+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 07skc0024p21c started at 16:19:36 on 21-Jan-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 07skc0024p21c in P2(1)/c CELL 0.71073 5.5883 22.5838 7.3581 90.000 98.578 90.000 ZERR 4.00 0.0002 0.0012 0.0004 0.000 0.003 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 32 40 8 16 V = 918.24 F(000) = 416.0 Mu = 0.12 mm-1 Cell Wt = 792.72 Rho = 1.434 MERG 2 OMIT -3.00 55.00 EXTI 0.03402 SHEL 7 0.77 HTAB O4A O1A HTAB N21 O4B EQIV_$1 -x+1, -y+1, -z+2 HTAB N23 O1B_$1 HTAB N23 O1A_$1 FMAP 2 PLAN 10 SIZE 0.14 0.26 0.40 ACTA BOND $H WGHT 0.08060 0.05040 L.S. 4 TEMP -153.00 FVAR 0.73699 MOLE 1 C1 1 -0.033472 0.593434 0.836408 11.00000 0.02207 0.01943 = 0.02562 0.00312 0.00597 0.00130 C2 1 -0.241364 0.556304 0.750945 11.00000 0.01981 0.02237 = 0.02995 0.00423 0.00205 0.00139 AFIX 43 H2 2 -0.393504 0.575885 0.731861 11.00000 -1.20000 AFIX 0 C3 1 -0.246045 0.499600 0.697089 11.00000 0.01882 0.02269 = 0.02658 0.00368 -0.00156 -0.00093 AFIX 43 H3 2 -0.402234 0.485139 0.648717 11.00000 -1.20000 AFIX 0 C4 1 -0.046702 0.455202 0.700288 11.00000 0.02134 0.02188 = 0.02537 0.00010 0.00180 -0.00359 O1A 4 0.179184 0.570731 0.873197 11.00000 0.01838 0.02207 = 0.03955 -0.00423 -0.00058 0.00064 O1B 4 -0.074272 0.646048 0.873293 11.00000 0.02775 0.01817 = 0.03529 -0.00040 0.00479 0.00210 O4A 4 0.171608 0.469343 0.769150 11.00000 0.02069 0.01722 = 0.04714 -0.00784 -0.00036 0.00073 AFIX 147 H4 2 0.175285 0.504881 0.803147 11.00000 -1.50000 AFIX 0 O4B 4 -0.100141 0.405486 0.636975 11.00000 0.02943 0.02064 = 0.03818 -0.00461 -0.00041 -0.00282 MOLE 2 C22 1 0.476532 0.358638 0.853825 11.00000 0.02425 0.01707 = 0.02866 -0.00130 0.00447 -0.00058 AFIX 43 H22 2 0.493095 0.399945 0.876700 11.00000 -1.20000 AFIX 0 C24 1 0.550313 0.262319 0.857359 11.00000 0.02998 0.01794 = 0.02424 0.00037 0.01016 -0.00229 C25 1 0.331118 0.272238 0.754042 11.00000 0.02880 0.02012 = 0.02740 -0.00328 0.00936 -0.00444 AFIX 43 H25 2 0.225626 0.243017 0.693617 11.00000 -1.20000 AFIX 0 C26 1 0.688645 0.206801 0.904746 11.00000 0.03843 0.01966 = 0.03360 -0.00099 0.01008 0.00361 AFIX 137 H26A 2 0.598683 0.173180 0.844296 11.00000 -1.50000 H26B 2 0.711660 0.201017 1.038215 11.00000 -1.50000 H26C 2 0.846765 0.209614 0.862961 11.00000 -1.50000 AFIX 0 N21 3 0.289848 0.332711 0.753039 11.00000 0.02284 0.02119 = 0.02838 -0.00158 0.00364 -0.00094 AFIX 43 H21 2 0.161196 0.350829 0.695149 11.00000 -1.20000 AFIX 0 N23 3 0.636606 0.317575 0.917635 11.00000 0.02323 0.01863 = 0.02707 -0.00161 0.00277 -0.00077 AFIX 43 H23 2 0.776009 0.324320 0.987417 11.00000 -1.20000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 07skc0024p21c in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1B