+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 15:06:21 on 09-Oct-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 03src0048 in P2(1) CELL 0.71073 8.6737 22.2346 9.8649 90.000 104.924 90.000 ZERR 4.00 0.0002 0.0004 0.0002 0.000 0.001 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N BR O UNIT 68 116 8 4 4 V = 1838.33 F(000) = 752.0 Mu = 2.24 mm-1 Cell Wt = 1429.33 Rho = 1.291 MERG 2 OMIT -3.00 55.00 OMIT -3 21 2 TWIN BASF 0.65754 EXTI 0.00912 BIND C2 C3 DFIX 0.001 1.54 C2 C3 FMAP 2 PLAN 10 SIZE 0.12 0.14 0.48 ACTA BOND $H WGHT 0.02390 2.09270 L.S. 10 TEMP -153.00 FVAR 0.48862 0.64862 PART 1 C1 1 0.994967 0.279168 0.714439 21.00000 0.12189 0.05294 = 0.14189 -0.00274 0.02842 -0.02213 AFIX 137 H1A 2 0.897840 0.274791 0.638019 21.00000 -1.50000 H1B 2 1.076542 0.251242 0.699686 21.00000 -1.50000 H1C 2 0.970956 0.270126 0.804067 21.00000 -1.50000 AFIX 0 C2 1 1.051896 0.338659 0.716664 21.00000 0.06059 0.06995 = 0.07044 -0.01572 0.04005 -0.01563 AFIX 23 H2A 2 1.160907 0.341556 0.779442 21.00000 -1.20000 H2B 2 1.055614 0.351129 0.621218 21.00000 -1.20000 AFIX 0 PART 2 C1' 1 1.038984 0.309380 0.629862 -21.00000 0.12353 0.06298 = 0.06408 -0.02046 0.04846 -0.01641 AFIX 137 H1'1 2 1.138262 0.332650 0.650394 -21.00000 -1.50000 H1'2 2 1.060819 0.267859 0.607114 -21.00000 -1.50000 H1'3 2 0.961653 0.327399 0.549878 -21.00000 -1.50000 AFIX 0 C2' 1 0.969668 0.309745 0.759998 -21.00000 0.07695 0.04359 = 0.07841 -0.01216 0.03547 -0.02784 AFIX 23 H2'1 2 0.871296 0.285254 0.743973 -21.00000 -1.20000 H2'2 2 1.048460 0.294941 0.844748 -21.00000 -1.20000 AFIX 0 PART 0 C3 1 0.932121 0.381202 0.772679 11.00000 0.12287 0.07800 = 0.06222 -0.01868 0.02269 0.05002 AFIX 23 H3A 2 0.906939 0.364255 0.857280 11.00000 -1.20000 H3B 2 0.831801 0.388351 0.699491 11.00000 -1.20000 AFIX 0 C4 1 1.027936 0.435988 0.805099 11.00000 0.04842 0.13504 = 0.03095 -0.02167 0.01219 0.01777 AFIX 23 H4A 2 1.122489 0.427369 0.883438 11.00000 -1.20000 H4B 2 1.066741 0.446941 0.722371 11.00000 -1.20000 AFIX 0 C5 1 0.942842 0.488029 0.843755 11.00000 0.03430 0.07806 = 0.01954 0.00331 0.00725 -0.01458 AFIX 23 H5A 2 0.851360 0.498231 0.763864 11.00000 -1.20000 H5B 2 1.015617 0.523093 0.861759 11.00000 -1.20000 AFIX 0 C6 1 0.734461 0.469812 0.970327 11.00000 0.02309 0.03310 = 0.02579 0.00123 0.00182 0.00055 AFIX 43 H6 2 0.646264 0.471981 0.890063 11.00000 -1.20000 AFIX 0 C7 1 0.978379 0.470851 1.104979 11.00000 0.02183 0.02561 = 0.02028 0.00357 0.00273 0.00083 C8 1 1.141757 0.476287 1.159914 11.00000 0.02079 0.03682 = 0.02729 0.00222 0.00509 -0.00126 AFIX 43 H8 2 1.211322 0.485302 1.102401 11.00000 -1.20000 AFIX 0 C9 1 1.197665 0.467901 1.302423 11.00000 0.02160 0.03988 = 0.02784 0.00223 -0.00106 0.00174 AFIX 43 H9 2 1.308950 0.470787 1.344728 11.00000 -1.20000 AFIX 0 C10 1 1.093189 0.455140 1.386632 11.00000 0.03376 0.04205 = 0.02078 0.00059 0.00236 0.00574 AFIX 43 H10 2 1.135988 0.449143 1.484465 11.00000 -1.20000 AFIX 0 C11 1 0.931403 0.451110 1.331582 11.00000 0.03628 0.03520 = 0.02214 0.00044 0.00997 0.00227 AFIX 43 H11 2 0.860995 0.443287 1.389020 11.00000 -1.20000 AFIX 0 C12 1 0.875609 0.459051 1.187460 11.00000 0.02283 0.02413 = 0.02430 0.00090 0.00687 0.00248 C13 1 0.572844 0.450200 1.140625 11.00000 0.02404 0.04578 = 0.03295 -0.00076 0.00964 0.00504 AFIX 23 H13A 2 0.581503 0.470455 1.231653 11.00000 -1.20000 H13B 2 0.484633 0.469548 1.070122 11.00000 -1.20000 AFIX 0 C14 1 0.532002 0.385144 1.153981 11.00000 0.03669 0.04439 = 0.04396 0.00385 0.01746 0.00018 AFIX 23 H14A 2 0.622755 0.365195 1.220407 11.00000 -1.20000 H14B 2 0.438540 0.382669 1.193932 11.00000 -1.20000 AFIX 0 C15 1 0.494437 0.351317 1.014749 11.00000 0.06813 0.05024 = 0.05542 -0.00139 0.02524 -0.01318 AFIX 23 H15A 2 0.423020 0.376297 0.941833 11.00000 -1.20000 H15B 2 0.594673 0.344918 0.986347 11.00000 -1.20000 AFIX 0 C16 1 0.413976 0.289692 1.022326 11.00000 0.08188 0.05998 = 0.07291 -0.01370 0.02236 -0.01187 AFIX 23 H16A 2 0.379504 0.272498 0.926704 11.00000 -1.20000 H16B 2 0.317489 0.295869 1.056671 11.00000 -1.20000 AFIX 0 C17 1 0.517873 0.247159 1.113212 11.00000 0.15005 0.06177 = 0.07673 0.00482 0.01085 0.00082 AFIX 137 H17A 2 0.559292 0.265121 1.206207 11.00000 -1.50000 H17B 2 0.457693 0.210653 1.121596 11.00000 -1.50000 H17C 2 0.606992 0.236901 1.073380 11.00000 -1.50000 AFIX 0 C18 1 1.526428 0.833229 1.508373 11.00000 0.11167 0.04598 = 0.05467 -0.01004 0.01110 -0.00378 AFIX 137 H18A 2 1.605383 0.814236 1.585721 11.00000 -1.50000 H18B 2 1.562545 0.873754 1.492372 11.00000 -1.50000 H18C 2 1.423776 0.835795 1.532346 11.00000 -1.50000 AFIX 0 C19 1 1.507340 0.796200 1.377261 11.00000 0.08162 0.04280 = 0.04980 -0.00484 0.02761 -0.01234 AFIX 23 H19A 2 1.609343 0.796257 1.349750 11.00000 -1.20000 H19B 2 1.425263 0.815003 1.300257 11.00000 -1.20000 AFIX 0 C20 1 1.459767 0.732219 1.395677 11.00000 0.03507 0.04656 = 0.03635 0.00106 0.01114 0.00406 AFIX 23 H20A 2 1.546172 0.712496 1.467264 11.00000 -1.20000 H20B 2 1.362886 0.732344 1.431154 11.00000 -1.20000 AFIX 0 C21 1 1.426689 0.695623 1.260954 11.00000 0.02894 0.04626 = 0.03501 0.00030 0.01603 0.00027 AFIX 23 H21A 2 1.521161 0.697803 1.222303 11.00000 -1.20000 H21B 2 1.335820 0.714004 1.191442 11.00000 -1.20000 AFIX 0 C22 1 1.389020 0.630742 1.279462 11.00000 0.02109 0.04079 = 0.03775 -0.00570 0.01215 0.00028 AFIX 23 H22A 2 1.477269 0.612629 1.352200 11.00000 -1.20000 H22B 2 1.381569 0.609028 1.190391 11.00000 -1.20000 AFIX 0 C23 1 1.227119 0.613481 1.449809 11.00000 0.02561 0.03182 = 0.02414 0.00067 -0.00115 -0.00247 AFIX 43 H23 2 1.314745 0.611380 1.530554 11.00000 -1.20000 AFIX 0 C24 1 1.087486 0.623816 1.230760 11.00000 