+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 04src1114 started at 21:44:38 on 20-Feb-2005 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 04src1114 in P-1 CELL 0.71073 11.0194 13.2296 16.9834 110.038 93.940 109.791 ZERR 2.00 0.0006 0.0021 0.0040 0.011 0.010 0.012 LATT 1 SFAC C H N O CL MN UNIT 76 76 32 20 4 2 V = 2140.29 F(000) = 1034.0 Mu = 0.51 mm-1 Cell Wt = 2009.37 Rho = 1.559 MERG 2 OMIT -3.00 55.00 OMIT -2 -2 2 OMIT -2 -2 3 EXTI 0.00417 SHEL 7 0.77 DFIX 0.84 0.01 O1 H1WA O1 H1WB O2 H2WA O2 H2WB DANG 1.35 0.01 H1WA H1WB H2WA H2WB DANG -2.65 0.04 MN1 H1WA MN1 H1WB MN1 H2WA MN1 H2WB DELU 0.01 SIMU 0.01 FMAP 2 PLAN 5 ACTA SIZE 0.04 0.16 0.42 BOND $H BUMP 0.01000 WGHT 0.09120 4.29040 L.S. 20 TEMP -153.00 FVAR 0.55757 0.80404 MOLE 1 C1 1 0.777601 -0.293317 0.299763 11.00000 0.03446 0.02516 = 0.03552 0.00428 0.01167 0.00675 AFIX 43 H1 2 0.720239 -0.307864 0.249250 11.00000 -1.20000 AFIX 0 C2 1 0.852141 -0.359472 0.294067 11.00000 0.04301 0.02426 = 0.04693 0.00172 0.01841 0.00897 AFIX 43 H2 2 0.846557 -0.418078 0.240810 11.00000 -1.20000 AFIX 0 C3 1 0.934744 -0.339096 0.366885 11.00000 0.03922 0.02585 = 0.05958 0.01286 0.02196 0.01558 AFIX 43 H3 2 0.986612 -0.384144 0.364887 11.00000 -1.20000 AFIX 0 C4 1 0.941712 -0.252500 0.443055 11.00000 0.03166 0.02335 = 0.04818 0.01328 0.01322 0.01393 AFIX 43 H4 2 0.998412 -0.237280 0.494072 11.00000 -1.20000 AFIX 0 C5 1 0.864601 -0.187536 0.444346 11.00000 0.02530 0.02034 = 0.03829 0.01190 0.01138 0.00783 C6 1 0.871345 -0.090584 0.523971 11.00000 0.02329 0.01947 = 0.03211 0.01201 0.00781 0.00732 C7 1 0.951976 -0.060906 0.601526 11.00000 0.02711 0.02632 = 0.03706 0.01504 0.00415 0.01228 AFIX 43 H7 2 1.003405 -0.104659 0.605250 11.00000 -1.20000 AFIX 0 C8 1 0.957790 0.031385 0.672907 11.00000 0.02958 0.02936 = 0.03042 0.01306 0.00048 0.01056 AFIX 43 H8 2 1.012554 0.051716 0.726146 11.00000 -1.20000 AFIX 0 C9 1 0.882732 0.094056 0.665962 11.00000 0.02894 0.02287 = 0.02698 0.00847 0.00406 0.00979 AFIX 43 H9 2 0.884680 0.158664 0.713919 11.00000 -1.20000 AFIX 0 C10 1 0.804384 0.059520 0.586613 11.00000 0.02144 0.02114 = 0.02759 0.01165 0.00458 0.00833 C11 1 0.724672 0.126977 0.575884 11.00000 0.01967 0.02127 = 0.02557 0.01188 0.00519 0.00674 C12 1 0.504164 0.119507 0.415022 11.00000 0.02859 0.02121 = 0.02222 0.00876 0.00604 0.00968 C13 1 0.433782 0.197163 0.414046 11.00000 0.02585 0.02259 = 0.02533 0.01257 0.00380 0.00871 C14 1 0.355266 0.184896 0.341220 11.00000 0.03094 0.02672 = 0.02551 0.01232 0.00234 0.00686 AFIX 43 H14 2 0.344812 0.125380 0.287267 11.00000 -1.20000 AFIX 0 C15 1 0.292630 0.261343 0.349054 11.00000 0.03017 0.03254 = 0.03063 0.01742 -0.00129 0.01016 AFIX 43 H15 2 0.237794 0.254298 0.300188 11.00000 -1.20000 AFIX 0 C16 1 0.309601 0.347757 0.427632 11.00000 0.02474 0.02759 = 0.03764 0.01869 0.00213 0.00970 AFIX 43 H16 2 0.267027 0.400797 0.433876 11.00000 -1.20000 AFIX 0 C17 1 0.391347 0.355258 0.498058 11.00000 0.02362 0.02176 = 0.03184 0.01578 0.00485 0.00825 C18 1 0.417009 0.443778 0.586074 11.00000 0.02219 0.01958 = 0.03385 0.01353 0.00572 0.00728 C19 1 0.361166 0.527273 0.607656 11.00000 0.02601 0.02201 = 0.04276 0.01514 0.00422 0.00958 AFIX 43 H19 2 0.304030 0.530988 0.565161 11.00000 -1.20000 AFIX 0 C20 1 0.390287 0.603806 0.691292 11.00000 0.03006 0.02408 = 0.04468 0.01271 0.00628 0.01413 AFIX 43 H20 2 0.353367 0.661367 0.707339 11.00000 -1.20000 AFIX 0 C21 1 0.473226 0.597031 0.752008 11.00000 0.03034 0.01863 = 0.03548 0.00828 0.00613 0.00910 AFIX 43 H21 2 0.493927 0.649125 0.810318 11.00000 -1.20000 AFIX 0 C22 1 0.525743 0.512384 0.725979 11.00000 0.02548 0.01666 = 0.03037 0.00913 0.00529 0.00659 C23 1 0.613958 0.493733 0.785747 11.00000 0.02819 0.01792 = 0.02917 0.00793 0.00376 0.00693 C24 1 0.713634 0.294044 0.817807 11.00000 0.03505 0.02123 = 0.01890 0.00726 0.00497 0.01165 C25 1 0.833739 0.294589 0.864698 11.00000 0.03382 0.01958 = 0.02072 0.00709 0.00127 0.00827 C26 1 0.828884 0.199091 0.883379 11.00000 0.04140 0.02377 = 0.03609 0.01378 -0.00946 0.00274 AFIX 43 H26 2 0.747790 0.134870 0.871059 11.00000 -1.20000 AFIX 0 C27 1 0.945790 0.200036 0.920555 11.00000 0.04980 0.03220 = 0.05381 0.02228 -0.00901 0.00812 AFIX 43 H27 2 0.946570 0.134571 0.931659 11.00000 -1.20000 AFIX 0 C28 1 1.060700 0.296970 0.941177 11.00000 0.04041 0.03546 = 0.04808 0.01791 -0.01027 0.00915 AFIX 43 H28 2 1.141546 0.299352 0.966813 11.00000 -1.20000 AFIX 0 C29 1 1.056221 0.391028 0.923832 11.00000 0.03518 0.02607 = 0.02495 0.00827 -0.00159 0.00819 C30 1 1.176929 0.496979 0.944181 11.00000 0.03689 0.02493 = 0.02255 0.00491 0.00157 0.00971 C31 1 1.178522 0.582365 0.914156 11.00000 0.03927 0.03049 = 0.03142 0.01212 0.00423 0.00861 AFIX 43 H31 2 1.100875 0.575085 0.880798 11.00000 -1.20000 AFIX 0 C32 1 1.294331 0.678172 0.933303 11.00000 0.04823 0.03235 = 0.03846 0.01456 0.00799 0.00409 AFIX 43 H32 2 1.297620 0.737629 0.913226 11.00000 -1.20000 AFIX 0 C33 1 1.405276 0.686164 0.982101 11.00000 0.03729 0.03696 = 0.03713 0.00769 0.00785 -0.00023 AFIX 43 H33 2 1.486420 0.750870 0.995930 11.00000 -1.20000 AFIX 0 C34 1 1.395859 0.598739 1.010176 11.00000 0.03148 0.04124 = 0.03132 0.00489 0.00302 0.00603 AFIX 43 H34 2 1.472458 0.604895 1.043919 11.00000 -1.20000 AFIX 0 N1 3 0.781877 -0.209552 0.372868 11.00000 0.02845 0.02189 = 0.03246 0.00589 0.00825 0.00791 N2 3 0.797209 -0.030509 0.516811 11.00000 0.02184 0.01963 = 0.02732 0.00968 0.00553 0.00726 N3 3 0.729071 0.214931 0.634600 11.00000 0.01522 0.00709 = 0.01374 0.00143 0.00035 0.00471 N4 3 0.648608 0.085635 0.497981 11.00000 0.02704 0.02122 = 0.02227 0.00811 0.00505 0.01302 AFIX 43 H4A 2 0.644474 0.022143 0.456056 11.00000 -1.20000 AFIX 0 N5 3 0.577211 0.150059 0.488386 11.00000 0.02538 0.02105 = 0.02400 0.01083 0.00523 0.01188 N6 3 0.486162 0.027356 0.343371 11.00000 0.04559 0.03082 = 0.02678 0.00324 -0.00470 0.01934 AFIX 93 H6A 2 0.526576 -0.019711 0.343464 11.00000 -1.20000 H6B 2 0.433917 0.013858 0.296187 11.00000 -1.20000 AFIX 0 N7 3 0.451161 0.281341 0.490755 11.00000 0.02406 0.02094 = 0.02616 0.01123 0.00484 0.00907 N8 3 0.498410 0.437371 0.644475 11.00000 0.02681 0.01801 = 0.02900 0.01040 0.00437 0.00861 N9 3 0.655957 0.569308 0.867153 11.00000 0.04065 0.02340 = 0.02720 0.00356 -0.00072 0.01537 AFIX 93 H9A 2 0.706941 0.559022 0.903382 11.00000 -1.20000 H9B 2 0.632700 0.629489 0.884667 11.00000 -1.20000 AFIX 0 N10 3 0.640977 0.401776 0.751878 11.00000 0.03094 0.02033 = 0.02435 0.00731 -0.00056 0.01118 N11 3 0.734267 0.394244 0.807584 11.00000 0.03153 0.01779 = 0.02402 0.00531 -0.00269 0.00835 AFIX 43 H11 2 0.807013 0.455775 0.836106 11.00000 -1.20000 AFIX 0 N12 3 0.607866 0.210868 0.792418 11.00000 0.01932 0.01189 = 0.01615 0.00610 -0.00142 0.00307 AFIX 93 H12A 2 0.539304 0.214568 0.765548 11.00000 -1.20000 H12B 2 0.600239 0.147255 0.801000 11.00000 -1.20000 AFIX 0 N13 3 0.945476 0.388538 0.883979 11.00000 0.03034 0.02261 = 0.02127 0.00792 0.00183 0.00820 N14 3 1.284124 0.504686 0.992584 11.00000 0.03442 0.03386 = 0.02886 0.00748 0.00127 0.01070 O1 4 0.435419 0.161765 0.643395 11.00000 0.02763 0.02306 = 0.02425 0.00850 0.00529 0.00816 O2 4 0.760596 0.425031 0.588021 11.00000 0.03149 0.03496 = 0.05783 0.02794 0.00772 0.01259 MN1 6 0.587598 0.297877 0.608294 11.00000 0.02498 0.01779 = 0.02266 0.00827 0.00242 0.00942 H1WA 2 0.381630 0.182801 0.673442 11.00000 -1.50000 H1WB 2 0.398256 0.155852 0.594640 11.00000 -1.50000 H2WA 2 0.784795 0.397016 0.543401 11.00000 -1.50000 H2WB 2 0.825445 0.466281 0.628093 11.00000 -1.50000 MOLE 2 O41 4 0.720508 0.015338 0.979349 11.00000 0.10970 0.03186 = 0.03892 0.00886 0.01544 0.01781 O42 4 0.690714 -0.179719 0.939494 11.00000 0.09762 0.03223 = 0.06655 0.02365 0.02318 0.01931 O43 4 0.557570 -0.129285 0.859702 11.00000 0.06278 0.05732 = 0.09616 0.00820 -0.00002 0.02465 O44 4 0.779797 -0.079899 0.854829 11.00000 0.06594 0.06053 = 0.03839 0.01902 0.01518 0.00827 CL41 5 0.688097 -0.092231 0.909380 11.00000 0.06558 0.02342 = 0.03846 0.00819 0.01398 0.00556 MOLE 3 PART 1 O51 4 1.004475 0.287708 0.373660 21.00000 0.04296 0.07058 = 0.06050 0.04246 0.02254 0.03800 O52 4 0.799727 0.248249 0.298583 21.00000 0.05122 0.06134 = 0.06983 -0.00808 -0.01464 0.02720 O53 4 0.924218 0.434937 0.396305 21.00000 0.06319 0.03524 = 0.07650 0.01704 0.01089 0.01788 O54 4 0.833508 0.292884 0.447567 21.00000 0.06222 0.08722 = 0.07651 0.04603 0.04192 0.03636 CL51 5 0.890175 0.314082 0.377660 21.00000 0.02837 0.03445 = 0.04474 0.01711 0.00822 0.01686 PART 2 SAME O51 > CL51 O56 4 0.851290 0.307836 0.239193 -21.00000 0.03265 0.06043 = 0.09525 0.03726 -0.00784 0.00711 O57 4 1.033506 0.381364 0.348774 -21.00000 0.05010 0.09208 = 0.05270 0.02708 -0.00027 -0.00291 O58 4 1.051535 0.445342 0.240955 -21.00000 0.06062 0.05457 = 0.06667 0.02744 0.01245 -0.00151 O59 4 1.032291 0.260055 0.207892 -21.00000 0.06392 0.06308 = 0.08944 0.00006 0.00503 0.02849 CL56 5 0.990594 0.345605 0.258946 -21.00000 0.03740 0.03923 = 0.04512 0.02017 0.00297 0.01298 MOLE 4 PART 1 C61 1 0.681357 -0.093236 1.167489 21.00000 0.05270 0.09534 = 0.05314 0.03867 0.01476 0.02471 C62 1 0.616024 -0.015318 1.155686 21.00000 0.05084 0.07098 = 0.03958 0.03249 0.01434 0.01365 AFIX 137 H62A 2 0.652827 0.016361 1.114290 21.00000 -1.50000 H62B 2 0.631542 0.048904 1.210732 21.00000 -1.50000 H62C 2 0.520975 -0.060259 1.134319 21.00000 -1.50000 AFIX 0 N61 3 0.731268 -0.154627 1.173568 21.00000 0.08278 0.12963 = 0.10899 0.07791 0.00866 0.05356 PART 2 SAME C61 > N61 C63 1 0.710390 -0.093202 1.144597 -21.00000 0.06766 0.10959 = 0.07707 0.03093 0.00862 0.02742 C64 1 0.621744 -0.032372 1.127832 -21.00000 0.06375 0.07897 = 0.07497 0.01140 0.01272 0.02093 AFIX 137 H64A 2 0.578898 -0.068616 1.066999 -21.00000 -1.50000 H64B 2 0.675099 0.050404 1.143134 -21.00000 -1.50000 H64C 2 0.554371 -0.039882 1.162608 -21.00000 -1.50000 AFIX 0 N63 3 0.797275 -0.123967 1.128958 -21.00000 0.06804 0.12558 = 0.10414 0.03728 -0.01193 0.03926 MOLE 5 PART 1 SAME C61 > N61 C71 1 1.035935 0.305223 0.192598 21.00000 0.04327 0.04769 = 0.04414 0.02560 0.00858 0.01535 C72 1 0.971893 0.176922 0.151501 21.00000 0.05355 0.04910 = 0.05775 0.00245 -0.00162 0.01355 AFIX 137 H72A 2 0.898377 0.154555 0.104848 21.00000 -1.50000 H72B 2 0.938588 0.145905 0.193967 21.00000 -1.50000 H72C 2 1.036164 0.145058 0.128383 21.00000 -1.50000 AFIX 0 N71 3 1.084159 0.401819 0.224486 21.00000 0.05249 0.04265 = 0.06408 0.03206 0.01332 0.01112 PART 2 SAME C61 > N61 C73 1 0.804283 0.249309 0.391391 -21.00000 0.05979 0.06544 = 0.07258 0.01918 0.00844 0.00731 C74 1 0.771420 0.124886 0.329907 -21.00000 0.04223 0.06995 = 0.08624 0.03570 0.04213 0.01892 AFIX 137 H74A 2 0.727981 0.071117 0.356581 -21.00000 -1.50000 H74B 2 0.852767 0.115162 0.316214 -21.00000 -1.50000 H74C 2 0.712264 0.107935 0.277175 -21.00000 -1.50000 AFIX 0 N73 3 0.826482 0.344224 0.439823 -21.00000 0.06012 0.07161 = 0.06389 0.03710 0.03251 0.04655 HKLF 4 Covalent radii and connectivity table for 04src1114 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 CL 0.990 MN 1.370 C1 - N1 C2 C2 - C3 C1 C3 - C2 C4 C4 - C3 C5 C5 - N1 C4 C6 C6 - N2 C7 C5 C7 - C8 C6 C8 - C7 C9 C9 - C8 C10 C10 - N2 C9 C11 C11 - N3 N4 C10 C12 - N5 N6 C13 C13 - N7 C14 C12 C14 - C15 C13 C15 - C16 C14 C16 - C15 C17 C17 - N7 C16 C18 C18 - N8 C19 C17 C19 - C20 C18 C20 - C19 C21 C21 - C20 C22 C22 - N8 C21 C23 C23 - N10 N9 C22 C24 - N12 N11 C25 C25 - N13 C26 C24 C26 - C27 C25 C27 - C28 C26 C28 - C27 C29 C29 - N13 C28 C30 C30 - N14 C31 C29 C31 - C32 C30 C32 - C33 C31 C33 - C34 C32 C34 - N14 C33 N1 - C1 C5 N2 - C10 C6 N3 - C11 Mn1 N4 - C11 N5 N5 - C12 N4 Mn1 N6 - C12 N7 - C17 C13 Mn1 N8 - C18 C22 Mn1 N9 - C23 N10 - C23 N11 Mn1 N11 - C24 N10 N12 - C24 N13 - C29 C25 N14 - C30 C34 O1 - Mn1 O2 - Mn1 Mn1 - O2 N5 N10 N3 O1 N8 N7 O41 - Cl41 O42 - Cl41 O43 - Cl41 O44 - Cl41 Cl41 - O41 O44 O42 O43 O51_a - Cl51_a O52_a - Cl51_a O53_a - Cl51_a O54_a - Cl51_a Cl51_a - O52_a O51_a O53_a O54_a O56_b - Cl56_b O57_b - Cl56_b O58_b - Cl56_b O59_b - Cl56_b Cl56_b - O59_b O58_b O56_b O57_b C61_a - N61_a C62_a C62_a - C61_a N61_a - C61_a C63_b - N63_b C64_b C64_b - C63_b N63_b - C63_b C71_a - N71_a C72_a C72_a - C71_a N71_a - C71_a C73_b - N73_b C74_b C74_b - C73_b N73_b - C73_b 42164 Reflections read, of which 112 rejected -14 =< h =< 14, -17 =< k =< 17, -22 =< l =< 22, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 9802 Unique reflections, of which 0 suppressed R(int) = 0.0542 R(sigma) = 0.0520 Friedel opposites merged Maximum memory for data reduction = 7025 / 100470 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 = 8940 / 1023624 wR2 = 0.1885 before cycle 1 for 9802 data and 721 / 721 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint 2.9610 3.0000 -0.0390 0.0100 BUMP C24 N3 2.0241 2.1000 -0.0759 0.0100 BUMP H4A H6A 2.0682 2.1000 -0.0318 0.0100 BUMP H14 H6B 2.0564 2.1000 -0.0436 0.0100 BUMP H21 H9B 2.0332 2.1000 -0.0668 0.0100 BUMP H26 H12B 2.8023 2.6500 0.1523 0.0400 DANG Mn1 H1WA 2.2176 2.6500 -0.4324 0.0400 DANG Mn1 H1WB 1.3049 1.3500 -0.0451 0.0100 DANG H1WA H1WB 0.0624 0.0200 SAME/SADI C71_a N71_a C63_b N63_b -0.0314 0.0100 SIMU U11 Cl51_a C73_b -0.0310 0.0100 SIMU U22 Cl51_a C73_b Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 20. 4. 6. 28. 0. 0. 0. 204. 564. 0. 0. rms sigma 0.010 0.010 0.033 0.030 0.000 0.000 0.000 0.010 0.015 0.000 0.000 rms deviation 0.030 0.019 0.190 0.040 0.000 0.000 0.000 0.005 0.014 0.000 0.000 GooF = S = 1.026; Restrained GooF = 1.022 for 826 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0912 * P )^2 + 4.29 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55758 0.00139 0.010 OSF 2 0.80415 0.00254 0.042 FVAR 2 3 0.00418 0.00132 0.008 EXTI Mean shift/esd = 0.022 Maximum = -0.510 for U22 C63_b Max. shift = 0.004 A for C63_b Max. dU =-0.003 for C63_b Least-squares cycle 2 Maximum vector length = 511 Memory required = 8940 / 1023624 wR2 = 0.1886 before cycle 2 for 9802 data and 721 / 721 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint 2.9611 3.0000 -0.0389 0.0100 BUMP C24 N3 2.0242 2.1000 -0.0758 0.0100 BUMP H4A H6A 2.0682 2.1000 -0.0318 0.0100 BUMP H14 H6B 2.0565 2.1000 -0.0435 0.0100 BUMP H21 H9B 2.0335 2.1000 -0.0665 0.0100 BUMP H26 H12B 2.8017 2.6500 0.1517 0.0400 DANG Mn1 H1WA 2.2176 2.6500 -0.4324 0.0400 DANG Mn1 H1WB 1.3051 1.3500 -0.0449 0.0100 DANG H1WA H1WB 0.0618 0.0200 SAME/SADI C71_a N71_a C63_b N63_b -0.0313 0.0100 SIMU U11 Cl51_a C73_b -0.0309 0.0100 SIMU U22 Cl51_a C73_b Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 19. 4. 6. 28. 0. 0. 0. 204. 564. 0. 0. rms sigma 0.010 0.010 0.033 0.030 0.000 0.000 0.000 0.010 0.015 0.000 0.000 rms deviation 0.031 0.019 0.190 0.040 0.000 0.000 0.000 0.005 0.014 0.000 0.000 GooF = S = 1.026; Restrained GooF = 1.022 for 825 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0912 * P )^2 + 4.29 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55756 0.00139 -0.020 OSF 2 0.80423 0.00254 0.034 FVAR 2 3 0.00418 0.00132 -0.001 EXTI Mean shift/esd = 0.010 Maximum = -0.176 for U22 C63_b Max. shift = 0.004 A for C63_b Max. dU =-0.001 for C63_b Least-squares cycle 3 Maximum vector length = 511 Memory required = 8940 / 1023624 wR2 = 0.1886 before cycle 3 for 9802 data and 721 / 721 parameters Disagreeable restraints before cycle 3 Observed Target Error Sigma Restraint 2.9611 3.0000 -0.0389 0.0100 BUMP C24 N3 2.0244 2.1000 -0.0756 0.0100 BUMP H4A H6A 2.0682 2.1000 -0.0318 0.0100 BUMP H14 H6B 2.0565 2.1000 -0.0435 0.0100 BUMP H21 H9B 2.0335 2.1000 -0.0665 0.0100 BUMP H26 H12B 2.8010 2.6500 0.1510 0.0400 DANG Mn1 H1WA 2.2177 2.6500 -0.4323 0.0400 DANG Mn1 H1WB 1.3051 1.3500 -0.0449 0.0100 DANG H1WA H1WB 0.0624 0.0200 SAME/SADI C71_a N71_a C63_b N63_b -0.0312 0.0100 SIMU U11 Cl51_a C73_b -0.0308 0.0100 SIMU U22 Cl51_a C73_b Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 19. 4. 6. 28. 0. 0. 0. 204. 564. 0. 0. rms sigma 0.010 0.010 0.033 0.030 0.000 0.000 0.000 0.010 0.015 0.000 0.000 rms deviation 0.031 0.019 0.190 0.040 0.000 0.000 0.000 0.005 0.014 0.000 0.000 GooF = S = 1.026; Restrained GooF = 1.022 for 825 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0912 * P )^2 + 4.29 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55754 0.00139 -0.014 OSF 2 0.80423 0.00254 -0.002 FVAR 2 3 0.00417 0.00132 -0.003 EXTI Mean shift/esd = 0.004 Maximum = 0.114 for z C64_b Max. shift = 0.005 A for C63_b Max. dU = 0.000 for C62_a Least-squares cycle 4 Maximum vector length = 511 Memory required = 8940 / 1023624 wR2 = 0.1886 before cycle 4 for 9802 data and 721 / 721 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint 2.9611 3.0000 -0.0389 0.0100 BUMP C24 N3 2.0244 2.1000 -0.0756 0.0100 BUMP H4A H6A 2.0682 2.1000 -0.0318 0.0100 BUMP H14 H6B 2.0565 2.1000 -0.0435 0.0100 BUMP H21 H9B 2.0336 2.1000 -0.0664 0.0100 BUMP H26 H12B 2.8006 2.6500 0.1506 0.0400 DANG Mn1 H1WA 2.2177 2.6500 -0.4323 0.0400 DANG Mn1 H1WB 1.3051 1.3500 -0.0449 0.0100 DANG H1WA H1WB 0.0635 0.0200 SAME/SADI C71_a N71_a C63_b N63_b -0.0312 0.0100 SIMU U11 Cl51_a C73_b -0.0308 0.0100 SIMU U22 Cl51_a C73_b Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 19. 4. 6. 28. 0. 0. 0. 204. 564. 0. 0. rms sigma 0.010 0.010 0.033 0.030 0.000 0.000 0.000 0.010 0.015 0.000 0.000 rms deviation 0.031 0.019 0.189 0.040 0.000 0.000 0.000 0.005 0.014 0.000 0.000 GooF = S = 1.026; Restrained GooF = 1.023 for 825 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0912 * P )^2 + 4.29 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55753 0.00139 -0.005 OSF 2 0.80420 0.00254 -0.009 FVAR 2 3 0.00417 0.00132 -0.002 EXTI Mean shift/esd = 0.002 Maximum = 0.062 for y C74_b Max. shift = 0.002 A for H64A_b Max. dU = 0.000 for C63_b Least-squares cycle 5 Maximum vector length = 511 Memory required = 8940 / 1023624 wR2 = 0.1886 before cycle 5 for 9802 data and 721 / 721 parameters Disagreeable restraints before cycle 5 Observed Target Error Sigma Restraint 2.9611 3.0000 -0.0389 0.0100 BUMP C24 N3 2.0244 2.1000 -0.0756 0.0100 BUMP H4A H6A 2.0682 2.1000 -0.0318 0.0100 BUMP H14 H6B 2.0565 2.1000 -0.0435 0.0100 BUMP H21 H9B 2.0336 2.1000 -0.0664 0.0100 BUMP H26 H12B 2.8003 2.6500 0.1503 0.0400 DANG Mn1 H1WA 2.2178 2.6500 -0.4322 0.0400 DANG Mn1 H1WB 1.3051 1.3500 -0.0449 0.0100 DANG H1WA H1WB 0.0631 0.0200 SAME/SADI C71_a N71_a C63_b N63_b -0.0312 0.0100 SIMU U11 Cl51_a C73_b -0.0308 0.0100 SIMU U22 Cl51_a C73_b Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 20. 4. 6. 28. 0. 0. 0. 204. 564. 0. 0. rms sigma 0.010 0.010 0.033 0.030 0.000 0.000 0.000 0.010 0.015 0.000 0.000 rms deviation 0.030 0.019 0.189 0.040 0.000 0.000 0.000 0.005 0.014 0.000 0.000 GooF = S = 1.026; Restrained GooF = 1.022 for 826 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0912 * P )^2 + 4.29 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55753 0.00139 0.001 OSF 2 0.80419 0.00254 -0.006 FVAR 2 3 0.00417 0.00132 0.000 EXTI Mean shift/esd = 0.001 Maximum = 0.031 for z C63_b Max. shift = 0.001 A for C63_b Max. dU = 0.000 for C64_b Least-squares cycle 6 Maximum vector length = 511 Memory required = 8940 / 1023624 wR2 = 0.1886 before cycle 6 for 9802 data and 721 / 721 parameters Disagreeable restraints before cycle 6 Observed Target Error Sigma Restraint 2.9611 3.0000 -0.0389 0.0100 BUMP C24 N3 2.0244 2.1000 -0.0756 0.0100 BUMP H4A H6A 2.0683 2.1000 -0.0317 0.0100 BUMP H14 H6B 2.0565 2.1000 -0.0435 0.0100 BUMP H21 H9B 2.0336 2.1000 -0.0664 0.0100 BUMP H26 H12B 2.8001 2.6500 0.1501 0.0400 DANG Mn1 H1WA 2.2177 2.6500 -0.4323 0.0400 DANG Mn1 H1WB 1.3051 1.3500 -0.0449 0.0100 DANG H1WA H1WB 0.0631 0.0200 SAME/SADI C71_a N71_a C63_b N63_b -0.0312 0.0100 SIMU U11 Cl51_a C73_b -0.0308 0.0100 SIMU U22 Cl51_a C73_b Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 20. 