+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 18:09:00 on 11-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh117 in P2(1)2(1)2(1) CELL 0.71073 3.8114 11.3360 18.3264 90.000 90.000 90.000 ZERR 4.00 0.0004 0.0014 0.0017 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 UNIT 36 32 8 4 V = 791.81 F(000) = 336.0 Mu = 0.09 mm-1 Cell Wt = 640.70 Rho = 1.344 MERG 2 OMIT -3.00 55.00 OMIT 0 2 3 OMIT 0 2 1 OMIT 0 1 3 OMIT 0 4 2 TWIN DFIX 0.88 0.02 N1 H1N EQIV $1 x-1/2, -y+1/2, -z+1 HTAB N1 N2_$1 FMAP 2 PLAN 5 SIZE 0.08 0.10 0.16 ACTA HTAB 2.00000 BOND $H L.S. 16 TEMP -153.00 WGHT 0.054800 0.255200 BASF 0.3 FVAR 1.38503 C1 1 -0.146145 0.433546 0.360873 11.00000 0.02295 0.02422 = 0.02244 -0.00081 0.00323 -0.00098 C2 1 -0.082234 0.315364 0.341895 11.00000 0.02261 0.02522 = 0.02403 0.00082 0.00104 -0.00074 C3 1 -0.158719 0.273689 0.271922 11.00000 0.02886 0.02564 = 0.02738 -0.00225 0.00006 0.00207 AFIX 43 H3 2 -0.114840 0.193545 0.259826 11.00000 -1.20000 AFIX 0 C4 1 -0.297805 0.348967 0.220517 11.00000 0.03110 0.03375 = 0.02278 -0.00097 -0.00218 -0.00035 AFIX 43 H4 2 -0.349376 0.321185 0.172801 11.00000 -1.20000 AFIX 0 C5 1 -0.362326 0.466245 0.239044 11.00000 0.02995 0.03123 = 0.02429 0.00526 -0.00039 0.00511 AFIX 43 H5 2 -0.457367 0.518221 0.203508 11.00000 -1.20000 AFIX 0 C6 1 -0.290107 0.508253 0.308444 11.00000 0.02878 0.02217 = 0.02665 0.00010 0.00179 0.00227 AFIX 43 H6 2 -0.338859 0.588170 0.320303 11.00000 -1.20000 AFIX 0 C7 1 0.065839 0.580531 0.450109 11.00000 0.02560 0.02431 = 0.02913 -0.00385 0.00302 0.00122 C8 1 0.131928 0.597869 0.530572 11.00000 0.03504 0.03392 = 0.03106 -0.00720 0.00103 -0.00272 AFIX 137 H8A 2 0.372087 0.626367 0.537929 11.00000 -1.50000 H8B 2 0.101062 0.522627 0.556110 11.00000 -1.50000 H8C 2 -0.034440 0.655873 0.549938 11.00000 -1.50000 AFIX 0 C9 1 0.073371 0.236511 0.394404 11.00000 0.02723 0.02134 = 0.02826 -0.00186 0.00271 -0.00105 N1 3 -0.069903 0.472163 0.432238 11.00000 0.03464 0.02333 = 0.02049 0.00027 -0.00037 -0.00242 N2 3 0.200360 0.173101 0.435697 11.00000 0.04255 0.02860 = 0.03212 0.00377 -0.00315 0.00335 O1 4 0.128839 0.656534 0.404853 11.00000 0.04355 0.02314 = 0.03322 0.00012 0.00588 -0.00493 H1N 2 -0.087824 0.416075 0.465346 11.00000 0.04136 HKLF 4 Covalent radii and connectivity table for 2008lsh117 in P2(1)2(1)2(1) C 0.770 H 0.320 N 0.700 O 0.660 C1 - C6 C2 N1 C2 - C3 C1 C9 C3 - C4 C2 C4 - C3 C5 C5 - C6 C4 C6 - C5 C1 C7 - O1 N1 C8 C8 - C7 C9 - N2 C2 N1 - C7 C1 N2 - C9 O1 - C7 Operators for generating equivalent atoms: $1 x-1/2, -y+1/2, -z+1 9035 Reflections read, of which 60 rejected -4 =< h =< 4, -14 =< k =< 13, -21 =< l =< 23, Max. 2-theta = 54.88 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 3 8 2 193.68 12.29 4 76.62 4 0 4 19.78 6.28 3 93.59 -4 1 5 29.08 6.29 2 263.95 -2 10 6 49.46 7.35 3 195.77 -3 5 11 52.16 8.58 3 105.07 -1 7 16 43.08 4.66 5 28.70 -2 1 17 69.33 5.50 5 76.17 7 Inconsistent equivalents 1792 Unique reflections, of which 0 suppressed R(int) = 0.0973 R(sigma) = 0.0713 Friedel opposites not merged Maximum memory for data reduction = 1268 / 17473 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 = 1563 / 147425 wR2 = 0.1321 before cycle 1 for 1792 data and 115 / 115 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 