+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 07skc0021p-1 started at 12:29:47 on 05-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 07skc0021p-1 in P-1 CELL 0.71073 7.2807 7.9336 9.4910 67.216 76.457 67.849 ZERR 2.00 0.0004 0.0005 0.0006 0.002 0.003 0.004 LATT 1 SFAC C H N O UNIT 14 30 2 8 V = 465.64 F(000) = 192.0 Mu = 0.10 mm-1 Cell Wt = 354.40 Rho = 1.264 MERG 2 OMIT -3.00 55.00 OMIT 0 1 2 OMIT 1 0 0 SHEL 7 0.77 HTAB N21 O1B EQIV_$1 -x+1, -y, -z+2 HTAB O1B O1B_$1 EQIV_$2 -x+2, -y+1, -z+1 HTAB O6B O6B_$2 EQIV_$3 x-1, y, z HTAB N21 O1A_$3 EQIV_$4 -x+1, -y+1, -z+1 HTAB N21 O6A_$4 FMAP 2 PLAN 10 SIZE 0.04 0.09 0.17 ACTA BOND $H WGHT 0.01770 0.37800 L.S. 4 TEMP -153.00 FVAR 1.39834 MOLE 1 C1 1 0.653264 0.145941 0.800801 11.00000 0.01799 0.01212 = 0.01633 -0.00394 -0.00201 -0.00312 C2 1 0.656414 0.249496 0.629431 11.00000 0.01825 0.01850 = 0.01412 -0.00264 -0.00026 -0.00551 AFIX 23 H2A 2 0.634610 0.169801 0.580374 11.00000 -1.20000 H2B 2 0.789643 0.264196 0.588114 11.00000 -1.20000 AFIX 0 C3 1 0.497714 0.448920 0.586985 11.00000 0.01869 0.01849 = 0.01431 -0.00367 -0.00080 -0.00556 AFIX 23 H3A 2 0.364338 0.434681 0.628494 11.00000 -1.20000 H3B 2 0.519915 0.529325 0.635137 11.00000 -1.20000 AFIX 0 C4 1 1.010466 0.486679 0.922746 11.00000 0.02135 0.02081 = 0.01416 -0.00714 -0.00161 -0.00357 AFIX 23 H4A 2 1.135859 0.506899 0.862686 11.00000 -1.20000 H4B 2 1.018361 0.352847 0.940270 11.00000 -1.20000 AFIX 0 C5 1 0.835735 0.626847 0.831226 11.00000 0.02599 0.02895 = 0.01689 -0.00983 -0.00541 0.00237 AFIX 23 H5A 2 0.715012 0.590426 0.883962 11.00000 -1.20000 H5B 2 0.812718 0.757456 0.832537 11.00000 -1.20000 AFIX 0 C6 1 0.859699 0.636685 0.665813 11.00000 0.01755 0.02172 = 0.01491 -0.00517 -0.00204 -0.00709 O1A 4 0.794911 0.101287 0.872705 11.00000 0.01732 0.03138 = 0.01987 -0.00236 -0.00538 -0.00846 O1B 4 0.489270 0.107731 0.866245 11.00000 0.01868 0.02541 = 0.01430 0.00237 -0.00332 -0.01009 AFIX 147 H1 2 0.503756 0.036231 0.957923 10.50000 -1.50000 AFIX 0 O6A 4 0.761564 0.782227 0.571281 11.00000 0.03396 0.02489 = 0.01616 -0.00357 -0.00660 0.00111 O6B 4 0.984065 0.487179 0.634966 11.00000 0.02844 0.02080 = 0.01541 -0.00766 -0.00522 -0.00145 AFIX 147 H6 2 0.993568 0.507276 0.540308 10.50000 -1.50000 AFIX 0 MOLE 2 C22 1 0.269658 -0.132115 0.765966 11.00000 0.03142 0.02214 = 0.02862 -0.00829 -0.00243 -0.00691 AFIX 137 H22A 2 0.406605 -0.162190 0.716385 11.00000 -1.50000 H22B 2 0.187262 -0.165321 0.719231 11.00000 -1.50000 H22C 2 0.269124 -0.206875 0.875862 11.00000 -1.50000 AFIX 0 N21 3 0.188299 0.075805 0.745513 11.00000 0.01813 0.01924 = 0.01600 -0.00325 -0.00410 -0.00500 AFIX 137 H21A 2 0.059860 0.104410 0.788996 11.00000 -1.50000 H21B 2 0.192337 0.145263 0.643466 11.00000 -1.50000 H21C 2 0.262543 0.105922 0.791469 11.