++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXTL XLMP CRYSTAL STRUCTURE REFINEMENT - MULTI-CPU VERSION + + Copyright(c) Bruker AXS Inc. 1993-2014 Version 2014/7 + + marc003 started at 14:45:17 on 17-Aug-2015 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Command line parameters: marc003 -a50000 -b3000 -c624 -t2 -a sets the approximate maximum number of atoms including hydrogens. -b sets the maximum number of full-matrix parameters (leave unchanged for CGLS). For example -b9000 allows refinement of 1000 anisotropic atoms or 3000 with BLOC 1. For a 32-bit version, -b times the square root of the number of threads should not exceed about 65500. -c sets the reflection buffer size. This depends on the CPU cache size but will rarely need changing. -t sets the number of threads, otherwise the multi-CPU version sets this equal to the number of available CPUs. For optimal performance on systems with hyperthreading, usually the hyperthreading should be switched off or -t used to halve the number of threads; e.g. -t4 rather than -t8 for an Intel i7 processor. Running 2 threads on 2 processors marc003.res created by SHELXL-2014/7 TITL marc003 in P2(1)/c CELL 0.71073 17.27970 6.93830 21.12070 90.0000 104.0129 90.0000 ZERR 4.00 0.00260 0.00110 0.00330 0.0000 0.0024 0.0000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H O UNIT 112 120 28 V = 2456.84 F(000) = 1016.0 Mu = 0.09 mm-1 Cell Wt = 1914.07 Rho = 1.294 OMIT 1 0 0 ACTA CONF L.S. 10 BOND $H FMAP 2 PLAN 20 SIZE 0.287 0.31 0.322 TEMP -73.150 HTAB EADP C12 C12' EADP C22 C22' EADP C21 C21' SADI O6 C12 O6 C12' SADI C21 C22 C21' C22' SADI O5 C21 O5 C21' SADI O5 C22 O5 C22' EQIV $1 x, y+1, z EQIV $2 -x+1, y+1/2, -z+3/2 HTAB O1 O7_$2 EQIV $3 x, y-1, z HTAB O2 O4_$3 EQIV $4 -x+1, -y+1, -z+1 HTAB O3 O4_$4 WGHT 0.034800 FVAR 0.38034 0.72301 0.64934 C1 1 0.302103 0.342262 0.577165 11.00000 0.02543 0.02342 = 0.02796 -0.00377 0.00194 -0.00243 C2 1 0.366001 0.217347 0.555426 11.00000 0.02597 0.02504 = 0.02740 -0.00562 0.00060 -0.00274 C3 1 0.399547 0.361282 0.513297 11.00000 0.02741 0.03078 = 0.03048 -0.00073 0.00768 0.00286 AFIX 13 H3A 2 0.433094 0.461697 0.541025 11.00000 -1.20000 AFIX 0 C4 1 0.324220 0.449144 0.470743 11.00000 0.02777 0.02838 = 0.02739 0.00037 0.00299 0.00023 AFIX 13 H4 2 0.300881 0.355643 0.435215 11.00000 -1.20000 AFIX 0 C5 1 0.265309 0.470492 0.515895 11.00000 0.02621 0.02607 = 0.03013 -0.00128 0.00449 0.00065 AFIX 13 H5 2 0.269803 0.607048 0.531503 11.00000 -1.20000 AFIX 0 C6 1 0.197183 0.349730 0.639725 11.00000 0.03426 0.02465 = 0.03835 -0.00102 0.00854 0.00026 AFIX 43 H6 2 0.204239 0.485585 0.640976 11.00000 -1.20000 AFIX 0 C7 1 0.142753 0.270524 0.670703 11.00000 0.03190 0.03374 = 0.03966 -0.00484 0.01280 0.00075 AFIX 43 H7 2 0.113096 0.351200 0.692515 11.00000 -1.20000 AFIX 0 C8 1 0.131851 0.073498 0.669690 11.00000 0.03228 0.03717 = 0.03999 -0.00046 0.01075 -0.00699 C9 1 0.174760 -0.039247 0.636499 11.00000 0.04399 0.02785 = 0.06462 -0.00713 0.02213 -0.00880 AFIX 43 H9 2 0.167126 -0.174920 0.634927 11.00000 -1.20000 AFIX 0 C10 1 0.228427 0.041821 0.605649 11.00000 0.03820 0.02889 = 0.05043 -0.01027 0.01807 -0.00475 AFIX 43 H10 2 0.256999 -0.038910 0.582929 11.00000 -1.20000 AFIX 0 C11 1 0.241659 0.239964 0.607095 11.00000 0.02507 0.02634 = 0.02526 -0.00161 0.00093 -0.00063 PART 1 C12 1 0.035983 0.092183 0.734739 21.00000 0.08366 0.06210 = 0.10654 -0.01190 0.07202 -0.01993 AFIX 137 H12A 2 0.072593 0.159711 0.770564 21.00000 -1.50000 H12B 2 0.000830 0.008076 0.752492 21.00000 -1.50000 H12C 2 0.003801 0.186579 0.705153 21.00000 -1.50000 AFIX 0 PART 2 C12' 1 0.070120 0.077128 0.757698 -21.00000 0.08366 0.06210 = 0.10654 -0.01190 0.07202 -0.01993 AFIX 137 H12D 2 0.122272 0.115381 0.784799 -21.00000 -1.50000 H12E 2 0.043818 -0.009588 0.782581 -21.00000 -1.50000 H12F 2 0.037070 0.192031 0.744834 -21.00000 -1.50000 AFIX 0 PART 0 C13 1 0.490649 0.227007 0.649995 11.00000 0.02952 0.02277 = 0.03682 0.00007 0.00465 -0.00043 AFIX 43 H13 2 0.490859 0.363547 0.646686 11.00000 -1.20000 AFIX 0 C14 1 0.551028 0.136547 0.695224 11.00000 0.02685 0.02875 = 0.03344 -0.00489 0.00047 -0.00128 AFIX 43 H14 2 0.591128 0.210973 0.723470 11.00000 -1.20000 AFIX 0 C15 1 0.552958 -0.062472 0.699284 11.00000 0.02720 0.03052 = 0.02443 0.00102 0.00375 0.00420 C16 1 0.491743 -0.169113 0.661126 11.00000 0.03917 0.02402 = 0.03027 0.00134 0.00351 0.00009 AFIX 43 H16 2 0.491189 -0.305408 0.665290 11.00000 -1.20000 AFIX 0 C17 1 0.431102 -0.076169 0.616708 11.00000 0.02877 0.02775 = 0.03006 -0.00145 0.00272 -0.00329 AFIX 43 H17 2 0.389279 -0.150913 0.590586 11.00000 -1.20000 AFIX 0 C18 1 0.429428 0.122657 0.609102 11.00000 0.02563 0.02515 = 0.02762 -0.00171 0.00574 0.00060 C19 1 0.633080 -0.343718 0.733056 11.00000 0.04765 0.03596 = 0.04478 -0.00210 -0.00339 0.01798 AFIX 137 H19A 2 0.593148 -0.421242 0.747498 11.00000 -1.50000 H19B 2 0.686472 -0.378008 0.758793 11.00000 -1.50000 H19C 2 0.629508 -0.368936 0.686782 11.00000 -1.50000 AFIX 0 C20 1 0.335953 0.638202 0.440073 11.00000 0.02905 0.03352 = 0.02937 -0.00043 0.00768 0.00673 PART 1 C21 1 0.270195 0.869504 0.362052 31.00000 0.05170 0.04436 = 0.04886 0.02106 0.00606 0.00322 AFIX 23 H21A 2 0.324336 0.916161 0.362044 31.00000 -1.20000 H21B 2 0.245833 0.960434 0.387735 31.00000 -1.20000 AFIX 0 C22 1 0.220320 0.854985 0.294036 31.00000 0.08536 