+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 20:20:48 on 11-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh171 in P2(1)/n CELL 0.71073 11.1083 4.8283 15.2681 90.000 99.170 90.000 ZERR 4.00 0.0006 0.0003 0.0007 0.000 0.003 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 36 44 4 4 V = 808.43 F(000) = 320.0 Mu = 0.08 mm-1 Cell Wt = 596.75 Rho = 1.226 MERG 2 OMIT -3.00 55.00 DFIX 0.88 0.02 N1 H1N FMAP 2 PLAN 5 ACTA EQIV $1 x, y+1, z HTAB N1 O1_$1 HTAB SIZE 0.21 0.1 0.06 BOND $H L.S. 16 TEMP -153.00 WGHT 0.066100 0.510000 FVAR 1.56852 C1 1 0.303482 -0.037606 0.006476 11.00000 0.02463 0.01708 = 0.02500 -0.00033 0.00520 -0.00269 C2 1 0.195517 0.060522 -0.043205 11.00000 0.02512 0.01667 = 0.02790 0.00141 0.00726 -0.00003 C3 1 0.163395 -0.039927 -0.129446 11.00000 0.02882 0.02360 = 0.02638 0.00201 0.00294 0.00038 AFIX 43 H3 2 0.090497 0.024265 -0.164692 11.00000 -1.20000 AFIX 0 C4 1 0.235402 -0.231456 -0.165003 11.00000 0.03612 0.02416 = 0.02595 -0.00148 0.00693 -0.00109 AFIX 43 H4 2 0.210802 -0.299585 -0.223489 11.00000 -1.20000 AFIX 0 C5 1 0.343092 -0.322971 -0.115095 11.00000 0.03185 0.02416 = 0.03302 -0.00366 0.01183 0.00188 AFIX 43 H5 2 0.393260 -0.451835 -0.139484 11.00000 -1.20000 AFIX 0 C6 1 0.377311 -0.225597 -0.029375 11.00000 0.02411 0.02327 = 0.03212 -0.00091 0.00513 0.00219 AFIX 43 H6 2 0.451314 -0.287229 0.005020 11.00000 -1.20000 AFIX 0 C7 1 0.370551 -0.113363 0.165249 11.00000 0.02625 0.01960 = 0.02894 0.00010 0.00538 0.00006 C8 1 0.402285 0.025271 0.254177 11.00000 0.03675 0.02409 = 0.02826 0.00072 -0.00065 0.00173 AFIX 137 H8A 2 0.341464 -0.023809 0.291516 11.00000 -1.50000 H8B 2 0.403026 0.226590 0.246109 11.00000 -1.50000 H8C 2 0.483038 -0.036660 0.282833 11.00000 -1.50000 AFIX 0 C9 1 0.116288 0.267446 -0.005574 11.00000 0.02753 0.02280 = 0.03314 -0.00213 0.00566 0.00388 AFIX 137 H9A 2 0.040987 0.296076 -0.047663 11.00000 -1.50000 H9B 2 0.160029 0.443629 0.004849 11.00000 -1.50000 H9C 2 0.096244 0.197405 0.050600 11.00000 -1.50000 AFIX 0 N1 3 0.338291 0.057706 0.095402 11.00000 0.02730 0.01570 = 0.02614 -0.00191 0.00222 0.00066 O1 4 0.372541 -0.367504 0.158215 11.00000 0.05204 0.01703 = 0.03605 0.00109 0.00696 0.00099 H1N 2 0.339033 0.238761 0.105595 11.00000 0.03317 HKLF 4 Covalent radii and connectivity table for 2008lsh171 in P2(1)/n C 0.770 H 0.320 N 0.700 O 0.660 C1 - C6 C2 N1 C2 - C3 C1 C9 C3 - C4 C2 C4 - C5 C3 C5 - C4 C6 C6 - C5 C1 C7 - O1 N1 C8 C8 - C7 C9 - C2 N1 - C7 C1 O1 - C7 Operators for generating equivalent atoms: $1 x, y+1, z 11046 Reflections read, of which 802 rejected -14 =< h =< 13, -6 =< k =< 5, -18 =< l =< 19, Max. 2-theta = 54.98 0 Systematic absence violations 0 Inconsistent equivalents 1842 Unique reflections, of which 0 suppressed R(int) = 0.0426 R(sigma) = 0.0316 Friedel opposites merged Maximum memory for data reduction = 1310 / 18638 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 = 1614 / 137210 wR2 = 0.1322 before cycle 1 for 1842 data and 106 / 106 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 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.959; Restrained GooF = 0.958 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0661 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.56852 0.00523 0.000 OSF Mean shift/esd = 0.002 Maximum = -0.006 for U12 C1 Max. shift = 0.000 A for C1 Max. dU = 0.000 for H1N Least-squares cycle 2 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1322 before cycle 2 for 1842 data and 106 / 106 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 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.959; Restrained GooF = 0.958 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0661 