+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008src0227 started at 14:46:30 on 25-Apr-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src0227 in P2(1)/c CELL 0.71073 15.8475 15.8514 6.9724 90.000 98.498 90.000 ZERR 4.00 0.0014 0.0014 0.0004 0.000 0.006 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H S UNIT 88 48 12 V = 1732.27 F(000) = 768.0 Mu = 0.43 mm-1 Cell Wt = 1489.98 Rho = 1.428 MERG 2 OMIT -3.00 55.00 OMIT -1 0 2 OMIT 2 6 6 OMIT -6 7 6 OMIT -3 1 6 OMIT 0 8 3 OMIT 5 4 6 OMIT -3 13 6 OMIT -1 12 1 OMIT -2 14 4 OMIT 6 4 3 EXTI 0.01274 FMAP 2 PLAN 10 SIZE 0.01 0.02 0.45 ACTA BOND WGHT 0.09950 11.80930 L.S. 4 TEMP -153.00 FVAR 0.36047 C1 1 0.201176 0.321655 0.168971 11.00000 0.02610 0.01625 = 0.01800 0.00570 0.00140 0.00242 C2 1 0.233543 0.240519 0.181430 11.00000 0.02973 0.01291 = 0.01480 0.00476 0.00647 -0.00243 C3 1 0.323667 0.238045 0.202264 11.00000 0.02582 0.01441 = 0.02173 -0.00237 0.00550 0.00028 C4 1 0.358318 0.318522 0.210251 11.00000 0.03034 0.01479 = 0.01984 0.00052 0.00285 -0.00012 C5 1 0.453608 0.318050 0.233978 11.00000 0.02636 0.02090 = 0.02388 -0.00209 0.00540 -0.00641 AFIX 23 H5A 2 0.478986 0.346505 0.355291 11.00000 -1.20000 H5B 2 0.474997 0.344943 0.122372 11.00000 -1.20000 AFIX 0 C6 1 0.471293 0.223532 0.241674 11.00000 0.02597 0.03229 = 0.01671 0.00070 0.00070 0.00149 C7 1 0.548962 0.181291 0.265290 11.00000 0.02869 0.03722 = 0.02201 -0.00237 0.00145 0.00129 AFIX 43 H7 2 0.601148 0.211715 0.278471 11.00000 -1.20000 AFIX 0 C8 1 0.548764 0.093405 0.269249 11.00000 0.03417 0.03720 = 0.03185 0.00152 0.00453 0.01880 AFIX 43 H8 2 0.601415 0.063716 0.286141 11.00000 -1.20000 AFIX 0 C9 1 0.471452 0.047927 0.248516 11.00000 0.04299 0.02588 = 0.03882 -0.00020 0.00815 0.00823 AFIX 43 H9 2 0.472716 -0.011990 0.249942 11.00000 -1.20000 AFIX 0 C10 1 0.393646 0.089482 0.226086 11.00000 0.03323 0.02377 = 0.02351 -0.00185 0.00268 0.00716 AFIX 43 H10 2 0.341661 0.058763 0.214182 11.00000 -1.20000 AFIX 0 C11 1 0.393469 0.177670 0.221393 11.00000 0.02664 0.02251 = 0.01546 0.00237 0.00277 0.00208 C12 1 0.110851 0.324237 0.145046 11.00000 0.02719 0.01391 = 0.01808 0.00423 0.00560 0.00454 C13 1 0.076279 0.243883 0.137782 11.00000 0.02928 0.01215 = 0.01771 0.00673 0.00395 0.00277 C14 1 -0.014910 0.245138 0.107371 11.00000 0.02752 0.02287 = 0.00973 0.00080 0.00097 -0.00031 C15 1 -0.045585 0.326019 0.098083 11.00000 0.02895 0.01942 = 0.01901 0.00120 0.00147 0.00027 C16 1 -0.142286 0.329118 0.065326 11.00000 0.03131 0.02325 = 0.02200 0.00243 0.00364 0.00185 AFIX 23 H16A 2 -0.164712 0.356920 -0.058928 11.00000 -1.20000 H16B 2 -0.164806 0.358089 0.172914 11.00000 -1.20000 AFIX 0 C17 1 -0.162520 0.235323 0.060933 11.00000 0.02987 0.01848 = 0.01763 0.00114 0.00691 