+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 21:22:05 on 10-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh076 in P2(1)/n CELL 0.71073 4.7969 12.4977 14.6790 90.000 98.336 90.000 ZERR 4.00 0.0001 0.0003 0.0003 0.000 0.001 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O I UNIT 32 32 4 4 4 V = 870.71 F(000) = 496.0 Mu = 3.62 mm-1 Cell Wt = 1044.22 Rho = 1.991 MERG 2 OMIT -3.00 55.00 OMIT 1 2 2 OMIT 1 0 1 OMIT 2 0 0 EQIV $1 x-1, y, z HTAB N1 O1_$1 DFIX 0.88 0.02 N1 H1N FMAP 2 PLAN 5 SIZE 0.20 0.30 0.80 ACTA BOND $H L.S. 20 TEMP -153.00 WGHT 0.016700 1.589900 EXTI 0.009907 FVAR 0.60878 C1 1 0.559572 0.058427 0.140978 11.00000 0.00934 0.01340 = 0.01436 -0.00147 0.00012 -0.00072 C2 1 0.478595 0.015430 0.221108 11.00000 0.00991 0.01636 = 0.01503 -0.00097 0.00126 -0.00157 C3 1 0.559606 -0.087334 0.250223 11.00000 0.01700 0.01881 = 0.02236 0.00520 0.00257 -0.00188 AFIX 43 H3 2 0.496654 -0.116825 0.303309 11.00000 -1.20000 AFIX 0 C4 1 0.733204 -0.146706 0.201245 11.00000 0.01955 0.01457 = 0.03003 0.00214 -0.00005 0.00283 AFIX 43 H4 2 0.790932 -0.216626 0.221192 11.00000 -1.20000 AFIX 0 C5 1 0.822041 -0.103536 0.123069 11.00000 0.01473 0.01798 = 0.02449 -0.00672 0.00163 0.00370 AFIX 43 H5 2 0.943877 -0.143463 0.090357 11.00000 -1.20000 AFIX 0 C6 1 0.733501 -0.002412 0.092646 11.00000 0.01246 0.01905 = 0.01501 -0.00249 0.00158 0.00115 AFIX 43 H6 2 0.791796 0.025782 0.038338 11.00000 -1.20000 AFIX 0 C7 1 0.618391 0.235064 0.072167 11.00000 0.01307 0.01647 = 0.01378 -0.00082 0.00422 0.00020 C8 1 0.464326 0.335675 0.038537 11.00000 0.01739 0.01919 = 0.02555 0.00656 0.00644 0.00202 AFIX 137 H8A 2 0.594735 0.384718 0.014125 11.00000 -1.50000 H8B 2 0.388692 0.370042 0.089753 11.00000 -1.50000 H8C 2 0.309231 0.317778 -0.010166 11.00000 -1.50000 AFIX 0 N1 3 0.460875 0.160390 0.108310 11.00000 0.00857 0.01532 = 0.01515 0.00164 0.00436 0.00241 O1 4 0.870926 0.223386 0.067721 11.00000 0.01203 0.02244 = 0.03295 0.00349 0.00839 0.00142 I1 5 0.247957 0.106141 0.304054 11.00000 0.01900 0.02055 = 0.01801 -0.00186 0.00889 -0.00212 H1N 2 0.288659 0.172664 0.110602 11.00000 0.01680 HKLF 4 Covalent radii and connectivity table for 2008lsh076 in P2(1)/n C 0.770 H 0.320 N 0.700 O 0.660 I 1.330 C1 - C6 C2 N1 C2 - C3 C1 I1 C3 - C4 C2 C4 - C5 C3 C5 - C6 C4 C6 - C5 C1 C7 - O1 N1 C8 C8 - C7 N1 - C7 C1 O1 - C7 I1 - C2 Operators for generating equivalent atoms: $1 x-1, y, z h k l Fo^2 Sigma Why rejected -2 0 1 12.64 1.37 observed but should be systematically absent -2 0 1 7.91 0.97 observed but should be systematically absent -3 0 2 3.88 0.88 observed but should be systematically absent 1 0 2 9.46 1.39 observed but should be systematically absent 1 0 2 6.18 1.14 observed but should be systematically absent 1 0 2 8.82 1.33 observed but should be systematically absent 3 0 2 3.48 0.73 observed but should be systematically absent -4 0 3 6.49 1.25 observed but should be systematically absent -4 0 3 5.64 0.97 observed but should be systematically absent 2 0 3 10.25 1.82 observed but should be systematically absent 2 0 9 19.73 3.63 observed but should be systematically absent 11493 Reflections read, of which 261 rejected -6 =< h =< 6, -16 =< k =< 15, -17 =< l =< 19, Max. 2-theta = 54.99 11 Systematic absence violations 0 Inconsistent equivalents 1995 Unique reflections, of which 0 suppressed R(int) = 0.0264 R(sigma) = 0.0201 Friedel opposites merged Maximum memory for data reduction = 1215 / 20178 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 = 1492 / 138232 wR2 = 0.0449 before cycle 1 for 1995 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 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.005; Restrained GooF = 1.005 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0167 * P )^2 + 1.