+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0034p21c started at 14:40:11 on 11-Jul-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0034p21c in P2(1)/c CELL 0.71073 6.4624 18.8186 7.1493 90.000 98.878 90.000 ZERR 4.00 0.0004 0.0010 0.0005 0.000 0.004 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 28 40 8 16 V = 859.03 F(000) = 392.0 Mu = 0.12 mm-1 Cell Wt = 744.68 Rho = 1.439 MERG 2 OMIT -3.00 55.00 OMIT 1 1 1 OMIT 0 1 1 SHEL 7 0.77 HTAB N23 O2A FMAP 2 PLAN 10 SIZE 0.01 0.05 0.06 ACTA BOND $H WGHT 0.03280 0.51270 L.S. 4 TEMP -153.00 FVAR 0.63811 MOLE 1 C1 1 0.433725 0.565205 0.647754 11.00000 0.02401 0.01647 = 0.01786 -0.00173 0.00298 0.00133 C2 1 0.650949 0.597722 0.732073 11.00000 0.01976 0.01890 = 0.02165 0.00007 0.00150 0.00066 C3 1 0.109013 0.587754 0.459361 11.00000 0.01753 0.02728 = 0.03365 -0.00074 -0.00567 -0.00301 AFIX 137 H3A 2 0.118159 0.545004 0.382786 11.00000 -1.50000 H3B 2 0.036259 0.625309 0.379959 11.00000 -1.50000 H3C 2 0.031249 0.576852 0.563156 11.00000 -1.50000 AFIX 0 O1A 4 0.377304 0.506443 0.682582 11.00000 0.02599 0.02147 = 0.03074 0.00416 -0.00111 -0.00417 O1B 4 0.318418 0.611595 0.536653 11.00000 0.01791 0.01832 = 0.03021 0.00209 -0.00278 -0.00059 O2A 4 0.771423 0.554532 0.831164 11.00000 0.02234 0.01962 = 0.03034 0.00268 -0.00530 0.00035 O2B 4 0.683757 0.660244 0.697080 11.00000 0.02643 0.01847 = 0.03550 0.00279 -0.00529 -0.00383 MOLE 2 C22 1 1.304511 0.603045 1.056118 11.00000 0.02050 0.01504 = 0.02087 0.00011 0.00173 0.00073 AFIX 43 H22 2 1.341957 0.555204 1.087439 11.00000 -1.20000 AFIX 0 C24 1 1.127016 0.697303 0.945335 11.00000 0.02535 0.01787 = 0.02731 0.00487 -0.00033 0.00210 AFIX 43 H24 2 1.016634 0.726552 0.885089 11.00000 -1.20000 AFIX 0 C25 1 1.318209 0.719572 1.028945 11.00000 0.02552 0.01562 = 0.03117 0.00047 0.00002 0.00011 AFIX 43 H25 2 1.368041 0.767129 1.038406 11.00000 -1.20000 AFIX 0 C26 1 1.641110 0.658952 1.200597 11.00000 0.01834 0.02791 = 0.02735 -0.00164 -0.00262 -0.00154 AFIX 137 H26A 2 1.639362 0.670984 1.333711 11.00000 -1.50000 H26B 2 1.725722 0.693905 1.144468 11.00000 -1.50000 H26C 2 1.701694 0.611526 1.192363 11.00000 -1.50000 AFIX 0 N21 3 1.426084 0.659612 1.097539 11.00000 0.01777 0.01796 = 0.01940 -0.00020 -0.00058 -0.00040 N23 3 1.121723 0.624923 0.963428 11.00000 0.02035 0.02088 = 0.02172 0.00119 -0.00251 -0.00290 AFIX 43 H23 2 1.014717 0.597418 0.920638 11.00000 0.03487 AFIX 0 HKLF 4 Covalent radii and connectivity table for 06skc0034p21c in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1A O1B C2 C2 - O2B O2A C1 C3 - O1B O1A - C1 O1B - C1 C3 O2A - C2 O2B - C2 C22 - N23 N21 C24 - C25 N23 C25 - C24 N21 C26 - N21 N21 - C22 C25 C26 N23 - C22 C24 11615 Reflections read, of which 293 rejected -8 =< h =< 8, -24 =< k =< 24, -9 =< l =< 9, Max. 2-theta = 54.96 0 Systematic absence violations 0 Inconsistent equivalents 1972 Unique reflections, of which 0 suppressed R(int) = 0.1031 R(sigma) = 0.0812 Friedel opposites merged Maximum memory for data reduction = 1329 / 19694 