+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - MSDOS 32-BIT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-1 + + S92 started at 14:02:47 on 16-Jul-1999 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P2(1)/c CELL 0.71073 7.824 12.991 7.620 90.00 104.97 90.00 ZERR 4.00 0.002 0.003 0.002 0.00 0.03 0.00 LATT 1 SYMM -X, .5+Y, .5-Z SFAC C H N O S UNIT 24 32 8 8 4 V = 748.22 F(000) = 360.0 Mu = 0.38 mm-1 Cell Wt = 688.82 Rho = 1.529 ACTA L.S. 4 FMAP 2 PLAN 10 BOND WGHT 0.043800 0.266200 FVAR 0.55560 S1 5 0.60449 0.83868 0.04022 11.00000 0.02051 0.02709 = 0.01654 -0.00177 0.00060 -0.00362 O1 4 0.59752 0.72874 0.01663 11.00000 0.03181 0.02755 = 0.02760 -0.00672 0.00372 -0.00784 O2 4 0.56360 0.90303 -0.11979 11.00000 0.02922 0.03678 = 0.01693 0.00183 0.00097 -0.00403 N1 3 1.31603 0.95149 0.48847 11.00000 0.02047 0.04099 = 0.02977 -0.00384 -0.00108 -0.00228 N2 3 0.45935 0.86704 0.15048 11.00000 0.01937 0.03515 = 0.02096 0.00161 0.00267 -0.00114 C1 1 1.14973 0.92395 0.38740 11.00000 0.01662 0.03180 = 0.01986 -0.00454 0.00448 0.00025 C2 1 1.08403 0.82483 0.39307 11.00000 0.02311 0.02985 = 0.03497 0.00808 -0.00082 0.00414 C3 1 0.91885 0.79857 0.28625 11.00000 0.02543 0.02067 = 0.03785 0.00196 0.00340 -0.00006 C4 1 0.81640 0.87088 0.17061 11.00000 0.01728 0.02368 = 0.01760 -0.00156 0.00238 -0.00188 C5 1 0.88025 0.97015 0.16515 11.00000 0.02365 0.02697 = 0.03178 0.00736 0.00008 -0.00116 C6 1 1.04559 0.99593 0.27306 11.00000 0.02508 0.02488 = 0.03818 0.00287 0.00118 -0.00588 H1A 2 1.33960 1.01476 0.50316 11.00000 0.04897 H1B 2 1.36631 0.91454 0.58248 11.00000 0.05169 H2A 2 0.45263 0.93306 0.16024 11.00000 0.03771 H2B 2 0.47677 0.83522 0.25847 11.00000 0.03911 H2 2 1.15432 0.77335 0.46405 11.00000 0.04926 H3 2 0.86945 0.73083 0.29328 11.00000 0.04562 H5 2 0.81119 1.02379 0.09097 11.00000 0.03858 H6 2 1.08896 1.06318 0.26554 11.00000 0.04378 HKLF 4 1 0.0000 0.0000 1.0000 0.0000-1.0000 0.0000 1.0000 0.0000 0.0000 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 S1 - O1 O2 N2 C4 O1 - S1 O2 - S1 N1 - C1 N2 - S1 C1 - N1 C6 C2 C2 - C3 C1 C3 - C2 C4 C4 - C5 C3 S1 C5 - C6 C4 C6 - C5 C1 h k l Fo^2 Sigma Why rejected -1 0 1 0.54 0.11 observed but should be systematically absent 1 0 1 2.40 0.33 observed but should be systematically absent 7148 Reflections read, of which 212 rejected -9 =< h =< 10, -16 =< k =< 16, -9 =< l =< 9, Max. 2-theta = 54.91 2 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 1 0 0 400.13 9.98 4 101.08 -1 1 1 40.63 0.11 4 203.91 -1 3 3 4.98 0.22 4 4.78 -4 4 3 80.33 0.22 5 53.96 4 Inconsistent equivalents 1704 Unique reflections, of which 0 suppressed R(int) = 0.0390 R(sigma) = 0.0426 Friedel opposites merged Maximum memory for data reduction = 1104 / 16822 Least-squares cycle 1 Maximum vector length = 511 Memory required = 1416 / 167963 wR2 = 0.0926 before cycle 1 for 1704 data and 132 / 132 parameters GooF = S = 1.055; Restrained GooF = 1.055 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0438 * P )^2 + 0.