+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2005src0300 started at 12:58:18 on 02-Apr-2005 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2005src0300 in P-1 CELL 0.71073 12.2768 12.3338 14.6278 84.969 71.244 73.580 ZERR 2.00 0.0022 0.0020 0.0025 0.012 0.013 0.014 LATT 1 SFAC C H LI B O F AL P UNIT 76 66 2 2 4 30 2 2 V = 2011.76 F(000) = 896.0 Mu = 0.19 mm-1 Cell Wt = 1764.69 Rho = 1.457 MERG 2 OMIT -3.00 55.00 OMIT -3 1 1 OMIT 2 -2 5 OMIT 2 4 0 OMIT -3 -1 3 OMIT 1 1 2 OMIT -2 -4 8 OMIT 1 7 9 OMIT -3 1 0 OMIT 3 1 2 OMIT -3 3 0 OMIT 2 0 3 OMIT 3 1 1 OMIT -3 0 3 OMIT 3 0 0 OMIT 2 8 11 OMIT -1 -5 2 OMIT 3 0 1 OMIT 2 1 3 OMIT -1 1 2 OMIT 2 -9 3 OMIT -3 3 6 OMIT -4 3 3 OMIT 3 2 1 OMIT 1 3 3 OMIT -1 2 1 OMIT -2 3 3 EXTI 0.09165 FMAP 2 PLAN 10 SIZE 0.20 0.20 0.50 ACTA BOND WGHT 0.07610 0.77890 L.S. 4 TEMP -153.00 FVAR 1.01950 H2B 2 0.383167 0.784115 0.353867 11.00000 0.03900 H3B 2 0.434009 0.778154 0.219515 11.00000 0.03583 H1B 2 0.453715 0.648632 0.289438 11.00000 0.05393 MOLE 1 C1 1 0.611530 0.893656 0.281887 11.00000 0.02154 0.02877 = 0.03145 -0.00075 -0.00783 -0.00543 C2 1 0.604726 0.953721 0.360951 11.00000 0.04522 0.03355 = 0.03466 0.00101 -0.01854 -0.01177 AFIX 43 H2 2 0.596045 0.917916 0.422100 11.00000 -1.20000 AFIX 0 C3 1 0.610501 1.065671 0.351390 11.00000 0.05450 0.03658 = 0.04966 -0.00479 -0.02403 -0.01452 AFIX 43 H3 2 0.605209 1.105644 0.405979 11.00000 -1.20000 AFIX 0 C4 1 0.623926 1.118697 0.262554 11.00000 0.04158 0.02982 = 0.05426 0.00155 -0.01393 -0.01217 AFIX 43 H4 2 0.630054 1.194252 0.255611 11.00000 -1.20000 AFIX 0 C5 1 0.628355 1.060824 0.183907 11.00000 0.03616 0.03467 = 0.03859 0.00437 -0.00603 -0.00725 AFIX 43 H5 2 0.635856 1.097469 0.123174 11.00000 -1.20000 AFIX 0 C6 1 0.621912 0.949633 0.193197 11.00000 0.03099 0.03274 = 0.03005 -0.00147 -0.00645 -0.00442 AFIX 43 H6 2 0.624574 0.911048 0.138762 11.00000 -1.20000 AFIX 0 C7 1 0.628424 0.695535 0.404822 11.00000 0.02982 0.02663 = 0.02736 -0.00073 -0.00823 -0.00617 C8 1 0.541134 0.658004 0.475884 11.00000 0.03458 0.04165 = 0.03789 0.00654 -0.01068 -0.01358 AFIX 43 H8 2 0.468987 0.658816 0.464454 11.00000 -1.20000 AFIX 0 C9 1 0.558360 0.619004 0.564147 11.00000 0.04501 0.05889 = 0.03725 0.01506 -0.00633 -0.02292 AFIX 43 H9 2 0.498205 0.592996 0.612166 11.00000 -1.20000 AFIX 0 C10 1 0.662437 0.618138 0.581796 11.00000 0.05338 0.05237 = 0.03094 0.01130 -0.01517 -0.01572 AFIX 43 H10 2 0.672990 0.593659 0.642546 11.00000 -1.20000 AFIX 0 C11 1 0.751709 0.653127 0.510560 11.00000 0.04038 0.04644 = 0.03666 0.00498 -0.01904 -0.01255 AFIX 43 H11 2 0.824226 0.650885 0.522004 11.00000 -1.20000 AFIX 0 C12 1 0.735072 0.691419 0.422550 11.00000 0.02987 0.03829 = 0.02884 0.00167 -0.00847 -0.01017 AFIX 43 H12 2 0.796554 0.715019 0.373965 11.00000 -1.20000 AFIX 0 C13 1 0.698280 0.575719 0.072025 11.00000 0.02194 0.03311 = 0.03032 -0.00456 -0.00756 -0.00819 C14 1 0.718236 0.462748 0.051522 11.00000 0.02252 0.03264 = 0.03708 -0.00429 -0.00906 -0.00470 C15 1 0.684697 0.426397 -0.019964 11.00000 0.02839 0.03538 = 0.04234 -0.01351 -0.00702 -0.00790 C16 1 0.627548 0.505071 -0.073892 11.00000 0.02921 0.04723 = 0.03292 -0.01073 -0.00951 -0.01252 C17 1 0.602803 0.618883 -0.054997 11.00000 0.02762 0.04277 = 0.03076 -0.00111 -0.01057 -0.00980 C18 1 0.637773 0.650656 0.016956 11.00000 0.02486 0.03186 = 0.03098 -0.00349 -0.00805 -0.00838 C19 1 0.873651 0.729373 0.078259 11.00000 0.02181 0.02551 = 0.02882 -0.00015 -0.00789 -0.00437 C20 1 0.911042 0.737645 -0.021484 11.00000 0.02511 0.02780 = 0.02902 -0.00341 -0.00886 -0.00358 C21 1 0.992344 0.796460 -0.073046 11.00000 0.03074 0.03157 = 0.02549 0.00146 -0.00520 -0.00417 C22 1 1.041219 0.850021 -0.024369 11.00000 0.02896 0.02889 = 0.03859 0.00555 -0.00720 -0.00934 C23 1 1.007028 0.845590 0.075141 11.00000 0.03126 0.03163 = 0.03716 0.00130 -0.01348 -0.01142 C24 1 0.925015 0.786765 0.122994 11.00000 0.02647 0.03092 = 0.02679 0.00195 -0.00963 -0.00682 C25 1 0.857534 0.513123 0.227883 11.00000 0.02621 0.02840 = 0.02807 -0.00230 -0.00826 -0.00575 C26 1 0.976027 0.491965 0.224935 11.00000 0.02819 0.02754 = 0.02917 -0.00190 -0.00960 -0.00614 C27 1 1.027557 0.411643 0.282268 11.00000 0.03092 0.03225 = 0.03508 -0.00476 -0.01533 -0.00247 C28 1 0.959470 0.349187 0.345929 11.00000 0.04555 0.03028 = 0.03179 0.00226 -0.01635 -0.00251 C29 1 0.840987 0.366025 0.351848 11.00000 0.04105 0.02955 = 0.02999 0.00180 -0.00475 -0.00919 C30 1 0.794872 0.446604 0.292564 11.00000 0.02704 0.03132 = 0.03134 -0.00178 -0.00657 -0.00641 C31 1 1.159289 0.720875 0.286757 11.00000 0.03657 0.05155 = 0.05170 -0.01746 -0.01495 -0.00666 AFIX 23 H31A 2 1.106876 0.717454 0.248498 11.00000 -1.20000 H31B 2 1.243087 0.692347 0.245456 11.00000 -1.20000 AFIX 0 C32 1 1.137161 0.646576 0.370733 11.00000 0.07821 0.04571 = 0.07535 -0.00181 -0.02411 -0.00963 AFIX 137 H32A 2 1.187630 0.650419 0.409739 11.00000 -1.50000 H32B 2 1.156131 0.568651 0.348800 11.00000 -1.50000 H32C 2 1.052935 