+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 15:56:40 on 03-Aug-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 01mel003 in P2(1)/c CELL 0.71073 21.7299 21.3998 17.0880 90 91.318 90 ZERR 16 0.0004 0.0004 0.0004 0 0.003 0 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H N O S UNIT 256 592 16 64 16 V = 7944.08 F(000) = 3008.0 Mu = 0.18 mm-1 Cell Wt = 5432.42 Rho = 1.136 SHEL 7 0.84 ISOR 0.005 C52 C30 C12 DFIX 1.54 0.002 C52 C51 SIZE 0.1 0.1 0.1 OMIT 2 6 0 TEMP -153 HTAB HTAB O10 O3 HTAB O4 O9 HTAB O8 O13 HTAB O15 O6 FMAP 2 PLAN 30 BOND L.S. 4 WGHT 0.136800 1.099900 EXTI 0.000000 FVAR 0.14637 C1 1 0.368571 -0.042676 0.673781 11.00000 0.02820 0.02950 = 0.04151 -0.00011 -0.00736 0.00760 AFIX 23 H1A 2 0.360779 0.000560 0.691624 11.00000 -1.20000 H1B 2 0.328256 -0.063965 0.668256 11.00000 -1.20000 AFIX 0 C2 1 0.398095 -0.040005 0.593360 11.00000 0.04154 0.03864 = 0.03833 0.00369 -0.00537 0.00755 AFIX 23 H2A 2 0.436806 -0.015683 0.597094 11.00000 -1.20000 H2B 2 0.408278 -0.082850 0.576052 11.00000 -1.20000 AFIX 0 C3 1 0.354421 -0.009682 0.533665 11.00000 0.07707 0.05159 = 0.03706 -0.00251 -0.00780 0.02460 AFIX 23 H3A 2 0.345576 0.033764 0.549831 11.00000 -1.20000 H3B 2 0.315073 -0.033004 0.531441 11.00000 -1.20000 AFIX 0 C4 1 0.383103 -0.009486 0.452521 11.00000 0.10248 0.05465 = 0.04174 0.00499 -0.00754 0.02597 AFIX 33 H4A 2 0.354604 0.010238 0.414724 11.00000 -1.50000 H4B 2 0.391212 -0.052565 0.436260 11.00000 -1.50000 H4C 2 0.421824 0.013994 0.454713 11.00000 -1.50000 AFIX 0 C5 1 0.419423 -0.143026 0.712912 11.00000 0.03504 0.02485 = 0.03846 -0.00198 -0.00551 0.00230 AFIX 23 H5A 2 0.441603 -0.163876 0.756916 11.00000 -1.20000 H5B 2 0.447164 -0.142756 0.667761 11.00000 -1.20000 AFIX 0 C6 1 0.362973 -0.181754 0.691219 11.00000 0.04526 0.03214 = 0.07720 -0.01392 -0.02354 0.00060 AFIX 23 H6A 2 0.345068 -0.166694 0.640869 11.00000 -1.20000 H6B 2 0.331606 -0.176619 0.731834 11.00000 -1.20000 AFIX 0 C7 1 0.379724 -0.250959 0.683907 11.00000 0.06166 0.03279 = 0.05710 -0.01339 -0.00793 -0.00363 AFIX 23 H7A 2 0.345359 -0.273080 0.656818 11.00000 -1.20000 H7B 2 0.416434 -0.254783 0.650989 11.00000 -1.20000 AFIX 0 C8 1 0.392654 -0.281890 0.759867 11.00000 0.08597 0.03732 = 0.08359 0.00868 -0.00226 -0.01144 AFIX 33 H8A 2 0.403468 -0.325732 0.750935 11.00000 -1.50000 H8B 2 0.356034 -0.279743 0.792179 11.00000 -1.50000 H8C 2 0.427033 -0.260700 0.786847 11.00000 -1.50000 AFIX 0 C9 1 0.469117 -0.045969 0.748188 11.00000 0.02695 0.03406 = 0.03178 -0.00131 0.00019 -0.00094 AFIX 23 H9A 2 0.492203 -0.050114 0.699183 11.00000 -1.20000 H9B 2 0.492044 -0.069394 0.789433 11.00000 -1.20000 AFIX 0 C10 1 0.467989 0.022810 0.771195 11.00000 0.03903 0.02902 = 0.05322 -0.00373 0.00139 -0.00780 AFIX 23 H10A 2 0.443259 0.046177 0.731591 11.00000 -1.20000 H10B 2 0.447349 0.026965 0.821981 11.00000 -1.20000 AFIX 0 C11 1 0.586352 0.031096 0.766834 11.00000 0.03795 0.07512 = 0.13908 -0.02493 0.00719 -0.00366 AFIX 33 H11A 2 0.615284 0.060727 0.791328 11.00000 -1.50000 H11B 2 0.593947 0.028585 0.710612 11.00000 -1.50000 H11C 2 0.592085 -0.010251 0.790556 11.00000 -1.50000 AFIX 0 C12 1 0.528281 0.050646 0.777834 11.00000 0.08966 0.08872 = 0.19356 -0.02903 0.00891 -0.01701 AFIX 23 H12A 2 0.524743 0.088047 0.743930 11.00000 -1.20000 H12B 2 0.529770 0.067003 0.832038 11.00000 -1.20000 AFIX 0 C13 1 0.370325 -0.073823 0.810966 11.00000 0.03074 0.03241 = 0.04401 -0.00275 0.01022 -0.00202 AFIX 23 H13A 2 0.329242 -0.092397 0.800406 11.00000 -1.20000 H13B 2 0.364079 -0.029536 0.825529 11.00000 -1.20000 AFIX 0 C14 1 0.400422 -0.107775 0.880405 11.00000 0.05635 0.07985 = 0.03565 0.00409 0.00586 0.01270 AFIX 23 H14A 2 0.407318 -0.151883 0.865491 11.00000 -1.20000 H14B 2 0.441218 -0.088729 0.891479 11.00000 -1.20000 AFIX 0 C15 1 0.365004 -0.106548 0.952143 11.00000 0.07742 0.06764 = 0.05393 0.00643 0.01296 -0.00568 AFIX 23 H15A 2 0.324079 -0.125334 0.941146 11.00000 -1.20000 H15B 2 0.358451 -0.062489 0.967528 11.00000 -1.20000 AFIX 0 C16 1 0.395031 -0.140620 1.019623 11.00000 0.08692 0.08355 = 0.04754 0.02186 0.00132 -0.00173 AFIX 33 H16A 2 0.368986 -0.137531 1.065527 11.00000 -1.50000 H16B 2 0.435300 -0.121899 1.031688 11.00000 -1.50000 H16C 2 0.400415 -0.184679 1.005717 11.00000 -1.50000 AFIX 0 C17 1 0.309768 0.303624 0.892048 11.00000 0.04228 0.03622 = 0.02073 0.00329 -0.00038 -0.00374 AFIX 23 H17A 2 0.345507 0.312987 0.859113 11.00000 -1.20000 H17B 2 0.281328 0.276792 0.860883 11.00000 -1.20000 AFIX 0 C18 1 0.277240 0.364245 0.909485 11.00000 0.06522 0.03648 = 0.02784 -0.00122 0.00317 -0.00207 AFIX 23 H18A 2 0.301081 0.387949 0.949637 11.00000 -1.20000 H18B 2 0.236033 0.355339 0.930362 11.00000 -1.20000 AFIX 0 C19 1 0.270536 0.403549 0.834146 11.00000 0.07229 0.04372 = 0.04632 0.00417 0.00254 0.00415 AFIX 23 H19A 2 0.252089 0.444387 0.847426 11.00000 -1.20000 H19B 2 0.312037 0.411666 0.813692 11.00000 -1.20000 AFIX 0 C20 1 0.231625 0.373283 0.770538 11.00000 0.07948 0.06636 = 0.05501 0.00740 -0.02427 0.00879 AFIX 33 H20A 2 0.229959 0.400540 0.724452 11.00000 -1.50000 H20B 2 0.189880 0.366630 0.789395 11.00000 -1.50000 H20C 2 0.249745 0.333008 0.756426 11.00000 -1.50000 AFIX 0 C21 1 0.281492 0.254792 1.020388 11.00000 0.03469 0.03464 = 0.01807 0.00062 0.00186 -0.00144 AFIX 23 H21A 2 0.298945 0.231151 1.065482 11.00000 -1.20000 H21B 2 0.267150 0.295565 1.040387 11.00000 -1.20000 AFIX 0 C22 1 0.226401 0.219408 0.988004 11.00000 0.03217 0.04121 = 0.03716 0.00274 -0.00368 -0.00452 AFIX 23 H22A 2 0.240270 0.179975 0.963774 11.00000 -1.20000 H22B 2 0.205366 0.244738 0.946952 11.00000 -1.20000 AFIX 0 C23 1 0.181677 0.204804 1.052498 11.00000 0.05003 0.10526 = 0.04214 0.01164 -0.00457 -0.02844 AFIX 23 H23A 2 0.147017 0.180113 1.030066 11.00000 -1.20000 H23B 2 0.202888 0.178642 1.092563 11.00000 -1.20000 AFIX 0 C24 1 0.156332 0.261962 1.091528 11.00000 0.05655 0.19231 = 0.05447 -0.04926 0.02262 -0.03136 AFIX 33 H24A 2 0.127921 0.249280 1.132317 11.00000 -1.50000 H24B 2 0.134326 0.287679 1.052554 11.00000 -1.50000 H24C 2 0.190230 0.286179 1.115150 11.00000 -1.50000 AFIX 0 C25 1 0.357991 0.206517 0.930851 11.00000 0.04135 0.04928 = 0.02381 -0.00833 -0.00137 0.01106 AFIX 23 H25A 2 0.392265 0.216884 0.895945 11.00000 -1.20000 H25B 2 0.325416 0.186074 0.898496 11.00000 -1.20000 AFIX 0 C26 1 0.381247 0.160136 0.991804 11.00000 0.05265 0.04929 = 0.03248 -0.01128 -0.00877 0.01620 AFIX 23 H26A 2 0.412866 0.180322 1.025920 11.00000 -1.20000 H26B 2 0.346797 0.146990 1.024963 11.00000 -1.20000 AFIX 0 C27 1 0.408700 0.103313 0.952720 11.00000 0.05202 0.07312 = 0.04681 -0.01819 -0.01323 0.03010 AFIX 23 H27A 2 0.377596 0.084302 0.916796 11.00000 -1.20000 H27B 2 0.444234 0.116317 0.921347 11.00000 -1.20000 AFIX 0 C28 1 0.429472 0.055686 1.012587 11.00000 0.08112 0.05831 = 0.07292 -0.02229 -0.03557 0.02985 AFIX 33 H28A 2 0.447877 0.019909 0.986032 11.00000 -1.50000 H28B 2 0.394013 0.041583 1.042291 11.00000 -1.50000 H28C 2 0.460043 0.074572 1.048397 11.00000 -1.50000 AFIX 0 C29 1 0.381534 0.301805 1.010026 11.00000 0.04394 0.06540 = 0.02207 -0.00664 -0.00314 -0.02979 AFIX 23 H29A 2 0.361623 0.336841 1.037562 11.00000 -1.20000 H29B 2 0.399026 0.273311 1.050395 11.00000 -1.20000 AFIX 0 C30 1 0.433903 0.327837 0.962829 11.00000 0.07081 0.12522 = 0.05177 -0.00415 -0.00187 -0.04571 AFIX 23 H30A 2 0.417746 0.355964 0.921201 11.00000 -1.20000 H30B 2 0.456925 0.293476 0.938045 11.00000 -1.20000 AFIX 0 C31 1 0.479515 0.367014 1.024756 11.00000 0.06387 0.07405 = 0.17147 0.01986 0.04086 -0.01512 AFIX 23 H31A 2 0.500986 0.401962 0.999003 11.00000 -1.20000 H31B 2 0.457130 0.382753 1.070557 11.00000 -1.20000 AFIX 0 C32 1 0.519038 0.318368 1.044254 11.00000 0.08946 0.07374 = 0.19687 0.05769 0.03299 0.01253 AFIX 33 H32A 2 0.551193 0.333505 1.080670 11.00000 -1.50000 H32B 2 0.538022 0.302402 0.996780 11.00000 -1.50000 H32C 2 0.495859 0.284783 1.069104 11.00000 -1.50000 AFIX 0 C33 1 0.817422 0.195004 0.896409 11.00000 0.04023 0.04241 = 0.02878 0.00303 -0.00933 -0.00629 AFIX 23 H33A 2 0.794329 0.225031 0.862862 11.00000 -1.20000 H33B 2 0.851146 0.177798 0.864928 11.00000 -1.20000 AFIX 0 C34 1 0.774977 0.142504 0.916491 11.00000 0.06036 0.05386 = 0.04378 0.00964 -0.01732 -0.02331 AFIX 23 H34A 2 0.740159 0.159035 0.946594 11.00000 -1.20000 H34B 2 0.797355 0.111781 0.949808 11.00000 -1.20000 AFIX 0 C35 1 0.750128 0.109981 0.842327 11.00000 0.06623 0.04849 = 0.05967 0.00014 -0.01975 -0.01593 AFIX 23 H35A 2 0.716659 0.081125 0.856845 11.00000 -1.20000 H35B 2 0.732200 0.141894 0.806592 11.00000 -1.20000 AFIX 0 C36 1 0.797378 0.074370 0.800181 11.00000 0.10592 0.06700 = 0.08025 -0.01145 -0.01782 -0.01315 AFIX 33 H36A 2 0.778815 0.055886 0.752774 11.00000 -1.50000 H36B 2 0.813794 0.041116 0.834116 11.00000 -1.50000 H36C 2 0.830832 0.102513 0.785729 11.00000 -1.50000 AFIX 0 C37 1 0.884590 0.187348 1.017502 11.00000 0.04348 0.03922 = 0.03047 0.01195 -0.01326 -0.00206 AFIX 23 H37A 2 0.902929 0.212358 1.060840 11.00000 -1.20000 H37B 2 0.856707 0.156330 1.041000 11.00000 -1.20000 AFIX 0 C38 1 0.935478 0.152649 0.978277 11.00000 0.05122 0.04123 = 0.05212 0.01259 -0.00523 0.00713 AFIX 23 H38A 2 0.962880 0.182374 0.951561 11.00000 -1.20000 H38B 2 0.918124 0.123312 0.938783 11.00000 -1.20000 AFIX 0 C39 1 0.971535 0.116799 1.041463 11.00000 0.06578 0.07308 = 0.08220 0.02232 0.00849 0.03594 AFIX 23 H39A 2 0.986367 0.147018 1.081505 11.00000 -1.20000 H39B 2 0.942952 0.087751 1.067324 11.00000 -1.20000 AFIX 0 C40 1 1.021967 0.082487 1.015873 11.00000 0.15397 0.12769 = 0.12438 0.04083 0.02221 0.01011 AFIX 33 H40A 2 1.041231 0.060505 1.060385 11.00000 -1.50000 H40B 2 1.051950 0.110876 0.992833 11.00000 -1.50000 H40C 2 1.008083 0.052020 0.976458 11.00000 -1.50000 AFIX 0 C41 1 0.797666 0.257825 1.018659 11.00000 0.02785 0.04696 = 0.02455 0.00242 -0.00204 -0.00797 AFIX 23 H41A 2 0.774599 0.222723 1.041737 11.00000 -1.20000 H41B 2 0.819037 0.280098 1.062183 11.00000 -1.20000 AFIX 0 C42 1 0.752016 0.302065 0.980641 11.00000 0.03548 0.07120 = 0.03854 0.00680 -0.00498 0.00624 AFIX 23 H42A 2 0.731582 0.281398 0.935190 11.00000 -1.20000 H42B 2 0.773772 0.339525 0.961511 11.00000 -1.20000 AFIX 0 C43 1 0.703861 0.321534 1.039374 11.00000 0.04608 0.05980 = 0.04324 0.00141 -0.00108 0.00477 AFIX 23 H43A 2 0.671573 0.346295 1.011786 11.00000 -1.20000 H43B 2 0.684138 0.283521 1.060283 11.00000 -1.20000 AFIX 0 C44 1 0.729880 0.359893 1.107623 11.00000 0.05300 0.05133 = 0.05667 0.00249 -0.00428 0.00619 AFIX 33 H44A 2 0.696795 0.369998 1.143530 11.00000 -1.50000 H44B 2 0.747780 0.398636 1.087723 11.00000 -1.50000 H44C 2 0.761793 0.335709 1.135496 11.00000 -1.50000 AFIX 0 C45 1 0.884721 0.281956 0.929720 11.00000 0.03142 0.03229 = 0.02612 0.00591 -0.00196 -0.00126 AFIX 23 H45A 2 0.912281 0.262528 0.891322 11.00000 -1.20000 H45B 2 0.856872 0.310691 0.900480 11.00000 -1.20000 AFIX 0 C46 1 0.923659 0.320223 0.986200 11.00000 0.03720 0.03910 = 0.03294 0.00132 -0.00427 -0.00312 AFIX 23 H46A 2 0.956314 0.293565 1.009927 11.00000 -1.20000 H46B 2 0.897727 0.336047 1.028766 11.00000 -1.20000 AFIX 0 C47 1 0.952657 0.374623 0.944300 11.00000 0.03179 0.02699 = 0.04600 0.00205 0.00728 0.00131 AFIX 23 H47A 2 0.920063 0.404422 0.927637 11.00000 -1.20000 H47B 2 0.972878 0.359146 0.896725 11.00000 -1.20000 AFIX 0 C48 1 0.999703 0.408312 0.995699 11.00000 0.05502 0.03804 = 0.06531 -0.00456 0.00416 -0.01042 AFIX 33 H48A 2 1.017507 0.443001 0.966396 11.00000 -1.50000 H48B 2 1.032384 0.379119 1.011695 11.00000 -1.50000 H48C 2 0.979650 0.424611 1.042257 11.00000 -1.50000 AFIX 0 C49 1 0.955080 0.549423 0.753172 11.00000 0.02696 0.05920 = 0.04274 0.00348 0.00020 -0.00832 AFIX 23 H49A 2 0.978429 0.572054 0.712963 11.00000 -1.20000 H49B 2 0.964093 0.569926 0.804090 11.00000 -1.20000 AFIX 0 C50 1 0.978703 0.483213 0.757427 11.00000 0.03530 0.07143 = 0.05856 0.01050 -0.00182 0.01138 AFIX 23 H50A 2 0.971533 0.461229 0.707063 11.00000 -1.20000 H50B 2 0.958461 0.459609 0.799502 11.00000 -1.20000 AFIX 0 C51 1 1.050969 0.491160 0.776207 11.00000 0.11773 0.11931 = 0.15763 -0.00455 -0.01984 0.07517 AFIX 23 H51A 2 1.069086 0.520852 0.738745 11.00000 -1.20000 H51B 2 1.057427 0.507971 0.829742 11.00000 -1.20000 AFIX 0 C52 1 1.082182 0.427278 0.769430 11.00000 0.25606 0.26578 = 0.25966 0.01223 0.00416 -0.00427 AFIX 33 H52A 2 1.126242 0.431508 0.781823 11.00000 -1.50000 H52B 2 1.076578 0.411448 0.715925 11.00000 -1.50000 H52C 2 1.063695 0.398003 0.806207 11.00000 -1.50000 AFIX 0 C53 1 0.871209 0.626691 0.736380 11.00000 0.03636 0.03041 = 0.03719 -0.00348 0.00312 -0.00554 AFIX 23 H53A 2 0.825882 0.631296 0.733429 11.00000 -1.20000 H53B 2 0.885505 0.643709 0.787513 11.00000 -1.20000 AFIX 0 C54 1 0.898696 0.665955 0.671973 11.00000 0.04385 0.03872 = 0.03056 -0.00134 -0.00135 -0.01369 AFIX 23 H54A 2 0.943587 0.658346 0.670347 11.00000 -1.20000 H54B 2 0.880252 0.653524 0.620794 11.00000 -1.20000 AFIX 0 C55 1 0.886972 0.734822 0.685873 11.00000 0.04942 0.03124 = 0.03364 0.00456 -0.00575 -0.00836 AFIX 23 H55A 2 0.902953 0.746512 0.738584 11.00000 -1.20000 H55B 2 0.842081 0.742780 0.684112 11.00000 -1.20000 AFIX 0 C56 1 0.917797 0.774924 0.624765 11.00000 0.04851 0.05620 = 0.04635 0.01089 -0.00593 -0.01731 AFIX 33 H56A 2 0.909092 0.819085 0.634900 11.00000 -1.50000 H56B 2 0.901815 0.763607 0.572573 11.00000 -1.50000 H56C 2 0.962370 0.767949 0.627399 11.00000 -1.50000 AFIX 0 C57 1 0.847210 0.523854 0.793383 11.00000 0.02986 0.03160 = 0.05694 0.00129 0.00491 -0.00706 AFIX 23 H57A 2 0.850900 0.478238 0.785058 11.00000 -1.20000 H57B 2 0.803699 0.535377 0.782705 11.00000 -1.20000 AFIX 0 C58 1 0.862479 0.537778 0.879113 11.00000 0.03579 0.03517 = 0.04454 0.00033 0.00805 -0.00459 AFIX 23 H58A 2 0.904390 0.522381 0.892415 11.00000 -1.20000 H58B 2 0.861834 0.583506 0.887834 11.00000 -1.20000 AFIX 0 C59 1 0.816471 0.506640 0.931556 11.00000 0.04151 0.04408 = 0.06170 0.01555 0.01449 0.00546 AFIX 23 H59A 2 0.775744 0.526558 0.923052 11.00000 -1.20000 H59B 2 0.812540 0.462122 0.916496 11.00000 -1.20000 AFIX 0 C60 1 0.833876 0.510501 1.016561 11.00000 0.06905 0.05288 = 0.05454 0.00621 0.02449 0.00298 AFIX 33 H60A 2 0.802158 0.490124 1.047444 11.00000 -1.50000 H60B 2 0.837451 0.554453 1.032117 11.00000 -1.50000 H60C 2 0.873428 0.489457 1.025850 11.00000 -1.50000 AFIX 0 C61 1 0.873235 0.529181 0.654574 11.00000 0.03915 0.03568 = 0.03887 -0.00825 0.00418 -0.00331 AFIX 23 H61A 2 0.903155 0.546695 