+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008src0843 started at 12:00:29 on 12-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src0843 in P-1 CELL 0.71073 8.2973 13.8488 18.2558 98.021 90.671 91.166 ZERR 4.00 0.0003 0.0005 0.0005 0.002 0.002 0.002 LATT 1 SFAC C H N O UNIT 96 92 4 24 V = 2076.55 F(000) = 888.0 Mu = 0.10 mm-1 Cell Wt = 1685.74 Rho = 1.348 MERG 2 OMIT -3.00 55.00 OMIT 0 -2 6 OMIT 0 1 4 TWIN 1.00 0.00 0.00 0.00 -1.00 0.00 0.00 0.00 -1.00 2 BASF 0.20668 EXTI 0.02557 SHEL 7 0.77 eadp c10 c110 eadp c11 c111 SADI C10 C11 C110 C111 SADI O5 C10 O5 C110 FMAP 2 PLAN 5 SIZE 0.16 0.28 0.43 ACTA BOND $H WGHT 0.20000 L.S. 8 TEMP -153.00 FVAR 0.23059 0.62659 MOLE 1 C1 1 0.557648 0.792723 0.333622 11.00000 0.02305 0.04477 = 0.02707 0.01849 0.00492 0.00259 C2 1 0.690582 0.650779 0.287719 11.00000 0.02743 0.03882 = 0.02039 0.01348 0.00190 -0.00065 C3 1 0.530681 0.615491 0.314203 11.00000 0.02162 0.03908 = 0.02529 0.01636 0.00087 -0.00384 AFIX 13 H3 2 0.465985 0.575582 0.273907 11.00000 -1.20000 AFIX 0 C4 1 0.445867 0.709290 0.346858 11.00000 0.02109 0.04089 = 0.02502 0.01992 -0.00080 0.00018 AFIX 13 H4 2 0.335613 0.714359 0.325202 11.00000 -1.20000 AFIX 0 C5 1 0.442738 0.699343 0.431333 11.00000 0.01930 0.04818 = 0.03114 0.02640 -0.00148 0.00362 C6 1 0.308213 0.625120 0.441540 11.00000 0.02444 0.03729 = 0.02997 0.01857 0.00190 0.00063 AFIX 23 H6A 2 0.207706 0.639077 0.415590 11.00000 -1.20000 H6B 2 0.285608 0.624009 0.494547 11.00000 -1.20000 AFIX 0 C7 1 0.381745 0.528464 0.405864 11.00000 0.02381 0.03980 = 0.02816 0.02024 -0.00032 -0.00173 AFIX 23 H7A 2 0.318311 0.498784 0.361873 11.00000 -1.20000 H7B 2 0.388783 0.481059 0.441596 11.00000 -1.20000 AFIX 0 C8 1 0.552646 0.562877 0.383972 11.00000 0.02177 0.03376 = 0.02539 0.01630 0.00269 -0.00092 C9 1 0.443384 0.793744 0.482526 11.00000 0.02852 0.04210 = 0.02826 0.01752 0.00137 0.00403 PART 1 C10 1 0.284835 0.932915 0.519196 21.00000 0.03420 0.05135 = 0.06657 0.00620 0.00674 0.00103 AFIX 23 H10A 2 0.257533 0.977882 0.483471 21.00000 -1.20000 H10B 2 0.387843 0.955653 0.544355 21.00000 -1.20000 AFIX 0 C11 1 0.155225 0.931485 0.574170 21.00000 0.08920 0.05208 = 0.07036 0.00714 0.04391 0.00174 AFIX 137 H11A 2 0.054713 0.906782 0.548921 21.00000 -1.50000 H11B 2 0.139727 0.997766 0.599477 21.00000 -1.50000 H11C 2 0.185485 0.888960 0.610483 21.00000 -1.50000 AFIX 0 PART 0 C12 1 0.835306 0.809865 0.286114 11.00000 0.02331 0.03462 = 0.03545 0.01460 0.00195 -0.00026 C13 1 0.976482 0.812436 0.327936 11.00000 0.03020 0.04418 = 0.04347 0.02077 0.00027 0.00574 AFIX 43 H13 2 0.984512 0.775261 0.367751 11.00000 -1.20000 AFIX 0 C14 1 1.106199 0.870189 0.310801 11.00000 0.02690 0.04945 = 0.05666 0.01119 -0.00133 -0.00082 AFIX 43 H14 2 1.203002 0.873822 0.339456 11.00000 -1.20000 AFIX 0 C15 1 1.092821 0.922529 0.251351 11.00000 0.02755 0.04308 = 0.05770 0.01159 0.01355 -0.00154 AFIX 43 H15 2 1.182372 0.960247 0.238497 11.00000 -1.20000 AFIX 0 C16 1 0.951157 0.920306 0.210875 11.00000 0.04273 0.03941 = 0.04735 0.02157 0.00998 -0.00599 AFIX 43 H16 2 0.942756 0.957407 0.171031 11.00000 -1.20000 AFIX 0 C17 1 0.821457 0.864123 0.228271 11.00000 0.03449 0.04044 = 0.03476 0.01832 0.00290 -0.00414 AFIX 43 H17 2 0.723397 0.862733 0.200716 11.00000 -1.20000 AFIX 0 C18 1 0.679167 0.487054 0.379850 11.00000 0.01956 0.03524 = 0.02199 0.01488 0.00203 0.00155 C19 1 0.832851 0.509226 0.409605 11.00000 0.01878 0.03873 = 0.02498 0.01542 -0.00177 -0.00619 AFIX 43 H19 2 0.858997 0.573892 0.431848 11.00000 -1.20000 AFIX 0 C20 1 0.949314 0.437104 0.407064 11.00000 0.01905 0.04273 = 0.02823 0.01656 -0.00158 -0.00152 AFIX 43 H20 2 1.053312 0.452538 0.428331 11.00000 -1.20000 AFIX 0 C21 1 0.912926 0.344521 0.373921 11.00000 0.02381 0.04101 = 0.02323 0.01508 -0.00027 0.00702 C22 1 0.760373 0.321934 0.341517 11.00000 0.02987 0.03393 = 0.02753 0.01042 -0.00224 -0.00111 AFIX 43 H22 2 0.736094 0.257899 0.317404 11.00000 -1.20000 AFIX 0 C23 1 0.645975 0.392826 0.344765 11.00000 0.02169 0.03976 = 0.02892 0.01638 -0.00596 0.00066 AFIX 43 H23 2 0.542730 0.377241 0.322725 11.00000 -1.20000 AFIX 0 C24 1 1.145185 0.276419 0.422665 11.00000 0.03357 0.05067 = 0.05427 0.00670 -0.01784 0.01451 AFIX 137 H24A 2 1.229233 0.321392 0.409469 11.00000 -1.50000 H24B 2 1.191147 0.212131 0.424381 11.00000 -1.50000 H24C 2 1.102363 0.301416 0.471280 11.00000 -1.50000 AFIX 0 N1 3 0.698858 0.751637 0.303360 11.00000 0.02008 0.03601 = 0.03096 0.01712 0.00452 0.00002 O1 4 0.535365 0.878810 0.347411 11.00000 0.03627 0.03377 = 0.05070 0.02174 0.01228 0.00736 O2 4 0.796752 0.601464 0.258420 11.00000 0.03041 0.04332 = 0.03519 0.01694 0.01116 0.00203 O3 4 0.586389 0.645919 0.440169 11.00000 0.01858 0.03766 = 0.02713 0.01521 -0.00034 0.00251 O4 4 0.558200 0.829305 0.518398 11.00000 0.04672 0.04517 = 0.06027 -0.00273 -0.02432 0.00918 O5 4 0.300191 0.834501 0.480920 11.00000 0.02422 0.05071 = 0.05646 0.00525 0.00057 0.00581 O6 4 1.018243 0.268147 0.368600 11.00000 0.02558 0.04352 = 0.03955 0.00568 -0.00637 0.00996 PART 2 C110 1 0.289579 0.926254 0.529309 -21.00000 0.03420 0.05135 = 0.06657 0.00620 0.00674 0.00103 AFIX 23 H10C 2 0.355161 0.977200 0.509780 -21.00000 -1.20000 H10D 2 0.331123 0.919248 0.579308 -21.00000 -1.20000 AFIX 0 C111 1 0.117699 0.954398 0.533185 -21.00000 0.08920 0.05208 = 0.07036 0.00714 0.04391 0.00174 AFIX 137 H11D 2 0.072874 0.951228 0.482980 -21.00000 -1.50000 H11E 2 0.109937 1.021040 0.559051 -21.00000 -1.50000 H11F 2 0.056930 0.909487 0.560080 -21.00000 -1.50000 AFIX 0 MOLE 2 PART 0 C31 1 0.049464 0.213617 0.161999 11.00000 0.02720 0.03994 = 0.02614 0.02107 -0.00398 -0.00452 C32 1 0.188009 0.354770 0.212063 11.00000 0.02292 0.04335 = 0.02107 0.01880 -0.00243 -0.00501 C33 1 0.027558 0.390126 0.186239 11.00000 0.02109 0.03699 = 0.02271 0.01749 -0.00031 0.00381 AFIX 13 H33 2 -0.033419 0.428086 0.227140 11.00000 -1.20000 AFIX 0 C34 1 -0.062182 0.295486 0.151944 11.00000 0.02336 0.04032 = 0.02393 0.01698 0.00199 -0.00560 AFIX 13 H34 2 -0.169947 0.287370 0.174552 11.00000 -1.20000 AFIX 0 C35 1 -0.075450 0.311397 0.069122 11.00000 0.01898 0.03912 = 0.02621 0.02172 0.00186 -0.00422 C36 1 -0.207869 0.387536 