+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 13:12:32 on 20-May-2002 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P-1 CELL 0.71069 13.4080 15.8470 17.0230 73.042 74.733 68.046 ZERR 2.00 0.0050 0.0050 0.0050 0.005 0.005 0.005 LATT 1 SFAC C H N O F UNIT 124 180 18 20 2 V = 3159.95 F(000) = 1228.0 Mu = 0.08 mm-1 Cell Wt = 2280.86 Rho = 1.199 MERG 2 SHEL 7 0.84 FMAP 2 PLAN 25 SIZE 0.01 0.04 0.06 ACTA ISOR 0.005 $C ISOR 0.0008 F1 HTAB HTAB N3 F1 HTAB N5 F1 L.S. 4 TEMP -153.00 WGHT 0.144700 EXTI 0.010076 FVAR 0.05969 MOLE 1 F1 5 0.414833 0.648303 0.188504 11.00000 0.00118 0.00151 = 0.00044 -0.00020 -0.00043 -0.00080 O1 4 0.053402 0.335397 0.216309 11.00000 0.09851 0.07840 = 0.15554 -0.01147 -0.05489 -0.03411 O2 4 -0.067519 0.458180 0.156779 11.00000 0.07460 0.12553 = 0.08185 -0.01473 -0.03607 -0.03899 O3 4 -0.012131 0.755026 0.081851 11.00000 0.09383 0.09913 = 0.11893 0.00495 -0.05605 -0.02239 O4 4 0.131901 0.768695 0.106805 11.00000 0.10889 0.06850 = 0.11756 -0.03019 -0.01765 -0.01847 O5 4 0.358867 0.297768 0.279609 11.00000 0.06444 0.05500 = 0.08794 -0.01220 -0.01502 -0.02054 O6 4 0.770985 0.418653 0.344032 11.00000 0.05463 0.06321 = 0.07374 -0.00175 -0.03674 -0.02471 O7 4 0.535713 0.864337 0.116631 11.00000 0.10859 0.07181 = 0.08829 0.00726 -0.06402 -0.03428 O8 4 0.636355 0.928052 0.146656 11.00000 0.09835 0.07338 = 0.17285 -0.02576 -0.05056 -0.03320 O9 4 0.937618 0.735009 0.285184 11.00000 0.12189 0.08864 = 0.09209 -0.02785 -0.03096 -0.05430 O10 4 0.948673 0.592340 0.351459 11.00000 0.07777 0.08058 = 0.08958 0.01105 -0.05313 -0.01891 N1 3 0.015227 0.419689 0.188734 11.00000 0.07915 0.06252 = 0.08674 -0.00437 -0.02811 -0.03105 N2 3 0.076758 0.723135 0.107943 11.00000 0.11468 0.08229 = 0.08891 -0.01040 -0.04727 -0.00097 N3 3 0.339607 0.453796 0.238974 11.00000 0.03093 0.03863 = 0.10623 -0.01261 -0.01468 -0.01484 AFIX 43 H3 2 0.373345 0.493128 0.235805 11.00000 -1.20000 AFIX 0 N4 3 0.529866 0.418832 0.292668 11.00000 0.04743 0.05589 = 0.06294 -0.01821 -0.00849 -0.01692 N5 3 0.644849 0.535314 0.272436 11.00000 0.05276 0.04104 = 0.06330 -0.01827 -0.01510 -0.01528 AFIX 43 H5 2 0.584161 0.548178 0.254057 11.00000 -1.20000 AFIX 0 N6 3 0.605962 0.859971 0.150013 11.00000 0.08878 0.05849 = 0.05813 -0.00925 -0.02117 -0.01006 N7 3 0.906695 0.665336 0.306953 11.00000 0.06224 0.08122 = 0.06606 -0.03471 -0.00621 -0.02623 AFIX 66 C1 1 0.180805 0.435371 0.215945 11.00000 0.06534 0.06711 = 0.06786 -0.01331 -0.01392 -0.02086 AFIX 43 H1 2 0.205508 0.370632 0.240048 11.00000 -1.20000 AFIX 65 C2 1 0.083131 0.474437 0.185454 11.00000 0.05728 0.05916 = 0.05986 -0.01112 -0.01453 -0.01938 C3 1 0.046986 0.569160 0.150189 11.00000 0.05880 0.06223 = 0.06265 -0.01875 -0.01569 -0.01551 AFIX 43 H3A 2 -0.019770 0.595859 0.129349 11.00000 -1.20000 AFIX 65 C4 1 0.108514 0.624818 0.145415 11.00000 0.05901 0.06046 = 0.06677 -0.01318 -0.01050 -0.02111 C5 1 0.206189 0.585753 0.175906 11.00000 0.04918 0.04910 = 0.05015 -0.01033 -0.00677 -0.01419 AFIX 43 H5A 2 0.248241 0.623793 0.172643 11.00000 -1.20000 AFIX 65 C6 1 0.242335 0.491031 0.211171 11.00000 0.05935 0.06135 = 0.05886 -0.01545 -0.01389 -0.01756 AFIX 0 C7 1 0.390230 0.362541 0.271070 11.00000 0.05974 0.06054 = 0.06094 -0.01265 -0.00767 -0.01905 C8 1 0.498472 0.343306 0.298594 11.00000 0.05899 0.06212 = 0.06168 -0.01469 -0.01239 -0.01701 C9 1 0.580989 0.259571 0.320741 11.00000 0.04806 0.04720 = 0.05050 -0.00757 -0.00943 -0.01636 C10 1 0.665525 0.283626 0.335061 11.00000 0.04814 0.05391 = 0.04924 -0.00873 -0.01405 -0.01326 C11 1 0.630901 0.381602 0.311639 11.00000 0.05505 0.05502 = 0.05156 -0.01374 -0.01113 -0.01804 C12 1 0.691711 0.443250 0.312525 11.00000 0.05260 0.05558 = 0.05414 -0.01242 -0.01256 -0.01912 AFIX 66 C13 1 0.685087 0.609226 0.258627 11.00000 0.05428 0.05251 = 0.05044 -0.01077 -0.00595 -0.01821 C14 1 0.630005 0.694961 0.212938 11.00000 0.06647 0.06391 = 0.06337 -0.01476 -0.01484 -0.01927 AFIX 43 H14 2 0.568085 0.701602 0.191651 11.00000 -1.20000 AFIX 65 C15 1 0.665521 0.770977 0.198394 11.00000 0.05915 0.05828 = 0.05540 -0.01161 -0.00840 -0.01827 C16 1 0.756120 0.761260 0.229540 11.00000 0.06684 0.05961 = 0.06229 -0.01637 -0.01018 -0.02025 AFIX 43 H16 2 0.780393 0.813214 0.219599 11.00000 -1.20000 AFIX 65 C17 1 0.811202 0.675525 0.275229 11.00000 0.05280 0.05653 = 0.05287 -0.01009 -0.01292 -0.01843 C18 1 0.775687 0.599508 0.289774 11.00000 0.06018 0.06260 = 0.05852 -0.01320 -0.01106 -0.01708 AFIX 43 H18 2 0.813334 0.540912 0.321000 11.00000 -1.20000 AFIX 66 C19 1 0.586533 0.160966 0.327455 11.00000 0.05585 0.05657 = 0.05408 -0.01233 -0.01407 -0.01651 C20 1 0.505217 0.126056 0.379231 11.00000 0.05785 0.05737 = 0.05116 -0.01348 -0.01340 -0.01477 AFIX 43 H20 2 0.443587 0.165311 0.408805 11.00000 -1.20000 AFIX 65 C21 1 0.514074 0.033712 0.387735 11.00000 0.06967 0.06572 = 0.06126 -0.01336 -0.01679 -0.02245 AFIX 43 H21 2 0.458498 0.009853 0.423122 11.00000 -1.20000 AFIX 65 C22 1 0.604248 -0.023725 0.344464 11.00000 0.07230 0.07246 = 0.06987 -0.01355 -0.01993 -0.02340 AFIX 43 H22 2 0.610301 -0.086838 0.350276 11.00000 -1.20000 AFIX 65 C23 1 0.685564 0.011183 0.292687 11.00000 0.07704 0.07851 = 0.07849 -0.01664 -0.01329 -0.02483 AFIX 43 H23 2 0.747194 -0.028072 0.263113 11.00000 -1.20000 AFIX 65 C24 1 0.676708 0.103528 0.284182 11.00000 0.05793 0.05318 = 0.05272 -0.01200 -0.00965 -0.01392 AFIX 43 H24 2 0.732285 0.127386 0.248795 11.00000 -1.20000 AFIX 66 C25 1 0.769511 0.215717 0.356043 11.00000 0.04448 0.04450 = 0.04422 -0.01149 -0.01189 -0.01358 C26 1 0.770181 0.137415 0.419927 11.00000 0.05813 0.06068 = 0.05695 -0.01583 -0.01362 -0.01922 AFIX 43 H26 2 0.703238 0.129281 0.451426 11.00000 -1.20000 AFIX 65 C27 1 0.868799 0.071013 0.437724 11.00000 0.07110 0.07110 = 0.06770 -0.01553 -0.01719 -0.01982 AFIX 43 H27 2 0.869257 0.017497 0.481386 11.00000 -1.20000 AFIX 65 C28 1 0.966748 0.082913 0.391636 11.00000 0.07785 0.07426 = 0.07518 -0.02199 -0.01610 -0.01841 AFIX 43 H28 2 1.034149 0.037530 0.403800 11.00000 -1.20000 AFIX 65 C29 1 0.966080 0.161214 0.327752 11.00000 0.07749 0.07402 = 0.07395 -0.01907 -0.01511 -0.02310 AFIX 43 H29 2 1.033024 0.169347 0.296253 11.00000 -1.20000 AFIX 65 C30 1 0.867462 0.227617 0.309954 11.00000 0.06324 0.05982 = 0.06337 -0.01421 -0.01467 -0.01674 AFIX 43 H30 2 0.867005 0.281132 0.266292 11.00000 -1.20000 AFIX 0 MOLE 2 N8 3 0.520836 0.218099 0.065824 11.00000 0.06585 0.07130 = 0.06506 -0.01950 -0.02171 -0.01383 C31 1 0.471862 0.160537 0.141130 11.00000 0.05710 0.05746 = 0.05903 -0.01243 -0.01413 -0.01750 AFIX 23 H31A 2 0.420332 0.203354 0.177025 11.00000 -1.20000 H31B 2 0.531407 0.118719 0.172279 11.00000 -1.20000 AFIX 0 C32 1 0.412085 0.101043 0.131606 11.00000 0.05782 0.05454 = 0.05600 -0.01197 -0.01156 -0.01949 AFIX 23 H32A 2 0.347065 0.141917 0.106165 11.00000 -1.20000 H32B 2 0.460397 0.059907 0.093275 11.00000 -1.20000 AFIX 0 C33 1 0.376577 0.042358 0.213103 11.00000 0.07001 0.06858 = 0.07177 -0.01644 -0.01419 -0.02278 AFIX 23 H33A 2 0.440808 0.005250 0.240626 11.00000 -1.20000 H33B 2 0.348033 -0.001679 0.202231 11.00000 -1.20000 AFIX 0 C34 1 0.287281 0.100866 0.273101 11.00000 0.09034 0.08695 = 0.09073 -0.01993 -0.01587 -0.03169 AFIX 137 H34A 2 0.219426 0.129994 