+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 14:08:45 on 23-Jan-2002 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 02SOT007 in Pn CELL 0.71073 13.2385 16.9228 15.0678 90.000 99.944 90.000 ZERR 2 0.0004 0.0005 0.0004 0.000 0.002 0.000 LATT -1 SYMM 1/2 + X, - Y, 1/2 + Z SFAC C H N O CL UNIT 136 192 16 8 8 V = 3324.96 F(000) = 1320.0 Mu = 0.23 mm-1 Cell Wt = 2462.66 Rho = 1.230 SHEL 7 0.84 OMIT 0 1 -2 FMAP 2 PLAN 60 ACTA SIZE 0.15 0.15 0.1 TEMP -153 MPLA N5 C26 C27 C28 C29 5 H14 H5 MPLA N2 C8 C9 C10 C11 5 H32 H23 HTAB N1 N5 HTAB N3 N5 HTAB N4 N2 HTAB N6 N2 HTAB L.S. 1 WGHT 0.034500 EXTI 0.003416 FVAR 0.18992 MOLE 1 C1 1 0.558447 0.720373 0.817154 11.00000 0.02702 0.03357 = 0.02329 -0.00409 0.00113 -0.00278 AFIX 43 H1 2 0.582148 0.685707 0.775599 11.00000 -1.20000 AFIX 0 C2 1 0.622299 0.740044 0.897309 11.00000 0.02472 0.04169 = 0.03371 -0.00277 -0.00271 -0.00040 AFIX 43 H2 2 0.690330 0.720003 0.909170 11.00000 -1.20000 AFIX 0 C3 1 0.588498 0.788045 0.959652 11.00000 0.03215 0.03383 = 0.02687 -0.00799 -0.00698 -0.00395 AFIX 43 H3 2 0.632137 0.800384 1.014821 11.00000 -1.20000 AFIX 0 C4 1 0.490929 0.817838 0.941058 11.00000 0.03277 0.03371 = 0.02441 -0.00777 0.00415 -0.00404 AFIX 43 H4 2 0.467193 0.851418 0.983618 11.00000 -1.20000 AFIX 0 C5 1 0.426618 0.799841 0.861508 11.00000 0.01794 0.03201 = 0.02753 -0.00584 0.00586 -0.00279 AFIX 43 H5 2 0.358967 0.820649 0.850015 11.00000 -1.20000 AFIX 0 C6 1 0.460403 0.751276 0.797904 11.00000 0.01782 0.02829 = 0.02645 0.00498 0.00498 -0.00640 C7 1 0.416189 0.709862 0.636525 11.00000 0.02290 0.01884 = 0.02392 0.00090 0.00015 0.00027 C8 1 0.324550 0.696826 0.567311 11.00000 0.02031 0.02017 = 0.02021 0.00099 0.00119 -0.00238 C9 1 0.161443 0.691624 0.510186 11.00000 0.02121 0.02010 = 0.01958 0.00014 0.00250 0.00180 C10 1 0.214624 0.675854 0.440037 11.00000 0.02569 0.02023 = 0.01983 -0.00312 0.00168 0.00260 C11 1 0.318640 0.679891 0.476081 11.00000 0.01872 0.02735 = 0.01816 0.00081 0.00838 0.00132 C12 1 0.050703 0.695543 0.509012 11.00000 0.02098 0.01729 = 0.02237 0.00319 -0.00040 -0.00190 C13 1 -0.073255 0.726262 0.613384 11.00000 0.01629 0.02507 = 0.03107 0.00529 0.00665 -0.00017 C14 1 -0.077255 0.763503 0.695193 11.00000 0.02021 0.03968 = 0.03251 0.00055 0.00652 -0.00343 AFIX 43 H14 2 -0.015918 0.780533 0.732636 11.00000 -1.20000 AFIX 0 C15 1 -0.171400 0.775541 0.721585 11.00000 0.02982 0.04754 = 0.03165 -0.00344 0.00889 0.00239 AFIX 43 H15 2 -0.174265 0.800767 0.777419 11.00000 -1.20000 AFIX 0 C16 1 -0.260855 0.751251 0.667574 11.00000 0.02333 0.04387 = 0.04403 0.00703 0.01352 0.00616 AFIX 43 H16 2 -0.325340 0.760811 0.685095 11.00000 -1.20000 AFIX 0 C17 1 -0.255479 0.712968 0.587938 11.00000 0.01571 0.04230 = 0.04093 0.01166 0.00444 -0.00399 AFIX 43 H17 2 -0.316973 0.695190 0.551324 11.00000 -1.20000 AFIX 0 C18 1 -0.161700 0.699557 0.559512 11.00000 0.01999 0.02666 = 0.03083 0.00695 0.00171 0.00135 AFIX 43 H18 2 -0.158995 0.672769 0.504564 11.00000 -1.20000 AFIX 0 C53 1 0.866852 0.465805 0.720963 11.00000 0.02241 0.02837 = 0.01818 0.00456 -0.00078 0.00250 AFIX 23 H53A 2 0.810191 0.446949 0.750629 11.00000 -1.20000 H53B 2 0.929210 0.435972 0.747217 11.00000 -1.20000 AFIX 0 C54 1 0.885022 0.552376 0.743325 11.00000 0.02539 0.03131 = 0.02096 0.00080 0.00022 -0.00277 AFIX 23 H54A 2 0.829745 0.584371 0.707785 11.00000 -1.20000 H54B 2 0.951066 0.569116 0.726948 11.00000 -1.20000 AFIX 0 C55 1 0.887226 0.566721 0.843849 11.00000 0.02817 0.03373 = 0.02334 -0.00064 -0.00263 0.00182 AFIX 23 H55A 2 0.935384 0.528793 0.878824 11.00000 -1.20000 H55B 2 0.913492 0.620656 0.859272 11.00000 -1.20000 AFIX 0 C56 1 0.783180 0.558058 0.871320 11.00000 0.03292 0.04489 = 0.02988 -0.00907 0.00879 0.00368 AFIX 137 H56A 2 0.733406 0.591623 0.832888 11.00000 -1.50000 H56B 2 0.787619 0.574147 0.934354 11.00000 -1.50000 H56C 2 0.761092 0.502791 0.864521 11.00000 -1.50000 AFIX 0 C57 1 0.745262 0.490083 0.577370 11.00000 0.01707 0.02469 = 0.01984 -0.00288 0.00001 -0.00114 AFIX 23 H57A 2 0.726595 0.471387 0.514412 11.00000 -1.20000 H57B 2 0.762512 0.546886 0.575082 11.00000 -1.20000 AFIX 0 C58 1 0.651556 0.482233 0.622337 11.00000 0.02417 0.03494 = 0.02486 0.00403 0.00352 0.00593 AFIX 23 H58A 2 0.641770 0.426239 0.637891 11.00000 -1.20000 H58B 2 0.661289 0.513619 0.678616 11.00000 -1.20000 AFIX 0 C59 1 0.558935 0.511437 0.558899 11.00000 0.02279 0.05167 = 0.02231 0.00174 0.00388 0.00347 AFIX 23 H59A 2 0.552154 0.480871 0.502156 11.00000 -1.20000 H59B 2 0.570101 0.567441 0.544246 11.00000 -1.20000 AFIX 0 C60 1 0.459743 0.505205 0.595000 11.00000 0.02178 0.03388 = 0.03683 -0.00011 0.00386 0.00582 AFIX 137 H60A 2 0.447898 0.450003 0.609973 11.00000 -1.50000 H60B 2 0.402954 0.523737 0.549213 11.00000 -1.50000 H60C 2 0.463973 0.537829 0.649253 11.00000 -1.50000 AFIX 0 C61 1 0.816988 0.358332 0.611231 11.00000 0.02585 0.02193 = 0.02262 -0.00440 0.00530 -0.00211 AFIX 23 H61A 2 0.764922 0.345500 0.648928 11.00000 -1.20000 H61B 2 0.785499 0.348146 0.547773 11.00000 -1.20000 AFIX 0 C62 1 0.905725 0.302325 0.636016 11.00000 0.03212 0.03044 = 0.03586 -0.00099 0.00845 0.00289 AFIX 23 H62A 2 0.941230 0.313864 0.698015 11.00000 -1.20000 H62B 2 0.955333 0.310215 0.594600 11.00000 -1.20000 AFIX 0 C63 1 0.869463 0.217419 0.630589 11.00000 0.03456 0.03003 = 0.03128 -0.00012 0.00640 0.00684 AFIX 23 H63A 2 0.930184 0.182301 0.640079 11.00000 -1.20000 H63B 2 0.831273 0.207343 0.569148 11.00000 -1.20000 AFIX 0 C64 1 0.800636 0.195610 0.698995 11.00000 0.05657 0.03149 = 0.03839 -0.00090 0.01808 -0.00120 AFIX 137 H64A 2 0.832591 0.213774 0.759063 11.00000 -1.50000 H64B 2 0.791779 0.138135 0.699802 11.00000 -1.50000 H64C 2 0.733567 0.220988 0.681821 11.00000 -1.50000 AFIX 0 C65 1 0.928047 0.470148 0.575073 11.00000 0.02077 0.02788 = 0.02471 0.00356 0.00795 -0.00251 