+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0172 started at 09:21:04 on 27-Feb-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0172 in P2(1)/n CELL 0.71073 13.0885 12.5754 14.4854 90.000 110.753 90.000 ZERR 4.00 0.0002 0.0003 0.0003 0.000 0.001 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H O S SE UNIT 80 104 16 8 8 V = 2229.50 F(000) = 1112.0 Mu = 3.53 mm-1 Cell Wt = 2209.79 Rho = 1.646 MERG 2 OMIT -3.00 55.00 OMIT 1 1 1 SHEL 7 0.77 FMAP 2 PLAN 10 SIZE 0.09 0.23 0.33 ACTA BOND $H WGHT 0.01780 3.12820 L.S. 4 TEMP -153.00 FVAR 0.25168 MOLE 1 C1 1 0.800146 0.174630 0.165277 11.00000 0.02105 0.01453 = 0.01766 0.00276 0.00820 0.00197 C2 1 0.785343 0.102674 0.087224 11.00000 0.02463 0.01450 = 0.02319 0.00273 0.01129 -0.00098 C3 1 0.878491 0.055969 0.078718 11.00000 0.02711 0.01917 = 0.02588 0.00210 0.01309 0.00233 AFIX 43 H3 2 0.870824 0.006873 0.026841 11.00000 -1.20000 AFIX 0 C4 1 0.982048 0.080160 0.144855 11.00000 0.02578 0.02421 = 0.03363 0.00794 0.01407 0.00763 AFIX 43 H4 2 1.044335 0.048096 0.137292 11.00000 -1.20000 AFIX 0 C5 1 0.995395 0.150543 0.221692 11.00000 0.02185 0.02624 = 0.03379 0.00598 0.00413 -0.00204 AFIX 43 H5 2 1.066499 0.166610 0.266755 11.00000 -1.20000 AFIX 0 C6 1 0.904734 0.197375 0.232563 11.00000 0.02706 0.02334 = 0.01955 0.00162 0.00316 -0.00151 AFIX 43 H6 2 0.913422 0.245007 0.285716 11.00000 -1.20000 AFIX 0 C7 1 0.671531 0.367910 0.133063 11.00000 0.02762 0.01600 = 0.02646 0.00039 0.01414 0.00309 C8 1 0.634501 0.355661 0.021780 11.00000 0.04628 0.02271 = 0.02585 0.00687 0.01642 0.00708 AFIX 137 H8A 2 0.568220 0.312005 -0.001529 11.00000 -1.50000 H8B 2 0.692332 0.321141 0.004360 11.00000 -1.50000 H8C 2 0.619041 0.425928 -0.009347 11.00000 -1.50000 AFIX 0 C9 1 0.582168 0.419603 0.163181 11.00000 0.03210 0.03190 = 0.03672 -0.00103 0.01758 0.00731 AFIX 137 H9A 2 0.565943 0.490650 0.133803 11.00000 -1.50000 H9B 2 0.607337 0.425469 0.235262 11.00000 -1.50000 H9C 2 0.516004 0.375788 0.139762 11.00000 -1.50000 AFIX 0 C10 1 0.777859 0.431244 0.174686 11.00000 0.03339 0.01934 = 0.04455 0.00092 0.01823 -0.00358 AFIX 137 H10A 2 0.834021 0.397952 0.154068 11.00000 -1.50000 H10B 2 0.802310 0.432022 0.246934 11.00000 -1.50000 H10C 2 0.765365 0.504334 0.149723 11.00000 -1.50000 AFIX 0 C21 1 0.690353 -0.148449 -0.120075 11.00000 0.01729 0.01307 = 0.02201 -0.00487 0.00573 -0.00311 C22 1 0.697517 -0.218103 -0.193604 11.00000 0.01678 0.01739 = 0.01424 -0.00101 0.00417 -0.00249 C23 1 0.710958 -0.327315 -0.176072 11.00000 0.02060 0.01630 = 0.01794 -0.00130 0.00467 0.00075 AFIX 43 H23 2 0.718265 -0.372907 -0.225660 11.00000 -1.20000 AFIX 0 C24 1 0.713717 -0.369602 -0.087175 11.00000 0.02537 0.01410 = 0.02387 0.00346 0.00811 0.00343 AFIX 43 H24 2 0.723095 -0.443869 -0.075143 11.00000 -1.20000 AFIX 0 C25 1 0.702539 -0.301660 -0.015635 11.00000 0.02835 0.02237 = 0.01674 0.00314 0.00432 0.00078 AFIX 43 H25 2 0.701592 -0.330268 0.044755 11.00000 -1.20000 AFIX 0 C26 1 0.692790 -0.193149 -0.031097 11.00000 0.02478 0.02210 = 0.01794 -0.00034 0.00615 -0.00099 AFIX 43 H26 2 0.687652 -0.148123 0.019740 11.00000 -1.20000 AFIX 0 C27 1 0.548695 -0.184159 -0.393471 11.00000 0.01920 0.01658 = 0.01630 0.00026 0.00474 0.00105 C28 1 0.549012 -0.150500 -0.494907 11.00000 0.03239 0.02366 = 0.01852 0.00232 0.01109 -0.00155 AFIX 137 H28A 2 0.590870 -0.202146 -0.517782 11.00000 -1.50000 H28B 2 0.582631 -0.080088 -0.489943 11.00000 -1.50000 H28C 2 0.473740 -0.147714 -0.541946 11.00000 -1.50000 AFIX 0 C29 1 0.508700 -0.297982 -0.395672 11.00000 0.02466 0.02206 = 0.02537 -0.00138 0.00620 -0.00436 AFIX 137 H29A 2 0.434989 -0.304239 -0.445130 11.00000 -1.50000 H29B 2 0.507157 -0.316954 -0.330561 11.00000 -1.50000 H29C 2 0.558178 -0.346114 -0.412746 11.00000 -1.50000 AFIX 0 C30 1 0.482163 -0.106691 -0.355707 11.00000 0.02057 0.02847 = 0.02085 0.00140 0.00773 0.00357 AFIX 137 H30A 2 0.406398 -0.105392 -0.401820 11.00000 -1.50000 H30B 2 0.513653 -0.035266 -0.350550 11.00000 -1.50000 H30C 2 0.483854 -0.129830 -0.290578 11.00000 -1.50000 AFIX 0 O1 3 0.593234 0.174326 0.142106 11.00000 0.02493 0.02503 = 0.02757 -0.00368 0.01372 -0.00576 O2 3 0.725662 0.252433 0.295008 11.00000 0.04098 0.03397 = 0.01768 0.00051 0.01435 -0.00018 O21 3 0.751415 -0.252248 -0.348401 11.00000 0.02511 0.01860 = 0.02583 -0.00206 0.01420 0.00244 O22 3 0.725843 -0.066537 -0.304545 11.00000 0.02644 0.01597 = 0.02559 -0.00125 0.01214 -0.00394 S3 4 0.691212 -0.176547 -0.312432 11.00000 0.01962 0.01389 = 0.01813 -0.00035 0.00882 -0.00102 S4 4 0.690403 0.236615 0.189425 11.00000 0.02416 0.01933 = 0.01687 -0.00044 0.01042 -0.00086 SE1 5 0.640709 0.066007 -0.005423 11.00000 0.02201 0.01928 = 0.02224 -0.00493 0.00786 -0.00088 SE2 5 0.682595 0.005044 -0.139312 11.00000 0.03303 0.01378 = 0.02012 -0.00208 0.01059 -0.00086 HKLF 4 Covalent radii and connectivity table for 2009src0172 in P2(1)/n C 0.770 H 0.320 O 0.660 S 1.030 SE 1.170 C1 - C6 C2 S4 C2 - C3 C1 Se1 C3 - C4 C2 C4 - C5 C3 C5 - C6 C4 C6 - C5 C1 C7 - C8 C10 C9 S4 C8 - C7 C9 - C7 C10 - C7 C21 - C26 C22 Se2 C22 - C23 C21 S3 C23 - C24 C22 C24 - C23 C25 C25 - C26 C24 C26 - C25 C21 C27 - C29 C28 C30 S3 C28 - C27 C29 - C27 C30 - C27 O1 - S4 O2 - S4 O21 - S3 O22 - S3 S3 - O21 O22 C22 C27 S4 - O1 O2 C1 C7 Se1 - C2 Se2 Se2 - C21 Se1 36130 Reflections read, of which 951 rejected -16 =< h =< 16, -16 =< k =< 16, -18 =< l =< 18, Max. 2-theta = 54.96 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 11 1 0 -0.02 0.16 9 1.23 1 Inconsistent equivalents 5099 Unique reflections, of which 0 suppressed R(int) = 0.0752 R(sigma) = 0.0518 Friedel opposites merged Maximum memory for data reduction = 2682 / 50725 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 = 3430 / 322903 wR2 = 0.0759 before cycle 1 for 5099 data and 259 / 259 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0178 * P )^2 + 3.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.25152 0.00026 -0.596 OSF Mean shift/su = 0.034 Maximum = -0.596 for OSF Max. shift = 0.001 A for H28A Max. dU = 0.000 for C6 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3430 / 322903 wR2 = 0.0758 before cycle 2 for 5099 data and 259 / 259 parameters GooF = S = 1.045; Restrained GooF = 1.045 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0178 * P )^2 + 3.