2.97 Time profile in seconds ----------------------- 0.05: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: 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. 0.63: 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 0.38: 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 0.02: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.02: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0067p21c finished at 09:15:48 Total CPU time: 1.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++