+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 10:46:59 on 05-Jun-2002 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 02SOT064 in Pbca CELL 0.71073 6.0816 24.8503 31.1200 90.000 90.000 90.000 ZERR 8.00 0.0004 0.0016 0.0027 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N O FE UNIT 240 208 16 24 8 V = 4703.15 F(000) = 2160.0 Mu = 0.68 mm-1 Cell Wt = 4147.02 Rho = 1.464 MERG 2 OMIT -3.00 55.00 OMIT 5 4 1 OMIT 2 0 14 OMIT 1 4 7 OMIT 2 2 14 EXTI 0.00044 FMAP 2 PLAN 10 SIZE 0.03 0.03 0.20 ACTA BOND $H WGHT 0.04000 4.99410 L.S. 4 TEMP -153.00 FVAR 0.08509 C1 1 0.720878 0.435945 0.079778 11.00000 0.03140 0.06008 = 0.02079 0.00078 -0.00016 -0.00459 AFIX 43 H1 2 0.868228 0.435512 0.069650 11.00000 -1.20000 AFIX 0 C2 1 0.592162 0.390708 0.089799 11.00000 0.06175 0.03160 = 0.02377 -0.00900 -0.01569 0.01718 AFIX 43 H2 2 0.636838 0.354182 0.087579 11.00000 -1.20000 AFIX 0 C3 1 0.384903 0.409168 0.103735 11.00000 0.03799 0.03260 = 0.02338 0.00189 -0.01225 -0.01495 AFIX 43 H3 2 0.265300 0.387111 0.112416 11.00000 -1.20000 AFIX 0 C4 1 0.385052 0.465421 0.102627 11.00000 0.02938 0.03006 = 0.02107 0.00510 -0.00470 0.00267 AFIX 43 H4 2 0.266999 0.488355 0.110643 11.00000 -1.20000 AFIX 0 C5 1 0.592819 0.481781 0.087411 11.00000 0.04848 0.02431 = 0.02276 0.00237 -0.00570 -0.00356 AFIX 43 H5 2 0.638444 0.517933 0.083054 11.00000 -1.20000 AFIX 0 C6 1 0.549041 0.459532 0.203932 11.00000 0.02977 0.02403 = 0.02309 -0.00207 -0.00456 0.00641 AFIX 43 H6 2 0.412872 0.474226 0.213211 11.00000 -1.20000 AFIX 0 C7 1 0.732276 0.489195 0.189752 11.00000 0.03816 0.01788 = 0.03227 0.00020 -0.00894 -0.00697 AFIX 43 H7 2 0.741245 0.527289 0.187886 11.00000 -1.20000 AFIX 0 C8 1 0.900259 0.452582 0.178793 11.00000 0.02164 0.04568 = 0.02130 0.00473 -0.00542 -0.00527 AFIX 43 H8 2 1.041913 0.461627 0.168145 11.00000 -1.20000 AFIX 0 C9 1 0.820779 0.400218 0.186435 11.00000 0.02532 0.02388 = 0.02149 0.00133 -0.00243 0.00556 AFIX 43 H9 2 0.900210 0.367791 0.181914 11.00000 -1.20000 AFIX 0 C10 1 0.601864 0.404055 0.202039 11.00000 0.02468 0.01760 = 0.01533 -0.00146 -0.00554 0.00351 C11 1 0.453709 0.358135 0.215090 11.00000 0.03450 0.02154 = 0.01735 -0.00398 0.00153 0.00430 AFIX 23 H11A 2 0.467840 0.351663 0.246358 11.00000 -1.20000 H11B 2 0.298794 0.367655 0.208949 11.00000 -1.20000 AFIX 0 C12 1 0.565604 0.262920 0.210785 11.00000 0.01622 0.02358 = 0.02613 0.00364 0.00210 -0.00408 C13 1 0.633638 0.219859 0.181054 11.00000 0.02241 0.01133 = 0.02712 0.00634 0.00021 0.00062 C14 1 0.574925 0.204514 0.139405 11.00000 0.02622 0.01340 = 0.02523 0.00370 0.00466 -0.00275 C15 1 0.720860 0.161234 0.127419 11.00000 0.02433 0.01623 = 0.02578 -0.00185 0.00718 -0.00412 C16 1 0.861328 0.153511 0.161489 11.00000 0.02550 0.02029 = 0.02422 -0.00865 0.00626 -0.00446 C17 1 0.404004 0.230004 0.112170 11.00000 0.02760 0.01467 = 0.02157 -0.00107 0.00158 -0.00224 C18 1 0.205805 0.247738 0.129305 11.00000 0.02998 0.01888 = 0.03389 -0.00132 -0.00211 -0.00485 AFIX 43 H18 2 0.173769 0.241138 0.158715 11.00000 -1.20000 AFIX 0 C19 1 0.052837 0.275161 0.103879 11.00000 0.02353 0.02535 = 0.03792 -0.00331 0.00083 -0.00456 AFIX 43 H19 2 -0.082191 0.286891 0.116037 11.00000 -1.20000 AFIX 0 C20 1 0.097676 0.285199 0.061195 11.00000 0.03601 0.02370 = 0.04391 -0.00439 -0.01254 0.00488 AFIX 43 H20 2 -0.006291 0.303859 0.043960 11.00000 -1.20000 AFIX 0 C21 1 0.295010 0.267998 0.043428 11.00000 0.04918 0.02049 = 0.02539 -0.00285 -0.00589 -0.00187 AFIX 43 H21 2 0.326300 0.274813 0.014019 11.00000 -1.20000 AFIX 0 C22 1 0.445601 0.240948 0.068665 11.00000 0.03054 0.02293 = 0.03479 0.00148 0.00030 0.00256 AFIX 43 H22 2 0.580501 0.229478 0.056295 11.00000 -1.20000 AFIX 0 C23 1 0.717105 0.132228 0.085524 11.00000 0.02583 0.01584 = 0.02501 0.00383 0.00008 -0.00160 C24 1 0.898991 0.133938 0.058369 