+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008src0880 started at 11:40:59 on 17-Sep-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src0880 in P2(1)/c CELL 0.71073 12.7644 11.9584 29.2566 90.000 98.801 90.000 ZERR 4.00 0.0002 0.0002 0.0005 0.000 0.001 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H O F P CL AU UNIT 192 112 4 24 8 16 8 V = 4413.20 F(000) = 2536.0 Mu = 7.02 mm-1 Cell Wt = 5329.51 Rho = 2.005 MERG 2 OMIT -3.00 55.00 OMIT -4 9 18 OMIT -8 4 18 OMIT -12 1 22 OMIT -6 8 16 OMIT -4 13 8 OMIT -14 1 18 OMIT -10 2 20 OMIT -9 1 19 shel 7 0.77 FMAP 2 PLAN 5 bond $H SIZE 0.22 0.36 0.44 ACTA WGHT 0.02330 37.49390 L.S. 10 TEMP -153.00 FVAR 0.15112 AU1 7 0.001598 0.758503 0.604850 11.00000 0.01638 0.01616 = 0.01714 -0.00328 -0.00027 -0.00283 AU2 7 0.494836 0.633795 0.649652 11.00000 0.01748 0.01700 = 0.02370 0.00185 0.00288 -0.00296 MOLE 1 C1 1 0.226757 0.886908 0.574151 11.00000 0.02167 0.01617 = 0.01881 0.00688 0.00293 -0.00735 C2 1 0.276940 0.787761 0.564395 11.00000 0.02577 0.02645 = 0.01253 0.01016 -0.00370 0.00318 C3 1 0.344927 0.781448 0.531900 11.00000 0.03462 0.03276 = 0.02550 0.00826 0.01176 0.01882 AFIX 43 H3 2 0.376463 0.712339 0.525547 11.00000 -1.20000 AFIX 0 C4 1 0.365914 0.877738 0.508927 11.00000 0.03408 0.05152 = 0.02393 0.00876 0.00646 0.02104 AFIX 43 H4 2 0.412755 0.875632 0.486641 11.00000 -1.20000 AFIX 0 C5 1 0.318509 0.977369 0.518456 11.00000 0.03201 0.03533 = 0.02879 0.01326 0.00025 0.00439 AFIX 43 H5 2 0.333638 1.043313 0.502574 11.00000 -1.20000 AFIX 0 C6 1 0.249572 0.983197 0.550581 11.00000 0.02178 0.02234 = 0.02723 0.00805 0.00875 -0.00179 AFIX 43 H6 2 0.217899 1.052495 0.556565 11.00000 -1.20000 AFIX 0 C7 1 0.263121 0.500356 0.594938 11.00000 0.01637 0.02218 = 0.01824 0.00254 0.00317 0.00055 C8 1 0.228772 0.596827 0.570883 11.00000 0.01969 0.02049 = 0.01762 0.00031 -0.00008 0.00607 C9 1 0.161579 0.593688 0.528116 11.00000 0.03115 0.03241 = 0.01677 -0.00485 0.00009 0.01683 AFIX 43 H9 2 0.140037 0.660647 0.511877 11.00000 -1.20000 AFIX 0 C10 1 0.127619 0.490453 0.510282 11.00000 0.01711 0.04982 = 0.01411 -0.00289 0.00971 -0.00006 AFIX 43 H10 2 0.084744 0.486212 0.480780 11.00000 -1.20000 AFIX 0 C11 1 0.155446 0.392981 0.534980 11.00000 0.02054 0.03400 = 0.01854 -0.00888 0.00580 -0.00469 AFIX 43 H11 2 0.127262 0.323119 0.523542 11.00000 -1.20000 AFIX 0 C12 1 0.225181 0.398064 0.576791 11.00000 0.01415 0.02533 = 0.02303 0.00149 0.00462 0.00234 AFIX 43 H12 2 0.246801 0.330993 0.592928 11.00000 -1.20000 AFIX 0 C13 1 0.219043 0.884567 0.672370 11.00000 0.01953 0.01624 = 0.01964 0.00260 -0.00268 -0.00147 C14 1 0.329747 0.878429 0.676940 11.00000 0.01697 0.02346 = 0.03267 0.00371 -0.00503 -0.00075 AFIX 43 H14 2 0.364341 0.874368 0.650454 11.00000 -1.20000 AFIX 0 C15 1 0.387811 0.878433 0.721318 11.00000 0.01827 0.01073 = 0.03523 -0.00324 -0.00131 0.00179 AFIX 43 H15 2 0.462784 0.871609 0.725010 11.00000 -1.20000 AFIX 0 C16 1 0.338586 0.888177 0.760215 11.00000 0.03081 0.02239 = 0.02034 -0.00295 -0.00596 0.00071 AFIX 43 H16 2 0.379600 0.890430 0.790171 11.00000 -1.20000 AFIX 0 C17 1 0.229531 0.894567 0.755017 11.00000 0.03728 0.02569 = 0.02227 -0.00535 0.00658 -0.00386 AFIX 43 H17 2 0.195509 0.901383 0.781581 11.00000 -1.20000 AFIX 0 C18 1 0.169024 0.891153 0.711451 11.00000 0.02376 0.02448 = 0.02153 -0.00292 0.00052 -0.00201 AFIX 43 H18 2 0.093855 0.893289 0.708234 11.00000 -1.20000 AFIX 0 C19 1 0.075899 1.025034 0.610146 11.00000 0.02065 0.02555 = 0.02362 0.00300 0.00258 0.00462 C20 1 0.110527 1.113738 0.639253 11.00000 0.02611 0.02034 = 0.03208 -0.00712 0.01547 0.00005 AFIX 43 H20 2 0.167320 1.103306 0.663940 11.00000 -1.20000 AFIX 0 C21 1 0.062094 1.217728 0.632260 11.00000 0.04990 0.01931 = 0.04874 -0.00282 0.02708 -0.00322 AFIX 43 H21 2 0.083971 1.277789 0.652766 11.00000 -1.20000 AFIX 0 C22 1 -0.019369 1.233610 0.594723 11.00000 0.02907 0.01865 = 0.07283 0.01279 0.02092 0.00522 AFIX 43 H22 2 -0.051671 1.304984 0.589514 11.00000 -1.20000 AFIX 0 C23 1 -0.052274 1.146928 0.565720 11.00000 0.02307 0.03582 = 0.06025 0.02314 0.00054 0.00737 AFIX 43 H23 2 -0.106909 1.158510 0.540231 11.00000 -1.20000 AFIX 0 C24 1 -0.006486 1.041981 0.573199 11.00000 0.02375 0.02176 = 0.03835 0.00972 0.00080 -0.00174 AFIX 43 H24 2 -0.030941 0.981593 0.553292 11.00000 -1.20000 AFIX 0 C25 1 0.398159 0.367640 0.657768 11.00000 0.01172 0.01900 = 0.01958 0.00400 0.00102 -0.00232 C26 1 0.465979 0.325110 0.627773 11.00000 0.01962 0.02700 = 0.02449 0.00514 0.00475 0.00592 AFIX 43 H26 2 0.491306 0.372974 0.605961 11.00000 -1.20000 AFIX 0 C27 1 0.495206 0.213149 0.630433 11.00000 0.01153 0.04122 = 0.03443 0.00522 0.01015 0.00488 AFIX 43 H27 2 0.538643 0.183440 0.609749 11.00000 -1.20000 AFIX 0 C28 1 0.460678 0.145061 0.663402 11.00000 0.02679 0.01430 = 0.03482 0.00429 0.00512 0.00526 AFIX 43 H28 2 0.481193 0.068634 0.665308 11.00000 -1.20000 AFIX 0 C29 1 0.396865 0.186556 0.693561 11.00000 0.03011 0.02064 = 0.03859 0.00315 -0.00098 -0.00448 AFIX 43 H29 2 0.374736 0.139097 0.716313 11.00000 -1.20000 AFIX 0 C30 1 0.365102 0.297714 0.690586 11.00000 0.01744 0.02432 = 0.02903 0.01068 0.00033 -0.00078 AFIX 43 H30 2 0.320557 0.325968 0.711110 11.00000 -1.20000 AFIX 0 C31 1 0.277087 0.545300 0.692592 11.00000 0.02119 0.01094 = 0.01890 0.00966 -0.00191 0.00042 C32 1 0.329282 0.584118 0.735006 11.00000 0.02059 0.02354 = 0.02071 0.00428 0.00415 -0.00406 AFIX 43 H32 2 0.404339 0.590617 