+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 11:10:00 on 09-Oct-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 02src649 in P2(1)/c CELL 0.71073 13.0933 10.3440 15.4112 90.000 111.319 90.000 ZERR 4.00 0.0005 0.0004 0.0007 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O FE UNIT 104 80 8 8 4 V = 1944.42 F(000) = 928.0 Mu = 0.80 mm-1 Cell Wt = 1793.16 Rho = 1.531 MERG 2 OMIT -3.00 55.00 OMIT 1 5 0 OMIT -3 5 2 OMIT -6 2 4 FMAP 2 PLAN 10 SIZE 0.12 0.28 0.50 ACTA BOND $H WGHT 0.04520 0.55840 L.S. 10 TEMP -153.00 FVAR 0.37842 MOLE 1 C1 1 0.521877 0.724680 0.309582 11.00000 0.01344 0.02495 = 0.01529 0.00110 0.00385 0.00085 C2 1 0.440239 0.635410 0.316224 11.00000 0.01728 0.02197 = 0.02068 0.00216 0.00679 -0.00037 AFIX 43 H2 2 0.442439 0.543899 0.311989 11.00000 -1.20000 AFIX 0 C3 1 0.356371 0.708938 0.330185 11.00000 0.01711 0.03340 = 0.02001 0.00412 0.00860 -0.00050 AFIX 43 H3 2 0.292948 0.674701 0.338020 11.00000 -1.20000 AFIX 0 C4 1 0.382473 0.842313 0.330576 11.00000 0.02171 0.02903 = 0.01652 -0.00263 0.00652 0.00435 AFIX 43 H4 2 0.339572 0.912366 0.338209 11.00000 -1.20000 AFIX 0 C5 1 0.483540 0.852197 0.317597 11.00000 0.01805 0.02128 = 0.01660 -0.00128 0.00490 -0.00101 AFIX 43 H5 2 0.520078 0.930489 0.314664 11.00000 -1.20000 AFIX 0 C6 1 0.620766 0.687976 0.294699 11.00000 0.01565 0.02137 = 0.01436 0.00138 0.00371 0.00245 AFIX 43 H6 2 0.627363 0.599809 0.280284 11.00000 -1.20000 AFIX 0 C7 1 0.703780 0.766167 0.299272 11.00000 0.01554 0.02092 = 0.02005 0.00008 0.00616 0.00101 AFIX 43 H7 2 0.698774 0.856133 0.309467 11.00000 -1.20000 AFIX 0 C8 1 0.802548 0.713690 0.288620 11.00000 0.01800 0.02313 = 0.01666 0.00224 0.00667 0.00003 C9 1 0.901781 0.798025 0.311540 11.00000 0.01723 0.02087 = 0.01642 0.00409 0.00584 0.00125 C10 1 0.999250 0.973851 0.387494 11.00000 0.02534 0.02426 = 0.02519 -0.00143 0.01129 -0.00540 AFIX 43 H10 2 1.005044 1.047790 0.425560 11.00000 -1.20000 AFIX 0 C11 1 1.086468 0.945728 0.360066 11.00000 0.01813 0.02757 = 0.02553 0.00445 0.00586 -0.00558 AFIX 43 H11 2 1.150313 0.998326 0.379313 11.00000 -1.20000 AFIX 0 C12 1 1.078039 0.839251 0.304041 11.00000 0.01721 0.02921 = 0.03042 0.00414 0.01247 0.00156 AFIX 43 H12 2 1.135069 0.819040 0.281926 11.00000 -1.20000 AFIX 0 C13 1 0.985371 0.762072 0.280382 11.00000 0.01732 0.02279 = 0.02165 0.00057 0.00800 0.00169 AFIX 43 H13 2 0.978882 0.686430 0.243797 11.00000 -1.20000 AFIX 0 C14 1 0.380052 0.737062 0.075433 11.00000 0.01604 0.02468 = 0.01482 -0.00137 0.00251 -0.00177 C15 1 0.299120 0.650928 0.086456 11.00000 0.01881 0.02253 = 0.02140 -0.00338 0.00389 -0.00175 AFIX 43 H15 2 0.298959 0.559371 0.081565 11.00000 -1.20000 AFIX 0 C16 1 0.219742 0.726772 0.105886 11.00000 0.01238 0.03274 = 0.02380 -0.00249 0.00387 -0.00343 AFIX 43 H16 2 0.157241 0.694614 0.116363 11.00000 -1.20000 AFIX 0 C17 1 0.249613 0.859230 0.107026 11.00000 0.01651 0.02726 = 0.02209 -0.00145 0.00303 0.00457 AFIX 43 H17 2 0.210347 0.930755 0.117905 11.00000 -1.20000 AFIX 0 C18 1 0.348023 0.865630 0.089115 11.00000 0.02063 0.02261 = 0.01624 0.00206 0.00297 0.00113 AFIX 43 H18 2 0.386550 0.942492 0.086572 11.00000 -1.20000 AFIX 0 C19 1 0.478209 0.695188 0.060992 11.00000 0.01945 0.02319 = 0.01377 -0.00196 0.00429 0.00182 AFIX 43 H19 2 0.484281 0.605496 0.050514 11.00000 -1.20000 AFIX 0 C20 1 0.561296 0.770818 0.060989 11.00000 0.01886 0.02324 = 0.01688 -0.00283 0.00537 0.00119 AFIX 43 H20 2 0.558099 0.861300 0.070256 11.00000 -1.20000 AFIX 0 C21 1 0.656986 0.715373 0.046842 11.00000 0.01879 0.02622 = 0.01453 0.00020 0.00496 0.00212 C22 1 0.753289 0.802290 0.057906 11.00000 0.01830 0.02340 = 0.01549 0.00285 0.00561 0.00230 C23 1 0.846068 0.989573 0.113290 11.00000 0.02308 0.02339 = 0.03288 -0.00280 0.01001 -0.00048 AFIX 43 H23 2 0.850828 1.070350 0.143849 11.00000 -1.20000 AFIX 0 C24 1 0.931252 0.954958 0.084922 11.00000 0.01861 0.02974 = 0.02894 0.00586 0.00743 -0.00108 AFIX 43 H24 2 0.992909 1.009976 0.096555 11.00000 -1.20000 AFIX 0 C25 1 0.924392 0.838724 0.039395 11.00000 0.02132 0.03359 = 0.02197 0.00608 0.01084 0.00494 AFIX 43 H25 2 0.980646 0.812911 0.017817 11.00000 -1.20000 AFIX 0 C26 1 0.834080 0.760087 0.025598 11.00000 0.02145 0.02747 = 0.01706 0.00101 0.00715 0.00303 AFIX 43 H26 2 0.827444 0.679225 -0.005202 11.00000 -1.20000 AFIX 0 N1 3 0.907262 0.903483 0.363788 11.00000 0.02024 0.02488 = 0.02321 -0.00009 0.01069 -0.00381 N2 3 0.757442 0.916340 0.100347 11.00000 0.01959 0.02400 = 0.02574 -0.00044 0.00863 0.00126 O1 4 0.807751 0.601624 0.263534 11.00000 0.02260 0.02215 = 0.03588 -0.00549 0.01465 -0.00247 O2 4 0.662260 0.601310 0.026847 11.00000 0.02355 0.02319 = 0.03029 -0.00441 0.01090 0.00095 FE1 5 0.371045 0.758166 0.206130 11.00000 0.01254 0.02006 = 0.01676 -0.00026 0.00498 0.00011 HKLF 4 Covalent radii and connectivity table for 02src649 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 FE 1.240 C1 - C5 C2 C6 Fe1 C2 - C3 C1 Fe1 C3 - C2 C4 Fe1 C4 - C5 C3 Fe1 C5 - C4 C1 Fe1 C6 - C7 C1 C7 - C6 C8 C8 - O1 C7 C9 C9 - N1 C13 C8 C10 - N1 C11 C11 - C12 C10 C12 - C11 C13 C13 - C12 C9 C14 - C18 C15 C19 Fe1 C15 - C16 C14 Fe1 C16 - C15 C17 Fe1 C17 - C18 C16 Fe1 C18 - C17 C14 Fe1 C19 - C20 C14 C20 - C19 C21 C21 - O2 C20 C22 C22 - N2 C26 C21 C23 - N2 C24 C24 - C25 C23 C25 - C24 C26 C26 - C25 C22 N1 - C10 C9 N2 - C23 C22 O1 - C8 O2 - C21 Fe1 - C18 C17 C16 C2 C3 C5 C4 C15 C1 C14 h k l Fo^2 Sigma Why rejected 6 0 3 4.96 1.24 observed but should be systematically absent 16561 Reflections read, of which 504 rejected -14 =< h =< 17, -13 =< k =< 13, -20 =< l =< 18, Max. 2-theta = 54.97 1 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 1 2 4 1905.65 25.94 6 190.78 -1 2 6 281.17 4.13 5 39.11 2 3 7 301.04 5.25 6 27.33 -1 2 8 286.02 3.47 5 58.09 2 3 9 36.91 0.94 6 5.03 -3 3 12 109.16 2.25 5 21.23 -4 3 14 40.97 1.19 4 12.96 -6 4 15 65.46 1.26 3 31.55 8 Inconsistent equivalents 4424 Unique reflections, of which 0 suppressed R(int) = 0.0534 R(sigma) = 0.0461 Friedel opposites merged Maximum memory for data reduction = 2795 / 44363 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 = 3558 / 350077 wR2 = 0.0922 before cycle 1 for 4424 data and 280 / 280 parameters GooF = S = 1.029; Restrained GooF = 1.029 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0452 * P )^2 + 0.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.37916 0.00059 1.273 OSF Mean shift/su = 0.154 Maximum = 1.273 for OSF Max. shift = 0.002 A for C22 Max. dU = 0.000 for C26 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3558 / 350077 wR2 = 0.0920 before cycle 2 for 4424 data and 280 / 280 parameters GooF = S = 1.028; Restrained GooF = 1.028 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0452 * P )^2 + 0.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.37931 0.00058 0.250 OSF Mean shift/su = 0.051 Maximum = 0.309 for U22 C15 Max. shift = 0.001 A for C22 Max. dU = 0.000 for C26 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3558 / 350077 wR2 = 0.0920 before cycle 3 for 4424 data and 280 / 280 parameters GooF = S = 1.027; Restrained GooF = 1.027 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0452 * P )^2 + 0.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.37932 0.00058 0.007 OSF Mean shift/su = 0.002 Maximum = 0.013 for U22 C24 Max. shift = 0.000 A for C21 Max. dU = 0.000 for C24 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3558 / 350077 wR2 = 0.0920 before cycle 4 for 4424 data and 280 / 280 parameters GooF = S = 1.027; Restrained GooF = 1.027 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0452 * P )^2 + 0.