TITL s93 in P2(1)/c CELL 0.71073 23.0236 12.4019 15.5740 90.000 109.102 90.000 ZERR 4.00 0.0022 0.0006 0.0010 0.000 0.007 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H P CL FE PD O UNIT 152 304 8 8 4 4 24 MERG 2 OMIT -3.00 55.00 OMIT -1 1 2 OMIT 4 0 0 SHEL 7 0.77 DFIX 0.84 0.02 O51 H51A O51 H51B O52 H52A O52 H52B O53 H53A O53 H53B DFIX 0.84 0.02 O54 H54A O54 H54B O55 H55A O55 H55B DFIX 0.84 0.005 O56 H56A O56 H56B DANG 1.35 0.02 H51A H51B H52A H52B H53A H53B H54A H54B H55A H55B DANG 1.35 0.005 H56A H56B EQIV $1 -X+1, Y+1/2, -Z-1/2 EQIV $2 X, -Y-1/2, Z+1/2 EQIV $3 -X+1, Y-1/2, -Z-1/2 EQIV $4 X, -Y+1/2, Z+1/2 EQIV $5 X, Y+1, Z EQIV $6 -X+2, -Y+1, -Z HTAB O51 CL11_$1 HTAB O51 O54_$1 HTAB O52 CL11_$2 HTAB O52 O51_$4 HTAB O53 CL11 HTAB O53 O52 HTAB O54 O55_$3 HTAB O54 CL11_$1 HTAB O55 O54_$4 HTAB O55 O53_$5 HTAB O56 CL1 HTAB O56 CL1_$6 FMAP 2 PLAN 5 SIZE 0.02 0.18 0.24 BOND $H L.S. 10 TEMP -153.00 WGHT 0.032300 6.387600 FVAR 0.23199 MOLE 1 C1 1 0.864674 0.023522 0.084048 11.00000 0.01063 0.01175 = 0.01354 -0.00043 0.00380 -0.00078 C2 1 0.845080 0.011586 -0.014468 11.00000 0.01066 0.01472 = 0.01373 -0.00120 0.00378 -0.00064 C3 1 0.842839 -0.100501 -0.034557 11.00000 0.01307 0.01520 = 0.01858 -0.00558 0.00399 -0.00022 C4 1 0.858451 -0.159029 0.047987 11.00000 0.01434 0.01133 = 0.02414 -0.00212 0.00136 0.00189 C5 1 0.871467 -0.084043 0.121970 11.00000 0.01137 0.00979 = 0.01770 0.00026 0.00068 -0.00044 C6 1 0.696867 0.009750 0.001276 11.00000 0.01155 0.01181 = 0.01339 0.00176 0.00440 -0.00068 C7 1 0.695792 -0.081618 -0.057490 11.00000 0.01003 0.01348 = 0.01614 -0.00037 0.00072 -0.00141 C8 1 0.710918 -0.175485 -0.002336 11.00000 0.01285 0.01197 = 0.02348 0.00152 0.00166 -0.00374 C9 1 0.723401 -0.144980 0.089879 11.00000 0.01394 0.01740 = 0.02109 0.00651 0.00236 -0.00349 C10 1 0.715155 -0.031875 0.094315 11.00000 0.01185 0.01913 = 0.01389 0.00122 0.00369 -0.00427 C11 1 0.833444 0.097022 -0.086180 11.00000 0.01759 0.01887 = 0.01199 -0.00007 0.00507 -0.00002 AFIX 137 H11A 2 0.862532 0.088457 -0.119668 11.00000 -1.50000 H11B 2 0.838846 0.168323 -0.057511 11.00000 -1.50000 H11C 2 0.791346 0.090155 -0.128255 11.00000 -1.50000 AFIX 0 C12 1 0.830312 -0.149491 -0.126590 11.00000 0.02163 0.02425 = 0.02365 -0.01297 0.00589 -0.00179 AFIX 137 H12A 2 0.869257 -0.169896 -0.134875 11.00000 -1.50000 H12B 2 0.808922 -0.096990 -0.173253 11.00000 -1.50000 H12C 2 0.804549 -0.213694 -0.131954 11.00000 -1.50000 AFIX 0 C13 1 0.863781 -0.279088 0.056187 11.00000 0.02536 0.01163 = 0.04217 -0.00515 -0.00050 0.00165 AFIX 137 H13A 2 0.836139 -0.312430 0.000818 11.00000 -1.50000 H13B 2 0.852472 -0.302823 0.108619 11.00000 -1.50000 H13C 