+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 15:13:44 on 22-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh032 in P2(1)/c CELL 0.71073 13.2432 9.5856 7.4783 90.000 103.345 90.000 ZERR 4.00 0.0003 0.0003 0.0002 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 40 52 4 8 V = 923.69 F(000) = 384.0 Mu = 0.09 mm-1 Cell Wt = 716.86 Rho = 1.289 MERG 2 OMIT -3.00 55.00 OMIT -1 2 1 OMIT -12 0 2 OMIT -6 3 3 DFIX 0.88 0.02 N1 H1N FMAP 2 PLAN 5 ACTA SIZE 0.4 0.1 0.1 EQIV $1 -x, y+1/2, -z-1/2 HTAB N1 O1_$1 HTAB BOND $H L.S. 16 TEMP -153.00 WGHT 0.0336 0.4711 FVAR 1.45663 C1 1 0.153398 0.422390 -0.080832 11.00000 0.01673 0.01688 = 0.01808 -0.00220 0.00257 0.00094 C2 1 0.179963 0.326052 0.060823 11.00000 0.01812 0.02091 = 0.02227 0.00241 0.00530 -0.00184 AFIX 43 H2 2 0.128118 0.267008 0.088927 11.00000 -1.20000 AFIX 0 C3 1 0.282376 0.315292 0.162353 11.00000 0.02096 0.02212 = 0.02080 0.00524 0.00438 0.00073 AFIX 43 H3 2 0.299974 0.249318 0.259362 11.00000 -1.20000 AFIX 0 C4 1 0.358477 0.401174 0.121318 11.00000 0.01624 0.02030 = 0.01942 -0.00114 0.00207 0.00031 C5 1 0.332544 0.496557 -0.022458 11.00000 0.01926 0.01842 = 0.02369 0.00209 0.00423 -0.00331 AFIX 43 H5 2 0.384677 0.554029 -0.052545 11.00000 -1.20000 AFIX 0 C6 1 0.230727 0.507559 -0.121512 11.00000 0.02122 0.01701 = 0.02078 0.00303 0.00296 -0.00034 AFIX 43 H6 2 0.213251 0.573779 -0.218245 11.00000 -1.20000 AFIX 0 C7 1 -0.025746 0.345299 -0.223198 11.00000 0.01974 0.02030 = 0.01921 -0.00347 0.00562 -0.00018 C8 1 -0.127544 0.395372 -0.340588 11.00000 0.01922 0.02676 = 0.02768 -0.00380 0.00101 -0.00006 AFIX 137 H8A 2 -0.149510 0.332816 -0.446061 11.00000 -1.50000 H8B 2 -0.119059 0.490047 -0.384371 11.00000 -1.50000 H8C 2 -0.180247 0.395807 -0.267651 11.00000 -1.50000 AFIX 0 C9 1 0.491000 0.314158 0.372549 11.00000 0.02080 0.02432 = 0.02202 0.00374 0.00112 0.00176 AFIX 23 H9A 2 0.483920 0.214257 0.338365 11.00000 -1.20000 H9B 2 0.446320 0.333971 0.458944 11.00000 -1.20000 AFIX 0 C10 1 0.602839 0.348545 0.460348 11.00000 0.02334 0.02566 = 0.02688 0.00086 -0.00220 -0.00011 AFIX 137 H10A 2 0.647494 0.314307 0.382026 11.00000 -1.50000 H10B 2 0.622761 0.303775 0.581192 11.00000 -1.50000 H10C 2 0.610776 0.449850 0.474754 11.00000 -1.50000 AFIX 0 N1 3 0.050452 0.442134 -0.186107 11.00000 0.01721 0.01719 = 0.02215 0.00097 0.00204 0.00099 O1 4 -0.014396 0.224426 -0.165736 11.00000 0.02584 0.01876 = 0.02941 -0.00024 0.00268 -0.00364 O2 4 0.461507 0.400065 0.211985 11.00000 0.01627 0.02745 = 0.02402 0.00681 0.00146 -0.00165 H1N 2 0.036308 0.526857 -0.237519 11.00000 0.03372 HKLF 4 Covalent radii and connectivity table for 2008lsh032 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 C1 - C2 C6 N1 C2 - C1 C3 C3 - C4 C2 C4 - O2 C3 C5 C5 - C6 C4 C6 - C5 C1 C7 - O1 N1 C8 C8 - C7 C9 - O2 C10 C10 - C9 N1 - C7 C1 O1 - C7 O2 - C4 C9 Operators for generating equivalent atoms: $1 -x, y+1/2, -z-1/2 h k l Fo^2 Sigma Why rejected -7 0 7 33.81 7.78 observed but should be systematically absent 10123 Reflections read, of which 380 rejected -17 =< h =< 16, -12 =< k =< 12, -9 =< l =< 9, Max. 2-theta = 54.97 1 Systematic absence violations 0 Inconsistent equivalents 2105 Unique reflections, of which 0 suppressed R(int) = 0.0259 R(sigma) = 0.0251 Friedel opposites merged Maximum memory for data reduction = 1491 / 20971 