+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 22:13:15 on 13-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh037 in P1 New: P-1 CELL 0.71073 5.7366 8.5492 10.6373 93.974 99.351 95.314 ZERR 2.00 0.0002 0.0005 0.0006 0.002 0.003 0.003 LATT 1 SFAC C H N O UNIT 22 26 2 6 V = 510.65 F(000) = 220.0 Mu = 0.10 mm-1 Cell Wt = 414.45 Rho = 1.348 MERG 2 OMIT -3.00 55.00 OMIT -2 3 0 OMIT -1 0 1 OMIT 0 -2 2 OMIT -1 1 2 EXTI 0.20030 DFIX 0.88 0.02 N1 H1N EQIV $1 -x+1, -y+1, -z HTAB N1 O2_$1 FMAP 2 PLAN 5 SIZE 0.20 0.50 0.60 ACTA HTAB 2.00000 BOND $H WGHT 0.0976 0.0965 L.S. 10 TEMP -153.00 FVAR 2.00651 C1 1 0.301394 0.534277 0.270919 11.00000 0.01989 0.01742 = 0.02032 0.00088 0.00513 0.00066 C2 1 0.281682 0.460875 0.147557 11.00000 0.01893 0.01882 = 0.01869 0.00013 0.00513 0.00048 AFIX 43 H2 2 0.401805 0.484804 0.097927 11.00000 -1.20000 AFIX 0 C3 1 0.086714 0.352863 0.097174 11.00000 0.02071 0.01728 = 0.01906 0.00035 0.00462 0.00162 C4 1 -0.091551 0.317672 0.169053 11.00000 0.02090 0.02021 = 0.02341 0.00000 0.00576 -0.00178 AFIX 43 H4 2 -0.225959 0.245226 0.134174 11.00000 -1.20000 AFIX 0 C5 1 -0.070329 0.389586 0.291890 11.00000 0.02269 0.02688 = 0.02253 0.00087 0.00999 -0.00345 AFIX 43 H5 2 -0.190835 0.365420 0.341229 11.00000 -1.20000 AFIX 0 C6 1 0.125329 0.496869 0.344060 11.00000 0.02628 0.02492 = 0.01853 0.00029 0.00720 -0.00155 AFIX 43 H6 2 0.138974 0.544261 0.428752 11.00000 -1.20000 AFIX 0 C7 1 0.543093 0.745054 0.424151 11.00000 0.02210 0.02349 = 0.02066 0.00013 0.00495 -0.00213 C8 1 0.776171 0.848434 0.446781 11.00000 0.02429 0.03050 = 0.02502 -0.00360 0.00475 -0.00498 AFIX 137 H8A 2 0.746214 0.959369 0.455162 11.00000 -1.50000 H8B 2 0.859282 0.830134 0.374434 11.00000 -1.50000 H8C 2 0.874493 0.822985 0.525454 11.00000 -1.50000 AFIX 0 C9 1 0.073193 0.272036 -0.032838 11.00000 0.01858 0.01805 = 0.02054 0.00131 0.00477 0.00053 C10 1 -0.154453 0.075680 -0.185384 11.00000 0.02587 0.02177 = 0.02017 -0.00356 0.00467 -0.00038 AFIX 23 H10A 2 -0.023560 0.008848 -0.189946 11.00000 -1.20000 H10B 2 -0.160384 0.146169 -0.255599 11.00000 -1.20000 AFIX 0 C11 1 -0.389068 -0.025632 -0.195719 11.00000 0.02511 0.02507 = 0.02897 -0.00255 0.00217 -0.00418 AFIX 137 H11A 2 -0.380100 -0.094734 -0.125711 11.00000 -1.50000 H11B 2 -0.422475 -0.089903 -0.277788 11.00000 -1.50000 H11C 2 -0.516351 0.042226 -0.190343 11.00000 -1.50000 AFIX 0 N1 3 0.503743 0.643072 0.316534 11.00000 0.01998 0.02384 = 0.01960 -0.00330 0.00688 -0.00234 O1 4 0.400426 0.756212 0.497694 11.00000 0.03367 0.03854 = 0.02640 -0.01227 0.01516 -0.01142 O2 4 0.218280 0.295541 -0.102642 11.00000 0.02553 0.02859 = 0.02095 -0.00205 0.00889 -0.00250 O3 4 -0.118799 0.166981 -0.062674 11.00000 0.02472 0.02452 = 0.02102 -0.00475 0.00594 -0.00690 H1N 2 0.608391 0.646498 0.265065 11.00000 0.03060 HKLF 4 Covalent radii and connectivity table for 2008lsh037 in P1 New: P-1 C 0.770 H 0.320 N 0.700 O 0.660 C1 - C2 C6 N1 C2 - C3 C1 C3 - C2 C4 C9 C4 - C5 C3 C5 - C4 C6 C6 - C5 C1 C7 - O1 N1 C8 C8 - C7 C9 - O2 O3 C3 C10 - O3 C11 C11 - C10 N1 - C7 C1 O1 - C7 O2 - C9 O3 - C9 C10 Operators for generating equivalent atoms: $1 -x+1, -y+1, -z 11955 Reflections read, of which 14 rejected -6 =< h =< 7, -11 =< k =< 11, -13 =< l =< 13, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 2337 Unique reflections, of which 0 suppressed R(int) = 0.0334 R(sigma) = 0.0270 Friedel opposites merged Maximum memory for data reduction = 1574 / 23384 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 = 1963 / 179723 wR2 = 0.1460 before cycle 1 for 2337 data and 143 / 143 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 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.040; Restrained GooF = 1.040 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0976 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.00921 0.00875 0.309 OSF 2 0.21079 0.03519 0.298 EXTI Mean shift/esd = 0.437 Maximum = -1.581 for U11 O2 Max. shift = 0.008 A for H1N Max. dU = 0.001 for H1N Least-squares cycle 2 Maximum vector length = 511 Memory required = 1963 / 179723 wR2 = 0.1443 before cycle 2 for 2337 data and 143 / 143 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 0.008 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.032; Restrained GooF = 1.032 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0976 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.00597 0.00865 -0.374 OSF 2 0.21007 0.03539 -0.020 EXTI Mean shift/esd = 0.166 Maximum = -0.605 for U11 O2 Max. shift = 0.003 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 3 Maximum vector length = 511 Memory required = 1963 / 179723 wR2 = 0.1442 before cycle 3 for 2337 data and 143 / 143 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.032; Restrained GooF = 1.031 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0976 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.00572 0.00863 -0.029 OSF 2 0.20859 0.03532 -0.042 EXTI Mean shift/esd = 0.013 Maximum = -0.042 for EXTI Max. shift = 0.000 A for H8B Max. dU = 0.000 for H1N Least-squares cycle 4 Maximum vector length = 511 Memory required = 1963 / 179723 wR2 = 0.1442 before cycle 4 for 2337 data and 143 / 143 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.032; Restrained GooF = 1.031 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0976 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.00572 0.00863 0.000 OSF 2 0.20870 0.03524 0.003 EXTI Mean shift/esd = 0.003 Maximum = -0.016 for tors H8A Max. shift = 0.000 A for H8B Max. dU = 0.000 for H1N Least-squares cycle 5 Maximum vector length = 511 Memory required = 1963 / 179723 wR2 = 0.1442 before cycle 5 for 2337 data and 143 / 143 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.032; Restrained GooF = 1.031 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0976 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.00575 0.00863 0.003 OSF 2 0.20882 0.03524 0.003 EXTI Mean shift/esd = 0.001 Maximum = -0.007 for tors H8A Max. shift = 0.000 A for H8B Max. dU = 0.000 for H1N Least-squares cycle 6 Maximum vector