0.00304 C18 1 -0.241840 0.197330 0.037832 11.00000 0.02179 0.03502 = 0.02498 0.00018 0.00863 -0.00201 AFIX 43 H18 2 -0.292507 0.230171 0.025004 11.00000 -1.20000 AFIX 0 C19 1 -0.245492 0.108676 0.033834 11.00000 0.02891 0.03463 = 0.02958 -0.00467 0.00730 -0.00347 AFIX 43 H19 2 -0.299402 0.081287 0.014704 11.00000 -1.20000 AFIX 0 C20 1 -0.171168 0.060458 0.057531 11.00000 0.03771 0.02179 = 0.02344 0.00079 0.00662 -0.00321 AFIX 43 H20 2 -0.174987 0.000647 0.057185 11.00000 -1.20000 AFIX 0 C21 1 -0.090900 0.099233 0.081852 11.00000 0.03184 0.01935 = 0.02825 0.00072 0.01093 0.00342 AFIX 43 H21 2 -0.040235 0.066346 0.097064 11.00000 -1.20000 AFIX 0 C22 1 -0.086863 0.187271 0.083286 11.00000 0.02845 0.02309 = 0.01700 0.00530 0.00774 0.00330 S1 3 0.281894 0.397342 0.187542 11.00000 0.02924 0.01505 = 0.02960 -0.00037 0.00470 -0.00181 S2 3 0.153083 0.164670 0.159920 11.00000 0.02572 0.01526 = 0.02095 -0.00005 0.00463 0.00122 S3 3 0.033169 0.402115 0.119528 11.00000 0.02920 0.01490 = 0.02644 0.00135 0.00368 0.00214 HKLF 4 1.0 0.00 0.00 1.00 0.00 -1.00 0.00 1.00 0.00 0.00 Covalent radii and connectivity table for 2008src0227 in P2(1)/c C 0.770 H 0.320 S 1.030 C1 - C2 C12 S1 C2 - C1 C3 S2 C3 - C4 C2 C11 C4 - C3 C5 S1 C5 - C4 C6 C6 - C7 C11 C5 C7 - C6 C8 C8 - C7 C9 C9 - C10 C8 C10 - C9 C11 C11 - C10 C6 C3 C12 - C13 C1 S3 C13 - C12 C14 S2 C14 - C15 C13 C22 C15 - C14 C16 S3 C16 - C15 C17 C17 - C18 C22 C16 C18 - C17 C19 C19 - C20 C18 C20 - C19 C21 C21 - C22 C20 C22 - C21 C17 C14 S1 - C4 C1 S2 - C13 C2 S3 - C15 C12 h k l Fo^2 Sigma Why rejected 5 0 5 24.62 5.44 observed but should be systematically absent 20148 Reflections read, of which 440 rejected -20 =< h =< 20, -20 =< k =< 20, -8 =< l =< 9, Max. 2-theta = 54.98 1 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 6 14 1 0.13 0.20 5 2.01 2 10 2 35.24 3.25 7 16.34 2 Inconsistent equivalents 3940 Unique reflections, of which 0 suppressed R(int) = 0.1068 R(sigma) = 0.1097 Friedel opposites merged Maximum memory for data reduction = 1950 / 39369 Default effective X-H distances for T = -153.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 1.00 0.99 0.98 0.95 0.88 0.91 1.12 0.84 0.95 0.88 0.95 Note that these distances are chosen to give the best fit to the X-ray data and so avoid the introduction of systematic error. The true internuclear distances are longer and do not vary with temperature ! The apparent variation with temperature is caused by libration. Least-squares cycle 1 Maximum vector length = 511 Memory required = 2519 / 280299 wR2 = 0.2819 before cycle 1 for 3940 data and 227 / 227 parameters GooF = S = 1.104; Restrained GooF = 1.104 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0995 * P )^2 + 11.81 