O1A C2 C2 - C3 C1 C3 - C2 C4 C4 - O4B O4A C3 O1A - C1 O1B - C1 O4A - C4 O4B - C4 C22 - N21 N23 C24 - C25 N23 C26 C25 - C24 N21 C26 - C24 N21 - C22 C25 N23 - C22 C24 Operators for generating equivalent atoms: $1 -x+1, -y+1, -z+2 10605 Reflections read, of which 209 rejected -7 =< h =< 6, -29 =< k =< 29, -9 =< l =< 9, Max. 2-theta = 54.97 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 4 7 6 -2.79 2.59 2 14.44 1 Inconsistent equivalents 2102 Unique reflections, of which 0 suppressed R(int) = 0.0623 R(sigma) = 0.0576 Friedel opposites merged Maximum memory for data reduction = 1481 / 21008 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 = 1839 / 164630 wR2 = 0.1421 before cycle 1 for 2102 data and 130 / 130 parameters GooF = S = 1.045; Restrained GooF = 1.045 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0806 * P )^2 + 0.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.73706 0.00282 0.025 OSF 2 0.03418 0.00622 0.026 EXTI Mean shift/esd = 0.011 Maximum = 0.038 for U11 O1A Max. shift = 0.000 A for H4 Max. dU = 0.000 for C22 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1839 / 164630 wR2 = 0.1421 before cycle 2 for 2102 data and 130 / 130 parameters GooF = S = 1.045; Restrained GooF = 1.045 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0806 * P )^2 + 0.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.73712 0.00282 0.020 OSF 2 0.03425 0.00623 0.011 EXTI Mean shift/esd = 0.004 Maximum = 0.020 for OSF Max. shift = 0.000 A for H4 Max. dU = 0.000 for C2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1839 / 164630 wR2 = 0.1421 before cycle 3 for 2102 data and 130 / 130 parameters GooF = S = 1.045; Restrained GooF = 1.045 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0806 * P )^2 + 0.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.73712 0.00282 0.001 OSF 2 0.03426 0.00624 0.001 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for U11 C25 Max. shift = 0.000 A for H4 Max. dU = 0.000 for C25 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1839 / 164630 wR2 = 0.1421 before cycle 4 for 2102 data and 130 / 130 parameters GooF = S = 1.045; Restrained GooF = 1.045 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0806 * P )^2 + 0.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.73712 0.00282 0.000 OSF 2 0.03426 0.00624 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y O1B Max. shift = 0.000 A for H26C Max. dU = 0.000 for C25 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 H2 -0.3935 0.5759 0.7319 43 0.950 0.000 C2 C3 C1 H3 -0.4022 0.4851 0.6487 43 0.950 0.000 C3 C2 C4 H4 0.1753 0.5049 0.8031 147 0.840 0.000 O4A C4 H4 H22 0.4931 0.3999 0.8767 43 0.950 0.000 C22 N21 N23 