+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0064p-1 started at 15:35:44 on 06-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0064p-1 in P-1 CELL 0.71069 9.2652 10.5292 10.5973 105.472 99.121 93.957 ZERR 4.00 0.0006 0.0010 0.0010 0.045 0.005 0.005 LATT 1 SFAC C H N O UNIT 32 60 4 16 V = 977.01 F(000) = 408.0 Mu = 0.10 mm-1 Cell Wt = 756.84 Rho = 1.286 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 HTAB N21 O31A EQIV_$1 -x+2, -y-2, -z+1 HTAB O4A O31A_$1 EQIV_$2 -x+1, -y-2, -z+1 HTAB N21 O1A_$2 EQIV_$3 -x+1, -y-1, -z+1 HTAB N21 O34B_$3 HTAB O34A O1B_$3 EQIV_$4 x-1, y, z-1 HTAB N41A O4B_$4 HTAB N41A O31B_$4 HTAB N41B O4B_$4 HTAB N41B O31B_$4 EQIV_$6 -x+1, -y-1, -z HTAB N41A O34A_$6 HTAB N41B O34A_$6 EQIV_$7 x, y, z-1 HTAB N41A O1A_$7 HTAB N41B O1A_$7 FMAP 2 PLAN 10 SIZE 0.13 0.15 0.18 ACTA BOND $H WGHT 0.08620 0.15910 L.S. 4 TEMP -153.00 FVAR 0.85973 0.46679 MOLE 1 C1 1 0.591794 -0.894864 0.633809 11.00000 0.02315 0.02504 = 0.02946 0.00354 0.00099 0.00478 C2 1 0.701244 -0.992482 0.623756 11.00000 0.02317 0.02425 = 0.03473 0.00843 0.00496 0.00387 AFIX 43 H2 2 0.667948 -1.082373 0.614809 11.00000 -1.20000 AFIX 0 C3 1 0.842090 -0.960452 0.626644 11.00000 0.02391 0.02450 = 0.04025 0.01180 0.00591 0.00637 AFIX 43 H3 2 0.876259 -0.870271 0.637808 11.00000 -1.20000 AFIX 0 C4 1 0.949447 -1.059229 0.613205 11.00000 0.02198 0.02753 = 0.04392 0.01542 0.01172 0.00636 O1A 4 0.473530 -0.921634 0.667399 11.00000 0.01898 0.03110 = 0.04572 0.01032 0.00850 0.00489 O1B 4 0.627376 -0.789009 0.604030 11.00000 0.02291 0.02542 = 0.04453 0.01319 0.00707 0.00619 O4A 4 0.894385 -1.179126 0.553250 11.00000 0.02093 0.02508 = 0.05682 0.01222 0.00932 0.00862 AFIX 147 H4 2 0.962175 -1.228208 0.547096 11.00000 -1.50000 AFIX 0 O4B 4 1.082209 -1.023743 0.654813 11.00000 0.01868 0.03210 = 0.06419 0.01509 0.00540 0.00696 MOLE 2 C22 1 0.654526 -0.856986 0.179772 11.00000 0.03134 0.04188 = 0.03589 0.00417 0.00588 0.00867 AFIX 23 H22A 2 0.558408 -0.901153 0.125159 11.00000 -1.20000 H22B 2 0.728958 -0.918868 0.159637 11.00000 -1.20000 AFIX 0 C23 1 0.694912 -0.734284 0.141569 11.00000 0.02999 0.04885 = 0.03407 0.00785 0.00466 0.00363 AFIX 23 H23A 2 0.787074 -0.686102 0.200702 11.00000 -1.20000 H23B 2 0.616349 -0.675470 0.154205 11.00000 -1.20000 AFIX 0 C24 1 0.716144 -0.766360 -0.002958 11.00000 0.04298 0.06670 = 0.03163 0.00794 0.00427 0.00505 AFIX 23 H24A 2 0.794575 -0.825370 -0.015190 11.00000 -1.20000 H24B 2 0.623958 -0.815015 -0.061669 11.00000 -1.20000 AFIX 0 C25 1 0.756710 -0.644524 -0.044477 11.00000 0.07709 0.09053 = 0.04207 0.02445 0.01864 0.00203 AFIX 137 H25A 2 0.674713 -0.590426 -0.042279 11.00000 -1.50000 H25B 2 0.777602 -0.671152 -0.135065 11.00000 -1.50000 H25C 2 0.844216 -0.592703 0.016890 11.00000 -1.50000 AFIX 0 N21 3 0.644891 -0.829636 0.323193 11.00000 0.02496 0.03426 = 0.03776 0.00975 0.00619 0.00722 AFIX 137 H21A 2 0.734406 -0.793436 0.373970 11.00000 -1.50000 H21B 2 0.616917 -0.906796 0.340689 11.00000 -1.50000 H21C 2 0.577459 -0.771950 0.342636 11.00000 -1.50000 AFIX 0 MOLE 3 C31 1 0.909678 -0.600103 0.593800 11.00000 0.02194 0.02072 = 0.04529 0.01130 0.00830 0.00443 C32 1 0.793224 -0.510158 0.603740 11.00000 0.02071 0.02454 = 0.04168 0.00930 0.00649 0.00303 AFIX 43 H32 2 0.761870 -0.479611 0.686632 11.00000 -1.20000 AFIX 0 C33 1 0.731462 -0.470918 0.501767 11.00000 0.02022 0.02376 = 0.04361 0.00853 0.01013 0.00222 AFIX 43 H33 2 0.762012 -0.503029 0.418711 11.00000 -1.20000 AFIX 0 C34 1 0.616997 -0.379386 0.510466 11.00000 0.01561 0.02109 = 0.04643 0.01082 0.00655 0.00112 O31A 4 0.915312 -0.670092 0.474697 11.00000 0.02330 0.02662 = 0.04247 0.00868 0.00623 0.00745 O31B 4 0.993688 -0.602537 0.695382 11.00000 0.03009 0.03654 = 0.04327 0.01129 0.00146 0.01283 O34A 4 0.571915 -0.353047 0.399043 11.00000 0.02187 0.03180 = 0.04750 0.01621 0.00731 0.01067 AFIX 147 H34 2 0.502556 -0.305924 0.407435 11.00000 -1.50000 AFIX 0 O34B 4 0.571995 -0.334391 0.614623 11.00000 0.02585 