+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 07skc0020p21c started at 12:17:34 on 23-Jan-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 07skc0020p21c in P2(1)/c CELL 0.71073 5.7536 14.8551 10.1829 90.000 100.799 90.000 ZERR 2.00 0.0006 0.0024 0.0015 0.000 0.009 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 28 48 4 16 V = 854.92 F(000) = 372.0 Mu = 0.11 mm-1 Cell Wt = 696.70 Rho = 1.353 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 HTAB O4A O1B EQIV_$1 x-1, y, z HTAB N22 O1A_$1 FMAP 2 PLAN 10 SIZE 0.01 0.04 0.20 ACTA BOND $H WGHT 0.00000 2.58650 L.S. 4 TEMP -153.00 FVAR 0.73026 MOLE 1 C1 1 0.477449 0.418990 0.706190 11.00000 0.02504 0.02619 = 0.03164 -0.00018 0.00802 -0.00434 C2 1 0.254357 0.416540 0.604579 11.00000 0.01890 0.03042 = 0.03155 -0.00293 0.00677 -0.00098 AFIX 43 H2 2 0.116544 0.434195 0.636785 11.00000 -1.20000 AFIX 0 C3 1 0.217060 0.393542 0.475675 11.00000 0.01933 0.03130 = 0.02742 0.00264 0.00268 0.00717 AFIX 43 H3 2 0.057118 0.398445 0.430953 11.00000 -1.20000 AFIX 0 C4 1 0.383638 0.361455 0.389838 11.00000 0.02721 0.02219 = 0.02208 0.00169 0.00245 -0.00138 O1A 4 0.456697 0.430799 0.825020 11.00000 0.02784 0.04013 = 0.02273 -0.00491 0.00578 0.00357 O1B 4 0.677403 0.409029 0.671002 11.00000 0.02006 0.04844 = 0.02659 -0.00497 0.00489 -0.00173 O4A 4 0.612578 0.364957 0.435212 11.00000 0.02361 0.04387 = 0.02622 -0.00310 0.00694 0.00154 AFIX 147 H4 2 0.637841 0.381942 0.515309 11.00000 0.05011 AFIX 0 O4B 4 0.303733 0.332531 0.278453 11.00000 0.03355 0.04730 = 0.02582 -0.00877 0.00461 -0.00572 MOLE 2 C21 1 -0.266470 0.346426 1.114261 11.00000 0.03050 0.03263 = 0.02632 0.00188 0.00810 -0.00451 AFIX 137 H21A 2 -0.354968 0.292473 1.079310 11.00000 0.03752 H21B 2 -0.374179 0.389686 1.144157 11.00000 0.02651 H21C 2 -0.141838 0.329826 1.189831 11.00000 0.02484 AFIX 0 C23 1 -0.026821 0.472200 1.058504 11.00000 0.02673 0.02621 = 0.01823 -0.00299 0.00482 0.00082 AFIX 23 H23A 2 0.122749 0.456146 1.119195 11.00000 0.03363 H23B 2 -0.124381 0.508000 1.109759 11.00000 0.02593 AFIX 0 C27 1 -0.003886 0.321768 0.953601 11.00000 0.03306 0.02515 = 0.03454 -0.00217 0.00862 0.00234 AFIX 137 H27A 2 0.064577 0.349790 0.882445 11.00000 -1.50000 H27B 2 -0.098860 0.269510 0.917627 11.00000 -1.50000 H27C 2 0.123456 0.302317 1.025918 11.00000 -1.50000 AFIX 0 N22 3 -0.157075 0.388138 1.006489 11.00000 0.02405 0.02423 = 0.02349 -0.00247 0.00371 -0.00244 AFIX 13 H22 2 -0.278605 0.404402 0.936803 11.00000 0.06486 AFIX 0 HKLF 4 Covalent radii and connectivity table for 07skc0020p21c in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1A O1B C2 C2 - C3 C1 C3 - C2 C4 C4 - O4B O4A C3 O1A - C1 O1B - C1 O4A - C4 O4B - C4 C21 - N22 C23 - N22 C23_$2 C27 - N22 N22 - C27 C21 C23 Operators for generating equivalent atoms: $1 x-1, y, z $2 -x, -y+1, -z+2 8850 Reflections read, of which 258 rejected -7 =< h =< 7, -19 =< k =< 19, -13 =< l =< 13, Max. 2-theta = 54.96 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 5 6 4 8.23 4.11 2 22.38 1 Inconsistent equivalents 1949 Unique reflections, of which 0 suppressed R(int) = 0.0894 R(sigma) = 0.0942 Friedel opposites merged Maximum memory for data reduction = 1419 / 19544 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 = 1754 / 151991 wR2 = 0.1836 before cycle 1 for 1949 data and 119 / 119 parameters GooF = S = 1.159; Restrained GooF = 1.159 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 2.