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.25148 0.00026 -0.162 OSF Mean shift/su = 0.011 Maximum = -0.162 for OSF Max. shift = 0.001 A for H28A Max. dU = 0.000 for C6 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3430 / 322903 wR2 = 0.0758 before cycle 3 for 5099 data and 259 / 259 parameters GooF = S = 1.045; Restrained GooF = 1.045 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0178 * P )^2 + 3.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.25148 0.00026 0.002 OSF Mean shift/su = 0.000 Maximum = 0.002 for OSF Max. shift = 0.000 A for H28C Max. dU = 0.000 for C22 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3430 / 322903 wR2 = 0.0758 before cycle 4 for 5099 data and 259 / 259 parameters GooF = S = 1.045; Restrained GooF = 1.045 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0178 * P )^2 + 3.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.25148 0.00026 0.001 OSF Mean shift/su = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H8A Max. dU = 0.000 for C26 Largest correlation matrix elements 0.500 U13 C9 / U33 C9 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 0.8708 0.0069 0.0268 43 0.950 0.000 C3 C4 C2 H4 1.0443 0.0481 0.1373 43 0.950 0.000 C4 C5 C3 H5 1.0665 0.1666 0.2668 43 0.950 0.000 C5 C6 C4 H6 0.9134 0.2450 0.2857 43 0.950 0.000 C6 C5 C1 H8A 0.5682 0.3120 -0.0015 137 0.980 0.000 C8 C7 H8A H8B 0.6923 0.3212 0.0043 137 0.980 0.000 C8 C7 H8A H8C 0.6189 0.4259 -0.0093 137 0.980 0.000 C8 C7 H8A H9A 0.5659 0.4906 0.1338 137 0.980 0.000 C9 C7 H9A H9B 0.6074 0.4255 0.2353 137 0.980 0.000 C9 C7 H9A H9C 0.5160 0.3758 0.1398 137 0.980 0.000 C9 C7 H9A H10A 0.8340 0.3979 0.1541 137 0.980 0.000 C10 C7 H10A H10B 0.8023 0.4321 0.2469 137 0.980 0.000 C10 C7 H10A H10C 0.7654 0.5043 0.1497 137 0.980 0.000 C10 C7 H10A H23 0.7183 -0.3729 -0.2257 43 0.950 0.000 C23 C24 C22 H24 0.7231 -0.4439 -0.0752 43 0.950 0.000 C24 C23 C25 H25 0.7016 -0.3303 0.0447 43 0.950 0.000 C25 C26 C24 H26 0.6876 -0.1481 0.0197 43 0.950 0.000 C26 C25 C21 H28A 0.5907 -0.2022 -0.5179 137 0.980 0.000 C28 C27 H28A H28B 0.5828 -0.0801 -0.4899 137 0.980 0.000 C28 C27 H28A H28C 0.4737 -0.1476 -0.5419 137 0.980 0.000 C28 C27 H28A H29A 0.4349 -0.3042 -0.4451 137 0.980 0.000 C29 C27 H29A H29B 0.5072 -0.3170 -0.3305 137 0.980 0.000 C29 C27 H29A H29C 0.5581 -0.3461 -0.4128 137 0.980 0.000 C29 C27 H29A H30A 0.4064 -0.1054 -0.4018 137 0.980 0.000 C30 C27 H30A H30B 0.5137 -0.0353 -0.3505 137 0.980 0.000 C30 C27 H30A H30C 0.4838 -0.1299 -0.2906 137 0.980 0.000 C30 C27 H30A 2009src0172 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.80015 0.17462 0.16528 1.00000 0.02104 0.01442 0.01763 0.00276 0.00819 0.00198 0.01733 0.00601 0.00024 0.00024 0.00022 0.00000 0.00149 0.00152 0.00154 0.00122 0.00123 0.00122 0.00062 C2 0.78535 0.10268 0.08722 1.00000 0.02454 0.01439 0.02317 0.00273 0.01124 -0.00092 0.01995 0.00628 0.00025 0.00024 0.00023 0.00000 0.00161 0.00158 0.00168 0.00127 0.00132 0.00124 0.00066 C3 0.87848 0.05597 0.07872 1.00000 0.02706 0.01908 0.02582 0.00212 0.01303 0.00239 0.02300 0.00664 0.00025 0.00025 0.00024 0.00000 0.00168 0.00170 0.00175 