0.02427 0.02743 = 0.02538 0.00106 0.00571 0.00381 C25 1 1.032447 0.631418 1.086612 11.00000 0.03291 0.03965 = 0.02311 0.00338 0.01043 0.00496 AFIX 43 H25 2 1.102957 0.638853 1.029063 11.00000 -1.20000 AFIX 0 C26 1 0.870875 0.627588 1.032235 11.00000 0.04218 0.04210 = 0.02008 -0.00033 0.00428 0.00763 AFIX 43 H26 2 0.828963 0.633191 0.934164 11.00000 -1.20000 AFIX 0 C27 1 0.764635 0.615844 1.113882 11.00000 0.02441 0.03692 = 0.02958 -0.00404 0.00044 0.00205 AFIX 43 H27 2 0.653656 0.612928 1.070290 11.00000 -1.20000 AFIX 0 C28 1 0.819179 0.608381 1.257884 11.00000 0.02781 0.03679 = 0.02631 -0.00302 0.00618 0.00005 AFIX 43 H28 2 0.748493 0.600216 1.314876 11.00000 -1.20000 AFIX 0 C29 1 0.981036 0.613439 1.313658 11.00000 0.02768 0.02924 = 0.02055 0.00036 0.00503 -0.00258 C30 1 1.014058 0.596184 1.573834 11.00000 0.03713 0.06047 = 0.02257 0.00339 0.00679 -0.01281 AFIX 23 H30A 2 0.936735 0.562554 1.553098 11.00000 -1.20000 H30B 2 1.103168 0.584055 1.653950 11.00000 -1.20000 AFIX 0 C31 1 0.934363 0.650304 1.613773 11.00000 0.04869 0.11699 = 0.02279 -0.00485 0.01079 0.01880 AFIX 23 H31A 2 0.875813 0.637909 1.683077 11.00000 -1.20000 H31B 2 0.854449 0.664826 1.529418 11.00000 -1.20000 AFIX 0 C32 1 1.040174 0.701264 1.673593 11.00000 0.11626 0.07253 = 0.06266 -0.02426 -0.03101 0.04798 AFIX 23 H32A 2 1.121766 0.687525 1.757697 11.00000 -1.20000 H32B 2 1.095928 0.715642 1.603893 11.00000 -1.20000 AFIX 0 C33 1 0.944224 0.752905 1.713815 11.00000 0.25935 0.13934 = 0.13594 -0.06224 -0.06525 0.14287 AFIX 23 H33A 2 0.853239 0.734091 1.741147 11.00000 -1.20000 H33B 2 0.898234 0.775504 1.626264 11.00000 -1.20000 AFIX 0 C34 1 1.000553 0.791795 1.806615 11.00000 0.20333 0.10396 = 0.13297 -0.04622 0.03547 0.06330 AFIX 137 H34A 2 1.068612 0.819737 1.771438 11.00000 -1.50000 H34B 2 0.912918 0.814080 1.829228 11.00000 -1.50000 H34C 2 1.063850 0.771755 1.891209 11.00000 -1.50000 AFIX 0 N1 3 0.884506 0.476894 0.967658 11.00000 0.02164 0.03798 = 0.02201 0.00264 0.00275 -0.00275 N2 3 0.722545 0.459292 1.099241 11.00000 0.02145 0.02876 = 0.02617 -0.00125 0.00279 0.00174 N3 3 1.239667 0.623050 1.320265 11.00000 0.02537 0.03079 = 0.02505 -0.00164 0.00554 -0.00032 N4 3 1.075927 0.607278 1.450991 11.00000 0.02784 0.03447 = 0.01911 0.00062 0.00133 -0.00342 BR1 4 0.622932 0.509158 0.511721 11.00000 0.02865 0.05351 = 0.02736 -0.00180 0.00679 -0.00289 O1 5 0.402316 0.454320 0.714577 11.00000 0.06382 0.05498 = 0.04273 -0.00389 0.02341 -0.00464 O2 5 1.560975 0.623525 1.701078 11.00000 0.06486 0.06056 = 0.04672 -0.00775 0.02761 -0.00931 H1O 2 0.459212 0.469584 0.642694 11.00000 0.06680 H2O 2 0.377772 0.481618 0.743106 11.00000 0.05045 H3O 2 1.588533 0.593201 1.652734 11.00000 0.06148 H4O 2 1.512220 0.609793 1.767753 11.00000 0.09048 MOLE 2 BR2 4 0.340405 0.570763 0.905780 11.00000 0.02898 0.05036 = 0.02697 0.00020 0.00705 -0.00080 HKLF 4 Covalent radii and connectivity table for 03src0048 in P2(1) C 0.770 H 0.320 N 0.700 BR 1.140 O 0.660 C1_a - C2_a C2_a - C1_a C3 C1'_b - C2'_b C2'_b - C1'_b C3 C3 - C4 C2_a C2'_b C4 - C3 C5 C5 - N1 C4 C6 - N1 N2 C7 - C12 C8 N1 C8 - C9 C7 C9 - C8 C10 C10 - C11 C9 C11 - C10 C12 C12 - C7 N2 C11 C13 - N2 C14 C14 - C13 C15 C15 - C14 C16 C16 - C17 C15 C17 - C16 C18 - C19 C19 - C20 C18 C20 - C19 C21 C21 - C22 C20 C22 - N3 C21 C23 - N4 N3 C24 - N3 C25 C29 C25 - C26 C24 C26 - C25 C27 C27 - C28 C26 C28 - C29 C27 C29 - C28 N4 C24 C30 - N4 C31 C31 - C32 C30 C32 - C31 C33 C33 - C34 C32 C34 - C33 N1 - C6 C7 C5 N2 - C6 C12 C13 N3 - C23 C24 C22 N4 - C23 C29 C30 Br1 - no bonds found O1 - no bonds found O2 - no bonds found Br2 - no bonds found Floating origin restraints generated 14283 Reflections read, of which 24 rejected -10 =< h =< 11, -28 =< k =< 26, -12 =< l =< 12, Max. 2-theta = 54.95 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 2 -8 0 66.10 1.38 3 7.27 6 -14 2 82.71 2.79 3 14.29 -7 -13 2 22.29 2.02 2 10.34 4 -12 2 157.31 4.83 2 24.99 5 -9 2 192.96 5.46 2 30.50 7 -5 3 22.39 0.81 3 5.96 -7 0 3 4.46 0.81 3 4.89 -7 9 3 24.19 1.65 2 8.40 5 -12 4 63.39 2.88 2 19.55 6 -11 4 78.66 3.70 2 20.15 7 -3 4 26.59 1.17 2 7.67 -8 1 4 11.24 1.01 3 5.13 -8 0 5 36.28 1.85 3 10.66 13 Inconsistent equivalents 7353 Unique reflections, of which 0 suppressed R(int) = 0.0410 R(sigma) = 0.0487 Friedel opposites not merged Maximum memory for data reduction = 4865 / 74189 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 = 6189 / 543952 wR2 = 0.0958 before cycle 1 for 7353 data and 421 / 421 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 1.540 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 1.604 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.112; Restrained GooF = 1.111 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0239 * P )^2 + 2.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 Shifts scaled down to reduce maximum shift/su from 29.68 to 15.00 N value su shift/su parameter 1 0.48853 0.00071 -0.126 OSF 2 0.64959 0.01941 0.050 FVAR 2 3 0.53808 0.01062 -11.250 BASF 1 4 0.00913 0.00067 0.015 EXTI Mean shift/su = 0.052 Maximum = -11.250 for BASF 1 Max. shift = 0.004 A for H4O Max. dU =-0.002 for H3O Least-squares cycle 2 Maximum vector length = 511 Memory required = 6189 / 543952 wR2 = 0.0920 before cycle 2 for 7353 data and 421 / 421 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 1.540 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 1.603 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.066; Restrained GooF = 1.066 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0239 * P )^2 + 2.