+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 12:41:24 on 13-Nov-2000 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P2(1)/n CELL 0.71073 12.1793 9.6098 13.3527 90.000 101.921 90.000 ZERR 4.00 0.0024 0.0019 0.0027 0.000 0.030 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O S UNIT 52 68 20 8 8 V = 1529.10 F(000) = 712.0 Mu = 0.36 mm-1 Cell Wt = 1357.74 Rho = 1.474 MERG 2 SHEL 7 0.84 ACTA FMAP 2 PLAN 20 BOND L.S. 1 WGHT 0.054100 0.896500 EXTI 0.005397 FVAR 0.46890 S12 5 1.001748 0.132900 0.846963 11.00000 0.03032 0.02166 = 0.05243 -0.00501 0.01971 0.00092 C17 1 0.896878 0.227088 0.888770 11.00000 0.02505 0.01926 = 0.01801 -0.00017 0.00694 0.00081 N13 3 0.920227 0.359150 0.903858 11.00000 0.02984 0.01898 = 0.03789 -0.00355 0.01628 -0.00350 N22 3 0.749235 -0.379195 0.881827 11.00000 0.03165 0.01355 = 0.03507 -0.00105 0.00820 -0.00222 C24 1 0.682817 -0.281118 0.899464 11.00000 0.02711 0.02451 = 0.02601 -0.00304 0.00369 -0.00064 C22 1 0.852128 -0.322698 0.856651 11.00000 0.02425 0.02756 = 0.03097 0.00179 0.00831 0.00162 C18 1 1.024880 0.387965 0.883036 11.00000 0.03315 0.02300 = 0.04494 -0.00175 0.01863 -0.00679 C19 1 1.080318 0.282416 0.851901 11.00000 0.02535 0.03030 = 0.04820 -0.00123 0.01711 -0.00211 C21 1 0.834841 -0.166100 0.863891 11.00000 0.03430 0.02566 = 0.03222 -0.00161 0.00907 -0.00588 C25 1 0.573778 -0.307990 0.927224 11.00000 0.03117 0.03587 = 0.05314 -0.00522 0.01593 -0.00524 H13 2 0.895557 0.148287 1.106179 11.00000 0.01200 H16 2 0.716033 0.512210 1.238586 11.00000 0.02817 H12 2 0.964049 0.226336 1.270628 11.00000 0.02311 H15 2 0.649372 0.439828 1.069436 11.00000 0.02213 H22A 2 0.859330 -0.352341 0.787117 11.00000 0.04163 H22B 2 0.913466 -0.349871 0.903951 11.00000 0.03038 H21A 2 0.827742 -0.118864 0.796156 11.00000 0.03979 H25A 2 0.549680 -0.397240 0.906679 11.00000 0.04810 H19 2 1.146990 0.278483 0.835807 11.00000 0.04134 H21B 2 0.890175 -0.124081 0.916639 11.00000 0.02720 H25B 2 0.531228 -0.229752 0.898622 11.00000 0.06808 H11 2 0.955655 0.403882 1.394955 11.00000 0.03527 H10 2 0.858438 0.494198 1.391565 11.00000 0.04343 H25C 2 0.582991 -0.300372 0.999213 11.00000 0.05460 H18 2 1.050800 0.476369 0.894217 11.00000 0.03824 H21N 2 0.692356 -0.085736 0.898270 11.00000 0.05925 H22 2 0.735267 -0.461192 0.883286 11.00000 0.03121 MOLE 1 S11 5 0.710380 0.225234 0.946717 11.00000 0.01969 0.01421 = 0.02188 -0.00023 0.00436 -0.00195 O11 4 0.631266 0.113671 0.955925 11.00000 0.02236 0.01926 = 0.02924 0.00097 0.00579 -0.00589 N12 3 