0.671015 0.409770 11.00000 -1.50000 AFIX 0 C33 1 1.016746 0.892290 0.362027 11.00000 0.03466 0.04919 = 0.04648 -0.00582 -0.00813 -0.00694 AFIX 23 H33A 2 0.997441 0.869093 0.430630 11.00000 -1.20000 H33B 2 0.964564 0.868488 0.332994 11.00000 -1.20000 AFIX 0 C34 1 0.996428 1.015438 0.355048 11.00000 0.05308 0.04752 = 0.05692 -0.00166 -0.00594 -0.01100 AFIX 137 H34A 2 1.038552 1.039687 0.392731 11.00000 -1.50000 H34B 2 0.910658 1.052197 0.380443 11.00000 -1.50000 H34C 2 1.026507 1.036648 0.287312 11.00000 -1.50000 AFIX 0 C35 1 1.308378 1.082078 0.164742 11.00000 0.05277 0.04636 = 0.04559 0.01612 -0.02454 -0.01948 AFIX 23 H35A 2 1.385646 1.101509 0.140829 11.00000 -1.20000 H35B 2 1.243548 1.152393 0.168097 11.00000 -1.20000 AFIX 0 C36 1 1.304666 1.000271 0.097428 11.00000 0.06959 0.06300 = 0.03650 0.01044 -0.02117 -0.02654 AFIX 137 H36A 2 1.372545 0.933169 0.090584 11.00000 -1.50000 H36B 2 1.309087 1.035732 0.034178 11.00000 -1.50000 H36C 2 1.229922 0.978090 0.123235 11.00000 -1.50000 AFIX 0 C37 1 1.299623 1.105758 0.327114 11.00000 0.03960 0.03596 = 0.05323 -0.00934 -0.01923 -0.00452 AFIX 23 H37A 2 1.238755 1.179016 0.330342 11.00000 -1.20000 H37B 2 1.379291 1.120314 0.306753 11.00000 -1.20000 AFIX 0 C38 1 1.277056 1.050468 0.424733 11.00000 0.05000 0.06475 = 0.04046 -0.01655 -0.01451 -0.01119 AFIX 137 H38A 2 1.199228 1.034029 0.443568 11.00000 -1.50000 H38B 2 1.277362 1.101460 0.472343 11.00000 -1.50000 H38C 2 1.339875 0.979893 0.421891 11.00000 -1.50000 AFIX 0 LI1 3 1.280941 0.883461 0.285591 11.00000 0.03099 0.03859 = 0.04183 0.00383 -0.01019 -0.01004 B1 4 0.449580 0.737025 0.289970 11.00000 0.02496 0.03429 = 0.03757 -0.00087 -0.01102 -0.00701 O1 5 1.138023 0.840511 0.312455 11.00000 0.03275 0.05097 = 0.03959 -0.00008 -0.01139 -0.01656 O2 5 1.294223 1.032820 0.258700 11.00000 0.03493 0.03378 = 0.03422 0.00146 -0.01270 -0.01051 F1 6 0.775804 0.380630 0.100528 11.00000 0.04151 0.03074 = 0.05696 -0.00613 -0.02510 -0.00002 F2 6 0.708061 0.315054 -0.037382 11.00000 0.04972 0.03638 = 0.06273 -0.01925 -0.02036 -0.00715 F3 6 0.595176 0.471766 -0.143960 11.00000 0.04588 0.06081 = 0.04328 -0.01863 -0.01901 -0.01412 F4 6 0.546433 0.696081 -0.107568 11.00000 0.05136 0.05059 = 0.04110 0.00383 -0.02845 -0.01289 F5 6 0.614527 0.763911 0.030592 11.00000 0.03943 0.03053 = 0.03819 0.00030 -0.01784 -0.00931 F6 6 0.869114 0.685065 -0.075359 11.00000 0.03793 0.04470 = 0.02767 -0.00540 -0.00935 -0.01404 F7 6 1.025866 0.799477 -0.170047 11.00000 0.04857 0.04958 = 0.02511 0.00292 -0.00201 -0.01698 F8 6 1.122267 0.904860 -0.072448 11.00000 0.04282 0.04456 = 0.04683 0.00869 -0.00566 -0.02377 F9 6 1.053919 0.898560 0.123698 11.00000 0.04791 0.05017 = 0.04728 0.00334 -0.02098 -0.02902 F10 6 0.895297 0.783838 0.221017 11.00000 0.03599 0.04886 = 0.02621 0.00085 -0.01147 -0.01896 F11 6 1.048286 0.549567 0.163941 11.00000 0.02478 0.03510 = 0.04612 0.00532 -0.01107 -0.00889 F12 6 1.143854 0.391986 0.274856 11.00000 0.03191 0.04200 = 0.05739 0.00159 -0.02559 -0.00225 F13 6 1.009160 0.269671 0.400940 11.00000 0.06005 0.04390 = 0.04496 0.01266 -0.02506 -0.00155 F14 6 0.775375 0.304145 0.412921 11.00000 0.05240 0.04358 = 0.04592 0.01478 -0.00418 -0.01454 F15 6 0.678792 0.461400 0.299621 11.00000 0.02645 0.04063 = 0.04921 0.00324 -0.00734 -0.01128 AL2 7 0.768434 0.634474 0.157441 11.00000 0.02122 0.02714 = 0.02653 -0.00040 -0.00875 -0.00642 P1 8 0.605891 0.746290 0.288839 11.00000 0.02420 0.02763 = 0.02741 -0.00003 -0.00938 -0.00744 HKLF 4 Covalent radii and connectivity table for 2005src0300 in P-1 C 0.770 H 0.320 LI 1.520 B 0.820 O 0.660 F 0.640 AL 1.250 P 1.100 C1 - C2 C6 P1 C2 - C3 C1 C3 - C4 C2 C4 - C3 C5 C5 - C4 C6 C6 - C5 C1 C7 - C8 C12 P1 C8 - C7 C9 C9 - C10 C8 C10 - C9 C11 C11 - C10 C12 C12 - C11 C7 C13 - C18 C14 Al2 C14 - F1 C13 C15 C15 - F2 C16 C14 C16 - F3 C15 C17 C17 - F4 C18 C16 C18 - F5 C17 C13 C19 - C20 C24 Al2 C20 - F6 C19 C21 C21 - F7 C22 C20 C22 - F8 C21 C23 C23 - F9 C24 C22 C24 - F10 C23 C19 C25 - C30 C26 Al2 C26 - F11 C27 C25 C27 - F12 C28 C26 C28 - F13 C27 C29 C29 - F14 C30 C28 C30 - F15 C29 C25 C31 - C32 O1 C32 - C31 C33 - O1 C34 C34 - C33 C35 - O2 C36 C36 - C35 C37 - O2 C38 C38 - C37 Li1 - O1 O2 B1_$2 B1 - P1 Li1_$1 O1 - C33 C31 Li1 O2 - C35 C37 Li1 F1 - C14 F2 - C15 F3 - C16 F4 - C17 F5 - C18 F6 - C20 F7 - C21 F8 - C22 F9 - C23 F10 - C24 F11 - C26 F12 - C27 F13 - C28 F14 - C29 F15 - C30 Al2 - C25 C13 C19 P1 P1 - C1 C7 B1 Al2 Operators for generating equivalent atoms: $1 x-1, y, z $2 x+1, y, z 41305 Reflections read, of which 109 rejected -15 =< h =< 15, -15 =< k =< 16, -19 =< l =< 18, Max. 2-theta = 55.00 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -9 -9 4 26.79 2.16 2 17.58 1 Inconsistent equivalents 9117 Unique reflections, of which 0 suppressed R(int) = 0.0603 R(sigma) = 0.0479 Friedel opposites merged Maximum memory for data reduction = 4339 / 91676 Default effective X-H distances for T = -153.0 