+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 13:57:05 on 30-Aug-2005 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P2(1)/c CELL 0.71073 8.8690 8.9150 9.9620 90.000 110.400 90.000 ZERR 2.00 0.0020 0.0020 0.0020 0.000 0.030 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O S UNIT 24 24 6 6 4 V = 738.27 F(000) = 322.0 Mu = 0.37 mm-1 Cell Wt = 620.73 Rho = 1.396 MERG 2 FMAP 2 ACTA PLAN 10 WGHT 0.04800 0.34400 L.S. 4 FVAR 1.06936 S11 5 0.080010 0.143220 0.788510 11.00000 0.01591 0.01379 = 0.01735 -0.00151 0.00553 -0.00067 O11 4 0.005370 0.138000 0.634270 11.00000 0.02048 0.02527 = 0.01736 -0.00435 0.00425 -0.00385 O12 4 0.114810 0.003640 0.866000 11.00000 0.02247 0.01519 = 0.03005 0.00274 0.00822 -0.00095 C14 1 0.261270 0.241140 0.827640 11.00000 0.01545 0.01497 = 0.01695 -0.00178 0.00517 -0.00053 C13 1 0.266720 0.371040 0.750800 11.00000 0.01668 0.01771 = 0.01772 0.00133 0.00478 0.00128 C15 1 0.400050 0.189230 0.934600 11.00000 0.02011 0.01570 = 0.01887 0.00140 0.00568 0.00123 C16 1 0.544420 0.264620 0.963040 11.00000 0.01680 0.02044 = 0.01974 0.00001 0.00310 0.00138 C12 1 0.410180 0.447730 0.780800 11.00000 0.01946 0.01810 = 0.01834 0.00115 0.00661 -0.00108 N11 3 0.694810 0.468120 0.910560 11.00000 0.01700 0.02595 = 0.02754 -0.00011 0.00707 -0.00350 C11 1 0.551970 0.395260 0.886180 11.00000 0.01555 0.01980 = 0.01825 -0.00304 0.00685 -0.00019 N12 3 -0.044990 0.233730 0.843620 11.00000 0.02141 0.02108 = 0.02350 -0.00170 0.01029 0.00248 H16 2 0.642070 0.230050 1.038770 11.00000 0.02065 H13 2 0.173320 0.409260 0.681800 11.00000 0.02481 H15 2 0.395820 0.097410 0.989320 11.00000 0.03038 H12 2 0.411190 0.542520 0.727600 11.00000 0.02840 H10 2 0.780230 0.445700 0.989460 11.00000 0.03446 H17 2 -0.014290 0.247510 0.934550 11.00000 0.03895 H18 2 -0.075610 0.317980 0.800470 11.00000 0.03187 H11 2 0.691760 0.557840 0.879510 11.00000 0.03626 HKLF 4 Covalent radii and connectivity table for s92 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 S11 - O12 O11 N12 C14 O11 - S11 O12 - S11 C14 - C15 C13 S11 C13 - C12 C14 C15 - C16 C14 C16 - C15 C11 C12 - C13 C11 N11 - C11 C11 - N11 C12 C16 N12 - S11 h k l Fo^2 Sigma Why rejected -3 0 7 6.60 1.65 observed but should be systematically absent -2 0 5 46.61 3.88 observed but should be systematically absent -1 0 1 1.53 0.35 observed but should be systematically absent -1 0 3 1.64 0.23 observed but should be systematically absent 0 0 1 1.06 0.24 observed but should be systematically absent 0 0 1 1.18 0.24 observed but should be systematically absent 0 7 0 5.65 1.41 observed but should be systematically absent 0 11 0 11.97 2.93 observed but should be systematically absent 1 0 5 2.44 0.35 observed but should be systematically absent 2 0 1 9.47 1.07 observed but should be systematically absent 2 0 3 2.10 0.47 observed but should be systematically absent 13564 Reflections read, of which 432 rejected -12 =< h =< 