+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 11:05:52 on 23-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009lsh011 in Cc CELL 0.71073 3.8456 22.1895 9.4477 90.000 90.048 90.000 ZERR 4.00 0.0010 0.0045 0.0024 0.000 0.015 0.000 LATT -7 SYMM X, - Y, 1/2 + Z SFAC C H N O UNIT 36 32 8 4 V = 806.19 F(000) = 336.0 Mu = 0.09 mm-1 Cell Wt = 640.70 Rho = 1.320 MERG 2 OMIT -3.00 50.00 TWIN DFIX 1.4 0.02 N1A C7A ISOR 0.01 N1B ISOR 0.005 N1A FMAP 2 PLAN 5 SIZE 0.01 0.02 0.38 EQIV $1 x, -y+1, z+1/2 EQIV $2 x, -y+1, z-1/2 HTAB N1A O1A_$1 HTAB N1B O1B_$2 HTAB BOND $H ACTA L.S. 12 TEMP -153.00 WGHT 0.0412 0.9056 BASF 2.27401 FVAR 0.72228 0.50513 C1 1 0.874623 0.599420 0.098969 11.00000 0.04176 0.02232 = 0.05518 0.00017 0.00339 -0.00493 C2 1 0.796458 0.627981 -0.028647 11.00000 0.03987 0.02910 = 0.04370 -0.00277 0.00281 -0.00370 AFIX 43 H2 2 0.850858 0.609028 -0.116031 11.00000 -1.20000 AFIX 0 C3 1 0.640031 0.683792 -0.027319 11.00000 0.05571 0.02601 = 0.04140 0.00442 0.00166 -0.00129 AFIX 43 H3 2 0.585367 0.702929 -0.114491 11.00000 -1.20000 AFIX 0 C4 1 0.561281 0.712410 0.098023 11.00000 0.03499 0.02783 = 0.04655 -0.00108 0.00002 -0.00556 C5 1 0.637830 0.683491 0.226635 11.00000 0.05480 0.02376 = 0.03941 -0.00583 0.00294 -0.00149 AFIX 43 H5 2 0.582099 0.702572 0.313724 11.00000 -1.20000 AFIX 0 C6 1 0.792790 0.627787 0.226900 11.00000 0.04788 0.02666 = 0.04713 0.00517 -0.00456 -0.00167 AFIX 43 H6 2 0.844589 0.608453 0.314121 11.00000 -1.20000 AFIX 0 PART 1 C7A 1 1.131163 0.503213 0.015255 21.00000 0.05947 0.02292 = 0.05618 0.00212 0.00265 0.00023 C8A 1 1.313997 0.446563 0.068631 21.00000 0.07318 0.03086 = 0.04661 -0.00324 -0.00613 0.00200 AFIX 137 H8A1 2 1.485701 0.433376 -0.001423 21.00000 -1.50000 H8A2 2 1.142214 0.414545 0.083246 21.00000 -1.50000 H8A3 2 1.431504 0.455385 0.158353 21.00000 -1.50000 AFIX 0 N1A 3 1.047474 0.542945 0.122450 21.00000 0.04244 0.02997 = 0.03291 -0.00297 0.00020 -0.00344 AFIX 43 H1A 2 1.103068 0.533122 0.209827 21.00000 -1.20000 AFIX 0 O1A 4 1.069011 0.513426 -0.109113 21.00000 0.06138 0.03460 = 0.04097 -0.00172 -0.01018 0.00380 PART 2 SAME C7A > O1A C7B 1 1.126485 0.503554 0.181066 -21.00000 0.05145 0.02876 = 0.04562 0.00775 -0.00480 -0.01672 C8B 1 1.313221 0.446866 0.129642 -21.00000 0.03740 0.02682 = 0.05784 -0.00301 0.00062 0.00129 AFIX 137 H8B1 2 1.166637 0.411545 0.147421 -21.00000 -1.50000 H8B2 2 1.533819 0.442432 0.180596 -21.00000 -1.50000 H8B3 2 1.358979 0.450261 0.027927 -21.00000 -1.50000 AFIX 0 N1B 3 1.035966 0.542206 0.074869 -21.00000 0.05467 0.02187 = 0.03171 0.00660 -0.01329 -0.00794 AFIX 43 H1B 2 1.079041 0.531389 -0.012997 -21.00000 -1.20000 AFIX 0 O1B 4 1.073868 0.512563 0.305996 -21.00000 0.07550 0.03133 = 0.04364 0.00354 0.00274 -0.00622 PART 0 C9 1 0.402132 0.771184 0.099101 11.00000 0.04445 0.03210 = 0.03862 -0.00281 -0.00626 -0.00328 N2 3 0.280677 0.818342 0.099431 11.00000 0.06608 0.03189 = 0.05554 -0.00061 0.00102 0.00213 HKLF 4 Covalent radii and connectivity table for 2009lsh011 in Cc C 0.770 