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 Shifts scaled down to reduce maximum shift/su from 19.20 to 15.00 N value su shift/su parameter 1 0.48863 0.00068 0.139 OSF 2 0.65037 0.01859 0.042 FVAR 2 3 0.38545 0.01018 -15.000 BASF 1 4 0.00914 0.00064 0.013 EXTI Mean shift/su = 0.050 Maximum = -15.000 for BASF 1 Max. shift = 0.003 A for H2O Max. dU =-0.001 for H3O Least-squares cycle 3 Maximum vector length = 511 Memory required = 6189 / 543952 wR2 = 0.0896 before cycle 3 for 7353 data and 421 / 421 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 1.540 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 1.603 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.039; Restrained GooF = 1.039 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0239 * P )^2 + 2.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.48864 0.00066 0.022 OSF 2 0.65006 0.01807 -0.017 FVAR 2 3 0.34278 0.00989 -4.313 BASF 1 4 0.00914 0.00063 -0.001 EXTI Mean shift/su = 0.029 Maximum = -4.313 for BASF 1 Max. shift = 0.003 A for H1O Max. dU = 0.001 for H3O Least-squares cycle 4 Maximum vector length = 511 Memory required = 6189 / 543952 wR2 = 0.0895 before cycle 4 for 7353 data and 421 / 421 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 1.540 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 1.604 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.037 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0239 * P )^2 + 2.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.48864 0.00066 0.000 OSF 2 0.64942 0.01805 -0.036 FVAR 2 3 0.34260 0.00987 -0.019 BASF 1 4 0.00914 0.00062 -0.003 EXTI Mean shift/su = 0.020 Maximum = -0.078 for U13 O2 Max. shift = 0.003 A for H1O Max. dU = 0.001 for H3O Least-squares cycle 5 Maximum vector length = 511 Memory required = 6189 / 543952 wR2 = 0.0895 before cycle 5 for 7353 data and 421 / 421 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 1.540 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 1.604 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.037 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0239 * P )^2 + 2.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.48864 0.00066 -0.006 OSF 2 0.64919 0.01809 -0.013 FVAR 2 3 0.34241 0.00987 -0.019 BASF 1 4 0.00913 0.00062 -0.003 EXTI Mean shift/su = 0.003 Maximum = 0.029 for U11 H3O Max. shift = 0.001 A for H3O Max. dU = 0.001 for H3O Least-squares cycle 6 Maximum vector length = 511 Memory required = 6189 / 543952 wR2 = 0.0895 before cycle 6 for 7353 data and 421 / 421 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 1.540 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 1.604 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.037 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0239 * P )^2 + 2.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.48864 0.00066 0.002 OSF 2 0.64911 0.01811 -0.004 FVAR 2 3 0.34240 0.00987 -0.001 BASF 1 4 0.00913 0.00062 0.001 EXTI Mean shift/su = 0.001 Maximum = -0.016 for z H3O Max. shift = 0.001 A for H3O Max. dU = 0.000 for H3O Least-squares cycle 7 Maximum vector length = 511 Memory required = 6189 / 543952 wR2 = 0.0895 before cycle 7 for 7353 data and 421 / 421 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 1.540 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 1.604 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.037 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0239 * P )^2 + 2.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.48864 0.00066 0.001 OSF 2 0.64904 0.01811 -0.004 FVAR 2 3 0.34240 0.00987 0.000 BASF 1 4 0.00914 0.00062 0.001 EXTI Mean shift/su = 0.001 Maximum = 0.011 for U11 H3O Max. shift = 0.001 A for H3O Max. dU = 0.000 for H3O Least-squares cycle 8 Maximum vector length = 511 Memory required = 6189 / 543952 wR2 = 0.0895 before cycle 8 for 7353 data and 421 / 421 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 1.540 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 1.604 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.037 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0239 * P )^2 + 2.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.48864 0.00066 -0.001 OSF 2 0.64900 0.01812 -0.002 FVAR 2 3 0.34240 0.00987 0.000 BASF 1 4 0.00913 0.00062 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.007 for U11 H3O Max. shift = 0.001 A for H3O Max. dU = 0.000 for H3O Least-squares cycle 9 Maximum vector length = 511 Memory required = 6189 / 543952 wR2 = 0.0895 before cycle 9 for 7353 data and 421 / 421 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 1.540 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 1.604 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.037 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0239 * P )^2 + 2.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.48864 0.00066 0.000 OSF 2 0.64898 0.01812 -0.001 FVAR 2 3 0.34239 0.00987 0.000 BASF 1 4 0.00913 0.00062 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.005 for U11 H3O Max. shift = 0.000 A for H3O Max. dU = 0.000 for H3O Least-squares cycle 10 Maximum vector length = 511 Memory required = 6189 / 543952 wR2 = 0.0895 before cycle 10 for 7353 data and 421 / 421 parameters Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 1.540 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 1.604 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.037 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0239 * P )^2 + 2.