+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0040p-1 started at 15:33:42 on 06-May-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0040p-1 in P-1 CELL 0.71073 5.7490 6.5410 9.9030 80.396 78.704 71.706 ZERR 1.00 0.0025 0.0028 0.0045 0.021 0.020 0.025 LATT 1 SFAC C H N O UNIT 12 20 2 6 V = 344.50 F(000) = 154.0 Mu = 0.11 mm-1 Cell Wt = 288.30 Rho = 1.390 MERG 2 OMIT -3.00 50.00 OMIT 0 0 1 SHEL 7 0.84 EQIV_$1 x, y+1, z HTAB O1A O22_$1 EQIV_$2 -x+1, -y, -z+1 HTAB N21 O22_$2 EQIV_$3 -x+1, -y+1, -z FMAP 2 PLAN 10 SIZE 0.07 0.11 0.16 ACTA CONF BOND $H WGHT 0.12430 L.S. 4 TEMP -153.00 FVAR 1.15037 MOLE 1 C1 1 0.576179 0.666693 0.118704 11.00000 0.06600 0.05875 = 0.05422 -0.01249 -0.01295 -0.03120 C2 1 0.584110 0.570249 -0.009347 11.00000 0.07559 0.06263 = 0.05055 -0.01827 -0.00615 -0.03283 AFIX 23 H2A 2 0.756298 0.482834 -0.039052 11.00000 -1.20000 H2B 2 0.537289 0.688847 -0.084289 11.00000 -1.20000 AFIX 0 O1A 4 0.732751 0.786394 0.100549 11.00000 0.08026 0.08638 = 0.05081 -0.02406 0.00106 -0.05228 AFIX 147 H1 2 0.712063 0.847925 0.171784 11.00000 0.07601 AFIX 0 O1B 4 0.446131 0.640907 0.226581 11.00000 0.07678 0.08278 = 0.05044 -0.02152 0.00417 -0.04553 MOLE 2 C22 1 0.773021 0.082550 0.352545 11.00000 0.05847 0.05670 = 0.04718 -0.01444 -0.00298 -0.02785 C23 1 0.974705 0.154639 0.256692 11.00000 0.06689 0.06163 = 0.05149 -0.01462 -0.00294 -0.03177 AFIX 23 H23A 2 0.916896 0.229787 0.168656 11.00000 -1.20000 H23B 2 1.121103 0.029095 0.235796 11.00000 -1.20000 AFIX 0 C24 1 1.039272 0.309888 0.333644 11.00000 0.05914 0.06537 = 0.05255 -0.01190 -0.00162 -0.03888 AFIX 23 H24A 2 1.207465 0.245884 0.359123 11.00000 -1.20000 H24B 2 1.032454 0.449572 0.275336 11.00000 -1.20000 AFIX 0 C25 1 0.842794 0.342499 0.463547 11.00000 0.05885 0.05663 = 0.05356 -0.01224 -0.00609 -0.03442 AFIX 23 H25A 2 0.920996 0.316676 0.547858 11.00000 -1.20000 H25B 2 0.727271 0.491067 0.457361 11.00000 -1.20000 AFIX 0 N21 3 0.714445 0.182597 0.465304 11.00000 0.05982 0.05769 = 0.04840 -0.00899 -0.00055 -0.03694 AFIX 43 H21 2 0.605764 0.154469 0.536204 11.00000 0.02171 AFIX 0 O22 4 0.673285 -0.051038 0.331901 11.00000 0.07042 0.07234 = 0.05824 -0.02410 -0.00304 -0.04267 HKLF 4 Covalent radii and connectivity table for 06skc0040p-1 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1B O1A C2 C2 - C1 C2_$3 O1A - C1 O1B - C1 C22 - O22 N21 C23 C23 - C22 C24 C24 - C25 C23 C25 - N21 C24 N21 - C22 C25 O22 - C22 Operators for generating equivalent atoms: $1 x, y+1, z $2 -x+1, -y, -z+1 $3 -x+1, -y+1, -z 6445 Reflections read, of which 463 rejected -6 =< h =< 6, -7 =< k =< 7, -11 =< l =< 11, Max. 2-theta = 50.00 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 3 6 1 57.03 4.88 6 32.03 1 Inconsistent equivalents 1199 Unique reflections, of which 0 suppressed R(int) = 0.1351 R(sigma) = 0.1246 Friedel opposites merged Maximum memory for data reduction = 1337 / 11877 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 = 1608 / 123716 wR2 = 0.2255 before cycle 1 for 1199 data and 94 / 94 parameters