H 0.320 N 0.700 O 0.660 C1 - C2 C6 N1B_b N1A_a C2 - C3 C1 C3 - C2 C4 C4 - C3 C5 C9 C5 - C6 C4 C6 - C5 C1 C7A_a - O1A_a N1A_a C8A_a C8A_a - C7A_a N1A_a - C7A_a C1 O1A_a - C7A_a C7B_b - O1B_b N1B_b C8B_b C8B_b - C7B_b N1B_b - C7B_b C1 O1B_b - C7B_b C9 - N2 C4 N2 - C9 Operators for generating equivalent atoms: $1 x, -y+1, z+1/2 $2 x, -y+1, z-1/2 Floating origin restraints generated 4221 Reflections read, of which 497 rejected -4 =< h =< 4, -26 =< k =< 26, -11 =< l =< 11, Max. 2-theta = 49.97 0 Systematic absence violations 0 Inconsistent equivalents 1348 Unique reflections, of which 0 suppressed R(int) = 0.0811 R(sigma) = 0.0971 Friedel opposites not merged Maximum memory for data reduction = 1674 / 16171 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 = 2087 / 186746 wR2 = 0.1679 before cycle 1 for 1348 data and 149 / 149 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 6. 0. 0. 0. 0. 0. 12. 0. rms sigma 0.000 0.020 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.008 0.000 rms deviation 0.000 0.019 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.009 0.000 GooF = S = 1.134; Restrained GooF = 1.131 for 21 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0412 * P )^2 + 0.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72227 0.00345 -0.004 OSF 2 0.50506 0.01339 -0.006 FVAR 2 3 2.25658 5.95461 -0.003 BASF 1 Mean shift/esd = 0.004 Maximum = -0.026 for y N2 Max. shift = 0.001 A for H8A2_a Max. dU = 0.000 for C7A_a Least-squares cycle 2 Maximum vector length = 511 Memory required = 2087 / 186746 wR2 = 0.1680 before cycle 2 for 1348 data and 149 / 149 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 6. 0. 0. 0. 0. 0. 12. 0. rms sigma 0.000 0.020 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.008 0.000 rms deviation 0.000 0.019 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.009 0.000 GooF = S = 1.134; Restrained GooF = 1.131 for 21 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0412 * P )^2 + 0.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72226 0.00345 -0.003 OSF 2 0.50504 0.01339 -0.001 FVAR 2 3 2.24825 5.95509 -0.001 BASF 1 Mean shift/esd = 0.001 Maximum = -0.008 for y N2 Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C7A_a Least-squares cycle 3 Maximum vector length = 511 Memory required = 2087 / 186746 wR2 = 0.1679 before cycle 3 for 1348 data and 149 / 149 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 6. 0. 0. 0. 0. 0. 12. 0. rms sigma 0.000 0.020 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.008 0.000 rms deviation 0.000 0.019 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.009 0.000 GooF = S = 1.134; Restrained GooF = 1.131 for 21 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0412 * P )^2 + 0.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72226 0.00345 0.000 OSF 2 0.50503 0.01339 0.000 FVAR 2 3 2.24724 5.95480 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.001 for U33 C5 Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C8A_a Least-squares cycle 4 Maximum vector length = 511 Memory required = 2087 / 186746 wR2 = 0.1679 before cycle 4 for 1348 data and 149 / 149 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 6. 