+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXS-97 - CRYSTAL STRUCTURE SOLUTION - WinGX VERSION + + Copyright(C) George M. Sheldrick 1986-97 Release 97-2 + + shelxs started at 18:59:26 on 24 Nov 2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Read instructions and process reflection data : 2010sl0003a.hkl Data: 2413 unique, 2087 observed R(int) = 0.0396 R(sigma) = 0.0328 Systematic absence violations: 8 Bad equivalents: 0 ESEL Emin 1.200 Emax 5.000 DelU 0.005 renorm 0.700 axis 0 OMIT s 4.00 2theta(lim) 180.0 INIT nn 11 nf 16 s+ 0.800 s- 0.200 wr 0.200 PHAN steps 10 cool 0.900 Boltz 0.400 ns 140 mtpr 40 mnqr 10 TREF np 256. nE 221 kapscal 0.900 ntan 2 wn -0.950 FMAP code 8 PLAN npeaks -23 del1 0.500 del2 1.500 MORE verbosity 1 TIME t 9999999. 140 Reflections and 1221. unique TPR for phase annealing 221 Phases refined using 3494. unique TPR 246 Reflections and 4258. unique TPR for R(alpha) 2573 Unique negative quartets found, 1450 used for phase refinement 258 Unique NQR employed in phase annealing 128 Parallel refinements, highest memory = 6671 / 64159 Try Ralpha Nqual Sigma-1 M(abs) CFOM Seminvariants 13773. 0.040 -0.910 0.867 1.004 0.042* -++-- --++- --+-+ +-+-+ ----- Freq: 0 0 16 0 0 0 17 0 0 0 0 65 7 0 1 7 0 0 0 0 0 1 0 0 0 0 0 1 0 1 / 128 1086589. 0.040 -0.910 0.867 1.004 0.042 -++-- --++- --+-+ +-+-+ ----- Freq: 0 0 40 0 0 0 34 0 0 0 0 110 15 0 3 22 0 0 0 0 0 2 0 1 1 0 0 3 / 256 256. Phase sets refined - best is code 13773. with CFOM = 0.0416 Fourier and peaksearch RE = 0.335 for 18 atoms and 583 E-values Fourier and peaksearch RE = 0.331 for 18 atoms and 583 E-values Fourier and peaksearch +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + shelxs finished at 18:59:27 Total CPU time: 1.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ When solving structures with SHELXS-97 please quote the following reference : G. M. Sheldrick (2008) Acta Cryst., A64, 112-122. +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2010sl0003a started at 19:17:56 on 24-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Read instructions and data - 2010sl0003a.hkl Data: 2407 unique, 0 suppressed R(int) = 0.0402 R(sigma) = 0.0329 Systematic absence violations: 0 Bad equivalents: 0 wR2 = 0.4380 before cycle 1 for 2407 data and 73 / 73 parameters GooF = S = 3.852; Restrained GooF = 3.852 for 0 restraints Mean shift/su = 1.822 Maximum = -6.900 for OSF at 19:17:57 Max. shift = 0.021 A for C3 Max. dU =-0.006 for C10 wR2 = 0.3596 before cycle 2 for 2407 data and 73 / 73 parameters GooF = S = 2.847; Restrained GooF = 2.847 for 0 restraints Mean shift/su = 0.927 Maximum = 5.078 for U11 F4 at 19:17:57 Max. shift = 0.009 A for C11 Max. dU = 0.003 for F4 wR2 = 0.3499 before cycle 3 for 2407 data and 73 / 73 parameters GooF = S = 2.745; Restrained GooF = 2.745 for 0 restraints Mean shift/su = 0.163 Maximum = 0.861 for U11 F4 at 19:17:57 Max. shift = 0.002 A for C3 Max. dU = 0.001 for F4 wR2 = 0.3501 before cycle 4 for 2407 data and 73 / 73 parameters GooF = S = 2.739; Restrained GooF = 2.739 for 0 restraints Mean shift/su = 0.057 Maximum = -0.178 for z F4 at 19:17:57 Max. shift = 0.001 A for C13 Max. dU = 0.000 for C13 wR2 = 0.3502 before cycle 5 for 2407 data and 73 / 73 parameters GooF = S = 2.738; Restrained GooF = 2.738 for 0 restraints Mean shift/su = 0.016 Maximum = 0.051 for y C13 at 19:17:57 Max. shift = 0.000 A for C13 Max. dU = 0.000 for C3 wR2 = 0.3502 before cycle 6 for 2407 data and 73 / 73 parameters GooF = S = 2.738; Restrained GooF = 2.738 for 0 restraints Mean shift/su = 0.005 Maximum = 0.018 for y C13 at 19:17:57 Max. shift = 0.000 A for C13 Max. dU = 0.000 for C13 wR2 = 0.3502 before cycle 7 for 2407 data and 73 / 73 parameters GooF = S = 2.739; Restrained GooF = 2.739 for 0 restraints Mean shift/su = 0.001 Maximum = 0.006 for y C13 at 19:17:57 Max. shift = 0.000 A for C13 Max. dU = 0.000 for C13 wR2 = 0.3502 before cycle 8 for 2407 data and 73 / 73 parameters GooF = S = 2.739; Restrained GooF = 2.739 for 0 restraints Mean shift/su = 0.000 Maximum = 0.002 for y C13 at 19:17:58 Max. shift = 0.000 A for C13 Max. dU = 0.000 for C13 wR2 = 0.3502 before cycle 9 for 2407 data and 73 / 73 parameters GooF = S = 2.739; Restrained GooF = 2.739 for 0 restraints Mean shift/su = 0.000 Maximum = 0.001 for y C13 at 19:17:58 Max. shift = 0.000 A for C13 Max. dU = 0.000 for C13 wR2 = 0.3502 before