+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2005src1438 started at 16:38:30 on 01-Dec-2005 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2005src1438 in P2(1)/c CELL 0.71073 12.1544 19.3432 20.2595 90.000 104.435 90.000 ZERR 4.00 0.0003 0.0005 0.0003 0.000 0.001 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H B O F FE UNIT 180 108 4 12 96 4 V = 4612.74 F(000) = 2272.0 Mu = 0.47 mm-1 Cell Wt = 4553.30 Rho = 1.639 MERG 2 OMIT -3.00 55.00 OMIT 2 0 2 OMIT -2 2 3 SHEL 7 0.77 DFIX 31 0.02 C57 F51A C57 F52A C57 F53A C57 F51B C57 F52B C57 F53B DANG 31.6333 0.02 F51A F52A F51A F53A F52A F53A F51B F52B F51B F53B F52B F53B DELU SIMU ISOR 0.01 F51A > F53B FMAP 2 PLAN 10 SIZE 0.02 0.16 0.22 ACTA BOND $H WGHT 0.03970 5.55010 L.S. 20 TEMP -153.00 FVAR 0.35890 0.82441 1.28282 MOLE 1 C1 1 0.566738 0.956012 0.208972 11.00000 0.02590 0.02082 = 0.02698 0.00350 0.00547 -0.00325 C2 1 0.627252 0.893029 0.209489 11.00000 0.02488 0.02202 = 0.02405 -0.00217 0.01001 -0.00412 C3 1 0.646005 0.863152 0.275660 11.00000 0.01773 0.02265 = 0.02589 0.00161 0.00578 -0.00181 C4 1 0.601447 0.909877 0.317311 11.00000 0.01675 0.02836 = 0.02042 -0.00209 0.00420 -0.00493 C5 1 0.551046 0.966270 0.276307 11.00000 0.02389 0.02048 = 0.03266 -0.00480 0.00966 -0.00342 C6 1 0.534028 1.005708 0.150668 11.00000 0.04833 0.03288 = 0.04193 0.01598 0.00719 -0.00042 AFIX 137 H6A 2 0.597148 1.037571 0.151767 11.00000 -1.50000 H6B 2 0.466985 1.032012 0.154493 11.00000 -1.50000 H6C 2 0.516550 0.980058 0.107594 11.00000 -1.50000 AFIX 0 C7 1 0.670656 0.865028 0.151801 11.00000 0.04865 0.03960 = 0.03575 -0.00818 0.02459 -0.00367 AFIX 137 H7A 2 0.745662 0.884743 0.153719 11.00000 -1.50000 H7B 2 0.617987 0.877439 0.108384 11.00000 -1.50000 H7C 2 0.676706 0.814587 0.155568 11.00000 -1.50000 AFIX 0 C8 1 0.712752 0.798771 0.299741 11.00000 0.03119 0.03370 = 0.05097 0.01427 0.01158 0.01108 AFIX 137 H8A 2 0.700079 0.765071 0.262485 11.00000 -1.50000 H8B 2 0.687998 0.779060 0.338215 11.00000 -1.50000 H8C 2 0.793790 0.810117 0.314257 11.00000 -1.50000 AFIX 0 C9 1 0.613953 0.902738 0.392532 11.00000 0.02768 0.04961 = 0.02310 -0.00401 0.00609 -0.01226 AFIX 137 H9A 2 0.680509 0.928955 0.417253 11.00000 -1.50000 H9B 2 0.623759 0.853857 0.405370 11.00000 -1.50000 H9C 2 0.545763 0.920738 0.404128 11.00000 -1.50000 AFIX 0 C10 1 0.498426 1.027979 0.301304 11.00000 0.04969 0.02777 = 0.06141 -0.01229 0.02444 0.00112 AFIX 137 H10A 2 0.455184 1.012914 0.333590 11.00000 -1.50000 H10B 2 0.447401 1.051265 0.262580 11.00000 -1.50000 H10C 2 0.558327 1.060059 0.324066 11.00000 -1.50000 AFIX 0 C11 1 0.337713 0.919648 0.203078 11.00000 0.02619 0.04184 = 0.03485 0.00806 0.00583 -0.00043 C12 1 0.439465 0.809409 0.168377 11.00000 0.03557 0.04450 = 0.03378 -0.00740 0.00839 -0.01150 C13 1 0.423865 0.823441 0.297395 11.00000 0.02302 0.02439 = 0.03072 -0.00433 0.00047 -0.00591 O11 4 0.256711 0.949849 0.182283 11.00000 0.02947 0.07093 = 0.06547 0.02621 0.00727 0.01656 O12 4 0.421290 0.769918 0.125876 11.00000 0.06502 0.06467 = 0.04923 -0.03257 0.01948 -0.02719 O13 4 0.400049 0.792838 0.339499 11.00000 0.04308 0.03410 = 0.03340 0.00175 0.00923 -0.01450 FE1 6 0.470620 0.874222 0.234702 11.00000 0.01971 0.02113 = 0.02090 -0.00008 0.00298 -0.00060 MOLE 2 C21 1 -0.140251 0.740861 0.015754 11.00000 0.01828 0.01504 = 0.01648 -0.00275 0.00318 -0.00141 C22 1 -0.223201 0.787226 -0.017797 11.00000 0.02204 0.01529 = 0.01692 -0.00155 0.00308 -0.00122 AFIX 43 H22 2 -0.202304 0.823317 -0.044067 11.00000 -1.20000 AFIX 0 C23 1 -0.336593 0.782286 -0.014005 11.00000 0.01851 0.01870 = 0.01902 -0.00292 0.00055 0.00232 C24 1 -0.370565 0.731057 0.023881 11.00000 0.01456 0.02100 = 0.02116 -0.00460 0.00385 -0.00051 AFIX 43 H24 2 -0.447422 0.727558 0.026305 11.00000 -1.20000 AFIX 0 C25 1 -0.288697 0.684489 0.058567 11.00000 0.02097 0.01606 = 0.01792 -0.00182 0.00570 -0.00148 C26 1 -0.176795 0.689401 0.054447 11.00000 0.01670 0.01691 = 0.01887 -0.00020 0.00254 0.00091 AFIX 43 H26 2 -0.123008 0.656895 0.078585 11.00000 -1.20000 AFIX 0 C27 1 -0.420404 0.833885 -0.051837 11.00000 0.02360 0.02132 = 0.02740 0.00068 0.00118 0.00183 C28 1 -0.325237 0.629818 0.100600 11.00000 0.01978 0.02459 = 0.02905 0.00247 0.00812 0.00011 C31 1 0.035550 0.674329 -0.016731 11.00000 0.01745 0.01842 = 0.01561 0.00212 0.00396 -0.00236 C32 1 -0.036252 0.621447 -0.048132 11.00000 0.01475 0.02005 = 0.01535 0.00192 0.00366 -0.00039 AFIX 43 H32 2 -0.114995 0.624854 -0.050152 11.00000 -1.20000 AFIX 0 C33 1 0.002493 0.563698 -0.076742 11.00000 0.01700 0.01912 = 0.01535 0.00217 0.00326 -0.00178 C34 1 0.116746 0.556151 -0.074001 11.00000 0.01990 0.01754 = 0.02089 0.00247 0.00745 0.00135 AFIX 43 H34 2 0.143856 0.516583 -0.092828 11.00000 -1.20000 AFIX 0 C35 1 0.190581 0.607962 -0.043000 11.00000 0.01586 0.02444 = 0.02066 0.00249 0.00650 -0.00207 C36 1 0.151065 0.665976 -0.016130 11.00000 0.01623 0.02095 = 0.02018 0.00015 0.00351 -0.00447 AFIX 43 H36 2 0.203448 0.701296 0.003341 11.00000 -1.20000 AFIX 0 C37 1 -0.080340 0.511194 -0.113619 11.00000 0.01992 0.01931 = 0.02062 0.00019 0.00571 -0.00003 C38 1 0.314899 0.598019 -0.036851 11.00000 0.02041 0.02982 = 0.04207 -0.00021 0.01042 -0.00319 C41 1 0.060410 0.751207 0.098023 11.00000 0.01671 0.01839 = 0.02107 -0.00085 0.00647 -0.00537 C42 1 0.135800 0.703219 0.135832 11.00000 0.01867 0.02067 = 0.02225 0.00011 0.00480 -0.00266 AFIX 43 H42 2 0.159594 0.665267 0.113033 11.00000 -1.20000 AFIX 0 C43 1 0.177628 0.709350 0.206694 11.00000 0.01876 0.02502 = 0.02251 0.00274 0.00152 -0.00603 C44 1 0.145297 0.763743 0.241615 11.00000 0.02263 0.03151 = 0.01993 -0.00286 0.00168 -0.00707 AFIX 43 H44 2 0.172757 0.767545 0.289666 11.00000 -1.20000 AFIX 0 C45 1 0.071302 0.813012 0.204635 11.00000 0.02183 0.02661 = 0.02299 -0.00488 0.00775 -0.00508 C46 1 0.030310 0.806732 0.134944 11.00000 0.01889 0.02304 = 0.02310 -0.00149 0.00426 -0.00243 AFIX 43 H46 2 -0.019997 0.841091 0.111038 11.00000 -1.20000 AFIX 0 C47 1 0.260926 0.657219 0.244460 11.00000 0.03322 0.02718 = 0.02585 0.00024 -0.00153 -0.00246 C48 1 0.034762 0.870689 0.243026 11.00000 0.03696 0.03650 = 0.02687 -0.00817 0.00889 -0.00208 C51 1 0.023464 0.809536 -0.027897 11.00000 0.02062 0.01923 = 0.02119 -0.00083 0.00772 -0.00183 C52 1 0.101026 0.862281 -0.002570 11.00000 0.02904 0.03037 = 0.02102 -0.00199 0.00328 -0.01213 AFIX 43 H52 2 0.141368 0.861253 0.044065 11.00000 -1.20000 AFIX 0 C53 1 0.121125 0.916309 -0.043458 11.00000 0.04386 0.03354 = 0.03004 -0.00257 0.00721 -0.02319 C54 1 0.063262 0.920507 -0.111237 11.00000 0.04532 0.02873 = 0.02846 0.00381 0.01032 -0.01511 AFIX 43 H54 2 0.076074 0.957898 -0.138798 11.00000 -1.20000 AFIX 0 C55 1 -0.013622 0.869103 -0.137995 11.00000 0.03219 0.02607 = 0.02207 0.00095 0.00699 -0.00636 C56 1 -0.031259 0.814347 -0.097569 11.00000 0.02217 0.02058 = 0.02053 -0.00061 0.00462 -0.00576 AFIX 43 H56 2 -0.082363 0.778693 -0.117797 11.00000 -1.20000 AFIX 0 C57 1 0.204920 0.971484 -0.013282 11.00000 0.07943 0.05315 = 0.03817 0.00025 0.00938 -0.04830 C58 1 -0.082648 0.873710 -0.210215 11.00000 0.04354 0.03050 = 0.02514 0.00376 0.00619 -0.00836 B21 3 -0.004413 0.744113 0.016516 11.00000 0.01723 0.01776 = 0.01840 -0.00139 0.00386 -0.00184 F21 5 -0.394268 0.898197 -0.030810 11.00000 0.04863 0.01729 = 0.05263 -0.00158 -0.01335 0.00649 F22 5 -0.427623 0.833238 -0.118634 11.00000 0.05851 0.05183 = 0.02522 0.00433 -0.00232 0.02652 F23 5 -0.525778 0.822923 -0.045847 11.00000 0.02284 0.04660 = 0.07986 0.02181 0.00907 0.01134 F24 5 -0.371423 0.656939 0.148436 11.00000 0.07319 0.03944 = 0.06438 0.01622 0.05581 0.01545 F25 5 -0.403840 0.587917 0.062620 11.00000 0.04101 0.04474 = 0.05100 0.01888 -0.00948 -0.02583 F26 5 -0.241816 0.588867 0.133273 11.00000 0.02759 0.02930 = 0.03281 0.01235 0.00733 0.00146 F31 5 -0.145901 0.536304 -0.172170 11.00000 0.03910 0.03026 = 0.02727 0.00552 -0.01047 -0.01223 F32 5 -0.153308 0.490431 -0.077744 11.00000 0.03202 0.03245 = 0.03440 -0.00437 0.01403 -0.01536 F33 5 -0.030982 0.454417 -0.129513 11.00000 0.02610 0.02679 = 0.05650 -0.01864 0.00741 -0.00046 F34 5 0.335972 0.573868 -0.094538 11.00000 0.02915 0.05371 = 0.06527 -0.02055 0.02791 -0.00510 F35 5 0.360546 0.551719 0.011209 11.00000 0.02232 0.05875 = 0.07855 0.02937 0.00628 0.00964 F36 5 0.374653 0.656104 -0.021905 11.00000 0.01881 0.03742 = 0.06867 -0.01093 0.01379 -0.00891 F41 5 0.243731 0.593932 0.218993 11.00000 0.05515 0.02259 = 0.06113 0.00121 -0.02452 -0.00116 F42 5 0.368217 0.672715 0.242703 11.00000 0.02757 0.03399 = 0.05669 0.00017 -0.00205 0.00352 F43 5 0.264048 0.654316 0.310798 11.00000 0.06062 0.06631 = 0.03126 0.01914 0.00430 0.01584 F44 5 -0.021448 0.847837 0.287394 11.00000 0.07276 0.05346 = 0.07252 -0.02409 0.05530 -0.01402 F45 5 -0.031576 0.916759 0.203029 11.00000 0.08851 0.05317 = 0.04341 -0.01738 0.00154 0.03585 F46 5 0.122326 0.906714 0.280112 11.00000 0.05504 0.04960 = 0.04519 -0.02805 0.01607 -0.01567 PART 1 F51A 5 0.298929 0.945656 0.028828 21.00000 0.06008 0.09744 = 0.07810 -0.01165 -0.00558 -0.05524 F52A 5 0.166935 1.013756 0.026286 21.00000 0.10873 0.05663 = 0.10743 -0.04287 0.00769 -0.03852 F53A 5 0.242063 