+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 16:12:16 on 17-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh005 in Cc CELL 0.71073 4.6142 17.0417 9.5621 90.000 93.378 90.000 ZERR 4.00 0.0002 0.0009 0.0006 0.000 0.003 0.000 LATT -7 SYMM X, - Y, 1/2 + Z SFAC C H N O F UNIT 32 32 4 4 4 V = 750.60 F(000) = 320.0 Mu = 0.11 mm-1 Cell Wt = 612.62 Rho = 1.355 MERG 2 OMIT -3.00 55.00 DFIX 0.88 0.02 N1 H1N FMAP 2 PLAN 5 TWIN EQIV $1 x, -y, z-1/2 HTAB N1 O1_$1 HTAB SIZE 0.8 0.08 0.06 ACTA BOND $H L.S. 16 TEMP -153.00 WGHT 0.017500 0.466500 BASF 0.39454 FVAR 0.96533 C1 1 0.945808 0.103328 0.916686 11.00000 0.01759 0.01913 = 0.02362 -0.00244 0.00123 -0.00144 C2 1 0.844534 0.121656 1.046904 11.00000 0.02749 0.02854 = 0.02244 -0.00227 0.00229 0.00000 AFIX 43 H2 2 0.911551 0.093029 1.127711 11.00000 -1.20000 AFIX 0 C3 1 0.645707 0.181782 1.058191 11.00000 0.02546 0.03106 = 0.03067 -0.00968 0.00544 -0.00095 AFIX 43 H3 2 0.573962 0.194516 1.146490 11.00000 -1.20000 AFIX 0 C4 1 0.553501 0.222745 0.940519 11.00000 0.02364 0.01994 = 0.04595 -0.00574 0.00122 0.00325 C5 1 0.647962 0.206332 0.810810 11.00000 0.02730 0.02829 = 0.03725 0.00671 -0.00181 0.00108 AFIX 43 H5 2 0.578894 0.235435 0.730914 11.00000 -1.20000 AFIX 0 C6 1 0.847533 0.146004 0.798876 11.00000 0.02459 0.02795 = 0.02472 0.00249 0.00192 0.00094 AFIX 43 H6 2 0.917390 0.133772 0.709962 11.00000 -1.20000 AFIX 0 C7 1 1.266975 -0.009137 0.985567 11.00000 0.02436 0.02483 = 0.02233 0.00268 -0.00020 -0.00181 C8 1 1.471309 -0.067369 0.926093 11.00000 0.02997 0.02681 = 0.03569 0.00277 0.00089 0.00519 AFIX 137 H8A 2 1.658087 -0.065824 0.980404 11.00000 -1.50000 H8B 2 1.500607 -0.054061 0.828224 11.00000 -1.50000 H8C 2 1.388424 -0.120180 0.930883 11.00000 -1.50000 AFIX 0 N1 3 1.148627 0.043175 0.893407 11.00000 0.02590 0.02362 = 0.01588 -0.00032 0.00326 0.00263 O1 4 1.212787 -0.010618 1.109986 11.00000 0.04448 0.04168 = 0.02254 0.00966 0.00599 0.00933 F1 5 0.357388 0.282540 0.953027 11.00000 0.03584 0.03184 = 0.06537 -0.00910 0.00239 0.01473 H1N 2 1.188401 0.035386 0.806310 11.00000 0.01958 HKLF 4 Covalent radii and connectivity table for 2008lsh005 in Cc C 0.770 H 0.320 N 0.700 O 0.660 F 0.640 C1 - C2 C6 N1 C2 - C3 C1 C3 - C4 C2 C4 - C5 C3 F1 C5 - C4 C6 C6 - C5 C1 C7 - O1 N1 C8 C8 - C7 N1 - C7 C1 O1 - C7 F1 - C4 Operators for generating equivalent atoms: $1 x, -y, z-1/2 Floating origin restraints generated h k l Fo^2 Sigma Why rejected 2 0 1 5.87 1.30 observed but should be systematically absent 4180 Reflections read, of which 64 rejected -5 =< h =< 5, -21 =< k =< 21, -12 =< l =< 12, Max. 2-theta = 54.97 1 Systematic absence violations 0 Inconsistent equivalents 1523 Unique reflections, of which 0 suppressed R(int) = 0.0279 R(sigma) = 0.0348 Friedel opposites not merged Maximum memory for data reduction = 1207 / 18042 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 = 1493 / 138232 wR2 = 0.0773 before cycle 1 for 1523 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 = 1.096; Restrained GooF = 1.095 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0175 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96533 0.00194 0.002 OSF 2 0.39463 0.88736 0.000 BASF 1 Mean shift/esd = 0.002 Maximum = 0.006 for U22 F1 Max. shift = 0.000 A for C7 Max. dU = 0.000 for C7 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1493 / 138232 wR2 = 0.0773 before cycle 2 for 1523 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 = 1.096; Restrained GooF = 1.095 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0175 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96533 