+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 18:54:55 on 18-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh009 in P-1 CELL 0.71073 5.0214 6.8411 12.2219 89.465 80.477 79.234 ZERR 2.00 0.0003 0.0005 0.0010 0.004 0.004 0.004 LATT 1 SFAC C H N O UNIT 18 18 2 6 V = 406.67 F(000) = 188.0 Mu = 0.11 mm-1 Cell Wt = 358.34 Rho = 1.463 MERG 2 OMIT -3.00 55.00 FMAP 2 PLAN 5 ACTA DFIX 0.84 0.02 O2 H2O DFIX 0.88 0.02 N1 H1N EQIV $1 x-1, y, z EQIV $2 -x+1, -y+1, -z+2 HTAB N1 O1_$1 HTAB O2 O3_$2 HTAB SIZE 0.12 0.08 0.02 BOND $H L.S. 16 TEMP -153.00 WGHT 0.0283 0.6157 FVAR 1.09223 C1 1 0.652967 -0.284330 0.732003 11.00000 0.02314 0.01937 = 0.02468 -0.00344 -0.00105 -0.00667 C2 1 0.826742 -0.265782 0.806985 11.00000 0.02522 0.02121 = 0.02833 -0.00068 -0.00581 -0.00306 AFIX 43 H2 2 0.967538 -0.374263 0.818028 11.00000 -1.20000 AFIX 0 C3 1 0.793872 -0.088632 0.865509 11.00000 0.02789 0.02396 = 0.02609 -0.00134 -0.00854 -0.00515 AFIX 43 H3 2 0.915209 -0.075166 0.915746 11.00000 -1.20000 AFIX 0 C4 1 0.584581 0.070782 0.851727 11.00000 0.02324 0.02038 = 0.02182 -0.00122 -0.00222 -0.00541 C5 1 0.407248 0.049977 0.777878 11.00000 0.02537 0.02215 = 0.02989 0.00048 -0.00642 -0.00275 AFIX 43 H5 2 0.262360 0.156772 0.768711 11.00000 -1.20000 AFIX 0 C6 1 0.442224 -0.126341 0.717863 11.00000 0.02565 0.02473 = 0.03026 -0.00276 -0.00908 -0.00446 AFIX 43 H6 2 0.322479 -0.139754 0.666958 11.00000 -1.20000 AFIX 0 C7 1 0.914110 -0.583226 0.626471 11.00000 0.02804 0.02016 = 0.02341 0.00071 -0.00425 -0.00391 C8 1 0.884047 -0.770142 0.568792 11.00000 0.03390 0.02189 = 0.03142 -0.00420 -0.00437 -0.00459 AFIX 137 H8A 2 1.023013 -0.796529 0.501576 11.00000 -1.50000 H8B 2 0.700226 -0.752666 0.548640 11.00000 -1.50000 H8C 2 0.909389 -0.882570 0.618715 11.00000 -1.50000 AFIX 0 C9 1 0.548455 0.260503 0.914109 11.00000 0.02574 0.01926 = 0.02436 -0.00070 -0.00446 -0.00399 N1 3 0.675130 -0.464038 0.671308 11.00000 0.02321 0.02091 = 0.02984 -0.00379 -0.00668 -0.00449 O1 4 1.142390 -0.545721 0.631594 11.00000 0.02470 0.02816 = 0.03485 -0.00381 -0.00651 -0.00614 O2 4 0.736419 0.272124 0.974126 11.00000 0.03133 0.02504 = 0.03743 -0.00714 -0.01239 -0.00376 O3 4 0.350790 0.396772 0.907999 11.00000 0.03377 0.02055 = 0.03294 -0.00388 -0.00839 -0.00089 H1N 2 0.518734 -0.489037 0.657543 11.00000 0.04707 H2O 2 0.701274 0.384535 1.009531 11.00000 0.10482 HKLF 4 Covalent radii and connectivity table for 2008lsh009 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 C1 - C2 C6 N1 C2 - C3 C1 C3 - C2 C4 C4 - C5 C3 C9 C5 - C6 C4 C6 - C5 C1 C7 - O1 N1 C8 C8 - C7 C9 - O3 O2 C4 N1 - C7 C1 O1 - C7 O2 - C9 O3 - C9 Operators for generating equivalent atoms: $1 x-1, y, z $2 -x+1, -y+1, -z+2 6987 Reflections read, of which 19 rejected -6 =< h =< 6, -8 =< k =< 8, -15 =< l =< 15, Max. 2-theta = 54.98 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -4 -5 1 0.46 0.39 3 2.95 1 Inconsistent equivalents 1841 Unique reflections, of which 0 suppressed R(int) = 0.0578 R(sigma) = 0.0572 Friedel opposites merged Maximum memory for data reduction = 1358 / 18182 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 = 1695 / 161171 wR2 = 0.1474 before cycle 1 for 1841 data and 127 / 127 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.014 