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55560 0.00139 -0.002 OSF Mean shift/esd = 0.005 Maximum = 0.057 for y S1 Max. shift = 0.000 A for H1B Max. dU = 0.000 for H1A Least-squares cycle 2 Maximum vector length = 511 Memory required = 1416 / 167963 wR2 = 0.0926 before cycle 2 for 1704 data and 132 / 132 parameters GooF = S = 1.055; Restrained GooF = 1.055 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0438 * P )^2 + 0.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55560 0.00139 0.001 OSF Mean shift/esd = 0.002 Maximum = 0.020 for y S1 Max. shift = 0.000 A for H1A Max. dU = 0.000 for H1B Least-squares cycle 3 Maximum vector length = 511 Memory required = 1416 / 167963 wR2 = 0.0927 before cycle 3 for 1704 data and 132 / 132 parameters GooF = S = 1.055; Restrained GooF = 1.055 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0438 * P )^2 + 0.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55560 0.00139 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for y H2 Max. shift = 0.000 A for H2 Max. dU = 0.000 for H1B Least-squares cycle 4 Maximum vector length = 511 Memory required = 1416 / 167963 wR2 = 0.0926 before cycle 4 for 1704 data and 132 / 132 parameters GooF = S = 1.055; Restrained GooF = 1.055 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0438 * P )^2 + 0.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55560 0.00139 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y S1 Max. shift = 0.000 A for H2 Max. dU = 0.000 for H3 Largest correlation matrix elements 0.556 U33 S1 / OSF 0.555 U11 S1 / OSF 0.534 U22 S1 / OSF s92 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq S1 0.60449 0.83868 0.04022 1.00000 0.02051 0.02709 0.01654 -0.00177 0.00060 -0.00362 0.02215 0.00070 0.00005 0.00003 0.00005 0.00000 0.00024 0.00025 0.00022 0.00015 0.00016 0.00015 0.00016 O1 0.59752 0.72874 0.01663 1.00000 0.03181 0.02756 0.02760 -0.00672 0.00372 -0.00784 0.02972 0.00213 0.00016 0.00009 0.00016 0.00000 0.00070 0.00068 0.00065 0.00049 0.00053 0.00049 0.00031 O2 0.56360 0.90303 -0.11979 1.00000 0.02922 0.03678 0.01693 0.00183 0.00097 -0.00403 0.02856 0.00216 0.00015 0.00010 0.00015 0.00000 0.00064 0.00070 0.00056 0.00048 0.00047 0.00052 0.00030 N1 1.31603 0.95149 0.48847 1.00000 0.02047 0.04099 0.02977 -0.00384 -0.00108 -0.00228 0.03181 0.00301 0.00019 0.00015 0.00022 0.00000 0.00074 0.00098 0.00083 0.00077 0.00063 0.00068 0.00037 N2 0.45935 0.86704 0.15048 1.00000 0.01937 0.03515 0.02096 0.00161 0.00267 -0.00114 0.02563 0.00280 0.00018 0.00013 0.00020 0.00000 0.00069 0.00088 0.00072 