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.56852 0.00523 -0.001 OSF Mean shift/esd = 0.001 Maximum = 0.002 for U12 C7 Max. shift = 0.000 A for H8C Max. dU = 0.000 for H1N Least-squares cycle 3 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1322 before cycle 3 for 1842 data and 106 / 106 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 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.959; Restrained GooF = 0.958 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0661 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.56851 0.00523 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H1N Max. dU = 0.000 for C9 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1322 before cycle 4 for 1842 data and 106 / 106 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 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.959; Restrained GooF = 0.958 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0661 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.56852 0.00523 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 5 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1322 before cycle 5 for 1842 data and 106 / 106 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 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.959; Restrained GooF = 0.958 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0661 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.56851 0.00523 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 6 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1322 before cycle 6 for 1842 data and 106 / 106 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 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.959; Restrained GooF = 0.958 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0661 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.56852 0.00523 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O1 Max. shift = 0.000 A for H8A Max. dU = 0.000 for H1N Least-squares cycle 7 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1322 before cycle 7 for 1842 data and 106 / 106 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 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.959; Restrained GooF = 0.958 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0661 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.56852 0.00523 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O1 Max. shift = 0.000 A for H8B Max. dU = 0.000 for H1N Least-squares cycle 8 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1322 before cycle 8 for 1842 data and 106 / 106 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 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.959; Restrained GooF = 0.958 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0661 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.56852 0.00523 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 9 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1322 before cycle 9 for 1842 data and 106 / 106 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 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.959; Restrained GooF = 0.958 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0661 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.56852 0.00523 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 10 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1322 before cycle 10 for 1842 data and 106 / 106 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 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.959; Restrained GooF = 0.958 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0661 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.56852 