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.73027 0.00259 0.002 OSF Mean shift/esd = 0.001 Maximum = 0.002 for OSF Max. shift = 0.000 A for H27B Max. dU = 0.000 for H23B Least-squares cycle 2 Maximum vector length = 511 Memory required = 1754 / 151991 wR2 = 0.1836 before cycle 2 for 1949 data and 119 / 119 parameters GooF = S = 1.159; Restrained GooF = 1.159 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 2.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.73027 0.00259 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for U11 O1B Max. shift = 0.000 A for H4 Max. dU = 0.000 for H21B Least-squares cycle 3 Maximum vector length = 511 Memory required = 1754 / 151991 wR2 = 0.1836 before cycle 3 for 1949 data and 119 / 119 parameters GooF = S = 1.159; Restrained GooF = 1.159 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 2.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.73027 0.00259 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H27A Max. dU = 0.000 for H4 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1754 / 151991 wR2 = 0.1836 before cycle 4 for 1949 data and 119 / 119 parameters GooF = S = 1.159; Restrained GooF = 1.159 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 2.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.73027 0.00259 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z N22 Max. shift = 0.000 A for H4 Max. dU = 0.000 for H23B 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 0.1165 0.4342 0.6368 43 0.950 0.000 C2 C3 C1 H3 0.0571 0.3984 0.4310 43 0.950 0.000 C3 C2 C4 H4 0.6378 0.3819 0.5153 147 0.840 0.000 O4A C4 H4 H21A -0.3550 0.2925 1.0793 137 0.980 0.000 C21 N22 H21A H21B -0.3742 0.3897 1.1442 137 0.980 0.000 C21 N22 H21A H21C -0.1418 0.3298 1.1898 137 0.980 0.000 C21 N22 H21A H23A 0.1227 0.4561 1.1192 23 0.990 0.000 C23 N22 C23_$2 H23B -0.1244 0.5080 1.1098 23 0.990 0.000 C23 N22 C23_$2 H27A 0.0646 0.3498 0.8824 137 0.980 0.000 C27 N22 H27A H27B -0.0989 0.2695 0.9176 137 0.980 0.000 C27 N22 H27A H27C 0.1235 0.3023 1.0259 137 0.980 0.000 C27 N22 H27A H22 -0.2786 0.4044 0.9368 13 0.930 0.000 N22 C27 C21 C23 07skc0020p21c in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.47745 0.41899 0.70619 1.00000 0.02504 0.02619 0.03164 -0.00018 0.00802 -0.00434 0.02727 0.00790 0.00072 0.00030 0.00042 0.00000 0.00224 0.00250 0.00234 0.00204 0.00179 0.00191 0.00097 C2 0.25436 0.41654 0.60458 1.00000 0.01890 0.03042 0.03155 -0.00293 0.00677 -0.00098 0.02669 0.00756 0.00069 0.00030 0.00041 0.00000 0.00207 0.00251 0.00226 0.00205 0.00172 0.00185 0.00096 H2 0.11654 0.43420 0.63679 1.00000 0.03203 0.00000 0.00000 C3 0.21706 0.39354 0.47567 1.00000 0.01933 0.03130 0.02742 0.00264 0.00268 0.00717 0.02624 0.00798 0.00070 0.00030 0.00041 0.00000 0.00209 0.00256 