+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2005src0633 started at 19:42:08 on 14-May-2005 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2005src0633 in P-1 CELL 0.71073 8.5452 15.8511 16.0041 99.750 96.414 91.167 ZERR 2.00 0.0020 0.0049 0.0031 0.017 0.020 0.017 LATT 1 SFAC C H LI B O F P UNIT 76 90 2 4 16 30 2 V = 2121.38 F(000) = 1000.0 Mu = 0.18 mm-1 Cell Wt = 1948.54 Rho = 1.525 MERG 2 OMIT -3.00 55.00 OMIT -1 5 8 OMIT 0 2 1 OMIT 0 1 2 EXTI 0.00522 FMAP 2 PLAN 10 SIZE 0.04 0.12 0.12 ACTA BOND $H WGHT 0.04480 1.79570 L.S. 4 TEMP -153.00 FVAR 0.38857 LI1 3 0.862731 0.704262 0.231598 11.00000 0.04030 0.03186 = 0.03329 0.00495 0.00449 -0.00093 H1P 2 0.944987 0.172992 0.086387 11.00000 0.02574 H1B 2 0.737439 0.297861 0.040049 11.00000 0.03395 H3B 2 0.906418 0.353945 0.119542 11.00000 0.03999 H2B 2 0.702110 0.344488 0.149561 11.00000 0.03539 MOLE 1 C1 1 0.689088 0.127749 0.121795 11.00000 0.03036 0.02712 = 0.02758 0.00594 -0.00122 -0.00829 C2 1 0.543102 0.164669 0.159550 11.00000 0.02824 0.04140 = 0.04124 0.00858 0.00155 -0.00818 AFIX 137 H2A 2 0.453258 0.123795 0.141185 11.00000 -1.50000 H2B 2 0.519265 0.218660 0.139640 11.00000 -1.50000 H2C 2 0.563301 0.175195 0.222002 11.00000 -1.50000 AFIX 0 C3 1 0.652635 0.107969 0.024171 11.00000 0.04472 0.03668 = 0.02948 0.00540 -0.00566 -0.01652 AFIX 137 H3A 2 0.559796 0.068813 0.008425 11.00000 -1.50000 H3B 2 0.743128 0.081167 -0.000597 11.00000 -1.50000 H3C 2 0.631716 0.161303 0.002378 11.00000 -1.50000 AFIX 0 C4 1 0.731280 0.043904 0.153086 11.00000 0.04549 0.02638 = 0.03858 0.00845 -0.00343 -0.01169 AFIX 137 H4A 2 0.754006 0.054896 0.215442 11.00000 -1.50000 H4B 2 0.824322 0.021073 0.127834 11.00000 -1.50000 H4C 2 0.642474 0.002162 0.135978 11.00000 -1.50000 AFIX 0 C5 1 1.098842 0.139249 0.277040 11.00000 0.02521 0.01970 = 0.02587 0.00462 0.00416 -0.00408 C6 1 1.156944 0.078003 0.216804 11.00000 0.02704 0.02524 = 0.02384 0.00434 0.00352 -0.00193 C7 1 1.258553 0.015841 0.236065 11.00000 0.02950 0.02090 = 0.03321 -0.00238 0.01009 0.00102 C8 1 1.305624 0.010231 0.319513 11.00000 0.02853 0.01837 = 0.04106 0.00927 0.00522 0.00371 C9 1 1.253467 0.068891 0.382554 11.00000 0.02768 0.02501 = 0.02797 0.01103 0.00123 -0.00227 C10 1 1.157550 0.131739 0.360284 11.00000 0.02368 0.02141 = 0.02488 0.00292 0.00596 -0.00012 C11 1 1.106299 0.303604 0.273691 11.00000 0.02347 0.02132 = 0.02236 0.00652 0.00100 0.00326 C12 1 1.193780 0.318327 0.208736 11.00000 0.02550 0.02319 = 0.02640 0.00298 0.00072 -0.00282 C13 1 1.292382 0.388879 0.212523 11.00000 0.02497 0.03246 = 0.03208 0.01072 0.00346 -0.00391 C14 1 1.313694 0.448689 0.286080 11.00000 0.02645 0.02038 = 0.04011 0.00919 -0.00478 -0.00800 C15 1 1.237584 0.435852 0.354266 11.00000 0.02804 0.02028 = 0.02824 0.00200 -0.00582 -0.00137 C16 1 1.138497 0.364835 0.347233 11.00000 0.02469 0.02401 = 0.02227 0.00705 0.00068 0.00184 C17 1 0.844046 0.232423 0.325402 11.00000 0.02142 0.02226 = 0.02003 0.00290 -0.00210 -0.00298 C18 1 0.766085 0.308787 0.339770 11.00000 0.02555 0.02512 = 0.02337 0.00487 -0.00026 -0.00108 C19 1 0.640246 0.321357 0.386610 11.00000 0.02491 0.03154 = 0.02860 0.00082 0.00003 0.00472 C20 1 0.581510 0.255321 0.420500 11.00000 0.02164 0.04501 = 0.02425 0.00087 0.00360 -0.00061 C21 1 0.654131 0.178899 0.409789 11.00000 0.02576 0.03733 = 0.02387 0.00902 0.00183 -0.00874 C22 1 0.781982 0.169181 0.363745 11.00000 0.02491 0.02516 = 0.02554 0.00507 0.00003 0.00096 C31 1 0.563697 0.696094 0.322236 11.00000 0.02690 0.02663 = 0.03638 0.00512 0.00441 0.00186 AFIX 23 H31A 2 0.501796 0.674135 0.363284 11.00000 -1.20000 H31B 2 0.493253 0.695935 0.268714 11.00000 -1.20000 AFIX 0 C32 1 0.623969 0.785913 0.358391 11.00000 0.02958 0.02717 = 0.03841 0.00711 0.00796 0.00382 AFIX 23 H32A 2 0.535027 0.823856 0.368800 11.00000 -1.20000 H32B 2 0.691537 0.787306 0.413086 11.00000 -1.20000 AFIX 0 C33 1 0.803724 0.890467 0.328786 11.00000 0.04625 0.01860 = 0.03391 0.00615 0.00599 -0.00396 AFIX 23 H33A 2 0.741311 0.930498 0.364931 11.00000 -1.20000 H33B 2 0.828489 0.917876 0.280397 11.00000 -1.20000 AFIX 0 C34 1 0.953777 0.874132 0.380058 11.00000 0.04186 0.02732 = 0.02962 -0.00005 0.00759 -0.01029 AFIX 23 H34A 2 1.018297 0.927985 0.398906 11.00000 -1.20000 H34B 2 0.931036 0.850746 0.431188 11.00000 -1.20000 AFIX 0 C35 1 1.156948 0.772250 0.370147 11.00000 0.03009 0.04967 = 0.03138 0.00645 -0.00247 -0.00604 AFIX 23 H35A 2 1.212803 0.814259 0.417459 11.00000 -1.20000 H35B 2 1.234184 0.751057 0.330565 11.00000 -1.20000 AFIX 0 C36 1 1.092896 0.698612 0.405511 11.00000 0.03254 0.04232 = 0.02984 0.00487 -0.00345 -0.00137 AFIX 23 H36A 2 1.179750 0.669813 0.434296 11.00000 -1.20000 H36B 2 1.019431 0.719112 0.447510 11.00000 -1.20000 AFIX 0 C37 1 0.915217 0.576284 0.359272 11.00000 0.03638 0.02774 = 0.03400 0.01082 0.00430 0.00589 AFIX 23 H37A 2 0.969068 0.556562 0.410121 11.00000 -1.20000 H37B 2 0.898972 0.526514 0.312197 11.00000 -1.20000 AFIX 0 C38 1 0.759246 0.610244 0.378863 11.00000 0.03434 0.02701 = 0.03132 0.01107 0.00609 0.00278 AFIX 23 H38A 2 0.690329 0.564201 0.391551 11.00000 -1.20000 H38B 2 0.773140 0.656906 0.429046 11.00000 -1.20000 AFIX 0 B1 4 0.792971 0.315967 0.109802 11.00000 0.03579 0.02938 = 0.03314 0.01173 -0.00286 -0.00315 B2 4 0.984590 0.219259 0.261866 11.00000 0.02572 0.01930 = 0.02070 0.00476 0.00225 -0.00181 O5 5 0.691115 0.641743 0.305341 11.00000 0.02994 0.02177 = 0.02848 0.00637 0.00212 0.00342 O6 5 0.712719 0.813306 0.296838 11.00000 0.03651 0.02186 = 0.03082 0.00635 0.00314 -0.00514 O7 5 1.035505 0.813681 0.325970 11.00000 0.03692 0.04089 = 0.02532 0.00424 0.00588 0.00082 O8 5 1.012364 0.640816 0.335191 11.00000 0.03049 0.03592 = 0.02594 0.00227 0.00342 -0.00283 F1 6 1.117091 