+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 16:22:37 on 14-Jun-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0647 in P2(1)/n CELL 0.71073 11.3163 11.8126 33.2617 90.000 99.350 90.000 ZERR 4.00 0.0003 0.0002 0.0007 0.000 0.001 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H S BR UNIT 184 232 12 8 V = 4387.18 F(000) = 1808.0 Mu = 2.02 mm-1 Cell Wt = 3467.70 Rho = 1.313 MERG 2 OMIT -3.00 55.00 OMIT -2 0 8 OMIT -7 0 23 OMIT 2 2 2 OMIT -8 2 26 OMIT -5 1 21 FMAP 2 PLAN 20 SIZE 0.04 0.10 0.40 ACTA BOND WGHT 0.04160 8.40250 L.S. 4 TEMP -153.00 FVAR 0.09211 C1 1 0.762055 0.332074 -0.169488 11.00000 0.01959 0.02016 = 0.02372 -0.00066 -0.00015 0.00427 C2 1 0.825782 0.421356 -0.148896 11.00000 0.01861 0.02339 = 0.01924 0.00110 0.00034 0.00390 C3 1 0.809616 0.427312 -0.107587 11.00000 0.02014 0.02157 = 0.02001 -0.00056 -0.00084 0.00695 C4 1 0.737444 0.343188 -0.097594 11.00000 0.02468 0.02254 = 0.02060 0.00036 0.00072 0.00701 C5 1 0.714209 0.350355 -0.053941 11.00000 0.02733 0.02229 = 0.02435 0.00274 0.00486 0.00307 C6 1 0.787377 0.457713 -0.040618 11.00000 0.02439 0.02236 = 0.02348 0.00151 0.00230 0.00643 C7 1 0.804697 0.509937 -0.002822 11.00000 0.02228 0.03058 = 0.01902 0.00034 0.00152 0.00714 AFIX 43 H7 2 0.770082 0.479902 0.019076 11.00000 -1.20000 AFIX 0 C8 1 0.873794 0.607008 0.002121 11.00000 0.02414 0.02806 = 0.02222 -0.00392 -0.00364 0.00938 C9 1 0.926082 0.652855 -0.029103 11.00000 0.01982 0.02922 = 0.02463 -0.00162 -0.00285 0.00210 AFIX 43 H9 2 0.971378 0.720738 -0.024773 11.00000 -1.20000 AFIX 0 C10 1 0.911988 0.599068 -0.066845 11.00000 0.02319 0.02858 = 0.02086 -0.00163 -0.00015 0.00464 AFIX 43 H10 2 0.949092 0.628081 -0.088340 11.00000 -1.20000 AFIX 0 C11 1 0.842368 0.502095 -0.072167 11.00000 0.01946 0.02407 = 0.01793 -0.00223 0.00012 0.00758 C12 1 0.770899 0.250580 -0.027150 11.00000 0.03666 0.03395 = 0.02360 0.00453 -0.00087 0.00409 AFIX 23 H12A 2 0.857176 0.247302 -0.029139 11.00000 -1.20000 H12B 2 0.764699 0.267695 0.001570 11.00000 -1.20000 AFIX 0 C13 1 0.717560 0.134448 -0.037278 11.00000 0.03685 0.02934 = 0.03499 0.00388 -0.00062 0.00114 AFIX 23 H13A 2 0.724048 0.114929 -0.065782 11.00000 -1.20000 H13B 2 0.631616 0.135132 -0.034719 11.00000 -1.20000 AFIX 0 C14 1 0.783599 0.044777 -0.008293 11.00000 0.04784 0.03931 = 0.05511 0.01379 -0.00798 0.00639 AFIX 23 H14A 2 0.767218 0.058398 0.019650 11.00000 -1.20000 H14B 2 0.870956 0.052371 -0.007781 11.00000 -1.20000 AFIX 0 C15 1 0.743903 -0.077669 -0.021674 11.00000 0.04452 0.03581 = 0.05784 0.01855 0.02003 0.01554 AFIX 23 H15A 2 0.758079 -0.089505 -0.049969 11.00000 -1.20000 H15B 2 0.795053 -0.131994 -0.004053 11.00000 -1.20000 AFIX 0 C16 1 0.616104 -0.103803 -0.019792 11.00000 0.05017 0.04737 = 0.03698 0.00830 0.00682 0.00361 AFIX 23 H16A 2 0.564104 -0.054194 -0.039121 11.00000 -1.20000 H16B 2 0.599701 -0.087300 0.007958 11.00000 -1.20000 AFIX 0 C17 1 0.585651 -0.225665 -0.030046 11.00000 0.06605 0.04083 = 0.05445 0.01099 0.00779 0.00294 AFIX 137 H17A 2 0.614534 -0.246072 -0.055312 11.00000 -1.50000 H17B 2 0.498621 -0.235841 -0.033655 11.00000 -1.50000 H17C 2 0.623987 -0.274363 -0.007844 11.00000 -1.50000 AFIX 0 C18 1 0.580401 0.366678 -0.052206 11.00000 0.02801 0.03143 = 0.02532 0.00088 0.00680 -0.00211 AFIX 23 H18A 2 0.535932 0.300119 -0.064876 11.00000 -1.20000 H18B 2 0.569428 0.369232 -0.023291 11.00000 -1.20000 AFIX 0 C19 1 0.526082 0.473248 -0.073428 11.00000 0.02408 0.03489 = 0.07247 0.00850 0.01248 0.00255 AFIX 23 H19A 2 0.552252 0.538921 -0.055711 11.00000 -1.20000 H19B 2 0.559542 0.483128 -0.098917 11.00000 -1.20000 AFIX 0 C20 1 0.394097 0.476151 -0.083678 11.00000 0.02732 0.07091 = 0.04668 0.01542 0.00530 0.00739 AFIX 23 H20A 2 0.360560 0.457385 -0.058798 11.00000 -1.20000 H20B 2 0.368589 0.415878 -0.103913 11.00000 -1.20000 AFIX 0 C21 1 0.340014 0.585153 -0.100267 11.00000 0.02963 0.04749 = 0.08208 -0.00040 0.00851 0.00186 AFIX 23 H21A 2 0.355906 0.641789 -0.078108 11.00000 -1.20000 H21B 2 0.385049 0.609825 -0.121872 11.00000 -1.20000 AFIX 0 C22 1 0.212936 0.592705 -0.117160 11.00000 0.03304 0.09664 = 0.08962 0.03895 0.00289 0.00526 AFIX 23 H22A 2 0.167304 0.564943 -0.096145 11.00000 -1.20000 H22B 2 0.197249 0.539467 -0.140403 11.00000 -1.20000 AFIX 0 C23 1 0.163055 0.702599 -0.131274 11.00000 0.03737 0.05260 = 0.12451 0.01816 0.00764 0.01110 AFIX 137 H23A 2 0.156619 0.750723 -0.107727 11.00000 -1.50000 H23B 2 0.083424 0.691800 -0.147456 11.00000 -1.50000 H23C 2 0.215691 0.738926 -0.148098 11.00000 -1.50000 AFIX 0 C24 1 0.777425 0.327112 -0.210974 11.00000 0.01930 0.02379 = 0.02317 -0.00298 0.00155 0.00392 C25 1 0.853868 0.410839 -0.220830 11.00000 0.02040 0.02074 = 0.02435 -0.00268 0.00111 0.00158 C26 1 0.872131 0.403352 -0.262167 11.00000 0.02062 0.02264 = 0.02147 -0.00342 0.00036 -0.00026 C27 1 0.808142 0.317096 -0.282195 11.00000 0.01988 0.02351 = 0.02398 -0.00373 0.00228 -0.00119 C28 1 0.827253 0.303385 -0.325844 11.00000 0.02308 0.02568 = 0.01830 -0.00315 0.00168 -0.00516 C29 1 0.920684 0.396505 -0.326994 11.00000 0.01866 0.02631 = 0.02233 -0.00363 -0.00093 -0.00047 C30 1 0.977416 0.425827 -0.359198 11.00000 0.02603 0.03353 = 0.01975 -0.00667 0.00218 -0.00748 AFIX 43 