0.617653 11.00000 -1.20000 H61B 2 0.880844 0.483630 0.657754 11.00000 -1.20000 AFIX 0 C62 1 0.809627 0.538943 0.620122 11.00000 0.03848 0.03840 = 0.05738 -0.00663 -0.01095 -0.00235 AFIX 23 H62A 2 0.799945 0.584146 0.619266 11.00000 -1.20000 H62B 2 0.779127 0.517779 0.653149 11.00000 -1.20000 AFIX 0 C63 1 0.805265 0.513215 0.538103 11.00000 0.06802 0.06625 = 0.08461 -0.03646 -0.03568 0.02309 AFIX 23 H63A 2 0.839541 0.530597 0.507737 11.00000 -1.20000 H63B 2 0.810863 0.467339 0.540535 11.00000 -1.20000 AFIX 0 C64 1 0.747413 0.526585 0.496126 11.00000 0.09385 0.07829 = 0.12225 -0.03383 -0.04422 0.01230 AFIX 33 H64A 2 0.748013 0.507298 0.444133 11.00000 -1.50000 H64B 2 0.742402 0.571894 0.490614 11.00000 -1.50000 H64C 2 0.713026 0.509529 0.525478 11.00000 -1.50000 AFIX 0 N1 3 0.406822 -0.076100 0.736094 11.00000 0.02400 0.02677 = 0.03141 -0.00328 -0.00195 0.00134 N2 3 0.332462 0.266685 0.963205 11.00000 0.03226 0.03919 = 0.02138 -0.00577 0.00016 -0.00632 N3 3 0.846043 0.230856 0.965345 11.00000 0.03548 0.03397 = 0.02511 0.00573 -0.00854 -0.00156 N4 3 0.886768 0.556875 0.734156 11.00000 0.03101 0.03480 = 0.03622 -0.00040 -0.00009 -0.00663 O1 4 0.465622 0.310039 0.655509 11.00000 0.03928 0.05843 = 0.02686 0.00437 0.00092 -0.01239 O2 4 0.423242 0.351864 0.774036 11.00000 0.05072 0.06363 = 0.03648 -0.01393 0.00755 -0.02435 O3 4 0.359097 0.290944 0.684922 11.00000 0.03419 0.04210 = 0.03385 0.00401 -0.00913 -0.00757 O4 4 0.439587 0.242416 0.763594 11.00000 0.03838 0.06131 = 0.04341 0.01583 -0.01494 -0.00981 O5 4 0.777526 0.370054 0.651213 11.00000 0.07881 0.05873 = 0.04142 0.01080 -0.00964 0.02675 O6 4 0.873265 0.361061 0.723150 11.00000 0.03015 0.03750 = 0.09873 -0.00820 0.00836 -0.00094 O7 4 0.778402 0.379046 0.790430 11.00000 0.05495 0.04945 = 0.04718 -0.01529 0.01428 -0.00440 O8 4 0.796965 0.279788 0.731994 11.00000 0.03509 0.03332 = 0.05733 0.00687 0.00022 -0.00193 O9 4 0.382242 0.143542 0.703751 11.00000 0.03122 0.03659 = 0.08162 0.01095 0.01344 0.00674 O10 4 0.290682 0.199800 0.738233 11.00000 0.02964 0.03446 = 0.04171 -0.00548 0.00532 -0.00508 O11 4 0.286027 0.118232 0.640200 11.00000 0.08190 0.03765 = 0.03400 -0.00626 -0.01157 -0.00113 O12 4 0.301834 0.093806 0.775912 11.00000 0.05890 0.04621 = 0.04325 0.01600 0.00232 -0.00780 O13 4 0.885630 0.211148 0.678878 11.00000 0.04065 0.05179 = 0.03841 -0.00728 -0.01560 0.00937 O14 4 0.994871 0.188909 0.666951 11.00000 0.04735 0.09510 = 0.03713 -0.00348 0.00067 0.02611 O15 4 0.962122 0.280663 0.734590 11.00000 0.05044 0.04545 = 0.12377 -0.00824 -0.03851 0.00815 O16 4 0.946728 0.180013 0.791556 11.00000 0.04834 0.07843 = 0.03351 0.00850 -0.00430 0.01892 S1 5 0.421534 0.303107 0.716027 11.00000 0.03304 0.04426 = 0.02107 0.00071 -0.00273 -0.01339 S2 5 0.806483 0.351380 0.723667 11.00000 0.03329 0.02907 = 0.03323 -0.00060 0.00171 0.00281 S3 5 0.316697 0.134641 0.713183 11.00000 0.03559 0.02620 = 0.02878 0.00283 0.00188 -0.00098 S4 5 0.947483 0.211006 0.717576 11.00000 0.03881 0.04211 = 0.03391 -0.00300 -0.00657 0.01437 H10 2 0.312497 0.224655 0.718630 11.00000 0.02661 H4 2 0.424490 0.210095 0.741473 11.00000 0.09006 H8 2 0.829394 0.260240 0.708970 11.00000 0.13206 H15 2 0.931921 0.302466 0.732774 11.00000 0.16712 HKLF 4 1.0 0.00 0.00 1.00 0.00 -1.00 0.00 1.00 0.00 0.00 Covalent radii and connectivity table for 01mel003 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 C1 - N1 C2 C2 - C3 C1 C3 - C2 C4 C4 - C3 C5 - N1 C6 C6 - C5 C7 C7 - C8 C6 C8 - C7 C9 - N1 C10 C10 - C12 C9 C11 - C12 C12 - C11 C10 C13 - N1 C14 C14 - C15 C13 C15 - C14 C16 C16 - C15 C17 - C18 N2 C18 - C17 C19 C19 - C20 C18 C20 - C19 C21 - C22 N2 C22 - C21 C23 C23 - C24 C22 C24 - C23 C25 - N2 C26 C26 - C27 C25 C27 - C28 C26 C28 - C27 C29 - C30 N2 C30 - C29 C31 C31 - C32 C30 C32 - C31 C33 - C34 N3 C34 - C33 C35 C35 - C36 C34 C36 - C35 C37 - C38 N3 C38 - C37 C39 C39 - C40 C38 C40 - C39 C41 - C42 N3 C42 - C41 C43 C43 - C44 C42 C44 - C43 C45 - C46 N3 C46 - C45 C47 C47 - C46 C48 C48 - C47 C49 - C50 N4 C50 - C49 C51 C51 - C52 C50 C52 - C51 C53 - C54 N4 C54 - C55 C53 C55 - C54 C56 C56 - C55 C57 - N4 C58 C58 - C59 C57 C59 - C60 C58 C60 - C59 C61 - C62 N4 C62 - C61 C63 C63 - C64 C62 C64 - C63 N1 - C9 C5 C1 C13 N2 - C25 C21 C29 C17 N3 - C45 C41 C37 C33 N4 - C61 C57 C49 C53 O1 - S1 O2 - S1 O3 - S1 O4 - S1 O5 - S2 O6 - S2 O7 - S2 O8 - S2 O9 - S3 O10 - S3 O11 - S3 O12 - S3 O13 - S4 O14 - S4 O15 - S4 O16 - S4 S1 - O1 O2 O3 O4 S2 - O5 O7 O6 O8 S3 - O12 O11 O9 O10 S4 - O16 O14 O13 O15 h k l Fo^2 Sigma Why rejected -1 0 3 2.45 0.56 observed but should be systematically absent 1 0 3 5.79 0.80 observed but should be systematically absent 45381 Reflections read, of which 6663 rejected -25 =< h =< 25, -25 =< k =< 24, -20 =< l =< 20, Max. 2-theta = 50.05 2 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -3 1 1 456.87 6.29 8 37.90 2 2 1 12.07 0.27 6 1.91 -2 0 2 1020.03 18.40 4 142.25 2 0 2 79.72 2.09 2 34.35 0 2 2 4.51 0.16 5 0.84 -3 4 2 413.57 5.58 6 33.83 -4 5 2 106.46 1.20 6 9.63 1 2 3 1136.23 19.22 5 97.97 -6 8 3 0.91 0.11 4 0.79 -6 9 3 50.70 0.12 4 24.38 -5 9 3 163.09 0.76 4 41.40 1 3 4 116.10 1.69 6 9.56 1 4 4 126.82 2.17 5 13.51 0 5 4 226.26 3.20 6 20.43 -6 6 4 46.88 0.34 4 16.78 -7 7 4 7.97 0.21 4 1.93 1 4 5 148.11 0.21 5 91.29 1 5 5 54.44 0.21 5 14.75 0 6 5 26.30 0.21 5 4.77 0 4 6 3.30 0.46 3 2.47 2 6 8 7.55 0.22 4 4.68 3 8 9 4.37 0.41 3 3.07 3 9 9 5.48 0.19 4 1.69 3 7 10 15.08 0.60 4 5.31 24 Inconsistent equivalents 13981 Unique reflections, of which 0 suppressed R(int) = 0.0680 R(sigma) = 0.0968 Friedel opposites merged Maximum memory for data reduction = 9246 / 138599 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 = 11997 / 1181912 wR2 = 0.2369 before cycle 1 for 13981 data and 810 / 810 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint 1.5316 1.5400 -0.0084 0.0020 DFIX C52 C51 -0.0426 0.0050 ISOR U22 C30 0.0309 0.0050 ISOR U33 C30 0.0457 0.0050 ISOR U12 C30 0.0342 0.0050 ISOR U11 C12 0.0352 0.0050 ISOR U22 C12 -0.0697 0.0050 ISOR U33 C12 0.0290 0.0050 ISOR U23 C12 0.0170 0.0050 ISOR U12 C12 Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 18. 0. rms sigma 0.000 0.002 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.005 0.000 rms deviation 0.000 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.028 0.000 GooF = S = 1.021; Restrained GooF = 1.041 for 19 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1368 * P )^2 + 1.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.14636 0.00037 -0.020 OSF 2 0.00000 0.00032 -1.143 EXTI Mean shift/esd = 0.028 Maximum = -1.143 for EXTI Max. shift = 0.013 A for H8 Max. dU = 0.003 for H8 Least-squares cycle 2 Maximum vector length = 511 Memory required = 11997 / 1181912 wR2 = 0.2369 before cycle 2 for 13981 data and 810 / 810 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint 1.5315 1.5400 -0.0085 0.0020 DFIX C52 C51 -0.0427 0.0050 ISOR U22 C30 0.0310 0.0050 ISOR U33 C30 0.0457 0.0050 ISOR U12 C30 0.0342 0.0050 ISOR U11 C12 0.0353 0.0050 ISOR U22 C12 -0.0697 0.0050 ISOR U33 C12 0.0290 0.0050 ISOR U23 C12 0.0170 0.0050 ISOR U12 C12 Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 18. 