0. 0. 0. 0. 0. 12. 0. rms sigma 0.000 0.020 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.008 0.000 rms deviation 0.000 0.019 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.009 0.000 GooF = S = 1.134; Restrained GooF = 1.131 for 21 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0412 * P )^2 + 0.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72226 0.00345 0.000 OSF 2 0.50503 0.01339 0.000 FVAR 2 3 2.24717 5.95490 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.001 for y N1B_b Max. shift = 0.000 A for H8B1_b Max. dU = 0.000 for N1A_a Least-squares cycle 5 Maximum vector length = 511 Memory required = 2087 / 186746 wR2 = 0.1679 before cycle 5 for 1348 data and 149 / 149 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 6. 0. 0. 0. 0. 0. 12. 0. rms sigma 0.000 0.020 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.008 0.000 rms deviation 0.000 0.019 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.009 0.000 GooF = S = 1.134; Restrained GooF = 1.131 for 21 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0412 * P )^2 + 0.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72226 0.00345 0.000 OSF 2 0.50503 0.01339 0.000 FVAR 2 3 2.24570 5.95481 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for BASF 1 Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C8A_a Least-squares cycle 6 Maximum vector length = 511 Memory required = 2087 / 186746 wR2 = 0.1679 before cycle 6 for 1348 data and 149 / 149 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 6. 0. 0. 0. 0. 0. 12. 0. rms sigma 0.000 0.020 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.008 0.000 rms deviation 0.000 0.019 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.009 0.000 GooF = S = 1.134; Restrained GooF = 1.131 for 21 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0412 * P )^2 + 0.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72226 0.00345 0.000 OSF 2 0.50503 0.01339 0.000 FVAR 2 3 2.24528 5.95486 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for y C9 Max. shift = 0.000 A for H8B1_b Max. dU = 0.000 for C7B_b Least-squares cycle 7 Maximum vector length = 511 Memory required = 2087 / 186746 wR2 = 0.1679 before cycle 7 for 1348 data and 149 / 149 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 6. 0. 0. 0. 0. 0. 12. 0. rms sigma 0.000 0.020 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.008 0.000 rms deviation 0.000 0.019 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.009 0.000 GooF = S = 1.134; Restrained GooF = 1.131 for 21 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0412 * P )^2 + 0.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72226 0.00345 0.000 OSF 2 0.50503 0.01339 0.000 FVAR 2 3 2.24647 5.95475 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for BASF 1 Max. shift = 0.000 A for H8B1_b Max. dU = 0.000 for N1A_a Least-squares cycle 8 Maximum vector length = 511 Memory required = 2087 / 186746 wR2 = 0.1679 before cycle 8 for 1348 data and 149 / 149 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 6. 