4. 6. 28. 0. 0. 0. 204. 564. 0. 0. rms sigma 0.010 0.010 0.033 0.030 0.000 0.000 0.000 0.010 0.015 0.000 0.000 rms deviation 0.030 0.019 0.189 0.040 0.000 0.000 0.000 0.005 0.014 0.000 0.000 GooF = S = 1.026; Restrained GooF = 1.022 for 826 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0912 * P )^2 + 4.29 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55753 0.00139 0.001 OSF 2 0.80418 0.00254 -0.003 FVAR 2 3 0.00417 0.00132 0.001 EXTI Mean shift/esd = 0.001 Maximum = -0.023 for tors H64A_b Max. shift = 0.001 A for C63_b Max. dU = 0.000 for C63_b Least-squares cycle 7 Maximum vector length = 511 Memory required = 8940 / 1023624 wR2 = 0.1886 before cycle 7 for 9802 data and 721 / 721 parameters Disagreeable restraints before cycle 7 Observed Target Error Sigma Restraint 2.9611 3.0000 -0.0389 0.0100 BUMP C24 N3 2.0243 2.1000 -0.0757 0.0100 BUMP H4A H6A 2.0683 2.1000 -0.0317 0.0100 BUMP H14 H6B 2.0565 2.1000 -0.0435 0.0100 BUMP H21 H9B 2.0336 2.1000 -0.0664 0.0100 BUMP H26 H12B 2.8000 2.6500 0.1500 0.0400 DANG Mn1 H1WA 2.2177 2.6500 -0.4323 0.0400 DANG Mn1 H1WB 1.3051 1.3500 -0.0449 0.0100 DANG H1WA H1WB 0.0631 0.0200 SAME/SADI C71_a N71_a C63_b N63_b -0.0312 0.0100 SIMU U11 Cl51_a C73_b -0.0308 0.0100 SIMU U22 Cl51_a C73_b Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 20. 4. 6. 28. 0. 0. 0. 204. 564. 0. 0. rms sigma 0.010 0.010 0.033 0.030 0.000 0.000 0.000 0.010 0.015 0.000 0.000 rms deviation 0.030 0.019 0.189 0.040 0.000 0.000 0.000 0.005 0.014 0.000 0.000 GooF = S = 1.026; Restrained GooF = 1.022 for 826 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0912 * P )^2 + 4.29 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55753 0.00139 0.001 OSF 2 0.80417 0.00254 -0.002 FVAR 2 3 0.00418 0.00132 0.001 EXTI Mean shift/esd = 0.001 Maximum = 0.013 for z C63_b Max. shift = 0.000 A for C63_b Max. dU = 0.000 for C63_b Least-squares cycle 8 Maximum vector length = 511 Memory required = 8940 / 1023624 wR2 = 0.1886 before cycle 8 for 9802 data and 721 / 721 parameters Disagreeable restraints before cycle 8 Observed Target Error Sigma Restraint 2.9611 3.0000 -0.0389 0.0100 BUMP C24 N3 2.0244 2.1000 -0.0756 0.0100 BUMP H4A H6A 2.0683 2.1000 -0.0317 0.0100 BUMP H14 H6B 2.0565 2.1000 -0.0435 0.0100 BUMP H21 H9B 2.0336 2.1000 -0.0664 0.0100 BUMP H26 H12B 2.7999 2.6500 0.1499 0.0400 DANG Mn1 H1WA 2.2178 2.6500 -0.4322 0.0400 DANG Mn1 H1WB 1.3051 1.3500 -0.0449 0.0100 DANG H1WA H1WB 0.0631 0.0200 SAME/SADI C71_a N71_a C63_b N63_b -0.0312 0.0100 SIMU U11 Cl51_a C73_b -0.0308 0.0100 SIMU U22 Cl51_a C73_b Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 20. 4. 6. 28. 0. 0. 0. 204. 564. 0. 0. rms sigma 0.010 0.010 0.033 0.030 0.000 0.000 0.000 0.010 0.015 0.000 0.000 rms deviation 0.030 0.019 0.189 0.040 0.000 0.000 0.000 0.005 0.014 0.000 0.000 GooF = S = 1.026; Restrained GooF = 1.023 for 826 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0912 * P )^2 + 4.29 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55753 0.00139 0.000 OSF 2 0.80417 0.00254 -0.002 FVAR 2 3 0.00418 0.00132 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.007 for z C63_b Max. shift = 0.000 A for N63_b Max. dU = 0.000 for C63_b Least-squares cycle 9 Maximum vector length = 511 Memory required = 8940 / 1023624 wR2 = 0.1886 before cycle 9 for 9802 data and 721 / 721 parameters Disagreeable restraints before cycle 9 Observed Target Error Sigma Restraint 2.9611 3.0000 -0.0389 0.0100 BUMP C24 N3 2.0244 2.1000 -0.0756 0.0100 BUMP H4A H6A 2.0683 2.1000 -0.0317 0.0100 BUMP H14 H6B 2.0565 2.1000 -0.0435 0.0100 BUMP H21 H9B 2.0336 2.1000 -0.0664 0.0100 BUMP H26 H12B 2.7999 2.6500 0.1499 0.0400 DANG Mn1 H1WA 2.2178 2.6500 -0.4322 0.0400 DANG Mn1 H1WB 1.3051 1.3500 -0.0449 0.0100 DANG H1WA H1WB 0.0631 0.0200 SAME/SADI C71_a N71_a C63_b N63_b -0.0312 0.0100 SIMU U11 Cl51_a C73_b -0.0308 0.0100 SIMU U22 Cl51_a C73_b Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 20. 4. 6. 28. 0. 0. 0. 204. 564. 0. 0. rms sigma 0.010 0.010 0.033 0.030 0.000 0.000 0.000 0.010 0.015 0.000 0.000 rms deviation 0.030 0.019 0.189 0.040 0.000 0.000 0.000 0.005 0.014 0.000 0.000 GooF = S = 1.026; Restrained GooF = 1.022 for 826 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0912 * P )^2 + 4.29 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55753 0.00139 0.000 OSF 2 0.80417 0.00254 -0.001 FVAR 2 3 0.00418 0.00132 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.005 for z C63_b Max. shift = 0.000 A for N63_b Max. dU = 0.000 for C74_b Least-squares cycle 10 Maximum vector length = 511 Memory required = 8940 / 1023624 wR2 = 0.1886 before cycle 10 for 9802 data and 721 / 721 parameters Disagreeable restraints before cycle 10 Observed Target Error Sigma Restraint 2.9611 3.0000 -0.0389 0.0100 BUMP C24 N3 2.0243 2.1000 -0.0757 0.0100 BUMP H4A H6A 2.0683 2.1000 -0.0317 0.0100 BUMP H14 H6B 2.0565 2.1000 -0.0435 0.0100 BUMP H21 H9B 2.0336 2.1000 -0.0664 0.0100 BUMP H26 H12B 2.7999 2.6500 0.1499 0.0400 DANG Mn1 H1WA 2.2178 2.6500 -0.4322 0.0400 DANG Mn1 H1WB 1.3051 1.3500 -0.0449 0.0100 DANG H1WA H1WB 0.0631 0.0200 SAME/SADI C71_a N71_a C63_b N63_b -0.0312 0.0100 SIMU U11 Cl51_a C73_b -0.0308 0.0100 SIMU U22 Cl51_a C73_b Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 20. 4. 6. 28. 0. 0. 0. 204. 564. 0. 0. rms sigma 0.010 0.010 0.033 0.030 0.000 0.000 0.000 0.010 0.015 0.000 0.000 rms deviation 0.030 0.019 0.189 0.040 0.000 0.000 0.000 0.005 0.014 0.000 0.000 GooF = S = 1.026; Restrained GooF = 1.022 for 826 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0912 * P )^2 + 4.29 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55753 0.00139 0.000 OSF 2 0.80416 0.00254 -0.001 FVAR 2 3 0.00418 0.00132 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.006 for z C64_b Max. shift = 0.000 A for C63_b Max. dU = 0.000 for C63_b Least-squares cycle 11 Maximum vector length = 511 Memory required = 8940 / 1023624 wR2 = 0.1886 before cycle 11 for 9802 data and 721 / 721 parameters Disagreeable restraints before cycle 11 Observed Target Error Sigma Restraint 2.9611 3.0000 -0.0389 0.0100 BUMP C24 N3 2.0243 2.1000 -0.0757 0.0100 BUMP H4A H6A 2.0683 2.1000 -0.0317 0.0100 BUMP H14 H6B 2.0565 2.1000 -0.0435 0.0100 BUMP H21 H9B 2.0336 2.1000 -0.0664 0.0100 BUMP H26 H12B 2.7998 2.6500 0.1498 0.0400 DANG Mn1 H1WA 2.2178 2.6500 -0.4322 0.0400 DANG Mn1 H1WB 1.3051 1.3500 -0.0449 0.0100 DANG H1WA H1WB 0.0631 0.0200 SAME/SADI C71_a N71_a C63_b N63_b -0.0312 0.0100 SIMU U11 Cl51_a C73_b -0.0308 0.0100 SIMU U22 Cl51_a C73_b Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 20. 4. 6. 28. 0. 0. 0. 204. 564. 0. 0. rms sigma 0.010 0.010 0.033 0.030 0.000 0.000 0.000 0.010 0.015 0.000 0.000 rms deviation 0.030 0.019 0.189 0.040 0.000 0.000 0.000 0.005 0.014 0.000 0.000 GooF = S = 1.026; Restrained GooF = 1.023 for 826 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0912 * P )^2 + 4.29 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55753 0.00139 0.000 OSF 2 0.80416 0.00254 -0.001 FVAR 2 3 0.00418 0.00132 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.003 for y C74_b Max. shift = 0.000 A for N63_b Max. dU = 0.000 for C63_b Least-squares cycle 12 Maximum vector length = 511 Memory required = 8940 / 1023624 wR2 = 0.1886 before cycle 12 for 9802 data and 721 / 721 parameters Disagreeable restraints before cycle 12 Observed Target Error Sigma Restraint 2.9611 3.0000 -0.0389 0.0100 BUMP C24 N3 2.0244 2.1000 -0.0756 0.0100 BUMP H4A H6A 2.0683 2.1000 -0.0317 0.0100 BUMP H14 H6B 2.0565 2.1000 -0.0435 0.0100 BUMP H21 H9B 2.0336 2.1000 -0.0664 0.0100 BUMP H26 H12B 2.7998 2.6500 0.1498 0.0400 DANG Mn1 H1WA 2.2177 2.6500 -0.4323 0.0400 DANG Mn1 H1WB 1.3051 1.3500 -0.0449 0.0100 DANG H1WA H1WB 0.0631 0.0200 SAME/SADI C71_a N71_a C63_b N63_b -0.0312 0.0100 SIMU U11 Cl51_a C73_b -0.0308 0.0100 SIMU U22 Cl51_a C73_b Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 20. 4. 6. 28. 0. 0. 0. 204. 564. 0. 0. rms sigma 0.010 0.010 0.033 0.030 0.000 0.000 0.000 0.010 0.015 0.000 0.000 rms deviation 0.030 0.019 0.189 0.040 0.000 0.000 0.000 0.005 0.014 0.000 0.000 GooF = S = 1.026; Restrained GooF = 1.022 for 826 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0912 * P )^2 + 4.29 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55753 0.00139 0.001 OSF 2 0.80416 0.00254 0.000 FVAR 2 3 0.00418 0.00132 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.005 for y H1WB Max. shift = 0.000 A for N63_b Max. dU = 0.000 for C74_b Least-squares cycle 13 Maximum vector length = 511 Memory required = 8940 / 1023624 wR2 = 0.1886 before cycle 13 for 9802 data and 721 / 721 parameters Disagreeable restraints before cycle 13 Observed Target Error Sigma Restraint 2.9611 3.0000 -0.0389 0.0100 BUMP C24 N3 2.0243 2.1000 -0.0757 0.0100 BUMP H4A H6A 2.0683 2.1000 -0.0317 0.0100 BUMP H14 H6B 2.0565 2.1000 -0.0435 0.0100 BUMP H21 H9B 2.0336 2.1000 -0.0664 0.0100 BUMP H26 H12B 2.7998 2.6500 0.1498 0.0400 DANG Mn1 H1WA 2.2178 2.6500 -0.4322 0.0400 DANG Mn1 H1WB 1.3051 1.3500 -0.0449 0.0100 DANG H1WA H1WB 0.0631 0.0200 SAME/SADI C71_a N71_a C63_b N63_b -0.0312 0.0100 SIMU U11 Cl51_a C73_b -0.0308 0.0100 SIMU U22 Cl51_a C73_b Summary of restraints applied in cycle 13 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 20. 