+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008lsh008 started at 11:27:33 on 23-Jun-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh008 in P2(1)/c CELL 0.71073 11.6779 9.4902 7.4186 90.000 106.515 90.000 ZERR 4.00 0.0009 0.0007 0.0006 0.000 0.005 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 36 44 4 4 V = 788.25 F(000) = 320.0 Mu = 0.08 mm-1 Cell Wt = 596.75 Rho = 1.257 MERG 2 OMIT -3.00 55.00 OMIT 0 2 1 FMAP 2 PLAN 5 ACTA EQIV $1 -x+1, y-1/2, -z+1/2 HTAB N1 O1_$1 BOND $H L.S. 6 SIZE 0.26 0.2 0.06 TEMP -153.00 WGHT 0.054200 0.226600 EXTI 0.056442 FVAR 1.56405 C1 1 0.675499 0.072809 0.218406 11.00000 0.02190 0.01947 = 0.01705 -0.00301 0.00578 -0.00056 C2 1 0.707702 0.183598 0.118861 11.00000 0.02531 0.02022 = 0.02027 0.00156 0.00656 0.00216 AFIX 43 H2 2 0.649878 0.251257 0.057052 11.00000 -1.20000 AFIX 0 C3 1 0.824660 0.194302 0.110735 11.00000 0.02727 0.02127 = 0.02014 0.00087 0.00889 -0.00150 AFIX 43 H3 2 0.845575 0.270083 0.042608 11.00000 -1.20000 AFIX 0 C4 1 0.912443 0.097527 0.199238 11.00000 0.02334 0.02171 = 0.02171 -0.00424 0.00845 -0.00155 C5 1 0.878096 -0.013155 0.296206 11.00000 0.02331 0.01885 = 0.02575 -0.00025 0.00551 0.00324 AFIX 43 H5 2 0.935706 -0.081462 0.356679 11.00000 -1.20000 AFIX 0 C6 1 0.761995 -0.025748 0.306342 11.00000 0.02572 0.01783 = 0.02202 0.00164 0.00782 -0.00058 AFIX 43 H6 2 0.741074 -0.102035 0.373647 11.00000 -1.20000 AFIX 0 C7 1 0.467091 0.143672 0.199499 11.00000 0.02414 0.02114 = 0.01856 -0.00338 0.00518 0.00024 C8 1 0.353451 0.088611 0.230799 11.00000 0.02270 0.02671 = 0.02850 -0.00272 0.00817 -0.00078 AFIX 137 H8A 2 0.331598 0.146979 0.324884 11.00000 -1.50000 H8B 2 0.365422 -0.008928 0.275589 11.00000 -1.50000 H8C 2 0.289305 0.091915 0.112313 11.00000 -1.50000 AFIX 0 C9 1 1.039876 0.111239 0.193193 11.00000 0.02578 0.02655 = 0.03255 -0.00070 0.01144 -0.00057 AFIX 137 H9A 2 1.041040 0.148227 0.070391 11.00000 -1.50000 H9B 2 1.078405 0.018537 0.212930 11.00000 -1.50000 H9C 2 1.083043 0.175868 0.292327 11.00000 -1.50000 AFIX 0 N1 3 0.558494 0.050435 0.232738 11.00000 0.02083 0.01758 = 0.02426 0.00063 0.00714 -0.00033 O1 4 0.474896 0.265964 0.147304 11.00000 0.02980 0.02065 = 0.03260 0.00322 0.01219 0.00398 H1N 2 0.544779 -0.035666 0.275953 11.00000 0.02741 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 2008lsh008 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 C1 - C6 C2 N1 C2 - C3 C1 C3 - C2 C4 C4 - C3 C5 C9 C5 - C6 C4 C6 - C5 C1 C7 - O1 N1 C8 C8 - C7 C9 - C4 N1 - C7 C1 O1 - C7 Operators for generating equivalent atoms: $1 -x+1, y-1/2, -z+1/2 9341 Reflections read, of which 329 rejected -15 =< h =< 14, -12 =< k =< 12, -9 =< l =< 9, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 1807 Unique reflections, of which 0 suppressed R(int) = 0.0538 R(sigma) = 0.0484 Friedel opposites merged Maximum memory for data reduction = 1308 / 18100 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 = 1610 / 138341 wR2 = 0.1155 before cycle 1 for 1807 data and 107 / 107 parameters GooF = S = 1.036; Restrained GooF = 1.036 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0542 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.56405 0.00574 -0.001 OSF 2 0.05645 0.01510 0.000 EXTI Mean shift/esd = 0.003 Maximum = 0.008 for U13 N1 Max. shift = 0.000 A for H8C Max. dU = 0.000 for C1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1610 / 138341 wR2 = 0.1155 before cycle 2 for 1807 data and 107 / 107 parameters GooF = S = 1.036; Restrained GooF = 1.036 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0542 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.56405 0.00574 0.001 OSF 2 0.05645 0.01510 0.000 EXTI Mean shift/esd = 0.001 Maximum = 0.003 for U13 N1 Max. shift = 0.000 A for H8A Max. dU = 0.000 for C1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1610 / 138341 wR2 = 0.1155 before cycle 3 for 1807 data and 107 / 107 parameters GooF = S = 1.036; Restrained GooF = 1.036 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0542 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.56405 0.00574 -0.001 OSF 2 0.05645 0.01510 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for H8C Max. dU = 0.000 for H1N Least-squares cycle 4 Maximum vector length = 511 Memory required = 1610 / 138341 wR2 = 0.1155 before cycle 4 for 1807 data and 107 / 107 parameters GooF = S = 1.036; Restrained GooF = 1.036 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0542 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.56405 0.00574 0.000 OSF 2 0.05644 0.01510 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y O1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for C1 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1610 / 138341 wR2 = 0.1155 before cycle 5 for 1807 data and 107 / 107 parameters GooF = S = 1.036; Restrained GooF = 1.036 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0542 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.56405 0.00574 0.000 OSF 2 0.05644 0.01510 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H1N Max. dU = 0.000 for C5 Least-squares cycle 6 Maximum vector length = 511 Memory required = 1610 / 138341 wR2 = 0.1155 before cycle 6 for 1807 data and 107 / 107 parameters GooF = S = 1.036; Restrained GooF = 1.036 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0542 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.56405 0.00574 0.000 OSF 2 0.05644 0.01510 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x C3 Max. shift = 0.000 A for H1N Max. dU = 0.000 for C6 Largest correlation matrix elements 0.620 EXTI / OSF Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.6499 0.2513 0.0571 43 0.950 0.000 C2 C3 C1 H3 0.8456 0.2701 0.0426 43 0.950 0.000 C3 C2 C4 H5 0.9357 -0.0815 0.3567 43 0.950 0.000 C5 C6 C4 H6 0.7411 -0.1020 0.3736 43 0.950 0.000 C6 C5 C1 H8A 0.3316 0.1470 0.3249 137 0.980 0.000 C8 C7 H8A H8B 0.3654 -0.0089 0.2756 137 0.980 0.000 C8 C7 H8A H8C 0.2893 0.0919 0.1123 137 0.980 0.000 C8 C7 H8A H9A 1.0410 0.1482 0.0704 137 0.980 0.000 C9 C4 H9A H9B 1.0784 0.0185 0.2129 137 0.980 0.000 C9 C4 H9A H9C 1.0830 0.1759 