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.48864 0.00066 -0.001 OSF 2 0.64896 0.01812 -0.001 FVAR 2 3 0.34239 0.00987 0.000 BASF 1 4 0.00913 0.00062 -0.001 EXTI Mean shift/su = 0.000 Maximum = 0.003 for U11 H3O Max. shift = 0.000 A for H3O Max. dU = 0.000 for H3O Largest correlation matrix elements 0.692 U12 C33 / U22 C33 0.631 U13 C33 / U23 C33 0.554 U13 C1'_b / U11 C1'_b 0.687 U12 C33 / U11 C33 0.592 U13 C2_a / U11 C2_a 0.528 U13 C2_a / U33 C2_a 0.659 EXTI / OSF 0.568 y C33 / x C33 Idealized hydrogen atom generation before cycle 11 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.8978 0.2748 0.6381 137 0.980 0.000 C1_a C2_a H1A_a H1B 0.9709 0.2702 0.8041 137 0.980 0.000 C1_a C2_a H1A_a H1C 1.0765 0.2513 0.6997 137 0.980 0.000 C1_a C2_a H1A_a H2A 1.0556 0.3511 0.6212 23 0.990 0.000 C2_a C1_a C3 H2B 1.1609 0.3415 0.7795 23 0.990 0.000 C2_a C1_a C3 H1'1 1.1383 0.3326 0.6504 137 0.980 0.000 C1'_b C2'_b H1'1_b H1'2 0.9617 0.3274 0.5499 137 0.980 0.000 C1'_b C2'_b H1'1_b H1'3 1.0608 0.2678 0.6071 137 0.980 0.000 C1'_b C2'_b H1'1_b H2'1 1.0484 0.2949 0.8447 23 0.990 0.000 C2'_b C1'_b C3 H2'2 0.8713 0.2853 0.7440 23 0.990 0.000 C2'_b C1'_b C3 H3A 0.8318 0.3884 0.6995 23 0.990 0.000 C3 C4 C2_a H3B 0.9069 0.3643 0.8573 23 0.990 0.000 C3 C4 C2_a H4A 1.0667 0.4469 0.7224 23 0.990 0.000 C4 C3 C5 H4B 1.1225 0.4274 0.8834 23 0.990 0.000 C4 C3 C5 H5A 1.0156 0.5231 0.8618 23 0.990 0.000 C5 N1 C4 H5B 0.8514 0.4982 0.7639 23 0.990 0.000 C5 N1 C4 H6 0.6463 0.4720 0.8901 43 0.950 0.000 C6 N1 N2 H8 1.2113 0.4853 1.1024 43 0.950 0.000 C8 C9 C7 H9 1.3089 0.4708 1.3447 43 0.950 0.000 C9 C8 C10 H10 1.1360 0.4491 1.4845 43 0.950 0.000 C10 C11 C9 H11 0.8610 0.4433 1.3890 43 0.950 0.000 C11 C10 C12 H13A 0.4846 0.4695 1.0701 23 0.990 0.000 C13 N2 C14 H13B 0.5815 0.4705 1.2317 23 0.990 0.000 C13 N2 C14 H14A 0.4385 0.3827 1.1939 23 0.990 0.000 C14 C13 C15 H14B 0.6228 0.3652 1.2204 23 0.990 0.000 C14 C13 C15 H15A 0.5947 0.3449 0.9864 23 0.990 0.000 C15 C14 C16 H15B 0.4230 0.3763 0.9419 23 0.990 0.000 C15 C14 C16 H16A 0.3175 0.2959 1.0567 23 0.990 0.000 C16 C17 C15 H16B 0.3795 0.2725 0.9267 23 0.990 0.000 C16 C17 C15 H17A 0.5592 0.2651 1.2062 137 0.980 0.000 C17 C16 H17A H17B 0.6070 0.2369 1.0734 137 0.980 0.000 C17 C16 H17A H17C 0.4577 0.2106 1.1215 137 0.980 0.000 C17 C16 H17A H18A 1.6055 0.8143 1.5857 137 0.980 0.000 C18 C19 H18A H18B 1.4238 0.8357 1.5324 137 0.980 0.000 C18 C19 H18A H18C 1.5624 0.8738 1.4923 137 0.980 0.000 C18 C19 H18A H19A 1.4253 0.8150 1.3003 23 0.990 0.000 C19 C20 C18 H19B 1.6093 0.7963 1.3497 23 0.990 0.000 C19 C20 C18 H20A 1.3629 0.7323 1.4312 23 0.990 0.000 C20 C19 C21 H20B 1.5462 0.7125 1.4673 23 0.990 0.000 C20 C19 C21 H21A 1.3358 0.7140 1.1914 23 0.990 0.000 C21 C22 C20 H21B 1.5211 0.6978 1.2223 23 0.990 0.000 C21 C22 C20 H22A 1.3816 0.6090 1.1904 23 0.990 0.000 C22 N3 C21 H22B 1.4773 0.6126 1.3522 23 0.990 0.000 C22 N3 C21 H23 1.3147 0.6114 1.5305 43 0.950 0.000 C23 N4 N3 H25 1.1030 0.6389 1.0291 43 0.950 0.000 C25 C26 C24 H26 0.8290 0.6332 0.9342 43 0.950 0.000 C26 C25 C27 H27 0.6537 0.6129 1.0703 43 0.950 0.000 C27 C28 C26 H28 0.7485 0.6002 1.3149 43 0.950 0.000 C28 C29 C27 H30A 1.1032 0.5841 1.6539 23 0.990 0.000 C30 N4 C31 H30B 0.9367 0.5626 1.5531 23 0.990 0.000 C30 N4 C31 H31A 0.8544 0.6648 1.5294 23 0.990 0.000 C31 C32 C30 H31B 0.8758 0.6379 1.6831 23 0.990 0.000 C31 C32 C30 H32A 1.0959 0.7156 1.6039 23 0.990 0.000 C32 C31 C33 H32B 1.1217 0.6875 1.7577 23 0.990 0.000 C32 C31 C33 H33A 0.8984 0.7755 1.6262 23 0.990 0.000 C33 C34 C32 H33B 0.8532 0.7341 1.7410 23 0.990 0.000 C33 C34 C32 H34A 1.0687 0.8197 1.7716 137 0.980 0.000 C34 C33 H34A H34B 1.0636 0.7717 1.8912 137 0.980 0.000 C34 C33 H34A H34C 0.9128 0.8141 1.8291 137 0.980 0.000 C34 C33 H34A 03src0048 in P2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1_a 0.99496 0.27919 0.71448 0.64896 0.12210 0.05287 0.14186 -0.00272 0.02826 -0.02226 0.10666 0.03093 0.00198 0.00069 0.00205 0.01812 0.01177 0.00935 0.01552 0.00865 0.01030 0.00807 0.00574 H1A_a 0.89783 0.27481 0.63806 0.64896 0.15999 0.01812 0.00000 H1B_a 0.97094 0.27016 0.80411 0.64896 0.15999 0.01812 0.00000 H1C_a 1.07652 0.25125 0.69974 0.64896 0.15999 0.01812 0.00000 C2_a 1.05190 0.33865 0.71667 0.64896 0.06056 0.06985 0.07051 -0.01572 0.04004 -0.01562 0.06271 0.02033 0.00113 0.00046 0.00114 0.01812 0.00564 0.00701 0.00670 0.00512 0.00485 0.00460 0.00341 H2A_a 1.05563 0.35111 0.62123 0.64896 0.07525 0.01812 0.00000 H2B_a 1.16090 0.34155 0.77946 0.64896 0.07525 0.01812 0.00000 C1'_b 1.03897 0.30937 0.62988 0.35104 0.12359 0.06288 0.06400 -0.02042 0.04845 -0.01661 0.07902 0.04149 0.00274 0.00099 0.00221 0.01812 0.01749 0.01376 0.01245 0.01002 0.01156 0.01133 0.00715 H1'1_b 1.13827 0.33263 0.65042 0.35104 0.11853 0.01812 0.00000 H1'2_b 0.96166 0.32740 0.54989 0.35104 0.11853 0.01812 0.00000 H1'3_b 1.06078 0.26785 0.60713 0.35104 0.11853 0.01812 0.00000 C2'_b 0.96965 0.30975 0.75999 0.35104 0.07698 0.04347 0.07866 -0.01223 0.03562 -0.02784 0.06351 0.03831 0.00250 0.00096 0.00225 0.01812 0.01224 0.01279 0.01270 0.00941 0.00982 0.00993 0.00592 H2'1_b 1.04844 0.29495 0.84475 0.35104 0.07621 0.01812 0.00000 H2'2_b 0.87128 0.28526 0.74397 0.35104 0.07621 0.01812 0.00000 C3 0.93211 0.38121 0.77267 1.00000 0.12282 0.07794 0.06220 -0.01873 0.02270 0.04993 0.08786 0.01601 0.00102 0.00034 0.00074 0.00000 0.00648 0.00516 0.00404 0.00354 0.00402 0.00478 0.00256 H3A_a 0.83181 0.38836 0.69946 1.00000 0.10543 0.00000 0.00000 H3B_a 0.90690 0.36427 0.85726 1.00000 0.10543 0.00000 0.00000 C4 1.02792 0.43598 0.80509 1.00000 0.04846 0.13498 0.03094 -0.02164 0.01221 0.01782 0.07110 0.01182 0.00067 0.00035 0.00053 0.00000 0.00322 0.00651 0.00260 0.00323 0.00229 0.00360 0.00205 H4A 1.06674 0.44693 0.72237 1.00000 0.08532 0.00000 0.00000 H4B 1.12247 0.42735 0.88344 1.00000 0.08532 0.00000 0.00000 C5 0.94284 0.48803 0.84375 1.00000 0.03428 0.07813 0.01954 0.00332 0.00725 -0.01458 0.04392 