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 07skc0021p-1 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1A O1B C2 C2 - C1 C3 C3 - C3_$4 C2 C4 - C5 C4_$5 C5 - C6 C4 C6 - O6A O6B C5 O1A - C1 O1B - C1 O6A - C6 O6B - C6 C22 - N21 N21 - C22 Operators for generating equivalent atoms: $1 -x+1, -y, -z+2 $2 -x+2, -y+1, -z+1 $3 x-1, y, z $4 -x+1, -y+1, -z+1 $5 -x+2, -y+1, -z+2 6449 Reflections read, of which 38 rejected -9 =< h =< 9, -10 =< k =< 10, -12 =< l =< 12, Max. 2-theta = 54.96 0 Systematic absence violations 0 Inconsistent equivalents 2121 Unique reflections, of which 0 suppressed R(int) = 0.0463 R(sigma) = 0.0503 Friedel opposites merged Maximum memory for data reduction = 1722 / 21570 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 = 2069 / 145148 wR2 = 0.1197 before cycle 1 for 2121 data and 113 / 113 parameters GooF = S = 1.150; Restrained GooF = 1.150 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0177 * P )^2 + 0.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.39835 0.00337 0.002 OSF Mean shift/esd = 0.003 Maximum = -0.012 for U22 O1B Max. shift = 0.000 A for H6 Max. dU = 0.000 for C5 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2069 / 145148 wR2 = 0.1197 before cycle 2 for 2121 data and 113 / 113 parameters GooF = S = 1.150; Restrained GooF = 1.150 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0177 * P )^2 + 0.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.39834 0.00337 -0.003 OSF Mean shift/esd = 0.001 Maximum = -0.004 for U22 O1B Max. shift = 0.000 A for H6 Max. dU = 0.000 for C5 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2069 / 145148 wR2 = 0.1197 before cycle 3 for 2121 data and 113 / 113 parameters GooF = S = 1.150; Restrained GooF = 1.150 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0177 * P )^2 + 0.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.39834 0.00337 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x C4 Max. shift = 0.000 A for H22C Max. dU = 0.000 for O6B Least-squares cycle 4 Maximum vector length = 511 Memory required = 2069 / 145148 wR2 = 0.1197 before cycle 4 for 2121 data and 113 / 113 parameters GooF = S = 1.150; Restrained GooF = 1.150 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0177 * P )^2 + 0.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.39834 0.00337 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H1 Max. dU = 0.000 for O6B 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 H2A 0.6346 0.1698 0.5804 23 0.990 0.000 C2 C1 C3 H2B 0.7896 0.2642 0.5881 23 0.990 0.000 C2 C1 C3 H3A 0.3643 0.4347 0.6285 23 0.990 0.000 C3 C3_$4 C2 H3B 0.5199 0.5293 0.6351 23 0.990 0.000 C3 C3_$4 C2 H4A 1.1359 0.5069 0.8627 23 0.990 0.000 C4 C5 C4_$5 