+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009skc0163 started at 14:02:20 on 17-Feb-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009skc0163 in P-1 CELL 0.71073 9.4410 10.7119 13.1912 73.838 86.183 70.395 ZERR 4.00 0.0003 0.0003 0.0004 0.002 0.002 0.002 LATT 1 SFAC C H O UNIT 44 96 8 V = 1206.51 F(000) = 424.0 Mu = 0.07 mm-1 Cell Wt = 753.21 Rho = 1.037 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 FMAP 2 PLAN 10 OMIT -1 1 1 SIZE 0.16 0.20 0.32 ACTA HTAB O2 O22 EQIV_$1 -x+2, -y, -z HTAB O1 O2_$1 EQIV_$2 x-1, y+1, z HTAB O21 O1_$2 EQIV_$3 -x+1, -y+1, -z HTAB O22 O21_$3 BOND $H WGHT 0.05520 0.32960 L.S. 8 TEMP -153.00 FVAR 1.00384 MOLE 1 C1 1 0.851829 -0.192620 0.136134 11.00000 0.02160 0.01874 = 0.02451 -0.00526 0.00264 -0.00197 C2 1 0.809656 -0.070134 0.037661 11.00000 0.02920 0.02102 = 0.03068 -0.00344 0.00676 -0.00102 AFIX 23 H2A 2 0.879028 -0.093031 -0.019160 11.00000 -1.20000 H2B 2 0.706614 -0.054398 0.013231 11.00000 -1.20000 AFIX 0 C3 1 1.005628 -0.208446 0.180558 11.00000 0.02156 0.02382 = 0.03798 -0.00973 0.00731 -0.00499 AFIX 23 H3A 2 1.000420 -0.120252 0.193370 11.00000 -1.20000 H3B 2 1.026260 -0.279384 0.249401 11.00000 -1.20000 AFIX 0 C4 1 0.861478 -0.320689 0.100824 11.00000 0.02677 0.02252 = 0.02090 -0.00768 0.00189 -0.00259 AFIX 23 H4A 2 0.764811 -0.302337 0.065005 11.00000 -1.20000 H4B 2 0.940647 -0.332373 0.047789 11.00000 -1.20000 AFIX 0 C5 1 0.894923 -0.456811 0.187037 11.00000 0.02488 0.02442 = 0.02104 -0.00682 0.00165 -0.00609 AFIX 23 H5A 2 0.972599 -0.463353 0.236937 11.00000 -1.20000 H5B 2 0.802579 -0.458179 0.226905 11.00000 -1.20000 AFIX 0 C6 1 0.949550 -0.580838 0.142337 11.00000 0.02774 0.02333 = 0.02717 -0.00811 0.00239 -0.00501 AFIX 23 H6A 2 1.033487 -0.572284 0.094805 11.00000 -1.20000 H6B 2 0.866805 -0.579621 0.099345 11.00000 -1.20000 AFIX 0 C7 1 1.002532 -0.718803 0.225815 11.00000 0.02724 0.02295 = 0.04097 -0.00509 -0.00076 -0.00693 AFIX 33 H7A 2 1.035849 -0.793437 0.191288 11.00000 -1.50000 H7B 2 0.919468 -0.729560 0.272217 11.00000 -1.50000 H7C 2 1.086382 -0.722214 0.267670 11.00000 -1.50000 AFIX 0 C8 1 0.738724 -0.170384 0.224605 11.00000 0.02122 0.02257 = 0.02538 -0.00934 0.00266 -0.00460 AFIX 23 H8A 2 0.771726 -0.252682 0.285881 11.00000 -1.20000 H8B 2 0.743793 -0.091161 0.247118 11.00000 -1.20000 AFIX 0 C9 1 0.574738 -0.144174 0.197622 11.00000 0.02205 0.02584 = 0.02878 -0.00977 0.00297 -0.00552 AFIX 23 H9A 2 0.570147 -0.211456 0.160570 11.00000 -1.20000 H9B 2 0.532693 -0.050843 0.148898 11.00000 -1.20000 AFIX 0 C10 1 0.478441 -0.155781 0.295182 11.00000 0.02535 0.03087 = 0.03661 -0.01221 0.00756 -0.01070 AFIX 23 H10A 2 0.513694 -0.251972 0.340136 11.00000 -1.20000 H10B 2 0.492087 -0.096114 0.336467 11.00000 -1.20000 AFIX 0 C11 1 0.312165 -0.114757 0.268157 11.00000 0.02449 0.04348 = 0.05401 -0.01481 0.00914 -0.01161 AFIX 33 H11A 2 0.255758 -0.123606 0.333386 11.00000 -1.50000 H11B 2 0.297457 -0.175147 0.229000 11.00000 -1.50000 H11C 2 0.276038 -0.019059 0.224657 11.00000 -1.50000 AFIX 0 C21 1 0.470531 0.355930 0.224683 11.00000 0.01946 0.01834 = 0.02103 -0.00499 0.00252 -0.00307 C22 1 0.495830 0.487342 0.155261 11.00000 0.02289 0.01985 = 0.02501 -0.00233 0.00487 -0.00106 AFIX 23 H22A 2 0.501543 0.544983 0.200896 11.00000 -1.20000 H22B 2 0.593712 0.461484 0.120770 11.00000 -1.20000 AFIX 0 C23 1 0.433779 0.277405 0.154634 11.00000 0.02328 0.02544 = 0.02261 -0.00921 0.00277 -0.00235 AFIX 23 H23A 2 0.416040 0.193964 0.200629 11.00000 -1.20000 H23B 2 0.339124 0.336186 0.114050 11.00000 -1.20000 AFIX 0 C24 1 0.618736 0.270113 0.288329 11.00000 0.01901 0.02051 = 0.02430 -0.00446 0.00062 -0.00463 AFIX 23 H24A 2 0.697501 0.241653 0.238075 11.00000 -1.20000 H24B 2 0.648243 0.330894 0.320937 11.00000 -1.20000 AFIX 0 C25 1 0.619458 0.141424 0.375231 11.00000 0.02487 