+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 16:19:31 on 28-Feb-2002 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 02sjc002 in P2(1) CELL 0.71073 11.3936 10.8972 19.5047 90.000 104.239 90.000 ZERR 4.00 0.0003 0.0003 0.0007 0.000 0.001 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H UNIT 108 192 V = 2347.27 F(000) = 840.0 Mu = 0.06 mm-1 Cell Wt = 1490.62 Rho = 1.055 MERG 2 OMIT -3.00 55.00 EXTI 0.03873 FMAP 2 PLAN 20 SIZE 0.04 0.35 0.40 ACTA BOND $H CONF MOVE 1 1 1 -1 WGHT 0.05630 L.S. 4 TEMP -153.00 FVAR 0.29820 MOLE 1 C1A 1 0.529586 0.479438 0.115535 11.00000 0.02738 0.03131 = 0.02507 -0.00165 0.00622 -0.00524 AFIX 23 H1A1 2 0.478036 0.547573 0.124720 11.00000 -1.20000 H1A2 2 0.611582 0.491214 0.146749 11.00000 -1.20000 AFIX 0 C2A 1 0.537620 0.486361 0.038524 11.00000 0.03646 0.03390 = 0.02681 0.00287 0.00892 -0.00723 AFIX 23 H2A1 2 0.568729 0.567974 0.029322 11.00000 -1.20000 H2A2 2 0.595142 0.423501 0.029992 11.00000 -1.20000 AFIX 0 C3A 1 0.413846 0.465384 -0.011936 11.00000 0.03701 0.03590 = 0.02359 0.00361 0.00882 -0.00421 AFIX 23 H3A1 2 0.358534 0.533053 -0.006994 11.00000 -1.20000 H3A2 2 0.421982 0.465125 -0.061314 11.00000 -1.20000 AFIX 0 C4A 1 0.360846 0.343460 0.004207 11.00000 0.03362 0.03544 = 0.02406 0.00028 0.00404 -0.00578 AFIX 23 H4A1 2 0.411721 0.275463 -0.005899 11.00000 -1.20000 H4A2 2 0.278611 0.333624 -0.027053 11.00000 -1.20000 AFIX 0 C5A 1 0.353906 0.335882 0.081391 11.00000 0.03010 0.02756 = 0.02500 -0.00104 0.00523 -0.00130 AFIX 13 H5A 2 0.300561 0.405182 0.088467 11.00000 -1.20000 AFIX 0 C6A 1 0.293007 0.219645 0.098030 11.00000 0.03439 0.03356 = 0.02510 0.00007 0.00192 -0.00757 AFIX 23 H6A1 2 0.344077 0.148001 0.093622 11.00000 -1.20000 H6A2 2 0.214125 0.209723 0.063228 11.00000 -1.20000 AFIX 0 C7A 1 0.272624 0.222806 0.172730 11.00000 0.03203 0.02757 = 0.02742 -0.00042 0.00642 -0.00769 AFIX 23 H7A1 2 0.209783 0.284751 0.174311 11.00000 -1.20000 H7A2 2 0.241931 0.141859 0.183452 11.00000 -1.20000 AFIX 0 C8A 1 0.388061 0.253587 0.229843 11.00000 0.02455 0.01913 = 0.02083 -0.00099 0.00332 0.00007 AFIX 13 H8A 2 0.444519 0.182022 0.235122 11.00000 -1.20000 AFIX 0 C9A 1 0.452571 0.367398 0.209569 11.00000 0.02307 0.02427 = 0.02118 -0.00295 0.00663 0.00129 AFIX 13 H9A 2 0.394723 0.437263 0.206929 11.00000 -1.20000 AFIX 0 C10A 1 0.477648 0.357377 0.134940 11.00000 0.02202 0.02463 = 0.02209 -0.00057 0.00544 -0.00302 C11A 1 0.564294 0.399813 0.269331 11.00000 0.02547 0.03340 = 0.02429 -0.00107 0.00780 -0.00832 AFIX 23 H11A 2 0.625527 0.334090 0.273032 11.00000 -1.20000 H11B 2 0.600266 0.476933 0.257037 11.00000 -1.20000 AFIX 0 C12A 1 0.534454 0.415454 0.340982 11.00000 0.02913 0.03290 = 0.02223 -0.00174 0.00333 -0.00692 AFIX 23 H12A 2 0.481360 0.487934 0.339079 11.00000 -1.20000 H12B 2 0.610275 0.431182 0.377490 11.00000 -1.20000 AFIX 0 C13A 1 0.471431 0.302777 0.362525 11.00000 0.01786 0.02599 = 0.01925 -0.00034 0.00413 -0.00044 C14A 1 0.358912 0.277674 0.301035 11.00000 0.02070 0.01891 = 0.02707 0.00089 0.00331 -0.00008 AFIX 13 H14A 2 0.310153 0.354986 0.294862 11.00000 -1.20000 AFIX 0 C15A 1 0.286154 0.183656 0.331277 11.00000 0.02787 0.03134 = 0.02656 0.00051 0.00692 -0.00758 AFIX 23 H15A 2 0.317196 0.099580 0.327930 11.00000 -1.20000 H15B 2 0.199379 0.186520 0.306170 11.00000 -1.20000 AFIX 0 C16A 1 0.305168 0.223518 0.409265 11.00000 0.02136 0.02846 = 0.02526 0.00305 0.00586 0.00093 AFIX 23 H16A 2 0.230146 0.260784 0.416884 11.00000 -1.20000 H16B 2 0.326340 0.151659 0.440956 11.00000 -1.20000 AFIX 0 C17A 1 0.409611 0.318322 0.425095 11.00000 0.02185 0.02231 = 0.02144 0.00129 0.00382 0.00250 AFIX 13 H17A 2 0.371290 0.401464 0.419928 11.00000 -1.20000 AFIX 0 C18A 1 0.568257 0.253819 0.132767 11.00000 0.03340 0.03477 = 0.02886 0.00160 0.01056 0.00660 AFIX 137 H18A 2 0.647724 0.275579 0.162953 11.00000 -1.50000 H18B 2 0.574899 0.242309 0.084033 11.00000 -1.50000 H18C 2 0.539918 0.177542 0.149931 11.00000 -1.50000 AFIX 0 C19A 1 0.557745 0.192502 0.376142 11.00000 0.02957 0.03500 = 0.02619 -0.00035 0.00512 0.00662 AFIX 137 H19A 2 0.516398 0.121713 0.390505 11.00000 -1.50000 H19B 2 0.629383 0.212790 0.413836 11.00000 -1.50000 H19C 2 0.582596 0.172556 0.332783 11.00000 -1.50000 AFIX 0 C20A 1 0.488802 0.309725 0.501521 11.00000 0.02568 0.02570 = 0.02066 -0.00126 0.00538 -0.00051 AFIX 13 H20A 2 0.525265 0.225762 0.508112 11.00000 -1.20000 AFIX 0 C21A 1 0.591963 0.402248 0.514738 11.00000 0.03430 0.04664 = 0.02256 -0.00442 0.00609 -0.00738 AFIX 137 H21A 2 0.559154 0.484628 0.502210 11.00000 -1.50000 H21B 2 0.648059 0.381190 0.485686 11.00000 -1.50000 H21C 2 0.635117 0.400513 0.564831 11.00000 -1.50000 AFIX 0 C22A 1 0.412806 0.326084 0.555654 11.00000 0.02720 0.03382 = 0.02520 0.00043 0.00850 0.00027 AFIX 23 H22A 2 0.379774 0.410534 0.551509 11.00000 -1.20000 H22B 2 0.343390 0.268697 0.543788 11.00000 -1.20000 AFIX 0 C23A 1 0.481927 0.304120 0.632247 11.00000 0.02987 0.03374 = 0.02576 0.00419 0.00962 0.00385 AFIX 23 H23A 2 0.518036 0.221012 0.635910 11.00000 -1.20000 H23B 2 0.549196 0.363958 0.644731 11.00000 -1.20000 AFIX 0 C24A 1 0.405621 0.314922 0.685796 11.00000 0.03294 0.03904 = 0.02633 0.00322 0.01255 0.00203 AFIX 23 H24A 2 0.336741 0.257177 0.672099 11.00000 -1.20000 H24B 2 0.371664 0.398922 0.682951 11.00000 -1.20000 AFIX 0 C25A 1 0.471379 0.289438 0.762330 11.00000 0.03579 0.02640 = 0.02390 0.00186 0.01091 0.00521 AFIX 13 H25A 2 0.511440 0.207493 0.763839 11.00000 -1.20000 AFIX 0 C26A 1 0.569511 0.383511 0.791707 11.00000 0.05603 0.04275 = 0.03299 -0.00310 0.00366 -0.00362 AFIX 137 H26A 2 0.629610 0.382839 0.763377 11.00000 -1.50000 H26B 2 0.609059 0.362996 0.840883 11.00000 -1.50000 H26C 2 0.533082 0.465300 0.789786 11.00000 -1.50000 AFIX 0 C27A 1 0.381870 0.282064 0.808780 11.00000 0.05232 0.04928 = 0.02792 0.00685 0.01621 0.00693 AFIX 137 H27A 2 0.425491 0.262862 0.857467 11.00000 -1.50000 H27B 2 0.322240 0.217572 0.790920 11.00000 -1.50000 H27C 2 0.340312 0.361014 0.807827 11.00000 -1.50000 AFIX 0 MOLE 2 C1B 1 -0.101259 0.395106 0.094211 11.00000 0.03458 0.03078 = 0.02401 -0.00058 0.00726 -0.00389 AFIX 23 H1B1 2 -0.178547 0.381715 0.107709 11.00000 -1.20000 H1B2 2 -0.048044 0.324074 0.111527 11.00000 -1.20000 AFIX 0 C2B 1 -0.126740 0.400026 0.013229 11.00000 0.04614 0.03560 = 0.02279 -0.00577 0.00601 -0.00494 AFIX 23 H2B1 2 -0.160430 0.320306 -0.006732 11.00000 -1.20000 H2B2 2 -0.187977 0.464229 -0.004922 11.00000 -1.20000 AFIX 0 C3B 1 -0.013170 0.427533 -0.010805 11.00000 0.05075 0.03549 = 0.02442 -0.00009 0.01289 -0.00099 AFIX 23 H3B1 2 -0.034276 0.437970 -0.062821 11.00000 -1.20000 H3B2 2 0.043200 0.357210 0.001032 11.00000 -1.20000 AFIX 0 C4B 1 0.049570 0.543170 0.023944 11.00000 0.03723 0.03474 = 0.02342 0.00347 0.01074 0.00236 AFIX 23 H4B1 2 -0.002126 0.615312 0.006769 11.00000 -1.20000 H4B2 2 0.127016 0.554098 0.010250 11.00000 -1.20000 AFIX 0 C5B 1 0.074421 0.536253 0.104533 11.00000 0.02987 0.02734 = 0.02031 0.00293 0.00914 0.00150 AFIX 13 H5B 2 0.127135 0.462602 0.118783 11.00000 -1.20000 AFIX 0 C6B 1 0.147614 0.644969 0.141160 11.00000 0.02922 0.03439 = 0.02261 0.00357 0.00957 -0.00204 AFIX 23 H6B1 2 0.099192 0.720897 0.129191 11.00000 -1.20000 H6B2 2 0.221676 0.654006 0.123653 11.00000 -1.20000 AFIX 0 C7B 1 0.183194 0.628763 0.221281 11.00000 0.02585 0.03010 = 0.02747 