+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2010sl0005a started at 08:07:12 on 08-Apr-2011 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2010sl0005a CELL 0.71073 6.2066 7.7799 21.3938 90.000 90.000 90.000 ZERR 4.00 0.0003 0.0004 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 F UNIT 52 0 4 12 V = 1033.04 F(000) = 448.0 Mu = 0.13 mm-1 Cell Wt = 908.56 Rho = 1.460 MERG 2 OMIT -3.00 50.00 OMIT 0 1 3 SHEL 7 0.77 HFIX 43 -1.20 C2 C5 C7 C8 C10 C11 C12 C13 FMAP 2 PLAN 20 SIZE 0.06 0.28 0.32 ACTA BOND $H WGHT 0.14650 0.69840 L.S. 20 TEMP 23.00 FVAR 0.23807 F1 4 0.282364 0.764477 0.153429 11.00000 0.05132 0.03336 = 0.03845 -0.01181 -0.01164 -0.00378 F2 4 -0.271071 0.046587 -0.305065 11.00000 0.03560 0.03759 = 0.03371 -0.00996 -0.00343 -0.00277 F3 4 -0.096653 0.605259 0.142229 11.00000 0.04413 0.05140 = 0.03665 -0.00950 0.00873 -0.00097 N1 3 0.121351 0.364369 -0.056311 11.00000 0.02406 0.03242 = 0.02489 0.00145 0.00158 0.00183 C1 1 -0.222432 0.123411 -0.249915 11.00000 0.03208 0.02879 = 0.02362 0.00263 -0.00136 -0.00510 C2 1 -0.062734 0.374318 -0.081917 11.00000 0.02568 0.02648 = 0.02503 0.00407 -0.00061 -0.00139 C3 1 -0.117734 0.282985 -0.139027 11.00000 0.02452 0.02417 = 0.02681 0.00636 0.00004 0.00172 C4 1 0.155659 0.463823 -0.001186 11.00000 0.03162 0.02361 = 0.02514 0.00053 -0.00272 0.00117 C5 1 -0.000609 0.479244 0.045322 11.00000 0.02664 0.03029 = 0.02720 0.00319 -0.00067 0.00082 C6 1 0.047994 0.584669 0.096945 11.00000 0.03239 0.03110 = 0.02160 -0.00158 0.00228 -0.00141 C7 1 -0.019679 0.096136 -0.225281 11.00000 0.02699 0.02853 = 0.02567 0.00414 0.00318 -0.00016 C8 1 0.032403 0.178440 -0.169805 11.00000 0.02287 0.02757 = 0.02315 0.00085 0.00388 0.00021 C9 1 0.247424 0.666413 0.102079 11.00000 0.03360 0.02764 = 0.02864 -0.00282 -0.01137 0.00117 C10 1 -0.322984 0.304818 -0.165534 11.00000 0.02651 0.02838 = 0.02441 -0.00108 -0.00176 -0.00071 C11 1 -0.377092 0.224874 -0.221800 11.00000 0.02621 0.03360 = 0.02683 -0.00172 -0.00006 -0.00189 C12 1 0.401359 0.646269 0.057744 11.00000 0.03518 0.02828 = 0.03241 0.00248 -0.00732 0.00245 C13 1 0.357461 0.542473 0.005708 11.00000 0.02058 0.03260 = 0.03623 0.00441 -0.00166 0.00363 HKLF 4 Covalent radii and connectivity table for 2010sl0005a C 0.770 H 0.320 N 0.700 F 0.640 F1 - C9 F2 - C1 F3 - C6 N1 - C2 C4 C1 - F2 C11 C7 C2 - N1 C3 C3 - C8 C10 C2 C4 - C5 C13 N1 C5 - C4 C6 C6 - F3 C9 C5 C7 - C1 C8 C8 - C7 C3 C9 - F1 C12 C6 C10 - C11 C3 C11 - C1 C10 C12 - C9 C13 C13 - C4 C12 13164 Reflections read, of which 1550 rejected -7 =< h =< 7, -8 =< k =< 9, -21 =< l =< 25, Max. 2-theta = 49.96 0 Systematic absence violations 0 Inconsistent equivalents 1816 Unique reflections, of which 0 suppressed R(int) = 0.0556 R(sigma) = 0.0396 Friedel opposites not merged Maximum memory for data reduction = 1449 / 18302 Default effective X-H distances for T = 23.