+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 17:27:31 on 02-Aug-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 99SRC156 in P2(1)/c CELL 0.71073 10.102 20.609 18.706 90.00 103.59 90.00 ZERR 4.00 0.002 0.004 0.004 0.00 0.03 0.00 LATT 1 SYMM -X, .5+Y, .5-Z SFAC C H O BI UNIT 184 148 24 4 V = 3785.41 F(000) = 1776.0 Mu = 4.71 mm-1 Cell Wt = 3578.94 Rho = 1.570 L.S. 4 BOND FMAP 2 PLAN 10 HFIX 147 O6 O3 OMIT 1 1 1 OMIT -1 2 4 OMIT 2 2 8 WGHT 0.100000 FVAR 0.14333 BI1 4 0.35841 0.35812 0.40245 11.00000 0.01691 0.01498 = 0.01669 0.00037 0.00058 0.00055 O1 3 0.45728 0.26491 0.45695 11.00000 0.02494 0.02086 = 0.01870 0.00026 -0.00208 0.00067 O2 3 0.57259 0.33511 0.53857 11.00000 0.02624 0.01949 = 0.02825 -0.00261 0.00075 -0.00175 O3 3 0.68166 0.24265 0.63318 11.00000 0.03095 0.03255 = 0.01295 -0.00283 -0.00501 0.00478 O4 3 0.26567 0.43883 0.32595 11.00000 0.02683 0.01776 = 0.02438 0.00030 -0.00163 0.00110 O5 3 0.37154 0.50387 0.41569 11.00000 0.02677 0.02448 = 0.02048 0.00466 -0.00052 0.00102 O6 3 0.23542 0.60770 0.34470 11.00000 0.02548 0.01777 = 0.02584 -0.00267 0.00533 0.00284 C1 1 0.54613 0.27935 0.51647 11.00000 0.02049 0.02352 = 0.01714 -0.00078 0.00303 0.00231 C2 1 0.62141 0.22156 0.55960 11.00000 0.02031 0.02345 = 0.01327 -0.00198 -0.00050 0.00123 C3 1 0.51734 0.16891 0.56394 11.00000 0.02256 0.02693 = 0.01885 0.00662 -0.00017 0.00157 C4 1 0.49979 0.11468 0.51934 11.00000 0.02877 0.03035 = 0.03516 0.00345 0.00437 -0.00009 AFIX 43 H4 2 0.55737 0.10764 0.48794 11.00000 -1.20000 AFIX 0 C5 1 0.39595 0.07030 0.52113 11.00000 0.03381 0.03414 = 0.04676 0.00394 -0.00294 -0.00834 AFIX 43 H5 2 0.38516 0.03389 0.49094 11.00000 -1.20000 AFIX 0 C6 1 0.31028 0.07986 0.56670 11.00000 0.02752 0.04437 = 0.05026 0.01861 0.00220 -0.00607 AFIX 43 H6 2 0.24160 0.05009 0.56781 11.00000 -1.20000 AFIX 0 C7 1 0.32657 0.13432 0.61131 11.00000 0.03106 0.07019 = 0.04402 0.01047 0.01529 -0.00365 AFIX 43 H7 2 0.26851 0.14123 0.64248 11.00000 -1.20000 AFIX 0 C8 1 0.42911 0.17854 0.60962 11.00000 0.03400 0.04327 = 0.03257 -0.00090 0.00983 -0.00257 AFIX 43 H8 2 0.43888 0.21513 0.63950 11.00000 -1.20000 AFIX 0 C9 1 0.73645 0.19947 0.52392 11.00000 0.01908 0.02175 = 0.02445 -0.00339 0.00269 -0.00033 C10 1 0.76243 0.22807 0.46197 11.00000 0.03197 0.03035 = 0.02779 0.00393 0.00721 0.00648 AFIX 43 H10 2 0.70336 0.25962 0.43709 11.00000 -1.20000 AFIX 0 C11 1 0.87575 0.21041 0.43617 11.00000 0.03958 0.03322 = 0.03644 