+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007may0002 started at 12:59:29 on 29-Sep-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007may0002 in I4(1)/a CELL 0.71073 22.5496 22.5496 6.3581 90.000 90.000 90.000 ZERR 16.00 0.0004 0.0004 0.0002 0.000 0.000 0.000 LATT 2 SYMM 1/2 - X, - Y, 1/2 + Z SYMM 3/4 - Y, 1/4 + X, 1/4 + Z SYMM 3/4 + Y, 3/4 - X, 3/4 + Z SFAC C H O UNIT 144 160 48 V = 3233.00 F(000) = 1408.0 Mu = 0.10 mm-1 Cell Wt = 2658.72 Rho = 1.366 MERG 2 OMIT -3.00 55.00 OMIT -1 2 1 FMAP 2 PLAN 5 SIZE 0.12 0.12 0.30 ACTA EQIV $1 y - 1/4, -x + 3/4, z - 1/4 HTAB O3 O3_$1 BOND $H L.S. 6 TEMP -153.00 WGHT 0.050900 1.982100 EXTI 0.001899 FVAR 0.29151 C1 1 0.283765 0.373562 0.404163 11.00000 0.02945 0.03007 = 0.02129 0.00174 -0.00107 -0.00760 AFIX 23 H1A 2 0.325614 0.381764 0.441162 11.00000 -1.20000 H1B 2 0.261371 0.411242 0.413008 11.00000 -1.20000 AFIX 0 C2 1 0.280346 0.349343 0.183301 11.00000 0.01944 0.02514 = 0.02388 -0.00189 -0.00113 0.00072 AFIX 13 H2 2 0.299220 0.309216 0.181499 11.00000 -1.20000 AFIX 0 C3 1 0.185488 0.314549 0.277987 11.00000 0.02180 0.01789 = 0.02426 -0.00025 0.00299 0.00186 C4 1 0.130477 0.291675 0.223214 11.00000 0.02296 0.02621 = 0.03024 -0.00247 -0.00139 0.00328 AFIX 43 H4 2 0.115775 0.297116 0.084529 11.00000 -1.20000 AFIX 0 C5 1 0.096895 0.260979 0.369388 11.00000 0.02044 0.02703 = 0.04243 -0.00589 0.00562 -0.00076 AFIX 43 H5 2 0.059325 0.245322 0.330831 11.00000 -1.20000 AFIX 0 C6 1 0.118188 0.253087 0.572578 11.00000 0.02932 0.02427 = 0.03920 -0.00074 0.01478 -0.00068 AFIX 43 H6 2 0.095517 0.231292 0.672003 11.00000 -1.20000 AFIX 0 C7 1 0.172370 0.276920 0.630423 11.00000 0.03195 0.02495 = 0.02466 -0.00109 0.00708 0.00338 AFIX 43 H7 2 0.186701 0.271786 0.769742 11.00000 -1.20000 AFIX 0 C8 1 0.205801 0.308397 0.484288 11.00000 0.02193 0.02036 = 0.02433 -0.00346 0.00083 0.00220 C9 1 0.310061 0.387307 0.018773 11.00000 0.02547 0.02729 = 0.02373 0.00016 -0.00035 -0.00174 AFIX 23 H9A 2 0.353219 0.388314 0.047120 11.00000 -1.20000 H9B 2 0.304198 0.368799 -0.120882 11.00000 -1.20000 AFIX 0 O1 3 0.259249 0.331170 0.549498 11.00000 0.02998 0.03343 = 0.02074 0.00304 -0.00327 -0.00801 O2 3 0.218480 0.342931 0.125799 11.00000 0.02109 0.02825 = 0.02176 0.00267 -0.00211 -0.00309 O3 3 0.288312 0.446357 0.012322 11.00000 0.03385 0.02304 = 0.03307 0.00182 -0.00795 -0.00399 H1O 2 0.256606 0.447486 -0.066905 11.00000 0.05937 HKLF 4 Covalent radii and connectivity table for 2007may0002 in I4(1)/a C 0.770 H 0.320 O 0.660 C1 - O1 C2 C2 - O2 C9 C1 C3 - O2 C4 C8 C4 - C5 C3 C5 - C4 C6 C6 - C7 C5 C7 - C6 C8 C8 - O1 C7 C3 C9 - O3 C2 O1 - C8 C1 O2 - C3 C2 O3 - C9 Operators for generating equivalent atoms: $1 y-1/4, -x+3/4, z-1/4 13907 Reflections read, of which 727 rejected -28 =< h =< 29, -29 =< k =< 29, -8 =< l =< 7, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 1858 Unique reflections, of which 0 suppressed R(int) = 0.0690 R(sigma) = 0.0530 Friedel opposites merged Maximum memory for data reduction = 1345 / 25013 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 = 1660 / 145264 wR2 = 0.1221 before cycle 1 for 1858 data and 114 / 114 parameters GooF = S = 1.052; Restrained GooF = 1.052 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0509 * P )^2 + 1.