0.002 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.091; Restrained GooF = 1.091 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0548 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.38021 0.00508 -0.949 OSF 2 3.73002 2.51666 1.363 BASF 1 Mean shift/esd = 0.078 Maximum = 1.363 for BASF 1 Max. shift = 0.002 A for H1N Max. dU = 0.000 for N2 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1563 / 147425 wR2 = 0.1319 before cycle 2 for 1792 data and 115 / 115 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 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.089; Restrained GooF = 1.089 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0548 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.37914 0.00506 -0.211 OSF 2 4.87743 2.51063 0.457 BASF 1 Mean shift/esd = 0.026 Maximum = 0.457 for BASF 1 Max. shift = 0.001 A for H1N Max. dU = 0.000 for O1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1563 / 147425 wR2 = 0.1319 before cycle 3 for 1792 data and 115 / 115 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 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.090; Restrained GooF = 1.089 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0548 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.37912 0.00506 -0.004 OSF 2 4.88390 2.51003 0.003 BASF 1 Mean shift/esd = 0.002 Maximum = -0.015 for tors H8A Max. shift = 0.000 A for H8C Max. dU = 0.000 for H1N Least-squares cycle 4 Maximum vector length = 511 Memory required = 1563 / 147425 wR2 = 0.1319 before cycle 4 for 1792 data and 115 / 115 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 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.089; Restrained GooF = 1.089 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0548 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.37912 0.00506 -0.001 OSF 2 4.88493 2.50963 0.000 BASF 1 Mean shift/esd = 0.001 Maximum = -0.010 for tors H8A Max. shift = 0.000 A for H8C Max. dU = 0.000 for H1N Least-squares cycle 5 Maximum vector length = 511 Memory required = 1563 / 147425 wR2 = 0.1319 before cycle 5 for 1792 data and 115 / 115 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 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.090; Restrained GooF = 1.089 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0548 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.37912 0.00506 0.000 OSF 2 4.88472 2.50968 0.000 BASF 1 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 6 Maximum vector length = 511 Memory required = 1563 / 147425 wR2 = 0.1319 before cycle 6 for 1792 data and 115 / 115 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 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.089; Restrained GooF = 1.089 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0548 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.37912 0.00506 0.000 OSF 2 4.88486 2.50962 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = -0.005 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 = 1563 / 147425 wR2 = 0.1319 before cycle 7 for 1792 data and 115 / 115 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 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.090; Restrained GooF = 1.089 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0548 