TITL SHELXL INS file, from DIRDIF output for S92 CELL 0.71073 11.04250 15.40280 16.02740 90.0000 90.0000 90.0000 ZERR 4 0.0002 0.0003 0.0004 0.0000 0.0000 0.0000 LATT -1 SYMM 1/2+X , 1/2-Y , -Z SYMM -X , 1/2+Y , 1/2-Z SYMM 1/2-X , -Y , 1/2+Z SFAC C H N O F PD UNIT 96 96 8 16 24 8 ACTA TEMP -123 SIZE .2 .15 .1 HTAB BOND $H OMIT 0 51 OMIT 9 1 11 OMIT 5 0 6 OMIT -8 8 8 OMIT 0 5 4 OMIT 3 2 18 OMIT 2 0 6 OMIT 4 0 0 OMIT 3 12 8 DFIX 1.33 .008 C2' f1' C2' f2' C2' f3' C2' f1" C2' f2" C2' f3" CONF O2 Pd1 Pd2 O1 CONF O2' Pd2 Pd1 O1' ISOR .008 F1' F2' ISOR .004 F3' L.S. 1 BOND FMAP 2 MPLA 4 O1' o2 C10 N1' Pd1 MPLA 4 O1 o2' C20 N1 Pd2 PLAN 10 WGHT 0.035200 EXTI 0.000932 FVAR 0.19412 PART 0 PD1 6 0.190898 0.052598 0.204123 11.00000 0.02613 0.02853 = 0.02357 0.00263 -0.00091 0.00223 PD2 6 0.071467 0.153013 0.075097 11.00000 0.02714 0.02493 = 0.02197 0.00409 0.00164 0.00050 N1' 3 0.324821 0.138180 0.228614 11.00000 0.03075 0.03076 = 0.02942 0.00053 -0.00234 0.00233 N1 3 0.193272 0.153982 -0.017411 11.00000 0.03071 0.02572 = 0.02256 0.00385 0.00032 0.00153 O1 4 -0.059795 0.166337 0.165631 11.00000 0.03071 0.03443 = 0.02852 0.00608 0.00230 0.00423 O2 4 0.045726 0.115680 0.276216 11.00000 0.03171 0.03524 = 0.03023 0.00619 0.00104 0.00514 O1' 4 0.066433 -0.042105 0.172929 11.00000 0.03457 0.02899 = 0.03217 0.00529 -0.00400 0.00146 O2' 4 0.004939 0.021612 0.052967 11.00000 0.03352 0.03084 = 0.03101 0.00202 -0.00495 -0.00150 F1 5 -0.247320 0.120360 0.275018 11.00000 0.03271 0.07429 = 0.07665 -0.00660 0.01773 -0.00851 F2 5 -0.188089 0.251895 0.285041 11.00000 0.07246 0.03866 = 0.06209 0.01003 0.02581 0.02255 F3 5 -0.135161 0.159069 0.375680 11.00000 0.06212 0.08406 = 0.02988 0.01304 0.01896 0.01980 PART 1 F1' 5 -0.069962 -0.137410 0.006907 10.63000 0.11750 0.07625 = 0.04844 -0.02202 0.02513 -0.05433 F2' 5 -0.187723 -0.093663 0.105194 10.63000 0.02404 0.05144 = 0.15456 0.00215 -0.00855 -0.01418 F3' 5 -0.053746 -0.183520 0.132506 10.63000 0.06952 0.02896 = 0.06612 0.02451 -0.02897 -0.02218 PART 2 F1" 5 -0.001273 -0.182923 0.070553 10.37000 0.10474 F2" 5 -0.149370 -0.133593 0.145995 10.37000 0.13205 F3" 5 -0.131378 -0.114524 0.016701 10.37000 0.06199 PART 0 C1 1 -0.043785 0.147326 0.241129 11.00000 0.03152 0.01969 = 0.02607 0.00547 0.00005 -0.00412 C2 1 -0.154155 0.170069 0.295563 11.00000 0.03522 0.03531 = 0.03144 0.00786 0.00891 0.00270 C1' 1 0.007821 -0.037114 0.105718 11.00000 0.03212 0.02473 = 0.03034 0.00609 0.00447 0.00125 C2' 1 -0.072840 -0.114517 0.086750 11.00000 0.04497 0.04039 = 0.03548 0.00073 -0.00085 -0.00842 C10 1 0.321116 -0.002364 0.139537 11.00000 0.03636 0.03496 = 0.02531 0.00454 -0.00468 0.00752 C11 1 0.429122 0.047040 0.138161 11.00000 0.03068 0.04198 = 0.03515 0.00032 0.00405 0.00351 C12 1 0.529016 0.020103 0.092354 11.00000 0.03792 0.06528 = 0.04446 -0.00719 0.00634 0.00239 AFIX 43 H12 2 0.600690 0.054211 0.091787 11.00000 0.06471 AFIX 0 C13 1 0.523839 -0.056317 0.047690 11.00000 0.04482 0.06126 = 0.03573 -0.00603 0.01217 0.01687 AFIX 43 H13 2 0.592018 -0.075167 0.016407 11.00000 0.05003 AFIX 0 C14 1 0.419006 -0.105403 0.048619 11.00000 0.05878 0.04097 = 0.03488 -0.00422 -0.00623 0.02025 AFIX 43 H14 2 0.415233 -0.157760 0.017398 11.00000 0.03072 AFIX 0 C15 1 0.318003 -0.078585 0.095298 11.00000 0.03647 0.03799 = 0.04569 -0.00125 -0.00536 0.00538 