+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 21:07:00 on 11-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009lsh008 in Pbca CELL 0.71073 10.5174 9.4252 16.2656 90.000 90.000 90.000 ZERR 8.00 0.0002 0.0004 0.0006 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N O CL UNIT 64 64 8 8 8 V = 1612.39 F(000) = 704.0 Mu = 0.41 mm-1 Cell Wt = 1356.83 Rho = 1.397 MERG 2 OMIT -3.00 55.00 OMIT 1 1 1 DFIX 0.88 0.01 N1 H1N FMAP 2 PLAN 5 SIZE 0.08 0.66 0.66 ACTA EQIV $1 -x+3/2, y+1/2, z HTAB N1 O1_$1 HTAB BOND $H L.S. 16 TEMP -153.00 WGHT 0.038200 1.058900 FVAR 0.17292 C1 1 0.975369 -0.015845 0.622427 11.00000 0.01416 0.01334 = 0.01538 0.00370 0.00055 -0.00065 C2 1 1.043736 0.066814 0.677841 11.00000 0.01773 0.02064 = 0.01717 0.00101 0.00251 -0.00363 C3 1 1.172412 0.045743 0.691877 11.00000 0.01804 0.03515 = 0.02549 0.00559 -0.00369 -0.00771 AFIX 43 H3 2 1.216936 0.104112 0.729803 11.00000 -1.20000 AFIX 0 C4 1 1.235235 -0.061037 0.650131 11.00000 0.01405 0.03751 = 0.03677 0.01157 -0.00031 0.00103 AFIX 43 H4 2 1.323040 -0.077528 0.659955 11.00000 -1.20000 AFIX 0 C5 1 1.169715 -0.144136 0.593808 11.00000 0.02230 0.02813 = 0.03218 0.00748 0.00759 0.00713 AFIX 43 H5 2 1.213059 -0.217074 0.564834 11.00000 -1.20000 AFIX 0 C6 1 1.040898 -0.121146 0.579575 11.00000 0.02272 0.01839 = 0.01802 0.00230 0.00203 0.00153 AFIX 43 H6 2 0.997193 -0.177660 0.540330 11.00000 -1.20000 AFIX 0 C7 1 0.755339 -0.090287 0.594917 11.00000 0.01881 0.01408 = 0.02465 -0.00054 -0.00362 -0.00114 C8 1 0.624184 -0.035301 0.576544 11.00000 0.01657 0.02023 = 0.04351 0.00110 -0.00930 -0.00055 AFIX 137 H8A 2 0.616645 -0.015838 0.517560 11.00000 -1.50000 H8B 2 0.609438 0.052315 0.607553 11.00000 -1.50000 H8C 2 0.560982 -0.106541 0.592542 11.00000 -1.50000 AFIX 0 N1 3 0.844466 0.010785 0.608933 11.00000 0.01492 0.00979 = 0.02221 -0.00050 -0.00126 0.00005 O1 4 0.779525 -0.217450 0.595760 11.00000 0.02167 0.01247 = 0.05668 -0.00237 -0.00502 -0.00196 CL1 5 0.967531 0.199691 0.733505 11.00000 0.02505 0.03055 = 0.03140 -0.01632 0.00411 -0.00861 H1N 2 0.816875 0.098120 0.609985 11.00000 0.02372 HKLF 4 Covalent radii and connectivity table for 2009lsh008 in Pbca C 0.770 H 0.320 N 0.700 O 0.660 CL 0.990 C1 - C2 C6 N1 C2 - C3 C1 Cl1 C3 - C4 C2 C4 - C3 C5 C5 - C4 C6 C6 - C5 C1 C7 - O1 N1 C8 C8 - C7 N1 - C7 C1 O1 - C7 Cl1 - C2 Operators for generating equivalent atoms: $1 -x+3/2, y+1/2, z 12449 Reflections read, of which 970 rejected -13 =< h =< 13, -12 =< k =< 12, -18 =< l =< 21, Max. 2-theta = 54.99 0 Systematic absence violations 0 Inconsistent equivalents 1843 Unique reflections, of which 0 suppressed R(int) = 0.0431 R(sigma) = 0.0303 Friedel opposites merged Maximum memory for data reduction = 1233 / 18429 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 = 1515 / 137102 wR2 = 0.0967 before cycle 1 for 1843 data and 105 / 105 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 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 = 1.105; Restrained GooF = 1.105 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0382 * P )^2 + 1.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17292 0.00041 -0.005 OSF Mean shift/esd = 0.003 Maximum = 0.017 for U13 Cl1 Max. shift = 0.000 A for H8C Max. dU = 0.000 for H1N Least-squares cycle 2 Maximum vector length = 511 Memory required = 1515 / 137102 wR2 = 0.0967 before cycle 2 for 1843 data and 105 / 105 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 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 = 1.105; Restrained GooF = 1.105 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0382 * P )^2 + 1.