0.063677 11.00000 0.02456 0.04033 = 0.02683 0.01825 -0.00370 -0.00032 AFIX 23 H36A 2 -0.240585 0.389948 0.011650 11.00000 -1.20000 H36B 2 -0.304003 0.373787 0.092456 11.00000 -1.20000 AFIX 0 C37 1 -0.121005 0.481385 0.097461 11.00000 0.02128 0.04099 = 0.02548 0.01669 -0.00309 0.00170 AFIX 23 H37A 2 -0.176490 0.512310 0.142145 11.00000 -1.20000 H37B 2 -0.113063 0.528422 0.061434 11.00000 -1.20000 AFIX 0 C38 1 0.047415 0.445519 0.117243 11.00000 0.01632 0.03693 = 0.02367 0.01980 0.00083 -0.00075 C39 1 -0.090325 0.220306 0.013752 11.00000 0.02409 0.04017 = 0.03216 0.02374 0.00310 -0.00629 C40 1 -0.276391 0.094369 -0.039962 11.00000 0.03534 0.04486 = 0.04789 0.01620 -0.00186 -0.00756 AFIX 23 H40A 2 -0.200259 0.090968 -0.081549 11.00000 -1.20000 H40B 2 -0.387057 0.096443 -0.060466 11.00000 -1.20000 AFIX 0 C41 1 -0.260840 0.006033 -0.002780 11.00000 0.05048 0.04722 = 0.06360 0.01253 -0.00316 -0.00425 AFIX 137 H41A 2 -0.151827 0.004461 0.018205 11.00000 -1.50000 H41B 2 -0.280676 -0.052415 -0.038912 11.00000 -1.50000 H41C 2 -0.339768 0.007820 0.036878 11.00000 -1.50000 AFIX 0 C42 1 0.327430 0.196989 0.209412 11.00000 0.02498 0.03016 = 0.03023 0.01372 -0.00208 -0.00226 C43 1 0.318631 0.145992 0.268906 11.00000 0.02958 0.04663 = 0.03355 0.02441 0.00057 0.00229 AFIX 43 H43 2 0.224883 0.149430 0.298455 11.00000 -1.20000 AFIX 0 C44 1 0.445627 0.090066 0.285539 11.00000 0.03505 0.04302 = 0.04108 0.01939 -0.00793 0.00206 AFIX 43 H44 2 0.440401 0.055949 0.327157 11.00000 -1.20000 AFIX 0 C45 1 0.579846 0.083553 0.242029 11.00000 0.03083 0.03828 = 0.05873 0.00849 -0.01451 0.00485 AFIX 43 H45 2 0.666841 0.044229 0.253176 11.00000 -1.20000 AFIX 0 C46 1 0.588529 0.133915 0.182291 11.00000 0.02434 0.04866 = 0.05560 0.00957 0.00321 -0.00412 AFIX 43 H46 2 0.681697 0.129103 0.152356 11.00000 -1.20000 AFIX 0 C47 1 0.463428 0.191208 0.165510 11.00000 0.03136 0.04994 = 0.04061 0.02173 0.00198 -0.01205 AFIX 43 H47 2 0.470021 0.226316 0.124461 11.00000 -1.20000 AFIX 0 C48 1 0.180752 0.520859 0.121585 11.00000 0.02046 0.03487 = 0.02140 0.01830 -0.00457 -0.00181 C49 1 0.333631 0.498143 0.093710 11.00000 0.02190 0.02804 = 0.03031 0.01417 -0.00295 0.00164 AFIX 43 H49 2 0.356798 0.432639 0.074533 11.00000 -1.20000 AFIX 0 C50 1 0.453072 0.571258 0.093825 11.00000 0.01364 0.04514 = 0.02667 0.01614 -0.00307 -0.00095 AFIX 43 H50 2 0.555659 0.555363 0.073531 11.00000 -1.20000 AFIX 0 C51 1 0.422565 0.665015 0.122931 11.00000 0.01911 0.04043 = 0.02548 0.01550 -0.00178 -0.00559 C52 1 0.273017 0.688419 0.153928 11.00000 0.02818 0.03471 = 0.03144 0.01201 0.00362 -0.00151 AFIX 43 H52 2 0.252327 0.753408 0.175392 11.00000 -1.20000 AFIX 0 C53 1 0.153826 0.615387 0.153130 11.00000 0.02402 0.04078 = 0.02786 0.01305 0.00341 -0.00277 AFIX 43 H53 2 0.052432 0.631224 0.174729 11.00000 -1.20000 AFIX 0 C54 1 0.658164 0.730414 0.072067 11.00000 0.03297 0.04885 = 0.05173 0.01329 0.01491 -0.01064 AFIX 137 H54A 2 0.737980 0.687505 0.089746 11.00000 -1.50000 H54B 2 0.708936 0.793988 0.068222 11.00000 -1.50000 H54C 2 0.616709 0.701157 0.023339 11.00000 -1.50000 AFIX 0 N31 3 0.194545 0.255509 0.192837 11.00000 0.02191 0.03859 = 0.02925 0.01801 -0.00544 -0.00385 O31 4 0.024073 0.127666 0.143870 11.00000 0.03194 0.03879 = 0.04902 0.02323 -0.01072 -0.00715 O32 4 0.297174 0.404274 0.244053 11.00000 0.03166 0.04392 = 0.03701 0.01950 -0.01289 -0.00551 O33 4 0.069866 0.364656 0.059407 11.00000 0.01897 0.03584 = 0.02423 0.01762 0.00177 -0.00236 O34 4 0.016222 0.185880 -0.024641 11.00000 0.03325 0.04855 = 0.04458 0.00822 0.01055 -0.00692 O35 4 -0.242459 0.183425 0.011943 11.00000 0.02409 0.04346 = 0.04350 0.01463 -0.00049 -0.01055 O36 4 0.528508 0.742912 0.122826 11.00000 0.02267 0.04084 = 0.04020 0.01001 0.00232 -0.00822 HKLF 4 Covalent radii and connectivity table for 2008src0843 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1 N1 C4 C2 - O2 N1 C3 C3 - C2 C4 C8 C4 - C1 C3 C5 C5 - O3 C9 C6 C4 C6 - C5 C7 C7 - C6 C8 C8 - O3 C18 C7 C3 C9 - O4 O5 C5 C10_a - O5 C11_a C11_a - C10_a C12 - C17 C13 N1 C13 - C12 C14 C14 - C15 C13 C15 - C16 C14 C16 - C15 C17 C17 - C16 C12 C18 - C19 C23 C8 C19 - C18 C20 C20 - C21 C19 C21 - C20 O6 C22 C22 - C23 C21 C23 - C22 C18 C24 - O6 N1 - C2 C1 C12 O1 - C1 O2 - C2 O3 - C5 C8 O4 - C9 O5 - C9 C110_b C10_a O6 - C21 C24 C110_b - O5 C111_b C111_b - C110_b C31 - O31 N31 C34 C32 - O32 N31 C33 C33 - C32 C34 C38 C34 - C31 C33 C35 C35 - O33 C39 C36 C34 C36 - C37 C35 C37 - C36 C38 C38 - O33 C48 C37 C33 C39 - O34 O35 C35 C40 - O35 C41 C41 - C40 C42 - C43 C47 N31 C43 - C44 C42 C44 - C45 C43 C45 - C44 C46 C46 - C45 C47 C47 - C46 C42 C48 - C53 C49 C38 C49 - C48 C50 C50 - C51 C49 C51 - C50 O36 C52 C52 - C51 C53 C53 - C48 C52 C54 - O36 N31 - C32 C31 C42 O31 - C31 O32 - C32 O33 - C35 C38 O34 - C39 O35 - C39 C40 O36 - C51 C54 45153 Reflections read, of which 129 rejected -10 =< h =< 10, -17 =< k =< 17, -23 =< l =< 23, Max. 2-theta = 54.97 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 3 6 0 19.52 1.07 8 5.82 -2 -10 3 11.85 0.73 6 5.16 -4 5 3 1.50 0.15 6 0.88 -2 -1 13 54.77 2.13 7 13.62 4 Inconsistent equivalents 9500 Unique reflections, of which 0 suppressed R(int) = 0.0820 R(sigma) = 0.0721 Friedel opposites merged Maximum memory for data reduction = 5433 / 93295 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 = 7074 / 774198 wR2 = 0.3725 before cycle 1 for 9500 data and 573 / 573 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 2. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.445; Restrained GooF = 1.445 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23060 0.00127 0.004 OSF 2 0.62673 0.01584 0.009 FVAR 2 3 0.20668 0.00324 0.001 BASF 1 4 0.02557 0.00658 0.001 EXTI Mean shift/esd = 0.001 Maximum = 0.009 for FVAR 2 Max. shift = 0.001 A for H11D_b Max. dU = 0.000 for C11_a Least-squares cycle 2 Maximum vector length = 511 Memory required = 7074 / 774198 wR2 = 0.3725 before cycle 2 for 9500 data and 573 / 573 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 2. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.445; Restrained GooF = 1.445 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23059 0.00127 0.000 OSF 2 0.62687 0.01585 0.009 FVAR 2 3 0.20669 0.00324 0.001 BASF 1 4 0.02557 0.00658 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.009 for FVAR 2 Max. shift = 0.001 A for H11D_b Max. dU = 0.000 for C11_a Least-squares cycle 3 Maximum vector length = 511 Memory required = 7074 / 774198 wR2 = 0.3725 before cycle 3 for 9500 data and 573 / 573 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 2. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.445; Restrained GooF = 1.445 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23059 0.00127 0.000 OSF 2 0.62696 0.01585 0.006 FVAR 2 3 0.20669 0.00324 0.000 BASF 1 4 0.02557 0.00658 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.006 for FVAR 2 Max. shift = 0.000 A for H11D_b Max. dU = 0.000 for C11_a Least-squares cycle 4 Maximum vector length = 511 Memory required = 7074 / 774198 wR2 = 0.3725 before cycle 4 for 9500 data and 573 / 573 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 2. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.445; Restrained GooF = 1.445 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23060 0.00127 0.000 OSF 2 0.62702 0.01585 0.004 FVAR 2 3 0.20669 0.00324 0.000 BASF 1 4 0.02557 0.00658 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.004 for FVAR 2 Max. shift = 0.000 A for H11D_b Max. dU = 0.000 for C11_a Least-squares cycle 5 Maximum vector length = 511 Memory required = 7074 / 774198 wR2 = 0.3725 before cycle 5 for 9500 data and 573 / 573 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 2. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.445; Restrained GooF = 1.445 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23060 0.00127 0.000 OSF 2 0.62706 0.01585 0.003 FVAR 2 3 0.20669 0.00324 0.000 BASF 1 4 0.02557 0.00658 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.003 for FVAR 2 Max. shift = 0.000 A for H11D_b Max. dU = 0.000 for C11_a Least-squares cycle 6 Maximum vector length = 511 Memory required = 7074 / 774198 wR2 = 0.3725 before cycle 6 for 9500 data and 573 / 573 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 2. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.445; Restrained GooF = 1.445 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23060 0.00127 0.001 OSF 2 0.62709 0.01585 0.002 FVAR 2 3 0.20669 0.00324 0.000 BASF 1 4 0.02558 0.00658 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.002 for FVAR 2 Max. shift = 0.000 A for H11D_b Max. dU = 0.000 for C11_a Least-squares cycle 7 Maximum vector length = 511 Memory required = 7074 / 774198 wR2 = 0.3725 before cycle 7 for 9500 data and 573 / 573 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 2. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.445; Restrained GooF = 1.445 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23060 0.00127 0.000 OSF 2 0.62711 0.01585 0.001 FVAR 2 3 0.20669 0.00324 0.000 BASF 1 4 0.02558 0.00658 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for FVAR 2 Max. shift = 0.000 A for H11D_b Max. dU = 0.000 for C11_a Least-squares cycle 8 Maximum vector length = 511 Memory required = 7074 / 774198 wR2 = 0.3725 before cycle 8 for 9500 data and 573 / 573 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 2. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.445; Restrained GooF = 1.445 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23060 0.00127 0.000 OSF 2 0.62712 0.01585 0.001 FVAR 2 3 0.20669 0.00324 0.000 BASF 1 4 0.02558 0.00658 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for FVAR 2 Max. shift = 0.000 A for H11D_b Max. dU = 0.000 for C11_a Largest correlation matrix elements -0.949 z C110_b / z C10_a -0.826 z C10_a / y C10_a 0.671 x C111_b / x C110_b -0.891 z C110_b / U33 C10_a 0.786 y C110_b / U33 C10_a 0.646 U13 C11_a / U11 C11_a -0.883 z C110_b / y C110_b -0.775 y C110_b / U23 C10_a -0.631 x C110_b / U13 C10_a -0.879 y C110_b / y C10_a 0.767 z C110_b / U23 C10_a 0.616 U13 C10_a / x C10_a 0.876 U33 C10_a / z C10_a -0.754 U33 C10_a / y C10_a -0.615 x C111_b / x C10_a -0.857 x C110_b / x C10_a 0.740 U23 C10_a / y C10_a 0.579 y C110_b / U22 C10_a 0.845 z C110_b / y C10_a -0.740 U23 C10_a / z C10_a -0.557 U22 C10_a / y C10_a 0.845 y C110_b / z C10_a -0.673 U23 C10_a / U33 C10_a -0.538 z C11_a / FVAR 2 Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 0.4660 0.5756 0.2739 13 1.000 0.000 C3 C2 C4 C8 H4 0.3356 0.7144 0.3252 13 1.000 0.000 C4 C1 C3 C5 H6A 0.2077 0.6391 0.4156 23 0.990 0.000 C6 C5 C7 H6B 0.2856 0.6240 0.4945 23 0.990 0.000 C6 C5 C7 H7A 0.3183 0.4988 0.3619 23 0.990 0.000 C7 C6 C8 H7B 0.3888 0.4811 0.4416 23 0.990 0.000 C7 C6 C8 H10A 0.2576 0.9779 0.4835 23 0.990 0.000 C10_a O5 C11_a H10B 0.3878 0.9556 0.5444 23 0.990 0.000 C10_a O5 C11_a H11A 0.0547 0.9068 0.5489 137 0.980 0.000 C11_a C10_a H11A_a H11B 0.1397 0.9978 0.5995 137 0.980 0.000 C11_a C10_a H11A_a H11C 0.1854 0.8890 0.6105 137 0.980 0.000 C11_a C10_a H11A_a H13 0.9845 0.7753 0.3678 43 0.950 0.000 C13 C12 C14 H14 1.2030 0.8738 0.3395 43 0.950 0.000 C14 C15 C13 H15 1.1824 0.9602 0.2385 43 0.950 0.000 C15 C16 C14 H16 0.9428 0.9574 0.1710 43 0.950 0.000 C16 C15 C17 H17 0.7234 0.8627 0.2007 43 0.950 0.000 C17 C16 C12 H19 0.8590 0.5739 0.4318 43 0.950 0.000 C19 C18 C20 H20 1.0533 0.4525 0.4283 43 0.950 0.000 C20 C21 C19 H22 0.7361 0.2579 0.3174 43 0.950 0.000 C22 C23 C21 H23 0.5427 0.3772 0.3227 43 0.950 0.000 C23 C22 C18 H24A 1.2292 0.3214 0.4095 137 0.980 0.000 C24 O6 H24A H24B 1.1912 0.2121 0.4244 137 0.980 0.000 C24 O6 H24A H24C 1.1024 0.3014 0.4713 137 0.980 0.000 C24 O6 H24A H10C 0.3552 0.9772 0.5098 23 0.990 0.000 C110_b O5 C111_b H10D 0.3310 0.9192 0.5793 23 0.990 0.000 C110_b O5 C111_b H11D 0.0730 0.9514 0.4829 137 0.980 0.000 C111_b C110_b H11D_b H11E 0.1100 1.0210 0.5591 137 0.980 0.000 C111_b C110_b H11D_b H11F 0.0568 0.9095 0.5599 137 0.980 0.000 C111_b C110_b H11D_b H33 -0.0334 0.4281 0.2271 13 1.000 0.000 C33 C32 C34 C38 H34 -0.1699 0.2874 0.1746 13 1.000 0.000 C34 C31 C33 C35 H36A -0.2406 0.3899 0.0116 23 0.990 0.000 C36 C37 C35 H36B -0.3040 0.3738 0.0925 23 0.990 0.000 C36 C37 C35 H37A -0.1765 0.5123 0.1421 23 0.990 0.000 C37 C36 C38 H37B -0.1131 0.5284 0.0614 23 0.990 0.000 C37 C36 C38 