H25 0.2256 0.2430 0.6936 43 0.950 0.000 C25 C24 N21 H26A 0.5987 0.1732 0.8443 137 0.980 0.000 C26 C24 H26A H26B 0.7117 0.2010 1.0382 137 0.980 0.000 C26 C24 H26A H26C 0.8468 0.2096 0.8630 137 0.980 0.000 C26 C24 H26A H21 0.1612 0.3508 0.6951 43 0.880 0.000 N21 C22 C25 H23 0.7760 0.3243 0.9874 43 0.880 0.000 N23 C22 C24 07skc0024p21c in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.03347 0.59343 0.83641 1.00000 0.02207 0.01944 0.02565 0.00311 0.00598 0.00130 0.02214 0.00326 0.00029 0.00008 0.00025 0.00000 0.00092 0.00098 0.00101 0.00075 0.00071 0.00070 0.00042 C2 -0.24136 0.55630 0.75095 1.00000 0.01985 0.02238 0.02998 0.00423 0.00206 0.00139 0.02424 0.00334 0.00031 0.00008 0.00026 0.00000 0.00086 0.00099 0.00107 0.00077 0.00070 0.00069 0.00044 H2 -0.39350 0.57589 0.73186 1.00000 0.02908 0.00000 0.00000 C3 -0.24605 0.49960 0.69709 1.00000 0.01884 0.02270 0.02660 0.00368 -0.00155 -0.00093 0.02321 0.00330 0.00030 0.00008 0.00025 0.00000 0.00084 0.00099 0.00108 0.00076 0.00069 0.00070 0.00044 H3 -0.40224 0.48514 0.64872 1.00000 0.02786 0.00000 0.00000 C4 -0.04670 0.45520 0.70029 1.00000 0.02135 0.02190 0.02539 0.00009 0.00180 -0.00358 0.02305 0.00322 0.00030 0.00008 0.00025 0.00000 0.00090 0.00101 0.00100 0.00077 0.00068 0.00071 0.00043 O1A 0.17918 0.57073 0.87320 1.00000 0.01841 0.02207 0.03956 -0.00421 -0.00057 0.00063 0.02718 0.00219 0.00020 0.00006 0.00018 0.00000 0.00065 0.00072 0.00085 0.00060 0.00052 0.00051 0.00036 O1B -0.07427 0.64605 0.87330 1.00000 0.02777 0.01819 0.03531 -0.00039 0.00479 0.00209 0.02708 0.00233 0.00022 0.00006 0.00018 0.00000 0.00072 0.00072 0.00084 0.00055 0.00055 0.00051 0.00037 O4A 0.17161 0.46934 0.76915 1.00000 0.02070 0.01725 0.04715 -0.00784 -0.00035 0.00072 0.02892 0.00222 0.00021 0.00006 0.00019 0.00000 0.00065 0.00070 0.00090 0.00061 0.00055 0.00051 0.00037 H4 0.17529 0.50489 0.80310 1.00000 0.04338 0.00000 0.00000 O4B -0.10014 0.40549 0.63697 1.00000 0.02945 0.02067 0.03819 -0.00461 -0.00041 -0.00282 0.02999 0.00227 0.00022 0.00006 0.00019 0.00000 0.00072 0.00075 0.00087 0.00060 0.00057 0.00056 0.00037 C22 0.47653 0.35864 0.85383 1.00000 0.02428 0.01710 0.02868 -0.00130 0.00448 -0.00058 0.02330 0.00328 0.00030 0.00008 0.00025 0.00000 0.00090 0.00093 0.00108 0.00076 0.00073 0.00069 0.00043 H22 0.49309 0.39995 0.87671 1.00000 0.02796 0.00000 0.00000 C24 0.55032 0.26232 0.85736 1.00000 0.03000 0.01795 0.02427 0.00037 0.01016 -0.00229 0.02345 0.00330 0.00031 0.00008 0.00026 0.00000 0.00097 0.00095 0.00105 0.00072 0.00075 0.00071 0.00044 C25 0.33111 0.27224 0.75404 1.00000 0.02880 0.02015 0.02742 -0.00327 0.00935 -0.00443 0.02493 0.00346 0.00032 0.00008 0.00026 0.00000 0.00091 0.00099 0.00109 0.00077 0.00075 0.00074 