+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0082 started at 10:35:19 on 02-Feb-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0082 in P2(1)/n CELL 0.71073 5.8119 12.9400 11.9303 90.000 95.045 90.000 ZERR 4.00 0.0002 0.0005 0.0004 0.000 0.002 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H O UNIT 36 56 12 V = 893.75 F(000) = 368.0 Mu = 0.09 mm-1 Cell Wt = 680.81 Rho = 1.265 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 HTAB O1 O2 EQIV_$1 -x+1, -y+2, -z HTAB O1 O2_$1 FMAP 2 PLAN 10 SIZE 0.02 0.08 0.14 ACTA BOND $H WGHT 0.00580 0.89020 L.S. 4 TEMP -153.00 FVAR 0.83371 MOLE 1 C1 1 0.219326 0.907198 -0.178625 11.00000 0.01874 0.01954 = 0.02020 0.00134 0.00060 -0.00281 C2 1 0.146943 0.895412 -0.058579 11.00000 0.01768 0.01717 = 0.01966 -0.00065 0.00157 0.00374 C3 1 -0.042609 0.819238 -0.042682 11.00000 0.01866 0.02009 = 0.01837 -0.00087 0.00273 -0.00166 AFIX 23 H3A 2 -0.187197 0.841872 -0.085760 11.00000 -1.20000 H3B 2 -0.070680 0.815633 0.037879 11.00000 -1.20000 AFIX 0 C4 1 0.028371 0.711377 -0.084118 11.00000 0.01929 0.01918 = 0.01990 -0.00069 0.00128 0.00106 C5 1 0.079371 0.719133 -0.208668 11.00000 0.02735 0.01856 = 0.02099 -0.00165 0.00099 0.00055 AFIX 23 H5A 2 0.131014 0.650947 -0.234533 11.00000 -1.20000 H5B 2 -0.064052 0.737992 -0.255107 11.00000 -1.20000 AFIX 0 C6 1 0.262781 0.798548 -0.224769 11.00000 0.02263 0.02791 = 0.01456 0.00157 -0.00014 0.00321 C7 1 0.022077 0.959688 -0.252617 11.00000 0.02904 0.02281 = 0.02138 0.00311 -0.00259 0.00047 AFIX 137 H7A 2 0.065698 0.965857 -0.329835 11.00000 -1.50000 H7B 2 -0.006299 1.028633 -0.222751 11.00000 -1.50000 H7C 2 -0.118551 0.917940 -0.252298 11.00000 -1.50000 AFIX 0 C8 1 -0.167132 0.634090 -0.074850 11.00000 0.02514 0.02123 = 0.03171 -0.00083 0.00272 -0.00482 AFIX 137 H8A 2 -0.119551 0.566098 -0.100668 11.00000 -1.50000 H8B 2 -0.304509 0.657215 -0.121654 11.00000 -1.50000 H8C 2 -0.202974 0.629289 0.003727 11.00000 -1.50000 AFIX 0 C9 1 0.241725 0.674218 -0.011108 11.00000 0.02217 0.02544 = 0.02365 0.00226 0.00230 0.00246 AFIX 137 H9A 2 0.288988 0.606451 -0.037703 11.00000 -1.50000 H9B 2 0.205032 0.668602 0.067280 11.00000 -1.50000 H9C 2 0.367911 0.723780 -0.016101 11.00000 -1.50000 AFIX 0 O1 3 0.419453 0.967630 -0.181023 11.00000 0.02776 0.03726 = 0.02339 0.00073 0.00181 -0.01414 AFIX 147 H1 2 0.460658 0.988953 -0.115833 11.00000 -1.50000 AFIX 0 O2 3 0.249876 0.943183 0.017650 11.00000 0.02515 0.02796 = 0.02291 -0.00612 0.00085 -0.00423 O6 3 0.437719 0.779524 -0.268871 11.00000 0.03184 0.03922 = 0.03069 0.00306 0.01480 0.00703 HKLF 4 Covalent radii and connectivity table for 2009src0082 in P2(1)/n C 0.770 H 0.320 O 0.660 C1 - O1 C2 C6 C7 C2 - O2 C3 C1 C3 - C2 C4 C4 - C8 C9 C5 C3 C5 - C6 C4 C6 - O6 C5 C1 C7 - C1 C8 - C4 C9 - C4 O1 - C1 O2 - C2 O6 - C6 Operators for generating equivalent atoms: $1 -x+1, -y+2, -z 10637 Reflections read, of which 291 rejected -7 =< h =< 7, -16 =< k =< 16, -14 =< l =< 15, Max. 2-theta = 54.94 0 Systematic absence violations 0 Inconsistent equivalents 2059 Unique reflections, of which 0 suppressed R(int) = 0.0449 R(sigma) = 0.0412 Friedel opposites merged Maximum memory for data reduction = 1491 / 20364 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 = 1832 / 144126 wR2 = 0.1073 before cycle 1 for 2059 data and 113 / 113 parameters GooF = S = 1.081; Restrained GooF = 1.081 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0058 * P )^2 + 0.89 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.83371 0.00174 0.003 OSF Mean shift/su = 0.002 Maximum = 0.006 for U12 O1 Max. shift = 0.000 A for H9B Max. dU = 0.000 for C1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1832 / 144126 wR2 = 0.1074 before cycle 2 for 2059 data and 113 / 113 parameters GooF = S = 1.081; Restrained GooF = 1.081 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0058 * P )^2 + 0.89 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.83371 0.00174 -0.001 OSF Mean shift/su = 0.001 Maximum = 0.002 for U23 O2 Max. shift = 0.000 A for H9B Max. dU = 0.000 for C1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1832 / 144126 wR2 = 0.1074 before cycle 3 for 2059 data and 113 / 113 parameters GooF = S = 1.081; Restrained GooF = 1.081 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0058 * P )^2 + 0.89 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.83371 0.00174 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H9B Max. dU = 0.000 for C1 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1832 / 144126 wR2 = 0.1074 before cycle 4 for 2059 data and 113 / 113 parameters GooF = S = 1.081; Restrained GooF = 1.081 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0058 * P )^2 + 0.89 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.83371 0.00174 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y O1 Max. shift = 0.000 A for H1 Max. dU = 0.000 for O6 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 H3A -0.1872 0.8419 -0.0858 23 0.990 0.000 C3 C2 C4 H3B -0.0707 0.8156 0.0379 23 0.990 0.000 C3 C2 C4 H5A 0.1310 0.6509 -0.2345 23 0.990 0.000 C5 C6 C4 H5B -0.0641 0.7380 -0.2551 23 0.990 0.000 C5 C6 C4 H7A 0.0657 0.9659 -0.3298 137 0.980 0.000 C7 C1 H7A H7B -0.0063 1.0286 -0.2228 137 0.980 0.000 C7 C1 H7A H7C -0.1186 0.9179 -0.2523 137 0.980 0.000 C7 C1 H7A H8A -0.1196 0.5661 -0.1007 137 0.980 