11.00000 0.02703 0.02458 = 0.02884 0.00578 -0.00151 0.00064 AFIX 43 H24 2 1.026729 0.153346 0.066649 11.00000 -1.20000 AFIX 0 C25 1 0.893514 0.107433 0.019450 11.00000 0.04056 0.03194 = 0.02610 0.00336 0.00831 0.01442 AFIX 43 H25 2 1.017562 0.109066 0.000942 11.00000 -1.20000 AFIX 0 C26 1 0.710852 0.078641 0.007034 11.00000 0.04750 0.03058 = 0.02092 -0.00160 -0.00801 0.00684 AFIX 43 H26 2 0.709694 0.060085 -0.019655 11.00000 -1.20000 AFIX 0 C27 1 0.528062 0.076914 0.033840 11.00000 0.03297 0.03279 = 0.03121 -0.00561 -0.01301 0.00312 AFIX 43 H27 2 0.400811 0.057397 0.025437 11.00000 -1.20000 AFIX 0 C28 1 0.532183 0.103590 0.072598 11.00000 0.03032 0.02762 = 0.02573 0.00041 -0.00102 0.00034 AFIX 43 H28 2 0.406811 0.102415 0.090784 11.00000 -1.20000 AFIX 0 C29 1 1.051142 0.117689 0.165631 11.00000 0.02645 0.02062 = 0.02200 0.00282 0.00404 -0.00554 C30 1 1.351819 0.094131 0.209149 11.00000 0.02578 0.03050 = 0.03621 -0.00251 -0.00516 0.01027 AFIX 137 H30A 2 1.308235 0.056237 0.211022 11.00000 -1.50000 H30B 2 1.425857 0.104776 0.235797 11.00000 -1.50000 H30C 2 1.452302 0.099005 0.184840 11.00000 -1.50000 AFIX 0 N1 3 0.512440 0.309503 0.191697 11.00000 0.03687 0.02056 = 0.01888 -0.00031 0.00183 -0.00329 N2 3 0.803406 0.188137 0.193475 11.00000 0.02745 0.02066 = 0.02051 -0.00380 -0.00039 -0.00309 O1 4 0.565708 0.256157 0.250059 11.00000 0.02934 0.02539 = 0.02065 0.00108 0.00163 0.00194 O2 4 1.106838 0.084344 0.139742 11.00000 0.03274 0.02969 = 0.02917 -0.00583 0.00005 0.00373 O3 4 1.159314 0.127025 0.202959 11.00000 0.02999 0.02953 = 0.02596 -0.00318 -0.00545 0.00482 FE1 5 0.626900 0.438204 0.142674 11.00000 0.02969 0.02350 = 0.02113 0.00050 -0.00335 -0.00094 H1N 2 0.508452 0.311353 0.166116 11.00000 0.04217 H2N 2 0.886774 0.196712 0.214054 11.00000 0.00637 HKLF 4 Covalent radii and connectivity table for 02SOT064 in Pbca C 0.770 H 0.320 N 0.700 O 0.660 FE 1.240 C1 - C5 C2 Fe1 C2 - C1 C3 Fe1 C3 - C4 C2 Fe1 C4 - C3 C5 Fe1 C5 - C1 C4 Fe1 C6 - C7 C10 Fe1 C7 - C6 C8 Fe1 C8 - C9 C7 Fe1 C9 - C8 C10 Fe1 C10 - C6 C9 C11 Fe1 C11 - N1 C10 C12 - O1 N1 C13 C13 - N2 C14 C12 C14 - C13 C15 C17 C15 - C16 C14 C23 C16 - N2 C15 C29 C17 - C18 C22 C14 C18 - C17 C19 C19 - C20 C18 C20 - C19 C21 C21 - C22 C20 C22 - C21 C17 C23 - C28 C24 C15 C24 - C25 C23 C25 - C26 C24 C26 - C25 C27 C27 - C28 C26 C28 - C27 C23 C29 - O2 O3 C16 C30 - O3 N1 - C12 C11 N2 - C13 C16 O1 - C12 O2 - C29 O3 - C29 C30 Fe1 - C9 C6 C2 C8 C3 C10 C1 C7 C5 C4 11518 Reflections read, of which 805 rejected -6 =< h =< 6, -28 =< k =< 27, -38 =< l =< 28, Max. 2-theta = 52.01 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 4 2 3 29.83 0.97 3 13.19 4 3 6 5.93 0.59 4 5.98 6 3 17 -2.64 1.91 2 11.90 3 Inconsistent equivalents 3464 Unique reflections, of which 0 suppressed R(int) = 0.0691 R(sigma) = 0.1134 Friedel opposites merged Maximum memory for data reduction = 3307 / 35441 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 = 4218 / 423337 wR2 = 0.1247 before cycle 1 for 3464 data and 335 / 335 parameters GooF = S = 0.988; Restrained GooF = 0.988 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0400 * P )^2 + 4.99 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.08510 0.00020 0.046 OSF 2 0.00046 0.00015 0.147 EXTI Mean shift/esd = 0.145 Maximum = -0.819 for U11 Fe1 Max. shift = 0.029 A for H1N Max. dU =-0.002 for H1N Least-squares cycle 2 Maximum vector length = 511 Memory required = 4218 / 423337 wR2 = 0.1244 before cycle 2 for 3464 data and 335 / 335 parameters GooF = S = 0.987; Restrained GooF = 0.987 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0400 * P )^2 + 4.99 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.08508 0.00020 -0.082 OSF 2 0.00047 0.00015 0.046 EXTI Mean shift/esd = 0.049 Maximum = -0.287 for U11 Fe1 Max. shift = 0.013 A for H1N Max. dU =-0.002 for