+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 19:31:36 on 10-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh057 in Pbca CELL 0.71073 10.5132 9.4393 15.1635 90.000 90.000 90.000 ZERR 8.00 0.0004 0.0003 0.0005 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 F UNIT 64 64 8 8 8 V = 1504.78 F(000) = 640.0 Mu = 0.11 mm-1 Cell Wt = 1225.23 Rho = 1.352 MERG 2 OMIT -3.00 55.00 OMIT 0 0 4 OMIT 0 2 3 OMIT 1 0 4 OMIT 1 1 3 OMIT 1 1 1 EADP C1A C1B EADP C2A C2B EADP C4A C3B EADP C4A C4B EADP C5A C5B EADP C6A C6B DFIX 0.88 0.02 N1 H1N EQIV $1 -x+1/2, y+1/2, z HTAB N1 O1_$1 FMAP 2 PLAN 5 SIZE 0.50 0.60 0.80 ACTA BOND $H WGHT 0.05380 0.54240 L.S. 10 TEMP -153.00 FVAR 0.31893 0.82232 C7 1 0.244279 -0.100018 0.595311 11.00000 0.02431 0.01491 = 0.02869 0.00005 0.00401 0.00083 C8 1 0.377674 -0.055534 0.572568 11.00000 0.02386 0.02186 = 0.04743 -0.00030 0.00943 0.00018 AFIX 137 H8A 2 0.438193 -0.108899 0.608800 11.00000 -1.50000 H8B 2 0.387754 0.046028 0.584014 11.00000 -1.50000 H8C 2 0.393994 -0.074744 0.510071 11.00000 -1.50000 AFIX 0 N1 3 0.161396 0.006517 0.609076 11.00000 0.02030 0.01151 = 0.02844 -0.00048 0.00047 -0.00040 O1 4 0.213657 -0.225523 0.599282 11.00000 0.02771 0.01257 = 0.07386 0.00164 0.00915 0.00198 PART 1 C1A 1 0.027778 -0.010353 0.628356 21.00000 0.01566 0.01566 = 0.02011 0.00269 -0.00022 -0.00006 C2A 1 -0.029880 0.085673 0.684168 21.00000 0.02143 0.01532 = 0.02585 -0.00032 -0.00013 -0.00164 C3A 1 -0.158409 0.082783 0.703861 21.00000 0.01866 0.02759 = 0.03039 0.00022 0.00726 0.00464 AFIX 43 H3A 2 -0.195348 0.151611 0.741721 21.00000 -1.20000 AFIX 0 C4A 1 -0.231715 -0.024056 0.666466 21.00000 0.01827 0.03474 = 0.03505 0.00307 0.00199 -0.00289 AFIX 43 H4A 2 -0.320072 -0.029885 0.679080 21.00000 -1.20000 AFIX 0 C5A 1 -0.175459 -0.121905 0.610784 21.00000 0.02715 0.02893 = 0.03198 -0.00029 -0.00314 -0.00873 AFIX 43 H5A 2 -0.226360 -0.194416 0.585442 21.00000 -1.20000 AFIX 0 C6A 1 -0.047623 -0.116916 0.591147 21.00000 0.02413 0.01624 = 0.02386 -0.00278 -0.00076 -0.00535 AFIX 43 H6A 2 -0.010996 -0.185142 0.552722 21.00000 -1.20000 AFIX 0 F1A 5 0.044817 0.190431 0.719626 21.00000 0.03188 0.02397 = 0.04078 -0.01501 0.00221 -0.00098 PART 2 SAME C1A > F1A C1B 1 0.046590 -0.002674 0.629181 -21.00000 0.01566 0.01566 = 0.02011 0.00269 -0.00022 -0.00006 C2B 1 -0.036609 -0.092076 0.593215 -21.00000 0.02143 0.01532 = 0.02585 -0.00032 -0.00013 -0.00164 C3B 1 -0.170250 -0.104912 0.613339 -21.00000 0.01827 0.03474 = 0.03505 0.00307 0.00199 -0.00289 AFIX 43 H3B 2 -0.223572 -0.175746 0.588558 -21.00000 -1.20000 AFIX 0 C4B 1 -0.213760 -0.001858 0.673431 -21.00000 0.01827 0.03474 = 0.03505 0.00307 0.00199 -0.00289 AFIX 43 H4B 2 -0.300587 -0.000424 0.690762 -21.00000 -1.20000 AFIX 0 C5B 1 -0.131634 0.095148 0.706448 -21.00000 0.02715 0.02893 = 0.03198 -0.00029 -0.00314 -0.00873 AFIX 43 H5B 2 -0.163995 0.163599 0.746523 -21.00000 -1.20000 