1.006679 -0.058722 21.00000 0.16787 0.14816 = 0.04222 0.00905 0.00963 -0.14100 PART 2 F51B 5 0.218951 0.985533 0.048114 -21.00000 0.15466 0.16065 = 0.02621 -0.01366 0.01268 -0.12850 F52B 5 0.168650 1.033785 -0.043608 -21.00000 0.07229 0.03361 = 0.09265 0.01419 -0.02775 -0.04684 F53B 5 0.301216 0.961798 -0.025531 -21.00000 0.04869 0.11745 = 0.19449 -0.08448 0.03888 -0.04906 PART 0 F54 5 -0.041531 0.916651 -0.247515 11.00000 0.14568 0.12287 = 0.03071 0.03472 -0.01736 -0.09875 F55 5 -0.188774 0.892301 -0.213628 11.00000 0.07242 0.12549 = 0.03483 -0.00531 -0.00790 0.05586 F56 5 -0.093857 0.813527 -0.242502 11.00000 0.06996 0.05160 = 0.02839 -0.00829 -0.00378 0.00476 HKLF 4 Covalent radii and connectivity table for 2005src1438 in P2(1)/c C 0.770 H 0.320 B 0.820 O 0.660 F 0.640 FE 1.240 C1 - C2 C5 C6 Fe1 C2 - C1 C3 C7 Fe1 C3 - C2 C4 C8 Fe1 C4 - C5 C3 C9 Fe1 C5 - C4 C1 C10 Fe1 C6 - C1 C7 - C2 C8 - C3 C9 - C4 C10 - C5 C11 - O11 Fe1 C12 - O12 Fe1 C13 - O13 Fe1 O11 - C11 O12 - C12 O13 - C13 Fe1 - C13 C12 C11 C3 C5 C1 C4 C2 C21 - C22 C26 B21 C22 - C21 C23 C23 - C24 C22 C27 C24 - C23 C25 C25 - C26 C24 C28 C26 - C25 C21 C27 - F21 F23 F22 C23 C28 - F26 F25 F24 C25 C31 - C32 C36 B21 C32 - C31 C33 C33 - C34 C32 C37 C34 - C33 C35 C35 - C36 C34 C38 C36 - C35 C31 C37 - F33 F32 F31 C33 C38 - F36 F35 F34 C35 C41 - C42 C46 B21 C42 - C41 C43 C43 - C44 C42 C47 C44 - C43 C45 C45 - C46 C44 C48 C46 - C45 C41 C47 - F41 F43 F42 C43 C48 - F45 F44 F46 C45 C51 - C52 C56 B21 C52 - C53 C51 C53 - C54 C52 C57 C54 - C55 C53 C55 - C54 C56 C58 C56 - C55 C51 C57 - F51B_b F53B_b F52A_a F53A_a F51A_a F52B_b C53 C58 - F54 F55 F56 C55 B21 - C31 C51 C21 C41 F21 - C27 F22 - C27 F23 - C27 F24 - C28 F25 - C28 F26 - C28 F31 - C37 F32 - C37 F33 - C37 F34 - C38 F35 - C38 F36 - C38 F41 - C47 F42 - C47 F43 - C47 F44 - C48 F45 - C48 F46 - C48 F51A_a - C57 F52A_a - C57 F53A_a - C57 F51B_b - C57 F52B_b - C57 F53B_b - C57 F54 - C58 F55 - C58 F56 - C58 h k l Fo^2 Sigma Why rejected 0 11 0 36.90 9.11 observed but should be systematically absent 7 0 7 31.79 7.22 observed but should be systematically absent 0 0 9 6.36 1.40 observed but should be systematically absent 0 0 11 57.51 12.48 observed but should be systematically absent 0 0 11 63.43 13.82 observed but should be systematically absent 0 0 11 41.89 8.88 observed but should be systematically absent 0 0 11 33.60 8.25 observed but should be systematically absent 0 0 13 94.00 17.59 observed but should be systematically absent 0 0 13 110.05 21.38 observed but should be systematically absent 0 0 13 152.03 28.65 observed but should be systematically absent 0 0 13 155.97 24.03 observed but should be systematically absent 0 0 15 16.38 2.03 observed but should be systematically absent 0 0 15 20.31 2.96 observed but should be systematically absent 0 0 15 16.40 1.59 observed but should be systematically absent 57642 Reflections read, of which 1101 rejected -15 =< h =< 15, -25 =< k =< 25, -26 =< l =< 26, Max. 2-theta = 54.97 14 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 0 1 17 0.11 0.12 5 1.11 1 Inconsistent equivalents 10558 Unique reflections, of which 0 suppressed R(int) = 0.0523 R(sigma) = 0.0415 Friedel opposites merged Maximum memory for data reduction = 6542 / 105526 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 = 8323 / 988914 wR2 = 0.1143 before cycle 1 for 10558 data and 701 / 701 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint 1.3744 1.2828 0.0916 0.0200 DFIX C57 F52B_b 2.0326 2.0952 -0.0626 0.0200 DANG F51B_b F52B_b -0.0361 0.0100 DELU C57 F53B_b 0.0552 0.0100 ISOR U12 F51A_a 0.0377 0.0100 ISOR U22 F52A_a 0.0429 0.0100 ISOR U23 F52A_a 0.0385 0.0100 ISOR U12 F52A_a -0.0455 0.0100 ISOR U11 F53A_a 0.0801 0.0100 ISOR U33 F53A_a 0.1410 0.0100 ISOR U12 F53A_a -0.0391 0.0100 ISOR U11 F51B_b -0.0451 0.0100 ISOR U22 F51B_b 0.0894 0.0100 ISOR U33 F51B_b 0.1285 0.0100 ISOR U12 F51B_b 0.0411 0.0100 ISOR U22 F52B_b 0.0464 0.0100 ISOR U13 F52B_b 0.0468 0.0100 ISOR U12 F52B_b 0.0700 0.0100 ISOR U11 F53B_b -0.0758 0.0100 ISOR U33 F53B_b 0.0845 0.0100 ISOR U23 F53B_b 0.0491 0.0100 ISOR U12 F53B_b Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 6. 6. 0. 0. 0. 0. 253. 492. 36. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.010 0.063 0.010 0.000 rms deviation 0.000 0.050 0.041 0.000 0.000 0.000 0.000 0.005 0.028 0.051 0.000 GooF = S = 1.021; Restrained GooF = 1.033 for 793 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0397 * P )^2 + 5.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.35888 0.00041 -0.039 OSF 2 0.84428 0.00675 2.942 FVAR 2 3 1.28841 0.00543 1.030 FVAR 3 651 0.09181 0.01004 -6.261 U11 F51B_b 652 0.09173 0.00990 -6.962 U22 F51B_b 656 -0.06310 0.00762 8.585 U12 F51B_b 660 0.04870 0.00711 -3.317 U11 F52B_b 662 0.06546 0.00817 -3.326 U33 F52B_b 665 -0.03002 0.00461 3.644 U12 F52B_b 670 0.07925 0.00905 -4.220 U22 F53B_b 671 0.10880 0.01108 -7.733 U33 F53B_b 672 -0.02874 0.00831 6.707 U23 F53B_b 674 -0.02842 0.00542 3.811 U12 F53B_b Mean shift/esd = 0.179 Maximum = 8.585 for U12 F51B_b Max. shift = 0.060 A for F53B_b Max. dU =-0.041 for F51B_b Least-squares cycle 2 Maximum vector length = 511 Memory required = 8323 / 988914 wR2 = 0.1149 before cycle 2 for 10558 data and 701 / 701 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint 1.3904 1.2884 0.1020 0.0200 DFIX C57 F52B_b -0.0326 0.0100 DELU C57 F53B_b -0.0304 0.0100 DELU C57 F52B_b 0.0534 0.0100 ISOR U12 F51A_a 0.0373 0.0100 ISOR U22 F52A_a 0.0421 0.0100 ISOR U23 F52A_a 0.0370 0.0100 ISOR U12 F52A_a -0.0444 0.0100 ISOR U11 F53A_a 0.0726 0.0100 ISOR U33 F53A_a 0.1322 0.0100 ISOR U12 F53A_a 0.0391 0.0100 ISOR U33 F51B_b 0.0631 0.0100 ISOR U12 F51B_b 0.0300 0.0100 ISOR U12 F52B_b 0.0318 0.0100 ISOR U11 F53B_b -0.0305 0.0100 ISOR U33 F53B_b Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 6. 6. 0. 0. 0. 0. 253. 492. 36. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.010 0.063 0.010 0.000 rms deviation 0.000 0.055 0.038 0.000 0.000 0.000 0.000 0.005 0.023 0.036 0.000 GooF = S = 1.026; Restrained GooF = 1.017 for 793 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0397 * P )^2 + 5.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.35888 0.00040 -0.015 OSF 2 0.85092 0.00578 1.149 FVAR 2 3 1.28811 0.00531 -0.056 FVAR 3 656 -0.04129 0.00698 3.125 U12 F51B_b Mean shift/esd = 0.052 Maximum = 3.125 for U12 F51B_b Max. shift = 0.022 A for F51B_b Max. dU =-0.007 for F51B_b Least-squares cycle 3 Maximum vector length = 511 Memory required = 8323 / 988914 wR2 = 0.1150 before cycle 3 for 10558 data and 701 / 701 parameters Disagreeable restraints before cycle 3 Observed Target Error Sigma Restraint 1.2266 1.2881 -0.0615 0.0200 DFIX C57 F51B_b 1.3886 1.2881 0.1005 0.0200 DFIX C57 F52B_b -0.0324 0.0100 DELU C57 F53B_b -0.0301 0.0100 DELU C57 F52B_b 0.0526 0.0100 ISOR U12 F51A_a 0.0373 0.0100 ISOR U22 F52A_a 0.0425 0.0100 ISOR U23 F52A_a 0.0360 0.0100 ISOR U12 F52A_a -0.0446 0.0100 ISOR U11 F53A_a 0.0727 0.0100 ISOR U33 F53A_a 0.1326 0.0100 ISOR U12 F53A_a 0.0413 0.0100 ISOR U12 F51B_b 0.0301 0.0100 ISOR U12 F52B_b Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 6. 6. 0. 0. 0. 0. 253. 492. 36. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.010 0.063 0.010 0.000 rms deviation 0.000 0.055 0.039 0.000 0.000 0.000 0.000 0.005 0.022 0.035 0.000 GooF = S = 1.027; Restrained GooF = 1.016 for 793 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0397 * P )^2 + 5.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.35888 0.00040 -0.003 OSF 2 0.85304 0.00570 0.370 FVAR 2 3 1.28826 0.00535 0.027 FVAR 3 Mean shift/esd = 0.022 Maximum = -0.629 for y F52A_a Max. shift = 0.009 A for F51B_b Max. dU = 0.001 for F53A_a Least-squares cycle 4 Maximum vector length = 511 Memory required = 8323 / 988914 wR2 = 0.1150 before cycle 4 for 10558 data and 701 / 701 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint 1.3863 1.2883 0.0980 0.0200 DFIX C57 F52B_b -0.0332 0.0100 DELU C57 F53B_b 0.0526 0.0100 ISOR U12 F51A_a 0.0373 0.0100 ISOR U22 F52A_a 0.0432 0.0100 ISOR U23 F52A_a 0.0363 0.0100 ISOR U12 F52A_a -0.0455 0.0100 ISOR U11 F53A_a 0.0736 0.0100 ISOR U33 F53A_a 0.1336 0.0100 ISOR U12 F53A_a 0.0423 0.0100 ISOR U12 F51B_b 0.0300 0.0100 ISOR U12 F52B_b Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 6. 6. 0. 0. 0. 0. 253. 492. 36. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.010 0.063 0.010 0.000 rms deviation 0.000 0.053 0.037 0.000 0.000 0.000 0.000 0.005 0.023 0.035 0.000 GooF = S = 1.027; Restrained GooF = 1.015 for 793 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0397 * P )^2 + 5.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.35888 0.00040 -0.004 OSF 2 0.85362 0.00565 0.103 FVAR 2 3 1.28860 0.00536 0.063 FVAR 3 Mean shift/esd = 0.009 Maximum = -0.315 for z F53B_b Max. shift = 0.008 A for F53B_b Max. dU = 0.000 for F51B_b Least-squares cycle 5 Maximum vector length = 511 Memory required = 8323 / 988914 wR2 = 0.1150 before cycle 5 for 10558 data and 701 / 701 parameters Disagreeable restraints before cycle 5 Observed Target Error Sigma Restraint 1.3855 1.2886 0.0969 0.0200 DFIX C57 F52B_b -0.0333 0.0100 DELU C57 F53B_b 0.0526 0.0100 ISOR U12 F51A_a 0.0372 0.0100 ISOR U22 F52A_a 0.0431 0.0100 ISOR U23 F52A_a 0.0366 0.0100 ISOR U12 F52A_a -0.0455 0.0100 ISOR U11 F53A_a 0.0736 0.0100 ISOR U33 F53A_a 0.1337 0.0100 ISOR U12 F53A_a 0.0423 0.0100 ISOR U12 F51B_b Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 6. 