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. Least-squares cycle 1 Maximum vector length = 511 Memory required = 5716 / 740234 wR2 = 0.1502 before cycle 1 for 9117 data and 549 / 549 parameters GooF = S = 1.130; Restrained GooF = 1.130 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0761 * P )^2 + 0.78 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.01926 0.00249 -0.095 OSF 2 0.09140 0.00511 -0.048 EXTI Mean shift/esd = 0.027 Maximum = 0.129 for U11 C33 Max. shift = 0.001 A for H2B Max. dU = 0.000 for H3B Least-squares cycle 2 Maximum vector length = 511 Memory required = 5716 / 740234 wR2 = 0.1501 before cycle 2 for 9117 data and 549 / 549 parameters GooF = S = 1.130; Restrained GooF = 1.130 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0761 * P )^2 + 0.78 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.01931 0.00249 0.017 OSF 2 0.09139 0.00511 -0.002 EXTI Mean shift/esd = 0.010 Maximum = 0.060 for U11 C33 Max. shift = 0.001 A for H34A Max. dU = 0.000 for H2B Least-squares cycle 3 Maximum vector length = 511 Memory required = 5716 / 740234 wR2 = 0.1501 before cycle 3 for 9117 data and 549 / 549 parameters GooF = S = 1.130; Restrained GooF = 1.130 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0761 * P )^2 + 0.78 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.01933 0.00249 0.008 OSF 2 0.09140 0.00510 0.000 EXTI Mean shift/esd = 0.001 Maximum = 0.012 for tors H34A Max. shift = 0.000 A for H34A Max. dU = 0.000 for H1B Least-squares cycle 4 Maximum vector length = 511 Memory required = 5716 / 740234 wR2 = 0.1501 before cycle 4 for 9117 data and 549 / 549 parameters GooF = S = 1.130; Restrained GooF = 1.130 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0761 * P )^2 + 0.78 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.01932 0.00249 -0.001 OSF 2 0.09139 0.00511 -0.001 EXTI Mean shift/esd = 0.000 Maximum = 0.006 for tors H34A Max. shift = 0.000 A for H34C Max. dU = 0.000 for H1B Largest correlation matrix elements 0.668 EXTI / OSF -0.535 U13 F12 / U33 F12 -0.506 U13 C35 / U33 C35 -0.548 U13 F4 / U33 F4 -0.526 U13 F4 / U11 F4 -0.503 U13 F1 / U33 F1 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.5960 0.9179 0.4221 43 0.950 0.000 C2 C3 C1 H3 0.6052 1.1056 0.4060 43 0.950 0.000 C3 C4 C2 H4 0.6301 1.1942 0.2556 43 0.950 0.000 C4 C3 C5 H5 0.6358 1.0975 0.1232 43 0.950 0.000 C5 C4 C6 H6 0.6246 0.9110 0.1388 43 0.950 0.000 C6 C5 C1 H8 0.4690 0.6589 0.4645 43 0.950 0.000 C8 C7 C9 H9 0.4982 0.5930 0.6121 43 0.950 0.000 C9 C10 C8 H10 0.6730 0.5936 0.6425 43 0.950 0.000 C10 C9 C11 H11 0.8242 0.6509 0.5220 43 0.950 0.000 C11 C10 C12 H12 0.7965 0.7151 0.3740 43 0.950 0.000 C12 C11 C7 H31A 1.1069 0.7174 0.2485 23 0.990 0.000 C31 C32 O1 H31B 1.2431 0.6923 0.2455 23 0.990 0.000 C31 C32 O1 H32A 1.1877 0.6504 0.4097 137 0.980 0.000 C32 C31 H32A H32B 1.1561 0.5687 0.3488 137 0.980 0.000 C32 C31 H32A H32C 1.0530 0.6711 0.4098 137 0.980 0.000 C32 C31 H32A H33A 0.9974 0.8691 0.4306 23 0.990 0.000 C33 O1 C34 H33B 0.9646 0.8685 0.3330 23 0.990 0.000 C33 O1 C34 H34A 1.0387 1.0397 0.3926 137 0.980 0.000 C34 C33 H34A H34B 0.9107 1.0522 0.3805 137 0.980 0.000 C34 C33 H34A H34C 1.0264 1.0367 0.2873 137 0.980 0.000 C34 C33 H34A H35A 1.3857 1.1015 0.1408 23 0.990 0.000 C35 O2 C36 H35B 1.2436 1.1524 0.1681 23 0.990 0.000 C35 O2 C36 H36A 1.3725 0.9332 0.0906 137 0.980 0.000 C36 C35 H36A H36B 1.3091 1.0357 0.0342 137 0.980 0.000 C36 C35 H36A H36C 1.2299 0.9781 0.1232 137 0.980 0.000 C36 C35 H36A H37A 1.2387 1.1790 0.3304 23 0.990 0.000 C37 O2 C38 H37B 1.3793 1.1203 0.3068 23 0.990 0.000 C37 O2 C38 H38A 1.1992 1.0341 0.4436 137 0.980 0.000 C38 C37 H38A H38B 1.2775 1.1014 0.4723 137 0.980 0.000 C38 C37 H38A H38C 1.3398 0.9799 0.4219 137 0.980 0.000 C38 C37 H38A 2005src0300 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq H2B 0.38316 0.78403 0.35393 1.00000 0.03882 0.03711 0.00225 0.00215 0.00184 0.00000 0.00642 H3B 0.43392 0.77813 0.21953 1.00000 0.03567 0.03536 0.00216 0.00204 0.00175 0.00000 0.00617 H1B 0.45381 0.64867 0.28941 1.00000 0.05399 0.04340 0.00260 0.00253 0.00207 0.00000 0.00790 C1 0.61152 0.89366 0.28189 1.00000 0.02153 0.02882 0.03142 -0.00080 -0.00784 -0.00544 0.02759 0.00285 0.00016 0.00016 0.00014 0.00000 0.00084 0.00092 0.00093 0.00072 0.00071 0.00070 0.00039 C2 0.60472 0.95373 0.36094 1.00000 0.04531 0.03361 0.03460 0.00102 -0.01854 -0.01179 0.03613 0.00308 0.00021 0.00018 0.00016 0.00000 0.00120 0.00105 0.00105 0.00082 0.00092 0.00090 0.00046 H2 0.59604 0.91793 0.42209 1.00000 0.04336 0.00000 0.00000 C3 0.61051 1.06567 0.35138 1.00000 0.05450 0.03658 0.04964 -0.00479 -0.02407 -0.01447 0.04416 0.00337 0.00024 0.00020 0.00018 0.00000 0.00142 0.00117 0.00133 0.00098 0.00112 0.00104 0.00054 H3 0.60521 1.10565 0.40596 1.00000 0.05299 0.00000 0.00000 C4 0.62394 1.11868 0.26255 1.00000 0.04147 0.02977 0.05435 0.00150 -0.01389 -0.01207 0.04166 0.00355 0.00021 0.00019 0.00018 0.00000 0.00121 0.00106 0.00136 0.00094 0.00103 