0.2923 137 0.980 0.000 C9 C4 H9A 2008lsh008 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.67550 0.07281 0.21841 1.00000 0.02190 0.01947 0.01705 -0.00301 0.00578 -0.00056 0.01943 0.00253 0.00012 0.00014 0.00018 0.00000 0.00073 0.00070 0.00063 0.00052 0.00053 0.00052 0.00033 C2 0.70770 0.18360 0.11886 1.00000 0.02531 0.02022 0.02027 0.00156 0.00656 0.00216 0.02192 0.00270 0.00013 0.00014 0.00019 0.00000 0.00077 0.00068 0.00067 0.00054 0.00055 0.00055 0.00033 H2 0.64988 0.25126 0.05705 1.00000 0.02630 0.00000 0.00000 C3 0.82466 0.19430 0.11074 1.00000 0.02727 0.02127 0.02014 0.00087 0.00889 -0.00150 0.02245 0.00270 0.00013 0.00015 0.00019 0.00000 0.00079 0.00070 0.00067 0.00054 0.00056 0.00056 0.00034 H3 0.84557 0.27008 0.04261 1.00000 0.02694 0.00000 0.00000 C4 0.91244 0.09753 0.19924 1.00000 0.02334 0.02171 0.02171 -0.00424 0.00845 -0.00155 0.02183 0.00261 0.00013 0.00014 0.00019 0.00000 0.00075 0.00072 0.00069 0.00055 0.00056 0.00055 0.00034 C5 0.87810 -0.01316 0.29621 1.00000 0.02331 0.01885 0.02575 -0.00025 0.00551 0.00324 0.02294 0.00270 0.00013 0.00015 0.00019 0.00000 0.00075 0.00070 0.00071 0.00056 0.00057 0.00054 0.00034 H5 0.93571 -0.08146 0.35668 1.00000 0.02753 0.00000 0.00000 C6 0.76199 -0.02575 0.30634 1.00000 0.02572 0.01783 0.02202 0.00164 0.00782 -0.00058 0.02164 0.00263 0.00013 0.00014 0.00019 0.00000 0.00079 0.00069 0.00069 0.00053 0.00057 0.00053 0.00034 H6 0.74107 -0.10203 0.37365 1.00000 0.02597 0.00000 0.00000 C7 0.46709 0.14367 0.19950 1.00000 0.02414 0.02114 0.01856 -0.00338 0.00518 0.00024 0.02146 0.00260 0.00013 0.00015 0.00019 0.00000 0.00078 0.00071 0.00064 0.00055 0.00053 0.00054 0.00034 C8 0.35345 0.08861 0.23080 1.00000 0.02270 0.02671 0.02850 -0.00272 0.00817 -0.00078 0.02579 0.00282 0.00013 0.00016 0.00021 0.00000 0.00079 0.00078 0.00076 0.00060 0.00059 0.00057 0.00036 H8A 0.33160 0.14698 0.32488 1.00000 0.03868 0.00000 0.00000 H8B 0.36542 -0.00893 0.27559 1.00000 0.03868 0.00000 0.00000 H8C 0.28931 0.09191 0.11231 1.00000 0.03868 0.00000 0.00000 C9 1.03988 0.11124 0.19319 1.00000 0.02578 0.02655 0.03255 -0.00070 0.01144 -0.00057 0.02765 0.00297 0.00013 0.00016 0.00022 0.00000 0.00082 0.00077 0.00080 0.00063 0.00063 0.00060 0.00037 H9A 1.04104 0.14823 0.07039 1.00000 0.04147 0.00000 0.00000 H9B 1.07841 0.01854 0.21293 1.00000 0.04147 0.00000 0.00000 H9C 1.08304 0.17587 0.29233 1.00000 0.04147 0.00000 0.00000 N1 0.55849 0.05043 0.23274 1.00000 0.02083 0.01758 0.02426 0.00063 0.00714 -0.00033 0.02074 0.00222 0.00010 0.00013 0.00016 0.00000 0.00065 0.00062 0.00062 0.00049 0.00047 0.00046 0.00031 O1 0.47490 0.26596 0.14730 1.00000 0.02980 0.02065 0.03260 0.00322 0.01219 0.00398 0.02700 0.00203 0.00009 0.00010 0.00015 0.00000 0.00061 0.00054 0.00059 0.00042 0.00045 0.00041 0.00030 H1N 0.54478 -0.03567 0.27595 1.00000 0.02741 0.03203 0.00144 0.00191 0.00232 0.00000 0.00423 Final Structure Factor Calculation for 2008lsh008 in P2(1)/c Total number of l.s. parameters = 107 Maximum vector length = 511 Memory required = 1503 / 22995 wR2 = 0.1155 before