+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 05src0044 started at 11:13:19 on 20-Jan-2005 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 05src0044 in P2(1)/n CELL 0.71073 6.2302 7.2368 13.1129 90.000 90.852 90.000 ZERR 4.00 0.0019 0.0011 0.0119 0.000 0.044 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 20 16 16 12 V = 591.15 F(000) = 344.0 Mu = 0.16 mm-1 Cell Wt = 672.49 Rho = 1.889 MERG 2 OMIT -3.00 55.00 OMIT 0 0 2 OMIT -1 2 1 OMIT 1 2 2 OMIT -1 2 6 OMIT -1 2 4 OMIT 1 2 1 EXTI 0.08580 SHEL 7 0.77 EQIV $1 X-1/2, -Y+1/2, Z-1/2 EQIV $2 -X-1, -Y, -Z+1 EQIV $3 -X+1, -Y+1, -Z+1 EQIV $4 -X-1/2, Y+1/2, -Z+1/2 HTAB N1 O2_$1 HTAB N2 O1_$2 HTAB N3 O3_$3 HTAB N4 O1_$4 FMAP 2 PLAN 5 SIZE 0.02 0.07 0.10 ACTA BOND $H WGHT 0.05070 1.70900 L.S. 20 TEMP -153.00 FVAR 1.16796 MOLE 1 C1 1 -0.358113 0.111428 0.381510 11.00000 0.02017 0.02078 = 0.01761 0.00093 0.00026 0.00132 C2 1 -0.051108 0.265116 0.364878 11.00000 0.01998 0.01657 = 0.01673 -0.00203 -0.00083 0.00396 C3 1 -0.071973 0.217184 0.464992 11.00000 0.01859 0.01851 = 0.01986 -0.00083 -0.00077 -0.00031 C4 1 0.085845 0.266122 0.538269 11.00000 0.02018 0.01674 = 0.01952 -0.00131 0.00059 0.00134 C5 1 0.275228 0.420146 0.395407 11.00000 0.01855 0.01952 = 0.02266 -0.00293 -0.00211 0.00166 N1 3 -0.226719 0.200433 0.313194 11.00000 0.01795 0.02094 = 0.01575 -0.00121 0.00126 0.00043 N2 3 -0.264220 0.124571 0.475029 11.00000 0.01867 0.02157 = 0.01815 0.00114 0.00067 -0.00041 N3 3 0.255321 0.363748 0.494082 11.00000 0.01659 0.01981 = 0.02094 -0.00281 -0.00352 -0.00101 N4 3 0.114893 0.365181 0.328606 11.00000 0.01890 0.02354 = 0.01772 0.00075 -0.00202 -0.00099 O1 4 -0.531817 0.032549 0.359743 11.00000 0.02056 0.02667 = 0.01921 -0.00111 0.00083 -0.00285 O2 4 0.081870 0.231667 0.630244 11.00000 0.02542 0.02680 = 0.01578 -0.00176 -0.00197 0.00052 O3 4 0.426423 0.515881 0.367588 11.00000 0.02001 0.02819 = 0.02301 -0.00070 -0.00240 -0.00407 H1 2 -0.261144 0.223657 0.244436 11.00000 0.01986 H2 2 -0.306860 0.080318 0.535321 11.00000 0.02551 H3 2 0.358692 0.395416 0.544906 11.00000 0.03452 H4 2 0.127106 0.409388 0.270102 11.00000 0.03153 HKLF 4 Covalent radii and connectivity table for 05src0044 in P2(1)/n C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1 N2 N1 C2 - N4 N1 C3 C3 - C2 N2 C4 C4 - O2 N3 C3 C5 - O3 N3 N4 N1 - C2 C1 N2 - C1 C3 N3 - C5 C4 N4 - C2 C5 O1 - C1 O2 - C4 O3 - C5 Operators for generating equivalent atoms: $1 x-1/2, -y+1/2, z-1/2 $2 -x-1, -y, -z+1 $3 -x+1, -y+1, -z+1 $4 -x-1/2, y+1/2, -z+1/2 5709 Reflections read, of which 270 rejected -8 =< h =< 7, -8 =< k =< 9, -17 =< l =< 14, Max. 2-theta = 54.95 0 Systematic absence violations 0 Inconsistent equivalents 1348 Unique reflections, of which 0 suppressed R(int) = 0.0481 R(sigma) = 0.0439 Friedel opposites merged Maximum memory for data reduction = 1239 / 13564 Least-squares cycle 1 Maximum vector length = 511 Memory required = 1515 / 160020 wR2 = 0.1780 before cycle 1 for 1348 data and 126 / 126 parameters GooF = S = 1.173; Restrained GooF = 1.173 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0507 * P )^2 + 1.