+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 15:01:19 on 22-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh023 in P2(1)/c CELL 0.71073 13.8770 9.5769 7.4415 90.000 103.022 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 40 44 4 12 V = 963.53 F(000) = 408.0 Mu = 0.10 mm-1 Cell Wt = 772.79 Rho = 1.332 MERG 2 OMIT -3.00 55.00 OMIT 11 8 3 DFIX 0.88 0.02 N1 H1N EQIV $1 -x, y-1/2, -z+1/2 HTAB N1 O1_$1 FMAP 2 PLAN 5 ACTA SIZE 0.02 0.24 0.40 BOND $H L.S. 16 TEMP -153.00 WGHT 0.024000 0.966300 FVAR 0.90553 C1 1 0.150175 0.402598 0.202334 11.00000 0.02687 0.02501 = 0.02474 0.00365 0.00570 -0.00002 C2 1 0.206629 0.516614 0.279776 11.00000 0.03079 0.02561 = 0.03278 -0.00318 0.00853 -0.00125 AFIX 43 H2 2 0.178511 0.587069 0.341894 11.00000 -1.20000 AFIX 0 C3 1 0.304706 0.526569 0.265448 11.00000 0.02935 0.03014 = 0.03309 -0.00010 0.00616 -0.00484 AFIX 43 H3 2 0.343657 0.604458 0.317051 11.00000 -1.20000 AFIX 0 C4 1 0.345188 0.423771 0.176692 11.00000 0.02668 0.03634 = 0.02491 0.00667 0.00745 0.00144 C5 1 0.290140 0.310437 0.098309 11.00000 0.03238 0.02983 = 0.02791 0.00048 0.00920 0.00405 AFIX 43 H5 2 0.318809 0.240370 0.036508 11.00000 -1.20000 AFIX 0 C6 1 0.192268 0.300428 0.111178 11.00000 0.03228 0.02498 = 0.02913 -0.00142 0.00717 -0.00096 AFIX 43 H6 2 0.153521 0.223029 0.057218 11.00000 -1.20000 AFIX 0 C7 1 -0.013585 0.476394 0.256083 11.00000 0.02737 0.02616 = 0.02962 0.00494 0.00402 0.00180 C8 1 -0.116108 0.421012 0.246991 11.00000 0.02635 0.03094 = 0.03817 0.00152 0.00727 0.00099 AFIX 137 H8A 2 -0.147807 0.476242 0.328403 11.00000 -1.50000 H8B 2 -0.112027 0.323191 0.286646 11.00000 -1.50000 H8C 2 -0.155225 0.427553 0.120004 11.00000 -1.50000 AFIX 0 C9 1 0.515692 0.383804 0.288419 11.00000 0.03007 0.03159 = 0.03640 0.00196 0.00493 -0.00324 C10 1 0.613946 0.412456 0.246344 11.00000 0.02909 0.04489 = 0.04149 -0.00202 0.00674 -0.00316 AFIX 137 H10A 2 0.626550 0.513225 0.252493 11.00000 -1.50000 H10B 2 0.614138 0.378404 0.122237 11.00000 -1.50000 H10C 2 0.665705 0.364565 0.336658 11.00000 -1.50000 AFIX 0 N1 3 0.050499 0.382204 0.212327 11.00000 0.02582 0.02153 = 0.03241 -0.00002 0.00718 -0.00255 O1 4 0.009599 0.597599 0.299768 11.00000 0.03221 0.02308 = 0.05130 -0.00154 0.00974 0.00263 O2 4 0.442712 0.440064 0.156498 11.00000 0.02488 0.04452 = 0.03418 0.00683 0.00868 0.00086 O3 4 0.500107 0.322930 0.419067 11.00000 0.03415 0.07016 = 0.04965 0.02566 0.00464 -0.00417 H1N 2 0.029528 0.296111 0.198682 11.00000 0.03274 HKLF 4 Covalent radii and connectivity table for 2008lsh023 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 C1 - C2 C6 N1 C2 - C1 C3 C3 - C4 C2 C4 - C3 C5 O2 C5 - C4 C6 C6 - C5 C1 C7 - O1 N1 C8 C8 - C7 C9 - O3 O2 C10 C10 - C9 N1 - C7 C1 O1 - C7 O2 - C9 C4 O3 - C9 Operators for generating equivalent atoms: $1 -x, y-1/2, -z+1/2 11374 Reflections read, of which 425 rejected -17 =< h =< 18, -12 =< k =< 12, -9 =< l =< 9, Max. 2-theta = 54.96 0 Systematic absence violations 0 Inconsistent equivalents 2187 Unique reflections, of which 0 suppressed R(int) = 0.0515 R(sigma) = 0.0421 Friedel opposites merged Maximum memory for data reduction = 1450 / 21870 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 = 1814 / 168098 wR2 = 0.1311 before cycle 1 for 2187 data and 133 / 133 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 = 1.123; Restrained GooF = 1.122 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0240 * P )^2 + 0.