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17292 0.00041 0.000 OSF Mean shift/esd = 0.001 Maximum = 0.006 for U13 Cl1 Max. shift = 0.000 A for H8C Max. dU = 0.000 for H1N Least-squares cycle 3 Maximum vector length = 511 Memory required = 1515 / 137102 wR2 = 0.0967 before cycle 3 for 1843 data and 105 / 105 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 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 = 1.105; Restrained GooF = 1.105 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0382 * P )^2 + 1.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17292 0.00041 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C4 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 4 Maximum vector length = 511 Memory required = 1515 / 137102 wR2 = 0.0967 before cycle 4 for 1843 data and 105 / 105 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 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 = 1.105; Restrained GooF = 1.105 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0382 * P )^2 + 1.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17292 0.00041 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x C2 Max. shift = 0.000 A for H8A Max. dU = 0.000 for H1N Least-squares cycle 5 Maximum vector length = 511 Memory required = 1515 / 137102 wR2 = 0.0967 before cycle 5 for 1843 data and 105 / 105 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 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 = 1.105; Restrained GooF = 1.105 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0382 * P )^2 + 1.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17292 0.00041 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x C2 Max. shift = 0.000 A for H8A Max. dU = 0.000 for H1N Least-squares cycle 6 Maximum vector length = 511 Memory required = 1515 / 137102 wR2 = 0.0967 before cycle 6 for 1843 data and 105 / 105 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 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 = 1.105; Restrained GooF = 1.105 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0382 * P )^2 + 1.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17292 0.00041 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x C2 Max. shift = 0.000 A for H8A Max. dU = 0.000 for H1N Least-squares cycle 7 Maximum vector length = 511 Memory required = 1515 / 137102 wR2 = 0.0967 before cycle 7 for 1843 data and 105 / 105 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 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 = 1.105; Restrained GooF = 1.105 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0382 * P )^2 + 1.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17292 0.00041 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x C2 Max. shift = 0.000 A for H8A Max. dU = 0.000 for H1N Least-squares cycle 8 Maximum vector length = 511 Memory required = 1515 / 137102 wR2 = 0.0967 before cycle 8 for 1843 data and 105 / 105 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 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 = 1.105; Restrained GooF = 1.105 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0382 * P )^2 + 1.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17292 0.00041 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x C2 Max. shift = 0.000 A for H8A Max. dU = 0.000 for H1N Least-squares cycle 9 Maximum vector length = 511 Memory required = 1515 / 137102 wR2 = 0.0967 before cycle 9 for 1843 data and 105 / 105 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 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 = 1.105; Restrained GooF = 1.105 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0382 * P )^2 + 1.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17292 0.00041 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 10 Maximum vector length = 511 Memory required = 1515 / 137102 wR2 = 0.0967 before cycle 10 for 1843 data and 105 / 105 parameters Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 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 = 1.105; Restrained GooF = 1.105 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0382 * P )^2 + 1.