+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 16:58:02 on 22-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh080 in Cc CELL 0.71073 8.4447 19.2810 7.3108 90.000 117.051 90.000 ZERR 4.00 0.0003 0.0012 0.0005 0.000 0.004 0.000 LATT -7 SYMM X, - Y, 1/2 + Z SFAC C H N O UNIT 44 52 4 12 V = 1060.14 F(000) = 440.0 Mu = 0.09 mm-1 Cell Wt = 828.90 Rho = 1.298 MERG 2 OMIT -3.00 55.00 OMIT -1 1 0 OMIT 1 1 0 TWIN FMAP 2 DFIX 0.88 0.02 N1 H1N EQIV $1 x+1, -y+1, z+1/2 HTAB N1 O3_$1 HTAB PLAN 5 SIZE 0.06 0.26 0.70 ACTA BOND $H L.S. 16 TEMP -153.00 WGHT 0.038200 0.403400 EXTI 0.015202 BASF 1.76592 FVAR 0.68493 C1 1 0.871299 0.598633 1.042787 11.00000 0.01996 0.02090 = 0.02058 -0.00312 0.00956 -0.00058 C2 1 0.758435 0.648504 0.907441 11.00000 0.02397 0.01980 = 0.02537 0.00117 0.01230 -0.00105 AFIX 43 H2 2 0.806514 0.687693 0.871404 11.00000 -1.20000 AFIX 0 C3 1 0.575220 0.640334 0.825911 11.00000 0.02188 0.02089 = 0.02364 -0.00013 0.00981 0.00090 AFIX 43 H3 2 0.498688 0.674394 0.734543 11.00000 -1.20000 AFIX 0 C4 1 0.501938 0.582980 0.876016 11.00000 0.02244 0.02108 = 0.02132 -0.00644 0.01094 -0.00223 C5 1 0.615410 0.533092 1.009917 11.00000 0.02657 0.02238 = 0.02394 -0.00214 0.01312 -0.00345 AFIX 43 H5 2 0.567054 0.493719 1.044750 11.00000 -1.20000 AFIX 0 C6 1 0.797580 0.540628 1.092079 11.00000 0.02606 0.01969 = 0.02249 -0.00014 0.01098 0.00043 AFIX 43 H6 2 0.873624 0.506290 1.182673 11.00000 -1.20000 AFIX 0 C7 1 1.161089 0.658881 1.146656 11.00000 0.02373 0.02468 = 0.02194 -0.00165 0.01029 -0.00082 C8 1 1.358083 0.645820 1.261144 11.00000 0.02360 0.02934 = 0.02983 -0.00147 0.01064 -0.00190 AFIX 137 H8A 2 1.415542 0.684271 1.356068 11.00000 -1.50000 H8B 2 1.407175 0.642233 1.163123 11.00000 -1.50000 H8C 2 1.379810 0.602451 1.338792 11.00000 -1.50000 AFIX 0 C9 1 0.307451 0.574395 0.794592 11.00000 0.02325 0.02394 = 0.02166 -0.00666 0.01056 -0.00192 C10 1 0.024000 0.626121 0.601544 11.00000 0.01769 0.03603 = 0.02558 -0.00250 0.00855 -0.00082 AFIX 23 H10A 2 -0.005694 0.617808 0.716037 11.00000 -1.20000 H10B 2 -0.029406 0.588633 0.499029 11.00000 -1.20000 AFIX 0 C11 1 -0.045622 0.695599 0.504583 11.00000 0.02782 0.03794 = 0.03979 -0.00104 0.01610 0.00654 AFIX 137 H11A 2 -0.023883 0.701543 0.384767 11.00000 -1.50000 H11B 2 0.015330 0.732408 0.604524 11.00000 -1.50000 H11C 2 -0.173664 0.698102 0.461303 11.00000 -1.50000 AFIX 0 N1 3 1.057534 0.602694 1.134011 11.00000 0.02080 0.01906 = 0.02582 0.00272 0.00927 0.00240 O1 4 1.100355 0.715463 1.072010 11.00000 0.02604 0.02383 = 0.04043 0.00357 0.01075 -0.00017 O2 4 0.216104 0.627585 0.677440 11.00000 0.01841 0.02868 = 0.03073 0.00018 0.00921 -0.00060 O3 4 0.237256 0.525058 0.833579 11.00000 0.02693 0.02629 = 0.03341 -0.00294 0.01294 -0.00634 H1N 2 1.110902 0.564409 1.194941 11.00000 0.03095 HKLF 4 Covalent radii and connectivity table for 2008lsh080 in Cc C 0.770 H 0.320 N 0.700 O 0.660 C1 - C2 N1 C6 C2 - C3 C1 C3 - C2 C4 C4 - C3 C5 C9 C5 - C6 C4 C6 - C5 C1 C7 - O1 N1 C8 C8 - C7 C9 - O3 O2 C4 C10 - O2 C11 C11 - C10 N1 - C7 C1 O1 - C7 O2 - C9 C10 O3 - C9 Operators for generating equivalent atoms: $1 x+1, -y+1, z+1/2 Floating origin restraints generated 6080 Reflections read, of which 84 rejected -10 =< h =< 10, -24 =< k =< 24, -9 =< l =< 9, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 2256 Unique reflections, of which 0 suppressed R(int) = 0.0318 R(sigma) = 0.0415 Friedel opposites not merged Maximum memory for data reduction = 1581 / 27651 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 = 1977 / 180891 wR2 = 0.0850 before cycle 1 for 2256 data and 144 / 144 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 0.006 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.022; Restrained GooF = 1.021 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0382 * P )^2 + 0.