+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008src0864 started at 16:18:55 on 25-Jul-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src0864 in P2(1)/c CELL 0.71073 8.9260 15.4665 17.7890 90.000 99.900 90.000 ZERR 4.00 0.0008 0.0007 0.0015 0.000 0.003 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O S UNIT 108 112 16 12 4 V = 2419.27 F(000) = 1032.0 Mu = 0.17 mm-1 Cell Wt = 1954.38 Rho = 1.341 MERG 2 OMIT -3.00 55.00 FMAP 2 PLAN 20 SIZE 0.05 0.12 0.34 ACTA BOND $H WGHT 0.06640 1.34090 L.S. 4 TEMP -153.00 FVAR 0.51962 C1 1 0.084975 0.380352 0.161571 11.00000 0.02449 0.01828 = 0.02031 0.00081 0.00174 -0.00255 C2 1 -0.084930 0.369267 0.163346 11.00000 0.02461 0.01649 = 0.01991 0.00106 0.00524 -0.00125 C3 1 -0.161669 0.453314 0.129154 11.00000 0.02597 0.01641 = 0.02613 0.00206 -0.00005 -0.00059 AFIX 13 H3 2 -0.219598 0.444885 0.076339 11.00000 -1.20000 AFIX 0 C4 1 0.345751 0.336935 0.172276 11.00000 0.02539 0.02119 = 0.03753 -0.00371 0.00336 -0.00116 AFIX 23 H4A 2 0.410603 0.289274 0.196644 11.00000 -1.20000 H4B 2 0.374839 0.390232 0.202046 11.00000 -1.20000 AFIX 0 C5 1 0.375518 0.349625 0.091392 11.00000 0.03273 0.03530 = 0.04671 0.00384 0.01294 0.00017 AFIX 33 H5A 2 0.483244 0.363117 0.092821 11.00000 -1.50000 H5B 2 0.312957 0.397417 0.067232 11.00000 -1.50000 H5C 2 0.349542 0.296520 0.061979 11.00000 -1.50000 AFIX 0 C6 1 0.154334 0.228089 0.199975 11.00000 0.02720 0.01751 = 0.02273 0.00465 0.00498 0.00132 AFIX 23 H6A 2 0.045884 0.223814 0.205101 11.00000 -1.20000 H6B 2 0.216267 0.217351 0.250846 11.00000 -1.20000 AFIX 0 C7 1 0.189604 0.158758 0.144813 11.00000 0.03676 0.01823 = 0.02884 0.00283 0.00643 0.00499 AFIX 33 H7A 2 0.167282 0.101634 0.164016 11.00000 -1.50000 H7B 2 0.297365 0.161820 0.140304 11.00000 -1.50000 H7C 2 0.126868 0.168194 0.094613 11.00000 -1.50000 AFIX 0 C8 1 -0.159535 0.290967 0.119231 11.00000 0.02245 0.01443 = 0.02108 0.00221 0.00109 -0.00180 C9 1 -0.124606 0.270336 0.048237 11.00000 0.02519 0.02144 = 0.02538 0.00548 0.00466 -0.00232 AFIX 43 H9 2 -0.050706 0.303395 0.028316 11.00000 -1.20000 AFIX 0 C10 1 -0.196428 0.201986 0.006079 11.00000 0.02886 0.02440 = 0.01766 0.00114 0.00215 0.00146 AFIX 43 H10 2 -0.169417 0.187388 -0.041717 11.00000 -1.20000 AFIX 0 C11 1 -0.307131 0.155202 0.033593 11.00000 0.02256 0.01534 = 0.02391 0.00209 -0.00145 0.00057 C12 1 -0.342932 0.175075 0.103980 11.00000 0.02989 0.01843 = 0.02301 0.00168 0.00538 -0.00303 AFIX 43 H12 2 -0.418699 0.142823 0.123193 11.00000 -1.20000 AFIX 0 C13 1 -0.268269 0.242192 0.146741 11.00000 0.02620 0.02058 = 0.02262 0.00012 0.00698 0.00013 AFIX 43 H13 2 -0.292163 0.254819 0.195591 11.00000 -1.20000 AFIX 0 C14 1 -0.349090 0.061857 -0.075864 11.00000 0.06458 0.03957 = 0.03130 -0.01393 0.01066 -0.01237 AFIX 33 H14A 2 -0.414858 0.013830 -0.096850 11.00000 -1.50000 H14B 2 -0.242643 0.043141 -0.067948 11.00000 -1.50000 H14C 2 -0.363188 0.110540 -0.111645 11.00000 -1.50000 AFIX 0 C15 1 -0.002373 0.365662 0.309255 11.00000 0.02730 0.01900 = 0.01794 -0.00175 0.00545 0.00030 C16 1 0.022310 0.286923 0.346594 11.00000 0.02501 0.02017 = 0.02433 -0.00158 0.01090 -0.00101 AFIX 43 H16 2 -0.039711 0.238460 0.329553 11.00000 -1.20000 AFIX 0 C17 1 0.138849 0.279482 0.409322 11.00000 0.02799 0.02468 = 0.02541 0.00413 0.00653 0.00567 AFIX 43 H17 2 0.156428 0.225588 0.434940 11.00000 -1.20000 AFIX 0 C18 1 0.228455 0.349323 0.434418 11.00000 0.03005 0.03955 = 0.02796 0.00089 0.00012 0.00107 AFIX 43 H18 2 0.308950 0.343292 0.476595 11.00000 -1.20000 AFIX 0 C19 1 0.201686 0.428838 0.398267 11.00000 0.04368 0.02420 = 0.03044 -0.00396 0.00109 -0.01174 AFIX 43 H19 2 0.262475 0.477467 0.416218 11.00000 -1.20000 AFIX 0 C20 1 0.086148 0.436858 0.336036 