0.02784 = 0.04387 0.00997 0.01023 0.00996 MOLE 4 PART 1 C42A 1 0.286201 -0.742202 -0.147279 21.00000 0.03470 0.04862 = 0.01447 0.00384 0.00646 0.01709 AFIX 23 H42A 2 0.336835 -0.650585 -0.111781 21.00000 -1.20000 H42B 2 0.359753 -0.805760 -0.144531 21.00000 -1.20000 AFIX 0 C43A 1 0.164012 -0.765666 -0.068711 21.00000 0.03895 0.05146 = 0.03915 0.02206 -0.00393 0.01130 AFIX 23 H43A 2 0.098419 -0.694894 -0.064635 21.00000 -1.20000 H43B 2 0.104067 -0.851808 -0.115479 21.00000 -1.20000 AFIX 0 C44A 1 0.231696 -0.765795 0.073211 21.00000 0.03502 0.07802 = 0.02909 0.01245 0.00058 0.00482 AFIX 23 H44A 2 0.318553 -0.815553 0.072027 21.00000 -1.20000 H44B 2 0.263155 -0.673824 0.130119 21.00000 -1.20000 AFIX 0 C45A 1 0.117085 -0.829928 0.124577 21.00000 0.12674 0.11901 = 0.04025 0.04260 -0.00793 -0.00392 AFIX 137 H45A 2 0.026869 -0.787550 0.113243 21.00000 -1.50000 H45B 2 0.150820 -0.820731 0.219364 21.00000 -1.50000 H45C 2 0.097147 -0.924265 0.075372 21.00000 -1.50000 AFIX 0 N41A 3 0.218318 -0.760745 -0.257997 21.00000 0.04046 0.04141 = 0.05694 0.02024 0.02943 0.00478 AFIX 137 H41A 2 0.164605 -0.842060 -0.284592 21.00000 -1.50000 H41B 2 0.281998 -0.757130 -0.314432 21.00000 -1.50000 H41C 2 0.156822 -0.697120 -0.259011 21.00000 -1.50000 AFIX 0 PART 2 C42B 1 0.306322 -0.695613 -0.124465 -21.00000 0.05472 0.05438 = 0.03898 -0.01304 0.01392 0.00697 AFIX 23 H42C 2 0.403246 -0.729678 -0.115090 -21.00000 -1.20000 H42D 2 0.326620 -0.599071 -0.111976 -21.00000 -1.20000 AFIX 0 C43B 1 0.244723 -0.709370 -0.014757 -21.00000 0.10605 0.09382 = 0.03016 0.02219 -0.00761 -0.03999 AFIX 23 H43C 2 0.327680 -0.684874 0.061903 -21.00000 -1.20000 H43D 2 0.179880 -0.638158 0.002305 -21.00000 -1.20000 AFIX 0 C44B 1 0.166180 -0.820063 -0.002898 -21.00000 0.08336 0.11347 = 0.03888 0.01837 -0.00182 -0.03341 AFIX 23 H44C 2 0.227473 -0.894209 -0.016928 -21.00000 -1.20000 H44D 2 0.077825 -0.845493 -0.074342 -21.00000 -1.20000 AFIX 0 C45B 1 0.114596 -0.801010 0.138638 -21.00000 0.03761 0.07441 = 0.08330 0.04877 0.01299 -0.01261 AFIX 137 H45D 2 0.201399 -0.779779 0.209966 -21.00000 -1.50000 H45E 2 0.058186 -0.883219 0.138708 -21.00000 -1.50000 H45F 2 0.052839 -0.728449 0.153291 -21.00000 -1.50000 AFIX 0 N41B 3 0.223802 -0.762413 -0.284844 -21.00000 0.01511 0.03111 = 0.03214 0.01074 0.00854 0.00558 AFIX 137 H41D 2 0.192616 -0.849694 -0.298501 -21.00000 -1.50000 H41E 2 0.289008 -0.754708 -0.338946 -21.00000 -1.50000 H41F 2 0.145254 -0.718884 -0.303632 -21.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 06skc0064p-1 in P-1 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 C22 - N21 C23 C23 - C22 C24 C24 - C25 C23 C25 - C24 N21 - C22 C31 - O31B O31A C32 C32 - C33 C31 C33 - C32 C34 C34 - O34B O34A C33 O31A - C31 O31B - C31 O34A - C34 O34B - C34 C42A_a - N41A_a C43A_a C43A_a - C44A_a C42A_a C44A_a - C45A_a C43A_a C45A_a - C44A_a N41A_a - C42A_a C42B_b - C43B_b N41B_b C43B_b - C44B_b C42B_b C44B_b - C43B_b C45B_b C45B_b - C44B_b N41B_b - C42B_b Operators for generating equivalent atoms: $1 -x+2, -y-2, -z+1 $2 -x+1, -y-2, -z+1 $3 -x+1, -y-1, -z+1 $4 x-1, y, z-1 $6 -x+1, -y-1, -z $7 x, y, z-1 19777 Reflections read, of which 37 rejected -12 =< h =< 11, -13 =< k =< 13, -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) 6 1 5 81.22 3.19 4 16.10 -4 -9 6 53.93 19.97 2 130.14 5 -8 6 34.28 5.43 6 28.41 -3 -6 10 26.85 15.83 3 89.59 4 Inconsistent equivalents 4473 Unique reflections, of which 0 suppressed R(int) = 0.0847 R(sigma) = 0.0962 Friedel opposites merged Maximum memory for data reduction = 3830 / 44533 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 = 4743 / 360836 wR2 = 0.1821 before cycle 1 for 4473 data and 289 / 289 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0862 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.85971 0.00254 -0.009 OSF 2 0.46678 0.01076 -0.001 FVAR 2 Mean shift/esd = 0.001 Maximum = -0.009 for OSF Max. shift = 0.000 A for H41A_a Max. dU = 0.000 for C44B_b