+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 18:35:22 on 18-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh007 in P2(1)/c CELL 0.71073 9.5782 10.3047 9.4258 90.000 109.285 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 I UNIT 32 32 4 4 4 V = 878.13 F(000) = 496.0 Mu = 3.59 mm-1 Cell Wt = 1044.22 Rho = 1.975 MERG 2 OMIT -3.00 55.00 OMIT 2 1 2 OMIT -1 2 2 OMIT 0 1 2 OMIT -3 2 3 OMIT -2 0 2 OMIT -3 4 3 OMIT -2 4 1 OMIT 0 3 3 OMIT -3 0 2 OMIT -2 2 1 OMIT 1 2 1 OMIT 0 1 4 OMIT 4 1 0 OMIT 2 3 3 OMIT 0 2 1 FMAP 2 SIZE 0.4 0.2 0.16 EQIV $1 x, -y+1/2, z+1/2 HTAB N1 O1_$1 HTAB PLAN 5 DFIX 0.88 0.02 N1 H1N ACTA BOND $H L.S. 18 TEMP -153.00 WGHT 0.0253 0.7411 FVAR 0.21668 C1 1 1.360964 0.389503 0.453692 11.00000 0.01622 0.01466 = 0.01474 -0.00040 0.00399 -0.00287 C2 1 1.328353 0.413290 0.300494 11.00000 0.02252 0.02008 = 0.01352 0.00166 0.00594 0.00040 AFIX 43 H2 2 1.383839 0.371844 0.246502 11.00000 -1.20000 AFIX 0 C3 1 1.214516 0.497755 0.227241 11.00000 0.02229 0.02215 = 0.01671 0.00386 0.00423 0.00074 AFIX 43 H3 2 1.191172 0.512895 0.122542 11.00000 -1.20000 AFIX 0 C4 1 1.134894 0.559981 0.305528 11.00000 0.01668 0.01535 = 0.02527 0.00157 0.00287 0.00074 C5 1 1.167717 0.538825 0.459074 11.00000 0.02248 0.02250 = 0.02164 -0.00404 0.00845 0.00039 AFIX 43 H5 2 1.113500 0.582264 0.512979 11.00000 -1.20000 AFIX 0 C6 1 1.280161 0.453838 0.532013 11.00000 0.02133 0.02060 = 0.01652 -0.00419 0.00741 -0.00148 AFIX 43 H6 2 1.302930 0.438871 0.636677 11.00000 -1.20000 AFIX 0 C7 1 1.545127 0.211581 0.487534 11.00000 0.02059 0.01676 = 0.01363 -0.00023 0.00421 -0.00324 C8 1 1.657813 0.135568 0.608287 11.00000 0.02894 0.01960 = 0.02115 0.00289 0.00334 0.00625 AFIX 137 H8A 2 1.628510 0.044049 0.601513 11.00000 -1.50000 H8B 2 1.663663 0.169777 0.707099 11.00000 -1.50000 H8C 2 1.754684 0.143352 0.594924 11.00000 -1.50000 AFIX 0 N1 3 1.474574 0.304985 0.538326 11.00000 0.02078 0.01932 = 0.00911 0.00078 0.00190 0.00090 O1 4 1.518738 0.186751 0.353835 11.00000 0.03897 0.02987 = 0.01261 -0.00098 0.00845 0.00987 I1 5 0.958654 0.683484 0.191962 11.00000 0.02164 0.02303 = 0.03861 0.00211 0.00091 0.00481 H1N 2 1.496970 0.311318 0.636915 11.00000 0.03058 HKLF 4 Covalent radii and connectivity table for 2008lsh007 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 I 1.330 C1 - C2 C6 N1 C2 - C3 C1 C3 - C4 C2 C4 - C3 C5 I1 C5 - C6 C4 C6 - C5 C1 C7 - O1 N1 C8 C8 - C7 N1 - C7 C1 O1 - C7 I1 - C4 Operators for generating equivalent atoms: $1 x, -y+1/2, z+1/2 h k l Fo^2 Sigma Why rejected 0 0 9 0.12 0.02 observed but should be systematically absent -1 0 5 0.05 0.01 observed but should be systematically absent -1 0 3 0.09 0.01 observed but should be systematically absent 1 0 5 0.57 0.13 observed but should be systematically absent 1 0 9 0.37 0.08 observed but should be systematically absent -2 0 3 0.21 0.05 observed but should be systematically absent -2 0 3 0.27 0.05 observed but should be systematically absent -2 0 3 0.55 0.11 observed but should be systematically absent -2 0 1 0.33 0.07 observed but should be systematically absent 2 0 7 0.84 0.21 observed but should be systematically absent -9 0 1 0.65 0.13 observed but should be systematically absent 11187 Reflections read, of which 385 rejected -12 =< h =< 12, -13 =< k =< 13, -11 =< l =< 12, Max. 2-theta = 54.96 11 Systematic absence violations 0 Inconsistent equivalents 1990 Unique reflections, of which 0 suppressed R(int) = 0.0239 R(sigma) = 0.0214 Friedel opposites merged Maximum memory for data