H1N Least-squares cycle 3 Maximum vector length = 511 Memory required = 4218 / 423337 wR2 = 0.1243 before cycle 3 for 3464 data and 335 / 335 parameters GooF = S = 0.986; Restrained GooF = 0.986 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0400 * P )^2 + 4.99 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.08508 0.00020 -0.006 OSF 2 0.00047 0.00015 -0.001 EXTI Mean shift/esd = 0.005 Maximum = 0.067 for x H1N Max. shift = 0.003 A for H1N Max. dU =-0.001 for H1N Least-squares cycle 4 Maximum vector length = 511 Memory required = 4218 / 423337 wR2 = 0.1243 before cycle 4 for 3464 data and 335 / 335 parameters GooF = S = 0.986; Restrained GooF = 0.986 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0400 * P )^2 + 4.99 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.08508 0.00020 -0.003 OSF 2 0.00047 0.00015 -0.002 EXTI Mean shift/esd = 0.001 Maximum = 0.020 for x H1N Max. shift = 0.001 A for H1N Max. dU = 0.000 for H1N Largest correlation matrix elements 0.525 U11 H1N / U33 N1 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 0.8680 0.4355 0.0697 43 0.950 0.000 C1 C5 C2 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C2 ** H2 0.6378 0.3542 0.0875 43 0.950 0.000 C2 C1 C3 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C3 ** H3 0.2656 0.3871 0.1124 43 0.950 0.000 C3 C4 C2 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C4 ** H4 0.2674 0.4884 0.1107 43 0.950 0.000 C4 C3 C5 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C5 ** H5 0.6391 0.5179 0.0829 43 0.950 0.000 C5 C1 C4 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C6 ** H6 0.4133 0.4743 0.2134 43 0.950 0.000 C6 C7 C10 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C7 ** H7 0.7413 0.5273 0.1877 43 0.950 0.000 C7 C6 C8 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C8 ** H8 1.0414 0.4616 0.1682 43 0.950 0.000 C8 C9 C7 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C9 ** H9 0.9004 0.3678 0.1819 43 0.950 0.000 C9 C8 C10 H11A 0.4680 0.3517 0.2463 23 0.990 0.000 C11 N1 C10 H11B 0.2990 0.3677 0.2089 23 0.990 0.000 C11 N1 C10 H18 0.1735 0.2410 0.1587 43 0.950 0.000 C18 C17 C19 H19 -0.0821 0.2869 0.1160 43 0.950 0.000 C19 C20 C18 H20 -0.0053 0.3040 0.0440 43 0.950 0.000 C20 C19 C21 H21 0.3265 0.2748 0.0140 43 0.950 0.000 C21 C22 C20 H22 0.5807 0.2294 0.0563 43 0.950 0.000 C22 C21 C17 H24 1.0266 0.1535 0.0667 43 0.950 0.000 C24 C25 C23 H25 1.0179 0.1091 0.0009 43 0.950 0.000 C25 C26 C24 H26 0.7109 0.0600 -0.0196 43 0.950 0.000 C26 C25 C27 H27 0.4016 0.0574 0.0253 43 0.950 0.000 C27 C28 C26 H28 0.4066 0.1024 0.0907 43 0.950 0.000 C28 C27 C23 H30A 1.3085 0.0562 0.2110 137 0.980 0.000 C30 O3 H30A H30B 1.4259 0.1047 0.2358 137 0.980 0.000 C30 O3 H30A H30C 1.4525 0.0990 0.1849 137 0.980 0.000 C30 O3 H30A 02SOT064 in Pbca ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.72058 0.43596 0.07981 1.00000 0.03423 0.05792 0.02105 0.00072 -0.00001 -0.00457 0.03773 0.00896 0.00085 0.00024 0.00016 0.00000 0.00328 0.00417 0.00289 0.00291 0.00237 0.00329 0.00139 H1 0.86799 0.43553 0.06972 1.00000 0.04528 0.00000 0.00000 C2 0.59281 0.39074 0.08975 1.00000 0.06179 0.03142 0.02353 -0.00926 -0.01450 0.01880 0.03891 0.00877 0.00092 0.00022 0.00015 0.00000 0.00415 0.00350 0.00307 0.00265 0.00277 0.00314 0.00144 H2 0.63781 0.35425 0.08747 1.00000 0.04670 0.00000 0.00000 C3 0.38507 0.40913 0.10375 1.00000 0.03956 0.03175 0.02312 0.00225 -0.01355 -0.01515 0.03148 0.00755 0.00082 0.00020 0.00015 0.00000 0.00347 0.00335 0.00284 0.00257 0.00247 0.00271 0.00128 H3 0.26555 0.38705 0.11244 1.00000 0.03777 0.00000 0.00000 C4 0.38537 0.46544 0.10264 1.00000 0.03141 0.02990 0.02056 0.00487 -0.00589 0.00242 0.02729 0.00791 0.00078 0.00019 0.00014 0.00000 0.00326 0.00326 0.00274 0.00242 0.00231 0.00250 0.00119 H4 0.26744 0.48839 0.11069 1.00000 