+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2005slh0246 started at 13:33:03 on 10-Apr-2005 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2005slh0246 in P2(1)2(1)2(1) CELL 0.71073 10.9213 11.8985 14.8920 90.000 90.000 90.000 ZERR 4.00 0.0008 0.0007 0.0011 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N BR I UNIT 72 52 24 8 4 V = 1935.17 F(000) = 1144.0 Mu = 5.80 mm-1 Cell Wt = 2400.26 Rho = 2.060 MERG 2 OMIT -3.00 55.00 OMIT 1 3 3 OMIT 3 0 1 OMIT -1 3 3 OMIT 0 3 3 FMAP 2 PLAN 5 SIZE 0.25 0.46 0.60 ACTA BOND $H L.S. 6 TEMP -153.00 WGHT 0.063100 13.695701 EXTI 0.004508 FVAR 0.28414 MOLE 1 C1 1 0.295405 -0.165307 -0.067375 11.00000 0.01805 0.01677 = 0.01307 -0.00274 0.00157 0.00381 C2 1 0.230933 -0.273683 0.047581 11.00000 0.01360 0.02016 = 0.01685 -0.00399 -0.00028 0.00569 C3 1 0.171162 -0.312335 -0.093387 11.00000 0.01350 0.01545 = 0.01420 -0.00258 0.00067 0.00230 C4 1 0.363162 -0.067101 -0.102744 11.00000 0.01420 0.01618 = 0.01518 -0.00101 0.00039 0.00140 C5 1 0.349343 -0.025989 -0.188037 11.00000 0.01889 0.02313 = 0.01842 -0.00062 -0.00228 0.00087 AFIX 43 H5 2 0.295842 -0.062817 -0.228832 11.00000 -1.20000 AFIX 0 C6 1 0.413215 0.069541 -0.215475 11.00000 0.02142 0.01838 = 0.01683 0.00759 -0.00111 0.00389 AFIX 43 H6 2 0.401128 0.099054 -0.274082 11.00000 -1.20000 AFIX 0 C7 1 0.494719 0.121570 -0.156818 11.00000 0.02620 0.01943 = 0.02507 0.00080 0.00787 0.00073 AFIX 43 H7 2 0.538689 0.187075 -0.173859 11.00000 -1.20000 AFIX 0 C8 1 0.509097 0.073888 -0.072525 11.00000 0.01802 0.01924 = 0.01995 0.00040 0.00242 -0.00163 AFIX 43 H8 2 0.566005 0.106358 -0.031847 11.00000 -1.20000 AFIX 0 C9 1 0.233429 -0.299606 0.145804 11.00000 0.01668 0.02113 = 0.01106 -0.00432 0.00098 0.00516 C10 1 0.154356 -0.377170 0.174612 11.00000 0.02431 0.02832 = 0.00298 0.00405 -0.00071 -0.00987 AFIX 43 H10 2 0.099444 -0.414329 0.135036 11.00000 -1.20000 AFIX 0 C11 1 0.157234 -0.399646 0.263802 11.00000 0.03498 0.03628 = 0.01872 0.00510 0.00013 -0.00922 AFIX 43 H11 2 0.102773 -0.455020 0.286537 11.00000 -1.20000 AFIX 0 C12 1 0.234444 -0.346892 0.323207 11.00000 0.02839 0.03795 = 0.01019 -0.00117 -0.00025 0.00487 AFIX 43 H12 2 0.233179 -0.366315 0.385076 11.00000 -1.20000 AFIX 0 C13 1 0.311828 -0.267517 0.292998 11.00000 0.03072 0.03005 = 0.02071 0.00083 -0.00622 0.00176 AFIX 43 H13 2 0.365298 -0.229734 0.333254 11.00000 -1.20000 AFIX 0 C14 1 0.107022 -0.385646 -0.159160 11.00000 0.01596 0.01515 = 0.01347 -0.00139 -0.00320 0.00339 C15 1 0.024322 -0.458036 -0.125851 11.00000 0.00696 0.01137 = 0.00593 -0.00234 -0.00094 -0.00004 AFIX 43 H15 2 0.007001 -0.460419 -0.063365 11.00000 -1.20000 AFIX 0 C16 1 -0.033369 -0.527204 -0.183707 11.00000 0.01433 0.02485 = 0.02583 -0.00121 -0.00262 -0.00089 AFIX 43 H16 2 -0.092211 -0.578702 -0.161027 11.00000 -1.20000 AFIX 0 C17 1 -0.009866 -0.525789 -0.274903 11.00000 0.01904 0.02914 = 0.02050 -0.00710 -0.00357 0.00167 AFIX 43 H17 2 -0.050989 -0.576525 -0.313848 11.00000 -1.20000 AFIX 0 C18 1 0.072389 -0.451362 -0.308299 11.00000 0.02885 0.02455 = 0.01532 -0.00636 -0.00157 -0.00201 AFIX 43 H18 2 0.087580 -0.447772 -0.371046 11.00000 -1.20000 AFIX 0 N1 3 0.233368 -0.224121 -0.127807 11.00000 0.01579 0.01790 = 0.01250 0.00169 -0.00256 0.00089 N2 3 0.301461 -0.185176 0.019267 11.00000 0.01996 0.01207 = 0.01314 0.00189 -0.00069 0.00288 N3 3 0.166254 -0.338086 -0.006484 11.00000 0.01594 0.01803 = 0.01331 -0.00186 -0.00396 0.00507 N4 3 0.444879 -0.016976 -0.046612 11.00000 0.01643 0.02637 = 0.00975 -0.00240 -0.00245 -0.00455 AFIX 43 H4 2 0.455929 -0.044495 0.007635 10.33333 -1.20000 AFIX 0 N5 3 0.312389 -0.241910 0.203107 11.00000 0.03896 0.03853 = 0.02550 -0.00475 -0.00471 -0.00066 AFIX 43 H5A 2 0.361852 -0.189856 0.181981 10.33333 -1.20000 AFIX 0 N6 3 0.134453 -0.380116 -0.249436 11.00000 0.03250 0.03565 = 0.02466 -0.00029 0.00015 -0.00481 AFIX 43 H6A 2 0.189900 -0.332680 -0.269484 10.33333 -1.20000 AFIX 0 MOLE 2 BR2 4 -0.023350 -0.089018 0.039905 11.00000 0.03143 0.03638 = 0.03760 -0.00235 -0.00289 -0.00665 BR1 4 0.291451 0.249964 0.048117 11.00000 0.05424 0.03694 = 0.03568 0.00026 -0.00306 -0.00147 I1 5 0.129559 0.083219 0.044210 11.00000 0.02110 0.02094 = 0.01364 -0.00193 -0.00088 0.00393 HKLF 4 Covalent radii and connectivity table for 2005slh0246 in P2(1)2(1)2(1) C 0.770 H 0.320 N 0.700 BR 1.140 I 1.330 C1 - N2 N1 C4 C2 - N3 N2 C9 C3 - N3 N1 C14 C4 - N4 C5 C1 C5 - C4 C6 C6 - C7 C5 C7 - C8 C6 C8 - N4 C7 C9 - C10 N5 C2 C10 - C9 C11 C11 - C10 C12 C12 - C13 C11 C13 - C12 N5 C14 - C15 N6 C3 C15 - C14 C16 C16 - C15 C17 C17 - C18 C16 C18 - C17 N6 N1 - C1 C3 N2 - C1 C2 N3 - C2 C3 N4 - C8 C4 N5 - C13 C9 N6 - C14 C18 Br2 - I1 Br1 - I1 I1 - Br2 Br1 h k l Fo^2 Sigma Why rejected 0 0 3 5.63 1.21 observed but should be systematically absent 21904 Reflections read, of which 97 rejected -13 =< h =< 14, -14 =< k =< 15, -18 =< l =< 19, Max. 2-theta = 54.98 1 Systematic absence violations 0 Inconsistent equivalents 4405 Unique reflections, of which 0 suppressed R(int) = 0.0343 R(sigma) = 0.0332 Friedel opposites not merged Maximum memory for data reduction = 2218 / 44130 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 = 2865 / 305032 wR2 = 0.1303 before cycle 1 for 4405 data and 245 / 245 parameters GooF = S = 1.102; Restrained GooF = 1.102 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0631 * P )^2 + 13.70 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.28403 0.00081 -0.130 OSF 2 0.00448 0.00047 -0.067 EXTI Mean shift/esd = 0.059 Maximum = 0.395 for x C6 Max. shift = 0.003 A for H6 Max. dU = 0.000 for C10 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2865 / 305032 wR2 = 0.1303 before cycle 2 for 4405 data and 245 / 245 parameters GooF = S = 1.102; Restrained GooF = 1.102 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0631 * P )^2 + 13.70 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.28400 0.00081 -0.039 