+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 16:12:58 on 15-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh170 in P2(1)/c CELL 0.71073 12.2837 9.4548 7.3046 90.000 99.932 90.000 ZERR 4.00 0.0004 0.0004 0.0003 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 36 44 4 4 V = 835.64 F(000) = 320.0 Mu = 0.08 mm-1 Cell Wt = 596.75 Rho = 1.186 MERG 2 OMIT -3.00 55.00 DFIX 0.88 0.02 N1 H1N FMAP 2 PLAN 5 ACTA SIZE 0.26 0.08 0.04 EQIV $1 -x+2, y-1/2, -z+1/2 HTAB N1 O1_$1 HTAB BOND $H L.S. 16 WGHT 0.046500 0.705700 FVAR 1.19989 C1 1 1.160003 0.566468 0.187601 11.00000 0.02866 0.02208 = 0.01993 -0.00483 0.00336 -0.00120 C2 1 1.239090 0.466309 0.260397 11.00000 0.03312 0.02277 = 0.02305 0.00081 0.00406 0.00092 AFIX 43 H2 2 1.219226 0.393318 0.333382 11.00000 -1.20000 AFIX 0 C3 1 1.346457 0.472944 0.226611 11.00000 0.03086 0.02821 = 0.02478 -0.00280 0.00281 0.00253 C4 1 1.374986 0.583663 0.117448 11.00000 0.02801 0.03191 = 0.02800 -0.00403 0.00513 -0.00225 AFIX 43 H4 2 1.446682 0.590185 0.093142 11.00000 -1.20000 AFIX 0 C5 1 1.296952 0.683806 0.045223 11.00000 0.03492 0.02647 = 0.02517 -0.00031 0.00633 -0.00439 AFIX 43 H5 2 1.317186 0.757311 -0.026589 11.00000 -1.20000 AFIX 0 C6 1 1.189024 0.676434 0.078109 11.00000 0.03117 0.02202 = 0.02278 0.00058 0.00227 0.00086 AFIX 43 H6 2 1.137031 0.743633 0.028006 11.00000 -1.20000 AFIX 0 C7 1 0.967483 0.639715 0.205720 11.00000 0.03011 0.02373 = 0.01753 -0.00444 0.00212 -0.00093 C8 1 0.862620 0.586372 0.261657 11.00000 0.03095 0.02843 = 0.02654 -0.00323 0.00424 0.00016 AFIX 137 H8A 2 0.843730 0.645223 0.358602 11.00000 -1.50000 H8B 2 0.873258 0.490891 0.305828 11.00000 -1.50000 H8C 2 0.803939 0.588954 0.156245 11.00000 -1.50000 AFIX 0 C9 1 1.430136 0.362641 0.305923 11.00000 0.03702 0.03835 = 0.04474 0.00632 0.00633 0.00958 AFIX 137 H9A 2 1.446949 0.372647 0.438584 11.00000 -1.50000 H9B 2 1.496368 0.374963 0.254551 11.00000 -1.50000 H9C 2 1.400357 0.270099 0.275121 11.00000 -1.50000 AFIX 0 N1 3 1.052277 0.546219 0.227016 11.00000 0.02961 0.02102 = 0.02324 0.00138 0.00452 -0.00055 O1 4 0.974499 0.760625 0.146716 11.00000 0.03644 0.02218 = 0.03013 0.00179 0.00682 0.00294 H1N 2 1.038897 0.460109 0.265931 11.00000 0.03462 HKLF 4 Covalent radii and connectivity table for 2008lsh170 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 C1 - C2 C6 N1 C2 - C3 C1 C3 - C2 C4 C9 C4 - C5 C3 C5 - C4 C6 C6 - C5 C1 C7 - O1 N1 C8 C8 - C7 C9 - C3 N1 - C7 C1 O1 - C7 Operators for generating equivalent atoms: $1 -x+2, y-1/2, -z+1/2 10092 Reflections read, of which 374 rejected -15 =< h =< 15, -12 =< k =< 11, -9 =< l =< 9, Max. 2-theta = 55.00 0 Systematic absence violations 0 Inconsistent equivalents 1912 Unique reflections, of which 0 suppressed R(int) = 0.0691 R(sigma) = 0.0445 Friedel opposites merged Maximum memory for data reduction = 1310 / 19032 Default effective X-H distances for T = 20.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 0.98 0.97 0.96 0.93 0.86 0.89 1.10 0.82 0.93 0.86 0.93 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 = 0.1460 before cycle 1 for 1912 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 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.079; Restrained GooF = 1.078 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0465 * P )^2 + 0.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.19989 0.00408 -0.001 OSF Mean shift/esd = 0.002 Maximum = -0.008 for tors H9A Max. shift = 0.000 A for H9C Max. dU = 0.000 for H1N Least-squares cycle 2 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1460 before cycle 2 for 1912 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 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.079; Restrained GooF = 1.078 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0465 * P )^2 + 0.