0.250211 11.00000 -1.50000 H34B 2 0.311707 0.149346 0.279167 11.00000 -1.50000 H34C 2 0.274393 0.060156 0.327763 11.00000 -1.50000 AFIX 0 C35 1 0.609930 0.157001 0.009733 11.00000 0.06969 0.07222 = 0.07121 -0.01771 -0.01456 -0.02106 AFIX 23 H35A 2 0.628774 0.196838 -0.044890 11.00000 -1.20000 H35B 2 0.581495 0.112288 -0.000093 11.00000 -1.20000 AFIX 0 C36 1 0.714229 0.102518 0.048955 11.00000 0.06506 0.06761 = 0.06851 -0.01373 -0.01334 -0.02161 AFIX 23 H36A 2 0.744377 0.147020 0.057127 11.00000 -1.20000 H36B 2 0.695438 0.063739 0.104230 11.00000 -1.20000 AFIX 0 C37 1 0.799567 0.040633 -0.006801 11.00000 0.08289 0.08154 = 0.08227 -0.01825 -0.01242 -0.02964 AFIX 23 H37A 2 0.864968 0.007574 0.020043 11.00000 -1.20000 H37B 2 0.821284 0.081022 -0.060146 11.00000 -1.20000 AFIX 0 C38 1 0.765345 -0.031856 -0.026425 11.00000 0.25284 0.25291 = 0.25268 -0.05399 -0.04270 -0.08172 AFIX 137 H38A 2 0.772006 -0.085997 0.020383 11.00000 -1.50000 H38B 2 0.812717 -0.051458 -0.076953 11.00000 -1.50000 H38C 2 0.689388 -0.004546 -0.035275 11.00000 -1.50000 AFIX 0 C39 1 0.560205 0.281466 0.093309 11.00000 0.06750 0.06296 = 0.06267 -0.01519 -0.01082 -0.02364 AFIX 23 H39A 2 0.615443 0.242255 0.129174 11.00000 -1.20000 H39B 2 0.497777 0.319693 0.127706 11.00000 -1.20000 AFIX 0 C40 1 0.609781 0.346427 0.022433 11.00000 0.06589 0.06468 = 0.06322 -0.01612 -0.01259 -0.02230 AFIX 23 H40A 2 0.554087 0.389706 -0.011771 11.00000 -1.20000 H40B 2 0.671007 0.309721 -0.013894 11.00000 -1.20000 AFIX 0 C41 1 0.651195 0.401738 0.059821 11.00000 0.07864 0.07558 = 0.07777 -0.01491 -0.01360 -0.02988 AFIX 23 H41A 2 0.668947 0.452717 0.014995 11.00000 -1.20000 H41B 2 0.591397 0.430684 0.101878 11.00000 -1.20000 AFIX 0 C42 1 0.750554 0.344995 0.100532 11.00000 0.08306 0.08534 = 0.08320 -0.01725 -0.01646 -0.02858 AFIX 137 H42A 2 0.729074 0.305883 0.153934 11.00000 -1.50000 H42B 2 0.782153 0.387016 0.110123 11.00000 -1.50000 H42C 2 0.804771 0.305345 0.063901 11.00000 -1.50000 AFIX 0 C43 1 0.436225 0.275464 0.011485 11.00000 0.07348 0.07380 = 0.07548 -0.01428 -0.01284 -0.02442 AFIX 23 H43A 2 0.414519 0.232750 -0.007908 11.00000 -1.20000 H43B 2 0.469846 0.312907 -0.038358 11.00000 -1.20000 AFIX 0 C44 1 0.332709 0.341673 0.053768 11.00000 0.06499 0.06670 = 0.06767 -0.01742 -0.01186 -0.02253 AFIX 23 H44A 2 0.351297 0.390900 0.065918 11.00000 -1.20000 H44B 2 0.302634 0.306494 0.107211 11.00000 -1.20000 AFIX 0 C45 1 0.245977 0.386869 -0.004226 11.00000 0.08609 0.08234 = 0.08352 -0.02032 -0.01337 -0.02515 AFIX 23 H45A 2 0.282524 0.403686 -0.062405 11.00000 -1.20000 H45B 2 0.193437 0.444872 0.012098 11.00000 -1.20000 AFIX 0 MOLE 3 N9 3 0.797931 0.303588 0.576980 11.00000 0.04331 0.05950 = 0.07401 -0.02847 -0.01846 -0.00807 C46 1 0.183075 0.320347 0.000254 11.00000 0.10763 0.10781 = 0.10842 -0.02397 -0.01861 -0.03354 AFIX 137 H46A 2 0.234819 0.262900 -0.016013 11.00000 -1.50000 H46B 2 0.130077 0.350844 -0.037768 11.00000 -1.50000 H46C 2 0.144641 0.305324 0.057369 11.00000 -1.50000 AFIX 0 C47 1 0.895791 0.268887 0.514619 11.00000 0.05226 0.05455 = 0.05162 -0.01355 -0.00870 -0.01401 AFIX 23 H47A 2 0.892154 0.317132 0.462205 11.00000 -1.20000 H47B 2 0.891597 0.212928 0.502630 11.00000 -1.20000 AFIX 0 C48 1 1.011130 0.242909 0.539817 11.00000 0.06036 0.06232 = 0.05919 -0.01452 -0.01118 -0.01849 AFIX 23 H48A 2 1.019411 0.299088 0.548095 11.00000 -1.20000 H48B 2 1.015938 0.195864 0.592976 11.00000 -1.20000 AFIX 0 C49 1 1.102036 0.204326 0.471883 11.00000 0.05863 0.06173 = 0.06433 -0.01479 -0.01422 -0.02233 AFIX 23 H49A 2 1.104007 0.254302 0.421071 11.00000 -1.20000 H49B 2 1.087672 0.154076 0.457741 11.00000 -1.20000 AFIX 0 C50 1 1.211865 0.166015 0.501142 11.00000 0.08021 0.08281 = 0.08371 -0.01754 -0.01816 -0.02621 AFIX 137 H50A 2 1.225683 0.215738 0.515504 11.00000 -1.50000 H50B 2 1.269887 0.142562 0.456397 11.00000 -1.50000 H50C 2 1.210588 0.115130 0.550322 11.00000 -1.50000 AFIX 0 C51 1 0.789780 0.396461 0.589626 11.00000 0.05791 0.05250 = 0.05722 -0.01205 -0.01106 -0.02009 AFIX 23 H51A 2 0.853397 0.388321 0.613550 11.00000 -1.20000 H51B 2 0.723130 0.417510 0.630556 11.00000 -1.20000 AFIX 0 C52 1 0.785877 0.471904 0.509626 11.00000 0.06092 0.06228 = 0.06029 -0.01503 -0.01166 -0.01753 AFIX 23 H52A 2 0.857504 0.457484 0.472132 11.00000 -1.20000 H52B 2 0.729907 0.474111 0.480343 11.00000 -1.20000 AFIX 0 C53 1 0.758191 0.565779 0.531216 11.00000 0.06586 0.06191 = 0.06589 -0.01235 -0.00967 -0.02389 AFIX 23 H53A 2 0.689467 0.576259 0.572322 11.00000 -1.20000 H53B 2 0.744331 0.615101 0.480199 11.00000 -1.20000 AFIX 0 C54 1 0.844981 0.577016 0.566631 11.00000 0.07003 0.06960 = 0.07080 -0.01207 -0.01634 -0.02463 AFIX 137 H54A 2 0.860635 0.528046 0.616747 11.00000 -1.50000 H54B 2 0.818085 0.638193 0.581013 11.00000 -1.50000 H54C 2 0.911867 0.572015 0.524841 11.00000 -1.50000 AFIX 0 C55 1 0.705892 0.306358 0.543846 11.00000 0.05899 0.05925 = 0.05763 -0.01264 -0.01081 -0.02030 AFIX 23 H55A 2 0.710535 0.241436 0.547896 11.00000 -1.20000 H55B 2 0.714625 0.336814 0.483898 11.00000 -1.20000 AFIX 0 C56 1 0.590189 0.357199 0.586604 11.00000 0.07244 0.06933 = 0.06965 -0.01755 -0.00739 -0.02443 AFIX 23 H56A 2 0.581217 0.329776 0.647216 11.00000 -1.20000 H56B 2 0.581703 0.423772 0.578814 11.00000 -1.20000 AFIX 0 C57 1 0.502646 0.349353 0.550733 11.00000 0.06348 0.06648 = 0.06266 -0.01518 -0.01057 -0.01843 AFIX 23 H57A 2 0.431248 0.391919 0.572047 11.00000 -1.20000 H57B 2 0.517149 0.371023 0.489386 11.00000 -1.20000 AFIX 0 C58 1 0.494082 0.253544 0.570142 11.00000 0.07767 0.07982 = 0.07816 -0.01830 -0.01396 -0.02532 AFIX 137 H58A 2 0.563628 0.210847 0.548082 11.00000 -1.50000 H58B 2 0.435930 0.255158 0.544339 11.00000 -1.50000 H58C 2 0.477086 0.231967 0.630697 11.00000 -1.50000 AFIX 0 C59 1 0.804586 0.237368 0.661996 11.00000 0.07208 0.07418 = 0.07072 -0.01751 -0.01207 -0.02166 AFIX 23 H59A 2 0.866608 0.238293 0.682580 11.00000 -1.20000 H59B 2 0.737260 0.262377 0.700835 11.00000 -1.20000 AFIX 0 C60 1 0.818275 0.137002 0.667017 11.00000 0.06568 0.06472 = 0.06116 -0.01164 -0.01213 -0.01844 AFIX 23 H60A 2 0.878371 0.112973 0.622759 11.00000 -1.20000 H60B 2 0.750335 0.132668 0.658327 11.00000 -1.20000 AFIX 0 C61 1 0.843825 0.079032 0.751806 11.00000 0.07395 0.07322 = 0.07296 -0.01255 -0.01180 -0.02031 AFIX 23 H61A 2 0.789265 0.109426 0.795531 11.00000 -1.20000 H61B 2 0.836961 0.017007 0.759152 11.00000 -1.20000 AFIX 0 C62 1 0.955997 0.066367 0.763531 11.00000 0.08121 0.08153 = 0.07720 -0.01642 -0.01726 -0.02572 AFIX 137 H62A 2 1.010594 0.035753 0.720793 11.00000 -1.50000 H62B 2 0.968109 0.027726 0.818940 11.00000 -1.50000 H62C 2 0.962554 0.127350 0.758518 11.00000 -1.50000 HKLF 4 Covalent radii and connectivity table for s92 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 F 0.640 F1 - no bonds found O1 - N1 O2 - N1 O3 - N2 O4 - N2 O5 - C7 O6 - C12 O7 - N6 O8 - N6 O9 - N7 O10 - N7 N1 - O1 O2 C2 N2 - O4 O3 C4 N3 - C7 C6 N4 - C11 C8 N5 - C12 C13 N6 - O7 O8 C15 N7 - O10 O9 C17 C1 - C2 C6 C2 - C1 C3 N1 C3 - C2 C4 C4 - C5 C3 N2 C5 - C4 C6 C6 - N3 C5 C1 C7 - O5 N3 C8 C8 - N4 C9 C7 C9 - C8 C10 C19 C10 - C11 C9 C25 C11 - N4 C10 C12 C12 - O6 N5 C11 C13 - C14 C18 N5 C14 - C13 C15 C15 - C16 C14 N6 C16 - C15 C17 C17 - C16 