+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 17:18:00 on 04-Aug-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 01ESP001 in P2(1) CELL 0.71073 7.8231 12.9445 17.3686 90 95.668 90 ZERR 2 0.0002 0.0003 0.0004 0 0.001 0 LATT -1 SYMM -X, 1/2+Y, -Z SFAC C N O S H UNIT 72 4 20 2 76 V = 1750.25 F(000) = 728.0 Mu = 0.15 mm-1 Cell Wt = 1381.49 Rho = 1.311 SHEL 7 0.84 TEMP -93 OMIT -2 7 14 OMIT -2 6 16 FMAP 2 PLAN 20 BOND L.S. 4 WGHT 0.059500 EXTI 0.014668 FVAR 0.49888 MOLE 1 C1 1 0.502590 0.553282 1.044838 11.00000 0.03382 0.04264 = 0.03402 0.00177 0.00474 -0.00708 AFIX 43 H1 5 0.557341 0.492205 1.029455 11.00000 -1.20000 AFIX 0 C2 1 0.508998 0.579494 1.123167 11.00000 0.04210 0.07217 = 0.03396 0.00861 -0.00232 -0.01349 AFIX 43 H2 5 0.565956 0.535387 1.161188 11.00000 -1.20000 AFIX 0 C3 1 0.432324 0.669756 1.145351 11.00000 0.04160 0.07958 = 0.03273 -0.01513 0.01394 -0.01762 AFIX 43 H3 5 0.438138 0.687880 1.198547 11.00000 -1.20000 AFIX 0 C4 1 0.348803 0.732475 1.091258 11.00000 0.04561 0.07162 = 0.04501 -0.01389 0.02185 0.00355 AFIX 43 H4 5 0.297524 0.794681 1.106698 11.00000 -1.20000 AFIX 0 C5 1 0.338272 0.705936 1.013719 11.00000 0.03377 0.06136 = 0.03596 -0.00480 0.01457 0.00762 AFIX 43 H5 5 0.277085 0.749239 0.976384 11.00000 -1.20000 AFIX 0 C6 1 0.416432 0.616460 0.989941 11.00000 0.01743 0.04337 = 0.02968 -0.00113 0.00666 -0.00732 C7 1 0.410277 0.591144 0.904933 11.00000 0.02104 0.04009 = 0.02896 0.00019 0.00694 -0.00448 AFIX 23 H7A 5 0.432380 0.516457 0.898674 11.00000 -1.20000 H7B 5 0.294037 0.606366 0.879618 11.00000 -1.20000 AFIX 0 C8 1 0.496653 0.757745 0.844478 11.00000 0.02384 0.03788 = 0.03257 -0.00059 0.00014 0.00737 AFIX 137 H8A 5 0.517079 0.802693 0.889858 11.00000 -1.50000 H8B 5 0.375597 0.762096 0.823957 11.00000 -1.50000 H8C 5 0.569269 0.779936 0.804687 11.00000 -1.50000 AFIX 0 C9 1 0.692905 0.606661 0.862556 11.00000 0.02197 0.03034 = 0.01657 -0.00273 0.00400 -0.00034 C10 1 0.876977 0.761315 0.888675 11.00000 0.01904 0.03076 = 0.02243 -0.00411 -0.00162 0.00267 C11 1 0.937517 0.851745 0.857944 11.00000 0.03433 0.03310 = 0.03075 -0.00571 0.00383 -0.00147 AFIX 43 H11 5 0.948680 0.856507 0.804090 11.00000 -1.20000 AFIX 0 C12 1 0.981463 0.934744 0.905856 11.00000 0.04874 0.03523 = 0.05034 -0.01243 0.00458 -0.00927 AFIX 43 H12 5 1.024331 0.996175 0.884818 11.00000 -1.20000 AFIX 0 C13 1 0.963532 0.929172 0.984477 11.00000 0.04497 0.04755 = 0.04851 -0.02446 -0.00312 -0.00517 AFIX 43 H13 5 0.993836 0.986429 1.017230 11.00000 -1.20000 AFIX 0 C14 1 0.901683 0.840256 1.014367 11.00000 0.04219 0.06036 = 0.02570 -0.01528 -0.00517 0.00455 AFIX 43 H14 5 0.887506 0.836621 1.067994 11.00000 -1.20000 AFIX 0 C15 1 0.859194 0.754906 0.967123 11.00000 0.02897 0.03990 = 0.02633 -0.00330 -0.00066 0.00549 AFIX 43 H15 5 0.818538 0.693122 0.988538 11.00000 -1.20000 AFIX 0 C16 1 0.935324 0.638107 0.787414 11.00000 0.01857 0.02324 = 0.01839 0.00316 0.00062 0.00234 C17 1 0.872924 0.554698 0.729350 11.00000 0.01539 0.02311 = 0.02094 0.00203 0.00372 -0.00092 C18 1 0.969847 0.454220 0.743234 11.00000 0.02428 0.02177 = 0.01590 -0.00216 0.00327 0.00191 C19 1 0.890368 0.366419 0.768435 11.00000 0.02463 0.02672 = 0.01824 -0.00167 0.00216 0.00215 AFIX 43 H19 5 0.772301 0.368485 0.776927 11.00000 -1.20000 AFIX 0 C20 1 0.982648 0.275857 0.781230 11.00000 0.03970 0.02296 = 0.02256 -0.00099 0.00032 0.00173 AFIX 43 H20 5 0.927601 0.216089 0.798752 11.00000 -1.20000 AFIX 0 C21 1 1.155213 0.271555 0.768671 11.00000 0.03648 0.02860 = 0.02835 -0.00053 0.00276 0.01593 AFIX 43 H21 5 1.217674 0.208949 0.777005 11.00000 -1.20000 AFIX 0 C22 1 1.235700 0.359318 0.743876 11.00000 0.02936 0.03579 = 0.03310 -0.00097 0.00761 0.01190 AFIX 43 H22 5 1.354018 0.357123 0.735848 11.00000 -1.20000 AFIX 0 C23 1 1.143306 0.450467 0.730771 11.00000 0.02429 0.02801 = 0.02715 0.00044 0.00709 0.00228 AFIX 43 H23 5 1.198326 0.510279 0.713308 11.00000 -1.20000 AFIX 0 C24 1 0.837448 0.590193 0.646780 11.00000 0.01506 0.02214 = 0.02256 -0.00083 0.00217 0.00014 AFIX 13 H24 5 0.873806 0.540032 0.607755 11.00000 -1.20000 AFIX 0 C25 1 0.855864 0.702051 0.624621 11.00000 0.01127 0.02252 = 0.02161 -0.00140 0.00494 -0.00026 AFIX 13 H25 5 0.836804 0.747245 0.669680 11.00000 -1.20000 AFIX 0 C26 1 1.133300 0.784150 0.644528 11.00000 0.01754 0.02431 = 0.02316 0.00888 0.00192 -0.00099 C27 1 1.318139 0.760565 0.637917 11.00000 0.01481 0.04377 = 0.03370 0.00563 0.00199 0.00009 AFIX 137 H27A 5 1.384200 0.825006 0.640299 11.00000 -1.50000 H27B 5 1.329527 0.725918 0.588515 11.00000 -1.50000 H27C 5 1.361987 0.715292 0.680597 11.00000 -1.50000 AFIX 0 C28 1 0.733640 0.733286 0.554964 11.00000 