0.075831 0.131866 11.00000 0.04215 0.03638 = 0.02404 -0.00007 0.00415 0.00663 F2 6 1.311401 -0.039839 0.173120 11.00000 0.04362 0.02864 = 0.04195 -0.00394 0.01179 0.00868 F3 6 1.401274 -0.051456 0.339065 11.00000 0.04341 0.03075 = 0.05507 0.01287 0.00636 0.01459 F4 6 1.294704 0.063497 0.465055 11.00000 0.03614 0.03743 = 0.03133 0.01416 0.00179 0.00801 F5 6 1.116404 0.189005 0.426370 11.00000 0.03263 0.02717 = 0.02280 0.00272 0.00365 0.00580 F6 6 1.182704 0.261187 0.134812 11.00000 0.03291 0.03473 = 0.02857 -0.00049 0.00914 -0.00774 F7 6 1.364796 0.400446 0.144795 11.00000 0.03987 0.04819 = 0.04018 0.01225 0.01048 -0.01740 F8 6 1.408891 0.518156 0.291087 11.00000 0.04016 0.02941 = 0.05603 0.01057 -0.00303 -0.01765 F9 6 1.261793 0.492565 0.427612 11.00000 0.03986 0.02608 = 0.03734 -0.00374 -0.00546 -0.00483 F10 6 1.069423 0.358534 0.418063 11.00000 0.03632 0.02847 = 0.02179 0.00266 0.00209 -0.00320 F11 6 0.813800 0.377505 0.308763 11.00000 0.03414 0.02336 = 0.03637 0.01024 0.00407 0.00453 F12 6 0.575923 0.398520 0.400142 11.00000 0.03361 0.04031 = 0.04121 -0.00108 0.00337 0.01304 F13 6 0.457479 0.266084 0.465718 11.00000 0.03299 0.06379 = 0.04049 0.00389 0.01618 0.00142 F14 6 0.602395 0.113072 0.444455 11.00000 0.03722 0.04689 = 0.03672 0.01454 0.00847 -0.01275 F15 6 0.845528 0.091105 0.358673 11.00000 0.03271 0.02348 = 0.03721 0.01022 0.00734 -0.00157 P1 7 0.857274 0.208836 0.144665 11.00000 0.02609 0.02266 = 0.02292 0.00545 0.00133 -0.00412 MOLE 2 C23 1 0.622565 0.583022 0.100749 11.00000 0.04672 0.03760 = 0.04815 -0.01068 -0.00133 -0.00919 AFIX 23 H23A 2 0.547564 0.569975 0.048029 11.00000 -1.20000 H23B 2 0.577047 0.557793 0.145614 11.00000 -1.20000 AFIX 0 C24 1 0.772561 0.542144 0.084626 11.00000 0.06958 0.02864 = 0.04116 0.00149 -0.01078 -0.00146 AFIX 23 H24A 2 0.757571 0.478996 0.074883 11.00000 -1.20000 H24B 2 0.811134 0.558961 0.033488 11.00000 -1.20000 AFIX 0 C25 1 1.042726 0.551922 0.144504 11.00000 0.05653 0.03929 = 0.04655 0.00330 0.02161 0.00786 AFIX 23 H25A 2 1.044455 0.498453 0.102507 11.00000 -1.20000 H25B 2 1.101510 0.542827 0.198951 11.00000 -1.20000 AFIX 0 C26 1 1.120305 0.621742 0.113598 11.00000 0.05310 0.03908 = 0.05345 -0.00055 0.01539 0.00306 AFIX 23 H26A 2 1.233389 0.610638 0.110955 11.00000 -1.20000 H26B 2 1.071346 0.626348 0.055574 11.00000 -1.20000 AFIX 0 C27 1 1.131499 0.775189 0.138819 11.00000 0.06899 0.04592 = 0.05397 0.01369 0.02564 -0.01159 AFIX 23 H27A 2 1.217845 0.766265 0.102228 11.00000 -1.20000 H27B 2 1.165872 0.822211 0.186891 11.00000 -1.20000 AFIX 0 C28 1 0.991477 0.799986 0.089203 11.00000 0.07769 0.05359 = 0.04595 0.02216 0.01613 -0.01070 AFIX 23 H28A 2 1.012349 0.856040 0.072305 11.00000 -1.20000 H28B 2 0.964999 0.757004 0.036641 11.00000 -1.20000 AFIX 0 C29 1 0.714372 0.804197 0.089709 11.00000 0.06789 0.03637 = 0.04625 0.01508 -0.01160 0.00553 AFIX 23 H29A 2 0.725741 0.834608 0.041420 11.00000 -1.20000 H29B 2 0.638744 0.835314 0.125000 11.00000 -1.20000 AFIX 0 C30 1 0.650205 0.716591 0.055899 11.00000 0.07622 0.04662 = 0.04239 0.01427 -0.01635 0.00343 AFIX 23 H30A 2 0.544891 0.718412 0.023599 11.00000 -1.20000 H30B 2 0.720614 0.685818 0.017010 11.00000 -1.20000 AFIX 0 O1 5 0.638830 0.673805 0.126860 11.00000 0.05200 0.02947 = 0.03118 0.00476 -0.00564 -0.00044 O2 5 0.881963 0.570289 0.157613 11.00000 0.03991 0.03074 = 0.02639 0.00322 0.00378 0.00183 O3 5 1.103199 0.699396 0.171308 11.00000 0.05867 0.03324 = 0.02994 0.00303 0.01554 -0.00730 O4 5 0.861611 0.805761 0.139413 11.00000 0.05851 0.04051 = 0.02706 0.00535 0.00413 -0.00515 HKLF 4 Covalent radii and connectivity table for 2005src0633 in P-1 C 0.770 H 0.320 LI 1.520 B 0.820 O 0.660 F 0.640 P 1.100 Li1 - O2 O5 O6 O8 O4 O3 O1 O7 C1 - C2 C4 C3 P1 C2 - C1 C3 - C1 C4 - C1 C5 - C6 C10 B2 C6 - F1 C7 C5 C7 - F2 C8 C6 C8 - F3 C7 C9 C9 - F4 C10 C8 C10 - F5 C9 C5 C11 - C16 C12 B2 C12 - F6 C13 C11 C13 - F7 C14 C12 C14 - F8 C15 C13 C15 - F9 C14 C16 C16 - F10 C15 C11 C17 - C22 C18 B2 C18 - F11 C19 C17 C19 - F12 C20 C18 C20 - F13 C21 C19 C21 - F14 C20 C22 C22 - F15 C21 C17 C31 - O5 C32 C32 - O6 C31 C33 - O6 C34 C34 - O7 C33 C35 - O7 C36 C36 - O8 C35 C37 - O8 C38 C38 - O5 C37 B1 - P1 B2 - C11 C5 C17 P1 O5 - C31 C38 Li1 O6 - C33 C32 Li1 O7 - C35 C34 Li1 O8 - C36 C37 Li1 F1 - C6 F2 - C7 F3 - C8 F4 - C9 F5 - C10 F6 - C12 F7 - C13 F8 - C14 F9 - C15 F10 - C16 F11 - C18 F12 - C19 F13 - C20 F14 - C21 F15 - C22 P1 - C1 B1 B2 C23 - O1 C24 C24 - O2 C23 C25 - O2 C26 C26 - O3 C25 C27 - O3 C28 C28 - O4 C27 C29 - O4 C30 C30 - O1 C29 O1 - C23 C30 Li1 O2 - C24 C25 Li1 O3 - C27 C26 Li1 O4 - C29 C28 Li1 48359 Reflections read, of which 94 rejected -11 =< h =< 11, -20 =< k =< 20, -20 =< l =< 19, 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) 6 11 4 47.53 9.42 2 47.47 -5 -12 6 3.53 2.70 3 19.74 -5 -8 6 21.34 4.23 2 41.31 -4 8 6 9.19 6.22 2 90.76 -4 -9 7 41.01 2.12 6 16.26 3 8 11 107.85 5.25 5 31.27 -2 5 12 58.28 2.20 2 12.12 -3 2 13 46.78 1.34 7 7.19 -2 -3 14 3.59 1.34 4 7.41 -1 -3 14 13.00 0.71 8 5.99 -2 -2 14 26.59 1.36 6 10.57 4 3 15 5.74 2.50 3 16.08 12 Inconsistent equivalents 9718 Unique reflections, of which 0 suppressed R(int) = 0.0649 R(sigma) = 0.0663 Friedel opposites merged Maximum memory for data reduction = 5339 / 97121 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 = 6986 / 830526 wR2 = 0.1270 before cycle 1 for 9718 data and 606 / 606 parameters GooF = S = 1.017; Restrained GooF = 1.017 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0448 * P )^2 + 1.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38856 0.00060 -0.022 OSF 2 0.00522 0.00069 -0.001 EXTI Mean shift/esd = 0.005 Maximum = -0.026 for U23 C23 Max. shift = 0.001 A for H1P Max. dU = 0.000 for H2B Least-squares cycle 2 Maximum vector length = 511 Memory required = 6986 / 830526 wR2 = 0.1270 before cycle 2 for 9718 data and 606 / 606 parameters GooF = S = 1.017; Restrained GooF = 1.017 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0448 * P )^2 + 1.