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.37912 0.00506 0.000 OSF 2 4.88519 2.50970 0.000 BASF 1 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 8 Maximum vector length = 511 Memory required = 1563 / 147425 wR2 = 0.1319 before cycle 8 for 1792 data and 115 / 115 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 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.089; Restrained GooF = 1.089 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0548 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.37912 0.00506 0.000 OSF 2 4.88488 2.50961 0.000 BASF 1 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 9 Maximum vector length = 511 Memory required = 1563 / 147425 wR2 = 0.1319 before cycle 9 for 1792 data and 115 / 115 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 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.089; Restrained GooF = 1.089 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0548 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.37912 0.00506 0.000 OSF 2 4.88482 2.50961 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = -0.002 for tors H8A Max. shift = 0.000 A for H8B Max. dU = 0.000 for H1N Least-squares cycle 10 Maximum vector length = 511 Memory required = 1563 / 147425 wR2 = 0.1319 before cycle 10 for 1792 data and 115 / 115 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 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.089; Restrained GooF = 1.089 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0548 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.37912 0.00506 0.000 OSF 2 4.88571 2.50953 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = -0.001 for tors H8A Max. shift = 0.000 A for H8C Max. dU = 0.000 for H1N Least-squares cycle 11 Maximum vector length = 511 Memory required = 1563 / 147425 wR2 = 0.1319 before cycle 11 for 1792 data and 115 / 115 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 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.089; Restrained GooF = 1.089 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0548 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.37911 0.00506 0.000 OSF 2 4.88574 2.50950 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = -0.001 for tors H8A Max. shift = 0.000 A for H8C Max. dU = 0.000 for H1N Least-squares cycle 12 Maximum vector length = 511 Memory required = 1563 / 147425 wR2 = 0.1319 before cycle 12 for 1792 data and 115 / 115 parameters Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.089; Restrained GooF = 1.089 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0548 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.37911 0.00506 0.000 OSF 2 4.88526 2.50955 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for tors H8A Max. shift = 0.000 A for H8A Max. dU = 0.000 for H1N Least-squares cycle 13 Maximum vector length = 511 Memory required = 1563 / 147425 wR2 = 0.1319 before cycle 13 for 1792 data and 115 / 115 parameters Summary of restraints applied in cycle 13 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.089; Restrained GooF = 1.089 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0548 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.37911 0.00506 0.000 OSF 2 4.88547 2.50958 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for