+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXS-97 - CRYSTAL STRUCTURE SOLUTION - WinGX VERSION + + Copyright(C) George M. Sheldrick 1986-97 Release 97-2 + + shelxs started at 22:29:39 on 27 Nov 2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Read instructions and process reflection data : 2010sl0004a.hkl Data: 2360 unique, 1894 observed R(int) = 0.0738 R(sigma) = 0.0622 Systematic absence violations: 0 Bad equivalents: 2 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 139 mtpr 40 mnqr 10 TREF np 256. nE 219 kapscal 0.900 ntan 2 wn -0.950 FMAP code 8 PLAN npeaks -22 del1 0.500 del2 1.500 MORE verbosity 1 TIME t 9999999. 139 Reflections and 822. unique TPR for phase annealing 219 Phases refined using 2756. unique TPR 272 Reflections and 4166. unique TPR for R(alpha) 1637 Unique negative quartets found, 1440 used for phase refinement 216 Unique NQR employed in phase annealing 128 Parallel refinements, highest memory = 6136 / 61412 Try Ralpha Nqual Sigma-1 M(abs) CFOM Seminvariants 74721. 0.043 -0.973 0.465 1.162 0.043* ++--+ ++--+ --+++ -+--- +++-+ Freq: 0 0 77 0 0 1 0 0 8 0 0 6 7 0 0 0 1 2 0 1 0 0 0 1 1 0 0 0 0 0 / 128 1094177. 0.043 -0.973 0.465 1.162 0.043 ++--+ ++--+ --+++ -+--- +++-+ Freq: 0 0 141 1 0 1 0 1 19 0 1 11 16 1 3 0 2 3 0 1 2 1 0 3 4 0 0 0 1 / 256 256. Phase sets refined - best is code 74721. with CFOM = 0.0428 Fourier and peaksearch RE = 0.182 for 17 atoms and 603 E-values Fourier and peaksearch RE = 0.178 for 17 atoms and 603 E-values Fourier and peaksearch +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + shelxs finished at 22:29:41 Total CPU time: 0.8 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 + + 2010sl0004a started at 22:33:13 on 27-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Read instructions and data - 2010sl0004a.hkl Data: 2360 unique, 0 suppressed R(int) = 0.0765 R(sigma) = 0.0633 Systematic absence violations: 0 Bad equivalents: 2 wR2 = 0.3934 before cycle 1 for 2360 data and 0 / 69 parameters GooF = S = 2.976; Restrained GooF = 2.976 for 0 restraints R1 = 0.1683 for 1734 Fo > 4sig(Fo) and 0.2028 for all 2360 data wR2 = 0.3934, GooF = S = 2.976, Restrained GooF = 2.976 for all data +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2010sl0004a finished at 22:33:14 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 + + 2010sl0004a started at 22:39:28 on 27-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Read instructions and data - 2010sl0004a.hkl Data: 2347 unique, 0 suppressed R(int) = 0.0765 R(sigma) = 0.0630 Systematic absence violations: 0 Bad equivalents: 2 wR2 = 0.3930 before cycle 1 for 2347 data and 69 / 69 parameters GooF = S = 2.966; Restrained GooF = 2.966 for 0 restraints Mean shift/su = 1.812 Maximum = 8.656 for U11 F2 at 22:39:29 Max. shift = 0.024 A for C7 Max. dU = 0.007 for F2 wR2 = 0.3133 before cycle 2 for 2347 data and 69 / 69 parameters GooF = S = 2.018; Restrained GooF = 2.018 for 0 restraints Mean shift/su = 0.897 Maximum = 5.142 for U11 F2 at 22:39:29 Max. shift = 0.009 A for C13 Max. dU = 0.004 for F2 wR2 = 0.3038 before cycle 3 for 2347 data and 69 / 69 parameters GooF = S = 1.943; Restrained GooF = 1.943 for 0 restraints Mean shift/su = 0.115 Maximum = 0.667 for U11 F2 at 22:39:29 Max. shift = 0.002 A for C2 Max. dU = 0.000 for F2 wR2 = 0.3036 before cycle 4 for 2347 data and 69 / 69 parameters GooF = S = 1.939; Restrained GooF = 1.939 for 0 restraints Mean shift/su = 0.023 Maximum = 0.104 for x C2 at 22:39:29 Max. shift = 0.000 A for C2 Max. dU = 0.000 for F3 wR2 = 0.3035 before cycle 5 for 2347 data and 69 / 69 parameters GooF = S = 1.939; Restrained GooF = 1.939 for 0 restraints Mean shift/su = 0.004 Maximum = 0.021 for x C2 at 22:39:29 Max. shift = 0.000 A for C2 Max. dU = 0.000 for F3 wR2 = 0.3035 before cycle 6 for 2347 data and 0 / 69 parameters GooF = S = 1.939; Restrained GooF = 1.939 for 0 restraints R1 = 0.1167 for 1731 Fo > 4sig(Fo) and 0.1460 for all 2347 data wR2 = 0.3035, GooF = S = 1.939, Restrained GooF = 1.939 for all data R1 = 0.1458 for 2347 unique reflections after merging for Fourier Highest peak 1.09 at 0.3312 0.7562 0.2367 [ 1.07 A from C1 ] Deepest hole -0.91 at 0.1394 0.0605 0.1539 [ 0.55 A from F3 ] +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2010sl0004a finished at 22:39:30 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 + + 2010sl0004a started at 22:42:46 on 27-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Read instructions and data - 2010sl0004a.hkl Data: 2347 unique, 0 suppressed R(int) = 0.0765 R(sigma) = 0.0630 Systematic absence violations: 0 Bad equivalents: 2 wR2 = 0.2928 before cycle 1 for 2347 data and 154 / 154 parameters GooF = S = 0.929; Restrained GooF = 0.929 for 0 restraints Mean shift/su = 1.479 Maximum = 8.682 for U22 F3 at 22:42:47 Max. shift = 0.008 A for C4 Max. dU =-0.002 for C12 wR2 = 0.2251 before cycle 2 for 2347 data and 154 / 154 parameters GooF = S = 0.715; Restrained GooF = 0.715 for 0 restraints Mean shift/su = 0.624 Maximum = 6.087 for U22 F3 at 22:42:47 Max. shift = 0.003 A for C6 Max. dU = 0.001 for F3 wR2 = 0.2175 before cycle 3 for 2347 data and 154 / 154 parameters GooF = S = 0.685; Restrained GooF = 0.685 for 0 restraints Mean shift/su = 0.112 Maximum = 0.835 for U22 F3 at 22:42:47 Max. shift = 0.001 A for C13 Max. dU = 0.000 for F3 wR2 = 0.2174 before cycle 4 for 2347 data and 154 / 154 parameters GooF = S = 0.685; Restrained GooF = 0.685 for 0 restraints Mean shift/su = 0.029 Maximum = -0.192 for U22 C8 at 22:42:47 Max. shift = 0.000 A for C1 Max. dU = 0.000 for C12 wR2 = 0.2174 before cycle 5 for 2347 data and 154 / 154 parameters GooF = S = 0.685; Restrained GooF = 0.685 for 0 restraints Mean shift/su = 0.007 Maximum = -0.030 for U22 C8 at 22:42:48 Max. shift = 0.000 A for H13 Max. dU = 0.000 for C7 wR2 = 0.2174 before cycle 6 for 2347 data and 0 / 154 parameters GooF = S = 0.685; Restrained GooF = 0.685 for 0 restraints R1 = 0.0620 for 1731 Fo > 4sig(Fo) and 0.0906 for all 2347 data wR2 = 0.2174, GooF = S = 0.685, Restrained GooF = 0.685 for all data R1 = 0.0905 for 2347 unique reflections after merging for Fourier Highest peak 0.56 at 0.3089 0.7166 -0.0002 [ 1.08 A from H2 ] Deepest hole -0.66 at 0.2305 0.0189 0.1238 [ 0.78 A from C7 ] +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2010sl0004a finished at 22:42:48 Total CPU time: 1.6 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 + + 2010sl0004a started at 22:44:34 on 27-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Read instructions and data - 2010sl0004a.hkl Data: 2346 unique, 0 suppressed R(int) = 0.0765 R(sigma) = 0.0629 Systematic absence violations: 0 Bad equivalents: 2 wR2 = 0.1520 before cycle 1 for 2346 data and 154 / 154 parameters GooF = S = 1.059; Restrained GooF = 1.059 for 0 restraints Mean shift/su = 0.401 Maximum = 1.693 for OSF at 22:44:35 Max. shift = 0.003 A for H5 Max. dU = 0.001 for C11 wR2 = 0.1503 before cycle 2 for 2346 data and 154 / 154 parameters GooF = S = 1.047; Restrained GooF = 1.047 for 0 restraints Mean shift/su = 0.152 Maximum = 0.601 for OSF at 22:44:35 Max. shift = 0.001 A for C5 Max. dU = 0.000 for C2 wR2 = 0.1502 before cycle 3 for 2346 data and 154 / 154 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Mean shift/su = 0.011 Maximum = 0.048 for OSF at 22:44:35 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C12 wR2 = 0.1502 before cycle 4 for 2346 data and 154 / 154 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Mean shift/su = 0.002 Maximum = 0.011 for U13 C6 at 22:44:35 Max. shift = 0.000 A for C6 Max. dU = 0.000 for C8 wR2 = 0.1502 before cycle 5 for 2346 data and 154 / 154 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Mean shift/su = 0.000 Maximum = -0.001 for x C5 at 22:44:35 Max. shift = 0.000 A for C5 Max. dU = 0.000 for C1 wR2 = 0.1502 before cycle 6 for 2346 data and 0 / 154 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints R1 = 0.0572 for 1730 Fo > 4sig(Fo) and 0.0868 for all 2346 data wR2 = 0.1502, GooF = S = 1.046, Restrained GooF = 1.046 for all data R1 = 0.0866 for 2346 unique reflections after merging for Fourier Highest peak 0.21 at 0.6164 0.6176 0.1204 [ 0.77 A from N1 ] Deepest hole -0.29 at 0.9193 0.3089 0.0407 [ 0.78 A from C9 ] +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2010sl0004a finished at 22:44:36 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 + + 2010sl0004a started at 22:46:27 on 27-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Read instructions and data - 2010sl0004a.hkl Data: 1815 unique, 0 suppressed R(int) = 0.0722 R(sigma) = 0.0532 Systematic absence violations: 0 Bad equivalents: 2 wR2 = 0.1371 before cycle 1 for 1815 data and 154 / 154 parameters GooF = S = 1.067; Restrained GooF = 1.067 for 0 restraints Mean shift/su = 0.542 Maximum = 1.819 for OSF at 22:46:28 Max. shift = 0.004 A for C9 Max. dU = 0.001 for C2 wR2 = 0.1330 before cycle 2 for 1815 data and 154 / 154 parameters GooF = S = 1.035; Restrained GooF = 1.035 for 0 restraints Mean shift/su = 0.205 Maximum = 0.641 for OSF at 22:46:28 Max. shift = 0.001 A for C11 Max. dU = 0.000 for C2 wR2 = 0.1327 before cycle 3 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.013 Maximum = 0.048 for U11 C2 at 22:46:28 Max. shift = 0.000 A for C11 Max. dU = 0.000 for C2 wR2 = 0.1327 before cycle 4 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.002 Maximum = 0.014 for U33 C2 at 22:46:28 Max. shift = 0.000 A for C1 Max. dU = 0.000 for C2 wR2 = 0.1327 before cycle 5 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.001 for U22 F3 at 22:46:28 Max. shift = 0.000 A for C11 Max. dU = 0.000 for C2 wR2 = 0.1327 before cycle 6 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x N1 at 22:46:29 Max. shift = 0.000 A for N1 Max. dU = 0.000 for C13 wR2 = 0.1327 before cycle 7 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F3 at 22:46:29 Max. shift = 0.000 A for C8 Max. dU = 0.000 for C4 wR2 = 0.1327 before cycle 8 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x N1 at 22:46:29 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C3 wR2 = 0.1327 before cycle 9 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x N1 at 22:46:29 Max. shift = 0.000 A for C8 Max. dU = 0.000 for C9 wR2 = 0.1327 before cycle 10 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x N1 at 22:46:29 Max. shift = 0.000 A for C8 Max. dU = 0.000 for C6 wR2 = 0.1327 before cycle 11 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x N1 at 