length = 511 Memory required = 1963 / 179723 wR2 = 0.1442 before cycle 6 for 2337 data and 143 / 143 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.032; Restrained GooF = 1.031 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0976 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.00575 0.00863 0.000 OSF 2 0.20881 0.03525 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 Least-squares cycle 7 Maximum vector length = 511 Memory required = 1963 / 179723 wR2 = 0.1442 before cycle 7 for 2337 data and 143 / 143 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.032; Restrained GooF = 1.031 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0976 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.00575 0.00863 0.000 OSF 2 0.20879 0.03525 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.002 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 = 1963 / 179723 wR2 = 0.1442 before cycle 8 for 2337 data and 143 / 143 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.032; Restrained GooF = 1.031 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0976 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.00575 0.00863 0.000 OSF 2 0.20880 0.03525 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for tors H8A Max. shift = 0.000 A for H8B Max. dU = 0.000 for C3 Least-squares cycle 9 Maximum vector length = 511 Memory required = 1963 / 179723 wR2 = 0.1442 before cycle 9 for 2337 data and 143 / 143 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.032; Restrained GooF = 1.031 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0976 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.00575 0.00863 0.000 OSF 2 0.20880 0.03525 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 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 = 1963 / 179723 wR2 = 0.1442 before cycle 10 for 2337 data and 143 / 143 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.032; Restrained GooF = 1.031 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0976 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.00575 0.00863 0.000 OSF 2 0.20880 0.03525 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y N1 Max. shift = 0.000 A for H8A Max. dU = 0.000 for C5 Largest correlation matrix elements 0.578 EXTI / OSF Idealized hydrogen atom generation before cycle 11 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.4019 0.4848 0.0977 43 0.950 0.000 C2 C3 C1 H4 -0.2261 0.2455 0.1343 43 0.950 0.000 C4 C5 C3 H5 -0.1906 0.3654 0.3415 43 0.950 0.000 C5 C4 C6 H6 0.1392 0.5444 0.4285 43 0.950 0.000 C6 C5 C1 H8A 0.7465 0.9593 0.4548 137 0.980 0.000 C8 C7 H8A H8B 0.8591 0.8297 0.3743 137 0.980 0.000 C8 C7 H8A H8C 0.8744 0.8230 0.5254 137 0.980 0.000 C8 C7 H8A H10A -0.0235 0.0090 -0.1901 23 0.990 0.000 C10 O3 C11 H10B -0.1604 0.1463 -0.2557 23 0.990 0.000 C10 O3 C11 H11A -0.3802 -0.0940 -0.1253 137 0.980 0.000 C11 C10 H11A H11B -0.4218 -0.0903 -0.2775 137 0.980 0.000 C11 C10 H11A H11C -0.5163 0.0424 -0.1909 137 0.980 0.000 C11 C10 H11A 2008lsh037 in P1 