0.00137 0.00139 0.00134 0.00069 H3 0.87082 0.00688 0.02684 1.00000 0.02760 0.00000 0.00000 C4 0.98203 0.08016 0.14486 1.00000 0.02571 0.02405 0.03358 0.00789 0.01407 0.00766 0.02682 0.00703 0.00027 0.00026 0.00025 0.00000 0.00173 0.00184 0.00195 0.00153 0.00148 0.00140 0.00075 H4 1.04431 0.04809 0.13730 1.00000 0.03218 0.00000 0.00000 C5 0.99540 0.15055 0.22170 1.00000 0.02176 0.02619 0.03375 0.00603 0.00412 -0.00207 0.02878 0.00693 0.00026 0.00027 0.00026 0.00000 0.00167 0.00190 0.00198 0.00156 0.00144 0.00140 0.00078 H5 1.06650 0.16662 0.26676 1.00000 0.03453 0.00000 0.00000 C6 0.90474 0.19736 0.23256 1.00000 0.02698 0.02326 0.01944 0.00161 0.00318 -0.00147 0.02459 0.00643 0.00025 0.00026 0.00023 0.00000 0.00170 0.00177 0.00166 0.00138 0.00134 0.00139 0.00071 H6 0.91342 0.24500 0.28571 1.00000 0.02951 0.00000 0.00000 C7 0.67154 0.36791 0.13307 1.00000 0.02754 0.01590 0.02638 0.00041 0.01409 0.00307 0.02205 0.00650 0.00025 0.00025 0.00024 0.00000 0.00171 0.00163 0.00173 0.00134 0.00139 0.00131 0.00068 C8 0.63448 0.35567 0.02177 1.00000 0.04625 0.02275 0.02584 0.00685 0.01646 0.00715 0.03062 0.00733 0.00030 0.00028 0.00024 0.00000 0.00214 0.00183 0.00184 0.00147 0.00162 0.00157 0.00080 H8A 0.56824 0.31196 -0.00152 1.00000 0.04593 0.00000 0.00000 H8B 0.69233 0.32122 0.00433 1.00000 0.04593 0.00000 0.00000 H8C 0.61894 0.42594 -0.00935 1.00000 0.04593 0.00000 0.00000 C9 0.58217 0.41960 0.16318 1.00000 0.03210 0.03185 0.03666 -0.00102 0.01762 0.00734 0.03207 0.00750 0.00028 0.00029 0.00027 0.00000 0.00192 0.00204 0.00209 0.00165 0.00163 0.00156 0.00082 H9A 0.56591 0.49063 0.13376 1.00000 0.04810 0.00000 0.00000 H9B 0.60736 0.42552 0.23526 1.00000 0.04810 0.00000 0.00000 H9C 0.51603 0.37576 0.13980 1.00000 0.04810 0.00000 0.00000 C10 0.77785 0.43125 0.17469 1.00000 0.03327 0.01928 0.04458 0.00096 0.01817 -0.00356 0.03119 0.00702 0.00027 0.00027 0.00028 0.00000 0.00190 0.00177 0.00222 0.00161 0.00166 0.00147 0.00080 H10A 0.83405 0.39791 0.15414 1.00000 0.04679 0.00000 0.00000 H10B 0.80225 0.43210 0.24694 1.00000 0.04679 0.00000 0.00000 H10C 0.76538 0.50432 0.14967 1.00000 0.04679 0.00000 0.00000 C21 0.69035 -0.14846 -0.12007 1.00000 0.01720 0.01302 0.02193 -0.00483 0.00568 -0.00309 0.01772 0.00570 0.00023 0.00024 0.00022 0.00000 0.00147 0.00153 0.00164 0.00124 0.00125 0.00117 0.00064 C22 0.69753 -0.21812 -0.19361 1.00000 0.01670 0.01727 0.01417 -0.00107 0.00414 -0.00248 0.01640 0.00567 0.00023 0.00024 0.00021 0.00000 0.00144 0.00157 0.00148 0.00120 0.00117 0.00118 0.00062 C23 0.71096 -0.32732 -0.17608 1.00000 0.02045 0.01633 0.01786 -0.00131 0.00460 0.00074 0.01881 0.00592 0.00023 0.00024 0.00022 0.00000 0.00151 0.00157 0.00158 0.00125 0.00123 0.00123 0.00064 H23 0.71827 -0.37291 -0.22566 1.00000 0.02257 0.00000 0.00000 C24 0.71370 -0.36960 -0.08718 1.00000 0.02533 0.01404 0.02381 0.00343 0.00810 0.00343 0.02123 0.00626 0.00024 0.00025 0.00023 0.00000 0.00164 0.00159 0.00170 0.00132 0.00135 0.00128 0.00067 H24 0.72307 -0.44386 -0.07516 1.00000 0.02547 0.00000 0.00000 C25 0.70252 -0.30167 -0.01564 1.00000 0.02824 0.02224 0.01673 0.00313 0.00428 0.00074 0.02340 0.00629 