0.00194 0.000 OSF 2 0.39469 0.88742 0.000 BASF 1 Mean shift/esd = 0.001 Maximum = 0.002 for U22 F1 Max. shift = 0.000 A for H8C Max. dU = 0.000 for C7 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1493 / 138232 wR2 = 0.0773 before cycle 3 for 1523 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 = 1.096; Restrained GooF = 1.095 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0175 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96533 0.00194 0.000 OSF 2 0.39460 0.88742 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for z O1 Max. shift = 0.000 A for H8B Max. dU = 0.000 for H1N Least-squares cycle 4 Maximum vector length = 511 Memory required = 1493 / 138232 wR2 = 0.0773 before cycle 4 for 1523 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 = 1.096; Restrained GooF = 1.095 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0175 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96533 0.00194 0.000 OSF 2 0.39456 0.88744 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for z O1 Max. shift = 0.000 A for H8B Max. dU = 0.000 for H1N Least-squares cycle 5 Maximum vector length = 511 Memory required = 1493 / 138232 wR2 = 0.0773 before cycle 5 for 1523 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 = 1.096; Restrained GooF = 1.095 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0175 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96533 0.00194 0.000 OSF 2 0.39458 0.88750 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for z O1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 6 Maximum vector length = 511 Memory required = 1493 / 138232 wR2 = 0.0773 before cycle 6 for 1523 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 = 1.096; Restrained GooF = 1.095 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0175 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96533 0.00194 0.000 OSF 2 0.39460 0.88744 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for z O1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 7 Maximum vector length = 511 Memory required = 1493 / 138232 wR2 = 0.0773 before cycle 7 for 1523 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 = 1.096; Restrained GooF = 1.095 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0175 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96533 0.00194 0.000 OSF 2 0.39463 0.88739 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for z O1 Max. shift = 0.000 A for C2 Max. dU = 0.000 for H1N Least-squares cycle 8 Maximum vector length = 511 Memory required = 1493 / 138232 wR2 = 0.0773 before cycle 8 for 1523 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 = 1.096; Restrained GooF = 1.095 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0175 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96533 0.00194 0.000 OSF 2 0.39458 0.88740 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for z O1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 9 Maximum vector length = 511 Memory required = 1493 / 138232 wR2 = 0.0773 before cycle 9 for 1523 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 = 1.096; Restrained GooF = 1.095 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0175 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96533 0.00194 0.000 OSF 2 0.39451 0.88740 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for z O1 Max. shift = 0.000 A for H8A Max. dU = 0.000 for H1N Least-squares cycle 10 Maximum vector length = 511 Memory required = 1493 / 138232 wR2 = 0.0773 before cycle 10 for 1523 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 = 