12, -11 =< k =< 11, -13 =< l =< 14, Max. 2-theta = 61.03 11 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 8 0 0 100.30 3.13 4 16.65 -3 2 5 5.44 0.22 11 2.86 2 Inconsistent equivalents 2135 Unique reflections, of which 0 suppressed R(int) = 0.0298 R(sigma) = 0.0245 Friedel opposites merged Maximum memory for data reduction = 1104 / 21169 ** Cell contents from UNIT instruction and atom list do not agree ** Unit-cell contents from UNIT instruction and atom list resp. C 24.00 24.00 H 24.00 32.00 N 6.00 8.00 O 6.00 8.00 S 4.00 4.00 Least-squares cycle 1 Maximum vector length = 511 Memory required = 1416 / 167963 wR2 = 0.0896 before cycle 1 for 2135 data and 132 / 132 parameters GooF = S = 1.056; Restrained GooF = 1.056 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0480 * P )^2 + 0.34 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.06821 0.00230 -0.502 OSF Mean shift/esd = 0.190 Maximum = -0.829 for U22 S11 Max. shift = 0.008 A for H10 Max. dU =-0.001 for H13 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1416 / 167963 wR2 = 0.0894 before cycle 2 for 2135 data and 132 / 132 parameters GooF = S = 1.056; Restrained GooF = 1.056 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0480 * P )^2 + 0.34 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.06746 0.00229 -0.324 OSF Mean shift/esd = 0.065 Maximum = -0.324 for OSF Max. shift = 0.003 A for H18 Max. dU = 0.000 for H13 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1416 / 167963 wR2 = 0.0894 before cycle 3 for 2135 data and 132 / 132 parameters GooF = S = 1.057; Restrained GooF = 1.057 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0480 * P )^2 + 0.34 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.06746 0.00229 -0.001 OSF Mean shift/esd = 0.004 Maximum = 0.018 for x H13 Max. shift = 0.000 A for H18 Max. dU = 0.000 for H17 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1416 / 167963 wR2 = 0.0894 before cycle 4 for 2135 data and 132 / 132 parameters GooF = S = 1.057; Restrained GooF = 1.057 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0480 * P )^2 + 0.34 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.06747 0.00229 0.004 OSF Mean shift/esd = 0.001 Maximum = 0.009 for y H10 Max. shift = 0.000 A for H10 Max. dU = 0.000 for H18 Largest correlation matrix elements 0.555 U22 S11 / OSF 0.545 U33 S11 / OSF 0.550 U11 S11 / OSF 0.504 U13 S11 / U33 S11 s92 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq S11 0.08002 0.14322 0.78850 1.00000 0.01580 0.01361 0.01726 -0.00152 0.00555 -0.00068 0.01562 0.00054 0.00003 0.00003 0.00003 0.00000 0.00016 0.00016 0.00016 0.00008 0.00011 0.00009 0.00010 O11 0.00539 0.13798 0.63434 1.00000 0.02045 0.02504 0.01732 -0.00431 0.00434 -0.00383 0.02153 0.00174 0.00011 0.00010 0.00010 0.00000 0.00044 0.00048 0.00043 0.00030 0.00033 0.00032 0.00020 O12 0.11481 0.00364 0.86599 1.00000 0.02218 0.01509 0.02955 0.00269 0.00801 -0.00102 0.02254 0.00186 0.00011 0.00010 0.00010 0.00000 0.00044 0.00041 0.00048 0.00033 0.00035 0.00032 0.00020 C14 0.26127 0.24115 0.82767 1.00000 0.01539 0.01487 0.01670 -0.00190 0.00521 -0.00059 0.01575 0.00224 0.00014 0.00013 0.00012 0.00000 0.00049 0.00050 0.00050 0.00037 0.00037 0.00038 0.00021 C13 0.26677 0.37103 0.75083 1.00000 0.01656 0.01748 0.01735 0.00119 0.00468 0.00135 0.01745 0.00240 0.00015 0.00013 0.00013 0.00000 0.00053 0.00053 0.00053 0.00038 0.00040 0.00039 0.00023 C15 0.40009 0.18930 0.93462 1.00000 0.02015 0.01550 0.01862 0.00128 0.00578 0.00126 0.01835 0.00239 0.00014 0.00013 0.00013 0.00000 0.00054 0.00054 0.00053 0.00039 0.00041 0.00042 0.00023 C16 0.54437 0.26463 0.96302 1.00000 0.01674 0.02028 0.01938 -0.00008 0.00303 0.00153 0.01966 0.00239 0.00014 0.00014 0.00013 0.00000 0.00053 0.00056 0.00055 0.00042 0.00041 0.00042 0.00024 C12 0.41013 0.44766 0.78079 1.00000 0.01959 0.01792 0.01816 0.00101 0.00674 -0.00105 0.01852 0.00237 0.00015 0.00014 0.00012 0.00000 0.00053 0.00054 0.00053 0.00040 0.00040 0.00042 0.00023 N11 0.69477 0.46811 0.91053 1.00000 0.01675 0.02587 0.02728 -0.00001 0.00690 -0.00342 0.02351 0.00228 0.00013 0.00014 0.00013 0.00000 0.00049 0.00058 0.00057 0.00042 0.00041 0.00041 0.00023 C11 0.55194 0.39526 0.88616 1.00000 0.01554 0.01962 0.01806 -0.00312 0.00694 -0.00020 0.01745 0.00233 0.00014 0.00014 0.00012 0.00000 0.00051 0.00053 0.00052 0.00041 0.00039 0.00041 0.00022 N12 -0.04495 0.23372 0.84359 1.00000 0.02117 0.02102 0.02320 -0.00172 0.01009 0.00245 0.02117 0.00228 0.00013 0.00013 0.00012 0.00000 0.00051 0.00052 0.00055 0.00039 0.00040 0.00040 0.00022 H16 0.64247 0.23022 1.03851 1.00000 0.02094 0.03320 0.00203 0.00184 0.00177 0.00000 0.00385 H13 0.17334 0.40886 0.68146 1.00000 0.02301 0.03382 0.00202 0.00200 0.00176 0.00000 0.00392 H15 0.39562 0.09784 0.98883 1.00000 0.02935 0.03639 0.00218 0.00211 0.00188 0.00000 0.00440 H12 0.41063 0.54287 0.72774 1.00000 0.02758 0.03473 0.00207 0.00206 0.00185 0.00000 0.00434 H10 0.77932 0.44525 0.98958 1.00000 0.03387 0.03854 0.00237 0.00221 0.00201 0.00000 0.00475 H17 -0.01426 0.24669 0.93380 1.00000 0.03911 0.04213 0.00245 0.00228 0.00226 0.00000 0.00521 H18 -0.07687 0.31805 0.79979 1.00000 0.03217 0.03854 0.00233 0.00238 0.00206 0.00000 0.00468 H11 0.69148 0.55832 0.87886 1.00000 0.03706 0.03848 0.00236 0.00241 0.00202 0.00000 0.00507 Final Structure Factor Calculation for s92 in P2(1)/c Total number of l.s. parameters = 132 Maximum vector length = 511 Memory required = 1284 / 24017 wR2 = 0.0894 before cycle 5 for 2135 data and 0 / 132 parameters GooF = S = 1.056; Restrained GooF = 1.056 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0480 * P )^2 + 0.34 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0322 for 1966 Fo > 4sig(Fo) and 0.0349 for all 2135 data wR2 = 0.0894, GooF = S = 1.056, Restrained GooF = 1.056 for all data Occupancy sum of asymmetric