AFIX 23 H65A 2 0.990108 0.440885 0.603257 11.00000 -1.20000 H65B 2 0.941687 0.527086 0.586531 11.00000 -1.20000 AFIX 0 C66 1 0.912163 0.456348 0.474098 11.00000 0.02417 0.04053 = 0.02626 -0.00145 0.00675 -0.00115 AFIX 23 H66A 2 0.891997 0.400661 0.461002 11.00000 -1.20000 H66B 2 0.855820 0.490548 0.444006 11.00000 -1.20000 AFIX 0 C67 1 1.008923 0.474202 0.436872 11.00000 0.02826 0.03332 = 0.02767 -0.00261 0.01032 0.00177 AFIX 23 H67A 2 1.059648 0.431521 0.454169 11.00000 -1.20000 H67B 2 1.039229 0.524352 0.462840 11.00000 -1.20000 AFIX 0 C68 1 0.984686 0.480978 0.334275 11.00000 0.03532 0.04248 = 0.02691 0.00225 0.00854 -0.00188 AFIX 137 H68A 2 0.949702 0.432904 0.309008 11.00000 -1.50000 H68B 2 1.048612 0.487599 0.310591 11.00000 -1.50000 H68C 2 0.940200 0.526778 0.317421 11.00000 -1.50000 AFIX 0 N1 3 0.392169 0.734024 0.717703 11.00000 0.01202 0.03771 = 0.01960 -0.00340 0.00209 -0.00205 AFIX 43 H1A 2 0.326464 0.739299 0.719679 11.00000 -1.20000 AFIX 0 N2 3 0.228782 0.704541 0.587645 11.00000 0.01693 0.02311 = 0.01962 -0.00122 0.00428 0.00160 N3 3 0.026439 0.717475 0.590571 11.00000 0.00968 0.03335 = 0.02032 0.00019 0.00159 -0.00110 AFIX 43 H3A 2 0.078549 0.727276 0.633918 11.00000 -1.20000 AFIX 0 N8 3 0.840709 0.446137 0.621146 11.00000 0.02145 0.02284 = 0.01861 -0.00163 0.00333 -0.00099 O1 4 0.504202 0.699587 0.623729 11.00000 0.01595 0.04454 = 0.03110 -0.00420 0.00668 -0.00133 O2 4 -0.013406 0.681664 0.442288 11.00000 0.01980 0.03648 = 0.02409 -0.00179 -0.00091 0.00169 CL1 5 0.417297 0.668365 0.415439 11.00000 0.02420 0.04476 = 0.02442 -0.00103 0.00933 0.00518 CL2 5 0.164596 0.658309 0.327856 11.00000 0.02818 0.04070 = 0.01928 -0.00199 0.00180 0.00373 MOLE 2 C19 1 0.155705 0.483596 0.805823 11.00000 0.02392 0.02843 = 0.02733 0.00443 0.00768 -0.00270 AFIX 43 H19 2 0.133722 0.499882 0.859747 11.00000 -1.20000 AFIX 0 C20 1 0.158912 0.404563 0.785955 11.00000 0.03273 0.03853 = 0.03768 0.01459 0.00872 -0.00231 AFIX 43 H20 2 0.140824 0.366523 0.826854 11.00000 -1.20000 AFIX 0 C21 1 0.188625 0.379886 0.705952 11.00000 0.02925 0.02571 = 0.04602 0.00124 0.00631 -0.00147 AFIX 43 H21 2 0.190014 0.325256 0.691705 11.00000 -1.20000 AFIX 0 C22 1 0.215945 0.435715 0.647816 11.00000 0.02458 0.03215 = 0.03027 0.00046 0.00252 -0.00062 AFIX 43 H22 2 0.236165 0.419342 0.593171 11.00000 -1.20000 AFIX 0 C23 1 0.214231 0.514558 0.668048 11.00000 0.02022 0.03041 = 0.03155 0.00357 0.00662 -0.00090 AFIX 43 H23 2 0.233604 0.552246 0.627372 11.00000 -1.20000 AFIX 0 C24 1 0.184379 0.540229 0.747682 11.00000 0.00815 0.03057 = 0.02991 0.00354 -0.00136 0.00308 C25 1 0.166252 0.660715 0.838952 11.00000 0.01390 0.04083 = 0.01858 0.00361 -0.00004 0.00013 C26 1 0.163609 0.747050 0.830776 11.00000 0.01714 0.03249 = 0.01918 0.00015 0.00024 -0.00049 C27 1 0.167899 0.863136 0.767474 11.00000 0.02117 0.02751 = 0.01955 -0.00317 0.00410 -0.00652 C28 1 0.142119 0.875495 0.852108 11.00000 0.01785 0.03075 = 0.03138 -0.00914 0.00340 -0.00320 C29 1 0.140126 0.802940 0.892283 11.00000 0.01927 0.04150 = 0.01568 0.00055 0.00462 -0.00195 C30 1 0.183522 0.921480 0.699088 11.00000 0.01911 0.02650 = 0.03067 -0.00215 0.00502 -0.00498 C31 1 0.246717 0.933030 0.553052 11.00000 0.01827 0.02298 = 0.02599 -0.00379 0.00063 -0.00325 C32 1 0.286694 0.889087 0.489723 11.00000 0.05043 0.02428 = 0.02710 -0.00054 0.01410 -0.00100 AFIX 43 H32 2 0.287182 0.833066 0.493817 11.00000 -1.20000 AFIX 0 C33 1 0.325869 0.925120 0.420729 11.00000 0.06596 0.03359 = 0.03410 -0.00264 0.02149 0.00005 AFIX 43 H33 2 0.353422 0.894004 0.378163 11.00000 -1.20000 AFIX 0 C34 1 0.324890 1.005697 0.413853 11.00000 0.05142 0.03630 = 0.03773 0.00481 0.01769 -0.00916 AFIX 43 H34 2 0.352070 1.030781 0.366710 11.00000 -1.20000 AFIX 0 C35 1 0.284502 1.050110 0.475308 11.00000 0.05087 0.02606 = 0.03487 -0.00043 0.00682 -0.00167 AFIX 43 H35 2 0.282990 1.106044 0.469880 11.00000 -1.20000 AFIX 0 C36 1 0.245879 1.014586 0.545187 11.00000 0.03876 0.03086 = 0.02983 -0.00735 0.01379 -0.00247 AFIX 43 H36 2 0.218830 1.046122 0.587695 11.00000 -1.20000 AFIX 0 N4 3 0.182632 0.622175 0.762315 11.00000 0.02640 0.02501 = 0.02273 0.00517 0.00412 -0.00234 AFIX 43 H4A 2 0.193242 0.652334 0.717242 11.00000 -1.20000 AFIX 0 N5 3 0.180124 0.784120 0.754257 11.00000 0.01714 0.02502 = 0.02272 -0.00166 0.00317 -0.00096 N6 3 0.212503 0.891341 0.622563 11.00000 0.03745 0.01923 = 0.02890 -0.00545 0.01534 -0.00462 AFIX 43 H6 2 0.209167 0.839641 0.616495 11.00000 -1.20000 AFIX 0 O3 4 0.154768 0.626465 0.907910 11.00000 0.04058 0.03842 = 0.02247 0.00733 0.00832 0.00714 O4 4 0.171183 0.992864 0.710154 11.00000 0.05386 0.02880 = 0.03562 -0.01054 0.02000 -0.00895 CL3 5 0.109479 0.787365 0.997452 11.00000 0.04612 0.05763 = 0.02530 0.00126 0.01724 0.00688 CL4 5 0.117535 0.964021 0.902102 11.00000 0.05744 0.03714 = 0.04145 -0.01183 0.02470 -0.00025 MOLE 3 C37 1 0.985988 0.896325 0.425580 11.00000 0.05699 0.03489 = 0.03364 -0.00322 0.00982 0.00388 AFIX 23 H37A 2 0.976441 0.844695 0.453900 11.00000 -1.20000 H37B 2 1.059841 0.901427 0.422665 11.00000 -1.20000 AFIX 0 C38 1 0.958354 0.960574 0.486819 11.00000 0.09567 0.04101 = 0.03624 -0.00144 0.01123 0.01595 AFIX 23 H38A 2 1.020335 0.992903 0.507248 11.00000 -1.20000 H38B 2 0.906672 0.995410 0.450947 11.00000 -1.20000 AFIX 0 C39 1 0.919606 0.935408 0.563355 11.00000 0.14792 0.05036 = 0.05438 0.00060 0.04726 0.02913 AFIX 23 H39A 2 0.970423 0.898961 0.597661 11.00000 -1.20000 H39B 2 0.856628 0.904351 0.542403 11.00000 -1.20000 AFIX 0 C40 1 0.894217 0.997268 0.627522 11.00000 0.09578 0.04626 = 0.05344 -0.01434 0.03607 -0.00448 AFIX 137 H40A 2 0.956887 1.025427 0.654019 11.00000 -1.50000 H40B 2 0.864345 0.971946 0.675460 11.00000 -1.50000 H40C 2 0.844852 1.034794 0.594956 11.00000 -1.50000 AFIX 0 C41 1 0.813306 0.889759 0.329204 11.00000 