+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 16:42:32 on 15-May-2002 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL DIRDIF output for 02SOT056 CELL 0.71073 10.4568 11.6216 11.7872 61.172 70.776 67.863 ZERR 2.00 0.0004 0.0005 0.0006 0.002 0.002 0.002 LATT 1 SFAC C H N O FE UNIT 58 48 4 6 2 V = 1143.03 F(000) = 524.0 Mu = 0.70 mm-1 Cell Wt = 1008.70 Rho = 1.465 FMAP 2 PLAN 10 BOND $H OMIT -3 55 OMIT 0 0 1 OMIT 3 2 0 EXTI TEMP -153 SIZE 0.14 0.1 0.02 ACTA WGHT 0.04580 0.54720 L.S. 4 FVAR 0.38201 C1 1 0.091170 0.112964 0.185311 11.00000 0.02660 0.02382 = 0.02447 -0.00451 -0.00606 -0.00775 AFIX 43 H1 2 0.147318 0.081255 0.246769 11.00000 -1.20000 AFIX 0 C2 1 0.111274 0.057075 0.095651 11.00000 0.02655 0.02085 = 0.03325 -0.01005 -0.00157 -0.00627 AFIX 43 H2 2 0.182530 -0.017946 0.088089 11.00000 -1.20000 AFIX 0 C3 1 0.003714 0.135471 0.019227 11.00000 0.03183 0.02776 = 0.03046 -0.01216 -0.00420 -0.01510 AFIX 43 H3 2 -0.007834 0.121320 -0.047612 11.00000 -1.20000 AFIX 0 C4 1 -0.082899 0.239048 0.062770 11.00000 0.02041 0.02529 = 0.02958 -0.00822 -0.00475 -0.00881 AFIX 43 H4 2 -0.161690 0.304814 0.029647 11.00000 -1.20000 AFIX 0 C5 1 -0.028877 0.225330 0.165671 11.00000 0.02493 0.02247 = 0.02260 -0.00819 -0.00007 -0.00887 AFIX 43 H5 2 -0.065757 0.280309 0.211861 11.00000 -1.20000 AFIX 0 C6 1 0.175214 0.428357 -0.062826 11.00000 0.02255 0.01996 = 0.02268 -0.00805 -0.00295 -0.00802 AFIX 43 H6 2 0.137860 0.488448 -0.022102 11.00000 -1.20000 AFIX 0 C7 1 0.123916 0.434018 -0.163625 11.00000 0.02319 0.02391 = 0.02165 -0.00439 -0.00559 -0.00717 AFIX 43 H7 2 0.046883 0.498829 -0.200776 11.00000 -1.20000 AFIX 0 C8 1 0.210881 0.323398 -0.197650 11.00000 0.02806 0.03301 = 0.01980 -0.01220 -0.00262 -0.01064 AFIX 43 H8 2 0.201440 0.303872 -0.261819 11.00000 -1.20000 AFIX 0 C9 1 0.314284 0.248099 -0.117095 11.00000 0.02191 0.02877 = 0.02125 -0.01253 -0.00125 -0.00710 AFIX 43 H9 2 0.383413 0.169225 -0.117405 11.00000 -1.20000 AFIX 0 C10 1 0.293750 0.314305 -0.035799 11.00000 0.02053 0.02164 = 0.01710 -0.00621 -0.00176 -0.00798 C11 1 0.500001 0.185652 0.072390 11.00000 0.02084 0.02093 = 0.02019 -0.00767 -0.00191 -0.00796 C12 1 0.562920 0.164610 0.178695 11.00000 0.01658 0.01984 = 0.01920 -0.00682 -0.00185 -0.00648 C13 1 0.531844 0.226664 0.263546 11.00000 0.01918 0.02049 = 0.01751 -0.00715 -0.00069 -0.00881 C14 1 0.631694 0.150694 0.348835 11.00000 0.01734 0.01994 = 0.01900 -0.00772 -0.00050 -0.00744 C15 1 0.719923 0.045125 0.312376 11.00000 0.01780 0.02298 = 0.01771 -0.00870 -0.00134 -0.00817 C16 1 0.844538 -0.064994 0.355663 11.00000 0.01763 0.02088 = 0.01765 -0.00664 -0.00036 -0.00885 C17 1 1.013818 -0.161570 0.490095 11.00000 0.02179 0.02777 = 0.02748 -0.00940 -0.00971 -0.00262 AFIX 137 H17A 2 0.993850 -0.248743 0.541817 11.00000 -1.50000 H17B 2 1.046645 -0.139391 0.542297 11.00000 -1.50000 H17C 2 1.084806 -0.164684 0.414499 11.00000 -1.50000 AFIX 0 C18 1 0.412442 0.343894 0.273302 11.00000 0.01789 0.02229 = 0.02285 -0.01178 -0.00492 -0.00522 C19 1 0.407472 0.476426 0.179933 11.00000 0.02449 0.02491 = 0.02051 -0.00943 -0.00408 -0.00681 AFIX 43 H19 2 0.480999 0.493283 0.108647 11.00000 -1.20000 AFIX 0 C20 1 0.294467 0.583927 0.191498 11.00000 0.03637 0.01913 = 0.02803 -0.00923 -0.01367 -0.00382 AFIX 43 H20 2 0.291656 0.671860 0.127172 11.00000 -1.20000 AFIX 0 C21 1 0.186073 0.560708 0.298332 11.00000 0.02426 0.02727 = 0.04491 -0.01924 -0.01059 -0.00013 AFIX 43 H21 2 0.109920 0.632674 0.305917 11.00000 -1.20000 AFIX 0 C22 1 0.191424 0.429922 0.393897 11.00000 0.02559 0.02997 = 0.04448 -0.01715 0.00540 -0.00661 AFIX 43 H22 2 0.119701 0.414084 0.467043 11.00000 -1.20000 AFIX 0 C23 1 0.303568 0.322056 0.381055 11.00000 0.02578 0.02167 = 0.03559 -0.00907 0.00209 -0.00688 AFIX 43 H23 2 0.305796 0.234193 