0.00219 0.00198 0.00170 0.00183 0.00097 H3 0.05712 0.39845 0.43095 1.00000 0.03148 0.00000 0.00000 C4 0.38364 0.36146 0.38984 1.00000 0.02721 0.02219 0.02208 0.00169 0.00245 -0.00138 0.02411 0.00761 0.00071 0.00029 0.00040 0.00000 0.00232 0.00231 0.00205 0.00188 0.00169 0.00183 0.00092 O1A 0.45670 0.43080 0.82502 1.00000 0.02784 0.04013 0.02273 -0.00491 0.00578 0.00357 0.03010 0.00539 0.00049 0.00022 0.00027 0.00000 0.00163 0.00200 0.00154 0.00144 0.00122 0.00139 0.00075 O1B 0.67740 0.40903 0.67100 1.00000 0.02006 0.04844 0.02659 -0.00497 0.00489 -0.00173 0.03163 0.00535 0.00047 0.00022 0.00028 0.00000 0.00153 0.00222 0.00155 0.00148 0.00121 0.00139 0.00079 O4A 0.61258 0.36496 0.43521 1.00000 0.02361 0.04387 0.02622 -0.00310 0.00694 0.00154 0.03094 0.00567 0.00047 0.00023 0.00030 0.00000 0.00162 0.00212 0.00166 0.00158 0.00123 0.00139 0.00077 H4 0.63784 0.38194 0.51531 1.00000 0.05011 0.00000 0.01652 O4B 0.30373 0.33253 0.27845 1.00000 0.03355 0.04730 0.02582 -0.00877 0.00461 -0.00572 0.03568 0.00550 0.00052 0.00023 0.00029 0.00000 0.00177 0.00220 0.00164 0.00155 0.00134 0.00154 0.00083 C21 -0.26647 0.34643 1.11426 1.00000 0.03050 0.03263 0.02632 0.00188 0.00810 -0.00451 0.02946 0.00820 0.00075 0.00031 0.00041 0.00000 0.00239 0.00276 0.00221 0.00205 0.00189 0.00208 0.00104 H21A -0.35497 0.29247 1.07931 1.00000 0.03752 0.00000 0.01327 H21B -0.37418 0.38969 1.14416 1.00000 0.02651 0.00000 0.01164 H21C -0.14184 0.32983 1.18983 1.00000 0.02484 0.00000 0.01127 C23 -0.02682 0.47220 1.05850 1.00000 0.02673 0.02621 0.01823 -0.00299 0.00482 0.00082 0.02365 0.00760 0.00072 0.00028 0.00039 0.00000 0.00226 0.00245 0.00202 0.00182 0.00174 0.00189 0.00094 H23A 0.12275 0.45615 1.11920 1.00000 0.03363 0.00000 0.01240 H23B -0.12438 0.50800 1.10976 1.00000 0.02594 0.00000 0.01152 C27 -0.00389 0.32177 0.95360 1.00000 0.03306 0.02515 0.03454 -0.00217 0.00862 0.00234 0.03062 0.00837 0.00076 0.00030 0.00045 0.00000 0.00250 0.00255 0.00247 0.00206 0.00199 0.00198 0.00105 H27A 0.06458 0.34979 0.88245 1.00000 0.04593 0.00000 0.00000 H27B -0.09886 0.26951 0.91763 1.00000 0.04593 0.00000 0.00000 H27C 0.12346 0.30232 1.02592 1.00000 0.04593 0.00000 0.00000 N22 -0.15708 0.38814 1.00649 1.00000 0.02405 0.02423 0.02349 -0.00247 0.00371 -0.00244 0.02402 0.00618 0.00058 0.00024 0.00033 0.00000 0.00184 0.00202 0.00177 0.00155 0.00150 0.00150 0.00081 H22 -0.27861 0.40440 0.93680 1.00000 0.06486 0.00000 0.01804 Final Structure Factor Calculation for 07skc0020p21c in P2(1)/c Total number of l.s. parameters = 119 Maximum vector length = 511 Memory required = 1635 / 22995 wR2 = 0.1836 before cycle 5 for 1949 data and 0 / 119 parameters GooF = S = 1.159; Restrained GooF = 1.159 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 2.