0.00261 0.00906 -0.00322 AFIX 23 H7B1 2 0.222472 0.704905 0.243417 11.00000 -1.20000 H7B2 2 0.242905 0.561326 0.233563 11.00000 -1.20000 AFIX 0 C8B 1 0.074170 0.599746 0.251459 11.00000 0.02242 0.02384 = 0.02034 0.00236 0.00481 -0.00018 AFIX 13 H8B 2 0.020449 0.673580 0.245057 11.00000 -1.20000 AFIX 0 C9B 1 0.000402 0.490766 0.212275 11.00000 0.02436 0.02182 = 0.02325 0.00119 0.00773 0.00185 AFIX 13 H9B 2 0.056782 0.418980 0.219372 11.00000 -1.20000 AFIX 0 C10B 1 -0.041013 0.511982 0.130838 11.00000 0.02781 0.02396 = 0.02125 0.00008 0.00712 -0.00044 C11B 1 -0.103153 0.455697 0.246638 11.00000 0.02940 0.03226 = 0.02046 -0.00223 0.00648 -0.00752 AFIX 23 H11C 2 -0.165298 0.521142 0.236591 11.00000 -1.20000 H11D 2 -0.141475 0.379145 0.224509 11.00000 -1.20000 AFIX 0 C12B 1 -0.062371 0.436749 0.326752 11.00000 0.02957 0.03473 = 0.02317 0.00025 0.00754 -0.00936 AFIX 23 H12C 2 -0.009947 0.363188 0.336761 11.00000 -1.20000 H12D 2 -0.134362 0.421580 0.345442 11.00000 -1.20000 AFIX 0 C13B 1 0.007202 0.547715 0.365079 11.00000 0.02070 0.02865 = 0.01695 0.00043 0.00440 0.00086 C14B 1 0.112950 0.569765 0.330152 11.00000 0.02025 0.02368 = 0.02331 0.00351 0.00464 0.00001 AFIX 13 H14B 2 0.158923 0.490832 0.334260 11.00000 -1.20000 AFIX 0 C15B 1 0.195004 0.661017 0.379431 11.00000 0.02755 0.03588 = 0.02335 0.00174 0.00381 -0.00875 AFIX 23 H15C 2 0.166480 0.746333 0.368744 11.00000 -1.20000 H15D 2 0.279685 0.654507 0.375344 11.00000 -1.20000 AFIX 0 C16B 1 0.184220 0.621711 0.453955 11.00000 0.02467 0.03097 = 0.02224 -0.00028 0.00330 -0.00050 AFIX 23 H16C 2 0.168048 0.694098 0.480904 11.00000 -1.20000 H16D 2 0.260476 0.582875 0.480446 11.00000 -1.20000 AFIX 0 C17B 1 0.077624 0.528749 0.443650 11.00000 0.02186 0.02435 = 0.02346 0.00023 0.00371 -0.00078 AFIX 13 H17B 2 0.113606 0.444582 0.447310 11.00000 -1.20000 AFIX 0 C18B 1 -0.130949 0.619868 0.112875 11.00000 0.02822 0.03329 = 0.02277 -0.00041 0.00634 0.00121 AFIX 137 H18D 2 -0.206290 0.598224 0.125683 11.00000 -1.50000 H18E 2 -0.148233 0.637159 0.062065 11.00000 -1.50000 H18F 2 -0.095476 0.692778 0.139460 11.00000 -1.50000 AFIX 0 C19B 1 -0.074954 0.660099 0.359134 11.00000 0.02558 0.04675 = 0.02294 0.00050 0.00506 0.00598 AFIX 137 H19D 2 -0.028653 0.729155 0.384460 11.00000 -1.50000 H19E 2 -0.142917 0.641379 0.379935 11.00000 -1.50000 H19F 2 -0.105969 0.681822 0.309193 11.00000 -1.50000 AFIX 0 C20B 1 0.008280 0.539684 0.501706 11.00000 0.02485 0.03842 = 0.01932 0.00113 0.00588 -0.00269 AFIX 13 H20B 2 -0.026104 0.624446 0.499399 11.00000 -1.20000 AFIX 0 C21B 1 -0.096814 0.449421 0.489684 11.00000 0.04114 0.08315 = 0.02550 0.00204 0.00874 -0.02264 AFIX 137 H21D 2 -0.157773 0.472175 0.446697 11.00000 -1.50000 H21E 2 -0.133212 0.451548 0.530262 11.00000 -1.50000 H21F 2 -0.067101 0.366440 0.484354 11.00000 -1.50000 AFIX 0 C22B 1 0.092032 0.521809 0.575834 11.00000 0.02500 0.03934 = 0.02063 0.00037 0.00627 -0.00233 AFIX 23 H22C 2 0.122003 0.436189 0.580368 11.00000 -1.20000 H22D 2 0.162981 0.576652 0.581159 11.00000 -1.20000 AFIX 0 C23B 1 0.029972 0.548365 0.635400 11.00000 0.03253 0.03485 = 0.02382 0.00326 0.00634 0.00345 AFIX 23 H23C 2 -0.003198 0.632739 0.629449 11.00000 -1.20000 H23D 2 -0.038956 0.491140 0.631062 11.00000 -1.20000 AFIX 0 C24B 1 0.113463 0.536239 0.709778 11.00000 0.02988 0.04403 = 0.02060 0.00095 0.00701 -0.00180 AFIX 23 H24C 2 0.181229 0.595032 0.714505 11.00000 -1.20000 H24D 2 0.148355 0.452558 0.715242 11.00000 -1.20000 AFIX 0 C25B 1 0.051034 0.559458 0.769427 11.00000 0.03173 0.02540 = 0.01923 -0.00012 0.00620 0.00173 AFIX 13 H25B 2 0.012102 0.642240 0.761928 11.00000 -1.20000 AFIX 0 C26B 1 -0.046719 0.465347 0.769812 11.00000 0.03859 0.03465 = 0.02540 0.00266 0.01034 0.00187 AFIX 137 H26D 2 -0.010038 0.383721 0.778747 11.00000 -1.50000 H26E 2 -0.105831 0.465703 0.723845 11.00000 -1.50000 H26F 2 -0.087505 0.485755 0.807094 11.00000 -1.50000 AFIX 0 C27B 1 0.142801 0.559837 0.841009 11.00000 0.04123 0.04911 = 0.02118 -0.00138 0.00686 -0.00412 AFIX 137 H27D 2 0.102165 0.582446 0.878013 11.00000 -1.50000 H27E 2 0.206869 0.619443 0.840235 11.00000 -1.50000 H27F 2 0.178355 0.477865 0.850790 11.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 02sjc002 in P2(1) C 0.770 H 0.320 C1A - C2A C10A C2A - C3A C1A C3A - C4A C2A C4A - C3A C5A C5A - C6A C4A C10A C6A - C5A C7A C7A - C6A C8A C8A - C14A C7A C9A C9A - C11A C8A C10A C10A - C18A C1A C5A C9A C11A - C12A C9A C12A - C11A C13A C13A - C12A C19A C14A C17A C14A - C15A C8A C13A C15A - C14A C16A C16A - C15A C17A C17A - C20A C16A C13A C18A - C10A C19A - C13A C20A - C21A C22A C17A C21A - C20A C22A - C23A C20A C23A - C24A C22A C24A - C23A C25A C25A - C26A C24A C27A C26A - C25A C27A - C25A C1B - C2B C10B C2B - C3B C1B C3B - C2B C4B C4B - C3B C5B C5B - C6B C4B C10B C6B - C5B C7B C7B - C6B C8B C8B - C14B C7B C9B C9B - C11B C8B C10B C10B - C1B C18B C5B C9B C11B - C12B C9B C12B - C11B C13B C13B - C19B C12B C14B C17B C14B - C8B C15B C13B C15B - C14B C16B C16B - C15B C17B C17B - C20B C16B C13B C18B - C10B C19B - C13B C20B - C21B C22B C17B C21B - C20B C22B - C23B C20B C23B - C22B C24B C24B - C25B C23B C25B - C26B C27B C24B C26B - C25B C27B - C25B Floating origin restraints generated 9288 Reflections read, of which 10 rejected -14 =< h =< 14, -14 =< k =< 11, -25 =< l =< 25, Max. 2-theta = 54.99 0 Systematic absence violations 0 Inconsistent equivalents 9278 Unique reflections, of which 0 suppressed R(int) = 0.0000 R(sigma) = 0.1225 Friedel opposites not merged Maximum memory for data reduction = 7681 / 93550 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 = 9403 / 655154 wR2 = 0.1362 before cycle 1 for 9278 data and 498 / 498 parameters GooF = S = 0.986; Restrained GooF = 0.986 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0563 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29954 0.00052 2.580 OSF 2 0.04493 0.00212 2.920 EXTI Mean shift/esd = 0.135 Maximum = 2.920 for EXTI Max. shift = 0.006 A for H18B Max. dU = 0.000 for C27A Least-squares cycle 2 Maximum vector length = 511 Memory required = 9403 / 655154 wR2 = 0.1367 before cycle 2 for 9278 data and 498 / 498 parameters GooF = S = 0.991; Restrained GooF = 0.991 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0563 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29987 0.00053 0.636 OSF 2 0.04694 0.00234 0.862 EXTI Mean shift/esd = 0.043 Maximum = 0.862 for EXTI Max. shift = 0.002 A for H27D Max. dU = 0.000 for C27A Least-squares cycle 3 Maximum vector length = 511 Memory required = 9403 / 655154 wR2 = 0.1369 before cycle 3 for 9278 data and 498 / 498 parameters GooF = S = 0.992; Restrained GooF = 0.992 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0563 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29986 0.00053 -0.017 OSF 2 0.04687 0.00241 -0.028 EXTI Mean shift/esd = 0.003 Maximum = -0.028 for EXTI Max. shift = 0.000 A for H19D Max. dU = 0.000 for C6B Least-squares cycle 4 Maximum vector length = 511 Memory required = 9403 / 655154 wR2 = 0.1369 before cycle 4 for 9278 data and 498 / 498 parameters GooF = S = 0.992; Restrained GooF = 0.992 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0563 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29986 0.00053 0.000 OSF 2 0.04681 0.00240 -0.025 EXTI Mean shift/esd = 0.001 Maximum = -0.025 for EXTI Max. shift = 