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.68493 0.00155 -0.002 OSF 2 1.76596 0.97658 0.000 BASF 1 3 0.01520 0.00230 0.000 EXTI Mean shift/esd = 0.002 Maximum = -0.008 for U12 O2 Max. shift = 0.000 A for C6 Max. dU = 0.000 for C6 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1977 / 180891 wR2 = 0.0849 before cycle 2 for 2256 data and 144 / 144 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 0.006 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.022; Restrained GooF = 1.021 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0382 * P )^2 + 0.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.68493 0.00155 0.000 OSF 2 1.76582 0.97609 0.000 BASF 1 3 0.01520 0.00230 0.000 EXTI Mean shift/esd = 0.001 Maximum = -0.002 for U12 O2 Max. shift = 0.000 A for H8C Max. dU = 0.000 for H1N Least-squares cycle 3 Maximum vector length = 511 Memory required = 1977 / 180891 wR2 = 0.0850 before cycle 3 for 2256 data and 144 / 144 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 0.006 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.022; Restrained GooF = 1.021 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0382 * P )^2 + 0.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.68493 0.00155 0.000 OSF 2 1.76579 0.97624 0.000 BASF 1 3 0.01520 0.00230 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y C5 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 4 Maximum vector length = 511 Memory required = 1977 / 180891 wR2 = 0.0850 before cycle 4 for 2256 data and 144 / 144 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 0.006 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.022; Restrained GooF = 1.021 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0382 * P )^2 + 0.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.68493 0.00155 0.000 OSF 2 1.76590 0.97623 0.000 BASF 1 3 0.01520 0.00230 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y O2 Max. shift = 0.000 A for H1N Max. dU = 0.000 for C9 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1977 / 180891 wR2 = 0.0850 before cycle 5 for 2256 data and 144 / 144 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 0.006 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.022; Restrained GooF = 1.021 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0382 * P )^2 + 0.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.68493 0.00155 0.000 OSF 2 1.76577 0.97623 0.000 BASF 1 3 0.01520 0.00230 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y O2 Max. shift = 0.000 A for H1N Max. dU = 0.000 for O1 Least-squares cycle 6 Maximum vector length = 511 Memory required = 1977 / 180891 wR2 = 0.0850 before cycle 6 for 2256 data and 144 / 144 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 0.006 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.022; Restrained GooF = 1.021 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0382 * P )^2 + 0.