0. 0. 0. 0. 0. 12. 0. rms sigma 0.000 0.020 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.008 0.000 rms deviation 0.000 0.019 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.009 0.000 GooF = S = 1.134; Restrained GooF = 1.131 for 21 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0412 * P )^2 + 0.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72226 0.00345 0.000 OSF 2 0.50503 0.01339 0.000 FVAR 2 3 2.24502 5.95488 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for BASF 1 Max. shift = 0.000 A for H8A1_a Max. dU = 0.000 for C8A_a Least-squares cycle 9 Maximum vector length = 511 Memory required = 2087 / 186746 wR2 = 0.1679 before cycle 9 for 1348 data and 149 / 149 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 6. 0. 0. 0. 0. 0. 12. 0. rms sigma 0.000 0.020 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.008 0.000 rms deviation 0.000 0.019 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.009 0.000 GooF = S = 1.134; Restrained GooF = 1.131 for 21 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0412 * P )^2 + 0.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72226 0.00345 0.000 OSF 2 0.50503 0.01339 0.000 FVAR 2 3 2.24573 5.95474 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for y C9 Max. shift = 0.000 A for H8A3_a Max. dU = 0.000 for N1B_b Least-squares cycle 10 Maximum vector length = 511 Memory required = 2087 / 186746 wR2 = 0.1680 before cycle 10 for 1348 data and 149 / 149 parameters Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 6. 0. 0. 0. 0. 0. 12. 0. rms sigma 0.000 0.020 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.008 0.000 rms deviation 0.000 0.019 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.009 0.000 GooF = S = 1.134; Restrained GooF = 1.131 for 21 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0412 * P )^2 + 0.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72226 0.00345 0.000 OSF 2 0.50503 0.01339 0.000 FVAR 2 3 2.24620 5.95495 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for y C9 Max. shift = 0.000 A for H8B1_b Max. dU = 0.000 for N1A_a Least-squares cycle 11 Maximum vector length = 511 Memory required = 2087 / 186746 wR2 = 0.1679 before cycle 11 for 1348 data and 149 / 149 parameters Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 6. 0. 0. 0. 0. 0. 12. 0. rms sigma 0.000 0.020 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.008 0.000 rms deviation 0.000 0.019 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.009 0.000 GooF = S = 1.134; Restrained GooF = 1.131 for 21 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0412 * P )^2 + 0.