++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XL - CRYSTAL STRUCTURE REFINEMENT - SHELXTL Version 2008/4 + + Copyright(c) 2008 Bruker Analytical X-ray Solutions All Rights Reserved + + cfc1s started at 11:38:48 on 26-Jan-2011 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL cfc1s in P1 CELL 1.54178 5.4215 5.0420 21.6621 90.000 95.886 90.000 ZERR 2.00 0.0006 0.0006 0.0028 0.000 0.008 0.000 LATT -1 SFAC C H O UNIT 34 28 2 V = 589.02 F(000) = 248.0 Mu = 0.63 mm-1 Cell Wt = 468.56 Rho = 1.321 TEMP -173.150 SIZE 0.022 0.042 0.255 L.S. 4 BOND FMAP 2 PLAN 20 LIST 4 WGHT 0.100000 FVAR 0.39333 O1 3 0.62345 0.21397 0.58818 11.00000 0.02696 0.05250 = 0.05168 0.00286 0.00198 0.00258 O2 3 0.29777 -0.07248 0.45772 11.00000 0.03834 0.01726 = 0.05433 -0.00307 0.00212 0.01039 O3 3 0.11667 0.44005 0.08899 11.00000 0.02717 0.04046 = 0.04143 -0.00052 0.00431 -0.00234 O4 3 0.78805 0.72845 0.95781 11.00000 0.04545 0.01761 = 0.05988 0.00197 -0.00098 -0.00811 C5 1 0.38901 0.55461 0.62648 11.00000 0.00850 0.04527 = 0.05150 -0.00075 0.01246 -0.00920 C6 1 -0.12610 0.09178 0.12701 11.00000 0.01902 0.04160 = 0.04028 -0.00138 0.00537 0.00645 O7 3 -0.25032 0.33791 0.03730 11.00000 0.03946 0.02941 = 0.05571 0.00483 -0.00166 -0.00790 C8 1 0.53517 0.79796 0.72091 11.00000 0.01897 0.02196 = 0.07866 0.00264 0.00891 0.00259 AFIX 43 H8A 2 0.65360 0.82413 0.75584 11.00000 -1.20000 AFIX 0 C9 1 -0.32099 -0.06006 0.12108 11.00000 0.03801 0.02965 = 0.04308 -0.00127 0.00495 -0.00290 AFIX 43 H9A 2 -0.44133 -0.03580 0.08646 11.00000 -1.20000 AFIX 0 O10 3 0.25266 0.32200 0.53654 11.00000 0.04473 0.03561 = 0.04435 0.00262 -0.00215 0.00476 C11 1 0.43094 0.34874 0.58106 11.00000 0.01608 0.03494 = 0.03074 0.00431 0.00276 -0.01178 C12 1 0.99437 0.85129 0.96651 11.00000 0.05162 0.02330 = 0.03139 -0.00774 0.00953 -0.00486 O13 3 0.66199 -0.16524 0.51047 11.00000 0.03134 0.03544 = 0.04773 -0.00523 -0.00132 0.00066 C14 1 0.88391 1.30036 0.82692 11.00000 0.03916 0.03129 = 0.03894 0.00239 -0.00170 0.00118 AFIX 43 H14A 2 0.75843 1.32769 0.79358 11.00000 -1.20000 AFIX 0 C15 1 0.33598 0.94617 0.71441 11.00000 0.03223 0.04393 = 0.05558 0.00224 0.00884 -0.01761 AFIX 43 H15A 2 0.32166 1.08472 0.74355 11.00000 -1.20000 AFIX 0 C16 1 -0.18605 -0.30372 0.21326 11.00000 0.03275 0.04778 = 0.04598 -0.00646 0.01065 -0.01416 AFIX 43 H16A 2 -0.21091 -0.43781 0.24281 11.00000 -1.20000 AFIX 0 C17 1 0.60427 -0.80491 0.33281 11.00000 0.04529 0.01347 = 0.03993 -0.00499 0.01563 0.01338 AFIX 43 H17A 2 0.63517 -0.92947 0.30161 11.00000 -1.20000 AFIX 0 O18 3 1.15751 0.82430 1.01061 11.00000 0.03908 0.04026 = 0.03166 0.00032 -0.00579 0.00115 C19 1 1.08750 1.45142 0.83191 11.00000 0.05606 0.01790 = 0.04149 0.00732 0.00786 0.01498 AFIX 43 H19A 2 1.10895 1.58245 0.80140 11.00000 -1.20000 AFIX 0 C20 1 0.85596 1.10481 0.87016 11.00000 0.04356 0.00783 = 0.04171 -0.00395 -0.00516 -0.00579 AFIX 43 H20A 2 0.71582 0.99102 0.86443 11.00000 -1.20000 AFIX 0 C21 1 0.57773 0.60071 0.67729 11.00000 0.02643 0.03593 = 0.05484 0.00679 0.00667 -0.01829 AFIX 43 H21A 2 0.72689 0.50048 0.68119 11.00000 -1.20000 AFIX 0 C22 1 0.17690 0.71969 0.62177 11.00000 0.02934 0.01955 = 0.05579 0.00527 0.00833 -0.00398 AFIX 43 H22A 2 0.05712 0.69766 0.58695 11.00000 -1.20000 AFIX 0 C23 1 0.35959 -0.45739 0.37024 11.00000 0.04210 0.01869 = 0.03848 0.00435 -0.00029 0.01696 AFIX 43 H23A 2 0.21789 -0.34552 0.36563 11.00000 -1.20000 AFIX 0 C24 1 0.53119 -0.42160 0.41876 11.00000 0.06099 -0.00037 = 0.03059 0.00349 0.00442 0.00689 C25 1 0.74671 -0.57105 0.42529 11.00000 0.03357 0.03761 = 0.04332 -0.00566 -0.00311 0.00661 AFIX 43 H25A 2 0.87527 -0.53896 0.45763 11.00000 -1.20000 AFIX 0 C26 1 1.01717 1.07129 0.91896 11.00000 0.03602 0.01171 = 0.03529 -0.00582 0.00465 -0.00371 C27 1 -0.35892 -0.26374 0.16559 11.00000 0.03423 0.00092 = 0.07916 0.00195 0.00549 0.00338 AFIX 43 H27A 2 -0.50518 -0.36871 0.16117 11.00000 -1.20000 AFIX 0 C28 1 0.51169 -0.20763 0.46682 11.00000 0.04801 0.00678 = 0.05083 0.00185 0.00162 0.01251 C29 1 0.13459 0.91086 0.66498 11.00000 0.01460 0.00901 = 0.08316 0.00105 0.00932 0.00222 AFIX 43 H29A 2 -0.01407 1.01173 0.66275 11.00000 -1.20000 AFIX 0 C30 1 0.07416 0.04355 0.17657 11.00000 0.01596 0.04988 = 0.05011 0.00133 0.01068 0.00182 AFIX 43 H30A 2 0.22497 0.14051 0.17836 11.00000 -1.20000 AFIX 0 C31 1 0.03732 -0.14706 0.22063 11.00000 0.04863 0.03790 = 0.04821 -0.00109 0.00568 -0.00058 AFIX 43 H31A 2 0.15733 -0.17423 0.25518 11.00000 -1.20000 AFIX 0 C32 1 -0.07999 0.29113 0.08060 11.00000 0.01627 0.02614 = 0.04602 -0.00106 0.00034 0.00459 C33 1 0.76376 -0.77275 0.38126 11.00000 0.05051 0.03813 = 0.03722 0.00604 0.00224 -0.00128 AFIX 43 H33A 2 0.89946 -0.89243 0.38721 11.00000 -1.20000 AFIX 0 C34 1 1.26769 1.41724 0.88159 11.00000 0.04202 0.06186 = 0.02908 -0.00404 0.01115 -0.01263 AFIX 43 H34A 2 1.40899 1.52976 0.88487 11.00000 -1.20000 AFIX 0 C35 1 1.24963 1.23172 0.92500 11.00000 0.02988 0.03044 = 0.04879 0.00355 -0.00010 -0.00102 AFIX 43 H35A 2 1.37734 1.20370 0.95778 11.00000 -1.20000 AFIX 0 C36 1 0.38504 -0.65291 0.32710 11.00000 0.06020 0.04931 = 0.01722 -0.00068 -0.00551 -0.01784 AFIX 43 H36A 2 0.25822 -0.68465 0.29431 11.00000 -1.20000 AFIX 0 HKLF 4 Covalent radii and connectivity table for cfc1s in P1 C 0.770 H 0.320 O 0.660 O1 - C11 O2 - C28 O3 - C32 O4 - C12 C5 - C22 C21 C11 C6 - C9 C32 C30 O7 - C32 C8 - C15 C21 C9 - C6 C27 O10 - C11 C11 - O1 O10 C5 C12 - O18 O4 C26 O13 - C28 C14 - C19 C20 C15 - C8 C29 C16 - C27 C31 C17 - C33 C36 O18 - C12 C19 - C14 C34 C20 - C26 C14 C21 - C8 C5 C22 - C29 C5 C23 - C24 C36 C24 - C23 C25 C28 C25 - C24 C33 C26 - C20 C35 C12 C27 - C16 C9 C28 - O13 O2 C24 C29 - C22 C15 C30 - C31 C6 C31 - C30 C16 C32 - O7 O3 C6 C33 - C17 C25 C34 - C35 C19 C35 - C34 C26 C36 - C23 C17 Floating origin restraints generated 3923 Reflections read, of which 0 rejected -5 =< h =< 6, -5 =< k =< 5, -25 =< l =< 25, Max. 2-theta = 134.07 0 Systematic absence violations 0 Inconsistent equivalents 2701 Unique reflections, of which 0 suppressed R(int) = 0.0439 R(sigma) = 0.0849 Friedel opposites not merged Maximum memory for data reduction = 2583 / 28286 Default effective X-H distances for T = -173.2 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 1.00 0.99 0.98 0.95 0.88 0.91 1.12 0.84 0.95 0.88 0.95 Note that these distances are chosen to give the best fit to the X-ray data and so avoid the introduction of systematic error. The true internuclear distances are longer and do not vary with temperature ! The apparent variation with temperature is caused by libration. ** Cell contents from UNIT instruction and atom list do not agree ** Unit-cell contents from UNIT instruction and atom list resp. C 34.00 28.00 H 28.00 20.00 O 2.00 8.00 Least-squares cycle 1 Maximum vector length = 511 Memory required = 3460 / 407748 wR2 = 0.2386 before cycle 1 for 2701 data and 325 / 325 parameters GooF = S = 1.434; Restrained GooF = 1.433 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39368 0.00222 0.159 OSF Mean shift/esd = 0.202 Maximum = 1.030 for U22 C5 Max. shift = 0.011 A for H31A Max. dU = 0.002 for C5 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3460 / 407748 wR2 = 0.2370 before cycle 2 for 2701 data and 325 / 325 parameters GooF = S = 1.423; Restrained GooF = 1.422 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39416 0.00221 0.216 OSF Mean shift/esd = 0.195 Maximum = 1.081 for U22 C5 Max. shift = 0.010 A for C16 Max. dU = 0.002 for C5 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3460 / 407748 wR2 = 0.2358 before cycle 3 for 2701 data and 325 / 325 parameters GooF = S = 1.416; Restrained GooF = 1.415 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39432 0.00220 0.072 OSF Mean shift/esd = 0.110 Maximum = 0.511 for U33 O1 Max. shift = 0.005 A for C30 Max. dU = 0.001 for C33 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3460 / 407748 wR2 = 0.2354 before cycle 4 for 2701 data and 325 / 325 parameters GooF = S = 1.413; Restrained GooF = 1.413 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.39428 0.00220 -0.019 OSF Mean shift/esd = 0.073 Maximum = -0.279 for x C32 Max. shift = 0.003 A for C32 Max. dU = 0.000 for C8 Largest correlation matrix elements -0.789 U23 O13 / U23 O10 0.760 z O18 / z O7 -0.744 U33 O13 / U33 O10 -0.786 U23 C31 / U23 C14 0.757 z O2 / z O1 0.743 z C30 / z C20 0.783 z C31 / z C14 0.755 z C25 / z C22 -0.741 U23 C35 / U23 C9 0.775 z O13 / z O10 -0.755 U23 C32 / U23 C12 -0.739 U33 C31 / U33 C14 0.774 z C32 / z C12 -0.750 U23 C19 / U23 C16 0.738 z C26 / z C6 -0.771 U23 C25 / U23 C22 -0.748 U23 C30 / U23 C20 0.737 z C35 / z C9 -0.767 U23 O2 / U23 O1 -0.747 U23 C34 / U23 C27 -0.736 U13 O2 / U13 O1 -0.762 U23 O18 / U23 O7 -0.746 U33 O2 / U33 O1 0.734 z C34 / z C27 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H8A 0.6530 0.8230 0.7554 43 0.950 0.002 C8 C15 C21 H9A -0.4413 -0.0396 0.0865 43 0.950 0.003 C9 C6 C27 H14A 0.7595 1.3201 0.7929 43 0.950 0.001 C14 C19 C20 H15A 0.3211 1.0821 0.7441 43 0.950 0.001 C15 C8 C29 H16A -0.2150 -0.4303 0.2433 43 0.950 0.002 C16 C27 C31 H17A 0.6328 -0.9330 0.3021 43 0.950 0.000 C17 C33 C36 H19A 1.1071 1.5870 0.8018 43 0.950 0.002 C19 C14 C34 H20A 0.7133 0.9959 0.8643 43 0.950 0.001 C20 C26 C14 H21A 0.7284 0.5044 0.6810 43 0.950 0.002 C21 C8 C5 H22A 0.0579 0.6981 0.5870 43 0.950 0.001 C22 C29 C5 H23A 0.2226 -0.3406 0.3653 43 0.950 0.002 C23 C24 C36 H25A 0.8756 -0.5402 0.4578 43 0.950 0.000 C25 C24 C33 H27A -0.5045 -0.3680 0.1612 43 0.950 0.003 C27 C16 C9 H29A -0.0132 1.0121 0.6623 43 0.950 0.000 C29 C22 C15 H30A 0.2227 0.1467 0.1784 43 0.950 0.001 C30 C31 C6 H31A 0.1580 -0.1851 0.2544 43 0.950 0.001 C31 C30 C16 H33A 0.9017 -0.8923 0.3865 43 0.950 0.001 C33 C17 C25 H34A 1.4094 1.5328 0.8852 43 0.950 0.004 C34 C35 C19 H35A 1.3765 1.1977 0.9578 43 0.950 0.003 C35 C34 C26 H36A 0.2570 -0.6849 0.2941 43 0.950 0.001 C36 C23 C17 cfc1s in P1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq O1 0.62393 0.21272 0.58805 1.00000 0.02320 0.04382 0.06160 0.00443 0.00452 0.00373 0.04286 0.01404 0.00122 0.00143 0.00042 0.00000 0.00373 0.00411 0.00594 0.00402 0.00347 0.00293 0.00200 O2 0.29874 -0.07322 0.45760 1.00000 0.04231 0.02347 0.04651 -0.00456 0.00001 0.00969 0.03774 0.01283 0.00127 0.00126 0.00038 0.00000 0.00408 0.00341 0.00505 0.00329 0.00352 0.00276 0.00179 O3 0.11658 0.44058 0.08888 1.00000 0.02641 0.04550 0.04183 -0.00233 0.00331 -0.00200 0.03793 0.01216 0.00114 0.00142 0.00037 0.00000 0.00354 0.00419 0.00449 0.00341 0.00301 0.00274 0.00175 O4 0.78820 0.72880 0.95782 1.00000 0.04533 0.01681 0.05920 0.00323 -0.00039 -0.00782 0.04084 0.01285 0.00122 0.00130 0.00041 0.00000 0.00407 0.00318 0.00533 0.00313 0.00346 0.00266 0.00194 C5 0.38990 0.55470 0.62686 1.00000 