+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 04src0821 started at 15:42:39 on 19-Oct-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 04src0821 in P2(1)/c CELL 0.71073 7.9737 24.1031 7.8367 90.000 118.410 90.000 ZERR 4.00 0.0008 0.0019 0.0007 0.000 0.005 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H S BR UNIT 40 40 12 8 V = 1324.75 F(000) = 752.0 Mu = 6.56 mm-1 Cell Wt = 1544.72 Rho = 1.936 MERG 2 OMIT -3.00 55.00 FMAP 2 PLAN 10 SIZE 0.05 0.14 0.38 ACTA BOND $H WGHT 0.07140 15.18640 L.S. 4 TEMP -153.00 FVAR 0.29577 C10 1 1.549356 0.164884 0.351245 11.00000 0.03401 0.04092 = 0.03223 -0.00121 0.01732 0.00033 AFIX 137 H10A 2 1.616234 0.129807 0.404040 11.00000 -1.50000 H10B 2 1.636709 0.191392 0.339872 11.00000 -1.50000 H10C 2 1.440326 0.158342 0.222883 11.00000 -1.50000 AFIX 0 C7 1 1.274443 0.169860 0.651090 11.00000 0.04205 0.02404 = 0.03938 0.00032 0.02680 -0.00327 AFIX 23 H7A 2 1.383805 0.178476 0.779382 11.00000 -1.20000 H7B 2 1.208200 0.205243 0.594503 11.00000 -1.20000 AFIX 0 C8 1 1.351640 0.147010 0.521811 11.00000 0.04469 0.03343 = 0.04367 0.00965 0.03100 0.00498 AFIX 23 H8A 2 1.243598 0.136518 0.394887 11.00000 -1.20000 H8B 2 1.426703 0.113090 0.581850 11.00000 -1.20000 AFIX 0 C6 1 0.926435 0.124076 0.882173 11.00000 0.04001 0.03437 = 0.03607 0.00298 0.02770 0.00377 C9 1 1.477563 0.188883 0.489334 11.00000 0.05004 0.04172 = 0.04101 0.00315 0.02918 -0.00070 AFIX 23 H9A 2 1.588319 0.198486 0.615489 11.00000 -1.20000 H9B 2 1.404078 0.223262 0.432464 11.00000 -1.20000 AFIX 0 C5 1 1.139597 0.132877 0.681948 11.00000 0.14292 0.06517 = 0.16319 -0.06430 0.14518 -0.06544 C1 1 0.852655 0.137543 1.001047 11.00000 0.05094 0.01462 = 0.04416 -0.00094 0.03347 0.00180 C2 1 0.758980 0.045768 0.867388 11.00000 0.05188 0.02869 = 0.04869 -0.01441 0.03402 -0.01872 C3 1 0.872271 0.069626 0.801633 11.00000 0.03483 0.04131 = 0.02758 0.00749 0.02047 0.00818 C4 1 1.095557 0.085622 0.636194 11.00000 0.38143 0.12503 = 0.41534 -0.18496 0.39052 -0.17837 AFIX 43 H4 2 1.167773 0.070048 0.580466 11.00000 -1.20000 AFIX 0 S1 3 0.716135 0.085801 1.022619 11.00000 0.04386 0.03561 = 0.04149 0.00448 0.03107 -0.00026 S2 3 0.936924 0.037394 0.642778 11.00000 0.05935 0.03163 = 0.05101 -0.01068 0.04220 -0.01039 S3 3 1.072360 0.171139 0.841106 11.00000 0.05150 0.02583 = 0.04746 -0.00458 0.03736 -0.00626 BR1 4 0.883088 0.206255 1.122887 11.00000 0.05547 0.03126 = 0.04529 -0.00004 0.03751 0.00449 BR2 4 0.646490 -0.024820 0.794154 11.00000 0.06393 0.04043 = 0.05273 -0.00577 0.03857 -0.01776 HKLF 4 1.0 0.00 0.00 1.00 0.00 -1.00 0.00 1.00 0.00 0.00 Covalent radii and connectivity table for 04src0821 in P2(1)/c C 0.770 H 0.320 S 1.030 BR 1.140 C10 - C9 C7 - C5 C8 C8 - C7 C9 C6 - C1 C3 S3 C9 - C8 C10 C5 - C4 C7 S3 C1 - C6 S1 Br1 C2 - C3 S1 Br2 C3 - C2 C6 S2 C4 - C5 S2 S1 - C2 C1 S2 - C4 C3 S3 - C6 C5 Br1 - C1 Br2 - C2 10682 Reflections read, of which 219 rejected -9 =< h =< 10, -30 =< k =< 31, -9 =< l =< 10, Max. 2-theta = 54.98 0 Systematic absence violations 0 Inconsistent equivalents 3000 Unique reflections, of which 0 suppressed R(int) = 0.0887 R(sigma) = 0.0936 Friedel opposites merged Maximum memory for data reduction = 1422 / 30466 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 = 1799 / 172736 wR2 = 0.2113 before cycle 1 for 3000 data and 137 / 137 parameters GooF = S = 1.067; Restrained GooF = 1.067 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0714 * P )^2 + 15.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.29577 0.00115 -0.004 OSF Mean shift/su = 0.002 Maximum = 0.008 for y Br1 Max. shift = 0.000 A for C4 Max. dU = 0.000 for C4 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1799 / 172736 wR2 = 0.2113 before cycle 2 for 3000 data and 137 / 137 parameters GooF = S = 1.067; Restrained GooF = 1.067 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0714 * P )^2 + 15.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.29577 0.00115 0.000 OSF Mean shift/su = 0.001 Maximum = -0.003 for U12 Br1 Max. shift = 0.000 A for H10B Max. dU = 0.000 for C5 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1799 / 172736 wR2 = 0.2113 before cycle 3 for 3000 data and 137 / 137 parameters GooF = S = 1.067; Restrained GooF = 1.067 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0714 * P )^2 + 15.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.29577 0.00115 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for U22 C4 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C4 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1799 / 172736 wR2 = 0.2113 before cycle 4 for 3000 data and 137 / 137 parameters GooF = S = 1.067; Restrained GooF = 1.067 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0714 * P )^2 + 15.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.29577 0.00115 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z S1 Max. shift = 0.000 A for C4 Max. dU = 0.000 for C4 Largest correlation matrix elements 0.951 U13 C4 / U33 C4 0.818 U33 C4 / U11 C4 0.713 U13 C1 / U11 C1 0.950 U13 C4 / U11 C4 0.757 U13 Br1 / U11 Br1 0.711 U13 S3 / U33 S3 0.939 U12 C4 / U23 C4 0.747 U13 S2 / U11 S2 0.709 U13 C6 / U11 C6 0.914 z C4 / x C4 0.743 U13 S3 / U11 S3 0.708 U13 C8 / U11 C8 0.890 U13 C5 / U11 C5 0.730 U13 Br1 / U33 Br1 0.707 U13 C2 / U11 C2 0.887 U13 C5 / U33 C5 0.728 U13 S1 / U11 S1 -0.697 U13 C4 / U23 C4 0.857 U12 C5 / U23 C5 0.727 U13 S2 / U33 S2 -0.697 U23 C4 / U33 C4 0.842 z C5 / x C5 0.725 U13 Br2 / U11 Br2 -0.693 U12 C4 / U11 C4 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H10A 1.6162 0.1298 0.4040 137 0.980 0.000 C10 C9 H10A H10B 1.6367 0.1914 0.3398 137 0.980 0.000 