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72226 0.00345 0.000 OSF 2 0.50503 0.01339 0.000 FVAR 2 3 2.24597 5.95500 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for y C9 Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C8A_a Least-squares cycle 12 Maximum vector length = 511 Memory required = 2087 / 186746 wR2 = 0.1679 before cycle 12 for 1348 data and 149 / 149 parameters Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 6. 0. 0. 0. 0. 0. 12. 0. rms sigma 0.000 0.020 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.008 0.000 rms deviation 0.000 0.019 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.009 0.000 GooF = S = 1.134; Restrained GooF = 1.131 for 21 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0412 * P )^2 + 0.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72226 0.00345 0.000 OSF 2 0.50503 0.01339 0.000 FVAR 2 3 2.24462 5.95474 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for BASF 1 Max. shift = 0.000 A for H8A3_a Max. dU = 0.000 for N1A_a Largest correlation matrix elements -0.851 y C8B_b / y C8A_a 0.738 U23 C8B_b / U23 C8A_a -0.674 y O1B_b / y O1A_a -0.844 y N1B_b / y N1A_a 0.734 U23 O1B_b / U23 O1A_a -0.656 U13 C8B_b / x C8B_b -0.832 x C8B_b / x C8A_a 0.730 U23 C8B_b / y C8A_a 0.644 U23 C8A_a / y C8A_a -0.819 x N1B_b / x N1A_a -0.727 U13 N1B_b / x N1A_a -0.639 U23 C8B_b / y C8B_b -0.804 U22 C8B_b / U22 C8A_a -0.711 y C8B_b / U23 C8A_a -0.636 U23 N1B_b / y N1A_a -0.803 U22 N1B_b / U22 N1A_a -0.707 U11 C8B_b / U11 C8A_a -0.628 U33 C7B_b / U33 C7A_a 0.780 U13 C8B_b / x C8A_a 0.688 x N1B_b / U13 N1A_a 0.613 U13 C8A_a / x C8A_a -0.740 x C8B_b / U13 C8A_a 0.674 z N1B_b / U33 N1A_a 0.610 z O1B_b / z O1A_a Idealized hydrogen atom generation before cycle 13 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.8509 0.6090 -0.1160 43 0.950 0.000 C2 C3 C1 H3 0.5854 0.7029 -0.1145 43 0.950 0.000 C3 C2 C4 H5 0.5821 0.7026 0.3137 43 0.950 0.000 C5 C6 C4 H6 0.8446 0.6085 0.3141 43 0.950 0.000 C6 C5 C1 H8A1 1.4858 0.4334 -0.0014 137 0.980 0.000 C8A_a C7A_a H8A1_a H8A2 1.1422 0.4145 0.0832 137 0.980 0.000 C8A_a C7A_a H8A1_a H8A3 1.4314 0.4554 0.1584 137 0.980 0.000 C8A_a C7A_a H8A1_a H1A 1.1030 0.5331 0.2098 43 0.880 0.000 N1A_a C7A_a C1 H8B1 1.1666 0.4115 0.1474 137 0.980 0.000 C8B_b C7B_b H8B1_b H8B2 1.5337 0.4424 0.1806 137 0.980 0.000 C8B_b C7B_b H8B1_b H8B3 1.3591 0.4503 0.0279 137 0.980 0.000 C8B_b C7B_b H8B1_b H1B 1.0791 0.5314 -0.0130 43 0.880 0.000 N1B_b C7B_b C1 2009lsh011 in Cc ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.87462 0.59942 0.09898 1.00000 0.04175 0.02231 0.05518 0.00017 0.00341 -0.00492 0.03975 0.00894 0.00121 0.00016 0.00067 0.00000 0.00363 0.00220 0.00312 0.00267 0.00319 0.00225 0.00135 C2 0.79646 0.62798 -0.02865 1.00000 0.03990 0.02907 0.04371 -0.00275 0.00282 -0.00368 0.03756 0.00961 0.00120 0.00021 0.00067 0.00000 0.00327 0.00277 0.00325 0.00245 0.00244 0.00222 0.00126 H2 0.85086 0.60902 -0.11603 1.00000 0.04508 0.00000 0.00000 C3 0.64002 0.68379 -0.02732 1.00000 0.05569 0.02600 0.04140 0.00443 0.00165 -0.00130 0.04103 0.00867 0.00123 0.00021 0.00060 0.00000 0.00372 0.00278 0.00372 0.00251 0.00297 0.00258 0.00146 H3 0.58536 0.70293 -0.11449 1.00000 0.04924 0.00000 0.00000 C4 0.56127 0.71241 0.09802 1.00000 0.03500 0.02781 0.04655 -0.00108 0.00003 -0.00556 0.03645 0.00903 0.00129 0.00016 0.00071 0.00000 0.00285 0.00222 0.00274 0.00311 0.00251 0.00228 0.00111 C5 0.63783 0.68349 0.22664 1.00000 0.05479 0.02373 0.03942 -0.00584 0.00296 -0.00149 0.03931 0.00841 0.00119 0.00021 0.00058 0.00000 0.00373 0.00272 0.00372 0.00241 0.00291 0.00251 0.00143 H5 0.58210 0.70258 0.31372 1.00000 0.04717 0.00000 0.00000 C6 0.79281 0.62778 0.22690 1.00000 0.04788 0.02664 0.04712 0.00516 -0.00457 -0.00167 0.04055 0.00927 0.00129 0.00021 0.00069 0.00000 0.00348 0.00272 0.00333 0.00253 0.00257 0.00227 0.00131 H6 0.84462 0.60845 0.31412 1.00000 0.04866 0.00000 0.00000 C7A_a 1.13114 0.50321 0.01526 0.50503 0.05938 0.02289 0.05612 0.00207 0.00262 0.00017 0.04613 0.01976 0.00300 0.00046 0.00116 0.01339 0.00818 0.00645 0.01026 0.00590 0.00613 0.00510 0.00385 C8A_a 1.31399 0.44656 0.06862 0.50503 0.07316 0.03088 0.04655 -0.00321 -0.00614 0.00200 0.05020 0.04430 0.00703 0.00083 0.00174 0.01339 0.01251 0.00838 0.01131 0.00767 0.01039 0.00636 0.00535 H8A1_a 1.48581 0.43339 -0.00141 0.50503 0.07530 0.01339 0.00000 H8A2_a 1.14223 0.41453 0.08315 0.50503 0.07530 0.01339 0.00000 H8A3_a 1.43135 0.45536 0.15838 0.50503 0.07530 0.01339 0.00000 N1A_a 1.04744 0.54294 0.12246 0.50503 0.04247 0.03000 0.03291 -0.00296 0.00021 -0.00345 0.03513 0.02691 0.00461 0.00069 0.00161 0.01339 0.00572 0.00615 0.00616 0.00416 0.00458 0.00371 0.00473 H1A_a 1.10300 0.53311 0.20984 0.50503 0.04215 0.01339 0.00000 O1A_a 1.06902 0.51343 -0.10911 0.50503 0.06141 0.03456 0.04094 -0.00175 -0.01017 0.00381 0.04564 0.01703 0.00196 0.00040 0.00105 0.01339 0.00552 0.00470 0.00557 0.00514 0.00372 0.00346 0.00280 C7B_b 1.12646 0.50355 0.18107 0.49497 0.05141 0.02877 0.04570 0.00776 -0.00482 -0.01673 0.04196 0.01766 0.00284 0.00046 0.00110 0.01339 0.00775 0.00705 0.00969 0.00579 0.00574 0.00522 0.00382 C8B_b 1.31323 0.44687 0.12964 0.49497 0.03742 0.02676 0.05786 -0.00304 0.00060 0.00129 0.04068 0.03809 0.00564 0.00074 0.00192 0.01339 0.00892 0.00788 0.01207 0.00792 0.00939 0.00541 0.00442 H8B1_b 1.16658 0.41155 0.14735 0.49497 0.06102 0.01339 0.00000 H8B2_b 1.53374 0.44242 0.18065 0.49497 0.06102 0.01339 0.00000 H8B3_b 1.35914 0.45028 0.02794 0.49497 0.06102 0.01339 0.00000 N1B_b 1.03600 0.54221 0.07488 0.49497 0.05466 0.02182 0.03167 0.00660 -0.01329 -0.00793 0.03606 0.03163 0.00468 0.00065 0.00170 0.01339 0.00700 0.00638 0.00706 0.00509 0.00613 0.00457 0.00425 H1B_b 1.07913 0.53140 -0.01299 0.49497 0.04327 0.01339 0.00000 O1B_b 1.07388 0.51256 0.30601 0.49497 0.07551 0.03138 0.04363 0.00351 0.00274 -0.00623 0.05017 0.01398 0.00218 0.00041 0.00111 0.01339 0.00640 0.00473 0.00614 0.00503 0.00411 0.00376 0.00292 C9 0.40214 0.77118 0.09910 1.00000 0.04446 0.03205 0.03863 -0.00282 -0.00625 -0.00327 0.03838 0.00901 0.00132 0.00019 0.00068 0.00000 0.00331 0.00251 0.00280 0.00254 0.00273 0.00235 0.00126 N2 0.28067 0.81834 0.09943 1.00000 0.06606 0.03191 