AFIX 0 C6B 1 -0.009235 0.100682 0.686466 -21.00000 0.02413 0.01624 = 0.02386 -0.00278 -0.00076 -0.00535 AFIX 43 H6B 2 0.042169 0.174004 0.710374 -21.00000 -1.20000 AFIX 0 F1B 5 0.003522 -0.188222 0.529052 -21.00000 0.03806 0.02389 = 0.03019 -0.00725 -0.00041 -0.00443 PART 0 H1N 2 0.191552 0.093128 0.606791 11.00000 0.03362 HKLF 4 Covalent radii and connectivity table for 2008lsh057 in Pbca C 0.770 H 0.320 N 0.700 O 0.660 F 0.640 C7 - O1 N1 C8 C8 - C7 N1 - C1B_b C7 C1A_a O1 - C7 C1A_a - C2A_a C6A_a N1 C2A_a - F1A_a C1A_a C3A_a C3A_a - C2A_a C4A_a C4A_a - C5A_a C3A_a C5A_a - C6A_a C4A_a C6A_a - C5A_a C1A_a F1A_a - C2A_a C1B_b - N1 C2B_b C6B_b C2B_b - C1B_b F1B_b C3B_b C3B_b - C4B_b C2B_b C4B_b - C5B_b C3B_b C5B_b - C6B_b C4B_b C6B_b - C5B_b C1B_b F1B_b - C2B_b Operators for generating equivalent atoms: $1 -x+1/2, y+1/2, z h k l Fo^2 Sigma Why rejected 1 4 0 0.84 0.21 observed but should be systematically absent 3 0 3 0.52 0.13 observed but should be systematically absent 6 0 3 0.89 0.20 observed but should be systematically absent 13328 Reflections read, of which 1112 rejected -13 =< h =< 13, -12 =< k =< 12, -19 =< l =< 18, Max. 2-theta = 54.96 3 Systematic absence violations 0 Inconsistent equivalents 1716 Unique reflections, of which 0 suppressed R(int) = 0.0359 R(sigma) = 0.0236 Friedel opposites merged Maximum memory for data reduction = 1849 / 17230 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 = 2255 / 169120 wR2 = 0.1056 before cycle 1 for 1716 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. 15. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.002 0.000 0.037 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.041 for 16 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0538 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31893 0.00093 0.000 OSF 2 0.82228 0.00250 -0.015 FVAR 2 Mean shift/esd = 0.007 Maximum = -0.032 for U22 N1 Max. shift = 0.000 A for H3B_b Max. dU = 0.000 for H1N Least-squares cycle 2 Maximum vector length = 511 Memory required = 2255 / 169120 wR2 = 0.1056 before cycle 2 for 1716 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. 15. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.000 0.037 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.041 for 16 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0538 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31892 0.00093 -0.011 OSF 2 0.82227 0.00250 -0.006 FVAR 2 Mean shift/esd = 0.003 Maximum = 0.012 for tors H8A Max. shift = 0.000 A for C3B_b Max. dU = 0.000 for H1N Least-squares cycle 3 Maximum vector length = 511 Memory required = 2255 / 169120 wR2 = 0.1056 before cycle 3 for 1716 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. 15. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.000 0.037 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.041 for 16 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0538 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31892 0.00093 0.000 OSF 2 0.82227 0.00250 0.000 FVAR 2 Mean shift/esd = 0.001 Maximum = 0.005 for tors H8A Max. shift = 0.000 A for C3B_b Max. dU = 0.000 for H1N Least-squares cycle 4 Maximum vector length = 511 Memory required = 2255 / 169120 wR2 = 0.1056 before cycle 4 for 1716 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. 15. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.000 0.037 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.041 for 16 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0538 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31892 0.00093 0.000 OSF 2 0.82227 0.00250 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.002 for x C3B_b Max. shift = 0.000 A for H3B_b Max. dU = 0.000 for H1N Least-squares cycle 5 Maximum vector length = 511 Memory required = 2255 / 169120 wR2 = 0.1056 before cycle 5 for 1716 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. 15. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.000 0.037 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.041 for 16 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0538 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31892 0.00093 0.000 OSF 2 0.82227 0.00250 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.002 for x C3B_b Max. shift = 0.000 A for H3B_b Max. dU = 0.000 for C1A_a Least-squares cycle 6 Maximum vector length = 511 Memory required = 2255 / 169120 wR2 = 0.1056 before cycle 6 for 1716 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. 15. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.000 0.037 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.041 for 16 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0538 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31892 0.00093 0.000 OSF 2 0.82227 0.00250 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.001 for x C3B_b Max. shift = 0.000 A for C3B_b Max. dU = 0.000 for C2A_a Least-squares cycle 7 Maximum vector length = 511 Memory required = 2255 / 169120 wR2 = 0.1056 before cycle 7 for 1716 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. 15. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.000 0.037 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.041 for 16 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0538 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31892 0.00093 0.000 OSF 2 0.82227 0.00250 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.001 for x C3B_b Max. shift = 0.000 A for H3B_b Max. dU = 0.000 for C1A_a Least-squares cycle 8 Maximum vector length = 511 Memory required = 2255 / 169120 wR2 = 0.1056 before cycle 8 for 1716 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. 15. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.000 0.037 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.041 for 16 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0538 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31892 0.00093 0.000 OSF 2 0.82227 0.00250 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for x C2B_b Max. shift = 0.000 A for C2B_b Max. dU = 0.000 for F1B_b Least-squares cycle 9 Maximum vector length = 511 Memory required = 2255 / 169120 wR2 = 0.1056 before cycle 9 for 1716 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. 15. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.000 0.037 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.041 for 16 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0538 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31892 0.00093 0.000 OSF 2 0.82227 0.00250 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for x C5A_a Max. shift = 0.000 A for C3B_b Max. dU = 0.000 for C2A_a Least-squares cycle 10 Maximum vector length = 511 Memory required = 2255 / 169120 wR2 = 0.1056 before cycle 10 for 1716 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. 15. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.000 0.037 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.041 for 16 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0538 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.31892 0.00093 0.000 OSF 2 0.82227 0.00250 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for z C7 Max. shift = 0.000 A for C1B_b Max. dU = 0.000 for C1A_a Largest correlation matrix elements -0.983 z C1B_b / z C1A_a -0.928 y C3B_b / y C5A_a 0.887 U12 C1A_a / y C1A_a -0.979 y C1B_b / y C1A_a -0.921 z C2B_b / z C6A_a -0.882 z C5B_b / z C3A_a -0.969 z C3B_b / z C5A_a -0.913 x C1B_b / U11 C1A_a -0.870 x C6B_b / U11 C2A_a -0.945 z C1B_b / U13 C1A_a -0.908 y C1B_b / U12 C1A_a -0.866 y C2B_b / U22 C6A_a -0.937 z C6B_b / z C2A_a -0.906 y C6B_b / y C2A_a -0.861 x C2B_b / x C6A_a 0.935 U13 C1A_a / z C1A_a -0.898 x C1B_b / x C1A_a -0.857 y C3B_b / U22 C5A_a -0.935 z C4B_b / z C4A_a -0.892 y C4B_b / y C4A_a -0.856 y C5B_b / y C3A_a -0.933 x C3B_b / x C5A_a -0.890 y C4B_b / U22 C4A_a 0.854 U11 C1A_a / x C1A_a Idealized hydrogen atom generation before cycle 11 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H8A 0.4382 -0.1089 0.6088 137 0.980 0.000 C8 C7 H8A H8B 0.3878 0.0460 0.5840 137 0.980 0.000 C8 C7 H8A H8C 0.3940 -0.0747 0.5101 137 0.980 0.000 C8 C7 H8A H3A -0.1954 0.1516 0.7417 43 0.950 0.000 C3A_a C2A_a C4A_a H4A -0.3201 -0.0299 0.6791 43 0.950 0.000 C4A_a C5A_a C3A_a H5A -0.2264 -0.1944 0.5854 43 0.950 0.000 C5A_a C6A_a C4A_a H6A -0.0110 -0.1851 0.5527 43 0.950 0.000 C6A_a C5A_a C1A_a H3B -0.2235 -0.1758 0.5886 43 0.950 0.000 C3B_b C4B_b C2B_b H4B -0.3006 -0.0005 0.6908 43 0.950 0.000 C4B_b C5B_b C3B_b H5B -0.1640 0.1636 0.7465 43 0.950 0.000 C5B_b C6B_b C4B_b H6B 0.0421 0.1740 0.7104 43 0.950 0.000 C6B_b C5B_b C1B_b 2008lsh057 in Pbca ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C7 