0.02147 = 0.02711 -0.00351 0.00017 -0.00604 AFIX 23 H25A 2 0.553504 0.169128 0.432283 11.00000 -1.20000 H25B 2 0.578019 0.084713 0.346043 11.00000 -1.20000 AFIX 0 C26 1 0.777332 0.055201 0.421348 11.00000 0.02812 0.02508 = 0.02982 -0.00274 -0.00303 -0.00471 AFIX 23 H26A 2 0.844484 0.032209 0.363511 11.00000 -1.20000 H26B 2 0.816391 0.110491 0.453883 11.00000 -1.20000 AFIX 0 C27 1 0.781236 -0.077763 0.504092 11.00000 0.04118 0.02828 = 0.03254 0.00087 -0.00622 -0.00326 AFIX 33 H27A 2 0.884696 -0.129091 0.531130 11.00000 -1.50000 H27B 2 0.744860 -0.133980 0.471965 11.00000 -1.50000 H27C 2 0.716660 -0.055657 0.562351 11.00000 -1.50000 AFIX 0 C28 1 0.334276 0.390725 0.295411 11.00000 0.01843 0.02264 = 0.02238 -0.00582 0.00190 -0.00570 AFIX 23 H28A 2 0.244007 0.445794 0.249003 11.00000 -1.20000 H28B 2 0.318985 0.303400 0.335434 11.00000 -1.20000 AFIX 0 C29 1 0.342862 0.469098 0.374200 11.00000 0.02760 0.02759 = 0.02903 -0.01260 0.00740 -0.01075 AFIX 23 H29A 2 0.436912 0.418986 0.417524 11.00000 -1.20000 H29B 2 0.346871 0.561141 0.334912 11.00000 -1.20000 AFIX 0 C30 1 0.209690 0.486553 0.446839 11.00000 0.02838 0.02729 = 0.02200 -0.00811 0.00545 -0.00722 AFIX 23 H30A 2 0.115405 0.529267 0.403294 11.00000 -1.20000 H30B 2 0.210870 0.394549 0.490436 11.00000 -1.20000 AFIX 0 C31 1 0.210138 0.574369 0.519093 11.00000 0.05693 0.04496 = 0.03759 -0.02325 0.01922 -0.02107 AFIX 33 H31A 2 0.121865 0.582271 0.563520 11.00000 -1.50000 H31B 2 0.207040 0.666269 0.476521 11.00000 -1.50000 H31C 2 0.301799 0.531367 0.563971 11.00000 -1.50000 AFIX 0 O1 3 1.127142 -0.245981 0.113105 11.00000 0.02319 0.02684 = 0.05264 -0.00785 0.01475 -0.00217 AFIX 147 H1 2 1.126108 -0.176546 0.063577 11.00000 -1.50000 AFIX 0 O2 3 0.815547 0.054581 0.054970 11.00000 0.03218 0.01928 = 0.05849 -0.00577 0.00911 -0.00138 AFIX 147 H2 2 0.732803 0.095867 0.077605 11.00000 -1.50000 AFIX 0 O21 3 0.380636 0.567190 0.075663 11.00000 0.03086 0.02623 = 0.02711 0.00126 0.00490 0.00706 AFIX 147 H21 2 0.305309 0.613192 0.102779 11.00000 -1.50000 AFIX 0 O22 3 0.548111 0.236737 0.082109 11.00000 0.03538 0.02566 = 0.02812 -0.01043 0.01141 -0.00366 AFIX 147 H22 2 0.560317 0.307127 0.040155 11.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 2009skc0163 in P-1 C 0.770 H 0.320 O 0.660 C1 - C2 C3 C4 C8 C2 - O2 C1 C3 - O1 C1 C4 - C5 C1 C5 - C6 C4 C6 - C5 C7 C7 - C6 C8 - C9 C1 C9 - C8 C10 C10 - C11 C9 C11 - C10 C21 - C23 C22 C24 C28 C22 - O21 C21 C23 - O22 C21 C24 - C25 C21 C25 - C26 C24 C26 - C27 C25 C27 - C26 C28 - C29 C21 C29 - C30 C28 C30 - C31 C29 C31 - C30 O1 - C3 O2 - C2 O21 - C22 O22 - C23 Operators for generating equivalent atoms: $1 -x+2, -y, -z $2 x-1, y+1, z $3 -x+1, -y+1, -z 25792 Reflections read, of which 25 rejected -12 =< h =< 12, -13 =< k =< 13, -17 =< l =< 17, Max. 2-theta = 54.96 0 Systematic absence violations 0 Inconsistent equivalents 5523 Unique reflections, of which 0 suppressed R(int) = 0.0582 R(sigma) = 0.0536 Friedel opposites merged Maximum memory for data reduction = 3556 / 56124 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 = 4392 / 295389 wR2 = 0.1346 before cycle 1 for 5523 data and 239 / 239 parameters GooF = S = 1.029; Restrained GooF = 1.029 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0552 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.00449 0.00181 0.358 OSF Mean shift/su = 0.043 Maximum = 0.358 for OSF Max. shift = 0.001 A for H22 Max. dU = 0.000 for O21 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4392 / 295389 wR2 = 0.1346 before cycle 2 for 5523 data and 239 / 239 parameters GooF = S = 1.029; Restrained GooF = 1.029 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0552 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.00462 0.00181 0.070 OSF Mean shift/su = 0.015 Maximum = 0.070 for OSF Max. shift = 0.001 A for H22 Max. dU = 0.000 for O21 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4392 / 295389 wR2 = 0.1346 before cycle 3 for 5523 data and 239 / 239 parameters GooF = S = 1.029; Restrained GooF = 1.029 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0552 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.00462 0.00181 0.004 OSF Mean shift/su = 0.001 Maximum = -0.009 for tors H22 Max. shift = 0.000 A for H22 Max. dU = 0.000 for C31 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4392 / 295389 wR2 = 0.1346 before cycle 4 for 5523 data and 239 / 239 parameters GooF = S = 1.029; Restrained GooF = 1.029 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0552 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.00463 0.00181 0.000 OSF Mean shift/su = 0.000 Maximum = -0.002 for tors H22 Max. shift = 0.000 A for H22 Max. dU = 0.000 for C31 Least-squares cycle 5 Maximum vector length = 511 Memory required = 4392 / 295389 wR2 = 0.1346 before cycle 5 for 5523 data and 239 / 239 parameters GooF = S = 1.029; Restrained GooF = 1.029 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0552 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.00463 0.00181 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for tors H1 Max. shift = 0.000 A for H1 Max. dU = 0.000 for C11 Least-squares cycle 6 Maximum vector length = 511 Memory required = 4392 / 295389 wR2 = 0.1346 before cycle 6 for 5523 data and 239 / 239 parameters GooF = S = 1.029; Restrained GooF = 1.029 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0552 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.00463 0.00181 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x C7 Max. shift = 0.000 A for H1 Max. dU = 0.000 for C11 Least-squares cycle 7 Maximum vector length = 511 Memory required = 4392 / 295389 wR2 = 0.1346 before cycle 7 for 5523 data and 239 / 239 parameters GooF = S = 1.029; Restrained GooF = 1.029 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0552 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.00463 0.00181 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x C7 Max. shift = 0.000 A for H1 Max. dU = 0.000 for C11 Least-squares cycle 8 Maximum vector length = 511 Memory required = 4392 / 295389 wR2 = 0.1346 before cycle 8 for 5523 data and 239 / 239 parameters GooF = S = 1.029; Restrained GooF = 1.029 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0552 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.00463 0.00181 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x C7 Max. shift = 0.000 A for H1 Max. dU = 0.000 for C10 Largest correlation matrix elements -0.510 U23 C31 / U33 C31 Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2A 0.8791 -0.0931 -0.0192 23 0.990 0.000 C2 O2 C1 H2B 0.7066 -0.0544 0.0132 23 0.990 0.000 C2 O2 C1 H3A 1.0004 -0.1202 0.1934 23 0.990 0.000 C3 O1 C1 H3B 1.0262 -0.2794 0.2494 23 0.990 0.000 C3 O1 C1 H4A 0.7648 -0.3023 0.0650 23 0.990 0.000 C4 C5 C1 H4B 0.9406 -0.3324 0.0478 23 0.990 0.000 C4 C5 C1 H5A 0.9726 -0.4633 0.2369 23 0.990 0.000 C5 C6 C4 H5B 0.8026 -0.4582 0.2269 23 0.990 0.000 C5 C6 C4 H6A 1.0335 -0.5723 0.0948 23 0.990 0.000 C6 C5 C7 H6B 0.8668 -0.5796 0.0994 23 0.990 0.000 C6 C5 C7 H7A 1.0358 -0.7934 0.1913 33 0.980 0.000 C7 C6 H7A H7B 0.9195 -0.7296 0.2722 33 0.980 0.000 C7 C6 H7A H7C 1.0864 -0.7222 0.2677 33 0.980 0.000 C7 C6 H7A H8A 0.7718 -0.2527 0.2859 23 0.990 0.000 C8 C9 C1 H8B 0.7438 -0.0912 0.2471 23 0.990 0.000 C8 C9 C1 H9A 0.5701 -0.2115 0.1606 23 0.990 0.000 C9 C8 C10 H9B 0.5327 -0.0509 0.1489 23 0.990 0.000 C9 C8 C10 H10A 0.5137 -0.2519 0.3401 23 0.990 0.000 C10 C11 C9 H10B 0.4921 -0.0961 0.3365 23 0.990 0.000 C10 C11 C9 H11A 0.2557 -0.1236 0.3334 33 0.980 0.000 C11 C10 H11A H11B 0.2974 -0.1751 0.2290 33 0.980 0.000 C11 C10 H11A H11C 0.2760 -0.0190 0.2247 33 0.980 0.000 C11 C10 H11A H22A 0.5016 0.5450 0.2009 23 0.990 0.000 C22 O21 C21 H22B 0.5937 0.4615 0.1208 23 0.990 0.000 C22 O21 C21 H23A 0.4160 0.1940 0.2006 23 0.990 0.000 C23 O22 C21 H23B 0.3391 0.3362 0.1141 23 0.990 0.000 C23 O22 C21 H24A 0.6975 0.2417 0.2381 23 0.990 0.000 C24 C25 C21 H24B 0.6482 0.3309 0.3209 23 0.990 0.000 C24 C25 C21 H25A 0.5535 0.1691 0.4323 23 0.990 0.000 C25 C26 C24 H25B 0.5780 0.0847 0.3460 23 0.990 0.000 C25 C26 C24 H26A 0.8445 0.0322 0.3635 23 0.990 0.000 C26 C27 C25 H26B 0.8163 0.1105 0.4539 23 0.990 0.000 C26 C27 C25 H27A 0.8847 -0.1291 0.5311 33 0.980 0.000 C27 C26 H27A H27B 0.7448 -0.1340 0.4720 33 0.980 0.000 C27 C26 H27A H27C 0.7166 -0.0556 0.5624 33 0.980 0.000 C27 C26 H27A H28A 0.2440 0.4458 0.2490 23 0.990 0.000 C28 C29 C21 H28B 0.3190 0.3034 0.3354 23 0.990 0.000 C28 C29 C21 H29A 0.4369 0.4190 0.4175 23 0.990 0.000 C29 C30 C28 H29B 0.3469 0.5611 0.3349 23 0.990 0.000 C29 C30 C28 H30A 0.1154 0.5293 0.4033 23 0.990 0.000 C30 C31 C29 H30B 0.2108 0.3946 0.4904 23 0.990 0.000 C30 C31 C29 H31A 0.1218 0.5823 0.5635 33 0.980 0.000 C31 C30 H31A H31B 0.2070 0.6663 0.4765 33 0.980 0.000 C31 C30 H31A H31C 0.3018 0.5314 0.5640 33 0.980 0.000 C31 C30 H31A H1 1.1260 -0.1765 0.0635 147 0.840 0.000 O1 C3 H1 H2 0.7328 0.0958 0.0776 147 0.840 0.000 O2 C2 H2 H21 0.3053 0.6132 0.1028 147 0.840 0.000 O21 C22 H21 H22 0.5601 0.3072 0.0400 147 0.840 0.000 O22 C23 H22 2009skc0163 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.85184 -0.19263 0.13613 1.00000 0.02160 0.01878 0.02454 -0.00529 0.00266 -0.00197 0.02310 0.00226 0.00016 0.00014 0.00012 0.00000 0.00072 0.00071 0.00078 0.00060 0.00059 0.00059 0.00033 C2 0.80969 -0.07015 0.03766 1.00000 0.02920 0.02107 0.03075 -0.00348 0.00679 -0.00103 0.02997 0.00259 0.00018 0.00015 0.00013 0.00000 0.00082 0.00076 0.00089 0.00066 0.00068 0.00065 0.00037 H2A 0.87907 -0.09306 -0.01916 1.00000 0.03596 0.00000 0.00000 H2B 0.70665 -0.05442 0.01322 1.00000 0.03596 0.00000 0.00000 C3 1.00561 -0.20844 0.18055 1.00000 0.02158 0.02384 0.03800 -0.00974 0.00732 -0.00498 0.02850 0.00245 0.00017 0.00016 0.00013 0.00000 0.00075 0.00077 0.00094 0.00069 0.00066 0.00062 0.00036 H3A 1.00039 -0.12025 0.19337 1.00000 0.03420 0.00000 0.00000 H3B 1.02624 -0.27938 0.24940 1.00000 0.03420 0.00000 0.00000 C4 0.86146 -0.32068 0.10083 1.00000 0.02678 0.02258 0.02093 -0.00770 0.00192 -0.00259 0.02457 0.00230 0.00017 0.00015 0.00012 0.00000 0.00077 0.00074 0.00077 0.00062 0.00060 0.00062 0.00033 H4A 0.76479 -0.30232 0.06501 1.00000 0.02948 0.00000 0.00000 H4B 0.94063 -0.33237 0.04779 1.00000 0.02948 0.00000 0.00000 C5 0.89490 -0.45680 0.18704 1.00000 0.02488 0.02446 0.02110 -0.00685 0.00166 -0.00608 0.02394 0.00227 0.00017 0.00015 0.00012 0.00000 0.00075 0.00076 0.00077 0.00061 0.00059 0.00062 0.00033 H5A 0.97258 -0.46334 0.23694 1.00000 0.02873 0.00000 0.00000 H5B 0.80256 -0.45816 0.22691 1.00000 0.02873 0.00000 0.00000 C6 0.94953 -0.58083 0.14234 1.00000 0.02777 0.02338 0.02721 -0.00813 0.00236 -0.00503 0.02683 0.00240 0.00018 0.00015 0.00012 0.00000 0.00079 0.00076 0.00084 0.00065 0.00064 0.00064 0.00035 H6A 1.03345 -0.57227 0.09480 1.00000 0.03220 0.00000 0.00000 H6B 0.86678 -0.57961 0.09935 1.00000 0.03220 0.00000 0.00000 C7 1.00253 -0.71880 0.22582 1.00000 0.02731 0.02299 0.04100 -0.00509 -0.00078 -0.00697 0.03147 0.00255 0.00018 0.00016 0.00014 0.00000 0.00081 0.00078 0.00099 0.00071 0.00071 0.00066 0.00038 H7A 1.03584 -0.79343 0.19129 1.00000 0.04721 0.00000 0.00000 H7B 0.91947 -0.72956 0.27222 1.00000 0.04721 0.00000 0.00000 H7C 1.08638 -0.72221 0.26767 1.00000 0.04721 0.00000 0.00000 C8 0.73876 -0.17041 0.22460 1.00000 0.02125 0.02260 0.02543 -0.00934 0.00266 -0.00460 0.02329 0.00221 0.00016 0.00015 0.00012 0.00000 0.00072 0.00073 0.00080 0.00062 0.00059 