4. 6. 28. 0. 0. 0. 204. 564. 0. 0. rms sigma 0.010 0.010 0.033 0.030 0.000 0.000 0.000 0.010 0.015 0.000 0.000 rms deviation 0.030 0.019 0.189 0.040 0.000 0.000 0.000 0.005 0.014 0.000 0.000 GooF = S = 1.026; Restrained GooF = 1.022 for 826 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0912 * P )^2 + 4.29 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55753 0.00139 0.001 OSF 2 0.80416 0.00254 0.000 FVAR 2 3 0.00418 0.00132 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.004 for z H1WA Max. shift = 0.000 A for H64C_b Max. dU = 0.000 for C74_b Least-squares cycle 14 Maximum vector length = 511 Memory required = 8940 / 1023624 wR2 = 0.1886 before cycle 14 for 9802 data and 721 / 721 parameters Disagreeable restraints before cycle 14 Observed Target Error Sigma Restraint 2.9611 3.0000 -0.0389 0.0100 BUMP C24 N3 2.0244 2.1000 -0.0756 0.0100 BUMP H4A H6A 2.0683 2.1000 -0.0317 0.0100 BUMP H14 H6B 2.0565 2.1000 -0.0435 0.0100 BUMP H21 H9B 2.0336 2.1000 -0.0664 0.0100 BUMP H26 H12B 2.7998 2.6500 0.1498 0.0400 DANG Mn1 H1WA 2.2178 2.6500 -0.4322 0.0400 DANG Mn1 H1WB 1.3051 1.3500 -0.0449 0.0100 DANG H1WA H1WB 0.0631 0.0200 SAME/SADI C71_a N71_a C63_b N63_b -0.0312 0.0100 SIMU U11 Cl51_a C73_b -0.0308 0.0100 SIMU U22 Cl51_a C73_b Summary of restraints applied in cycle 14 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 20. 4. 6. 28. 0. 0. 0. 204. 564. 0. 0. rms sigma 0.010 0.010 0.033 0.030 0.000 0.000 0.000 0.010 0.015 0.000 0.000 rms deviation 0.030 0.019 0.189 0.040 0.000 0.000 0.000 0.005 0.014 0.000 0.000 GooF = S = 1.026; Restrained GooF = 1.022 for 826 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0912 * P )^2 + 4.29 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55753 0.00139 -0.001 OSF 2 0.80416 0.00254 0.000 FVAR 2 3 0.00418 0.00132 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.004 for z C64_b Max. shift = 0.000 A for H64A_b Max. dU = 0.000 for C64_b Least-squares cycle 15 Maximum vector length = 511 Memory required = 8940 / 1023624 wR2 = 0.1886 before cycle 15 for 9802 data and 721 / 721 parameters Disagreeable restraints before cycle 15 Observed Target Error Sigma Restraint 2.9611 3.0000 -0.0389 0.0100 BUMP C24 N3 2.0243 2.1000 -0.0757 0.0100 BUMP H4A H6A 2.0683 2.1000 -0.0317 0.0100 BUMP H14 H6B 2.0565 2.1000 -0.0435 0.0100 BUMP H21 H9B 2.0336 2.1000 -0.0664 0.0100 BUMP H26 H12B 2.7998 2.6500 0.1498 0.0400 DANG Mn1 H1WA 2.2178 2.6500 -0.4322 0.0400 DANG Mn1 H1WB 1.3051 1.3500 -0.0449 0.0100 DANG H1WA H1WB 0.0631 0.0200 SAME/SADI C71_a N71_a C63_b N63_b -0.0312 0.0100 SIMU U11 Cl51_a C73_b -0.0308 0.0100 SIMU U22 Cl51_a C73_b Summary of restraints applied in cycle 15 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 20. 4. 6. 28. 0. 0. 0. 204. 564. 0. 0. rms sigma 0.010 0.010 0.033 0.030 0.000 0.000 0.000 0.010 0.015 0.000 0.000 rms deviation 0.030 0.019 0.189 0.040 0.000 0.000 0.000 0.005 0.014 0.000 0.000 GooF = S = 1.026; Restrained GooF = 1.022 for 826 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0912 * P )^2 + 4.29 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55753 0.00139 0.001 OSF 2 0.80416 0.00254 0.000 FVAR 2 3 0.00418 0.00132 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.003 for z H1WA Max. shift = 0.000 A for H64A_b Max. dU = 0.000 for C64_b Least-squares cycle 16 Maximum vector length = 511 Memory required = 8940 / 1023624 wR2 = 0.1886 before cycle 16 for 9802 data and 721 / 721 parameters Disagreeable restraints before cycle 16 Observed Target Error Sigma Restraint 2.9611 3.0000 -0.0389 0.0100 BUMP C24 N3 2.0243 2.1000 -0.0757 0.0100 BUMP H4A H6A 2.0683 2.1000 -0.0317 0.0100 BUMP H14 H6B 2.0565 2.1000 -0.0435 0.0100 BUMP H21 H9B 2.0336 2.1000 -0.0664 0.0100 BUMP H26 H12B 2.7998 2.6500 0.1498 0.0400 DANG Mn1 H1WA 2.2178 2.6500 -0.4322 0.0400 DANG Mn1 H1WB 1.3051 1.3500 -0.0449 0.0100 DANG H1WA H1WB 0.0631 0.0200 SAME/SADI C71_a N71_a C63_b N63_b -0.0312 0.0100 SIMU U11 Cl51_a C73_b -0.0308 0.0100 SIMU U22 Cl51_a C73_b Summary of restraints applied in cycle 16 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 20. 4. 6. 28. 0. 0. 0. 204. 564. 0. 0. rms sigma 0.010 0.010 0.033 0.030 0.000 0.000 0.000 0.010 0.015 0.000 0.000 rms deviation 0.030 0.019 0.189 0.040 0.000 0.000 0.000 0.005 0.014 0.000 0.000 GooF = S = 1.026; Restrained GooF = 1.022 for 826 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0912 * P )^2 + 4.29 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55753 0.00139 0.000 OSF 2 0.80416 0.00254 0.000 FVAR 2 3 0.00418 0.00132 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.004 for z H1WA Max. shift = 0.000 A for H1WA Max. dU = 0.000 for C74_b Least-squares cycle 17 Maximum vector length = 511 Memory required = 8940 / 1023624 wR2 = 0.1886 before cycle 17 for 9802 data and 721 / 721 parameters Disagreeable restraints before cycle 17 Observed Target Error Sigma Restraint 2.9611 3.0000 -0.0389 0.0100 BUMP C24 N3 2.0244 2.1000 -0.0756 0.0100 BUMP H4A H6A 2.0683 2.1000 -0.0317 0.0100 BUMP H14 H6B 2.0565 2.1000 -0.0435 0.0100 BUMP H21 H9B 2.0336 2.1000 -0.0664 0.0100 BUMP H26 H12B 2.7998 2.6500 0.1498 0.0400 DANG Mn1 H1WA 2.2178 2.6500 -0.4322 0.0400 DANG Mn1 H1WB 1.3051 1.3500 -0.0449 0.0100 DANG H1WA H1WB 0.0631 0.0200 SAME/SADI C71_a N71_a C63_b N63_b -0.0312 0.0100 SIMU U11 Cl51_a C73_b -0.0308 0.0100 SIMU U22 Cl51_a C73_b Summary of restraints applied in cycle 17 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 20. 4. 6. 28. 0. 0. 0. 204. 564. 0. 0. rms sigma 0.010 0.010 0.033 0.030 0.000 0.000 0.000 0.010 0.015 0.000 0.000 rms deviation 0.030 0.019 0.189 0.040 0.000 0.000 0.000 0.005 0.014 0.000 0.000 GooF = S = 1.026; Restrained GooF = 1.022 for 826 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0912 * P )^2 + 4.29 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55753 0.00139 0.000 OSF 2 0.80416 0.00254 0.000 FVAR 2 3 0.00418 0.00132 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for tors H62A_a Max. shift = 0.000 A for H64C_b Max. dU = 0.000 for C64_b Least-squares cycle 18 Maximum vector length = 511 Memory required = 8940 / 1023624 wR2 = 0.1886 before cycle 18 for 9802 data and 721 / 721 parameters Disagreeable restraints before cycle 18 Observed Target Error Sigma Restraint 2.9611 3.0000 -0.0389 0.0100 BUMP C24 N3 2.0243 2.1000 -0.0757 0.0100 BUMP H4A H6A 2.0683 2.1000 -0.0317 0.0100 BUMP H14 H6B 2.0565 2.1000 -0.0435 0.0100 BUMP H21 H9B 2.0336 2.1000 -0.0664 0.0100 BUMP H26 H12B 2.7998 2.6500 0.1498 0.0400 DANG Mn1 H1WA 2.2178 2.6500 -0.4322 0.0400 DANG Mn1 H1WB 1.3051 1.3500 -0.0449 0.0100 DANG H1WA H1WB 0.0631 0.0200 SAME/SADI C71_a N71_a C63_b N63_b -0.0312 0.0100 SIMU U11 Cl51_a C73_b -0.0308 0.0100 SIMU U22 Cl51_a C73_b Summary of restraints applied in cycle 18 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 20. 4. 6. 28. 0. 0. 0. 204. 564. 0. 0. rms sigma 0.010 0.010 0.033 0.030 0.000 0.000 0.000 0.010 0.015 0.000 0.000 rms deviation 0.030 0.019 0.189 0.040 0.000 0.000 0.000 0.005 0.014 0.000 0.000 GooF = S = 1.026; Restrained GooF = 1.022 for 826 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0912 * P )^2 + 4.29 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55753 0.00139 0.001 OSF 2 0.80416 0.00254 0.000 FVAR 2 3 0.00418 0.00132 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.002 for y C64_b Max. shift = 0.000 A for H64A_b Max. dU = 0.000 for C74_b Least-squares cycle 19 Maximum vector length = 511 Memory required = 8940 / 1023624 wR2 = 0.1886 before cycle 19 for 9802 data and 721 / 721 parameters Disagreeable restraints before cycle 19 Observed Target Error Sigma Restraint 2.9611 3.0000 -0.0389 0.0100 BUMP C24 N3 2.0243 2.1000 -0.0757 0.0100 BUMP H4A H6A 2.0683 2.1000 -0.0317 0.0100 BUMP H14 H6B 2.0565 2.1000 -0.0435 0.0100 BUMP H21 H9B 2.0336 2.1000 -0.0664 0.0100 BUMP H26 H12B 2.7998 2.6500 0.1498 0.0400 DANG Mn1 H1WA 2.2177 2.6500 -0.4323 0.0400 DANG Mn1 H1WB 1.3051 1.3500 -0.0449 0.0100 DANG H1WA H1WB 0.0631 0.0200 SAME/SADI C71_a N71_a C63_b N63_b -0.0312 0.0100 SIMU U11 Cl51_a C73_b -0.0308 0.0100 SIMU U22 Cl51_a C73_b Summary of restraints applied in cycle 19 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 20. 4. 6. 28. 0. 0. 0. 204. 564. 0. 0. rms sigma 0.010 0.010 0.033 0.030 0.000 0.000 0.000 0.010 0.015 0.000 0.000 rms deviation 0.030 0.019 0.189 0.040 0.000 0.000 0.000 0.005 0.014 0.000 0.000 GooF = S = 1.026; Restrained GooF = 1.022 for 826 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0912 * P )^2 + 4.29 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55753 0.00139 -0.001 OSF 2 0.80416 0.00254 0.000 FVAR 2 3 0.00418 0.00132 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for z C64_b Max. shift = 0.000 A for H64B_b Max. dU = 0.000 for C74_b Least-squares cycle 20 Maximum vector length = 511 Memory required = 8940 / 1023624 wR2 = 0.1886 before cycle 20 for 9802 data and 721 / 721 parameters Disagreeable restraints before cycle 20 Observed Target Error Sigma Restraint 2.9611 3.0000 -0.0389 0.0100 BUMP C24 N3 2.0244 2.1000 -0.0756 0.0100 BUMP H4A H6A 2.0683 2.1000 -0.0317 0.0100 BUMP H14 H6B 2.0565 2.1000 -0.0435 0.0100 BUMP H21 H9B 2.0336 2.1000 -0.0664 0.0100 BUMP H26 H12B 2.7998 2.6500 0.1498 0.0400 DANG Mn1 H1WA 2.2177 2.6500 -0.4323 0.0400 DANG Mn1 H1WB 1.3051 1.3500 -0.0449 0.0100 DANG H1WA H1WB 0.0631 0.0200 SAME/SADI C71_a N71_a C63_b N63_b -0.0312 0.0100 SIMU U11 Cl51_a C73_b -0.0308 0.0100 SIMU U22 Cl51_a C73_b Summary of restraints applied in cycle 20 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 20. 