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.68493 0.00155 0.000 OSF 2 1.76568 0.97619 0.000 BASF 1 3 0.01520 0.00230 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y N1 Max. shift = 0.000 A for H8B Max. dU = 0.000 for H1N Least-squares cycle 7 Maximum vector length = 511 Memory required = 1977 / 180891 wR2 = 0.0850 before cycle 7 for 2256 data and 144 / 144 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 0.006 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.022; Restrained GooF = 1.021 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0382 * P )^2 + 0.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.68493 0.00155 0.000 OSF 2 1.76575 0.97623 0.000 BASF 1 3 0.01520 0.00230 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y N1 Max. shift = 0.000 A for H11C Max. dU = 0.000 for H1N Least-squares cycle 8 Maximum vector length = 511 Memory required = 1977 / 180891 wR2 = 0.0850 before cycle 8 for 2256 data and 144 / 144 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 0.006 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.022; Restrained GooF = 1.021 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0382 * P )^2 + 0.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.68493 0.00155 0.000 OSF 2 1.76578 0.97625 0.000 BASF 1 3 0.01520 0.00230 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y N1 Max. shift = 0.000 A for H11C Max. dU = 0.000 for H1N Least-squares cycle 9 Maximum vector length = 511 Memory required = 1977 / 180891 wR2 = 0.0850 before cycle 9 for 2256 data and 144 / 144 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 0.006 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.022; Restrained GooF = 1.021 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0382 * P )^2 + 0.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.68493 0.00155 0.000 OSF 2 1.76584 0.97623 0.000 BASF 1 3 0.01520 0.00230 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y N1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for C10 Least-squares cycle 10 Maximum vector length = 511 Memory required = 1977 / 180891 wR2 = 0.0850 before cycle 10 for 2256 data and 144 / 144 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 0.006 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.022; Restrained GooF = 1.021 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0382 * P )^2 + 0.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.68493 0.00155 0.000 OSF 2 1.76571 0.97623 0.000 BASF 1 3 0.01520 0.00230 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y N1 Max. shift = 0.000 A for H11C Max. dU = 0.000 for H1N Least-squares cycle 11 Maximum vector length = 511 Memory required = 1977 / 180891 wR2 = 0.0850 before cycle 11 for 2256 data and 144 / 144 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 0.006 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.022; Restrained GooF = 1.021 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0382 * P )^2 + 0.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.68493 0.00155 0.000 OSF 2 1.76562 0.97624 0.000 BASF 1 3 0.01520 0.00230 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y N1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for N1 Least-squares cycle 12 Maximum vector length = 511 Memory required = 1977 / 180891 wR2 = 0.0850 before cycle 12 for 2256 data and 144 / 144 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 0.006 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.022; Restrained GooF = 1.021 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0382 * P )^2 + 0.