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29151 0.00095 -0.004 OSF 2 0.00190 0.00046 0.000 EXTI Mean shift/esd = 0.002 Maximum = -0.007 for U13 O2 Max. shift = 0.000 A for C5 Max. dU = 0.000 for H1O Least-squares cycle 2 Maximum vector length = 511 Memory required = 1660 / 145264 wR2 = 0.1221 before cycle 2 for 1858 data and 114 / 114 parameters GooF = S = 1.052; Restrained GooF = 1.052 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0509 * P )^2 + 1.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29151 0.00095 0.000 OSF 2 0.00190 0.00046 0.000 EXTI Mean shift/esd = 0.001 Maximum = -0.003 for U13 O2 Max. shift = 0.000 A for O1 Max. dU = 0.000 for H1O Least-squares cycle 3 Maximum vector length = 511 Memory required = 1660 / 145264 wR2 = 0.1221 before cycle 3 for 1858 data and 114 / 114 parameters GooF = S = 1.052; Restrained GooF = 1.052 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0509 * P )^2 + 1.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29151 0.00095 0.000 OSF 2 0.00190 0.00046 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for U22 O1 Max. shift = 0.000 A for H1O Max. dU = 0.000 for C2 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1660 / 145264 wR2 = 0.1221 before cycle 4 for 1858 data and 114 / 114 parameters GooF = S = 1.052; Restrained GooF = 1.052 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0509 * P )^2 + 1.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29151 0.00095 0.000 OSF 2 0.00190 0.00046 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y C5 Max. shift = 0.000 A for H1O Max. dU = 0.000 for O2 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1660 / 145264 wR2 = 0.1221 before cycle 5 for 1858 data and 114 / 114 parameters GooF = S = 1.052; Restrained GooF = 1.052 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0509 * P )^2 + 1.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29151 0.00095 0.000 OSF 2 0.00190 0.00046 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H1O Max. dU = 0.000 for H1O Least-squares cycle 6 Maximum vector length = 511 Memory required = 1660 / 145264 wR2 = 0.1221 before cycle 6 for 1858 data and 114 / 114 parameters GooF = S = 1.052; Restrained GooF = 1.052 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0509 * P )^2 + 1.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29151 0.00095 0.000 OSF 2 0.00190 0.00046 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y O1 Max. shift = 0.000 A for H1O Max. dU = 0.000 for H1O No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.3256 0.3818 0.4412 23 0.990 0.000 C1 O1 C2 H1B 0.2614 0.4112 0.4130 23 0.990 0.000 C1 O1 C2 H2 0.2992 0.3092 0.1815 13 1.000 0.000 C2 O2 C9 C1 H4 0.1158 0.2971 0.0845 43 0.950 0.000 C4 C5 C3 H5 0.0593 0.2453 0.3308 43 0.950 0.000 C5 C4 C6 H6 0.0955 0.2313 0.6720 43 0.950 0.000 C6 C7 C5 H7 0.1867 0.2718 0.7697 43 0.950 0.000 C7 C6 C8 H9A 0.3532 0.3883 0.0471 23 0.990 0.000 C9 O3 C2 H9B 0.3042 0.3688 -0.1209 23 0.990 0.000 C9 O3 C2 2007may0002 in I4(1)/a ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.28376 0.37356 0.40416 1.00000 0.02945 0.03007 0.02129 0.00174 -0.00107 -0.00760 0.02694 0.00296 0.00008 0.00008 0.00026 0.00000 0.00095 0.00096 0.00086 0.00070 0.00069 0.00075 0.00042 H1A 0.32561 0.38176 0.44116 1.00000 0.03233 0.00000 0.00000 H1B 0.26137 0.41124 0.41301 1.00000 0.03233 0.00000 0.00000 C2 0.28035 0.34934 0.18330 1.00000 0.01944 0.02514 0.02388 -0.00189 -0.00113 0.00072 0.02282 0.00275 0.00007 0.00007 0.00025 0.00000 0.00084 0.00089 0.00084 0.00070 0.00065 0.00068 0.00038 H2 0.29922 0.30922 0.18150 1.00000 0.02738 0.00000 0.00000 C3 0.18549 0.31455 0.27799 1.00000 0.02180 0.01789 0.02426 -0.00025 0.00299 0.00186 0.02132 0.00280 0.00007 0.00007 0.00025 0.00000 0.00083 0.00080 0.00086 0.00065 0.00066 0.00066 0.00037 C4 0.13048 0.29167 0.22321 1.00000 0.02296 0.02621 0.03024 -0.00247 -0.00139 0.00328 0.02647 0.00293 0.00007 0.00007 0.00028 0.00000 0.00087 0.00093 0.00093 0.00072 0.00071 0.00071 0.00041 H4 0.11577 0.29712 0.08453 1.00000 0.03176 0.00000 0.00000 C5 0.09690 0.26098 0.36939 1.00000 0.02044 0.02703 0.04243 -0.00589 0.00562 -0.00076 0.02997 0.00313 0.00008 0.00008 0.00030 0.00000 0.00088 0.00095 0.00112 0.00078 0.00077 0.00070 0.00044 H5 0.05932 0.24532 0.33083 1.00000 0.03596 0.00000 0.00000 C6 0.11819 0.25309 0.57258 1.00000 0.02932 0.02427 0.03920 -0.00074 0.01478 -0.00068 0.03093 0.00333 0.00008 0.00008 0.00032 0.00000 0.00097 0.00093 0.00105 0.00078 0.00080 0.00073 0.00044 H6 0.09552 0.23129 0.67200 1.00000 0.03712 0.00000 0.00000 C7 0.17237 0.27692 0.63042 1.00000 0.03195 0.02495 0.02466 -0.00109 0.00708 0.00338 0.02719 0.00308 0.00008 0.00007 0.00027 0.00000 0.00100 0.00093 0.00087 0.00070 0.00072 0.00073 0.00042 H7 0.18670 0.27179 0.76974 1.00000 0.03262 0.00000 0.00000 C8 0.20580 0.30840 0.48429 1.00000 0.02193 0.02036 0.02433 -0.00346 0.00083 0.00220 0.02221 0.00270 0.00007 0.00007 0.00025 0.00000 0.00085 0.00083 0.00085 0.00066 0.00067 0.00066 0.00038 C9 0.31006 0.38731 0.01877 1.00000 0.02547 0.02729 0.02373 0.00016 -0.00035 -0.00174 0.02550 0.00296 0.00008 0.00007 0.00027 0.00000 0.00090 0.00093 0.00087 0.00069 0.00069 0.00072 0.00040 H9A 0.35322 0.38831 0.04712 1.00000 0.03060 0.00000 0.00000 H9B 0.30420 0.36880 -0.12088 1.00000 0.03060 0.00000 0.00000 O1 0.25925 0.33117 0.54950 1.00000 0.02998 0.03343 0.02074 0.00304 -0.00327 -0.00801 0.02805 0.00197 0.00005 0.00005 0.00018 0.00000 0.00069 0.00070 0.00060 0.00051 0.00050 0.00051 0.00033 O2 0.21848 0.34293 0.12580 1.00000 0.02109 0.02825 0.02176 0.00267 -0.00211 -0.00309 0.02370 0.00185 0.00005 0.00005 0.00016 0.00000 0.00063 0.00066 0.00060 0.00047 0.00045 0.00047 0.00031 O3 0.28831 0.44636 0.01232 1.00000 0.03385 0.02304 0.03307 0.00182 -0.00795 -0.00399 0.02999 0.00220 0.00006 0.00005 0.00020 0.00000 0.00076 0.00068 0.00072 0.00052 0.00058 0.00054 0.00034 H1O 0.25661 0.44749 -0.06690 1.00000 0.05937 0.04453 0.00114 0.00104 0.00394 0.00000 0.00733 Final Structure Factor Calculation for 2007may0002 in I4(1)/a Total number of l.s. parameters = 114 Maximum vector length = 511 Memory required = 1546 / 21973 wR2 = 0.1221 before cycle 7 for 1858 data and 0 / 114 parameters GooF = S = 1.052; Restrained GooF = 1.052 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0509 * P )^2 + 1.