+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2010src0794a started at 18:25:21 on 10-Sep-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2010src0794a CELL 0.71073 9.9484 7.9134 16.0131 90.000 104.340 90.000 ZERR 4.00 0.0011 0.0010 0.0022 0.000 0.008 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 60 40 8 12 V = 1221.36 F(000) = 552.0 Mu = 0.10 mm-1 Cell Wt = 1065.00 Rho = 1.448 MERG 2 OMIT -3.00 50.00 SHEL 7 0.84 EQIV $1 [ -x+1, -y+1, -z ] HTAB N1 O1_$1 SIZE 0.02 0.14 0.16 ACTA BOND $H WGHT 0.01690 2.73210 L.S. 20 TEMP -153.00 FVAR 1.05309 C1 1 0.393434 0.705779 0.021583 11.00000 0.02465 0.02800 = 0.03086 0.00133 0.01030 -0.00091 C2 1 0.322403 0.874577 0.018817 11.00000 0.02367 0.02288 = 0.02954 -0.00008 0.00547 0.00146 C3 1 0.333119 0.952886 -0.062866 11.00000 0.02252 0.02567 = 0.02861 -0.00005 0.00674 0.00016 C4 1 0.285679 1.102337 -0.106460 11.00000 0.03032 0.02415 = 0.02803 -0.00341 0.00568 -0.00151 AFIX 43 H4 2 0.239673 1.184722 -0.080446 11.00000 -1.20000 AFIX 0 C5 1 0.305905 1.129940 -0.187577 11.00000 0.03657 0.02522 = 0.03061 0.00139 0.00302 0.00067 AFIX 43 H5 2 0.273680 1.231946 -0.217077 11.00000 -1.20000 AFIX 0 C6 1 0.373023 1.010174 -0.226927 11.00000 0.02843 0.03644 = 0.02820 0.00175 0.00484 0.00185 AFIX 43 H6 2 0.386364 1.032091 -0.282648 11.00000 -1.20000 AFIX 0 C7 1 0.420616 0.859139 -0.185573 11.00000 0.02828 0.03012 = 0.02871 -0.00376 0.00851 0.00225 AFIX 43 H7 2 0.464924 0.776125 -0.212302 11.00000 -1.20000 AFIX 0 C8 1 0.400860 0.835023 -0.104427 11.00000 0.02367 0.02308 = 0.02720 -0.00131 0.00300 0.00033 C9 1 0.257884 0.910286 0.081184 11.00000 0.02805 0.02598 = 0.02758 0.00073 0.00683 -0.00124 AFIX 43 H9 2 0.263123 0.824008 0.123122 11.00000 -1.20000 AFIX 0 C10 1 0.180477 1.061893 0.094698 11.00000 0.02695 0.02719 = 0.02501 -0.00196 0.00642 0.00113 C11 1 0.218358 1.223869 0.074654 11.00000 0.02488 0.03258 = 0.02690 -0.00120 0.00704 0.00134 AFIX 43 H11 2 0.296316 1.237723 0.051000 11.00000 -1.20000 AFIX 0 C12 1 0.144310 1.364695 0.088641 11.00000 0.02946 0.02218 = 0.02889 0.00021 0.00258 -0.00407 AFIX 43 H12 2 0.170849 1.474822 0.075330 11.00000 -1.20000 AFIX 0 C13 1 0.030711 1.340717 0.122499 11.00000 0.02555 0.02461 = 0.02814 -0.00398 0.00195 0.00383 C14 1 -0.008224 1.183317 0.145423 11.00000 0.02780 0.03268 = 0.02823 -0.00379 0.01029 0.00140 AFIX 43 H14 2 -0.085409 1.171036 0.169939 11.00000 -1.20000 AFIX 0 C15 1 0.067631 1.043820 0.131910 11.00000 0.03038 0.02495 = 0.03267 -0.00050 0.00702 -0.00050 AFIX 43 H15 2 0.043017 0.934754 0.147999 11.00000 -1.20000 AFIX 0 N1 3 0.438205 0.692541 -0.051675 11.00000 0.03231 0.02283 = 0.02825 0.00098 0.01077 0.00478 AFIX 43 H1 2 0.484687 0.605705 -0.064415 11.00000 -1.20000 AFIX 0 N2 3 -0.048288 1.489014 0.138154 11.00000 0.03247 0.02800 = 0.03743 -0.00443 0.00568 0.00455 O1 4 0.407939 0.598039 0.078842 11.00000 0.03888 0.02643 = 0.03567 0.00642 0.01411 0.00354 O2 4 0.001279 1.629268 0.131691 11.00000 0.05380 0.02714 = 0.06657 -0.00319 0.02311 0.00265 O3 4 -0.158968 1.467254 0.156714 11.00000 0.03128 0.04259 = 0.08275 -0.01089 0.02043 0.00344 HKLF 4 Covalent radii and connectivity table for 2010src0794a C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1 N1 