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.68493 0.00155 0.000 OSF 2 1.76578 0.97628 0.000 BASF 1 3 0.01520 0.00230 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y N1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for C2 Least-squares cycle 13 Maximum vector length = 511 Memory required = 1977 / 180891 wR2 = 0.0850 before cycle 13 for 2256 data and 144 / 144 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 0.006 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.022; Restrained GooF = 1.021 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0382 * P )^2 + 0.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.68493 0.00155 0.000 OSF 2 1.76580 0.97626 0.000 BASF 1 3 0.01520 0.00230 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y N1 Max. shift = 0.000 A for H11A Max. dU = 0.000 for H1N Least-squares cycle 14 Maximum vector length = 511 Memory required = 1977 / 180891 wR2 = 0.0850 before cycle 14 for 2256 data and 144 / 144 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 0.006 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.022; Restrained GooF = 1.021 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0382 * P )^2 + 0.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.68493 0.00155 0.000 OSF 2 1.76585 0.97624 0.000 BASF 1 3 0.01520 0.00230 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y N1 Max. shift = 0.000 A for H11B Max. dU = 0.000 for C6 Least-squares cycle 15 Maximum vector length = 511 Memory required = 1977 / 180891 wR2 = 0.0850 before cycle 15 for 2256 data and 144 / 144 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 0.006 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.022; Restrained GooF = 1.021 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0382 * P )^2 + 0.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.68493 0.00155 0.000 OSF 2 1.76584 0.97623 0.000 BASF 1 3 0.01520 0.00230 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y N1 Max. shift = 0.000 A for H11A Max. dU = 0.000 for O2 Least-squares cycle 16 Maximum vector length = 511 Memory required = 1977 / 180891 wR2 = 0.0850 before cycle 16 for 2256 data and 144 / 144 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 0.006 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.022; Restrained GooF = 1.021 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0382 * P )^2 + 0.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.68493 0.00155 0.000 OSF 2 1.76590 0.97624 0.000 BASF 1 3 0.01520 0.00230 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y N1 Max. shift = 0.000 A for C11 Max. dU = 0.000 for C9 Largest correlation matrix elements 0.565 U13 C2 / U11 C2 0.545 EXTI / OSF 0.522 U13 N1 / U11 N1 0.563 U13 C8 / U11 C8 0.543 U13 C6 / U11 C6 0.519 U13 O2 / U33 O2 0.558 U13 C5 / U11 C5 0.535 U13 C7 / U11 C7 0.516 U13 O2 / U11 O2 0.555 U13 C4 / U11 C4 0.528 U13 C10 / U11 C10 0.513 U13 C9 / U33 C9 0.554 U13 C1 / U11 C1 0.526 U13 C1 / U33 C1 0.510 U13 C5 / U33 C5 0.550 U13 C11 / U11 C11 0.523 U13 C9 / U11 C9 0.510 U13 