GooF = S = 0.962; Restrained GooF = 0.962 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1243 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.15037 0.00869 0.000 OSF Mean shift/esd = 0.001 Maximum = -0.004 for U12 O22 Max. shift = 0.000 A for C24 Max. dU = 0.000 for H1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1608 / 123716 wR2 = 0.2255 before cycle 2 for 1199 data and 94 / 94 parameters GooF = S = 0.962; Restrained GooF = 0.962 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1243 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.15037 0.00869 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for U12 O22 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1608 / 123716 wR2 = 0.2255 before cycle 3 for 1199 data and 94 / 94 parameters GooF = S = 0.962; Restrained GooF = 0.962 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1243 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.15037 0.00869 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for U22 C23 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H1 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1608 / 123716 wR2 = 0.2255 before cycle 4 for 1199 data and 94 / 94 parameters GooF = S = 0.962; Restrained GooF = 0.962 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1243 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.15037 0.00869 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C23 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H21 Largest correlation matrix elements -0.589 U12 O1A / U22 O1A -0.549 U12 O22 / U11 O22 -0.522 U12 O1B / U11 O1B -0.581 U12 O1B / U22 O1B -0.546 U12 C25 / U22 C25 -0.515 U12 C22 / U22 C22 -0.573 U12 N21 / U22 N21 -0.525 U12 O1A / U11 O1A -0.513 U12 C24 / U11 C24 -0.570 U12 O22 / U22 O22 -0.525 U12 C2 / U22 C2 -0.512 U12 C1 / U22 C1 -0.555 U12 C24 / U22 C24 -0.524 U12 C23 / U22 C23 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2A 0.7563 0.4828 -0.0391 23 0.990 0.000 C2 C1 C2_$3 H2B 0.5373 0.6888 -0.0843 23 0.990 0.000 C2 C1 C2_$3 H1 0.7121 0.8479 0.1718 147 0.840 0.000 O1A C1 H1 H23A 0.9169 0.2298 0.1687 23 0.990 0.000 C23 C22 C24 H23B 1.1211 0.0291 0.2358 23 0.990 0.000 C23 C22 C24 H24A 1.2075 0.2459 0.3591 23 0.990 0.000 C24 C25 C23 H24B 1.0325 0.4496 0.2753 23 0.990 0.000 C24 C25 C23 H25A 0.9210 0.3167 0.5479 23 0.990 0.000 C25 N21 C24 H25B 0.7273 0.4911 0.4574 23 0.990 0.000 C25 N21 C24 H21 0.6058 0.1545 0.5362 43 0.880 0.000 N21 C22 C25 06skc0040p-1 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.57618 0.66669 0.11870 1.00000 0.06601 0.05875 0.05422 -0.01249 -0.01295 -0.03120 0.05530 0.00618 0.00095 0.00077 0.00054 0.00000 0.00343 0.00352 0.00329 0.00260 0.00292 0.00304 0.00141 C2 0.58411 0.57025 -0.00935 1.00000 0.07559 0.06263 0.05055 -0.01827 -0.00615 -0.03283 0.05898 0.00585 0.00095 0.00079 0.00049 0.00000 0.00367 0.00348 0.00289 0.00252 0.00257 0.00289 0.00148 H2A 0.75630 0.48284 -0.03905 1.00000 0.07077 0.00000 0.00000 H2B 0.53729 0.68885 -0.08429 1.00000 0.07077 0.00000 0.00000 O1A 