H40A -0.2003 0.0910 -0.0815 23 0.990 0.000 C40 O35 C41 H40B -0.3871 0.0964 -0.0605 23 0.990 0.000 C40 O35 C41 H41A -0.1518 0.0045 0.0182 137 0.980 0.000 C41 C40 H41A H41B -0.2807 -0.0524 -0.0389 137 0.980 0.000 C41 C40 H41A H41C -0.3398 0.0078 0.0369 137 0.980 0.000 C41 C40 H41A H43 0.2249 0.1494 0.2985 43 0.950 0.000 C43 C44 C42 H44 0.4404 0.0559 0.3272 43 0.950 0.000 C44 C45 C43 H45 0.6668 0.0442 0.2532 43 0.950 0.000 C45 C44 C46 H46 0.6817 0.1291 0.1524 43 0.950 0.000 C46 C45 C47 H47 0.4700 0.2263 0.1245 43 0.950 0.000 C47 C46 C42 H49 0.3568 0.4326 0.0745 43 0.950 0.000 C49 C48 C50 H50 0.5557 0.5554 0.0735 43 0.950 0.000 C50 C51 C49 H52 0.2523 0.7534 0.1754 43 0.950 0.000 C52 C51 C53 H53 0.0524 0.6312 0.1747 43 0.950 0.000 C53 C48 C52 H54A 0.7380 0.6875 0.0897 137 0.980 0.000 C54 O36 H54A H54B 0.7089 0.7940 0.0682 137 0.980 0.000 C54 O36 H54A H54C 0.6167 0.7012 0.0233 137 0.980 0.000 C54 O36 H54A 2008src0843 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.55765 0.79272 0.33362 1.00000 0.02305 0.04477 0.02706 0.01849 0.00492 0.00259 0.03029 0.00966 0.00061 0.00039 0.00025 0.00000 0.00236 0.00318 0.00231 0.00213 0.00192 0.00215 0.00111 C2 0.69058 0.65078 0.28772 1.00000 0.02743 0.03882 0.02040 0.01348 0.00189 -0.00065 0.02800 0.00889 0.00062 0.00036 0.00023 0.00000 0.00252 0.00284 0.00211 0.00192 0.00190 0.00213 0.00107 C3 0.53068 0.61549 0.31420 1.00000 0.02162 0.03909 0.02529 0.01636 0.00087 -0.00384 0.02760 0.00884 0.00057 0.00036 0.00025 0.00000 0.00229 0.00277 0.00219 0.00199 0.00186 0.00203 0.00104 H3 0.46598 0.57558 0.27391 1.00000 0.03312 0.00000 0.00000 C4 0.44587 0.70929 0.34686 1.00000 0.02109 0.04089 0.02502 0.01991 -0.00080 0.00018 0.02757 0.00874 0.00058 0.00035 0.00023 0.00000 0.00227 0.00281 0.00218 0.00199 0.00183 0.00204 0.00105 H4 0.33561 0.71436 0.32520 1.00000 0.03308 0.00000 0.00000 C5 0.44274 0.69934 0.43133 1.00000 0.01930 0.04819 0.03113 0.02640 -0.00148 0.00362 0.03087 0.00944 0.00058 0.00038 0.00025 0.00000 0.00224 0.00314 0.00237 0.00227 0.00189 0.00211 0.00115 C6 0.30821 0.62512 0.44154 1.00000 0.02444 0.03729 0.02997 0.01857 0.00190 0.00063 0.02924 0.00916 0.00061 0.00035 0.00026 0.00000 0.00235 0.00277 0.00233 0.00204 0.00194 0.00203 0.00107 H6A 0.20771 0.63908 0.41559 1.00000 0.03509 0.00000 0.00000 H6B 0.28561 0.62401 0.49455 1.00000 0.03509 0.00000 0.00000 C7 0.38175 0.52846 0.40586 1.00000 0.02381 0.03980 0.02816 0.02024 -0.00032 -0.00174 0.02916 0.00915 0.00059 0.00037 0.00026 0.00000 0.00238 0.00288 0.00230 0.00207 0.00191 0.00206 0.00109 H7A 0.31831 0.49878 0.36187 1.00000 0.03499 0.00000 0.00000 H7B 0.38878 0.48106 0.44160 1.00000 0.03499 0.00000 0.00000 C8 0.55265 0.56288 0.38397 1.00000 0.02178 0.03376 0.02539 0.01630 0.00269 -0.00092 0.02582 0.00862 0.00057 0.00035 0.00024 0.00000 0.00227 0.00266 0.00219 0.00194 0.00182 0.00195 0.00102 C9 0.44338 0.79374 0.48253 1.00000 0.02852 0.04210 0.02827 0.01753 0.00137 0.00403 0.03172 0.00978 0.00062 0.00039 0.00026 0.00000 0.00254 0.00300 0.00233 0.00212 0.00204 0.00222 0.00113 C10_a 0.28484 0.93291 0.51920 0.62712 0.03420 0.05135 0.06658 0.00620 0.00674 0.00103 0.05085 0.03775 0.00242 0.00152 0.00208 0.01585 0.00352 0.00483 0.00967 0.00547 0.00414 0.00305 0.00478 H10A_a 0.25760 0.97789 0.48348 0.62712 0.06103 0.01585 0.00000 H10B_a 0.38783 0.95563 0.54439 0.62712 0.06103 0.01585 0.00000 C11_a 0.15517 0.93149 0.57415 0.62712 0.08938 0.05206 0.07049 0.00710 0.04414 0.00166 0.07044 0.02767 0.00192 0.00092 0.00080 0.01585 0.00901 0.00646 0.00870 0.00567 0.00827 0.00575 0.00390 H11A_a 0.05467 0.90681 0.54888 0.62712 0.10566 0.01585 0.00000 H11B_a 0.13968 0.99777 0.59946 0.62712 0.10566 0.01585 0.00000 H11C_a 0.18536 0.88895 0.61046 0.62712 0.10566 0.01585 0.00000 C12 0.83531 0.80987 0.28611 1.00000 0.02330 0.03463 0.03545 0.01460 0.00195 -0.00026 0.03020 0.00927 0.00061 0.00037 0.00027 0.00000 0.00240 0.00270 0.00249 0.00207 0.00199 0.00206 0.00107 C13 0.97648 0.81244 0.32794 1.00000 0.03020 0.04419 0.04347 0.02077 0.00027 0.00574 0.03783 0.01025 0.00067 0.00040 0.00029 0.00000 0.00276 0.00318 0.00288 0.00249 0.00230 0.00238 0.00126 H13 0.98451 0.77526 0.36775 1.00000 0.04539 0.00000 0.00000 C14 1.10620 0.87019 0.31080 1.00000 0.02690 0.04945 0.05665 0.01119 -0.00132 -0.00082 0.04402 0.01074 0.00071 0.00043 0.00033 0.00000 0.00278 0.00357 0.00348 0.00280 0.00255 0.00246 0.00139 H14 1.20300 0.87382 0.33945 1.00000 0.05282 0.00000 0.00000 C15 1.09282 0.92253 0.25135 1.00000 0.02755 0.04308 0.05771 0.01159 0.01355 -0.00154 0.04228 0.01065 0.00070 0.00042 0.00031 0.00000 0.00277 0.00331 0.00343 0.00271 0.00253 0.00235 0.00137 H15 1.18237 0.96025 0.23850 1.00000 0.05073 0.00000 0.00000 C16 0.95116 0.92031 0.21087 1.00000 0.04273 0.03942 0.04735 0.02157 0.00998 -0.00600 0.04171 0.01078 0.00074 0.00040 0.00031 0.00000 0.00329 0.00313 0.00306 0.00247 0.00262 0.00258 0.00135 H16 0.94276 0.95741 0.17103 1.00000 0.05006 0.00000 0.00000 C17 0.82146 0.86412 0.22827 1.00000 0.03448 0.04044 0.03477 0.01832 0.00290 -0.00414 0.03537 0.00974 0.00070 0.00037 0.00027 0.00000 0.00284 0.00295 0.00261 0.00223 0.00223 0.00234 0.00120 H17 0.72340 0.86273 0.20072 1.00000 0.04245 0.00000 0.00000 C18 0.67917 0.48705 0.37985 1.00000 0.01956 0.03524 0.02198 0.01488 0.00203 0.00155 0.02454 0.00856 0.00056 0.00035 0.00023 0.00000 0.00218 0.00264 0.00210 0.00187 0.00175 0.00190 0.00099 C19 0.83285 0.50923 0.40961 1.00000 0.01878 0.03872 0.02498 0.01542 -0.00176 -0.00619 0.02656 0.00868 0.00056 0.00037 0.00024 0.00000 0.00217 0.00273 0.00217 0.00195 0.00178 0.00195 0.00103 H19 0.85900 0.57389 0.43185 1.00000 0.03187 0.00000 0.00000 C20 0.94931 0.43710 0.40706 1.00000 0.01905 0.04273 0.02823 0.01655 -0.00158 -0.00152 0.02895 0.00882 0.00058 0.00036 0.00024 0.00000 0.00221 0.00295 0.00229 0.00210 0.00189 0.00202 0.00107 H20 1.05331 0.45254 0.42833 1.00000 0.03474 0.00000 0.00000 C21 0.91293 0.34452 0.37392 1.00000 0.02380 0.04102 0.02323 0.01508 -0.00027 0.00702 0.02826 0.00925 0.00059 0.00038 0.00024 0.00000 0.00241 0.00291 0.00215 0.00199 0.00184 0.00206 0.00106 C22 0.76037 0.32193 0.34152 1.00000 0.02987 0.03393 0.02754 0.01041 -0.00224 -0.00111 0.02991 