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.60878 0.00104 0.003 OSF 2 0.00991 0.00059 -0.001 EXTI Mean shift/esd = 0.003 Maximum = 0.050 for U23 I1 Max. shift = 0.000 A for H8A Max. dU = 0.000 for H1N Least-squares cycle 2 Maximum vector length = 511 Memory required = 1492 / 138232 wR2 = 0.0449 before cycle 2 for 1995 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 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.005; Restrained GooF = 1.005 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0167 * P )^2 + 1.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.60878 0.00104 0.000 OSF 2 0.00991 0.00059 0.000 EXTI Mean shift/esd = 0.001 Maximum = 0.018 for U23 I1 Max. shift = 0.000 A for H8C Max. dU = 0.000 for N1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1492 / 138232 wR2 = 0.0449 before cycle 3 for 1995 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 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.005; Restrained GooF = 1.005 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0167 * P )^2 + 1.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.60878 0.00104 0.000 OSF 2 0.00991 0.00059 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for U23 I1 Max. shift = 0.000 A for H8C Max. dU = 0.000 for H1N Least-squares cycle 4 Maximum vector length = 511 Memory required = 1492 / 138232 wR2 = 0.0449 before cycle 4 for 1995 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 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.005; Restrained GooF = 1.005 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0167 * P )^2 + 1.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.60878 0.00104 -0.001 OSF 2 0.00991 0.00059 -0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 5 Maximum vector length = 511 Memory required = 1492 / 138232 wR2 = 0.0449 before cycle 5 for 1995 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 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.005; Restrained GooF = 1.006 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0167 * P )^2 + 1.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.60878 0.00104 0.000 OSF 2 0.00991 0.00059 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for EXTI Max. shift = 0.000 A for H8A Max. dU = 0.000 for H1N Least-squares cycle 6 Maximum vector length = 511 Memory required = 1492 / 138232 wR2 = 0.0449 before cycle 6 for 1995 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 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.005; Restrained GooF = 1.006 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0167 * P )^2 + 1.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.60878 0.00104 0.000 OSF 2 0.00991 0.00059 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for tors H8A Max. shift = 0.000 A for H8C Max. dU = 0.000 for H1N Least-squares cycle 7 Maximum vector length = 511 Memory required = 1492 / 138232 wR2 = 0.0449 before cycle 7 for 1995 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 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.005; Restrained GooF = 1.006 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0167 * P )^2 + 1.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.60878 0.00104 0.000 OSF 2 0.00991 0.00059 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for U11 I1 Max. shift = 0.000 A for H8A Max. dU = 0.000 for O1 Least-squares cycle 8 Maximum vector length = 511 Memory required = 1492 / 138232 wR2 = 0.0449 before cycle 8 for 1995 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 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.005; Restrained GooF = 1.006 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0167 * P )^2 + 1.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.60878 0.00104 0.000 OSF 2 0.00991 0.00059 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H8A Max. dU = 0.000 for H1N Least-squares cycle 9 Maximum vector length = 511 Memory required = 1492 / 138232 wR2 = 0.0449 before cycle 9 for 1995 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 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.005; Restrained GooF = 1.005 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0167 * P )^2 + 1.