+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 09:33:58 on 02-Oct-2002 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 02esp301 in P2(1)/c CELL 0.71073 5.4079 16.6855 16.5870 90.000 89.040 90.000 ZERR 4.00 0.0009 0.0029 0.0026 0.000 0.000 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O S UNIT 72 60 4 8 4 V = 1496.49 F(000) = 648.0 Mu = 0.22 mm-1 Cell Wt = 1237.48 Rho = 1.373 MERG 2 TWIN 1.00 0.00 0.00 0.00 -1.00 0.00 0.00 0.00 -1.00 2 BASF 0.18778 SHEL 7 0.84 FMAP 2 PLAN 20 SIZE 0.10 0.20 0.20 ACTA WGHT 0.14540 2.12460 L.S. 4 TEMP -153.00 FVAR 0.40264 MOLE 1 S1 5 0.013116 0.115430 0.143292 11.00000 0.04867 0.02096 = 0.02123 -0.00038 -0.00266 0.00548 N1 3 0.078324 0.100119 0.299551 11.00000 0.04489 0.01781 = 0.02262 -0.00126 -0.00711 0.00541 O1 4 -0.366793 0.219446 0.131606 11.00000 0.06287 0.02556 = 0.01736 0.00224 -0.00013 -0.00013 O2 4 0.385717 0.005057 0.308800 11.00000 0.05999 0.02998 = 0.03300 -0.00495 -0.01743 0.01264 C1 1 -0.554652 0.303144 0.232313 11.00000 0.04951 0.02007 = 0.02621 0.00038 -0.00698 0.00206 AFIX 137 H1A 2 -0.527122 0.351291 0.199537 11.00000 -1.50000 H1B 2 -0.523708 0.315489 0.289019 11.00000 -1.50000 H1C 2 -0.725968 0.285131 0.226651 11.00000 -1.50000 AFIX 0 C2 1 -0.379763 0.237308 0.203999 11.00000 0.03799 0.01418 = 0.02881 0.00168 0.00055 -0.00459 C3 1 -0.238574 0.195570 0.264754 11.00000 0.04611 0.02223 = 0.01711 0.00109 -0.00263 -0.00321 AFIX 43 H3 2 -0.269225 0.206685 0.320198 11.00000 -1.20000 AFIX 0 C4 1 -0.064950 0.141377 0.243631 11.00000 0.04858 0.01343 = 0.02290 -0.00108 -0.00672 -0.00369 C5 1 0.047052 0.109859 0.386368 11.00000 0.04682 0.01851 = 0.01930 0.00097 -0.00564 0.00528 C6 1 0.220613 0.153015 0.428782 11.00000 0.04636 0.02140 = 0.03151 0.00340 -0.00353 -0.00049 AFIX 43 H6 2 0.358331 0.176423 0.401377 11.00000 -1.20000 AFIX 0 C7 1 0.191679 0.161955 0.512633 11.00000 0.05867 0.02475 = 0.02705 -0.00253 -0.01266 0.00141 AFIX 43 H7 2 0.311145 0.190933 0.542211 11.00000 -1.20000 AFIX 0 C8 1 -0.012916 0.128211 0.552565 11.00000 0.05027 0.02823 = 0.02703 0.00210 -0.00622 0.01111 AFIX 43 H8 2 -0.033998 0.134810 0.609151 11.00000 -1.20000 AFIX 0 C9 1 -0.185133 0.085013 0.509140 11.00000 0.04709 0.03127 = 0.03242 0.01011 -0.00252 0.01036 AFIX 43 H9 2 -0.323057 0.061442 0.536286 11.00000 -1.20000 AFIX 0 C10 1 -0.156551 0.075955 0.425210 11.00000 0.04844 0.02511 = 0.03383 0.00301 -0.01096 0.00588 AFIX 43 H10 2 -0.275429 0.046924 0.395434 11.00000 -1.20000 AFIX 0 C11 1 0.258020 0.048125 0.266824 11.00000 0.03929 0.01506 = 0.03252 -0.00116 -0.00798 -0.00981 C12 1 0.269693 0.051613 0.175797 11.00000 0.04334 0.01916 = 0.02569 -0.00223 -0.00433 -0.00303 AFIX 