0.445338 11.00000 -1.20000 AFIX 0 C24 1 0.633309 0.183911 0.454232 11.00000 0.01532 0.02400 = 0.02296 -0.01342 -0.00315 -0.00315 C25 1 0.645060 0.312032 0.423727 11.00000 0.01900 0.02372 = 0.02501 -0.00962 -0.00530 -0.00443 AFIX 43 H25 2 0.657879 0.374108 0.336330 11.00000 -1.20000 AFIX 0 C26 1 0.637668 0.346987 0.523418 11.00000 0.02085 0.02702 = 0.04044 -0.02021 -0.00832 -0.00204 AFIX 43 H26 2 0.645657 0.432346 0.502507 11.00000 -1.20000 AFIX 0 C27 1 0.618530 0.255639 0.653287 11.00000 0.01965 0.03772 = 0.03112 -0.02292 -0.00362 -0.00299 AFIX 43 H27 2 0.612492 0.279727 0.719902 11.00000 -1.20000 AFIX 0 C28 1 0.608354 0.128364 0.684186 11.00000 0.02059 0.03358 = 0.02263 -0.01369 -0.00194 -0.00291 AFIX 43 H28 2 0.596561 0.066466 0.771743 11.00000 -1.20000 AFIX 0 C29 1 0.615570 0.092239 0.585890 11.00000 0.02043 0.02343 = 0.02526 -0.01184 -0.00174 -0.00435 AFIX 43 H29 2 0.608544 0.006252 0.607759 11.00000 -1.20000 AFIX 0 N1 3 0.373811 0.278957 0.057654 11.00000 0.01924 0.02863 = 0.02371 -0.01701 -0.00458 -0.00326 N2 3 0.676570 0.055919 0.209692 11.00000 0.01579 0.02044 = 0.02030 -0.00993 -0.00218 -0.00240 O1 4 0.560537 0.120410 0.004712 11.00000 0.02555 0.03302 = 0.02850 -0.01983 -0.00762 0.00048 O2 4 0.900738 -0.151684 0.312907 11.00000 0.02461 0.02431 = 0.02778 -0.01393 -0.00734 -0.00146 O3 4 0.887166 -0.058690 0.447305 11.00000 0.01997 0.02384 = 0.02345 -0.01165 -0.00769 -0.00101 FE1 5 0.119142 0.254648 -0.003826 11.00000 0.01961 0.02010 = 0.01973 -0.00805 -0.00359 -0.00557 H1N 2 0.343837 0.312805 0.107769 11.00000 0.02217 H2N 2 0.716493 0.002780 0.168855 11.00000 0.03440 HKLF 4 Covalent radii and connectivity table for DIRDIF output for 02SOT056 C 0.770 H 0.320 N 0.700 O 0.660 FE 1.240 C1 - C2 C5 Fe1 C2 - C1 C3 Fe1 C3 - C4 C2 Fe1 C4 - C3 C5 Fe1 C5 - C1 C4 Fe1 C6 - C10 C7 Fe1 C7 - C8 C6 Fe1 C8 - C9 C7 Fe1 C9 - C8 C10 Fe1 C10 - N1 C9 C6 Fe1 C11 - O1 N1 C12 C12 - N2 C13 C11 C13 - C12 C14 C18 C14 - C15 C13 C24 C15 - N2 C14 C16 C16 - O2 O3 C15 C17 - O3 C18 - C23 C19 C13 C19 - C20 C18 C20 - C21 C19 C21 - C20 C22 C22 - C21 C23 C23 - C22 C18 C24 - C29 C25 C14 C25 - C26 C24 C26 - C27 C25 C27 - C26 C28 C28 - C27 C29 C29 - C28 C24 N1 - C11 C10 N2 - C12 C15 O1 - C11 O2 - C16 O3 - C16 C17 Fe1 - C7 C3 C2 C9 C8 C1 C4 C6 C10 C5 16615 Reflections read, of which 6 rejected -13 =< h =< 13, -15 =< k =< 14, -15 =< l =< 15, Max. 2-theta = 54.99 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 0 1 0 215.35 9.02 2 64.95 1 1 0 85.61 1.78 3 29.69 4 8 0 36.88 0.82 5 5.12 5 9 0 53.45 0.98 5 13.40 1 -5 1 90.66 0.96 5 16.96 1 -4 1 206.86 1.00 5 73.11 3 -7 2 75.33 1.63 5 10.85 5 11 2 39.40 0.92 5 8.14 3 -6 3 64.98 0.99 4 26.21 2 -5 3 33.04 0.86 5 5.97 5 6 14 12.33 3.01 2 17.48 11 Inconsistent equivalents 5111 Unique reflections, of which 0 suppressed R(int) = 0.0439 R(sigma) = 0.0588 Friedel opposites merged Maximum memory for data reduction = 3138 / 52373 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 = 4022 / 411142 wR2 = 0.1049 before cycle 1 for 5111 data and 326 / 326 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0458 * P )^2 + 0.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38284 0.00064 1.294 OSF 2 0.00121 0.00086 1.409 EXTI Mean shift/esd = 0.084 Maximum = 1.409 for EXTI Max. shift = 0.005 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 2 Maximum vector length = 511 Memory required = 4022 / 411142 wR2 = 0.1048 before cycle 2 for 5111 data and 326 / 326 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0458 * P )^2 + 0.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38303 0.00065 0.282 OSF 2 0.00163 0.00091 0.456 EXTI Mean shift/esd = 0.028 Maximum = 0.456 for EXTI Max. shift = 0.002 A for H1N Max. dU = 0.000 for Fe1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4022 / 411142 wR2 = 0.1048 before cycle 3 for 5111 data and 326 / 326 parameters GooF = S = 1.039; Restrained GooF = 1.039 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0458 * P )^2 + 0.