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 0.98 0.97 0.96 0.93 0.86 0.89 1.10 0.82 0.93 0.86 0.93 Note that these distances are chosen to give the best fit to the X-ray data and so avoid the introduction of systematic error. The true internuclear distances are longer and do not vary with temperature ! The apparent variation with temperature is caused by libration. ** Cell contents from UNIT instruction and atom list do not agree ** Unit-cell contents from UNIT instruction and atom list resp. C 52.00 52.00 H 0.00 32.00 N 4.00 4.00 F 12.00 12.00 Least-squares cycle 1 Maximum vector length = 511 Memory required = 1852 / 192626 wR2 = 0.1785 before cycle 1 for 1816 data and 154 / 154 parameters GooF = S = 0.902; Restrained GooF = 0.902 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1465 * P )^2 + 0.70 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24131 0.00123 2.635 OSF Mean shift/su = 0.775 Maximum = 2.873 for U22 F2 Max. shift = 0.013 A for H5 Max. dU = 0.002 for F2 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1852 / 192626 wR2 = 0.1669 before cycle 2 for 1816 data and 154 / 154 parameters GooF = S = 0.844; Restrained GooF = 0.844 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1465 * P )^2 + 0.70 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24225 0.00116 0.815 OSF Mean shift/su = 0.273 Maximum = 1.130 for U22 F2 Max. shift = 0.004 A for H5 Max. dU = 0.001 for F2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1852 / 192626 wR2 = 0.1656 before cycle 3 for 1816 data and 154 / 154 parameters GooF = S = 0.837; Restrained GooF = 0.837 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1465 * P )^2 + 0.70 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24232 0.00115 0.061 OSF Mean shift/su = 0.038 Maximum = 0.213 for U11 C7 Max. shift = 0.001 A for H11 Max. dU = 0.000 for C10 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1852 / 192626 wR2 = 0.1656 before cycle 4 for 1816 data and 154 / 154 parameters GooF = S = 0.836; Restrained GooF = 0.836 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1465 * P )^2 + 0.70 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24234 0.00115 0.012 OSF Mean shift/su = 0.015 Maximum = -0.110 for U11 F3 Max. shift = 0.000 A for C4 Max. dU = 0.000 for F3 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1852 / 192626 wR2 = 0.1656 before cycle 5 for 1816 data and 154 / 154 parameters GooF = S = 0.836; Restrained GooF = 0.836 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1465 * P )^2 + 0.70 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24234 0.00115 0.002 OSF Mean shift/su = 0.005 Maximum = 0.026 for U11 C7 Max. shift = 0.000 A for C6 Max. dU = 0.000 for C7 Least-squares cycle 6 Maximum vector length = 511 Memory required = 1852 / 192626 wR2 = 0.1655 before cycle 6 for 1816 data and 154 / 154 parameters GooF = S = 0.836; Restrained GooF = 0.836 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1465 * P )^2 + 0.70 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24234 0.00115 0.002 OSF Mean shift/su = 0.002 Maximum = 0.012 for U11 C9 Max. shift = 0.000 A for C12 Max. dU = 0.000 for C9 Least-squares cycle 7 Maximum vector length = 511 Memory required = 1852 / 192626 wR2 = 0.1655 before cycle 7 for 1816 data and 154 / 154 parameters GooF = S = 0.836; Restrained GooF = 0.836 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1465 * P )^2 + 0.70 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24234 0.00115 0.000 OSF Mean shift/su = 