0.00834 0.06208 0.04557 0.00105 0.01212 -0.00981 0.03802 0.01815 0.00154 0.00208 0.00054 0.00000 0.00422 0.00645 0.00702 0.00537 0.00377 0.00400 0.00271 C6 -0.12626 0.09213 0.12694 1.00000 0.02074 0.04308 0.03942 -0.00254 0.00549 0.00607 0.03425 0.01982 0.00177 0.00206 0.00056 0.00000 0.00449 0.00562 0.00626 0.00456 0.00376 0.00381 0.00239 O7 -0.24902 0.33553 0.03737 1.00000 0.03971 0.02671 0.05087 0.00541 -0.00315 -0.01043 0.03964 0.01291 0.00124 0.00131 0.00040 0.00000 0.00382 0.00342 0.00530 0.00343 0.00349 0.00277 0.00191 C8 0.53437 0.79717 0.72045 1.00000 0.01568 0.02334 0.08771 0.00102 0.01348 0.00244 0.04168 0.01998 0.00167 0.00178 0.00062 0.00000 0.00484 0.00484 0.00896 0.00519 0.00478 0.00358 0.00290 H8A 0.65296 0.82296 0.75536 1.00000 0.05002 0.00000 0.00000 C9 -0.32123 -0.06205 0.12122 1.00000 0.03391 0.04140 0.04167 -0.00249 0.00449 -0.00381 0.03895 0.02004 0.00198 0.00210 0.00057 0.00000 0.00547 0.00588 0.00677 0.00508 0.00456 0.00442 0.00261 H9A -0.44128 -0.03963 0.08647 1.00000 0.04674 0.00000 0.00000 O10 0.25375 0.32241 0.53672 1.00000 0.04125 0.03809 0.04618 0.00265 -0.00181 0.00111 0.04227 0.01419 0.00135 0.00152 0.00041 0.00000 0.00428 0.00416 0.00531 0.00381 0.00368 0.00312 0.00198 C11 0.42945 0.35048 0.58115 1.00000 0.01691 0.04353 0.02585 0.00680 0.00330 -0.01258 0.02869 0.01584 0.00148 0.00191 0.00046 0.00000 0.00436 0.00522 0.00520 0.00415 0.00362 0.00376 0.00233 C12 0.99055 0.85022 0.96655 1.00000 0.04875 0.02281 0.03653 -0.00419 0.00962 -0.00227 0.03567 0.01971 0.00205 0.00188 0.00056 0.00000 0.00628 0.00490 0.00658 0.00446 0.00491 0.00424 0.00248 O13 0.66290 -0.16446 0.51056 1.00000 0.03627 0.03317 0.04718 -0.00565 -0.00165 0.00281 0.03929 0.01334 0.00127 0.00144 0.00041 0.00000 0.00398 0.00400 0.00532 0.00366 0.00347 0.00296 0.00187 C14 0.88322 1.29686 0.82681 1.00000 0.04012 0.02992 0.03976 0.00099 -0.00400 0.00195 0.03716 0.01915 0.00192 0.00206 0.00059 0.00000 0.00566 0.00523 0.00659 0.00497 0.00495 0.00426 0.00255 H14A 0.75947 1.32007 0.79289 1.00000 0.04459 0.00000 0.00000 C15 0.33588 0.94522 0.71457 1.00000 0.03404 0.04486 0.05493 0.00523 0.00869 -0.01749 0.04432 0.02024 0.00181 0.00222 0.00061 0.00000 0.00575 0.00616 0.00812 0.00577 0.00512 0.00485 0.00301 H15A 0.32106 1.08214 0.74409 1.00000 0.05319 0.00000 0.00000 C16 -0.18693 -0.29978 0.21316 1.00000 0.03182 0.05308 0.04915 -0.00403 0.01379 -0.01369 0.04401 0.02011 0.00181 0.00237 0.00059 0.00000 0.00549 0.00656 0.00759 0.00570 0.00489 0.00462 0.00296 H16A -0.21497 -0.43032 0.24328 1.00000 0.05282 0.00000 0.00000 C17 0.60333 -0.80641 0.33297 1.00000 0.04438 0.01286 0.04243 -0.00618 0.01450 0.01432 0.03253 0.01855 0.00174 0.00159 0.00053 0.00000 0.00548 0.00454 0.00629 0.00427 0.00456 0.00362 0.00235 H17A 0.63275 -0.93298 0.30208 1.00000 0.03904 0.00000 0.00000 O18 1.15819 0.82264 1.01071 1.00000 0.03868 0.04711 0.03551 -0.00037 -0.00480 0.00334 0.04103 0.01323 0.00127 0.00144 0.00038 0.00000 0.00392 0.00422 0.00465 0.00357 0.00326 0.00313 0.00186 C19 1.08775 1.45407 0.83199 1.00000 0.05810 0.01571 0.03813 0.00477 0.00426 0.01428 0.03736 0.01940 0.00194 0.00173 0.00051 0.00000 0.00673 0.00466 0.00644 0.00440 0.00500 0.00398 0.00268 H19A 1.10711 1.58697 0.80178 1.00000 0.04483 0.00000 0.00000 C20 0.85501 1.10750 0.86971 1.00000 0.04458 0.00862 0.04634 -0.00525 -0.00166 -0.00649 0.03362 0.01662 0.00179 0.00157 0.00052 0.00000 0.00527 0.00426 0.00669 0.00410 0.00459 0.00355 0.00241 H20A 0.71328 0.99586 0.86427 1.00000 0.04034 0.00000 0.00000 C21 0.57812 0.60271 0.67726 1.00000 0.02449 0.03305 0.05756 