22:46:29 Max. shift = 0.000 A for C7 Max. dU = 0.000 for N1 wR2 = 0.1327 before cycle 12 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x N1 at 22:46:29 Max. shift = 0.000 A for C8 Max. dU = 0.000 for C12 wR2 = 0.1327 before cycle 13 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x N1 at 22:46:30 Max. shift = 0.000 A for C7 Max. dU = 0.000 for C1 wR2 = 0.1327 before cycle 14 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x N1 at 22:46:30 Max. shift = 0.000 A for F2 Max. dU = 0.000 for C3 wR2 = 0.1327 before cycle 15 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x N1 at 22:46:30 Max. shift = 0.000 A for C7 Max. dU = 0.000 for F2 wR2 = 0.1327 before cycle 16 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x N1 at 22:46:30 Max. shift = 0.000 A for C4 Max. dU = 0.000 for F1 wR2 = 0.1327 before cycle 17 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x F2 at 22:46:30 Max. shift = 0.000 A for C8 Max. dU = 0.000 for C7 wR2 = 0.1327 before cycle 18 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for OSF at 22:46:30 Max. shift = 0.000 A for C4 Max. dU = 0.000 for F3 wR2 = 0.1327 before cycle 19 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x N1 at 22:46:30 Max. shift = 0.000 A for C8 Max. dU = 0.000 for F3 wR2 = 0.1327 before cycle 20 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x N1 at 22:46:31 Max. shift = 0.000 A for C1 Max. dU = 0.000 for C13 wR2 = 0.1327 before cycle 21 for 1815 data and 0 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints R1 = 0.0493 for 1473 Fo > 4sig(Fo) and 0.0668 for all 1815 data wR2 = 0.1327, GooF = S = 1.032, Restrained GooF = 1.032 for all data R1 = 0.0667 for 1815 unique reflections after merging for Fourier Highest peak 0.17 at 0.5959 0.1474 0.1574 [ 1.39 A from H11 ] Deepest hole -0.26 at 0.2343 0.0338 0.1178 [ 0.83 A from C7 ] +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2010sl0004a finished at 22:46:31 Total CPU time: 3.4 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 + + 2010sl0004a started at 22:00:16 on 29-Mar-2011 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Read instructions and data - 2010sl0004a.hkl Data: 1815 unique, 0 suppressed R(int) = 0.0722 R(sigma) = 0.0532 Systematic absence violations: 0 Bad equivalents: 2 wR2 = 0.1371 before cycle 1 for 1815 data and 154 / 154 parameters GooF = S = 1.067; Restrained GooF = 1.067 for 0 restraints Mean shift/su = 0.542 Maximum = 1.819 for OSF at 22:00:29 Max. shift = 0.004 A for C9 Max. dU = 0.001 for C2 wR2 = 0.1330 before cycle 2 for 1815 data and 154 / 154 parameters GooF = S = 1.035; Restrained GooF = 1.035 for 0 restraints Mean shift/su = 0.205 Maximum = 0.641 for OSF at 22:00:30 Max. shift = 0.001 A for C11 Max. dU = 0.000 for C2 wR2 = 0.1327 before cycle 3 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.013 Maximum = 0.048 for U11 C2 at 22:00:31 Max. shift = 0.000 A for C11 Max. dU = 0.000 for C2 wR2 = 0.1327 before cycle 4 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.002 Maximum = 0.014 for U33 C2 at 22:00:31 Max. shift = 0.000 A for C1 Max. dU = 0.000 for C2 wR2 = 0.1327 before cycle 5 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.001 for U22 F3 at 22:00:32 Max. shift = 0.000 A for C11 Max. dU = 0.000 for C2 wR2 = 0.1327 before cycle 6 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x N1 at 22:00:33 Max. shift = 0.000 A for N1 Max. dU = 0.000 for C13 wR2 = 0.1327 before cycle 7 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F3 