cycle 10 for 2407 data and 73 / 73 parameters GooF = S = 2.739; Restrained GooF = 2.739 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F2 at 19:17:58 Max. shift = 0.000 A for C7 Max. dU = 0.000 for C4 wR2 = 0.3502 before cycle 11 for 2407 data and 73 / 73 parameters GooF = S = 2.739; Restrained GooF = 2.739 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F2 at 19:17:58 Max. shift = 0.000 A for C12 Max. dU = 0.000 for C4 wR2 = 0.3502 before cycle 12 for 2407 data and 73 / 73 parameters GooF = S = 2.739; Restrained GooF = 2.739 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F2 at 19:17:58 Max. shift = 0.000 A for C13 Max. dU = 0.000 for C5 wR2 = 0.3502 before cycle 13 for 2407 data and 73 / 73 parameters GooF = S = 2.739; Restrained GooF = 2.739 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F2 at 19:17:58 Max. shift = 0.000 A for F4 Max. dU = 0.000 for C13 wR2 = 0.3502 before cycle 14 for 2407 data and 73 / 73 parameters GooF = S = 2.739; Restrained GooF = 2.739 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F2 at 19:17:58 Max. shift = 0.000 A for C12 Max. dU = 0.000 for F2 wR2 = 0.3502 before cycle 15 for 2407 data and 73 / 73 parameters GooF = S = 2.739; Restrained GooF = 2.739 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F2 at 19:17:58 Max. shift = 0.000 A for C5 Max. dU = 0.000 for C6 wR2 = 0.3502 before cycle 16 for 2407 data and 73 / 73 parameters GooF = S = 2.739; Restrained GooF = 2.739 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F2 at 19:17:58 Max. shift = 0.000 A for C12 Max. dU = 0.000 for C12 wR2 = 0.3502 before cycle 17 for 2407 data and 73 / 73 parameters GooF = S = 2.739; Restrained GooF = 2.739 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F2 at 19:17:58 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C12 wR2 = 0.3502 before cycle 18 for 2407 data and 73 / 73 parameters GooF = S = 2.739; Restrained GooF = 2.739 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F2 at 19:17:58 Max. shift = 0.000 A for C12 Max. dU = 0.000 for F3 wR2 = 0.3502 before cycle 19 for 2407 data and 73 / 73 parameters GooF = S = 2.739; Restrained GooF = 2.739 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F2 at 19:17:58 Max. shift = 0.000 A for F3 Max. dU = 0.000 for N1 wR2 = 0.3502 before cycle 20 for 2407 data and 73 / 73 parameters GooF = S = 2.739; Restrained GooF = 2.739 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F2 at 19:17:59 Max. shift = 0.000 A for C3 Max. dU = 0.000 for F2 wR2 = 0.3502 before cycle 21 for 2407 data and 0 / 73 parameters GooF = S = 2.739; Restrained GooF = 2.739 for 0 restraints R1 = 0.1170 for 2013 Fo > 4sig(Fo) and 0.1279 for all 2407 data wR2 = 0.3502, GooF = S = 2.739, Restrained GooF = 2.739 for all data ** Extinction (EXTI) or solvent water (SWAT) correction may be required ** R1 = 0.1279 for 2407 unique reflections after merging for Fourier Highest peak 1.06 at 0.3460 0.0345 0.3924 [ 0.47 A from F1 ] Deepest hole -1.79 at 0.5320 0.0817 0.8829 [ 0.56 A from F4 ] +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2010sl0003a finished at 19:17:59 Total CPU time: 2.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ When refining structures with SHELXL-97 please quote the following reference: G. M. Sheldrick (2008) Acta Cryst., A64, 112-122. +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2010sl0003a started at 19:24:13 on 24-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Read instructions and data - 2010sl0003a.hkl Data: 2407 unique, 0 suppressed R(int) = 0.0402 R(sigma) = 0.0329 Systematic absence violations: 0 Bad equivalents: 0 wR2 = 0.3122 before cycle 1 for 2407 data and 73 / 73 parameters GooF = S = 1.052; Restrained GooF = 1.052 for 0 restraints Mean shift/su = 0.377 Maximum = 1.903 for OSF at 19:24:14 Max. shift = 0.006 A for C12 Max. dU = 0.001 for C9 wR2 = 0.3101 before cycle 2 for 2407 data and 73 / 73 parameters GooF = S = 1.051; Restrained GooF = 1.051 for 0 restraints Mean shift/su = 0.161 Maximum = -0.663 for x C12 at 19:24:14 Max. shift = 0.003 A for C12 Max. dU = 0.000 for C9 wR2 = 0.3098 before cycle 3 for 2407 data and 73 / 73 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints Mean shift/su = 0.024 Maximum = 0.099 for z F4 at 19:24:14 Max. shift = 0.000 A for C6 Max. dU = 0.000 for C13 wR2 = 0.3098 before cycle 4 for 2407 data and 73 / 73 