+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 11:57:48 on 04-Jul-2002 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 02SOT077 in P-1 CELL 0.71073 11.0968 11.1517 11.9917 102.233 95.688 92.374 ZERR 2.00 0.0004 0.0004 0.0005 0.002 0.002 0.003 LATT 1 SFAC C H N O FE CL UNIT 60 54 4 10 2 6 V = 1440.14 F(000) = 676.0 Mu = 0.85 mm-1 Cell Wt = 1315.47 Rho = 1.517 MERG 2 ISOR 0.001 C30 FMAP 2 PLAN 20 OMIT -1 4 2 OMIT -1 2 0 OMIT 1 0 2 OMIT 2 0 0 OMIT -4 -1 1 OMIT -2 5 2 BOND $H OMIT 0-3 55 TEMP -153 SIZE 0.16 0.12 0.06 ACTA L.S. 4 WGHT 0.079900 2.059600 EXTI 0.000000 FVAR 0.41471 O5 4 1.620198 0.344606 0.499148 11.00000 0.03160 0.03545 = 0.02024 0.01164 -0.00313 0.00490 O4 4 1.561839 0.564044 0.637443 11.00000 0.01211 0.05447 = 0.04623 0.02286 0.01010 0.01105 AFIX 147 H4 2 1.603011 0.503022 0.618066 11.00000 -1.50000 AFIX 0 C30 1 1.514740 0.571435 0.582110 11.00000 0.05231 0.04900 = 0.04979 0.00369 0.00859 0.01741 AFIX 137 H30A 2 1.505667 0.658904 0.584228 11.00000 -1.50000 H30B 2 1.435491 0.530980 0.585475 11.00000 -1.50000 H30C 2 1.547016 0.533215 0.510784 11.00000 -1.50000 AFIX 0 MOLE 1 C1 1 0.750689 0.515002 0.866117 11.00000 0.02027 0.02309 = 0.02267 -0.00126 0.00424 -0.00061 C2 1 0.854730 0.595063 0.884389 11.00000 0.01726 0.02275 = 0.02088 0.00241 0.00182 0.00101 C3 1 0.936707 0.538263 0.808867 11.00000 0.01939 0.02012 = 0.02132 0.00289 0.00098 0.00162 C4 1 0.878149 0.427211 0.745872 11.00000 0.01825 0.02011 = 0.02506 0.00121 0.00353 0.00081 C5 1 0.638831 0.514019 0.919817 11.00000 0.02096 0.02682 = 0.02510 0.00051 0.00334 0.00225 C6 1 0.880230 0.714889 0.965045 11.00000 0.02089 0.02277 = 0.02001 0.00169 0.00469 -0.00040 C7 1 0.802805 0.810917 0.963900 11.00000 0.02333 0.02514 = 0.02516 0.00291 0.00223 0.00223 AFIX 43 H7 2 0.729412 0.797341 0.913707 11.00000 -1.20000 AFIX 0 C8 1 0.832374 0.925221 1.035218 11.00000 0.03290 0.02260 = 0.03511 0.00428 0.01004 0.00516 AFIX 43 H8 2 0.779255 0.989648 1.033697 11.00000 -1.20000 AFIX 0 C9 1 0.939174 0.946286 1.108948 11.00000 0.03815 0.02318 = 0.03010 -0.00241 0.00752 -0.00358 AFIX 43 H9 2 0.959856 1.025240 1.157059 11.00000 -1.20000 AFIX 0 C10 1 1.015812 0.851321 1.112115 11.00000 0.02654 0.03349 = 0.02705 -0.00178 -0.00129 -0.00476 AFIX 43 H10 2 1.088275 0.865015 1.163597 11.00000 -1.20000 AFIX 0 C11 1 0.986975 0.736949 1.040593 11.00000 0.02223 0.02707 = 0.02629 0.00251 0.00451 0.00239 AFIX 43 H11 2 1.040245 0.672768 1.042844 11.00000 -1.20000 AFIX 0 C12 1 1.060674 0.586743 0.800062 11.00000 0.01939 0.02011 = 0.01996 -0.00026 0.00422 -0.00095 C13 1 1.161167 0.521488 0.825305 11.00000 0.02210 0.02348 = 0.02920 0.00577 0.00434 -0.00066 AFIX 43 H13 2 1.149592 0.446867 0.850234 11.00000 -1.20000 AFIX 0 C14 1 1.277085 0.564450 0.814353 11.00000 0.01996 0.03477 = 0.03851 0.00370 -0.00011 0.00056 AFIX 43 H14 2 1.344585 0.518827 0.830599 11.00000 -1.20000 AFIX 0 C15 1 1.294635 0.673666 0.779800 11.00000 0.02354 0.03434 = 0.05150 0.00515 0.01095 -0.00838 AFIX 43 H15 2 1.374328 0.703082 0.772215 11.00000 -1.20000 AFIX 0 C16 1 1.197009 0.740297 0.756232 11.00000 0.03504 0.02645 = 0.05232 0.00982 0.01117 -0.00661 AFIX 43 H16 2 1.209697 0.816083 0.733614 11.00000 -1.20000 AFIX 0 C17 1 1.080009 0.696752 0.765516 11.00000 0.02723 0.02635 = 0.03450 0.00733 0.00403 0.00277 AFIX 43 H17 2 1.012906 0.742402 0.748163 11.00000 -1.20000 AFIX 0 C18 1 0.910477 0.330079 0.651096 11.00000 0.01934 0.02298 = 0.02532 0.00108 0.00256 0.00027 C19 1 1.062094 0.277483 0.514848 11.00000 0.01956 0.02757 = 0.02298 -0.00038 0.00262 0.00210 C20 1 1.030359 0.149765 0.469611 11.00000 0.02541 0.02634 = 0.02683 -0.00345 -0.00258 0.00451 AFIX 43 H20 2 0.968524 0.101303 0.492023 11.00000 -1.20000 AFIX 0 C21 1 1.109021 0.109109 0.384661 11.00000 0.02911 0.03842 = 0.02298 -0.00471 -0.00163 0.01100 AFIX 43 H21 2 1.108677 0.027815 0.339971 11.00000 -1.20000 AFIX 0 C22 1 1.188312 0.209936 0.377464 11.00000 0.02919 0.04907 = 0.02281 0.00549 0.00660 0.01350 AFIX 43 H22 2 1.249587 0.207998 0.327235 11.00000 -1.20000 AFIX 0 C23 1 1.159303 0.314688 0.459323 11.00000 0.02520 0.03630 = 0.02721 0.00751 0.00357 0.00287 AFIX 43 H23 2 1.198224 0.394817 0.473854 11.00000 -1.20000 AFIX 0 C24 1 1.266017 0.198245 0.709260 11.00000 0.03444 0.03515 = 0.02338 -0.00170 -0.00170 0.00784 AFIX 43 H24 2 1.232074 0.249043 0.770768 11.00000 -1.20000 AFIX 0 C25 1 1.230584 