reduction = 1251 / 20010 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 = 1491 / 137102 wR2 = 0.0546 before cycle 1 for 1990 data and 105 / 105 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 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.087; Restrained GooF = 1.087 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0253 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.21488 0.00030 -6.081 OSF 96 0.02115 0.00011 -4.538 U11 I1 97 0.02245 0.00011 -5.208 U22 I1 98 0.03806 0.00012 -4.493 U33 I1 Mean shift/esd = 0.713 Maximum = -6.081 for OSF Max. shift = 0.011 A for H1N Max. dU =-0.003 for H1N Least-squares cycle 2 Maximum vector length = 511 Memory required = 1491 / 137102 wR2 = 0.0528 before cycle 2 for 1990 data and 105 / 105 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 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.055; Restrained GooF = 1.054 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0253 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.21430 0.00029 -2.026 OSF Mean shift/esd = 0.248 Maximum = -2.026 for OSF Max. shift = 0.005 A for H8B Max. dU =-0.001 for H1N Least-squares cycle 3 Maximum vector length = 511 Memory required = 1491 / 137102 wR2 = 0.0527 before cycle 3 for 1990 data and 105 / 105 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 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.053; Restrained GooF = 1.053 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0253 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.21430 0.00028 0.005 OSF Mean shift/esd = 0.007 Maximum = -0.074 for tors H8A Max. shift = 0.001 A for H8A Max. dU = 0.000 for H1N Least-squares cycle 4 Maximum vector length = 511 Memory required = 1491 / 137102 wR2 = 0.0527 before cycle 4 for 1990 data and 105 / 105 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 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.053; Restrained GooF = 1.053 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0253 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.21430 0.00028 0.010 OSF Mean shift/esd = 0.002 Maximum = -0.021 for tors H8A Max. shift = 0.000 A for H8A Max. dU = 0.000 for H1N Least-squares cycle 5 Maximum vector length = 511 Memory required = 1491 / 137102 wR2 = 0.0527 before cycle 5 for 1990 data and 105 / 105 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 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.053; Restrained GooF = 1.052 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0253 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.21430 0.00028 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.006 for tors H8A Max. shift = 0.000 A for H8A Max. dU = 0.000 for H1N Least-squares cycle 6 Maximum vector length = 511 Memory required = 1491 / 137102 wR2 = 0.0527 before cycle 6 for 1990 data and 105 / 105 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 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.053; Restrained GooF = 1.053 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0253 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.21430 0.00028 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.002 for tors H8A Max. shift = 0.000 A for H8A Max. dU = 0.000 for H1N Least-squares cycle 7 Maximum vector length = 511 Memory required = 1491 / 137102 wR2 = 0.0527 before cycle 7 for 1990 data and 105 / 105 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 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.053; Restrained GooF = 1.053 