C18 N7 C18 - C17 C13 C19 - C20 C24 C9 C20 - C19 C21 C21 - C20 C22 C22 - C21 C23 C23 - C24 C22 C24 - C23 C19 C25 - C26 C30 C10 C26 - C27 C25 C27 - C26 C28 C28 - C27 C29 C29 - C30 C28 C30 - C29 C25 N8 - C31 C43 C39 C35 C31 - N8 C32 C32 - C33 C31 C33 - C32 C34 C34 - C33 C35 - N8 C36 C36 - C37 C35 C37 - C36 C38 C38 - C37 C39 - N8 C40 C40 - C39 C41 C41 - C42 C40 C42 - C41 C43 - N8 C44 C44 - C43 C45 C45 - C44 C46 N9 - C55 C47 C51 C59 C46 - C45 C47 - N9 C48 C48 - C49 C47 C49 - C48 C50 C50 - C49 C51 - N9 C52 C52 - C53 C51 C53 - C52 C54 C54 - C53 C55 - N9 C56 C56 - C57 C55 C57 - C58 C56 C58 - C57 C59 - C60 N9 C60 - C59 C61 C61 - C62 C60 C62 - C61 19538 Reflections read, of which 347 rejected -15 =< h =< 15, -18 =< k =< 18, -17 =< l =< 18, Max. 2-theta = 50.04 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 11 4 0 2.72 1.00 2 8.99 -5 9 0 6.07 1.98 2 27.92 -13 -12 1 2.57 0.89 2 4.45 -9 -10 1 5.32 0.99 2 31.28 10 16 1 6.30 1.00 2 37.03 10 9 2 4.49 0.99 2 26.32 1 -11 3 9.85 1.97 2 27.26 11 3 3 2.41 0.99 2 29.76 -3 -13 4 1.58 0.99 2 19.74 -2 -13 4 2.96 1.96 2 19.24 -7 -12 4 10.76 0.99 2 40.28 -5 -9 6 3.18 1.00 2 12.44 8 2 6 2.16 0.58 4 3.93 -8 5 6 3.05 0.89 3 4.98 -3 8 6 1.10 0.71 3 4.23 -1 10 9 1.13 0.71 3 3.54 0 -3 10 2.31 0.58 4 4.74 1 -3 10 4.48 0.57 4 5.24 -2 -2 10 1.61 0.71 3 3.66 10 13 10 3.71 1.00 2 26.08 12 6 11 9.27 1.99 2 27.07 1 1 14 9.79 0.69 3 7.97 0 2 14 2.69 0.99 2 13.51 23 Inconsistent equivalents 8690 Unique reflections, of which 0 suppressed R(int) = 0.2915 R(sigma) = 0.7011 Friedel opposites merged Maximum memory for data reduction = 7164 / 90373 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 = 9388 / 986167 wR2 = 0.4036 before cycle 1 for 8690 data and 700 / 700 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 378. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.005 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.000 GooF = S = 0.812; Restrained GooF = 0.797 for 378 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1447 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.05969 0.00034 -0.003 OSF 2 0.01008 0.00178 0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.003 for OSF Max. shift = 0.000 A for H34C Max. dU = 0.000 for O3 Least-squares cycle 2 Maximum vector length = 511 Memory required = 9388 / 986167 wR2 = 0.4036 before cycle 2 for 8690 data and 700 / 700 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 378. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.005 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.000 GooF = S = 0.812; Restrained GooF = 0.797 for 378 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1447 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.05969 0.00034 0.000 OSF 2 0.01008 0.00178 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for U13 F1 Max. shift = 0.000 A for H34C Max. dU = 0.000 for O3 Least-squares cycle 3 Maximum vector length = 511 Memory required = 9388 / 986167 wR2 = 0.4036 before cycle 3 for 8690 data and 700 / 700 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 378. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.005 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.000 GooF = S = 0.812; Restrained GooF = 0.797 for 378 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1447 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.05969 0.00034 0.000 OSF 2 0.01008 0.00178 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for U22 O4 Max. shift = 0.000 A for H34B Max. dU = 0.000 for O3 Least-squares cycle 4 Maximum vector length = 511 Memory required = 9388 / 986167 wR2 = 0.4036 before cycle 4 for 8690 data and 700 / 700 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 378. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.005 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.000 GooF = S = 0.812; Restrained GooF = 0.797 for 378 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1447 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.05969 0.00034 0.001 OSF 2 0.01008 0.00178 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H34B Max. dU = 0.000 for O4 Largest correlation matrix elements 0.929 U33 C38 / U11 C38 0.691 z C19 / rotX C19 0.638 U33 F1 / U22 F1 0.929 U33 C38 / U22 C38 -0.690 x C19 / rotZ C19 0.637 U33 F1 / U11 F1 0.928 U22 C38 / U11 C38 0.677 U33 C46 / U22 C46 0.633 U22 F1 / U11 F1 -0.799 U12 C38 / U22 C38 0.677 U33 C46 / U11 C46 0.630 EXTI / OSF -0.798 U12 C38 / U11 C38 0.673 U22 C46 / U11 C46 0.619 x C1 / rotZ C1 -0.794 U12 C38 / U33 C38 -0.645 U23 C38 / U22 C38 -0.607 y C25 / rotZ C25 -0.777 z C1 / rotX C1 -0.644 U23 C38 / U11 C38 0.599 U33 C34 / U11 C34 0.746 x C13 / rotZ C13 -0.642 U23 C38 / U33 C38 0.598 U33 C34 / U22 C34 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 0.3733 0.4931 0.2358 43 0.880 0.000 N3 C7 C6 H5 0.5842 0.5482 0.2541 43 0.880 0.000 N5 C12 C13 H1 0.2055 0.3706 0.2400 43 0.950 0.000 C1 C2 C6 H3A -0.0198 0.5959 0.1293 43 0.950 0.000 C3 C2 C4 H5A 0.2482 0.6238 0.1726 43 0.950 0.000 C5 C4 C6 H14 0.5681 0.7016 0.1917 43 0.950 0.000 C14 C13 C15 H16 0.7804 0.8132 0.2196 43 0.950 0.000 C16 C15 C17 H18 0.8133 0.5409 0.3210 43 0.950 0.000 C18 C17 C13 H20 0.4436 0.1653 0.4088 43 0.950 0.000 C20 C19 C21 H21 0.4585 0.0099 0.4231 43 0.950 0.000 C21 C20 C22 H22 0.6103 -0.0868 0.3503 43 0.950 0.000 C22 C21 C23 H23 0.7472 -0.0281 0.2631 43 0.950 0.000 C23 C24 C22 H24 0.7323 0.1274 0.2488 43 0.950 0.000 C24 C23 C19 H26 0.7032 0.1293 0.4514 43 0.950 0.000 C26 C27 C25 H27 0.8693 0.0175 0.4814 43 0.950 0.000 C27 C26 C28 H28 1.0341 0.0375 0.4038 43 0.950 0.000 C28 C27 C29 H29 1.0330 0.1693 0.2963 43 0.950 0.000 C29 C30 C28 H30 0.8670 0.2811 0.2663 43 0.950 0.000 C30 C29 C25 H31A 0.4203 0.2034 0.1770 23 0.990 0.000 C31 N8 C32 H31B 0.5314 0.1187 0.1723 23 0.990 0.000 C31 N8 C32 H32A 0.3471 0.1419 0.1062 23 0.990 0.000 C32 C33 C31 H32B 0.4604 0.0599 0.0933 23 0.990 0.000 C32 C33 C31 H33A 0.4408 0.0053 0.2406 23 0.990 0.000 C33 C32 C34 H33B 0.3480 -0.0017 0.2022 23 0.990 0.000 C33 C32 C34 H34A 0.2194 0.1300 0.2502 137 0.980 0.000 C34 C33 H34A H34B 0.3117 0.1493 0.2792 137 0.980 0.000 C34 C33 H34A H34C 0.2744 0.0602 0.3278 137 0.980 0.000 C34 C33 H34A H35A 0.6288 0.1968 -0.0449 23 0.990 0.000 C35 N8 C36 H35B 0.5815 0.1123 -0.0001 23 0.990 0.000 C35 N8 C36 H36A 0.7444 0.1470 0.0571 23 0.990 0.000 C36 C37 C35 H36B 0.6954 0.0637 0.1042 23 0.990 0.000 C36 C37 C35 H37A 0.8650 0.0076 0.0200 23 0.990 0.000 C37 C36 C38 H37B 0.8213 0.0810 -0.0601 23 0.990 0.000 C37 C36 C38 H38A 0.7720 -0.0860 0.0204 137 0.980 0.000 C38 C37 H38A H38B 0.8127 -0.0515 -0.0770 137 0.980 0.000 C38 C37 H38A H38C 0.6894 -0.0045 -0.0353 137 0.980 0.000 C38 C37 H38A H39A 0.6154 0.2423 0.1292 23 0.990 0.000 C39 N8 C40 H39B 0.4978 0.3197 0.1277 23 0.990 0.000 C39 N8 C40 H40A 0.5541 0.3897 -0.0118 23 0.990 0.000 C40 C39 C41 H40B 0.6710 0.3097 -0.0139 23 0.990 0.000 C40 C39 C41 H41A 0.6689 0.4527 0.0150 23 0.990 0.000 C41 C42 C40 H41B 0.5914 0.4307 0.1019 23 0.990 0.000 C41 C42 C40 H42A 0.7291 0.3059 0.1539 137 0.980 0.000 C42 C41 H42A H42B 0.7822 0.3870 0.1101 137 0.980 0.000 C42 C41 H42A H42C 0.8048 0.3053 0.0639 137 0.980 0.000 C42 C41 H42A H43A 0.4145 0.2328 -0.0079 23 0.990 0.000 C43 N8 C44 H43B 0.4698 0.3129 -0.0384 23 0.990 0.000 C43 N8 C44 H44A 0.3513 0.3909 0.0659 23 0.990 0.000 C44 C43 C45 H44B 0.3026 0.3065 0.1072 23 0.990 0.000 C44 C43 C45 H45A 0.2825 0.4037 -0.0624 23 0.990 0.000 C45 C44 C46 H45B 0.1934 0.4449 0.0121 23 0.990 0.000 C45 C44 C46 H46A 0.2348 0.2629 -0.0160 137 0.980 0.000 C46 C45 H46A H46B 0.1301 0.3508 -0.0378 137 0.980 0.000 C46 C45 H46A H46C 0.1446 0.3053 0.0574 137 0.980 0.000 C46 C45 H46A H47A 0.8922 0.3171 0.4622 23 0.990 0.000 C47 N9 C48 H47B 0.8916 0.2129 0.5026 23 0.990 0.000 C47 N9 C48 H48A 1.0194 0.2991 0.5481 23 0.990 0.000 C48 C49 C47 H48B 1.0159 0.1959 0.5930 23 0.990 0.000 C48 C49 C47 H49A 1.1040 0.2543 0.4211 23 0.990 0.000 C49 C48 C50 H49B 1.0877 0.1541 0.4577 23 0.990 0.000 C49 C48 C50 H50A 1.2257 0.2157 0.5155 137 0.980 0.000 C50 C49 H50A H50B 1.2699 0.1426 0.4564 137 0.980 0.000 C50 C49 H50A H50C 1.2106 0.1151 0.5503 137 0.980 0.000 C50 C49 H50A H51A 0.8534 0.3883 0.6136 23 0.990 0.000 C51 N9 C52 H51B 0.7231 0.4175 0.6306 23 0.990 0.000 C51 N9 C52 H52A 0.8575 0.4575 0.4721 23 0.990 0.000 C52 C53 C51 H52B 0.7299 0.4741 0.4803 23 0.990 0.000 C52 C53 C51 H53A 0.6895 0.5763 0.5723 23 0.990 0.000 C53 C52 C54 H53B 0.7443 0.6151 0.4802 23 0.990 0.000 C53 C52 C54 H54A 0.8606 0.5280 0.6167 137 0.980 0.000 C54 C53 H54A H54B 0.8181 0.6382 0.5810 137 0.980 0.000 C54 C53 H54A H54C 0.9119 0.5720 0.5248 137 0.980 0.000 C54 C53 H54A H55A 0.7105 0.2414 0.5479 23 0.990 0.000 C55 N9 C56 H55B 0.7146 0.3368 0.4839 23 0.990 0.000 C55 N9 C56 H56A 0.5812 0.3298 0.6472 23 0.990 0.000 C56 C57 C55 H56B 0.5817 0.4238 0.5788 23 0.990 0.000 C56 C57 C55 H57A 0.4312 0.3919 0.5720 23 0.990 0.000 C57 C58 C56 H57B 0.5171 0.3710 0.4894 23 0.990 0.000 C57 C58 C56 H58A 0.5636 0.2108 0.5481 137 0.980 0.000 C58 C57 H58A H58B 0.4359 0.2552 0.5443 137 0.980 0.000 C58 C57 H58A H58C 0.4771 0.2320 0.6307 137 0.980 0.000 C58 C57 H58A H59A 0.8666 0.2383 0.6826 23 0.990 0.000 C59 C60 N9 H59B 0.7373 0.2624 0.7008 23 0.990 0.000 C59 C60 N9 H60A 0.8784 0.1130 0.6228 23 0.990 0.000 C60 C59 C61 H60B 0.7503 0.1327 0.6583 23 0.990 0.000 C60 C59 C61 H61A 0.7893 0.1094 0.7955 23 0.990 0.000 C61 C62 C60 H61B 0.8370 0.0170 0.7592 23 0.990 0.000 C61 C62 C60 H62A 1.0106 0.0358 0.7208 137 0.980 0.000 C62 C61 H62A H62B 0.9681 0.0277 0.8189 137 0.980 0.000 C62 C61 H62A H62C 0.9626 0.1273 0.7585 137 0.980 0.000 C62 C61 H62A s92 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq F1 0.41483 0.64830 0.18850 1.00000 0.00118 0.00151 0.00044 -0.00020 -0.00043 -0.00080 0.00088 0.00693 0.00041 0.00035 0.00034 0.00000 0.00160 0.00160 0.00164 0.00095 0.00094 0.00099 0.00137 O1 0.05340 0.33540 0.21631 1.00000 0.09851 0.07841 0.15554 -0.01148 -0.05489 -0.03411 0.10557 0.01782 0.00114 0.00106 0.00101 0.00000 0.01149 0.01068 0.01600 0.01051 0.01037 0.00938 0.00531 O2 -0.06752 0.45818 0.15678 1.00000 0.07460 0.12553 0.08186 -0.01473 -0.03607 -0.03899 0.08912 0.01712 0.00110 0.00096 0.00085 0.00000 0.01004 0.01195 0.01092 0.00856 0.00830 0.00889 0.00445 O3 -0.01213 0.75503 0.08185 1.00000 0.09383 0.09912 0.11892 0.00494 -0.05604 -0.02239 0.10540 0.02059 0.00127 0.00098 0.00098 0.00000 0.01131 0.01120 0.01387 0.00930 0.01022 0.00901 0.00514 O4 0.13190 0.76870 0.10680 1.00000 0.10889 0.06852 0.11757 -0.03020 -0.01764 -0.01849 0.09948 0.02269 0.00132 0.00096 0.00102 0.00000 0.01311 0.01066 0.01382 0.00928 0.01007 0.00908 0.00522 O5 0.35887 0.29777 0.27961 1.00000 0.06444 0.05500 0.08794 -0.01220 -0.01502 -0.02054 0.06911 0.01570 0.00087 0.00075 0.00075 0.00000 0.00818 0.00774 0.01028 0.00677 0.00671 0.00660 0.00358 O6 0.77098 0.41865 0.34403 1.00000 0.05463 0.06321 0.07374 -0.00175 -0.03674 -0.02471 0.05988 0.01345 0.00084 0.00069 0.00071 0.00000 0.00741 0.00781 0.00913 0.00622 0.00651 0.00608 0.00330 O7 0.53571 0.86434 0.11663 1.00000 0.10859 0.07182 0.08829 0.00726 -0.06402 -0.03428 0.08401 0.01766 0.00116 0.00082 0.00086 0.00000 0.01125 0.00921 0.01182 0.00742 0.00926 0.00795 0.00450 O8 0.63636 0.92805 0.14666 1.00000 0.09835 0.07338 0.17285 -0.02576 -0.05056 -0.03320 0.10787 0.01964 0.00111 0.00098 0.00105 0.00000 0.01124 0.00993 0.01699 0.00991 0.01030 0.00872 0.00546 O9 0.93762 0.73501 0.28518 1.00000 0.12189 0.08864 0.09209 -0.02785 -0.03096 -0.05429 0.09031 0.01723 0.00114 0.00097 0.00086 0.00000 0.01230 0.01035 0.01184 0.00861 0.00871 0.00942 0.00451 O10 0.94867 0.59234 0.35146 1.00000 0.07778 0.08057 0.08958 0.01105 -0.05313 -0.01891 0.08346 0.01721 0.00103 0.00097 0.00087 0.00000 0.00984 0.01028 0.01134 0.00837 0.00808 0.00802 0.00446 N1 0.01523 0.41969 0.18873 1.00000 0.07916 0.06252 0.08674 -0.00437 -0.02811 -0.03105 0.07354 0.02106 0.00143 0.00122 0.00106 0.00000 0.01286 0.01173 0.01398 0.01005 0.01025 0.01042 0.00480 N2 0.07676 0.72314 0.10794 1.00000 0.11464 0.08230 0.08892 -0.01039 -0.04728 -0.00095 0.10036 0.03222 0.00189 0.00132 0.00123 0.00000 0.01897 0.01590 0.01555 0.01178 0.01338 0.01311 0.00643 N3 0.33961 0.45380 0.23897 1.00000 0.03093 0.03863 0.10622 -0.01261 -0.01468 -0.01484 0.05763 0.01655 0.00091 0.00083 0.00087 0.00000 0.00791 0.00854 0.01253 0.00793 0.00773 0.00667 0.00405 H3 0.37335 0.49313 0.23580 1.00000 0.06915 0.00000 0.00000 N4 0.52987 0.41883 0.29267 1.00000 0.04743 0.05590 0.06294 -0.01821 -0.00849 -0.01692 0.05434 0.01740 0.00103 0.00087 0.00084 0.00000 0.00896 0.00923 0.01059 0.00745 0.00723 0.00737 0.00378 N5 0.64485 0.53531 0.27244 1.00000 0.05277 0.04104 0.06330 -0.01827 -0.01510 -0.01528 0.04969 0.01569 0.00097 0.00080 0.00078 0.00000 0.00882 0.00837 0.01037 0.00723 0.00727 0.00701 0.00365 H5 0.58416 0.54818 0.25406 1.00000 0.05963 0.00000 0.00000 N6 0.60596 0.85997 0.15001 1.00000 0.08879 0.05849 0.05813 -0.00925 -0.02117 -0.01007 0.07163 0.02699 0.00141 0.00105 0.00097 0.00000 0.01380 0.01136 0.01223 0.00897 0.00975 0.00995 0.00460 N7 0.90669 0.66534 0.30695 1.00000 0.06224 0.08122 0.06606 -0.03470 -0.00621 -0.02623 0.06562 0.02002 0.00119 0.00133 0.00105 0.00000 0.01130 0.01347 0.01287 0.01040 0.00887 0.01058 0.00444 C1 0.18080 0.43537 0.21595 1.00000 0.06534 0.06711 0.06786 -0.01331 -0.01392 -0.02086 0.06672 0.01452 0.00089 0.00055 0.00068 0.00000 0.00660 0.00659 0.00688 0.00451 0.00450 0.00460 0.00523 H1 0.20551 0.37063 0.24005 1.00000 0.08007 0.00000 0.00000 C2 0.08313 0.47444 0.18545 1.00000 0.05728 0.05916 0.05986 -0.01112 -0.01453 -0.01938 0.05808 0.01149 0.00083 0.00070 0.00071 0.00000 0.00622 0.00624 0.00650 0.00442 0.00443 0.00450 0.00477 C3 0.04699 0.56916 0.15019 1.00000 0.05880 0.06223 0.06265 -0.01875 -0.01569 -0.01551 0.06018 0.01296 0.00070 0.00074 0.00071 0.00000 0.00625 0.00635 0.00653 0.00448 0.00441 0.00448 0.00486 H3A -0.01977 0.59586 0.12935 1.00000 0.07222 0.00000 0.00000 C4 0.10851 0.62482 0.14541 1.00000 0.05901 0.06046 0.06678 -0.01318 -0.01050 -0.02111 0.06173 0.01435 0.00085 0.00054 0.00067 0.00000 0.00636 0.00641 0.00674 0.00451 0.00446 0.00458 0.00498 C5 0.20619 0.58575 0.17591 1.00000 0.04918 0.04910 0.05015 -0.01033 -0.00677 -0.01419 0.05044 0.01135 0.00079 0.00069 0.00069 0.00000 0.00594 0.00591 0.00616 0.00430 0.00428 0.00433 0.00444 H5A 0.24824 0.62379 0.17264 1.00000 0.06053 0.00000 0.00000 C6 0.24234 0.49103 0.21117 1.00000 0.05935 0.06135 0.05886 -0.01545 -0.01389 -0.01756 0.05912 0.01302 0.00070 