0.073096 0.660129 11.00000 0.03380 0.02970 = 0.02754 0.00577 -0.00093 0.00301 AFIX 43 H25 2 1.168214 0.025578 0.682875 11.00000 -1.20000 AFIX 0 C26 1 1.303607 0.031015 0.571720 11.00000 0.03448 0.03441 = 0.02764 -0.00083 -0.00324 0.01146 AFIX 43 H26 2 1.299407 -0.049861 0.525484 11.00000 -1.20000 AFIX 0 C27 1 1.383843 0.129439 0.563707 11.00000 0.02447 0.05242 = 0.03518 0.00771 0.00186 0.01228 AFIX 43 H27 2 1.442299 0.126865 0.510621 11.00000 -1.20000 AFIX 0 C28 1 1.361539 0.234143 0.649934 11.00000 0.02780 0.03535 = 0.04149 0.00637 -0.00854 -0.00216 AFIX 43 H28 2 1.402996 0.313104 0.664752 11.00000 -1.20000 AFIX 0 N1 3 0.768329 0.415297 0.782692 11.00000 0.01737 0.02323 = 0.02813 -0.00290 0.00599 -0.00463 N2 3 1.007651 0.357160 0.599930 11.00000 0.02017 0.02088 = 0.02566 -0.00236 0.00680 -0.00100 O1 4 0.627265 0.610410 1.001613 11.00000 0.02294 0.02798 = 0.03408 -0.00468 0.01230 -0.00284 AFIX 147 H1 2 0.559085 0.604619 1.025524 11.00000 -1.50000 AFIX 0 O2 4 0.562184 0.426565 0.889069 11.00000 0.01993 0.02928 = 0.03512 -0.00487 0.00831 -0.00553 O3 4 0.848748 0.232394 0.620896 11.00000 0.03036 0.02664 = 0.03713 -0.00761 0.01260 -0.00768 FE1 5 1.209658 0.175147 0.537599 11.00000 0.02140 0.02952 = 0.02195 -0.00027 0.00238 0.00428 H1N 2 0.724919 0.360696 0.757575 11.00000 0.03449 H2N 2 1.044932 0.421601 0.622568 11.00000 0.03814 MOLE 2 C29 1 0.456975 0.925417 0.194614 11.00000 0.02812 0.03704 = 0.03557 0.01222 0.00847 0.00374 AFIX 13 H29 2 0.533682 0.891273 0.221767 11.00000 -1.20000 AFIX 0 CL1 6 0.341309 0.886097 0.272511 11.00000 0.02534 0.03286 = 0.03547 0.00418 0.00722 -0.00242 CL2 6 0.479584 1.087518 0.221616 11.00000 0.05621 0.03969 = 0.06379 0.01746 0.00581 -0.01298 CL3 6 0.421660 0.862990 0.047505 11.00000 0.07793 0.05315 = 0.03199 0.00981 0.01280 0.02146 HKLF 4 Covalent radii and connectivity table for 02SOT077 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 FE 1.240 CL 0.990 O5 - no bonds found O4 - C30 C30 - O4 C1 - N1 C2 C5 C2 - C1 C3 C6 C3 - C4 C2 C12 C4 - N1 C3 C18 C5 - O2 O1 C1 C6 - C11 C7 C2 C7 - C8 C6 C8 - C7 C9 C9 - C8 C10 C10 - C11 C9 C11 - C10 C6 C12 - C17 C13 C3 C13 - C14 C12 C14 - C15 C13 C15 - C16 C14 C16 - C15 C17 C17 - C16 C12 C18 - O3 N2 C4 C19 - N2 C23 C20 Fe1 C20 - C21 C19 Fe1 C21 - C20 C22 Fe1 C22 - C21 C23 Fe1 C23 - C19 C22 Fe1 C24 - C25 C28 Fe1 C25 - C26 C24 Fe1 C26 - C27 C25 Fe1 C27 - C26 C28 Fe1 C28 - C24 C27 Fe1 N1 - C4 C1 N2 - C18 C19 O1 - C5 O2 - C5 O3 - C18 Fe1 - C21 C27 C22 C28 C26 C25 C24 C23 C20 C19 C29 - Cl3 Cl1 Cl2 Cl1 - C29 Cl2 - C29 Cl3 - C29 21411 Reflections read, of which 30 rejected -14 =< h =< 14, -14 =< k =< 14, -15 =< l =< 15, Max. 2-theta = 54.96 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -3 0 1 1261.90 24.47 6 158.18 -1 1 1 1007.78 32.51 3 191.92 -10 2 1 181.35 2.87 4 39.60 -9 -4 2 146.96 2.44 6 15.47 -8 -3 2 318.69 3.74 7 42.67 -3 0 2 125.59 3.07 4 16.69 -10 4 4 12.08 1.00 2 13.56 -9 3 7 9.98 0.89 3 5.75 -9 3 8 13.91 0.84 4 4.62 9 Inconsistent equivalents 6433 Unique reflections, of which 0 suppressed R(int) = 0.0476 R(sigma) = 0.0492 Friedel opposites merged Maximum memory for data reduction = 3528 / 64500 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 = 4543 / 489360 wR2 = 0.1536 before cycle 1 for 6433 data and 382 / 382 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint 0.0073 0.0010 ISOR U23 C30 -0.0141 0.0010 ISOR U12 C30 Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 6. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.007 0.000 GooF = S = 1.024; Restrained GooF = 1.045 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 2.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41483 0.00100 0.123 OSF 2 0.00000 0.00121 -2.827 EXTI Mean shift/esd = 0.016 Maximum = -2.827 for EXTI Max. shift = 0.004 A for H30A Max. dU = 0.000 for H2N Least-squares cycle 2 Maximum vector length = 511 Memory required = 4543 / 489360 wR2 = 0.1538 before cycle 2 for 6433 data and 382 / 382 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint 0.0074 0.0010 ISOR U23 C30 -0.0133 0.0010 ISOR U12 C30 Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 6. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.006 0.000 GooF = S = 1.026; Restrained GooF = 1.045 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 2.