at 22:00:33 Max. shift = 0.000 A for C8 Max. dU = 0.000 for C4 wR2 = 0.1327 before cycle 8 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x N1 at 22:00:35 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C3 wR2 = 0.1327 before cycle 9 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x N1 at 22:00:36 Max. shift = 0.000 A for C8 Max. dU = 0.000 for C9 wR2 = 0.1327 before cycle 10 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x N1 at 22:00:36 Max. shift = 0.000 A for C8 Max. dU = 0.000 for C6 wR2 = 0.1327 before cycle 11 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x N1 at 22:00:37 Max. shift = 0.000 A for C7 Max. dU = 0.000 for N1 wR2 = 0.1327 before cycle 12 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x N1 at 22:00:38 Max. shift = 0.000 A for C8 Max. dU = 0.000 for C12 wR2 = 0.1327 before cycle 13 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x N1 at 22:00:38 Max. shift = 0.000 A for C7 Max. dU = 0.000 for C1 wR2 = 0.1327 before cycle 14 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x N1 at 22:00:39 Max. shift = 0.000 A for F2 Max. dU = 0.000 for C3 wR2 = 0.1327 before cycle 15 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x N1 at 22:00:40 Max. shift = 0.000 A for C7 Max. dU = 0.000 for F2 wR2 = 0.1327 before cycle 16 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x N1 at 22:00:41 Max. shift = 0.000 A for C4 Max. dU = 0.000 for F1 wR2 = 0.1327 before cycle 17 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x F2 at 22:00:41 Max. shift = 0.000 A for C8 Max. dU = 0.000 for C7 wR2 = 0.1327 before cycle 18 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for OSF at 22:00:42 Max. shift = 0.000 A for C4 Max. dU = 0.000 for F3 wR2 = 0.1327 before cycle 19 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x N1 at 22:00:43 Max. shift = 0.000 A for C8 Max. dU = 0.000 for F3 wR2 = 0.1327 before cycle 20 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x N1 at 22:00:44 Max. shift = 0.000 A for C1 Max. dU = 0.000 for C13 wR2 = 0.1327 before cycle 21 for 1815 data and 0 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints R1 = 0.0493 for 1473 Fo > 4sig(Fo) and 0.0668 for all 1815 data wR2 = 0.1327, GooF = S = 1.032, Restrained GooF = 1.032 for all data R1 = 0.0667 for 1815 unique reflections after merging for Fourier Highest peak 0.17 at 0.5959 0.1474 0.1574 [ 1.39 A from H11 ] Deepest hole -0.26 at 0.2343 0.0338 0.1178 [ 0.83 A from C7 ] +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2010sl0004a finished at 22:00:44 Total CPU time: 6.4 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 + + 2010sl0004a started at 22:17:25 on 29-Mar-2011 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Read instructions and data - 2010sl0004a.hkl Data: 1815 unique, 0 suppressed R(int) = 0.0722 R(sigma) = 0.0532 Systematic absence violations: 0 Bad equivalents: 2 ** Cell contents from UNIT instruction and atom list do not agree ** wR2 = 0.1371 before cycle 1 for 1815 data and 154 / 154 parameters GooF = S = 1.067; Restrained GooF = 1.067 for 0 restraints Mean shift/su = 0.542 Maximum = 1.819 for OSF at 22:17:39 Max. shift = 0.004 A for C9 Max. dU = 0.001 for C2 wR2 = 0.1330 before cycle 2 for 1815 data and 154 / 154 parameters GooF = S = 1.035; Restrained GooF = 1.035 for 0 restraints Mean shift/su = 0.205 Maximum = 0.641 for OSF at 22:17:40 Max. shift = 0.001 A for C11 Max. dU = 0.000 for C2 wR2 = 0.1327 before cycle 3 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.013 