Least-squares cycle 2 Maximum vector length = 511 Memory required = 4743 / 360836 wR2 = 0.1821 before cycle 2 for 4473 data and 289 / 289 parameters GooF = S = 1.031; Restrained GooF = 1.031 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0862 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.85971 0.00254 0.002 OSF 2 0.46677 0.01076 -0.001 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.002 for OSF Max. shift = 0.000 A for H41A_a Max. dU = 0.000 for C44B_b Least-squares cycle 3 Maximum vector length = 511 Memory required = 4743 / 360836 wR2 = 0.1821 before cycle 3 for 4473 data and 289 / 289 parameters GooF = S = 1.031; Restrained GooF = 1.031 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0862 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.85971 0.00254 0.000 OSF 2 0.46676 0.01076 -0.001 FVAR 2 Mean shift/esd = 0.000 Maximum = -0.001 for FVAR 2 Max. shift = 0.000 A for H45A_a Max. dU = 0.000 for N41A_a Least-squares cycle 4 Maximum vector length = 511 Memory required = 4743 / 360836 wR2 = 0.1821 before cycle 4 for 4473 data and 289 / 289 parameters GooF = S = 1.031; Restrained GooF = 1.031 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0862 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.85971 0.00254 0.000 OSF 2 0.46676 0.01076 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for U22 C42A_a Max. shift = 0.000 A for H45A_a Max. dU = 0.000 for N41A_a Largest correlation matrix elements -0.981 y N41B_b / y N41A_a 0.845 y N41B_b / U23 N41A_a -0.800 U11 N41B_b / U11 N41A_a -0.960 x N41B_b / x N41A_a -0.842 x C42B_b / x C42A_a -0.797 U12 C42B_b / x C42B_b 0.931 z N41B_b / U33 N41A_a -0.833 y C45B_b / y C45A_a -0.772 z C42B_b / U33 C42A_a -0.918 z N41B_b / z N41A_a -0.820 U12 N41B_b / U12 N41A_a 0.767 U12 C42B_b / x C42A_a -0.895 U33 N41B_b / z N41A_a 0.812 U33 N41B_b / z N41B_b -0.759 x C42B_b / U12 C42A_a -0.882 z C45B_b / z C45A_a -0.810 U33 N41A_a / z N41A_a -0.757 U11 C45B_b / U11 C45A_a -0.853 x C45B_b / x C45A_a -0.806 y C45B_b / U22 C45A_a -0.740 U23 C42B_b / z C42B_b -0.848 U22 N41B_b / U22 N41A_a -0.802 U23 N41A_a / y N41A_a 0.735 U12 C42A_a / x C42A_a Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.6679 -1.0824 0.6148 43 0.950 0.000 C2 C3 C1 H3 0.8763 -0.8703 0.6378 43 0.950 0.000 C3 C2 C4 H4 0.9622 -1.2282 0.5471 147 0.840 0.000 O4A C4 H4 H22A 0.5584 -0.9012 0.1252 23 0.990 0.000 C22 N21 C23 H22B 0.7290 -0.9189 0.1596 23 0.990 0.000 C22 N21 C23 H23A 0.7871 -0.6861 0.2007 23 0.990 0.000 C23 C22 C24 H23B 0.6164 -0.6755 0.1542 23 0.990 0.000 C23 C22 C24 H24A 0.7946 -0.8254 -0.0152 23 0.990 0.000 C24 C25 C23 H24B 0.6240 -0.8150 -0.0617 23 0.990 0.000 C24 C25 C23 H25A 0.6747 -0.5904 -0.0423 137 0.980 0.000 C25 C24 H25A H25B 0.7776 -0.6712 -0.1351 137 0.980 0.000 C25 C24 H25A H25C 0.8442 -0.5927 0.0169 137 0.980 0.000 C25 C24 H25A H21A 0.7344 -0.7934 0.3740 137 0.910 0.000 N21 C22 H21A H21B 0.6169 -0.9068 0.3407 137 0.910 0.000 N21 C22 H21A H21C 0.5775 -0.7720 0.3426 137 0.910 0.000 N21 C22 H21A H32 0.7619 -0.4796 0.6866 43 0.950 0.000 C32 C33 C31 H33 0.7620 -0.5030 0.4187 43 0.950 0.000 C33 C32 C34 H34 0.5026 -0.3059 0.4074 147 0.840 0.000 O34A C34 H34 H42A 0.3368 -0.6506 -0.1118 23 0.990 0.000 C42A_a N41A_a C43A_a H42B 0.3597 -0.8058 -0.1445 23 0.990 0.000 C42A_a N41A_a C43A_a H43A 0.0984 -0.6949 -0.0646 23 0.990 0.000 C43A_a C44A_a C42A_a H43B 0.1041 -0.8518 -0.1155 23 0.990 0.000 C43A_a C44A_a C42A_a H44A 0.3186 -0.8155 0.0720 23 0.990 0.000 C44A_a C45A_a C43A_a H44B 0.2632 -0.6738 0.1301 23 0.990 0.000 C44A_a C45A_a C43A_a H45A 0.0269 -0.7876 0.1132 137 0.980 0.000 C45A_a C44A_a H45A_a H45B 0.1508 -0.8207 0.2194 137 0.980 0.000 C45A_a C44A_a H45A_a H45C 0.0972 -0.9243 0.0754 137 0.980 0.000 C45A_a C44A_a H45A_a H41A 0.1646 -0.8421 -0.2846 137 0.910 0.000 N41A_a C42A_a H41A_a H41B 0.2820 -0.7571 -0.3144 137 0.910 0.000 N41A_a C42A_a H41A_a H41C 0.1568 -0.6971 -0.2590 137 0.910 0.000 N41A_a C42A_a H41A_a H42C 0.4032 -0.7297 -0.1151 23 0.990 0.000 C42B_b C43B_b N41B_b H42D 0.3266 -0.5991 -0.1120 23 0.990 0.000 C42B_b C43B_b N41B_b H43C 0.3277 -0.6849 0.0619 23 0.990 0.000 C43B_b C44B_b C42B_b H43D 0.1799 -0.6382 0.0023 23 0.990 0.000 C43B_b C44B_b C42B_b H44C 0.2275 -0.8942 -0.0169 23 0.990 0.000 C44B_b C43B_b C45B_b H44D 0.0778 -0.8455 -0.0743 23 0.990 0.000 C44B_b C43B_b C45B_b H45D 0.2014 -0.7798 0.2100 137 0.980 0.000 C45B_b C44B_b H45D_b H45E 0.0582 -0.8832 0.1387 137 0.980 0.000 C45B_b C44B_b H45D_b H45F 0.0528 -0.7284 0.1533 137 0.980 0.000 C45B_b C44B_b H45D_b H41D 0.1926 -0.8497 -0.2985 137 0.910 0.000 N41B_b C42B_b H41D_b H41E 0.2890 -0.7547 -0.3389 137 0.910 0.000 N41B_b C42B_b H41D_b H41F 0.1453 -0.7189 -0.3036 137 0.910 0.000 N41B_b C42B_b H41D_b 06skc0064p-1 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.59179 -0.89486 0.63381 1.00000 0.02315 0.02504 0.02947 0.00354 0.00099 0.00478 0.02704 0.00512 0.00026 0.00025 0.00025 0.00000 0.00125 0.00148 0.00140 0.00114 0.00107 0.00103 0.00059 C2 0.70124 -0.99248 0.62376 1.00000 0.02317 0.02425 0.03473 0.00843 0.00496 0.00387 0.02735 0.00516 0.00025 0.00025 0.00025 0.00000 0.00124 0.00143 0.00147 0.00116 0.00108 0.00101 0.00059 H2 0.66795 -1.08237 0.61481 1.00000 0.03282 0.00000 0.00000 C3 0.84209 -0.96045 0.62664 1.00000 0.02392 0.02450 0.04026 0.01180 0.00591 0.00637 0.02886 0.00535 0.00025 0.00025 0.00025 0.00000 0.00126 0.00144 0.00157 0.00121 0.00112 0.00102 0.00060 H3 0.87626 -0.87027 0.63781 1.00000 0.03463 0.00000 0.00000 C4 0.94945 -1.05923 0.61321 1.00000 0.02198 0.02754 0.04392 0.01542 0.01172 0.00636 0.02928 0.00577 0.00026 0.00026 0.00027 0.00000 0.00127 0.00156 0.00160 0.00127 0.00115 0.00107 0.00061 O1A 0.47353 -0.92163 0.66740 1.00000 0.01898 0.03110 0.04573 0.01032 0.00850 0.00490 0.03165 0.00358 0.00017 0.00017 0.00018 0.00000 0.00086 0.00107 0.00113 0.00087 0.00078 0.00071 0.00045 O1B 0.62738 -0.78901 0.60403 1.00000 0.02291 0.02542 0.04453 0.01320 0.00707 0.00619 0.03004 0.00352 0.00017 0.00016 0.00017 0.00000 0.00087 0.00105 0.00111 0.00087 0.00079 0.00072 0.00044 O4A 0.89438 -1.17913 0.55325 1.00000 0.02093 0.02508 0.05682 0.01223 0.00932 0.00862 0.03361 0.00372 0.00017 0.00017 0.00019 0.00000 0.00086 0.00108 0.00122 0.00093 0.00085 0.00074 0.00046 H4 0.96217 -1.22821 0.54710 1.00000 0.05041 0.00000 0.00000 O4B 1.08221 -1.02374 0.65481 1.00000 0.01868 0.03210 0.06420 0.01509 0.00540 0.00696 0.03809 0.00386 0.00017 0.00018 0.00020 0.00000 0.00089 0.00111 0.00132 0.00096 0.00085 0.00074 0.00050 C22 0.65453 -0.85699 0.17977 1.00000 0.03134 0.04188 0.03589 0.00417 0.00588 0.00868 0.03752 0.00578 0.00029 0.00029 0.00026 0.00000 0.00143 0.00180 0.00160 0.00135 0.00122 0.00121 0.00069 H22A 0.55841 -0.90115 0.12516 1.00000 0.04503 0.00000 0.00000 H22B 0.72896 -0.91887 0.15964 1.00000 0.04503 0.00000 0.00000 C23 0.69491 -0.73428 0.14157 1.00000 0.02999 0.04885 0.03407 0.00785 0.00466 0.00363 0.03858 0.00577 0.00029 0.00029 0.00026 0.00000 0.00142 0.00191 0.00156 0.00140 0.00120 0.00124 0.00070 H23A 0.78707 -0.68610 0.20070 1.00000 0.04629 0.00000 0.00000 H23B 0.61635 -0.67547 0.15420 1.00000 0.04629 0.00000 0.00000 C24 0.71614 -0.76636 -0.00296 1.00000 0.04298 0.06671 0.03163 0.00794 0.00427 0.00505 0.04863 0.00636 0.00033 0.00034 0.00028 0.00000 0.00172 0.00228 0.00164 0.00156 0.00134 0.00152 0.00082 H24A 0.79457 -0.82537 -0.01519 1.00000 0.05836 0.00000 0.00000 H24B 0.62396 -0.81501 -0.06167 1.00000 0.05836 0.00000 0.00000 C25 0.75671 -0.64452 -0.04448 1.00000 0.07709 0.09053 0.04207 0.02445 0.01864 0.00203 0.06828 0.00799 0.00041 0.00041 0.00033 0.00000 0.00248 0.00301 0.00199 0.00201 0.00177 0.00212 0.00107 H25A 0.67471 -0.59043 -0.04228 1.00000 0.10242 0.00000 0.00000 H25B 0.77760 -0.67115 -0.13506 1.00000 0.10242 0.00000 0.00000 H25C 0.84421 -0.59270 0.01689 1.00000 0.10242 0.00000 0.00000 N21 0.64489 -0.82964 0.32319 1.00000 0.02497 0.03427 0.03777 0.00975 0.00619 0.00723 0.03218 0.00449 0.00022 0.00021 