H30 2 0.961484 0.386224 -0.384355 11.00000 -1.20000 AFIX 0 C31 1 1.058840 0.515303 -0.353744 11.00000 0.02460 0.03428 = 0.02380 -0.00088 0.00195 -0.00575 C32 1 1.083200 0.575063 -0.317520 11.00000 0.02191 0.02875 = 0.03044 0.00040 0.00503 -0.00559 AFIX 43 H32 2 1.138864 0.635876 -0.314818 11.00000 -1.20000 AFIX 0 C33 1 1.025500 0.545423 -0.285014 11.00000 0.02546 0.02388 = 0.02226 -0.00587 -0.00019 -0.00125 AFIX 43 H33 2 1.041386 0.585640 -0.259983 11.00000 -1.20000 AFIX 0 C34 1 0.944380 0.456097 -0.289832 11.00000 0.02095 0.02281 = 0.02057 -0.00297 0.00488 0.00012 C35 1 0.711711 0.327350 -0.356272 11.00000 0.02465 0.03165 = 0.02125 -0.00310 0.00085 -0.00575 AFIX 23 H35A 2 0.729483 0.319734 -0.384324 11.00000 -1.20000 H35B 2 0.651254 0.269295 -0.352620 11.00000 -1.20000 AFIX 0 C36 1 0.658268 0.443976 -0.351710 11.00000 0.02736 0.03462 = 0.03822 0.00211 -0.00298 -0.00262 AFIX 23 H36A 2 0.642396 0.452368 -0.323456 11.00000 -1.20000 H36B 2 0.717923 0.502095 -0.356082 11.00000 -1.20000 AFIX 0 C37 1 0.543114 0.466139 -0.380931 11.00000 0.02682 0.04310 = 0.02820 0.00336 -0.00121 -0.00666 AFIX 23 H37A 2 0.482381 0.409989 -0.375769 11.00000 -1.20000 H37B 2 0.558151 0.454604 -0.409145 11.00000 -1.20000 AFIX 0 C38 1 0.492483 0.584281 -0.377541 11.00000 0.02513 0.03981 = 0.04274 0.01326 -0.00034 -0.00342 AFIX 23 H38A 2 0.421832 0.593638 -0.399119 11.00000 -1.20000 H38B 2 0.553360 0.640225 -0.382751 11.00000 -1.20000 AFIX 0 C39 1 0.455548 0.610983 -0.336653 11.00000 0.04216 0.04320 = 0.03973 0.00251 0.00133 0.00199 AFIX 23 H39A 2 0.526795 0.605684 -0.315100 11.00000 -1.20000 H39B 2 0.397063 0.553481 -0.330754 11.00000 -1.20000 AFIX 0 C40 1 0.400271 0.727878 -0.335169 11.00000 0.03888 0.04202 = 0.06575 -0.00827 -0.00327 -0.00293 AFIX 137 H40A 2 0.457710 0.785340 -0.340928 11.00000 -1.50000 H40B 2 0.379899 0.741005 -0.308018 11.00000 -1.50000 H40C 2 0.327564 0.732654 -0.355604 11.00000 -1.50000 AFIX 0 C41 1 0.875954 0.184413 -0.333120 11.00000 0.02458 0.02739 = 0.02709 -0.00719 0.00262 -0.00475 AFIX 23 H41A 2 0.812707 0.128132 -0.330652 11.00000 -1.20000 H41B 2 0.892591 0.180713 -0.361406 11.00000 -1.20000 AFIX 0 C42 1 0.989664 0.150532 -0.304117 11.00000 0.02592 0.02890 = 0.03438 -0.00864 0.00156 -0.00389 AFIX 23 H42A 2 1.060259 0.181789 -0.314393 11.00000 -1.20000 H42B 2 0.987519 0.184032 -0.276962 11.00000 -1.20000 AFIX 0 C43 1 1.003159 0.023348 -0.299834 11.00000 0.03669 0.02583 = 0.06837 -0.00778 -0.01125 -0.00263 AFIX 23 H43A 2 1.003282 -0.009692 -0.327181 11.00000 -1.20000 H43B 2 0.932616 -0.007185 -0.289328 11.00000 -1.20000 AFIX 0 C44 1 1.115723 -0.014783 -0.271856 11.00000 0.03678 0.02826 = 0.04539 -0.00760 0.00013 0.00052 AFIX 23 H44A 2 1.186573 0.010895 -0.283336 11.00000 -1.20000 H44B 2 1.118543 0.022004 -0.244974 11.00000 -1.20000 AFIX 0 C45 1 1.122908 -0.140938 -0.265955 11.00000 0.06135 0.03037 = 0.15312 0.00133 -0.04694 0.00003 AFIX 23 H45A 2 1.120048 -0.177298 -0.292913 11.00000 -1.20000 H45B 2 1.051477 -0.166271 -0.254740 11.00000 -1.20000 AFIX 0 C46 1 1.233193 -0.181654 -0.238201 11.00000 0.06067 0.03726 = 0.08766 0.00177 -0.01446 0.00800 AFIX 137 H46A 2 1.304496 -0.161550 -0.249885 11.00000 -1.50000 H46B 2 1.229370 -0.264052 -0.235230 11.00000 -1.50000 H46C 2 1.237498 -0.145863 -0.211422 11.00000 -1.50000 AFIX 0 S1 3 0.682843 0.255462 -0.138124 11.00000 0.02604 0.02175 = 0.02070 -0.00063 0.00299 -0.00043 S2 3 0.906868 0.498426 -0.179701 11.00000 0.02089 0.02317 = 0.01942 -0.00388 0.00129 -0.00061 S3 3 0.725527 0.239943 -0.252110 11.00000 0.02452 0.02544 = 0.02007 -0.00275 0.00268 -0.00532 BR1 4 0.895429 0.682042 0.053555 11.00000 0.03130 0.03742 = 0.02232 -0.00826 0.00060 0.00419 BR2 4 1.135923 0.558424 -0.398060 11.00000 0.03926 0.06586 = 0.02856 -0.00388 0.01086 -0.02484 HKLF 4 Covalent radii and connectivity table for 2009src0647 in P2(1)/n C 0.770 H 0.320 S 1.030 BR 1.140 C1 - C2 C24 S1 C2 - C1 C3 S2 C3 - C4 C2 C11 C4 - C3 C5 S1 C5 - C4 C18 C6 C12 C6 - C7 C11 C5 C7 - C8 C6 C8 - C7 C9 Br1 C9 - C8 C10 C10 - C11 C9 C11 - C10 C6 C3 C12 - C13 C5 C13 - C12 C14 C14 - C13 C15 C15 - C16 C14 C16 - C15 C17 C17 - C16 C18 - C19 C5 C19 - C20 C18 C20 - C19 C21 C21 - C22 C20 C22 - C21 C23 C23 - C22 C24 - C25 C1 S3 C25 - C24 C26 S2 C26 - C27 C25 C34 C27 - C26 C28 S3 C28 - C27 C29 C41 C35 C29 - C30 C34 C28 C30 - C29 C31 C31 - C32 C30 Br2 C32 - C31 C33 C33 - C34 C32 C34 - C33 C29 C26 C35 - C36 C28 C36 - C37 C35 C37 - C36 C38 C38 - C39 C37 C39 - C38 C40 C40 - C39 C41 - C42 C28 C42 - C43 C41 C43 - C42 C44 C44 - C45 C43 C45 - C44 C46 C46 - C45 S1 - C4 C1 S2 - C2 C25 S3 - C27 C24 Br1 - C8 Br2 - C31 49377 Reflections read, of which 1288 rejected -14 =< h =< 14, -15 =< k =< 13, -43 =< l =< 43, Max. 2-theta = 54.99 0 Systematic absence violations 0 Inconsistent equivalents 10019 Unique reflections, of which 0 suppressed R(int) = 0.0706 R(sigma) = 0.0595 Friedel opposites merged Maximum memory for data reduction = 4655 / 100146 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 = 6064 / 606011 wR2 = 0.1255 before cycle 1 for 10019 data and 464 / 464 parameters GooF = S = 1.039; Restrained GooF = 1.039 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0416 * P )^2 + 8.