4. 6. 28. 0. 0. 0. 204. 564. 0. 0. rms sigma 0.010 0.010 0.033 0.030 0.000 0.000 0.000 0.010 0.015 0.000 0.000 rms deviation 0.030 0.019 0.189 0.040 0.000 0.000 0.000 0.005 0.014 0.000 0.000 GooF = S = 1.026; Restrained GooF = 1.022 for 826 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0912 * P )^2 + 4.29 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55753 0.00139 0.000 OSF 2 0.80416 0.00254 0.000 FVAR 2 3 0.00418 0.00132 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.005 for y H1WB Max. shift = 0.000 A for H64A_b Max. dU = 0.000 for C64_b Largest correlation matrix elements 0.899 tors H74A_b / x C74_b 0.638 U12 O51_a / U22 O51_a 0.613 U23 O51_a / U22 O51_a 0.848 y H1WA / x H1WA 0.637 U23 N71_a / U33 N71_a 0.605 U12 O51_a / U11 O51_a 0.793 z C74_b / z C64_b 0.631 y O59_b / x O59_b 0.605 y N63_b / x N63_b 0.741 z C73_b / x C73_b 0.630 tors H64A_b / y C64_b 0.604 z O58_b / y O58_b 0.727 y C63_b / x C63_b 0.621 U23 N61_a / U33 N61_a 0.602 U23 C62_a / U33 C62_a 0.690 z H2WA / x H2WA -0.621 z H2WB / x H2WB 0.601 U23 O2 / U22 O2 0.678 z H2WB / z H2WA 0.616 z H2WB / x H2WA 0.593 U23 O54_a / U22 O54_a 0.645 z C74_b / z C63_b 0.613 U23 O51_a / U33 O51_a 0.593 U23 N61_a / U22 N61_a Idealized hydrogen atom generation before cycle 21 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.7202 -0.3078 0.2492 43 0.950 0.000 C1 N1 C2 H2 0.8466 -0.4181 0.2408 43 0.950 0.000 C2 C3 C1 H3 0.9866 -0.3841 0.3649 43 0.950 0.000 C3 C2 C4 H4 0.9984 -0.2373 0.4941 43 0.950 0.000 C4 C3 C5 H7 1.0034 -0.1047 0.6052 43 0.950 0.000 C7 C8 C6 H8 1.0126 0.0517 0.7261 43 0.950 0.000 C8 C7 C9 H9 0.8847 0.1586 0.7139 43 0.950 0.000 C9 C8 C10 H14 0.3448 0.1254 0.2873 43 0.950 0.000 C14 C15 C13 H15 0.2378 0.2543 0.3002 43 0.950 0.000 C15 C16 C14 H16 0.2670 0.4008 0.4339 43 0.950 0.000 C16 C15 C17 H19 0.3040 0.5310 0.5652 43 0.950 0.000 C19 C20 C18 H20 0.3534 0.6614 0.7073 43 0.950 0.000 C20 C19 C21 H21 0.4939 0.6491 0.8103 43 0.950 0.000 C21 C20 C22 H26 0.7478 0.1348 0.8711 43 0.950 0.000 C26 C27 C25 H27 0.9466 0.1346 0.9316 43 0.950 0.000 C27 C28 C26 H28 1.1416 0.2993 0.9668 43 0.950 0.000 C28 C27 C29 H31 1.1009 0.5751 0.8808 43 0.950 0.000 C31 C32 C30 H32 1.2976 0.7377 0.9132 43 0.950 0.000 C32 C33 C31 H33 1.4864 0.7509 0.9959 43 0.950 0.000 C33 C34 C32 H34 1.4725 0.6049 1.0439 43 0.950 0.000 C34 N14 C33 H4A 0.6445 0.0222 0.4561 43 0.880 0.000 N4 C11 N5 H6A 0.5265 -0.0197 0.3435 93 0.880 0.000 N6 C12 N5 H6B 0.4339 0.0138 0.2962 93 0.880 0.000 N6 C12 N5 H9A 0.7069 0.5590 0.9034 93 0.880 0.000 N9 C23 N10 H9B 0.6327 0.6295 0.8847 93 0.880 0.000 N9 C23 N10 H11 0.8070 0.4558 0.8361 43 0.880 0.000 N11 C24 N10 H12A 0.5393 0.2146 0.7656 93 0.880 0.000 N12 C24 N11 H12B 0.6002 0.1472 0.8010 93 0.880 0.000 N12 C24 N11 H62A 0.6529 0.0164 1.1143 137 0.980 0.000 C62_a C61_a H62A_a H62B 0.6315 0.0489 1.2108 137 0.980 0.000 C62_a C61_a H62A_a H62C 0.5210 -0.0602 1.1343 137 0.980 0.000 C62_a C61_a H62A_a H64A 0.5788 -0.0686 1.0673 137 0.980 0.000 C64_b C63_b H64A_b H64B 0.6753 0.0504 1.1433 137 0.980 0.000 C64_b C63_b H64A_b H64C 0.5544 -0.0394 1.1629 137 0.980 0.000 C64_b C63_b H64A_b H72A 0.8983 0.1545 0.1049 137 0.980 0.000 C72_a C71_a H72A_a H72B 0.9387 0.1459 0.1940 137 0.980 0.000 C72_a C71_a H72A_a H72C 1.0362 0.1451 0.1284 137 0.980 0.000 C72_a C71_a H72A_a H74A 0.7279 0.0715 0.3566 137 0.980 0.000 C74_b C73_b H74A_b H74B 0.8529 0.1156 0.3164 137 0.980 0.000 C74_b C73_b H74A_b H74C 0.7125 0.1086 0.2773 137 0.980 0.000 C74_b C73_b H74A_b 04src1114 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.77760 -0.29331 0.29975 1.00000 0.03448 0.02518 0.03550 0.00429 0.01164 0.00678 0.03499 0.00912 0.00037 0.00032 0.00025 0.00000 0.00180 0.00176 0.00184 0.00144 0.00147 0.00144 0.00080 H1 0.72025 -0.30784 0.24924 1.00000 0.04199 0.00000 0.00000 C2 0.85215 -0.35947 0.29406 1.00000 0.04293 0.02434 0.04691 0.00172 0.01837 0.00901 0.04219 0.01002 0.00040 0.00033 0.00028 0.00000 0.00206 0.00184 0.00214 0.00160 0.00169 0.00158 0.00092 H2 0.84657 -0.41808 0.24080 1.00000 0.05063 0.00000 0.00000 C3 0.93475 -0.33908 0.36688 1.00000 0.03923 0.02584 0.05953 0.01284 0.02192 0.01557 0.04114 0.01033 0.00040 0.00033 0.00029 0.00000 0.00196 0.00182 0.00238 0.00170 0.00175 0.00158 0.00089 H3 0.98664 -0.38412 0.36488 1.00000 0.04937 0.00000 0.00000 C4 0.94171 -0.25250 0.44306 1.00000 0.03171 0.02332 0.04823 0.01326 0.01326 0.01398 0.03340 0.00906 0.00034 0.00029 0.00025 0.00000 0.00172 0.00170 0.00205 0.00150 0.00152 0.00141 0.00077 H4 0.99841 -0.23729 0.49408 1.00000 0.04009 0.00000 0.00000 C5 0.86458 -0.18753 0.44435 1.00000 0.02531 0.02031 0.03830 0.01188 0.01133 0.00786 0.02786 0.00849 0.00032 0.00029 0.00023 0.00000 0.00153 0.00155 0.00175 0.00134 0.00131 0.00125 0.00068 C6 0.87134 -0.09059 0.52397 1.00000 0.02334 0.01945 0.03211 0.01199 0.00782 0.00736 0.02455 0.00802 0.00031 0.00028 0.00021 0.00000 0.00146 0.00150 0.00161 0.00127 0.00123 0.00120 0.00064 C7 0.95197 -0.06092 0.60153 1.00000 0.02711 0.02628 0.03699 0.01499 0.00412 0.01225 0.02895 0.00830 0.00033 0.00029 0.00022 0.00000 0.00158 0.00168 0.00178 0.00141 0.00134 0.00135 0.00070 H7 1.00338 -0.10469 0.60525 1.00000 0.03474 0.00000 0.00000 C8 0.95780 0.03138 0.67291 1.00000 0.02958 0.02939 0.03039 0.01304 0.00048 0.01057 0.02993 0.00863 0.00034 0.00031 0.00023 0.00000 0.00164 0.00176 0.00168 0.00140 0.00133 0.00139 0.00072 H8 1.01257 0.05173 0.72615 1.00000 0.03592 0.00000 0.00000 C9 0.88272 0.09405 0.66596 1.00000 0.02892 0.02287 0.02699 0.00848 0.00407 0.00979 0.02678 0.00825 0.00032 0.00029 0.00022 0.00000 0.00159 0.00162 0.00159 0.00131 0.00127 0.00131 0.00067 H9 0.88465 0.15864 0.71392 1.00000 0.03213 0.00000 0.00000 C10 0.80439 0.05953 0.58661 1.00000 0.02148 0.02118 0.02756 0.01166 0.00458 0.00836 0.02278 0.00774 0.00029 0.00027 0.00021 0.00000 0.00140 0.00150 0.00154 0.00124 0.00117 0.00119 0.00062 C11 0.72466 0.12696 0.57587 1.00000 0.01972 0.02123 0.02553 0.01179 0.00520 0.00680 0.02168 0.00766 0.00029 0.00027 0.00020 0.00000 0.00138 0.00150 0.00149 0.00123 0.00113 0.00117 0.00061 C12 0.50417 0.11952 0.41503 1.00000 0.02857 0.02126 0.02220 0.00875 0.00602 0.00973 0.02386 0.00792 0.00032 0.00028 0.00020 0.00000 0.00155 0.00154 0.00146 0.00122 0.00120 0.00127 0.00063 C13 0.43379 0.19717 0.41405 1.00000 0.02590 0.02257 0.02530 0.01254 0.00383 0.00876 0.02393 0.00798 0.00031 0.00028 0.00021 0.00000 0.00149 0.00155 0.00150 0.00124 0.00119 0.00124 0.00063 C14 0.35527 0.18490 0.34121 1.00000 0.03091 0.02680 0.02550 0.01235 0.00232 0.00692 0.02851 0.00843 0.00033 0.00030 0.00022 0.00000 0.00165 0.00170 0.00159 0.00135 0.00128 0.00135 0.00070 H14 0.34483 0.12539 0.28726 1.00000 0.03421 0.00000 0.00000 C15 0.29262 0.26135 0.34906 1.00000 0.03024 0.03255 0.03066 0.01745 -0.00128 0.01018 0.03064 0.00876 0.00034 0.00032 0.00023 0.00000 0.00166 0.00183 0.00168 0.00144 0.00134 0.00142 0.00073 H15 0.23777 0.25431 0.30019 1.00000 0.03677 0.00000 0.00000 C16 0.30960 0.34776 0.42764 1.00000 0.02476 0.02762 0.03760 0.01866 0.00209 0.00972 0.02864 0.00849 0.00032 0.00030 0.00023 0.00000 0.00154 0.00171 0.00178 0.00143 0.00133 0.00133 0.00070 H16 0.26703 0.40081 0.43388 1.00000 0.03436 0.00000 0.00000 C17 0.39134 0.35525 0.49806 1.00000 0.02365 0.02178 0.03181 0.01575 0.00485 0.00828 0.02442 0.00810 0.00031 0.00028 0.00021 0.00000 0.00146 0.00153 0.00159 0.00128 0.00122 0.00122 0.00064 C18 0.41701 0.44377 0.58607 1.00000 0.02217 0.01964 0.03384 0.01353 0.00572 0.00729 0.02455 0.00807 0.00031 0.00028 0.00022 0.00000 0.00143 0.00149 0.00162 0.00127 0.00122 0.00120 0.00064 C19 0.36116 0.52727 0.60765 1.00000 0.02598 0.02196 0.04280 0.01512 0.00421 0.00956 0.02961 0.00871 0.00033 0.00030 0.00024 0.00000 0.00157 0.00161 0.00187 0.00142 0.00138 0.00130 0.00071 H19 0.30402 0.53098 0.56516 1.00000 0.03553 0.00000 0.00000 C20 0.39029 0.60381 0.69130 1.00000 0.03012 0.02406 0.04466 0.01271 0.00625 0.01411 0.03220 0.00894 0.00035 0.00031 0.00024 0.00000 0.00167 0.00170 0.00198 0.00148 0.00145 0.00139 0.00075 H20 0.35337 0.66137 0.70735 1.00000 0.03864 0.00000 0.00000 C21 0.47322 0.59703 0.75201 1.00000 0.03034 0.01865 0.03548 0.00828 0.00610 0.00910 0.02895 0.00845 0.00033 0.00029 0.00023 0.00000 0.00165 0.00157 0.00177 0.00135 0.00135 0.00131 0.00070 H21 0.49394 0.64913 0.81032 1.00000 0.03474 0.00000 0.00000 C22 0.52573 0.51237 0.72598 1.00000 0.02546 0.01668 0.03037 0.00913 0.00530 0.00663 0.02464 0.00795 0.00031 0.00027 0.00021 0.00000 0.00149 0.00145 0.00157 0.00123 0.00122 0.00119 0.00064 C23 0.61396 0.49373 0.78575 1.00000 0.02824 0.01796 0.02912 0.00791 0.00374 0.00700 0.02614 0.00804 0.00032 0.00028 0.00022 0.00000 0.00157 0.00151 0.00160 0.00125 0.00127 0.00125 0.00066 C24 0.71365 0.29406 0.81782 1.00000 0.03497 0.02118 0.01899 0.00729 0.00497 0.01158 0.02503 0.00796 0.00033 0.00028 0.00019 0.00000 0.00165 0.00155 0.00144 0.00121 0.00123 0.00132 0.00065 C25 0.83374 0.29460 0.86469 1.00000 0.03378 0.01958 0.02073 0.00711 0.00128 0.00825 0.02573 0.00792 0.00033 0.00028 0.00020 0.00000 0.00161 0.00151 0.00148 0.00121 0.00124 0.00127 0.00066 C26 0.82889 0.19907 0.88337 1.00000 0.04140 0.02376 0.03603 0.01377 -0.00936 0.00280 0.03684 0.00879 0.00038 0.00032 0.00024 0.00000 0.00192 0.00174 0.00189 0.00149 0.00153 