+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 14:45:08 on 23-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh175 in Cc CELL 0.71073 4.4884 22.1684 9.5284 90.000 90.048 90.000 ZERR 4.00 0.0005 0.0027 0.0013 0.000 0.007 0.000 LATT -7 SYMM X, - Y, 1/2 + Z SFAC C H N O F UNIT 36 32 4 8 12 V = 948.08 F(000) = 448.0 Mu = 0.15 mm-1 Cell Wt = 876.66 Rho = 1.535 MERG 2 OMIT -3.00 55.00 TWIN BASF 0.47352 DFIX 1.4 0.02 N1A C7A EXYZ N1A N1B EADP N1A N1B EQIV $1 x, -y, z+1/2 EQIV $2 x, -y, z-1/2 HTAB N1A O1A_$1 HTAB N1B O1B_$2 FMAP 2 PLAN 5 SIZE 0.04 0.04 0.48 ACTA BOND $H WGHT 0.0088 0.9061 L.S. 18 TEMP -153.00 FVAR 0.96286 0.50889 C1 1 -0.225023 0.089127 0.601904 11.00000 0.02707 0.02887 = 0.02545 0.00022 0.00030 0.00427 C2 1 -0.128913 0.114206 0.476876 11.00000 0.04349 0.04619 = 0.02011 -0.00710 0.00421 -0.00714 AFIX 43 H2 2 -0.193399 0.097408 0.390304 11.00000 -1.20000 AFIX 0 C3 1 0.059883 0.163431 0.476707 11.00000 0.04482 0.04256 = 0.02493 -0.00141 0.00799 -0.00393 AFIX 43 H3 2 0.126051 0.180340 0.390585 11.00000 -1.20000 AFIX 0 C4 1 0.150138 0.187459 0.601094 11.00000 0.02670 0.03364 = 0.03396 0.00175 0.00032 0.00102 C5 1 0.060425 0.163899 0.727328 11.00000 0.04059 0.04238 = 0.03435 -0.00688 -0.00906 -0.00647 AFIX 43 H5 2 0.126071 0.181238 0.813126 11.00000 -1.20000 AFIX 0 C6 1 -0.127967 0.114276 0.727332 11.00000 0.04495 0.04513 = 0.02457 0.00480 -0.00774 -0.00983 AFIX 43 H6 2 -0.191131 0.097353 0.813937 11.00000 -1.20000 AFIX 0 PART 1 C7A 1 -0.529289 0.005278 0.498093 21.00000 0.03748 0.02897 = 0.02549 -0.00589 -0.00708 0.00395 C8A 1 -0.732183 -0.045504 0.545914 21.00000 0.03864 0.03440 = 0.04000 0.00013 -0.00334 -0.00953 AFIX 137 H8A1 2 -0.937777 -0.036512 0.518240 21.00000 -1.50000 H8A2 2 -0.720922 -0.049392 0.648233 21.00000 -1.50000 H8A3 2 -0.668818 -0.083388 0.502137 21.00000 -1.50000 AFIX 0 N1A 3 -0.419676 0.039544 0.602611 21.00000 0.03213 0.03312 = 0.02171 0.00072 -0.00005 -0.00166 AFIX 43 H1A 2 -0.481181 0.028953 0.686747 21.00000 -1.20000 AFIX 0 O1A 4 -0.464153 0.013065 0.376094 21.00000 0.05680 0.03991 = 0.01956 -0.00823 0.00103 -0.00281 PART 2 SAME C7A > O1A C7B 1 -0.527341 0.005257 0.705840 -21.00000 0.03321 0.03124 = 0.02442 0.00990 0.00021 0.00608 C8B 1 -0.736801 -0.045374 0.658627 -21.00000 0.04747 0.03968 = 0.03366 0.00451 0.00073 -0.01010 AFIX 137 H8B1 2 -0.669504 -0.083763 0.698604 -21.00000 -1.50000 H8B2 2 -0.735486 -0.048048 0.555967 -21.00000 -1.50000 H8B3 2 -0.939451 -0.036710 0.691096 -21.00000 -1.50000 AFIX 0 N1B 3 -0.419676 0.039544 0.602611 -21.00000 0.03213 0.03312 = 0.02171 0.00072 -0.00005 -0.00166 AFIX 43 H1B 2 -0.482935 0.029050 0.518649 -21.00000 -1.20000 AFIX 0 O1B 4 -0.466756 0.013924 0.828838 -21.00000 0.05643 0.03849 = 0.02168 0.01213 -0.00448 -0.00024 PART 0 C9 1 0.221969 0.291957 0.600944 11.00000 0.03031 0.04150 = 0.03547 -0.00188 -0.00386 -0.00321 O2 4 0.349959 0.237488 0.602062 11.00000 0.02451 0.03524 = 0.04943 0.00003 -0.00262 -0.00455 F1 5 0.050942 0.301121 0.714144 11.00000 0.05005 0.05118 = 0.05769 -0.01167 0.01573 -0.00345 F2 5 0.433730 0.332983 0.601697 11.00000 0.04110 0.03988 = 0.07872 0.00039 -0.00239 -0.01272 F3 5 0.050623 0.301076 0.490209 11.00000 0.05144 0.04742 = 0.05827 0.01281 -0.01932 -0.00373 HKLF 4 Covalent radii and connectivity table for 2008lsh175 in Cc C 0.770 H 0.320 N 0.700 O 0.660 F 0.640 C1 - C2 C6 N1B_b N1A_a C2 - C3 C1 C3 - C4 C2 C4 - C3 C5 O2 C5 - C4 C6 C6 - C5 C1 C7A_a - O1A_a N1A_a C8A_a C8A_a - C7A_a N1A_a - C7A_a C1 O1A_a - C7A_a C7B_b - O1B_b N1B_b C8B_b C8B_b - C7B_b N1B_b - C7B_b C1 O1B_b - C7B_b C9 - F2 F3 O2 F1 O2 - C9 C4 F1 - C9 F2 - C9 F3 - C9 Operators