+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + ssf1327 started at 12:17:10 on 06-May-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL ssf1327 in P-1 CELL 0.69050 11.1890 11.2080 21.9060 84.512 85.814 89.942 ZERR 8.00 0.0070 0.0060 0.0130 0.007 0.007 0.007 LATT 1 SFAC C H N O UNIT 88 184 8 32 V = 2727.21 F(000) = 1024.0 Mu = 0.09 mm-1 Cell Wt = 1866.43 Rho = 1.136 MERG 2 OMIT 1 -2 2 OMIT 1 3 6 OMIT 4 -2 1 OMIT -1 -1 4 OMIT -1 -2 2 TWIN 0.00 -1.00 0.00 -1.00 0.00 0.00 0.00 0.00 -1.00 2 BASF 0.14020 EXTI 0.07560 SHEL 7 0.77 CONF HTAB N45 O31A HTAB N45 O52B HTAB N85 O52A EQIV_$1 x+1, y, z-1 HTAB N25 O72A_$1 HTAB N25 O71A_$1 EQIV_$2 -x+1, -y+3, -z HTAB N25 O1A_$2 EQIV_$3 x, y-1, z HTAB N25 O1A_$3 EQIV_$4 -x+1, -y+1, -z+1 HTAB N45 O31A_$4 EQIV_$5 x+1, y-1, z+1 HTAB N65 O1B_$5 EQIV_$6 -x+1, -y+1, -z+2 HTAB N65 O72B_$6 EQIV_$7 x+1, y, z HTAB N65 O72B_$7 EQIV_$8 -x, -y+2, -z+1 HTAB N85 O52A_$8 HTAB N85 O51B_$8 EQIV_$9 x-1, y, z HTAB N85 O31B_$9 HTAB N85 O32B_$9 FMAP 2 PLAN 20 MPLA C71 O71A O71B MPLA C72 O72A O72B SIZE 0.01 0.04 0.04 ACTA BOND $H WGHT 0.12220 10.97510 L.S. 4 TEMP -153.00 FVAR 0.25661 MOLE 1 C1 1 0.346002 1.775250 0.003017 11.00000 0.03562 0.03504 = 0.04257 -0.00877 0.00098 -0.00050 C2 1 0.379665 1.668710 0.046032 11.00000 0.03324 0.03962 = 0.04507 -0.00534 -0.00185 -0.00531 C3 1 0.378432 1.457096 0.063253 11.00000 0.03600 0.03568 = 0.07250 0.00115 -0.00955 -0.00773 AFIX 137 H3A 2 0.459625 1.464287 0.076579 11.00000 -1.50000 H3B 2 0.374459 1.388319 0.038997 11.00000 -1.50000 H3C 2 0.321195 1.445405 0.099394 11.00000 -1.50000 AFIX 0 O1A 4 0.405598 1.869708 0.008370 11.00000 0.04141 0.03351 = 0.04478 -0.00435 -0.01267 -0.01448 O1B 4 0.264418 1.763871 -0.031622 11.00000 0.04277 0.03442 = 0.04296 -0.00036 -0.01246 -0.01596 O2A 4 0.349351 1.563725 0.026569 11.00000 0.03519 0.02600 = 0.05460 -0.00486 -0.00820 -0.00912 O2B 4 0.428959 1.674742 0.093843 11.00000 0.07715 0.04537 = 0.05374 -0.00370 -0.03166 -0.00889 MOLE 2 C21 1 0.435847 1.188620 0.185753 11.00000 0.05987 0.04802 = 0.06177 -0.00701 0.01176 0.00300 AFIX 137 H21A 2 0.445044 1.233878 0.145124 11.00000 -1.50000 H21B 2 0.493733 1.218229 0.212309 11.00000 -1.50000 H21C 2 0.354357 1.198941 0.204030 11.00000 -1.50000 AFIX 0 C22 1 0.458438 1.055043 0.179160 11.00000 0.04039 0.03347 = 0.03794 -0.01072 -0.00283 0.00176 C23 1 0.591101 1.045560 0.156628 11.00000 0.03483 0.03326 = 0.02932 -0.00225 0.00114 -0.01140 AFIX 23 H23A 2 0.606118 1.110708 0.123113 11.00000 -1.20000 H23B 2 0.637685 1.066332 0.190893 11.00000 -1.20000 AFIX 0 C24 1 0.649349 0.933896 0.133388 11.00000 0.02884 0.03490 = 0.02959 -0.00044 -0.00369 -0.00829 C26 1 0.432892 0.987977 0.243717 11.00000 0.04738 0.05824 = 0.04837 0.00234 0.01397 0.00306 AFIX 137 H26A 2 0.353518 1.010236 0.260833 11.00000 -1.50000 H26B 2 0.493849 1.009792 0.270673 11.00000 -1.50000 H26C 2 0.435098 0.901343 0.240613 11.00000 -1.50000 AFIX 0 C27 1 0.373621 1.014162 0.133989 11.00000 0.03073 0.07168 = 0.08644 -0.03335 -0.00239 0.00553 AFIX 137 H27A 2 0.392429 1.057414 0.093398 11.00000 -1.50000 H27B 2 0.290814 1.030859 0.148315 11.00000 -1.50000 H27C 2 0.382983 0.927877 0.131156 11.00000 -1.50000 AFIX 0 C28 1 0.785847 0.954997 0.125707 11.00000 0.02618 0.04443 = 0.03888 -0.00844 -0.00356 -0.00697 AFIX 137 H28A 2 0.815962 0.964111 0.165915 11.00000 -1.50000 H28B 2 0.803609 1.027918 0.098147 11.00000 -1.50000 H28C 2 0.824818 0.886386 0.108171 11.00000 -1.50000 AFIX 0 C29 1 0.621845 0.816682 0.172173 11.00000 0.03995 0.03365 = 0.03820 -0.00473 -0.00088 -0.00073 AFIX 137 H29A 2 0.641724 0.823989 0.214496 11.00000 -1.50000 H29B 2 0.669566 0.752540 0.155265 11.00000 -1.50000 H29C 2 0.536440 0.797638 0.171867 11.00000 -1.50000 AFIX 0 N25 3 0.612978 0.916410 0.069067 11.00000 0.02754 0.03273 = 0.03183 -0.00261 -0.00252 -0.00916 AFIX 137 H25A 2 0.663142 0.862972 0.051823 11.00000 -1.50000 H25B 2 0.617648 0.987821 0.045441 11.00000 -1.50000 H25C 2 0.536442 0.888004 0.071559 11.00000 -1.50000 AFIX 0 MOLE 3 C31 1 0.720712 0.660102 0.490759 11.00000 0.03052 0.02446 = 0.03352 -0.00419 -0.00589 -0.01039 C32 1 0.832462 0.627606 0.451196 11.00000 0.02799 0.03413 = 0.05032 -0.00383 -0.00343 -0.00806 C33 1 1.043697 0.625107 0.441908 11.00000 0.03501 0.02837 = 0.05837 -0.00692 0.00004 -0.00253 AFIX 137 H33A 2 1.041781 0.538649 0.438334 11.00000 -1.50000 H33B 2 1.111297 0.644316 0.465353 11.00000 -1.50000 H33C 2 1.053002 0.668298 0.400766 11.00000 -1.50000 AFIX 0 O31A 4 0.624614 0.609956 0.479452 11.00000 0.03395 0.03728 = 0.04156 -0.00697 -0.00356 -0.00976 O31B 4 0.732325 0.732453 0.529670 11.00000 0.03242 0.04528 = 0.04541 -0.01683 -0.00226 -0.01177 O32A 4 0.830525 0.576710 0.405134 11.00000 0.04476 0.10163 = 0.06105 -0.05119 -0.00624 -0.00036 O32B 4 0.932787 0.660690 0.473371 11.00000 0.02549 0.03425 = 0.05107 -0.01330 -0.00185 -0.00803 MOLE 4 C41 1 0.663137 0.407114 0.713622 11.00000 0.07449 0.05310 = 0.06384 -0.00496 -0.04291 0.01056 AFIX 137 H41A 2 0.731453 0.462566 0.706238 11.00000 -1.50000 H41B 2 0.691234 0.324817 0.710893 11.00000 -1.50000 H41C 2 0.624399 0.414198 0.754695 11.00000 -1.50000 AFIX 0 C42 1 0.571118 0.438641 0.664222 11.00000 0.04134 0.03222 = 0.03856 0.00389 -0.01326 -0.00321 C43 1 0.549573 0.572949 0.660660 11.00000 0.03559 0.04402 = 0.03799 -0.00575 -0.00909 -0.00599 AFIX 23 H43A 2 0.622033 0.610927 0.638369 11.00000 -1.20000 H43B 2 0.549038 0.594893 0.703395 11.00000 -1.20000 AFIX 0 C44 1 0.443300 0.636775 0.633017 11.00000 0.03947 0.03023 = 0.02348 -0.00678 -0.00172 -0.00052 C46 1 0.458389 0.361061 0.684392 11.00000 0.06027 0.04235 = 0.05240 0.00180 -0.00250 -0.00522 AFIX 137 H46A 2 0.422562 0.384447 0.723619 11.00000 -1.50000 H46B 2 0.480928 0.276355 0.689279 11.00000 -1.50000 H46C 2 0.400212 0.373197 0.653063 11.00000 -1.50000 AFIX 0 C47 1 0.627926 0.398535 0.603208 11.00000 0.04698 0.03082 = 0.05492 -0.00486 -0.01048 -0.00618 AFIX 137 H47A 2 0.567955 0.402835 0.572638 11.00000 -1.50000 H47B 2 0.656259 0.315910 0.610064 11.00000 -1.50000 H47C 2 0.695628 0.451399 0.588187 11.00000 -1.50000 AFIX 0 C48 1 0.324071 0.612338 0.669456 11.00000 0.04345 0.03949 = 0.04040 -0.00859 0.00421 -0.00131 AFIX 137 H48A 2 0.332582 0.623152 0.712797 11.00000 -1.50000 H48B 2 0.298526 0.529864 0.665824 11.00000 -1.50000 H48C 2 0.263983 0.668190 0.653318 11.00000 -1.50000 AFIX 0 C49 1 0.470305 0.772318 0.627157 11.00000 0.04292 0.02053 = 0.04254 -0.00687 -0.00680 -0.00019 AFIX 137 H49A 2 0.400261 0.816480 0.613024 11.00000 -1.50000 H49B 2 0.539200 0.790182 0.597433 11.00000 -1.50000 H49C 2 0.488632 0.796509 0.667288 11.00000 -1.50000 AFIX 0 N45 3 0.425965 0.609602 0.567712 11.00000 0.02806 0.02633 = 0.03670 -0.00302 -0.00459 -0.00353 AFIX 137 H45A 2 0.497504 0.616282 0.545032 11.00000 0.06893 H45B 2 0.373076 0.662519 0.550824 11.00000 0.03392 H45C 2 0.396917 0.533705 0.568102 11.00000 0.03337 AFIX 0 MOLE 5 C51 1 0.330074 0.898267 0.455057 11.00000 0.03001 0.03333 = 0.04087 -0.00833 0.00066 -0.00415 C52 1 0.222856 0.848806 0.499365 11.00000 0.02800 0.02821 = 0.04011 -0.00676 -0.00386 -0.00346 C53 1 0.540535 0.898431 0.435873 11.00000 0.03520 0.03437 = 0.06442 -0.00325 0.00244 -0.01553 AFIX 137 H53A 2 0.539405 0.866667 0.395762 11.00000 -1.50000 H53B 2 0.612263 0.869950 0.455793 11.00000 -1.50000 H53C 2 