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38855 0.00060 -0.011 OSF 2 0.00522 0.00069 -0.003 EXTI Mean shift/esd = 0.002 Maximum = -0.011 for OSF Max. shift = 0.000 A for H3B Max. dU = 0.000 for H2B Least-squares cycle 3 Maximum vector length = 511 Memory required = 6986 / 830526 wR2 = 0.1270 before cycle 3 for 9718 data and 606 / 606 parameters GooF = S = 1.017; Restrained GooF = 1.017 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0448 * P )^2 + 1.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38855 0.00060 0.002 OSF 2 0.00522 0.00069 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.002 for U33 C28 Max. shift = 0.000 A for H3B Max. dU = 0.000 for C30 Least-squares cycle 4 Maximum vector length = 511 Memory required = 6986 / 830526 wR2 = 0.1270 before cycle 4 for 9718 data and 606 / 606 parameters GooF = S = 1.017; Restrained GooF = 1.017 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0448 * P )^2 + 1.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38855 0.00060 0.000 OSF 2 0.00522 0.00069 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for U33 C28 Max. shift = 0.000 A for H3B Max. dU = 0.000 for H1P Largest correlation matrix elements 0.536 EXTI / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2A 0.4533 0.1238 0.1412 137 0.980 0.000 C2 C1 H2A H2B 0.5193 0.2187 0.1396 137 0.980 0.000 C2 C1 H2A H2C 0.5633 0.1752 0.2220 137 0.980 0.000 C2 C1 H2A H3A 0.5598 0.0688 0.0084 137 0.980 0.000 C3 C1 H3A H3B 0.7431 0.0812 -0.0006 137 0.980 0.000 C3 C1 H3A H3C 0.6317 0.1613 0.0024 137 0.980 0.000 C3 C1 H3A H4A 0.7540 0.0549 0.2154 137 0.980 0.000 C4 C1 H4A H4B 0.8243 0.0211 0.1278 137 0.980 0.000 C4 C1 H4A H4C 0.6425 0.0022 0.1360 137 0.980 0.000 C4 C1 H4A H31A 0.5018 0.6741 0.3633 23 0.990 0.000 C31 O5 C32 H31B 0.4932 0.6959 0.2687 23 0.990 0.000 C31 O5 C32 H32A 0.5350 0.8239 0.3688 23 0.990 0.000 C32 O6 C31 H32B 0.6915 0.7873 0.4131 23 0.990 0.000 C32 O6 C31 H33A 0.7413 0.9305 0.3649 23 0.990 0.000 C33 O6 C34 H33B 0.8285 0.9179 0.2804 23 0.990 0.000 C33 O6 C34 H34A 1.0183 0.9280 0.3989 23 0.990 0.000 C34 O7 C33 H34B 0.9310 0.8507 0.4312 23 0.990 0.000 C34 O7 C33 H35A 1.2128 0.8143 0.4175 23 0.990 0.000 C35 O7 C36 H35B 1.2342 0.7511 0.3306 23 0.990 0.000 C35 O7 C36 H36A 1.1798 0.6698 0.4343 23 0.990 0.000 C36 O8 C35 H36B 1.0194 0.7191 0.4475 23 0.990 0.000 C36 O8 C35 H37A 0.9691 0.5566 0.4101 23 0.990 0.000 C37 O8 C38 H37B 0.8990 0.5265 0.3122 23 0.990 0.000 C37 O8 C38 H38A 0.6903 0.5642 0.3916 23 0.990 0.000 C38 O5 C37 H38B 0.7731 0.6569 0.4290 23 0.990 0.000 C38 O5 C37 H23A 0.5476 0.5700 0.0480 23 0.990 0.000 C23 O1 C24 H23B 0.5770 0.5578 0.1456 23 0.990 0.000 C23 O1 C24 H24A 0.7576 0.4790 0.0749 23 0.990 0.000 C24 O2 C23 H24B 0.8111 0.5590 0.0335 23 0.990 0.000 C24 O2 C23 H25A 1.0444 0.4985 0.1025 23 0.990 0.000 C25 O2 C26 H25B 1.1015 0.5428 0.1989 23 0.990 0.000 C25 O2 C26 H26A 1.2334 0.6106 0.1110 23 0.990 0.000 C26 O3 C25 H26B 1.0714 0.6264 0.0556 23 0.990 0.000 C26 O3 C25 H27A 1.2178 0.7663 0.1022 23 0.990 0.000 C27 O3 C28 H27B 1.1659 0.8222 0.1869 23 0.990 0.000 C27 O3 C28 H28A 1.0124 0.8560 0.0723 23 0.990 0.000 C28 O4 C27 H28B 0.9650 0.7570 0.0366 23 0.990 0.000 C28 O4 C27 H29A 0.7257 0.8346 0.0414 23 0.990 0.000 C29 O4 C30 H29B 0.6387 0.8353 0.1250 23 0.990 0.000 C29 O4 C30 H30A 0.5449 0.7184 0.0236 23 0.990 0.000 C30 O1 C29 H30B 0.7206 0.6858 0.0170 23 0.990 0.000 C30 O1 C29 2005src0633 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Li1 0.86273 0.70426 0.23160 1.00000 0.04030 0.03186 0.03327 0.00495 0.00449 -0.00093 0.03524 0.00845 0.00053 0.00028 0.00027 0.00000 0.00256 0.00241 0.00238 0.00187 0.00190 0.00196 0.00100 H1P 0.94505 0.17298 0.08637 1.00000 0.02570 0.04534 0.00276 0.00151 0.00147 0.00000 0.00632 H1B 0.73741 0.29786 0.04005 1.00000 0.03396 0.05059 0.00298 0.00163 0.00164 0.00000 0.00698 H3B 0.90636 0.35397 0.11955 1.00000 0.03995 0.05406 0.00329 0.00175 0.00168 0.00000 0.00751 H2B 0.70214 0.34446 0.14955 1.00000 0.03549 0.04988 0.00313 0.00168 0.00164 0.00000 0.00711 C1 0.68909 0.12775 0.12180 1.00000 0.03035 0.02713 0.02757 0.00594 -0.00122 -0.00829 0.02869 0.00455 0.00029 0.00016 0.00015 0.00000 0.00134 0.00133 0.00128 0.00102 0.00102 0.00106 0.00055 C2 0.54310 0.16467 0.15955 1.00000 0.02823 0.04140 0.04123 0.00859 0.00154 -0.00819 0.03711 0.00518 0.00030 0.00018 0.00018 0.00000 0.00141 0.00162 0.00156 0.00124 0.00115 0.00120 0.00063 H2A 0.45326 0.12380 0.14120 1.00000 0.05566 0.00000 0.00000 H2B 0.51926 0.21866 0.13963 1.00000 0.05566 0.00000 0.00000 H2C 0.56331 0.17521 0.22200 1.00000 0.05566 0.00000 0.00000 C3 0.65264 0.10797 0.02417 1.00000 0.04472 0.03667 0.02948 0.00539 -0.00565 -0.01652 0.03801 0.00478 0.00034 0.00018 0.00016 0.00000 0.00163 0.00156 0.00140 0.00115 0.00116 0.00127 0.00065 H3A 0.55980 0.06881 0.00842 1.00000 0.05702 0.00000 0.00000 H3B 0.74313 0.08117 -0.00060 1.00000 0.05702 0.00000 0.00000 H3C 0.63171 0.16130 0.00238 1.00000 0.05702 0.00000 0.00000 C4 0.73128 0.04390 0.15309 1.00000 0.04550 0.02638 0.03859 0.00845 -0.00343 -0.01169 0.03731 0.00505 0.00034 0.00017 0.00017 0.00000 0.00166 0.00140 0.00151 0.00114 0.00122 0.00121 0.00064 H4A 0.75403 0.05490 0.21544 1.00000 0.05597 0.00000 0.00000 H4B 0.82431 0.02107 0.12783 1.00000 0.05597 0.00000 0.00000 H4C 0.64247 0.00217 0.13599 1.00000 0.05597 0.00000 0.00000 C5 1.09884 0.13925 0.27704 1.00000 0.02520 0.01968 0.02587 0.00461 0.00416 -0.00409 0.02348 0.00434 0.00027 0.00014 0.00014 0.00000 0.00123 0.00119 