0.00148 0.00084 H26 0.74781 0.13485 0.87106 1.00000 0.04421 0.00000 0.00000 C27 0.94580 0.20003 0.92054 1.00000 0.04970 0.03227 0.05369 0.02225 -0.00891 0.00818 0.04688 0.01022 0.00043 0.00037 0.00029 0.00000 0.00222 0.00204 0.00238 0.00184 0.00187 0.00171 0.00101 H27 0.94658 0.13457 0.93165 1.00000 0.05625 0.00000 0.00000 C28 1.06073 0.29697 0.94116 1.00000 0.04032 0.03546 0.04789 0.01792 -0.01008 0.00916 0.04334 0.00981 0.00041 0.00036 0.00027 0.00000 0.00197 0.00205 0.00223 0.00177 0.00170 0.00162 0.00094 H28 1.14159 0.29935 0.96679 1.00000 0.05201 0.00000 0.00000 C29 1.05623 0.39102 0.92382 1.00000 0.03518 0.02606 0.02493 0.00825 -0.00159 0.00818 0.03067 0.00833 0.00035 0.00031 0.00022 0.00000 0.00169 0.00168 0.00159 0.00134 0.00132 0.00138 0.00072 C30 1.17693 0.49698 0.94418 1.00000 0.03692 0.02492 0.02259 0.00493 0.00158 0.00970 0.03027 0.00836 0.00036 0.00030 0.00021 0.00000 0.00171 0.00165 0.00156 0.00130 0.00131 0.00138 0.00072 C31 1.17851 0.58237 0.91415 1.00000 0.03924 0.03043 0.03143 0.01211 0.00421 0.00855 0.03525 0.00924 0.00038 0.00033 0.00024 0.00000 0.00187 0.00186 0.00180 0.00150 0.00147 0.00151 0.00079 H31 1.10086 0.57508 0.88079 1.00000 0.04229 0.00000 0.00000 C32 1.29434 0.67819 0.93331 1.00000 0.04815 0.03231 0.03849 0.01453 0.00800 0.00402 0.04276 0.00992 0.00042 0.00036 0.00026 0.00000 0.00216 0.00199 0.00205 0.00166 0.00168 0.00168 0.00092 H32 1.29762 0.73766 0.91324 1.00000 0.05131 0.00000 0.00000 C33 1.40529 0.68618 0.98209 1.00000 0.03727 0.03691 0.03713 0.00771 0.00780 -0.00025 0.04316 0.00964 0.00040 0.00036 0.00026 0.00000 0.00193 0.00211 0.00202 0.00167 0.00158 0.00165 0.00094 H33 1.48644 0.75088 0.99592 1.00000 0.05179 0.00000 0.00000 C34 1.39586 0.59874 1.01017 1.00000 0.03155 0.04116 0.03132 0.00487 0.00298 0.00597 0.03981 0.00920 0.00037 0.00036 0.00024 0.00000 0.00178 0.00214 0.00185 0.00160 0.00145 0.00157 0.00087 H34 1.47246 0.60488 1.04390 1.00000 0.04778 0.00000 0.00000 N1 0.78188 -0.20956 0.37287 1.00000 0.02851 0.02190 0.03243 0.00588 0.00826 0.00796 0.02937 0.00705 0.00028 0.00025 0.00019 0.00000 0.00140 0.00141 0.00149 0.00116 0.00115 0.00115 0.00062 N2 0.79721 -0.03051 0.51681 1.00000 0.02180 0.01965 0.02736 0.00969 0.00553 0.00725 0.02298 0.00655 0.00025 0.00023 0.00017 0.00000 0.00123 0.00130 0.00134 0.00107 0.00103 0.00104 0.00054 N3 0.72907 0.21492 0.63460 1.00000 0.01534 0.00718 0.01386 0.00148 0.00036 0.00476 0.01291 0.00538 0.00022 0.00019 0.00014 0.00000 0.00107 0.00105 0.00108 0.00086 0.00085 0.00087 0.00045 N4 0.64862 0.08564 0.49799 1.00000 0.02703 0.02128 0.02227 0.00815 0.00508 0.01304 0.02258 0.00651 0.00025 0.00023 0.00016 0.00000 0.00131 0.00133 0.00126 0.00105 0.00102 0.00109 0.00054 H4A 0.64450 0.02216 0.45606 1.00000 0.02710 0.00000 0.00000 N5 0.57721 0.15006 0.48839 1.00000 0.02539 0.02105 0.02398 0.01080 0.00524 0.01187 0.02207 0.00657 0.00026 0.00023 0.00017 0.00000 0.00127 0.00131 0.00127 0.00105 0.00101 0.00106 0.00053 N6 0.48615 0.02734 0.34336 1.00000 0.04560 0.03081 0.02676 0.00325 -0.00464 0.01930 0.03606 0.00718 0.00032 0.00026 0.00018 0.00000 0.00180 0.00166 0.00150 0.00126 0.00129 0.00143 0.00072 H6A 0.52655 -0.01974 0.34346 1.00000 0.04327 0.00000 0.00000 H6B 0.43390 0.01384 0.29618 1.00000 0.04327 0.00000 0.00000 N7 0.45117 0.28134 0.49075 1.00000 0.02403 0.02097 0.02615 0.01123 0.00483 0.00906 0.02305 0.00656 0.00026 0.00023 0.00017 0.00000 0.00127 0.00132 0.00131 0.00107 0.00103 0.00106 0.00054 N8 0.49841 0.43737 0.64448 1.00000 0.02682 0.01802 0.02898 0.01038 0.00436 0.00864 0.02434 0.00667 0.00026 0.00023 0.00018 0.00000 0.00132 0.00129 0.00136 0.00108 0.00106 0.00107 0.00055 N9 0.65596 0.56930 0.86716 1.00000 0.04067 0.02341 0.02719 0.00361 -0.00070 0.01537 0.03179 0.00701 0.00030 0.00025 0.00018 0.00000 0.00165 0.00150 0.00145 0.00118 0.00122 0.00130 0.00066 H9A 0.70693 0.55901 0.90339 1.00000 0.03815 0.00000 0.00000 H9B 0.63271 0.62949 0.88467 1.00000 0.03815 0.00000 0.00000 N10 0.64097 0.40177 0.75189 1.00000 0.03095 0.02032 0.02431 0.00731 -0.00059 0.01117 0.02558 0.00665 0.00027 0.00024 0.00017 0.00000 0.00139 0.00133 0.00131 0.00107 0.00107 0.00112 0.00057 N11 0.73426 0.39425 0.80759 1.00000 0.03156 0.01785 0.02405 0.00538 -0.00263 0.00838 0.02607 0.00669 0.00028 0.00024 0.00017 0.00000 0.00141 0.00131 0.00133 0.00108 0.00109 0.00111 0.00058 H11 0.80701 0.45579 0.83611 1.00000 0.03129 0.00000 0.00000 N12 0.60786 0.21086 0.79242 1.00000 0.01944 0.01201 0.01616 0.00611 -0.00137 0.00312 0.01681 0.00560 0.00023 0.00020 0.00015 0.00000 0.00116 0.00116 0.00115 0.00094 0.00091 0.00095 0.00049 H12A 0.53930 0.21456 0.76555 1.00000 0.02017 0.00000 0.00000 H12B 0.60023 0.14725 0.80100 1.00000 0.02017 0.00000 0.00000 N13 0.94548 0.38854 0.88398 1.00000 0.03039 0.02262 0.02128 0.00795 0.00184 0.00823 0.02570 0.00666 0.00027 0.00024 0.00017 0.00000 0.00137 0.00138 0.00130 0.00109 0.00106 0.00111 0.00057 N14 1.28413 0.50469 0.99259 1.00000 0.03441 0.03389 0.02886 0.00751 0.00128 0.01072 0.03473 0.00749 0.00030 0.00028 0.00019 0.00000 0.00153 0.00166 0.00151 0.00128 0.00121 0.00129 0.00068 O1 0.43541 0.16176 0.64339 1.00000 0.02764 0.02300 0.02424 0.00845 0.00523 0.00813 0.02566 0.00555 0.00022 0.00020 0.00015 0.00000 0.00114 0.00118 0.00114 0.00095 0.00090 0.00095 0.00048 O2 0.76059 0.42503 0.58802 1.00000 0.03143 0.03490 0.05786 0.02792 0.00772 0.01257 0.03873 0.00724 0.00025 0.00025 0.00020 0.00000 0.00130 0.00151 0.00176 0.00137 0.00120 0.00114 0.00062 Mn1 0.58760 0.29788 0.60830 1.00000 0.02497 0.01778 0.02264 0.00826 0.00241 0.00941 0.02150 0.00116 0.00005 0.00004 0.00003 0.00000 0.00026 0.00026 0.00026 0.00019 0.00018 0.00020 0.00016 H1WA 0.38178 0.18311 0.67347 1.00000 0.03225 0.05703 0.00160 0.00272 0.00069 0.00000 0.00000 H1WB 0.39824 0.15581 0.59461 1.00000 0.03225 0.03238 0.00206 0.00094 0.00060 0.00000 0.00000 H2WA 0.78489 0.39687 0.54346 1.00000 0.03225 0.06169 0.00273 0.00272 0.00117 0.00000 0.00000 H2WB 0.82544 0.46621 0.62813 1.00000 0.03225 0.03638 0.00199 0.00274 0.00121 0.00000 0.00000 O41 0.72052 0.01534 0.97935 1.00000 0.10955 0.03184 0.03890 0.00890 0.01541 0.01775 0.06421 0.00849 0.00041 0.00027 0.00020 0.00000 0.00288 0.00164 0.00168 0.00134 0.00173 0.00175 0.00098 O42 0.69072 -0.17972 0.93949 1.00000 0.09741 0.03213 0.06646 0.02356 0.02310 0.01911 0.06544 0.00907 0.00040 0.00028 0.00023 0.00000 0.00271 0.00169 0.00222 0.00159 0.00196 0.00175 0.00097 O43 0.55756 -0.12929 0.85970 1.00000 0.06276 0.05723 0.09607 0.00816 0.00001 0.02459 0.07875 0.00955 0.00038 0.00034 0.00029 0.00000 0.00220 0.00233 0.00298 0.00209 0.00200 0.00187 0.00117 O44 0.77981 -0.07989 0.85483 1.00000 0.06594 0.06047 0.03838 0.01900 0.01511 0.00827 0.05935 0.00816 0.00034 0.00031 0.00020 0.00000 0.00205 0.00215 0.00165 0.00153 0.00147 0.00170 0.00089 Cl41 0.68809 -0.09223 0.90938 1.00000 0.06549 0.02339 0.03841 0.00818 0.01395 0.00554 0.04666 0.00250 0.00011 0.00008 0.00006 0.00000 0.00067 0.00047 0.00053 0.00039 0.00046 0.00044 0.00028 O51_a 1.00448 0.28772 0.37367 0.80416 0.04290 0.07045 0.06044 0.04237 0.02247 0.03788 0.04794 0.01038 0.00035 0.00036 0.00025 0.00254 0.00191 0.00261 0.00232 0.00209 0.00170 0.00189 0.00094 O52_a 0.79972 0.24824 0.29857 0.80416 0.05116 0.06119 0.06987 -0.00808 -0.01456 0.02709 0.07034 0.01002 0.00042 0.00041 0.00030 0.00254 0.00234 0.00275 0.00273 0.00223 0.00202 0.00210 0.00137 O53_a 0.92421 0.43494 0.39631 0.80416 0.06302 0.03521 0.07639 0.01703 0.01083 0.01784 0.06008 0.01034 0.00042 0.00034 0.00030 0.00254 0.00257 0.00208 0.00292 0.00199 0.00216 0.00187 0.00111 O54_a 0.83351 0.29289 0.44757 0.80416 0.06218 0.08696 0.07651 0.04585 0.04189 0.03625 0.06761 0.01495 0.00052 0.00054 0.00035 0.00254 0.00275 0.00378 0.00307 0.00300 0.00234 0.00278 0.00134 Cl51_a 0.89018 0.31409 0.37766 0.80416 0.02839 0.03443 0.04472 0.01709 0.00821 0.01686 0.03401 0.00282 0.00010 0.00010 0.00007 0.00254 0.00055 0.00062 0.00065 0.00050 0.00044 0.00046 0.00032 O56_b 0.85127 0.30774 0.23916 0.19584 0.03266 0.06038 0.09458 0.03705 -0.00773 0.00699 0.06483 0.03924 0.00115 0.00153 0.00127 0.00254 0.00534 0.00849 0.00966 0.00760 0.00612 0.00556 0.00405 O57_b 1.03352 0.38134 0.34878 0.19584 0.05009 0.09181 0.05259 0.02712 -0.00024 -0.00282 0.07428 0.03884 0.00166 0.00181 0.00085 0.00254 0.00773 0.01018 0.00609 0.00649 0.00602 0.00789 0.00471 O58_b 1.05154 0.44536 0.24096 0.19584 0.06044 0.05462 0.06658 0.02748 0.01250 -0.00157 0.06622 0.04908 0.00205 0.00153 0.00139 0.00254 0.00841 0.00728 0.00822 0.00696 0.00746 0.00677 0.00457 O59_b 1.03232 0.26005 0.20791 0.19584 0.06384 0.06313 0.08909 0.00006 0.00496 0.02840 0.08001 0.05282 0.00220 0.00178 0.00147 0.00254 0.00730 0.00740 0.00831 0.00726 0.00752 0.00679 0.00490 Cl56_b 0.99059 0.34561 0.25895 0.19584 0.03731 0.03913 0.04504 0.02012 0.00292 0.01287 0.04028 0.01213 0.00047 0.00044 0.00032 0.00254 0.00236 0.00256 0.00261 0.00205 0.00191 0.00193 0.00130 C61_a 0.68125 -0.09324 1.16757 0.80416 0.05271 0.09435 0.05287 0.03817 0.01486 0.02425 0.06489 0.02033 0.00071 0.00075 0.00048 0.00254 0.00371 0.00450 0.00362 0.00333 0.00271 0.00314 0.00179 C62_a 0.61602 -0.01530 1.15572 0.80416 0.05109 0.07251 0.04032 0.03344 0.01484 0.01449 0.05372 0.01695 0.00067 0.00061 0.00041 0.00254 0.00313 0.00409 0.00313 0.00297 0.00255 0.00285 0.00150 H62A_a 0.65291 0.01638 1.11434 0.80416 0.08058 0.00254 0.00000 H62B_a 0.63150 0.04893 1.21076 0.80416 0.08058 0.00254 0.00000 H62C_a 0.52097 -0.06021 1.13430 0.80416 0.08058 0.00254 0.00000 N61_a 0.73127 -0.15462 1.17357 0.80416 0.08264 0.12860 0.10854 0.07723 0.00845 0.05305 