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.37932 0.00058 0.001 OSF Mean shift/su = 0.001 Maximum = 0.003 for x C10 Max. shift = 0.000 A for H10 Max. dU = 0.000 for C23 Least-squares cycle 5 Maximum vector length = 511 Memory required = 3558 / 350077 wR2 = 0.0920 before cycle 5 for 4424 data and 280 / 280 parameters GooF = S = 1.027; Restrained GooF = 1.027 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0452 * P )^2 + 0.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.37932 0.00058 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z Fe1 Max. shift = 0.000 A for C8 Max. dU = 0.000 for C18 Least-squares cycle 6 Maximum vector length = 511 Memory required = 3558 / 350077 wR2 = 0.0920 before cycle 6 for 4424 data and 280 / 280 parameters GooF = S = 1.027; Restrained GooF = 1.027 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0452 * P )^2 + 0.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.37932 0.00058 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z Fe1 Max. shift = 0.000 A for H10 Max. dU = 0.000 for C17 Least-squares cycle 7 Maximum vector length = 511 Memory required = 3558 / 350077 wR2 = 0.0920 before cycle 7 for 4424 data and 280 / 280 parameters GooF = S = 1.027; Restrained GooF = 1.027 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0452 * P )^2 + 0.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.37932 0.00058 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z Fe1 Max. shift = 0.000 A for C24 Max. dU = 0.000 for C21 Least-squares cycle 8 Maximum vector length = 511 Memory required = 3558 / 350077 wR2 = 0.0920 before cycle 8 for 4424 data and 280 / 280 parameters GooF = S = 1.027; Restrained GooF = 1.027 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0452 * P )^2 + 0.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.37932 0.00058 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z Fe1 Max. shift = 0.000 A for C2 Max. dU = 0.000 for C19 Least-squares cycle 9 Maximum vector length = 511 Memory required = 3558 / 350077 wR2 = 0.0920 before cycle 9 for 4424 data and 280 / 280 parameters GooF = S = 1.027; Restrained GooF = 1.027 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0452 * P )^2 + 0.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.37932 0.00058 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z Fe1 Max. shift = 0.000 A for C14 Max. dU = 0.000 for C4 Least-squares cycle 10 Maximum vector length = 511 Memory required = 3558 / 350077 wR2 = 0.0920 before cycle 10 for 4424 data and 280 / 280 parameters GooF = S = 1.027; Restrained GooF = 1.027 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0452 * P )^2 + 0.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.37932 0.00058 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z Fe1 Max. shift = 0.000 A for C13 Max. dU = 0.000 for C25 Largest correlation matrix elements 0.557 U22 Fe1 / OSF 0.533 U33 Fe1 / OSF 0.530 U11 Fe1 / OSF Idealized hydrogen atom generation before cycle 11 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 C2 ** H2 0.4425 0.5439 0.3120 43 0.950 0.000 C2 C3 C1 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C3 ** H3 0.2929 0.6748 0.3380 43 0.950 0.000 C3 C2 C4 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C4 ** H4 0.3395 0.9124 0.3382 43 0.950 0.000 C4 C5 C3 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C5 ** H5 0.5201 0.9304 0.3146 43 0.950 0.000 C5 C4 C1 H6 0.6274 0.5997 0.2803 43 0.950 0.000 C6 C7 C1 H7 0.6988 0.8562 0.3094 43 0.950 0.000 C7 C6 C8 H10 1.0050 1.0479 0.4255 43 0.950 0.000 C10 N1 C11 H11 1.1503 0.9983 0.3793 43 0.950 0.000 