0.00122 0.00094 0.00095 0.00096 0.00050 C6 1.15695 0.07800 0.21680 1.00000 0.02704 0.02524 0.02382 0.00433 0.00352 -0.00194 0.02535 0.00450 0.00028 0.00015 0.00015 0.00000 0.00126 0.00127 0.00123 0.00096 0.00095 0.00101 0.00051 C7 1.25856 0.01584 0.23607 1.00000 0.02950 0.02089 0.03320 -0.00238 0.01010 0.00102 0.02820 0.00467 0.00029 0.00015 0.00016 0.00000 0.00133 0.00126 0.00138 0.00101 0.00105 0.00103 0.00055 C8 1.30562 0.01023 0.31951 1.00000 0.02852 0.01837 0.04105 0.00927 0.00522 0.00372 0.02870 0.00487 0.00029 0.00015 0.00016 0.00000 0.00132 0.00122 0.00148 0.00105 0.00108 0.00102 0.00055 C9 1.25347 0.06889 0.38255 1.00000 0.02767 0.02501 0.02795 0.01103 0.00121 -0.00228 0.02632 0.00460 0.00028 0.00015 0.00015 0.00000 0.00130 0.00129 0.00129 0.00101 0.00100 0.00104 0.00053 C10 1.15755 0.13174 0.36028 1.00000 0.02367 0.02140 0.02487 0.00291 0.00597 -0.00012 0.02321 0.00440 0.00027 0.00015 0.00014 0.00000 0.00121 0.00121 0.00121 0.00094 0.00093 0.00096 0.00050 C11 1.10630 0.30360 0.27369 1.00000 0.02346 0.02132 0.02237 0.00652 0.00100 0.00326 0.02215 0.00437 0.00027 0.00014 0.00014 0.00000 0.00119 0.00119 0.00116 0.00091 0.00091 0.00094 0.00048 C12 1.19378 0.31833 0.20874 1.00000 0.02549 0.02318 0.02639 0.00297 0.00072 -0.00282 0.02540 0.00440 0.00027 0.00015 0.00015 0.00000 0.00125 0.00125 0.00125 0.00097 0.00096 0.00100 0.00052 C13 1.29238 0.38888 0.21252 1.00000 0.02497 0.03245 0.03205 0.01072 0.00346 -0.00392 0.02928 0.00482 0.00028 0.00016 0.00016 0.00000 0.00128 0.00142 0.00136 0.00110 0.00102 0.00107 0.00055 C14 1.31369 0.44869 0.28608 1.00000 0.02645 0.02038 0.04009 0.00919 -0.00477 -0.00800 0.02930 0.00455 0.00028 0.00015 0.00016 0.00000 0.00130 0.00126 0.00146 0.00107 0.00107 0.00102 0.00056 C15 1.23758 0.43585 0.35426 1.00000 0.02804 0.02027 0.02822 0.00199 -0.00583 -0.00137 0.02650 0.00436 0.00028 0.00015 0.00015 0.00000 0.00130 0.00123 0.00128 0.00097 0.00100 0.00100 0.00053 C16 1.13850 0.36484 0.34723 1.00000 0.02468 0.02401 0.02226 0.00705 0.00068 0.00183 0.02344 0.00443 0.00027 0.00015 0.00014 0.00000 0.00122 0.00125 0.00118 0.00094 0.00092 0.00098 0.00050 C17 0.84405 0.23242 0.32540 1.00000 0.02141 0.02225 0.02003 0.00290 -0.00210 -0.00298 0.02172 0.00413 0.00026 0.00014 0.00014 0.00000 0.00116 0.00121 0.00113 0.00091 0.00089 0.00094 0.00048 C18 0.76608 0.30879 0.33977 1.00000 0.02556 0.02511 0.02337 0.00487 -0.00027 -0.00109 0.02487 0.00442 0.00027 0.00015 0.00014 0.00000 0.00125 0.00128 0.00120 0.00097 0.00094 0.00101 0.00051 C19 0.64025 0.32136 0.38661 1.00000 0.02490 0.03152 0.02859 0.00082 0.00003 0.00474 0.02904 0.00470 0.00028 0.00016 0.00015 0.00000 0.00128 0.00141 0.00129 0.00105 0.00100 0.00107 0.00055 C20 0.58151 0.25532 0.42050 1.00000 0.02161 0.04502 0.02423 0.00087 0.00360 -0.00062 0.03084 0.00475 0.00028 0.00018 0.00015 0.00000 0.00125 0.00161 0.00126 0.00111 0.00098 0.00113 0.00058 C21 0.65413 0.17890 0.40979 1.00000 0.02575 0.03731 0.02388 0.00902 0.00183 -0.00874 0.02876 0.00462 0.00028 0.00017 0.00015 0.00000 0.00128 0.00149 0.00124 0.00106 0.00098 0.00111 0.00056 C22 0.78198 0.16918 0.36374 1.00000 0.02490 0.02514 0.02552 0.00505 0.00002 0.00096 0.02533 0.00449 0.00027 0.00015 0.00015 0.00000 0.00125 0.00129 0.00123 0.00098 0.00096 0.00101 0.00052 C31 0.56369 0.69610 0.32224 1.00000 0.02690 0.02662 0.03638 0.00511 0.00440 0.00186 0.02994 0.00482 0.00029 0.00016 0.00017 0.00000 0.00132 0.00134 0.00141 0.00107 0.00106 0.00106 0.00056 H31A 0.50179 0.67414 0.36328 1.00000 0.03593 0.00000 0.00000 H31B 0.49325 0.69594 0.26871 1.00000 0.03593 0.00000 0.00000 C32 0.62397 0.78591 0.35839 1.00000 0.02957 0.02716 0.03842 0.00712 0.00797 0.00381 0.03120 0.00503 0.00030 0.00016 0.00017 0.00000 0.00136 0.00136 0.00146 0.00109 0.00110 0.00108 0.00057 H32A 0.53503 0.82386 0.36880 1.00000 0.03744 0.00000 0.00000 H32B 0.69153 0.78731 0.41309 1.00000 0.03744 0.00000 0.00000 C33 0.80372 0.89047 0.32879 1.00000 0.04626 0.01860 0.03391 0.00616 0.00599 -0.00396 0.03270 0.00485 0.00032 0.00015 0.00017 0.00000 0.00160 0.00126 0.00141 0.00104 0.00117 0.00112 0.00059 H33A 0.74131 0.93050 0.36493 1.00000 0.03924 0.00000 0.00000 H33B 0.82849 0.91788 0.28040 1.00000 0.03924 0.00000 0.00000 C34 0.95378 0.87413 0.38006 1.00000 0.04185 0.02732 0.02962 -0.00006 0.00759 -0.01029 0.03341 0.00487 0.00031 0.00017 0.00016 0.00000 0.00155 0.00137 0.00135 0.00105 0.00113 0.00115 0.00060 H34A 1.01830 0.92798 0.39891 1.00000 0.04009 0.00000 0.00000 H34B 0.93104 0.85074 0.43119 1.00000 0.04009 0.00000 0.00000 C35 1.15695 0.77225 0.37015 1.00000 0.03008 0.04967 0.03138 0.00645 -0.00246 -0.00602 0.03767 0.00518 0.00031 0.00019 0.00017 0.00000 0.00143 0.00175 0.00143 0.00123 0.00110 0.00126 0.00064 H35A 1.21280 0.81426 0.41746 1.00000 0.04521 0.00000 0.00000 H35B 1.23418 0.75106 0.33057 1.00000 0.04521 0.00000 0.00000 C36 1.09290 0.69861 0.40551 1.00000 0.03254 0.04230 0.02984 0.00487 -0.00346 -0.00137 0.03564 0.00486 0.00032 0.00018 0.00016 0.00000 0.00144 0.00163 0.00139 0.00118 0.00109 0.00121 0.00062 H36A 1.17975 0.66981 0.43429 1.00000 0.04276 0.00000 0.00000 H36B 1.01943 0.71911 0.44751 1.00000 0.04276 0.00000 0.00000 C37 0.91522 0.57628 0.35927 1.00000 0.03637 0.02771 0.03401 0.01083 0.00430 0.00588 0.03198 0.00522 0.00030 0.00016 0.00017 0.00000 0.00146 0.00138 0.00139 0.00109 0.00111 0.00113 0.00058 H37A 0.96907 0.55656 0.41012 1.00000 0.03837 0.00000 0.00000 H37B 0.89897 0.52652 0.31220 1.00000 0.03837 0.00000 0.00000 C38 0.75925 0.61024 0.37887 1.00000 0.03434 0.02700 0.03132 0.01108 0.00609 0.00278 0.02999 0.00509 0.00030 0.00016 0.00016 0.00000 0.00142 0.00135 0.00135 0.00106 0.00107 0.00109 0.00056 H38A 0.69033 0.56420 0.39155 1.00000 0.03598 0.00000 0.00000 H38B 0.77314 