H4B 1.0184 0.3528 0.9403 23 0.990 0.000 C4 C5 C4_$5 H5A 0.7150 0.5904 0.8840 23 0.990 0.000 C5 C6 C4 H5B 0.8127 0.7575 0.8325 23 0.990 0.000 C5 C6 C4 H1 0.5038 0.0362 0.9579 147 0.840 0.000 O1B C1 H1 H6 0.9936 0.5073 0.5403 147 0.840 0.000 O6B C6 H6 H22A 0.4066 -0.1622 0.7164 137 0.980 0.000 C22 N21 H22A H22B 0.1873 -0.1653 0.7192 137 0.980 0.000 C22 N21 H22A H22C 0.2691 -0.2069 0.8759 137 0.980 0.000 C22 N21 H22A H21A 0.0599 0.1044 0.7890 137 0.910 0.000 N21 C22 H21A H21B 0.1923 0.1453 0.6435 137 0.910 0.000 N21 C22 H21A H21C 0.2625 0.1059 0.7915 137 0.910 0.000 N21 C22 H21A 07skc0021p-1 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.65326 0.14594 0.80080 1.00000 0.01799 0.01211 0.01634 -0.00394 -0.00201 -0.00312 0.01622 0.00238 0.00026 0.00025 0.00020 0.00000 0.00086 0.00086 0.00089 0.00070 0.00068 0.00068 0.00037 C2 0.65641 0.24950 0.62943 1.00000 0.01824 0.01850 0.01412 -0.00264 -0.00026 -0.00551 0.01822 0.00254 0.00027 0.00027 0.00020 0.00000 0.00088 0.00095 0.00089 0.00074 0.00068 0.00072 0.00039 H2A 0.63461 0.16980 0.58038 1.00000 0.02187 0.00000 0.00000 H2B 0.78965 0.26420 0.58811 1.00000 0.02187 0.00000 0.00000 C3 0.49771 0.44892 0.58699 1.00000 0.01869 0.01849 0.01431 -0.00367 -0.00080 -0.00556 0.01802 0.00250 0.00027 0.00027 0.00020 0.00000 0.00086 0.00095 0.00092 0.00074 0.00068 0.00072 0.00038 H3A 0.36433 0.43468 0.62850 1.00000 0.02162 0.00000 0.00000 H3B 0.51992 0.52933 0.63513 1.00000 0.02162 0.00000 0.00000 C4 1.01046 0.48668 0.92275 1.00000 0.02134 0.02080 0.01416 -0.00714 -0.00161 -0.00357 0.01937 0.00246 0.00027 0.00028 0.00020 0.00000 0.00091 0.00098 0.00092 0.00076 0.00071 0.00075 0.00040 H4A 1.13586 0.50690 0.86269 1.00000 0.02324 0.00000 0.00000 H4B 1.01836 0.35284 0.94027 1.00000 0.02324 0.00000 0.00000 C5 0.83573 0.62684 0.83123 1.00000 0.02598 0.02894 0.01689 -0.00983 -0.00541 0.00236 0.02611 0.00282 0.00030 0.00031 0.00022 0.00000 0.00103 0.00114 0.00100 0.00085 0.00079 0.00084 0.00046 H5A 0.71501 0.59042 0.88396 1.00000 0.03133 0.00000 0.00000 H5B 0.81271 0.75746 0.83254 1.00000 0.03133 0.00000 0.00000 C6 0.85970 0.63668 0.66581 1.00000 0.01754 0.02172 0.01491 -0.00518 -0.00203 -0.00709 0.01803 0.00239 0.00026 0.00028 0.00020 0.00000 0.00087 0.00098 0.00089 0.00075 0.00069 0.00074 0.00039 O1A 0.79491 0.10129 0.87271 1.00000 0.01732 0.03137 0.01987 -0.00236 -0.00538 -0.00845 0.02398 0.00180 0.00019 0.00021 0.00015 0.00000 0.00065 0.00082 0.00072 0.00061 0.00054 0.00058 0.00033 O1B 0.48927 0.10773 0.86624 1.00000 0.01868 0.02540 0.01430 0.00237 -0.00333 -0.01009 0.02109 0.00177 0.00019 0.00020 0.00014 0.00000 0.00065 0.00078 0.00066 0.00056 0.00051 0.00056 0.00031 H1 0.50376 0.03623 0.95793 0.50000 0.03164 0.00000 0.00000 O6A 0.76156 0.78223 0.57128 1.00000 0.03395 