0.541606 0.986231 0.430185 11.00000 -1.50000 AFIX 0 O51A 4 0.433878 0.857422 0.474383 11.00000 0.03035 0.02966 = 0.04272 -0.00185 0.00281 -0.00259 O51B 4 0.318677 0.963774 0.408689 11.00000 0.04483 0.05925 = 0.04476 0.01731 0.00132 -0.00906 O52A 4 0.130201 0.909537 0.493592 11.00000 0.03445 0.03969 = 0.04086 0.00737 -0.00133 -0.00298 O52B 4 0.238003 0.756857 0.533369 11.00000 0.03761 0.03713 = 0.04179 0.00487 -0.00233 0.00031 MOLE 6 C61 1 0.983355 0.348546 0.784530 11.00000 0.05284 0.07301 = 0.06843 -0.03364 -0.01395 -0.01353 AFIX 137 H61A 2 1.039504 0.282751 0.792644 11.00000 -1.50000 H61B 2 1.003536 0.389069 0.743424 11.00000 -1.50000 H61C 2 0.901541 0.316473 0.786745 11.00000 -1.50000 AFIX 0 C62 1 0.991969 0.438639 0.832881 11.00000 0.04270 0.03097 = 0.03906 -0.01384 -0.01533 -0.00936 C63 1 1.127208 0.463993 0.836650 11.00000 0.03930 0.03781 = 0.04158 -0.00882 0.00052 -0.00672 AFIX 23 H63A 2 1.160264 0.390405 0.857637 11.00000 -1.20000 H63B 2 1.162983 0.469976 0.793772 11.00000 -1.20000 AFIX 0 C64 1 1.180264 0.569917 0.866512 11.00000 0.02985 0.03267 = 0.03077 -0.00541 0.00026 0.00033 C66 1 0.919665 0.549511 0.814448 11.00000 0.04736 0.05912 = 0.05036 -0.00791 -0.01095 -0.00893 AFIX 137 H66A 2 0.955664 0.589740 0.775785 11.00000 -1.50000 H66B 2 0.919615 0.604337 0.846720 11.00000 -1.50000 H66C 2 0.837109 0.525923 0.808958 11.00000 -1.50000 AFIX 0 C67 1 0.935884 0.379179 0.894363 11.00000 0.04306 0.05003 = 0.06472 -0.01618 -0.00503 -0.01897 AFIX 137 H67A 2 0.857711 0.344808 0.888118 11.00000 -1.50000 H67B 2 0.925502 0.439277 0.923974 11.00000 -1.50000 H67C 2 0.988642 0.315501 0.910236 11.00000 -1.50000 AFIX 0 C68 1 1.161561 0.693204 0.831312 11.00000 0.04975 0.03716 = 0.03410 -0.00150 0.00119 -0.00625 AFIX 137 H68A 2 1.207005 0.754164 0.849223 11.00000 -1.50000 H68B 2 1.076174 0.713177 0.834283 11.00000 -1.50000 H68C 2 1.189590 0.690803 0.788008 11.00000 -1.50000 AFIX 0 C69 1 1.313519 0.544654 0.870008 11.00000 0.03352 0.03561 = 0.04433 -0.00575 0.00796 -0.00057 AFIX 137 H69A 2 1.351048 0.608969 0.889346 11.00000 -1.50000 H69B 2 1.351134 0.540716 0.828428 11.00000 -1.50000 H69C 2 1.324096 0.468024 0.894498 11.00000 -1.50000 AFIX 0 N65 3 1.131153 0.576972 0.931817 11.00000 0.02811 0.02849 = 0.03939 -0.00255 0.00192 -0.01098 AFIX 137 H65A 2 1.172351 0.633642 0.948944 11.00000 -1.50000 H65B 2 1.139123 0.504574 0.953713 11.00000 -1.50000 H65C 2 1.052267 0.596969 0.932310 11.00000 -1.50000 AFIX 0 MOLE 7 C71 1 -0.113797 0.833745 0.951194 11.00000 0.03259 0.03090 = 0.03575 -0.00601 0.00952 -0.00346 C72 1 -0.160962 0.718148 0.990891 11.00000 0.02901 0.02641 = 0.04083 -0.01010 0.00392 -0.00642 C73 1 -0.107627 1.045727 0.942847 11.00000 0.03657 0.03097 = 0.05500 0.00545 -0.00046 -0.00465 AFIX 137 H73A 2 -0.019954 1.043587 0.937455 11.00000 -1.50000 H73B 2 -0.132324 1.111431 0.967353 11.00000 -1.50000 H73C 2 -0.140570 1.058365 0.902505 11.00000 -1.50000 AFIX 0 O71A 4 -0.152490 0.931890 0.974557 11.00000 0.03530 0.02145 = 0.04715 0.00250 0.00525 -0.00559 O71B 4 -0.052725 0.832259 0.905648 11.00000 0.10235 0.03730 = 0.07303 -0.00843 0.03834 -0.00695 O72A 4 -0.242825 0.729558 1.029969 11.00000 0.04085 0.03085 = 0.05089 -0.00769 0.00519 -0.01045 O72B 4 -0.105157 0.625286 0.979763 11.00000 0.03186 0.03072 = 0.04706 -0.00583 0.00044 -0.00513 MOLE 8 C81 1 -0.011251 0.990983 0.743793 11.00000 0.05901 0.04670 = 0.05970 -0.02366 -0.00728 -0.00471 AFIX 137 H81A 2 0.003194 1.069227 0.758473 11.00000 -1.50000 H81B 2 0.016705 0.927426 0.773159 11.00000 -1.50000 H81C 2 -0.097238 0.980576 0.739932 11.00000 -1.50000 AFIX 0 C82 1 0.057478 0.984237 0.680424 11.00000 0.05073 0.03762 = 0.04454 -0.01046 -0.02083 -0.01401 C83 1 0.050526 0.857674 0.658435 11.00000 0.02893 0.03747 = 0.03042 0.00172 -0.00422 -0.00346 AFIX 23 H83A 2 0.116030 0.853933 0.625769 11.00000 -1.20000 H83B 2 0.072199 0.801143 0.693374 11.00000 -1.20000 AFIX 0 C84 1 -0.060525 0.803844 0.633857 11.00000 0.03275 0.03563 = 0.03495 -0.00917 0.00142 -0.00990 C86 1 0.191705 1.002812 0.689781 11.00000 0.04193 0.06192 = 0.06522 -0.01209 -0.01390 -0.01548 AFIX 137 H86A 2 0.239194 0.997032 0.650788 11.00000 -1.50000 H86B 2 0.217495 0.941005 0.720704 11.00000 -1.50000 H86C 2 0.203430 1.082161 0.703775 11.00000 -1.50000 AFIX 0 C87 1 0.016386 1.079959 0.634729 11.00000 0.09949 0.03556 = 0.07255 0.00269 -0.03449 -0.03364 AFIX 137 H87A 2 0.053345 1.068234 0.593802 11.00000 -1.50000 H87B 2 0.039831 1.158572 0.646178 11.00000 -1.50000 H87C 2 -0.071016 1.075957 0.634187 11.00000 -1.50000 AFIX 0 C88 1 -0.177196 0.815684 0.673786 11.00000 0.02894 0.03548 = 0.04568 -0.00895 -0.00832 -0.00144 AFIX 137 H88A 2 -0.198237 0.900555 0.673965 11.00000 -1.50000 H88B 2 -0.166493 0.781567 0.715905 11.00000 -1.50000 H88C 2 -0.241572 0.772512 0.657058 11.00000 -1.50000 AFIX 0 C89 1 -0.035782 0.672449 0.626312 11.00000 0.04577 0.03166 = 0.03615 -0.00276 -0.00996 0.00255 AFIX 137 H89A 2 -0.019115 0.630664 0.666131 11.00000 -1.50000 H89B 2 0.033684 0.665988 0.596892 11.00000 -1.50000 H89C 2 -0.105967 0.636006 0.611051 11.00000 -1.50000 AFIX 0 N85 3 -0.079430 0.863052 0.570033 11.00000 0.02820 0.03271 = 0.03403 -0.00677 -0.00594 -0.00344 AFIX 137 H85A 2 -0.111653 0.937003 0.573119 11.00000 -1.50000 H85B 2 -0.130148 0.817332 0.551287 11.00000 -1.50000 H85C 2 -0.007820 0.870307 0.547439 11.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for ssf1327 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1B O1A C2 C2 - O2B O2A C1 C3 - O2A O1A - C1 O1B - C1 O2A - C2 C3 O2B - C2 C21 - C22 C22 - C27 C23 C21 C26 C23 - C24 C22 C24 - C29 C23 N25 C28 C26 - C22 C27 - C22 C28 - C24 C29 - C24 N25 - C24 C31 - O31B O31A C32 C32 - O32A O32B C31 C33 - O32B O31A - C31 O31B - C31 O32A - C32 O32B - C32 C33 C41 - C42 C42 - C43 C47 C46 C41 C43 - C42 C44 C44 - C48 N45 C43 C49 C46 - C42 C47 - C42 C48 - C44 C49 - C44 N45 - C44 C51 - O51B O51A C52 C52 - O52B O52A C51 C53 - O51A O51A - C51 C53 O51B - C51 O52A - C52 O52B - C52 C61 - C62 C62 - C66 C67 C61 C63 C63 - C64 C62 C64 - N65 C69 C68 C63 C66 - C62 C67 - C62 C68 - C64 C69 - C64 N65 - C64 C71 - O71B O71A C72 C72 - O72A O72B C71 C73 - O71A O71A - C71 C73 O71B - C71 O72A - C72 O72B - C72 C81 - C82 C82 - C87 C83 C81 C86 C83 - C84 C82 C84 - N85 C89 C88 C83 C86 - C82 C87 - C82 C88 - C84 C89 - C84 N85 - C84 Operators for generating equivalent atoms: $1 x+1, y, z-1 $2 -x+1, -y+3, -z $3 x, y-1, z $4 -x+1, -y+1, -z+1 $5 x+1, y-1, z+1 $6 -x+1, -y+1, -z+2 $7 x+1, y, z $8 -x, -y+2, -z+1 $9 x-1, y, z 14917 Reflections read, of which 17 rejected -11 =< h =< 11, -11 =< k =< 11, -22 =< l =< 23, Max. 2-theta = 42.67 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -1 2 0 45.69 1.71 2 8.67 1 3 2 8.33 0.90 2 4.91 2 Inconsistent equivalents 6612 Unique reflections, of which 0 suppressed R(int) = 0.0668 R(sigma) = 0.0859 Friedel opposites merged Maximum memory for data reduction = 7848 / 65352 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 = 9763 / 833990 wR2 = 0.2715 before cycle 1 for 6612 data and 610 / 610 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1222 * P )^2 + 10.