6. 0. 0. 0. 0. 253. 492. 36. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.010 0.063 0.010 0.000 rms deviation 0.000 0.053 0.036 0.000 0.000 0.000 0.000 0.005 0.023 0.035 0.000 GooF = S = 1.026; Restrained GooF = 1.015 for 793 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0397 * P )^2 + 5.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.35888 0.00040 -0.002 OSF 2 0.85405 0.00562 0.076 FVAR 2 3 1.28866 0.00537 0.011 FVAR 3 Mean shift/esd = 0.007 Maximum = -0.236 for z F53B_b Max. shift = 0.006 A for F53B_b Max. dU = 0.000 for F53B_b Least-squares cycle 6 Maximum vector length = 511 Memory required = 8323 / 988914 wR2 = 0.1150 before cycle 6 for 10558 data and 701 / 701 parameters Disagreeable restraints before cycle 6 Observed Target Error Sigma Restraint 1.3857 1.2887 0.0971 0.0200 DFIX C57 F52B_b -0.0334 0.0100 DELU C57 F53B_b 0.0524 0.0100 ISOR U12 F51A_a 0.0372 0.0100 ISOR U22 F52A_a 0.0431 0.0100 ISOR U23 F52A_a 0.0367 0.0100 ISOR U12 F52A_a -0.0457 0.0100 ISOR U11 F53A_a 0.0737 0.0100 ISOR U33 F53A_a 0.1338 0.0100 ISOR U12 F53A_a 0.0422 0.0100 ISOR U12 F51B_b Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 6. 6. 0. 0. 0. 0. 253. 492. 36. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.010 0.063 0.010 0.000 rms deviation 0.000 0.053 0.036 0.000 0.000 0.000 0.000 0.005 0.023 0.035 0.000 GooF = S = 1.027; Restrained GooF = 1.015 for 793 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0397 * P )^2 + 5.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.35888 0.00040 0.001 OSF 2 0.85426 0.00560 0.038 FVAR 2 3 1.28868 0.00537 0.005 FVAR 3 Mean shift/esd = 0.005 Maximum = -0.177 for z F53B_b Max. shift = 0.004 A for F53B_b Max. dU = 0.000 for F53B_b Least-squares cycle 7 Maximum vector length = 511 Memory required = 8323 / 988914 wR2 = 0.1150 before cycle 7 for 10558 data and 701 / 701 parameters Disagreeable restraints before cycle 7 Observed Target Error Sigma Restraint 1.3857 1.2887 0.0970 0.0200 DFIX C57 F52B_b -0.0336 0.0100 DELU C57 F53B_b 0.0524 0.0100 ISOR U12 F51A_a 0.0371 0.0100 ISOR U22 F52A_a 0.0431 0.0100 ISOR U23 F52A_a 0.0367 0.0100 ISOR U12 F52A_a -0.0458 0.0100 ISOR U11 F53A_a 0.0738 0.0100 ISOR U33 F53A_a 0.1338 0.0100 ISOR U12 F53A_a 0.0421 0.0100 ISOR U12 F51B_b Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 6. 6. 0. 0. 0. 0. 253. 492. 36. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.010 0.063 0.010 0.000 rms deviation 0.000 0.053 0.036 0.000 0.000 0.000 0.000 0.005 0.023 0.035 0.000 GooF = S = 1.027; Restrained GooF = 1.015 for 793 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0397 * P )^2 + 5.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.35888 0.00040 0.000 OSF 2 0.85446 0.00559 0.035 FVAR 2 3 1.28870 0.00537 0.003 FVAR 3 Mean shift/esd = 0.003 Maximum = -0.140 for z F53B_b Max. shift = 0.003 A for F53B_b Max. dU = 0.000 for F53B_b Least-squares cycle 8 Maximum vector length = 511 Memory required = 8323 / 988914 wR2 = 0.1150 before cycle 8 for 10558 data and 701 / 701 parameters Disagreeable restraints before cycle 8 Observed Target Error Sigma Restraint 1.3857 1.2887 0.0970 0.0200 DFIX C57 F52B_b -0.0337 0.0100 DELU C57 F53B_b 0.0523 0.0100 ISOR U12 F51A_a 0.0371 0.0100 ISOR U22 F52A_a 0.0431 0.0100 ISOR U23 F52A_a 0.0367 0.0100 ISOR U12 F52A_a -0.0459 0.0100 ISOR U11 F53A_a 0.0738 0.0100 ISOR U33 F53A_a 0.1339 0.0100 ISOR U12 F53A_a 0.0421 0.0100 ISOR U12 F51B_b Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 6. 6. 0. 0. 0. 0. 253. 492. 36. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.010 0.063 0.010 0.000 rms deviation 0.000 0.053 0.036 0.000 0.000 0.000 0.000 0.005 0.023 0.035 0.000 GooF = S = 1.027; Restrained GooF = 1.015 for 793 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0397 * P )^2 + 5.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.35887 0.00040 -0.002 OSF 2 0.85459 0.00558 0.024 FVAR 2 3 1.28871 0.00537 0.001 FVAR 3 Mean shift/esd = 0.003 Maximum = -0.106 for z F53B_b Max. shift = 0.003 A for F53B_b Max. dU = 0.000 for F53B_b Least-squares cycle 9 Maximum vector length = 511 Memory required = 8323 / 988914 wR2 = 0.1150 before cycle 9 for 10558 data and 701 / 701 parameters Disagreeable restraints before cycle 9 Observed Target Error Sigma Restraint 1.3857 1.2887 0.0970 0.0200 DFIX C57 F52B_b -0.0338 0.0100 DELU C57 F53B_b 0.0523 0.0100 ISOR U12 F51A_a 0.0371 0.0100 ISOR U22 F52A_a 0.0431 0.0100 ISOR U23 F52A_a 0.0368 0.0100 ISOR U12 F52A_a -0.0460 0.0100 ISOR U11 F53A_a 0.0738 0.0100 ISOR U33 F53A_a 0.1339 0.0100 ISOR U12 F53A_a 0.0421 0.0100 ISOR U12 F51B_b Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 6. 6. 0. 0. 0. 0. 253. 492. 36. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.010 0.063 0.010 0.000 rms deviation 0.000 0.053 0.035 0.000 0.000 0.000 0.000 0.005 0.023 0.035 0.000 GooF = S = 1.027; Restrained GooF = 1.015 for 793 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0397 * P )^2 + 5.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.35887 0.00040 0.001 OSF 2 0.85470 0.00557 0.018 FVAR 2 3 1.28871 0.00537 0.001 FVAR 3 Mean shift/esd = 0.002 Maximum = -0.080 for z F53B_b Max. shift = 0.002 A for F53B_b Max. dU = 0.000 for F53B_b Least-squares cycle 10 Maximum vector length = 511 Memory required = 8323 / 988914 wR2 = 0.1150 before cycle 10 for 10558 data and 701 / 701 parameters Disagreeable restraints before cycle 10 Observed Target Error Sigma Restraint 1.3857 1.2887 0.0970 0.0200 DFIX C57 F52B_b -0.0339 0.0100 DELU C57 F53B_b 0.0523 0.0100 ISOR U12 F51A_a 0.0370 0.0100 ISOR U22 F52A_a 0.0431 0.0100 ISOR U23 F52A_a 0.0368 0.0100 ISOR U12 F52A_a -0.0460 0.0100 ISOR U11 F53A_a 0.0739 0.0100 ISOR U33 F53A_a 0.1339 0.0100 ISOR U12 F53A_a 0.0421 0.0100 ISOR U12 F51B_b Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 6. 6. 0. 0. 0. 0. 253. 492. 36. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.010 0.063 0.010 0.000 rms deviation 0.000 0.053 0.035 0.000 0.000 0.000 0.000 0.005 0.023 0.035 0.000 GooF = S = 1.027; Restrained GooF = 1.015 for 793 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0397 * P )^2 + 5.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.35887 0.00040 -0.001 OSF 2 0.85477 0.00556 0.014 FVAR 2 3 1.28871 0.00537 0.000 FVAR 3 Mean shift/esd = 0.001 Maximum = -0.061 for z F53B_b Max. shift = 0.001 A for F53B_b Max. dU = 0.000 for F53B_b Least-squares cycle 11 Maximum vector length = 511 Memory required = 8323 / 988914 wR2 = 0.1150 before cycle 11 for 10558 data and 701 / 701 parameters Disagreeable restraints before cycle 11 Observed Target Error Sigma Restraint 1.3857 1.2887 0.0970 0.0200 DFIX C57 F52B_b -0.0340 0.0100 DELU C57 F53B_b 0.0523 0.0100 ISOR U12 F51A_a 0.0370 0.0100 ISOR U22 F52A_a 0.0431 0.0100 ISOR U23 F52A_a 0.0368 0.0100 ISOR U12 F52A_a -0.0461 0.0100 ISOR U11 F53A_a 0.0739 0.0100 ISOR U33 F53A_a 0.1339 0.0100 ISOR U12 F53A_a 0.0421 0.0100 ISOR U12 F51B_b Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 6. 6. 0. 0. 0. 0. 253. 492. 36. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.010 0.063 0.010 0.000 rms deviation 0.000 0.053 0.035 0.000 0.000 0.000 0.000 0.005 0.023 0.035 0.000 GooF = S = 1.027; Restrained GooF = 1.015 for 793 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0397 * P )^2 + 5.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.35887 0.00040 0.000 OSF 2 0.85483 0.00556 0.010 FVAR 2 3 1.28872 0.00537 0.001 FVAR 3 Mean shift/esd = 0.001 Maximum = -0.047 for z F53B_b Max. shift = 0.001 A for F53B_b Max. dU = 0.000 for F53B_b Least-squares cycle 12 Maximum vector length = 511 Memory required = 8323 / 988914 wR2 = 0.1150 before cycle 12 for 10558 data and 701 / 701 parameters Disagreeable restraints before cycle 12 Observed Target Error Sigma Restraint 1.3857 1.2887 0.0970 0.0200 DFIX C57 F52B_b -0.0340 0.0100 DELU C57 F53B_b 0.0522 0.0100 ISOR U12 F51A_a 0.0370 0.0100 ISOR U22 F52A_a 0.0431 0.0100 ISOR U23 F52A_a 0.0368 0.0100 ISOR U12 F52A_a -0.0461 0.0100 ISOR U11 F53A_a 0.0739 0.0100 ISOR U33 F53A_a 0.1340 0.0100 ISOR U12 F53A_a 0.0420 0.0100 ISOR U12 F51B_b Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 6. 6. 0. 0. 0. 0. 253. 492. 36. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.010 0.063 0.010 0.000 rms deviation 0.000 0.053 0.035 0.000 0.000 0.000 0.000 0.005 0.023 0.035 0.000 GooF = S = 1.027; Restrained GooF = 1.015 for 793 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0397 * P )^2 + 5.