0. rms sigma 0.000 0.002 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.005 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.028 0.000 GooF = S = 1.021; Restrained GooF = 1.041 for 19 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1368 * P )^2 + 1.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.14635 0.00037 -0.038 OSF 2 0.00000 0.00032 -1.519 EXTI Mean shift/esd = 0.018 Maximum = -1.519 for EXTI Max. shift = 0.008 A for H8 Max. dU = 0.003 for H8 Least-squares cycle 3 Maximum vector length = 511 Memory required = 11997 / 1181912 wR2 = 0.2369 before cycle 3 for 13981 data and 810 / 810 parameters Disagreeable restraints before cycle 3 Observed Target Error Sigma Restraint 1.5314 1.5400 -0.0086 0.0020 DFIX C52 C51 -0.0427 0.0050 ISOR U22 C30 0.0311 0.0050 ISOR U33 C30 0.0456 0.0050 ISOR U12 C30 0.0341 0.0050 ISOR U11 C12 0.0354 0.0050 ISOR U22 C12 -0.0698 0.0050 ISOR U33 C12 0.0290 0.0050 ISOR U23 C12 0.0170 0.0050 ISOR U12 C12 Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 18. 0. rms sigma 0.000 0.002 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.005 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.028 0.000 GooF = S = 1.021; Restrained GooF = 1.041 for 19 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1368 * P )^2 + 1.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.14635 0.00037 0.003 OSF 2 0.00000 0.00032 -1.517 EXTI Mean shift/esd = 0.007 Maximum = -1.517 for EXTI Max. shift = 0.003 A for H8 Max. dU = 0.002 for H8 Least-squares cycle 4 Maximum vector length = 511 Memory required = 11997 / 1181912 wR2 = 0.2369 before cycle 4 for 13981 data and 810 / 810 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint 1.5313 1.5400 -0.0087 0.0020 DFIX C52 C51 -0.0427 0.0050 ISOR U22 C30 0.0311 0.0050 ISOR U33 C30 0.0456 0.0050 ISOR U12 C30 0.0341 0.0050 ISOR U11 C12 0.0354 0.0050 ISOR U22 C12 -0.0698 0.0050 ISOR U33 C12 0.0290 0.0050 ISOR U23 C12 0.0170 0.0050 ISOR U12 C12 Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 18. 0. rms sigma 0.000 0.002 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.005 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.028 0.000 GooF = S = 1.021; Restrained GooF = 1.041 for 19 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1368 * P )^2 + 1.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.14635 0.00037 0.000 OSF 2 0.00000 0.00032 -1.517 EXTI Mean shift/esd = 0.004 Maximum = -1.517 for EXTI Max. shift = 0.002 A for H15 Max. dU = 0.001 for H15 Largest correlation matrix elements 0.591 U22 C52 / U11 C52 0.588 U33 C52 / U22 C52 0.589 U33 C52 / U11 C52 0.534 y C52 / y C51 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.3608 0.0006 0.6916 23 0.990 0.000 C1 N1 C2 H1B 0.3283 -0.0640 0.6683 23 0.990 0.000 C1 N1 C2 H2A 0.4368 -0.0157 0.5971 23 0.990 0.000 C2 C3 C1 H2B 0.4083 -0.0829 0.5760 23 0.990 0.000 C2 C3 C1 H3A 0.3456 0.0338 0.5498 23 0.990 0.000 C3 C2 C4 H3B 0.3151 -0.0330 0.5314 23 0.990 0.000 C3 C2 C4 H4A 0.3546 0.0103 0.4148 33 0.980 0.000 C4 C3 H4A H4B 0.3913 -0.0525 0.4363 33 0.980 0.000 C4 C3 H4A H4C 0.4218 0.0140 0.4548 33 0.980 0.000 C4 C3 H4A H5A 0.4416 -0.1639 0.7569 23 0.990 0.000 C5 N1 C6 H5B 0.4471 -0.1428 0.6678 23 0.990 0.000 C5 N1 C6 H6A 0.3450 -0.1667 0.6409 23 0.990 0.000 C6 C5 C7 H6B 0.3316 -0.1766 0.7319 23 0.990 0.000 C6 C5 C7 H7A 0.3454 -0.2731 0.6568 23 0.990 0.000 C7 C8 C6 H7B 0.4164 -0.2548 0.6510 23 0.990 0.000 C7 C8 C6 H8A 0.4035 -0.3257 0.7509 33 0.980 0.000 C8 C7 H8A H8B 0.3560 -0.2798 0.7922 33 0.980 0.000 C8 C7 H8A H8C 0.4270 -0.2607 0.7869 33 0.980 0.000 C8 C7 H8A H9A 0.4922 -0.0501 0.6992 23 0.990 0.000 C9 N1 C10 H9B 0.4921 -0.0694 0.7895 23 0.990 0.000 C9 N1 C10 H10A 0.4432 0.0462 0.7316 23 0.990 0.000 C10 C12 C9 H10B 0.4474 0.0270 0.8220 23 0.990 0.000 C10 C12 C9 H11A 0.6153 0.0608 0.7913 33 0.980 0.000 C11 C12 H11A H11B 0.5940 0.0286 0.7106 33 0.980 0.000 C11 C12 H11A H11C 0.5921 -0.0102 0.7906 33 0.980 0.000 C11 C12 H11A H12A 0.5247 0.0879 0.7436 23 0.990 0.000 C12 C11 C10 H12B 0.5297 0.0672 0.8318 23 0.990 0.000 C12 C11 C10 H13A 0.3292 -0.0924 0.8004 23 0.990 0.000 C13 N1 C14 H13B 0.3641 -0.0295 0.8255 23 0.990 0.000 C13 N1 C14 H14A 0.4073 -0.1519 0.8655 23 0.990 0.000 C14 C15 C13 H14B 0.4412 -0.0888 0.8914 23 0.990 0.000 C14 C15 C13 H15A 0.3241 -0.1253 0.9412 23 0.990 0.000 C15 C14 C16 H15B 0.3585 -0.0625 0.9676 23 0.990 0.000 C15 C14 C16 H16A 0.3690 -0.1375 1.0655 33 0.980 0.000 C16 C15 H16A H16B 0.4353 -0.1219 1.0317 33 0.980 0.000 C16 C15 H16A H16C 0.4004 -0.1847 1.0057 33 0.980 0.000 C16 C15 H16A H17A 0.3455 0.3130 0.8591 23 0.990 0.000 C17 C18 N2 H17B 0.2813 0.2768 0.8609 23 0.990 0.000 C17 C18 N2 H18A 0.3011 0.3879 0.9496 23 0.990 0.000 C18 C17 C19 H18B 0.2360 0.3553 0.9304 23 0.990 0.000 C18 C17 C19 H19A 0.2521 0.4444 0.8474 23 0.990 0.000 C19 C20 C18 H19B 0.3120 0.4117 0.8136 23 0.990 0.000 C19 C20 C18 H20A 0.2299 0.4005 0.7245 33 0.980 0.000 C20 C19 H20A H20B 0.1899 0.3666 0.7895 33 0.980 0.000 C20 C19 H20A H20C 0.2497 0.3330 0.7565 33 0.980 0.000 C20 C19 H20A H21A 0.2990 0.2312 1.0655 23 0.990 0.000 C21 C22 N2 H21B 0.2672 0.2956 1.0404 23 0.990 0.000 C21 C22 N2 H22A 0.2403 0.1800 0.9638 23 0.990 0.000 C22 C21 C23 H22B 0.2054 0.2447 0.9470 23 0.990 0.000 C22 C21 C23 H23A 0.1470 0.1801 1.0301 23 0.990 0.000 C23 C24 C22 H23B 0.2029 0.1787 1.0926 23 0.990 0.000 C23 C24 C22 H24A 0.1279 0.2493 1.1323 33 0.980 0.000 C24 C23 H24A H24B 0.1343 0.2877 1.0525 33 0.980 0.000 C24 C23 H24A H24C 0.1902 0.2862 1.1151 33 0.980 0.000 C24 C23 H24A H25A 0.3923 0.2169 0.8959 23 0.990 0.000 C25 N2 C26 H25B 0.3254 0.1861 0.8985 23 0.990 0.000 C25 N2 C26 H26A 0.4129 0.1803 1.0259 23 0.990 0.000 C26 C27 C25 H26B 0.3468 0.1470 1.0250 23 0.990 0.000 C26 C27 C25 H27A 0.3776 0.0843 0.9168 23 0.990 0.000 C27 C28 C26 H27B 0.4442 0.1163 0.9214 23 0.990 0.000 C27 C28 C26 H28A 0.4479 0.0199 0.9860 33 0.980 0.000 C28 C27 H28A H28B 0.3940 0.0416 1.0423 33 0.980 0.000 C28 C27 H28A H28C 0.4601 0.0746 1.0484 33 0.980 0.000 C28 C27 H28A H29A 0.3616 0.3369 1.0374 23 0.990 0.000 C29 C30 N2 H29B 0.3990 0.2733 1.0503 23 0.990 0.000 C29 C30 N2 H30A 0.4177 0.3560 0.9213 23 0.990 0.000 C30 C29 C31 H30B 0.4569 0.2935 0.9381 23 0.990 0.000 C30 C29 C31 H31A 0.5010 0.4019 0.9988 23 0.990 0.000 C31 C32 C30 H31B 0.4572 0.3828 1.0704 23 0.990 0.000 C31 C32 C30 H32A 0.5512 0.3335 1.0806 33 0.980 0.000 C32 C31 H32A H32B 0.5381 0.3024 0.9967 33 0.980 0.000 C32 C31 H32A H32C 0.4959 0.2848 1.0691 33 0.980 0.000 C32 C31 H32A H33A 0.7943 0.2250 0.8629 23 0.990 0.000 C33 C34 N3 H33B 0.8512 0.1778 0.8650 23 0.990 0.000 C33 C34 N3 H34A 0.7402 0.1590 0.9466 23 0.990 0.000 C34 C33 C35 H34B 0.7974 0.1118 0.9498 23 0.990 0.000 C34 C33 C35 H35A 0.7167 0.0811 0.8569 23 0.990 0.000 C35 C36 C34 H35B 0.7322 0.1419 0.8066 23 0.990 0.000 C35 C36 C34 H36A 0.7788 0.0559 0.7528 33 0.980 0.000 C36 C35 H36A H36B 0.8138 0.0411 0.8341 33 0.980 0.000 C36 C35 H36A H36C 0.8309 0.1025 0.7857 33 0.980 0.000 C36 C35 H36A H37A 0.9029 0.2124 1.0609 23 0.990 0.000 C37 C38 N3 H37B 0.8567 0.1563 1.0410 23 0.990 0.000 C37 C38 N3 H38A 0.9629 0.1824 0.9516 23 0.990 0.000 C38 C37 C39 H38B 0.9181 0.1233 0.9388 23 0.990 0.000 C38 C37 C39 H39A 0.9864 0.1471 1.0816 23 0.990 0.000 C39 C40 C38 H39B 0.9430 0.0878 