0.24428 -0.10002 0.59531 1.00000 0.02431 0.01490 0.02868 0.00004 0.00401 0.00083 0.02263 0.00205 0.00012 0.00012 0.00008 0.00000 0.00057 0.00052 0.00057 0.00043 0.00047 0.00045 0.00027 C8 0.37767 -0.05554 0.57257 1.00000 0.02387 0.02187 0.04742 -0.00029 0.00942 0.00019 0.03105 0.00238 0.00012 0.00013 0.00010 0.00000 0.00060 0.00060 0.00075 0.00056 0.00054 0.00047 0.00031 H8A 0.43819 -0.10893 0.60878 1.00000 0.04658 0.00000 0.00000 H8B 0.38776 0.04602 0.58404 1.00000 0.04658 0.00000 0.00000 H8C 0.39398 -0.07471 0.51007 1.00000 0.04658 0.00000 0.00000 N1 0.16140 0.00652 0.60908 1.00000 0.02029 0.01149 0.02844 -0.00048 0.00047 -0.00039 0.02007 0.00169 0.00009 0.00010 0.00007 0.00000 0.00048 0.00044 0.00053 0.00036 0.00038 0.00035 0.00024 O1 0.21366 -0.22552 0.59928 1.00000 0.02770 0.01256 0.07385 0.00165 0.00916 0.00198 0.03804 0.00176 0.00009 0.00009 0.00008 0.00000 0.00049 0.00044 0.00074 0.00042 0.00045 0.00034 0.00029 C1A_a 0.02777 -0.01035 0.62836 0.82227 0.01563 0.01565 0.02010 0.00269 -0.00022 -0.00006 0.01713 0.00745 0.00031 0.00068 0.00048 0.00250 0.00136 0.00098 0.00054 0.00060 0.00132 0.00117 0.00051 C2A_a -0.02988 0.08567 0.68417 0.82227 0.02142 0.01532 0.02583 -0.00032 -0.00013 -0.00163 0.02086 0.00508 0.00023 0.00038 0.00027 0.00250 0.00139 0.00116 0.00077 0.00075 0.00101 0.00086 0.00055 C3A_a -0.15841 0.08278 0.70386 0.82227 0.01865 0.02758 0.03038 0.00022 0.00726 0.00465 0.02554 0.00455 0.00017 0.00034 0.00022 0.00250 0.00118 0.00112 0.00084 0.00076 0.00105 0.00106 0.00055 H3A_a -0.19535 0.15161 0.74172 0.82227 0.03065 0.00250 0.00000 C4A_a -0.23171 -0.02405 0.66646 0.82227 0.01826 0.03475 0.03503 0.00307 0.00199 -0.00289 0.02935 0.00484 0.00028 0.00043 0.00032 0.00250 0.00118 0.00172 0.00114 0.00100 0.00099 0.00087 0.00060 H4A_a -0.32007 -0.02988 0.67907 0.82227 0.03521 0.00250 0.00000 C5A_a -0.17547 -0.12190 0.61078 0.82227 0.02712 0.02893 0.03197 -0.00029 -0.00315 -0.00874 0.02934 0.00737 0.00043 0.00051 0.00044 0.00250 0.00089 0.00153 0.00085 0.00103 0.00073 0.00086 0.00055 H5A_a -0.22637 -0.19441 0.58544 0.82227 0.03520 0.00250 0.00000 C6A_a -0.04763 -0.11692 0.59115 0.82227 0.02411 0.01623 0.02384 -0.00279 -0.00076 -0.00536 0.02139 0.00496 0.00029 0.00026 0.00024 0.00250 0.00094 0.00130 0.00071 0.00092 0.00067 0.00082 0.00053 H6A_a -0.01100 -0.18514 0.55273 0.82227 0.02567 0.00250 0.00000 F1A_a 0.04482 0.19043 0.71963 0.82227 0.03188 0.02396 0.04076 -0.01501 0.00221 -0.00098 0.03220 0.00150 0.00009 0.00009 0.00006 0.00250 0.00053 0.00049 0.00056 0.00039 0.00039 0.00037 0.00031 C1B_b 0.04662 -0.00268 0.62918 0.17773 0.01563 0.01565 0.02010 0.00269 -0.00022 -0.00006 0.01713 0.03935 0.00188 0.00347 0.00242 0.00250 0.00136 0.00098 0.00054 0.00060 0.00132 0.00117 0.00051 C2B_b -0.03658 -0.09207 0.59322 0.17773 0.02142 0.01532 0.02583 -0.00032 -0.00013 -0.00163 0.02086 0.03030 0.00160 0.00167 0.00130 0.00250 0.00139 0.00116 