C7 / U33 C7 0.548 U13 O1 / U11 O1 0.523 U13 O3 / U11 O3 0.508 U13 O3 / U33 O3 Idealized hydrogen atom generation before cycle 17 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.8065 0.6877 0.8714 43 0.950 0.000 C2 C3 C1 H3 0.4987 0.6744 0.7345 43 0.950 0.000 C3 C2 C4 H5 0.5671 0.4937 1.0448 43 0.950 0.000 C5 C6 C4 H6 0.8736 0.5063 1.1827 43 0.950 0.000 C6 C5 C1 H8A 1.4155 0.6843 1.3561 137 0.980 0.000 C8 C7 H8A H8B 1.4072 0.6422 1.1631 137 0.980 0.000 C8 C7 H8A H8C 1.3798 0.6025 1.3388 137 0.980 0.000 C8 C7 H8A H10A -0.0057 0.6178 0.7160 23 0.990 0.000 C10 O2 C11 H10B -0.0294 0.5886 0.4990 23 0.990 0.000 C10 O2 C11 H11A -0.0239 0.7015 0.3848 137 0.980 0.000 C11 C10 H11A H11B 0.0153 0.7324 0.6045 137 0.980 0.000 C11 C10 H11A H11C -0.1737 0.6981 0.4613 137 0.980 0.000 C11 C10 H11A 2008lsh080 in Cc ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.87130 0.59863 1.04279 1.00000 0.01996 0.02090 0.02058 -0.00312 0.00956 -0.00058 0.02035 0.00323 0.00020 0.00008 0.00024 0.00000 0.00084 0.00076 0.00085 0.00066 0.00067 0.00059 0.00034 C2 0.75843 0.64850 0.90744 1.00000 0.02397 0.01980 0.02537 0.00117 0.01230 -0.00105 0.02263 0.00336 0.00021 0.00008 0.00024 0.00000 0.00089 0.00080 0.00084 0.00063 0.00070 0.00060 0.00036 H2 0.80651 0.68769 0.87140 1.00000 0.02716 0.00000 0.00000 C3 0.57522 0.64033 0.82591 1.00000 0.02188 0.02089 0.02364 -0.00013 0.00981 0.00090 0.02235 0.00342 0.00021 0.00008 0.00025 0.00000 0.00084 0.00077 0.00084 0.00066 0.00065 0.00060 0.00035 H3 0.49869 0.67439 0.73454 1.00000 0.02682 0.00000 0.00000 C4 0.50194 0.58298 0.87602 1.00000 0.02244 0.02108 0.02132 -0.00644 0.01094 -0.00223 0.02124 0.00329 0.00020 0.00009 0.00023 0.00000 0.00088 0.00078 0.00083 0.00064 0.00065 0.00058 0.00035 C5 0.61541 0.53309 1.00992 1.00000 0.02657 0.02238 0.02394 -0.00214 0.01312 -0.00345 0.02367 0.00343 0.00021 0.00009 0.00025 0.00000 0.00090 0.00083 0.00086 0.00065 0.00070 0.00064 0.00036 H5 0.56705 0.49372 1.04475 1.00000 0.02840 0.00000 0.00000 C6 0.79758 0.54063 1.09208 1.00000 0.02606 0.01969 0.02249 -0.00014 0.01098 0.00043 0.02277 0.00332 0.00020 0.00009 0.00024 0.00000 0.00090 0.00079 0.00084 0.00064 0.00068 0.00060 0.00035 H6 0.87362 0.50629 1.18267 1.00000 0.02733 0.00000 0.00000 C7 1.16109 0.65888 1.14666 1.00000 0.02373 0.02468 0.02194 -0.00165 0.01029 -0.00082 0.02349 0.00337 0.00021 0.00009 0.00024 0.00000 0.00087 0.00084 0.00080 0.00065 0.00068 0.00060 0.00035 C8 1.35808 0.64582 1.26114 1.00000 0.02360 0.02934 0.02983 -0.00147 0.01064 -0.00190 0.02816 0.00376 0.00022 0.00009 0.00028 0.00000 0.00090 0.00084 0.00091 0.00074 0.00073 0.00069 0.00038 H8A 1.41554 0.68427 1.35607 1.00000 0.04225 0.00000 0.00000 H8B 1.40718 0.64223 1.16312 1.00000 0.04225 0.00000 0.00000 H8C 1.37981 0.60245 1.33879 1.00000 0.04225 0.00000 0.00000 C9 0.30745 0.57439 0.79459 1.00000 0.02325 0.02394 0.02166 -0.00666 0.01056 -0.00192 0.02281 0.00339 0.00022 0.00009 0.00025 0.00000 0.00081 0.00083 0.00087 0.00067 0.00066 0.00062 0.00035 C10 0.02400 0.62612 0.60154 1.00000 0.01769 0.03603 0.02558 -0.00250 0.00855 -0.00082 0.02693 0.00368 0.00022 0.00009 0.00027 0.00000 0.00083 0.00098 0.00093 0.00070 0.00069 0.00063 0.00039 H10A -0.00569 0.61781 0.71604 1.00000 0.03231 0.00000 0.00000 H10B -0.02941 0.58863 0.49903 1.00000 0.03231 0.00000 0.00000 C11 -0.04562 0.69560 0.50458 