0.001 Maximum = 0.006 for U11 C9 Max. shift = 0.000 A for C12 Max. dU = 0.000 for C9 Least-squares cycle 8 Maximum vector length = 511 Memory required = 1852 / 192626 wR2 = 0.1655 before cycle 8 for 1816 data and 154 / 154 parameters GooF = S = 0.836; Restrained GooF = 0.836 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1465 * P )^2 + 0.70 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24234 0.00115 0.000 OSF Mean shift/su = 0.000 Maximum = 0.003 for U11 C9 Max. shift = 0.000 A for C12 Max. dU = 0.000 for C9 Least-squares cycle 9 Maximum vector length = 511 Memory required = 1852 / 192626 wR2 = 0.1655 before cycle 9 for 1816 data and 154 / 154 parameters GooF = S = 0.836; Restrained GooF = 0.836 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1465 * P )^2 + 0.70 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24234 0.00115 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for U11 C9 Max. shift = 0.000 A for C12 Max. dU = 0.000 for C9 Least-squares cycle 10 Maximum vector length = 511 Memory required = 1852 / 192626 wR2 = 0.1655 before cycle 10 for 1816 data and 154 / 154 parameters GooF = S = 0.836; Restrained GooF = 0.836 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1465 * P )^2 + 0.70 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24234 0.00115 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for U11 C3 Max. shift = 0.000 A for C12 Max. dU = 0.000 for C12 Least-squares cycle 11 Maximum vector length = 511 Memory required = 1852 / 192626 wR2 = 0.1655 before cycle 11 for 1816 data and 154 / 154 parameters GooF = S = 0.836; Restrained GooF = 0.836 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1465 * P )^2 + 0.70 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24234 0.00115 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for U11 C9 Max. shift = 0.000 A for H12 Max. dU = 0.000 for C9 Least-squares cycle 12 Maximum vector length = 511 Memory required = 1852 / 192626 wR2 = 0.1655 before cycle 12 for 1816 data and 154 / 154 parameters GooF = S = 0.836; Restrained GooF = 0.836 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1465 * P )^2 + 0.70 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24234 0.00115 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for U11 C3 Max. shift = 0.000 A for H8 Max. dU = 0.000 for C3 Least-squares cycle 13 Maximum vector length = 511 Memory required = 1852 / 192626 wR2 = 0.1655 before cycle 13 for 1816 data and 154 / 154 parameters GooF = S = 0.836; Restrained GooF = 0.836 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1465 * P )^2 + 0.70 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24234 0.00115 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z F1 Max. shift = 0.000 A for H12 Max. dU = 0.000 for C8 Least-squares cycle 14 Maximum vector length = 511 Memory required = 1852 / 192626 wR2 = 0.1655 before cycle 14 for 1816 data and 154 / 154 parameters GooF = S = 0.836; Restrained GooF = 0.836 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1465 * P )^2 + 0.70 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24234 0.00115 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z C8 Max. shift = 0.000 A for