+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - MSDOS 32-BIT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-1 + + S92 started at 09:56:52 on 22-Jul-1999 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in Pbca CELL 0.71073 14.600 5.572 18.483 90.00 90.00 90.00 ZERR 8.00 0.003 0.001 0.004 0.00 0.00 0.00 LATT 1 SYMM .5-X, -Y, .5+Z SYMM -X, .5+Y, .5-Z SYMM .5+X, .5-Y, -Z SFAC C H N O S UNIT 48 64 16 16 8 V = 1503.61 F(000) = 720.0 Mu = 0.38 mm-1 Cell Wt = 1377.63 Rho = 1.521 ACTA L.S. 4 FMAP 2 PLAN 10 BOND WGHT 0.0545 0.7425 FVAR 0.36961 S1 5 0.89586 0.24460 0.55985 11.00000 0.01539 0.01853 = 0.01728 -0.00077 0.00051 0.00039 O1 4 0.84401 0.02916 0.54526 11.00000 0.02402 0.02247 = 0.02319 -0.00425 -0.00095 -0.00333 O2 4 0.99238 0.24536 0.54362 11.00000 0.01639 0.02674 = 0.02518 0.00053 0.00323 0.00265 N1 3 0.86626 0.44472 0.87305 11.00000 0.03461 0.03815 = 0.02020 -0.00379 -0.00172 -0.00789 N2 3 0.85182 0.45573 0.51079 11.00000 0.02037 0.02416 = 0.02222 0.00457 -0.00083 0.00178 C1 1 0.87324 0.39798 0.80029 11.00000 0.01668 0.02602 = 0.01960 -0.00134 -0.00265 0.00249 C2 1 0.83427 0.19120 0.77074 11.00000 0.01875 0.02438 = 0.02180 0.00284 0.00057 -0.00292 C3 1 0.83820 0.14706 0.69715 11.00000 0.01763 0.01795 = 0.02295 -0.00152 -0.00122 -0.00250 C4 1 0.88193 0.31023 0.65189 11.00000 0.01543 0.02048 = 0.01687 -0.00114 -0.00019 0.00146 C5 1 0.92073 0.51911 0.68042 11.00000 0.01944 0.01851 = 0.02392 0.00141 -0.00046 -0.00110 C6 1 0.91590 0.56307 0.75358 11.00000 0.02163 0.01903 = 0.02335 -0.00320 -0.00320 -0.00048 H1A 2 0.84462 0.32198 0.89906 11.00000 0.04724 H1B 2 0.90452 0.54810 0.88983 11.00000 0.04222 H2A 2 0.79090 0.49187 0.52216 11.00000 0.03563 H2B 2 0.88598 0.57194 0.50660 11.00000 0.03955 H2 2 0.80520 0.07728 0.80317 11.00000 0.02922 H3 2 0.81249 0.00380 0.67714 11.00000 0.02248 H5 2 0.95031 0.63725 0.64958 11.00000 0.02310 H6 2 0.94139 0.70569 0.77252 11.00000 0.02668 HKLF 4 1 0.0000-1.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 0.0000-1.0000 Covalent radii and connectivity table for s92 in Pbca C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 S1 - O2 O1 N2 C4 O1 - S1 O2 - S1 N1 - C1 N2 - S1 C1 - N1 C2 C6 C2 - C3 C1 C3 - C2 C4 C4 - C3 C5 S1 C5 - C6 C4 C6 - C5 C1 h k l Fo^2 Sigma Why rejected 3 0 1 1.85 0.44 observed but should be systematically absent 1 0 3 4.38 0.55 observed but should be systematically absent 3 0 3 2.93 0.65 observed but should be systematically absent 0 1 2 4.08 0.43 observed but should be systematically absent 0 1 10 2.83 0.54 observed but should be systematically absent 1 1 0 0.86 0.11 observed but should be systematically absent 17797 Reflections read, of which 1701 rejected -18 =< h =< 18, -6 =< k =< 7, -23 =< l =< 23, Max. 2-theta = 54.90 6 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 2 0 0 303.98 7.10 5 36.48 0 2 0 