0.04581 0.02849 = 0.04258 0.00785 0.01483 0.00982 AFIX 23 H41A 2 0.777343 0.897202 0.266490 11.00000 -1.20000 H41B 2 0.793197 0.933927 0.365564 11.00000 -1.20000 AFIX 0 C42 1 0.777001 0.813255 0.364816 11.00000 0.04113 0.03773 = 0.03353 0.00379 -0.00006 0.00365 AFIX 23 H42A 2 0.822603 0.799165 0.421826 11.00000 -1.20000 H42B 2 0.781225 0.770456 0.320814 11.00000 -1.20000 AFIX 0 C43 1 0.666589 0.819894 0.381643 11.00000 0.05737 0.03414 = 0.04382 0.00750 0.01069 0.00026 AFIX 23 H43A 2 0.648102 0.770544 0.410285 11.00000 -1.20000 H43B 2 0.662326 0.863846 0.424200 11.00000 -1.20000 AFIX 0 C44 1 0.590291 0.834133 0.296651 11.00000 0.04755 0.04500 = 0.04765 0.00312 0.00431 0.00210 AFIX 137 H44A 2 0.604247 0.885339 0.270896 11.00000 -1.50000 H44B 2 0.520727 0.834182 0.310714 11.00000 -1.50000 H44C 2 0.596289 0.792137 0.253080 11.00000 -1.50000 AFIX 0 C45 1 0.963932 0.823002 0.283992 11.00000 0.03390 0.02693 = 0.03146 -0.00353 0.00401 0.00630 AFIX 23 H45A 2 1.038754 0.828082 0.285769 11.00000 -1.20000 H45B 2 0.952526 0.775289 0.318974 11.00000 -1.20000 AFIX 0 C46 1 0.912896 0.810565 0.187154 11.00000 0.04308 0.03671 = 0.02856 0.00161 0.00431 0.00124 AFIX 23 H46A 2 0.931796 0.854486 0.149821 11.00000 -1.20000 H46B 2 0.837521 0.811536 0.183525 11.00000 -1.20000 AFIX 0 C47 1 0.943888 0.732832 0.149715 11.00000 0.03301 0.03191 = 0.02864 -0.00274 0.00499 -0.00567 AFIX 23 H47A 2 1.018255 0.733791 0.147811 11.00000 -1.20000 H47B 2 0.930946 0.689245 0.190119 11.00000 -1.20000 AFIX 0 C48 1 0.885074 0.717660 0.056223 11.00000 0.05071 0.04365 = 0.02751 0.00310 -0.00288 -0.00334 AFIX 137 H48A 2 0.811578 0.714888 0.058301 11.00000 -1.50000 H48B 2 0.907611 0.667528 0.033572 11.00000 -1.50000 H48C 2 0.897845 0.760712 0.016089 11.00000 -1.50000 AFIX 0 C49 1 0.947954 0.970559 0.280721 11.00000 0.05836 0.02304 = 0.04405 0.00510 0.01962 0.00094 AFIX 23 H49A 2 0.909162 0.967914 0.218434 11.00000 -1.20000 H49B 2 0.920733 1.015830 0.310895 11.00000 -1.20000 AFIX 0 C50 1 1.059637 0.986770 0.276194 11.00000 0.08244 0.06686 = 0.07401 0.02771 0.03319 -0.01562 AFIX 23 H50A 2 1.098387 0.991938 0.338275 11.00000 -1.20000 H50B 2 1.088015 0.940994 0.247780 11.00000 -1.20000 AFIX 0 C51 1 1.075640 1.060835 0.223700 11.00000 0.11016 0.04926 = 0.09553 -0.00921 0.05551 -0.01131 AFIX 23 H51A 2 1.035982 1.104562 0.244649 11.00000 -1.20000 H51B 2 1.149083 1.075528 0.237101 11.00000 -1.20000 AFIX 0 C52 1 1.047090 1.053068 0.133004 11.00000 0.20741 0.16148 = 0.08013 0.05226 -0.04211 -0.06423 AFIX 137 H52A 2 1.054615 0.997788 0.115898 11.00000 -1.50000 H52B 2 1.090730 1.086568 0.102366 11.00000 -1.50000 H52C 2 0.975349 1.069252 0.115390 11.00000 -1.50000 AFIX 0 N7 3 0.927242 0.894565 0.330193 11.00000 0.04292 0.02517 = 0.02844 0.00468 0.00618 0.00525 HKLF 4 Covalent radii and connectivity table for 02SOT007 in Pn C 0.770 H 0.320 N 0.700 O 0.660 CL 0.990 C1 - C6 C2 C2 - C3 C1 C3 - C4 C2 C4 - C3 C5 C5 - C4 C6 C6 - C1 C5 N1 C7 - O1 N1 C8 C8 - N2 C11 C7 C9 - N2 C10 C12 C10 - C11 C9 Cl2 C11 - C10 C8 Cl1 C12 - O2 N3 C9 C13 - C18 C14 N3 C14 - C15 C13 C15 - C16 C14 C16 - C17 C15 C17 - C16 C18 C18 - C13 C17 C53 - C54 N8 C54 - C53 C55 C55 - C56 C54 C56 - C55 C57 - N8 C58 C58 - C59 C57 C59 - C58 C60 C60 - C59 C61 - C62 N8 C62 - C61 C63 C63 - C62 C64 C64 - C63 C65 - N8 C66 C66 - C67 C65 C67 - C66 C68 C68 - C67 N1 - C7 C6 N2 - C9 C8 N3 - C12 C13 N8 - C65 C57 C61 C53 O1 - C7 O2 - C12 Cl1 - C11 Cl2 - C10 C19 - C20 C24 C20 - C19 C21 C21 - C22 C20 C22 - C23 C21 C23 - C22 C24 C24 - C19 C23 N4 C25 - O3 N4 C26 C26 - N5 C29 C25 C27 - N5 C28 C30 C28 - C29 C27 Cl4 C29 - C28 C26 Cl3 C30 - O4 N6 C27 C31 - C32 C36 N6 C32 - C33 C31 C33 - C34 C32 C34 - C33 C35 C35 - C34 C36 C36 - C35 C31 N4 - C25 C24 N5 - C26 C27 N6 - C30 C31 O3 - C25 O4 - C30 Cl3 - C29 Cl4 - C28 C37 - C38 N7 C38 - C39 C37 C39 - C38 C40 C40 - C39 C41 - N7 C42 C42 - C41 C43 C43 - C44 C42 C44 - C43 C45 - C46 N7 C46 - C45 C47 C47 - C48 C46 C48 - C47 C49 - C50 N7 C50 - C51 C49 C51 - C52 C50 C52 - C51 N7 - C41 C37 C45 C49 Floating origin restraints generated 22399 Reflections read, of which 3305 rejected -15 =< h =< 14, -20 =< k =< 20, -17 =< l =< 17, Max. 2-theta = 50.05 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -7 5 -12 9.28 0.97 2 4.97 3 6 -12 16.25 0.87 3 6.28 -4 3 -10 20.18 0.99 2 22.40 -3 3 -10 13.37 0.83 3 4.52 -5 4 -10 18.88 0.92 3 8.69 2 5 -10 41.06 0.98 3 24.69 3 10 -10 15.05 0.97 2 13.77 0 3 -8 52.34 1.70 3 17.86 -4 4 -8 42.41 0.90 4 9.81 1 4 -8 33.53 0.80 4 6.80 -5 5 -8 52.10 1.00 3 30.12 -6 6 -8 22.62 0.96 3 11.63 2 10 -8 16.06 0.96 2 15.32 2 11 -8 10.61 0.91 2 6.66 1 10 -7 8.85 0.87 3 5.14 -2 2 -6 50.16 1.76 3 9.95 1 3 -6 61.79 1.62 4 8.46 1 8 -6 19.35 0.96 2 15.81 -2 3 -5 27.46 0.88 3 9.66 1 3 -5 408.58 12.13 3 76.08 1 6 -5 146.67 4.52 3 24.27 -1 7 -4 127.11 3.38 4 18.10 -1 2 -3 48.80 1.01 2 45.91 0 2 -3 204.90 5.15 3 53.84 -1 5 -3 67.58 1.91 3 16.17 -1 2 -1 24.70 0.59 3 5.08 26 Inconsistent equivalents 10094 Unique reflections, of which 0 suppressed R(int) = 0.0588 R(sigma) = 0.0981 Friedel opposites not merged Maximum memory for data reduction = 7512 / 102364 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 = 9859 / 1102162 wR2 = 0.0983 before cycle 1 for 10094 data and 766 / 766 parameters GooF = S = 0.987; Restrained GooF = 0.987 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0345 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.18992 0.00023 0.013 OSF 2 0.00342 0.00039 0.000 EXTI Mean shift/esd = 0.001 Maximum = 0.013 for OSF Max. shift = 0.000 A for H52A Max. dU = 0.000 for C51 Largest correlation matrix elements 0.562 EXTI / OSF Idealized hydrogen atom generation before cycle 2 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.5821 0.6857 0.7756 43 0.950 0.000 C1 C6 C2 H2 0.6903 0.7200 0.9092 43 0.950 0.000 C2 C3 C1 H3 0.6321 