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.19988 0.00408 0.000 OSF Mean shift/esd = 0.001 Maximum = -0.009 for tors H9A Max. shift = 0.000 A for H9B Max. dU = 0.000 for H1N Least-squares cycle 3 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1460 before cycle 3 for 1912 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 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.079; Restrained GooF = 1.078 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0465 * P )^2 + 0.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.19988 0.00408 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.006 for tors H9A Max. shift = 0.000 A for H9B Max. dU = 0.000 for H1N Least-squares cycle 4 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1460 before cycle 4 for 1912 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 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.079; Restrained GooF = 1.078 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0465 * P )^2 + 0.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.19988 0.00408 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.004 for tors H9A Max. shift = 0.000 A for H9B Max. dU = 0.000 for H1N Least-squares cycle 5 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1460 before cycle 5 for 1912 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 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.079; Restrained GooF = 1.078 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0465 * P )^2 + 0.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.19988 0.00408 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.003 for tors H9A Max. shift = 0.000 A for H9B Max. dU = 0.000 for H1N Least-squares cycle 6 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1460 before cycle 6 for 1912 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 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.079; Restrained GooF = 1.078 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0465 * P )^2 + 0.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.19988 0.00408 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.002 for tors H9A Max. shift = 0.000 A for H9B Max. dU = 0.000 for H1N Least-squares cycle 7 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1460 before cycle 7 for 1912 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 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.079; Restrained GooF = 1.078 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0465 * P )^2 + 0.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.19988 0.00408 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for tors H9A Max. shift = 0.000 A for H9C Max. dU = 0.000 for H1N Least-squares cycle 8 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1460 before cycle 8 for 1912 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 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.079; Restrained GooF = 1.078 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0465 * P )^2 + 0.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.19988 0.00408 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for tors H9A Max. shift = 0.000 A for H9C Max. dU = 0.000 for H1N Least-squares cycle 9 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1460 before cycle 9 for 1912 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 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.079; Restrained GooF = 1.078 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0465 * P )^2 + 0.