+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 15:58:06 on 22-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh071 in C2/c CELL 0.71073 17.5403 13.7630 7.7717 90.000 101.876 90.000 ZERR 8.00 0.0005 0.0003 0.0002 0.000 0.001 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N O UNIT 80 88 8 24 V = 1835.99 F(000) = 816.0 Mu = 0.10 mm-1 Cell Wt = 1545.58 Rho = 1.398 MERG 2 OMIT -3.00 55.00 OMIT 4 0 0 OMIT 0 4 0 OMIT -1 1 1 OMIT 0 2 0 DFIX 0.88 0.02 N1 H1N EQIV $1 -x+3/2, y+1/2, -z+1/2 HTAB N1 O2_$1 FMAP 2 PLAN 5 SIZE 0.30 0.44 0.54 ACTA HTAB 2.00000 BOND $H WGHT 0.05600 0.83660 L.S. 16 TEMP -153.00 FVAR 0.56467 C1 1 0.858322 0.223703 0.145522 11.00000 0.01854 0.01755 = 0.01586 0.00101 0.00281 -0.00068 C2 1 0.916011 0.165817 0.098125 11.00000 0.01871 0.02171 = 0.02576 0.00218 0.00912 -0.00134 AFIX 43 H2 2 0.960377 0.194885 0.066860 11.00000 -1.20000 AFIX 0 C3 1 0.908065 0.065204 0.097001 11.00000 0.02050 0.02099 = 0.02506 0.00047 0.00922 0.00194 AFIX 43 H3 2 0.947561 0.025797 0.065720 11.00000 -1.20000 AFIX 0 C4 1 0.843167 0.021440 0.140987 11.00000 0.01874 0.01844 = 0.01600 0.00001 0.00298 -0.00054 C5 1 0.785604 0.079954 0.186537 11.00000 0.01622 0.02033 = 0.02312 -0.00038 0.00629 -0.00296 AFIX 43 H5 2 0.740942 0.050831 0.216308 11.00000 -1.20000 AFIX 0 C6 1 0.792831 0.179903 0.188839 11.00000 0.01766 0.01930 = 0.02354 -0.00175 0.00611 0.00010 AFIX 43 H6 2 0.753153 0.219048 0.219974 11.00000 -1.20000 AFIX 0 C7 1 0.913008 0.387733 0.101657 11.00000 0.01997 0.02033 = 0.01631 0.00006 0.00372 -0.00186 C8 1 0.899207 0.493809 0.134137 11.00000 0.02373 0.01885 = 0.02363 -0.00158 0.00862 -0.00260 AFIX 137 H8A 2 0.935398 0.533565 0.083459 11.00000 -1.50000 H8B 2 0.907750 0.505715 0.260988 11.00000 -1.50000 H8C 2 0.845512 0.511009 0.079048 11.00000 -1.50000 AFIX 0 C9 1 0.832668 -0.085554 0.143769 11.00000 0.01905 0.01954 = 0.01760 0.00060 0.00480 0.00078 C10 1 0.889157 -0.239988 0.120329 11.00000 0.02848 0.01623 = 0.03114 0.00123 0.01119 0.00237 AFIX 137 H10A 2 0.891136 -0.261390 0.241436 11.00000 -1.50000 H10B 2 0.932751 -0.268680 0.076950 11.00000 -1.50000 H10C 2 0.839881 -0.260897 0.045623 11.00000 -1.50000 AFIX 0 N1 3 0.861868 0.325927 0.156747 11.00000 0.01756 0.01669 = 0.02497 -0.00072 0.00833 -0.00056 O1 4 0.965300 0.360311 0.031236 11.00000 0.03109 0.02192 = 0.03422 -0.00109 0.02010 -0.00296 O2 4 0.773608 -0.124636 0.168827 11.00000 0.02274 0.01901 = 0.03575 0.00026 0.01164 -0.00215 O3 4 0.894656 -0.134518 0.115838 11.00000 0.02191 0.01600 = 0.03067 0.00065 0.01003 0.00216 H1N 2 0.823668 0.352131 0.195936 11.00000 0.02438 HKLF 4 Covalent radii and connectivity table for 2008lsh071 in C2/c C 0.770 H 0.320 N 0.700 O 0.660 C1 - C2 C6 N1 C2 - C3 C1 C3 - C4 C2 C4 - C3 C5 C9 C5 - C6 C4 C6 - C5 C1 C7 - O1 N1 C8 C8 - C7 C9 - O2 O3 C4 C10 - O3 N1 - C7 C1 O1 - C7 O2 - C9 O3 - C9 C10 Operators for generating equivalent atoms: $1 -x+3/2, y+1/2, -z+1/2 14404 Reflections read, of which 351 rejected -22 =< h =< 22, -17 =< k =< 16, -10 =< l =< 10, Max. 2-theta = 55.00 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 1 13 1 0.01 0.19 5 1.10 1 Inconsistent equivalents 2098 Unique reflections, of which 0 suppressed R(int) = 0.0402 R(sigma) = 0.0282 Friedel opposites merged Maximum memory for data reduction = 1467 / 24993 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 = 1822 / 168098 wR2 = 0.1063 before cycle 1 for 2098 data and 133 / 133 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 