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.90553 0.00240 0.001 OSF Mean shift/esd = 0.002 Maximum = 0.006 for U13 O2 Max. shift = 0.000 A for H8A Max. dU = 0.000 for C4 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1814 / 168098 wR2 = 0.1311 before cycle 2 for 2187 data and 133 / 133 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 = 1.123; Restrained GooF = 1.122 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0240 * P )^2 + 0.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.90553 0.00240 -0.001 OSF Mean shift/esd = 0.001 Maximum = 0.002 for U13 O2 Max. shift = 0.000 A for H8A Max. dU = 0.000 for C4 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1814 / 168098 wR2 = 0.1311 before cycle 3 for 2187 data and 133 / 133 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 = 1.123; Restrained GooF = 1.122 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0240 * P )^2 + 0.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.90553 0.00240 0.000 OSF 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 4 Maximum vector length = 511 Memory required = 1814 / 168098 wR2 = 0.1311 before cycle 4 for 2187 data and 133 / 133 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 = 1.123; Restrained GooF = 1.122 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0240 * P )^2 + 0.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.90553 0.00240 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for tors H8A Max. shift = 0.000 A for H8B Max. dU = 0.000 for C5 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1814 / 168098 wR2 = 0.1311 before cycle 5 for 2187 data and 133 / 133 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 = 1.123; Restrained GooF = 1.122 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0240 * P )^2 + 0.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.90553 0.00240 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 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 = 1814 / 168098 wR2 = 0.1311 before cycle 6 for 2187 data and 133 / 133 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 = 1.123; Restrained GooF = 1.122 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0240 * P )^2 + 0.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.90553 0.00240 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for tors H8A Max. shift = 0.000 A for H8B Max. dU = 0.000 for H1N Least-squares cycle 7 Maximum vector length = 511 Memory required = 1814 / 168098 wR2 = 0.1311 before cycle 7 for 2187 data and 133 / 133 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 = 1.123; Restrained GooF = 1.122 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0240 * P )^2 + 0.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.90553 0.00240 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for tors H8A Max. shift = 0.000 A for H8B Max. dU = 0.000 for H1N Least-squares cycle 8 Maximum vector length = 511 Memory required = 1814 / 168098 wR2 = 0.1311 before cycle 8 for 2187 data and 133 / 133 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 = 1.123; Restrained GooF = 1.122 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0240 * P )^2 + 0.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.90553 0.00240 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for tors H8A Max. shift = 0.000 A for H8C Max. dU = 0.000 for O1 Least-squares cycle 9 Maximum vector length = 511 Memory required = 1814 / 168098 wR2 = 0.1311 before cycle 9 for 2187 data and 133 / 133 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 = 1.123; Restrained GooF = 1.122 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0240 * P )^2 + 0.