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.16759 0.00824 -0.045 OSF 2 0.08535 0.01340 -0.034 EXTI Mean shift/esd = 0.007 Maximum = -0.045 for OSF Max. shift = 0.001 A for H4 Max. dU = 0.000 for H4 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1515 / 160020 wR2 = 0.1780 before cycle 2 for 1348 data and 126 / 126 parameters GooF = S = 1.174; Restrained GooF = 1.174 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0507 * P )^2 + 1.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.16746 0.00824 -0.015 OSF 2 0.08516 0.01337 -0.015 EXTI Mean shift/esd = 0.003 Maximum = -0.015 for OSF Max. shift = 0.000 A for H4 Max. dU = 0.000 for H4 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1515 / 160020 wR2 = 0.1780 before cycle 3 for 1348 data and 126 / 126 parameters GooF = S = 1.174; Restrained GooF = 1.174 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0507 * P )^2 + 1.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.16745 0.00824 -0.001 OSF 2 0.08514 0.01336 -0.001 EXTI Mean shift/esd = 0.000 Maximum = 0.004 for U11 H4 Max. shift = 0.000 A for H4 Max. dU = 0.000 for H4 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1515 / 160020 wR2 = 0.1780 before cycle 4 for 1348 data and 126 / 126 parameters GooF = S = 1.174; Restrained GooF = 1.174 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0507 * P )^2 + 1.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.16745 0.00824 0.000 OSF 2 0.08514 0.01335 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.002 for x H4 Max. shift = 0.000 A for H4 Max. dU = 0.000 for H4 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1515 / 160020 wR2 = 0.1780 before cycle 5 for 1348 data and 126 / 126 parameters GooF = S = 1.174; Restrained GooF = 1.174 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0507 * P )^2 + 1.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.16746 0.00824 0.000 OSF 2 0.08514 0.01335 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for x H4 Max. shift = 0.000 A for H4 Max. dU = 0.000 for H4 Least-squares cycle 6 Maximum vector length = 511 Memory required = 1515 / 160020 wR2 = 0.1780 before cycle 6 for 1348 data and 126 / 126 parameters GooF = S = 1.174; Restrained GooF = 1.174 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0507 * P )^2 + 1.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.16746 0.00824 0.000 OSF 2 0.08514 0.01335 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for x H4 Max. shift = 0.000 A for H4 Max. dU = 0.000 for H4 Least-squares cycle 7 Maximum vector length = 511 Memory required = 1515 / 160020 wR2 = 0.1780 before cycle 7 for 1348 data and 126 / 126 parameters GooF = S = 1.174; Restrained GooF = 1.174 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0507 * P )^2 + 1.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.16746 0.00824 0.000 OSF 2 0.08514 0.01335 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x H4 Max. shift = 0.000 A for H4 Max. dU = 0.000 for H4 Least-squares cycle 8 Maximum vector length = 511 Memory required = 1515 / 160020 wR2 = 0.1780 before cycle 8 for 1348 data and 126 / 126 parameters GooF = S = 1.174; Restrained GooF = 1.174 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0507 * P )^2 + 1.