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41469 0.00100 -0.149 OSF 2 0.00000 0.00121 -3.772 EXTI Mean shift/esd = 0.019 Maximum = -3.772 for EXTI Max. shift = 0.004 A for H30A Max. dU = 0.000 for H2N Least-squares cycle 3 Maximum vector length = 511 Memory required = 4543 / 489360 wR2 = 0.1539 before cycle 3 for 6433 data and 382 / 382 parameters Disagreeable restraints before cycle 3 Observed Target Error Sigma Restraint 0.0074 0.0010 ISOR U23 C30 -0.0123 0.0010 ISOR U12 C30 Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 6. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.006 0.000 GooF = S = 1.027; Restrained GooF = 1.044 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 2.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41468 0.00100 -0.009 OSF 2 0.00000 0.00121 -3.776 EXTI Mean shift/esd = 0.017 Maximum = -3.776 for EXTI Max. shift = 0.003 A for H30A Max. dU = 0.000 for H2N Least-squares cycle 4 Maximum vector length = 511 Memory required = 4543 / 489360 wR2 = 0.1541 before cycle 4 for 6433 data and 382 / 382 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint 0.0074 0.0010 ISOR U23 C30 -0.0116 0.0010 ISOR U12 C30 Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 6. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.006 0.000 GooF = S = 1.028; Restrained GooF = 1.044 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 2.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41467 0.00100 -0.005 OSF 2 0.00000 0.00121 -3.778 EXTI Mean shift/esd = 0.015 Maximum = -3.778 for EXTI Max. shift = 0.002 A for H30A Max. dU = 0.000 for H2N Largest correlation matrix elements 0.510 U11 Fe1 / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H4 1.6033 0.5032 0.6183 147 0.840 0.000 O4 C30 H4 H30A 1.5065 0.6588 0.5835 137 0.980 0.000 C30 O4 H30A H30B 1.4353 0.5317 0.5859 137 0.980 0.000 C30 O4 H30A H30C 1.5468 0.5321 0.5109 137 0.980 0.000 C30 O4 H30A H7 0.7294 0.7973 0.9137 43 0.950 0.000 C7 C8 C6 H8 0.7792 0.9896 1.0337 43 0.950 0.000 C8 C7 C9 H9 0.9599 1.0252 1.1571 43 0.950 0.000 C9 C8 C10 H10 1.0883 0.8650 1.1636 43 0.950 0.000 C10 C11 C9 H11 1.0402 0.6728 1.0428 43 0.950 0.000 C11 C10 C6 H13 1.1496 0.4469 0.8502 43 0.950 0.000 C13 C14 C12 H14 1.3446 0.5188 0.8306 43 0.950 0.000 C14 C15 C13 H15 1.3743 0.7031 0.7722 43 0.950 0.000 C15 C16 C14 H16 1.2097 0.8161 0.7336 43 0.950 0.000 C16 C15 C17 H17 1.0129 0.7424 0.7482 43 0.950 0.000 C17 C16 C12 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C20 ** H20 0.9685 0.1013 0.4920 43 0.950 0.000 C20 C21 C19 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C21 ** H21 1.1087 0.0278 0.3400 43 0.950 0.000 C21 C20 C22 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C22 ** H22 1.2496 0.2080 0.3272 43 0.950 0.000 C22 C21 C23 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C23 ** H23 1.1982 0.3948 0.4739 43 0.950 0.000 C23 C19 C22 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C24 ** H24 1.2321 0.2491 0.7708 43 0.950 0.000 C24 C25 C28 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C25 ** H25 1.1682 0.0256 0.6829 43 0.950 0.000 C25 C26 C24 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C26 ** H26 1.2994 -0.0499 0.5255 43 0.950 0.000 C26 C27 C25 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C27 ** H27 1.4423 0.1269 0.5106 43 0.950 0.000 C27 C26 C28 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C28 ** H28 1.4030 0.3131 0.6648 43 0.950 0.000 C28 C24 C27 H1 0.5590 0.6047 1.0255 147 0.840 0.000 O1 C5 H1 H29 0.5337 0.8913 0.2218 13 1.000 0.000 C29 Cl3 Cl1 Cl2 02SOT077 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq O5 1.62020 0.34461 0.49915 1.00000 0.03158 0.03546 0.02025 0.01166 -0.00315 0.00492 0.02859 0.00434 0.00020 0.00021 0.00018 0.00000 0.00117 0.00122 0.00105 0.00091 0.00087 0.00093 0.00049 O4 1.56186 0.56412 0.63752 1.00000 0.01223 0.05470 0.04569 0.02240 0.00999 0.01083 0.03512 0.00551 0.00020 0.00025 0.00024 0.00000 0.00105 0.00164 0.00150 0.00126 0.00103 0.00098 0.00057 H4 1.60325 0.50324 0.61829 1.00000 0.05267 0.00000 0.00000 C30 1.51487 0.57135 0.58211 1.00000 0.05225 0.04907 0.04975 0.00362 0.00837 0.01425 0.05092 0.00986 0.00046 0.00043 0.00043 0.00000 0.00134 0.00132 0.00133 0.00092 0.00094 0.00094 0.00106 H30A 1.50651 0.65878 0.58351 1.00000 0.07637 0.00000 0.00000 H30B 1.43533 0.53174 0.58592 1.00000 0.07637 0.00000 0.00000 H30C 1.54681 0.53213 0.51091 1.00000 0.07637 0.00000 0.00000 C1 0.75069 0.51500 