New: P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.30143 0.53429 0.27099 1.00000 0.01940 0.01746 0.01972 0.00083 0.00514 0.00054 0.01878 0.00239 0.00021 0.00014 0.00012 0.00000 0.00059 0.00058 0.00060 0.00044 0.00045 0.00045 0.00029 C2 0.28189 0.46086 0.14737 1.00000 0.01855 0.01854 0.01873 0.00067 0.00551 0.00068 0.01847 0.00236 0.00021 0.00014 0.00011 0.00000 0.00058 0.00059 0.00060 0.00045 0.00043 0.00044 0.00029 H2 0.40188 0.48477 0.09766 1.00000 0.02216 0.00000 0.00000 C3 0.08684 0.35294 0.09737 1.00000 0.02035 0.01750 0.01830 0.00039 0.00467 0.00173 0.01863 0.00232 0.00020 0.00014 0.00011 0.00000 0.00059 0.00059 0.00059 0.00044 0.00044 0.00045 0.00029 C4 -0.09156 0.31781 0.16920 1.00000 0.02066 0.01960 0.02306 0.00030 0.00600 -0.00186 0.02118 0.00241 0.00021 0.00015 0.00012 0.00000 0.00059 0.00060 0.00063 0.00046 0.00046 0.00044 0.00031 H4 -0.22606 0.24547 0.13426 1.00000 0.02542 0.00000 0.00000 C5 -0.07032 0.38958 0.29201 1.00000 0.02295 0.02614 0.02278 0.00113 0.01035 -0.00360 0.02367 0.00248 0.00022 0.00015 0.00012 0.00000 0.00061 0.00067 0.00064 0.00050 0.00048 0.00049 0.00031 H5 -0.19063 0.36540 0.34146 1.00000 0.02840 0.00000 0.00000 C6 0.12552 0.49688 0.34387 1.00000 0.02657 0.02449 0.01782 -0.00040 0.00732 -0.00123 0.02292 0.00244 0.00022 0.00015 0.00012 0.00000 0.00065 0.00065 0.00059 0.00047 0.00047 0.00050 0.00031 H6 0.13921 0.54437 0.42854 1.00000 0.02750 0.00000 0.00000 C7 0.54287 0.74523 0.42426 1.00000 0.02207 0.02300 0.02037 -0.00004 0.00481 -0.00191 0.02204 0.00241 0.00022 0.00015 0.00012 0.00000 0.00061 0.00064 0.00061 0.00047 0.00047 0.00047 0.00030 C8 0.77611 0.84830 0.44664 1.00000 0.02389 0.03007 0.02439 -0.00388 0.00467 -0.00514 0.02685 0.00255 0.00023 0.00017 0.00013 0.00000 0.00064 0.00070 0.00067 0.00051 0.00049 0.00051 0.00033 H8A 0.74646 0.95931 0.45484 1.00000 0.04028 0.00000 0.00000 H8B 0.85906 0.82965 0.37428 1.00000 0.04028 0.00000 0.00000 H8C 0.87442 0.82295 0.52535 1.00000 0.04028 0.00000 0.00000 C9 0.07349 0.27213 -0.03291 1.00000 0.01869 0.01754 0.01958 0.00103 0.00430 0.00085 0.01858 0.00237 0.00021 0.00014 0.00011 0.00000 0.00057 0.00057 0.00061 0.00044 0.00044 0.00044 0.00029 C10 -0.15443 0.07577 -0.18548 1.00000 0.02538 0.02176 0.01925 -0.00396 0.00409 -0.00016 0.02254 0.00240 0.00022 0.00015 0.00012 0.00000 0.00064 0.00062 0.00061 0.00046 0.00047 0.00048 0.00031 H10A -0.02351 0.00897 -0.19008 1.00000 0.02705 0.00000 0.00000 H10B -0.16044 0.14631 -0.25567 1.00000 0.02705 0.00000 0.00000 C11 -0.38888 -0.02549 -0.19572 1.00000 0.02545 0.02489 0.02790 -0.00211 0.00170 -0.00347 0.02699 0.00255 0.00023 0.00016 0.00013 0.00000 0.00067 0.00067 0.00071 0.00051 0.00051 0.00051 0.00033 H11A -0.38020 -0.09403 -0.12534 1.00000 0.04049 0.00000 0.00000 H11B -0.42182 -0.09034 -0.27751 1.00000 0.04049 0.00000 0.00000 H11C -0.51633 0.04239 -0.19093 1.00000 0.04049 0.00000 0.00000 N1 0.50376 0.64308 0.31655 1.00000 0.01988 0.02363 0.01906 -0.00328 0.00697 -0.00272 0.02100 0.00201 0.00018 0.00013 0.00010 0.00000 0.00054 