0.000 A for H18B Max. dU = 0.000 for C4B Largest correlation matrix elements 0.561 EXTI / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A1 0.3884 0.5089 0.8533 23 0.990 0.000 C1A C2A C10A H1A2 0.5219 0.4524 0.8753 23 0.990 0.000 C1A C2A C10A H2A1 0.4049 0.5766 0.9699 23 0.990 0.000 C2A C3A C1A H2A2 0.4313 0.4321 0.9706 23 0.990 0.000 C2A C3A C1A H3A1 0.5779 0.5349 1.0613 23 0.990 0.000 C3A C4A C2A H3A2 0.6414 0.4669 1.0070 23 0.990 0.000 C3A C4A C2A H4A1 0.7214 0.6663 1.0270 23 0.990 0.000 C4A C3A C5A H4A2 0.5883 0.7245 1.0059 23 0.990 0.000 C4A C3A C5A H5A 0.6993 0.5948 0.9115 13 1.000 0.000 C5A C6A C4A C10A H6A1 0.7858 0.7902 0.9368 23 0.990 0.000 C6A C5A C7A H6A2 0.6559 0.8520 0.9064 23 0.990 0.000 C6A C5A C7A H7A1 0.7903 0.7153 0.8257 23 0.990 0.000 C7A C6A C8A H7A2 0.7581 0.8582 0.8166 23 0.990 0.000 C7A C6A C8A H8A 0.5555 0.8179 0.7649 13 1.000 0.000 C8A C14A C7A C9A H9A 0.6052 0.5627 0.7931 13 1.000 0.000 C9A C11A C8A C10A H11A 0.3997 0.5231 0.7430 23 0.990 0.000 C11A C12A C9A H11B 0.3745 0.6659 0.7270 23 0.990 0.000 C11A C12A C9A H12A 0.3898 0.5688 0.6225 23 0.990 0.000 C12A C11A C13A H12B 0.5187 0.5121 0.6609 23 0.990 0.000 C12A C11A C13A H14A 0.6898 0.6450 0.7051 13 1.000 0.000 C14A C15A C8A C13A H15A 0.8006 0.8133 0.6939 23 0.990 0.000 C15A C14A C16A H15B 0.6828 0.9004 0.6722 23 0.990 0.000 C15A C14A C16A H16A 0.7698 0.7392 0.5831 23 0.990 0.000 C16A C15A C17A H16B 0.6736 0.8484 0.5591 23 0.990 0.000 C16A C15A C17A H17A 0.6286 0.5986 0.5801 13 1.000 0.000 C17A C20A C16A C13A H18A 0.3524 0.7247 0.8368 137 0.980 0.000 C18A C10A H18A H18B 0.4604 0.8227 0.8504 137 0.980 0.000 C18A C10A H18A H18C 0.4247 0.7574 0.9159 137 0.980 0.000 C18A C10A H18A H19A 0.4837 0.8784 0.6097 137 0.980 0.000 C19A C13A H19A H19B 0.4171 0.8272 0.6672 137 0.980 0.000 C19A C13A H19A H19C 0.3707 0.7873 0.5860 137 0.980 0.000 C19A C13A H19A H20A 0.4747 0.7741 0.4919 13 1.000 0.000 C20A C21A C22A C17A H21A 0.4409 0.5153 0.4977 137 0.980 0.000 C21A C20A H21A H21B 0.3649 0.5995 0.4352 137 0.980 0.000 C21A C20A H21A H21C 0.3521 0.6187 0.5144 137 0.980 0.000 C21A C20A H21A H22A 0.6565 0.7315 0.4562 23 0.990 0.000 C22A C23A C20A H22B 0.6203 0.5896 0.4485 23 0.990 0.000 C22A C23A C20A H23A 0.4508 0.6361 0.3553 23 0.990 0.000 C23A C24A C22A H23B 0.4819 0.7790 0.3641 23 0.990 0.000 C23A C24A C22A H24A 0.6284 0.6012 0.3171 23 0.990 0.000 C24A C23A C25A H24B 0.6632 0.7429 0.3279 23 0.990 0.000 C24A C23A C25A H25A 0.4886 0.7925 0.2361 13 1.000 0.000 C25A C26A C24A C27A H26A 0.3706 0.6168 0.2367 137 0.980 0.000 C26A C25A H26A H26B 0.4671 0.5347 0.2100 137 0.980 0.000 C26A C25A H26A H26C 0.3908 0.6371 0.1592 137 0.980 0.000 C26A C25A H26A H27A 0.5744 0.7368 0.1425 137 0.980 0.000 C27A C25A H27A H27B 0.6597 0.6389 0.1922 137 0.980 0.000 C27A C25A H27A H27C 0.6777 0.7824 0.2090 137 0.980 0.000 C27A C25A H27A H1B1 1.1784 0.6182 0.8923 23 0.990 0.000 C1B C2B C10B H1B2 1.0479 0.6759 0.8885 23 0.990 0.000 C1B C2B C10B H2B1 1.1879 0.5357 1.0049 23 0.990 0.000 C2B C3B C1B H2B2 1.1604 0.6796 1.0067 23 0.990 0.000 C2B C3B C1B H3B1 0.9569 0.6429 0.9989 23 0.990 0.000 C3B C2B C4B H3B2 1.0344 0.5621 1.0628 23 0.990 0.000 C3B C2B C4B H4B1 0.8730 0.4459 0.9897 23 0.990 0.000 C4B C3B C5B H4B2 1.0021 0.3846 0.9932 23 0.990 0.000 C4B C3B C5B H5B 0.8730 0.5374 0.8813 13 1.000 0.000 C5B C6B C4B C10B H6B1 0.7783 0.3461 0.8764 23 0.990 0.000 C6B C5B C7B H6B2 0.9007 0.2790 0.8708 23 0.990 0.000 C6B C5B C7B H7B1 0.7570 0.4387 0.7664 23 0.990 0.000 C7B C6B C8B H7B2 0.7775 0.2951 0.7566 23 0.990 0.000 C7B C6B C8B H8B 0.9795 0.3264 0.7549 13 1.000 0.000 C8B C14B C7B C9B H9B 0.9432 0.5810 0.7806 13 1.000 0.000 C9B C11B C8B C10B H11C 1.1414 0.6210 0.7755 23 0.990 0.000 C11B C12B C9B H11D 1.1654 0.4790 0.7634 23 0.990 0.000 C11B C12B C9B H12C 1.1343 0.5785 0.6545 23 0.990 0.000 C12B C11B C13B H12D 1.0099 0.6368 0.6632 23 0.990 0.000 C12B C11B C13B H14B 0.8411 0.5091 0.6657 13 1.000 0.000 C14B C8B C15B C13B H15C 0.7203 0.3456 0.6247 23 0.990 0.000 C15B C14B C16B H15D 0.8335 0.2537 0.6313 23 0.990 0.000 C15B C14B C16B H16C 0.7395 0.4171 0.5196 23 0.990 0.000 C16B C15B C17B H16D 0.8319 0.3059 0.5191 23 0.990 0.000 C16B C15B C17B H17B 0.8864 0.5554 0.5527 13 1.000 0.000 C17B C20B C16B C13B H18D 1.2063 0.4018 0.8744 137 0.980 0.000 C18B C10B H18D H18E 1.0955 0.3072 0.8604 137 0.980 0.000 C18B C10B H18D H18F 1.1481 0.3627 0.9379 137 0.980 0.000 C18B C10B H18D H19D 1.0287 0.2708 0.6157 137 0.980 0.000 C19B C13B H19D H19E 1.1061 0.3183 0.6909 137 0.980 0.000 C19B C13B H19D H19F 1.1429 0.3586 0.6201 137 0.980 0.000 C19B C13B H19D H20B 1.0261 0.3756 0.5006 13 1.000 0.000 C20B C21B C22B C17B H21D 1.1577 0.5282 0.5534 137 0.980 0.000 C21B C20B H21D H21E 1.0670 0.6338 0.5155 137 0.980 0.000 C21B C20B H21D H21F 1.1334 0.5484 0.4698 137 0.980 0.000 C21B C20B H21D H22C 0.8371 0.4233 0.4188 23 0.990 0.000 C22B C23B C20B H22D 0.8780 0.5638 0.4196 23 0.990 0.000 C22B C23B C20B H23C 1.0032 0.3673 0.3706 23 0.990 0.000 C23B C22B C24B H23D 1.0389 0.5089 0.3690 23 0.990 0.000 C23B C22B C24B H24C 0.8189 0.4048 0.2855 23 0.990 0.000 C24B C25B C23B H24D 0.8517 0.5473 0.2847 23 0.990 0.000 C24B C25B C23B H25B 0.9878 0.3578 0.2381 13 1.000 0.000 C25B C26B C27B C24B H26D 1.0100 0.6163 0.2212 137 0.980 0.000 C26B C25B H26D H26E 1.0876 0.5142 0.1930 137 0.980 0.000 C26B C25B H26D H26F 1.1057 0.5345 0.2762 137 0.980 0.000 C26B C25B H26D H27D 0.8980 0.4182 0.1219 137 0.980 0.000 C27B C25B H27D H27E 0.8212 0.5221 0.1493 137 0.980 0.000 C27B C25B H27D H27F 0.7934 0.3802 0.1596 137 0.980 0.000 C27B C25B H27D 02sjc002 in P2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1A 0.47040 0.52056 0.88447 1.00000 0.02742 0.03165 0.02530 -0.00145 0.00610 -0.00520 0.02819 0.00496 0.00025 0.00025 0.00013 0.00000 0.00161 0.00151 0.00159 0.00120 0.00125 0.00134 0.00064 H1A1 0.38838 0.50889 0.85326 1.00000 0.03383 0.00000 0.00000 H1A2 0.52187 0.45237 0.87526 1.00000 0.03383 0.00000 0.00000 C2A 0.46242 0.51369 0.96141 1.00000 0.03702 0.03363 0.02688 0.00273 0.00887 -0.00699 0.03233 0.00513 0.00025 0.00027 0.00013 0.00000 0.00181 0.00160 0.00164 0.00124 0.00135 0.00142 0.00069 H2A1 0.40491 0.57657 0.96993 1.00000 0.03880 0.00000 0.00000 H2A2 0.43127 0.43209 0.97061 1.00000 0.03880 0.00000 0.00000 C3A 0.58612 0.53462 1.01191 1.00000 0.03754 0.03672 0.02381 0.00335 0.00915 -0.00445 0.03241 0.00509 0.00025 0.00026 0.00014 0.00000 0.00182 0.00170 0.00159 0.00125 0.00136 0.00146 0.00070 H3A1 0.57792 0.53489 1.06127 1.00000 0.03889 0.00000 0.00000 H3A2 0.64144 0.46694 1.00699 1.00000 0.03889 0.00000 0.00000 C4A 0.63913 0.65651 0.99577 1.00000 0.03424 0.03624 0.02386 0.00003 0.00398 -0.00574 0.03200 0.00518 0.00027 0.00026 0.00014 0.00000 0.00176 0.00177 0.00161 0.00121 0.00132 0.00142 0.00071 H4A1 0.72139 0.66632 1.02700 1.00000 0.03840 0.00000 0.00000 H4A2 0.58829 0.72453 1.00590 1.00000 0.03840 0.00000 0.00000 C5A 0.64597 0.66408 0.91858 1.00000 0.03102 0.02753 0.02529 -0.00073 0.00557 -0.00114 0.02818 0.00488 0.00025 0.00024 0.00013 0.00000 0.00166 0.00158 0.00160 0.00113 0.00128 0.00129 0.00067 H5A 0.69932 0.59479 0.91150 1.00000 0.03382 0.00000 0.00000 C6A 0.70695 0.78035 0.90200 1.00000 0.03459 0.03385 0.02540 -0.00014 0.00226 -0.00761 0.03217 0.00513 0.00027 0.00026 0.00014 0.00000 0.00176 0.00162 0.00167 0.00123 0.00136 0.00141 0.00071 