+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 14:15:37 on 18-Dec-2000 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in C2/c CELL 0.71073 18.1753 8.1029 16.5347 90.000 91.079 90.000 ZERR 8.00 0.0036 0.0016 0.0033 0.000 0.030 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N O S UNIT 96 104 24 16 8 V = 2434.68 F(000) = 1104.0 Mu = 0.26 mm-1 Cell Wt = 2106.51 Rho = 1.437 MERG 2 FMAP 2 PLAN 20 ACTA BOND L.S. 10 WGHT 0.055500 1.766800 EXTI 0.001468 FVAR 0.29268 N13 3 0.536551 0.262982 0.942459 11.00000 0.02710 0.02534 = 0.02916 0.00118 -0.00235 0.00136 C18 1 0.601072 0.346430 0.952433 11.00000 0.02759 0.03451 = 0.03744 -0.00271 -0.00158 -0.00056 C21 1 0.480964 0.490092 0.874496 11.00000 0.03982 0.02509 = 0.02637 -0.00143 0.00011 0.00427 C20 1 0.545505 0.574019 0.886063 11.00000 0.04639 0.02494 = 0.03499 -0.00003 0.00710 -0.00142 C19 1 0.607115 0.502265 0.924955 11.00000 0.03293 0.03514 = 0.04353 -0.00540 0.00613 -0.00538 C22 1 0.415444 0.563075 0.831450 11.00000 0.05451 0.02716 = 0.04342 0.00598 -0.01183 0.00688 H15 2 0.437543 0.078493 0.739934 11.00000 0.03021 H16 2 0.381000 -0.013598 0.621369 11.00000 0.04361 H13 2 0.268098 -0.106057 0.866079 11.00000 0.03661 H17 2 0.531204 0.165455 0.964914 11.00000 0.04769 H20 2 0.549000 0.687549 0.867471 11.00000 0.04829 H18 2 0.639777 0.289060 0.980550 11.00000 0.03923 H19 2 0.651927 0.560252 0.931532 11.00000 0.04233 H12 2 0.208041 -0.192787 0.747713 11.00000 0.04989 H11 2 0.207458 -0.179058 0.601174 11.00000 0.04539 H22C 2 0.428846 0.672388 0.811265 11.00000 0.04932 H10 2 0.274443 -0.121710 0.557562 11.00000 0.04847 H22B 2 0.372583 0.566643 0.868795 11.00000 0.05811 H22A 2 0.402959 0.498202 0.787313 11.00000 0.05336 MOLE 1 S11 5 0.402563 0.048659 0.905353 11.00000 0.02510 0.02456 = 0.01836 0.00006 -0.00290 0.00239 O12 4 0.472539 -0.037873 0.911227 11.00000 0.02750 0.02468 = 0.02957 0.00016 -0.00881 0.00440 N11 3 0.255458 -0.160694 0.600114 11.00000 0.03281 0.05509 = 0.02523 -0.00254 -0.00285 -0.01607 C14 1 0.357016 -0.010582 0.815508 11.00000 0.02020 0.02289 = 0.01960 0.00099 -0.00138 0.00224 N12 3 0.412236 0.242355 0.893837 11.00000 0.02823 0.02370 = 0.03073 -0.00271 -0.00645 0.00458 O11 4 0.353155 0.014463 0.970694 11.00000 0.03854 0.04320 = 0.01947 0.00091 0.00288 -0.00133 C15 1 0.390896 0.016969 0.741990 11.00000 0.01937 0.03064 = 0.02325 0.00112 -0.00025 -0.00378 C16 1 0.356915 -0.033060 0.670814 11.00000 0.02310 0.03258 = 0.01942 0.00084 0.00256 -0.00127 C17 1 0.475867 0.324546 0.904027 11.00000 0.02872 0.02484 = 0.01956 -0.00350 -0.00020 0.00472 C12 1 0.255465 -0.139940 0.746183 11.00000 0.02391 0.03776 = 0.02889 0.00169 0.00081 -0.01022 C13 1 0.289632 -0.089801 0.817233 11.00000 0.02576 0.03155 = 0.02183 0.00343 0.00313 -0.00206 C11 1 0.288261 -0.110768 0.671447 11.00000 0.02485 0.02801 = 0.02313 -0.00140 -0.00255 -0.00294 HKLF 4 Covalent radii and connectivity table for s92 in C2/c C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 N13 - C17 C18 C18 - C19 N13 C21 - C20 C17 C22 C20 - C21 C19 C19 - C18 C20 C22 - C21 S11 - O11 O12 N12 C14 O12 - S11 N11 - C11 C14 - C13 C15 S11 N12 - C17 S11 O11 - S11 C15 - C16 C14 C16 - C15 C11 C17 - N12 N13 C21 C12 - C13 C11 C13 - C12 C14 C11 - N11 C16 C12 13369 Reflections read, of which 614 rejected -23 =< h =< 22, -10 =< k =< 10, -21 =< l =< 21, Max. 2-theta = 54.95 0 Systematic absence violations 0 Inconsistent equivalents 2764 Unique reflections, of which 0 suppressed R(int) = 0.0379 R(sigma) = 0.0328 Friedel opposites merged Maximum memory for data reduction = 1608 / 33087 Least-squares cycle 1 Maximum vector length = 511 Memory required = 2118 / 268637 wR2 = 0.1035 before cycle 1 for 2764 data and 216 / 216 parameters GooF = S = 1.053; Restrained GooF = 1.053 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0555 * P )^2 + 1.77 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.29268 0.00075 0.004 OSF 2 0.00147 0.00057 0.000 EXTI Mean shift/esd = 0.003 Maximum = 0.022 for U13 S11 Max. shift = 0.000 A for H22B Max. dU = 0.000 for H17 Largest correlation matrix elements 0.584 U33 S11 / OSF 0.564 U11 S11 / OSF 0.562 U22 S11 / OSF s92 in C2/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq N13 0.53655 0.26298 0.94246 1.00000 0.02710 0.02534 0.02916 0.00118 -0.00235 0.00136 0.02724 0.00230 0.00007 0.00018 0.00008 0.00000 0.00069 0.00071 0.00071 0.00056 0.00054 0.00056 0.00031 C18 0.60107 0.34643 0.95243 1.00000 0.02759 0.03451 0.03744 -0.00271 -0.00158 -0.00056 0.03321 0.00298 0.00009 0.00022 0.00011 0.00000 0.00083 0.00092 0.00092 0.00072 0.00069 0.00071 0.00038 C21 0.48096 0.49009 0.87450 1.00000 0.03982 0.02509 0.02637 -0.00143 0.00011 0.00427 0.03043 0.00293 0.00010 0.00021 0.00010 0.00000 0.00094 0.00080 0.00081 0.00063 0.00068 0.00070 0.00037 C20 0.54550 0.57402 0.88606 1.00000 0.04639 0.02494 0.03499 -0.00003 0.00710 -0.00142 0.03536 0.00321 0.00011 0.00022 0.00011 0.00000 0.00105 0.00085 0.00093 0.00070 0.00076 0.00075 0.00040 C19 0.60711 0.50226 0.92496 1.00000 0.03293 0.03514 0.04353 -0.00540 0.00613 -0.00538 0.03713 0.00328 0.00010 0.00023 