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 / 154280 wR2 = 0.1230 before cycle 1 for 1972 data and 121 / 121 parameters GooF = S = 1.044; Restrained GooF = 1.044 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0328 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.63810 0.00172 -0.004 OSF Mean shift/esd = 0.002 Maximum = -0.005 for U12 O1B Max. shift = 0.000 A for H3C Max. dU = 0.000 for H23 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1660 / 154280 wR2 = 0.1230 before cycle 2 for 1972 data and 121 / 121 parameters GooF = S = 1.043; Restrained GooF = 1.043 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0328 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.63810 0.00172 -0.001 OSF Mean shift/esd = 0.001 Maximum = -0.002 for U12 O1B Max. shift = 0.000 A for H26C Max. dU = 0.000 for H23 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1660 / 154280 wR2 = 0.1230 before cycle 3 for 1972 data and 121 / 121 parameters GooF = S = 1.043; Restrained GooF = 1.043 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0328 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.63810 0.00172 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C1 Max. dU = 0.000 for H23 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1660 / 154280 wR2 = 0.1230 before cycle 4 for 1972 data and 121 / 121 parameters GooF = S = 1.043; Restrained GooF = 1.043 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0328 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.63810 0.00172 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C26 Max. dU = 0.000 for H23 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 0.1182 0.5450 0.3828 137 0.980 0.000 C3 O1B H3A H3B 0.0363 0.6253 0.3800 137 0.980 0.000 C3 O1B H3A H3C 0.0312 0.5769 0.5632 137 0.980 0.000 C3 O1B H3A H22 1.3420 0.5552 1.0874 43 0.950 0.000 C22 N23 N21 H24 1.0166 0.7266 0.8851 43 0.950 0.000 C24 C25 N23 H25 1.3680 0.7671 1.0384 43 0.950 0.000 C25 C24 N21 H26A 1.6394 0.6710 1.3337 137 0.980 0.000 C26 N21 H26A H26B 1.7257 0.6939 1.1445 137 0.980 0.000 C26 N21 H26A H26C 1.7017 0.6115 1.1924 137 0.980 0.000 C26 N21 H26A H23 1.0147 0.5974 0.9206 43 0.880 0.000 N23 C22 C24 06skc0034p21c in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.43372 0.56521 0.64775 1.00000 0.02401 0.01647 0.01786 -0.00173 0.00298 0.00133 0.01947 0.00422 0.00036 0.00012 0.00032 0.00000 0.00129 0.00128 0.00120 0.00100 0.00100 0.00101 0.00053 C2 0.65095 0.59772 0.73207 1.00000 0.01976 0.01890 0.02165 0.00007 0.00150 0.00066 0.02028 0.00424 0.00035 0.00013 0.00033 0.00000 0.00126 0.00133 0.00124 0.00105 0.00098 0.00103 0.00054 C3 0.10901 0.58775 0.45936 1.00000 0.01753 0.02728 0.03365 -0.00074 -0.00567 -0.00301 0.02717 0.00430 0.00036 0.00014 0.00037 0.00000 0.00127 0.00144 0.00149 0.00119 0.00109 0.00105 0.00061 H3A 0.11816 0.54500 0.38278 1.00000 0.04075 0.00000 0.00000 H3B 0.03626 0.62531 0.37996 1.00000 0.04075 0.00000 0.00000 H3C 0.03125 0.57685 0.56316 1.00000 0.04075 0.00000 0.00000 O1A 0.37730 0.50644 0.68258 1.00000 0.02598 0.02147 0.03074 