TITL SHELXL INS file, from DIRDIF output for S92 CELL 0.71073 12.6771 16.0582 16.0851 110.325 93.158 96.365 ZERR 2.00 0.0025 0.0032 0.0032 0.030 0.030 0.030 LATT 1 SFAC C H SI P RU UNIT 132 132 4 8 2 MERG 2 FMAP 2 PLAN 10 OMIT -3 55 OMIT 2 2 2 OMIT 2 5 3 OMIT -4 4 0 ISOR 0.001 C58 C57 C59 SIZE 0.2 0.075 0.05 TEMP -123 ACTA BOND L.S. 4 WGHT 0.056500 EXTI 0.000000 FVAR 0.18491 C1 1 0.453452 0.311399 0.454249 11.00000 0.02720 0.01889 = 0.02468 0.00774 -0.00103 0.00184 C2 1 0.402699 0.283882 0.515959 11.00000 0.02849 0.04327 = 0.03898 0.02404 -0.00184 -0.00188 AFIX 43 H2 2 0.327019 0.276705 0.512894 11.00000 -1.20000 AFIX 0 C3 1 0.460477 0.266645 0.582097 11.00000 0.04471 0.06345 = 0.05197 0.04202 -0.00541 -0.00404 AFIX 43 H3 2 0.424421 0.248102 0.624287 11.00000 -1.20000 AFIX 0 C4 1 0.570743 0.276315 0.587059 11.00000 0.04445 0.05035 = 0.04664 0.02981 -0.01298 -0.00046 AFIX 43 H4 2 0.610431 0.264951 0.632876 11.00000 -1.20000 AFIX 0 C5 1 0.622731 0.302476 0.525332 11.00000 0.02696 0.03860 = 0.04922 0.01699 -0.00901 0.00287 AFIX 43 H5 2 0.698377 0.308551 0.528227 11.00000 -1.20000 AFIX 0 C6 1 0.564742 0.320025 0.458754 11.00000 0.02954 0.02915 = 0.03235 0.01179 -0.00017 -0.00013 AFIX 43 H6 2 0.600898 0.337923 0.416228 11.00000 -1.20000 AFIX 0 C7 1 0.474237 0.380351 0.313088 11.00000 0.01807 0.02901 = 0.02484 0.01385 -0.00104 0.00120 C8 1 0.509126 0.471966 0.335590 11.00000 0.02738 0.03032 = 0.02939 0.01166 0.00058 0.00024 AFIX 43 H8 2 0.479766 0.514579 0.382363 11.00000 -1.20000 AFIX 0 C9 1 0.586255 0.500971 0.290086 11.00000 0.03480 0.02942 = 0.04696 0.02084 0.00385 -0.00502 AFIX 43 H9 2 0.608860 0.563321 0.305406 11.00000 -1.20000 AFIX 0 C10 1 0.630399 0.439550 0.222523 11.00000 0.03396 0.05062 = 0.05084 0.02753 0.01492 -0.00581 AFIX 43 H10 2 0.683310 0.459678 0.191584 11.00000 -1.20000 AFIX 0 C11 1 0.597616 0.349332 0.200189 11.00000 0.03197 0.04606 = 0.03700 0.01375 0.01463 0.00540 AFIX 43 H11 2 0.628011 0.307210 0.153748 11.00000 -1.20000 AFIX 0 C12 1 0.520309 0.319393 0.245125 11.00000 0.02484 0.02926 = 0.03416 0.01046 0.00641 0.00228 AFIX 43 H12 2 0.498599 0.256875 0.229466 11.00000 -1.20000 AFIX 0 C13 1 0.318409 0.437060 0.438920 11.00000 0.02808 0.02128 = 0.01896 0.00407 0.00351 0.00158 AFIX 23 H13A 2 0.278340 0.423126 0.484673 11.00000 -1.20000 H13B 2 0.377628 0.485710 0.469827 11.00000 -1.20000 AFIX 0 C14 1 0.244823 0.467910 0.380964 11.00000 0.02770 0.01769 = 0.02669 0.00646 0.00459 0.00267 AFIX 23 H14A 2 0.288329 0.501059 0.350212 11.00000 -1.20000 H14B 2 0.200323 0.509501 0.419284 11.00000 -1.20000 AFIX 0 C15 1 0.155557 0.407672 0.199969 11.00000 0.03424 0.01720 = 0.02048 0.00777 0.00548 0.00540 C16 1 0.252661 0.428514 0.169777 11.00000 0.03310 0.02891 = 0.03001 0.01542 0.00883 0.00708 AFIX 43 H16 2 0.317409 0.424540 0.199943 11.00000 -1.20000 AFIX 0 C17 1 0.255957 0.454849 0.096622 11.00000 0.05357 0.03748 = 0.03683 0.01969 0.01887 0.00593 AFIX 43 H17 2 0.322645 0.470367 0.077792 11.00000 -1.20000 AFIX 0 C18 1 0.161559 0.458567 0.050724 11.00000 0.07119 0.03613 = 0.02567 0.01628 0.00579 0.00738 AFIX 43 H18 2 0.163594 0.476283 0.000229 11.00000 -1.20000 AFIX 0 C19 1 0.065931 0.436747 0.078247 11.00000 0.05438 0.03761 = 0.03131 0.01422 -0.00638 0.00653 AFIX 43 H19 2 0.001630 0.439659 0.046767 11.00000 -1.20000 AFIX 0 C20 1 0.061341 0.410271 0.151859 11.00000 0.03547 0.02430 = 0.02914 0.00934 0.00004 0.00362 AFIX 43 H20 2 -0.005827 0.393948 0.169459 11.00000 -1.20000 AFIX 0 C21 1 0.024055 0.390384 0.332888 11.00000 0.02365 0.02268 = 0.02080 0.00805 0.00453 0.00712 C22 1 -0.007891 0.475265 0.356794 11.00000 0.02811 0.02637 = 0.04024 0.01137 0.00987 0.00360 AFIX 43 H22 2 0.040731 0.524525 0.356302 11.00000 -1.20000 AFIX 0 C23 1 -0.108730 0.488694 0.381064 11.00000 0.03108 0.02339 = 0.05711 0.00747 0.01688 0.01010 AFIX 43 H23 2 -0.129021 0.547026 0.397402 11.00000 -1.20000 AFIX 0 C24 1 -0.181312 0.417203 0.381822 11.00000 0.02560 0.03177 = 0.04243 0.00736 0.01322 0.00735 AFIX 43 H24 2 -0.251191 0.426394 0.398063 11.00000 -1.20000 AFIX 0 C25 1 -0.150742 0.333132 0.358801 11.00000 0.02630 0.02616 = 0.03920 0.00611 0.00977 -0.00093 AFIX 43 H25 2 -0.199558 0.284166 0.359704 11.00000 -1.20000 AFIX 0 C26 1 -0.049169 0.319530 0.334319 11.00000 0.02695 0.02225 = 0.02622 0.00681 0.00753 0.00443 AFIX 43 H26 2 -0.029150 0.261125 0.318288 11.00000 -1.20000 AFIX 0 C27 1 0.008808 0.169854 0.103577 11.00000 0.02687 0.01779 = 0.01897 0.00378 0.00084 0.00185 C28 1 0.056729 0.177793 0.030642 11.00000 0.02756 0.02468 = 0.02305 0.00694 0.00276 0.00212 AFIX 43 H28 2 0.128322 0.166559 0.023610 11.00000 -1.20000 AFIX 0 C29 1 0.000945 0.201974 -0.031974 11.00000 0.04298 0.03232 = 0.02298 0.01233 0.00569 0.00497 AFIX 43 H29 2 0.034189 0.206312 -0.082100 11.00000 -1.20000 AFIX 0 C30 1 -0.102790 0.219840 -0.022015 11.00000 0.04136 0.04025 = 0.02791 