C2 C2 - C9 C3 C1 C3 - C4 C8 C2 C4 - C5 C3 C5 - C4 C6 C6 - C7 C5 C7 - C8 C6 C8 - C7 N1 C3 C9 - C2 C10 C10 - C11 C15 C9 C11 - C12 C10 C12 - C13 C11 C13 - C14 C12 N2 C14 - C13 C15 C15 - C14 C10 N1 - C1 C8 N2 - O3 O2 C13 O1 - C1 O2 - N2 O3 - N2 Operators for generating equivalent atoms: $1 -x+1, -y+1, -z 6679 Reflections read, of which 1187 rejected -11 =< h =< 10, -9 =< k =< 8, -19 =< l =< 18, Max. 2-theta = 50.00 0 Systematic absence violations 0 Inconsistent equivalents 2062 Unique reflections, of which 0 suppressed R(int) = 0.0526 R(sigma) = 0.0690 Friedel opposites merged Maximum memory for data reduction = 1702 / 20715 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 = 2183 / 224810 wR2 = 0.1509 before cycle 1 for 2062 data and 181 / 181 parameters GooF = S = 1.075; Restrained GooF = 1.075 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0169 * P )^2 + 2.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.04803 0.00335 -1.509 OSF Mean shift/su = 0.239 Maximum = -1.509 for OSF Max. shift = 0.002 A for C5 Max. dU =-0.001 for O3 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2183 / 224810 wR2 = 0.1498 before cycle 2 for 2062 data and 181 / 181 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0169 * P )^2 + 2.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.04765 0.00332 -0.117 OSF Mean shift/su = 0.078 Maximum = -0.327 for U13 C10 Max. shift = 0.001 A for C5 Max. dU = 0.000 for C1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2183 / 224810 wR2 = 0.1497 before cycle 3 for 2062 data and 181 / 181 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0169 * P )^2 + 2.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.04764 0.00332 -0.001 OSF Mean shift/su = 0.005 Maximum = 0.021 for U11 C3 Max. shift = 0.000 A for C2 Max. dU = 0.000 for O2 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2183 / 224810 wR2 = 0.1497 before cycle 4 for 2062 data and 181 / 181 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0169 * P )^2 + 2.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.04765 0.00332 0.004 OSF Mean shift/su = 0.001 Maximum = -0.007 for U13 C8 Max. shift = 0.000 A for H6 Max. dU = 0.000 for C13 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2183 / 224810 wR2 = 0.1497 before cycle 5 for 2062 data and 181 / 181 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0169 * P )^2 + 2.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.04766 0.00332 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for x C5 Max. shift = 0.000 A for C5 Max. dU = 0.000 for C10 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2183 / 224810 wR2 = 0.1497 before cycle 6 for 2062 data and 181 / 181 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0169 * P )^2 + 2.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.04766 0.00332 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for U23 C12 Max. shift = 0.000 A for C5 Max. dU = 0.000 for C15 Least-squares cycle 7 Maximum vector length = 511 Memory required = 2183 / 224810 wR2 = 0.1497 before cycle 7 for 2062 data and 181 / 181 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0169 * P )^2 + 2.