0.00899 0.00055 0.00025 0.00042 0.00000 0.00232 0.00392 0.00188 0.00199 0.00164 0.00227 0.00130 H5A 1.01564 0.52309 0.86177 1.00000 0.05271 0.00000 0.00000 H5B 0.85137 0.49824 0.76386 1.00000 0.05271 0.00000 0.00000 C6 0.73446 0.46981 0.97033 1.00000 0.02308 0.03310 0.02577 0.00124 0.00180 0.00055 0.02814 0.00776 0.00047 0.00019 0.00041 0.00000 0.00204 0.00240 0.00197 0.00166 0.00155 0.00170 0.00088 H6 0.64626 0.47198 0.89006 1.00000 0.03377 0.00000 0.00000 C7 0.97839 0.47085 1.10498 1.00000 0.02184 0.02560 0.02027 0.00356 0.00273 0.00082 0.02306 0.00738 0.00044 0.00018 0.00039 0.00000 0.00189 0.00218 0.00175 0.00149 0.00142 0.00155 0.00082 C8 1.14175 0.47629 1.15991 1.00000 0.02080 0.03682 0.02730 0.00222 0.00510 -0.00126 0.02851 0.00754 0.00045 0.00019 0.00040 0.00000 0.00192 0.00246 0.00192 0.00169 0.00149 0.00167 0.00088 H8 1.21132 0.48530 1.10240 1.00000 0.03421 0.00000 0.00000 C9 1.19766 0.46790 1.30243 1.00000 0.02158 0.03991 0.02782 0.00223 -0.00107 0.00174 0.03113 0.00823 0.00049 0.00021 0.00043 0.00000 0.00205 0.00273 0.00204 0.00181 0.00158 0.00182 0.00097 H9 1.30894 0.47079 1.34473 1.00000 0.03736 0.00000 0.00000 C10 1.09318 0.45514 1.38663 1.00000 0.03381 0.04202 0.02077 0.00059 0.00237 0.00576 0.03306 0.00796 0.00049 0.00021 0.00040 0.00000 0.00227 0.00259 0.00180 0.00169 0.00157 0.00191 0.00093 H10 1.13598 0.44914 1.48446 1.00000 0.03967 0.00000 0.00000 C11 0.93141 0.45111 1.33158 1.00000 0.03627 0.03517 0.02214 0.00044 0.00995 0.00226 0.03075 0.00848 0.00054 0.00022 0.00043 0.00000 0.00238 0.00261 0.00191 0.00174 0.00171 0.00197 0.00097 H11 0.86101 0.44329 1.38902 1.00000 0.03689 0.00000 0.00000 C12 0.87561 0.45905 1.18746 1.00000 0.02284 0.02412 0.02429 0.00089 0.00686 0.00249 0.02360 0.00752 0.00044 0.00018 0.00040 0.00000 0.00197 0.00207 0.00182 0.00154 0.00149 0.00158 0.00079 C13 0.57285 0.45020 1.14063 1.00000 0.02401 0.04577 0.03296 -0.00076 0.00964 0.00504 0.03382 0.00838 0.00047 0.00021 0.00043 0.00000 0.00204 0.00275 0.00214 0.00190 0.00164 0.00185 0.00095 H13A 0.48463 0.46955 1.07013 1.00000 0.04059 0.00000 0.00000 H13B 0.58151 0.47045 1.23166 1.00000 0.04059 0.00000 0.00000 C14 0.53201 0.38515 1.15398 1.00000 0.03668 0.04441 0.04399 0.00384 0.01746 0.00018 0.04039 0.00919 0.00055 0.00022 0.00049 0.00000 0.00252 0.00293 0.00260 0.00208 0.00204 0.00206 0.00108 H14A 0.43854 0.38267 1.19392 1.00000 0.04847 0.00000 0.00000 H14B 0.62276 0.36520 1.22041 1.00000 0.04847 0.00000 0.00000 C15 0.49446 0.35132 1.01478 1.00000 0.06824 0.05023 0.05545 -0.00141 0.02531 -0.01323 0.05625 0.01079 0.00073 0.00025 0.00059 0.00000 0.00369 0.00327 0.00312 0.00261 0.00274 0.00274 0.00138 H15A 0.59470 0.34492 0.98638 1.00000 0.06750 0.00000 0.00000 H15B 0.42304 0.37630 0.94186 1.00000 0.06750 0.00000 0.00000 C16 0.41399 0.28969 1.02235 1.00000 0.08200 0.05999 0.07295 -0.01370 0.02240 -0.01187 0.07120 0.01247 0.00083 0.00029 0.00072 0.00000 0.00455 0.00399 0.00405 0.00312 0.00343 0.00332 0.00173 H16A 0.31750 0.29586 1.05669 1.00000 0.08544 0.00000 0.00000 H16B 0.37953 0.27249 0.92673 1.00000 0.08544 0.00000 0.00000 C17 0.51786 0.24717 1.11322 1.00000 0.15021 0.06174 0.07673 0.00484 0.01076 0.00080 0.09962 0.01582 0.00117 0.00033 0.00081 0.00000 0.00783 0.00476 0.00481 0.00374 0.00480 0.00468 0.00265 H17A 0.55919 0.26512 1.20624 1.00000 0.14943 0.00000 0.00000 H17B 0.60704 0.23694 1.07344 1.00000 0.14943 0.00000 0.00000 H17C 0.45771 0.21065 1.12153 1.00000 0.14943 0.00000 0.00000 C18 1.52643 0.83323 1.50837 1.00000 0.11165 0.04598 0.05463 -0.01003 0.01107 -0.00379 0.07266 0.01155 0.00094 0.00027 0.00065 0.00000 0.00561 0.00368 0.00336 0.00273 0.00333 0.00344 0.00186 H18A 1.60550 0.81427 1.58568 1.00000 0.10899 0.00000 0.00000 H18B 1.42381 0.83575 1.53242 1.00000 0.10899 0.00000 0.00000 H18C 1.56239 0.87377 1.49232 1.00000 0.10899 0.00000 0.00000 C19 1.50733 0.79620 1.37726 1.00000 0.08166 0.04278 0.04983 -0.00486 0.02765 -0.01234 0.05612 0.01068 0.00075 0.00024 0.00056 0.00000 0.00400 0.00305 0.00295 0.00235 0.00273 0.00272 0.00138 H19A 1.42525 0.81500 1.30026 1.00000 0.06734 0.00000 0.00000 H19B 1.60934 0.79626 1.34974 1.00000 0.06734 0.00000 0.00000 C20 1.45977 0.73222 1.39567 1.00000 0.03505 0.04655 0.03638 0.00105 0.01114 0.00405 0.03897 0.00891 0.00055 0.00022 0.00046 0.00000 0.00242 0.00289 0.00232 0.00201 0.00185 0.00206 0.00103 H20A 1.36289 0.73234 1.43115 1.00000 0.04676 0.00000 0.00000 H20B 1.54617 0.71250 1.46726 1.00000 0.04676 0.00000 0.00000 C21 1.42668 0.69562 1.26096 1.00000 0.02892 0.04627 0.03500 0.00033 0.01602 0.00028 0.03530 0.00850 0.00050 0.00021 0.00044 0.00000 0.00218 0.00283 0.00219 0.00193 0.00175 0.00191 0.00098 H21A 1.33581 0.71400 1.19145 1.00000 0.04236 0.00000 0.00000 H21B 1.52115 0.69780 1.22230 1.00000 0.04236 0.00000 0.00000 C22 1.38902 0.63074 1.27946 1.00000 0.02110 0.04083 0.03773 -0.00570 0.01215 0.00031 0.03238 0.00805 0.00045 0.00021 0.00044 0.00000 0.00194 0.00259 0.00218 0.00190 0.00163 0.00180 0.00092 H22A 1.38158 0.60903 1.19039 1.00000 0.03885 0.00000 0.00000 H22B 1.47727 0.61263 1.35220 1.00000 0.03885 0.00000 0.00000 C23 1.22711 0.61348 1.44980 1.00000 0.02561 0.03182 0.02413 0.00067 -0.00114 -0.00247 0.02858 0.00793 0.00051 0.00019 0.00042 0.00000 0.00217 0.00241 0.00192 0.00168 0.00159 0.00179 0.00091 H23 1.31474 0.61137 1.53055 1.00000 0.03429 0.00000 0.00000 C24 1.08749 0.62382 1.23076 1.00000 0.02427 0.02743 0.02537 0.00107 0.00571 0.00382 0.02581 0.00800 0.00048 0.00020 0.00042 0.00000 0.00205 0.00232 0.00189 0.00167 0.00155 0.00168 0.00087 C25 1.03244 0.63142 1.08661 1.00000 0.03291 0.03965 0.02310 0.00341 0.01045 0.00493 0.03129 0.00817 0.00049 0.00021 0.00040 