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17292 0.00041 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x C2 Max. shift = 0.000 A for H8A Max. dU = 0.000 for O1 Least-squares cycle 11 Maximum vector length = 511 Memory required = 1515 / 137102 wR2 = 0.0967 before cycle 11 for 1843 data and 105 / 105 parameters Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 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 = 1.105; Restrained GooF = 1.105 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0382 * P )^2 + 1.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17292 0.00041 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x C2 Max. shift = 0.000 A for H8A Max. dU = 0.000 for H1N Least-squares cycle 12 Maximum vector length = 511 Memory required = 1515 / 137102 wR2 = 0.0967 before cycle 12 for 1843 data and 105 / 105 parameters Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 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 = 1.105; Restrained GooF = 1.105 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0382 * P )^2 + 1.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17292 0.00041 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x C2 Max. shift = 0.000 A for H8A Max. dU = 0.000 for H1N Least-squares cycle 13 Maximum vector length = 511 Memory required = 1515 / 137102 wR2 = 0.0967 before cycle 13 for 1843 data and 105 / 105 parameters Summary of restraints applied in cycle 13 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 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 = 1.105; Restrained GooF = 1.105 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0382 * P )^2 + 1.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17292 0.00041 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 C4 Least-squares cycle 14 Maximum vector length = 511 Memory required = 1515 / 137102 wR2 = 0.0967 before cycle 14 for 1843 data and 105 / 105 parameters Summary of restraints applied in cycle 14 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 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 = 1.105; Restrained GooF = 1.105 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0382 * P )^2 + 1.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17292 0.00041 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x C2 Max. shift = 0.000 A for H8A Max. dU = 0.000 for H1N Least-squares cycle 15 Maximum vector length = 511 Memory required = 1515 / 137102 wR2 = 0.0967 before cycle 15 for 1843 data and 105 / 105 parameters Summary of restraints applied in cycle 15 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 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 = 1.105; Restrained GooF = 1.105 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0382 * P )^2 + 1.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17292 0.00041 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x C2 Max. shift = 0.000 A for H8A Max. dU = 0.000 for N1 Least-squares cycle 16 Maximum vector length = 511 Memory required = 1515 / 137102 wR2 = 0.0967 before cycle 16 for 1843 data and 105 / 105 parameters Summary of restraints applied in cycle 16 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 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 = 1.105; Restrained GooF = 1.105 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0382 * P )^2 + 1.