C11 C12 C10 H12 1.1350 0.8189 0.2819 43 0.950 0.000 C12 C11 C13 H13 0.9788 0.6864 0.2438 43 0.950 0.000 C13 C12 C9 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C15 ** H15 0.2990 0.5594 0.0816 43 0.950 0.000 C15 C16 C14 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C16 ** H16 0.1572 0.6947 0.1163 43 0.950 0.000 C16 C15 C17 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C17 ** H17 0.2103 0.9308 0.1179 43 0.950 0.000 C17 C18 C16 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C18 ** H18 0.3866 0.9426 0.0866 43 0.950 0.000 C18 C17 C14 H19 0.4842 0.6054 0.0506 43 0.950 0.000 C19 C20 C14 H20 0.5582 0.8613 0.0702 43 0.950 0.000 C20 C19 C21 H23 0.8508 1.0706 0.1437 43 0.950 0.000 C23 N2 C24 H24 0.9929 1.0099 0.0966 43 0.950 0.000 C24 C25 C23 H25 0.9806 0.8128 0.0178 43 0.950 0.000 C25 C24 C26 H26 0.8274 0.6792 -0.0052 43 0.950 0.000 C26 C25 C22 02src649 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.52176 0.72470 0.30959 1.00000 0.01379 0.02487 0.01523 0.00118 0.00379 0.00052 0.01838 0.00350 0.00014 0.00017 0.00012 0.00000 0.00087 0.00086 0.00085 0.00070 0.00067 0.00068 0.00036 C2 0.44026 0.63537 0.31624 1.00000 0.01726 0.02258 0.02063 0.00219 0.00675 -0.00021 0.02019 0.00351 0.00014 0.00017 0.00012 0.00000 0.00093 0.00086 0.00086 0.00074 0.00070 0.00070 0.00037 H2 0.44250 0.54386 0.31202 1.00000 0.02423 0.00000 0.00000 C3 0.35633 0.70898 0.33019 1.00000 0.01741 0.03354 0.01995 0.00402 0.00859 -0.00041 0.02313 0.00379 0.00015 0.00019 0.00012 0.00000 0.00096 0.00096 0.00091 0.00080 0.00075 0.00077 0.00040 H3 0.29290 0.67476 0.33802 1.00000 0.02776 0.00000 0.00000 C4 0.38243 0.84232 0.33058 1.00000 0.02186 0.02945 0.01651 -0.00266 0.00647 0.00435 0.02275 0.00362 0.00015 0.00018 0.00012 0.00000 0.00098 0.00095 0.00083 0.00076 0.00071 0.00075 0.00040 H4 0.33953 0.91238 0.33822 1.00000 0.02730 0.00000 0.00000 C5 0.48355 0.85219 0.31759 1.00000 0.01800 0.02199 0.01661 -0.00133 0.00484 -0.00094 0.01928 0.00341 0.00014 0.00017 0.00011 0.00000 0.00093 0.00085 0.00083 0.00071 0.00069 0.00069 0.00037 H5 0.52013 0.93045 0.31465 1.00000 0.02313 0.00000 0.00000 C6 0.62075 0.68785 0.29470 1.00000 0.01559 0.02118 0.01456 0.00135 0.00381 0.00235 0.01758 0.00334 0.00013 0.00017 0.00011 0.00000 0.00091 0.00085 0.00082 0.00069 0.00067 0.00067 0.00036 H6 0.62737 0.59967 0.28033 1.00000 0.02109 0.00000 0.00000 C7 0.70382 0.76622 0.29927 1.00000 0.01589 0.02136 0.01988 0.00015 0.00598 0.00085 0.01919 0.00356 0.00014 0.00016 0.00012 0.00000 0.00091 0.00085 0.00089 0.00070 0.00071 0.00067 0.00037 H7 0.69880 0.85619 0.30943 1.00000 0.02303 0.00000 0.00000 C8 0.80246 0.71369 0.28863 1.00000 0.01794 0.02331 0.01673 0.00230 0.00672 -0.00021 0.01921 0.00360 0.00015 0.00017 0.00012 0.00000 0.00094 0.00086 0.00084 0.00072 0.00070 0.00070 0.00037 C9 0.90185 0.79816 0.31154 1.00000 0.01739 0.02095 0.01643 0.00406 0.00575 0.00120 0.01837 0.00349 0.00014 0.00016 0.00012 0.00000 0.00092 0.00082 0.00084 0.00072 0.00069 0.00069 0.00036 C10 0.99922 0.97393 0.38750 1.00000 0.02567 0.02472 0.02500 -0.00153 0.01104 -0.00546 0.02462 0.00370 0.00016 0.00018 0.00013 0.00000 0.00104 0.00091 0.00093 0.00078 0.00077 0.00077 0.00040 H10 1.00497 1.04791 0.42552 1.00000 0.02955 0.00000 0.00000 C11 1.08649 0.94574 0.36007 1.00000 0.01816 0.02730 0.02575 0.00448 0.00612 -0.00552 0.02425 0.00368 0.00015 0.00017 0.00012 0.00000 0.00096 0.00094 0.00096 0.00079 0.00076 0.00075 0.00041 H11 1.15035 0.99831 0.37931 1.00000 0.02911 0.00000 0.00000 C12 1.07802 0.83919 0.30403 1.00000 0.01708 0.02992 0.03044 0.00418 0.01242 0.00127 0.02476 0.00380 0.00015 0.00018 0.00013 0.00000 0.00096 0.00096 0.00098 0.00082 0.00078 0.00075 0.00040 H12 1.13504 0.81892 0.28191 1.00000 