+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2010sl0006a started at 22:04:14 on 29-Mar-2011 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2010sl0006a CELL 0.71073 6.4649 7.6187 21.2897 90.000 90.000 90.000 ZERR 4.00 0.0004 0.0004 0.0013 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 16 V = 1048.61 F(000) = 484.0 Mu = 0.14 mm-1 Cell Wt = 984.56 Rho = 1.559 MERG 2 OMIT -3.00 50.00 SHEL 7 0.77 OMIT 0 1 3 PLAN 20 SIZE 0.1 0.08 0.08 BOND $H WGHT 0.13760 3.79290 L.S. 20 TEMP 20 ACTA FVAR 0.22981 ANIS F1 4 0.748778 0.729873 0.152809 11.00000 0.02533 F2 4 1.270841 1.477271 -0.305398 11.00000 0.02533 F3 4 1.118928 0.879287 0.139571 11.00000 0.02533 F4 4 0.523572 0.990408 -0.033063 11.00000 0.02533 N1 3 0.896967 1.146315 -0.055414 11.00000 0.02533 C1 1 0.978043 0.908476 0.096633 11.00000 0.02533 C2 1 1.122593 1.229858 -0.140407 11.00000 0.02533 C3 1 0.869140 1.043540 -0.001453 11.00000 0.02533 C4 1 1.064125 1.135746 -0.082847 11.00000 0.02533 AFIX 43 H4 2 1.162667 1.061177 -0.065507 11.00000 -1.20000 AFIX 0 C5 1 1.225028 1.397610 -0.250595 11.00000 0.02533 C6 1 0.778362 0.831532 0.104662 11.00000 0.02533 C7 1 1.022040 1.011825 0.045008 11.00000 0.02533 AFIX 43 H7 2 1.152923 1.061009 0.040670 11.00000 -1.20000 AFIX 0 C8 1 1.316766 1.215128 -0.166910 11.00000 0.02533 AFIX 43 H8 2 1.415769 1.146889 -0.146709 11.00000 -1.20000 AFIX 0 C9 1 0.667632 0.969169 0.007261 11.00000 0.02533 C10 1 0.631078 0.856662 0.060329 11.00000 0.02533 AFIX 43 H10 2 0.504197 0.800210 0.064278 11.00000 -1.20000 AFIX 0 C11 1 1.367034 1.294669 -0.220046 11.00000 0.02533 AFIX 43 H11 2 1.498997 1.280704 -0.236703 11.00000 -1.20000 AFIX 0 C12 1 0.978594 1.333436 -0.171393 11.00000 0.02533 AFIX 43 H12 2 0.846098 1.343981 -0.154804 11.00000 -1.20000 AFIX 0 C13 1 1.025403 1.418873 -0.224696 11.00000 0.02533 AFIX 43 H13 2 0.928319 1.490632 -0.244181 11.00000 -1.20000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 2010sl0006a C 0.770 H 0.320 N 0.700 F 0.640 F1 - C6 F2 - C5 F3 - C1 F4 - C9 N1 - C4 C3 C1 - F3 C7 C6 C2 - C8 C12 C4 C3 - N1 C7 C9 C4 - N1 C2 C5 - F2 C11 C13 C6 - F1 C10 C1 C7 - C1 C3 C8 - C11 C2 C9 - F4 C3 C10 C10 - C6 C9 C11 - C8 C5 C12 - C13 C2 C13 - C12 C5 10253 Reflections read, of which 1261 rejected -7 =< h =< 7, -8 =< k =< 9, -25 =< l =< 24, Max. 2-theta = 49.95 0 Systematic absence violations 0 Inconsistent equivalents 1831 Unique reflections, of which 0 suppressed R(int) = 0.1050 R(sigma) = 0.0869 Friedel opposites not merged Maximum memory for data reduction = 1456 / 18421 Default effective X-H distances for T = 20.0 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 28.00 N 4.00 4.00 F 16.00 16.00 Least-squares cycle 1 Maximum vector length = 511 Memory required = 1874 / 203273 wR2 = 0.2851 before cycle 1 for 1831 data and 163 / 163 parameters GooF = S = 1.184; Restrained GooF = 1.184 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1376 * P )^2 + 3.