+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 18:45:49 on 18-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh008 in P2(1)/c CELL 0.71073 11.6779 9.4902 7.4186 90.000 106.515 90.000 ZERR 4.00 0.0009 0.0007 0.0006 0.000 0.005 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 36 44 4 4 V = 788.25 F(000) = 320.0 Mu = 0.08 mm-1 Cell Wt = 596.75 Rho = 1.257 MERG 2 OMIT -3.00 55.00 OMIT 0 2 1 FMAP 2 PLAN 5 ACTA SIZE 0.26 0.2 0.06 DFIX 0.88 0.02 N1 H1N BOND $H EQIV $1 -x+1, y-1/2, -z+1/2 HTAB N1 O1_$1 L.S. 16 TEMP -153.00 WGHT 0.0569 0.2251 FVAR 0.49095 C1 1 0.675430 0.072797 0.218482 11.00000 0.02197 0.01931 = 0.01748 -0.00248 0.00626 -0.00054 C2 1 0.707621 0.183749 0.118689 11.00000 0.02507 0.02045 = 0.02044 0.00205 0.00725 0.00201 AFIX 43 H2 2 0.649782 0.251378 0.056835 11.00000 -1.20000 AFIX 0 C3 1 0.824632 0.194437 0.110584 11.00000 0.02654 0.02187 = 0.02030 0.00120 0.00877 -0.00103 AFIX 43 H3 2 0.845608 0.270257 0.042585 11.00000 -1.20000 AFIX 0 C4 1 0.912380 0.097450 0.199053 11.00000 0.02352 0.02184 = 0.02188 -0.00404 0.00843 -0.00124 C5 1 0.878183 -0.013296 0.296446 11.00000 0.02350 0.01831 = 0.02598 -0.00001 0.00554 0.00363 AFIX 43 H5 2 0.935876 -0.081433 0.357183 11.00000 -1.20000 AFIX 0 C6 1 0.761876 -0.025969 0.306428 11.00000 0.02416 0.01789 = 0.02257 0.00137 0.00762 -0.00066 AFIX 43 H6 2 0.740874 -0.102330 0.373525 11.00000 -1.20000 AFIX 0 C7 1 0.467110 0.143789 0.199506 11.00000 0.02269 0.02106 = 0.01884 -0.00314 0.00489 0.00004 C8 1 0.353441 0.088522 0.230994 11.00000 0.02200 0.02626 = 0.02873 -0.00266 0.00833 -0.00119 AFIX 137 H8A 2 0.331394 0.147105 0.324701 11.00000 -1.50000 H8B 2 0.365624 -0.008867 0.276336 11.00000 -1.50000 H8C 2 0.289335 0.091364 0.112436 11.00000 -1.50000 AFIX 0 C9 1 1.039933 0.111042 0.193393 11.00000 0.02467 0.02646 = 0.03159 -0.00031 0.01039 -0.00086 AFIX 137 H9A 2 1.041247 0.147178 0.070249 11.00000 -1.50000 H9B 2 1.078620 0.018457 0.214403 11.00000 -1.50000 H9C 2 1.082848 0.176327 0.291848 11.00000 -1.50000 AFIX 0 N1 3 0.558459 0.050354 0.232766 11.00000 0.02034 0.01723 = 0.02401 0.00074 0.00671 -0.00034 O1 4 0.474919 0.265962 0.147392 11.00000 0.02889 0.02082 = 0.03242 0.00333 0.01180 0.00413 H1N 2 0.544765 -0.033532 0.276854 11.00000 0.02733 HKLF 4 Covalent radii and connectivity table for 2008lsh008 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 C1 - C6 C2 N1 C2 - C3 C1 C3 - C2 C4 C4 - C3 C5 C9 C5 - C6 C4 C6 - C5 C1 C7 - O1 N1 C8 C8 - C7 C9 - C4 N1 - C7 C1 O1 - C7 Operators for generating equivalent atoms: $1 -x+1, y-1/2, -z+1/2 9341 Reflections read, of which 329 rejected -15 =< h =< 14, -12 =< k =< 12, -9 =< l =< 9, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 1807 Unique reflections, of which 0 suppressed R(int) = 0.0538 R(sigma) = 0.0484 Friedel opposites merged Maximum memory for data reduction = 1313 / 18100 Default effective X-H distances for T = -153.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 1.00 0.99 0.98 0.95 0.88 0.91 1.12 0.84 0.95 0.88 0.95 Note that these distances are chosen to give the best fit to the X-ray data and so avoid the introduction of systematic error. The true internuclear distances are longer and do not vary with temperature ! The apparent variation with temperature is caused by libration. Least-squares cycle 1 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1192 before cycle 1 for 1807 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 0.012 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.045; Restrained GooF = 1.045 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0569 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.49039 0.00147 -0.384 OSF Mean shift/esd = 0.429 Maximum = 1.091 for y C6 Max. shift = 0.011 A for H1N Max. dU =-0.001 for H1N Least-squares cycle 2 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1177 before cycle 2 for 1807 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 0.015 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.034; Restrained GooF = 1.034 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0569 