OSF 2 0.00446 0.00047 -0.031 EXTI Mean shift/esd = 0.023 Maximum = 0.133 for x C6 Max. shift = 0.001 A for C18 Max. dU = 0.000 for N5 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2865 / 305032 wR2 = 0.1303 before cycle 3 for 4405 data and 245 / 245 parameters GooF = S = 1.102; Restrained GooF = 1.102 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0631 * P )^2 + 13.70 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.28400 0.00081 -0.005 OSF 2 0.00446 0.00047 -0.005 EXTI Mean shift/esd = 0.003 Maximum = -0.021 for U11 C18 Max. shift = 0.000 A for N5 Max. dU = 0.000 for C18 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2865 / 305032 wR2 = 0.1303 before cycle 4 for 4405 data and 245 / 245 parameters GooF = S = 1.102; Restrained GooF = 1.102 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0631 * P )^2 + 13.70 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.28400 0.00081 0.000 OSF 2 0.00446 0.00047 0.000 EXTI Mean shift/esd = 0.001 Maximum = 0.003 for U22 N6 Max. shift = 0.000 A for C16 Max. dU = 0.000 for N6 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2865 / 305032 wR2 = 0.1303 before cycle 5 for 4405 data and 245 / 245 parameters GooF = S = 1.102; Restrained GooF = 1.102 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0631 * P )^2 + 13.70 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.28400 0.00081 0.000 OSF 2 0.00446 0.00047 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for U22 N6 Max. shift = 0.000 A for C17 Max. dU = 0.000 for C6 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2865 / 305032 wR2 = 0.1303 before cycle 6 for 4405 data and 245 / 245 parameters GooF = S = 1.102; Restrained GooF = 1.102 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0631 * P )^2 + 13.70 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.28400 0.00081 -0.001 OSF 2 0.00446 0.00047 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for C10 Max. dU = 0.000 for C7 Largest correlation matrix elements 0.656 EXTI / OSF 0.588 U11 I1 / OSF 0.601 U33 I1 / OSF 0.587 U22 I1 / OSF Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H5 0.2958 -0.0627 -0.2288 43 0.950 0.000 C5 C4 C6 H6 0.4017 0.0990 -0.2741 43 0.950 0.000 C6 C7 C5 H7 0.5387 0.1870 -0.1738 43 0.950 0.000 C7 C8 C6 H8 0.5657 0.1066 -0.0318 43 0.950 0.000 C8 N4 C7 H10 0.0994 -0.4144 0.1349 43 0.950 0.000 C10 C9 C11 H11 0.1024 -0.4546 0.2867 43 0.950 0.000 C11 C10 C12 H12 0.2337 -0.3664 0.3851 43 0.950 0.000 C12 C13 C11 H13 0.3653 -0.2294 0.3330 43 0.950 0.000 C13 C12 N5 H15 0.0071 -0.4606 -0.0634 43 0.950 0.000 C15 C14 C16 H16 -0.0926 -0.5783 -0.1610 43 0.950 0.000 C16 C15 C17 H17 -0.0511 -0.5767 -0.3137 43 0.950 0.000 C17 C18 C16 H18 0.0879 -0.4476 -0.3710 43 0.950 0.000 C18 C17 N6 H4 0.4561 -0.0445 0.0075 43 0.880 0.000 N4 C8 C4 H5A 0.3619 -0.1901 0.1821 43 0.880 0.000 N5 C13 C9 H6A 0.1903 -0.3329 -0.2695 43 0.880 0.000 N6 C14 C18 2005slh0246 