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.60878 0.00104 -0.001 OSF 2 0.00991 0.00059 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 10 Maximum vector length = 511 Memory required = 1492 / 138232 wR2 = 0.0449 before cycle 10 for 1995 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 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.005; Restrained GooF = 1.005 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0167 * P )^2 + 1.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.60878 0.00104 0.000 OSF 2 0.00991 0.00059 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for U22 I1 Max. shift = 0.000 A for H8A Max. dU = 0.000 for H1N Least-squares cycle 11 Maximum vector length = 511 Memory required = 1492 / 138232 wR2 = 0.0449 before cycle 11 for 1995 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 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.005; Restrained GooF = 1.005 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0167 * P )^2 + 1.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.60878 0.00104 0.000 OSF 2 0.00991 0.00059 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y I1 Max. shift = 0.000 A for H8B Max. dU = 0.000 for H1N Least-squares cycle 12 Maximum vector length = 511 Memory required = 1492 / 138232 wR2 = 0.0449 before cycle 12 for 1995 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 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.005; Restrained GooF = 1.005 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0167 * P )^2 + 1.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.60878 0.00104 0.000 OSF 2 0.00991 0.00059 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for EXTI Max. shift = 0.000 A for H8C Max. dU = 0.000 for H1N Least-squares cycle 13 Maximum vector length = 511 Memory required = 1492 / 138232 wR2 = 0.0449 before cycle 13 for 1995 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 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.005; Restrained GooF = 1.005 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0167 * P )^2 + 1.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.60878 0.00104 0.000 OSF 2 0.00991 0.00059 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y I1 Max. shift = 0.000 A for H8C Max. dU = 0.000 for H1N Least-squares cycle 14 Maximum vector length = 511 Memory required = 1492 / 138232 wR2 = 0.0449 before cycle 14 for 1995 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 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.005; Restrained GooF = 1.005 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0167 * P )^2 + 1.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.60878 0.00104 0.000 OSF 2 0.00991 0.00059 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y I1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 15 Maximum vector length = 511 Memory required = 1492 / 138232 wR2 = 0.0449 before cycle 15 for 1995 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 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.005; Restrained GooF = 1.006 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0167 * P )^2 + 1.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.60878 0.00104 0.000 OSF 2 0.00991 0.00059 0.000 EXTI 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 16 Maximum vector length = 511 Memory required = 1492 / 138232 wR2 = 0.0449 before cycle 16 for 1995 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 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.005; Restrained GooF = 1.005 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0167 * P )^2 + 1.