0.00073 0.00069 0.00000 0.00633 0.00632 0.00657 0.00446 0.00445 0.00452 0.00485 C7 0.39023 0.36254 0.27107 1.00000 0.05974 0.06054 0.06094 -0.01265 -0.00767 -0.01905 0.06118 0.02549 0.00143 0.00139 0.00111 0.00000 0.00657 0.00655 0.00682 0.00457 0.00448 0.00468 0.00513 C8 0.49847 0.34331 0.29859 1.00000 0.05899 0.06212 0.06168 -0.01469 -0.01239 -0.01701 0.06099 0.02397 0.00138 0.00123 0.00109 0.00000 0.00639 0.00638 0.00664 0.00449 0.00445 0.00457 0.00494 C9 0.58099 0.25957 0.32074 1.00000 0.04806 0.04720 0.05051 -0.00757 -0.00943 -0.01636 0.04878 0.02063 0.00123 0.00104 0.00098 0.00000 0.00589 0.00587 0.00618 0.00431 0.00428 0.00434 0.00439 C10 0.66553 0.28363 0.33506 1.00000 0.04814 0.05391 0.04924 -0.00873 -0.01405 -0.01326 0.05079 0.02100 0.00123 0.00107 0.00099 0.00000 0.00590 0.00604 0.00617 0.00432 0.00431 0.00435 0.00446 C11 0.63090 0.38160 0.31164 1.00000 0.05505 0.05502 0.05156 -0.01374 -0.01113 -0.01804 0.05289 0.02197 0.00137 0.00112 0.00102 0.00000 0.00611 0.00617 0.00635 0.00439 0.00440 0.00445 0.00461 C12 0.69171 0.44325 0.31253 1.00000 0.05260 0.05558 0.05414 -0.01242 -0.01257 -0.01912 0.05279 0.02252 0.00138 0.00117 0.00108 0.00000 0.00610 0.00621 0.00643 0.00442 0.00447 0.00449 0.00463 C13 0.68509 0.60923 0.25863 1.00000 0.05428 0.05251 0.05044 -0.01077 -0.00595 -0.01821 0.05282 0.01220 0.00085 0.00063 0.00068 0.00000 0.00602 0.00602 0.00625 0.00436 0.00433 0.00443 0.00454 C14 0.63001 0.69496 0.21294 1.00000 0.06647 0.06391 0.06337 -0.01476 -0.01484 -0.01927 0.06415 0.01179 0.00073 0.00078 0.00069 0.00000 0.00652 0.00649 0.00675 0.00451 0.00446 0.00457 0.00510 H14 0.56809 0.70160 0.19165 1.00000 0.07697 0.00000 0.00000 C15 0.66552 0.77098 0.19839 1.00000 0.05915 0.05828 0.05540 -0.01161 -0.00840 -0.01827 0.05827 0.01509 0.00084 0.00059 0.00064 0.00000 0.00626 0.00629 0.00649 0.00446 0.00441 0.00450 0.00483 C16 0.75612 0.76126 0.22954 1.00000 0.06684 0.05961 0.06229 -0.01637 -0.01018 -0.02025 0.06243 0.01243 0.00086 0.00063 0.00069 0.00000 0.00652 0.00645 0.00671 0.00449 0.00446 0.00455 0.00505 H16 0.78039 0.81321 0.21960 1.00000 0.07491 0.00000 0.00000 C17 0.81120 0.67553 0.27523 1.00000 0.05280 0.05653 0.05287 -0.01009 -0.01292 -0.01843 0.05344 0.01159 0.00072 0.00077 0.00069 0.00000 0.00605 0.00613 0.00632 0.00438 0.00439 0.00444 0.00458 C18 0.77569 0.59951 0.28977 1.00000 0.06018 0.06260 0.05852 -0.01320 -0.01106 -0.01708 0.06106 0.01475 0.00083 0.00058 0.00064 0.00000 0.00633 0.00635 0.00656 0.00445 0.00442 0.00448 0.00491 H18 0.81333 0.54091 0.32100 1.00000 0.07328 0.00000 0.00000 C19 0.58653 0.16097 0.32745 1.00000 0.05585 0.05657 0.05408 -0.01233 -0.01407 -0.01651 0.05497 0.01262 0.00088 0.00054 0.00067 0.00000 0.00613 0.00613 0.00635 0.00440 0.00435 0.00442 0.00465 C20 0.50522 0.12606 0.37923 1.00000 0.05785 0.05737 0.05116 -0.01348 -0.01340 -0.01477 0.05540 0.01448 0.00074 0.00069 0.00065 0.00000 0.00617 0.00615 0.00633 0.00441 0.00435 0.00441 0.00467 H20 0.44359 0.16531 0.40881 1.00000 0.06647 0.00000 0.00000 C21 0.51407 0.03371 0.38774 1.00000 0.06967 0.06572 0.06126 -0.01336 -0.01679 -0.02245 0.06433 0.01411 0.00080 0.00073 0.00064 0.00000 0.00659 0.00657 0.00677 0.00452 0.00448 0.00458 0.00516 H21 0.45850 0.00985 0.42312 1.00000 0.07720 0.00000 0.00000 C22 0.60425 -0.02372 0.34446 1.00000 0.07231 0.07246 0.06987 -0.01355 -0.01993 -0.02340 0.07038 0.01342 0.00093 0.00055 0.00072 0.00000 0.00674 0.00674 0.00697 0.00457 0.00452 0.00465 0.00538 H22 0.61030 -0.08684 0.35028 1.00000 0.08446 0.00000 0.00000 C23 0.68556 0.01118 0.29269 1.00000 0.07704 0.07852 0.07850 -0.01664 -0.01329 -0.02483 0.07820 0.01532 0.00077 0.00070 0.00069 0.00000 0.00712 0.00709 0.00733 0.00464 0.00458 0.00473 0.00582 H23 0.74719 -0.02807 0.26311 1.00000 0.09384 0.00000 0.00000 C24 0.67671 0.10353 0.28418 1.00000 0.05793 0.05318 0.05272 -0.01200 -0.00965 -0.01392 0.05567 0.01425 0.00077 0.00074 0.00062 0.00000 0.00612 0.00605 0.00632 0.00437 0.00434 0.00439 0.00464 H24 0.73228 0.12739 0.24879 1.00000 0.06680 0.00000 0.00000 C25 0.76951 0.21572 0.35604 1.00000 0.04448 0.04450 0.04422 -0.01149 -0.01189 -0.01358 0.04334 0.01380 0.00069 0.00064 0.00067 0.00000 0.00568 0.00564 0.00593 0.00422 0.00421 0.00424 0.00410 C26 0.77018 0.13741 0.41993 1.00000 0.05813 0.06068 0.05695 -0.01583 -0.01362 -0.01922 0.05711 0.01375 0.00071 0.00075 0.00063 0.00000 0.00621 0.00625 0.00645 0.00443 0.00439 0.00446 0.00474 H26 0.70324 0.12928 0.45143 1.00000 0.06853 0.00000 0.00000 C27 0.86880 0.07101 0.43772 1.00000 0.07110 0.07110 0.06770 -0.01553 -0.01719 -0.01982 0.06972 0.01508 0.00093 0.00062 0.00061 0.00000 0.00677 0.00679 0.00699 0.00455 0.00454 0.00466 0.00540 H27 0.86926 0.01750 0.48139 1.00000 0.08367 0.00000 0.00000 C28 0.96675 0.08291 0.39164 1.00000 0.07785 0.07426 0.07519 -0.02199 -0.01610 -0.01841 0.07569 0.01489 0.00071 0.00068 0.00074 0.00000 0.00701 0.00691 0.00715 0.00461 0.00459 0.00466 0.00562 H28 1.03415 0.03753 0.40380 1.00000 0.09083 0.00000 0.00000 C29 0.96608 0.16121 0.32775 1.00000 0.07750 0.07402 0.07395 -0.01907 -0.01511 -0.02310 0.07444 0.01454 0.00070 0.00079 0.00068 0.00000 0.00698 0.00690 0.00716 0.00460 0.00456 0.00467 0.00562 H29 1.03302 0.16935 0.29625 1.00000 0.08933 0.00000 0.00000 C30 0.86746 0.22762 0.30995 1.00000 0.06324 0.05982 0.06337 -0.01421 -0.01467 -0.01674 0.06212 0.01479 0.00090 0.00063 0.00059 0.00000 0.00637 0.00631 0.00660 0.00444 0.00445 0.00452 0.00493 H30 0.86700 0.28113 0.26629 1.00000 0.07454 0.00000 0.00000 N8 0.52084 0.21810 0.06582 1.00000 0.06585 0.07130 0.06506 -0.01951 -0.02171 -0.01383 0.06669 0.01849 0.00112 0.00096 0.00092 0.00000 0.01022 0.01030 0.01162 0.00887 0.00835 0.00847 0.00420 C31 0.47186 0.16054 0.14113 1.00000 0.05710 0.05746 0.05903 -0.01243 -0.01413 -0.01750 0.05736 0.02063 0.00129 0.00108 0.00107 0.00000 0.00619 0.00619 0.00647 0.00446 0.00442 0.00446 0.00474 H31A 0.42033 0.20335 0.17702 1.00000 0.06883 0.00000 0.00000 H31B 0.53141 0.11872 0.17228 1.00000 0.06883 0.00000 0.00000 C32 0.41208 0.10104 0.13161 1.00000 0.05782 0.05454 0.05601 -0.01197 -0.01156 -0.01949 0.05535 0.02040 0.00128 0.00104 0.00101 0.00000 0.00608 0.00608 0.00636 0.00441 0.00436 0.00441 0.00463 H32A 0.34706 0.14192 0.10617 1.00000 0.06642 0.00000 0.00000 H32B 0.46040 0.05991 0.09327 1.00000 0.06642 0.00000 0.00000 C33 0.37658 0.04236 0.21310 1.00000 0.07001 0.06858 0.07177 -0.01644 -0.01419 -0.02278 0.06931 0.02347 0.00137 0.00112 0.00106 0.00000 0.00665 0.00668 0.00695 0.00457 0.00452 0.00461 0.00530 H33A 0.44081 0.00525 0.24063 1.00000 0.08317 0.00000 0.00000 H33B 0.34803 -0.00168 0.20223 1.00000 0.08317 0.00000 0.00000 C34 0.28728 0.10087 0.27310 1.00000 0.09034 0.08695 0.09073 -0.01993 -0.01587 -0.03169 0.08820 0.02552 0.00149 0.00128 0.00122 0.00000 0.00761 0.00752 0.00786 0.00473 0.00469 0.00488 0.00635 H34A 0.21943 0.13000 0.25021 1.00000 0.13229 0.00000 0.00000 H34B 0.31171 0.14934 0.27917 1.00000 0.13229 0.00000 0.00000 H34C 0.27439 0.06016 0.32776 1.00000 0.13229 0.00000 0.00000 C35 0.60993 0.15700 0.00973 1.00000 0.06969 0.07222 0.07121 -0.01771 -0.01456 -0.02106 0.07060 0.02359 0.00137 0.00119 0.00117 0.00000 0.00666 0.00666 0.00691 0.00458 0.00455 0.00462 0.00529 H35A 0.62877 0.19684 -0.04489 