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36047 0.00221 0.001 OSF 2 0.01273 0.00355 -0.004 EXTI Mean shift/esd = 0.002 Maximum = -0.012 for U12 S3 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C18 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2519 / 280299 wR2 = 0.2819 before cycle 2 for 3940 data and 227 / 227 parameters GooF = S = 1.104; Restrained GooF = 1.104 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0995 * P )^2 + 11.81 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36047 0.00220 -0.001 OSF 2 0.01272 0.00355 -0.003 EXTI Mean shift/esd = 0.001 Maximum = -0.005 for U33 C19 Max. shift = 0.000 A for C13 Max. dU = 0.000 for C18 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2519 / 280299 wR2 = 0.2819 before cycle 3 for 3940 data and 227 / 227 parameters GooF = S = 1.104; Restrained GooF = 1.104 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0995 * P )^2 + 11.81 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36047 0.00220 -0.002 OSF 2 0.01271 0.00355 -0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for OSF Max. shift = 0.000 A for C13 Max. dU = 0.000 for C19 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2519 / 280299 wR2 = 0.2819 before cycle 4 for 3940 data and 227 / 227 parameters GooF = S = 1.104; Restrained GooF = 1.104 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0995 * P )^2 + 11.81 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.36047 0.00220 0.000 OSF 2 0.01271 0.00355 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z C15 Max. shift = 0.000 A for C15 Max. dU = 0.000 for C20 Largest correlation matrix elements 0.578 EXTI / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H5A 0.4790 0.3465 0.3553 23 0.990 0.000 C5 C4 C6 H5B 0.4750 0.3449 0.1224 23 0.990 0.000 C5 C4 C6 H7 0.6011 0.2117 0.2785 43 0.950 0.000 C7 C6 C8 H8 0.6014 0.0637 0.2861 43 0.950 0.000 C8 C7 C9 H9 0.4727 -0.0120 0.2499 43 0.950 0.000 C9 C10 C8 H10 0.3417 0.0588 0.2142 43 0.950 0.000 C10 C9 C11 H16A -0.1647 0.3569 -0.0589 23 0.990 0.000 C16 C15 C17 H16B -0.1648 0.3581 0.1729 23 0.990 0.000 C16 C15 C17 H18 -0.2925 0.2302 0.0250 43 0.950 0.000 C18 C17 C19 H19 -0.2994 0.0813 0.0147 43 0.950 0.000 C19 C20 C18 H20 -0.1750 0.0006 0.0572 43 0.950 0.000 C20 C19 C21 H21 -0.0402 0.0663 0.0971 43 0.950 0.000 C21 C22 C20 2008src0227 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.20118 0.32165 0.16897 1.00000 0.02609 0.01627 0.01801 0.00570 0.00140 0.00244 0.02031 0.01119 0.00040 0.00036 0.00085 0.00000 0.00329 0.00280 0.00297 0.00223 0.00233 0.00245 0.00124 C2 0.23355 0.24052 0.18144 1.00000 0.02974 0.01293 0.01480 0.00477 0.00646 -0.00242 0.01884 0.01097 0.00040 0.00035 0.00081 0.00000 0.00328 0.00265 0.00282 0.00206 0.00233 0.00237 0.00122 C3 