0.000 C8 C4 H8A H8B -0.3045 0.6572 -0.1217 137 0.980 0.000 C8 C4 H8A H8C -0.2030 0.6293 0.0037 137 0.980 0.000 C8 C4 H8A H9A 0.2890 0.6065 -0.0377 137 0.980 0.000 C9 C4 H9A H9B 0.2050 0.6686 0.0673 137 0.980 0.000 C9 C4 H9A H9C 0.3679 0.7238 -0.0161 137 0.980 0.000 C9 C4 H9A H1 0.4607 0.9890 -0.1158 147 0.840 0.000 O1 C1 H1 2009src0082 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.21933 0.90720 -0.17863 1.00000 0.01874 0.01954 0.02020 0.00134 0.00060 -0.00281 0.01955 0.00303 0.00029 0.00014 0.00014 0.00000 0.00081 0.00090 0.00082 0.00068 0.00066 0.00067 0.00037 C2 0.14694 0.89541 -0.05858 1.00000 0.01768 0.01717 0.01966 -0.00065 0.00157 0.00374 0.01817 0.00303 0.00028 0.00013 0.00014 0.00000 0.00079 0.00085 0.00082 0.00066 0.00064 0.00066 0.00035 C3 -0.04261 0.81924 -0.04268 1.00000 0.01866 0.02009 0.01837 -0.00087 0.00273 -0.00166 0.01898 0.00296 0.00029 0.00013 0.00014 0.00000 0.00080 0.00091 0.00081 0.00067 0.00063 0.00068 0.00036 H3A -0.18720 0.84187 -0.08576 1.00000 0.02277 0.00000 0.00000 H3B -0.07068 0.81563 0.03788 1.00000 0.02277 0.00000 0.00000 C4 0.02837 0.71138 -0.08412 1.00000 0.01929 0.01918 0.01990 -0.00069 0.00128 0.00106 0.01948 0.00305 0.00029 0.00013 0.00014 0.00000 0.00080 0.00091 0.00084 0.00068 0.00065 0.00069 0.00037 C5 0.07937 0.71913 -0.20867 1.00000 0.02735 0.01856 0.02099 -0.00165 0.00099 0.00055 0.02237 0.00317 0.00031 0.00014 0.00015 0.00000 0.00091 0.00091 0.00087 0.00069 0.00070 0.00074 0.00039 H5A 0.13101 0.65095 -0.23453 1.00000 0.02684 0.00000 0.00000 H5B -0.06405 0.73799 -0.25511 1.00000 0.02684 0.00000 0.00000 C6 0.26278 0.79855 -0.22477 1.00000 0.02263 0.02791 0.01456 0.00157 -0.00014 0.00321 0.02180 0.00318 0.00030 0.00015 0.00014 0.00000 0.00085 0.00099 0.00079 0.00071 0.00067 0.00075 0.00038 C7 0.02208 0.95969 -0.25262 1.00000 0.02904 0.02281 0.02138 0.00311 -0.00259 0.00047 0.02469 0.00328 0.00032 0.00015 0.00015 0.00000 0.00095 0.00096 0.00089 0.00072 0.00073 0.00078 0.00040 H7A 0.06570 0.96586 -0.32984 1.00000 0.03704 0.00000 0.00000 H7B -0.00630 1.02863 -0.22275 1.00000 0.03704 0.00000 0.00000 H7C -0.11855 0.91794 -0.25230 1.00000 0.03704 0.00000 0.00000 C8 -0.16713 0.63409 -0.07485 1.00000 0.02514 0.02123 0.03171 -0.00083 0.00272 -0.00482 0.02601 0.00329 0.00032 0.00014 0.00016 0.00000 0.00091 0.00096 0.00100 0.00079 0.00075 0.00077 0.00041 H8A -0.11955 0.56610 -0.10067 1.00000 0.03902 0.00000 0.00000 H8B -0.30451 0.65722 -0.12165 1.00000 0.03902 0.00000 0.00000 H8C -0.20297 0.62929 0.00373 1.00000 0.03902 0.00000 0.00000 C9 0.24172 0.67422 -0.01111 1.00000 0.02217 0.02544 0.02365 0.00226 0.00230 0.00246 0.02374 0.00330 0.00030 0.00015 0.00015 0.00000 