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25659 0.00146 -0.013 OSF 2 0.14023 0.00242 0.011 BASF 1 3 0.07551 0.00634 -0.015 EXTI Mean shift/esd = 0.001 Maximum = -0.015 for EXTI Max. shift = 0.000 A for H21A Max. dU = 0.000 for H45A Least-squares cycle 2 Maximum vector length = 511 Memory required = 9763 / 833990 wR2 = 0.2715 before cycle 2 for 6612 data and 610 / 610 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1222 * P )^2 + 10.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25658 0.00146 -0.010 OSF 2 0.14024 0.00242 0.005 BASF 1 3 0.07543 0.00634 -0.011 EXTI Mean shift/esd = 0.001 Maximum = -0.011 for EXTI Max. shift = 0.000 A for H61C Max. dU = 0.000 for H45A Least-squares cycle 3 Maximum vector length = 511 Memory required = 9763 / 833990 wR2 = 0.2715 before cycle 3 for 6612 data and 610 / 610 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1222 * P )^2 + 10.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25658 0.00146 -0.001 OSF 2 0.14024 0.00242 0.001 BASF 1 3 0.07542 0.00633 -0.002 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for EXTI Max. shift = 0.000 A for H61C Max. dU = 0.000 for H45A Least-squares cycle 4 Maximum vector length = 511 Memory required = 9763 / 833990 wR2 = 0.2715 before cycle 4 for 6612 data and 610 / 610 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1222 * P )^2 + 10.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25658 0.00146 0.000 OSF 2 0.14024 0.00242 0.000 BASF 1 3 0.07542 0.00633 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for EXTI Max. shift = 0.000 A for H53C Max. dU = 0.000 for H45C Largest correlation matrix elements 0.765 EXTI / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3A 0.4596 1.4643 0.0766 137 0.980 0.000 C3 O2A H3A H3B 0.3745 1.3883 0.0390 137 0.980 0.000 C3 O2A H3A H3C 0.3212 1.4454 0.0994 137 0.980 0.000 C3 O2A H3A H21A 0.4451 1.2339 0.1451 137 0.980 0.000 C21 C22 H21A H21B 0.4937 1.2182 0.2123 137 0.980 0.000 C21 C22 H21A H21C 0.3544 1.1989 0.2040 137 0.980 0.000 C21 C22 H21A H23A 0.6061 1.1107 0.1231 23 0.990 0.000 C23 C24 C22 H23B 0.6377 1.0663 0.1909 23 0.990 0.000 C23 C24 C22 H26A 0.3535 1.0102 0.2608 137 0.980 0.000 C26 C22 H26A H26B 0.4938 1.0098 0.2707 137 0.980 0.000 C26 C22 H26A H26C 0.4351 0.9013 0.2406 137 0.980 0.000 C26 C22 H26A H27A 0.3924 1.0574 0.0934 137 0.980 0.000 C27 C22 H27A H27B 0.2908 1.0309 0.1483 137 0.980 0.000 C27 C22 H27A H27C 0.3830 0.9279 0.1312 137 0.980 0.000 C27 C22 H27A H28A 0.8160 0.9641 0.1659 137 0.980 0.000 C28 C24 H28A H28B 0.8036 1.0279 0.0981 137 0.980 0.000 C28 C24 H28A H28C 0.8248 0.8864 0.1082 137 0.980 0.000 C28 C24 H28A H29A 0.6417 0.8240 0.2145 137 0.980 0.000 C29 C24 H29A H29B 0.6696 0.7525 0.1553 137 0.980 0.000 C29 C24 H29A H29C 0.5364 0.7976 0.1719 137 0.980 0.000 C29 C24 H29A H25A 0.6631 0.8630 0.0518 137 0.910 0.000 N25 C24 H25A H25B 0.6177 0.9878 0.0454 137 0.910 0.000 N25 C24 H25A H25C 0.5364 0.8880 0.0716 137 0.910 0.000 N25 C24 H25A H33A 1.0418 0.5386 0.4383 137 0.980 0.000 C33 O32B H33A H33B 1.1113 0.6443 0.4653 137 0.980 0.000 C33 O32B H33A H33C 1.0530 0.6683 0.4008 137 0.980 0.000 C33 O32B H33A H41A 0.7315 0.4626 0.7062 137 0.980 0.000 C41 C42 H41A H41B 0.6912 0.3248 0.7109 137 0.980 0.000 C41 C42 H41A H41C 0.6244 0.4142 0.7547 137 0.980 0.000 C41 C42 H41A H43A 0.6220 0.6109 0.6384 23 0.990 0.000 C43 C42 C44 H43B 0.5490 0.5949 0.7034 23 0.990 0.000 C43 C42 C44 H46A 0.4226 0.3845 0.7236 137 0.980 0.000 C46 C42 H46A H46B 0.4809 0.2764 0.6893 137 0.980 0.000 C46 C42 H46A H46C 0.4002 0.3732 0.6531 137 0.980 0.000 C46 C42 H46A H47A 0.5680 0.4028 0.5726 137 0.980 0.000 C47 C42 H47A H47B 0.6563 0.3159 0.6101 137 0.980 0.000 C47 C42 H47A H47C 0.6956 0.4514 0.5882 137 0.980 0.000 C47 C42 H47A H48A 0.3326 0.6232 0.7128 137 0.980 0.000 C48 C44 H48A H48B 0.2985 0.5299 0.6658 137 0.980 0.000 C48 C44 H48A H48C 0.2640 0.6682 0.6533 137 0.980 0.000 C48 C44 H48A H49A 0.4003 0.8165 0.6130 137 0.980 0.000 C49 C44 H49A H49B 0.5392 0.7902 0.5974 137 0.980 0.000 C49 C44 H49A H49C 0.4886 0.7965 0.6673 137 0.980 0.000 C49 C44 H49A H45A 0.4975 0.6163 0.5450 137 0.910 0.000 N45 C44 H45A H45B 0.3731 0.6625 0.5508 137 0.910 0.000 N45 C44 H45A H45C 0.3969 0.5337 0.5681 137 0.910 0.000 N45 C44 H45A H53A 0.5394 0.8667 0.3958 137 0.980 0.000 C53 O51A H53A H53B 0.6123 0.8700 0.4558 137 0.980 0.000 C53 O51A H53A H53C 0.5416 0.9862 0.4302 137 0.980 0.000 C53 O51A H53A H61A 1.0395 0.2827 0.7926 137 0.980 0.000 C61 C62 H61A H61B 1.0035 0.3891 0.7434 137 0.980 0.000 C61 C62 H61A H61C 0.9015 0.3165 0.7867 137 0.980 0.000 C61 C62 H61A H63A 1.1603 0.3904 0.8576 23 0.990 0.000 C63 C64 C62 H63B 1.1630 0.4700 0.7938 23 0.990 0.000 C63 C64 C62 H66A 0.9557 0.5897 0.7758 137 0.980 0.000 C66 C62 H66A H66B 0.9196 0.6043 0.8467 137 0.980 0.000 C66 C62 H66A H66C 0.8371 0.5259 0.8090 137 0.980 0.000 C66 C62 H66A H67A 0.8577 0.3448 0.8881 137 0.980 0.000 C67 C62 H67A H67B 0.9255 0.4393 0.9240 137 0.980 0.000 C67 C62 H67A H67C 0.9886 0.3155 0.9102 137 0.980 0.000 C67 C62 H67A H68A 1.2070 0.7542 0.8492 137 0.980 0.000 C68 C64 H68A H68B 1.0762 0.7132 0.8343 137 0.980 0.000 C68 C64 H68A H68C 1.1896 0.6908 0.7880 137 0.980 0.000 C68 C64 H68A H69A 1.3511 0.6090 0.8893 137 0.980 0.000 C69 C64 H69A H69B 1.3511 0.5407 0.8284 137 0.980 0.000 C69 C64 H69A H69C 1.3241 0.4680 0.8945 137 0.980 0.000 C69 C64 H69A H65A 1.1724 0.6336 0.9489 137 0.910 0.000 N65 C64 H65A H65B 1.1391 0.5046 0.9537 137 0.910 0.000 N65 C64 H65A H65C 1.0523 0.5970 0.9323 137 0.910 0.000 N65 C64 H65A H73A -0.0200 1.0436 0.9375 137 0.980 0.000 C73 O71A H73A H73B -0.1323 1.1114 0.9674 137 0.980 0.000 C73 O71A H73A H73C -0.1406 1.0584 0.9025 137 0.980 0.000 C73 O71A H73A H81A 0.0032 1.0692 0.7585 137 0.980 0.000 C81 C82 H81A H81B 0.0167 0.9274 0.7732 137 0.980 0.000 C81 C82 H81A H81C -0.0972 0.9806 0.7399 137 0.980 0.000 C81 C82 H81A H83A 0.1160 0.8539 0.6258 23 0.990 0.000 C83 C84 C82 H83B 0.0722 0.8011 0.6934 23 0.990 0.000 C83 C84 C82 H86A 0.2392 0.9970 0.6508 137 0.980 0.000 C86 C82 H86A H86B 0.2175 0.9410 0.7207 137 0.980 0.000 C86 C82 H86A H86C 0.2034 1.0822 0.7038 137 0.980 0.000 C86 C82 H86A H87A 0.0533 1.0682 0.5938 137 0.980 0.000 C87 C82 H87A H87B 0.0398 1.1586 0.6462 137 0.980 0.000 C87 C82 H87A H87C -0.0710 1.0760 0.6342 137 0.980 0.000 C87 C82 H87A H88A -0.1982 0.9006 0.6740 137 0.980 0.000 C88 C84 H88A H88B -0.1665 0.7816 0.7159 137 0.980 0.000 C88 C84 H88A H88C -0.2416 0.7725 0.6571 137 0.980 0.000 C88 C84 H88A H89A -0.0191 0.6307 0.6661 137 0.980 0.000 C89 C84 H89A H89B 0.0337 0.6660 0.5969 137 0.980 0.000 C89 C84 H89A H89C -0.1060 0.6360 0.6110 137 0.980 0.000 C89 C84 H89A H85A -0.1117 0.9370 0.5731 137 0.910 0.000 N85 C84 H85A H85B -0.1301 0.8173 0.5513 137 0.910 0.000 N85 C84 H85A H85C -0.0078 0.8703 0.5474 137 0.910 0.000 N85 C84 H85A ssf1327 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.34600 1.77525 0.00302 1.00000 0.03562 0.03504 0.04255 -0.00876 0.00098 -0.00051 0.03760 0.01404 0.00075 0.00073 0.00038 0.00000 0.00482 0.00509 0.00513 0.00401 0.00414 0.00396 0.00203 C2 0.37967 1.66871 0.04603 1.00000 0.03323 0.03962 0.04506 -0.00534 -0.00184 -0.00531 0.03927 0.01392 0.00072 0.00074 0.00041 0.00000 0.00467 0.00539 0.00554 0.00421 0.00417 0.00377 0.00208 C3 0.37843 1.45710 0.06325 1.00000 0.03599 0.03566 0.07250 0.00115 -0.00955 -0.00773 0.04818 0.01455 0.00077 0.00076 0.00045 0.00000 0.00495 0.00526 0.00662 0.00468 0.00454 0.00388 0.00236 H3A 0.45963 1.46428 0.07658 1.00000 