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.09208 0.00012 -0.238 OSF Mean shift/esd = 0.016 Maximum = -0.238 for OSF Max. shift = 0.002 A for H17C Max. dU = 0.000 for C32 Least-squares cycle 2 Maximum vector length = 511 Memory required = 6064 / 606011 wR2 = 0.1255 before cycle 2 for 10019 data and 464 / 464 parameters GooF = S = 1.039; Restrained GooF = 1.039 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0416 * P )^2 + 8.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.09208 0.00012 -0.042 OSF Mean shift/esd = 0.005 Maximum = -0.042 for OSF Max. shift = 0.001 A for H17C Max. dU = 0.000 for C32 Least-squares cycle 3 Maximum vector length = 511 Memory required = 6064 / 606011 wR2 = 0.1255 before cycle 3 for 10019 data and 464 / 464 parameters GooF = S = 1.039; Restrained GooF = 1.039 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0416 * P )^2 + 8.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.09208 0.00012 -0.001 OSF Mean shift/esd = 0.000 Maximum = 0.005 for tors H23A Max. shift = 0.000 A for H23A Max. dU = 0.000 for C14 Least-squares cycle 4 Maximum vector length = 511 Memory required = 6064 / 606011 wR2 = 0.1255 before cycle 4 for 10019 data and 464 / 464 parameters GooF = S = 1.039; Restrained GooF = 1.039 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0416 * P )^2 + 8.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.09208 0.00012 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.002 for tors H23A Max. shift = 0.000 A for H23A Max. dU = 0.000 for C22 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H7 0.7701 0.4799 0.0191 43 0.950 0.000 C7 C8 C6 H9 0.9714 0.7207 -0.0248 43 0.950 0.000 C9 C8 C10 H10 0.9491 0.6281 -0.0883 43 0.950 0.000 C10 C11 C9 H12A 0.8572 0.2473 -0.0291 23 0.990 0.000 C12 C13 C5 H12B 0.7647 0.2677 0.0016 23 0.990 0.000 C12 C13 C5 H13A 0.7241 0.1149 -0.0658 23 0.990 0.000 C13 C12 C14 H13B 0.6316 0.1351 -0.0347 23 0.990 0.000 C13 C12 C14 H14A 0.7672 0.0584 0.0197 23 0.990 0.000 C14 C13 C15 H14B 0.8709 0.0524 -0.0078 23 0.990 0.000 C14 C13 C15 H15A 0.7580 -0.0895 -0.0500 23 0.990 0.000 C15 C16 C14 H15B 0.7951 -0.1320 -0.0041 23 0.990 0.000 C15 C16 C14 H16A 0.5641 -0.0542 -0.0391 23 0.990 0.000 C16 C15 C17 H16B 0.5997 -0.0873 0.0080 23 0.990 0.000 C16 C15 C17 H17A 0.6144 -0.2460 -0.0554 137 0.980 0.000 C17 C16 H17A H17B 0.4987 -0.2359 -0.0336 137 0.980 0.000 C17 C16 H17A H17C 0.6242 -0.2744 -0.0079 137 0.980 0.000 C17 C16 H17A H18A 0.5359 0.3001 -0.0649 23 0.990 0.000 C18 C19 C5 H18B 0.5694 0.3692 -0.0233 23 0.990 0.000 C18 C19 C5 H19A 0.5523 0.5389 -0.0557 23 0.990 0.000 C19 C20 C18 H19B 0.5595 0.4831 -0.0989 23 0.990 0.000 C19 C20 C18 H20A 0.3606 0.4574 -0.0588 23 0.990 0.000 C20 C19 C21 H20B 0.3686 0.4159 -0.1039 23 0.990 0.000 C20 C19 C21 H21A 0.3559 0.6418 -0.0781 23 0.990 0.000 C21 C22 C20 H21B 0.3850 0.6098 -0.1219 23 0.990 0.000 C21 C22 C20 H22A 0.1673 0.5650 -0.0961 23 0.990 0.000 C22 C21 C23 H22B 0.1972 0.5395 -0.1404 23 0.990 0.000 C22 C21 C23 H23A 0.1567 0.7508 -0.1077 137 0.980 0.000 C23 C22 H23A H23B 0.0834 0.6918 -0.1474 137 0.980 0.000 C23 C22 H23A H23C 0.2157 0.7389 -0.1481 137 0.980 0.000 C23 C22 H23A H30 0.9615 0.3862 -0.3844 43 0.950 0.000 C30 C29 C31 H32 1.1389 0.6359 -0.3148 43 0.950 0.000 C32 C31 C33 H33 1.0414 0.5857 -0.2600 43 0.950 0.000 C33 C34 C32 H35A 0.7295 0.3197 -0.3843 23 0.990 0.000 C35 C36 C28 H35B 0.6512 0.2693 -0.3526 23 0.990 0.000 C35 C36 C28 H36A 0.6424 0.4524 -0.3235 23 0.990 0.000 C36 C37 C35 H36B 0.7179 0.5021 -0.3561 23 0.990 0.000 C36 C37 C35 H37A 0.4824 0.4100 -0.3758 23 0.990 0.000 C37 C36 C38 H37B 0.5581 0.4546 -0.4092 23 0.990 0.000 C37 C36 C38 H38A 0.5534 0.6402 -0.3827 23 0.990 0.000 C38 C39 C37 H38B 0.4219 0.5937 -0.3991 23 0.990 0.000 C38 C39 C37 H39A 0.5268 0.6056 -0.3151 23 0.990 0.000 C39 C38 C40 H39B 0.3970 0.5535 -0.3308 23 0.990 0.000 C39 C38 C40 H40A 0.4578 0.7853 -0.3409 137 0.980 0.000 C40 C39 H40A H40B 0.3798 0.7410 -0.3080 137 0.980 0.000 C40 C39 H40A H40C 0.3276 0.7327 -0.3556 137 0.980 0.000 C40 C39 H40A H41A 0.8127 0.1281 -0.3307 23 0.990 0.000 C41 C42 C28 H41B 0.8926 0.1807 -0.3614 23 0.990 0.000 C41 C42 C28 H42A 1.0603 0.1818 -0.3144 23 0.990 0.000 C42 C43 C41 H42B 0.9875 0.1840 -0.2770 23 0.990 0.000 C42 C43 C41 H43A 1.0033 -0.0097 -0.3272 23 0.990 0.000 C43 C42 C44 H43B 0.9326 -0.0072 -0.2893 23 0.990 0.000 C43 C42 C44 H44A 1.1866 0.0109 -0.2833 23 0.990 0.000 C44 C45 C43 H44B 1.1186 0.0220 -0.2450 23 0.990 0.000 C44 C45 C43 H45A 1.1200 -0.1773 -0.2929 23 0.990 0.000 C45 C44 C46 H45B 1.0515 -0.1662 -0.2547 23 0.990 0.000 C45 C44 C46 H46A 1.3045 -0.1615 -0.2499 137 0.980 0.000 C46 C45 H46A H46B 1.2294 -0.2641 -0.2352 137 0.980 0.000 C46 C45 H46A H46C 1.2375 -0.1459 -0.2114 137 0.980 0.000 C46 C45 H46A 2009src0647 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.76205 0.33208 -0.16949 1.00000 0.01955 0.02017 0.02367 -0.00066 -0.00013 0.00430 0.02153 0.00589 0.00029 0.00027 0.00010 0.00000 0.00163 0.00162 0.00159 0.00125 0.00130 0.00129 0.00067 C2 0.82579 0.42135 -0.14890 1.00000 0.01854 0.02337 0.01924 0.00111 0.00034 0.00389 0.02069 0.00587 0.00029 0.00027 0.00009 0.00000 0.00159 0.00163 0.00149 0.00124 0.00124 0.00130 0.00065 C3 