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.16746 0.00824 0.000 OSF 2 0.08514 0.01335 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H4 Max. dU = 0.000 for H4 Least-squares cycle 9 Maximum vector length = 511 Memory required = 1515 / 160020 wR2 = 0.1780 before cycle 9 for 1348 data and 126 / 126 parameters GooF = S = 1.174; Restrained GooF = 1.174 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0507 * P )^2 + 1.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.16746 0.00824 0.000 OSF 2 0.08514 0.01335 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H4 Max. dU = 0.000 for H4 Least-squares cycle 10 Maximum vector length = 511 Memory required = 1515 / 160020 wR2 = 0.1780 before cycle 10 for 1348 data and 126 / 126 parameters GooF = S = 1.174; Restrained GooF = 1.174 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0507 * P )^2 + 1.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.16746 0.00824 0.000 OSF 2 0.08514 0.01335 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z C4 Max. shift = 0.000 A for H3 Max. dU = 0.000 for H4 Least-squares cycle 11 Maximum vector length = 511 Memory required = 1515 / 160020 wR2 = 0.1780 before cycle 11 for 1348 data and 126 / 126 parameters GooF = S = 1.174; Restrained GooF = 1.174 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0507 * P )^2 + 1.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.16746 0.00824 0.000 OSF 2 0.08514 0.01335 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z C4 Max. shift = 0.000 A for H4 Max. dU = 0.000 for H4 Least-squares cycle 12 Maximum vector length = 511 Memory required = 1515 / 160020 wR2 = 0.1780 before cycle 12 for 1348 data and 126 / 126 parameters GooF = S = 1.174; Restrained GooF = 1.174 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0507 * P )^2 + 1.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.16746 0.00824 0.000 OSF 2 0.08514 0.01335 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z C4 Max. shift = 0.000 A for H3 Max. dU = 0.000 for H4 Least-squares cycle 13 Maximum vector length = 511 Memory required = 1515 / 160020 wR2 = 0.1780 before cycle 13 for 1348 data and 126 / 126 parameters GooF = S = 1.174; Restrained GooF = 1.174 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0507 * P )^2 + 1.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.16746 0.00824 0.000 OSF 2 0.08514 0.01335 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z C4 Max. shift = 0.000 A for H2 Max. dU = 0.000 for H3 Least-squares cycle 14 Maximum vector length = 511 Memory required = 1515 / 160020 wR2 = 0.1780 before cycle 14 for 1348 data and 126 / 126 parameters GooF = S = 1.174; Restrained GooF = 1.174 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0507 * P )^2 + 1.