0.07227 0.00000 0.00000 H3B 0.37446 1.38832 0.03900 1.00000 0.07227 0.00000 0.00000 H3C 0.32120 1.44541 0.09940 1.00000 0.07227 0.00000 0.00000 O1A 0.40560 1.86971 0.00837 1.00000 0.04140 0.03350 0.04478 -0.00436 -0.01267 -0.01448 0.03938 0.00802 0.00048 0.00047 0.00025 0.00000 0.00328 0.00331 0.00343 0.00260 0.00263 0.00262 0.00140 O1B 0.26442 1.76387 -0.03162 1.00000 0.04276 0.03441 0.04295 -0.00035 -0.01247 -0.01596 0.03979 0.00848 0.00049 0.00047 0.00025 0.00000 0.00341 0.00325 0.00340 0.00259 0.00289 0.00255 0.00142 O2A 0.34935 1.56373 0.02657 1.00000 0.03519 0.02599 0.05458 -0.00485 -0.00821 -0.00912 0.03827 0.00814 0.00046 0.00045 0.00026 0.00000 0.00314 0.00315 0.00361 0.00269 0.00263 0.00239 0.00140 O2B 0.42896 1.67474 0.09384 1.00000 0.07715 0.04537 0.05373 -0.00370 -0.03166 -0.00888 0.05749 0.00988 0.00062 0.00054 0.00030 0.00000 0.00472 0.00386 0.00416 0.00307 0.00369 0.00320 0.00178 C21 0.43585 1.18862 0.18575 1.00000 0.05985 0.04802 0.06176 -0.00701 0.01175 0.00301 0.05723 0.01727 0.00092 0.00084 0.00047 0.00000 0.00631 0.00595 0.00640 0.00483 0.00496 0.00465 0.00259 H21A 0.44506 1.23388 0.14513 1.00000 0.08585 0.00000 0.00000 H21B 0.49372 1.21822 0.21232 1.00000 0.08585 0.00000 0.00000 H21C 0.35435 1.19894 0.20402 1.00000 0.08585 0.00000 0.00000 C22 0.45844 1.05504 0.17916 1.00000 0.04039 0.03346 0.03792 -0.01071 -0.00284 0.00177 0.03679 0.01286 0.00072 0.00071 0.00037 0.00000 0.00487 0.00468 0.00492 0.00380 0.00379 0.00370 0.00200 C23 0.59110 1.04556 0.15663 1.00000 0.03482 0.03325 0.02931 -0.00226 0.00114 -0.01140 0.03267 0.01226 0.00067 0.00069 0.00035 0.00000 0.00456 0.00456 0.00441 0.00352 0.00350 0.00345 0.00186 H23A 0.60612 1.11071 0.12311 1.00000 0.03921 0.00000 0.00000 H23B 0.63768 1.06633 0.19089 1.00000 0.03921 0.00000 0.00000 C24 0.64935 0.93390 0.13339 1.00000 0.02883 0.03491 0.02957 -0.00044 -0.00369 -0.00829 0.03119 0.01188 0.00066 0.00069 0.00034 0.00000 0.00429 0.00463 0.00439 0.00354 0.00338 0.00344 0.00184 C26 0.43289 0.98798 0.24372 1.00000 0.04736 0.05823 0.04836 0.00234 0.01397 0.00306 0.05266 0.01694 0.00084 0.00088 0.00041 0.00000 0.00558 0.00610 0.00573 0.00465 0.00442 0.00449 0.00245 H26A 0.35352 1.01024 0.26083 1.00000 0.07899 0.00000 0.00000 H26B 0.49385 1.00979 0.27067 1.00000 0.07899 0.00000 0.00000 H26C 0.43510 0.90134 0.24061 1.00000 0.07899 0.00000 0.00000 C27 0.37362 1.01416 0.13399 1.00000 0.03073 0.07168 0.08642 -0.03334 -0.00238 0.00552 0.06138 0.01520 0.00079 0.00098 0.00051 0.00000 0.00508 0.00701 0.00769 0.00589 0.00488 0.00457 0.00285 H27A 0.39243 1.05742 0.09340 1.00000 0.09207 0.00000 0.00000 H27B 0.29081 1.03085 0.14832 1.00000 0.09207 0.00000 0.00000 H27C 0.38299 0.92788 0.13116 1.00000 0.09207 0.00000 0.00000 C28 0.78585 0.95500 0.12571 1.00000 0.02617 0.04443 0.03887 -0.00844 -0.00356 -0.00697 0.03614 0.01250 0.00066 0.00076 0.00038 0.00000 0.00432 0.00504 0.00482 0.00391 0.00356 0.00358 0.00196 H28A 0.81596 0.96411 0.16592 1.00000 0.05421 0.00000 0.00000 H28B 0.80361 1.02792 0.09815 1.00000 0.05421 0.00000 0.00000 H28C 0.82482 0.88638 0.10817 1.00000 0.05421 0.00000 0.00000 C29 0.62185 0.81668 0.17217 1.00000 0.03995 0.03364 0.03818 -0.00472 -0.00088 -0.00073 0.03727 0.01330 0.00074 0.00070 0.00037 0.00000 0.00486 0.00469 0.00484 0.00374 0.00379 0.00365 0.00197 H29A 0.64173 0.82399 0.21449 1.00000 0.05591 0.00000 0.00000 H29B 0.66956 0.75254 0.15526 1.00000 0.05591 0.00000 0.00000 H29C 0.53644 0.79764 0.17187 1.00000 0.05591 0.00000 0.00000 N25 0.61298 0.91641 0.06907 1.00000 0.02753 0.03273 0.03183 -0.00261 -0.00251 -0.00916 0.03070 0.00938 0.00054 0.00055 0.00027 0.00000 0.00343 0.00372 0.00371 0.00289 0.00277 0.00277 0.00152 H25A 0.66314 0.86297 0.05182 1.00000 0.04605 0.00000 0.00000 H25B 0.61765 0.98782 0.04544 1.00000 0.04605 0.00000 0.00000 H25C 0.53644 0.88801 0.07156 1.00000 0.04605 0.00000 0.00000 C31 0.72071 0.66010 0.49076 1.00000 0.03052 0.02446 0.03352 -0.00419 -0.00590 -0.01038 0.02923 0.01179 0.00067 0.00066 0.00035 0.00000 0.00458 0.00418 0.00456 0.00370 0.00352 0.00341 0.00181 C32 0.83246 0.62761 0.45120 1.00000 0.02798 0.03412 0.05033 -0.00383 -0.00343 -0.00805 0.03746 0.01364 0.00069 0.00072 0.00041 0.00000 0.00470 0.00474 0.00569 0.00427 0.00395 0.00356 0.00204 C33 1.04370 0.62511 0.44191 1.00000 0.03501 0.02836 0.05836 -0.00692 0.00003 -0.00252 0.04057 0.01388 0.00072 0.00072 0.00042 0.00000 0.00483 0.00459 0.00561 0.00404 0.00407 0.00360 0.00209 H33A 1.04179 0.53865 0.43834 1.00000 0.06085 0.00000 0.00000 H33B 1.11130 0.64432 0.46535 1.00000 0.06085 0.00000 0.00000 H33C 1.05300 0.66829 0.40076 1.00000 0.06085 0.00000 0.00000 O31A 0.62461 0.60996 0.47945 1.00000 0.03394 0.03727 0.04156 -0.00697 -0.00357 -0.00976 0.03734 0.00825 0.00046 0.00047 0.00024 0.00000 0.00325 0.00322 0.00331 0.00257 0.00250 0.00257 0.00137 O31B 0.73233 0.73245 0.52967 1.00000 0.03241 0.04527 0.04540 -0.01682 -0.00227 -0.01177 0.04024 0.00833 0.00046 0.00050 0.00025 0.00000 0.00315 0.00349 0.00346 0.00297 0.00257 0.00253 0.00143 O32A 0.83052 0.57671 0.40513 1.00000 0.04474 0.10163 0.06104 -0.05119 -0.00623 -0.00036 0.06622 0.01021 0.00056 0.00069 0.00032 0.00000 0.00393 0.00569 0.00439 0.00435 0.00321 0.00359 0.00206 O32B 0.93279 0.66069 0.47337 1.00000 0.02548 0.03424 0.05106 -0.01330 -0.00185 -0.00804 0.03637 0.00793 0.00044 0.00046 0.00025 0.00000 0.00306 0.00311 0.00353 0.00263 0.00255 0.00234 0.00136 C41 0.66314 0.40712 0.71362 1.00000 0.07450 0.05309 0.06384 -0.00496 -0.04291 0.01056 0.06200 0.01544 0.00096 0.00090 0.00047 0.00000 0.00714 0.00620 0.00662 0.00505 0.00558 0.00512 0.00287 H41A 0.73146 0.46256 0.70623 1.00000 0.09300 0.00000 0.00000 H41B 0.69123 0.32482 0.71090 1.00000 0.09300 0.00000 0.00000 H41C 0.62440 0.41421 0.75469 1.00000 0.09300 0.00000 0.00000 C42 0.57112 0.43864 0.66422 1.00000 0.04133 0.03221 0.03855 0.00389 -0.01326 -0.00321 0.03732 0.01282 0.00072 0.00071 0.00037 0.00000 0.00491 0.00472 0.00498 0.00377 0.00389 0.00370 0.00203 C43 0.54957 0.57295 0.66066 1.00000 0.03558 0.04400 0.03798 -0.00575 -0.00909 -0.00598 0.03875 0.01277 0.00072 0.00074 0.00039 0.00000 0.00474 0.00525 0.00484 0.00394 0.00377 0.00381 0.00203 H43A 0.62203 0.61093 0.63837 1.00000 0.04650 0.00000 0.00000 H43B 0.54904 0.59489 0.70339 1.00000 0.04650 0.00000 0.00000 C44 0.44330 0.63677 0.63302 1.00000 0.03946 0.03022 0.02347 -0.00678 -0.00172 -0.00052 0.03081 0.01203 0.00069 0.00067 0.00033 0.00000 0.00465 0.00439 0.00424 0.00341 0.00348 0.00349 0.00184 C46 0.45839 0.36106 0.68439 1.00000 0.06028 0.04234 0.05239 0.00181 -0.00250 -0.00521 0.05215 0.01550 0.00086 0.00082 0.00044 0.00000 0.00618 0.00543 0.00586 0.00445 0.00470 0.00446 0.00240 H46A 0.42256 0.38445 0.72362 1.00000 0.07823 0.00000 0.00000 H46B 0.48093 0.27636 0.68928 1.00000 0.07823 0.00000 0.00000 H46C 0.40021 0.37319 0.65306 1.00000 0.07823 0.00000 0.00000 C47 0.62793 0.39853 0.60321 1.00000 0.04698 0.03081 0.05490 -0.00486 -0.01048 -0.00618 0.04384 0.01341 0.00078 0.00074 0.00040 0.00000 0.00529 0.00474 0.00577 0.00409 0.00432 0.00385 0.00219 H47A 0.56796 0.40284 0.57264 1.00000 0.06577 0.00000 0.00000 H47B 0.65626 0.31591 0.61006 1.00000 0.06577 0.00000 0.00000 H47C 0.69563 0.45140 0.58819 1.00000 0.06577 0.00000 0.00000 C48 0.32407 0.61234 0.66946 1.00000 0.04345 0.03948 