13 H12 2 0.427887 0.078676 0.159630 11.00000 -1.20000 AFIX 0 C13 1 0.264155 -0.029515 0.134857 11.00000 0.04527 0.02028 = 0.02144 0.00071 -0.00783 0.00295 C14 1 0.456322 -0.052711 0.082733 11.00000 0.04284 0.01807 = 0.02232 0.00291 0.00266 -0.00483 AFIX 43 H14 2 0.596430 -0.018995 0.075342 11.00000 -1.20000 AFIX 0 C15 1 0.442696 -0.125835 0.041221 11.00000 0.05922 0.02359 = 0.02069 -0.00178 -0.00219 0.01053 AFIX 43 H15 2 0.571811 -0.141540 0.005031 11.00000 -1.20000 AFIX 0 C16 1 0.237851 -0.175082 0.053682 11.00000 0.05909 0.01732 = 0.02337 -0.00284 -0.01049 0.00578 AFIX 43 H16 2 0.226209 -0.224358 0.025305 11.00000 -1.20000 AFIX 0 C17 1 0.050993 -0.152758 0.107131 11.00000 0.04972 0.01856 = 0.03403 0.00197 -0.00588 -0.00521 AFIX 43 H17 2 -0.086308 -0.187390 0.115839 11.00000 -1.20000 AFIX 0 C18 1 0.061881 -0.080051 0.148342 11.00000 0.04565 0.02470 = 0.02796 -0.00305 -0.00041 0.00311 AFIX 43 H18 2 -0.066592 -0.065096 0.185099 11.00000 -1.20000 AFIX 0 HKLF 4 1.0 -1.00 0.00 0.00 0.00 0.00 1.00 0.00 1.00 0.00 Covalent radii and connectivity table for 02esp301 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 S1 - C4 C12 N1 - C4 C11 C5 O1 - C2 O2 - C11 C1 - C2 C2 - O1 C3 C1 C3 - C4 C2 C4 - C3 N1 S1 C5 - C6 C10 N1 C6 - C5 C7 C7 - C8 C6 C8 - C9 C7 C9 - C8 C10 C10 - C5 C9 C11 - O2 N1 C12 C12 - C11 C13 S1 C13 - C14 C18 C12 C14 - C13 C15 C15 - C16 C14 C16 - C17 C15 C17 - C16 C18 C18 - C17 C13 4160 Reflections read, of which 525 rejected -3 =< h =< 6, -19 =< k =< 18, -16 =< l =< 19, Max. 2-theta = 50.04 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -1 3 2 899.51 27.69 4 211.04 -1 3 3 513.12 10.69 3 248.55 -2 8 4 100.63 4.70 3 28.45 -1 9 4 23.94 0.92 2 15.89 -3 6 6 3.04 1.05 2 7.38 -2 3 11 7.16 1.04 2 5.66 -2 4 11 30.62 3.37 2 22.88 7 Inconsistent equivalents 2272 Unique reflections, of which 0 suppressed R(int) = 0.0624 R(sigma) = 0.1064 Friedel opposites merged Maximum memory for data reduction = 1859 / 23780 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 = 2414 / 250142 wR2 = 0.2486 before cycle 1 for 2272 data and 201 / 201 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1454 * P )^2 + 2.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40330 0.00245 0.270 OSF 2 0.18963 0.00430 0.430 BASF 1 Mean shift/esd = 0.042 Maximum = 0.430 for BASF 1 Max. shift = 0.003 A for H1C Max. dU = 0.000 for C7 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2414 / 250142 wR2 = 0.2483 before cycle 2 for 2272 data and 201 / 201 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1454 * P )^2 + 2.