for generating equivalent atoms: $1 x, -y, z+1/2 $2 x, -y, z-1/2 Floating origin restraints generated 3001 Reflections read, of which 46 rejected -5 =< h =< 5, -28 =< k =< 28, -10 =< l =< 12, Max. 2-theta = 54.93 0 Systematic absence violations 0 Inconsistent equivalents 1681 Unique reflections, of which 0 suppressed R(int) = 0.0488 R(sigma) = 0.0721 Friedel opposites not merged Maximum memory for data reduction = 1794 / 20538 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 = 2261 / 209053 wR2 = 0.1212 before cycle 1 for 1681 data and 167 / 167 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. 6. 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 0.055 0.000 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.144; Restrained GooF = 1.144 for 9 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0088 * P )^2 + 0.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96257 0.00291 -0.100 OSF 2 0.50893 0.01098 0.004 FVAR 2 3 0.47856 1.44276 0.003 BASF 1 Mean shift/esd = 0.012 Maximum = -0.100 for OSF Max. shift = 0.001 A for H8A1_a Max. dU = 0.000 for C8B_b Least-squares cycle 2 Maximum vector length = 511 Memory required = 2261 / 209053 wR2 = 0.1212 before cycle 2 for 1681 data and 167 / 167 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. 6. 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 0.055 0.000 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.144; Restrained GooF = 1.144 for 9 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0088 * P )^2 + 0.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96247 0.00291 -0.033 OSF 2 0.50892 0.01098 -0.001 FVAR 2 3 0.48121 1.44241 0.002 BASF 1 Mean shift/esd = 0.004 Maximum = -0.033 for OSF Max. shift = 0.001 A for H8A2_a Max. dU = 0.000 for O2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2261 / 209053 wR2 = 0.1211 before cycle 3 for 1681 data and 167 / 167 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. 6. 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 0.055 0.000 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.144; Restrained GooF = 1.144 for 9 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0088 * P )^2 + 0.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96247 0.00291 0.000 OSF 2 0.50890 0.01098 -0.002 FVAR 2 3 0.48138 1.44224 0.000 BASF 1 Mean shift/esd = 0.001 Maximum = 0.007 for tors H8A1_a Max. shift = 0.001 A for H8B2_b Max. dU = 0.000 for C8B_b Least-squares cycle 4 Maximum vector length = 511 Memory required = 2261 / 209053 wR2 = 0.1212 before cycle 4 for 1681 data and 167 / 167 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. 6. 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 0.055 0.000 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.144; Restrained GooF = 1.144 for 9 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0088 * P )^2 + 0.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96247 0.00291 0.000 OSF 2 0.50890 0.01098 0.000 FVAR 2 3 0.48136 1.44236 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.005 for tors H8B1_b Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C8B_b Least-squares cycle 5 Maximum vector length = 511 Memory required = 2261 / 209053 wR2 = 0.1212 before cycle 5 for 1681 data and 167 / 167 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. 6. 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 0.055 0.000 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.144; Restrained GooF = 1.144 for 9 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0088 * P )^2 + 0.