0.03275 0.00000 0.00000 C5 0.59332 0.48179 0.08735 1.00000 0.04871 0.02387 0.02248 0.00289 -0.00422 -0.00540 0.03169 0.00820 0.00084 0.00020 0.00015 0.00000 0.00372 0.00322 0.00288 0.00241 0.00253 0.00278 0.00130 H5 0.63910 0.51792 0.08291 1.00000 0.03802 0.00000 0.00000 C6 0.54924 0.45955 0.20399 1.00000 0.03003 0.02447 0.02177 -0.00202 -0.00472 0.00643 0.02542 0.00762 0.00076 0.00018 0.00014 0.00000 0.00309 0.00311 0.00271 0.00236 0.00221 0.00243 0.00117 H6 0.41327 0.47426 0.21336 1.00000 0.03051 0.00000 0.00000 C7 0.73235 0.48919 0.18968 1.00000 0.03823 0.01779 0.03106 -0.00083 -0.00902 -0.00664 0.02903 0.00768 0.00081 0.00019 0.00015 0.00000 0.00329 0.00281 0.00306 0.00247 0.00244 0.00265 0.00124 H7 0.74131 0.52728 0.18769 1.00000 0.03483 0.00000 0.00000 C8 0.89969 0.45259 0.17883 1.00000 0.02152 0.04489 0.02188 0.00488 -0.00568 -0.00519 0.02943 0.00788 0.00076 0.00020 0.00015 0.00000 0.00302 0.00362 0.00278 0.00252 0.00220 0.00258 0.00126 H8 1.04139 0.46164 0.16821 1.00000 0.03532 0.00000 0.00000 C9 0.82080 0.40022 0.18645 1.00000 0.02420 0.02402 0.02088 0.00154 -0.00228 0.00628 0.02303 0.00761 0.00071 0.00019 0.00014 0.00000 0.00317 0.00305 0.00270 0.00234 0.00212 0.00225 0.00117 H9 0.90040 0.36782 0.18193 1.00000 0.02764 0.00000 0.00000 C10 0.60200 0.40406 0.20206 1.00000 0.02501 0.01711 0.01484 -0.00124 -0.00610 0.00380 0.01899 0.00722 0.00072 0.00017 0.00013 0.00000 0.00297 0.00289 0.00246 0.00213 0.00208 0.00222 0.00109 C11 0.45391 0.35814 0.21506 1.00000 0.03384 0.02177 0.01658 -0.00413 0.00127 0.00462 0.02406 0.00763 0.00073 0.00017 0.00014 0.00000 0.00305 0.00297 0.00262 0.00223 0.00212 0.00231 0.00118 H11A 0.46803 0.35165 0.24632 1.00000 0.02888 0.00000 0.00000 H11B 0.29902 0.36769 0.20893 1.00000 0.02888 0.00000 0.00000 C12 0.56529 0.26291 0.21079 1.00000 0.01549 0.02349 0.02619 0.00323 0.00201 -0.00447 0.02172 0.00784 0.00067 0.00020 0.00016 0.00000 0.00275 0.00318 0.00310 0.00242 0.00208 0.00216 0.00114 C13 0.63396 0.21984 0.18112 1.00000 0.02132 0.01158 0.02716 0.00601 0.00071 -0.00002 0.02002 0.00796 0.00072 0.00017 0.00015 0.00000 0.00276 0.00262 0.00280 0.00226 0.00229 0.00225 0.00107 C14 0.57500 0.20453 0.13941 1.00000 0.02754 0.01301 0.02461 0.00341 0.00423 -0.00280 0.02172 0.00766 0.00071 0.00017 0.00015 0.00000 0.00291 0.00265 0.00288 0.00225 0.00221 0.00217 0.00113 C15 0.72049 0.16122 0.12733 1.00000 0.02580 0.01565 0.02569 -0.00232 0.00663 -0.00461 0.02238 0.00774 0.00072 0.00018 0.00015 0.00000 0.00290 0.00287 0.00281 0.00230 0.00228 0.00223 0.00115 C16 0.86118 0.15348 0.16154 1.00000 0.02443 0.02033 0.02457 -0.00863 0.00570 -0.00415 0.02311 0.00778 0.00074 0.00018 0.00015 0.00000 0.00293 0.00286 0.00272 0.00238 0.00232 0.00233 0.00113 C17 0.40419 0.23002 0.11220 1.00000 0.02707 0.01457 0.02151 -0.00119 0.00148 -0.00285 0.02105 0.00735 0.00074 0.00017 0.00014 0.00000 0.00313 0.00271 0.00279 0.00219 0.00222 0.00220 0.00113 C18 0.20579 0.24767 0.12929 1.00000 0.03010 0.01855 0.03411 -0.00169 -0.00246 -0.00573 0.02759 0.00753 0.00075 0.00018 0.00016 0.00000 0.00333 0.00285 0.00305 0.00243 0.00249 0.00236 0.00123 H18 0.17346 0.24097 0.15867 1.00000 0.03310 0.00000 0.00000 C19 0.05296 0.27516 0.10386 1.00000 0.02531 0.02491 0.03755 -0.00372 0.00038 -0.00453 0.02926 0.00776 0.00079 0.00018 0.00016 0.00000 0.00310 0.00311 0.00336 0.00261 0.00241 0.00233 0.00125 H19 -0.08214 0.28690 0.11598 1.00000 0.03511 0.00000 0.00000 C20 0.09837 0.28521 0.06121 1.00000 0.03660 0.02352 0.04324 -0.00385 -0.01363 0.00579 0.03445 0.00802 0.00082 0.00019 0.00017 0.00000 0.00351 0.00320 0.00371 0.00266 0.00275 0.00244 0.00135 H20 -0.00531 0.30396 0.04397 1.00000 0.04134 0.00000 0.00000 C21 0.29530 0.26798 0.04345 1.00000 0.04938 0.02062 0.02511 -0.00246 -0.00542 -0.00061 0.03170 0.00780 0.00083 0.00018 0.00016 0.00000 0.00373 