0.01550 -0.00266 0.00906 AFIX 43 H30 2 -0.140983 0.236344 -0.065037 11.00000 -1.20000 AFIX 0 C31 1 -0.150151 0.213430 0.051051 11.00000 0.03282 0.04133 = 0.03459 0.01189 0.00067 0.01353 AFIX 43 H31 2 -0.221220 0.226031 0.058506 11.00000 -1.20000 AFIX 0 C32 1 -0.095041 0.188748 0.113844 11.00000 0.02746 0.03184 = 0.02624 0.00880 0.00390 0.00566 AFIX 43 H32 2 -0.128460 0.184761 0.164019 11.00000 -1.20000 AFIX 0 C33 1 -0.024074 0.073351 0.221688 11.00000 0.02202 0.02086 = 0.02744 0.01042 0.00734 0.00410 C34 1 -0.097923 0.006777 0.158845 11.00000 0.02671 0.02635 = 0.03006 0.00901 0.00405 0.00147 AFIX 43 H34 2 -0.095656 -0.003119 0.097249 11.00000 -1.20000 AFIX 0 C35 1 -0.173909 -0.044572 0.185437 11.00000 0.02719 0.03111 = 0.04606 0.01117 0.00512 -0.00464 AFIX 43 H35 2 -0.223440 -0.089628 0.142239 11.00000 -1.20000 AFIX 0 C36 1 -0.177873 -0.030495 0.274376 11.00000 0.03171 0.03713 = 0.05524 0.02378 0.01381 -0.00414 AFIX 43 H36 2 -0.229857 -0.066326 0.292413 11.00000 -1.20000 AFIX 0 C37 1 -0.107313 0.034938 0.337401 11.00000 0.04405 0.04580 = 0.03710 0.02098 0.01359 -0.00181 AFIX 43 H37 2 -0.111544 0.045217 0.398882 11.00000 -1.20000 AFIX 0 C38 1 -0.029643 0.086144 0.311110 11.00000 0.03359 0.02507 = 0.02963 0.01036 0.00468 -0.00250 AFIX 43 H38 2 0.020162 0.130377 0.354841 11.00000 -1.20000 AFIX 0 C39 1 0.146960 0.041712 0.117140 11.00000 0.02222 0.02208 = 0.01959 0.00389 0.00475 0.00170 AFIX 23 H39A 2 0.092340 -0.007074 0.077856 11.00000 -1.20000 H39B 2 0.195761 0.061374 0.079486 11.00000 -1.20000 AFIX 0 C40 1 0.209110 0.009054 0.181141 11.00000 0.02604 0.01913 = 0.02964 0.00869 0.00523 0.00299 AFIX 23 H40A 2 0.255343 -0.033942 0.147320 11.00000 -1.20000 H40B 2 0.158271 -0.022979 0.208092 11.00000 -1.20000 AFIX 0 C41 1 0.299305 0.054145 0.358982 11.00000 0.03067 0.02189 = 0.03216 0.01186 0.00052 0.00193 C42 1 0.240424 0.081829 0.430875 11.00000 0.04799 0.03549 = 0.03792 0.02101 0.01086 0.01253 AFIX 43 H42 2 0.196042 0.126789 0.435123 11.00000 -1.20000 AFIX 0 C43 1 0.245038 0.045143 0.496787 11.00000 0.07900 0.04630 = 0.04185 0.02774 0.01810 0.01461 AFIX 43 H43 2 0.203496 0.065008 0.545516 11.00000 -1.20000 AFIX 0 C44 1 0.308442 -0.019243 0.492884 11.00000 0.07255 0.05985 = 0.05798 0.04607 0.00597 0.01263 AFIX 43 H44 2 0.312831 -0.042711 0.539458 11.00000 -1.20000 AFIX 0 C45 1 0.365349 -0.049494 0.421522 11.00000 0.06988 0.05949 = 0.08169 0.05270 0.01697 0.03144 AFIX 43 