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 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 0.62 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.09460 0.00364 0.652 OSF Mean shift/esd = 0.111 Maximum = 0.652 for OSF Max. shift = 0.011 A for H1N Max. dU =-0.003 for H2O Least-squares cycle 2 Maximum vector length = 511 Memory required = 1695 / 161171 wR2 = 0.1473 before cycle 2 for 1841 data and 127 / 127 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.018 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.090; Restrained GooF = 1.090 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 0.62 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.09477 0.00364 0.047 OSF Mean shift/esd = 0.039 Maximum = -0.136 for U11 H2O Max. shift = 0.004 A for H1N Max. dU =-0.002 for H2O Least-squares cycle 3 Maximum vector length = 511 Memory required = 1695 / 161171 wR2 = 0.1473 before cycle 3 for 1841 data and 127 / 127 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.090; Restrained GooF = 1.090 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 0.62 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.09481 0.00364 0.010 OSF Mean shift/esd = 0.005 Maximum = -0.039 for U11 H2O Max. shift = 0.001 A for H1N Max. dU =-0.001 for H2O Least-squares cycle 4 Maximum vector length = 511 Memory required = 1695 / 161171 wR2 = 0.1473 before cycle 4 for 1841 data and 127 / 127 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.090; Restrained GooF = 1.090 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 0.62 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.09481 0.00364 0.001 OSF Mean shift/esd = 0.001 Maximum = -0.012 for U11 H2O Max. shift = 0.000 A for H1N Max. dU = 0.000 for H2O Least-squares cycle 5 Maximum vector length = 511 Memory required = 1695 / 161171 wR2 = 0.1473 before cycle 5 for 1841 data and 127 / 127 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.090; Restrained GooF = 1.090 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 0.62 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.09481 0.00364 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.003 for U11 H2O Max. shift = 0.000 A for H1N Max. dU = 0.000 for H2O Least-squares cycle 6 Maximum vector length = 511 Memory required = 1695 / 161171 wR2 = 0.1473 before cycle 6 for 1841 data and 127 / 127 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.090; Restrained GooF = 1.090 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 0.62 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.09482 0.00364 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for U11 H2O Max. shift = 0.000 A for H1N Max. dU = 0.000 for H2O Least-squares cycle 7 Maximum vector length = 511 Memory required = 1695 / 161171 wR2 = 0.1473 before cycle 7 for 1841 data and 127 / 127 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.090; Restrained GooF = 1.090 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 0.62 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.09482 0.00364 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for U11 H2O Max. shift = 0.000 A for H2O Max. dU = 0.000 for H2O Least-squares cycle 8 Maximum vector length = 511 Memory required = 1695 / 161171 wR2 = 0.1473 before cycle 8 for 1841 data