0.8004 1.0148 43 0.950 0.000 C3 C4 C2 H4 0.4672 0.8514 0.9836 43 0.950 0.000 C4 C3 C5 H5 0.3590 0.8206 0.8500 43 0.950 0.000 C5 C4 C6 H14 -0.0159 0.7805 0.7326 43 0.950 0.000 C14 C15 C13 H15 -0.1743 0.8008 0.7774 43 0.950 0.000 C15 C16 C14 H16 -0.3253 0.7608 0.6851 43 0.950 0.000 C16 C17 C15 H17 -0.3170 0.6952 0.5513 43 0.950 0.000 C17 C16 C18 H18 -0.1590 0.6728 0.5046 43 0.950 0.000 C18 C13 C17 H53A 0.8102 0.4469 0.7506 23 0.990 0.000 C53 C54 N8 H53B 0.9292 0.4360 0.7472 23 0.990 0.000 C53 C54 N8 H54A 0.8297 0.5844 0.7078 23 0.990 0.000 C54 C53 C55 H54B 0.9511 0.5691 0.7269 23 0.990 0.000 C54 C53 C55 H55A 0.9354 0.5288 0.8788 23 0.990 0.000 C55 C56 C54 H55B 0.9135 0.6207 0.8593 23 0.990 0.000 C55 C56 C54 H56A 0.7334 0.5916 0.8329 137 0.980 0.000 C56 C55 H56A H56B 0.7876 0.5741 0.9344 137 0.980 0.000 C56 C55 H56A H56C 0.7611 0.5028 0.8645 137 0.980 0.000 C56 C55 H56A H57A 0.7266 0.4714 0.5144 23 0.990 0.000 C57 N8 C58 H57B 0.7625 0.5469 0.5751 23 0.990 0.000 C57 N8 C58 H58A 0.6418 0.4262 0.6379 23 0.990 0.000 C58 C59 C57 H58B 0.6613 0.5136 0.6786 23 0.990 0.000 C58 C59 C57 H59A 0.5522 0.4809 0.5022 23 0.990 0.000 C59 C58 C60 H59B 0.5701 0.5674 0.5442 23 0.990 0.000 C59 C58 C60 H60A 0.4479 0.4500 0.6100 137 0.980 0.000 C60 C59 H60A H60B 0.4030 0.5237 0.5492 137 0.980 0.000 C60 C59 H60A H60C 0.4640 0.5378 0.6493 137 0.980 0.000 C60 C59 H60A H61A 0.7649 0.3455 0.6489 23 0.990 0.000 C61 C62 N8 H61B 0.7855 0.3481 0.5478 23 0.990 0.000 C61 C62 N8 H62A 0.9412 0.3139 0.6980 23 0.990 0.000 C62 C61 C63 H62B 0.9553 0.3102 0.5946 23 0.990 0.000 C62 C61 C63 H63A 0.9302 0.1823 0.6401 23 0.990 0.000 C63 C62 C64 H63B 0.8313 0.2073 0.5691 23 0.990 0.000 C63 C62 C64 H64A 0.8326 0.2138 0.7591 137 0.980 0.000 C64 C63 H64A H64B 0.7918 0.1381 0.6998 137 0.980 0.000 C64 C63 H64A H64C 0.7336 0.2210 0.6818 137 0.980 0.000 C64 C63 H64A H65A 0.9901 0.4409 0.6033 23 0.990 0.000 C65 N8 C66 H65B 0.9417 0.5271 0.5865 23 0.990 0.000 C65 N8 C66 H66A 0.8920 0.4007 0.4610 23 0.990 0.000 C66 C67 C65 H66B 0.8558 0.4905 0.4440 23 0.990 0.000 C66 C67 C65 H67A 1.0596 0.4315 0.4542 23 0.990 0.000 C67 C66 C68 H67B 1.0392 0.5244 0.4628 23 0.990 0.000 C67 C66 C68 H68A 0.9497 0.4329 0.3090 137 0.980 0.000 C68 C67 H68A H68B 1.0486 0.4876 0.3106 137 0.980 0.000 C68 C67 H68A H68C 0.9402 0.5268 0.3174 137 0.980 0.000 C68 C67 H68A H1A 0.3265 0.7393 0.7197 43 0.880 0.000 N1 C7 C6 H3A 0.0785 0.7273 0.6339 43 0.880 0.000 N3 C12 C13 H19 0.1337 0.4999 0.8597 43 0.950 0.000 C19 C20 C24 H20 0.1408 0.3665 0.8269 43 0.950 0.000 C20 C19 C21 H21 0.1900 0.3253 0.6917 43 0.950 0.000 C21 C22 C20 H22 0.2362 0.4193 0.5932 43 0.950 0.000 C22 C23 C21 H23 0.2336 0.5522 0.6274 43 0.950 0.000 C23 C22 C24 H32 0.2872 0.8331 0.4938 43 0.950 0.000 C32 C33 C31 H33 0.3534 0.8940 0.3782 43 0.950 0.000 C33 C34 C32 H34 0.3521 1.0308 0.3667 43 0.950 0.000 C34 C33 C35 H35 0.2830 1.1060 0.4699 43 0.950 0.000 C35 C34 C36 H36 0.2188 1.0461 0.5877 43 0.950 0.000 C36 C35 C31 H4A 0.1932 0.6523 0.7172 43 0.880 0.000 N4 C25 C24 H6 0.2092 0.8396 0.6165 43 0.880 0.000 N6 C30 C31 H37A 0.9764 0.8447 0.4539 23 0.990 0.000 C37 C38 N7 H37B 1.0598 0.9014 0.4227 23 0.990 0.000 C37 C38 N7 H38A 1.0203 0.9929 0.5072 23 0.990 0.000 C38 C39 C37 H38B 0.9067 0.9954 0.4509 23 0.990 0.000 C38 C39 C37 H39A 0.9704 0.8990 0.5977 23 0.990 0.000 C39 C38 C40 H39B 0.8566 0.9044 0.5424 23 0.990 0.000 C39 C38 C40 H40A 0.9569 1.0254 0.6540 137 0.980 0.000 C40 C39 H40A H40B 0.8643 0.9719 0.6755 137 0.980 0.000 C40 C39 H40A H40C 0.8449 1.0348 0.5950 137 0.980 0.000 C40 C39 H40A H41A 0.7773 0.8972 0.2665 23 0.990 0.000 C41 N7 C42 H41B 0.7932 0.9339 0.3656 23 0.990 0.000 C41 N7 C42 H42A 0.8226 0.7992 0.4218 23 0.990 0.000 C42 C41 C43 H42B 0.7812 0.7705 0.3208 23 0.990 0.000 C42 C41 C43 H43A 0.6481 0.7705 0.4103 23 0.990 0.000 C43 C44 C42 H43B 0.6623 0.8638 0.4242 23 0.990 0.000 C43 C44 C42 H44A 0.6042 0.8853 0.2709 137 0.980 0.000 C44 C43 H44A H44B 0.5207 0.8342 0.3107 137 0.980 0.000 C44 C43 H44A H44C 0.5963 0.7921 0.2531 137 0.980 0.000 C44 C43 H44A H45A 1.0388 0.8281 0.2858 23 0.990 0.000 C45 C46 N7 H45B 0.9525 0.7753 0.3190 23 0.990 0.000 C45 C46 N7 H46A 0.9318 0.8545 0.1498 23 0.990 0.000 C46 C45 C47 H46B 0.8375 0.8115 0.1835 23 0.990 0.000 C46 C45 C47 H47A 1.0183 0.7338 0.1478 23 0.990 0.000 C47 C48 C46 H47B 0.9309 0.6892 0.1901 23 0.990 0.000 C47 C48 C46 H48A 0.8116 0.7149 0.0583 137 0.980 0.000 C48 C47 H48A H48B 0.9076 0.6675 0.0336 137 0.980 0.000 C48 C47 H48A H48C 0.8978 0.7607 0.0161 137 0.980 0.000 C48 C47 H48A H49A 0.9092 0.9679 0.2184 23 0.990 0.000 C49 C50 N7 H49B 0.9207 1.0158 0.3109 23 0.990 0.000 C49 C50 N7 H50A 1.0984 0.9919 0.3383 23 0.990 0.000 C50 C51 C49 H50B 1.0880 0.9410 0.2478 23 0.990 0.000 C50 C51 C49 H51A 1.0360 1.1046 0.2446 23 0.990 0.000 C51 C52 C50 H51B 1.1491 1.0755 0.2371 23 0.990 0.000 C51 C52 C50 H52A 1.0546 0.9978 0.1159 137 0.980 0.000 C52 C51 H52A H52B 1.0907 1.0866 0.1024 137 0.980 0.000 C52 C51 H52A H52C 0.9754 1.0693 0.1154 137 0.980 0.000 C52 C51 H52A 02SOT007 in Pn ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.55845 0.72037 0.81715 1.00000 0.02702 0.03357 0.02329 -0.00409 0.00113 -0.00278 0.02834 0.00688 0.00031 0.00022 0.00024 0.00000 0.00269 0.00228 0.00209 0.00185 0.00187 0.00199 0.00096 H1 0.58215 0.68571 0.77560 1.00000 0.03401 0.00000 0.00000 C2 0.62230 0.74004 0.89731 1.00000 0.02472 0.04169 0.03371 -0.00277 -0.00271 -0.00040 0.03429 0.00712 0.00033 0.00023 0.00026 0.00000 0.00271 0.00250 0.00235 0.00214 0.00202 0.00210 0.00103 H2 0.69033 0.72000 0.90917 1.00000 0.04115 0.00000 0.00000 C3 0.58850 0.78804 0.95965 1.00000 0.03215 0.03383 0.02687 -0.00799 -0.00698 -0.00395 0.03238 0.00709 0.00033 0.00022 0.00025 0.00000 0.00297 0.00236 0.00219 0.00195 0.00199 0.00207 0.00104 H3 0.63214 0.80038 1.01482 1.00000 0.03886 