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40339 0.00245 0.038 OSF 2 0.19035 0.00430 0.168 BASF 1 Mean shift/esd = 0.018 Maximum = 0.168 for BASF 1 Max. shift = 0.002 A for H1C Max. dU = 0.000 for N1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2414 / 250142 wR2 = 0.2482 before cycle 3 for 2272 data and 201 / 201 parameters GooF = S = 1.031; Restrained GooF = 1.031 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1454 * P )^2 + 2.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40340 0.00245 0.003 OSF 2 0.19043 0.00430 0.018 BASF 1 Mean shift/esd = 0.004 Maximum = -0.020 for U23 C8 Max. shift = 0.001 A for H1A Max. dU = 0.000 for N1 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2414 / 250142 wR2 = 0.2482 before cycle 4 for 2272 data and 201 / 201 parameters GooF = S = 1.031; Restrained GooF = 1.031 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1454 * P )^2 + 2.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40340 0.00245 0.001 OSF 2 0.19046 0.00430 0.005 BASF 1 Mean shift/esd = 0.001 Maximum = -0.006 for y C13 Max. shift = 0.000 A for H1A Max. dU = 0.000 for C1 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A -0.5278 0.3512 0.1994 137 0.980 0.000 C1 C2 H1A H1B -0.5231 0.3157 0.2890 137 0.980 0.000 C1 C2 H1A H1C -0.7260 0.2850 0.2270 137 0.980 0.000 C1 C2 H1A H3 -0.2694 0.2066 0.3202 43 0.950 0.000 C3 C4 C2 H6 0.3585 0.1764 0.4013 43 0.950 0.000 C6 C5 C7 H7 0.3109 0.1910 0.5423 43 0.950 0.000 C7 C8 C6 H8 -0.0342 0.1348 0.6091 43 0.950 0.000 C8 C9 C7 H9 -0.3230 0.0615 0.5364 43 0.950 0.000 C9 C8 C10 H10 -0.2756 0.0469 0.3954 43 0.950 0.000 C10 C5 C9 H12 0.4280 0.0787 0.1596 13 1.000 0.000 C12 C11 C13 S1 H14 0.5964 -0.0190 0.0753 43 0.950 0.000 C14 C13 C15 H15 0.5719 -0.1416 0.0050 43 0.950 0.000 C15 C16 C14 H16 0.2262 -0.2244 0.0253 43 0.950 0.000 C16 C17 C15 H17 -0.0863 -0.1874 0.1159 43 0.950 0.000 C17 C16 C18 H18 -0.0664 -0.0651 0.1851 43 0.950 0.000 C18 C17 C13 02esp301 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq S1 0.01314 0.11543 0.14330 1.00000 0.04878 0.02099 0.02128 -0.00035 -0.00269 0.00541 0.03033 0.00268 0.00035 0.00008 0.00009 0.00000 0.00108 0.00075 0.00080 0.00058 0.00093 0.00073 0.00051 N1 0.07819 0.10011 0.29958 1.00000 0.04548 0.01821 0.02267 -0.00109 -0.00739 0.00538 0.02871 0.00873 0.00105 0.00028 0.00030 0.00000 0.00373 0.00233 0.00263 0.00200 0.00265 0.00239 0.00137 O1 -0.36681 0.21946 0.13165 1.00000 0.06303 0.02544 0.01753 0.00209 -0.00028 0.00049 0.03534 0.00734 0.00093 0.00024 0.00024 0.00000 0.00340 0.00213 0.00227 0.00177 0.00234 0.00221 0.00122 O2 0.38575 0.00506 0.30880 1.00000 0.05959 0.03002 0.03299 -0.00496 -0.01721 0.01279 0.04068 0.00793 0.00104 0.00026 0.00028 0.00000 0.00351 0.00225 0.00259 0.00198 0.00263 0.00240 0.00133 