0.80962 0.42732 -0.10759 1.00000 0.02008 0.02156 0.02001 -0.00058 -0.00084 0.00692 0.02101 0.00589 0.00029 0.00027 0.00009 0.00000 0.00163 0.00162 0.00153 0.00125 0.00125 0.00132 0.00066 C4 0.73744 0.34319 -0.09759 1.00000 0.02465 0.02250 0.02057 0.00036 0.00072 0.00703 0.02290 0.00611 0.00031 0.00027 0.00010 0.00000 0.00177 0.00168 0.00156 0.00126 0.00132 0.00136 0.00070 C5 0.71422 0.35036 -0.05394 1.00000 0.02728 0.02226 0.02433 0.00277 0.00487 0.00305 0.02455 0.00635 0.00032 0.00028 0.00010 0.00000 0.00185 0.00169 0.00165 0.00131 0.00140 0.00140 0.00071 C6 0.78737 0.45770 -0.04061 1.00000 0.02434 0.02228 0.02346 0.00148 0.00225 0.00644 0.02354 0.00621 0.00031 0.00028 0.00010 0.00000 0.00175 0.00166 0.00162 0.00130 0.00135 0.00138 0.00070 C7 0.80471 0.50992 -0.00282 1.00000 0.02236 0.03057 0.01898 0.00038 0.00154 0.00718 0.02417 0.00613 0.00030 0.00029 0.00010 0.00000 0.00175 0.00184 0.00154 0.00133 0.00131 0.00143 0.00071 H7 0.77011 0.47988 0.01908 1.00000 0.02901 0.00000 0.00000 C8 0.87379 0.60701 0.00212 1.00000 0.02406 0.02804 0.02223 -0.00393 -0.00367 0.00934 0.02560 0.00620 0.00031 0.00029 0.00010 0.00000 0.00179 0.00180 0.00163 0.00134 0.00135 0.00143 0.00074 C9 0.92608 0.65286 -0.02910 1.00000 0.01977 0.02917 0.02468 -0.00158 -0.00283 0.00211 0.02526 0.00617 0.00030 0.00030 0.00010 0.00000 0.00171 0.00183 0.00166 0.00136 0.00136 0.00139 0.00073 H9 0.97136 0.72075 -0.02478 1.00000 0.03031 0.00000 0.00000 C10 0.91199 0.59907 -0.06685 1.00000 0.02318 0.02849 0.02090 -0.00160 -0.00017 0.00463 0.02460 0.00603 0.00030 0.00029 0.00010 0.00000 0.00176 0.00181 0.00157 0.00132 0.00133 0.00142 0.00072 H10 0.94911 0.62807 -0.08834 1.00000 0.02953 0.00000 0.00000 C11 0.84235 0.50209 -0.07217 1.00000 0.01938 0.02405 0.01791 -0.00223 0.00009 0.00757 0.02078 0.00582 0.00029 0.00027 0.00009 0.00000 0.00164 0.00167 0.00148 0.00125 0.00125 0.00132 0.00067 C12 0.77089 0.25056 -0.02714 1.00000 0.03671 0.03395 0.02356 0.00451 -0.00096 0.00401 0.03206 0.00678 0.00035 0.00031 0.00011 0.00000 0.00215 0.00204 0.00171 0.00148 0.00153 0.00168 0.00083 H12A 0.85717 0.24728 -0.02912 1.00000 0.03847 0.00000 0.00000 H12B 0.76466 0.26767 0.00157 1.00000 0.03847 0.00000 0.00000 C13 0.71757 0.13446 -0.03728 1.00000 0.03693 0.02935 0.03499 0.00392 -0.00064 0.00115 0.03448 0.00701 0.00037 0.00031 0.00012 0.00000 0.00221 0.00198 0.00202 0.00158 0.00168 0.00167 0.00086 H13A 0.72410 0.11495 -0.06578 1.00000 0.04137 0.00000 0.00000 H13B 0.63162 0.13515 -0.03473 1.00000 0.04137 0.00000 0.00000 C14 0.78358 0.04477 -0.00829 1.00000 0.04788 0.03928 0.05521 0.01374 -0.00798 0.00646 0.04928 0.00847 0.00043 0.00036 0.00014 0.00000 0.00273 0.00243 0.00274 0.00203 0.00217 0.00205 0.00115 H14A 0.76716 0.05839 0.01965 1.00000 0.05914 0.00000 0.00000 H14B 0.87094 0.05236 -0.00776 1.00000 0.05914 0.00000 0.00000 C15 0.74389 -0.07767 -0.02168 1.00000 0.04454 0.03578 0.05797 0.01864 0.02003 0.01555 0.04480 0.00897 0.00040 0.00034 0.00014 0.00000 0.00255 0.00226 0.00271 0.00197 0.00215 0.00194 0.00107 H15A 0.75804 -0.08948 -0.04998 1.00000 0.05376 0.00000 0.00000 H15B 0.79505 -0.13201 -0.00407 1.00000 0.05376 0.00000 0.00000 C16 0.61611 -0.10381 -0.01978 1.00000 0.05019 0.04733 0.03697 0.00832 0.00682 0.00362 0.04486 0.00825 0.00041 0.00037 0.00013 0.00000 0.00273 0.00256 0.00223 0.00188 0.00197 0.00212 0.00104 H16A 0.56410 -0.05419 -0.03910 1.00000 0.05383 0.00000 0.00000 H16B 0.59973 -0.08733 0.00797 1.00000 0.05383 0.00000 0.00000 C17 0.58568 -0.22567 -0.03005 1.00000 0.06611 0.04082 0.05446 0.01102 0.00771 0.00300 0.05403 0.00920 0.00048 0.00038 0.00015 0.00000 0.00335 0.00255 0.00284 0.00212 0.00245 0.00232 0.00123 H17A 0.61442 -0.24600 -0.05535 1.00000 0.08104 0.00000 0.00000 H17B 0.49866 -0.23590 -0.03361 1.00000 0.08104 0.00000 0.00000 H17C 0.62416 -0.27439 -0.00788 1.00000 0.08104 0.00000 0.00000 C18 0.58038 0.36667 -0.05221 1.00000 0.02806 0.03143 0.02523 0.00084 0.00682 -0.00212 0.02797 0.00664 0.00032 0.00031 0.00010 0.00000 0.00191 0.00191 0.00171 0.00144 0.00146 0.00153 0.00076 H18A 0.53593 0.30011 -0.06488 1.00000 0.03356 0.00000 0.00000 H18B 0.56940 0.36922 -0.02330 1.00000 0.03356 0.00000 0.00000 C19 0.52608 0.47323 -0.07343 1.00000 0.02404 0.03490 0.07249 0.00846 0.01255 0.00260 0.04329 0.00842 0.00035 0.00035 0.00015 0.00000 0.00204 0.00222 0.00303 0.00204 0.00201 0.00171 0.00104 H19A 0.55226 0.53890 -0.05571 1.00000 0.05194 0.00000 0.00000 H19B 0.55954 0.48311 -0.09892 1.00000 0.05194 0.00000 0.00000 C20 0.39409 0.47615 -0.08368 1.00000 0.02730 0.07087 0.04664 0.01548 0.00529 0.00738 0.04835 0.00899 0.00037 0.00042 0.00014 0.00000 0.00219 0.00317 0.00248 0.00224 0.00188 0.00213 0.00113 H20A 0.36055 0.45738 -0.05880 1.00000 0.05802 0.00000 0.00000 H20B 0.36857 0.41589 -0.10391 1.00000 0.05802 0.00000 0.00000 C21 0.34001 0.58516 -0.10026 1.00000 0.02957 0.04750 0.08220 -0.00040 0.00851 0.00185 0.05315 0.00896 0.00039 0.00040 0.00017 0.00000 0.00233 0.00269 0.00359 0.00240 0.00233 0.00198 0.00123 H21A 0.35592 0.64179 -0.07810 1.00000 0.06379 0.00000 0.00000 H21B 0.38504 0.60983 -0.12187 1.00000 0.06379 0.00000 0.00000 C22 0.21296 0.59275 -0.11715 1.00000 0.03309 0.09659 0.08954 0.03893 0.00299 