1.096; Restrained GooF = 1.095 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0175 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96533 0.00194 0.000 OSF 2 0.39453 0.88743 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for z O1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for C4 Least-squares cycle 11 Maximum vector length = 511 Memory required = 1493 / 138232 wR2 = 0.0773 before cycle 11 for 1523 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 = 1.096; Restrained GooF = 1.095 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0175 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96533 0.00194 0.000 OSF 2 0.39456 0.88741 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for z O1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 12 Maximum vector length = 511 Memory required = 1493 / 138232 wR2 = 0.0773 before cycle 12 for 1523 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 = 1.096; Restrained GooF = 1.095 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0175 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96533 0.00194 0.000 OSF 2 0.39460 0.88739 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for z O1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 13 Maximum vector length = 511 Memory required = 1493 / 138232 wR2 = 0.0773 before cycle 13 for 1523 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 = 1.096; Restrained GooF = 1.095 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0175 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96533 0.00194 0.000 OSF 2 0.39459 0.88743 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for z O1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 14 Maximum vector length = 511 Memory required = 1493 / 138232 wR2 = 0.0773 before cycle 14 for 1523 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 = 1.096; Restrained GooF = 1.095 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0175 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96533 0.00194 0.000 OSF 2 0.39459 0.88742 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for z O1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 15 Maximum vector length = 511 Memory required = 1493 / 138232 wR2 = 0.0773 before cycle 15 for 1523 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 = 1.096; Restrained GooF = 1.095 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0175 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96533 0.00194 0.000 OSF 2 0.39461 0.88743 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for z O1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for F1 Least-squares cycle 16 Maximum vector length = 511 Memory required = 1493 / 138232 wR2 = 0.0773 before cycle 16 for 1523 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 = 1.096; Restrained GooF = 1.095 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0175 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96533 0.00194 0.000 OSF 2 0.39457 0.88741 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for z O1 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 H2 0.9116 0.0930 1.1277 43 0.950 0.000 C2 C3 C1 H3 0.5740 0.1945 1.1465 43 0.950 0.000 C3 C4 C2 H5 0.5789 0.2354 0.7309 43 0.950 0.000 C5 C4 C6 H6 0.9174 0.1338 0.7100 43 0.950 0.000 C6 C5 C1 H8A 1.6581 -0.0658 0.9804 137 0.980 0.000 C8 C7 H8A H8B 1.5006 -0.0541 0.8282 137 0.980 0.000 C8 C7 H8A H8C 1.3884 -0.1202 0.9309 137 0.980 0.000 C8 C7 H8A 2008lsh005 in Cc ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.94581 0.10333 0.91669 1.00000 0.01759 0.01913 0.02362 -0.00244 0.00123 -0.00144 