0.00000 0.00000 C4 0.49093 0.81784 0.94106 1.00000 0.03277 0.03371 0.02441 -0.00777 0.00415 -0.00404 0.03039 0.00703 0.00033 0.00023 0.00025 0.00000 0.00284 0.00237 0.00210 0.00183 0.00194 0.00205 0.00099 H4 0.46719 0.85142 0.98362 1.00000 0.03647 0.00000 0.00000 C5 0.42662 0.79984 0.86151 1.00000 0.01794 0.03201 0.02753 -0.00584 0.00586 -0.00279 0.02560 0.00666 0.00030 0.00021 0.00024 0.00000 0.00246 0.00229 0.00215 0.00188 0.00186 0.00182 0.00094 H5 0.35897 0.82065 0.85002 1.00000 0.03072 0.00000 0.00000 C6 0.46040 0.75128 0.79790 1.00000 0.01782 0.02829 0.02645 0.00498 0.00498 -0.00640 0.02405 0.00669 0.00030 0.00021 0.00023 0.00000 0.00251 0.00217 0.00212 0.00182 0.00185 0.00188 0.00091 C7 0.41619 0.70986 0.63653 1.00000 0.02290 0.01884 0.02392 0.00090 0.00015 0.00027 0.02235 0.00661 0.00032 0.00020 0.00023 0.00000 0.00269 0.00208 0.00204 0.00173 0.00186 0.00183 0.00090 C8 0.32455 0.69683 0.56731 1.00000 0.02031 0.02017 0.02021 0.00099 0.00119 -0.00238 0.02051 0.00653 0.00029 0.00020 0.00022 0.00000 0.00242 0.00199 0.00194 0.00165 0.00175 0.00173 0.00087 C9 0.16144 0.69162 0.51019 1.00000 0.02121 0.02010 0.01958 0.00014 0.00250 0.00180 0.02042 0.00655 0.00029 0.00020 0.00023 0.00000 0.00247 0.00202 0.00193 0.00163 0.00171 0.00172 0.00087 C10 0.21462 0.67585 0.44004 1.00000 0.02569 0.02023 0.01983 -0.00312 0.00168 0.00260 0.02218 0.00663 0.00030 0.00020 0.00023 0.00000 0.00255 0.00197 0.00192 0.00166 0.00173 0.00180 0.00088 C11 0.31864 0.67989 0.47608 1.00000 0.01872 0.02735 0.01816 0.00081 0.00838 0.00132 0.02079 0.00659 0.00029 0.00020 0.00022 0.00000 0.00242 0.00217 0.00185 0.00169 0.00168 0.00174 0.00087 C12 0.05070 0.69554 0.50901 1.00000 0.02098 0.01729 0.02237 0.00319 -0.00040 -0.00190 0.02071 0.00698 0.00030 0.00020 0.00024 0.00000 0.00254 0.00200 0.00207 0.00168 0.00187 0.00175 0.00087 C13 -0.07326 0.72626 0.61338 1.00000 0.01629 0.02507 0.03107 0.00529 0.00665 -0.00017 0.02384 0.00699 0.00029 0.00021 0.00024 0.00000 0.00246 0.00209 0.00219 0.00186 0.00186 0.00177 0.00090 C14 -0.07726 0.76350 0.69519 1.00000 0.02021 0.03968 0.03251 0.00055 0.00652 -0.00343 0.03057 0.00746 0.00031 0.00022 0.00025 0.00000 0.00262 0.00248 0.00229 0.00203 0.00190 0.00198 0.00098 H14 -0.01592 0.78053 0.73264 1.00000 0.03668 0.00000 0.00000 C15 -0.17140 0.77554 0.72158 1.00000 0.02982 0.04754 0.03165 -0.00344 0.00889 0.00239 0.03591 0.00804 0.00034 0.00024 0.00027 0.00000 0.00293 0.00264 0.00224 0.00209 0.00209 0.00217 0.00105 H15 -0.17427 0.80077 0.77742 1.00000 0.04309 0.00000 0.00000 C16 -0.26085 0.75125 0.66757 1.00000 0.02333 0.04387 0.04403 0.00703 0.01352 0.00616 0.03616 0.00824 0.00034 0.00024 0.00028 0.00000 0.00283 0.00273 0.00256 0.00225 0.00221 0.00212 0.00108 H16 -0.32534 0.76081 0.68509 1.00000 0.04340 0.00000 0.00000 C17 -0.25548 0.71297 0.58794 1.00000 0.01571 0.04230 0.04093 0.01166 0.00444 -0.00399 0.03303 0.00781 0.00032 0.00023 0.00026 0.00000 0.00253 0.00253 0.00256 0.00215 0.00202 0.00198 0.00104 H17 -0.31697 0.69519 0.55132 1.00000 0.03964 0.00000 0.00000 C18 -0.16170 0.69956 0.55951 1.00000 0.01999 0.02666 0.03083 0.00695 0.00171 0.00135 0.02614 0.00722 0.00030 0.00021 0.00026 0.00000 0.00263 0.00217 0.00213 0.00179 0.00193 0.00190 0.00094 H18 -0.15900 0.67277 0.50456 1.00000 0.03137 0.00000 0.00000 C53 0.86685 0.46580 0.72096 1.00000 0.02241 0.02837 0.01818 0.00456 -0.00078 0.00250 0.02350 0.00631 0.00029 0.00020 0.00022 0.00000 0.00245 0.00213 0.00193 0.00171 0.00171 0.00179 0.00090 H53A 0.81019 0.44695 0.75063 1.00000 0.02820 0.00000 0.00000 H53B 0.92921 0.43597 0.74722 1.00000 0.02820 0.00000 0.00000 C54 0.88502 0.55238 0.74332 1.00000 0.02539 0.03131 0.02096 0.00080 0.00022 -0.00277 0.02633 0.00646 0.00030 0.00021 0.00022 0.00000 0.00260 0.00227 0.00197 0.00179 0.00172 0.00187 0.00094 H54A 0.82975 0.58437 0.70778 1.00000 0.03160 0.00000 0.00000 H54B 0.95107 0.56912 0.72695 1.00000 0.03160 0.00000 0.00000 C55 0.88723 0.56672 0.84385 1.00000 0.02817 0.03373 0.02334 -0.00064 -0.00263 0.00182 0.02925 0.00674 0.00030 0.00023 0.00023 0.00000 0.00279 0.00233 0.00199 0.00188 0.00184 0.00191 0.00098 H55A 0.93538 0.52879 0.87882 1.00000 0.03510 0.00000 0.00000 H55B 0.91349 0.62066 0.85927 1.00000 0.03510 0.00000 0.00000 C56 0.78318 0.55806 0.87132 1.00000 0.03292 0.04489 0.02988 -0.00907 0.00879 0.00368 0.03550 0.00759 0.00033 0.00023 0.00027 0.00000 0.00276 0.00257 0.00206 0.00224 0.00188 0.00233 0.00101 H56A 0.73341 0.59162 0.83289 1.00000 0.05324 0.00000 0.00000 H56B 0.78762 0.57415 0.93435 1.00000 0.05324 0.00000 0.00000 H56C 0.76109 0.50279 0.86452 1.00000 0.05324 0.00000 0.00000 C57 0.74526 0.49008 0.57737 1.00000 0.01707 0.02469 0.01984 -0.00288 0.00001 -0.00114 0.02091 0.00652 0.00028 0.00021 0.00022 0.00000 0.00233 0.00208 0.00188 0.00169 0.00168 0.00173 0.00087 H57A 0.72660 0.47139 0.51441 1.00000 0.02509 0.00000 0.00000 H57B 0.76251 0.54689 0.57508 1.00000 0.02509 0.00000 0.00000 C58 0.65156 0.48223 0.62234 1.00000 0.02417 0.03494 0.02486 0.00403 0.00352 0.00593 0.02808 0.00715 0.00030 0.00023 0.00024 0.00000 0.00260 0.00233 0.00204 0.00182 0.00183 0.00188 0.00097 H58A 0.64177 0.42624 0.63789 1.00000 0.03369 0.00000 0.00000 H58B 0.66129 0.51362 0.67862 1.00000 0.03369 0.00000 0.00000 C59 0.55894 0.51144 0.55890 1.00000 0.02279 0.05167 0.02231 0.00174 0.00388 0.00347 0.03226 0.00749 0.00031 0.00025 0.00024 0.00000 0.00260 0.00262 0.00199 0.00202 0.00182 0.00207 0.00100 H59A 0.55215 0.48087 0.50216 1.00000 0.03871 0.00000 0.00000 H59B 0.57010 0.56744 0.54425 1.00000 0.03871 0.00000 0.00000 C60 0.45974 0.50520 0.59500 1.00000 0.02178 0.03388 0.03683 -0.00011 0.00386 0.00582 0.03097 0.00726 0.00030 0.00023 0.00026 0.00000 0.00262 0.00232 0.00230 0.00197 0.00195 0.00193 0.00100 H60A 0.44790 0.45000 0.60997 1.00000 0.04646 0.00000 0.00000 H60B 