0.00088 0.00098 0.00090 0.00075 0.00070 0.00075 0.00040 H9A 0.28899 0.60645 -0.03770 1.00000 0.03560 0.00000 0.00000 H9B 0.20503 0.66860 0.06728 1.00000 0.03560 0.00000 0.00000 H9C 0.36791 0.72378 -0.01610 1.00000 0.03560 0.00000 0.00000 O1 0.41945 0.96763 -0.18102 1.00000 0.02776 0.03726 0.02339 0.00073 0.00181 -0.01414 0.02950 0.00228 0.00022 0.00011 0.00011 0.00000 0.00070 0.00084 0.00067 0.00060 0.00055 0.00060 0.00034 H1 0.46066 0.98895 -0.11583 1.00000 0.04424 0.00000 0.00000 O2 0.24988 0.94318 0.01765 1.00000 0.02515 0.02796 0.02291 -0.00612 0.00085 -0.00423 0.02542 0.00215 0.00021 0.00010 0.00010 0.00000 0.00065 0.00072 0.00065 0.00055 0.00051 0.00056 0.00031 O6 0.43772 0.77952 -0.26887 1.00000 0.03184 0.03922 0.03069 0.00306 0.01480 0.00703 0.03321 0.00267 0.00024 0.00011 0.00012 0.00000 0.00074 0.00086 0.00075 0.00063 0.00060 0.00064 0.00035 Final Structure Factor Calculation for 2009src0082 in P2(1)/n Total number of l.s. parameters = 113 Maximum vector length = 511 Memory required = 1719 / 21973 wR2 = 0.1074 before cycle 5 for 2059 data and 0 / 113 parameters GooF = S = 1.081; Restrained GooF = 1.081 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0058 * P )^2 + 0.89 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0545 for 1631 Fo > 4sig(Fo) and 0.0737 for all 2059 data wR2 = 0.1074, GooF = S = 1.081, Restrained GooF = 1.081 for all data Occupancy sum of asymmetric unit = 12.00 for non-hydrogen and 14.00 for hydrogen atoms Principal mean square atomic displacements U 0.0232 0.0191 0.0163 C1 0.0214 0.0195 0.0136 C2 0.0216 0.0182 0.0172 C3 0.0210 0.0193 0.0181 C4 0.0278 0.0216 0.0177 C5 0.0294 0.0220 0.0140 C6 0.0319 0.0244 0.0177 C7 0.0318 0.0283 0.0180 C8 0.0277 0.0228 0.0207 C9 0.0476 0.0234 0.0175 O1 0.0329 0.0258 0.0176 O2 0.0480 0.0340 0.0176 O6 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.009 0.016 0.026 0.034 0.044 0.056 0.072 0.096 0.141 1.000 Number in group 233. 185. 214. 191. 211. 209. 200. 205. 204. 207. GooF 1.031 1.172 1.179 1.115 1.173 1.056 0.991 1.028 0.936 1.107 K 3.731 1.560 1.144 1.035 0.976 0.992 1.023 0.992 1.005 1.002 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.14 1.32 1.66 inf Number in group 217. 208. 194. 212. 203. 204. 206. 203. 205. 207. GooF 1.223 1.101 1.167 1.102 1.090 1.004 1.005 0.926 0.900 1.229 K 1.123 1.076 1.065 1.008 1.005 0.985 0.996 0.987 1.020 0.997 R1 0.181 0.167 0.158 0.130 0.099 0.066 0.047 0.042 0.036 0.029 Recommended weighting scheme: WGHT 0.0058 0.8902 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) 6 4 6 3.92 23.18 3.78 0.040 0.81 -4 0 10 5.48 24.46 3.66 0.041 0.96 -2 0 10 597.61 478.52 3.59 0.180 1.13 1 13 6 