tors H8A Max. shift = 0.000 A for H8B Max. dU = 0.000 for H1N Least-squares cycle 14 Maximum vector length = 511 Memory required = 1563 / 147425 wR2 = 0.1319 before cycle 14 for 1792 data and 115 / 115 parameters Summary of restraints applied in cycle 14 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.089; Restrained GooF = 1.089 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0548 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.37911 0.00506 0.000 OSF 2 4.88525 2.50962 0.000 BASF 1 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 15 Maximum vector length = 511 Memory required = 1563 / 147425 wR2 = 0.1319 before cycle 15 for 1792 data and 115 / 115 parameters Summary of restraints applied in cycle 15 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.090; Restrained GooF = 1.089 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0548 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.37912 0.00506 0.000 OSF 2 4.88537 2.50966 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H8C Max. dU = 0.000 for H1N Least-squares cycle 16 Maximum vector length = 511 Memory required = 1563 / 147425 wR2 = 0.1319 before cycle 16 for 1792 data and 115 / 115 parameters Summary of restraints applied in cycle 16 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.089; Restrained GooF = 1.089 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0548 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.37912 0.00506 0.000 OSF 2 4.88502 2.50957 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for z O1 Max. shift = 0.000 A for H8C Max. dU = 0.000 for C3 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 17 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 -0.1149 0.1935 0.2598 43 0.950 0.000 C3 C4 C2 H4 -0.3493 0.3212 0.1728 43 0.950 0.000 C4 C3 C5 H5 -0.4573 0.5182 0.2035 43 0.950 0.000 C5 C6 C4 H6 -0.3389 0.5882 0.3203 43 0.950 0.000 C6 C5 C1 H8A 0.3722 0.6262 0.5379 137 0.980 0.000 C8 C7 H8A H8B 0.1007 0.5227 0.5561 137 0.980 0.000 C8 C7 H8A H8C -0.0342 0.6560 0.5499 137 0.980 0.000 C8 C7 H8A 2008lsh117 in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.14616 0.43354 0.36087 1.00000 0.02278 0.02400 0.02220 -0.00081 0.00316 -0.00095 0.02299 0.00374 0.00056 0.00019 0.00011 0.00000 0.00106 0.00114 0.00094 0.00083 0.00085 0.00089 0.00048 C2 -0.08224 0.31536 0.34190 1.00000 0.02244 0.02501 0.02383 0.00079 0.00103 -0.00072 0.02376 0.00382 0.00062 0.00020 0.00011 0.00000 0.00110 0.00111 0.00093 0.00084 0.00082 0.00094 0.00047 C3 -0.15873 0.27368 0.27192 1.00000 0.02867 0.02545 0.02717 -0.00222 0.00002 0.00207 0.02710 0.00391 0.00060 0.00021 0.00012 0.00000 0.00127 0.00119 0.00102 0.00088 0.00095 0.00102 0.00052 H3 -0.11488 0.19353 0.25983 1.00000 0.03252 0.00000 0.00000 C4 -0.29780 0.34898 0.22051 1.00000 0.03089 0.03350 0.02261 -0.00097 -0.00219 -0.00031 0.02900 0.00403 0.00064 0.00022 0.00012 0.00000 0.00121 0.00134 0.00099 0.00095 0.00087 0.00108 0.00053 H4 -0.34935 0.32121 0.17279 1.00000 0.03480 0.00000 0.00000 C5 -0.36230 0.46625 0.23904 1.00000 0.02974 0.03101 0.02409 0.00524 -0.00041 0.00510 0.02828 0.00413 0.00062 0.00021 0.00011 0.00000 0.00122 0.00126 0.00097 0.00091 0.00089 0.00102 0.00052 H5 -0.45730 0.51823 0.20350 1.00000 0.03394 0.00000 0.00000 