0.32367 0.23804 0.20226 1.00000 0.02580 0.01441 0.02173 -0.00239 0.00548 0.00027 0.02045 0.01105 0.00040 0.00036 0.00086 0.00000 0.00318 0.00271 0.00309 0.00220 0.00238 0.00240 0.00125 C4 0.35832 0.31852 0.21025 1.00000 0.03035 0.01479 0.01981 0.00051 0.00283 -0.00011 0.02174 0.01125 0.00041 0.00036 0.00087 0.00000 0.00343 0.00278 0.00303 0.00225 0.00244 0.00249 0.00129 C5 0.45361 0.31805 0.23398 1.00000 0.02635 0.02090 0.02388 -0.00209 0.00539 -0.00641 0.02354 0.01141 0.00041 0.00038 0.00093 0.00000 0.00331 0.00303 0.00325 0.00239 0.00249 0.00258 0.00133 H5A 0.47899 0.34650 0.35529 1.00000 0.02825 0.00000 0.00000 H5B 0.47500 0.34494 0.12237 1.00000 0.02825 0.00000 0.00000 C6 0.47129 0.22353 0.24167 1.00000 0.02596 0.03229 0.01673 0.00069 0.00070 0.00149 0.02524 0.01169 0.00041 0.00042 0.00087 0.00000 0.00336 0.00343 0.00297 0.00255 0.00240 0.00280 0.00136 C7 0.54896 0.18129 0.26529 1.00000 0.02870 0.03720 0.02204 -0.00237 0.00147 0.00129 0.02954 0.01269 0.00045 0.00044 0.00093 0.00000 0.00360 0.00390 0.00336 0.00272 0.00261 0.00298 0.00151 H7 0.60115 0.21172 0.27846 1.00000 0.03545 0.00000 0.00000 C8 0.54877 0.09340 0.26925 1.00000 0.03417 0.03717 0.03190 0.00150 0.00455 0.01880 0.03445 0.01418 0.00047 0.00047 0.00102 0.00000 0.00401 0.00391 0.00388 0.00295 0.00298 0.00331 0.00168 H8 0.60142 0.06371 0.28614 1.00000 0.04134 0.00000 0.00000 C9 0.47145 0.04793 0.24852 1.00000 0.04299 0.02587 0.03886 -0.00021 0.00816 0.00822 0.03569 0.01425 0.00050 0.00045 0.00106 0.00000 0.00451 0.00355 0.00417 0.00299 0.00335 0.00319 0.00170 H9 0.47271 -0.01199 0.24995 1.00000 0.04283 0.00000 0.00000 C10 0.39365 0.08948 0.22608 1.00000 0.03324 0.02376 0.02352 -0.00184 0.00270 0.00717 0.02699 0.01264 0.00046 0.00041 0.00091 0.00000 0.00359 0.00323 0.00341 0.00251 0.00263 0.00279 0.00142 H10 0.34166 0.05876 0.21417 1.00000 0.03239 0.00000 0.00000 C11 0.39347 0.17767 0.22139 1.00000 0.02664 0.02252 0.01545 0.00237 0.00274 0.00207 0.02157 0.01143 0.00041 0.00038 0.00084 0.00000 0.00325 0.00307 0.00293 0.00227 0.00232 0.00253 0.00127 C12 0.11085 0.32424 0.14505 1.00000 0.02721 0.01390 0.01808 0.00422 0.00560 0.00453 0.01950 0.01135 0.00040 0.00035 0.00084 0.00000 0.00327 0.00269 0.00297 0.00215 0.00235 0.00241 0.00123 C13 0.07628 0.24389 0.13779 1.00000 0.02929 0.01215 0.01772 0.00673 0.00396 0.00277 0.01967 0.01130 0.00040 0.00036 0.00083 0.00000 0.00333 0.00264 0.00298 0.00209 0.00239 0.00236 0.00125 C14 -0.01491 0.24514 0.10737 1.00000 0.02752 0.02287 0.00972 0.00077 0.00096 -0.00033 0.02022 0.01069 0.00039 0.00038 0.00079 0.00000 0.00328 0.00297 0.00275 0.00218 0.00225 0.00253 0.00125 C15 -0.04558 0.32602 0.09808 1.00000 0.02895 0.01942 0.01901 0.00118 0.00148 0.00028 0.02267 0.01130 0.00041 0.00038 