0.00416 -0.00111 -0.00417 0.02664 0.00302 0.00026 0.00009 0.00024 0.00000 0.00095 0.00094 0.00098 0.00080 0.00076 0.00075 0.00043 O1B 0.31842 0.61160 0.53665 1.00000 0.01792 0.01832 0.03021 0.00209 -0.00278 -0.00060 0.02283 0.00284 0.00023 0.00008 0.00023 0.00000 0.00087 0.00091 0.00098 0.00074 0.00072 0.00069 0.00041 O2A 0.77142 0.55453 0.83116 1.00000 0.02234 0.01962 0.03034 0.00268 -0.00530 0.00035 0.02509 0.00287 0.00025 0.00008 0.00024 0.00000 0.00091 0.00091 0.00097 0.00077 0.00075 0.00071 0.00043 O2B 0.68376 0.66024 0.69708 1.00000 0.02643 0.01847 0.03549 0.00279 -0.00529 -0.00383 0.02786 0.00296 0.00026 0.00009 0.00025 0.00000 0.00097 0.00093 0.00101 0.00080 0.00077 0.00074 0.00044 C22 1.30451 0.60304 1.05612 1.00000 0.02050 0.01504 0.02087 0.00011 0.00173 0.00073 0.01896 0.00408 0.00035 0.00012 0.00032 0.00000 0.00122 0.00123 0.00125 0.00101 0.00100 0.00101 0.00053 H22 1.34196 0.55520 1.08744 1.00000 0.02275 0.00000 0.00000 C24 1.12702 0.69730 0.94533 1.00000 0.02535 0.01787 0.02731 0.00487 -0.00033 0.00210 0.02397 0.00446 0.00039 0.00013 0.00035 0.00000 0.00134 0.00128 0.00140 0.00108 0.00108 0.00103 0.00057 H24 1.01663 0.72655 0.88509 1.00000 0.02877 0.00000 0.00000 C25 1.31821 0.71957 1.02895 1.00000 0.02552 0.01562 0.03117 0.00047 0.00002 0.00011 0.02456 0.00457 0.00038 0.00013 0.00036 0.00000 0.00136 0.00128 0.00146 0.00108 0.00113 0.00103 0.00058 H25 1.36804 0.76713 1.03841 1.00000 0.02947 0.00000 0.00000 C26 1.64111 0.65895 1.20060 1.00000 0.01834 0.02791 0.02735 -0.00164 -0.00262 -0.00154 0.02518 0.00427 0.00036 0.00013 0.00035 0.00000 0.00127 0.00143 0.00134 0.00115 0.00104 0.00107 0.00058 H26A 1.63936 0.67098 1.33371 1.00000 0.03777 0.00000 0.00000 H26B 1.72572 0.69390 1.14447 1.00000 0.03777 0.00000 0.00000 H26C 1.70169 0.61153 1.19236 1.00000 0.03777 0.00000 0.00000 N21 1.42608 0.65961 1.09754 1.00000 0.01777 0.01796 0.01940 -0.00020 -0.00058 -0.00040 0.01874 0.00337 0.00029 0.00010 0.00026 0.00000 0.00102 0.00104 0.00097 0.00086 0.00080 0.00083 0.00044 N23 1.12172 0.62492 0.96343 1.00000 0.02035 0.02087 0.02172 0.00118 -0.00251 -0.00290 0.02159 0.00358 0.00031 0.00010 0.00027 0.00000 0.00108 0.00110 0.00107 0.00088 0.00087 0.00088 0.00048 H23 1.01472 0.59742 0.92064 1.00000 0.03489 0.00000 0.00782 Final Structure Factor Calculation for 06skc0034p21c in P2(1)/c Total number of l.s. parameters = 121 Maximum vector length = 511 Memory required = 1539 / 22995 wR2 = 0.1230 before cycle 5 for 1972 data and 0 / 121 parameters GooF = S = 1.043; Restrained GooF = 1.043 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0328 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0609 for 1279 Fo > 4sig(Fo) and 0.1145 for all 1972 data wR2 = 0.1230, GooF = S = 1.043, Restrained GooF = 1.043 for all data Occupancy sum of asymmetric unit = 13.00 for non-hydrogen and 10.00 for hydrogen atoms Principal mean square atomic displacements U 0.0244 0.0189 0.0151 C1 0.0230 0.0195 0.0184 C2 0.0400 0.0279 0.0137 C3 0.0378 0.0234 0.0187 O1A 0.0345 0.0180 0.0160 O1B 0.0385 0.0203 0.0165 O2A 0.0447 0.0219 0.0169 O2B 0.0225 0.0195 0.0149 C22 0.0322 0.0248 0.0149 C24 0.0343 0.0237 0.0156 C25 0.0317 0.0281 0.0157 C26 0.0228 0.0180 0.0154 N21 0.0291 0.0201 0.0156 N23 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.007 0.013 0.020 0.029 0.038 0.048 0.061 0.081 0.120 1.000 Number in group 211. 