C6 -0.29014 0.50826 0.30844 1.00000 0.02860 0.02199 0.02645 0.00013 0.00176 0.00226 0.02568 0.00392 0.00060 0.00020 0.00011 0.00000 0.00121 0.00110 0.00106 0.00088 0.00087 0.00094 0.00051 H6 -0.33894 0.58817 0.32031 1.00000 0.03082 0.00000 0.00000 C7 0.06581 0.58052 0.45011 1.00000 0.02542 0.02410 0.02890 -0.00386 0.00300 0.00119 0.02614 0.00386 0.00061 0.00020 0.00011 0.00000 0.00112 0.00117 0.00107 0.00091 0.00087 0.00101 0.00050 C8 0.13193 0.59787 0.53057 1.00000 0.03485 0.03372 0.03081 -0.00718 0.00101 -0.00270 0.03313 0.00426 0.00071 0.00023 0.00012 0.00000 0.00141 0.00136 0.00109 0.00100 0.00104 0.00111 0.00058 H8A 0.37223 0.62624 0.53793 1.00000 0.04969 0.00000 0.00000 H8B 0.10067 0.52266 0.55613 1.00000 0.04969 0.00000 0.00000 H8C -0.03416 0.65598 0.54992 1.00000 0.04969 0.00000 0.00000 C9 0.07335 0.23652 0.39440 1.00000 0.02704 0.02113 0.02811 -0.00186 0.00271 -0.00105 0.02542 0.00385 0.00062 0.00020 0.00012 0.00000 0.00111 0.00105 0.00101 0.00088 0.00093 0.00097 0.00048 N1 -0.06989 0.47217 0.43224 1.00000 0.03446 0.02313 0.02025 0.00023 -0.00039 -0.00245 0.02594 0.00325 0.00054 0.00017 0.00009 0.00000 0.00107 0.00097 0.00082 0.00074 0.00077 0.00088 0.00045 N2 0.20040 0.17310 0.43570 1.00000 0.04227 0.02840 0.03189 0.00373 -0.00313 0.00332 0.03418 0.00380 0.00060 0.00019 0.00011 0.00000 0.00120 0.00109 0.00097 0.00089 0.00095 0.00097 0.00051 O1 0.12885 0.65654 0.40485 1.00000 0.04332 0.02292 0.03299 0.00013 0.00586 -0.00489 0.03307 0.00288 0.00048 0.00014 0.00008 0.00000 0.00103 0.00085 0.00081 0.00070 0.00076 0.00077 0.00044 H1N -0.08831 0.41621 0.46539 1.00000 0.04136 0.05181 0.00844 0.00213 0.00124 0.00000 0.00773 Final Structure Factor Calculation for 2008lsh117 in P2(1)2(1)2(1) Total number of l.s. parameters = 115 Maximum vector length = 511 Memory required = 1450 / 25046 wR2 = 0.1319 before cycle 17 for 1792 data and 2 / 115 parameters Summary of restraints applied in cycle 17 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.089; Restrained GooF = 1.089 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0548 * P )^2 + 0.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0557 for 1546 Fo > 4sig(Fo) and 0.0673 for all 1792 data wR2 = 0.1319, GooF = S = 1.089, Restrained GooF = 1.089 for all data Occupancy sum of asymmetric unit = 12.00 for non-hydrogen and 8.00 for hydrogen atoms Principal mean square atomic displacements U 0.0263 0.0233 0.0193 C1 0.0254 0.0243 0.0216 C2 0.0301 0.0279 0.0234 C3 0.0336 0.0314 0.0220 C4 0.0367 0.0278 0.0203 C5 0.0301 0.0257 0.0213 C6 0.0318 0.0261 0.0206 C7 0.0408 0.0337 0.0249 C8 0.0308 0.0248 0.0206 C9 0.0350 0.0226 0.0202 N1 0.0435 0.0342 0.0249 N2 0.0468 0.0308 0.0216 O1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.025 0.040 0.052 0.064 0.078 0.091 0.113 0.146 0.198 1.000 Number in group 181. 191. 170. 184. 181. 169. 180. 177. 181. 178. GooF 1.097 1.033 0.985 1.166 1.105 1.049 0.983 1.113 0.922 1.375 K 2.257 1.280 1.094 1.042 0.987 1.002 0.997 1.001 1.013 0.982 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.31 1.64 inf Number in group 183. 177. 181. 177. 178. 182. 181. 175. 179. 