0.00066 0.00055 0.00062 0.00033 C1 1.14973 0.92395 0.38740 1.00000 0.01662 0.03180 0.01986 -0.00454 0.00448 0.00025 0.02280 0.00300 0.00020 0.00013 0.00021 0.00000 0.00074 0.00089 0.00075 0.00066 0.00060 0.00063 0.00035 C2 1.08403 0.82483 0.39307 1.00000 0.02311 0.02985 0.03497 0.00808 -0.00082 0.00414 0.03085 0.00354 0.00023 0.00014 0.00027 0.00000 0.00087 0.00093 0.00099 0.00077 0.00075 0.00069 0.00042 C3 0.91885 0.79857 0.28625 1.00000 0.02543 0.02067 0.03785 0.00196 0.00340 -0.00006 0.02887 0.00344 0.00023 0.00014 0.00026 0.00000 0.00086 0.00080 0.00098 0.00076 0.00074 0.00070 0.00040 C4 0.81640 0.87088 0.17061 1.00000 0.01728 0.02368 0.01760 -0.00156 0.00238 -0.00188 0.01992 0.00283 0.00020 0.00012 0.00020 0.00000 0.00072 0.00077 0.00073 0.00062 0.00059 0.00060 0.00033 C5 0.88025 0.97015 0.16515 1.00000 0.02365 0.02697 0.03178 0.00736 0.00008 -0.00116 0.02877 0.00328 0.00023 0.00014 0.00025 0.00000 0.00083 0.00088 0.00092 0.00073 0.00073 0.00070 0.00040 C6 1.04559 0.99593 0.27306 1.00000 0.02508 0.02488 0.03818 0.00287 0.00118 -0.00588 0.03067 0.00339 0.00023 0.00014 0.00026 0.00000 0.00086 0.00087 0.00099 0.00076 0.00075 0.00070 0.00041 H1A 1.33960 1.01476 0.50316 1.00000 0.04897 0.04857 0.00317 0.00209 0.00336 0.00000 0.00707 H1B 1.36631 0.91454 0.58248 1.00000 0.05169 0.04848 0.00334 0.00197 0.00366 0.00000 0.00682 H2A 0.45263 0.93306 0.16024 1.00000 0.03771 0.04083 0.00268 0.00185 0.00287 0.00000 0.00596 H2B 0.47677 0.83522 0.25847 1.00000 0.03911 0.04444 0.00296 0.00157 0.00352 0.00000 0.00590 H2 1.15432 0.77335 0.46405 1.00000 0.04926 0.04516 0.00324 0.00185 0.00325 0.00000 0.00659 H3 0.86945 0.73083 0.29328 1.00000 0.04562 0.04427 0.00303 0.00178 0.00309 0.00000 0.00626 H5 0.81119 1.02379 0.09097 1.00000 0.03858 0.03923 0.00267 0.00163 0.00293 0.00000 0.00561 H6 1.08896 1.06318 0.26554 1.00000 0.04378 0.04276 0.00286 0.00173 0.00304 0.00000 0.00591 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 = 0.0926 before cycle 5 for 1704 data and 0 / 132 parameters GooF = S = 1.055; Restrained GooF = 1.055 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0438 * P )^2 + 0.27 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0359 for 1438 Fo > 4sig(Fo) and 0.0465 for all 1704 data wR2 = 0.0926, GooF = S = 1.055, Restrained GooF = 1.055 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 0.0289 0.0236 0.0140 S1 0.0379 0.0334 0.0178 O1 0.0401 0.0294 0.0161 O2 0.0423 0.0358 0.0173 N1 0.0356 0.0233 0.0180 N2 0.0335 0.0184 0.0166 C1 0.0444 0.0311 0.0170 C2 0.0414 0.0248 0.0204 C3 0.0242 0.0203 0.0152 C4 0.0423 0.0241 0.0199 C5 0.0455 0.0274 0.0191 C6 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.019 0.036 0.055 0.075 0.095 0.120 0.154 0.197 0.275 1.000 Number in group 181. 161. 173. 170. 168. 172. 171. 