0.01376 0.02243 = 0.01899 -0.00286 0.00476 -0.00022 AFIX 13 H28 5 0.612640 0.723591 0.567509 11.00000 -1.20000 AFIX 0 C29 1 0.630063 0.608636 0.460084 11.00000 0.02232 0.01664 = 0.02963 0.00076 -0.00362 0.00188 C30 1 0.674892 0.556084 0.388576 11.00000 0.02685 0.03373 = 0.03878 -0.01324 -0.00277 0.00646 AFIX 137 H30A 5 0.592462 0.500435 0.374987 11.00000 -1.50000 H30B 5 0.790854 0.527069 0.397543 11.00000 -1.50000 H30C 5 0.670882 0.606141 0.346105 11.00000 -1.50000 AFIX 0 C31 1 0.757913 0.845058 0.529991 11.00000 0.01698 0.02006 = 0.02169 -0.00164 0.00659 0.00151 AFIX 13 H31 5 0.880630 0.855330 0.520254 11.00000 -1.20000 AFIX 0 C32 1 0.815273 0.995297 0.606413 11.00000 0.02298 0.01708 = 0.04039 0.00132 -0.01215 0.00282 C33 1 0.789399 1.044399 0.682257 11.00000 0.03994 0.02511 = 0.04344 -0.00736 -0.01296 0.00636 AFIX 137 H33A 5 0.901329 1.060351 0.710158 11.00000 -1.50000 H33B 5 0.726669 0.996762 0.713121 11.00000 -1.50000 H33C 5 0.723230 1.108285 0.673232 11.00000 -1.50000 AFIX 0 C34 1 0.644447 0.877166 0.458854 11.00000 0.01517 0.02487 = 0.02362 0.00296 0.00413 -0.00084 AFIX 23 H34A 5 0.662065 0.951417 0.448487 11.00000 -1.20000 H34B 5 0.675664 0.837364 0.413625 11.00000 -1.20000 AFIX 0 C35 1 0.368780 0.806680 0.413288 11.00000 0.02011 0.02137 = 0.02225 0.00562 -0.00081 0.00040 C36 1 0.187287 0.797448 0.431967 11.00000 0.02175 0.03559 = 0.02441 0.00463 0.00001 -0.00224 AFIX 137 H36A 5 0.109763 0.802479 0.384222 11.00000 -1.50000 H36B 5 0.161851 0.853214 0.467254 11.00000 -1.50000 H36C 5 0.171048 0.730587 0.456694 11.00000 -1.50000 AFIX 0 N1 2 0.825486 0.675106 0.838707 11.00000 0.01932 0.02458 = 0.02151 -0.00069 0.00384 0.00015 N2 2 0.538435 0.651130 0.866746 11.00000 0.01902 0.03261 = 0.02391 -0.00114 0.00431 0.00016 O1 3 0.728421 0.517289 0.877932 11.00000 0.03341 0.02805 = 0.02934 0.00487 0.00986 0.00395 O2 3 1.079477 0.673792 0.784341 11.00000 0.01522 0.03212 = 0.02701 -0.00003 0.00162 -0.00179 O3 3 1.033097 0.710039 0.607720 11.00000 0.01184 0.02815 = 0.02344 0.00213 0.00466 0.00137 O4 3 1.078572 0.857044 0.677183 11.00000 0.01992 0.02595 = 0.03822 0.00288 0.00158 -0.00314 O5 3 0.763017 0.669453 0.489938 11.00000 0.01671 0.02513 = 0.02098 -0.00505 0.00194 0.00109 O6 3 0.496564 0.601810 0.488672 11.00000 0.02357 0.02734 = 0.03838 -0.00289 0.00311 -0.00637 O7 3 0.723260 0.905658 0.596338 11.00000 0.01914 0.01836 = 0.02531 -0.00296 0.00143 0.00030 O8 3 0.904500 1.027294 0.559460 11.00000 0.02734 0.02872 = 0.05016 0.00678 -0.00144 -0.00775 O9 3 0.465549 0.858894 0.469752 11.00000 0.01644 0.02607 = 0.02037 0.00036 0.00194 0.00119 O10 3 0.425281 0.772160 0.356360 11.00000 0.02820 0.02778 = 0.02441 -0.00264 0.00527 -0.00046 S1 4 0.648554 0.551211 0.691555 11.00000 0.01694 0.02396 = 0.02319 0.00281 0.00115 -0.00219 HKLF 4 Covalent radii and connectivity table for 01ESP001 in P2(1) C 0.770 N 0.700 O 0.660 S 1.030 H 0.320 C1 - C6 C2 C2 - C3 C1 C3 - C4 C2 C4 - C3 C5 C5 - C4 C6 C6 - C1 C5 C7 C7 - N2 C6 C8 - N2 C9 - O1 N2 N1 C10 - C15 C11 N1 C11 - C12 C10 C12 - C11 C13 C13 - C14 C12 C14 - C13 C15 C15 - C10 C14 C16 - O2 N1 C17 C17 - C24 C18 C16 S1 C18 - C19 C23 C17 C19 - C20 C18 C20 - C19 C21 C21 - C22 C20 C22 - C21 C23 C23 - C22 C18 C24 - C17 C25 S1 C25 - O3 C24 C28 C26 - O4 O3 C27 C27 - C26 C28 - O5 C25 C31 C29 - O6 O5 C30 C30 - C29 C31 - O7 C34 C28 C32 - O8 O7 C33 C33 - C32 C34 - O9 C31 C35 - O10 O9 C36 C36 - C35 N1 - C16 C10 C9 N2 - C9 C8 C7 O1 - C9 O2 - C16 O3 - C26 C25 O4 - C26 O5 - C29 C28 O6 - C29 O7 - C32 C31 O8 - C32 O9 - C35 C34 O10 - C35 S1 - C24 C17 Floating origin restraints generated 15087 Reflections read, of which 1894 rejected -9 =< h =< 9, -15 =< k =< 15, -20 =< l =< 20, Max. 2-theta = 50.05 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 2 -2 1 84.60 2.64 2 18.10 6 1 2 200.83 5.77 3 30.41 1 2 2 361.25 11.33 2 89.88 -2 -1 3 333.43 9.67 2 59.90 1 2 3 89.21 0.22 2 216.10 1 3 3 161.20 2.27 2 88.41 0 2 4 361.55 11.81 2 105.44 0 4 4 675.41 8.67 3 186.22 1 -5 5 29.32 0.93 2 5.37 2 7 5 20.92 0.73 2 19.07 2 9 5 32.12 0.94 2 31.86 4 11 6 6.15 0.94 2 12.98 -2 -5 7 317.64 7.61 3 43.15 3 5 7 47.14 0.87 2 35.24 4 8 7 49.54 1.09 2 53.38 0 11 7 32.62 0.78 2 54.56 4 2 8 275.56 8.39 2 43.11 -1 5 8 156.09 4.61 3 24.90 -1 6 8 18.49 0.33 3 7.97 -1 7 8 35.85 0.44 3 14.62 5 8 8 3.55 1.07 2 6.88 -1 5 9 6.79 0.39 3 3.43 -1 6 9 40.47 0.81 3 12.73 -2 10 11 18.93 0.86 3 6.22 -2 11 11 9.93 0.97 2 8.28 -1 5 12 344.40 11.73 3 91.23 4 4 13 43.31 2.32 2 13.64 27 Inconsistent equivalents 5997 Unique reflections, of which 0 suppressed R(int) = 0.0762 R(sigma) = 0.0679 Friedel opposites not merged Maximum memory for data reduction = 3868 / 60108 