0.00529 0.07385 0.01161 0.00044 0.00053 0.00019 0.00000 0.00268 0.00443 0.00421 0.00345 0.00269 0.00278 0.00175 H22A 0.16733 0.56504 -0.09612 1.00000 0.08862 0.00000 0.00000 H22B 0.19724 0.53947 -0.14038 1.00000 0.08862 0.00000 0.00000 C23 0.16308 0.70261 -0.13129 1.00000 0.03741 0.05257 0.12460 0.01821 0.00756 0.01104 0.07215 0.01113 0.00046 0.00044 0.00020 0.00000 0.00280 0.00315 0.00523 0.00317 0.00305 0.00237 0.00171 H23A 0.15669 0.75079 -0.10775 1.00000 0.10822 0.00000 0.00000 H23B 0.08342 0.69179 -0.14745 1.00000 0.10822 0.00000 0.00000 H23C 0.21568 0.73888 -0.14813 1.00000 0.10822 0.00000 0.00000 C24 0.77743 0.32711 -0.21097 1.00000 0.01928 0.02376 0.02314 -0.00296 0.00154 0.00394 0.02227 0.00593 0.00029 0.00028 0.00010 0.00000 0.00165 0.00167 0.00158 0.00129 0.00130 0.00133 0.00068 C25 0.85387 0.41086 -0.22083 1.00000 0.02036 0.02072 0.02428 -0.00268 0.00111 0.00160 0.02207 0.00587 0.00029 0.00027 0.00010 0.00000 0.00166 0.00162 0.00162 0.00127 0.00131 0.00130 0.00068 C26 0.87214 0.40336 -0.26217 1.00000 0.02056 0.02261 0.02144 -0.00340 0.00038 -0.00023 0.02187 0.00575 0.00029 0.00027 0.00010 0.00000 0.00167 0.00165 0.00156 0.00126 0.00129 0.00132 0.00068 C27 0.80814 0.31710 -0.28219 1.00000 0.01982 0.02347 0.02394 -0.00370 0.00227 -0.00120 0.02255 0.00587 0.00030 0.00028 0.00010 0.00000 0.00164 0.00168 0.00160 0.00131 0.00130 0.00134 0.00068 C28 0.82726 0.30338 -0.32584 1.00000 0.02309 0.02560 0.01828 -0.00313 0.00168 -0.00514 0.02251 0.00575 0.00030 0.00028 0.00009 0.00000 0.00172 0.00172 0.00149 0.00127 0.00129 0.00138 0.00069 C29 0.92069 0.39649 -0.32699 1.00000 0.01863 0.02629 0.02227 -0.00361 -0.00092 -0.00046 0.02287 0.00582 0.00030 0.00028 0.00010 0.00000 0.00164 0.00173 0.00159 0.00130 0.00127 0.00134 0.00069 C30 0.97743 0.42582 -0.35920 1.00000 0.02595 0.03347 0.01977 -0.00667 0.00217 -0.00742 0.02657 0.00601 0.00031 0.00030 0.00010 0.00000 0.00183 0.00193 0.00157 0.00139 0.00136 0.00151 0.00074 H30 0.96150 0.38621 -0.38435 1.00000 0.03188 0.00000 0.00000 C31 1.05883 0.51530 -0.35374 1.00000 0.02456 0.03430 0.02374 -0.00088 0.00197 -0.00572 0.02775 0.00627 0.00032 0.00031 0.00010 0.00000 0.00184 0.00194 0.00166 0.00144 0.00141 0.00152 0.00076 C32 1.08321 0.57506 -0.31752 1.00000 0.02185 0.02868 0.03040 0.00036 0.00500 -0.00556 0.02689 0.00639 0.00031 0.00030 0.00010 0.00000 0.00175 0.00185 0.00179 0.00144 0.00143 0.00144 0.00074 H32 1.13889 0.63585 -0.31482 1.00000 0.03227 0.00000 0.00000 C33 1.02549 0.54543 -0.28501 1.00000 0.02538 0.02385 0.02228 -0.00588 -0.00019 -0.00126 0.02429 0.00590 0.00030 0.00028 0.00010 0.00000 0.00179 0.00170 0.00161 0.00131 0.00136 0.00139 0.00071 H33 1.04136 0.58566 -0.25998 1.00000 0.02914 0.00000 0.00000 C34 0.94438 0.45609 -0.28983 1.00000 0.02095 0.02283 0.02059 -0.00290 0.00489 0.00012 0.02128 0.00587 0.00029 0.00027 0.00010 0.00000 0.00166 0.00164 0.00153 0.00125 0.00129 0.00133 0.00066 C35 0.71171 0.32733 -0.35627 1.00000 0.02460 0.03158 0.02125 -0.00304 0.00086 -0.00578 0.02613 0.00601 0.00031 0.00029 0.00010 0.00000 0.00180 0.00188 0.00159 0.00137 0.00137 0.00147 0.00074 H35A 0.72947 0.31970 -0.38432 1.00000 0.03136 0.00000 0.00000 H35B 0.65125 0.26929 -0.35261 1.00000 0.03136 0.00000 0.00000 C36 0.65827 0.44397 -0.35172 1.00000 0.02731 0.03455 0.03823 0.00210 -0.00294 -0.00261 0.03428 0.00680 0.00034 0.00032 0.00012 0.00000 0.00198 0.00207 0.00208 0.00165 0.00162 0.00164 0.00086 H36A 0.64242 0.45239 -0.32346 1.00000 0.04114 0.00000 0.00000 H36B 0.71793 0.50208 -0.35610 1.00000 0.04114 0.00000 0.00000 C37 0.54310 0.46612 -0.38094 1.00000 0.02687 0.04303 0.02817 0.00331 -0.00120 -0.00670 0.03332 0.00671 0.00033 0.00033 0.00011 0.00000 0.00197 0.00224 0.00184 0.00160 0.00153 0.00167 0.00085 H37A 0.48237 0.40998 -0.37577 1.00000 0.03998 0.00000 0.00000 H37B 0.55812 0.45457 -0.40915 1.00000 0.03998 0.00000 0.00000 C38 0.49249 0.58430 -0.37754 1.00000 0.02508 0.03980 0.04271 0.01329 -0.00033 -0.00342 0.03651 0.00739 0.00035 0.00033 0.00012 0.00000 0.00196 0.00222 0.00221 0.00175 0.00167 0.00167 0.00090 H38A 0.55339 0.64024 -0.38274 1.00000 0.04381 0.00000 0.00000 H38B 0.42185 0.59369 -0.39912 1.00000 0.04381 0.00000 0.00000 C39 0.45554 0.61096 -0.33665 1.00000 0.04209 0.04315 0.03973 0.00248 0.00122 0.00200 0.04226 0.00794 0.00040 0.00036 0.00012 0.00000 0.00250 0.00243 0.00226 0.00183 0.00187 0.00194 0.00099 H39A 0.52677 0.60564 -0.31510 1.00000 0.05071 0.00000 0.00000 H39B 0.39703 0.55346 -0.33077 1.00000 0.05071 0.00000 0.00000 C40 0.40028 0.72788 -0.33517 1.00000 0.03889 0.04202 0.06568 -0.00831 -0.00325 -0.00293 0.05017 0.00804 0.00041 0.00037 0.00015 0.00000 0.00253 0.00250 0.00308 0.00218 0.00222 0.00202 0.00115 H40A 0.45776 0.78533 -0.34090 1.00000 0.07526 0.00000 0.00000 H40B 0.37983 0.74098 -0.30802 1.00000 0.07526 0.00000 0.00000 H40C 0.32762 0.73269 -0.35562 1.00000 0.07526 0.00000 0.00000 C41 0.87595 0.18441 -0.33312 1.00000 0.02459 0.02735 0.02707 -0.00719 0.00270 -0.00477 0.02650 0.00604 0.00031 0.00029 0.00010 0.00000 0.00180 0.00180 0.00171 0.00141 0.00141 0.00146 0.00074 H41A 0.81270 0.12814 -0.33065 1.00000 0.03180 0.00000 0.00000 H41B 0.89258 0.18072 -0.36141 1.00000 0.03180 0.00000 0.00000 C42 