167. 170. 171. GooF 0.937 1.075 1.105 1.138 1.131 0.998 1.014 0.961 0.993 1.177 K 1.233 1.018 0.984 0.958 0.963 0.983 1.002 1.018 1.033 0.981 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.67 inf Number in group 176. 173. 164. 170. 173. 170. 167. 171. 171. 169. GooF 0.818 0.895 0.928 0.927 0.874 0.942 1.077 0.951 1.156 1.709 K 1.007 1.032 1.033 1.010 1.010 1.020 1.018 1.024 1.012 0.957 R1 0.086 0.078 0.070 0.063 0.045 0.039 0.034 0.024 0.031 0.045 Recommended weighting scheme: WGHT 0.0438 0.2662 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 3 1.25 7.70 4.55 0.033 2.06 3 5 0 82.20 58.33 4.28 0.090 1.81 1 6 0 156.73 117.98 4.23 0.128 2.08 -2 3 1 21.60 12.56 3.95 0.042 2.85 1 4 1 6.23 1.60 3.86 0.015 2.67 2 2 1 662.11 810.12 3.85 0.335 2.77 1 8 0 109.05 81.75 3.84 0.106 1.59 1 3 3 2.97 0.20 3.50 0.005 1.94 6 2 1 57.05 77.05 3.40 0.103 1.17 1 2 1 1830.53 2148.86 3.22 0.545 3.81 -2 4 4 19.14 11.80 3.22 0.040 1.61 -1 6 9 20.83 49.04 3.12 0.082 0.78 0 3 2 20.68 13.33 3.04 0.043 2.80 -3 1 3 218.75 181.13 3.03 0.158 2.02 -2 6 1 479.48 407.01 3.00 0.237 1.88 1 7 5 24.41 36.32 3.00 0.071 1.11 0 3 1 2391.73 2780.22 2.92 0.620 3.73 0 0 4 34.13 47.49 2.88 0.081 1.84 -2 1 1 325.82 383.41 2.87 0.230 3.63 -3 5 2 29.87 40.53 2.85 0.075 1.76 2 8 4 2.88 8.10 2.81 0.033 1.11 2 4 2 883.20 767.08 2.79 0.326 1.90 -1 8 3 39.16 28.69 2.77 0.063 1.37 3 11 5 28.99 45.03 2.76 0.079 0.82 -1 4 5 60.47 46.95 2.73 0.081 1.38 -1 3 1 4800.77 5514.24 2.72 0.874 3.54 -3 2 2 19.36 27.34 2.71 0.062 2.24 1 12 1 199.07 165.23 2.66 0.151 1.05 -2 4 1 250.64 214.52 2.64 0.172 2.46 -4 10 4 7.71 1.54 2.62 0.015 0.99 6 4 2 12.02 19.62 2.62 0.052 1.05 1 9 0 166.16 140.02 2.56 0.139 1.42 -5 4 8 16.57 29.84 2.55 0.064 0.86 -1 1 1 131.61 1827.10 2.52 0.503 5.54 1 6 3 6.43 2.81 2.51 0.020 1.53 -2 11 1 81.74 99.93 2.48 0.118 1.13 5 2 3 5.97 11.20 2.47 0.039 1.14 0 10 0 192.92 160.60 2.46 0.149 1.30 1 15 2 43.67 59.68 2.45 0.091 0.83 0 2 1 4322.54 4903.38 2.44 0.824 4.87 -4 1 5 50.29 63.02 2.41 0.093 1.33 -1 9 7 44.18 59.24 2.40 0.091 0.86 0 14 2 19.47 29.25 2.40 0.064 0.90 -2 7 1 15.35 21.64 2.39 0.055 1.67 -3 6 1 22.42 29.98 2.38 0.064 1.66 -2 4 3 266.62 231.16 2.36 0.179 1.91 -1 5 1 8.50 4.86 2.34 0.026 2.39 -1 1 3 663.14 583.72 2.33 0.284 2.49 0 15 2 10.38 3.42 2.32 0.022 0.84 4 9 2 42.67 53.87 2.29 0.086 1.05 Bond lengths and angles S1 - Distance Angles O1 1.4388 (0.0013) O2 1.4444 (0.0012) 118.43 (0.07) N2 1.6199 (0.0016) 106.36 (0.08) 105.91 (0.08) C4 1.7493 (0.0016) 107.94 (0.07) 108.17 (0.08) 109.85 (0.08) S1 - O1 O2 N2 O1 - Distance Angles S1 1.4388 (0.0013) O1 - O2 - Distance Angles S1 1.4444 (0.0012) O2 - N1 - Distance Angles C1 1.3771 (0.0021) N1 - N2 - Distance Angles S1 1.6199 (0.0016) N2 - C1 - Distance Angles N1 1.3771 (0.0021) C6 1.3895 (0.0024) 