0.805425 0.153422 0.902505 11.00000 0.02488 0.01483 = 0.02521 -0.00243 0.00865 -0.00167 O12 4 0.656483 0.344870 0.889806 11.00000 0.02525 0.01822 = 0.02311 0.00209 0.00180 0.00011 C13 1 0.859234 0.221957 1.131757 11.00000 0.01787 0.01610 = 0.02736 0.00108 0.00919 0.00191 C15 1 0.713892 0.394720 1.111858 11.00000 0.01471 0.02145 = 0.02578 0.00225 0.00526 0.00262 N21 3 0.723647 -0.156808 0.889517 11.00000 0.03311 0.01731 = 0.04081 -0.00150 0.01198 0.00096 C14 1 0.765875 0.285576 1.071572 11.00000 0.01621 0.01673 = 0.02097 0.00052 0.00649 -0.00263 C12 1 0.900053 0.267117 1.230411 11.00000 0.01887 0.02271 = 0.02356 0.00458 0.00363 0.00189 C11 1 0.848472 0.377344 1.271503 11.00000 0.02057 0.02621 = 0.02055 0.00065 0.00842 -0.00547 N11 3 0.888834 0.421147 1.370055 11.00000 0.02763 0.04357 = 0.02380 -0.00856 0.00298 0.00532 C16 1 0.753582 0.439280 1.210775 11.00000 0.01954 0.02334 = 0.02439 -0.00350 0.00996 0.00091 HKLF 4 Covalent radii and connectivity table for s92 in P2(1)/n C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 S12 - C19 C17 C17 - N13 N12 S12 N13 - C17 C18 N22 - C24 C22 C24 - N22 N21 C25 C22 - N22 C21 C18 - C19 N13 C19 - C18 S12 C21 - N21 C22 C25 - C24 S11 - O12 O11 N12 C14 O11 - S11 N12 - C17 S11 O12 - S11 C13 - C12 C14 C15 - C16 C14 N21 - C24 C21 C14 - C15 C13 S11 C12 - C13 C11 C11 - N11 C12 C16 N11 - C11 C16 - C15 C11 h k l Fo^2 Sigma Why rejected 0 3 0 1.62 0.22 observed but should be systematically absent 2 0 5 7.73 1.52 observed but should be systematically absent 11591 Reflections read, of which 1662 rejected -14 =< h =< 14, -11 =< k =< 11, -15 =< l =< 15, Max. 2-theta = 50.05 2 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -2 5 3 190.68 0.53 5 65.14 -2 7 6 164.84 0.75 4 70.63 2 8 7 28.82 0.68 6 5.86 -2 8 8 21.24 1.87 2 14.66 4 Inconsistent equivalents 2697 Unique reflections, of which 0 suppressed R(int) = 0.0387 R(sigma) = 0.0363 Friedel opposites merged Maximum memory for data reduction = 1912 / 26898 Least-squares cycle 1 Maximum vector length = 511 Memory required = 2546 / 334495 wR2 = 0.0918 before cycle 1 for 2697 data and 268 / 268 parameters GooF = S = 0.941; Restrained GooF = 0.941 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0541 * P )^2 + 0.