0.02011 0.00276 0.00033 0.00010 0.00017 0.00000 0.00080 0.00078 0.00089 0.00065 0.00064 0.00064 0.00035 C2 0.84453 0.12166 1.04690 1.00000 0.02749 0.02854 0.02244 -0.00227 0.00229 0.00000 0.02612 0.00323 0.00038 0.00011 0.00020 0.00000 0.00097 0.00093 0.00089 0.00070 0.00073 0.00071 0.00040 H2 0.91155 0.09303 1.12771 1.00000 0.03135 0.00000 0.00000 C3 0.64571 0.18178 1.05819 1.00000 0.02546 0.03106 0.03067 -0.00968 0.00544 -0.00095 0.02891 0.00314 0.00039 0.00012 0.00020 0.00000 0.00093 0.00099 0.00100 0.00075 0.00073 0.00071 0.00041 H3 0.57396 0.19452 1.14649 1.00000 0.03470 0.00000 0.00000 C4 0.55350 0.22274 0.94052 1.00000 0.02364 0.01994 0.04595 -0.00574 0.00122 0.00325 0.02987 0.00310 0.00037 0.00010 0.00021 0.00000 0.00099 0.00091 0.00124 0.00078 0.00085 0.00074 0.00046 C5 0.64796 0.20633 0.81081 1.00000 0.02730 0.02829 0.03725 0.00671 -0.00181 0.00108 0.03109 0.00352 0.00041 0.00012 0.00021 0.00000 0.00092 0.00102 0.00110 0.00080 0.00076 0.00079 0.00043 H5 0.57889 0.23543 0.73091 1.00000 0.03731 0.00000 0.00000 C6 0.84753 0.14600 0.79888 1.00000 0.02459 0.02795 0.02472 0.00249 0.00192 0.00094 0.02573 0.00304 0.00035 0.00010 0.00019 0.00000 0.00092 0.00089 0.00084 0.00070 0.00070 0.00073 0.00038 H6 0.91739 0.13377 0.70996 1.00000 0.03088 0.00000 0.00000 C7 1.26697 -0.00914 0.98557 1.00000 0.02436 0.02483 0.02233 0.00268 -0.00020 -0.00181 0.02390 0.00300 0.00037 0.00010 0.00018 0.00000 0.00091 0.00089 0.00096 0.00066 0.00067 0.00068 0.00038 C8 1.47131 -0.06737 0.92609 1.00000 0.02997 0.02681 0.03569 0.00277 0.00089 0.00519 0.03086 0.00352 0.00040 0.00010 0.00022 0.00000 0.00100 0.00094 0.00100 0.00081 0.00077 0.00081 0.00042 H8A 1.65809 -0.06582 0.98040 1.00000 0.04629 0.00000 0.00000 H8B 1.50061 -0.05406 0.82822 1.00000 0.04629 0.00000 0.00000 H8C 1.38842 -0.12018 0.93088 1.00000 0.04629 0.00000 0.00000 N1 1.14863 0.04318 0.89341 1.00000 0.02590 0.02362 0.01588 -0.00032 0.00326 0.00263 0.02172 0.00250 0.00030 0.00008 0.00015 0.00000 0.00073 0.00070 0.00068 0.00056 0.00053 0.00059 0.00030 O1 1.21279 -0.01062 1.10999 1.00000 0.04448 0.04168 0.02254 0.00966 0.00599 0.00933 0.03607 0.00251 0.00030 0.00008 0.00014 0.00000 0.00088 0.00079 0.00076 0.00059 0.00055 0.00067 0.00036 F1 0.35739 0.28254 0.95303 1.00000 0.03584 0.03184 0.06537 -0.00910 0.00239 0.01473 0.04437 0.00216 0.00024 0.00007 0.00014 0.00000 0.00067 0.00064 0.00092 0.00059 0.00057 0.00054 0.00035 H1N 1.18840 0.03539 0.80631 1.00000 0.01958 0.03143 0.00402 0.00110 0.00163 0.00000 0.00486 Final Structure Factor Calculation for 2008lsh005 in Cc Total number of l.s. parameters = 106 Maximum vector length = 511 Memory required = 1389 / 26068 wR2 = 0.0773 before cycle 17 for 1523 data and 2 / 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 = 1.096; Restrained GooF = 1.095 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0175 * P )^2 + 0.47 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0347 for 1447 Fo > 4sig(Fo) and 0.0367 for all 1523 data wR2 = 0.0773, GooF = S = 1.096, Restrained GooF = 1.095 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 0.0247 0.0191 0.0165 C1 0.0293 0.0275 0.0215 C2 0.0410 0.0257 0.0200 C3 0.0474 0.0251 0.0171 C4 0.0416 0.0285 0.0232 C5 0.0295 0.0244 0.0234 C6 0.0282 0.0229 0.0206 C7 0.0365 0.0336 0.0225 C8 0.0277 0.0222 0.0153 N1 0.0548 0.0350 0.0185 O1 0.0687 0.0468 0.0177 F1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.025 0.040 0.051 0.063 0.078 0.100 0.125 0.154 0.213 1.000 Number in group 153. 160. 144. 156. 149. 158. 155. 144. 151. 