0.02971 0.00000 0.00000 C13 0.98532 0.76208 0.28040 1.00000 0.01757 0.02308 0.02157 0.00061 0.00795 0.00165 0.02051 0.00374 0.00015 0.00016 0.00013 0.00000 0.00091 0.00087 0.00094 0.00072 0.00073 0.00069 0.00038 H13 0.97878 0.68640 0.24384 1.00000 0.02461 0.00000 0.00000 C14 0.37998 0.73711 0.07545 1.00000 0.01649 0.02439 0.01479 -0.00130 0.00240 -0.00187 0.01947 0.00349 0.00015 0.00016 0.00012 0.00000 0.00089 0.00088 0.00084 0.00070 0.00068 0.00069 0.00037 C15 0.29913 0.65098 0.08646 1.00000 0.01871 0.02359 0.02128 -0.00351 0.00386 -0.00174 0.02215 0.00347 0.00015 0.00018 0.00012 0.00000 0.00097 0.00089 0.00089 0.00075 0.00072 0.00071 0.00039 H15 0.29899 0.55942 0.08158 1.00000 0.02658 0.00000 0.00000 C16 0.21973 0.72684 0.10588 1.00000 0.01278 0.03257 0.02379 -0.00255 0.00374 -0.00329 0.02386 0.00368 0.00015 0.00018 0.00013 0.00000 0.00090 0.00099 0.00095 0.00079 0.00073 0.00073 0.00041 H16 0.15722 0.69468 0.11634 1.00000 0.02863 0.00000 0.00000 C17 0.24960 0.85932 0.10703 1.00000 0.01652 0.02807 0.02200 -0.00133 0.00297 0.00457 0.02332 0.00357 0.00015 0.00018 0.00012 0.00000 0.00093 0.00094 0.00089 0.00078 0.00071 0.00074 0.00040 H17 0.21033 0.93084 0.11791 1.00000 0.02799 0.00000 0.00000 C18 0.34804 0.86573 0.08911 1.00000 0.02063 0.02338 0.01620 0.00206 0.00288 0.00126 0.02113 0.00350 0.00015 0.00017 0.00011 0.00000 0.00098 0.00088 0.00083 0.00073 0.00070 0.00071 0.00038 H18 0.38660 0.94257 0.08656 1.00000 0.02536 0.00000 0.00000 C19 0.47815 0.69512 0.06100 1.00000 0.01932 0.02337 0.01394 -0.00201 0.00436 0.00167 0.01934 0.00342 0.00014 0.00017 0.00011 0.00000 0.00094 0.00086 0.00081 0.00071 0.00068 0.00072 0.00037 H19 0.48419 0.60541 0.05055 1.00000 0.02321 0.00000 0.00000 C20 0.56137 0.77082 0.06097 1.00000 0.01932 0.02329 0.01684 -0.00270 0.00528 0.00108 0.02018 0.00358 0.00015 0.00017 0.00012 0.00000 0.00095 0.00086 0.00086 0.00071 0.00071 0.00071 0.00038 H20 0.55820 0.86131 0.07021 1.00000 0.02421 0.00000 0.00000 C21 0.65686 0.71537 0.04685 1.00000 0.01885 0.02647 0.01449 0.00025 0.00493 0.00166 0.02025 0.00367 0.00015 0.00018 0.00012 0.00000 0.00094 0.00090 0.00085 0.00072 0.00069 0.00072 0.00037 C22 0.75337 0.80250 0.05790 1.00000 0.01831 0.02338 0.01561 0.00280 0.00564 0.00227 0.01925 0.00354 0.00015 0.00017 0.00012 0.00000 0.00094 0.00086 0.00083 0.00072 0.00069 0.00071 0.00037 C23 0.84613 0.98977 0.11327 1.00000 0.02344 0.02372 0.03285 -0.00280 0.00993 -0.00061 0.02675 0.00386 0.00016 0.00018 0.00013 0.00000 0.00104 0.00091 0.00103 0.00082 0.00081 0.00077 0.00042 H23 0.85084 1.07064 0.14370 1.00000 0.03210 0.00000 0.00000 C24 0.93123 0.95494 0.08493 1.00000 0.01867 0.02973 0.02911 0.00595 0.00756 -0.00116 0.02615 0.00388 0.00016 0.00018 0.00013 0.00000 0.00097 0.00095 0.00099 0.00084 0.00077 0.00078 0.00041 H24 0.99294 1.00988 0.09659 1.00000 0.03138 0.00000 0.00000 C25 0.92438 0.83866 0.03938 1.00000 0.02109 0.03409 0.02200 0.00611 0.01076 0.00479 0.02491 0.00385 0.00016 0.00018 0.00012 0.00000 0.00099 0.00102 0.00091 0.00082 0.00075 0.00079 0.00041 H25 0.98063 0.81283 0.01781 1.00000 0.02989 0.00000 0.00000 C26 0.83405 0.76010 0.02560 1.00000 0.02186 0.02801 0.01692 0.00111 0.00703 0.00303 0.02227 0.00385 0.00016 0.00017 0.00013 0.00000 0.00098 0.00096 0.00087 0.00073 0.00073 0.00074 0.00040 H26 0.82735 0.67921 -0.00517 1.00000 0.02672 0.00000 0.00000 N1 0.90726 0.90346 0.36379 1.00000 0.02029 0.02496 0.02334 0.00001 0.01078 -0.00399 0.02207 0.00301 0.00012 0.00014 0.00010 0.00000 0.00082 0.00076 0.00077 0.00066 0.00063 0.00062 0.00033 N2 0.75740 0.91622 0.10036 1.00000 0.01959 0.02435 0.02587 -0.00030 0.00870 0.00092 0.02315 0.00310 0.00013 0.00014 0.00011 0.00000 0.00082 0.00076 0.00080 0.00066 0.00064 0.00062 0.00034 