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints Mean shift/su = 0.006 Maximum = -0.024 for U11 F3 at 19:24:14 Max. shift = 0.000 A for C6 Max. dU = 0.000 for F3 wR2 = 0.3098 before cycle 5 for 2407 data and 73 / 73 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints Mean shift/su = 0.001 Maximum = 0.005 for z F4 at 19:24:14 Max. shift = 0.000 A for F4 Max. dU = 0.000 for F3 wR2 = 0.3098 before cycle 6 for 2407 data and 73 / 73 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints Mean shift/su = 0.000 Maximum = 0.001 for z F4 at 19:24:14 Max. shift = 0.000 A for F4 Max. dU = 0.000 for C8 wR2 = 0.3098 before cycle 7 for 2407 data and 73 / 73 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for z F4 at 19:24:14 Max. shift = 0.000 A for C13 Max. dU = 0.000 for C1 wR2 = 0.3098 before cycle 8 for 2407 data and 73 / 73 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F1 at 19:24:14 Max. shift = 0.000 A for C7 Max. dU = 0.000 for F1 wR2 = 0.3098 before cycle 9 for 2407 data and 73 / 73 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y C3 at 19:24:14 Max. shift = 0.000 A for C10 Max. dU = 0.000 for C8 wR2 = 0.3098 before cycle 10 for 2407 data and 73 / 73 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y C3 at 19:24:15 Max. shift = 0.000 A for F1 Max. dU = 0.000 for F2 wR2 = 0.3098 before cycle 11 for 2407 data and 73 / 73 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y C3 at 19:24:15 Max. shift = 0.000 A for C7 Max. dU = 0.000 for C2 wR2 = 0.3098 before cycle 12 for 2407 data and 73 / 73 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F1 at 19:24:15 Max. shift = 0.000 A for C10 Max. dU = 0.000 for C12 wR2 = 0.3098 before cycle 13 for 2407 data and 73 / 73 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F1 at 19:24:15 Max. shift = 0.000 A for C7 Max. dU = 0.000 for F2 wR2 = 0.3098 before cycle 14 for 2407 data and 73 / 73 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y C3 at 19:24:15 Max. shift = 0.000 A for C7 Max. dU = 0.000 for C6 wR2 = 0.3098 before cycle 15 for 2407 data and 73 / 73 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y C3 at 19:24:15 Max. shift = 0.000 A for C10 Max. dU = 0.000 for F3 wR2 = 0.3098 before cycle 16 for 2407 data and 73 / 73 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y C3 at 19:24:15 Max. shift = 0.000 A for N1 Max. dU = 0.000 for F3 wR2 = 0.3098 before cycle 17 for 2407 data and 73 / 73 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y C3 at 19:24:15 Max. shift = 0.000 A for N1 Max. dU = 0.000 for C8 wR2 = 0.3098 before cycle 18 for 2407 data and 73 / 73 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y C3 at 19:24:15 Max. shift = 0.000 A for F1 Max. dU = 0.000 for F2 wR2 = 0.3098 before cycle 19 for 2407 data and 73 / 73 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y C3 at 19:24:15 Max. shift = 0.000 A for C10 Max. dU = 0.000 for F3 wR2 = 0.3098 before cycle 20 for 2407 data and 73 / 73 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y C3 at 19:24:15 Max. shift = 0.000 A for F1 Max. dU = 0.000 for F2 wR2 = 0.3098 before cycle 21 for 2407 data and 0 / 73 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints R1 = 0.1139 for 2013 Fo > 4sig(Fo) and 0.1246 for all 2407 data wR2 = 0.3098, GooF = S = 1.050, Restrained GooF = 1.050 for all data ** Extinction (EXTI) or solvent water (SWAT) correction may be required ** R1 = 0.1246 for 2407 unique reflections after merging for Fourier Highest peak 1.01 at 0.3430 0.0347 0.3959 [ 0.50 A from F1 ] Deepest hole -1.82 at 0.5326 0.0816 0.8817 [ 0.56 A from F4 ] +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2010sl0003a finished at 19:24:15 Total CPU time: 2.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ When refining structures with SHELXL-97 please quote the following reference: G. M. Sheldrick (2008) Acta Cryst., A64, 112-122. +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2010sl0003a started at 19:25:47 on 24-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Read instructions and data - 2010sl0003a.hkl Data: 2407 unique, 0 suppressed R(int) = 0.0402 R(sigma) = 0.0329 Systematic absence violations: 0 Bad equivalents: 0 +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2010sl0003a started at 19:27:42 on 24-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Read instructions and data - 2010sl0003a.hkl Data: 2413 unique, 0 suppressed R(int) = 0.0402 R(sigma) = 0.0330 Systematic absence violations: 0 Bad equivalents: 0 wR2 = 0.4144 before cycle 1 for 2413 data and 0 / 73 parameters GooF = S = 3.591; Restrained GooF = 3.591 for 0 restraints R1 = 0.1365 for 2017 Fo > 4sig(Fo) and 0.1511 for all 2413 data wR2 = 0.4144, GooF = S = 3.591, Restrained GooF = 3.591 for all data ** Extinction (EXTI) or solvent water (SWAT) correction may be required ** +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2010sl0003a finished at 19:27:42 Total CPU time: 0.