0.00059 0.00033 H8A 0.77176 -0.25272 0.28587 1.00000 0.02794 0.00000 0.00000 H8B 0.74384 -0.09120 0.24712 1.00000 0.02794 0.00000 0.00000 C9 0.57474 -0.14418 0.19762 1.00000 0.02211 0.02586 0.02880 -0.00975 0.00295 -0.00555 0.02583 0.00229 0.00016 0.00016 0.00012 0.00000 0.00075 0.00077 0.00085 0.00066 0.00062 0.00062 0.00034 H9A 0.57014 -0.21147 0.16058 1.00000 0.03100 0.00000 0.00000 H9B 0.53271 -0.05086 0.14889 1.00000 0.03100 0.00000 0.00000 C10 0.47842 -0.15575 0.29518 1.00000 0.02541 0.03092 0.03662 -0.01222 0.00756 -0.01073 0.03030 0.00245 0.00017 0.00017 0.00013 0.00000 0.00080 0.00085 0.00095 0.00073 0.00069 0.00068 0.00037 H10A 0.51366 -0.25194 0.34015 1.00000 0.03635 0.00000 0.00000 H10B 0.49207 -0.09608 0.33646 1.00000 0.03635 0.00000 0.00000 C11 0.31212 -0.11472 0.26817 1.00000 0.02451 0.04354 0.05404 -0.01484 0.00917 -0.01161 0.04067 0.00282 0.00018 0.00019 0.00016 0.00000 0.00084 0.00104 0.00120 0.00091 0.00079 0.00077 0.00045 H11A 0.25572 -0.12357 0.33340 1.00000 0.06100 0.00000 0.00000 H11B 0.29740 -0.17510 0.22901 1.00000 0.06100 0.00000 0.00000 H11C 0.27599 -0.01902 0.22467 1.00000 0.06100 0.00000 0.00000 C21 0.47055 0.35592 0.22468 1.00000 0.01946 0.01836 0.02106 -0.00500 0.00251 -0.00305 0.02064 0.00215 0.00015 0.00014 0.00011 0.00000 0.00069 0.00069 0.00075 0.00058 0.00057 0.00057 0.00031 C22 0.49585 0.48732 0.15525 1.00000 0.02291 0.01991 0.02504 -0.00236 0.00489 -0.00106 0.02521 0.00242 0.00016 0.00015 0.00012 0.00000 0.00074 0.00072 0.00081 0.00061 0.00061 0.00060 0.00034 H22A 0.50158 0.54496 0.20088 1.00000 0.03025 0.00000 0.00000 H22B 0.59373 0.46146 0.12076 1.00000 0.03025 0.00000 0.00000 C23 0.43378 0.27741 0.15463 1.00000 0.02325 0.02546 0.02265 -0.00920 0.00278 -0.00232 0.02483 0.00226 0.00016 0.00016 0.00012 0.00000 0.00075 0.00076 0.00079 0.00063 0.00060 0.00062 0.00034 H23A 0.41604 0.19396 0.20063 1.00000 0.02980 0.00000 0.00000 H23B 0.33912 0.33619 0.11406 1.00000 0.02980 0.00000 0.00000 C24 0.61872 0.27013 0.28833 1.00000 0.01904 0.02055 0.02434 -0.00451 0.00064 -0.00464 0.02215 0.00222 0.00016 0.00015 0.00012 0.00000 0.00069 0.00071 0.00078 0.00060 0.00058 0.00058 0.00032 H24A 0.69750 0.24167 0.23808 1.00000 0.02658 0.00000 0.00000 H24B 0.64821 0.33091 0.32094 1.00000 0.02658 0.00000 0.00000 C25 0.61944 0.14144 0.37523 1.00000 0.02486 0.02150 0.02716 -0.00354 0.00017 -0.00601 0.02557 0.00236 0.00017 0.00015 0.00012 0.00000 0.00076 0.00074 0.00083 0.00063 0.00062 0.00062 0.00034 H25A 0.55348 0.16915 0.43228 1.00000 0.03068 0.00000 0.00000 H25B 0.57801 0.08472 0.34604 1.00000 0.03068 0.00000 0.00000 C26 0.77729 0.05523 0.42136 1.00000 0.02816 0.02512 0.02985 -0.00277 -0.00303 -0.00474 0.02959 0.00250 0.00018 0.00016 0.00013 0.00000 0.00081 0.00079 0.00088 0.00066 0.00066 0.00066 0.00036 H26A 0.84445 0.03223 0.36353 1.00000 0.03551 0.00000 0.00000 H26B 0.81634 0.11052 0.45390 1.00000 0.03551 0.00000 0.00000 C27 0.78119 -0.07774 0.50411 1.00000 0.04125 0.02833 0.03258 0.00087 -0.00624 -0.00331 0.03780 0.00281 0.00021 0.00017 0.00014 0.00000 0.00098 0.00088 0.00096 0.00074 0.00077 0.00076 0.00042 H27A 0.88465 -0.12907 0.53115 1.00000 0.05669 0.00000 0.00000 H27B 0.74482 -0.13395 0.47198 1.00000 0.05669 0.00000 0.00000 H27C 0.71662 -0.05563 0.56237 1.00000 0.05669 0.00000 0.00000 C28 0.33430 0.39071 0.29541 1.00000 0.01849 0.02267 0.02241 -0.00582 0.00188 -0.00573 0.02160 0.00217 0.00016 0.00015 0.00012 0.00000 0.00069 0.00072 0.00076 0.00060 0.00057 0.00058 0.00031 H28A 0.24403 0.44576 0.24900 1.00000 0.02592 0.00000 0.00000 H28B 0.31903 0.30338 0.33543 1.00000 0.02592 0.00000 0.00000 C29 0.34286 0.46909 0.37420 1.00000 0.02763 0.02763 0.02905 -0.01259 0.00736 -0.01078 0.02696 0.00228 0.00017 0.00016 0.00013 0.00000 0.00080 0.00080 0.00085 0.00067 0.00065 0.00066 0.00035 H29A 0.43690 0.41898 