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.46885 0.00116 -0.039 OSF 2 0.00525 0.00152 -0.096 EXTI Mean shift/esd = 0.196 Maximum = 0.791 for U11 C11 Max. shift = 0.017 A for H22B Max. dU =-0.003 for H21N Largest correlation matrix elements 0.543 EXTI / OSF 0.516 U22 S11 / OSF 0.512 U33 S11 / OSF s92 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq S12 1.00176 0.13290 0.84696 1.00000 0.03032 0.02168 0.05255 -0.00501 0.01972 0.00089 0.03324 0.00106 0.00005 0.00005 0.00005 0.00000 0.00033 0.00029 0.00038 0.00022 0.00026 0.00020 0.00019 C17 0.89692 0.22710 0.88872 1.00000 0.02482 0.01926 0.01817 -0.00046 0.00678 0.00064 0.02041 0.00345 0.00016 0.00018 0.00014 0.00000 0.00106 0.00096 0.00093 0.00070 0.00078 0.00074 0.00042 N13 0.92018 0.35911 0.90390 1.00000 0.03011 0.01895 0.03767 -0.00370 0.01628 -0.00353 0.02757 0.00316 0.00014 0.00016 0.00014 0.00000 0.00098 0.00086 0.00102 0.00067 0.00080 0.00066 0.00041 N22 0.74931 -0.37918 0.88185 1.00000 0.03157 0.01336 0.03563 -0.00124 0.00849 -0.00236 0.02663 0.00325 0.00015 0.00018 0.00013 0.00000 0.00101 0.00089 0.00104 0.00067 0.00078 0.00071 0.00041 C24 0.68274 -0.28117 0.89946 1.00000 0.02756 0.02468 0.02583 -0.00299 0.00375 -0.00070 0.02628 0.00359 0.00017 0.00019 0.00015 0.00000 0.00112 0.00106 0.00109 0.00079 0.00087 0.00082 0.00046 C22 0.85221 -0.32268 0.85673 1.00000 0.02478 0.02749 0.03087 0.00142 0.00881 0.00180 0.02727 0.00420 0.00018 0.00022 0.00018 0.00000 0.00113 0.00107 0.00119 0.00089 0.00096 0.00087 0.00045 C18 1.02486 0.38798 0.88300 1.00000 0.03231 0.02319 0.04510 -0.00149 0.01840 -0.00663 0.03203 0.00431 0.00018 0.00023 0.00018 0.00000 0.00122 0.00111 0.00134 0.00092 0.00101 0.00090 0.00050 C19 1.08032 0.28240 0.85197 1.00000 0.02572 0.03033 0.04815 -0.00142 0.01715 -0.00234 0.03336 0.00425 0.00020 0.00022 0.00018 0.00000 0.00120 0.00118 0.00142 0.00095 0.00106 0.00090 0.00052 C21 0.83490 -0.16609 0.86397 1.00000 0.03402 0.02576 0.03229 -0.00142 0.00935 -0.00568 0.03033 0.00427 0.00019 0.00022 0.00018 0.00000 0.00125 0.00109 0.00123 0.00092 0.00101 0.00091 0.00049 C25 0.57381 -0.30798 0.92724 1.00000 0.03122 0.03572 0.05307 -0.00466 0.01537 -0.00547 0.03904 0.00501 0.00020 0.00028 0.00023 0.00000 0.00131 0.00140 0.00170 0.00118 0.00116 0.00107 0.00057 H13 0.89592 0.14889 1.10606 1.00000 0.01391 0.03366 0.00153 0.00191 0.00138 0.00000 0.00452 H16 0.71624 0.51209 1.23846 1.00000 0.02873 0.03828 0.00176 0.00221 0.00154 0.00000 0.00558 H12 0.96415 0.22647 1.27065 1.00000 0.02365 0.03794 0.00185 0.00200 0.00157 0.00000 0.00527 H15 0.64947 0.44025 1.06968 1.00000 0.02160 0.03748 0.00176 0.00202 0.00153 0.00000 0.00501 H22A 0.86008 -0.35191 0.78741 1.00000 0.04017 0.04603 0.00202 0.00234 0.00199 0.00000 0.00659 H22B 0.91481 -0.35033 0.90399 1.00000 