C8 Max. dU = 0.000 for N1 Least-squares cycle 15 Maximum vector length = 511 Memory required = 1852 / 192626 wR2 = 0.1655 before cycle 15 for 1816 data and 154 / 154 parameters GooF = S = 0.836; Restrained GooF = 0.836 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1465 * P )^2 + 0.70 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24234 0.00115 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z F1 Max. shift = 0.000 A for C4 Max. dU = 0.000 for C9 Least-squares cycle 16 Maximum vector length = 511 Memory required = 1852 / 192626 wR2 = 0.1655 before cycle 16 for 1816 data and 154 / 154 parameters GooF = S = 0.836; Restrained GooF = 0.836 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1465 * P )^2 + 0.70 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24234 0.00115 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z F1 Max. shift = 0.000 A for C13 Max. dU = 0.000 for C8 Least-squares cycle 17 Maximum vector length = 511 Memory required = 1852 / 192626 wR2 = 0.1655 before cycle 17 for 1816 data and 154 / 154 parameters GooF = S = 0.836; Restrained GooF = 0.836 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1465 * P )^2 + 0.70 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24234 0.00115 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C13 Max. dU = 0.000 for F3 Least-squares cycle 18 Maximum vector length = 511 Memory required = 1852 / 192626 wR2 = 0.1655 before cycle 18 for 1816 data and 154 / 154 parameters GooF = S = 0.836; Restrained GooF = 0.836 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1465 * P )^2 + 0.70 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24234 0.00115 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z F1 Max. shift = 0.000 A for C5 Max. dU = 0.000 for C6 Least-squares cycle 19 Maximum vector length = 511 Memory required = 1852 / 192626 wR2 = 0.1655 before cycle 19 for 1816 data and 154 / 154 parameters GooF = S = 0.836; Restrained GooF = 0.836 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1465 * P )^2 + 0.70 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24234 0.00115 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z F1 Max. shift = 0.000 A for F2 Max. dU = 0.000 for F3 Least-squares cycle 20 Maximum vector length = 511 Memory required = 1852 / 192626 wR2 = 0.1655 before cycle 20 for 1816 data and 154 / 154 parameters GooF = S = 0.836; Restrained GooF = 0.836 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1465 * P )^2 + 0.70 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24234 0.00115 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z F1 Max. shift = 0.000 A for C5 Max. dU = 0.000 for C13 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 21 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 -0.1668 0.4415 -0.0634 43 0.930 0.000 C2 N1 C3 H5 -0.1309 0.4243 0.0427 43 0.930 0.000 C5 C4 C6 H7 0.0788 0.0254 -0.2453 43 0.930 0.000 C7 C1 C8 H8 0.1697 0.1636 -0.1526 43 0.930 0.000 C8 C7 C3 H10 -0.4232 0.3725 -0.1453 43 0.930 0.000 C10 C11 C3 H11 -0.5106 0.2397 -0.2395 43 0.930 0.000 C11 C1 C10 H12 0.5341 0.6992 0.0619 43 0.930 0.000 C12 C9 C13 H13 0.4622 0.5265 -0.0246 43 0.930 0.000 C13 C4 C12 2010sl0005a ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq F1 0.28257 0.76389 0.15349 1.00000 0.05011 0.03477 0.03788 -0.01056 -0.01110 -0.00414 0.04092 0.00323 0.00037 0.00026 0.00009 0.00000 0.00131 0.00111 0.00114 0.00090 0.00093 0.00094 0.00058 F2 -0.27097 0.04683 -0.30505 1.00000 0.03765 0.04259 0.03416 -0.00977 -0.00446 -0.00407 0.03813 0.00329 0.00034 0.00027 0.00009 0.00000 0.00116 0.00122 0.00103 0.00092 0.00090 0.00091 0.00056 F3 -0.09626 0.60502 0.14222 1.00000 0.04559 0.05324 0.03776 -0.00809 0.00891 -0.00369 0.04553 0.00362 0.00035 0.00029 0.00009 0.00000 0.00124 0.00128 0.00115 0.00105 0.00097 0.00113 0.00061 N1 0.12176 0.36420 -0.05614 1.00000 0.02360 0.03206 0.02644 0.00054 0.00082 0.00099 0.02736 0.00472 0.00042 0.00037 0.00012 0.00000 0.00135 0.00138 0.00132 0.00118 0.00111 0.00125 0.00062 C1 -0.22243 0.12371 -0.25005 1.00000 0.03374 0.02773 0.02439 0.00020 -0.00010 -0.00650 0.02862 0.00551 0.00054 0.00043 0.00015 0.00000 0.00166 0.00162 0.00152 0.00141 0.00137 0.00142 0.00071 C2 -0.06198 0.37319 -0.08207 1.00000 0.02587 0.02551 0.02783 0.00206 0.00313 0.00177 0.02640 0.00562 0.00052 0.00041 0.00014 0.00000 0.00159 0.00154 0.00163 0.00136 0.00131 0.00135 0.00071 H2 -0.16684 0.44148 -0.06343 1.00000 0.03168 0.00000 0.00000 C3 -0.11730 0.28284 -0.13916 1.00000 0.02468 0.02338 0.02801 0.00530 0.00045 -0.00069 0.02536 0.00545 0.00049 0.00038 0.00015 0.00000 0.00157 0.00150 0.00155 0.00131 0.00132 0.00137 0.00069 C4 0.15621 0.46329 -0.00100 1.00000 0.03128 0.02485 0.02606 0.00206 -0.00179 0.00345 0.02739 0.00578 0.00055 0.00042 0.00014 0.00000 0.00179 0.00153 0.00163 0.00135 0.00131 0.00134 0.00072 C5 0.00080 0.48074 0.04569 1.00000 0.02864 0.03091 0.02885 0.00422 -0.00187 -0.00344 0.02947 0.00575 0.00055 0.00041 0.00015 0.00000 0.00173 0.00172 0.00166 0.00132 0.00136 0.00146 0.00076 H5 -0.13089 0.42432 0.04268 1.00000 0.03536 0.00000 0.00000 C6 0.04754 0.58442 0.09677 1.00000 0.03592 0.03052 0.02188 -0.00054 0.00100 0.00070 0.02944 0.00555 0.00056 0.00042 0.00014 0.00000 0.00178 0.00176 0.00154 0.00130 0.00141 0.00142 0.00076 C7 -0.01974 0.09668 -0.22522 1.00000 0.02930 0.02822 0.02721 0.00124 0.00358 0.00125 0.02824 0.00553 0.00055 0.00042 0.00014 0.00000 0.00173 0.00165 0.00157 0.00133 0.00130 0.00141 0.00074 H7 0.07879 0.02544 -0.24526 1.00000 0.03389 0.00000 0.00000 C8 0.03321 0.17834 -0.16968 1.00000 0.02339 0.03085 0.02565 0.00118 0.00064 0.00138 0.02663 0.00553 0.00052 0.00041 0.00014 0.00000 0.00152 0.00167 0.00158 0.00138 0.00130 0.00127 0.00071 H8 0.16973 0.16359 -0.15259 1.00000 0.03196 0.00000 0.00000 C9 0.24661 0.66617 0.10244 1.00000 0.03744 0.02666 0.02995 -0.00272 -0.01072 0.00009 0.03135 0.00559 0.00060 0.00043 0.00015 0.00000 0.00183 0.00169 0.00168 0.00132 0.00150 0.00143 0.00077 C10 -0.32184 0.30426 -0.16556 1.00000 0.02574 0.02823 0.02660 -0.00237 0.00093 0.00284 0.02686 0.00555 0.00050 0.00043 0.00015 0.00000 0.00164 0.00165 0.00151 0.00136 0.00129 0.00129 0.00072 H10 -0.42325 0.37245 -0.14533 1.00000 0.03223 0.00000 0.00000 C11 -0.37524 0.22478 -0.22169 1.00000 0.02231 0.03661 0.02912 0.00028 -0.00261 -0.00147 0.02935 0.00564 0.00054 0.00043 0.00015 0.00000 0.00149 0.00181 0.00159 0.00144 