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96247 0.00291 0.000 OSF 2 0.50890 0.01098 0.000 FVAR 2 3 0.48132 1.44236 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.004 for tors H8B1_b Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C8B_b Least-squares cycle 6 Maximum vector length = 511 Memory required = 2261 / 209053 wR2 = 0.1212 before cycle 6 for 1681 data and 167 / 167 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. 6. 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 0.055 0.000 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.144; Restrained GooF = 1.144 for 9 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0088 * P )^2 + 0.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96247 0.00291 0.000 OSF 2 0.50890 0.01098 0.000 FVAR 2 3 0.48118 1.44240 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.003 for tors H8B1_b Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C8B_b Least-squares cycle 7 Maximum vector length = 511 Memory required = 2261 / 209053 wR2 = 0.1211 before cycle 7 for 1681 data and 167 / 167 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. 6. 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 0.055 0.000 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.144; Restrained GooF = 1.144 for 9 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0088 * P )^2 + 0.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96247 0.00291 0.000 OSF 2 0.50890 0.01098 0.000 FVAR 2 3 0.48124 1.44228 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.002 for tors H8B1_b Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C8B_b Least-squares cycle 8 Maximum vector length = 511 Memory required = 2261 / 209053 wR2 = 0.1211 before cycle 8 for 1681 data and 167 / 167 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. 6. 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 0.055 0.000 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.144; Restrained GooF = 1.144 for 9 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0088 * P )^2 + 0.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96248 0.00291 0.000 OSF 2 0.50890 0.01098 0.000 FVAR 2 3 0.48137 1.44226 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.002 for tors H8B1_b Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C8B_b Least-squares cycle 9 Maximum vector length = 511 Memory required = 2261 / 209053 wR2 = 0.1211 before cycle 9 for 1681 data and 167 / 167 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. 6. 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 0.055 0.000 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.144; Restrained GooF = 1.144 for 9 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0088 * P )^2 + 0.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96248 0.00291 0.000 OSF 2 0.50889 0.01098 0.000 FVAR 2 3 0.48136 1.44222 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.001 for tors H8B1_b Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C8B_b Least-squares cycle 10 Maximum vector length = 511 Memory required = 2261 / 209053 wR2 = 0.1211 before cycle 10 for 1681 data and 167 / 167 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. 6. 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 0.055 0.000 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.144; Restrained GooF = 1.144 for 9 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0088 * P )^2 + 0.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96248 0.00291 0.000 OSF 2 0.50889 0.01098 0.000 FVAR 2 3 0.48135 1.44219 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.001 for tors H8B1_b Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C8B_b Least-squares cycle 11 Maximum vector length = 511 Memory required = 2261 / 209053 wR2 = 0.1211 before cycle 11 for 1681 data and 167 / 167 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. 