0.03070 0.04284 0.00195 0.00220 0.00182 0.00000 0.00598 H21A 0.82864 -0.11885 0.79652 1.00000 0.04120 0.04382 0.00196 0.00236 0.00194 0.00000 0.00641 H25A 0.55028 -0.39648 0.90660 1.00000 0.04941 0.05306 0.00219 0.00292 0.00198 0.00000 0.00717 H19 1.14744 0.27890 0.83558 1.00000 0.04145 0.04551 0.00226 0.00239 0.00188 0.00000 0.00686 H21B 0.89049 -0.12352 0.91732 1.00000 0.02719 0.04368 0.00187 0.00212 0.00173 0.00000 0.00554 H25B 0.53087 -0.22855 0.89878 1.00000 0.06897 0.05676 0.00265 0.00328 0.00240 0.00000 0.00929 H11 0.95583 0.40362 1.39542 1.00000 0.03525 0.04662 0.00226 0.00245 0.00185 0.00000 0.00671 H10 0.85855 0.49552 1.39154 1.00000 0.04241 0.04571 0.00221 0.00264 0.00185 0.00000 0.00713 H25C 0.58320 -0.29966 0.99967 1.00000 0.05267 0.05328 0.00225 0.00277 0.00232 0.00000 0.00799 H18 1.05129 0.47689 0.89369 1.00000 0.03798 0.04583 0.00201 0.00258 0.00176 0.00000 0.00631 H21N 0.69214 -0.08720 0.89841 1.00000 0.05643 0.05375 0.00241 0.00306 0.00217 0.00000 0.00877 H22 0.73521 -0.45983 0.88255 1.00000 0.03197 0.04267 0.00187 0.00256 0.00163 0.00000 0.00633 S11 0.71038 0.22523 0.94673 1.00000 0.01977 0.01419 0.02193 -0.00019 0.00440 -0.00193 0.01862 0.00081 0.00004 0.00004 0.00003 0.00000 0.00028 0.00026 0.00027 0.00017 0.00019 0.00016 0.00017 O11 0.63130 0.11372 0.95590 1.00000 0.02245 0.01934 0.02905 0.00091 0.00574 -0.00579 0.02356 0.00237 0.00011 0.00013 0.00010 0.00000 0.00072 0.00066 0.00076 0.00053 0.00058 0.00052 0.00032 N12 0.80538 0.15336 0.90251 1.00000 0.02460 0.01489 0.02528 -0.00240 0.00876 -0.00142 0.02107 0.00283 0.00013 0.00015 0.00012 0.00000 0.00089 0.00078 0.00087 0.00061 0.00070 0.00061 0.00037 O12 0.65652 0.34490 0.88980 1.00000 0.02494 0.01827 0.02318 0.00207 0.00168 0.00017 0.02260 0.00233 0.00011 0.00012 0.00010 0.00000 0.00073 0.00067 0.00072 0.00051 0.00056 0.00052 0.00032 C13 0.85920 0.22199 1.13176 1.00000 0.01846 0.01609 0.02712 0.00109 0.00902 0.00192 0.01994 0.00352 0.00015 0.00018 0.00015 0.00000 0.00098 0.00093 0.00104 0.00074 0.00081 0.00072 0.00041 C15 0.71383 0.39468 1.11185 1.00000 0.01462 0.02165 0.02553 0.00211 0.00536 0.00258 0.02043 0.00352 0.00015 0.00019 0.00015 0.00000 0.00094 0.00097 0.00104 0.00077 0.00079 0.00076 0.00041 N21 0.72366 -0.15679 0.88952 1.00000 0.03289 0.01725 0.04127 -0.00171 0.01207 0.00078 0.02983 0.00336 0.00015 0.00018 0.00014 0.00000 0.00103 0.00090 0.00110 0.00074 0.00083 0.00074 0.00043 C14 0.76583 0.28555 1.07158 1.00000 0.01668 0.01684 0.02086 0.00058 0.00644 -0.00248 0.01776 