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.04766 0.00332 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y C15 Max. shift = 0.000 A for C15 Max. dU = 0.000 for C13 Least-squares cycle 8 Maximum vector length = 511 Memory required = 2183 / 224810 wR2 = 0.1497 before cycle 8 for 2062 data and 181 / 181 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0169 * P )^2 + 2.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.04766 0.00332 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y C13 Max. shift = 0.000 A for O1 Max. dU = 0.000 for N2 Least-squares cycle 9 Maximum vector length = 511 Memory required = 2183 / 224810 wR2 = 0.1497 before cycle 9 for 2062 data and 181 / 181 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0169 * P )^2 + 2.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.04766 0.00332 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y C13 Max. shift = 0.000 A for C13 Max. dU = 0.000 for O3 Least-squares cycle 10 Maximum vector length = 511 Memory required = 2183 / 224810 wR2 = 0.1497 before cycle 10 for 2062 data and 181 / 181 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0169 * P )^2 + 2.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.04766 0.00332 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y O2 Max. shift = 0.000 A for N1 Max. dU = 0.000 for N1 Least-squares cycle 11 Maximum vector length = 511 Memory required = 2183 / 224810 wR2 = 0.1497 before cycle 11 for 2062 data and 181 / 181 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0169 * P )^2 + 2.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.04766 0.00332 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y O2 Max. shift = 0.000 A for O2 Max. dU = 0.000 for O3 Least-squares cycle 12 Maximum vector length = 511 Memory required = 2183 / 224810 wR2 = 0.1497 before cycle 12 for 2062 data and 181 / 181 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0169 * P )^2 + 2.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.04766 0.00332 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y O2 Max. shift = 0.000 A for N1 Max. dU = 0.000 for C7 Least-squares cycle 13 Maximum vector length = 511 Memory required = 2183 / 224810 wR2 = 0.1497 before cycle 13 for 2062 data and 181 / 181 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0169 * P )^2 + 2.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.04766 0.00332 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y O2 Max. shift = 0.000 A for C6 Max. dU = 0.000 for O3 Least-squares cycle 14 Maximum vector length = 511 Memory required = 2183 / 224810 wR2 = 0.1497 before cycle 14 for 2062 data and 181 / 181 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0169 * P )^2 + 2.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.04766 0.00332 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for O2 Max. dU = 0.000 for C4 Least-squares cycle 15 Maximum vector length = 511 Memory required = 2183 / 224810 wR2 = 0.1497 before cycle 15 for 2062 data and 181 / 181 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0169 * P )^2 + 2.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.04766 0.00332 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y C15 Max. shift = 0.000 A for N1 Max. dU = 0.000 for C11 Least-squares cycle 16 Maximum vector length = 511 Memory required = 2183 / 224810 wR2 = 0.1497 before cycle 16 for 2062 data and 181 / 181 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0169 * P )^2 + 2.