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.60878 0.00104 0.000 OSF 2 0.00991 0.00059 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for U33 I1 Max. shift = 0.000 A for H8A Max. dU = 0.000 for H1N Least-squares cycle 17 Maximum vector length = 511 Memory required = 1492 / 138232 wR2 = 0.0449 before cycle 17 for 1995 data and 106 / 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 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.005; Restrained GooF = 1.005 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0167 * P )^2 + 1.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.60878 0.00104 -0.001 OSF 2 0.00991 0.00059 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 18 Maximum vector length = 511 Memory required = 1492 / 138232 wR2 = 0.0449 before cycle 18 for 1995 data and 106 / 106 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 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.005; Restrained GooF = 1.006 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0167 * P )^2 + 1.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.60878 0.00104 0.000 OSF 2 0.00991 0.00059 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for EXTI Max. shift = 0.000 A for H1N Max. dU = 0.000 for C8 Least-squares cycle 19 Maximum vector length = 511 Memory required = 1492 / 138232 wR2 = 0.0449 before cycle 19 for 1995 data and 106 / 106 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 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.005; Restrained GooF = 1.005 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0167 * P )^2 + 1.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.60878 0.00104 0.000 OSF 2 0.00991 0.00059 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y I1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 20 Maximum vector length = 511 Memory required = 1492 / 138232 wR2 = 0.0449 before cycle 20 for 1995 data and 106 / 106 parameters Summary of restraints applied in cycle 20 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 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.005; Restrained GooF = 1.006 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0167 * P )^2 + 1.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.60878 0.00104 0.000 OSF 2 0.00991 0.00059 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y I1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Largest correlation matrix elements 0.781 EXTI / OSF 0.696 U33 I1 / OSF 0.696 U22 I1 / OSF 0.692 U11 I1 / OSF Idealized hydrogen atom generation before cycle 21 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 0.4967 -0.1168 0.3033 43 0.950 0.000 C3 C4 C2 H4 0.7909 -0.2166 0.2212 43 0.950 0.000 C4 C5 C3 H5 0.9439 -0.1435 0.0904 43 0.950 0.000 C5 C6 C4 H6 0.7918 0.0258 0.0383 43 0.950 0.000 C6 C5 C1 H8A 0.5947 0.3847 0.0141 137 0.980 0.000 C8 C7 H8A H8B 0.3887 0.3700 0.0898 137 0.980 0.000 C8 C7 H8A H8C 0.3092 0.3178 -0.0102 137 0.980 0.000 C8 C7 H8A 2008lsh076 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.55957 0.05843 0.14098 1.00000 0.00934 0.01340 0.01436 -0.00147 0.00012 -0.00072 0.01252 0.00357 0.00041 0.00016 0.00014 0.00000 0.00089 0.00095 0.00095 0.00075 0.00072 0.00072 0.00039 C2 0.47860 0.01543 0.22111 1.00000 0.00991 0.01636 0.01503 -0.00097 0.00126 -0.00157 0.01382 0.00364 0.00042 0.00017 0.00014 0.00000 0.00088 0.00099 0.00097 0.00078 0.00072 0.00076 0.00040 C3 0.55961 -0.08733 0.25022 1.00000 0.01700 0.01881 0.02236 0.00520 0.00257 -0.00188 0.01942 0.00426 0.00049 0.00018 0.00017 0.00000 0.00107 0.00106 0.00116 0.00087 0.00087 0.00085 0.00046 H3 0.49665 -0.11683 0.30331 1.00000 0.02330 0.00000 0.00000 C4 0.73320 -0.14671 0.20125 1.00000 0.01955 0.01457 0.03003 0.00214 -0.00005 0.00283 0.02174 0.00421 0.00047 0.00019 0.00016 0.00000 0.00113 0.00109 0.00130 0.00088 0.00094 0.00084 0.00049 H4 0.79093 -0.21663 0.22119 1.00000 0.02609 0.00000 0.00000 C5 0.82204 -0.10354 0.12307 1.00000 0.01473 0.01798 0.02449 -0.00672 0.00163 0.00370 0.01919 0.00407 0.00049 0.00017 0.00017 0.00000 0.00107 0.00110 0.00120 0.00084 0.00088 0.00080 0.00047 H5 0.94388 -0.14346 0.09036 1.00000 0.02303 0.00000 0.00000 C6 0.73350 -0.00241 0.09265 1.00000 0.01246 0.01905 0.01501 -0.00249 0.00158 0.00115 0.01555 0.00377 0.00044 0.00017 0.00015 0.00000 0.00094 0.00103 0.00098 0.00081 0.00075 0.00080 0.00041 H6 0.79180 0.02578 0.03834 1.00000 0.01866 0.00000 0.00000 C7 0.61839 0.23506 0.07217 1.00000 0.01307 0.01647 0.01378 -0.00082 0.00422 0.00020 0.01421 0.00379 0.00044 0.00017 0.00014 0.00000 0.00095 0.00100 0.00095 0.00077 0.00074 0.00078 0.00040 C8 0.46433 0.33568 0.03854 1.00000 0.01739 0.01919 0.02555 0.00656 0.00644 0.00202 0.02038 0.00441 0.00047 0.00018 0.00016 0.00000 0.00106 0.00109 0.00118 0.00090 0.00087 0.00087 0.00046 H8A 0.59473 0.38471 0.01412 1.00000 0.03057 0.00000 0.00000 H8B 0.38871 0.37005 0.08975 1.00000 0.03057 0.00000 0.00000 H8C 0.30922 0.31778 -0.01016 1.00000 0.03057 0.00000 0.00000 N1 0.46088 0.16039 0.10831 1.00000 0.00857 0.01532 0.01515 0.00164 0.00436 0.00241 0.01276 0.00323 0.00036 0.00014 0.00012 0.00000 0.00081 0.00087 0.00085 0.00067 0.00064 0.00066 0.00035 O1 0.87093 0.22339 0.06772 1.00000 0.01203 0.02244 0.03295 0.00349 0.00839 0.00142 0.02197 0.00308 0.00032 0.00013 0.00012 0.00000 0.00074 0.00082 0.00093 0.00070 0.00064 0.00062 0.00035 I1 0.24796 0.10614 0.30405 1.00000 0.01900 0.02055 0.01801 -0.00186 0.00889 -0.00212 0.01857 0.00025 0.00003 0.00001 0.00001 0.00000 0.00011 0.00011 0.00011 0.00005 0.00006 0.00005 0.00008 H1N 0.28866 0.17266 0.11060 1.00000 0.01680 0.04559 0.00372 0.00213 0.00178 0.00000 0.00644 Final Structure Factor Calculation for 2008lsh076 in P2(1)/n Total number of l.s. parameters = 106 Maximum vector length = 511 Memory required = 1386 / 24017 wR2 = 0.0449 before cycle 21 for 1995 data and 0 / 106 parameters Summary of restraints applied in cycle 21 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 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.005; Restrained GooF = 1.006 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0167 * P )^2 + 1.59 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0184 for 1929 Fo > 4sig(Fo) and 0.0194 for all 1995 data wR2 = 0.0449, GooF = S = 1.005, Restrained GooF = 1.006 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 0.0158 0.0130 0.0088 C1 0.0170 0.0149 0.0095 C2 0.0266 0.0177 0.0140 C3 0.0319 0.0205 0.0129 C4 0.0299 0.0167 0.0110 C5 0.0206 0.0138 0.0122 C6 0.0167 0.0153 0.0106 C7 0.0303 0.0161 0.0148 C8 0.0178 0.0136 0.0068 N1 0.0346 0.0214 0.0099 O1 0.0254 0.0191 0.0112 I1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.030 0.057 0.091 0.127 0.168 0.212 0.261 0.330 0.429 1.000 Number in group 204. 201. 195. 198. 199. 199. 200. 201. 197. 201. GooF 1.480 0.955 0.982 1.074 0.859 0.837 0.842 0.803 0.949 1.075 K 1.526 1.032 0.976 0.973 0.985 0.991 0.998 0.999 1.009 1.004 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.96 1.04 1.14 1.31 1.60 inf Number in group 209. 190. 205. 195. 198. 200. 201. 200. 196. 201. GooF 0.984 0.805 0.896 0.801 0.820 0.887 0.787 1.001 1.269 1.526 K 0.977 0.988 0.999 1.003 1.006 1.012 1.013 1.014 1.003 0.993 R1 0.036 0.028 0.026 0.018 0.020 0.017 0.014 0.015 0.016 0.018 Recommended weighting scheme: WGHT 0.0108 1.1789 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 7 4 22.95 0.96 4.87 0.006 1.49 -3 6 5 27.12 0.64 4.56 0.005 1.21 0 1 9 345.52 249.57 4.36 0.091 1.60 3 0 5 20.68 1.75 4.35 0.008 1.31 3 12 3 82.05 7.32 4.19 0.016 0.84 2 7 3 16.72 0.33 4.18 0.003 1.34 0 6 1 3899.81 4356.09 4.06 0.381 2.06 0 0 6 64.36 118.68 4.06 0.063 2.42 1 6 1 2810.61 3148.99 3.86 0.324 1.88 -1 4 5 199.83 136.32 3.77 0.067 2.02 2 6 5 13.08 0.10 3.73 0.002 1.33 -2 7 5 13.93 0.26 3.73 0.003 1.33 0 2 8 27.07 7.43 3.73 0.016 1.74 -1 2 1 1448.63 1667.27 3.70 0.235 3.77 1 4 3 313.01 404.60 