C10 C9 H10A H10C 1.4403 0.1583 0.2229 137 0.980 0.000 C10 C9 H10A H7A 1.3838 0.1785 0.7794 23 0.990 0.000 C7 C5 C8 H7B 1.2082 0.2052 0.5945 23 0.990 0.000 C7 C5 C8 H8A 1.2436 0.1365 0.3949 23 0.990 0.000 C8 C7 C9 H8B 1.4267 0.1131 0.5819 23 0.990 0.000 C8 C7 C9 H9A 1.5883 0.1985 0.6155 23 0.990 0.000 C9 C8 C10 H9B 1.4041 0.2233 0.4325 23 0.990 0.000 C9 C8 C10 H4 1.1678 0.0700 0.5805 43 0.950 0.000 C4 C5 S2 04src0821 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C10 1.54936 0.16488 0.35124 1.00000 0.03402 0.04093 0.03223 -0.00120 0.01733 0.00033 0.03509 0.02191 0.00141 0.00044 0.00137 0.00000 0.00530 0.00607 0.00480 0.00436 0.00437 0.00442 0.00222 H10A 1.61625 0.12981 0.40405 1.00000 0.05263 0.00000 0.00000 H10B 1.63669 0.19139 0.33985 1.00000 0.05263 0.00000 0.00000 H10C 1.44032 0.15834 0.22289 1.00000 0.05263 0.00000 0.00000 C7 1.27444 0.16986 0.65109 1.00000 0.04206 0.02406 0.03938 0.00034 0.02681 -0.00325 0.03212 0.02213 0.00144 0.00039 0.00144 0.00000 0.00567 0.00501 0.00509 0.00411 0.00468 0.00419 0.00211 H7A 1.38380 0.17848 0.77938 1.00000 0.03854 0.00000 0.00000 H7B 1.20820 0.20524 0.59450 1.00000 0.03854 0.00000 0.00000 C8 1.35164 0.14701 0.52182 1.00000 0.04469 0.03342 0.04366 0.00963 0.03099 0.00495 0.03650 0.02436 0.00147 0.00044 0.00150 0.00000 0.00594 0.00559 0.00546 0.00460 0.00499 0.00460 0.00228 H8A 1.24361 0.13652 0.39489 1.00000 0.04380 0.00000 0.00000 H8B 1.42671 0.11309 0.58186 1.00000 0.04380 0.00000 0.00000 C6 0.92643 0.12408 0.88217 1.00000 0.04000 0.03436 0.03607 0.00299 0.02770 0.00379 0.03287 0.02215 0.00137 0.00042 0.00135 0.00000 0.00559 0.00575 0.00501 0.00425 0.00465 0.00431 0.00219 C9 1.47757 0.18889 0.48934 1.00000 0.05005 0.04171 0.04100 0.00314 0.02917 -0.00070 0.04117 0.02468 0.00160 0.00046 0.00153 0.00000 0.00658 0.00631 0.00556 0.00495 0.00527 0.00511 0.00248 H9A 1.58833 0.19849 0.61550 1.00000 0.04941 0.00000 0.00000 H9B 1.40408 0.22327 0.43247 1.00000 0.04941 0.00000 0.00000 C5 1.13960 0.13288 0.68195 1.00000 0.14289 0.06516 0.16316 -0.06429 0.14515 -0.06544 0.09408 0.03718 0.00255 0.00061 0.00275 0.00000 0.01428 0.00960 0.01546 0.01024 0.01403 0.00976 0.00654 C1 0.85266 0.13754 1.00106 1.00000 0.05092 0.01460 0.04416 -0.00094 0.03345 0.00181 0.03212 0.02225 0.00145 0.00037 0.00143 0.00000 0.00605 0.00453 0.00531 0.00398 0.00500 0.00402 0.00214 C2 0.75898 0.04576 0.86738 1.00000 0.05189 0.02868 0.04867 -0.01438 0.03402 -0.01871 0.03894 0.02228 0.00155 0.00042 0.00153 0.00000 0.00656 0.00554 0.00596 0.00473 0.00546 0.00472 0.00247 C3 0.87227 0.06963 0.80163 1.00000 0.03483 0.04134 0.02758 0.00749 0.02047 0.00818 0.03228 0.02206 0.00135 0.00043 0.00128 0.00000 0.00534 0.00598 0.00453 0.00417 0.00426 0.00434 0.00217 C4 1.09557 0.08562 0.63621 1.00000 0.38154 0.12503 0.41545 -0.18502 0.39061 -0.17843 0.22492 