0.00913 0.00063 0.00037 0.00025 0.00000 0.00256 0.00269 0.00230 0.00198 0.00199 0.00209 0.00108 H22 0.73609 0.25790 0.31740 1.00000 0.03589 0.00000 0.00000 C23 0.64598 0.39283 0.34476 1.00000 0.02169 0.03977 0.02892 0.01638 -0.00596 0.00066 0.02908 0.00869 0.00059 0.00035 0.00024 0.00000 0.00231 0.00288 0.00229 0.00206 0.00190 0.00205 0.00107 H23 0.54273 0.37724 0.32272 1.00000 0.03489 0.00000 0.00000 C24 1.14519 0.27642 0.42267 1.00000 0.03358 0.05067 0.05426 0.00670 -0.01785 0.01451 0.04619 0.01030 0.00074 0.00044 0.00032 0.00000 0.00309 0.00355 0.00334 0.00278 0.00265 0.00265 0.00147 H24A 1.22923 0.32140 0.40947 1.00000 0.06929 0.00000 0.00000 H24B 1.19115 0.21213 0.42438 1.00000 0.06929 0.00000 0.00000 H24C 1.10236 0.30141 0.47128 1.00000 0.06929 0.00000 0.00000 N1 0.69886 0.75164 0.30336 1.00000 0.02007 0.03601 0.03096 0.01713 0.00452 0.00002 0.02781 0.00748 0.00049 0.00030 0.00021 0.00000 0.00195 0.00229 0.00202 0.00172 0.00161 0.00169 0.00091 O1 0.53536 0.87881 0.34741 1.00000 0.03627 0.03377 0.05070 0.02174 0.01228 0.00736 0.03856 0.00721 0.00047 0.00026 0.00020 0.00000 0.00211 0.00210 0.00213 0.00167 0.00178 0.00166 0.00091 O2 0.79675 0.60146 0.25842 1.00000 0.03041 0.04332 0.03519 0.01693 0.01116 0.00203 0.03512 0.00680 0.00045 0.00026 0.00018 0.00000 0.00196 0.00211 0.00182 0.00155 0.00158 0.00165 0.00085 O3 0.58639 0.64592 0.44017 1.00000 0.01858 0.03766 0.02713 0.01521 -0.00035 0.00251 0.02676 0.00603 0.00039 0.00025 0.00017 0.00000 0.00158 0.00195 0.00158 0.00140 0.00130 0.00138 0.00076 O4 0.55820 0.82930 0.51840 1.00000 0.04672 0.04517 0.06027 -0.00273 -0.02432 0.00918 0.05176 0.00713 0.00055 0.00030 0.00024 0.00000 0.00259 0.00247 0.00252 0.00201 0.00216 0.00199 0.00118 O5 0.30019 0.83450 0.48092 1.00000 0.02422 0.05071 0.05647 0.00525 0.00057 0.00581 0.04394 0.00723 0.00046 0.00030 0.00022 0.00000 0.00191 0.00237 0.00232 0.00191 0.00175 0.00171 0.00098 O6 1.01824 0.26815 0.36860 1.00000 0.02558 0.04352 0.03955 0.00569 -0.00637 0.00996 0.03616 0.00649 0.00044 0.00027 0.00019 0.00000 0.00189 0.00213 0.00189 0.00163 0.00155 0.00163 0.00087 C110_b 0.28958 0.92625 0.52931 0.37288 0.03420 0.05135 0.06658 0.00620 0.00674 0.00103 0.05085 0.06111 0.00384 0.00276 0.00379 0.01585 0.00352 0.00483 0.00967 0.00547 0.00414 0.00305 0.00478 H10C_b 0.35524 0.97718 0.50981 0.37288 0.06103 0.01585 0.00000 H10D_b 0.33104 0.91923 0.57932 0.37288 0.06103 0.01585 0.00000 C111_b 0.11772 0.95443 0.53314 0.37288 0.08938 0.05206 0.07049 0.00710 0.04414 0.00166 0.07044 0.04911 0.00321 0.00169 0.00145 0.01585 0.00901 0.00646 0.00870 0.00567 0.00827 0.00575 0.00390 H11D_b 0.07302 0.95137 0.48292 0.37288 0.10566 0.01585 0.00000 H11E_b 0.10996 1.02104 0.55907 0.37288 0.10566 0.01585 0.00000 H11F_b 0.05685 0.90947 0.55995 0.37288 0.10566 0.01585 0.00000 C31 0.04946 0.21362 0.16200 1.00000 0.02720 0.03995 0.02615 0.02107 -0.00398 -0.00452 0.02964 0.00919 0.00062 0.00038 0.00025 0.00000 0.00246 0.00295 0.00226 0.00209 0.00192 0.00213 0.00110 C32 0.18801 0.35477 0.21206 1.00000 0.02292 0.04335 0.02107 0.01880 -0.00244 -0.00501 0.02786 0.00865 0.00058 0.00037 0.00023 0.00000 0.00236 0.00291 0.00211 0.00198 0.00183 0.00209 0.00108 C33 0.02756 0.39013 0.18624 1.00000 0.02109 0.03699 0.02271 0.01749 -0.00031 0.00381 0.02563 0.00873 0.00056 0.00035 0.00024 0.00000 0.00226 0.00266 0.00209 0.00190 0.00180 0.00195 0.00100 H33 -0.03342 0.42809 0.22714 1.00000 0.03075 0.00000 0.00000 C34 -0.06218 0.29549 0.15194 1.00000 0.02336 0.04032 0.02393 0.01698 0.00199 -0.00560 0.02809 0.00845 0.00059 0.00035 0.00023 0.00000 0.00235 0.00281 0.00219 0.00198 0.00185 0.00207 0.00107 H34 -0.16995 0.28737 0.17455 1.00000 0.03371 0.00000 0.00000 C35 -0.07545 0.31140 0.06912 1.00000 0.01898 0.03912 0.02621 0.02172 0.00186 -0.00422 0.02653 0.00860 0.00056 0.00035 0.00023 0.00000 0.00218 0.00279 0.00220 0.00201 0.00177 0.00194 0.00105 C36 -0.20787 0.38754 0.06368 1.00000 0.02456 0.04033 0.02683 0.01825 -0.00369 -0.00032 0.02933 0.00875 0.00060 0.00035 0.00025 0.00000 0.00237 0.00284 0.00229 0.00204 0.00189 0.00208 0.00109 H36A -0.24058 0.38995 0.01165 1.00000 0.03520 0.00000 0.00000 H36B -0.30400 0.37379 0.09246 1.00000 0.03520 0.00000 0.00000 C37 -0.12101 0.48138 0.09746 1.00000 0.02128 0.04098 0.02548 0.01669 -0.00309 0.00170 0.02812 0.00871 0.00057 0.00037 0.00025 0.00000 0.00231 0.00289 0.00225 0.00205 0.00183 0.00202 0.00107 H37A -0.17649 0.51231 0.14214 1.00000 0.03375 0.00000 0.00000 H37B -0.11306 0.52842 0.06143 1.00000 0.03375 0.00000 0.00000 C38 0.04742 0.44552 0.11724 1.00000 0.01632 0.03693 0.02367 0.01980 0.00083 -0.00075 0.02418 0.00841 0.00053 0.00035 0.00023 0.00000 0.00209 0.00268 0.00212 0.00194 0.00172 0.00184 0.00100 C39 -0.09033 0.22031 0.01375 1.00000 0.02409 0.04018 0.03215 0.02374 0.00310 -0.00629 0.03044 0.00925 0.00059 0.00037 0.00026 0.00000 0.00240 0.00291 0.00239 0.00216 0.00201 0.00211 0.00113 C40 -0.27639 0.09437 -0.03996 1.00000 0.03534 0.04486 0.04789 0.01620 -0.00186 -0.00755 0.04191 0.00978 0.00072 0.00038 0.00030 0.00000 0.00298 0.00326 0.00302 0.00251 0.00246 0.00249 0.00132 H40A -0.20026 0.09097 -0.08155 1.00000 0.05029 0.00000 0.00000 H40B -0.38706 0.09644 -0.06047 1.00000 0.05029 0.00000 0.00000 C41 -0.26084 0.00603 -0.00278 1.00000 0.05047 0.04722 0.06360 0.01253 -0.00316 -0.00425 0.05342 0.01219 0.00086 0.00047 0.00039 0.00000 0.00379 0.00355 0.00356 0.00285 0.00317 0.00298 0.00156 H41A -0.15183 0.00446 0.01821 1.00000 0.08012 0.00000 0.00000 H41B -0.28067 -0.05241 -0.03891 1.00000 0.08012 0.00000 0.00000 H41C -0.33977 0.00782 0.03688 1.00000 0.08012 0.00000 0.00000 C42 0.32743 0.19699 0.20941 1.00000 0.02498 0.03016 0.03024 0.01373 -0.00208 -0.00226 0.02761 0.00866 0.00060 0.00034 0.00025 0.00000 0.00238 0.00256 0.00232 0.00194 0.00193 0.00199 0.00103 C43 0.31863 0.14599 0.26891 1.00000 0.02958 0.04663 0.03355 0.02441 0.00057 0.00229 0.03478 0.00956 0.00065 0.00038 0.00026 0.00000 0.00262 0.00313 0.00249 0.00226 0.00215 0.00232 0.00119 H43 0.22488 0.14943 0.29846 1.00000 0.04174 0.00000 0.00000 C44 0.44563 0.09007 0.28554 1.00000 0.03505 0.04302 0.04108 0.01939 -0.00793 0.00206 0.03849 0.00994 0.00069 0.00040 0.00029 