O1 0.80776 0.60166 0.26353 1.00000 0.02267 0.02222 0.03602 -0.00549 0.01469 -0.00250 0.02584 0.00254 0.00011 0.00012 0.00009 0.00000 0.00071 0.00064 0.00075 0.00058 0.00059 0.00053 0.00030 O2 0.66227 0.60134 0.02684 1.00000 0.02363 0.02315 0.03049 -0.00444 0.01100 0.00107 0.02543 0.00254 0.00011 0.00012 0.00009 0.00000 0.00071 0.00065 0.00071 0.00057 0.00057 0.00054 0.00029 Fe1 0.37105 0.75816 0.20613 1.00000 0.01262 0.02010 0.01689 -0.00026 0.00504 0.00010 0.01663 0.00048 0.00002 0.00002 0.00002 0.00000 0.00014 0.00015 0.00015 0.00010 0.00010 0.00009 0.00009 Final Structure Factor Calculation for 02src649 in P2(1)/c Total number of l.s. parameters = 280 Maximum vector length = 511 Memory required = 3278 / 24017 wR2 = 0.0920 before cycle 11 for 4424 data and 0 / 280 parameters GooF = S = 1.027; Restrained GooF = 1.027 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0452 * P )^2 + 0.56 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0357 for 3520 Fo > 4sig(Fo) and 0.0511 for all 4424 data wR2 = 0.0920, GooF = S = 1.027, Restrained GooF = 1.027 for all data Occupancy sum of asymmetric unit = 31.00 for non-hydrogen and 20.00 for hydrogen atoms Principal mean square atomic displacements U 0.0250 0.0169 0.0132 C1 0.0243 0.0192 0.0171 C2 0.0348 0.0198 0.0149 C3 0.0329 0.0199 0.0154 C4 0.0223 0.0197 0.0158 C5 0.0220 0.0175 0.0132 C6 0.0215 0.0203 0.0158 C7 0.0242 0.0180 0.0155 C8 0.0234 0.0177 0.0140 C9 0.0308 0.0239 0.0191 C10 0.0354 0.0225 0.0149 C11 0.0344 0.0261 0.0138 C12 0.0236 0.0214 0.0165 C13 0.0248 0.0208 0.0128 C14 0.0272 0.0232 0.0161 C15 0.0333 0.0261 0.0121 C16 0.0322 0.0232 0.0145 C17 0.0250 0.0239 0.0145 C18 0.0253 0.0192 0.0135 C19 0.0254 0.0193 0.0159 C20 0.0269 0.0194 0.0145 C21 0.0246 0.0185 0.0147 C22 0.0341 0.0233 0.0229 C23 0.0367 0.0235 0.0183 C24 0.0374 0.0205 0.0169 C25 0.0293 0.0208 0.0167 C26 0.0273 0.0237 0.0153 N1 0.0261 0.0244 0.0189 N2 0.0381 0.0203 0.0191 O1 0.0328 0.0244 0.0191 O2 0.0201 0.0172 0.0126 Fe1 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 0.030 0.041 0.054 0.070 0.089 0.115 0.161 1.000 Number in group 469. 464. 393. 445. 442. 456. 434. 437. 439. 445. GooF 0.891 0.958 1.050 1.065 1.071 1.099 1.016 0.929 1.017 1.158 K 0.748 1.021 0.999 0.978 0.983 0.980 0.982 1.001 1.018 1.027 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.31 1.64 inf Number in group 443. 453. 436. 453. 427. 446. 438. 442. 443. 443. GooF 0.948 0.891 0.897 0.955 0.943 0.993 1.044 0.876 1.252 1.359 K 1.017 1.021 1.023 0.990 1.013 1.018 1.031 1.022 1.036 1.008 R1 0.133 0.096 0.071 0.070 0.048 0.044 0.040 0.030 0.035 0.029 Recommended weighting scheme: WGHT 0.0455 0.4340 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)/su Fc/Fc(max) Resolution(A) 1 7 0 45.76 86.14 5.15 0.036 1.47 0 3 4 709.05 977.62 5.07 0.120 2.49 -5 4 4 195.29 284.37 4.79 0.065 1.79 -3 3 2 158.81 236.42 4.79 0.059 2.68 -2 6 2 28.65 62.16 4.70 0.030 1.65 -1 5 2 114.58 74.65 4.65 0.033 1.99 -6 1 4 69.29 34.18 4.02 0.022 2.09 -3 4 10 236.26 320.02 4.01 0.069 1.32 -11 3 7 415.21 542.61 3.95 0.089 1.11 -4 4 2 466.91 595.52 3.91 0.094 2.03 -5 4 3 203.59 148.59 3.80 0.047 1.83 -6 3 4 116.97 178.25 3.79 0.051 1.81 3 0 2 162.75 114.99 3.55 0.041 3.09 -5 1 10 377.83 474.65 3.54 0.083 1.48 -1 6 2 991.02 1197.48 3.47 0.133 1.68 1 2 6 81.37 115.65 3.43 0.041 2.03 -1 7 2 63.46 41.20 3.41 0.025 1.45 -8 3 4 342.55 433.13 3.37 0.080 1.48 6 5 11 40.84 85.39 3.37 0.035 0.86 -9 7 1 155.81 214.77 3.28 0.056 1.02 -1 7 5 166.61 126.81 3.26 0.043 1.33 -4 6 2 83.31 116.02 3.25 0.041 1.52 -12 4 7 457.85 589.84 3.23 0.093 1.00 -6 5 4 206.81 264.56 3.23 0.062 1.48 -9 8 1 218.82 289.38 3.20 0.065 0.95 -1 9 5 112.87 152.44 3.14 0.047 1.08 1 13 4 954.89 718.40 3.13 