+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 14:08:26 on 17-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh001 in Pbca CELL 0.71073 9.6630 9.2888 19.8221 90.000 90.000 90.000 ZERR 8.00 0.0003 0.0002 0.0005 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 F UNIT 72 64 8 8 24 V = 1779.19 F(000) = 832.0 Mu = 0.14 mm-1 Cell Wt = 1625.31 Rho = 1.517 MERG 2 OMIT -3.00 55.00 OMIT 1 2 3 EADP C7A C7B EADP C8A C8B EADP N1A N1B EADP O1A O1B EQIV $1 x-1/2, y, -z+3/2 EQIV $2 x+1/2, y, -z+3/2 HTAB N1A O1A_$1 HTAB N1B O1B_$2 FMAP 2 PLAN 5 SIZE 0.16 0.16 0.50 ACTA HTAB 2.00000 BOND $H WGHT 0.04800 2.03860 L.S. 16 TEMP -153.00 FVAR 0.24369 0.83032 C1 1 0.750867 0.362357 0.656273 11.00000 0.01638 0.01840 = 0.01768 0.00284 0.00033 -0.00046 C2 1 0.875609 0.319917 0.627377 11.00000 0.01661 0.02908 = 0.02644 -0.00319 -0.00027 -0.00180 AFIX 43 H2 2 0.960678 0.353967 0.645338 11.00000 -1.20000 AFIX 0 C3 1 0.875508 0.227446 0.572087 11.00000 0.01751 0.02748 = 0.02534 -0.00162 0.00184 0.00279 AFIX 43 H3 2 0.960695 0.198980 0.552226 11.00000 -1.20000 AFIX 0 C4 1 0.751582 0.176612 0.545820 11.00000 0.02195 0.01661 = 0.02007 0.00233 0.00074 0.00114 C5 1 0.627729 0.214870 0.576204 11.00000 0.01775 0.02713 = 0.02743 -0.00175 -0.00231 -0.00167 AFIX 43 H5 2 0.542997 0.177419 0.559388 11.00000 -1.20000 AFIX 0 C6 1 0.626964 0.307295 0.630874 11.00000 0.01369 0.02946 = 0.02598 -0.00290 0.00098 -0.00130 AFIX 43 H6 2 0.541632 0.333479 0.651268 11.00000 -1.20000 AFIX 0 C9 1 0.751967 0.090661 0.482275 11.00000 0.02159 0.02044 = 0.02323 0.00156 0.00000 -0.00153 PART 1 C7A 1 0.843042 0.518482 0.747933 21.00000 0.02070 0.02315 = 0.01871 0.00249 -0.00301 -0.00124 C8A 1 0.795035 0.620553 0.802476 21.00000 0.02721 0.03315 = 0.02504 -0.00540 -0.00172 0.00178 AFIX 137 H8A1 2 0.835638 0.591954 0.845753 21.00000 -1.50000 H8A2 2 0.693886 0.617226 0.805718 21.00000 -1.50000 H8A3 2 0.824445 0.718683 0.791333 21.00000 -1.50000 AFIX 0 N1A 3 0.739025 0.460002 0.709942 21.00000 0.01142 0.02302 = 0.02019 -0.00098 -0.00080 -0.00005 AFIX 43 H1A 2 0.654418 0.486926 0.720458 21.00000 -1.20000 AFIX 0 O1A 4 0.965967 0.490789 0.738962 21.00000 0.01318 0.04102 = 0.03274 -0.00535 -0.00532 0.00182 PART 2 SAME C7A > O1A C7B 1 0.658133 0.519556 0.748283 -21.00000 0.02070 0.02315 = 0.01871 0.00249 -0.00301 -0.00124 C8B 1 0.707803 0.626667 0.801163 -21.00000 0.02721 0.03315 = 0.02504 -0.00540 -0.00172 0.00178 AFIX 137 H8B1 2 0.809070 0.624204 0.803596 -21.00000 -1.50000 H8B2 2 0.668917 0.600982 0.845210 -21.00000 -1.50000 H8B3 2 0.677387 0.723745 0.788715 -21.00000 -1.50000 AFIX 0 N1B 3 0.765270 0.462375 0.712419 -21.00000 0.01142 0.02302 = 0.02019 -0.00098 -0.00080 -0.00005 AFIX 43 H1BN 2 0.849640 0.487877 0.724102 -21.00000 -1.20000 AFIX 0 O1B 4 0.535429 0.491575 0.739462 -21.00000 0.01318 0.04102 = 0.03274 -0.00535 -0.00532 0.00182 PART 0 F1 5 0.762152 0.175013 0.427355 11.00000 0.09268 0.03062 = 0.01965 0.00295 0.00055 -0.00169 F2 5 0.638341 0.012895 0.473272 11.00000 0.03677 0.05114 = 0.04288 -0.02238 0.00657 -0.01707 F3 5 0.858485 -0.000412 0.477979 11.00000 0.04050 0.04788 = 0.04220 -0.01985 -0.01082 0.02378 HKLF 4 Covalent radii and connectivity table for 2008lsh001 in Pbca C 0.770 H 0.320 N 0.700 O 0.660 F 0.640 C1 - C2 C6 N1A_a N1B_b C2 - C1 C3 C3 - C4 C2 C4 - C5 C3 C9 C5 - C6 C4 C6 - C5 C1 C9 - F2 F3 F1 C4 