0.40295 0.52374 0.54921 1.00000 0.04646 0.00000 0.00000 H60C 0.46397 0.53783 0.64925 1.00000 0.04646 0.00000 0.00000 C61 0.81699 0.35833 0.61123 1.00000 0.02585 0.02193 0.02262 -0.00440 0.00530 -0.00211 0.02333 0.00656 0.00030 0.00020 0.00024 0.00000 0.00251 0.00206 0.00194 0.00169 0.00172 0.00181 0.00089 H61A 0.76492 0.34550 0.64893 1.00000 0.02800 0.00000 0.00000 H61B 0.78550 0.34815 0.54777 1.00000 0.02800 0.00000 0.00000 C62 0.90573 0.30233 0.63602 1.00000 0.03212 0.03044 0.03586 -0.00099 0.00845 0.00289 0.03250 0.00735 0.00032 0.00021 0.00027 0.00000 0.00286 0.00230 0.00233 0.00192 0.00204 0.00204 0.00103 H62A 0.94123 0.31386 0.69801 1.00000 0.03900 0.00000 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0.28577 1.00000 0.03715 0.00000 0.00000 H45B 0.95253 0.77529 0.31897 1.00000 0.03715 0.00000 0.00000 C46 0.91290 0.81056 0.18715 1.00000 0.04308 0.03671 0.02856 0.00161 0.00431 0.00124 0.03634 0.00755 0.00035 0.00023 0.00025 0.00000 0.00303 0.00250 0.00221 0.00198 0.00203 0.00215 0.00107 H46A 0.93180 0.85449 0.14982 1.00000 0.04361 0.00000 0.00000 H46B 0.83752 0.81154 0.18352 1.00000 0.04361 0.00000 0.00000 C47 0.94389 0.73283 0.14971 1.00000 0.03301 0.03191 0.02864 -0.00274 0.00499 -0.00567 0.03122 0.00700 0.00033 0.00022 0.00024 0.00000 0.00276 0.00234 0.00216 0.00187 0.00192 0.00194 0.00101 H47A 1.01826 0.73379 0.14781 1.00000 0.03747 0.00000 0.00000 H47B 0.93095 0.68925 0.19012 1.00000 0.03747 0.00000 0.00000 C48 0.88507 0.71766 0.05622 1.00000 0.05071 0.04365 0.02751 0.00310 -0.00288 -0.00334 0.04177 0.00761 0.00037 0.00025 0.00026 0.00000 0.00335 0.00273 0.00224 0.00205 0.00211 0.00223 0.00117 H48A 0.81158 0.71489 0.05830 1.00000 0.06265 0.00000 0.00000 H48B 0.90761 0.66753 0.03357 1.00000 0.06265 0.00000 0.00000 H48C 0.89784 0.76071 0.01609 1.00000 0.06265 0.00000 0.00000 C49 0.94795 0.97056 0.28072 1.00000 0.05836 0.02304 0.04405 0.00510 0.01962 0.00094 0.04054 0.00840 0.00037 0.00022 0.00029 0.00000 0.00354 0.00229 0.00256 0.00197 0.00236 0.00217 0.00116 H49A 0.90916 0.96791 0.21843 1.00000 0.04864 0.00000 0.00000 H49B 0.92073 1.01583 0.31090 1.00000 0.04864 0.00000 0.00000 C50 1.05964 0.98677 0.27619 1.00000 0.08244 0.06686 0.07401 0.02771 0.03319 -0.01562 0.07210 0.01081 0.00045 0.00031 0.00037 0.00000 0.00500 0.00375 0.00367 0.00309 0.00342 0.00325 0.00173 H50A 1.09839 0.99194 0.33827 1.00000 0.08652 0.00000 0.00000 H50B 1.08802 0.94099 0.24778 1.00000 0.08652 0.00000 0.00000 C51 1.07564 1.06083 0.22370 1.00000 0.11018 0.04925 0.09554 -0.00920 0.05553 -0.01131 0.08051 0.01183 0.00053 0.00030 0.00041 0.00000 0.00571 0.00332 0.00474 0.00333 0.00425 0.00336 0.00194 H51A 1.03598 1.10456 0.24465 1.00000 0.09661 0.00000 0.00000 H51B 1.14908 1.07553 0.23710 1.00000 0.09661 0.00000 0.00000 C52 1.04709 1.05307 0.13300 1.00000 0.20745 0.16148 0.08011 0.05226 -0.04207 -0.06420 0.15762 0.01391 0.00075 0.00049 0.00047 0.00000 0.01010 0.00798 0.00526 0.00570 0.00574 0.00719 0.00402 H52A 1.05462 0.99779 0.11590 1.00000 0.23643 0.00000 0.00000 H52B 1.09074 1.08657 0.10237 1.00000 0.23643 0.00000 0.00000 H52C 0.97535 1.06925 0.11539 1.00000 0.23643 0.00000 0.00000 N7 0.92724 0.89456 0.33019 1.00000 0.04292 0.02517 0.02844 0.00468 0.00618 0.00525 0.03217 0.00593 0.00027 0.00017 0.00020 0.00000 0.00259 0.00189 0.00184 0.00154 0.00167 0.00167 0.00086 Final Structure Factor Calculation for 02SOT007 in Pn Total number of l.s. parameters = 766 Maximum vector length = 511 Memory required = 9095 / 26068 wR2 = 0.0984 before cycle 2 for 10094 data and 2 / 766 parameters GooF = S = 0.988; Restrained GooF = 0.987 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0345 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0476 for 7453 Fo > 4sig(Fo) and 0.0819 for all 10094 data wR2 = 0.0984, GooF = S = 0.988, Restrained GooF = 0.987 for all data Flack x parameter = -0.0474 with esd 0.0428 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Occupancy sum of asymmetric unit = 84.00 for non-hydrogen and 96.00 for hydrogen atoms Principal mean square atomic displacements U 0.0352 0.0295 0.0203 C1 0.0433 0.0383 0.0213 C2 0.0450 0.0368 0.0154 C3 0.0390 0.0323 0.0199 C4 0.0363 0.0235 0.0170 C5 0.0344 0.0246 0.0131 C6 0.0282 0.0204 0.0185 C7 0.0246 0.0192 0.0177 C8 0.0229 0.0198 0.0185 C9 0.0288 0.0210 0.0168 C10 0.0278 0.0225 0.0121 C11 0.0282 0.0182 0.0157 C12 0.0342 0.0224 0.0150 C13 0.0403 0.0326 0.0188 C14 0.0485 0.0338 0.0254 C15 0.0529 0.0369 0.0187 C16 0.0543 0.0302 0.0145 C17 0.0365 0.0233 0.0186 C18 0.0301 0.0259 0.0145 C53 0.0332 0.0265 0.0193 C54 0.0363 0.0322 0.0193 C55 0.0498 0.0345 0.0222 C56 0.0261 0.0217 0.0149 C57 0.0381 0.0255 0.0207 C58 0.0521 0.0225 0.0221 C59 0.0379 0.0356 0.0194 C60 0.0281 0.0240 0.0179 C61 0.0368 0.0336 0.0271 C62 0.0395 0.0313 0.0248 C63 0.0595 0.0321 0.0313 C64 0.0302 0.0259 0.0158 C65 0.0408 0.0273 0.0221 C66 0.0343 0.0325 0.0204 C67 0.0432 0.0357 0.0247 C68 0.0384 0.0193 0.0118 N1 0.0238 0.0198 0.0157 N2 0.0334 0.0207 0.0096 N3 0.0236 0.0213 0.0181 N8 0.0458 0.0300 0.0149 O1 0.0373 0.0273 0.0175 O2 0.0460 0.0283 0.0172 Cl1 0.0423 0.0278 0.0190 Cl2 0.0324 0.0276 0.0185 C19 0.0529 0.0340 0.0211 C20 0.0463 0.0298 0.0250 C21 0.0326 0.0311 0.0241 C22 0.0346 0.0278 0.0190 C23 0.0342 0.0288 0.0073 C24 0.0414 0.0200 0.0129 C25 0.0325 0.0218 0.0155 C26 0.0319 0.0193 0.0169 C27 0.0402 0.0233 0.0168 C28 0.0417 0.0195 0.0147 C29 0.0318 0.0277 0.0165 C30 0.0290 0.0240 0.0154 C31 0.0516 0.0243 0.0233 C32 0.0687 0.0345 0.0259 C33 0.0572 0.0417 0.0229 C34 0.0512 0.0348 0.0259 C35 0.0444 0.0317 0.0205 C36 0.0307 0.0255 0.0180 N4 0.0259 0.0221 0.0170 N5 0.0439 0.0216 0.0167 N6 0.0477 0.0333 0.0194 O3 0.0624 0.0307 0.0208 O4 0.0613 0.0457 0.0181 Cl3 0.0663 0.0431 0.0209 Cl4 0.0577 0.0375 0.0296 C37 0.1006 0.0389 0.0334 C38 0.1595 0.0514 0.0312 C39 0.1040 0.0535 0.0297 C40 0.0555 0.0353 0.0235 C41 0.0464 0.0399 0.0284 C42 0.0574 0.0474 0.0298 C43 0.0524 0.0480 0.0412 C44 0.0398 0.0309 0.0221 C45 0.0439 0.0369 0.0282 C46 0.0382 0.0298 0.0257 C47 0.0577 0.0424 0.0252 C48 0.0628 0.0372 0.0216 C49 0.0988 0.0921 0.0254 C50 0.1378 0.0565 0.0472 C51 0.3043 0.1168 0.0517 C52 may be split into 1.0576 1.0463 0.1264 and 1.0366 1.0598 0.1396 0.0444 0.0307 0.0214 N7 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.025 0.038 0.049 0.059 0.072 0.086 0.103 0.128 0.174 1.000 Number in group 1018. 