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1029 for 1190 Fo > 4sig(Fo) and 0.1739 for all 1949 data wR2 = 0.1836, GooF = S = 1.159, Restrained GooF = 1.159 for all data Occupancy sum of asymmetric unit = 12.00 for non-hydrogen and 12.00 for hydrogen atoms Principal mean square atomic displacements U 0.0326 0.0289 0.0203 C1 0.0340 0.0280 0.0180 C2 0.0348 0.0282 0.0158 C3 0.0292 0.0227 0.0204 C4 0.0425 0.0274 0.0203 O1A 0.0495 0.0255 0.0198 O1B 0.0445 0.0270 0.0213 O4A 0.0513 0.0333 0.0225 O4B 0.0362 0.0298 0.0223 C21 0.0279 0.0261 0.0169 C23 0.0359 0.0325 0.0235 C27 0.0269 0.0247 0.0204 N22 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.007 0.014 0.021 0.029 0.039 0.050 0.063 0.088 0.128 1.000 Number in group 208. 183. 206. 198. 198. 180. 190. 204. 186. 196. GooF 1.254 1.243 1.210 1.282 1.208 1.207 1.096 1.102 0.961 0.959 K 28.095 4.583 1.970 1.560 1.145 1.098 1.040 1.021 0.991 0.997 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.14 1.32 1.66 inf Number in group 202. 190. 196. 201. 186. 195. 195. 194. 194. 196. GooF 1.208 1.180 1.263 1.254 1.272 1.219 1.060 1.053 0.940 1.089 K 1.423 1.155 1.233 1.270 1.067 1.025 1.018 0.991 1.020 0.997 R1 0.435 0.349 0.316 0.310 0.247 0.194 0.120 0.105 0.065 0.037 Recommended weighting scheme: WGHT 0.0000 2.5867 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 0 2 1420.75 1736.40 3.71 0.307 5.00 5 10 3 164.72 50.36 3.52 0.052 0.84 -1 14 1 13.60 82.50 3.34 0.067 1.04 -2 11 3 46.96 0.37 3.29 0.004 1.18 0 3 10 44.97 5.87 3.16 0.018 0.98 -1 17 6 57.38 6.58 3.02 0.019 0.78 2 5 6 24.44 2.53 2.96 0.012 1.21 2 8 6 34.04 0.08 2.92 0.002 1.08 -4 7 4 22.28 0.81 2.87 0.007 1.13 4 13 1 54.14 13.67 2.85 0.027 0.88 3 6 10 83.64 7.27 2.84 0.020 0.78 0 15 5 217.02 127.85 2.83 0.083 0.89 -2 9 9 57.80 9.67 2.83 0.023 0.92 5 10 0 47.99 1.14 2.82 0.008 0.90 -2 8 11 116.57 46.52 2.78 0.050 0.82 -6 1 8 -8.61 22.94 2.76 0.035 0.83 -2 1 4 20.63 2.32 2.71 0.011 2.06 -7 2 2 -21.66 31.31 2.69 0.041 0.82 1 17 1 65.81 10.05 2.66 0.023 0.86 3 12 6 80.24 6.80 2.65 0.019 0.84 4 7 8 198.26 9.44 2.64 0.023 0.80 -4 5 1 22.87 4.60 2.61 0.016 1.29 6 2 3 62.01 1.28 2.58 0.008 0.86 0 14 6 74.38 25.91 2.58 0.038 0.90 -4 11 9 138.06 71.38 2.56 0.062 0.79 -5 4 5 37.16 3.03 2.56 0.013 1.03 -2 5 1 48.13 19.82 2.53 0.033 2.06 1 17 3 56.80 8.05 2.52 0.021 0.83 -2 8 10 62.35 20.22 2.50 0.033 0.88 -1 2 3 348.76 443.17 2.47 0.155 2.89 3 16 1 76.26 20.96 2.44 0.034 0.82 -4 6 11 28.93 0.38 2.39 0.005 0.80 -5 4 8 23.26 0.68 2.38 0.006 0.90 -1 6 8 97.93 50.43 2.37 0.052 1.13 2 13 3 49.59 11.43 2.36 0.025 0.99 5 3 5 140.41 10.82 2.36 0.024 0.90 -1 2 11 28.20 2.98 2.34 0.013 0.92 -3 4 11 29.48 70.55 2.34 0.062 0.86 1 15 6 33.73 0.52 2.34 0.005 0.83 -1 14 5 43.23 10.77 2.34 0.024 0.94 -3 12 2 32.33 0.06 2.34 0.002 1.03 6 6 3 80.72 3.59 2.32 0.014 0.82 1 1 1 2137.26 2358.22 2.30 0.358 4.37 -2 13 6 32.63 0.64 2.30 0.006 0.92 0 7 1 31.73 10.51 2.30 0.024 2.08 3 9 6 -13.37 12.51 2.29 0.026 0.94 1 12 4 87.28 149.14 2.29 0.090 1.07 -4 5 9 173.89 116.75 2.28 0.080 0.92 1 2 2 289.80 222.03 2.28 0.110 3.12 -3 8 7 2.72 32.16 2.27 0.042 1.04 Bond lengths and angles C1 - Distance Angles O1A 1.2503 (0.0047) O1B 1.2761 (0.0047) 122.86 (0.38) C2 1.4906 (0.0057) 116.70 (0.36) 120.44 (0.36) C1 - O1A O1B C2 - Distance Angles C3 1.3342 (0.0056) C1 1.4906 (0.0057) 130.39 (0.39) H2 0.9500 114.80 114.80 C2 - C3 C1 C3 - Distance Angles C2 1.3342 (0.0056) C4 1.4912 (0.0055) 130.99 (0.38) H3 