0.00012 0.00000 0.00094 0.00093 0.00106 0.00080 0.00078 0.00078 0.00042 C22 0.41544 0.56307 0.83145 1.00000 0.05451 0.02716 0.04342 0.00598 -0.01183 0.00688 0.04185 0.00379 0.00013 0.00024 0.00014 0.00000 0.00123 0.00092 0.00110 0.00082 0.00095 0.00085 0.00047 H15 0.43754 0.07850 0.73994 1.00000 0.03021 0.03285 0.00104 0.00237 0.00112 0.00000 0.00461 H16 0.38100 -0.01360 0.62137 1.00000 0.04363 0.03699 0.00112 0.00266 0.00136 0.00000 0.00569 H13 0.26810 -0.10605 0.86608 1.00000 0.03661 0.03419 0.00109 0.00251 0.00126 0.00000 0.00510 H17 0.53120 0.16545 0.96492 1.00000 0.04771 0.03904 0.00117 0.00313 0.00138 0.00000 0.00606 H20 0.54900 0.68755 0.86747 1.00000 0.04829 0.03824 0.00115 0.00298 0.00130 0.00000 0.00584 H18 0.63978 0.28907 0.98054 1.00000 0.03923 0.03450 0.00111 0.00261 0.00120 0.00000 0.00518 H19 0.65193 0.56026 0.93154 1.00000 0.04234 0.03867 0.00119 0.00264 0.00130 0.00000 0.00553 H12 0.20804 -0.19279 0.74771 1.00000 0.04989 0.03942 0.00123 0.00287 0.00132 0.00000 0.00595 H11 0.20746 -0.17904 0.60118 1.00000 0.04540 0.04051 0.00133 0.00284 0.00131 0.00000 0.00580 H22C 0.42884 0.67238 0.81126 1.00000 0.04933 0.03944 0.00118 0.00311 0.00135 0.00000 0.00596 H10 0.27444 -0.12172 0.55756 1.00000 0.04846 0.03899 0.00126 0.00291 0.00149 0.00000 0.00631 H22B 0.37259 0.56666 0.86879 1.00000 0.05812 0.04323 0.00138 0.00314 0.00156 0.00000 0.00703 H22A 0.40296 0.49820 0.78731 1.00000 0.05335 0.04506 0.00125 0.00310 0.00151 0.00000 0.00653 S11 0.40256 0.04866 0.90535 1.00000 0.02510 0.02456 0.01836 0.00006 -0.00290 0.00239 0.02272 0.00061 0.00002 0.00005 0.00002 0.00000 0.00023 0.00023 0.00021 0.00013 0.00014 0.00014 0.00015 O12 0.47254 -0.03787 0.91123 1.00000 0.02750 0.02468 0.02957 0.00016 -0.00881 0.00440 0.02737 0.00185 0.00006 0.00013 0.00007 0.00000 0.00058 0.00056 0.00060 0.00043 0.00045 0.00044 0.00027 N11 0.25546 -0.16069 0.60011 1.00000 0.03281 0.05509 0.02523 -0.00254 -0.00285 -0.01607 0.03775 0.00255 0.00009 0.00022 0.00009 0.00000 0.00084 0.00103 0.00076 0.00068 0.00062 0.00073 0.00038 C14 0.35702 -0.01058 0.81551 1.00000 0.02020 0.02289 0.01960 0.00099 -0.00138 0.00224 0.02092 0.00252 0.00008 0.00019 0.00009 0.00000 0.00070 0.00072 0.00069 0.00055 0.00055 0.00057 0.00031 N12 0.41224 0.24235 0.89384 1.00000 0.02823 0.02370 0.03073 -0.00271 -0.00645 0.00458 0.02764 0.00221 0.00007 0.00017 0.00008 0.00000 0.00069 0.00069 0.00071 0.00053 0.00054 0.00054 0.00031 O11 0.35316 0.01446 0.97069 1.00000 0.03854 0.04320 0.01947 0.00091 0.00288 -0.00133 0.03370 0.00207 0.00007 0.00016 