+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 17:59:10 on 30-Mar-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh140 in P2(1)2(1)2 CELL 0.71073 9.5899 14.5337 4.6028 90.000 90.000 90.000 ZERR 2.00 0.0010 0.0014 0.0003 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, Z SYMM 1/2 - X, 1/2 + Y, - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N O UNIT 30 32 4 2 V = 641.52 F(000) = 256.0 Mu = 0.08 mm-1 Cell Wt = 480.60 Rho = 1.244 MERG 2 OMIT -3.00 55.00 EQIV $1 x, y, z+1 HTAB N1 O1_$1 DFIX 0.88 0.02 N1 H1N FMAP 2 PLAN 5 SIZE 0.06 0.06 0.26 ACTA HTAB BOND $H L.S. 10 TEMP -153.00 WGHT 0.0487 0.0965 EXTI 0.078391 FVAR 0.55910 C1 1 0.634857 0.142816 0.329676 11.00000 0.02484 0.02436 = 0.01966 0.00280 -0.00371 -0.00409 C2 1 0.607514 0.231142 0.431514 11.00000 0.02912 0.02382 = 0.03073 0.00120 -0.00304 -0.00164 AFIX 43 H2 2 0.537712 0.240094 0.575216 11.00000 -1.20000 AFIX 0 C3 1 0.681418 0.306833 0.325100 11.00000 0.03170 0.02727 = 0.03893 0.00788 -0.01238 -0.00632 C4 1 0.782812 0.292029 0.115343 11.00000 0.03905 0.04113 = 0.03750 0.01393 -0.00946 -0.01662 AFIX 43 H4 2 0.833974 0.342648 0.039911 11.00000 -1.20000 AFIX 0 C5 1 0.810079 0.203786 0.014823 11.00000 0.03106 0.05462 = 0.02998 0.00339 0.00245 -0.01184 AFIX 43 H5 2 0.879476 0.194687 -0.129635 11.00000 -1.20000 AFIX 0 C6 1 0.737362 0.128853 0.122539 11.00000 0.03153 0.03452 = 0.02677 0.00081 -0.00002 -0.00225 AFIX 43 H6 2 0.757599 0.068544 0.055032 11.00000 -1.20000 AFIX 0 C7 1 0.500000 0.000000 0.292943 10.50000 0.02562 0.01938 = 0.01935 0.00000 0.00000 0.00303 C8 1 0.648929 0.402146 0.435254 11.00000 0.05936 0.02322 = 0.07290 0.00297 -0.01254 -0.00752 AFIX 137 H8A 2 0.728802 0.442634 0.399271 11.00000 -1.50000 H8B 2 0.630046 0.399570 0.644344 11.00000 -1.50000 H8C 2 0.566821 0.426189 0.333749 11.00000 -1.50000 AFIX 0 N1 3 0.559601 0.068472 0.452241 11.00000 0.03402 0.02057 = 0.01424 0.00027 0.00161 -0.00573 O1 4 0.500000 0.000000 0.022748 10.50000 0.03909 0.02766 = 0.01552 0.00000 0.00000 -0.00717 H1N 2 0.543295 0.065083 0.637132 11.00000 0.03084 HKLF 4 1 0 1 0 0 0 -1 -1 0 0 Covalent radii and connectivity table for 2008lsh140 in P2(1)2(1)2 C 0.770 H 0.320 N 0.700 O 0.660 C1 - C6 C2 N1 C2 - C1 C3 C3 - C4 C2 C8 C4 - C3 C5 C5 - C6 C4 C6 - C1 C5 C7 - O1 N1 N1_$2 C8 - C3 N1 - C7 C1 O1 - C7 Operators for generating equivalent atoms: $1 x, y, z+1 $2 -x+1, -y, z 6289 Reflections read, of which 43 rejected -12 =< h =< 12, -18 =< k =< 16, -5 =< l =< 5, Max. 2-theta = 54.98 0 Systematic absence violations 0 Inconsistent equivalents 1458 Unique reflections, of which 0 suppressed R(int) = 0.0537 R(sigma) = 0.0532 Friedel opposites not merged Maximum memory for data reduction = 1191 / 14303 Special position constraints for C7 x = 0.5000 y = 0.0000 U23 = 0 U13 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for O1 x = 0.5000 y = 0.0000 U23 = 0 U13 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof 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 = 1448 / 118136 wR2 = 0.0974 before cycle 1 for 1458 data and 89 / 89 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 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.149; Restrained GooF = 0.149 