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 = 1840 / 157721 wR2 = 0.0961 before cycle 1 for 2105 data and 124 / 124 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.048; Restrained GooF = 1.048 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0336 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.45873 0.00317 0.662 OSF Mean shift/esd = 0.222 Maximum = -0.665 for z C4 Max. shift = 0.002 A for H1N Max. dU =-0.001 for H1N Least-squares cycle 2 Maximum vector length = 511 Memory required = 1840 / 157721 wR2 = 0.0958 before cycle 2 for 2105 data and 124 / 124 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.018 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.047; Restrained GooF = 1.046 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0336 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.45867 0.00316 -0.018 OSF Mean shift/esd = 0.080 Maximum = 0.250 for U11 C2 Max. shift = 0.001 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 3 Maximum vector length = 511 Memory required = 1840 / 157721 wR2 = 0.0957 before cycle 3 for 2105 data and 124 / 124 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.046; Restrained GooF = 1.046 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0336 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.45868 0.00315 0.004 OSF Mean shift/esd = 0.005 Maximum = 0.020 for U23 C3 Max. shift = 0.000 A for H8B Max. dU = 0.000 for C7 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1840 / 157721 wR2 = 0.0957 before cycle 4 for 2105 data and 124 / 124 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.046; Restrained GooF = 1.046 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0336 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.45870 0.00315 0.006 OSF Mean shift/esd = 0.001 Maximum = 0.006 for OSF Max. shift = 0.000 A for H1N Max. dU = 0.000 for C1 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1840 / 157721 wR2 = 0.0957 before cycle 5 for 2105 data and 124 / 124 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.046; Restrained GooF = 1.046 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0336 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.45870 0.00316 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 6 Maximum vector length = 511 Memory required = 1840 / 157721 wR2 = 0.0957 before cycle 6 for 2105 data and 124 / 124 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.046; Restrained GooF = 1.046 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0336 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.45870 0.00316 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y C6 Max. shift = 0.000 A for H1N Max. dU = 0.000 for C9 Least-squares cycle 7 Maximum vector length = 511 Memory required = 1840 / 157721 wR2 = 0.0957 before cycle 7 for 2105 data and 124 / 124 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.046; Restrained GooF = 1.046 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0336 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.45870 0.00316 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y C6 Max. shift = 0.000 A for H10A Max. dU = 0.000 for C3 Least-squares cycle 8 Maximum vector length = 511 Memory required = 1840 / 157721 wR2 = 0.0957 before cycle 8 for 2105 data and 124 / 124 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.046; Restrained