0.02489 0.01616 -0.00356 -0.00660 0.00112 0.02859 0.00203 0.00022 0.00021 0.00016 0.00000 0.00080 0.00080 0.00070 0.00059 0.00059 0.00062 0.00035 O6B 0.98406 0.48718 0.63497 1.00000 0.02844 0.02079 0.01540 -0.00766 -0.00522 -0.00144 0.02247 0.00179 0.00020 0.00019 0.00015 0.00000 0.00074 0.00073 0.00068 0.00057 0.00056 0.00057 0.00032 H6 0.99358 0.50729 0.54031 0.50000 0.03370 0.00000 0.00000 C22 0.26966 -0.13212 0.76597 1.00000 0.03142 0.02213 0.02862 -0.00829 -0.00243 -0.00691 0.02807 0.00291 0.00032 0.00030 0.00025 0.00000 0.00110 0.00108 0.00113 0.00089 0.00087 0.00086 0.00047 H22A 0.40661 -0.16219 0.71639 1.00000 0.04211 0.00000 0.00000 H22B 0.18726 -0.16533 0.71923 1.00000 0.04211 0.00000 0.00000 H22C 0.26912 -0.20688 0.87586 1.00000 0.04211 0.00000 0.00000 N21 0.18830 0.07581 0.74551 1.00000 0.01813 0.01924 0.01600 -0.00325 -0.00410 -0.00500 0.01850 0.00204 0.00022 0.00022 0.00018 0.00000 0.00075 0.00084 0.00077 0.00064 0.00059 0.00062 0.00034 H21A 0.05985 0.10441 0.78900 1.00000 0.02775 0.00000 0.00000 H21B 0.19234 0.14527 0.64347 1.00000 0.02775 0.00000 0.00000 H21C 0.26255 0.10592 0.79147 1.00000 0.02775 0.00000 0.00000 Final Structure Factor Calculation for 07skc0021p-1 in P-1 Total number of l.s. parameters = 113 Maximum vector length = 511 Memory required = 1956 / 22995 wR2 = 0.1197 before cycle 5 for 2121 data and 0 / 113 parameters GooF = S = 1.150; Restrained GooF = 1.150 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0177 * P )^2 + 0.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0546 for 1695 Fo > 4sig(Fo) and 0.0746 for all 2121 data wR2 = 0.1197, GooF = S = 1.150, Restrained GooF = 1.150 for all data Occupancy sum of asymmetric unit = 12.00 for non-hydrogen and 15.00 for hydrogen atoms Principal mean square atomic displacements U 0.0198 0.0168 0.0120 C1 0.0235 0.0181 0.0131 C2 0.0217 0.0184 0.0139 C3 0.0262 0.0188 0.0132 C4 0.0444 0.0190 0.0149 C5 0.0224 0.0170 0.0147 C6 0.0375 0.0202 0.0143 O1A 0.0350 0.0169 0.0115 O1B 0.0477 0.0240 0.0141 O6A 0.0352 0.0187 0.0135 O6B 0.0336 0.0286 0.0220 C22 0.0222 0.0192 0.0140 N21 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.021 0.033 0.046 0.060 0.078 0.096 0.128 0.182 1.000 Number in group 233. 192. 222. 215. 203. 214. 209. 212. 210. 211. GooF 1.185 1.193 1.304 1.202 1.170 1.166 1.039 0.919 0.933 1.312 K 4.593 1.714 1.057 0.986 1.003 0.989 1.016 1.007 1.014 1.017 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.32 1.65 inf Number in group 214. 210. 213. 212. 218. 209. 210. 210. 214. 