0.00000 0.00291 0.00318 0.00280 0.00242 0.00240 0.00243 0.00126 H44 0.44040 0.05595 0.32716 1.00000 0.04618 0.00000 0.00000 C45 0.57985 0.08355 0.24203 1.00000 0.03083 0.03828 0.05872 0.00849 -0.01451 0.00485 0.04251 0.00984 0.00070 0.00041 0.00032 0.00000 0.00294 0.00313 0.00347 0.00262 0.00266 0.00237 0.00138 H45 0.66684 0.04423 0.25318 1.00000 0.05102 0.00000 0.00000 C46 0.58853 0.13391 0.18229 1.00000 0.02434 0.04866 0.05561 0.00957 0.00321 -0.00412 0.04270 0.01010 0.00068 0.00042 0.00033 0.00000 0.00272 0.00354 0.00337 0.00274 0.00249 0.00241 0.00137 H46 0.68170 0.12910 0.15236 1.00000 0.05124 0.00000 0.00000 C47 0.46343 0.19121 0.16551 1.00000 0.03136 0.04994 0.04061 0.02173 0.00198 -0.01205 0.03934 0.00989 0.00068 0.00041 0.00029 0.00000 0.00280 0.00338 0.00281 0.00253 0.00229 0.00246 0.00131 H47 0.47002 0.22632 0.12446 1.00000 0.04721 0.00000 0.00000 C48 0.18075 0.52086 0.12158 1.00000 0.02046 0.03487 0.02140 0.01830 -0.00457 -0.00181 0.02429 0.00820 0.00056 0.00034 0.00023 0.00000 0.00218 0.00269 0.00207 0.00190 0.00175 0.00192 0.00101 C49 0.33363 0.49814 0.09371 1.00000 0.02190 0.02804 0.03031 0.01417 -0.00295 0.00164 0.02580 0.00870 0.00057 0.00035 0.00025 0.00000 0.00227 0.00244 0.00230 0.00190 0.00188 0.00191 0.00100 H49 0.35680 0.43264 0.07453 1.00000 0.03096 0.00000 0.00000 C50 0.45307 0.57126 0.09382 1.00000 0.01364 0.04514 0.02667 0.01614 -0.00307 -0.00095 0.02748 0.00837 0.00055 0.00036 0.00024 0.00000 0.00204 0.00303 0.00223 0.00211 0.00178 0.00198 0.00107 H50 0.55566 0.55536 0.07353 1.00000 0.03297 0.00000 0.00000 C51 0.42257 0.66501 0.12293 1.00000 0.01912 0.04043 0.02548 0.01550 -0.00178 -0.00559 0.02741 0.00854 0.00057 0.00037 0.00024 0.00000 0.00222 0.00292 0.00219 0.00199 0.00181 0.00200 0.00106 C52 0.27302 0.68842 0.15393 1.00000 0.02818 0.03471 0.03145 0.01201 0.00362 -0.00151 0.03075 0.00923 0.00063 0.00038 0.00026 0.00000 0.00255 0.00273 0.00241 0.00207 0.00203 0.00211 0.00110 H52 0.25233 0.75341 0.17539 1.00000 0.03690 0.00000 0.00000 C53 0.15383 0.61539 0.15313 1.00000 0.02402 0.04078 0.02786 0.01305 0.00341 -0.00277 0.03013 0.00885 0.00061 0.00036 0.00025 0.00000 0.00242 0.00292 0.00229 0.00204 0.00196 0.00215 0.00109 H53 0.05243 0.63122 0.17473 1.00000 0.03615 0.00000 0.00000 C54 0.65816 0.73041 0.07207 1.00000 0.03297 0.04886 0.05173 0.01329 0.01491 -0.01064 0.04397 0.01040 0.00073 0.00042 0.00030 0.00000 0.00299 0.00340 0.00324 0.00270 0.00258 0.00256 0.00141 H54A 0.73798 0.68751 0.08975 1.00000 0.06596 0.00000 0.00000 H54B 0.70893 0.79399 0.06822 1.00000 0.06596 0.00000 0.00000 H54C 0.61671 0.70115 0.02334 1.00000 0.06596 0.00000 0.00000 N31 0.19454 0.25551 0.19284 1.00000 0.02191 0.03859 0.02925 0.01801 -0.00544 -0.00385 0.02876 0.00716 0.00049 0.00030 0.00021 0.00000 0.00200 0.00241 0.00198 0.00174 0.00163 0.00175 0.00093 O31 0.02407 0.12767 0.14387 1.00000 0.03194 0.03879 0.04901 0.02323 -0.01072 -0.00715 0.03849 0.00659 0.00046 0.00027 0.00020 0.00000 0.00198 0.00218 0.00212 0.00171 0.00170 0.00165 0.00092 O32 0.29717 0.40427 0.24405 1.00000 0.03167 0.04392 0.03701 0.01950 -0.01289 -0.00551 0.03641 0.00628 0.00046 0.00026 0.00018 0.00000 0.00200 0.00213 0.00186 0.00160 0.00161 0.00166 0.00089 O33 0.06987 0.36466 0.05941 1.00000 0.01897 0.03584 0.02424 0.01762 0.00177 -0.00236 0.02510 0.00575 0.00038 0.00024 0.00016 0.00000 0.00157 0.00189 0.00153 0.00136 0.00127 0.00137 0.00074 O34 0.01622 0.18588 -0.02464 1.00000 0.03324 0.04855 0.04459 0.00822 0.01055 -0.00691 0.04199 0.00688 0.00048 0.00028 0.00020 0.00000 0.00215 0.00237 0.00209 0.00176 0.00177 0.00177 0.00097 O35 -0.24246 0.18343 0.01194 1.00000 0.02409 0.04346 0.04351 0.01463 -0.00049 -0.01055 0.03637 0.00633 0.00043 0.00026 0.00019 0.00000 0.00179 0.00220 0.00197 0.00165 0.00154 0.00158 0.00089 O36 0.52851 0.74291 0.12283 1.00000 0.02267 0.04084 0.04020 0.01001 0.00232 -0.00822 0.03426 0.00613 0.00043 0.00026 0.00019 0.00000 0.00178 0.00208 0.00185 0.00158 0.00149 0.00151 0.00085 Final Structure Factor Calculation for 2008src0843 in P-1 Total number of l.s. parameters = 573 Maximum vector length = 511 Memory required = 6501 / 22995 wR2 = 0.3725 before cycle 9 for 9500 data and 0 / 573 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 2. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.445; Restrained GooF = 1.445 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.2000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1252 for 6712 Fo > 4sig(Fo) and 0.1586 for all 9500 data wR2 = 0.3725, GooF = S = 1.445, Restrained GooF = 1.445 for all data Occupancy sum of asymmetric unit = 62.00 for non-hydrogen and 46.00 for hydrogen atoms Principal mean square atomic displacements U 0.0507 0.0240 0.0161 C1 0.0417 0.0277 0.0146 C2 0.0451 0.0225 0.0151 C3 0.0484 0.0212 0.0131 C4 0.0596 0.0210 0.0120 C5 0.0463 0.0246 0.0168 C6 0.0489 0.0237 0.0148 C7 0.0410 0.0228 0.0137 C8 0.0484 0.0281 0.0186 C9 0.0682 0.0513 0.0330 C10_a 0.1240 0.0521 0.0352 C11_a 0.0436 0.0254 0.0217 C12 0.0569 0.0325 0.0240 C13 0.0580 0.0473 0.0268 C14 0.0624 0.0430 0.0214 C15 0.0582 0.0481 0.0188 C16 0.0499 0.0361 0.0201 C17 0.0401 0.0196 0.0139 C18 0.0454 0.0189 0.0154 C19 0.0481 0.0202 0.0186 C20 0.0458 0.0242 0.0148 C21 0.0379 0.0292 0.0226 C22 0.0462 0.0262 0.0148 C23 0.0703 0.0514 0.0169 C24 0.0448 0.0231 0.0155 N1 0.0636 0.0304 0.0216 O1 0.0520 0.0349 0.0185 O2 0.0430 0.0204 0.0168 O3 0.0863 0.0416 0.0273 O4 0.0577 0.0509 0.0232 O5 0.0489 0.0407 0.0189 O6 0.0682 0.0513 0.0330 C110_b 0.1240 0.0521 0.0352 C111_b 0.0509 0.0256 0.0125 C31 0.0502 0.0217 0.0117 C32 0.0435 0.0215 0.0119 C33 0.0467 0.0248 0.0128 C34 0.0493 0.0207 0.0096 C35 0.0475 0.0253 0.0152 C36 0.0461 0.0235 0.0148 C37 0.0454 0.0166 0.0106 C38 0.0536 0.0273 0.0104 C39 0.0575 0.0390 0.0292 C40 0.0661 0.0513 0.0428 C41 0.0395 0.0242 0.0191 C42 0.0577 0.0296 0.0170 C43 0.0553 0.0384 0.0217 C44 0.0658 0.0397 0.0221 C45 0.0561 0.0491 0.0230 C46 0.0628 0.0369 0.0184 C47 0.0432 0.0205 0.0091 C48 0.0383 0.0235 0.0156 C49 0.0493 0.0205 0.0126 C50 0.0465 0.0192 0.0166 C51 0.0397 0.0308 0.0217 C52 0.0441 0.0277 0.0186 C53 0.0595 0.0547 0.0178 C54 0.0483 0.0215 0.0165 N31 0.0652 0.0271 0.0231 O31 0.0593 0.0314 0.0185 O32 0.0432 0.0202 0.0119 O33 0.0539 0.0481 0.0240 O34 0.0538 0.0371 0.0183 O35 0.0460 0.0386 0.0182 O36 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.012 0.018 0.024 0.031 0.039 0.049 0.063 0.084 0.124 1.000 Number in group 1092. 