H6A1 0.78582 0.79022 0.93682 1.00000 0.03861 0.00000 0.00000 H6A2 0.65590 0.85201 0.90641 1.00000 0.03861 0.00000 0.00000 C7A 0.72739 0.77720 0.82729 1.00000 0.03223 0.02808 0.02775 -0.00041 0.00628 -0.00767 0.02954 0.00489 0.00025 0.00025 0.00013 0.00000 0.00172 0.00151 0.00166 0.00117 0.00132 0.00134 0.00067 H7A1 0.79026 0.71528 0.82573 1.00000 0.03545 0.00000 0.00000 H7A2 0.75807 0.85816 0.81658 1.00000 0.03545 0.00000 0.00000 C8A 0.61197 0.74638 0.77013 1.00000 0.02483 0.01952 0.02096 -0.00094 0.00344 0.00009 0.02215 0.00466 0.00024 0.00022 0.00013 0.00000 0.00154 0.00141 0.00150 0.00105 0.00119 0.00118 0.00061 H8A 0.55552 0.81795 0.76485 1.00000 0.02658 0.00000 0.00000 C9A 0.54738 0.63260 0.79043 1.00000 0.02328 0.02484 0.02128 -0.00317 0.00621 0.00135 0.02301 0.00471 0.00023 0.00024 0.00013 0.00000 0.00152 0.00140 0.00149 0.00109 0.00118 0.00122 0.00061 H9A 0.60520 0.56272 0.79305 1.00000 0.02761 0.00000 0.00000 C10A 0.52248 0.64262 0.86510 1.00000 0.02165 0.02488 0.02269 -0.00055 0.00561 -0.00298 0.02305 0.00474 0.00023 0.00023 0.00013 0.00000 0.00154 0.00143 0.00152 0.00111 0.00121 0.00122 0.00062 C11A 0.43571 0.60020 0.73069 1.00000 0.02598 0.03341 0.02444 -0.00088 0.00782 -0.00838 0.02766 0.00476 0.00024 0.00026 0.00013 0.00000 0.00159 0.00165 0.00159 0.00118 0.00126 0.00133 0.00066 H11A 0.39975 0.52307 0.74297 1.00000 0.03319 0.00000 0.00000 H11B 0.37447 0.66591 0.72699 1.00000 0.03319 0.00000 0.00000 C12A 0.46557 0.58457 0.65899 1.00000 0.02906 0.03333 0.02279 -0.00174 0.00333 -0.00677 0.02893 0.00499 0.00025 0.00025 0.00014 0.00000 0.00168 0.00161 0.00154 0.00117 0.00127 0.00135 0.00068 H12A 0.38976 0.56884 0.62247 1.00000 0.03471 0.00000 0.00000 H12B 0.51868 0.51211 0.66088 1.00000 0.03471 0.00000 0.00000 C13A 0.52853 0.69722 0.63748 1.00000 0.01823 0.02590 0.01924 -0.00008 0.00417 -0.00042 0.02120 0.00477 0.00023 0.00023 0.00013 0.00000 0.00140 0.00142 0.00143 0.00112 0.00113 0.00120 0.00059 C14A 0.64103 0.72234 0.69891 1.00000 0.02110 0.01916 0.02715 0.00088 0.00316 0.00011 0.02295 0.00469 0.00023 0.00022 0.00013 0.00000 0.00150 0.00137 0.00159 0.00106 0.00120 0.00117 0.00062 H14A 0.68979 0.64502 0.70507 1.00000 0.02754 0.00000 0.00000 C15A 0.71380 0.81628 0.66878 1.00000 0.02821 0.03143 0.02688 0.00033 0.00717 -0.00758 0.02877 0.00508 0.00025 0.00025 0.00014 0.00000 0.00162 0.00158 0.00162 0.00117 0.00128 0.00130 0.00067 H15A 0.80057 0.81334 0.69389 1.00000 0.03453 0.00000 0.00000 H15B 0.68281 0.90037 0.67217 1.00000 0.03453 0.00000 0.00000 C16A 0.69475 0.77650 0.59073 1.00000 0.02176 0.02876 0.02546 0.00328 0.00604 0.00104 0.02528 0.00480 0.00024 0.00024 0.00013 0.00000 0.00152 0.00150 0.00157 0.00114 0.00122 0.00126 0.00063 H16A 0.76976 0.73923 0.58309 1.00000 0.03034 0.00000 0.00000 H16B 0.67359 0.84840 0.55907 1.00000 0.03034 0.00000 0.00000 C17A 0.59029 0.68174 0.57488 1.00000 0.02201 0.02229 0.02208 0.00143 0.00405 0.00269 0.02236 0.00470 0.00023 0.00023 0.00013 0.00000 0.00149 0.00140 0.00152 0.00110 0.00116 0.00121 0.00061 H17A 0.62864 0.59862 0.58006 1.00000 0.02684 0.00000 0.00000 C18A 0.43175 0.74628 0.86726 1.00000 0.03402 0.03526 0.02913 0.00136 0.01075 0.00634 0.03228 0.00551 0.00026 0.00025 0.00015 0.00000 0.00178 0.00170 0.00172 0.00125 0.00139 0.00140 0.00071 H18A 0.35242 0.72474 0.83684 1.00000 0.04842 0.00000 0.00000 H18B 0.46035 0.82268 0.85039 1.00000 0.04842 0.00000 0.00000 H18C 0.42471 0.75744 0.91595 1.00000 0.04842 0.00000 0.00000 C19A 0.44221 0.80750 0.62386 1.00000 0.03049 0.03562 0.02634 -0.00042 0.00543 0.00641 0.03109 0.00531 0.00025 0.00025 0.00014 0.00000 0.00170 0.00172 0.00168 0.00123 0.00132 0.00136 0.00070 H19A 0.48366 0.87838 0.60967 1.00000 0.04664 0.00000 0.00000 H19B 0.41710 0.82725 0.66716 1.00000 0.04664 0.00000 0.00000 H19C 0.37072 0.78732 0.58603 1.00000 0.04664 0.00000 0.00000 C20A 0.51125 0.69020 0.49847 1.00000 0.02592 0.02604 0.02063 -0.00119 0.00534 -0.00036 0.02426 0.00489 0.00025 0.00025 0.00013 0.00000 0.00154 0.00147 0.00146 0.00112 0.00119 0.00125 0.00062 H20A 0.47473 0.77413 0.49187 1.00000 0.02911 0.00000 0.00000 C21A 0.40813 0.59772 0.48527 1.00000 0.03472 0.04694 0.02263 -0.00424 0.00619 -0.00739 0.03491 0.00495 0.00025 0.00027 0.00014 0.00000 0.00183 0.00190 0.00165 0.00130 0.00136 0.00151 0.00074 H21A 0.44094 0.51532 0.49773 1.00000 0.05237 0.00000 0.00000 H21B 0.36489 0.59954 0.43519 1.00000 0.05237 0.00000 0.00000 H21C 0.35210 0.61872 0.51437 1.00000 0.05237 0.00000 0.00000 C22A 0.58715 0.67401 0.44435 1.00000 0.02742 0.03422 0.02526 0.00057 0.00832 0.00036 0.02865 0.00517 0.00025 0.00026 0.00013 0.00000 0.00157 0.00167 0.00162 0.00121 0.00127 0.00133 0.00067 H22A 0.65650 0.73148 0.45622 1.00000 0.03438 0.00000 0.00000 H22B 0.62029 0.58960 0.44850 1.00000 0.03438 0.00000 0.00000 C23A 0.51808 0.69592 0.36776 1.00000 0.03037 0.03396 0.02601 0.00418 0.01020 0.00402 0.02954 0.00543 0.00026 0.00027 0.00014 0.00000 0.00168 0.00162 0.00163 0.00122 0.00131 0.00137 0.00067 H23A 0.45084 0.63605 0.35527 1.00000 0.03545 0.00000 0.00000 H23B 0.48193 0.77901 0.36408 1.00000 0.03545 0.00000 0.00000 C24A 0.59438 0.68514 0.31424 1.00000 0.03359 0.03899 0.02655 0.00327 0.01262 0.00183 0.03213 0.00559 0.00026 0.00028 0.00014 0.00000 0.00174 0.00172 0.00166 0.00127 0.00135 0.00143 0.00070 H24A 0.62839 0.60116 0.31710 1.00000 0.03856 0.00000 0.00000 H24B 0.66323 0.74292 0.32793 1.00000 0.03856 0.00000 0.00000 C25A 0.52868 0.71056 0.23769 1.00000 0.03628 0.02658 0.02408 0.00179 0.01108 0.00500 0.02834 0.00522 0.00026 0.00025 0.00013 0.00000 0.00174 0.00149 0.00162 0.00114 0.00132 0.00135 0.00067 H25A 0.48860 0.79251 0.23614 1.00000 0.03401 0.00000 0.00000 C26A 0.43055 0.61638 0.20829 1.00000 0.05756 0.04272 0.03313 -0.00289 0.00374 -0.00355 0.04577 0.00560 0.00030 0.00029 0.00016 0.00000 0.00227 0.00193 0.00189 0.00142 0.00160 0.00172 0.00085 H26A 0.37061 0.61677 0.23672 1.00000 0.06865 0.00000 0.00000 H26B 0.46708 0.53465 0.21004 1.00000 0.06865 0.00000 0.00000 H26C 0.39079 0.63706 0.15917 1.00000 0.06865 0.00000 0.00000 C27A 0.61808 0.71780 0.19120 1.00000 0.05377 0.04944 0.02831 0.00686 0.01667 0.00703 0.04269 0.00612 0.00029 0.00029 0.00015 0.00000 0.00219 0.00196 0.00180 0.00141 0.00159 0.00171 0.00083 H27A 0.57438 0.73678 0.14250 1.00000 0.06404 0.00000 0.00000 H27B 0.65971 0.63887 0.19225 1.00000 0.06404 0.00000 0.00000 H27C 0.67765 0.78239 0.20895 1.00000 0.06404 0.00000 0.00000 C1B 1.10115 0.60482 0.90578 1.00000 0.03452 0.03089 0.02435 -0.00047 0.00749 -0.00388 0.02988 0.00490 0.00026 0.00024 0.00013 0.00000 0.00173 0.00164 0.00161 0.00117 0.00130 0.00138 0.00068 H1B1 1.17843 0.61820 0.89228 1.00000 0.03585 0.00000 0.00000 H1B2 1.04794 0.67585 0.88847 1.00000 0.03585 0.00000 0.00000 C2B 1.12665 0.59993 0.98673 1.00000 0.04653 0.03615 0.02275 -0.00566 0.00636 -0.00488 0.03552 0.00520 0.00027 0.00027 0.00013 0.00000 0.00198 0.00173 0.00167 0.00124 0.00141 0.00152 0.00075 H2B1 1.18787 0.53570 1.00487 1.00000 0.04263 0.00000 0.00000 H2B2 1.16038 0.67964 1.00667 1.00000 0.04263 0.00000 0.00000 C3B 1.01329 0.57253 1.01076 1.00000 0.05053 0.03625 0.02445 -0.00008 0.01252 -0.00120 0.03650 0.00564 0.00029 0.00027 0.00015 0.00000 0.00208 0.00172 0.00165 0.00125 0.00147 0.00152 0.00076 H3B1 0.95693 0.64287 0.99891 1.00000 0.04380 0.00000 0.00000 H3B2 1.03443 0.56215 1.06278 