211. GooF 1.213 1.132 1.188 1.070 1.092 1.095 1.076 1.032 1.126 1.430 K 1.065 1.054 1.029 1.046 1.010 1.016 0.979 1.000 1.012 1.022 R1 0.171 0.148 0.141 0.099 0.089 0.075 0.063 0.043 0.043 0.034 Recommended weighting scheme: WGHT 0.0177 0.3777 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 4 3 485.12 343.36 5.94 0.256 1.77 0 2 1 3543.06 2488.29 4.78 0.690 3.67 6 3 0 14.66 0.29 3.76 0.007 1.16 0 5 4 253.19 177.53 3.62 0.184 1.40 0 3 3 518.11 383.38 3.57 0.271 2.20 0 1 1 1579.51 1191.79 3.56 0.478 6.59 0 0 2 640.98 736.98 3.43 0.376 4.35 -1 -6 2 11.81 26.02 3.42 0.071 1.07 2 1 2 14.38 25.30 3.30 0.070 3.18 -1 -8 2 11.47 0.65 3.18 0.011 0.82 -4 0 7 15.94 5.18 3.13 0.032 0.95 5 9 3 15.69 1.21 3.04 0.015 0.85 6 3 7 2.22 8.04 2.99 0.039 1.00 -1 -1 1 3.18 8.50 2.93 0.040 4.19 -3 3 3 58.69 41.39 2.86 0.089 1.33 1 -1 1 5.40 11.75 2.84 0.047 3.59 0 3 2 217.56 175.15 2.74 0.183 2.40 -3 -4 6 4.61 0.37 2.74 0.008 0.92 7 -3 2 7.45 1.10 2.72 0.015 0.78 -2 5 4 26.00 39.24 2.71 0.087 1.14 0 6 5 116.05 92.55 2.62 0.133 1.16 2 -2 7 8.57 16.76 2.59 0.057 1.01 -1 3 5 4.19 14.72 2.59 0.053 1.52 -7 -3 1 31.18 44.46 2.57 0.092 0.97 8 6 1 1.32 5.64 2.55 0.033 0.84 1 2 3 0.63 3.94 2.54 0.027 2.88 -2 -2 8 2.49 8.04 2.54 0.039 0.91 0 7 1 13.73 2.83 2.53 0.023 1.02 8 8 5 -0.19 4.36 2.50 0.029 0.78 4 8 2 5.64 0.00 2.49 0.000 0.96 -3 0 9 4.96 0.14 2.48 0.005 0.86 6 7 0 20.97 34.52 2.47 0.081 0.90 0 -2 1 317.23 363.80 2.47 0.264 2.91 1 1 8 17.17 26.76 2.45 0.072 1.15 -2 -1 9 17.31 9.41 2.45 0.042 0.87 -1 1 1 3060.06 3319.57 2.44 0.797 4.00 -4 -2 6 90.78 0.77 2.41 0.012 0.99 -1 5 11 181.49 152.11 2.41 0.171 0.78 1 6 10 36.24 25.61 2.40 0.070 0.87 9 6 5 4.65 0.06 2.38 0.003 0.78 9 1 1 11.30 2.84 2.38 0.023 0.77 1 -5 4 52.26 69.41 2.36 0.115 0.99 -2 -1 7 34.30 46.13 2.35 0.094 1.08 3 3 1 163.87 140.48 2.35 0.164 2.07 2 -3 5 94.26 119.28 2.34 0.151 1.11 -5 5 0 2.69 0.07 2.32 0.004 0.84 3 -3 8 36.61 20.49 2.31 0.063 0.81 -4 4 6 -1.46 1.51 2.30 0.017 0.91 -4 0 2 -0.18 1.75 2.30 0.018 1.51 8 2 3 -2.11 3.28 2.30 0.025 0.89 Bond lengths and angles C1 - Distance Angles O1A 1.2336 (0.0021) O1B 1.2974 (0.0021) 122.70 (0.16) C2 1.5109 (0.0024) 122.81 (0.16) 114.49 (0.15) C1 - O1A O1B C2 - Distance Angles C1 1.5109 (0.0024) C3 1.5318 (0.0025) 112.82 (0.15) H2A 0.9900 109.02 109.02 H2B 0.9900 109.02 109.02 107.80 C2 - C1 C3 H2A C3 - Distance Angles C3_$4 1.5305 (0.0035) C2 1.5318 (0.0025) 112.08 (0.19) H3A 0.9900 109.19 109.19 H3B 0.9900 109.19 109.19 107.90 C3 - C3_$4 C2 H3A C4 - Distance Angles C5 1.5206 (0.0026) C4_$5 1.5263 (0.0034) 111.63 (0.19) H4A 0.9900 109.29 109.29 H4B 0.9900 109.29 109.29 107.95 C4 - C5 C4_$5 H4A C5 - Distance Angles C6 1.5127 (0.0025) C4 1.5206 (0.0026) 115.61 (0.15) H5A 0.9900 108.38 108.38 H5B 0.9900 108.38 108.38 107.44 C5 - C6 C4 H5A C6 - Distance Angles O6A 1.2347 (0.0023) O6B 1.2835 (0.0023) 124.61 (0.17) C5 1.5127 (0.0025) 119.72 (0.17) 115.67 (0.16) C6 - O6A O6B O1A - Distance Angles C1 1.2336 (0.0021) O1A - O1B - Distance