862. 931. 926. 942. 952. 989. 908. 955. 943. GooF 0.949 1.112 1.380 1.574 1.560 1.638 1.806 1.644 1.360 1.228 K 1.108 1.065 1.089 1.057 1.101 1.106 1.128 1.095 1.075 1.056 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.64 inf Number in group 974. 938. 960. 934. 948. 968. 936. 936. 961. 945. GooF 1.102 1.223 1.215 1.244 1.279 1.581 1.537 1.656 1.651 1.787 K 1.053 1.075 1.087 1.092 1.067 1.092 1.084 1.082 1.069 1.056 R1 0.271 0.248 0.216 0.191 0.159 0.146 0.123 0.120 0.115 0.127 Recommended weighting scheme: WGHT 0.2000 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) -3 9 5 2.17 144.68 5.18 0.064 1.22 -5 4 10 1.59 118.77 4.83 0.058 1.13 3 -3 7 51.17 12.49 4.56 0.019 1.81 2 9 3 8.55 110.07 4.56 0.056 1.34 -4 9 3 8.41 108.29 4.47 0.056 1.19 4 10 4 -1.49 41.05 4.40 0.034 1.07 -3 8 6 10.49 85.77 4.34 0.050 1.27 -1 7 3 0.26 17.82 4.31 0.023 1.76 2 11 1 17.56 149.84 4.17 0.066 1.17 -5 -1 4 359.39 116.86 4.12 0.058 1.56 -4 0 3 632.83 203.98 4.11 0.077 1.97 3 6 10 19.42 125.56 4.11 0.060 1.19 -3 -2 4 62.48 19.78 4.08 0.024 2.28 3 -12 5 6.25 96.83 4.08 0.053 1.06 8 0 3 633.56 203.33 4.02 0.076 1.02 1 -12 5 17.67 129.25 4.02 0.061 1.13 -7 0 3 234.05 69.68 3.93 0.045 1.17 -4 7 2 16.25 94.30 3.93 0.052 1.40 4 9 4 0.74 43.48 3.92 0.035 1.14 -1 -4 4 489.49 173.22 3.91 0.071 2.76 -4 -2 3 549.76 195.88 3.90 0.075 1.91 -1 -3 5 587.55 213.97 3.87 0.078 2.86 -1 -4 8 317.80 115.61 3.87 0.058 1.96 2 -1 5 319.27 115.94 3.81 0.058 2.72 -4 -3 7 165.02 59.37 3.74 0.041 1.57 -4 -7 10 411.43 139.73 3.73 0.063 1.18 -1 -3 3 471.74 174.91 3.73 0.071 3.53 -5 -5 6 144.60 44.25 3.72 0.036 1.32 -4 10 5 -3.64 43.67 3.71 0.035 1.07 2 -3 3 152.50 53.71 3.70 0.039 2.86 2 -5 9 565.96 214.16 3.68 0.078 1.61 -1 -6 4 200.24 71.30 3.66 0.045 2.09 -8 -3 4 240.18 84.35 3.64 0.049 0.99 -2 -4 5 39.61 13.13 3.61 0.019 2.25 5 10 3 -3.99 19.32 3.61 0.024 1.01 4 11 4 2.16 37.68 3.61 0.033 1.00 2 -3 11 555.20 206.96 3.61 0.077 1.51 -3 0 1 162.14 61.86 3.59 0.042 2.74 -8 -1 1 257.50 95.47 3.57 0.052 1.03 -3 -10 17 403.51 142.56 3.57 0.064 0.86 7 -3 4 333.63 126.44 3.56 0.060 1.12 1 -8 2 6.57 36.54 3.56 0.032 1.70 -5 -6 11 574.04 218.32 3.55 0.079 1.08 2 -10 8 19.56 105.90 3.54 0.055 1.20 -2 -4 6 123.97 47.68 3.54 0.037 2.10 4 1 3 207.75 75.27 3.52 0.047 1.91 3 1 6 429.34 155.63 3.51 0.067 1.97 -3 8 4 24.20 101.31 3.50 0.054 1.35 10 -2 2 91.22 22.99 3.50 0.026 0.82 -5 -2 5 118.05 42.75 3.49 0.035 1.49 Bond lengths and angles C1 - Distance Angles O1 1.2022 (0.0061) N1 1.3987 (0.0064) 124.71 (0.46) C4 1.5143 (0.0066) 128.10 (0.45) 107.17 (0.42) C1 - O1 N1 C2 - Distance Angles O2 1.2092 (0.0060) N1 1.3862 (0.0062) 124.16 (0.45) C3 1.5124 (0.0065) 127.25 (0.46) 108.58 (0.42) C2 - O2 N1 C3 - Distance Angles C2 1.5124 (0.0065) C4 1.5391 (0.0070) 104.46 (0.39) C8 1.5638 (0.0059) 111.51 (0.38) 101.79 (0.36) H3 1.0000 112.76 112.76 112.76 C3 - C2 C4 C8 C4 - Distance Angles C1 1.5143 (0.0066) C3 1.5391 (0.0070) 105.82 (0.39) C5 1.5678 (0.0058) 110.28 (0.39) 102.01 (0.36) H4 1.0000 112.68 112.68 112.68 C4 - C1 C3 C5 C5 - Distance Angles O3 1.4348 (0.0057) C9 1.4971 (0.0073) 111.51 (0.40) C6 1.5326 (0.0066) 102.87 (0.36) 116.78 (0.41) C4 1.5678 (0.0058) 101.89 (0.37) 115.18 (0.38) 106.92 (0.39) C5 - O3 C9 C6 C6 - Distance Angles C5 1.5326 (0.0066) C7 1.5451 (0.0070) 101.88 (0.39) H6A 0.9900 111.39 111.39 H6B 0.9900 111.39 111.39 109.26 C6 - C5 C7 H6A C7 - Distance Angles C6 1.5451 (0.0070) C8 1.5609 (0.0066) 102.03 (0.39) H7A 0.9900 111.36 111.36 H7B 0.9900 111.36 111.36 109.23 C7 - C6 C8 H7A C8 - Distance Angles O3 1.4507 (0.0057) C18 1.4950 (0.0066) 113.35 (0.38) C7 1.5609 (0.0066) 102.22 (0.37) 115.13 (0.38) C3 1.5638 (0.0059) 100.50 (0.35) 116.51 (0.37) 107.26 (0.37) C8 - O3 C18 C7 C9 - Distance Angles O4 1.2064 (0.0063) O5 1.3275 (0.0062) 124.73 (0.50) C5 1.4971 (0.0073) 125.22 (0.47) 110.02 (0.44) C9 - O4 O5 C10_a - Distance Angles O5 1.4510 (0.0111) C11_a 1.4812 (0.0247) 107.96 (1.67) H10A_a 0.9900 110.11 110.11 H10B_a 0.9900 110.11 110.11 108.44 C10_a - O5 C11_a H10A_a C11_a - Distance Angles C10_a 1.4812 (0.0249) H11A_a 0.9800 109.47 H11B_a 0.9800 109.47 109.47 H11C_a 0.9800 109.47 109.47 109.47 C11_a - C10_a H11A_a H11B_a C12 - Distance Angles C17 1.3838 (0.0065) C13 1.3878 (0.0073) 121.07 (0.48) N1 1.4399 (0.0060) 118.75 (0.45) 120.17 (0.43) C12 - C17 C13 C13 - Distance Angles C12 1.3878 (0.0073) C14 1.3924 (0.0078) 119.16 (0.49) H13 0.9500 120.42 120.42 C13 - C12 C14 C14 - Distance Angles C15 1.3912 (0.0078) C13 1.3924 (0.0078) 119.43 (0.54) H14 0.9500 120.29 120.29 C14 - C15 C13 C15 - Distance Angles C16 1.3786 (0.0083) C14 1.3912 (0.0078) 120.78 (0.52) H15 0.9500 119.61 119.61 C15 - C16 C14 C16 - Distance Angles C15 1.3786 (0.0083) C17 1.3810 (0.0072) 119.97 (0.50) H16 0.9500 120.01 120.01 C16 - C15 C17 C17 - Distance Angles C16 1.3810 (0.0072) C12 1.3838 (0.0065) 119.55 (0.52) H17 0.9500 120.23 120.22 C17 - C16 C12 C18 - Distance Angles C19 1.3917 (0.0064) C23 1.3917 (0.0066) 118.58 (0.45) C8 1.4950 (0.0066) 121.06 (0.43) 120.35 (0.43) C18 - C19 C23 C19 - Distance Angles C18 1.3917 (0.0064) C20 1.4003 (0.0069) 120.61 (0.45) H19 0.9500 119.69 119.69 C19 - C18 C20 C20 - Distance Angles C21 1.3655 (0.0069) C19 1.4003 (0.0069) 119.79 (0.45) H20 0.9500 120.10 120.10 C20 - C21 C19 C21 - Distance Angles C20 1.3655 (0.0069) O6 1.3794 (0.0058) 124.49 (0.45) C22 1.4017 (0.0069) 120.20 (0.46) 115.30 (0.44) C21 - C20 O6 C22 - Distance Angles C23 1.3753 (0.0069) C21 1.4017 (0.0069) 119.75 (0.45) H22 0.9500 120.13 120.13 C22 - C23 C21 C23 - Distance Angles C22 1.3753 (0.0069) C18 1.3917 (0.0066) 121.00 (0.45) H23 0.9500 119.50 119.50 C23 - C22 C18 C24 - Distance Angles O6 1.4269 (0.0059) H24A 0.9800 109.47 H24B 0.9800 109.47 109.47 H24C 0.9800 109.47 109.47 109.47 C24 - O6 H24A H24B N1 - Distance Angles C2 1.3862 (0.0062) C1 1.3987 (0.0064) 113.65 (0.41) C12 1.4399 (0.0060) 123.67 (0.41) 