0.00007 0.00000 0.00068 0.00071 0.00057 0.00048 0.00048 0.00056 0.00030 C15 0.39090 0.01697 0.74199 1.00000 0.01937 0.03064 0.02325 0.00112 -0.00025 -0.00378 0.02443 0.00266 0.00008 0.00020 0.00009 0.00000 0.00071 0.00082 0.00075 0.00061 0.00057 0.00062 0.00033 C16 0.35692 -0.03306 0.67081 1.00000 0.02310 0.03258 0.01942 0.00084 0.00256 -0.00127 0.02501 0.00271 0.00008 0.00020 0.00009 0.00000 0.00074 0.00084 0.00074 0.00061 0.00058 0.00063 0.00034 C17 0.47587 0.32455 0.90403 1.00000 0.02872 0.02484 0.01956 -0.00350 -0.00020 0.00472 0.02438 0.00260 0.00008 0.00019 0.00009 0.00000 0.00077 0.00076 0.00069 0.00057 0.00057 0.00062 0.00033 C12 0.25546 -0.13994 0.74618 1.00000 0.02391 0.03776 0.02889 0.00169 0.00081 -0.01022 0.03018 0.00289 0.00009 0.00022 0.00010 0.00000 0.00078 0.00093 0.00082 0.00067 0.00061 0.00069 0.00037 C13 0.28963 -0.08980 0.81723 1.00000 0.02576 0.03155 0.02183 0.00343 0.00313 -0.00206 0.02635 0.00280 0.00009 0.00021 0.00010 0.00000 0.00078 0.00083 0.00075 0.00063 0.00059 0.00065 0.00034 C11 0.28826 -0.11077 0.67145 1.00000 0.02485 0.02801 0.02313 -0.00140 -0.00255 -0.00294 0.02537 0.00258 0.00008 0.00020 0.00009 0.00000 0.00075 0.00078 0.00074 0.00061 0.00058 0.00063 0.00033 Final Structure Factor Calculation for s92 in C2/c Total number of l.s. parameters = 216 Maximum vector length = 511 Memory required = 1902 / 24017 wR2 = 0.1035 before cycle 2 for 2764 data and 0 / 216 parameters GooF = S = 1.053; Restrained GooF = 1.053 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0555 * P )^2 + 1.77 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0374 for 2341 Fo > 4sig(Fo) and 0.0471 for all 2764 data wR2 = 0.1035, GooF = S = 1.053, Restrained GooF = 1.053 for all data Occupancy sum of asymmetric unit = 18.00 for non-hydrogen and 13.00 for hydrogen atoms Principal mean square atomic displacements U 0.0313 0.0270 0.0235 N13 0.0393 0.0333 0.0270 C18 0.0410 0.0269 0.0234 C21 0.0492 0.0321 0.0248 C20 0.0493 0.0337 0.0285 C19 0.0633 0.0407 0.0215 C22 0.0280 0.0232 0.0169 S11 0.0387 0.0258 0.0176 O12 0.0635 0.0290 0.0207 N11 0.0242 0.0213 0.0173 C14 0.0385 0.0239 0.0205 N12 0.0436 0.0385 0.0191 O11 0.0320 0.0231 0.0182 C15 0.0328 0.0240 0.0183 C16 0.0324 0.0232 0.0175 C17 0.0433 0.0289 0.0184 C12 0.0329 0.0271 0.0191 C13 0.0298 0.0264 0.0199 C11 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.016 0.030 0.045 0.060 0.078 0.097 0.122 0.161 0.226 1.000 Number in group 295. 266. 269. 277. 279. 275. 275. 277. 274. 