0.08742 = 0.05108 0.03299 -0.00861 -0.00643 AFIX 137 H22A 2 0.245267 0.765113 0.269159 31.00000 -1.50000 H22B 2 0.215794 0.982339 0.273398 31.00000 -1.50000 H22C 2 0.167072 0.807946 0.294784 31.00000 -1.50000 AFIX 0 PART 2 C21' 1 0.270594 0.860550 0.357399 -31.00000 0.05170 0.04436 = 0.04886 0.02106 0.00606 0.00322 AFIX 23 H21C 2 0.306150 0.861202 0.327020 -31.00000 -1.20000 H21D 2 0.287128 0.965493 0.389595 -31.00000 -1.20000 AFIX 0 C22' 1 0.185297 0.886370 0.320711 -31.00000 0.08536 0.08742 = 0.05108 0.03299 -0.00861 -0.00643 AFIX 137 H22D 2 0.171393 0.788420 0.286401 -31.00000 -1.50000 H22E 2 0.178286 1.014948 0.300941 -31.00000 -1.50000 H22F 2 0.150509 0.872604 0.350832 -31.00000 -1.50000 AFIX 0 PART 0 C23 1 0.126081 0.593082 0.472331 11.00000 0.03439 0.04737 = 0.04395 0.00297 0.00493 0.00730 AFIX 43 H23 2 0.144234 0.715492 0.490015 11.00000 -1.20000 AFIX 0 C24 1 0.047098 0.570961 0.438793 11.00000 0.03700 0.07147 = 0.05632 0.00565 0.00288 0.01404 AFIX 43 H24 2 0.011599 0.677524 0.433676 11.00000 -1.20000 AFIX 0 C25 1 0.020376 0.395735 0.413110 11.00000 0.02953 0.08614 = 0.05161 0.00700 -0.00004 -0.00192 AFIX 43 H25 2 -0.033680 0.380683 0.389851 11.00000 -1.20000 AFIX 0 C26 1 0.071539 0.240992 0.420836 11.00000 0.03817 0.06179 = 0.05103 -0.00164 -0.00252 -0.00978 AFIX 43 H26 2 0.052727 0.118922 0.403250 11.00000 -1.20000 AFIX 0 C27 1 0.150359 0.263196 0.454210 11.00000 0.03159 0.04637 = 0.04650 -0.00160 0.00325 -0.00122 AFIX 43 H27 2 0.185487 0.155923 0.459231 11.00000 -1.20000 AFIX 0 C28 1 0.178889 0.440582 0.480531 11.00000 0.02854 0.04103 = 0.02661 0.00358 0.00574 0.00086 O1 3 0.344840 0.481516 0.623385 11.00000 0.03488 0.02497 = 0.02720 -0.00295 0.00265 -0.00390 AFIX 147 H1 2 0.356397 0.432630 0.660884 11.00000 -1.20000 AFIX 0 O2 3 0.323846 0.073828 0.511673 11.00000 0.02952 0.02887 = 0.03155 -0.00906 0.00416 0.00062 AFIX 147 H2 2 0.354966 0.022210 0.491684 11.00000 -1.20000 AFIX 0 O3 3 0.442391 0.267961 0.472606 11.00000 0.03011 0.04679 = 0.03817 0.00049 0.01049 0.00757 AFIX 147 H3 2 0.490538 0.257521 0.492599 11.00000 -1.20000 AFIX 0 O4 3 0.391049 0.748159 0.458867 11.00000 0.03317 0.03232 = 0.04404 0.00170 0.00750 -0.00083 O5 3 0.274199 0.676186 0.390041 11.00000 0.03860 0.04993 = 0.04331 0.01884 -0.00394 -0.00332 O6 3 0.080781 -0.021274 0.699762 11.00000 0.05883 0.04340 = 0.06951 -0.00499 0.03859 -0.01373 O7 3 0.618547 -0.142301 0.742014 11.00000 0.03714 0.02967 = 0.03317 0.00000 -0.00192 0.00649 HKLF 4 Covalent radii and connectivity table for marc003 in P2(1)/c C 0.770 H 0.320 O 0.660 C1 - O1 C11 C2 C5 C2 - O2 C18 C3 C1 C3 - O3 C4 C2 C4 - C20 C3 C5 C5 - C28 C4 C1 C6 - C11 C7 C7 - C8 C6 C8 - O6 C7 C9 C9 - C10 C8 C10 - C9 C11 C11 - C6 C10 C1 C12_a - O6 C12'_b - O6 C13 - C14 C18 C14 - C13 C15 C15 - C16 O7 C14 C16 - C15 C17 C17 - C16 C18 C18 - C17 C13 C2 C19 - O7 C20 - O4 O5 C4 C21_a - O5 C22_a C22_a - C21_a C21'_b - O5 C22'_b C22'_b - C21'_b C23 - C28 C24 C24 - C25 C23 C25 - C24 C26 C26 - C25 C27 C27 - C26 C28 C28 - C23 C27 C5 O1 - C1 O2 - C2 O3 - C3 O4 - C20 O5 - C20 C21'_b C21_a O6 - C8 C12_a C12'_b O7 - C15 C19 Operators for generating equivalent atoms: $2 -x+1, y+1/2, -z+3/2 $3 x, y-1, z $4 -x+1, -y+1, -z+1 25603 Reflections read, of which 1141 rejected -22 =< h =< 22, -9 =< k =< 9, -26 =< l =< 27, Max. 2-theta = 55.23 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 0 0 2 1647.15 6.13 5 30.91 0 1 2 2162.71 6.27 9 86.58 2 0 4 4526.47 20.71 3 110.62 3 Inconsistent equivalents 5682 Unique reflections, of which 0 suppressed R(int) = 0.0604 R(sigma) = 0.0818 Friedel opposites merged Maximum memory for data reduction = 4747 / 57401 Number of data for d > 0.767A (CIF: max) and d > 0.833A (CIF: full) (ignoring systematic absences): Unique reflections found (point group) 5682 4453 Unique reflections possible (point group) 5685 4454 Unique reflections found (Laue group) 5682 4453 Unique reflections possible (Laue group) 5685 4454 Default effective X-H and X-D distances for T = -73.2C 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 = 623 Memory required = 5763 / 501149 wR2 = 0.0908 before cycle 1 for 5682 data and 335 / 335 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU RIGU SIMU ISOR SUMP Number 0 0 0 4 0 0 0 0 0 0 0 0 rms sigma 0.0000 0.0000 0.0000 0.0200 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 rms deviation 0.0000 0.0000 0.0000 0.0158 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 GooF = S = 0.823; Restrained GooF = 0.823 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0348 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38034 0.00042 -0.005 OSF 2 0.72301 0.02343 0.000 FVAR 2 3 0.64934 0.00663 0.000 FVAR 3 Mean shift/esd = 0.002 Maximum = 0.007 for U12 O2 Max. shift = 0.000 A for H12B_a Max. dU = 0.000 for O1 Least-squares cycle 2 Maximum vector length = 623 Memory required = 5763 / 501149 wR2 = 0.0908 before cycle 2 for 5682 data and 335 / 335 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU RIGU SIMU ISOR SUMP Number 0 0 0 4 0 0 0 0 0 0 0 0 rms sigma 0.0000 0.0000 0.0000 0.0200 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 rms deviation 0.0000 0.0000 0.0000 0.0158 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 GooF = S = 0.823; Restrained GooF = 0.823 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0348 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38034 