122.57 (0.41) N1 - C2 C1 O1 - Distance Angles C1 1.2022 (0.0061) O1 - O2 - Distance Angles C2 1.2092 (0.0060) O2 - O3 - Distance Angles C5 1.4348 (0.0057) C8 1.4507 (0.0057) 98.57 (0.35) O3 - C5 O4 - Distance Angles C9 1.2064 (0.0063) O4 - O5 - Distance Angles C9 1.3275 (0.0063) C110_b 1.4477 (0.0154) 113.80 (1.89) C10_a 1.4510 (0.0111) 117.68 (1.10) 8.74 (5.00) O5 - C9 C110_b O6 - Distance Angles C21 1.3794 (0.0058) C24 1.4269 (0.0060) 115.98 (0.38) O6 - C21 C110_b - Distance Angles O5 1.4477 (0.0154) C111_b 1.4859 (0.0273) 108.29 (2.25) H10C_b 0.9900 110.04 110.04 H10D_b 0.9900 110.04 110.04 108.39 C110_b - O5 C111_b H10C_b C111_b - Distance Angles C110_b 1.4859 (0.0274) H11D_b 0.9800 109.47 H11E_b 0.9800 109.47 109.47 H11F_b 0.9800 109.47 109.47 109.47 C111_b - C110_b H11D_b H11E_b C31 - Distance Angles O31 1.2037 (0.0059) N31 1.4026 (0.0062) 125.17 (0.47) C34 1.5080 (0.0070) 127.04 (0.45) 107.70 (0.41) C31 - O31 N31 C32 - Distance Angles O32 1.2174 (0.0056) N31 1.3728 (0.0063) 123.59 (0.45) C33 1.5201 (0.0065) 127.12 (0.47) 109.29 (0.40) C32 - O32 N31 C33 - Distance Angles C32 1.5201 (0.0065) C34 1.5442 (0.0066) 103.79 (0.39) C38 1.5721 (0.0055) 111.79 (0.36) 101.80 (0.34) H33 1.0000 112.87 112.87 112.87 C33 - C32 C34 C38 C34 - Distance Angles C31 1.5080 (0.0071) C33 1.5442 (0.0066) 105.74 (0.39) C35 1.5610 (0.0055) 111.54 (0.39) 101.22 (0.34) H34 1.0000 112.54 112.54 112.54 C34 - C31 C33 C35 C35 - Distance Angles O33 1.4264 (0.0052) C39 1.5044 (0.0070) 111.32 (0.37) C36 1.5501 (0.0067) 103.16 (0.35) 115.43 (0.39) C34 1.5610 (0.0055) 102.35 (0.35) 115.83 (0.37) 107.23 (0.37) C35 - O33 C39 C36 C36 - Distance Angles C37 1.5221 (0.0068) C35 1.5501 (0.0067) 101.41 (0.38) H36A 0.9900 111.49 111.49 H36B 0.9900 111.49 111.49 109.32 C36 - C37 C35 H36A C37 - Distance Angles C36 1.5221 (0.0067) C38 1.5480 (0.0065) 102.72 (0.39) H37A 0.9900 111.22 111.22 H37B 0.9900 111.22 111.22 109.14 C37 - C36 C38 H37A C38 - Distance Angles O33 1.4445 (0.0057) C48 1.4989 (0.0060) 112.97 (0.35) C37 1.5480 (0.0065) 102.10 (0.35) 115.12 (0.38) C33 1.5721 (0.0055) 100.74 (0.34) 116.55 (0.36) 107.50 (0.34) C38 - O33 C48 C37 C39 - Distance Angles O34 1.1994 (0.0061) O35 1.3503 (0.0056) 124.38 (0.48) C35 1.5044 (0.0070) 125.24 (0.44) 110.37 (0.42) C39 - O34 O35 C40 - Distance Angles O35 1.4669 (0.0061) C41 1.4866 (0.0083) 111.08 (0.47) H40A 0.9900 109.42 109.42 H40B 0.9900 109.42 109.42 108.03 C40 - O35 C41 H40A C41 - Distance Angles C40 1.4866 (0.0083) H41A 0.9800 109.47 H41B 0.9800 109.47 109.47 H41C 0.9800 109.47 109.47 109.47 C41 - C40 H41A H41B C42 - Distance Angles C43 1.3775 (0.0061) C47 1.3889 (0.0073) 120.19 (0.49) N31 1.4356 (0.0062) 119.51 (0.44) 120.30 (0.42) C42 - C43 C47 C43 - Distance Angles C44 1.3761 (0.0075) C42 1.3775 (0.0061) 120.01 (0.50) H43 0.9500 120.00 120.00 C43 - C44 C42 C44 - Distance Angles C45 1.3726 (0.0082) C43 1.3761 (0.0075) 120.04 (0.49) H44 0.9500 119.98 119.98 C44 - C45 C43 C45 - Distance Angles C44 1.3726 (0.0082) C46 1.3759 (0.0078) 120.07 (0.52) H45 0.9500 119.96 119.96 C45 - C44 C46 C46 - Distance Angles C45 1.3759 (0.0078) C47 1.3765 (0.0082) 120.59 (0.53) H46 0.9500 119.70 119.70 C46 - C45 C47 C47 - Distance Angles C46 1.3765 (0.0082) C42 1.3889 (0.0073) 119.09 (0.48) H47 0.9500 120.45 120.45 C47 - C46 C42 C48 - Distance Angles C53 1.3783 (0.0067) C49 1.3977 (0.0067) 118.36 (0.43) C38 1.4989 (0.0060) 120.03 (0.42) 121.60 (0.43) C48 - C53 C49 C49 - Distance Angles C48 1.3977 (0.0067) C50 1.4021 (0.0063) 120.53 (0.45) H49 0.9500 119.73 119.73 C49 - C48 C50 C50 - Distance Angles C51 1.3625 (0.0069) C49 1.4021 (0.0063) 120.25 (0.44) H50 0.9500 119.87 119.87 C50 - C51 C49 C51 - Distance Angles C50 1.3625 (0.0069) O36 1.3779 (0.0056) 124.91 (0.43) C52 1.3952 (0.0071) 120.09 (0.44) 114.98 (0.45) C51 - C50 O36 C52 - Distance Angles C51 1.3952 (0.0071) C53 1.3986 (0.0066) 119.43 (0.46) H52 0.9500 120.28 120.28 C52 - C51 C53 C53 - Distance Angles C48 1.3783 (0.0067) C52 1.3986 (0.0066) 121.22 (0.46) H53 0.9500 119.39 119.39 C53 - C48 C52 C54 - Distance Angles O36 1.4255 (0.0063) H54A 0.9800 109.47 H54B 0.9800 109.47 109.47 H54C 0.9800 109.47 109.47 109.47 C54 - O36 H54A H54B N31 - Distance Angles C32 1.3728 (0.0063) C31 1.4026 (0.0062) 113.11 (0.41) C42 1.4356 (0.0062) 124.70 (0.39) 121.83 (0.40) N31 - C32 C31 O31 - Distance Angles C31 1.2037 (0.0059) O31 - O32 - Distance Angles C32 1.2174 (0.0056) O32 - O33 - Distance Angles C35 1.4264 (0.0052) C38 1.4445 (0.0057) 98.18 (0.32) O33 - C35 O34 - Distance Angles C39 1.1994 (0.0061) O34 - O35 - Distance Angles C39 1.3503 (0.0056) C40 1.4669 (0.0061) 116.85 (0.42) O35 - C39 O36 - Distance Angles C51 1.3779 (0.0056) C54 1.4255 (0.0063) 116.92 (0.39) O36 - C51 FMAP and GRID set by program FMAP 2 1 38 GRID -2.857 -2 -1 2.857 2 1 R1 = 0.1409 for 9500 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.78 at 0.7718 0.1335 0.4844 [ 0.95 A from O5 ] Deepest hole -0.89 at 0.2740 0.8597 0.0133 [ 0.74 A from O35 ] Mean = 0.00, Rms deviation from mean = 0.14 e/A^3, Highest memory used = 6284 / 58856 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2282 0.8665 0.5156 1.00000 0.05 0.78 0.95 O5 0.96 C110 1.02 C10 1.45 C11 Q2 1 0.5034 0.8839 0.5522 1.00000 0.05 0.73 1.02 O4 1.41 H10B 1.58 H10D 1.71 C9 Q3 1 0.0996 0.2937 0.0282 1.00000 0.05 0.70 1.10 O33 1.65 C35 1.78 O34 1.85 C39 Q4 1 0.4146 0.7210 0.4681 1.00000 0.05 0.66 0.74 C5 1.03 C9 1.59 C6 1.82 O3 Q5 1 0.3902 0.4593 0.3713 1.00000 0.05 0.64 0.85 H7A 1.07 C7 1.28 H7B 1.87 H23 Shortest distances between peaks (including symmetry equivalents) 1 2 2.37 1 4 2.62 2 4 2.63 Time profile in seconds ----------------------- 0.23: 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. 1.13: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 5.55: Structure factors and derivatives 31.50: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 2.03: Solve l.s. equations 0.00: Generate HTAB table 0.13: Other dependent quantities, CIF, tables 0.42: Analysis of variance 0.08: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008src0843 finished at 12:03:51 Total CPU time: 41.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++