0.04039 -0.00858 0.00421 -0.00131 0.04116 0.01380 0.00074 0.00076 0.00038 0.00000 0.00514 0.00500 0.00503 0.00399 0.00396 0.00390 0.00208 H48A 0.33258 0.62315 0.71280 1.00000 0.06173 0.00000 0.00000 H48B 0.29853 0.52986 0.66583 1.00000 0.06173 0.00000 0.00000 H48C 0.26398 0.66819 0.65332 1.00000 0.06173 0.00000 0.00000 C49 0.47031 0.77232 0.62716 1.00000 0.04292 0.02053 0.04253 -0.00686 -0.00680 -0.00020 0.03490 0.01240 0.00074 0.00064 0.00038 0.00000 0.00482 0.00416 0.00492 0.00354 0.00379 0.00343 0.00191 H49A 0.40026 0.81648 0.61302 1.00000 0.05235 0.00000 0.00000 H49B 0.53920 0.79018 0.59743 1.00000 0.05235 0.00000 0.00000 H49C 0.48863 0.79651 0.66729 1.00000 0.05235 0.00000 0.00000 N45 0.42597 0.60960 0.56771 1.00000 0.02805 0.02632 0.03669 -0.00302 -0.00459 -0.00353 0.03024 0.00956 0.00055 0.00055 0.00028 0.00000 0.00374 0.00379 0.00393 0.00293 0.00311 0.00294 0.00155 H45A 0.49751 0.61628 0.54503 1.00000 0.06888 0.00000 0.03199 H45B 0.37308 0.66252 0.55082 1.00000 0.03392 0.00000 0.02184 H45C 0.39691 0.53371 0.56810 1.00000 0.03337 0.00000 0.02144 C51 0.33007 0.89827 0.45506 1.00000 0.03000 0.03333 0.04087 -0.00833 0.00066 -0.00415 0.03458 0.01253 0.00069 0.00073 0.00040 0.00000 0.00481 0.00475 0.00532 0.00427 0.00383 0.00363 0.00195 C52 0.22286 0.84881 0.49936 1.00000 0.02801 0.02820 0.04010 -0.00676 -0.00386 -0.00346 0.03181 0.01187 0.00068 0.00072 0.00037 0.00000 0.00466 0.00473 0.00499 0.00407 0.00368 0.00371 0.00189 C53 0.54053 0.89843 0.43587 1.00000 0.03520 0.03436 0.06441 -0.00325 0.00244 -0.01553 0.04504 0.01394 0.00074 0.00076 0.00043 0.00000 0.00491 0.00493 0.00615 0.00437 0.00429 0.00382 0.00226 H53A 0.53940 0.86666 0.39576 1.00000 0.06756 0.00000 0.00000 H53B 0.61226 0.86995 0.45579 1.00000 0.06756 0.00000 0.00000 H53C 0.54160 0.98623 0.43018 1.00000 0.06756 0.00000 0.00000 O51A 0.43388 0.85742 0.47438 1.00000 0.03034 0.02966 0.04271 -0.00184 0.00281 -0.00258 0.03461 0.00836 0.00045 0.00044 0.00024 0.00000 0.00319 0.00298 0.00327 0.00247 0.00250 0.00237 0.00132 O51B 0.31868 0.96377 0.40869 1.00000 0.04482 0.05924 0.04475 0.01731 0.00132 -0.00906 0.05126 0.01031 0.00052 0.00058 0.00029 0.00000 0.00367 0.00412 0.00386 0.00342 0.00290 0.00295 0.00163 O52A 0.13020 0.90954 0.49359 1.00000 0.03443 0.03967 0.04086 0.00737 -0.00133 -0.00297 0.03911 0.00900 0.00048 0.00049 0.00025 0.00000 0.00334 0.00328 0.00334 0.00258 0.00252 0.00270 0.00139 O52B 0.23800 0.75686 0.53337 1.00000 0.03761 0.03712 0.04178 0.00487 -0.00233 0.00030 0.03942 0.00888 0.00047 0.00050 0.00025 0.00000 0.00328 0.00352 0.00340 0.00292 0.00259 0.00253 0.00140 C61 0.98335 0.34855 0.78453 1.00000 0.05283 0.07300 0.06844 -0.03364 -0.01396 -0.01352 0.06254 0.01410 0.00089 0.00097 0.00048 0.00000 0.00607 0.00713 0.00695 0.00570 0.00513 0.00508 0.00287 H61A 1.03950 0.28275 0.79265 1.00000 0.09381 0.00000 0.00000 H61B 1.00354 0.38907 0.74342 1.00000 0.09381 0.00000 0.00000 H61C 0.90154 0.31648 0.78674 1.00000 0.09381 0.00000 0.00000 C62 0.99197 0.43864 0.83288 1.00000 0.04269 0.03096 0.03904 -0.01384 -0.01533 -0.00935 0.03627 0.01141 0.00072 0.00069 0.00037 0.00000 0.00494 0.00460 0.00489 0.00379 0.00391 0.00372 0.00201 C63 1.12721 0.46399 0.83665 1.00000 0.03928 0.03780 0.04158 -0.00882 0.00052 -0.00672 0.03940 0.01268 0.00073 0.00074 0.00039 0.00000 0.00488 0.00494 0.00510 0.00394 0.00387 0.00379 0.00206 H63A 1.16026 0.39040 0.85764 1.00000 0.04727 0.00000 0.00000 H63B 1.16298 0.46997 0.79377 1.00000 0.04727 0.00000 0.00000 C64 1.18026 0.56992 0.86651 1.00000 0.02984 0.03267 0.03077 -0.00541 0.00026 0.00033 0.03106 0.01229 0.00066 0.00068 0.00034 0.00000 0.00434 0.00452 0.00450 0.00353 0.00343 0.00341 0.00184 C66 0.91966 0.54951 0.81445 1.00000 0.04735 0.05911 0.05036 -0.00790 -0.01095 -0.00892 0.05173 0.01464 0.00082 0.00085 0.00043 0.00000 0.00549 0.00618 0.00574 0.00473 0.00439 0.00458 0.00240 H66A 0.95566 0.58974 0.77579 1.00000 0.07760 0.00000 0.00000 H66B 0.91961 0.60434 0.84672 1.00000 0.07760 0.00000 0.00000 H66C 0.83711 0.52592 0.80896 1.00000 0.07760 0.00000 0.00000 C67 0.93588 0.37918 0.89436 1.00000 0.04305 0.05002 0.06471 -0.01618 -0.00503 -0.01897 0.05184 0.01377 0.00081 0.00084 0.00043 0.00000 0.00531 0.00579 0.00646 0.00486 0.00458 0.00428 0.00244 H67A 0.85771 0.34481 0.88812 1.00000 0.07776 0.00000 0.00000 H67B 0.92550 0.43928 0.92397 1.00000 0.07776 0.00000 0.00000 H67C 0.98864 0.31550 0.91024 1.00000 0.07776 0.00000 0.00000 C68 1.16156 0.69320 0.83131 1.00000 0.04973 0.03715 0.03410 -0.00150 0.00119 -0.00625 0.04066 0.01381 0.00079 0.00073 0.00037 0.00000 0.00529 0.00496 0.00477 0.00382 0.00393 0.00392 0.00207 H68A 1.20701 0.75416 0.84922 1.00000 0.06099 0.00000 0.00000 H68B 1.07617 0.71318 0.83429 1.00000 0.06099 0.00000 0.00000 H68C 1.18958 0.69080 0.78801 1.00000 0.06099 0.00000 0.00000 C69 1.31352 0.54465 0.87001 1.00000 0.03351 0.03560 0.04432 -0.00575 0.00797 -0.00057 0.03822 0.01378 0.00069 0.00074 0.00039 0.00000 0.00466 0.00479 0.00504 0.00385 0.00375 0.00358 0.00200 H69A 1.35105 0.60897 0.88934 1.00000 0.05733 0.00000 0.00000 H69B 1.35113 0.54071 0.82843 1.00000 0.05733 0.00000 0.00000 H69C 1.32410 0.46803 0.89450 1.00000 0.05733 0.00000 0.00000 N65 1.13115 0.57697 0.93182 1.00000 0.02809 0.02848 0.03939 -0.00255 0.00192 -0.01098 0.03224 0.00983 0.00055 0.00056 0.00028 0.00000 0.00351 0.00364 0.00397 0.00294 0.00289 0.00275 0.00155 H65A 1.17236 0.63364 0.94895 1.00000 0.04836 0.00000 0.00000 H65B 1.13912 0.50457 0.95371 1.00000 0.04836 0.00000 0.00000 H65C 1.05227 0.59698 0.93231 1.00000 0.04836 0.00000 0.00000 C71 -0.11380 0.83375 0.95119 1.00000 0.03259 0.03089 0.03574 -0.00600 0.00952 -0.00346 0.03348 0.01273 0.00070 0.00070 0.00038 0.00000 0.00455 0.00488 0.00508 0.00384 0.00395 0.00360 0.00192 C72 -0.16096 0.71815 0.99089 1.00000 0.02900 0.02640 0.04082 -0.01010 0.00392 -0.00642 0.03195 0.01214 0.00070 0.00069 0.00038 0.00000 0.00447 0.00472 0.00501 0.00373 0.00399 0.00369 0.00188 C73 -0.10763 1.04573 0.94285 1.00000 0.03656 0.03096 0.05500 0.00545 -0.00047 -0.00465 0.04159 0.01433 0.00075 0.00072 0.00042 0.00000 0.00477 0.00477 0.00562 0.00404 0.00404 0.00370 0.00212 H73A -0.01996 1.04359 0.93746 1.00000 0.06239 0.00000 0.00000 H73B -0.13232 1.11143 0.96735 1.00000 0.06239 0.00000 0.00000 H73C -0.14057 1.05837 0.90251 1.00000 0.06239 0.00000 0.00000 O71A -0.15249 0.93189 0.97456 1.00000 0.03529 0.02144 0.04714 0.00250 0.00525 -0.00559 0.03540 0.00850 0.00046 0.00044 0.00024 0.00000 0.00306 0.00300 0.00341 0.00254 0.00253 0.00235 0.00135 O71B -0.05272 0.83226 0.90565 1.00000 0.10234 0.03729 0.07302 -0.00843 0.03834 -0.00695 0.07288 0.01279 0.00073 0.00056 0.00035 0.00000 0.00590 0.00394 0.00511 0.00348 0.00467 0.00367 0.00226 O72A -0.24282 0.72956 1.02997 1.00000 0.04084 0.03085 0.05087 -0.00769 0.00519 -0.01045 0.04102 0.00856 0.00050 0.00047 0.00027 0.00000 0.00347 0.00320 0.00366 0.00267 0.00304 0.00254 0.00144 O72B -0.10516 0.62529 0.97976 1.00000 0.03185 0.03072 0.04705 -0.00583 0.00044 -0.00513 0.03656 0.00831 0.00046 0.00047 0.00025 0.00000 0.00302 0.00329 0.00348 0.00261 0.00250 0.00255 0.00136 C81 -0.01125 0.99098 0.74379 1.00000 0.05900 0.04670 0.05969 -0.02366 -0.00728 -0.00471 0.05379 0.01453 0.00087 0.00085 0.00044 0.00000 0.00609 0.00572 0.00626 0.00479 0.00487 0.00450 