+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 11:36:05 on 29-May-2002 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 02SOT050 IN P-1 CELL 0.71073 9.3589 16.0760 17.6270 86.856 89.616 84.448 ZERR 4.00 0.0007 0.0020 0.0030 0.012 0.012 0.009 LATT 1 SFAC C FE N O H UNIT 140 4 12 8 116 V = 2635.63 F(000) = 1208.0 Mu = 0.61 mm-1 Cell Wt = 2317.85 Rho = 1.460 MERG 0 SHEL 7 0.87 omit 5 16 6 OMIT -3 -1 4 OMIT 5 -2 4 OMIT 2 10 -1 OMIT -1 7 -2 OMIT 0 7 4 OMIT 6 -2 1 OMIT 1 -7 2 OMIT 1 2 6 OMIT -1 -2 -6 OMIT 7 -6 -5 OMIT 0 -7 -4 OMIT 5 10 2 OMIT -5 -10 -2 OMIT -3 -10 3 OMIT -4 -14 3 OMIT 3 10 -3 OMIT -2 -10 -1 OMIT 4 10 0 OMIT -4 -10 0 OMIT 2 10 1 OMIT 5 -7 0 OMIT 4 7 4 OMIT -4 -14 -10 OMIT -3 -14 -2 OMIT -5 2 2 OMIT 3 16 7 OMIT 6 9 13 OMIT -5 -2 -3 HTAB N2 O1_$1 EQIV $1 -x+2, -y, -z HTAB N5 O3_$2 EQIV $2 -x+1, -y+1, -z+1 FMAP 2 HTAB PLAN 20 SIZE 0.10 0.15 0.25 ACTA L.S. 4 TEMP -153.00 WGHT 0.057400 9.050400 BASF 0.44516 FVAR 1.14430 MOLE 1 FE1 2 0.804529 0.016610 0.369386 11.00000 0.01524 0.01984 = 0.01454 -0.00058 0.00306 -0.00088 N1 3 0.766378 -0.017887 0.167349 11.00000 0.01119 0.02293 = 0.01287 -0.00093 0.00228 0.00496 AFIX 43 H1 5 0.683940 0.008209 0.180923 11.00000 -1.20000 AFIX 0 N2 3 0.792589 0.089623 -0.017582 11.00000 0.00711 0.01755 = 0.01073 -0.00438 0.00204 -0.00092 AFIX 43 H2 5 0.879718 0.073393 -0.033390 11.00000 -1.20000 AFIX 0 N3 3 0.609545 0.181417 -0.181103 11.00000 0.00887 0.02522 = 0.01140 0.00064 0.00222 -0.00151 AFIX 43 H3 5 0.526461 0.179520 -0.157717 11.00000 -1.20000 AFIX 0 O1 4 0.944114 -0.022134 0.081152 11.00000 0.01929 0.03391 = 0.02146 0.01027 0.00979 0.00875 O2 4 0.849767 0.172982 -0.158688 11.00000 0.01736 0.02671 = 0.01415 0.00218 0.00239 -0.00049 C1 1 0.660840 0.117842 0.344583 11.00000 0.02253 0.02701 = 0.02521 0.00012 0.00115 0.00954 AFIX 43 H1 5 0.666913 0.158316 0.303641 11.00000 -1.20000 AFIX 0 C2 1 0.716959 0.121921 0.417995 11.00000 0.02186 0.02448 = 0.02723 -0.01071 0.00305 0.00753 AFIX 43 H2 5 0.767879 0.165561 0.435303 11.00000 -1.20000 AFIX 0 C3 1 0.684368 0.049931 0.461306 11.00000 0.01710 0.03683 = 0.02026 -0.00200 0.00376 -0.00089 AFIX 43 H3 5 0.708971 0.036757 0.513067 11.00000 -1.20000 AFIX 0 C4 1 0.608157 0.000290 0.414111 11.00000 0.02008 0.02914 = 0.03020 -0.00431 0.00895 -0.00067 AFIX 43 H4 5 0.573453 -0.051941 0.428409 11.00000 -1.20000 AFIX 0 C5 1 0.593906 0.042971 0.342513 11.00000 0.01465 0.04114 = 0.02334 -0.00764 -0.00128 0.00890 AFIX 43 H5 5 0.547006 0.024534 0.299762 11.00000 -1.20000 AFIX 0 C6 1 0.965379 0.019847 0.291745 11.00000 0.01412 0.02483 = 0.01733 0.00100 0.00256 -0.00214 AFIX 43 H6 5 0.972342 0.061520 0.251903 11.00000 -1.20000 AFIX 0 C7 1 1.020504 0.022070 0.365659 11.00000 0.01633 0.02563 = 0.02304 -0.00377 0.00352 -0.00377 AFIX 43 H7 5 1.071614 0.065101 0.384001 11.00000 -1.20000 AFIX 0 C8 1 0.986781 -0.050538 0.407719 11.00000 0.01847 0.02555 = 0.01255 0.00052 0.00114 0.00430 AFIX 43 H8 5 1.010228 -0.064829 0.459454 11.00000 -1.20000 AFIX 0 C9 1 0.911405 -0.098599 0.358923 11.00000 0.02051 0.01383 = 0.01547 0.00197 -0.00211 0.00572 AFIX 43 H9 5 0.876111 -0.150925 0.372182 11.00000 -1.20000 AFIX 0 C10 1 0.898147 -0.054420 0.286617 11.00000 0.01333 0.01765 = 0.01369 0.00094 0.00436 0.00443 C11 1 0.832393 -0.084316 0.217710 11.00000 0.01673 0.01611 = 0.01344 0.00198 -0.00131 0.00319 AFIX 23 H11A 5 0.907542 -0.117431 0.189344 11.00000 -1.20000 H11B 5 0.758895 -0.121997 0.233845 11.00000 -1.20000 AFIX 0 C12 1 0.824651 0.005967 0.100868 11.00000 0.01424 0.01444 = 0.01349 -0.00231 0.00072 -0.00076 C13 1 0.735013 0.065879 0.050757 11.00000 0.01222 0.01630 = 0.01296 -0.00203 0.00198 -0.00607 C14 1 0.597828 0.104864 0.055226 11.00000 0.01555 0.01091 = 0.01236 -0.00131 -0.00025 -0.00336 C15 1 0.571529 0.154079 -0.013049 11.00000 0.01241 0.01200 = 0.01537 -0.00196 0.00190 -0.00311 C16 1 0.694401 0.142102 -0.057189 11.00000 0.01269 0.01335 = 0.01089 -0.00028 0.00024 -0.00102 C17 1 0.728236 0.168125 -0.136348 11.00000 0.01500 0.00963 = 0.01963 -0.00069 0.00531 0.00014 C18 1 0.603572 0.197964 -0.260914 11.00000 0.02122 0.01365 = 0.01457 0.00010 -0.00256 -0.00349 C19 1 0.475047 0.234597 -0.290386 11.00000 0.02422 0.02470 = 0.01523 -0.00156 0.00059 0.00207 AFIX 43 H19 5 0.397690 0.249609 -0.257108 11.00000 -1.20000 AFIX 0 C20 1 0.457721 0.249662 -0.367763 11.00000 0.02669 0.02738 = 0.02317 0.00004 -0.00827 0.00608 AFIX 43 H20 5 0.369021 0.274918 -0.387868 11.00000 -1.20000 AFIX 0 C21 1 0.570610 0.227633 -0.415507 11.00000 0.02901 0.03069 = 0.01358 0.00040 -0.00443 -0.00216 AFIX 43 H21 5 0.560217 0.238179 -0.468839 11.00000 -1.20000 AFIX 0 C22 1 0.697550 0.190627 -0.386264 11.00000 0.02486 0.02772 = 0.01782 -0.00690 0.00088 -0.00223 AFIX 43 H22 5 0.774764 0.175557 -0.419613 11.00000 -1.20000 AFIX 0 C23 1 0.715118 0.174827 -0.308827 11.00000 0.01335 0.02079 = 0.01724 -0.00165 0.00117 0.00179 AFIX 43 H23 5 0.803167 0.148316 -0.288991 11.00000 -1.20000 AFIX 0 C24 1 0.494463 0.103032 0.118628 11.00000 0.00606 0.01741 = 0.01635 0.00245 -0.00407 -0.00173 C25 1 0.472346 0.170745 0.164461 11.00000 0.02101 0.01233 = 0.01671 -0.00112 0.00452 -0.00610 AFIX 43 H25 5 0.527138 0.217196 0.156326 11.00000 -1.20000 AFIX 0 C26 1 0.370896 0.170785 0.221868 11.00000 0.01957 0.01809 = 0.02110 -0.00569 0.00652 0.00402 AFIX 43 H26 5 0.356774 0.217125 0.253196 11.00000 -1.20000 AFIX 0 C27 1 0.290597 0.104322 0.233815 11.00000 0.01680 0.02467 = 0.01870 -0.00007 0.00857 0.00164 AFIX 43 H27 5 0.221416 0.104502 0.273507 11.00000 -1.20000 AFIX 0 C28 1 0.310264 0.037640 0.188429 11.00000 0.01918 0.02438 = 0.02885 0.00181 0.00606 -0.01009 AFIX 43 H28 5 0.254103 -0.008229 0.196438 11.00000 -1.20000 AFIX 0 C29 1 0.411198 0.036945 0.131256 11.00000 0.01852 0.01807 = 0.02415 -0.00490 0.00380 -0.00537 AFIX 43 H29 5 0.423917 -0.009527 0.100020 11.00000 -1.20000 AFIX 0 C30 1 0.306611 0.169377 -0.032049 11.00000 0.01970 0.01991 = 0.01749 0.00079 -0.00102 -0.00169 AFIX 43 H30 5 0.305603 0.111481 -0.018229 11.00000 -1.20000 AFIX 0 C31 1 0.180101 0.216489 -0.050969 11.00000 0.01649 0.02466 = 0.01625 -0.00195 0.00105 -0.00522 AFIX 43 H31 5 0.092847 0.190814 -0.051054 11.00000 -1.20000 AFIX 0 C32 1 0.179565 0.301197 -0.069883 11.00000 0.01926 0.03066 = 0.01366 -0.00681 -0.00264 0.00712 AFIX 43 H32 5 0.092126 0.334055 -0.082274 11.00000 -1.20000 AFIX 0 C33 1 0.306703 0.337269 -0.070558 11.00000 0.02369 0.01994 = 0.01146 0.00130 -0.00153 0.00030 AFIX 43 H33 5 0.306875 0.395341 -0.083814 11.00000 -1.20000 AFIX 0 C34 1 0.434685 0.290098 -0.052166 11.00000 0.01126 0.02018 = 0.01483 -0.00085 -0.00039 -0.00297 AFIX 43 H34 5 0.521702 0.316050 -0.052814 11.00000 -1.20000 AFIX 0 C35 1 0.436643 0.205448 -0.032860 11.00000 0.01160 0.01695 = 0.00915 -0.00200 0.00069 -0.00089 MOLE 2 FE2 2 0.211463 0.495421 0.138532 11.00000 0.01761 0.01675 = 0.01264 0.00007 0.00221 -0.00398 N4 3 0.324570 0.559828 0.320003 11.00000 0.00910 0.03174 = 0.01118 -0.00439 