H45 2 0.407743 -0.095703 0.417493 11.00000 -1.20000 AFIX 0 C46 1 0.362011 -0.013470 0.354626 11.00000 0.05691 0.04633 = 0.05703 0.03314 0.02177 0.02525 AFIX 43 H46 2 0.402594 -0.034864 0.305501 11.00000 -1.20000 AFIX 0 C47 1 0.426733 0.095660 0.235515 11.00000 0.02294 0.02008 = 0.04492 0.01082 0.00856 0.00786 C48 1 0.516423 0.117377 0.298566 11.00000 0.02792 0.02656 = 0.05876 0.01217 -0.00054 0.00611 AFIX 43 H48 2 0.506953 0.132498 0.359993 11.00000 -1.20000 AFIX 0 C49 1 0.618252 0.116859 0.271717 11.00000 0.02589 0.03433 = 0.09516 0.01833 -0.00051 0.00461 AFIX 43 H49 2 0.678215 0.130637 0.314655 11.00000 -1.20000 AFIX 0 C50 1 0.632976 0.096567 0.183509 11.00000 0.02853 0.04765 = 0.11463 0.02363 0.03142 0.01208 AFIX 43 H50 2 0.703225 0.097016 0.165775 11.00000 -1.20000 AFIX 0 C51 1 0.546763 0.075485 0.120173 11.00000 0.04411 0.04337 = 0.07356 0.01624 0.03378 0.01122 AFIX 43 H51 2 0.557577 0.061746 0.059134 11.00000 -1.20000 AFIX 0 C52 1 0.444235 0.074448 0.146055 11.00000 0.02971 0.03014 = 0.04721 0.00873 0.01678 0.00490 AFIX 43 H52 2 0.384972 0.059056 0.102196 11.00000 -1.20000 AFIX 0 C53 1 0.285512 0.230784 0.168987 11.00000 0.02000 0.01548 = 0.03385 0.00725 -0.00071 0.00226 C54 1 0.322185 0.230621 0.103129 11.00000 0.02143 0.02329 = 0.03281 0.00787 0.00409 0.00302 C55 1 0.370946 0.236890 0.029431 11.00000 0.03557 0.03788 = 0.02893 0.01379 0.01190 0.00626 C56 1 0.415653 0.244987 -0.032944 11.00000 0.04110 0.05241 = 0.03738 0.01936 0.01019 0.00532 C57 1 0.456406 0.172752 -0.223763 11.00000 0.14802 0.08954 = 0.08127 0.03914 0.06228 0.01567 AFIX 137 H57A 2 0.465370 0.116621 -0.214590 11.00000 -1.50000 H57B 2 0.503527 0.180688 -0.267526 11.00000 -1.50000 H57C 2 0.382126 0.170553 -0.245761 11.00000 -1.50000 AFIX 0 C58 1 0.453647 0.369428 -0.133530 11.00000 0.12131 0.09339 = 0.09589 0.04282 0.01526 0.01276 AFIX 137 H58A 2 0.379302 0.357985 -0.159393 11.00000 -1.50000 H58B 2 0.500266 0.385582 -0.173774 11.00000 -1.50000 H58C 2 0.461834 0.418818 -0.075857 11.00000 -1.50000 AFIX 0 C59 1 0.631978 0.287265 -0.079237 11.00000 0.03457 0.60599 = 0.24329 0.33522 0.02586 0.03367 AFIX 137 H59A 2 0.643714 0.330214 -0.017865 11.00000 -1.50000 H59B 2 0.672400 0.311665 -0.117808 11.00000 -1.50000 H59C 2 0.655986 0.230674 -0.081375 11.00000 -1.50000 AFIX 0 C60 1 0.157775 0.258137 0.406327 11.00000 0.01630 0.01796 = 0.04374 0.01801 -0.00609 -0.00229 C61 1 0.121576 0.271759 0.469396 11.00000 