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.17292 0.00041 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 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 H3 1.2169 0.1041 0.7298 43 0.950 0.000 C3 C4 C2 H4 1.3230 -0.0775 0.6600 43 0.950 0.000 C4 C3 C5 H5 1.2131 -0.2171 0.5648 43 0.950 0.000 C5 C4 C6 H6 0.9972 -0.1777 0.5403 43 0.950 0.000 C6 C5 C1 H8A 0.6166 -0.0158 0.5176 137 0.980 0.000 C8 C7 H8A H8B 0.6094 0.0523 0.6076 137 0.980 0.000 C8 C7 H8A H8C 0.5610 -0.1065 0.5925 137 0.980 0.000 C8 C7 H8A 2009lsh008 in Pbca ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.97537 -0.01585 0.62243 1.00000 0.01416 0.01334 0.01538 0.00370 0.00055 -0.00065 0.01429 0.00267 0.00014 0.00016 0.00009 0.00000 0.00072 0.00073 0.00074 0.00059 0.00055 0.00060 0.00032 C2 1.04374 0.06681 0.67784 1.00000 0.01773 0.02064 0.01717 0.00101 0.00251 -0.00363 0.01851 0.00287 0.00015 0.00018 0.00010 0.00000 0.00079 0.00084 0.00078 0.00064 0.00060 0.00065 0.00035 C3 1.17241 0.04574 0.69188 1.00000 0.01804 0.03515 0.02549 0.00559 -0.00369 -0.00771 0.02623 0.00321 0.00016 0.00021 0.00011 0.00000 0.00083 0.00106 0.00091 0.00079 0.00067 0.00075 0.00041 H3 1.21694 0.10411 0.72980 1.00000 0.03147 0.00000 0.00000 C4 1.23524 -0.06104 0.65013 1.00000 0.01405 0.03751 0.03677 0.01157 -0.00031 0.00103 0.02945 0.00358 0.00017 0.00022 0.00012 0.00000 0.00082 0.00114 0.00107 0.00088 0.00072 0.00077 0.00044 H4 1.32304 -0.07753 0.65995 1.00000 0.03533 0.00000 0.00000 C5 1.16972 -0.14414 0.59381 1.00000 0.02230 0.02813 0.03218 0.00748 0.00759 0.00713 0.02754 0.00361 0.00017 0.00021 0.00012 0.00000 0.00089 0.00100 0.00101 0.00081 0.00073 0.00077 0.00042 H5 1.21306 -0.21707 0.56483 1.00000 0.03304 0.00000 0.00000 C6 1.04090 -0.12115 0.57958 1.00000 0.02272 0.01839 0.01802 0.00230 0.00203 0.00153 0.01971 0.00310 0.00016 0.00018 0.00010 0.00000 0.00086 0.00082 0.00082 0.00064 0.00062 0.00068 0.00036 H6 0.99719 -0.17766 0.54033 1.00000 0.02365 0.00000 0.00000 C7 0.75534 -0.09029 0.59492 1.00000 0.01881 0.01408 0.02465 -0.00054 -0.00362 -0.00114 0.01918 0.00290 0.00017 0.00018 0.00011 0.00000 0.00080 0.00081 0.00086 0.00067 0.00065 0.00063 0.00035 C8 0.62418 -0.03530 0.57654 1.00000 0.01657 0.02023 0.04351 0.00110 -0.00930 -0.00055 0.02677 0.00313 0.00016 0.00020 0.00013 0.00000 0.00082 0.00090 0.00112 0.00079 0.00074 0.00069 0.00042 H8A 0.61664 -0.01584 0.51756 1.00000 0.04015 0.00000 0.00000 H8B 0.60944 0.05231 0.60755 1.00000 0.04015 0.00000 0.00000 H8C 0.56098 -0.10654 0.59254 1.00000 0.04015 0.00000 0.00000 N1 0.84447 0.01078 0.60893 1.00000 0.01492 0.00979 0.02221 -0.00050 -0.00126 0.00005 0.01564 0.00231 0.00013 0.00014 0.00008 0.00000 0.00065 0.00064 0.00070 0.00055 0.00051 0.00051 0.00029 O1 0.77953 -0.21745 0.59576 1.00000 0.02167 0.01247 0.05668 -0.00237 -0.00502 -0.00196 0.03027 0.00226 0.00012 0.00013 0.00010 0.00000 0.00068 0.00065 0.00091 0.00059 0.00058 0.00049 0.00034 Cl1 0.96753 0.19969 0.73351 1.00000 0.02505 0.03055 0.03140 -0.01632 0.00411 -0.00861 0.02900 0.00071 0.00004 0.00005 0.00003 0.00000 0.00025 0.00026 0.00027 0.00019 0.00017 0.00018 0.00016 H1N 0.81687 0.09812 0.60999 1.00000 0.02372 0.03212 0.00177 0.00119 0.00122 0.00000 0.00528 Final Structure Factor Calculation for 2009lsh008 in Pbca Total number of l.s. parameters = 105 Maximum vector length = 511 Memory required = 1410 / 24017 wR2 = 0.0967 before cycle 17 for 1843 data and 0 / 105 parameters Summary of restraints applied in cycle 17 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.010 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 = 1.105; Restrained GooF = 1.105 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0382 * P )^2 + 1.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0389 for 1567 Fo > 4sig(Fo) and 0.0490 for all 1843 data wR2 = 0.0967, GooF = S = 1.105, Restrained GooF = 1.105 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 0.0182 0.0143 0.0103 C1 0.0232 0.0190 0.0134 C2 0.0409 0.0229 0.0148 C3 0.0487 0.0256 0.0140 C4 0.0431 0.0226 0.0170 C5 0.0244 0.0189 0.0159 C6 0.0264 0.0175 0.0136 C7 0.0465 0.0202 0.0137 C8 0.0224 0.0147 0.0098 N1 0.0575 0.0215 0.0118 O1 0.0505 0.0230 0.0135 Cl1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.022 0.035 0.048 0.061 0.076 0.096 0.128 0.187 1.000 Number in group 194. 