0.740298 11.00000 -1.20000 AFIX 0 C33 1 0.270709 0.613066 0.769293 11.00000 0.03134 0.01986 = 0.02059 0.00248 0.00205 -0.00667 AFIX 43 H33 2 0.305626 0.640060 0.798195 11.00000 -1.20000 AFIX 0 C34 1 0.161981 0.602877 0.761663 11.00000 0.02881 0.02027 = 0.02474 -0.00159 0.01757 0.00187 AFIX 43 H34 2 0.122803 0.624309 0.785360 11.00000 -1.20000 AFIX 0 C35 1 0.109160 0.562756 0.720906 11.00000 0.01645 0.03976 = 0.03186 -0.00221 0.00747 0.00097 AFIX 43 H35 2 0.034299 0.554194 0.716510 11.00000 -1.20000 AFIX 0 C36 1 0.167582 0.534218 0.685421 11.00000 0.02601 0.02427 = 0.02471 0.00238 -0.00414 -0.00310 AFIX 43 H36 2 0.131997 0.507408 0.656608 11.00000 -1.20000 AFIX 0 O1 3 0.259754 0.697135 0.592406 11.00000 0.03204 0.01943 = 0.01617 0.00508 0.00040 0.00234 P1 5 0.135633 0.886568 0.616230 11.00000 0.01614 0.01328 = 0.01618 -0.00165 -0.00123 -0.00025 P2 5 0.356711 0.511960 0.648184 11.00000 0.01542 0.01433 = 0.01882 0.00246 0.00030 -0.00161 MOLE 2 C41 1 -0.134015 0.663306 0.590384 11.00000 0.01786 0.01151 = 0.02411 -0.00506 0.00696 -0.00283 C42 1 -0.216908 0.706646 0.559368 11.00000 0.02033 0.02090 = 0.02155 -0.00177 -0.00029 0.00124 C43 1 -0.310967 0.650047 0.543651 11.00000 0.01501 0.02539 = 0.02490 -0.00863 0.00756 0.00643 C44 1 -0.324097 0.545474 0.562192 11.00000 0.01960 0.02223 = 0.02578 -0.00886 0.00208 -0.00409 C45 1 -0.244566 0.497334 0.593831 11.00000 0.01794 0.02731 = 0.02043 -0.00310 0.00645 -0.00679 C46 1 -0.152500 0.559417 0.607224 11.00000 0.01604 0.02782 = 0.01713 -0.00812 0.00213 0.00243 F42 4 -0.206776 0.808973 0.540604 11.00000 0.02595 0.02175 = 0.03591 0.00279 -0.00306 0.00083 F44 4 -0.412547 0.486682 0.547358 11.00000 0.01842 0.04167 = 0.03351 -0.00561 0.00181 -0.01276 F46 4 -0.075930 0.509283 0.637421 11.00000 0.02613 0.02931 = 0.02898 0.00512 -0.00688 -0.00866 CL43 6 -0.406745 0.704787 0.502140 11.00000 0.01914 0.03908 = 0.04443 0.00269 -0.00540 0.00222 CL45 6 -0.261782 0.365094 0.615320 11.00000 0.02995 0.03101 = 0.03645 0.00542 0.00403 -0.01263 MOLE 3 C51 1 0.622364 0.743440 0.656987 11.00000 0.01568 0.02138 = 0.02716 0.00136 0.01217 -0.00695 C52 1 0.626066 0.840329 0.632356 11.00000 0.01646 0.02386 = 0.02308 0.00088 0.00368 0.00286 C53 1 0.712364 0.910107 0.636437 11.00000 0.02554 0.02130 = 0.02114 0.00990 0.00738 -0.00946 C54 1 0.802738 0.880226 0.666583 11.00000 0.01835 0.01510 = 0.02505 -0.00754 0.00735 0.00099 C55 1 0.803206 0.786877 0.693255 11.00000 0.02199 0.02855 = 0.02426 -0.00150 0.00270 0.00480 C56 1 0.712185 0.719441 0.687773 11.00000 0.02094 0.01175 = 0.03498 0.01268 0.00711 0.00313 F52 4 0.539297 0.873083 0.602101 11.00000 0.03262 0.03677 = 0.03229 0.01113 -0.00774 -0.00568 F54 4 0.890481 0.943733 0.669728 11.00000 0.02218 0.02181 = 0.04408 -0.00328 0.00908 -0.00879 F56 4 0.717101 0.625649 0.713331 11.00000 0.03333 0.02162 = 0.04703 0.01275 -0.00028 -0.00092 CL53 6 0.715250 1.029769 0.603599 11.00000 0.04245 0.02120 = 0.03368 0.00566 0.01170 0.00144 CL55 6 0.911201 0.753287 0.734156 11.00000 0.02263 0.03986 = 0.05500 0.01035 -0.00575 0.00176 HKLF 4 Covalent radii and connectivity table for 2008src0880 in P2(1)/c C 0.770 H 0.320 O 0.660 F 0.640 P 1.100 CL 0.990 AU 1.440 Au1 - C41 P1 Au2 - C51 P2 C1 - C6 C2 P1 C2 - C3 O1 C1 C3 - C4 C2 C4 - C3 C5 C5 - C4 C6 C6 - C5 C1 C7 - C8 C12 P2 C8 - O1 C7 C9 C9 - C10 C8 C10 - C9 C11 C11 - C10 C12 C12 - C7 C11 C13 - C18 C14 P1 C14 - C15 C13 C15 - C16 C14 C16 - C17 C15 C17 - C16 C18 C18 - C17 C13 C19 - C20 C24 P1 C20 - C19 C21 C21 - C20 C22 C22 - C23 C21 C23 - C22 C24 C24 - C23 C19 C25 - C30 C26 P2 C26 - C27 C25 C27 - C28 C26 C28 - C29 C27 C29 - C28 C30 C30 - C25 C29 C31 - C36 C32 P2 C32 - C33 C31 C33 - C34 C32 C34 - C35 C33 C35 - C34 C36 C36 - C31 C35 O1 - C8 C2 P1 - C13 C1 C19 Au1 P2 - C31 C25 C7 Au2 C41 - C46 C42 Au1 C42 - F42 C41 C43 C43 - C44 C42 Cl43 C44 - F44 C43 C45 C45 - C44 C46 Cl45 C46 - F46 C41 C45 F42 - C42 F44 - C44 F46 - C46 Cl43 - C43 Cl45 - C45 C51 - C52 C56 Au2 C52 - F52 C51 C53 C53 - C52 C54 Cl53 C54 - F54 C55 C53 C55 - C54 C56 Cl55 C56 - F56 C51 C55 F52 - C52 F54 - C54 F56 - C56 Cl53 - C53 Cl55 - C55 h k l Fo^2 Sigma Why rejected 1 0 5 6.91 1.51 observed but should be systematically absent 29207 Reflections read, of which 972 rejected -16 =< h =< 16, -15 =< k =< 14, -37 =< l =< 37, Max. 2-theta = 54.97 1 Systematic absence violations 0 Inconsistent equivalents 9418 Unique reflections, of which 0 suppressed R(int) = 0.0404 R(sigma) = 0.0471 Friedel opposites merged Maximum memory for data reduction = 4482 / 94995 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 = 5950 / 769289 wR2 = 0.0969 before cycle 1 for 9418 data and 568 / 568 parameters GooF = S = 1.107; Restrained GooF = 1.107 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0233 * P )^2 + 37.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15113 0.00015 0.057 OSF Mean shift/esd = 0.012 Maximum = 0.073 for U23 Au1 Max. shift = 0.000 A for C27 Max. dU = 0.000 for C32 Least-squares cycle 2 Maximum vector length = 511 Memory required = 5950 / 769289 wR2 = 0.0969 before cycle 2 for 9418 data and 568 / 568 parameters GooF = S = 1.107; Restrained GooF = 1.107 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0233 * P )^2 + 37.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15113 0.00015 0.018 OSF Mean shift/esd = 0.005 Maximum = 0.027 for U23 Au1 Max. shift = 0.000 A for C2 Max. dU = 0.000 for C32 Least-squares cycle 3 Maximum vector length = 511 Memory required = 5950 / 769289 wR2 = 0.0968 before cycle 3 for 9418 data and 568 / 568 parameters GooF = S = 1.107; Restrained GooF = 1.107 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0233 * P )^2 + 37.