0.00248 H81A 0.00319 1.06923 0.75847 1.00000 0.08068 0.00000 0.00000 H81B 0.01671 0.92743 0.77316 1.00000 0.08068 0.00000 0.00000 H81C -0.09724 0.98057 0.73993 1.00000 0.08068 0.00000 0.00000 C82 0.05748 0.98424 0.68042 1.00000 0.05073 0.03761 0.04452 -0.01045 -0.02083 -0.01401 0.04300 0.01205 0.00078 0.00075 0.00039 0.00000 0.00547 0.00509 0.00531 0.00416 0.00428 0.00404 0.00223 C83 0.05053 0.85767 0.65843 1.00000 0.02893 0.03746 0.03041 0.00172 -0.00422 -0.00345 0.03248 0.01200 0.00066 0.00069 0.00036 0.00000 0.00435 0.00473 0.00445 0.00362 0.00342 0.00346 0.00187 H83A 0.11603 0.85393 0.62577 1.00000 0.03898 0.00000 0.00000 H83B 0.07220 0.80114 0.69337 1.00000 0.03898 0.00000 0.00000 C84 -0.06053 0.80384 0.63386 1.00000 0.03274 0.03562 0.03494 -0.00916 0.00142 -0.00989 0.03425 0.01216 0.00068 0.00071 0.00036 0.00000 0.00453 0.00473 0.00477 0.00373 0.00361 0.00355 0.00194 C86 0.19170 1.00281 0.68978 1.00000 0.04192 0.06190 0.06521 -0.01210 -0.01390 -0.01547 0.05546 0.01409 0.00079 0.00091 0.00047 0.00000 0.00541 0.00646 0.00646 0.00515 0.00467 0.00456 0.00257 H86A 0.23919 0.99704 0.65079 1.00000 0.08318 0.00000 0.00000 H86B 0.21750 0.94100 0.72070 1.00000 0.08318 0.00000 0.00000 H86C 0.20343 1.08216 0.70378 1.00000 0.08318 0.00000 0.00000 C87 0.01638 1.07996 0.63473 1.00000 0.09951 0.03555 0.07256 0.00269 -0.03450 -0.03365 0.06830 0.01484 0.00107 0.00083 0.00050 0.00000 0.00855 0.00556 0.00715 0.00503 0.00631 0.00540 0.00322 H87A 0.05334 1.06824 0.59380 1.00000 0.10245 0.00000 0.00000 H87B 0.03982 1.15857 0.64618 1.00000 0.10245 0.00000 0.00000 H87C -0.07102 1.07595 0.63419 1.00000 0.10245 0.00000 0.00000 C88 -0.17719 0.81568 0.67379 1.00000 0.02894 0.03547 0.04567 -0.00895 -0.00832 -0.00144 0.03609 0.01256 0.00067 0.00073 0.00038 0.00000 0.00441 0.00466 0.00505 0.00385 0.00372 0.00348 0.00195 H88A -0.19824 0.90055 0.67396 1.00000 0.05413 0.00000 0.00000 H88B -0.16649 0.78157 0.71591 1.00000 0.05413 0.00000 0.00000 H88C -0.24157 0.77251 0.65706 1.00000 0.05413 0.00000 0.00000 C89 -0.03578 0.67245 0.62631 1.00000 0.04577 0.03165 0.03615 -0.00277 -0.00996 0.00255 0.03755 0.01287 0.00076 0.00069 0.00037 0.00000 0.00510 0.00470 0.00478 0.00370 0.00387 0.00374 0.00199 H89A -0.01912 0.63066 0.66613 1.00000 0.05632 0.00000 0.00000 H89B 0.03368 0.66599 0.59689 1.00000 0.05632 0.00000 0.00000 H89C -0.10597 0.63601 0.61105 1.00000 0.05632 0.00000 0.00000 N85 -0.07943 0.86305 0.57003 1.00000 0.02819 0.03270 0.03402 -0.00678 -0.00594 -0.00344 0.03122 0.00964 0.00054 0.00055 0.00027 0.00000 0.00354 0.00370 0.00380 0.00295 0.00280 0.00278 0.00152 H85A -0.11166 0.93700 0.57312 1.00000 0.04684 0.00000 0.00000 H85B -0.13015 0.81733 0.55129 1.00000 0.04684 0.00000 0.00000 H85C -0.00782 0.87031 0.54744 1.00000 0.04684 0.00000 0.00000 Final Structure Factor Calculation for ssf1327 in P-1 Total number of l.s. parameters = 610 Maximum vector length = 511 Memory required = 9153 / 22995 wR2 = 0.2715 before cycle 5 for 6612 data and 0 / 610 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1222 * P )^2 + 10.98 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0988 for 4985 Fo > 4sig(Fo) and 0.1253 for all 6612 data wR2 = 0.2715, GooF = S = 1.050, Restrained GooF = 1.050 for all data Occupancy sum of asymmetric unit = 64.00 for non-hydrogen and 92.00 for hydrogen atoms Principal mean square atomic displacements U 0.0463 0.0349 0.0317 C1 0.0459 0.0419 0.0300 C2 0.0752 0.0416 0.0278 C3 0.0573 0.0417 0.0191 O1A 0.0607 0.0382 0.0205 O1B 0.0556 0.0400 0.0192 O2A 0.0952 0.0459 0.0314 O2B 0.0785 0.0504 0.0428 C21 0.0428 0.0403 0.0272 C22 0.0460 0.0300 0.0220 C23 0.0418 0.0289 0.0229 C24 0.0724 0.0541 0.0315 C26 0.1036 0.0509 0.0297 C27 0.0483 0.0373 0.0228 C28 0.0416 0.0371 0.0331 C29 0.0399 0.0318 0.0204 N25 0.0394 0.0331 0.0152 C31 0.0504 0.0399 0.0221 C32 0.0593 0.0354 0.0270 C33 0.0465 0.0411 0.0244 O31A 0.0603 0.0387 0.0218 O31B 0.1255 0.0453 0.0279 O32A 0.0552 0.0347 0.0192 O32B 0.1051 0.0540 0.0269 C41 0.0531 0.0322 0.0267 C42 0.0477 0.0417 0.0269 C43 0.0397 0.0318 0.0210 C44 0.0619 0.0559 0.0387 C46 0.0588 0.0450 0.0277 C47 0.0511 0.0393 0.0330 C48 0.0462 0.0391 0.0193 C49 0.0372 0.0305 0.0230 N45 0.0447 0.0322 0.0269 C51 0.0408 0.0315 0.0232 C52 0.0661 0.0499 0.0191 C53 0.0453 0.0321 0.0263 O51A 0.0782 0.0485 0.0271 O51B 0.0527 0.0359 0.0287 O52A 0.0494 0.0376 0.0312 O52B 0.0961 0.0646 0.0269 C61 0.0527 0.0434 0.0128 C62 0.0497 0.0376 0.0308 C63 0.0346 0.0314 0.0272 C64 0.0644 0.0546 0.0361 C66 0.0731 0.0587 0.0238 C67 0.0531 0.0375 0.0313 C68 0.0519 0.0353 0.0274 C69 0.0423 0.0373 0.0171 N65 0.0480 0.0296 0.0229 C71 0.0474 0.0279 0.0205 C72 0.0595 0.0391 0.0261 C73 0.0526 0.0356 0.0180 O71A 0.1384 0.0437 0.0365 O71B 0.0587 0.0402 0.0241 O72A 0.0484 0.0354 0.0259 O72B 0.0714 0.0603 0.0297 C81 0.0668 0.0464 0.0158 C82 0.0418 0.0284 0.0273 C83 0.0479 0.0313 0.0235 C84 0.0708 0.0682 0.0274 C86 0.1293 0.0564 0.0191 C87 0.0481 0.0349 0.0252 C88 0.0490 0.0333 0.0304 C89 0.0367 0.0340 0.0229 N85 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.028 0.042 0.056 0.071 0.087 0.107 0.132 0.168 0.238 1.000 Number in group 665. 666. 660. 661. 668. 655. 657. 656. 661. 663. GooF 1.169 1.110 1.039 1.064 1.009 0.968 1.019 1.039 0.990 1.078 K 3.136 1.612 1.265 1.230 1.099 1.095 1.075 1.045 0.985 1.023 Resolution(A) 0.95 0.98 1.02 1.07 1.12 1.20 1.29 1.41 1.60 2.02 inf Number in group 680. 667. 642. 660. 661. 662. 660. 656. 663. 661. GooF 0.846 0.833 0.885 0.890 1.008 0.892 0.969 0.911 1.339 1.633 K 1.077 1.043 1.067 1.028 1.018 1.017 1.002 1.000 0.994 1.070 R1 0.206 0.179 0.172 0.131 0.136 0.112 0.113 0.098 0.094 0.095 Recommended weighting scheme: WGHT 0.1221 10.9851 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 4 1 748.94 22.78 6.73 0.037 2.50 -1 3 5 452.63 20.63 5.80 0.035 2.84 -1 -5 1 285.06 23.37 5.56 0.037 2.15 -2 -3 4 265.52 36.19 5.55 0.046 2.56 3 3 3 861.91 311.56 5.48 0.135 2.57 -1 -2 3 1322.84 533.58 5.24 0.177 3.89 0 8 2 834.88 302.73 5.17 0.133 1.40 -1 2 5 454.36 73.01 5.11 0.065 3.37 -5 4 2 184.29 704.23 5.07 0.203 1.73 -4 2 1 837.21 319.57 5.02 0.137 2.48 -5 -1 4 147.62 2.58 4.98 0.012 1.97 4 1 4 165.87 12.16 4.93 0.027 2.52 -2 1 1 1357.85 3037.78 4.82 0.422 4.85 -5 -1 1 217.28 4.53 4.76 0.016 2.16 -4 5 3 494.73 172.02 4.56 0.100 1.71 3 3 9 587.51 226.01 4.53 0.115 1.89 3 1 6 391.74 118.23 4.53 0.083 2.66 2 2 3 482.25 153.30 4.44 0.095 3.64 -2 -1 3 1218.56 527.04 4.43 0.176 3.91 2 4 7 266.94 68.15 4.36 0.063 2.07 1 4 9 158.75 13.14 4.34 0.028 1.91 4 -3 2 303.23 91.01 4.24 0.073 2.19 0 8 7 140.24 7.09 4.22 0.020 1.32 -1 -5 4 148.51 1.02 4.18 0.008 1.96 1 4 4 252.58 67.96 4.10 0.063 2.53 -4 5 4 124.20 8.60 4.02 0.022 1.68 -6 1 3 99.44 387.37 4.02 0.151 1.76 4 -1 9 394.17 150.04 3.96 0.094 1.85 2 2 2 11242.53 6828.20 3.95 0.632 3.85 4 -5 1 125.39 443.96 3.88 0.161 1.74 0 -6 5 852.37 410.81 3.88 0.155 1.65 -2 -3 3 185.52 43.24 3.86 0.050 2.72 5 4 2 809.47 405.92 3.79 0.154 1.75 1 -5 1 828.89 418.42 3.79 0.156 2.16 -4 -2 10 111.20 5.56 3.71 0.018 1.56 4 5 4 1339.44 747.92 3.70 0.209 1.72 2 4 3 811.58 399.50 3.69 0.153 2.44 3 6 0 150.57 19.20 3.66 0.034 1.66 -3 3 0 215.35 33.45 3.64 0.044 2.64 2 9 1 190.58 36.16 3.63 0.046 1.21 8 0 3 106.47 2.84 3.61 0.013 1.39 -5 1 0 871.85 415.09 3.60 0.156 2.19 8 5 6 161.29 