Default effective X-H distances for T = -93.0 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 = 5126 / 583345 wR2 = 0.1038 before cycle 1 for 5997 data and 448 / 448 parameters GooF = S = 1.027; Restrained GooF = 1.027 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0595 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.49888 0.00093 0.003 OSF 2 0.01467 0.00182 0.001 EXTI Mean shift/esd = 0.002 Maximum = -0.011 for U11 S1 Max. shift = 0.000 A for H27A Max. dU = 0.000 for C16 Least-squares cycle 2 Maximum vector length = 511 Memory required = 5126 / 583345 wR2 = 0.1038 before cycle 2 for 5997 data and 448 / 448 parameters GooF = S = 1.027; Restrained GooF = 1.027 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0595 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.49888 0.00093 0.000 OSF 2 0.01467 0.00182 0.000 EXTI Mean shift/esd = 0.001 Maximum = -0.004 for U11 S1 Max. shift = 0.000 A for H27A Max. dU = 0.000 for C33 Least-squares cycle 3 Maximum vector length = 511 Memory required = 5126 / 583345 wR2 = 0.1038 before cycle 3 for 5997 data and 448 / 448 parameters GooF = S = 1.027; Restrained GooF = 1.027 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0595 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.49888 0.00093 -0.001 OSF 2 0.01467 0.00182 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for tors H27A Max. shift = 0.000 A for H27B Max. dU = 0.000 for O8 Least-squares cycle 4 Maximum vector length = 511 Memory required = 5126 / 583345 wR2 = 0.1038 before cycle 4 for 5997 data and 448 / 448 parameters GooF = S = 1.027; Restrained GooF = 1.027 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0595 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.49888 0.00093 -0.002 OSF 2 0.01467 0.00182 -0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for OSF Max. shift = 0.000 A for H27A Max. dU = 0.000 for C3 Largest correlation matrix elements 0.541 EXTI / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.5573 0.4922 1.0295 43 0.950 0.000 C1 C6 C2 H2 0.5660 0.5354 1.1612 43 0.950 0.000 C2 C3 C1 H3 0.4381 0.6879 1.1985 43 0.950 0.000 C3 C4 C2 H4 0.2975 0.7947 1.1067 43 0.950 0.000 C4 C3 C5 H5 0.2771 0.7492 0.9764 43 0.950 0.000 C5 C4 C6 H7A 0.4324 0.5165 0.8987 23 0.990 0.000 C7 N2 C6 H7B 0.2940 0.6064 0.8796 23 0.990 0.000 C7 N2 C6 H8A 0.5171 0.8027 0.8899 137 0.980 0.000 C8 N2 H8A H8B 0.3756 0.7621 0.8240 137 0.980 0.000 C8 N2 H8A H8C 0.5693 0.7799 0.8047 137 0.980 0.000 C8 N2 H8A H11 0.9487 0.8565 0.8041 43 0.950 0.000 C11 C12 C10 H12 1.0243 0.9962 0.8848 43 0.950 0.000 C12 C11 C13 H13 0.9938 0.9864 1.0172 43 0.950 0.000 C13 C14 C12 H14 0.8875 0.8366 1.0680 43 0.950 0.000 C14 C13 C15 H15 0.8185 0.6931 0.9885 43 0.950 0.000 C15 C10 C14 H19 0.7723 0.3685 0.7769 43 0.950 0.000 C19 C20 C18 H20 0.9276 0.2161 0.7988 43 0.950 0.000 C20 C19 C21 H21 1.2177 0.2089 0.7770 43 0.950 0.000 C21 C22 C20 H22 1.3540 0.3571 0.7358 43 0.950 0.000 C22 C21 C23 H23 1.1983 0.5103 0.7133 43 0.950 0.000 C23 C22 C18 H24 0.8738 0.5400 0.6078 13 1.000 0.000 C24 C17 C25 S1 H25 0.8368 0.7472 0.6697 13 1.000 0.000 C25 O3 C24 C28 H27A 1.3842 0.8250 0.6403 137 0.980 0.000 C27 C26 H27A H27B 1.3295 0.7259 0.5885 137 0.980 0.000 C27 C26 H27A H27C 1.3620 0.7153 0.6806 137 0.980 0.000 C27 C26 H27A H28 0.6126 0.7236 0.5675 13 1.000 0.000 C28 O5 C25 C31 H30A 0.5925 0.5004 0.3750 137 0.980 0.000 C30 C29 H30A H30B 0.7909 0.5271 0.3975 137 0.980 0.000 C30 C29 H30A H30C 0.6709 0.6061 0.3461 137 0.980 0.000 C30 C29 H30A H31 0.8806 0.8553 0.5203 13 1.000 0.000 C31 O7 C34 C28 H33A 0.9013 1.0604 0.7102 137 0.980 0.000 C33 C32 H33A H33B 0.7267 0.9968 0.7131 137 0.980 0.000 C33 C32 H33A H33C 0.7232 1.1083 0.6732 137 0.980 0.000 C33 C32 H33A H34A 0.6621 0.9514 0.4485 23 0.990 0.000 C34 O9 C31 H34B 0.6757 0.8374 0.4136 23 0.990 0.000 C34 O9 C31 H36A 0.1098 0.8025 0.3842 137 0.980 0.000 C36 C35 H36A H36B 0.1618 0.8532 0.4673 137 0.980 0.000 C36 C35 H36A H36C 0.1711 0.7306 0.4567 137 0.980 0.000 C36 C35 H36A 01ESP001 in P2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.50259 0.55328 1.04484 1.00000 0.03382 0.04264 0.03402 0.00177 0.00474 -0.00708 0.03673 0.00493 0.00035 0.00026 0.00015 0.00000 0.00147 0.00148 0.00145 0.00142 0.00114 0.00136 0.00062 H1 0.55734 0.49221 1.02945 1.00000 0.04408 0.00000 0.00000 C2 0.50900 0.57949 1.12317 1.00000 0.04210 0.07217 0.03396 0.00861 -0.00232 -0.01349 0.04982 0.00561 0.00041 0.00029 0.00018 0.00000 0.00182 0.00242 0.00157 0.00163 0.00134 0.00166 0.00087 H2 0.56596 0.53539 1.16119 1.00000 0.05978 0.00000 0.00000 C3 0.43232 0.66976 1.14535 1.00000 0.04160 0.07958 0.03273 -0.01513 0.01394 -0.01762 0.05062 0.00564 0.00041 0.00031 0.00018 0.00000 0.00178 0.00253 0.00161 0.00176 0.00143 0.00173 0.00089 H3 0.43814 0.68788 1.19855 1.00000 0.06075 0.00000 0.00000 C4 0.34880 0.73247 1.09126 1.00000 0.04561 0.07162 0.04501 -0.01389 0.02185 0.00355 0.05292 0.00625 0.00043 0.00030 0.00019 0.00000 0.00191 0.00236 0.00190 0.00180 0.00157 0.00170 0.00089 H4 0.29752 0.79468 1.10670 1.00000 0.06351 0.00000 0.00000 C5 0.33827 0.70594 1.01372 1.00000 0.03377 0.06136 0.03596 -0.00480 0.01457 0.00762 0.04296 0.00566 0.00038 0.00026 0.00017 0.00000 0.00159 0.00193 0.00154 0.00151 0.00127 0.00148 0.00072 H5 0.27708 0.74924 0.97638 1.00000 0.05155 0.00000 0.00000 C6 0.41643 0.61646 0.98994 1.00000 0.01743 0.04337 0.02968 -0.00113 0.00666 -0.00732 0.02987 0.00447 0.00031 0.00021 0.00014 0.00000 0.00121 0.00164 0.00134 0.00128 0.00102 0.00109 0.00061 C7 0.41028 0.59114 0.90493 1.00000 0.02104 0.04009 0.02896 0.00019 0.00694 -0.00448 0.02973 0.00462 0.00032 0.00022 0.00014 0.00000 0.00131 0.00144 0.00131 0.00119 0.00103 0.00109 0.00058 H7A 0.43238 0.51646 0.89867 1.00000 0.03568 0.00000 0.00000 H7B 0.29404 0.60637 0.87962 1.00000 0.03568 0.00000 0.00000 C8 0.49665 0.75775 0.84448 1.00000 0.02384 0.03788 0.03257 -0.00059 0.00014 0.00737 0.03161 0.00490 0.00033 0.00022 0.00016 0.00000 0.00130 0.00147 0.00139 0.00129 0.00105 0.00116 0.00059 H8A 0.51708 0.80269 0.88986 1.00000 0.04741 0.00000 0.00000 H8B 0.37560 0.76210 0.82396 1.00000 0.04741 0.00000 0.00000 H8C 0.56927 0.77994 0.80469 1.00000 0.04741 0.00000 0.00000 C9 0.69291 0.60666 0.86256 1.00000 0.02197 0.03034 0.01657 -0.00273 0.00400 -0.00034 0.02282 0.00424 0.00031 0.00020 0.00013 0.00000 0.00130 0.00145 0.00113 0.00108 0.00093 0.00104 0.00054 C10 0.87698 0.76131 0.88868 1.00000 0.01904 0.03076 0.02243 -0.00411 -0.00162 0.00267 0.02432 0.00422 0.00029 0.00020 0.00014 0.00000 0.00119 0.00131 0.00121 0.00114 0.00093 0.00103 0.00053 C11 0.93752 0.85174 0.85794 1.00000 0.03433 0.03310 0.03075 -0.00571 0.00383 -0.00147 0.03269 0.00469 0.00034 0.00021 0.00016 0.00000 0.00149 0.00141 0.00139 0.00124 0.00114 0.00116 0.00061 H11 0.94868 0.85651 0.80409 1.00000 0.03923 0.00000 0.00000 C12 0.98146 0.93474 0.90586 1.00000 0.04874 0.03523 0.05034 -0.01243 0.00458 -0.00927 0.04479 0.00529 0.00041 0.00024 0.00019 0.00000 0.00186 0.00157 0.00180 0.00151 0.00142 0.00140 0.00074 H12 1.02433 0.99617 0.88482 1.00000 0.05375 0.00000 0.00000 C13 0.96353 0.92917 0.98448 1.00000 0.04497 0.04755 0.04851 -0.02446 -0.00312 -0.00517 0.04752 0.00519 0.00040 0.00026 0.00019 0.00000 0.00193 0.00188 0.00191 0.00161 0.00145 0.00150 0.00081 H13 0.99384 0.98643 1.01723 1.00000 0.05703 0.00000 0.00000 C14 0.90168 0.84026 1.01437 1.00000 0.04219 0.06036 0.02570 -0.01528 -0.00517 0.00455 0.04332 0.00512 0.00039 0.00026 0.00017 0.00000 0.00174 0.00206 0.00142 0.00148 0.00124 0.00148 0.00077 H14 0.88751 0.83662 1.06799 1.00000 0.05198 0.00000 0.00000 C15 0.85919 0.75491 0.96712 1.00000 0.02897 0.03990 0.02633 -0.00330 -0.00066 0.00549 0.03196 0.00478 0.00033 0.00023 0.00015 0.00000 0.00142 0.00152 0.00137 0.00125 0.00106 0.00120 0.00061 H15 0.81854 0.69312 0.98854 1.00000 0.03835 0.00000 0.00000 C16 0.93532 0.63811 0.78741 1.00000 0.01857 0.02324 0.01839 0.00316 0.00062 0.00234 0.02015 0.00407 0.00029 0.00018 0.00013 0.00000 0.00129 0.00116 0.00113 0.00102 0.00093 0.00101 0.00050 C17 0.87292 0.55470 0.72935 1.00000 0.01539 0.02311 0.02094 0.00203 0.00372 -0.00092 0.01968 0.00401 0.00027 0.00019 0.00013 0.00000 0.00108 0.00110 0.00112 0.00108 0.00086 0.00098 0.00047 C18 0.96985 0.45422 0.74323 1.00000 0.02428 0.02177 0.01590 -0.00216 0.00327 0.00191 0.02057 0.00409 0.00030 0.00018 0.00013 0.00000 0.00132 0.00119 0.00110 0.00100 0.00095 0.00098 0.00051 C19 0.89037 0.36642 0.76844 1.00000 0.02463 0.02672 0.01824 -0.00167 0.00216 0.00215 0.02319 0.00416 0.00031 0.00019 0.00013 0.00000 0.00128 0.00124 0.00114 0.00105 0.00092 0.00105 0.00051 H19 0.77230 0.36849 0.77693 1.00000 0.02783 0.00000 0.00000 C20 0.98265 0.27586 0.78123 1.00000 0.03970 0.02296 0.02256 -0.00099 0.00032 0.00173 0.02859 0.00442 0.00034 0.00020 0.00014 0.00000 0.00155 0.00120 0.00122 0.00111 0.00105 0.00112 0.00057 H20 0.92760 0.21609 0.79875 1.00000 0.03431 0.00000 0.00000 C21 1.15521 0.27156 0.76867 1.00000 0.03648 0.02860 0.02835 -0.00053 0.00276 0.01593 0.03117 0.00481 0.00034 0.00021 0.00015 0.00000 0.00154 0.00132 0.00136 0.00123 0.00112 0.00119 0.00060 H21 1.21767 0.20895 0.77700 1.00000 0.03741 0.00000 0.00000 C22 1.23570 0.35932 0.74388 1.00000 0.02936 0.03579 0.03310 -0.00097 0.00761 0.01190 0.03245 0.00493 0.00035 0.00021 0.00015 0.00000 0.00142 