26.22 6.46 3.41 0.021 0.87 -1 1 1 2212.94 2430.49 3.18 0.407 4.98 -4 9 3 98.98 137.12 3.12 0.097 1.00 0 1 2 5226.12 5600.53 2.97 0.617 5.40 -5 7 8 29.44 10.49 2.90 0.027 0.85 0 7 12 25.53 9.38 2.87 0.025 0.87 -5 6 11 25.08 7.15 2.85 0.022 0.77 5 5 5 19.93 37.07 2.80 0.050 0.94 0 3 6 4.87 0.04 2.77 0.002 1.80 -6 5 6 0.92 9.48 2.76 0.025 0.85 -1 0 7 2056.40 1840.62 2.72 0.354 1.67 -3 0 9 146.42 198.39 2.71 0.116 1.14 -5 7 7 21.78 6.86 2.71 0.022 0.88 -2 10 12 36.54 1.55 2.68 0.010 0.77 0 13 3 25.99 9.36 2.68 0.025 0.97 4 8 4 53.68 79.77 2.67 0.074 0.99 -5 5 8 7.48 0.03 2.65 0.002 0.90 0 7 11 9.67 2.27 2.63 0.012 0.93 6 8 4 35.04 14.06 2.62 0.031 0.78 -4 5 12 171.84 129.20 2.61 0.094 0.81 -2 0 4 8.17 19.80 2.60 0.037 2.17 -2 2 13 74.31 105.92 2.55 0.085 0.89 6 9 0 25.45 3.06 2.54 0.014 0.80 2 0 12 38.54 65.61 2.54 0.067 0.91 -2 2 14 16.51 2.32 2.54 0.013 0.83 4 0 10 48.67 81.46 2.49 0.074 0.88 -7 4 2 -1.72 5.75 2.48 0.020 0.80 4 7 9 22.29 40.61 2.47 0.053 0.83 1 2 15 46.20 68.98 2.45 0.068 0.77 3 6 10 66.59 91.48 2.44 0.079 0.89 -4 13 2 1.82 16.31 2.44 0.033 0.82 5 0 5 12.10 2.78 2.42 0.014 1.01 2 2 0 293.51 252.32 2.42 0.131 2.64 -5 12 4 95.39 53.52 2.40 0.060 0.77 -2 4 1 1104.04 1011.30 2.38 0.262 2.15 -4 3 12 3.42 15.90 2.38 0.033 0.84 0 2 6 1494.20 1381.92 2.37 0.307 1.89 2 1 4 922.04 837.26 2.37 0.239 1.96 -4 8 8 32.47 18.97 2.33 0.036 0.90 2 9 6 12.90 24.07 2.33 0.040 1.06 -4 8 7 56.90 81.68 2.31 0.075 0.94 -3 9 3 258.49 301.91 2.30 0.143 1.12 6 2 8 111.37 82.21 2.29 0.075 0.77 6 8 2 103.35 67.53 2.28 0.068 0.81 0 14 4 7.33 19.60 2.26 0.037 0.88 -1 13 7 -4.13 3.95 2.25 0.016 0.85 -1 2 14 9.32 23.07 2.24 0.040 0.84 Bond lengths and angles C1 - Distance Angles O1 1.4039 (0.0021) C2 1.5354 (0.0023) 111.70 (0.14) C6 1.5388 (0.0025) 109.83 (0.14) 108.06 (0.14) C7 1.5417 (0.0024) 108.58 (0.14) 109.08 (0.14) 109.56 (0.14) C1 - O1 C2 C6 C2 - Distance Angles O2 1.2130 (0.0021) C3 1.5027 (0.0024) 123.94 (0.16) C1 1.5354 (0.0023) 119.42 (0.15) 116.55 (0.14) C2 - O2 C3 C3 - Distance Angles C2 1.5027 (0.0024) C4 1.5487 (0.0024) 109.39 (0.14) H3A 0.9900 109.80 109.80 H3B 0.9900 109.80 109.80 108.25 C3 - C2 C4 H3A C4 - Distance Angles C8 1.5250 (0.0024) C9 1.5289 (0.0024) 108.94 (0.15) C5 1.5438 (0.0024) 108.65 (0.14) 110.74 (0.14) C3 1.5487 (0.0024) 110.29 (0.14) 109.09 (0.14) 109.13 (0.14) C4 - C8 C9 C5 C5 - Distance Angles C6 1.5051 (0.0025) C4 1.5438 (0.0024) 111.43 (0.14) H5A 0.9900 109.34 109.34 H5B 0.9900 109.34 109.34 107.98 C5 - C6 C4 H5A C6 - Distance Angles O6 1.2105 (0.0021) C5 1.5051 (0.0025) 123.23 (0.18) C1 1.5388 (0.0025) 120.79 (0.17) 115.96 (0.15) C6 - O6 C5 C7 - Distance Angles C1 1.5417 (0.0024) H7A 