34.56 1.13 3 9.80 18 2 0 261.26 14.47 3 91.20 0 0 2 8.36 0.11 2 94.69 1 0 2 567.55 9.14 5 113.90 8 4 2 179.65 2.35 12 13.50 12 4 10 7.42 1.14 5 5.98 7 Inconsistent equivalents 1707 Unique reflections, of which 0 suppressed R(int) = 0.0407 R(sigma) = 0.0292 Friedel opposites merged Maximum memory for data reduction = 1128 / 17191 Least-squares cycle 1 Maximum vector length = 511 Memory required = 1440 / 167963 wR2 = 0.0949 before cycle 1 for 1707 data and 132 / 132 parameters GooF = S = 1.014; Restrained GooF = 1.014 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0545 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36961 0.00099 -0.003 OSF Mean shift/esd = 0.008 Maximum = 0.124 for z S1 Max. shift = 0.000 A for C6 Max. dU = 0.000 for H1A Least-squares cycle 2 Maximum vector length = 511 Memory required = 1440 / 167963 wR2 = 0.0949 before cycle 2 for 1707 data and 132 / 132 parameters GooF = S = 1.014; Restrained GooF = 1.014 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0545 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36961 0.00099 0.000 OSF Mean shift/esd = 0.003 Maximum = 0.044 for z S1 Max. shift = 0.000 A for H5 Max. dU = 0.000 for H1A Least-squares cycle 3 Maximum vector length = 511 Memory required = 1440 / 167963 wR2 = 0.0949 before cycle 3 for 1707 data and 132 / 132 parameters GooF = S = 1.014; Restrained GooF = 1.014 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0545 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36961 0.00099 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for U23 N2 Max. shift = 0.000 A for H1A Max. dU = 0.000 for H1A Least-squares cycle 4 Maximum vector length = 511 Memory required = 1440 / 167963 wR2 = 0.0949 before cycle 4 for 1707 data and 132 / 132 parameters GooF = S = 1.014; Restrained GooF = 1.014 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0545 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36961 0.00099 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z S1 Max. shift = 0.000 A for H1A Max. dU = 0.000 for H1B Largest correlation matrix elements 0.563 U11 S1 / OSF 0.546 U33 S1 / OSF 0.537 U22 S1 / OSF s92 in Pbca ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq S1 0.89586 0.24460 0.55985 1.00000 0.01539 0.01853 0.01728 -0.00077 0.00051 0.00039 0.01707 0.00060 0.00002 0.00006 0.00002 0.00000 0.00023 0.00024 0.00024 0.00012 0.00012 0.00012 0.00015 O1 0.84401 0.02916 0.54526 1.00000 0.02402 0.02247 0.02319 -0.00425 -0.00095 -0.00333 0.02323 0.00182 0.00007 0.00020 0.00006 0.00000 0.00057 0.00057 0.00059 0.00044 0.00042 0.00043 0.00027 O2 0.99238 0.24536 0.54362 1.00000 0.01639 0.02674 0.02518 0.00053 0.00323 0.00265 0.02277 0.00195 0.00008 0.00018 0.00006 0.00000 0.00057 0.00064 0.00060 0.00043 0.00044 0.00040 0.00028 N1 0.86626 0.44472 0.87305 1.00000 0.03461 0.03815 0.02020 -0.00379 -0.00172 -0.00789 0.03099 0.00273 0.00011 0.00031 0.00008 0.00000 0.00081 0.00086 0.00073 0.00065 0.00061 0.00071 0.00035 N2 0.85182 0.45573 0.51079 1.00000 0.02037 0.02416 0.02222 0.00457 -0.00083 0.00178 0.02225 0.00251 0.00009 0.00026 0.00008 0.00000 0.00066 0.00071 0.00069 0.00055 0.00052 0.00054 0.00030 C1 0.87324 0.39798 0.80029 1.00000 0.01668 0.02602 0.01960 -0.00134 -0.00265 0.00249 0.02077 0.00268 0.00010 0.00029 0.00008 0.00000 0.00069 0.00080 0.00075 0.00060 0.00054 0.00059 0.00033 C2 0.83427 0.19120 0.77074 1.00000 0.01875 0.02438 0.02180 0.00284 0.00057 -0.00292 0.02164 0.00273 0.00010 0.00029 0.00009 0.00000 0.00072 0.00076 0.00078 0.00063 0.00058 0.00061 0.00033 C3 0.83820 0.14706 0.69715 1.00000 0.01763 0.01795 0.02295 -0.00152 -0.00122 -0.00250 0.01951 0.00263 0.00010 0.00028 0.00008 0.00000 0.00070 0.00076 0.00077 0.00059 0.00054 0.00060 0.00033 C4 0.88193 0.31023 0.65189 1.00000 0.01543 0.02048 0.01687 -0.00114 -0.00019 0.00146 0.01759 0.00253 0.00010 0.00028 0.00008 0.00000 0.00064 0.00070 0.00070 0.00058 0.00054 0.00054 0.00030 C5 0.92073 0.51911 0.68042 1.00000 0.01944 0.01851 0.02392 0.00141 -0.00046 -0.00110 0.02063 0.00270 0.00010 0.00027 0.00009 0.00000 0.00070 0.00074 0.00080 0.00060 0.00059 0.00059 0.00033 C6 0.91590 0.56307 0.75358 1.00000 0.02163 0.01903 0.02335 -0.00320 -0.00320 -0.00048 0.02133 0.00268 0.00010 0.00027 0.00009 0.00000 0.00072 0.00073 0.00079 0.00061 0.00059 0.00060 0.00033 H1A 0.84462 0.32198 0.89906 1.00000 0.04724 0.04140 0.00158 0.00446 0.00138 0.00000 0.00633 H1B 0.90452 0.54810 0.88983 1.00000 0.04222 0.04239 0.00149 0.00420 0.00128 0.00000 0.00610 H2A 0.79090 0.49187 0.52216 1.00000 0.03563 0.03481 0.00146 0.00346 0.00120 0.00000 0.00525 H2B 0.88598 0.57194 0.50660 1.00000 0.03955 0.04083 0.00161 0.00401 0.00127 0.00000 0.00601 H2 0.80520 0.07728 0.80317 1.00000 0.02922 0.03333 0.00134 0.00354 0.00106 0.00000 0.00498 H3 0.81249 0.00380 0.67714 1.00000 0.02248 0.03305 0.00125 0.00323 0.00102 0.00000 0.00446 H5 0.95031 0.63725 0.64958 1.00000 0.02310 0.03045 0.00119 0.00337 0.00098 0.00000 0.00442 H6 0.94139 0.70569 0.77252 1.00000 0.02668 0.03582 0.00125 0.00355 0.00110 0.00000 0.00480 Final Structure Factor Calculation for s92 in Pbca Total number of l.s. parameters = 132 Maximum vector length = 511 Memory required = 1308 / 24017 wR2 = 0.0949 before cycle 5 for 1707 data and 0 / 132 parameters GooF = S = 1.014; Restrained GooF = 1.014 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0545 * P )^2 + 0.74 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0339 for 1433 Fo > 4sig(Fo) and 0.0426 for all 1707 data wR2 = 0.0949, GooF = S = 1.014, Restrained GooF = 1.014 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 0.0189 0.0171 0.0152 S1 0.0279 0.0246 0.0171 O1 0.0281 0.0253 0.0149 O2 0.0446 0.0297 0.0186 N1 0.0280 0.0214 0.0174 N2 0.0272 0.0202 0.0149 C1 0.0268 0.0212 0.0169 C2 0.0234 0.0203 0.0148 C3 0.0212 0.0166 0.0150 C4 0.0244 0.0199 0.0176 C5 0.0265 0.0210 0.0165 C6 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.013 0.029 0.045 0.065 0.090 0.118 0.161 0.215 0.306 1.000 Number in group 171. 