0.00144 0.00144 0.00122 0.00114 0.00117 0.00061 H22 1.35402 0.35712 0.73585 1.00000 0.03894 0.00000 0.00000 C23 1.14331 0.45047 0.73077 1.00000 0.02429 0.02801 0.02715 0.00044 0.00709 0.00228 0.02618 0.00450 0.00031 0.00020 0.00014 0.00000 0.00132 0.00129 0.00130 0.00110 0.00103 0.00104 0.00055 H23 1.19833 0.51028 0.71331 1.00000 0.03142 0.00000 0.00000 C24 0.83745 0.59019 0.64678 1.00000 0.01506 0.02214 0.02256 -0.00083 0.00217 0.00014 0.01990 0.00404 0.00028 0.00018 0.00013 0.00000 0.00114 0.00114 0.00116 0.00100 0.00093 0.00089 0.00049 H24 0.87381 0.54003 0.60776 1.00000 0.02388 0.00000 0.00000 C25 0.85586 0.70205 0.62462 1.00000 0.01127 0.02252 0.02161 -0.00140 0.00494 -0.00026 0.01825 0.00406 0.00027 0.00018 0.00013 0.00000 0.00108 0.00115 0.00115 0.00101 0.00088 0.00089 0.00047 H25 0.83680 0.74724 0.66968 1.00000 0.02190 0.00000 0.00000 C26 1.13330 0.78415 0.64453 1.00000 0.01754 0.02431 0.02316 0.00888 0.00192 -0.00099 0.02168 0.00431 0.00030 0.00019 0.00014 0.00000 0.00120 0.00123 0.00119 0.00107 0.00094 0.00101 0.00052 C27 1.31814 0.76056 0.63792 1.00000 0.01481 0.04377 0.03370 0.00563 0.00200 0.00009 0.03079 0.00481 0.00029 0.00023 0.00016 0.00000 0.00122 0.00157 0.00140 0.00131 0.00100 0.00112 0.00059 H27A 1.38420 0.82501 0.64029 1.00000 0.04618 0.00000 0.00000 H27B 1.32953 0.72591 0.58852 1.00000 0.04618 0.00000 0.00000 H27C 1.36199 0.71530 0.68060 1.00000 0.04618 0.00000 0.00000 C28 0.73364 0.73329 0.55496 1.00000 0.01376 0.02243 0.01899 -0.00286 0.00476 -0.00022 0.01818 0.00399 0.00028 0.00017 0.00013 0.00000 0.00109 0.00118 0.00113 0.00096 0.00089 0.00089 0.00048 H28 0.61264 0.72359 0.56751 1.00000 0.02182 0.00000 0.00000 C29 0.63006 0.60864 0.46008 1.00000 0.02232 0.01664 0.02963 0.00076 -0.00362 0.00188 0.02327 0.00426 0.00031 0.00018 0.00014 0.00000 0.00137 0.00111 0.00127 0.00103 0.00104 0.00093 0.00053 C30 0.67489 0.55608 0.38858 1.00000 0.02685 0.03373 0.03878 -0.01324 -0.00277 0.00646 0.03352 0.00460 0.00032 0.00023 0.00015 0.00000 0.00135 0.00138 0.00145 0.00136 0.00112 0.00122 0.00060 H30A 0.59246 0.50044 0.37499 1.00000 0.05028 0.00000 0.00000 H30B 0.79085 0.52707 0.39754 1.00000 0.05028 0.00000 0.00000 H30C 0.67089 0.60614 0.34611 1.00000 0.05028 0.00000 0.00000 C31 0.75791 0.84506 0.52999 1.00000 0.01698 0.02006 0.02169 -0.00164 0.00659 0.00151 0.01927 0.00406 0.00029 0.00017 0.00013 0.00000 0.00113 0.00117 0.00117 0.00098 0.00093 0.00089 0.00049 H31 0.88063 0.85533 0.52025 1.00000 0.02312 0.00000 0.00000 C32 0.81527 0.99530 0.60641 1.00000 0.02298 0.01708 0.04039 0.00132 -0.01215 0.00282 0.02783 0.00437 0.00033 0.00018 0.00016 0.00000 0.00136 0.00125 0.00157 0.00118 0.00122 0.00101 0.00061 C33 0.78940 1.04440 0.68226 1.00000 0.03994 0.02511 0.04344 -0.00736 -0.01296 0.00636 0.03730 0.00461 0.00036 0.00022 0.00016 0.00000 0.00158 0.00132 0.00159 0.00137 0.00125 0.00124 0.00066 H33A 0.90133 1.06035 0.71016 1.00000 0.05595 0.00000 0.00000 H33B 0.72667 0.99676 0.71312 1.00000 0.05595 0.00000 0.00000 H33C 0.72323 1.10828 0.67323 1.00000 0.05595 0.00000 0.00000 C34 0.64445 0.87717 0.45885 1.00000 0.01517 0.02487 0.02362 0.00296 0.00413 -0.00084 0.02108 0.00412 0.00028 0.00018 0.00013 0.00000 0.00117 0.00119 0.00118 0.00103 0.00092 0.00096 0.00050 H34A 0.66207 0.95142 0.44849 1.00000 0.02529 0.00000 0.00000 H34B 0.67566 0.83736 0.41362 1.00000 0.02529 0.00000 0.00000 C35 0.36878 0.80668 0.41329 1.00000 0.02011 0.02137 0.02225 0.00562 -0.00081 0.00040 0.02143 0.00413 0.00030 0.00018 0.00014 0.00000 0.00122 0.00116 0.00123 0.00105 0.00100 0.00094 0.00051 C36 0.18729 0.79745 0.43197 1.00000 0.02175 0.03559 0.02441 0.00463 0.00001 -0.00224 0.02740 0.00450 0.00032 0.00020 0.00015 0.00000 0.00129 0.00148 0.00124 0.00110 0.00100 0.00104 0.00057 H36A 0.10976 0.80247 0.38422 1.00000 0.04110 0.00000 0.00000 H36B 0.16185 0.85322 0.46725 1.00000 0.04110 0.00000 0.00000 H36C 0.17105 0.73059 0.45670 1.00000 0.04110 0.00000 0.00000 N1 0.82549 0.67511 0.83871 1.00000 0.01932 0.02458 0.02151 -0.00069 0.00384 0.00015 0.02168 0.00340 0.00024 0.00015 0.00011 0.00000 0.00105 0.00108 0.00099 0.00088 0.00080 0.00080 0.00045 N2 0.53844 0.65113 0.86675 1.00000 0.01902 0.03261 0.02391 -0.00114 0.00431 0.00016 0.02504 0.00360 0.00025 0.00017 0.00011 0.00000 0.00106 0.00112 0.00102 0.00093 0.00082 0.00087 0.00046 O1 0.72842 0.51729 0.87793 1.00000 0.03341 0.02805 0.02934 0.00487 0.00986 0.00395 0.02982 0.00322 0.00023 0.00013 0.00010 0.00000 0.00104 0.00097 0.00098 0.00080 0.00079 0.00077 0.00042 O2 1.07948 0.67379 0.78434 1.00000 0.01522 0.03212 0.02701 -0.00003 0.00162 -0.00179 0.02481 0.00283 0.00020 0.00013 0.00009 0.00000 0.00086 