0.00044 H25 0.22562 0.24302 0.69362 1.00000 0.02992 0.00000 0.00000 C26 0.68864 0.20680 0.90475 1.00000 0.03844 0.01968 0.03362 -0.00098 0.01009 0.00361 0.03010 0.00382 0.00035 0.00009 0.00029 0.00000 0.00107 0.00098 0.00115 0.00083 0.00083 0.00079 0.00047 H26A 0.59868 0.17318 0.84430 1.00000 0.04515 0.00000 0.00000 H26B 0.71166 0.20102 1.03821 1.00000 0.04515 0.00000 0.00000 H26C 0.84676 0.20961 0.86296 1.00000 0.04515 0.00000 0.00000 N21 0.28984 0.33271 0.75304 1.00000 0.02286 0.02121 0.02840 -0.00158 0.00365 -0.00093 0.02417 0.00271 0.00026 0.00007 0.00021 0.00000 0.00079 0.00086 0.00095 0.00066 0.00062 0.00061 0.00040 H21 0.16119 0.35083 0.69514 1.00000 0.02901 0.00000 0.00000 N23 0.63661 0.31758 0.91764 1.00000 0.02326 0.01863 0.02709 -0.00161 0.00278 -0.00077 0.02309 0.00275 0.00026 0.00007 0.00022 0.00000 0.00078 0.00079 0.00091 0.00064 0.00062 0.00060 0.00039 H23 0.77601 0.32432 0.98741 1.00000 0.02771 0.00000 0.00000 Final Structure Factor Calculation for 07skc0024p21c in P2(1)/c Total number of l.s. parameters = 130 Maximum vector length = 511 Memory required = 1709 / 22995 wR2 = 0.1421 before cycle 5 for 2102 data and 0 / 130 parameters GooF = S = 1.045; Restrained GooF = 1.045 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0806 * P )^2 + 0.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0519 for 1467 Fo > 4sig(Fo) and 0.0854 for all 2102 data wR2 = 0.1421, GooF = S = 1.045, Restrained GooF = 1.045 for all data Occupancy sum of asymmetric unit = 14.00 for non-hydrogen and 10.00 for hydrogen atoms Principal mean square atomic displacements U 0.0278 0.0205 0.0182 C1 0.0322 0.0219 0.0186 C2 0.0316 0.0210 0.0170 C3 0.0270 0.0241 0.0180 C4 0.0425 0.0211 0.0179 O1A 0.0354 0.0282 0.0177 O1B 0.0511 0.0203 0.0153 O4A 0.0422 0.0294 0.0184 O4B 0.0288 0.0241 0.0169 C22 0.0333 0.0204 0.0167 C24 0.0345 0.0221 0.0182 C25 0.0410 0.0307 0.0186 C26 0.0288 0.0232 0.0206 N21 0.0277 0.0233 0.0182 N23 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 0.041 0.052 0.067 0.090 0.130 1.000 Number in group 227. 208. 210. 206. 223. 195. 206. 209. 207. 211. GooF 0.824 0.917 1.071 1.123 1.112 1.238 1.059 0.997 0.970 1.105 K 0.046 0.898 0.880 0.834 0.944 0.951 0.991 1.014 1.044 1.036 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.66 inf Number in group 210. 214. 209. 214. 203. 216. 207. 207. 212. 