277. GooF 0.937 1.088 1.110 1.157 1.103 0.963 1.070 0.996 1.031 1.060 K 1.165 0.900 0.940 0.955 0.967 0.973 0.996 1.013 1.030 1.016 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.64 inf Number in group 283. 280. 268. 274. 277. 277. 274. 276. 277. 278. GooF 1.001 0.974 0.861 0.933 0.942 0.952 1.018 0.960 1.078 1.608 K 0.985 0.985 1.013 1.034 1.036 1.024 1.046 1.033 1.019 0.995 R1 0.113 0.101 0.062 0.059 0.049 0.040 0.038 0.030 0.029 0.033 Recommended weighting scheme: WGHT 0.0566 1.6983 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) -4 2 4 32.39 0.56 6.13 0.003 2.46 6 2 4 474.65 276.76 6.08 0.074 2.08 8 2 2 235.34 116.63 5.99 0.048 1.92 0 2 6 90.17 39.32 4.61 0.028 2.28 4 2 2 1500.77 2057.80 4.51 0.202 2.83 6 2 0 910.03 643.95 4.25 0.113 2.43 -6 0 8 3811.69 2826.50 4.24 0.237 1.72 11 1 12 32.88 86.57 4.11 0.041 1.04 -6 4 1 111.19 192.83 3.96 0.062 1.68 11 1 0 1353.35 1024.80 3.92 0.143 1.62 -7 7 14 52.88 177.59 3.90 0.059 0.79 7 3 1 1058.70 795.22 3.90 0.126 1.86 -21 1 9 114.46 5.09 3.82 0.010 0.78 -1 1 6 48.73 98.24 3.72 0.044 2.59 8 0 14 91.23 158.31 3.34 0.056 1.04 9 3 1 701.36 541.18 3.21 0.104 1.61 -4 0 8 1248.80 1574.28 3.21 0.177 1.89 -8 6 14 324.17 455.59 3.07 0.095 0.83 12 4 2 254.83 349.69 3.06 0.083 1.20 2 0 2 523.11 672.93 3.03 0.116 6.06 5 3 2 202.41 282.08 3.02 0.075 2.09 3 1 6 4207.13 3513.14 2.99 0.264 2.38 -2 2 2 1626.13 1991.86 2.96 0.199 3.39 5 1 20 1705.55 1308.11 2.96 0.161 0.80 -9 3 1 97.27 51.08 2.95 0.032 1.61 -2 2 3 468.00 364.30 2.87 0.085 3.08 -6 2 8 15.26 39.91 2.87 0.028 1.58 -9 1 12 606.97 772.52 2.86 0.124 1.14 -11 5 1 703.84 895.89 2.86 0.133 1.16 -6 2 19 -14.34 30.49 2.85 0.025 0.82 20 4 7 434.50 639.84 2.83 0.113 0.78 13 3 0 213.67 149.05 2.82 0.054 1.24 9 3 10 -3.35 15.24 2.72 0.017 1.15 -6 0 2 389.50 298.59 2.71 0.077 2.86 8 0 2 1997.33 2403.57 2.70 0.219 2.18 7 3 4 771.07 952.66 2.70 0.138 1.70 15 3 0 371.53 484.49 2.70 0.098 1.11 -10 0 2 62.66 102.88 2.69 0.045 1.78 0 6 0 842.19 661.49 2.69 0.115 1.35 9 1 2 153.80 107.99 2.68 0.046 1.90 2 8 1 243.37 179.41 2.67 0.060 1.00 8 0 8 293.12 383.27 2.67 0.087 1.51 -12 0 18 2081.31 1566.72 2.66 0.176 0.79 -2 0 8 2522.81 3008.29 2.65 0.245 2.02 7 1 0 1016.43 837.85 2.62 0.129 2.47 9 1 4 75.97 116.07 2.62 0.048 1.76 8 0 18 2519.83 2014.65 2.61 0.200 0.85 7 1 13 4.04 22.07 2.60 0.021 1.12 -7 1 13 97.18 145.39 2.58 0.054 1.14 -18 2 9 -5.15 29.17 2.54 0.024 0.87 Bond lengths and angles N13 - Distance Angles C17 1.3575 (0.0020) C18 1.3610 (0.0022) 124.39 (0.15) N13 - C17 C18 - Distance Angles C19 1.3471 (0.0027) N13 1.3610 (0.0022) 120.02 (0.17) C18 - C19 