in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.29534 -0.16546 -0.06731 1.00000 0.01826 0.01668 0.01288 -0.00267 0.00172 0.00389 0.01594 0.01231 0.00066 0.00057 0.00047 0.00000 0.00344 0.00319 0.00330 0.00235 0.00256 0.00271 0.00143 C2 0.23099 -0.27373 0.04749 1.00000 0.01356 0.02030 0.01706 -0.00381 -0.00016 0.00578 0.01697 0.01213 0.00058 0.00055 0.00052 0.00000 0.00285 0.00316 0.00313 0.00309 0.00300 0.00241 0.00128 C3 0.17120 -0.31220 -0.09337 1.00000 0.01322 0.01556 0.01423 -0.00259 0.00076 0.00243 0.01434 0.01258 0.00066 0.00060 0.00048 0.00000 0.00310 0.00318 0.00325 0.00261 0.00260 0.00258 0.00134 C4 0.36327 -0.06707 -0.10277 1.00000 0.01435 0.01626 0.01517 -0.00113 0.00048 0.00149 0.01526 0.01159 0.00063 0.00055 0.00044 0.00000 0.00305 0.00315 0.00291 0.00243 0.00251 0.00272 0.00128 C5 0.34939 -0.02602 -0.18806 1.00000 0.01924 0.02286 0.01821 -0.00031 -0.00227 0.00092 0.02010 0.01311 0.00067 0.00062 0.00051 0.00000 0.00367 0.00354 0.00334 0.00281 0.00277 0.00276 0.00148 H5 0.29579 -0.06275 -0.22884 1.00000 0.02412 0.00000 0.00000 C6 0.41357 0.06952 -0.21544 1.00000 0.02152 0.01840 0.01661 0.00732 -0.00122 0.00368 0.01885 0.01325 0.00068 0.00061 0.00049 0.00000 0.00331 0.00342 0.00319 0.00291 0.00262 0.00279 0.00141 H6 0.40175 0.09898 -0.27410 1.00000 0.02261 0.00000 0.00000 C7 0.49474 0.12146 -0.15681 1.00000 0.02539 0.01973 0.02541 0.00085 0.00765 0.00070 0.02351 0.01441 0.00076 0.00065 0.00054 0.00000 0.00391 0.00344 0.00388 0.00292 0.00317 0.00301 0.00159 H7 0.53874 0.18696 -0.17383 1.00000 0.02821 0.00000 0.00000 C8 0.50896 0.07395 -0.07258 1.00000 0.01796 0.01925 0.02000 0.00084 0.00253 -0.00161 0.01907 0.01299 0.00066 0.00064 0.00047 0.00000 0.00321 0.00326 0.00327 0.00278 0.00254 0.00300 0.00137 H8 0.56566 0.10658 -0.03184 1.00000 0.02288 0.00000 0.00000 C9 0.23363 -0.29965 0.14585 1.00000 0.01653 0.02112 0.01104 -0.00406 0.00112 0.00491 0.01623 0.01244 0.00066 0.00061 0.00045 0.00000 0.00333 0.00334 0.00312 0.00266 0.00263 0.00270 0.00136 C10 0.15428 -0.37726 0.17455 1.00000 0.02507 0.02841 0.00296 0.00422 -0.00085 -0.01010 0.01881 0.01280 0.00071 0.00067 0.00044 0.00000 0.00397 0.00371 0.00287 0.00260 0.00256 0.00293 0.00157 H10 0.09943 -0.41443 0.13494 1.00000 0.02257 0.00000 0.00000 C11 0.15708 -0.39954 0.26387 1.00000 0.03538 0.03685 0.01863 0.00543 0.00014 -0.00966 0.03029 0.01517 0.00080 0.00078 0.00054 0.00000 0.00450 0.00471 0.00382 0.00338 0.00315 0.00379 0.00188 H11 0.10238 -0.45465 0.28671 1.00000 0.03635 0.00000 0.00000 C12 0.23467 -0.34684 0.32326 1.00000 0.02853 0.03775 0.01023 -0.00174 -0.00033 0.00479 0.02550 0.01430 0.00079 0.00072 0.00051 0.00000 0.00425 0.00452 0.00340 0.00305 0.00306 0.00342 0.00170 H12 0.23371 -0.36637 0.38512 1.00000 0.03060 0.00000 0.00000 C13 0.31192 -0.26737 0.29285 1.00000 0.03018 0.03001 0.02072 0.00105 -0.00609 0.00188 0.02697 0.01448 0.00079 0.00072 0.00053 0.00000 0.00427 0.00421 0.00387 0.00319 0.00328 0.00334 0.00171 H13 0.36533 -0.22938 0.33303 1.00000 0.03236 0.00000 0.00000 C14 0.10721 -0.38572 -0.15920 1.00000 0.01576 0.01545 0.01348 -0.00128 -0.00325 0.00348 0.01490 0.01162 0.00062 0.00056 0.00046 0.00000 0.00338 0.00311 0.00304 0.00243 0.00253 0.00247 0.00138 C15 0.02434 -0.45812 -0.12590 1.00000 0.00719 0.01126 0.00586 -0.00215 -0.00101 -0.00025 0.00810 0.01040 0.00056 0.00051 0.00041 0.00000 0.00273 0.00269 0.00268 0.00215 0.00220 0.00218 0.00113 H15 0.00712 -0.46056 -0.06340 1.00000 0.00972 0.00000 0.00000 C16 -0.03355 -0.52710 -0.18369 1.00000 0.01486 0.02426 0.02569 -0.00113 -0.00252 -0.00085 0.02160 0.01325 0.00069 0.00066 0.00055 0.00000 0.00343 0.00372 0.00400 0.00314 0.00299 0.00285 0.00154 H16 -0.09264 -0.57835 -0.16100 1.00000 0.02593 0.00000 0.00000 C17 -0.01000 -0.52589 -0.27480 1.00000 0.01920 0.02903 0.02047 -0.00698 -0.00359 0.00170 0.02290 0.01331 0.00072 0.00068 0.00052 0.00000 0.00361 0.00402 0.00367 0.00303 0.00301 0.00307 0.00158 H17 -0.05109 -0.57665 -0.31375 1.00000 0.02748 0.00000 0.00000 C18 0.07271 -0.45122 -0.30823 1.00000 0.02875 0.02451 0.01545 -0.00630 -0.00125 -0.00207 0.02290 0.01308 0.00076 0.00064 0.00053 0.00000 0.00408 0.00370 0.00343 0.00292 0.00310 0.00303 0.00160 H18 0.08792 -0.44759 -0.37097 1.00000 0.02748 0.00000 0.00000 N1 0.23323 -0.22417 -0.12774 1.00000 0.01590 0.01772 0.01229 0.00160 -0.00237 0.00086 0.01531 0.01015 0.00055 0.00049 0.00038 0.00000 0.00281 0.00294 0.00269 0.00221 0.00224 0.00227 0.00118 N2 0.30151 -0.18512 0.01927 1.00000 0.01995 0.01209 0.01306 0.00201 -0.00076 0.00294 0.01503 0.01037 0.00056 0.00047 0.00039 0.00000 0.00298 0.00258 0.00283 0.00202 0.00218 0.00225 0.00119 N3 0.16622 -0.33805 -0.00650 1.00000 0.01596 0.01784 0.01339 -0.00222 -0.00391 0.00509 0.01573 0.01068 0.00058 0.00050 0.00041 0.00000 0.00286 0.00280 0.00278 0.00226 0.00224 0.00222 0.00122 N4 0.44494 -0.01697 -0.04671 1.00000 0.01651 0.02645 0.00970 -0.00237 -0.00269 -0.00466 0.01755 0.00990 0.00049 0.00050 0.00044 0.00000 0.00273 0.00290 0.00253 0.00267 0.00248 0.00221 0.00113 H4 0.45612 -0.04455 0.00751 0.33333 0.02106 0.00000 0.00000 N5 0.31244 -0.24206 0.20322 1.00000 0.03798 0.03840 0.02565 -0.00470 -0.00478 -0.00095 0.03401 0.01319 0.00073 0.00071 0.00049 0.00000 0.00420 0.00406 0.00377 0.00323 0.00319 0.00342 0.00165 H5A 0.36195 -0.19005 0.18208 0.33333 0.04081 0.00000 0.00000 N6 0.13476 -0.38024 -0.24950 1.00000 0.03166 0.03572 0.02472 -0.00037 -0.00011 -0.00452 0.03070 0.01321 0.00075 0.00064 0.00049 0.00000 0.00376 0.00384 0.00343 0.00292 0.00319 0.00326 0.00157 H6A 0.19034 -0.33292 -0.26952 0.33333 0.03684 0.00000 0.00000 Br2 -0.02334 -0.08901 0.03991 1.00000 0.03139 0.03637 0.03759 -0.00243 -0.00286 -0.00663 0.03511 0.00151 0.00007 0.00008 0.00007 0.00000 0.00041 0.00043 0.00045 0.00049 0.00039 0.00036 0.00021 Br1 0.29145 0.24996 0.04814 1.00000 0.05419 0.03690 0.03564 0.00029 -0.00305 -0.00150 0.04224 0.00176 0.00009 0.00008 0.00007 0.00000 0.00056 