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38303 0.00065 0.003 OSF 2 0.00162 0.00093 -0.009 EXTI Mean shift/esd = 0.001 Maximum = -0.011 for y H2N Max. shift = 0.000 A for H2N Max. dU = 0.000 for H1N Least-squares cycle 4 Maximum vector length = 511 Memory required = 4022 / 411142 wR2 = 0.1048 before cycle 4 for 5111 data and 326 / 326 parameters GooF = S = 1.039; Restrained GooF = 1.039 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0458 * P )^2 + 0.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38303 0.00065 0.000 OSF 2 0.00161 0.00093 -0.009 EXTI Mean shift/esd = 0.000 Maximum = -0.009 for EXTI Max. shift = 0.000 A for H2N Max. dU = 0.000 for H1N Largest correlation matrix elements -0.618 U23 C27 / U22 C27 -0.570 U23 C29 / U22 C29 -0.551 U23 C15 / U22 C15 -0.606 U23 C26 / U22 C26 -0.570 U23 N1 / U22 N1 -0.546 U23 C14 / U22 C14 -0.605 U23 C21 / U22 C21 -0.567 U23 O3 / U22 O3 -0.546 U23 C26 / U33 C26 -0.597 U23 Fe1 / U22 Fe1 -0.564 U23 C27 / U33 C27 -0.546 U23 C3 / U22 C3 -0.589 U23 C22 / U22 C22 -0.564 U23 C19 / U22 C19 -0.545 U23 C20 / U22 C20 -0.586 U23 O1 / U22 O1 -0.562 U23 C9 / U22 C9 -0.544 U23 C25 / U22 C25 -0.586 U23 C24 / U22 C24 -0.557 U23 C28 / U22 C28 0.544 U33 Fe1 / OSF -0.585 U23 C18 / U22 C18 -0.553 U23 C8 / U22 C8 -0.544 U23 O2 / U22 O2 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C1 ** H1 0.1486 0.0806 0.2481 43 0.950 0.000 C1 C2 C5 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C2 ** H2 0.1840 -0.0195 0.0879 43 0.950 0.000 C2 C1 C3 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C3 ** H3 -0.0081 0.1210 -0.0491 43 0.950 0.000 C3 C4 C2 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C4 ** H4 -0.1635 0.3062 0.0290 43 0.950 0.000 C4 C3 C5 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C5 ** H5 -0.0666 0.2815 0.2128 43 0.950 0.000 C5 C1 C4 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C6 ** H6 0.1370 0.4897 -0.0212 43 0.950 0.000 C6 C10 C7 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C7 ** H7 0.0452 0.5002 -0.2016 43 0.950 0.000 C7 C8 C6 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C8 ** H8 0.2012 0.3035 -0.2632 43 0.950 0.000 C8 C9 C7 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C9 ** H9 0.3849 0.1675 -0.1174 43 0.950 0.000 C9 C8 C10 H17A 0.9935 -0.2506 0.5429 137 0.980 0.000 C17 O3 H17A H17B 1.0474 -0.1389 0.5434 137 0.980 0.000 C17 O3 H17A H17C 1.0863 -0.1648 0.4129 137 0.980 0.000 C17 O3 H17A H19 0.4825 0.4936 0.1071 43 0.950 0.000 C19 C20 C18 H20 0.2916 0.6738 0.1258 43 0.950 0.000 C20 C21 C19 H21 0.1083 0.6343 0.3061 43 0.950 0.000 C21 C20 C22 H22 0.1181 0.4137 0.4686 43 0.950 0.000 C22 C21 C23 H23 0.3059 0.2323 0.4467 43 0.950 0.000 C23 C22 C18 H25 0.6581 0.3755 0.3345 43 0.950 0.000 C25 C26 C24 H26 0.6459 0.4343 0.5020 43 0.950 0.000 C26 C27 C25 H27 0.6124 0.2802 0.7214 43 0.950 0.000 C27 C26 C28 H28 0.5963 0.0651 0.7737 43 0.950 0.000 C28 C27 C29 H29 0.6083 0.0044 0.6082 43 0.950 0.000 C29 C28 C24 DIRDIF output for 02SOT056 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.09119 0.11296 0.18532 1.00000 0.02653 0.02393 0.02460 -0.00465 -0.00604 -0.00766 0.02664 0.00316 0.00024 0.00023 0.00023 0.00000 0.00123 0.00123 0.00116 0.00101 0.00095 0.00094 0.00051 H1 0.14856 0.08056 0.24809 1.00000 0.03196 0.00000 0.00000 C2 0.11124 0.05711 0.09565 1.00000 0.02660 0.02093 0.03318 -0.01009 -0.00165 -0.00620 0.02842 0.00320 0.00025 0.00023 0.00023 0.00000 0.00125 0.00122 0.00130 0.00106 0.00102 0.00093 0.00053 H2 0.18403 -0.01953 0.08792 1.00000 0.03410 0.00000 0.00000 C3 0.00369 0.13548 0.01920 1.00000 0.03200 0.02779 0.03056 -0.01225 -0.00418 -0.01512 0.02804 0.00305 0.00025 0.00024 0.00024 0.00000 0.00133 0.00130 0.00125 0.00109 0.00103 0.00102 0.00053 H3 -0.00809 0.12101 -0.04908 1.00000 0.03364 0.00000 0.00000 C4 -0.08298 0.23908 0.06277 1.00000 0.02055 0.02538 0.02946 -0.00833 -0.00455 -0.00889 0.02549 0.00296 0.00024 0.00023 0.00022 0.00000 0.00115 0.00124 0.00123 0.00104 0.00094 0.00091 0.00050 H4 -0.16349 0.30624 0.02896 1.00000 0.03058 0.00000 0.00000 C5 -0.02891 0.22537 0.16565 1.00000 0.02486 0.02270 0.02259 -0.00815 -0.00019 -0.00881 0.02420 0.00301 0.00023 0.00023 0.00022 0.00000 0.00119 0.00120 0.00113 0.00098 0.00092 0.00091 0.00049 H5 -0.06657 0.28154 0.21282 1.00000 0.02904 0.00000 0.00000 C6 0.17519 0.42834 -0.06278 1.00000 0.02260 0.01997 0.02270 -0.00801 -0.00295 -0.00805 0.02160 0.00282 0.00023 0.00022 0.00021 0.00000 0.00113 0.00113 0.00110 0.00095 0.00089 0.00087 0.00047 H6 0.13701 0.48971 -0.02116 1.00000 0.02593 0.00000 0.00000 C7 0.12389 0.43398 -0.16363 1.00000 0.02318 0.02394 0.02172 -0.00450 -0.00548 -0.00721 0.02437 0.00300 0.00024 0.00023 0.00021 0.00000 0.00118 0.00120 0.00112 0.00098 0.00092 0.00091 0.00049 H7 0.04520 0.50017 -0.20159 1.00000 0.02924 0.00000 0.00000 C8 0.21084 0.32342 -0.19761 1.00000 0.02805 0.03308 0.01988 -0.01214 -0.00254 -0.01074 0.02607 0.00306 0.00024 0.00024 0.00022 0.00000 0.00125 0.00134 0.00110 0.00103 0.00093 0.00098 0.00050 H8 0.20120 0.30348 -0.26316 1.00000 0.03128 0.00000 0.00000 C9 0.31428 0.24808 -0.11709 1.00000 0.02206 0.02905 0.02121 -0.01266 -0.00124 -0.00717 0.02367 0.00288 0.00023 0.00024 0.00021 0.00000 0.00115 0.00126 0.00109 0.00099 0.00089 0.00092 0.00048 H9 0.38489 0.16751 -0.11741 1.00000 0.02841 0.00000 0.00000 C10 0.29375 0.31431 -0.03580 1.00000 0.02038 0.02173 0.01733 -0.00634 -0.00177 -0.00793 0.02023 0.00280 0.00022 0.00022 0.00020 0.00000 0.00111 0.00115 0.00103 0.00092 0.00085 0.00086 0.00046 C11 0.50005 0.18561 0.07241 1.00000 0.02066 0.02081 0.02027 -0.00756 -0.00194 -0.00789 0.02067 0.00282 0.00022 0.00022 0.00021 0.00000 0.00111 0.00114 0.00108 0.00095 0.00088 0.00087 0.00046 C12 0.56289 0.16462 0.17868 1.00000 0.01643 0.01989 0.01920 -0.00682 -0.00180 -0.00640 0.01890 0.00275 0.00021 0.00021 0.00020 0.00000 0.00105 0.00111 0.00103 0.00090 0.00083 0.00082 0.00044 C13 0.53183 0.22667 0.26356 1.00000 0.01918 0.02033 0.01742 -0.00706 -0.00065 -0.00883 0.01883 0.00267 0.00022 0.00021 0.00020 0.00000 0.00108 0.00112 0.00104 0.00091 0.00083 0.00085 0.00045 C14 0.63166 0.15068 0.34884 1.00000 0.01729 0.01995 0.01904 -0.00780 -0.00037 -0.00746 0.01883 0.00269 0.00021 0.00021 0.00020 0.00000 0.00107 0.00111 0.00104 0.00091 0.00083 0.00082 0.00045 C15 0.71990 0.04513 0.31237 1.00000 0.01783 0.02306 0.01776 -0.00882 -0.00137 -0.00813 0.01897 0.00269 0.00022 0.00021 0.00020 0.00000 0.00106 0.00115 0.00102 0.00092 0.00083 0.00085 0.00045 C16 0.84450 -0.06497 0.35567 1.00000 0.01776 0.02087 0.01776 -0.00662 -0.00042 -0.00888 0.01891 0.00275 0.00022 0.00022 0.00020 0.00000 0.00106 0.00113 0.00103 0.00093 0.00084 0.00084 0.00045 C17 1.01388 -0.16157 0.49010 1.00000 0.02175 0.02768 0.02766 -0.00945 -0.00993 -0.00232 0.02637 0.00311 0.00023 0.00024 0.00023 0.00000 0.00119 0.00127 0.00121 0.00104 0.00095 0.00092 0.00051 H17A 0.99351 -0.25057 0.54293 1.00000 0.03956 0.00000 0.00000 H17B 1.04739 -0.13890 0.54337 1.00000 0.03956 0.00000 0.00000 H17C 1.08634 -0.16476 0.41293 1.00000 0.03956 0.00000 0.00000 C18 0.41245 0.34395 0.27327 1.00000 0.01771 0.02240 0.02290 -0.01190 -0.00492 -0.00523 0.01952 0.00268 0.00022 0.00022 0.00021 0.00000 0.00108 0.00116 0.00109 0.00096 0.00086 0.00084 0.00045 C19 0.40741 0.47641 0.17994 1.00000 0.02442 0.02482 0.02061 -0.00952 -0.00419 -0.00672 0.02309 0.00287 0.00023 0.00022 0.00021 0.00000 0.00119 0.00123 0.00110 