153. GooF 1.093 1.221 1.113 1.135 0.957 1.130 1.018 1.117 0.917 1.210 K 1.165 1.068 0.977 0.986 1.016 1.007 0.997 1.001 1.009 0.997 Resolution(A) 0.77 0.80 0.84 0.88 0.93 1.00 1.08 1.18 1.36 1.72 inf Number in group 158. 152. 147. 152. 155. 152. 153. 149. 155. 150. GooF 1.107 1.126 1.149 1.043 0.978 0.957 1.161 0.876 1.094 1.393 K 1.044 1.023 1.030 1.006 0.993 0.999 0.991 1.000 1.030 0.991 R1 0.098 0.082 0.071 0.051 0.046 0.030 0.027 0.022 0.026 0.022 Recommended weighting scheme: WGHT 0.0154 0.4740 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) 3 9 3 36.63 12.65 4.71 0.034 1.10 -3 9 -3 40.96 12.67 4.42 0.034 1.10 -4 12 -2 135.85 186.61 3.81 0.129 0.87 0 4 5 312.61 261.08 3.55 0.152 1.74 -3 9 3 19.91 7.04 3.39 0.025 1.13 -5 9 -4 22.58 41.41 3.36 0.061 0.77 -1 5 -4 365.12 429.05 3.26 0.195 1.77 3 9 -3 18.47 7.05 3.20 0.025 1.13 1 1 -8 179.21 223.23 3.20 0.141 1.17 -3 11 1 69.55 94.56 3.20 0.092 1.09 -1 3 -10 18.80 35.72 3.18 0.056 0.91 4 4 -9 22.81 42.52 3.04 0.061 0.79 1 5 -4 12.28 22.04 2.89 0.044 1.83 0 4 2 631.92 704.29 2.81 0.250 3.18 0 2 -1 2519.51 2758.24 2.79 0.495 6.36 3 5 -9 14.28 25.36 2.79 0.047 0.87 0 4 -5 302.16 261.25 2.77 0.152 1.74 1 7 5 195.03 164.00 2.74 0.121 1.41 1 9 7 59.59 81.55 2.72 0.085 1.06 0 6 -10 121.00 92.51 2.72 0.091 0.90 0 2 1 2535.37 2758.47 2.68 0.495 6.36 -1 7 9 102.72 128.02 2.64 0.107 0.96 4 12 -5 19.11 9.22 2.62 0.029 0.82 0 4 -4 647.32 581.30 2.55 0.227 2.08 0 2 3 1126.16 1226.99 2.52 0.330 2.98 0 4 -2 636.15 704.37 2.50 0.250 3.18 -1 5 4 13.55 22.01 2.48 0.044 1.83 -1 7 1 657.93 597.14 2.47 0.230 2.11 3 11 -1 74.56 94.63 2.46 0.092 1.09 4 8 5 27.38 43.40 2.45 0.062 0.88 1 15 -9 115.82 83.64 2.44 0.086 0.77 -2 2 5 113.83 93.75 2.44 0.091 1.49 -2 6 -9 145.67 173.11 2.43 0.124 0.89 4 6 -9 35.17 21.92 2.42 0.044 0.77 -4 10 -3 17.16 29.05 2.39 0.051 0.90 0 4 0 1554.94 1680.55 2.35 0.386 4.26 1 1 -6 297.93 261.99 2.35 0.152 1.53 4 8 7 41.45 26.60 2.32 0.049 0.79 5 1 4 262.19 226.32 2.32 0.142 0.84 2 20 -2 9.35 0.60 2.29 0.007 0.79 0 2 -3 1123.24 1227.11 2.29 0.330 2.98 1 11 10 71.85 49.41 2.25 0.066 0.79 -2 6 -8 6.03 1.61 2.24 0.012 0.97 2 2 -5 113.92 93.74 2.23 0.091 1.49 0 8 5 19.00 11.82 2.23 0.032 1.42 0 14 8 51.83 69.81 2.22 0.079 0.85 0 12 -9 118.75 93.63 2.20 0.091 0.85 1 3 -7 120.83 142.98 2.19 0.113 1.29 0 20 1 145.02 111.14 2.18 0.099 0.85 4 6 -3 1.90 0.11 2.17 0.003 1.03 Bond lengths and angles C1 - Distance Angles C2 1.3910 (0.0024) C6 1.3941 (0.0023) 119.72 (0.15) N1 1.4145 (0.0021) 124.32 (0.14) 115.95 (0.14) C1 - C2 C6 C2 - Distance Angles C3 1.3838 (0.0025) C1 1.3910 (0.0024) 119.69 (0.17) H2 0.9500 120.15 120.16 C2 - C3 C1 C3 - Distance Angles C4 1.3704 (0.0026) C2 1.3838 (0.0025) 119.23 (0.17) H3 0.9500 120.38 120.38 C3 - C4 C2 C4 - Distance Angles C5 1.3676 (0.0027) C3 1.3704 (0.0026) 122.71 (0.16) F1 1.3727 (0.0020) 118.54 (0.17) 118.75 (0.16) C4 - C5 C3 C5 - Distance Angles C4 1.3676 (0.0027) C6 1.3894 (0.0025) 118.30 (0.17) H5 0.9500 120.85 120.85 C5 - C4 C6 C6 - Distance Angles C5 1.3894 (0.0025) C1 1.3941 (0.0023) 120.35 (0.17) H6 0.9500 119.83 119.83 C6 - C5 C1 C7 - Distance Angles O1 1.2303 (0.0020) N1 1.3464 (0.0022) 123.29 (0.16) C8 1.5035 (0.0025) 121.33 (0.16) 115.38 (0.16) C7 - O1 N1 C8 - Distance Angles C7 1.5035 (0.0025) 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 1.3464 (0.0022) C1 1.4145 (0.0021) 128.57 (0.15) H1N 0.8734 (0.0146) 115.06 (1.27) 116.00 (1.28) N1 - C7 C1 O1 - Distance Angles C7 1.2303 (0.0020) O1 - F1 - Distance Angles C4 1.3727 (0.0020) F1 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.873(15) 1.934(15) 2.7990(19) 170.5(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)