0.00322 0.00015 0.00017 0.00014 0.00000 0.00093 0.00090 0.00094 0.00068 0.00075 0.00068 0.00040 C12 0.90009 0.26716 1.23041 1.00000 0.01862 0.02282 0.02363 0.00435 0.00344 0.00163 0.02182 0.00364 0.00017 0.00019 0.00015 0.00000 0.00102 0.00097 0.00101 0.00077 0.00082 0.00077 0.00042 C11 0.84858 0.37742 1.27153 1.00000 0.02135 0.02602 0.02066 0.00060 0.00867 -0.00535 0.02205 0.00348 0.00016 0.00019 0.00014 0.00000 0.00099 0.00099 0.00100 0.00075 0.00080 0.00077 0.00042 N11 0.88889 0.42113 1.37003 1.00000 0.02801 0.04323 0.02366 -0.00817 0.00274 0.00518 0.03200 0.00347 0.00017 0.00022 0.00013 0.00000 0.00109 0.00118 0.00097 0.00081 0.00083 0.00089 0.00044 C16 0.75355 0.43924 1.21073 1.00000 0.01960 0.02334 0.02480 -0.00355 0.01020 0.00101 0.02177 0.00351 0.00016 0.00020 0.00014 0.00000 0.00098 0.00100 0.00102 0.00077 0.00081 0.00077 0.00042 Final Structure Factor Calculation for s92 in P2(1)/n Total number of l.s. parameters = 268 Maximum vector length = 511 Memory required = 2278 / 24017 wR2 = 0.0914 before cycle 2 for 2697 data and 0 / 268 parameters GooF = S = 0.936; Restrained GooF = 0.936 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0541 * P )^2 + 0.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0344 for 2267 Fo > 4sig(Fo) and 0.0433 for all 2697 data wR2 = 0.0914, GooF = S = 0.936, Restrained GooF = 0.936 for all data Occupancy sum of asymmetric unit = 22.00 for non-hydrogen and 17.00 for hydrogen atoms Principal mean square atomic displacements U 0.0558 0.0254 0.0185 S12 0.0252 0.0194 0.0166 C17 0.0432 0.0216 0.0179 N13 0.0360 0.0308 0.0130 N22 0.0296 0.0272 0.0220 C24 0.0323 0.0270 0.0225 C22 0.0498 0.0285 0.0179 C18 0.0502 0.0304 0.0194 C19 0.0377 0.0305 0.0228 C21 0.0554 0.0358 0.0260 C25 0.0219 0.0203 0.0136 S11 0.0293 0.0268 0.0145 O11 0.0284 0.0204 0.0144 N12 0.0285 0.0219 0.0174 O12 0.0284 0.0171 0.0144 C13 0.0265 0.0212 0.0135 C15 0.0425 0.0300 0.0170 N21 0.0217 0.0187 0.0129 C14 0.0276 0.0205 0.0174 C12 0.0296 0.0229 0.0137 C11 0.0489 0.0264 0.0207 N11 0.0286 0.0232 0.0135 C16 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.017 0.033 0.051 0.070 0.093 0.119 0.150 0.196 0.267 1.000 Number in group 284. 256. 276. 275. 259. 268. 275. 264. 269. 271. GooF 0.819 0.994 0.953 0.981 0.958 0.970 0.901 0.901 0.956 0.925 K 0.892 0.988 1.001 0.956 0.969 0.972 0.996 1.005 1.020 1.015 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.06 1.14 1.25 1.43 1.79 inf Number in group 270. 280. 263. 269. 268. 267. 274. 268. 267. 