C1 -0.55466 0.30316 0.23234 1.00000 0.04926 0.02053 0.02636 0.00036 -0.00694 0.00210 0.03198 0.01096 0.00139 0.00034 0.00037 0.00000 0.00458 0.00290 0.00316 0.00247 0.00320 0.00299 0.00162 H1A -0.52778 0.35123 0.19939 1.00000 0.04797 0.00000 0.00000 H1B -0.52311 0.31569 0.28897 1.00000 0.04797 0.00000 0.00000 H1C -0.72596 0.28503 0.22695 1.00000 0.04797 0.00000 0.00000 C2 -0.37964 0.23730 0.20398 1.00000 0.03814 0.01423 0.02897 0.00183 0.00021 -0.00464 0.02712 0.01027 0.00126 0.00032 0.00038 0.00000 0.00389 0.00276 0.00363 0.00247 0.00308 0.00275 0.00149 C3 -0.23859 0.19555 0.26476 1.00000 0.04632 0.02201 0.01723 0.00097 -0.00260 -0.00329 0.02850 0.01046 0.00134 0.00034 0.00036 0.00000 0.00421 0.00292 0.00304 0.00241 0.00309 0.00291 0.00150 H3 -0.26938 0.20663 0.32020 1.00000 0.03420 0.00000 0.00000 C4 -0.06488 0.14137 0.24363 1.00000 0.04829 0.01339 0.02310 -0.00113 -0.00678 -0.00371 0.02819 0.00997 0.00131 0.00033 0.00035 0.00000 0.00435 0.00267 0.00307 0.00234 0.00312 0.00282 0.00155 C5 0.04705 0.10985 0.38639 1.00000 0.04653 0.01839 0.01932 0.00104 -0.00549 0.00566 0.02803 0.01059 0.00136 0.00032 0.00035 0.00000 0.00462 0.00278 0.00300 0.00233 0.00315 0.00299 0.00162 C6 0.22074 0.15300 0.42872 1.00000 0.04632 0.02183 0.03142 0.00314 -0.00341 -0.00030 0.03316 0.01120 0.00138 0.00036 0.00040 0.00000 0.00462 0.00303 0.00355 0.00270 0.00345 0.00303 0.00168 H6 0.35852 0.17635 0.40131 1.00000 0.03979 0.00000 0.00000 C7 0.19161 0.16199 0.51270 1.00000 0.05934 0.02501 0.02716 -0.00256 -0.01273 0.00148 0.03704 0.01179 0.00152 0.00038 0.00040 0.00000 0.00517 0.00327 0.00345 0.00271 0.00367 0.00346 0.00183 H7 0.31092 0.19100 0.54231 1.00000 0.04445 0.00000 0.00000 C8 -0.01303 0.12819 0.55253 1.00000 0.05037 0.02837 0.02669 0.00205 -0.00589 0.01154 0.03508 0.01163 0.00146 0.00034 0.00039 0.00000 0.00482 0.00318 0.00332 0.00257 0.00374 0.00350 0.00173 H8 -0.03417 0.13477 0.60911 1.00000 0.04210 0.00000 0.00000 C9 -0.18514 0.08502 0.50918 1.00000 0.04724 0.03102 0.03235 0.01031 -0.00245 0.00993 0.03685 0.01232 0.00143 0.00038 0.00041 0.00000 0.00457 0.00346 0.00378 0.00296 0.00342 0.00350 0.00174 H9 -0.32302 0.06147 0.53636 1.00000 0.04422 0.00000 0.00000 C10 -0.15674 0.07591 0.42520 1.00000 0.04846 0.02494 0.03386 0.00291 -0.01122 0.00595 0.03563 0.01166 0.00141 0.00036 0.00042 0.00000 0.00456 0.00322 0.00372 0.00286 0.00350 0.00338 0.00170 H10 -0.27563 0.04688 0.39543 1.00000 0.04276 0.00000 0.00000 C11 0.25780 0.04810 0.26681 1.00000 0.03906 0.01556 0.03236 -0.00116 -0.00791 -0.00956 0.02891 0.00991 0.00129 0.00033 0.00038 0.00000 0.00389 0.00267 0.00349 0.00260 0.00337 0.00283 0.00152 C12 0.26975 0.05164 0.17577 