1.00000 0.08472 0.00000 0.00000 H35B 0.58150 0.11229 -0.00009 1.00000 0.08472 0.00000 0.00000 C36 0.71423 0.10252 0.04895 1.00000 0.06506 0.06761 0.06851 -0.01374 -0.01334 -0.02161 0.06685 0.02276 0.00127 0.00114 0.00112 0.00000 0.00654 0.00652 0.00680 0.00451 0.00448 0.00457 0.00515 H36A 0.74438 0.14702 0.05713 1.00000 0.08022 0.00000 0.00000 H36B 0.69544 0.06374 0.10423 1.00000 0.08022 0.00000 0.00000 C37 0.79957 0.04063 -0.00680 1.00000 0.08290 0.08154 0.08228 -0.01825 -0.01242 -0.02964 0.08155 0.02531 0.00150 0.00126 0.00125 0.00000 0.00721 0.00720 0.00746 0.00467 0.00461 0.00479 0.00594 H37A 0.86497 0.00757 0.02004 1.00000 0.09786 0.00000 0.00000 H37B 0.82128 0.08102 -0.06015 1.00000 0.09786 0.00000 0.00000 C38 0.76534 -0.03186 -0.02642 1.00000 0.25284 0.25291 0.25268 -0.05399 -0.04270 -0.08172 0.25311 0.05267 0.00321 0.00259 0.00245 0.00000 0.01899 0.01897 0.01912 0.00626 0.00585 0.00760 0.01851 H38A 0.77201 -0.08600 0.02038 1.00000 0.37967 0.00000 0.00000 H38B 0.81272 -0.05146 -0.07695 1.00000 0.37967 0.00000 0.00000 H38C 0.68939 -0.00455 -0.03527 1.00000 0.37967 0.00000 0.00000 C39 0.56020 0.28147 0.09331 1.00000 0.06750 0.06296 0.06267 -0.01519 -0.01082 -0.02364 0.06331 0.02218 0.00137 0.00112 0.00109 0.00000 0.00649 0.00640 0.00671 0.00451 0.00447 0.00456 0.00504 H39A 0.61544 0.24226 0.12917 1.00000 0.07598 0.00000 0.00000 H39B 0.49778 0.31969 0.12771 1.00000 0.07598 0.00000 0.00000 C40 0.60978 0.34643 0.02243 1.00000 0.06589 0.06468 0.06322 -0.01612 -0.01259 -0.02230 0.06341 0.02148 0.00136 0.00112 0.00108 0.00000 0.00648 0.00643 0.00668 0.00450 0.00445 0.00453 0.00503 H40A 0.55409 0.38971 -0.01177 1.00000 0.07609 0.00000 0.00000 H40B 0.67101 0.30972 -0.01389 1.00000 0.07609 0.00000 0.00000 C41 0.65119 0.40174 0.05982 1.00000 0.07865 0.07559 0.07778 -0.01491 -0.01360 -0.02988 0.07619 0.02337 0.00147 0.00122 0.00120 0.00000 0.00697 0.00695 0.00728 0.00460 0.00457 0.00473 0.00567 H41A 0.66895 0.45272 0.01500 1.00000 0.09143 0.00000 0.00000 H41B 0.59140 0.43068 0.10188 1.00000 0.09143 0.00000 0.00000 C42 0.75055 0.34500 0.10053 1.00000 0.08307 0.08534 0.08320 -0.01725 -0.01646 -0.02858 0.08323 0.02477 0.00145 0.00124 0.00119 0.00000 0.00734 0.00734 0.00759 0.00468 0.00465 0.00482 0.00607 H42A 0.72907 0.30588 0.15393 1.00000 0.12485 0.00000 0.00000 H42B 0.78215 0.38702 0.11012 1.00000 0.12485 0.00000 0.00000 H42C 0.80477 0.30534 0.06390 1.00000 0.12485 0.00000 0.00000 C43 0.43622 0.27546 0.01149 1.00000 0.07348 0.07380 0.07549 -0.01428 -0.01284 -0.02442 0.07448 0.02499 0.00140 0.00120 0.00119 0.00000 0.00695 0.00692 0.00719 0.00459 0.00461 0.00471 0.00562 H43A 0.41452 0.23275 -0.00791 1.00000 0.08938 0.00000 0.00000 H43B 0.46985 0.31291 -0.03836 1.00000 0.08938 0.00000 0.00000 C44 0.33271 0.34167 0.05377 1.00000 0.06499 0.06670 0.06767 -0.01742 -0.01186 -0.02253 0.06532 0.02238 0.00128 0.00114 0.00110 0.00000 0.00654 0.00648 0.00679 0.00450 0.00448 0.00457 0.00511 H44A 0.35130 0.39090 0.06592 1.00000 0.07839 0.00000 0.00000 H44B 0.30263 0.30649 0.10721 1.00000 0.07839 0.00000 0.00000 C45 0.24598 0.38687 -0.00423 1.00000 0.08609 0.08234 0.08353 -0.02032 -0.01337 -0.02515 0.08431 0.02500 0.00152 0.00127 0.00127 0.00000 0.00736 0.00731 0.00758 0.00469 0.00465 0.00479 0.00609 H45A 0.28252 0.40369 -0.06240 1.00000 0.10117 0.00000 0.00000 H45B 0.19344 0.44487 0.01210 1.00000 0.10117 0.00000 0.00000 N9 0.79793 0.30359 0.57698 1.00000 0.04331 0.05950 0.07401 -0.02847 -0.01846 -0.00807 0.05661 0.01648 0.00097 0.00088 0.00090 0.00000 0.00874 0.00936 0.01167 0.00827 0.00766 0.00709 0.00389 C46 0.18308 0.32035 0.00025 1.00000 0.10763 0.10781 0.10843 -0.02397 -0.01861 -0.03354 0.10819 0.02783 0.00169 0.00138 0.00140 0.00000 0.00861 0.00862 0.00880 0.00489 0.00483 0.00511 0.00753 H46A 0.23482 0.26290 -0.01601 1.00000 0.16229 0.00000 0.00000 H46B 0.13008 0.35084 -0.03777 1.00000 0.16229 0.00000 0.00000 H46C 0.14464 0.30532 0.05737 1.00000 0.16229 0.00000 0.00000 C47 0.89579 0.26889 0.51462 1.00000 0.05227 0.05455 0.05162 -0.01355 -0.00870 -0.01401 0.05336 0.02092 0.00121 0.00107 0.00103 0.00000 0.00602 0.00601 0.00624 0.00437 0.00437 0.00436 0.00454 H47A 0.89215 0.31713 0.46221 1.00000 0.06403 0.00000 0.00000 H47B 0.89160 0.21293 0.50263 1.00000 0.06403 0.00000 0.00000 C48 1.01113 0.24291 0.53982 1.00000 0.06036 0.06232 0.05919 -0.01452 -0.01118 -0.01849 0.06052 0.02163 0.00121 0.00110 0.00105 0.00000 0.00631 0.00629 0.00655 0.00444 0.00443 0.00448 0.00487 H48A 1.01941 0.29909 0.54810 1.00000 0.07262 0.00000 0.00000 H48B 1.01594 0.19586 0.59298 1.00000 0.07262 0.00000 0.00000 C49 1.10204 0.20433 0.47188 1.00000 0.05863 0.06173 0.06434 -0.01479 -0.01422 -0.02233 0.05969 0.02113 0.00122 0.00112 0.00107 0.00000 0.00627 0.00626 0.00659 0.00443 0.00444 0.00450 0.00482 H49A 1.10401 0.25430 0.42107 1.00000 0.07162 0.00000 0.00000 H49B 1.08767 0.15408 0.45774 1.00000 0.07162 0.00000 0.00000 C50 1.21186 0.16602 0.50114 1.00000 0.08021 0.08281 0.08371 -0.01754 -0.01816 -0.02621 0.08156 0.02382 0.00138 0.00121 0.00121 0.00000 0.00720 0.00721 0.00744 0.00465 0.00463 0.00474 0.00593 H50A 1.22569 0.21574 0.51550 1.00000 0.12233 0.00000 0.00000 H50B 1.26989 0.14256 0.45640 1.00000 0.12233 0.00000 0.00000 H50C 1.21059 0.11513 0.55032 1.00000 0.12233 0.00000 0.00000 C51 0.78978 0.39646 0.58963 1.00000 0.05791 0.05250 0.05722 -0.01205 -0.01106 -0.02009 0.05492 0.02130 0.00131 0.00103 0.00101 0.00000 0.00607 0.00604 0.00638 0.00442 0.00435 0.00439 0.00459 H51A 0.85340 0.38832 0.61355 1.00000 0.06590 0.00000 0.00000 H51B 0.72313 0.41751 0.63056 1.00000 0.06590 0.00000 0.00000 C52 0.78588 0.47190 0.50963 1.00000 0.06092 0.06228 0.06029 -0.01503 -0.01166 -0.01753 0.06122 0.02206 0.00134 0.00104 0.00105 0.00000 0.00633 0.00635 0.00654 0.00448 0.00441 0.00446 0.00490 H52A 0.85750 0.45748 0.47213 1.00000 0.07346 0.00000 0.00000 H52B 0.72991 0.47411 0.48034 1.00000 0.07346 0.00000 0.00000 C53 0.75819 0.56578 0.53122 1.00000 0.06586 0.06192 0.06589 -0.01235 -0.00967 -0.02389 0.06425 0.02163 0.00134 0.00108 0.00111 0.00000 0.00647 0.00650 0.00678 0.00449 0.00445 0.00456 0.00510 H53A 0.68947 0.57626 0.57232 1.00000 0.07710 0.00000 0.00000 H53B 0.74433 0.61510 0.48020 1.00000 0.07710 0.00000 0.00000 C54 0.84498 0.57702 0.56663 1.00000 0.07003 0.06960 0.07080 -0.01207 -0.01634 -0.02463 0.06936 0.02175 0.00133 0.00112 0.00111 0.00000 0.00674 0.00672 0.00700 0.00453 0.00453 0.00463 0.00537 H54A 0.86063 0.52805 0.61675 1.00000 0.10405 0.00000 0.00000 H54B 0.81809 0.63819 0.58101 1.00000 0.10405 0.00000 0.00000 H54C 0.91187 0.57201 0.52484 1.00000 0.10405 0.00000 0.00000 C55 0.70589 0.30636 0.54385 1.00000 0.05899 0.05925 0.05763 -0.01264 -0.01081 -0.02030 0.05810 0.02119 0.00122 0.00109 0.00105 0.00000 0.00628 0.00621 0.00654 0.00442 0.00444 0.00447 0.00479 H55A 0.71054 0.24144 0.54790 1.00000 0.06972 0.00000 0.00000 H55B 0.71463 0.33681 0.48390 1.00000 0.06972 0.00000 0.00000 C56 0.59019 0.35720 0.58660 1.00000 0.07244 0.06934 0.06965 -0.01755 -0.00739 -0.02443 0.07042 0.02328 0.00133 0.00119 0.00118 0.00000 0.00683 0.00672 0.00701 0.00456 0.00453 0.00465 0.00543 H56A 0.58122 0.32978 0.64722 1.00000 0.08451 0.00000 0.00000 H56B 0.58170 0.42377 0.57881 1.00000 0.08451 0.00000 