1.0674 23 0.990 0.000 C39 C40 C38 H40A 1.0413 0.0606 1.0605 33 0.980 0.000 C40 C39 H40A H40B 1.0520 0.1109 0.9929 33 0.980 0.000 C40 C39 H40A H40C 1.0081 0.0521 0.9765 33 0.980 0.000 C40 C39 H40A H41A 0.7746 0.2227 1.0417 23 0.990 0.000 C41 C42 N3 H41B 0.8190 0.2801 1.0622 23 0.990 0.000 C41 C42 N3 H42A 0.7316 0.2814 0.9351 23 0.990 0.000 C42 C41 C43 H42B 0.7738 0.3395 0.9615 23 0.990 0.000 C42 C41 C43 H43A 0.6716 0.3463 1.0118 23 0.990 0.000 C43 C44 C42 H43B 0.6841 0.2835 1.0602 23 0.990 0.000 C43 C44 C42 H44A 0.6968 0.3700 1.1436 33 0.980 0.000 C44 C43 H44A H44B 0.7478 0.3986 1.0878 33 0.980 0.000 C44 C43 H44A H44C 0.7618 0.3357 1.1356 33 0.980 0.000 C44 C43 H44A H45A 0.9123 0.2625 0.8913 23 0.990 0.000 C45 C46 N3 H45B 0.8569 0.3107 0.9005 23 0.990 0.000 C45 C46 N3 H46A 0.9563 0.2936 1.0099 23 0.990 0.000 C46 C45 C47 H46B 0.8977 0.3360 1.0288 23 0.990 0.000 C46 C45 C47 H47A 0.9200 0.4044 0.9276 23 0.990 0.000 C47 C46 C48 H47B 0.9729 0.3592 0.8967 23 0.990 0.000 C47 C46 C48 H48A 1.0175 0.4430 0.9664 33 0.980 0.000 C48 C47 H48A H48B 1.0324 0.3791 1.0117 33 0.980 0.000 C48 C47 H48A H48C 0.9796 0.4246 1.0422 33 0.980 0.000 C48 C47 H48A H49A 0.9784 0.5720 0.7130 23 0.990 0.000 C49 C50 N4 H49B 0.9641 0.5699 0.8041 23 0.990 0.000 C49 C50 N4 H50A 0.9716 0.4612 0.7071 23 0.990 0.000 C50 C49 C51 H50B 0.9585 0.4596 0.7995 23 0.990 0.000 C50 C49 C51 H51A 1.0689 0.5207 0.7384 23 0.990 0.001 C51 C52 C50 H51B 1.0572 0.5085 0.8295 23 0.990 0.001 C51 C52 C50 H52A 1.1264 0.4320 0.7828 33 0.980 0.001 C52 C51 H52A H52B 1.0770 0.4112 0.7170 33 0.980 0.001 C52 C51 H52A H52C 1.0640 0.3984 0.8074 33 0.980 0.000 C52 C51 H52A H53A 0.8259 0.6313 0.7334 23 0.990 0.000 C53 C54 N4 H53B 0.8855 0.6437 0.7875 23 0.990 0.000 C53 C54 N4 H54A 0.9436 0.6583 0.6704 23 0.990 0.000 C54 C55 C53 H54B 0.8803 0.6535 0.6208 23 0.990 0.000 C54 C55 C53 H55A 0.9029 0.7465 0.7386 23 0.990 0.000 C55 C54 C56 H55B 0.8421 0.7428 0.6841 23 0.990 0.000 C55 C54 C56 H56A 0.9091 0.8191 0.6349 33 0.980 0.000 C56 C55 H56A H56B 0.9018 0.7636 0.5726 33 0.980 0.000 C56 C55 H56A H56C 0.9624 0.7679 0.6274 33 0.980 0.000 C56 C55 H56A H57A 0.8509 0.4782 0.7850 23 0.990 0.000 C57 N4 C58 H57B 0.8037 0.5354 0.7827 23 0.990 0.000 C57 N4 C58 H58A 0.9044 0.5224 0.8925 23 0.990 0.000 C58 C59 C57 H58B 0.8618 0.5835 0.8879 23 0.990 0.000 C58 C59 C57 H59A 0.7757 0.5266 0.9230 23 0.990 0.000 C59 C60 C58 H59B 0.8126 0.4621 0.9164 23 0.990 0.000 C59 C60 C58 H60A 0.8021 0.4901 1.0474 33 0.980 0.000 C60 C59 H60A H60B 0.8374 0.5544 1.0321 33 0.980 0.000 C60 C59 H60A H60C 0.8734 0.4894 1.0258 33 0.980 0.000 C60 C59 H60A H61A 0.9032 0.5467 0.6176 23 0.990 0.000 C61 C62 N4 H61B 0.8809 0.4836 0.6577 23 0.990 0.000 C61 C62 N4 H62A 0.7999 0.5841 0.6193 23 0.990 0.000 C62 C61 C63 H62B 0.7791 0.5177 0.6531 23 0.990 0.000 C62 C61 C63 H63A 0.8396 0.5306 0.5078 23 0.990 0.000 C63 C64 C62 H63B 0.8108 0.4674 0.5405 23 0.990 0.000 C63 C64 C62 H64A 0.7481 0.5073 0.4440 33 0.980 0.000 C64 C63 H64A H64B 0.7425 0.5719 0.4905 33 0.980 0.000 C64 C63 H64A H64C 0.7130 0.5096 0.5253 33 0.980 0.000 C64 C63 H64A 01mel003 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.36858 -0.04267 0.67378 1.00000 0.02809 0.02950 0.04159 -0.00001 -0.00733 0.00762 0.03318 0.00699 0.00018 0.00019 0.00022 0.00000 0.00235 0.00227 0.00241 0.00195 0.00194 0.00182 0.00099 H1A 0.36079 0.00057 0.69162 1.00000 0.03982 0.00000 0.00000 H1B 0.32826 -0.06396 0.66826 1.00000 0.03982 0.00000 0.00000 C2 0.39809 -0.04001 0.59334 1.00000 0.04157 0.03868 0.03832 0.00372 -0.00546 0.00754 0.03962 0.00754 0.00020 0.00020 0.00023 0.00000 0.00271 0.00252 0.00246 0.00207 0.00207 0.00207 0.00108 H2A 0.43681 -0.01569 0.59706 1.00000 0.04755 0.00000 0.00000 H2B 0.40826 -0.08285 0.57603 1.00000 0.04755 0.00000 0.00000 C3 0.35442 -0.00968 0.53367 1.00000 0.07738 0.05165 0.03695 -0.00248 -0.00785 0.02464 0.05547 0.00892 0.00025 0.00023 0.00024 0.00000 0.00382 0.00303 0.00264 0.00231 0.00256 0.00271 0.00139 H3A 0.34556 0.03376 0.54985 1.00000 0.06656 0.00000 0.00000 H3B 0.31508 -0.03302 0.53142 1.00000 0.06656 0.00000 0.00000 C4 0.38312 -0.00946 0.45256 1.00000 0.10280 0.05451 0.04163 0.00490 -0.00762 0.02614 0.06646 0.00961 0.00028 0.00024 0.00026 0.00000 0.00465 0.00326 0.00290 0.00248 0.00294 0.00308 0.00161 H4A 0.35463 0.01026 0.41475 1.00000 0.09968 0.00000 0.00000 H4B 0.39125 -0.05253 0.43629 1.00000 0.09968 0.00000 0.00000 H4C 0.42183 0.01404 0.45478 1.00000 0.09968 0.00000 0.00000 C5 0.41942 -0.14303 0.71293 1.00000 0.03500 0.02485 0.03838 -0.00194 -0.00551 0.00233 0.03284 0.00653 0.00018 0.00017 0.00024 0.00000 0.00243 0.00216 0.00237 0.00187 0.00195 0.00185 0.00098 H5A 0.44161 -0.16387 0.75692 1.00000 0.03941 0.00000 0.00000 H5B 0.44714 -0.14276 0.66776 1.00000 0.03941 0.00000 0.00000 C6 0.36297 -0.18176 0.69127 1.00000 0.04524 0.03216 0.07735 -0.01396 -0.02350 0.00057 0.05197 0.00719 0.00021 0.00019 0.00030 0.00000 0.00295 0.00254 0.00345 0.00245 0.00259 0.00215 0.00132 H6A 0.34504 -0.16669 0.64093 1.00000 0.06236 0.00000 0.00000 H6B 0.33162 -0.17663 0.73191 1.00000 0.06236 0.00000 0.00000 C7 0.37973 -0.25096 0.68393 1.00000 0.06155 0.03268 0.05735 -0.01341 -0.00797 -0.00366 0.05067 0.00779 0.00024 0.00020 0.00027 0.00000 0.00335 0.00259 0.00302 0.00236 0.00259 0.00227 0.00127 H7A 0.34537 -0.27308 0.65682 1.00000 0.06081 0.00000 0.00000 H7B 0.41645 -0.25477 0.65102 1.00000 0.06081 0.00000 0.00000 C8 0.39265 -0.28190 0.75989 1.00000 0.08587 0.03729 0.08324 0.00844 -0.00241 -0.01138 0.06886 0.00907 0.00027 0.00022 0.00031 0.00000 0.00435 0.00288 0.00394 0.00283 0.00336 0.00279 0.00160 H8A 0.40346 -0.32574 0.75095 1.00000 0.10330 0.00000 0.00000 H8B 0.35603 -0.27976 0.79219 1.00000 0.10330 0.00000 0.00000 H8C 0.42703 -0.26072 0.78688 1.00000 0.10330 0.00000 0.00000 C9 0.46913 -0.04597 0.74821 1.00000 0.02695 0.03407 0.03174 -0.00141 0.00017 -0.00093 0.03093 0.00644 0.00017 0.00018 0.00023 0.00000 0.00228 0.00235 0.00217 0.00190 0.00181 0.00183 0.00095 H9A 0.49222 -0.05013 0.69921 1.00000 0.03711 0.00000 0.00000 H9B 0.49205 -0.06939 0.78947 1.00000 0.03711 0.00000 0.00000 C10 0.46798 0.02283 0.77120 1.00000 0.03913 0.02902 0.05307 -0.00376 0.00135 -0.00788 0.04040 0.00706 0.00020 0.00018 0.00027 0.00000 0.00268 0.00237 0.00275 0.00213 0.00220 0.00201 0.00109 H10A 0.44320 0.04618 0.73163 1.00000 0.04848 0.00000 0.00000 H10B 0.44741 0.02699 0.82203 1.00000 0.04848 0.00000 0.00000 C11 0.58638 0.03111 0.76682 1.00000 0.03803 0.07533 0.13779 -0.02414 0.00691 -0.00331 0.08364 0.01024 0.00024 0.00027 0.00040 0.00000 0.00339 0.00410 0.00563 0.00399 0.00350 0.00295 0.00193 H11A 0.61526 0.06077 0.79134 1.00000 0.12546 0.00000 0.00000 H11B 0.59404 0.02856 0.71062 1.00000 0.12546 0.00000 0.00000 H11C 0.59210 -0.01022 0.79060 1.00000 0.12546 0.00000 0.00000 C12 0.52825 0.05065 0.77769 1.00000 0.08972 0.08837 0.19368 -0.02895 0.00890 -0.01697 0.12384 0.01304 0.00034 0.00034 0.00054 0.00000 0.00409 0.00385 0.00497 0.00377 0.00387 0.00342 0.00259 H12A 0.52471 0.08794 0.74360 1.00000 0.14861 0.00000 0.00000 H12B 0.52972 0.06719 0.83181 1.00000 0.14861 0.00000 0.00000 C13 0.37032 -0.07383 0.81094 1.00000 0.03078 0.03248 0.04392 -0.00274 0.01018 -0.00199 0.03559 0.00716 