0.00000 0.00222 0.00254 0.00186 0.00173 0.00164 0.00192 0.00091 H25 1.10295 0.63885 1.02906 1.00000 0.03755 0.00000 0.00000 C26 0.87088 0.62759 1.03223 1.00000 0.04219 0.04208 0.02008 -0.00033 0.00426 0.00764 0.03547 0.00842 0.00052 0.00022 0.00041 0.00000 0.00255 0.00268 0.00177 0.00170 0.00167 0.00202 0.00098 H26 0.82897 0.63319 0.93416 1.00000 0.04257 0.00000 0.00000 C27 0.76464 0.61584 1.11388 1.00000 0.02439 0.03692 0.02957 -0.00406 0.00044 0.00204 0.03149 0.00780 0.00049 0.00020 0.00042 0.00000 0.00206 0.00254 0.00202 0.00179 0.00160 0.00176 0.00092 H27 0.65366 0.61293 1.07029 1.00000 0.03779 0.00000 0.00000 C28 0.81919 0.60838 1.25789 1.00000 0.02782 0.03679 0.02630 -0.00301 0.00617 0.00004 0.03045 0.00807 0.00050 0.00021 0.00043 0.00000 0.00223 0.00258 0.00199 0.00174 0.00167 0.00184 0.00096 H28 0.74851 0.60021 1.31488 1.00000 0.03654 0.00000 0.00000 C29 0.98103 0.61344 1.31365 1.00000 0.02769 0.02922 0.02056 0.00036 0.00503 -0.00257 0.02604 0.00729 0.00046 0.00018 0.00038 0.00000 0.00204 0.00227 0.00175 0.00153 0.00150 0.00162 0.00083 C30 1.01406 0.59618 1.57383 1.00000 0.03711 0.06046 0.02255 0.00340 0.00678 -0.01277 0.04021 0.00896 0.00057 0.00023 0.00044 0.00000 0.00248 0.00321 0.00198 0.00187 0.00174 0.00213 0.00114 H30A 1.10316 0.58405 1.65395 1.00000 0.04825 0.00000 0.00000 H30B 0.93673 0.56255 1.55309 1.00000 0.04825 0.00000 0.00000 C31 0.93437 0.65031 1.61377 1.00000 0.04871 0.11698 0.02276 -0.00484 0.01078 0.01881 0.06253 0.01113 0.00064 0.00032 0.00048 0.00000 0.00308 0.00547 0.00218 0.00270 0.00205 0.00319 0.00174 H31A 0.85445 0.66483 1.52941 1.00000 0.07504 0.00000 0.00000 H31B 0.87582 0.63792 1.68308 1.00000 0.07504 0.00000 0.00000 C32 1.04017 0.70127 1.67358 1.00000 0.11615 0.07253 0.06259 -0.02426 -0.03091 0.04788 0.09367 0.01343 0.00099 0.00034 0.00072 0.00000 0.00616 0.00475 0.00401 0.00339 0.00384 0.00440 0.00286 H32A 1.09594 0.71563 1.60388 1.00000 0.11241 0.00000 0.00000 H32B 1.12175 0.68753 1.75769 1.00000 0.11241 0.00000 0.00000 C33 0.94429 0.75293 1.71378 1.00000 0.25951 0.13934 0.13588 -0.06220 -0.06532 0.14291 0.19962 0.02431 0.00177 0.00054 0.00124 0.00000 0.01596 0.00996 0.00911 0.00802 0.00945 0.01079 0.00816 H33A 0.89844 0.77555 1.62623 1.00000 0.23954 0.00000 0.00000 H33B 0.85320 0.73413 1.74099 1.00000 0.23954 0.00000 0.00000 C34 1.00051 0.79178 1.80660 1.00000 0.20334 0.10392 0.13282 -0.04617 0.03563 0.06315 0.14810 0.02144 0.00147 0.00046 0.00112 0.00000 0.01205 0.00809 0.00908 0.00693 0.00834 0.00787 0.00472 H34A 1.06870 0.81971 1.77155 1.00000 0.22215 0.00000 0.00000 H34B 1.06365 0.77173 1.89124 1.00000 0.22215 0.00000 0.00000 H34C 0.91283 0.81409 1.82910 1.00000 0.22215 0.00000 0.00000 N1 0.88450 0.47689 0.96766 1.00000 0.02163 0.03798 0.02200 0.00265 0.00275 -0.00275 0.02773 0.00621 0.00037 0.00016 0.00032 0.00000 0.00160 0.00200 0.00158 0.00138 0.00123 0.00141 0.00073 N2 0.72255 0.45929 1.09924 1.00000 0.02143 0.02877 0.02618 -0.00125 0.00280 0.00173 0.02607 0.00617 0.00037 0.00015 0.00032 0.00000 0.00161 0.00185 0.00159 0.00135 0.00126 0.00139 0.00069 N3 1.23967 0.62305 1.32026 1.00000 0.02536 0.03078 0.02505 -0.00165 0.00554 -0.00031 0.02724 0.00616 0.00038 0.00015 0.00032 0.00000 0.00169 0.00193 0.00155 0.00137 0.00129 0.00140 0.00071 N4 1.07593 0.60728 1.45099 1.00000 0.02781 0.03448 0.01910 0.00062 0.00133 -0.00342 0.02800 0.00642 0.00041 0.00016 0.00033 0.00000 0.00182 0.00202 0.00156 0.00137 0.00131 0.00149 0.00078 Br1 0.62293 0.50916 0.51172 1.00000 0.02866 0.05352 0.02736 -0.00180 0.00679 -0.00289 0.03659 0.00073 0.00004 0.00002 0.00004 0.00000 0.00021 0.00027 0.00019 0.00019 0.00014 0.00019 0.00012 O1 0.40231 0.45432 0.71458 1.00000 0.06383 0.05500 0.04272 -0.00390 0.02342 -0.00463 0.05206 0.00791 0.00050 0.00021 0.00041 0.00000 0.00251 0.00265 0.00207 0.00186 0.00180 0.00207 0.00096 O2 1.56098 0.62353 1.70108 1.00000 0.06487 0.06060 0.04670 -0.00776 0.02761 -0.00933 0.05495 0.00762 0.00049 0.00020 0.00041 0.00000 0.00249 0.00265 0.00208 0.00193 0.00186 0.00204 0.00097 H1O 0.45912 0.46957 0.64277 1.00000 0.06685 0.11203 0.00701 0.00268 0.00640 0.00000 0.01745 H2O 0.37772 0.48163 0.74320 1.00000 0.05027 0.11035 0.00690 0.00256 0.00610 0.00000 0.01934 H3O 1.58864 0.59327 1.65249 1.00000 0.06192 0.11073 0.00675 0.00258 0.00616 0.00000 0.01845 H4O 1.51215 0.60984 1.76762 1.00000 0.09068 0.13453 0.00840 0.00308 0.00779 0.00000 0.02349 Br2 0.34041 0.57076 0.90578 1.00000 0.02898 0.05037 0.02697 0.00020 0.00705 -0.00080 0.03547 0.00072 0.00004 0.00002 0.00004 0.00000 0.00020 0.00026 0.00018 0.00019 0.00014 0.00019 0.00011 Final Structure Factor Calculation for 03src0048 in P2(1) Total number of l.s. parameters = 421 Maximum vector length = 511 Memory required = 5770 / 26068 wR2 = 0.0895 before cycle 11 for 7353 data and 2 / 421 parameters Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 1.540 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 1.604 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.037 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0239 * P )^2 + 2.09 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0403 for 6655 Fo > 4sig(Fo) and 0.0480 for all 7353 data wR2 = 0.0895, GooF = S = 1.037, Restrained GooF = 1.037 for all data Occupancy sum of asymmetric unit = 42.00 for non-hydrogen and 58.00 for hydrogen atoms Principal mean square atomic displacements U 0.1460 0.1277 0.0463 C1_a 0.0982 0.0563 0.0337 C2_a 0.1332 0.0652 0.0386 C1'_b 0.1017 0.0614 0.0274 C2'_b 0.1620 0.0732 0.0284 C3 0.1447 0.0460 0.0226 C4 0.0834 0.0299 0.0185 C5 0.0334 0.0305 0.0206 C6 0.0278 0.0238 0.0176 C7 0.0376 0.0272 0.0207 C8 0.0403 0.0352 0.0179 C9 