0.05554 -0.00062 0.00102 0.00212 0.05117 0.00884 0.00121 0.00017 0.00067 0.00000 0.00338 0.00204 0.00259 0.00285 0.00263 0.00238 0.00124 Final Structure Factor Calculation for 2009lsh011 in Cc Total number of l.s. parameters = 149 Maximum vector length = 511 Memory required = 1940 / 25046 wR2 = 0.1679 before cycle 13 for 1348 data and 2 / 149 parameters Summary of restraints applied in cycle 13 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 6. 0. 0. 0. 0. 0. 12. 0. rms sigma 0.000 0.020 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.008 0.000 rms deviation 0.000 0.019 0.000 0.015 0.000 0.000 0.000 0.000 0.000 0.009 0.000 GooF = S = 1.134; Restrained GooF = 1.131 for 21 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0412 * P )^2 + 0.91 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0699 for 893 Fo > 4sig(Fo) and 0.1246 for all 1348 data wR2 = 0.1679, GooF = S = 1.134, Restrained GooF = 1.131 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 0.0560 0.0421 0.0211 C1 0.0462 0.0388 0.0277 C2 0.0559 0.0425 0.0247 C3 0.0466 0.0380 0.0247 C4 0.0555 0.0406 0.0218 C5 0.0530 0.0432 0.0254 C6 0.0608 0.0548 0.0228 C7A_a 0.0747 0.0457 0.0302 C8A_a 0.0434 0.0343 0.0276 N1A_a 0.0662 0.0367 0.0340 O1A_a 0.0639 0.0430 0.0191 C7B_b 0.0582 0.0376 0.0263 C8B_b 0.0632 0.0265 0.0185 N1B_b 0.0765 0.0445 0.0295 O1B_b 0.0486 0.0376 0.0290 C9 0.0663 0.0555 0.0318 N2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.015 0.026 0.032 0.041 0.053 0.065 0.081 0.104 0.144 1.000 Number in group 141. 130. 148. 132. 127. 137. 129. 134. 134. 136. GooF 1.173 1.166 1.218 1.225 1.220 1.070 1.138 0.934 0.981 1.174 K 2.505 0.774 0.954 0.870 1.070 0.993 0.977 1.014 1.014 1.026 Resolution(A) 0.84 0.87 0.91 0.95 1.01 1.07 1.15 1.26 1.47 1.81 inf Number in group 141. 138. 126. 138. 134. 138. 128. 139. 131. 135. GooF 1.294 1.233 1.188 1.199 1.142 0.980 1.034 1.089 0.959 1.165 K 1.022 1.133 1.083 1.037 0.974 1.011 1.003 0.979 1.061 1.013 R1 0.296 0.293 0.317 0.167 0.135 0.082 0.077 0.093 0.053 0.037 Recommended weighting scheme: WGHT 0.0411 0.9029 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 5 -8 139.19 41.95 4.07 0.051 0.85 -1 25 -2 148.30 48.74 3.68 0.055 0.85 0 12 0 426.93 329.57 3.47 0.142 1.85 0 4 -4 1641.26 1295.89 3.08 0.281 2.17 -4 0 4 126.60 11.86 3.04 0.027 0.89 -2 22 1 41.82 4.79 3.02 0.017 0.89 -4 0 -2 -3.56 22.53 2.97 0.037 0.94 0 14 -4 24.64 3.58 2.95 0.015 1.32 1 17 6 -4.63 11.75 2.91 0.027 0.97 -3 15 -2 32.70 2.68 2.88 0.013 0.95 -2 8 -8 211.23 140.31 2.74 0.092 0.95 0 12 8 45.25 83.63 2.73 0.071 1.00 -3 5 0 40.83 70.92 2.69 0.066 1.23 3 15 2 38.05 2.64 2.59 0.013 0.95 0 14 -3 19.03 45.33 2.59 0.053 1.42 -2 6 1 3045.19 2546.64 2.53 0.394 1.68 0 10 -6 33.66 2.15 2.51 0.011 1.28 0 10 -8 -10.08 8.82 2.48 0.023 1.04 0 12 -10 59.41 2.30 2.47 0.012 0.84 0 6 0 1894.93 2162.20 2.43 0.363 3.70 0 10 6 42.42 2.15 2.37 0.011 1.28 -1 5 -3 1001.61 807.27 2.36 0.222 2.14 -4 10 0 84.36 52.71 2.35 0.057 0.88 -3 19 2 -12.06 10.60 2.33 0.025 0.85 -1 19 -6 