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0487 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.76438 0.00574 210.037 OSF 2 0.07719 0.01103 -0.109 EXTI Mean shift/esd = 2.668 Maximum = 210.037 for OSF Max. shift = 0.017 A for H1N Max. dU = 0.000 for C6 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1448 / 118136 wR2 = 0.1140 before cycle 2 for 1458 data and 89 / 89 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 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.096; Restrained GooF = 1.096 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0487 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.76632 0.00679 0.286 OSF 2 0.07751 0.01324 0.024 EXTI Mean shift/esd = 0.127 Maximum = 0.445 for U33 N1 Max. shift = 0.008 A for H1N Max. dU = 0.000 for C6 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1448 / 118136 wR2 = 0.1138 before cycle 3 for 1458 data and 89 / 89 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 0.015 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.094; Restrained GooF = 1.094 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0487 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.76750 0.00678 0.174 OSF 2 0.07781 0.01322 0.023 EXTI Mean shift/esd = 0.122 Maximum = 0.448 for U33 N1 Max. shift = 0.007 A for H1N Max. dU = 0.000 for C6 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1448 / 118136 wR2 = 0.1137 before cycle 4 for 1458 data and 89 / 89 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 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.093; Restrained GooF = 1.093 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0487 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.76747 0.00678 -0.005 OSF 2 0.07780 0.01323 0.000 EXTI Mean shift/esd = 0.006 Maximum = -0.041 for tors H8A Max. shift = 0.001 A for H8C Max. dU = 0.000 for H1N Least-squares cycle 5 Maximum vector length = 511 Memory required = 1448 / 118136 wR2 = 0.1137 before cycle 5 for 1458 data and 89 / 89 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 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.093; Restrained GooF = 1.093 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0487 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.76740 0.00678 -0.010 OSF 2 0.07780 0.01323 -0.001 EXTI Mean shift/esd = 0.003 Maximum = -0.026 for tors H8A Max. shift = 0.000 A for H8C Max. dU = 0.000 for H1N Least-squares cycle 6 Maximum vector length = 511 Memory required = 1448 / 118136 wR2 = 0.1137 before cycle 6 for 1458 data and 89 / 89 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 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.093; Restrained GooF = 1.093 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0487 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.76740 0.00678 0.000 OSF 2 0.07779 0.01323 0.000 EXTI Mean shift/esd = 0.001 Maximum = -0.017 for tors H8A Max. shift = 0.000 A for H8C Max. dU = 0.000 for C8 Least-squares cycle 7 Maximum vector length = 511 Memory required = 1448 / 118136 wR2 = 0.1137 before cycle 7 for 1458 data and 89 / 89 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 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.093; Restrained GooF = 1.093 