and 127 / 127 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.090; Restrained GooF = 1.090 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 0.62 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.09482 0.00364 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O1 Max. shift = 0.000 A for H2O Max. dU = 0.000 for H2O Least-squares cycle 9 Maximum vector length = 511 Memory required = 1695 / 161171 wR2 = 0.1473 before cycle 9 for 1841 data and 127 / 127 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.090; Restrained GooF = 1.090 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 0.62 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.09482 0.00364 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O1 Max. shift = 0.000 A for H8B Max. dU = 0.000 for H2O Least-squares cycle 10 Maximum vector length = 511 Memory required = 1695 / 161171 wR2 = 0.1473 before cycle 10 for 1841 data and 127 / 127 parameters Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.090; Restrained GooF = 1.090 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 0.62 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.09482 0.00364 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C3 Max. shift = 0.000 A for H8B Max. dU = 0.000 for H1N Least-squares cycle 11 Maximum vector length = 511 Memory required = 1695 / 161171 wR2 = 0.1473 before cycle 11 for 1841 data and 127 / 127 parameters Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.090; Restrained GooF = 1.090 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 0.62 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.09482 0.00364 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H2O Least-squares cycle 12 Maximum vector length = 511 Memory required = 1695 / 161171 wR2 = 0.1473 before cycle 12 for 1841 data and 127 / 127 parameters Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.090; Restrained GooF = 1.090 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 0.62 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.09482 0.00364 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C3 Max. shift = 0.000 A for H8B Max. dU = 0.000 for H2O Least-squares cycle 13 Maximum vector length = 511 Memory required = 1695 / 161171 wR2 = 0.1473 before cycle 13 for 1841 data and 127 / 127 parameters Summary of restraints applied in cycle 13 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.090; Restrained GooF = 1.090 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 0.62 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.09482 0.00364 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C3 Max. shift = 0.000 A for C3 Max. dU = 0.000 for H1N Least-squares cycle 14 Maximum vector length = 511 Memory required = 1695 / 161171 wR2 = 0.1473 before cycle 14 for 1841 data and 127 / 127 parameters Summary of restraints applied in cycle 14 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.090; Restrained GooF = 1.090 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 0.62 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.09482 0.00364 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O1 Max. shift = 0.000 A for H8C Max. dU = 0.000 for H1N Least-squares cycle 15 Maximum vector length = 511 Memory required = 1695 / 161171 