0.9800 109.47 H7B 0.9800 109.47 109.47 H7C 0.9800 109.47 109.47 109.47 C7 - C1 H7A H7B C8 - Distance Angles C4 1.5250 (0.0024) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - C4 H8A H8B C9 - Distance Angles C4 1.5289 (0.0024) H9A 0.9800 109.47 H9B 0.9800 109.47 109.47 H9C 0.9800 109.47 109.47 109.47 C9 - C4 H9A H9B O1 - Distance Angles C1 1.4039 (0.0021) H1 0.8400 109.47 O1 - C1 O2 - Distance Angles C2 1.2130 (0.0021) O2 - O6 - Distance Angles C6 1.2105 (0.0021) O6 - Specified hydrogen bonds (with su's except fixed and riding H) D-H H...A D...A <(DHA) 0.84 2.18 2.6646(18) 117.1 O1-H1...O2 0.84 2.15 2.8575(18) 141.6 O1-H1...O2_$1 FMAP and GRID set by program FMAP 2 1 10 GRID -3.571 -2 -2 3.571 2 2 R1 = 0.0737 for 2059 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.32 at 0.1769 0.8986 0.8790 [ 0.76 A from C1 ] Deepest hole -0.22 at 0.1791 0.8181 0.0198 [ 1.37 A from C2 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 2037 / 16665 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1769 0.8986 -0.1210 1.00000 0.05 0.32 0.76 C1 0.78 C2 1.77 O2 1.86 O1 Q2 1 -0.0028 0.7630 -0.0653 1.00000 0.05 0.27 0.73 C4 0.82 C3 1.48 H3A 1.49 H3B Q3 1 0.1509 0.7633 -0.2229 1.00000 0.05 0.25 0.74 C5 0.80 C6 1.32 H5B 1.46 H5A Q4 1 0.0645 0.7252 -0.1376 1.00000 0.05 0.24 0.71 C4 0.86 C5 1.54 H5B 1.58 H5A Q5 1 0.1133 0.9461 -0.2035 1.00000 0.05 0.23 0.78 C7 0.83 C1 1.28 H7B 1.47 H7C Q6 1 0.2454 0.8526 -0.1936 1.00000 0.05 0.22 0.75 C1 0.80 C6 1.77 O6 1.80 O1 Q7 1 0.1199 0.6994 -0.0475 1.00000 0.05 0.18 0.68 C4 0.86 C9 1.47 H9B 1.49 H9C Q8 1 0.0438 0.8660 -0.0500 1.00000 0.05 0.18 0.72 C2 0.80 C3 1.41 H3A 1.45 H3B Q9 1 -0.2694 0.5992 -0.1439 1.00000 0.05 0.18 0.83 H8B 1.06 H8A 1.07 C8 1.81 H8C Q10 1 0.1779 0.6230 0.0860 1.00000 0.05 0.18 0.66 H9B 1.41 C9 1.68 H9A 2.15 H9C Shortest distances between peaks (including symmetry equivalents) 2 4 1.09 2 7 1.10 4 7 1.14 1 6 1.15 1 5 1.19 1 8 1.27 3 4 1.27 3 6 1.31 2 8 1.37 5 6 1.43 7 10 1.88 4 6 2.10 4 8 2.11 1 3 2.13 2 3 2.15 6 8 2.17 5 8 2.17 1 2 2.17 7 8 2.20 3 7 2.27 1 4 2.34 3 5 2.39 2 6 2.48 4 9 2.53 3 8 2.58 2 10 2.70 2 9 2.74 1 7 2.75 7 9 2.77 6 7 2.78 4 5 2.98 9 10 2.99 2 5 3.00 4 10 3.00 Time profile in seconds ----------------------- 0.02: Read and process instructions 0.00: Fit rigid groups 0.02: 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. 0.48: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.30: Structure factors and derivatives 0.22: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.05: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0082 finished at 10:35:20 Total CPU time: 1.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++