Maximum = 0.048 for U11 C2 at 22:17:40 Max. shift = 0.000 A for C11 Max. dU = 0.000 for C2 wR2 = 0.1327 before cycle 4 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.002 Maximum = 0.014 for U33 C2 at 22:17:41 Max. shift = 0.000 A for C1 Max. dU = 0.000 for C2 wR2 = 0.1327 before cycle 5 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.001 for U22 F3 at 22:17:42 Max. shift = 0.000 A for C11 Max. dU = 0.000 for C2 wR2 = 0.1327 before cycle 6 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x N1 at 22:17:42 Max. shift = 0.000 A for N1 Max. dU = 0.000 for C13 wR2 = 0.1327 before cycle 7 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for y F3 at 22:17:44 Max. shift = 0.000 A for C8 Max. dU = 0.000 for C4 wR2 = 0.1327 before cycle 8 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x N1 at 22:17:45 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C3 wR2 = 0.1327 before cycle 9 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x N1 at 22:17:45 Max. shift = 0.000 A for C8 Max. dU = 0.000 for C9 wR2 = 0.1327 before cycle 10 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x N1 at 22:17:46 Max. shift = 0.000 A for C8 Max. dU = 0.000 for C6 wR2 = 0.1327 before cycle 11 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x N1 at 22:17:47 Max. shift = 0.000 A for C7 Max. dU = 0.000 for N1 wR2 = 0.1327 before cycle 12 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x N1 at 22:17:48 Max. shift = 0.000 A for C8 Max. dU = 0.000 for C12 wR2 = 0.1327 before cycle 13 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x N1 at 22:17:48 Max. shift = 0.000 A for C7 Max. dU = 0.000 for C1 wR2 = 0.1327 before cycle 14 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x N1 at 22:17:49 Max. shift = 0.000 A for F2 Max. dU = 0.000 for C3 wR2 = 0.1327 before cycle 15 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x N1 at 22:17:50 Max. shift = 0.000 A for C7 Max. dU = 0.000 for F2 wR2 = 0.1327 before cycle 16 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x N1 at 22:17:51 Max. shift = 0.000 A for C4 Max. dU = 0.000 for F1 wR2 = 0.1327 before cycle 17 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x F2 at 22:17:51 Max. shift = 0.000 A for C8 Max. dU = 0.000 for C7 wR2 = 0.1327 before cycle 18 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for OSF at 22:17:52 Max. shift = 0.000 A for C4 Max. dU = 0.000 for F3 wR2 = 0.1327 before cycle 19 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x N1 at 22:17:53 Max. shift = 0.000 A for C8 Max. dU = 0.000 for F3 wR2 = 0.1327 before cycle 20 for 1815 data and 154 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Mean shift/su = 0.000 Maximum = 0.000 for x N1 at 22:17:54 Max. shift = 0.000 A for C1 Max. dU = 0.000 for C13 wR2 = 0.1327 before cycle 21 for 1815 data and 0 / 154 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints R1 = 0.0493 for 1473 Fo > 4sig(Fo) and 0.0668 for all 1815 data wR2 = 0.1327, GooF = S = 1.032, Restrained GooF = 1.032 for all data R1 = 0.0667 for 1815 unique reflections after merging for Fourier Highest peak 0.17 at 0.5959 0.1474 0.1574 [ 1.39 A from H11 ] Deepest hole -0.26 at 0.2343 0.0338 0.1178 [ 0.83 A from C7 ] +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2010sl0004a finished at 22:17:56 Total CPU time: 6.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ When refining structures with SHELXL-97 please quote the following reference: G. M. Sheldrick (2008) Acta Cryst., A64, 112-122.