0.00099 0.00091 0.00091 0.00048 H19 0.48248 0.49360 0.10708 1.00000 0.02771 0.00000 0.00000 C20 0.29446 0.58398 0.19146 1.00000 0.03624 0.01944 0.02791 -0.00928 -0.01366 -0.00400 0.02695 0.00297 0.00025 0.00023 0.00023 0.00000 0.00136 0.00117 0.00123 0.00101 0.00105 0.00096 0.00052 H20 0.29164 0.67380 0.12576 1.00000 0.03234 0.00000 0.00000 C21 0.18606 0.56075 0.29831 1.00000 0.02427 0.02754 0.04498 -0.01929 -0.01078 -0.00020 0.03121 0.00314 0.00025 0.00025 0.00026 0.00000 0.00126 0.00134 0.00149 0.00121 0.00110 0.00096 0.00056 H21 0.10827 0.63426 0.30606 1.00000 0.03745 0.00000 0.00000 C22 0.19139 0.42991 0.39389 1.00000 0.02578 0.03005 0.04440 -0.01725 0.00511 -0.00658 0.03599 0.00357 0.00026 0.00025 0.00027 0.00000 0.00131 0.00143 0.00151 0.00126 0.00113 0.00103 0.00062 H22 0.11810 0.41372 0.46859 1.00000 0.04319 0.00000 0.00000 C23 0.30357 0.32208 0.38106 1.00000 0.02597 0.02172 0.03557 -0.00913 0.00206 -0.00695 0.03082 0.00333 0.00024 0.00024 0.00024 0.00000 0.00127 0.00127 0.00136 0.00111 0.00104 0.00096 0.00056 H23 0.30589 0.23232 0.44674 1.00000 0.03699 0.00000 0.00000 C24 0.63333 0.18386 0.45424 1.00000 0.01510 0.02398 0.02309 -0.01346 -0.00321 -0.00297 0.01982 0.00273 0.00021 0.00022 0.00021 0.00000 0.00104 0.00117 0.00110 0.00097 0.00085 0.00083 0.00045 C25 0.64507 0.31205 0.42374 1.00000 0.01878 0.02384 0.02549 -0.00999 -0.00540 -0.00427 0.02280 0.00284 0.00022 0.00022 0.00022 0.00000 0.00111 0.00120 0.00116 0.00100 0.00090 0.00087 0.00048 H25 0.65813 0.37546 0.33446 1.00000 0.02737 0.00000 0.00000 C26 0.63771 0.34707 0.52335 1.00000 0.02057 0.02725 0.04020 -0.02019 -0.00831 -0.00192 0.02717 0.00297 0.00023 0.00024 0.00024 0.00000 0.00117 0.00126 0.00139 0.00114 0.00101 0.00092 0.00052 H26 0.64590 0.43426 0.50197 1.00000 0.03260 0.00000 0.00000 C27 0.61854 0.25562 0.65332 1.00000 0.01954 0.03794 0.03116 -0.02313 -0.00357 -0.00287 0.02740 0.00305 0.00023 0.00025 0.00023 0.00000 0.00116 0.00141 0.00128 0.00116 0.00096 0.00096 0.00052 H27 0.61237 0.28021 0.72138 1.00000 0.03288 0.00000 0.00000 C28 0.60834 0.12831 0.68423 1.00000 0.02033 0.03365 0.02281 -0.01376 -0.00186 -0.00299 0.02655 0.00308 0.00023 0.00024 0.00023 0.00000 0.00116 0.00134 0.00114 0.00105 0.00091 0.00095 0.00051 H28 0.59632 0.06506 0.77366 1.00000 0.03186 0.00000 0.00000 C29 0.61552 0.09224 0.58588 1.00000 0.02014 0.02354 0.02534 -0.01188 -0.00171 -0.00416 0.02337 0.00297 0.00022 0.00023 0.00022 0.00000 0.00113 0.00119 0.00117 0.00101 0.00091 0.00088 0.00048 H29 0.60825 0.00443 0.60821 1.00000 0.02805 0.00000 0.00000 N1 0.37382 0.27895 0.05762 1.00000 0.01941 0.02855 0.02375 -0.01701 -0.00463 -0.00321 0.02193 0.00249 0.00019 0.00020 0.00019 0.00000 0.00098 0.00106 0.00100 0.00091 0.00078 0.00077 0.00041 N2 0.67656 0.05592 0.20972 1.00000 0.01589 0.02039 0.02032 -0.01005 -0.00229 -0.00232 0.01920 0.00242 0.00018 0.00018 0.00018 0.00000 0.00092 0.00098 0.00094 0.00083 0.00073 0.00072 0.00039 O1 0.56055 0.12042 0.00472 1.00000 0.02560 0.03298 0.02854 -0.01985 -0.00764 0.00050 0.02776 0.00206 0.00016 0.00016 0.00015 0.00000 0.00087 0.00092 0.00086 0.00077 0.00069 0.00068 0.00037 O2 0.90073 -0.15166 0.31289 1.00000 0.02453 0.02438 0.02782 -0.01397 -0.00731 -0.00140 0.02506 0.00199 0.00016 0.00015 0.00015 0.00000 0.00084 0.00087 0.00084 0.00074 0.00067 0.00065 0.00036 O3 0.88717 -0.05869 0.44730 1.00000 0.01999 0.02394 0.02357 -0.01166 -0.00783 -0.00093 0.02215 0.00192 0.00015 0.00015 0.00014 0.00000 0.00078 0.00084 0.00078 0.00068 0.00063 0.00060 0.00034 Fe1 0.11915 0.25465 -0.00383 1.00000 0.01973 0.02025 0.01990 -0.00811 -0.00364 -0.00559 0.01989 0.00040 0.00003 0.00003 0.00003 0.00000 0.00018 0.00019 0.00018 0.00014 0.00012 0.00012 0.00012 H1N 0.34395 0.31347 0.10728 1.00000 0.02261 0.03285 0.00259 0.00246 0.00242 0.00000 