0.00087 0.00000 0.00340 0.00301 0.00306 0.00229 0.00245 0.00256 0.00131 C16 -0.14229 0.32912 0.06532 1.00000 0.03132 0.02323 0.02201 0.00245 0.00365 0.00185 0.02555 0.01197 0.00042 0.00039 0.00093 0.00000 0.00358 0.00317 0.00323 0.00245 0.00256 0.00273 0.00137 H16A -0.16471 0.35692 -0.05893 1.00000 0.03066 0.00000 0.00000 H16B -0.16481 0.35809 0.17291 1.00000 0.03066 0.00000 0.00000 C17 -0.16252 0.23532 0.06093 1.00000 0.02987 0.01849 0.01763 0.00112 0.00692 0.00304 0.02165 0.01125 0.00041 0.00037 0.00083 0.00000 0.00335 0.00295 0.00310 0.00225 0.00247 0.00256 0.00130 C18 -0.24184 0.19733 0.03783 1.00000 0.02176 0.03501 0.02496 0.00017 0.00862 -0.00201 0.02672 0.01211 0.00042 0.00043 0.00092 0.00000 0.00325 0.00367 0.00341 0.00269 0.00254 0.00277 0.00143 H18 -0.29251 0.23017 0.02500 1.00000 0.03207 0.00000 0.00000 C19 -0.24549 0.10868 0.03383 1.00000 0.02893 0.03464 0.02952 -0.00466 0.00730 -0.00343 0.03073 0.01284 0.00046 0.00044 0.00099 0.00000 0.00360 0.00377 0.00369 0.00287 0.00282 0.00296 0.00152 H19 -0.29940 0.08129 0.01470 1.00000 0.03688 0.00000 0.00000 C20 -0.17117 0.06045 0.05753 1.00000 0.03770 0.02178 0.02345 0.00079 0.00663 -0.00322 0.02743 0.01224 0.00045 0.00041 0.00091 0.00000 0.00385 0.00314 0.00338 0.00250 0.00275 0.00283 0.00144 H20 -0.17499 0.00064 0.05719 1.00000 0.03292 0.00000 0.00000 C21 -0.09090 0.09923 0.08185 1.00000 0.03184 0.01935 0.02827 0.00072 0.01093 0.00341 0.02583 0.01233 0.00044 0.00038 0.00093 0.00000 0.00356 0.00302 0.00349 0.00252 0.00275 0.00271 0.00140 H21 -0.04023 0.06635 0.09706 1.00000 0.03100 0.00000 0.00000 C22 -0.08686 0.18727 0.08329 1.00000 0.02842 0.02310 0.01703 0.00530 0.00776 0.00329 0.02241 0.01193 0.00041 0.00039 0.00085 0.00000 0.00342 0.00304 0.00302 0.00233 0.00243 0.00258 0.00131 S1 0.28189 0.39734 0.18754 1.00000 0.02924 0.01505 0.02960 -0.00037 0.00470 -0.00181 0.02459 0.00292 0.00011 0.00009 0.00023 0.00000 0.00090 0.00075 0.00092 0.00059 0.00067 0.00062 0.00044 S2 0.15308 0.16467 0.15992 1.00000 0.02572 0.01526 0.02095 -0.00005 0.00463 0.00122 0.02053 0.00284 0.00010 0.00009 0.00022 0.00000 0.00079 0.00069 0.00076 0.00057 0.00055 0.00061 0.00040 S3 0.03317 0.40211 0.11953 1.00000 0.02920 0.01490 0.02644 0.00134 0.00367 0.00213 0.02356 0.00293 0.00010 0.00009 0.00023 0.00000 0.00088 0.00073 0.00087 0.00057 0.00064 0.00061 0.00043 Final Structure Factor Calculation for 2008src0227 in P2(1)/c Total number of l.s. parameters = 227 Maximum vector length = 511 Memory required = 2292 / 21973 wR2 = 0.2819 before cycle 5 for 3940 data and 0 / 227 parameters GooF = S = 1.104; Restrained GooF = 1.104 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0995 * P )^2 + 11.81 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1079 