+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 10:53:07 on 03-Aug-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 00SOT039 in P-1 CELL 0.71073 7.9539 9.5523 10.6949 97.614 110.439 104.170 ZERR 2.00 0.0016 0.0019 0.0021 0.030 0.030 0.030 LATT 1 SFAC C H O F BR UNIT 28 28 4 6 2 V = 716.69 F(000) = 352.0 Mu = 2.90 mm-1 Cell Wt = 702.32 Rho = 1.627 L.S. 4 BOND FMAP 2 PLAN 10 SIZE 0.35 0.35 0.35 TEMP 25 OMIT -5 -3 2 OMIT 0 0 1 OMIT -3 55 WGHT 0.0791 0.1443 EXTI 0.015343 FVAR 0.85223 BR1 5 0.078140 0.904398 0.860511 11.00000 0.12393 0.10583 = 0.17667 0.03362 0.09630 0.01110 F1 4 0.783063 1.465812 0.527823 11.00000 0.07708 0.15435 = 0.06700 0.05678 0.03677 0.04906 F2 4 0.938342 1.310691 0.551216 11.00000 0.10109 0.14340 = 0.09342 0.03171 0.06775 0.05792 F3 4 1.041044 1.516427 0.703357 11.00000 0.05619 0.11540 = 0.08719 0.03468 0.03232 0.01455 O1 3 0.900834 1.264475 0.786175 11.00000 0.05410 0.07825 = 0.05704 0.01273 0.01777 0.03142 AFIX 83 H1 2 0.999394 1.328996 0.838311 11.00000 -1.50000 AFIX 0 O2 3 0.734933 1.546562 1.003148 11.00000 0.05931 0.08952 = 0.04457 0.01036 0.02098 0.03154 C1 1 0.237535 0.993271 0.777826 11.00000 0.07587 0.05480 = 0.09175 -0.00075 0.03830 0.00914 C2 1 0.181082 1.078996 0.689140 11.00000 0.05294 0.07403 = 0.10415 -0.00002 0.02977 0.00805 AFIX 43 H2 2 0.062869 1.091887 0.667404 11.00000 -1.20000 AFIX 0 C3 1 0.300392 1.146409 0.631929 11.00000 0.05315 0.07174 = 0.07551 0.00430 0.01749 0.01762 AFIX 43 H3 2 0.260537 1.204359 0.571295 11.00000 -1.20000 AFIX 0 C4 1 0.478658 1.130429 0.662100 11.00000 0.05469 0.06147 = 0.05710 -0.00823 0.02090 0.01070 C5 1 0.529605 1.040864 0.752100 11.00000 0.06699 0.07254 = 0.07553 0.00743 0.02480 0.02609 AFIX 43 H5 2 0.646769 1.025962 0.774014 11.00000 -1.20000 AFIX 0 C6 1 0.412690 0.975089 0.808342 11.00000 0.09500 0.06451 = 0.09097 0.01513 0.04408 0.02703 AFIX 43 H6 2 0.451259 0.916541 0.868696 11.00000 -1.20000 AFIX 0 C7 1 0.605614 1.203765 0.599166 11.00000 0.05641 0.07594 = 0.05296 -0.00055 0.01672 0.02077 AFIX 23 H7A 2 0.534026 1.242231 0.525859 11.00000 -1.20000 H7B 2 0.647947 1.129723 0.558422 11.00000 -1.20000 AFIX 0 C8 1 0.778620 1.330924 0.700777 11.00000 0.04998 0.06967 = 0.04521 0.01456 0.01846 0.02400 C9 1 0.885532 1.407479 0.621469 11.00000 0.05476 0.10458 = 0.05862 0.02023 0.02545 0.03092 C10 1 0.727333 1.444749 0.783165 11.00000 0.03972 0.06428 = 0.04043 0.01152 0.01526 0.01392 C11 1 0.769577 1.450964 0.914952 11.00000 0.04022 0.07110 = 0.04832 0.01124 0.01406 0.01892 AFIX 43 H11 2 0.828478 1.384079 0.951441 11.00000 -1.20000 AFIX 0 C12 1 0.654127 1.653745 0.945028 11.00000 0.06529 0.07680 = 0.07253 0.00610 0.02562 0.02718 AFIX 23 H12A 2 0.754134 1.737919 0.948236 11.00000 -1.20000 H12B 2 0.591347 1.689597 0.999555 11.00000 -1.20000 AFIX 0 C13 1 0.515039 1.588739 0.799390 11.00000 0.06938 0.08651 = 0.07058 0.01361 0.02184 0.04226 AFIX 23 H13A 2 0.461386 1.663178 0.763593 11.00000 -1.20000 H13B 2 0.413072 1.505866 0.795682 11.00000 -1.20000 AFIX 0 C14 1 0.612865 1.535802 0.712414 11.00000 0.06156 0.07291 = 0.05409 0.01629 0.01806 0.02551 AFIX 23 H14A 2 0.519448 1.476431 0.623075 11.00000 -1.20000 H14B 2 0.694470 1.620721 0.698715 11.00000 -1.20000 HKLF 4 Covalent radii and connectivity table for 00SOT039 in P-1 C 0.770 H 0.320 O 0.660 F 0.640 BR 1.140 Br1 - C1 F1 - C9 F2 - C9 F3 - C9 O1 - C8 O2 - C11 C12 C1 - C2 C6 Br1 C2 - C1 C3 C3 - C2 C4 C4 - C3 C5 C7 C5 - C6 C4 C6 - C5 C1 C7 - C4 C8 C8 - O1 C7 C10 C9 C9 - F3 F1 F2 C8 C10 - C11 C14 C8 C11 - C10 O2 C12 - O2 C13 C13 - C12 C14 C14 - C10 C13 5358 Reflections read, of which 4 rejected -10 =< h =< 10, -12 =< k =< 12, -13 =< l =< 13, Max. 2-theta = 54.94 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -1 0 1 143.00 4.82 2 24.18 3 0 3 53.78 2.95 2 26.01 -2 -2 5 723.90 16.52 3 125.00 3 Inconsistent equivalents 2944 Unique reflections, of which 0 suppressed R(int) = 0.0494 R(sigma) = 0.0781 Friedel opposites merged Maximum memory for data reduction = 1721 / 30338 Default effective X-H distances for T = 25.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 0.98 0.97 0.96 0.93 0.86 0.89 1.10 0.82 0.93 0.86 0.93 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 = 2221 / 227038 wR2 = 0.1798 before cycle 1 for 2944 data and 182 / 182 parameters GooF = S = 1.002; Restrained GooF = 1.002 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0791 * P )^2 + 0.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.85161 0.00360 -0.171 OSF 2 0.01503 0.00387 -0.081 EXTI Mean shift/esd = 0.075 Maximum = -0.436 for z Br1 Max. shift = 0.001 A for C2 Max. dU = 0.000 for C4 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2221 / 227038 wR2 = 0.1797 before cycle 2 for 2944 data and 182 / 182 parameters GooF = S = 1.002; Restrained GooF = 1.002 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0791 * P )^2 + 0.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.85116 0.00360 -0.125 OSF 2 0.01485 0.00385 -0.047 EXTI Mean shift/esd = 0.025 Maximum = -0.137 for z Br1 Max. shift = 0.000 A for C2 Max. dU = 0.000 for C4 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2221 / 227038 wR2 = 0.1797 before cycle 3 for 2944 data and 182 / 182 parameters GooF = S = 1.002; Restrained GooF = 1.002 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0791 * P )^2 + 0.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.85113 0.00359 -0.010 OSF 2 0.01481 0.00383 -0.010 EXTI Mean shift/esd = 0.002 Maximum = -0.010 for OSF Max. shift = 0.000 A for C3 Max. dU = 0.000 for C6 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2221 / 227038 wR2 = 0.1797 before cycle 4 for 2944 data and 182 / 182 parameters GooF = S = 1.002; Restrained GooF = 1.002 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0791 * P )^2 + 0.