0.00025 0.00026 0.00023 0.00000 0.00170 0.00175 0.00159 0.00135 0.00132 0.00137 0.00070 H25 0.70157 -0.33029 0.04474 1.00000 0.02808 0.00000 0.00000 C26 0.69278 -0.19313 -0.03111 1.00000 0.02472 0.02206 0.01783 -0.00036 0.00616 -0.00099 0.02191 0.00621 0.00024 0.00026 0.00023 0.00000 0.00164 0.00174 0.00162 0.00131 0.00130 0.00132 0.00068 H26 0.68763 -0.14810 0.01973 1.00000 0.02630 0.00000 0.00000 C27 0.54872 -0.18415 -0.39346 1.00000 0.01915 0.01655 0.01620 0.00025 0.00474 0.00103 0.01771 0.00589 0.00023 0.00024 0.00021 0.00000 0.00148 0.00159 0.00154 0.00123 0.00120 0.00121 0.00063 C28 0.54901 -0.15050 -0.49492 1.00000 0.03232 0.02366 0.01845 0.00233 0.01108 -0.00154 0.02425 0.00655 0.00027 0.00026 0.00022 0.00000 0.00180 0.00178 0.00163 0.00136 0.00139 0.00141 0.00071 H28A 0.59074 -0.20222 -0.51785 1.00000 0.03637 0.00000 0.00000 H28B 0.58275 -0.08015 -0.48994 1.00000 0.03637 0.00000 0.00000 H28C 0.47372 -0.14759 -0.54191 1.00000 0.03637 0.00000 0.00000 C29 0.50868 -0.29800 -0.39568 1.00000 0.02464 0.02199 0.02536 -0.00132 0.00621 -0.00431 0.02471 0.00626 0.00026 0.00026 0.00024 0.00000 0.00167 0.00175 0.00177 0.00139 0.00138 0.00136 0.00072 H29A 0.43494 -0.30422 -0.44508 1.00000 0.03707 0.00000 0.00000 H29B 0.50721 -0.31700 -0.33055 1.00000 0.03707 0.00000 0.00000 H29C 0.55810 -0.34613 -0.41283 1.00000 0.03707 0.00000 0.00000 C30 0.48215 -0.10670 -0.35569 1.00000 0.02053 0.02840 0.02081 0.00142 0.00771 0.00358 0.02314 0.00651 0.00025 0.00026 0.00023 0.00000 0.00159 0.00186 0.00167 0.00139 0.00130 0.00136 0.00070 H30A 0.40640 -0.10536 -0.40184 1.00000 0.03472 0.00000 0.00000 H30B 0.51367 -0.03528 -0.35047 1.00000 0.03472 0.00000 0.00000 H30C 0.48378 -0.12989 -0.29059 1.00000 0.03472 0.00000 0.00000 O1 0.59323 0.17432 0.14210 1.00000 0.02476 0.02499 0.02753 -0.00369 0.01366 -0.00578 0.02457 0.00426 0.00017 0.00018 0.00016 0.00000 0.00116 0.00124 0.00127 0.00100 0.00098 0.00097 0.00050 O2 0.72566 0.25244 0.29501 1.00000 0.04097 0.03387 0.01753 0.00045 0.01431 -0.00024 0.02973 0.00465 0.00019 0.00019 0.00016 0.00000 0.00140 0.00140 0.00118 0.00102 0.00103 0.00111 0.00055 O21 0.75141 -0.25227 -0.34840 1.00000 0.02499 0.01851 0.02579 -0.00204 0.01420 0.00248 0.02169 0.00429 0.00017 0.00017 0.00016 0.00000 0.00113 0.00116 0.00120 0.00095 0.00094 0.00091 0.00047 O22 0.72584 -0.06653 -0.30454 1.00000 0.02639 0.01585 0.02557 -0.00126 0.01214 -0.00401 0.02181 0.00419 0.00017 0.00017 0.00016 0.00000 0.00115 0.00111 0.00119 0.00094 0.00095 0.00091 0.00047 S3 0.69121 -0.17655 -0.31243 1.00000 0.01958 0.01383 0.01809 -0.00035 0.00882 -0.00101 0.01659 0.00148 0.00006 0.00006 0.00005 0.00000 0.00037 0.00037 0.00038 0.00029 0.00030 0.00029 0.00016 S4 0.69040 0.23662 0.18942 1.00000 0.02411 0.01928 0.01682 -0.00044 0.01040 -0.00085 0.01922 0.00154 0.00006 0.00006 0.00005 0.00000 0.00039 0.00040 0.00038 0.00031 0.00031 0.00031 0.00017 Se1 0.64071 0.06601 -0.00542 1.00000 0.02196 0.01922 0.02218 -0.00493 0.00784 -0.00088 0.02112 0.00062 0.00002 0.00003 0.00002 0.00000 0.00016 0.00017 0.00017 0.00013 0.00013 0.00013 0.00009 Se2 0.68259 0.00504 -0.13931 1.00000 0.03297 0.01372 