wR2 = 0.1473 before cycle 15 for 1841 data and 127 / 127 parameters Summary of restraints applied in cycle 15 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.090; Restrained GooF = 1.090 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 0.62 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.09482 0.00364 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C3 Max. shift = 0.000 A for C3 Max. dU = 0.000 for H2O Least-squares cycle 16 Maximum vector length = 511 Memory required = 1695 / 161171 wR2 = 0.1473 before cycle 16 for 1841 data and 127 / 127 parameters Summary of restraints applied in cycle 16 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.090; Restrained GooF = 1.090 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 0.62 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.09482 0.00364 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O1 Max. shift = 0.000 A for H8B Max. dU = 0.000 for H2O Largest correlation matrix elements -0.648 z H2O / y H2O Idealized hydrogen atom generation before cycle 17 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.9676 -0.3742 0.8178 43 0.950 0.000 C2 C3 C1 H3 0.9152 -0.0753 0.9157 43 0.950 0.000 C3 C2 C4 H5 0.2624 0.1566 0.7688 43 0.950 0.000 C5 C6 C4 H6 0.3226 -0.1397 0.6669 43 0.950 0.000 C6 C5 C1 H8A 1.0222 -0.7960 0.5013 137 0.980 0.000 C8 C7 H8A H8B 0.6998 -0.7530 0.5492 137 0.980 0.000 C8 C7 H8A H8C 0.9107 -0.8827 0.6186 137 0.980 0.000 C8 C7 H8A 2008lsh009 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.65295 -0.28425 0.73203 1.00000 0.02312 0.01939 0.02466 -0.00321 -0.00116 -0.00697 0.02230 0.00380 0.00051 0.00035 0.00021 0.00000 0.00127 0.00115 0.00137 0.00101 0.00105 0.00100 0.00055 C2 0.82668 -0.26571 0.80689 1.00000 0.02501 0.02126 0.02841 -0.00048 -0.00584 -0.00297 0.02491 0.00396 0.00053 0.00037 0.00022 0.00000 0.00132 0.00121 0.00146 0.00105 0.00111 0.00103 0.00058 H2 0.96759 -0.37417 0.81785 1.00000 0.02989 0.00000 0.00000 C3 0.79385 -0.08869 0.86548 1.00000 0.02752 0.02409 0.02614 -0.00123 -0.00855 -0.00522 0.02539 0.00409 0.00055 0.00037 0.00023 0.00000 0.00134 0.00126 0.00139 0.00106 0.00110 0.00106 0.00058 H3 0.91517 -0.07531 0.91574 1.00000 0.03046 0.00000 0.00000 C4 0.58461 0.07073 0.85172 1.00000 0.02304 0.02025 0.02180 -0.00094 -0.00214 -0.00529 0.02171 0.00387 0.00051 0.00035 0.00021 0.00000 0.00125 0.00116 0.00134 0.00101 0.00104 0.00100 0.00054 C5 0.40734 0.04987 0.77791 1.00000 0.02515 0.02226 0.03001 0.00065 -0.00654 -0.00281 0.02579 0.00408 0.00054 0.00038 0.00023 0.00000 0.00133 0.00121 0.00148 0.00107 0.00112 0.00104 0.00058 H5 0.26237 0.15664 0.76879 1.00000 0.03095 0.00000 0.00000 C6 0.44231 -0.12636 0.71785 1.00000 0.02538 0.02481 0.03022 -0.00249 -0.00905 -0.00453 0.02630 0.00407 0.00054 0.00038 0.00023 0.00000 0.00133 0.00126 0.00149 0.00109 0.00115 0.00106 0.00059 H6 0.32265 -0.13974 0.66690 1.00000 0.03156 0.00000 0.00000 C7 0.91416 -0.58335 0.62646 1.00000 0.02791 0.02015 0.02381 0.00109 -0.00431 -0.00384 0.02405 0.00405 0.00054 0.00036 0.00022 0.00000 0.00138 0.00117 0.00138 0.00101 0.00108 0.00105 0.00057 C8 0.88408 -0.77011 0.56884 1.00000 0.03438 0.02195 0.03140 -0.00411 -0.00411 -0.00444 0.02948 0.00424 0.00060 0.00038 0.00024 0.00000 0.00149 0.00124 0.00155 0.00110 0.00120 