1.00000 0.04298 0.01919 0.02599 -0.00223 -0.00447 -0.00306 0.02934 0.01052 0.00141 0.00034 0.00037 0.00000 0.00405 0.00278 0.00321 0.00249 0.00314 0.00294 0.00152 H12 0.42797 0.07871 0.15963 1.00000 0.03521 0.00000 0.00000 C13 0.26416 -0.02955 0.13484 1.00000 0.04516 0.02047 0.02143 0.00067 -0.00795 0.00308 0.02894 0.01036 0.00132 0.00034 0.00037 0.00000 0.00421 0.00287 0.00313 0.00248 0.00337 0.00287 0.00156 C14 0.45631 -0.05269 0.08273 1.00000 0.04238 0.01830 0.02254 0.00301 0.00263 -0.00452 0.02778 0.01036 0.00131 0.00033 0.00035 0.00000 0.00425 0.00273 0.00306 0.00234 0.00318 0.00291 0.00152 H14 0.59637 -0.01895 0.07534 1.00000 0.03333 0.00000 0.00000 C15 0.44274 -0.12585 0.04121 1.00000 0.05940 0.02385 0.02060 -0.00139 -0.00210 0.00993 0.03460 0.01107 0.00149 0.00033 0.00037 0.00000 0.00505 0.00307 0.00310 0.00246 0.00345 0.00328 0.00175 H15 0.57188 -0.14156 0.00503 1.00000 0.04152 0.00000 0.00000 C16 0.23789 -0.17510 0.05367 1.00000 0.05902 0.01759 0.02339 -0.00263 -0.01049 0.00558 0.03323 0.01109 0.00143 0.00035 0.00037 0.00000 0.00510 0.00290 0.00336 0.00242 0.00354 0.00318 0.00179 H16 0.22624 -0.22437 0.02527 1.00000 0.03987 0.00000 0.00000 C17 0.05099 -0.15279 0.10716 1.00000 0.04951 0.01867 0.03428 0.00201 -0.00564 -0.00515 0.03410 0.01087 0.00141 0.00035 0.00039 0.00000 0.00483 0.00285 0.00352 0.00272 0.00366 0.00316 0.00173 H17 -0.08629 -0.18743 0.11590 1.00000 0.04092 0.00000 0.00000 C18 0.06201 -0.08009 0.14832 1.00000 0.04519 0.02458 0.02848 -0.00343 -0.00039 0.00325 0.03275 0.01052 0.00131 0.00035 0.00038 0.00000 0.00426 0.00318 0.00345 0.00265 0.00346 0.00302 0.00158 H18 -0.06643 -0.06512 0.18509 1.00000 0.03930 0.00000 0.00000 Final Structure Factor Calculation for 02esp301 in P2(1)/c Total number of l.s. parameters = 201 Maximum vector length = 511 Memory required = 2213 / 24017 wR2 = 0.2481 before cycle 5 for 2272 data and 0 / 201 parameters GooF = S = 1.031; Restrained GooF = 1.031 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1454 * P )^2 + 2.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0824 for 1672 Fo > 4sig(Fo) and 0.1122 for all 2272 data wR2 = 0.2481, GooF = S = 1.031, Restrained GooF = 1.031 for all data Occupancy sum of asymmetric unit = 22.00 for non-hydrogen and 15.00 for hydrogen atoms Principal mean square atomic displacements U 0.0499 0.0211 0.0200 S1 0.0482 0.0207 0.0172 N1 0.0630 0.0259 0.0170 O1 0.0716 0.0263 0.0241 O2 0.0509 0.0248 0.0202 C1 0.0390 0.0292 0.0131 C2 0.0469 0.0217 0.0169 C3 0.0499 0.0220 0.0126 C4 0.0483 0.0200 0.0158 C5 0.0468 0.0318 0.0209 C6 0.0633 0.0261 0.0217 C7 0.0558 0.0289 0.0205 C8 0.0525 0.0395 0.0186 C9 0.0543 0.0319 0.0206 C10 0.0456 0.0297 0.0115 C11 0.0440 0.0262 0.0178 C12 0.0474 0.0213 0.0181 C13 0.0436 0.0241 0.0157 C14 0.0620 0.0219 0.0199 C15 0.0622 0.0210 0.0165 C16 0.0518 0.0327 0.0178 C17 0.0457 0.0303 0.0222 C18 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.018 0.030 0.039 0.050 0.063 0.077 0.095 0.121 0.165 1.000 Number in group 227. 