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.04766 0.00332 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y C15 Max. shift = 0.000 A for C15 Max. dU = 0.000 for O3 Least-squares cycle 17 Maximum vector length = 511 Memory required = 2183 / 224810 wR2 = 0.1497 before cycle 17 for 2062 data and 181 / 181 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0169 * P )^2 + 2.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.04766 0.00332 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y O2 Max. shift = 0.000 A for N1 Max. dU = 0.000 for C13 Least-squares cycle 18 Maximum vector length = 511 Memory required = 2183 / 224810 wR2 = 0.1497 before cycle 18 for 2062 data and 181 / 181 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0169 * P )^2 + 2.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.04766 0.00332 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C15 Max. dU = 0.000 for O3 Least-squares cycle 19 Maximum vector length = 511 Memory required = 2183 / 224810 wR2 = 0.1497 before cycle 19 for 2062 data and 181 / 181 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0169 * P )^2 + 2.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.04766 0.00332 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 C9 Least-squares cycle 20 Maximum vector length = 511 Memory required = 2183 / 224810 wR2 = 0.1497 before cycle 20 for 2062 data and 181 / 181 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0169 * P )^2 + 2.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.04766 0.00332 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y C15 Max. shift = 0.000 A for H14 Max. dU = 0.000 for C15 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 0.2396 1.1846 -0.0805 43 0.950 0.000 C4 C5 C3 H5 0.2736 1.2322 -0.2171 43 0.950 0.000 C5 C4 C6 H6 0.3865 1.0319 -0.2826 43 0.950 0.000 C6 C7 C5 H7 0.4648 0.7763 -0.2122 43 0.950 0.000 C7 C8 C6 H9 0.2631 0.8241 0.1230 43 0.950 0.000 C9 C2 C10 H11 0.2960 1.2377 0.0508 43 0.950 0.000 C11 C12 C10 H12 0.1708 1.4747 0.0753 43 0.950 0.000 C12 C13 C11 H14 -0.0854 1.1711 0.1699 43 0.950 0.000 C14 C13 C15 H15 0.0430 0.9348 0.1480 43 0.950 0.000 C15 C14 C10 H1 0.4847 0.6058 -0.0644 43 0.880 0.000 N1 C1 C8 2010src0794a ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.39353 0.70566 0.02152 1.00000 0.02355 0.02829 0.02917 0.00156 0.00914 -0.00155 0.02654 0.00635 0.00033 0.00043 0.00022 0.00000 0.00173 0.00188 0.00199 0.00157 0.00148 0.00147 0.00078 C2 0.32235 0.87451 0.01884 1.00000 0.02341 0.02247 0.03141 -0.00016 0.00719 0.00006 0.02569 0.00627 0.00033 0.00041 0.00022 0.00000 0.00170 0.00174 0.00202 0.00143 0.00148 0.00141 0.00078 C3 0.33302 0.95284 -0.06284 1.00000 0.02363 0.02484 0.02982 -0.00039 0.00661 -0.00030 0.02610 0.00620 0.00032 0.00042 0.00022 0.00000 0.00173 0.00178 0.00200 0.00146 0.00148 0.00144 0.00078 C4 0.28567 1.10221 -0.10655 1.00000 0.03095 0.02331 0.02950 -0.00241 0.00594 -0.00046 0.02819 0.00627 0.00034 0.00042 0.00022 0.00000 0.00189 0.00178 0.00205 0.00147 0.00154 0.00150 