0.00042 0.000 OSF 2 0.72300 0.02343 0.000 FVAR 2 3 0.64934 0.00663 0.000 FVAR 3 Mean shift/esd = 0.001 Maximum = 0.002 for U12 O2 Max. shift = 0.000 A for H12E_b Max. dU = 0.000 for O1 Least-squares cycle 3 Maximum vector length = 623 Memory required = 5763 / 501149 wR2 = 0.0908 before cycle 3 for 5682 data and 335 / 335 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU RIGU SIMU ISOR SUMP Number 0 0 0 4 0 0 0 0 0 0 0 0 rms sigma 0.0000 0.0000 0.0000 0.0200 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 rms deviation 0.0000 0.0000 0.0000 0.0158 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 GooF = S = 0.823; Restrained GooF = 0.823 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0348 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38034 0.00042 0.000 OSF 2 0.72301 0.02343 0.000 FVAR 2 3 0.64934 0.00663 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = -0.001 for z O1 Max. shift = 0.000 A for H12E_b Max. dU = 0.000 for C12_a Least-squares cycle 4 Maximum vector length = 623 Memory required = 5763 / 501149 wR2 = 0.0908 before cycle 4 for 5682 data and 335 / 335 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU RIGU SIMU ISOR SUMP Number 0 0 0 4 0 0 0 0 0 0 0 0 rms sigma 0.0000 0.0000 0.0000 0.0200 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 rms deviation 0.0000 0.0000 0.0000 0.0158 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 GooF = S = 0.823; Restrained GooF = 0.823 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0348 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38034 0.00042 0.000 OSF 2 0.72301 0.02343 0.000 FVAR 2 3 0.64934 0.00663 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.001 for z C19 Max. shift = 0.000 A for C21'_b Max. dU = 0.000 for C12_a Least-squares cycle 5 Maximum vector length = 623 Memory required = 5763 / 501149 wR2 = 0.0908 before cycle 5 for 5682 data and 335 / 335 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU RIGU SIMU ISOR SUMP Number 0 0 0 4 0 0 0 0 0 0 0 0 rms sigma 0.0000 0.0000 0.0000 0.0200 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 rms deviation 0.0000 0.0000 0.0000 0.0158 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 GooF = S = 0.823; Restrained GooF = 0.823 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0348 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38034 0.00042 0.000 OSF 2 0.72301 0.02343 0.000 FVAR 2 3 0.64934 0.00663 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.001 for z O1 Max. shift = 0.000 A for H12F_b Max. dU = 0.000 for C12_a Least-squares cycle 6 Maximum vector length = 623 Memory required = 5763 / 501149 wR2 = 0.0908 before cycle 6 for 5682 data and 335 / 335 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU RIGU SIMU ISOR SUMP Number 0 0 0 4 0 0 0 0 0 0 0 0 rms sigma 0.0000 0.0000 0.0000 0.0200 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 rms deviation 0.0000 0.0000 0.0000 0.0158 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 GooF = S = 0.823; Restrained GooF = 0.823 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0348 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38034 0.00042 0.000 OSF 2 0.72301 0.02343 0.000 FVAR 2 3 0.64934 0.00663 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.001 for z C13 Max. shift = 0.000 A for C21'_b Max. dU = 0.000 for C21_a Least-squares cycle 7 Maximum vector length = 623 Memory required = 5763 / 501149 wR2 = 0.0908 before cycle 7 for 5682 data and 335 / 335 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU RIGU SIMU ISOR SUMP Number 0 0 0 4 0 0 0 0 0 0 0 0 rms sigma 0.0000 0.0000 0.0000 0.0200 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 rms deviation 0.0000 0.0000 0.0000 0.0158 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 GooF = S = 0.823; Restrained GooF = 0.823 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0348 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38034 0.00042 0.000 OSF 2 0.72301 0.02343 0.000 FVAR 2 3 0.64934 0.00663 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = -0.001 for z O1 Max. shift = 0.000 A for H12F_b Max. dU = 0.000 for C22_a Least-squares cycle 8 Maximum vector length = 623 Memory required = 5763 / 501149 wR2 = 0.0908 before cycle 8 for 5682 data and 335 / 335 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU RIGU SIMU ISOR SUMP Number 0 0 0 4 0 0 0 0 0 0 0 0 rms sigma 0.0000 0.0000 0.0000 0.0200 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 rms deviation 0.0000 0.0000 0.0000 0.0158 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 GooF = S = 0.823; Restrained GooF = 0.823 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0348 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38034 0.00042 0.000 OSF 2 0.72301 0.02343 0.000 FVAR 2 3 0.64934 0.00663 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.001 for z C17 Max. shift = 0.000 A for H12E_b Max. dU = 0.000 for C12_a Least-squares cycle 9 Maximum vector length = 623 Memory required = 5763 / 501149 wR2 = 0.0908 before cycle 9 for 5682 data and 335 / 335 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU RIGU SIMU ISOR SUMP Number 0 0 0 4 0 0 0 0 0 0 0 0 rms sigma 0.0000 0.0000 0.0000 0.0200 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 rms deviation 0.0000 0.0000 0.0000 0.0158 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 