244. 213. 231. 240. 221. 213. 230. 224. 229. GooF 0.942 1.022 0.970 1.013 1.033 1.232 1.129 0.988 0.966 0.994 K 1.545 1.274 1.136 0.988 1.048 1.043 1.009 1.036 1.046 1.042 Resolution(A) 0.84 0.87 0.91 0.96 1.02 1.08 1.17 1.29 1.49 1.86 inf Number in group 231. 233. 223. 231. 217. 232. 223. 227. 226. 229. GooF 0.943 1.089 0.903 0.988 1.105 0.925 0.950 1.087 1.048 1.229 K 1.091 1.089 1.078 1.063 1.039 1.025 1.021 1.010 1.020 1.054 R1 0.209 0.199 0.171 0.133 0.128 0.091 0.085 0.090 0.076 0.074 Recommended weighting scheme: WGHT 0.1428 2.1372 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 10 4 -6.64 142.02 7.24 0.070 1.34 -5 3 3 12.68 199.06 5.04 0.083 1.04 -1 5 4 855.43 389.74 4.51 0.116 2.33 -1 4 3 4694.37 2334.22 4.43 0.284 2.82 -1 5 6 264.85 88.73 4.21 0.055 1.97 -1 5 2 2614.76 1272.54 4.10 0.209 2.68 -1 1 5 437.59 203.86 4.05 0.084 2.77 5 7 3 100.04 13.19 3.98 0.021 0.97 5 10 0 197.25 37.49 3.86 0.036 0.91 6 4 5 119.94 23.41 3.79 0.028 0.85 5 10 1 328.51 135.20 3.79 0.068 0.91 -1 9 2 1133.83 621.11 3.72 0.146 1.71 5 2 2 121.67 3.42 3.66 0.011 1.07 -1 4 9 473.72 182.55 3.66 0.079 1.60 -1 8 1 1068.00 576.51 3.65 0.141 1.93 -1 3 5 1505.80 809.06 3.62 0.167 2.51 5 2 4 52.48 0.21 3.60 0.003 1.04 5 1 4 339.14 149.06 3.59 0.072 1.05 3 7 5 6.15 53.92 3.55 0.043 1.33 4 1 1 30.85 167.05 3.54 0.076 1.34 -4 5 4 12.97 78.73 3.53 0.052 1.19 -1 2 2 1733.44 887.13 3.53 0.175 3.96 -1 5 1 870.84 497.74 3.44 0.131 2.79 5 11 3 107.78 2.81 3.34 0.010 0.87 1 7 1 1006.01 555.29 3.22 0.138 2.16 6 1 3 209.10 96.51 3.22 0.058 0.89 5 10 5 317.33 155.07 3.15 0.073 0.88 5 1 0 140.38 24.40 3.01 0.029 1.08 -1 7 6 324.03 173.44 3.01 0.077 1.71 6 2 6 95.01 16.77 2.99 0.024 0.86 1 2 1 5658.01 3352.02 2.98 0.340 4.39 -3 1 11 50.51 132.60 2.91 0.068 1.14 5 5 4 298.22 162.24 2.89 0.075 1.00 -1 6 6 854.52 534.28 2.86 0.136 1.84 1 3 2 4211.57 2686.99 2.84 0.304 3.53 5 7 4 504.01 297.84 2.82 0.101 0.96 -1 10 3 291.58 166.21 2.79 0.076 1.53 -1 6 7 303.13 175.64 2.79 0.078 1.70 6 1 2 383.86 226.06 2.77 0.088 0.90 3 3 4 72.85 153.55 2.73 0.073 1.59 5 2 6 172.06 58.67 2.73 0.045 1.01 -1 14 1 841.37 521.84 2.72 0.134 1.16 -5 1 4 0.00 40.52 2.69 0.037 1.04 4 6 8 52.29 118.06 2.67 0.064 1.06 -2 12 2 913.39 512.75 2.66 0.133 1.22 -1 2 6 3197.89 2143.14 2.62 0.272 2.35 -4 7 12 174.58 328.83 2.61 0.106 0.89 5 5 5 53.03 