1.00000 0.04380 0.00000 0.00000 C4B 0.95044 0.45679 0.97603 1.00000 0.03742 0.03478 0.02380 0.00333 0.01074 0.00228 0.03144 0.00528 0.00027 0.00026 0.00014 0.00000 0.00179 0.00166 0.00163 0.00121 0.00134 0.00143 0.00070 H4B1 0.87297 0.44595 0.98971 1.00000 0.03773 0.00000 0.00000 H4B2 1.00208 0.38463 0.99323 1.00000 0.03773 0.00000 0.00000 C5B 0.92569 0.46376 0.89549 1.00000 0.03043 0.02711 0.02060 0.00302 0.00907 0.00165 0.02556 0.00498 0.00025 0.00024 0.00013 0.00000 0.00163 0.00147 0.00150 0.00109 0.00124 0.00127 0.00064 H5B 0.87299 0.53742 0.88125 1.00000 0.03067 0.00000 0.00000 C6B 0.85235 0.35501 0.85885 1.00000 0.02955 0.03447 0.02260 0.00373 0.00973 -0.00184 0.02829 0.00487 0.00025 0.00025 0.00013 0.00000 0.00165 0.00162 0.00155 0.00119 0.00125 0.00137 0.00066 H6B1 0.77829 0.34606 0.87637 1.00000 0.03395 0.00000 0.00000 H6B2 0.90071 0.27905 0.87082 1.00000 0.03395 0.00000 0.00000 C7B 0.81675 0.37122 0.77871 1.00000 0.02629 0.03080 0.02787 0.00267 0.00917 -0.00371 0.02788 0.00506 0.00024 0.00026 0.00013 0.00000 0.00160 0.00155 0.00159 0.00120 0.00126 0.00133 0.00065 H7B1 0.75705 0.43866 0.76643 1.00000 0.03346 0.00000 0.00000 H7B2 0.77747 0.29508 0.75658 1.00000 0.03346 0.00000 0.00000 C8B 0.92581 0.40023 0.74852 1.00000 0.02222 0.02433 0.02053 0.00229 0.00483 -0.00002 0.02243 0.00480 0.00024 0.00023 0.00013 0.00000 0.00152 0.00146 0.00150 0.00109 0.00116 0.00119 0.00061 H8B 0.97951 0.32638 0.75493 1.00000 0.02692 0.00000 0.00000 C9B 0.99962 0.50918 0.78775 1.00000 0.02468 0.02212 0.02379 0.00139 0.00782 0.00214 0.02321 0.00498 0.00024 0.00023 0.00013 0.00000 0.00153 0.00139 0.00149 0.00112 0.00118 0.00123 0.00061 H9B 0.94322 0.58095 0.78065 1.00000 0.02785 0.00000 0.00000 C10B 1.04092 0.48801 0.86918 1.00000 0.02796 0.02384 0.02136 0.00025 0.00701 -0.00036 0.02422 0.00497 0.00025 0.00023 0.00013 0.00000 0.00162 0.00149 0.00149 0.00107 0.00122 0.00121 0.00063 C11B 1.10322 0.54438 0.75338 1.00000 0.02974 0.03272 0.02084 -0.00212 0.00630 -0.00722 0.02775 0.00497 0.00024 0.00026 0.00013 0.00000 0.00166 0.00162 0.00154 0.00117 0.00125 0.00133 0.00066 H11C 1.14145 0.62098 0.77549 1.00000 0.03330 0.00000 0.00000 H11D 1.16544 0.47900 0.76344 1.00000 0.03330 0.00000 0.00000 C12B 1.06235 0.56325 0.67323 1.00000 0.02982 0.03521 0.02357 0.00033 0.00760 -0.00924 0.02935 0.00480 0.00025 0.00025 0.00013 0.00000 0.00170 0.00167 0.00160 0.00119 0.00131 0.00134 0.00069 H12C 1.13432 0.57849 0.65453 1.00000 0.03523 0.00000 0.00000 H12D 1.00987 0.63678 0.66322 1.00000 0.03523 0.00000 0.00000 C13B 0.99284 0.45227 0.63488 1.00000 0.02061 0.02887 0.01690 0.00046 0.00419 0.00070 0.02220 0.00493 0.00024 0.00024 0.00013 0.00000 0.00146 0.00146 0.00143 0.00109 0.00115 0.00126 0.00060 C14B 0.88707 0.43015 0.66984 1.00000 0.02087 0.02383 0.02349 0.00359 0.00481 0.00005 0.02284 0.00486 0.00023 0.00024 0.00013 0.00000 0.00150 0.00142 0.00153 0.00109 0.00119 0.00122 0.00061 H14B 0.84111 0.50909 0.66573 1.00000 0.02741 0.00000 0.00000 C15B 0.80500 0.33903 0.62063 1.00000 0.02782 0.03600 0.02352 0.00184 0.00379 -0.00850 0.02955 0.00482 0.00025 0.00025 0.00013 0.00000 0.00162 0.00167 0.00159 0.00119 0.00126 0.00137 0.00068 H15C 0.72034 0.34562 0.62473 1.00000 0.03546 0.00000 0.00000 H15D 0.83346 0.25370 0.63132 1.00000 0.03546 0.00000 0.00000 C16B 0.81577 0.37830 0.54605 1.00000 0.02489 0.03120 0.02238 -0.00055 0.00351 -0.00053 0.02656 0.00493 0.00025 0.00025 0.00013 0.00000 0.00155 0.00155 0.00150 0.00114 0.00120 0.00128 0.00064 H16C 0.73952 0.41715 0.51956 1.00000 0.03187 0.00000 0.00000 H16D 0.83192 0.30590 0.51911 1.00000 0.03187 0.00000 0.00000 C17B 0.92240 0.47125 0.55634 1.00000 0.02196 0.02468 0.02369 0.00008 0.00379 -0.00067 0.02376 0.00485 0.00024 0.00023 0.00013 0.00000 0.00149 0.00147 0.00152 0.00109 0.00118 0.00121 0.00062 H17B 0.88644 0.55543 0.55270 1.00000 0.02852 0.00000 0.00000 C18B 1.13091 0.38010 0.88712 1.00000 0.02851 0.03387 0.02317 -0.00015 0.00633 0.00127 0.02852 0.00507 0.00024 0.00024 0.00013 0.00000 0.00167 0.00164 0.00155 0.00121 0.00125 0.00134 0.00067 H18D 1.20631 0.40185 0.87440 1.00000 0.04278 0.00000 0.00000 H18E 1.09552 0.30725 0.86044 1.00000 0.04278 0.00000 0.00000 H18F 1.14807 0.36266 0.93791 1.00000 0.04278 0.00000 0.00000 C19B 1.07501 0.33992 0.64091 1.00000 0.02606 0.04746 0.02307 0.00039 0.00502 0.00594 0.03237 0.00544 0.00025 0.00027 0.00014 0.00000 0.00161 0.00188 0.00161 0.00128 0.00126 0.00145 0.00071 H19D 1.02872 0.27080 0.61565 1.00000 0.04856 0.00000 0.00000 H19E 1.10607 0.31834 0.69087 1.00000 0.04856 0.00000 0.00000 H19F 1.14295 0.35858 0.62007 1.00000 0.04856 0.00000 0.00000 C20B 0.99168 0.46034 0.49831 1.00000 0.02526 0.03869 0.01937 0.00113 0.00609 -0.00255 0.02767 0.00523 0.00025 0.00027 0.00014 0.00000 0.00157 0.00173 0.00147 0.00121 0.00120 0.00135 0.00066 H20B 1.02611 0.37560 0.50064 1.00000 0.03320 0.00000 0.00000 C21B 1.09684 0.55075 0.51034 1.00000 0.04222 0.08300 0.02590 0.00196 0.00920 -0.02301 0.05023 0.00553 0.00028 0.00033 0.00015 0.00000 0.00213 0.00275 0.00183 0.00170 0.00156 0.00191 0.00097 H21D 1.15768 0.52820 0.55342 1.00000 0.07535 0.00000 0.00000 H21E 1.06704 0.63376 0.51550 1.00000 0.07535 0.00000 0.00000 H21F 1.13341 0.54844 0.46984 1.00000 0.07535 0.00000 0.00000 C22B 0.90802 0.47818 0.42417 1.00000 0.02531 0.03953 0.02117 0.00026 0.00624 -0.00218 0.02858 0.00514 0.00025 0.00026 0.00013 0.00000 0.00161 0.00176 0.00155 0.00117 0.00125 0.00132 0.00068 H22C 0.83707 0.42333 0.41884 1.00000 0.03429 0.00000 0.00000 H22D 0.87803 0.56379 0.41963 1.00000 0.03429 0.00000 0.00000 C23B 0.96997 0.45166 0.36461 1.00000 0.03284 0.03536 0.02369 0.00315 0.00603 0.00328 0.03079 0.00529 0.00026 0.00026 0.00014 0.00000 0.00176 0.00166 0.00163 0.00124 0.00134 0.00146 0.00069 H23C 1.00319 0.36731 0.37058 1.00000 0.03695 0.00000 0.00000 H23D 1.03889 0.50890 0.36895 1.00000 0.03695 0.00000 0.00000 C24B 0.88666 0.46369 0.29021 1.00000 0.03066 0.04431 0.02073 0.00122 0.00683 -0.00181 0.03181 0.00536 0.00026 0.00027 0.00013 0.00000 0.00173 0.00183 0.00158 0.00126 0.00129 0.00142 0.00070 H24C 0.81893 0.40485 0.28548 1.00000 0.03817 0.00000 0.00000 H24D 0.85169 0.54733 0.28474 1.00000 0.03817 0.00000 0.00000 C25B 0.94890 0.44060 0.23059 1.00000 0.03203 0.02528 0.01930 -0.00003 0.00586 0.00130 0.02562 0.00494 0.00025 0.00024 0.00013 0.00000 0.00166 0.00150 0.00152 0.00110 0.00124 0.00133 0.00064 H25B 0.98784 0.35782 0.23807 1.00000 0.03074 0.00000 0.00000 C26B 1.04671 0.53472 0.23022 1.00000 0.03953 0.03513 0.02580 0.00236 0.01072 0.00207 0.03302 0.00532 0.00026 0.00026 0.00014 0.00000 0.00186 0.00163 0.00163 0.00125 0.00136 0.00145 0.00070 H26D 1.01003 0.61633 0.22119 1.00000 0.04953 0.00000 0.00000 H26E 1.08762 0.51420 0.19302 1.00000 0.04953 0.00000 0.00000 H26F 1.10571 0.53447 0.27623 1.00000 0.04953 0.00000 0.00000 C27B 0.85719 0.44023 0.15897 1.00000 0.04191 0.04957 0.02167 -0.00127 0.00692 -0.00454 0.03787 0.00541 0.00027 0.00029 0.00014 0.00000 0.00193 0.00193 0.00166 0.00134 0.00140 0.00161 0.00076 H27D 0.89799 0.41817 0.12195 1.00000 0.05681 0.00000 0.00000 H27E 0.82124 0.52206 0.14932 1.00000 0.05681 0.00000 0.00000 H27F 0.79340 0.38022 0.15960 1.00000 0.05681 0.00000 0.00000 Final Structure Factor Calculation for 02sjc002 in P2(1) Total number of l.s. parameters = 498 Maximum vector length = 511 Memory