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 F1 - C9 F2 - C9 F3 - C9 Operators for generating equivalent atoms: $1 x-1/2, y, -z+3/2 $2 x+1/2, y, -z+3/2 h k l Fo^2 Sigma Why rejected 0 1 2 0.59 0.13 observed but should be systematically absent 20015 Reflections read, of which 1671 rejected -12 =< h =< 10, -11 =< k =< 12, -25 =< l =< 23, Max. 2-theta = 54.99 1 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 7 9 9 -0.40 0.20 3 1.41 1 Inconsistent equivalents 2036 Unique reflections, of which 0 suppressed R(int) = 0.0499 R(sigma) = 0.0292 Friedel opposites merged Maximum memory for data reduction = 1809 / 20542 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 = 2236 / 179578 wR2 = 0.1479 before cycle 1 for 2036 data and 142 / 142 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.117; Restrained GooF = 1.116 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0480 * P )^2 + 2.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24368 0.00088 -0.008 OSF 2 0.83032 0.00252 0.001 FVAR 2 Mean shift/esd = 0.002 Maximum = -0.008 for OSF Max. shift = 0.000 A for H8B3_b Max. dU = 0.000 for C8A_a Least-squares cycle 2 Maximum vector length = 511 Memory required = 2236 / 179578 wR2 = 0.1479 before cycle 2 for 2036 data and 142 / 142 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.117; Restrained GooF = 1.116 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0480 * P )^2 + 2.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24368 0.00088 -0.002 OSF 2 0.83032 0.00252 0.000 FVAR 2 Mean shift/esd = 0.001 Maximum = -0.003 for U33 F1 Max. shift = 0.000 A for N1B_b Max. dU = 0.000 for C8A_a Least-squares cycle 3 Maximum vector length = 511 Memory required = 2236 / 179578 wR2 = 0.1479 before cycle 3 for 2036 data and 142 / 142 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.117; Restrained GooF = 1.116 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0480 * P )^2 + 2.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24368 0.00088 0.000 OSF 2 0.83032 0.00252 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for U11 C2 Max. shift = 0.000 A for H8B3_b Max. dU = 0.000 for C4 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2236 / 179578 wR2 = 0.1479 before cycle 4 for 2036 data and 142 / 142 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.117; Restrained GooF = 1.116 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0480 * P )^2 + 2.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24368 0.00088 0.000 OSF 2 0.83032 0.00252 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for tors H8A1_a Max. shift = 0.000 A for H8A2_a Max. dU = 0.000 for N1A_a Least-squares cycle 5 Maximum vector length = 511 Memory required = 2236 / 179578 wR2 = 0.1479 before cycle 5 for 2036 data and 142 / 142 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.117; Restrained GooF = 1.116 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0480 * P )^2 + 2.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24368 0.00088 0.000 OSF 2 0.83032 0.00252 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for z C1 Max. shift = 0.000 A for H8A3_a Max. dU = 0.000 for F1 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2236 / 179578 wR2 = 0.1479 before cycle 6 for 2036 data and 142 / 142 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.117; Restrained GooF = 1.116 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0480 * P )^2 + 2.