0.00091 0.00051 H4 0.63009 1.19423 0.25560 1.00000 0.05000 0.00000 0.00000 C5 0.62834 1.06082 0.18392 1.00000 0.03616 0.03463 0.03859 0.00434 -0.00599 -0.00724 0.03863 0.00357 0.00020 0.00019 0.00017 0.00000 0.00111 0.00110 0.00111 0.00086 0.00089 0.00088 0.00049 H5 0.63581 1.09747 0.12319 1.00000 0.04635 0.00000 0.00000 C6 0.62192 0.94962 0.19321 1.00000 0.03095 0.03278 0.03002 -0.00148 -0.00643 -0.00443 0.03280 0.00322 0.00018 0.00018 0.00015 0.00000 0.00099 0.00101 0.00096 0.00077 0.00078 0.00080 0.00043 H6 0.62461 0.91103 0.13877 1.00000 0.03936 0.00000 0.00000 C7 0.62842 0.69553 0.40483 1.00000 0.02987 0.02663 0.02741 -0.00073 -0.00826 -0.00620 0.02838 0.00286 0.00017 0.00016 0.00014 0.00000 0.00095 0.00090 0.00089 0.00071 0.00075 0.00074 0.00039 C8 0.54115 0.65802 0.47588 1.00000 0.03457 0.04171 0.03788 0.00654 -0.01067 -0.01357 0.03790 0.00347 0.00020 0.00019 0.00016 0.00000 0.00108 0.00117 0.00111 0.00089 0.00088 0.00091 0.00048 H8 0.46899 0.65885 0.46446 1.00000 0.04548 0.00000 0.00000 C9 0.55837 0.61899 0.56414 1.00000 0.04502 0.05878 0.03729 0.01504 -0.00632 -0.02288 0.04768 0.00407 0.00023 0.00023 0.00017 0.00000 0.00132 0.00150 0.00118 0.00106 0.00099 0.00114 0.00059 H9 0.49822 0.59298 0.61215 1.00000 0.05722 0.00000 0.00000 C10 0.66243 0.61812 0.58179 1.00000 0.05337 0.05233 0.03096 0.01130 -0.01519 -0.01573 0.04543 0.00386 0.00024 0.00022 0.00017 0.00000 0.00141 0.00139 0.00108 0.00096 0.00100 0.00113 0.00056 H10 0.67298 0.59362 0.64254 1.00000 0.05452 0.00000 0.00000 C11 0.75170 0.65313 0.51056 1.00000 0.04042 0.04634 0.03667 0.00494 -0.01907 -0.01254 0.03951 0.00338 0.00021 0.00020 0.00016 0.00000 0.00117 0.00125 0.00110 0.00091 0.00093 0.00097 0.00049 H11 0.82422 0.65089 0.52201 1.00000 0.04741 0.00000 0.00000 C12 0.73506 0.69144 0.42256 1.00000 0.02982 0.03829 0.02881 0.00165 -0.00841 -0.01013 0.03237 0.00308 0.00018 0.00018 0.00014 0.00000 0.00097 0.00107 0.00095 0.00078 0.00077 0.00082 0.00042 H12 0.79653 0.71506 0.37398 1.00000 0.03885 0.00000 0.00000 C13 0.69827 0.57572 0.07203 1.00000 0.02181 0.03319 0.03034 -0.00454 -0.00750 -0.00817 0.02813 0.00275 0.00016 0.00017 0.00014 0.00000 0.00085 0.00099 0.00093 0.00074 0.00072 0.00074 0.00039 C14 0.71824 0.46276 0.05150 1.00000 0.02249 0.03270 0.03708 -0.00424 -0.00907 -0.00471 0.03111 0.00297 0.00017 0.00017 0.00015 0.00000 0.00088 0.00101 0.00103 0.00079 0.00077 0.00076 0.00042 C15 0.68470 0.42642 -0.01997 1.00000 0.02839 0.03536 0.04231 -0.01351 -0.00697 -0.00787 0.03563 0.00304 0.00018 0.00018 0.00016 0.00000 0.00097 0.00107 0.00113 0.00087 0.00084 0.00082 0.00046 C16 0.62756 0.50507 -0.07388 1.00000 0.02919 0.04723 0.03291 -0.01074 -0.00949 -0.01254 0.03530 0.00294 0.00018 0.00020 0.00015 0.00000 0.00099 0.00122 0.00102 0.00087 0.00081 0.00089 0.00046 C17 0.60280 0.61888 -0.05499 1.00000 0.02757 0.04283 0.03075 -0.00110 -0.01056 -0.00981 0.03320 0.00304 0.00018 0.00019 0.00015 0.00000 0.00095 0.00115 0.00098 0.00083 0.00079 0.00084 0.00044 C18 0.63779 0.65065 0.01695 1.00000 0.02481 0.03183 0.03095 -0.00348 -0.00796 -0.00835 0.02899 0.00284 0.00017 0.00017 0.00014 0.00000 0.00089 0.00098 0.00094 0.00075 0.00074 0.00075 0.00040 C19 0.87366 0.72938 0.07825 1.00000 0.02178 0.02549 0.02883 -0.00014 -0.00791 -0.00430 0.02578 0.00275 0.00016 0.00015 0.00013 0.00000 0.00084 0.00088 0.00090 0.00069 0.00070 0.00069 0.00038 C20 0.91104 0.73766 -0.02148 1.00000 0.02507 0.02782 0.02904 -0.00339 -0.00887 -0.00359 0.02773 0.00282 0.00017 0.00016 0.00014 0.00000 0.00088 0.00092 0.00091 0.00071 0.00072 0.00072 0.00039 C21 0.99233 0.79647 -0.07302 1.00000 0.03074 0.03162 0.02546 0.00146 -0.00521 -0.00412 0.03116 0.00313 0.00018 0.00017 0.00014 0.00000 0.00097 0.00099 0.00090 0.00074 0.00074 0.00078 0.00042 C22 1.04121 0.85002 -0.02437 1.00000 0.02892 0.02884 0.03862 0.00557 -0.00719 -0.00929 0.03298 0.00321 0.00018 0.00017 0.00015 0.00000 0.00098 0.00098 0.00107 0.00080 0.00082 0.00079 0.00044 C23 1.00702 0.84558 0.07514 1.00000 0.03119 0.03161 0.03719 0.00125 -0.01346 -0.01139 0.03207 0.00295 0.00018 0.00017 0.00015 0.00000 0.00099 0.00100 0.00105 0.00080 0.00083 0.00081 0.00042 C24 0.92502 0.78677 0.12298 1.00000 0.02647 0.03086 0.02671 0.00194 -0.00961 -0.00672 0.02802 0.00285 0.00017 0.00016 0.00014 0.00000 0.00091 0.00095 0.00089 0.00072 0.00073 0.00075 0.00039 C25 0.85752 0.51311 0.22790 1.00000 0.02625 0.02837 0.02808 -0.00237 -0.00823 -0.00574 0.02781 0.00280 0.00017 0.00016 0.00014 0.00000 0.00091 0.00092 0.00090 0.00071 0.00072 0.00073 0.00039 C26 0.97601 0.49197 0.22494 1.00000 0.02822 0.02749 0.02916 -0.00195 -0.00958 -0.00613 0.02829 0.00281 0.00017 0.00016 0.00014 0.00000 0.00092 0.00092 0.00091 0.00072 0.00074 0.00074 0.00039 C27 1.02756 0.41163 0.28228 1.00000 0.03082 0.03234 0.03501 -0.00480 -0.01526 -0.00245 0.03246 0.00297 0.00018 0.00018 0.00015 0.00000 0.00099 0.00101 0.00102 0.00080 0.00082 0.00080 0.00043 C28 0.95945 0.34920 0.34592 1.00000 0.04560 