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.16746 0.00824 0.000 OSF 2 0.08514 0.01335 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z C4 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H4 Least-squares cycle 15 Maximum vector length = 511 Memory required = 1515 / 160020 wR2 = 0.1780 before cycle 15 for 1348 data and 126 / 126 parameters GooF = S = 1.174; Restrained GooF = 1.174 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0507 * P )^2 + 1.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.16746 0.00824 0.000 OSF 2 0.08514 0.01335 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z C4 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H1 Least-squares cycle 16 Maximum vector length = 511 Memory required = 1515 / 160020 wR2 = 0.1780 before cycle 16 for 1348 data and 126 / 126 parameters GooF = S = 1.174; Restrained GooF = 1.174 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0507 * P )^2 + 1.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.16746 0.00824 0.000 OSF 2 0.08514 0.01335 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z C4 Max. shift = 0.000 A for H2 Max. dU = 0.000 for H3 Least-squares cycle 17 Maximum vector length = 511 Memory required = 1515 / 160020 wR2 = 0.1780 before cycle 17 for 1348 data and 126 / 126 parameters GooF = S = 1.174; Restrained GooF = 1.174 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0507 * P )^2 + 1.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.16746 0.00824 0.000 OSF 2 0.08514 0.01335 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z C4 Max. shift = 0.000 A for H2 Max. dU = 0.000 for H2 Least-squares cycle 18 Maximum vector length = 511 Memory required = 1515 / 160020 wR2 = 0.1780 before cycle 18 for 1348 data and 126 / 126 parameters GooF = S = 1.174; Restrained GooF = 1.174 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0507 * P )^2 + 1.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.16746 0.00824 0.000 OSF 2 0.08514 0.01335 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z C4 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H4 Least-squares cycle 19 Maximum vector length = 511 Memory required = 1515 / 160020 wR2 = 0.1780 before cycle 19 for 1348 data and 126 / 126 parameters GooF = S = 1.174; Restrained GooF = 1.174 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0507 * P )^2 + 1.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.16746 0.00824 0.000 OSF 2 0.08514 0.01335 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H1 Max. dU = 0.000 for N1 Least-squares cycle 20 Maximum vector length = 511 Memory required = 1515 / 160020 wR2 = 0.1780 before cycle 20 for 1348 data and 126 / 126 parameters GooF = S = 1.174; Restrained GooF = 1.174 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0507 * P )^2 + 1.