C21 - Distance Angles C20 1.3662 (0.0026) C17 1.4311 (0.0023) 118.67 (0.15) C22 1.4975 (0.0026) 122.89 (0.17) 118.44 (0.16) C21 - C20 C17 C20 - Distance Angles C21 1.3662 (0.0026) C19 1.4066 (0.0028) 122.16 (0.16) C20 - C21 C19 - Distance Angles C18 1.3471 (0.0027) C20 1.4066 (0.0028) 118.19 (0.17) C19 - C18 C22 - Distance Angles C21 1.4975 (0.0026) C22 - S11 - Distance Angles O11 1.4446 (0.0013) O12 1.4540 (0.0011) 114.38 (0.07) N12 1.5911 (0.0014) 110.51 (0.08) 112.66 (0.07) C14 1.7539 (0.0015) 106.91 (0.07) 108.84 (0.07) 102.71 (0.07) S11 - O11 O12 N12 O12 - Distance Angles S11 1.4540 (0.0011) O12 - N11 - Distance Angles C11 1.3725 (0.0021) N11 - C14 - Distance Angles C13 1.3835 (0.0022) C15 1.3910 (0.0022) 119.94 (0.14) S11 1.7539 (0.0015) 120.89 (0.12) 119.12 (0.11) C14 - C13 C15 N12 - Distance Angles C17 1.3424 (0.0021) S11 1.5911 (0.0014) 124.83 (0.11) N12 - C17 O11 - Distance Angles S11 1.4446 (0.0013) O11 - C15 - Distance Angles C16 1.3796 (0.0022) C14 1.3910 (0.0022) 119.99 (0.14) C15 - C16 C16 - Distance Angles C15 1.3796 (0.0022) C11 1.3979 (0.0022) 120.75 (0.15) C16 - C15 C17 - Distance Angles N12 1.3424 (0.0021) N13 1.3575 (0.0020) 124.53 (0.14) C21 1.4311 (0.0023) 118.90 (0.14) 116.55 (0.14) C17 - N12 N13 C12 - Distance Angles C13 1.3796 (0.0023) C11 1.4021 (0.0023) 120.59 (0.15) C12 - C13 C13 - Distance Angles C12 1.3796 (0.0023) C14 1.3835 (0.0022) 120.23 (0.15) C13 - C12 C11 - Distance Angles N11 1.3725 (0.0021) C16 1.3979 (0.0022) 119.98 (0.15) C12 1.4021 (0.0023) 121.51 (0.15) 118.48 (0.14) C11 - N11 C16 FMAP and GRID set by program FMAP 2 2 12 GRID -2.778 -2 -1 2.778 2 1 R1 = 0.0467 for 2764 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.26 at 0.4037 0.1415 0.4057 [ 1.51 A from O12 ] Deepest hole -0.40 at 0.3694 0.0903 0.9005 [ 0.69 A from S11 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 2653 / 27336 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4037 -0.1415 0.9057 1.00000 0.05 0.26 1.51 O12 1.54 S11 1.91 O11 2.01 C14 Q2 1 0.3739 -0.0047 0.8411 1.00000 0.05 0.25 0.52 C14 1.25 S11 1.68 C15 1.72 C13 Q3 1 0.4739 0.1399 0.8996 1.00000 0.05 0.24 1.40 N12 1.45 O12 1.50 S11 1.50 C17 Q4 1 0.4779 0.4134 0.8809 1.00000 0.05 0.23 0.63 C21 0.82 C17 1.79 C20 1.84 C22 Q5 1 0.3352 -0.0535 0.8173 1.00000 0.05 0.22 0.53 C14 0.88 C13 1.53 H13 1.72 C15 Q6 1 0.2379 -0.0551 0.6007 1.00000 0.05 0.21 0.91 N11 1.12 H10 1.15 H11 1.54 C11 Q7 1 0.3515 0.1111 0.9690 1.00000 0.05 0.21 0.78 O11 1.50 S11 1.99 N12 2.05 H10 Q8 1 0.2749 -0.1317 0.7238 1.00000 0.05 0.18 0.52 