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.49010 0.00145 -0.202 OSF Mean shift/esd = 0.148 Maximum = 0.393 for U13 C9 Max. shift = 0.004 A for H1N Max. dU = 0.000 for C4 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1176 before cycle 3 for 1807 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 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.033; Restrained GooF = 1.033 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0569 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.49010 0.00144 0.006 OSF Mean shift/esd = 0.008 Maximum = -0.041 for x H1N Max. shift = 0.001 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 4 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1176 before cycle 4 for 1807 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 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.033; Restrained GooF = 1.032 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0569 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.49013 0.00144 0.019 OSF Mean shift/esd = 0.002 Maximum = 0.019 for OSF Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 5 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1176 before cycle 5 for 1807 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 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.033; Restrained GooF = 1.032 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0569 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.49013 0.00144 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for tors H8A Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 6 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1176 before cycle 6 for 1807 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 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.033; Restrained GooF = 1.033 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0569 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.49013 0.00145 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x C2 Max. shift = 0.000 A for H8B Max. dU = 0.000 for H1N Least-squares cycle 7 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1176 before cycle 7 for 1807 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 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.033; Restrained GooF = 1.033 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0569 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.49013 0.00145 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H1N Max. dU = 0.000 for C9 Least-squares cycle 8 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1176 before cycle 8 for 1807 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 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.033; Restrained GooF = 1.032 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0569 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.49013 0.00144 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x C2 Max. shift = 0.000 A for H1N Max. dU = 0.000 for C9 Least-squares cycle 9 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1176 before cycle 9 for 1807 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 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.033; Restrained GooF = 1.032 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0569 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.49013 0.00144 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x N1 Max. shift = 0.000 A for H9A Max. dU = 0.000 for C9 Least-squares cycle 10 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1176 before cycle 10 for 1807 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 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.033; Restrained GooF = 1.033 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0569 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.49013 0.00145 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 = 1614 / 137210 wR2 = 0.1176 before cycle 11 for 1807 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 