GooF = S = 0.823; Restrained GooF = 0.823 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0348 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38034 0.00042 0.000 OSF 2 0.72301 0.02343 0.000 FVAR 2 3 0.64934 0.00663 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.001 for z O1 Max. shift = 0.000 A for H12E_b Max. dU = 0.000 for C12_a Least-squares cycle 10 Maximum vector length = 623 Memory required = 5763 / 501149 wR2 = 0.0908 before cycle 10 for 5682 data and 335 / 335 parameters Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU RIGU SIMU ISOR SUMP Number 0 0 0 4 0 0 0 0 0 0 0 0 rms sigma 0.0000 0.0000 0.0000 0.0200 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 rms deviation 0.0000 0.0000 0.0000 0.0158 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 GooF = S = 0.823; Restrained GooF = 0.823 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0348 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38034 0.00042 0.000 OSF 2 0.72301 0.02343 0.000 FVAR 2 3 0.64934 0.00663 0.000 FVAR 3 Mean shift/esd = 0.000 Maximum = 0.001 for z C13 Max. shift = 0.000 A for H12E_b Max. dU = 0.000 for C12_a Largest correlation matrix elements -0.961 x C21'_b / x C21_a 0.810 x C12'_b / FVAR 2 -0.736 U33 C21_a / z C21_a -0.961 z C21'_b / z C21_a 0.794 U13 C12_a / U11 C12_a 0.735 U12 C12_a / y C12_a 0.952 x C12_a / FVAR 2 0.787 x C12'_b / z C12_a 0.723 U33 C12_a / z C12_a -0.943 y C21'_b / y C21_a 0.769 U13 C12_a / z C12_a -0.721 z C22'_b / x C22_a 0.926 z C12_a / FVAR 2 0.750 U11 C12_a / x C12_a 0.720 U13 C12_a / FVAR 2 0.886 z C12_a / x C12_a 0.747 U13 C12_a / x C12_a -0.713 x C22_a / FVAR 3 0.847 U13 C12_a / U33 C12_a -0.739 y C12'_b / U12 C12_a -0.699 y C12'_b / U23 C12_a 0.827 U12 C12_a / U23 C12_a 0.736 z C21'_b / U33 C21_a 0.688 U23 C12_a / y C12_a Idealized hydrogen atom generation before cycle 11 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3A 0.4331 0.4617 0.5410 13 1.000 0.000 C3 O3 C4 C2 H4 0.3009 0.3556 0.4352 13 1.000 0.000 C4 C20 C3 C5 H5 0.2698 0.6070 0.5315 13 1.000 0.000 C5 C28 C4 C1 H6 0.2042 0.4856 0.6410 43 0.950 0.000 C6 C11 C7 H7 0.1131 0.3512 0.6925 43 0.950 0.000 C7 C8 C6 H9 0.1671 -0.1749 0.6349 43 0.950 0.000 C9 C10 C8 H10 0.2570 -0.0389 0.5829 43 0.950 0.000 C10 C9 C11 H12A 0.0726 0.1597 0.7706 137 0.980 0.000 C12_a O6 H12A_a H12B 0.0008 0.0081 0.7525 137 0.980 0.000 C12_a O6 H12A_a H12C 0.0038 0.1866 0.7052 137 0.980 0.000 C12_a O6 H12A_a H12D 0.1223 0.1154 0.7848 137 0.980 0.000 C12'_b O6 H12D_b H12E 0.0438 -0.0096 0.7826 137 0.980 0.000 C12'_b O6 H12D_b H12F 0.0371 0.1920 0.7448 137 0.980 0.000 C12'_b O6 H12D_b H13 0.4909 0.3635 0.6467 43 0.950 0.000 C13 C14 C18 H14 0.5911 0.2110 0.7235 43 0.950 0.000 C14 C13 C15 H16 0.4912 -0.3054 0.6653 43 0.950 0.000 C16 C15 C17 H17 0.3893 -0.1509 0.5906 43 0.950 0.000 C17 C16 C18 H19A 0.5931 -0.4212 0.7475 137 0.980 0.000 C19 O7 H19A H19B 0.6865 -0.3780 0.7588 137 0.980 0.000 C19 O7 H19A H19C 0.6295 -0.3689 0.6868 137 0.980 0.000 C19 O7 H19A H21A 0.3243 0.9162 0.3620 23 0.990 0.000 C21_a O5 C22_a H21B 0.2458 0.9604 0.3877 23 0.990 0.000 C21_a O5 C22_a H22A 0.2453 0.7651 0.2692 137 0.980 0.000 C22_a C21_a H22A_a H22B 0.2158 0.9823 0.2734 137 0.980 0.000 C22_a C21_a H22A_a H22C 0.1671 0.8079 0.2948 137 0.980 0.000 C22_a C21_a H22A_a H21C 0.3061 0.8612 0.3270 23 0.990 0.000 C21'_b O5 C22'_b H21D 0.2871 0.9655 0.3896 23 0.990 0.000 C21'_b O5 C22'_b H22D 0.1714 0.7884 0.2864 137 0.980 0.000 C22'_b C21'_b H22D_b H22E 0.1783 1.0149 0.3009 137 0.980 0.000 C22'_b C21'_b H22D_b H22F 0.1505 0.8726 0.3508 137 0.980 0.000 C22'_b C21'_b H22D_b H23 0.1442 0.7155 0.4900 43 0.950 0.000 C23 C28 C24 H24 0.0116 0.6775 0.4337 43 0.950 0.000 C24 C25 C23 H25 -0.0337 0.3807 0.3899 43 0.950 0.000 C25 C24 C26 H26 0.0527 0.1189 0.4033 43 0.950 0.000 C26 C25 C27 H27 0.1855 0.1559 0.4592 43 0.950 0.000 C27 C26 C28 H1 0.3564 0.4326 0.6609 147 0.840 0.000 O1 C1 H1 H2 0.3550 0.0222 0.4917 147 0.840 0.000 O2 C2 H2 H3 0.4905 0.2575 0.4926 147 0.840 0.000 O3 C3 H3 marc003 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.30210 0.34226 0.57717 1.00000 0.02543 0.02342 0.02796 -0.00377 0.00194 -0.00243 0.02638 0.00286 0.00009 0.00022 0.00008 0.00000 0.00092 0.00084 0.00097 0.00080 0.00074 0.00070 0.00039 C2 0.36600 0.21735 0.55543 1.00000 0.02597 0.02504 0.02740 -0.00562 0.00060 -0.00274 0.02714 0.00281 0.00009 0.00022 0.00008 0.00000 0.00094 0.00090 0.00100 0.00079 0.00077 0.00069 0.00040 C3 0.39955 0.36128 0.51330 1.00000 0.02741 0.03078 0.03048 -0.00073 0.00768 0.00286 0.02944 0.00317 0.00009 0.00023 0.00008 0.00000 0.00098 0.00097 0.00102 0.00083 0.00080 0.00073 0.00041 H3A 0.43309 0.46170 0.54102 1.00000 0.03533 0.00000 0.00000 C4 0.32422 0.44914 0.47074 1.00000 0.02777 0.02838 0.02739 0.00037 0.00299 0.00023 0.02848 0.00300 0.00009 0.00022 0.00008 0.00000 0.00097 0.00092 0.00101 0.00080 0.00078 0.00071 0.00041 H4 0.30088 0.35564 0.43522 1.00000 0.03418 0.00000 0.00000 C5 0.26531 0.47049 0.51589 1.00000 0.02621 0.02607 0.03013 -0.00128 0.00449 0.00065 0.02787 0.00291 0.00009 0.00023 0.00008 0.00000 0.00097 0.00088 0.00102 0.00080 0.00079 0.00070 0.00040 H5 0.26980 0.60705 0.53150 1.00000 0.03344 0.00000 0.00000 C6 0.19718 0.34973 0.63972 1.00000 0.03426 0.02465 0.03835 -0.00102 0.00854 0.00026 0.03246 0.00306 0.00010 0.00024 0.00008 0.00000 0.00105 