0.65690 0.42905 1.00000 0.03598 0.00000 0.00000 B1 0.79297 0.31596 0.10980 1.00000 0.03578 0.02938 0.03314 0.01172 -0.00285 -0.00316 0.03261 0.00603 0.00038 0.00020 0.00020 0.00000 0.00170 0.00161 0.00164 0.00126 0.00131 0.00134 0.00067 B2 0.98459 0.21926 0.26187 1.00000 0.02570 0.01930 0.02071 0.00476 0.00225 -0.00181 0.02183 0.00498 0.00031 0.00017 0.00016 0.00000 0.00139 0.00133 0.00129 0.00101 0.00103 0.00107 0.00055 O5 0.69111 0.64174 0.30534 1.00000 0.02993 0.02176 0.02849 0.00637 0.00212 0.00343 0.02655 0.00309 0.00019 0.00010 0.00010 0.00000 0.00092 0.00087 0.00090 0.00069 0.00070 0.00070 0.00037 O6 0.71272 0.81330 0.29684 1.00000 0.03651 0.02185 0.03081 0.00635 0.00313 -0.00514 0.02966 0.00314 0.00020 0.00010 0.00010 0.00000 0.00100 0.00089 0.00092 0.00071 0.00074 0.00074 0.00039 O7 1.03551 0.81368 0.32597 1.00000 0.03691 0.04090 0.02531 0.00425 0.00588 0.00082 0.03438 0.00338 0.00021 0.00012 0.00010 0.00000 0.00103 0.00109 0.00091 0.00077 0.00075 0.00083 0.00042 O8 1.01237 0.64081 0.33519 1.00000 0.03048 0.03591 0.02594 0.00227 0.00341 -0.00283 0.03119 0.00319 0.00020 0.00011 0.00010 0.00000 0.00094 0.00102 0.00090 0.00074 0.00071 0.00077 0.00040 F1 1.11709 0.07583 0.13187 1.00000 0.04215 0.03638 0.02403 -0.00007 0.00415 0.00664 0.03472 0.00273 0.00017 0.00009 0.00008 0.00000 0.00087 0.00085 0.00075 0.00061 0.00062 0.00068 0.00035 F2 1.31140 -0.03984 0.17312 1.00000 0.04361 0.02864 0.04194 -0.00394 0.01179 0.00868 0.03862 0.00290 0.00018 0.00009 0.00009 0.00000 0.00091 0.00081 0.00088 0.00066 0.00070 0.00068 0.00037 F3 1.40127 -0.05146 0.33906 1.00000 0.04340 0.03075 0.05507 0.01287 0.00636 0.01460 0.04220 0.00316 0.00018 0.00010 0.00010 0.00000 0.00093 0.00085 0.00100 0.00072 0.00075 0.00071 0.00039 F4 1.29470 0.06350 0.46506 1.00000 0.03614 0.03742 0.03132 0.01416 0.00179 0.00801 0.03407 0.00283 0.00017 0.00009 0.00009 0.00000 0.00083 0.00086 0.00079 0.00064 0.00062 0.00067 0.00035 F5 1.11640 0.18901 0.42637 1.00000 0.03261 0.02717 0.02280 0.00272 0.00365 0.00580 0.02762 0.00252 0.00016 0.00008 0.00008 0.00000 0.00077 0.00074 0.00069 0.00056 0.00056 0.00060 0.00031 F6 1.18270 0.26119 0.13481 1.00000 0.03290 0.03473 0.02857 -0.00049 0.00914 -0.00774 0.03246 0.00261 0.00016 0.00009 0.00009 0.00000 0.00079 0.00082 0.00075 0.00061 0.00059 0.00064 0.00034 F7 1.36480 0.40045 0.14480 1.00000 0.03986 0.04818 0.04018 0.01225 0.01048 -0.01740 0.04202 0.00294 0.00018 0.00010 0.00010 0.00000 0.00089 0.00099 0.00088 0.00073 0.00069 0.00074 0.00039 F8 1.40889 0.51816 0.29109 1.00000 0.04015 0.02941 0.05602 0.01056 -0.00302 -0.01765 0.04241 0.00282 0.00018 0.00009 0.00010 0.00000 0.00090 0.00084 0.00101 0.00072 0.00073 0.00069 0.00040 F9 1.26179 0.49257 0.42761 1.00000 0.03985 0.02608 0.03734 -0.00374 -0.00546 -0.00482 0.03636 0.00257 0.00017 0.00009 0.00009 0.00000 0.00087 0.00079 0.00084 0.00063 0.00065 0.00065 0.00036 F10 1.06942 0.35854 0.41806 1.00000 0.03631 0.02847 0.02179 0.00265 0.00210 -0.00320 0.02921 0.00251 0.00016 0.00009 0.00008 0.00000 0.00080 0.00076 0.00070 0.00056 0.00057 0.00061 0.00032 F11 0.81380 0.37751 0.30876 1.00000 0.03414 0.02336 0.03636 0.01024 0.00407 0.00453 0.03065 0.00270 0.00016 0.00009 0.00009 0.00000 0.00079 0.00074 0.00080 0.00060 0.00061 0.00061 0.00033 F12 0.57592 0.39852 0.40014 1.00000 0.03360 0.04031 0.04121 -0.00108 0.00337 0.01304 0.03924 0.00291 0.00017 0.00010 0.00010 0.00000 0.00083 0.00091 0.00088 0.00069 0.00066 0.00070 0.00038 F13 0.45748 0.26608 0.46572 1.00000 0.03299 0.06379 0.04049 0.00388 0.01618 0.00142 0.04545 0.00314 0.00018 0.00011 0.00010 0.00000 0.00086 0.00113 0.00091 0.00078 0.00070 0.00078 0.00042 F14 0.60240 0.11307 0.44446 1.00000 0.03722 0.04688 0.03671 0.01453 0.00846 -0.01275 0.03930 0.00289 0.00017 0.00010 0.00009 0.00000 0.00086 0.00095 0.00084 0.00071 0.00066 0.00072 0.00038 F15 0.84553 0.09110 0.35867 1.00000 0.03271 0.02347 0.03721 0.01022 0.00734 -0.00157 0.03034 0.00266 0.00016 0.00008 0.00009 0.00000 0.00078 0.00074 0.00080 0.00061 0.00061 0.00060 0.00033 P1 0.85727 0.20884 0.14467 1.00000 0.02609 0.02266 0.02292 0.00544 0.00133 -0.00412 0.02390 0.00116 0.00007 0.00004 0.00004 0.00000 0.00033 0.00033 0.00031 0.00024 0.00024 0.00025 0.00015 C23 0.62257 0.58302 0.10075 1.00000 0.04671 0.03761 0.04815 -0.01073 -0.00132 -0.00921 0.04696 0.00530 0.00036 0.00019 0.00020 0.00000 0.00179 0.00169 0.00178 0.00134 0.00137 0.00138 0.00076 H23A 0.54757 0.56997 0.04803 1.00000 0.05635 0.00000 0.00000 H23B 0.57705 0.55779 0.14561 1.00000 0.05635 0.00000 0.00000 C24 0.77256 0.54214 0.08463 1.00000 0.06959 0.02865 0.04118 0.00149 -0.01081 -0.00144 0.04838 0.00549 0.00039 0.00019 0.00019 0.00000 0.00218 0.00154 0.00169 0.00125 0.00148 0.00145 0.00078 H24A 0.75756 0.47900 0.07489 1.00000 0.05805 0.00000 0.00000 H24B 0.81113 0.55896 0.03349 1.00000 0.05805 0.00000 0.00000 C25 1.04272 0.55192 0.14450 1.00000 0.05654 0.03931 0.04659 0.00330 0.02164 0.00786 0.04668 0.00637 0.00037 0.00019 0.00020 0.00000 0.00196 0.00171 0.00176 0.00134 0.00146 0.00146 0.00075 H25A 1.04444 0.49846 0.10250 1.00000 0.05602 0.00000 0.00000 H25B 1.10150 0.54282 0.19894 1.00000 0.05602 0.00000 0.00000 C26 1.12031 0.62174 0.11360 1.00000 0.05310 0.03906 0.05344 -0.00056 0.01538 0.00306 0.04882 0.00616 0.00039 0.00019 0.00021 0.00000 0.00191 0.00173 0.00190 0.00141 0.00150 0.00144 0.00077 H26A 1.23339 0.61064 0.11096 1.00000 0.05858 0.00000 0.00000 H26B 1.07136 0.62635 0.05558 1.00000 0.05858 0.00000 0.00000 C27 1.13149 0.77519 0.13882 1.00000 0.06898 0.04592 0.05398 0.01370 0.02564 -0.01158 0.05448 0.00679 0.00042 0.00021 0.00021 0.00000 0.00231 0.00190 0.00198 0.00154 0.00172 0.00166 0.00087 H27A 1.21783 0.76626 0.10222 1.00000 0.06537 0.00000 0.00000 