6. 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 0.055 0.000 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.144; Restrained GooF = 1.144 for 9 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0088 * P )^2 + 0.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96247 0.00291 0.000 OSF 2 0.50889 0.01098 0.000 FVAR 2 3 0.48140 1.44218 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.001 for tors H8B1_b Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C8B_b Least-squares cycle 12 Maximum vector length = 511 Memory required = 2261 / 209053 wR2 = 0.1211 before cycle 12 for 1681 data and 167 / 167 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. 6. 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 0.055 0.000 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.144; Restrained GooF = 1.144 for 9 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0088 * P )^2 + 0.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96248 0.00291 0.000 OSF 2 0.50889 0.01098 0.000 FVAR 2 3 0.48133 1.44217 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for tors H8B1_b Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C8B_b Least-squares cycle 13 Maximum vector length = 511 Memory required = 2261 / 209053 wR2 = 0.1211 before cycle 13 for 1681 data and 167 / 167 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. 6. 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 0.055 0.000 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.144; Restrained GooF = 1.144 for 9 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0088 * P )^2 + 0.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96248 0.00291 0.000 OSF 2 0.50889 0.01098 0.000 FVAR 2 3 0.48128 1.44221 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for tors H8B1_b Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C8A_a Least-squares cycle 14 Maximum vector length = 511 Memory required = 2261 / 209053 wR2 = 0.1211 before cycle 14 for 1681 data and 167 / 167 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. 6. 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 0.055 0.000 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.144; Restrained GooF = 1.144 for 9 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0088 * P )^2 + 0.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96247 0.00291 0.000 OSF 2 0.50889 0.01098 0.000 FVAR 2 3 0.48135 1.44221 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for tors H8B1_b Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C8B_b Least-squares cycle 15 Maximum vector length = 511 Memory required = 2261 / 209053 wR2 = 0.1211 before cycle 15 for 1681 data and 167 / 167 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. 6. 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 0.055 0.000 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.144; Restrained GooF = 1.144 for 9 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0088 * P )^2 + 0.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96247 0.00291 0.000 OSF 2 0.50889 0.01098 0.000 FVAR 2 3 0.48140 1.44219 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for tors H8B1_b Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C8A_a Least-squares cycle 16 Maximum vector length = 511 Memory required = 2261 / 209053 wR2 = 0.1211 before cycle 16 for 1681 data and 167 / 167 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. 6. 