0.00523 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for C8 Least-squares cycle 11 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1322 before cycle 11 for 1842 data and 106 / 106 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 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.959; Restrained GooF = 0.958 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0661 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.56852 0.00523 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for C7 Least-squares cycle 12 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1322 before cycle 12 for 1842 data and 106 / 106 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 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.959; Restrained GooF = 0.958 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0661 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.56852 0.00523 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 13 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1322 before cycle 13 for 1842 data and 106 / 106 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 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.959; Restrained GooF = 0.958 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0661 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.56852 0.00523 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for C7 Least-squares cycle 14 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1322 before cycle 14 for 1842 data and 106 / 106 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 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.959; Restrained GooF = 0.958 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0661 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.56852 0.00523 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 15 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1322 before cycle 15 for 1842 data and 106 / 106 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 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.959; Restrained GooF = 0.958 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0661 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.56852 0.00523 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O1 Max. shift = 0.000 A for H9C Max. dU = 0.000 for C5 Least-squares cycle 16 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1322 before cycle 16 for 1842 data and 106 / 106 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 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.959; Restrained GooF = 0.958 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0661 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.56851 0.00523 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N 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 H3 0.0905 0.0243 -0.1647 43 0.950 0.000 C3 C4 C2 H4 0.2108 -0.2996 -0.2235 43 0.950 0.000 C4 C5 C3 H5 0.3933 -0.4518 -0.1395 43 0.950 0.000 C5 C4 C6 H6 0.4513 -0.2872 0.0050 43 0.950 0.000 C6 C5 C1 H8A 0.3415 -0.0238 0.2915 137 0.980 0.000 C8 C7 H8A H8B 0.4030 0.2266 0.2461 137 0.980 0.000 C8 C7 H8A H8C 0.4830 -0.0367 0.2828 137 0.980 0.000 C8 C7 H8A H9A 0.0410 0.2961 -0.0477 137 0.980 0.000 C9 C2 H9A H9B 0.1600 0.4436 0.0048 137 0.980 0.000 C9 C2 H9A H9C 0.0962 0.1974 0.0506 137 0.980 0.000 C9 C2 H9A 2008lsh171 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.30348 -0.03761 0.00648 1.00000 0.02463 0.01708 0.02500 -0.00033 0.00520 -0.00269 0.02210 0.00238 0.00012 0.00027 0.00009 0.00000 0.00066 0.00061 0.00066 0.00049 0.00050 0.00050 0.00031 C2 0.19552 0.06052 -0.04320 1.00000 0.02512 0.01667 0.02790 0.00141 0.00726 -0.00003 0.02290 0.00251 0.00012 0.00027 0.00009 0.00000 0.00066 0.00060 0.00068 0.00049 0.00051 0.00049 0.00031 C3 0.16340 -0.03993 -0.12945 1.00000 0.02882 0.02360 0.02638 0.00201 0.00294 0.00038 0.02642 0.00262 0.00013 0.00030 0.00009 0.00000 0.00070 0.00070 0.00070 0.00054 0.00053 0.00056 0.00032 H3 0.09050 0.02426 -0.16469 1.00000 0.03171 0.00000 0.00000 C4 0.23540 -0.23146 -0.16500 1.00000 0.03612 0.02416 0.02595 -0.00148 0.00693 -0.00109 0.02853 0.00270 0.00014 0.00030 0.00010 0.00000 0.00079 0.00070 0.00068 0.00054 0.00056 0.00059 0.00034 H4 0.21080 -0.29958 -0.22349 1.00000 0.03423 0.00000 0.00000 C5 0.34309 -0.32297 -0.11509 1.00000 0.03185 0.02416 0.03302 -0.00366 0.01183 0.00188 0.02895 0.00273 0.00013 0.00030 0.00010 0.00000 0.00073 0.00070 0.00075 0.00058 0.00057 0.00059 0.00034 H5 0.39326 -0.45184 -0.13948 1.00000 0.03474 0.00000 0.00000 C6 0.37731 -0.22560 -0.02937 1.00000 0.02411 0.02327 0.03212 -0.00091 0.00513 0.00219 0.02643 0.00264 0.00013 0.00029 0.00010 0.00000 0.00066 0.00068 0.00074 0.00055 0.00053 0.00054 0.00032 H6 0.45131 -0.28723 0.00502 1.00000 0.03172 0.00000 0.00000 C7 0.37055 -0.11336 0.16525 1.00000 0.02625 0.01960 0.02894 0.00010 0.00538 0.00006 0.02482 0.00254 0.00012 0.00028 0.00009 0.00000 0.00068 0.00065 0.00070 0.00052 0.00052 0.00053 0.00031 C8 0.40229 0.02527 0.25418 1.00000 0.03675 0.02409 0.02826 0.00072 -0.00065 0.00173 0.03034 0.00265 0.00014 0.00031 0.00009 0.00000 0.00079 0.00071 0.00073 0.00057 0.00057 0.00061 0.00035 H8A 0.34146 -0.02381 0.29152 1.00000 0.04551 0.00000 0.00000 H8B 0.40303 0.22659 0.24611 1.00000 0.04551 0.00000 0.00000 H8C 0.48304 -0.03666 0.28283 1.00000 0.04551 0.00000 0.00000 C9 0.11629 0.26745 -0.00557 1.00000 0.02753 0.02280 0.03314 -0.00213 0.00566 0.00388 0.02773 0.00267 0.00013 0.00030 0.00010 0.00000 0.00070 0.00070 0.00075 0.00055 0.00056 0.00055 0.00033 H9A 0.04099 0.29608 -0.04766 1.00000 0.04160 0.00000 0.00000 H9B 0.16003 0.44363 0.00485 1.00000 0.04160 0.00000 0.00000 H9C 0.09624 0.19740 0.05060 1.00000 0.04160 0.00000 0.00000 N1 0.33829 0.05771 0.09540 1.00000 0.02730 0.01570 0.02614 -0.00191 0.00222 0.00066 0.02327 0.00209 0.00011 0.00024 0.00008 0.00000 0.00060 0.00055 0.00060 0.00044 0.00044 0.00044 0.00029 O1 0.37254 -0.36750 0.15822 1.00000 0.05204 0.01703 0.03605 0.00109 0.00696 0.00099 0.03505 0.00204 0.00011 0.00021 0.00007 0.00000 0.00071 0.00052 0.00060 0.00042 0.00049 0.00047 0.00031 H1N 0.33903 0.23876 0.10559 1.00000 0.03317 0.02957 0.00162 0.00300 0.00117 0.00000 0.00455 Final Structure Factor Calculation for 2008lsh171 in P2(1)/n Total number of l.s. parameters = 106 Maximum vector length = 511 Memory required = 1508 / 22995 wR2 = 0.1322 before cycle 17 for 1842 data and 0 / 106 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 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.959; Restrained GooF = 0.958 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0661 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0475 for 1556 Fo > 4sig(Fo) and 0.0587 for all 1842 data wR2 = 0.1322, GooF = S = 0.959, Restrained GooF = 0.958 for all data Occupancy sum of asymmetric unit = 11.00 for non-hydrogen and 11.00 for hydrogen atoms Principal mean square atomic displacements U 0.0263 0.0238 0.0162 C1 0.0295 0.0227 0.0164 C2 0.0299 0.0269 0.0225 C3 0.0364 0.0259 0.0233 C4 0.0383 0.0285 0.0200 C5 0.0322 0.0259 0.0212 C6 0.0291 0.0257 0.0196 C7 0.0409 0.0267 0.0234 C8 0.0336 0.0297 0.0199 C9 0.0295 0.0250 0.0153 N1 0.0522 0.0360 0.0170 O1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.013 0.025 0.039 0.052 0.069 0.090 0.118 0.160 0.233 1.000 Number in group 185. 184. 204. 167. 188. 181. 181. 186. 181. 