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.19988 0.00408 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for tors H9A Max. shift = 0.000 A for H9A Max. dU = 0.000 for H1N Least-squares cycle 10 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1460 before cycle 10 for 1912 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 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.079; Restrained GooF = 1.079 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0465 * P )^2 + 0.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.19988 0.00408 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for tors H9A Max. shift = 0.000 A for H9A Max. dU = 0.000 for H1N Least-squares cycle 11 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1460 before cycle 11 for 1912 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 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.079; Restrained GooF = 1.079 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0465 * P )^2 + 0.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.19988 0.00408 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for tors H9A Max. shift = 0.000 A for H9C Max. dU = 0.000 for H1N Least-squares cycle 12 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1460 before cycle 12 for 1912 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 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.079; Restrained GooF = 1.078 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0465 * P )^2 + 0.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.19988 0.00408 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x N1 Max. shift = 0.000 A for H9B Max. dU = 0.000 for H1N Least-squares cycle 13 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1460 before cycle 13 for 1912 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 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.079; Restrained GooF = 1.078 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0465 * P )^2 + 0.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.19988 0.00408 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 Least-squares cycle 14 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1460 before cycle 14 for 1912 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 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.079; Restrained GooF = 1.078 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0465 * P )^2 + 0.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.19988 0.00408 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 Least-squares cycle 15 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1460 before cycle 15 for 1912 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 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.079; Restrained GooF = 1.078 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0465 * P )^2 + 0.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.19988 0.00408 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 16 Maximum vector length = 511 Memory required = 1614 / 137210 wR2 = 0.1460 before cycle 16 for 1912 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 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.079; Restrained GooF = 1.079 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0465 * P )^2 + 0.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.19988 0.00408 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 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 1.2192 0.3933 0.3334 43 0.930 0.000 C2 C3 C1 H4 1.4467 0.5902 0.0931 43 0.930 0.000 C4 C5 C3 H5 1.3172 0.7573 -0.0266 43 0.930 0.000 C5 C4 C6 H6 1.1370 0.7436 0.0280 43 0.930 0.000 C6 C5 C1 H8A 0.8437 0.6452 0.3586 137 0.960 0.000 C8 C7 H8A H8B 0.8733 0.4909 0.3058 137 0.960 0.000 C8 C7 H8A H8C 0.8039 0.5890 0.1562 137 0.960 0.000 C8 C7 H8A H9A 1.4470 0.3727 0.4386 137 0.960 0.000 C9 C3 H9A H9B 1.4963 0.3749 0.2545 137 0.960 0.000 C9 C3 H9A H9C 1.4003 0.2701 0.2752 137 0.960 0.000 C9 C3 H9A 2008lsh170 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 