+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008src0842 started at 10:23:23 on 15-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src0842 in P-1 CELL 0.71073 9.5497 10.3189 11.1034 104.436 107.828 104.170 ZERR 2.00 0.0004 0.0004 0.0004 0.002 0.002 0.002 LATT 1 SFAC C H N O S UNIT 42 38 2 10 2 V = 945.55 F(000) = 416.0 Mu = 0.20 mm-1 Cell Wt = 794.86 Rho = 1.396 MERG 2 OMIT -3.00 55.00 OMIT -2 0 2 OMIT -1 1 3 SHEL 7 0.77 SADI C5 C18 C5 C118 delu 0.01 c18 > s2 simu 0.01 c18 > s2 isor 0.01 c18 c118 EADP C18 C118 EADP C19 C120 FMAP 2 PLAN 5 SIZE 0.12 0.22 0.28 ACTA BOND $H WGHT 0.05270 0.32530 L.S. 15 TEMP -153.00 FVAR 1.04728 0.49463 C1 1 0.148442 0.686494 0.488220 11.00000 0.01846 0.01794 = 0.01768 0.00721 0.00912 0.00792 C2 1 0.063597 0.845106 0.394165 11.00000 0.01745 0.01834 = 0.01712 0.00649 0.00868 0.00878 C3 1 -0.065737 0.700949 0.313219 11.00000 0.01609 0.01670 = 0.01952 0.00719 0.00701 0.00725 AFIX 13 H3 2 -0.168869 0.701333 0.317141 11.00000 -1.20000 AFIX 0 C4 1 -0.007304 0.595711 0.372921 11.00000 0.01640 0.01543 = 0.01848 0.00660 0.00599 0.00558 AFIX 13 H4 2 -0.083349 0.542588 0.404012 11.00000 -1.20000 AFIX 0 C5 1 0.006995 0.494886 0.249720 11.00000 0.01911 0.01653 = 0.01964 0.00820 0.00666 0.00748 C6 1 -0.161294 0.397642 0.148668 11.00000 0.02040 0.01844 = 0.02118 0.00506 0.00426 0.00618 AFIX 23 H6A 2 -0.225778 0.359392 0.195238 11.00000 -1.20000 H6B 2 -0.160370 0.317368 0.078433 11.00000 -1.20000 AFIX 0 C7 1 -0.221023 0.503287 0.087959 11.00000 0.02104 0.02066 = 0.02000 0.00431 0.00358 0.00766 AFIX 23 H7A 2 -0.246999 0.472944 -0.010507 11.00000 -1.20000 H7B 2 -0.314100 0.513684 0.105327 11.00000 -1.20000 AFIX 0 C8 1 -0.077733 0.642157 0.165679 11.00000 0.01548 0.02044 = 0.01888 0.00744 0.00554 0.00956 C9 1 -0.065535 0.751022 0.096324 11.00000 0.02019 0.01980 = 0.01419 0.00447 0.00388 0.00841 C10 1 -0.196067 0.896186 0.010502 11.00000 0.03848 0.03596 = 0.02984 0.02320 0.01490 0.02288 AFIX 23 H10A 2 -0.179754 0.868069 -0.074757 11.00000 -1.20000 H10B 2 -0.110562 0.986698 0.073625 11.00000 -1.20000 AFIX 0 C11 1 -0.351743 0.915154 -0.016404 11.00000 0.06750 0.10603 = 0.08006 0.07724 0.04964 0.06979 AFIX 137 H11A 2 -0.435484 0.824760 -0.078270 11.00000 -1.50000 H11B 2 -0.355819 0.988722 -0.057364 11.00000 -1.50000 H11C 2 -0.365921 0.944409 0.068793 11.00000 -1.50000 AFIX 0 C12 1 0.323137 0.942534 0.588386 11.00000 0.01623 0.01555 = 0.01658 0.00618 0.00474 0.00426 C13 1 0.467474 0.926821 0.607562 11.00000 0.01945 0.01835 = 0.02037 0.00601 0.00710 0.00815 AFIX 43 H13 2 0.473755 0.840027 0.558906 11.00000 -1.20000 AFIX 0 C14 1 0.602422 1.039361 0.698617 11.00000 0.01631 0.02349 = 0.02205 0.00839 0.00607 0.00769 AFIX 43 H14 2 0.701828 1.028896 0.713812 11.00000 -1.20000 AFIX 0 C15 1 0.594009 1.167261 0.767906 11.00000 0.01957 0.01943 = 0.02021 0.00628 0.00439 0.00405 AFIX 43 H15 2 0.687305 1.245050 0.828088 11.00000 -1.20000 AFIX 0 C16 1 0.449029 1.180901 0.748882 11.00000 0.02603 0.01960 = 0.02938 0.00279 0.00792 0.01051 AFIX 43 H16 2 0.442958 1.268093 0.796910 11.00000 -1.20000 AFIX 0 C17 1 0.312077 1.067910 0.659958 11.00000 0.01833 0.02020 = 0.02906 0.00565 0.00741 0.00910 AFIX 43 H17 2 0.212407 1.076496 0.648420 11.00000 -1.20000 AFIX 0 N1 3 0.182324 0.827839 0.492339 11.00000 0.01569 0.01471 = 0.01859 0.00626 0.00518 0.00618 O1 4 0.232495 0.648187 0.567187 11.00000 0.02209 0.02002 = 0.02132 0.00987 0.00453 0.00731 O2 4 0.065336 0.956731 0.376797 11.00000 0.02109 0.01803 = 0.02446 0.00938 0.00753 0.00937 O3 4 0.053179 0.592876 0.183750 11.00000 0.01866 0.01925 = 0.02041 0.01016 0.00784 0.01036 O4 4 0.044149 0.800573 0.070024 11.00000 0.02391 0.02748 = 0.02638 0.01319 0.01124 0.01072 O5 4 -0.195714 0.784366 0.069938 11.00000 0.02359 0.03043 = 0.02650 0.01726 0.01110 0.01609 PART 1 S1 5 0.311460 0.492326 0.298029 21.00000 0.02432 0.02323 = 0.03085 0.01464 0.00956 0.01379 C18 1 0.121544 0.424087 0.283472 21.00000 0.02431 0.02056 = 0.02188 0.00774 0.00945 -0.00413 C19 1 0.354983 0.376949 0.343071 21.00000 0.02203 0.01456 = 0.02796 0.01341 0.01102 0.01124 AFIX 43 H19 2 0.460538 0.381765 0.362326 21.00000 -1.20000 AFIX 0 C20 1 0.260542 0.266182 0.359497 21.00000 0.01584 0.02017 = 0.02757 0.00605 0.00941 0.01331 AFIX 43 H20 2 0.281123 0.190015 0.386417 21.00000 -1.20000 AFIX 0 C21 1 0.104330 0.304452 0.319321 21.00000 0.02421 0.02677 = 0.03280 0.00404 0.00821 0.00712 AFIX 43 H21 2 0.008899 0.250025 0.320080 21.00000 -1.20000 AFIX 0 PART 2 same S1 > C21 S2 5 0.068611 0.269035 0.321014 -21.00000 0.02483 0.01721 = 0.02728 0.00974 0.01167 0.01154 C118 1 0.122886 0.419663 0.283657 -21.00000 