4.19 2.59 0.012 0.99 -1 1 6 98.55 55.78 2.58 0.044 2.42 -1 8 10 652.78 367.98 2.57 0.113 1.26 Bond lengths and angles S1 - Distance Angles C4 1.7640 (0.0062) C12 1.8367 (0.0070) 92.03 (0.30) S1 - C4 N1 - Distance Angles C4 1.3993 (0.0078) C11 1.4052 (0.0083) 115.70 (0.51) C5 1.4560 (0.0076) 123.02 (0.53) 121.29 (0.51) N1 - C4 C11 O1 - Distance Angles C2 1.2370 (0.0072) O1 - O2 - Distance Angles C11 1.2230 (0.0074) O2 - C1 - Distance Angles C2 1.5198 (0.0088) C1 - C2 - Distance Angles O1 1.2370 (0.0072) C3 1.4523 (0.0086) 122.42 (0.57) C1 1.5198 (0.0088) 119.92 (0.56) 117.62 (0.54) C2 - O1 C3 C3 - Distance Angles C4 1.3458 (0.0093) C2 1.4523 (0.0086) 120.92 (0.56) C3 - C4 C4 - Distance Angles C3 1.3458 (0.0093) N1 1.3993 (0.0078) 123.31 (0.55) S1 1.7640 (0.0062) 124.43 (0.47) 112.26 (0.47) C4 - C3 N1 C5 - Distance Angles C6 1.3840 (0.0092) C10 1.3878 (0.0099) 121.16 (0.58) N1 1.4560 (0.0076) 119.44 (0.63) 119.40 (0.58) C5 - C6 C10 C6 - Distance Angles C5 1.3840 (0.0092) C7 1.4072 (0.0091) 119.47 (0.68) C6 - C5 C7 - Distance Angles C8 1.3981 (0.0103) C6 1.4072 (0.0091) 119.96 (0.64) C7 - C8 C8 - Distance Angles C9 1.3873 (0.0098) C7 1.3981 (0.0103) 119.81 (0.62) C8 - C9 C9 - Distance Angles C8 1.3873 (0.0098) C10 1.4071 (0.0098) 120.41 (0.70) C9 - C8 C10 - Distance Angles C5 1.3878 (0.0100) C9 1.4071 (0.0098) 119.19 (0.64) C10 - C5 C11 - Distance Angles O2 1.2230 (0.0074) N1 1.4052 (0.0083) 122.43 (0.60) C12 1.5115 (0.0086) 125.23 (0.65) 112.34 (0.53) C11 - O2 N1 C12 - Distance Angles C11 1.5115 (0.0086) C13 1.5158 (0.0080) 114.30 (0.50) S1 1.8367 (0.0070) 107.20 (0.48) 111.45 (0.43) C12 - C11 C13 C13 - Distance Angles C14 1.3950 (0.0095) C18 1.3957 (0.0093) 120.36 (0.55) C12 1.5158 (0.0080) 120.31 (0.58) 119.32 (0.61) C13 - C14 C18 C14 - Distance Angles C13 1.3950 (0.0095) C15 1.4041 (0.0080) 120.00 (0.64) C14 - C13 C15 - Distance Angles C16 1.3920 (0.0098) C14 1.4041 (0.0080) 119.24 (0.66) C15 - C16 C16 - Distance Angles C17 1.3847 (0.0101) C15 1.3920 (0.0098) 120.46 (0.57) C16 - C17 C17 - Distance Angles C16 1.3847 (0.0101) C18 1.3939 (0.0086) 120.74 (0.66) C17 - C16 C18 - Distance Angles C17 1.3939 (0.0086) C13 1.3957 (0.0093) 119.16 (0.65) C18 - C17 FMAP and GRID set by program FMAP 2 1 14 GRID -4.545 24 -2 4.545 1 2 R1 = 0.0989 for 2272 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.60 at 0.1885 0.6126 0.3700 [ 1.12 A from S1 ] Deepest hole -0.44 at 0.4333 0.7220 0.8391 [ 1.03 A from C2 ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 2654 / 25366 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.1885 0.1126 0.1300 1.00000 0.05 0.60 1.12 S1 2.03 O1 2.07 C4 2.20 H12 Q2 1 0.2041 0.1078 