30.39 3.55 0.042 1.16 1 -1 3 26717.99 17094.08 3.47 1.000 5.30 2 4 2 11966.60 7565.20 3.47 0.665 2.49 0 8 3 116.58 17.51 3.45 0.032 1.39 10 1 6 25.54 181.86 3.43 0.103 1.09 1 -4 1 246.71 599.92 3.43 0.187 2.66 8 -1 2 -20.30 110.36 3.42 0.080 1.38 2 7 2 566.32 282.21 3.41 0.128 1.54 Bond lengths and angles C1 - Distance Angles O1B 1.2431 (0.0096) O1A 1.2711 (0.0096) 127.26 (0.77) C2 1.5137 (0.0122) 119.06 (0.72) 113.65 (0.74) C1 - O1B O1A C2 - Distance Angles O2B 1.2262 (0.0099) O2A 1.3413 (0.0097) 122.24 (0.77) C1 1.5137 (0.0122) 125.07 (0.75) 112.69 (0.72) C2 - O2B O2A C3 - Distance Angles O2A 1.4261 (0.0101) H3A 0.9800 109.47 H3B 0.9800 109.47 109.47 H3C 0.9800 109.47 109.47 109.47 C3 - O2A H3A H3B O1A - Distance Angles C1 1.2711 (0.0096) O1A - O1B - Distance Angles C1 1.2431 (0.0096) O1B - O2A - Distance Angles C2 1.3413 (0.0097) C3 1.4261 (0.0101) 117.44 (0.65) O2A - C2 O2B - Distance Angles C2 1.2262 (0.0099) O2B - C21 - Distance Angles C22 1.5367 (0.0122) H21A 0.9800 109.47 H21B 0.9800 109.47 109.47 H21C 0.9800 109.47 109.47 109.47 C21 - C22 H21A H21B C22 - Distance Angles C27 1.5213 (0.0125) C23 1.5365 (0.0111) 113.00 (0.67) C21 1.5367 (0.0122) 108.20 (0.76) 106.00 (0.67) C26 1.5442 (0.0120) 111.24 (0.77) 111.22 (0.68) 106.81 (0.70) C22 - C27 C23 C21 C23 - Distance Angles C24 1.5238 (0.0111) C22 1.5365 (0.0111) 124.77 (0.63) H23A 0.9900 106.13 106.13 H23B 0.9900 106.13 106.13 106.34 C23 - C24 C22 H23A C24 - Distance Angles C29 1.5138 (0.0110) C23 1.5238 (0.0111) 116.37 (0.64) N25 1.5251 (0.0096) 106.26 (0.59) 110.77 (0.61) C28 1.5403 (0.0105) 109.72 (0.65) 108.05 (0.61) 105.10 (0.58) C24 - C29 C23 N25 C26 - Distance Angles C22 1.5442 (0.0120) H26A 0.9800 109.47 H26B 0.9800 109.47 109.47 H26C 0.9800 109.47 109.47 109.47 C26 - C22 H26A H26B C27 - Distance Angles C22 1.5213 (0.0125) H27A 0.9800 109.47 H27B 0.9800 109.47 109.47 H27C 0.9800 109.47 109.47 109.47 C27 - C22 H27A H27B C28 - Distance Angles C24 1.5403 (0.0105) H28A 0.9800 109.47 H28B 0.9800 109.47 109.47 H28C 0.9800 109.47 109.47 109.47 C28 - C24 H28A H28B C29 - Distance Angles C24 1.5138 (0.0110) H29A 0.9800 109.47 H29B 0.9800 109.47 109.47 H29C 0.9800 109.47 109.47 109.47 C29 - C24 H29A H29B N25 - Distance Angles C24 1.5251 (0.0096) H25A 0.9100 109.47 H25B 0.9100 109.47 109.47 H25C 0.9100 109.47 109.47 109.47 N25 - C24 H25A H25B C31 - Distance Angles O31B 1.2448 (0.0087) O31A 1.2650 (0.0087) 126.73 (0.71) C32 1.5324 (0.0114) 118.08 (0.65) 115.18 (0.66) C31 - O31B O31A C32 - Distance Angles O32A 1.2072 (0.0098) O32B 1.3223 (0.0094) 123.13 (0.75) C31 1.5324 (0.0114) 124.44 (0.71) 112.43 (0.70) C32 - O32A O32B C33 - Distance Angles O32B 1.4494 (0.0096) H33A 0.9800 109.47 H33B 0.9800 109.47 109.47 H33C 0.9800 109.47 109.47 109.47 C33 - O32B H33A H33B O31A - Distance Angles C31 1.2650 (0.0088) O31A - O31B - Distance Angles C31 1.2448 (0.0087) O31B - O32A - Distance Angles C32 1.2072 (0.0098) O32A - O32B - Distance Angles C32 1.3223 (0.0095) C33 1.4494 (0.0096) 116.49 (0.63) O32B - C32 C41 - Distance Angles C42 1.5636 (0.0116) H41A 0.9800 109.47 H41B 0.9800 109.47 109.47 H41C 0.9800 109.47 109.47 109.47 C41 - C42 H41A H41B C42 - Distance Angles C43 1.5198 (0.0116) C47 1.5436 (0.0119) 112.39 (0.68) C46 1.5458 (0.0121) 114.43 (0.71) 108.72 (0.68) C41 1.5636 (0.0116) 107.88 (0.67) 106.50 (0.73) 106.47 (0.73) C42 - C43 C47 C46 C43 - Distance Angles C42 1.5198 (0.0116) C44 1.5208 (0.0112) 125.24 (0.66) H43A 0.9900 106.01 106.01 H43B 0.9900 106.01 106.01 106.29 C43 - C42 C44 H43A C44 - Distance Angles C48 1.5150 (0.0112) N45 1.5169 (0.0095) 106.62 (0.61) C43 1.5208 (0.0112) 114.80 (0.67) 113.82 (0.61) C49 1.5407 (0.0107) 109.37 (0.63) 104.16 (0.60) 107.50 (0.63) C44 - C48 N45 C43 C46 - Distance Angles C42 1.5458 (0.0121) H46A 0.9800 109.47 H46B 0.9800 109.47 109.47 H46C 0.9800 109.47 109.47 109.47 C46 - C42 H46A H46B C47 - Distance Angles C42 1.5436 (0.0119) H47A 0.9800 109.47 H47B 0.9800 109.47 109.47 H47C 0.9800 109.47 109.47 109.47 C47 - C42 H47A H47B C48 - Distance Angles C44 1.5150 (0.0112) H48A 0.9800 109.47 H48B 0.9800 109.47 109.47 H48C 0.9800 109.47 109.47 109.47 C48 - C44 H48A H48B C49 - Distance Angles C44 1.5407 (0.0107) H49A 0.9800 109.47 H49B 0.9800 109.47 109.47 H49C 0.9800 109.47 109.47 109.47 C49 - C44 H49A H49B N45 - Distance Angles C44 1.5169 (0.0095) H45A 0.9100 109.47 H45B 0.9100 109.47 109.47 H45C 0.9100 109.47 109.47 109.47 N45 - C44 H45A H45B C51 - Distance Angles O51B 1.2096 (0.0097) O51A 1.3310 (0.0097) 125.25 (0.72) C52 1.5547 (0.0114) 123.53 (0.74) 111.21 (0.72) C51 - O51B O51A C52 - Distance Angles O52B 1.2316 (0.0093) O52A 1.2471 (0.0094) 129.03 (0.73) C51 1.5547 (0.0114) 118.16 (0.71) 112.79 (0.72) C52 - O52B O52A C53 - Distance Angles O51A 1.4584 (0.0096) H53A 0.9800 109.47 H53B 0.9800 109.47 109.47 H53C 0.9800 109.47 109.47 109.47 C53 - O51A H53A H53B O51A - Distance Angles C51 1.3310 (0.0097) C53 1.4584 (0.0096) 115.62 (0.64) O51A - C51 O51B - Distance Angles C51 1.2096 (0.0097) O51B - O52A - Distance Angles C52 1.2471 (0.0094) O52A - O52B - Distance Angles C52 1.2316 (0.0093) O52B - C61 - Distance Angles C62 1.5396 (0.0115) H61A 0.9800 109.47 H61B 0.9800 109.47 109.47 H61C 0.9800 109.47 109.47 109.47 C61 - C62 H61A H61B C62 - Distance Angles C66 1.5203 (0.0123) C67 1.5355 (0.0124) 108.48 (0.74) C61 1.5396 (0.0115) 109.20 (0.73) 107.63 (0.71) C63 1.5495 (0.0112) 113.87 (0.68) 111.00 (0.67) 106.46 (0.69) C62 - C66 C67 C61 C63 - Distance Angles C64 1.5481 (0.0109) C62 1.5495 (0.0112) 125.55 (0.67) H63A 0.9900 105.93 105.93 H63B 0.9900 105.93 105.93 106.25 C63 - C64 C62 H63A C64 - Distance Angles N65 1.5038 (0.0096) C69 1.5234 (0.0110) 105.63 (0.61) C68 1.5385 (0.0113) 107.28 (0.59) 110.33 (0.64) C63 1.5481 (0.0109) 112.90 (0.60) 106.41 (0.62) 113.98 (0.66) C64 - N65 C69 C68 C66 - Distance Angles C62 1.5203 (0.0123) H66A 0.9800 109.47 H66B 0.9800 109.47 109.47 H66C 0.9800 109.47 109.47 109.47 C66 - C62 H66A H66B C67 - Distance Angles C62 1.5355 (0.0124) H67A 0.9800 109.47 H67B 0.9800 109.47 109.47 H67C 0.9800 109.47 109.47 109.47 C67 - C62 H67A H67B C68 - Distance Angles C64 1.5385 (0.0112) H68A 0.9800 109.47 H68B 0.9800 109.47 109.47 H68C 0.9800 109.47 109.47 109.47 C68 - C64 H68A H68B C69 - Distance Angles C64 1.5234 (0.0110) H69A 0.9800 109.47 H69B 0.9800 109.47 109.47 H69C 0.9800 109.47 109.47 109.47 C69 - C64 H69A H69B N65 - Distance Angles C64 1.5038 (0.0096) H65A 0.9100 109.47 H65B 0.9100 109.47 109.47 H65C 0.9100 109.47 109.47 109.47 N65 - C64 H65A H65B C71 - Distance Angles O71B 1.1689 (0.0095) O71A 1.3167 (0.0093) 124.55 (0.74) C72 1.5596 (0.0112) 123.40 (0.74) 112.05 (0.66) C71 - O71B O71A C72 - Distance Angles O72A 1.2225 (0.0091) O72B 1.2480 (0.0092) 128.30 (0.74) C71 1.5596 (0.0113) 117.38 (0.69) 114.25 (0.69) C72 - O72A O72B C73 - Distance Angles O71A 1.4640 (0.0093) H73A 0.9800 109.47 H73B 0.9800 109.47 109.47 H73C 0.9800 109.47 109.47 109.47 C73 - O71A H73A H73B O71A - Distance Angles C71 1.3167 (0.0093) C73 1.4640 (0.0094) 116.52 (0.61) O71A - C71 O71B - Distance Angles C71 1.1689 (0.0095) O71B - O72A - Distance Angles C72 1.2225 (0.0092) O72A - O72B - Distance Angles C72 1.2480 (0.0092) O72B - C81 - Distance Angles C82 1.5454 (0.0129) H81A 0.9800 109.47 H81B 0.9800 109.47 109.47 H81C 0.9800 