0.00192 -0.00070 AFIX 43 H4A 5 0.233665 0.571821 0.307667 11.00000 -1.20000 AFIX 0 N5 3 0.312407 0.598605 0.520445 11.00000 0.00777 0.02176 = 0.01235 -0.00191 -0.00187 -0.00008 AFIX 43 H5A 5 0.401360 0.583475 0.534947 11.00000 -1.20000 AFIX 0 N6 3 0.138999 0.679343 0.687726 11.00000 0.00861 0.02637 = 0.01016 -0.00259 -0.00205 -0.00064 AFIX 43 H6A 5 0.052750 0.684255 0.667417 11.00000 -1.20000 AFIX 0 O3 4 0.488633 0.534193 0.412443 11.00000 0.01324 0.03230 = 0.01223 -0.00127 -0.00001 0.00475 O4 4 0.372342 0.638689 0.663698 11.00000 0.01230 0.04026 = 0.01660 -0.00610 -0.00050 -0.00120 C36 1 0.182580 0.392615 0.205961 11.00000 0.03215 0.02246 = 0.02339 0.00558 -0.00093 -0.00669 AFIX 43 H36 5 0.247309 0.367628 0.243815 11.00000 -1.20000 AFIX 0 C37 1 0.183133 0.373170 0.129469 11.00000 0.03598 0.01372 = 0.02576 -0.00153 0.00529 -0.00381 AFIX 43 H37 5 0.248524 0.333217 0.106348 11.00000 -1.20000 AFIX 0 C38 1 0.070125 0.423109 0.093124 11.00000 0.03201 0.02621 = 0.02169 -0.00253 0.00312 -0.01440 AFIX 43 H38 5 0.045340 0.422804 0.040971 11.00000 -1.20000 AFIX 0 C39 1 -0.000275 0.473743 0.147108 11.00000 0.01470 0.02254 = 0.03461 0.00145 0.00000 -0.01060 AFIX 43 H39 5 -0.081121 0.513411 0.137885 11.00000 -1.20000 AFIX 0 C40 1 0.070113 0.455350 0.217351 11.00000 0.03151 0.02456 = 0.01934 -0.00139 0.00968 -0.01371 AFIX 43 H40 5 0.046049 0.480642 0.263791 11.00000 -1.20000 AFIX 0 C41 1 0.421957 0.508883 0.120097 11.00000 0.01414 0.02224 = 0.01752 0.00073 0.00607 0.00385 AFIX 43 H41 5 0.498164 0.465288 0.120729 11.00000 -1.20000 AFIX 0 C42 1 0.339527 0.539886 0.055986 11.00000 0.02017 0.02685 = 0.01030 -0.00139 0.00498 -0.00633 AFIX 43 H42 5 0.349926 0.520528 0.006102 11.00000 -1.20000 AFIX 0 C43 1 0.238653 0.604945 0.079312 11.00000 0.01789 0.02160 = 0.01856 0.00819 0.00034 -0.00914 AFIX 43 H43 5 0.169445 0.636860 0.047697 11.00000 -1.20000 AFIX 0 C44 1 0.258521 0.614233 0.157458 11.00000 0.01690 0.01508 = 0.01801 -0.00315 0.00541 -0.00282 AFIX 43 H44 5 0.205643 0.653834 0.187470 11.00000 -1.20000 AFIX 0 C45 1 0.371065 0.554275 0.183598 11.00000 0.01314 0.01923 = 0.01445 -0.00112 0.00051 -0.00681 C46 1 0.430563 0.541074 0.261937 11.00000 0.01586 0.03584 = 0.01226 -0.00280 0.00330 -0.00234 AFIX 23 H46A 5 0.471145 0.482076 0.269958 11.00000 -1.20000 H46B 5 0.509775 0.576978 0.267017 11.00000 -1.20000 AFIX 0 C47 1 0.365385 0.558865 0.392693 11.00000 0.01606 0.01886 = 0.01346 -0.00045 0.00215 -0.00511 C48 1 0.260105 0.591282 0.449199 11.00000 0.01718 0.01712 = 0.00872 0.00110 -0.00077 -0.00580 C49 1 0.115547 0.619515 0.449579 11.00000 0.01282 0.01227 = 0.01197 0.00313 0.00042 -0.00384 C50 1 0.081776 0.646040 0.523460 11.00000 0.01576 0.00910 = 0.01335 0.00008 0.00410 -0.00264 C51 1 0.207519 0.632441 0.565204 11.00000 0.00980 0.01532 = 0.00950 -0.00074 0.00090 0.00163 C52 1 0.248300 0.650275 0.642985 11.00000 0.01149 0.01544 = 0.01622 0.00015 -0.00023 -0.00376 C53 1 0.147781 0.702732 0.763493 11.00000 0.01580 0.01715 = 0.01125 -0.00294 -0.00045 -0.00781 C54 1 0.255142 0.668972 0.812182 11.00000 0.01539 0.02404 = 0.01728 0.00173 -0.00034 -0.00444 AFIX 43 H54 5 0.329168 0.629619 0.795243 11.00000 -1.20000 AFIX 0 C55 1 0.253162 0.693511 0.886439 11.00000 0.02091 0.03160 = 0.01506 -0.00043 -0.00352 -0.01190 AFIX 43 H55 5 0.327178 0.670751 0.920299 11.00000 -1.20000 AFIX 0 C56 1 0.146686 0.749939 0.912121 11.00000 0.03534 0.02439 = 0.00833 -0.00345 0.00378 -0.01480 AFIX 43 H56 5 0.146778 0.765730 0.963270 11.00000 -1.20000 AFIX 0 C57 1 0.039634 0.783466 0.862980 11.00000 0.03064 0.01967 = 0.02156 -0.00529 0.00529 -0.00384 AFIX 43 H57 5 -0.034237 0.822817 0.880079 11.00000 -1.20000 AFIX 0 C58 1 0.039979 0.759752 0.788884 11.00000 0.02273 0.02162 = 0.01685 0.00186 -0.00032 -0.00036 AFIX 43 H58 5 -0.034109 0.782661 0.755130 11.00000 -1.20000 AFIX 0 C59 1 0.018700 0.674342 0.322893 11.00000 0.01408 0.01384 = 0.01561 0.00071 0.00219 -0.00197 AFIX 43 H59 5 0.091383 0.711739 0.319336 11.00000 -1.20000 AFIX 0 C60 1 -0.077795 0.674014 0.263955 11.00000 0.01932 0.01718 = 0.01413 0.00482 0.00182 0.00352 AFIX 43 H60 5 -0.070503 0.710198 0.219938 11.00000 -1.20000 AFIX 0 C61 1 -0.184308 0.620953 0.269538 11.00000 0.01680 0.02685 = 0.01141 -0.00312 -0.00436 0.00095 AFIX 43 H61 5 -0.249546 0.619499 0.228680 11.00000 -1.20000 AFIX 0 C62 1 -0.197201 0.569550 0.334363 11.00000 0.01054 0.02455 = 0.02082 -0.00147 0.00359 -0.00409 AFIX 43 H62 5 -0.273126 0.534394 0.338765 11.00000 -1.20000 AFIX 0 C63 1 -0.100148 0.569596 0.392052 11.00000 0.01221 0.01782 = 0.01360 -0.00034 0.00169 0.00259 AFIX 43 H63 5 -0.108787 0.533918 0.436285 11.00000 -1.20000 AFIX 0 C64 1 0.011507 0.621390 0.386816 11.00000 0.00991 0.01378 = 0.01072 -0.00269 0.00144 0.00227 C65 1 -0.161789 0.631075 0.578804 11.00000 0.01547 0.02470 = 0.02031 0.00069 0.00216 -0.00146 AFIX 43 H65 5 -0.135525 0.572811 0.587783 11.00000 -1.20000 AFIX 0 C66 1 -0.298152 0.664192 0.597297 11.00000 0.01423 0.03984 = 0.01837 -0.00271 0.00379 -0.00135 AFIX 43 H66 5 -0.365345 0.628518 0.618105 11.00000 -1.20000 AFIX 0 C67 1 -0.337350 0.748351 0.585822 11.00000 0.01283 0.04507 = 0.01939 -0.01474 0.00072 0.00813 AFIX 43 H67 5 -0.431130 0.771127 0.598971 11.00000 -1.20000 AFIX 0 C68 1 -0.239348 0.799798 0.554973 11.00000 0.02598 0.02423 = 0.03730 -0.00618 -0.00606 0.01131 AFIX 43 H68 5 -0.265618 0.858181 0.546975 11.00000 -1.20000 AFIX 0 C69 1 -0.103559 0.766397 0.535824 11.00000 0.01894 0.02256 = 0.02394 0.00049 -0.00046 -0.00050 AFIX 43 H69 5 -0.037150 0.802209 0.514407 11.00000 -1.20000 AFIX 0 C70 1 -0.062169 0.681705 0.547208 11.00000 0.01487 0.02072 = 0.00697 -0.00083 -0.00072 -0.00284 HKLF 5 Covalent radii and connectivity table for 02SOT050 IN P-1 C 0.770 FE 1.240 N 0.700 O 0.660 H 0.320 Fe1 - C8 C5 C4 C6 C7 C3 C9 C2 C1 C10 N1 - C12 C11 N2 - C16 C13 N3 - C17 C18 O1 - C12 O2 - C17 C1 - C2 C5 Fe1 C2 - C1 C3 Fe1 C3 - C2 C4 Fe1 C4 - C5 C3 Fe1 C5 - C4 C1 Fe1 C6 - C7 C10 Fe1 C7 - C6 C8 Fe1 C8 - C7 C9 Fe1 C9 - C8 C10 Fe1 C10 - C6 C9 C11 Fe1 C11 - N1 C10 C12 - O1 N1 C13 C13 - N2 C14 C12 C14 - C13 C15 C24 C15 - C16 C14 C35 C16 - N2 C15 C17 C17 - O2 N3 C16 C18 - C23 C19 N3 C19 - C18 C20 C20 - C21 C19 C21 - C22 C20 C22 - C21 C23 C23 - C18 C22 C24 - C29 C25 C14 C25 - C26 C24 C26 - C27 C25 C27 - C28 C26 C28 - C27 C29 C29 - C28 C24 C30 - C31 C35 C31 - C30 C32 C32 - C33 C31 C33 - C32 C34 C34 - C35 C33 C35 - C34 C30 C15 Fe2 - C36 C42 C37 C41 C45 C43 C40 C38 C44 C39 N4 - C47 C46 N5 - C51 C48 N6 - C52 C53 O3 - C47 O4 - C52 C36 - C37 C40 Fe2 C37 - C36 C38 Fe2 C38 - C37 C39 Fe2 C39 - C38 C40 Fe2 C40 - C36 C39 Fe2 C41 - C42 C45 Fe2 C42 - C41 C43 Fe2 C43 - C44 C42 Fe2 C44 - C43 C45 Fe2 C45 - C44 C41 C46 Fe2 C46 - N4 C45 C47 - O3 N4 C48 C48 - N5 C49 C47 C49 - C48 C50 C64 C50 - C51 C49 C70 C51 - N5 C50 C52 C52 - O4 N6 C51 C53 - C54 C58 N6 C54 - C53 C55 C55 - C56 C54 C56 - C55 C57 C57 - C56 C58 C58 - C57 C53 C59 - C64 C60 C60 - C61 C59 C61 - C60 C62 C62 - C63 C61 C63 - C62 C64 C64 - C59 C63 C49 C65 - C66 C70 C66 - C67 C65 C67 - C66 C68 C68 - C69 C67 C69 - C68 C70 C70 - C69 C65 C50 Operators for generating equivalent atoms: $1 -x+2, -y, -z $2 -x+1, -y+1, -z+1 30908 Reflections read, of which 9046 rejected -10 =< h =< 10, -18 =< k =< 18, -20 =< l =< 20, Max. 2-theta = 48.21 0 Systematic absence violations 0 Data suppressed, R(sigma) = 0.0643 Maximum memory for data reduction = 6645 / 255 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 = 8630 / 1055947 wR2 = 0.1543 before cycle 1 for 21893 data and 740 / 740 parameters GooF = S = 1.045; Restrained GooF = 1.045 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0574 * P )^2 + 9.