1.16000 0.56647 0.18760 1.00000 0.02866 0.02208 0.01993 -0.00483 0.00336 -0.00120 0.02365 0.00309 0.00014 0.00019 0.00023 0.00000 0.00090 0.00081 0.00081 0.00066 0.00068 0.00069 0.00039 C2 1.23909 0.46631 0.26040 1.00000 0.03312 0.02277 0.02305 0.00081 0.00406 0.00092 0.02640 0.00330 0.00015 0.00019 0.00024 0.00000 0.00096 0.00085 0.00088 0.00067 0.00072 0.00071 0.00041 H2 1.21923 0.39332 0.33338 1.00000 0.03169 0.00000 0.00000 C3 1.34646 0.47294 0.22661 1.00000 0.03086 0.02821 0.02478 -0.00280 0.00281 0.00253 0.02819 0.00340 0.00016 0.00020 0.00026 0.00000 0.00096 0.00094 0.00089 0.00072 0.00073 0.00074 0.00042 C4 1.37499 0.58366 0.11745 1.00000 0.02801 0.03191 0.02800 -0.00403 0.00513 -0.00225 0.02927 0.00339 0.00016 0.00020 0.00026 0.00000 0.00091 0.00099 0.00095 0.00077 0.00074 0.00077 0.00042 H4 1.44668 0.59018 0.09314 1.00000 0.03513 0.00000 0.00000 C5 1.29695 0.68381 0.04522 1.00000 0.03492 0.02647 0.02517 -0.00031 0.00633 -0.00439 0.02872 0.00341 0.00016 0.00020 0.00026 0.00000 0.00101 0.00091 0.00092 0.00072 0.00076 0.00076 0.00043 H5 1.31719 0.75731 -0.02659 1.00000 0.03446 0.00000 0.00000 C6 1.18902 0.67643 0.07811 1.00000 0.03117 0.02202 0.02278 0.00058 0.00227 0.00086 0.02561 0.00327 0.00015 0.00019 0.00025 0.00000 0.00093 0.00083 0.00087 0.00066 0.00070 0.00071 0.00040 H6 1.13703 0.74363 0.02801 1.00000 0.03073 0.00000 0.00000 C7 0.96748 0.63971 0.20572 1.00000 0.03011 0.02373 0.01753 -0.00444 0.00212 -0.00093 0.02402 0.00313 0.00015 0.00019 0.00024 0.00000 0.00094 0.00083 0.00077 0.00065 0.00066 0.00071 0.00039 C8 0.86262 0.58637 0.26166 1.00000 0.03095 0.02843 0.02654 -0.00323 0.00424 0.00016 0.02873 0.00342 0.00015 0.00020 0.00026 0.00000 0.00096 0.00093 0.00092 0.00074 0.00074 0.00076 0.00042 H8A 0.84373 0.64522 0.35860 1.00000 0.04309 0.00000 0.00000 H8B 0.87326 0.49089 0.30583 1.00000 0.04309 0.00000 0.00000 H8C 0.80394 0.58895 0.15625 1.00000 0.04309 0.00000 0.00000 C9 1.43014 0.36264 0.30592 1.00000 0.03702 0.03835 0.04474 0.00633 0.00633 0.00958 0.04012 0.00440 0.00018 0.00024 0.00032 0.00000 0.00113 0.00116 0.00123 0.00095 0.00094 0.00092 0.00052 H9A 1.44699 0.37269 0.43858 1.00000 0.06018 0.00000 0.00000 H9B 1.49635 0.37492 0.25449 1.00000 0.06018 0.00000 0.00000 H9C 1.40034 0.27010 0.27519 1.00000 0.06018 0.00000 0.00000 N1 1.05228 0.54622 0.22702 1.00000 0.02961 0.02102 0.02324 0.00138 0.00452 -0.00055 0.02463 0.00277 0.00013 0.00016 0.00021 0.00000 0.00080 0.00075 0.00074 0.00058 0.00060 0.00059 0.00036 O1 0.97450 0.76063 0.14672 1.00000 0.03644 0.02218 0.03013 0.00179 0.00682 0.00294 0.02946 0.00243 0.00011 0.00013 0.00018 0.00000 0.00074 0.00065 0.00070 0.00052 0.00055 0.00053 0.00034 H1N 1.03890 0.46011 0.26593 1.00000 0.03463 0.03939 0.00177 0.00182 0.00305 0.00000 0.00597 Final Structure Factor Calculation for 2008lsh170 in P2(1)/c Total number of l.s. parameters = 106 Maximum vector length = 511 Memory required = 1508 / 22995 wR2 = 0.1460 before cycle 17 for 1912 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 0.007 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.079; Restrained GooF = 1.078 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0465 * P )^2 + 0.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0589 for 1540 Fo > 4sig(Fo) and 0.0761 for all 1912 data wR2 = 0.1460, GooF = S = 1.079, Restrained GooF = 1.078 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 0.0290 0.0259 0.0160 C1 0.0335 0.0237 0.0221 C2 0.0342 0.0272 0.0232 C3 0.0348 0.0277 0.0253 C4 0.0368 0.0252 0.0241 C5 0.0324 0.0230 0.0215 C6 0.0309 0.0260 0.0152 C7 0.0318 0.0302 0.0241 C8 0.0499 0.0430 0.0275 C9 0.0297 0.0239 0.0203 N1 0.0371 0.0298 0.0214 O1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.021 0.033 0.046 0.062 0.078 0.098 0.130 0.188 1.000 Number in group 205. 