0.00081 H4 0.23965 1.18456 -0.08052 1.00000 0.03383 0.00000 0.00000 C5 0.30578 1.13018 -0.18762 1.00000 0.03591 0.02452 0.02967 0.00170 0.00236 0.00015 0.03105 0.00643 0.00035 0.00043 0.00023 0.00000 0.00199 0.00184 0.00210 0.00152 0.00156 0.00158 0.00084 H5 0.27355 1.23220 -0.21710 1.00000 0.03726 0.00000 0.00000 C6 0.37305 1.01011 -0.22687 1.00000 0.02893 0.03666 0.02801 0.00210 0.00508 0.00183 0.03155 0.00662 0.00034 0.00045 0.00023 0.00000 0.00186 0.00209 0.00206 0.00157 0.00153 0.00163 0.00085 H6 0.38650 1.03189 -0.28258 1.00000 0.03786 0.00000 0.00000 C7 0.42052 0.85926 -0.18549 1.00000 0.02907 0.02968 0.02831 -0.00333 0.00872 0.00264 0.02874 0.00644 0.00034 0.00044 0.00022 0.00000 0.00183 0.00193 0.00207 0.00149 0.00151 0.00155 0.00081 H7 0.46480 0.77625 -0.21224 1.00000 0.03448 0.00000 0.00000 C8 0.40090 0.83494 -0.10442 1.00000 0.02367 0.02346 0.02642 -0.00153 0.00332 -0.00119 0.02503 0.00602 0.00032 0.00041 0.00021 0.00000 0.00169 0.00178 0.00199 0.00141 0.00142 0.00146 0.00077 C9 0.25789 0.91040 0.08110 1.00000 0.02842 0.02557 0.02686 0.00109 0.00643 -0.00190 0.02702 0.00623 0.00033 0.00043 0.00022 0.00000 0.00179 0.00180 0.00196 0.00142 0.00151 0.00149 0.00079 H9 0.26311 0.82406 0.12301 1.00000 0.03243 0.00000 0.00000 C10 0.18056 1.06182 0.09483 1.00000 0.02732 0.02614 0.02458 -0.00198 0.00452 0.00059 0.02635 0.00618 0.00033 0.00042 0.00021 0.00000 0.00181 0.00183 0.00193 0.00142 0.00148 0.00150 0.00079 C11 0.21823 1.22380 0.07463 1.00000 0.02457 0.03429 0.02614 -0.00213 0.00764 0.00004 0.02810 0.00629 0.00034 0.00044 0.00022 0.00000 0.00176 0.00199 0.00198 0.00152 0.00147 0.00157 0.00081 H11 0.29604 1.23766 0.05083 1.00000 0.03372 0.00000 0.00000 C12 0.14421 1.36460 0.08865 1.00000 0.02852 0.02277 0.02827 -0.00077 0.00259 -0.00348 0.02730 0.00608 0.00033 0.00042 0.00022 0.00000 0.00181 0.00176 0.00196 0.00144 0.00149 0.00150 0.00079 H12 0.17080 1.47470 0.07534 1.00000 0.03276 0.00000 0.00000 C13 0.03083 1.34087 0.12246 1.00000 0.02572 0.02524 0.02749 -0.00431 0.00100 0.00355 0.02713 0.00616 0.00033 0.00042 0.00022 0.00000 0.00177 0.00180 0.00196 0.00144 0.00147 0.00150 0.00079 C14 -0.00816 1.18332 0.14540 1.00000 0.02713 0.03248 0.02818 -0.00274 0.01073 0.00204 0.02858 0.00642 0.00035 0.00043 0.00022 0.00000 0.00179 0.00200 0.00200 0.00150 0.00151 0.00156 0.00081 H14 -0.08538 1.17106 0.16988 1.00000 0.03430 0.00000 0.00000 C15 0.06767 1.04384 0.13194 1.00000 0.03073 0.02576 0.03210 -0.00103 0.00833 -0.00225 0.02944 0.00646 0.00034 0.00044 0.00022 0.00000 0.00189 0.00189 0.00211 0.00151 0.00160 0.00154 0.00083 H15 0.04298 0.93479 0.14801 1.00000 0.03532 0.00000 0.00000 N1 0.43818 0.69262 -0.05165 1.00000 0.03138 0.02253 0.02844 0.00145 0.01097 0.00516 0.02682 0.00525 0.00028 0.00034 0.00018 0.00000 0.00154 0.00149 0.00167 0.00120 0.00127 0.00123 0.00068 H1 0.48468 0.60579 -0.06439 1.00000 0.03219 0.00000 0.00000 N2 -0.04835 1.48912 0.13815 1.00000 0.03218 0.02818 0.03676 -0.00497 0.00543 0.00539 0.03292 0.00565 0.00031 0.00038 0.00019 0.00000 0.00176 0.00176 0.00191 0.00134 0.00142 0.00140 0.00075 O1 0.40804 0.59803 0.07886 1.00000 0.03830 0.02718 0.03496 0.00611 0.01421 0.00368 0.03258 0.00468 0.00024 0.00029 0.00016 0.00000 