2 0.906223 -0.300658 0.064494 11.00000 -1.50000 AFIX 0 C14 1 0.891556 -0.118746 0.219345 11.00000 0.01958 0.01504 = 0.01937 0.00493 -0.00089 -0.00092 AFIX 137 H14A 2 0.879256 -0.193791 0.223050 11.00000 -1.50000 H14B 2 0.872211 -0.072476 0.253249 11.00000 -1.50000 H14C 2 0.936355 -0.112697 0.245496 11.00000 -1.50000 AFIX 0 C15 1 0.680446 -0.085490 -0.158357 11.00000 0.01875 0.02116 = 0.01533 -0.00335 0.00082 0.00265 AFIX 137 H15A 2 0.698224 -0.150642 -0.175274 11.00000 -1.50000 H15B 2 0.697348 -0.021671 -0.178805 11.00000 -1.50000 H15C 2 0.635698 -0.086697 -0.187164 11.00000 -1.50000 AFIX 0 C16 1 0.708174 -0.288152 -0.036308 11.00000 0.02226 0.01247 = 0.03403 -0.00231 -0.00024 -0.00220 AFIX 137 H16A 2 0.734327 -0.334427 0.011939 11.00000 -1.50000 H16B 2 0.722719 -0.290092 -0.088806 11.00000 -1.50000 H16C 2 0.665669 -0.314134 -0.054429 11.00000 -1.50000 AFIX 0 C17 1 0.738872 -0.219676 0.169471 11.00000 0.02504 0.02410 = 0.02841 0.01249 0.00427 -0.00312 AFIX 137 H17A 2 0.701653 -0.235407 0.184623 11.00000 -1.50000 H17B 2 0.769463 -0.185686 0.221698 11.00000 -1.50000 H17C 2 0.755647 -0.286927 0.154295 11.00000 -1.50000 AFIX 0 C18 1 0.716851 0.021362 0.181315 11.00000 0.01747 0.02611 = 0.01349 0.00158 0.00591 -0.00517 AFIX 137 H18A 2 0.676551 0.014575 0.189407 11.00000 -1.50000 H18B 2 0.727003 0.097850 0.179257 11.00000 -1.50000 H18C 2 0.748109 -0.013470 0.232264 11.00000 -1.50000 AFIX 0 C19 1 0.977947 0.138867 0.124595 11.00000 0.01254 0.01989 = 0.01474 -0.00049 0.00471 -0.00062 AFIX 13 H19 2 1.002029 0.201819 0.158112 11.00000 -1.20000 AFIX 0 C20 1 0.975948 0.149591 0.026009 11.00000 0.01843 0.03149 = 0.01706 0.00005 0.00960 -0.00108 AFIX 137 H20A 2 1.017771 0.159294 0.024183 11.00000 -1.50000 H20B 2 0.950816 0.212135 -0.001851 11.00000 -1.50000 H20C 2 0.957974 0.084228 -0.007585 11.00000 -1.50000 AFIX 0 C21 1 1.013506 0.037670 0.167689 11.00000 0.01643 0.02805 = 0.02565 0.00521 0.00947 0.00553 AFIX 137 H21A 2 0.990438 -0.026477 0.138869 11.00000 -1.50000 H21B 2 1.019095 0.036826 0.232829 11.00000 -1.50000 H21C 2 1.053783 0.037777 0.159000 11.00000 -1.50000 AFIX 0 C22 1 0.921005 0.135620 0.262528 11.00000 0.01571 0.01682 = 0.01188 -0.00155 0.00391 -0.00178 AFIX 13 H22 2 0.941898 0.064663 0.281484 11.00000 -1.20000 AFIX 0 C23 1 0.865507 0.140327 0.295299 11.00000 0.02000 0.02931 = 0.01653 -0.00044 0.00750 -0.00072 AFIX 137 H23A 2 0.878250 0.121737 0.359975 11.00000 -1.50000 H23B 2 0.834315 0.088938 0.260553 11.00000 -1.50000 H23C 2 0.848275 0.213334 0.286437 11.00000 -1.50000 AFIX 0 C24 1 0.966165 0.224789 0.309082 11.00000 0.02804 0.03463 = 0.01589 -0.01001 0.00511 -0.01261 AFIX 137 H24A 2 0.947371 0.295273 