0.01811 0.01393 = 0.01721 0.00466 0.00402 0.01772 C119 1 0.235265 0.265452 0.361696 -21.00000 0.02675 0.02543 = 0.03000 0.01558 0.02036 0.01448 AFIX 43 H119 2 0.253605 0.192722 0.395777 -21.00000 -1.20000 AFIX 0 C120 1 0.360058 0.355626 0.354155 -21.00000 0.02985 0.02107 = 0.02933 0.01904 0.00453 0.01828 AFIX 43 H120 2 0.464448 0.356606 0.373697 -21.00000 -1.20000 AFIX 0 C121 1 0.276719 0.459603 0.302183 -21.00000 0.05621 0.02097 = 0.03693 0.01627 0.01275 0.01481 AFIX 43 H121 2 0.329094 0.540402 0.286055 -21.00000 -1.20000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 2008src0842 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 C1 - O1 N1 C4 C2 - O2 N1 C3 C3 - C2 C4 C8 C4 - C1 C3 C5 C5 - O3 C18_a C118_b C6 C4 C6 - C5 C7 C7 - C8 C6 C8 - O3 C9 C7 C3 C9 - O4 O5 C8 C10 - O5 C11 C11 - C10 C12 - C13 C17 N1 C13 - C14 C12 C14 - C13 C15 C15 - C16 C14 C16 - C15 C17 C17 - C12 C16 N1 - C2 C1 C12 O1 - C1 O2 - C2 O3 - C8 C5 O4 - C9 O5 - C9 C10 S1_a - C19_a C18_a C18_a - C21_a C5 S1_a C19_a - C20_a S1_a C20_a - C19_a C21_a C21_a - C18_a C20_a S2_b - C119_b C118_b C118_b - C121_b C5 S2_b C119_b - C120_b S2_b C120_b - C119_b C121_b C121_b - C118_b C120_b 21248 Reflections read, of which 13 rejected -12 =< h =< 12, -13 =< k =< 13, -14 =< l =< 13, Max. 2-theta = 54.97 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -11 5 5 11.94 1.22 2 8.85 -7 9 6 -1.22 4.31 2 29.11 5 -8 8 -8.17 2.89 3 16.74 -6 1 10 -0.08 0.23 5 2.31 4 Inconsistent equivalents 4327 Unique reflections, of which 0 suppressed R(int) = 0.0491 R(sigma) = 0.0432 Friedel opposites merged Maximum memory for data reduction = 2915 / 43650 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 = 3725 / 360545 wR2 = 0.1284 before cycle 1 for 4327 data and 288 / 288 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 11. 0. 0. 0. 5. 24. 12. 0. rms sigma 0.000 0.000 0.000 0.031 0.000 0.000 0.000 0.010 0.010 0.010 0.000 rms deviation 0.000 0.000 0.000 0.019 0.000 0.000 0.000 0.016 0.006 0.006 0.000 GooF = S = 1.204; Restrained GooF = 1.201 for 52 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0527 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.04669 0.00225 -0.264 OSF 2 0.49485 0.00307 0.072 FVAR 2 223 0.02004 0.00123 -3.465 U11 C18_a 228 0.00633 0.00129 8.097 U12 C18_a Mean shift/esd = 0.169 Maximum = 8.097 for U12 C18_a Max. shift = 0.058 A for C18_a Max. dU =-0.005 for C18_a Least-squares cycle 2 Maximum vector length = 511 Memory required = 3725 / 360545 wR2 = 0.1135 before cycle 2 for 4327 data and 288 / 288 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 11. 0. 0. 0. 5. 24. 12. 0. rms sigma 0.000 0.000 0.000 0.031 0.000 0.000 0.000 0.010 0.010 0.010 0.000 rms deviation 0.000 0.000 0.000 0.010 0.000 0.000 0.000 0.012 0.005 0.001 0.000 GooF = S = 1.062; Restrained GooF = 1.057 for 52 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0527 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.04677 0.00198 0.044 OSF 2 0.49456 0.00271 -0.108 FVAR 2 Mean shift/esd = 0.066 Maximum = 1.035 for U12 C18_a Max. shift = 0.036 A for C18_a Max. dU = 0.001 for C19_a Least-squares cycle 3 Maximum vector length = 511 Memory required = 3725 / 360545 wR2 = 0.1129 before cycle 3 for 4327 data and 288 / 288 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 11. 0. 0. 0. 5. 24. 12. 0. rms sigma 0.000 0.000 0.000 0.031 0.000 0.000 0.000 0.010 0.010 0.010 0.000 rms deviation 0.000 0.000 0.000 0.010 0.000 0.000 0.000 0.012 0.006 0.002 0.000 GooF = S = 1.056; Restrained GooF = 1.051 for 52 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0527 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.04677 0.00197 -0.003 OSF 2 0.49445 0.00269 -0.040 FVAR 2 Mean shift/esd = 0.039 Maximum = -0.549 for U22 C18_a Max. shift = 0.020 A for C118_b Max. dU = 0.000 for C18_a Least-squares cycle 4 Maximum vector length = 511 Memory required = 3725 / 360545 wR2 = 0.1127 before cycle 4 for 4327 data and 288 / 288 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 11. 0. 0. 0. 5. 24. 12. 0. rms sigma 0.000 0.000 0.000 0.031 0.000 0.000 0.000 0.010 0.010 0.010 0.000 rms deviation 0.000 0.000 0.000 0.009 0.000 0.000 0.000 0.013 0.006 0.002 0.000 GooF = S = 1.054; Restrained GooF = 1.050 for 52 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0527 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.04677 0.00197 -0.001 OSF 2 0.49442 0.00269 -0.012 FVAR 2 Mean shift/esd = 0.021 Maximum = -0.977 for U12 C18_a Max. shift = 0.025 A for C18_a Max. dU = 0.000 for C21_a Least-squares cycle 5 Maximum vector length = 511 Memory required = 3725 / 360545 wR2 = 0.1127 before cycle 5 for 4327 data and 288 / 288 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 11. 