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.056; Restrained GooF = 1.056 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0560 * P )^2 + 0.84 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.56466 0.00149 -0.004 OSF Mean shift/esd = 0.007 Maximum = -0.021 for U22 O1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 2 Maximum vector length = 511 Memory required = 1822 / 168098 wR2 = 0.1063 before cycle 2 for 2098 data and 133 / 133 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 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.056; Restrained GooF = 1.056 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0560 * P )^2 + 0.84 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.56465 0.00149 -0.010 OSF Mean shift/esd = 0.003 Maximum = -0.010 for OSF Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 3 Maximum vector length = 511 Memory required = 1822 / 168098 wR2 = 0.1063 before cycle 3 for 2098 data and 133 / 133 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 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.056; Restrained GooF = 1.056 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0560 * P )^2 + 0.84 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.56465 0.00149 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x N1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 4 Maximum vector length = 511 Memory required = 1822 / 168098 wR2 = 0.1063 before cycle 4 for 2098 data and 133 / 133 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 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.056; Restrained GooF = 1.056 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0560 * P )^2 + 0.84 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.56465 0.00149 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x N1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 5 Maximum vector length = 511 Memory required = 1822 / 168098 wR2 = 0.1063 before cycle 5 for 2098 data and 133 / 133 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 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.056; Restrained GooF = 1.056 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0560 * P )^2 + 0.84 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.56465 0.00149 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x N1 Max. shift = 0.000 A for H8B Max. dU = 0.000 for H1N Least-squares cycle 6 Maximum vector length = 511 Memory required = 1822 / 168098 wR2 = 0.1063 before cycle 6 for 2098 data and 133 / 133 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 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.056; Restrained GooF = 1.056 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0560 * P )^2 + 0.84 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.56465 0.00149 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x N1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for C6 Least-squares cycle 7 Maximum vector length = 511 Memory required = 1822 / 168098 wR2 = 0.1063 before cycle 7 for 2098 data and 133 / 133 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 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.056; Restrained GooF = 1.056 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0560 * P )^2 + 0.84 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.56465 0.00149 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x N1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 8 Maximum vector length = 511 Memory required = 