0.00303 0.00296 0.00250 0.00264 0.00257 0.00130 H21 0.32651 0.27475 0.01404 1.00000 0.03804 0.00000 0.00000 C22 0.44585 0.24094 0.06868 1.00000 0.02909 0.02323 0.03439 0.00204 0.00053 0.00207 0.02891 0.00787 0.00076 0.00018 0.00016 0.00000 0.00307 0.00310 0.00322 0.00252 0.00242 0.00234 0.00125 H22 0.58073 0.22945 0.05632 1.00000 0.03469 0.00000 0.00000 C23 0.71702 0.13225 0.08555 1.00000 0.02590 0.01547 0.02522 0.00341 0.00041 -0.00195 0.02220 0.00786 0.00076 0.00017 0.00015 0.00000 0.00308 0.00283 0.00283 0.00225 0.00231 0.00225 0.00116 C24 0.89897 0.13399 0.05838 1.00000 0.02716 0.02445 0.02845 0.00588 -0.00124 -0.00081 0.02669 0.00830 0.00075 0.00018 0.00015 0.00000 0.00312 0.00315 0.00306 0.00237 0.00234 0.00225 0.00123 H24 1.02658 0.15345 0.06666 1.00000 0.03203 0.00000 0.00000 C25 0.89381 0.10742 0.01941 1.00000 0.03964 0.03176 0.02594 0.00355 0.00683 0.01284 0.03245 0.00938 0.00084 0.00020 0.00016 0.00000 0.00334 0.00331 0.00298 0.00254 0.00251 0.00271 0.00129 H25 1.01788 0.10909 0.00091 1.00000 0.03894 0.00000 0.00000 C26 0.71174 0.07863 0.00703 1.00000 0.04555 0.03058 0.02172 -0.00137 -0.00640 0.00687 0.03262 0.00904 0.00088 0.00019 0.00016 0.00000 0.00359 0.00337 0.00282 0.00245 0.00272 0.00271 0.00132 H26 0.71089 0.06000 -0.01963 1.00000 0.03914 0.00000 0.00000 C27 0.52873 0.07691 0.03375 1.00000 0.03067 0.03229 0.03384 -0.00586 -0.01465 0.00290 0.03226 0.00817 0.00081 0.00019 0.00016 0.00000 0.00318 0.00341 0.00334 0.00265 0.00269 0.00243 0.00132 H27 0.40160 0.05740 0.02528 1.00000 0.03872 0.00000 0.00000 C28 0.53215 0.10360 0.07260 1.00000 0.02871 0.02811 0.02518 0.00035 -0.00091 0.00040 0.02733 0.00812 0.00076 0.00018 0.00015 0.00000 0.00305 0.00320 0.00292 0.00245 0.00231 0.00243 0.00121 H28 0.40662 0.10239 0.09075 1.00000 0.03280 0.00000 0.00000 C29 1.05117 0.11776 0.16562 1.00000 0.02689 0.02031 0.02215 0.00218 0.00486 -0.00557 0.02312 0.00830 0.00073 0.00019 0.00015 0.00000 0.00318 0.00308 0.00294 0.00244 0.00230 0.00240 0.00117 C30 1.35197 0.09409 0.20916 1.00000 0.02547 0.03100 0.03562 -0.00241 -0.00475 0.01007 0.03070 0.00813 0.00071 0.00019 0.00015 0.00000 0.00307 0.00318 0.00312 0.00257 0.00233 0.00239 0.00126 H30A 1.30849 0.05618 0.21099 1.00000 0.04604 0.00000 0.00000 H30B 1.42586 0.10471 0.23583 1.00000 0.04604 0.00000 0.00000 H30C 1.45254 0.09902 0.18487 1.00000 0.04604 0.00000 0.00000 N1 0.51217 0.30951 0.19169 1.00000 0.03637 0.02034 0.01878 0.00000 0.00185 -0.00327 0.02516 0.00697 0.00066 0.00016 0.00014 0.00000 0.00267 0.00277 0.00258 0.00210 0.00205 0.00191 0.00104 N2 0.80362 0.18812 0.19349 1.00000 0.02691 0.02103 0.01974 -0.00364 -0.00057 -0.00237 0.02256 0.00732 0.00065 0.00015 0.00013 0.00000 0.00270 0.00254 0.00234 0.00205 0.00199 0.00207 0.00101 O1 0.56577 0.25614 0.25007 1.00000 0.02931 0.02537 0.02063 0.00109 0.00167 0.00183 0.02510 0.00500 0.00044 0.00012 0.00010 0.00000 0.00196 0.00197 0.00205 0.00153 0.00140 0.00145 0.00080 O2 1.10663 0.08437 0.13975 1.00000 0.03214 0.02957 0.02935 -0.00575 -0.00045 0.00364 0.03035 0.00536 0.00048 0.00013 0.00010 0.00000 0.00206 0.00207 0.00206 0.00172 0.00160 0.00154 0.00083 O3 1.15920 0.12699 0.20296 1.00000 0.03007 0.02941 0.02589 -0.00336 -0.00578 0.00458 0.02845 0.00514 0.00047 0.00012 0.00010 0.00000 0.00209 0.00208 0.00199 0.00161 0.00153 0.00155 0.00083 Fe1 0.62689 0.43820 0.14267 1.00000 0.02917 0.02358 0.02124 0.00053 -0.00339 -0.00097 0.02467 0.00110 0.00010 0.00003 0.00002 0.00000 0.00046 0.00046 0.00041 0.00034 0.00031 0.00032 0.00025 H1N 0.51508 0.31131 0.16552 1.00000 0.03763 0.08416 0.00779 0.00188 0.00164 0.00000 0.01666 H2N 0.88467 0.19650 0.21419 1.00000 0.00475 0.06651 0.00595 0.00146 0.00126 0.00000 0.01171 Final Structure Factor Calculation for 02SOT064 in Pbca Total number of l.s. parameters = 335 Maximum vector length = 511 