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.85113 0.00359 0.000 OSF 2 0.01481 0.00383 -0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for U12 C4 Max. shift = 0.000 A for C3 Max. dU = 0.000 for F2 Largest correlation matrix elements 0.734 U13 Br1 / U11 Br1 0.598 U23 F1 / U22 F1 0.550 z F2 / x F2 0.724 U13 Br1 / U33 Br1 0.581 U12 F1 / U23 F1 0.544 U13 C9 / U11 C9 0.665 U13 F2 / U33 F2 0.580 U12 F2 / U11 F2 0.537 U22 Br1 / OSF 0.665 U13 F2 / U11 F2 0.577 U12 F2 / U22 F2 0.536 U13 F1 / U11 F1 0.620 U12 Br1 / U23 Br1 0.571 U13 F3 / U11 F3 0.534 U12 C9 / U23 C9 0.614 z Br1 / x Br1 0.560 U12 F1 / U22 F1 0.533 U12 C8 / U22 C8 0.611 U12 C13 / U22 C13 0.558 U12 C13 / U11 C13 0.531 U12 O1 / U22 O1 0.607 U12 F2 / U23 F2 0.551 U13 F1 / U33 F1 0.531 U11 Br1 / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.9994 1.3290 0.8383 83 0.820 0.000 O1 C8 H1 H2 0.0629 1.0918 0.6675 43 0.930 0.000 C2 C1 C3 H3 0.2606 1.2045 0.5715 43 0.930 0.000 C3 C2 C4 H5 0.6467 1.0260 0.7738 43 0.930 0.000 C5 C6 C4 H6 0.4515 0.9165 0.8688 43 0.930 0.000 C6 C5 C1 H7A 0.5340 1.2421 0.5258 23 0.970 0.000 C7 C4 C8 H7B 0.6479 1.1296 0.5585 23 0.970 0.000 C7 C4 C8 H11 0.8286 1.3842 0.9515 43 0.930 0.000 C11 C10 O2 H12A 0.7541 1.7379 0.9483 23 0.970 0.000 C12 O2 C13 H12B 0.5913 1.6895 0.9995 23 0.970 0.000 C12 O2 C13 H13A 0.4615 1.6633 0.7637 23 0.970 0.000 C13 C12 C14 H13B 0.4131 1.5059 0.7957 23 0.970 0.000 C13 C12 C14 H14A 0.5194 1.4764 0.6231 23 0.970 0.000 C14 C10 C13 H14B 0.6945 1.6207 0.6986 23 0.970 0.000 C14 C10 C13 00SOT039 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Br1 0.07811 0.90437 0.86045 1.00000 0.12373 0.10569 0.17641 0.03359 0.09621 0.01109 0.12962 0.00217 0.00011 0.00009 0.00010 0.00000 0.00067 0.00066 0.00089 0.00056 0.00062 0.00047 0.00047 F1 0.78305 1.46581 0.52783 1.00000 0.07665 0.15441 0.06681 0.05675 0.03682 0.04907 0.09127 0.00786 0.00039 0.00041 0.00027 0.00000 0.00179 0.00310 0.00168 0.00203 0.00149 0.00212 0.00104 F2 0.93830 1.31073 0.55123 1.00000 0.10116 0.14349 0.09295 0.03164 0.06759 0.05812 0.09999 0.00893 0.00046 0.00043 0.00032 0.00000 0.00221 0.00303 0.00215 0.00213 0.00193 0.00228 0.00108 F3 1.04102 1.51641 0.70337 1.00000 0.05623 0.11487 0.08682 0.03447 0.03206 0.01444 0.08627 0.00756 0.00037 0.00038 0.00030 0.00000 0.00160 0.00251 0.00195 0.00189 0.00153 0.00176 0.00092 O1 0.90083 1.26452 0.78619 1.00000 0.05399 0.07803 0.05672 0.01255 0.01754 0.03139 0.06248 0.00728 0.00039 0.00036 0.00028 0.00000 0.00164 0.00218 0.00171 0.00167 0.00146 0.00167 0.00084 H1 