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.90553 0.00240 0.000 OSF 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 10 Maximum vector length = 511 Memory required = 1814 / 168098 wR2 = 0.1311 before cycle 10 for 2187 data and 133 / 133 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 = 1.123; Restrained GooF = 1.122 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0240 * P )^2 + 0.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.90553 0.00240 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for tors H8A Max. shift = 0.000 A for H8B Max. dU = 0.000 for O1 Least-squares cycle 11 Maximum vector length = 511 Memory required = 1814 / 168098 wR2 = 0.1311 before cycle 11 for 2187 data and 133 / 133 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 = 1.123; Restrained GooF = 1.122 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0240 * P )^2 + 0.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.90553 0.00240 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y O1 Max. shift = 0.000 A for H8B Max. dU = 0.000 for C6 Least-squares cycle 12 Maximum vector length = 511 Memory required = 1814 / 168098 wR2 = 0.1311 before cycle 12 for 2187 data and 133 / 133 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 = 1.123; Restrained GooF = 1.122 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0240 * P )^2 + 0.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.90553 0.00240 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y O1 Max. shift = 0.000 A for H8A Max. dU = 0.000 for H1N Least-squares cycle 13 Maximum vector length = 511 Memory required = 1814 / 168098 wR2 = 0.1311 before cycle 13 for 2187 data and 133 / 133 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 = 1.123; Restrained GooF = 1.122 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0240 * P )^2 + 0.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.90553 0.00240 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y O1 Max. shift = 0.000 A for H8A Max. dU = 0.000 for O1 Least-squares cycle 14 Maximum vector length = 511 Memory required = 1814 / 168098 wR2 = 0.1311 before cycle 14 for 2187 data and 133 / 133 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 = 1.123; Restrained GooF = 1.122 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0240 * P )^2 + 0.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.90553 0.00240 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x C10 Max. shift = 0.000 A for H8C Max. dU = 0.000 for H1N Least-squares cycle 15 Maximum vector length = 511 Memory required = 1814 / 168098 wR2 = 0.1311 before cycle 15 for 2187 data and 133 / 133 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 = 1.123; Restrained GooF = 1.122 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0240 * P )^2 + 0.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.90553 0.00240 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y O1 Max. shift = 0.000 A for H8A Max. dU = 0.000 for H1N Least-squares cycle 16 Maximum vector length = 511 Memory required = 1814 / 168098 wR2 = 0.1311 before cycle 16 for 2187 data and 133 / 133 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 = 1.123; Restrained GooF = 1.122 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0240 * P )^2 + 0.