0.00638 0.00715 -0.01750 0.03816 0.01806 0.00173 0.00190 0.00057 0.00000 0.00464 0.00537 0.00769 0.00509 0.00443 0.00397 0.00276 H21A 0.72841 0.50442 0.68102 1.00000 0.04579 0.00000 0.00000 C22 0.17737 0.72026 0.62190 1.00000 0.03074 0.02353 0.05140 0.00827 0.00706 -0.00187 0.03503 0.01967 0.00174 0.00181 0.00059 0.00000 0.00541 0.00493 0.00727 0.00506 0.00461 0.00399 0.00252 H22A 0.05792 0.69807 0.58702 1.00000 0.04203 0.00000 0.00000 C23 0.36230 -0.45526 0.37031 1.00000 0.04359 0.01910 0.03767 0.00433 -0.00037 0.01560 0.03377 0.01830 0.00180 0.00169 0.00051 0.00000 0.00537 0.00469 0.00626 0.00427 0.00447 0.00364 0.00245 H23A 0.22263 -0.34060 0.36533 1.00000 0.04052 0.00000 0.00000 C24 0.53141 -0.42055 0.41906 1.00000 0.05982 -0.00761 0.03483 0.00279 0.00370 0.00661 0.02910 0.01694 0.00182 0.00140 0.00047 0.00000 0.00597 0.00312 0.00559 0.00330 0.00432 0.00304 0.00230 C25 0.74716 -0.57151 0.42541 1.00000 0.03501 0.03070 0.04958 -0.00842 -0.00244 0.00479 0.03890 0.01904 0.00187 0.00193 0.00058 0.00000 0.00584 0.00550 0.00749 0.00548 0.00504 0.00427 0.00269 H25A 0.87559 -0.54020 0.45782 1.00000 0.04668 0.00000 0.00000 C26 1.01729 1.07146 0.91906 1.00000 0.03464 0.01206 0.03658 -0.00422 0.00387 -0.00282 0.02775 0.01743 0.00171 0.00164 0.00052 0.00000 0.00463 0.00375 0.00541 0.00352 0.00374 0.00310 0.00208 C27 -0.35867 -0.26232 0.16554 1.00000 0.03639 0.00526 0.08082 0.00367 0.00401 0.00277 0.04096 0.01951 0.00176 0.00167 0.00062 0.00000 0.00567 0.00412 0.00908 0.00474 0.00525 0.00343 0.00296 H27A -0.50447 -0.36802 0.16119 1.00000 0.04916 0.00000 0.00000 C28 0.50981 -0.20649 0.46692 1.00000 0.04726 0.00217 0.05538 -0.00084 0.00013 0.01325 0.03530 0.01906 0.00194 0.00164 0.00058 0.00000 0.00583 0.00378 0.00760 0.00421 0.00497 0.00333 0.00269 C29 0.13509 0.91053 0.66473 1.00000 0.01246 -0.00016 0.09578 0.00284 0.01053 0.00354 0.03568 0.01885 0.00157 0.00152 0.00060 0.00000 0.00396 0.00352 0.00892 0.00412 0.00418 0.00259 0.00284 H29A -0.01319 1.01210 0.66225 1.00000 0.04282 0.00000 0.00000 C30 0.07344 0.04690 0.17616 1.00000 0.01698 0.04991 0.04412 0.00203 0.00702 0.00202 0.03674 0.01923 0.00164 0.00200 0.00054 0.00000 0.00448 0.00628 0.00705 0.00524 0.00427 0.00404 0.00255 H30A 0.22270 0.14674 0.17841 1.00000 0.04408 0.00000 0.00000 C31 0.03621 -0.15188 0.22052 1.00000 0.04781 0.04097 0.04722 0.00134 0.00787 0.00055 0.04513 0.02261 0.00216 0.00227 0.00066 0.00000 0.00679 0.00613 0.00765 0.00581 0.00566 0.00504 0.00292 H31A 0.15799 -0.18510 0.25437 1.00000 0.05415 0.00000 0.00000 C32 -0.08309 0.29127 0.08075 1.00000 0.01831 0.02745 0.04112 -0.00391 0.00060 0.00198 0.02913 0.01692 0.00159 0.00177 0.00053 0.00000 0.00456 0.00495 0.00624 0.00452 0.00396 0.00357 0.00224 C33 0.76486 -0.77394 0.38102 1.00000 0.05619 0.05391 0.02738 0.00509 0.00144 -0.00376 0.04602 0.02021 0.00210 0.00228 0.00050 0.00000 0.00636 0.00657 0.00536 0.00475 0.00459 0.00476 0.00283 H33A 0.90167 -0.89232 0.38654 1.00000 0.05522 0.00000 0.00000 C34 1.26841 1.41991 0.88159 1.00000 0.03946 0.05540 0.02988 -0.00644 0.01045 -0.01115 0.04110 0.01863 0.00190 0.00225 0.00051 0.00000 0.00592 0.00686 0.00571 0.00509 0.00453 0.00479 0.00277 H34A 1.40943 1.53284 0.88520 1.00000 0.04932 0.00000 0.00000 C35 1.24861 1.22847 0.92523 1.00000 0.03438 0.02201 0.05102 0.00399 0.00061 -0.00076 0.03606 0.01910 0.00187 0.00186 0.00056 0.00000 0.00518 0.00489 0.00740 0.00475 0.00467 0.00369 0.00261 H35A 1.37648 1.19769 0.95781 1.00000 0.04328 0.00000 0.00000 C36 0.38430 -0.65345 0.32677 1.00000 0.06361 0.04626 0.01376 0.00090 -0.00955 -0.01696 0.04215 