H27B 1.16588 0.82221 0.18689 1.00000 0.06537 0.00000 0.00000 C28 0.99148 0.79999 0.08921 1.00000 0.07767 0.05364 0.04595 0.02219 0.01611 -0.01071 0.05700 0.00707 0.00043 0.00023 0.00021 0.00000 0.00247 0.00206 0.00187 0.00157 0.00171 0.00178 0.00089 H28A 1.01235 0.85605 0.07232 1.00000 0.06840 0.00000 0.00000 H28B 0.96500 0.75702 0.03664 1.00000 0.06840 0.00000 0.00000 C29 0.71437 0.80420 0.08971 1.00000 0.06791 0.03636 0.04626 0.01507 -0.01162 0.00552 0.05060 0.00585 0.00040 0.00019 0.00020 0.00000 0.00220 0.00172 0.00179 0.00138 0.00154 0.00152 0.00081 H29A 0.72574 0.83461 0.04142 1.00000 0.06072 0.00000 0.00000 H29B 0.63875 0.83531 0.12500 1.00000 0.06072 0.00000 0.00000 C30 0.65020 0.71659 0.05590 1.00000 0.07626 0.04665 0.04240 0.01429 -0.01638 0.00343 0.05610 0.00617 0.00044 0.00020 0.00020 0.00000 0.00238 0.00194 0.00178 0.00146 0.00160 0.00170 0.00089 H30A 0.54488 0.71842 0.02360 1.00000 0.06732 0.00000 0.00000 H30B 0.72060 0.68582 0.01701 1.00000 0.06732 0.00000 0.00000 O1 0.63883 0.67380 0.12686 1.00000 0.05198 0.02946 0.03119 0.00478 -0.00565 -0.00043 0.03843 0.00340 0.00023 0.00011 0.00011 0.00000 0.00119 0.00101 0.00099 0.00078 0.00084 0.00086 0.00045 O2 0.88196 0.57029 0.15761 1.00000 0.03989 0.03073 0.02639 0.00321 0.00377 0.00183 0.03254 0.00329 0.00021 0.00011 0.00010 0.00000 0.00104 0.00098 0.00091 0.00073 0.00075 0.00080 0.00041 O3 1.10320 0.69940 0.17131 1.00000 0.05867 0.03322 0.02994 0.00303 0.01554 -0.00732 0.04023 0.00360 0.00024 0.00012 0.00011 0.00000 0.00127 0.00106 0.00099 0.00079 0.00087 0.00091 0.00047 O4 0.86161 0.80576 0.13941 1.00000 0.05850 0.04051 0.02705 0.00535 0.00413 -0.00515 0.04224 0.00362 0.00024 0.00012 0.00011 0.00000 0.00130 0.00114 0.00098 0.00082 0.00088 0.00096 0.00048 Final Structure Factor Calculation for 2005src0633 in P-1 Total number of l.s. parameters = 606 Maximum vector length = 511 Memory required = 6380 / 26061 wR2 = 0.1270 before cycle 5 for 9718 data and 0 / 606 parameters GooF = S = 1.017; Restrained GooF = 1.017 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0448 * P )^2 + 1.80 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0577 for 6586 Fo > 4sig(Fo) and 0.1019 for all 9718 data wR2 = 0.1270, GooF = S = 1.017, Restrained GooF = 1.017 for all data Occupancy sum of asymmetric unit = 65.00 for non-hydrogen and 45.00 for hydrogen atoms Principal mean square atomic displacements U 0.0410 0.0334 0.0313 Li1 0.0401 0.0265 0.0195 C1 0.0477 0.0401 0.0235 C2 0.0617 0.0314 0.0210 C3 0.0568 0.0351 0.0200 C4 0.0286 0.0256 0.0162 C5 0.0294 0.0241 0.0225 C6 0.0406 0.0263 0.0177 C7 0.0413 0.0286 0.0163 C8 0.0346 0.0262 0.0181 C9 0.0278 0.0213 0.0205 C10 0.0251 0.0242 0.0172 C11 0.0290 0.0270 0.0202 C12 0.0381 0.0289 0.0208 C13 0.0469 0.0268 0.0142 C14 0.0386 0.0230 0.0180 C15 0.0265 0.0252 0.0186 C16 0.0271 0.0223 0.0158 C17 0.0291 0.0240 0.0215 C18 0.0381 0.0261 0.0229 C19 0.0475 0.0239 0.0212 C20 0.0439 0.0235 0.0188 C21 0.0286 0.0251 0.0223 C22 0.0365 0.0274 0.0259 C31 0.0396 0.0287 0.0253 C32 0.0475 0.0337 0.0170 C33 0.0506 0.0284 0.0212 C34 0.0526 0.0357 0.0247 C35 0.0432 0.0391 0.0246 C36 0.0387 0.0348 0.0224 C37 0.0366 0.0319 0.0214 C38 0.0452 0.0293 0.0233 B1 0.0269 0.0210 0.0175 B2 0.0311 0.0285 0.0200 O5 0.0393 0.0308 0.0189 O6 0.0417 0.0369 0.0246 O7 0.0393 0.0288 0.0255 O8 0.0462 0.0356 0.0224 F1 0.0502 0.0457 0.0199 F2 0.0558 0.0499 0.0209 F3 0.0439 0.0366 0.0217 F4 0.0354 0.0256 0.0219 F5 0.0477 0.0261 0.0236 F6 0.0645 0.0430 0.0186 F7 0.0644 0.0474 0.0154 F8 0.0507 0.0392 0.0191 F9 0.0386 0.0275 0.0215 F10 0.0375 0.0346 0.0199 F11 0.0560 0.0381 0.0236 F12 0.0665 0.0472 0.0227 F13 0.0582 0.0401 0.0196 F14 0.0388 0.0329 0.0193 F15 0.0305 0.0225 0.0188 P1 0.0656 0.0527 0.0227 C23 0.0801 0.0381 0.0269 C24 0.0663 0.0442 0.0295 C25 0.0641 0.0480 0.0343 C26 0.0837 0.0535 0.0263 C27 0.0844 0.0610 0.0257 C28 0.0808 0.0449 0.0261 C29 0.0912 0.0487 0.0284 C30 0.0578 0.0298 0.0277 O1 0.0400 0.0317 0.0260 O2 0.0651 0.0309 0.0247 O3 0.0613 0.0384 0.0270 O4 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.006 0.012 0.018 0.025 0.033 0.041 0.054 0.071 0.107 1.000 Number in group 1013. 1014. 962. 1009. 968. 860. 1038. 925. 967. 962. GooF 1.032 0.992 1.002 1.000 1.035 1.022 1.062 0.995 0.994 1.031 K 13.125 3.106 1.517 1.186 1.067 1.090 0.996 1.001 1.005 1.012 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.64 inf Number in group 982. 960. 978. 994. 967. 946. 971. 970. 982. 968. GooF 0.963 0.961 0.999 0.985 1.019 0.919 0.932 0.891 1.021 1.392 K 1.338 1.138 1.102 1.092 1.019 1.028 1.011 1.026 1.017 1.005 R1 0.336 0.273 0.209 0.176 0.125 0.083 0.059 0.050 0.042 0.035 Recommended weighting scheme: WGHT 0.0446 1.8056 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 -4 17 934.30 1441.26 5.91 0.136 0.93 -2 -1 3 302.18 188.13 4.96 0.049 3.48 1 -1 2 898.23 1352.71 4.94 0.131 5.39 -3 1 7 211.50 129.32 4.36 0.041 1.83 -2 -1 2 407.67 578.12 4.36 0.086 3.85 -3 4 1 79.96 152.36 4.34 0.044 2.31 -3 -15 6 101.01 0.11 4.24 0.001 0.97 -2 -8 1 372.52 252.81 4.09 0.057 1.78 0 -9 5 83.45 34.06 3.98 0.021 1.64 -1 3 1 320.01 223.36 3.92 0.053 4.24 1 -7 5 1061.72 1351.74 3.84 0.131 1.92 -2 7 1 124.77 70.68 3.79 0.030 1.97 1 2 4 300.14 205.51 3.71 0.051 2.95 -1 12 11 1417.22 75.54 3.68 0.031 0.89 -2 -3 7 311.51 429.25 3.65 0.074 2.03 3 4 3 413.59 553.99 3.63 0.084 1.93 -9 -6 9 143.15 39.88 3.58 0.023 0.84 4 -4 1 136.63 212.52 3.54 0.052 1.88 2 -1 3 1057.31 1321.87 3.54 0.130 3.14 -2 3 7 25.35 3.12 3.50 0.006 1.85 -2 -8 5 58.80 115.36 3.47 0.038 1.68 -1 4 4 477.03 361.82 3.47 0.068 2.52 -2 4 7 1085.27 877.17 3.45 0.106 1.74 6 -10 12 896.93 11.15 3.40 0.012 0.84 3 6 2 21.76 0.20 3.40 0.002 1.75 2 -6 6 255.00 176.08 3.39 0.047 1.79 -4 -4 4 26.77 0.58 3.36 0.003 1.79 -3 -16 7 85.11 14.28 3.36 0.013 0.91 4 3 1 632.02 798.19 3.31 0.101 1.88 1 7 13 172.89 251.82 3.29 0.057 0.97 5 12 5 265.65 41.86 3.26 0.023 0.91 -1 2 1 365.27 274.06 3.25 0.059 5.40 -3 -1 5 1343.51 1110.81 3.23 0.119 2.24 2 0 15 151.68 288.31 3.21 0.061 0.99 -4 -5 5 269.35 194.10 3.19 0.050 1.65 2 -4 9 21.43 0.10 3.19 0.001 1.53 -5 -13 10 134.92 16.46 3.19 0.014 0.91 0 -8 5 169.29 103.38 3.17 0.036 1.80 5 -10 16 239.52 17.99 3.17 0.015 0.77 0 -6 14 576.66 0.00 3.16 0.000 1.10 -2 8 2 124.96 77.05 3.14 0.031 1.71 -6 2 10 303.52 410.99 3.13 0.072 1.09 0 -6 6 754.28 938.73 3.13 0.109 2.03 -2 -15 12 243.47 361.63 3.12 0.068 0.88 7 -11 7 21.71 109.67 3.10 0.037 0.87 2 -8 1 434.22 331.29 3.10 0.065 1.81 0 3 0 21.53 56.79 3.09 0.027 5.20 -1 -3 3 25.24 5.85 3.08 0.009 3.74 -2 5 9 37.71 13.15 3.08 0.013 1.39 6 11 6 306.25 0.54 3.07 0.003 0.86 Bond lengths and angles Li1 - Distance Angles O2 2.2682 (0.0047) O5 2.2911 (0.0047) 85.41 (0.16) O6 2.3450 (0.0047) 150.85 (0.22) 72.73 (0.14) O8 2.3534 (0.0048) 79.48 (0.16) 72.11 (0.14) 110.55 (0.18) O4 2.3594 (0.0049) 110.33 (0.19) 139.06 (0.22) 77.13 (0.15) 146.10 (0.22) O3 2.3630 (0.0049) 71.96 (0.14) 148.42 (0.22) 135.19 (0.21) 82.10 (0.16) 71.23 (0.14) O1 2.3823 (0.0048) 71.75 (0.14) 78.95 (0.15) 85.05 (0.16) 140.45 (0.21) 71.36 (0.14) 112.81 (0.18) O7 2.4453 (0.0048) 137.85 (0.22) 111.58 (0.18) 69.90 (0.13) 70.58 (0.14) 82.36 (0.15) 75.08 (0.14) 147.20 (0.21) Li1 - O2 O5 O6 O8 O4 O3 O1 C1 - Distance Angles C2 1.5304 (0.0036) C4 1.5335 (0.0036) 110.75 (0.22) C3 1.5355 (0.0034) 108.69 (0.22) 108.03 (0.21) P1 1.8707 (0.0025) 110.82 (0.17) 112.53 (0.17) 105.80 (0.17) C1 - C2 C4 C3 C2 - Distance Angles C1 1.5304 (0.0036) H2A 0.9800 109.47 H2B 0.9800 109.47 109.47 H2C 0.9800 109.47 109.47 109.47 C2 - C1 H2A H2B C3 - Distance Angles C1 1.5355 (0.0034) H3A 0.9800 109.47 H3B 0.9800 109.47 109.47 H3C 0.9800 109.47 109.47 109.47 C3 - C1 H3A H3B C4 - Distance Angles C1 1.5335 (0.0036) H4A 0.9800 109.47 H4B 0.9800 109.47 109.47 H4C 0.9800 109.47 109.47 109.47 C4 - C1 H4A H4B C5 - Distance Angles C6 1.3885 (0.0032) C10 1.3955 (0.0032) 112.09 (0.21) B2 1.6499 (0.0035) 128.90 (0.20) 118.87 (0.20) C5 - C6 C10 C6 - Distance Angles F1 1.3584 (0.0027) C7 1.3776 (0.0035) 114.25 (0.20) C5 1.3885 (0.0032) 121.23 (0.21) 124.52 (0.22) C6 - F1 C7 C7 - Distance Angles F2 1.3470 (0.0026) C8 1.3692 (0.0035) 119.74 (0.22) C6 1.3776 (0.0035) 120.29 (0.22) 119.97 (0.21) C7 - F2 C8 C8 - Distance Angles F3 1.3421 (0.0028) C7 1.3692 (0.0035) 120.51 (0.22) C9 1.3714 (0.0034) 120.74 (0.22) 118.75 (0.22) C8 - F3 C7 C9 - Distance Angles F4 1.3455 (0.0027) C10 1.3709 (0.0033) 120.86 (0.21) C8 1.3714 (0.0034) 119.94 (0.21) 119.19 (0.22) C9 - F4 C10 C10 - Distance Angles F5 1.3554 (0.0025) C9 1.3709 (0.0033) 115.40 (0.20) C5 1.3955 (0.0032) 119.24 (0.20) 125.35 (0.21) C10 - F5 C9 C11 - Distance Angles C16 1.3903 (0.0032) C12 1.3938 (0.0032) 112.75 (0.21) B2 1.6488 (0.0034) 125.72 (0.20) 121.49 (0.19) C11 - C16 C12 C12 - Distance Angles F6 1.3556 (0.0026) C13 1.3753 (0.0034) 115.46 (0.20) C11 1.3938 (0.0032) 119.73 (0.20) 124.80 (0.22) C12 - F6 C13 C13 - Distance Angles F7 1.3431 (0.0027) C14 1.3729 (0.0035) 120.07 (0.22) C12 1.3753 (0.0034) 120.76 (0.22) 119.15 (0.22) C13 - F7 C14 C14 - Distance Angles F8 1.3415 (0.0027) C15 1.3724 (0.0035) 120.76 (0.22) C13 1.3729 (0.0035) 120.17 (0.23) 119.06 (0.22) C14 - F8 C15 C15 - Distance Angles F9 1.3452 (0.0027) C14 1.3724 (0.0035) 119.55 (0.21) C16 1.3761 (0.0033) 120.67 (0.21) 119.77 (0.21) C15 - F9 C14 C16 - Distance Angles F10 1.3523 (0.0026) C15 1.3761 (0.0033) 114.89 (0.20) C11 1.3903 (0.0032) 120.83 (0.20) 124.27 (0.21) C16 - F10 C15 C17 - Distance Angles C22 1.3864 (0.0033) C18 1.3909 (0.0033) 112.79 (0.21) B2 1.6526 (0.0034) 125.27 (0.21) 121.73 (0.20) C17 - C22 C18 C18 - Distance Angles F11 1.3451 (0.0027) C19 1.3770 (0.0034) 115.13 (0.21) C17 1.3909 (0.0033) 120.49 (0.21) 124.37 (0.23) C18 - F11 C19 C19 - Distance Angles F12 1.3452 (0.0029) C20 1.3688 (0.0037) 119.79 (0.22) C18 1.3770 (0.0034) 120.34 (0.23) 119.87 (0.23) C19 - F12 C20 C20 - Distance Angles F13 1.3465 (0.0028) C21 1.3660 (0.0037) 120.51 (0.24) C19 1.3688 (0.0037) 120.75 (0.24) 118.71 (0.22) C20 - F13 C21 C21 - Distance Angles F14 1.3505 (0.0028) C20 1.3660 (0.0037) 120.40 (0.22) C22 1.3816 (0.0034) 119.86 (0.23) 119.74 (0.23) C21 - F14 C20 C22 - Distance Angles F15 1.3551 (0.0027) C21 1.3816 (0.0034) 114.32 (0.21) C17 1.3864 (0.0033) 121.20 (0.21) 124.48 (0.23) C22 - F15 C21 C31 - Distance Angles O5 1.4234 (0.0029) C32 1.5005 (0.0035) 110.56 (0.20) H31A 0.9900 109.54 109.54 H31B 0.9900 109.54 109.54 108.09 C31 - O5 C32 H31A C32 - Distance Angles O6 1.4257 (0.0029) C31 1.5005 (0.0035) 106.70 (0.20) H32A 0.9900 110.38 110.38 H32B 0.9900 110.38 110.38 108.60 C32 - O6 C31 H32A C33 - Distance Angles O6 1.4223 (0.0029) C34 1.4950 (0.0038) 111.52 (0.20) H33A 0.9900 109.32 109.32 H33B 0.9900 109.32 109.32 107.97 C33 - O6 C34 H33A C34 - Distance Angles O7 1.4271 (0.0030) C33 1.4950 (0.0038) 106.82 (0.20) H34A 0.9900 110.36 110.36 H34B 0.9900 110.36 110.36 108.59 C34 - O7 C33 H34A C35 - Distance Angles O7 1.4245 (0.0032) C36 1.4997 (0.0038) 111.89 (0.21) H35A 0.9900 109.24 109.24 H35B 0.9900 109.24 109.24 107.92 C35 - O7 C36 H35A C36 - Distance Angles O8 1.4253 (0.0030) C35 1.4997 (0.0038) 106.93 (0.20) H36A 0.9900 110.33 110.33 H36B 0.9900 110.33 110.33 108.57 C36 - O8 C35 H36A C37 - Distance Angles O8 1.4333 (0.0030) C38 1.4933 (0.0035) 110.90 (0.20) H37A 0.9900 109.46 109.46 H37B 0.9900 109.46 109.46 108.05 C37 - O8 C38 H37A C38 - Distance Angles O5 1.4250 (0.0029) C37 1.4933 (0.0035) 106.99 (0.19) H38A 0.9900 110.32 110.32 H38B 0.9900 110.32 