0.00019 0.00019 0.00022 0.00000 0.00242 0.00235 0.00253 0.00202 0.00202 0.00189 0.00102 H13A 0.32924 -0.09241 0.80037 1.00000 0.04270 0.00000 0.00000 H13B 0.36407 -0.02954 0.82551 1.00000 0.04270 0.00000 0.00000 C14 0.40043 -0.10779 0.88040 1.00000 0.05643 0.07979 0.03573 0.00422 0.00586 0.01263 0.05724 0.00938 0.00023 0.00026 0.00025 0.00000 0.00338 0.00372 0.00268 0.00259 0.00245 0.00284 0.00139 H14A 0.40731 -0.15190 0.86549 1.00000 0.06869 0.00000 0.00000 H14B 0.44124 -0.08876 0.89145 1.00000 0.06869 0.00000 0.00000 C15 0.36505 -0.10656 0.95219 1.00000 0.07738 0.06762 0.05390 0.00642 0.01303 -0.00571 0.06612 0.01009 0.00027 0.00026 0.00028 0.00000 0.00411 0.00362 0.00327 0.00284 0.00300 0.00307 0.00153 H15A 0.32411 -0.12532 0.94122 1.00000 0.07935 0.00000 0.00000 H15B 0.35852 -0.06249 0.96758 1.00000 0.07935 0.00000 0.00000 C16 0.39507 -0.14062 1.01962 1.00000 0.08725 0.08340 0.04736 0.02172 0.00110 -0.00189 0.07268 0.01003 0.00027 0.00027 0.00028 0.00000 0.00447 0.00415 0.00314 0.00295 0.00302 0.00340 0.00168 H16A 0.36903 -0.13754 1.06553 1.00000 0.10902 0.00000 0.00000 H16B 0.43534 -0.12190 1.03168 1.00000 0.10902 0.00000 0.00000 H16C 0.40045 -0.18468 1.00570 1.00000 0.10902 0.00000 0.00000 C17 0.30977 0.30363 0.89202 1.00000 0.04229 0.03619 0.02084 0.00333 -0.00038 -0.00367 0.03312 0.00689 0.00019 0.00018 0.00021 0.00000 0.00261 0.00240 0.00202 0.00186 0.00184 0.00201 0.00099 H17A 0.34551 0.31300 0.85909 1.00000 0.03975 0.00000 0.00000 H17B 0.28133 0.27680 0.86085 1.00000 0.03975 0.00000 0.00000 C18 0.27724 0.36424 0.90949 1.00000 0.06529 0.03643 0.02791 -0.00119 0.00305 -0.00216 0.04318 0.00774 0.00023 0.00019 0.00023 0.00000 0.00329 0.00253 0.00233 0.00201 0.00224 0.00230 0.00116 H18A 0.30108 0.38794 0.94964 1.00000 0.05182 0.00000 0.00000 H18B 0.23604 0.35532 0.93038 1.00000 0.05182 0.00000 0.00000 C19 0.27052 0.40355 0.83411 1.00000 0.07261 0.04361 0.04609 0.00406 0.00249 0.00419 0.05409 0.00861 0.00025 0.00021 0.00026 0.00000 0.00373 0.00280 0.00286 0.00238 0.00264 0.00259 0.00132 H19A 0.25209 0.44440 0.84738 1.00000 0.06490 0.00000 0.00000 H19B 0.31201 0.41165 0.81363 1.00000 0.06490 0.00000 0.00000 C20 0.23161 0.37328 0.77063 1.00000 0.07962 0.06623 0.05505 0.00754 -0.02433 0.00903 0.06736 0.00877 0.00026 0.00025 0.00029 0.00000 0.00414 0.00361 0.00323 0.00276 0.00294 0.00302 0.00157 H20A 0.22993 0.40052 0.72452 1.00000 0.10104 0.00000 0.00000 H20B 0.18988 0.36665 0.78953 1.00000 0.10104 0.00000 0.00000 H20C 0.24973 0.33300 0.75654 1.00000 0.10104 0.00000 0.00000 C21 0.28150 0.25479 1.02041 1.00000 0.03466 0.03470 0.01801 0.00063 0.00186 -0.00150 0.02910 0.00643 0.00018 0.00018 0.00020 0.00000 0.00241 0.00231 0.00191 0.00176 0.00174 0.00185 0.00094 H21A 0.29896 0.23115 1.06551 1.00000 0.03493 0.00000 0.00000 H21B 0.26716 0.29556 1.04041 1.00000 0.03493 0.00000 0.00000 C22 0.22641 0.21940 0.98802 1.00000 0.03220 0.04117 0.03711 0.00271 -0.00373 -0.00449 0.03690 0.00689 0.00019 0.00020 0.00023 0.00000 0.00244 0.00252 0.00238 0.00205 0.00196 0.00199 0.00103 H22A 0.24029 0.17996 0.96381 1.00000 0.04428 0.00000 0.00000 H22B 0.20538 0.24472 0.94696 1.00000 0.04428 0.00000 0.00000 C23 0.18169 0.20481 1.05251 1.00000 0.05004 0.10541 0.04211 0.01172 -0.00461 -0.02850 0.06594 0.00898 0.00024 0.00028 0.00028 0.00000 0.00328 0.00462 0.00288 0.00310 0.00252 0.00318 0.00161 H23A 0.14703 0.18011 1.03008 1.00000 0.07913 0.00000 0.00000 H23B 0.20290 0.17865 1.09258 1.00000 0.07913 0.00000 0.00000 C24 0.15634 0.26196 1.09152 1.00000 0.05670 0.19193 0.05430 -0.04925 0.02255 -0.03144 0.10065 0.01021 0.00027 0.00036 0.00032 0.00000 0.00389 0.00764 0.00350 0.00443 0.00307 0.00445 0.00253 H24A 0.12793 0.24928 1.13231 1.00000 0.15097 0.00000 0.00000 H24B 0.13434 0.28767 1.05254 1.00000 0.15097 0.00000 0.00000 H24C 0.19024 0.28618 1.11514 1.00000 0.15097 0.00000 0.00000 C25 0.35799 0.20652 0.93086 1.00000 0.04133 0.04939 0.02395 -0.00838 -0.00142 0.01104 0.03826 0.00735 0.00020 0.00019 0.00022 0.00000 0.00266 0.00273 0.00212 0.00202 0.00192 0.00217 0.00107 H25A 0.39225 0.21688 0.89594 1.00000 0.04591 0.00000 0.00000 H25B 0.32541 0.18607 0.89852 1.00000 0.04591 0.00000 0.00000 C26 0.38126 0.16014 0.99184 1.00000 0.05266 0.04927 0.03246 -0.01118 -0.00873 0.01625 0.04494 0.00782 0.00022 0.00021 0.00024 0.00000 0.00306 0.00281 0.00235 0.00218 0.00216 0.00233 0.00119 H26A 0.41288 0.18033 1.02594 1.00000 0.05393 0.00000 0.00000 H26B 0.34682 0.14699 1.02501 1.00000 0.05393 0.00000 0.00000 C27 0.40871 0.10333 0.95275 1.00000 0.05200 0.07299 0.04684 -0.01821 -0.01317 0.03009 0.05750 0.00864 0.00023 0.00024 0.00026 0.00000 0.00321 0.00351 0.00288 0.00266 0.00244 0.00276 0.00142 H27A 0.37761 0.08432 0.91683 1.00000 0.06900 0.00000 0.00000 H27B 0.44425 0.11633 0.92138 1.00000 0.06900 0.00000 0.00000 C28 0.42949 0.05570 1.01259 1.00000 0.08115 0.05818 0.07297 -0.02238 -0.03565 0.02971 0.07134 0.00895 0.00026 0.00024 0.00030 0.00000 0.00419 0.00339 0.00361 0.00293 0.00318 0.00304 0.00171 H28A 0.44789 0.01993 0.98602 1.00000 0.10701 0.00000 0.00000 H28B 0.39403 0.04159 1.04230 1.00000 0.10701 0.00000 0.00000 H28C 0.46006 0.07458 1.04840 1.00000 0.10701 0.00000 0.00000 C29 0.38150 0.30182 1.00993 1.00000 0.04411 0.06464 0.02171 -0.00653 -0.00298 -0.02889 0.04354 0.00647 0.00020 0.00022 0.00022 0.00000 0.00279 0.00311 0.00213 0.00213 0.00196 0.00239 0.00119 H29A 0.36156 0.33685 1.03745 1.00000 0.05225 0.00000 0.00000 H29B 0.39898 0.27335 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0.73824 1.00000 0.02956 0.03451 0.04176 -0.00551 0.00532 -0.00511 0.03521 0.00495 0.00014 0.00014 0.00017 0.00000 0.00168 0.00175 0.00177 0.00147 0.00140 0.00145 0.00073 O11 0.28603 0.11822 0.64019 1.00000 0.08189 0.03767 0.03405 -0.00622 -0.01162 -0.00111 0.05140 0.00505 0.00016 0.00013 0.00016 0.00000 0.00251 0.00176 0.00170 0.00140 0.00165 0.00165 0.00087 O12 0.30184 0.09380 0.77591 1.00000 0.05891 0.04624 0.04313 0.01601 0.00227 -0.00785 0.04941 0.00530 0.00015 0.00014 0.00016 0.00000 0.00215 0.00187 0.00177 0.00151 0.00157 0.00158 0.00083 O13 0.88564 0.21114 0.67888 1.00000 0.04059 0.05184 0.03841 -0.00726 -0.01559 0.00939 0.04387 0.00475 0.00013 0.00013 0.00016 0.00000 0.00184 0.00190 0.00164 0.00146 0.00140 0.00148 0.00077 O14 0.99486 0.18891 0.66692 1.00000 0.04727 0.09514 0.03720 -0.00355 0.00065 0.02611 0.05987 0.00587 0.00015 0.00016 0.00017 0.00000 0.00207 0.00265 0.00174 0.00176 0.00154 0.00190 0.00096 O15 0.96210 0.28067 0.73461 1.00000 0.05048 0.04545 0.12343 -0.00809 -0.03844 0.00802 0.07374 0.00623 0.00018 0.00017 0.00026 0.00000 0.00241 0.00218 0.00345 0.00216 0.00232 0.00184 0.00127 O16 0.94673 0.18002 0.79156 1.00000 0.04838 0.07836 0.03361 0.00842 -0.00426 0.01897 0.05353 0.00564 0.00014 0.00016 0.00016 0.00000 0.00203 0.00238 0.00169 0.00165 0.00147 0.00174 0.00089 S1 0.42153 0.30311 0.71603 1.00000 0.03303 0.04424 0.02106 0.00071 -0.00272 -0.01340 0.03283 0.00168 0.00005 0.00005 0.00005 0.00000 0.00061 0.00066 0.00051 0.00048 0.00044 0.00050 0.00029 S2 0.80648 0.35138 0.72366 1.00000 0.03330 0.02907 0.03322 -0.00061 0.00171 0.00281 0.03185 0.00179 0.00005 0.00005 0.00006 0.00000 0.00062 0.00058 0.00060 0.00047 0.00048 0.00046 