0.00091 0.00112 0.00086 0.00087 0.00075 0.00043 H6 0.20424 0.48559 0.64098 1.00000 0.03896 0.00000 0.00000 C7 0.14275 0.27052 0.67070 1.00000 0.03190 0.03374 0.03966 -0.00484 0.01280 0.00075 0.03439 0.00307 0.00009 0.00024 0.00008 0.00000 0.00104 0.00104 0.00117 0.00091 0.00088 0.00078 0.00044 H7 0.11310 0.35120 0.69251 1.00000 0.04127 0.00000 0.00000 C8 0.13185 0.07350 0.66969 1.00000 0.03228 0.03717 0.03999 -0.00046 0.01075 -0.00699 0.03614 0.00322 0.00010 0.00025 0.00009 0.00000 0.00108 0.00108 0.00117 0.00094 0.00089 0.00081 0.00045 C9 0.17476 -0.03925 0.63650 1.00000 0.04399 0.02785 0.06462 -0.00713 0.02213 -0.00880 0.04395 0.00343 0.00011 0.00025 0.00010 0.00000 0.00120 0.00099 0.00144 0.00102 0.00107 0.00085 0.00050 H9 0.16713 -0.17492 0.63493 1.00000 0.05273 0.00000 0.00000 C10 0.22843 0.04182 0.60565 1.00000 0.03820 0.02889 0.05043 -0.01027 0.01807 -0.00475 0.03792 0.00313 0.00010 0.00024 0.00009 0.00000 0.00112 0.00098 0.00128 0.00093 0.00096 0.00080 0.00047 H10 0.25700 -0.03891 0.58293 1.00000 0.04550 0.00000 0.00000 C11 0.24166 0.23996 0.60709 1.00000 0.02507 0.02634 0.02526 -0.00161 0.00093 -0.00063 0.02644 0.00283 0.00009 0.00023 0.00008 0.00000 0.00093 0.00089 0.00097 0.00078 0.00076 0.00071 0.00039 C12_a 0.03598 0.09218 0.73474 0.72301 0.08366 0.06210 0.10654 -0.01190 0.07202 -0.01993 0.07570 0.02646 0.00082 0.00083 0.00064 0.02343 0.00598 0.00202 0.00543 0.00285 0.00502 0.00311 0.00255 H12A_a 0.07259 0.15971 0.77056 0.72301 0.11355 0.02343 0.00000 H12B_a 0.00083 0.00808 0.75249 0.72301 0.11355 0.02343 0.00000 H12C_a 0.00380 0.18658 0.70515 0.72301 0.11355 0.02343 0.00000 C12'_b 0.07012 0.07713 0.75770 0.27699 0.08366 0.06210 0.10654 -0.01190 0.07202 -0.01993 0.07570 0.03971 0.00155 0.00283 0.00098 0.02343 0.00598 0.00202 0.00543 0.00285 0.00502 0.00311 0.00255 H12D_b 0.12227 0.11538 0.78480 0.27699 0.11355 0.02343 0.00000 H12E_b 0.04382 -0.00959 0.78258 0.27699 0.11355 0.02343 0.00000 H12F_b 0.03707 0.19203 0.74483 0.27699 0.11355 0.02343 0.00000 C13 0.49065 0.22701 0.65000 1.00000 0.02952 0.02277 0.03682 0.00007 0.00465 -0.00043 0.03028 0.00299 0.00009 0.00022 0.00008 0.00000 0.00099 0.00088 0.00109 0.00083 0.00083 0.00073 0.00042 H13 0.49086 0.36355 0.64669 1.00000 0.03634 0.00000 0.00000 C14 0.55103 0.13655 0.69522 1.00000 0.02685 0.02875 0.03344 -0.00489 0.00047 -0.00128 0.03085 0.00300 0.00009 0.00023 0.00008 0.00000 0.00098 0.00094 0.00107 0.00086 0.00080 0.00072 0.00042 H14 0.59113 0.21097 0.72347 1.00000 0.03702 0.00000 0.00000 C15 0.55296 -0.06247 0.69928 1.00000 0.02720 0.03052 0.02443 0.00102 0.00375 0.00420 0.02781 0.00300 0.00009 0.00023 0.00008 0.00000 0.00098 0.00096 0.00098 0.00081 0.00077 0.00073 0.00040 C16 0.49174 -0.16911 0.66113 1.00000 0.03917 0.02402 0.03027 0.00134 0.00351 0.00009 0.03199 0.00305 0.00010 0.00024 0.00008 0.00000 0.00108 0.00088 0.00105 0.00083 0.00086 0.00078 0.00042 H16 0.49119 -0.30541 0.66529 1.00000 0.03839 0.00000 0.00000 C17 0.43110 -0.07617 0.61671 1.00000 0.02877 0.02775 0.03006 -0.00145 0.00272 -0.00329 0.02961 0.00302 0.00009 0.00022 0.00008 0.00000 0.00097 0.00093 0.00104 0.00082 0.00079 0.00072 0.00041 H17 0.38928 -0.15091 0.59059 1.00000 0.03554 0.00000 0.00000 C18 0.42943 0.12266 0.60910 1.00000 0.02563 0.02515 0.02762 -0.00171 0.00574 0.00060 0.02626 0.00290 0.00009 0.00022 0.00008 0.00000 0.00094 0.00089 0.00100 0.00078 0.00076 0.00070 0.00039 C19 0.63308 -0.34372 0.73306 1.00000 0.04765 0.03596 0.04478 -0.00210 -0.00339 0.01798 0.04530 0.00335 0.00010 0.00024 0.00009 0.00000 0.00122 0.00108 0.00126 0.00099 0.00097 0.00088 0.00052 H19A 0.59315 -0.42124 0.74750 1.00000 0.06795 0.00000 0.00000 H19B 0.68647 -0.37801 0.75879 1.00000 0.06795 0.00000 0.00000 H19C 0.62951 -0.36894 0.68678 1.00000 0.06795 0.00000 0.00000 C20 0.33595 0.63820 0.44007 1.00000 0.02905 0.03352 0.02937 -0.00043 0.00768 0.00673 0.03054 0.00332 0.00010 0.00024 0.00008 0.00000 0.00104 0.00101 0.00104 0.00087 0.00083 0.00081 0.00041 C21_a 0.27019 0.86950 0.36205 0.64934 0.05170 0.04436 0.04886 0.02106 0.00606 0.00322 0.04935 0.01813 0.00062 0.00129 0.00056 0.00663 0.00139 0.00150 0.00207 0.00150 0.00116 0.00098 0.00093 H21A_a 0.32434 0.91616 0.36204 0.64934 0.05922 0.00663 0.00000 H21B_a 0.24583 0.96043 0.38774 0.64934 0.05922 0.00663 0.00000 C22_a 0.22032 0.85498 0.29404 0.64934 0.08536 0.08742 0.05108 0.03299 -0.00861 -0.00643 0.07893 0.00886 0.00036 0.00073 0.00025 0.00663 0.00424 0.00270 0.00339 0.00270 0.00220 0.00259 0.00165 H22A_a 0.24527 0.76511 0.26916 0.64934 0.11839 0.00663 0.00000 H22B_a 0.21579 0.98234 0.27340 0.64934 0.11839 0.00663 0.00000 H22C_a 0.16707 0.80795 0.29478 0.64934 0.11839 0.00663 0.00000 C21'_b 0.27059 0.86055 0.35740 0.35066 0.05170 0.04436 0.04886 0.02106 0.00606 0.00322 0.04935 0.03524 0.00108 0.00240 0.00110 0.00663 0.00139 0.00150 0.00207 0.00150 0.00116 0.00098 0.00093 H21C_b 0.30615 0.86120 0.32702 0.35066 0.05922 0.00663 0.00000 H21D_b 0.28713 0.96549 0.38959 0.35066 0.05922 0.00663 0.00000 C22'_b 0.18530 0.88637 0.32071 0.35066 0.08536 0.08742 0.05108 0.03299 -0.00861 -0.00643 0.07893 0.01908 0.00059 0.00145 0.00051 0.00663 0.00424 0.00270 0.00339 0.00270 0.00220 0.00259 0.00165 H22D_b 0.17139 0.78842 0.28640 0.35066 0.11839 0.00663 0.00000 H22E_b 0.17829 1.01495 0.30094 0.35066 0.11839 0.00663 0.00000 H22F_b 0.15051 0.87260 0.35083 0.35066 0.11839 