1822 / 168098 wR2 = 0.1063 before cycle 8 for 2098 data and 133 / 133 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 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.056; Restrained GooF = 1.056 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0560 * P )^2 + 0.84 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.56465 0.00149 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x N1 Max. shift = 0.000 A for H8A Max. dU = 0.000 for O1 Least-squares cycle 9 Maximum vector length = 511 Memory required = 1822 / 168098 wR2 = 0.1063 before cycle 9 for 2098 data and 133 / 133 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 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.056; Restrained GooF = 1.056 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0560 * P )^2 + 0.84 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.56465 0.00149 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x N1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for O2 Least-squares cycle 10 Maximum vector length = 511 Memory required = 1822 / 168098 wR2 = 0.1063 before cycle 10 for 2098 data and 133 / 133 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 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.056; Restrained GooF = 1.056 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0560 * P )^2 + 0.84 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.56465 0.00149 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x N1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 11 Maximum vector length = 511 Memory required = 1822 / 168098 wR2 = 0.1063 before cycle 11 for 2098 data and 133 / 133 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 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.056; Restrained GooF = 1.056 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0560 * P )^2 + 0.84 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.56465 0.00149 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x N1 Max. shift = 0.000 A for C8 Max. dU = 0.000 for H1N Least-squares cycle 12 Maximum vector length = 511 Memory required = 1822 / 168098 wR2 = 0.1063 before cycle 12 for 2098 data and 133 / 133 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 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.056; Restrained GooF = 1.056 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0560 * P )^2 + 0.84 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.56465 0.00149 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x N1 Max. shift = 0.000 A for H10B Max. dU = 0.000 for H1N Least-squares cycle 13 Maximum vector length = 511 Memory required = 1822 / 168098 wR2 = 0.1063 before cycle 13 for 2098 data and 133 / 133 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 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.056; Restrained GooF = 1.056 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0560 * P )^2 + 0.84 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.56465 0.00149 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x N1 Max. shift = 0.000 A for H8A Max. dU = 0.000 for H1N Least-squares cycle 14 Maximum vector length = 511 Memory required = 1822 / 168098 wR2 = 0.1063 before cycle 14 for 2098 data and 133 / 133 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 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.056; Restrained GooF = 1.056 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0560 * P )^2 + 0.84 