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.35887 0.00040 -0.001 OSF 2 0.85488 0.00555 0.008 FVAR 2 3 1.28872 0.00537 0.000 FVAR 3 Mean shift/esd = 0.001 Maximum = -0.035 for z F53B_b Max. shift = 0.001 A for F53B_b Max. dU = 0.000 for F53B_b Least-squares cycle 13 Maximum vector length = 511 Memory required = 8323 / 988914 wR2 = 0.1150 before cycle 13 for 10558 data and 701 / 701 parameters Disagreeable restraints before cycle 13 Observed Target Error Sigma Restraint 1.3857 1.2887 0.0970 0.0200 DFIX C57 F52B_b -0.0340 0.0100 DELU C57 F53B_b 0.0522 0.0100 ISOR U12 F51A_a 0.0370 0.0100 ISOR U22 F52A_a 0.0431 0.0100 ISOR U23 F52A_a 0.0368 0.0100 ISOR U12 F52A_a -0.0461 0.0100 ISOR U11 F53A_a 0.0739 0.0100 ISOR U33 F53A_a 0.1340 0.0100 ISOR U12 F53A_a 0.0420 0.0100 ISOR U12 F51B_b Summary of restraints applied in cycle 13 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 6. 6. 0. 0. 0. 0. 253. 492. 36. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.010 0.063 0.010 0.000 rms deviation 0.000 0.053 0.035 0.000 0.000 0.000 0.000 0.005 0.023 0.035 0.000 GooF = S = 1.027; Restrained GooF = 1.015 for 793 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0397 * P )^2 + 5.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.35887 0.00040 -0.002 OSF 2 0.85491 0.00555 0.006 FVAR 2 3 1.28872 0.00537 0.000 FVAR 3 Mean shift/esd = 0.001 Maximum = -0.027 for z F53B_b Max. shift = 0.001 A for F53B_b Max. dU = 0.000 for F53B_b Least-squares cycle 14 Maximum vector length = 511 Memory required = 8323 / 988914 wR2 = 0.1150 before cycle 14 for 10558 data and 701 / 701 parameters Disagreeable restraints before cycle 14 Observed Target Error Sigma Restraint 1.3857 1.2887 0.0970 0.0200 DFIX C57 F52B_b -0.0341 0.0100 DELU C57 F53B_b 0.0522 0.0100 ISOR U12 F51A_a 0.0370 0.0100 ISOR U22 F52A_a 0.0431 0.0100 ISOR U23 F52A_a 0.0368 0.0100 ISOR U12 F52A_a -0.0462 0.0100 ISOR U11 F53A_a 0.0739 0.0100 ISOR U33 F53A_a 0.1340 0.0100 ISOR U12 F53A_a 0.0420 0.0100 ISOR U12 F51B_b Summary of restraints applied in cycle 14 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 6. 6. 0. 0. 0. 0. 253. 492. 36. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.010 0.063 0.010 0.000 rms deviation 0.000 0.053 0.035 0.000 0.000 0.000 0.000 0.005 0.023 0.035 0.000 GooF = S = 1.027; Restrained GooF = 1.015 for 793 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0397 * P )^2 + 5.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.35887 0.00040 0.001 OSF 2 0.85493 0.00555 0.004 FVAR 2 3 1.28872 0.00537 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = -0.020 for z F53B_b Max. shift = 0.000 A for F53B_b Max. dU = 0.000 for F53B_b Least-squares cycle 15 Maximum vector length = 511 Memory required = 8323 / 988914 wR2 = 0.1150 before cycle 15 for 10558 data and 701 / 701 parameters Disagreeable restraints before cycle 15 Observed Target Error Sigma Restraint 1.3857 1.2887 0.0970 0.0200 DFIX C57 F52B_b -0.0341 0.0100 DELU C57 F53B_b 0.0522 0.0100 ISOR U12 F51A_a 0.0370 0.0100 ISOR U22 F52A_a 0.0431 0.0100 ISOR U23 F52A_a 0.0368 0.0100 ISOR U12 F52A_a -0.0462 0.0100 ISOR U11 F53A_a 0.0739 0.0100 ISOR U33 F53A_a 0.1340 0.0100 ISOR U12 F53A_a 0.0420 0.0100 ISOR U12 F51B_b Summary of restraints applied in cycle 15 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 6. 6. 0. 0. 0. 0. 253. 492. 36. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.010 0.063 0.010 0.000 rms deviation 0.000 0.053 0.035 0.000 0.000 0.000 0.000 0.005 0.023 0.035 0.000 GooF = S = 1.027; Restrained GooF = 1.015 for 793 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0397 * P )^2 + 5.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.35887 0.00040 0.000 OSF 2 0.85495 0.00555 0.003 FVAR 2 3 1.28872 0.00537 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = -0.015 for z F53B_b Max. shift = 0.000 A for F53B_b Max. dU = 0.000 for F53B_b Least-squares cycle 16 Maximum vector length = 511 Memory required = 8323 / 988914 wR2 = 0.1150 before cycle 16 for 10558 data and 701 / 701 parameters Disagreeable restraints before cycle 16 Observed Target Error Sigma Restraint 1.3857 1.2887 0.0970 0.0200 DFIX C57 F52B_b -0.0341 0.0100 DELU C57 F53B_b 0.0522 0.0100 ISOR U12 F51A_a 0.0370 0.0100 ISOR U22 F52A_a 0.0431 0.0100 ISOR U23 F52A_a 0.0369 0.0100 ISOR U12 F52A_a -0.0462 0.0100 ISOR U11 F53A_a 0.0739 0.0100 ISOR U33 F53A_a 0.1340 0.0100 ISOR U12 F53A_a 0.0420 0.0100 ISOR U12 F51B_b Summary of restraints applied in cycle 16 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 6. 6. 0. 0. 0. 0. 253. 492. 36. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.010 0.063 0.010 0.000 rms deviation 0.000 0.053 0.035 0.000 0.000 0.000 0.000 0.005 0.023 0.035 0.000 GooF = S = 1.027; Restrained GooF = 1.015 for 793 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0397 * P )^2 + 5.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.35887 0.00040 0.000 OSF 2 0.85496 0.00555 0.002 FVAR 2 3 1.28872 0.00537 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = -0.012 for z F53B_b Max. shift = 0.000 A for F53B_b Max. dU = 0.000 for F53B_b Least-squares cycle 17 Maximum vector length = 511 Memory required = 8323 / 988914 wR2 = 0.1150 before cycle 17 for 10558 data and 701 / 701 parameters Disagreeable restraints before cycle 17 Observed Target Error Sigma Restraint 1.3857 1.2887 0.0969 0.0200 DFIX C57 F52B_b -0.0341 0.0100 DELU C57 F53B_b 0.0522 0.0100 ISOR U12 F51A_a 0.0370 0.0100 ISOR U22 F52A_a 0.0431 0.0100 ISOR U23 F52A_a 0.0369 0.0100 ISOR U12 F52A_a -0.0462 0.0100 ISOR U11 F53A_a 0.0739 0.0100 ISOR U33 F53A_a 0.1340 0.0100 ISOR U12 F53A_a 0.0420 0.0100 ISOR U12 F51B_b Summary of restraints applied in cycle 17 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 6. 6. 0. 0. 0. 0. 253. 492. 36. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.010 0.063 0.010 0.000 rms deviation 0.000 0.053 0.035 0.000 0.000 0.000 0.000 0.005 0.023 0.035 0.000 GooF = S = 1.027; Restrained GooF = 1.016 for 793 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0397 * P )^2 + 5.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.35887 0.00040 0.000 OSF 2 0.85498 0.00555 0.002 FVAR 2 3 1.28872 0.00537 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = -0.009 for z F53B_b Max. shift = 0.000 A for F53B_b Max. dU = 0.000 for F53B_b Least-squares cycle 18 Maximum vector length = 511 Memory required = 8323 / 988914 wR2 = 0.1150 before cycle 18 for 10558 data and 701 / 701 parameters Disagreeable restraints before cycle 18 Observed Target Error Sigma Restraint 1.3857 1.2887 0.0969 0.0200 DFIX C57 F52B_b -0.0341 0.0100 DELU C57 F53B_b 0.0522 0.0100 ISOR U12 F51A_a 0.0370 0.0100 ISOR U22 F52A_a 0.0431 0.0100 ISOR U23 F52A_a 0.0369 0.0100 ISOR U12 F52A_a -0.0462 0.0100 ISOR U11 F53A_a 0.0739 0.0100 ISOR U33 F53A_a 0.1340 0.0100 ISOR U12 F53A_a 0.0420 0.0100 ISOR U12 F51B_b Summary of restraints applied in cycle 18 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 6. 6. 0. 0. 0. 0. 253. 492. 36. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.010 0.063 0.010 0.000 rms deviation 0.000 0.053 0.035 0.000 0.000 0.000 0.000 0.005 0.023 0.035 0.000 GooF = S = 1.027; Restrained GooF = 1.016 for 793 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0397 * P )^2 + 5.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.35887 0.00040 0.000 OSF 2 0.85498 0.00555 0.002 FVAR 2 3 1.28873 0.00537 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = -0.007 for z F53B_b Max. shift = 0.000 A for F53B_b Max. dU = 0.000 for F53B_b Least-squares cycle 19 Maximum vector length = 511 Memory required = 8323 / 988914 wR2 = 0.1150 before cycle 19 for 10558 data and 701 / 701 parameters Disagreeable restraints before cycle 19 Observed Target Error Sigma Restraint 1.3857 1.2887 0.0969 0.0200 DFIX C57 F52B_b -0.0341 0.0100 DELU C57 F53B_b 0.0522 0.0100 ISOR U12 F51A_a 0.0370 0.0100 ISOR U22 F52A_a 0.0431 0.0100 ISOR U23 F52A_a 0.0369 0.0100 ISOR U12 F52A_a -0.0462 0.0100 ISOR U11 F53A_a 0.0739 0.0100 ISOR U33 F53A_a 0.1340 0.0100 ISOR U12 F53A_a 0.0420 0.0100 ISOR U12 F51B_b Summary of restraints applied in cycle 19 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 6. 6. 0. 0. 0. 0. 253. 492. 36. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.010 0.063 0.010 0.000 rms deviation 0.000 0.053 0.035 0.000 0.000 0.000 0.000 0.005 0.023 0.035 0.000 GooF = S = 1.027; Restrained GooF = 1.015 for 793 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0397 * P )^2 + 5.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.35887 0.00040 0.001 OSF 2 0.85499 0.00555 0.001 FVAR 2 3 1.28872 0.00537 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = -0.005 for z F53B_b Max. shift = 0.000 A for F53B_b Max. dU = 0.000 for F53B_b Least-squares cycle 20 Maximum vector length = 511 Memory required = 8323 / 988914 wR2 = 0.1150 before cycle 20 for 10558 data and 701 / 701 parameters Disagreeable restraints before cycle 20 Observed Target Error Sigma Restraint 1.3857 1.2887 0.0969 0.0200 DFIX C57 F52B_b -0.0341 0.0100 DELU C57 F53B_b 0.0522 0.0100 ISOR U12 F51A_a 0.0370 0.0100 ISOR U22 F52A_a 0.0431 0.0100 ISOR U23 F52A_a 0.0369 0.0100 ISOR U12 F52A_a -0.0462 0.0100 ISOR U11 F53A_a 0.0739 0.0100 ISOR U33 F53A_a 0.1340 0.0100 ISOR U12 F53A_a 0.0420 0.0100 ISOR U12 F51B_b Summary of restraints applied in cycle 20 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 6. 6. 0. 0. 0. 0. 253. 492. 36. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.010 0.063 0.010 0.000 rms deviation 0.000 0.053 0.035 0.000 0.000 0.000 0.000 0.005 0.023 0.035 0.000 GooF = S = 1.027; Restrained GooF = 1.016 for 793 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0397 * P )^2 + 5.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.35887 0.00040 0.000 OSF 2 0.85499 0.00555 0.001 FVAR 2 3 1.28873 0.00537 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = -0.004 for z F53B_b Max. shift = 0.000 A for F53B_b Max. dU = 0.000 for F53B_b Largest correlation matrix elements -0.769 U12 F53A_a / U22 F53A_a 0.615 U13 F44 / U11 F44 0.518 U13 F53B_b / U11 F53B_b -0.766 y F53A_a / x F53A_a 0.606 U13 F44 / U33 F44 0.512 U11 F53A_a / FVAR 2 -0.761 U12 F53A_a / U11 F53A_a -0.604 U12 F54 / U11 F54 -0.512 y F54 / x F54 -0.680 U13 F53A_a / U23 F53A_a 0.555 z F24 / x F24 -0.511 U12 F53A_a / FVAR 2 0.638 U13 F24 / U11 F24 0.553 U12 F24 / U23 F24 -0.500 U13 F54 / U23 F54 0.626 U13 F24 / U33 F24 0.548 z F44 / x F44 -0.616 U12 F54 / U22 F54 0.544 U12 F44 / U23 F44 Idealized hydrogen atom generation before cycle 21 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H6A 0.5972 1.0375 0.1517 137 0.980 0.000 C6 C1 H6A H6B 0.4670 1.0321 0.1545 137 0.980 0.000 C6 C1 H6A H6C 0.5164 0.9801 0.1076 137 0.980 0.000 C6 C1 H6A H7A 0.7456 0.8848 0.1537 137 0.980 0.000 C7 C2 H7A H7B 0.6180 0.8774 0.1084 137 0.980 0.000 C7 C2 H7A H7C 0.6768 0.8146 0.1556 137 0.980 0.000 C7 C2 H7A H8A 0.7001 0.7651 0.2625 137 0.980 0.000 C8 C3 H8A H8B 0.6880 0.7791 0.3382 137 0.980 0.000 C8 C3 H8A H8C 0.7938 0.8101 0.3143 137 0.980 0.000 C8 C3 H8A H9A 0.6804 0.9290 0.4172 137 0.980 0.000 C9 C4 H9A H9B 0.6240 0.8539 0.4054 137 0.980 0.000 C9 C4 H9A H9C 0.5457 0.9206 0.4041 137 0.980 0.000 C9 C4 H9A H10A 0.4552 1.0129 0.3336 137 0.980 0.000 C10 C5 H10A H10B 0.4474 1.0513 0.2626 137 0.980 0.000 C10 C5 H10A H10C 0.5583 1.0601 0.3241 137 0.980 0.000 C10 C5 H10A H22 -0.2023 0.8233 -0.0441 43 0.950 0.000 C22 C21 C23 H24 -0.4474 0.7276 0.0263 43 0.950 0.000 C24 C23 C25 H26 -0.1230 0.6569 0.0786 43 0.950 0.000 C26 C25 C21 H32 -0.1150 0.6249 -0.0502 43 0.950 0.000 C32 C31 C33 H34 0.1439 0.5166 -0.0928 43 0.950 0.000 C34 C33 C35 H36 0.2035 0.7013 0.0033 43 0.950 0.000 C36 C35 C31 H42 0.1596 0.6653 0.1130 43 0.950 0.000 C42 C41 C43 H44 0.1728 0.7675 0.2897 43 0.950 0.000 C44 C43 C45 H46 -0.0200 0.8411 0.1110 43 0.950 0.000 C46 C45 C41 H52 0.1414 0.8613 0.0441 43 0.950 0.000 C52 C53 C51 H54 0.0761 0.9579 -0.1388 43 0.950 0.000 C54 C55 C53 H56 -0.0824 0.7787 -0.1178 43 0.950 0.000 C56 C55 C51 2005src1438 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.56673 0.95601 0.20897 1.00000 0.02585 0.02091 0.02682 0.00350 0.00541 -0.00321 0.02473 0.00443 0.00020 0.00012 0.00012 0.00000 0.00114 0.00112 0.00119 0.00091 0.00093 0.00088 0.00048 C2 0.62725 0.89303 0.20949 1.00000 0.02482 0.02197 0.02409 -0.00215 0.00998 -0.00418 0.02294 0.00430 0.00019 0.00012 0.00012 0.00000 0.00110 0.00111 0.00115 0.00088 0.00091 0.00087 0.00046 C3 0.64601 0.86315 0.27566 1.00000 0.01769 0.02263 0.02589 0.00164 0.00577 -0.00183 0.02201 0.00422 0.00018 0.00012 0.00012 0.00000 0.00099 0.00114 0.00115 0.00089 0.00085 0.00083 0.00045 C4 0.60145 0.90988 0.31731 1.00000 0.01678 0.02834 0.02041 -0.00221 0.00422 -0.00494 0.02192 0.00408 0.00018 0.00012 0.00011 0.00000 0.00100 0.00121 0.00110 0.00089 0.00083 0.00086 0.00045 C5 0.55104 0.96627 0.27632 1.00000 0.02386 0.02047 0.03260 -0.00477 0.00961 -0.00341 0.02519 0.00439 0.00019 0.00012 0.00012 0.00000 0.00112 0.00111 0.00128 0.00093 0.00096 0.00087 0.00048 C6 0.53402 1.00571 0.15067 1.00000 0.04825 0.03292 0.04195 0.01586 0.00713 -0.00047 0.04177 0.00586 0.00026 0.00015 0.00015 0.00000 0.00168 0.00147 0.00161 0.00123 0.00130 0.00124 0.00068 H6A 0.59718 1.03753 0.15173 1.00000 0.06266 0.00000 0.00000 H6B 0.46704 1.03206 0.15453 1.00000 0.06266 0.00000 0.00000 H6C 0.51645 0.98006 0.10759 1.00000 0.06266 0.00000 0.00000 C7 0.67066 0.86503 0.15181 1.00000 0.04875 0.03958 0.03573 -0.00820 0.02463 -0.00369 0.03885 0.00557 0.00025 0.00015 0.00014 0.00000 0.00163 0.00157 0.00149 0.00121 0.00127 0.00127 0.00064 H7A 0.74564 0.88477 0.15371 1.00000 0.05828 0.00000 0.00000 H7B 0.61796 0.87742 0.10839 1.00000 0.05828 0.00000 0.00000 H7C 0.67676 0.81459 0.15559 1.00000 0.05828 0.00000 0.00000 C8 0.71277 0.79878 0.29976 1.00000 0.03109 0.03367 0.05098 0.01421 0.01159 0.01106 0.03834 0.00587 0.00023 0.00014 0.00015 0.00000 0.00135 0.00144 0.00172 0.00125 0.00122 0.00112 0.00064 H8A 0.70014 0.76508 0.26251 1.00000 0.05751 0.00000 0.00000 H8B 0.68799 0.77906 0.33822 1.00000 0.05751 0.00000 0.00000 H8C 0.79380 0.81014 0.31430 1.00000 0.05751 0.00000 0.00000 C9 0.61396 0.90274 0.39253 1.00000 0.02779 0.04960 0.02295 -0.00395 0.00612 -0.01217 0.03348 0.00469 0.00021 0.00015 0.00012 0.00000 0.00125 0.00163 0.00124 0.00112 0.00099 0.00114 0.00058 H9A 0.68041 0.92905 0.41725 1.00000 0.05023 0.00000 0.00000 H9B 0.62396 0.85387 0.40539 1.00000 0.05023 0.00000 0.00000 H9C 0.54570 0.92064 0.40411 1.00000 0.05023 0.00000 0.00000 C10 0.49842 1.02798 0.30130 1.00000 0.04984 0.02771 0.06144 -0.01231 0.02453 0.00111 0.04444 0.00598 0.00026 0.00014 0.00017 0.00000 0.00172 0.00141 0.00198 0.00132 0.00149 0.00125 0.00071 H10A 0.45518 1.01292 0.33359 1.00000 0.06666 0.00000 0.00000 H10B 0.44739 1.05125 0.26258 1.00000 0.06666 0.00000 0.00000 H10C 0.55832 1.06006 0.32406 1.00000 0.06666 0.00000 0.00000 C11 0.33771 0.91964 0.20308 1.00000 0.02622 0.04181 0.03486 0.00797 0.00583 -0.00045 0.03461 0.00518 0.00022 0.00015 0.00014 0.00000 0.00123 0.00154 0.00144 0.00118 0.00106 0.00111 0.00059 C12 0.43946 0.80941 0.16838 1.00000 0.03561 0.04453 0.03383 -0.00743 0.00833 -0.01163 0.03805 0.00513 0.00023 0.00015 0.00014 0.00000 0.00142 0.00162 0.00146 0.00123 0.00114 0.00121 0.00062 C13 0.42386 0.82344 0.29740 1.00000 0.02300 0.02438 0.03080 -0.00437 0.00041 -0.00599 0.02718 0.00431 0.00020 0.00012 0.00013 0.00000 0.00113 0.00120 0.00131 0.00100 0.00096 0.00092 0.00051 O11 0.25672 0.94985 0.18227 1.00000 0.02945 0.07087 0.06546 0.02611 0.00730 0.01651 0.05606 0.00471 0.00017 0.00013 0.00012 0.00000 0.00106 0.00158 0.00148 0.00123 0.00099 0.00104 0.00061 O12 0.42129 0.76991 0.12588 1.00000 0.06511 0.06471 0.04923 -0.03254 0.01951 -0.02714 0.05875 0.00390 0.00020 0.00013 0.00011 0.00000 0.00149 0.00152 0.00133 0.00117 0.00112 0.00122 0.00064 O13 0.40004 0.79283 0.33949 1.00000 0.04304 0.03416 0.03339 0.00181 0.00924 -0.01449 0.03692 0.00339 0.00016 0.00010 0.00009 0.00000 0.00108 0.00102 0.00102 0.00082 0.00083 0.00084 0.00043 Fe1 0.47062 0.87422 0.23470 1.00000 0.01972 0.02112 0.02090 -0.00008 0.00298 -0.00059 0.02095 0.00059 0.00003 0.00002 0.00002 0.00000 0.00016 0.00017 0.00017 0.00013 0.00012 0.00013 0.00009 C21 -0.14024 0.74086 0.01575 1.00000 0.01823 0.01498 0.01658 -0.00274 0.00327 -0.00139 0.01679 0.00381 0.00017 0.00011 0.00010 0.00000 0.00097 0.00099 0.00101 0.00078 0.00079 0.00078 0.00041 C22 -0.22322 0.78722 -0.01780 1.00000 0.02208 0.01533 0.01687 -0.00159 0.00307 -0.00124 0.01841 0.00389 0.00018 0.00011 0.00011 0.00000 0.00103 0.00101 0.00105 0.00079 0.00082 0.00080 0.00042 H22 -0.20233 0.82331 -0.04408 1.00000 0.02209 0.00000 0.00000 C23 -0.33658 0.78229 -0.01401 1.00000 0.01854 0.01870 0.01901 -0.00293 0.00055 0.00226 0.01948 0.00397 0.00018 0.00011 0.00011 0.00000 0.00100 0.00105 0.00107 0.00083 0.00082 0.00082 0.00043 C24 -0.37056 0.73106 0.02389 1.00000 0.01454 0.02097 0.02111 -0.00456 0.00378 -0.00051 0.01899 0.00392 0.00017 0.00011 0.00011 0.00000 0.00095 0.00106 0.00108 0.00084 0.00081 0.00080 0.00043 H24 -0.44742 0.72757 0.02631 1.00000 0.02279 0.00000 0.00000 C25 -0.28869 0.68449 0.05858 1.00000 0.02102 0.01603 0.01787 -0.00190 0.00566 -0.00160 0.01816 0.00396 0.00018 0.00011 0.00011 0.00000 0.00103 0.00101 0.00105 0.00080 0.00082 0.00080 0.00042 C26 -0.17680 0.68940 0.05445 1.00000 0.01666 0.01693 0.01887 -0.00022 0.00250 0.00091 0.01783 0.00392 0.00017 0.00011 0.00011 0.00000 0.00096 0.00102 0.00106 0.00080 0.00080 0.00078 0.00042 H26 -0.12302 0.65689 0.07858 1.00000 0.02139 0.00000 0.00000 C27 -0.42043 0.83389 -0.05183 1.00000 0.02358 0.02127 0.02746 0.00073 0.00118 0.00182 0.02502 0.00438 0.00019 0.00012 0.00012 0.00000 0.00110 0.00113 0.00124 0.00093 0.00092 0.00090 0.00048 C28 -0.32524 0.62982 0.10060 1.00000 0.01969 0.02459 0.02916 0.00252 0.00805 0.00015 0.02413 0.00444 0.00018 0.00012 0.00012 0.00000 0.00104 0.00117 0.00124 0.00095 0.00090 0.00089 0.00047 C31 0.03555 0.67433 -0.01673 1.00000 0.01745 0.01846 0.01560 0.00210 0.00396 -0.00241 0.01720 0.00393 0.00017 0.00011 0.00010 0.00000 0.00096 0.00102 0.00101 0.00080 0.00078 0.00079 0.00041 C32 -0.03625 0.62145 -0.04813 1.00000 0.01476 0.02003 0.01534 0.00191 0.00370 -0.00039 0.01672 0.00388 0.00017 0.00011 0.00010 0.00000 0.00092 0.00102 0.00099 0.00080 0.00075 0.00079 0.00040 H32 -0.11499 0.62486 -0.05015 1.00000 0.02007 0.00000 0.00000 C33 0.00248 0.56370 -0.07674 1.00000 0.01693 0.01915 0.01547 0.00221 0.00327 -0.00179 0.01732 0.00391 0.00017 0.00011 0.00010 0.00000 0.00096 0.00103 0.00101 0.00080 0.00078 0.00079 