0.99939 1.32904 0.83833 1.00000 0.09372 0.00000 0.00000 O2 0.73493 1.54657 1.00316 1.00000 0.05904 0.08925 0.04450 0.01032 0.02091 0.03147 0.06314 0.00727 0.00039 0.00038 0.00027 0.00000 0.00176 0.00238 0.00155 0.00165 0.00138 0.00178 0.00085 C1 0.23759 0.99319 0.77790 1.00000 0.07619 0.05456 0.09172 -0.00042 0.03861 0.00937 0.07666 0.01279 0.00079 0.00057 0.00059 0.00000 0.00336 0.00312 0.00367 0.00302 0.00293 0.00274 0.00140 C2 0.18118 1.07890 0.68927 1.00000 0.05294 0.07389 0.10453 -0.00020 0.03001 0.00787 0.08205 0.01263 0.00071 0.00064 0.00062 0.00000 0.00274 0.00358 0.00397 0.00345 0.00284 0.00272 0.00153 H2 0.06294 1.09175 0.66753 1.00000 0.09846 0.00000 0.00000 C3 0.30047 1.14644 0.63202 1.00000 0.05295 0.07173 0.07492 0.00416 0.01734 0.01718 0.07069 0.01133 0.00063 0.00059 0.00051 0.00000 0.00266 0.00335 0.00313 0.00273 0.00246 0.00256 0.00132 H3 0.26062 1.20446 0.57145 1.00000 0.08483 0.00000 0.00000 C4 0.47851 1.13042 0.66213 1.00000 0.05407 0.06137 0.05664 -0.00796 0.02041 0.01090 0.06150 0.01075 0.00063 0.00054 0.00046 0.00000 0.00249 0.00296 0.00253 0.00250 0.00215 0.00233 0.00119 C5 0.52952 1.04088 0.75200 1.00000 0.06661 0.07231 0.07587 0.00730 0.02523 0.02570 0.07279 0.01237 0.00072 0.00059 0.00053 0.00000 0.00298 0.00340 0.00315 0.00293 0.00264 0.00282 0.00135 H5 0.64668 1.02599 0.77378 1.00000 0.08735 0.00000 0.00000 C6 0.41278 0.97498 0.80845 1.00000 0.09417 0.06415 0.09075 0.01485 0.04322 0.02694 0.08112 0.01396 0.00082 0.00061 0.00059 0.00000 0.00393 0.00335 0.00368 0.00298 0.00326 0.00309 0.00146 H6 0.45146 0.91648 0.86882 1.00000 0.09735 0.00000 0.00000 C7 0.60559 1.20369 0.59921 1.00000 0.05624 0.07582 0.05242 -0.00106 0.01652 0.02054 0.06467 0.01091 0.00060 0.00057 0.00045 0.00000 0.00255 0.00336 0.00248 0.00243 0.00216 0.00252 0.00123 H7A 0.53405 1.24212 0.52585 1.00000 0.07761 0.00000 0.00000 H7B 0.64793 1.12961 0.55854 1.00000 0.07761 0.00000 0.00000 C8 0.77868 1.33094 0.70083 1.00000 0.05000 0.06961 0.04513 0.01460 0.01849 0.02393 0.05393 0.01029 0.00056 0.00051 0.00039 0.00000 0.00232 0.00303 0.00228 0.00230 0.00200 0.00239 0.00110 C9 0.88549 1.40746 0.62144 1.00000 0.05478 0.10381 0.05854 0.02029 0.02581 0.03070 0.07020 0.01332 0.00068 0.00068 0.00050 0.00000 0.00275 0.00422 0.00277 0.00303 0.00247 0.00310 0.00138 C10 0.72738 1.44479 0.78319 1.00000 0.03975 0.06386 0.04057 0.01156 0.01534 0.01413 0.04874 0.00965 0.00052 0.00049 0.00038 0.00000 0.00196 0.00279 0.00226 0.00209 0.00174 0.00204 0.00100 C11 0.76964 1.45102 0.91498 1.00000 0.04031 0.07122 0.04797 0.01132 0.01422 0.01933 0.05407 0.01002 0.00053 0.00052 0.00042 0.00000 0.00208 0.00304 0.00243 0.00224 0.00185 0.00216 0.00109 H11 0.82862 1.38418 0.95148 1.00000 0.06488 0.00000 0.00000 C12 0.65410 1.65369 0.94503 1.00000 