179. GooF 0.979 1.051 1.103 1.050 0.984 1.066 1.001 0.938 1.067 1.536 K 1.078 1.136 1.083 1.008 0.999 1.000 1.002 1.017 1.023 0.968 R1 0.152 0.147 0.102 0.100 0.085 0.055 0.041 0.037 0.044 0.047 Recommended weighting scheme: WGHT 0.0551 0.2503 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 2 0 338.38 717.42 7.18 0.369 3.16 0 1 4 4.10 20.69 6.62 0.063 4.25 0 2 4 267.96 526.40 6.54 0.316 3.56 1 9 5 154.04 273.77 5.13 0.228 1.14 0 5 6 123.12 92.01 3.45 0.132 1.82 1 4 0 30.18 49.18 3.22 0.097 2.27 2 10 8 73.69 114.49 3.17 0.148 0.90 -4 4 10 23.62 6.76 3.03 0.036 0.81 0 11 2 14.38 26.39 3.01 0.071 1.02 2 4 16 12.28 24.53 3.00 0.068 0.93 0 1 8 46.60 33.74 2.93 0.080 2.25 -2 8 12 7.18 0.31 2.88 0.008 0.91 1 7 19 3.13 13.20 2.84 0.050 0.81 1 9 2 29.55 44.89 2.79 0.092 1.19 4 4 8 12.86 24.80 2.76 0.069 0.84 -4 3 6 44.06 78.32 2.67 0.122 0.88 3 0 6 14.60 22.79 2.65 0.066 1.17 1 4 14 41.22 55.41 2.65 0.103 1.13 1 12 5 26.44 8.75 2.64 0.041 0.89 -2 3 20 6.05 17.12 2.64 0.057 0.81 1 8 4 16.76 26.28 2.61 0.071 1.28 -2 11 8 67.83 39.61 2.59 0.087 0.84 2 10 6 10.80 24.00 2.56 0.068 0.93 3 5 16 10.30 19.41 2.51 0.061 0.80 0 4 6 94.56 75.19 2.49 0.120 2.08 1 13 10 46.47 18.45 2.44 0.059 0.77 0 3 17 47.18 35.83 2.41 0.083 1.04 0 11 9 7.81 2.18 2.40 0.020 0.92 3 10 2 18.23 7.40 2.38 0.038 0.84 0 8 0 61.40 42.97 2.37 0.090 1.42 1 11 4 87.89 114.16 2.37 0.147 0.97 2 0 16 5.26 0.80 2.37 0.012 0.98 2 0 10 26.76 35.86 2.34 0.083 1.32 0 11 10 11.86 2.26 2.34 0.021 0.90 2 6 11 31.50 41.83 2.32 0.089 1.04 0 5 20 6.59 0.43 2.31 0.009 0.85 0 0 4 31.28 43.26 2.29 0.091 4.58 -1 11 15 13.14 28.19 2.27 0.073 0.77 3 3 16 15.96 8.32 2.27 0.040 0.83 0 2 8 502.43 427.84 2.24 0.285 2.12 0 0 10 463.76 393.26 2.23 0.273 1.83 2 5 13 39.90 51.28 2.23 0.099 1.01 -4 3 9 44.45 30.90 2.23 0.077 0.84 -3 11 2 30.84 16.16 2.22 0.055 0.80 -1 4 20 11.42 4.74 2.22 0.030 0.85 0 8 4 53.74 69.12 2.21 0.115 1.35 3 1 2 22.50 30.99 2.21 0.077 1.25 0 9 17 29.83 10.92 2.19 0.046 0.82 1 1 1 3360.40 4798.85 2.19 0.955 3.54 -1 13 3 23.78 8.74 2.19 0.041 0.84 Bond lengths and angles C1 - Distance Angles C6 1.3933 (0.0031) C2 1.4053 (0.0031) 118.50 (0.19) N1 1.4097 (0.0027) 122.15 (0.20) 119.33 (0.19) C1 - C6 C2 C2 - Distance Angles C3 1.3974 (0.0030) C1 1.4053 (0.0031) 120.88 (0.20) C9 1.4410 (0.0031) 119.27 (0.20) 119.83 (0.19) C2 - C3 C1 C3 - Distance Angles C4 1.3775 (0.0033) C2 1.3974 (0.0030) 119.89 (0.22) H3 0.9500 120.05 120.05 C3 - C4 C2 C4 - Distance Angles C3 1.3775 (0.0033) C5 1.3939 (0.0035) 119.49 (0.21) H4 0.9500 120.26 120.26 C4 - C3 C5 C5 - Distance Angles C6 1.3857 (0.0031) C4 1.3939 (0.0035) 121.09 (0.20) H5 0.9500 119.46 119.46 C5 - C6 C4 C6 - Distance Angles C5 1.3857 (0.0031) C1 1.3933 (0.0031) 120.14 (0.21) H6 0.9500 119.93 119.93 C6 - C5 C1 C7 - Distance Angles O1 1.2200 (0.0028) N1 1.3724 (0.0030) 122.97 (0.20) C8 1.5088 (0.0030) 122.65 (0.21) 114.38 (0.20) C7 - O1 N1 C8 - Distance Angles C7 1.5088 (0.0030) 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 N2 1.1507 (0.0030) C2 1.4410 (0.0031) 179.18 (0.25) C9 - N2 N1 - Distance Angles C7 1.3724 (0.0031) C1 1.4097 (0.0027) 125.25 (0.19) H1N 0.8812 (0.0173) 120.65 (1.92) 113.56 (1.89) N1 - C7 C1 N2 - Distance Angles C9 1.1507 (0.0030) N2 - O1 - Distance Angles C7 1.2200 (0.0028) O1 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.881(17) 2.23(2) 3.055(3) 157(3) N1-H1N...N2_$1 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)