3.60 0.116 2.22 4 12 0 44.05 4.01 3.58 0.012 0.78 -2 3 5 666.62 798.72 3.56 0.163 1.79 2 2 2 327.14 249.79 3.55 0.091 2.05 -2 2 5 16.29 2.35 3.54 0.009 1.89 -1 0 1 4417.85 4910.38 3.43 0.404 4.72 -4 7 1 33.60 2.73 3.32 0.010 0.99 1 12 1 25.66 6.50 3.32 0.015 1.01 -3 2 3 1998.23 1778.43 3.27 0.243 1.53 -1 7 4 138.10 93.61 3.13 0.056 1.55 5 9 1 126.80 187.94 3.11 0.079 0.78 -1 2 6 1007.39 1151.47 3.10 0.196 2.15 4 11 2 296.99 383.73 3.02 0.113 0.81 1 5 1 474.56 394.41 2.97 0.114 2.16 -2 1 1 1158.30 1307.33 2.96 0.208 2.36 -1 3 1 250.98 314.21 2.86 0.102 3.12 -2 5 8 97.08 64.47 2.86 0.046 1.32 -1 3 6 5664.84 5276.62 2.82 0.419 2.01 -1 0 7 13651.49 12745.88 2.78 0.651 2.01 2 0 8 10443.00 9791.05 2.78 0.570 1.35 1 6 4 12.57 29.88 2.75 0.032 1.65 -2 2 1 14606.28 15547.34 2.69 0.719 2.24 -5 1 1 28.17 7.50 2.68 0.016 0.95 4 7 5 27.02 11.68 2.64 0.020 0.90 1 7 9 29.41 13.34 2.61 0.021 1.13 1 7 6 74.80 49.18 2.61 0.040 1.34 3 5 5 31.86 15.48 2.54 0.023 1.16 -4 3 15 312.74 406.21 2.54 0.116 0.80 -1 5 7 13.54 2.87 2.52 0.010 1.57 -3 12 1 93.68 58.51 2.52 0.044 0.87 -1 4 6 837.60 941.19 2.50 0.177 1.85 0 2 0 1398.46 1574.38 2.46 0.229 6.25 -2 9 8 15.28 3.53 2.45 0.011 1.04 -1 2 10 17175.54 16315.10 2.45 0.736 1.41 -5 4 6 293.79 363.86 2.45 0.110 0.89 4 9 4 146.60 200.95 2.42 0.082 0.85 Bond lengths and angles C1 - Distance Angles C6 1.3961 (0.0029) C2 1.3984 (0.0029) 118.52 (0.19) N1 1.4185 (0.0027) 120.81 (0.19) 120.65 (0.18) C1 - C6 C2 C2 - Distance Angles C3 1.3910 (0.0031) C1 1.3984 (0.0029) 120.92 (0.20) I1 2.0934 (0.0021) 117.97 (0.16) 121.05 (0.15) C2 - C3 C1 C3 - Distance Angles C4 1.3909 (0.0034) C2 1.3910 (0.0031) 119.69 (0.22) H3 0.9500 120.16 120.16 C3 - C4 C2 C4 - Distance Angles C5 1.3897 (0.0035) C3 1.3909 (0.0034) 119.86 (0.22) H4 0.9500 120.07 120.07 C4 - C5 C3 C5 - Distance Angles C6 1.3864 (0.0031) C4 1.3897 (0.0035) 120.24 (0.21) H5 0.9500 119.88 119.88 C5 - C6 C4 C6 - Distance Angles C5 1.3864 (0.0031) C1 1.3961 (0.0029) 120.70 (0.21) H6 0.9500 119.65 119.65 C6 - C5 C1 C7 - Distance Angles O1 1.2312 (0.0026) N1 1.3563 (0.0027) 123.19 (0.20) C8 1.5050 (0.0030) 121.45 (0.20) 115.36 (0.18) C7 - O1 N1 C8 - Distance Angles C7 1.5050 (0.0030) 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 1.3563 (0.0027) C1 1.4185 (0.0027) 124.95 (0.18) H1N 0.8457 (0.0166) 119.58 (1.84) 115.44 (1.84) N1 - C7 C1 O1 - Distance Angles C7 1.2312 (0.0026) O1 - I1 - Distance Angles C2 2.0934 (0.0021) I1 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.846(17) 2.109(18) 2.915(2) 159(2) N1-H1N...O1_$1 FMAP and GRID set by program FMAP 2 1 9 GRID -4.167 -2 -2 4.167 2 2 R1 = 0.0190 for 1995 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.55 at 0.2536 0.6072 0.4143 [ 0.91 A from H1N ] Deepest hole -0.64 at 0.1831 0.6082 0.1367 [ 0.89 A from I1 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 1884 / 17232 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2464 0.1072 0.0857 1.00000 0.05 0.55 0.91 H1N 1.23 N1 1.71 C1 2.30 O1 Q2 1 0.2470 0.1837 0.1981 1.00000 0.05 0.43 1.33 H1N 1.81 N1 1.83 I1 2.38 C2 Q3 1 0.6884 -0.1038 0.2425 1.00000 0.05 0.41 0.68 C3 0.86 C4 1.38 H3 1.54 H4 Q4 1 0.2736 0.3249 0.0483 1.00000 0.05 0.38 0.90 H8C 0.95 H8B 0.96 C8 1.85 H8A Q5 1 0.5030 0.3446 -0.0230 1.00000 0.05 0.38 0.82 H8A 0.96 C8 1.03 H8C 1.85 H8B Shortest distances between peaks (including symmetry equivalents) 4 5 1.64 1 2 1.91 1 4 2.78 2 4 2.84 Time profile in seconds ----------------------- 0.09: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.59: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.13: Structure factors and derivatives 0.86: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.25: Solve l.s. equations 0.00: Generate HTAB table 0.06: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + shelxl finished at 21:22:08 Total CPU time: 3.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++