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.16746 0.00824 0.000 OSF 2 0.08514 0.01335 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z C4 Max. shift = 0.000 A for H4 Max. dU = 0.000 for H4 Largest correlation matrix elements 0.648 EXTI / OSF 05src0044 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.35812 0.11143 0.38151 1.00000 0.02015 0.02075 0.01759 0.00094 0.00025 0.00131 0.01950 0.00550 0.00050 0.00043 0.00024 0.00000 0.00150 0.00155 0.00155 0.00115 0.00115 0.00115 0.00070 C2 -0.05111 0.26512 0.36488 1.00000 0.01997 0.01655 0.01669 -0.00202 -0.00083 0.00396 0.01775 0.00522 0.00048 0.00042 0.00023 0.00000 0.00148 0.00143 0.00146 0.00112 0.00113 0.00113 0.00065 C3 -0.07197 0.21719 0.46499 1.00000 0.01857 0.01850 0.01984 -0.00083 -0.00076 -0.00031 0.01898 0.00533 0.00049 0.00043 0.00024 0.00000 0.00146 0.00145 0.00156 0.00115 0.00116 0.00116 0.00068 C4 0.08584 0.26612 0.53827 1.00000 0.02015 0.01672 0.01952 -0.00132 0.00059 0.00134 0.01879 0.00535 0.00049 0.00042 0.00024 0.00000 0.00148 0.00143 0.00152 0.00114 0.00115 0.00114 0.00067 C5 0.27523 0.42015 0.39541 1.00000 0.01852 0.01951 0.02264 -0.00294 -0.00212 0.00166 0.02024 0.00536 0.00049 0.00043 0.00025 0.00000 0.00149 0.00149 0.00163 0.00121 0.00120 0.00118 0.00070 N1 -0.22672 0.20043 0.31319 1.00000 0.01793 0.02092 0.01573 -0.00120 0.00127 0.00043 0.01818 0.00455 0.00041 0.00036 0.00021 0.00000 0.00126 0.00135 0.00133 0.00101 0.00097 0.00099 0.00063 N2 -0.26422 0.12457 0.47503 1.00000 0.01866 0.02156 0.01811 0.00114 0.00067 -0.00042 0.01944 0.00467 0.00042 0.00037 0.00022 0.00000 0.00128 0.00136 0.00138 0.00105 0.00100 0.00102 0.00063 N3 0.25532 0.36375 0.49408 1.00000 0.01658 0.01978 0.02091 -0.00280 -0.00351 -0.00102 0.01913 0.00451 0.00041 0.00036 0.00021 0.00000 0.00127 0.00134 0.00141 0.00102 0.00101 0.00100 0.00063 N4 0.11489 0.36518 0.32861 1.00000 0.01887 0.02350 0.01772 0.00074 -0.00201 -0.00099 0.02005 0.00466 0.00042 0.00039 0.00022 0.00000 0.00131 0.00140 0.00141 0.00109 0.00102 0.00103 0.00064 O1 -0.53182 0.03255 0.35974 1.00000 0.02054 0.02665 0.01919 -0.00110 0.00083 -0.00284 0.02212 0.00385 0.00035 0.00032 0.00017 0.00000 0.00112 0.00124 0.00118 0.00091 0.00086 0.00091 0.00058 O2 0.08187 0.23167 0.63025 1.00000 0.02541 0.02678 0.01574 -0.00175 -0.00197 0.00053 0.02266 0.00388 0.00037 0.00032 0.00017 0.00000 0.00118 0.00124 0.00114 0.00089 0.00087 0.00093 0.00058 O3 0.42642 0.51588 0.36759 1.00000 0.01999 0.02816 0.02299 -0.00070 -0.00239 -0.00406 0.02374 0.00385 0.00035 0.00033 0.00018 0.00000 0.00112 0.00129 0.00127 0.00094 0.00089 0.00092 0.00060 H1 -0.26108 0.22367 0.24443 1.00000 0.01984 0.06645 0.00574 0.00537 0.00304 0.00000 0.00928 H2 -0.30692 0.08030 0.53528 1.00000 0.02553 0.07003 0.00635 0.00557 0.00342 0.00000 0.00997 H3 0.35869 0.39548 0.54487 1.00000 0.03457 0.08130 0.00719 0.00595 0.00354 0.00000 0.01125 H4 0.12728 0.40948 0.27003 1.00000 0.03183 0.07524 0.00695 0.00606 0.00364 0.00000 0.01132 Final Structure Factor Calculation for 05src0044 in P2(1)/n Total number of l.s. parameters = 126 Maximum vector length = 511 Memory required = 1389 / 22995 wR2 = 0.1780 before cycle 21 for 1348 data and 0 / 126 parameters GooF = S = 1.174; Restrained GooF = 1.174 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0507 * P )^2 + 1.