0.00056 0.00054 0.00041 0.00040 0.00041 0.00028 O1 0.40047 0.75608 0.49757 1.00000 0.03307 0.03854 0.02630 -0.01187 0.01495 -0.01113 0.03317 0.00182 0.00017 0.00012 0.00009 0.00000 0.00055 0.00061 0.00052 0.00041 0.00041 0.00043 0.00031 O2 0.21831 0.29557 -0.10255 1.00000 0.02445 0.02859 0.02067 -0.00228 0.00868 -0.00249 0.02457 0.00171 0.00015 0.00011 0.00008 0.00000 0.00048 0.00051 0.00048 0.00036 0.00036 0.00036 0.00027 O3 -0.11891 0.16698 -0.06270 1.00000 0.02432 0.02407 0.02048 -0.00464 0.00592 -0.00648 0.02360 0.00171 0.00016 0.00011 0.00008 0.00000 0.00048 0.00049 0.00048 0.00036 0.00035 0.00036 0.00027 H1N 0.60722 0.64746 0.26510 1.00000 0.03176 0.03292 0.00262 0.00203 0.00149 0.00000 0.00418 Final Structure Factor Calculation for 2008lsh037 in P1 New: P-1 Total number of l.s. parameters = 143 Maximum vector length = 511 Memory required = 1820 / 22995 wR2 = 0.1442 before cycle 11 for 2337 data and 0 / 143 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.032; Restrained GooF = 1.031 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0976 * P )^2 + 0.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0498 for 1999 Fo > 4sig(Fo) and 0.0579 for all 2337 data wR2 = 0.1442, GooF = S = 1.032, Restrained GooF = 1.031 for all data Occupancy sum of asymmetric unit = 15.00 for non-hydrogen and 13.00 for hydrogen atoms Principal mean square atomic displacements U 0.0219 0.0177 0.0167 C1 0.0217 0.0179 0.0158 C2 0.0211 0.0183 0.0164 C3 0.0265 0.0208 0.0162 C4 0.0336 0.0236 0.0138 C5 0.0311 0.0219 0.0158 C6 0.0279 0.0196 0.0186 C7 0.0385 0.0236 0.0185 C8 0.0206 0.0181 0.0170 C9 0.0285 0.0240 0.0151 C10 0.0323 0.0303 0.0183 C11 0.0309 0.0171 0.0150 N1 0.0612 0.0221 0.0162 O1 0.0354 0.0219 0.0163 O2 0.0364 0.0194 0.0150 O3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.012 0.023 0.036 0.048 0.063 0.085 0.110 0.151 0.216 1.000 Number in group 253. 215. 245. 233. 228. 238. 229. 233. 229. 234. GooF 1.006 1.104 1.051 1.074 1.078 1.009 0.918 0.933 0.863 1.233 K 1.965 1.063 0.961 0.961 0.981 0.981 1.006 1.016 1.022 1.037 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.31 1.65 inf Number in group 240. 232. 231. 235. 233. 236. 231. 231. 235. 233. GooF 1.018 0.922 0.921 0.917 0.934 0.979 0.874 1.075 1.116 1.439 K 1.066 1.063 1.052 1.017 1.037 1.030 1.040 1.064 1.045 0.996 R1 0.110 0.093 0.072 0.060 0.054 0.051 0.042 0.041 0.043 0.058 Recommended weighting scheme: WGHT 0.0857 0.1143 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) 1 -4 3 650.70 1913.83 8.15 0.760 1.79 0 -1 3 1312.60 3314.42 7.45 1.000 3.33 1 0 0 104.50 283.51 7.28 0.292 5.63 -4 -1 6 1.93 5.75 4.63 0.042 1.18 -3 -3 7 3.38 1.03 4.26 0.018 1.17 3 -5 1 1.91 0.04 3.77 0.003 1.31 2 4 0 18.39 11.65 3.65 0.059 1.61 4 5 1 12.05 19.82 3.57 0.077 1.01 0 0 2 2.69 5.62 3.57 0.041 5.23 -1 1 4 48.55 34.19 3.30 0.102 2.41 -5 -3 8 15.89 24.25 3.17 0.086 0.88 0 -3 4 2.11 4.46 3.15 0.037 2.01 1 -1 8 3.55 1.54 3.13 0.022 1.23 2 0 4 0.83 0.01 3.12 0.002 1.77 -1 -1 2 43.45 61.83 3.09 0.137 3.75 5 4 0 8.26 