Angles C1 1.2974 (0.0021) H1 0.8400 109.47 O1B - C1 O6A - Distance Angles C6 1.2347 (0.0023) O6A - O6B - Distance Angles C6 1.2835 (0.0023) H6 0.8400 109.47 O6B - C6 C22 - Distance Angles N21 1.4760 (0.0025) H22A 0.9800 109.47 H22B 0.9800 109.47 109.47 H22C 0.9800 109.47 109.47 109.47 C22 - N21 H22A H22B N21 - Distance Angles C22 1.4760 (0.0025) H21A 0.9100 109.47 H21B 0.9100 109.47 109.47 H21C 0.9100 109.47 109.47 109.47 N21 - C22 H21A H21B Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.91 1.95 2.828(2) 161.6 N21-H21C...O1B 0.84 1.62 2.453(2) 173.6 O1B-H1...O1B_$1 0.84 1.62 2.452(3) 171.6 O6B-H6...O6B_$2 0.91 1.91 2.799(2) 164.3 N21-H21A...O1A_$3 0.91 1.87 2.760(2) 163.5 N21-H21B...O6A_$4 FMAP and GRID set by program FMAP 2 1 21 GRID -2.778 -2 -2 2.778 2 2 R1 = 0.0746 for 2121 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.36 at 0.3557 0.7834 0.2838 [ 0.76 A from C2 ] Deepest hole -0.26 at 0.0160 0.4431 0.8010 [ 1.24 A from H4B ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 2013 / 16365 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.6443 0.2166 0.7162 1.00000 0.05 0.36 0.76 C2 0.78 C1 1.44 H2B 1.50 H2A Q2 1 1.0000 0.5000 1.0000 0.50000 0.05 0.31 0.76 C4 1.44 H4A 1.44 H4B 1.44 H4A Q3 1 0.8360 0.6122 0.7559 1.00000 0.05 0.28 0.77 C5 0.79 C6 1.32 H5A 1.53 H5B Q4 1 0.3526 0.0167 0.9753 1.00000 0.05 0.26 1.13 H1 1.20 H1 1.44 O1B 1.76 O1A Q5 1 0.9029 0.1585 0.8010 1.00000 0.05 0.26 1.03 O1A 1.05 H21A 1.86 C1 1.94 N21 Q6 1 0.8966 0.5441 0.8856 1.00000 0.05 0.26 0.72 C5 0.86 C4 1.23 H5A 1.40 H4B Q7 1 0.7791 0.0267 0.9782 1.00000 0.05 0.25 0.95 O1A 1.84 C1 2.03 H1 2.03 H21C Q8 1 0.1165 0.0548 0.9359 1.00000 0.05 0.24 1.41 H21A 1.54 H21C 1.72 N21 1.86 O1A Q9 1 0.1159 0.1396 0.8383 1.00000 0.05 0.24 0.86 H21A 1.03 H21C 1.11 N21 1.79 H21B Q10 1 0.3572 0.0918 0.8771 1.00000 0.05 0.23 0.99 O1B 1.13 H21C 1.30 H1 1.80 H1 Shortest distances between peaks (including symmetry equivalents) 4 10 0.89 8 9 0.91 4 7 1.08 7 8 1.08 3 6 1.25 2 6 1.33 5 9 1.61 7 10 1.68 4 8 1.73 9 10 1.75 8 10 1.81 5 7 1.84 7 9 1.85 5 8 1.97 1 5 2.04 4 9 2.10 8 8 2.11 4 4 2.20 5 8 2.42 7 8 2.48 4 10 2.50 2 3 2.55 1 7 2.56 1 10 2.56 6 6 2.65 8 9 2.75 4 5 2.78 7 9 2.79 1 4 2.79 Time profile in seconds ----------------------- 0.08: 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 0.02: 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. 0.30: 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 0.19: Structure factors and derivatives 0.25: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.05: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.00: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 07skc0021p-1 finished at 12:29:48 Total CPU time: 1.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++