0.06578 0.07636 0.07205 0.00591 0.02518 0.02741 0.07225 0.01201 0.00069 0.00059 0.00049 0.00000 0.00288 0.00357 0.00321 0.00289 0.00259 0.00288 0.00138 H12A 0.75411 1.73789 0.94827 1.00000 0.08670 0.00000 0.00000 H12B 0.59129 1.68952 0.99954 1.00000 0.08670 0.00000 0.00000 C13 0.51510 1.58878 0.79942 1.00000 0.06877 0.08619 0.07027 0.01311 0.02110 0.04180 0.07412 0.01246 0.00068 0.00063 0.00048 0.00000 0.00299 0.00381 0.00313 0.00291 0.00264 0.00302 0.00143 H13A 0.46150 1.66326 0.76366 1.00000 0.08894 0.00000 0.00000 H13B 0.41309 1.50592 0.79568 1.00000 0.08894 0.00000 0.00000 C14 0.61288 1.53581 0.71237 1.00000 0.06110 0.07283 0.05379 0.01610 0.01787 0.02549 0.06302 0.01176 0.00064 0.00057 0.00045 0.00000 0.00260 0.00319 0.00249 0.00244 0.00215 0.00252 0.00120 H14A 0.51944 1.47641 0.62305 1.00000 0.07563 0.00000 0.00000 H14B 0.69446 1.62072 0.69863 1.00000 0.07563 0.00000 0.00000 Final Structure Factor Calculation for 00SOT039 in P-1 Total number of l.s. parameters = 182 Maximum vector length = 511 Memory required = 2039 / 24017 wR2 = 0.1797 before cycle 5 for 2944 data and 0 / 182 parameters GooF = S = 1.002; Restrained GooF = 1.002 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0791 * P )^2 + 0.14 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0576 for 1389 Fo > 4sig(Fo) and 0.1379 for all 2944 data wR2 = 0.1797, GooF = S = 1.002, Restrained GooF = 1.002 for all data Occupancy sum of asymmetric unit = 20.00 for non-hydrogen and 14.00 for hydrogen atoms Principal mean square atomic displacements U 0.1945 0.1273 0.0671 Br1 0.1587 0.0683 0.0468 F1 0.1467 0.1091 0.0441 F2 0.1271 0.0809 0.0508 F3 0.0843 0.0583 0.0448 O1 0.0936 0.0530 0.0429 O2 0.1077 0.0716 0.0507 C1 0.1225 0.0740 0.0497 C2 0.0931 0.0666 0.0524 C3 0.0885 0.0552 0.0408 C4 0.0904 0.0677 0.0602 C5 0.0989 0.0831 0.0613 C6 0.0901 0.0568 0.0471 C7 0.0703 0.0473 0.0443 C8 0.1043 0.0578 0.0485 C9 0.0656 0.0413 0.0394 C10 0.0727 0.0510 0.0384 C11 0.0923 0.0668 0.0576 C12 0.1028 0.0697 0.0499 C13 0.0745 0.0640 0.0506 C14 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.004 0.007 0.012 0.016 0.022 0.032 0.046 0.071 0.126 1.000 Number in group 328. 265. 346. 270. 265. 309. 290. 285. 290. 296. GooF 0.810 0.828 0.879 0.934 0.962 1.115 1.221 1.162 1.077 0.963 K 4.956 1.142 0.720 0.917 0.955 1.021 1.014 0.981 1.027 1.014 Resolution(A) 0.77 0.81 0.84 0.88 0.94 1.00 1.08 1.18 1.35 1.71 inf Number in group 295. 295. 298. 291. 297. 290. 299. 292. 294. 