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.90553 0.00240 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x C10 Max. shift = 0.000 A for H8A 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 0.1785 0.5871 0.3419 43 0.950 0.000 C2 C1 C3 H3 0.3437 0.6045 0.3171 43 0.950 0.000 C3 C4 C2 H5 0.3188 0.2404 0.0365 43 0.950 0.000 C5 C4 C6 H6 0.1535 0.2230 0.0572 43 0.950 0.000 C6 C5 C1 H8A -0.1478 0.4762 0.3284 137 0.980 0.000 C8 C7 H8A H8B -0.1120 0.3232 0.2867 137 0.980 0.000 C8 C7 H8A H8C -0.1552 0.4275 0.1200 137 0.980 0.000 C8 C7 H8A H10A 0.6265 0.5132 0.2525 137 0.980 0.000 C10 C9 H10A H10B 0.6141 0.3784 0.1222 137 0.980 0.000 C10 C9 H10A H10C 0.6657 0.3646 0.3367 137 0.980 0.000 C10 C9 H10A 2008lsh023 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.15018 0.40260 0.20233 1.00000 0.02687 0.02501 0.02474 0.00365 0.00570 -0.00002 0.02556 0.00384 0.00015 0.00021 0.00027 0.00000 0.00100 0.00104 0.00104 0.00079 0.00080 0.00084 0.00044 C2 0.20663 0.51661 0.27978 1.00000 0.03079 0.02561 0.03278 -0.00318 0.00853 -0.00125 0.02951 0.00397 0.00016 0.00023 0.00029 0.00000 0.00107 0.00108 0.00114 0.00087 0.00088 0.00088 0.00047 H2 0.17851 0.58707 0.34189 1.00000 0.03541 0.00000 0.00000 C3 0.30471 0.52657 0.26545 1.00000 0.02935 0.03014 0.03309 -0.00010 0.00616 -0.00484 0.03100 0.00409 0.00016 0.00023 0.00030 0.00000 0.00107 0.00115 0.00116 0.00092 0.00088 0.00092 0.00048 H3 0.34366 0.60446 0.31705 1.00000 0.03720 0.00000 0.00000 C4 0.34519 0.42377 0.17669 1.00000 0.02668 0.03634 0.02491 0.00667 0.00745 0.00144 0.02905 0.00414 0.00015 0.00024 0.00028 0.00000 0.00103 0.00121 0.00108 0.00088 0.00082 0.00090 0.00048 C5 0.29014 0.31044 0.09831 1.00000 0.03238 0.02983 0.02791 0.00048 0.00920 0.00405 0.02966 0.00415 0.00016 0.00023 0.00029 0.00000 0.00110 0.00113 0.00110 0.00085 0.00087 0.00090 0.00048 H5 0.31881 0.24037 0.03651 1.00000 0.03559 0.00000 0.00000 C6 0.19227 0.30043 0.11118 1.00000 0.03228 0.02498 0.02913 -0.00142 0.00717 -0.00096 0.02876 0.00406 0.00016 0.00022 0.00029 0.00000 0.00109 0.00108 0.00114 0.00083 0.00087 0.00088 0.00047 H6 0.15352 0.22303 0.05722 1.00000 0.03451 0.00000 0.00000 C7 -0.01359 0.47639 0.25608 1.00000 0.02737 0.02616 0.02962 0.00494 0.00402 0.00180 0.02810 0.00404 0.00015 0.00022 0.00029 0.00000 0.00105 0.00110 0.00109 0.00086 0.00084 0.00086 0.00046 C8 -0.11611 0.42101 0.24699 1.00000 0.02634 0.03094 0.03817 0.00152 0.00727 0.00099 0.03182 0.00416 0.00015 0.00024 0.00032 0.00000 0.00107 0.00114 0.00125 0.00094 0.00090 0.00089 0.00050 H8A -0.14781 0.47625 0.32840 1.00000 0.04773 0.00000 0.00000 H8B -0.11203 0.32319 0.28666 1.00000 0.04773 0.00000 0.00000 H8C -0.15522 0.42755 0.12000 1.00000 0.04773 0.00000 0.00000 C9 0.51569 0.38380 0.28842 1.00000 0.03007 0.03159 0.03640 0.00196 0.00493 -0.00324 0.03309 0.00411 0.00016 0.00024 0.00031 0.00000 0.00112 0.00118 0.00128 0.00095 0.00093 0.00095 0.00051 C10 0.61395 0.41246 0.24634 1.00000 0.02909 0.04489 0.04149 -0.00202 0.00674 -0.00316 0.03868 0.00450 0.00016 0.00027 0.00034 0.00000 0.00115 0.00139 0.00136 0.00108 0.00097 0.00103 0.00056 H10A 0.62655 0.51322 0.25249 1.00000 0.05802 0.00000 0.00000 H10B 0.61414 0.37840 0.12224 1.00000 0.05802 0.00000 0.00000 H10C 0.66570 0.36457 0.33666 1.00000 0.05802 0.00000 0.00000 N1 0.05050 0.38220 0.21233 1.00000 0.02582 0.02153 0.03241 -0.00002 0.00718 -0.00255 0.02649 0.00332 0.00013 0.00018 0.00025 0.00000 0.00086 0.00091 0.00095 0.00072 0.00071 0.00073 0.00039 O1 0.00960 0.59760 0.29977 1.00000 0.03221 0.02308 0.05130 -0.00154 0.00974 0.00263 0.03547 0.00293 0.00011 0.00016 0.00023 0.00000 