1043. 1046. 958. 1040. 1001. 969. 1012. 995. 1012. GooF 0.853 0.952 0.975 0.944 1.018 0.988 1.006 0.986 1.069 1.062 K 1.126 1.007 1.001 1.002 1.006 1.015 1.003 0.998 1.005 1.011 Resolution(A) 0.84 0.88 0.92 0.97 1.02 1.10 1.19 1.31 1.50 1.88 inf Number in group 1049. 981. 1015. 997. 1018. 996. 1018. 1004. 1010. 1006. GooF 0.898 0.902 0.963 0.989 0.905 1.002 0.954 0.955 1.046 1.219 K 1.056 1.066 1.031 1.004 0.989 0.993 0.999 1.007 1.026 1.003 R1 0.249 0.203 0.154 0.130 0.087 0.062 0.052 0.041 0.032 0.026 Recommended weighting scheme: WGHT 0.0347 0.0000 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 1 -2 506.21 881.56 6.37 0.129 6.46 -1 17 -3 0.00 123.37 4.57 0.048 0.97 -1 1 -2 1551.32 1893.50 4.16 0.189 5.67 -1 1 -5 319.14 391.54 4.02 0.086 2.75 1 1 5 320.38 390.43 3.80 0.086 2.75 1 4 -1 863.44 1041.63 3.73 0.140 3.94 -7 10 -9 28.01 225.50 3.70 0.065 0.95 6 2 -2 996.61 804.34 3.67 0.123 2.12 3 10 -3 117.47 53.60 3.54 0.032 1.53 6 14 -6 56.29 242.76 3.47 0.068 1.00 4 6 11 365.60 559.27 3.47 0.103 1.09 -1 4 1 949.54 1100.48 3.45 0.144 3.94 4 7 4 1361.62 1168.68 3.43 0.149 1.65 0 12 5 40.32 91.88 3.42 0.042 1.27 -3 0 -7 5313.71 4443.79 3.40 0.290 1.79 1 13 9 284.19 99.94 3.40 0.043 1.01 -1 0 -5 3688.69 4478.15 3.37 0.291 2.79 4 3 12 255.42 353.33 3.37 0.082 1.08 12 7 -8 169.46 442.81 3.36 0.091 0.94 9 11 -6 403.25 601.77 3.34 0.107 1.02 2 15 -9 28.56 208.08 3.31 0.063 0.93 -2 3 13 112.72 177.61 3.30 0.058 1.14 -7 9 1 134.66 216.04 3.29 0.064 1.33 -2 1 2 2536.67 2926.57 3.27 0.235 5.13 0 4 7 1081.20 1300.45 3.22 0.157 1.90 1 1 -17 305.52 158.87 3.21 0.055 0.88 7 0 -3 4404.29 3611.00 3.20 0.261 1.85 -1 13 6 483.83 608.18 3.19 0.107 1.16 2 1 -12 123.18 73.71 3.16 0.037 1.25 1 8 0 8766.48 7667.39 3.16 0.381 2.09 1 7 3 407.34 473.18 3.14 0.095 2.12 11 11 -2 56.57 225.68 3.13 0.065 0.95 -1 2 12 104.87 155.20 3.13 0.054 1.24 -1 2 2 1515.03 1735.10 3.12 0.181 5.39 -10 1 -4 446.40 697.96 3.07 0.115 1.17 -7 0 5 306.80 396.19 3.06 0.087 1.72 -1 14 -7 312.46 65.40 3.05 0.035 1.04 -1 6 6 324.03 413.49 3.04 0.088 1.88 -8 13 -8 698.24 292.73 3.04 0.074 0.85 0 1 2 3137.41 3681.46 3.03 0.264 6.80 3 5 -15 0.00 161.41 3.01 0.055 0.96 -10 12 8 28.00 188.06 3.00 0.060 0.90 3 1 6 1727.48 1479.52 3.00 0.167 1.99 7 7 -3 65.59 112.63 2.98 0.046 1.47 -12 7 1 84.36 197.70 2.98 0.061 1.00 -3 11 -5 198.01 281.40 2.97 0.073 1.27 3 5 -7 1754.72 1529.91 2.95 0.170 1.75 4 17 7 -28.28 208.22 2.94 0.063 0.85 3 14 0 65.65 136.68 2.93 0.051 1.16 -3 14 0 63.42 128.26 2.92 0.049 1.16 Bond lengths and angles C1 - Distance Angles C6 1.3829 (0.0051) C2 1.3898 (0.0052) 119.98 (0.36) C1 - C6 C2 - Distance Angles C3 1.3739 (0.0053) C1 1.3898 (0.0052) 120.98 (0.39) C2 - C3 C3 - Distance Angles C4 1.3697 (0.0054) C2 1.3739 (0.0053) 119.00 (0.35) C3 - C4 C4 - Distance Angles C3 1.3697 (0.0054) C5 1.3791 (0.0051) 121.02 (0.36) C4 - C3 C5 - Distance Angles C4 1.3791 (0.0051) C6 1.3936 (0.0049) 120.31 (0.37) C5 - C4 C6 - Distance Angles C1 1.3829 (0.0051) C5 1.3936 (0.0049) 118.68 (0.33) N1 1.4087 (0.0045) 122.76 (0.33) 118.54 (0.35) C6 - C1 C5 C7 - Distance Angles O1 1.2258 (0.0043) N1 1.3780 (0.0044) 123.58 (0.33) C8 1.4735 (0.0050) 123.79 (0.33) 112.63 (0.34) C7 - O1 N1 C8 - Distance Angles N2 1.3611 (0.0044) C11 1.3931 (0.0046) 110.25 (0.31) C7 1.4735 (0.0050) 120.76 (0.31) 128.92 (0.35) C8 - N2 C11 C9 - Distance Angles N2 1.3584 (0.0044) C10 1.3932 (0.0049) 109.88 (0.32) C12 1.4646 (0.0050) 120.67 (0.31) 129.45 (0.33) C9 - N2 C10 C10 - Distance Angles C11 1.3920 (0.0052) C9 1.3932 (0.0049) 106.86 (0.31) Cl2 1.7313 (0.0035) 125.12 (0.29) 127.98 (0.30) C10 - C11 C9 C11 - Distance Angles C10 1.3920 (0.0052) C8 1.3931 (0.0046) 106.16 (0.32) Cl1 1.7294 (0.0035) 125.09 (0.27) 128.73 (0.30) C11 - C10 C8 C12 - Distance Angles O2 1.2213 (0.0040) N3 1.3739 (0.0043) 123.49 (0.35) C9 1.4646 (0.0050) 123.58 (0.33) 112.93 (0.31) C12 - O2 N3 C13 - Distance Angles C18 1.3805 (0.0051) C14 1.3936 (0.0050) 120.68 (0.37) N3 1.4279 (0.0045) 123.35 (0.34) 115.97 (0.34) C13 - C18 C14 C14 - Distance Angles C15 1.3871 (0.0053) C13 1.3936 (0.0050) 119.56 (0.38) C14 - C15 C15 - Distance Angles C16 1.3787 (0.0056) C14 1.3871 (0.0053) 120.64 (0.38) C15 - C16 C16 - Distance Angles C17 1.3763 (0.0053) C15 1.3787 (0.0056) 119.11 (0.40) C16 - C17 C17 - Distance Angles C16 1.3763 (0.0053) C18 1.4000 (0.0051) 121.68 (0.39) C17 - C16 C18 - Distance Angles C13 1.3805 (0.0051) C17 1.4000 (0.0051) 118.29 (0.37) C18 - C13 C53 - Distance Angles C54 1.5132 (0.0047) N8 1.5208 (0.0042) 115.62 (0.27) C53 - C54 C54 - Distance Angles C53 1.5132 (0.0047) C55 1.5293 (0.0046) 110.45 (0.29) C54 - C53 C55 - Distance Angles C56 1.5123 (0.0053) C54 1.5293 (0.0047) 113.15 (0.31) C55 - C56 C56 - Distance Angles C55 1.5123 (0.0053) C56 - C57 - Distance Angles N8 1.5156 (0.0044) C58 1.5185 (0.0049) 116.54 (0.28) C57 - N8 C58 - Distance Angles C59 1.5022 (0.0051) C57 1.5185 (0.0049) 109.10 (0.29) C58 - C59 C59 - Distance Angles C58 1.5022 (0.0051) C60 1.5093 (0.0055) 114.40 (0.31) C59 - C58 C60 - Distance Angles C59 1.5093 (0.0055) C60 - C61 - Distance Angles C62 1.5054 (0.0051) N8 1.5207 (0.0043) 116.86 (0.30) C61 - C62 C62 - Distance Angles C61 1.5054 (0.0050) C63 1.5127 (0.0051) 110.97 (0.34) C62 - C61 C63 - Distance