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0487 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.76739 0.00678 0.000 OSF 2 0.07779 0.01323 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.011 for tors H8A Max. shift = 0.000 A for H8C Max. dU = 0.000 for H1N Least-squares cycle 8 Maximum vector length = 511 Memory required = 1448 / 118136 wR2 = 0.1137 before cycle 8 for 1458 data and 89 / 89 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 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.093; Restrained GooF = 1.093 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0487 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.76740 0.00678 0.000 OSF 2 0.07779 0.01323 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.007 for tors H8A Max. shift = 0.000 A for H8C Max. dU = 0.000 for H1N Least-squares cycle 9 Maximum vector length = 511 Memory required = 1448 / 118136 wR2 = 0.1137 before cycle 9 for 1458 data and 89 / 89 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 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.093; Restrained GooF = 1.093 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0487 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.76740 0.00678 0.000 OSF 2 0.07779 0.01323 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.004 for tors H8A Max. shift = 0.000 A for H8C Max. dU = 0.000 for H1N Least-squares cycle 10 Maximum vector length = 511 Memory required = 1448 / 118136 wR2 = 0.1137 before cycle 10 for 1458 data and 89 / 89 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 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.093; Restrained GooF = 1.093 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0487 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.76739 0.00678 0.000 OSF 2 0.07779 0.01323 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.003 for tors H8A Max. shift = 0.000 A for H8C Max. dU = 0.000 for H1N Largest correlation matrix elements 0.536 EXTI / OSF Idealized hydrogen atom generation before cycle 11 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.5378 0.2401 0.5753 43 0.950 0.000 C2 C1 C3 H4 0.8339 0.3426 0.0399 43 0.950 0.000 C4 C3 C5 H5 0.8795 0.1947 -0.1296 43 0.950 0.000 C5 C6 C4 H6 0.7576 0.0685 0.0550 43 0.950 0.000 C6 C1 C5 H8A 0.7284 0.4428 0.3975 137 0.980 0.000 C8 C3 H8A H8B 0.6309 0.3997 0.6447 137 0.980 0.000 C8 C3 H8A H8C 0.5663 0.4259 0.3351 137 0.980 0.000 C8 C3 H8A 2008lsh140 in P2(1)2(1)2 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.63485 0.14283 0.32967 1.00000 0.02478 0.02437 0.01961 0.00289 -0.00373 -0.00403 0.02292 0.00298 0.00019 0.00012 0.00038 0.00000 0.00096 0.00088 0.00082 0.00068 0.00076 0.00073 0.00041 C2 0.60756 0.23114 0.43155 1.00000 0.02906 0.02391 0.03058 0.00120 -0.00307 -0.00163 0.02785 0.00322 0.00021 0.00012 0.00043 0.00000 0.00099 0.00092 0.00096 0.00071 0.00082 0.00073 0.00044 H2 0.53780 0.24009 0.57534 1.00000 0.03342 0.00000 0.00000 C3 0.68140 0.30681 0.32514 1.00000 0.03176 0.02724 0.03881 0.00782 -0.01241 -0.00633 0.03260 0.00335 0.00021 0.00013 0.00046 0.00000 0.00109 0.00102 0.00106 0.00086 0.00087 0.00082 0.00049 C4 0.78279 0.29202 0.11536 1.00000 0.03896 0.04094 0.03742 0.01382 -0.00942 -0.01653 0.03911 0.00336 0.00023 0.00015 0.00042 0.00000 0.00125 0.00123 0.00113 0.00092 0.00096 0.00098 0.00056 H4 0.83393 0.34265 0.03993 1.00000 0.04693 0.00000 0.00000 C5 0.81008 0.20380 0.01482 1.00000 0.03102 0.05467 0.02994 0.00342 0.00246 -0.01185 0.03855 0.00348 0.00021 0.00015 0.00047 0.00000 0.00105 0.00134 0.00103 0.00098 0.00088 0.00099 0.00052 H5 0.87949 0.19470 -0.12962 1.00000 0.04626 0.00000 0.00000 C6 0.73735 0.12886 0.12254 1.00000 0.03149 0.03436 0.02672 0.00083 0.00003 -0.00239 0.03086 0.00335 0.00021 0.00014 0.00040 0.00000 0.00110 0.00109 0.00099 0.00074 0.00079 0.00082 0.00048 H6 0.75758 0.06855 0.05503 1.00000 0.03703 0.00000 0.00000 C7 0.50000 0.00000 0.29293 0.50000 0.02572 0.01935 0.01937 0.00000 0.00000 0.00302 0.02148 0.00238 0.00000 0.00000 0.00052 0.00000 0.00130 0.00114 0.00113 0.00000 0.00000 0.00098 0.00053 C8 0.64892 0.40214 0.43523 1.00000 0.05937 0.02328 0.07300 0.00283 -0.01236 -0.00749 0.05188 0.00412 0.00027 0.00014 0.00065 0.00000 0.00156 0.00106 0.00181 0.00103 0.00138 0.00097 0.00070 H8A 0.72845 0.44276 0.39751 1.00000 0.07782 0.00000 0.00000 H8B 0.63094 0.39967 0.64468 1.00000 0.07782 0.00000 0.00000 H8C 0.56627 0.42594 0.33507 1.00000 0.07782 0.00000 0.00000 N1 0.55960 0.06848 0.45225 1.00000 0.03402 0.02045 0.01415 0.00020 0.00163 -0.00578 0.02287 0.00255 0.00016 0.00009 0.00032 0.00000 0.00085 0.00071 0.00069 0.00056 0.00065 0.00064 0.00037 O1 0.50000 0.00000 0.02278 0.50000 0.03909 0.02763 0.01539 0.00000 0.00000 -0.00714 0.02737 0.00162 0.00000 0.00000 0.00035 0.00000 0.00105 0.00089 0.00084 0.00000 0.00000 0.00079 0.00045 H1N 0.54347 0.06487 0.63731 1.00000 0.03113 0.03333 0.00218 0.00132 0.00345 0.00000 0.00536 Final Structure Factor Calculation for 2008lsh140 in P2(1)2(1)2 Total number of l.s. parameters = 89 Maximum vector length = 511 Memory required = 1361 / 25046 wR2 = 0.1137 before cycle 11 for 1458 data and 2 / 89 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 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.093; Restrained GooF = 1.093 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0487 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0465 for 1201 Fo > 4sig(Fo) and 0.0632 for all 1458 data wR2 = 0.1137, GooF = S = 1.093, Restrained GooF = 1.093 for all data Flack x parameter = 0.3719 with esd 2.3459 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 9.00 for non-hydrogen and 8.00 for hydrogen atoms Principal mean square atomic displacements U 0.0306 0.0206 0.0175 C1 0.0334 0.0267 0.0234 C2 0.0522 0.0233 0.0223 C3 0.0661 0.0288 0.0224 C4 0.0598 0.0320 0.0239 C5 0.0358 0.0302 0.0266 C6 0.0269 0.0194 0.0181 C7 0.0810 0.0529 0.0218 C8 0.0362 0.0185 0.0139 N1 0.0425 0.0242 0.0154 O1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.022 0.033 0.047 0.060 0.073 0.092 0.115 0.146 0.202 1.000 Number in group 147. 150. 146. 149. 140. 146. 142. 146. 147. 145. GooF 1.089 1.176 1.192 1.136 1.092 1.009 0.927 0.975 1.150 1.145 K 1.973 1.116 1.023 0.955 1.025 0.962 1.011 1.001 1.024 1.012 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.66 inf Number in group 149. 144. 146. 148. 145. 142. 148. 146. 143. 