0.00095 0.00088 0.00077 0.00068 0.00071 0.00039 O3 1.03310 0.71004 0.60772 1.00000 0.01184 0.02815 0.02344 0.00213 0.00466 0.00137 0.02095 0.00279 0.00019 0.00012 0.00009 0.00000 0.00076 0.00086 0.00083 0.00073 0.00065 0.00065 0.00036 O4 1.07857 0.85704 0.67718 1.00000 0.01992 0.02595 0.03822 0.00288 0.00158 -0.00314 0.02812 0.00310 0.00022 0.00014 0.00010 0.00000 0.00086 0.00089 0.00101 0.00085 0.00073 0.00074 0.00040 O5 0.76302 0.66945 0.48994 1.00000 0.01671 0.02513 0.02098 -0.00505 0.00194 0.00109 0.02093 0.00268 0.00019 0.00012 0.00009 0.00000 0.00081 0.00085 0.00081 0.00071 0.00064 0.00066 0.00036 O6 0.49656 0.60181 0.48867 1.00000 0.02357 0.02734 0.03838 -0.00289 0.00311 -0.00637 0.02976 0.00304 0.00023 0.00013 0.00011 0.00000 0.00095 0.00090 0.00102 0.00081 0.00078 0.00072 0.00041 O7 0.72326 0.90566 0.59634 1.00000 0.01914 0.01836 0.02531 -0.00296 0.00143 0.00030 0.02099 0.00267 0.00020 0.00012 0.00009 0.00000 0.00084 0.00078 0.00086 0.00070 0.00065 0.00063 0.00036 O8 0.90450 1.02729 0.55946 1.00000 0.02734 0.02872 0.05016 0.00678 -0.00144 -0.00775 0.03576 0.00320 0.00023 0.00014 0.00012 0.00000 0.00099 0.00099 0.00117 0.00089 0.00090 0.00076 0.00046 O9 0.46555 0.85889 0.46975 1.00000 0.01644 0.02607 0.02037 0.00036 0.00194 0.00119 0.02095 0.00274 0.00019 0.00012 0.00009 0.00000 0.00079 0.00083 0.00081 0.00073 0.00064 0.00066 0.00036 O10 0.42528 0.77216 0.35636 1.00000 0.02820 0.02778 0.02441 -0.00264 0.00527 -0.00046 0.02662 0.00296 0.00021 0.00013 0.00010 0.00000 0.00093 0.00089 0.00089 0.00079 0.00072 0.00073 0.00038 S1 0.64855 0.55121 0.69156 1.00000 0.01694 0.02396 0.02319 0.00281 0.00115 -0.00219 0.02142 0.00096 0.00007 0.00004 0.00003 0.00000 0.00028 0.00029 0.00030 0.00025 0.00022 0.00024 0.00015 Final Structure Factor Calculation for 01ESP001 in P2(1) Total number of l.s. parameters = 448 Maximum vector length = 511 Memory required = 4680 / 26068 wR2 = 0.1038 before cycle 5 for 5997 data and 2 / 448 parameters GooF = S = 1.027; Restrained GooF = 1.027 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0595 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0418 for 5488 Fo > 4sig(Fo) and 0.0475 for all 5997 data wR2 = 0.1038, GooF = S = 1.027, Restrained GooF = 1.027 for all data Flack x parameter = 0.0117 with esd 0.0638 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Occupancy sum of asymmetric unit = 49.00 for non-hydrogen and 38.00 for hydrogen atoms Principal mean square atomic displacements U 0.0468 0.0348 0.0287 C1 0.0804 0.0380 0.0311 C2 0.0909 0.0364 0.0246 C3 0.0777 0.0586 0.0225 C4 0.0636 0.0449 0.0203 C5 0.0455 0.0301 0.0140 C6 0.0411 0.0304 0.0177 C7 0.0416 0.0328 0.0205 C8 0.0309 0.0224 0.0152 C9 0.0338 0.0221 0.0170 C10 0.0381 0.0338 0.0261 C11 0.0589 0.0496 0.0259 C12 0.0730 0.0482 0.0213 C13 0.0690 0.0421 0.0188 C14 0.0436 0.0279 0.0243 C15 0.0251 0.0198 0.0156 C16 0.0243 0.0205 0.0143 C17 0.0253 0.0218 0.0146 C18 0.0284 0.0234 0.0178 C19 0.0407 0.0234 0.0217 C20 0.0491 0.0284 0.0160 C21 0.0450 0.0340 0.0184 C22 0.0310 0.0274 0.0201 C23 0.0232 0.0215 0.0150 C24 0.0238 0.0210 0.0099 C25 0.0328 0.0177 0.0145 C26 0.0463 0.0312 0.0148 C27 0.0242 0.0185 0.0118 C28 0.0338 0.0204 0.0156 C29 0.0537 0.0252 0.0216 C30 0.0243 0.0207 0.0129 C31 0.0509 0.0194 0.0132 C32 0.0635 0.0261 0.0224 C33 0.0273 0.0219 0.0141 C34 0.0282 0.0207 0.0154 C35 0.0380 0.0236 0.0206 C36 0.0247 0.0223 0.0181 N1 0.0328 0.0244 0.0179 N2 0.0405 0.0261 0.0228 O1 0.0323 0.0271 0.0150 O2 0.0292 0.0229 0.0108 O3 0.0393 0.0265 0.0185 O4 0.0287 0.0180 0.0161 O5 0.0391 0.0314 0.0188 O6 0.0266 0.0191 0.0172 O7 0.0550 0.0322 0.0201 O8 0.0262 0.0204 0.0163 O9 0.0304 0.0275 0.0219 O10 0.0271 0.0209 0.0163 S1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.037 0.056 0.070 0.085 0.101 0.119 0.146 0.181 0.235 1.000 Number in group 607. 641. 562. 608. 592. 589. 607. 599. 592. 600. GooF 0.864 0.969 1.036 1.003 1.083 1.068 1.086 1.082 1.094 0.974 K 1.017 0.985 0.977 0.987 0.996 1.008 1.021 1.030 1.033 1.016 Resolution(A) 0.84 0.87 0.91 0.95 1.01 1.07 1.15 1.27 1.45 1.81 inf Number in group 610. 589. 599. 625. 579. 605. 601. 593. 591. 