Angles C62 1.5127 (0.0051) C64 1.5340 (0.0053) 114.33 (0.32) C63 - C62 C64 - Distance Angles C63 1.5340 (0.0053) C64 - C65 - Distance Angles N8 1.5037 (0.0043) C66 1.5176 (0.0046) 115.90 (0.29) C65 - N8 C66 - Distance Angles C67 1.5149 (0.0054) C65 1.5176 (0.0046) 111.15 (0.32) C66 - C67 C67 - Distance Angles C66 1.5149 (0.0054) C68 1.5280 (0.0049) 110.26 (0.34) C67 - C66 C68 - Distance Angles C67 1.5280 (0.0049) C68 - N1 - Distance Angles C7 1.3780 (0.0044) C6 1.4087 (0.0045) 127.65 (0.33) N1 - C7 N2 - Distance Angles C9 1.3584 (0.0044) C8 1.3611 (0.0044) 106.84 (0.27) N2 - C9 N3 - Distance Angles C12 1.3739 (0.0043) C13 1.4279 (0.0045) 127.74 (0.31) N3 - C12 N8 - Distance Angles C65 1.5037 (0.0044) C57 1.5156 (0.0044) 108.43 (0.26) C61 1.5207 (0.0043) 112.39 (0.26) 107.11 (0.26) C53 1.5208 (0.0042) 109.61 (0.26) 110.69 (0.25) 108.59 (0.25) N8 - C65 C57 C61 O1 - Distance Angles C7 1.2258 (0.0043) O1 - O2 - Distance Angles C12 1.2213 (0.0040) O2 - Cl1 - Distance Angles C11 1.7294 (0.0035) Cl1 - Cl2 - Distance Angles C10 1.7313 (0.0035) Cl2 - C19 - Distance Angles C20 1.3728 (0.0050) C24 1.3946 (0.0048) 120.70 (0.35) C19 - C20 C20 - Distance Angles C19 1.3728 (0.0050) C21 1.3950 (0.0053) 120.27 (0.37) C20 - C19 C21 - Distance Angles C22 1.3785 (0.0053) C20 1.3950 (0.0053) 119.21 (0.37) C21 - C22 C22 - Distance Angles C23 1.3697 (0.0051) C21 1.3785 (0.0052) 120.66 (0.37) C22 - C23 C23 - Distance Angles C22 1.3697 (0.0051) C24 1.3959 (0.0052) 120.83 (0.36) C23 - C22 C24 - Distance Angles C19 1.3946 (0.0048) C23 1.3959 (0.0052) 118.31 (0.34) N4 1.4050 (0.0044) 124.48 (0.33) 117.18 (0.33) C24 - C19 C23 C25 - Distance Angles O3 1.2220 (0.0041) N4 1.3756 (0.0045) 123.35 (0.34) C26 1.4661 (0.0051) 122.65 (0.34) 114.01 (0.32) C25 - O3 N4 C26 - Distance Angles N5 1.3630 (0.0044) C29 1.3963 (0.0049) 109.65 (0.30) C25 1.4661 (0.0051) 121.65 (0.32) 128.61 (0.33) C26 - N5 C29 C27 - Distance Angles N5 1.3657 (0.0044) C28 1.3917 (0.0048) 109.56 (0.32) C30 1.4673 (0.0050) 121.45 (0.31) 128.98 (0.35) C27 - N5 C28 C28 - Distance Angles C29 1.3712 (0.0050) C27 1.3917 (0.0048) 107.24 (0.32) Cl4 1.7327 (0.0037) 124.25 (0.28) 128.50 (0.31) C28 - C29 C27 C29 - Distance Angles C28 1.3712 (0.0050) C26 1.3963 (0.0049) 106.86 (0.29) Cl3 1.7226 (0.0034) 124.66 (0.29) 128.44 (0.29) C29 - C28 C26 C30 - Distance Angles O4 1.2342 (0.0043) N6 1.3746 (0.0044) 122.62 (0.34) C27 1.4673 (0.0050) 121.72 (0.34) 115.66 (0.33) C30 - O4 N6 C31 - Distance Angles C32 1.3849 (0.0049) C36 1.3851 (0.0050) 118.32 (0.34) N6 1.4013 (0.0044) 117.13 (0.31) 124.52 (0.33) C31 - C32 C36 C32 - Distance Angles C33 1.3812 (0.0052) C31 1.3849 (0.0049) 121.29 (0.36) C32 - C33 C33 - Distance Angles C34 1.3674 (0.0055) C32 1.3812 (0.0052) 119.83 (0.39) C33 - C34 C34 - Distance Angles C33 1.3674 (0.0055) C35 1.3708 (0.0055) 119.69 (0.38) C34 - C33 C35 - Distance Angles C34 1.3708 (0.0056) C36 1.3847 (0.0052) 120.93 (0.38) C35 - C34 C36 - Distance Angles C35 1.3847 (0.0052) C31 1.3851 (0.0050) 119.94 (0.36) C36 - C35 N4 - Distance Angles C25 1.3756 (0.0045) C24 1.4050 (0.0044) 127.51 (0.31) N4 - C25 N5 - Distance Angles C26 1.3630 (0.0044) C27 1.3657 (0.0044) 106.67 (0.28) N5 - C26 N6 - Distance Angles C30 1.3746 (0.0044) C31 1.4013 (0.0044) 127.82 (0.31) N6 - C30 O3 - Distance Angles C25 1.2220 (0.0041) O3 - O4 - Distance Angles C30 1.2342 (0.0043) O4 - Cl3 - Distance Angles C29 1.7226 (0.0034) Cl3 - Cl4 - Distance Angles C28 1.7327 (0.0037) Cl4 - C37 - Distance Angles C38 1.5113 (0.0054) N7 1.5118 (0.0048) 117.11 (0.35) C37 - C38 C38 - Distance Angles C39 1.4067 (0.0062) C37 1.5113 (0.0054) 116.34 (0.39) C38 - C39 C39 - Distance Angles C38 1.4067 (0.0063) C40 1.5020 (0.0059) 118.07 (0.44) C39 - C38 C40 - Distance Angles C39 1.5020 (0.0059) C40 - C41 - Distance Angles N7 1.5080 (0.0053) C42 1.5113 (0.0052) 114.93 (0.33) C41 - N7 C42 - Distance Angles C41 1.5113 (0.0052) C43 1.5302 (0.0060) 111.55 (0.34) C42 - C41 C43 - Distance Angles C44 1.5072 (0.0060) C42 1.5302 (0.0060) 112.96 (0.36) C43 - C44 C44 - Distance Angles C43 1.5072 (0.0060) C44 - C45 - Distance Angles C46 1.5131 (0.0053) N7 1.5179 (0.0044) 115.36 (0.31) C45 - C46 C46 - Distance Angles C45 1.5131 (0.0053) C47 1.5156 (0.0052) 112.04 (0.33) C46 - C45 C47 - Distance Angles C48 1.5092 (0.0053) C46 1.5156 (0.0052) 111.46 (0.35) C47 - C48 C48 - Distance Angles C47 1.5092 (0.0053) C48 - C49 - Distance Angles C50 1.5168 (0.0066) N7 1.5347 (0.0047) 115.51 (0.36) C49 - C50 C50 - Distance Angles C51 1.5164 (0.0066) C49 1.5168 (0.0066) 113.45 (0.48) C50 - C51 C51 - Distance Angles C52 1.3599 (0.0076) C50 1.5164 (0.0066) 113.87 (0.55) C51 - C52 C52 - Distance Angles C51 1.3599 (0.0076) C52 - N7 - Distance Angles C41 1.5080 (0.0053) C37 1.5118 (0.0048) 111.09 (0.31) C45 1.5179 (0.0045) 110.56 (0.30) 107.39 (0.29) C49 1.5347 (0.0047) 107.62 (0.30) 109.85 (0.31) 110.34 (0.29) N7 - C41 C37 C45 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 2.22 3.072(4) 161.5 N1-H1A...N5 0.88 2.28 3.124(4) 161.9 N3-H3A...N5 0.88 2.27 3.130(4) 167.4 N4-H4A...N2 0.88 2.35 3.218(4) 168.9 N6-H6...N2 Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 12.1496 (0.0099) x + 1.4299 (0.0336) y + 3.3715 (0.0284) z = 5.8563 (0.0324) * -0.0037 (0.0023) N5 * 0.0006 (0.0023) C26 * 0.0053 (0.0023) C27 * -0.0049 (0.0023) C28 * 0.0026 (0.0023) C29 -2.4636 (0.0044) H14 2.5443 (0.0043) H5 Rms deviation of fitted atoms = 0.0038 0.5647 (0.0233) x + 16.5310 (0.0058) y - 3.2222 (0.0236) z = 9.8797 (0.0168) Angle to previous plane (with approximate esd) = 87.69 ( 0.15 ) * 0.0027 (0.0020) N2 * -0.0052 (0.0021) C8 * 0.0008 (0.0021) C9 * -0.0038 (0.0022) C10 * 0.0055 (0.0022) C11 2.4627 (0.0042) H32 -2.6401 (0.0044) H23 Rms deviation of fitted atoms = 0.0040 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)