GooF = 1.046 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0336 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.45870 0.00316 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y C6 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 9 Maximum vector length = 511 Memory required = 1840 / 157721 wR2 = 0.0957 before cycle 9 for 2105 data and 124 / 124 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.046; Restrained GooF = 1.046 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0336 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.45870 0.00316 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y C6 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 10 Maximum vector length = 511 Memory required = 1840 / 157721 wR2 = 0.0957 before cycle 10 for 2105 data and 124 / 124 parameters Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.046; Restrained GooF = 1.046 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0336 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.45870 0.00316 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y C6 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 11 Maximum vector length = 511 Memory required = 1840 / 157721 wR2 = 0.0957 before cycle 11 for 2105 data and 124 / 124 parameters Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.046; Restrained GooF = 1.046 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0336 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.45870 0.00316 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y C6 Max. shift = 0.000 A for H8B Max. dU = 0.000 for H1N Least-squares cycle 12 Maximum vector length = 511 Memory required = 1840 / 157721 wR2 = 0.0957 before cycle 12 for 2105 data and 124 / 124 parameters Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.046; Restrained GooF = 1.046 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0336 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.45870 0.00316 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y C6 Max. shift = 0.000 A for H8C Max. dU = 0.000 for H1N Least-squares cycle 13 Maximum vector length = 511 Memory required = 1840 / 157721 wR2 = 0.0957 before cycle 13 for 2105 data and 124 / 124 parameters Summary of restraints applied in cycle 13 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.046; Restrained GooF = 1.046 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0336 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.45870 0.00316 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y C6 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 14 Maximum vector length = 511 Memory required = 1840 / 157721 wR2 = 0.0957 before cycle 14 for 2105 data and 124 / 124 parameters Summary of restraints applied in cycle 14 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.046; Restrained GooF = 1.046 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0336 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.45870 0.00316 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y C6 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 15 Maximum vector length = 511 Memory required = 1840 / 157721 wR2 = 0.0957 before cycle 15 for 2105 data and 124 / 124 parameters Summary of restraints applied in cycle 15 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.046; Restrained