0.00077 0.00075 0.00101 0.00086 0.00055 C3B_b -0.17019 -0.10494 0.61335 0.17773 0.01826 0.03475 0.03503 0.00307 0.00199 -0.00289 0.02935 0.03986 0.00196 0.00280 0.00217 0.00250 0.00118 0.00172 0.00114 0.00100 0.00099 0.00087 0.00060 H3B_b -0.22349 -0.17579 0.58856 0.17773 0.03521 0.00250 0.00000 C4B_b -0.21376 -0.00189 0.67344 0.17773 0.01826 0.03475 0.03503 0.00307 0.00199 -0.00289 0.02935 0.03274 0.00169 0.00247 0.00173 0.00250 0.00118 0.00172 0.00114 0.00100 0.00099 0.00087 0.00060 H4B_b -0.30059 -0.00048 0.69077 0.17773 0.03521 0.00250 0.00000 C5B_b -0.13163 0.09513 0.70645 0.17773 0.02712 0.02893 0.03197 -0.00029 -0.00315 -0.00874 0.02934 0.02910 0.00147 0.00213 0.00133 0.00250 0.00089 0.00153 0.00085 0.00103 0.00073 0.00086 0.00055 H5B_b -0.16399 0.16359 0.74651 0.17773 0.03520 0.00250 0.00000 C6B_b -0.00925 0.10066 0.68647 0.17773 0.02411 0.01623 0.02384 -0.00279 -0.00076 -0.00536 0.02139 0.03109 0.00160 0.00219 0.00147 0.00250 0.00094 0.00130 0.00071 0.00092 0.00067 0.00082 0.00053 H6B_b 0.04215 0.17398 0.71038 0.17773 0.02567 0.00250 0.00000 F1B_b 0.00353 -0.18822 0.52906 0.17773 0.03805 0.02391 0.03019 -0.00722 -0.00036 -0.00446 0.03072 0.00691 0.00043 0.00042 0.00026 0.00250 0.00246 0.00216 0.00226 0.00166 0.00178 0.00176 0.00130 H1N 0.19155 0.09312 0.60678 1.00000 0.03369 0.02398 0.00143 0.00143 0.00097 0.00000 0.00405 Final Structure Factor Calculation for 2008lsh057 in Pbca Total number of l.s. parameters = 133 Maximum vector length = 511 Memory required = 2122 / 24017 wR2 = 0.1056 before cycle 11 for 1716 data and 0 / 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. 15. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.003 0.000 0.037 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.036; Restrained GooF = 1.041 for 16 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0538 * P )^2 + 0.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0394 for 1482 Fo > 4sig(Fo) and 0.0474 for all 1716 data wR2 = 0.1056, GooF = S = 1.036, Restrained GooF = 1.041 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 0.0311 0.0220 0.0148 C7 0.0507 0.0219 0.0205 C8 0.0285 0.0203 0.0115 N1 0.0757 0.0261 0.0123 O1 0.0214 0.0156 0.0144 C1A_a 0.0258 0.0218 0.0149 C2A_a 0.0346 0.0281 0.0139 C3A_a 0.0380 0.0327 0.0174 C4A_a 0.0375 0.0318 0.0187 C5A_a 0.0270 0.0244 0.0128 C6A_a 0.0499 0.0316 0.0152 F1A_a 0.0214 0.0156 0.0144 C1B_b 0.0258 0.0218 0.0149 C2B_b 0.0380 0.0327 0.0174 C3B_b 0.0380 0.0327 0.0174 C4B_b 0.0375 0.0318 0.0187 C5B_b 0.0270 0.0244 0.0128 C6B_b 0.0397 0.0340 0.0184 F1B_b Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.014 0.026 0.038 0.052 0.068 0.088 0.110 0.148 0.215 1.000 Number in group 181. 170. 174. 171. 168. 169. 168. 174. 168. 173. GooF 1.144 0.970 1.006 1.062 1.004 1.084 1.003 1.048 0.986 1.033 K 1.936 1.036 0.986 0.975 0.976 0.982 1.009 1.006 1.008 0.994 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.63 inf Number in group 173. 