11.00000 0.03322 0.02256 = 0.02951 0.00017 0.00249 -0.00045 AFIX 43 H20 2 0.067139 0.491262 0.311455 11.00000 -1.20000 AFIX 0 C21 1 -0.262852 0.476983 0.185213 11.00000 0.02405 0.01590 = 0.03064 0.00090 0.00423 0.00033 C22 1 -0.384990 0.541427 0.170955 11.00000 0.02261 0.01732 = 0.03617 0.00342 0.00001 0.00053 C23 1 -0.486935 0.550987 0.221520 11.00000 0.03096 0.02085 = 0.02914 -0.00646 0.00261 -0.00106 AFIX 43 H23 2 -0.474756 0.516884 0.266577 11.00000 -1.20000 AFIX 0 C24 1 -0.606050 0.609651 0.206973 11.00000 0.03263 0.02436 = 0.03715 -0.00606 0.00886 0.00159 AFIX 43 H24 2 -0.676808 0.614448 0.241009 11.00000 -1.20000 AFIX 0 C25 1 -0.620818 0.660856 0.142778 11.00000 0.03847 0.03546 = 0.05380 0.01387 0.01240 0.01379 AFIX 43 H25 2 -0.700760 0.702050 0.133101 11.00000 -1.20000 AFIX 0 C26 1 -0.519736 0.652570 0.092312 11.00000 0.04351 0.04686 = 0.05827 0.03108 0.02053 0.02146 AFIX 43 H26 2 -0.530813 0.687891 0.048010 11.00000 -1.20000 AFIX 0 C27 1 -0.402919 0.593172 0.106135 11.00000 0.03283 0.03870 = 0.04914 0.01381 0.01250 0.00847 AFIX 43 H27 2 -0.334260 0.587598 0.071111 11.00000 -1.20000 AFIX 0 N1 3 0.132073 0.458621 0.145072 11.00000 0.02944 0.01624 = 0.03818 0.00098 0.00570 -0.00198 N2 3 0.185446 0.316751 0.174893 11.00000 0.02388 0.01992 = 0.02691 -0.00074 0.00306 -0.00208 N3 3 -0.121294 0.371484 0.242928 11.00000 0.02450 0.01879 = 0.02042 -0.00173 0.00332 0.00381 N4 3 -0.227634 0.436666 0.248956 11.00000 0.02334 0.01646 = 0.02915 -0.00153 0.00493 0.00587 O1 4 -0.012005 0.572292 0.060271 11.00000 0.04497 0.02367 = 0.03329 0.00930 0.01288 0.00217 O2 4 0.003812 0.583422 0.198326 11.00000 0.03420 0.01429 = 0.04035 -0.00198 0.00783 -0.00119 O3 4 -0.388052 0.088328 -0.004259 11.00000 0.03234 0.02282 = 0.02620 -0.00586 0.00014 -0.00387 S1 5 -0.003960 0.528707 0.132132 11.00000 0.03128 0.01563 = 0.03274 0.00269 0.00880 -0.00184 HKLF 4 Covalent radii and connectivity table for 2008src0864 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 C1 - N2 N1 C2 C2 - N3 C8 C1 C3 C3 - C21 C2 S1 C4 - N2 C5 C5 - C4 C6 - N2 C7 C7 - C6 C8 - C13 C9 C2 C9 - C10 C8 C10 - C11 C9 C11 - O3 C12 C10 C12 - C11 C13 C13 - C8 C12 C14 - O3 C15 - C16 C20 N3 C16 - C15 C17 C17 - C18 C16 C18 - C17 C19 C19 - C20 C18 C20 - C19 C15 C21 - N4 C22 C3 C22 - C27 C23 C21 C23 - C24 C22 C24 - C25 C23 C25 - C24 C26 C26 - C27 C25 C27 - C26 C22 N1 - C1 S1 N2 - C1 C4 C6 N3 - N4 C15 C2 N4 - C21 N3 O1 - S1 O2 - S1 O3 - C11 C14 S1 - O1 O2 N1 C3 32207 Reflections read, of which 575 rejected -11 =< h =< 11, -19 =< k =< 18, -22 =< l =< 22, Max. 2-theta = 54.43 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 3 16 2 -2.15 1.67 3 14.55 -2 16 5 -7.65 6.41 3 41.89 2 Inconsistent equivalents 5360 Unique reflections, of which 0 suppressed R(int) = 0.1765 R(sigma) = 0.1476 Friedel opposites merged Maximum memory for data reduction = 3114 / 53126 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 = 4018 / 397687 wR2 = 0.1744 before cycle 1 for 5360 data and 316 / 316 parameters GooF = S = 1.011; Restrained GooF = 1.011 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0664 * P )^2 + 1.34 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.51872 0.00128 -0.700 OSF Mean shift/esd = 0.043 Maximum = -0.700 for OSF Max. shift = 0.001 A for H14C Max. dU = 0.000 for C18 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4018 / 397687 wR2 = 0.1743 before cycle 2 for 5360 data and 316 / 316 parameters GooF = S = 1.010; Restrained GooF = 1.010 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0664 * P )^2 + 1.34 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.51849 0.00128 -0.185 OSF Mean shift/esd = 0.015 Maximum = -0.185 for OSF Max. shift = 0.000 A for H14C Max. dU = 0.000 for C18 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4018 / 397687 wR2 = 0.1743 before cycle 3 for 5360 data and 316 / 316 parameters GooF = S = 1.010; Restrained GooF = 1.010 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0664 * P )^2 + 1.34 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.51848 0.00128 -0.003 OSF Mean shift/esd = 0.001 Maximum = -0.005 for U13 C18 Max. shift = 0.000 A for O1 Max. dU = 0.000 for C26 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4018 / 397687 wR2 = 0.1743 before cycle 4 for 5360 data and 316 / 316 parameters GooF = S = 1.010; Restrained GooF = 1.010 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0664 * P )^2 + 1.34 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.51848 0.00128 -0.001 OSF Mean shift/esd = 0.000 Maximum = 0.002 for U11 C22 Max. shift = 0.000 A for C19 Max. dU = 0.000 for C22 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 -0.2196 0.4449 0.0763 13 1.000 0.000 C3 C21 C2 S1 H4A 0.4106 0.2893 0.1966 23 0.990 0.000 C4 N2 C5 H4B 0.3748 0.3902 0.2021 23 0.990 0.000 C4 N2 C5 H5A 0.4833 0.3631 0.0928 33 0.980 0.000 C5 C4 H5A H5B 0.3130 0.3974 0.0672 33 0.980 0.000 C5 C4 H5A H5C 0.3496 0.2965 0.0620 33 0.980 0.000 C5 C4 H5A H6A 0.0459 0.2238 0.2051 23 0.990 0.000 C6 N2 C7 H6B 0.2163 0.2173 0.2508 23 0.990 0.000 C6 N2 C7 H7A 0.1673 0.1016 0.1640 33 0.980 0.000 C7 C6 H7A H7B 0.2973 0.1618 0.1403 33 0.980 0.000 C7 C6 H7A H7C 0.1268 0.1682 0.0946 33 0.980 0.000 C7 C6 H7A H9 -0.0507 0.3034 0.0283 43 0.950 0.000 C9 C10 C8 H10 -0.1694 0.1874 -0.0417 43 0.950 0.000 C10 C11 C9 H12 -0.4187 0.1428 0.1232 43 0.950 0.000 C12 C11 C13 H13 -0.2921 0.2548 0.1956 43 0.950 0.000 C13 C8 C12 H14A -0.4148 0.0139 -0.0969 33 0.980 0.000 C14 O3 H14A H14B -0.2426 0.0432 -0.0679 33 0.980 0.000 C14 O3 H14A H14C -0.3631 0.1106 -0.1116 33 0.980 0.000 C14 O3 H14A H16 -0.0397 0.2385 0.3296 43 0.950 0.000 C16 C15 C17 H17 0.1565 0.2256 0.4349 43 0.950 0.000 C17 C18 C16 H18 0.3089 0.3433 0.4766 43 0.950 0.000 C18 C17 C19 H19 0.2625 0.4774 0.4162 43 0.950 0.000 C19 C20 C18 H20 0.0672 0.4913 0.3114 43 0.950 0.000 C20 C19 C15 H23 -0.4747 0.5169 0.2666 43 0.950 0.000 C23 C24 C22 H24 -0.6768 0.6144 0.2410 43 0.950 0.000 C24 C25 C23 H25 -0.7007 0.7021 0.1331 43 0.950 0.000 C25 C24 C26 H26 -0.5309 0.6878 0.0480 43 0.950 0.000 C26 C27 C25 H27 -0.3342 0.5876 0.0711 43 0.950 0.000 C27 C26 C22 2008src0864 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.08498 0.38037 0.16157 1.00000 0.02435 0.01806 0.02018 0.00070 0.00180 -0.00255 0.02110 0.00623 0.00043 0.00021 0.00019 0.00000 0.00231 0.00182 0.00191 0.00135 0.00162 0.00147 0.00081 C2 -0.08495 0.36926 0.16333 1.00000 0.02443 0.01637 0.01971 0.00097 0.00521 -0.00130 0.02000 0.00629 0.00042 0.00020 0.00019 0.00000 0.00227 0.00170 0.00185 0.00133 0.00160 0.00142 0.00079 C3 -0.16167 0.45332 0.12915 1.00000 0.02577 0.01635 0.02590 0.00203 -0.00019 -0.00062 0.02322 0.00655 0.00043 0.00020 0.00020 0.00000 0.00231 0.00177 0.00202 0.00139 0.00167 0.00142 0.00083 H3 -0.21958 0.44489 0.07633 1.00000 0.02787 0.00000 0.00000 C4 0.34574 0.33692 0.17228 1.00000 0.02526 0.02121 0.03738 -0.00370 0.00337 -0.00124 0.02819 0.00677 0.00044 0.00023 0.00021 0.00000 0.00239 0.00191 0.00230 0.00156 0.00182 0.00153 0.00089 H4A 0.41059 0.28926 0.19665 1.00000 0.03382 0.00000 0.00000 H4B 0.37483 0.39021 0.20206 1.00000 0.03382 0.00000 0.00000 C5 0.37553 0.34962 0.09139 1.00000 0.03273 0.03523 0.04645 0.00372 0.01282 0.00021 0.03743 0.00796 0.00051 0.00025 0.00023 0.00000 0.00265 0.00229 0.00264 0.00184 0.00205 0.00185 0.00102 H5A 0.48325 0.36311 0.09283 1.00000 0.05614 0.00000 0.00000 H5B 0.31297 0.39741 0.06724 1.00000 0.05614 0.00000 0.00000 H5C 