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0467 for 1345 Fo > 4sig(Fo) and 0.0720 for all 1858 data wR2 = 0.1221, GooF = S = 1.052, Restrained GooF = 1.052 for all data Occupancy sum of asymmetric unit = 12.00 for non-hydrogen and 10.00 for hydrogen atoms Principal mean square atomic displacements U 0.0376 0.0223 0.0209 C1 0.0267 0.0226 0.0192 C2 0.0263 0.0207 0.0169 C3 0.0322 0.0262 0.0209 C4 0.0456 0.0252 0.0190 C5 0.0499 0.0242 0.0187 C6 0.0367 0.0258 0.0190 C7 0.0264 0.0230 0.0172 C8 0.0284 0.0245 0.0236 C9 0.0409 0.0236 0.0197 O1 0.0306 0.0213 0.0192 O2 0.0423 0.0260 0.0216 O3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.015 0.023 0.031 0.042 0.053 0.068 0.089 0.131 1.000 Number in group 196. 185. 181. 184. 195. 173. 195. 177. 188. 184. GooF 0.911 0.915 0.969 1.145 1.258 1.067 1.178 1.018 1.023 0.962 K 2.181 1.168 1.021 0.954 0.966 1.003 0.990 1.014 1.012 1.016 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.65 inf Number in group 191. 200. 175. 177. 192. 180. 186. 184. 186. 187. GooF 1.034 1.061 0.907 1.090 1.087 0.998 0.957 0.921 1.074 1.318 K 1.028 1.047 1.034 1.059 1.013 0.999 1.013 1.006 1.022 1.009 R1 0.214 0.185 0.144 0.117 0.102 0.066 0.044 0.034 0.039 0.032 Recommended weighting scheme: WGHT 0.0485 2.1342 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) 0 1 1 1050.95 2171.37 5.53 0.128 6.12 -1 3 4 377.85 227.32 4.00 0.042 1.55 -1 7 2 164.51 88.96 3.72 0.026 2.25 12 12 6 840.90 523.42 3.55 0.063 0.83 -4 24 0 68.51 217.25 3.36 0.041 0.93 -1 11 6 121.94 215.11 3.25 0.040 0.94 -8 9 1 557.74 419.19 3.22 0.056 1.80 8 13 7 674.48 454.64 3.13 0.059 0.77 -3 9 2 718.49 554.35 3.12 0.065 1.90 -2 12 0 244.46 152.31 3.08 0.034 1.85 -6 14 2 66.66 22.32 3.02 0.013 1.34 5 9 4 88.14 149.94 3.00 0.034 1.29 -8 19 3 -15.18 51.33 2.97 0.020 0.97 -4 5 7 97.32 201.94 2.93 0.039 0.88 -5 11 2 25.24 0.67 2.84 0.002 1.61 -10 12 4 444.40 591.88 2.84 0.067 1.07 -11 13 4 75.69 133.16 2.79 0.032 1.02 0 5 7 591.54 404.27 2.76 0.055 0.89 -10 13 5 206.60 356.72 2.74 0.052 0.93 -4 8 0 362.90 263.79 2.74 0.045 2.52 -13 25 2 217.10 401.27 2.73 0.055 0.78 -2 4 8 78.62 200.02 2.70 0.039 0.79 1 6 7 75.63 0.10 2.69 0.001 0.88 4 8 2 963.65 789.06 2.67 0.077 1.98 -4 11 5 81.26 137.74 2.61 0.032 1.06 -3 19 2 57.66 8.67 2.61 0.008 1.10 8 12 6 1037.61 785.59 2.59 0.077 0.88 -3 11 2 66.12 30.49 2.58 0.015 1.68 4 9 3 319.42 239.70 2.58 0.043 1.56 14 21 1 125.66 20.76 2.54 0.013 0.88 -12 21 1 260.39 366.47 2.53 0.053 0.92 9 9 6 74.36 156.95 2.52 0.035 0.91 1 2 1 12240.89 14895.13 2.51 0.336 5.38 -1 12 1 1054.85 871.04 2.51 0.081 1.80 16 22 0 218.82 59.52 2.48 0.021 0.83 11 11 4 158.43 99.29 2.46 0.027 1.07 -7 12 1 318.43 242.07 2.45 0.043 1.57 -6 7 3 150.73 213.29 2.45 0.040 1.60 7 20 5 902.22 647.22 2.45 0.070 0.82 -8 22 2 785.66 997.49 2.44 0.087 0.92 18 18 2 -30.98 30.79 2.44 0.015 0.85 -9 13 2 474.76 592.48 2.44 0.067 1.30 -11 19 4 -20.55 34.19 2.43 0.016 0.86 -1 10 1 1280.39 1075.00 2.42 0.090 2.12 -6 22 2 273.70 181.23 2.42 0.037 0.94 0 12 0 7106.21 6110.94 