0.00029 S3 0.31670 0.13464 0.71319 1.00000 0.03559 0.02622 0.02881 0.00282 0.00188 -0.00097 0.03019 0.00174 0.00005 0.00004 0.00006 0.00000 0.00062 0.00055 0.00057 0.00045 0.00046 0.00046 0.00028 S4 0.94748 0.21101 0.71757 1.00000 0.03881 0.04211 0.03390 -0.00299 -0.00656 0.01436 0.03839 0.00193 0.00005 0.00005 0.00006 0.00000 0.00067 0.00067 0.00061 0.00051 0.00050 0.00052 0.00031 H10 0.31247 0.22455 0.71878 1.00000 0.02650 0.06762 0.00180 0.00182 0.00217 0.00000 0.01274 H4 0.42471 0.21057 0.74177 1.00000 0.08782 0.10226 0.00277 0.00264 0.00335 0.00000 0.02233 H8 0.82941 0.26036 0.70750 1.00000 0.14092 0.12075 0.00345 0.00332 0.00390 0.00000 0.02966 H15 0.93146 0.30268 0.73254 1.00000 0.17094 0.15054 0.00399 0.00390 0.00490 0.00000 0.03787 Final Structure Factor Calculation for 01mel003 in P2(1)/c Total number of l.s. parameters = 810 Maximum vector length = 511 Memory required = 11187 / 24017 wR2 = 0.2369 before cycle 5 for 13981 data and 0 / 810 parameters Disagreeable restraints before cycle 5 Observed Target Error Sigma Restraint 1.5313 1.5400 -0.0087 0.0020 DFIX C52 C51 -0.0427 0.0050 ISOR U22 C30 0.0311 0.0050 ISOR U33 C30 0.0456 0.0050 ISOR U12 C30 0.0341 0.0050 ISOR U11 C12 0.0355 0.0050 ISOR U22 C12 -0.0698 0.0050 ISOR U33 C12 0.0290 0.0050 ISOR U23 C12 0.0170 0.0050 ISOR U12 C12 Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 18. 0. rms sigma 0.000 0.002 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.005 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.028 0.000 GooF = S = 1.021; Restrained GooF = 1.041 for 19 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1368 * P )^2 + 1.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0735 for 8005 Fo > 4sig(Fo) and 0.1357 for all 13981 data wR2 = 0.2369, GooF = S = 1.021, Restrained GooF = 1.041 for all data Occupancy sum of asymmetric unit = 88.00 for non-hydrogen and 148.00 for hydrogen atoms Principal mean square atomic displacements U 0.0464 0.0337 0.0195 C1 0.0488 0.0421 0.0279 C2 0.0940 0.0386 0.0338 C3 0.1150 0.0501 0.0342 C4 0.0439 0.0303 0.0243 C5 0.0941 0.0370 0.0248 C6 0.0703 0.0562 0.0255 C7 0.0929 0.0801 0.0336 C8 0.0348 0.0313 0.0268 C9 0.0538 0.0430 0.0244 C10 0.1462 0.0672 0.0376 C11 0.2018 0.1001 0.0697 C12 0.0492 0.0319 0.0257 C13 0.0859 0.0513 0.0345 C14 0.0825 0.0701 0.0458 C15 0.0943 0.0866 0.0371 C16 0.0443 0.0349 0.0201 C17 0.0655 0.0364 0.0276 C18 0.0733 0.0486 0.0404 C19 0.0970 0.0698 0.0353 C20 0.0362 0.0333 0.0179 C21 0.0455 0.0362 0.0290 C22 0.1199 0.0401 0.0379 C23 0.2156 0.0549 0.0314 C24 may be split into 0.1542 0.2706 1.0879 and 0.1585 0.2533 1.0951 0.0592 0.0343 0.0213 C25 0.0730 0.0350 0.0268 C26 0.1043 0.0376 0.0306 C27 0.1341 0.0427 0.0372 C28 0.0851 0.0295 0.0160 C29 0.1511 0.0537 0.0427 C30 0.1824 0.0852 0.0386 C31 0.2252 0.0814 0.0511 C32 may be split into 0.5213 0.3215 1.0542 and 0.5168 0.3152 1.0342 0.0517 0.0371 0.0231 C33 0.0904 0.0385 0.0300 C34 0.0888 0.0531 0.0336 C35 0.1179 0.0846 0.0522 C36 0.0572 0.0388 0.0178 C37 0.0608 0.0550 0.0290 C38 0.1180 0.0717 0.0314 C39 0.1814 0.1399 0.0844 C40 0.0503 0.0262 0.0230 C41 0.0733 0.0432 0.0291 C42 0.0611 0.0464 0.0417 C43 0.0610 0.0564 0.0436 C44 0.0371 0.0306 0.0222 C45 0.0433 0.0365 0.0298 C46 0.0486 0.0291 0.0267 C47 0.0681 0.0574 0.0328 C48 0.0619 0.0422 0.0249 C49 0.0790 0.0556 0.0309 C50 0.2011 0.1508 0.0426 C51 0.2728 0.2543 0.2479 C52 0.0422 0.0348 0.0268 C53 0.0553 0.0318 0.0261 C54 0.0558 0.0316 0.0272 C55 0.0760 0.0409 0.0344 C56 0.0576 0.0377 0.0230 C57 0.0487 0.0378 0.0289 C58 0.0759 0.0373 0.0331 C59 0.0866 0.0525 0.0364 C60 0.0477 0.0367 0.0290 C61 0.0645 0.0406 0.0297 C62 0.1411 0.0440 0.0357 C63 0.1710 0.0723 0.0529 C64 0.0341 0.0250 0.0232 N1 0.0438 0.0297 0.0194 N2 0.0432 0.0331 0.0187 N3 0.0399 0.0364 0.0259 N4 0.0650 0.0338 0.0259 O1 0.0865 0.0349 0.0290 O2 0.0515 0.0351 0.0240 O3 0.0783 0.0408 0.0249 O4 0.0977 0.0557 0.0260 O5 0.1003 0.0364 0.0293 O6 0.0723 0.0482 0.0304 O7 0.0590 0.0360 0.0306 O8 0.0871 0.0358 0.0261 O9 0.0470 0.0324 0.0263 O10 0.0855 0.0414 0.0273 O11 0.0656 0.0554 0.0272 O12 0.0663 0.0420 0.0233 O13 0.1068 0.0378 0.0350 O14 0.1436 0.0456 0.0321 O15 0.0880 0.0451 0.0275 O16 0.0534 0.0253 0.0197 S1 0.0349 0.0332 0.0275 S2 0.0358 0.0306 0.0242 S3 0.0574 0.0332 0.0246 S4 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.015 0.023 0.032 0.042 0.054 0.068 0.091 0.133 1.000 Number in group 1540. 1274. 1416. 1479. 1342. 1431. 1349. 1362. 1386. 1402. GooF 0.773 0.867 1.011 1.136 1.162 1.135 1.103 1.120 1.008 0.821 K 4.943 1.105 1.181 1.097 1.034 1.040 1.019 1.013 1.012 1.030 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.06 1.14 1.25 1.43 1.80 inf Number in group 1432. 1393. 1388. 1376. 1423. 1373. 1396. 1402. 1399. 1399. GooF 0.790 0.845 0.863 0.897 0.887 0.926 0.953 1.024 1.097 1.658 K 1.087 1.087 1.038 1.042 1.018 1.018 1.015 1.021 1.032 1.030 R1 0.344 0.303 0.253 0.200 0.151 0.113 0.087 0.079 0.069 0.069 Recommended weighting scheme: WGHT 0.1135 3.0620 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) 7 3 5 403.82 38.96 8.02 0.016 2.16 0 3 1 493.85 153.46 7.82 0.032 6.58 -1 4 2 28.35 241.67 7.82 0.041 4.45 3 1 1 59.32 289.80 6.85 0.045 6.32 1 6 0 158.83 611.40 6.69 0.065 3.52 -2 7 1 308.56 1077.09 6.61 0.086 2.90 -1 2 4 205.01 66.53 6.46 0.021 3.92 5 3 2 377.61 120.47 6.42 0.029 3.38 4 1 1 436.63 158.42 6.37 0.033 5.00 4 0 4 570.89 204.85 6.21 0.037 3.32 3 1 7 1037.03 443.34 6.07 0.055 2.28 0 9 4 804.09 341.30 6.02 0.048 2.08 5 3 0 2.67 86.06 5.77 0.024 3.71 2 5 3 23.47 132.03 5.55 0.030 3.25 -5 1 5 1593.04 783.32 5.29 0.073 2.69 -2 9 3 6.96 97.17 5.25 0.026 2.15 0 4 0 1162.23 586.80 5.08 0.063 5.35 -9 6 3 323.81 112.93 5.05 0.028 1.90 6 2 2 347.47 839.24 5.04 0.076 3.16 -3 8 2 413.31 194.43 4.98 0.037 2.41 4 8 4 333.96 784.10 4.82 0.073 2.08 3 3 0 471.04 236.99 4.75 0.040 5.08 3 0 2 52.31 163.62 4.67 0.033 5.46 -1 2 2 409.93 185.63 4.56 0.036 6.41 -3 9 4 261.06 117.43 4.51 0.028 2.00 4 2 3 220.75 101.96 4.51 0.026 3.65 0 9 3 14.98 120.10 4.43 0.029 2.19 7 16 0 85.51 362.13 4.41 0.050 1.23 -2 8 5 220.01 89.07 4.35 0.025 2.07 -1 8 1 97.93 241.34 4.34 0.041 2.62 10 7 5 373.45 144.55 4.33 0.031 1.56 2 3 1 13.73 58.16 4.28 0.020 5.61 -3 6 2 664.11 369.34 4.24 0.050 3.01 8 5 2 415.73 883.04 4.23 0.078 2.20 8 3 2 307.64 109.96 4.22 0.027 2.42 2 1 2 3959.86 1850.73 4.11 0.113 6.34 1 2 2 146.31 49.74 4.10 0.018 6.35 8 8 10 741.53 347.03 4.10 0.049 1.26 6 5 1 240.78 496.91 4.09 0.058 2.72 8 1 0 488.84 263.29 4.06 0.042 2.69 10 15 2 389.89 112.44 4.06 0.028 1.18 4 1 2 25.19 94.70 4.05 0.025 4.44 9 3 11 1227.17 676.29 4.04 0.068 1.27 8 4 10 218.94 24.99 3.94 0.013 1.38 5 4 0 659.71 1242.89 3.93 0.092 3.37 0 2 3 351.66 669.54 3.90 0.068 5.03 1 5 1 2196.39 1317.12 3.90 0.095 4.07 -4 4 5 115.20 43.28 3.89 0.017 2.56 -3 6 3 161.67 338.23 3.86 0.048 2.80 -8 1 2 792.15 460.39 3.85 0.056 2.59 Bond lengths and angles C1 - Distance Angles N1 1.5153 (0.0046) C2 1.5312 (0.0054) 114.48 (0.31) C1 - N1 C2 - Distance Angles C3 1.5222 (0.0056) C1 1.5312 (0.0054) 110.47 (0.35) C2 - C3 C3 - Distance Angles C2 1.5222 (0.0056) C4 1.5328 (0.0063) 110.28 (0.39) C3 - C2 C4 - Distance Angles C3 1.5328 (0.0063) C4 - C5 - Distance