0.34955 0.29652 0.06198 1.00000 0.05614 0.00000 0.00000 C6 0.15434 0.22809 0.19998 1.00000 0.02697 0.01741 0.02260 0.00462 0.00490 0.00125 0.02225 0.00654 0.00044 0.00020 0.00019 0.00000 0.00230 0.00175 0.00195 0.00136 0.00163 0.00147 0.00081 H6A 0.04589 0.22383 0.20511 1.00000 0.02671 0.00000 0.00000 H6B 0.21628 0.21735 0.25085 1.00000 0.02671 0.00000 0.00000 C7 0.18958 0.15875 0.14481 1.00000 0.03648 0.01821 0.02870 0.00268 0.00631 0.00501 0.02771 0.00694 0.00047 0.00021 0.00020 0.00000 0.00260 0.00186 0.00212 0.00146 0.00183 0.00158 0.00090 H7A 0.16725 0.10163 0.16401 1.00000 0.04157 0.00000 0.00000 H7B 0.29733 0.16181 0.14029 1.00000 0.04157 0.00000 0.00000 H7C 0.12683 0.16819 0.09461 1.00000 0.04157 0.00000 0.00000 C8 -0.15952 0.29097 0.11923 1.00000 0.02239 0.01420 0.02093 0.00220 0.00106 -0.00180 0.01949 0.00617 0.00041 0.00020 0.00019 0.00000 0.00222 0.00167 0.00190 0.00132 0.00157 0.00135 0.00079 C9 -0.12459 0.27035 0.04826 1.00000 0.02493 0.02141 0.02524 0.00552 0.00467 -0.00228 0.02382 0.00656 0.00043 0.00021 0.00020 0.00000 0.00230 0.00182 0.00206 0.00145 0.00166 0.00150 0.00083 H9 -0.05067 0.30341 0.02834 1.00000 0.02858 0.00000 0.00000 C10 -0.19645 0.20198 0.00607 1.00000 0.02878 0.02416 0.01749 0.00102 0.00223 0.00150 0.02369 0.00646 0.00044 0.00021 0.00020 0.00000 0.00238 0.00188 0.00187 0.00142 0.00165 0.00156 0.00084 H10 -0.16945 0.18739 -0.04173 1.00000 0.02842 0.00000 0.00000 C11 -0.30711 0.15520 0.03357 1.00000 0.02250 0.01509 0.02389 0.00198 -0.00151 0.00057 0.02114 0.00616 0.00041 0.00020 0.00019 0.00000 0.00220 0.00170 0.00196 0.00137 0.00163 0.00143 0.00080 C12 -0.34296 0.17508 0.10399 1.00000 0.02970 0.01840 0.02285 0.00166 0.00531 -0.00303 0.02355 0.00651 0.00044 0.00021 0.00019 0.00000 0.00238 0.00179 0.00201 0.00142 0.00169 0.00148 0.00084 H12 -0.41875 0.14284 0.12319 1.00000 0.02826 0.00000 0.00000 C13 -0.26827 0.24219 0.14675 1.00000 0.02612 0.02039 0.02240 0.00004 0.00695 0.00017 0.02264 0.00649 0.00043 0.00021 0.00020 0.00000 0.00230 0.00183 0.00197 0.00140 0.00163 0.00148 0.00082 H13 -0.29213 0.25481 0.19561 1.00000 0.02717 0.00000 0.00000 C14 -0.34902 0.06188 -0.07586 1.00000 0.06454 0.03926 0.03102 -0.01390 0.01046 -0.01223 0.04467 0.00780 0.00059 0.00027 0.00023 0.00000 0.00356 0.00242 0.00244 0.00183 0.00225 0.00219 0.00119 H14A -0.41475 0.01385 -0.09687 1.00000 0.06701 0.00000 0.00000 H14B -0.24256 0.04318 -0.06793 1.00000 0.06701 0.00000 0.00000 H14C -0.36311 0.11058 -0.11163 1.00000 0.06701 0.00000 0.00000 C15 -0.00238 0.36565 0.30926 1.00000 0.02704 0.01877 0.01790 -0.00182 0.00530 0.00028 0.02107 0.00632 0.00043 0.00021 0.00019 0.00000 0.00232 0.00178 0.00186 0.00139 0.00161 0.00147 0.00081 C16 0.02232 0.28693 0.34660 1.00000 0.02486 0.01987 0.02424 -0.00151 0.01078 -0.00094 0.02222 0.00663 0.00042 0.00021 0.00019 0.00000 0.00232 0.00183 0.00203 0.00140 0.00171 0.00144 0.00083 H16 -0.03971 0.23847 0.32958 1.00000 0.02666 0.00000 0.00000 C17 0.13887 0.27950 0.40931 1.00000 0.02776 0.02452 0.02522 0.00413 0.00645 0.00558 0.02561 0.00687 0.00044 0.00022 0.00020 0.00000 0.00237 0.00194 0.00205 0.00149 0.00175 0.00159 0.00086 H17 0.15648 0.22561 0.43492 1.00000 0.03073 0.00000 0.00000 C18 0.22844 0.34933 0.43440 1.00000 0.02980 0.03931 0.02772 0.00088 0.00012 0.00100 0.03285 0.00724 0.00047 0.00025 0.00022 0.00000 0.00256 0.00238 0.00218 0.00170 0.00185 0.00180 0.00096 H18 0.30895 0.34329 0.47657 1.00000 0.03942 0.00000 0.00000 C19 0.20169 0.42882 0.39827 1.00000 0.04333 0.02421 0.03019 -0.00394 0.00103 -0.01161 0.03320 0.00703 0.00050 0.00023 0.00022 0.00000 0.00282 0.00204 0.00229 0.00160 0.00199 0.00176 0.00099 H19 0.26247 0.47745 0.41624 1.00000 0.03984 0.00000 0.00000 C20 0.08617 