210. GooF 0.954 0.934 0.963 1.050 0.985 1.003 0.989 1.024 1.034 1.427 K 0.876 0.983 0.997 0.980 1.033 1.023 1.039 1.025 1.048 1.028 R1 0.290 0.231 0.157 0.123 0.088 0.070 0.049 0.045 0.039 0.049 Recommended weighting scheme: WGHT 0.0809 0.0479 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) 1 2 0 4592.95 8977.42 5.77 0.648 4.96 1 0 0 511.79 958.94 5.55 0.212 5.53 0 1 1 431.21 794.37 5.44 0.193 6.93 1 0 2 110.83 161.15 3.97 0.087 2.85 -2 5 1 37.62 56.34 3.97 0.051 2.33 0 1 2 82.35 118.00 3.87 0.074 3.59 2 10 1 8.61 2.81 3.32 0.011 1.66 -1 10 4 2.12 9.33 3.00 0.021 1.41 0 4 0 6.38 14.37 2.97 0.026 5.65 -2 10 3 13.89 22.28 2.87 0.032 1.49 0 5 4 8.07 3.80 2.86 0.013 1.69 1 16 4 29.25 45.81 2.85 0.046 1.07 3 11 4 11.50 18.97 2.84 0.030 1.04 -3 6 1 13.13 19.50 2.83 0.030 1.66 -1 1 2 26844.92 21384.47 2.80 1.000 3.24 1 13 4 18.95 28.56 2.79 0.037 1.20 3 7 0 123.24 90.25 2.75 0.065 1.60 -3 11 5 14.01 23.75 2.74 0.033 1.06 2 17 6 -2.58 10.53 2.74 0.022 0.83 -1 6 1 333.91 425.97 2.73 0.141 2.95 2 2 0 247.24 197.37 2.72 0.096 2.68 3 18 2 219.12 169.08 2.71 0.089 0.98 6 6 1 -6.28 36.57 2.70 0.041 0.87 -1 16 2 19.12 9.95 2.68 0.022 1.30 0 2 1 497.14 631.88 2.67 0.172 6.12 -5 10 5 -3.71 7.12 2.67 0.018 0.88 2 20 3 69.70 94.50 2.66 0.066 0.94 2 1 4 176.01 139.05 2.63 0.081 1.42 1 1 3 8.49 12.61 2.61 0.024 2.10 6 4 1 14.58 39.49 2.61 0.043 0.89 2 6 2 55.19 71.35 2.59 0.058 1.81 2 21 2 9.66 1.70 2.58 0.009 0.95 3 22 0 152.08 108.80 2.58 0.071 0.90 5 2 4 9.98 21.57 2.57 0.032 0.88 6 6 0 1.54 14.27 2.57 0.026 0.89 -2 1 7 37.57 54.99 2.56 0.051 1.02 -1 4 2 19.28 26.13 2.56 0.035 2.83 1 9 3 105.58 79.69 2.53 0.061 1.61 3 1 2 37.45 48.38 2.52 0.048 1.55 4 4 4 48.57 63.67 2.51 0.055 1.01 3 16 0 5.84 11.33 2.50 0.023 1.12 -3 4 1 45.50 34.12 2.50 0.040 1.76 0 26 4 -0.23 14.09 2.47 0.026 0.78 -1 7 1 378.37 308.30 2.42 0.120 2.67 1 15 1 34.04 25.00 2.41 0.034 1.41 -3 21 4 115.83 85.11 2.39 0.063 0.85 -6 7 5 16.83 0.02 2.38 0.001 0.81 -4 6 3 -1.40 1.90 2.38 0.009 1.22 1 18 0 87.73 66.21 2.37 0.056 1.22 5 7 2 22.52 33.15 2.35 0.039 0.97 Bond lengths and angles C1 - Distance Angles O1B 1.2474 (0.0022) O1A 1.2855 (0.0021) 121.83 (0.16) C2 1.4934 (0.0025) 118.07 (0.15) 120.09 (0.16) C1 - O1B O1A C2 - Distance Angles C3 1.3396 (0.0027) C1 1.4934 (0.0025) 129.86 (0.17) H2 0.9500 115.07 115.07 C2 - C3 C1 C3 - Distance Angles C2 1.3396 (0.0027) C4 1.4964 (0.0025) 130.86 (0.17) H3 0.9500 114.57 114.57 C3 - C2 C4 C4 - Distance Angles O4B 1.2350 (0.0022) O4A 1.2894 (0.0021) 122.33 (0.17) C3 1.4964 (0.0025) 117.75 (0.16) 119.92 (0.16) C4 - O4B O4A O1A - Distance Angles C1 1.2855 (0.0021) O1A - O1B - Distance Angles C1 1.2474 (0.0022) O1B - O4A - Distance Angles C4 1.2894 (0.0021) H4 0.8400 109.47 O4A - C4 O4B - Distance Angles C4 1.2350 (0.0022) O4B - C22 - Distance Angles N21 1.3231 (0.0023) N23 1.3249 (0.0024) 108.85 (0.16) H22 0.9500 125.57 125.57 C22 - N21 N23 C24 - Distance Angles C25 1.3605 (0.0027) N23 1.3866 (0.0023) 105.77 (0.16) C26 1.4869 (0.0026) 131.54 (0.17) 122.69 (0.16) C24 - C25 N23 C25 - Distance Angles C24 1.3605 (0.0027) N21 