required = 8907 / 23002 wR2 = 0.1369 before cycle 5 for 9278 data and 2 / 498 parameters GooF = S = 0.992; Restrained GooF = 0.992 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0563 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0616 for 5989 Fo > 4sig(Fo) and 0.1185 for all 9278 data wR2 = 0.1369, GooF = S = 0.992, Restrained GooF = 0.992 for all data Flack x parameter = 2.2559 with esd 5.1705 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 54.00 for non-hydrogen and 96.00 for hydrogen atoms Principal mean square atomic displacements U 0.0352 0.0257 0.0237 C1A 0.0431 0.0305 0.0234 C2A 0.0422 0.0336 0.0215 C3A 0.0421 0.0304 0.0235 C4A 0.0320 0.0276 0.0249 C5A 0.0441 0.0292 0.0232 C6A 0.0386 0.0278 0.0222 C7A 0.0266 0.0209 0.0190 C8A 0.0272 0.0233 0.0185 C9A 0.0267 0.0226 0.0198 C10A 0.0389 0.0245 0.0196 C11A 0.0387 0.0272 0.0209 C12A 0.0259 0.0195 0.0181 C13A 0.0292 0.0206 0.0190 C14A 0.0378 0.0270 0.0216 C15A 0.0308 0.0235 0.0216 C16A 0.0249 0.0233 0.0188 C17A 0.0412 0.0298 0.0258 C18A 0.0406 0.0270 0.0257 C19A 0.0264 0.0261 0.0204 C20A 0.0505 0.0324 0.0219 C21A 0.0343 0.0281 0.0236 C22A 0.0379 0.0278 0.0229 C23A 0.0407 0.0339 0.0218 C24A 0.0387 0.0245 0.0218 C25A 0.0625 0.0434 0.0314 C26A 0.0600 0.0445 0.0236 C27A 0.0371 0.0284 0.0241 C1B 0.0489 0.0370 0.0207 C2B 0.0506 0.0362 0.0227 C3B 0.0392 0.0337 0.0214 C4B 0.0317 0.0268 0.0182 C5B 0.0359 0.0302 0.0188 C6B 0.0336 0.0292 0.0209 C7B 0.0255 0.0223 0.0195 C8B 0.0269 0.0218 0.0209 C9B 0.0280 0.0239 0.0208 C10B 0.0386 0.0242 0.0205 C11B 0.0423 0.0247 0.0210 C12B 0.0289 0.0208 0.0169 C13B 0.0275 0.0210 0.0200 C14B 0.0428 0.0236 0.0223 C15B 0.0312 0.0270 0.0214 C16B 0.0257 0.0245 0.0211 C17B 0.0342 0.0283 0.0231 C18B 0.0491 0.0252 0.0228 C19B 0.0393 0.0248 0.0189 C20B 0.0942 0.0324 0.0241 C21B 0.0399 0.0250 0.0209 C22B 0.0377 0.0318 0.0229 C23B 0.0447 0.0304 0.0203 C24B 0.0326 0.0250 0.0192 C25B 0.0405 0.0345 0.0240 C26B 0.0517 0.0404 0.0215 C27B Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.016 0.020 0.025 0.030 0.036 0.045 0.057 0.080 1.000 Number in group 1076. 937. 781. 982. 888. 930. 968. 856. 928. 932. GooF 0.846 0.885 0.903 0.980 0.937 0.950 0.967 0.985 0.920 1.431 K 1.004 1.126 1.056 1.107 1.036 1.046 1.026 1.010 1.002 1.030 Resolution(A) 0.77 0.81 0.85 0.89 0.94 1.00 1.08 1.19 1.36 1.71 inf Number in group 946. 943. 910. 932. 924. 923. 918. 930. 920. 932. GooF 0.908 0.888 0.894 0.895 0.955 0.966 0.961 0.897 0.915 1.489 K 1.212 1.133 1.127 1.076 1.011 0.992 1.000 1.022 1.023 1.020 R1 0.295 0.263 0.239 0.190 0.146 0.088 0.062 0.041 0.044 0.053 Recommended weighting scheme: WGHT 0.0565 0.0000 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 1 -2 0 -3.31 68012.28 27.61 1.000 4.89 2 1 0 29265.90 18834.26 6.48 0.526 4.93 2 -1 0 28318.98 18834.19 6.08 0.526 4.93 2 -2 0 25053.86 17333.18 5.52 0.505 3.88 3 -8 4 3.34 26.80 5.31 0.020 1.21 2 2 0 24197.41 17333.46 5.22 0.505 3.88 1 -1 1 1016.80 1496.64 4.59 0.148 6.78 1 -3 0 18043.65 13690.67 4.22 0.449 3.45 3 9 8 -4.45 39.09 4.02 0.024 1.00 5 -1 0 171.19 234.88 4.02 0.059 2.16 0 4 8 78.04 113.44 3.79 0.041 1.79 10 -9 0 399.00 201.23 3.69 0.054 0.82 1 -11 2 15.58 36.02 3.65 0.023 0.98 3 -10 6 4.45 28.27 3.64 0.020 0.97 -2 0 8 11860.37 9404.68 3.58 0.372 2.40 -10 6 5 55.66 86.21 3.56 0.036 0.96 -5 2 17 37.86 85.20 3.52 0.035 1.09 1 3 0 17157.47 13691.28 3.52 0.449 3.45 0 0 8 9757.19 7841.74 3.46 0.340 2.36 5 -9 7 11.13 44.71 3.41 0.026 0.95 -1 -11 1 52.32 77.64 3.39 0.034 0.99 -8 2 17 107.90 16.85 3.38 0.016 0.98 0 -11 12 212.68 114.79 3.37 0.041 0.84 -2 -4 7 16.70 35.27 3.32 0.023 1.92 -4 -2 25 375.51 188.30 3.25 0.053 0.77 0 0 9 7594.65 6181.45 3.23 0.301 2.10 -1 -2 1 11742.46 9470.33 3.22 0.373 4.86 8 1 8 185.26 262.96 3.21 0.062 1.08 -8 0 16 42.32 109.51 3.20 0.040 1.03 -2 0 4 419.48 516.49 3.18 0.087 4.13 -5 0 8 27.81 3.86 3.18 0.008 1.86 -11 5 5 1.11 24.84 3.13 0.019 0.94 3 -5 0 9639.13 7923.54 3.12 0.341 1.88 -1 -11 3 16.69 37.33 3.10 0.023 0.98 -2 7 10 70.18 107.14 3.10 0.040 1.21 4 -6 6 70.18 100.63 3.07 0.038 1.30 -5 -2 16 71.21 31.01 3.07 0.021 1.14 -1 -8 1 46.76 68.81 3.04 0.032 1.35 6 3 2 132.57 92.80 3.02 0.037 1.56 7 0 9 51.17 15.33 3.01 0.015 1.13 5 -5 2 103.69 139.43 3.00 0.045 1.49 7 0 0 89.18 126.26 2.99 0.043 1.58 -8 -7 1 12.24 60.88 2.98 0.030 1.04 -10 -3 17 103.47 32.58 2.98 0.022 0.88 2 1 15 110.35 157.41 2.95 0.048 1.16 8 -7 4 2.22 24.45 2.93 0.019 0.97 -4 9 10 80.20 121.27 2.90 0.042 1.00 0 0 17 26.71 61.33 2.86 0.030 1.11 11 -5 5 231.58 103.89 2.85 0.039 0.84 -4 5 15 113.69 164.91 2.84 0.049 1.10 Bond lengths and angles C1A - Distance Angles C2A 1.5275 (0.0034) C10A 1.5408 (0.0034) 113.75 (0.22) H1A1 0.9900 108.81 108.81 H1A2 0.9900 108.81 108.81 107.68 C1A - C2A C10A H1A1 C2A - Distance Angles C3A 1.5250 (0.0036) C1A 1.5275 (0.0034) 111.00 (0.23) H2A1 0.9900 109.44 109.44 H2A2 0.9900 109.44 109.44 108.04 C2A - C3A C1A H2A1 C3A - Distance Angles C4A 1.5238 (0.0038) C2A 1.5250 (0.0036) 110.32 (0.23) H3A1 0.9900 109.59 109.59 H3A2 0.9900 109.59 109.59 108.12 C3A - C4A C2A H3A1 C4A - Distance Angles C3A 1.5238 (0.0038) C5A 1.5288 (0.0036) 111.67 (0.21) H4A1 0.9900 109.29 109.29 H4A2 0.9900 109.29 109.29 107.95 C4A - C3A C5A H4A1 C5A - Distance Angles C6A 1.5177 (0.0037) C4A 1.5288 (0.0036) 113.06 (0.21) C10A 1.5493 (0.0036) 111.72 (0.22) 113.39 (0.23) H5A 1.0000 105.98 105.98 105.98 C5A - C6A C4A C10A C6A - Distance Angles C5A 1.5177 (0.0037) C7A 1.5316 (0.0036) 111.63 (0.22) H6A1 0.9900 109.29 109.29 H6A2 0.9900 109.29 109.29 107.95 C6A - C5A C7A H6A1 C7A - Distance Angles C6A 1.5316 (0.0036) C8A 1.5376 (0.0035) 113.07 (0.23) H7A1 0.9900 108.97 108.97 H7A2 0.9900 108.97 108.97 107.77 C7A - C6A C8A H7A1 C8A - Distance Angles C14A 1.5277 (0.0035) C7A 1.5376 (0.0035) 111.03 (0.22) C9A 1.5424 (0.0035) 108.63 (0.19) 111.49 (0.21) H8A 1.0000 108.54 108.54 108.54 C8A - C14A C7A C9A C9A - Distance Angles C11A 1.5401 (0.0034) C8A 1.5424 (0.0035) 110.34 (0.21) C10A 1.5546 (0.0034) 114.70 (0.21) 113.12 (0.20) H9A 1.0000 105.98 105.98 105.98 C9A - C11A C8A C10A C10A - Distance Angles C18A 1.5388 (0.0036) C1A 1.5408 (0.0034) 108.98 (0.22) C5A 1.5493 (0.0036) 112.06 (0.22) 107.82 (0.21) C9A 1.5546 (0.0034) 110.85 (0.21) 109.82 (0.20) 107.25 (0.21) C10A - C18A C1A C5A C11A - Distance Angles C12A 1.5279 (0.0035) C9A 1.5401 (0.0034) 112.93 (0.22) H11A 0.9900 109.00 109.00 H11B 0.9900 109.00 109.00 107.79 C11A - C12A C9A H11A C12A - Distance Angles C11A 1.5279 (0.0035) C13A 1.5315 (0.0036) 112.71 (0.21) H12A 0.9900 109.05 109.05 H12B 0.9900 109.05 109.05 107.81 C12A - C11A C13A H12A C13A - Distance Angles C12A 1.5315 (0.0036) C19A 1.5342 (0.0036) 110.60 (0.22) C14A 1.5486 (0.0035) 106.50 (0.21) 111.65 (0.21) C17A 1.5611 (0.0036) 117.34 (0.22) 110.01 (0.21) 100.24 (0.20) C13A - C12A C19A C14A C14A - Distance Angles C15A 1.5234 (0.0035) C8A 1.5277 (0.0035) 119.73 (0.21) C13A 1.5486 (0.0035) 104.22 (0.21) 114.24 (0.22) H14A 1.0000 105.88 105.88 105.88 C14A - C15A C8A C13A C15A - Distance Angles C14A 1.5234 (0.0035) C16A 1.5460 (0.0035) 103.51 (0.21) H15A 0.9900 111.06 111.06 H15B 0.9900 111.06 111.06 109.03 C15A - C14A C16A H15A C16A - Distance Angles C15A 1.5460 (0.0035) C17A 1.5484 (0.0036) 107.37 (0.20) H16A 0.9900 110.24 110.24 H16B 0.9900 110.24 110.24 108.51 C16A - C15A C17A H16A C17A - Distance Angles