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24368 0.00088 0.000 OSF 2 0.83032 0.00252 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for z C1 Max. shift = 0.000 A for H8A2_a Max. dU = 0.000 for F2 Least-squares cycle 7 Maximum vector length = 511 Memory required = 2236 / 179578 wR2 = 0.1479 before cycle 7 for 2036 data and 142 / 142 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.117; Restrained GooF = 1.116 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0480 * P )^2 + 2.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24368 0.00088 0.000 OSF 2 0.83032 0.00252 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for z C1 Max. shift = 0.000 A for H8A3_a Max. dU = 0.000 for N1A_a Least-squares cycle 8 Maximum vector length = 511 Memory required = 2236 / 179578 wR2 = 0.1479 before cycle 8 for 2036 data and 142 / 142 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.117; Restrained GooF = 1.116 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0480 * P )^2 + 2.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24368 0.00088 0.000 OSF 2 0.83032 0.00252 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for z C1 Max. shift = 0.000 A for H8B3_b Max. dU = 0.000 for N1A_a Least-squares cycle 9 Maximum vector length = 511 Memory required = 2236 / 179578 wR2 = 0.1479 before cycle 9 for 2036 data and 142 / 142 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.117; Restrained GooF = 1.116 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0480 * P )^2 + 2.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24368 0.00088 0.000 OSF 2 0.83032 0.00252 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for z C1 Max. shift = 0.000 A for N1B_b Max. dU = 0.000 for N1A_a Least-squares cycle 10 Maximum vector length = 511 Memory required = 2236 / 179578 wR2 = 0.1479 before cycle 10 for 2036 data and 142 / 142 parameters Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.117; Restrained GooF = 1.116 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0480 * P )^2 + 2.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24368 0.00088 0.000 OSF 2 0.83032 0.00252 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for z C1 Max. shift = 0.000 A for H8B3_b Max. dU = 0.000 for N1A_a Least-squares cycle 11 Maximum vector length = 511 Memory required = 2236 / 179578 wR2 = 0.1479 before cycle 11 for 2036 data and 142 / 142 parameters Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.117; Restrained GooF = 1.116 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0480 * P )^2 + 2.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24368 0.00088 0.000 OSF 2 0.83032 0.00252 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for z C1 Max. shift = 0.000 A for N1B_b Max. dU = 0.000 for N1A_a Least-squares cycle 12 Maximum vector length = 511 Memory required = 2236 / 179578 wR2 = 0.1479 before cycle 12 for 2036 data and 142 / 142 parameters Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.117; Restrained GooF = 1.116 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0480 * P )^2 + 2.