0.00041 C34 0.11676 0.55616 -0.07400 1.00000 0.01996 0.01746 0.02096 0.00247 0.00746 0.00142 0.01904 0.00413 0.00018 0.00011 0.00011 0.00000 0.00101 0.00104 0.00110 0.00083 0.00084 0.00081 0.00043 H34 0.14387 0.51660 -0.09283 1.00000 0.02285 0.00000 0.00000 C35 0.19059 0.60796 -0.04300 1.00000 0.01591 0.02446 0.02060 0.00251 0.00651 -0.00207 0.01998 0.00416 0.00018 0.00012 0.00011 0.00000 0.00097 0.00113 0.00110 0.00086 0.00082 0.00082 0.00044 C36 0.15108 0.66597 -0.01612 1.00000 0.01615 0.02098 0.02024 0.00017 0.00353 -0.00438 0.01930 0.00405 0.00017 0.00011 0.00011 0.00000 0.00097 0.00108 0.00108 0.00084 0.00081 0.00081 0.00043 H36 0.20347 0.70129 0.00334 1.00000 0.02316 0.00000 0.00000 C37 -0.08034 0.51120 -0.11362 1.00000 0.01991 0.01932 0.02060 0.00018 0.00577 0.00000 0.01982 0.00409 0.00018 0.00011 0.00011 0.00000 0.00102 0.00106 0.00110 0.00084 0.00085 0.00083 0.00044 C38 0.31490 0.59801 -0.03685 1.00000 0.02038 0.02983 0.04215 -0.00023 0.01036 -0.00314 0.03033 0.00485 0.00020 0.00013 0.00014 0.00000 0.00112 0.00128 0.00148 0.00111 0.00104 0.00095 0.00054 C41 0.06041 0.75120 0.09802 1.00000 0.01663 0.01838 0.02110 -0.00085 0.00647 -0.00538 0.01839 0.00393 0.00017 0.00011 0.00011 0.00000 0.00096 0.00103 0.00107 0.00083 0.00081 0.00080 0.00042 C42 0.13581 0.70321 0.13583 1.00000 0.01871 0.02067 0.02221 0.00012 0.00479 -0.00264 0.02059 0.00407 0.00018 0.00011 0.00011 0.00000 0.00101 0.00108 0.00111 0.00087 0.00084 0.00084 0.00044 H42 0.15961 0.66527 0.11303 1.00000 0.02471 0.00000 0.00000 C43 0.17763 0.70934 0.20669 1.00000 0.01865 0.02500 0.02251 0.00275 0.00154 -0.00604 0.02269 0.00415 0.00018 0.00012 0.00011 0.00000 0.00102 0.00116 0.00114 0.00090 0.00085 0.00086 0.00046 C44 0.14529 0.76375 0.24161 1.00000 0.02259 0.03159 0.01989 -0.00285 0.00165 -0.00711 0.02533 0.00423 0.00019 0.00013 0.00012 0.00000 0.00111 0.00128 0.00113 0.00094 0.00089 0.00094 0.00049 H44 0.17277 0.76755 0.28966 1.00000 0.03040 0.00000 0.00000 C45 0.07129 0.81303 0.20465 1.00000 0.02187 0.02665 0.02295 -0.00490 0.00779 -0.00509 0.02343 0.00423 0.00019 0.00012 0.00012 0.00000 0.00108 0.00120 0.00115 0.00092 0.00089 0.00089 0.00047 C46 0.03031 0.80674 0.13494 1.00000 0.01887 0.02306 0.02306 -0.00146 0.00423 -0.00240 0.02184 0.00411 0.00018 0.00012 0.00011 0.00000 0.00103 0.00112 0.00113 0.00089 0.00086 0.00085 0.00045 H46 -0.01999 0.84110 0.11102 1.00000 0.02621 0.00000 0.00000 C47 0.26092 0.65722 0.24447 1.00000 0.03315 0.02720 0.02589 0.00022 -0.00154 -0.00244 0.03032 0.00459 0.00022 0.00013 0.00013 0.00000 0.00130 0.00128 0.00127 0.00099 0.00100 0.00103 0.00054 C48 0.03475 0.87068 0.24302 1.00000 0.03696 0.03647 0.02688 -0.00815 0.00888 -0.00207 0.03327 0.00486 0.00022 0.00014 0.00013 0.00000 0.00138 0.00145 0.00129 0.00109 0.00105 0.00113 0.00056 C51 0.02348 0.80954 -0.02789 1.00000 0.02062 0.01916 0.02123 -0.00080 0.00779 -0.00176 0.01988 0.00412 0.00018 0.00011 0.00011 0.00000 0.00103 0.00105 0.00110 0.00085 0.00086 0.00083 0.00044 C52 0.10102 0.86228 -0.00257 1.00000 0.02897 0.03034 0.02103 -0.00195 0.00321 -0.01213 0.02732 0.00432 0.00020 0.00013 0.00012 0.00000 0.00120 0.00129 0.00116 0.00095 0.00093 0.00099 0.00051 H52 0.14136 0.86126 0.04406 1.00000 0.03278 0.00000 0.00000 C53 0.12113 0.91631 -0.04346 1.00000 0.04396 0.03361 0.03024 -0.00238 0.00735 -0.02286 0.03627 0.00473 0.00024 0.00014 0.00013 0.00000 0.00150 0.00141 0.00135 0.00110 0.00113 0.00119 0.00062 C54 0.06326 0.92051 -0.11124 1.00000 0.04533 0.02864 0.02851 0.00380 0.01041 -0.01511 0.03395 0.00482 0.00023 0.00013 0.00013 0.00000 0.00151 0.00132 0.00131 0.00104 0.00112 0.00114 0.00059 H54 0.07607 0.95790 -0.13880 1.00000 0.04074 0.00000 0.00000 C55 -0.01362 0.86912 -0.13800 1.00000 0.03215 0.02603 0.02215 0.00097 0.00706 -0.00631 0.02673 0.00447 0.00021 0.00012 0.00012 0.00000 0.00123 0.00122 0.00116 0.00094 0.00095 0.00099 0.00050 C56 -0.03126 0.81435 -0.09757 1.00000 0.02210 0.02062 0.02051 -0.00068 0.00464 -0.00574 0.02120 0.00416 0.00018 0.00011 0.00011 0.00000 0.00107 0.00110 0.00110 0.00085 0.00087 0.00085 0.00045 H56 -0.08237 0.77870 -0.11780 1.00000 0.02543 0.00000 0.00000 C57 0.20499 0.97147 -0.01332 1.00000 0.07985 0.05300 0.03747 0.00052 0.00997 -0.04756 0.05760 0.00578 0.00033 0.00018 0.00016 0.00000 0.00241 0.00200 0.00169 0.00145 0.00162 0.00180 0.00095 C58 -0.08266 0.87372 -0.21021 1.00000 0.04361 0.03043 0.02513 0.00375 0.00622 -0.00826 0.03347 0.00492 0.00023 0.00014 0.00013 0.00000 0.00148 0.00134 0.00127 0.00105 0.00107 0.00116 0.00057 B21 -0.00442 0.74411 0.01650 1.00000 0.01726 0.01779 0.01836 -0.00139 0.00380 -0.00181 0.01792 0.00446 0.00020 0.00012 0.00012 0.00000 0.00107 0.00115 0.00117 0.00091 0.00090 0.00089 0.00047 F21 -0.39427 0.89820 -0.03081 1.00000 0.04867 0.01727 0.05262 -0.00155 -0.01337 0.00651 0.04412 0.00285 0.00014 0.00007 0.00008 0.00000 0.00095 0.00070 0.00101 0.00067 0.00076 0.00066 0.00042 F22 -0.42764 0.83324 -0.11863 1.00000 0.05853 0.05184 0.02528 0.00434 -0.00232 0.02654 0.04748 0.00332 0.00015 0.00009 0.00008 0.00000 0.00106 0.00104 0.00081 0.00071 0.00071 0.00085 0.00044 F23 -0.52577 0.82292 -0.04585 1.00000 0.02283 0.04657 0.07990 0.02191 0.00909 0.01132 0.05043 0.00355 0.00013 0.00009 0.00010 0.00000 0.00076 0.00100 0.00128 0.00091 0.00078 0.00069 0.00046 F24 -0.37141 0.65694 0.14845 1.00000 0.07322 0.03943 0.06442 0.01619 0.05588 0.01540 0.05216 0.00402 0.00016 0.00009 0.00009 0.00000 0.00121 0.00093 0.00116 0.00083 0.00101 0.00086 0.00049 F25 -0.40384 0.58792 0.06262 1.00000 0.04095 0.04479 0.05095 0.01886 -0.00947 -0.02583 0.04927 0.00292 0.00014 0.00009 0.00009 0.00000 0.00091 0.00098 0.00101 0.00079 0.00075 0.00077 0.00046 F26 -0.24181 0.58887 0.13327 1.00000 0.02758 0.02932 0.03284 0.01235 0.00734 0.00147 0.02995 0.00273 0.00011 0.00007 0.00007 0.00000 0.00070 0.00076 0.00077 0.00060 0.00058 0.00058 0.00031 F31 -0.14589 0.53630 -0.17217 1.00000 0.03905 0.03022 0.02729 0.00553 -0.01045 -0.01221 0.03550 0.00252 0.00013 0.00007 0.00007 0.00000 0.00083 0.00078 0.00075 0.00061 0.00061 0.00064 0.00035 F32 -0.15331 0.49043 -0.07774 1.00000 0.03198 0.03243 0.03444 -0.00438 0.01405 -0.01534 0.03193 0.00258 0.00012 0.00007 0.00007 0.00000 0.00075 0.00078 0.00079 0.00062 0.00062 0.00061 0.00033 F33 -0.03099 0.45442 -0.12952 1.00000 0.02608 0.02680 0.05655 -0.01870 0.00745 -0.00053 0.03698 0.00265 0.00012 0.00007 0.00008 0.00000 0.00073 0.00076 0.00100 0.00069 0.00067 0.00059 0.00036 F34 0.33596 0.57386 -0.09454 1.00000 0.02913 0.05366 0.06528 -0.02054 0.02788 -0.00507 0.04650 0.00313 0.00013 0.00009 0.00009 0.00000 0.00079 0.00104 0.00112 0.00087 0.00078 0.00073 0.00043 F35 0.36054 0.55173 0.01120 1.00000 0.02236 0.05872 0.07854 0.02938 0.00621 0.00960 0.05433 0.00371 0.00013 0.00010 0.00010 0.00000 0.00077 0.00113 0.00128 0.00098 0.00079 0.00075 0.00049 F36 0.37465 0.65611 -0.02191 1.00000 0.01882 0.03742 0.06865 -0.01096 0.01380 -0.00895 0.04112 0.00283 0.00012 0.00008 0.00009 0.00000 0.00069 0.00087 0.00112 0.00079 0.00070 0.00062 0.00039 F41 0.24373 0.59394 0.21899 1.00000 0.05519 0.02261 0.06108 0.00120 -0.02451 -0.00116 0.05320 0.00293 0.00015 0.00008 0.00009 0.00000 0.00106 0.00079 0.00112 0.00075 0.00086 0.00073 0.00050 F42 0.36822 0.67271 0.24270 1.00000 0.02756 0.03406 0.05671 0.00012 -0.00207 0.00350 0.04167 0.00292 0.00012 0.00008 0.00009 0.00000 0.00077 0.00085 0.00103 0.00074 0.00069 0.00064 0.00039 F43 0.26405 0.65432 0.31080 1.00000 0.06062 0.06639 0.03123 0.01914 0.00432 0.01582 0.05401 0.00368 0.00016 0.00010 0.00008 0.00000 0.00113 0.00122 0.00090 0.00083 0.00078 0.00095 0.00047 F44 -0.02144 0.84784 0.28739 1.00000 0.07279 0.05346 0.07243 -0.02410 0.05528 -0.01404 0.05964 0.00382 0.00017 0.00010 0.00010 0.00000 0.00127 0.00111 0.00128 0.00097 0.00108 0.00096 0.00054 F45 -0.03157 0.91676 0.20303 1.00000 0.08840 0.05320 0.04342 -0.01746 0.00152 0.03577 0.06432 0.00375 0.00018 0.00010 0.00009 0.00000 0.00148 0.00116 0.00104 0.00087 0.00096 0.00107 0.00059 F46 0.12233 0.90672 0.28011 1.00000 0.05496 0.04954 0.04522 -0.02801 0.01607 -0.01568 0.04927 0.00297 0.00015 0.00009 0.00009 0.00000 0.00104 0.00103 0.00098 0.00082 0.00081 0.00083 0.00044 F51A_a 0.29911 0.94566 0.02843 0.85499 0.05886 0.09260 0.08611 -0.01096 -0.00873 -0.05220 0.08394 0.00441 0.00024 0.00016 0.00017 0.00555 0.00166 0.00215 0.00228 0.00163 0.00146 0.00152 0.00116 F52A_a 0.16718 1.01365 0.02716 0.85499 0.10408 0.05670 0.11135 -0.04306 0.01000 -0.03686 0.09370 0.00562 0.00032 0.00017 0.00020 0.00555 0.00257 0.00189 0.00274 0.00186 0.00205 0.00172 0.00124 F53A_a 0.24096 1.00717 -0.05884 0.85499 0.16615 0.13874 0.04602 0.00981 0.00965 -0.13399 0.11994 0.00502 0.00044 0.00024 0.00014 0.00555 0.00415 0.00354 0.00155 0.00176 0.00190 0.00340 0.00209 F51B_b 0.22526 0.98210 0.04841 0.14501 0.07527 0.08049 0.04641 -0.00829 0.00955 -0.04203 0.06839 0.02579 0.00161 0.00098 0.00059 0.00555 0.00862 0.00862 0.00534 0.00522 0.00536 0.00690 0.00462 F52B_b 0.16691 1.03476 -0.04221 0.14501 0.04562 0.02665 0.06610 0.00044 -0.01036 -0.02946 0.05043 0.02163 0.00110 0.00053 0.00079 0.00555 0.00625 0.00459 0.00751 0.00468 0.00522 0.00423 