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 0.055 0.000 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.144; Restrained GooF = 1.144 for 9 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0088 * P )^2 + 0.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96248 0.00291 0.000 OSF 2 0.50889 0.01098 0.000 FVAR 2 3 0.48143 1.44221 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C8B_b Least-squares cycle 17 Maximum vector length = 511 Memory required = 2261 / 209053 wR2 = 0.1211 before cycle 17 for 1681 data and 167 / 167 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. 6. 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 0.055 0.000 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.144; Restrained GooF = 1.144 for 9 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0088 * P )^2 + 0.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96247 0.00291 0.000 OSF 2 0.50889 0.01098 0.000 FVAR 2 3 0.48135 1.44223 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for y F2 Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C8A_a Least-squares cycle 18 Maximum vector length = 511 Memory required = 2261 / 209053 wR2 = 0.1211 before cycle 18 for 1681 data and 167 / 167 parameters Summary of restraints applied in cycle 18 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 6. 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 0.055 0.000 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.144; Restrained GooF = 1.144 for 9 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0088 * P )^2 + 0.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96247 0.00291 0.000 OSF 2 0.50889 0.01098 0.000 FVAR 2 3 0.48142 1.44220 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for y F2 Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C8A_a Largest correlation matrix elements -0.680 y O1B_b / y O1A_a -0.559 y O1B_b / z O1A_a 0.539 z O1B_b / y O1A_a 0.593 y O1B_b / U23 O1A_a -0.555 U23 O1B_b / y O1A_a 0.527 y O1B_b / FVAR 2 -0.575 U33 C8B_b / U33 C8A_a 0.543 U23 O1B_b / U23 O1A_a -0.524 y O1A_a / FVAR 2 Idealized hydrogen atom generation before cycle 19 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 -0.1934 0.0974 0.3903 43 0.950 0.000 C2 C3 C1 H3 0.1261 0.1803 0.3906 43 0.950 0.000 C3 C4 C2 H5 0.1260 0.1812 0.8131 43 0.950 0.000 C5 C4 C6 H6 -0.1911 0.0973 0.8139 43 0.950 0.000 C6 C5 C1 H8A1 -0.9377 -0.0366 0.5180 137 0.980 0.000 C8A_a C7A_a H8A1_a H8A2 -0.7215 -0.0493 0.6483 137 0.980 0.000 C8A_a C7A_a H8A1_a H8A3 -0.6685 -0.0834 0.5024 137 0.980 0.000 C8A_a C7A_a H8A1_a H1A -0.4811 0.0289 0.6867 43 0.880 0.000 N1A_a C7A_a C1 H8B1 -0.6698 -0.0838 0.6988 137 0.980 0.000 C8B_b C7B_b H8B1_b H8B2 -0.7351 -0.0481 0.5560 137 0.980 0.000 C8B_b C7B_b H8B1_b H8B3 -0.9396 -0.0367 0.6909 137 0.980 0.000 C8B_b C7B_b H8B1_b H1B -0.4829 0.0290 0.5186 43 0.880 0.000 N1B_b C7B_b C1 2008lsh175 in Cc ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.22504 0.08913 0.60191 1.00000 0.02703 0.02883 0.02540 0.00020 0.00030 0.00425 0.02709 0.00607 0.00070 0.00013 0.00040 0.00000 0.00149 0.00138 0.00176 0.00149 0.00132 0.00133 0.00067 C2 -0.12890 0.11421 0.47687 1.00000 0.04343 0.04615 0.02012 -0.00711 0.00422 -0.00716 0.03656 0.00647 0.00078 0.00018 0.00039 0.00000 0.00201 0.00218 0.00200 0.00166 0.00154 0.00183 0.00086 H2 -0.19337 0.09740 0.39030 1.00000 0.04388 0.00000 0.00000 C3 0.05989 0.16343 0.47671 1.00000 0.04478 0.04250 0.02493 -0.00141 0.00801 -0.00393 0.03740 0.00695 0.00082 0.00018 0.00042 0.00000 0.00218 0.00215 0.00238 0.00176 0.00165 0.00169 0.00092 H3 0.12606 0.18034 0.39059 1.00000 0.04488 0.00000 0.00000 C4 0.15015 0.18746 0.60107 1.00000 0.02667 0.03360 0.03398 0.00173 0.00033 0.00101 0.03142 0.00631 