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15113 0.00015 0.002 OSF Mean shift/esd = 0.000 Maximum = 0.003 for U13 C10 Max. shift = 0.000 A for C10 Max. dU = 0.000 for C28 Least-squares cycle 4 Maximum vector length = 511 Memory required = 5950 / 769289 wR2 = 0.0968 before cycle 4 for 9418 data and 568 / 568 parameters GooF = S = 1.107; Restrained GooF = 1.107 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0233 * P )^2 + 37.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15113 0.00015 0.001 OSF Mean shift/esd = 0.000 Maximum = -0.004 for z Au2 Max. shift = 0.000 A for C53 Max. dU = 0.000 for C29 Least-squares cycle 5 Maximum vector length = 511 Memory required = 5950 / 769289 wR2 = 0.0968 before cycle 5 for 9418 data and 568 / 568 parameters GooF = S = 1.107; Restrained GooF = 1.107 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0233 * P )^2 + 37.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15113 0.00015 -0.002 OSF Mean shift/esd = 0.000 Maximum = -0.002 for OSF Max. shift = 0.000 A for C45 Max. dU = 0.000 for C30 Least-squares cycle 6 Maximum vector length = 511 Memory required = 5950 / 769289 wR2 = 0.0968 before cycle 6 for 9418 data and 568 / 568 parameters GooF = S = 1.107; Restrained GooF = 1.107 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0233 * P )^2 + 37.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15113 0.00015 -0.001 OSF Mean shift/esd = 0.000 Maximum = 0.003 for z Au2 Max. shift = 0.000 A for C51 Max. dU = 0.000 for C53 Least-squares cycle 7 Maximum vector length = 511 Memory required = 5950 / 769289 wR2 = 0.0968 before cycle 7 for 9418 data and 568 / 568 parameters GooF = S = 1.107; Restrained GooF = 1.107 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0233 * P )^2 + 37.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15113 0.00015 0.002 OSF Mean shift/esd = 0.000 Maximum = 0.003 for z Au2 Max. shift = 0.000 A for H21 Max. dU = 0.000 for F54 Least-squares cycle 8 Maximum vector length = 511 Memory required = 5950 / 769289 wR2 = 0.0968 before cycle 8 for 9418 data and 568 / 568 parameters GooF = S = 1.107; Restrained GooF = 1.107 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0233 * P )^2 + 37.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15113 0.00015 -0.001 OSF Mean shift/esd = 0.000 Maximum = 0.003 for z Au2 Max. shift = 0.000 A for C51 Max. dU = 0.000 for C5 Least-squares cycle 9 Maximum vector length = 511 Memory required = 5950 / 769289 wR2 = 0.0968 before cycle 9 for 9418 data and 568 / 568 parameters GooF = S = 1.107; Restrained GooF = 1.107 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0233 * P )^2 + 37.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15113 0.00015 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.003 for z Au2 Max. shift = 0.000 A for C20 Max. dU = 0.000 for C16 Least-squares cycle 10 Maximum vector length = 511 Memory required = 5950 / 769289 wR2 = 0.0968 before cycle 10 for 9418 data and 568 / 568 parameters GooF = S = 1.107; Restrained GooF = 1.107 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0233 * P )^2 + 37.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.15113 0.00015 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.003 for z Au2 Max. shift = 0.000 A for C24 Max. dU = 0.000 for C22 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 11 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 0.3765 0.7123 0.5255 43 0.950 0.000 C3 C4 C2 H4 0.4127 0.8756 0.4866 43 0.950 0.000 C4 C3 C5 H5 0.3336 1.0433 0.5026 43 0.950 0.000 C5 C4 C6 H6 0.2179 1.0525 0.5566 43 0.950 0.000 C6 C5 C1 H9 0.1400 0.6606 0.5119 43 0.950 0.000 C9 C10 C8 H10 0.0848 0.4862 0.4808 43 0.950 0.000 C10 C9 C11 H11 0.1273 0.3231 0.5236 43 0.950 0.000 C11 C10 C12 H12 0.2468 0.3310 0.5929 43 0.950 0.000 C12 C7 C11 H14 0.3644 0.8744 0.6505 43 0.950 0.000 C14 C15 C13 H15 0.4628 0.8716 0.7250 43 0.950 0.000 C15 C16 C14 H16 0.3796 0.8904 0.7902 43 0.950 0.000 C16 C17 C15 H17 0.1955 0.9014 0.7816 43 0.950 0.000 C17 C16 C18 H18 0.0939 0.8933 0.7082 43 0.950 0.000 C18 C17 C13 H20 0.1673 1.1033 0.6640 43 0.950 0.000 C20 C19 C21 H21 0.0840 1.2778 0.6528 43 0.950 0.000 C21 C20 C22 H22 -0.0517 1.3050 0.5895 43 0.950 0.000 C22 C23 C21 H23 -0.1069 1.1585 0.5402 43 0.950 0.000 C23 C22 C24 H24 -0.0309 0.9816 0.5533 43 0.950 0.000 C24 C23 C19 H26 0.4913 0.3730 0.6060 43 0.950 0.000 C26 C27 C25 H27 0.5386 0.1835 0.6098 43 0.950 0.000 C27 C28 C26 H28 0.4812 0.0686 0.6653 43 0.950 0.000 C28 C29 C27 H29 0.3748 0.1391 0.7163 43 0.950 0.000 C29 C28 C30 H30 0.3205 0.3260 0.7111 43 0.950 0.000 C30 C25 C29 H32 0.4043 0.5906 0.7403 43 0.950 0.000 C32 C33 C31 H33 0.3056 0.6401 0.7982 43 0.950 0.000 C33 C34 C32 H34 0.1228 0.6243 0.7854 43 0.950 0.000 C34 C35 C33 H35 0.0343 0.5542 0.7165 43 0.950 0.000 C35 C34 C36 H36 0.1320 0.5074 0.6566 43 0.950 0.000 C36 C31 C35 2008src0880 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Au1 0.00160 0.75850 0.60485 1.00000 0.01639 0.01617 0.01714 -0.00327 -0.00028 -0.00284 0.01686 0.00040 0.00002 0.00002 0.00001 0.00000 0.00012 0.00013 0.00011 0.00009 0.00009 0.00009 0.00007 Au2 0.49484 0.63379 0.64965 1.00000 0.01749 0.01701 0.02370 0.00185 0.00287 -0.00296 