unit = 11.00 for non-hydrogen and 8.00 for hydrogen atoms Principal mean square atomic displacements U 0.0179 0.0159 0.0130 S11 0.0275 0.0227 0.0145 O11 0.0310 0.0223 0.0143 O12 0.0180 0.0156 0.0136 C14 0.0189 0.0184 0.0150 C13 0.0212 0.0190 0.0149 C15 0.0238 0.0201 0.0151 C16 0.0204 0.0188 0.0164 C12 0.0285 0.0266 0.0154 N11 0.0221 0.0164 0.0139 C11 0.0242 0.0235 0.0158 N12 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.021 0.038 0.058 0.079 0.101 0.128 0.159 0.198 0.281 1.000 Number in group 221. 207. 214. 214. 217. 209. 215. 211. 212. 215. GooF 1.060 1.011 1.100 1.209 1.086 0.927 1.106 1.015 1.020 1.000 K 1.102 0.961 0.931 0.947 0.966 0.993 1.006 1.017 1.024 1.001 Resolution(A) 0.70 0.74 0.77 0.80 0.85 0.89 0.97 1.07 1.22 1.52 inf Number in group 220. 208. 216. 213. 212. 211. 216. 214. 211. 214. GooF 1.007 0.823 0.916 0.786 0.894 0.762 0.952 1.118 1.042 1.837 K 0.961 1.001 1.026 1.044 1.041 1.025 1.009 1.013 1.011 0.984 R1 0.064 0.047 0.044 0.037 0.035 0.028 0.030 0.026 0.023 0.037 Recommended weighting scheme: WGHT 0.0452 0.3658 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) -1 2 5 10.15 1.88 6.16 0.016 1.81 2 3 1 168.38 115.38 5.26 0.129 2.23 -2 0 4 45.51 25.20 5.24 0.060 2.43 -1 4 2 79.77 122.46 5.16 0.133 2.03 3 1 0 13.34 4.61 5.06 0.026 2.65 2 1 4 90.19 129.94 4.56 0.137 1.75 4 3 1 3.19 0.09 4.22 0.004 1.60 3 1 2 25.18 42.09 4.16 0.078 2.03 -1 7 3 12.55 22.78 3.59 0.057 1.19 -7 4 2 3.06 0.13 3.56 0.004 1.10 0 2 3 25.32 39.12 3.51 0.075 2.55 7 4 1 31.82 48.36 3.50 0.084 1.01 -1 0 6 71.10 51.36 3.47 0.086 1.64 6 5 0 8.80 3.64 3.37 0.023 1.09 2 4 3 9.86 4.56 3.36 0.026 1.55 1 1 2 696.30 840.34 3.35 0.349 3.32 2 5 3 40.86 28.11 3.33 0.064 1.37 -7 3 1 16.65 8.94 3.27 0.036 1.14 4 0 0 25.08 15.60 3.21 0.048 2.08 0 0 4 505.64 418.62 3.20 0.246 2.33 -1 0 4 72.53 95.70 3.18 0.118 2.48 -2 6 6 3.89 0.92 3.18 0.012 1.11 1 2 0 201.17 247.55 3.12 0.189 3.93 1 3 2 68.26 51.48 3.11 0.086 2.28 3 1 3 183.37 149.38 3.03 0.147 1.75 0 2 5 143.06 115.66 2.97 0.130 1.72 2 1 2 546.31 646.94 2.93 0.306 2.56 -1 3 4 1162.32 998.20 2.89 0.380 1.91 -1 7 6 24.71 35.55 2.83 0.072 1.01 -2 4 4 25.10 35.93 2.83 0.072 1.64 0 2 7 257.94 216.09 2.80 0.177 1.28 0 0 8 6.50 13.33 2.75 0.044 1.17 -4 0 6 166.01 201.54 2.74 0.171 1.53 0 4 0 7.35 13.84 2.71 0.045 2.23 5 3 4 115.12 141.33 2.71 0.143 1.09 0 5 3 479.90 411.54 2.70 0.244 1.55 -2 9 5 27.09 38.20 2.67 0.074 0.89 -2 0 2 1586.00 1836.39 2.61 0.516 3.84 -4 3 6 23.52 16.25 2.58 0.049 1.36 -1 5 1 130.79 108.08 2.58 0.125 1.74 -6 1 1 16.80 9.28 2.56 0.037 1.43 6 4 1 318.03 372.78 2.55 0.232 1.13 -3 2 6 49.02 37.31 2.52 0.074 1.52 -11 5 7 23.24 34.90 2.47 0.071 0.72 1 0 0 1359.00 1562.82 2.46 0.476 8.31 3 1 1 175.33 207.27 2.45 0.173 2.35 3 0 2 35.94 47.08 2.44 0.083 2.09 9 2 5 39.54 52.05 2.43 0.087 0.72 0 1 1 212.15 248.52 2.42 0.190 6.45 -1 8 4 61.32 76.99 2.42 0.106 1.02 Bond lengths and angles S11 - Distance Angles O12 