C20A 1.5428 (0.0035) C16A 1.5484 (0.0036) 112.98 (0.20) C13A 1.5611 (0.0036) 118.74 (0.21) 104.12 (0.20) H17A 1.0000 106.77 106.77 106.77 C17A - C20A C16A C13A C18A - Distance Angles C10A 1.5388 (0.0037) H18A 0.9800 109.47 H18B 0.9800 109.47 109.47 H18C 0.9800 109.47 109.47 109.47 C18A - C10A H18A H18B C19A - Distance Angles C13A 1.5342 (0.0036) H19A 0.9800 109.47 H19B 0.9800 109.47 109.47 H19C 0.9800 109.47 109.47 109.47 C19A - C13A H19A H19B C20A - Distance Angles C21A 1.5211 (0.0036) C22A 1.5303 (0.0037) 110.54 (0.21) C17A 1.5428 (0.0035) 111.53 (0.21) 111.40 (0.22) H20A 1.0000 107.73 107.73 107.73 C20A - C21A C22A C17A C21A - Distance Angles C20A 1.5211 (0.0036) H21A 0.9800 109.47 H21B 0.9800 109.47 109.47 H21C 0.9800 109.47 109.47 109.47 C21A - C20A H21A H21B C22A - Distance Angles C23A 1.5264 (0.0035) C20A 1.5303 (0.0037) 114.47 (0.22) H22A 0.9900 108.64 108.64 H22B 0.9900 108.64 108.64 107.59 C22A - C23A C20A H22A C23A - Distance Angles C24A 1.5185 (0.0038) C22A 1.5264 (0.0035) 114.60 (0.23) H23A 0.9900 108.61 108.61 H23B 0.9900 108.61 108.61 107.57 C23A - C24A C22A H23A C24A - Distance Angles C23A 1.5185 (0.0038) C25A 1.5219 (0.0036) 115.70 (0.24) H24A 0.9900 108.35 108.35 H24B 0.9900 108.35 108.36 107.43 C24A - C23A C25A H24A C25A - Distance Angles C26A 1.5222 (0.0040) C24A 1.5219 (0.0036) 112.67 (0.23) C27A 1.5232 (0.0039) 110.32 (0.24) 110.72 (0.24) H25A 1.0000 107.64 107.64 107.64 C25A - C26A C24A C27A C26A - Distance Angles C25A 1.5222 (0.0040) H26A 0.9800 109.47 H26B 0.9800 109.47 109.47 H26C 0.9800 109.47 109.47 109.47 C26A - C25A H26A H26B C27A - Distance Angles C25A 1.5232 (0.0039) H27A 0.9800 109.47 H27B 0.9800 109.47 109.47 H27C 0.9800 109.47 109.47 109.47 C27A - C25A H27A H27B C1B - Distance Angles C2B 1.5343 (0.0035) C10B 1.5362 (0.0035) 113.54 (0.22) H1B1 0.9900 108.86 108.86 H1B2 0.9900 108.86 108.86 107.71 C1B - C2B C10B H1B1 C2B - Distance Angles C3B 1.5083 (0.0041) C1B 1.5343 (0.0035) 111.52 (0.24) H2B1 0.9900 109.32 109.32 H2B2 0.9900 109.32 109.32 107.97 C2B - C3B C1B H2B1 C3B - Distance Angles C2B 1.5083 (0.0041) C4B 1.5243 (0.0038) 111.73 (0.24) H3B1 0.9900 109.27 109.27 H3B2 0.9900 109.27 109.27 107.94 C3B - C2B C4B H3B1 C4B - Distance Angles C3B 1.5243 (0.0038) C5B 1.5283 (0.0035) 111.31 (0.22) H4B1 0.9900 109.37 109.37 H4B2 0.9900 109.37 109.37 108.00 C4B - C3B C5B H4B1 C5B - Distance Angles C6B 1.5229 (0.0036) C4B 1.5283 (0.0035) 112.64 (0.21) C10B 1.5454 (0.0037) 112.97 (0.21) 113.13 (0.23) H5B 1.0000 105.76 105.76 105.76 C5B - C6B C4B C10B C6B - Distance Angles C5B 1.5229 (0.0036) C7B 1.5255 (0.0034) 111.57 (0.21) H6B1 0.9900 109.31 109.31 H6B2 0.9900 109.31 109.31 107.96 C6B - C5B C7B H6B1 C7B - Distance Angles C6B 1.5255 (0.0034) C8B 1.5332 (0.0035) 112.41 (0.21) H7B1 0.9900 109.12 109.12 H7B2 0.9900 109.12 109.12 107.85 C7B - C6B C8B H7B1 C8B - Distance Angles C14B 1.5241 (0.0034) C7B 1.5332 (0.0035) 111.69 (0.21) C9B 1.5446 (0.0035) 108.78 (0.19) 111.23 (0.21) H8B 1.0000 108.35 108.35 108.35 C8B - C14B C7B C9B C9B - Distance Angles C11B 1.5425 (0.0035) C8B 1.5446 (0.0035) 110.94 (0.21) C10B 1.5586 (0.0035) 114.09 (0.21) 112.47 (0.20) H9B 1.0000 106.24 106.24 106.24 C9B - C11B C8B C10B C10B - Distance Angles C1B 1.5362 (0.0035) C18B 1.5427 (0.0036) 109.28 (0.22) C5B 1.5454 (0.0037) 107.83 (0.21) 111.46 (0.21) C9B 1.5586 (0.0035) 109.84 (0.20) 111.17 (0.21) 107.18 (0.21) C10B - C1B C18B C5B C11B - Distance Angles C12B 1.5313 (0.0034) C9B 1.5425 (0.0035) 113.83 (0.22) H11C 0.9900 108.79 108.79 H11D 0.9900 108.79 108.79 107.67 C11B - C12B C9B H11C C12B - Distance Angles C11B 1.5313 (0.0034) C13B 1.5356 (0.0036) 112.48 (0.21) H12C 0.9900 109.10 109.10 H12D 0.9900 109.10 109.10 107.84 C12B - C11B C13B H12C C13B - Distance Angles C19B 1.5281 (0.0037) C12B 1.5356 (0.0036) 111.14 (0.23) C14B 1.5425 (0.0035) 111.79 (0.22) 105.85 (0.21) C17B 1.5583 (0.0034) 109.86 (0.21) 116.97 (0.21) 100.71 (0.20) C13B - C19B C12B C14B C14B - Distance Angles C8B 1.5241 (0.0034) C15B 1.5298 (0.0035) 118.28 (0.21) C13B 1.5425 (0.0035) 114.48 (0.21) 104.33 (0.21) H14B 1.0000 106.31 106.31 106.31 C14B - C8B C15B C13B C15B - Distance Angles C14B 1.5298 (0.0035) C16B 1.5498 (0.0035) 103.43 (0.21) H15C 0.9900 111.07 111.07 H15D 0.9900 111.07 111.07 109.04 C15B - C14B C16B H15C C16B - Distance Angles C15B 1.5498 (0.0035) C17B 1.5564 (0.0037) 107.35 (0.20) H16C 0.9900 110.24 110.24 H16D 0.9900 110.24 110.25 108.52 C16B - C15B C17B H16C C17B - Distance Angles C20B 1.5355 (0.0036) C16B 1.5564 (0.0037) 112.40 (0.21) C13B 1.5583 (0.0034) 118.72 (0.22) 103.73 (0.20) H17B 1.0000 107.13 107.13 107.13 C17B - C20B C16B C13B C18B - Distance Angles C10B 1.5427 (0.0036) H18D 0.9800 109.47 H18E 0.9800 109.47 109.47 H18F 0.9800 109.47 109.47 109.47 C18B - C10B H18D H18E C19B - Distance Angles C13B 1.5281 (0.0037) H19D 0.9800 109.47 H19E 0.9800 109.47 109.47 H19F 0.9800 109.47 109.47 109.47 C19B - C13B H19D H19E C20B - Distance Angles C21B 1.5242 (0.0039) C22B 1.5361 (0.0036) 110.21 (0.22) C17B 1.5355 (0.0036) 111.32 (0.23) 111.82 (0.22) H20B 1.0000 107.77 107.77 107.77 C20B - C21B C22B C17B C21B - Distance Angles C20B 1.5242 (0.0039) H21D 0.9800 109.47 H21E 0.9800 109.47 109.47 H21F 0.9800 109.47 109.47 109.47 C21B - C20B H21D H21E C22B - Distance Angles C23B 1.5280 (0.0036) C20B 1.5361 (0.0036) 113.34 (0.23) H22C 0.9900 108.91 108.91 H22D 0.9900 108.91 108.91 107.73 C22B - C23B C20B H22C C23B - Distance Angles C22B 1.5280 (0.0036) C24B 1.5318 (0.0037) 114.18 (0.23) H23C 0.9900 108.71 108.71 H23D 0.9900 108.71 108.71 107.63 C23B - C22B C24B H23C C24B - Distance Angles C25B 1.5244 (0.0036) C23B 1.5318 (0.0037) 114.35 (0.23) H24C 0.9900 108.67 108.67 H24D 0.9900 108.67 108.67 107.60 C24B - C25B C23B H24C C25B - Distance Angles C26B 1.5159 (0.0039) C27B 1.5249 (0.0036) 109.65 (0.22) C24B 1.5244 (0.0036) 111.86 (0.22) 110.90 (0.23) H25B 1.0000 108.10 108.10 108.10 C25B - C26B C27B C24B C26B - Distance Angles C25B 1.5159 (0.0039) H26D 0.9800 109.47 H26E 0.9800 109.47 109.47 H26F 0.9800 109.47 109.47 109.47 C26B - C25B H26D H26E C27B - Distance Angles C25B 1.5249 (0.0036) H27D 0.9800 109.47 H27E 0.9800 109.47 109.47 H27F 0.9800 109.47 109.47 109.47 C27B - C25B H27D H27E Selected torsion angles -56.99 ( 0.32) C10A - C1A - C2A - C3A 55.76 ( 0.31) C1A - C2A - C3A - C4A -55.52 ( 0.32) C2A - C3A - C4A - C5A -175.71 ( 0.25) C3A - C4A - C5A - C6A 55.79 ( 0.31) C3A - C4A - C5A - C10A 172.44 ( 0.24) C4A - C5A - C6A - C7A -58.20 ( 0.32) C10A - C5A - C6A - C7A 51.96 ( 0.32) C5A - C6A - C7A - C8A -170.10 ( 0.21) C6A - C7A - C8A - C14A -48.82 ( 0.30) C6A - C7A - C8A - C9A -54.59 ( 0.28) C14A - C8A - C9A - C11A -177.25 ( 0.21) C7A - C8A - C9A - C11A 175.41 ( 0.21) C14A - C8A - C9A - C10A 52.75 ( 0.29) C7A - C8A - C9A - C10A -67.97 ( 0.28) C2A - C1A - C10A - C18A 53.88 ( 0.29) C2A - C1A - C10A - C5A 170.43 ( 0.22) C2A - C1A - C10A - C9A -62.30 ( 0.29) C6A - C5A - C10A - C18A 66.89 ( 0.29) C4A - C5A - C10A - C18A 177.78 ( 0.21) C6A - C5A - C10A - C1A -53.04 ( 0.28) C4A - C5A - C10A - C1A 59.57 ( 0.28) C6A - C5A - C10A - C9A -171.25 ( 0.21) C4A - C5A - C10A - C9A -62.27 ( 0.28) C11A - C9A - C10A - C18A 65.49 ( 0.28) C8A - C9A - C10A - C18A 58.20 ( 0.29) C11A - C9A - C10A - C1A -174.04 ( 0.22) C8A - C9A - C10A - C1A 175.11 ( 0.22) C11A - C9A - C10A - C5A -57.14 ( 