0.00111 0.00062 H8A 1.02216 -0.79598 0.50134 1.00000 0.04423 0.00000 0.00000 H8B 0.69978 -0.75298 0.54918 1.00000 0.04423 0.00000 0.00000 H8C 0.91074 -0.88271 0.61857 1.00000 0.04423 0.00000 0.00000 C9 0.54843 0.26040 0.91408 1.00000 0.02572 0.01952 0.02421 -0.00046 -0.00443 -0.00429 0.02311 0.00390 0.00052 0.00036 0.00021 0.00000 0.00133 0.00117 0.00138 0.00102 0.00108 0.00104 0.00056 N1 0.67514 -0.46397 0.67121 1.00000 0.02281 0.02106 0.03008 -0.00370 -0.00683 -0.00438 0.02431 0.00339 0.00045 0.00031 0.00019 0.00000 0.00116 0.00104 0.00127 0.00090 0.00096 0.00089 0.00051 O1 1.14231 -0.54573 0.63165 1.00000 0.02494 0.02815 0.03508 -0.00350 -0.00649 -0.00608 0.02905 0.00284 0.00037 0.00027 0.00016 0.00000 0.00099 0.00097 0.00113 0.00082 0.00084 0.00080 0.00047 O2 0.73644 0.27203 0.97412 1.00000 0.03158 0.02492 0.03760 -0.00731 -0.01257 -0.00371 0.03074 0.00291 0.00040 0.00028 0.00017 0.00000 0.00105 0.00097 0.00120 0.00086 0.00089 0.00083 0.00048 O3 0.35074 0.39684 0.90798 1.00000 0.03341 0.02049 0.03320 -0.00370 -0.00841 -0.00080 0.02923 0.00288 0.00039 0.00025 0.00016 0.00000 0.00106 0.00089 0.00112 0.00078 0.00086 0.00080 0.00047 H1N 0.51971 -0.48896 0.65630 1.00000 0.04507 0.03768 0.00474 0.00478 0.00276 0.00000 0.00979 H2O 0.70165 0.38462 1.01048 1.00000 0.09813 0.05291 0.00973 0.00430 0.00357 0.00000 0.01685 Final Structure Factor Calculation for 2008lsh009 in P-1 Total number of l.s. parameters = 127 Maximum vector length = 511 Memory required = 1568 / 22995 wR2 = 0.1473 before cycle 17 for 1841 data and 0 / 127 parameters Summary of restraints applied in cycle 17 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 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 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.090; Restrained GooF = 1.090 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 0.62 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0640 for 1328 Fo > 4sig(Fo) and 0.0995 for all 1841 data wR2 = 0.1473, GooF = S = 1.090, Restrained GooF = 1.090 for all data Occupancy sum of asymmetric unit = 13.00 for non-hydrogen and 9.00 for hydrogen atoms Principal mean square atomic displacements U 0.0293 0.0214 0.0163 C1 0.0291 0.0246 0.0210 C2 0.0307 0.0251 0.0204 C3 0.0249 0.0210 0.0192 C4 0.0305 0.0253 0.0216 C5 0.0336 0.0249 0.0205 C6 0.0282 0.0239 0.0200 C7 0.0352 0.0332 0.0201 C8 0.0258 0.0243 0.0192 C9 0.0323 0.0225 0.0181 N1 0.0372 0.0273 0.0226 O1 0.0450 0.0278 0.0194 O2 0.0387 0.0299 0.0191 O3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.014 0.021 0.029 0.038 0.048 0.063 0.086 0.124 1.000 Number in group 213. 173. 180. 183. 175. 181. 198. 170. 184. 184. GooF 1.200 1.204 1.153 1.199 1.020 1.050 1.017 0.928 1.065 1.007 K 5.719 1.609 1.077 1.133 1.033 0.973 0.983 0.993 1.002 1.000 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.16 1.32 1.66 inf Number in group 184. 190. 184. 181. 182. 187. 183. 182. 185. 