0.73275 0.78639 0.10055 1.00000 0.08026 0.08638 0.05081 -0.02406 0.00106 -0.05228 0.06547 0.00436 0.00065 0.00058 0.00033 0.00000 0.00250 0.00274 0.00218 0.00198 0.00179 0.00228 0.00113 H1 0.71206 0.84792 0.17178 1.00000 0.07600 0.00000 0.01823 O1B 0.44613 0.64091 0.22658 1.00000 0.07678 0.08279 0.05044 -0.02152 0.00417 -0.04554 0.06502 0.00429 0.00066 0.00059 0.00037 0.00000 0.00249 0.00267 0.00209 0.00183 0.00190 0.00214 0.00116 C22 0.77302 0.08255 0.35254 1.00000 0.05847 0.05669 0.04718 -0.01444 -0.00298 -0.02784 0.05119 0.00673 0.00089 0.00079 0.00049 0.00000 0.00309 0.00323 0.00303 0.00255 0.00234 0.00283 0.00135 C23 0.97470 0.15464 0.25669 1.00000 0.06689 0.06163 0.05148 -0.01461 -0.00294 -0.03177 0.05679 0.00594 0.00092 0.00080 0.00050 0.00000 0.00334 0.00335 0.00296 0.00248 0.00254 0.00286 0.00142 H23A 0.91689 0.22979 0.16866 1.00000 0.06815 0.00000 0.00000 H23B 1.12110 0.02910 0.23579 1.00000 0.06815 0.00000 0.00000 C24 1.03927 0.30989 0.33364 1.00000 0.05914 0.06537 0.05255 -0.01190 -0.00162 -0.03888 0.05447 0.00583 0.00090 0.00080 0.00045 0.00000 0.00316 0.00330 0.00290 0.00249 0.00248 0.00280 0.00139 H24A 1.20747 0.24588 0.35912 1.00000 0.06536 0.00000 0.00000 H24B 1.03246 0.44957 0.27534 1.00000 0.06536 0.00000 0.00000 C25 0.84279 0.34250 0.46355 1.00000 0.05884 0.05663 0.05356 -0.01224 -0.00608 -0.03443 0.05181 0.00577 0.00088 0.00075 0.00046 0.00000 0.00305 0.00324 0.00294 0.00245 0.00245 0.00274 0.00136 H25A 0.92099 0.31668 0.54786 1.00000 0.06217 0.00000 0.00000 H25B 0.72727 0.49107 0.45736 1.00000 0.06217 0.00000 0.00000 N21 0.71444 0.18260 0.46530 1.00000 0.05982 0.05770 0.04840 -0.00900 -0.00054 -0.03695 0.05136 0.00462 0.00069 0.00058 0.00040 0.00000 0.00266 0.00264 0.00245 0.00213 0.00205 0.00227 0.00115 H21 0.60576 0.15447 0.53620 1.00000 0.02171 0.00000 0.00981 O22 0.67328 -0.05104 0.33190 1.00000 0.07042 0.07235 0.05824 -0.02410 -0.00304 -0.04268 0.06077 0.00405 0.00060 0.00054 0.00032 0.00000 0.00228 0.00239 0.00212 0.00174 0.00169 0.00204 0.00112 Final Structure Factor Calculation for 06skc0040p-1 in P-1 Total number of l.s. parameters = 94 Maximum vector length = 511 Memory required = 1514 / 22995 wR2 = 0.2255 before cycle 5 for 1199 data and 0 / 94 parameters GooF = S = 0.962; Restrained GooF = 0.962 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1243 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0724 for 539 Fo > 4sig(Fo) and 0.1812 for all 1199 data wR2 = 0.2255, GooF = S = 0.962, Restrained GooF = 0.962 for all data Occupancy sum of asymmetric unit = 10.00 for non-hydrogen and 10.00 for hydrogen atoms Principal mean square atomic displacements U 0.0730 0.0587 0.0341 C1 0.0830 0.0583 0.0356 C2 0.1107 0.0514 0.0343 O1A 0.1036 0.0493 0.0422 O1B 0.0697 0.0473 0.0366 C22 0.0780 0.0514 0.0410 C23 0.0809 0.0505 0.0320 C24 0.0731 0.0529 0.0295 C25 0.0763 0.0472 0.0306 N21 0.0949 0.0570 0.0303 O22 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.006 0.010 0.015 0.020 0.026 0.035 0.049 0.068 0.104 1.000 Number in group 130. 