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24368 0.00088 0.000 OSF 2 0.83032 0.00252 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for z C1 Max. shift = 0.000 A for N1B_b Max. dU = 0.000 for N1A_a Least-squares cycle 13 Maximum vector length = 511 Memory required = 2236 / 179578 wR2 = 0.1479 before cycle 13 for 2036 data and 142 / 142 parameters Summary of restraints applied in cycle 13 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.117; Restrained GooF = 1.116 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0480 * P )^2 + 2.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24368 0.00088 0.000 OSF 2 0.83032 0.00252 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for z C1 Max. shift = 0.000 A for H8A1_a Max. dU = 0.000 for F3 Least-squares cycle 14 Maximum vector length = 511 Memory required = 2236 / 179578 wR2 = 0.1479 before cycle 14 for 2036 data and 142 / 142 parameters Summary of restraints applied in cycle 14 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.117; Restrained GooF = 1.116 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0480 * P )^2 + 2.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24368 0.00088 0.000 OSF 2 0.83032 0.00252 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for z C1 Max. shift = 0.000 A for N1B_b Max. dU = 0.000 for F1 Least-squares cycle 15 Maximum vector length = 511 Memory required = 2236 / 179578 wR2 = 0.1479 before cycle 15 for 2036 data and 142 / 142 parameters Summary of restraints applied in cycle 15 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.117; Restrained GooF = 1.116 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0480 * P )^2 + 2.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24368 0.00088 0.000 OSF 2 0.83032 0.00252 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for z C1 Max. shift = 0.000 A for H8B3_b Max. dU = 0.000 for N1A_a Least-squares cycle 16 Maximum vector length = 511 Memory required = 2236 / 179578 wR2 = 0.1479 before cycle 16 for 2036 data and 142 / 142 parameters Summary of restraints applied in cycle 16 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.117; Restrained GooF = 1.116 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0480 * P )^2 + 2.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24368 0.00088 0.000 OSF 2 0.83032 0.00252 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for z C1 Max. shift = 0.000 A for N1B_b Max. dU = 0.000 for N1A_a Largest correlation matrix elements -0.954 y N1B_b / y N1A_a -0.877 z N1B_b / U13 N1A_a 0.776 U11 N1A_a / x N1A_a -0.940 z N1B_b / z N1A_a 0.873 U12 N1A_a / y N1A_a -0.536 z N1B_b / U33 N1A_a -0.905 y N1B_b / U12 N1A_a 0.830 U13 N1A_a / z N1A_a 0.512 U33 N1A_a / z N1A_a -0.900 x N1B_b / U11 N1A_a -0.796 x N1B_b / x N1A_a Idealized hydrogen atom generation before cycle 17 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.9607 0.3540 0.6453 43 0.950 0.000 C2 C1 C3 H3 0.9607 0.1990 0.5522 43 0.950 0.000 C3 C4 C2 H5 0.5430 0.1774 0.5594 43 0.950 0.000 C5 C6 C4 H6 0.5416 0.3335 0.6513 43 0.950 0.000 C6 C5 C1 H8A1 0.8356 0.5920 0.8458 137 0.980 0.000 C8A_a C7A_a H8A1_a H8A2 0.6939 0.6172 0.8057 137 0.980 0.000 C8A_a C7A_a H8A1_a H8A3 0.8244 0.7187 0.7913 137 0.980 0.000 C8A_a C7A_a H8A1_a H1A 0.6544 0.4869 0.7205 43 0.880 0.000 N1A_a C7A_a C1 H8B1 0.8091 0.6242 0.8036 137 0.980 0.000 C8B_b C7B_b H8B1_b H8B2 0.6689 0.6010 0.8452 137 0.980 0.000 C8B_b C7B_b H8B1_b H8B3 0.6774 0.7237 0.7887 137 0.980 0.000 C8B_b C7B_b H8B1_b H1BN 0.8496 0.4879 0.7241 43 0.880 0.000 N1B_b C7B_b C1 