Memory required = 3883 / 24017 wR2 = 0.1243 before cycle 5 for 3464 data and 0 / 335 parameters GooF = S = 0.986; Restrained GooF = 0.986 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0400 * P )^2 + 4.99 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0573 for 2134 Fo > 4sig(Fo) and 0.1185 for all 3464 data wR2 = 0.1243, GooF = S = 0.986, Restrained GooF = 0.986 for all data Occupancy sum of asymmetric unit = 36.00 for non-hydrogen and 26.00 for hydrogen atoms Principal mean square atomic displacements U 0.0588 0.0334 0.0210 C1 0.0763 0.0232 0.0172 C2 0.0559 0.0254 0.0131 C3 0.0340 0.0320 0.0159 C4 0.0506 0.0242 0.0202 C5 0.0361 0.0210 0.0192 C6 0.0453 0.0268 0.0150 C7 0.0474 0.0249 0.0160 C8 0.0304 0.0224 0.0162 C9 0.0292 0.0159 0.0119 C10 0.0354 0.0231 0.0137 C11 0.0284 0.0240 0.0127 C12 0.0293 0.0213 0.0095 C13 0.0306 0.0235 0.0112 C14 0.0337 0.0196 0.0139 C15 0.0357 0.0200 0.0136 C16 0.0281 0.0212 0.0139 C17 0.0354 0.0316 0.0158 C18 0.0388 0.0288 0.0202 C19 0.0553 0.0268 0.0212 C20 0.0505 0.0253 0.0193 C21 0.0349 0.0295 0.0223 C22 0.0265 0.0261 0.0141 C23 0.0330 0.0268 0.0202 C24 0.0514 0.0243 0.0216 C25 0.0497 0.0280 0.0201 C26 0.0493 0.0302 0.0173 C27 0.0290 0.0281 0.0249 C28 0.0313 0.0235 0.0145 C29 0.0423 0.0323 0.0175 C30 0.0372 0.0198 0.0185 N1 0.0278 0.0235 0.0163 N2 0.0304 0.0247 0.0202 O1 0.0371 0.0309 0.0231 O2 0.0379 0.0256 0.0218 O3 0.0306 0.0234 0.0200 Fe1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.009 0.017 0.026 0.036 0.047 0.058 0.074 0.097 0.141 1.000 Number in group 382. 327. 335. 341. 377. 321. 343. 347. 346. 345. GooF 0.856 0.923 0.934 0.967 1.006 1.036 1.117 1.055 0.964 0.991 K 0.893 1.547 0.998 1.015 1.000 1.029 0.997 0.992 1.014 1.021 Resolution(A) 0.81 0.86 0.91 0.96 1.02 1.10 1.19 1.32 1.51 1.89 inf Number in group 352. 346. 349. 342. 349. 343. 343. 353. 339. 348. GooF 0.927 0.913 0.948 1.053 1.017 0.966 0.959 0.926 1.103 1.038 K 1.073 1.092 1.045 1.010 1.021 1.000 1.025 1.016 1.023 1.004 R1 0.378 0.296 0.223 0.179 0.150 0.110 0.089 0.060 0.043 0.030 Recommended weighting scheme: WGHT 0.0420 3.1206 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 8 10 442.18 124.86 4.66 0.022 1.78 3 0 6 925.71 592.09 3.69 0.048 1.89 6 9 19 -640.36 843.74 3.68 0.057 0.82 2 1 17 2278.47 2980.39 3.65 0.108 1.57 3 2 4 2101.95 1652.95 3.65 0.080 1.94 6 1 11 0.00 978.81 3.58 0.062 0.95 4 16 4 1877.62 903.35 3.43 0.059 1.08 0 12 28 -140.91 319.17 3.39 0.035 0.98 2 0 30 0.00 467.62 3.37 0.043 0.98 1 4 5 1790.35 1412.90 3.36 0.074 3.56 3 6 6 1664.12 1268.41 3.34 0.070 1.72 4 4 25 853.92 1787.06 3.28 0.084 0.95 1 11 2 1185.70 1525.22 3.24 0.077 2.10 5 17 8 139.54 580.58 3.18 0.048 0.91 2 7 5 1453.03 1824.91 3.16 0.085 2.17 2 1 23 652.77 1135.02 3.15 0.067 1.23 0 2 16 22268.53 18441.32 3.13 0.269 1.92 2 8 6 6417.85 5511.31 3.07 0.147 2.00 0 12 1 5706.28 6709.80 3.06 0.162 2.07 1 20 16 425.49 11.08 3.05 0.007 1.03 3 14 15 704.65 1162.77 3.00 0.067 1.12 2 2 12 3773.07 3166.58 3.00 0.111 1.95 2 7 9 1003.52 1295.16 2.99 0.071 1.92 3 4 26 682.00 1093.74 2.93 0.065 1.02 5 7 9 0.00 400.33 2.90 0.040 1.09 2 10 3 355.57 203.09 2.87 0.028 1.89 0 2 17 991.33 665.00 2.86 0.051 1.81 3 5 6 188.78 377.34 2.83 0.038 1.77 1 21 22 1995.97 1287.86 2.81 0.071 0.90 1 22 1 2480.89 3246.70 2.78 0.113 1.11 1 8 7 249.26 52.85 2.78 0.014 2.35 1 5 22 2126.42 2730.37 2.73 0.103 1.33 4 2 18 3224.58 4111.29 2.72 0.127 1.14 3 2 24 91.41 422.83 2.72 0.041 1.09 0 16 8 570.62 883.66 2.72 0.059 1.44 0 12 8 20954.73 18209.81 2.72 0.267 1.83 2 13 8 402.90 633.02 2.70 0.050 1.49 5 7 14 518.51 919.02 2.69 0.060 1.02 4 5 17 1153.62 1541.71 2.68 0.078 1.14 0 8 22 16365.79 13881.06 2.68 0.233 1.29 2 22 8 0.00 368.01 2.67 0.038 1.02 1 19 15 849.74 1264.09 2.65 0.070 1.09 4 18 17 708.68 1.63 2.64 0.003 0.89 1 24 22 2159.45 1065.47 2.63 0.065 