0.00021 0.00000 0.00107 0.00135 0.00129 0.00105 0.00094 0.00091 0.00054 H21A 0.73440 -0.79344 0.37397 1.00000 0.04827 0.00000 0.00000 H21B 0.61692 -0.90679 0.34069 1.00000 0.04827 0.00000 0.00000 H21C 0.57746 -0.77195 0.34264 1.00000 0.04827 0.00000 0.00000 C31 0.90968 -0.60010 0.59380 1.00000 0.02194 0.02072 0.04529 0.01130 0.00830 0.00443 0.02859 0.00552 0.00025 0.00024 0.00028 0.00000 0.00126 0.00143 0.00175 0.00129 0.00124 0.00101 0.00061 C32 0.79322 -0.51016 0.60374 1.00000 0.02071 0.02454 0.04168 0.00930 0.00649 0.00303 0.02888 0.00522 0.00025 0.00024 0.00027 0.00000 0.00119 0.00144 0.00158 0.00123 0.00112 0.00099 0.00060 H32 0.76187 -0.47961 0.68663 1.00000 0.03465 0.00000 0.00000 C33 0.73146 -0.47092 0.50177 1.00000 0.02022 0.02376 0.04361 0.00853 0.01013 0.00222 0.02892 0.00532 0.00024 0.00024 0.00027 0.00000 0.00117 0.00141 0.00161 0.00123 0.00113 0.00099 0.00060 H33 0.76201 -0.50303 0.41871 1.00000 0.03470 0.00000 0.00000 C34 0.61700 -0.37939 0.51047 1.00000 0.01561 0.02109 0.04643 0.01083 0.00655 0.00112 0.02741 0.00524 0.00024 0.00024 0.00028 0.00000 0.00115 0.00143 0.00172 0.00128 0.00117 0.00098 0.00061 O31A 0.91531 -0.67009 0.47470 1.00000 0.02330 0.02662 0.04247 0.00868 0.00623 0.00745 0.03076 0.00357 0.00017 0.00017 0.00018 0.00000 0.00089 0.00104 0.00114 0.00089 0.00079 0.00072 0.00045 O31B 0.99369 -0.60254 0.69538 1.00000 0.03009 0.03654 0.04328 0.01129 0.00146 0.01283 0.03679 0.00385 0.00019 0.00018 0.00019 0.00000 0.00096 0.00115 0.00116 0.00092 0.00088 0.00080 0.00048 O34A 0.57191 -0.35305 0.39904 1.00000 0.02187 0.03180 0.04750 0.01621 0.00731 0.01067 0.03226 0.00375 0.00017 0.00017 0.00018 0.00000 0.00090 0.00112 0.00118 0.00091 0.00080 0.00074 0.00046 H34 0.50256 -0.30593 0.40743 1.00000 0.04839 0.00000 0.00000 O34B 0.57199 -0.33439 0.61462 1.00000 0.02585 0.02784 0.04388 0.00997 0.01023 0.00996 0.03178 0.00367 0.00017 0.00017 0.00018 0.00000 0.00092 0.00103 0.00115 0.00088 0.00084 0.00075 0.00045 C42A_a 0.28620 -0.74221 -0.14728 0.46676 0.03470 0.04861 0.01448 0.00384 0.00646 0.01708 0.03277 0.02865 0.00175 0.00142 0.00140 0.01076 0.00566 0.00838 0.00619 0.00580 0.00437 0.00587 0.00284 H42A_a 0.33683 -0.65059 -0.11178 0.46676 0.03933 0.01076 0.00000 H42B_a 0.35974 -0.80577 -0.14453 0.46676 0.03933 0.01076 0.00000 C43A_a 0.16401 -0.76567 -0.06871 0.46676 0.03894 0.05145 0.03914 0.02206 -0.00393 0.01130 0.04233 0.02160 0.00090 0.00093 0.00089 0.01076 0.00427 0.00535 0.00500 0.00417 0.00366 0.00353 0.00243 H43A_a 0.09842 -0.69490 -0.06464 0.46676 0.05079 0.01076 0.00000 H43B_a 0.10407 -0.85181 -0.11548 0.46676 0.05079 0.01076 0.00000 C44A_a 0.23170 -0.76579 0.07321 0.46676 0.03502 0.07801 0.02908 0.01245 0.00058 0.00482 0.04858 0.02129 0.00083 0.00093 0.00089 0.01076 0.00397 0.00603 0.00476 0.00429 0.00365 0.00371 0.00266 H44A_a 0.31855 -0.81555 0.07203 0.46676 0.05830 0.01076 0.00000 H44B_a 0.26315 -0.67382 0.13012 0.46676 0.05830 0.01076 0.00000 C45A_a 0.11709 -0.82993 0.12457 0.46676 0.12675 0.11900 0.04026 0.04260 -0.00793 -0.00391 0.09493 0.05314 0.00256 0.00306 0.00234 0.01076 0.01572 0.01729 0.00802 0.00887 0.00794 0.01085 0.00895 H45A_a 0.02687 -0.78756 0.11324 0.46676 0.14240 0.01076 0.00000 H45B_a 0.15082 -0.82073 0.21936 0.46676 0.14240 0.01076 0.00000 H45C_a 0.09716 -0.92427 0.07537 0.46676 0.14240 0.01076 0.00000 N41A_a 0.21832 -0.76075 -0.25799 0.46676 0.04046 0.04141 0.05692 0.02024 0.02942 0.00478 0.04268 0.06595 0.00272 0.00334 0.00303 0.01076 0.00665 0.00685 0.01523 0.00819 0.00637 0.00462 0.00648 H41A_a 0.16460 -0.84206 -0.28459 0.46676 0.06402 0.01076 0.00000 H41B_a 0.28199 -0.75713 -0.31443 0.46676 0.06402 0.01076 0.00000 H41C_a 0.15683 -0.69712 -0.25900 0.46676 0.06402 0.01076 0.00000 C42B_b 0.30632 -0.69561 -0.12447 0.53324 0.05471 0.05437 0.03899 -0.01303 0.01392 0.00696 0.05386 0.02971 0.00216 0.00134 0.00172 0.01076 0.00554 0.00767 0.00604 0.00560 0.00431 0.00626 0.00390 H42C_b 0.40324 -0.72968 -0.11509 0.53324 0.06464 