0.1614 1.00000 0.05 0.58 1.03 C12 1.09 S1 1.30 H12 2.04 C11 Q3 1 0.5997 0.0041 0.3153 1.00000 0.05 0.38 1.16 O2 1.66 H10 2.16 C11 2.56 C10 Q4 1 -0.1434 -0.0885 0.1475 1.00000 0.05 0.34 0.85 H18 1.12 C18 1.64 C17 1.76 H17 Q5 1 0.1493 0.1429 0.2647 1.00000 0.05 0.33 0.99 N1 1.22 C4 1.69 C11 2.16 C5 Q6 1 -0.6904 0.3159 0.1795 1.00000 0.05 0.32 0.96 H1C 1.11 H1A 1.17 C1 2.04 H1B Q7 1 -0.5750 0.2212 0.1290 1.00000 0.05 0.30 1.13 O1 1.67 C2 2.10 H1C 2.15 H7 Q8 1 -0.1385 -0.1529 0.0922 1.00000 0.05 0.29 0.76 H17 1.06 C17 1.88 C18 2.16 C16 Q9 1 0.2899 -0.0432 0.3183 1.00000 0.05 0.28 0.97 O2 1.76 C11 2.20 H1A 2.37 H8 Q10 1 0.1348 -0.2217 -0.0657 1.00000 0.05 0.27 1.60 H16 1.65 O1 2.21 C16 2.34 S1 Q11 1 -0.1610 -0.1742 0.0634 1.00000 0.05 0.26 0.99 H17 1.41 C17 1.83 H15 2.16 C16 Q12 1 0.2387 -0.1720 0.1066 1.00000 0.05 0.26 0.88 C16 1.06 C17 1.61 H16 1.72 C15 Q13 1 -0.1681 0.2171 0.1485 1.00000 0.05 0.26 1.12 O1 1.49 C2 1.96 S1 1.99 C3 Q14 1 -0.0542 -0.1166 0.0333 1.00000 0.05 0.26 1.49 C17 1.82 H17 1.89 C16 2.11 C18 Q15 1 -0.3564 0.3132 0.2478 1.00000 0.05 0.25 1.12 C1 1.12 H1B 1.39 H1A 1.47 C2 Q16 1 0.0597 0.1605 0.4077 1.00000 0.05 0.25 0.92 C5 0.95 C6 1.64 H6 1.85 C10 Q17 1 0.0847 -0.1112 0.0836 1.00000 0.05 0.25 0.82 C17 1.20 C18 1.43 C16 1.66 H17 Q18 1 0.4525 0.1417 0.5423 1.00000 0.05 0.25 1.12 H7 1.54 C7 1.81 H9 2.24 C9 Q19 1 0.5183 0.0554 0.1533 1.00000 0.05 0.25 0.63 H12 1.39 C12 1.84 H14 2.00 C13 Q20 1 0.2888 0.0117 0.1395 1.00000 0.05 0.24 0.71 C13 0.90 C12 1.39 H12 1.68 C14 Shortest distances between peaks (including symmetry equivalents) 8 11 0.61 14 17 1.14 11 14 1.22 8 14 1.23 12 17 1.37 10 13 1.38 8 17 1.40 4 8 1.41 19 20 1.46 4 17 1.66 2 20 1.70 11 17 1.73 1 13 1.77 2 5 1.83 3 9 1.85 1 19 1.88 6 7 1.89 2 19 1.91 4 11 2.00 4 14 2.00 8 12 2.08 1 10 2.13 6 15 2.15 1 2 2.20 12 14 2.21 7 13 2.23 11 12 2.29 2 7 2.30 5 16 2.43 6 18 2.49 13 15 2.50 17 20 2.51 12 15 2.52 4 12 2.57 7 10 2.59 10 14 2.60 9 15 2.66 7 18 2.71 2 13 2.73 1 7 2.77 10 11 2.77 7 15 2.78 7 19 2.84 11 16 2.85 3 19 2.86 4 20 2.87 5 13 2.88 1 5 2.95 5 7 2.98 1 14 2.99 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. 0.22: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.06: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.78: Structure factors and derivatives 0.61: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.06: Solve l.s. equations 0.00: Generate HTAB table 0.06: Other dependent quantities, CIF, tables 0.16: Analysis of variance 0.06: Merge reflections for Fourier and .fcf 0.09: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 09:34:01 Total elapsed time: 3.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++