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0253 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.21430 0.00028 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for y I1 Max. shift = 0.000 A for H8B Max. dU = 0.000 for H1N Least-squares cycle 8 Maximum vector length = 511 Memory required = 1491 / 137102 wR2 = 0.0527 before cycle 8 for 1990 data and 105 / 105 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 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.053; Restrained GooF = 1.053 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0253 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.21430 0.00028 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for y I1 Max. shift = 0.000 A for H8B Max. dU = 0.000 for H1N Least-squares cycle 9 Maximum vector length = 511 Memory required = 1491 / 137102 wR2 = 0.0527 before cycle 9 for 1990 data and 105 / 105 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 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.053; Restrained GooF = 1.052 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0253 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.21430 0.00028 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for y I1 Max. shift = 0.000 A for H8C Max. dU = 0.000 for C4 Least-squares cycle 10 Maximum vector length = 511 Memory required = 1491 / 137102 wR2 = 0.0527 before cycle 10 for 1990 data and 105 / 105 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 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.053; Restrained GooF = 1.053 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0253 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.21430 0.00028 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for y I1 Max. shift = 0.000 A for H8C Max. dU = 0.000 for C1 Least-squares cycle 11 Maximum vector length = 511 Memory required = 1491 / 137102 wR2 = 0.0527 before cycle 11 for 1990 data and 105 / 105 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 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.053; Restrained GooF = 1.053 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0253 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.21430 0.00028 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for y I1 Max. shift = 0.000 A for H8C Max. dU = 0.000 for H1N Least-squares cycle 12 Maximum vector length = 511 Memory required = 1491 / 137102 wR2 = 0.0527 before cycle 12 for 1990 data and 105 / 105 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 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.053; Restrained GooF = 1.053 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0253 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.21430 0.00028 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for y I1 Max. shift = 0.000 A for H8B Max. dU = 0.000 for H1N Least-squares cycle 13 Maximum vector length = 511 Memory required = 1491 / 137102 wR2 = 0.0527 before cycle 13 for 1990 data and 105 / 105 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 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.053; Restrained GooF = 1.053 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0253 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.21430 0.00028 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for y I1 Max. shift = 0.000 A for H8C Max. dU = 0.000 for N1 Least-squares cycle 14 Maximum vector length = 511 Memory required = 1491 / 137102 wR2 = 0.0527 before cycle 14 for 1990 data and 105 / 105 