0.43686 0.33603 1.00000 0.03313 0.02233 0.02931 0.00022 0.00249 -0.00052 0.02860 0.00685 0.00046 0.00023 0.00021 0.00000 0.00259 0.00193 0.00218 0.00152 0.00187 0.00161 0.00091 H20 0.06719 0.49126 0.31144 1.00000 0.03432 0.00000 0.00000 C21 -0.26288 0.47700 0.18519 1.00000 0.02385 0.01576 0.03050 0.00077 0.00410 0.00031 0.02344 0.00649 0.00042 0.00021 0.00020 0.00000 0.00224 0.00177 0.00211 0.00149 0.00169 0.00145 0.00083 C22 -0.38499 0.54143 0.17097 1.00000 0.02232 0.01719 0.03589 0.00340 -0.00015 0.00045 0.02575 0.00673 0.00044 0.00021 0.00021 0.00000 0.00223 0.00181 0.00224 0.00149 0.00173 0.00145 0.00085 C23 -0.48691 0.55097 0.22153 1.00000 0.03069 0.02076 0.02890 -0.00636 0.00246 -0.00106 0.02710 0.00655 0.00045 0.00022 0.00021 0.00000 0.00248 0.00188 0.00212 0.00145 0.00179 0.00153 0.00088 H23 -0.47474 0.51686 0.26658 1.00000 0.03252 0.00000 0.00000 C24 -0.60603 0.60964 0.20698 1.00000 0.03235 0.02425 0.03694 -0.00605 0.00891 0.00161 0.03083 0.00687 0.00047 0.00022 0.00022 0.00000 0.00262 0.00201 0.00242 0.00164 0.00191 0.00163 0.00095 H24 -0.67678 0.61445 0.24102 1.00000 0.03700 0.00000 0.00000 C25 -0.62082 0.66085 0.14277 1.00000 0.03821 0.03543 0.05367 0.01390 0.01232 0.01378 0.04192 0.00846 0.00052 0.00026 0.00025 0.00000 0.00289 0.00237 0.00286 0.00200 0.00226 0.00194 0.00111 H25 -0.70074 0.70206 0.13310 1.00000 0.05030 0.00000 0.00000 C26 -0.51978 0.65254 0.09229 1.00000 0.04319 0.04681 0.05827 0.03123 0.02049 0.02145 0.04803 0.00958 0.00054 0.00027 0.00027 0.00000 0.00310 0.00269 0.00303 0.00224 0.00242 0.00219 0.00125 H26 -0.53091 0.68782 0.04797 1.00000 0.05764 0.00000 0.00000 C27 -0.40289 0.59317 0.10614 1.00000 0.03281 0.03860 0.04881 0.01391 0.01258 0.00857 0.03941 0.00830 0.00051 0.00025 0.00025 0.00000 0.00278 0.00241 0.00277 0.00194 0.00212 0.00186 0.00107 H27 -0.33420 0.58760 0.07113 1.00000 0.04730 0.00000 0.00000 N1 0.13208 0.45860 0.14508 1.00000 0.02916 0.01611 0.03817 0.00100 0.00581 -0.00201 0.02781 0.00562 0.00037 0.00017 0.00018 0.00000 0.00205 0.00153 0.00191 0.00127 0.00152 0.00126 0.00075 N2 0.18546 0.31673 0.17491 1.00000 0.02368 0.01971 0.02676 -0.00077 0.00297 -0.00212 0.02354 0.00527 0.00035 0.00017 0.00016 0.00000 0.00191 0.00154 0.00172 0.00120 0.00139 0.00127 0.00070 N3 -0.12126 0.37147 0.24293 1.00000 0.02442 0.01854 0.02029 -0.00169 0.00320 0.00385 0.02116 0.00522 0.00035 0.00017 0.00016 0.00000 0.00190 0.00146 0.00159 0.00115 0.00135 0.00122 0.00068 N4 -0.22763 0.43666 0.24896 1.00000 0.02324 0.01618 0.02892 -0.00160 0.00475 0.00584 0.02275 0.00536 0.00035 0.00017 0.00017 0.00000 0.00188 0.00148 0.00176 0.00122 0.00140 0.00122 0.00070 O1 -0.01201 0.57231 0.06027 1.00000 0.04494 0.02346 0.03313 0.00936 0.01291 0.00215 0.03311 0.00500 0.00033 0.00015 0.00014 0.00000 0.00192 0.00136 0.00158 0.00108 0.00135 0.00118 0.00068 O2 0.00384 0.58342 0.19833 1.00000 0.03399 0.01412 0.04012 -0.00205 0.00778 -0.00117 0.02924 0.00453 0.00030 0.00014 0.00014 0.00000 0.00174 0.00122 0.00163 0.00105 0.00128 0.00105 0.00064 O3 -0.38806 0.08832 -0.00425 1.00000 0.03218 0.02268 0.02608 -0.00585 0.00013 -0.00388 0.02756 0.00433 0.00030 0.00014 0.00014 0.00000 0.00172 0.00129 0.00143 0.00102 0.00119 0.00109 0.00062 S1 -0.00396 0.52870 0.13213 1.00000 0.03114 0.01551 0.03263 0.00269 0.00878 -0.00183 0.02604 0.00176 0.00012 0.00005 0.00005 0.00000 0.00060 0.00045 0.00054 0.00037 0.00043 0.00038 0.00026 Final Structure Factor Calculation for 2008src0864 in P2(1)/c Total number of l.s. parameters = 316 Maximum vector length = 511 Memory required = 3702 / 24017 wR2 = 0.1743 before cycle 5 for 5360 data and 0 / 316 parameters GooF = S = 1.010; Restrained GooF = 1.010 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0664 * P )^2 + 1.34 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0749 for 2847 Fo > 4sig(Fo) and 0.1647 for all 5360 data wR2 = 0.1743, GooF = S = 1.010, Restrained GooF = 1.010 for all data Occupancy sum of asymmetric unit = 35.00 for non-hydrogen and 28.00 for hydrogen atoms Principal mean square atomic displacements U 0.0265 0.0197 0.0171 C1 0.0248 0.0196 0.0156 C2 0.0317 0.0220 0.0159 C3 0.0388 0.0256 0.0201 C4 0.0487 0.0347 0.0288 C5 0.0274 0.0247 0.0147 C6 0.0378 0.0287 0.0167 C7 0.0258 0.0194 0.0133 C8 0.0298 0.0252 0.0165 C9 0.0297 0.0240 0.0173 C10 0.0300 0.0191 0.0144 C11 0.0305 0.0234 0.0168 C12 0.0272 0.0204 0.0203 C13 0.0699 0.0436 0.0206 C14 0.0271 0.0201 0.0160 C15 0.0304 0.0197 0.0165 C16 0.0332 0.0239 0.0197 C17 0.0394 0.0347 0.0244 C18 0.0503 0.0321 0.0172 C19 0.0353 0.0282 0.0223 C20 0.0307 0.0239 0.0157 C21 0.0392 0.0216 0.0164 C22 0.0343 0.0298 0.0172 C23 0.0396 0.0322 0.0207 C24 0.0639 0.0398 0.0221 C25 0.0910 0.0345 0.0186 C26 0.0602 0.0316 0.0264 C27 0.0383 0.0294 0.0157 N1 0.0276 0.0244 0.0187 N2 0.0270 0.0206 0.0160 N3 0.0294 0.0264 0.0125 N4 0.0479 0.0342 0.0173 O1 0.0404 0.0334 0.0139 O2 0.0359 0.0300 0.0168 O3 0.0348 0.0287 0.0146 S1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.009 0.018 0.027 0.038 0.049 0.063 0.080 0.107 0.156 1.000 Number in group 580. 524. 504. 570. 519. 523. 536. 537. 531. 536. GooF 0.955 0.997 0.982 0.991 1.017 1.078 1.062 1.036 0.998 0.983 K 8.443 2.726 1.218 1.182 1.126 1.041 1.030 1.000 1.017 0.968 Resolution(A) 0.78 0.81 0.84 0.88 0.92 0.98 1.06 1.16 1.33 1.67 inf Number in group 548. 530. 533. 532. 547. 530. 531. 535. 535. 539. GooF 0.905 0.897 0.959 1.024 0.980 0.984 1.020 0.927 0.996 1.337 K 1.059 1.051 0.993 1.009 1.094 1.007 1.023 1.015 1.033 0.953 R1 0.387 0.378 0.316 0.270 0.214 0.141 0.097 0.081 0.066 0.060 Recommended weighting scheme: WGHT 0.0647 1.4272 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) -1 2 4 165.66 54.71 5.37 0.036 3.71 0 2 3 283.11 146.63 5.25 0.059 4.66 -2 1 3 206.69 74.43 4.35 0.042 3.73 2 0 2 178.48 368.02 4.10 0.094 3.68 0 3 4 57.95 3.62 3.97 0.009 3.34 2 4 0 738.26 505.80 3.91 0.110 2.90 5 2 7 153.14 25.42 3.62 0.025 1.32 -1 2 3 3144.67 4070.99 3.55 0.313 4.37 -5 4 4 226.51 80.14 3.51 0.044 1.59 1 13 8 103.10 219.21 3.51 0.073 1.03 -5 6 7 117.77 1.87 3.51 0.007 1.34 -6 8 9 592.93 393.08 3.50 0.097 1.07 -4 17 3 374.93 36.73 3.46 0.030 0.84 8 6 4 635.12 1074.43 3.39 0.161 0.95 0 17 4 768.84 135.42 3.38 0.057 0.89 -3 4 7 913.88 690.17 3.38 0.129 1.84 -8 5 12 123.53 2.69 3.34 0.008 0.92 3 13 4 -19.54 56.76 3.24 0.037 1.05 -1 11 9 88.15 21.12 3.24 0.023 1.15 -7 5 15 324.72 104.04 3.23 0.050 0.90 -7 4 14 4054.04 88.40 3.23 0.046 0.94 -8 10 1 -26.81 132.80 3.22 0.057 0.90 2 8 10 177.92 79.30 3.17 0.044 1.20 -5 3 14 103.79 6.99 3.12 0.013 1.09 -6 6 1 948.48 607.04 3.08 0.121 1.28 -1 7 6 254.43 166.96 3.05 0.063 1.76 0 1 5 107.90 41.97 3.04 0.032 3.42 -4 1 3 176.16 73.76 3.01 0.042 2.16 1 2 3 1523.75 1215.47 3.00 0.171 3.90 3 6 13 147.90 38.29 2.96 0.030 1.05 0 4 2 37.35 0.32 2.93 0.003 3.54 -2 5 13 187.01 74.87 2.92 0.042 1.24 -2 0 18 -65.11 127.80 2.91 0.055 0.99 -3 5 5 131.65 55.97 2.91 0.037 1.93 -5 16 8 165.35 315.11 2.89 0.087 0.81 1 12 7 300.44 201.91 2.87 0.070 1.13 3 16 2 -8.00 148.12 2.86 0.060 0.91 1 2 5 263.83 176.01 2.85 0.065 2.86 -2 1 10 759.38 580.64 2.85 0.118 1.72 2 4 14 70.27 0.05 2.85 0.001 1.10 -5 5 15 9.25 86.78 2.84 0.046 1.00 3 2 7 450.95 332.16 2.82 0.089 1.72 8 6 9 42.25 285.35 2.81 0.083 0.84 1 9 2 534.24 410.63 2.81 0.099 1.65 -2 6 6 275.36 191.60 2.81 0.068 1.85 5 11 3 104.50 257.44 2.80 0.079 1.06 -2 7 9 159.69 83.12 2.78 0.045 1.44 0 16 11 237.61 31.95 2.77 0.028 0.83 2 6 2 555.29 425.18 