C12 0.92 C11 1.38 H12 1.60 C13 Q9 1 0.6100 0.4083 0.9190 1.00000 0.05 0.18 0.77 C18 0.77 C19 1.46 H19 1.50 H18 Q10 1 0.5186 0.5014 0.8649 1.00000 0.05 0.18 0.71 C21 0.84 C20 1.61 H20 1.76 C17 Q11 1 0.4384 0.2529 0.8814 1.00000 0.05 0.18 0.53 N12 0.96 C17 1.83 S11 2.03 N13 Q12 1 0.2539 0.0565 0.7452 1.00000 0.05 0.17 1.59 C12 1.79 C13 1.93 C11 2.15 H12 Q13 1 0.3371 -0.0402 0.9033 1.00000 0.05 0.17 1.23 O11 1.39 S11 1.49 H13 1.52 C14 Q14 1 0.4838 0.0860 1.0178 1.00000 0.05 0.17 1.40 H17 1.46 O12 2.03 O12 2.08 H17 Q15 1 0.2763 -0.1736 0.8810 1.00000 0.05 0.17 0.62 H13 1.28 C13 2.26 C14 2.27 C12 Q16 1 0.3737 0.0090 0.7835 1.00000 0.05 0.15 0.63 C14 0.76 C15 1.49 H15 1.82 C13 Q17 1 0.3682 -0.0146 0.7023 1.00000 0.05 0.15 0.58 C16 0.81 C15 1.36 H16 1.59 H15 Q18 1 0.5837 0.5252 0.9050 1.00000 0.05 0.15 0.57 C19 0.85 C20 1.34 H19 1.58 H20 Q19 1 0.4178 -0.1057 0.9567 1.00000 0.05 0.14 1.37 O12 1.53 S11 1.55 O11 1.65 H17 Q20 1 0.4915 0.5317 0.9033 1.00000 0.05 0.14 0.61 C21 1.08 C20 1.70 C17 1.75 H20 Shortest distances between peaks (including symmetry equivalents) 10 20 0.85 2 5 0.89 1 19 0.92 2 16 0.96 5 16 1.04 4 20 1.05 4 10 1.06 9 18 1.08 3 11 1.16 2 13 1.27 10 18 1.36 16 17 1.36 5 13 1.43 1 13 1.46 4 11 1.49 13 15 1.58 8 12 1.61 1 2 1.63 14 14 1.63 7 13 1.66 18 20 1.68 13 19 1.78 5 15 1.80 14 19 1.84 8 17 1.98 5 8 1.98 3 14 2.01 9 10 2.02 5 17 2.03 1 5 2.03 5 12 2.08 13 16 2.14 7 19 2.14 4 18 2.16 14 19 2.20 2 19 2.21 6 8 2.22 3 4 2.24 12 17 2.28 12 16 2.29 2 17 2.30 8 16 2.33 2 15 2.34 2 3 2.36 2 7 2.36 1 15 2.36 9 20 2.38 3 14 2.40 1 16 2.41 1 14 2.43 3 19 2.43 7 11 2.45 4 9 2.47 2 11 2.48 11 20 2.48 1 7 2.49 10 11 2.50 7 14 2.53 3 7 2.53 6 12 2.56 1 3 2.62 8 15 2.62 8 12 2.63 2 12 2.72 11 14 2.74 5 19 2.76 11 16 2.80 2 8 2.81 3 16 2.83 15 16 2.83 5 7 2.85 3 13 2.89 15 19 2.89 6 17 2.90 12 15 2.94 1 14 2.97 Time profile in seconds ----------------------- 0.17: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.05: 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. 1.77: 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 1.32: Structure factors and derivatives 1.52: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.11: Apply other restraints 0.11: Solve l.s. equations 0.00: Generate HTAB table 0.16: Other dependent quantities, CIF, tables 0.83: Analysis of variance 0.28: Merge reflections for Fourier and .fcf 0.41: Fourier summations 0.52: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 14:15:44 Total elapsed time: 7.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++