110.32 108.57 C38 - O5 C37 H38A B1 - Distance Angles P1 1.9461 (0.0031) H1B 1.1496 (0.0256) 105.70 (1.29) H3B 1.1121 (0.0279) 102.24 (1.41) 115.23 (1.87) H2B 1.1128 (0.0262) 109.44 (1.37) 109.08 (1.83) 114.46 (1.93) B1 - P1 H1B H3B B2 - Distance Angles C11 1.6488 (0.0034) C5 1.6499 (0.0035) 104.85 (0.18) C17 1.6526 (0.0034) 113.33 (0.19) 113.65 (0.19) P1 2.0398 (0.0027) 107.36 (0.15) 116.37 (0.16) 101.43 (0.15) B2 - C11 C5 C17 O5 - Distance Angles C31 1.4234 (0.0029) C38 1.4250 (0.0029) 112.94 (0.18) Li1 2.2911 (0.0047) 110.22 (0.18) 116.17 (0.18) O5 - C31 C38 O6 - Distance Angles C33 1.4223 (0.0029) C32 1.4257 (0.0029) 113.24 (0.19) Li1 2.3450 (0.0047) 112.43 (0.18) 112.58 (0.17) O6 - C33 C32 O7 - Distance Angles C35 1.4245 (0.0032) C34 1.4271 (0.0030) 114.26 (0.19) Li1 2.4453 (0.0048) 108.63 (0.19) 113.83 (0.18) O7 - C35 C34 O8 - Distance Angles C36 1.4253 (0.0030) C37 1.4333 (0.0030) 114.13 (0.19) Li1 2.3534 (0.0049) 115.82 (0.18) 108.44 (0.18) O8 - C36 C37 F1 - Distance Angles C6 1.3584 (0.0027) F1 - F2 - Distance Angles C7 1.3470 (0.0026) F2 - F3 - Distance Angles C8 1.3421 (0.0028) F3 - F4 - Distance Angles C9 1.3455 (0.0027) F4 - F5 - Distance Angles C10 1.3554 (0.0025) F5 - F6 - Distance Angles C12 1.3556 (0.0026) F6 - F7 - Distance Angles C13 1.3431 (0.0027) F7 - F8 - Distance Angles C14 1.3415 (0.0027) F8 - F9 - Distance Angles C15 1.3452 (0.0027) F9 - F10 - Distance Angles C16 1.3523 (0.0026) F10 - F11 - Distance Angles C18 1.3451 (0.0027) F11 - F12 - Distance Angles C19 1.3452 (0.0029) F12 - F13 - Distance Angles C20 1.3465 (0.0028) F13 - F14 - Distance Angles C21 1.3505 (0.0028) F14 - F15 - Distance Angles C22 1.3551 (0.0027) F15 - P1 - Distance Angles C1 1.8707 (0.0025) B1 1.9461 (0.0031) 110.61 (0.13) B2 2.0398 (0.0027) 115.87 (0.11) 116.00 (0.12) H1P 1.3229 (0.0230) 98.37 (1.02) 105.43 (1.03) 108.47 (1.02) P1 - C1 B1 B2 C23 - Distance Angles O1 1.4282 (0.0033) C24 1.4766 (0.0043) 113.62 (0.24) H23A 0.9900 108.84 108.84 H23B 0.9900 108.84 108.84 107.70 C23 - O1 C24 H23A C24 - Distance Angles O2 1.4142 (0.0033) C23 1.4766 (0.0043) 107.15 (0.23) H24A 0.9900 110.29 110.29 H24B 0.9900 110.29 110.29 108.54 C24 - O2 C23 H24A C25 - Distance Angles O2 1.4408 (0.0034) C26 1.4621 (0.0042) 111.49 (0.25) H25A 0.9900 109.33 109.33 H25B 0.9900 109.33 109.33 107.97 C25 - O2 C26 H25A C26 - Distance Angles O3 1.4289 (0.0033) C25 1.4621 (0.0042) 108.09 (0.24) H26A 0.9900 110.08 110.08 H26B 0.9900 110.08 110.08 108.42 C26 - O3 C25 H26A C27 - Distance Angles O3 1.4142 (0.0034) C28 1.4591 (0.0049) 111.95 (0.27) H27A 0.9900 109.22 109.22 H27B 0.9900 109.22 109.22 107.91 C27 - O3 C28 H27A C28 - Distance Angles O4 1.4366 (0.0037) C27 1.4591 (0.0049) 109.64 (0.25) H28A 0.9900 109.74 109.74 H28B 0.9900 109.74 109.74 108.21 C28 - O4 C27 H28A C29 - Distance Angles O4 1.4089 (0.0036) C30 1.4731 (0.0044) 112.82 (0.25) H29A 0.9900 109.02 109.02 H29B 0.9900 109.02 109.02 107.80 C29 - O4 C30 H29A C30 - Distance Angles O1 1.4290 (0.0035) C29 1.4731 (0.0044) 107.67 (0.25) H30A 0.9900 110.17 110.17 H30B 0.9900 110.17 110.17 108.47 C30 - O1 C29 H30A O1 - Distance Angles C23 1.4282 (0.0033) C30 1.4290 (0.0035) 111.62 (0.22) Li1 2.3823 (0.0049) 107.90 (0.19) 112.32 (0.21) O1 - C23 C30 O2 - Distance Angles C24 1.4142 (0.0033) C25 1.4408 (0.0034) 113.68 (0.22) Li1 2.2682 (0.0047) 118.41 (0.20) 111.63 (0.19) O2 - C24 C25 O3 - Distance Angles C27 1.4142 (0.0034) C26 1.4289 (0.0033) 114.80 (0.22) Li1 2.3630 (0.0049) 110.88 (0.21) 113.62 (0.20) O3 - C27 C26 O4 - Distance Angles C29 1.4089 (0.0036) C28 1.4366 (0.0037) 112.87 (0.24) Li1 2.3594 (0.0049) 110.96 (0.20) 113.83 (0.21) O4 - C29 C28 FMAP and GRID set by program FMAP 2 3 37 GRID -1.471 -2 -2 1.471 2 2 R1 = 0.1013 for 9718 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.73 at 0.5814 0.7608 0.0992 [ 1.12 A from C30 ] Deepest hole -0.31 at 0.9223 0.2375 0.1444 [ 0.71 A from P1 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 5836 / 35471 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5814 0.7608 0.0992 1.00000 0.05 0.73 1.12 C30 1.25 H29B 1.28 H30A 1.35 C29 Q2 1 0.7011 0.5414 0.1336 1.00000 0.05 0.63 1.05 C24 1.10 C23 1.13 H23B 1.38 H24A Q3 1 0.9606 0.5686 0.0958 1.00000 0.05 0.58 1.06 C25 1.25 O2 1.35 H25A 1.52 H24B Q4 1 1.0186 0.8459 0.1408 1.00000 0.05 0.51 1.01 C28 1.13 H28A 1.47 O4 1.47 H27B Q5 1 1.0717 0.7485 0.0863 1.00000 0.05 0.40 0.96 C27 1.07 C28 1.17 H28B 1.26 H27A Q6 1 0.6481 0.6166 0.0591 1.00000 0.05 0.35 0.96 C23 1.10 H23A 1.30 O1 1.53 H30B Q7 1 0.4951 0.5603 0.0591 1.00000 0.05 0.27 0.53 H23A 1.22 C23 1.49 H23B 2.21 O1 Q8 1 0.6202 0.2209 0.4281 1.00000 0.05 0.25 0.66 C20 0.76 C21 1.70 F13 1.78 F14 Q9 1 0.9207 0.2320 0.3196 1.00000 0.05 0.25 0.67 C17 1.12 B2 1.81 C22 1.83 C18 Q10 1 0.8182 0.2745 0.1318 1.00000 0.05 0.25 0.82 B1 1.14 P1 1.51 H3B 1.52 H2B Shortest distances between peaks (including symmetry equivalents) 6 7 1.57 4 5 1.73 2 6 1.85 2 7 2.07 1 6 2.37 2 3 2.41 7 7 2.46 3 6 2.82 Time profile in seconds ----------------------- 0.03: Read and process instructions 0.00: Fit rigid groups 0.01: Interpret restraints etc. 0.01: 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 0.01: Analyse other restraints etc. 2.66: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.00: Generate idealized H-atoms 5.96: Structure factors and derivatives 32.03: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.01: Apply other restraints 2.34: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.26: Analysis of variance 0.10: Merge reflections for Fourier and .fcf 0.10: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2005src0633 finished at 19:42:56 Total CPU time: 43.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++