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.56465 0.00149 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x N1 Max. shift = 0.000 A for H10B Max. dU = 0.000 for H1N Least-squares cycle 15 Maximum vector length = 511 Memory required = 1822 / 168098 wR2 = 0.1063 before cycle 15 for 2098 data and 133 / 133 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 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.056; Restrained GooF = 1.056 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0560 * P )^2 + 0.84 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.56465 0.00149 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x N1 Max. shift = 0.000 A for H8A Max. dU = 0.000 for H1N Least-squares cycle 16 Maximum vector length = 511 Memory required = 1822 / 168098 wR2 = 0.1063 before cycle 16 for 2098 data and 133 / 133 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 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.056; Restrained GooF = 1.056 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0560 * P )^2 + 0.84 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.56465 0.00149 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x N1 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 H2 0.9604 0.1949 0.0669 43 0.950 0.000 C2 C3 C1 H3 0.9476 0.0258 0.0657 43 0.950 0.000 C3 C4 C2 H5 0.7409 0.0508 0.2163 43 0.950 0.000 C5 C6 C4 H6 0.7532 0.2190 0.2200 43 0.950 0.000 C6 C5 C1 H8A 0.9354 0.5336 0.0835 137 0.980 0.000 C8 C7 H8A H8B 0.9077 0.5057 0.2610 137 0.980 0.000 C8 C7 H8A H8C 0.8455 0.5110 0.0790 137 0.980 0.000 C8 C7 H8A H10A 0.8911 -0.2614 0.2414 137 0.980 0.000 C10 O3 H10A H10B 0.9328 -0.2687 0.0770 137 0.980 0.000 C10 O3 H10A H10C 0.8399 -0.2609 0.0456 137 0.980 0.000 C10 O3 H10A 2008lsh071 in C2/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.85832 0.22370 0.14552 1.00000 0.01853 0.01755 0.01585 0.00101 0.00280 -0.00069 0.01741 0.00199 0.00006 0.00008 0.00014 0.00000 0.00054 0.00055 0.00053 0.00039 0.00041 0.00040 0.00025 C2 0.91601 0.16582 0.09813 1.00000 0.01870 0.02171 0.02575 0.00218 0.00912 -0.00134 0.02140 0.00221 0.00007 0.00009 0.00016 0.00000 0.00057 0.00059 0.00061 0.00045 0.00047 0.00043 0.00026 H2 0.96038 0.19488 0.06686 1.00000 0.02569 0.00000 0.00000 C3 0.90806 0.06520 0.09700 1.00000 0.02049 0.02099 0.02505 0.00047 0.00922 0.00194 0.02153 0.00222 0.00007 0.00008 0.00015 0.00000 0.00056 0.00059 0.00061 0.00044 0.00046 0.00043 0.00026 H3 0.94756 0.02580 0.06572 1.00000 0.02583 0.00000 0.00000 C4 0.84317 0.02144 0.14099 1.00000 0.01873 0.01844 0.01600 0.00001 0.00298 -0.00054 0.01781 0.00200 0.00006 0.00008 0.00014 0.00000 0.00055 0.00057 0.00055 0.00040 0.00043 0.00041 0.00025 C5 0.78561 0.07996 0.18654 1.00000 0.01621 0.02033 0.02311 -0.00038 0.00629 -0.00295 0.01956 0.00211 0.00006 0.00009 0.00015 0.00000 0.00053 0.00057 0.00058 0.00043 0.00044 0.00040 0.00026 H5 0.74094 0.05083 0.21631 1.00000 0.02347 0.00000 0.00000 C6 0.79283 0.17990 0.18884 1.00000 0.01766 0.01929 0.02352 -0.00175 0.00611 0.00011 0.01989 0.00210 0.00007 0.00008 0.00015 0.00000 0.00054 0.00059 0.00059 0.00042 0.00045 0.00041 0.00026 H6 0.75315 0.21905 0.21997 1.00000 0.02387 0.00000 0.00000 C7 0.91301 0.38773 0.10166 1.00000 0.01997 0.02032 0.01630 0.00006 0.00372 -0.00186 0.01887 0.00203 0.00006 0.00008 0.00014 0.00000 0.00055 0.00057 0.00054 0.00041 0.00044 0.00042 0.00025 C8 0.89921 0.49381 0.13413 1.00000 0.02372 0.01884 0.02363 -0.00158 0.00862 -0.00260 0.02153 0.00217 0.00007 0.00008 0.00015 