2008lsh001 in Pbca ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.75087 0.36236 0.65627 1.00000 0.01638 0.01840 0.01768 0.00284 0.00033 -0.00046 0.01749 0.00332 0.00021 0.00020 0.00009 0.00000 0.00086 0.00089 0.00084 0.00069 0.00078 0.00072 0.00039 C2 0.87561 0.31992 0.62738 1.00000 0.01661 0.02908 0.02644 -0.00319 -0.00027 -0.00180 0.02404 0.00361 0.00021 0.00023 0.00011 0.00000 0.00100 0.00110 0.00103 0.00088 0.00080 0.00081 0.00046 H2 0.96068 0.35397 0.64534 1.00000 0.02885 0.00000 0.00000 C3 0.87551 0.22745 0.57209 1.00000 0.01751 0.02747 0.02533 -0.00162 0.00184 0.00279 0.02344 0.00366 0.00022 0.00023 0.00011 0.00000 0.00101 0.00108 0.00107 0.00083 0.00081 0.00080 0.00046 H3 0.96069 0.19898 0.55223 1.00000 0.02813 0.00000 0.00000 C4 0.75158 0.17661 0.54582 1.00000 0.02195 0.01661 0.02007 0.00233 0.00074 0.00114 0.01954 0.00343 0.00021 0.00020 0.00009 0.00000 0.00092 0.00091 0.00091 0.00072 0.00081 0.00078 0.00041 C5 0.62773 0.21487 0.57620 1.00000 0.01775 0.02713 0.02743 -0.00175 -0.00231 -0.00167 0.02410 0.00364 0.00022 0.00023 0.00011 0.00000 0.00103 0.00108 0.00109 0.00085 0.00083 0.00080 0.00047 H5 0.54300 0.17742 0.55939 1.00000 0.02892 0.00000 0.00000 C6 0.62696 0.30730 0.63087 1.00000 0.01369 0.02946 0.02598 -0.00290 0.00098 -0.00130 0.02304 0.00351 0.00021 0.00023 0.00011 0.00000 0.00096 0.00107 0.00102 0.00086 0.00079 0.00079 0.00045 H6 0.54163 0.33348 0.65127 1.00000 0.02765 0.00000 0.00000 C9 0.75197 0.09066 0.48228 1.00000 0.02158 0.02044 0.02323 0.00156 0.00000 -0.00153 0.02175 0.00353 0.00022 0.00022 0.00010 0.00000 0.00093 0.00096 0.00096 0.00077 0.00085 0.00081 0.00043 C7A_a 0.84304 0.51848 0.74793 0.83032 0.02070 0.02315 0.01870 0.00249 -0.00301 -0.00124 0.02085 0.00411 0.00024 0.00026 0.00012 0.00252 0.00109 0.00110 0.00102 0.00091 0.00094 0.00093 0.00048 C8A_a 0.79504 0.62055 0.80248 0.83032 0.02721 0.03314 0.02504 -0.00541 -0.00172 0.00178 0.02846 0.00474 0.00030 0.00034 0.00015 0.00252 0.00138 0.00133 0.00119 0.00102 0.00116 0.00122 0.00059 H8A1_a 0.83564 0.59195 0.84575 0.83032 0.04269 0.00252 0.00000 H8A2_a 0.69389 0.61722 0.80572 0.83032 0.04269 0.00252 0.00000 H8A3_a 0.82444 0.71868 0.79133 0.83032 0.04269 0.00252 0.00000 N1A_a 0.73902 0.46000 0.70994 0.83032 0.01142 0.02302 0.02018 -0.00098 -0.00080 -0.00005 0.01821 0.00795 0.00036 0.00071 0.00028 0.00252 0.00197 0.00089 0.00096 0.00071 0.00148 0.00166 0.00079 H1A_a 0.65442 0.48693 0.72046 0.83032 0.02185 0.00252 0.00000 O1A_a 0.96597 0.49079 0.73896 0.83032 0.01318 0.04102 0.03273 -0.00535 -0.00532 0.00182 0.02898 0.00328 0.00019 0.00021 0.00009 0.00252 0.00091 0.00103 0.00102 0.00081 0.00077 0.00082 0.00045 C7B_b 0.65813 0.51956 0.74828 0.16968 0.02070 0.02315 0.01870 0.00249 -0.00301 -0.00124 0.02085 0.01757 0.00106 0.00122 0.00056 0.00252 0.00109 0.00110 0.00102 0.00091 0.00094 0.00093 0.00048 C8B_b 0.70780 0.62667 0.80116 0.16968 0.02721 0.03314 0.02504 -0.00541 -0.00172 0.00178 0.02846 0.02034 0.00153 0.00157 0.00069 0.00252 0.00138 0.00133 0.00119 0.00102 0.00116 0.00122 0.00059 H8B1_b 0.80907 0.62421 0.80360 0.16968 0.04269 0.00252 0.00000 H8B2_b 0.66892 0.60098 0.84521 0.16968 0.04269 0.00252 0.00000 H8B3_b 0.67738 0.72374 0.78872 0.16968 0.04269 0.00252 0.00000 N1B_b 0.76527 0.46237 0.71242 0.16968 0.01142 0.02302 0.02018 -0.00098 -0.00080 -0.00005 0.01821 0.05251 0.00256 0.00401 