0.289034 11.00000 -1.50000 H24B 2 1.003712 0.217662 0.292951 11.00000 -1.50000 H24C 2 0.976366 0.218604 0.375110 11.00000 -1.50000 AFIX 0 C25 1 0.613788 0.156327 -0.149815 11.00000 0.01467 0.01904 = 0.01511 0.00167 0.00195 0.00011 AFIX 13 H25 2 0.593456 0.227620 -0.150001 11.00000 -1.20000 AFIX 0 C26 1 0.645327 0.170243 -0.222076 11.00000 0.02729 0.02221 = 0.01433 0.00127 0.00527 0.00004 AFIX 137 H26A 2 0.648115 0.100119 -0.249470 11.00000 -1.50000 H26B 2 0.686724 0.199539 -0.193616 11.00000 -1.50000 H26C 2 0.621267 0.219953 -0.269255 11.00000 -1.50000 AFIX 0 C27 1 0.559604 0.076920 -0.178897 11.00000 0.02069 0.02785 = 0.02439 0.00094 0.00147 -0.00452 AFIX 137 H27A 2 0.545717 0.068367 -0.245087 11.00000 -1.50000 H27B 2 0.525765 0.104879 -0.160205 11.00000 -1.50000 H27C 2 0.572775 0.006875 -0.149945 11.00000 -1.50000 AFIX 0 C28 1 0.612670 0.164012 0.037120 11.00000 0.01484 0.02020 = 0.01986 -0.00124 0.00881 -0.00202 AFIX 13 H28 2 0.640289 0.172845 0.101323 11.00000 -1.20000 AFIX 0 C29 1 0.570797 0.067225 0.036565 11.00000 0.01917 0.02696 = 0.03007 0.00310 0.01289 -0.00393 AFIX 137 H29A 2 0.553760 0.074762 0.086264 11.00000 -1.50000 H29B 2 0.594754 0.000454 0.044629 11.00000 -1.50000 H29C 2 0.537193 0.064781 -0.021551 11.00000 -1.50000 AFIX 0 C30 1 0.574554 0.267884 0.012353 11.00000 0.02060 0.02334 = 0.03411 -0.00090 0.01546 0.00382 AFIX 137 H30A 2 0.546286 0.262663 -0.050138 11.00000 -1.50000 H30B 2 0.602082 0.329567 0.017418 11.00000 -1.50000 H30C 2 0.550963 0.277728 0.053970 11.00000 -1.50000 AFIX 0 C31 1 0.723835 0.243967 -0.014108 11.00000 0.01262 0.01205 = 0.01378 -0.00022 0.00509 -0.00056 AFIX 13 H31 2 0.749782 0.218334 -0.050469 11.00000 -1.20000 AFIX 0 C32 1 0.767637 0.249404 0.084403 11.00000 0.01155 0.01294 = 0.01342 0.00042 0.00393 -0.00156 AFIX 13 H32 2 0.773644 0.174692 0.109954 11.00000 -1.20000 AFIX 0 C33 1 0.745329 0.321298 0.147262 11.00000 0.01755 0.01798 = 0.01656 -0.00254 0.00750 -0.00041 AFIX 23 H33A 2 0.766870 0.299436 0.210903 11.00000 -1.20000 H33B 2 0.700891 0.308160 0.134585 11.00000 -1.20000 AFIX 0 C34 1 0.755257 0.442983 0.138436 11.00000 0.02580 0.01649 = 0.02059 -0.00472 0.00905 0.00243 AFIX 23 H34A 2 0.716375 0.475774 0.099404 11.00000 -1.20000 H34B 2 0.765978 0.476718 0.199255 11.00000 -1.20000 AFIX 0 C35 1 0.805388 0.466780 0.098530 11.00000 0.02155 0.00703 = 0.02531 -0.00180 0.00454 0.00072 AFIX 43 H35 2 0.843279 0.491919 0.139631 11.00000 -1.20000 AFIX 0 C36 1 0.802377 0.456234 0.010097 11.00000 0.01839 0.00849 = 0.02560 0.00244 0.00632 0.00111 AFIX 43 H36 2 0.839395 0.470987 -0.002139 11.00000 -1.20000 AFIX 0 C37 1 0.748473 0.424449 -0.070685 11.00000 0.02079 0.01285 = 