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ When refining structures with SHELXL-97 please quote the following reference: G. M. Sheldrick (2008) Acta Cryst., A64, 112-122. +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2010sl0003a started at 19:30:33 on 24-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Read instructions and data - 2010sl0003a.hkl Data: 2407 unique, 0 suppressed R(int) = 0.0402 R(sigma) = 0.0329 Systematic absence violations: 0 Bad equivalents: 0 wR2 = 0.4139 before cycle 1 for 2407 data and 73 / 73 parameters GooF = S = 3.579; Restrained GooF = 3.579 for 0 restraints Mean shift/su = 1.954 Maximum = 8.115 for U11 F4 at 19:30:33 Max. shift = 0.023 A for C11 Max. dU = 0.006 for F4 wR2 = 0.3210 before cycle 2 for 2407 data and 73 / 73 parameters GooF = S = 2.506; Restrained GooF = 2.506 for 0 restraints Mean shift/su = 0.950 Maximum = 6.146 for U11 F4 at 19:30:33 Max. shift = 0.009 A for C11 Max. dU = 0.004 for F4 wR2 = 0.3101 before cycle 3 for 2407 data and 73 / 73 parameters GooF = S = 2.398; Restrained GooF = 2.398 for 0 restraints Mean shift/su = 0.222 Maximum = 1.069 for U11 F4 at 19:30:33 Max. shift = 0.003 A for F4 Max. dU = 0.001 for F4 wR2 = 0.3102 before cycle 4 for 2407 data and 73 / 73 parameters GooF = S = 2.393; Restrained GooF = 2.393 for 0 restraints Mean shift/su = 0.080 Maximum = -0.290 for z C12 at 19:30:34 Max. shift = 0.001 A for C12 Max. dU = 0.000 for F4 wR2 = 0.3103 before cycle 5 for 2407 data and 73 / 73 parameters GooF = S = 2.393; Restrained GooF = 2.393 for 0 restraints Mean shift/su = 0.022 Maximum = -0.081 for y F4 at 19:30:34 Max. shift = 0.000 A for N1 Max. dU = 0.000 for F4 wR2 = 0.3103 before cycle 6 for 2407 data and 0 / 73 parameters GooF = S = 2.394; Restrained GooF = 2.394 for 0 restraints R1 = 0.0994 for 2013 Fo > 4sig(Fo) and 0.1106 for all 2407 data wR2 = 0.3103, GooF = S = 2.394, Restrained GooF = 2.394 for all data ** Extinction (EXTI) or solvent water (SWAT) correction may be required ** R1 = 0.1105 for 2407 unique reflections after merging for Fourier Highest peak 1.08 at 0.1591 0.0339 0.6060 [ 0.50 A from F1 ] Deepest hole -1.84 at 0.9720 0.0830 0.1168 [ 0.59 A from F4 ] +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2010sl0003a finished at 19:30:34 Total CPU time: 1.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ When refining structures with SHELXL-97 please quote the following reference: G. M. Sheldrick (2008) Acta Cryst., A64, 112-122. +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2010sl0003a started at 19:32:29 on 24-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Read instructions and data - 2010sl0003a.hkl Data: 2407 unique, 0 suppressed R(int) = 0.0402 R(sigma) = 0.0329 Systematic absence violations: 0 Bad equivalents: 0 wR2 = 0.4139 before cycle 1 for 2407 data and 163 / 163 parameters GooF = S = 3.650; Restrained GooF = 3.650 for 0 restraints Mean shift/su = 1.815 Maximum = 8.449 for U22 F4 at 19:32:29 Max. shift = 0.028 A for C11 Max. dU =-0.006 for C10 wR2 = 0.2067 before cycle 2 for 2407 data and 163 / 163 parameters GooF = S = 1.610; Restrained GooF = 1.610 for 0 restraints Mean shift/su = 1.330 Maximum = 10.422 for U22 F4 at 19:32:30 Max. shift = 0.011 A for C11 Max. dU = 0.005 for F4 wR2 = 0.1524 before cycle 3 for 2407 data and 163 / 163 parameters GooF = S = 1.165; Restrained GooF = 1.165 for 0 restraints Mean shift/su = 0.459 Maximum = 2.033 for U22 F4 at 19:32:30 Max. shift = 0.003 A for H13 Max. dU = 0.001 for F4 wR2 = 0.1496 before cycle 4 for 2407 data and 163 / 163 parameters GooF = S = 1.139; Restrained GooF = 1.139 for 0 restraints Mean shift/su = 0.112 Maximum = -0.668 for z C12 at 19:32:30 Max. shift = 0.001 A for C12 Max. dU = 0.000 for C7 wR2 = 0.1494 before cycle 5 for 2407 data and 163 / 163 parameters GooF = S = 1.137; Restrained GooF = 1.137 for 0 