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.033; Restrained GooF = 1.033 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0569 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.49013 0.00145 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 12 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1176 before cycle 12 for 1807 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 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.033; Restrained GooF = 1.033 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0569 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.49013 0.00145 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x N1 Max. shift = 0.000 A for N1 Max. dU = 0.000 for H1N Least-squares cycle 13 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1176 before cycle 13 for 1807 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 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.033; Restrained GooF = 1.033 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0569 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.49013 0.00145 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x C2 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 14 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1176 before cycle 14 for 1807 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 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.033; Restrained GooF = 1.033 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0569 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.49013 0.00144 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x N1 Max. shift = 0.000 A for H9A Max. dU = 0.000 for H1N Least-squares cycle 15 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1176 before cycle 15 for 1807 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 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.033; Restrained GooF = 1.033 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0569 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.49013 0.00145 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 16 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1176 before cycle 16 for 1807 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 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.033; Restrained GooF = 1.033 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0569 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.49013 0.00144 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x N1 Max. shift = 0.000 A for H9C 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 0.6499 0.2513 0.0570 43 0.950 0.000 C2 C3 C1 H3 0.8456 0.2701 0.0426 43 0.950 0.000 C3 C2 C4 H5 0.9357 -0.0815 0.3567 43 0.950 0.000 C5 C6 C4 H6 0.7411 -0.1021 0.3736 43 0.950 0.000 C6 C5 C1 H8A 0.3315 0.1470 0.3248 137 0.980 0.000 C8 C7 H8A H8B 0.3654 -0.0089 0.2756 137 0.980 0.000 C8 C7 H8A H8C 0.2893 0.0918 0.1123 137 0.980 0.000 C8 C7 H8A H9A 1.0411 0.1482 0.0704 137 0.980 0.000 C9 C4 H9A H9B 1.0784 0.0185 0.2130 137 0.980 0.000 C9 C4 H9A H9C 1.0831 0.1759 0.2923 137 0.980 0.000 C9 C4 H9A 2008lsh008 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.67549 0.07284 0.21840 1.00000 0.02158 0.01902 0.01668 -0.00292 0.00569 -0.00054 0.01904 0.00255 0.00012 0.00014 0.00018 0.00000 0.00072 0.00069 0.00062 0.00052 0.00053 0.00052 0.00031 C2 0.70770 0.18362 0.11885 1.00000 0.02498 0.01987 0.01995 0.00161 0.00652 0.00215 0.02157 0.00272 0.00013 0.00014 0.00019 0.00000 0.00077 0.00068 0.00066 0.00054 0.00055 0.00055 0.00032 H2 0.64989 0.25128 0.05701 1.00000 0.02588 0.00000 0.00000 C3 0.82466 0.19431 0.11076 1.00000 0.02686 0.02093 0.01980 0.00088 0.00876 -0.00146 0.02209 0.00272 0.00013 0.00015 0.00019 0.00000 0.00079 0.00070 0.00067 0.00054 0.00056 0.00057 0.00033 H3 0.84558 0.27009 0.04264 1.00000 0.02651 0.00000 0.00000 C4 0.91246 0.09753 0.19925 1.00000 0.02295 0.02132 0.02140 -0.00417 0.00837 -0.00152 0.02146 0.00263 0.00013 0.00015 0.00019 0.00000 0.00075 0.00071 0.00069 0.00055 0.00056 0.00055 0.00033 C5 0.87808 -0.01317 0.29623 1.00000 0.02300 0.01849 