185. 205. 172. 195. 196. 180. 196. 186. 192. GooF 1.259 1.127 1.097 1.135 1.028 1.047 0.953 0.983 1.021 1.092 K 4.409 1.166 1.024 1.027 1.003 0.979 0.986 0.993 1.015 1.019 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.32 1.65 inf Number in group 196. 187. 195. 193. 185. 191. 194. 191. 191. 189. GooF 1.214 1.209 1.078 1.166 0.984 0.885 0.975 0.831 1.116 1.239 K 1.061 1.093 1.033 1.037 1.015 1.000 1.002 1.002 1.018 1.014 R1 0.189 0.172 0.138 0.121 0.079 0.061 0.054 0.041 0.054 0.039 Recommended weighting scheme: WGHT 0.0456 0.7087 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) 7 11 0 8.56 0.52 3.53 0.009 0.77 7 3 7 8.34 0.07 3.19 0.003 0.80 6 8 5 6.17 0.00 3.18 0.000 0.80 7 6 6 12.09 27.48 3.06 0.068 0.79 3 6 3 4.39 0.07 3.05 0.003 1.22 -5 2 2 150.36 196.36 3.02 0.181 1.99 9 6 3 7.30 1.20 2.94 0.014 0.90 -11 1 3 160.70 207.81 2.93 0.186 1.07 -1 3 3 766.87 634.06 2.90 0.326 1.93 7 2 7 7.40 0.58 2.86 0.010 0.81 0 2 8 32.64 53.56 2.78 0.095 0.88 -13 0 4 5.47 0.06 2.75 0.003 0.89 -7 5 8 29.06 13.93 2.74 0.048 0.78 -2 4 5 33.13 51.05 2.73 0.092 1.24 -12 7 1 6.86 0.56 2.68 0.010 0.82 -1 8 5 6.73 0.24 2.67 0.006 0.92 0 3 4 172.33 136.52 2.59 0.151 1.56 -14 5 2 -0.88 4.87 2.59 0.029 0.79 -1 0 4 326.19 265.61 2.58 0.211 1.83 2 7 7 27.81 45.49 2.58 0.087 0.80 4 9 5 6.56 16.83 2.57 0.053 0.80 -5 7 6 0.73 8.31 2.57 0.037 0.88 -6 3 6 -0.55 5.98 2.56 0.032 1.05 7 6 5 15.94 30.26 2.56 0.071 0.86 -7 6 3 4.87 13.94 2.55 0.048 1.10 8 9 2 17.99 8.95 2.50 0.039 0.82 -9 10 1 45.30 23.99 2.48 0.063 0.78 -2 3 2 0.74 5.27 2.47 0.030 2.30 0 10 3 5.39 1.05 2.46 0.013 0.88 -10 5 5 18.98 8.63 2.44 0.038 0.90 -6 7 2 5.35 0.00 2.40 0.001 1.10 -12 8 1 24.12 13.15 2.40 0.047 0.77 -10 7 4 159.00 121.93 2.40 0.143 0.85 5 5 7 1.09 7.44 2.39 0.035 0.81 -3 2 4 2.28 0.00 2.35 0.001 1.65 3 9 1 5.34 1.02 2.34 0.013 1.00 13 5 1 1.03 7.26 2.34 0.035 0.82 -7 0 2 3.57 9.81 2.34 0.040 1.67 10 4 5 4.66 14.54 2.33 0.049 0.81 -4 4 3 20.18 31.70 2.31 0.073 1.55 -12 1 5 -0.14 5.06 2.30 0.029 0.90 -2 9 5 14.21 25.03 2.28 0.065 0.85 -1 1 4 64.15 47.47 2.28 0.089 1.79 1 2 0 74.32 56.10 2.27 0.097 4.40 -11 1 7 12.74 0.56 2.27 0.010 0.82 1 3 0 195.94 236.79 2.27 0.199 3.05 -13 7 2 19.51 10.00 2.27 0.041 0.77 -9 0 2 44.64 61.23 2.23 0.101 1.34 -4 7 7 0.74 6.26 2.23 0.032 0.82 -12 2 4 5.43 0.72 2.23 0.011 0.93 Bond lengths and angles C1 - Distance Angles C2 1.3947 (0.0025) C6 1.3950 (0.0025) 119.64 (0.17) N1 1.4149 (0.0024) 116.42 (0.16) 123.91 (0.16) C1 - C2 C6 C2 - Distance Angles C3 1.3844 (0.0027) C1 1.3947 (0.0025) 121.58 (0.17) H2 0.9300 119.21 119.21 C2 - C3 C1 C3 - Distance Angles C2 1.3844 (0.0027) C4 1.3967 (0.0027) 118.44 (0.17) C9 1.5081 (0.0027) 120.49 (0.18) 121.07 (0.18) C3 - C2 C4 C4 - Distance Angles C5 1.3853 (0.0027) C3 1.3967 (0.0027) 120.29 (0.18) H4 0.9300 119.85 119.85 C4 - C5 C3 C5 - Distance Angles C4 1.3853 (0.0027) C6 1.3893 (0.0027) 121.20 (0.17) H5 0.9300 119.40 119.40 C5 - C4 C6 C6 - Distance Angles C5 1.3893 (0.0027) C1 1.3950 (0.0025) 118.84 (0.17) H6 0.9300 120.58 120.58 C6 - C5 C1 C7 - Distance Angles O1 1.2300 (0.0022) N1 1.3545 (0.0023) 123.22 (0.17) C8 1.5040 (0.0026) 121.46 (0.16) 115.32 (0.16) C7 - O1 N1 C8 - Distance Angles C7 1.5040 (0.0026) H8A 0.9600 109.47 H8B 0.9600 109.47 109.47 H8C 0.9600 109.47 109.47 109.47 C8 - C7 H8A H8B C9 - Distance Angles C3 1.5081 (0.0027) H9A 0.9600 109.47 H9B 0.9600 109.47 109.47 H9C 0.9600 109.47 109.47 109.47 C9 - C3 H9A H9B N1 - Distance Angles C7 1.3545 (0.0023) C1 1.4149 (0.0024) 128.02 (0.15) H1N 0.8870 (0.0156) 117.03 (1.43) 114.89 (1.43) N1 - C7 C1 O1 - Distance Angles C7 1.2300 (0.0022) O1 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.887(16) 2.007(16) 2.8905(19) 174(2) 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)