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 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.053; Restrained GooF = 1.052 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0253 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.21430 0.00028 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for y I1 Max. shift = 0.000 A for H8C Max. dU = 0.000 for C5 Least-squares cycle 15 Maximum vector length = 511 Memory required = 1491 / 137102 wR2 = 0.0527 before cycle 15 for 1990 data and 105 / 105 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 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.053; Restrained GooF = 1.053 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0253 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.21430 0.00028 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for y I1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for I1 Least-squares cycle 16 Maximum vector length = 511 Memory required = 1491 / 137102 wR2 = 0.0527 before cycle 16 for 1990 data and 105 / 105 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 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.053; Restrained GooF = 1.052 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0253 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.21430 0.00028 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for y I1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 17 Maximum vector length = 511 Memory required = 1491 / 137102 wR2 = 0.0527 before cycle 17 for 1990 data and 105 / 105 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 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.053; Restrained GooF = 1.053 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0253 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.21430 0.00028 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for y I1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 18 Maximum vector length = 511 Memory required = 1491 / 137102 wR2 = 0.0527 before cycle 18 for 1990 data and 105 / 105 parameters Summary of restraints applied in cycle 18 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 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.053; Restrained GooF = 1.053 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0253 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.21430 0.00028 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for y I1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Largest correlation matrix elements 0.619 U22 I1 / OSF 0.616 U11 I1 / OSF 0.605 U33 I1 / OSF Idealized hydrogen atom generation before cycle 19 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 1.3838 0.3719 0.2463 43 0.950 0.000 C2 C3 C1 H3 1.1912 0.5135 0.1226 43 0.950 0.000 C3 C4 C2 H5 1.1142 0.5829 0.5130 43 0.950 0.000 C5 C6 C4 H6 1.3029 0.4387 0.6365 43 0.950 0.000 C6 C5 C1 H8A 1.6278 0.0446 0.6026 137 0.980 0.000 C8 C7 H8A H8B 1.6647 0.1710 0.7070 137 0.980 0.000 C8 C7 H8A H8C 1.7544 0.1426 0.5941 137 0.980 0.000 C8 C7 H8A 2008lsh007 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 1.36084 0.38952 0.45362 1.00000 0.01588 0.01350 0.01397 -0.00075 0.00385 -0.00319 0.01472 0.00355 0.00020 0.00018 0.00020 0.00000 0.00083 0.00082 0.00082 0.00064 0.00065 0.00067 0.00034 C2 1.32831 0.41334 0.30036 1.00000 0.02172 0.01922 0.01365 0.00123 0.00613 -0.00008 0.01813 0.00383 0.00022 0.00019 0.00021 0.00000 0.00093 0.00091 0.00084 0.00068 0.00070 0.00075 0.00037 H2 1.38376 0.37189 0.24633 1.00000 0.02175 0.00000 0.00000 C3 1.21438 0.49802 