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 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 0.582930 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 0.770563 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 -0.009587 0.782581 -21.00000 -1.50000 H12F 2 0.037070 0.192032 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 0.916162 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 0.765112 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 0.861201 0.327020 -31.00000 -1.20000 H21D 2 0.287128 0.965492 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 0.02855 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 REM marc003 in P2(1)/c REM R1 = 0.0456 for 3068 Fo > 4sig(Fo) and 0.0928 for all 5682 data REM 335 parameters refined using 4 restraints END WGHT 0.0350 0.0000 REM Instructions for potential hydrogen bonds HTAB C21' O2_$1 HTAB O1 O7_$2 HTAB O2 O4_$3 HTAB O3 O4_$4 REM Highest difference peak 0.183, deepest hole -0.189, 1-sigma level 0.040 Q1 1 0.4023 0.1672 0.5822 11.00000 0.05 0.18 Q2 1 0.2734 0.2782 0.5925 11.00000 0.05 0.17 Q3 1 0.4442 0.0294 0.6013 11.00000 0.05 0.17 Q4 1 0.2023 -0.2066 0.6784 11.00000 0.05 0.17 Q5 1 0.3005 0.4642 0.4952 11.00000 0.05 0.16 Q6 1 0.3237 0.5547 0.4670 11.00000 0.05 0.16 Q7 1 0.3361 0.2729 0.5716 11.00000 0.05 0.16 Q8 1 0.0953 0.1821 0.7827 11.00000 0.05 0.16 Q9 1 0.2276 0.4664 0.4950 11.00000 0.05 0.15 Q10 1 0.2482 0.1466 0.6134 11.00000 0.05 0.15 Q11 1 0.1106 0.0444 0.6811 11.00000 0.05 0.15 Q12 1 0.2067 0.9425 0.3563 11.00000 0.05 0.15 Q13 1 0.5348 -0.0958 0.6647 11.00000 0.05 0.15 Q14 1 0.5075 -0.2965 0.6433 11.00000 0.05 0.14 Q15 1 0.4561 0.1690 0.6304 11.00000 0.05 0.14 Q16 1 0.2434 0.0251 0.5979 11.00000 0.05 0.14 Q17 1 0.2638 0.7861 0.3208 11.00000 0.05 0.14 Q18 1 0.3586 0.4330 0.4985 11.00000 0.05 0.14 Q19 1 0.2366 0.2750 0.6441 11.00000 0.05 0.14 Q20 1 0.5718 0.0332 0.6854 11.00000 0.05 0.14