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0675 for 1159 Fo > 4sig(Fo) and 0.0771 for all 1348 data wR2 = 0.1780, GooF = S = 1.174, Restrained GooF = 1.174 for all data Occupancy sum of asymmetric unit = 12.00 for non-hydrogen and 4.00 for hydrogen atoms Principal mean square atomic displacements U 0.0219 0.0193 0.0173 C1 0.0233 0.0165 0.0135 C2 0.0206 0.0188 0.0175 C3 0.0207 0.0200 0.0158 C4 0.0257 0.0178 0.0173 C5 0.0212 0.0183 0.0150 N1 0.0219 0.0189 0.0175 N2 0.0241 0.0197 0.0136 N3 0.0240 0.0202 0.0160 N4 0.0279 0.0194 0.0190 O1 0.0275 0.0254 0.0150 O2 0.0299 0.0243 0.0171 O3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.014 0.027 0.037 0.051 0.064 0.081 0.104 0.135 0.184 1.000 Number in group 143. 141. 126. 132. 135. 133. 134. 138. 133. 133. GooF 1.427 1.174 0.949 1.054 1.169 1.012 1.444 1.032 0.827 1.433 K 5.870 1.521 1.207 1.082 1.058 1.032 1.097 1.007 1.004 1.017 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.62 inf Number in group 135. 135. 141. 130. 133. 134. 136. 138. 131. 135. GooF 0.730 0.821 0.834 0.788 0.744 1.123 1.243 1.249 1.476 2.039 K 0.981 1.025 1.048 1.025 0.990 1.051 1.018 1.007 1.026 1.027 R1 0.128 0.139 0.099 0.076 0.075 0.068 0.059 0.073 0.062 0.070 Recommended weighting scheme: WGHT 0.0505 1.7115 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) 2 4 2 733.73 365.73 6.19 0.205 1.52 -1 2 3 744.17 445.65 5.92 0.226 2.55 2 4 8 184.43 61.18 5.81 0.084 1.13 1 0 5 216.89 64.00 5.75 0.086 2.40 2 2 3 38.24 1.36 5.32 0.013 2.07 -3 6 3 149.89 64.27 5.14 0.086 1.02 3 6 2 211.44 79.17 5.06 0.095 1.03 -2 2 6 37.05 0.14 4.80 0.004 1.61 1 4 8 36.53 3.87 4.79 0.021 1.19 1 1 7 89.77 31.57 4.52 0.060 1.73 3 0 3 216.31 51.16 4.33 0.077 1.86 -1 0 9 62.79 12.91 4.32 0.038 1.42 1 2 5 101.12 39.08 4.30 0.067 2.00 1 4 1 57.75 14.88 3.99 0.041 1.72 1 0 1 86.43 33.78 3.95 0.062 5.59 1 2 8 17.21 0.04 3.89 0.002 1.45 -2 4 6 46.81 10.95 3.87 0.035 1.28 -1 0 7 206.85 121.37 3.75 0.118 1.80 -3 0 1 77.56 34.11 3.70 0.063 2.06 2 2 2 243.76 155.30 3.63 0.133 2.21 -1 3 4 20.32 3.65 3.49 0.020 1.86 -2 0 10 356.70 89.34 3.47 0.101 1.21 -3 1 3 150.13 84.33 3.25 0.098 1.83 -1 0 1 1100.14 1521.86 3.22 0.418 5.66 -1 1 9 13.31 0.86 3.19 0.010 1.40 -4 2 1 100.21 54.45 3.17 0.079 1.42 2 4 3 26.58 8.07 3.14 0.030 1.47 -2 6 3 23.13 6.03 3.10 0.026 1.09 -2 8 5 41.67 9.37 3.06 0.033 0.83 -3 1 4 41.11 15.89 3.04 0.043 1.72 1 6 6 170.36 110.74 2.97 0.113 1.04 2 0 8 55.82 2.74 2.94 0.018 1.44 -2 5 11 21.34 2.32 2.92 0.016 0.89 -2 0 2 645.46 438.02 2.92 0.224 2.83 1 0 15 30.36 5.02 2.91 0.024 0.86 5 3 3 16.75 0.85 2.90 0.010 1.07 -1 5 5 48.03 22.74 2.88 0.051 1.24 1 5 4 62.81 32.18 2.87 0.061 1.29 -5 3 1 52.31 24.49 2.82 0.053 1.10 1 0 3 143.05 92.04 2.81 0.103 3.55 2 0 0 9.43 0.86 2.80 0.010 3.11 0 0 6 5023.42 4158.45 2.74 0.691 2.19 -5 2 1 252.46 180.95 2.67 0.144 1.17 -1 4 9 9.66 0.81 2.63 0.010 1.12 -2 1 9 12.14 0.66 2.63 0.009 1.31 4 4 1 12.57 1.83 2.58 0.014 1.17 1 5 12 8.73 0.08 2.47 0.003 0.86 -2 0 4 2315.30 1914.17 2.38 0.469 2.27 -1 6 2 36.22 17.82 2.38 0.045 1.17 -4 4 2 35.68 7.25 2.35 0.029 1.16 Bond lengths and angles C1 - Distance Angles O1 1.2527 (0.0038) N2 1.3542 (0.0043) 126.76 (0.30) N1 1.3818 (0.0041) 