0.22717 1.00000 0.02178 0.02055 0.01588 0.00316 0.00405 -0.00064 0.01994 0.00395 0.00022 0.00019 0.00022 0.00000 0.00093 0.00094 0.00088 0.00070 0.00071 0.00076 0.00038 H3 1.19117 0.51352 0.12255 1.00000 0.02392 0.00000 0.00000 C4 1.13480 0.55969 0.30548 1.00000 0.01654 0.01496 0.02424 0.00161 0.00256 0.00055 0.01961 0.00388 0.00021 0.00018 0.00022 0.00000 0.00087 0.00087 0.00098 0.00072 0.00073 0.00071 0.00038 C5 1.16800 0.53903 0.45899 1.00000 0.02106 0.02186 0.02176 -0.00462 0.00811 -0.00010 0.02130 0.00393 0.00022 0.00020 0.00022 0.00000 0.00095 0.00099 0.00097 0.00075 0.00077 0.00078 0.00040 H5 1.11423 0.58292 0.51302 1.00000 0.02556 0.00000 0.00000 C6 1.28027 0.45380 0.53187 1.00000 0.02042 0.02018 0.01506 -0.00321 0.00645 -0.00151 0.01841 0.00376 0.00021 0.00019 0.00021 0.00000 0.00091 0.00094 0.00086 0.00068 0.00070 0.00075 0.00037 H6 1.30295 0.43871 0.63650 1.00000 0.02209 0.00000 0.00000 C7 1.54508 0.21185 0.48749 1.00000 0.01971 0.01578 0.01339 0.00014 0.00453 -0.00312 0.01653 0.00382 0.00022 0.00019 0.00021 0.00000 0.00093 0.00084 0.00085 0.00069 0.00070 0.00074 0.00036 C8 1.65781 0.13587 0.60832 1.00000 0.02749 0.01935 0.01937 0.00201 0.00288 0.00528 0.02327 0.00429 0.00024 0.00021 0.00023 0.00000 0.00106 0.00099 0.00095 0.00076 0.00079 0.00083 0.00041 H8A 1.62775 0.04459 0.60257 1.00000 0.03491 0.00000 0.00000 H8B 1.66473 0.17097 0.70705 1.00000 0.03491 0.00000 0.00000 H8C 1.75437 0.14257 0.59406 1.00000 0.03491 0.00000 0.00000 N1 1.47432 0.30530 0.53814 1.00000 0.01994 0.01729 0.00851 0.00008 0.00279 0.00020 0.01572 0.00330 0.00020 0.00015 0.00018 0.00000 0.00085 0.00080 0.00074 0.00054 0.00061 0.00060 0.00033 O1 1.51874 0.18661 0.35397 1.00000 0.03866 0.02715 0.01215 -0.00093 0.00820 0.00987 0.02603 0.00330 0.00020 0.00013 0.00017 0.00000 0.00097 0.00087 0.00068 0.00052 0.00065 0.00062 0.00036 I1 0.95865 0.68348 0.19197 1.00000 0.02099 0.02226 0.03788 0.00213 0.00070 0.00480 0.02927 0.00028 0.00001 0.00001 0.00002 0.00000 0.00010 0.00011 0.00012 0.00005 0.00007 0.00005 0.00008 H1N 1.49733 0.31217 0.63567 1.00000 0.02609 0.04549 0.00318 0.00222 0.00199 0.00000 0.00719 Final Structure Factor Calculation for 2008lsh007 in P2(1)/c Total number of l.s. parameters = 105 Maximum vector length = 511 Memory required = 1386 / 24017 wR2 = 0.0527 before cycle 19 for 1990 data and 0 / 105 parameters Summary of restraints applied in cycle 19 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 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.053; Restrained GooF = 1.053 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0253 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0197 for 1874 Fo > 4sig(Fo) and 0.0215 for all 1990 data wR2 = 0.0527, GooF = S = 1.053, Restrained GooF = 1.053 for all data Occupancy sum of asymmetric unit = 11.00 for non-hydrogen and 8.00 for hydrogen atoms Principal mean square atomic displacements U 0.0186 0.0144 0.0112 C1 0.0219 0.0195 0.0130 C2 0.0250 0.0205 0.0143 C3 0.0283 0.0163 0.0143 C4 0.0265 0.0211 0.0164 C5 0.0223 0.0196 0.0133 C6 0.0222 0.0141 0.0133 C7 0.0335 0.0213 0.0150 C8 0.0214 0.0173 0.0085 N1 0.0456 0.0217 0.0109 O1 0.0463 0.0258 0.0157 I1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.026 0.052 0.081 0.114 0.152 0.196 0.249 0.321 0.419 1.000 Number in group 204. 196. 202. 198. 201. 193. 200. 199. 197. 200. GooF 1.232 1.072 1.259 1.167 1.061 0.965 0.797 0.960 0.886 1.024 K 1.266 1.009 0.963 0.972 0.988 0.999 1.001 1.009 1.011 0.992 Resolution(A) 0.77 0.80 0.83 0.86 0.91 0.97 1.04 1.14 1.29 1.59 inf Number in group 201. 