TITL pbca in Pbca CELL 0.71073 14.7295 14.7023 26.7711 90.000 90.000 90.000 ZERR 16.00 0.0004 0.0004 0.0008 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N O UNIT 288 224 64 16 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 FMAP 2 PLAN 5 DFIX 0.89 0.01 N4 H4A N4 H4B N24 H24A N24 H24B size 0.34 0.12 0.05 EQIV $1 -x, -y+1, -z EQIV $2 -x+1/2, y-1/2, z HTAB N1 O21_$1 HTAB N4 O1 HTAB N4 N22_$2 HTAB N21 O1_$1 HTAB N24 O21 acta BOND $H L.S. 9 TEMP -153.00 WGHT 0.010000 9.386000 EXTI 0.000714 FVAR 0.08828 MOLE 1 C1 1 0.186304 0.449788 0.048849 11.00000 0.01933 0.01473 = 0.01932 -0.00145 0.00160 0.00206 C2 1 0.252818 0.450397 0.087439 11.00000 0.01742 0.01919 = 0.01607 -0.00022 0.00002 0.00158 C3 1 0.330214 0.507221 0.086656 11.00000 0.02033 0.02096 = 0.01875 -0.00301 -0.00115 0.00044 C4 1 0.337663 0.574489 0.047857 11.00000 0.02070 0.01927 = 0.02174 0.00051 -0.00107 -0.00240 AFIX 43 H4 2 0.385887 0.617394 0.047619 11.00000 -1.20000 AFIX 0 C5 1 0.273590 0.574407 0.011785 11.00000 0.02148 0.01687 = 0.01841 -0.00111 0.00048 -0.00029 C6 1 0.265214 0.390965 0.127211 11.00000 0.01996 0.01889 = 0.01941 -0.00256 0.00093 0.00322 C7 1 0.275455 0.637616 -0.031489 11.00000 0.01474 0.02198 = 0.02091 0.00118 0.00002 0.00056 C8 1 0.301665 0.728238 -0.024873 11.00000 0.02249 0.02472 = 0.02423 0.00002 -0.00046 -0.00166 AFIX 43 H8 2 0.319920 0.748845 0.007226 11.00000 -1.20000 AFIX 0 C9 1 0.301194 0.788085 -0.064749 11.00000 0.02387 0.02106 = 0.03243 0.00449 -0.00137 -0.00198 AFIX 43 H9 2 0.318120 0.849759 -0.059716 11.00000 -1.20000 AFIX 0 C10 1 0.276226 0.758747 -0.111960 11.00000 0.02624 0.02540 = 0.02734 0.00947 0.00286 0.00354 AFIX 43 H10 2 0.275814 0.800007 -0.139268 11.00000 -1.20000 AFIX 0 C11 1 0.251838 0.668547 -0.118958 11.00000 0.02948 0.02748 = 0.01994 -0.00027 -0.00034 0.00175 AFIX 43 H11 2 0.235704 0.647850 -0.151381 11.00000 -1.20000 AFIX 0 C12 1 0.250750 0.608419 -0.079267 11.00000 0.02549 0.02037 = 0.02236 -0.00029 0.00116 0.00001 AFIX 43 H12 2 0.233134 0.546993 -0.084493 11.00000 -1.20000 AFIX 0 C13 1 0.396513 0.365223 0.184785 11.00000 0.02591 0.01982 = 0.02004 -0.00097 -0.00544 -0.00047 C14 1 0.487282 0.346677 0.176170 11.00000 0.02716 0.03481 = 0.02406 0.00335 -0.00031 0.00041 AFIX 43 H14 2 0.516460 0.368904 0.146972 11.00000 -1.20000 AFIX 0 C15 1 0.535122 0.295209 0.210723 11.00000 0.02565 0.05069 = 0.02959 0.00294 -0.00226 0.01211 AFIX 43 H15 2 0.597467 0.282068 0.205198 11.00000 -1.20000 AFIX 0 C16 1 0.492287 0.262874 0.253290 11.00000 0.04146 0.03240 = 0.02213 0.00223 -0.00551 0.01157 AFIX 43 H16 2 0.525034 0.227163 0.276743 11.00000 -1.20000 AFIX 0 C17 1 0.401585 0.282811 0.261510 11.00000 0.03803 0.02995 = 0.01867 -0.00029 -0.00170 0.00403 AFIX 43 H17 2 0.372298 0.260520 0.290660 11.00000 -1.20000 AFIX 0 C18 1 0.353221 0.334930 0.227628 11.00000 0.02494 0.03001 = 0.02047 -0.00074 -0.00116 0.00137 AFIX 43 H18 2 0.291389 0.349677 0.233653 11.00000 -1.20000 AFIX 0 N1 3 0.201290 0.512862 0.011960 11.00000 0.02002 0.01960 = 0.01606 0.00043 -0.00324 -0.00084 AFIX 43 H1 2 0.162893 0.514661 -0.013204 11.00000 -1.20000 AFIX 0 N2 3 0.389216 0.485880 0.122680 11.00000 0.02582 0.02316 = 0.02108 0.00485 -0.00464 -0.00416 N3 3 0.346447 0.414225 0.147672 11.00000 0.02167 0.02116 = 0.01971 0.00286 -0.00297 -0.00255 N4 3 0.209229 0.322811 0.144049 11.00000 0.02075 0.02265 = 0.02247 0.00331 -0.00115 0.00064 AFIX 2 0.8900 H4A 2 0.166565 0.312250 0.121393 11.00000 -1.50000 H4B 2 0.238350 0.273114 0.154349 11.00000 -1.50000 AFIX 0 O1 4 0.120931 0.395999 0.047342 11.00000 0.02056 0.02125 = 0.02263 0.00202 -0.00119 -0.00196 MOLE 2 C21 1 -0.005938 0.572338 0.069875 11.00000 0.01787 0.01741 = 0.02065 -0.00102 0.00058 0.00058 C22 1 0.057418 0.588330 0.109274 11.00000 0.02162 0.01723 = 0.01752 -0.00155 0.00090 0.00084 C23 1 0.122186 0.659331 0.107680 11.00000 0.02231 0.01696 = 0.01948 -0.00201 -0.00051 -0.00094 C24 1 0.122919 0.720425 0.066310 11.00000 0.02437 0.01795 = 0.02220 -0.00004 -0.00114 -0.00495 AFIX 43 H24 2 0.163956 0.770224 0.065081 11.00000 -1.20000 AFIX 0 C25 1 0.063410 0.705095 0.029021 11.00000 0.01954 0.01914 = 0.01929 -0.00013 0.00016 -0.00062 C26 1 0.075893 0.541068 0.153102 11.00000 0.02085 0.01837 = 0.01949 -0.00233 0.00283 0.00226 C27 1 0.058980 0.763224 -0.016311 11.00000 0.01573 0.02215 = 0.02223 0.00255 -0.00105 -0.00027 C28 1 0.074930 0.856921 -0.012507 11.00000 0.02341 0.02403 = 0.03045 0.00218 -0.00711 -0.00308 AFIX 43 H28 2 0.088268 0.883072 0.019102 11.00000 -1.20000 AFIX 0 C29 1 0.071352 0.911706 -0.054650 11.00000 0.02411 0.02258 = 0.04227 0.01049 -0.00279 -0.00138 AFIX 43 H29 2 0.082263 0.975184 -0.051840 11.00000 -1.20000 AFIX 0 C30 1 0.051849 0.873867 -0.100900 11.00000 0.02052 0.03801 = 0.02858 0.01490 0.00501 0.00238 AFIX 43 H30 2 0.048787 0.911442 -0.129720 11.00000 -1.20000 AFIX 0 C31 1 0.036870 0.781237 -0.104928 11.00000 0.02347 0.04125 = 0.01966 0.00600 0.00428 0.00272 AFIX 43 H31 2 0.023585 0.755437 -0.136631 11.00000 -1.20000 AFIX 0 C32 1 0.041072 0.725721 -0.063110 11.00000 0.01784 0.02701 = 0.02100 0.00201 0.00072 -0.00045 AFIX 43 H32 2 0.031735 0.662061 -0.066361 11.00000 -1.20000 AFIX 0 C33 1 0.193910 0.564662 0.220207 11.00000 0.02713 0.01862 = 0.01646 -0.00155 -0.00210 0.00404 C34 1 0.286593 0.581287 0.221876 11.00000 0.03013 0.02139 = 0.02111 0.00027 -0.00124 -0.00092 AFIX 43 H34 2 0.317411 0.603547 0.193201 11.00000 -1.20000 AFIX 0 C35 1 0.333854 0.565081 0.265847 11.00000 0.02964 0.02463 = 0.02637 0.00120 -0.00544 -0.00145 AFIX 43 H35 2 0.397280 0.576511 0.267277 11.00000 -1.20000 AFIX 0 C36 1 0.289146 0.532379 0.307608 11.00000 0.03634 0.02363 = 0.02042 -0.00021 -0.00615 0.00571 AFIX 43 H36 2 0.321667 0.521519 0.337667 11.00000 -1.20000 AFIX 0 C37 1 0.196971 0.515615 0.305346 11.00000 0.03450 0.03109 = 0.01850 0.00417 0.00418 0.00773 AFIX 43 H37 2 0.166419 0.492705 0.333953 11.00000 -1.20000 AFIX 0 C38 1 0.148344 0.531831 0.261758 11.00000 0.02612 0.02838 = 0.02316 0.00420 0.00027 0.00424 AFIX 43 H38 2 0.084874 0.520588 0.260465 11.00000 -1.20000 AFIX 0 N21 3 0.003328 0.632013 0.030593 11.00000 0.01985 0.01993 = 0.01720 -0.00113 -0.00390 -0.00236 AFIX 43 H21 2 -0.031547 0.623280 0.004338 11.00000 -1.20000 AFIX 0 N22 3 0.177154 0.658216 0.147083 11.00000 0.02858 0.01911 = 0.01728 0.00307 -0.00281 -0.00212 N23 3 0.146435 0.584968 0.175192 11.00000 0.02488 0.02073 = 0.01676 0.00070 -0.00152 -0.00056 N24 3 0.032304 0.466457 0.172318 11.00000 0.02549 0.02517 = 0.02589 0.00795 -0.00201 -0.00288 AFIX 2 0.8900 H24A 2 -0.006941 0.443008 0.150572 11.00000 -1.50000 H24B 2 0.066096 0.427936 0.190289 11.00000 -1.50000 AFIX 0 O21 4 -0.065387 0.511747 0.069572 11.00000 0.02132 0.01978 = 0.02803 0.00229 -0.00310 -0.00303 HKLF 4 REM pbca in Pbca REM R1 = 0.0654 for 5012 Fo > 4sig(Fo) and 0.0912 for all 6537 data REM 428 parameters refined using 4 restraints END WGHT 0.0000 9.3967 REM Highest difference peak 0.320, deepest hole -0.263, 1-sigma level 0.062 Q1 1 0.2524 0.4142 0.1032 11.00000 0.05 0.32 Q2 1 0.2481 0.6809 -0.0287 11.00000 0.05 0.31 Q3 1 0.2461 0.6179 -0.0529 11.00000 0.05 0.28 Q4 1 0.0711 0.6380 0.1122 11.00000 0.05 0.27 Q5 1 0.2274 0.4419 0.0667 11.00000 0.05 0.27