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.14623 0.00121 1.594 OSF 2 0.44495 0.00066 -0.326 BASF 1 Mean shift/esd = 0.254 Maximum = 1.594 for OSF Max. shift = 0.003 A for C3 Max. dU = 0.001 for C60 Least-squares cycle 2 Maximum vector length = 511 Memory required = 8630 / 1055947 wR2 = 0.1540 before cycle 2 for 21893 data and 740 / 740 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0574 * P )^2 + 9.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.14688 0.00121 0.536 OSF 2 0.44489 0.00065 -0.090 BASF 1 Mean shift/esd = 0.088 Maximum = 0.536 for OSF Max. shift = 0.001 A for H3 Max. dU = 0.000 for C60 Least-squares cycle 3 Maximum vector length = 511 Memory required = 8630 / 1055947 wR2 = 0.1541 before cycle 3 for 21893 data and 740 / 740 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0574 * P )^2 + 9.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.14691 0.00121 0.025 OSF 2 0.44489 0.00065 0.004 BASF 1 Mean shift/esd = 0.005 Maximum = -0.053 for z C64 Max. shift = 0.000 A for C64 Max. dU = 0.000 for C22 Least-squares cycle 4 Maximum vector length = 511 Memory required = 8630 / 1055947 wR2 = 0.1541 before cycle 4 for 21893 data and 740 / 740 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0574 * P )^2 + 9.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.14691 0.00121 0.003 OSF 2 0.44489 0.00065 0.004 BASF 1 Mean shift/esd = 0.001 Maximum = 0.011 for U12 C34 Max. shift = 0.000 A for C4 Max. dU = 0.000 for C18 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.6839 0.0083 0.1807 43 0.880 0.000 N1 C12 C11 H2 0.8798 0.0735 -0.0334 43 0.880 0.000 N2 C16 C13 H3 0.5266 0.1794 -0.1579 43 0.880 0.000 N3 C17 C18 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C1 ** H1 0.6670 0.1584 0.3036 43 0.950 0.000 C1 C2 C5 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C2 ** H2 0.7676 0.1656 0.4354 43 0.950 0.000 C2 C1 C3 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C3 ** H3 0.7091 0.0368 0.5128 43 0.950 0.000 C3 C2 C4 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C4 ** H4 0.5733 -0.0518 0.4287 43 0.950 0.000 C4 C5 C3 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C5 ** H5 0.5473 0.0243 0.2999 43 0.950 0.000 C5 C4 C1 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C6 ** H6 0.9723 0.0615 0.2521 43 0.950 0.000 C6 C7 C10 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C7 ** H7 1.0713 0.0650 0.3841 43 0.950 0.000 C7 C6 C8 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C8 ** H8 1.0105 -0.0648 0.4594 43 0.950 0.000 C8 C7 C9 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C9 ** H9 0.8762 -0.1509 0.3722 43 0.950 0.000 C9 C8 C10 H11A 0.9077 -0.1174 0.1893 23 0.990 0.000 C11 N1 C10 H11B 0.7591 -0.1220 0.2338 23 0.990 0.000 C11 N1 C10 H19 0.3977 0.2496 -0.2571 43 0.950 0.000 C19 C18 C20 H20 0.3691 0.2751 -0.3880 43 0.950 0.000 C20 C21 C19 H21 0.5605 0.2379 -0.4688 43 0.950 0.000 C21 C22 C20 H22 0.7748 0.1753 -0.4196 43 0.950 0.000 C22 C21 C23 H23 0.8030 0.1486 -0.2890 43 0.950 0.000 C23 C18 C22 H25 0.5272 0.2171 0.1561 43 0.950 0.000 C25 C26 C24 H26 0.3567 0.2173 0.2532 43 0.950 0.000 C26 C27 C25 H27 0.2214 0.1042 0.2734 43 0.950 0.000 C27 C28 C26 H28 0.2543 -0.0082 0.1964 43 0.950 0.000 C28 C27 C29 H29 0.4237 -0.0094 0.0998 43 0.950 0.000 C29 C28 C24 H30 0.3055 0.1116 -0.0181 43 0.950 0.000 C30 C31 C35 H31 0.0931 0.1908 -0.0512 43 0.950 0.000 C31 C30 C32 H32 0.0922 0.3338 -0.0821 43 0.950 0.000 C32 C33 C31 H33 0.3066 0.3953 -0.0839 43 0.950 0.000 C33 C32 C34 H34 0.5216 0.3159 -0.0527 43 0.950 0.000 C34 C35 C33 H4A 0.2338 0.5717 0.3078 43 0.880 0.000 N4 C47 C46 H5A 0.4013 0.5834 0.5349 43 0.880 0.000 N5 C51 C48 H6A 0.0529 0.6842 0.6674 43 0.880 0.000 N6 C52 C53 ** Bond(s) to Fe2 ignored in idealizing H-atoms attached to C36 ** H36 0.2476 0.3680 0.2436 43 0.950 0.000 C36 C37 C40 ** Bond(s) to Fe2 ignored in idealizing H-atoms attached to C37 ** H37 0.2483 0.3332 0.1063 43 0.950 0.000 C37 C36 C38 ** Bond(s) to Fe2 ignored in idealizing H-atoms attached to C38 ** H38 0.0452 0.4227 0.0411 43 0.950 0.000 C38 C37 C39 ** Bond(s) to Fe2 ignored in idealizing H-atoms attached to C39 ** H39 -0.0814 0.5133 0.1380 43 0.950 0.000 C39 C38 C40 ** Bond(s) to Fe2 ignored in idealizing H-atoms attached to C40 ** H40 0.0461 0.4805 0.2638 43 0.950 0.000 C40 C36 C39 ** Bond(s) to Fe2 ignored in idealizing H-atoms attached to C41 ** H41 0.4982 0.4652 0.1209 43 0.950 0.000 C41 C42 C45 ** Bond(s) to Fe2 ignored in idealizing H-atoms attached to C42 ** H42 0.3503 0.5207 0.0061 43 0.950 0.000 C42 C41 C43 ** Bond(s) to Fe2 ignored in idealizing H-atoms attached to C43 ** H43 0.1690 0.6366 0.0478 43 0.950 0.000 C43 C44 C42 ** Bond(s) to Fe2 ignored in idealizing H-atoms attached to C44 ** H44 0.2055 0.6536 0.1877 43 0.950 0.000 C44 C43 C45 H46A 0.4710 0.4821 0.2699 23 0.990 0.000 C46 N4 C45 H46B 0.5097 0.5770 0.2671 23 0.990 0.000 C46 N4 C45 H54 0.3290 0.6295 0.7951 43 0.950 0.000 C54 C53 C55 H55 0.3272 0.6706 0.9203 43 0.950 0.000 C55 C56 C54 H56 0.1469 0.7658 0.9632 43 0.950 0.000 C56 C55 C57 H57 -0.0343 0.8229 0.8800 43 0.950 0.000 C57 C56 C58 H58 -0.0344 0.7826 0.7552 43 0.950 0.000 C58 C57 C53 H59 0.0913 0.7118 0.3192 43 0.950 0.000 C59 C64 C60 H60 -0.0705 0.7103 0.2201 43 0.950 0.000 C60 C61 C59 H61 -0.2494 0.6195 0.2286 43 0.950 0.000 C61 C60 C62 H62 -0.2730 0.5345 0.3387 43 0.950 0.000 C62 C63 C61 H63 -0.1090 0.5340 0.4364 43 0.950 0.000 C63 C62 C64 H65 -0.1358 0.5729 0.5877 43 0.950 0.000 C65 C66 C70 H66 -0.3654 0.6287 0.6180 43 0.950 0.000 C66 C67 C65 H67 -0.4311 0.7711 0.5990 43 0.950 0.000 C67 C66 C68 H68 -0.2654 0.8582 0.5471 43 0.950 0.000 C68 C69 C67 H69 -0.0372 0.8020 0.5142 43 0.950 0.000 C69 C68 C70 02SOT050 IN P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Fe1 0.80450 0.01660 0.36938 1.00000 0.01538 0.02042 0.01468 -0.00087 0.00301 -0.00084 0.01690 0.00091 0.00006 0.00003 0.00003 0.00000 0.00033 0.00035 0.00030 0.00025 0.00024 0.00026 0.00015 N1 0.76641 -0.01781 0.16720 1.00000 0.01090 0.02218 0.01231 -0.00133 0.00160 0.00615 0.01563 0.00475 0.00031 0.00019 0.00016 0.00000 0.00182 0.00187 0.00166 0.00138 0.00130 0.00141 0.00072 H1 0.68394 0.00828 0.18074 1.00000 0.01876 0.00000 0.00000 N2 0.79263 0.08964 -0.01756 1.00000 0.00719 