0.03023 0.03179 0.00224 -0.01639 -0.00249 0.03660 0.00332 0.00021 0.00018 0.00015 0.00000 0.00122 0.00102 0.00101 0.00080 0.00090 0.00089 0.00047 C29 0.84099 0.36603 0.35185 1.00000 0.04107 0.02949 0.03000 0.00181 -0.00473 -0.00923 0.03526 0.00331 0.00020 0.00017 0.00015 0.00000 0.00115 0.00099 0.00098 0.00078 0.00084 0.00086 0.00046 C30 0.79489 0.44662 0.29255 1.00000 0.02699 0.03131 0.03136 -0.00182 -0.00657 -0.00637 0.03070 0.00302 0.00018 0.00017 0.00014 0.00000 0.00093 0.00098 0.00096 0.00076 0.00076 0.00076 0.00041 C31 1.15931 0.72086 0.28676 1.00000 0.03663 0.05146 0.05176 -0.01759 -0.01502 -0.00657 0.04630 0.00348 0.00022 0.00022 0.00019 0.00000 0.00118 0.00140 0.00137 0.00110 0.00103 0.00103 0.00057 H31A 1.10692 0.71742 0.24849 1.00000 0.05555 0.00000 0.00000 H31B 1.24312 0.69234 0.24547 1.00000 0.05555 0.00000 0.00000 C32 1.13718 0.64658 0.37072 1.00000 0.07824 0.04578 0.07532 -0.00190 -0.02406 -0.00964 0.06778 0.00519 0.00033 0.00026 0.00025 0.00000 0.00216 0.00152 0.00205 0.00140 0.00170 0.00145 0.00084 H32A 1.18768 0.65039 0.40971 1.00000 0.10167 0.00000 0.00000 H32B 1.15610 0.56866 0.34879 1.00000 0.10167 0.00000 0.00000 H32C 1.05296 0.67105 0.40977 1.00000 0.10167 0.00000 0.00000 C33 1.01675 0.89230 0.36201 1.00000 0.03489 0.04919 0.04659 -0.00586 -0.00820 -0.00691 0.04522 0.00389 0.00021 0.00022 0.00019 0.00000 0.00116 0.00135 0.00129 0.00104 0.00098 0.00100 0.00055 H33A 0.99743 0.86910 0.43061 1.00000 0.05427 0.00000 0.00000 H33B 0.96457 0.86851 0.33297 1.00000 0.05427 0.00000 0.00000 C34 0.99644 1.01543 0.35504 1.00000 0.05319 0.04759 0.05689 -0.00165 -0.00597 -0.01101 0.05575 0.00462 0.00027 0.00023 0.00022 0.00000 0.00154 0.00144 0.00157 0.00118 0.00123 0.00119 0.00067 H34A 1.03868 1.03966 0.39264 1.00000 0.08363 0.00000 0.00000 H34B 0.91069 1.05220 0.38054 1.00000 0.08363 0.00000 0.00000 H34C 1.02640 1.03666 0.28730 1.00000 0.08363 0.00000 0.00000 C35 1.30838 1.08206 0.16473 1.00000 0.05265 0.04636 0.04559 0.01611 -0.02451 -0.01938 0.04563 0.00376 0.00024 0.00022 0.00018 0.00000 0.00141 0.00132 0.00128 0.00103 0.00110 0.00111 0.00056 H35A 1.38565 1.10149 0.14081 1.00000 0.05476 0.00000 0.00000 H35B 1.24355 1.15238 0.16807 1.00000 0.05476 0.00000 0.00000 C36 1.30467 1.00027 0.09743 1.00000 0.06954 0.06304 0.03643 0.01040 -0.02113 -0.02641 0.05400 0.00408 0.00028 0.00026 0.00018 0.00000 0.00179 0.00166 0.00123 0.00112 0.00120 0.00139 0.00066 H36A 1.37254 0.93316 0.09060 1.00000 0.08099 0.00000 0.00000 H36B 1.30911 1.03572 0.03418 1.00000 0.08099 0.00000 0.00000 H36C 1.22992 0.97810 0.12323 1.00000 0.08099 0.00000 0.00000 C37 1.29961 1.10576 0.32712 1.00000 0.03961 0.03597 0.05321 -0.00939 -0.01925 -0.00450 0.04234 0.00336 0.00022 0.00020 0.00018 0.00000 0.00118 0.00115 0.00136 0.00099 0.00104 0.00094 0.00053 H37A 1.23874 1.17901 0.33035 1.00000 0.05080 0.00000 0.00000 H37B 1.37927 1.12032 0.30676 1.00000 0.05080 0.00000 0.00000 C38 1.27705 1.05049 0.42473 1.00000 0.04998 0.06483 0.04047 -0.01654 -0.01454 -0.01121 0.05148 0.00381 0.00025 0.00025 0.00018 0.00000 0.00143 0.00165 0.00126 0.00114 0.00108 0.00123 0.00063 H38A 1.19918 1.03414 0.44361 1.00000 0.07722 0.00000 0.00000 H38B 1.27747 1.10145 0.47232 1.00000 0.07722 0.00000 0.00000 H38C 1.33981 0.97986 0.42187 1.00000 0.07722 0.00000 0.00000 Li1 1.28094 0.88347 0.28559 1.00000 0.03097 0.03858 0.04187 0.00371 -0.01027 -0.00999 0.03750 0.00569 0.00032 0.00032 0.00028 0.00000 0.00174 0.00188 0.00193 0.00150 0.00149 0.00146 0.00078 B1 0.44958 0.73703 0.28997 1.00000 0.02497 0.03428 0.03762 -0.00086 -0.01105 -0.00700 0.03211 0.00350 0.00020 0.00021 0.00018 0.00000 0.00102 0.00118 0.00119 0.00092 0.00089 0.00088 0.00047 O1 1.13801 0.84053 0.31246 1.00000 0.03276 0.05105 0.03966 -0.00005 -0.01144 -0.01658 0.03996 0.00228 0.00014 0.00014 0.00011 0.00000 0.00077 0.00094 0.00082 0.00068 0.00064 0.00069 0.00036 O2 1.29422 1.03282 0.25870 1.00000 0.03493 0.03380 0.03419 0.00146 -0.01269 -0.01053 0.03364 0.00212 0.00013 0.00012 0.00010 0.00000 0.00075 0.00075 0.00074 0.00058 0.00060 0.00060 0.00032 F1 0.77581 0.38063 0.10052 1.00000 0.04149 0.03077 0.05694 -0.00612 -0.02507 -0.00001 0.04233 0.00188 0.00012 0.00011 0.00010 0.00000 0.00071 0.00063 0.00081 0.00055 0.00062 0.00053 0.00032 F2 0.70806 0.31506 -0.03738 1.00000 0.04971 0.03639 0.06272 -0.01926 -0.02039 -0.00710 0.04860 0.00191 0.00013 0.00011 0.00011 0.00000 0.00080 0.00070 0.00089 0.00062 0.00068 0.00059 0.00036 F3 0.59518 0.47178 -0.14396 1.00000 0.04593 0.06080 0.04330 -0.01862 -0.01904 -0.01414 0.04757 0.00183 0.00013 0.00013 0.00010 0.00000 0.00076 0.00088 0.00074 0.00063 0.00061 0.00066 0.00035 F4 0.54644 0.69608 -0.10757 1.00000 0.05133 0.05060 0.04108 0.00385 -0.02840 -0.01287 0.04460 0.00193 0.00013 0.00012 0.00010 0.00000 0.00080 0.00079 0.00071 0.00058 0.00062 0.00064 0.00033 F5 0.61453 0.76390 0.03059 1.00000 0.03945 0.03050 0.03818 0.00030 -0.01785 -0.00931 0.03464 0.00170 0.00011 0.00010 0.00009 0.00000 