0. 0. 0. 5. 24. 12. 0. rms sigma 0.000 0.000 0.000 0.031 0.000 0.000 0.000 0.010 0.010 0.010 0.000 rms deviation 0.000 0.000 0.000 0.010 0.000 0.000 0.000 0.013 0.006 0.001 0.000 GooF = S = 1.054; Restrained GooF = 1.050 for 52 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0527 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.04678 0.00197 0.008 OSF 2 0.49434 0.00269 -0.028 FVAR 2 Mean shift/esd = 0.013 Maximum = -0.184 for z C18_a Max. shift = 0.028 A for C18_a Max. dU = 0.000 for C119_b Least-squares cycle 6 Maximum vector length = 511 Memory required = 3725 / 360545 wR2 = 0.1127 before cycle 6 for 4327 data and 288 / 288 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 11. 0. 0. 0. 5. 24. 12. 0. rms sigma 0.000 0.000 0.000 0.031 0.000 0.000 0.000 0.010 0.010 0.010 0.000 rms deviation 0.000 0.000 0.000 0.009 0.000 0.000 0.000 0.013 0.006 0.001 0.000 GooF = S = 1.054; Restrained GooF = 1.050 for 52 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0527 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.04680 0.00197 0.012 OSF 2 0.49438 0.00269 0.015 FVAR 2 Mean shift/esd = 0.011 Maximum = -0.193 for U22 C18_a Max. shift = 0.019 A for C18_a Max. dU = 0.000 for C119_b Least-squares cycle 7 Maximum vector length = 511 Memory required = 3725 / 360545 wR2 = 0.1127 before cycle 7 for 4327 data and 288 / 288 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 11. 0. 0. 0. 5. 24. 12. 0. rms sigma 0.000 0.000 0.000 0.031 0.000 0.000 0.000 0.010 0.010 0.010 0.000 rms deviation 0.000 0.000 0.000 0.009 0.000 0.000 0.000 0.013 0.006 0.001 0.000 GooF = S = 1.054; Restrained GooF = 1.050 for 52 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0527 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.04678 0.00197 -0.013 OSF 2 0.49439 0.00269 0.001 FVAR 2 Mean shift/esd = 0.005 Maximum = -0.171 for U33 C18_a Max. shift = 0.011 A for C18_a Max. dU = 0.000 for C18_a Least-squares cycle 8 Maximum vector length = 511 Memory required = 3725 / 360545 wR2 = 0.1126 before cycle 8 for 4327 data and 288 / 288 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 11. 0. 0. 0. 5. 24. 12. 0. rms sigma 0.000 0.000 0.000 0.031 0.000 0.000 0.000 0.010 0.010 0.010 0.000 rms deviation 0.000 0.000 0.000 0.009 0.000 0.000 0.000 0.013 0.006 0.001 0.000 GooF = S = 1.054; Restrained GooF = 1.050 for 52 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0527 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.04678 0.00197 0.001 OSF 2 0.49441 0.00269 0.010 FVAR 2 Mean shift/esd = 0.004 Maximum = -0.144 for U12 C18_a Max. shift = 0.007 A for C18_a Max. dU = 0.000 for C18_a Least-squares cycle 9 Maximum vector length = 511 Memory required = 3725 / 360545 wR2 = 0.1127 before cycle 9 for 4327 data and 288 / 288 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 11. 0. 0. 0. 5. 24. 12. 0. rms sigma 0.000 0.000 0.000 0.031 0.000 0.000 0.000 0.010 0.010 0.010 0.000 rms deviation 0.000 0.000 0.000 0.009 0.000 0.000 0.000 0.013 0.006 0.001 0.000 GooF = S = 1.055; Restrained GooF = 1.050 for 52 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0527 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.04678 0.00197 0.001 OSF 2 0.49441 0.00269 -0.002 FVAR 2 Mean shift/esd = 0.003 Maximum = -0.077 for U33 C18_a Max. shift = 0.005 A for C18_a Max. dU = 0.000 for C18_a Least-squares cycle 10 Maximum vector length = 511 Memory required = 3725 / 360545 wR2 = 0.1126 before cycle 10 for 4327 data and 288 / 288 parameters Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 11. 0. 0. 0. 5. 24. 12. 0. rms sigma 0.000 0.000 0.000 0.031 0.000 0.000 0.000 0.010 0.010 0.010 0.000 rms deviation 0.000 0.000 0.000 0.009 0.000 0.000 0.000 0.013 0.006 0.001 0.000 GooF = S = 1.054; Restrained GooF = 1.050 for 52 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0527 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.04678 0.00197 0.002 OSF 2 0.49441 0.00269 0.002 FVAR 2 Mean shift/esd = 0.002 Maximum = -0.037 for U12 C18_a Max. shift = 0.003 A for C18_a Max. dU = 0.000 for C119_b Least-squares cycle 11 Maximum vector length = 511 Memory required = 3725 / 360545 wR2 = 0.1126 before cycle 11 for 4327 data and 288 / 288 parameters Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 11. 0. 0. 0. 5. 24. 12. 