restraints Mean shift/su = 0.025 Maximum = 0.120 for z F2 at 19:32:30 Max. shift = 0.000 A for C6 Max. dU = 0.000 for F3 wR2 = 0.1494 before cycle 6 for 2407 data and 0 / 163 parameters GooF = S = 1.137; Restrained GooF = 1.137 for 0 restraints R1 = 0.0518 for 2013 Fo > 4sig(Fo) and 0.0605 for all 2407 data wR2 = 0.1494, GooF = S = 1.137, Restrained GooF = 1.137 for all data ** Extinction (EXTI) or solvent water (SWAT) correction may be required ** R1 = 0.0605 for 2407 unique reflections after merging for Fourier Highest peak 0.77 at 0.0848 0.1392 0.8973 [ 1.69 A from C4 ] Deepest hole -0.87 at 0.4614 0.1123 0.8401 [ 0.77 A from C11 ] +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2010sl0003a finished at 19:32:30 Total CPU time: 1.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ When refining structures with SHELXL-97 please quote the following reference: G. M. Sheldrick (2008) Acta Cryst., A64, 112-122. +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2010sl0003a started at 19:38:38 on 24-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Read instructions and data - 2010sl0003a.hkl Data: 1849 unique, 0 suppressed R(int) = 0.0382 R(sigma) = 0.0284 Systematic absence violations: 0 Bad equivalents: 0 wR2 = 0.4125 before cycle 1 for 1849 data and 163 / 163 parameters GooF = S = 3.986; Restrained GooF = 3.986 for 0 restraints Mean shift/su = 1.508 Maximum = 7.085 for U22 F4 at 19:38:39 Max. shift = 0.028 A for C11 Max. dU = 0.006 for F4 wR2 = 0.2008 before cycle 2 for 1849 data and 163 / 163 parameters GooF = S = 1.701; Restrained GooF = 1.701 for 0 restraints Mean shift/su = 1.166 Maximum = 8.528 for U22 F4 at 19:38:39 Max. shift = 0.011 A for C11 Max. dU = 0.004 for F4 wR2 = 0.1432 before cycle 3 for 1849 data and 163 / 163 parameters GooF = S = 1.191; Restrained GooF = 1.191 for 0 restraints Mean shift/su = 0.461 Maximum = 1.817 for U22 F4 at 19:38:39 Max. shift = 0.003 A for C13 Max. dU = 0.001 for F4 wR2 = 0.1395 before cycle 4 for 1849 data and 163 / 163 parameters GooF = S = 1.156; Restrained GooF = 1.156 for 0 restraints Mean shift/su = 0.116 Maximum = 0.643 for U23 C12 at 19:38:39 Max. shift = 0.001 A for C12 Max. dU = 0.000 for C7 wR2 = 0.1393 before cycle 5 for 1849 data and 163 / 163 parameters GooF = S = 1.153; Restrained GooF = 1.153 for 0 restraints Mean shift/su = 0.029 Maximum = 0.142 for z F2 at 19:38:39 Max. shift = 0.000 A for C6 Max. dU = 0.000 for F3 wR2 = 0.1393 before cycle 6 for 1849 data and 0 / 163 parameters GooF = S = 1.153; Restrained GooF = 1.153 for 0 restraints R1 = 0.0487 for 1633 Fo > 4sig(Fo) and 0.0537 for all 1849 data wR2 = 0.1393, GooF = S = 1.153, Restrained GooF = 1.153 for all data ** Extinction (EXTI) or solvent water (SWAT) correction may be required ** R1 = 0.0536 for 1849 unique reflections after merging for Fourier Highest peak 0.77 at 0.2085 0.1265 0.9776 [ 1.72 A from C11 ] Deepest hole -0.83 at 0.4758 0.1095 0.8543 [ 0.87 A from C11 ] +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2010sl0003a finished at 19:38:40 Total CPU time: 1.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ When refining structures with SHELXL-97 please quote the following reference: G. M. Sheldrick (2008) Acta Cryst., A64, 112-122. +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2010sl0003a started at 19:39:11 on 24-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Read instructions and data - 2010sl0003a.hkl Data: 1849 unique, 0 suppressed R(int) = 0.0382 R(sigma) = 0.0284 Systematic absence violations: 0 Bad equivalents: 0 wR2 = 0.4125 before cycle 1 for 1849 data and 163 / 163 parameters GooF = S = 3.986; Restrained GooF = 3.986 for 0 restraints Mean shift/su = 1.508 Maximum = 7.085 for U22 F4 at 19:39:12 Max. shift = 0.028 A for C11 Max. dU = 0.006 for F4 wR2 = 0.2008 before cycle 2 for 1849 data and 163 / 163 parameters GooF = S = 1.701; Restrained GooF = 1.701 for 0 restraints Mean shift/su = 1.166 Maximum = 8.528 for U22 F4 at 19:39:12 Max. shift = 0.011 A for C11 Max. dU = 0.004 for F4 wR2 = 0.1432 before cycle 3 for 1849 data and 163 / 163 parameters GooF = S = 1.191; Restrained GooF = 1.191 for 0 restraints Mean shift/su = 0.461 Maximum = 1.817 for U22 F4 at 19:39:12 Max. shift = 0.003 A for C13 Max. dU = 0.001 for F4 wR2 = 0.1395 before cycle 4 for 1849 data and 163 / 163 parameters GooF = S = 1.156; Restrained GooF = 1.156 for 0 