0.98966 0.15053 -0.30412 1.00000 0.02586 0.02892 0.03439 -0.00867 0.00155 -0.00390 0.03010 0.00630 0.00033 0.00030 0.00011 0.00000 0.00188 0.00190 0.00193 0.00150 0.00154 0.00151 0.00080 H42A 1.06026 0.18178 -0.31439 1.00000 0.03612 0.00000 0.00000 H42B 0.98752 0.18403 -0.27696 1.00000 0.03612 0.00000 0.00000 C43 1.00315 0.02335 -0.29983 1.00000 0.03662 0.02592 0.06834 -0.00780 -0.01128 -0.00266 0.04583 0.00728 0.00039 0.00033 0.00015 0.00000 0.00241 0.00206 0.00299 0.00192 0.00212 0.00176 0.00111 H43A 1.00326 -0.00969 -0.32718 1.00000 0.05499 0.00000 0.00000 H43B 0.93261 -0.00717 -0.28932 1.00000 0.05499 0.00000 0.00000 C44 1.11572 -0.01478 -0.27186 1.00000 0.03674 0.02827 0.04532 -0.00762 0.00014 0.00049 0.03750 0.00706 0.00037 0.00032 0.00013 0.00000 0.00225 0.00200 0.00229 0.00168 0.00181 0.00169 0.00092 H44A 1.18657 0.01087 -0.28335 1.00000 0.04500 0.00000 0.00000 H44B 1.11857 0.02204 -0.24498 1.00000 0.04500 0.00000 0.00000 C45 1.12289 -0.14092 -0.26594 1.00000 0.06139 0.03030 0.15307 0.00136 -0.04708 0.00001 0.08876 0.00978 0.00053 0.00041 0.00023 0.00000 0.00365 0.00258 0.00623 0.00311 0.00382 0.00244 0.00233 H45A 1.11996 -0.17731 -0.29289 1.00000 0.10651 0.00000 0.00000 H45B 1.05148 -0.16622 -0.25470 1.00000 0.10651 0.00000 0.00000 C46 1.23321 -0.18165 -0.23820 1.00000 0.06053 0.03722 0.08782 0.00170 -0.01453 0.00799 0.06481 0.00931 0.00048 0.00039 0.00018 0.00000 0.00342 0.00261 0.00399 0.00250 0.00291 0.00240 0.00152 H46A 1.30450 -0.16150 -0.24989 1.00000 0.09722 0.00000 0.00000 H46B 1.22942 -0.26405 -0.23525 1.00000 0.09722 0.00000 0.00000 H46C 1.23753 -0.14590 -0.21141 1.00000 0.09722 0.00000 0.00000 S1 0.68284 0.25546 -0.13812 1.00000 0.02602 0.02173 0.02069 -0.00063 0.00298 -0.00043 0.02290 0.00150 0.00008 0.00007 0.00002 0.00000 0.00043 0.00041 0.00038 0.00031 0.00032 0.00034 0.00018 S2 0.90687 0.49843 -0.17970 1.00000 0.02087 0.02316 0.01939 -0.00388 0.00129 -0.00061 0.02136 0.00144 0.00007 0.00007 0.00002 0.00000 0.00041 0.00041 0.00037 0.00030 0.00031 0.00032 0.00017 S3 0.72553 0.23994 -0.25211 1.00000 0.02451 0.02542 0.02006 -0.00276 0.00268 -0.00532 0.02343 0.00146 0.00008 0.00007 0.00002 0.00000 0.00043 0.00043 0.00038 0.00031 0.00032 0.00034 0.00018 Br1 0.89543 0.68204 0.05355 1.00000 0.03128 0.03741 0.02231 -0.00826 0.00060 0.00419 0.03075 0.00064 0.00003 0.00003 0.00001 0.00000 0.00020 0.00021 0.00017 0.00014 0.00014 0.00016 0.00010 Br2 1.13593 0.55842 -0.39806 1.00000 0.03923 0.06585 0.02856 -0.00388 0.01086 -0.02484 0.04395 0.00073 0.00004 0.00004 0.00001 0.00000 0.00024 0.00030 0.00020 0.00018 0.00017 0.00021 0.00013 Final Structure Factor Calculation for 2009src0647 in P2(1)/n Total number of l.s. parameters = 464 Maximum vector length = 511 Memory required = 5600 / 22995 wR2 = 0.1255 before cycle 5 for 10019 data and 0 / 464 parameters GooF = S = 1.039; Restrained GooF = 1.039 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0416 * P )^2 + 8.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0520 for 7578 Fo > 4sig(Fo) and 0.0762 for all 10019 data wR2 = 0.1255, GooF = S = 1.039, Restrained GooF = 1.039 for all data Occupancy sum of asymmetric unit = 51.00 for non-hydrogen and 58.00 for hydrogen atoms Principal mean square atomic displacements U 0.0279 0.0214 0.0153 C1 0.0257 0.0213 0.0150 C2 0.0298 0.0199 0.0133 C3 0.0316 0.0211 0.0160 C4 0.0291 0.0246 0.0199 C5 0.0300 0.0241 0.0165 C6 0.0349 0.0203 0.0172 C7 0.0408 0.0206 0.0153 C8 0.0326 0.0270 0.0162 C9 0.0328 0.0226 0.0184 C10 0.0314 0.0172 0.0137 C11 0.0408 0.0353 0.0201 C12 0.0440 0.0332 0.0262 C13 0.0732 0.0496 0.0251 C14 0.0757 0.0361 0.0226 C15 0.0537 0.0486 0.0323 C16 0.0669 0.0606 0.0346 C17 0.0325 0.0286 0.0228 C18 0.0743 0.0332 0.0224 C19 0.0786 0.0405 0.0259 C20 0.0827 0.0477 0.0291 C21 0.1329 0.0568 0.0318 C22 0.1302 0.0551 0.0311 C23 0.0291 0.0208 0.0169 C24 0.0276 0.0197 0.0189 C25 0.0266 0.0217 0.0173 C26 0.0275 0.0216 0.0185 C27 0.0297 0.0220 0.0159 C28 0.0292 0.0234 0.0159 C29 0.0388 0.0251 0.0158 C30 0.0370 0.0253 0.0209 C31 0.0319 0.0304 0.0184 C32 0.0307 0.0260 0.0162 C33 0.0249 0.0214 0.0176 C34 0.0348 0.0256 0.0179 C35 0.0454 0.0337 0.0238 C36 0.0476 0.0302 0.0222 C37 0.0574 0.0280 0.0241 C38 0.0475 0.0442 0.0350 C39 0.0739 0.0437 0.0329 C40 0.0346 0.0269 0.0180 C41 0.0410 0.0295 0.0198 C42 0.0824 0.0332 0.0219 C43 0.0524 0.0349 0.0253 C44 0.1989 0.0371 0.0302 C45 0.1094 0.0517 0.0334 C46 0.0263 0.0220 0.0204 S1 0.0258 0.0218 0.0165 S2 0.0303 0.0223 0.0177 S3 0.0445 0.0292 0.0186 Br1 0.0808 0.0297 0.0214 Br2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.014 0.026 0.037 0.050 0.065 0.083 0.104 0.137 0.195 1.000 Number in group 1047. 1036. 933. 1001. 992. 1037. 990. 984. 996. 1003. GooF 0.943 0.979 0.959 1.035 1.103 1.093 1.081 1.108 1.093 0.983 K 2.986 1.397 1.138 1.030 1.034 1.012 1.000 1.006 1.006 0.994 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.31 1.65 inf Number in group 1001. 1024. 1017. 974. 1020. 993. 986. 996. 1001. 