0.02561 0.01173 = 0.02683 -0.00033 -0.00860 0.00411 C62 1 0.069509 0.274054 0.547640 11.00000 0.03515 0.02750 = 0.02517 0.00899 0.00742 0.00299 C63 1 0.026809 0.275283 0.614164 11.00000 0.04717 0.03603 = 0.03036 0.01125 0.01388 0.00735 C64 1 0.067163 0.344092 0.810984 11.00000 0.08071 0.07173 = 0.03897 0.01766 -0.00523 -0.00650 AFIX 137 H64A 2 0.130598 0.313894 0.808649 11.00000 -1.50000 H64B 2 0.035932 0.350477 0.866901 11.00000 -1.50000 H64C 2 0.087334 0.403549 0.807837 11.00000 -1.50000 AFIX 0 C65 1 -0.156452 0.329068 0.724008 11.00000 0.05287 0.07265 = 0.06350 0.03361 0.01905 0.01981 AFIX 137 H65A 2 -0.139619 0.391400 0.727751 11.00000 -1.50000 H65B 2 -0.188853 0.327640 0.777509 11.00000 -1.50000 H65C 2 -0.206526 0.295767 0.671190 11.00000 -1.50000 AFIX 0 C66 1 -0.064085 0.160973 0.712654 11.00000 0.07999 0.04269 = 0.04682 0.02212 0.01382 -0.00094 AFIX 137 H66A 2 -0.116344 0.127027 0.661550 11.00000 -1.50000 H66B 2 -0.094000 0.161822 0.767792 11.00000 -1.50000 H66C 2 0.000952 0.132481 0.707050 11.00000 -1.50000 AFIX 0 SI1 3 0.490536 0.267287 -0.117608 11.00000 0.04030 0.08964 = 0.04640 0.04607 0.01772 0.00989 SI2 3 -0.031886 0.276686 0.715605 11.00000 0.04042 0.03495 = 0.02397 0.01273 0.01020 0.00331 P1 4 0.372589 0.337033 0.370211 11.00000 0.02034 0.01939 = 0.01999 0.00698 0.00243 0.00177 P2 4 0.156283 0.371837 0.296265 11.00000 0.02037 0.01833 = 0.01958 0.00737 0.00466 0.00315 P3 4 0.082699 0.136856 0.186276 11.00000 0.02019 0.01832 = 0.01893 0.00661 0.00457 0.00196 P4 4 0.292855 0.102671 0.271159 11.00000 0.02069 0.01932 = 0.02456 0.00907 0.00477 0.00390 RU1 5 0.223201 0.237609 0.285147 11.00000 0.01841 0.01725 = 0.01700 0.00663 0.00486 0.00247 HKLF 4 REM SHELXL INS file, from DIRDIF output for S92 REM R1 = 0.0460 for 9761 Fo > 4sig(Fo) and 0.0753 for all 13576 data REM 665 parameters refined using 18 restraints END WGHT 0.0519 0.3370 REM Highest difference peak 0.764, deepest hole -0.806, 1-sigma level 0.088 Q1 1 0.3332 0.2892 0.1515 11.00000 0.05 0.76 Q2 1 0.5309 0.1785 -0.1891 11.00000 0.05 0.72 Q3 1 0.1530 0.2917 0.4513 11.00000 0.05 0.66 Q4 1 0.5419 0.3013 -0.0796 11.00000 0.05 0.56 Q5 1 0.5099 0.3641 -0.1233 11.00000 0.05 0.51 Q6 1 0.6049 0.3459 -0.0498 11.00000 0.05 0.51 Q7 1 0.2541 0.3330 0.3266 11.00000 0.05 0.45 Q8 1 0.2174 0.2424 0.1998 11.00000 0.05 0.44 Q9 1 0.2411 0.1987 0.1965 11.00000 0.05 0.44 Q10 1 0.3193 0.3013 0.3144 11.00000 0.05 0.43