0.01629 0.01133 -0.00369 0.00206 -0.00101 0.01151 0.00449 0.00031 0.00018 0.00015 0.00000 0.00170 0.00176 0.00159 0.00129 0.00128 0.00137 0.00069 H2 0.87982 0.07353 -0.03337 1.00000 0.01382 0.00000 0.00000 N3 0.60966 0.18140 -0.18121 1.00000 0.00878 0.02407 0.01314 0.00068 0.00195 -0.00115 0.01543 0.00475 0.00031 0.00018 0.00016 0.00000 0.00180 0.00194 0.00167 0.00138 0.00137 0.00141 0.00072 H3 0.52656 0.17938 -0.15787 1.00000 0.01851 0.00000 0.00000 O1 0.94410 -0.02210 0.08113 1.00000 0.01930 0.03275 0.02172 0.01030 0.00943 0.00770 0.02573 0.00458 0.00029 0.00017 0.00014 0.00000 0.00173 0.00180 0.00152 0.00126 0.00127 0.00135 0.00068 O2 0.84977 0.17298 -0.15873 1.00000 0.01682 0.02774 0.01382 0.00265 0.00331 -0.00101 0.01969 0.00411 0.00027 0.00016 0.00013 0.00000 0.00165 0.00166 0.00142 0.00116 0.00116 0.00125 0.00062 C1 0.66091 0.11791 0.34454 1.00000 0.02314 0.02634 0.02353 0.00117 0.00168 0.00952 0.02521 0.00682 0.00042 0.00026 0.00023 0.00000 0.00257 0.00262 0.00240 0.00188 0.00188 0.00200 0.00102 H1 0.66701 0.15836 0.30359 1.00000 0.03026 0.00000 0.00000 C2 0.71681 0.12191 0.41800 1.00000 0.02275 0.02524 0.02850 -0.01153 0.00435 0.00612 0.02570 0.00694 0.00043 0.00025 0.00023 0.00000 0.00257 0.00256 0.00247 0.00194 0.00194 0.00194 0.00101 H2 0.76758 0.16555 0.43543 1.00000 0.03084 0.00000 0.00000 C3 0.68433 0.04999 0.46106 1.00000 0.01737 0.03581 0.02121 -0.00355 0.00392 -0.00107 0.02484 0.00658 0.00041 0.00026 0.00023 0.00000 0.00246 0.00276 0.00225 0.00198 0.00179 0.00199 0.00100 H3 0.70915 0.03678 0.51279 1.00000 0.02981 0.00000 0.00000 C4 0.60817 0.00036 0.41425 1.00000 0.02041 0.03014 0.02813 -0.00494 0.00998 -0.00078 0.02626 0.00689 0.00043 0.00027 0.00023 0.00000 0.00252 0.00269 0.00249 0.00203 0.00192 0.00199 0.00102 H4 0.57335 -0.05180 0.42869 1.00000 0.03151 0.00000 0.00000 C5 0.59405 0.04289 0.34263 1.00000 0.01532 0.04104 0.02313 -0.00937 -0.00154 0.00884 0.02696 0.00705 0.00042 0.00027 0.00023 0.00000 0.00244 0.00296 0.00238 0.00205 0.00179 0.00205 0.00105 H5 0.54727 0.02433 0.29989 1.00000 0.03235 0.00000 0.00000 C6 0.96534 0.01979 0.29188 1.00000 0.01365 0.02556 0.01884 0.00240 0.00233 -0.00169 0.01951 0.00618 0.00040 0.00024 0.00022 0.00000 0.00228 0.00241 0.00217 0.00178 0.00170 0.00182 0.00092 H6 0.97227 0.06153 0.25210 1.00000 0.02341 0.00000 0.00000 C7 1.02029 0.02194 0.36574 1.00000 0.01680 0.02634 0.02150 -0.00407 0.00284 -0.00384 0.02134 0.00647 0.00040 0.00025 0.00021 0.00000 0.00230 0.00243 0.00226 0.00186 0.00177 0.00186 0.00094 H7 1.07127 0.06501 0.38411 1.00000 0.02561 0.00000 0.00000 C8 0.98688 -0.05050 0.40770 1.00000 0.01961 0.02564 0.01307 0.00102 0.00005 0.00422 0.01993 0.00633 0.00040 0.00024 0.00021 0.00000 0.00239 0.00247 0.00202 0.00173 0.00170 0.00183 0.00092 H8 1.01045 -0.06478 0.45942 1.00000 0.02392 0.00000 0.00000 C9 0.91150 -0.09860 0.35894 1.00000 0.02210 0.01491 0.01283 0.00206 -0.00179 0.00572 0.01720 0.00614 0.00040 0.00023 0.00020 0.00000 0.00231 0.00212 0.00199 0.00160 0.00169 0.00175 0.00088 H9 0.87617 -0.15091 0.37223 1.00000 0.02064 0.00000 0.00000 C10 0.89833 -0.05445 0.28659 1.00000 0.01250 0.01835 0.01493 0.00085 0.00442 0.00402 0.01570 0.00618 0.00039 0.00023 0.00020 0.00000 0.00220 0.00218 0.00201 0.00166 0.00160 0.00169 0.00087 C11 0.83256 -0.08431 0.21769 1.00000 0.01545 0.01734 0.01495 0.00162 -0.00086 0.00198 0.01624 0.00592 0.00039 0.00023 0.00020 0.00000 0.00226 0.00222 0.00201 0.00164 0.00164 0.00172 0.00087 H11A 0.90770 -0.11744 0.18933 1.00000 0.01948 0.00000 0.00000 H11B 0.75906 -0.12199 0.23383 1.00000 0.01948 0.00000 0.00000 C12 0.82452 0.00591 0.10100 1.00000 0.01357 0.01391 0.01276 -0.00291 0.00122 -0.00083 0.01337 0.00574 0.00040 0.00022 0.00020 0.00000 0.00230 0.00213 0.00197 0.00157 0.00165 0.00171 0.00084 C13 0.73499 0.06579 0.05076 1.00000 0.01222 0.01511 0.01183 -0.00174 0.00268 -0.00678 0.01267 0.00557 0.00038 0.00022 0.00019 0.00000 0.00219 0.00208 0.00197 0.00157 0.00156 0.00167 0.00083 C14 0.59799 0.10480 0.05516 1.00000 0.01520 0.01091 0.01143 -0.00263 -0.00137 -0.00343 0.01229 0.00550 0.00038 0.00022 0.00019 0.00000 0.00227 0.00204 0.00195 0.00152 0.00156 0.00169 0.00083 C15 0.57135 0.15404 -0.01304 1.00000 0.01188 0.01169 0.01456 -0.00228 0.00247 -0.00309 0.01254 0.00560 0.00038 0.00022 0.00019 0.00000 0.00215 0.00204 0.00198 0.00155 0.00158 0.00165 0.00083 C16 0.69426 0.14201 -0.05710 1.00000 0.01431 0.01286 0.01031 -0.00061 -0.00103 -0.00046 0.01255 0.00562 0.00038 0.00022 0.00019 0.00000 0.00220 0.00209 0.00192 0.00153 0.00159 0.00166 0.00083 C17 0.72838 0.16812 -0.13626 1.00000 0.01651 0.00974 0.01863 -0.00042 0.00516 -0.00039 0.01505 0.00606 0.00041 0.00022 0.00021 0.00000 0.00237 0.00203 0.00208 0.00163 0.00180 0.00169 0.00085 C18 0.60357 0.19806 -0.26088 1.00000 0.02028 0.01652 0.01288 -0.00041 -0.00191 -0.00317 0.01648 0.00587 0.00040 0.00023 0.00020 0.00000 0.00243 0.00224 0.00205 0.00161 0.00171 0.00180 0.00089 C19 0.47509 0.23462 -0.29035 1.00000 0.02297 0.02649 0.01732 -0.00177 0.00121 0.00197 0.02253 0.00630 0.00043 0.00024 0.00022 0.00000 0.00255 0.00245 0.00218 0.00181 0.00179 0.00192 0.00096 H19 0.39771 0.24959 -0.25706 1.00000 0.02703 0.00000 0.00000 C20 0.45769 0.24972 -0.36781 1.00000 0.02608 0.02807 0.02317 0.00116 -0.00740 0.00527 0.02635 0.00658 0.00045 0.00025 0.00022 0.00000 0.00260 0.00251 0.00238 0.00193 0.00199 0.00195 0.00100 H20 0.36908 0.27506 -0.38797 1.00000 0.03162 0.00000 0.00000 C21 0.57085 0.22748 -0.41543 1.00000 0.02983 0.02909 0.01540 0.00052 -0.00450 -0.00332 0.02479 0.00643 0.00044 0.00025 0.00023 0.00000 0.00277 0.00264 0.00216 0.00183 0.00197 0.00206 0.00101 H21 0.56054 0.23793 -0.46878 1.00000 0.02974 0.00000 0.00000 C22 0.69756 0.19054 -0.38627 1.00000 0.02481 0.02862 0.01790 -0.00529 0.00023 -0.00140 0.02371 0.00628 0.00044 0.00025 0.00022 0.00000 0.00260 0.00254 0.00228 0.00183 0.00183 0.00194 0.00097 H22 0.77476 0.17534 -0.41958 1.00000 0.02845 0.00000 0.00000 C23 0.71491 0.17499 -0.30884 1.00000 0.01354 0.02006 0.01859 -0.00125 0.00115 0.00097 0.01757 0.00604 0.00040 0.00023 0.00021 0.00000 0.00228 0.00227 0.00220 0.00169 0.00166 0.00173 0.00089 H23 0.80301 0.14859 -0.28898 1.00000 0.02108 0.00000 0.00000 C24 0.49444 0.10293 0.11868 1.00000 0.00795 0.01700 0.01557 0.00211 -0.00414 -0.00186 0.01356 0.00567 0.00038 0.00023 0.00019 0.00000 0.00206 0.00212 0.00203 0.00160 0.00155 0.00165 0.00085 C25 0.47240 0.17065 0.16433 1.00000 0.02179 0.01254 0.01620 -0.00026 0.00554 -0.00634 0.01658 0.00602 0.00040 0.00022 0.00020 0.00000 0.00238 0.00210 0.00207 0.00160 0.00166 0.00175 0.00089 H25 0.52723 0.21706 0.15607 1.00000 0.01990 0.00000 0.00000 C26 0.37084 0.17092 0.22189 1.00000 0.02022 0.01848 0.02102 -0.00636 0.00563 0.00372 0.02010 0.00639 0.00040 0.00024 0.00021 0.00000 0.00240 0.00230 0.00219 0.00174 0.00180 0.00184 0.00093 H26 0.35668 0.21727 0.25321 1.00000 0.02413 0.00000 0.00000 C27 0.29064 0.10420 0.23368 1.00000 