AFIX 43 H15 2 0.247071 -0.113473 0.096232 11.00000 0.09056 AFIX 0 C16 1 0.423484 0.124613 0.189137 11.00000 0.03231 0.03732 = 0.03222 0.00101 0.00172 -0.00382 AFIX 43 H16 2 0.489996 0.163524 0.193011 11.00000 0.02497 AFIX 0 C17 1 0.309303 0.212383 0.286379 11.00000 0.03356 0.03548 = 0.03834 -0.00549 0.00030 0.00135 AFIX 13 H17 2 0.226196 0.236116 0.276678 11.00000 0.02633 AFIX 0 C18 1 0.312315 0.179055 0.374580 11.00000 0.05734 0.04586 = 0.04093 -0.00878 0.00117 0.00413 AFIX 33 H18A 2 0.253293 0.131983 0.380799 11.00000 0.04954 H18B 2 0.292040 0.226295 0.413084 11.00000 0.05661 H18C 2 0.393574 0.157175 0.387317 11.00000 0.05293 AFIX 0 C19 1 0.399035 0.287077 0.270210 11.00000 0.04344 0.03952 = 0.07228 -0.00684 0.00181 -0.00324 AFIX 33 H19A 2 0.391005 0.306871 0.212363 11.00000 0.04278 H19B 2 0.481882 0.266569 0.279813 11.00000 0.03209 H19C 2 0.381308 0.335313 0.308166 11.00000 0.04247 AFIX 0 C20 1 0.132153 0.271577 0.089906 11.00000 0.02915 0.02436 = 0.02842 0.00673 -0.00149 0.00215 C21 1 0.224110 0.293897 0.032086 11.00000 0.03079 0.02721 = 0.03261 0.00491 0.00585 0.00359 C22 1 0.278044 0.374348 0.033537 11.00000 0.03686 0.03236 = 0.04819 0.00744 0.00514 -0.00260 AFIX 43 H22 2 0.337988 0.388597 -0.006714 11.00000 0.03285 AFIX 0 C23 1 0.245279 0.434594 0.093430 11.00000 0.04324 0.02824 = 0.04750 0.00065 0.00395 -0.00175 AFIX 43 H23 2 0.282144 0.490316 0.094228 11.00000 0.07678 AFIX 0 C24 1 0.157953 0.413035 0.152509 11.00000 0.03444 0.03102 = 0.04618 -0.00685 0.00209 0.00587 AFIX 43 H24 2 0.136086 0.453710 0.194442 11.00000 0.01717 AFIX 0 C25 1 0.101789 0.330587 0.150109 11.00000 0.02795 0.03688 = 0.03470 0.00155 0.00270 0.00069 AFIX 43 H25 2 0.042433 0.316059 0.190680 11.00000 0.01965 AFIX 0 C26 1 0.253935 0.224503 -0.024986 11.00000 0.03351 0.03378 = 0.03241 0.00258 0.00720 0.00755 AFIX 43 H26 2 0.315371 0.230816 -0.066033 11.00000 0.02992 AFIX 0 C27 1 0.210204 0.077438 -0.072186 11.00000 0.03479 0.03171 = 0.02608 -0.00408 0.00557 0.00592 AFIX 13 H27 2 0.200480 0.024154 -0.037174 11.00000 0.02637 AFIX 0 C28 1 0.334352 0.074047 -0.112303 11.00000 0.04030 0.03850 = 0.03643 -0.01120 0.00300 0.00299 AFIX 33 H28A 2 0.396677 0.074003 -0.068773 11.00000 0.04493 H28B 2 0.345249 0.124887 -0.148292 11.00000 0.08992 H28C 2 0.341431 0.021057 -0.145794 11.00000 0.04962 AFIX 0 C29 1 0.109073 0.077601 -0.137564 11.00000 0.03918 0.05068 = 0.03074 -0.00996 -0.00065 0.00900 AFIX 33 H29A 2 0.030293 0.079928 -0.109499 11.00000 0.01642 H29B 2 0.114123 0.024578 -0.171181 11.00000 0.12528 H29C 2 0.118085 0.128401 -0.173852 11.00000 0.05190 AFIX 0 HKLF 4 REM SHELXL INS file, from DIRDIF output for S92 REM R1 = 0.0296 for 4674 Fo > 4sig(Fo) and 0.0343 for all 5039 data REM 380 parameters refined using 24 restraints END WGHT 0.0374 0.0000 REM Highest difference peak 0.673, deepest hole -0.526, 1-sigma level 0.079 Q1 1 0.0042 -0.1669 0.0282 11.00000 0.05 0.67 Q2 1 -0.1773 -0.0963 0.0463 11.00000 0.05 0.64 Q3 1 -0.0953 -0.1584 0.1547 11.00000 0.05 0.60 Q4 1 -0.0254 -0.1964 0.0994 11.00000 0.05 0.44 Q5 1 -0.1840 -0.1122 0.1301 11.00000 0.05 0.38 Q6 1 0.3206 -0.0537 0.1565 11.00000 0.05 0.32 Q7 1 -0.0866 0.0625 0.1237 11.00000 0.05 0.32 Q8 1 0.3162 0.1758 0.2416 11.00000 0.05 0.31 Q9 1 -0.1745 -0.0615 0.1315 11.00000 0.05 0.30 Q10 1 0.0747 0.2855 -0.0661 11.00000 0.05 0.29