119. 133. 109. 118. 111. 123. 121. 116. 119. GooF 0.851 0.871 0.908 0.980 0.902 1.002 0.994 1.043 1.048 1.016 K -3.228 -1.124 1.329 0.886 0.917 0.989 0.966 1.003 1.053 1.002 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.06 1.14 1.26 1.44 1.80 inf Number in group 120. 127. 116. 117. 120. 121. 119. 121. 118. 120. GooF 0.792 0.855 0.874 0.849 0.964 1.057 0.969 0.980 1.074 1.147 K 1.067 0.967 0.941 0.991 1.082 1.119 1.015 1.037 1.084 0.965 R1 0.543 0.497 0.401 0.299 0.248 0.148 0.125 0.095 0.084 0.055 Recommended weighting scheme: WGHT 0.1243 0.0000 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 -3 2 14.65 5.64 4.38 0.027 1.82 5 4 2 306.15 49.75 3.59 0.080 1.06 2 3 3 94.29 64.09 3.40 0.090 1.84 -2 2 4 8.21 17.40 3.30 0.047 1.41 1 0 10 39.90 19.37 3.17 0.050 0.98 3 -3 4 41.86 26.44 3.12 0.058 1.08 -2 4 0 37.84 21.34 3.08 0.052 1.20 2 3 2 255.09 182.29 2.98 0.153 1.94 -4 -3 3 145.06 97.57 2.97 0.112 1.13 -3 -2 1 10.71 2.12 2.96 0.016 1.70 -4 -1 3 28.92 42.97 2.69 0.074 1.21 1 1 8 15.93 24.84 2.68 0.056 1.24 1 -2 1 0.08 3.10 2.65 0.020 2.31 0 0 2 7.97 5.18 2.65 0.026 4.82 -1 -4 2 21.82 31.46 2.65 0.063 1.46 2 -1 2 27.89 39.34 2.65 0.071 2.10 5 4 3 0.29 6.37 2.59 0.029 1.06 3 5 5 279.73 209.24 2.55 0.163 1.13 -5 -3 3 -0.77 1.46 2.55 0.014 0.97 -1 -5 4 -5.21 2.78 2.48 0.019 1.07 2 -2 2 1055.29 796.45 2.45 0.319 1.70 4 7 3 -5.41 4.48 2.45 0.024 0.88 3 -1 1 21.68 14.32 2.42 0.043 1.61 1 0 1 10.76 7.98 2.40 0.032 5.05 3 -3 3 93.93 65.28 2.37 0.091 1.13 0 3 0 27.92 38.73 2.36 0.070 2.06 -5 -4 1 -5.04 5.86 2.35 0.027 1.01 3 1 3 26.92 36.50 2.33 0.068 1.78 4 2 3 17.27 24.68 2.27 0.056 1.39 -1 1 2 3.29 0.90 2.21 0.011 2.83 -2 -6 1 -4.13 2.66 2.19 0.018 1.04 4 2 0 20.29 12.67 2.18 0.040 1.39 0 0 4 16.19 12.02 2.13 0.039 2.41 -1 -5 6 9.54 0.11 2.08 0.004 0.94 0 4 1 24.03 31.60 2.06 0.064 1.55 2 -4 4 6.50 0.40 2.06 0.007 1.06 -1 5 0 10.65 3.00 2.05 0.020 1.13 -4 -4 1 165.39 126.40 2.04 0.127 1.16 -4 -2 6 -5.56 2.48 2.03 0.018 0.96 0 -1 8 -5.87 1.47 2.03 0.014 1.16 -2 3 0 5.84 2.19 2.01 0.017 1.45 4 1 1 3.29 7.16 2.00 0.030 1.43 -3 -5 2 140.58 108.78 2.00 0.118 1.10 3 2 9 14.83 6.21 1.99 0.028 1.02 -3 -1 1 25.85 33.64 1.98 0.066 1.78 -1 3 3 39.34 50.80 1.97 0.081 1.57 6 4 4 -8.53 1.75 1.96 0.015 0.91 4 6 5 22.46 13.88 1.94 0.042 0.95 -1 1 8 226.01 178.67 1.94 0.151 1.13 -2 2 0 -2.83 0.55 1.94 0.008 1.79 Bond lengths and angles C1 - Distance Angles O1B 1.1979 (0.0057) O1A 1.3370 (0.0056) 122.87 (0.43) C2 1.4948 (0.0064) 124.66 (0.44) 112.47 (0.46) C1 - O1B O1A C2 - Distance Angles C1 1.4948 (0.0064) C2_$3 1.4984 (0.0087) 113.58 (0.52) H2A 0.9900 108.85 108.85 H2B 0.9900 108.85 108.85 107.70 C2 - C1 C2_$3 H2A O1A - Distance Angles C1 1.3370 (0.0056) H1 0.8400 109.47 O1A - C1 O1B - Distance Angles C1 1.1979 (0.0057) O1B - C22 - Distance Angles O22 1.2467 (0.0052) N21 1.3217 (0.0057) 124.34 (0.43) C23 1.4935 (0.0069) 126.34 (0.42) 109.32 (0.39) C22 - O22 N21 C23 - Distance Angles C22 1.4935 (0.0069) C24 1.5347 (0.0057) 105.53 (0.37) H23A 0.9900 110.64 110.64 H23B 