0.0457 0.0334 0.0201 C10 0.0381 0.0334 0.0208 C11 0.0263 0.0237 0.0208 C12 0.0470 0.0331 0.0214 C13 0.0491 0.0425 0.0295 C14 0.0767 0.0521 0.0399 C15 0.0893 0.0740 0.0503 C16 0.1614 0.0772 0.0603 C17 0.1175 0.0612 0.0393 C18 0.0864 0.0428 0.0392 C19 0.0479 0.0367 0.0323 C20 0.0463 0.0387 0.0209 C21 0.0452 0.0340 0.0179 C22 0.0365 0.0304 0.0188 C23 0.0300 0.0258 0.0217 C24 0.0427 0.0304 0.0209 C25 0.0513 0.0351 0.0200 C26 0.0418 0.0314 0.0213 C27 0.0377 0.0282 0.0254 C28 0.0316 0.0260 0.0205 C29 0.0674 0.0315 0.0218 C30 0.1228 0.0439 0.0208 C31 0.1980 0.0433 0.0397 C32 0.4646 0.0913 0.0429 C33 may be split into 0.9636 0.7595 1.6964 and 0.9250 0.7464 1.7312 0.2529 0.1485 0.0429 C34 0.0394 0.0243 0.0195 N1 0.0312 0.0267 0.0203 N2 0.0312 0.0263 0.0242 N3 0.0370 0.0290 0.0180 N4 0.0539 0.0288 0.0271 Br1 0.0678 0.0530 0.0354 O1 0.0764 0.0535 0.0350 O2 0.0504 0.0290 0.0270 Br2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.030 0.044 0.057 0.070 0.085 0.101 0.125 0.159 0.219 1.000 Number in group 761. 749. 716. 763. 711. 713. 738. 732. 729. 741. GooF 1.110 1.010 1.073 1.047 1.054 1.022 0.995 0.976 1.008 1.071 K 1.255 1.062 1.023 1.008 1.016 1.002 1.002 1.002 1.001 1.004 Resolution(A) 0.77 0.81 0.84 0.89 0.94 1.01 1.09 1.20 1.37 1.72 inf Number in group 749. 726. 750. 716. 754. 714. 752. 718. 736. 738. GooF 1.040 1.086 1.024 1.070 1.032 1.029 0.990 0.885 1.018 1.175 K 1.015 1.031 1.014 1.026 1.002 1.001 1.006 1.008 1.002 1.001 R1 0.135 0.111 0.085 0.069 0.056 0.044 0.037 0.028 0.027 0.023 Recommended weighting scheme: WGHT 0.0238 2.0904 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)/su Fc/Fc(max) Resolution(A) 6 -11 3 407.32 594.66 4.29 0.126 1.01 -3 0 4 1995.31 1632.87 4.22 0.209 2.10 1 -5 0 4033.13 4785.16 4.20 0.357 3.93 -4 20 2 238.03 392.80 4.03 0.102 0.99 7 -2 2 291.46 163.43 3.93 0.066 1.09 -9 -15 2 -5.03 41.69 3.68 0.033 0.81 1 -11 0 1251.55 1514.93 3.60 0.201 1.96 -4 0 2 2301.37 2689.91 3.44 0.268 2.13 -1 -5 12 94.74 3.67 3.44 0.010 0.80 1 -7 0 7132.44 8260.56 3.34 0.469 2.97 -1 20 1 39.26 120.41 3.33 0.057 1.10 9 3 1 289.72 170.46 3.31 0.067 0.90 1 8 0 404.84 307.15 3.25 0.090 2.64 2 17 6 373.47 582.08 3.25 0.124 0.95 0 0 4 159.68 240.70 3.24 0.080 2.38 -9 -1 4 39.85 5.08 3.22 0.012 0.95 -1 -23 3 386.23 265.45 3.20 0.084 0.93 -7 -20 2 173.37 66.42 3.20 0.042 0.83 8 3 3 162.19 71.96 3.19 0.044 0.92 -2 20 2 75.63 146.31 3.16 0.062 1.06 2 -28 1 74.25 14.57 3.14 0.020 0.77 4 19 6 303.50 438.78 3.13 0.108 0.81 -7 -4 4 273.58 192.76 3.13 0.072 1.17 -3 22 7 90.47 7.93 3.08 0.015 0.81 -6 -22 3 85.44 17.74 3.04 0.022 0.82 5 -9 3 550.44 686.45 3.03 0.135 1.18 -2 -2 2 2415.12 2101.76 3.02 0.237 3.47 5 -19 5 247.55 138.27 3.01 0.061 0.81 10 2 0 203.72 103.96 2.98 0.053 0.84 0 -6 0 25247.66 28821.53 2.96 0.876 3.71 -3 21 1 241.28 350.48 2.96 0.097 0.99 3 3 10 29.86 75.88 2.95 0.045 0.83 0 -20 3 286.58 199.45 2.94 0.073 1.05 0 -12 1 4738.29 5338.34 2.93 0.377 1.82 -10 -10 3 -4.98 30.02 2.91 0.028 0.81 -11 -4 3 110.99 33.20 2.90 0.030 0.78 -6 12 2 39.12 82.17 2.90 0.047 1.14 5 12 4 258.78 342.62 2.89 0.096 1.02 4 14 7 30.37 86.58 2.88 0.048 0.86 0 -18 5 1562.40 1329.51 2.88 0.188 1.04 -3 -19 3 673.92 542.10 2.86 0.120 1.05 7 0 2 323.36 225.66 2.84 0.078 1.10 -8 0 11 242.95 151.79 2.84 0.064 0.77 -4 -22 1 536.00 419.09 2.84 0.106 0.92 8 0 2 57.55 0.11 2.82 0.002 0.97 -9 -13 6 40.26 96.46 2.81 0.051 0.81 0 12 0 2148.94 1813.36 2.80 0.220 1.85 5 -5 0 1279.15 1473.43 2.80 0.198 1.57 5 16 1 558.94 719.98 2.79 0.138 1.04 -1 20 9 209.45 87.86 2.79 0.048 0.78 Bond lengths and angles C1_a - Distance Angles C2_a 1.4096 (0.0177) H1A_a 0.9800 109.47 H1B_a 0.9800 109.47 109.47 H1C_a 0.9800 109.47 109.47 109.47 C1_a - C2_a H1A_a H1B_a C2_a - Distance Angles C1_a 1.4096 (0.0177) C3 1.6048 (0.0110) 107.64 (1.02) H2A_a 0.9900 110.18 110.18 H2B_a 0.9900 110.18 110.18 108.48 C2_a - C1_a C3 H2A_a C1'_b - Distance Angles C2'_b 1.5513 (0.0287) H1'1_b 0.9800 109.47 H1'2_b 0.9800 109.47 109.47 H1'3_b 0.9800 109.47 109.47 109.47 C1'_b - C2'_b H1'1_b H1'2_b C2'_b - Distance Angles C1'_b 1.5513 (0.0287) C3 1.6331 (0.0231) 101.30 (1.48) H2'1_b 0.9900 111.51 111.51 H2'2_b 0.9900 111.51 111.51 109.33 C2'_b - C1'_b C3 H2'1_b C3 - Distance Angles C4 1.4625 (0.0102) C2_a 1.6048 (0.0111) 100.63 (0.67) C2'_b 1.6331 (0.0232) 135.53 (0.91) 40.58 (0.72) H3A_a 0.9900 111.65 111.65 104.81 H3B_a 0.9900 111.65 111.65 77.64 109.43 C3 - C4 C2_a C2'_b H3A_a C4 - Distance Angles C3 1.4625 (0.0103) C5 1.4746 (0.0080) 114.59 (0.48) H4A 0.9900 108.62 108.62 H4B 0.9900 108.62 108.62 107.57 C4 - C3 C5 H4A C5 - Distance Angles N1 1.4595 (0.0049) C4 1.4746 (0.0080) 112.83 (0.45) H5A 0.9900 109.02 109.02 H5B 0.9900 109.02 109.02 107.80 C5 - N1 C4 H5A C6 - Distance Angles N1 1.3179 (0.0050) N2 1.3230 (0.0049) 111.24 (0.34) H6 0.9500 124.38 124.38 C6 - N1 N2 C7 - Distance Angles C12 1.3781 (0.0052) C8 1.3858 (0.0053) 122.51 (0.35) N1 1.3957 (0.0045) 106.67 (0.32) 130.80 (0.35) C7 - C12 C8 C8 - Distance Angles C9 1.3767 (0.0053) C7 1.3858 (0.0053) 116.31 (0.35) H8 0.9500 121.84 121.84 C8 - C9 C7 C9 - Distance Angles C8 1.3767 (0.0053) C10 1.4069 (0.0058) 121.28 (0.37) H9 0.9500 119.36 119.36 C9 - C8 C10 C10 - Distance Angles C11 1.3709 (0.0060) C9 1.4069 (0.0058) 121.91 (0.37) H10 0.9500 119.05 119.05 C10 - C11 C9 C11 - Distance Angles C10 1.3709 (0.0060) C12 1.3901 (0.0052) 116.62 (0.37) H11 0.9500 121.69 121.69 C11 - C10 C12 C12 - Distance Angles C7 1.3781 (0.0052) N2 1.3874 (0.0048) 106.80 (0.32) C11 1.3901 (0.0052) 121.35 (0.35) 131.83 (0.34) C12 - C7 N2 C13 - Distance Angles N2 1.4719 (0.0049) C14 1.5030 (0.0066) 113.65 (0.35) H13A 0.9900 108.83 108.83 H13B 0.9900 