0.00141 0.00135 0.00151 0.00111 0.00114 0.00110 0.00062 O2 0.00128 1.62928 0.13161 1.00000 0.05386 0.02566 0.06700 -0.00296 0.02274 0.00275 0.04747 0.00544 0.00029 0.00032 0.00019 0.00000 0.00176 0.00148 0.00205 0.00132 0.00150 0.00132 0.00076 O3 -0.15891 1.46729 0.15676 1.00000 0.03066 0.04183 0.08222 -0.01099 0.02066 0.00342 0.05039 0.00535 0.00026 0.00035 0.00020 0.00000 0.00148 0.00171 0.00233 0.00151 0.00150 0.00129 0.00081 Final Structure Factor Calculation for 2010src0794a Total number of l.s. parameters = 181 Maximum vector length = 511 Memory required = 2002 / 22995 wR2 = 0.1497 before cycle 21 for 2062 data and 0 / 181 parameters GooF = S = 1.064; Restrained GooF = 1.064 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0169 * P )^2 + 2.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0623 for 1475 Fo > 4sig(Fo) and 0.1026 for all 2062 data wR2 = 0.1497, GooF = S = 1.064, Restrained GooF = 1.064 for all data Occupancy sum of asymmetric unit = 20.00 for non-hydrogen and 10.00 for hydrogen atoms Principal mean square atomic displacements U 0.0304 0.0284 0.0209 C1 0.0315 0.0232 0.0225 C2 0.0299 0.0249 0.0235 C3 0.0326 0.0295 0.0225 C4 0.0413 0.0280 0.0239 C5 0.0373 0.0311 0.0262 C6 0.0332 0.0300 0.0230 C7 0.0293 0.0246 0.0212 C8 0.0300 0.0270 0.0241 C9 0.0298 0.0261 0.0231 C10 0.0348 0.0263 0.0231 C11 0.0348 0.0265 0.0207 C12 0.0375 0.0221 0.0219 C13 0.0339 0.0307 0.0211 C14 0.0326 0.0308 0.0249 C15 0.0349 0.0257 0.0199 N1 0.0436 0.0319 0.0232 N2 0.0432 0.0308 0.0238 O1 0.0692 0.0485 0.0248 O2 0.0850 0.0417 0.0245 O3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.016 0.030 0.044 0.059 0.076 0.096 0.123 0.154 0.224 1.000 Number in group 215. 202. 208. 210. 201. 200. 210. 202. 206. 208. GooF 1.072 1.082 1.185 1.106 1.067 0.918 0.977 1.108 0.923 1.161 K 3.551 1.094 0.929 0.942 0.988 0.991 0.959 0.988 1.013 1.015 Resolution(A) 0.84 0.87 0.91 0.96 1.01 1.07 1.15 1.27 1.45 1.81 inf Number in group 209. 203. 207. 212. 202. 206. 203. 208. 206. 206. GooF 1.187 1.119 1.169 1.030 1.150 1.053 0.935 0.904 0.941 1.108 K 1.102 1.044 1.015 0.980 1.022 1.010 0.985 1.002 1.051 0.989 R1 0.282 0.207 0.170 0.158 0.115 0.080 0.065 0.065 0.051 0.037 Recommended weighting scheme: WGHT 0.0298 2.2718 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 2 12 78.24 203.46 4.78 0.144 1.11 6 4 6 51.51 150.44 4.44 0.124 1.05 3 7 7 61.69 152.52 3.99 0.124 0.93 -5 1 18 121.24 16.20 3.83 0.041 0.87 6 1 5 264.15 390.63 3.79 0.199 1.28 1 6 11 41.79 4.92 3.59 0.022 0.94 -10 2 13 78.44 9.85 3.51 0.032 0.84 -9 1 11 -1.62 38.20 3.34 0.062 0.97 6 3 7 30.14 102.69 3.33 0.102 1.07 -7 5 4 194.86 330.39 3.32 0.183 1.05 1 2 0 1283.57 1550.46 3.24 0.397 3.66 -10 3 10 15.02 61.82 3.17 0.079 0.88 5 4 4 169.16 271.70 3.09 0.166 1.23 7 6 3 4.62 40.82 3.00 0.064 0.91 5 6 6 -7.93 26.67 3.00 0.052 0.96 5 4 12 73.90 0.42 2.89 0.007 0.87 0 1 3 56.72 24.02 2.89 0.049 4.33 5 0 14 -13.37 53.19 2.85 0.074 0.87 -6 6 8 41.98 91.20 2.85 0.096 0.97 0 1 2 2837.74 3230.60 2.84 0.573 5.54 1 6 6 20.10 56.30 2.81 0.076 1.15 2 6 11 -14.92 26.27 2.76 0.052 0.92 0 7 2 2461.52 2129.94 2.76 0.465 1.12 -2 2 12 29.22 5.05 2.75 0.023 1.26 6 1 4 58.47 106.24 2.69 0.104 1.35 -4 6 10 119.21 185.54 2.69 