restraints Mean shift/su = 0.116 Maximum = 0.643 for U23 C12 at 19:39:12 Max. shift = 0.001 A for C12 Max. dU = 0.000 for C7 wR2 = 0.1393 before cycle 5 for 1849 data and 163 / 163 parameters GooF = S = 1.153; Restrained GooF = 1.153 for 0 restraints Mean shift/su = 0.029 Maximum = 0.142 for z F2 at 19:39:12 Max. shift = 0.000 A for C6 Max. dU = 0.000 for F3 wR2 = 0.1393 before cycle 6 for 1849 data and 163 / 163 parameters GooF = S = 1.153; Restrained GooF = 1.153 for 0 restraints Mean shift/su = 0.006 Maximum = -0.032 for U23 C7 at 19:39:12 Max. shift = 0.000 A for C3 Max. dU = 0.000 for C13 wR2 = 0.1393 before cycle 7 for 1849 data and 163 / 163 parameters GooF = S = 1.153; Restrained GooF = 1.153 for 0 restraints Mean shift/su = 0.001 Maximum = -0.007 for U23 C7 at 19:39:13 Max. shift = 0.000 A for C3 Max. dU = 0.000 for C13 wR2 = 0.1393 before cycle 8 for 1849 data and 163 / 163 parameters GooF = S = 1.153; Restrained GooF = 1.153 for 0 restraints Mean shift/su = 0.000 Maximum = -0.002 for y F4 at 19:39:13 Max. shift = 0.000 A for C3 Max. dU = 0.000 for C13 wR2 = 0.1393 before cycle 9 for 1849 data and 163 / 163 parameters GooF = S = 1.153; Restrained GooF = 1.153 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for U22 C11 at 19:39:13 Max. shift = 0.000 A for C3 Max. dU = 0.000 for C11 wR2 = 0.1393 before cycle 10 for 1849 data and 163 / 163 parameters GooF = S = 1.153; Restrained GooF = 1.153 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for OSF at 19:39:13 Max. shift = 0.000 A for C4 Max. dU = 0.000 for F4 wR2 = 0.1393 before cycle 11 for 1849 data and 163 / 163 parameters GooF = S = 1.153; Restrained GooF = 1.153 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F3 at 19:39:13 Max. shift = 0.000 A for C6 Max. dU = 0.000 for C11 wR2 = 0.1393 before cycle 12 for 1849 data and 163 / 163 parameters GooF = S = 1.153; Restrained GooF = 1.153 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F3 at 19:39:13 Max. shift = 0.000 A for C5 Max. dU = 0.000 for N1 wR2 = 0.1393 before cycle 13 for 1849 data and 163 / 163 parameters GooF = S = 1.153; Restrained GooF = 1.153 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F3 at 19:39:13 Max. shift = 0.000 A for C6 Max. dU = 0.000 for F4 wR2 = 0.1393 before cycle 14 for 1849 data and 163 / 163 parameters GooF = S = 1.153; Restrained GooF = 1.153 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F3 at 19:39:14 Max. shift = 0.000 A for C3 Max. dU = 0.000 for C12 wR2 = 0.1393 before cycle 15 for 1849 data and 163 / 163 parameters GooF = S = 1.153; Restrained GooF = 1.153 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F3 at 19:39:14 Max. shift = 0.000 A for F3 Max. dU = 0.000 for F4 wR2 = 0.1393 before cycle 16 for 1849 data and 163 / 163 parameters GooF = S = 1.153; Restrained GooF = 1.153 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F2 at 19:39:14 Max. shift = 0.000 A for C6 Max. dU = 0.000 for C12 wR2 = 0.1393 before cycle 17 for 1849 data and 163 / 163 parameters GooF = S = 1.153; Restrained GooF = 1.153 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F3 at 19:39:14 Max. shift = 0.000 A for F3 Max. dU = 0.000 for C3 wR2 = 0.1393 before cycle 18 for 1849 data and 163 / 163 parameters GooF = S = 1.153; Restrained GooF = 1.153 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y C3 at 19:39:14 Max. shift = 0.000 A for C3 Max. dU = 0.000 for C12 wR2 = 0.1393 before cycle 19 for 1849 data and 163 / 163 parameters GooF = S = 1.153; Restrained GooF = 1.153 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F3 at 19:39:14 Max. shift = 0.000 A for C6 Max. dU = 0.000 for C3 wR2 = 0.1393 before cycle 20 for 1849 data and 163 / 163 parameters GooF = S = 1.153; Restrained GooF = 1.153 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F3 at 19:39:15 Max. shift = 0.000 A for C6 Max. dU = 0.000 for F4 wR2 = 0.1393 before cycle 21 for 1849 data and 0 / 163 parameters GooF = S = 1.153; Restrained GooF = 1.153 for 0 restraints R1 = 0.0487 for 1633 Fo > 4sig(Fo) and 0.0537 for all 1849 data wR2 = 0.1393, GooF = S = 1.153, Restrained GooF = 1.153 for all data ** Extinction (EXTI) or solvent water (SWAT) correction may be required ** R1 = 0.0537 for 1849 unique reflections after merging for Fourier Highest peak 0.77 at 0.2085 0.1265 0.9776 [ 1.72 A from C11 ] Deepest hole -0.83 at 0.4758 0.1095 0.8543 [ 0.87 A from C11 ] +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2010sl0003a finished at 19:39:15 Total CPU time: 3.