13.16 3.07 0.063 0.95 0 4 6 9.48 5.87 3.05 0.042 1.29 3 -2 3 4.69 2.53 3.00 0.028 1.51 6 -5 1 -1.64 1.82 3.00 0.023 0.85 3 2 1 12.62 8.55 2.86 0.051 1.59 4 -6 8 -0.61 2.31 2.83 0.026 0.80 -2 -3 8 2.86 1.29 2.80 0.020 1.18 -6 2 5 4.80 8.50 2.79 0.051 0.91 1 -1 3 1.10 2.51 2.76 0.028 2.72 -5 0 11 -0.45 1.25 2.71 0.019 0.80 1 3 3 27.74 38.27 2.70 0.107 1.87 -2 -5 4 0.85 0.01 2.70 0.002 1.31 5 3 2 11.72 17.16 2.68 0.072 0.96 0 3 6 103.31 79.36 2.63 0.155 1.43 4 4 0 14.22 20.09 2.61 0.078 1.12 -1 0 7 0.67 0.03 2.59 0.003 1.51 -4 3 4 38.09 28.53 2.58 0.093 1.24 -4 -2 12 2.71 5.28 2.57 0.040 0.79 -1 2 11 5.97 9.22 2.56 0.053 0.93 -4 -6 1 13.96 19.83 2.56 0.077 0.96 6 -1 3 5.49 8.74 2.55 0.051 0.88 -4 8 1 3.23 1.47 2.54 0.021 0.89 -1 -9 2 3.68 6.82 2.54 0.045 0.92 -5 -3 4 4.63 7.69 2.52 0.048 1.01 -5 -4 1 3.14 5.47 2.51 0.041 0.97 2 0 5 1.18 0.32 2.50 0.010 1.56 3 -10 3 1.12 3.78 2.48 0.034 0.79 -2 3 7 3.17 1.70 2.47 0.023 1.26 -2 -4 7 6.15 9.27 2.46 0.053 1.20 -7 -2 5 118.31 88.16 2.45 0.163 0.77 0 1 5 2875.84 2265.64 2.45 0.827 1.99 -6 -4 6 161.31 119.84 2.44 0.190 0.81 -3 -1 3 24.18 18.19 2.44 0.074 1.73 0 -1 1 142.12 199.33 2.43 0.245 6.88 4 3 2 0.86 2.47 2.42 0.027 1.13 Bond lengths and angles C1 - Distance Angles C2 1.4002 (0.0017) C6 1.3966 (0.0017) 119.55 (0.11) N1 1.4148 (0.0015) 117.39 (0.10) 123.05 (0.11) C1 - C2 C6 C2 - Distance Angles C3 1.3905 (0.0017) C1 1.4002 (0.0017) 120.00 (0.11) H2 0.9500 120.00 120.00 C2 - C3 C1 C3 - Distance Angles C2 1.3905 (0.0017) C4 1.3966 (0.0017) 120.50 (0.11) C9 1.4922 (0.0016) 119.11 (0.11) 120.38 (0.11) C3 - C2 C4 C4 - Distance Angles C5 1.3860 (0.0017) C3 1.3966 (0.0017) 119.31 (0.11) H4 0.9500 120.35 120.35 C4 - C5 C3 C5 - Distance Angles C4 1.3860 (0.0017) C6 1.3948 (0.0017) 120.82 (0.11) H5 0.9500 119.59 119.59 C5 - C4 C6 C6 - Distance Angles C5 1.3948 (0.0017) C1 1.3966 (0.0017) 119.81 (0.11) H6 0.9500 120.09 120.09 C6 - C5 C1 C7 - Distance Angles O1 1.2228 (0.0016) N1 1.3664 (0.0016) 123.59 (0.11) C8 1.5074 (0.0017) 121.30 (0.11) 115.10 (0.11) C7 - O1 N1 C8 - Distance Angles C7 1.5074 (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 C9 - Distance Angles O2 1.2120 (0.0015) O3 1.3379 (0.0014) 123.91 (0.11) C3 1.4922 (0.0016) 125.13 (0.11) 110.95 (0.10) C9 - O2 O3 C10 - Distance Angles O3 1.4485 (0.0015) C11 1.5146 (0.0017) 105.99 (0.10) H10A 0.9900 110.54 110.54 H10B 0.9900 110.54 110.54 108.70 C10 - O3 C11 H10A C11 - Distance Angles C10 1.5146 (0.0017) H11A 0.9800 109.47 H11B 0.9800 109.47 109.47 H11C 0.9800 109.47 109.47 109.47 C11 - C10 H11A H11B N1 - Distance Angles C7 1.3664 (0.0016) C1 1.4148 (0.0015) 127.53 (0.10) H1N 0.8703 (0.0133) 118.66 (1.15) 113.64 (1.14) N1 - C7 C1 O1 - Distance Angles C7 1.2228 (0.0016) O1 - O2 - Distance Angles C9 1.2120 (0.0015) O2 - O3 - Distance Angles C9 1.3379 (0.0014) C10 1.4485 (0.0015) 117.67 (0.09) O3 - C9 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.870(13) 2.195(14) 3.0313(13) 161.1(15) N1-H1N...O2_$1 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)