for 2605 Fo > 4sig(Fo) and 0.1583 for all 3940 data wR2 = 0.2819, GooF = S = 1.104, Restrained GooF = 1.104 for all data Occupancy sum of asymmetric unit = 25.00 for non-hydrogen and 12.00 for hydrogen atoms Principal mean square atomic displacements U 0.0269 0.0229 0.0111 C1 0.0302 0.0186 0.0077 C2 0.0264 0.0214 0.0136 C3 0.0306 0.0199 0.0147 C4 0.0311 0.0229 0.0167 C5 0.0326 0.0267 0.0164 C6 0.0380 0.0293 0.0214 C7 0.0546 0.0319 0.0168 C8 0.0465 0.0383 0.0223 C9 0.0379 0.0237 0.0193 C10 0.0275 0.0225 0.0147 C11 0.0292 0.0183 0.0110 C12 0.0298 0.0216 0.0076 C13 0.0281 0.0229 0.0097 C14 0.0297 0.0204 0.0179 C15 0.0318 0.0248 0.0201 C16 0.0311 0.0177 0.0161 C17 0.0353 0.0280 0.0169 C18 0.0388 0.0278 0.0256 C19 0.0384 0.0236 0.0203 C20 0.0365 0.0229 0.0182 C21 0.0319 0.0223 0.0131 C22 0.0299 0.0291 0.0148 S1 0.0260 0.0205 0.0151 S2 0.0296 0.0266 0.0145 S3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.007 0.014 0.021 0.028 0.036 0.046 0.060 0.080 0.121 1.000 Number in group 418. 415. 412. 371. 375. 386. 379. 394. 397. 393. GooF 1.243 1.225 1.213 1.046 1.004 1.013 0.912 1.053 1.238 0.996 K 30.378 4.579 3.173 1.658 1.192 1.096 1.038 1.043 1.033 1.045 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.31 1.66 inf Number in group 406. 389. 389. 398. 389. 393. 401. 387. 397. 391. GooF 0.966 0.921 0.954 1.017 1.020 1.163 1.307 1.081 1.127 1.387 K 0.988 1.068 1.102 1.076 1.279 1.070 1.087 1.018 1.055 1.086 R1 0.238 0.276 0.228 0.192 0.210 0.144 0.135 0.088 0.118 0.094 Recommended weighting scheme: WGHT 0.0995 11.8103 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) 2 1 3 567.83 116.40 6.45 0.038 2.10 -10 8 3 1532.03 583.23 6.10 0.085 1.14 2 8 6 303.17 18.45 6.09 0.015 0.97 1 7 6 1155.53 392.60 6.06 0.070 1.01 11 1 3 2026.04 840.36 6.00 0.103 1.14 -1 1 1 884.83 3144.13 5.92 0.198 6.16 3 12 3 500.02 105.65 5.84 0.036 1.10 -11 4 6 282.64 13.90 5.80 0.013 0.94 -10 4 3 855.94 270.13 5.66 0.058 1.32 -3 4 3 287.76 31.20 5.64 0.020 1.94 3 2 3 1876.09 830.17 5.60 0.102 1.94 0 4 3 358.72 72.37 5.39 0.030 1.99 -13 2 3 2331.05 1101.30 5.34 0.117 1.13 -6 6 3 190.59 0.41 5.32 0.002 1.53 11 3 3 1854.01 862.73 5.02 0.104 1.11 0 2 3 1216.95 550.35 4.85 0.083 2.21 -6 2 3 842.25 341.48 4.77 0.065 1.82 5 0 6 293.51 56.39 4.74 0.027 1.03 -6 11 6 410.28 68.26 4.56 0.029 0.88 0 12 3 216.45 23.09 4.54 0.017 1.15 -6 5 6 241.14 40.96 4.53 0.023 1.05 8 9 3 627.26 222.17 4.52 0.053 1.09 -8 9 3 180.27 12.40 4.31 0.012 1.19 6 8 3 1593.48 837.41 4.28 0.102 1.25 2 4 3 181.95 29.28 4.14 0.019 1.87 5 9 3 166.45 16.92 4.07 0.015 1.24 2 5 3 128.94 7.81 4.06 0.010 1.76 3 6 3 938.72 466.88 3.99 0.076 1.59 1 3 3 736.05 339.22 3.98 0.065 2.05 -5 1 3 1194.96 631.11 3.93 0.089 1.98 -5 5 3 1564.90 881.72 3.89 