172. 170. 174. 169. 172. 175. 168. 170. 173. GooF 0.955 0.956 0.899 0.965 0.894 0.901 1.070 0.944 1.338 1.312 K 0.973 1.031 0.997 0.997 1.021 1.008 1.015 1.016 1.028 0.976 R1 0.112 0.093 0.070 0.063 0.044 0.040 0.036 0.030 0.043 0.034 Recommended weighting scheme: WGHT 0.0536 0.5457 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 4 6 8.10 0.10 5.82 0.003 1.55 2 2 0 100.41 152.82 4.63 0.120 3.51 0 4 0 398.20 304.74 3.99 0.169 2.36 10 0 4 50.75 77.96 3.48 0.086 1.01 3 5 8 118.41 87.18 3.38 0.090 1.25 1 6 13 9.87 21.65 3.32 0.045 0.93 5 1 7 14.18 26.06 3.19 0.049 1.49 4 5 0 5.28 0.62 3.16 0.008 1.53 5 3 3 193.33 150.93 3.16 0.119 1.65 3 5 4 3.24 0.02 3.09 0.001 1.52 0 6 5 61.75 42.56 3.03 0.063 1.40 3 5 6 5.33 1.23 2.99 0.011 1.39 4 0 18 39.82 16.96 2.91 0.040 0.80 2 5 5 4.41 0.37 2.90 0.006 1.53 6 2 0 762.05 638.99 2.85 0.245 1.64 4 6 8 9.25 3.54 2.85 0.018 1.10 3 6 13 38.16 54.19 2.67 0.071 0.91 0 4 18 27.53 72.64 2.63 0.083 0.79 1 1 11 12.40 6.30 2.61 0.024 1.35 6 6 5 115.58 91.34 2.61 0.093 1.09 2 10 10 14.32 27.24 2.61 0.051 0.79 6 5 5 3.37 0.05 2.60 0.002 1.18 1 3 3 138.74 171.61 2.57 0.127 2.59 2 1 0 769.63 902.92 2.55 0.291 4.59 3 7 14 52.31 74.51 2.53 0.084 0.82 11 5 6 34.63 21.48 2.53 0.045 0.81 7 8 2 39.37 54.75 2.53 0.072 0.92 9 6 11 26.99 14.47 2.52 0.037 0.78 6 4 0 14.55 7.57 2.50 0.027 1.41 3 10 9 22.94 11.30 2.49 0.033 0.80 12 3 3 6.23 1.07 2.47 0.010 0.83 9 5 10 8.33 1.39 2.46 0.011 0.83 3 7 15 65.44 86.92 2.46 0.090 0.79 11 7 2 11.62 3.45 2.45 0.018 0.78 9 1 3 28.39 40.55 2.44 0.062 1.13 3 4 3 1016.11 880.61 2.44 0.288 1.83 2 5 3 830.33 720.15 2.40 0.260 1.68 1 5 4 109.98 135.91 2.39 0.113 1.67 5 4 4 6.89 2.71 2.37 0.016 1.45 1 2 2 354.03 302.68 2.35 0.169 3.74 6 0 2 111.98 89.28 2.34 0.092 1.71 11 4 2 74.63 57.55 2.32 0.074 0.88 4 5 6 17.81 26.82 2.32 0.050 1.31 2 5 0 236.35 199.36 2.31 0.137 1.78 3 2 9 951.61 831.76 2.29 0.280 1.45 7 7 2 55.65 71.80 2.26 0.082 0.99 6 2 6 126.88 154.51 2.25 0.120 1.38 4 2 4 83.59 66.22 2.25 0.079 1.96 0 2 17 66.15 86.25 2.23 0.090 0.88 6 1 9 112.60 91.96 2.23 0.093 1.20 Bond lengths and angles C7 - Distance Angles O1 1.2291 (0.0014) N1 1.3469 (0.0014) 122.86 (0.11) C8 1.5040 (0.0017) 121.64 (0.11) 115.49 (0.10) C7 - O1 N1 C8 - Distance Angles C7 1.5040 (0.0017) 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 C1B_b 1.2476 (0.0198) C7 1.3469 (0.0014) 127.71 (1.52) C1A_a 1.4437 (0.0033) 3.37 (1.34) 125.35 (0.27) H1N 0.8775 (0.0129) 115.08 (1.76) 117.11 (1.03) 117.53 (1.05) N1 - C1B_b C7 C1A_a O1 - Distance Angles C7 1.2291 (0.0014) O1 - C1A_a - Distance Angles C2A_a 1.3803 (0.0041) C6A_a 1.3994 (0.0035) 118.06 (0.24) N1 1.4437 (0.0033) 118.62 (0.28) 123.28 (0.35) C1A_a - C2A_a C6A_a C2A_a - Distance Angles F1A_a 1.3725 (0.0028) C1A_a 1.3803 (0.0041) 117.52 (0.21) C3A_a 1.3841 (0.0025) 119.23 (0.27) 123.24 (0.23) C2A_a - F1A_a C1A_a