0.00402 F53B_b 0.29988 0.96381 -0.03082 0.14501 0.05117 0.08101 0.10325 -0.02937 0.02540 -0.02749 0.07739 0.03063 0.00114 0.00092 0.00107 0.00555 0.00586 0.00841 0.00981 0.00738 0.00621 0.00527 0.00506 F54 -0.04153 0.91665 -0.24751 1.00000 0.14576 0.12297 0.03068 0.03484 -0.01741 -0.09877 0.10678 0.00376 0.00024 0.00014 0.00010 0.00000 0.00228 0.00209 0.00102 0.00117 0.00118 0.00187 0.00112 F55 -0.18877 0.89230 -0.21363 1.00000 0.07247 0.12542 0.03483 -0.00531 -0.00788 0.05591 0.08134 0.00448 0.00019 0.00014 0.00009 0.00000 0.00139 0.00202 0.00104 0.00112 0.00092 0.00138 0.00076 F56 -0.09386 0.81353 -0.24251 1.00000 0.06996 0.05168 0.02836 -0.00830 -0.00379 0.00483 0.05284 0.00323 0.00016 0.00009 0.00008 0.00000 0.00122 0.00108 0.00087 0.00076 0.00079 0.00091 0.00047 Final Structure Factor Calculation for 2005src1438 in P2(1)/c Total number of l.s. parameters = 701 Maximum vector length = 511 Memory required = 7622 / 25039 wR2 = 0.1150 before cycle 21 for 10558 data and 0 / 701 parameters Disagreeable restraints before cycle 21 Observed Target Error Sigma Restraint 1.3857 1.2887 0.0969 0.0200 DFIX C57 F52B_b -0.0341 0.0100 DELU C57 F53B_b 0.0522 0.0100 ISOR U12 F51A_a 0.0370 0.0100 ISOR U22 F52A_a 0.0431 0.0100 ISOR U23 F52A_a 0.0369 0.0100 ISOR U12 F52A_a -0.0462 0.0100 ISOR U11 F53A_a 0.0739 0.0100 ISOR U33 F53A_a 0.1340 0.0100 ISOR U12 F53A_a 0.0420 0.0100 ISOR U12 F51B_b Summary of restraints applied in cycle 21 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 6. 6. 0. 0. 0. 0. 253. 492. 36. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.010 0.063 0.010 0.000 rms deviation 0.000 0.053 0.035 0.000 0.000 0.000 0.000 0.005 0.023 0.035 0.000 GooF = S = 1.027; Restrained GooF = 1.016 for 793 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0397 * P )^2 + 5.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0483 for 8351 Fo > 4sig(Fo) and 0.0672 for all 10558 data wR2 = 0.1150, GooF = S = 1.027, Restrained GooF = 1.016 for all data Occupancy sum of asymmetric unit = 74.00 for non-hydrogen and 27.00 for hydrogen atoms Principal mean square atomic displacements U 0.0309 0.0254 0.0179 C1 0.0298 0.0209 0.0182 C2 0.0268 0.0226 0.0166 C3 0.0303 0.0206 0.0149 C4 0.0347 0.0228 0.0181 C5 0.0580 0.0465 0.0209 C6 0.0575 0.0385 0.0205 C7 0.0593 0.0355 0.0203 C8 0.0550 0.0239 0.0215 C9 0.0681 0.0439 0.0214 C10 0.0477 0.0300 0.0262 C11 0.0532 0.0347 0.0263 C12 0.0364 0.0295 0.0157 C13 0.0945 0.0516 0.0221 O11 0.1010 0.0529 0.0224 O12 0.0548 0.0338 0.0222 O13 0.0232 0.0211 0.0185 Fe1 0.0192 0.0185 0.0127 C21 0.0233 0.0178 0.0141 C22 0.0266 0.0165 0.0154 C23 0.0258 0.0167 0.0145 C24 0.0217 0.0180 0.0148 C25 0.0208 0.0171 0.0156 C26 0.0328 0.0229 0.0194 C27 0.0303 0.0236 0.0185 C28 0.0215 0.0164 0.0137 C31 0.0208 0.0148 0.0145 C32 0.0216 0.0160 0.0143 C33 0.0235 0.0175 0.0161 C34 0.0260 0.0204 0.0135 C35 0.0241 0.0202 0.0136 C36 0.0209 0.0194 0.0191 C37 0.0422 0.0307 0.0181 C38 0.0234 0.0202 0.0115 C41 0.0231 0.0219 0.0168 C42 0.0324 0.0207 0.0150 C43 0.0356 0.0246 0.0158 C44 0.0319 0.0198 0.0186 C45 0.0246 0.0233 0.0177 C46 0.0425 0.0270 0.0215 C47 0.0414 0.0364 0.0220 C48 0.0236 0.0190 0.0170 C51 0.0425 0.0229 0.0166 C52 0.0630 0.0305 0.0153 C53 0.0551 0.0305 0.0162 C54 0.0365 0.0236 0.0202 C55 0.0274 0.0206 0.0156 C56 0.1190 0.0375 0.0163 C57 0.0497 0.0287 0.0220 C58 0.0196 0.0188 0.0154 B21 0.0860 0.0306 0.0158 F21 0.0860 0.0376 0.0188 F22 0.0916 0.0417 0.0180 F23 0.1060 0.0336 0.0168 F24 0.0986 0.0326 0.0166 F25 0.0437 0.0275 0.0185 F26 0.0654 0.0244 0.0168 F31 0.0489 0.0311 0.0158 F32 0.0672 0.0260 0.0177 F33 0.0823 0.0405 0.0167 F34 0.1010 0.0429 0.0192 F35 0.0721 0.0366 0.0146 F36 0.1102 0.0268 0.0226 F41 0.0657 0.0350 0.0243 F42 0.0803 0.0604 0.0213 F43 0.1124 0.0461 0.0205 F44 0.1252 0.0452 0.0225 F45 0.0793 0.0495 0.0191 F46 0.1379 0.0972 0.0168 F51A_a 0.1358 0.1238 0.0215 F52A_a 0.2992 0.0469 0.0137 F53A_a may be split into 0.2547 0.9986 -0.0616 and 0.2273 1.0157 -0.0561 0.1209 0.0504 0.0338 F51B_b 0.0970 0.0498 0.0045 F52B_b 0.1254 0.0720 0.0348 F53B_b 0.2655 0.0386 0.0162 F54 may be split into -0.0299 0.9089 -0.2519 and -0.0532 0.9244 -0.2431 0.1688 0.0493 0.0260 F55 0.0833 0.0509 0.0243 F56 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.012 0.024 0.035 0.048 0.062 0.078 0.098 0.129 0.191 1.000 Number in group 1072. 1089. 1004. 1116. 1024. 1040. 1055. 1039. 1059. 1060. GooF 1.079 1.017 1.013 1.009 1.050 1.040 0.998 1.029 0.996 1.034 K 4.449 1.399 1.104 1.039 1.020 1.010 1.003 0.999 1.003 1.005 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.32 1.66 inf Number in group 1093. 1051. 1052. 1068. 1033. 1038. 1062. 1054. 1052. 1055. GooF 0.977 0.940 0.964 0.948 0.925 0.940 0.963 0.925 1.142 1.432 K 1.008 1.032 1.051 1.028 1.015 1.016 1.003 0.995 0.993 1.011 R1 0.178 0.141 0.125 0.102 0.073 0.064 0.051 0.041 0.039 0.032 Recommended weighting scheme: WGHT 0.0390 5.7280 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 0 2 3042.68 7103.49 10.79 0.308 6.75 0 0 14 428.46 13.22 7.75 0.013 1.40 -6 9 3 327.06 1.66 7.00 0.005 1.47 -3 9 6 817.76 295.06 6.89 0.063 1.72 3 6 3 155.55 5.10 6.27 0.008 2.21 0 14 7 189.28 3.86 5.90 0.007 1.24 3 3 6 656.00 343.82 5.69 0.068 2.13 4 6 3 1846.00 1209.28 5.65 0.127 1.96 0 12 6 1556.01 1020.75 4.79 0.117 1.45 3 9 0 2185.31 1587.89 4.55 0.146 1.88 3 5 6 723.61 1103.10 4.49 0.122 1.95 0 0 12 7323.56 5683.33 4.43 0.276 1.63 -6 3 9 283.35 80.20 4.28 0.033 1.63 -2 5 7 381.56 210.13 4.21 0.053 2.28 -1 5 2 72.42 9.70 4.15 0.011 3.53 -6 2 3 1470.38 1069.03 3.99 0.120 1.98 6 0 0 3791.85 2905.29 3.83 0.197 1.96 -2 7 4 323.72 171.84 3.81 0.048 2.33 -1 4 11 3914.08 3154.97 3.81 0.205 1.71 3 9 1 877.61 605.17 3.70 0.090 1.86 -4 7 4 735.82 502.38 3.64 0.082 1.99 -2 15 19 164.94 447.29 3.62 0.077 0.82 -1 4 10 1562.32 2025.04 3.62 0.165 1.86 -1 11 17 89.79 5.91 3.62 0.009 0.98 -12 3 1 111.73 5.69 3.51 0.009 0.98 3 0 12 459.45 276.72 3.50 0.061 1.39 -6 9 12 60.21 0.39 3.47 0.002 1.20 -4 7 25 82.21 270.70 3.46 0.060 0.78 6 2 1 268.10 444.70 3.45 0.077 1.87 -6 18 9 282.68 123.67 3.41 0.041 0.91 2 8 1 429.42 272.41 3.41 0.060 2.20 -2 2 15 1010.22 721.32 3.39 0.098 1.34 -2 8 2 852.88 1154.25 3.38 0.124 2.23 -4 7 10 240.30 399.14 3.34 0.073 1.54 3 17 9 267.93 495.23 3.32 0.081 0.95 3 8 2 647.75 448.88 3.31 0.078 1.96 -2 7 9 392.63 245.21 3.31 0.057 1.74 -5 1 2 65.74 158.23 3.30 0.046 2.41 -6 12 12 94.76 7.76 3.28 0.010 1.08 -2 8 7 237.25 389.80 3.27 0.072 1.83 2 10 0 2704.62 2195.60 3.24 0.171 1.84 -4 1 10 331.12 204.63 3.24 0.052 1.85 5 3 0 1525.84 1196.00 3.23 0.127 2.21 -2 2 9 86.74 186.24 3.23 0.050 2.18 2 0 16 490.14 738.36 3.22 0.099 1.14 9 13 4 143.36 288.93 3.21 0.062 0.93 11 12 5 337.66 164.87 3.21 0.047 0.83 -1 8 4 2949.49 2425.07 3.20 0.180 2.18 3 9 9 538.92 350.77 3.18 0.069 1.35 -3 3 10 1048.07 797.40 3.17 0.103 1.88 Bond lengths and angles C1 - Distance Angles C2 1.4217 (0.0032) C5 1.4377 (0.0034) 107.59 (0.20) C6 1.4979 (0.0034) 126.22 (0.23) 126.00 (0.23) Fe1 2.1078 (0.0023) 70.89 (0.13) 69.89 (0.13) 128.48 (0.18) C1 - C2 C5 C6 C2 - Distance Angles C1 1.4217 (0.0032) C3 1.4252 (0.0032) 108.39 (0.20) C7 1.4982 (0.0033) 125.89 (0.22) 125.61 (0.22) Fe1 2.1218 (0.0022) 69.83 (0.13) 69.31 (0.12) 129.59 (0.17) C2 - C1 C3 C7 C3 - Distance Angles C2 1.4252 (0.0032) C4 1.4318 (0.0031) 107.64 (0.19) C8 1.4999 (0.0033) 126.13 (0.22) 125.85 (0.22) Fe1 2.0969 (0.0022) 71.20 (0.13) 70.87 (0.12) 128.88 (0.17) C3 - C2 C4 C8 C4 - Distance Angles C5 1.4148 (0.0033) C3 1.4318 (0.0031) 108.23 (0.19) C9 1.4996 (0.0032) 125.94 (0.22) 125.68 (0.22) Fe1 2.1163 (0.0021) 69.93 (0.13) 69.40 (0.12) 129.75 (0.16) C4 - C5 C3 C9 C5 - Distance Angles C4 1.4148 (0.0033) C1 1.4377 (0.0034) 108.07 (0.20) C10 1.5004 (0.0034) 125.03 (0.23) 126.77 (0.23) Fe1 2.1037 (0.0023) 70.89 (0.13) 70.19 (0.13) 127.88 (0.18) C5 - C4 C1 C10 C6 - Distance Angles C1 1.4979 (0.0034) H6A 0.9800 109.47 H6B 0.9800 109.47 109.47 H6C 0.9800 109.47 109.47 109.47 C6 - C1 H6A H6B C7 - Distance Angles C2 1.4982 (0.0033) H7A 0.9800 109.47 H7B 0.9800 109.47 109.47 H7C 0.9800 109.47 109.47 109.47 C7 - C2 H7A H7B C8 - Distance Angles C3 1.4999 (0.0033) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - C3 H8A H8B C9 - Distance Angles C4 1.4996 (0.0032) H9A 0.9800 109.47 H9B 0.9800 109.47 109.47 H9C 0.9800 109.47 109.47 109.47 C9 - C4 H9A H9B C10 - Distance Angles C5 1.5004 (0.0034) H10A 0.9800 109.47 H10B 0.9800 109.47 109.47 H10C 0.9800 109.47 109.47 109.47 C10 - C5 H10A H10B C11 - Distance Angles O11 1.1320 (0.0031) Fe1 1.8100 (0.0026) 177.42 (0.25) C11 - O11 C12 - Distance Angles O12 1.1311 (0.0033) Fe1 1.8074 (0.0028) 178.21 (0.27) C12 - O12 C13 - Distance Angles O13 1.1334 (0.0029) Fe1 1.8060 (0.0026) 175.98 (0.21) C13 - O13 O11 - Distance Angles C11 1.1320 (0.0031) O11 - O12 - Distance Angles C12 1.1311 (0.0033) O12 - O13 - Distance Angles C13 1.1334 (0.0029) O13 - Fe1 - Distance Angles C13 1.8060 (0.0026) C12 1.8074 (0.0028) 95.82 (0.12) C11 1.8100 (0.0026) 95.93 (0.11) 94.04 (0.13) C3 2.0969 (0.0022) 97.66 (0.10) 103.14 (0.11) 156.82 (0.11) C5 2.1037 (0.0023) 112.00 (0.10) 151.08 (0.11) 90.89 (0.11) 66.60 (0.09) C1 2.1078 (0.0023) 150.83 (0.10) 111.29 (0.11) 92.81 (0.11) 66.61 (0.09) 39.92 (0.09) C4 2.1163 (0.0022) 85.82 (0.09) 142.27 (0.11) 123.37 (0.11) 39.73 (0.09) 39.17 (0.09) 66.26 (0.09) C2 2.1218 (0.0022) 136.15 (0.10) 88.53 (0.11) 127.35 (0.11) 39.48 (0.09) 66.19 (0.09) 39.28 (0.09) 65.93 (0.09) Fe1 - C13 C12 C11 C3 C5 C1 C4 C21 - Distance Angles C22 1.3934 (0.0029) C26 1.4058 (0.0029) 115.89 (0.19) B21 1.6484 (0.0031) 125.55 (0.19) 118.49 (0.18) C21 - C22 C26 C22 - Distance Angles C21 1.3934 (0.0029) C23 1.4022 (0.0030) 122.08 (0.20) H22 0.9500 118.96 118.96 C22 - C21 C23 C23 - Distance Angles C24 1.3783 (0.0031) C22 1.4022 (0.0030) 120.96 (0.20) C27 1.4942 (0.0030) 120.33 (0.20) 118.71 (0.20) C23 - C24 C22 C24 - Distance Angles C23 1.3783 (0.0031) C25 1.3954 (0.0030) 118.01 (0.19) H24 0.9500 121.00 121.00 C24 - C23 C25 C25 - Distance Angles C26 1.3864 (0.0029) C24 1.3954 (0.0030) 120.82 (0.20) C28 1.4930 (0.0030) 121.25 (0.19) 117.92 (0.19) C25 - C26 C24 C26 - Distance Angles C25 1.3864 (0.0029) C21 1.4058 (0.0029) 122.23 (0.20) H26 0.9500 118.88 118.88 C26 - C25 C21 C27 - Distance Angles F21 1.3276 (0.0027) F23 1.3328 (0.0027) 106.18 (0.20) F22 1.3344 (0.0028) 106.50 (0.20) 105.61 (0.19) C23 1.4942 (0.0030) 112.53 (0.18) 113.27 (0.20) 112.20 (0.19) C27 - F21 F23 F22 C28 - Distance Angles F26 1.3264 (0.0026) F25 1.3399 (0.0027) 105.80 (0.19) F24 1.3420 (0.0027) 106.16 (0.19) 106.54 (0.19) C25 1.4930 (0.0030) 114.11 (0.18) 111.83 (0.19) 111.87 (0.19) C28 - F26 F25 F24 C31 - Distance Angles C32 1.3914 (0.0029) C36 1.4105 (0.0028) 115.43 (0.19) B21 1.6353 (0.0032) 125.33 (0.18) 119.23 (0.18) C31 - C32 C36 C32 - Distance Angles C31 1.3914 (0.0029) C33 1.3933 (0.0029) 122.76 (0.19) H32 0.9500 118.62 118.62 C32 - C31 C33 C33 - Distance Angles C34 1.3839 (0.0029) C32 1.3933 (0.0029) 120.50 (0.19) C37 1.4925 (0.0029) 119.56 (0.19) 119.87 (0.18) C33 - C34 C32 C34 - Distance Angles C33 1.3839 (0.0029) C35 1.3865 (0.0030) 118.16 (0.20) H34 0.9500 120.92 120.92 C34 - C33 C35 C35 - Distance Angles C36 1.3844 (0.0031) C34 1.3865 (0.0030) 121.00 (0.19) C38 1.4973 (0.0030) 120.88 (0.20) 118.07 (0.20) C35 - C36 C34 C36 - Distance Angles C35 1.3844 (0.0031) C31 1.4105 (0.0028) 122.11 (0.20) H36 0.9500 118.94 118.94 C36 - C35 C31 C37 - Distance Angles F33 1.3290 (0.0025) F32 1.3408 (0.0025) 106.46 (0.18) F31 1.3441 (0.0025) 106.77 (0.18) 105.07 (0.17) C33 1.4925 (0.0029) 113.26 (0.18) 112.78 (0.18) 111.93 (0.17) C37 - F33 F32 F31 C38 - Distance Angles F36 1.3313 (0.0028) F35 1.3369 (0.0030) 107.21 (0.21) F34 1.3413 (0.0030) 106.27 (0.20) 105.47 (0.21) C35 1.4973 (0.0030) 113.10 (0.20) 111.94 (0.20) 112.34 (0.20) C38 - F36 F35 F34 C41 - Distance Angles C42 1.3922 (0.0030) C46 1.4085 (0.0030) 116.04 (0.20) B21 1.6488 (0.0031) 125.47 (0.19) 118.22 (0.19) C41 - C42 C46 C42 - Distance Angles C41 1.3922 (0.0030) C43 1.4034 (0.0031) 121.83 (0.21) H42 0.9500 119.09 119.09 C42 - C41 C43 C43 - Distance Angles C44 1.3788 (0.0033) C42 1.4034 (0.0031) 120.83 (0.21) C47 1.4969 (0.0033) 119.65 (0.21) 119.50 (0.21) C43 - C44 C42 C44 - Distance Angles C43 1.3788 (0.0033) C45 1.3939 (0.0033) 118.34 (0.21) H44 0.9500 120.83 120.83 C44 - C43 C45 C45 - Distance Angles C46 1.3808 (0.0031) C44 1.3939 (0.0033) 120.61 (0.21) C48 1.4891 (0.0034) 121.43 (0.22) 117.92 (0.21) C45 - C46 C44 C46 - Distance Angles C45 1.3808 (0.0032) C41 1.4085 (0.0030) 122.35 (0.21) H46 0.9500 118.83 118.83 C46 - C45 C41 C47 - Distance Angles F41 1.3247 (0.0029) F43 1.3361 (0.0030) 108.37 (0.21) F42 1.3473 (0.0029) 104.77 (0.21) 104.53 (0.20) C43 1.4969 (0.0033) 113.72 (0.20) 112.87 (0.22) 111.86 (0.20) C47 - F41 F43 F42 C48 - Distance Angles F45 1.3323 (0.0032) F44 1.3327 (0.0031) 107.33 (0.23) F46 1.3360 (0.0030) 105.64 (0.23) 105.32 (0.21) C45 1.4891 (0.0034) 113.42 (0.21) 111.94 (0.22) 112.63 (0.21) C48 - F45 F44 F46 C51 - Distance Angles C52 1.3969 (0.0030) C56 1.4057 (0.0030) 115.31 (0.20) B21 1.6364 (0.0032) 125.19 (0.20) 119.48 (0.19) C51 - C52 C56 C52 - Distance Angles C53 1.3925 (0.0034) C51 1.3969 (0.0030) 122.15 (0.22) H52 0.9500 118.93 118.93 C52 - C53 C51 C53 - Distance Angles C54 1.3803 (0.0037) C52 1.3925 (0.0034) 120.96 (0.22) C57 1.4967 (0.0036) 119.35 (0.24) 119.67 (0.24) C53 - C54 C52 C54 - Distance Angles C55 1.3794 (0.0033) C53 1.3803 (0.0037) 118.41 (0.23) H54 0.9500 120.79 120.79 C54 - C55 C53 C55 - Distance Angles C54 1.3794 (0.0033) C56 1.3880 (0.0031) 120.49 (0.22) C58 1.4969 (0.0034) 120.07 (0.22) 119.38 (0.21) C55 - C54 C56 C56 - Distance Angles C55 1.3880 (0.0031) C51 1.4057 (0.0031) 122.62 (0.20) H56 0.9500 118.69 118.69 C56 - C55 C51 C57 - Distance Angles F51B_b 1.2301 (0.0119) F53B_b 1.2969 (0.0120) 109.30 (1.06) F52A_a 1.3181 (0.0047) 43.66 (0.96) 135.45 (0.74) F53A_a 1.3113 (0.0037) 127.56 (0.75) 52.60 (0.88) 109.93 (0.37) F51A_a 1.3383 (0.0046) 59.79 (0.99) 56.75 (0.97) 102.32 (0.31) 104.98 (0.37) F52B_b 1.3857 (0.0107) 104.06 (1.01) 102.22 (0.95) 65.45 (0.73) 51.14 (0.63) 137.68 (0.52) C53 1.4967 (0.0036) 118.52 (0.73) 111.63 (0.75) 112.81 (0.31) 113.64 (0.27) 112.32 (0.29) 109.62 (0.52) C57 - F51B_b F53B_b F52A_a F53A_a F51A_a F52B_b C58 - Distance Angles F54 1.3035 (0.0030) F55 1.3239 (0.0033) 107.82 (0.27) F56 1.3257 (0.0031) 106.29 (0.24) 103.52 (0.23) C55 1.4969 (0.0034) 113.70 (0.22) 111.63 (0.22) 113.19 (0.22) C58 - F54 F55 F56 B21 - Distance Angles C31 1.6353 (0.0032) C51 1.6364 (0.0032) 106.78 (0.17) C21 1.6484 (0.0031) 111.37 (0.17) 111.63 (0.17) C41 1.6488 (0.0031) 111.36 (0.17) 111.92 (0.17) 103.88 (0.17) B21 - C31 C51 C21 F21 - Distance Angles C27 1.3276 (0.0027) F21 - F22 - Distance Angles C27 1.3344 (0.0028) F22 - F23 - Distance Angles C27 1.3328 (0.0027) F23 - F24 - Distance Angles C28 1.3420 (0.0027) F24 - F25 - Distance Angles C28 1.3399 (0.0027) F25 - F26 - Distance Angles C28 1.3264 (0.0026) F26 - F31 - Distance Angles C37 1.3441 (0.0025) F31 - F32 - Distance Angles C37 1.3408 (0.0025) F32 - F33 - Distance Angles C37 1.3290 (0.0025) F33 - F34 - Distance Angles C38 1.3413 (0.0030) F34 - F35 - Distance Angles C38 1.3369 (0.0030) F35 - F36 - Distance Angles C38 1.3313 (0.0028) F36 - F41 - Distance Angles C47 1.3247 (0.0029) F41 - F42 - Distance Angles C47 1.3473 (0.0029) F42 - F43 - Distance Angles C47 1.3361 (0.0030) F43 - F44 - Distance Angles C48 1.3327 (0.0031) F44 - F45 - Distance Angles C48 1.3323 (0.0032) F45 - F46 - Distance Angles C48 1.3360 (0.0030) F46 - F51A_a - Distance Angles C57 1.3383 (0.0046) F51A_a - F52A_a - Distance Angles C57 1.3181 (0.0047) F52A_a - F53A_a - Distance Angles C57 1.3113 (0.0037) F53A_a - F51B_b - Distance Angles C57 1.2301 (0.0119) F51B_b - F52B_b - Distance Angles C57 1.3857 (0.0107) F52B_b - F53B_b - Distance Angles C57 1.2969 (0.0120) F53B_b - F54 - Distance Angles C58 1.3035 (0.0030) F54 - F55 - Distance Angles C58 1.3239 (0.0033) F55 - F56 - Distance Angles C58 1.3257 (0.0031) F56 - FMAP and GRID set by program FMAP 2 2 88 GRID -1.176 -1 -1 1.176 1 1 R1 = 0.0654 for 10558 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.57 at 0.2209 0.6152 0.2869 [ 0.98 A from F43 ] Deepest hole -0.55 at 0.2426 0.1416 0.2115 [ 0.94 A from F55 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 7392 /119619 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2209 0.6152 0.2869 1.00000 0.05 0.57 0.98 F43 1.36 C47 1.53 F41 2.41 C43 Q2 1 -0.0933 0.9367 -0.2273 1.00000 0.05 0.52 0.92 F54 1.27 C58 1.52 F55 2.25 C55 Q3 1 -0.0928 0.8756 0.2149 1.00000 0.05 0.49 1.15 F45 1.52 C48 1.60 F44 2.05 H7A Q4 1 -0.1265 0.9283 -0.2210 1.00000 0.05 0.43 1.07 F55 1.18 C58 1.30 F54 2.21 C55 Q5 1 -0.0063 0.8895 -0.2431 1.00000 0.05 0.41 0.67 F54 1.31 C58 1.82 F56 2.19 C55 Q6 1 -0.0483 0.8453 -0.2530 1.00000 0.05 0.41 0.89 F56 1.19 C58 1.39 F54 2.25 F55 Q7 1 -0.3697 0.8688 -0.1028 1.00000 0.05 0.40 0.98 F22 1.49 C27 1.66 F21 2.26 H22 Q8 1 0.1418 1.0367 -0.0115 1.00000 0.05 0.38 0.76 F52B 0.89 F52A 1.48 C57 1.73 F51B Q9 1 0.2790 0.9831 -0.0525 1.00000 0.05 0.37 0.58 F53B 0.65 F53A 1.36 C57 1.74 F52B Q10 1 -0.4884 0.8561 -0.0124 1.00000 0.05 0.35 0.96 F23 1.36 C27 1.52 F21 2.34 C23 Shortest distances between peaks (including symmetry equivalents) 2 4 0.48 5 6 0.99 2 5 1.49 4 5 1.80 2 6 1.96 4 6 2.05 8 9 2.29 7 10 2.61 1 5 2.68 Time profile in seconds ----------------------- 0.09: Read and process instructions 0.00: Fit rigid groups 0.01: Interpret restraints etc. 0.00: Generate connectivity array 0.01: 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. 7.80: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.01: OSF, H-atoms from difference map 0.08: Set up l.s. refinement 0.00: Generate idealized H-atoms 32.27: Structure factors and derivatives 156.27: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.41: Apply other restraints 14.13: Solve l.s. equations 0.00: Generate HTAB table 0.15: Other dependent quantities, CIF, tables 0.36: Analysis of variance 0.10: Merge reflections for Fourier and .fcf 0.27: Fourier summations 0.10: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2005src1438 finished at 16:43:14 Total CPU time: 212.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++