0.83 4 20 4 426.87 71.01 2.60 0.017 0.95 4 4 26 855.13 154.14 2.59 0.025 0.93 5 10 13 354.11 99.45 2.59 0.020 0.99 1 12 21 1372.10 769.14 2.59 0.055 1.18 2 14 22 142.30 500.14 2.55 0.044 1.04 3 21 22 801.34 334.43 2.55 0.036 0.83 Bond lengths and angles C1 - Distance Angles C5 1.3969 (0.0066) C2 1.4006 (0.0068) 108.04 (0.47) Fe1 2.0381 (0.0050) 70.23 (0.29) 69.82 (0.29) H1 0.9500 125.98 125.98 125.55 C1 - C5 C2 Fe1 C2 - Distance Angles C1 1.4006 (0.0068) C3 1.4124 (0.0065) 107.75 (0.46) Fe1 2.0363 (0.0048) 69.96 (0.29) 69.76 (0.27) H2 0.9500 126.13 126.13 125.73 C2 - C1 C3 Fe1 C3 - Distance Angles C4 1.3998 (0.0061) C2 1.4124 (0.0066) 108.34 (0.43) Fe1 2.0375 (0.0044) 70.08 (0.25) 69.67 (0.26) H3 0.9500 125.83 125.83 126.00 C3 - C4 C2 Fe1 C4 - Distance Angles C3 1.3998 (0.0061) C5 1.4110 (0.0060) 107.30 (0.43) Fe1 2.0414 (0.0045) 69.78 (0.26) 69.91 (0.26) H4 0.9500 126.35 126.35 125.55 C4 - C3 C5 Fe1 C5 - Distance Angles C1 1.3969 (0.0067) C4 1.4110 (0.0060) 108.56 (0.45) Fe1 2.0443 (0.0047) 69.75 (0.28) 69.69 (0.27) H5 0.9500 125.72 125.72 126.42 C5 - C1 C4 Fe1 C6 - Distance Angles C7 1.4075 (0.0062) C10 1.4172 (0.0058) 108.46 (0.41) Fe1 2.0361 (0.0045) 69.90 (0.27) 69.77 (0.25) H6 0.9500 125.77 125.77 126.15 C6 - C7 C10 Fe1 C7 - Distance Angles C6 1.4075 (0.0062) C8 1.4060 (0.0062) 108.07 (0.41) Fe1 2.0389 (0.0045) 69.69 (0.25) 69.72 (0.27) H7 0.9500 125.97 125.97 126.19 C7 - C6 C8 Fe1 C8 - Distance Angles C9 1.4071 (0.0061) C7 1.4060 (0.0062) 108.12 (0.41) Fe1 2.0364 (0.0044) 69.69 (0.25) 69.91 (0.26) H8 0.9500 125.94 125.94 126.04 C8 - C9 C7 Fe1 C9 - Distance Angles C8 1.4071 (0.0061) C10 1.4197 (0.0057) 108.37 (0.40) Fe1 2.0342 (0.0043) 69.86 (0.26) 69.79 (0.24) H9 0.9500 125.82 125.82 126.11 C9 - C8 C10 Fe1 C10 - Distance Angles C6 1.4172 (0.0058) C9 1.4197 (0.0057) 106.98 (0.39) C11 1.5089 (0.0059) 126.11 (0.40) 126.90 (0.39) Fe1 2.0392 (0.0043) 69.53 (0.25) 69.41 (0.25) 127.01 (0.30) C10 - C6 C9 C11 C11 - Distance Angles N1 1.4542 (0.0055) C10 1.5089 (0.0059) 110.43 (0.36) H11A 0.9900 109.57 109.57 H11B 0.9900 109.57 109.57 108.11 C11 - N1 C10 H11A C12 - Distance Angles O1 1.2340 (0.0052) N1 1.3410 (0.0058) 123.87 (0.47) C13 1.4741 (0.0062) 121.40 (0.45) 114.68 (0.42) C12 - O1 N1 C13 - Distance Angles N2 1.3543 (0.0055) C14 1.3993 (0.0061) 107.50 (0.41) C12 1.4741 (0.0062) 117.42 (0.41) 134.90 (0.44) C13 - N2 C14 C14 - Distance Angles C13 1.3993 (0.0061) C15 1.4432 (0.0059) 106.69 (0.40) C17 1.4822 (0.0059) 126.39 (0.41) 126.85 (0.41) C14 - C13 C15 C15 - Distance Angles C16 1.3792 (0.0062) C14 1.4432 (0.0058) 106.46 (0.40) C23 1.4864 (0.0060) 128.06 (0.40) 125.47 (0.41) C15 - C16 C14 C16 - Distance Angles N2 1.3607 (0.0055) C15 1.3792 (0.0062) 108.43 (0.40) C29 1.4626 (0.0063) 121.58 (0.43) 129.91 (0.42) C16 - N2 C15 C17 - Distance Angles C18 1.3896 (0.0060) C22 1.4043 (0.0064) 117.69 (0.43) C14 1.4822 (0.0059) 121.66 (0.40) 120.46 (0.41) C17 - C18 C22 C18 - Distance Angles C17 1.3896 (0.0060) C19 1.3988 (0.0063) 120.97 (0.47) H18 0.9500 119.51 119.51 C18 - C17 C19 C19 - Distance Angles C20 1.3785 (0.0067) C18 1.3988 (0.0063) 120.01 (0.48) H19 0.9500 120.00 120.00 C19 - C20 C18 C20 - Distance Angles C19 1.3785 (0.0067) C21 1.3868 (0.0063) 120.04 (0.47) H20 0.9500 119.98 119.98 C20 - C19 C21 C21 - Distance Angles C22 1.3806 (0.0062) C20 1.3868 (0.0063) 119.77 (0.48) H21 0.9500 120.12 120.12 C21 - C22 C20 C22 - Distance Angles C21 1.3806 (0.0062) C17 1.4043 (0.0064) 121.52 (0.46) H22 0.9500 119.24 119.24 C22 - C21 C17 C23 - Distance Angles C28 1.3905 (0.0060) C24 1.3933 (0.0060) 118.83 (0.45) C15 1.4864 (0.0060) 120.86 (0.41) 120.30 (0.40) C23 - C28 C24 C24 - Distance Angles C25 1.3813 (0.0062) C23 1.3933 (0.0060) 120.00 (0.45) H24 0.9500 120.00 120.00 C24 - C25 C23 C25 - Distance Angles C26 1.3735 (0.0064) C24 1.3813 (0.0062) 120.91 (0.47) H25 0.9500 119.55 119.55 C25 - C26 C24 C26 - Distance Angles C25 1.3735 (0.0064) C27 1.3901 (0.0065) 119.58 (0.46) H26 0.9500 120.21 120.21 C26 - C25 C27 C27 - Distance Angles C28 1.3791 (0.0062) C26 1.3901 (0.0065) 119.84 (0.44) H27 0.9500 120.08 120.08 C27 - C28 C26 C28 - Distance Angles C27 1.3791 (0.0062) C23 1.3905 (0.0060) 120.83 (0.45) H28 0.9500 119.59 119.59 C28 - C27 C23 C29 - Distance Angles O2 1.2042 (0.0049) O3 1.3546 (0.0053) 123.67 (0.43) C16 1.4626 (0.0063) 125.55 (0.43) 110.78 (0.41) C29 - O2 O3 C30 - Distance Angles O3 1.4423 (0.0049) H30A 0.9800 109.47 H30B 0.9800 109.47 109.47 H30C 0.9800 109.47 109.47 109.47 C30 - O3 H30A H30B N1 - Distance Angles C12 1.3410 (0.0058) C11 1.4542 (0.0055) 123.69 (0.42) H1N 0.8159 (0.0491) 118.99 (3.48) 117.30 (3.48) N1 - C12 C11 N2 - Distance Angles C13 1.3543 (0.0054) C16 1.3607 (0.0055) 110.88 (0.42) H2N 0.8374 (0.0374) 121.48 (2.61) 124.61 (2.64) N2 - C13 C16 O1 - Distance Angles C12 1.2340 (0.0052) O1 - O2 - Distance Angles C29 1.2042 (0.0050) O2 - O3 - Distance Angles C29 1.3546 (0.0053) C30 1.4423 (0.0049) 114.39 (0.36) O3 - C29 Fe1 - Distance Angles C9 2.0342 (0.0044) C6 2.0361 (0.0045) 68.14 (0.18) C2 2.0363 (0.0048) 109.39 (0.19) 152.29 (0.22) C8 2.0364 (0.0045) 40.45 (0.17) 67.99 (0.18) 129.17 (0.21) C3 2.0375 (0.0044) 130.70 (0.19) 118.82 (0.20) 40.57 (0.19) 168.18 (0.21) C10 2.0392 (0.0043) 40.80 (0.16) 40.70 (0.17) 118.98 (0.20) 68.45 (0.18) 109.73 (0.18) C1 2.0381 (0.0050) 117.91 (0.20) 166.27 (0.22) 40.21 (0.20) 107.90 (0.20) 67.77 (0.20) 151.54 (0.21) C7 2.0389 (0.0045) 68.00 (0.19) 40.41 (0.17) 166.48 (0.22) 40.36 (0.18) 150.91 (0.21) 68.39 (0.18) 128.14 (0.21) C5 2.0443 (0.0047) 150.21 (0.19) 128.90 (0.19) 67.39 (0.21) 116.98 (0.19) 67.37 (0.19) 167.50 (0.20) 40.02 (0.19) C4 2.0414 (0.0045) 168.44 (0.19) 108.58 (0.19) 67.99 (0.19) 149.90 (0.19) 40.14 (0.17) 129.61 (0.18) 67.95 (0.20) Fe1 - C9 C6 C2 C8 C3 C10 C1 FMAP and GRID set by program FMAP 2 3 34 GRID -0.806 -2 -1 0.806 2 1 R1 = 0.1164 for 3464 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.52 at 0.8633 0.4336 0.1443 [ 1.19 A from C8 ] Deepest hole -0.47 at 0.6302 0.4667 0.1432 [ 0.71 A from FE1 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 3700 / 29353 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.8633 0.4336 0.1443 1.00000 0.05 0.52 1.19 C8 1.44 FE1 1.49 H8 1.57 C9 Q2 1 0.6409 0.0597 0.0725 1.00000 0.05 0.37 1.28 C28 1.45 C27 1.72 H5 1.86 H28 Q3 1 1.2663 0.0392 0.1465 1.00000 0.05 0.32 1.50 O2 1.70 H4 2.07 H30A 2.22 H30C Q4 1 0.5626 0.4333 0.1858 1.00000 0.05 0.32 0.87 C6 0.92 C10 1.40 FE1 1.61 H6 Q5 1 0.6055 0.5466 0.1063 1.00000 0.05 0.31 1.04 H5 1.72 C5 1.91 O2 2.42 C4 Q6 1 0.6960 0.4763 0.1593 1.00000 0.05 0.30 1.02 C7 1.16 FE1 1.50 C8 1.57 H7 Q7 1 0.5823 0.3818 0.1412 1.00000 0.05 0.29 1.43 FE1 1.62 C2 1.81 C3 1.84 H2 Q8 1 0.2805 0.4025 0.0994 1.00000 0.05 0.29 0.56 H3 0.67 C3 1.69 C4 1.95 C2 Q9 1 0.3043 0.2391 0.0586 1.00000 0.05 0.28 0.86 C21 0.92 C22 1.65 H21 1.70 C20 Q10 1 0.6432 0.1878 0.1920 1.00000 0.05 0.28 0.87 C13 0.98 N2 1.64 H2N 1.74 C14 Shortest distances between peaks (including symmetry equivalents) 1 6 1.54 4 6 1.58 4 7 1.89 2 5 1.89 1 7 2.14 1 4 2.24 7 8 2.31 5 6 2.47 6 7 2.51 3 5 2.59 1 8 3.00 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. 0.27: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.06: Set up l.s. refinement 0.00: Generate idealized H-atoms 2.41: Structure factors and derivatives 2.23: 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 0.00: Other dependent quantities, CIF, tables 0.22: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.11: Fourier summations 0.11: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 10:47:05 Total elapsed time: 5.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++