cycle 7 for 1807 data and 0 / 107 parameters GooF = S = 1.036; Restrained GooF = 1.036 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0542 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0464 for 1415 Fo > 4sig(Fo) and 0.0655 for all 1807 data wR2 = 0.1155, GooF = S = 1.036, Restrained GooF = 1.036 for all data Occupancy sum of asymmetric unit = 11.00 for non-hydrogen and 11.00 for hydrogen atoms Principal mean square atomic displacements U 0.0220 0.0214 0.0149 C1 0.0261 0.0210 0.0186 C2 0.0277 0.0217 0.0179 C3 0.0268 0.0217 0.0170 C4 0.0277 0.0241 0.0171 C5 0.0258 0.0222 0.0170 C6 0.0254 0.0228 0.0162 C7 0.0305 0.0247 0.0221 C8 0.0332 0.0265 0.0233 C9 0.0243 0.0205 0.0174 N1 0.0353 0.0265 0.0191 O1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.016 0.031 0.046 0.063 0.083 0.105 0.132 0.177 0.250 1.000 Number in group 184. 192. 170. 185. 173. 184. 179. 178. 180. 182. GooF 1.010 0.962 1.045 1.083 1.081 1.028 1.163 0.997 0.916 1.058 K 2.353 1.091 1.032 0.972 0.975 1.003 0.985 1.005 1.014 1.024 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.66 inf Number in group 181. 183. 179. 183. 182. 178. 178. 183. 180. 180. GooF 1.008 1.086 1.008 0.996 1.009 1.114 0.999 0.881 1.023 1.203 K 0.999 1.065 1.024 1.028 1.003 1.010 1.039 1.030 1.033 1.000 R1 0.163 0.166 0.135 0.092 0.071 0.069 0.041 0.035 0.036 0.033 Recommended weighting scheme: WGHT 0.0476 0.2500 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) -6 11 1 18.08 44.17 4.83 0.106 0.79 -11 1 3 105.99 142.76 3.59 0.190 1.04 -11 2 2 11.68 4.25 3.34 0.033 1.04 -12 4 2 6.39 14.94 3.21 0.062 0.90 -6 0 2 38.46 23.59 3.19 0.077 1.89 1 3 0 284.15 349.02 3.16 0.297 3.04 -3 3 3 20.27 12.56 3.11 0.056 1.87 -9 8 1 0.96 7.02 3.10 0.042 0.87 -6 10 2 16.26 28.95 3.09 0.086 0.85 7 9 1 88.87 116.16 3.07 0.172 0.86 -3 2 7 3.29 0.28 2.94 0.008 1.03 9 9 0 8.06 0.07 2.94 0.004 0.80 -5 7 5 35.76 48.73 2.87 0.111 0.97 -4 5 1 90.50 72.16 2.85 0.135 1.59 -11 0 2 33.90 48.85 2.83 0.111 1.06 14 0 0 90.79 56.14 2.83 0.119 0.80 0 1 1 248.57 334.90 2.80 0.291 5.69 -6 3 2 19.55 11.80 2.75 0.055 1.62 -11 3 6 20.28 31.12 2.75 0.089 0.88 11 2 0 37.91 51.16 2.73 0.114 1.00 -2 4 2 226.94 189.86 2.70 0.219 1.96 -5 11 2 4.99 14.67 2.70 0.061 0.80 0 2 0 804.22 958.23 2.64 0.493 4.75 2 0 2 607.19 721.75 2.63 0.428 2.68 -4 7 6 31.95 46.42 2.63 0.108 0.91 -7 3 9 16.70 1.43 2.60 0.019 0.78 -9 1 5 37.26 49.50 2.59 0.112 1.10 -4 3 2 22.52 15.88 2.58 0.063 2.00 -10 8 5 66.55 42.95 2.56 0.104 0.78 -4 11 1 9.57 19.90 2.54 0.071 0.83 -7 2 9 46.01 67.08 2.54 0.130 0.79 -4 6 3 87.97 70.79 2.53 0.134 1.27 4 2 6 -1.48 1.58 2.51 0.020 0.97 4 6 5 16.63 25.40 2.51 0.080 0.93 -11 1 1 61.71 78.71 2.49 0.141 1.04 -4 2 5 13.19 8.44 2.46 0.046 1.38 -5 0 2 4568.14 3944.24 2.45 1.000 2.20 7 3 6 13.16 6.12 2.44 0.039 0.82 -4 5 6 8.04 1.80 2.44 0.021 1.03 -3 2 3 35.59 27.19 2.42 0.083 2.09 8 7 4 13.08 5.30 2.42 0.037 0.79 -10 3 2 21.17 29.28 2.41 0.086 1.10 1 4 2 36.55 28.54 2.40 0.085 1.89 -1 1 5 47.05 37.27 2.39 0.097 1.45 -13 5 3 65.69 45.17 2.39 0.107 0.81 6 3 6 -1.49 