0.06055 0.00441 0.00087 0.00463 0.00000 0.03792 0.01713 0.04090 0.02335 0.03821 0.02234 0.01878 H4 1.16781 0.07004 0.58052 1.00000 0.26991 0.00000 0.00000 S1 0.71614 0.08580 1.02262 1.00000 0.04386 0.03560 0.04149 0.00448 0.03106 -0.00026 0.03591 0.00590 0.00037 0.00011 0.00036 0.00000 0.00148 0.00144 0.00133 0.00112 0.00123 0.00113 0.00060 S2 0.93692 0.03739 0.64278 1.00000 0.05935 0.03163 0.05101 -0.01067 0.04220 -0.01039 0.04080 0.00625 0.00042 0.00011 0.00041 0.00000 0.00173 0.00137 0.00153 0.00119 0.00144 0.00121 0.00066 S3 1.07236 0.17114 0.84111 1.00000 0.05150 0.02583 0.04745 -0.00458 0.03736 -0.00626 0.03593 0.00586 0.00038 0.00010 0.00038 0.00000 0.00159 0.00129 0.00143 0.00108 0.00133 0.00109 0.00061 Br1 0.88309 0.20626 1.12289 1.00000 0.05547 0.03126 0.04529 -0.00004 0.03751 0.00449 0.03845 0.00252 0.00016 0.00004 0.00015 0.00000 0.00068 0.00057 0.00058 0.00044 0.00053 0.00046 0.00032 Br2 0.64649 -0.02482 0.79415 1.00000 0.06393 0.04043 0.05273 -0.00577 0.03856 -0.01776 0.04793 0.00255 0.00018 0.00005 0.00017 0.00000 0.00080 0.00068 0.00068 0.00051 0.00062 0.00054 0.00037 Final Structure Factor Calculation for 04src0821 in P2(1)/c Total number of l.s. parameters = 137 Maximum vector length = 511 Memory required = 1662 / 22995 wR2 = 0.2112 before cycle 5 for 3000 data and 0 / 137 parameters GooF = S = 1.067; Restrained GooF = 1.067 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0714 * P )^2 + 15.19 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0806 for 2089 Fo > 4sig(Fo) and 0.1188 for all 3000 data wR2 = 0.2112, GooF = S = 1.067, Restrained GooF = 1.067 for all data Occupancy sum of asymmetric unit = 15.00 for non-hydrogen and 10.00 for hydrogen atoms Principal mean square atomic displacements U 0.0412 0.0344 0.0297 C10 0.0461 0.0287 0.0216 C7 0.0544 0.0326 0.0225 C8 0.0461 0.0330 0.0195 C6 0.0519 0.0429 0.0287 C9 0.2360 0.0334 0.0129 C5 may be split into 1.1688 0.1291 0.6985 and 1.1104 0.1366 0.6654 0.0554 0.0269 0.0140 C1 0.0672 0.0314 0.0183 C2 0.0481 0.0295 0.0192 C3 0.6250 0.0355 0.0142 C4 may be split into 1.1458 0.0794 0.6640 and 1.0453 0.0918 0.6084 0.0504 0.0368 0.0206 S1 0.0703 0.0284 0.0236 S2 0.0602 0.0253 0.0223 S3 0.0608 0.0326 0.0219 Br1 0.0748 0.0423 0.0267 Br2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.012 0.020 0.030 0.041 0.053 0.067 0.085 0.114 0.169 1.000 Number in group 331. 269. 305. 306. 295. 300. 304. 297. 291. 302. GooF 1.161 1.180 1.024 0.946 0.981 1.146 1.056 1.090 1.067 0.992 K 5.836 2.028 1.342 1.178 1.021 1.030 1.057 1.016 0.995 1.006 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.31 1.67 inf Number in group 303. 301. 303. 300. 298. 296. 301. 296. 300. 