0.00125 0.00148 0.00074 H11 -0.51062 0.23965 -0.23952 1.00000 0.03522 0.00000 0.00000 C12 0.40100 0.64549 0.05780 1.00000 0.02983 0.03069 0.03598 0.00396 -0.00749 -0.00113 0.03217 0.00584 0.00057 0.00042 0.00016 0.00000 0.00175 0.00166 0.00179 0.00149 0.00143 0.00151 0.00079 H12 0.53411 0.69924 0.06186 1.00000 0.03860 0.00000 0.00000 C13 0.35686 0.54248 0.00581 1.00000 0.02244 0.03357 0.03439 0.00287 0.00131 0.00378 0.03014 0.00595 0.00053 0.00044 0.00016 0.00000 0.00165 0.00172 0.00170 0.00153 0.00136 0.00138 0.00075 H13 0.46219 0.52651 -0.02456 1.00000 0.03616 0.00000 0.00000 Final Structure Factor Calculation for 2010sl0005a Total number of l.s. parameters = 154 Maximum vector length = 511 Memory required = 1700 / 25046 wR2 = 0.1655 before cycle 21 for 1816 data and 2 / 154 parameters GooF = S = 0.836; Restrained GooF = 0.836 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1465 * P )^2 + 0.70 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0551 for 1540 Fo > 4sig(Fo) and 0.0658 for all 1816 data wR2 = 0.1655, GooF = S = 0.836, Restrained GooF = 0.836 for all data Flack x parameter = -0.1489 with su 1.2974 Expected values are 0 (within 3 su'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 Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 17.00 for non-hydrogen and 8.00 for hydrogen atoms Principal mean square atomic displacements U 0.0569 0.0442 0.0217 F1 0.0491 0.0404 0.0249 F2 0.0603 0.0454 0.0308 F3 0.0322 0.0265 0.0233 N1 0.0379 0.0244 0.0236 C1 0.0314 0.0243 0.0235 C2 0.0315 0.0248 0.0198 C3 0.0329 0.0275 0.0217 C4 0.0362 0.0269 0.0253 C5 0.0361 0.0305 0.0218 C6 0.0327 0.0275 0.0245 C7 0.0314 0.0254 0.0231 C8 0.0452 0.0274 0.0214 C9 0.0307 0.0272 0.0227 C10 0.0368 0.0299 0.0213 C11 0.0423 0.0297 0.0245 C12 0.0377 0.0314 0.0213 C13 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.016 0.026 0.037 0.046 0.058 0.072 0.089 0.115 0.155 1.000 Number in group 186. 179. 182. 183. 178. 191. 180. 177. 178. 182. GooF 0.847 0.888 0.984 0.857 0.850 0.754 0.839 0.628 0.774 0.891 K 1.027 0.916 0.904 0.952 1.003 0.997 1.023 1.037 1.067 0.970 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.06 1.14 1.25 1.43 1.81 inf Number in group 189. 183. 176. 180. 181. 180. 181. 182. 182. 182. GooF 0.869 0.787 0.751 0.702 0.786 0.688 0.665 0.760 0.838 1.318 K 0.966 0.989 1.018 1.024 1.075 1.066 1.062 1.047 1.046 0.936 R1 0.145 0.125 0.086 0.070 0.062 0.051 0.048 0.048 0.046 0.060 ** Extinction (EXTI) or solvent water (SWAT) correction may be required ** Recommended weighting scheme: WGHT 0.0985 0.3335 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) 0 1 2 262.56 906.22 7.47 0.223 6.29 0 2 9 43.21 17.76 5.12 0.031 2.03 0 2 0 69.63 35.71 4.38 0.044 3.89 0 2 5 69.10 127.99 3.99 0.084 2.88 1 2 0 6.32 18.39 3.91 0.032 3.30 1 0 10 15.78 5.22 3.87 0.017 2.02 1 0 4 52.10 94.81 3.75 0.072 4.05 0 1 11 180.05 113.31 3.63 0.079 1.89 1 0 3 66.00 39.34 3.53 0.046 4.68 2 0 1 330.49 522.29 3.44 0.169 3.07 3 3 0 47.70 27.43 3.42 0.039 1.62 0 4 3 4.16 0.17 3.37 0.003 1.88 4 3 0 9.60 2.24 3.32 0.011 1.33 0 1 8 39.20 66.46 3.18 0.060 2.53 3 7 3 -3.55 5.38 3.16 0.017 0.97 2 0 8 177.02 121.68 2.99 0.082 2.03 0 0 6 485.18 713.06 