0.41754 1.00000 0.03235 0.00000 0.00000 H29B 0.34688 0.56113 0.33491 1.00000 0.03235 0.00000 0.00000 C30 0.20966 0.48658 0.44684 1.00000 0.02837 0.02732 0.02204 -0.00812 0.00543 -0.00721 0.02637 0.00235 0.00017 0.00016 0.00012 0.00000 0.00079 0.00079 0.00079 0.00064 0.00062 0.00065 0.00034 H30A 0.11538 0.52930 0.40329 1.00000 0.03164 0.00000 0.00000 H30B 0.21082 0.39459 0.49045 1.00000 0.03164 0.00000 0.00000 C31 0.21010 0.57440 0.51909 1.00000 0.05692 0.04497 0.03765 -0.02325 0.01922 -0.02103 0.04374 0.00287 0.00023 0.00020 0.00015 0.00000 0.00121 0.00107 0.00106 0.00088 0.00090 0.00094 0.00048 H31A 0.12183 0.58230 0.56351 1.00000 0.06560 0.00000 0.00000 H31B 0.20700 0.66630 0.47651 1.00000 0.06560 0.00000 0.00000 H31C 0.30176 0.53141 0.56396 1.00000 0.06560 0.00000 0.00000 O1 1.12712 -0.24596 0.11311 1.00000 0.02324 0.02688 0.05268 -0.00787 0.01477 -0.00217 0.03717 0.00198 0.00012 0.00011 0.00010 0.00000 0.00057 0.00059 0.00081 0.00055 0.00054 0.00048 0.00031 H1 1.12602 -0.17655 0.06353 1.00000 0.05576 0.00000 0.00000 O2 0.81557 0.05456 0.05496 1.00000 0.03221 0.01932 0.05854 -0.00579 0.00912 -0.00138 0.03997 0.00197 0.00013 0.00011 0.00011 0.00000 0.00065 0.00056 0.00085 0.00055 0.00059 0.00049 0.00033 H2 0.73283 0.09584 0.07761 1.00000 0.05995 0.00000 0.00000 O21 0.38066 0.56718 0.07566 1.00000 0.03091 0.02631 0.02715 0.00123 0.00494 0.00705 0.03447 0.00188 0.00013 0.00011 0.00009 0.00000 0.00061 0.00059 0.00061 0.00047 0.00048 0.00048 0.00030 H21 0.30533 0.61316 0.10278 1.00000 0.05170 0.00000 0.00000 O22 0.54809 0.23675 0.08211 1.00000 0.03543 0.02569 0.02814 -0.01042 0.01140 -0.00366 0.03130 0.00177 0.00013 0.00011 0.00009 0.00000 0.00063 0.00057 0.00063 0.00048 0.00049 0.00050 0.00028 H22 0.56010 0.30716 0.04004 1.00000 0.04695 0.00000 0.00000 Final Structure Factor Calculation for 2009skc0163 in P-1 Total number of l.s. parameters = 239 Maximum vector length = 511 Memory required = 4153 / 21973 wR2 = 0.1346 before cycle 9 for 5523 data and 0 / 239 parameters GooF = S = 1.029; Restrained GooF = 1.029 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0552 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0528 for 3893 Fo > 4sig(Fo) and 0.0835 for all 5523 data wR2 = 0.1346, GooF = S = 1.029, Restrained GooF = 1.029 for all data Occupancy sum of asymmetric unit = 26.00 for non-hydrogen and 48.00 for hydrogen atoms Principal mean square atomic displacements U 0.0302 0.0230 0.0161 C1 0.0464 0.0251 0.0185 C2 0.0412 0.0264 0.0179 C3 0.0337 0.0224 0.0177 C4 0.0281 0.0234 0.0203 C5 0.0320 0.0272 0.0213 C6 0.0432 0.0284 0.0228 C7 0.0266 0.0255 0.0178 C8 0.0296 0.0278 0.0201 C9 0.0395 0.0293 0.0221 C10 0.0562 0.0437 0.0220 C11 0.0260 0.0200 0.0160 C21 0.0383 0.0207 0.0166 C22 0.0332 0.0244 0.0169 C23 0.0263 0.0220 0.0182 C24 0.0303 0.0258 0.0206 C25 0.0347 0.0326 0.0214 C26 0.0495 0.0429 0.0210 C27 0.0245 0.0223 0.0180 C28 0.0351 0.0252 0.0205 C29 0.0331 0.0272 0.0188 C30 0.0671 0.0420 0.0221 C31 0.0651 0.0305 0.0158 O1 0.0679 0.0344 0.0176 O2 0.0630 0.0245 0.0159 O21 0.0487 0.0287 0.0165 O22 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.009 0.017 0.026 0.035 0.046 0.060 0.076 0.101 0.151 1.000 Number in group 622. 521. 573. 496. 563. 566. 534. 545. 550. 553. GooF 0.917 0.890 1.014 1.086 1.123 1.175 1.108 1.041 0.979 0.923 K 3.940 1.309 1.035 1.006 1.026 1.004 1.002 1.001 1.024 0.984 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.64 inf Number in group 576. 531. 551. 550. 560. 554. 557. 536. 552. 