0.86612 1.00000 0.02026 0.02306 0.02266 -0.00126 0.00423 -0.00061 0.02285 0.00567 0.00026 0.00027 0.00026 0.00000 0.00141 0.00143 0.00143 0.00114 0.00113 0.00110 0.00060 C2 0.85473 0.59506 0.88439 1.00000 0.01727 0.02276 0.02087 0.00241 0.00183 0.00103 0.02067 0.00553 0.00025 0.00026 0.00025 0.00000 0.00134 0.00138 0.00139 0.00111 0.00107 0.00106 0.00057 C3 0.93671 0.53827 0.80887 1.00000 0.01938 0.02009 0.02131 0.00287 0.00098 0.00162 0.02058 0.00553 0.00025 0.00026 0.00025 0.00000 0.00137 0.00135 0.00139 0.00110 0.00110 0.00106 0.00057 C4 0.87814 0.42721 0.74587 1.00000 0.01823 0.02008 0.02505 0.00117 0.00350 0.00081 0.02161 0.00558 0.00026 0.00026 0.00025 0.00000 0.00137 0.00136 0.00148 0.00115 0.00113 0.00106 0.00059 C5 0.63883 0.51402 0.91982 1.00000 0.02096 0.02682 0.02510 0.00052 0.00332 0.00224 0.02498 0.00587 0.00027 0.00028 0.00026 0.00000 0.00145 0.00153 0.00152 0.00122 0.00118 0.00116 0.00063 C6 0.88023 0.71489 0.96505 1.00000 0.02088 0.02278 0.02001 0.00170 0.00470 -0.00037 0.02155 0.00559 0.00026 0.00026 0.00025 0.00000 0.00140 0.00141 0.00139 0.00111 0.00111 0.00110 0.00058 C7 0.80280 0.81092 0.96390 1.00000 0.02335 0.02512 0.02515 0.00290 0.00223 0.00223 0.02493 0.00593 0.00027 0.00027 0.00026 0.00000 0.00149 0.00150 0.00152 0.00121 0.00120 0.00116 0.00063 H7 0.72941 0.79734 0.91370 1.00000 0.02992 0.00000 0.00000 C8 0.83237 0.92522 1.03522 1.00000 0.03287 0.02260 0.03511 0.00426 0.01005 0.00514 0.02997 0.00664 0.00031 0.00029 0.00029 0.00000 0.00171 0.00151 0.00176 0.00130 0.00138 0.00124 0.00069 H8 0.77925 0.98965 1.03370 1.00000 0.03596 0.00000 0.00000 C9 0.93918 0.94628 1.10895 1.00000 0.03816 0.02318 0.03009 -0.00241 0.00752 -0.00359 0.03160 0.00647 0.00031 0.00029 0.00029 0.00000 0.00184 0.00152 0.00169 0.00128 0.00140 0.00130 0.00072 H9 0.95986 1.02524 1.15706 1.00000 0.03792 0.00000 0.00000 C10 1.01582 0.85131 1.11211 1.00000 0.02653 0.03347 0.02707 -0.00176 -0.00130 -0.00476 0.03075 0.00609 0.00030 0.00030 0.00028 0.00000 0.00161 0.00172 0.00163 0.00133 0.00128 0.00128 0.00070 H10 1.08828 0.86501 1.16360 1.00000 0.03690 0.00000 0.00000 C11 0.98697 0.73695 1.04059 1.00000 0.02223 0.02707 0.02628 0.00250 0.00450 0.00235 0.02554 0.00595 0.00027 0.00028 0.00026 0.00000 0.00147 0.00152 0.00156 0.00123 0.00119 0.00116 0.00063 H11 1.04024 0.67277 1.04284 1.00000 0.03064 0.00000 0.00000 C12 1.06068 0.58674 0.80006 1.00000 0.01935 0.02010 0.01997 -0.00028 0.00420 -0.00096 0.02042 0.00546 0.00026 0.00026 0.00024 0.00000 0.00136 0.00134 0.00138 0.00108 0.00108 0.00105 0.00057 C13 1.16117 0.52148 0.82531 1.00000 0.02209 0.02350 0.02919 0.00580 0.00433 -0.00065 0.02487 0.00593 0.00027 0.00028 0.00027 0.00000 0.00147 0.00145 0.00158 0.00122 0.00121 0.00114 0.00062 H13 1.14960 0.44686 0.85023 1.00000 0.02985 0.00000 0.00000 C14 1.27708 0.56445 0.81436 1.00000 0.01995 0.03479 0.03847 0.00372 -0.00013 0.00056 0.03197 0.00638 0.00028 0.00031 0.00030 0.00000 0.00150 0.00175 0.00185 0.00144 0.00133 0.00126 0.00072 H14 1.34458 0.51883 0.83061 1.00000 0.03836 0.00000 0.00000 C15 1.29464 0.67367 0.77980 1.00000 0.02353 0.03433 0.05154 0.00518 0.01094 -0.00835 0.03691 0.00693 0.00031 0.00032 0.00033 0.00000 0.00162 0.00181 0.00220 0.00159 0.00151 0.00134 0.00081 H15 1.37433 0.70308 0.77222 1.00000 0.04429 0.00000 0.00000 C16 1.19701 0.74030 0.75623 1.00000 0.03504 0.02649 0.05228 0.00984 0.01115 -0.00663 0.03756 0.00717 0.00032 0.00031 0.00034 0.00000 0.00187 0.00165 0.00222 0.00154 0.00163 0.00137 0.00081 H16 1.20970 0.81608 0.73361 1.00000 0.04507 0.00000 0.00000 C17 1.08001 0.69676 0.76551 1.00000 0.02724 0.02635 0.03447 0.00731 0.00402 0.00277 0.02918 0.00646 0.00030 0.00029 0.00029 0.00000 0.00160 0.00155 0.00175 0.00132 0.00132 0.00122 0.00068 H17 1.01291 0.74241 0.74816 1.00000 0.03501 0.00000 0.00000 C18 0.91048 0.33007 0.65110 1.00000 0.01935 0.02296 0.02532 0.00104 0.00254 0.00025 0.02320 0.00571 0.00026 0.00027 0.00026 0.00000 0.00140 0.00142 0.00148 0.00116 0.00115 0.00111 0.00061 C19 1.06209 0.27749 0.51484 1.00000 0.01955 0.02755 0.02297 -0.00038 0.00261 0.00212 0.02420 0.00575 0.00026 0.00028 0.00026 0.00000 0.00142 0.00153 0.00148 0.00120 0.00114 0.00114 0.00062 C20 1.03035 0.14976 0.46961 1.00000 0.02541 0.02634 0.02683 -0.00345 -0.00259 0.00449 0.02787 0.00595 0.00029 0.00029 0.00027 0.00000 0.00154 0.00155 0.00158 0.00124 0.00123 0.00120 