1007. GooF 0.941 0.975 0.937 0.969 0.989 0.939 0.963 1.060 1.027 1.475 K 0.977 0.994 1.014 1.020 1.025 1.026 1.018 1.002 1.000 0.993 R1 0.179 0.156 0.127 0.105 0.094 0.072 0.060 0.047 0.038 0.038 Recommended weighting scheme: WGHT 0.0411 8.4545 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 1 2 1107.78 3431.56 8.34 0.171 6.95 0 2 0 6014.66 14559.16 8.20 0.353 5.91 -1 1 3 468.86 1535.83 8.20 0.115 6.92 -6 1 24 588.56 2342.60 7.97 0.142 1.19 -5 2 23 2102.01 4347.36 7.84 0.193 1.27 -9 0 27 30.67 1444.66 7.63 0.111 0.95 -6 2 25 148.87 924.87 7.29 0.089 1.14 -6 0 24 161.53 1754.49 7.28 0.123 1.20 -7 2 19 866.91 2045.05 6.06 0.132 1.25 4 2 6 360.26 103.27 5.35 0.030 2.17 -10 1 27 109.69 1059.15 5.31 0.095 0.90 -5 0 23 234.72 865.56 5.20 0.086 1.30 -12 1 25 990.76 2033.39 4.45 0.132 0.82 3 4 2 8586.11 6637.27 4.42 0.238 2.26 -3 2 6 1888.64 1303.66 4.21 0.106 2.91 -3 5 10 577.50 307.46 4.16 0.051 1.77 -4 5 5 383.69 742.12 4.16 0.080 1.79 5 11 14 684.17 1441.82 4.06 0.111 0.87 -1 3 18 1021.94 1544.33 3.99 0.115 1.67 -10 1 26 188.72 775.16 3.90 0.081 0.91 -1 3 15 1389.85 947.07 3.88 0.090 1.93 -3 1 3 646.29 1027.77 3.87 0.094 3.54 -4 4 7 364.56 162.63 3.86 0.037 1.95 -1 3 19 1079.90 667.89 3.86 0.076 1.60 -1 2 12 916.94 581.67 3.82 0.071 2.50 -4 3 2 1212.37 1748.89 3.81 0.122 2.30 -4 4 4 150.61 27.80 3.79 0.015 2.03 3 4 7 213.83 439.31 3.75 0.061 2.00 4 11 25 372.63 845.72 3.71 0.085 0.78 2 3 2 5123.82 4065.92 3.65 0.187 3.10 -4 2 17 1599.28 1085.05 3.59 0.096 1.66 7 6 7 1640.82 1082.08 3.55 0.096 1.16 8 7 9 922.38 495.63 3.49 0.065 1.00 -1 4 1 327.61 565.20 3.45 0.070 2.85 -4 0 18 2447.41 3423.19 3.37 0.171 1.65 4 4 1 1866.19 2458.41 3.36 0.145 2.01 0 4 6 1082.30 755.15 3.33 0.080 2.60 -10 6 13 297.32 61.53 3.27 0.023 0.95 1 6 0 3614.19 2874.64 3.23 0.157 1.94 1 8 2 1703.16 1250.31 3.23 0.103 1.46 -1 4 9 76.81 202.56 3.21 0.042 2.29 3 11 22 654.02 310.21 3.21 0.052 0.83 -2 7 33 744.71 356.84 3.20 0.055 0.87 -12 0 20 1303.32 2334.35 3.20 0.141 0.87 -4 2 18 3146.17 5489.72 3.18 0.217 1.59 0 2 17 618.57 386.39 3.17 0.058 1.84 2 2 8 429.04 679.38 3.16 0.076 2.73 6 0 2 731.77 444.32 3.16 0.062 1.82 -6 1 11 2816.88 2196.18 3.15 0.137 1.69 -7 12 15 9.82 217.70 3.13 0.043 0.81 Bond lengths and angles C1 - Distance Angles C2 1.3931 (0.0045) C24 1.4197 (0.0044) 111.94 (0.29) S1 1.7363 (0.0034) 112.07 (0.24) 135.99 (0.26) C1 - C2 C24 C2 - Distance Angles C1 1.3931 (0.0045) C3 1.4171 (0.0043) 112.10 (0.29) S2 1.7396 (0.0034) 112.78 (0.24) 135.12 (0.26) C2 - C1 C3 C3 - Distance Angles C4 1.3615 (0.0047) C2 1.4171 (0.0043) 112.18 (0.29) C11 1.4708 (0.0043) 109.01 (0.29) 138.69 (0.31) C3 - C4 C2 C4 - Distance Angles C3 1.3615 (0.0047) C5 1.5194 (0.0045) 113.35 (0.29) S1 1.7327 (0.0033) 113.51 (0.25) 132.98 (0.26) C4 - C3 C5 C5 - Distance Angles C4 1.5194 (0.0045) C18 1.5371 (0.0048) 111.54 (0.28) C6 1.5395 (0.0048) 98.78 (0.26) 111.90 (0.28) C12 1.5523 (0.0047) 112.76 (0.28) 113.04 (0.29) 107.91 (0.27) C5 - C4 C18 C6 C6 - Distance Angles C7 1.3853 (0.0045) C11 1.4055 (0.0046) 119.79 (0.32) C5 1.5395 (0.0048) 128.19 (0.31) 112.01 (0.28) C6 - C7 C11 C7 - Distance Angles C8 1.3826 (0.0049) C6 1.3853 (0.0045) 118.12 (0.32) C7 - C8 C8 - Distance Angles C7 1.3826 (0.0049) C9 1.3863 (0.0049) 122.47 (0.31) Br1 1.9068 (0.0033) 118.68 (0.26) 118.84 (0.26) C8 - C7 C9 C9 - Distance Angles C8 1.3863 (0.0049) C10 1.3928 (0.0045) 119.79 (0.33) C9 - C8 C10 - Distance Angles C11 1.3855 (0.0047) C9 1.3928 (0.0045) 118.15 (0.32) C10 - C11 C11 - Distance Angles C10 1.3855 (0.0047) C6 1.4055 (0.0046) 121.64 (0.29) C3 1.4708 (0.0043) 131.51 (0.31) 106.84 (0.29) C11 - C10 C6 C12 - Distance Angles C13 1.5140 (0.0052) C5 1.5523 (0.0047) 116.59 (0.30) C12 - C13 C13 - Distance Angles C12 1.5140 (0.0052) C14 1.5415 (0.0052) 110.38 (0.32) C13 - C12 C14 - Distance Angles C13 1.5415 (0.0052) C15 1.5579 (0.0061) 111.80 (0.35) C14 - C13 C15 - Distance Angles C16 1.4898 (0.0060) C14 1.5579 (0.0061) 114.65 (0.37) C15 - C16 C16 - Distance Angles C15 1.4898 (0.0060) C17 1.5064 (0.0062) 112.10 (0.40) C16 - C15 C17 - Distance Angles C16 1.5064 (0.0062) C17 - C18 - Distance Angles C19 1.5229 (0.0052) C5 1.5371 (0.0048) 114.34 (0.29) C18 - C19 C19 - Distance Angles C20 1.4775 (0.0055) C18 1.5229 (0.0052) 116.29 (0.35) C19 - C20 C20 - Distance Angles C19 1.4775 (0.0055) C21 1.4923 (0.0062) 116.35 (0.39) C20 - C19 C21 - Distance Angles C22 1.4588 (0.0062) C20 1.4923 (0.0062) 120.98 (0.43) C21 - C22 C22 - Distance Angles C21 1.4588 (0.0062) C23 1.4621 (0.0070) 118.89 (0.49) C22 - C21 C23 - Distance Angles C22 1.4621 (0.0070) C23 - C24 - Distance Angles C25 1.3880 (0.0047) C1 1.4197 (0.0044) 112.31 (0.29) S3 1.7368 (0.0033) 112.36 (0.25) 135.32 (0.27) C24 - C25 C1 C25 - Distance Angles C24 1.3880 (0.0047) C26 1.4261 (0.0044) 112.15 (0.28) S2 1.7419 (0.0032) 112.71 (0.25) 135.13 (0.26) C25 - C24 C26 C26 - Distance Angles C27 1.3600 (0.0044) C25 1.4261 (0.0044) 111.70 (0.30) C34 1.4654 (0.0046) 108.54 (0.28) 139.65 (0.30) C26 - C27 C25 C27 - Distance Angles C26 1.3600 (0.0044) C28 1.5109 (0.0044) 113.76 (0.29) S3 1.7349 (0.0034) 113.90 (0.25) 132.27 (0.24) C27 - C26 C28 C28 - Distance Angles C27 1.5109 (0.0044) C29 1.5304 (0.0046) 98.88 (0.25) C41 1.5429 (0.0047) 111.04 (0.27) 112.64 (0.28) C35 1.5442 (0.0046) 111.83 (0.28) 111.52 (0.27) 110.48 (0.26) C28 - C27 C29 C41 C29 - Distance Angles C30 1.3796 (0.0047) C34 1.4097 (0.0044) 120.61 (0.31) C28 