0.02539 -0.00024 0.00539 0.00323 0.02260 0.00271 0.00013 0.00015 0.00020 0.00000 0.00075 0.00070 0.00071 0.00056 0.00057 0.00054 0.00033 H5 0.93568 -0.08148 0.35672 1.00000 0.02712 0.00000 0.00000 C6 0.76202 -0.02576 0.30634 1.00000 0.02522 0.01744 0.02170 0.00164 0.00767 -0.00054 0.02125 0.00264 0.00013 0.00014 0.00019 0.00000 0.00078 0.00068 0.00069 0.00054 0.00057 0.00053 0.00033 H6 0.74109 -0.10206 0.37363 1.00000 0.02550 0.00000 0.00000 C7 0.46709 0.14368 0.19951 1.00000 0.02366 0.02074 0.01821 -0.00334 0.00507 0.00021 0.02105 0.00262 0.00013 0.00015 0.00019 0.00000 0.00078 0.00070 0.00064 0.00055 0.00053 0.00054 0.00032 C8 0.35344 0.08859 0.23079 1.00000 0.02222 0.02628 0.02812 -0.00266 0.00804 -0.00076 0.02536 0.00283 0.00013 0.00016 0.00021 0.00000 0.00078 0.00077 0.00075 0.00061 0.00059 0.00057 0.00035 H8A 0.33155 0.14698 0.32482 1.00000 0.03804 0.00000 0.00000 H8B 0.36543 -0.00893 0.27564 1.00000 0.03804 0.00000 0.00000 H8C 0.28931 0.09184 0.11228 1.00000 0.03804 0.00000 0.00000 C9 1.03989 0.11124 0.19323 1.00000 0.02536 0.02618 0.03214 -0.00062 0.01131 -0.00056 0.02724 0.00299 0.00013 0.00016 0.00022 0.00000 0.00081 0.00077 0.00080 0.00063 0.00063 0.00060 0.00036 H9A 1.04106 0.14820 0.07042 1.00000 0.04087 0.00000 0.00000 H9B 1.07842 0.01854 0.21300 1.00000 0.04087 0.00000 0.00000 H9C 1.08305 0.17588 0.29235 1.00000 0.04087 0.00000 0.00000 N1 0.55851 0.05046 0.23272 1.00000 0.02048 0.01710 0.02394 0.00071 0.00705 -0.00034 0.02035 0.00222 0.00010 0.00012 0.00016 0.00000 0.00064 0.00061 0.00062 0.00048 0.00047 0.00046 0.00029 O1 0.47489 0.26598 0.14730 1.00000 0.02938 0.02025 0.03215 0.00320 0.01206 0.00400 0.02658 0.00205 0.00009 0.00010 0.00015 0.00000 0.00061 0.00053 0.00058 0.00042 0.00045 0.00041 0.00028 H1N 0.54492 -0.03451 0.27537 1.00000 0.02677 0.03110 0.00144 0.00154 0.00227 0.00000 0.00426 Final Structure Factor Calculation for 2008lsh008 in P2(1)/c Total number of l.s. parameters = 106 Maximum vector length = 511 Memory required = 1508 / 22995 wR2 = 0.1176 before cycle 17 for 1807 data and 0 / 106 parameters Summary of restraints applied in cycle 17 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.033; Restrained GooF = 1.033 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0569 * P )^2 + 0.23 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0467 for 1416 Fo > 4sig(Fo) and 0.0658 for all 1807 data wR2 = 0.1176, GooF = S = 1.033, Restrained GooF = 1.033 for all data Occupancy sum of asymmetric unit = 11.00 for non-hydrogen and 11.00 for hydrogen atoms Principal mean square atomic displacements U 0.0217 0.0209 0.0146 C1 0.0258 0.0207 0.0182 C2 0.0273 0.0214 0.0176 C3 0.0264 0.0213 0.0167 C4 0.0273 0.0237 0.0168 C5 0.0253 0.0218 0.0166 C6 0.0249 0.0224 0.0159 C7 0.0300 0.0244 0.0217 C8 0.0328 0.0261 0.0228 C9 0.0240 0.0201 0.0169 N1 0.0349 0.0261 0.0187 O1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.017 0.031 0.046 0.063 0.084 0.106 0.132 0.178 0.251 1.000 Number in group 195. 177. 173. 179. 181. 186. 173. 183. 179. 181. GooF 1.011 0.967 1.042 1.097 1.085 1.017 1.138 0.998 0.902 1.054 K 2.236 1.074 1.029 0.970 0.978 1.002 0.984 1.010 1.015 1.006 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.66 inf Number in group 181. 183. 179. 183. 182. 178. 178. 183. 180. 180. GooF 1.006 1.076 1.003 0.990 1.001 1.103 0.978 0.871 1.035 1.227 K 0.992 1.059 1.020 1.024 1.002 1.010 1.036 1.031 1.036 0.976 R1 0.162 0.165 0.134 0.091 0.070 0.069 0.041 0.035 0.037 0.035 Recommended weighting scheme: WGHT 0.0487 0.2533 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) -6 11 1 18.39 45.14 4.86 0.107 0.79 -11 1 3 107.69 145.34 3.55 0.192 1.04 -11 2 2 11.87 4.32 3.36 0.033 1.04 -6 0 2 39.16 23.76 3.26 0.078 1.89 -12 4 2 6.51 15.28 3.24 0.062 0.90 -3 3 3 20.64 12.60 3.21 0.056 1.87 0 2 0 770.40 959.74 3.20 0.493 4.75 -9 8 1 0.98 7.21 3.14 0.043 0.87 -6 10 2 16.56 29.41 3.08 0.086 0.85 1 3 0 285.05 349.59 3.03 0.297 3.04 7 9 1 90.35 117.82 3.00 0.173 0.86 -3 2 7 3.35 0.28 2.98 0.008 1.03 9 9 0 8.19 0.07 2.94 0.004 0.80 0 1 1 246.49 