0.01700 0.00209 0.00211 0.00045 0.00000 0.00670 0.00596 0.00441 0.00423 0.00452 0.00504 0.00273 H36A 0.25698 -0.68486 0.29409 1.00000 0.05057 0.00000 0.00000 Final Structure Factor Calculation for cfc1s in P1 Total number of l.s. parameters = 325 Maximum vector length = 511 Memory required = 3137 / 24024 wR2 = 0.2352 before cycle 5 for 2701 data and 2 / 325 parameters GooF = S = 1.412; Restrained GooF = 1.411 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0744 for 1925 Fo > 4sig(Fo) and 0.1013 for all 2701 data wR2 = 0.2352, GooF = S = 1.412, Restrained GooF = 1.411 for all data Flack x parameter = 0.3907 with esd 0.8050 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 36.00 for non-hydrogen and 20.00 for hydrogen atoms Principal mean square atomic displacements U 0.0627 0.0434 0.0225 O1 0.0533 0.0410 0.0189 O2 0.0467 0.0409 0.0262 O3 0.0628 0.0451 0.0146 O4 0.0638 0.0469 0.0033 C5 0.0455 0.0389 0.0184 C6 0.0592 0.0389 0.0208 O7 0.0880 0.0238 0.0132 C8 0.0447 0.0398 0.0323 C9 0.0514 0.0400 0.0355 O10 0.0505 0.0251 0.0105 C11 0.0506 0.0347 0.0216 C12 0.0527 0.0343 0.0309 O13 0.0490 0.0336 0.0289 C14 0.0596 0.0543 0.0191 C15 0.0632 0.0466 0.0222 C16 0.0538 0.0397 0.0040 C17 0.0500 0.0441 0.0290 O18 0.0625 0.0387 0.0108 C19 0.0526 0.0416 0.0067 C20 0.0595 0.0458 0.0091 C21 0.0537 0.0311 0.0203 C22 0.0520 0.0386 0.0107 C23 0.0607 0.0350 -0.0084 C24 ** NON POSITIVE DEFINITE ** 0.0569 0.0333 0.0265 C25 0.0374 0.0347 0.0111 C26 0.0814 0.0366 0.0049 C27 0.0595 0.0478 -0.0014 C28 ** NON POSITIVE DEFINITE ** 0.0959 0.0123 -0.0011 C29 ** NON POSITIVE DEFINITE ** 0.0507 0.0436 0.0159 C30 0.0504 0.0443 0.0407 C31 0.0429 0.0266 0.0179 C32 0.0604 0.0512 0.0264 C33 0.0629 0.0350 0.0255 C34 0.0528 0.0339 0.0214 C35 0.0778 0.0373 0.0113 C36 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.013 0.022 0.033 0.044 0.058 0.075 0.099 0.130 0.193 1.000 Number in group 276. 273. 281. 263. 265. 270. 271. 266. 269. 267. GooF 1.044 1.167 1.370 1.508 1.795 1.638 1.563 1.337 1.434 1.091 K 0.766 0.632 0.920 1.055 1.102 1.067 1.051 1.000 1.049 1.053 Resolution(A) 0.84 0.90 0.94 0.99 1.04 1.12 1.20 1.36 1.58 2.05 inf Number in group 285. 255. 284. 259. 270. 266. 279. 261. 270. 272. GooF 1.422 1.090 1.203 1.297 1.238 1.275 1.450 1.543 1.682 1.759 K 1.121 1.074 1.091 1.025 0.994 1.015 0.951 0.952 1.056 1.080 R1 0.154 0.142 0.131 0.126 0.088 0.088 0.123 0.086 0.076 0.069 Recommended weighting scheme: WGHT 0.1074 1.1207 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 1 4 -2 52.30 0.02 7.88 0.002 1.22 -2 0 1 94.99 2.00 6.46 0.018 2.71 -1 -5 2 80.99 13.87 5.90 0.047 0.99 6 1 -4 65.17 15.66 5.79 0.050 0.89 3 1 -1 29.01 3.44 5.53 0.023 1.70 -1 2 -1 142.03 57.97 5.34 0.096 2.26 3 -2 -1 62.72 10.86 5.31 0.042 1.47 2 -4 -3 455.60 161.63 4.91 0.160 1.14 3 -3 1 48.86 7.89 4.60 0.035 1.22 1 -2 -1 85.05 32.22 4.47 0.072 2.28 2 -2 -2 138.44 55.05 4.33 0.094 1.84 2 3 -1 40.94 18.21 4.32 0.054 1.43 -2 -2 2 144.04 59.19 4.29 0.097 1.84 0 -5 2 53.20 17.44 4.27 0.053 1.00 2 -4 -1 61.88 13.28 4.27 0.046 1.14 2 -3 -1 49.21 10.51 4.16 0.041 1.43 2 2 -2 115.10 59.79 4.08 0.098 1.84 1 -3 -2 130.59 56.20 4.07 0.095 1.59 1 -4 -2 69.35 4.78 4.06 0.028 1.22 3 2 -1 53.85 22.89 4.03 0.060 1.47 0 -5 0 35.57 11.42 3.89 0.043 1.01 -2 4 3 358.20 161.65 3.81 0.160 1.14 6 2 -3 47.54 21.14 3.76 0.058 0.85 5 1 -3 94.34 41.92 3.67 0.082 1.06 1 2 -1 64.40 35.34 3.61 0.075 2.28 -2 1 -1 66.07 32.06 3.60 0.071 2.34 2 -1 1 59.96 31.55 3.51 0.071 2.34 1 -3 0 337.55 173.87 3.43 0.166 1.60 0 3 0 37.06 16.77 3.43 0.052 1.68 2 -4 1 57.02 22.58 3.40 