0. rms sigma 0.000 0.000 0.000 0.031 0.000 0.000 0.000 0.010 0.010 0.010 0.000 rms deviation 0.000 0.000 0.000 0.009 0.000 0.000 0.000 0.013 0.006 0.001 0.000 GooF = S = 1.054; Restrained GooF = 1.050 for 52 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0527 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.04679 0.00197 0.000 OSF 2 0.49441 0.00269 -0.001 FVAR 2 Mean shift/esd = 0.001 Maximum = 0.018 for x C18_a Max. shift = 0.002 A for C18_a Max. dU = 0.000 for C18_a Least-squares cycle 12 Maximum vector length = 511 Memory required = 3725 / 360545 wR2 = 0.1126 before cycle 12 for 4327 data and 288 / 288 parameters Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 11. 0. 0. 0. 5. 24. 12. 0. rms sigma 0.000 0.000 0.000 0.031 0.000 0.000 0.000 0.010 0.010 0.010 0.000 rms deviation 0.000 0.000 0.000 0.009 0.000 0.000 0.000 0.013 0.006 0.001 0.000 GooF = S = 1.054; Restrained GooF = 1.050 for 52 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0527 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.04678 0.00197 -0.001 OSF 2 0.49441 0.00269 0.001 FVAR 2 Mean shift/esd = 0.001 Maximum = 0.012 for x C118_b Max. shift = 0.002 A for C18_a Max. dU = 0.000 for C119_b Least-squares cycle 13 Maximum vector length = 511 Memory required = 3725 / 360545 wR2 = 0.1126 before cycle 13 for 4327 data and 288 / 288 parameters Summary of restraints applied in cycle 13 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 11. 0. 0. 0. 5. 24. 12. 0. rms sigma 0.000 0.000 0.000 0.031 0.000 0.000 0.000 0.010 0.010 0.010 0.000 rms deviation 0.000 0.000 0.000 0.009 0.000 0.000 0.000 0.013 0.006 0.001 0.000 GooF = S = 1.054; Restrained GooF = 1.050 for 52 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0527 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.04678 0.00197 -0.001 OSF 2 0.49441 0.00269 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.009 for x C18_a Max. shift = 0.001 A for C18_a Max. dU = 0.000 for C18_a Least-squares cycle 14 Maximum vector length = 511 Memory required = 3725 / 360545 wR2 = 0.1126 before cycle 14 for 4327 data and 288 / 288 parameters Summary of restraints applied in cycle 14 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 11. 0. 0. 0. 5. 24. 12. 0. rms sigma 0.000 0.000 0.000 0.031 0.000 0.000 0.000 0.010 0.010 0.010 0.000 rms deviation 0.000 0.000 0.000 0.009 0.000 0.000 0.000 0.013 0.006 0.001 0.000 GooF = S = 1.054; Restrained GooF = 1.050 for 52 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0527 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.04678 0.00197 0.001 OSF 2 0.49441 0.00269 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.006 for x C118_b Max. shift = 0.001 A for C18_a Max. dU = 0.000 for C119_b Least-squares cycle 15 Maximum vector length = 511 Memory required = 3725 / 360545 wR2 = 0.1126 before cycle 15 for 4327 data and 288 / 288 parameters Summary of restraints applied in cycle 15 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 11. 0. 0. 0. 5. 24. 12. 0. rms sigma 0.000 0.000 0.000 0.031 0.000 0.000 0.000 0.010 0.010 0.010 0.000 rms deviation 0.000 0.000 0.000 0.009 0.000 0.000 0.000 0.013 0.006 0.001 0.000 GooF = S = 1.054; Restrained GooF = 1.050 for 52 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0527 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.04678 0.00197 -0.001 OSF 2 0.49441 0.00269 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.004 for x C18_a Max. shift = 0.001 A for C18_a Max. dU = 0.000 for C119_b Largest correlation matrix elements -0.999 z C118_b / z C18_a -0.977 U22 C19_a / y C19_a -0.940 x C118_b / y C18_a -0.999 y C118_b / y C18_a 0.977 y C120_b / U22 C19_a -0.935 U12 C19_a / x C19_a -0.999 x C118_b / x C18_a 0.964 z C120_b / U23 C19_a 0.932 x C120_b / U12 C19_a -0.994 z C120_b / z C19_a -0.963 U23 C19_a / z C19_a -0.931 x C119_b / x C20_a -0.985 x C120_b / x C19_a 0.941 y C118_b / x C118_b -0.912 z C121_b / z S1_a -0.984 z C119_b / z C20_a 0.941 y C18_a / x C18_a -0.903 z C118_b / U33 C18_a -0.981 y C120_b / y C19_a -0.940 y C118_b / x C18_a 0.903 U33 C18_a / z C18_a -0.980 y C119_b / y C20_a -0.940 U11 C119_b / x C20_a -0.896 z C120_b / U33 C19_a Idealized hydrogen atom generation before cycle 16 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 -0.1689 0.7013 0.3172 13 1.000 0.000 C3 C2 C4 C8 H4 -0.0833 0.5426 0.4040 13 1.000 0.000 C4 C1 C3 C5 H6A -0.2258 0.3594 0.1952 23 0.990 0.000 C6 C5 C7 H6B -0.1603 0.3174 0.0784 23 0.990 0.000 C6 C5 C7 H7A -0.2470 0.4730 -0.0105 23 0.990 0.000 C7 C8 C6 H7B -0.3141 0.5137 0.1054 23 0.990 0.000 C7 C8 C6 H10A -0.1798 0.8681 -0.0748 23 0.990 0.000 C10 O5 C11 H10B -0.1106 0.9867 0.0736 23 0.990 0.000 C10 O5 C11 H11A -0.4355 0.8247 -0.0781 137 0.980 0.000 C11 C10 H11A H11B -0.3559 0.9886 -0.0575 137 0.980 0.000 C11 C10 H11A H11C -0.3658 0.9446 0.0688 137 