0.00045 0.00048 0.00046 0.00048 0.00041 0.00025 I1 0.12956 0.08322 0.04421 1.00000 0.02107 0.02092 0.01362 -0.00192 -0.00089 0.00393 0.01854 0.00076 0.00004 0.00004 0.00003 0.00000 0.00022 0.00022 0.00020 0.00019 0.00018 0.00018 0.00015 Final Structure Factor Calculation for 2005slh0246 in P2(1)2(1)2(1) Total number of l.s. parameters = 245 Maximum vector length = 511 Memory required = 2622 / 26068 wR2 = 0.1303 before cycle 7 for 4405 data and 2 / 245 parameters GooF = S = 1.102; Restrained GooF = 1.102 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0631 * P )^2 + 13.70 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0441 for 4005 Fo > 4sig(Fo) and 0.0498 for all 4405 data wR2 = 0.1303, GooF = S = 1.102, Restrained GooF = 1.102 for all data Flack x parameter = 0.1241 with esd 0.0206 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF ** Possible racemic twin or wrong absolute structure - try TWIN refinement ** Occupancy sum of asymmetric unit = 27.00 for non-hydrogen and 13.00 for hydrogen atoms Principal mean square atomic displacements U 0.0215 0.0163 0.0100 C1 0.0251 0.0161 0.0098 C2 0.0181 0.0145 0.0105 C3 0.0174 0.0153 0.0131 C4 0.0233 0.0207 0.0164 C5 0.0259 0.0214 0.0092 C6 0.0331 0.0196 0.0177 C7 0.0217 0.0201 0.0154 C8 0.0249 0.0153 0.0085 C9 0.0374 0.0168 0.0022 C10 0.0464 0.0279 0.0166 C11 0.0399 0.0265 0.0101 C12 0.0336 0.0298 0.0175 C13 0.0206 0.0132 0.0108 C14 0.0120 0.0076 0.0047 C15 0.0266 0.0240 0.0142 C16 0.0337 0.0200 0.0151 C17 0.0298 0.0270 0.0120 C18 0.0182 0.0171 0.0106 N1 0.0209 0.0144 0.0097 N2 0.0238 0.0132 0.0102 N3 0.0284 0.0163 0.0079 N4 0.0403 0.0391 0.0226 N5 0.0387 0.0288 0.0247 N6 0.0410 0.0387 0.0256 Br2 0.0548 0.0368 0.0351 Br1 0.0253 0.0172 0.0132 I1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.030 0.045 0.061 0.078 0.096 0.119 0.145 0.179 0.247 1.000 Number in group 466. 422. 435. 439. 454. 439. 437. 437. 434. 442. GooF 1.094 1.057 1.069 1.245 0.991 0.900 1.322 1.006 1.148 1.127 K 1.157 1.024 0.971 0.985 0.982 1.010 1.013 1.011 1.024 1.007 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.31 1.64 inf Number in group 445. 448. 440. 432. 442. 436. 443. 436. 442. 441. GooF 0.892 0.779 0.841 0.771 0.742 0.570 0.575 0.748 1.355 2.412 K 0.971 1.005 0.999 1.006 1.024 1.029 1.032 1.018 0.996 1.006 R1 0.098 0.068 0.061 0.053 0.044 0.029 0.025 0.027 0.043 0.065 Recommended weighting scheme: WGHT 0.0673 13.1242 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) 0 2 0 3847.67 1830.18 6.74 0.119 5.95 1 0 2 2074.01 4932.45 6.42 0.196 6.15 3 0 6 35.50 500.56 5.88 0.062 2.05 1 2 4 1144.14 2492.65 5.87 0.139 3.03 4 0 1 602.38 167.81 5.78 0.036 2.69 0 2 2 209.04 831.32 5.77 0.080 4.65 -1 2 4 902.91 2034.97 5.65 0.126 3.03 3 0 5 1466.41 2923.91 5.64 0.151 2.31 1 3 5 4567.71 2718.22 5.59 0.145 2.33 0 4 0 2145.49 1104.36 5.59 0.093 2.97 1 4 6 1226.89 2506.99 5.53 0.139 1.88 3 5 3 1437.61 679.32 5.44 0.073 1.85 0 0 6 337.56 27.51 5.40 