189. 195. 213. 179. 204. 189. 209. 185. 198. GooF 1.158 1.158 0.967 1.001 0.989 0.990 1.114 1.005 1.031 0.998 K 20.173 3.497 1.761 1.247 1.023 1.027 1.011 0.988 1.004 0.987 Resolution(A) 0.77 0.79 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.66 inf Number in group 200. 199. 195. 202. 196. 193. 198. 194. 200. 195. GooF 1.000 0.875 1.021 0.984 1.079 1.065 1.052 0.966 1.107 1.247 K 1.071 1.210 1.115 1.110 1.049 1.006 0.997 0.999 1.016 0.979 R1 0.349 0.257 0.232 0.193 0.138 0.102 0.064 0.062 0.051 0.033 Recommended weighting scheme: WGHT 0.0328 0.5123 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) -3 3 6 39.20 4.02 4.50 0.013 1.09 3 9 0 19.49 1.39 4.04 0.008 1.49 -1 3 1 108.59 79.14 3.28 0.057 3.98 0 5 5 0.08 13.25 3.19 0.023 1.32 0 4 0 7330.13 8543.98 3.09 0.589 4.70 1 10 5 23.84 0.79 3.08 0.006 1.09 -1 4 2 36.86 22.12 3.01 0.030 2.71 -5 6 3 14.09 33.02 3.00 0.037 1.12 1 1 0 1230.35 1406.50 2.99 0.239 6.05 -6 8 5 117.37 71.63 2.92 0.054 0.86 2 15 0 26.35 9.99 2.90 0.020 1.17 0 22 1 49.70 113.06 2.86 0.068 0.85 2 1 1 958.95 843.86 2.83 0.185 2.72 2 8 1 373.86 317.36 2.74 0.113 1.79 -1 10 1 99.52 74.37 2.71 0.055 1.77 1 10 3 70.70 45.54 2.67 0.043 1.40 -1 1 8 20.26 0.25 2.63 0.003 0.89 6 1 4 92.56 54.80 2.63 0.047 0.85 4 15 5 -4.98 65.88 2.60 0.052 0.77 5 4 3 58.82 97.40 2.60 0.063 1.03 5 12 1 31.81 11.67 2.58 0.022 0.96 -8 4 3 15.33 53.98 2.56 0.047 0.78 -1 7 2 145.22 177.55 2.54 0.085 2.09 1 6 4 22.52 6.58 2.53 0.016 1.45 -3 22 2 91.04 28.30 2.52 0.034 0.78 4 5 4 12.65 0.85 2.51 0.006 1.06 6 5 2 19.10 38.34 2.51 0.039 0.95 -4 8 3 87.29 64.77 2.51 0.051 1.22 -5 4 7 49.33 3.44 2.50 0.012 0.84 6 12 2 49.48 103.64 2.49 0.065 0.83 3 12 5 50.88 0.56 2.49 0.005 0.90 -3 5 5 11.83 0.05 2.46 0.001 1.20 -3 12 3 30.09 13.42 2.44 0.023 1.16 1 11 2 278.33 236.42 2.42 0.098 1.47 1 4 1 363.50 315.14 2.41 0.113 3.22 -7 5 3 31.70 0.57 2.40 0.005 0.87 -7 8 2 54.39 11.36 2.39 0.021 0.86 -2 12 7 17.39 0.06 2.38 0.002 0.85 -2 6 3 164.42 136.72 2.38 0.074 1.72 -1 20 2 86.38 53.75 2.38 0.047 0.91 -2 18 6 48.05 2.72 2.37 0.011 0.78 2 18 2 11.28 0.21 2.34 0.003 0.94 -4 1 5 55.24 76.22 2.32 0.056 1.15 5 4 2 190.37 230.16 2.32 0.097 1.11 -3 14 1 13.44 2.24 2.28 0.010 1.14 -3 5 7 22.72 4.22 2.27 0.013 0.94 -3 9 6 14.30 0.19 2.26 0.003 0.98 2 20 0 36.75 73.95 2.26 0.055 0.90 1 0 2 308.03 359.02 2.26 0.121 2.91 -3 3 7 27.20 7.86 2.25 0.018 0.96 Bond lengths and angles C1 - Distance Angles O1A 1.2024 (0.0027) O1B 1.3288 (0.0027) 124.61 (0.21) C2 1.5644 (0.0033) 124.24 (0.21) 111.13 (0.20) C1 - O1A O1B C2 - Distance Angles O2B 1.2281 (0.0028) O2A 1.2643 (0.0028) 128.27 (0.22) C1 1.5644 (0.0033) 117.98 (0.20) 113.75 (0.20) C2 - O2B O2A C3 - Distance Angles O1B 1.4516 (0.0027) H3A 0.9800 109.47 H3B 0.9800 109.47 109.47 H3C 0.9800 109.47 109.47 109.47 C3 - O1B H3A H3B O1A - Distance Angles C1 1.2024 (0.0028) O1A - O1B - Distance Angles C1 1.3288 (0.0027) C3 1.4516 (0.0027) 115.36 (0.18) O1B - C1 O2A - Distance Angles C2 1.2643 (0.0028) O2A - O2B - Distance Angles C2 1.2281 (0.0028) O2B - C22 - Distance Angles N23 1.3275 (0.0029) N21 1.3290 (0.0029) 108.22 (0.20) H22 0.9500 125.89 125.89 C22 - N23 N21 C24 - Distance Angles C25 1.3534 (0.0034) N23 1.3692 (0.0030) 107.50 (0.21) H24 0.9500 126.25 126.25 C24 - C25 N23 C25 - Distance Angles C24 1.3534 (0.0034) N21 1.3763 (0.0030) 106.33 (0.21) H25 0.9500 126.83 126.83 C25 - C24 N21 C26 - Distance Angles N21 1.4690 (0.0029) H26A 0.9800 109.47 H26B 0.9800 109.47 109.47 H26C 0.9800 109.47 109.47 109.47 C26 - N21 H26A H26B N21 - Distance Angles C22 1.3290 (0.0029) C25 1.3763 (0.0030) 109.13 (0.19) C26 1.4690 (0.0029) 125.87 (0.19) 125.00 (0.20) N21 - C22 C25 N23 - Distance Angles C22 1.3275 (0.0029) C24 1.3692 (0.0030) 108.81 (0.20) H23 0.8800 125.60 125.60 N23 - C22 C24 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 1.80 2.667(3) 170.5 N23-H23...O2A FMAP and GRID set by program FMAP 2 1 17 GRID -3.571 24 -2 3.571 1 2 R1 = 0.1144 for 1972 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.22 at 0.1750 0.2943 0.2135 [ 1.34 A from O2B ] Deepest hole -0.26 at 0.2258 0.6558 0.1021 [ 1.19 A from C22 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 1823 / 20566 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.8250 0.7057 0.7865 1.00000 0.05 0.22 1.34 O2B 1.38 H24 2.11 C24 2.19 H26B Q2 1 1.3295 0.5034 1.1829 1.00000 0.05 0.22 1.20 H22 1.27 O2A 2.00 C2 2.00 O1A Q3 1 1.0601 0.7027 0.6401 1.00000 0.05 0.21 1.87 H24 2.16 C24 2.24 H24 2.29 H25 Q4 1 1.5721 0.5304 1.1025 1.00000 0.05 0.21 1.55 H22 1.67 O1A 1.81 H26C 2.19 C22 Q5 1 1.6828 0.6303 0.9576 1.00000 0.05 0.21 1.70 H26C 1.71 C2 1.78 H26B 1.83 O2A Q6 1 0.1748 0.5212 0.2377 1.00000 0.05 0.20 1.24 H3A 1.56 O2A 1.76 H22 2.11 C3 Q7 1 1.7238 0.7709 1.0932 1.00000 0.05 0.20 1.49 H26B 1.54 O2B 2.15 H26A 2.27 H25 Q8 1 0.4270 0.6265 0.4653 1.00000 0.05 0.20 0.97 O1B 1.74 C1 1.97 H26A 2.12 H25 Q9 1 0.4658 0.4414 0.6924 1.00000 0.05 0.20 1.35 O1A 1.77 H26C 1.85 H22 2.19 C26 Q10 1 0.8831 0.6124 1.0653 1.00000 0.05 0.19 1.46 H23 1.59 H26C 1.82 N23 1.97 H26B Shortest distances between peaks (including symmetry equivalents) 2 6 1.18 5 10 1.44 1 7 1.50 4 9 1.61 2 9 1.80 2 4 1.82 8 9 1.90 1 3 1.97 4 4 1.98 1 5 2.17 3 7 2.20 4 5 2.31 2 4 2.32 6 9 2.40 4 10 2.58 1 10 2.64 1 7 2.68 6 10 2.70 2 5 2.71 7 8 2.78 5 7 2.82 4 6 2.88 6 8 2.90 Time profile in seconds ----------------------- 0.06: 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. 0.53: 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 0.28: Structure factors and derivatives 0.22: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.03: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0034p21c finished at 14:40:12 Total CPU time: 1.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++