0.00067 H20 0.96851 0.10130 0.49202 1.00000 0.03344 0.00000 0.00000 C21 1.10902 0.10911 0.38467 1.00000 0.02911 0.03839 0.02299 -0.00470 -0.00163 0.01099 0.03192 0.00643 0.00029 0.00032 0.00027 0.00000 0.00167 0.00182 0.00157 0.00134 0.00128 0.00138 0.00073 H21 1.10867 0.02781 0.33998 1.00000 0.03830 0.00000 0.00000 C22 1.18832 0.20994 0.37747 1.00000 0.02919 0.04903 0.02283 0.00549 0.00660 0.01352 0.03346 0.00705 0.00031 0.00034 0.00028 0.00000 0.00169 0.00205 0.00158 0.00143 0.00128 0.00146 0.00075 H22 1.24959 0.20800 0.32724 1.00000 0.04015 0.00000 0.00000 C23 1.15931 0.31469 0.45932 1.00000 0.02517 0.03632 0.02721 0.00752 0.00358 0.00289 0.02940 0.00656 0.00029 0.00032 0.00028 0.00000 0.00159 0.00175 0.00161 0.00135 0.00127 0.00129 0.00068 H23 1.19823 0.39482 0.47386 1.00000 0.03528 0.00000 0.00000 C24 1.26601 0.19825 0.70926 1.00000 0.03446 0.03519 0.02335 -0.00172 -0.00170 0.00783 0.03238 0.00647 0.00031 0.00032 0.00028 0.00000 0.00177 0.00176 0.00158 0.00133 0.00132 0.00137 0.00073 H24 1.23206 0.24905 0.77076 1.00000 0.03886 0.00000 0.00000 C25 1.23059 0.07310 0.66013 1.00000 0.03378 0.02966 0.02756 0.00576 -0.00091 0.00303 0.03067 0.00650 0.00031 0.00030 0.00028 0.00000 0.00173 0.00164 0.00162 0.00131 0.00133 0.00131 0.00069 H25 1.16822 0.02558 0.68287 1.00000 0.03680 0.00000 0.00000 C26 1.30361 0.03102 0.57172 1.00000 0.03448 0.03438 0.02762 -0.00083 -0.00326 0.01146 0.03348 0.00671 0.00031 0.00032 0.00029 0.00000 0.00178 0.00177 0.00166 0.00137 0.00136 0.00139 0.00074 H26 1.29941 -0.04986 0.52549 1.00000 0.04018 0.00000 0.00000 C27 1.38384 0.12945 0.56371 1.00000 0.02447 0.05245 0.03517 0.00772 0.00183 0.01231 0.03745 0.00734 0.00031 0.00036 0.00031 0.00000 0.00166 0.00219 0.00187 0.00162 0.00138 0.00148 0.00081 H27 1.44229 0.12688 0.51062 1.00000 0.04494 0.00000 0.00000 C28 1.36155 0.23413 0.64993 1.00000 0.02773 0.03537 0.04151 0.00638 -0.00853 -0.00215 0.03613 0.00673 0.00031 0.00033 0.00032 0.00000 0.00169 0.00183 0.00198 0.00152 0.00146 0.00136 0.00079 H28 1.40302 0.31309 0.66476 1.00000 0.04336 0.00000 0.00000 N1 0.76833 0.41530 0.78269 1.00000 0.01739 0.02321 0.02813 -0.00290 0.00599 -0.00465 0.02410 0.00530 0.00023 0.00025 0.00023 0.00000 0.00122 0.00129 0.00137 0.00106 0.00103 0.00102 0.00055 N2 1.00764 0.35715 0.59993 1.00000 0.02014 0.02084 0.02565 -0.00239 0.00681 -0.00099 0.02310 0.00520 0.00023 0.00024 0.00022 0.00000 0.00124 0.00125 0.00131 0.00103 0.00101 0.00100 0.00053 O1 0.62727 0.61041 1.00161 1.00000 0.02293 0.02797 0.03407 -0.00469 0.01230 -0.00284 0.02953 0.00421 0.00019 0.00020 0.00020 0.00000 0.00110 0.00113 0.00122 0.00093 0.00092 0.00086 0.00050 H1 0.55904 0.60468 1.02545 1.00000 0.04429 0.00000 0.00000 O2 0.56218 0.42656 0.88907 1.00000 0.01992 0.02928 0.03512 -0.00487 0.00829 -0.00554 0.02972 0.00413 0.00019 0.00020 0.00020 0.00000 0.00105 0.00115 0.00124 0.00095 0.00091 0.00086 0.00050 O3 0.84875 0.23240 0.62089 1.00000 0.03039 0.02663 0.03712 -0.00761 0.01260 -0.00769 0.03321 0.00427 0.00021 0.00020 0.00020 0.00000 0.00120 0.00116 0.00130 0.00097 0.00100 0.00092 0.00054 Fe1 1.20966 0.17515 0.53760 1.00000 0.02139 0.02951 0.02195 -0.00027 0.00238 0.00428 0.02508 0.00084 0.00004 0.00004 0.00004 0.00000 0.00025 0.00026 0.00024 0.00018 0.00017 0.00017 0.00015 H1N 0.72493 0.36074 0.75756 1.00000 0.03433 0.08412 0.00371 0.00375 0.00351 0.00000 0.01081 H2N 1.04495 0.42154 0.62253 1.00000 0.03793 0.08471 0.00369 0.00390 0.00349 0.00000 0.01108 C29 0.45698 0.92542 0.19461 1.00000 0.02806 0.03705 0.03560 0.01226 0.00845 0.00375 0.03253 0.00706 0.00031 0.00032 0.00030 0.00000 0.00167 0.00179 0.00181 0.00146 0.00138 0.00134 0.00072 H29 0.53368 0.89128 0.22177 1.00000 0.03904 0.00000 0.00000 Cl1 0.34131 0.88610 0.27251 1.00000 0.02532 0.03286 0.03547 0.00418 0.00721 -0.00242 0.03156 0.00156 0.00007 0.00007 0.00007 0.00000 0.00039 0.00041 0.00043 0.00032 0.00031 0.00030 0.00020 Cl2 0.47958 1.08752 0.22162 1.00000 0.05620 0.03970 0.06378 0.01746 0.00581 -0.01298 0.05281 0.00208 0.00010 0.00009 0.00010 0.00000 0.00062 0.00052 0.00067 0.00047 0.00050 0.00044 0.00028 Cl3 0.42166 0.86299 0.04750 1.00000 0.07794 0.05314 0.03198 0.00981 0.01280 0.02147 0.05332 0.00232 0.00011 0.00010 0.00008 0.00000 0.00076 0.00059 0.00049 0.00042 0.00047 0.00052 0.00029 Final Structure Factor Calculation for 02SOT077 in P-1 Total number of l.s. parameters = 382 Maximum vector length = 511 Memory required = 4161 / 25039 wR2 = 0.1542 before cycle 5 for 6433 data and 0 / 382 parameters Disagreeable restraints before cycle 5 Observed Target Error Sigma Restraint 0.0074 0.0010 ISOR U23 C30 -0.0110 0.0010 ISOR U12 C30 Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 6. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.006 0.000 GooF = S = 1.029; Restrained GooF = 1.043 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0799 * P )^2 + 2.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0551 for 5023 Fo > 4sig(Fo) and 0.0746 for all 6433 data wR2 = 0.1542, GooF = S = 1.029, Restrained GooF = 1.043 for all data Occupancy sum of asymmetric unit = 41.00 for non-hydrogen and 27.00 for hydrogen atoms Principal mean square atomic displacements U 0.0367 0.0347 0.0143 O5 0.0615 0.0347 0.0092 O4 0.0639 0.0529 0.0360 C30 0.0315 0.0194 0.0177 C1 0.0250 0.0198 0.0173 C2 0.0235 0.0194 0.0189 C3 0.0282 0.0188 0.0179 C4 0.0326 0.0224 0.0199 C5 0.0270 0.0201 0.0176 C6 0.0286 0.0234 0.0228 C7 0.0399 0.0293 0.0207 C8 0.0449 0.0308 0.0191 C9 0.0421 0.0314 0.0187 C10 0.0309 0.0249 0.0208 C11 0.0272 0.0179 0.0162 C12 0.0295 0.0251 0.0200 C13 0.0429 0.0334 0.0196 C14 0.0565 0.0383 0.0159 C15 0.0546 0.0391 0.0190 C16 0.0345 0.0276 0.0255 C17 0.0297 0.0208 0.0191 C18 0.0332 0.0205 0.0189 C19 0.0417 0.0230 0.0189 C20 0.0532 0.0236 0.0189 C21 0.0542 0.0267 0.0195 C22 0.0364 0.0270 0.0248 C23 0.0474 0.0291 0.0206 C24 0.0369 0.0294 0.0257 C25 0.0518 0.0246 0.0241 C26 0.0564 0.0354 0.0205 C27 0.0504 0.0366 0.0214 C28 0.0389 0.0194 0.0140 N1 0.0348 0.0183 0.0162 N2 0.0499 0.0221 0.0165 O1 0.0503 0.0227 0.0162 O2 0.0580 0.0232 0.0185 O3 0.0349 0.0215 0.0188 Fe1 0.0408 0.0321 0.0248 C29 0.0408 0.0315 0.0224 Cl1 0.0688 0.0621 0.0275 Cl2 0.0858 0.0441 0.0301 Cl3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.012 0.023 0.033 0.046 0.060 0.075 0.095 0.123 0.177 1.000 Number in group 692. 646. 591. 674. 634. 627. 647. 643. 630. 649. GooF 0.860 1.014 1.055 1.042 1.118 1.047 1.076 1.058 0.990 1.035 K 1.893 0.945 0.992 0.986 0.983 0.981 0.997 1.003 1.029 1.039 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.98 1.05 1.16 1.32 1.66 inf Number in group 663. 632. 639. 641. 656. 629. 644. 639. 645. 645. GooF 0.890 0.845 0.899 0.909 0.919 0.950 0.965 0.988 1.210 1.531 K 1.068 1.042 1.033 1.007 1.013 1.004 1.036 1.032 1.032 1.028 R1 0.179 0.136 0.109 0.091 0.070 0.068 0.056 0.052 0.050 0.050 Recommended weighting scheme: WGHT 0.0823 1.9283 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) -3 3 4 224.38 105.93 5.46 0.055 1.89 1 -6 1 43.94 6.35 5.41 0.013 1.84 -3 3 3 768.20 1297.52 5.15 0.192 2.12 -1 0 3 92.13 207.98 4.99 0.077 3.80 -1 4 4 407.06 235.28 4.85 0.082 1.81 2 0 3 637.37 397.41 4.56 0.106 3.02 -4 -2 2 59.75 20.72 4.32 0.024 2.38 -4 2 0 42.13 107.03 4.27 0.055 2.52 -2 5 3 48.65 14.28 4.22 0.020 1.71 0 4 3 662.74 436.84 4.16 0.112 2.03 -3 -1 3 288.07 171.30 4.07 0.070 2.81 -1 -3 1 245.51 145.75 4.07 0.064 3.47 1 5 0 278.68 447.72 3.95 0.113 2.11 -1 5 1 488.40 321.32 3.85 0.096 2.05 5 0 5 18.66 0.17 3.84 0.002 1.52 0 -2 1 6.03 45.25 3.76 0.036 5.40 -6 0 2 521.17 347.14 3.73 0.099 1.81 -2 2 5 589.92 404.71 3.65 0.107 1.95 -5 2 4 226.16 358.11 3.65 0.101 1.72 3 -1 3 41.58 93.35 3.64 0.052 2.57 -1 -4 7 4.91 31.80 3.54 0.030 1.58 -2 6 2 740.81 522.37 3.54 0.122 1.61 -5 5 3 320.10 481.52 3.51 0.117 1.44 0 -3 1 60.96 119.13 3.51 0.058 3.70 -5 2 5 10.74 42.22 3.50 0.035 1.57 -5 -5 8 -1.11 19.12 3.47 0.023 1.19 0 6 0 393.41 267.11 3.45 0.087 1.81 -1 -1 2 302.25 198.79 3.43 0.075 5.20 -8 -7 5 -1.74 19.73 3.42 0.024 1.00 -3 3 5 159.81 95.86 3.35 0.052 1.69 -7 -9 8 93.16 183.62 3.34 0.072 0.88 1 -3 4 21.96 58.12 3.34 0.041 2.46 -5 3 1 10.89 39.50 3.32 0.034 1.91 -13 2 7 -36.66 91.03 3.31 0.051 0.78 -4 4 4 554.15 782.01 3.29 0.149 1.59 1 5 2 1959.80 1475.95 3.24 0.205 1.85 0 0 2 1278.40 944.43 3.24 0.164 5.82 -3 5 1 108.54 56.00 3.19 0.040 1.86 -5 -3 1 39.34 81.01 3.17 0.048 1.87 -8 -5 5 182.45 282.92 3.17 0.090 1.11 -1 5 0 285.71 416.06 3.15 0.109 2.16 0 6 1 292.46 425.46 3.14 0.110 1.73 -3 5 3 430.16 306.35 3.09 0.093 1.64 -4 6 1 276.52 188.97 3.07 0.073 1.52 -9 -4 4 115.49 189.60 3.06 0.073 1.09 -5 4 4 94.52 53.80 3.05 0.039 1.48 -4 -4 3 41.98 82.43 3.04 0.048 1.86 -11 5 5 101.55 177.65 3.04 0.071 0.87 -7 -5 7 40.33 79.86 2.98 0.048 1.11 -2 1 1 1482.30 1133.22 2.97 0.180 4.63 Bond lengths and angles O4 - Distance Angles C30 0.8231 (0.0047) H4 0.8400 109.44 O4 - C30 C30 - Distance Angles O4 0.8231 (0.0047) H30A 0.9800 109.45 H30B 0.9800 109.47 109.47 H30C 0.9800 109.50 109.47 109.47 C30 - O4 H30A H30B C1 - Distance Angles N1 1.3641 (0.0039) C2 1.3998 (0.0040) 107.96 (0.25) C5 1.4547 (0.0042) 117.57 (0.26) 134.35 (0.27) C1 - N1 C2 C2 - Distance Angles C1 1.3998 (0.0040) C3 1.4201 (0.0040) 106.59 (0.25) C6 1.4725 (0.0039) 128.94 (0.26) 124.46 (0.25) C2 - C1 C3 C3 - Distance Angles C4 1.4024 (0.0040) C2 1.4201 (0.0040) 106.86 (0.25) C12 1.4789 (0.0040) 126.84 (0.26) 126.29 (0.25) C3 - C4 C2 C4 - Distance Angles N1 1.3474 (0.0039) C3 1.4024 (0.0040) 108.15 (0.25) C18 1.4782 (0.0040) 117.89 (0.26) 133.93 (0.27) C4 - N1 C3 C5 - Distance Angles O2 1.2358 (0.0036) O1 1.3128 (0.0036) 123.85 (0.28) C1 1.4547 (0.0042) 120.76 (0.27) 115.39 (0.26) C5 - O2 O1 C6 - Distance Angles C11 1.3975 (0.0042) C7 1.4019 (0.0041) 118.56 (0.27) C2 1.4725 (0.0039) 119.90 (0.26) 121.44 (0.26) C6 - C11 C7 C7 - Distance Angles C8 1.3826 (0.0043) C6 1.4019 (0.0042) 120.54 (0.28) H7 0.9500 119.73 119.73 C7 - C8 C6 C8 - Distance Angles C7 1.3826 (0.0043) C9 1.3867 (0.0049) 120.33 (0.30) H8 0.9500 119.84 119.84 C8 - C7 C9 C9 - Distance Angles C8 1.3867 (0.0049) C10 1.3898 (0.0048) 119.67 (0.29) H9 0.9500 120.16 120.16 C9 - C8 C10 C10 - Distance Angles C11 1.3831 (0.0043) C9 1.3898 (0.0048) 120.24 (0.30) H10 0.9500 119.88 119.88 C10 - C11 C9 C11 - Distance Angles C10 1.3831 (0.0043) C6 1.3975 (0.0042) 120.64 (0.29) H11 0.9500 119.68 119.68 C11 - C10 C6 C12 - Distance Angles C17 1.3907 (0.0043) C13 1.3995 (0.0042) 118.63 (0.27) C3 1.4789 (0.0040) 121.05 (0.27) 120.32 (0.26) C12 - C17 C13 C13 - Distance Angles C14 1.3821 (0.0044) C12 1.3995 (0.0042) 120.70 (0.29) H13 0.9500 119.65 119.65 C13 - C14 C12 C14 - Distance Angles C15 1.3796 (0.0050) C13 1.3821 (0.0044) 119.93 (0.31) H14 0.9500 120.04 120.04 C14 - C15 C13 C15 - Distance Angles C16 1.3786 (0.0052) C14 1.3796 (0.0050) 120.27 (0.31) H15 0.9500 119.86 119.86 C15 - C16 C14 C16 - Distance Angles C15 1.3786 (0.0052) C17 1.3904 (0.0047) 120.11 (0.32) H16 0.9500 119.95 119.95 C16 - C15 C17 C17 - Distance Angles C16 1.3904 (0.0047) C12 1.3907 (0.0043) 120.36 (0.31) H17 0.9500 119.82 119.82 C17 - C16 C12 C18 - Distance Angles O3 1.2283 (0.0036) N2 1.3464 (0.0040) 123.36 (0.28) C4 1.4782 (0.0040) 120.50 (0.27) 116.12 (0.26) C18 - O3 N2 C19 - Distance Angles N2 1.4064 (0.0038) C23 1.4148 (0.0045) 123.74 (0.28) C20 1.4283 (0.0043) 127.24 (0.28) 109.02 (0.27) Fe1 2.0632 (0.0030) 127.53 (0.22) 69.38 (0.18) 69.55 (0.17) C19 - N2 C23 C20 C20 - Distance Angles C21 1.4207 (0.0045) C19 1.4283 (0.0043) 106.83 (0.29) Fe1 2.0586 (0.0031) 68.44 (0.18) 69.90 (0.17) H20 0.9500 126.58 126.58 126.63 C20 - C21 C19 Fe1 C21 - Distance Angles C20 1.4207 (0.0045) C22 1.4214 (0.0052) 108.86 (0.29) Fe1 2.0264 (0.0031) 70.87 (0.18) 69.69 (0.18) H21 0.9500 125.57 125.57 125.45 C21 - C20 C22 Fe1 C22 - Distance Angles C21 1.4214 (0.0052) C23 1.4281 (0.0047) 107.70 (0.29) Fe1 2.0316 (0.0034) 69.30 (0.19) 70.21 (0.18) H22 0.9500 126.15 126.15 125.91 C22 - C21 C23 Fe1 C23 - Distance Angles C19 1.4148 (0.0045) C22 1.4281 (0.0047) 107.59 (0.29) Fe1 2.0499 (0.0033) 70.39 (0.18) 68.83 (0.19) H23 0.9500 126.21 126.21 126.14 C23 - C19 C22 Fe1 C24 - Distance Angles C25 1.4176 (0.0047) C28 1.4230 (0.0053) 107.74 (0.30) Fe1 2.0497 (0.0033) 69.45 (0.18) 69.37 (0.19) H24 0.9500 126.13 126.13 126.62 C24 - C25 C28 Fe1 C25 - Distance Angles C26 1.4113 (0.0049) C24 1.4176 (0.0047) 108.48 (0.31) Fe1 2.0423 (0.0033) 69.79 (0.20) 70.01 (0.19) H25 0.9500 125.76 125.76 126.02 C25 - C26 C24 Fe1 C26 - Distance Angles C27 1.4098 (0.0054) C25 1.4113 (0.0049) 108.37 (0.30) Fe1 2.0422 (0.0034) 69.30 (0.20) 69.79 (0.19) H26 0.9500 125.82 125.82 126.67 C26 - C27 C25 Fe1 C27 - Distance Angles C26 1.4098 (0.0054) C28 1.4339 (0.0052) 107.85 (0.32) Fe1 2.0305 (0.0033) 70.20 (0.19) 69.83 (0.19) H27 0.9500 126.07 126.07 125.49 C27 - C26 C28 Fe1 C28 - Distance Angles C24 1.4230 (0.0053) C27 1.4339 (0.0052) 107.56 (0.31) Fe1 2.0422 (0.0033) 69.93 (0.19) 68.95 (0.19) H28 0.9500 126.22 126.22 126.46 C28 - C24 C27 Fe1 N1 - Distance Angles C4 1.3474 (0.0039) C1 1.3641 (0.0039) 110.42 (0.25) H1N 0.7498 (0.0417) 121.93 (3.15) 127.64 (3.16) N1 - C4 C1 N2 - Distance Angles C18 1.3464 (0.0040) C19 1.4064 (0.0038) 126.90 (0.27) H2N 0.7944 (0.0425) 119.82 (2.98) 112.92 (2.99) N2 - C18 C19 O1 - Distance Angles C5 1.3128 (0.0036) H1 0.8400 109.47 O1 - C5 O2 - Distance Angles C5 1.2358 (0.0036) O2 - O3 - Distance Angles C18 1.2283 (0.0036) O3 - Fe1 - Distance Angles C21 2.0264 (0.0031) C27 2.0305 (0.0033) 120.45 (0.14) C22 2.0316 (0.0034) 41.01 (0.15) 106.20 (0.14) C28 2.0422 (0.0033) 157.89 (0.15) 41.23 (0.15) 122.71 (0.15) C26 2.0422 (0.0034) 105.41 (0.13) 40.50 (0.15) 121.51 (0.14) 68.49 (0.14) C25 2.0423 (0.0033) 121.62 (0.14) 68.34 (0.15) 157.68 (0.14) 68.35 (0.14) 40.43 (0.14) C24 2.0497 (0.0033) 158.68 (0.15) 68.79 (0.14) 159.70 (0.15) 40.70 (0.15) 68.25 (0.13) 40.54 (0.13) C23 2.0499 (0.0033) 68.73 (0.14) 123.72 (0.14) 40.96 (0.13) 108.93 (0.14) 158.96 (0.14) 159.81 (0.13) 124.34 (0.13) C20 2.0586 (0.0031) 40.69 (0.13) 156.30 (0.14) 68.83 (0.14) 160.70 (0.14) 120.94 (0.14) 107.00 (0.14) 123.72 (0.14) C19 2.0632 (0.0030) 68.02 (0.12) 160.96 (0.14) 68.14 (0.12) 125.31 (0.13) 158.08 (0.14) 123.81 (0.13) 109.85 (0.13) Fe1 - C21 C27 C22 C28 C26 C25 C24 C29 - Distance Angles Cl3 1.7522 (0.0036) Cl1 1.7541 (0.0033) 110.93 (0.19) Cl2 1.7703 (0.0036) 111.00 (0.19) 109.20 (0.19) H29 1.0000 108.55 108.55 108.55 C29 - Cl3 Cl1 Cl2 Cl1 - Distance Angles C29 1.7541 (0.0033) Cl1 - Cl2 - Distance Angles C29 1.7703 (0.0036) Cl2 - Cl3 - Distance Angles C29 1.7522 (0.0036) Cl3 - FMAP and GRID set by program FMAP 2 1 28 GRID -2.000 -2 -2 2.000 2 2 R1 = 0.0726 for 6433 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.55 at 0.4506 0.5365 0.5680 [ 0.30 A from H30B ] Deepest hole -0.58 at 0.4852 0.3342 0.4061 [ 0.15 A from H30A ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 3991 / 28007 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 1.5071 0.5872 0.5118 1.00000 0.05 1.41 0.77 H30C 0.89 C30 1.04 H30A 1.40 H30C Q2 1 1.5532 0.5969 0.5891 1.00000 0.05 1.24 0.49 C30 0.75 O4 0.89 H30A 1.05 H30C Q3 1 0.5193 1.0431 0.1618 1.00000 0.05 0.80 0.94 CL2 1.60 C29 1.98 H29 2.33 CL3 Q4 1 1.5514 0.5893 0.6727 1.00000 0.05 0.62 0.48 O4 1.10 C30 1.24 H4 1.51 H30A Q5 1 1.5732 0.5265 0.6203 1.00000 0.05 0.56 0.43 H4 0.46 O4 0.97 C30 1.33 H30C Q6 1 0.3626 0.8054 0.0391 1.00000 0.05 0.49 0.88 CL3 2.19 C29 2.73 H29 2.79 CL1 Q7 1 1.2348 0.7651 0.6608 1.00000 0.05 0.38 1.01 H16 1.34 C16 2.00 C15 2.18 H15 Q8 1 1.0360 0.3177 0.5598 1.00000 0.05 0.36 0.69 N2 0.72 C19 1.23 H2N 1.85 C18 Q9 1 0.9165 0.4796 0.7864 1.00000 0.05 0.36 0.67 C3 0.76 C4 1.76 N1 1.76 C2 Q10 1 1.0536 0.2417 0.5168 1.00000 0.05 0.35 0.41 C19 1.07 C20 1.59 N2 1.68 C23 Q11 1 0.7049 0.5131 0.8952 1.00000 0.05 0.35 0.65 C1 0.82 C5 1.77 N1 1.80 O1 Q12 1 1.0970 0.5576 0.7973 1.00000 0.05 0.31 0.53 C12 0.90 C13 1.61 H13 1.69 C17 Q13 1 0.8979 0.5801 0.8424 1.00000 0.05 0.31 0.73 C2 0.73 C3 1.83 C1 1.84 C4 Q14 1 0.2753 0.9904 0.3644 1.00000 0.05 0.30 1.67 CL1 1.92 H21 2.07 H26 2.32 C21 Q15 1 0.7541 0.4673 0.8368 1.00000 0.05 0.30 0.58 C1 0.81 N1 1.36 H1N 1.73 C5 Q16 1 1.1620 0.7784 0.8804 1.00000 0.05 0.30 1.55 C16 1.65 C17 2.01 H16 2.14 H17 Q17 1 1.2429 0.6841 0.7249 1.00000 0.05 0.29 0.86 C15 0.87 C16 1.50 H15 1.52 H16 Q18 1 1.2389 0.1342 0.5950 1.00000 0.05 0.29 0.94 FE1 1.15 C25 1.38 C26 1.40 C24 Q19 1 1.1383 0.1985 0.7624 1.00000 0.05 0.29 1.15 H24 1.61 C24 2.02 H25 2.04 C25 Q20 1 0.8872 0.4411 0.7228 1.00000 0.05 0.29 0.36 C4 1.38 C3 1.40 C18 1.61 N1 Shortest distances between peaks (including symmetry equivalents) 9 20 0.82 4 5 0.89 8 10 0.93 2 5 0.96 1 2 1.00 11 15 1.00 2 4 1.03 9 13 1.22 7 17 1.30 1 5 1.71 13 20 1.87 1 1 1.90 1 5 1.92 1 4 1.94 9 15 1.96 13 15 1.98 15 20 2.10 9 12 2.13 1 2 2.19 16 17 2.23 12 13 2.34 18 19 2.38 11 13 2.42 12 17 2.44 12 16 2.50 12 20 2.60 10 18 2.62 1 4 2.64 6 16 2.74 9 11 2.80 2 5 2.80 7 16 2.81 2 2 2.82 8 20 2.85 14 18 2.96 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. 0.44: 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 1.83: Structure factors and derivatives 9.25: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.44: Solve l.s. equations 0.00: Generate HTAB table 0.06: Other dependent quantities, CIF, tables 0.27: Analysis of variance 0.06: Merge reflections for Fourier and .fcf 0.16: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 11:58:01 Total elapsed time: 12.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++