0.015 2.48 -1 4 6 1246.31 2495.02 5.39 0.139 1.88 -1 2 6 3159.00 5400.76 5.30 0.205 2.24 2 1 6 128.46 576.86 5.10 0.067 2.22 3 1 4 3523.33 2139.20 5.04 0.129 2.54 0 2 5 2305.73 1277.57 4.98 0.100 2.66 -3 1 4 3469.59 2104.65 4.96 0.128 2.54 3 6 4 383.36 96.15 4.94 0.027 1.58 -3 5 3 1374.63 693.67 4.90 0.073 1.85 1 2 6 3311.78 5372.69 4.88 0.204 2.24 4 0 2 17.04 304.28 4.79 0.049 2.56 3 0 7 241.81 739.93 4.74 0.076 1.84 4 0 8 563.14 195.34 4.62 0.039 1.54 6 3 0 261.74 46.72 4.51 0.019 1.65 3 6 3 229.93 31.30 4.49 0.016 1.64 -3 1 3 615.14 237.60 4.43 0.043 2.85 -1 4 2 786.42 1523.17 4.43 0.109 2.68 2 0 1 9981.90 6992.40 4.40 0.233 5.13 3 0 3 1359.87 2345.83 4.36 0.135 2.94 -7 3 4 451.75 144.24 4.33 0.033 1.35 3 0 4 556.66 1162.81 4.32 0.095 2.60 0 4 2 2151.78 1322.17 4.25 0.101 2.76 -1 3 5 4225.84 2824.08 4.24 0.148 2.33 5 1 3 1029.00 540.54 4.12 0.065 1.97 -2 1 6 215.05 626.81 4.11 0.070 2.22 4 0 0 200.18 32.66 4.10 0.016 2.73 1 2 2 1157.55 1993.67 4.08 0.124 4.28 4 5 0 318.35 754.85 4.07 0.076 1.79 -2 3 1 3783.25 2574.89 4.02 0.141 3.14 2 4 0 14158.35 19431.30 3.98 0.388 2.61 0 4 5 9503.85 6927.43 3.96 0.232 2.10 1 3 7 6122.63 4371.85 3.92 0.184 1.85 0 3 1 552.79 245.93 3.91 0.044 3.83 3 2 0 167863.27 128995.52 3.90 1.000 3.11 -5 4 5 1413.05 2283.42 3.84 0.133 1.52 2 1 0 86.89 0.48 3.77 0.002 4.96 1 4 2 606.57 1123.71 3.73 0.093 2.68 2 2 5 2088.62 3156.91 3.72 0.156 2.39 Bond lengths and angles C1 - Distance Angles N2 1.3121 (0.0093) N1 1.3259 (0.0092) 126.82 (0.69) C4 1.4832 (0.0095) 117.70 (0.63) 115.48 (0.61) C1 - N2 N1 C2 - Distance Angles N3 1.3162 (0.0093) N2 1.3717 (0.0090) 124.16 (0.70) C9 1.4972 (0.0101) 119.23 (0.64) 116.56 (0.61) C2 - N3 N2 C3 - Distance Angles N3 1.3309 (0.0091) N1 1.3482 (0.0093) 124.69 (0.67) C14 1.4882 (0.0096) 119.03 (0.65) 116.26 (0.62) C3 - N3 N1 C4 - Distance Angles N4 1.3593 (0.0087) C5 1.3693 (0.0099) 119.07 (0.64) C1 1.4832 (0.0095) 117.11 (0.60) 123.81 (0.64) C4 - N4 C5 C5 - Distance Angles C4 1.3693 (0.0099) C6 1.3964 (0.0105) 120.38 (0.70) H5 0.9500 119.81 119.81 C5 - C4 C6 C6 - Distance Angles C7 1.3893 (0.0112) C5 1.3964 (0.0105) 119.93 (0.68) H6 0.9500 120.04 120.04 C6 - C7 C5 C7 - Distance Angles C8 1.3845 (0.0105) C6 1.3893 (0.0112) 117.34 (0.71) H7 0.9500 121.33 121.33 C7 - C8 C6 C8 - Distance Angles N4 1.3444 (0.0093) C7 1.3845 (0.0105) 122.00 (0.70) H8 0.9500 119.00 119.00 C8 - N4 C7 C9 - Distance Angles C10 1.3366 (0.0105) N5 1.3929 (0.0103) 122.98 (0.67) C2 1.4972 (0.0101) 116.27 (0.63) 120.71 (0.68) C9 - C10 N5 C10 - Distance Angles C9 1.3366 (0.0105) C11 1.3567 (0.0099) 115.72 (0.72) H10 0.9500 122.14 122.14 C10 - C9 C11 C11 - Distance Angles C10 1.3567 (0.0099) C12 1.3760 (0.0118) 123.71 (0.81) H11 0.9500 118.14 118.14 C11 - C10 C12 C12 - Distance Angles C13 1.3458 (0.0120) C11 1.3760 (0.0118) 119.34 (0.75) H12 0.9500 120.33 120.33 C12 - C13 C11 C13 - Distance Angles C12 1.3458 (0.0120) N5 1.3683 (0.0106) 119.04 (0.78) H13 