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.23818 0.00176 4.766 OSF 4 0.15358 0.00019 3.995 z F1 5 0.03748 0.00232 5.233 U11 F1 6 0.03193 0.00219 3.019 U22 F1 8 0.00614 0.00189 3.244 U23 F1 14 0.03701 0.00234 4.983 U11 F2 15 0.03550 0.00224 4.550 U22 F2 17 0.00773 0.00188 4.110 U23 F2 20 1.12154 0.00070 3.756 x F3 23 0.03470 0.00230 4.084 U11 F3 24 0.03914 0.00221 6.248 U22 F3 26 0.00722 0.00200 3.610 U23 F3 27 -0.00650 0.00197 -3.295 U13 F3 31 -0.03382 0.00021 -3.542 z F4 33 0.03942 0.00231 6.104 U22 F4 34 0.03549 0.00228 4.459 U33 F4 92 0.78213 0.00124 3.046 x C6 94 0.10322 0.00038 -3.804 z C6 119 0.67264 0.00122 4.102 x C9 121 0.00889 0.00037 4.365 z C9 139 -0.22151 0.00037 -3.971 z C11 157 -0.22609 0.00037 -3.787 z C13 Mean shift/su = 1.313 Maximum = 6.248 for U22 F3 Max. shift = 0.050 A for C9 Max. dU = 0.009 for F2 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1874 / 203273 wR2 = 0.1840 before cycle 2 for 1831 data and 163 / 163 parameters GooF = S = 0.721; Restrained GooF = 0.721 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1376 * P )^2 + 3.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24420 0.00115 5.217 OSF 14 0.04237 0.00165 3.243 U11 F2 15 0.04204 0.00159 4.108 U22 F2 17 0.01218 0.00130 3.431 U23 F2 24 0.04716 0.00159 5.028 U22 F3 33 0.04710 0.00170 4.512 U22 F4 Mean shift/su = 0.798 Maximum = 5.217 for OSF Max. shift = 0.014 A for C9 Max. dU = 0.005 for F3 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1874 / 203273 wR2 = 0.1731 before cycle 3 for 1831 data and 163 / 163 parameters GooF = S = 0.670; Restrained GooF = 0.670 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1376 * P )^2 + 3.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24439 0.00111 0.170 OSF Mean shift/su = 0.124 Maximum = -0.791 for U13 C9 Max. shift = 0.002 A for C12 Max. dU = 0.001 for C7 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1874 / 203273 wR2 = 0.1728 before cycle 4 for 1831 data and 163 / 163 parameters GooF = S = 0.668; Restrained GooF = 0.668 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1376 * P )^2 + 3.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24441 0.00111 0.018 OSF Mean shift/su = 0.022 Maximum = 0.182 for U22 C6 Max. shift = 0.001 A for C4 Max. dU = 0.000 for C6 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1874 / 203273 wR2 = 0.1728 before cycle 5 for 1831 data and 163 / 163 parameters GooF = S = 0.668; Restrained GooF = 0.668 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1376 * P )^2 + 3.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24441 0.00111 0.005 OSF Mean shift/su = 0.006 Maximum = 0.031 for U23 C1 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C7 Least-squares cycle 6 Maximum vector length = 511 Memory required = 1874 / 203273 wR2 = 0.1728 before cycle 6 for 1831 data and 163 / 163 parameters GooF = S = 0.668; Restrained GooF = 0.668 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1376 * P )^2 + 3.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24441 0.00111 -0.002 OSF Mean shift/su = 0.001 Maximum = 0.012 for y C11 Max. shift = 0.000 A for C11 Max. dU = 0.000 for C6 Least-squares cycle 7 Maximum vector length = 511 Memory required = 1874 / 203273 wR2 = 0.1728 before cycle 7 for 1831 data and 163 / 163 parameters GooF = S = 0.668; Restrained GooF = 0.668 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1376 * P )^2 + 3.