556. GooF 0.917 0.932 0.976 1.007 0.983 1.071 1.004 0.991 1.119 1.245 K 1.021 1.073 1.050 1.023 1.018 1.006 0.996 1.016 1.027 0.971 R1 0.210 0.180 0.165 0.145 0.103 0.083 0.056 0.045 0.046 0.036 Recommended weighting scheme: WGHT 0.0489 0.3719 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)/su Fc/Fc(max) Resolution(A) -5 2 8 19.29 37.65 4.49 0.060 1.16 -5 -1 5 11.92 3.57 4.41 0.018 1.48 -6 0 7 9.70 22.20 4.26 0.046 1.16 -1 -1 1 1728.28 2373.13 4.19 0.473 6.23 3 10 8 15.31 35.87 4.07 0.058 1.00 -4 0 7 24.46 11.82 3.89 0.033 1.42 4 4 1 42.16 26.11 3.84 0.050 2.04 2 2 7 21.43 9.63 3.82 0.030 1.79 0 -6 3 28.14 14.25 3.80 0.037 1.39 4 2 4 27.20 12.61 3.63 0.034 1.98 -7 1 7 60.57 40.19 3.63 0.062 1.04 2 9 9 24.68 43.52 3.61 0.064 1.04 -2 1 8 33.73 52.64 3.51 0.070 1.52 6 4 1 24.58 40.66 3.49 0.062 1.52 -1 -5 7 12.25 25.78 3.49 0.049 1.20 -6 2 8 37.92 57.84 3.48 0.074 1.06 3 -5 10 50.19 27.95 3.40 0.051 0.86 3 1 8 29.84 16.79 3.40 0.040 1.45 0 0 2 681.21 932.44 3.35 0.296 6.33 -11 -5 1 18.98 2.01 3.33 0.014 0.85 7 5 5 22.65 37.90 3.26 0.060 1.21 8 9 5 33.17 55.77 3.16 0.072 0.96 -3 3 3 49.38 33.92 3.15 0.057 1.86 3 8 9 88.47 63.75 3.14 0.077 1.11 0 3 5 8.75 3.48 3.12 0.018 2.33 -3 -9 4 36.03 20.10 3.10 0.044 0.99 4 4 5 4.57 0.41 3.09 0.006 1.75 5 7 8 174.35 133.81 3.08 0.112 1.16 6 3 2 47.54 33.16 3.07 0.056 1.55 1 -4 5 19.45 9.60 3.07 0.030 1.47 -6 2 9 179.77 139.04 3.07 0.114 1.01 0 9 8 7.86 18.47 3.06 0.042 1.03 -9 0 5 17.26 29.95 3.06 0.053 0.93 -6 1 9 38.94 55.49 2.97 0.072 1.03 0 2 6 87.59 66.44 2.96 0.079 2.16 4 4 2 172.64 138.44 2.96 0.114 2.03 -2 0 5 145.43 114.67 2.95 0.104 2.23 -1 3 7 22.29 13.48 2.92 0.036 1.72 5 -6 4 19.41 8.02 2.89 0.027 0.93 5 -2 2 47.56 33.91 2.89 0.057 1.44 2 5 2 73.50 55.43 2.88 0.072 2.12 3 3 5 125.03 159.68 2.87 0.123 2.05 -8 5 0 0.53 12.18 2.87 0.034 0.85 -6 0 1 24.18 14.98 2.85 0.038 1.48 6 1 0 19.05 11.06 2.84 0.032 1.54 2 -3 2 23.80 14.97 2.84 0.038 2.02 -4 1 7 80.93 61.68 2.82 0.076 1.41 -1 12 2 -3.00 8.31 2.76 0.028 0.80 6 5 10 143.06 107.56 2.75 0.101 1.04 -4 -7 5 28.92 41.90 2.74 0.063 1.11 Bond lengths and angles C1 - Distance Angles C2 1.5286 (0.0021) C3 1.5403 (0.0022) 108.97 (0.13) C4 1.5404 (0.0020) 106.72 (0.12) 110.35 (0.12) C8 1.5416 (0.0019) 111.90 (0.11) 106.51 (0.12) 112.39 (0.12) C1 - C2 C3 C4 C2 - Distance Angles O2 1.4357 (0.0020) C1 1.5286 (0.0021) 113.34 (0.14) H2A 0.9900 108.90 108.90 H2B 0.9900 108.90 108.90 107.73 C2 - O2 C1 H2A C3 - Distance Angles O1 1.4223 (0.0018) C1 1.5403 (0.0022) 113.86 (0.14) H3A 0.9900 108.78 108.78 H3B 0.9900 108.78 108.78 107.67 C3 - O1 C1 H3A C4 - Distance Angles C5 1.5280 (0.0021) C1 1.5404 (0.0020) 116.80 (0.12) H4A 0.9900 108.10 108.10 H4B 0.9900 108.10 108.10 107.30 C4 - C5 C1 H4A C5 - Distance Angles C6 1.5214 (0.0020) C4 1.5280 (0.0021) 112.29 (0.12) H5A 0.9900 109.15 109.15 H5B 0.9900 109.15 109.15 107.87 C5 - C6 C4 H5A C6 - Distance Angles C5 1.5214 (0.0020) C7 1.5226 (0.0021) 114.13 (0.13) H6A 0.9900 108.72 108.72 H6B 0.9900 108.72 108.72 107.63 C6 - C5 C7 H6A C7 - Distance Angles C6 1.5226 (0.0021) H7A 0.9800 109.47 H7B 0.9800 109.47 109.47 H7C 0.9800 109.47 109.47 109.47 C7 - C6 H7A H7B C8 - Distance Angles C9 1.5261 (0.0021) C1 1.5416 (0.0019) 116.59 (0.13) H8A 0.9900 108.14 108.14 H8B 0.9900 108.14 108.14 107.32 C8 - C9 C1 H8A C9 - Distance Angles C8 1.5261 (0.0021) C10 1.5263 (0.0021) 112.62 (0.13) H9A 0.9900 109.07 109.07 H9B 0.9900 109.07 109.07 107.83 C9 - C8 C10 H9A C10 - Distance Angles C11 1.5196 (0.0023) C9 1.5263 (0.0021) 112.91 (0.14) H10A 0.9900 109.00 109.00 H10B 0.9900 109.01 109.00 107.79 C10 - C11 C9 H10A C11 - Distance Angles C10 1.5196 (0.0023) H11A 0.9800 109.47 H11B 0.9800 109.47 109.47 H11C 0.9800 109.47 109.47 109.47 C11 - C10 H11A H11B C21 - Distance Angles C23 1.5339 (0.0021) C22 1.5349 (0.0020) 109.68 (0.12) C24 1.5397 (0.0020) 110.88 (0.11) 105.97 (0.12) C28 1.5414 (0.0019) 106.36 (0.12) 111.08 (0.11) 112.90 (0.12) C21 - C23 C22 C24 C22 - Distance Angles O21 1.4299 (0.0019) C21 1.5349 (0.0020) 113.66 (0.13) H22A 0.9900 108.83 108.83 H22B 0.9900 108.83 108.83 107.69 C22 - O21 C21 H22A C23 - Distance Angles O22 1.4313 (0.0017) C21 1.5339 (0.0021) 114.58 (0.12) H23A 0.9900 108.62 108.62 H23B 0.9900 108.62 108.62 107.57 C23 - O22 C21 H23A C24 - Distance Angles C25 1.5263 (0.0020) C21 1.5397 (0.0020) 117.40 (0.12) H24A 0.9900 107.95 107.95 H24B 0.9900 107.95 107.95 107.22 C24 - C25 C21 H24A C25 - Distance Angles C26 1.5259 (0.0021) C24 1.5263 (0.0020) 112.07 (0.12) H25A 0.9900 109.20 109.20 H25B 0.9900 109.20 109.20 107.90 C25 - C26 C24 H25A C26 - Distance Angles C27 1.5251 (0.0022) C25 1.5259 (0.0021) 112.72 (0.13) H26A 0.9900 109.05 109.05 H26B 0.9900 109.05 109.05 107.81 C26 - C27 C25 H26A C27 - Distance Angles C26 1.5251 (0.0022) H27A 0.9800 109.47 H27B 0.9800 109.47 109.47 H27C 0.9800 109.47 109.47 109.47 C27 - C26 H27A H27B C28 - Distance Angles C29 1.5279 (0.0021) C21 1.5414 (0.0019) 116.98 (0.12) H28A 0.9900 108.05 108.05 H28B 0.9900 108.05 108.05 107.27 C28 - C29 C21 H28A C29 - Distance Angles C30 1.5219 (0.0020) C28 1.5279 (0.0020) 112.74 (0.13) H29A 0.9900 109.04 109.04 H29B 0.9900 109.04 109.04 107.81 C29 - C30 C28 H29A C30 - Distance Angles C31 1.5150 (0.0023) C29 1.5219 (0.0020) 113.21 (0.14) H30A 0.9900 108.94 108.94 H30B 0.9900 108.94 108.94 107.75 C30 - C31 C29 H30A C31 - Distance Angles C30 1.5150 (0.0023) H31A 0.9800 109.47 H31B 0.9800 109.47 109.47 H31C 0.9800 109.47 109.47 109.47 C31 - C30 H31A H31B O1 - Distance Angles C3 1.4223 (0.0018) H1 0.8400 109.47 O1 - C3 O2 - Distance Angles C2 1.4357 (0.0020) H2 0.8400 109.47 O2 - C2 O21 - Distance Angles C22 1.4299 (0.0019) H21 0.8400 109.47 O21 - C22 O22 - Distance Angles C23 1.4313 (0.0017) H22 0.8400 109.47 O22 - C23 Specified hydrogen bonds (with su's except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.90 2.6973(15) 159.2 O2-H2...O22 0.84 1.92 2.7323(17) 162.3 O1-H1...O2_$1 0.84 1.87 2.6754(14) 159.5 O21-H21...O1_$2 0.84 1.92 2.7429(16) 164.6 O22-H22...O21_$3 FMAP and GRID set by program FMAP 2 3 34 GRID -1.613 -2 -2 1.613 2 2 R1 = 0.0835 for 5523 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.21 at 0.8544 0.7601 0.1195 [ 0.60 A from C1 ] Deepest hole -0.23 at 0.3925 0.3984 0.1892 [ 0.82 A from C21 ] Mean = 0.00, Rms deviation from mean = 0.04 e/A^3, Highest memory used = 3925 / 25853 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.8544 -0.2399 0.1195 1.00000 0.05 0.21 0.60 C1 0.94 C4 1.55 H4A 1.55 H4B Q2 1 0.4763 0.4162 0.1895 1.00000 0.05 0.20 0.70 C21 0.84 C22 1.51 H22B 1.52 H22A Q3 1 1.0968 -0.2171 0.0397 1.00000 0.05 0.19 0.73 H1 0.96 O1 2.01 C3 2.10 H2A Q4 1 0.0758 0.4741 0.4388 1.00000 0.05 0.18 0.82 H30A 1.33 C30 1.37 H30B 2.15 H31A Q5 1 0.2836 0.6234 0.5032 1.00000 0.05 0.18 0.76 H31B 0.98 C31 1.05 H31C 1.80 H31A Q6 1 1.1949 -0.1043 0.0470 1.00000 0.05 0.17 1.14 H1 1.30 O2 1.73 H2 1.82 O1 Q7 1 0.4487 0.3280 0.1931 1.00000 0.05 0.17 0.65 C21 0.89 C23 1.48 H23B 1.54 H23A Q8 1 0.9176 -0.1997 0.1570 1.00000 0.05 0.16 0.67 C1 0.87 C3 1.51 H3B 1.51 H3A Q9 1 0.4131 0.3769 0.2514 1.00000 0.05 0.16 0.64 C21 0.91 C28 1.52 H28A 1.58 H28B Q10 1 0.4417 0.6409 0.0469 1.00000 0.05 0.16 1.10 O21 1.13 H22 1.52 H21 1.80 C22 Shortest distances between peaks (including symmetry equivalents) 7 9 1.02 2 7 1.05 2 9 1.05 1 8 1.06 3 6 1.78 4 4 2.15 3 8 2.21 1 3 2.51 2 10 2.54 6 10 2.93 Time profile in seconds ----------------------- 0.02: 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. 1.17: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.00: Generate idealized H-atoms 2.44: Structure factors and derivatives 4.16: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.31: Solve l.s. equations 0.00: Generate HTAB table 0.08: Other dependent quantities, CIF, tables 0.08: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009skc0163 finished at 14:02:29 Total CPU time: 8.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++