0.00071 0.00014 0.00044 0.00000 0.00154 0.00169 0.00207 0.00160 0.00154 0.00133 0.00077 C5 0.06042 0.16390 0.72734 1.00000 0.04057 0.04233 0.03428 -0.00688 -0.00902 -0.00649 0.03906 0.00654 0.00080 0.00018 0.00045 0.00000 0.00211 0.00217 0.00266 0.00185 0.00169 0.00165 0.00097 H5 0.12604 0.18124 0.81314 1.00000 0.04688 0.00000 0.00000 C6 -0.12795 0.11427 0.72732 1.00000 0.04493 0.04508 0.02455 0.00480 -0.00775 -0.00983 0.03819 0.00621 0.00078 0.00018 0.00040 0.00000 0.00210 0.00218 0.00212 0.00171 0.00161 0.00180 0.00089 H6 -0.19107 0.09734 0.81392 1.00000 0.04583 0.00000 0.00000 C7A_a -0.52929 0.00528 0.49809 0.50889 0.03743 0.02896 0.02554 -0.00592 -0.00710 0.00395 0.03065 0.01026 0.00140 0.00028 0.00069 0.01098 0.00396 0.00354 0.00480 0.00301 0.00297 0.00275 0.00207 C8A_a -0.73224 -0.04551 0.54592 0.50889 0.03863 0.03434 0.04002 0.00015 -0.00335 -0.00955 0.03766 0.01315 0.00181 0.00035 0.00094 0.01098 0.00406 0.00424 0.00653 0.00321 0.00362 0.00293 0.00234 H8A1_a -0.93773 -0.03658 0.51795 0.50889 0.05650 0.01098 0.00000 H8A2_a -0.72152 -0.04930 0.64827 0.50889 0.05650 0.01098 0.00000 H8A3_a -0.66846 -0.08342 0.50239 0.50889 0.05650 0.01098 0.00000 N1A_a -0.41967 0.03954 0.60261 0.50889 0.03210 0.03305 0.02166 0.00072 -0.00004 -0.00164 0.02894 0.00479 0.00057 0.00011 0.00034 0.01098 0.00148 0.00125 0.00147 0.00143 0.00119 0.00125 0.00060 H1A_a -0.48114 0.02894 0.68674 0.50889 0.03473 0.01098 0.00000 O1A_a -0.46416 0.01307 0.37609 0.50889 0.05680 0.03984 0.01954 -0.00823 0.00101 -0.00278 0.03873 0.01363 0.00128 0.00036 0.00072 0.01098 0.00377 0.00370 0.00382 0.00293 0.00263 0.00272 0.00178 C7B_b -0.52735 0.00526 0.70583 0.49111 0.03321 0.03117 0.02450 0.00986 0.00026 0.00611 0.02963 0.01240 0.00141 0.00030 0.00072 0.01098 0.00387 0.00386 0.00471 0.00310 0.00302 0.00284 0.00213 C8B_b -0.73681 -0.04539 0.65862 0.49111 0.04749 0.03966 0.03353 0.00453 0.00064 -0.01012 0.04023 0.01386 0.00203 0.00038 0.00098 0.01098 0.00479 0.00470 0.00645 0.00346 0.00381 0.00345 0.00247 H8B1_b -0.66982 -0.08375 0.69881 0.49111 0.06034 0.01098 0.00000 H8B2_b -0.73507 -0.04814 0.55597 0.49111 0.06034 0.01098 0.00000 H8B3_b -0.93957 -0.03667 0.69086 0.49111 0.06034 0.01098 0.00000 N1B_b -0.41967 0.03954 0.60261 0.49111 0.03210 0.03305 0.02166 0.00072 -0.00004 -0.00164 0.02894 0.00479 0.00057 0.00011 0.00034 0.01098 0.00148 0.00125 0.00147 0.00143 0.00119 0.00125 0.00060 H1B_b -0.48288 0.02904 0.51864 0.49111 0.03473 0.01098 0.00000 O1B_b -0.46675 0.01392 0.82883 0.49111 0.05639 0.03846 0.02158 0.01212 -0.00447 -0.00023 0.03881 0.01038 0.00135 0.00037 0.00073 0.01098 0.00383 0.00370 0.00387 0.00302 0.00266 0.00277 0.00184 C9 0.22196 0.29195 0.60092 1.00000 0.03029 0.04151 0.03547 -0.00192 -0.00387 -0.00320 0.03576 0.00663 0.00075 0.00016 0.00048 0.00000 0.00168 0.00187 0.00224 0.00189 0.00156 0.00152 0.00082 O2 0.34996 0.23748 0.60206 1.00000 0.02449 0.03516 0.04936 0.00001 -0.00258 -0.00453 0.03634 0.00433 0.00047 0.00009 0.00034 0.00000 0.00120 0.00117 0.00168 0.00126 0.00115 0.00098 0.00062 F1 0.05094 0.30112 0.71416 1.00000 0.05003 0.05112 0.05761 -0.01164 0.01576 -0.00345 0.05291 0.00446 0.00050 0.00011 0.00031 0.00000 0.00135 0.00147 0.00198 0.00124 0.00122 0.00109 0.00074 F2 0.43375 0.33298 0.60170 1.00000 0.04104 0.03987 0.07865 0.00039 -0.00236 -0.01273 0.05319 0.00443 0.00048 0.00009 0.00035 0.00000 0.00121 0.00103 0.00174 0.00141 0.00118 0.00097 0.00064 F3 0.05060 0.30108 0.49022 1.00000 0.05140 0.04738 0.05822 0.01278 -0.01928 -0.00372 0.05234 0.00429 0.00050 0.00011 0.00031 0.00000 0.00134 0.00138 0.00201 0.00118 0.00118 0.00106 0.00073 Final Structure Factor Calculation for 2008lsh175 in Cc Total number of l.s. parameters = 167 Maximum vector length = 511 Memory required = 2096 / 26068 wR2 = 0.1211 before cycle 19 for 1681 data and 2 / 167 parameters Summary of restraints applied in cycle 19 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 6. 