0.01943 0.00044 0.00002 0.00002 0.00001 0.00000 0.00012 0.00014 0.00012 0.00010 0.00009 0.00009 0.00007 C1 0.22675 0.88691 0.57415 1.00000 0.02161 0.01616 0.01880 0.00697 0.00290 -0.00743 0.01888 0.01121 0.00051 0.00054 0.00021 0.00000 0.00321 0.00323 0.00291 0.00254 0.00253 0.00258 0.00133 C2 0.27696 0.78775 0.56439 1.00000 0.02576 0.02641 0.01256 0.01020 -0.00371 0.00323 0.02227 0.01208 0.00054 0.00059 0.00021 0.00000 0.00344 0.00376 0.00280 0.00266 0.00255 0.00287 0.00146 C3 0.34492 0.78143 0.53190 1.00000 0.03468 0.03264 0.02549 0.00829 0.01183 0.01894 0.03018 0.01478 0.00060 0.00066 0.00024 0.00000 0.00409 0.00425 0.00348 0.00317 0.00309 0.00342 0.00171 H3 0.37646 0.71233 0.52554 1.00000 0.03622 0.00000 0.00000 C4 0.36590 0.87772 0.50893 1.00000 0.03418 0.05146 0.02392 0.00860 0.00634 0.02104 0.03632 0.01534 0.00063 0.00072 0.00025 0.00000 0.00424 0.00538 0.00349 0.00360 0.00317 0.00384 0.00196 H4 0.41273 0.87562 0.48665 1.00000 0.04359 0.00000 0.00000 C5 0.31850 0.97739 0.51846 1.00000 0.03203 0.03538 0.02882 0.01332 0.00018 0.00438 0.03254 0.01416 0.00060 0.00069 0.00025 0.00000 0.00400 0.00443 0.00366 0.00339 0.00318 0.00341 0.00176 H5 0.33364 1.04334 0.50258 1.00000 0.03905 0.00000 0.00000 C6 0.24957 0.98317 0.55058 1.00000 0.02170 0.02240 0.02715 0.00796 0.00880 -0.00184 0.02322 0.01242 0.00053 0.00060 0.00023 0.00000 0.00330 0.00357 0.00331 0.00290 0.00275 0.00277 0.00143 H6 0.21788 1.05246 0.55656 1.00000 0.02787 0.00000 0.00000 C7 0.26313 0.50036 0.59494 1.00000 0.01630 0.02221 0.01816 0.00258 0.00318 0.00050 0.01883 0.01135 0.00049 0.00056 0.00021 0.00000 0.00302 0.00351 0.00289 0.00260 0.00243 0.00256 0.00132 C8 0.22876 0.59682 0.57088 1.00000 0.01969 0.02046 0.01772 0.00035 -0.00009 0.00609 0.01960 0.01161 0.00050 0.00056 0.00021 0.00000 0.00317 0.00340 0.00294 0.00259 0.00253 0.00262 0.00135 C9 0.16158 0.59368 0.52812 1.00000 0.03115 0.03246 0.01674 -0.00489 0.00007 0.01682 0.02716 0.01291 0.00057 0.00064 0.00022 0.00000 0.00379 0.00411 0.00305 0.00288 0.00281 0.00319 0.00162 H9 0.14004 0.66064 0.51189 1.00000 0.03259 0.00000 0.00000 C10 0.12763 0.49045 0.51028 1.00000 0.01692 0.04987 0.01415 -0.00281 0.00985 0.00010 0.02620 0.01271 0.00052 0.00067 0.00022 0.00000 0.00317 0.00485 0.00285 0.00308 0.00249 0.00313 0.00160 H10 0.08477 0.48621 0.48078 1.00000 0.03144 0.00000 0.00000 C11 0.15545 0.39299 0.53498 1.00000 0.02049 0.03410 0.01854 -0.00901 0.00580 -0.00464 0.02408 0.01192 0.00052 0.00064 0.00022 0.00000 0.00327 0.00408 0.00301 0.00292 0.00261 0.00293 0.00148 H11 0.12725 0.32313 0.52355 1.00000 0.02890 0.00000 0.00000 C12 0.22518 0.39807 0.57679 1.00000 0.01414 0.02526 0.02312 0.00150 0.00465 0.00239 0.02065 0.01175 0.00049 0.00059 0.00022 0.00000 0.00299 0.00360 0.00312 0.00278 0.00256 0.00262 0.00137 H12 0.24679 0.33100 0.59293 1.00000 0.02478 0.00000 0.00000 C13 0.21905 0.88457 0.67237 1.00000 0.01958 0.01614 0.01965 0.00263 -0.00271 -0.00150 0.01905 0.01106 0.00051 0.00054 0.00022 0.00000 0.00314 0.00325 0.00294 0.00255 0.00255 0.00255 0.00134 C14 0.32976 0.87844 0.67694 1.00000 0.01701 0.02343 0.03260 0.00378 -0.00501 -0.00076 0.02527 0.01180 0.00052 0.00057 0.00025 0.00000 0.00319 0.00369 0.00365 0.00305 0.00285 0.00272 0.00154 H14 0.36436 0.87439 0.65046 1.00000 0.03032 0.00000 0.00000 C15 0.38780 0.87841 0.72132 1.00000 0.01811 0.01072 0.03532 -0.00337 -0.00122 0.00180 0.02194 0.01128 0.00052 0.00052 0.00024 0.00000 0.00316 0.00312 0.00366 0.00278 0.00285 0.00248 0.00144 H15 0.46278 0.87156 0.72501 1.00000 0.02633 0.00000 0.00000 C16 0.33859 0.88817 0.76021 1.00000 0.03082 0.02234 0.02033 -0.00308 -0.00600 0.00075 0.02553 0.01188 0.00057 0.00058 0.00023 0.00000 0.00378 0.00365 0.00312 0.00281 0.00287 0.00297 0.00155 H16 0.37960 0.89044 0.79016 1.00000 0.03064 0.00000 0.00000 C17 0.22953 0.89457 0.75501 1.00000 0.03735 0.02564 0.02225 -0.00537 0.00662 -0.00378 0.02820 0.01251 0.00060 0.00061 0.00024 0.00000 0.00417 0.00387 0.00331 0.00294 0.00305 0.00321 0.00160 H17 0.19551 0.90137 0.78158 1.00000 0.03384 0.00000 0.00000 C18 0.16902 0.89117 0.71145 1.00000 0.02377 0.02437 0.02164 -0.00288 0.00044 -0.00193 0.02358 0.01176 0.00056 0.00058 0.00023 0.00000 0.00342 0.00369 0.00316 0.00283 0.00275 0.00286 0.00146 H18 0.09385 0.89332 0.70823 1.00000 0.02829 0.00000 0.00000 C19 0.07590 1.02504 0.61015 1.00000 0.02067 0.02553 0.02360 0.00298 0.00261 0.00468 0.02335 0.01240 0.00052 0.00060 0.00023 0.00000 0.00329 0.00375 0.00318 0.00286 0.00270 0.00278 0.00145 C20 0.11052 1.11374 0.63926 1.00000 0.02603 0.02025 0.03211 -0.00714 0.01557 0.00006 0.02497 0.01285 0.00056 0.00058 0.00025 0.00000 0.00354 0.00358 0.00359 0.00297 0.00296 0.00285 0.00148 H20 0.16729 1.10330 0.66396 1.00000 0.02996 0.00000 0.00000 C21 0.06208 1.21772 0.63226 1.00000 0.04990 0.01943 0.04869 -0.00282 0.02708 -0.00329 0.03730 0.01598 0.00069 0.00065 0.00030 0.00000 0.00510 0.00395 0.00481 0.00354 0.00413 0.00355 0.00192 H21 0.08397 1.27779 0.65276 1.00000 0.04476 0.00000 0.00000 C22 -0.01938 1.23364 0.59473 1.00000 0.02916 0.01859 0.07282 0.01274 0.02096 0.00522 0.03882 0.01688 0.00063 0.00066 0.00033 0.00000 0.00401 0.00382 0.00607 0.00400 0.00411 0.00322 0.00205 H22 -0.05169 1.30501 0.58952 1.00000 0.04658 0.00000 0.00000 C23 -0.05226 1.14691 0.56572 1.00000 0.02303 0.03572 0.06023 0.02319 0.00059 0.00735 0.04026 0.01643 0.00060 0.00070 0.00032 0.00000 0.00377 0.00473 0.00539 0.00427 0.00377 0.00338 