0.00066 0.00060 0.00063 0.00047 0.00052 0.00050 0.00028 F6 0.86912 0.68507 -0.07536 1.00000 0.03793 0.04469 0.02772 -0.00542 -0.00937 -0.01403 0.03601 0.00172 0.00011 0.00011 0.00008 0.00000 0.00065 0.00069 0.00058 0.00049 0.00049 0.00054 0.00029 F7 1.02586 0.79949 -0.17005 1.00000 0.04853 0.04964 0.02510 0.00292 -0.00201 -0.01697 0.04281 0.00205 0.00012 0.00012 0.00009 0.00000 0.00077 0.00077 0.00059 0.00052 0.00052 0.00061 0.00032 F8 1.12226 0.90486 -0.07244 1.00000 0.04283 0.04451 0.04686 0.00871 -0.00569 -0.02377 0.04474 0.00207 0.00012 0.00012 0.00010 0.00000 0.00073 0.00074 0.00076 0.00058 0.00059 0.00060 0.00033 F9 1.05392 0.89855 0.12370 1.00000 0.04789 0.05018 0.04725 0.00331 -0.02098 -0.02898 0.04371 0.00183 0.00013 0.00012 0.00010 0.00000 0.00076 0.00078 0.00075 0.00059 0.00061 0.00063 0.00033 F10 0.89530 0.78384 0.22101 1.00000 0.03602 0.04880 0.02623 0.00084 -0.01149 -0.01895 0.03499 0.00170 0.00011 0.00011 0.00008 0.00000 0.00063 0.00071 0.00056 0.00049 0.00047 0.00054 0.00028 F11 1.04828 0.54957 0.16395 1.00000 0.02478 0.03510 0.04612 0.00531 -0.01108 -0.00890 0.03547 0.00184 0.00010 0.00010 0.00009 0.00000 0.00056 0.00063 0.00069 0.00051 0.00050 0.00047 0.00028 F12 1.14385 0.39199 0.27486 1.00000 0.03194 0.04202 0.05739 0.00156 -0.02559 -0.00223 0.04263 0.00195 0.00011 0.00011 0.00010 0.00000 0.00065 0.00071 0.00081 0.00059 0.00060 0.00054 0.00032 F13 1.00915 0.26967 0.40094 1.00000 0.06005 0.04391 0.04495 0.01266 -0.02505 -0.00152 0.05097 0.00236 0.00014 0.00012 0.00010 0.00000 0.00091 0.00077 0.00076 0.00060 0.00068 0.00066 0.00037 F14 0.77537 0.30414 0.41292 1.00000 0.05236 0.04363 0.04592 0.01476 -0.00418 -0.01452 0.05066 0.00243 0.00013 0.00012 0.00010 0.00000 0.00085 0.00076 0.00077 0.00060 0.00063 0.00064 0.00037 F15 0.67880 0.46140 0.29962 1.00000 0.02645 0.04063 0.04924 0.00322 -0.00735 -0.01128 0.03958 0.00195 0.00011 0.00011 0.00010 0.00000 0.00059 0.00068 0.00074 0.00055 0.00053 0.00050 0.00030 Al2 0.76843 0.63447 0.15744 1.00000 0.02122 0.02714 0.02653 -0.00040 -0.00876 -0.00640 0.02463 0.00080 0.00005 0.00005 0.00004 0.00000 0.00027 0.00029 0.00028 0.00021 0.00021 0.00021 0.00015 P1 0.60589 0.74629 0.28884 1.00000 0.02422 0.02764 0.02745 -0.00001 -0.00940 -0.00743 0.02599 0.00070 0.00004 0.00004 0.00003 0.00000 0.00025 0.00026 0.00025 0.00018 0.00018 0.00019 0.00014 Final Structure Factor Calculation for 2005src0300 in P-1 Total number of l.s. parameters = 549 Maximum vector length = 511 Memory required = 5167 / 27083 wR2 = 0.1501 before cycle 5 for 9117 data and 0 / 549 parameters GooF = S = 1.130; Restrained GooF = 1.130 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0761 * P )^2 + 0.78 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0573 for 7606 Fo > 4sig(Fo) and 0.0684 for all 9117 data wR2 = 0.1501, GooF = S = 1.130, Restrained GooF = 1.130 for all data Occupancy sum of asymmetric unit = 59.00 for non-hydrogen and 33.00 for hydrogen atoms Principal mean square atomic displacements U 0.0319 0.0295 0.0214 C1 0.0467 0.0332 0.0285 C2 0.0590 0.0450 0.0284 C3 0.0553 0.0414 0.0283 C4 0.0506 0.0336 0.0316 C5 0.0389 0.0326 0.0269 C6 0.0312 0.0279 0.0260 C7 0.0467 0.0362 0.0308 C8 0.0666 0.0516 0.0249 C9 0.0572 0.0534 0.0257 C10 0.0485 0.0421 0.0280 C11 0.0386 0.0304 0.0281 C12 0.0367 0.0269 0.0208 C13 0.0398 0.0314 0.0221 C14 0.0536 0.0286 0.0247 C15 0.0533 0.0301 0.0225 C16 0.0431 0.0310 0.0255 C17 0.0352 0.0278 0.0240 C18 0.0290 0.0272 0.0211 C19 0.0331 0.0267 0.0234 C20 0.0406 0.0283 0.0245 C21 0.0443 0.0299 0.0248 C22 0.0379 0.0323 0.0259 C23 0.0322 0.0275 0.0243 C24 0.0310 0.0271 0.0254 C25 0.0312 0.0276 0.0261 C26 0.0437 0.0286 0.0251 C27 0.0517 0.0332 0.0248 C28 0.0480 0.0308 0.0269 C29 0.0337 0.0322 0.0262 C30 0.0700 0.0360 0.0329 C31 0.0827 0.0752 0.0455 C32 0.0541 0.0479 0.0337 C33 0.0725 0.0497 0.0451 C34 0.0639 0.0438 0.0292 C35 0.0740 0.0560 0.0320 C36 0.0593 0.0359 0.0318 C37 0.0742 0.0501 0.0302 C38 0.0455 0.0364 0.0306 Li1 0.0379 0.0345 0.0240 B1 0.0515 0.0397 0.0286 O1 0.0366 0.0327 0.0316 O2 0.0637 0.0364 0.0268 F1 0.0738 0.0477 0.0243 F2 0.0731 0.0471 0.0224 F3 0.0579 0.0511 0.0249 F4 0.0434 0.0310 0.0295 F5 0.0473 0.0359 0.0249 F6 0.0562 0.0492 0.0229 F7 0.0573 0.0529 0.0240 F8 0.0621 0.0455 0.0236 F9 0.0507 0.0304 0.0239 F10 0.0494 0.0331 0.0239 F11 0.0596 0.0472 0.0211 F12 0.0727 0.0559 0.0244 F13 0.0747 0.0499 0.0274 F14 0.0538 0.0399 0.0251 F15 0.0276 0.0263 0.0200 Al2 0.0278 0.0275 0.0227 P1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.010 0.020 0.030 0.042 0.054 0.069 0.089 0.119 0.176 1.000 Number in group 940. 915. 902. 955. 864. 894. 926. 898. 914. 909. GooF 1.153 1.132 1.126 1.056 1.054 1.068 1.037 0.949 0.902 1.653 K 3.569 1.225 1.080 1.021 0.996 0.989 1.011 1.005 1.007 1.017 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.14 1.30 1.61 inf Number in group 937. 905. 916. 920. 882. 916. 921. 901. 911. 