0.137 0.99 -5 1 9 2.49 27.59 2.67 0.053 1.45 7 3 2 133.23 200.72 2.65 0.143 1.17 -1 4 7 1363.98 1177.28 2.64 0.346 1.50 -3 2 11 18.72 49.83 2.61 0.071 1.34 4 6 8 90.06 147.30 2.61 0.122 0.95 -2 3 17 57.30 17.92 2.59 0.043 0.89 -7 3 8 54.27 94.33 2.57 0.098 1.15 -4 5 7 78.52 137.12 2.57 0.118 1.21 1 9 0 -0.59 24.67 2.57 0.050 0.88 -3 0 2 545.76 666.12 2.57 0.260 3.27 -6 2 10 36.93 78.59 2.52 0.089 1.22 2 1 0 8990.59 9844.13 2.49 1.000 4.12 -3 8 9 -13.73 33.85 2.46 0.059 0.86 3 5 8 35.84 1.07 2.43 0.010 1.09 -5 8 3 289.77 201.50 2.43 0.143 0.88 1 2 17 57.03 0.01 2.43 0.001 0.87 -2 9 2 -0.57 28.73 2.42 0.054 0.86 9 3 4 -3.04 18.59 2.40 0.043 0.91 -5 7 7 123.13 190.50 2.38 0.139 0.94 3 7 0 23.66 1.65 2.38 0.013 1.07 -3 5 11 903.69 753.72 2.38 0.277 1.06 1 7 9 627.54 503.35 2.38 0.226 0.93 9 4 3 -22.22 15.75 2.37 0.040 0.89 -5 2 5 -5.36 11.61 2.37 0.034 1.68 Bond lengths and angles C1 - Distance Angles O1 1.2345 (0.0039) N1 1.3559 (0.0043) 125.96 (0.31) C2 1.5078 (0.0045) 126.88 (0.31) 107.15 (0.28) C1 - O1 N1 C2 - Distance Angles C9 1.3426 (0.0046) C3 1.4747 (0.0047) 136.24 (0.31) C1 1.5078 (0.0045) 118.27 (0.30) 105.14 (0.28) C2 - C9 C3 C3 - Distance Angles C4 1.3948 (0.0047) C8 1.4116 (0.0045) 117.71 (0.31) C2 1.4747 (0.0047) 135.37 (0.31) 106.76 (0.28) C3 - C4 C8 C4 - Distance Angles C5 1.3795 (0.0049) C3 1.3948 (0.0047) 119.90 (0.32) H4 0.9500 120.05 120.05 C4 - C5 C3 C5 - Distance Angles C4 1.3795 (0.0049) C6 1.3979 (0.0048) 120.75 (0.32) H5 0.9500 119.63 119.63 C5 - C4 C6 C6 - Distance Angles C7 1.3900 (0.0048) C5 1.3979 (0.0048) 120.88 (0.34) H6 0.9500 119.56 119.56 C6 - C7 C5 C7 - Distance Angles C8 1.3733 (0.0047) C6 1.3900 (0.0048) 117.39 (0.32) H7 0.9500 121.31 121.31 C7 - C8 C6 C8 - Distance Angles C7 1.3733 (0.0047) N1 1.4017 (0.0041) 127.17 (0.31) C3 1.4116 (0.0045) 123.36 (0.31) 109.44 (0.29) C8 - C7 N1 C9 - Distance Angles C2 1.3426 (0.0046) C10 1.4696 (0.0046) 130.36 (0.32) H9 0.9500 114.82 114.82 C9 - C2 C10 C10 - Distance Angles C11 1.3958 (0.0047) C15 1.4019 (0.0047) 118.73 (0.31) C9 1.4696 (0.0046) 122.25 (0.30) 118.99 (0.30) C10 - C11 C15 C11 - Distance Angles C12 1.3842 (0.0047) C10 1.3958 (0.0047) 121.16 (0.31) H11 0.9500 119.42 119.42 C11 - C12 C10 C12 - Distance Angles C13 1.3796 (0.0047) C11 1.3842 (0.0047) 118.27 (0.31) H12 0.9500 120.86 120.86 C12 - C13 C11 C13 - Distance Angles C14 1.3821 (0.0048) C12 1.3796 (0.0047) 122.52 (0.31) N2 1.4690 (0.0043) 118.51 (0.30) 118.92 (0.30) C13 - C14 C12 C14 - Distance Angles C13 1.3821 (0.0048) C15 1.3835 (0.0047) 118.59 (0.32) H14 0.9500 120.70 120.70 C14 - C13 C15 C15 - Distance Angles C14 1.3835 (0.0047) C10 1.4019 (0.0047) 120.66 (0.32) H15 0.9500 119.67 119.67 C15 - C14 C10 N1 - Distance Angles C1 1.3559 (0.0043) C8 1.4017 (0.0041) 111.43 (0.27) H1 0.8800 124.29 124.29 N1 - C1 C8 N2 - Distance Angles O3 1.2210 (0.0037) O2 1.2290 (0.0038) 123.62 (0.30) C13 1.4690 (0.0043) 118.84 (0.30) 117.55 (0.29) N2 - O3 O2 O1 - Distance Angles C1 1.2345 (0.0039) O1 - O2 - Distance Angles N2 1.2290 (0.0038) O2 - O3 - Distance Angles N2 1.2210 (0.0037) O3 - Specified hydrogen bonds (with su's except fixed and riding H) D-H H...A D...A <(DHA) 0.88 1.98 2.855(4) 173.3 N1-H1...O1_$1 FMAP and GRID