0.00000 0.00058 0.00057 0.00059 0.00044 0.00046 0.00044 0.00026 H8A 0.93540 0.53356 0.08346 1.00000 0.03229 0.00000 0.00000 H8B 0.90775 0.50572 0.26098 1.00000 0.03229 0.00000 0.00000 H8C 0.84551 0.51101 0.07904 1.00000 0.03229 0.00000 0.00000 C9 0.83267 -0.08555 0.14377 1.00000 0.01904 0.01953 0.01759 0.00060 0.00480 0.00078 0.01857 0.00210 0.00006 0.00008 0.00014 0.00000 0.00053 0.00057 0.00055 0.00041 0.00042 0.00042 0.00025 C10 0.88916 -0.23999 0.12033 1.00000 0.02847 0.01623 0.03114 0.00123 0.01118 0.00237 0.02455 0.00231 0.00007 0.00008 0.00016 0.00000 0.00064 0.00057 0.00066 0.00046 0.00052 0.00046 0.00028 H10A 0.89113 -0.26139 0.24143 1.00000 0.03683 0.00000 0.00000 H10B 0.93275 -0.26868 0.07696 1.00000 0.03683 0.00000 0.00000 H10C 0.83988 -0.26090 0.04561 1.00000 0.03683 0.00000 0.00000 N1 0.86187 0.32593 0.15675 1.00000 0.01755 0.01669 0.02496 -0.00072 0.00833 -0.00056 0.01917 0.00177 0.00006 0.00007 0.00013 0.00000 0.00049 0.00050 0.00053 0.00036 0.00039 0.00036 0.00024 O1 0.96530 0.36031 0.03123 1.00000 0.03108 0.02191 0.03421 -0.00109 0.02009 -0.00296 0.02715 0.00171 0.00005 0.00006 0.00012 0.00000 0.00048 0.00044 0.00052 0.00034 0.00039 0.00034 0.00023 O2 0.77361 -0.12464 0.16883 1.00000 0.02274 0.01900 0.03575 0.00026 0.01164 -0.00214 0.02502 0.00161 0.00005 0.00006 0.00012 0.00000 0.00045 0.00044 0.00053 0.00033 0.00037 0.00031 0.00023 O3 0.89466 -0.13452 0.11584 1.00000 0.02190 0.01600 0.03066 0.00065 0.01002 0.00216 0.02219 0.00155 0.00005 0.00005 0.00011 0.00000 0.00044 0.00042 0.00048 0.00031 0.00035 0.00030 0.00022 H1N 0.82366 0.35214 0.19594 1.00000 0.02440 0.02732 0.00080 0.00102 0.00190 0.00000 0.00347 Final Structure Factor Calculation for 2008lsh071 in C2/c Total number of l.s. parameters = 133 Maximum vector length = 511 Memory required = 1689 / 22995 wR2 = 0.1063 before cycle 17 for 2098 data and 0 / 133 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 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.056; Restrained GooF = 1.056 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0560 * P )^2 + 0.84 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0380 for 1738 Fo > 4sig(Fo) and 0.0484 for all 2098 data wR2 = 0.1063, GooF = S = 1.056, Restrained GooF = 1.056 for all data Occupancy sum of asymmetric unit = 14.00 for non-hydrogen and 11.00 for hydrogen atoms Principal mean square atomic displacements U 0.0195 0.0173 0.0154 C1 0.0276 0.0222 0.0144 C2 0.0273 0.0212 0.0161 C3 0.0194 0.0181 0.0160 C4 0.0238 0.0212 0.0137 C5 0.0243 0.0190 0.0164 C6 0.0221 0.0183 0.0162 C7 0.0276 0.0194 0.0176 C8 0.0204 0.0186 0.0168 C9 0.0344 0.0235 0.0158 C10 0.0261 0.0166 0.0148 N1 0.0441 0.0220 0.0153 O1 0.0369 0.0213 0.0168 O2 0.0320 0.0196 0.0150 O3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.012 0.022 0.034 0.048 0.063 0.082 0.107 0.140 0.203 1.000 Number in group 219. 207. 220. 204. 203. 217. 200. 214. 203. 211. GooF 0.879 0.972 1.146 1.064 1.121 1.049 1.143 1.186 0.976 0.990 K 1.226 0.999 0.889 0.954 0.968 1.004 0.999 1.012 1.016 1.010 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.04 1.15 1.31 1.66 inf Number in group 218. 205. 209. 215. 202. 213. 206. 209. 210. 