0.9500 120.48 120.48 C13 - C12 N5 C14 - Distance Angles C15 1.3443 (0.0094) N6 1.3794 (0.0099) 122.46 (0.65) C3 1.4882 (0.0096) 116.73 (0.61) 120.80 (0.65) C14 - C15 N6 C15 - Distance Angles C14 1.3443 (0.0094) C16 1.3469 (0.0098) 118.09 (0.64) H15 0.9500 120.96 120.96 C15 - C14 C16 C16 - Distance Angles C15 1.3469 (0.0098) C17 1.3811 (0.0113) 122.27 (0.73) H16 0.9500 118.86 118.86 C16 - C15 C17 C17 - Distance Angles C18 1.3613 (0.0115) C16 1.3811 (0.0113) 119.32 (0.72) H17 0.9500 120.34 120.34 C17 - C18 C16 C18 - Distance Angles C17 1.3613 (0.0115) N6 1.3919 (0.0106) 119.29 (0.74) H18 0.9500 120.35 120.35 C18 - C17 N6 N1 - Distance Angles C1 1.3259 (0.0092) C3 1.3482 (0.0093) 114.13 (0.60) N1 - C1 N2 - Distance Angles C1 1.3121 (0.0093) C2 1.3717 (0.0090) 114.16 (0.64) N2 - C1 N3 - Distance Angles C2 1.3162 (0.0093) C3 1.3309 (0.0091) 115.94 (0.68) N3 - C2 N4 - Distance Angles C8 1.3444 (0.0093) C4 1.3593 (0.0087) 121.20 (0.65) H4 0.8800 119.40 119.40 N4 - C8 C4 N5 - Distance Angles C13 1.3683 (0.0106) C9 1.3929 (0.0103) 119.18 (0.78) H5A 0.8800 120.41 120.41 N5 - C13 C9 N6 - Distance Angles C14 1.3794 (0.0099) C18 1.3919 (0.0106) 118.53 (0.72) H6A 0.8800 120.73 120.73 N6 - C14 C18 Br2 - Distance Angles I1 2.6442 (0.0010) Br2 - Br1 - Distance Angles I1 2.6582 (0.0011) Br1 - I1 - Distance Angles Br2 2.6442 (0.0010) Br1 2.6582 (0.0011) 177.47 (0.03) I1 - Br2 FMAP and GRID set by program FMAP 2 3 19 GRID -1.563 -2 -2 1.563 2 2 R1 = 0.0490 for 2511 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.37 at 0.1377 0.0938 0.0386 [ 0.18 A from I1 ] Deepest hole -1.93 at 0.3158 0.2213 0.0428 [ 0.44 A from BR1 ] Mean = 0.00, Rms deviation from mean = 0.20 e/A^3, Highest memory used = 2690 / 21701 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2867 -0.0785 0.0456 1.00000 0.05 1.05 1.34 N2 1.98 H4 1.98 C1 2.33 N4 Q2 1 0.3666 -0.0832 0.3863 1.00000 0.05 0.95 1.91 H13 2.35 I1 2.36 H17 2.45 H18 Q3 1 -0.0444 -0.0827 -0.0397 1.00000 0.05 0.90 1.21 BR2 2.14 H18 2.42 H17 2.77 C18 Q4 1 0.2396 0.3069 -0.0030 1.00000 0.05 0.77 1.17 BR1 1.83 H12 2.22 H8 2.65 C12 Q5 1 0.2980 0.2580 0.1213 1.00000 0.05 0.74 1.10 BR1 1.86 H6A 2.52 H16 2.52 N6 Shortest distances between peaks (including symmetry equivalents) 4 5 2.04 2 3 2.98 Time profile in seconds ----------------------- 0.03: 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 0.01: Analyse other restraints etc. 1.11: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.01: Set up l.s. refinement 0.01: Generate idealized H-atoms 3.16: Structure factors and derivatives 2.99: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.25: Solve l.s. equations 0.00: Generate HTAB table 0.01: Other dependent quantities, CIF, tables 0.14: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.04: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2005slh0246 finished at 13:33:11 Total CPU time: 7.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++