0.00082 0.00082 0.00105 0.00069 0.00072 0.00065 0.00040 O2 0.44271 0.44006 0.15650 1.00000 0.02488 0.04452 0.03418 0.00683 0.00868 0.00086 0.03420 0.00295 0.00010 0.00017 0.00021 0.00000 0.00076 0.00097 0.00087 0.00070 0.00062 0.00069 0.00039 O3 0.50011 0.32293 0.41907 1.00000 0.03415 0.07016 0.04965 0.02566 0.00464 -0.00417 0.05208 0.00370 0.00012 0.00022 0.00026 0.00000 0.00091 0.00134 0.00110 0.00098 0.00079 0.00089 0.00053 H1N 0.02953 0.29611 0.19868 1.00000 0.03274 0.03805 0.00166 0.00183 0.00326 0.00000 0.00647 Final Structure Factor Calculation for 2008lsh023 in P2(1)/c Total number of l.s. parameters = 133 Maximum vector length = 511 Memory required = 1681 / 22995 wR2 = 0.1311 before cycle 17 for 2187 data and 0 / 133 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 = 1.123; Restrained GooF = 1.122 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0240 * P )^2 + 0.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0594 for 1664 Fo > 4sig(Fo) and 0.0869 for all 2187 data wR2 = 0.1311, GooF = S = 1.123, Restrained GooF = 1.122 for all data Occupancy sum of asymmetric unit = 14.00 for non-hydrogen and 11.00 for hydrogen atoms Principal mean square atomic displacements U 0.0287 0.0268 0.0211 C1 0.0344 0.0297 0.0244 C2 0.0353 0.0329 0.0249 C3 0.0394 0.0265 0.0212 C4 0.0356 0.0282 0.0252 C5 0.0324 0.0294 0.0245 C6 0.0338 0.0286 0.0219 C7 0.0386 0.0308 0.0260 C8 0.0397 0.0321 0.0275 C9 0.0460 0.0416 0.0285 C10 0.0324 0.0268 0.0202 N1 0.0516 0.0327 0.0221 O1 0.0479 0.0310 0.0237 O2 0.0903 0.0337 0.0323 O3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.015 0.024 0.033 0.042 0.054 0.072 0.096 0.144 1.000 Number in group 236. 204. 229. 225. 215. 208. 219. 213. 220. 218. GooF 1.218 1.172 1.184 1.146 1.155 1.211 0.949 1.043 0.950 1.153 K 5.738 1.339 1.130 1.011 1.010 0.978 0.992 0.994 1.003 1.003 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.31 1.66 inf Number in group 219. 224. 222. 214. 219. 216. 216. 218. 219. 220. GooF 1.272 1.202 1.072 1.126 0.998 0.959 1.043 0.945 1.060 1.446 K 1.147 1.067 1.049 1.006 0.994 0.999 0.999 0.995 1.015 0.998 R1 0.246 0.221 0.178 0.140 0.099 0.075 0.057 0.052 0.048 0.035 Recommended weighting scheme: WGHT 0.0240 0.9659 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 4 0 38.91 12.80 4.89 0.031 2.36 2 4 1 134.96 88.99 3.89 0.082 2.11 -7 9 5 1.70 26.20 3.82 0.044 0.83 -7 6 4 13.71 37.27 3.70 0.053 1.09 4 4 0 42.34 20.31 3.67 0.039 1.95 11 6 4 5.28 29.68 3.49 0.047 0.80 -10 9 5 81.54 22.12 3.32 0.041 0.77 3 4 1 182.31 134.41 3.32 0.101 1.97 -6 4 5 11.87 0.24 3.26 0.004 1.19 -2 0 4 347.87 277.81 3.08 0.144 1.86 4 1 3 979.71 842.19 3.06 0.252 1.75 7 3 0 194.13 148.34 3.03 0.106 1.65 -2 2 1 922.71 1068.82 3.02 0.283 3.64 11 1 6 2.14 18.68 2.97 0.037 0.78 -15 3 2 8.98 0.05 2.82 0.002 0.89 -16 1 6 -2.41 8.93 2.75 0.026 0.78 -3 2 8 9.85 0.08 2.73 0.002 0.91 -6 10 1 13.71 0.92 2.71 0.008 0.88 -3 2 4 23.96 11.63 2.71 0.030 1.71 -7 0 2 167.23 124.34 2.69 0.097 1.89 -3 1 5 871.02 759.84 2.68 0.239 1.46 2 9 6 10.52 27.50 2.65 0.045 0.78 1 6 8 30.99 11.09 2.64 0.029 0.78 9 3 6 14.09 0.00 2.59 0.000 0.82 -1 0 8 -6.69 7.16 2.57 0.023 0.92 0 2 4 1587.83 1420.54 2.56 0.327 1.70 -12 0 8 16.48 3.18 2.55 0.015 0.80 -12 2 8 -3.82 4.67 2.53 0.019 0.79 2 3 3 521.81 448.60 2.53 0.184 1.77 -15 6 4 23.98 7.04 2.51 0.023 0.78 -9 6 7 11.38 0.86 2.51 0.008 0.82 3 0 2 2247.31 2519.69 2.50 0.435 2.56 15 3 2 14.21 3.15 2.50 0.015 0.81 0 7 2 -0.20 8.34 2.50 0.025 1.28 9 1 7 31.57 4.23 2.50 