0.01076 0.00000 H42D_b 0.32662 -0.59907 -0.11198 0.53324 0.06464 0.01076 0.00000 C43B_b 0.24472 -0.70937 -0.01476 0.53324 0.10607 0.09382 0.03017 0.02219 -0.00761 -0.03999 0.08059 0.02049 0.00121 0.00091 0.00077 0.01076 0.00703 0.00652 0.00435 0.00416 0.00446 0.00563 0.00308 H43C_b 0.32768 -0.68487 0.06190 0.53324 0.09670 0.01076 0.00000 H43D_b 0.17988 -0.63816 0.00230 0.53324 0.09670 0.01076 0.00000 C44B_b 0.16618 -0.82006 -0.00290 0.53324 0.08336 0.11349 0.03889 0.01837 -0.00181 -0.03341 0.08288 0.02215 0.00108 0.00110 0.00095 0.01076 0.00597 0.00787 0.00544 0.00536 0.00471 0.00568 0.00309 H44C_b 0.22747 -0.89421 -0.01693 0.53324 0.09945 0.01076 0.00000 H44D_b 0.07783 -0.84549 -0.07434 0.53324 0.09945 0.01076 0.00000 C45B_b 0.11459 -0.80101 0.13864 0.53324 0.03761 0.07441 0.08330 0.04877 0.01299 -0.01261 0.06063 0.04021 0.00150 0.00234 0.00195 0.01076 0.00542 0.00767 0.01090 0.00686 0.00518 0.00427 0.00410 H45D_b 0.20140 -0.77978 0.20996 0.53324 0.09095 0.01076 0.00000 H45E_b 0.05819 -0.88322 0.13871 0.53324 0.09095 0.01076 0.00000 H45F_b 0.05284 -0.72845 0.15329 0.53324 0.09095 0.01076 0.00000 N41B_b 0.22380 -0.76241 -0.28485 0.53324 0.01511 0.03111 0.03214 0.01074 0.00855 0.00558 0.02515 0.05021 0.00187 0.00255 0.00260 0.01076 0.00407 0.00465 0.00643 0.00379 0.00409 0.00337 0.00262 H41D_b 0.19262 -0.84969 -0.29851 0.53324 0.03772 0.01076 0.00000 H41E_b 0.28901 -0.75470 -0.33895 0.53324 0.03772 0.01076 0.00000 H41F_b 0.14525 -0.71889 -0.30363 0.53324 0.03772 0.01076 0.00000 Final Structure Factor Calculation for 06skc0064p-1 in P-1 Total number of l.s. parameters = 289 Maximum vector length = 511 Memory required = 4454 / 22995 wR2 = 0.1821 before cycle 5 for 4473 data and 0 / 289 parameters GooF = S = 1.031; Restrained GooF = 1.031 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0862 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0657 for 2463 Fo > 4sig(Fo) and 0.1410 for all 4473 data wR2 = 0.1821, GooF = S = 1.031, Restrained GooF = 1.031 for all data Occupancy sum of asymmetric unit = 26.00 for non-hydrogen and 30.00 for hydrogen atoms Principal mean square atomic displacements U 0.0362 0.0235 0.0214 C1 0.0351 0.0246 0.0223 C2 0.0404 0.0265 0.0197 C3 0.0449 0.0238 0.0191 C4 0.0462 0.0310 0.0177 O1A 0.0446 0.0256 0.0199 O1B 0.0574 0.0275 0.0159 O4A 0.0655 0.0318 0.0170 O4B 0.0503 0.0338 0.0285 C22 0.0514 0.0345 0.0298 C23 0.0704 0.0441 0.0314 C24 0.0953 0.0752 0.0343 C25 0.0383 0.0352 0.0231 N21 0.0454 0.0216 0.0188 C31 0.0421 0.0242 0.0203 C32 0.0447 0.0238 0.0183 C33 0.0467 0.0207 0.0147 C34 0.0435 0.0293 0.0195 O31A 0.0492 0.0399 0.0213 O31B 0.0480 0.0322 0.0166 O34A 0.0444 0.0321 0.0188 O34B 0.0580 0.0269 0.0134 C42A_a 0.0547 0.0516 0.0207 C43A_a 0.0801 0.0393 0.0263 C44A_a 0.1523 0.1066 0.0259 C45A_a 0.0676 0.0413 0.0191 N41A_a 0.0843 0.0548 0.0224 C42B_b 0.1603 0.0547 0.0268 C43B_b 0.1518 0.0596 0.0372 C44B_b 0.1052 0.0577 0.0190 C45B_b 0.0335 0.0290 0.0129 N41B_b Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.007 0.013 0.020 0.028 0.036 0.048 0.062 0.083 0.125 1.000 Number in group 493. 409. 448. 452. 433. 464. 446. 445. 437. 446. GooF 0.866 0.905 0.961 1.018 1.109 1.111 1.141 1.144 1.041 0.981 K 5.872 1.696 0.885 0.927 0.960 0.950 0.977 0.990 1.019 1.000 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.66 inf Number in group 468. 428. 456. 443. 446. 445. 451. 438. 452. 