271. GooF 0.850 0.860 0.865 0.816 0.862 0.886 0.774 0.795 1.068 1.411 K 1.007 1.009 1.002 1.012 1.020 1.017 1.017 1.023 1.020 0.997 R1 0.088 0.081 0.057 0.051 0.047 0.036 0.028 0.029 0.034 0.035 Recommended weighting scheme: WGHT 0.0508 0.5356 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) -5 2 4 167.77 108.07 4.79 0.078 1.96 0 3 4 141.54 197.66 3.85 0.106 2.29 4 1 3 125.09 176.31 3.81 0.100 2.19 1 3 1 278.01 364.84 3.77 0.144 2.97 -1 0 5 31.10 56.98 3.77 0.057 2.67 -6 2 1 -1.25 12.14 3.59 0.026 1.87 -5 2 3 28.45 12.47 3.54 0.027 2.07 -1 4 3 0.20 7.48 3.48 0.021 2.11 -4 5 3 31.98 54.56 3.42 0.056 1.57 -4 3 5 12.55 28.51 3.32 0.040 1.82 4 1 2 595.60 731.43 3.31 0.203 2.44 -2 2 4 9.34 1.90 3.30 0.010 2.64 -1 1 3 32.48 53.23 3.28 0.055 4.00 3 0 3 10.63 1.29 3.21 0.009 2.67 0 2 5 474.25 386.11 3.21 0.148 2.30 -8 6 8 33.00 12.42 3.16 0.026 0.98 -10 2 7 52.64 83.22 3.03 0.069 1.09 2 5 3 26.45 14.09 2.98 0.028 1.65 9 5 6 162.38 215.33 2.97 0.110 0.91 3 2 3 114.81 151.59 2.93 0.093 2.34 -9 1 11 24.04 51.29 2.90 0.054 0.99 -7 1 3 981.51 831.66 2.84 0.217 1.68 5 10 2 89.63 128.30 2.82 0.085 0.87 -1 4 2 237.15 191.12 2.80 0.104 2.24 4 2 1 46.22 67.12 2.79 0.062 2.41 -13 3 3 11.39 37.68 2.79 0.046 0.90 2 5 9 506.43 416.67 2.78 0.153 1.10 -2 1 8 742.40 629.48 2.74 0.189 1.64 -1 2 5 252.14 308.54 2.73 0.132 2.33 4 2 2 265.09 217.08 2.71 0.111 2.23 1 9 1 493.01 600.26 2.70 0.184 1.06 1 10 5 85.83 60.30 2.70 0.058 0.89 -2 4 1 357.05 427.25 2.66 0.155 2.23 -6 9 5 356.55 436.03 2.64 0.157 0.91 6 0 0 25.91 46.44 2.63 0.051 1.99 -8 5 7 475.78 570.65 2.62 0.179 1.08 8 1 2 86.61 115.71 2.61 0.081 1.38 1 3 11 195.33 242.78 2.61 0.117 1.09 -1 3 1 2408.13 2772.14 2.60 0.396 3.05 6 2 2 117.15 150.89 2.60 0.092 1.69 -4 5 14 52.87 21.35 2.59 0.035 0.85 5 2 3 141.23 111.55 2.54 0.079 1.79 3 2 1 729.45 848.31 2.53 0.219 2.88 2 3 5 98.89 126.87 2.53 0.085 1.83 8 1 5 11.69 23.54 2.51 0.036 1.18 0 4 6 71.44 95.41 2.50 0.073 1.61 2 4 0 865.49 1007.19 2.50 0.238 2.23 -6 1 7 109.58 140.70 2.50 0.089 1.51 -9 2 6 196.48 243.00 2.49 0.117 1.21 -6 1 6 354.63 297.00 2.49 0.129 1.62 Bond lengths and angles S12 - Distance Angles C19 1.7197 (0.0022) C17 1.7478 (0.0019) 89.55 (0.10) S12 - C19 C17 - Distance Angles N13 1.3064 (0.0024) N12 1.3652 (0.0024) 129.80 (0.17) S12 1.7478 (0.0019) 113.77 (0.14) 116.41 (0.13) C17 - N13 N12 N13 - Distance Angles C17 1.3064 (0.0024) C18 1.3882 (0.0027) 109.97 (0.17) N13 - C17 N22 - Distance Angles C24 1.2956 (0.0026) C22 1.4669 (0.0028) 111.63 (0.17) N22 - C24 C24 - Distance Angles N22 1.2956 (0.0026) N21 1.3122 (0.0026) 112.26 (0.19) C25 1.4722 (0.0031) 123.29 (0.19) 124.45 (0.20) C24 - N22 N21 C22 - Distance Angles N22 1.4669 (0.0028) C21 1.5253 (0.0030) 102.41 (0.17) C22 - N22 C18 - Distance Angles C19 1.3315 (0.0031) N13 1.3882 (0.0027) 117.14 (0.19) C18 - C19 C19 - Distance Angles C18 1.3315 (0.0031) S12 1.7197 (0.0022) 109.56 (0.17) C19 - C18 C21 - Distance Angles N21 1.4666 (0.0029) C22 1.5253 (0.0030) 102.78 (0.16) C21 - N21 C25 - Distance Angles C24 1.4722 (0.0031) C25 - S11 - Distance Angles O12 1.4576 (0.0013) O11 1.4628 (0.0013) 112.86 (0.08) N12 1.5643 (0.0016) 116.09 (0.08) 105.03 (0.08) C14 1.7624 (0.0019) 106.09 (0.08) 106.98 (0.08) 109.48 (0.09) S11 - O12 O11 N12 O11 - Distance Angles S11 1.4628 (0.0013) O11 - N12 - Distance Angles C17 1.3652 (0.0024) S11 1.5643 (0.0016) 120.67 (0.13) N12 - C17 O12 - Distance Angles S11 1.4576 (0.0013) O12 - C13 - Distance Angles C12 1.3787 (0.0028) C14 1.3908 (0.0026) 120.30 (0.18) C13 - C12 C15 - Distance Angles C16 1.3773 (0.0027) C14 1.3895 (0.0025) 120.51 (0.17) C15 - C16 N21 - Distance Angles C24 1.3122 (0.0026) C21 1.4666 (0.0029) 110.88 (0.17) N21 - C24 C14 - Distance Angles C15 1.3895 (0.0025) C13 1.3908 (0.0026) 119.44 (0.17) S11 1.7624 (0.0019) 119.87 (0.14) 120.66 (0.14) C14 - C15 C13 C12 - Distance Angles C13 1.3787 (0.0028) C11 1.3999 (0.0027) 120.68 (0.18) C12 - C13 C11 - Distance Angles N11 1.3714 (0.0026) C12 1.3999 (0.0027) 120.48 (0.18) C16 1.4011 (0.0028) 121.00 (0.18) 118.50 (0.18) C11 - N11 C12 N11 - Distance Angles C11 1.3714 (0.0026) N11 - C16 - Distance Angles C15 1.3773 (0.0027) C11 1.4011 (0.0028) 120.54 (0.18) C16 - C15 FMAP and GRID set by program FMAP 2 2 13 GRID -2.500 -2 -2 2.500 2 2 R1 = 0.0430 for 2697 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.25 at 0.1312 0.2400 0.1461 [ 0.82 A from C22 ] Deepest hole -0.33 at 0.2569 0.2291 0.4395 [ 0.74 A from S11 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 2396 / 17696 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.8688 -0.2400 0.8539 1.00000 0.05 0.25 0.82 C22 0.85 C21 1.32 H22B 1.38 H22A Q2 1 0.9040 0.2866 0.8976 1.00000 0.05 0.25 0.59 C17 0.72 N13 1.77 N12 1.81 C18 Q3 1 0.5797 -0.1858 0.8759 1.00000 0.05 0.23 0.83 H25B 1.37 C25 1.53 C24 1.64 H21N Q4 1 0.8039 0.2554 1.0986 1.00000 0.05 0.22 0.60 C14 0.79 C13 1.51 H13 1.76 C15 Q5 1 0.7088 0.3504 0.9376 1.00000 0.05 0.21 0.80 O12 1.21 S11 1.89 C14 2.02 H22 Q6 1 0.7603 0.3481 1.0886 1.00000 0.05 0.20 0.65 C14 0.83 C15 