175. 174. 165. 169. 171. 172. 172. 167. 171. GooF 0.943 0.999 1.011 1.129 1.008 1.023 1.006 1.014 0.993 1.009 K 1.554 0.999 1.009 0.952 0.967 0.969 1.002 1.011 1.033 0.988 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.66 inf Number in group 178. 165. 178. 162. 173. 168. 173. 168. 172. 170. GooF 0.910 0.874 0.831 0.856 0.829 0.983 0.914 0.870 1.070 1.697 K 1.009 1.016 1.032 1.009 1.013 1.048 1.023 1.014 1.008 0.961 R1 0.103 0.068 0.054 0.038 0.037 0.044 0.031 0.023 0.027 0.047 Recommended weighting scheme: WGHT 0.0545 0.7425 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 3 1 4 37.85 14.56 5.22 0.030 2.87 3 1 6 301.58 212.24 4.74 0.116 2.36 4 0 2 83.63 47.97 4.70 0.055 3.39 5 1 6 73.05 119.77 4.48 0.087 1.98 9 0 4 541.60 419.75 3.84 0.164 1.53 2 3 2 193.36 262.46 3.73 0.129 1.77 6 2 4 224.42 168.24 3.62 0.104 1.70 7 0 6 191.24 256.22 3.51 0.128 1.73 1 2 4 184.77 245.66 3.45 0.125 2.35 5 4 6 93.08 131.60 3.35 0.092 1.16 8 1 0 7.55 0.52 3.31 0.006 1.73 4 2 2 517.14 417.66 3.27 0.163 2.15 2 1 6 349.04 440.82 3.26 0.168 2.53 7 3 4 10.95 2.35 3.19 0.012 1.33 0 0 18 953.10 749.18 3.11 0.218 1.03 1 1 3 191.38 246.96 3.11 0.125 3.98 2 3 5 56.78 37.55 3.07 0.049 1.62 2 1 2 1092.86 1312.29 3.00 0.289 3.99 2 3 3 1199.34 1009.74 2.93 0.254 1.73 8 2 4 8.12 18.31 2.85 0.034 1.45 2 2 1 23.28 13.02 2.79 0.029 2.58 3 3 4 489.27 406.74 2.78 0.161 1.62 6 1 4 341.39 280.54 2.77 0.134 2.01 8 1 4 1095.52 935.03 2.68 0.244 1.62 5 1 4 1587.92 1851.91 2.60 0.344 2.26 3 2 6 453.77 541.11 2.58 0.186 1.90 11 1 19 22.82 49.76 2.56 0.056 0.78 1 1 16 399.24 333.42 2.53 0.146 1.13 1 2 16 77.75 104.08 2.51 0.081 1.06 8 5 10 58.30 39.03 2.48 0.050 0.85 5 1 1 35.04 23.28 2.48 0.039 2.56 6 0 2 2040.40 1774.53 2.45 0.336 2.35 1 0 2 4154.53 6257.23 2.43 0.631 7.81 6 0 0 2758.23 2397.35 2.42 0.391 2.43 10 6 0 2009.82 1565.47 2.42 0.316 0.78 4 5 16 19.32 43.80 2.41 0.053 0.78 9 6 2 112.52 78.74 2.40 0.071 0.80 4 0 6 9.57 3.00 2.40 0.014 2.35 5 6 4 1.81 12.05 2.38 0.028 0.87 3 4 1 53.50 38.16 2.36 0.049 1.34 0 2 17 20.43 36.24 2.36 0.048 1.01 6 5 7 30.39 17.13 2.35 0.033 0.95 15 0 14 13.26 47.03 2.35 0.055 0.78 10 5 3 -2.95 4.85 2.35 0.018 0.88 1 2 6 859.55 744.10 2.34 0.218 2.05 1 7 4 408.61 534.97 2.32 0.185 0.78 5 2 5 10.97 5.26 2.30 0.018 1.77 4 2 4 1195.46 1044.40 2.29 0.258 2.00 3 0 4 5601.53 6383.33 2.27 0.638 3.35 6 4 6 115.13 91.33 2.27 0.076 1.13 Bond lengths and angles S1 - Distance Angles O2 1.4407 (0.0012) O1 1.4446 (0.0011) 118.43 (0.07) N2 1.6185 (0.0014) 105.65 (0.07) 106.93 (0.07) C4 1.7518 (0.0015) 108.37 (0.07) 107.09 (0.07) 110.25 (0.07) S1 - O2 O1 N2 O1 - Distance Angles S1 1.4446 (0.0011) O1 - O2 - Distance Angles S1 1.4407 (0.0012) O2 - N1 - Distance Angles C1 1.3736 (0.0021) N1 - N2 - Distance Angles S1 1.6185 (0.0014) N2 - C1 - Distance Angles N1 1.3736 (0.0021) C2 1.3963 (0.0022) 120.61 (0.15) C6 1.4068 (0.0022) 120.64 (0.15) 118.68 (0.14) C1 - N1 C2 C2 - Distance Angles C3 1.3834 (0.0023) C1 1.3963 (0.0022) 120.95 (0.15) C2 - C3 C3 - Distance Angles C2 1.3834 (0.0023) C4 1.3907 (0.0022) 119.62 (0.14) C3 - C2 C4 - Distance Angles C3 1.3907 (0.0022) C5 1.3977 (0.0022) 120.23 (0.14) S1 1.7518 (0.0015) 120.06 (0.12) 119.55 (0.12) C4 - C3 C5 C5 - Distance Angles C6 1.3761 (0.0023) C4 1.3977 (0.0022) 119.88 (0.14) C5 - C6 C6 - Distance Angles C5 1.3761 (0.0023) C1 1.4068 (0.0022) 120.61 (0.14) C6 - C5 FMAP and GRID set by program FMAP 2 2 10 GRID -3.571 24 -2 3.571 1 2 R1 = 0.0423 for 1707 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.27 at 0.8993 0.0407 0.2773 [ 0.67 A from C1 ] Deepest hole -0.52 at 0.4176 0.1476 0.4384 [ 0.68 A from S1 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 2032 / 22384 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.8993 0.4593 0.7773 1.00000 0.05 0.27 0.67 C1 0.76 C6 1.51 H6 1.77 C2 Q2 1 0.8923 0.2795 0.6187 1.00000 0.05 0.27 0.65 C4 1.11 S1 1.80 C5 1.81 C3 Q3 1 0.8788 0.2870 0.9005 1.00000 0.05 0.23 0.54 H1A 1.03 N1 1.52 H1B 1.96 C1 Q4 1 0.8534 0.3069 0.7894 1.00000 0.05 0.22 0.62 C1 0.78 C2 1.48 H2 1.74 N1 Q5 1 0.8662 0.2307 0.6708 1.00000 0.05 0.21 0.61 C4 0.79 C3 1.49 H3 1.80 C5 Q6 1 0.8081 0.2523 0.9415 1.00000 0.05 0.20 1.03 H1A 1.84 N2 1.86 N1 2.03 H2A Q7 1 0.9165 0.3427 0.6707 1.00000 0.05 0.18 0.64 C4 1.00 C5 1.65 C3 1.76 H5 Q8 1 0.8630 0.0962 0.8708 1.00000 0.05 0.18 1.39 H1A 1.51 H2 1.94 N1 1.97 C2 Q9 1 0.8266 0.1959 0.7302 1.00000 0.05 0.17 0.69 C3 0.76 C2 1.47 H3 1.53 H2 Q10 1 0.8608 0.1434 0.9273 1.00000 0.05 0.17 1.15 H1A 1.64 N2 1.93 H2B 1.96 N1 Shortest distances between peaks (including symmetry equivalents) 5 7 0.96 3 10 0.98 6 10 1.01 2 5 1.07 8 10 1.08 2 7 1.08 1 4 1.10 3 8 1.22 5 9 1.25 3 6 1.29 4 9 1.32 6 8 1.76 7 9 1.90 4 8 1.91 1 9 2.01 1 7 2.09 3 4 2.09 4 5 2.24 2 9 2.32 4 7 2.39 1 5 2.39 1 3 2.49 4 10 2.71 8 9 2.71 1 8 2.71 4 6 2.90 Time profile in seconds ----------------------- 0.16: 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. 1.27: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.05: Set up l.s. refinement 0.00: Generate idealized H-atoms 2.30: Structure factors and derivatives 1.89: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.19: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.22: Analysis of variance 0.17: Merge reflections for Fourier and .fcf 0.28: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 09:56:59 Total elapsed time: 6.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++