C3A_a - Distance Angles C2A_a 1.3841 (0.0025) C4A_a 1.3901 (0.0031) 117.87 (0.27) H3A_a 0.9500 121.06 121.07 C3A_a - C2A_a C4A_a C4A_a - Distance Angles C5A_a 1.3840 (0.0038) C3A_a 1.3901 (0.0031) 119.74 (0.26) H4A_a 0.9500 120.13 120.13 C4A_a - C5A_a C3A_a C5A_a - Distance Angles C6A_a 1.3774 (0.0039) C4A_a 1.3840 (0.0038) 121.73 (0.28) H5A_a 0.9500 119.13 119.13 C5A_a - C6A_a C4A_a C6A_a - Distance Angles C5A_a 1.3774 (0.0039) C1A_a 1.3994 (0.0035) 119.35 (0.26) H6A_a 0.9500 120.33 120.33 C6A_a - C5A_a C1A_a F1A_a - Distance Angles C2A_a 1.3725 (0.0028) F1A_a - C1B_b - Distance Angles N1 1.2476 (0.0197) C2B_b 1.3321 (0.0168) 125.38 (1.97) C6B_b 1.4320 (0.0192) 119.84 (1.69) 114.24 (1.45) C1B_b - N1 C2B_b C2B_b - Distance Angles C1B_b 1.3321 (0.0168) F1B_b 1.3958 (0.0142) 119.93 (1.46) C3B_b 1.4426 (0.0166) 127.31 (1.48) 112.76 (1.36) C2B_b - C1B_b F1B_b C3B_b - Distance Angles C4B_b 1.4093 (0.0180) C2B_b 1.4426 (0.0166) 113.27 (1.52) H3B_b 0.9500 123.36 123.36 C3B_b - C4B_b C2B_b C4B_b - Distance Angles C5B_b 1.3545 (0.0149) C3B_b 1.4093 (0.0180) 119.89 (1.60) H4B_b 0.9500 120.05 120.05 C4B_b - C5B_b C3B_b C5B_b - Distance Angles C6B_b 1.3229 (0.0141) C4B_b 1.3545 (0.0149) 124.20 (1.74) H5B_b 0.9500 117.90 117.90 C5B_b - C6B_b C4B_b C6B_b - Distance Angles C5B_b 1.3229 (0.0140) C1B_b 1.4320 (0.0192) 120.73 (1.58) H6B_b 0.9500 119.64 119.64 C6B_b - C5B_b C1B_b F1B_b - Distance Angles C2B_b 1.3958 (0.0142) F1B_b - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.877(13) 1.984(13) 2.8540(13) 170.9(15) N1-H1N...O1_$1 FMAP and GRID set by program FMAP 2 2 14 GRID -2.273 24 -2 2.273 1 2 R1 = 0.0474 for 1716 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.24 at 0.5663 0.1385 0.4424 [ 0.83 A from H8A ] Deepest hole -0.22 at 0.8003 0.2340 0.4492 [ 0.75 A from O1 ] Mean = 0.00, Rms deviation from mean = 0.04 e/A^3, Highest memory used = 2395 / 20109 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4337 -0.1385 0.5576 1.00000 0.05 0.24 0.83 H8A 1.01 C8 1.03 H8C 1.85 H8B Q2 1 0.2273 -0.2029 0.6485 1.00000 0.05 0.22 0.79 O1 1.27 C7 2.14 H5B 2.18 N1 Q3 1 0.3116 -0.0719 0.5844 1.00000 0.05 0.21 0.73 C8 0.77 C7 1.37 H8B 1.42 H8C Q4 1 0.0057 0.0573 0.6385 1.00000 0.05 0.18 0.70 C1A 0.73 C1B 0.83 C2A 0.85 C6B Q5 1 0.0135 0.0203 0.6717 1.00000 0.05 0.17 0.73 C1A 0.76 C1B 0.79 C2A 0.83 C6B Shortest distances between peaks (including symmetry equivalents) 4 5 0.62 1 3 1.49 2 3 1.80 1 2 2.64 Time profile in seconds ----------------------- 0.06: 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. 0.70: 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 1.08: Structure factors and derivatives 0.64: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.06: Apply other restraints 0.16: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + shelxl finished at 19:31:39 Total CPU time: 2.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++