108.83 108.83 107.69 C13 - N2 C14 H13A C14 - Distance Angles C13 1.5030 (0.0066) C15 1.5254 (0.0069) 113.33 (0.39) H14A 0.9900 108.91 108.91 H14B 0.9900 108.91 108.91 107.73 C14 - C13 C15 H14A C15 - Distance Angles C14 1.5254 (0.0069) C16 1.5484 (0.0081) 112.79 (0.45) H15A 0.9900 109.03 109.03 H15B 0.9900 109.03 109.03 107.80 C15 - C14 C16 H15A C16 - Distance Angles C17 1.4467 (0.0097) C15 1.5484 (0.0081) 113.06 (0.60) H16A 0.9900 108.97 108.97 H16B 0.9900 108.97 108.97 107.77 C16 - C17 C15 H16A C17 - Distance Angles C16 1.4467 (0.0097) H17A 0.9800 109.47 H17B 0.9800 109.47 109.47 H17C 0.9800 109.47 109.47 109.47 C17 - C16 H17A H17B C18 - Distance Angles C19 1.5059 (0.0076) H18A 0.9800 109.47 H18B 0.9800 109.47 109.47 H18C 0.9800 109.47 109.47 109.47 C18 - C19 H18A H18B C19 - Distance Angles C20 1.5052 (0.0069) C18 1.5059 (0.0076) 112.70 (0.45) H19A 0.9900 109.05 109.05 H19B 0.9900 109.05 109.05 107.81 C19 - C20 C18 H19A C20 - Distance Angles C19 1.5052 (0.0069) C21 1.5213 (0.0061) 113.33 (0.39) H20A 0.9900 108.91 108.91 H20B 0.9900 108.91 108.91 107.73 C20 - C19 C21 H20A C21 - Distance Angles C22 1.5006 (0.0065) C20 1.5213 (0.0061) 113.95 (0.36) H21A 0.9900 108.76 108.76 H21B 0.9900 108.76 108.76 107.65 C21 - C22 C20 H21A C22 - Distance Angles N3 1.4622 (0.0048) C21 1.5006 (0.0065) 112.46 (0.34) H22A 0.9900 109.11 109.11 H22B 0.9900 109.11 109.11 107.85 C22 - N3 C21 H22A C23 - Distance Angles N4 1.3216 (0.0053) N3 1.3274 (0.0050) 110.66 (0.36) H23 0.9500 124.67 124.67 C23 - N4 N3 C24 - Distance Angles N3 1.3863 (0.0051) C25 1.3889 (0.0051) 132.33 (0.36) C29 1.4012 (0.0054) 106.79 (0.33) 120.87 (0.36) C24 - N3 C25 C25 - Distance Angles C26 1.3681 (0.0061) C24 1.3889 (0.0051) 116.18 (0.36) H25 0.9500 121.91 121.91 C25 - C26 C24 C26 - Distance Angles C25 1.3681 (0.0061) C27 1.3959 (0.0060) 123.17 (0.37) H26 0.9500 118.41 118.41 C26 - C25 C27 C27 - Distance Angles C28 1.3869 (0.0054) C26 1.3959 (0.0060) 120.78 (0.38) H27 0.9500 119.61 119.61 C27 - C28 C26 C28 - Distance Angles C29 1.3741 (0.0058) C27 1.3869 (0.0053) 116.37 (0.37) H28 0.9500 121.81 121.81 C28 - C29 C27 C29 - Distance Angles C28 1.3741 (0.0058) N4 1.3990 (0.0046) 131.70 (0.37) C24 1.4012 (0.0054) 122.59 (0.36) 105.63 (0.34) C29 - C28 N4 C30 - Distance Angles N4 1.4671 (0.0052) C31 1.4905 (0.0076) 112.07 (0.41) H30A 0.9900 109.20 109.20 H30B 0.9900 109.20 109.20 107.90 C30 - N4 C31 H30A C31 - Distance Angles C32 1.4817 (0.0101) C30 1.4905 (0.0076) 116.16 (0.49) H31A 0.9900 108.25 108.25 H31B 0.9900 108.25 108.25 107.38 C31 - C32 C30 H31A C32 - Distance Angles C31 1.4817 (0.0101) C33 1.5291 (0.0117) 110.81 (0.88) H32A 0.9900 109.48 109.48 H32B 0.9900 109.48 109.48 108.06 C32 - C31 C33 H32A C33 - Distance Angles C34 1.2620 (0.0132) C32 1.5291 (0.0117) 124.62 (1.14) H33A 0.9900 106.17 106.17 H33B 0.9900 106.17 106.17 106.36 C33 - C34 C32 H33A C34 - Distance Angles C33 1.2620 (0.0132) H34A 0.9800 109.47 H34B 0.9800 109.47 109.47 H34C 0.9800 109.47 109.47 109.47 C34 - C33 H34A H34B N1 - Distance Angles C6 1.3179 (0.0050) C7 1.3957 (0.0045) 107.54 (0.32) C5 1.4595 (0.0049) 126.45 (0.32) 125.99 (0.32) N1 - C6 C7 N2 - Distance Angles C6 1.3230 (0.0049) C12 1.3874 (0.0049) 107.73 (0.33) C13 1.4719 (0.0049) 125.71 (0.34) 126.55 (0.32) N2 - C6 C12 N3 - Distance Angles C23 1.3274 (0.0050) C24 1.3863 (0.0052) 108.32 (0.34) C22 1.4622 (0.0048) 125.58 (0.35) 126.09 (0.33) N3 - C23 C24 N4 - Distance Angles C23 1.3216 (0.0054) C29 1.3990 (0.0046) 108.59 (0.33) C30 1.4671 (0.0052) 126.85 (0.34) 124.56 (0.34) N4 - C23 C29 O1 - Distance Angles H1O 1.0195 (0.0630) H2O 0.7246 (0.0547) 103.62 (5.74) O1 - H1O O2 - Distance Angles H3O 0.8938 (0.0593) H4O 0.9198 (0.0746) 111.73 (5.64) O2 - H3O FMAP and GRID set by program FMAP 2 1 42 GRID -2.564 -1 -2 2.564 1 2 R1 = 0.0440 for 4240 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.65 at 0.3803 0.0524 0.4715 [ 0.98 A from BR1 ] Deepest hole -0.60 at 0.0240 0.2603 0.2995 [ 0.37 A from C33 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 5609 / 57552 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.6197 0.5524 0.5285 1.00000 0.05 0.65 0.98 BR1 1.60 H3O 2.29 H22B 2.47 O2 Q2 1 0.3408 0.5271 0.8958 1.00000 0.05 0.55 0.98 BR2 1.91 H2O 2.25 H13A 2.57 O1 Q3 1 0.6051 0.3324 1.0809 1.00000 0.05 0.40 0.95 H15A 1.10 C15 1.53 H14B 1.59 C14 Q4 1 0.6260 0.4626 0.5228 1.00000 0.05 0.40 1.04 BR1 2.10 H1O 2.54 H18C 2.71 H3A Q5 1 0.3392 0.6173 0.9093 1.00000 0.05 0.39 1.03 BR2 2.30 H4O 2.60 H32B 2.66 H25 Q6 1 0.3644 0.2600 1.0874 1.00000 0.05 0.36 0.91 H16A 1.08 C16 1.32 C17 1.35 H17C Q7 1 1.0267 0.7771 1.6793 1.00000 0.05 0.35 1.02 C33 1.10 H33A 1.30 H34A 1.37 C34 Q8 1 0.9184 0.3953 0.7232 1.00000 0.05 0.35 0.57 C3 0.74 H3A 1.41 C4 1.52 H3B Q9 1 1.0253 0.6959 1.6991 1.00000 0.05 0.34 0.33 C32 0.90 H32B 1.32 H32A 1.42 C31 Q10 1 0.5634 0.2793 1.0884 1.00000 0.05 0.30 0.88 C17 1.04 H17B 1.21 H17A 1.31 C16 Shortest distances between peaks (including symmetry equivalents) 3 10 1.24 6 10 1.78 7 9 1.81 1 4 2.00 2 5 2.01 3 6 2.65 Time profile in seconds ----------------------- 0.00: Read and process instructions 0.00: Fit rigid groups 0.02: Interpret restraints etc. 0.02: 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. 0.56: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.00: Generate idealized H-atoms 12.52: Structure factors and derivatives 14.25: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.06: Apply other restraints 1.06: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.11: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 15:06:55 Total CPU time: 28.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++