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 0.055 0.000 0.011 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.144; Restrained GooF = 1.144 for 9 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0088 * P )^2 + 0.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0517 for 1386 Fo > 4sig(Fo) and 0.0707 for all 1681 data wR2 = 0.1211, GooF = S = 1.144, Restrained GooF = 1.144 for all data Occupancy sum of asymmetric unit = 15.00 for non-hydrogen and 8.00 for hydrogen atoms Principal mean square atomic displacements U 0.0323 0.0254 0.0236 C1 0.0540 0.0376 0.0181 C2 0.0499 0.0402 0.0221 C3 0.0356 0.0321 0.0265 C4 0.0481 0.0458 0.0232 C5 0.0573 0.0355 0.0218 C6 0.0435 0.0282 0.0202 C7A_a 0.0473 0.0393 0.0264 C8A_a 0.0343 0.0309 0.0216 N1A_a 0.0574 0.0422 0.0166 O1A_a 0.0416 0.0306 0.0167 C7B_b 0.0546 0.0371 0.0289 C8B_b 0.0343 0.0309 0.0216 N1B_b 0.0572 0.0444 0.0149 O1B_b 0.0425 0.0376 0.0272 C9 0.0497 0.0368 0.0226 O2 0.0753 0.0475 0.0359 F1 0.0789 0.0530 0.0277 F2 0.0792 0.0452 0.0326 F3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.026 0.039 0.052 0.067 0.086 0.109 0.134 0.183 0.257 1.000 Number in group 176. 163. 170. 171. 165. 173. 162. 166. 167. 168. GooF 1.468 1.254 1.236 1.146 1.140 0.935 1.028 0.968 1.065 1.089 K 2.353 1.063 0.908 0.993 0.939 1.001 1.015 1.006 1.022 0.997 Resolution(A) 0.77 0.81 0.85 0.89 0.95 1.02 1.10 1.23 1.42 1.80 inf Number in group 171. 167. 169. 165. 176. 160. 168. 168. 169. 168. GooF 1.298 1.371 1.287 1.114 1.112 1.032 1.028 0.922 1.073 1.123 K 1.073 0.996 1.003 1.003 1.010 1.013 1.021 1.024 1.028 0.982 R1 0.272 0.232 0.165 0.106 0.072 0.062 0.047 0.039 0.035 0.028 Recommended weighting scheme: WGHT 0.0052 0.9160 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 17 6 -11.47 21.80 3.62 0.047 0.84 0 8 9 62.92 124.94 3.53 0.111 0.99 3 1 7 22.02 61.91 3.50 0.078 1.01 -3 7 9 50.56 2.72 3.43 0.016 0.83 -2 26 -3 -1.41 19.68 3.34 0.044 0.77 -4 12 6 32.26 4.36 3.34 0.021 0.82 -4 16 5 34.39 5.77 3.23 0.024 0.79 2 6 2 358.34 282.46 3.12 0.167 1.78 -4 16 4 43.87 13.99 3.11 0.037 0.82 -5 9 4 26.76 1.78 3.04 0.013 0.80 3 5 10 41.66 12.88 3.01 0.036 0.79 -5 3 4 11.60 30.47 2.88 0.055 0.83 -5 7 4 -5.43 12.18 2.86 0.035 0.81 -4 6 8 23.17 1.51 2.75 0.012 0.80 -2 12 9 60.96 0.10 2.75 0.003 0.85 -3 11 -7 202.36 151.22 2.75 0.123 0.90 -1 1 1 4154.95 4710.85 2.72 0.684 4.00 -1 19 -8 26.33 50.63 2.71 0.071 0.82 0 24 4 33.96 1.78 2.71 0.013 0.86 -2 0 6 577.56 439.73 2.70 0.209 1.30 1 9 7 7.44 31.48 2.68 0.056 1.15 -4 8 8 23.08 3.03 2.67 0.017 0.78 -3 19 4 -3.94 18.93 2.61 0.043 0.86 -4 12 5 48.93 23.45 2.54 0.048 0.86 -2 2 -4 2060.66 2477.02 2.53 0.496 1.62 -2 20 -1 43.65 72.72 2.44 0.085 0.99 0 14 9 104.26 149.70 2.44 0.122 0.88 2 22 -2 38.88 7.67 2.42 0.028 0.90 1 1 -4 451.72 378.25 2.40 0.194 2.10 3 21 -3 -16.01 15.12 2.39 0.039 0.83 2 24 5 -1.58 22.05 2.38 0.047 0.78 1 5 3 258.71 324.90 2.38 0.180 2.24 -4 8 -4 367.74 288.54 2.37 0.169 0.95 1 23 -1 -12.24 13.85 2.37 0.037 0.94 2 16 3 27.59 50.93 2.37 0.071 1.11 -1 7 0 1710.66 1939.57 2.33 0.439 2.59 -1 11 9 -20.18 17.43 2.31 0.042 0.92 -2 20 -5 19.90 4.42 2.27 0.021 0.88 2 4 8 55.46 84.65 2.24 0.092 1.03 -5 9 3 17.07 1.22 2.23 0.011 0.82 -1 23 -1 -6.41 14.02 2.23 0.037 0.94 -2 6 4 12.65 27.21 2.21 0.052 1.49 -4 14 -6 0.32 13.74 2.21 0.037 0.79 -1 1 4 444.53 378.27 