0.00000 C57 0.50265 0.34935 0.55073 1.00000 0.06348 0.06648 0.06267 -0.01518 -0.01057 -0.01843 0.06476 0.02169 0.00133 0.00113 0.00110 0.00000 0.00651 0.00655 0.00678 0.00450 0.00446 0.00453 0.00516 H57A 0.43125 0.39192 0.57205 1.00000 0.07771 0.00000 0.00000 H57B 0.51715 0.37102 0.48939 1.00000 0.07771 0.00000 0.00000 C58 0.49408 0.25354 0.57014 1.00000 0.07767 0.07983 0.07816 -0.01830 -0.01396 -0.02533 0.07819 0.02407 0.00144 0.00118 0.00118 0.00000 0.00707 0.00712 0.00732 0.00464 0.00457 0.00472 0.00580 H58A 0.56363 0.21085 0.54808 1.00000 0.11729 0.00000 0.00000 H58B 0.43593 0.25516 0.54434 1.00000 0.11729 0.00000 0.00000 H58C 0.47708 0.23197 0.63070 1.00000 0.11729 0.00000 0.00000 C59 0.80459 0.23737 0.66200 1.00000 0.07208 0.07418 0.07072 -0.01751 -0.01207 -0.02166 0.07254 0.02465 0.00146 0.00117 0.00117 0.00000 0.00685 0.00690 0.00706 0.00463 0.00453 0.00465 0.00553 H59A 0.86661 0.23829 0.68258 1.00000 0.08705 0.00000 0.00000 H59B 0.73726 0.26238 0.70083 1.00000 0.08705 0.00000 0.00000 C60 0.81828 0.13700 0.66702 1.00000 0.06568 0.06473 0.06116 -0.01164 -0.01214 -0.01844 0.06484 0.02291 0.00137 0.00108 0.00106 0.00000 0.00652 0.00657 0.00675 0.00451 0.00446 0.00453 0.00516 H60A 0.87837 0.11297 0.62276 1.00000 0.07781 0.00000 0.00000 H60B 0.75034 0.13267 0.65833 1.00000 0.07781 0.00000 0.00000 C61 0.84383 0.07903 0.75181 1.00000 0.07396 0.07322 0.07296 -0.01255 -0.01180 -0.02031 0.07533 0.02496 0.00141 0.00123 0.00115 0.00000 0.00692 0.00688 0.00712 0.00459 0.00455 0.00464 0.00560 H61A 0.78926 0.10943 0.79553 1.00000 0.09040 0.00000 0.00000 H61B 0.83696 0.01701 0.75915 1.00000 0.09040 0.00000 0.00000 C62 0.95600 0.06637 0.76353 1.00000 0.08121 0.08153 0.07720 -0.01642 -0.01726 -0.02572 0.07957 0.02390 0.00141 0.00122 0.00118 0.00000 0.00718 0.00714 0.00734 0.00462 0.00462 0.00473 0.00584 H62A 1.01059 0.03575 0.72079 1.00000 0.11936 0.00000 0.00000 H62B 0.96811 0.02773 0.81894 1.00000 0.11936 0.00000 0.00000 H62C 0.96255 0.12735 0.75852 1.00000 0.11936 0.00000 0.00000 Final Structure Factor Calculation for s92 in P-1 Total number of l.s. parameters = 700 Maximum vector length = 511 Memory required = 8688 / 24017 wR2 = 0.4036 before cycle 5 for 8690 data and 0 / 700 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 378. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.005 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.002 0.000 GooF = S = 0.812; Restrained GooF = 0.797 for 378 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1447 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1467 for 1664 Fo > 4sig(Fo) and 0.4882 for all 8690 data wR2 = 0.4036, GooF = S = 0.812, Restrained GooF = 0.797 for all data Occupancy sum of asymmetric unit = 82.00 for non-hydrogen and 90.00 for hydrogen atoms Principal mean square atomic displacements U 0.0017 0.0009 0.0000 F1 0.1685 0.0816 0.0666 O1 0.1292 0.0950 0.0432 O2 0.1493 0.1096 0.0572 O3 0.1187 0.1162 0.0635 O4 0.0896 0.0638 0.0539 O5 0.0930 0.0588 0.0278 O6 0.1426 0.0689 0.0405 O7 0.1781 0.0878 0.0577 O8 0.1282 0.0973 0.0454 O9 0.1262 0.0890 0.0352 O10 0.0998 0.0661 0.0547 N1 0.1485 0.0960 0.0566 N2 0.1087 0.0392 0.0250 N3 0.0649 0.0515 0.0466 N4 0.0658 0.0502 0.0331 N5 0.1009 0.0626 0.0514 N6 0.0908 0.0605 0.0456 N7 0.0693 0.0674 0.0634 C1 0.0631 0.0587 0.0525 C2 0.0708 0.0576 0.0521 C3 0.0672 0.0613 0.0567 C4 0.0545 0.0493 0.0475 C5 0.0651 0.0592 0.0531 C6 0.0653 0.0604 0.0578 C7 0.0652 0.0602 0.0576 C8 0.0531 0.0476 0.0456 C9 0.0571 0.0534 0.0419 C10 0.0561 0.0553 0.0473 C11 0.0564 0.0556 0.0463 C12 0.0569 0.0526 0.0489 C13 0.0694 0.0635 0.0596 C14 0.0617 0.0581 0.0550 C15 0.0674 0.0637 0.0561 C16 0.0580 0.0546 0.0477 C17 0.0658 0.0593 0.0581 C18 0.0599 0.0561 0.0489 C19 0.0635 0.0550 0.0477 C20 0.0715 0.0654 0.0561 C21 0.0778 0.0724 0.0610 C22 0.0793 0.0782 0.0770 C23 0.0626 0.0528 0.0517 C24 0.0489 0.0440 0.0371 C25 0.0628 0.0594 0.0491 C26 0.0764 0.0701 0.0627 C27 0.0864 0.0735 0.0672 C28 0.0795 0.0750 0.0688 C29 0.0679 0.0599 0.0585 C30 0.0837 0.0645 0.0518 N8 0.0617 0.0575 0.0528 C31 0.0587 0.0554 0.0520 C32 0.0729 0.0696 0.0655 C33 0.0915 0.0908 0.0824 C34 0.0754 0.0697 0.0667 C35 0.0695 0.0674 0.0637 C36 0.0856 0.0816 0.0774 C37 0.2549 0.2531 0.2514 C38 0.0683 0.0633 0.0584 C39 0.0664 0.0659 0.0579 C40 0.0814 0.0778 0.0693 C41 0.0866 0.0835 0.0796 C42 0.0774 0.0738 0.0723 C43 0.0696 0.0658 0.0605 C44 0.0883 0.0850 0.0797 C45 0.0839 0.0471 0.0389 N9 0.1094 0.1085 0.1067 C46 0.0583 0.0523 0.0495 C47 0.0637 0.0601 0.0578 C48 0.0655 0.0628 0.0508 C49 0.0857 0.0829 0.0761 C50 0.0588 0.0565 0.0495 C51 0.0653 0.0598 0.0585 C52 0.0681 0.0663 0.0584 C53 0.0757 0.0677 0.0647 C54 0.0602 0.0581 0.0560 C55 0.0772 0.0679 0.0661 C56 0.0692 0.0635 0.0616 C57 0.0803 0.0780 0.0763 C58 0.0762 0.0721 0.0694 C59 0.0700 0.0645 0.0601 C60 0.0833 0.0726 0.0700 C61 0.0827 0.0818 0.0741 C62 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.004 0.007 0.010 0.013 0.018 0.023 0.029 0.039 0.058 1.000 Number in group 1156. 829. 739. 761. 1033. 798. 800. 867. 845. 862. GooF 0.746 0.741 0.779 0.740 0.797 0.765 0.809 0.846 0.849 1.019 K 50.027 6.260 5.716 2.513 1.769 1.327 1.278 1.076 1.020 1.100 Resolution(A) 0.84 0.91 0.96 1.01 1.06 1.13 1.21 1.33 1.50 1.86 inf Number in group 886. 881. 872. 865. 851. 872. 866. 863. 865. 869. GooF 0.772 0.784 0.802 0.805 0.807 0.847 0.775 0.750 0.729 1.018 K 3.575 1.900 1.449 1.342 1.204 1.291 1.115 1.175 1.053 1.115 R1 1.024 0.964 0.817 0.709 0.590 0.475 0.448 0.396 0.248 0.133 Recommended weighting scheme: WGHT 0.1048 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) 2 0 1 1656.87 4188.56 6.42 0.151 6.08 -1 1 4 348762.56 182651.11 5.87 1.000 3.60 4 -4 14 1398.40 167.85 5.39 0.030 0.99 2 -11 3 994.65 159.67 5.19 0.030 1.13 -4 14 1 1119.90 0.23 5.03 0.001 0.90 -13 -3 3 1128.43 38.95 4.88 0.015 0.93 3 5 0 1497.06 739.40 4.50 0.064 2.81 2 3 2 2085.53 3763.47 4.45 0.144 4.68 6 -11 7 1945.08 0.09 4.43 0.001 0.87 14 11 9 976.79 17.89 4.34 0.010 0.90 7 17 1 21896.17 12.14 4.29 0.008 0.89 12 9 8 611.34 18.89 4.05 0.010 1.05 -2 1 1 2373.47 4018.95 4.04 0.148 4.75 6 -5 9 990.47 352.95 3.84 0.044 1.14 2 0 2 2777.20 4563.89 3.84 0.158 5.33 10 12 1 836.41 0.06 3.82 0.001 1.06 1 0 3 5768.38 9477.85 3.82 0.228 5.24 12 9 14 839.22 0.14 3.80 0.001 0.92 0 -7 15 839.22 1.59 3.79 0.003 0.87 3 -12 3 696.51 102.37 3.79 0.024 1.01 12 -1 4 1667.26 10.75 3.79 0.008 1.00 -8 -12 2 69.47 881.50 3.74 0.069 1.08 4 4 15 0.00 853.32 3.74 0.068 1.13 5 10 12 836.46 18.93 3.73 0.010 1.20 13 2 2 836.46 19.70 3.73 0.010 0.99 13 8 11 879.09 52.96 3.72 0.017 0.95 0 -12 10 828.02 15.35 3.71 0.009 0.87 5 -1 13 374.38 939.42 3.71 0.072 1.15 2 4 3 1749.23 2847.50 3.71 0.125 3.61 1 3 4 2307.50 1477.37 3.69 0.090 3.73 0 -2 1 1279.54 613.50 3.68 0.058 6.08 10 9 5 1294.15 558.35 3.67 0.055 1.24 -2 -1 7 833.75 32.72 3.66 0.013 1.99 -8 8 3 842.11 38.29 3.63 0.014 1.00 3 15 10 701.93 126.18 3.63 0.026 0.98 1 1 4 1706.85 786.87 3.61 0.066 4.24 12 -1 10 844.93 44.54 3.61 0.016 0.91 1 3 2 711.20 1450.09 3.57 0.089 4.99 10 17 7 569.78 7.79 3.56 0.007 0.88 1 4 4 2528.20 1461.82 3.56 0.089 3.25 1 3 3 5011.42 7864.86 3.55 0.208 4.38 13 9 4 1115.73 15.70 3.54 0.009 1.00 1 10 14 839.37 63.41 3.50 0.019 1.04 