0.02007 -0.00208 0.01058 -0.00086 0.02194 0.00063 0.00003 0.00002 0.00002 0.00000 0.00019 0.00016 0.00017 0.00013 0.00014 0.00013 0.00009 Final Structure Factor Calculation for 2009src0172 in P2(1)/n Total number of l.s. parameters = 259 Maximum vector length = 511 Memory required = 3171 / 24017 wR2 = 0.0758 before cycle 5 for 5099 data and 0 / 259 parameters GooF = S = 1.045; Restrained GooF = 1.045 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0178 * P )^2 + 3.13 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0366 for 3980 Fo > 4sig(Fo) and 0.0565 for all 5099 data wR2 = 0.0758, GooF = S = 1.045, Restrained GooF = 1.045 for all data Occupancy sum of asymmetric unit = 28.00 for non-hydrogen and 26.00 for hydrogen atoms Principal mean square atomic displacements U 0.0219 0.0172 0.0128 C1 0.0261 0.0211 0.0127 C2 0.0299 0.0207 0.0184 C3 0.0393 0.0240 0.0171 C4 0.0426 0.0229 0.0208 C5 0.0330 0.0228 0.0180 C6 0.0307 0.0208 0.0147 C7 0.0483 0.0263 0.0172 C8 0.0403 0.0359 0.0200 C9 0.0450 0.0309 0.0177 C10 0.0244 0.0185 0.0103 C21 0.0198 0.0162 0.0132 C22 0.0233 0.0175 0.0156 C23 0.0263 0.0248 0.0125 C24 0.0315 0.0235 0.0152 C25 0.0261 0.0219 0.0178 C26 0.0208 0.0167 0.0156 C27 0.0326 0.0245 0.0156 C28 0.0301 0.0255 0.0186 C29 0.0298 0.0206 0.0190 C30 0.0334 0.0227 0.0177 O1 0.0410 0.0339 0.0143 O2 0.0292 0.0219 0.0139 O21 0.0291 0.0220 0.0143 O22 0.0207 0.0155 0.0136 S3 0.0246 0.0191 0.0139 S4 0.0259 0.0219 0.0155 Se1 0.0331 0.0197 0.0130 Se2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.013 0.024 0.038 0.050 0.065 0.082 0.103 0.133 0.177 1.000 Number in group 538. 494. 551. 459. 523. 503. 504. 509. 504. 514. GooF 0.878 1.012 1.053 1.044 1.113 1.142 1.038 1.088 0.954 1.109 K 1.927 1.127 0.974 0.967 0.970 0.980 0.986 1.001 1.009 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 522. 515. 503. 498. 523. 507. 500. 512. 508. 511. GooF 0.992 0.976 1.039 0.965 0.974 0.984 0.983 0.956 1.013 1.467 K 0.954 0.993 0.971 0.991 1.006 1.013 1.023 1.021 1.012 0.974 R1 0.154 0.123 0.104 0.071 0.061 0.044 0.036 0.029 0.024 0.027 Recommended weighting scheme: WGHT 0.0166 3.1889 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) -7 1 17 1346.27 2111.46 4.46 0.115 0.85 -4 2 2 1152.69 1468.88 3.97 0.096 2.89 -6 1 4 138.55 52.06 3.93 0.018 2.08 4 12 7 167.41 462.24 3.91 0.054 0.84 0 6 5 283.48 107.98 3.90 0.026 1.66 -2 1 1 22800.45 38227.57 3.89 0.490 5.78 -2 0 8 737.85 494.63 3.80 0.056 1.80 2 1 0 156.68 75.03 3.79 0.022 5.50 4 2 1 134.30 56.09 3.64 0.019 2.54 0 0 2 369.10 582.40 3.64 0.061 6.77 -8 12 4 1219.38 1745.62 3.57 0.105 0.88 -1 1 7 1073.76 811.06 3.40 0.071 2.00 -3 0 1 31490.52 34711.89 3.38 0.467 4.36 3 2 1 6478.41 7270.64 3.33 0.214 3.11 -3 5 1 574.40 413.39 3.32 0.051 2.18 1 5 3 1539.33 1267.44 3.30 0.089 2.10 -9 3 17 581.61 934.11 3.27 0.077 0.81 13 8 1 551.46 180.38 3.27 0.034 0.79 5 1 0 6299.88 6998.90 3.21 0.210 2.40 1 6 3 2195.31 2588.36 3.20 0.128 1.84 -4 2 13 18.50 130.53 3.19 0.029 1.10 -16 3 10 172.87 396.21 3.19 0.050 0.78 1 12 0 480.61 279.97 3.13 0.042 1.04 -9 0 17 1019.39 1702.25 3.13 0.104 0.83 -3 12 11 908.18 453.56 3.12 0.053 