2.21 0.194 2.10 3 17 2 19.98 44.02 2.20 0.066 0.96 0 26 3 32.05 6.74 2.20 0.026 0.82 -1 19 5 21.80 39.66 2.19 0.063 0.97 0 6 -5 3053.40 2736.04 2.18 0.521 1.69 -1 19 -7 63.93 41.26 2.18 0.064 0.87 1 3 8 303.58 366.16 2.16 0.191 1.14 Bond lengths and angles C1 - Distance Angles C2 1.3841 (0.0050) C6 1.3883 (0.0052) 118.80 (0.31) N1A_a 1.4042 (0.0042) 120.86 (0.35) 120.34 (0.34) C1 - C2 C6 C2 - Distance Angles C3 1.3817 (0.0057) C1 1.3841 (0.0050) 120.65 (0.36) H2 0.9500 119.68 119.68 C2 - C3 C1 C3 - Distance Angles C4 1.3606 (0.0057) C2 1.3817 (0.0057) 119.37 (0.36) H3 0.9500 120.32 120.32 C3 - C4 C2 C4 - Distance Angles C3 1.3606 (0.0057) C5 1.3723 (0.0057) 121.81 (0.30) O2 1.4263 (0.0039) 119.79 (0.33) 118.37 (0.34) C4 - C3 C5 C5 - Distance Angles C4 1.3723 (0.0057) C6 1.3875 (0.0056) 118.75 (0.37) H5 0.9500 120.63 120.63 C5 - C4 C6 C6 - Distance Angles C5 1.3875 (0.0056) C1 1.3883 (0.0052) 120.61 (0.36) H6 0.9500 119.69 119.69 C6 - C5 C1 C7A_a - Distance Angles O1A_a 1.2113 (0.0082) N1A_a 1.3453 (0.0064) 122.79 (0.67) C8A_a 1.5185 (0.0086) 122.61 (0.64) 114.56 (0.59) C7A_a - O1A_a N1A_a C8A_a - Distance Angles C7A_a 1.5185 (0.0086) H8A1_a 0.9800 109.47 H8A2_a 0.9800 109.47 109.47 H8A3_a 0.9800 109.47 109.47 109.47 C8A_a - C7A_a H8A1_a H8A2_a N1A_a - Distance Angles C7A_a 1.3453 (0.0065) C1 1.4042 (0.0042) 131.73 (0.42) H1A_a 0.8800 114.13 114.13 N1A_a - C7A_a C1 O1A_a - Distance Angles C7A_a 1.2113 (0.0082) O1A_a - C7B_b - Distance Angles O1B_b 1.2182 (0.0085) C8B_b 1.5317 (0.0090) 122.32 (0.64) C7B_b - O1B_b C8B_b - Distance Angles C7B_b 1.5317 (0.0090) H8B1_b 0.9800 109.47 H8B2_b 0.9800 109.47 109.47 H8B3_b 0.9800 109.47 109.47 109.47 C8B_b - C7B_b H8B1_b H8B2_b O1B_b - Distance Angles C7B_b 1.2182 (0.0085) O1B_b - C9 - Distance Angles F2 1.3156 (0.0039) F3 1.3205 (0.0050) 108.60 (0.33) O2 1.3373 (0.0041) 108.29 (0.28) 113.25 (0.33) F1 1.3402 (0.0051) 107.76 (0.33) 106.64 (0.28) 112.13 (0.34) C9 - F2 F3 O2 O2 - Distance Angles C9 1.3373 (0.0041) C4 1.4263 (0.0039) 115.59 (0.25) O2 - C9 F1 - Distance Angles C9 1.3402 (0.0051) F1 - F2 - Distance Angles C9 1.3156 (0.0039) F2 - F3 - Distance Angles C9 1.3205 (0.0051) F3 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 2.03 2.862(9) 156.9 N1A_a-H1A_a...O1A_$1a 0.88 2.05 2.873(9) 156.3 N1B_b-H1B_b...O1B_$2b FMAP and GRID set by program FMAP 2 1 13 GRID -5.000 -1 -2 5.000 1 2 R1 = 0.0748 for 1073 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.20 at 0.5038 0.2430 0.6576 [ 0.88 A from O2 ] Deepest hole -0.21 at 0.1550 0.2071 0.4570 [ 0.88 A from H3 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 2541 / 22690 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5038 0.2430 0.6576 1.00000 0.05 0.20 0.88 O2 1.75 C9 2.08 C4 2.09 F2 Q2 1 0.5980 0.2017 0.6044 1.00000 0.05 0.20 1.37 O2 2.04 C4 2.53 C5 2.55 C3 Q3 1 -0.3993 0.1318 0.6017 1.00000 0.05 0.19 1.23 C1 1.74 C2 1.75 C6 2.05 N1A Q4 1 -0.9531 -0.0178 0.6016 1.00000 0.05 0.17 0.90 H8A1 0.95 H8B3 1.27 H8B2 1.27 C8B Q5 1 -0.0022 0.1705 0.8810 1.00000 0.05 0.17 0.90 H5 1.50 C5 1.94 H6 2.00 C6 Shortest distances between peaks (including symmetry equivalents) 1 2 1.13 2 3 1.55 1 3 2.56 Time profile in seconds ----------------------- 0.11: 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. 0.16: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 2.38: Structure factors and derivatives 1.39: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.41: Solve l.s. equations 0.00: Generate HTAB table 0.08: 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 14:45:13 Total CPU time: 4.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++