2.94 0.197 3.57 0 3 1 50.57 81.21 2.90 0.067 2.57 4 1 0 279.88 197.56 2.88 0.104 1.52 -6 5 5 3.73 15.62 2.84 0.029 0.84 3 0 4 4.59 11.71 2.79 0.025 1.93 1 8 11 -7.15 12.44 2.79 0.026 0.86 6 3 5 20.97 9.33 2.73 0.023 0.94 -2 2 7 511.43 371.73 2.72 0.143 1.90 3 1 3 194.31 139.32 2.67 0.087 1.93 -1 3 13 25.72 41.30 2.61 0.048 1.36 -4 1 21 3.95 18.97 2.56 0.032 0.85 -5 3 6 17.79 7.84 2.56 0.021 1.07 4 2 20 1.54 12.53 2.55 0.026 0.86 0 3 10 7.88 15.29 2.53 0.029 1.65 2 2 7 497.07 370.74 2.47 0.142 1.90 0 0 4 188.11 262.79 2.46 0.120 5.35 4 1 6 17.38 28.98 2.46 0.040 1.40 -1 4 21 11.16 23.50 2.46 0.036 0.89 -4 3 14 13.09 5.11 2.43 0.017 1.00 1 5 0 89.56 63.67 2.43 0.059 1.51 -2 8 7 3.89 14.43 2.41 0.028 0.89 3 0 10 11.23 5.39 2.40 0.017 1.49 4 0 5 13.80 23.85 2.38 0.036 1.46 4 0 0 5.08 0.18 2.37 0.003 1.55 0 4 14 95.33 68.13 2.36 0.061 1.20 1 2 10 5.45 11.43 2.34 0.025 1.79 -1 5 17 12.62 24.52 2.33 0.037 0.97 -7 2 1 67.00 43.94 2.32 0.049 0.86 -6 2 11 -2.76 4.35 2.29 0.015 0.89 0 1 6 296.31 399.28 2.28 0.148 3.24 -2 4 18 -0.36 6.71 2.27 0.019 0.96 3 7 4 0.81 7.49 2.27 0.020 0.96 -3 4 2 33.45 22.23 2.27 0.035 1.40 -4 5 9 23.42 37.12 2.24 0.045 1.00 Bond lengths and angles F1 - Distance Angles C9 1.3493 (0.0036) F1 - F2 - Distance Angles C1 1.3540 (0.0037) F2 - F3 - Distance Angles C6 1.3295 (0.0038) F3 - N1 - Distance Angles C2 1.2701 (0.0041) C4 1.4253 (0.0041) 117.81 (0.28) N1 - C2 C1 - Distance Angles F2 1.3540 (0.0037) C11 1.3733 (0.0049) 118.90 (0.29) C7 1.3817 (0.0049) 118.00 (0.29) 123.10 (0.31) C1 - F2 C11 C2 - Distance Angles N1 1.2701 (0.0041) C3 1.4503 (0.0043) 123.62 (0.29) H2 0.9300 118.19 118.19 C2 - N1 C3 C3 - Distance Angles C8 1.4000 (0.0043) C10 1.3994 (0.0044) 119.09 (0.29) C2 1.4503 (0.0043) 121.08 (0.29) 119.79 (0.28) C3 - C8 C10 C4 - Distance Angles C5 1.3953 (0.0046) C13 1.3970 (0.0047) 119.91 (0.29) N1 1.4253 (0.0041) 122.78 (0.30) 117.30 (0.28) C4 - C5 C13 C5 - Distance Angles C4 1.3953 (0.0046) C6 1.3889 (0.0045) 118.39 (0.32) H5 0.9300 120.81 120.81 C5 - C4 C6 C6 - Distance Angles F3 1.3295 (0.0038) C9 1.3949 (0.0051) 118.43 (0.28) C5 1.3889 (0.0045) 120.35 (0.30) 121.21 (0.32) C6 - F3 C9 C7 - Distance Angles C1 1.3817 (0.0049) C8 1.3868 (0.0044) 118.39 (0.32) H7 0.9300 120.81 120.81 C7 - C1 C8 C8 - Distance Angles C7 1.3868 (0.0044) C3 1.4000 (0.0043) 120.50 (0.31) H8 0.9300 119.75 119.75 C8 - C7 C3 C9 - Distance Angles F1 1.3493 (0.0036) C12 1.3625 (0.0051) 121.17 (0.30) C6 1.3949 (0.0051) 118.28 (0.31) 120.54 (0.29) C9 - F1 C12 C10 - Distance Angles C11 1.3908 (0.0047) C3 1.3994 (0.0044) 120.78 (0.30) H10 0.9300 119.61 119.61 C10 - C11 C3 C11 - Distance Angles C1 1.3733 (0.0049) C10 1.3908 (0.0047) 118.13 (0.31) H11 0.9300 120.94 120.94 C11 - C1 C10 C12 - Distance Angles C9 1.3625 (0.0051) C13 1.3979 (0.0048) 119.18 (0.33) H12 0.9300 120.41 120.41 C12 - C9 C13 C13 - Distance Angles C4 1.3970 (0.0047) C12 1.3979 (0.0048) 120.70 (0.31) H13 0.9300 119.65 119.65 C13 - C4 C12 FMAP and GRID set by program FMAP 2 3 24 GRID -1.190 -2 -2 1.190 2 2 R1 = 0.0647 for 1089 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.70 at 0.5696 0.7162 0.0742 [ 0.37 A from H12 ] Deepest hole -0.37 at 0.8948 0.5572 