1.00000 0.02782 0.03794 0.03979 -0.00104 0.01610 0.00654 0.03491 0.00442 0.00026 0.00010 0.00034 0.00000 0.00089 0.00101 0.00100 0.00087 0.00076 0.00079 0.00042 H11A -0.02388 0.70154 0.38477 1.00000 0.05236 0.00000 0.00000 H11B 0.01533 0.73241 0.60452 1.00000 0.05236 0.00000 0.00000 H11C -0.17366 0.69810 0.46130 1.00000 0.05236 0.00000 0.00000 N1 1.05753 0.60269 1.13401 1.00000 0.02080 0.01906 0.02582 0.00272 0.00927 0.00240 0.02240 0.00293 0.00018 0.00007 0.00022 0.00000 0.00068 0.00070 0.00073 0.00055 0.00055 0.00051 0.00031 O1 1.10036 0.71546 1.07201 1.00000 0.02604 0.02383 0.04043 0.00357 0.01075 -0.00017 0.03177 0.00266 0.00016 0.00006 0.00021 0.00000 0.00064 0.00061 0.00071 0.00055 0.00055 0.00047 0.00030 O2 0.21610 0.62759 0.67744 1.00000 0.01841 0.02868 0.03073 0.00018 0.00921 -0.00060 0.02669 0.00245 0.00015 0.00006 0.00018 0.00000 0.00058 0.00067 0.00070 0.00051 0.00051 0.00046 0.00029 O3 0.23726 0.52506 0.83358 1.00000 0.02693 0.02629 0.03341 -0.00294 0.01294 -0.00634 0.02917 0.00267 0.00017 0.00006 0.00021 0.00000 0.00062 0.00060 0.00067 0.00052 0.00050 0.00047 0.00029 H1N 1.11090 0.56441 1.19494 1.00000 0.03095 0.04319 0.00254 0.00090 0.00290 0.00000 0.00533 Final Structure Factor Calculation for 2008lsh080 in Cc Total number of l.s. parameters = 144 Maximum vector length = 511 Memory required = 1835 / 25046 wR2 = 0.0850 before cycle 17 for 2256 data and 2 / 144 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 0.006 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.022; Restrained GooF = 1.021 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0382 * P )^2 + 0.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0355 for 2073 Fo > 4sig(Fo) and 0.0410 for all 2256 data wR2 = 0.0850, GooF = S = 1.022, Restrained GooF = 1.021 for all data Occupancy sum of asymmetric unit = 15.00 for non-hydrogen and 13.00 for hydrogen atoms Principal mean square atomic displacements U 0.0239 0.0198 0.0173 C1 0.0257 0.0235 0.0187 C2 0.0244 0.0223 0.0203 C3 0.0277 0.0216 0.0144 C4 0.0288 0.0218 0.0204 C5 0.0264 0.0223 0.0196 C6 0.0255 0.0238 0.0211 C7 0.0318 0.0297 0.0230 C8 0.0296 0.0231 0.0158 C9 0.0367 0.0265 0.0176 C10 0.0432 0.0388 0.0227 C11 0.0277 0.0223 0.0171 N1 0.0463 0.0260 0.0231 O1 0.0331 0.0287 0.0183 O2 0.0345 0.0327 0.0202 O3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.022 0.032 0.043 0.053 0.064 0.078 0.097 0.124 0.179 1.000 Number in group 229. 238. 218. 252. 190. 231. 222. 223. 230. 223. GooF 0.989 1.029 0.993 1.027 1.104 0.982 1.132 0.960 0.980 1.025 K 1.014 0.986 0.988 0.983 0.980 0.993 1.006 1.006 1.021 1.021 Resolution(A) 0.77 0.80 0.83 0.88 0.93 0.99 1.06 1.16 1.33 1.68 inf Number in group 238. 213. 226. 227. 223. 233. 219. 224. 229. 224. GooF 1.014 1.065 1.074 0.986 0.971 1.086 0.917 0.838 1.024 1.199 K 1.012 1.057 0.999 0.999 1.019 1.014 1.020 1.015 1.017 1.014 R1 0.105 0.098 0.069 0.055 0.044 0.041 0.027 0.024 0.024 0.026 Recommended weighting scheme: WGHT 0.0364 0.3983 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 12 1 227.57 176.23 4.00 0.087 1.50 -3 21 1 34.81 71.47 3.66 0.056 0.87 6 0 -8 122.98 179.53 3.59 0.088 0.89 3 7 -2 242.13 192.91 3.55 0.091 1.91 -7 1 0 203.79 258.44 3.52 0.106 1.07 -2 10 0 1842.68 1584.06 3.44 0.262 1.72 -3 15 -2 117.43 153.73 3.42 0.082 1.02 2 4 -2 252.60 306.81 3.22 0.115 2.73 -1 19 