0.09485 0.02040 0.00075 0.00074 0.00052 0.00254 0.00440 0.00562 0.00513 0.00450 0.00375 0.00407 0.00214 C63_b 0.70995 -0.09335 1.14503 0.19584 0.06570 0.10412 0.07214 0.03070 0.00968 0.02477 0.08423 0.07173 0.00353 0.00256 0.00164 0.00254 0.00720 0.00748 0.00797 0.00718 0.00709 0.00638 0.00515 C64_b 0.62171 -0.03228 1.12811 0.19584 0.06291 0.07618 0.07347 0.01188 0.01279 0.01976 0.07790 0.03912 0.00206 0.00123 0.00092 0.00254 0.00984 0.01047 0.01189 0.01017 0.01010 0.00781 0.00677 H64A_b 0.57882 -0.06864 1.06728 0.19584 0.11686 0.00254 0.00000 H64B_b 0.67534 0.05040 1.14326 0.19584 0.11686 0.00254 0.00000 H64C_b 0.55437 -0.03942 1.16292 0.19584 0.11686 0.00254 0.00000 N63_b 0.79698 -0.12390 1.12905 0.19584 0.06706 0.12301 0.10305 0.03655 -0.01125 0.03826 0.10100 0.07818 0.00274 0.00308 0.00214 0.00254 0.00944 0.01097 0.01098 0.00989 0.00921 0.00822 0.00607 C71_a 1.03594 0.30521 0.19260 0.80416 0.04318 0.04765 0.04402 0.02553 0.00846 0.01528 0.04343 0.01549 0.00061 0.00056 0.00038 0.00254 0.00265 0.00303 0.00276 0.00238 0.00213 0.00249 0.00125 C72_a 0.97190 0.17693 0.15153 0.80416 0.05361 0.04920 0.05775 0.00255 -0.00160 0.01361 0.06126 0.01422 0.00062 0.00053 0.00043 0.00254 0.00337 0.00327 0.00362 0.00287 0.00279 0.00275 0.00162 H72A_a 0.89834 0.15455 0.10490 0.80416 0.09188 0.00254 0.00000 H72B_a 0.93866 0.14593 0.19402 0.80416 0.09188 0.00254 0.00000 H72C_a 1.03615 0.14506 0.12838 0.80416 0.09188 0.00254 0.00000 N71_a 1.08414 0.40183 0.22449 0.80416 0.05251 0.04268 0.06393 0.03201 0.01330 0.01113 0.05181 0.01476 0.00055 0.00049 0.00040 0.00254 0.00296 0.00281 0.00334 0.00264 0.00233 0.00230 0.00132 C73_b 0.80438 0.24963 0.39168 0.19584 0.05958 0.06525 0.07242 0.01908 0.00848 0.00737 0.07300 0.05249 0.00169 0.00158 0.00201 0.00254 0.00679 0.00657 0.00712 0.00650 0.00679 0.00645 0.00488 C74_b 0.77150 0.12535 0.33009 0.19584 0.04221 0.07036 0.08548 0.03471 0.04168 0.01833 0.06420 0.04263 0.00193 0.00151 0.00091 0.00254 0.01040 0.00966 0.01373 0.00921 0.01007 0.00969 0.00599 H74A_b 0.72788 0.07146 0.35663 0.19584 0.09631 0.00254 0.00000 H74B_b 0.85286 0.11560 0.31644 0.19584 0.09631 0.00254 0.00000 H74C_b 0.71250 0.10858 0.27735 0.19584 0.09631 0.00254 0.00000 N73_b 0.82664 0.34452 0.44001 0.19584 0.05977 0.07119 0.06421 0.03676 0.03222 0.04628 0.05510 0.05543 0.00243 0.00180 0.00145 0.00254 0.00830 0.00817 0.00878 0.00690 0.00714 0.00769 0.00434 Final Structure Factor Calculation for 04src1114 in P-1 Total number of l.s. parameters = 721 Maximum vector length = 511 Memory required = 8219 / 25039 wR2 = 0.1886 before cycle 21 for 9802 data and 0 / 721 parameters Disagreeable restraints before cycle 21 Observed Target Error Sigma Restraint 2.9611 3.0000 -0.0389 0.0100 BUMP C24 N3 2.0243 2.1000 -0.0757 0.0100 BUMP H4A H6A 2.0683 2.1000 -0.0317 0.0100 BUMP H14 H6B 2.0565 2.1000 -0.0435 0.0100 BUMP H21 H9B 2.0336 2.1000 -0.0664 0.0100 BUMP H26 H12B 2.7998 2.6500 0.1498 0.0400 DANG Mn1 H1WA 2.2178 2.6500 -0.4322 0.0400 DANG Mn1 H1WB 1.3051 1.3500 -0.0449 0.0100 DANG H1WA H1WB 0.0631 0.0200 SAME/SADI C71_a N71_a C63_b N63_b -0.0312 0.0100 SIMU U11 Cl51_a C73_b -0.0308 0.0100 SIMU U22 Cl51_a C73_b Summary of restraints applied in cycle 21 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 19. 4. 6. 28. 0. 0. 0. 204. 564. 0. 0. rms sigma 0.010 0.010 0.033 0.030 0.000 0.000 0.000 0.010 0.015 0.000 0.000 rms deviation 0.031 0.019 0.189 0.040 0.000 0.000 0.000 0.005 0.014 0.000 0.000 GooF = S = 1.026; Restrained GooF = 1.022 for 825 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0912 * P )^2 + 4.29 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0661 for 7386 Fo > 4sig(Fo) and 0.0906 for all 9802 data wR2 = 0.1886, GooF = S = 1.026, Restrained GooF = 1.022 for all data Occupancy sum of asymmetric unit = 67.00 for non-hydrogen and 38.00 for hydrogen atoms Principal mean square atomic displacements U 0.0520 0.0297 0.0233 C1 0.0706 0.0347 0.0213 C2 0.0687 0.0322 0.0225 C3 0.0507 0.0296 0.0200 C4 0.0406 0.0241 0.0189 C5 0.0324 0.0238 0.0174 C6 0.0384 0.0281 0.0204 C7 0.0377 0.0290 0.0230 C8 0.0305 0.0272 0.0227 C9 0.0281 0.0215 0.0188 C10 0.0264 0.0210 0.0176 C11 0.0289 0.0219 0.0208 C12 0.0290 0.0248 0.0180 C13 0.0376 0.0255 0.0224 C14 0.0433 0.0303 0.0184 C15 0.0421 0.0252 0.0186 C16 0.0337 0.0237 0.0158 C17 0.0341 0.0228 0.0168 C18 0.0442 0.0259 0.0187 C19 0.0464 0.0308 0.0194 C20 0.0376 0.0310 0.0183 C21 0.0310 0.0268 0.0161 C22 0.0316 0.0290 0.0179 C23 0.0354 0.0208 0.0188 C24 0.0371 0.0207 0.0194 C25 0.0644 0.0243 0.0218 C26 0.0794 0.0355 0.0257 C27 0.0698 0.0341 0.0261 C28 0.0423 0.0277 0.0220 C29 0.0398 0.0306 0.0204 C30 0.0449 0.0313 0.0296 C31 0.0616 0.0385 0.0281 C32 0.0658 0.0371 0.0266 C33 0.0575 0.0359 0.0260 C34 0.0395 0.0272 0.0213 N1 0.0275 0.0225 0.0189 N2 0.0187 0.0135 0.0065 N3 0.0283 0.0224 0.0171 N4 0.0260 0.0241 0.0161 N5 0.0581 0.0276 0.0225 N6 0.0266 0.0240 0.0185 N7 0.0301 0.0265 0.0164 N8 0.0478 0.0278 0.0197 N9 0.0367 0.0216 0.0185 N10 0.0393 0.0214 0.0175 N11 0.0256 0.0134 0.0114 N12 0.0333 0.0232 0.0207 N13 0.0399 0.0382 0.0261 N14 0.0294 0.0248 0.0228 O1 0.0605 0.0314 0.0243 O2 0.0273 0.0215 0.0157 Mn1 0.1188 0.0440 0.0299 O41 0.1049 0.0636 0.0278 O42 0.1228 0.0601 0.0534 O43 0.0920 0.0515 0.0346 O44 0.0785 0.0383 0.0231 Cl41 0.0799 0.0393 0.0246 O51_a 0.1272 0.0475 0.0363 O52_a 0.0813 0.0647 0.0342 O53_a 0.0964 0.0729 0.0335 O54_a 0.0448 0.0347 0.0225 Cl51_a 0.1090 0.0558 0.0296 O56_b 0.1271 0.0548 0.0409 O57_b 0.0966 0.0663 0.0357 O58_b 0.1279 0.0618 0.0503 O59_b 0.0513 0.0368 0.0328 Cl56_b 0.0986 0.0530 0.0431 C61_a 0.0823 0.0523 0.0266 C62_a 0.1451 0.0994 0.0401 N61_a 0.1134 0.0754 0.0639 C63_b 0.1068 0.0664 0.0605 C64_b 0.1336 0.1209 0.0485 N63_b 0.0542 0.0430 0.0330 C71_a 0.0843 0.0617 0.0378 C72_a 0.0679 0.0580 0.0295 N71_a 0.0933 0.0757 0.0500 C73_b 0.0991 0.0734 0.0201 C74_b 0.0858 0.0501 0.0293 N73_b Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.021 0.033 0.044 0.058 0.074 0.094 0.124 0.176 1.000 Number in group 980. 992. 1037. 912. 989. 998. 971. 963. 976. 984. GooF 1.024 1.002 1.075 1.008 1.037 1.067 1.001 0.992 1.001 1.045 K 4.294 1.450 1.132 1.026 1.011 1.003 0.997 1.011 1.018 1.015 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.31 1.65 inf Number in group 989. 985. 975. 998. 967. 983. 961. 976. 986. 982. GooF 0.959 0.833 0.907 0.887 0.844 0.856 0.870 0.887 1.111 1.753 K 0.966 1.026 1.032 1.038 1.036 1.017 1.019 1.025 1.017 1.010 R1 0.216 0.173 0.150 0.118 0.095 0.068 0.060 0.055 0.059 0.069 Recommended weighting scheme: WGHT 0.0902 4.4288 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 3 0 689.70 258.97 7.58 0.086 3.85 4 -4 5 92.92 1.23 7.28 0.006 2.04 -6 -6 6 840.45 184.29 6.70 0.072 1.15 2 -2 7 164.12 36.64 6.18 0.032 2.13 3 -6 6 499.93 184.86 6.16 0.072 1.89 4 -2 3 87.85 11.29 5.78 0.018 2.39 4 -2 4 324.45 127.41 5.76 0.060 2.20 -6 -3 12 157.97 22.46 5.73 0.025 1.13 2 -5 8 181.12 60.08 5.10 0.041 1.85 -3 0 5 640.65 347.01 4.88 0.099 2.58 -6 -6 8 6307.48 11078.96 4.88 0.561 1.12 -2 0 2 146.96 48.18 4.87 0.037 4.73 -3 -6 6 58.96 4.50 4.78 0.011 1.53 5 -3 3 1818.55 1126.28 4.74 0.179 2.00 4 0 1 53.39 5.96 4.60 0.013 2.42 -2 3 1 1246.17 2095.41 4.56 0.244 3.55 -7 0 1 66.98 11.51 4.49 0.018 1.47 0 -5 3 128.50 36.38 4.49 0.032 2.49 -7 -7 7 1298.50 695.69 4.44 0.141 0.98 -1 0 9 418.27 218.74 4.39 0.079 1.77 -6 -9 12 121.17 22.30 4.33 0.025 0.89 5 -5 4 1572.03 1006.04 4.32 0.169 1.83 0 0 3 1847.25 1181.74 4.29 0.183 5.20 -3 4 7 159.34 63.10 4.24 0.042 1.59 2 -3 4 34.11 1.30 4.16 0.006 3.13 5 -5 1 76.53 19.46 4.13 0.024 1.95 1 -4 2 73.21 15.52 4.12 0.021 3.30 -2 1 7 228.48 107.84 4.11 0.055 2.09 -6 9 6 60.54 2.05 4.08 0.008 1.06 -4 0 2 107.31 36.90 4.08 0.032 2.57 2 -6 1 202.55 90.12 4.05 0.051 2.15 0 5 4 22.08 98.64 4.03 0.053 1.71 2 -3 1 80.75 22.68 3.93 0.025 3.96 1 -3 5 944.95 603.30 3.93 0.131 3.03 1 -4 1 1153.21 1807.63 3.91 0.227 3.26 3 2 17 15.07 135.45 3.91 0.062 0.78 -3 -3 6 291.19 130.38 3.86 0.061 2.05 0 0 13 114.39 33.56 3.72 0.031 1.20 0 -3 1 11.41 71.53 3.72 0.045 4.10 0 6 0 92.31 28.32 3.70 0.028 1.91 2 -6 7 640.22 403.73 3.68 0.107 1.86 0 -7 2 202.42 92.63 3.68 0.051 1.75 2 -1 2 35.48 4.94 3.67 0.012 4.41 4 -5 3 28.04 0.02 3.67 0.001 2.15 2 2 5 142.39 62.38 3.66 0.042 1.93 -4 1 7 406.18 242.09 3.63 0.083 1.84 1 1 4 95.88 209.51 3.62 0.077 2.91 3 -4 7 1087.96 729.30 3.62 0.144 1.95 2 -1 7 16.51 75.97 3.62 0.046 2.04 -4 4 15 43.51 137.06 3.60 0.062 0.91 Bond lengths and angles C1 - Distance Angles N1 1.3363 (0.0046) C2 1.3749 (0.0056) 123.21 (0.38) H1 0.9500 118.40 118.40 C1 - N1 C2 C2 - Distance Angles C3 1.3717 (0.0063) C1 1.3749 (0.0056) 118.61 (0.36) H2 0.9500 120.70 120.70 C2 - C3 C1 C3 - Distance Angles C2 1.3717 (0.0063) C4 1.3795 (0.0053) 119.32 (0.37) H3 0.9500 120.34 120.34 C3 - C2 C4 C4 - Distance Angles C3 1.3795 (0.0053) C5 1.3950 (0.0047) 119.26 (0.37) H4 0.9500 120.37 120.37 C4 - C3 C5 C5 - Distance Angles N1 1.3472 (0.0047) C4 1.3950 (0.0047) 121.05 (0.33) C6 1.4873 (0.0047) 117.35 (0.29) 121.60 (0.32) C5 - N1 C4 C6 - Distance Angles N2 1.3438 (0.0041) C7 1.3882 (0.0047) 121.17 (0.30) C5 1.4873 (0.0047) 116.46 (0.29) 122.35 (0.30) C6 - N2 C7 C7 - Distance Angles C8 1.3736 (0.0049) C6 1.3882 (0.0047) 120.34 (0.31) H7 0.9500 119.83 119.83 C7 - C8 C6 C8 - Distance Angles C7 1.3736 (0.0049) C9 1.3797 (0.0047) 118.85 (0.31) H8 0.9500 120.57 120.57 C8 - C7 C9 C9 - Distance Angles C8 1.3797 (0.0047) C10 1.3861 (0.0046) 117.72 (0.31) H9 0.9500 121.14 121.14 C9 - C8 C10 C10 - Distance Angles N2 1.3364 (0.0042) C9 1.3861 (0.0046) 124.02 (0.29) C11 