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24441 0.00111 0.000 OSF Mean shift/su = 0.000 Maximum = 0.002 for U23 C13 Max. shift = 0.000 A for C1 Max. dU = 0.000 for C7 Least-squares cycle 8 Maximum vector length = 511 Memory required = 1874 / 203273 wR2 = 0.1728 before cycle 8 for 1831 data and 163 / 163 parameters GooF = S = 0.668; Restrained GooF = 0.668 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1376 * P )^2 + 3.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24441 0.00111 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for y C11 Max. shift = 0.000 A for C11 Max. dU = 0.000 for C13 Least-squares cycle 9 Maximum vector length = 511 Memory required = 1874 / 203273 wR2 = 0.1728 before cycle 9 for 1831 data and 163 / 163 parameters GooF = S = 0.668; Restrained GooF = 0.668 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1376 * P )^2 + 3.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24441 0.00111 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y N1 Max. shift = 0.000 A for N1 Max. dU = 0.000 for N1 Least-squares cycle 10 Maximum vector length = 511 Memory required = 1874 / 203273 wR2 = 0.1728 before cycle 10 for 1831 data and 163 / 163 parameters GooF = S = 0.668; Restrained GooF = 0.668 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1376 * P )^2 + 3.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24441 0.00111 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y C11 Max. shift = 0.000 A for C11 Max. dU = 0.000 for F2 Least-squares cycle 11 Maximum vector length = 511 Memory required = 1874 / 203273 wR2 = 0.1728 before cycle 11 for 1831 data and 163 / 163 parameters GooF = S = 0.668; Restrained GooF = 0.668 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1376 * P )^2 + 3.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24441 0.00111 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H10 Max. dU = 0.000 for F2 Least-squares cycle 12 Maximum vector length = 511 Memory required = 1874 / 203273 wR2 = 0.1728 before cycle 12 for 1831 data and 163 / 163 parameters GooF = S = 0.668; Restrained GooF = 0.668 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1376 * P )^2 + 3.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24441 0.00111 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y N1 Max. shift = 0.000 A for C13 Max. dU = 0.000 for C2 Least-squares cycle 13 Maximum vector length = 511 Memory required = 1874 / 203273 wR2 = 0.1728 before cycle 13 for 1831 data and 163 / 163 parameters GooF = S = 0.668; Restrained GooF = 0.668 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1376 * P )^2 + 3.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24441 0.00111 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y N1 Max. shift = 0.000 A for C10 Max. dU = 0.000 for C7 Least-squares cycle 14 Maximum vector length = 511 Memory required = 1874 / 203273 wR2 = 0.1728 before cycle 14 for 1831 data and 163 / 163 parameters GooF = S = 0.668; Restrained GooF = 0.668 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1376 * P )^2 + 3.