2.42 0.215 1.88 10 19 5 -6.39 107.61 2.41 0.029 0.81 9 10 7 72.61 138.23 2.37 0.032 0.80 14 19 3 66.13 169.36 2.37 0.036 0.87 5 24 1 1539.97 1223.01 2.35 0.096 0.91 Bond lengths and angles C1 - Distance Angles O1 1.4399 (0.0020) C2 1.5087 (0.0023) 109.72 (0.14) H1A 0.9900 109.72 109.72 H1B 0.9900 109.72 109.72 108.20 C1 - O1 C2 H1A C2 - Distance Angles O2 1.4494 (0.0019) C9 1.5087 (0.0023) 108.01 (0.13) C1 1.5087 (0.0023) 108.67 (0.13) 114.66 (0.14) H2 1.0000 108.45 108.45 108.45 C2 - O2 C9 C1 C3 - Distance Angles O2 1.3782 (0.0019) C4 1.3879 (0.0023) 118.61 (0.14) C8 1.3963 (0.0023) 121.91 (0.14) 119.47 (0.15) C3 - O2 C4 C4 - Distance Angles C5 1.3843 (0.0025) C3 1.3879 (0.0023) 120.42 (0.16) H4 0.9500 119.79 119.79 C4 - C5 C3 C5 - Distance Angles C4 1.3843 (0.0025) C6 1.3897 (0.0028) 119.95 (0.16) H5 0.9500 120.03 120.03 C5 - C4 C6 C6 - Distance Angles C7 1.3845 (0.0025) C5 1.3897 (0.0028) 120.14 (0.16) H6 0.9500 119.93 119.93 C6 - C7 C5 C7 - Distance Angles C6 1.3845 (0.0025) C8 1.3912 (0.0023) 119.92 (0.16) H7 0.9500 120.04 120.04 C7 - C6 C8 C8 - Distance Angles O1 1.3741 (0.0019) C7 1.3912 (0.0023) 117.67 (0.14) C3 1.3963 (0.0023) 122.28 (0.14) 120.02 (0.15) C8 - O1 C7 C9 - Distance Angles O3 1.4196 (0.0020) C2 1.5087 (0.0023) 113.51 (0.14) H9A 0.9900 108.87 108.87 H9B 0.9900 108.87 108.87 107.71 C9 - O3 C2 H9A O1 - Distance Angles C8 1.3741 (0.0019) C1 1.4399 (0.0020) 113.03 (0.12) O1 - C8 O2 - Distance Angles C3 1.3782 (0.0019) C2 1.4494 (0.0019) 112.88 (0.12) O2 - C3 O3 - Distance Angles C9 1.4196 (0.0020) H1O 0.8750 (0.0262) 109.04 (1.56) O3 - C9 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.87(3) 1.77(3) 2.6355(14) 171(2) O3-H1O...O3_$1 FMAP and GRID set by program FMAP 2 3 7 GRID -3.125 -2 24 3.125 2 1 R1 = 0.0720 for 1858 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.23 at 0.1241 0.4836 0.0275 [ 0.88 A from C2 ] Deepest hole -0.18 at 0.0755 0.5287 0.0087 [ 0.85 A from C3 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 2586 / 23641 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2664 0.3741 0.2775 1.00000 0.05 0.23 0.88 C2 0.89 C1 1.21 H1B 1.61 O2 Q2 1 0.1179 0.2486 0.4652 1.00000 0.05 0.21 0.69 C6 0.82 C5 1.46 H6 1.58 H5 Q3 1 0.3392 0.3621 0.4693 1.00000 0.05 0.19 0.57 H1A 1.34 C1 2.00 O1 2.11 H1B Q4 1 0.2725 0.3324 0.7104 1.00000 0.05 0.18 1.07 O1 1.53 H9B 2.15 C8 2.17 C1 Q5 1 0.1541 0.2456 0.5961 1.00000 0.05 0.17 0.84 C6 0.85 C7 1.44 H6 1.45 H7 Shortest distances between peaks (including symmetry equivalents) 2 5 1.17 1 3 2.06 3 4 2.25 4 5 2.71 1 4 2.91 Time profile in seconds ----------------------- 0.09: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.01: 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. 0.51: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.01: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.75: Structure factors and derivatives 0.88: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.15: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.12: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007may0002 finished at 12:59:47 Total CPU time: 2.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++