0.00212 H23 -0.10688 1.15848 0.54022 1.00000 0.04832 0.00000 0.00000 C24 -0.00647 1.04200 0.57321 1.00000 0.02383 0.02168 0.03838 0.00979 0.00079 -0.00176 0.02838 0.01347 0.00055 0.00061 0.00026 0.00000 0.00354 0.00374 0.00396 0.00320 0.00315 0.00290 0.00163 H24 -0.03093 0.98161 0.55330 1.00000 0.03405 0.00000 0.00000 C25 0.39814 0.36763 0.65778 1.00000 0.01165 0.01907 0.01950 0.00401 0.00103 -0.00231 0.01688 0.01087 0.00047 0.00053 0.00021 0.00000 0.00274 0.00330 0.00285 0.00256 0.00232 0.00240 0.00126 C26 0.46598 0.32512 0.62778 1.00000 0.01964 0.02720 0.02440 0.00516 0.00468 0.00590 0.02361 0.01259 0.00052 0.00060 0.00023 0.00000 0.00325 0.00383 0.00327 0.00291 0.00270 0.00282 0.00146 H26 0.49132 0.37299 0.60597 1.00000 0.02833 0.00000 0.00000 C27 0.49519 0.21317 0.63044 1.00000 0.01151 0.04129 0.03437 0.00527 0.01014 0.00484 0.02837 0.01363 0.00051 0.00067 0.00026 0.00000 0.00301 0.00459 0.00378 0.00342 0.00280 0.00297 0.00163 H27 0.53864 0.18347 0.60976 1.00000 0.03404 0.00000 0.00000 C28 0.46066 0.14506 0.66341 1.00000 0.02681 0.01426 0.03482 0.00423 0.00498 0.00525 0.02527 0.01273 0.00055 0.00058 0.00025 0.00000 0.00359 0.00337 0.00368 0.00291 0.00306 0.00277 0.00151 H28 0.48116 0.06863 0.66531 1.00000 0.03033 0.00000 0.00000 C29 0.39687 0.18656 0.69356 1.00000 0.03004 0.02056 0.03867 0.00325 -0.00103 -0.00451 0.03041 0.01277 0.00058 0.00062 0.00027 0.00000 0.00390 0.00370 0.00409 0.00325 0.00332 0.00305 0.00169 H29 0.37475 0.13910 0.71631 1.00000 0.03650 0.00000 0.00000 C30 0.36509 0.29771 0.69058 1.00000 0.01736 0.02426 0.02906 0.01073 0.00032 -0.00088 0.02390 0.01220 0.00052 0.00058 0.00024 0.00000 0.00318 0.00369 0.00348 0.00298 0.00276 0.00272 0.00149 H30 0.32053 0.32596 0.71111 1.00000 0.02868 0.00000 0.00000 C31 0.27708 0.54530 0.69260 1.00000 0.02126 0.01081 0.01896 0.00971 -0.00199 0.00040 0.01754 0.01119 0.00050 0.00051 0.00021 0.00000 0.00315 0.00300 0.00291 0.00244 0.00253 0.00243 0.00131 C32 0.32927 0.58412 0.73500 1.00000 0.02045 0.02351 0.02070 0.00441 0.00425 -0.00408 0.02144 0.01184 0.00053 0.00057 0.00022 0.00000 0.00323 0.00359 0.00306 0.00273 0.00262 0.00275 0.00139 H32 0.40432 0.59063 0.74029 1.00000 0.02573 0.00000 0.00000 C33 0.27071 0.61306 0.76929 1.00000 0.03128 0.01983 0.02058 0.00260 0.00215 -0.00672 0.02409 0.01213 0.00056 0.00057 0.00023 0.00000 0.00376 0.00352 0.00311 0.00275 0.00281 0.00291 0.00148 H33 0.30564 0.64005 0.79819 1.00000 0.02890 0.00000 0.00000 C34 0.16198 0.60288 0.76166 1.00000 0.02878 0.02021 0.02470 -0.00158 0.01761 0.00191 0.02315 0.01254 0.00055 0.00057 0.00023 0.00000 0.00363 0.00349 0.00327 0.00278 0.00286 0.00286 0.00143 H34 0.12280 0.62432 0.78536 1.00000 0.02778 0.00000 0.00000 C35 0.10915 0.56274 0.72090 1.00000 0.01648 0.03967 0.03185 -0.00227 0.00743 0.00102 0.02894 0.01320 0.00055 0.00066 0.00025 0.00000 0.00326 0.00455 0.00373 0.00339 0.00291 0.00306 0.00164 H35 0.03429 0.55416 0.71650 1.00000 0.03473 0.00000 0.00000 C36 0.16758 0.53423 0.68543 1.00000 0.02599 0.02425 0.02475 0.00252 -0.00417 -0.00321 0.02584 0.01226 0.00055 0.00059 0.00024 0.00000 0.00354 0.00373 0.00331 0.00295 0.00285 0.00294 0.00154 H36 0.13200 0.50742 0.65661 1.00000 0.03101 0.00000 0.00000 O1 0.25975 0.69714 0.59241 1.00000 0.03202 0.01940 0.01619 0.00516 0.00042 0.00231 0.02288 0.00826 0.00038 0.00039 0.00015 0.00000 0.00266 0.00246 0.00211 0.00189 0.00194 0.00203 0.00103 P1 0.13563 0.88657 0.61623 1.00000 0.01614 0.01329 0.01619 -0.00166 -0.00121 -0.00022 0.01559 0.00275 0.00013 0.00014 0.00005 0.00000 0.00075 0.00079 0.00071 0.00061 0.00061 0.00061 0.00032 P2 0.35671 0.51196 0.64818 1.00000 0.01544 0.01436 0.01882 0.00247 0.00030 -0.00162 0.01645 0.00284 0.00013 0.00014 0.00006 0.00000 0.00075 0.00081 0.00073 0.00064 0.00062 0.00062 0.00033 C41 -0.13402 0.66330 0.59039 1.00000 0.01786 0.01143 0.02410 -0.00497 0.00686 -0.00284 0.01742 0.01092 0.00049 0.00052 0.00022 0.00000 0.00302 0.00300 0.00306 0.00248 0.00253 0.00239 0.00127 C42 -0.21692 0.70664 0.55937 1.00000 0.02037 0.02077 0.02166 -0.00171 -0.00023 0.00128 0.02129 0.01153 0.00052 0.00057 0.00022 0.00000 0.00323 0.00355 0.00311 0.00269 0.00261 0.00265 0.00140 C43 -0.31097 0.65004 0.54366 1.00000 0.01500 0.02544 0.02492 -0.00866 0.00746 0.00656 0.02133 0.01184 0.00050 0.00058 0.00023 0.00000 0.00302 0.00367 0.00318 0.00282 0.00257 0.00267 0.00140 C44 -0.32409 0.54549 0.56219 1.00000 0.01968 0.02210 0.02579 -0.00883 0.00212 -0.00417 0.02266 0.01127 0.00052 0.00058 0.00023 0.00000 0.00322 0.00362 0.00330 0.00282 0.00271 0.00270 0.00144 C45 -0.24456 0.49733 0.59383 1.00000 0.01794 0.02716 0.02043 -0.00305 0.00648 -0.00677 0.02147 0.01136 0.00051 0.00059 0.00022 0.00000 0.00314 0.00379 0.00302 0.00277 0.00255 0.00272 0.00141 C46 -0.15251 0.55944 0.60722 1.00000 0.01607 0.02791 0.01704 -0.00819 0.00216 0.00253 0.02038 0.01123 0.00050 0.00058 0.00021 0.00000 0.00304 0.00372 0.00289 0.00271 0.00245 0.00266 0.00139 F42 -0.20677 0.80897 0.54060 1.00000 0.02591 0.02182 0.03587 0.00278 -0.00304 0.00083 0.02868 0.00708 0.00031 0.00034 0.00014 0.00000 0.00210 0.00213 0.00226 0.00183 0.00181 0.00169 0.00094 F44 -0.41255 0.48668 0.54736 1.00000 0.01842 0.04165 0.03347 -0.00563 0.00181 -0.01274 0.03140 0.00681 0.00030 0.00037 0.00014 0.00000 0.00196 0.00262 0.00218 0.00200 0.00174 0.00183 0.00099 F46 -0.07593 0.50928 0.63742 1.00000 0.02612 0.02926 0.02899 0.00516 -0.00689 -0.00870 0.02928 0.00670 0.00031 0.00034 