0.00161 0.00252 0.00197 0.00089 0.00096 0.00071 0.00148 0.00166 0.00079 H1BN_b 0.84964 0.48788 0.72410 0.16968 0.02185 0.00252 0.00000 O1B_b 0.53543 0.49158 0.73946 0.16968 0.01318 0.04102 0.03273 -0.00535 -0.00532 0.00182 0.02898 0.01470 0.00094 0.00106 0.00050 0.00252 0.00091 0.00103 0.00102 0.00081 0.00077 0.00082 0.00045 F1 0.76215 0.17501 0.42735 1.00000 0.09268 0.03062 0.01964 0.00295 0.00055 -0.00169 0.04765 0.00269 0.00019 0.00016 0.00006 0.00000 0.00131 0.00077 0.00065 0.00054 0.00074 0.00080 0.00048 F2 0.63834 0.01289 0.47327 1.00000 0.03676 0.05114 0.04287 -0.02238 0.00657 -0.01707 0.04359 0.00226 0.00015 0.00017 0.00007 0.00000 0.00083 0.00093 0.00084 0.00072 0.00064 0.00069 0.00043 F3 0.85848 -0.00041 0.47798 1.00000 0.04050 0.04788 0.04219 -0.01985 -0.01082 0.02378 0.04353 0.00247 0.00015 0.00016 0.00007 0.00000 0.00085 0.00090 0.00083 0.00070 0.00065 0.00070 0.00043 Final Structure Factor Calculation for 2008lsh001 in Pbca Total number of l.s. parameters = 142 Maximum vector length = 511 Memory required = 2094 / 24017 wR2 = 0.1479 before cycle 17 for 2036 data and 0 / 142 parameters Summary of restraints applied in cycle 17 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.017 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.117; Restrained GooF = 1.116 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0480 * P )^2 + 2.04 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0551 for 1543 Fo > 4sig(Fo) and 0.0728 for all 2036 data wR2 = 0.1479, GooF = S = 1.117, Restrained GooF = 1.116 for all data Occupancy sum of asymmetric unit = 14.00 for non-hydrogen and 8.00 for hydrogen atoms Principal mean square atomic displacements U 0.0209 0.0166 0.0150 C1 0.0313 0.0245 0.0163 C2 0.0286 0.0254 0.0163 C3 0.0229 0.0204 0.0154 C4 0.0291 0.0264 0.0168 C5 0.0312 0.0243 0.0135 C6 0.0241 0.0222 0.0190 C9 0.0256 0.0207 0.0162 C7A_a 0.0365 0.0267 0.0222 C8A_a 0.0233 0.0199 0.0113 N1A_a 0.0442 0.0309 0.0118 O1A_a 0.0256 0.0207 0.0162 C7B_b 0.0365 0.0267 0.0222 C8B_b 0.0233 0.0199 0.0113 N1B_b 0.0442 0.0309 0.0118 O1B_b 0.0927 0.0313 0.0189 F1 0.0773 0.0327 0.0208 F2 0.0810 0.0311 0.0185 F3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.015 0.024 0.034 0.048 0.065 0.091 0.132 0.210 1.000 Number in group 210. 202. 220. 183. 213. 196. 205. 201. 202. 204. GooF 1.356 1.124 1.354 0.952 1.073 0.977 1.119 0.948 1.029 1.102 K 6.985 1.996 1.334 1.047 1.006 0.949 1.001 0.998 1.007 1.000 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.64 inf Number in group 209. 201. 204. 201. 206. 206. 200. 201. 204. 204. GooF 0.890 0.916 0.891 0.846 0.904 1.051 1.251 1.113 1.459 1.579 K 0.944 0.978 0.987 0.988 1.008 1.034 1.029 1.036 1.022 0.981 R1 0.205 0.158 0.127 0.087 0.078 0.062 0.058 0.053 0.053 0.044 Recommended weighting scheme: WGHT 0.0480 2.0431 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) 2 3 10 61.61 4.56 6.57 0.017 1.58 2 1 1 1154.24 1988.12 6.30 0.351 4.19 8 1 2 211.31 71.74 5.72 0.067 1.19 2 3 6 28.22 0.10 5.50 0.003 2.05 2 5 6 37.82 3.94 5.24 0.016 1.54 8 3 4 39.39 5.74 4.92 0.019 1.10 8 3 6 36.03 4.40 4.63 0.017 1.07 8 5 2 51.37 8.70 4.35 0.023 1.01 8 1 8 24.55 0.00 4.32 0.000 1.08 4 2 0 19.81 0.04 4.27 0.002 2.14 8 3 2 136.66 53.70 4.27 0.058 1.12 1 1 12 39.61 8.69 4.19 0.023 1.60 2 1 14 22.85 1.43 4.10 0.009 1.34 8 1 6 72.16 23.31 4.09 0.038 1.13 9 1 6 23.16 