0.27) C8A - C9A - C10A - C5A 53.92 ( 0.29) C8A - C9A - C11A - C12A -176.93 ( 0.22) C10A - C9A - C11A - C12A -55.40 ( 0.32) C9A - C11A - C12A - C13A -66.65 ( 0.29) C11A - C12A - C13A - C19A 54.84 ( 0.29) C11A - C12A - C13A - C14A 166.06 ( 0.22) C11A - C12A - C13A - C17A -52.41 ( 0.32) C7A - C8A - C14A - C15A -175.35 ( 0.23) C9A - C8A - C14A - C15A -176.97 ( 0.21) C7A - C8A - C14A - C13A 60.08 ( 0.28) C9A - C8A - C14A - C13A 168.45 ( 0.21) C12A - C13A - C14A - C15A -70.73 ( 0.27) C19A - C13A - C14A - C15A 45.75 ( 0.25) C17A - C13A - C14A - C15A -59.09 ( 0.27) C12A - C13A - C14A - C8A 61.73 ( 0.28) C19A - C13A - C14A - C8A 178.21 ( 0.20) C17A - C13A - C14A - C8A -165.70 ( 0.22) C8A - C14A - C15A - C16A -36.48 ( 0.26) C13A - C14A - C15A - C16A 12.67 ( 0.27) C14A - C15A - C16A - C17A 145.62 ( 0.22) C15A - C16A - C17A - C20A 15.43 ( 0.26) C15A - C16A - C17A - C13A 81.90 ( 0.30) C12A - C13A - C17A - C20A -45.67 ( 0.31) C19A - C13A - C17A - C20A -163.37 ( 0.20) C14A - C13A - C17A - C20A -151.44 ( 0.22) C12A - C13A - C17A - C16A 80.99 ( 0.25) C19A - C13A - C17A - C16A -36.71 ( 0.24) C14A - C13A - C17A - C16A -178.80 ( 0.22) C16A - C17A - C20A - C21A -56.47 ( 0.31) C13A - C17A - C20A - C21A 57.16 ( 0.28) C16A - C17A - C20A - C22A 179.49 ( 0.22) C13A - C17A - C20A - C22A 62.14 ( 0.30) C21A - C20A - C22A - C23A -173.27 ( 0.21) C17A - C20A - C22A - C23A 177.57 ( 0.24) C20A - C22A - C23A - C24A -178.13 ( 0.23) C22A - C23A - C24A - C25A -65.29 ( 0.34) C23A - C24A - C25A - C26A 170.63 ( 0.25) C23A - C24A - C25A - C27A -55.36 ( 0.32) C10B - C1B - C2B - C3B 53.54 ( 0.31) C1B - C2B - C3B - C4B -54.03 ( 0.32) C2B - C3B - C4B - C5B -174.55 ( 0.25) C3B - C4B - C5B - C6B 55.82 ( 0.30) C3B - C4B - C5B - C10B 173.57 ( 0.22) C4B - C5B - C6B - C7B -56.71 ( 0.30) C10B - C5B - C6B - C7B 52.51 ( 0.30) C5B - C6B - C7B - C8B -173.64 ( 0.22) C6B - C7B - C8B - C14B -51.89 ( 0.28) C6B - C7B - C8B - C9B -52.12 ( 0.28) C14B - C8B - C9B - C11B -175.55 ( 0.20) C7B - C8B - C9B - C11B 178.74 ( 0.21) C14B - C8B - C9B - C10B 55.31 ( 0.29) C7B - C8B - C9B - C10B -66.95 ( 0.29) C2B - C1B - C10B - C18B 54.36 ( 0.30) C2B - C1B - C10B - C5B 170.84 ( 0.22) C2B - C1B - C10B - C9B 175.79 ( 0.21) C6B - C5B - C10B - C1B -54.74 ( 0.27) C4B - C5B - C10B - C1B -64.27 ( 0.29) C6B - C5B - C10B - C18B 65.20 ( 0.27) C4B - C5B - C10B - C18B 57.59 ( 0.27) C6B - C5B - C10B - C9B -172.95 ( 0.20) C4B - C5B - C10B - C9B 58.81 ( 0.29) C11B - C9B - C10B - C1B -173.70 ( 0.22) C8B - C9B - C10B - C1B -62.26 ( 0.28) C11B - C9B - C10B - C18B 65.23 ( 0.29) C8B - C9B - C10B - C18B 175.71 ( 0.22) C11B - C9B - C10B - C5B -56.81 ( 0.27) C8B - C9B - C10B - C5B 50.90 ( 0.30) C8B - C9B - C11B - C12B 179.18 ( 0.21) C10B - C9B - C11B - C12B -54.00 ( 0.32) C9B - C11B - C12B - C13B -65.98 ( 0.30) C11B - C12B - C13B - C19B 55.60 ( 0.28) C11B - C12B - C13B - C14B 166.77 ( 0.22) C11B - C12B - C13B - C17B -52.69 ( 0.32) C7B - C8B - C14B - C15B -175.84 ( 0.23) C9B - C8B - C14B - C15B -176.31 ( 0.22) C7B - C8B - C14B - C13B 60.54 ( 0.28) C9B - C8B - C14B - C13B 59.97 ( 0.29) C19B - C13B - C14B - C8B -61.18 ( 0.27) C12B - C13B - C14B - C8B 176.58 ( 0.20) C17B - C13B - C14B - C8B -70.84 ( 0.26) C19B - C13B - C14B - C15B 168.01 ( 0.20) C12B - C13B - C14B - C15B 45.77 ( 0.24) C17B - C13B - C14B - C15B -164.13 ( 0.22) C8B - C14B - C15B - C16B -35.59 ( 0.26) C13B - C14B - C15B - C16B 11.44 ( 0.28) C14B - C15B - C16B - C17B 145.88 ( 0.23) C15B - C16B - C17B - C20B 16.41 ( 0.27) C15B - C16B - C17B - C13B -44.85 ( 0.32) C19B - C13B - C17B - C20B 83.03 ( 0.31) C12B - C13B - C17B - C20B -162.89 ( 0.22) C14B - C13B - C17B - C20B 80.68 ( 0.26) C19B - C13B - C17B - C16B -151.44 ( 0.23) C12B - C13B - C17B - C16B -37.36 ( 0.24) C14B - C13B - C17B - C16B -179.02 ( 0.23) C16B - C17B - C20B - C21B -57.79 ( 0.33) C13B - C17B - C20B - C21B 57.22 ( 0.30) C16B - C17B - C20B - C22B 178.45 ( 0.21) C13B - C17B - C20B - C22B 63.07 ( 0.32) C21B - C20B - C22B - C23B -172.54 ( 0.22) C17B - C20B - C22B - C23B 177.57 ( 0.22) C20B - C22B - C23B - C24B 178.47 ( 0.23) C22B - C23B - C24B - C25B -63.58 ( 0.31) C23B - C24B - C25B - C26B 173.66 ( 0.23) C23B - C24B - C25B - C27B FMAP and GRID set by program FMAP 2 3 46 GRID -1.163 -2 -2 1.163 2 2 R1 = 0.1144 for 5625 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.63 at 0.4777 0.9543 0.1181 [ 0.13 A from H1A2 ] Deepest hole -0.62 at 0.5563 0.1903 0.3236 [ 1.24 A from C12A ] Mean = 0.00, Rms deviation from mean = 0.23 e/A^3, Highest memory used = 8136 / 39053 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5064 0.9549 0.8679 1.00000 0.05 0.60 1.54 H18B 1.84 H26B 2.02 H6A2 2.06 H3A1 Q2 1 1.0176 0.2022 0.6130 1.00000 0.05 0.57 0.76 H19D 1.67 C19B 2.04 H19E 2.11 H22D Q3 1 0.9662 0.6879 0.9908 1.00000 0.05 0.56 0.53 H3B1 1.38 C3B 1.98 H3B2 2.08 C2B Q4 1 1.0376 0.6606 0.7732 1.00000 0.05 0.56 1.25 H11C 1.42 H9B 1.57 C11B 1.75 C9B Q5 1 0.4686 0.4523 0.2524 1.00000 0.05 0.56 1.22 H26B 1.51 H8A 1.99 C26A 2.09 H26A Q6 1 0.4544 0.4711 0.9742 1.00000 0.05 0.55 0.50 H2A2 0.55 C2A 1.27 H2A1 1.65 C3A Q7 1 0.4973 0.4598 0.5089 1.00000 0.05 0.55 0.87 H21A 1.81 C21A 2.05 H20A 2.33 H17A Q8 1 0.5126 0.4569 1.0976 1.00000 0.05 0.55 1.43 H3A1 1.76 H18B 2.21 C3A 2.22 H6A2 Q9 1 1.0313 0.7008 0.6451 1.00000 0.05 0.54 0.84 H12D 1.61 C12B 1.76 H12C 1.87 H23C Q10 1 1.0173 0.6989 0.2164 1.00000 0.05 0.54 0.91 H26D 1.50 H8B 1.83 C26B 2.08 H18E Q11 1 0.9201 0.1783 0.8373 1.00000 0.05 0.53 1.32 H6B2 1.69 H26D 1.88 H26E 2.14 C26B Q12 1 0.4821 0.4534 0.7896 1.00000 0.05 0.53 1.37 H11A 1.62 H1A2 1.83 H9A 1.88 H25A Q13 1 0.4603 0.4412 0.4664 1.00000 0.05 0.53 1.07 H21A 1.80 H16B 1.87 C21A 1.88 H19A Q14 1 0.9869 0.1982 0.6689 1.00000 0.05 0.52 1.47 H19D 1.82 H15D 1.86 H19E 1.99 C19B Q15 1 0.5380 0.4623 1.0112 1.00000 0.05 0.52 0.96 C3A 1.20 H3A2 1.25 H3A1 1.26 C2A Q16 1 0.9582 0.2232 0.8808 1.00000 0.05 0.52 0.88 H6B2 1.86 C6B 1.94 H18E 2.06 H3B2 Q17 1 0.9647 0.7051 0.6440 1.00000 0.05 0.52 0.93 H12D 1.84 H23C 1.91 C12B 2.28 H16A Q18 1 1.0029 0.6898 0.4981 1.00000 0.05 0.52 0.95 H21E 1.84 C21B 2.05 H20B 2.28 H22D Q19 1 0.9743 0.6773 0.2509 1.00000 0.05 0.52 1.03 H26D 1.72 H8B 1.85 C26B 2.13 H26F Q20 1 0.9014 0.2238 0.6258 1.00000 0.05 0.51 0.87 H15D 1.60 H19D 1.65 C15B 2.22 H16D Shortest distances between peaks (including symmetry equivalents) 1 8 0.75 9 17 0.75 7 13 0.86 10 19 0.95 11 16 0.98 6 15 1.05 14 20 1.15 2 14 1.22 10 11 1.42 2 20 1.42 14 19 1.53 8 15 1.78 10 16 2.00 2 18 2.13 10 14 2.25 11 19 2.33 6 8 2.34 1 5 2.43 3 16 2.47 4 17 2.50 4 9 2.52 19 20 2.52 1 15 2.53 2 19 2.65 9 18 2.81 16 19 2.90 18 20 2.91 17 18 2.99 Time profile in seconds ----------------------- 0.11: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: 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. 0.22: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.06: Set up l.s. refinement 0.00: Generate idealized H-atoms 7.80: Structure factors and derivatives 25.98: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.09: Apply other restraints 2.31: Solve l.s. equations 0.00: Generate HTAB table 0.16: Other dependent quantities, CIF, tables 0.55: Analysis of variance 0.11: Merge reflections for Fourier and .fcf 0.17: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 16:20:09 Total elapsed time: 37.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++