302. GooF 0.991 0.964 0.960 0.995 1.089 1.070 1.150 1.149 1.210 1.062 K 0.957 1.094 1.089 1.118 1.077 1.007 1.016 1.006 0.999 1.011 R1 0.288 0.231 0.207 0.179 0.142 0.127 0.115 0.075 0.060 0.041 Recommended weighting scheme: WGHT 0.0715 15.1646 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)/su Fc/Fc(max) Resolution(A) 1 15 1 4240.41 9691.99 6.51 0.296 1.49 1 17 3 2375.13 4698.08 4.90 0.206 1.14 -2 15 1 -43.55 317.62 4.89 0.054 1.49 6 0 0 1219.29 361.80 4.88 0.057 1.17 2 0 0 174.77 2.96 4.81 0.005 3.51 1 4 5 240.40 21.57 4.25 0.014 1.22 -3 6 5 175.52 7.99 4.21 0.008 1.45 1 11 4 3296.29 5447.79 4.08 0.222 1.25 -1 12 8 377.06 1023.12 4.02 0.096 0.83 4 9 4 386.59 1002.06 3.84 0.095 0.95 2 10 4 176.18 0.05 3.78 0.001 1.16 4 1 0 186.07 17.47 3.75 0.013 1.75 0 6 3 277.65 70.13 3.70 0.025 1.99 -1 9 4 380.08 123.12 3.66 0.033 1.55 3 7 2 134.39 3.91 3.62 0.006 1.46 4 0 2 8929.84 5139.74 3.51 0.215 1.33 0 19 5 1165.92 2368.31 3.41 0.146 0.93 2 7 3 1123.29 1974.12 3.20 0.133 1.45 4 7 1 112.12 2.37 3.20 0.005 1.40 2 4 1 637.31 291.54 3.17 0.051 2.43 -2 9 5 125.77 3.80 3.12 0.006 1.35 4 11 4 1933.26 1205.74 3.12 0.104 0.92 -6 7 1 246.92 53.84 3.08 0.022 1.18 -5 7 1 186.18 40.43 3.03 0.019 1.39 2 2 7 151.46 0.91 3.03 0.003 0.85 -3 9 7 341.03 93.85 3.01 0.029 1.03 -3 14 2 1759.77 3009.63 2.97 0.165 1.43 -3 4 1 1534.51 999.43 2.94 0.095 2.41 -5 12 5 1893.17 3094.58 2.93 0.167 1.12 -5 7 8 171.58 19.34 2.91 0.013 0.93 -6 20 7 -348.95 382.36 2.91 0.059 0.78 -9 5 1 963.46 448.43 2.89 0.064 0.81 4 23 2 1273.43 517.66 2.88 0.068 0.82 0 2 6 195.41 35.56 2.84 0.018 1.14 -1 1 4 621.14 341.39 2.82 0.055 1.89 -3 7 8 154.80 19.87 2.80 0.013 0.94 3 5 1 227.43 74.53 2.78 0.026 1.81 6 2 0 1138.36 615.42 2.78 0.074 1.16 0 15 7 173.07 581.38 2.77 0.072 0.84 2 24 1 884.85 367.68 2.73 0.058 0.94 3 24 2 3742.02 2533.28 2.71 0.151 0.85 6 15 0 975.91 1785.83 2.70 0.127 0.95 2 12 4 173.45 21.95 2.69 0.014 1.10 4 10 4 460.38 949.96 2.69 0.093 0.93 5 21 0 1018.05 490.79 2.66 0.067 0.89 2 2 4 1355.82 1984.08 2.66 0.134 1.31 -10 6 5 382.96 874.42 2.65 0.089 0.78 0 12 5 117.78 338.44 2.65 0.055 1.14 -9 8 8 116.83 424.20 2.64 0.062 0.77 0 6 5 124.54 25.43 2.63 0.015 1.30 Bond lengths and angles C10 - Distance Angles C9 1.5566 (0.0128) H10A 0.9800 109.47 H10B 0.9800 109.47 109.47 H10C 0.9800 109.47 109.47 109.47 C10 - C9 H10A H10B C7 - Distance Angles C5 1.5022 (0.0138) C8 1.5172 (0.0123) 116.17 (0.87) H7A 0.9900 108.25 108.25 H7B 0.9900 108.25 108.25 107.37 C7 - C5 C8 H7A C8 - Distance Angles C7 1.5172 (0.0123) C9 1.5281 (0.0135) 112.27 (0.87) H8A 0.9900 109.15 109.15 H8B 0.9900 109.15 109.15 107.87 C8 - C7 C9 H8A C6 - Distance Angles C1 1.3568 (0.0117) C3 1.4310 (0.0140) 112.57 (0.82) S3 1.7609 (0.0095) 120.76 (0.78) 126.67 (0.63) C6 - C1 C3 C9 - Distance Angles C8 1.5281 (0.0135) C10 1.5566 (0.0128) 111.00 (0.87) H9A 0.9900 109.44 109.44 H9B 0.9900 109.44 109.44 108.03 C9 - C8 C10 H9A C5 - Distance Angles C4 1.1957 (0.0197) C7 1.5022 (0.0138) 130.37 (1.16) S3 1.8248 (0.0116) 123.13 (1.01) 106.01 (0.81) C5 - C4 C7 C1 - Distance Angles C6 1.3568 (0.0117) S1 1.7158 (0.0094) 113.35 (0.72) Br1 1.8689 (0.0090) 124.72 (0.73) 121.87 (0.49) C1 - C6 S1 C2 - Distance Angles C3 1.3621 (0.0127) S1 1.7098 (0.0098) 115.08 (0.76) Br2 1.8811 (0.0096) 124.91 (0.76) 119.99 (0.52) C2 - C3 S1 C3 - Distance Angles C2 1.3621 (0.0127) C6 1.4310 (0.0140) 109.61 (0.79) S2 1.7406 (0.0089) 123.88 (0.83) 126.51 (0.68) C3 - C2 C6 C4 - Distance Angles C5 1.1957 (0.0197) S2 1.7366 (0.0146) 137.98 (1.28) H4 0.9500 111.01 111.01 C4 - C5 S2 S1 - Distance Angles C2 1.7098 (0.0099) C1 1.7158 (0.0095) 89.39 (0.45) S1 - C2 S2 - Distance Angles C4 1.7366 (0.0147) C3 1.7406 (0.0089) 100.96 (0.61) S2 - C4 S3 - Distance Angles C6 1.7609 (0.0095) C5 1.8248 (0.0116) 103.53 (0.49) S3 - C6 Br1 - Distance Angles C1 1.8689 (0.0090) Br1 - Br2 - Distance Angles C2 1.8811 (0.0097) Br2 - FMAP and GRID set by program FMAP 2 2 36 GRID -0.758 -2 -2 0.758 2 2 R1 = 0.1153 for 3000 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.39 at 0.7650 0.2104 0.0321 [ 0.87 A from BR1 ] Deepest hole -1.03 at 0.8254 0.2346 0.6136 [ 1.49 A from BR1 ] Mean = 0.00, Rms deviation from mean = 0.20 e/A^3, Highest memory used = 1677 / 18942 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.7650 0.2104 1.0321 1.00000 0.05 1.39 0.87 BR1 1.95 C1 2.73 H10B 2.83 H7A Q2 1 1.0210 0.1010 0.5531 1.00000 0.05 0.92 0.74 C4 1.26 C5 1.32 H4 1.93 S2 Q3 1 0.8810 0.2433 1.1208 1.00000 0.05 0.76 0.89 BR1 2.65 H10B 2.66 S3 2.69 C1 Q4 1 0.8922 0.1000 1.2606 1.00000 0.05 0.75 1.75 S1 2.11 C1 2.53 H4 2.62 C4 Q5 1 1.0511 0.1432 0.6628 1.00000 0.05 0.74 0.69 C5 1.47 C4 1.49 S3 1.94 C7 Q6 1 1.2810 0.0980 0.8258 1.00000 0.05 0.72 1.43 C5 1.55 C4 1.82 H4 2.19 C7 Q7 1 1.3239 0.1259 0.1106 1.00000 0.05 0.69 1.21 H10C 2.11 C10 2.37 H10A 2.38 S3 Q8 1 0.7611 -0.0110 0.8816 1.00000 0.05 0.69 0.91 BR2 1.37 C2 2.34 C3 2.68 S1 Q9 1 0.9782 0.2041 0.6398 1.00000 0.05 0.67 1.60 S3 2.03 H7B 2.08 C5 2.27 BR1 Q10 1 1.6763 0.1910 0.8473 1.00000 0.05 0.67 1.62 H9A 1.86 C1 2.03 BR1 2.15 H7A Shortest distances between peaks (including symmetry equivalents) 1 3 1.16 2 5 1.28 1 10 1.36 3 9 1.46 5 9 1.56 5 6 1.99 2 4 2.02 2 6 2.16 6 7 2.20 3 10 2.35 1 9 2.55 2 9 2.64 7 8 2.86 4 5 2.97 Time profile in seconds ----------------------- 0.02: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.36: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.33: Structure factors and derivatives 0.34: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.06: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.08: Analysis of variance 0.00: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 04src0821 finished at 15:42:40 Total CPU time: 1.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++