1.59 H15 1.72 C13 Q7 1 0.5032 -0.2588 0.8726 1.00000 0.05 0.20 0.52 H25B 1.11 C25 1.48 H25A 1.82 H25C Q8 1 0.6534 0.1534 0.9544 1.00000 0.05 0.20 0.47 O11 1.00 S11 2.04 O12 2.11 N12 Q9 1 1.0593 0.2159 0.8556 1.00000 0.05 0.19 0.69 C19 1.05 S12 1.31 H19 1.76 C18 Q10 1 0.7703 -0.2575 0.8760 1.00000 0.05 0.19 1.16 N21 1.19 C24 1.20 N22 1.21 C21 Q11 1 0.8744 0.3186 1.2392 1.00000 0.05 0.18 0.61 C12 0.81 C11 1.40 H12 1.69 C13 Q12 1 0.6587 0.3053 0.8849 1.00000 0.05 0.17 0.39 O12 1.21 S11 2.13 O11 2.28 N12 Q13 1 1.0185 0.3172 0.8362 1.00000 0.05 0.17 0.81 C19 0.92 C18 1.61 H19 1.69 N13 Q14 1 0.7770 0.1787 0.9123 1.00000 0.05 0.17 0.46 N12 1.11 S11 1.62 C17 2.08 O11 Q15 1 0.9804 0.3721 0.9119 1.00000 0.05 0.17 0.73 N13 0.74 C18 1.38 H18 1.71 C17 Q16 1 0.7647 0.2836 1.0278 1.00000 0.05 0.16 0.58 C14 1.28 S11 1.72 C13 1.75 C15 Q17 1 0.6547 0.3836 0.8784 1.00000 0.05 0.16 0.40 O12 1.79 H22 1.83 S11 2.39 H21A Q18 1 1.0364 0.5236 0.8534 1.00000 0.05 0.16 0.69 H18 1.38 C18 2.13 H22B 2.31 N13 Q19 1 0.8344 0.0569 0.8822 1.00000 0.05 0.16 1.05 N12 1.80 C17 1.89 H21B 2.03 H21A Q20 1 0.8057 0.3983 1.2403 1.00000 0.05 0.16 0.63 C11 0.78 C16 1.54 H16 1.73 C12 Shortest distances between peaks (including symmetry equivalents) 12 17 0.76 5 12 0.94 5 17 0.97 4 16 1.00 4 6 1.03 6 16 1.03 9 13 1.10 11 20 1.14 3 7 1.16 2 15 1.23 1 10 1.30 13 15 1.31 5 16 1.41 14 19 1.46 8 14 1.73 8 12 1.74 2 13 1.78 15 18 1.85 12 14 1.86 14 16 1.87 2 14 1.91 5 14 1.91 8 16 1.95 5 6 1.98 4 11 1.99 13 18 2.00 9 15 2.01 5 8 2.04 6 20 2.04 12 16 2.08 2 9 2.19 6 11 2.21 4 20 2.33 2 19 2.36 11 18 2.36 16 17 2.36 4 5 2.40 3 10 2.42 8 17 2.43 14 17 2.45 4 14 2.55 4 8 2.56 18 20 2.61 2 5 2.61 2 16 2.67 6 8 2.73 6 18 2.73 8 19 2.74 6 12 2.78 3 13 2.84 7 13 2.84 6 17 2.86 4 18 2.86 11 16 2.88 6 14 2.90 2 18 2.92 1 19 2.92 2 12 2.96 9 18 2.97 16 20 2.99 7 9 2.99 Time profile in seconds ----------------------- 0.22: 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. 1.54: 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 1.72: Structure factors and derivatives 2.12: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.09: Apply other restraints 0.22: Solve l.s. equations 0.00: Generate HTAB table 0.13: Other dependent quantities, CIF, tables 0.55: Analysis of variance 0.27: Merge reflections for Fourier and .fcf 0.09: Fourier summations 0.45: Peaksearch 0.05: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 12:41:31 Total elapsed time: 7.5 secs + 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