605. GooF 0.892 0.986 1.022 1.062 1.008 1.040 0.983 1.054 1.103 1.106 K 1.022 1.008 1.029 1.027 1.023 1.031 1.023 1.034 1.027 1.005 R1 0.098 0.087 0.069 0.058 0.047 0.043 0.037 0.037 0.034 0.033 Recommended weighting scheme: WGHT 0.0595 0.0000 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 4 17 425.14 279.26 4.21 0.139 0.92 -3 -1 2 2825.01 2104.22 4.04 0.382 2.51 2 -8 6 731.34 533.58 4.04 0.193 1.31 2 -5 8 500.83 680.35 3.90 0.217 1.49 0 2 2 285.96 371.89 3.88 0.161 5.18 2 -4 9 491.59 668.22 3.77 0.215 1.48 1 -5 6 212.04 284.39 3.76 0.141 1.84 7 -2 1 87.47 54.53 3.62 0.062 1.09 0 4 17 344.55 249.12 3.59 0.132 0.97 -2 -9 9 642.24 475.86 3.46 0.182 1.12 -2 -7 4 533.60 405.40 3.44 0.168 1.58 -2 -9 8 563.05 430.48 3.37 0.173 1.16 4 -4 5 298.16 237.09 3.35 0.128 1.45 -1 -9 8 247.20 185.04 3.32 0.113 1.19 1 0 20 206.74 131.75 3.21 0.096 0.85 8 -5 1 754.72 581.58 3.20 0.201 0.91 1 2 4 2638.04 3297.88 3.20 0.479 3.17 -8 4 4 88.51 133.98 3.19 0.096 0.93 -2 -3 10 8.90 20.49 3.19 0.038 1.53 -2 6 3 82.74 104.36 3.17 0.085 1.82 1 -11 6 181.86 139.73 3.17 0.099 1.07 2 -7 8 380.72 498.29 3.15 0.186 1.30 8 -4 2 541.25 423.08 3.13 0.171 0.92 6 -6 3 585.85 470.93 3.10 0.181 1.07 -2 -11 8 224.36 168.59 3.08 0.108 1.01 -4 -3 2 52.57 35.01 3.07 0.049 1.77 -7 2 5 8.82 21.69 3.06 0.039 1.08 -6 5 1 104.05 137.28 3.06 0.098 1.16 0 3 2 974.61 1188.64 3.03 0.287 3.86 -5 -3 6 640.56 499.08 3.02 0.186 1.36 2 -4 6 496.61 404.65 3.02 0.168 1.83 2 -6 1 148.16 119.31 2.97 0.091 1.87 1 -8 1 463.53 567.04 2.95 0.198 1.57 -1 -5 4 2109.06 1723.92 2.90 0.346 2.16 3 -4 4 44.35 33.05 2.89 0.048 1.78 -4 3 15 66.44 41.46 2.89 0.054 1.01 0 -10 7 762.99 617.69 2.87 0.207 1.15 5 -6 6 771.27 637.18 2.87 0.210 1.12 6 7 4 31.09 48.85 2.86 0.058 1.01 -5 -2 2 467.97 371.61 2.85 0.161 1.52 1 1 2 634.95 762.84 2.85 0.230 5.08 3 -4 3 571.57 454.80 2.83 0.178 1.87 -7 7 3 26.71 43.69 2.81 0.055 0.95 -1 4 9 147.26 115.22 2.77 0.089 1.64 -4 3 12 280.44 227.73 2.76 0.126 1.17 0 2 1 1036.14 1243.79 2.76 0.294 6.06 -8 5 1 102.54 146.85 2.76 0.101 0.91 -1 6 3 82.97 100.83 2.75 0.084 1.97 -3 -3 11 156.23 194.78 2.75 0.116 1.34 0 7 4 18.86 25.07 2.69 0.042 1.70 Bond lengths and angles C1 - Distance Angles C6 1.3803 (0.0039) C2 1.3982 (0.0041) 119.77 (0.30) C1 - C6 C2 - Distance Angles C3 1.3853 (0.0052) C1 1.3982 (0.0041) 120.03 (0.32) C2 - C3 C3 - Distance Angles C4 1.3592 (0.0050) C2 1.3853 (0.0052) 120.22 (0.29) C3 - C4 C4 - Distance Angles C3 1.3592 (0.0051) C5 1.3844 (0.0045) 120.17 (0.32) C4 - C3 C5 - Distance Angles C4 1.3844 (0.0045) C6 1.3913 (0.0040) 120.64 (0.31) C5 - C4 C6 - Distance Angles C1 1.3803 (0.0039) C5 1.3913 (0.0040) 119.15 (0.25) C7 1.5085 (0.0035) 120.90 (0.25) 119.93 (0.25) C6 - C1 C5 C7 - Distance Angles N2 1.4763 (0.0033) C6 1.5085 (0.0035) 111.59 (0.21) C7 - N2 C8 - Distance Angles N2 1.4615 (0.0035) C8 - C9 - Distance Angles O1 1.2134 (0.0030) N2 1.3470 (0.0032) 125.64 (0.24) N1 1.4551 (0.0032) 119.28 (0.21) 115.07 (0.22) C9 - O1 N2 C10 - Distance Angles C15 1.3857 (0.0036) C11 1.3890 (0.0039) 119.96 (0.25) N1 1.4463 (0.0032) 119.66 (0.23) 120.33 (0.22) C10 - C15 C11 C11 - Distance Angles C12 1.3815 (0.0041) C10 1.3890 (0.0039) 119.86 (0.26) C11 - C12 C12 - Distance Angles C11 1.3815 (0.0041) C13 1.3883 (0.0046) 120.58 (0.30) C12 - C11 C13 - Distance Angles C14 1.3704 (0.0048) C12 1.3883 (0.0046) 119.34 (0.28) C13 - C14 C14 - Distance Angles C13 1.3704 (0.0048) C15 1.3966 (0.0042) 120.95 (0.28) C14 - C13 C15 - Distance Angles C10 1.3857 (0.0036) C14 1.3966 (0.0042) 119.29 (0.28) C15 - C10 C16 - Distance Angles O2 1.2247 (0.0028) N1 1.3830 (0.0030) 122.06 (0.22) C17 1.5244 (0.0033) 118.32 (0.21) 119.52 (0.20) C16 - O2 N1 C17 - Distance Angles C24 1.5054 (0.0032) C18 1.5128 (0.0033) 117.17 (0.19) C16 1.5244 (0.0033) 115.53 (0.20) 112.38 (0.18) S1 1.8128 (0.0022) 65.28 (0.12) 119.24 (0.17) 119.51 (0.16) C17 - C24 C18 C16 C18 - Distance Angles C19 1.3870 (0.0034) C23 1.3959 (0.0033) 119.56 (0.22) C17 1.5128 (0.0033) 121.44 (0.21) 119.00 (0.21) C18 - C19 C23 C19 - Distance Angles C20 1.3832 (0.0035) C18 1.3870 (0.0034) 120.14 (0.23) C19 - C20 C20 - Distance Angles C19 1.3832 (0.0035) C21 1.3897 (0.0037) 120.56 (0.24) C20 - C19 C21 - Distance Angles C22 1.3878 (0.0040) C20 1.3897 (0.0037) 119.57 (0.24) C21 - C22 C22 - Distance Angles C21 1.3878 (0.0040) C23 1.3906 (0.0036) 120.06 (0.24) C22 - C21 C23 - Distance Angles C22 1.3906 (0.0036) C18 1.3959 (0.0033) 120.11 (0.24) C23 - C22 C24 - Distance Angles C17 1.5054 (0.0032) C25 1.5088 (0.0033) 121.51 (0.21) S1 1.8084 (0.0023) 65.59 (0.12) 118.70 (0.16) C24 - C17 C25 C25 - Distance Angles O3 1.4490 (0.0026) C24 1.5088 (0.0033) 103.74 (0.17) C28 1.5208 (0.0032) 111.03 (0.17) 112.94 (0.19) C25 - O3 C24 C26 - Distance Angles O4 1.2014 (0.0030) O3 1.3581 (0.0029) 124.12 (0.21) C27 1.4934 (0.0034) 126.14 (0.23) 109.73 (0.21) C26 - O4 O3 C27 - Distance Angles C26 1.4934 (0.0034) C27 - C28 - Distance Angles O5 1.4361 (0.0027) C25 1.5208 (0.0032) 109.62 (0.18) C31 1.5277 (0.0032) 106.71 (0.17) 113.06 (0.18) C28 - O5 C25 C29 - Distance Angles O6 1.2031 (0.0031) O5 1.3653 (0.0029) 123.05 (0.22) C30 1.4881 (0.0036) 126.63 (0.22) 110.31 (0.21) C29 - O6 O5 C30 - Distance Angles C29 1.4881 (0.0036) C30 - C31 - Distance Angles O7 1.4417 (0.0028) C34 1.5069 (0.0032) 111.30 (0.18) C28 1.5277 (0.0032) 104.47 (0.17) 114.48 (0.19) C31 - O7 C34 C32 - Distance Angles O8 1.1984 (0.0033) O7 1.3676 (0.0030) 122.73 (0.24) C33 1.4943 (0.0040) 126.27 (0.24) 110.99 (0.24) C32 - O8 O7 C33 - Distance Angles C32 1.4943 (0.0040) C33 - C34 - Distance Angles O9 1.4501 (0.0027) C31 1.5069 (0.0032) 110.24 (0.18) C34 - O9 C35 - Distance Angles O10 1.2079 (0.0029) O9 1.3583 (0.0028) 123.52 (0.21) C36 1.4921 (0.0035) 125.54 (0.21) 110.94 (0.20) C35 - O10 O9 C36 - Distance Angles C35 1.4921 (0.0035) C36 - N1 - Distance Angles C16 1.3830 (0.0030) C10 1.4463 (0.0032) 119.99 (0.20) C9 1.4551 (0.0032) 118.57 (0.19) 117.59 (0.19) N1 - C16 C10 N2 - Distance Angles C9 1.3470 (0.0032) C8 1.4615 (0.0035) 124.58 (0.22) C7 1.4763 (0.0033) 116.89 (0.22) 118.13 (0.21) N2 - C9 C8 O1 - Distance Angles C9 1.2134 (0.0030) O1 - O2 - Distance Angles C16 1.2247 (0.0028) O2 - O3 - Distance Angles C26 1.3581 (0.0029) C25 1.4490 (0.0026) 118.32 (0.17) O3 - C26 O4 - Distance Angles C26 1.2014 (0.0030) O4 - O5 - Distance Angles C29 1.3653 (0.0029) C28 1.4361 (0.0027) 117.09 (0.18) O5 - C29 O6 - Distance Angles C29 1.2031 (0.0031) O6 - O7 - Distance Angles C32 1.3676 (0.0030) C31 1.4417 (0.0028) 115.20 (0.19) O7 - C32 O8 - Distance Angles C32 1.1984 (0.0033) O8 - O9 - Distance Angles C35 1.3583 (0.0028) C34 1.4501 (0.0027) 117.59 (0.18) O9 - C35 O10 - Distance Angles C35 1.2079 (0.0029) O10 - S1 - Distance Angles C24 1.8084 (0.0023) C17 1.8128 (0.0022) 49.13 (0.10) S1 - C24 FMAP and GRID set by program FMAP 2 1 19 GRID -3.125 -2 -2 3.125 2 2 R1 = 0.0354 for 3229 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.17 at 0.3507 0.0509 0.3090 [ 0.01 A from S1 ] Deepest hole -0.24 at 0.2567 0.0476 0.3215 [ 0.80 A from S1 ] Mean = 0.00, Rms deviation from mean = 0.04 e/A^3, Highest memory used = 4532 / 27688 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5717 0.5007 0.6422 1.00000 0.05 0.16 1.19 S1 2.37 C24 2.38 H34A 2.55 H24 Q2 1 0.7771 0.5284 0.5837 1.00000 0.05 0.16 0.84 H24 1.40 C24 2.23 S1 2.42 C25 Q3 1 0.9000 0.8982 0.8774 1.00000 0.05 0.15 0.76 C11 0.90 C12 1.47 H11 1.60 H12 Q4 1 0.7874 0.7245 0.5784 1.00000 0.05 0.15 0.57 C28 0.96 C25 1.36 H28 1.62 H25 Q5 1 0.8548 1.1181 0.6695 1.00000 0.05 0.14 1.05 H33C 1.07 H33A 1.12 C33 1.94 C32 Q6 1 1.4278 0.8316 0.7008 1.00000 0.05 0.14 1.08 H27A 1.61 C27 1.62 H27C 2.13 H8C Q7 1 0.5310 0.6023 0.8024 1.00000 0.05 0.14 1.28 N2 1.56 C9 2.10 C7 2.17 C8 Q8 1 0.4284 0.9835 0.4629 1.00000 0.05 0.13 1.64 O9 1.82 O6 1.91 H34A 2.18 C29 Q9 1 0.8092 1.1810 0.6410 1.00000 0.05 0.13 1.31 H33C 1.77 H36A 1.84 H36C 1.92 C33 Q10 1 0.9910 0.9586 0.8989 1.00000 0.05 0.13 0.34 C12 0.61 H12 1.57 C13 1.59 C11 Q11 1 0.8446 0.7197 0.8605 1.00000 0.05 0.13 0.70 N1 0.75 C10 1.85 C16 1.86 C11 Q12 1 0.6456 0.6407 0.6957 1.00000 0.05 0.13 1.16 S1 1.91 C24 2.12 H25 2.13 C17 Q13 1 0.5598 0.7722 0.4560 1.00000 0.05 0.13 1.38 O9 1.49 H34B 1.51 C34 1.66 C35 Q14 1 0.9410 0.4356 0.7710 1.00000 0.05 0.13 0.60 C18 0.98 C19 1.59 H19 1.76 C17 Q15 1 0.8247 0.8242 0.9774 1.00000 0.05 0.13 0.86 C14 0.96 C15 1.61 H14 1.71 H15 Q16 1 0.3997 0.6368 0.4232 1.00000 0.05 0.13 1.38 O6 1.88 H33C 1.89 C29 2.12 O10 Q17 1 0.7649 0.4570 0.9374 1.00000 0.05 0.12 1.30 O1 2.01 H13 2.27 H4 2.37 C9 Q18 1 0.4983 0.6819 0.7575 1.00000 0.05 0.12 1.58 H8C 1.68 H27C 1.80 C8 1.88 H8B Q19 1 0.1846 0.7637 0.5008 1.00000 0.05 0.12 0.88 H36C 1.27 C36 1.30 H36B 1.87 H27B Q20 1 1.1888 0.4075 0.8334 1.00000 0.05 0.12 1.75 C22 1.87 C23 2.08 H14 2.09 C21 Shortest distances between peaks (including symmetry equivalents) 5 9 1.00 3 10 1.10 7 18 1.30 12 18 1.73 2 8 1.82 1 8 1.84 9 16 1.97 1 2 2.02 1 12 2.09 3 15 2.12 14 20 2.16 7 12 2.19 13 16 2.20 6 18 2.22 3 11 2.36 5 16 2.45 11 15 2.46 2 4 2.54 10 15 2.63 4 12 2.65 9 19 2.69 4 13 2.71 2 12 2.71 16 19 2.79 8 13 2.93 7 11 2.98 Time profile in seconds ----------------------- 0.14: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: Generate connectivity array 0.02: 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. 2.20: 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 4.28: Structure factors and derivatives 8.84: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.08: Apply other restraints 1.28: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.11: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.13: Fourier summations 0.02: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 17:18:19 Total CPU time: 17.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++