0.9500 114.50 114.50 C3 - C2 C4 C4 - Distance Angles O4B 1.2194 (0.0048) O4A 1.3127 (0.0047) 121.33 (0.38) C3 1.4912 (0.0055) 119.08 (0.37) 119.59 (0.36) C4 - O4B O4A O1A - Distance Angles C1 1.2503 (0.0047) O1A - O1B - Distance Angles C1 1.2761 (0.0047) O1B - O4A - Distance Angles C4 1.3127 (0.0047) H4 0.8400 109.47 O4A - C4 O4B - Distance Angles C4 1.2194 (0.0048) O4B - C21 - Distance Angles N22 1.4978 (0.0050) H21A 0.9800 109.47 H21B 0.9800 109.47 109.47 H21C 0.9800 109.47 109.47 109.47 C21 - N22 H21A H21B C23 - Distance Angles N22 1.5009 (0.0052) C23_$2 1.5280 (0.0077) 109.57 (0.40) H23A 0.9900 109.76 109.76 H23B 0.9900 109.76 109.76 108.22 C23 - N22 C23_$2 H23A C27 - Distance Angles N22 1.4889 (0.0052) H27A 0.9800 109.47 H27B 0.9800 109.47 109.47 H27C 0.9800 109.47 109.47 109.47 C27 - N22 H27A H27B N22 - Distance Angles C27 1.4889 (0.0052) C21 1.4978 (0.0050) 110.46 (0.34) C23 1.5009 (0.0052) 112.85 (0.32) 109.65 (0.30) H22 0.9300 107.91 107.91 107.91 N22 - C27 C21 C23 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.61 2.449(4) 176.4 O4A-H4...O1B 0.93 1.77 2.686(4) 169.6 N22-H22...O1A_$1 FMAP and GRID set by program FMAP 2 1 16 GRID -3.846 24 -2 3.846 1 2 R1 = 0.1739 for 1949 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.30 at 0.1650 0.3201 0.6524 [ 1.63 A from C2 ] Deepest hole -0.31 at 0.0319 0.2727 0.8637 [ 1.01 A from H27B ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 1980 / 21235 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1650 0.3201 0.6524 1.00000 0.05 0.30 1.63 C2 1.72 H2 2.17 C3 2.22 H27C Q2 1 0.7669 0.4177 0.6249 1.00000 0.05 0.28 0.77 O1B 1.33 H4 1.99 C1 2.01 H2 Q3 1 0.5060 0.4672 0.5264 1.00000 0.05 0.28 1.49 H4 1.83 O1B 1.93 C2 1.94 O4A Q4 1 0.3573 0.3810 0.6579 1.00000 0.05 0.27 0.90 C2 0.95 C1 1.57 H2 1.85 O1A Q5 1 0.0385 0.4131 1.1988 1.00000 0.05 0.26 1.20 H23A 1.61 H21C 1.66 C23 1.84 H23B Q6 1 0.6294 0.4531 0.8434 1.00000 0.05 0.26 1.03 O1A 1.23 H22 1.59 C1 1.94 O1B Q7 1 0.4509 0.2979 0.7579 1.00000 0.05 0.25 1.89 C1 2.09 O1A 2.14 O4B 2.37 O1B Q8 1 0.6295 0.2789 0.3824 1.00000 0.05 0.25 1.40 O4A 1.70 H27B 1.88 C4 2.04 H4 Q9 1 0.0832 0.3384 0.7385 1.00000 0.05 0.25 1.50 H27A 1.79 H2 2.16 C2 2.35 C27 Q10 1 0.8074 0.3827 0.7423 1.00000 0.05 0.24 1.02 O1B 1.92 H27A 1.94 C1 2.15 H22 Shortest distances between peaks (including symmetry equivalents) 1 9 1.10 3 3 1.11 2 10 1.28 1 4 1.42 4 7 1.63 9 10 1.72 2 3 1.80 1 7 1.82 7 8 1.86 6 10 1.90 4 9 2.01 3 4 2.14 7 9 2.17 2 9 2.29 7 10 2.44 4 6 2.46 2 4 2.50 2 6 2.55 4 10 2.57 1 10 2.58 6 7 2.61 2 3 2.62 1 2 2.68 3 10 2.83 5 6 2.84 Time profile in seconds ----------------------- 0.05: 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 0.02: Analyse other restraints etc. 0.39: 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 0.27: Structure factors and derivatives 0.22: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.00: Solve l.s. equations 0.00: Generate HTAB table 0.06: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 07skc0020p21c finished at 12:17:36 Total CPU time: 1.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++