125.65 (0.29) 107.59 (0.27) C1 - O1 N2 C2 - Distance Angles N4 1.3546 (0.0042) N1 1.3614 (0.0039) 128.40 (0.29) C3 1.3659 (0.0045) 123.87 (0.28) 107.69 (0.28) C2 - N4 N1 C3 - Distance Angles C2 1.3659 (0.0045) N2 1.3805 (0.0041) 108.06 (0.27) C4 1.4097 (0.0044) 121.06 (0.29) 130.87 (0.30) C3 - C2 N2 C4 - Distance Angles O2 1.2322 (0.0040) N3 1.4028 (0.0041) 122.17 (0.28) C3 1.4097 (0.0044) 126.32 (0.30) 111.51 (0.28) C4 - O2 N3 C5 - Distance Angles O3 1.2291 (0.0040) N3 1.3642 (0.0044) 122.08 (0.28) N4 1.3774 (0.0040) 121.72 (0.31) 116.20 (0.29) C5 - O3 N3 N1 - Distance Angles C2 1.3614 (0.0039) C1 1.3818 (0.0041) 108.48 (0.27) H1 0.9388 (0.0393) 125.92 (2.29) 125.26 (2.27) N1 - C2 C1 N2 - Distance Angles C1 1.3542 (0.0043) C3 1.3805 (0.0041) 108.15 (0.27) H2 0.8966 (0.0448) 130.02 (2.61) 121.79 (2.60) N2 - C1 C3 N3 - Distance Angles C5 1.3642 (0.0044) C4 1.4028 (0.0041) 128.46 (0.27) H3 0.9478 (0.0470) 121.58 (2.71) 109.85 (2.69) N3 - C5 C4 N4 - Distance Angles C2 1.3546 (0.0042) C5 1.3774 (0.0040) 118.78 (0.28) H4 0.8370 (0.0473) 127.47 (3.00) 113.40 (3.00) N4 - C2 C5 O1 - Distance Angles C1 1.2527 (0.0038) O1 - O2 - Distance Angles C4 1.2322 (0.0040) O2 - O3 - Distance Angles C5 1.2291 (0.0040) O3 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.94(4) 1.81(4) 2.708(4) 160(3) N1-H1...O2_$1 0.90(4) 1.90(4) 2.772(4) 163(4) N2-H2...O1_$2 0.95(5) 1.86(5) 2.806(4) 172(4) N3-H3...O3_$3 0.84(5) 2.00(5) 2.792(4) 157(4) N4-H4...O1_$4 FMAP and GRID set by program FMAP 2 1 10 GRID -3.571 -2 -2 3.571 2 2 R1 = 0.0771 for 1348 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.38 at 0.0438 0.8129 0.3683 [ 0.85 A from O2 ] Deepest hole -0.35 at 0.1927 0.5185 0.3833 [ 0.89 A from C5 ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 1569 / 13515 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.0438 0.1871 0.6317 1.00000 0.05 0.38 0.85 O2 1.58 C4 2.20 H2 2.20 C3 Q2 1 0.4058 0.5205 0.2810 1.00000 0.05 0.36 1.14 O3 1.86 C5 1.92 H4 2.23 N4 Q3 1 0.2743 0.4223 0.2809 1.00000 0.05 0.31 0.93 H4 1.25 N4 1.50 C5 1.62 O3 Q4 1 0.4205 0.3669 0.3481 1.00000 0.05 0.28 1.11 O3 1.17 C5 1.92 N4 2.10 H4 Q5 1 0.4212 0.4817 0.4529 1.00000 0.05 0.28 1.15 O3 1.25 C5 1.42 H3 1.45 N3 Shortest distances between peaks (including symmetry equivalents) 2 3 1.08 3 4 1.32 2 4 1.42 5 5 1.59 4 5 1.61 2 5 2.27 1 3 2.41 3 5 2.46 1 2 2.49 1 4 2.88 4 5 2.98 Time profile in seconds ----------------------- 0.04: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.01: 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. 0.20: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.56: Structure factors and derivatives 0.72: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.05: Apply other restraints 0.20: Solve l.s. equations 0.00: Generate HTAB table 0.04: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.01: Merge reflections for Fourier and .fcf 0.01: Fourier summations 0.01: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 05src0044 finished at 11:13:21 Total CPU time: 2.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++