0.00014 0.00000 0.00209 0.00232 0.00206 0.00182 0.00174 0.00177 0.00096 Cl43 -0.40675 0.70479 0.50214 1.00000 0.01913 0.03908 0.04444 0.00269 -0.00544 0.00222 0.03529 0.00336 0.00014 0.00017 0.00007 0.00000 0.00081 0.00111 0.00106 0.00089 0.00077 0.00075 0.00044 Cl45 -0.26178 0.36510 0.61532 1.00000 0.02996 0.03102 0.03647 0.00543 0.00402 -0.01263 0.03259 0.00321 0.00015 0.00016 0.00006 0.00000 0.00092 0.00101 0.00093 0.00080 0.00076 0.00076 0.00041 C51 0.62235 0.74345 0.65698 1.00000 0.01562 0.02142 0.02713 0.00140 0.01221 -0.00698 0.02046 0.01181 0.00050 0.00056 0.00023 0.00000 0.00305 0.00356 0.00326 0.00277 0.00259 0.00256 0.00137 C52 0.62607 0.84032 0.63236 1.00000 0.01646 0.02374 0.02305 0.00099 0.00374 0.00282 0.02101 0.01189 0.00050 0.00058 0.00022 0.00000 0.00308 0.00359 0.00314 0.00275 0.00259 0.00264 0.00139 C53 0.71236 0.91012 0.63643 1.00000 0.02549 0.02123 0.02119 0.01002 0.00747 -0.00945 0.02223 0.01210 0.00054 0.00058 0.00022 0.00000 0.00349 0.00353 0.00310 0.00270 0.00270 0.00278 0.00144 C54 0.80273 0.88022 0.66658 1.00000 0.01838 0.01512 0.02508 -0.00759 0.00729 0.00099 0.01911 0.01126 0.00050 0.00054 0.00022 0.00000 0.00310 0.00323 0.00313 0.00262 0.00258 0.00250 0.00132 C55 0.80320 0.78688 0.69325 1.00000 0.02199 0.02845 0.02421 -0.00148 0.00278 0.00490 0.02497 0.01253 0.00054 0.00061 0.00024 0.00000 0.00342 0.00394 0.00329 0.00296 0.00275 0.00293 0.00150 C56 0.71218 0.71945 0.68777 1.00000 0.02097 0.01167 0.03503 0.01271 0.00704 0.00312 0.02227 0.01281 0.00052 0.00054 0.00025 0.00000 0.00328 0.00316 0.00366 0.00280 0.00285 0.00256 0.00144 F52 0.53929 0.87308 0.60210 1.00000 0.03262 0.03678 0.03226 0.01107 -0.00770 -0.00564 0.03521 0.00749 0.00034 0.00037 0.00015 0.00000 0.00235 0.00261 0.00224 0.00200 0.00188 0.00198 0.00107 F54 0.89048 0.94374 0.66973 1.00000 0.02217 0.02191 0.04409 -0.00322 0.00900 -0.00883 0.02898 0.00701 0.00031 0.00033 0.00015 0.00000 0.00201 0.00218 0.00244 0.00189 0.00186 0.00166 0.00094 F56 0.71710 0.62565 0.71333 1.00000 0.03342 0.02153 0.04704 0.01276 -0.00026 -0.00092 0.03467 0.00781 0.00034 0.00034 0.00016 0.00000 0.00236 0.00224 0.00261 0.00200 0.00206 0.00182 0.00106 Cl53 0.71525 1.02977 0.60360 1.00000 0.04246 0.02124 0.03370 0.00565 0.01170 0.00146 0.03185 0.00350 0.00016 0.00015 0.00006 0.00000 0.00105 0.00089 0.00089 0.00075 0.00080 0.00077 0.00040 Cl55 0.91120 0.75329 0.73415 1.00000 0.02263 0.03985 0.05504 0.01037 -0.00577 0.00175 0.04040 0.00369 0.00015 0.00017 0.00008 0.00000 0.00088 0.00118 0.00122 0.00097 0.00087 0.00079 0.00050 Final Structure Factor Calculation for 2008src0880 in P2(1)/c Total number of l.s. parameters = 568 Maximum vector length = 511 Memory required = 5382 / 26061 wR2 = 0.0968 before cycle 11 for 9418 data and 0 / 568 parameters GooF = S = 1.107; Restrained GooF = 1.107 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0233 * P )^2 + 37.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0343 for 7931 Fo > 4sig(Fo) and 0.0462 for all 9418 data wR2 = 0.0968, GooF = S = 1.107, Restrained GooF = 1.107 for all data Occupancy sum of asymmetric unit = 63.00 for non-hydrogen and 28.00 for hydrogen atoms Principal mean square atomic displacements U 0.0204 0.0191 0.0111 Au1 0.0246 0.0198 0.0139 Au2 0.0297 0.0199 0.0070 C1 0.0323 0.0289 0.0056 C2 0.0549 0.0210 0.0146 C3 0.0662 0.0239 0.0189 C4 0.0459 0.0348 0.0170 C5 0.0334 0.0236 0.0126 C6 0.0235 0.0170 0.0160 C7 0.0270 0.0186 0.0132 C8 0.0510 0.0170 0.0135 C9 0.0501 0.0221 0.0065 C10 0.0392 0.0191 0.0140 C11 0.0265 0.0223 0.0131 C12 0.0273 0.0157 0.0142 C13 0.0392 0.0225 0.0142 C14 0.0384 0.0174 0.0100 C15 0.0390 0.0226 0.0150 C16 0.0388 0.0275 0.0183 C17 0.0265 0.0260 0.0182 C18 0.0289 0.0237 0.0174 C19 0.0406 0.0221 0.0122 C20 0.0666 0.0262 0.0191 C21 0.0777 0.0231 0.0156 C22 0.0748 0.0308 0.0151 C23 0.0448 0.0233 0.0171 C24 0.0243 0.0154 0.0110 C25 0.0328 0.0216 0.0164 C26 0.0451 0.0318 0.0082 C27 0.0357 0.0282 0.0120 C28 0.0444 0.0282 0.0186 C29 0.0388 0.0174 0.0155 C30 0.0291 0.0194 0.0042 C31 0.0283 0.0215 0.0145 C32 0.0355 0.0211 0.0157 C33 0.0386 0.0209 0.0099 C34 0.0403 0.0317 0.0148 C35 0.0365 0.0227 0.0183 C36 0.0334 0.0232 0.0121 O1 0.0207 0.0143 0.0118 P1 0.0218 0.0147 0.0129 P2 0.0272 0.0155 0.0096 C41 0.0261 0.0198 0.0180 C42 0.0344 0.0230 0.0065 C43 0.0330 0.0218 0.0133 C44 0.0318 0.0194 0.0133 C45 0.0331 0.0160 0.0121 C46 0.0417 0.0241 0.0202 F42 0.0479 0.0338 0.0125 F44 0.0470 0.0241 0.0167 F46 0.0503 0.0392 0.0165 Cl43 0.0468 0.0344 0.0167 Cl45 0.0312 0.0244 0.0058 C51 0.0251 0.0226 0.0154 C52 0.0352 0.0267 0.0048 C53 0.0295 0.0185 0.0093 C54 0.0318 0.0238 0.0193 C55 0.0408 0.0199 0.0061 C56 0.0561 0.0294 0.0202 F52 0.0451 0.0289 0.0130 F54 0.0556 0.0322 0.0162 F56 0.0452 0.0315 0.0189 Cl53 0.0647 0.0371 0.0194 Cl55 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.020 0.037 0.057 0.076 0.098 0.123 0.153 0.195 0.267 1.000 Number in group 957. 927. 942. 947. 935. 950. 952. 923. 945. 940. GooF 0.926 0.868 0.936 0.976 1.164 1.191 1.642 1.057 1.131 0.968 K 1.769 1.141 1.023 1.020 0.996 1.007 1.004 1.010 1.007 0.994 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.17 1.34 1.69 inf Number in group 974. 933. 938. 920. 963. 933. 946. 922. 947. 