2.79 2.29 0.027 0.86 -11 2 1 39.94 50.90 2.29 0.114 1.03 7 2 5 32.82 47.36 2.29 0.110 0.92 -4 9 5 3.82 10.03 2.29 0.050 0.85 4 4 1 163.80 139.72 2.29 0.188 1.68 Bond lengths and angles C1 - Distance Angles C6 1.3950 (0.0019) C2 1.3965 (0.0019) 118.95 (0.13) N1 1.4163 (0.0018) 116.75 (0.12) 124.27 (0.12) C1 - C6 C2 C2 - Distance Angles C3 1.3879 (0.0020) C1 1.3965 (0.0019) 119.63 (0.13) H2 0.9500 120.19 120.19 C2 - C3 C1 C3 - Distance Angles C2 1.3879 (0.0020) C4 1.3938 (0.0020) 122.17 (0.13) H3 0.9500 118.92 118.92 C3 - C2 C4 C4 - Distance Angles C3 1.3938 (0.0020) C5 1.3949 (0.0020) 117.28 (0.13) C9 1.5071 (0.0020) 121.96 (0.13) 120.76 (0.13) C4 - C3 C5 C5 - Distance Angles C6 1.3842 (0.0020) C4 1.3949 (0.0020) 121.51 (0.13) H5 0.9500 119.24 119.24 C5 - C6 C4 C6 - Distance Angles C5 1.3842 (0.0020) C1 1.3950 (0.0019) 120.46 (0.13) H6 0.9500 119.77 119.77 C6 - C5 C1 C7 - Distance Angles O1 1.2350 (0.0018) N1 1.3541 (0.0018) 123.13 (0.13) C8 1.5044 (0.0020) 121.45 (0.13) 115.42 (0.12) C7 - O1 N1 C8 - Distance Angles C7 1.5044 (0.0020) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - C7 H8A H8B C9 - Distance Angles C4 1.5071 (0.0020) 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 N1 - Distance Angles C7 1.3541 (0.0018) C1 1.4163 (0.0019) 128.01 (0.12) H1N 0.9085 (0.0180) 116.30 (1.05) 115.59 (1.04) N1 - C7 C1 O1 - Distance Angles C7 1.2350 (0.0018) O1 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.908(18) 1.999(18) 2.9034(16) 173.6(15) N1-H1N...O1_$1 FMAP and GRID set by program FMAP 2 3 12 GRID -2.778 -2 -2 2.778 2 2 R1 = 0.0655 for 1807 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.24 at 0.8970 0.0524 0.2490 [ 0.62 A from C4 ] Deepest hole -0.22 at 0.4997 0.5336 0.2326 [ 0.81 A from N1 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 1727 / 15549 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.8970 0.0524 0.2490 1.00000 0.05 0.24 0.62 C4 0.78 C5 1.50 H5 1.76 C3 Q2 1 0.6815 0.1196 0.1500 1.00000 0.05 0.22 0.69 C1 0.75 C2 1.42 H2 1.84 N1 Q3 1 0.8840 0.1594 0.2153 1.00000 0.05 0.22 0.70 C4 0.94 C3 1.62 H3 1.75 C5 Q4 1 0.7323 0.0425 0.3073 1.00000 0.05 0.21 0.74 C6 0.84 C1 1.45 H6 1.81 C5 Q5 1 1.1066 0.0140 0.2769 1.00000 0.05 0.19 0.50 H9B 1.25 C9 1.57 H9C 1.97 H9A Shortest distances between peaks (including symmetry equivalents) 1 3 1.05 2 4 1.36 1 4 2.09 2 3 2.31 3 4 2.35 1 5 2.42 1 2 2.49 3 5 2.86 Time profile in seconds ----------------------- 0.18: Read and process instructions 0.01: 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. 0.65: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.01: OSF, H-atoms from difference map 0.01: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.63: Structure factors and derivatives 0.39: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.11: Solve l.s. equations 0.00: Generate HTAB table 0.01: Other dependent quantities, CIF, tables 0.04: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008lsh008 finished at 11:27:35 Total CPU time: 2.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++