185. GooF 1.050 1.053 1.067 1.016 0.997 0.983 0.920 0.864 0.800 0.776 K 2.329 1.060 0.976 0.961 0.966 0.978 0.988 1.009 1.014 1.019 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.14 1.31 1.62 inf Number in group 186. 183. 188. 183. 181. 185. 183. 188. 182. 183. GooF 1.090 1.090 1.028 0.928 0.843 0.952 0.809 0.799 0.939 1.050 K 1.044 1.062 1.030 1.012 1.025 1.009 1.029 1.015 1.026 1.002 R1 0.131 0.142 0.106 0.079 0.062 0.055 0.042 0.035 0.040 0.033 Recommended weighting scheme: WGHT 0.0367 0.5182 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) -1 1 2 2.24 9.75 4.04 0.049 3.92 2 2 16 1.17 7.41 3.65 0.043 0.85 -7 3 8 0.17 4.82 3.42 0.034 1.02 -7 5 8 13.06 25.48 3.32 0.079 0.78 0 3 3 27.67 16.74 3.26 0.064 1.53 3 0 9 3.90 0.58 3.24 0.012 1.44 6 0 2 179.91 139.32 3.16 0.185 1.71 3 3 11 -0.23 3.78 3.09 0.031 0.97 -9 3 10 12.99 23.39 3.06 0.076 0.87 0 5 11 10.08 1.48 3.05 0.019 0.79 8 2 13 9.76 3.60 3.03 0.030 0.78 -7 5 7 7.40 15.83 2.98 0.062 0.79 8 0 12 28.84 49.89 2.96 0.111 0.86 -4 4 14 4.61 0.02 2.95 0.002 0.80 12 0 4 20.72 33.43 2.90 0.091 0.86 -9 4 8 29.06 43.77 2.87 0.104 0.82 -12 2 5 5.38 1.21 2.85 0.017 0.86 13 1 1 13.13 4.51 2.84 0.033 0.82 5 0 5 290.51 236.17 2.79 0.241 1.65 -6 3 13 3.63 0.76 2.79 0.014 0.88 -6 3 7 13.57 22.64 2.76 0.075 1.10 -1 0 9 97.25 75.06 2.74 0.136 1.70 8 2 5 126.98 99.06 2.72 0.156 1.06 5 1 0 36.38 25.75 2.61 0.080 2.00 -7 4 9 -0.57 2.07 2.60 0.023 0.87 -10 4 3 36.00 23.78 2.58 0.077 0.82 9 1 6 12.20 20.07 2.56 0.070 1.01 -8 2 11 2.28 0.13 2.55 0.006 0.97 -2 4 3 26.84 38.37 2.55 0.097 1.16 -8 5 3 16.03 8.87 2.54 0.047 0.79 1 1 14 14.77 23.25 2.52 0.076 1.03 -14 1 6 33.27 52.44 2.50 0.114 0.77 10 4 1 6.80 2.28 2.48 0.024 0.81 -1 3 16 0.96 6.04 2.45 0.039 0.82 -11 2 12 -0.32 5.89 2.44 0.038 0.80 10 3 4 405.53 331.76 2.41 0.286 0.86 -1 4 15 28.48 19.13 2.39 0.069 0.78 11 0 3 3.95 0.85 2.38 0.014 0.95 6 5 2 6.22 2.31 2.37 0.024 0.84 -6 2 3 2.21 5.74 2.36 0.038 1.45 -8 3 7 4.13 9.61 2.36 0.049 0.99 2 1 1 103.61 128.32 2.36 0.178 3.44 5 1 4 106.41 131.45 2.35 0.180 1.67 -4 2 12 4.05 8.51 2.35 0.046 1.09 -9 3 5 6.10 11.65 2.34 0.054 0.96 -8 1 2 24.45 34.31 2.34 0.092 1.33 3 1 0 1.79 4.95 2.32 0.035 2.91 -7 0 7 95.50 75.79 2.32 0.137 1.38 1 4 14 46.03 33.18 2.32 0.090 0.79 4 3 11 14.11 22.23 2.31 0.074 0.94 Bond lengths and angles C1 - Distance Angles C6 1.3925 (0.0019) C2 1.3958 (0.0019) 121.10 (0.13) N1 1.4274 (0.0017) 119.79 (0.12) 119.11 (0.12) C1 - C6 C2 C2 - Distance Angles C3 1.3952 (0.0019) C1 1.3958 (0.0019) 117.60 (0.12) C9 1.5047 (0.0019) 120.93 (0.12) 121.47 (0.12) C2 - C3 C1 C3 - Distance Angles C4 1.3886 (0.0021) C2 1.3952 (0.0019) 121.59 (0.13) H3 0.9500 119.20 119.20 C3 - C4 C2 C4 - Distance Angles C5 1.3843 (0.0021) C3 1.3886 (0.0021) 119.90 (0.13) H4 0.9500 120.05 120.05 C4 - C5 C3 C5 - Distance Angles C4 1.3843 (0.0021) C6 1.3856 (0.0020) 119.64 (0.13) H5 0.9500 120.18 120.18 C5 - C4 C6 C6 - Distance Angles C5 1.3856 (0.0020) C1 1.3925 (0.0019) 120.16 (0.13) H6 0.9500 119.92 119.92 C6 - C5 C1 C7 - Distance Angles O1 1.2323 (0.0017) N1 1.3513 (0.0018) 123.10 (0.13) C8 1.5044 (0.0019) 121.12 (0.13) 115.77 (0.12) C7 - O1 N1 C8 - Distance Angles C7 1.5044 (0.0019) 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 C2 1.5047 (0.0019) H9A 0.9800 109.47 H9B 0.9800 109.47 109.47 H9C 0.9800 109.47 109.47 109.47 C9 - C2 H9A H9B N1 - Distance Angles C7 1.3513 (0.0018) C1 1.4274 (0.0017) 123.45 (0.12) H1N 0.8877 (0.0141) 118.01 (1.16) 118.54 (1.16) N1 - C7 C1 O1 - Distance Angles C7 1.2323 (0.0017) O1 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.888(14) 2.074(15) 2.9411(15) 165.1(16) 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)