335.22 2.86 0.291 5.69 -4 5 1 92.01 73.17 2.85 0.136 1.59 -5 7 5 36.38 49.40 2.82 0.112 0.97 -2 4 2 229.88 189.95 2.82 0.219 1.96 14 0 0 92.39 57.35 2.80 0.120 0.80 -11 0 2 34.48 49.55 2.80 0.112 1.06 -6 3 2 19.90 11.92 2.80 0.055 1.62 -11 3 6 20.63 31.71 2.76 0.090 0.88 -5 11 2 5.07 15.05 2.74 0.062 0.80 -4 3 2 22.91 15.83 2.73 0.063 2.00 11 2 0 38.60 52.16 2.73 0.115 1.00 2 0 2 601.78 723.97 2.72 0.428 2.68 1 4 2 37.19 28.29 2.64 0.085 1.89 -7 3 9 16.98 1.41 2.61 0.019 0.78 -4 7 6 32.51 47.07 2.60 0.109 0.91 -3 2 3 36.20 27.09 2.59 0.083 2.09 -4 11 1 9.74 20.38 2.57 0.072 0.83 -4 6 3 89.45 71.55 2.56 0.135 1.27 -7 2 9 46.80 68.47 2.56 0.132 0.79 -9 1 5 37.90 50.25 2.56 0.113 1.10 4 6 5 16.92 25.92 2.53 0.081 0.93 4 2 6 -1.51 1.58 2.51 0.020 0.97 -10 8 5 67.73 44.27 2.49 0.106 0.78 -11 1 1 62.78 80.17 2.48 0.142 1.04 -4 2 5 13.42 8.59 2.48 0.047 1.38 -1 1 5 47.89 37.58 2.47 0.098 1.45 -4 5 6 8.18 1.85 2.44 0.022 1.03 7 3 6 13.40 6.35 2.41 0.040 0.82 4 4 1 166.23 140.32 2.38 0.188 1.68 8 7 4 13.32 5.54 2.38 0.037 0.79 -13 5 3 66.85 46.08 2.37 0.108 0.81 -10 3 2 21.55 29.59 2.35 0.087 1.10 6 3 6 -1.52 2.88 2.33 0.027 0.86 -4 9 5 3.88 10.24 2.31 0.051 0.85 7 2 5 33.40 48.28 2.30 0.111 0.92 -4 4 4 53.88 43.11 2.28 0.104 1.40 5 6 2 2.56 0.05 2.27 0.003 1.15 Bond lengths and angles C1 - Distance Angles C6 1.3955 (0.0019) C2 1.3965 (0.0020) 118.94 (0.13) N1 1.4160 (0.0019) 116.75 (0.12) 124.28 (0.12) C1 - C6 C2 C2 - Distance Angles C3 1.3878 (0.0021) C1 1.3965 (0.0020) 119.62 (0.13) H2 0.9500 120.19 120.19 C2 - C3 C1 C3 - Distance Angles C2 1.3878 (0.0021) C4 1.3940 (0.0020) 122.19 (0.13) H3 0.9500 118.91 118.91 C3 - C2 C4 C4 - Distance Angles C3 1.3940 (0.0020) C5 1.3953 (0.0020) 117.25 (0.13) C9 1.5070 (0.0020) 121.97 (0.13) 120.77 (0.13) C4 - C3 C5 C5 - Distance Angles C6 1.3837 (0.0020) C4 1.3953 (0.0020) 121.52 (0.13) H5 0.9500 119.24 119.24 C5 - C6 C4 C6 - Distance Angles C5 1.3837 (0.0020) C1 1.3955 (0.0019) 120.46 (0.13) H6 0.9500 119.77 119.77 C6 - C5 C1 C7 - Distance Angles O1 1.2351 (0.0018) N1 1.3541 (0.0018) 123.12 (0.13) C8 1.5045 (0.0020) 121.46 (0.13) 115.43 (0.12) C7 - O1 N1 C8 - Distance Angles C7 1.5045 (0.0020) 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 C4 1.5070 (0.0020) H9A 0.9800 109.47 H9B 0.9800 109.47 109.47 H9C 0.9800 109.47 109.47 109.47 C9 - C4 H9A H9B N1 - Distance Angles C7 1.3541 (0.0018) C1 1.4160 (0.0019) 128.02 (0.12) H1N 0.8967 (0.0136) 116.25 (1.07) 115.63 (1.07) N1 - C7 C1 O1 - Distance Angles C7 1.2351 (0.0018) O1 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.897(14) 2.011(14) 2.9036(16) 173.6(16) N1-H1N...O1_$1 FMAP and GRID set by program FMAP 2 3 12 GRID -2.778 -2 -2 2.778 2 2 R1 = 0.0658 for 1807 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.21 at 0.8837 0.1603 0.2170 [ 0.71 A from C4 ] Deepest hole -0.26 at 0.4993 0.5333 0.2325 [ 0.80 A from N1 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 1732 / 15549 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.8837 0.1603 0.2170 1.00000 0.05 0.21 0.71 C4 0.94 C3 1.62 H3 1.76 C5 Q2 1 0.6817 0.1200 0.1490 1.00000 0.05 0.21 0.70 C1 0.74 C2 1.42 H2 1.84 N1 Q3 1 0.8972 0.0533 0.2503 1.00000 0.05 0.20 0.62 C4 0.78 C5 1.50 H5 1.76 C3 Q4 1 0.7332 0.0427 0.3079 1.00000 0.05 0.18 0.73 C6 0.85 C1 1.45 H6 1.80 C5 Q5 1 1.1072 0.0141 0.2788 1.00000 0.05 0.17 0.51 H9B 1.26 C9 1.57 H9C 1.98 H9A Shortest distances between peaks (including symmetry equivalents) 1 3 1.05 2 4 1.37 3 4 2.08 1 2 2.30 1 4 2.34 3 5 2.43 2 3 2.50 1 5 2.88 Time profile in seconds ----------------------- 0.11: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: 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. 0.50: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.78: Structure factors and derivatives 0.63: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.13: Solve l.s. equations 0.00: Generate HTAB table 0.09: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + shelxl finished at 18:45:51 Total CPU time: 2.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++