147. GooF 1.016 1.093 1.065 1.009 1.011 0.986 0.933 1.066 1.192 1.466 K 1.069 1.052 0.981 1.027 1.002 1.029 1.019 1.022 1.023 1.002 R1 0.164 0.200 0.119 0.087 0.066 0.046 0.038 0.035 0.039 0.032 Recommended weighting scheme: WGHT 0.0487 0.0941 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 1 3 64.46 44.75 4.02 0.112 1.53 3 1 1 66.43 91.66 3.95 0.160 2.58 0 2 2 10.30 5.73 3.76 0.040 2.19 0 1 2 1.06 4.27 3.65 0.035 2.27 0 2 1 161.02 203.84 3.65 0.239 3.89 3 2 3 8.90 4.45 3.51 0.035 1.36 6 0 1 14.63 22.07 3.45 0.079 1.51 12 3 0 77.34 56.43 3.09 0.126 0.79 1 8 0 149.02 123.26 3.00 0.186 1.78 -5 3 1 4.43 8.79 2.97 0.050 1.66 4 4 0 199.38 241.44 2.97 0.260 2.00 7 0 1 96.74 77.71 2.89 0.147 1.31 -3 1 1 73.11 91.55 2.85 0.160 2.58 2 6 0 13.78 9.39 2.80 0.051 2.16 2 8 5 5.12 13.40 2.79 0.061 0.81 1 2 1 355.27 425.18 2.75 0.345 3.60 -2 18 1 12.00 2.10 2.73 0.024 0.78 0 12 2 24.21 16.09 2.72 0.067 1.07 -11 2 1 8.36 2.52 2.69 0.027 0.85 -6 2 2 52.94 66.30 2.57 0.136 1.29 3 15 2 5.19 12.43 2.56 0.059 0.86 2 0 2 57.69 47.79 2.54 0.116 2.07 9 8 2 1.61 7.35 2.54 0.045 0.85 1 10 2 6.31 2.90 2.49 0.028 1.22 3 10 4 19.71 29.17 2.46 0.090 0.87 4 6 0 165.22 196.27 2.41 0.234 1.70 2 7 0 188.46 219.60 2.41 0.248 1.91 4 0 2 4.54 2.51 2.36 0.026 1.66 4 10 3 50.50 62.75 2.36 0.132 0.97 0 16 3 -4.07 2.71 2.33 0.028 0.78 7 7 4 10.87 0.27 2.32 0.009 0.81 0 7 2 59.26 49.74 2.31 0.118 1.54 -6 14 2 2.59 7.64 2.29 0.046 0.81 5 6 0 8.66 12.40 2.28 0.059 1.50 3 0 4 3.07 1.06 2.28 0.017 1.08 0 3 2 -0.18 0.91 2.28 0.016 2.08 9 3 2 5.65 1.44 2.26 0.020 0.95 -8 7 3 5.21 10.21 2.26 0.053 0.86 10 6 2 -2.01 2.41 2.26 0.026 0.83 2 15 3 11.31 0.85 2.25 0.015 0.81 7 0 3 2.75 0.15 2.25 0.006 1.02 3 6 1 23.51 18.44 2.23 0.072 1.78 1 15 2 11.37 4.86 2.21 0.037 0.89 7 12 0 -0.81 2.76 2.21 0.028 0.91 -4 16 1 6.99 0.79 2.19 0.015 0.84 -4 11 4 9.06 3.87 2.18 0.033 0.82 -6 5 1 105.89 89.82 2.17 0.158 1.34 2 2 2 98.23 84.46 2.16 0.154 2.00 3 4 5 2.45 5.93 2.16 0.041 0.86 -6 6 1 5.44 2.52 2.16 0.027 1.28 Bond lengths and angles C1 - Distance Angles C6 1.3843 (0.0026) C2 1.3913 (0.0024) 120.07 (0.17) N1 1.4167 (0.0022) 121.61 (0.16) 118.27 (0.16) C1 - C6 C2 C2 - Distance Angles C1 1.3913 (0.0024) C3 1.3967 (0.0026) 120.85 (0.18) H2 0.9500 119.58 119.58 C2 - C1 C3 C3 - Distance Angles C4 1.3871 (0.0031) C2 1.3967 (0.0026) 118.52 (0.18) C8 1.5077 (0.0028) 121.41 (0.19) 120.06 (0.19) C3 - C4 C2 C4 - Distance Angles C3 1.3871 (0.0031) C5 1.3881 (0.0029) 120.49 (0.19) H4 0.9500 119.75 119.75 C4 - C3 C5 C5 - Distance Angles C6 1.3851 (0.0027) C4 1.3881 (0.0029) 120.80 (0.20) H5 0.9500 119.60 119.60 C5 - C6 C4 C6 - Distance Angles C1 1.3843 (0.0026) C5 1.3851 (0.0027) 119.26 (0.18) H6 0.9500 120.37 120.37 C6 - C1 C5 C7 - Distance Angles O1 1.2434 (0.0030) N1 1.3620 (0.0018) 122.58 (0.10) N1_$2 1.3620 (0.0018) 122.58 (0.10) 114.85 (0.20) C7 - O1 N1 C8 - Distance Angles C3 1.5077 (0.0028) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - C3 H8A H8B N1 - Distance Angles C7 1.3620 (0.0018) C1 1.4167 (0.0022) 123.83 (0.15) H1N 0.8673 (0.0152) 114.19 (1.34) 121.88 (1.33) N1 - C7 C1 O1 - Distance Angles C7 1.2434 (0.0030) O1 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.867(15) 2.052(16) 2.866(2) 156.0(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)