0.980 0.000 C11 C10 H11A H13 0.4737 0.8400 0.5589 43 0.950 0.000 C13 C14 C12 H14 0.7018 1.0289 0.7138 43 0.950 0.000 C14 C13 C15 H15 0.6873 1.2450 0.8281 43 0.950 0.000 C15 C16 C14 H16 0.4430 1.2681 0.7969 43 0.950 0.000 C16 C15 C17 H17 0.2124 1.0765 0.6484 43 0.950 0.000 C17 C12 C16 H19 0.4626 0.3854 0.3692 43 0.950 0.000 C19_a C20_a S1_a H20 0.2810 0.1888 0.3859 43 0.950 0.000 C20_a C19_a C21_a H21 0.0088 0.2505 0.3205 43 0.950 0.000 C21_a C18_a C20_a H119 0.2545 0.1946 0.3966 43 0.950 0.000 C119_b C120_b S2_b H120 0.4638 0.3551 0.3688 43 0.950 0.000 C120_b C119_b C121_b H121 0.3287 0.5410 0.2865 43 0.950 0.000 C121_b C118_b C120_b 2008src0842 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.14843 0.68649 0.48821 1.00000 0.01847 0.01797 0.01769 0.00726 0.00911 0.00797 0.01699 0.00381 0.00017 0.00016 0.00015 0.00000 0.00074 0.00074 0.00072 0.00061 0.00063 0.00063 0.00031 C2 0.06360 0.84511 0.39416 1.00000 0.01747 0.01839 0.01708 0.00649 0.00863 0.00877 0.01660 0.00379 0.00017 0.00016 0.00015 0.00000 0.00073 0.00075 0.00071 0.00060 0.00062 0.00062 0.00031 C3 -0.06573 0.70095 0.31323 1.00000 0.01613 0.01672 0.01950 0.00719 0.00705 0.00723 0.01696 0.00380 0.00017 0.00016 0.00015 0.00000 0.00073 0.00072 0.00073 0.00060 0.00062 0.00061 0.00031 H3 -0.16886 0.70133 0.31716 1.00000 0.02035 0.00000 0.00000 C4 -0.00728 0.59573 0.37293 1.00000 0.01634 0.01541 0.01845 0.00659 0.00600 0.00558 0.01680 0.00374 0.00017 0.00015 0.00015 0.00000 0.00073 0.00071 0.00072 0.00060 0.00062 0.00060 0.00031 H4 -0.08332 0.54261 0.40402 1.00000 0.02015 0.00000 0.00000 C5 0.00697 0.49489 0.24972 1.00000 0.01916 0.01662 0.01944 0.00809 0.00665 0.00724 0.01807 0.00387 0.00018 0.00016 0.00015 0.00000 0.00076 0.00072 0.00073 0.00061 0.00064 0.00063 0.00032 C6 -0.16128 0.39766 0.14867 1.00000 0.02034 0.01846 0.02117 0.00512 0.00428 0.00619 0.02147 0.00388 0.00018 0.00016 0.00016 0.00000 0.00080 0.00077 0.00078 0.00064 0.00067 0.00066 0.00034 H6A -0.22577 0.35938 0.19522 1.00000 0.02576 0.00000 0.00000 H6B -0.16034 0.31740 0.07843 1.00000 0.02576 0.00000 0.00000 C7 -0.22105 0.50330 0.08797 1.00000 0.02107 0.02061 0.01994 0.00427 0.00359 0.00756 0.02220 0.00395 0.00019 0.00017 0.00016 0.00000 0.00080 0.00079 0.00076 0.00064 0.00067 0.00067 0.00034 H7A -0.24705 0.47296 -0.01050 1.00000 0.02664 0.00000 0.00000 H7B -0.31411 0.51370 0.10536 1.00000 0.02664 0.00000 0.00000 C8 -0.07774 0.64216 0.16568 1.00000 0.01541 0.02044 0.01883 0.00748 0.00551 0.00956 0.01774 0.00385 0.00017 0.00016 0.00015 0.00000 0.00072 0.00076 0.00073 0.00062 0.00061 0.00063 0.00031 C9 -0.06551 0.75102 0.09632 1.00000 0.02015 0.01976 0.01417 0.00451 0.00384 0.00850 0.01875 0.00382 0.00018 0.00016 0.00015 0.00000 0.00078 0.00076 0.00069 0.00060 0.00063 0.00065 0.00032 C10 -0.19608 0.89619 0.01050 1.00000 0.03848 0.03589 0.02991 0.02322 0.01492 0.02288 0.02997 0.00504 0.00022 0.00020 0.00019 0.00000 0.00102 0.00099 0.00090 0.00080 0.00082 0.00086 0.00040 H10A -0.17977 0.86807 -0.07476 1.00000 0.03596 0.00000 0.00000 H10B -0.11057 0.98669 0.07363 1.00000 0.03596 0.00000 0.00000 C11 -0.35175 0.91517 -0.01640 1.00000 0.06757 0.10598 0.07997 0.07705 0.04970 0.06972 0.06208 0.00810 0.00030 0.00033 0.00028 0.00000 0.00159 0.00211 0.00176 0.00174 0.00149 0.00165 0.00077 H11A -0.43551 0.82474 -0.07814 1.00000 0.09312 0.00000 0.00000 H11B -0.35589 0.98862 -0.05750 1.00000 0.09312 0.00000 0.00000 H11C -0.36585 0.94459 0.06882 1.00000 0.09312 0.00000 0.00000 C12 0.32314 0.94255 0.58839 1.00000 0.01619 0.01552 0.01653 0.00618 0.00474 0.00424 0.01665 0.00369 0.00017 0.00015 0.00015 0.00000 0.00073 0.00072 0.00070 0.00059 0.00061 0.00061 0.00031 C13 0.46747 0.92683 0.60758 1.00000 0.01941 0.01834 0.02037 0.00602 0.00711 0.00812 0.01939 0.00391 0.00018 0.00016 0.00015 0.00000 0.00077 0.00075 0.00076 0.00062 0.00065 0.00064 0.00032 H13 0.47374 0.84003 0.55892 1.00000 0.02327 0.00000 0.00000 C14 0.60243 1.03935 0.69862 1.00000 0.01633 0.02341 0.02205 0.00845 0.00609 0.00776 0.02070 0.00394 0.00018 0.00017 0.00016 0.00000 0.00075 0.00080 0.00078 0.00066 0.00065 0.00065 0.00033 H14 0.70183 1.02887 0.71379 1.00000 0.02484 0.00000 0.00000 C15 0.59403 1.16725 0.76792 1.00000 0.01951 0.01948 0.02019 0.00627 0.00439 0.00397 0.02130 0.00402 0.00019 0.00017 0.00016 0.00000 0.00078 0.00077 0.00077 0.00063 0.00065 0.00064 0.00033 H15 0.68733 1.24502 0.82811 1.00000 0.02556 0.00000 0.00000 C16 0.44902 1.18091 0.74889 1.00000 0.02595 0.01960 0.02940 0.00281 0.00793 0.01058 0.02638 0.00422 0.00019 0.00017 0.00017 0.00000 0.00088 0.00080 0.00088 0.00069 0.00075 0.00071 0.00037 H16 0.44295 1.26810 