211. GooF 1.011 1.069 0.979 1.025 0.974 1.081 0.975 0.932 1.176 1.286 K 1.047 1.029 1.020 1.012 1.002 1.018 1.032 1.024 1.036 0.982 R1 0.103 0.092 0.084 0.061 0.052 0.042 0.035 0.030 0.036 0.030 Recommended weighting scheme: WGHT 0.0560 0.8378 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) -4 2 1 304.99 460.64 5.12 0.123 3.53 10 4 0 764.94 546.29 4.99 0.134 1.54 -1 13 2 145.58 209.49 3.55 0.083 1.02 5 5 0 51.86 29.38 3.54 0.031 2.15 5 13 3 31.28 62.80 3.53 0.045 0.92 6 6 0 18.09 6.48 3.32 0.015 1.79 -13 7 4 386.74 500.70 3.28 0.128 1.03 1 13 0 194.13 271.96 3.23 0.095 1.06 4 12 1 61.37 95.56 3.20 0.056 1.09 -4 8 1 14.76 34.58 3.19 0.034 1.59 -4 16 2 555.72 407.74 3.14 0.116 0.83 6 16 0 1197.55 928.62 3.05 0.175 0.82 -2 4 4 13.08 28.65 3.03 0.031 1.69 -13 5 4 226.79 296.26 3.03 0.099 1.11 -8 4 2 4120.30 3453.45 3.00 0.337 1.77 -7 15 3 598.92 469.23 2.96 0.124 0.83 3 13 0 236.37 309.93 2.93 0.101 1.04 -19 5 5 275.10 202.29 2.90 0.082 0.82 -1 5 4 187.54 142.29 2.87 0.068 1.58 6 2 1 22.65 10.90 2.85 0.019 2.36 -11 7 5 53.35 86.12 2.83 0.053 1.04 0 14 0 89.49 150.05 2.78 0.070 0.98 9 3 1 1475.46 1239.89 2.77 0.202 1.65 3 13 1 308.39 388.83 2.76 0.113 1.03 -2 2 1 4424.20 5243.32 2.73 0.416 4.68 -14 8 3 57.64 85.11 2.72 0.053 0.99 -19 5 1 186.91 251.95 2.69 0.091 0.87 1 3 0 188.87 247.34 2.64 0.090 4.43 13 3 0 6.65 0.31 2.61 0.003 1.27 -5 17 2 547.98 419.87 2.60 0.118 0.78 -1 13 1 717.71 900.76 2.60 0.172 1.05 -4 6 2 120.52 90.93 2.59 0.055 1.86 -10 0 4 29.72 48.33 2.57 0.040 1.43 -12 8 5 78.73 110.84 2.56 0.060 0.97 0 16 0 604.20 471.95 2.55 0.125 0.86 2 14 2 74.48 106.43 2.55 0.059 0.94 -19 5 2 117.99 160.90 2.54 0.073 0.87 -14 4 3 30.29 52.26 2.52 0.041 1.14 -10 4 3 112.07 83.92 2.52 0.053 1.44 -13 5 2 182.17 230.08 2.52 0.087 1.20 3 1 0 15256.89 18088.13 2.51 0.772 5.28 -17 7 4 32.32 54.88 2.50 0.043 0.88 -15 7 3 373.95 456.47 2.46 0.123 0.98 -16 8 1 29.30 48.82 2.43 0.040 0.92 4 6 0 205.01 164.87 2.40 0.074 2.02 15 3 1 58.43 38.53 2.39 0.036 1.07 -5 5 2 4.26 0.03 2.39 0.001 1.98 -9 15 3 26.89 9.34 2.39 0.018 0.81 7 5 0 188.34 151.36 2.36 0.071 1.83 -12 4 1 119.43 89.01 2.36 0.054 1.35 Bond lengths and angles C1 - Distance Angles C2 1.3956 (0.0016) C6 1.3984 (0.0015) 119.58 (0.10) N1 1.4102 (0.0014) 124.11 (0.10) 116.31 (0.10) C1 - C2 C6 C2 - Distance Angles C3 1.3916 (0.0017) C1 1.3956 (0.0016) 119.51 (0.10) H2 0.9500 120.24 120.24 C2 - C3 C1 C3 - Distance Angles C4 1.3912 (0.0015) C2 1.3916 (0.0017) 121.01 (0.10) H3 0.9500 119.49 119.49 C3 - C4 C2 C4 - Distance Angles C3 1.3912 (0.0015) C5 1.3930 (0.0015) 118.99 (0.11) C9 1.4847 (0.0016) 122.90 (0.10) 118.11 (0.10) C4 - C3 C5 C5 - Distance Angles C6 1.3812 (0.0016) C4 1.3930 (0.0015) 120.64 (0.10) H5 0.9500 119.68 119.68 C5 - C6 C4 C6 - Distance Angles C5 1.3812 (0.0016) C1 1.3984 (0.0015) 120.26 (0.10) H6 0.9500 119.87 119.87 C6 - C5 C1 C7 - Distance Angles O1 1.2206 (0.0014) N1 1.3673 (0.0014) 123.36 (0.11) C8 1.5096 (0.0016) 122.35 (0.10) 114.28 (0.09) C7 - O1 N1 C8 - Distance Angles C7 1.5096 (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 1.2180 (0.0014) O3 1.3344 (0.0014) 123.46 (0.11) C4 1.4847 (0.0016) 123.54 (0.10) 113.01 (0.09) C9 - O2 O3 C10 - Distance Angles O3 1.4557 (0.0013) H10A 0.9800 109.47 H10B 0.9800 109.47 109.47 H10C 0.9800 109.47 109.47 109.47 C10 - O3 H10A H10B N1 - Distance Angles C7 1.3673 (0.0014) C1 1.4102 (0.0014) 128.66 (0.10) H1N 0.8695 (0.0129) 117.01 (0.97) 114.10 (0.97) N1 - C7 C1 O1 - Distance Angles C7 1.2206 (0.0014) O1 - O2 - Distance Angles C9 1.2180 (0.0014) O2 - O3 - Distance Angles C9 1.3344 (0.0014) C10 1.4557 (0.0013) 116.07 (0.09) O3 - C9 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.869(13) 2.204(13) 3.0452(13) 162.8(13) N1-H1N...O2_$1 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)