GooF = 1.046 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0336 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.45870 0.00316 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y C6 Max. shift = 0.000 A for H8C Max. dU = 0.000 for H1N Least-squares cycle 16 Maximum vector length = 511 Memory required = 1840 / 157721 wR2 = 0.0957 before cycle 16 for 2105 data and 124 / 124 parameters Summary of restraints applied in cycle 16 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.046; Restrained GooF = 1.046 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0336 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.45870 0.00316 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y C6 Max. shift = 0.000 A for H1N Max. dU = 0.000 for C1 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 17 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.1282 0.2670 0.0890 43 0.950 0.000 C2 C1 C3 H3 0.3000 0.2495 0.2594 43 0.950 0.000 C3 C4 C2 H5 0.3846 0.5540 -0.0525 43 0.950 0.000 C5 C6 C4 H6 0.2133 0.5737 -0.2182 43 0.950 0.000 C6 C5 C1 H8A -0.1496 0.3326 -0.4459 137 0.980 0.000 C8 C7 H8A H8B -0.1190 0.4899 -0.3846 137 0.980 0.000 C8 C7 H8A H8C -0.1802 0.3960 -0.2675 137 0.980 0.000 C8 C7 H8A H9A 0.4839 0.2143 0.3383 23 0.990 0.000 C9 O2 C10 H9B 0.4463 0.3341 0.4589 23 0.990 0.000 C9 O2 C10 H10A 0.6476 0.3142 0.3821 137 0.980 0.000 C10 C9 H10A H10B 0.6228 0.3039 0.5813 137 0.980 0.000 C10 C9 H10A H10C 0.6109 0.4499 0.4746 137 0.980 0.000 C10 C9 H10A 2008lsh032 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.15345 0.42235 -0.08080 1.00000 0.01668 0.01671 0.01805 -0.00226 0.00272 0.00097 0.01736 0.00204 0.00008 0.00012 0.00015 0.00000 0.00051 0.00051 0.00052 0.00041 0.00041 0.00041 0.00024 C2 0.18000 0.32607 0.06085 1.00000 0.01861 0.02083 0.02211 0.00235 0.00567 -0.00197 0.02036 0.00220 0.00009 0.00012 0.00016 0.00000 0.00054 0.00055 0.00056 0.00044 0.00045 0.00043 0.00025 H2 0.12817 0.26703 0.08897 1.00000 0.02443 0.00000 0.00000 C3 0.28239 0.31537 0.16234 1.00000 0.02126 0.02167 0.02056 0.00523 0.00446 0.00077 0.02122 0.00227 0.00009 0.00012 0.00016 0.00000 0.00056 0.00057 0.00056 0.00044 0.00045 0.00045 0.00025 H3 0.30002 0.24946 0.25942 1.00000 0.02547 0.00000 0.00000 C4 0.35841 0.40122 0.12117 1.00000 0.01617 0.02002 0.01935 -0.00115 0.00215 0.00032 0.01883 0.00210 0.00009 0.00012 0.00016 0.00000 0.00051 0.00055 0.00054 0.00043 0.00042 0.00042 0.00024 C5 0.33247 0.49653 -0.02246 1.00000 0.01942 0.01825 0.02358 0.00207 0.00435 -0.00359 0.02052 0.00218 0.00009 0.00012 0.00016 0.00000 0.00054 0.00054 0.00058 0.00044 0.00045 0.00042 0.00025 H5 0.38459 0.55405 -0.05252 1.00000 0.02462 0.00000 0.00000 C6 0.23073 0.50749 -0.12146 1.00000 0.02171 0.01689 0.02052 0.00306 0.00315 -0.00036 0.01999 0.00217 0.00009 0.00012 0.00016 0.00000 0.00056 0.00053 0.00055 0.00042 0.00044 0.00043 0.00025 H6 0.21325 0.57370 -0.21821 1.00000 0.02398 0.00000 0.00000 C7 -0.02572 0.34533 -0.22320 1.00000 0.02008 0.02039 0.01937 -0.00377 0.00601 -0.00032 0.01971 0.00214 0.00009 0.00012 0.00016 0.00000 0.00055 0.00055 0.00054 0.00043 0.00043 0.00043 0.00025 C8 -0.12752 0.39535 -0.34058 1.00000 0.01931 0.02707 0.02756 -0.00409 0.00117 -0.00034 0.02533 0.00228 0.00009 0.00013 0.00018 0.00000 0.00056 0.00063 0.00063 0.00050 0.00047 0.00047 0.00027 H8A -0.14955 0.33264 -0.44587 