109.47 109.47 109.47 C81 - C82 H81A H81B C82 - Distance Angles C87 1.4917 (0.0132) C83 1.5449 (0.0113) 112.86 (0.68) C81 1.5454 (0.0129) 110.59 (0.85) 111.83 (0.70) C86 1.5475 (0.0119) 109.92 (0.77) 104.65 (0.71) 106.64 (0.70) C82 - C87 C83 C81 C83 - Distance Angles C84 1.5359 (0.0106) C82 1.5449 (0.0113) 125.01 (0.67) H83A 0.9900 106.07 106.07 H83B 0.9900 106.07 106.07 106.31 C83 - C84 C82 H83A C84 - Distance Angles N85 1.5183 (0.0101) C89 1.5205 (0.0112) 106.19 (0.60) C88 1.5303 (0.0110) 107.59 (0.63) 109.88 (0.65) C83 1.5359 (0.0106) 109.96 (0.59) 108.08 (0.65) 114.81 (0.63) C84 - N85 C89 C88 C86 - Distance Angles C82 1.5475 (0.0119) H86A 0.9800 109.47 H86B 0.9800 109.47 109.47 H86C 0.9800 109.47 109.47 109.47 C86 - C82 H86A H86B C87 - Distance Angles C82 1.4917 (0.0132) H87A 0.9800 109.47 H87B 0.9800 109.47 109.47 H87C 0.9800 109.47 109.47 109.47 C87 - C82 H87A H87B C88 - Distance Angles C84 1.5303 (0.0110) H88A 0.9800 109.47 H88B 0.9800 109.47 109.47 H88C 0.9800 109.47 109.47 109.47 C88 - C84 H88A H88B C89 - Distance Angles C84 1.5205 (0.0112) H89A 0.9800 109.47 H89B 0.9800 109.47 109.47 H89C 0.9800 109.47 109.47 109.47 C89 - C84 H89A H89B N85 - Distance Angles C84 1.5183 (0.0101) H85A 0.9100 109.47 H85B 0.9100 109.47 109.47 H85C 0.9100 109.47 109.47 109.47 N85 - C84 H85A H85B Selected torsion angles -156.43 ( 0.83) O1B - C1 - C2 - O2B 21.87 ( 1.19) O1A - C1 - C2 - O2B 23.36 ( 1.03) O1B - C1 - C2 - O2A -158.34 ( 0.67) O1A - C1 - C2 - O2A -1.04 ( 1.14) O2B - C2 - O2A - C3 179.16 ( 0.66) C1 - C2 - O2A - C3 -50.91 ( 1.09) C27 - C22 - C23 - C24 -169.25 ( 0.75) C21 - C22 - C23 - C24 75.03 ( 0.96) C26 - C22 - C23 - C24 -46.82 ( 1.04) C22 - C23 - C24 - C29 74.65 ( 0.90) C22 - C23 - C24 - N25 -170.72 ( 0.71) C22 - C23 - C24 - C28 -166.04 ( 0.84) O31B - C31 - C32 - O32A 13.29 ( 1.20) O31A - C31 - C32 - O32A 14.50 ( 1.01) O31B - C31 - C32 - O32B -166.16 ( 0.65) O31A - C31 - C32 - O32B -4.34 ( 1.18) O32A - C32 - O32B - C33 175.12 ( 0.62) C31 - C32 - O32B - C33 81.19 ( 0.97) C47 - C42 - C43 - C44 -43.44 ( 1.12) C46 - C42 - C43 - C44 -161.71 ( 0.81) C41 - C42 - C43 - C44 69.36 ( 1.01) C42 - C43 - C44 - C48 -53.90 ( 1.05) C42 - C43 - C44 - N45 -168.71 ( 0.75) C42 - C43 - C44 - C49 157.75 ( 0.78) O51B - C51 - C52 - O52B -21.14 ( 0.94) O51A - C51 - C52 - O52B -20.59 ( 1.09) O51B - C51 - C52 - O52A 160.53 ( 0.63) O51A - C51 - C52 - O52A 1.03 ( 1.09) O51B - C51 - O51A - C53 179.89 ( 0.61) C52 - C51 - O51A - C53 43.97 ( 1.11) C66 - C62 - C63 - C64 -78.79 ( 0.99) C67 - C62 - C63 - C64 164.36 ( 0.81) C61 - C62 - C63 - C64 54.10 ( 1.04) C62 - C63 - C64 - N65 169.53 ( 0.76) C62 - C63 - C64 - C69 -68.64 ( 1.00) C62 - C63 - C64 - C68 -165.27 ( 0.88) O71B - C71 - C72 - O72A 13.70 ( 1.00) O71A - C71 - C72 - O72A 17.61 ( 1.20) O71B - C71 - C72 - O72B -163.43 ( 0.66) O71A - C71 - C72 - O72B -4.61 ( 1.21) O71B - C71 - O71A - C73 176.44 ( 0.63) C72 - C71 - O71A - C73 -51.19 ( 1.13) C87 - C82 - C83 - C84 74.26 ( 0.99) C81 - C82 - C83 - C84 -170.68 ( 0.75) C86 - C82 - C83 - C84 72.73 ( 0.92) C82 - C83 - C84 - N85 -171.77 ( 0.74) C82 - C83 - C84 - C89 -48.74 ( 1.06) C82 - C83 - C84 - C88 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.91 1.95 2.837(8) 163.6 N45-H45A...O31A 0.91 1.88 2.775(8) 165.4 N45-H45B...O52B 0.91 1.90 2.800(8) 170.2 N85-H85C...O52A 0.91 1.91 2.803(9) 168.3 N25-H25A...O72A_$1 0.91 2.64 3.216(8) 122.1 N25-H25A...O71A_$1 0.91 1.92 2.818(8) 168.1 N25-H25B...O1A_$2 0.91 2.11 2.831(8) 135.3 N25-H25C...O1A_$3 0.91 2.02 2.832(8) 147.2 N45-H45C...O31A_$4 0.91 1.89 2.785(8) 168.8 N65-H65A...O1B_$5 0.91 1.98 2.838(8) 157.7 N65-H65B...O72B_$6 0.91 2.02 2.844(8) 149.9 N65-H65C...O72B_$7 0.91 2.17 2.863(8) 132.5 N85-H85A...O52A_$8 0.91 2.59 3.336(9) 139.7 N85-H85A...O51B_$8 0.91 1.92 2.808(8) 164.2 N85-H85B...O31B_$9 0.91 2.62 3.244(8) 126.0 N85-H85B...O32B_$9 Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 9.5416 (0.0596) x + 0.7218 (0.1462) y + 12.7706 (0.1879) z = 11.6634 (0.1035) * 0.0000 (0.0001) C71 * 0.0000 (0.0001) O71A * 0.0000 (0.0000) O71B Rms deviation of fitted atoms = 0.0000 7.9766 (0.0521) x + 2.8923 (0.1402) y + 15.8652 (0.1735) z = 16.5139 (0.1003) Angle to previous plane (with approximate esd) = 15.75 ( 1.15 ) * 0.0000 (0.0001) C72 * 0.0000 (0.0001) O72A * 0.0000 (0.0000) O72B Rms deviation of fitted atoms = 0.0000 FMAP and GRID set by program FMAP 2 3 40 GRID -1.351 -2 -2 1.351 2 2 R1 = 0.1111 for 6612 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.38 at 0.8868 0.5353 -0.0013 [ 1.05 A from O72B ] Deepest hole -0.30 at 0.5943 0.4993 0.3865 [ 1.04 A from H45C ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 8132 / 26415 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.1132 0.5353 0.9987 1.00000 0.05 0.38 1.05 O72B 1.11 H65B 1.88 N65 2.06 H67B Q2 1 0.5667 1.6388 0.0977 1.00000 0.05 0.34 1.60 O2B 1.72 H69C 2.25 H29B 2.39 H3A Q3 1 1.1521 0.6413 0.8674 1.00000 0.05 0.32 0.86 C64 0.94 C68 1.37 H68B 1.42 H68A Q4 1 0.5551 1.1468 0.1871 1.00000 0.05 0.32 1.20 H21B 1.29 H23B 1.41 C23 1.42 C21 Q5 1 0.3474 0.6667 0.5815 1.00000 0.05 0.32 0.72 H45B 1.13 N45 1.62 C44 1.64 H45C Q6 1 0.5404 0.6031 0.5060 1.00000 0.05 0.31 0.97 H45A 1.07 O31A 1.80 N45 2.11 C31 Q7 1 -0.1084 0.7681 0.6466 1.00000 0.05 0.30 0.69 C84 1.11 C88 1.43 C89 1.49 H88C Q8 1 0.5231 1.1123 0.1766 1.00000 0.05 0.30 0.96 C22 1.16 C23 1.31 C21 1.43 H23B Q9 1 0.8769 0.5540 0.8660 1.00000 0.05 0.30 0.81 H66B 1.20 C66 1.42 H66C 1.83 H67B Q10 1 0.1813 0.8383 0.5547 1.00000 0.05 0.29 1.22 O52B 1.26 C52 1.63 O52A 1.70 H83A Q11 1 -0.1294 1.0263 1.0271 1.00000 0.05 0.28 1.55 H73B 1.67 O71A 1.68 H28B 1.84 C73 Q12 1 0.5098 0.4956 0.6769 1.00000 0.05 0.27 0.98 C42 1.00 C43 1.39 H43B 1.60 C46 Q13 1 0.2031 1.8856 -0.0348 1.00000 0.05 0.27 1.52 O1B 1.62 H28B 1.63 H73B 2.18 C1 Q14 1 0.6806 0.8418 0.0683 1.00000 0.05 0.27 0.47 H25A 1.13 N25 1.69 H25C 1.77 O72A Q15 1 0.9171 0.2943 0.8335 1.00000 0.05 0.27 1.06 H61C 1.35 C61 1.49 H67A 1.59 H61A Q16 1 0.5031 0.4034 0.7403 1.00000 0.05 0.26 1.03 H46A 1.42 H41C 1.48 C46 1.79 C42 Q17 1 0.3416 1.6864 -0.0355 1.00000 0.05 0.26 1.23 O1B 1.37 C1 1.85 O2A 1.86 C2 Q18 1 -0.0755 1.0463 0.7812 1.00000 0.05 0.26 1.00 H81A 1.26 H81C 1.26 C81 1.70 H81B Q19 1 0.5805 0.7973 0.4284 1.00000 0.05 0.26 1.13 H53A 1.13 H53B 1.24 C53 2.01 O51A Q20 1 -0.0264 0.8380 0.6561 1.00000 0.05 0.26 0.77 C84 0.90 C83 1.46 H83B 1.68 H83A Shortest distances between peaks (including symmetry equivalents) 4 8 0.60 7 20 1.25 11 13 1.30 12 16 1.65 6 6 2.53 2 14 2.61 6 19 2.65 1 1 2.66 13 17 2.72 5 10 2.73 5 6 2.76 1 9 2.91 11 14 3.00 Time profile in seconds ----------------------- 0.11: Read and process instructions 0.00: Fit rigid groups 0.03: Interpret restraints etc. 0.02: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.69: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 7.72: Structure factors and derivatives 15.41: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.05: Apply other restraints 1.64: Solve l.s. equations 0.00: Generate HTAB table 0.08: Other dependent quantities, CIF, tables 0.14: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.06: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + ssf1327 finished at 12:17:36 Total CPU time: 26.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++