0.1657 [ 0.63 A from F3 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 1623 / 13638 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5696 0.7162 0.0742 1.00000 0.05 0.70 0.37 H12 1.23 C12 2.13 C9 2.39 C13 Q2 1 0.6187 0.8338 0.0953 1.00000 0.05 0.23 1.37 H12 2.15 C12 2.49 F1 2.50 N1 Q3 1 -0.0442 0.4951 -0.1431 1.00000 0.05 0.22 1.62 C2 1.71 C3 1.91 H2 2.17 F1 Q4 1 -0.5988 0.2394 -0.2488 1.00000 0.05 0.21 0.58 H11 1.51 C11 2.38 F1 2.50 C1 Q5 1 -0.1624 0.0975 -0.3587 1.00000 0.05 0.19 1.39 F2 2.36 C1 2.45 H12 2.57 C2 Q6 1 -0.5455 0.1076 -0.2308 1.00000 0.05 0.19 1.07 H11 1.41 C11 2.05 C1 2.38 F2 Q7 1 -0.3765 0.5001 -0.0858 1.00000 0.05 0.19 1.46 H2 1.64 H10 1.66 H13 2.19 C2 Q8 1 0.2122 0.9557 0.1433 1.00000 0.05 0.18 1.57 F1 1.58 H10 1.94 C10 2.03 H2 Q9 1 -0.2826 0.4592 -0.0025 1.00000 0.05 0.18 1.38 H5 1.50 H2 1.73 H13 2.04 C5 Q10 1 -0.1986 0.3383 -0.0085 1.00000 0.05 0.18 1.35 H5 1.44 H2 1.81 C2 2.03 C5 Q11 1 -0.8168 0.2766 -0.2514 1.00000 0.05 0.17 1.94 H11 1.96 C7 2.06 H7 2.07 F1 Q12 1 -0.1029 0.3086 -0.2596 1.00000 0.05 0.17 1.63 C1 1.70 H7 1.88 C7 1.99 C11 Q13 1 -0.1377 -0.0470 -0.3537 1.00000 0.05 0.17 1.52 F2 1.95 C2 2.05 N1 2.07 C3 Q14 1 -0.5090 0.3448 -0.2628 1.00000 0.05 0.17 0.96 H11 1.53 C11 2.17 F3 2.40 C10 Q15 1 0.5974 0.7469 0.1440 1.00000 0.05 0.17 1.84 H12 1.97 F1 2.20 F3 2.22 F2 Q16 1 0.3866 0.9131 0.1509 1.00000 0.05 0.17 1.33 F1 2.21 H2 2.24 C2 2.28 H7 Q17 1 -0.5547 0.3819 -0.2334 1.00000 0.05 0.17 1.15 H11 1.67 C11 1.87 F2 2.05 H10 Q18 1 -0.2832 -0.0544 -0.3592 1.00000 0.05 0.17 1.40 F2 1.91 H10 2.17 N1 2.32 H8 Q19 1 -0.4329 0.3933 -0.0762 1.00000 0.05 0.16 1.49 H10 1.65 H13 1.72 H2 2.15 C10 Q20 1 0.4175 0.5916 -0.0627 1.00000 0.05 0.16 1.00 H13 1.56 C13 2.32 C4 2.55 N1 Shortest distances between peaks (including symmetry equivalents) 14 17 0.75 3 16 0.85 13 18 0.91 7 19 0.92 4 14 1.03 1 2 1.06 9 10 1.08 5 13 1.14 8 16 1.14 4 6 1.14 2 5 1.15 3 13 1.18 4 17 1.19 2 15 1.25 5 15 1.28 4 11 1.38 7 8 1.39 5 18 1.40 3 5 1.51 1 15 1.52 7 20 1.54 3 8 1.56 5 16 1.73 11 12 1.80 19 20 1.82 15 16 1.85 11 17 1.86 13 16 1.88 7 9 1.90 9 19 1.90 2 3 1.96 2 16 1.97 6 14 1.98 2 13 1.99 11 14 2.00 6 17 2.01 8 19 2.06 2 20 2.06 3 18 2.07 6 14 2.08 10 19 2.10 12 15 2.11 1 5 2.12 6 17 2.14 6 11 2.18 18 20 2.19 3 15 2.19 2 18 2.22 7 16 2.25 17 18 2.27 18 19 2.28 5 20 2.31 13 15 2.35 7 10 2.35 3 7 2.40 7 18 2.45 9 20 2.49 1 16 2.52 12 14 2.54 8 20 2.54 11 16 2.60 1 20 2.64 11 13 2.65 15 18 2.66 16 18 2.70 5 12 2.71 13 20 2.72 13 17 2.72 8 13 2.74 1 9 2.74 8 18 2.77 11 18 2.78 1 3 2.78 5 8 2.82 8 17 2.84 11 15 2.84 4 8 2.85 2 8 2.88 8 15 2.89 12 16 2.91 4 18 2.91 3 12 2.91 3 19 2.91 12 17 2.92 15 20 2.92 6 8 2.93 16 19 2.96 8 11 2.96 4 17 2.96 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. 0.55: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.05: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.67: Structure factors and derivatives 1.38: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.33: Solve l.s. equations 0.00: Generate HTAB table 0.06: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2010sl0005a finished at 08:07:16 Total CPU time: 4.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++