set by program FMAP 2 2 12 GRID -2.778 -2 -2 2.778 2 2 R1 = 0.1025 for 2062 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.25 at 0.4753 -0.0019 0.2011 [ 1.46 A from C6 ] Deepest hole -0.26 at 0.5694 0.1299 0.4978 [ 0.80 A from C1 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 2162 / 16629 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5247 1.0019 -0.2011 1.00000 0.05 0.25 1.46 C6 1.59 C7 1.66 H6 1.88 H7 Q2 1 0.3136 0.5414 0.0427 1.00000 0.05 0.24 1.07 O1 1.60 C1 1.71 H12 2.27 H1 Q3 1 0.3572 0.9190 0.0658 1.00000 0.05 0.24 0.83 C2 1.08 C9 1.64 H9 1.90 C1 Q4 1 0.1904 1.6384 0.0947 1.00000 0.05 0.24 1.34 H12 1.65 H9 2.11 O2 2.21 C12 Q5 1 0.4226 1.0289 -0.2988 1.00000 0.05 0.23 0.49 H6 1.37 C6 2.17 O1 2.24 H7 Q6 1 0.2897 0.8556 0.1437 1.00000 0.05 0.23 0.45 H9 1.07 C9 2.01 C10 2.11 C2 Q7 1 0.0738 1.0272 0.2388 1.00000 0.05 0.22 1.59 H15 1.70 C15 1.74 O3 1.96 C14 Q8 1 0.5104 1.0844 -0.1235 1.00000 0.05 0.22 1.96 C6 2.07 C5 2.07 C2 2.13 C7 Q9 1 -0.2314 1.2770 0.1823 1.00000 0.05 0.22 1.73 H14 1.76 O3 2.03 C8 2.18 C7 Q10 1 0.3053 1.2174 0.0755 1.00000 0.05 0.21 0.41 H11 0.86 C11 1.83 C10 2.03 C12 Q11 1 0.1179 1.3521 0.1354 1.00000 0.05 0.21 0.84 C13 0.86 C12 1.55 H12 1.86 C11 Q12 1 0.2894 1.0239 -0.2286 1.00000 0.05 0.21 0.83 C6 1.05 C5 1.45 H6 1.67 H5 Q13 1 -0.1216 1.6944 0.1563 1.00000 0.05 0.20 1.47 O2 1.75 H4 1.83 N2 1.84 O3 Q14 1 0.3657 0.5323 -0.1188 1.00000 0.05 0.20 1.41 H1 1.70 N1 2.00 O3 2.41 O1 Q15 1 0.2139 0.8376 0.1991 1.00000 0.05 0.20 1.42 H9 1.86 H15 2.12 C9 2.27 C15 Q16 1 0.1666 1.0492 0.1382 1.00000 0.05 0.19 0.75 C10 0.97 C15 1.57 H15 1.81 C9 Q17 1 0.0214 0.9151 0.0381 1.00000 0.05 0.19 1.73 H15 1.78 C15 1.99 C10 2.28 C9 Q18 1 -0.0560 0.8435 0.1393 1.00000 0.05 0.19 1.20 H15 1.80 O2 1.85 H4 2.03 C15 Q19 1 0.2577 1.0728 -0.1618 1.00000 0.05 0.19 0.84 C5 0.89 C4 1.57 H5 1.62 H4 Q20 1 0.1434 1.2687 -0.2250 1.00000 0.05 0.19 1.30 H5 1.92 C5 2.27 C14 2.34 O3 Shortest distances between peaks (including symmetry equivalents) 13 20 1.21 12 19 1.25 6 15 1.30 13 18 1.41 3 8 1.41 1 8 1.44 3 6 1.64 1 5 1.65 17 17 1.79 7 20 1.80 2 4 1.81 9 15 1.92 15 16 1.94 5 12 1.94 6 16 1.95 18 20 2.00 19 20 2.04 17 18 2.04 4 6 2.04 7 16 2.05 7 13 2.10 9 14 2.10 6 8 2.15 16 17 2.15 1 6 2.16 18 19 2.23 7 15 2.24 4 15 2.27 1 12 2.28 1 3 2.28 13 19 2.30 7 18 2.30 10 16 2.32 11 20 2.39 3 10 2.43 12 20 2.43 8 19 2.44 11 16 2.44 8 12 2.46 4 11 2.51 10 11 2.53 2 5 2.56 9 12 2.60 11 12 2.60 15 18 2.62 2 10 2.62 7 9 2.64 3 16 2.66 16 20 2.68 5 14 2.75 16 18 2.75 5 8 2.76 2 14 2.76 4 17 2.77 9 19 2.79 6 17 2.82 4 5 2.84 1 10 2.87 15 17 2.87 3 4 2.88 5 10 2.88 1 15 2.89 3 15 2.92 1 19 2.93 13 14 2.96 16 17 2.99 8 10 2.99 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 0.02: Analyse other restraints etc. 0.28: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.08: Structure factors and derivatives 1.48: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.06: Apply other restraints 0.33: Solve l.s. equations 0.00: Generate HTAB table 0.08: Other dependent quantities, CIF, tables 0.02: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2010src0794a finished at 18:25:25 Total CPU time: 3.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++