0.105 1.69 4 11 1 246.78 7.40 3.89 0.010 1.31 10 3 6 187.37 5.97 3.79 0.009 0.86 -2 13 1 165.68 0.04 3.77 0.001 1.19 -11 2 6 133.62 1.15 3.65 0.004 0.96 5 13 3 135.05 1.38 3.64 0.004 1.00 5 5 3 197.72 47.76 3.60 0.024 1.52 -8 5 3 766.34 388.34 3.57 0.070 1.44 0 13 1 799.87 417.01 3.47 0.072 1.20 -2 11 3 783.44 410.34 3.46 0.072 1.22 -8 7 3 205.85 54.11 3.38 0.026 1.31 10 1 6 162.35 0.11 3.33 0.001 0.87 7 1 6 114.23 14.02 3.30 0.013 0.96 -13 14 3 235.69 19.85 3.20 0.016 0.80 -8 10 6 206.41 32.71 3.18 0.020 0.88 -10 10 3 390.44 169.98 3.15 0.046 1.05 11 15 3 1339.45 745.63 3.13 0.097 0.77 -6 3 6 240.34 86.15 3.10 0.033 1.09 6 13 4 138.53 0.98 3.10 0.003 0.90 13 8 3 164.26 19.31 3.07 0.016 0.90 Bond lengths and angles C1 - Distance Angles C2 1.3826 (0.0078) C12 1.4170 (0.0084) 113.15 (0.53) S1 1.7446 (0.0062) 111.96 (0.46) 134.89 (0.46) C1 - C2 C12 C2 - Distance Angles C1 1.3826 (0.0078) C3 1.4146 (0.0088) 113.07 (0.52) S2 1.7428 (0.0060) 112.11 (0.46) 134.79 (0.45) C2 - C1 C3 C3 - Distance Angles C4 1.3868 (0.0081) C2 1.4146 (0.0088) 111.50 (0.52) C11 1.4539 (0.0084) 108.09 (0.55) 140.41 (0.55) C3 - C4 C2 C4 - Distance Angles C3 1.3868 (0.0081) C5 1.4947 (0.0089) 112.80 (0.52) S1 1.7310 (0.0063) 113.12 (0.48) 134.08 (0.45) C4 - C3 C5 C5 - Distance Angles C4 1.4947 (0.0089) C6 1.5237 (0.0089) 100.74 (0.48) C5 - C4 C6 - Distance Angles C7 1.3894 (0.0092) C11 1.4206 (0.0090) 120.40 (0.61) C5 1.5237 (0.0089) 129.28 (0.61) 110.32 (0.55) C6 - C7 C11 C7 - Distance Angles C6 1.3894 (0.0092) C8 1.3934 (0.0100) 118.66 (0.67) C7 - C6 C8 - Distance Angles C7 1.3934 (0.0100) C9 1.4105 (0.0108) 120.89 (0.65) C8 - C7 C9 - Distance Angles C10 1.3862 (0.0098) C8 1.4105 (0.0108) 120.89 (0.65) C9 - C10 C10 - Distance Angles C9 1.3862 (0.0098) C11 1.3983 (0.0086) 118.45 (0.68) C10 - C9 C11 - Distance Angles C10 1.3983 (0.0086) C6 1.4206 (0.0090) 120.70 (0.61) C3 1.4539 (0.0084) 131.23 (0.62) 108.05 (0.54) C11 - C10 C6 C12 - Distance Angles C13 1.3845 (0.0079) C1 1.4170 (0.0084) 111.41 (0.51) S3 1.7339 (0.0059) 112.34 (0.46) 136.24 (0.47) C12 - C13 C1 C13 - Distance Angles C12 1.3845 (0.0079) C14 1.4294 (0.0087) 112.24 (0.51) S2 1.7396 (0.0060) 113.14 (0.46) 134.58 (0.46) C13 - C12 C14 C14 - Distance Angles C15 1.3693 (0.0084) C13 1.4294 (0.0087) 111.35 (0.53) C22 1.4537 (0.0087) 108.57 (0.55) 140.08 (0.55) C14 - C15 C13 C15 - Distance Angles C14 1.3693 (0.0084) C16 1.5165 (0.0090) 112.41 (0.54) S3 1.7262 (0.0064) 113.77 (0.49) 133.79 (0.47) C15 - C14 C16 C16 - Distance Angles C15 1.5165 (0.0090) C17 1.5203 (0.0083) 100.18 (0.50) C16 - C15 C17 - Distance Angles C18 1.3817 (0.0089) C22 1.4095 (0.0086) 121.45 (0.58) C16 1.5203 (0.0083) 127.89 (0.59) 110.66 (0.56) C17 - C18 C22 C18 - Distance Angles C17 