0.00682 H2N 0.71583 0.00273 0.16907 1.00000 0.03461 0.03527 0.00278 0.00271 0.00258 0.00000 0.00742 Final Structure Factor Calculation for DIRDIF output for 02SOT056 Total number of l.s. parameters = 326 Maximum vector length = 511 Memory required = 3696 / 24017 wR2 = 0.1048 before cycle 5 for 5111 data and 0 / 326 parameters GooF = S = 1.040; Restrained GooF = 1.040 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0458 * P )^2 + 0.55 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0435 for 3995 Fo > 4sig(Fo) and 0.0651 for all 5111 data wR2 = 0.1048, GooF = S = 1.040, Restrained GooF = 1.040 for all data Occupancy sum of asymmetric unit = 35.00 for non-hydrogen and 24.00 for hydrogen atoms Principal mean square atomic displacements U 0.0334 0.0260 0.0205 C1 0.0391 0.0255 0.0207 C2 0.0360 0.0306 0.0176 C3 0.0332 0.0254 0.0179 C4 0.0295 0.0242 0.0189 C5 0.0241 0.0232 0.0176 C6 0.0313 0.0225 0.0192 C7 0.0337 0.0262 0.0183 C8 0.0291 0.0235 0.0184 C9 0.0236 0.0209 0.0162 C10 0.0228 0.0219 0.0173 C11 0.0219 0.0197 0.0151 C12 0.0227 0.0193 0.0145 C13 0.0219 0.0200 0.0146 C14 0.0237 0.0176 0.0156 C15 0.0227 0.0205 0.0135 C16 0.0318 0.0301 0.0173 C17 0.0247 0.0193 0.0146 C18 0.0249 0.0243 0.0200 C19 0.0401 0.0216 0.0191 C20 0.0456 0.0276 0.0204 C21 0.0562 0.0304 0.0213 C22 0.0480 0.0233 0.0211 C23 0.0266 0.0179 0.0150 C24 0.0256 0.0246 0.0182 C25 0.0414 0.0208 0.0193 C26 0.0426 0.0217 0.0179 C27 0.0374 0.0243 0.0180 C28 0.0270 0.0247 0.0185 C29 0.0321 0.0191 0.0146 N1 0.0224 0.0205 0.0147 N2 0.0418 0.0234 0.0181 O1 0.0321 0.0233 0.0197 O2 0.0293 0.0205 0.0167 O3 0.0204 0.0199 0.0194 Fe1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.014 0.027 0.040 0.053 0.067 0.082 0.102 0.130 0.178 1.000 Number in group 522. 515. 517. 520. 481. 513. 521. 514. 499. 509. GooF 0.902 0.987 1.057 1.128 1.110 1.136 1.054 0.952 0.956 1.086 K 1.717 1.072 1.020 0.990 0.982 0.982 0.986 0.995 1.018 1.023 Resolution(A) 0.77 0.80 0.84 0.87 0.92 0.98 1.05 1.16 1.32 1.66 inf Number in group 511. 530. 500. 506. 521. 505. 503. 514. 508. 513. GooF 0.912 0.926 0.901 0.899 0.954 1.063 1.015 0.930 1.198 1.458 K 1.062 1.040 1.022 1.004 0.994 1.014 1.025 1.031 1.036 0.997 R1 0.191 0.138 0.105 0.080 0.067 0.056 0.045 0.038 0.036 0.032 Recommended weighting scheme: WGHT 0.0418 0.5991 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) 4 2 5 73.76 36.92 5.28 0.037 1.97 4 4 6 141.82 86.54 4.83 0.057 1.78 1 7 5 24.99 6.39 4.20 0.015 1.55 1 5 5 19.89 43.62 4.03 0.040 1.96 4 -2 2 19.95 42.58 4.02 0.040 1.81 -3 3 0 515.52 403.90 4.00 0.123 2.03 3 5 1 8.73 28.96 4.00 0.033 2.08 -1 8 11 80.11 135.09 3.97 0.071 0.91 2 3 6 27.78 52.63 3.88 0.044 1.96 1 6 4 107.84 154.80 3.78 0.076 1.85 5 0 4 -5.21 9.87 3.78 0.019 1.68 -2 5 2 85.00 124.36 3.77 0.068 1.74 3 8 11 94.91 145.78 3.68 0.074 1.02 -1 7 6 46.61 77.62 3.66 0.054 1.31 3 -2 2 1123.23 917.79 3.63 0.185 2.11 -3 3 1 55.83 84.36 3.59 0.056 2.04 5 -6 3 80.14 122.40 3.56 0.067 1.00 1 -2 4 399.66 503.66 3.55 0.137 1.93 3 6 1 52.23 79.14 3.45 0.054 1.77 3 4 5 618.17 499.94 3.44 0.136 2.14 1 5 7 8.72 25.49 3.42 0.031 1.57 4 8 3 159.41 211.47 3.38 0.089 1.41 0 6 6 21.50 6.83 3.34 0.016 1.53 0 -3 4 34.06 14.22 3.34 0.023 1.70 3 1 5 52.38 32.27 3.30 0.035 2.05 2 5 6 17.38 3.81 3.29 0.012 1.81 2 5 2 191.45 244.28 3.26 0.095 2.30 0 4 4 429.10 338.05 3.24 0.112 2.30 7 6 5 3.48 20.68 3.23 0.028 1.36 -6 -7 2 240.06 307.26 3.22 0.107 1.07 -2 -5 1 89.83 121.60 3.17 0.067 1.81 -6 5 4 25.34 49.20 3.17 0.043 1.05 5 -1 2 210.10 164.92 3.14 0.078 1.74 0 -2 2 122.78 93.15 3.13 0.059 2.97 4 3 6 882.65 734.95 3.12 0.165 1.79 12 9 6 47.63 1.68 3.11 0.008 0.83 0 2 5 410.35 500.10 3.09 0.136 2.23 -1 5 4 264.95 212.03 3.09 0.089 1.81 2 11 7 180.38 235.09 3.07 0.093 1.02 -3 -1 3 155.16 196.79 3.07 0.086 2.05 -2 3 2 