0.79690 1.00000 0.03166 0.00000 0.00000 C17 0.31207 1.06791 0.65996 1.00000 0.01834 0.02017 0.02901 0.00570 0.00743 0.00911 0.02310 0.00406 0.00019 0.00017 0.00017 0.00000 0.00078 0.00079 0.00086 0.00068 0.00070 0.00067 0.00035 H17 0.21240 1.07648 0.64842 1.00000 0.02772 0.00000 0.00000 N1 0.18233 0.82784 0.49234 1.00000 0.01563 0.01478 0.01853 0.00629 0.00516 0.00622 0.01643 0.00314 0.00014 0.00013 0.00012 0.00000 0.00063 0.00061 0.00062 0.00051 0.00053 0.00052 0.00027 O1 0.23249 0.64817 0.56719 1.00000 0.02206 0.01996 0.02129 0.00985 0.00455 0.00728 0.02158 0.00272 0.00013 0.00011 0.00011 0.00000 0.00058 0.00056 0.00056 0.00047 0.00048 0.00048 0.00025 O2 0.06534 0.95673 0.37680 1.00000 0.02103 0.01801 0.02444 0.00938 0.00750 0.00940 0.02060 0.00274 0.00012 0.00011 0.00011 0.00000 0.00057 0.00055 0.00057 0.00046 0.00048 0.00046 0.00025 O3 0.05319 0.59288 0.18375 1.00000 0.01865 0.01926 0.02037 0.01020 0.00786 0.01041 0.01793 0.00264 0.00012 0.00011 0.00010 0.00000 0.00055 0.00054 0.00053 0.00045 0.00046 0.00046 0.00024 O4 0.04415 0.80059 0.07003 1.00000 0.02393 0.02744 0.02638 0.01319 0.01127 0.01075 0.02442 0.00295 0.00013 0.00012 0.00011 0.00000 0.00061 0.00062 0.00060 0.00051 0.00051 0.00051 0.00027 O5 -0.19572 0.78436 0.06994 1.00000 0.02359 0.03044 0.02646 0.01727 0.01111 0.01608 0.02365 0.00296 0.00013 0.00012 0.00011 0.00000 0.00060 0.00063 0.00059 0.00051 0.00050 0.00051 0.00026 S1_a 0.31163 0.49231 0.29806 0.49441 0.02396 0.02321 0.03087 0.01464 0.00957 0.01356 0.02418 0.00694 0.00028 0.00026 0.00029 0.00269 0.00076 0.00097 0.00061 0.00063 0.00055 0.00074 0.00042 C18_a 0.12200 0.42125 0.28267 0.49441 0.02033 0.01675 0.01956 0.00629 0.00665 0.00805 0.01888 0.18897 0.00790 0.00774 0.00911 0.00269 0.00101 0.00085 0.00172 0.00095 0.00093 0.00083 0.00058 C19_a 0.35592 0.37815 0.34601 0.49441 0.02568 0.01565 0.03111 0.01326 0.00864 0.01382 0.02241 0.06826 0.00249 0.00209 0.00324 0.00269 0.00121 0.00492 0.00210 0.00359 0.00129 0.00247 0.00164 H19_a 0.46261 0.38539 0.36915 0.49441 0.02689 0.00269 0.00000 C20_a 0.26082 0.26569 0.36006 0.49441 0.01689 0.02350 0.02734 0.00582 0.00832 0.01639 0.02141 0.05737 0.00203 0.00238 0.00249 0.00269 0.00359 0.00312 0.00361 0.00240 0.00310 0.00287 0.00229 H20_a 0.28100 0.18885 0.38588 0.49441 0.02570 0.00269 0.00000 C21_a 0.10427 0.30414 0.31925 0.49441 0.02454 0.02701 0.03219 0.00456 0.00822 0.00770 0.03011 0.02146 0.00096 0.00083 0.00097 0.00269 0.00313 0.00356 0.00253 0.00247 0.00226 0.00248 0.00181 H21_a 0.00880 0.25049 0.32051 0.49441 0.03613 0.00269 0.00000 S2_b 0.06861 0.26904 0.32104 0.50559 0.02492 0.01737 0.02738 0.00983 0.01176 0.01162 0.02157 0.00506 0.00022 0.00019 0.00023 0.00269 0.00086 0.00073 0.00054 0.00054 0.00057 0.00061 0.00038 C118_b 0.12308 0.42188 0.28450 0.50559 0.02033 0.01675 0.01956 0.00629 0.00665 0.00805 0.01888 0.18494 0.00774 0.00758 0.00891 0.00269 0.00101 0.00085 0.00172 0.00095 0.00093 0.00083 0.00058 C119_b 0.23538 0.26620 0.36110 0.50559 0.02592 0.02289 0.02993 0.01525 0.01957 0.01406 0.02168 0.05697 0.00189 0.00226 0.00246 0.00269 0.00587 0.00312 0.00342 0.00246 0.00437 0.00361 0.00253 H119_b 0.25449 0.19456 0.39659 0.50559 0.02601 0.00269 0.00000 C120_b 0.36004 0.35519 0.35155 0.50559 0.02568 0.01565 0.03111 0.01326 0.00864 0.01382 0.02241 0.06673 0.00240 0.00206 0.00318 0.00269 0.00121 0.00492 0.00210 0.00359 0.00129 0.00247 0.00164 H120_b 0.46377 0.35506 0.36881 0.50559 0.02689 0.00269 0.00000 C121_b 0.27610 0.45984 0.30206 0.50559 0.05197 0.02114 0.03726 0.01589 0.01266 0.01363 0.03668 0.02652 0.00108 0.00098 0.00117 0.00269 0.00604 0.00404 0.00297 0.00277 0.00351 0.00361 0.00259 H121_b 0.32866 0.54096 0.28646 0.50559 0.04402 0.00269 0.00000 Final Structure Factor Calculation for 2008src0842 in P-1 Total number of l.s. parameters = 288 Maximum vector length = 511 Memory required = 3437 / 24017 wR2 = 0.1126 before cycle 16 for 4327 data and 0 / 288 parameters Summary of restraints applied in cycle 16 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 11. 0. 0. 0. 5. 24. 12. 0. rms sigma 0.000 0.000 0.000 0.031 0.000 0.000 0.000 0.010 0.010 0.010 0.000 rms deviation 0.000 0.000 0.000 0.009 0.000 0.000 0.000 0.013 0.006 0.001 0.000 GooF = S = 1.054; Restrained GooF = 1.050 for 52 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0527 * P )^2 + 0.