4 40.78 69.04 3.09 0.055 0.88 6 0 2 148.52 188.11 3.00 0.090 1.02 3 13 5 55.75 29.70 2.99 0.036 0.82 4 2 -7 8.18 24.68 2.95 0.033 1.04 -10 6 2 77.34 49.57 2.94 0.046 0.79 -3 7 2 232.25 192.53 2.93 0.091 1.91 -7 17 3 3.94 19.96 2.88 0.029 0.83 -3 9 6 117.55 150.65 2.84 0.081 1.06 4 10 -3 17.57 9.39 2.79 0.020 1.36 -2 12 0 485.35 416.13 2.76 0.134 1.48 0 10 0 4.82 0.00 2.76 0.000 1.93 4 2 -5 425.93 366.03 2.74 0.126 1.40 3 15 5 83.14 54.41 2.68 0.048 0.78 -2 0 -6 231.82 182.78 2.66 0.089 0.94 -5 17 -1 4.30 14.45 2.66 0.025 0.87 -8 2 1 90.39 114.91 2.65 0.070 0.99 -10 4 2 68.15 43.59 2.61 0.043 0.81 -7 5 6 18.93 31.16 2.59 0.037 1.00 5 17 -4 89.76 113.43 2.57 0.070 0.90 0 8 7 113.19 150.69 2.56 0.081 0.87 2 8 1 42.11 30.91 2.52 0.037 1.81 2 12 0 475.09 417.26 2.51 0.134 1.48 2 12 -1 205.92 175.42 2.51 0.087 1.50 3 15 2 125.24 151.85 2.50 0.081 1.02 4 4 -7 21.78 32.92 2.48 0.038 1.02 -3 23 -1 30.87 48.33 2.47 0.046 0.78 6 8 2 34.35 47.38 2.46 0.045 0.94 2 12 4 116.75 143.46 2.45 0.079 1.01 -9 5 1 43.72 26.67 2.42 0.034 0.86 0 0 -2 1377.56 1559.08 2.41 0.260 3.26 -5 21 2 51.20 82.54 2.40 0.060 0.81 -1 1 -1 824.48 928.61 2.40 0.200 4.00 -4 6 5 292.17 251.84 2.39 0.104 1.29 2 8 6 20.75 33.26 2.39 0.038 0.87 -2 6 -2 103.10 84.11 2.39 0.060 1.72 -4 20 4 -5.58 5.41 2.39 0.015 0.83 -1 15 -6 -3.39 11.37 2.37 0.022 0.79 1 1 1 822.31 922.17 2.36 0.200 4.00 -3 17 4 1.42 12.96 2.35 0.024 0.96 8 16 -4 70.34 92.06 2.35 0.063 0.79 -5 19 1 109.79 153.88 2.33 0.082 0.86 -8 0 2 290.07 338.59 2.31 0.121 1.04 Bond lengths and angles C1 - Distance Angles C2 1.3980 (0.0022) N1 1.4037 (0.0021) 123.63 (0.14) C6 1.4044 (0.0022) 119.36 (0.14) 117.01 (0.14) C1 - C2 N1 C2 - Distance Angles C3 1.3911 (0.0022) C1 1.3980 (0.0022) 119.53 (0.14) H2 0.9500 120.24 120.24 C2 - C3 C1 C3 - Distance Angles C2 1.3911 (0.0022) C4 1.3951 (0.0021) 121.13 (0.15) H3 0.9500 119.43 119.43 C3 - C2 C4 C4 - Distance Angles C3 1.3951 (0.0021) C5 1.3959 (0.0023) 119.04 (0.15) C9 1.4798 (0.0022) 121.79 (0.14) 119.17 (0.14) C4 - C3 C5 C5 - Distance Angles C6 1.3813 (0.0022) C4 1.3959 (0.0023) 120.40 (0.15) H5 0.9500 119.80 119.80 C5 - C6 C4 C6 - Distance Angles C5 1.3813 (0.0022) C1 1.4044 (0.0022) 120.54 (0.15) H6 0.9500 119.73 119.73 C6 - C5 C1 C7 - Distance Angles O1 1.2233 (0.0020) N1 1.3687 (0.0021) 123.39 (0.14) C8 1.5050 (0.0022) 122.04 (0.15) 114.57 (0.14) C7 - O1 N1 C8 - Distance Angles C7 1.5050 (0.0022) 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 O3 1.2211 (0.0021) O2 1.3340 (0.0021) 123.26 (0.16) C4 1.4798 (0.0022) 124.12 (0.15) 112.59 (0.13) C9 - O3 O2 C10 - Distance Angles O2 1.4566 (0.0019) C11 1.5045 (0.0025) 106.92 (0.14) H10A 0.9900 110.34 110.34 H10B 0.9900 110.34 110.34 108.57 C10 - O2 C11 H10A C11 - Distance Angles C10 1.5045 (0.0025) H11A 0.9800 109.47 H11B 0.9800 109.47 109.47 H11C 0.9800 109.47 109.47 109.47 C11 - C10 H11A H11B N1 - Distance Angles C7 1.3687 (0.0021) C1 1.4037 (0.0021) 128.29 (0.13) H1N 0.8740 (0.0152) 117.94 (1.37) 113.68 (1.37) N1 - C7 C1 O1 - Distance Angles C7 1.2233 (0.0020) O1 - O2 - Distance Angles C9 1.3340 (0.0021) C10 1.4566 (0.0019) 116.64 (0.13) O2 - C9 O3 - Distance Angles C9 1.2211 (0.0021) O3 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.874(15) 2.039(16) 2.9130(19) 179.0(19) N1-H1N...O3_$1 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)