0.25 3.90 0.004 1.01 2 1 4 62.10 19.44 3.89 0.035 3.24 2 3 12 20.36 2.27 3.63 0.012 1.40 6 1 0 70.05 27.16 3.60 0.041 1.59 2 0 4 766.76 1015.68 3.49 0.251 3.46 1 1 8 26.57 5.87 3.47 0.019 2.32 2 1 8 45.53 16.46 3.41 0.032 2.15 5 5 10 14.12 0.03 3.24 0.001 1.11 9 1 10 12.66 0.07 3.21 0.002 0.94 8 5 4 37.96 10.26 3.04 0.025 0.99 8 7 6 16.60 0.04 3.04 0.002 0.86 3 2 8 230.72 160.34 3.03 0.100 1.81 8 3 0 62.90 27.19 3.01 0.041 1.13 3 5 12 10.51 0.01 3.00 0.001 1.15 0 6 14 106.07 168.75 2.96 0.102 1.04 4 5 5 10.34 0.15 2.93 0.003 1.38 4 2 10 589.78 463.16 2.86 0.170 1.46 11 0 8 40.58 13.05 2.82 0.028 0.83 2 1 10 59.69 29.31 2.81 0.043 1.80 4 9 1 15.58 2.85 2.81 0.013 0.95 4 0 6 33.50 67.89 2.79 0.065 1.95 5 1 8 13.46 2.00 2.72 0.011 1.50 8 5 0 16.78 1.16 2.70 0.008 1.01 7 1 2 16.08 0.07 2.68 0.002 1.35 4 0 4 764.86 618.61 2.68 0.196 2.17 5 2 9 74.07 41.55 2.68 0.051 1.39 2 3 8 125.15 81.74 2.63 0.071 1.80 3 1 1 119.75 177.52 2.62 0.105 3.01 3 1 8 34.39 14.49 2.60 0.030 1.92 5 2 8 55.00 28.32 2.58 0.042 1.45 2 3 14 23.64 7.71 2.57 0.022 1.24 9 3 5 9.76 0.51 2.56 0.006 0.98 4 0 0 322.46 418.59 2.53 0.161 2.42 4 5 7 11.29 1.28 2.46 0.009 1.31 0 2 7 431.61 342.41 2.43 0.146 2.42 6 5 10 14.45 2.20 2.43 0.012 1.04 Bond lengths and angles C1 - Distance Angles C2 1.3916 (0.0028) C6 1.3959 (0.0027) 119.39 (0.18) N1A_a 1.4027 (0.0048) 124.47 (0.22) 116.14 (0.22) N1B_b 1.4564 (0.0260) 114.36 (0.95) 126.25 (0.95) 10.18 (1.05) C1 - C2 C6 N1A_a C2 - Distance Angles C1 1.3916 (0.0028) C3 1.3925 (0.0030) 119.87 (0.19) H2 0.9500 120.06 120.06 C2 - C1 C3 C3 - Distance Angles C4 1.3885 (0.0029) C2 1.3925 (0.0030) 120.36 (0.19) H3 0.9500 119.82 119.82 C3 - C4 C2 C4 - Distance Angles C5 1.3861 (0.0028) C3 1.3885 (0.0029) 119.64 (0.18) C9 1.4913 (0.0027) 120.42 (0.19) 119.78 (0.18) C4 - C5 C3 C5 - Distance Angles C6 1.3826 (0.0030) C4 1.3861 (0.0028) 120.29 (0.19) H5 0.9500 119.85 119.85 C5 - C6 C4 C6 - Distance Angles C5 1.3826 (0.0030) C1 1.3959 (0.0027) 120.37 (0.19) H6 0.9500 119.81 119.81 C6 - C5 C1 C9 - Distance Angles F2 1.3263 (0.0024) F3 1.3350 (0.0024) 106.53 (0.17) F1 1.3449 (0.0023) 105.60 (0.17) 105.14 (0.17) C4 1.4913 (0.0027) 113.77 (0.17) 113.27 (0.17) 111.84 (0.17) C9 - F2 F3 F1 C7A_a - Distance Angles O1A_a 1.2283 (0.0030) N1A_a 1.3684 (0.0050) 123.20 (0.26) C8A_a 1.5110 (0.0035) 122.13 (0.23) 114.67 (0.24) C7A_a - O1A_a N1A_a C8A_a - Distance Angles C7A_a 1.5110 (0.0035) 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 1.3684 (0.0049) C1 1.4027 (0.0048) 127.89 (0.27) H1A_a 0.8800 116.05 116.05 N1A_a - C7A_a C1 O1A_a - Distance Angles C7A_a 1.2283 (0.0030) O1A_a - C7B_b - Distance Angles O1B_b 1.2264 (0.0119) N1B_b 1.3635 (0.0164) 125.25 (1.61) C8B_b 1.5228 (0.0129) 122.77 (1.07) 111.97 (1.52) C7B_b - O1B_b N1B_b C8B_b - Distance Angles C7B_b 1.5228 (0.0128) 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 1.3635 (0.0164) C1 1.4564 (0.0259) 125.05 (2.15) H1BN_b 0.8800 117.47 117.47 N1B_b - C7B_b C1 O1B_b - Distance Angles C7B_b 1.2264 (0.0119) O1B_b - F1 - Distance Angles C9 1.3449 (0.0023) F1 - F2 - Distance Angles C9 1.3263 (0.0024) F2 - F3 - Distance Angles C9 1.3350 (0.0024) F3 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 1.99 2.841(4) 161.9 N1A_a-H1A_a...O1A_$1a 0.88 1.94 2.79(3) 164.2 N1B_b-H1BN_b...O1B_$2b Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)