1.3817 (0.0089) C19 1.4066 (0.0095) 118.16 (0.63) C18 - C17 C19 - Distance Angles C20 1.3933 (0.0098) C18 1.4066 (0.0095) 120.94 (0.66) C19 - C20 C20 - Distance Angles C19 1.3933 (0.0098) C21 1.4004 (0.0095) 120.69 (0.61) C20 - C19 C21 - Distance Angles C22 1.3970 (0.0086) C20 1.4004 (0.0095) 118.63 (0.62) C21 - C22 C22 - Distance Angles C21 1.3970 (0.0086) C17 1.4095 (0.0086) 120.12 (0.61) C14 1.4537 (0.0087) 131.72 (0.60) 108.16 (0.53) C22 - C21 C17 S1 - Distance Angles C4 1.7310 (0.0063) C1 1.7446 (0.0062) 90.34 (0.29) S1 - C4 S2 - Distance Angles C13 1.7396 (0.0060) C2 1.7428 (0.0060) 90.18 (0.28) S2 - C13 S3 - Distance Angles C15 1.7262 (0.0064) C12 1.7339 (0.0059) 90.27 (0.30) S3 - C15 FMAP and GRID set by program FMAP 2 3 11 GRID -3.125 -2 -2 3.125 2 2 R1 = 0.1577 for 3940 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.39 at 0.9675 0.5997 0.2528 [ 1.53 A from H21 ] Deepest hole -0.86 at 0.6563 0.1013 0.0862 [ 0.97 A from H19 ] Mean = 0.00, Rms deviation from mean = 0.15 e/A^3, Highest memory used = 2795 / 23080 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0325 0.0997 0.2472 1.00000 0.05 1.39 1.53 H21 2.12 C21 2.33 S2 2.48 C22 Q2 1 0.0347 0.0972 -0.0639 1.00000 0.05 1.16 1.82 H21 2.20 S3 2.36 C21 2.50 S2 Q3 1 0.2795 0.1002 0.3330 1.00000 0.05 1.10 1.53 H10 2.06 C10 2.41 C11 2.41 S2 Q4 1 0.1540 0.3365 0.3082 1.00000 0.05 1.08 1.25 C12 1.33 C1 2.16 C13 2.24 C2 Q5 1 0.2800 0.1017 0.0224 1.00000 0.05 0.99 1.68 H10 2.13 C10 2.33 H20 2.34 S1 Q6 1 0.1528 0.3364 -0.0134 1.00000 0.05 0.97 1.38 C12 1.40 C1 2.26 C13 2.28 S2 Q7 1 0.5427 0.3324 0.4612 1.00000 0.05 0.83 1.18 H5A 1.97 C5 2.12 C7 2.37 H7 Q8 1 0.5394 0.3329 0.1404 1.00000 0.05 0.81 1.03 H5B 1.61 C5 1.91 H5A 2.21 C6 Q9 1 0.6555 0.0984 0.2028 1.00000 0.05 0.67 1.23 H8 1.61 H19 1.82 C8 2.09 H7 Q10 1 -0.0986 0.4028 0.1842 1.00000 0.05 0.63 1.26 H16B 1.54 C16 1.64 C15 1.99 H16A Shortest distances between peaks (including symmetry equivalents) 3 5 2.17 1 2 2.17 7 8 2.23 4 6 2.24 2 4 2.44 4 5 2.51 7 9 2.52 2 10 2.54 1 6 2.55 3 6 2.61 7 8 2.91 Time profile in seconds ----------------------- 0.03: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.05: 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 0.02: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.02: Analyse other restraints etc. 3.52: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.05: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.83: Structure factors and derivatives 1.13: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.34: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.00: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008src0227 finished at 14:46:36 Total CPU time: 6.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++