202. 198. 200. 194. 200. 198. 198. 199. 200. GooF 1.126 1.104 0.946 0.985 0.842 0.930 0.957 0.915 1.025 1.527 K 0.964 0.997 0.995 1.004 1.013 1.017 1.023 1.017 1.003 0.973 R1 0.049 0.039 0.032 0.025 0.019 0.017 0.017 0.014 0.012 0.020 Recommended weighting scheme: WGHT 0.0169 0.8486 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 0 986.34 1555.36 6.23 0.263 6.80 -1 4 5 6.79 0.14 4.13 0.002 1.51 1 1 3 431.75 530.98 4.10 0.154 2.50 0 0 4 1845.47 1610.17 3.44 0.268 2.22 -7 10 2 84.92 128.89 3.42 0.076 0.82 -6 11 5 94.26 143.92 3.37 0.080 0.78 -3 3 2 401.64 334.94 3.30 0.122 2.26 0 1 5 289.46 349.48 3.23 0.125 1.75 -1 9 8 149.02 211.50 3.20 0.097 0.81 -3 2 6 122.79 90.71 3.18 0.064 1.48 1 1 2 12438.42 13722.76 3.12 0.782 3.36 -3 1 3 31.23 16.48 3.09 0.027 2.51 5 0 2 75.14 107.92 3.01 0.069 1.51 10 1 3 229.48 289.30 2.98 0.114 0.79 -3 2 1 2039.06 2265.49 2.97 0.318 2.71 1 2 10 646.48 767.46 2.95 0.185 0.85 0 6 4 7.28 0.35 2.95 0.004 1.36 7 3 3 10.87 1.41 2.93 0.008 1.02 0 1 7 86.19 62.70 2.93 0.053 1.26 -1 3 3 4632.40 5082.37 2.92 0.476 2.32 -4 2 3 3721.64 4089.63 2.87 0.427 2.01 -1 7 5 9.56 1.18 2.86 0.007 1.16 -1 1 2 3294.28 3625.69 2.82 0.402 4.23 3 2 2 2067.07 1866.48 2.82 0.289 2.01 -3 11 3 16.51 4.24 2.81 0.014 0.88 -4 1 11 8.27 53.37 2.76 0.049 0.85 9 5 3 164.37 205.80 2.71 0.096 0.80 1 1 1 33.61 20.84 2.68 0.030 4.85 0 2 0 9065.30 10059.90 2.67 0.670 5.15 4 9 6 43.11 22.82 2.66 0.032 0.79 -2 4 3 4894.57 5309.92 2.61 0.487 1.95 0 2 11 103.67 139.31 2.60 0.079 0.80 9 3 4 38.42 61.00 2.60 0.052 0.80 -8 5 8 196.31 239.77 2.57 0.103 0.88 0 5 9 12.95 0.16 2.56 0.003 0.89 -2 4 9 424.70 364.75 2.55 0.128 0.96 9 7 1 24.57 49.91 2.54 0.047 0.81 -6 6 10 40.92 63.62 2.52 0.053 0.80 -3 5 2 283.14 242.11 2.51 0.104 1.70 -4 1 3 859.29 772.62 2.50 0.186 2.13 -8 10 3 361.92 443.99 2.44 0.141 0.78 -1 1 4 6862.01 7428.50 2.44 0.576 2.29 3 4 6 17.30 8.64 2.44 0.020 1.08 -9 8 3 13.31 0.10 2.43 0.002 0.82 -9 1 10 308.94 366.70 2.43 0.128 0.81 -9 8 5 -0.67 8.64 2.42 0.020 0.81 2 2 4 233.31 271.96 2.40 0.110 1.68 -1 4 1 11947.91 12834.25 2.38 0.757 2.44 -12 1 6 373.14 451.99 2.38 0.142 0.78 -8 10 4 150.72 191.41 2.38 0.092 0.78 Bond lengths and angles C1 - Distance Angles C2 1.3953 (0.0025) C6 1.3979 (0.0025) 119.31 (0.17) N1 1.4133 (0.0025) 123.97 (0.17) 116.70 (0.16) C1 - C2 C6 C2 - Distance Angles C3 1.3896 (0.0027) C1 1.3953 (0.0025) 119.65 (0.17) H2 0.9500 120.18 120.18 C2 - C3 C1 C3 - Distance Angles C4 1.3788 (0.0028) C2 1.3896 (0.0027) 120.39 (0.17) H3 0.9500 119.80 119.80 C3 - C4 C2 C4 - Distance Angles C3 1.3788 (0.0028) C5 1.3915 (0.0028) 120.61 (0.18) I1 2.1038 (0.0019) 119.96 (0.14) 119.41 (0.15) C4 - C3 C5 C5 - Distance Angles C6 1.3826 (0.0028) C4 1.3915 (0.0028) 119.14 (0.18) H5 0.9500 120.43 120.43 C5 - C6 C4 C6 - Distance Angles C5 1.3826 (0.0028) C1 1.3979 (0.0026) 120.87 (0.17) H6 0.9500 119.57 119.57 C6 - C5 C1 C7 - Distance Angles O1 1.2270 (0.0025) N1 1.3522 (0.0026) 123.77 (0.18) C8 1.5046 (0.0027) 121.28 (0.19) 114.92 (0.16) C7 - O1 N1 C8 - Distance Angles C7 1.5046 (0.0027) 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 N1 - Distance Angles C7 1.3522 (0.0026) C1 1.4133 (0.0025) 128.33 (0.16) H1N 0.8746 (0.0172) 116.56 (1.71) 115.01 (1.73) N1 - C7 C1 O1 - Distance Angles C7 1.2270 (0.0025) O1 - I1 - Distance Angles C4 2.1038 (0.0019) I1 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.875(17) 1.999(18) 2.866(2) 171(3) 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)