446. GooF 0.941 0.885 0.892 0.969 1.035 1.090 0.992 1.022 1.094 1.324 K 0.872 0.998 1.035 1.019 1.059 1.040 1.036 1.028 1.043 0.973 R1 0.413 0.344 0.286 0.212 0.190 0.144 0.089 0.071 0.056 0.046 Recommended weighting scheme: WGHT 0.0862 0.1590 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) -2 2 2 12.41 0.15 4.64 0.003 2.85 6 -9 2 -2.11 17.40 4.06 0.034 0.96 10 -1 2 -50.39 84.00 3.95 0.074 0.88 1 -2 1 8.86 2.80 3.86 0.013 4.51 -1 2 1 77.56 117.52 3.85 0.087 3.97 1 1 1 11.63 3.38 3.79 0.015 4.76 6 -8 1 79.96 124.28 3.68 0.090 1.04 -4 4 2 6.15 22.48 3.44 0.038 1.66 1 -4 4 9.89 2.72 3.40 0.013 2.02 0 -4 3 84.46 59.04 3.33 0.062 2.36 -4 4 0 126.70 91.57 3.33 0.077 1.79 -5 -1 5 112.76 165.16 3.31 0.103 1.50 2 3 4 25.12 12.81 3.27 0.029 1.56 -4 -9 1 23.19 2.05 3.27 0.012 0.99 -10 6 5 201.04 109.54 3.19 0.084 0.78 -1 -5 2 81.25 55.39 3.18 0.060 2.01 4 -1 2 18.08 8.17 3.15 0.023 1.98 -4 -2 3 24.21 14.37 3.09 0.030 1.96 -1 3 0 246.83 333.64 3.09 0.147 3.28 1 3 5 22.11 9.95 3.08 0.025 1.47 -2 -6 1 48.47 32.48 3.08 0.046 1.58 1 8 0 3.47 11.38 3.07 0.027 1.23 -7 0 8 57.11 99.98 3.02 0.080 1.00 -10 -1 7 41.53 1.11 3.02 0.008 0.84 4 -5 8 11.54 22.37 3.02 0.038 1.04 -3 0 5 70.52 49.39 3.01 0.057 1.84 4 -4 3 31.19 47.26 3.01 0.055 1.62 2 0 3 37.15 24.62 2.98 0.040 2.48 -3 0 6 127.56 94.56 2.92 0.078 1.59 -3 -1 2 73.25 99.70 2.91 0.080 2.76 0 -4 5 95.17 70.11 2.89 0.067 1.84 0 5 2 117.57 84.92 2.88 0.074 1.71 7 3 2 22.53 11.47 2.88 0.027 1.07 -2 -8 10 25.57 0.08 2.87 0.002 0.92 -8 2 4 24.59 48.64 2.87 0.056 1.09 2 -3 10 437.20 1.63 2.86 0.010 0.99 -6 3 4 46.04 63.89 2.85 0.064 1.28 -5 12 0 104.15 49.05 2.85 0.056 0.80 -1 -2 5 36.23 23.87 2.85 0.039 2.09 0 -11 9 71.38 40.60 2.83 0.051 0.83 4 -1 1 5.65 13.53 2.83 0.030 2.16 -10 3 6 -11.05 26.02 2.82 0.041 0.83 0 -1 11 26.47 55.05 2.81 0.060 0.93 -9 5 3 5.68 25.86 2.81 0.041 0.92 -7 0 5 4.88 20.03 2.79 0.036 1.19 -4 -9 3 19.56 38.95 2.78 0.050 1.01 -1 7 3 8.16 22.13 2.78 0.038 1.22 -5 1 0 23.85 15.48 2.78 0.032 1.83 -1 -1 10 2.63 14.56 2.77 0.031 1.04 8 -9 6 0.07 13.08 2.77 0.029 0.78 Bond lengths and angles C1 - Distance Angles O1A 1.2415 (0.0028) O1B 1.2730 (0.0029) 124.71 (0.22) C2 1.4886 (0.0033) 119.27 (0.23) 116.01 (0.21) C1 - O1A O1B C2 - Distance Angles C3 1.3186 (0.0032) C1 1.4886 (0.0033) 123.29 (0.23) H2 0.9500 118.35 118.35 C2 - C3 C1 C3 - Distance Angles C2 1.3186 (0.0032) C4 1.4832 (0.0034) 122.80 (0.23) H3 0.9500 118.60 118.60 C3 - C2 C4 C4 - Distance Angles O4B 1.2344 (0.0028) O4A 1.2799 (0.0031) 124.18 (0.22) C3 1.4832 (0.0034) 120.51 (0.24) 115.27 (0.20) C4 - O4B O4A O1A - Distance Angles C1 1.2415 (0.0028) O1A - O1B - Distance Angles C1 1.2730 (0.0029) O1B - O4A - Distance Angles C4 1.2799 (0.0031) H4 0.8400 109.47 O4A - C4 O4B - Distance Angles C4 1.2344 (0.0028) O4B - C22 - Distance Angles N21 1.4879 (0.0034) C23 1.4945 (0.0039) 112.89 (0.23) H22A 0.9900 109.01 109.01 H22B 0.9900 109.01 109.01 107.79 C22 - N21 C23 H22A C23 - Distance Angles C22 1.4945 (0.0039) C24 1.5255 (0.0039) 111.71 (0.25) H23A 0.9900 109.28 109.28 H23B 0.9900 109.28 109.28 107.94 C23 - C22 C24 H23A C24 - Distance Angles C25 1.5058 (0.0047) C23 1.5255 (0.0039) 112.94 (0.27) H24A 0.9900 109.00 109.00 H24B 0.9900 109.00 109.00 107.78 C24 - C25 C23 H24A C25 - Distance Angles C24 1.5058 (0.0047) H25A 0.9800 109.47 H25B 0.9800 109.47 109.47 H25C 0.9800 109.47 109.47 109.47 C25 - C24 H25A H25B N21 - Distance Angles C22 1.4879 (0.0034) 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 C31 - Distance Angles O31B 1.2317 (0.0029) O31A 1.2918 (0.0031) 124.87 (0.22) C32 1.4819 (0.0033) 119.67 (0.25) 115.45 (0.22) C31 - O31B O31A C32 - Distance Angles C33 1.3194 (0.0035) C31 1.4819 (0.0033) 122.45 (0.25) H32 0.9500 118.77 118.77 C32 - C33 C31 C33 - Distance Angles C32 1.3194 (0.0035) C34 1.4788 (0.0034) 123.19 (0.26) H33 0.9500 118.40 118.40 C33 - C32 C34 C34 - Distance Angles O34B 1.2292 (0.0030) O34A 1.2961 (0.0030) 124.99 (0.22) C33 1.4788 (0.0033) 121.85 (0.23) 113.16 (0.23) C34 - O34B O34A O31A - Distance Angles C31 1.2918 (0.0031) O31A - O31B - Distance Angles C31 1.2317 (0.0029) O31B - O34A - Distance Angles C34 1.2961 (0.0030) H34 0.8400 109.47 O34A - C34 O34B - Distance Angles C34 1.2292 (0.0030) O34B - C42A_a - Distance Angles N41A_a 1.1988 (0.0313) C43A_a 1.5511 (0.0194) 102.55 (1.67) H42A_a 0.9900 111.26 111.26 H42B_a 0.9900 111.26 111.26 109.16 C42A_a - N41A_a C43A_a H42A_a C43A_a - Distance Angles C44A_a 1.5354 (0.0130) C42A_a 1.5511 (0.0195) 110.65 (0.75) H43A_a 0.9900 109.52 109.52 H43B_a 0.9900 