1.4399 (0.0009) O11 1.4457 (0.0010) 118.34 (0.06) N12 1.6139 (0.0011) 107.10 (0.06) 105.25 (0.06) C14 1.7496 (0.0012) 107.64 (0.06) 107.33 (0.06) 111.17 (0.06) S11 - O12 O11 N12 O11 - Distance Angles S11 1.4457 (0.0010) O11 - O12 - Distance Angles S11 1.4399 (0.0009) O12 - C14 - Distance Angles C15 1.3965 (0.0017) C13 1.3982 (0.0016) 120.13 (0.11) S11 1.7496 (0.0012) 120.14 (0.09) 119.72 (0.09) C14 - C15 C13 C13 - Distance Angles C12 1.3813 (0.0017) C14 1.3982 (0.0016) 119.77 (0.11) C13 - C12 C15 - Distance Angles C16 1.3842 (0.0017) C14 1.3965 (0.0017) 120.11 (0.11) C15 - C16 C16 - Distance Angles C15 1.3842 (0.0017) C11 1.4082 (0.0017) 120.40 (0.11) C16 - C15 C12 - Distance Angles C13 1.3813 (0.0017) C11 1.4077 (0.0017) 120.86 (0.11) C12 - C13 N11 - Distance Angles C11 1.3678 (0.0016) N11 - C11 - Distance Angles N11 1.3678 (0.0016) C12 1.4077 (0.0017) 120.41 (0.12) C16 1.4082 (0.0017) 120.86 (0.11) 118.71 (0.11) C11 - N11 C12 N12 - Distance Angles S11 1.6139 (0.0011) N12 - FMAP and GRID set by program FMAP 2 2 15 GRID -2.083 -2 -2 2.083 2 2 R1 = 0.0346 for 2135 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.32 at 0.5585 0.1823 0.4071 [ 0.72 A from C11 ] Deepest hole -0.50 at 0.0064 0.1124 0.7641 [ 0.67 A from S11 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 1501 / 16224 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5585 0.3177 0.9071 1.00000 0.05 0.32 0.72 C11 0.77 C16 1.48 H16 1.80 N11 Q2 1 0.3342 0.2172 0.8811 1.00000 0.05 0.31 0.69 C15 0.71 C14 1.47 H15 1.81 C16 Q3 1 0.4839 0.4251 0.8309 1.00000 0.05 0.29 0.70 C12 0.71 C11 1.45 H12 1.80 N11 Q4 1 0.1995 0.2036 0.8217 1.00000 0.05 0.28 0.63 C14 1.13 S11 1.75 C15 1.84 C13 Q5 1 0.2533 0.3066 0.8063 1.00000 0.05 0.27 0.62 C14 0.83 C13 1.51 H13 1.81 C15 Q6 1 0.4774 0.2307 0.9437 1.00000 0.05 0.25 0.63 C16 0.76 C15 1.44 H16 1.54 H15 Q7 1 0.3419 0.4145 0.7747 1.00000 0.05 0.25 0.66 C12 0.73 C13 1.45 H12 1.46 H13 Q8 1 0.7716 0.3502 1.1432 1.00000 0.05 0.23 1.65 H16 1.77 H10 2.11 O11 2.22 N12 Q9 1 -0.0781 0.0653 0.7141 1.00000 0.05 0.19 1.42 O11 1.51 S11 1.93 O12 1.93 N12 Q10 1 0.0184 0.2009 0.8276 1.00000 0.05 0.19 0.70 N12 0.93 S11 1.26 H17 1.31 H18 Shortest distances between peaks (including symmetry equivalents) 4 5 1.07 2 4 1.14 2 5 1.15 3 7 1.19 1 6 1.20 2 6 1.21 1 3 1.26 5 7 1.35 8 9 1.48 4 10 1.63 9 10 1.67 2 7 2.07 3 6 2.08 5 6 2.09 1 7 2.10 1 2 2.11 3 5 2.24 4 6 2.35 6 7 2.36 8 10 2.36 5 10 2.36 4 7 2.40 2 3 2.43 1 8 2.47 1 5 2.54 7 8 2.58 4 9 2.62 2 10 2.67 7 9 2.73 5 9 2.75 6 8 2.88 Time profile in seconds ----------------------- 0.06: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.63: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.23: Structure factors and derivatives 0.31: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.05: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 13:57:07 Total CPU time: 1.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++