0.82 -4 3 1 879.99 700.39 3.12 0.066 2.56 9 11 1 687.77 976.43 3.07 0.078 0.86 -12 2 16 367.53 680.60 3.06 0.065 0.80 -1 5 5 944.78 1173.95 3.05 0.086 1.89 0 1 2 4620.53 5184.09 3.04 0.181 5.96 0 0 12 1163.21 852.67 3.04 0.073 1.13 4 2 2 22629.44 24534.72 3.02 0.393 2.31 0 2 6 1682.08 1997.95 3.01 0.112 2.12 0 5 5 2804.15 3209.54 3.01 0.142 1.84 -3 3 5 256.55 388.06 2.99 0.049 2.30 7 12 2 2521.13 1976.25 2.98 0.112 0.87 -10 1 10 71.39 0.59 2.98 0.002 1.12 -2 5 2 170.79 70.74 2.98 0.021 2.30 6 13 1 1936.77 2452.48 2.98 0.124 0.86 2 0 0 68392.88 83356.70 2.97 0.724 6.12 -7 6 7 5737.12 5109.28 2.96 0.179 1.28 3 2 14 414.41 676.28 2.95 0.065 0.87 -6 4 6 1829.30 2124.33 2.94 0.116 1.61 -8 3 6 571.31 750.31 2.93 0.069 1.45 -11 10 4 831.92 1203.99 2.93 0.087 0.86 0 2 0 838.33 655.06 2.93 0.064 6.29 -11 4 5 420.08 273.93 2.92 0.042 1.11 -5 3 11 274.01 133.70 2.89 0.029 1.24 -3 7 1 1006.51 780.56 2.87 0.070 1.66 0 3 6 5064.08 4509.52 2.84 0.168 1.99 Bond lengths and angles C1 - Distance Angles C6 1.4000 (0.0042) C2 1.4070 (0.0042) 120.86 (0.28) S4 1.7746 (0.0030) 115.67 (0.23) 123.39 (0.23) C1 - C6 C2 C2 - Distance Angles C3 1.3973 (0.0043) C1 1.4070 (0.0042) 117.72 (0.28) Se1 1.9486 (0.0031) 120.32 (0.24) 121.95 (0.22) C2 - C3 C1 C3 - Distance Angles C4 1.3882 (0.0045) C2 1.3973 (0.0043) 121.06 (0.31) H3 0.9500 119.47 119.47 C3 - C4 C2 C4 - Distance Angles C5 1.3839 (0.0049) C3 1.3882 (0.0045) 120.63 (0.30) H4 0.9500 119.68 119.68 C4 - C5 C3 C5 - Distance Angles C6 1.3826 (0.0046) C4 1.3839 (0.0049) 119.66 (0.30) H5 0.9500 120.17 120.17 C5 - C6 C4 C6 - Distance Angles C5 1.3826 (0.0046) C1 1.4000 (0.0041) 120.05 (0.31) H6 0.9500 119.97 119.97 C6 - C5 C1 C7 - Distance Angles C8 1.5178 (0.0044) C10 1.5296 (0.0044) 112.04 (0.28) C9 1.5306 (0.0043) 110.91 (0.28) 110.29 (0.28) S4 1.8195 (0.0032) 109.03 (0.22) 109.62 (0.23) 104.68 (0.22) C7 - C8 C10 C9 C8 - Distance Angles C7 1.5178 (0.0044) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - C7 H8A H8B C9 - Distance Angles C7 1.5306 (0.0043) H9A 0.9800 109.47 H9B 0.9800 109.47 109.47 H9C 0.9800 109.47 109.47 109.47 C9 - C7 H9A H9B C10 - Distance Angles C7 1.5296 (0.0044) H10A 0.9800 109.47 H10B 0.9800 109.47 109.47 H10C 0.9800 109.47 109.47 109.47 C10 - C7 H10A H10B C21 - Distance Angles C26 1.3958 (0.0043) C22 1.4078 (0.0041) 117.54 (0.28) Se2 1.9478 (0.0030) 120.93 (0.23) 121.50 (0.22) C21 - C26 C22 C22 - Distance Angles C23 1.3962 (0.0042) C21 1.4078 (0.0041) 120.81 (0.27) S3 1.7725 (0.0029) 115.23 (0.22) 123.96 (0.23) C22 - C23 C21 C23 - Distance Angles C24 1.3818 (0.0043) C22 1.3962 (0.0042) 120.53 (0.29) H23 0.9500 119.74 119.74 C23 - C24 C22 C24 - Distance Angles C23 1.3818 (0.0043) C25 1.3901 (0.0044) 118.91 (0.29) H24 0.9500 120.55 120.55 C24 - C23 C25 C25 - Distance Angles C26 1.3818 (0.0044) C24 1.3901 (0.0044) 120.95 (0.30) H25 0.9500 119.53 119.53 C25 - C26 C24 C26 - Distance Angles C25 1.3818 (0.0044) C21 1.3958 (0.0043) 121.19 (0.30) H26 0.9500 119.41 119.41 C26 - C25 C21 C27 - Distance Angles C29 1.5209 (0.0042) C28 1.5307 (0.0041) 110.98 (0.25) C30 1.5313 (0.0042) 111.77 (0.26) 111.25 (0.25) S3 1.8204 (0.0030) 109.25 (0.21) 104.71 (0.20) 108.59 (0.21) C27 - C29 C28 C30 C28 - Distance Angles C27 1.5307 (0.0041) H28A 0.9800 109.47 H28B 0.9800 109.47 109.47 H28C 0.9800 109.47 109.47 109.47 C28 - C27 H28A H28B C29 - Distance Angles C27 1.5209 (0.0042) H29A 0.9800 109.47 H29B 0.9800 109.47 109.47 H29C 0.9800 109.47 109.47 109.47 C29 - C27 H29A H29B C30 - Distance Angles C27 1.5313 (0.0042) H30A 0.9800 109.47 H30B 0.9800 109.47 109.47 H30C 0.9800 109.47 109.47 109.47 C30 - C27 H30A H30B O1 - Distance Angles S4 1.4434 (0.0022) O1 - O2 - Distance Angles S4 1.4463 (0.0022) O2 - O21 - Distance Angles S3 1.4456 (0.0021) O21 - O22 - Distance Angles S3 1.4477 (0.0022) O22 - S3 - Distance Angles O21 1.4456 (0.0021) O22 1.4477 (0.0022) 117.55 (0.13) C22 1.7725 (0.0029) 108.17 (0.13) 107.43 (0.13) C27 1.8204 (0.0030) 107.32 (0.13) 108.77 (0.13) 107.17 (0.13) S3 - O21 O22 C22 S4 - Distance Angles O1 1.4434 (0.0022) O2 1.4463 (0.0022) 118.30 (0.13) C1 1.7746 (0.0030) 107.85 (0.14) 106.96 (0.14) C7 1.8195 (0.0032) 108.83 (0.14) 106.94 (0.15) 107.51 (0.14) S4 - O1 O2 C1 Se1 - Distance Angles C2 1.9486 (0.0031) Se2 2.3245 (0.0004) 101.18 (0.09) Se1 - C2 Se2 - Distance Angles C21 1.9478 (0.0030) Se1 2.3245 (0.0004) 102.90 (0.09) Se2 - C21 FMAP and GRID set by program FMAP 2 3 21 GRID -1.389 -2 -2 1.389 2 2 R1 = 0.0543 for 5099 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.45 at 0.3187 0.8729 0.1390 [ 1.54 A from SE2 ] Deepest hole -0.65 at 0.3004 0.0250 0.0857 [ 0.82 A from SE2 ] Mean = 0.00, Rms deviation from mean = 0.11 e/A^3, Highest memory used = 3258 / 26859 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.6813 0.1271 -0.1390 1.00000 0.05 0.45 1.54 SE2 1.80 O21 2.31 SE1 2.72 H23 Q2 1 0.9159 0.2623 0.3654 1.00000 0.05 0.44 1.16 H6 2.05 C6 2.34 O2 2.42 H8A Q3 1 0.5541 0.0669 -0.0837 1.00000 0.05 0.43 1.29 SE1 2.25 SE2 3.18 H6 3.19 C2 Q4 1 0.6424 -0.0614 -0.0060 1.00000 0.05 0.38 1.23 H26 1.60 SE1 1.87 C26 2.25 C21 Q5 1 0.6808 -0.3278 -0.0662 1.00000 0.05 0.38 0.76 C25 0.80 C24 1.53 H25 1.58 H24 Q6 1 0.5791 -0.1384 -0.5775 1.00000 0.05 0.37 1.15 H28A 1.39 C28 1.45 H28B 1.64 H28C Q7 1 0.9472 0.4082 0.2638 1.00000 0.05 0.37 1.75 H10A 1.85 H10B 2.15 H6 2.15 C10 Q8 1 1.0759 -0.0281 0.1011 1.00000 0.05 0.36 1.23 H4 1.60 H29C 2.08 C4 2.22 H3 Q9 1 0.9820 0.1158 0.1812 1.00000 0.05 0.36 0.69 C4 0.70 C5 1.47 H4 1.48 H5 Q10 1 0.9375 0.3091 0.3377 1.00000 0.05 0.36 1.07 H6 2.00 C6 2.37 H10B 2.71 O2 Shortest distances between peaks (including symmetry equivalents) 2 10 0.82 7 10 1.68 3 4 2.07 3 7 2.18 3 10 2.20 1 3 2.22 2 7 2.47 6 7 2.66 8 9 2.67 2 3 2.73 1 7 2.92 8 8 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 0.00: Analyse other restraints etc. 1.64: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.44: Structure factors and derivatives 2.30: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.22: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.09: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.06: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0172 finished at 09:21:10 Total CPU time: 5.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++