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24441 0.00111 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y N1 Max. shift = 0.000 A for C13 Max. dU = 0.000 for C8 Least-squares cycle 15 Maximum vector length = 511 Memory required = 1874 / 203273 wR2 = 0.1728 before cycle 15 for 1831 data and 163 / 163 parameters GooF = S = 0.668; Restrained GooF = 0.668 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1376 * P )^2 + 3.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24441 0.00111 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y N1 Max. shift = 0.000 A for C10 Max. dU = 0.000 for C10 Least-squares cycle 16 Maximum vector length = 511 Memory required = 1874 / 203273 wR2 = 0.1728 before cycle 16 for 1831 data and 163 / 163 parameters GooF = S = 0.668; Restrained GooF = 0.668 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1376 * P )^2 + 3.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24441 0.00111 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y N1 Max. shift = 0.000 A for C1 Max. dU = 0.000 for C5 Least-squares cycle 17 Maximum vector length = 511 Memory required = 1874 / 203273 wR2 = 0.1728 before cycle 17 for 1831 data and 163 / 163 parameters GooF = S = 0.668; Restrained GooF = 0.668 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1376 * P )^2 + 3.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24441 0.00111 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y N1 Max. shift = 0.000 A for C5 Max. dU = 0.000 for C11 Least-squares cycle 18 Maximum vector length = 511 Memory required = 1874 / 203273 wR2 = 0.1728 before cycle 18 for 1831 data and 163 / 163 parameters GooF = S = 0.668; Restrained GooF = 0.668 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1376 * P )^2 + 3.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24441 0.00111 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y N1 Max. shift = 0.000 A for C8 Max. dU = 0.000 for C11 Least-squares cycle 19 Maximum vector length = 511 Memory required = 1874 / 203273 wR2 = 0.1728 before cycle 19 for 1831 data and 163 / 163 parameters GooF = S = 0.668; Restrained GooF = 0.668 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1376 * P )^2 + 3.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24441 0.00111 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x F2 Max. shift = 0.000 A for C5 Max. dU = 0.000 for F2 Least-squares cycle 20 Maximum vector length = 511 Memory required = 1874 / 203273 wR2 = 0.1728 before cycle 20 for 1831 data and 163 / 163 parameters GooF = S = 0.668; Restrained GooF = 0.668 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1376 * P )^2 + 3.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24441 0.00111 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y N1 Max. shift = 0.000 A for C8 Max. dU = 0.000 for F1 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 H4 1.1684 1.0591 -0.0664 43 0.930 0.000 C4 N1 C2 H7 1.1491 1.0649 0.0408 43 0.930 0.000 C7 C1 C3 H8 1.4154 1.1427 -0.1458 43 0.930 0.000 C8 C11 C2 H10 0.4995 0.8083 0.0645 43 0.930 0.000 C10 C6 C9 H11 1.5017 1.2828 -0.2392 43 0.930 0.000 C11 C8 C5 H12 0.8428 1.3458 -0.1547 43 0.930 0.000 C12 C13 C2 H13 0.9288 1.4881 -0.2471 43 0.930 0.000 C13 C12 C5 2010sl0006a ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq F1 0.74780 0.72937 0.15377 1.00000 0.04254 0.03651 0.03218 0.00815 0.00519 -0.00553 0.03708 0.00478 0.00045 0.00035 0.00011 0.00000 0.00162 0.00147 0.00157 0.00123 0.00130 0.00140 0.00073 F2 1.26968 1.47764 -0.30565 1.00000 0.04254 0.04200 0.03223 0.01212 0.00535 -0.00161 0.03892 0.00495 0.00044 0.00037 0.00012 0.00000 0.00164 0.00162 0.00150 0.00129 0.00135 0.00142 0.00074 F3 1.12266 0.87820 0.13953 1.00000 0.03843 0.04744 0.03158 0.01011 -0.01016 -0.00266 0.03915 0.00483 0.00045 0.00039 0.00012 0.00000 0.00156 0.00163 0.00142 0.00138 0.00128 0.00140 0.00073 F4 0.52195 0.99198 -0.03407 1.00000 0.02580 0.04727 0.03866 0.00523 -0.00618 -0.00170 0.03725 0.00464 0.00039 0.00038 0.00013 0.00000 0.00140 0.00173 0.00151 0.00142 0.00125 0.00138 0.00072 N1 0.89564 1.14602 -0.05531 1.00000 0.02477 0.03099 0.02443 0.00270 0.00018 0.00332 0.02673 0.00662 0.00059 0.00051 0.00016 0.00000 0.00209 0.00217 0.00194 0.00167 0.00161 0.00176 0.00091 C1 0.97493 0.90770 0.09563 1.00000 0.02931 0.02861 0.02239 -0.00048 -0.00516 0.00013 0.02677 0.00748 0.00071 0.00060 0.00019 0.00000 0.00250 0.00232 0.00230 0.00205 0.00188 0.00213 0.00105 C2 1.12023 1.22911 -0.14025 1.00000 0.02231 0.03170 0.02204 0.00128 -0.00069 0.00085 0.02535 0.00766 0.00068 0.00059 0.00020 0.00000 0.00221 0.00233 0.00219 0.00203 0.00186 0.00205 0.00100 C3 0.86676 1.04371 -0.00080 1.00000 0.02827 0.02541 0.02343 0.00048 -0.00124 0.00105 0.02571 0.00775 0.00071 0.00059 0.00020 0.00000 0.00239 0.00215 0.00228 0.00196 0.00196 0.00189 0.00098 C4 1.06898 1.13355 -0.08332 1.00000 0.03086 0.02519 0.01936 -0.00077 -0.00562 0.00086 0.02514 0.00742 0.00071 0.00059 0.00019 0.00000 0.00247 0.00227 0.00213 0.00194 0.00195 0.00188 0.00100 H4 1.16836 1.05908 -0.06638 1.00000 0.03016 0.00000 0.00000 C5 1.22126 1.39601 -0.25041 1.00000 0.03310 0.03164 0.02432 0.00289 0.00383 -0.00666 0.02969 0.00791 0.00073 0.00058 0.00022 0.00000 0.00264 0.00235 0.00234 0.00217 0.00209 0.00211 0.00106 C6 0.78362 0.83291 0.10291 1.00000 0.03386 0.02052 0.02575 0.00277 0.00198 0.00174 0.02671 0.00780 0.00072 0.00056 0.00021 0.00000 0.00267 0.00208 0.00238 0.00190 0.00204 0.00202 0.00103 C7 1.01913 1.01376 0.04474 1.00000 0.02153 0.02954 0.02591 -0.00516 0.00077 0.00248 0.02566 0.00766 0.00068 0.00059 0.00020 0.00000 0.00222 0.00246 0.00235 0.00195 0.00183 0.00210 0.00102 H7 1.14908 1.06491 0.04075 1.00000 0.03079 0.00000 0.00000 C8 1.31752 1.21160 -0.16623 1.00000 0.02962 0.02582 0.02759 -0.00066 -0.00317 0.00257 0.02768 0.00775 0.00072 0.00059 0.00022 0.00000 0.00251 0.00229 0.00234 0.00205 0.00196 0.00197 0.00104 H8 1.41536 1.14269 -0.14579 1.00000 0.03321 0.00000 0.00000 C9 0.67414 0.96588 0.00913 1.00000 0.02564 0.03165 0.02386 -0.00275 0.00150 0.00299 0.02705 0.00770 0.00068 0.00061 0.00020 0.00000 0.00234 0.00238 0.00222 0.00211 0.00190 0.00200 0.00103 C10 0.62909 0.85965 0.05977 1.00000 0.02310 0.02965 0.03369 -0.00210 0.00326 -0.00544 0.02881 0.00779 0.00074 0.00059 0.00021 0.00000 0.00240 0.00255 0.00257 0.00214 0.00199 0.00211 0.00108 H10 0.49949 0.80834 0.06449 1.00000 0.03457 0.00000 0.00000 C11 1.37046 1.29482 -0.22183 1.00000 0.02483 0.03352 0.03026 0.00148 -0.00043 -0.00220 0.02954 0.00781 0.00073 0.00061 0.00021 0.00000 0.00244 0.00271 0.00244 0.00209 0.00198 0.00214 0.00109 H11 1.50173 1.28277 -0.23917 1.00000 0.03544 0.00000 0.00000 C12 0.97492 1.33337 -0.17139 1.00000 0.02655 0.03116 0.02346 -0.00169 0.00524 -0.00069 0.02706 0.00778 0.00073 0.00059 0.00020 0.00000 0.00244 0.00239 0.00232 0.00200 0.00189 0.00200 0.00103 H12 0.84279 1.34580 -0.15470 1.00000 0.03247 0.00000 0.00000 C13 1.02510 1.41795 -0.22650 1.00000 0.03250 0.02837 0.03425 0.00059 -0.00307 -0.00064 0.03171 0.00830 0.00079 0.00063 0.00022 0.00000 0.00269 0.00243 0.00266 0.00210 0.00216 0.00218 0.00114 H13 0.92883 1.48814 -0.24706 1.00000 0.03805 0.00000 0.00000 Final Structure Factor Calculation for 2010sl0006a Total number of l.s. parameters = 163 Maximum vector length = 511 Memory required = 1713 / 25046 wR2 = 0.1728 before cycle 21 for 1831 data and 2 / 163 parameters GooF = S = 0.668; Restrained GooF = 0.668 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1376 * P )^2 + 3.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0541 for 1344 Fo > 4sig(Fo) and 0.0877 for all 1831 data wR2 = 0.1728, GooF = S = 0.668, Restrained GooF = 0.668 for all data Flack x parameter = -0.0671 with su 1.5829 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 = 18.00 for non-hydrogen and 7.00 for hydrogen atoms Principal mean square atomic displacements U 0.0458 0.0424 0.0230 F1 0.0506 0.0436 0.0226 F2 0.0555 0.0396 0.0223 F3 0.0505 0.0379 0.0233 F4 0.0332 0.0244 0.0226 N1 0.0321 0.0286 0.0196 C1 0.0319 0.0229 0.0212 C2 0.0288 0.0254 0.0229 C3 0.0333 0.0251 0.0171 C4 0.0391 0.0297 0.0202 C5 0.0347 0.0261 0.0193 C6 0.0334 0.0239 0.0197 C7 0.0328 0.0260 0.0242 C8 0.0333 0.0263 0.0215 C9 0.0368 0.0299 0.0198 C10 0.0346 0.0297 0.0243 C11 0.0325 0.0292 0.0195 C12 0.0367 0.0302 0.0283 C13 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.021 0.033 0.042 0.053 0.064 0.079 0.099 0.126 0.169 1.000 Number in group 193. 180. 180. 192. 178. 179. 182. 183. 182. 182. GooF 0.794 0.769 0.748 0.779 0.664 0.600 0.613 0.525 0.510 0.586 K 0.743 0.921 0.917 0.974 0.953 1.004 1.013 1.019 1.044 0.978 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.06 1.15 1.25 1.44 1.81 inf Number in group 189. 179. 182. 182. 188. 178. 183. 184. 185. 181. GooF 0.775 0.813 0.716 0.725 0.671 0.694 0.595 0.517 0.550 0.554 K 1.044 0.970 0.990 0.994 1.027 1.038 1.054 1.025 1.050 0.943 R1 0.232 0.225 0.176 0.126 0.076 0.076 0.057 0.049 0.043 0.040 ** Extinction (EXTI) or solvent water (SWAT) correction may be required ** Recommended weighting scheme: WGHT 0.0662 0.0000 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) 6 0 0 -10.98 33.07 4.29 0.043 1.08 6 0 6 115.08 47.75 3.75 0.052 1.03 4 0 13 -1.76 18.78 3.28 0.033 1.15 6 2 13 81.46 31.60 3.25 0.042 0.88 -5 6 3 12.98 57.88 3.21 0.057 0.90 4 3 15 21.96 0.84 3.20 0.007 0.98 1 3 23 -11.62 38.78 3.04 0.047 0.86 5 5 13 67.62 20.04 3.00 0.034 0.84 -4 5 14 10.68 67.47 2.99 0.062 0.90 5 2 14 92.34 50.05 2.90 0.053 0.95 5 5 1 8.28 38.57 2.87 0.047 0.98 0 8 11 -27.45 7.67 2.86 0.021 0.85 5 6 4 11.59 45.29 2.86 0.051 0.89 3 6 2 0.73 24.15 2.85 0.037 1.09 0 1 21 63.93 118.48 2.84 0.082 1.00 3 