1.5304 (0.0046) 127.62 (0.29) 111.76 (0.29) C29 - C30 C34 C30 - Distance Angles C29 1.3796 (0.0047) C31 1.3944 (0.0048) 118.05 (0.31) C30 - C29 C31 - Distance Angles C32 1.3849 (0.0048) C30 1.3944 (0.0048) 122.25 (0.33) Br2 1.9004 (0.0035) 119.11 (0.26) 118.63 (0.25) C31 - C32 C30 C32 - Distance Angles C31 1.3849 (0.0048) C33 1.3956 (0.0047) 119.60 (0.32) C32 - C31 C33 - Distance Angles C34 1.3907 (0.0045) C32 1.3956 (0.0047) 118.96 (0.30) C33 - C34 C34 - Distance Angles C33 1.3907 (0.0045) C29 1.4097 (0.0044) 120.53 (0.30) C26 1.4654 (0.0046) 132.47 (0.30) 106.99 (0.28) C34 - C33 C29 C35 - Distance Angles C36 1.5221 (0.0051) C28 1.5442 (0.0046) 114.10 (0.28) C35 - C36 C36 - Distance Angles C37 1.5166 (0.0049) C35 1.5221 (0.0051) 113.97 (0.31) C36 - C37 C37 - Distance Angles C36 1.5166 (0.0049) C38 1.5201 (0.0055) 113.94 (0.32) C37 - C36 C38 - Distance Angles C39 1.5193 (0.0056) C37 1.5201 (0.0055) 114.75 (0.32) C38 - C39 C39 - Distance Angles C38 1.5193 (0.0056) C40 1.5201 (0.0059) 113.07 (0.36) C39 - C38 C40 - Distance Angles C39 1.5201 (0.0059) C40 - C41 - Distance Angles C42 1.5308 (0.0049) C28 1.5429 (0.0047) 115.11 (0.27) C41 - C42 C42 - Distance Angles C43 1.5144 (0.0051) C41 1.5308 (0.0049) 112.35 (0.30) C42 - C43 C43 - Distance Angles C42 1.5144 (0.0051) C44 1.5187 (0.0055) 114.43 (0.32) C43 - C42 C44 - Distance Angles C45 1.5035 (0.0060) C43 1.5187 (0.0055) 113.34 (0.35) C44 - C45 C45 - Distance Angles C44 1.5035 (0.0060) C46 1.5057 (0.0067) 114.75 (0.41) C45 - C44 C46 - Distance Angles C45 1.5057 (0.0067) C46 - S1 - Distance Angles C4 1.7327 (0.0033) C1 1.7363 (0.0034) 90.12 (0.16) S1 - C4 S2 - Distance Angles C2 1.7396 (0.0034) C25 1.7419 (0.0032) 90.26 (0.16) S2 - C2 S3 - Distance Angles C27 1.7349 (0.0034) C24 1.7368 (0.0033) 89.89 (0.16) S3 - C27 Br1 - Distance Angles C8 1.9068 (0.0033) Br1 - Br2 - Distance Angles C31 1.9004 (0.0035) Br2 - FMAP and GRID set by program FMAP 2 3 39 GRID -0.694 -2 -2 0.694 2 2 R1 = 0.0727 for 10019 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.56 at 0.0047 0.3749 0.0844 [ 0.52 A from H10 ] Deepest hole -0.65 at 0.5923 0.8942 0.0878 [ 0.84 A from BR2 ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 5124 / 36522 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.9953 0.6251 -0.0844 1.00000 0.05 1.56 0.52 H10 1.23 C10 2.14 C9 2.17 H22A Q2 1 1.0821 0.6027 -0.2309 1.00000 0.05 0.75 1.02 H33 1.93 C33 2.32 H46B 2.80 H44A Q3 1 0.8183 0.1646 -0.0317 1.00000 0.05 0.69 1.07 H12A 1.17 C12 1.18 C13 1.54 H13A Q4 1 0.7468 -0.0071 0.0083 1.00000 0.05 0.63 0.88 H14A 0.96 C14 1.30 C15 1.65 H15B Q5 1 1.1777 0.5065 -0.3903 1.00000 0.05 0.55 0.79 BR2 1.96 C31 2.81 C30 2.86 H30 Q6 1 0.6920 -0.0407 0.0004 1.00000 0.05 0.53 1.10 C15 1.24 H16B 1.25 C16 1.51 C14 Q7 1 0.6963 0.2264 -0.0321 1.00000 0.05 0.49 0.88 C12 1.13 C13 1.30 H13B 1.35 H12B Q8 1 1.1265 0.5628 -0.3750 1.00000 0.05 0.45 0.79 BR2 1.26 C31 2.05 C32 2.16 H32 Q9 1 0.3469 0.4180 -0.0780 1.00000 0.05 0.44 0.78 H20A 0.91 C20 0.93 H20B 2.11 C21 Q10 1 0.6984 -0.1352 -0.0386 1.00000 0.05 0.43 0.97 C15 0.99 H15A 1.26 C16 1.45 H15B Q11 1 0.8546 0.0887 0.0067 1.00000 0.05 0.42 0.69 H14B 1.02 C14 1.20 H14A 2.03 C13 Q12 1 0.3991 0.6459 -0.1057 1.00000 0.05 0.41 0.69 H21B 1.02 C21 1.11 H21A 2.14 C20 Q13 1 0.3865 0.5274 -0.0691 1.00000 0.05 0.40 0.79 C20 0.96 H20A 1.28 C21 1.41 H21A Q14 1 0.8936 0.4618 -0.1599 1.00000 0.05 0.40 0.82 S2 1.02 C2 2.09 C25 2.12 C1 Q15 1 0.7205 0.3437 -0.0769 1.00000 0.05 0.37 0.74 C4 0.78 C5 1.84 C3 1.88 C6 Q16 1 0.8799 0.6011 0.0652 1.00000 0.05 0.37 1.06 BR1 2.09 C8 2.31 H7 2.32 H22A Q17 1 0.2250 0.6478 -0.0981 1.00000 0.05 0.36 0.90 C22 1.18 H22A 1.37 C23 1.45 H23A Q18 1 0.6455 -0.1780 -0.0259 1.00000 0.05 0.36 0.87 C17 0.97 C16 1.27 H17A 1.33 H17C Q19 1 0.3458 0.6684 -0.1064 1.00000 0.05 0.36 0.98 H21A 1.01 H21B 1.01 C21 1.74 C22 Q20 1 0.9173 0.6903 0.0259 1.00000 0.05 0.36 1.00 BR1 1.31 C8 1.90 C9 1.92 H9 Shortest distances between peaks (including symmetry equivalents) 12 19 0.65 4 6 0.75 10 18 0.94 5 8 1.06 9 13 1.38 17 19 1.46 3 7 1.56 3 11 1.56 4 11 1.67 6 10 1.72 16 20 1.78 12 13 1.87 6 18 1.88 12 17 2.03 13 19 2.08 7 15 2.08 4 10 2.18 6 11 2.38 13 17 2.39 4 18 2.50 7 11 2.60 3 4 2.62 9 16 2.68 1 17 2.72 3 15 2.72 9 12 2.94 Time profile in seconds ----------------------- 0.42: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.08: Generate connectivity array 0.08: 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 0.02: Generate ISOR restraints 0.00: Generate NCSY restraints 0.08: Analyse other restraints etc. 69.09: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.03: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.00: Generate idealized H-atoms 17.94: Structure factors and derivatives 15.72: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.36: Apply other restraints 5.44: Solve l.s. equations 0.00: Generate HTAB table 0.09: Other dependent quantities, CIF, tables 0.39: Analysis of variance 0.20: Merge reflections for Fourier and .fcf 0.91: Fourier summations 0.16: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + shelxl finished at 16:24:29 Total CPU time: 111.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++