0.060 1.14 2 0 1 31.65 13.05 3.39 0.046 2.64 -2 4 1 44.20 13.55 3.32 0.046 1.14 -1 -2 1 72.31 35.44 3.22 0.075 2.28 4 -3 0 75.72 30.46 3.20 0.070 1.05 -1 3 0 342.26 173.70 3.15 0.166 1.60 4 3 -3 33.18 17.32 3.14 0.052 1.05 3 1 -2 114.64 67.64 3.11 0.104 1.70 -2 1 2 261.25 148.84 3.06 0.154 2.37 2 -5 8 18.59 38.72 2.94 0.078 0.88 2 -3 -2 17.90 4.95 2.92 0.028 1.42 -1 3 -2 52.56 23.09 2.92 0.061 1.58 5 2 -3 28.45 16.74 2.91 0.052 1.00 2 1 -2 245.36 148.68 2.90 0.154 2.37 3 0 -2 23.10 10.89 2.88 0.042 1.80 3 -3 -3 36.08 12.61 2.87 0.045 1.22 -2 -1 2 258.23 148.72 2.87 0.154 2.37 -1 3 15 10.10 26.57 2.86 0.065 1.09 2 -2 0 344.95 208.19 2.81 0.182 1.84 -1 4 4 9.20 26.69 2.79 0.065 1.20 1 -3 2 51.59 23.23 2.77 0.061 1.58 Bond lengths and angles O1 - Distance Angles C11 1.2586 (0.0119) O1 - O2 - Distance Angles C28 1.3245 (0.0117) O2 - O3 - Distance Angles C32 1.3155 (0.0108) O3 - O4 - Distance Angles C12 1.2536 (0.0131) O4 - C5 - Distance Angles C22 1.4180 (0.0137) C21 1.4365 (0.0145) 117.82 (1.08) C11 1.4595 (0.0154) 122.60 (0.97) 119.48 (0.94) C5 - C22 C21 C6 - Distance Angles C9 1.3077 (0.0147) C32 1.4533 (0.0146) 122.08 (1.04) C30 1.4574 (0.0137) 120.60 (0.99) 116.85 (0.82) C6 - C9 C32 O7 - Distance Angles C32 1.2525 (0.0126) O7 - C8 - Distance Angles C15 1.3051 (0.0146) C21 1.3922 (0.0168) 122.20 (1.18) C8 - C15 C9 - Distance Angles C6 1.3077 (0.0147) C27 1.4221 (0.0155) 121.87 (1.08) C9 - C6 O10 - Distance Angles C11 1.2906 (0.0118) O10 - C11 - Distance Angles O1 1.2586 (0.0119) O10 1.2906 (0.0118) 124.98 (1.08) C5 1.4595 (0.0155) 119.23 (0.89) 115.77 (0.95) C11 - O1 O10 C12 - Distance Angles O18 1.2578 (0.0136) O4 1.2536 (0.0129) 127.85 (1.05) C26 1.5344 (0.0138) 118.66 (0.92) 113.28 (0.97) C12 - O18 O4 O13 - Distance Angles C28 1.2110 (0.0134) O13 - C14 - Distance Angles C19 1.3583 (0.0148) C20 1.3519 (0.0152) 120.28 (1.02) C14 - C19 C15 - Distance Angles C8 1.3051 (0.0146) C29 1.4630 (0.0159) 123.18 (1.27) C15 - C8 C16 - Distance Angles C27 1.3303 (0.0160) C31 1.4162 (0.0147) 122.30 (1.13) C16 - C27 C17 - Distance Angles C33 1.2999 (0.0159) C36 1.4108 (0.0148) 119.92 (1.06) C17 - C33 O18 - Distance Angles C12 1.2578 (0.0137) O18 - C19 - Distance Angles C14 1.3583 (0.0148) C34 1.3883 (0.0148) 119.79 (0.97) C19 - C14 C20 - Distance Angles C26 1.3255 (0.0138) C14 1.3519 (0.0153) 122.59 (0.87) C20 - C26 C21 - Distance Angles C8 1.3922 (0.0168) C5 1.4365 (0.0145) 118.21 (1.03) C21 - C8 C22 - Distance Angles C29 1.3701 (0.0167) C5 1.4180 (0.0138) 123.50 (1.07) C22 - C29 C23 - Distance Angles C24 1.3370 (0.0136) C36 1.3877 (0.0158) 122.10 (0.92) C23 - C24 C24 - Distance Angles C23 1.3370 (0.0136) C25 1.3905 (0.0129) 120.55 (0.96) C28 1.5094 (0.0139) 122.74 (0.84) 116.56 (0.90) C24 - C23 C25 C25 - Distance Angles C24 1.3905 (0.0129) C33 1.4123 (0.0163) 116.32 (1.00) C25 - C24 C26 - Distance Angles C20 1.3255 (0.0137) C35 1.4775 (0.0129) 119.12 (0.87) C12 1.5344 (0.0138) 122.67 (0.85) 117.81 (0.88) C26 - C20 C35 C27 - Distance Angles C16 1.3303 (0.0160) C9 1.4221 (0.0155) 119.17 (0.94) C27 - C16 C28 - Distance Angles O13 1.2110 (0.0133) O2 1.3245 (0.0117) 122.85 (1.00) C24 1.5094 (0.0139) 124.48 (0.90) 112.62 (0.89) C28 - O13 O2 C29 - Distance Angles C22 1.3701 (0.0167) C15 1.4630 (0.0159) 114.83 (0.96) C29 - C22 C30 - Distance Angles C31 1.4172 (0.0161) C6 1.4574 (0.0137) 117.38 (0.89) C30 - C31 C31 - Distance Angles C30 1.4172 (0.0161) C16 1.4162 (0.0147) 118.40 (1.14) C31 - C30 C32 - Distance Angles O7 1.2525 (0.0126) O3 1.3155 (0.0108) 121.09 (0.95) C6 1.4533 (0.0145) 119.06 (0.84) 119.45 (0.95) C32 - O7 O3 C33 - Distance Angles C17 1.2999 (0.0159) C25 1.4123 (0.0163) 123.29 (1.11) C33 - C17 C34 - Distance Angles C35 1.3630 (0.0153) C19 1.3883 (0.0147) 121.67 (0.95) C34 - C35 C35 - Distance Angles C34 1.3630 (0.0153) C26 1.4775 (0.0128) 116.31 (0.93) C35 - C34 C36 - Distance Angles C23 1.3877 (0.0158) C17 1.4108 (0.0148) 117.32 (0.91) C36 - C23 FMAP and GRID set by program FMAP 2 3 86 GRID -1.205 -2 -2 1.205 2 2 R1 = 0.1016 for 1764 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.33 at 0.4742 0.9622 0.5022 [ 1.17 A from C28 ] Deepest hole -0.30 at 0.3148 0.6372 0.6931 [ 1.51 A from C8 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 2689 / 18399 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4742 -0.0378 0.5022 1.00000 0.05 0.33 1.17 C28 1.20 O13 1.30 O2 2.32 O1 Q2 1 0.4453 -0.4380 0.3358 1.00000 0.05 0.33 0.92 C23 1.15 C36 1.51 H23A 1.79 H36A Q3 1 -0.3073 0.3746 -0.0102 1.00000 0.05 0.32 1.07 O7 1.99 H35A 2.00 O4 2.25 C32 Q4 1 0.2800 0.1226 0.4994 1.00000 0.05 0.32 1.31 O10 1.35 O2 2.19 C11 2.23 C28 Q5 1 0.6533 -0.1585 0.5576 1.00000 0.05 0.31 1.03 O13 2.00 O1 2.05 C28 2.34 H22A Q6 1 0.3824 0.3279 0.5064 1.00000 0.05 0.31 1.01 O10 1.62 C11 2.17 O1 2.31 O2 Q7 1 0.5510 -0.1916 0.5437 1.00000 0.05 0.31 1.00 O13 1.66 C28 2.27 O1 2.28 O2 Q8 1 0.6411 0.0428 0.5454 1.00000 0.05 0.30 1.27 O1 1.30 O13 2.12 C11 2.18 C28 Q9 1 0.2172 0.3205 0.4837 1.00000 0.05 0.30 1.14 O10 2.01 H25A 2.12 O2 2.30 C11 Q10 1 0.1015 -0.1717 0.4585 1.00000 0.05 0.29 1.18 O2 2.21 C28 2.22 H25A 2.29 H33A Q11 1 0.1282 0.5508 0.0517 1.00000 0.05 0.29 0.99 O3 1.65 O18 1.89 C32 2.31 O7 Q12 1 -0.2581 -0.2350 0.1285 1.00000 0.05 0.28 0.94 C9 1.02 C27 1.61 H9A 1.71 H27A Q13 1 1.0244 0.8029 1.0392 1.00000 0.05 0.28 1.00 O18 1.58 C12 2.10 O4 2.15 O3 Q14 1 0.4499 0.2036 0.5411 1.00000 0.05 0.27 1.15 C11 1.22 O10 1.32 O1 2.32 O13 Q15 1 1.1527 0.8726 1.0610 1.00000 0.05 0.27 1.12 O18 2.14 C12 2.26 H9A 2.27 O3 Q16 1 0.6598 -0.1187 0.4640 1.00000 0.05 0.27 0.93 C28 1.03 O13 1.90 C24 1.96 O2 Q17 1 0.9430 0.6849 0.9983 1.00000 0.05 0.27 1.13 C12 1.17 O4 1.36 O18 2.25 O7 Q18 1 -0.1286 0.2973 0.0051 1.00000 0.05 0.27 1.02 O7 1.63 C32 2.26 O3 2.39 C26 Q19 1 0.7115 0.7396 0.9148 1.00000 0.05 0.27 0.98 O4 1.69 H20A 1.87 C12 1.99 H34A Q20 1 0.7942 0.3256 0.5920 1.00000 0.05 0.27 1.08 O1 1.97 C11 2.19 H21A 2.36 H29A Shortest distances between peaks (including symmetry equivalents) 5 7 0.63 13 15 0.87 6 9 0.98 6 14 1.02 5 8 1.05 3 18 1.06 4 9 1.10 13 17 1.12 4 6 1.18 1 7 1.23 7 8 1.28 4 14 1.29 1 8 1.30 8 14 1.31 1 4 1.32 11 13 1.40 1 16 1.43 1 14 1.49 1 5 1.59 11 17 1.60 11 15 1.64 9 14 1.78 8 20 1.89 1 6 1.91 7 16 1.92 15 17 1.93 4 10 1.94 8 16 1.96 17 18 2.00 5 16 2.04 7 14 2.07 3 17 2.07 11 18 2.07 17 19 2.11 6 8 2.12 4 8 2.14 5 14 2.14 14 20 2.16 1 10 2.25 1 9 2.29 4 7 2.30 10 16 2.42 3 19 2.46 4 16 2.58 12 13 2.59 9 10 2.60 5 20 2.64 14 16 2.67 4 5 2.68 6 7 2.68 13 18 2.71 3 11 2.74 6 20 2.75 15 18 2.83 12 15 2.84 8 9 2.90 7 10 2.90 6 16 2.91 7 20 2.91 3 13 2.94 Time profile in seconds ----------------------- 0.00: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.02: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.05: Structure factors and derivatives 0.50: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.12: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.02: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.00: Fourier summations 0.02: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + cfc1s finished at 11:38:49 Total CPU time: 0.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++