3 17 -5.76 16.55 2.82 0.031 1.00 2 7 14 74.49 157.95 2.80 0.095 0.85 -7 1 9 -22.31 8.88 2.79 0.022 0.85 -6 5 2 -16.98 11.58 2.77 0.026 0.88 3 4 16 -2.61 19.31 2.72 0.033 0.97 6 5 0 41.77 99.57 2.70 0.075 0.88 -1 1 18 7.74 33.80 2.64 0.044 1.15 4 3 8 -7.44 1.33 2.60 0.009 1.21 -6 5 1 -9.00 26.55 2.57 0.039 0.88 0 4 22 -27.85 2.82 2.57 0.013 0.86 -5 5 9 -18.65 1.81 2.54 0.010 0.91 -2 4 16 -5.69 11.98 2.54 0.026 1.03 4 1 0 75.10 46.61 2.51 0.052 1.58 4 1 11 -2.53 9.15 2.51 0.023 1.22 2 5 11 24.58 57.86 2.50 0.057 1.12 1 5 20 -60.52 3.11 2.47 0.013 0.86 7 1 5 17.90 45.12 2.46 0.051 0.90 -4 2 16 -6.48 12.78 2.46 0.027 0.99 3 2 0 408.74 312.73 2.45 0.133 1.88 4 2 19 -7.70 8.85 2.44 0.022 0.90 2 6 15 -15.20 0.60 2.43 0.006 0.91 0 4 20 44.68 9.31 2.43 0.023 0.93 5 0 19 62.55 108.08 2.40 0.078 0.85 -6 2 11 29.34 3.14 2.40 0.013 0.91 1 8 4 16.53 49.56 2.39 0.053 0.93 6 3 10 116.53 72.06 2.37 0.064 0.90 0 3 11 -7.51 0.05 2.36 0.002 1.54 1 7 13 -7.37 28.14 2.36 0.040 0.90 5 6 8 28.28 67.19 2.36 0.062 0.86 -5 2 17 9.71 36.93 2.33 0.046 0.88 6 3 5 -5.18 9.16 2.33 0.023 0.97 5 0 16 64.68 31.48 2.29 0.042 0.93 3 5 8 67.51 105.43 2.28 0.078 1.13 2 0 19 533.36 411.83 2.27 0.153 1.06 -6 2 13 67.67 31.31 2.26 0.042 0.88 Bond lengths and angles F1 - Distance Angles C6 1.3595 (0.0050) F1 - F2 - Distance Angles C5 1.3666 (0.0053) F2 - F3 - Distance Angles C1 1.3550 (0.0050) F3 - F4 - Distance Angles C9 1.3614 (0.0051) F4 - N1 - Distance Angles C4 1.2730 (0.0059) C3 1.4104 (0.0056) 117.44 (0.40) N1 - C4 C1 - Distance Angles F3 1.3550 (0.0050) C7 1.3814 (0.0063) 119.48 (0.39) C6 1.3705 (0.0066) 119.28 (0.38) 121.24 (0.40) C1 - F3 C7 C2 - Distance Angles C8 1.3965 (0.0065) C12 1.3974 (0.0062) 118.71 (0.41) C4 1.4522 (0.0059) 119.40 (0.41) 121.84 (0.40) C2 - C8 C12 C3 - Distance Angles N1 1.4104 (0.0056) C7 1.4009 (0.0062) 124.50 (0.42) C9 1.3953 (0.0064) 118.53 (0.39) 116.96 (0.39) C3 - N1 C7 C4 - Distance Angles N1 1.2730 (0.0059) C2 1.4522 (0.0059) 123.67 (0.42) H4 0.9300 118.16 118.16 C4 - N1 C2 C5 - Distance Angles F2 1.3666 (0.0053) C11 1.3766 (0.0067) 118.34 (0.41) C13 1.3767 (0.0070) 118.29 (0.41) 123.36 (0.43) C5 - F2 C11 C6 - Distance Angles F1 1.3595 (0.0049) C10 1.3722 (0.0064) 119.68 (0.41) C1 1.3705 (0.0066) 119.01 (0.39) 121.30 (0.40) C6 - F1 C10 C7 - Distance Angles C1 1.3814 (0.0063) C3 1.4009 (0.0062) 119.52 (0.41) H7 0.9300 120.24 120.24 C7 - C1 C3 C8 - Distance Angles C11 1.3858 (0.0065) C2 1.3965 (0.0065) 121.34 (0.44) H8 0.9300 119.33 119.33 C8 - C11 C2 C9 - Distance Angles F4 1.3614 (0.0051) C3 1.3953 (0.0064) 118.72 (0.37) C10 1.3792 (0.0063) 117.46 (0.39) 123.80 (0.41) C9 - F4 C3 C10 - Distance Angles C6 1.3722 (0.0064) C9 1.3792 (0.0063) 117.17 (0.42) H10 0.9300 121.42 121.42 C10 - C6 C9 C11 - Distance Angles C8 1.3858 (0.0065) C5 1.3766 (0.0066) 117.44 (0.44) H11 0.9300 121.28 121.28 C11 - C8 C5 C12 - Distance Angles C13 1.3774 (0.0064) C2 1.3974 (0.0062) 120.78 (0.44) H12 0.9300 119.61 119.61 C12 - C13 C2 C13 - Distance Angles C12 1.3774 (0.0065) C5 1.3767 (0.0070) 118.37 (0.46) H13 0.9300 120.82 120.82 C13 - C12 C5 FMAP and GRID set by program FMAP 2 3 24 GRID -1.190 -2 -2 1.190 2 2 R1 = 0.0731 for 