109.52 109.52 108.08 C43A_a - C44A_a C42A_a H43A_a C44A_a - Distance Angles C45A_a 1.4698 (0.0225) C43A_a 1.5354 (0.0130) 106.82 (1.11) H44A_a 0.9900 110.36 110.36 H44B_a 0.9900 110.36 110.36 108.59 C44A_a - C45A_a C43A_a H44A_a C45A_a - Distance Angles C44A_a 1.4698 (0.0224) H45A_a 0.9800 109.47 H45B_a 0.9800 109.47 109.47 H45C_a 0.9800 109.47 109.47 109.47 C45A_a - C44A_a H45A_a H45B_a N41A_a - Distance Angles C42A_a 1.1988 (0.0312) H41A_a 0.9100 109.47 H41B_a 0.9100 109.47 109.47 H41C_a 0.9100 109.47 109.47 109.47 N41A_a - C42A_a H41A_a H41B_a C42B_b - Distance Angles C43B_b 1.4097 (0.0206) N41B_b 1.6864 (0.0300) 124.12 (1.47) H42C_b 0.9900 106.30 106.30 H42D_b 0.9900 106.30 106.30 106.42 C42B_b - C43B_b N41B_b H42C_b C43B_b - Distance Angles C44B_b 1.3761 (0.0136) C42B_b 1.4097 (0.0207) 127.80 (0.91) H43C_b 0.9900 105.35 105.35 H43D_b 0.9900 105.35 105.35 106.00 C43B_b - C44B_b C42B_b H43C_b C44B_b - Distance Angles C43B_b 1.3761 (0.0136) C45B_b 1.6119 (0.0202) 114.40 (1.09) H44C_b 0.9900 108.66 108.66 H44D_b 0.9900 108.66 108.66 107.60 C44B_b - C43B_b C45B_b H44C_b C45B_b - Distance Angles C44B_b 1.6119 (0.0202) H45D_b 0.9800 109.47 H45E_b 0.9800 109.47 109.47 H45F_b 0.9800 109.47 109.47 109.47 C45B_b - C44B_b H45D_b H45E_b N41B_b - Distance Angles C42B_b 1.6864 (0.0300) H41D_b 0.9100 109.47 H41E_b 0.9100 109.47 109.47 H41F_b 0.9100 109.47 109.47 109.47 N41B_b - C42B_b H41D_b H41E_b Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.91 2.01 2.895(3) 164.8 N21-H21A...O31A 0.84 1.61 2.453(2) 175.7 O4A-H4...O31A_$1 0.91 1.91 2.802(3) 165.0 N21-H21B...O1A_$2 0.91 1.88 2.783(3) 174.8 N21-H21C...O34B_$3 0.84 1.63 2.457(2) 168.9 O34A-H34...O1B_$3 0.91 1.91 2.81(3) 170.4 N41A_a-H41A_a...O4B_$4 0.91 1.93 2.82(3) 163.2 N41A_a-H41C_a...O31B_$4 0.91 1.94 2.83(3) 166.4 N41B_b-H41D_b...O4B_$4 0.91 1.93 2.822(19) 167.6 N41B_b-H41F_b...O31B_$4 0.91 2.17 3.00(3) 151.5 N41A_a-H41B_a...O34A_$6 0.91 1.95 2.78(2) 150.7 N41B_b-H41E_b...O34A_$6 0.91 2.56 3.09(3) 117.5 N41A_a-H41B_a...O1A_$7 0.91 2.54 2.98(2) 110.1 N41B_b-H41E_b...O1A_$7 FMAP and GRID set by program FMAP 2 1 24 GRID -2.381 -2 -2 2.381 2 2 R1 = 0.1409 for 4473 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.29 at 0.1223 0.2630 0.0179 [ 0.98 A from C44B ] Deepest hole -0.31 at 0.2640 0.7626 0.0937 [ 1.02 A from C24 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 4229 / 22230 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1223 -0.7370 0.0179 1.00000 0.05 0.29 0.98 C44B 1.03 C43A 1.08 H43A 1.19 C44A Q2 1 0.3056 -0.7748 -0.0264 1.00000 0.05 0.27 0.92 C43B 1.12 H43C 1.22 H44A 1.33 C44A Q3 1 0.2809 -0.6442 0.0858 1.00000 0.05 0.25 0.66 H43C 0.66 H44B 1.09 C43B 1.20 H43D Q4 1 0.0697 -0.7192 -0.0823 1.00000 0.05 0.23 0.35 H43A 1.04 C43A 1.32 H43D 1.36 H44D Q5 1 0.7819 -0.8997 0.0052 1.00000 0.05 0.23 0.87 H24A 1.59 C24 1.84 H22B 1.90 H24B Q6 1 1.0167 -1.2753 0.5413 1.00000 0.05 0.23 0.73 H4 0.89 O31A 1.57 O4A 1.91 C31 Q7 1 0.7909 -0.4644 0.7213 1.00000 0.05 0.21 0.40 H32 1.21 C32 1.99 H44B 2.18 C31 Q8 1 0.5485 -1.1264 0.5425 1.00000 0.05 0.21 1.22 H2 1.85 C2 2.01 H34 2.03 O1B Q9 1 0.6449 -0.9399 0.6265 1.00000 0.05 0.20 0.71 C1 0.78 C2 1.50 H2 1.68 O1B Q10 1 1.2299 -1.0370 0.6072 1.00000 0.05 0.20 1.53 O4B 1.65 H21B 1.89 H21A 2.04 H41D Shortest distances between peaks (including symmetry equivalents) 1 4 1.16 2 3 1.62 1 3 1.65 1 2 1.87 8 9 2.00 3 7 2.28 2 4 2.33 3 4 2.36 8 9 2.59 9 10 2.86 6 10 2.94 1 7 2.95 Time profile in seconds ----------------------- 0.09: Read and process instructions 0.00: Fit rigid groups 0.02: 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. 0.91: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.14: Structure factors and derivatives 2.33: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.06: Apply other restraints 0.27: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0064p-1 finished at 15:35:49 Total CPU time: 5.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++