0.01623 0.02590 0.02037 0.00082 0.00798 0.00152 0.02117 0.00645 0.00041 0.00024 0.00022 0.00000 0.00237 0.00253 0.00219 0.00185 0.00176 0.00190 0.00095 H27 0.22143 0.10425 0.27335 1.00000 0.02541 0.00000 0.00000 C28 0.31039 0.03771 0.18834 1.00000 0.02046 0.02308 0.02860 0.00137 0.00517 -0.00951 0.02369 0.00665 0.00042 0.00025 0.00022 0.00000 0.00245 0.00243 0.00237 0.00197 0.00195 0.00191 0.00097 H28 0.25429 -0.00818 0.19636 1.00000 0.02843 0.00000 0.00000 C29 0.41116 0.03699 0.13117 1.00000 0.01761 0.01844 0.02504 -0.00459 0.00439 -0.00521 0.02003 0.00626 0.00040 0.00024 0.00022 0.00000 0.00230 0.00224 0.00228 0.00177 0.00182 0.00179 0.00092 H29 0.42371 -0.00942 0.09985 1.00000 0.02404 0.00000 0.00000 C30 0.30663 0.16951 -0.03201 1.00000 0.02044 0.01984 0.01833 0.00043 -0.00152 -0.00213 0.01957 0.00609 0.00041 0.00025 0.00021 0.00000 0.00248 0.00231 0.00217 0.00172 0.00174 0.00191 0.00094 H30 0.30552 0.11163 -0.01814 1.00000 0.02349 0.00000 0.00000 C31 0.18032 0.21649 -0.05100 1.00000 0.01708 0.02307 0.01608 -0.00350 -0.00012 -0.00465 0.01848 0.00611 0.00042 0.00024 0.00020 0.00000 0.00238 0.00238 0.00211 0.00172 0.00169 0.00185 0.00091 H31 0.09312 0.19077 -0.05120 1.00000 0.02217 0.00000 0.00000 C32 0.17970 0.30102 -0.06981 1.00000 0.01931 0.03075 0.01293 -0.00578 -0.00249 0.00741 0.02146 0.00628 0.00043 0.00025 0.00021 0.00000 0.00248 0.00258 0.00205 0.00179 0.00171 0.00195 0.00095 H32 0.09216 0.33382 -0.08211 1.00000 0.02575 0.00000 0.00000 C33 0.30652 0.33726 -0.07058 1.00000 0.02269 0.02091 0.01320 0.00283 -0.00180 0.00160 0.01930 0.00627 0.00041 0.00025 0.00020 0.00000 0.00254 0.00232 0.00206 0.00172 0.00173 0.00190 0.00092 H33 0.30665 0.39532 -0.08391 1.00000 0.02316 0.00000 0.00000 C34 0.43457 0.28992 -0.05209 1.00000 0.01292 0.02206 0.01463 -0.00118 -0.00047 -0.00469 0.01633 0.00597 0.00040 0.00024 0.00019 0.00000 0.00227 0.00229 0.00204 0.00170 0.00163 0.00178 0.00088 H34 0.52160 0.31586 -0.05275 1.00000 0.01960 0.00000 0.00000 C35 0.43667 0.20538 -0.03273 1.00000 0.01191 0.01622 0.00740 -0.00234 0.00181 -0.00117 0.01180 0.00561 0.00038 0.00022 0.00019 0.00000 0.00218 0.00217 0.00182 0.00153 0.00151 0.00169 0.00082 Fe2 0.21144 0.49541 0.13854 1.00000 0.01786 0.01689 0.01281 0.00023 0.00222 -0.00402 0.01575 0.00089 0.00006 0.00003 0.00003 0.00000 0.00033 0.00032 0.00029 0.00024 0.00024 0.00025 0.00014 N4 0.32476 0.55976 0.32009 1.00000 0.00944 0.03182 0.01250 -0.00459 0.00201 -0.00097 0.01787 0.00487 0.00032 0.00019 0.00016 0.00000 0.00177 0.00209 0.00172 0.00140 0.00134 0.00144 0.00074 H4A 0.23383 0.57171 0.30777 1.00000 0.02145 0.00000 0.00000 N5 0.31233 0.59858 0.52042 1.00000 0.00798 0.02287 0.01223 -0.00223 -0.00281 -0.00044 0.01437 0.00458 0.00031 0.00018 0.00016 0.00000 0.00175 0.00194 0.00166 0.00137 0.00134 0.00140 0.00072 H5A 0.40128 0.58341 0.53490 1.00000 0.01724 0.00000 0.00000 N6 0.13916 0.67928 0.68770 1.00000 0.00902 0.02648 0.00930 -0.00325 -0.00229 -0.00055 0.01491 0.00465 0.00031 0.00018 0.00015 0.00000 0.00176 0.00194 0.00164 0.00137 0.00129 0.00141 0.00072 H6A 0.05290 0.68416 0.66740 1.00000 0.01790 0.00000 0.00000 O3 0.48865 0.53421 0.41246 1.00000 0.01247 0.03286 0.01319 -0.00053 -0.00034 0.00540 0.02003 0.00415 0.00027 0.00016 0.00013 0.00000 0.00161 0.00175 0.00137 0.00119 0.00116 0.00125 0.00063 O4 0.37233 0.63868 0.66366 1.00000 0.01278 0.03940 0.01823 -0.00553 -0.00030 -0.00096 0.02342 0.00423 0.00028 0.00017 0.00014 0.00000 0.00164 0.00187 0.00147 0.00127 0.00120 0.00129 0.00065 C36 0.18257 0.39279 0.20578 1.00000 0.03065 0.02021 0.02564 0.00576 -0.00140 -0.00457 0.02561 0.00662 0.00045 0.00025 0.00023 0.00000 0.00272 0.00246 0.00240 0.00185 0.00191 0.00206 0.00101 H36 0.24756 0.36795 0.24357 1.00000 0.03074 0.00000 0.00000 C37 0.18298 0.37319 0.12945 1.00000 0.03684 0.01305 0.02414 -0.00326 0.00535 -0.00336 0.02455 0.00640 0.00045 0.00024 0.00022 0.00000 0.00277 0.00222 0.00235 0.00178 0.00201 0.00198 0.00099 H37 0.24826 0.33318 0.10633 1.00000 0.02946 0.00000 0.00000 C38 0.07007 0.42305 0.09329 1.00000 0.03124 0.02717 0.02318 -0.00184 0.00262 -0.01378 0.02648 0.00664 0.00045 0.00026 0.00023 0.00000 0.00277 0.00251 0.00229 0.00192 0.00197 0.00210 0.00102 H38 0.04524 0.42275 0.04114 1.00000 0.03177 0.00000 0.00000 C39 -0.00047 0.47372 0.14723 1.00000 0.01507 0.02224 0.03461 0.00080 0.00150 -0.00982 0.02355 0.00624 0.00041 0.00025 0.00023 0.00000 0.00231 0.00235 0.00260 0.00200 0.00193 0.00184 0.00097 H39 -0.08139 0.51334 0.13803 1.00000 0.02825 0.00000 0.00000 C40 0.07007 0.45533 0.21733 1.00000 0.03070 0.02425 0.02051 -0.00266 0.00909 -0.01371 0.02442 0.00645 0.00044 0.00025 0.00022 0.00000 0.00271 0.00253 0.00227 0.00185 0.00192 0.00209 0.00102 H40 0.04607 0.48054 0.26382 1.00000 0.02931 0.00000 0.00000 C41 0.42206 0.50888 0.12017 1.00000 0.01509 0.02205 0.01763 0.00012 0.00407 0.00391 0.01869 0.00616 0.00040 0.00024 0.00020 0.00000 0.00228 0.00237 0.00219 0.00170 0.00169 0.00180 0.00093 H41 0.49817 0.46523 0.12087 1.00000 0.02243 0.00000 0.00000 C42 0.33969 0.53992 0.05599 1.00000 0.01924 0.02772 0.00951 -0.00124 0.00605 -0.00698 0.01853 0.00602 0.00039 0.00024 0.00020 0.00000 0.00242 0.00245 0.00199 0.00172 0.00165 0.00190 0.00092 H42 0.35034 0.52068 0.00607 1.00000 0.02224 0.00000 0.00000 C43 0.23847 0.60481 0.07937 1.00000 0.01710 0.02304 0.01926 0.00604 0.00013 -0.00913 0.01960 0.00607 0.00040 0.00024 0.00021 0.00000 0.00235 0.00236 0.00218 0.00179 0.00173 0.00189 0.00093 H43 0.16904 0.63661 0.04780 1.00000 0.02352 0.00000 0.00000 C44 0.25848 0.61409 0.15758 1.00000 0.01767 0.01477 0.01653 -0.00190 0.00649 -0.00262 0.01625 0.00588 0.00039 0.00023 0.00020 0.00000 0.00232 0.00218 0.00214 0.00164 0.00166 0.00174 0.00089 H44 0.20550 0.65358 0.18766 1.00000 0.01950 0.00000 0.00000 C45 0.37119 0.55438 0.18351 1.00000 0.01394 0.01909 0.01525 -0.00132 0.00014 -0.00546 0.01583 0.00579 0.00039 0.00023 0.00020 0.00000 0.00226 0.00226 0.00204 0.00169 0.00165 0.00178 0.00088 C46 0.43040 0.54111 0.26196 1.00000 0.01610 0.03577 0.01331 -0.00409 0.00436 -0.00306 0.02161 0.00629 0.00040 0.00026 0.00020 0.00000 0.00236 0.00264 0.00204 0.00177 0.00168 0.00189 0.00095 H46A 0.47096 0.48211 0.26993 1.00000 0.02593 0.00000 0.00000 H46B 0.50966 0.57697 0.26709 1.00000 0.02593 0.00000 0.00000 C47 0.36538 0.55884 0.39287 1.00000 0.01840 0.01776 0.01284 -0.00038 0.00149 -0.00597 0.01608 0.00597 0.00042 0.00023 0.00020 0.00000 0.00246 0.00225 0.00209 0.00162 0.00168 0.00181 0.00089 C48 0.26008 0.59133 0.44923 1.00000 0.01694 0.01818 0.00948 0.00047 0.00117 -0.00622 0.01462 0.00577 0.00039 0.00023 0.00019 0.00000 0.00237 0.00224 0.00197 0.00158 0.00158 0.00176 0.00087 C49 0.11555 0.61959 0.44953 1.00000 0.01246 0.01161 0.01305 0.00377 0.00167 -0.00296 0.01243 0.00582 0.00039 0.00022 0.00019 0.00000 0.00222 0.00203 0.00197 0.00154 0.00156 0.00162 0.00083 C50 0.08174 0.64610 0.52358 1.00000 0.01705 0.00926 0.01321 -0.00079 0.00411 -0.00389 0.01301 0.00573 0.00039 0.00021 0.00019 0.00000 0.00223 0.00205 0.00196 0.00154 0.00163 0.00165 0.00083 C51 0.20757 0.63241 0.56524 1.00000 0.01003 0.01631 0.00932 -0.00082 0.00128 0.00023 0.01199 0.00573 0.00038 0.00022 0.00019 0.00000 0.00215 0.00211 0.00188 0.00155 0.00157 0.00163 0.00082 C52 0.24830 0.65019 0.64291 1.00000 0.01178 0.01496 0.01737 0.00072 0.00043 -0.00340 0.01463 0.00601 0.00041 0.00022 0.00021 0.00000 0.00225 0.00215 0.00210 0.00161 0.00176 0.00171 0.00086 C53 0.14776 0.70277 0.76344 1.00000 0.01562 0.01758 0.01137 -0.00328 -0.00062 -0.00834 0.01432 0.00559 0.00040 0.00023 0.00019 0.00000 0.00225 0.00216 0.00198 0.00163 0.00164 0.00174 0.00086 C54 0.25511 0.66888 0.81210 1.00000 0.01592 0.02553 0.01688 0.00055 -0.00052 -0.00375 0.01939 0.00603 0.00041 0.00025 0.00021 0.00000 0.00234 0.00243 0.00214 0.00176 0.00173 0.00185 0.00092 H54 0.32903 0.62949 0.79513 1.00000 0.02327 0.00000 0.00000 C55 0.25324 0.69339 0.88644 1.00000 0.02109 0.03133 0.01615 -0.00053 -0.00315 -0.01226 0.02224 0.00607 0.00042 0.00025 0.00021 0.00000 0.00246 0.00259 0.00217 0.00184 0.00176 0.00202 0.00097 H55 0.32719 0.67057 0.92032 1.00000 0.02668 0.00000 0.00000 C56 0.14675 0.74993 0.91205 1.00000 0.03810 0.02333 0.00862 -0.00411 0.00509 -0.01637 0.02238 0.00622 0.00044 0.00024 0.00021 0.00000 0.00286 0.00242 0.00207 0.00171 0.00189 0.00213 0.00101 H56 0.14688 0.76579 0.96318 1.00000 0.02685 0.00000 0.00000 C57 0.03956 0.78351 0.86287 1.00000 0.02967 0.01986 0.02130 -0.00415 0.00466 -0.00197 0.02355 0.00629 0.00043 0.00024 0.00022 0.00000 0.00262 0.00228 0.00229 0.00184 0.00198 0.00188 0.00096 H57 -0.03426 0.82289 0.87997 1.00000 0.02826 0.00000 0.00000 C58 0.03983 0.75978 0.78888 1.00000 0.02201 0.02292 0.01565 0.00262 0.00073 0.00128 0.02056 0.00637 0.00042 0.00024 0.00021 0.00000 0.00251 0.00237 0.00213 0.00170 0.00175 0.00189 0.00094 H58 -0.03436 0.78263 0.75515 1.00000 0.02467 0.00000 0.00000 C59 0.01862 0.67440 0.32279 1.00000 0.01466 0.01456 0.01463 0.00122 0.00266 -0.00168 0.01469 0.00600 0.00039 0.00022 0.00020 0.00000 0.00221 0.00213 0.00202 0.00160 0.00166 0.00167 0.00085 H59 0.09135 0.71176 0.31917 1.00000 0.01762 0.00000 0.00000 C60 -0.07773 0.67403 0.26408 1.00000 0.02088 0.01897 0.01432 0.00386 0.00085 0.00412 0.01863 0.00621 0.00040 0.00024 0.00021 0.00000 0.00243 0.00225 0.00208 0.00163 0.00173 0.00184 0.00091 H60 -0.07048 0.71026 0.22009 1.00000 0.02236 0.00000 0.00000 C61 -0.18424 0.62100 0.26952 1.00000 0.01708 0.02708 0.01100 -0.00382 -0.00340 0.00092 0.01847 0.00608 0.00040 0.00024 0.00020 0.00000 0.00233 0.00239 0.00201 0.00168 0.00163 0.00188 0.00091 H61 -0.24939 0.61953 0.22863 1.00000 0.02216 0.00000 0.00000 C62 -0.19707 0.56966 0.33437 1.00000 0.01074 0.02474 0.02148 -0.00138 0.00370 -0.00546 0.01876 0.00623 0.00039 0.00024 0.00021 0.00000 0.00220 0.00237 0.00221 0.00177 0.00171 0.00178 0.00091 H62 -0.27299 0.53451 0.33875 1.00000 0.02251 0.00000 0.00000 C63 -0.10024 0.56965 0.39214 1.00000 0.01303 0.01681 0.01546 0.00020 0.00114 0.00350 0.01547 0.00587 0.00038 0.00023 0.00020 0.00000 0.00219 0.00218 0.00206 0.00160 0.00162 0.00171 0.00087 H63 -0.10901 0.53403 0.43640 1.00000 0.01856 0.00000 0.00000 C64 0.01139 0.62141 0.38682 1.00000 0.00925 0.01260 0.01234 -0.00390 0.00066 0.00220 0.01149 0.00555 0.00037 0.00022 0.00019 0.00000 0.00206 0.00203 0.00194 0.00154 0.00153 0.00161 0.00081 C65 -0.16188 0.63120 0.57874 1.00000 0.01600 0.02616 0.01966 -0.00017 0.00193 -0.00244 0.02063 0.00612 0.00040 0.00026 0.00021 0.00000 0.00239 0.00243 0.00217 0.00179 0.00177 0.00188 0.00094 H65 -0.13577 0.57292 0.58768 1.00000 0.02475 0.00000 0.00000 C66 -0.29816 0.66436 0.59723 1.00000 0.01359 0.04087 0.01819 -0.00269 0.00380 -0.00059 0.02433 0.00665 0.00042 0.00027 0.00022 0.00000 0.00243 0.00300 0.00220 0.00190 0.00172 0.00202 0.00101 H66 -0.36537 0.62868 0.61802 1.00000 0.02919 0.00000 0.00000 C67 -0.33731 0.74832 0.58585 1.00000 0.01302 0.04380 0.01910 -0.01492 -0.00046 0.00923 0.02560 0.00648 0.00043 0.00028 0.00022 0.00000 0.00235 0.00305 0.00223 0.00203 0.00177 0.00210 0.00103 H67 -0.43110 0.77107 0.59901 1.00000 0.03072 0.00000 0.00000 C68 -0.23926 0.79983 0.55502 1.00000 0.02604 0.02417 0.03765 -0.00705 -0.00652 0.00979 0.02985 0.00685 0.00046 0.00027 0.00024 0.00000 0.00278 0.00259 0.00271 0.00207 0.00211 0.00210 0.00108 H68 -0.26539 0.85823 0.54712 1.00000 0.03583 0.00000 0.00000 C69 -0.10354 0.76625 0.53578 1.00000 0.01913 0.02466 0.02266 -0.00107 -0.00037 -0.00194 0.02217 0.00630 0.00042 0.00025 0.00021 0.00000 0.00248 0.00256 0.00231 0.00180 0.00179 0.00194 0.00097 H69 -0.03717 0.80200 0.51422 1.00000 0.02660 0.00000 0.00000 C70 -0.06211 0.68167 0.54723 1.00000 0.01589 0.01804 0.00838 -0.00188 -0.00067 -0.00268 0.01399 0.00570 0.00039 0.00023 0.00019 0.00000 0.00224 0.00227 0.00187 0.00158 0.00158 0.00174 0.00085 Final Structure Factor Calculation for 02SOT050 IN P-1 Total number of l.s. parameters = 740 Maximum vector length = 511 Memory required = 7890 / 24017 wR2 = 0.1541 before cycle 5 for 21893 data and 0 / 740 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0574 * P )^2 + 9.05 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0591 for 17568 Fo > 4sig(Fo) and 0.0833 for all 21893 data wR2 = 0.1541, GooF = S = 1.042, Restrained GooF = 1.042 for all data Occupancy sum of asymmetric unit = 82.00 for non-hydrogen and 58.00 for hydrogen atoms Principal mean square atomic displacements U 0.0209 0.0179 0.0120 Fe1 0.0270 0.0128 0.0070 N1 0.0175 0.0108 0.0062 N2 0.0246 0.0137 0.0080 N3 0.0495 0.0168 0.0110 O1 0.0295 0.0183 0.0112 O2 0.0390 0.0229 0.0138 C1 0.0374 0.0294 0.0103 C2 0.0362 0.0236 0.0148 C3 0.0352 0.0304 0.0131 C4 0.0486 0.0205 0.0117 C5 0.0276 0.0184 0.0125 C6 0.0279 0.0208 0.0154 C7 0.0307 0.0163 0.0127 C8 0.0277 0.0152 0.0087 C9 0.0244 0.0146 0.0081 C10 0.0210 0.0159 0.0118 C11 0.0155 0.0141 0.0105 C12 0.0194 0.0116 0.0070 C13 0.0160 0.0131 0.0078 C14 0.0168 0.0113 0.0096 C15 0.0150 0.0126 0.0101 C16 0.0231 0.0124 0.0097 C17 0.0211 0.0159 0.0124 C18 0.0299 0.0209 0.0168 C19 0.0366 0.0280 0.0145 C20 0.0315 0.0288 0.0141 C21 0.0301 0.0247 0.0163 C22 0.0213 0.0188 0.0126 C23 0.0202 0.0144 0.0061 C24 0.0258 0.0151 0.0089 C25 0.0265 0.0247 0.0091 C26 0.0311 0.0225 0.0100 C27 0.0312 0.0283 0.0116 C28 0.0285 0.0175 0.0141 C29 0.0217 0.0199 0.0172 C30 0.0244 0.0167 0.0144 C31 0.0383 0.0145 0.0115 C32 0.0262 0.0205 0.0113 C33 0.0227 0.0147 0.0116 C34 0.0165 0.0125 0.0065 C35 0.0197 0.0163 0.0113 Fe2 0.0324 0.0129 0.0083 N4 0.0232 0.0133 0.0066 N5 0.0269 0.0111 0.0067 N6 0.0363 0.0132 0.0106 O3 0.0402 0.0173 0.0128 O4 0.0327 0.0285 0.0156 C36 0.0388 0.0224 0.0124 C37 0.0396 0.0231 0.0167 C38 0.0352 0.0266 0.0089 C39 0.0408 0.0205 0.0119 C40 0.0273 0.0180 0.0108 C41 0.0296 0.0196 0.0064 C42 0.0308 0.0184 0.0095 C43 0.0237 0.0145 0.0106 C44 0.0208 0.0152 0.0114 C45 0.0360 0.0189 0.0100 C46 0.0220 0.0145 0.0118 C47 0.0217 0.0133 0.0088 C48 0.0171 0.0134 0.0067 C49 0.0199 0.0113 0.0079 C50 0.0168 0.0109 0.0082 C51 0.0183 0.0153 0.0103 C52 0.0229 0.0126 0.0074 C53 0.0261 0.0167 0.0154 C54 0.0367 0.0177 0.0123 C55 0.0455 0.0140 0.0076 C56 0.0318 0.0222 0.0166 C57 0.0276 0.0198 0.0143 C58 0.0181 0.0148 0.0111 C59 0.0282 0.0166 0.0111 C60 0.0289 0.0173 0.0092 C61 0.0255 0.0222 0.0085 C62 0.0213 0.0151 0.0100 C63 0.0164 0.0116 0.0065 C64 0.0264 0.0204 0.0150 C65 0.0413 0.0203 0.0114 C66 0.0533 0.0157 0.0079 C67 0.0464 0.0292 0.0139 C68 0.0247 0.0227 0.0191 C69 0.0184 0.0155 0.0081 C70 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.034 0.062 0.087 0.113 0.139 0.167 0.201 0.245 0.323 1.000 Number in group 2214. 