0.103 0.77 -10 4 1 -13.08 14.99 3.12 0.015 1.13 -10 4 2 248.56 320.44 3.12 0.069 1.15 -14 0 8 1916.79 1531.89 3.06 0.150 0.93 -1 10 4 57.45 89.88 3.04 0.036 1.00 4 3 13 30.92 57.51 3.03 0.029 0.90 -4 7 10 -8.95 12.24 3.00 0.013 1.06 -1 4 1 320.26 263.87 2.99 0.062 2.52 0 5 4 2047.95 2399.61 2.98 0.188 1.79 2 11 7 48.22 133.42 2.94 0.044 0.83 -6 2 2 297.74 365.20 2.94 0.073 2.00 -4 10 2 212.98 162.22 2.91 0.049 0.99 0 2 2 9421.97 10873.52 2.89 0.400 4.20 2 0 0 74.10 49.07 2.88 0.027 6.10 -5 2 2 2025.94 2362.84 2.88 0.186 2.34 -6 6 2 295.01 362.72 2.87 0.073 1.35 -8 1 5 233.96 289.47 2.86 0.065 1.59 -9 2 6 362.70 444.79 2.85 0.081 1.37 4 7 8 265.54 332.79 2.85 0.070 1.00 3 7 6 247.01 304.18 2.84 0.067 1.14 -1 5 8 344.15 422.60 2.82 0.079 1.39 -4 4 4 165.87 205.02 2.78 0.055 1.93 -2 3 2 15.85 31.22 2.76 0.021 2.96 -1 9 1 2.66 16.72 2.75 0.016 1.14 Bond lengths and angles C1 - Distance Angles C5 1.4315 (0.0024) C2 1.4431 (0.0025) 107.05 (0.16) C6 1.4472 (0.0024) 128.13 (0.16) 124.79 (0.16) Fe1 2.0659 (0.0017) 69.30 (0.10) 68.81 (0.10) 125.52 (0.12) C1 - C5 C2 C6 C2 - Distance Angles C3 1.4162 (0.0026) C1 1.4431 (0.0025) 107.52 (0.16) Fe1 2.0484 (0.0017) 70.03 (0.10) 70.12 (0.10) H2 0.9500 126.24 126.24 125.21 C2 - C3 C1 Fe1 C3 - Distance Angles C2 1.4162 (0.0026) C4 1.4204 (0.0027) 108.90 (0.16) Fe1 2.0542 (0.0018) 69.59 (0.10) 70.10 (0.10) H3 0.9500 125.55 125.55 126.35 C3 - C2 C4 Fe1 C4 - Distance Angles C5 1.4130 (0.0026) C3 1.4204 (0.0027) 107.82 (0.16) Fe1 2.0618 (0.0017) 69.71 (0.10) 69.52 (0.10) H4 0.9500 126.09 126.09 126.25 C4 - C5 C3 Fe1 C5 - Distance Angles C4 1.4130 (0.0026) C1 1.4315 (0.0024) 108.69 (0.15) Fe1 2.0559 (0.0017) 70.16 (0.10) 70.06 (0.10) H5 0.9500 125.66 125.66 125.71 C5 - C4 C1 Fe1 C6 - Distance Angles C7 1.3377 (0.0025) C1 1.4472 (0.0024) 126.15 (0.16) H6 0.9500 116.92 116.92 C6 - C7 C1 C7 - Distance Angles C6 1.3377 (0.0025) C8 1.4643 (0.0025) 120.17 (0.16) H7 0.9500 119.92 119.92 C7 - C6 C8 C8 - Distance Angles O1 1.2316 (0.0021) C7 1.4643 (0.0025) 122.49 (0.16) C9 1.4993 (0.0025) 118.63 (0.16) 118.87 (0.15) C8 - O1 C7 C9 - Distance Angles N1 1.3409 (0.0023) C13 1.3948 (0.0025) 123.17 (0.16) C8 1.4993 (0.0025) 117.81 (0.16) 118.99 (0.16) C9 - N1 C13 C10 - Distance Angles N1 1.3397 (0.0023) C11 1.3858 (0.0026) 124.14 (0.17) H10 0.9500 117.93 117.93 C10 - N1 C11 C11 - Distance Angles C12 1.3796 (0.0026) C10 1.3858 (0.0026) 118.14 (0.17) H11 0.9500 120.93 120.93 C11 - C12 C10 C12 - Distance Angles C11 1.3796 (0.0026) C13 1.3859 (0.0026) 119.18 (0.17) H12 0.9500 120.41 120.41 C12 - C11 C13 C13 - Distance Angles C12 1.3859 (0.0026) C9 1.3948 (0.0025) 118.46 (0.17) H13 0.9500 120.77 120.77 C13 - C12 C9 C14 - Distance Angles C18 1.4330 (0.0024) C15 1.4401 (0.0026) 106.91 (0.16) C19 1.4487 (0.0025) 128.58 (0.16) 124.33 (0.16) Fe1 2.0708 (0.0018) 68.70 (0.10) 69.30 (0.10) 123.23 (0.12) C14 - C18 C15 C19 C15 - Distance Angles C16 1.4185 (0.0026) C14 1.4401 (0.0026) 108.00 (0.16) Fe1 2.0626 (0.0017) 69.23 (0.10) 69.92 (0.10) H15 0.9500 126.00 126.00 126.42 C15 - C16 C14 Fe1 C16 - Distance Angles C15 1.4185 (0.0026) C17 1.4234 (0.0025) 108.43 (0.16) Fe1 2.0473 (0.0018) 70.39 (0.10) 69.65 (0.10) H16 0.9500 125.78 125.78 125.76 C16 - C15 C17 Fe1 C17 - Distance Angles C18 1.4146 (0.0027) C16 1.4234 (0.0025) 107.96 (0.16) Fe1 2.0471 (0.0018) 69.74 (0.10) 69.67 (0.10) H17 0.9500 126.02 126.02 126.15 C17 - C18 C16 Fe1 C18 - Distance Angles C17 1.4146 (0.0027) C14 1.4330 (0.0024) 108.69 (0.16) Fe1 2.0460 (0.0017) 69.82 (0.10) 70.56 (0.10) H18 0.9500 125.66 125.66 125.54 C18 - C17 C14 Fe1 C19 - Distance Angles C20 1.3420 (0.0026) C14 1.4487 (0.0025) 126.23 (0.17) H19 0.9500 116.88 116.88 C19 - C20 C14 C20 - Distance Angles