145.47 185.59 3.05 0.083 2.39 -2 -2 4 469.60 388.40 3.03 0.120 1.78 1 -1 5 239.48 191.84 3.02 0.084 1.85 4 2 0 111.82 84.77 3.02 0.056 2.41 3 10 8 25.12 47.11 3.01 0.042 1.09 5 -2 2 31.61 16.61 2.99 0.025 1.57 -1 5 3 8.39 21.74 2.98 0.028 1.91 -2 7 9 101.39 144.65 2.97 0.073 1.02 -1 4 1 195.78 243.05 2.95 0.095 2.36 -1 1 6 127.54 165.78 2.92 0.079 1.69 Bond lengths and angles C1 - Distance Angles C2 1.4126 (0.0034) C5 1.4145 (0.0032) 108.32 (0.21) Fe1 2.0398 (0.0023) 69.47 (0.13) 70.21 (0.13) H1 0.9500 125.84 125.84 126.05 C1 - C2 C5 Fe1 C2 - Distance Angles C1 1.4126 (0.0034) C3 1.4179 (0.0034) 108.02 (0.20) Fe1 2.0336 (0.0023) 69.95 (0.13) 69.55 (0.13) H2 0.9500 125.99 125.99 126.09 C2 - C1 C3 Fe1 C3 - Distance Angles C4 1.4150 (0.0033) C2 1.4179 (0.0034) 107.78 (0.21) Fe1 2.0326 (0.0022) 70.09 (0.13) 69.63 (0.13) H3 0.9500 126.11 126.11 125.75 C3 - C4 C2 Fe1 C4 - Distance Angles C3 1.4150 (0.0033) C5 1.4188 (0.0032) 108.22 (0.21) Fe1 2.0432 (0.0022) 69.28 (0.13) 70.03 (0.12) H4 0.9500 125.89 125.89 126.37 C4 - C3 C5 Fe1 C5 - Distance Angles C1 1.4145 (0.0032) C4 1.4188 (0.0032) 107.65 (0.20) Fe1 2.0514 (0.0022) 69.33 (0.13) 69.42 (0.12) H5 0.9500 126.17 126.17 126.64 C5 - C1 C4 Fe1 C6 - Distance Angles C10 1.4175 (0.0030) C7 1.4225 (0.0032) 107.41 (0.20) Fe1 2.0424 (0.0021) 70.05 (0.12) 69.13 (0.12) H6 0.9500 126.30 126.30 126.10 C6 - C10 C7 Fe1 C7 - Distance Angles C8 1.4192 (0.0033) C6 1.4225 (0.0032) 108.04 (0.20) Fe1 2.0309 (0.0022) 69.82 (0.13) 70.00 (0.12) H7 0.9500 125.98 125.98 125.78 C7 - C8 C6 Fe1 C8 - Distance Angles C9 1.4136 (0.0032) C7 1.4192 (0.0033) 108.21 (0.20) Fe1 2.0372 (0.0022) 69.58 (0.13) 69.34 (0.12) H8 0.9500 125.89 125.89 126.76 C8 - C9 C7 Fe1 C9 - Distance Angles C8 1.4136 (0.0032) C10 1.4169 (0.0031) 107.72 (0.20) Fe1 2.0344 (0.0022) 69.79 (0.13) 70.32 (0.12) H9 0.9500 126.14 126.14 125.33 C9 - C8 C10 Fe1 C10 - Distance Angles N1 1.4121 (0.0028) C9 1.4169 (0.0031) 128.31 (0.20) C6 1.4175 (0.0030) 123.10 (0.20) 108.59 (0.19) Fe1 2.0506 (0.0021) 127.57 (0.15) 69.09 (0.12) 69.43 (0.12) C10 - N1 C9 C6 C11 - Distance Angles O1 1.2248 (0.0026) N1 1.3563 (0.0029) 123.86 (0.21) C12 1.4788 (0.0031) 120.53 (0.20) 115.61 (0.19) C11 - O1 N1 C12 - Distance Angles N2 1.3607 (0.0027) C13 1.3899 (0.0029) 107.96 (0.19) C11 1.4788 (0.0031) 116.21 (0.19) 135.76 (0.20) C12 - N2 C13 C13 - Distance Angles C12 1.3899 (0.0029) C14 1.4214 (0.0029) 107.12 (0.19) C18 1.4843 (0.0029) 128.02 (0.19) 124.73 (0.19) C13 - C12 C14 C14 - Distance Angles C15 1.3912 (0.0030) C13 1.4214 (0.0029) 106.78 (0.18) C24 1.4743 (0.0029) 129.51 (0.19) 123.72 (0.19) C14 - C15 C13 C15 - Distance Angles N2 1.3627 (0.0028) C14 1.3912 (0.0030) 108.05 (0.19) C16 1.4653 (0.0030) 116.99 (0.19) 134.91 (0.20) C15 - N2 C14 C16 - Distance Angles O2 1.2096 (0.0025) O3 1.3375 (0.0026) 124.50 (0.20) C15 1.4653 (0.0030) 123.00 (0.20) 112.49 (0.18) C16 - O2 O3 C17 - Distance Angles O3 1.4507 (0.0026) H17A 0.9800 109.47 H17B 0.9800 109.47 109.47 H17C 0.9800 109.47 109.47 109.47 C17 - O3 H17A H17B C18 - Distance Angles C23 1.3890 (0.0031) C19 1.3880 (0.0031) 118.37 (0.20) C13 1.4843 (0.0029) 119.36 (0.19) 122.24 (0.19) C18 - C23 C19 C19 - Distance Angles C20 1.3862 (0.0032) C18 1.3880 (0.0031) 120.98 (0.21) H19 0.9500 119.51 119.51 C19 - C20 C18 C20 - Distance Angles C21 1.3808 (0.0035) C19 1.3862 (0.0032) 120.09 (0.22) H20 0.9500 119.96 119.96 C20 - C21 C19 C21 - Distance Angles C20 1.3808 (0.0035) C22 1.3820 (0.0036) 119.60 (0.22) H21 0.9500 120.20 120.20 C21 - C20 C22 C22 - Distance Angles C21 1.3820 (0.0036) C23 1.3884 (0.0033) 120.18 (0.23) H22 0.9500 119.91 119.91 C22 - C21 C23 C23 - Distance Angles C22 1.3884 (0.0033) C18 1.3890 (0.0031) 120.74 (0.22) H23 0.9500 119.63 119.63 C23 - C22 C18 C24 - Distance Angles C29 1.3935 (0.0031) C25 1.3986 (0.0030) 118.73 (0.20) C14 1.4743 (0.0029) 121.16 (0.19) 120.01 (0.19) C24 - C29 C25 C25 - Distance Angles C26 1.3885 (0.0032) C24 1.3986 (0.0030) 120.30 (0.20) H25 0.9500 119.85 119.85 C25 - C26 C24 C26 - Distance Angles C27 1.3801 (0.0034) C25 1.3885 (0.0032) 120.21 (0.22) H26 0.9500 119.89 119.89 C26 - C27 C25 C27 - Distance Angles C26 1.3801 (0.0034) C28 1.3809 (0.0033) 119.86 (0.21) H27 0.9500 120.07 120.07 C27 - C26 C28 C28 - Distance Angles C27 1.3809 (0.0033) C29 1.3831 (0.0032) 120.46 (0.21) H28 0.9500 119.77 119.77 C28 - C27 C29 C29 - Distance Angles C28 1.3831 (0.0032) C24 1.3935 (0.0031) 120.42 (0.21) H29 0.9500 119.79 119.79 C29 - C28 C24 N1 - Distance Angles C11 1.3563 (0.0029) C10 1.4121 (0.0028) 125.51 (0.20) H1N 0.7828 (0.0249) 115.33 (1.83) 119.14 (1.83) N1 - C11 C10 N2 - Distance Angles C12 1.3607 (0.0027) C15 1.3627 (0.0028) 110.09 (0.18) H2N 0.8632 (0.0270) 124.55 (1.79) 125.36 (1.79) N2 - C12 C15 O1 - Distance Angles C11 1.2248 (0.0026) O1 - O2 - Distance Angles C16 1.2096 (0.0025) O2 - O3 - Distance Angles C16 1.3375 (0.0026) C17 1.4507 (0.0026) 115.15 (0.17) O3 - C16 Fe1 - Distance Angles C7 2.0309 (0.0022) C3 2.0326 (0.0022) 121.35 (0.10) C2 2.0336 (0.0023) 155.94 (0.10) 40.82 (0.10) C9 2.0344 (0.0022) 68.74 (0.09) 121.42 (0.09) 104.88 (0.09) C8 2.0372 (0.0022) 40.84 (0.09) 105.76 (0.10) 119.40 (0.10) 40.63 (0.09) C1 2.0398 (0.0023) 162.57 (0.09) 68.44 (0.10) 40.58 (0.10) 120.41 (0.09) 155.30 (0.10) C4 2.0432 (0.0022) 108.94 (0.09) 40.63 (0.09) 68.31 (0.09) 159.02 (0.09) 123.99 (0.09) 68.13 (0.09) C6 2.0424 (0.0021) 40.88 (0.09) 158.37 (0.09) 160.35 (0.10) 68.75 (0.09) 68.62 (0.09) 125.37 (0.09) 124.06 (0.09) C10 2.0506 (0.0021) 68.22 (0.09) 158.56 (0.09) 122.84 (0.09) 40.59 (0.09) 68.00 (0.09) 108.16 (0.09) 159.61 (0.09) C5 2.0514 (0.0022) 126.22 (0.09) 68.41 (0.09) 68.25 (0.09) 157.26 (0.09) 161.75 (0.09) 40.45 (0.09) 40.55 (0.09) Fe1 - C7 C3 C2 C9 C8 C1 C4 FMAP and GRID set by program FMAP 2 3 35 GRID -1.563 -2 -2 1.563 2 2 R1 = 0.0630 for 5111 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.46 at 0.3469 0.7633 -0.0010 [ 1.43 A from H20 ] Deepest hole -0.51 at 0.0418 0.2761 0.0132 [ 0.74 A from FE1 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 3585 / 29324 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3469 0.7633 -0.0010 1.00000 0.05 0.46 1.43 H20 1.72 C11 1.89 C12 1.91 O1 Q2 1 0.1744 0.3851 -0.1842 1.00000 0.05 0.34 0.69 C7 0.74 C8 1.49 H7 1.53 H8 Q3 1 0.6204 0.1431 0.5147 1.00000 0.05 0.30 0.64 C24 0.76 C29 1.48 H29 1.80 C25 Q4 1 0.4667 0.1614 0.6268 1.00000 0.05 0.30 1.50 C29 1.67 C28 1.92 H29 2.15 H28 Q5 1 0.6805 0.0873 0.3415 1.00000 0.05 0.29 0.67 C15 0.75 C14 1.77 N2 1.87 C13 Q6 1 -0.0624 0.3787 -0.1404 1.00000 0.05 0.27 1.86 H7 1.86 H4 2.14 C4 2.17 C7 Q7 1 0.1162 0.0978 0.1251 1.00000 0.05 0.26 0.73 C2 0.75 C1 1.48 H2 1.50 H1 Q8 1 -0.0151 0.3713 -0.0136 1.00000 0.05 0.26 1.53 FE1 1.66 C4 1.77 H6 1.80 H4 Q9 1 0.0227 0.2634 -0.1407 1.00000 0.05 0.25 1.57 H3 1.75 C3 2.00 H8 2.11 FE1 Q10 1 0.1179 0.0985 0.2196 1.00000 0.05 0.24 0.46 H1 0.49 C1 1.72 C5 1.77 C2 Shortest distances between peaks (including symmetry equivalents) 7 10 1.12 6 9 1.30 6 8 1.68 3 4 1.73 8 9 2.24 3 5 2.26 2 9 2.29 2 8 2.30 2 6 2.38 7 8 2.80 Time profile in seconds ----------------------- 0.11: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.38: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.39: Structure factors and derivatives 3.31: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.27: Solve l.s. equations 0.00: Generate HTAB table 0.17: Other dependent quantities, CIF, tables 0.20: Analysis of variance 0.11: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 16:42:38 Total elapsed time: 6.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++