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ When refining structures with SHELXL-97 please quote the following reference: G. M. Sheldrick (2008) Acta Cryst., A64, 112-122. +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2010sl0003a started at 19:46:44 on 24-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Read instructions and data - 2010sl0003a.hkl Data: 1848 unique, 0 suppressed R(int) = 0.0382 R(sigma) = 0.0271 Systematic absence violations: 0 Bad equivalents: 0 wR2 = 0.1144 before cycle 1 for 1848 data and 163 / 163 parameters GooF = S = 1.044; Restrained GooF = 1.044 for 0 restraints Mean shift/su = 0.269 Maximum = -0.868 for x F4 at 19:46:45 Max. shift = 0.001 A for C1 Max. dU = 0.000 for C13 wR2 = 0.1138 before cycle 2 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.098 Maximum = -0.303 for x F4 at 19:46:45 Max. shift = 0.000 A for C5 Max. dU = 0.000 for C13 wR2 = 0.1138 before cycle 3 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.005 Maximum = -0.021 for OSF at 19:46:45 Max. shift = 0.000 A for C5 Max. dU = 0.000 for C13 wR2 = 0.1138 before cycle 4 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.001 Maximum = -0.006 for U12 C4 at 19:46:45 Max. shift = 0.000 A for C6 Max. dU = 0.000 for C9 wR2 = 0.1138 before cycle 5 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x F3 at 19:46:45 Max. shift = 0.000 A for C6 Max. dU = 0.000 for C6 wR2 = 0.1138 before cycle 6 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x F2 at 19:46:46 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C12 wR2 = 0.1138 before cycle 7 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F2 at 19:46:46 Max. shift = 0.000 A for H13 Max. dU = 0.000 for C6 wR2 = 0.1138 before cycle 8 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F2 at 19:46:46 Max. shift = 0.000 A for C13 Max. dU = 0.000 for N1 wR2 = 0.1138 before cycle 9 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F2 at 19:46:46 Max. shift = 0.000 A for C7 Max. dU = 0.000 for F1 wR2 = 0.1138 before cycle 10 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F2 at 19:46:46 Max. shift = 0.000 A for C13 Max. dU = 0.000 for F3 wR2 = 0.1138 before cycle 11 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x F3 at 19:46:46 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C4 wR2 = 0.1138 before cycle 12 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x F3 at 19:46:47 Max. shift = 0.000 A for C13 Max. dU = 0.000 for C12 wR2 = 0.1138 before cycle 13 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F2 at 19:46:47 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C6 wR2 = 0.1138 before cycle 14 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F2 at 19:46:47 Max. shift = 0.000 A for C13 Max. dU = 0.000 for C7 wR2 = 0.1138 before cycle 15 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F2 at 19:46:47 Max. shift = 0.000 A for C7 Max. dU = 0.000 for C5 wR2 = 0.1138 before cycle 16 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F2 at 19:46:47 Max. shift = 0.000 A for C13 Max. dU = 0.000 for F4 wR2 = 0.1138 before cycle 17 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F2 at 19:46:47 Max. shift = 0.000 A for C3 Max. dU = 0.000 for C13 wR2 = 0.1138 before cycle 18 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F2 at 19:46:47 Max. shift = 0.000 A for C13 Max. dU = 0.000 for F4 wR2 = 0.1138 before cycle 19 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x F3 at 19:46:48 Max. shift = 0.000 A for C6 Max. dU = 0.000 for C8 wR2 = 0.1138 before cycle 20 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F2 at 19:46:48 Max. shift = 0.000 A for C13 Max. dU = 0.000 for C8 wR2 = 0.1138 before cycle 21 for 1848 data and 0 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints R1 = 0.0384 for 1632 Fo > 4sig(Fo) and 0.0435 for all 1848 data wR2 = 0.1138, GooF = S = 1.041, Restrained GooF = 1.041 for all data R1 = 0.0435 for 1848 unique reflections after merging for Fourier Highest peak 0.23 at 0.3336 0.1361 0.8873 [ 0.81 A from C8 ] Deepest hole -0.21 at 0.9590 0.0741 0.0293 [ 0.64 A from F4 ] +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2010sl0003a finished at 19:46:48 Total CPU time: 3.