183. GooF 1.197 1.199 1.208 1.188 1.051 1.107 1.093 0.844 0.895 1.047 K 1.060 1.109 1.088 1.040 1.002 1.018 0.991 0.999 1.016 0.988 R1 0.240 0.206 0.209 0.178 0.133 0.103 0.059 0.054 0.042 0.033 Recommended weighting scheme: WGHT 0.0230 0.6179 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 3 -4 4 51.42 111.98 6.49 0.110 1.05 4 -4 2 51.16 80.79 3.64 0.094 0.92 -4 5 4 13.95 0.30 3.47 0.006 0.77 -4 -5 8 14.46 0.25 3.35 0.005 0.79 5 -2 7 -1.67 6.47 3.23 0.026 0.85 5 1 9 14.24 1.49 3.20 0.013 0.87 4 1 11 11.40 2.81 3.16 0.017 0.90 3 4 13 15.66 0.29 3.08 0.006 0.80 -1 3 13 11.72 1.32 3.04 0.012 0.81 2 -5 10 -2.64 5.94 3.03 0.025 0.85 2 7 3 9.28 21.00 3.01 0.048 0.94 5 1 5 8.45 1.98 2.97 0.015 0.97 3 0 11 11.12 26.61 2.94 0.054 0.99 0 0 9 -1.45 3.05 2.89 0.018 1.34 -3 -6 6 4.30 14.44 2.87 0.040 0.88 -2 7 0 14.06 4.28 2.79 0.022 0.84 2 -5 12 -3.69 6.74 2.75 0.027 0.78 2 -4 7 7.92 1.52 2.72 0.013 1.08 -2 -3 13 14.43 28.43 2.69 0.055 0.79 3 0 13 8.13 0.00 2.68 0.000 0.87 -3 -3 7 265.53 212.52 2.63 0.152 1.04 -1 4 2 4.96 0.36 2.61 0.006 1.43 2 1 5 198.40 164.54 2.58 0.133 1.87 0 3 3 410.85 354.44 2.56 0.196 1.94 -5 -1 5 21.99 4.34 2.55 0.022 0.87 4 2 8 7.91 1.80 2.55 0.014 1.03 -1 -1 2 8066.45 9237.15 2.54 1.000 3.32 1 6 5 11.76 21.30 2.52 0.048 1.04 0 -5 10 6.23 16.21 2.51 0.042 0.91 -3 -1 12 8.71 1.75 2.46 0.014 0.80 3 2 12 14.71 6.20 2.46 0.026 0.91 1 -4 12 192.71 134.17 2.45 0.121 0.86 -3 -4 8 8.70 19.60 2.45 0.046 0.93 3 7 6 15.43 3.39 2.45 0.019 0.85 6 0 6 -3.34 3.66 2.44 0.020 0.80 -1 7 6 131.53 100.12 2.41 0.104 0.81 2 0 11 -0.92 3.82 2.38 0.020 1.07 2 0 6 138.08 112.69 2.37 0.110 1.69 -1 0 10 12.87 22.61 2.35 0.049 1.13 6 0 0 5.21 0.13 2.35 0.004 0.81 -2 2 0 403.09 353.25 2.35 0.196 1.81 1 0 1 2761.95 3037.16 2.34 0.573 4.80 4 0 1 18.66 10.79 2.34 0.034 1.23 5 0 10 -1.63 1.76 2.34 0.014 0.83 1 5 13 25.04 13.04 2.31 0.038 0.78 -4 1 2 13.79 23.02 2.31 0.050 1.11 2 -2 2 653.95 581.85 2.30 0.251 1.81 3 -4 8 28.14 15.37 2.29 0.041 0.93 5 -1 9 23.30 11.12 2.28 0.035 0.84 2 -6 5 6.84 16.06 2.28 0.042 0.91 Bond lengths and angles C1 - Distance Angles C2 1.3863 (0.0036) C6 1.3949 (0.0035) 120.09 (0.23) N1 1.4195 (0.0031) 121.85 (0.22) 118.02 (0.23) C1 - C2 C6 C2 - Distance Angles C3 1.3817 (0.0035) C1 1.3863 (0.0036) 119.66 (0.24) H2 0.9500 120.17 120.17 C2 - C3 C1 C3 - Distance Angles C2 1.3817 (0.0035) C4 1.3959 (0.0034) 120.81 (0.25) H3 0.9500 119.60 119.60 C3 - C2 C4 C4 - Distance Angles C5 1.3936 (0.0036) C3 1.3959 (0.0034) 119.25 (0.23) C9 1.4772 (0.0033) 119.67 (0.22) 121.08 (0.23) C4 - C5 C3 C5 - Distance Angles C6 1.3849 (0.0036) C4 1.3936 (0.0036) 120.06 (0.24) H5 0.9500 119.97 119.97 C5 - C6 C4 C6 - Distance Angles C5 1.3849 (0.0036) C1 1.3949 (0.0035) 120.11 (0.24) H6 0.9500 119.95 119.95 C6 - C5 C1 C7 - Distance Angles O1 1.2318 (0.0031) N1 1.3533 (0.0033) 123.50 (0.24) C8 1.5084 (0.0035) 121.28 (0.24) 115.21 (0.23) C7 - O1 N1 C8 - Distance Angles C7 1.5084 (0.0035) 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 O3 1.2407 (0.0030) O2 1.3017 (0.0031) 123.60 (0.23) C4 1.4772 (0.0033) 121.05 (0.23) 115.36 (0.21) C9 - O3 O2 N1 - Distance Angles C7 1.3533 (0.0033) C1 1.4195 (0.0031) 125.15 (0.22) H1N 0.8769 (0.0178) 119.26 (2.22) 115.21 (2.20) N1 - C7 C1 O1 - Distance Angles C7 1.2318 (0.0031) O1 - O2 - Distance Angles C9 1.3017 (0.0031) H2O 0.8670 (0.0193) 111.27 (3.16) O2 - C9 O3 - Distance Angles C9 1.2407 (0.0030) O3 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.877(18) 2.073(18) 2.949(3) 176(3) N1-H1N...O1_$1 0.867(19) 1.76(2) 2.623(3) 175(5) O2-H2O...O3_$2 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)