0.01772 0.00281 0.00581 0.00069 AFIX 23 H37A 2 0.764649 0.386239 -0.113892 11.00000 -1.20000 H37B 2 0.728750 0.491487 -0.101009 11.00000 -1.20000 AFIX 0 C38 1 0.698444 0.354035 -0.055399 11.00000 0.01795 0.01210 = 0.01762 0.00239 0.00348 0.00007 AFIX 23 H38A 2 0.665373 0.342554 -0.114095 11.00000 -1.20000 H38B 2 0.680382 0.391743 -0.014110 11.00000 -1.20000 AFIX 0 P1 3 0.900793 0.147204 0.137742 11.00000 0.01063 0.01002 = 0.01035 -0.00138 0.00308 -0.00141 P2 3 0.662955 0.140652 -0.031535 11.00000 0.01054 0.01120 = 0.01310 -0.00009 0.00354 -0.00043 CL1 4 0.947448 0.404458 0.104455 11.00000 0.01864 0.02110 = 0.03129 0.00140 0.00584 -0.00873 FE1 5 0.782437 -0.062295 0.035333 11.00000 0.01115 0.00862 = 0.01209 0.00016 0.00121 -0.00098 PD1 6 0.852376 0.310353 0.089815 11.00000 0.01244 0.00865 = 0.01486 -0.00054 0.00379 -0.00218 MOLE 2 CL11 4 0.538259 -0.224485 -0.146316 11.00000 0.03528 0.02810 = 0.03578 0.00295 0.01725 0.00159 MOLE 3 O51 7 0.569384 0.420469 -0.227120 11.00000 0.02897 0.03461 = 0.03844 0.00170 0.00393 0.00989 H51A 2 0.538323 0.387074 -0.262701 11.00000 -1.50000 H51B 2 0.554989 0.449090 -0.189452 11.00000 -1.50000 MOLE 4 O52 7 0.601896 -0.133703 0.231606 11.00000 0.03948 0.04310 = 0.04803 0.00723 0.02560 0.00188 H52A 2 0.586752 -0.178984 0.258829 11.00000 -1.50000 H52B 2 0.592511 -0.072071 0.245542 11.00000 -1.50000 MOLE 5 O53 7 0.588549 -0.251165 0.074350 11.00000 0.05027 0.05186 = 0.03740 0.00043 0.00639 -0.01435 H53A 2 0.575610 -0.219850 0.023855 11.00000 -1.50000 H53B 2 0.584595 -0.207451 0.113026 11.00000 -1.50000 MOLE 6 O54 7 0.467480 0.031129 -0.404010 11.00000 0.06340 0.02847 = 0.02474 -0.00208 0.01061 0.00277 H54A 2 0.444443 0.025118 -0.458344 11.00000 -1.50000 H54B 2 0.463034 0.096686 -0.390988 11.00000 -1.50000 MOLE 7 O55 7 0.588281 0.528874 0.092828 11.00000 0.05713 0.03650 = 0.03374 0.00781 0.00317 -0.00136 H55A 2 0.556222 0.526849 0.108663 11.00000 -1.50000 H55B 2 0.594899 0.594727 0.090160 11.00000 -1.50000 MOLE 8 O56 7 1.071595 0.423804 0.057835 11.00000 0.08072 0.14170 = 0.08526 0.01945 0.04530 0.01139 H56A 2 1.038273 0.413999 0.068757 11.00000 -1.50000 H56B 2 1.061367 0.452425 0.005490 11.00000 -1.50000 HKLF 4 1 0 0 -1 0 -1 0 -1 0 0 REM s93 in P2(1)/c REM R1 = 0.0320 for 8501 Fo > 4sig(Fo) and 0.0389 for all 9597 data REM 503 parameters refined using 18 restraints END WGHT 0.0324 6.3850 REM Highest difference peak 0.514, deepest hole -0.925, 1-sigma level 0.080 Q1 1 0.6611 0.1388 0.0225 11.00000 0.05 0.48 Q2 1 0.8555 0.2993 0.0474 11.00000 0.05 0.47 Q3 1 0.9797 0.1440 0.0724 11.00000 0.05 0.42 Q4 1 0.6315 0.1594 0.0009 11.00000 0.05 0.41 Q5 1 0.8635 0.0210 0.0268 11.00000 0.05 0.37