908. GooF 1.023 0.946 0.988 0.954 0.918 0.865 0.859 0.941 1.244 2.046 K 1.037 1.063 1.036 1.021 1.016 1.004 1.014 1.004 1.013 1.014 R1 0.151 0.114 0.098 0.081 0.062 0.046 0.038 0.037 0.044 0.084 Recommended weighting scheme: WGHT 0.0760 0.7806 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) -2 0 2 3420.94 9520.08 8.71 0.623 3.81 0 0 3 2738.80 6952.26 8.53 0.532 4.62 1 7 4 623.36 1537.34 7.98 0.250 1.58 0 3 1 9661.94 23694.87 7.95 0.982 3.79 -2 -1 6 1254.48 2940.36 7.80 0.346 1.94 3 -1 6 2197.66 5151.23 7.56 0.458 2.20 -3 -1 2 6013.58 17121.39 7.53 0.835 2.99 -1 1 3 362.04 933.28 7.51 0.195 3.57 6 -1 1 1890.09 6367.58 7.23 0.509 1.83 -2 -3 7 1404.62 3009.30 6.94 0.350 1.62 2 3 7 2407.59 5212.55 6.65 0.461 1.92 1 -4 5 2296.06 4773.23 6.55 0.441 2.01 -2 -5 4 1206.58 3010.99 6.33 0.350 1.88 1 -6 2 973.24 2049.57 6.28 0.289 1.82 -4 -1 1 6482.03 13006.50 6.26 0.728 2.68 6 1 2 266.79 131.96 6.10 0.073 2.03 0 9 3 106.46 15.74 5.86 0.025 1.26 -1 6 0 3185.01 6039.05 5.73 0.496 1.86 -6 0 1 3796.92 7416.51 5.71 0.550 1.78 -3 -1 1 12051.29 24557.71 5.41 1.000 3.45 8 5 0 1209.27 2078.46 5.26 0.291 1.38 3 -2 5 15.89 0.01 5.26 0.001 2.27 4 -5 1 4069.69 6950.60 5.23 0.532 1.63 0 9 0 32.99 4.17 5.12 0.013 1.31 3 -2 1 49.70 108.08 4.92 0.066 2.91 5 0 1 1187.86 1987.59 4.86 0.284 2.33 -5 -1 3 3601.60 6191.50 4.86 0.502 1.85 -2 6 4 14.14 0.07 4.80 0.002 1.48 1 -2 5 63.34 26.15 4.64 0.033 2.54 3 -3 2 1222.38 2071.69 4.61 0.290 2.43 1 -3 3 88.35 46.84 4.36 0.044 2.90 -3 -3 3 51.02 3.94 4.25 0.013 2.34 4 5 6 188.66 308.54 4.15 0.112 1.77 -5 -4 4 229.18 142.45 4.15 0.076 1.59 4 1 3 37.86 78.03 4.12 0.056 2.92 1 3 8 1820.94 3007.00 4.09 0.350 1.66 6 12 0 21.39 0.53 4.03 0.005 0.99 -4 -4 5 67.76 123.43 4.03 0.071 1.61 3 9 9 37.00 7.60 3.98 0.018 1.08 -1 3 5 2475.90 4216.54 3.97 0.414 2.06 6 8 6 3739.74 5705.55 3.97 0.482 1.30 10 0 0 223.74 139.56 3.96 0.075 1.12 2 -6 1 1457.06 2328.25 3.96 0.308 1.73 3 -2 2 13612.03 8321.44 3.96 0.582 2.87 1 -2 2 670.49 437.61 3.94 0.133 4.17 -2 -6 1 46.92 86.70 3.74 0.059 1.99 -2 4 1 48.24 87.71 3.73 0.060 2.28 -6 1 2 64.80 35.14 3.71 0.038 1.61 3 -5 5 99.94 59.70 3.69 0.049 1.62 6 0 9 11.17 0.25 3.68 0.003 1.42 Bond lengths and angles C1 - Distance Angles C2 1.3951 (0.0029) C6 1.4006 (0.0028) 118.12 (0.19) P1 1.8311 (0.0020) 123.26 (0.15) 118.62 (0.15) C1 - C2 C6 C2 - Distance Angles C3 1.3950 (0.0032) C1 1.3951 (0.0029) 120.87 (0.20) C2 - C3 C3 - Distance Angles C4 1.3846 (0.0035) C2 1.3950 (0.0032) 120.19 (0.22) C3 - C4 C4 - Distance Angles C3 1.3846 (0.0035) C5 1.3846 (0.0035) 119.54 (0.21) C4 - C3 C5 - Distance Angles C4 1.3846 (0.0035) C6 1.3883 (0.0032) 120.47 (0.21) C5 - C4 C6 - Distance Angles C5 1.3883 (0.0032) C1 1.4006 (0.0028) 120.78 (0.20) C6 - C5 C7 - Distance Angles C8 1.3864 (0.0030) C12 1.4008 (0.0028) 118.70 (0.18) P1 1.8343 (0.0020) 120.54 (0.16) 120.75 (0.15) C7 - C8 C12 C8 - Distance Angles C7 1.3864 (0.0030) C9 1.3971 (0.0032) 120.59 (0.21) C8 - C7 C9 - Distance Angles C10 1.3793 (0.0037) C8 1.3971 (0.0032) 120.22 (0.21) C9 - C10 C10 - Distance Angles C9 1.3793 (0.0037) C11 1.3884 (0.0034) 119.83 (0.21) C10 - C9 C11 - Distance Angles C10 1.3884 (0.0034) C12 1.3893 (0.0029) 120.04 (0.21) C11 - C10 C12 - Distance Angles C11 1.3893 (0.0029) C7 1.4008 (0.0028) 120.57 (0.20) C12 - C11 C13 - Distance Angles C18 1.3859 (0.0028) C14 1.3871 (0.0029) 114.23 (0.18) Al2 2.0080 (0.0020) 119.61 (0.15) 125.54 (0.15) C13 - C18 C14 C14 - Distance Angles F1 1.3541 (0.0024) C13 1.3871 (0.0029) 120.32 (0.18) C15 1.3881 (0.0030) 116.07 (0.18) 123.59 (0.19) C14 - F1 C13 C15 - Distance Angles F2 1.3510 (0.0025) C16 1.3755 (0.0033) 119.80 (0.19) C14 1.3881 (0.0030) 120.82 (0.20) 119.38 (0.20) C15 - F2 C16 C16 - Distance Angles F3 1.3436 (0.0024) C15 1.3755 (0.0033) 120.38 (0.20) C17 1.3828 (0.0032) 120.13 (0.20) 119.49 (0.19) C16 - F3 C15 C17 - Distance Angles F4 1.3484 (0.0024) C18 1.3797 (0.0028) 121.55 (0.19) C16 1.3828 (0.0032) 119.57 (0.18) 118.88 (0.19) C17 - F4 C18 C18 - Distance Angles F5 1.3636 (0.0023) C17 1.3797 (0.0028) 116.50 (0.18) C13 1.3859 (0.0028) 119.07 (0.17) 124.38 (0.19) C18 - F5 C17 C19 - Distance Angles C20 1.3853 (0.0027) C24 1.3876 (0.0028) 113.51 (0.18) Al2 2.0089 (0.0020) 126.48 (0.15) 119.78 (0.14) C19 - C20 C24 C20 - Distance Angles F6 1.3587 (0.0023) C19 1.3853 (0.0027) 120.29 (0.17) C21 1.3856 (0.0029) 115.61 (0.17) 124.10 (0.18) C20 - F6 C19 C21 - Distance Angles F7 1.3449 (0.0023) C22 1.3727 (0.0031) 119.70 (0.19) C20 1.3856 (0.0029) 120.83 (0.19) 119.45 (0.18) C21 - F7 C22 C22 - Distance Angles F8 1.3375 (0.0024) C21 1.3727 (0.0031) 120.70 (0.19) C23 1.3799 (0.0030) 120.03 (0.19) 119.26 (0.19) C22 - F8 C21 C23 - Distance Angles F9 1.3491 (0.0024) C24 1.3784 (0.0029) 121.30 (0.18) C22 1.3799 (0.0030) 119.74 (0.18) 118.96 (0.19) C23 - F9 C24 C24 - Distance Angles F10 1.3611 (0.0022) C23 1.3784 (0.0029) 116.68 (0.17) C19 1.3876 (0.0028) 118.60 (0.17) 124.71 (0.18) C24 - F10 C23 C25 - Distance Angles C30 1.3824 (0.0029) C26 1.3903 (0.0027) 114.32 (0.18) Al2 2.0070 (0.0020) 118.24 (0.14) 127.27 (0.15) C25 - C30 C26 C26 - Distance Angles F11 1.3506 (0.0024) C27 1.3880 (0.0028) 116.10 (0.17) C25 1.3903 (0.0027) 120.70 (0.17) 123.20 (0.19) C26 - F11 C27 C27 - Distance Angles F12 1.3485 (0.0024) C28 1.3771 (0.0032) 119.61 (0.18) C26 1.3880 (0.0028) 121.00 (0.19) 119.37 (0.19) C27 - F12 C28 C28 - Distance Angles F13 1.3494 (0.0024) C27 1.3771 (0.0032) 119.86 (0.20) C29 1.3847 (0.0032) 120.00 (0.20) 120.12 (0.18) C28 - F13 C27 C29 - Distance Angles F14 1.3396 (0.0025) C30 1.3810 (0.0029) 122.13 (0.20) C28 1.3847 (0.0033) 120.00 (0.19) 117.87 (0.19) C29 - F14 C30 C30 - Distance Angles F15 1.3553 (0.0023) C29 1.3810 (0.0029) 116.74 (0.18) C25 1.3824 (0.0029) 118.14 (0.17) 125.11 (0.19) C30 - F15 C29 C31 - Distance Angles C32 1.4664 (0.0043) O1 1.4846 (0.0030) 113.62 (0.21) C31 - C32 C32 - Distance Angles C31 1.4664 (0.0043) C32 - C33 - Distance Angles O1 1.4139 (0.0028) C34 1.4677 (0.0038) 108.67 (0.22) C33 - O1 C34 - Distance Angles C33 1.4677 (0.0038) C34 - C35 - Distance Angles O2 1.4312 (0.0027) C36 1.4892 (0.0039) 109.44 (0.20) C35 - O2 C36 - Distance Angles C35 1.4892 (0.0039) C36 - C37 - Distance Angles O2 1.4317 (0.0027) C38 1.5039 (0.0038) 109.21 (0.20) C37 - O2 C38 - Distance Angles C37 1.5039 (0.0038) C38 - Li1 - Distance Angles O1 1.8866 (0.0040) O2 1.8910 (0.0041) 124.68 (0.21) B1_$2 2.3460 (0.0043) 115.49 (0.19) 119.81 (0.19) Li1 - O1 O2 B1 - Distance Angles P1 1.9491 (0.0024) Li1_$1 2.3460 (0.0043) 129.11 (0.15) B1 - P1 O1 - Distance Angles C33 1.4139 (0.0028) C31 1.4846 (0.0030) 112.70 (0.18) Li1 1.8866 (0.0041) 134.10 (0.20) 112.67 (0.18) O1 - C33 C31 O2 - Distance Angles C35 1.4312 (0.0027) C37 1.4317 (0.0027) 112.70 (0.18) Li1 1.8910 (0.0041) 122.88 (0.18) 124.28 (0.18) O2 - C35 C37 F1 - Distance Angles C14 1.3541 (0.0024) F1 - F2 - Distance Angles C15 1.3510 (0.0025) F2 - F3 - Distance Angles C16 1.3436 (0.0024) F3 - F4 - Distance Angles C17 1.3484 (0.0024) F4 - F5 - Distance Angles C18 1.3636 (0.0023) F5 - F6 - Distance Angles C20 1.3587 (0.0023) F6 - F7 - Distance Angles C21 1.3449 (0.0023) F7 - F8 - Distance Angles C22 1.3375 (0.0024) F8 - F9 - Distance Angles C23 1.3491 (0.0024) F9 - F10 - Distance Angles C24 1.3611 (0.0022) F10 - F11 - Distance Angles C26 1.3506 (0.0024) F11 - F12 - Distance Angles C27 1.3485 (0.0024) F12 - F13 - Distance Angles C28 1.3494 (0.0024) F13 - F14 - Distance Angles C29 1.3396 (0.0025) F14 - F15 - Distance Angles C30 1.3553 (0.0023) F15 - Al2 - Distance Angles C25 2.0070 (0.0020) C13 2.0080 (0.0020) 113.87 (0.09) C19 2.0089 (0.0020) 110.91 (0.08) 109.05 (0.08) P1 2.4538 (0.0009) 103.01 (0.06) 109.11 (0.06) 110.77 (0.06) Al2 - C25 C13 C19 P1 - Distance Angles C1 1.8311 (0.0021) C7 1.8343 (0.0020) 104.78 (0.09) B1 1.9491 (0.0024) 110.73 (0.10) 109.00 (0.10) Al2 2.4538 (0.0009) 110.55 (0.07) 109.31 (0.07) 112.19 (0.08) P1 - C1 C7 B1 FMAP and GRID set by program FMAP 2 3 37 GRID -1.471 -2 -2 1.471 2 2 R1 = 0.0681 for 9117 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.78 at 0.9017 0.0121 0.3367 [ 0.89 A from H34B ] Deepest hole -0.47 at 0.4626 0.4020 0.2095 [ 1.84 A from F3 ] Mean = 0.00, Rms deviation from mean = 0.12 e/A^3, Highest memory used = 4807 / 37193 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.9017 1.0121 0.3367 1.00000 0.05 0.78 0.89 H34B 1.29 C34 1.57 H34C 1.72 H33B Q2 1 0.6742 0.7024 0.2231 1.00000 0.05 0.67 1.11 P1 1.36 AL2 2.41 C1 2.53 C7 Q3 1 1.0707 0.7905 0.3688 1.00000 0.05 0.63 1.23 O1 1.25 C33 1.30 H33A 1.48 C31 Q4 1 0.8376 0.5622 0.1901 1.00000 0.05 0.46 0.82 C25 1.23 AL2 1.88 C26 2.02 C30 Q5 1 0.9138 0.5033 0.5002 1.00000 0.05 0.46 1.84 H11 2.27 C11 2.30 H32B 2.42 H32C Q6 1 1.1033 0.9065 0.3288 1.00000 0.05 0.44 0.82 O1 1.07 C33 1.56 C34 1.76 H33A Q7 1 0.5078 0.6515 0.1546 1.00000 0.05 0.40 1.75 H3B 1.87 H1B 2.13 C18 2.14 B1 Q8 1 0.6642 1.0063 0.1782 1.00000 0.05 0.40 0.69 C5 0.95 C6 1.35 H5 1.60 H6 Q9 1 1.1777 0.8804 0.2652 1.00000 0.05 0.39 0.90 O1 1.40 LI1 2.00 C33 2.03 C31 Q10 1 0.7183 0.8823 0.1272 1.00000 0.05 0.38 1.06 H6 1.37 C6 2.21 C1 2.24 C19 Shortest distances between peaks (including symmetry equivalents) 6 9 1.07 3 6 1.60 8 10 1.63 5 5 2.09 3 9 2.12 2 4 2.19 1 6 2.42 2 10 2.61 2 7 2.78 Time profile in seconds ----------------------- 0.11: Read and process instructions 0.00: Fit rigid groups 0.02: Interpret restraints etc. 0.00: Generate connectivity array 0.02: 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. 1.72: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 2.55: Structure factors and derivatives 13.36: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 1.00: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.16: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.09: Fourier summations 0.00: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2005src0300 finished at 12:58:37 Total CPU time: 19.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++