119.48 (0.17) C2 1.3913 (0.0025) 121.76 (0.16) 118.74 (0.15) C1 - N1 C6 C2 - Distance Angles C3 1.3805 (0.0025) C1 1.3913 (0.0025) 120.50 (0.16) C2 - C3 C3 - Distance Angles C2 1.3805 (0.0025) C4 1.3916 (0.0023) 120.33 (0.16) C3 - C2 C4 - Distance Angles C5 1.3875 (0.0024) C3 1.3916 (0.0023) 119.57 (0.15) S1 1.7493 (0.0016) 120.07 (0.12) 120.31 (0.13) C4 - C5 C3 C5 - Distance Angles C6 1.3829 (0.0024) C4 1.3875 (0.0024) 119.74 (0.16) C5 - C6 C6 - Distance Angles C5 1.3829 (0.0024) C1 1.3895 (0.0024) 121.12 (0.17) C6 - C5 FMAP and GRID set by program FMAP 2 3 12 GRID -2.778 -2 -2 2.778 2 2 R1 = 0.0463 for 1704 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.25 at 0.9736 0.9772 0.2129 [ 0.67 A from C6 ] Deepest hole -0.48 at 0.6216 0.8125 0.1174 [ 0.66 A from S1 ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 1485 / 14940 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.9736 0.9772 0.2129 1.00000 0.05 0.25 0.67 C6 0.73 C5 1.43 H6 1.49 H5 Q2 1 1.3888 0.9852 0.4473 1.00000 0.05 0.25 0.75 H1A 0.84 N1 1.42 H1B 1.97 C1 Q3 1 1.0830 1.0225 0.2328 1.00000 0.05 0.25 0.58 H6 0.59 C6 1.68 C5 1.73 C1 Q4 1 1.1913 0.6628 0.3913 1.00000 0.05 0.22 1.59 H2 1.81 H5 2.27 C2 2.51 N2 Q5 1 1.0965 0.9552 0.3212 1.00000 0.05 0.22 0.70 C1 0.71 C6 1.46 H6 1.79 C2 Q6 1 1.1882 1.0686 0.2801 1.00000 0.05 0.22 0.76 H6 1.45 C6 1.93 H1A 2.10 C1 Q7 1 1.0385 1.0843 0.0885 1.00000 0.05 0.22 1.33 H6 1.81 C6 1.95 H5 2.11 C5 Q8 1 0.8472 1.0035 -0.0045 1.00000 0.05 0.21 0.89 H5 1.32 C5 2.23 C4 2.28 C6 Q9 1 0.9030 1.0825 -0.0607 1.00000 0.05 0.21 1.69 H5 2.04 C6 2.16 C5 2.30 C5 Q10 1 1.2010 0.9016 0.1669 1.00000 0.05 0.20 1.85 C1 2.02 H2A 2.04 C6 2.11 N2 Shortest distances between peaks (including symmetry equivalents) 3 6 1.01 9 10 1.01 1 3 1.02 3 5 1.09 1 5 1.13 8 9 1.23 3 7 1.33 7 9 1.34 6 7 1.63 7 8 1.67 5 6 1.70 8 10 1.72 1 8 1.73 5 10 1.74 2 2 1.76 7 8 1.82 1 7 1.83 1 9 1.86 3 9 1.91 4 9 1.95 3 10 1.95 3 8 1.98 1 6 2.01 5 9 2.05 2 6 2.06 4 7 2.11 1 10 2.14 8 9 2.19 7 9 2.24 3 8 2.24 4 10 2.24 6 8 2.25 2 5 2.27 4 8 2.29 7 10 2.33 6 10 2.35 8 8 2.38 1 8 2.39 5 7 2.40 1 7 2.41 1 9 2.43 3 9 2.44 2 10 2.51 6 9 2.56 7 7 2.56 2 3 2.57 5 8 2.62 9 9 2.65 7 10 2.69 1 4 2.75 3 7 2.76 3 4 2.79 5 8 2.80 6 9 2.96 Time profile in seconds ----------------------- 0.11: 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. 0.50: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.61: Structure factors and derivatives 1.80: 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 0.11: Other dependent quantities, CIF, tables 0.22: Analysis of variance 0.11: Merge reflections for Fourier and .fcf 0.11: Fourier summations 0.11: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 14:02:52 Total elapsed time: 4.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++