1.00000 0.03800 0.00000 0.00000 H8B -0.11901 0.48993 -0.38463 1.00000 0.03800 0.00000 0.00000 H8C -0.18017 0.39599 -0.26755 1.00000 0.03800 0.00000 0.00000 C9 0.49098 0.31423 0.37248 1.00000 0.02104 0.02419 0.02180 0.00393 0.00124 0.00178 0.02295 0.00230 0.00009 0.00013 0.00017 0.00000 0.00057 0.00060 0.00057 0.00046 0.00045 0.00046 0.00026 H9A 0.48389 0.21433 0.33832 1.00000 0.02754 0.00000 0.00000 H9B 0.44630 0.33406 0.45887 1.00000 0.02754 0.00000 0.00000 C10 0.60289 0.34860 0.46036 1.00000 0.02367 0.02539 0.02684 0.00089 -0.00195 -0.00006 0.02656 0.00232 0.00009 0.00014 0.00018 0.00000 0.00061 0.00063 0.00062 0.00049 0.00049 0.00048 0.00028 H10A 0.64756 0.31422 0.38215 1.00000 0.03984 0.00000 0.00000 H10B 0.62276 0.30395 0.58129 1.00000 0.03984 0.00000 0.00000 H10C 0.61086 0.44991 0.47459 1.00000 0.03984 0.00000 0.00000 N1 0.05045 0.44205 -0.18609 1.00000 0.01730 0.01689 0.02205 0.00098 0.00216 0.00100 0.01913 0.00183 0.00007 0.00010 0.00013 0.00000 0.00046 0.00047 0.00049 0.00037 0.00038 0.00036 0.00022 O1 -0.01439 0.22439 -0.16566 1.00000 0.02597 0.01878 0.02949 -0.00028 0.00288 -0.00362 0.02532 0.00159 0.00007 0.00009 0.00012 0.00000 0.00046 0.00042 0.00048 0.00034 0.00036 0.00034 0.00022 O2 0.46149 0.40008 0.21196 1.00000 0.01647 0.02747 0.02384 0.00689 0.00144 -0.00165 0.02311 0.00157 0.00006 0.00009 0.00011 0.00000 0.00040 0.00046 0.00044 0.00035 0.00033 0.00033 0.00021 H1N 0.03643 0.52657 -0.23737 1.00000 0.03276 0.02918 0.00115 0.00146 0.00207 0.00000 0.00412 Final Structure Factor Calculation for 2008lsh032 in P2(1)/c Total number of l.s. parameters = 124 Maximum vector length = 511 Memory required = 1716 / 22995 wR2 = 0.0957 before cycle 17 for 2105 data and 0 / 124 parameters Summary of restraints applied in cycle 17 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.046; Restrained GooF = 1.046 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0336 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0395 for 1909 Fo > 4sig(Fo) and 0.0442 for all 2105 data wR2 = 0.0957, GooF = S = 1.046, Restrained GooF = 1.046 for all data Occupancy sum of asymmetric unit = 13.00 for non-hydrogen and 13.00 for hydrogen atoms Principal mean square atomic displacements U 0.0210 0.0162 0.0149 C1 0.0242 0.0209 0.0160 C2 0.0264 0.0214 0.0159 C3 0.0218 0.0191 0.0156 C4 0.0256 0.0213 0.0147 C5 0.0244 0.0204 0.0151 C6 0.0238 0.0199 0.0154 C7 0.0331 0.0248 0.0180 C8 0.0278 0.0244 0.0166 C9 0.0356 0.0254 0.0187 C10 0.0238 0.0180 0.0156 N1 0.0331 0.0257 0.0172 O1 0.0344 0.0191 0.0158 O2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.016 0.031 0.047 0.064 0.087 0.110 0.141 0.187 0.272 1.000 Number in group 211. 212. 219. 204. 214. 205. 210. 208. 210. 212. GooF 1.119 1.075 1.092 1.021 0.989 0.970 1.099 1.111 1.024 0.941 K 2.119 1.096 1.011 0.996 0.984 1.000 1.008 1.006 1.003 1.006 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.65 inf Number in group 215. 218. 200. 212. 209. 211. 209. 210. 212. 