0.9900 110.64 110.64 108.76 C23 - C22 C24 H23A C24 - Distance Angles C25 1.5321 (0.0065) C23 1.5347 (0.0057) 105.10 (0.33) H24A 0.9900 110.73 110.73 H24B 0.9900 110.73 110.73 108.82 C24 - C25 C23 H24A C25 - Distance Angles N21 1.4533 (0.0054) C24 1.5321 (0.0065) 104.05 (0.34) H25A 0.9900 110.95 110.95 H25B 0.9900 110.95 110.95 108.96 C25 - N21 C24 H25A N21 - Distance Angles C22 1.3217 (0.0057) C25 1.4533 (0.0054) 115.04 (0.38) H21 0.8800 122.48 122.48 N21 - C22 C25 O22 - Distance Angles C22 1.2467 (0.0052) O22 - Selected torsion angles -1.49 ( 0.88) O1B - C1 - C2 - C2_$3 178.26 ( 0.53) O1A - C1 - C2 - C2_$3 -177.22 ( 0.48) O22 - C22 - C23 - C24 2.60 ( 0.53) N21 - C22 - C23 - C24 -7.63 ( 0.49) C22 - C23 - C24 - C25 9.60 ( 0.48) C23 - C24 - C25 - N21 -176.09 ( 0.45) O22 - C22 - N21 - C25 4.09 ( 0.56) C23 - C22 - N21 - C25 -8.90 ( 0.53) C24 - C25 - N21 - C22 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.77 2.603(4) 173.7 O1A-H1...O22_$1 0.88 2.07 2.935(5) 165.8 N21-H21...O22_$2 FMAP and GRID set by program FMAP 2 1 16 GRID -3.846 -2 -2 3.846 2 2 R1 = 0.1811 for 1199 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.24 at 0.3839 0.5163 0.7143 [ 1.32 A from O1B ] Deepest hole -0.25 at 0.1224 0.8855 0.6037 [ 0.90 A from C22 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 1541 / 12935 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.6161 0.4837 0.2857 1.00000 0.05 0.24 1.32 O1B 1.88 C1 1.94 H25B 2.27 H23A Q2 1 0.5077 0.1073 0.3032 1.00000 0.05 0.24 1.20 O22 1.64 C22 1.71 H24A 2.20 H1 Q3 1 1.1605 0.4551 0.3323 1.00000 0.05 0.22 1.02 H24B 1.30 H24A 1.34 C24 1.95 H25A Q4 1 1.0071 0.1984 0.5435 1.00000 0.05 0.21 0.78 H25A 1.38 C25 1.99 H24A 2.02 N21 Q5 1 0.6119 0.5866 0.3826 1.00000 0.05 0.19 1.08 H25B 1.90 O1B 1.90 C25 1.95 H21 Q6 1 0.5898 0.9405 0.0019 1.00000 0.05 0.19 1.45 O1A 1.88 H1 1.98 C1 2.10 H2B Q7 1 0.6949 0.6474 -0.1209 1.00000 0.05 0.17 0.88 H2B 1.23 H2A 1.27 C2 1.99 H24B Q8 1 0.5374 0.3344 0.4171 1.00000 0.05 0.17 1.28 N21 1.54 H21 1.85 H25B 1.89 C22 Q9 1 0.7843 0.3853 0.1047 1.00000 0.05 0.16 1.23 H23A 1.48 H2A 1.80 C2 1.86 C1 Q10 1 1.0522 0.2451 0.0636 1.00000 0.05 0.16 1.18 H23A 1.84 O1A 1.91 C23 2.04 H23B Shortest distances between peaks (including symmetry equivalents) 6 6 1.08 1 5 1.25 9 10 1.54 1 8 1.57 5 8 1.79 1 9 1.97 7 10 2.01 2 8 2.07 6 10 2.07 5 8 2.08 3 7 2.23 6 7 2.30 3 8 2.33 2 7 2.42 2 3 2.53 3 4 2.58 7 9 2.61 1 3 2.63 3 4 2.65 5 5 2.69 1 2 2.69 7 9 2.80 8 8 2.81 4 4 2.90 6 7 2.98 9 10 3.00 Time profile in seconds ----------------------- 0.09: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.02: 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. 0.38: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.09: Structure factors and derivatives 0.11: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.02: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.02: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0040p-1 finished at 15:33:43 Total CPU time: 0.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++