2.76 0.101 2.11 -6 9 5 47.10 130.08 2.75 0.056 1.11 Bond lengths and angles C1 - Distance Angles N2 1.3252 (0.0044) N1 1.3302 (0.0043) 119.03 (0.34) C2 1.5322 (0.0051) 123.71 (0.29) 117.26 (0.30) C1 - N2 N1 C2 - Distance Angles N3 1.5063 (0.0043) C8 1.5315 (0.0046) 110.77 (0.27) C1 1.5322 (0.0051) 112.98 (0.28) 115.01 (0.28) C3 1.5446 (0.0046) 101.45 (0.26) 109.85 (0.28) 105.73 (0.26) C2 - N3 C8 C1 C3 - Distance Angles C21 1.5013 (0.0050) C2 1.5446 (0.0046) 102.74 (0.27) S1 1.8216 (0.0036) 112.01 (0.24) 103.84 (0.24) H3 1.0000 112.51 112.51 112.51 C3 - C21 C2 S1 C4 - Distance Angles N2 1.4728 (0.0048) C5 1.5203 (0.0053) 112.72 (0.32) H4A 0.9900 109.05 109.05 H4B 0.9900 109.05 109.05 107.81 C4 - N2 C5 H4A C5 - Distance Angles C4 1.5203 (0.0053) H5A 0.9800 109.47 H5B 0.9800 109.47 109.47 H5C 0.9800 109.47 109.47 109.47 C5 - C4 H5A H5B C6 - Distance Angles N2 1.4826 (0.0042) C7 1.5227 (0.0047) 112.78 (0.28) H6A 0.9900 109.03 109.03 H6B 0.9900 109.03 109.03 107.80 C6 - N2 C7 H6A C7 - Distance Angles C6 1.5227 (0.0047) H7A 0.9800 109.47 H7B 0.9800 109.47 109.47 H7C 0.9800 109.47 109.47 109.47 C7 - C6 H7A H7B C8 - Distance Angles C13 1.3838 (0.0049) C9 1.3886 (0.0049) 118.51 (0.31) C2 1.5315 (0.0046) 121.29 (0.31) 120.11 (0.30) C8 - C13 C9 C9 - Distance Angles C10 1.3882 (0.0049) C8 1.3886 (0.0049) 120.75 (0.33) H9 0.9500 119.63 119.63 C9 - C10 C8 C10 - Distance Angles C11 1.3801 (0.0050) C9 1.3882 (0.0049) 120.01 (0.33) H10 0.9500 120.00 120.00 C10 - C11 C9 C11 - Distance Angles O3 1.3703 (0.0039) C12 1.3797 (0.0048) 115.40 (0.31) C10 1.3801 (0.0050) 124.81 (0.32) 119.79 (0.32) C11 - O3 C12 C12 - Distance Angles C11 1.3797 (0.0048) C13 1.3879 (0.0048) 119.99 (0.33) H12 0.9500 120.01 120.01 C12 - C11 C13 C13 - Distance Angles C8 1.3838 (0.0049) C12 1.3879 (0.0048) 120.92 (0.33) H13 0.9500 119.54 119.54 C13 - C8 C12 C14 - Distance Angles O3 1.4366 (0.0046) H14A 0.9800 109.47 H14B 0.9800 109.47 109.47 H14C 0.9800 109.47 109.47 109.47 C14 - O3 H14A H14B C15 - Distance Angles C16 1.3863 (0.0046) C20 1.3910 (0.0049) 119.81 (0.33) N3 1.4478 (0.0044) 118.62 (0.30) 121.57 (0.29) C15 - C16 C20 C16 - Distance Angles C15 1.3863 (0.0046) C17 1.3931 (0.0051) 119.44 (0.32) H16 0.9500 120.28 120.28 C16 - C15 C17 C17 - Distance Angles C18 1.3718 (0.0052) C16 1.3931 (0.0051) 120.58 (0.32) H17 0.9500 119.71 119.71 C17 - C18 C16 C18 - Distance Angles C17 1.3718 (0.0052) C19 1.3888 (0.0053) 120.15 (0.36) H18 0.9500 119.93 119.93 C18 - C17 C19 C19 - Distance Angles C20 1.3828 (0.0055) C18 1.3888 (0.0053) 119.69 (0.35) H19 0.9500 120.15 120.15 C19 - C20 C18 C20 - Distance Angles C19 1.3828 (0.0055) C15 1.3910 (0.0049) 120.30 (0.32) H20 0.9500 119.85 119.85 C20 - C19 C15 C21 - Distance Angles N4 1.2855 (0.0043) C22 1.4664 (0.0050) 122.95 (0.33) C3 1.5013 (0.0051) 112.56 (0.31) 124.44 (0.31) C21 - N4 C22 C22 - Distance Angles C27 1.3901 (0.0053) C23 1.3927 (0.0053) 118.69 (0.35) C21 1.4664 (0.0050) 120.68 (0.36) 120.62 (0.33) C22 - C27 C23 C23 - Distance Angles C24 1.3879 (0.0052) C22 1.3927 (0.0053) 120.89 (0.35) H23 0.9500 119.56 119.56 C23 - C24 C22 C24 - Distance Angles C25 1.3775 (0.0054) C23 1.3879 (0.0052) 119.45 (0.38) H24 0.9500 120.27 120.27 C24 - C25 C23 C25 - Distance Angles C24 1.3775 (0.0054) C26 1.3837 (0.0060) 120.29 (0.38) H25 0.9500 119.85 119.85 C25 - C24 C26 C26 - Distance Angles C27 1.3799 (0.0056) C25 1.3837 (0.0060) 120.21 (0.39) H26 0.9500 119.90 119.90 C26 - C27 C25 C27 - Distance Angles C26 1.3799 (0.0056) C22 1.3901 (0.0053) 120.44 (0.41) H27 0.9500 119.78 119.78 C27 - C26 C22 N1 - Distance Angles C1 1.3302 (0.0043) S1 1.6146 (0.0032) 112.57 (0.27) N1 - C1 N2 - Distance Angles C1 1.3252 (0.0044) C4 1.4728 (0.0048) 117.91 (0.28) C6 1.4826 (0.0042) 125.77 (0.32) 116.03 (0.29) N2 - C1 C4 N3 - Distance Angles N4 1.4016 (0.0038) C15 1.4478 (0.0044) 113.17 (0.25) C2 1.5063 (0.0043) 110.26 (0.25) 121.25 (0.29) N3 - N4 C15 N4 - Distance Angles C21 1.2855 (0.0043) N3 1.4016 (0.0038) 110.35 (0.28) N4 - C21 O1 - Distance Angles S1 1.4361 (0.0026) O1 - O2 - Distance Angles S1 1.4421 (0.0025) O2 - O3 - Distance Angles C11 1.3703 (0.0039) C14 1.4366 (0.0046) 117.54 (0.30) O3 - C11 S1 - Distance Angles O1 1.4361 (0.0026) O2 1.4421 (0.0025) 116.06 (0.15) N1 1.6146 (0.0032) 111.32 (0.17) 110.37 (0.16) C3 1.8216 (0.0037) 110.76 (0.17) 109.14 (0.16) 97.63 (0.15) S1 - O1 O2 N1 FMAP and GRID set by program FMAP 2 3 22 GRID -1.316 -2 -2 1.316 2 2 R1 = 0.1635 for 5360 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.48 at 0.5664 0.8456 0.2395 [ 1.28 A from H4B ] Deepest hole -0.48 at 0.9245 0.5546 0.1280 [ 0.75 A from S1 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 3597 / 24324 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4336 0.3456 0.2605 1.00000 0.05 0.48 1.28 H4B 1.42 H4A 1.63 C4 2.50 N2 Q2 1 -0.4301 0.1025 0.1427 1.00000 0.05 0.38 0.73 H12 1.59 C12 2.13 H24 2.33 H14A Q3 1 0.4803 0.4143 0.2778 1.00000 0.05 0.33 1.55 H4B 1.66 H23 2.24 H14C 2.37 C4 Q4 1 -0.1375 0.4148 0.1432 1.00000 0.05 0.28 0.67 C3 0.89 C2 1.37 H3 1.74 C21 Q5 1 -0.1390 0.5169 0.0248 1.00000 0.05 0.27 1.47 O1 1.68 H3 2.08 S1 2.14 C3 Q6 1 -0.0144 0.6608 0.0471 1.00000 0.05 0.27 1.39 O1 1.65 H9 1.69 H17 2.35 C17 Q7 1 -0.0568 0.3989 0.0154 1.00000 0.05 0.27 1.49 H9 1.63 O1 2.08 H3 2.19 C9 Q8 1 -0.1787 -0.0600 -0.0147 1.00000 0.05 0.26 1.89 H14B 2.08 H18 2.10 H19 2.10 C18 Q9 1 -0.2644 0.5356 0.0251 1.00000 0.05 0.26 1.37 H27 1.68 H3 1.93 H5B 2.24 C27 Q10 1 0.0848 0.5129 0.1134 1.00000 0.05 0.26 0.94 S1 1.06 N1 1.48 O1 2.09 O2 Q11 1 0.0404 0.1191 -0.0029 1.00000 0.05 0.25 1.93 H7C 2.16 H10 2.22 C18 2.48 C17 Q12 1 -0.2016 0.4744 -0.0213 1.00000 0.05 0.25 1.83 H3 2.26 O1 2.30 H5B 2.53 O1 Q13 1 -0.6018 0.6430 0.1079 1.00000 0.05 0.25 0.73 C25 0.84 C26 1.40 H25 1.50 H26 Q14 1 0.2125 0.4387 0.1870 1.00000 0.05 0.25 0.99 N1 1.46 C1 1.61 H4B 1.91 N2 Q15 1 -0.6452 0.7167 -0.0211 1.00000 0.05 0.25 1.52 H26 1.94 C10 2.03 C11 2.04 C9 Q16 1 0.1454 0.5008 0.4597 1.00000 0.05 0.24 1.45 H19 1.70 C19 2.08 H14B 2.39 C20 Q17 1 0.1269 0.6593 0.2346 1.00000 0.05 0.24 1.66 O2 1.76 H16 1.87 H24 2.26 H6A Q18 1 0.1599 0.4829 0.1998 1.00000 0.05 0.24 1.03 N1 1.81 C1 1.87 S1 2.08 O2 Q19 1 0.6210 0.3588 0.1701 1.00000 0.05 0.24 1.68 H5A 1.81 H13 2.10 C21 2.13 C13 Q20 1 -0.7412 0.5059 0.2488 1.00000 0.05 0.24 1.79 H24 2.12 N1 2.21 H20 2.21 C24 Shortest distances between peaks (including symmetry equivalents) 14 18 0.88 5 12 1.12 5 9 1.16 1 3 1.16 18 20 1.18 8 16 1.35 9 12 1.43 14 20 1.52 8 11 1.53 10 18 1.63 6 7 1.65 7 12 1.78 10 14 1.95 5 7 1.99 10 12 2.10 11 16 2.23 5 10 2.32 5 7 2.38 3 20 2.42 4 19 2.45 5 6 2.49 4 7 2.51 1 19 2.52 13 15 2.53 1 14 2.61 3 19 2.61 4 10 2.62 5 10 2.63 4 5 2.63 10 20 2.63 7 10 2.64 17 20 2.64 7 10 2.64 6 10 2.66 11 16 2.67 3 14 2.67 2 20 2.70 12 13 2.80 5 5 2.82 17 18 2.82 7 9 2.84 4 18 2.87 4 9 2.89 1 20 2.92 6 9 2.93 6 12 2.93 15 19 2.94 Time profile in seconds ----------------------- 0.16: 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. 5.73: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.03: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.67: Structure factors and derivatives 2.73: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.56: 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 0.09: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008src0864 finished at 16:19:07 Total CPU time: 11.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++