12 1 1 558.57 15.28 3.48 0.009 1.05 -7 -11 5 140.62 710.11 3.44 0.062 1.06 3 0 1 2660.68 4138.13 3.44 0.151 4.13 1 -3 3 874.20 132.19 3.36 0.027 3.04 10 -1 13 833.82 99.17 3.34 0.023 0.93 -1 3 2 1143.96 1966.64 3.33 0.104 3.80 3 -11 3 555.81 44.71 3.30 0.016 1.09 Bond lengths and angles O1 - Distance Angles N1 1.2313 (0.0163) O1 - O2 - Distance Angles N1 1.2317 (0.0170) O2 - O3 - Distance Angles N2 1.2533 (0.0201) O3 - O4 - Distance Angles N2 1.2049 (0.0205) O4 - O5 - Distance Angles C7 1.2063 (0.0181) O5 - O6 - Distance Angles C12 1.1991 (0.0171) O6 - O7 - Distance Angles N6 1.1938 (0.0174) O7 - O8 - Distance Angles N6 1.2704 (0.0172) O8 - O9 - Distance Angles N7 1.2454 (0.0159) O9 - O10 - Distance Angles N7 1.2064 (0.0167) O10 - N1 - Distance Angles O1 1.2313 (0.0163) O2 1.2317 (0.0169) 125.57 (1.58) C2 1.4561 (0.0159) 115.16 (1.55) 118.82 (1.51) N1 - O1 O2 N2 - Distance Angles O4 1.2049 (0.0205) O3 1.2533 (0.0200) 125.02 (2.03) C4 1.4432 (0.0195) 120.14 (1.91) 114.76 (2.01) N2 - O4 O3 N3 - Distance Angles C7 1.3605 (0.0193) C6 1.3638 (0.0133) 127.16 (1.26) N3 - C7 N4 - Distance Angles C11 1.3450 (0.0179) C8 1.3798 (0.0187) 104.82 (1.30) N4 - C11 N5 - Distance Angles C12 1.3959 (0.0181) C13 1.4012 (0.0127) 126.31 (1.25) N5 - C12 N6 - Distance Angles O7 1.1938 (0.0173) O8 1.2704 (0.0172) 125.14 (1.56) C15 1.4600 (0.0158) 120.09 (1.59) 114.76 (1.60) N6 - O7 O8 N7 - Distance Angles O10 1.2064 (0.0167) O9 1.2454 (0.0159) 125.61 (1.61) C17 1.4545 (0.0159) 118.84 (1.54) 115.55 (1.62) N7 - O10 O9 C1 - Distance Angles C2 1.3900 C6 1.3900 120.00 C1 - C2 C2 - Distance Angles C1 1.3900 C3 1.3900 120.00 N1 1.4561 (0.0159) 122.48 (1.04) 117.52 (1.04) C2 - C1 C3 C3 - Distance Angles C2 1.3900 C4 1.3900 120.00 C3 - C2 C4 - Distance Angles C5 1.3900 C3 1.3900 120.00 N2 1.4432 (0.0195) 117.26 (1.23) 122.72 (1.23) C4 - C5 C3 C5 - Distance Angles C4 1.3900 C6 1.3900 120.00 C5 - C4 C6 - Distance Angles N3 1.3638 (0.0133) C5 1.3900 119.00 (0.90) C1 1.3900 120.98 (0.90) 120.00 C6 - N3 C5 C7 - Distance Angles O5 1.2063 (0.0181) N3 1.3605 (0.0193) 126.92 (1.65) C8 1.5371 (0.0222) 118.61 (1.71) 114.47 (1.57) C7 - O5 N3 C8 - Distance Angles N4 1.3798 (0.0187) C9 1.3990 (0.0196) 110.98 (1.44) C7 1.5371 (0.0222) 117.71 (1.55) 130.85 (1.62) C8 - N4 C9 C9 - Distance Angles C8 1.3990 (0.0196) C10 1.4185 (0.0187) 106.59 (1.36) C19 1.5079 (0.0160) 129.44 (1.36) 123.95 (1.29) C9 - C8 C10 C10 - Distance Angles C11 1.4080 (0.0190) C9 1.4185 (0.0187) 103.83 (1.32) C25 1.4648 (0.0163) 131.53 (1.38) 123.91 (1.33) C10 - C11 C9 C11 - Distance Angles N4 1.3450 (0.0179) C10 1.4080 (0.0190) 113.39 (1.36) C12 1.4933 (0.0204) 120.26 (1.45) 126.20 (1.55) C11 - N4 C10 C12 - Distance Angles O6 1.1991 (0.0171) N5 1.3959 (0.0181) 122.74 (1.46) C11 1.4933 (0.0204) 125.26 (1.58) 112.00 (1.45) C12 - O6 N5 C13 - Distance Angles C14 1.3900 C18 1.3900 120.00 N5 1.4012 (0.0127) 117.61 (0.94) 122.38 (0.94) C13 - C14 C18 C14 - Distance Angles C13 1.3900 C15 1.3900 120.00 C14 - C13 C15 - Distance Angles C16 1.3900 C14 1.3900 120.00 N6 1.4600 (0.0158) 121.40 (1.09) 118.60 (1.09) C15 - C16 C14 C16 - Distance Angles C15 1.3900 C17 1.3900 120.00 C16 - C15 C17 - Distance Angles C16 1.3900 C18 1.3900 120.00 N7 1.4545 (0.0160) 119.86 (1.09) 120.13 (1.09) C17 - C16 C18 C18 - Distance Angles C17 1.3900 C13 1.3900 120.00 C18 - C17 C19 - Distance Angles C20 1.3900 C24 1.3900 120.00 C9 1.5079 (0.0160) 120.70 (0.92) 119.24 (0.92) C19 - C20 C24 C20 - Distance Angles C19 1.3900 C21 1.3900 120.00 C20 - C19 C21 - Distance Angles C20 1.3900 C22 1.3900 120.00 C21 - C20 C22 - Distance Angles C21 1.3900 C23 1.3900 120.00 C22 - C21 C23 - Distance Angles C24 1.3900 C22 1.3900 120.00 C23 - C24 C24 - Distance Angles C23 1.3900 C19 1.3900 120.00 C24 - C23 C25 - Distance Angles C26 1.3900 C30 1.3900 120.00 C10 1.4648 (0.0163) 119.91 (0.97) 120.04 (0.97) C25 - C26 C30 C26 - Distance Angles C27 1.3900 C25 1.3900 120.00 C26 - C27 C27 - Distance Angles C26 1.3900 C28 1.3900 120.00 C27 - C26 C28 - Distance Angles C27 1.3900 C29 1.3900 120.00 C28 - C27 C29 - Distance Angles C30 1.3900 C28 1.3900 120.00 C29 - C30 C30 - Distance Angles C29 1.3900 C25 1.3900 120.00 C30 - C29 N8 - Distance Angles C31 1.4930 (0.0187) C43 1.5033 (0.0196) 109.34 (1.29) C39 1.5187 (0.0189) 109.08 (1.29) 109.99 (1.28) C35 1.5329 (0.0206) 111.39 (1.28) 103.38 (1.36) 113.50 (1.28) N8 - C31 C43 C39 C31 - Distance Angles N8 1.4930 (0.0187) C32 1.5100 (0.0190) 120.12 (1.43) C31 - N8 C32 - Distance Angles C33 1.4989 (0.0199) C31 1.5100 (0.0190) 112.60 (1.46) C32 - C33 C33 - Distance Angles C32 1.4989 (0.0199) C34 1.5539 (0.0222) 112.96 (1.39) C33 - C32 C34 - Distance Angles C33 1.5539 (0.0222) C34 - C35 - Distance Angles N8 1.5329 (0.0206) C36 1.5490 (0.0210) 111.95 (1.46) C35 - N8 C36 - Distance Angles C37 1.5178 (0.0221) C35 1.5490 (0.0210) 110.69 (1.55) C36 - C37 C37 - Distance Angles C36 1.5178 (0.0221) C38 1.5298 (0.0358) 116.14 (2.05) C37 - C36 C38 - Distance Angles C37 1.5298 (0.0358) C38 - C39 - Distance Angles N8 1.5187 (0.0189) C40 1.5238 (0.0200) 114.89 (1.41) C39 - N8 C40 - Distance Angles C39 1.5238 (0.0200) C41 1.5353 (0.0214) 108.77 (1.47) C40 - C39 C41 - Distance Angles C42 1.5135 (0.0219) C40 1.5353 (0.0214) 114.87 (1.51) C41 - C42 C42 - Distance Angles C41 1.5135 (0.0219) C42 - C43 - Distance Angles N8 1.5033 (0.0196) C44 1.5398 (0.0218) 114.96 (1.56) C43 - N8 C44 - Distance Angles C43 1.5398 (0.0218) C45 1.5522 (0.0221) 109.96 (1.54) C44 - C43 C45 - Distance Angles C44 1.5522 (0.0221) C46 1.5532 (0.0233) 111.88 (1.54) C45 - C44 N9 - Distance Angles C55 1.4679 (0.0177) C47 1.4894 (0.0187) 104.36 (1.25) C51 1.5088 (0.0173) 113.86 (1.18) 111.46 (1.20) C59 1.5217 (0.0195) 110.42 (1.28) 110.87 (1.22) 105.98 (1.22) N9 - C55 C47 C51 C46 - Distance Angles C45 1.5532 (0.0233) C46 - C47 - Distance Angles N9 1.4894 (0.0186) C48 1.5860 (0.0200) 116.52 (1.34) C47 - N9 C48 - Distance Angles C49 1.5198 (0.0210) C47 1.5860 (0.0200) 110.11 (1.37) C48 - C49 C49 - Distance Angles C48 1.5198 (0.0210) C50 1.5253 (0.0209) 110.30 (1.48) C49 - C48 C50 - Distance Angles C49 1.5253 (0.0209) C50 - C51 - Distance Angles N9 1.5088 (0.0172) C52 1.5257 (0.0199) 113.59 (1.37) C51 - N9 C52 - Distance Angles C53 1.5232 (0.0201) C51 1.5257 (0.0199) 109.29 (1.44) C52 - C53 C53 - Distance Angles C52 1.5232 (0.0201) C54 1.5285 (0.0201) 115.75 (1.36) C53 - C52 C54 - Distance Angles C53 1.5285 (0.0201) C54 - C55 - Distance Angles N9 1.4679 (0.0177) C56 1.5487 (0.0207) 116.46 (1.36) C55 - N9 C56 - Distance Angles C57 1.5156 (0.0205) C55 1.5487 (0.0208) 111.22 (1.43) C56 - C57 C57 - Distance Angles C58 1.4984 (0.0196) C56 1.5156 (0.0205) 115.23 (1.44) C57 - C58 C58 - Distance Angles C57 1.4984 (0.0196) C58 - C59 - Distance Angles C60 1.5104 (0.0202) N9 1.5217 (0.0196) 117.42 (1.46) C59 - C60 C60 - Distance Angles C59 1.5104 (0.0202) C61 1.5153 (0.0210) 109.54 (1.47) C60 - C59 C61 - Distance Angles C62 1.5004 (0.0208) C60 1.5153 (0.0210) 113.24 (1.50) C61 - C62 C62 - Distance Angles C61 1.5004 (0.0208) C62 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 2.58 3.403(12) 156.8 N3-H3...F1 0.88 2.55 3.385(13) 157.7 N5-H5...F1 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)