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0427 for 3334 Fo > 4sig(Fo) and 0.0626 for all 4327 data wR2 = 0.1126, GooF = S = 1.054, Restrained GooF = 1.050 for all data Occupancy sum of asymmetric unit = 28.00 for non-hydrogen and 19.00 for hydrogen atoms Principal mean square atomic displacements U 0.0199 0.0164 0.0146 C1 0.0199 0.0170 0.0129 C2 0.0196 0.0172 0.0140 C3 0.0193 0.0163 0.0148 C4 0.0209 0.0191 0.0142 C5 0.0273 0.0195 0.0176 C6 0.0291 0.0203 0.0172 C7 0.0218 0.0197 0.0117 C8 0.0248 0.0177 0.0137 C9 0.0451 0.0322 0.0126 C10 0.1320 0.0389 0.0153 C11 0.0199 0.0153 0.0148 C12 0.0223 0.0195 0.0164 C13 0.0238 0.0228 0.0155 C14 0.0262 0.0208 0.0169 C15 0.0379 0.0251 0.0161 C16 0.0331 0.0209 0.0153 C17 0.0202 0.0159 0.0132 N1 0.0288 0.0208 0.0152 O1 0.0258 0.0218 0.0141 O2 0.0225 0.0192 0.0121 O3 0.0297 0.0224 0.0211 O4 0.0344 0.0227 0.0138 O5 0.0327 0.0266 0.0132 S1_a 0.0223 0.0191 0.0152 C18_a 0.0337 0.0272 0.0063 C19_a 0.0346 0.0248 0.0048 C20_a 0.0398 0.0268 0.0237 C21_a 0.0277 0.0240 0.0130 S2_b 0.0223 0.0191 0.0152 C118_b 0.0351 0.0165 0.0135 C119_b 0.0337 0.0272 0.0063 C120_b 0.0572 0.0375 0.0154 C121_b Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.012 0.023 0.036 0.050 0.064 0.082 0.105 0.137 0.190 1.000 Number in group 469. 401. 449. 413. 453. 413. 429. 442. 424. 434. GooF 0.879 0.967 1.137 1.196 1.121 1.101 1.047 0.986 1.049 1.035 K 1.597 0.944 0.873 0.909 0.963 0.984 0.986 1.016 1.030 0.992 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.65 inf Number in group 445. 434. 430. 428. 432. 430. 431. 430. 431. 436. GooF 0.934 1.012 0.992 1.017 1.060 1.105 1.069 0.917 1.028 1.347 K 1.013 1.009 0.995 1.002 1.020 1.014 1.023 1.026 1.024 0.966 R1 0.137 0.124 0.130 0.092 0.075 0.057 0.041 0.033 0.032 0.037 Recommended weighting scheme: WGHT 0.0535 0.3332 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 4 4 3 18.23 42.05 5.19 0.063 1.09 6 5 0 4.45 18.38 4.24 0.042 0.98 -5 -5 3 52.00 30.28 4.20 0.054 1.21 4 5 2 49.44 80.94 4.08 0.088 1.07 3 3 5 29.33 51.50 4.02 0.070 1.11 4 -4 2 269.94 206.49 3.96 0.140 1.77 1 -4 9 38.25 74.80 3.87 0.084 1.12 -10 8 2 6.07 18.44 3.76 0.042 0.85 -5 2 1 41.27 27.17 3.48 0.051 1.88 6 4 1 57.90 84.64 3.47 0.090 1.01 4 -10 10 -7.17 23.05 3.43 0.047 0.78 -3 4 3 163.81 126.63 3.42 0.110 1.82 -2 5 3 22.81 13.06 3.42 0.035 1.58 2 -4 1 56.41 78.30 3.41 0.086 2.45 1 1 0 4859.59 5969.55 3.31 0.753 5.43 -1 -9 4 65.67 44.80 3.30 0.065 1.07 8 -11 4 -0.94 9.77 3.27 0.030 0.79 3 -9 9 12.85 34.66 3.25 0.057 0.89 -6 8 8 38.92 61.17 3.19 0.076 0.82 -2 3 4 7.88 15.73 3.19 0.039 1.87 -7 2 3 200.35 160.41 3.14 0.123 1.36 5 3 3 286.43 364.38 3.13 0.186 1.07 0 1 2 8724.02 10519.91 3.12 1.000 3.85 -2 0 3 18.01 10.70 3.12 0.032 3.31 -6 1 10 -0.07 7.81 3.10 0.027 1.00 -6 5 0 16.24 8.48 3.10 0.028 1.39 4 -6 9 37.07 60.09 3.07 0.076 0.92 -6 -4 13 19.34 35.99 3.06 0.058 0.82 2 1 1 61.18 82.03 3.05 0.088 2.88 2 6 5 4.49 14.01 3.03 0.036 0.93 1 1 5 14.12 5.21 3.03 0.022 1.64 -9 8 5 -4.81 7.47 3.02 0.027 0.86 0 5 1 46.75 65.41 3.00 0.079 1.73 -9 5 1 14.51 24.24 3.00 0.048 1.01 0 -5 4 444.41 367.11 2.97 0.187 1.84 -6 -5 5 -0.83 4.78 2.96 0.021 1.10 3 -6 1 20.52 12.35 2.95 0.034 1.64 -1 0 2 1479.12 1758.48 2.93 0.409 5.27 -2 0 1 90.63 115.46 2.92 0.105 4.63 -5 -8 1 6.06 16.87 2.88 0.040 0.87 -7 4 1 35.22 49.60 2.88 0.069 1.30 -3 2 1 6.00 2.39 2.87 0.015 2.95 -2 -2 2 96.78 122.89 2.85 0.108 3.03 -2 5 1 149.28 118.80 2.84 0.106 1.88 2 9 4 67.44 39.41 2.84 0.061 0.78 3 -10 3 26.48 42.61 2.83 0.064 1.03 -5 3 11 115.00 82.48 2.81 0.089 0.88 -1 -1 2 6032.96 7116.24 2.78 0.822 4.94 -1 -8 11 56.46 80.69 2.78 0.088 0.88 2 -1 2 58.09 42.35 2.77 0.063 2.99 Bond lengths and angles C1 - Distance Angles O1 1.2112 (0.0018) N1 1.4003 (0.0019) 123.84 (0.14) C4 1.5105 (0.0021) 127.49 (0.14) 108.67 (0.12) C1 - O1 N1 C2 - Distance Angles O2 1.2114 (0.0018) N1 1.3945 (0.0019) 125.28 (0.14) C3 1.5166 (0.0021) 126.32 (0.14) 108.40 (0.12) C2 - O2 N1 C3 - Distance Angles C2 1.5166 (0.0021) C4 1.5358 (0.0020) 105.23 (0.12) C8 1.5558 (0.0021) 112.33 (0.12) 101.56 (0.11) H3 1.0000 112.34 112.34 112.34 C3 - C2 C4 C8 C4 - Distance Angles C1 1.5105 (0.0021) C3 1.5358 (0.0020) 104.99 (0.12) C5 1.5641 (0.0020) 113.84 (0.12) 101.65 (0.11) H4 1.0000 111.90 111.90 111.90 C4 - C1 C3 C5 C5 - Distance Angles O3 1.4499 (0.0018) C18_a 1.4897 (0.0090) 111.03 (4.38) C118_b 1.4961 (0.0084) 111.27 (4.27) 0.66 (7.10) C6 1.5469 (0.0021) 103.01 (0.12) 115.88 (3.04) 116.32 (2.97) C4 1.5641 (0.0020) 101.68 (0.11) 116.11 (3.63) 115.45 (3.54) 107.44 (0.12) C5 - O3 C18_a C118_b C6 C6 - Distance Angles C5 1.5469 (0.0021) C7 1.5504 (0.0022) 101.47 (0.12) H6A 0.9900 111.48 111.48 H6B 0.9900 111.48 111.48 109.31 C6 - C5 C7 H6A C7 - Distance Angles C8 1.5398 (0.0022) C6 1.5504 (0.0022) 101.45 (0.12) H7A 0.9900 111.48 111.48 H7B 0.9900 111.48 111.48 109.31 C7 - C8 C6 H7A C8 - Distance Angles O3 1.4390 (0.0017) C9 1.5135 (0.0021) 110.85 (0.12) C7 1.5398 (0.0022) 103.32 (0.11) 115.76 (0.13) C3 1.5558 (0.0021) 101.98 (0.11) 114.85 (0.12) 108.59 (0.12) C8 - O3 C9 C7 C9 - Distance Angles O4 1.2012 (0.0019) O5 1.3368 (0.0018) 125.31 (0.14) C8 1.5135 (0.0021) 125.53 (0.14) 109.17 (0.12) C9 - O4 O5 C10 - Distance Angles O5 1.4653 (0.0019) C11 1.4959 (0.0026) 107.68 (0.15) H10A 0.9900 110.17 110.17 H10B 0.9900 110.17 110.17 108.47 C10 - O5 C11 H10A C11 - Distance Angles C10 1.4959 (0.0026) H11A 0.9800 109.47 H11B 0.9800 109.47 109.47 H11C 0.9800 109.47 109.47 109.47 C11 - C10 H11A H11B C12 - Distance Angles C13 1.3851 (0.0021) C17 1.3863 (0.0021) 121.10 (0.14) N1 1.4352 (0.0019) 119.71 (0.13) 119.19 (0.13) C12 - C13 C17 C13 - Distance Angles C14 1.3840 (0.0022) C12 1.3851 (0.0021) 119.07 (0.14) H13 0.9500 120.46 120.46 C13 - C14 C12 C14 - Distance Angles C13 1.3840 (0.0022) C15 1.3869 (0.0022) 120.67 (0.14) H14 0.9500 119.67 119.67 C14 - C13 C15 C15 - Distance Angles C16 1.3833 (0.0022) C14 1.3869 (0.0022) 119.62 (0.15) H15 0.9500 120.19 120.19 C15 - C16 C14 C16 - Distance Angles C15 1.3833 (0.0022) C17 1.3905 (0.0023) 120.47 (0.14) H16 0.9500 119.77 119.77 C16 - C15 C17 C17 - Distance Angles C12 1.3863 (0.0021) C16 1.3905 (0.0023) 119.02 (0.14) H17 0.9500 120.49 120.49 C17 - C12 C16 N1 - Distance Angles C2 1.3945 (0.0019) C1 1.4003 (0.0019) 112.65 (0.12) C12 1.4352 (0.0019) 123.79 (0.12) 123.56 (0.12) N1 - C2 C1 O1 - Distance Angles C1 1.2112 (0.0018) O1 - O2 - Distance Angles C2 1.2114 (0.0018) O2 - O3 - Distance Angles C8 1.4390 (0.0017) C5 1.4499 (0.0018) 96.99 (0.10) O3 - C8 O4 - Distance Angles C9 1.2012 (0.0019) O4 - O5 - Distance Angles C9 1.3368 (0.0018) C10 1.4653 (0.0019) 115.24 (0.12) O5 - C9 S1_a - Distance Angles C19_a 1.5063 (0.0158) C18_a 1.7158 (0.0894) 91.66 (2.01) S1_a - C19_a C18_a - Distance Angles C21_a 1.3567 (0.0825) C5 1.4897 (0.0090) 127.98 (7.04) S1_a 1.7158 (0.0889) 110.00 (1.06) 121.61 (5.69) C18_a - C21_a C5 C19_a - Distance Angles C20_a 1.3627 (0.0109) S1_a 1.5063 (0.0158) 127.58 (1.97) H19_a 0.9500 116.21 116.21 C19_a - C20_a S1_a C20_a - Distance Angles C19_a 1.3627 (0.0108) C21_a 1.6009 (0.0173) 97.61 (1.83) H20_a 0.9500 131.19 131.19 C20_a - C19_a C21_a C21_a - Distance Angles C18_a 1.3567 (0.0826) C20_a 1.6009 (0.0174) 113.05 (2.89) H21_a 0.9500 123.48 123.47 C21_a - C18_a C20_a S2_b - Distance Angles C119_b 1.5267 (0.0149) C118_b 1.7231 (0.0898) 91.31 (1.77) S2_b - C119_b C118_b - Distance Angles C121_b 1.3543 (0.0786) C5 1.4961 (0.0084) 130.79 (6.57) S2_b 1.7231 (0.0894) 110.00 (1.29) 119.06 (5.70) C118_b - C121_b C5 C119_b - Distance Angles C120_b 1.3647 (0.0111) S2_b 1.5267 (0.0149) 127.19 (1.74) H119_b 0.9500 116.40 116.40 C119_b - C120_b S2_b C120_b - Distance Angles C119_b 1.3647 (0.0110) C121_b 1.6001 (0.0169) 97.62 (1.71) H120_b 0.9500 131.19 131.19 C120_b - C119_b C121_b C121_b - Distance Angles C118_b 1.3543 (0.0788) C120_b 1.6001 (0.0169) 113.67 (2.96) H121_b 0.9500 123.17 123.16 C121_b - C118_b C120_b FMAP and GRID set by program FMAP 2 1 25 GRID -2.273 -2 -2 2.273 2 2 R1 = 0.0623 for 4327 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.24 at 0.3024 0.9403 -0.0032 [ 0.78 A from H11B ] Deepest hole -0.28 at 0.0179 0.7424 0.1228 [ 0.80 A from C9 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 3335 / 23292 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.3024 1.0597 0.0032 1.00000 0.05 0.24 0.78 H11B 1.39 C11 1.63 H11C 2.15 H10B Q2 1 0.0108 0.5383 0.3208 1.00000 0.05 0.23 0.79 C5 0.81 C4 1.47 H4 1.85 C118 Q3 1 0.1294 0.8389 0.4591 1.00000 0.05 0.21 0.58 N1 0.83 C2 1.72 C1 1.81 O2 Q4 1 -0.0701 0.4409 0.2102 1.00000 0.05 0.21 0.72 C5 0.85 C6 1.45 H6A 1.51 H6B Q5 1 -0.0709 0.6789 0.2404 1.00000 0.05 0.20 0.77 C3 0.80 C8 1.47 H3 1.81 O3 Shortest distances between peaks (including symmetry equivalents) 2 4 1.24 2 5 2.07 4 5 2.40 3 5 2.43 2 3 2.85 Time profile in seconds ----------------------- 0.17: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: 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. 0.95: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.03: OSF, H-atoms from difference map 0.05: Set up l.s. refinement 0.00: Generate idealized H-atoms 2.33: Structure factors and derivatives 9.14: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.11: Apply other restraints 1.13: Solve l.s. equations 0.00: Generate HTAB table 0.06: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.00: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008src0842 finished at 10:24:37 Total CPU time: 14.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++