1095 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.23 at 0.2396 0.1895 0.0945 [ 1.47 A from H12 ] Deepest hole -0.26 at 0.5059 0.4374 0.0614 [ 0.82 A from C4 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 1630 / 13638 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.7396 1.3105 -0.0945 1.00000 0.05 0.23 1.47 H12 1.60 H7 1.81 N1 2.22 C7 Q2 1 1.2509 1.3016 -0.0939 1.00000 0.05 0.22 1.41 C2 1.74 C8 1.75 C4 1.95 H8 Q3 1 0.3754 0.8111 -0.0080 1.00000 0.05 0.20 1.74 H10 1.76 F4 2.22 C10 2.29 C9 Q4 1 0.5800 1.0432 0.0704 1.00000 0.05 0.20 1.45 C10 1.56 C9 1.87 H10 2.19 C6 Q5 1 0.7033 1.4073 -0.2493 1.00000 0.05 0.20 1.58 H13 1.63 H11 2.14 C13 2.26 H12 Q6 1 0.6996 0.9233 0.1909 1.00000 0.05 0.20 1.70 F1 1.82 C13 1.88 C5 2.07 C6 Q7 1 1.2682 1.0269 0.0526 1.00000 0.05 0.20 0.86 H7 1.62 C7 2.25 H10 2.29 C1 Q8 1 1.2186 0.9915 -0.0684 1.00000 0.05 0.19 0.61 H4 1.49 C4 2.09 F4 2.38 H8 Q9 1 0.2551 0.8184 0.0494 1.00000 0.05 0.19 1.61 H10 2.01 H7 2.13 C7 2.15 F3 Q10 1 1.2928 1.1782 -0.0473 1.00000 0.05 0.18 1.28 H4 1.67 C4 2.07 F4 2.26 H8 Q11 1 1.0358 1.2576 -0.2987 1.00000 0.05 0.18 1.90 C5 1.96 C13 2.10 F1 2.18 H13 Q12 1 0.8959 0.6689 0.0709 1.00000 0.05 0.18 1.60 C6 1.67 F4 1.96 C1 2.06 F1 Q13 1 1.5471 1.4245 -0.1882 1.00000 0.05 0.18 1.56 H11 1.67 C11 1.89 F3 2.13 H12 Q14 1 1.4041 1.2188 -0.0949 1.00000 0.05 0.18 1.23 H8 1.62 C8 2.04 H4 2.08 C2 Q15 1 1.5827 1.2151 -0.1355 1.00000 0.05 0.18 1.23 H8 1.84 C8 2.00 H12 2.33 H11 Q16 1 0.8705 1.4639 -0.2609 1.00000 0.05 0.18 0.51 H13 1.29 C13 2.25 C12 2.34 C5 Q17 1 1.1224 1.6243 -0.3326 1.00000 0.05 0.18 1.58 F2 1.72 C12 1.72 H12 1.85 C2 Q18 1 0.7449 1.2617 -0.1532 1.00000 0.05 0.18 0.90 H12 1.63 C12 2.32 H8 2.34 F2 Q19 1 1.3871 1.0232 0.0802 1.00000 0.05 0.18 1.78 H7 1.82 H10 1.90 H12 2.05 C10 Q20 1 1.4173 0.9791 -0.1512 1.00000 0.05 0.18 1.25 H8 1.91 C8 1.93 F1 2.22 F2 Shortest distances between peaks (including symmetry equivalents) 7 19 0.97 15 18 1.17 2 14 1.17 5 16 1.19 4 19 1.27 10 14 1.28 1 18 1.30 3 12 1.35 17 18 1.39 2 10 1.39 14 15 1.44 3 9 1.45 1 15 1.52 1 7 1.54 8 10 1.57 7 9 1.59 1 19 1.61 5 13 1.65 8 12 1.68 2 4 1.69 9 19 1.89 13 18 1.93 13 15 1.96 12 20 2.05 4 7 2.05 11 16 2.06 6 11 2.06 15 20 2.12 3 8 2.14 15 17 2.14 8 14 2.18 8 20 2.18 14 20 2.19 3 7 2.20 1 14 2.28 1 17 2.28 5 20 2.32 5 18 2.34 2 15 2.41 7 10 2.42 2 8 2.43 18 19 2.44 3 19 2.48 1 13 2.51 1 4 2.52 6 13 2.53 16 17 2.55 14 18 2.55 4 10 2.58 7 8 2.61 13 16 2.62 9 12 2.63 16 20 2.64 11 16 2.64 5 11 2.65 10 15 2.67 7 18 2.68 13 14 2.69 2 19 2.72 9 12 2.72 6 16 2.74 4 9 2.75 3 4 2.77 10 12 2.77 3 9 2.79 10 20 2.80 4 14 2.82 4 6 2.83 8 9 2.84 16 18 2.88 5 6 2.89 7 15 2.90 2 13 2.93 5 15 2.94 11 17 2.94 2 20 2.95 2 6 2.96 3 10 2.97 1 9 2.99 5 17 2.99 12 14 3.00 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. 1.45: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.97: Structure factors and derivatives 1.95: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.95: Solve l.s. equations 0.00: Generate HTAB table 0.06: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2010sl0006a finished at 22:04:42 Total CPU time: 6.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++