942. GooF 1.040 1.045 0.998 1.043 1.334 1.508 1.204 0.816 0.994 0.912 K 0.989 1.011 1.023 1.021 1.009 1.006 1.004 1.003 0.995 0.992 R1 0.086 0.078 0.071 0.059 0.060 0.051 0.041 0.028 0.024 0.020 Recommended weighting scheme: WGHT 0.0234 37.5830 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) -9 5 20 163.38 7773.60 14.34 0.135 0.99 -10 5 16 965.03 9836.02 12.84 0.152 1.01 -10 6 14 458.62 7823.49 12.62 0.135 1.00 -13 4 18 1710.54 10373.76 12.29 0.156 0.86 -6 7 19 7658.86 22735.35 12.11 0.231 1.05 -5 1 20 1100.89 7486.78 11.73 0.133 1.34 -11 3 20 762.64 8051.29 11.71 0.137 0.95 0 15 3 5378.98 17525.33 11.65 0.203 0.79 0 12 9 1051.48 7435.93 11.65 0.132 0.95 -10 3 19 1096.97 7155.41 10.46 0.130 1.02 -5 6 20 16233.41 34062.46 10.25 0.283 1.12 -2 12 13 254.33 4750.30 10.11 0.106 0.91 -12 5 15 104.71 4378.42 10.09 0.101 0.91 -10 2 21 883.80 6671.92 9.77 0.125 1.00 -9 6 13 3222.82 11200.06 9.69 0.162 1.08 -2 4 18 18982.57 35398.24 9.50 0.288 1.42 0 10 14 2510.29 8339.36 9.49 0.140 1.03 -11 5 7 445.98 3939.50 8.81 0.096 1.04 -7 6 21 -138.78 3028.18 8.81 0.084 1.02 2 11 5 2037.54 7519.44 8.76 0.133 1.05 -15 1 16 664.48 5598.67 8.22 0.115 0.81 -1 11 13 186.23 3030.75 8.09 0.084 0.98 -4 0 22 2493.86 7389.21 8.04 0.132 1.28 -3 14 11 5308.50 13586.56 8.03 0.179 0.80 -8 2 20 9656.91 18518.33 8.01 0.208 1.14 -3 6 35 1362.97 7957.69 7.97 0.137 0.77 -12 7 13 -101.00 2507.73 7.64 0.077 0.87 -12 0 20 15825.89 28242.01 7.61 0.257 0.92 -3 11 18 966.32 4390.71 7.46 0.101 0.90 -11 4 18 265.87 3679.38 7.40 0.093 0.96 -11 2 21 6933.48 16593.43 7.23 0.197 0.94 -10 5 21 513.52 3838.06 7.06 0.095 0.93 14 2 14 2757.38 8456.19 7.02 0.141 0.78 5 14 4 6726.31 16351.43 6.87 0.196 0.80 -6 5 12 74238.84 105903.83 6.71 0.498 1.40 -9 5 13 -138.87 1908.27 6.59 0.067 1.13 -7 10 14 6677.19 13752.66 6.14 0.180 0.93 0 11 10 196.85 3700.01 6.12 0.093 1.02 -11 4 21 52.01 2768.17 6.04 0.081 0.91 -6 11 11 2360.51 6090.46 5.86 0.120 0.93 6 14 6 3430.58 8987.33 5.82 0.145 0.77 -6 5 20 2044.47 5478.32 5.74 0.113 1.13 -5 6 17 134.71 1967.68 5.71 0.068 1.21 -1 11 15 165.16 1657.34 5.58 0.062 0.95 -2 11 16 599.25 3464.56 5.53 0.090 0.93 -3 14 7 1589.28 5060.18 5.52 0.109 0.83 -12 2 16 5236.56 9585.99 5.05 0.150 0.96 -3 5 24 9565.58 14788.18 4.77 0.186 1.08 1 14 8 2765.68 6329.50 4.74 0.122 0.83 0 14 1 433.80 4179.94 4.63 0.099 0.85 Bond lengths and angles Au1 - Distance Angles C41 2.0610 (0.0062) P1 2.2823 (0.0016) 171.09 (0.18) Au1 - C41 Au2 - Distance Angles C51 2.0756 (0.0063) P2 2.2825 (0.0017) 175.20 (0.19) Au2 - C51 C1 - Distance Angles C6 1.3953 (0.0087) C2 1.3981 (0.0096) 117.51 (0.63) P1 1.8184 (0.0069) 122.68 (0.54) 119.81 (0.48) C1 - C6 C2 C2 - Distance Angles C3 1.3835 (0.0096) O1 1.3963 (0.0078) 122.18 (0.64) C1 1.3981 (0.0096) 122.82 (0.64) 114.83 (0.59) C2 - C3 O1 C3 - Distance Angles C4 1.3799 (0.0111) C2 1.3835 (0.0096) 118.54 (0.69) H3 0.9500 120.73 120.73 C3 - C4 C2 C4 - Distance Angles C3 1.3799 (0.0110) C5 1.3841 (0.0109) 119.81 (0.74) H4 0.9500 120.09 120.09 C4 - C3 C5 C5 - Distance Angles C4 1.3841 (0.0109) C6 1.3839 (0.0101) 121.51 (0.74) H5 0.9500 119.24 119.24 C5 - C4 C6 C6 - Distance Angles C5 1.3839 (0.0101) C1 1.3953 (0.0087) 119.79 (0.69) H6 0.9500 120.10 120.10 C6 - C5 C1 C7 - Distance Angles C8 1.3872 (0.0087) C12 1.3907 (0.0092) 118.23 (0.56) P2 1.8174 (0.0061) 119.13 (0.49) 122.64 (0.49) C7 - C8 C12 C8 - Distance Angles O1 1.3842 (0.0079) C7 1.3872 (0.0087) 116.34 (0.52) C9 1.4048 (0.0084) 121.42 (0.59) 122.16 (0.64) C8 - O1 C7 C9 - Distance Angles C10 1.3838 (0.0103) C8 1.4048 (0.0084) 118.23 (0.65) H9 0.9500 120.88 120.88 C9 - C10 C8 C10 - Distance Angles C9 1.3838 (0.0104) C11 1.3886 (0.0102) 120.80 (0.60) H10 0.9500 119.60 119.60 C10 - C9 C11 C11 - Distance Angles C10 1.3886 (0.0102) C12 1.3996 (0.0086) 119.75 (0.65) H11 0.9500 120.13 120.13 C11 - C10 C12 C12 - Distance Angles C7 1.3907 (0.0092) C11 1.3996 (0.0086) 120.65 (0.63) H12 0.9500 119.68 119.68 C12 - C7 C11 C13 - Distance Angles C18 1.3945 (0.0092) C14 1.4008 (0.0090) 120.43 (0.59) P1 1.8156 (0.0061) 117.53 (0.48) 122.04 (0.53) C13 - C18 C14 C14 - Distance Angles C15 1.3929 (0.0090) C13 1.4008 (0.0090) 118.29 (0.69) H14 0.9500 120.85 120.85 C14 - C15 C13 C15 - Distance Angles C16 1.3863 (0.0097) C14 1.3929 (0.0090) 121.45 (0.63) H15 0.9500 119.27 119.27 C15 - C16 C14 C16 - Distance Angles C17 1.3791 (0.0101) C15 1.3863 (0.0098) 119.39 (0.60) H16 0.9500 120.30 120.30 C16 - C17 C15 C17 - Distance Angles C16 1.3791 (0.0101) C18 1.3862 (0.0090) 120.71 (0.68) H17 0.9500 119.65 119.65 C17 - C16 C18 C18 - Distance Angles C17 1.3862 (0.0091) C13 1.3945 (0.0093) 119.67 (0.65) H18 0.9500 120.17 120.17 C18 - C17 C13 C19 - Distance Angles C20 1.3895 (0.0095) C24 1.4025 (0.0090) 119.51 (0.66) P1 1.8203 (0.0071) 123.05 (0.50) 117.41 (0.54) C19 - C20 C24 C20 - Distance Angles C19 1.3895 (0.0094) C21 1.3899 (0.0102) 120.00 (0.70) H20 0.9500 120.00 120.00 C20 - C19 C21 C21 - Distance Angles C20 1.3899 (0.0102) C22 1.4048 (0.0120) 119.72 (0.75) H21 0.9500 120.14 120.14 C21 - C20 C22 C22 - Distance Angles C23 1.3649 (0.0122) C21 1.4048 (0.0120) 120.23 (0.71) H22 0.9500 119.89 119.89 C22 - C23 C21 C23 - Distance Angles C22 1.3649 (0.0122) C24 1.3872 (0.0102) 120.46 (0.74) H23 0.9500 119.77 119.77 C23 - C22 C24 C24 - Distance Angles C23 1.3872 (0.0102) C19 1.4025 (0.0091) 120.04 (0.73) H24 0.9500 119.98 119.98 C24 - C23 C19 C25 - Distance Angles C30 1.3866 (0.0089) C26 1.4181 (0.0092) 119.44 (0.62) P2 1.8143 (0.0066) 124.63 (0.53) 115.88 (0.48) C25 - C30 C26 C26 - Distance Angles C27 1.3887 (0.0101) C25 1.4181 (0.0092) 119.67 (0.66) H26 0.9500 120.17 120.17 C26 - C27 C25 C27 - Distance Angles C28 1.3849 (0.0100) C26 1.3887 (0.0101) 119.65 (0.69) H27 0.9500 120.17 120.17 C27 - C28 C26 C28 - Distance Angles C29 1.3810 (0.0105) C27 1.3849 (0.0100) 121.00 (0.68) H28 0.9500 119.50 119.50 C28 - C29 C27 C29 - Distance Angles C28 1.3810 (0.0106) C30 1.3886 (0.0100) 119.94 (0.72) H29 0.9500 120.03 120.03 C29 - C28 C30 C30 - Distance Angles C25 1.3866 (0.0089) C29 1.3886 (0.0100) 120.25 (0.71) H30 0.9500 119.88 119.88 C30 - C25 C29 C31 - Distance Angles C36 1.3876 (0.0091) C32 1.3948 (0.0086) 119.94 (0.64) P2 1.8124 (0.0071) 122.22 (0.50) 117.84 (0.50) C31 - C36 C32 C32 - Distance Angles C33 1.3835 (0.0095) C31 1.3948 (0.0086) 119.39 (0.62) H32 0.9500 120.31 120.31 C32 - C33 C31 C33 - Distance Angles C34 1.3770 (0.0096) C32 1.3835 (0.0095) 120.22 (0.62) H33 0.9500 119.89 119.89 C33 - C34 C32 C34 - Distance Angles C35 1.3643 (0.0095) C33 1.3770 (0.0096) 121.60 (0.64) H34 0.9500 119.20 119.20 C34 - C35 C33 C35 - Distance Angles C34 1.3643 (0.0096) C36 1.4094 (0.0100) 118.84 (0.64) H35 0.9500 120.58 120.58 C35 - C34 C36 C36 - Distance Angles C31 1.3876 (0.0091) C35 1.4094 (0.0100) 119.99 (0.62) H36 0.9500 120.00 120.00 C36 - C31 C35 O1 - Distance Angles C8 1.3842 (0.0079) C2 1.3963 (0.0078) 117.72 (0.49) O1 - C8 P1 - Distance Angles C13 1.8156 (0.0061) C1 1.8184 (0.0069) 105.37 (0.30) C19 1.8203 (0.0072) 106.22 (0.30) 103.50 (0.31) Au1 2.2823 (0.0016) 116.48 (0.22) 116.46 (0.21) 107.62 (0.23) P1 - C13 C1 C19 P2 - Distance Angles C31 1.8124 (0.0071) C25 1.8143 (0.0066) 106.30 (0.29) C7 1.8174 (0.0061) 105.31 (0.29) 101.40 (0.29) Au2 2.2825 (0.0016) 111.25 (0.21) 113.47 (0.20) 117.99 (0.22) P2 - C31 C25 C7 C41 - Distance Angles C46 1.3698 (0.0094) C42 1.3849 (0.0086) 114.74 (0.59) Au1 2.0610 (0.0061) 127.77 (0.47) 117.47 (0.48) C41 - C46 C42 C42 - Distance Angles F42 1.3556 (0.0079) C41 1.3849 (0.0086) 119.51 (0.57) C43 1.3935 (0.0090) 115.83 (0.56) 124.59 (0.64) C42 - F42 C41 C43 - Distance Angles C44 1.3831 (0.0099) C42 1.3935 (0.0090) 117.36 (0.60) Cl43 1.7159 (0.0066) 120.43 (0.51) 122.19 (0.56) C43 - C44 C42 C44 - Distance Angles F44 1.3446 (0.0072) C43 1.3831 (0.0099) 119.50 (0.59) C45 1.3897 (0.0091) 119.33 (0.62) 121.05 (0.61) C44 - F44 C43 C45 - Distance Angles C44 1.3897 (0.0091) C46 1.3946 (0.0087) 117.69 (0.64) Cl45 1.7282 (0.0072) 120.06 (0.51) 122.25 (0.52) C45 - C44 C46 C46 - Distance Angles F46 1.3534 (0.0071) C41 1.3698 (0.0094) 119.31 (0.57) C45 1.3946 (0.0087) 116.16 (0.61) 124.46 (0.60) C46 - F46 C41 F42 - Distance Angles C42 1.3556 (0.0079) F42 - F44 - Distance Angles C44 1.3446 (0.0072) F44 - F46 - Distance Angles C46 1.3534 (0.0071) F46 - Cl43 - Distance Angles C43 1.7159 (0.0067) Cl43 - Cl45 - Distance Angles C45 1.7282 (0.0072) Cl45 - C51 - Distance Angles C52 1.3688 (0.0092) C56 1.3757 (0.0090) 115.38 (0.59) Au2 2.0756 (0.0062) 124.76 (0.49) 119.85 (0.48) C51 - C52 C56 C52 - Distance Angles F52 1.3652 (0.0071) C51 1.3688 (0.0092) 119.61 (0.59) C53 1.3726 (0.0091) 116.27 (0.59) 124.12 (0.60) C52 - F52 C51 C53 - Distance Angles C52 1.3726 (0.0091) C54 1.3874 (0.0089) 118.46 (0.60) Cl53 1.7269 (0.0066) 122.73 (0.51) 118.73 (0.51) C53 - C52 C54 C54 - Distance Angles F54 1.3449 (0.0073) C55 1.3613 (0.0096) 119.56 (0.58) C53 1.3874 (0.0089) 120.04 (0.59) 120.40 (0.62) C54 - F54 C55 C55 - Distance Angles C54 1.3613 (0.0096) C56 1.4031 (0.0096) 118.34 (0.60) Cl55 1.7289 (0.0067) 121.36 (0.55) 120.28 (0.54) C55 - C54 C56 C56 - Distance Angles F56 1.3442 (0.0072) C51 1.3757 (0.0090) 120.11 (0.59) C55 1.4031 (0.0096) 116.66 (0.57) 123.20 (0.60) C56 - F56 C51 F52 - Distance Angles C52 1.3652 (0.0072) F52 - F54 - Distance Angles C54 1.3449 (0.0073) F54 - F56 - Distance Angles C56 1.3442 (0.0072) F56 - Cl53 - Distance Angles C53 1.7269 (0.0066) Cl53 - Cl55 - Distance Angles C55 1.7289 (0.0068) Cl55 - FMAP and GRID set by program FMAP 2 3 34 GRID -0.806 -2 -2 0.806 2 2 R1 = 0.0443 for 9418 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.99 at 0.4690 0.8474 0.2149 [ 1.40 A from H32 ] Deepest hole -0.95 at 0.5574 0.0028 0.1213 [ 1.73 A from H26 ] Mean = 0.00, Rms deviation from mean = 0.21 e/A^3, Highest memory used = 5004 / 36444 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4690 0.6526 0.7149 1.00000 0.05 0.99 1.40 H32 2.00 AU2 2.13 C32 2.61 H29 Q2 1 0.2808 0.5229 0.6264 1.00000 0.05 0.96 0.95 C7 1.08 P2 1.88 C8 1.96 C31 Q3 1 0.4627 0.4780 0.5790 1.00000 0.05 0.95 1.50 H26 1.96 F44 2.32 C26 2.63 P2 Q4 1 0.8128 1.0557 0.6231 1.00000 0.05 0.82 1.32 CL53 2.06 F54 2.23 C53 2.47 C54 Q5 1 0.1856 0.5954 0.6267 1.00000 0.05 0.80 1.59 H36 1.80 C8 1.85 C7 1.91 C36 Shortest distances between peaks (including symmetry equivalents) 2 5 1.49 2 3 2.93 Time profile in seconds ----------------------- 0.13: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: 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 0.02: Analyse other restraints etc. 7.21: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.00: Generate idealized H-atoms 11.14: Structure factors and derivatives 35.22: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.16: Apply other restraints 4.81: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.14: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.17: Fourier summations 0.06: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008src0880 finished at 11:42:14 Total CPU time: 59.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++