1.4905 (0.0043) 116.61 (0.27) 119.36 (0.29) C10 - N2 C9 C11 - Distance Angles N3 1.2292 (0.0039) N4 1.3389 (0.0040) 122.36 (0.28) C10 1.4905 (0.0043) 122.11 (0.28) 115.53 (0.28) C11 - N3 N4 C12 - Distance Angles N5 1.2885 (0.0041) N6 1.3393 (0.0042) 126.90 (0.30) C13 1.4856 (0.0044) 113.81 (0.28) 119.29 (0.28) C12 - N5 N6 C13 - Distance Angles N7 1.3420 (0.0042) C14 1.3875 (0.0045) 121.87 (0.30) C12 1.4856 (0.0044) 114.19 (0.27) 123.94 (0.30) C13 - N7 C14 C14 - Distance Angles C15 1.3823 (0.0049) C13 1.3875 (0.0045) 118.39 (0.32) H14 0.9500 120.80 120.80 C14 - C15 C13 C15 - Distance Angles C16 1.3778 (0.0052) C14 1.3823 (0.0049) 120.09 (0.31) H15 0.9500 119.95 119.95 C15 - C16 C14 C16 - Distance Angles C15 1.3778 (0.0052) C17 1.4006 (0.0045) 118.18 (0.31) H16 0.9500 120.91 120.91 C16 - C15 C17 C17 - Distance Angles N7 1.3307 (0.0040) C16 1.4006 (0.0045) 121.83 (0.32) C18 1.4845 (0.0048) 114.73 (0.27) 123.43 (0.30) C17 - N7 C16 C18 - Distance Angles N8 1.3350 (0.0042) C19 1.3954 (0.0046) 121.76 (0.32) C17 1.4845 (0.0048) 114.56 (0.28) 123.68 (0.30) C18 - N8 C19 C19 - Distance Angles C20 1.3704 (0.0052) C18 1.3954 (0.0046) 118.75 (0.32) H19 0.9500 120.63 120.63 C19 - C20 C18 C20 - Distance Angles C19 1.3704 (0.0052) C21 1.3768 (0.0049) 119.80 (0.32) H20 0.9500 120.10 120.10 C20 - C19 C21 C21 - Distance Angles C20 1.3768 (0.0049) C22 1.3855 (0.0045) 118.37 (0.33) H21 0.9500 120.82 120.82 C21 - C20 C22 C22 - Distance Angles N8 1.3380 (0.0043) C21 1.3855 (0.0045) 122.41 (0.30) C23 1.4949 (0.0046) 113.89 (0.28) 123.67 (0.31) C22 - N8 C21 C23 - Distance Angles N10 1.2994 (0.0042) N9 1.3330 (0.0043) 126.10 (0.31) C22 1.4949 (0.0046) 115.07 (0.29) 118.83 (0.29) C23 - N10 N9 C24 - Distance Angles N12 1.2219 (0.0041) N11 1.3410 (0.0042) 124.06 (0.31) C25 1.4933 (0.0046) 122.99 (0.30) 112.94 (0.29) C24 - N12 N11 C25 - Distance Angles N13 1.3407 (0.0043) C26 1.3899 (0.0047) 122.53 (0.31) C24 1.4933 (0.0046) 116.79 (0.28) 120.63 (0.31) C25 - N13 C26 C26 - Distance Angles C27 1.3892 (0.0054) C25 1.3899 (0.0047) 118.22 (0.35) H26 0.9500 120.89 120.89 C26 - C27 C25 C27 - Distance Angles C28 1.3794 (0.0058) C26 1.3892 (0.0054) 119.35 (0.37) H27 0.9500 120.32 120.32 C27 - C28 C26 C28 - Distance Angles C27 1.3794 (0.0058) C29 1.3887 (0.0052) 118.86 (0.36) H28 0.9500 120.57 120.57 C28 - C27 C29 C29 - Distance Angles N13 1.3387 (0.0044) C28 1.3887 (0.0052) 122.20 (0.34) C30 1.4818 (0.0050) 116.64 (0.31) 121.06 (0.33) C29 - N13 C28 C30 - Distance Angles N14 1.3450 (0.0046) C31 1.3854 (0.0051) 122.31 (0.34) C29 1.4818 (0.0050) 116.26 (0.32) 121.43 (0.33) C30 - N14 C31 C31 - Distance Angles C32 1.3808 (0.0055) C30 1.3854 (0.0051) 119.18 (0.37) H31 0.9500 120.41 120.41 C31 - C32 C30 C32 - Distance Angles C33 1.3805 (0.0061) C31 1.3808 (0.0054) 118.92 (0.39) H32 0.9500 120.54 120.54 C32 - C33 C31 C33 - Distance Angles C34 1.3711 (0.0061) C32 1.3805 (0.0061) 118.58 (0.37) H33 0.9500 120.71 120.71 C33 - C34 C32 C34 - Distance Angles N14 1.3456 (0.0050) C33 1.3711 (0.0061) 123.64 (0.38) H34 0.9500 118.18 118.18 C34 - N14 C33 N1 - Distance Angles C1 1.3363 (0.0045) C5 1.3472 (0.0047) 118.54 (0.31) N1 - C1 N2 - Distance Angles C10 1.3364 (0.0042) C6 1.3438 (0.0041) 117.89 (0.28) N2 - C10 N3 - Distance Angles C11 1.2292 (0.0039) Mn1 2.2875 (0.0022) 116.70 (0.20) N3 - C11 N4 - Distance Angles C11 1.3389 (0.0040) N5 1.3798 (0.0035) 114.97 (0.25) H4A 0.8800 122.51 122.51 N4 - C11 N5 N5 - Distance Angles C12 1.2885 (0.0041) N4 1.3798 (0.0035) 119.72 (0.26) Mn1 2.2520 (0.0027) 124.22 (0.21) 115.93 (0.18) N5 - C12 N4 N6 - Distance Angles C12 1.3393 (0.0042) H6A 0.8800 120.00 H6B 0.8800 120.00 120.00 N6 - C12 H6A N7 - Distance Angles C17 1.3307 (0.0041) C13 1.3420 (0.0042) 119.63 (0.27) Mn1 2.3149 (0.0027) 120.84 (0.22) 119.53 (0.20) N7 - C17 C13 N8 - Distance Angles C18 1.3350 (0.0042) C22 1.3380 (0.0043) 118.90 (0.28) Mn1 2.2985 (0.0027) 121.37 (0.22) 119.71 (0.21) N8 - C18 C22 N9 - Distance Angles C23 1.3330 (0.0044) H9A 0.8800 120.00 H9B 0.8800 120.00 120.00 N9 - C23 H9A N10 - Distance Angles C23 1.2994 (0.0043) N11 1.4006 (0.0037) 113.04 (0.27) Mn1 2.2673 (0.0028) 121.40 (0.22) 123.30 (0.20) N10 - C23 N11 N11 - Distance Angles C24 1.3410 (0.0042) N10 1.4006 (0.0037) 120.54 (0.27) H11 0.8800 119.73 119.73 N11 - C24 N10 N12 - Distance Angles C24 1.2219 (0.0041) H12A 0.8800 120.00 H12B 0.8800 120.00 120.00 N12 - C24 H12A N13 - Distance Angles C29 1.3387 (0.0044) C25 1.3407 (0.0044) 118.68 (0.29) N13 - C29 N14 - Distance Angles C30 1.3450 (0.0046) C34 1.3456 (0.0050) 117.37 (0.34) N14 - C30 O1 - Distance Angles Mn1 2.2887 (0.0023) H1WA 0.8635 (0.0094) 117.99 (2.22) H1WB 0.8643 (0.0096) 74.36 (1.26) 98.11 (1.22) O1 - Mn1 H1WA O2 - Distance Angles Mn1 2.2132 (0.0026) H2WA 0.8279 (0.0097) 113.47 (2.18) H2WB 0.8286 (0.0098) 118.84 (2.19) 109.90 (1.66) O2 - Mn1 H2WA Mn1 - Distance Angles O2 2.2132 (0.0027) N5 2.2520 (0.0027) 93.13 (0.11) N10 2.2673 (0.0028) 92.03 (0.11) 153.87 (0.10) N3 2.2875 (0.0022) 85.65 (0.09) 69.52 (0.09) 85.38 (0.09) O1 2.2887 (0.0024) 169.96 (0.09) 87.42 (0.09) 83.23 (0.10) 85.15 (0.08) N8 2.2985 (0.0027) 88.34 (0.10) 136.59 (0.10) 69.15 (0.10) 153.59 (0.09) 98.16 (0.09) N7 2.3149 (0.0027) 92.22 (0.10) 68.09 (0.09) 137.25 (0.10) 137.36 (0.09) 97.27 (0.09) 68.49 (0.10) Mn1 - O2 N5 N10 N3 O1 N8 O41 - Distance Angles Cl41 1.4155 (0.0032) O41 - O42 - Distance Angles Cl41 1.4243 (0.0034) O42 - O43 - Distance Angles Cl41 1.4469 (0.0040) O43 - O44 - Distance Angles Cl41 1.4237 (0.0033) O44 - Cl41 - Distance Angles O41 1.4155 (0.0032) O44 1.4237 (0.0034) 109.98 (0.22) O42 1.4243 (0.0034) 110.20 (0.21) 109.26 (0.23) O43 1.4469 (0.0040) 110.37 (0.25) 108.29 (0.24) 108.71 (0.25) Cl41 - O41 O44 O42 O51_a - Distance Angles Cl51_a 1.4163 (0.0033) O51_a - O52_a - Distance Angles Cl51_a 1.4083 (0.0042) O52_a - O53_a - Distance Angles Cl51_a 1.4239 (0.0040) O53_a - O54_a - Distance Angles Cl51_a 1.4455 (0.0049) O54_a - Cl51_a - Distance Angles O52_a 1.4083 (0.0042) O51_a 1.4163 (0.0034) 109.81 (0.26) O53_a 1.4239 (0.0040) 109.07 (0.29) 110.16 (0.25) O54_a 1.4455 (0.0049) 111.86 (0.33) 109.81 (0.27) 106.08 (0.32) Cl51_a - O52_a O51_a O53_a O56_b - Distance Angles Cl56_b 1.4191 (0.0120) O56_b - O57_b - Distance Angles Cl56_b 1.4246 (0.0130) O57_b - O58_b - Distance Angles Cl56_b 1.4108 (0.0142) O58_b - O59_b - Distance Angles Cl56_b 1.4068 (0.0145) O59_b - Cl56_b - Distance Angles O59_b 1.4068 (0.0145) O58_b 1.4108 (0.0142) 105.93 (1.37) O56_b 1.4191 (0.0120) 111.07 (1.21) 110.67 (1.18) O57_b 1.4246 (0.0130) 114.16 (1.36) 105.71 (1.18) 109.11 (1.10) Cl56_b - O59_b O58_b O56_b C61_a - Distance Angles N61_a 1.1513 (0.0089) C62_a 1.4983 (0.0089) 177.55 (0.81) C61_a - N61_a C62_a - Distance Angles C61_a 1.4983 (0.0089) H62A_a 0.9800 109.47 H62B_a 0.9800 109.47 109.47 H62C_a 0.9800 109.47 109.47 109.47 C62_a - C61_a H62A_a H62B_a N61_a - Distance Angles C61_a 1.1513 (0.0089) N61_a - C63_b - Distance Angles N63_b 1.1747 (0.0167) C64_b 1.5276 (0.0167) 149.14 (3.61) C63_b - N63_b C64_b - Distance Angles C63_b 1.5276 (0.0167) H64A_b 0.9800 109.47 H64B_b 0.9800 109.47 109.47 H64C_b 0.9800 109.47 109.47 109.47 C64_b - C63_b H64A_b H64B_b N63_b - Distance Angles C63_b 1.1747 (0.0166) N63_b - C71_a - Distance Angles N71_a 1.1116 (0.0076) C72_a 1.4748 (0.0083) 179.16 (0.67) C71_a - N71_a C72_a - Distance Angles C71_a 1.4748 (0.0083) H72A_a 0.9800 109.47 H72B_a 0.9800 109.47 109.47 H72C_a 0.9800 109.47 109.47 109.47 C72_a - C71_a H72A_a H72B_a N71_a - Distance Angles C71_a 1.1116 (0.0076) N71_a - C73_b - Distance Angles N73_b 1.1695 (0.0159) C74_b 1.5148 (0.0156) 178.15 (1.92) C73_b - N73_b C74_b - Distance Angles C73_b 1.5148 (0.0157) H74A_b 0.9800 109.47 H74B_b 0.9800 109.47 109.47 H74C_b 0.9800 109.47 109.47 109.47 C74_b - C73_b H74A_b H74B_b N73_b - Distance Angles C73_b 1.1695 (0.0159) N73_b - FMAP and GRID set by program FMAP 2 3 43 GRID -1.250 -2 -2 1.250 2 2 R1 = 0.0883 for 9802 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.14 at 0.2319 0.1007 0.0522 [ 1.06 A from O42 ] Deepest hole -0.81 at 0.6001 0.8469 0.4080 [ 0.05 A from H1WB ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 7561 / 40269 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.7681 -0.1007 0.9478 1.00000 0.05 1.14 1.06 O42 1.12 CL41 1.70 O44 1.71 O41 Q2 1 0.8933 0.2252 0.9625 1.00000 0.05 0.83 0.99 C27 1.35 C26 1.46 H27 1.87 H26 Q3 1 0.9085 -0.0299 1.1057 1.00000 0.05 0.66 1.61 N63 2.14 H72C 2.19 H72B 2.30 C63 Q4 1 0.7308 -0.2152 1.1173 1.00000 0.05 0.65 1.01 N61 1.12 N63 1.62 C63 1.83 C61 Q5 1 1.0205 0.3179 0.9839 1.00000 0.05 0.62 0.89 C28 1.46 C27 1.47 H28 1.61 C29 Shortest distances between peaks (including symmetry equivalents) 2 5 1.43 3 4 2.65 1 3 2.68 Time profile in seconds ----------------------- 0.06: Read and process instructions 0.00: Fit rigid groups 0.01: 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 0.01: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 1.52: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.07: Set up l.s. refinement 0.00: Generate idealized H-atoms 18.49: Structure factors and derivatives 146.97: Sum l.s. matrices 0.03: Generate and apply antibumping restraints 0.30: Apply other restraints 12.05: Solve l.s. equations 0.00: Generate HTAB table 0.17: Other dependent quantities, CIF, tables 0.17: Analysis of variance 0.06: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.06: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 04src1114 finished at 21:47:39 Total CPU time: 180.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++