209. GooF 1.074 1.191 1.002 0.935 0.845 1.007 0.961 0.872 1.102 1.359 K 1.040 1.052 1.037 1.013 0.993 0.995 0.990 0.998 1.009 1.006 R1 0.091 0.096 0.066 0.061 0.042 0.045 0.035 0.025 0.034 0.028 Recommended weighting scheme: WGHT 0.0296 0.4844 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) 0 3 3 25.80 10.39 4.88 0.049 1.93 1 2 0 16.43 6.96 4.15 0.040 4.49 10 1 3 152.16 199.26 3.90 0.215 1.04 1 4 2 68.43 47.06 3.86 0.104 1.94 -3 4 2 25.40 13.84 3.79 0.057 1.91 12 1 1 47.89 68.85 3.47 0.126 1.02 -5 9 6 0.68 8.55 3.46 0.045 0.80 -5 4 1 137.94 108.14 3.35 0.158 1.77 1 2 1 279.61 335.37 3.30 0.279 3.69 -9 9 5 14.07 5.93 3.16 0.037 0.79 12 5 3 136.37 103.80 3.09 0.155 0.82 5 0 2 97.29 75.82 3.03 0.133 1.91 11 1 2 112.85 141.83 3.01 0.181 1.04 6 0 2 41.08 57.06 2.94 0.115 1.69 -1 7 7 5.84 1.71 2.91 0.020 0.84 -7 2 3 68.81 51.76 2.89 0.110 1.57 10 0 2 355.98 415.66 2.81 0.310 1.13 5 10 4 4.41 0.38 2.81 0.009 0.78 -10 10 1 63.44 86.07 2.75 0.141 0.78 15 3 1 64.84 43.89 2.74 0.101 0.80 -10 5 6 73.60 55.21 2.74 0.113 0.89 14 1 2 35.36 23.56 2.73 0.074 0.84 1 8 5 13.93 22.97 2.72 0.073 0.91 -3 6 3 110.63 84.07 2.72 0.140 1.32 11 3 2 6.95 13.45 2.71 0.056 0.99 -9 8 1 48.89 35.66 2.64 0.091 0.93 -8 0 2 54.19 70.73 2.63 0.128 1.62 1 7 6 18.37 28.00 2.60 0.081 0.89 8 0 2 81.77 101.83 2.59 0.154 1.36 12 8 0 -0.93 1.49 2.58 0.019 0.80 -4 11 1 4.32 0.30 2.57 0.008 0.84 -11 8 3 120.97 97.50 2.56 0.150 0.84 2 10 4 31.14 21.13 2.54 0.070 0.83 2 0 0 1928.12 2165.16 2.53 0.708 6.44 -5 2 4 84.34 103.94 2.51 0.155 1.59 2 6 5 5.73 2.23 2.50 0.023 1.03 -3 6 6 4.08 1.10 2.48 0.016 0.98 16 1 0 206.66 169.61 2.48 0.198 0.80 5 3 2 561.76 500.76 2.46 0.341 1.64 -3 1 5 12.32 7.03 2.46 0.040 1.47 0 5 2 326.79 286.38 2.45 0.258 1.70 1 2 3 187.61 160.64 2.45 0.193 2.07 4 5 1 71.11 88.64 2.44 0.143 1.57 -2 5 2 113.24 93.84 2.43 0.147 1.69 2 6 4 6.00 2.56 2.43 0.024 1.15 -2 7 3 2.50 0.48 2.42 0.010 1.20 14 0 2 84.64 64.58 2.42 0.122 0.85 3 6 6 5.33 1.95 2.41 0.021 0.91 0 5 6 0.15 2.42 2.40 0.024 1.02 -9 0 8 0.86 5.29 2.38 0.035 0.86 Bond lengths and angles C1 - Distance Angles C2 1.3876 (0.0016) C6 1.3963 (0.0016) 119.05 (0.10) N1 1.4214 (0.0014) 123.57 (0.10) 117.36 (0.10) C1 - C2 C6 C2 - Distance Angles C1 1.3876 (0.0016) C3 1.3964 (0.0016) 120.46 (0.10) H2 0.9500 119.77 119.77 C2 - C1 C3 C3 - Distance Angles C4 1.3887 (0.0016) C2 1.3964 (0.0016) 119.91 (0.11) H3 0.9500 120.04 120.04 C3 - C4 C2 C4 - Distance Angles O2 1.3772 (0.0013) C3 1.3887 (0.0016) 124.95 (0.10) C5 1.3915 (0.0016) 115.20 (0.10) 119.85 (0.10) C4 - O2 C3 C5 - Distance Angles C6 1.3835 (0.0016) C4 1.3915 (0.0016) 119.96 (0.11) H5 0.9500 120.02 120.02 C5 - C6 C4 C6 - Distance Angles C5 1.3835 (0.0016) C1 1.3963 (0.0016) 120.75 (0.11) H6 0.9500 119.62 119.62 C6 - C5 C1 C7 - Distance Angles O1 1.2336 (0.0015) N1 1.3509 (0.0015) 123.26 (0.11) C8 1.5072 (0.0016) 121.50 (0.11) 115.24 (0.10) C7 - O1 N1 C8 - Distance Angles C7 1.5072 (0.0016) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - C7 H8A H8B C9 - Distance Angles O2 1.4333 (0.0014) C10 1.5123 (0.0016) 106.81 (0.10) H9A 0.9900 110.36 110.36 H9B 0.9900 110.36 110.36 108.59 C9 - O2 C10 H9A C10 - Distance Angles C9 1.5123 (0.0016) H10A 0.9800 109.47 H10B 0.9800 109.47 109.47 H10C 0.9800 109.47 109.47 109.47 C10 - C9 H10A H10B N1 - Distance Angles C7 1.3509 (0.0015) C1 1.4214 (0.0014) 126.74 (0.10) H1N 0.8972 (0.0131) 117.44 (0.98) 115.73 (0.98) N1 - C7 C1 O1 - Distance Angles C7 1.2336 (0.0015) O1 - O2 - Distance Angles C4 1.3772 (0.0013) C9 1.4333 (0.0014) 117.70 (0.09) O2 - C4 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.897(13) 2.027(13) 2.9219(13) 174.9(14) N1-H1N...O1_$1 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)