0.00663 0.00000 C23 0.12608 0.59308 0.47233 1.00000 0.03439 0.04737 0.04395 0.00297 0.00493 0.00730 0.04268 0.00359 0.00010 0.00027 0.00009 0.00000 0.00115 0.00120 0.00125 0.00099 0.00093 0.00086 0.00050 H23 0.14423 0.71549 0.49002 1.00000 0.05122 0.00000 0.00000 C24 0.04710 0.57096 0.43879 1.00000 0.03700 0.07147 0.05632 0.00565 0.00288 0.01404 0.05637 0.00408 0.00011 0.00033 0.00010 0.00000 0.00130 0.00160 0.00148 0.00127 0.00108 0.00104 0.00060 H24 0.01160 0.67752 0.43368 1.00000 0.06765 0.00000 0.00000 C25 0.02038 0.39573 0.41311 1.00000 0.02953 0.08614 0.05161 0.00700 -0.00004 -0.00192 0.05745 0.00416 0.00012 0.00035 0.00010 0.00000 0.00121 0.00179 0.00144 0.00134 0.00101 0.00116 0.00062 H25 -0.03368 0.38068 0.38985 1.00000 0.06894 0.00000 0.00000 C26 0.07154 0.24099 0.42084 1.00000 0.03817 0.06179 0.05103 -0.00164 -0.00252 -0.00978 0.05262 0.00363 0.00011 0.00031 0.00010 0.00000 0.00123 0.00139 0.00137 0.00117 0.00102 0.00104 0.00056 H26 0.05273 0.11892 0.40325 1.00000 0.06314 0.00000 0.00000 C27 0.15036 0.26320 0.45421 1.00000 0.03159 0.04637 0.04650 -0.00160 0.00325 -0.00122 0.04255 0.00331 0.00010 0.00027 0.00009 0.00000 0.00110 0.00117 0.00126 0.00102 0.00093 0.00086 0.00049 H27 0.18549 0.15592 0.45923 1.00000 0.05106 0.00000 0.00000 C28 0.17889 0.44058 0.48053 1.00000 0.02855 0.04103 0.02661 0.00358 0.00574 0.00086 0.03222 0.00319 0.00010 0.00025 0.00008 0.00000 0.00101 0.00108 0.00101 0.00089 0.00079 0.00080 0.00042 O1 0.34484 0.48152 0.62339 1.00000 0.03488 0.02497 0.02720 -0.00295 0.00265 -0.00390 0.02985 0.00186 0.00006 0.00014 0.00005 0.00000 0.00068 0.00062 0.00067 0.00054 0.00057 0.00050 0.00028 H1 0.35640 0.43263 0.66088 1.00000 0.03582 0.00000 0.00000 O2 0.32385 0.07383 0.51167 1.00000 0.02952 0.02887 0.03155 -0.00906 0.00416 0.00062 0.03054 0.00184 0.00006 0.00015 0.00006 0.00000 0.00066 0.00064 0.00072 0.00055 0.00054 0.00049 0.00029 H2 0.35497 0.02221 0.49168 1.00000 0.03664 0.00000 0.00000 O3 0.44239 0.26796 0.47261 1.00000 0.03011 0.04679 0.03817 0.00049 0.01049 0.00757 0.03797 0.00215 0.00006 0.00017 0.00006 0.00000 0.00069 0.00077 0.00078 0.00064 0.00059 0.00060 0.00032 H3 0.49054 0.25752 0.49260 1.00000 0.04557 0.00000 0.00000 O4 0.39105 0.74816 0.45887 1.00000 0.03317 0.03232 0.04404 0.00170 0.00750 -0.00083 0.03683 0.00215 0.00006 0.00016 0.00006 0.00000 0.00071 0.00068 0.00081 0.00061 0.00060 0.00055 0.00031 O5 0.27420 0.67619 0.39004 1.00000 0.03860 0.04993 0.04331 0.01884 -0.00394 -0.00332 0.04632 0.00223 0.00007 0.00017 0.00006 0.00000 0.00077 0.00081 0.00083 0.00069 0.00064 0.00059 0.00035 O6 0.08078 -0.02127 0.69976 1.00000 0.05883 0.04340 0.06951 -0.00499 0.03859 -0.01373 0.05329 0.00249 0.00008 0.00018 0.00007 0.00000 0.00090 0.00081 0.00104 0.00075 0.00081 0.00067 0.00038 O7 0.61855 -0.14230 0.74201 1.00000 0.03714 0.02967 0.03317 0.00000 -0.00192 0.00649 0.03512 0.00199 0.00006 0.00015 0.00005 0.00000 0.00071 0.00066 0.00073 0.00058 0.00057 0.00052 0.00031 Final Structure Factor Calculation for marc003 in P2(1)/c Total number of l.s. parameters = 335 Maximum vector length = 623 Memory required = 5428 / 26789 wR2 = 0.0908 before cycle 11 for 5682 data and 0 / 335 parameters Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU RIGU SIMU ISOR SUMP Number 0 0 0 4 0 0 0 0 0 0 0 0 rms sigma 0.0000 0.0000 0.0000 0.0200 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 rms deviation 0.0000 0.0000 0.0000 0.0158 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 GooF = S = 0.823; Restrained GooF = 0.823 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0348 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0456 for 3068 Fo > 4sig(Fo) and 0.0928 for all 5682 data wR2 = 0.0908, GooF = S = 0.823, Restrained GooF = 0.823 for all data Occupancy sum of asymmetric unit = 35.00 for non-hydrogen and 30.00 for H and D atoms Principal mean square atomic displacements U 0.0332 0.0267 0.0193 C1 0.0353 0.0282 0.0179 C2 0.0327 0.0304 0.0252 C3 0.0325 0.0284 0.0246 C4 0.0324 0.0258 0.0255 C5 0.0386 0.0343 0.0246 C6 0.0427 0.0336 0.0269 C7 0.0423 0.0396 0.0265 C8 0.0682 0.0397 0.0240 C9 0.0564 0.0325 0.0248 C10 0.0321 0.0266 0.0207 C11 0.1407 0.0597 0.0268 C12_a 0.1407 0.0597 0.0268 C12'_b 0.0393 0.0289 0.0227 C13 0.0411 0.0293 0.0222 C14 0.0337 0.0273 0.0224 C15 0.0429 0.0293 0.0237 C16 0.0355 0.0298 0.0235 C17 0.0291 0.0256 0.0241 C18 0.0735 0.0401 0.0223 C19 0.0386 0.0295 0.0236 C20 0.0700 0.0529 0.0252 C21_a 0.1273 0.0799 0.0296 C22_a 0.0700 0.0529 0.0252 C21'_b 0.1273 0.0799 0.0296 C22'_b 0.0507 0.0471 0.0303 C23 0.0765 0.0621 0.0305 C24 0.0883 0.0565 0.0276 C25 0.0686 0.0592 0.0301 C26 0.0510 0.0463 0.0304 C27 0.0419 0.0292 0.0256 C28 0.0391 0.0291 0.0213 O1 0.0414 0.0291 0.0210 O2 0.0497 0.0382 0.0260 O3 0.0453 0.0335 0.0317 O4 0.0746 0.0394 0.0249 O5 0.0863 0.0457 0.0279 O6 0.0507 0.0309 0.0238 O7 0 atoms may be split and 0 atoms NPD Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.005 0.010 0.016 0.022 0.028 0.036 0.047 0.063 0.098 1.000 Number in group 594. 553. 620. 564. 524. 577. 565. 553. 566. 566. GooF 0.524 0.535 0.568 0.682 0.739 0.845 0.928 0.949 1.008 1.197 K 1.718 1.308 1.091 1.079 1.073 1.045 0.988 0.978 0.999 1.003 Resolution(A) 0.77 0.79 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.66 inf Number in group 570. 573. 576. 572. 561. 565. 568. 562. 568. 