Angles N1 1.5127 (0.0045) C6 1.5191 (0.0055) 115.49 (0.32) C5 - N1 C6 - Distance Angles C5 1.5191 (0.0055) C7 1.5309 (0.0058) 110.82 (0.37) C6 - C5 C7 - Distance Angles C8 1.4782 (0.0063) C6 1.5309 (0.0058) 113.71 (0.40) C7 - C8 C8 - Distance Angles C7 1.4782 (0.0063) C8 - C9 - Distance Angles N1 1.5096 (0.0046) C10 1.5242 (0.0053) 115.34 (0.32) C9 - N1 C10 - Distance Angles C12 1.4406 (0.0077) C9 1.5242 (0.0053) 113.51 (0.44) C10 - C12 C11 - Distance Angles C12 1.3474 (0.0079) C11 - C12 - Distance Angles C11 1.3474 (0.0079) C10 1.4406 (0.0077) 135.61 (0.63) C12 - C11 C13 - Distance Angles N1 1.5208 (0.0047) C14 1.5262 (0.0058) 114.59 (0.33) C13 - N1 C14 - Distance Angles C15 1.4628 (0.0061) C13 1.5262 (0.0058) 114.80 (0.41) C14 - C15 C15 - Distance Angles C14 1.4628 (0.0061) C16 1.5000 (0.0068) 114.06 (0.48) C15 - C14 C16 - Distance Angles C15 1.5000 (0.0068) C16 - C17 - Distance Angles C18 1.5101 (0.0056) N2 1.5236 (0.0046) 115.60 (0.31) C17 - C18 C18 - Distance Angles C17 1.5101 (0.0055) C19 1.5427 (0.0057) 109.82 (0.34) C18 - C17 C19 - Distance Angles C20 1.5063 (0.0064) C18 1.5427 (0.0057) 114.05 (0.39) C19 - C20 C20 - Distance Angles C19 1.5063 (0.0064) C20 - C21 - Distance Angles C22 1.5109 (0.0052) N2 1.5151 (0.0046) 115.64 (0.29) C21 - C22 C22 - Distance Angles C21 1.5109 (0.0052) C23 1.5183 (0.0060) 110.62 (0.34) C22 - C21 C23 - Distance Angles C24 1.5035 (0.0080) C22 1.5183 (0.0060) 113.68 (0.46) C23 - C24 C24 - Distance Angles C23 1.5035 (0.0080) C24 - C25 - Distance Angles N2 1.5119 (0.0050) C26 1.5174 (0.0056) 115.15 (0.31) C25 - N2 C26 - Distance Angles C27 1.5160 (0.0058) C25 1.5174 (0.0057) 110.50 (0.35) C26 - C27 C27 - Distance Angles C28 1.5056 (0.0065) C26 1.5160 (0.0058) 111.01 (0.38) C27 - C28 C28 - Distance Angles C27 1.5056 (0.0065) C28 - C29 - Distance Angles C30 1.5148 (0.0062) N2 1.5159 (0.0046) 115.52 (0.32) C29 - C30 C30 - Distance Angles C29 1.5148 (0.0062) C31 1.6584 (0.0085) 107.09 (0.40) C30 - C29 C31 - Distance Angles C32 1.3866 (0.0083) C30 1.6584 (0.0084) 97.60 (0.60) C31 - C32 C32 - Distance Angles C31 1.3866 (0.0083) C32 - C33 - Distance Angles C34 1.4985 (0.0057) N3 1.5254 (0.0047) 116.27 (0.33) C33 - C34 C34 - Distance Angles C33 1.4985 (0.0057) C35 1.5329 (0.0061) 111.00 (0.37) C34 - C33 C35 - Distance Angles C36 1.4796 (0.0074) C34 1.5329 (0.0061) 113.67 (0.47) C35 - C36 C36 - Distance Angles C35 1.4796 (0.0074) C36 - C37 - Distance Angles C38 1.5030 (0.0060) N3 1.5262 (0.0047) 116.11 (0.32) C37 - C38 C38 - Distance Angles C37 1.5030 (0.0060) C39 1.5269 (0.0064) 107.65 (0.38) C38 - C37 C39 - Distance Angles C40 1.3976 (0.0087) C38 1.5269 (0.0064) 115.85 (0.55) C39 - C40 C40 - Distance Angles C39 1.3976 (0.0087) C40 - C41 - Distance Angles C42 1.5080 (0.0055) N3 1.5202 (0.0049) 115.91 (0.30) C41 - C42 C42 - Distance Angles C41 1.5080 (0.0055) C43 1.5248 (0.0059) 110.01 (0.34) C42 - C41 C43 - Distance Angles C44 1.5252 (0.0061) C42 1.5248 (0.0059) 113.78 (0.40) C43 - C44 C44 - Distance Angles C43 1.5252 (0.0061) C44 - C45 - Distance Angles C46 1.5100 (0.0052) N3 1.5155 (0.0048) 116.25 (0.30) C45 - C46 C46 - Distance Angles C45 1.5100 (0.0052) C47 1.5120 (0.0054) 110.38 (0.32) C46 - C45 C47 - Distance Angles C46 1.5120 (0.0053) C48 1.5153 (0.0057) 112.00 (0.35) C47 - C46 C48 - Distance Angles C47 1.5153 (0.0057) C48 - C49 - Distance Angles C50 1.5080 (0.0063) N4 1.5210 (0.0050) 116.01 (0.36) C49 - C50 C50 - Distance Angles C49 1.5080 (0.0063) C51 1.6015 (0.0091) 103.86 (0.44) C50 - C49 C51 - Distance Angles C52 1.5313 (0.0021) C50 1.6015 (0.0091) 109.22 (0.81) C51 - C52 C52 - Distance Angles C51 1.5313 (0.0021) C52 - C53 - Distance Angles C54 1.5178 (0.0053) N4 1.5322 (0.0048) 115.53 (0.32) C53 - C54 C54 - Distance Angles C55 1.5155 (0.0056) C53 1.5178 (0.0053) 110.77 (0.33) C54 - C55 C55 - Distance Angles C54 1.5155 (0.0056) C56 1.5188 (0.0056) 111.32 (0.36) C55 - C54 C56 - Distance Angles C55 1.5188 (0.0056) C56 - C57 - Distance Angles N4 1.5173 (0.0049) C58 1.5247 (0.0055) 115.87 (0.32) C57 - N4 C58 - Distance Angles C59 1.5117 (0.0056) C57 1.5247 (0.0055) 110.54 (0.36) C58 - C59 C59 - Distance Angles C60 1.4945 (0.0063) C58 1.5117 (0.0056) 113.28 (0.41) C59 - C60 C60 - Distance Angles C59 1.4945 (0.0063) C60 - C61 - Distance Angles C62 1.5043 (0.0056) N4 1.5062 (0.0049) 117.18 (0.34) C61 - C62 C62 - Distance Angles C61 1.5043 (0.0056) C63 1.5068 (0.0062) 110.55 (0.38) C62 - C61 C63 - Distance Angles C64 1.4610 (0.0069) C62 1.5068 (0.0062) 114.92 (0.47) C63 - C64 C64 - Distance Angles C63 1.4610 (0.0070) C64 - N1 - Distance Angles C9 1.5096 (0.0047) C5 1.5127 (0.0045) 105.85 (0.28) C1 1.5153 (0.0046) 111.73 (0.30) 111.25 (0.28) C13 1.5208 (0.0047) 110.78 (0.29) 110.58 (0.29) 106.73 (0.28) N1 - C9 C5 C1 N2 - Distance Angles C25 1.5119 (0.0050) C21 1.5151 (0.0046) 111.87 (0.30) C29 1.5159 (0.0046) 110.84 (0.33) 105.02 (0.26) C17 1.5236 (0.0046) 105.33 (0.27) 111.98 (0.30) 111.95 (0.31) N2 - C25 C21 C29 N3 - Distance Angles C45 1.5155 (0.0048) C41 1.5202 (0.0049) 111.36 (0.30) C37 1.5262 (0.0047) 111.90 (0.30) 105.01 (0.27) C33 1.5254 (0.0047) 105.83 (0.27) 112.23 (0.30) 110.65 (0.31) N3 - C45 C41 C37 N4 - Distance Angles C61 1.5062 (0.0049) C57 1.5173 (0.0049) 108.50 (0.30) C49 1.5210 (0.0050) 108.71 (0.31) 111.94 (0.31) C53 1.5322 (0.0048) 111.56 (0.31) 107.99 (0.29) 108.18 (0.30) N4 - C61 C57 C49 O1 - Distance Angles S1 1.4336 (0.0028) O1 - O2 - Distance Angles S1 1.4390 (0.0030) O2 - O3 - Distance Angles S1 1.4690 (0.0027) O3 - O4 - Distance Angles S1 1.5766 (0.0033) O4 - O5 - Distance Angles S2 1.4327 (0.0030) O5 - O6 - Distance Angles S2 1.4661 (0.0030) O6 - O7 - Distance Angles S2 1.4341 (0.0029) O7 - O8 - Distance Angles S2 1.5531 (0.0029) O8 - O9 - Distance Angles S3 1.4499 (0.0029) O9 - O10 - Distance Angles S3 1.5678 (0.0030) O10 - O11 - Distance Angles S3 1.4441 (0.0029) O11 - O12 - Distance Angles S3 1.4257 (0.0028) O12 - O13 - Distance Angles S4 1.4840 (0.0029) O13 - O14 - Distance Angles S4 1.4401 (0.0031) O14 - O15 - Distance Angles S4 1.5505 (0.0037) O15 - O16 - Distance Angles S4 1.4281 (0.0029) O16 - S1 - Distance Angles O1 1.4336 (0.0028) O2 1.4390 (0.0030) 114.50 (0.17) O3 1.4690 (0.0027) 112.60 (0.16) 112.75 (0.18) O4 1.5766 (0.0033) 107.14 (0.18) 103.87 (0.19) 104.93 (0.17) S1 - O1 O2 O3 S2 - Distance Angles O5 1.4327 (0.0030) O7 1.4341 (0.0029) 112.69 (0.19) O6 1.4661 (0.0030) 111.74 (0.22) 112.71 (0.20) O8 1.5531 (0.0029) 107.31 (0.19) 105.94 (0.18) 105.89 (0.17) S2 - O5 O7 O6 S3 - Distance Angles O12 1.4257 (0.0028) O11 1.4441 (0.0029) 113.09 (0.18) O9 1.4499 (0.0029) 113.83 (0.19) 111.80 (0.20) O10 1.5678 (0.0030) 104.51 (0.18) 106.87 (0.17) 105.94 (0.17) S3 - O12 O11 O9 S4 - Distance Angles O16 1.4281 (0.0029) O14 1.4401 (0.0031) 113.73 (0.19) O13 1.4840 (0.0029) 111.51 (0.19) 112.68 (0.18) O15 1.5505 (0.0037) 106.67 (0.22) 106.40 (0.24) 105.14 (0.18) S4 - O16 O14 O13 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.79(4) 1.85(4) 2.628(4) 171(4) O10-H10...O3 0.84(6) 1.82(6) 2.649(5) 171(6) O4-H4...O9 0.93(7) 1.69(7) 2.602(4) 166(7) O8-H8...O13 0.82(8) 1.78(8) 2.590(5) 170(9) O15-H15...O6 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)