2236. 2164. 2161. 2185. 2174. 2202. 2169. 2193. 2195. GooF 1.203 1.073 1.042 1.040 1.019 0.959 0.961 0.993 0.993 1.116 K 2.251 1.089 1.017 1.002 1.008 1.002 1.009 1.007 1.005 1.011 Resolution(A) 0.87 0.92 0.98 1.04 1.12 1.21 1.33 1.48 1.72 2.18 inf Number in group 2204. 2197. 2172. 2242. 2133. 2223. 2169. 2165. 2185. 2203. GooF 1.155 1.136 1.059 1.033 1.020 0.976 0.981 1.130 1.014 0.893 K 1.045 1.012 1.009 1.015 1.007 1.002 1.011 1.012 1.018 1.000 R1 0.172 0.136 0.114 0.096 0.082 0.073 0.061 0.053 0.050 0.042 Recommended weighting scheme: WGHT 0.0628 7.9069 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) 1 9 6 2609.91 6099.66 9.35 0.531 1.56 0 -10 -1 436.84 11.81 8.45 0.023 1.60 -1 11 6 1188.42 350.85 8.14 0.127 1.30 6 10 3 464.69 2.00 8.14 0.010 1.16 -2 10 -1 207.89 1015.39 8.12 0.217 1.46 0 10 1 415.76 11.81 8.11 0.023 1.60 6 8 12 598.04 1907.07 8.08 0.297 0.99 7 5 12 16.28 706.20 8.04 0.181 0.97 -6 -6 11 98.02 1004.83 7.62 0.216 1.04 -9 -9 2 435.73 1601.39 7.61 0.272 0.93 -2 3 13 182.10 893.74 7.59 0.203 1.27 -1 -10 2 1025.84 319.74 7.58 0.122 1.56 -2 -10 1 459.49 1384.68 7.45 0.253 1.54 1 10 -2 994.31 319.74 7.34 0.122 1.56 -4 -6 -3 2809.90 5378.29 7.23 0.499 1.78 -3 6 -5 300.11 0.46 7.19 0.005 1.67 0 11 3 1103.55 387.73 7.14 0.134 1.43 -1 6 9 390.66 25.17 7.13 0.034 1.58 2 -9 -1 1347.07 2836.01 7.13 0.362 1.61 -3 11 -6 342.79 0.27 7.01 0.004 1.15 6 10 3 341.20 2.00 6.96 0.010 1.16 4 7 3 2018.68 3951.40 6.91 0.428 1.66 -4 -7 -3 2009.39 3951.40 6.87 0.428 1.66 -2 -6 10 1268.29 2638.16 6.79 0.349 1.39 4 14 10 229.70 991.72 6.74 0.214 0.93 -4 -6 7 1453.49 629.90 6.74 0.171 1.46 1 15 -3 899.53 2025.49 6.62 0.306 1.04 2 -3 -13 260.60 893.74 6.58 0.203 1.27 -5 -12 -2 246.67 925.64 6.55 0.207 1.13 -2 10 -3 261.61 11.52 6.45 0.023 1.41 5 1 1 1443.14 2793.77 6.44 0.360 1.86 -3 -5 14 372.71 3.96 6.29 0.014 1.09 -6 -5 -8 1614.60 3023.07 6.22 0.374 1.23 -5 -15 -6 134.97 713.75 6.07 0.182 0.93 -4 0 11 93.08 494.86 6.03 0.151 1.32 -1 12 7 355.70 13.41 5.97 0.025 1.18 -3 -15 10 495.80 6.30 5.96 0.017 0.87 -3 -6 -5 399.89 46.37 5.87 0.046 1.86 3 15 -10 473.72 6.30 5.80 0.017 0.87 -3 10 3 637.54 1386.64 5.78 0.253 1.35 8 6 0 404.89 1057.77 5.74 0.221 1.11 5 -9 -6 873.52 1736.60 5.69 0.284 1.15 -4 6 3 1763.84 3060.96 5.67 0.376 1.62 -6 -10 -3 261.11 2.00 5.57 0.010 1.16 -5 2 1 249.61 26.97 5.57 0.035 1.77 -3 -6 6 935.35 1810.69 5.57 0.290 1.69 5 -7 -4 110.63 494.79 5.45 0.151 1.33 -7 -13 3 123.78 656.80 5.34 0.174 0.93 0 -16 9 535.76 13.69 5.27 0.025 0.87 2 -7 -6 960.64 1748.60 5.14 0.285 1.68 Bond lengths and angles Fe1 - Distance Angles C8 2.0278 (0.0038) C5 2.0273 (0.0040) 158.76 (0.17) C4 2.0299 (0.0040) 122.76 (0.16) 40.47 (0.16) C6 2.0284 (0.0038) 68.36 (0.15) 123.45 (0.16) 159.64 (0.16) C7 2.0301 (0.0038) 40.51 (0.15) 159.46 (0.17) 158.51 (0.16) 40.55 (0.15) C3 2.0293 (0.0039) 107.88 (0.16) 68.06 (0.16) 40.94 (0.15) 157.74 (0.16) 122.37 (0.16) C9 2.0353 (0.0036) 40.96 (0.15) 122.74 (0.17) 107.88 (0.17) 68.30 (0.15) 68.35 (0.16) 124.20 (0.16) C2 2.0384 (0.0038) 123.22 (0.16) 68.13 (0.17) 68.60 (0.17) 121.90 (0.16) 107.34 (0.17) 40.41 (0.16) 160.11 (0.15) C1 2.0387 (0.0039) 159.09 (0.17) 40.68 (0.16) 68.49 (0.17) 107.25 (0.16) 122.96 (0.17) 67.98 (0.16) 158.32 (0.15) C10 2.0438 (0.0036) 68.84 (0.15) 107.68 (0.16) 123.58 (0.16) 40.47 (0.14) 68.36 (0.15) 160.63 (0.16) 40.90 (0.14) Fe1 - C8 C5 C4 C6 C7 C3 C9 N1 - Distance Angles C12 1.3363 (0.0045) C11 1.4468 (0.0044) 123.16 (0.31) N1 - C12 N2 - Distance Angles C16 1.3552 (0.0044) C13 1.3671 (0.0042) 109.22 (0.30) N2 - C16 N3 - Distance Angles C17 1.3621 (0.0045) C18 1.4156 (0.0044) 127.96 (0.31) N3 - C17 O1 - Distance Angles C12 1.2216 (0.0041) O1 - O2 - Distance Angles C17 1.2089 (0.0040) O2 - C1 - Distance Angles C2 1.4069 (0.0056) C5 1.4134 (0.0055) 107.71 (0.37) Fe1 2.0387 (0.0039) 69.80 (0.23) 69.22 (0.23) C1 - C2 C5 C2 - Distance Angles C1 1.4069 (0.0056) C3 1.4049 (0.0055) 107.96 (0.37) Fe1 2.0384 (0.0038) 69.83 (0.23) 69.45 (0.23) C2 - C1 C3 C3 - Distance Angles C2 1.4049 (0.0056) C4 1.4197 (0.0055) 108.51 (0.37) Fe1 2.0293 (0.0039) 70.14 (0.23) 69.55 (0.22) C3 - C2 C4 C4 - Distance Angles C5 1.4032 (0.0057) C3 1.4197 (0.0055) 107.06 (0.37) Fe1 2.0299 (0.0040) 69.67 (0.23) 69.51 (0.22) C4 - C5 C3 C5 - Distance Angles C4 1.4032 (0.0057) C1 1.4134 (0.0055) 108.76 (0.37) Fe1 2.0273 (0.0040) 69.87 (0.23) 70.09 (0.23) C5 - C4 C1 C6 - Distance Angles C7 1.4063 (0.0052) C10 1.4086 (0.0050) 108.79 (0.34) Fe1 2.0284 (0.0037) 69.79 (0.22) 70.35 (0.21) C6 - C7 C10 C7 - Distance Angles C6 1.4063 (0.0052) C8 1.4050 (0.0052) 108.31 (0.35) Fe1 2.0301 (0.0038) 69.66 (0.22) 69.66 (0.22) C7 - C6 C8 C8 - Distance Angles C7 1.4050 (0.0052) C9 1.4216 (0.0052) 107.79 (0.33) Fe1 2.0278 (0.0038) 69.83 (0.22) 69.80 (0.21) C8 - C7 C9 C9 - Distance Angles C8 1.4216 (0.0052) C10 1.4253 (0.0049) 107.89 (0.33) Fe1 2.0353 (0.0036) 69.24 (0.21) 69.87 (0.21) C9 - C8 C10 C10 - Distance Angles C6 1.4086 (0.0050) C9 1.4253 (0.0049) 107.22 (0.33) C11 1.4885 (0.0050) 126.93 (0.33) 125.77 (0.33) Fe1 2.0438 (0.0036) 69.18 (0.21) 69.23 (0.20) 129.16 (0.26) C10 - C6 C9 C11 C11 - Distance Angles N1 1.4468 (0.0044) C10 1.4885 (0.0050) 113.96 (0.30) C11 - N1 C12 - Distance Angles O1 1.2216 (0.0041) N1 1.3363 (0.0045) 122.40 (0.34) C13 1.4742 (0.0050) 120.78 (0.32) 116.78 (0.33) C12 - O1 N1 C13 - Distance Angles N2 1.3671 (0.0042) C14 1.3753 (0.0048) 108.25 (0.31) C12 1.4742 (0.0050) 117.29 (0.32) 134.45 (0.32) C13 - N2 C14 C14 - Distance Angles C13 1.3753 (0.0048) C15 1.4126 (0.0048) 107.42 (0.31) C24 1.4769 (0.0048) 129.20 (0.32) 123.29 (0.33) C14 - C13 C15 C15 - Distance Angles C16 1.3875 (0.0048) C14 1.4126 (0.0048) 106.53 (0.31) C35 1.4709 (0.0049) 127.84 (0.32) 125.61 (0.31) C15 - C16 C14 C16 - Distance Angles N2 1.3552 (0.0044) C15 1.3875 (0.0048) 108.57 (0.31) C17 1.4768 (0.0049) 118.24 (0.31) 132.91 (0.33) C16 - N2 C15 C17 - Distance Angles O2 1.2089 (0.0040) N3 1.3621 (0.0045) 124.30 (0.34) C16 1.4768 (0.0049) 122.92 (0.34) 112.69 (0.31) C17 - O2 N3 C18 - Distance Angles C23 1.3733 (0.0050) C19 1.3781 (0.0051) 119.88 (0.34) N3 1.4156 (0.0044) 123.19 (0.33) 116.80 (0.33) C18 - C23 C19 C19 - Distance Angles C18 1.3781 (0.0051) C20 1.3816 (0.0053) 