0.018 0.77 -10 7 3 6.07 20.43 2.48 0.039 0.95 2 9 0 -0.38 8.01 2.48 0.025 1.05 -4 3 8 18.25 4.86 2.48 0.019 0.89 15 5 1 40.92 72.12 2.44 0.074 0.79 -6 9 5 66.96 40.71 2.42 0.055 0.84 1 4 2 269.73 224.48 2.41 0.130 1.94 -3 3 3 742.20 653.50 2.40 0.222 1.90 -3 5 1 126.63 96.90 2.40 0.085 1.75 1 4 1 236.03 283.38 2.39 0.146 2.22 5 1 3 10.19 21.82 2.39 0.040 1.61 -1 2 4 31.88 17.82 2.39 0.037 1.73 2 6 2 150.86 117.19 2.39 0.094 1.40 -15 3 6 64.11 37.42 2.39 0.053 0.79 0 5 8 15.87 1.71 2.39 0.011 0.82 5 4 1 9.12 20.17 2.38 0.039 1.68 Bond lengths and angles C1 - Distance Angles C2 1.3909 (0.0029) C6 1.3919 (0.0029) 119.65 (0.19) N1 1.4154 (0.0026) 123.53 (0.19) 116.81 (0.19) C1 - C2 C6 C2 - Distance Angles C1 1.3909 (0.0029) C3 1.3922 (0.0030) 119.41 (0.20) H2 0.9500 120.29 120.29 C2 - C1 C3 C3 - Distance Angles C4 1.3741 (0.0031) C2 1.3922 (0.0030) 120.02 (0.20) H3 0.9500 119.99 119.99 C3 - C4 C2 C4 - Distance Angles C3 1.3741 (0.0031) C5 1.3788 (0.0031) 121.32 (0.19) O2 1.4036 (0.0025) 118.70 (0.20) 119.86 (0.19) C4 - C3 C5 C5 - Distance Angles C4 1.3788 (0.0031) C6 1.3862 (0.0029) 118.90 (0.20) H5 0.9500 120.55 120.55 C5 - C4 C6 C6 - Distance Angles C5 1.3862 (0.0029) C1 1.3919 (0.0029) 120.69 (0.20) H6 0.9500 119.66 119.66 C6 - C5 C1 C7 - Distance Angles O1 1.2286 (0.0026) N1 1.3569 (0.0027) 123.02 (0.20) C8 1.5055 (0.0029) 122.22 (0.19) 114.76 (0.19) C7 - O1 N1 C8 - Distance Angles C7 1.5055 (0.0029) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - C7 H8A H8B C9 - Distance Angles O3 1.1944 (0.0027) O2 1.3534 (0.0026) 122.79 (0.20) C10 1.4916 (0.0030) 127.04 (0.21) 110.15 (0.19) C9 - O3 O2 C10 - Distance Angles C9 1.4916 (0.0030) H10A 0.9800 109.47 H10B 0.9800 109.47 109.47 H10C 0.9800 109.47 109.47 109.47 C10 - C9 H10A H10B N1 - Distance Angles C7 1.3569 (0.0027) C1 1.4154 (0.0026) 128.46 (0.18) H1N 0.8726 (0.0162) 115.89 (1.55) 115.37 (1.55) N1 - C7 C1 O1 - Distance Angles C7 1.2286 (0.0026) O1 - O2 - Distance Angles C9 1.3534 (0.0026) C4 1.4036 (0.0025) 117.39 (0.17) O2 - C9 O3 - Distance Angles C9 1.1944 (0.0027) O3 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.873(16) 1.978(17) 2.846(2) 173(2) N1-H1N...O1_$1 FMAP and GRID set by program FMAP 2 3 12 GRID -2.778 -2 -2 2.778 2 2 R1 = 0.0868 for 2187 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.30 at 0.8620 0.3437 0.1630 [ 0.88 A from H8C ] Deepest hole -0.28 at 0.1443 0.9862 0.1641 [ 0.12 A from H8A ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 1944 / 16926 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.1380 0.3437 0.1630 1.00000 0.05 0.30 0.88 H8C 0.93 H8B 0.97 C8 1.79 H8A Q2 1 -0.1193 0.3965 0.3520 1.00000 0.05 0.27 0.83 C8 0.86 H8A 0.87 H8B 1.71 H8C Q3 1 0.1676 0.4752 0.1855 1.00000 0.05 0.21 0.76 C1 0.88 C2 1.56 H2 1.82 C6 Q4 1 -0.1753 0.5275 0.1589 1.00000 0.05 0.21 1.06 H8C 1.33 H8A 1.38 C8 2.25 C7 Q5 1 -0.1570 0.4884 0.2207 1.00000 0.05 0.19 0.79 H8A 0.85 C8 0.95 H8C 1.73 H8B Shortest distances between peaks (including symmetry equivalents) 4 5 0.60 2 5 1.33 1 2 1.46 1 5 1.49 1 4 1.83 2 4 1.93 3 4 2.59 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. 0.56: 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 1.14: Structure factors and derivatives 1.06: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.22: Solve l.s. equations 0.00: Generate HTAB table 0.06: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + shelxl finished at 15:01:22 Total CPU time: 3.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++