C19 1.3420 (0.0026) C21 1.4619 (0.0026) 120.63 (0.17) H20 0.9500 119.68 119.68 C20 - C19 C21 C21 - Distance Angles O2 1.2277 (0.0022) C20 1.4619 (0.0026) 123.02 (0.17) C22 1.5105 (0.0027) 118.63 (0.17) 118.35 (0.16) C21 - O2 C20 C22 - Distance Angles N2 1.3378 (0.0023) C26 1.3922 (0.0026) 123.49 (0.17) C21 1.5105 (0.0027) 117.54 (0.16) 118.96 (0.16) C22 - N2 C26 C23 - Distance Angles N2 1.3417 (0.0024) C24 1.3841 (0.0027) 123.96 (0.17) H23 0.9500 118.02 118.02 C23 - N2 C24 C24 - Distance Angles C25 1.3791 (0.0026) C23 1.3841 (0.0027) 118.48 (0.18) H24 0.9500 120.76 120.76 C24 - C25 C23 C25 - Distance Angles C24 1.3791 (0.0026) C26 1.3862 (0.0027) 118.90 (0.18) H25 0.9500 120.55 120.55 C25 - C24 C26 C26 - Distance Angles C25 1.3862 (0.0027) C22 1.3922 (0.0026) 118.46 (0.17) H26 0.9500 120.77 120.77 C26 - C25 C22 N1 - Distance Angles C10 1.3397 (0.0023) C9 1.3409 (0.0023) 116.86 (0.16) N1 - C10 N2 - Distance Angles C23 1.3417 (0.0024) C22 1.3378 (0.0023) 116.69 (0.16) N2 - C23 O1 - Distance Angles C8 1.2316 (0.0022) O1 - O2 - Distance Angles C21 1.2277 (0.0022) O2 - Fe1 - Distance Angles C18 2.0460 (0.0017) C17 2.0471 (0.0018) 40.44 (0.07) C16 2.0473 (0.0018) 68.22 (0.07) 40.69 (0.07) C2 2.0484 (0.0017) 161.16 (0.07) 157.63 (0.08) 122.84 (0.08) C3 2.0542 (0.0018) 157.15 (0.08) 120.71 (0.08) 105.70 (0.08) 40.39 (0.07) C5 2.0559 (0.0017) 108.08 (0.07) 120.52 (0.07) 155.26 (0.07) 68.56 (0.07) 67.71 (0.07) C4 2.0618 (0.0017) 121.87 (0.07) 104.60 (0.07) 119.45 (0.08) 68.32 (0.07) 40.37 (0.07) 40.14 (0.07) C15 2.0626 (0.0017) 68.36 (0.07) 68.25 (0.07) 40.38 (0.07) 109.15 (0.07) 122.16 (0.08) 163.12 (0.07) 156.04 (0.08) C1 2.0659 (0.0017) 124.38 (0.07) 157.88 (0.07) 161.20 (0.08) 41.06 (0.07) 68.08 (0.07) 40.64 (0.07) 68.10 (0.07) C14 2.0708 (0.0018) 40.73 (0.07) 68.37 (0.07) 68.33 (0.07) 125.18 (0.07) 159.52 (0.07) 125.85 (0.07) 159.82 (0.07) Fe1 - C18 C17 C16 C2 C3 C5 C4 FMAP and GRID set by program FMAP 2 3 22 GRID -1.316 -2 -2 1.316 2 2 R1 = 0.0499 for 4424 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.46 at 0.1111 0.2535 0.1179 [ 1.25 A from C9 ] Deepest hole -0.56 at 0.3037 0.7604 0.1710 [ 0.85 A from FE1 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 3266 / 24332 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.8889 0.7535 0.3821 1.00000 0.05 0.46 1.25 C9 1.53 C8 1.61 N1 2.11 H25 Q2 1 0.5013 0.7745 0.3081 1.00000 0.05 0.34 0.58 C1 0.86 C5 1.63 H5 1.67 C2 Q3 1 0.7030 0.7694 0.0492 1.00000 0.05 0.34 0.71 C22 0.81 C21 1.74 N2 1.81 O2 Q4 1 0.5612 0.7228 0.2940 1.00000 0.05 0.33 0.64 C1 0.86 C6 1.60 H6 1.80 C5 Q5 1 0.7508 0.7373 0.2905 1.00000 0.05 0.30 0.73 C8 0.74 C7 1.49 H7 1.71 O1 Q6 1 0.2360 0.7843 0.1061 1.00000 0.05 0.29 0.63 C16 0.79 C17 1.44 H16 1.58 H17 Q7 1 0.6054 0.7590 0.0412 1.00000 0.05 0.29 0.75 C20 0.79 C21 1.38 H20 1.84 O2 Q8 1 0.2939 0.8633 0.0933 1.00000 0.05 0.28 0.69 C17 0.74 C18 1.46 H17 1.50 H18 Q9 1 0.4225 0.7265 0.0636 1.00000 0.05 0.28 0.65 C14 0.81 C19 1.54 H19 1.86 C18 Q10 1 0.3982 0.6619 0.3322 1.00000 0.05 0.27 0.73 C3 0.73 C2 1.42 H3 1.43 H2 Shortest distances between peaks (including symmetry equivalents) 2 4 1.03 6 8 1.18 3 7 1.24 1 5 1.85 2 10 1.92 8 9 2.37 4 10 2.49 4 5 2.51 7 9 2.56 6 9 2.81 Time profile in seconds ----------------------- 0.02: 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. 0.64: Read intensity data, sort/merge etc. 0.02: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.80: Structure factors and derivatives 3.83: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.45: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.00: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 11:10:08 Total CPU time: 6.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++