293. GooF 0.850 0.846 0.877 0.974 1.034 1.102 1.097 1.024 0.983 1.178 K 1.090 1.189 0.995 1.032 0.952 0.977 1.045 1.046 1.038 1.006 R1 0.608 0.491 0.455 0.351 0.251 0.156 0.105 0.070 0.046 0.041 Recommended weighting scheme: WGHT 0.0770 0.1604 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 1 1 28.66 15.77 3.95 0.031 1.92 2 -3 8 55.03 32.22 3.92 0.044 1.08 -6 7 4 27.86 13.11 3.59 0.028 1.02 -6 6 6 8.84 21.17 3.53 0.036 1.01 -7 4 6 46.16 71.16 3.47 0.065 1.04 -2 -1 11 9.35 21.44 3.38 0.036 0.96 4 -1 7 4.46 22.80 3.35 0.037 0.96 -3 -1 4 2.22 7.15 3.32 0.021 2.08 -2 -1 5 9.78 19.97 3.29 0.035 2.07 5 -2 6 0.32 11.02 3.25 0.026 0.95 3 -5 3 145.13 105.76 3.16 0.080 1.48 -3 -2 4 140.04 192.90 3.16 0.108 1.91 -2 -5 4 97.07 149.41 3.10 0.095 1.48 0 -4 8 56.23 35.76 3.09 0.046 1.20 -3 -7 5 1.01 14.24 3.05 0.029 1.06 2 -1 4 5.37 11.58 3.03 0.026 1.79 3 -4 6 133.22 98.74 3.00 0.077 1.18 3 -3 2 8.36 0.49 2.97 0.005 1.89 -2 2 5 27.66 43.51 2.94 0.051 1.85 -6 8 3 -2.85 5.35 2.89 0.018 0.97 -3 3 3 56.17 40.65 2.88 0.049 2.03 -6 -5 3 22.33 44.90 2.87 0.052 0.94 -4 7 5 23.02 41.42 2.86 0.050 1.07 3 -3 5 24.91 46.07 2.84 0.053 1.34 -6 4 5 222.65 171.29 2.82 0.102 1.19 5 -1 6 12.25 29.20 2.77 0.042 0.93 2 -2 7 -0.26 6.81 2.74 0.020 1.20 -5 0 10 -0.11 12.79 2.74 0.028 1.01 0 -7 7 36.08 51.03 2.72 0.055 1.08 1 1 2 44.69 33.20 2.67 0.045 2.91 2 0 2 59.24 43.24 2.66 0.051 2.44 -4 -7 5 3.15 19.02 2.66 0.034 0.98 0 6 9 34.26 0.67 2.63 0.006 0.79 -1 2 3 169.68 132.76 2.62 0.089 2.64 -3 1 3 182.03 231.98 2.62 0.118 2.42 -7 -1 6 44.32 59.58 2.61 0.060 1.04 1 0 0 1335.84 1733.69 2.58 0.323 7.08 4 -1 5 4.58 11.88 2.58 0.027 1.15 -3 -6 6 107.30 80.29 2.58 0.070 1.13 -3 -6 11 -6.21 5.54 2.57 0.018 0.86 3 0 7 29.89 44.17 2.56 0.052 1.03 1 2 8 46.92 29.10 2.56 0.042 1.03 5 0 2 15.16 24.88 2.54 0.039 1.23 -8 -3 9 41.73 6.71 2.52 0.020 0.82 1 1 8 44.39 66.36 2.49 0.063 1.08 -6 2 6 198.85 151.88 2.49 0.096 1.21 6 -3 2 5.24 0.20 2.48 0.003 1.12 -6 6 5 -3.16 4.64 2.48 0.017 1.06 2 3 5 4.11 11.87 2.47 0.027 1.19 2 0 5 37.03 26.24 2.47 0.040 1.48 Bond lengths and angles Br1 - Distance Angles C1 1.8874 (0.0055) Br1 - F1 - Distance Angles C9 1.3332 (0.0054) F1 - F2 - Distance Angles C9 1.3493 (0.0059) F2 - F3 - Distance Angles C9 1.3237 (0.0061) F3 - O1 - Distance Angles C8 1.4198 (0.0047) O1 - O2 - Distance Angles C11 1.3696 (0.0051) C12 1.4348 (0.0057) 115.21 (0.32) O2 - C11 C1 - Distance Angles C2 1.3633 (0.0079) C6 1.3764 (0.0076) 119.38 (0.53) Br1 1.8874 (0.0055) 119.97 (0.42) 120.64 (0.46) C1 - C2 C6 C2 - Distance Angles C1 1.3633 (0.0078) C3 1.3791 (0.0073) 119.61 (0.49) C2 - C1 C3 - Distance Angles C2 1.3791 (0.0073) C4 1.3904 (0.0064) 121.99 (0.51) C3 - C2 C4 - Distance Angles C3 1.3904 (0.0064) C5 1.3912 (0.0070) 116.46 (0.48) C7 1.4892 (0.0065) 121.39 (0.46) 122.15 (0.41) C4 - C3 C5 C5 - Distance Angles C6 1.3524 (0.0073) C4 1.3912 (0.0070) 121.56 (0.47) C5 - C6 C6 - Distance Angles C5 1.3524 (0.0073) C1 1.3764 (0.0076) 121.00 (0.53) C6 - C5 C7 - Distance Angles C4 1.4892 (0.0065) C8 1.5296 (0.0063) 113.87 (0.35) C7 - C4 C8 - Distance Angles O1 1.4198 (0.0047) C7 1.5296 (0.0063) 106.59 (0.36) C10 1.5295 (0.0060) 112.48 (0.30) 112.76 (0.33) C9 1.5300 (0.0064) 105.98 (0.32) 108.78 (0.35) 109.94 (0.38) C8 - O1 C7 C10 C9 - Distance Angles F3 1.3237 (0.0061) F1 1.3332 (0.0054) 106.84 (0.46) F2 1.3493 (0.0059) 106.94 (0.37) 105.51 (0.37) C8 1.5300 (0.0064) 112.31 (0.37) 113.40 (0.35) 111.36 (0.45) C9 - F3 F1 F2 C10 - Distance Angles C11 1.3192 (0.0055) C14 1.4965 (0.0061) 120.41 (0.39) C8 1.5295 (0.0060) 118.83 (0.38) 120.43 (0.33) C10 - C11 C14 C11 - Distance Angles C10 1.3192 (0.0055) O2 1.3696 (0.0051) 126.20 (0.40) C11 - C10 C12 - Distance Angles O2 1.4348 (0.0057) C13 1.4959 (0.0066) 111.72 (0.40) C12 - O2 C13 - Distance Angles C12 1.4959 (0.0066) C14 1.5170 (0.0063) 109.76 (0.38) C13 - C12 C14 - Distance Angles C10 1.4965 (0.0061) C13 1.5170 (0.0063) 109.43 (0.35) C14 - C10 FMAP and GRID set by program FMAP 2 1 22 GRID -2.632 -2 -2 2.632 2 2 R1 = 0.1339 for 2944 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.44 at 0.0179 0.1028 0.2465 [ 1.11 A from BR1 ] Deepest hole -0.55 at 0.1016 0.9433 0.9621 [ 1.03 A from BR1 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 2087 / 20145 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.0179 0.8972 0.7535 1.00000 0.05 0.44 1.11 BR1 1.92 C1 2.23 H2 2.39 C2 Q2 1 0.1346 0.8388 0.8216 1.00000 0.05 0.36 0.98 BR1 1.71 C1 2.29 H6 2.34 C6 Q3 1 0.9218 1.8356 0.9308 1.00000 0.05 0.25 1.52 H12A 1.71 BR1 2.46 C12 2.71 H14B Q4 1 0.8148 1.7378 0.8594 1.00000 0.05 0.23 1.21 H12A 1.71 H14B 1.90 C12 2.17 C14 Q5 1 0.3667 1.1058 0.6411 1.00000 0.05 0.21 0.72 C3 0.80 C4 1.51 H3 1.70 C2 Q6 1 1.0191 1.7049 0.6974 1.00000 0.05 0.20 1.86 F3 2.24 BR1 2.51 H14B 2.54 F1 Q7 1 -0.0563 0.7337 0.7449 1.00000 0.05 0.20 1.74 BR1 1.86 H14B 2.43 F3 2.71 C14 Q8 1 0.6809 1.2617 0.6557 1.00000 0.05 0.19 0.73 C7 0.82 C8 1.42 H7A 1.43 H7B Q9 1 0.8661 1.6579 0.9820 1.00000 0.05 0.18 1.30 H12A 1.40 O2 1.58 C12 1.81 H1 Q10 1 0.7452 1.1864 0.9142 1.00000 0.05 0.18 1.78 H11 1.79 H5 2.00 C5 2.23 O1 Shortest distances between peaks (including symmetry equivalents) 6 7 0.97 3 4 1.07 1 2 1.46 2 7 1.47 1 7 1.50 2 6 1.54 4 9 1.58 3 9 1.85 4 7 1.85 1 6 1.98 3 7 2.18 1 3 2.23 2 3 2.36 1 4 2.43 5 8 2.52 3 10 2.67 2 4 2.68 2 10 2.71 4 6 2.79 9 10 2.81 8 10 2.85 7 9 2.95 Time profile in seconds ----------------------- 0.19: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.80: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.66: Structure factors and derivatives 0.92: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.23: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.08: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 10:53:10 Total CPU time: 3.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++