1.3849 (0.0024) 107.50 (0.16) H25 0.9500 126.25 126.25 C25 - C24 N21 C26 - Distance Angles C24 1.4869 (0.0026) H26A 0.9800 109.47 H26B 0.9800 109.47 109.47 H26C 0.9800 109.47 109.47 109.47 C26 - C24 H26A H26B N21 - Distance Angles C22 1.3231 (0.0023) C25 1.3849 (0.0024) 108.46 (0.15) H21 0.8800 125.77 125.77 N21 - C22 C25 N23 - Distance Angles C22 1.3249 (0.0024) C24 1.3866 (0.0023) 109.41 (0.16) H23 0.8800 125.29 125.29 N23 - C22 C24 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.57 2.4127(18) 178.0 O4A-H4...O1A 0.88 1.91 2.761(2) 161.9 N21-H21...O4B 0.88 1.94 2.811(2) 169.6 N23-H23...O1B_$1 0.88 2.58 3.0526(19) 114.6 N23-H23...O1A_$1 FMAP and GRID set by program FMAP 2 1 16 GRID -3.846 24 -2 3.846 1 2 R1 = 0.0854 for 2102 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.29 at 0.0930 0.7405 0.5111 [ 1.17 A from H26C ] Deepest hole -0.38 at 0.1091 0.5014 0.7985 [ 0.38 A from H4 ] Mean = 0.00, Rms deviation from mean = 0.10 e/A^3, Highest memory used = 2076 / 22387 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.9070 0.2405 0.9889 1.00000 0.05 0.29 1.17 H26C 1.49 C26 1.50 H26B 2.03 H23 Q2 1 -0.0270 0.7021 0.9044 1.00000 0.05 0.28 1.31 O1B 1.54 H25 1.62 H23 2.35 H26C Q3 1 -0.4394 0.4238 0.5954 1.00000 0.05 0.27 1.45 H3 1.92 O4B 2.10 C3 2.22 H22 Q4 1 0.3893 0.5624 0.9805 1.00000 0.05 0.27 1.33 O1A 1.43 H22 2.09 H4 2.23 C22 Q5 1 -0.4681 0.5009 0.5718 1.00000 0.05 0.27 0.72 H3 1.43 C3 1.70 H3 2.07 H2 Q6 1 -0.5292 0.4691 0.5107 1.00000 0.05 0.26 1.20 H3 1.57 H3 1.96 C3 2.04 H2 Q7 1 -0.4422 0.4667 0.6356 1.00000 0.05 0.26 0.48 H3 1.35 C3 2.21 C4 2.36 O4B Q8 1 -0.3113 0.4095 0.5767 1.00000 0.05 0.26 1.20 O4B 1.88 H3 1.92 C4 2.23 C3 Q9 1 0.4576 0.4670 0.8260 1.00000 0.05 0.25 1.57 H22 1.59 O4A 1.67 H3 1.78 H4 Q10 1 -0.5531 0.4403 0.6935 1.00000 0.05 0.25 1.39 H3 1.62 H22 1.83 O4A 2.17 C3 Shortest distances between peaks (including symmetry equivalents) 3 8 0.81 5 6 0.89 5 7 0.90 5 6 0.91 6 7 0.97 7 10 1.00 3 7 1.01 5 5 1.06 3 10 1.09 9 10 1.14 3 6 1.26 6 6 1.45 6 10 1.52 7 8 1.58 7 9 1.58 1 2 1.61 4 9 1.68 5 7 1.70 5 10 1.74 3 5 1.75 6 7 1.80 6 8 1.83 8 10 1.84 3 9 2.11 3 5 2.12 5 9 2.12 5 8 2.24 6 9 2.33 5 10 2.38 4 10 2.44 4 9 2.49 7 7 2.50 5 8 2.53 3 6 2.54 6 10 2.62 8 9 2.72 4 7 2.87 6 8 2.92 9 9 2.94 6 9 2.95 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 0.00: 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. 0.48: 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 0.31: Structure factors and derivatives 0.27: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.06: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 07skc0024p21c finished at 16:19:38 Total CPU time: 1.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++