120.66 (0.37) C19 - C18 C20 - Distance Angles C21 1.3792 (0.0054) C19 1.3816 (0.0053) 119.02 (0.38) C20 - C21 C21 - Distance Angles C22 1.3644 (0.0053) C20 1.3792 (0.0054) 120.29 (0.37) C21 - C22 C22 - Distance Angles C21 1.3644 (0.0053) C23 1.3817 (0.0052) 120.77 (0.38) C22 - C21 C23 - Distance Angles C18 1.3733 (0.0050) C22 1.3817 (0.0052) 119.37 (0.36) C23 - C18 C24 - Distance Angles C29 1.3827 (0.0049) C25 1.3875 (0.0049) 118.49 (0.35) C14 1.4769 (0.0048) 121.35 (0.34) 120.03 (0.32) C24 - C29 C25 C25 - Distance Angles C26 1.3855 (0.0050) C24 1.3875 (0.0049) 120.35 (0.34) C25 - C26 C26 - Distance Angles C27 1.3735 (0.0050) C25 1.3855 (0.0050) 120.01 (0.36) C26 - C27 C27 - Distance Angles C28 1.3670 (0.0052) C26 1.3735 (0.0051) 120.01 (0.37) C27 - C28 C28 - Distance Angles C27 1.3670 (0.0052) C29 1.3754 (0.0051) 120.27 (0.37) C28 - C27 C29 - Distance Angles C28 1.3754 (0.0051) C24 1.3827 (0.0049) 120.85 (0.37) C29 - C28 C30 - Distance Angles C31 1.3729 (0.0052) C35 1.3960 (0.0050) 121.09 (0.37) C30 - C31 C31 - Distance Angles C30 1.3729 (0.0052) C32 1.3805 (0.0051) 120.16 (0.35) C31 - C30 C32 - Distance Angles C33 1.3716 (0.0053) C31 1.3805 (0.0051) 119.45 (0.36) C32 - C33 C33 - Distance Angles C32 1.3716 (0.0053) C34 1.3868 (0.0051) 120.59 (0.37) C33 - C32 C34 - Distance Angles C35 1.3813 (0.0048) C33 1.3868 (0.0051) 120.58 (0.34) C34 - C35 C35 - Distance Angles C34 1.3813 (0.0048) C30 1.3960 (0.0050) 118.11 (0.34) C15 1.4709 (0.0049) 121.42 (0.31) 120.46 (0.33) C35 - C34 C30 Fe2 - Distance Angles C36 2.0166 (0.0039) C42 2.0245 (0.0035) 142.74 (0.17) C37 2.0232 (0.0038) 40.51 (0.16) 112.80 (0.16) C41 2.0257 (0.0038) 112.06 (0.17) 40.85 (0.14) 107.72 (0.16) C45 2.0334 (0.0036) 108.36 (0.16) 68.93 (0.15) 132.76 (0.16) 41.03 (0.14) C43 2.0313 (0.0037) 174.81 (0.16) 40.88 (0.15) 144.62 (0.16) 68.62 (0.16) 68.57 (0.15) C40 2.0339 (0.0038) 40.60 (0.16) 175.78 (0.17) 68.34 (0.16) 143.19 (0.16) 113.53 (0.15) 136.06 (0.17) C38 2.0380 (0.0040) 67.69 (0.17) 110.11 (0.16) 40.27 (0.16) 133.61 (0.16) 172.61 (0.17) 115.84 (0.16) 67.92 (0.16) C44 2.0448 (0.0036) 134.54 (0.16) 68.51 (0.15) 173.03 (0.17) 68.49 (0.15) 40.64 (0.14) 40.49 (0.15) 110.88 (0.15) C39 2.0500 (0.0037) 67.74 (0.17) 135.82 (0.16) 67.86 (0.16) 173.78 (0.16) 145.19 (0.16) 112.18 (0.16) 40.34 (0.16) Fe2 - C36 C42 C37 C41 C45 C43 C40 N4 - Distance Angles C47 1.3394 (0.0045) C46 1.4422 (0.0044) 119.83 (0.31) N4 - C47 N5 - Distance Angles C51 1.3471 (0.0043) C48 1.3647 (0.0043) 109.93 (0.30) N5 - C51 N6 - Distance Angles C52 1.3500 (0.0044) C53 1.4121 (0.0043) 127.35 (0.31) N6 - C52 O3 - Distance Angles C47 1.2284 (0.0042) O3 - O4 - Distance Angles C52 1.2134 (0.0041) O4 - C36 - Distance Angles C37 1.3985 (0.0054) C40 1.4055 (0.0055) 108.71 (0.37) Fe2 2.0166 (0.0039) 70.00 (0.23) 70.36 (0.23) C36 - C37 C40 C37 - Distance Angles C36 1.3985 (0.0054) C38 1.3980 (0.0056) 107.71 (0.37) Fe2 2.0232 (0.0038) 69.49 (0.22) 70.44 (0.23) C37 - C36 C38 C38 - Distance Angles C37 1.3980 (0.0057) C39 1.4056 (0.0055) 108.37 (0.37) Fe2 2.0380 (0.0040) 69.29 (0.23) 70.35 (0.22) C38 - C37 C39 C39 - Distance Angles C38 1.4056 (0.0055) C40 1.4083 (0.0055) 107.88 (0.38) Fe2 2.0500 (0.0037) 69.43 (0.23) 69.22 (0.22) C39 - C38 C40 C40 - Distance Angles C36 1.4055 (0.0055) C39 1.4083 (0.0055) 107.32 (0.36) Fe2 2.0339 (0.0038) 69.04 (0.22) 70.44 (0.22) C40 - C36 C39 C41 - Distance Angles C42 1.4136 (0.0051) C45 1.4225 (0.0050) 108.13 (0.34) Fe2 2.0257 (0.0037) 69.53 (0.21) 69.78 (0.21) C41 - C42 C45 C42 - Distance Angles C41 1.4136 (0.0051) C43 1.4164 (0.0052) 107.82 (0.33) Fe2 2.0245 (0.0034) 69.62 (0.20) 69.82 (0.20) C42 - C41 C43 C43 - Distance Angles C44 1.4104 (0.0052) C42 1.4164 (0.0053) 108.25 (0.34) Fe2 2.0313 (0.0037) 70.27 (0.21) 69.30 (0.21) C43 - C44 C42 C44 - Distance Angles C43 1.4104 (0.0052) C45 1.4162 (0.0050) 108.20 (0.33) Fe2 2.0448 (0.0036) 69.24 (0.21) 69.25 (0.20) C44 - C43 C45 C45 - Distance Angles C44 1.4162 (0.0050) C41 1.4225 (0.0050) 107.60 (0.32) C46 1.4899 (0.0050) 127.40 (0.33) 124.99 (0.34) Fe2 2.0334 (0.0036) 70.12 (0.20) 69.20 (0.21) 126.97 (0.26) C45 - C44 C41 C46 C46 - Distance Angles N4 1.4422 (0.0044) C45 1.4899 (0.0050) 113.22 (0.31) C46 - N4 C47 - Distance Angles O3 1.2284 (0.0042) N4 1.3394 (0.0045) 121.27 (0.33) C48 1.4749 (0.0050) 120.19 (0.32) 118.50 (0.34) C47 - O3 N4 C48 - Distance Angles N5 1.3647 (0.0043) C49 1.3846 (0.0049) 107.74 (0.31) C47 1.4749 (0.0050) 115.81 (0.32) 136.43 (0.33) C48 - N5 C49 C49 - Distance Angles C48 1.3846 (0.0049) C50 1.4195 (0.0047) 107.15 (0.31) C64 1.4759 (0.0049) 128.13 (0.32) 124.70 (0.33) C49 - C48 C50 C50 - Distance Angles C51 1.3850 (0.0049) C49 1.4195 (0.0047) 106.47 (0.31) C70 1.4775 (0.0049) 129.32 (0.32) 124.20 (0.32) C50 - C51 C49 C51 - Distance Angles N5 1.3471 (0.0043) C50 1.3850 (0.0049) 108.68 (0.30) C52 1.4740 (0.0049) 117.04 (0.31) 134.21 (0.33) C51 - N5 C50 C52 - Distance Angles O4 1.2134 (0.0041) N6 1.3500 (0.0044) 123.65 (0.34) C51 1.4740 (0.0049) 120.92 (0.33) 115.43 (0.32) C52 - O4 N6 C53 - Distance Angles C54 1.3770 (0.0051) C58 1.3861 (0.0051) 120.21 (0.34) N6 1.4121 (0.0043) 122.34 (0.34) 117.41 (0.32) C53 - C54 C58 C54 - Distance Angles C53 1.3770 (0.0051) C55 1.3884 (0.0052) 118.73 (0.37) C54 - C53 C55 - Distance Angles C56 1.3737 (0.0054) C54 1.3884 (0.0051) 121.40 (0.37) C55 - C56 C56 - Distance Angles C55 1.3737 (0.0054) C57 1.3801 (0.0055) 119.44 (0.36) C56 - C55 C57 - Distance Angles C56 1.3801 (0.0055) C58 1.3787 (0.0052) 119.87 (0.38) C57 - C56 C58 - Distance Angles C57 1.3787 (0.0052) C53 1.3861 (0.0051) 120.34 (0.36) C58 - C57 C59 - Distance Angles C64 1.3816 (0.0047) C60 1.3778 (0.0050) 121.20 (0.35) C59 - C64 C60 - Distance Angles C61 1.3724 (0.0051) C59 1.3778 (0.0050) 119.61 (0.35) C60 - C61 C61 - Distance Angles C60 1.3724 (0.0051) C62 1.3843 (0.0050) 120.24 (0.35) C61 - C60 C62 - Distance Angles C63 1.3676 (0.0051) C61 1.3843 (0.0050) 119.88 (0.35) C62 - C63 C63 - Distance Angles C62 1.3676 (0.0051) C64 1.3968 (0.0049) 120.76 (0.35) C63 - C62 C64 - Distance Angles C59 1.3816 (0.0047) C63 1.3968 (0.0049) 118.24 (0.33) C49 1.4759 (0.0049) 121.98 (0.32) 119.77 (0.32) C64 - C59 C63 C65 - Distance Angles C66 1.3781 (0.0051) C70 1.3887 (0.0050) 121.02 (0.39) C65 - C66 C66 - Distance Angles C67 1.3682 (0.0055) C65 1.3781 (0.0051) 120.44 (0.38) C66 - C67 C67 - Distance Angles C66 1.3682 (0.0055) C68 1.3835 (0.0058) 119.48 (0.39) C67 - C66 C68 - Distance Angles C69 1.3789 (0.0053) C67 1.3835 (0.0058) 119.89 (0.40) C68 - C69 C69 - Distance Angles C68 1.3789 (0.0053) C70 1.3817 (0.0050) 121.33 (0.37) C69 - C68 C70 - Distance Angles C69 1.3817 (0.0050) C65 1.3887 (0.0050) 117.82 (0.36) C50 1.4775 (0.0049) 120.70 (0.32) 121.43 (0.34) C70 - C69 C65 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 1.98 2.843(4) 168.5 N2-H2...O1_$1 0.88 2.22 2.900(4) 133.5 N5-H5A...O3_$2 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)