176. 198. 177. 189. 173. 182. 184. 185. 185. GooF 1.205 1.133 1.108 1.221 0.955 1.245 0.934 1.111 0.993 1.109 K 3.334 1.229 1.070 0.999 0.989 1.008 0.991 0.997 1.011 0.989 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.64 inf Number in group 186. 188. 180. 183. 186. 184. 186. 181. 185. 184. GooF 0.967 0.824 0.957 0.903 1.003 1.040 0.899 1.115 1.286 1.757 K 0.984 1.008 0.997 1.010 1.006 1.008 1.011 1.009 1.010 0.980 R1 0.113 0.076 0.077 0.066 0.055 0.047 0.035 0.032 0.035 0.034 Recommended weighting scheme: WGHT 0.0381 1.0596 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) 0 4 4 275.49 163.34 5.61 0.070 2.04 3 0 8 279.49 165.12 5.46 0.070 1.76 10 0 6 170.23 341.91 5.06 0.101 0.98 1 2 2 118.97 64.85 4.75 0.044 3.80 2 5 3 61.11 24.66 4.44 0.027 1.69 1 1 11 30.01 6.49 4.07 0.014 1.45 2 2 0 2005.39 2422.49 3.72 0.268 3.51 0 2 0 5630.75 6673.71 3.60 0.444 4.71 1 4 6 740.94 594.42 3.58 0.133 1.75 3 2 11 33.45 9.55 3.55 0.017 1.31 4 3 4 15.79 2.63 3.53 0.009 1.81 5 3 3 98.33 61.72 3.49 0.043 1.66 1 3 5 258.87 340.04 3.38 0.100 2.21 3 2 5 1117.92 940.70 3.19 0.167 2.13 1 6 5 649.91 534.73 3.07 0.126 1.40 3 4 6 32.24 59.81 3.04 0.042 1.59 0 0 8 1029.02 1261.41 3.03 0.193 2.03 1 6 3 26.16 2.76 3.00 0.009 1.49 1 5 1 220.90 164.89 2.97 0.070 1.84 3 7 11 130.79 84.87 2.93 0.050 0.96 1 5 5 175.83 128.57 2.88 0.062 1.61 1 1 9 1066.64 904.78 2.82 0.164 1.75 1 7 1 155.30 110.91 2.79 0.057 1.33 3 11 3 80.32 35.91 2.72 0.033 0.82 5 4 8 16.38 2.48 2.70 0.009 1.24 3 8 15 177.35 245.46 2.70 0.085 0.78 4 1 7 8.11 0.06 2.69 0.001 1.71 6 2 0 296.65 234.57 2.69 0.083 1.64 4 0 4 33.27 55.55 2.67 0.041 2.21 0 2 2 2643.16 3019.92 2.66 0.299 4.08 4 6 6 48.44 26.88 2.64 0.028 1.21 8 6 0 32.98 1.23 2.59 0.006 1.01 5 2 4 6.41 0.09 2.58 0.002 1.74 2 0 6 424.54 509.79 2.56 0.123 2.41 4 0 8 2031.17 1781.02 2.52 0.230 1.61 4 9 1 -7.79 7.57 2.52 0.015 0.97 0 6 7 269.00 338.00 2.49 0.100 1.30 3 5 8 323.97 264.36 2.45 0.088 1.29 1 1 2 11.49 25.54 2.44 0.027 5.31 9 5 10 6.64 25.33 2.41 0.027 0.85 6 2 5 8.11 1.28 2.38 0.006 1.47 3 4 7 89.17 120.62 2.36 0.060 1.50 0 2 7 1145.07 1000.44 2.35 0.172 2.08 1 3 4 179.97 142.58 2.35 0.065 2.42 6 6 9 23.12 43.08 2.31 0.036 0.98 4 9 5 19.37 1.40 2.30 0.006 0.93 8 8 0 36.57 62.98 2.30 0.043 0.88 5 6 16 28.73 1.15 2.30 0.006 0.79 3 5 1 172.21 135.13 2.29 0.063 1.65 5 1 3 1635.20 1456.42 2.29 0.208 1.92 Bond lengths and angles C1 - Distance Angles C2 1.3915 (0.0022) C6 1.3949 (0.0023) 117.82 (0.14) N1 1.4166 (0.0020) 120.22 (0.14) 121.93 (0.14) C1 - C2 C6 C2 - Distance Angles C3 1.3868 (0.0024) C1 1.3915 (0.0022) 122.05 (0.16) Cl1 1.7409 (0.0017) 117.82 (0.14) 120.12 (0.12) C2 - C3 C1 C3 - Distance Angles C4 1.3822 (0.0029) C2 1.3868 (0.0024) 119.33 (0.17) H3 0.9500 120.33 120.33 C3 - C4 C2 C4 - Distance Angles C3 1.3822 (0.0029) C5 1.3884 (0.0029) 119.84 (0.16) H4 0.9500 120.08 120.08 C4 - C3 C5 C5 - Distance Angles C4 1.3884 (0.0029) C6 1.3914 (0.0025) 120.35 (0.18) H5 0.9500 119.83 119.83 C5 - C4 C6 C6 - Distance Angles C5 1.3914 (0.0025) C1 1.3949 (0.0023) 120.58 (0.17) H6 0.9500 119.71 119.71 C6 - C5 C1 C7 - Distance Angles O1 1.2253 (0.0021) N1 1.3558 (0.0021) 122.81 (0.16) C8 1.5036 (0.0023) 121.99 (0.15) 115.18 (0.15) C7 - O1 N1 C8 - Distance Angles C7 1.5036 (0.0023) 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 1.3558 (0.0021) C1 1.4166 (0.0020) 125.00 (0.14) H1N 0.8730 (0.0093) 115.85 (1.31) 119.15 (1.31) N1 - C7 C1 O1 - Distance Angles C7 1.2253 (0.0021) O1 - Cl1 - Distance Angles C2 1.7409 (0.0017) Cl1 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.873(9) 2.026(10) 2.8823(18) 166.7(18) 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)