76.49 18.82 2.30 0.034 0.91 2 18 5 47.25 13.94 2.28 0.029 0.91 1 17 7 23.73 53.87 2.28 0.057 0.91 0 16 -6 23.08 50.81 2.27 0.056 1.04 -2 20 4 -29.67 18.48 2.24 0.034 0.89 -2 12 -4 227.60 321.69 2.24 0.140 1.16 3 7 4 -7.15 55.32 2.23 0.058 1.06 0 20 -2 11.35 51.91 2.23 0.056 1.08 0 22 2 348.77 240.71 2.22 0.121 0.99 -3 7 5 43.12 16.66 2.21 0.032 1.01 3 7 -6 76.22 29.91 2.20 0.043 0.95 -2 18 6 -29.99 17.15 2.18 0.032 0.87 -3 5 4 109.85 78.79 2.17 0.069 1.09 3 7 -3 -17.60 19.45 2.17 0.034 1.11 2 20 3 65.93 22.56 2.16 0.037 0.92 -4 4 1 22.78 4.96 2.16 0.017 0.94 1 1 -9 15.75 38.10 2.14 0.048 1.01 -3 3 -1 70.84 99.48 2.13 0.078 1.25 0 12 -8 52.26 83.62 2.13 0.071 1.00 -3 5 -1 29.52 49.51 2.10 0.055 1.22 0 22 -6 15.16 39.41 2.10 0.049 0.85 0 18 3 1757.75 1526.18 2.10 0.305 1.15 2 14 1 -11.15 6.05 2.09 0.019 1.21 3 13 4 66.79 25.95 2.07 0.040 0.94 -3 7 2 5.00 24.75 2.06 0.039 1.15 2 12 0 53.96 83.34 2.06 0.071 1.33 Bond lengths and angles C1 - Distance Angles C2 1.3947 (0.0082) C6 1.3987 (0.0082) 119.61 (0.36) N1B_b 1.4314 (0.0156) 111.01 (0.74) 129.38 (0.77) N1A_a 1.4357 (0.0160) 129.02 (0.73) 111.33 (0.72) 18.14 (0.72) C1 - C2 C6 N1B_b C2 - Distance Angles C3 1.3770 (0.0071) C1 1.3947 (0.0082) 119.64 (0.49) H2 0.9500 120.18 120.18 C2 - C3 C1 C3 - Distance Angles C2 1.3770 (0.0072) C4 1.3776 (0.0072) 121.25 (0.46) H3 0.9500 119.37 119.37 C3 - C2 C4 C4 - Distance Angles C3 1.3776 (0.0072) C5 1.4051 (0.0073) 119.13 (0.37) C9 1.4407 (0.0063) 121.13 (0.52) 119.73 (0.51) C4 - C3 C5 C5 - Distance Angles C6 1.3723 (0.0071) C4 1.4051 (0.0073) 120.24 (0.44) H5 0.9500 119.88 119.88 C5 - C6 C4 C6 - Distance Angles C5 1.3723 (0.0071) C1 1.3987 (0.0082) 120.12 (0.50) H6 0.9500 119.94 119.94 C6 - C5 C1 C7A_a - Distance Angles O1A_a 1.2201 (0.0110) N1A_a 1.3809 (0.0109) 122.83 (1.14) C8A_a 1.5259 (0.0128) 124.12 (1.02) 113.03 (1.18) C7A_a - O1A_a N1A_a C8A_a - Distance Angles C7A_a 1.5259 (0.0128) H8A1_a 0.9800 109.47 H8A2_a 0.9800 109.47 109.47 H8A3_a 0.9800 109.47 109.47 109.47 C8A_a - C7A_a H8A1_a H8A2_a N1A_a - Distance Angles C7A_a 1.3809 (0.0109) C1 1.4357 (0.0160) 123.51 (1.32) H1A_a 0.8800 118.25 118.25 N1A_a - C7A_a C1 O1A_a - Distance Angles C7A_a 1.2201 (0.0110) O1A_a - C7B_b - Distance Angles O1B_b 1.2143 (0.0114) N1B_b 1.3648 (0.0127) 124.65 (1.24) C8B_b 1.5280 (0.0125) 121.56 (1.06) 113.78 (1.18) C7B_b - O1B_b N1B_b C8B_b - Distance Angles C7B_b 1.5280 (0.0125) H8B1_b 0.9800 109.47 H8B2_b 0.9800 109.47 109.47 H8B3_b 0.9800 109.47 109.47 109.47 C8B_b - C7B_b H8B1_b H8B2_b N1B_b - Distance Angles C7B_b 1.3648 (0.0127) C1 1.4314 (0.0155) 123.42 (1.41) H1B_b 0.8800 118.29 118.29 N1B_b - C7B_b C1 O1B_b - Distance Angles C7B_b 1.2143 (0.0114) O1B_b - C9 - Distance Angles N2 1.1458 (0.0051) C4 1.4407 (0.0063) 178.89 (0.57) C9 - N2 N2 - Distance Angles C9 1.1458 (0.0051) N2 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 2.00 2.829(18) 155.9 N1A_a-H1A_a...O1A_$1a 0.88 1.97 2.820(19) 162.3 N1B_b-H1B_b...O1B_$2b Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)