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ When refining structures with SHELXL-97 please quote the following reference: G. M. Sheldrick (2008) Acta Cryst., A64, 112-122. +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2010sl0003a started at 19:52:14 on 29-Mar-2011 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Read instructions and data - 2010sl0003a.hkl Data: 1848 unique, 0 suppressed R(int) = 0.0382 R(sigma) = 0.0271 Systematic absence violations: 0 Bad equivalents: 0 ** Cell contents from UNIT instruction and atom list do not agree ** wR2 = 0.1144 before cycle 1 for 1848 data and 163 / 163 parameters GooF = S = 1.044; Restrained GooF = 1.044 for 0 restraints Mean shift/su = 0.269 Maximum = -0.868 for x F4 at 19:52:36 Max. shift = 0.001 A for C1 Max. dU = 0.000 for C13 wR2 = 0.1138 before cycle 2 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.098 Maximum = -0.303 for x F4 at 19:52:37 Max. shift = 0.000 A for C5 Max. dU = 0.000 for C13 wR2 = 0.1138 before cycle 3 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.005 Maximum = -0.021 for OSF at 19:52:38 Max. shift = 0.000 A for C5 Max. dU = 0.000 for C13 wR2 = 0.1138 before cycle 4 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.001 Maximum = -0.006 for U12 C4 at 19:52:39 Max. shift = 0.000 A for C6 Max. dU = 0.000 for C9 wR2 = 0.1138 before cycle 5 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x F3 at 19:52:40 Max. shift = 0.000 A for C6 Max. dU = 0.000 for C6 wR2 = 0.1138 before cycle 6 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x F2 at 19:52:41 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C12 wR2 = 0.1138 before cycle 7 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F2 at 19:52:42 Max. shift = 0.000 A for H13 Max. dU = 0.000 for C6 wR2 = 0.1138 before cycle 8 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F2 at 19:52:43 Max. shift = 0.000 A for C13 Max. dU = 0.000 for N1 wR2 = 0.1138 before cycle 9 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F2 at 19:52:44 Max. shift = 0.000 A for C7 Max. dU = 0.000 for F1 wR2 = 0.1138 before cycle 10 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F2 at 19:52:45 Max. shift = 0.000 A for C13 Max. dU = 0.000 for F3 wR2 = 0.1138 before cycle 11 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x F3 at 19:52:46 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C4 wR2 = 0.1138 before cycle 12 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x F3 at 19:52:47 Max. shift = 0.000 A for C13 Max. dU = 0.000 for C12 wR2 = 0.1138 before cycle 13 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F2 at 19:52:48 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C6 wR2 = 0.1138 before cycle 14 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F2 at 19:52:49 Max. shift = 0.000 A for C13 Max. dU = 0.000 for C7 wR2 = 0.1138 before cycle 15 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F2 at 19:52:50 Max. shift = 0.000 A for C7 Max. dU = 0.000 for C5 wR2 = 0.1138 before cycle 16 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F2 at 19:52:51 Max. shift = 0.000 A for C13 Max. dU = 0.000 for F4 wR2 = 0.1138 before cycle 17 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F2 at 19:52:53 Max. shift = 0.000 A for C3 Max. dU = 0.000 for C13 wR2 = 0.1138 before cycle 18 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F2 at 19:52:54 Max. shift = 0.000 A for C13 Max. dU = 0.000 for F4 wR2 = 0.1138 before cycle 19 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x F3 at 19:52:55 Max. shift = 0.000 A for C6 Max. dU = 0.000 for C8 wR2 = 0.1138 before cycle 20 for 1848 data and 163 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F2 at 19:52:56 Max. shift = 0.000 A for C13 Max. dU = 0.000 for C8 wR2 = 0.1138 before cycle 21 for 1848 data and 0 / 163 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints R1 = 0.0384 for 1632 Fo > 4sig(Fo) and 0.0435 for all 1848 data wR2 = 0.1138, GooF = S = 1.041, Restrained GooF = 1.041 for all data R1 = 0.0435 for 1848 unique reflections after merging for Fourier Highest peak 0.23 at 0.3336 0.1361 0.8873 [ 0.81 A from C8 ] Deepest hole -0.21 at 0.9590 0.0741 0.0293 [ 0.64 A from F4 ] +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2010sl0003a finished at 19:52:57 Total CPU time: 6.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ When refining structures with SHELXL-97 please quote the following reference: G. M. Sheldrick (2008) Acta Cryst., A64, 112-122.