567. GooF 0.625 0.640 0.631 0.618 0.682 0.767 0.858 0.832 0.977 1.331 K 1.227 1.184 1.108 1.043 0.981 0.974 0.976 1.002 1.014 0.997 R1 0.249 0.236 0.211 0.168 0.154 0.096 0.070 0.047 0.043 0.029 Recommended weighting scheme: WGHT 0.0350 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). Error/esd is calculated as sqrt(wD^2/) where w is given by the weight formula, D = Fo^2-Fc^2 and <> refers to the average over all reflections. h k l Fo^2 Fc^2 Error/esd Fc/Fc(max) Resolution(A) 1 3 6 1473.45 1238.63 5.42 0.139 1.87 -5 4 1 46.89 83.45 5.04 0.036 1.55 1 4 0 382.63 295.57 4.82 0.068 1.73 9 3 2 168.61 210.08 4.73 0.057 1.40 -3 3 3 540.73 453.93 4.46 0.084 2.10 5 1 1 87.88 105.10 4.23 0.041 2.90 -5 1 3 443.96 516.59 4.22 0.090 3.02 -6 2 7 2454.34 2156.11 4.22 0.184 1.93 -13 2 12 39.53 87.43 4.09 0.037 1.11 5 3 7 2110.32 1859.69 4.00 0.171 1.50 -1 3 4 1554.02 1372.73 3.94 0.147 2.12 0 1 2 14950.62 17530.14 3.88 0.524 5.75 2 1 8 572.83 662.46 3.87 0.102 2.18 -4 2 5 48.49 72.83 3.85 0.034 2.42 2 3 5 5046.25 4519.07 3.82 0.266 1.91 3 0 10 45.01 87.94 3.80 0.037 1.79 -6 1 2 781.91 879.23 3.78 0.117 2.66 -4 3 3 4.54 21.96 3.66 0.019 2.01 8 3 13 12.20 57.64 3.61 0.030 1.02 -1 0 2 677.81 753.30 3.48 0.109 9.87 7 1 5 4565.83 4130.84 3.45 0.254 1.81 4 2 5 2543.47 2296.06 3.41 0.190 2.10 8 3 12 214.43 292.89 3.40 0.068 1.06 -16 1 6 221.25 353.58 3.38 0.074 1.06 -7 3 3 329.40 277.38 3.26 0.066 1.68 -8 5 2 4604.29 4176.06 3.26 0.256 1.17 2 3 6 101.56 72.96 3.25 0.034 1.81 4 2 4 12040.52 11002.55 3.23 0.415 2.23 -1 3 15 273.63 367.79 3.23 0.076 1.19 3 3 4 1041.02 932.40 3.22 0.121 1.91 12 3 8 135.21 197.10 3.18 0.056 1.01 5 1 7 3595.92 3272.13 3.18 0.226 1.90 6 3 5 94.37 68.53 3.18 0.033 1.55 4 3 5 5452.52 4976.96 3.17 0.279 1.74 7 0 2 3139.44 2800.13 3.17 0.209 2.22 -4 1 11 477.17 544.79 3.15 0.092 1.81 -5 1 10 393.81 451.80 3.14 0.084 1.90 -13 4 1 166.81 234.22 3.13 0.061 1.04 -7 0 8 19.55 41.05 3.11 0.025 2.01 -6 0 2 1135.16 1270.79 3.10 0.141 2.88 0 8 1 169.76 234.27 3.09 0.061 0.87 6 3 3 127.48 156.63 3.09 0.050 1.66 12 4 7 66.85 112.92 3.07 0.042 0.96 1 2 3 910.60 1004.49 3.06 0.125 2.98 -2 1 7 244.44 280.63 3.06 0.066 2.75 -14 7 2 117.01 83.04 3.05 0.036 0.77 3 2 6 382.87 343.39 3.05 0.073 2.10 -1 4 5 1110.24 996.17 3.02 0.125 1.60 9 1 3 16.81 30.55 3.02 0.022 1.65 3 4 8 36.64 67.47 3.02 0.033 1.35 Bond lengths and angles C1 - Distance Angles O1 1.4432 (0.0017) C11 1.5212 (0.0022) 108.76 (0.13) C2 1.5578 (0.0021) 106.78 (0.12) 118.03 (0.13) C5 1.5723 (0.0022) 102.51 (0.12) 115.12 (0.12) 104.27 (0.13) C1 - O1 C11 C2 C2 - Distance Angles O2 1.4318 (0.0017) C18 1.5220 (0.0021) 110.03 (0.12) C3 1.5411 (0.0022) 106.36 (0.13) 113.96 (0.13) C1 1.5578 (0.0021) 106.92 (0.12) 117.04 (0.14) 101.67 (0.12) C2 - O2 C18 C3 C3 - Distance Angles O3 1.4192 (0.0018) C4 1.5189 (0.0021) 108.83 (0.13) C2 1.5411 (0.0022) 112.23 (0.13) 102.33 (0.12) H3A 1.0000 111.04 111.04 111.04 C3 - O3 C4 C2 C4 - Distance Angles C20 1.4983 (0.0022) C3 1.5189 (0.0021) 114.89 (0.13) C5 1.5613 (0.0022) 110.95 (0.13) 105.59 (0.13) H4 1.0000 108.41 108.41 108.41 C4 - C20 C3 C5 C5 - Distance Angles C28 1.5135 (0.0021) C4 1.5613 (0.0022) 113.38 (0.13) C1 1.5723 (0.0022) 118.86 (0.13) 104.80 (0.12) H5 1.0000 106.33 106.33 106.33 C5 - C28 C4 C1 C6 - Distance Angles C11 1.3792 (0.0022) C7 1.3830 (0.0022) 122.82 (0.16) H6 0.9500 118.59 118.59 C6 - C11 C7 C7 - Distance Angles C8 1.3794 (0.0022) C6 1.3830 (0.0022) 119.50 (0.16) H7 0.9500 120.25 120.25 C7 - C8 C6 C8 - Distance Angles O6 1.3733 (0.0020) C7 1.3794 (0.0022) 124.61 (0.17) C9 1.3801 (0.0024) 116.61 (0.16) 118.78 (0.17) C8 - O6 C7 C9 - Distance Angles C10 1.3761 (0.0023) C8 1.3801 (0.0024) 121.02 (0.17) H9 0.9500 119.49 119.49 C9 - C10 C8 C10 - Distance Angles C9 1.3761 (0.0023) C11 1.3928 (0.0021) 121.26 (0.17) H10 0.9500 119.37 119.37 C10 - C9 C11 C11 - Distance Angles C6 1.3792 (0.0022) C10 1.3928 (0.0021) 116.59 (0.16) C1 1.5212 (0.0022) 118.15 (0.15) 125.24 (0.15) C11 - C6 C10 C12_a - Distance Angles O6 1.4288 (0.0046) H12A_a 0.9800 109.47 H12B_a 0.9800 109.47 109.47 H12C_a 0.9800 109.47 109.47 109.47 C12_a - O6 H12A_a H12B_a C12'_b - Distance Angles O6 1.4514 (0.0130) H12D_b 0.9800 109.47 H12E_b 0.9800 109.47 109.47 H12F_b 0.9800 109.47 109.47 109.47 C12'_b - O6 H12D_b H12E_b C13 - Distance Angles C14 1.3829 (0.0021) C18 1.3953 (0.0020) 121.62 (0.15) H13 0.9500 119.19 119.19 C13 - C14 C18 C14 - Distance Angles C13 1.3829 (0.0021) C15 1.3834 (0.0021) 119.91 (0.15) H14 0.9500 120.04 120.04 C14 - C13 C15 C15 - Distance Angles C16 1.3795 (0.0021) O7 1.3822 (0.0017) 123.92 (0.15) C14 1.3834 (0.0021) 119.71 (0.15) 116.37 (0.14) C15 - C16 O7 C16 - Distance Angles C15 1.3795 (0.0021) C17 1.3849 (0.0021) 119.56 (0.15) H16 0.9500 120.22 120.22 C16 - C15 C17 C17 - Distance Angles C16 1.3849 (0.0021) C18 1.3883 (0.0020) 122.16 (0.15) H17 0.9500 118.92 118.92 C17 - C16 C18 C18 - Distance Angles C17 1.3883 (0.0020) C13 1.3953 (0.0021) 116.91 (0.14) C2 1.5220 (0.0021) 120.41 (0.14) 122.57 (0.14) C18 - C17 C13 C19 - Distance Angles O7 1.4404 (0.0019) H19A 0.9800 109.47 H19B 0.9800 109.47 109.47 H19C 0.9800 109.47 109.47 109.47 C19 - O7 H19A H19B C20 - Distance Angles O4 1.2095 (0.0018) O5 1.3337 (0.0018) 123.41 (0.16) C4 1.4983 (0.0022) 126.05 (0.15) 110.46 (0.14) C20 - O4 O5 C21_a - Distance Angles O5 1.4607 (0.0071) C22_a 1.4889 (0.0093) 106.74 (0.64) H21A_a 0.9900 110.38 110.38 H21B_a 0.9900 110.38 110.38 108.60 C21_a - O5 C22_a H21A_a C22_a - Distance Angles C21_a 1.4889 (0.0093) H22A_a 0.9800 109.47 H22B_a 0.9800 109.47 109.47 H22C_a 0.9800 109.47 109.47 109.47 C22_a - C21_a H22A_a H22B_a C21'_b - Distance Angles O5 1.4473 (0.0127) C22'_b 1.5006 (0.0142) 105.97 (1.07) H21C_b 0.9900 110.54 110.54 H21D_b 0.9900 110.54 110.54 108.70 C21'_b - O5 C22'_b H21C_b C22'_b - Distance Angles C21'_b 1.5006 (0.0142) H22D_b 0.9800 109.47 H22E_b 0.9800 109.47 109.47 H22F_b 0.9800 109.47 109.47 109.47 C22'_b - C21'_b H22D_b H22E_b C23 - Distance Angles C28 1.3805 (0.0022) C24 1.3856 (0.0024) 121.24 (0.18) H23 0.9500 119.38 119.38 C23 - C28 C24 C24 - Distance Angles C25 1.3654 (0.0027) C23 1.3856 (0.0024) 119.88 (0.19) H24 0.9500 120.06 120.06 C24 - C25 C23 C25 - Distance Angles C24 1.3654 (0.0027) C26 1.3752 (0.0027) 120.15 (0.19) H25 0.9500 119.93 119.93 C25 - C24 C26 C26 - Distance Angles C25 1.3752 (0.0027) C27 1.3823 (0.0023) 119.95 (0.20) H26 0.9500 120.02 120.02 C26 - C25 C27 C27 - Distance Angles C26 1.3823 (0.0023) C28 1.3907 (0.0022) 120.84 (0.18) H27 0.9500 119.58 119.58 C27 - C26 C28 C28 - Distance Angles C23 1.3805 (0.0022) C27 1.3907 (0.0022) 117.94 (0.16) C5 1.5135 (0.0021) 120.00 (0.16) 122.04 (0.15) C28 - C23 C27 O1 - Distance Angles C1 1.4432 (0.0017) H1 0.8400 109.47 O1 - C1 O2 - Distance Angles C2 1.4318 (0.0017) H2 0.8400 109.47 O2 - C2 O3 - Distance Angles C3 1.4192 (0.0018) H3 0.8400 109.47 O3 - C3 O4 - Distance Angles C20 1.2095 (0.0018) O4 - O5 - Distance Angles C20 1.3337 (0.0019) C21'_b 1.4473 (0.0127) 119.08 (0.65) C21_a 1.4607 (0.0071) 116.91 (0.36) 4.62 (1.65) O5 - C20 C21'_b O6 - Distance Angles C8 1.3733 (0.0020) C12_a 1.4288 (0.0046) 117.68 (0.29) C12'_b 1.4514 (0.0130) 113.06 (0.80) 27.09 (0.74) O6 - C8 C12_a O7 - Distance Angles C15 1.3822 (0.0017) C19 1.4404 (0.0019) 116.39 (0.12) O7 - C15 Selected torsion angles 177.61 ( 0.12) O1 - C1 - C2 - O2 54.85 ( 0.17) C11 - C1 - C2 - O2 -74.32 ( 0.15) C5 - C1 - C2 - O2 53.74 ( 0.17) O1 - C1 - C2 - C18 -69.02 ( 0.18) C11 - C1 - C2 - C18 161.81 ( 0.13) C5 - C1 - C2 - C18 -71.08 ( 0.14) O1 - C1 - C2 - C3 166.16 ( 0.13) C11 - C1 - C2 - C3 36.99 ( 0.14) C5 - C1 - C2 - C3 -51.22 ( 0.16) O2 - C2 - C3 - O3 70.19 ( 0.17) C18 - C2 - C3 - O3 -162.96 ( 0.12) C1 - C2 - C3 - O3 65.27 ( 0.15) O2 - C2 - C3 - C4 -173.31 ( 0.13) C18 - C2 - C3 - C4 -46.46 ( 0.15) C1 - C2 - C3 - C4 -80.40 ( 0.17) O3 - C3 - C4 - C20 160.68 ( 0.13) C2 - C3 - C4 - C20 157.02 ( 0.13) O3 - C3 - C4 - C5 38.09 ( 0.16) C2 - C3 - C4 - C5 89.03 ( 0.16) C20 - C4 - C5 - C28 -145.90 ( 0.14) C3 - C4 - C5 - C28 -139.82 ( 0.13) C20 - C4 - C5 - C1 -14.74 ( 0.16) C3 - C4 - C5 - C1 -134.87 ( 0.14) O1 - C1 - C5 - C28 -16.96 ( 0.21) C11 - C1 - C5 - C28 113.94 ( 0.15) C2 - C1 - C5 - C28 97.23 ( 0.13) O1 - C1 - C5 - C4 -144.87 ( 0.13) C11 - C1 - C5 - C4 -13.97 ( 0.15) C2 - C1 - C5 - C4 0.26 ( 0.26) C11 - C6 - C7 - C8 178.65 ( 0.15) C6 - C7 - C8 - O6 -1.24 ( 0.26) C6 - C7 - C8 - C9 -178.95 ( 0.16) O6 - C8 - C9 - C10 0.95 ( 0.28) C7 - C8 - C9 - C10 0.35 ( 0.28) C8 - C9 - C10 - C11 0.99 ( 0.24) C7 - C6 - C11 - C10 -177.59 ( 0.14) C7 - C6 - C11 - C1 -1.28 ( 0.25) C9 - C10 - C11 - C6 177.18 ( 0.16) C9 - C10 - C11 - C1 43.69 ( 0.18) O1 - C1 - C11 - C6 165.45 ( 0.14) C2 - C1 - C11 - C6 -70.64 ( 0.19) C5 - C1 - C11 - C6 -134.75 ( 0.16) O1 - C1 - C11 - C10 -13.00 ( 0.23) C2 - C1 - C11 - C10 110.92 ( 0.18) C5 - C1 - C11 - C10 1.99 ( 0.27) C18 - C13 - C14 - C15 -4.24 ( 0.26) C13 - C14 - C15 - C16 175.00 ( 0.15) C13 - C14 - C15 - O7 -175.85 ( 0.15) O7 - C15 - C16 - C17 3.33 ( 0.26) C14 - C15 - C16 - C17 -0.14 ( 0.27) C15 - C16 - C17 - C18 -2.06 ( 0.26) C16 - C17 - C18 - C13 174.27 ( 0.15) C16 - C17 - C18 - C2 1.13 ( 0.26) C14 - C13 - C18 - C17 -175.11 ( 0.15) C14 - C13 - C18 - C2 -10.49 ( 0.21) O2 - C2 - C18 - C17 -129.84 ( 0.16) C3 - C2 - C18 - C17 111.78 ( 0.17) C1 - C2 - C18 - C17 165.62 ( 0.15) O2 - C2 - C18 - C13 46.27 ( 0.22) C3 - C2 - C18 - C13 -72.11 ( 0.20) C1 - C2 - C18 - C13 -21.50 ( 0.25) C3 - C4 - C20 - O4 98.16 ( 0.19) C5 - C4 - C20 - O4 161.86 ( 0.14) C3 - C4 - C20 - O5 -78.49 ( 0.17) C5 - C4 - C20 - O5 -0.07 ( 0.32) C28 - C23 - C24 - C25 0.43 ( 0.33) C23 - C24 - C25 - C26 -0.53 ( 0.33) C24 - C25 - C26 - C27 0.28 ( 0.31) C25 - C26 - C27 - C28 -0.18 ( 0.29) C24 - C23 - C28 - C27 178.42 ( 0.17) C24 - C23 - C28 - C5 0.08 ( 0.28) C26 - C27 - C28 - C23 -178.50 ( 0.17) C26 - C27 - C28 - C5 -112.69 ( 0.18) C4 - C5 - C28 - C23 123.53 ( 0.18) C1 - C5 - C28 - C23 65.86 ( 0.21) C4 - C5 - C28 - C27 -57.93 ( 0.23) C1 - C5 - C28 - C27 -2.21 ( 1.32) O4 - C20 - O5 - C21'_b 174.54 ( 1.31) C4 - C20 - O5 - C21'_b -6.82 ( 0.71) O4 - C20 - O5 - C21_a 169.93 ( 0.68) C4 - C20 - O5 - C21_a -161.41 ( 1.00) C22'_b - C21'_b - O5 - C20 156.97 ( 0.57) C22_a - C21_a - O5 - C20 -0.22 ( 0.78) C7 - C8 - O6 - C12_a 179.68 ( 0.76) C9 - C8 - O6 - C12_a -29.83 ( 1.24) C7 - C8 - O6 - C12'_b 150.06 ( 1.24) C9 - C8 - O6 - C12'_b 16.76 ( 0.23) C16 - C15 - O7 - C19 -162.44 ( 0.16) C14 - C15 - O7 - C19 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 2.06 2.8895(16) 170.5 O1-H1...O7_$2 0.84 2.17 2.8854(16) 143.5 O2-H2...O4_$3 0.84 2.06 2.8937(16) 176.1 O3-H3...O4_$4 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. Appropriate HTAB instructions appended to .res file for future use. D-H d(D-H) d(H..A)