0.00272 0.01437 0.00422 AFIX 43 H11 2 0.89157 0.22993 0.39413 11.00000 -1.20000 AFIX 0 C12 1 0.96445 0.16411 0.47273 11.00000 0.02747 0.03503 = 0.04875 -0.00680 0.01078 0.00487 AFIX 43 H12 2 1.04113 0.15285 0.45605 11.00000 -1.20000 AFIX 0 C13 1 0.93905 0.13455 0.53414 11.00000 0.02619 0.02850 = 0.04662 0.00127 0.00613 0.01097 AFIX 43 H13 2 0.99846 0.10299 0.55873 11.00000 -1.20000 AFIX 0 C14 1 0.82524 0.15156 0.55960 11.00000 0.02618 0.02938 = 0.02616 0.00414 0.00274 0.00455 AFIX 43 H14 2 0.80816 0.13087 0.60069 11.00000 -1.20000 AFIX 0 C15 1 0.30268 0.49528 0.35361 11.00000 0.01715 0.02050 = 0.02652 0.00428 0.00615 0.00245 C16 1 0.25598 0.55343 0.30078 11.00000 0.02198 0.01654 = 0.01863 0.00057 0.00258 0.00315 C17 1 0.12082 0.53858 0.24779 11.00000 0.02183 0.01522 = 0.02255 0.00003 0.00213 0.00425 C18 1 0.10169 0.54109 0.17196 11.00000 0.02323 0.02711 = 0.02363 0.00070 0.00414 0.00230 AFIX 43 H18 2 0.17307 0.55408 0.15165 11.00000 -1.20000 AFIX 0 C19 1 -0.02316 0.52438 0.12580 11.00000 0.03266 0.03143 = 0.02145 -0.00387 -0.00226 0.00289 AFIX 43 H19 2 -0.03459 0.52621 0.07504 11.00000 -1.20000 AFIX 0 C20 1 -0.12942 0.50520 0.15526 11.00000 0.02359 0.02691 = 0.03558 -0.00257 -0.00451 -0.00089 AFIX 43 H20 2 -0.21234 0.49340 0.12453 11.00000 -1.20000 AFIX 0 C21 1 -0.11235 0.50351 0.23136 11.00000 0.02061 0.03409 = 0.03968 0.00843 0.00559 -0.00209 AFIX 43 H21 2 -0.18459 0.49146 0.25148 11.00000 -1.20000 AFIX 0 C22 1 0.01105 0.51963 0.27667 11.00000 0.02423 0.03330 = 0.02429 0.00486 0.00601 0.00461 AFIX 43 H22 2 0.02178 0.51791 0.32740 11.00000 -1.20000 AFIX 0 C23 1 0.36924 0.56713 0.26080 11.00000 0.02003 0.02076 = 0.01975 0.00125 0.00009 0.00085 C24 1 0.43067 0.51615 0.23147 11.00000 0.02168 0.02328 = 0.02852 -0.00059 0.00574 -0.00109 AFIX 43 H24 2 0.40686 0.47349 0.23880 11.00000 -1.20000 AFIX 0 C25 1 0.52694 0.52899 0.19151 11.00000 0.02608 0.03582 = 0.03083 -0.00574 0.00797 0.00182 AFIX 43 H25 2 0.56756 0.49471 0.17236 11.00000 -1.20000 AFIX 0 C26 1 0.56336 0.59150 0.17972 11.00000 0.03195 0.04304 = 0.03179 -0.00210 0.01575 -0.00691 AFIX 43 H26 2 0.62836 0.59961 0.15293 11.00000 -1.20000 AFIX 0 C27 1 0.50241 0.64227 0.20809 11.00000 0.05184 0.02663 = 0.05895 0.00634 0.03012 -0.00761 AFIX 43 H27 2 0.52654 0.68479 0.20037 11.00000 -1.20000 AFIX 0 C28 1 0.40515 0.63013 0.24814 11.00000 0.03849 0.02328 = 0.04216 0.00015 0.01864 -0.00047 AFIX 43 H28 2 0.36395 0.66464 0.26655 11.00000 -1.20000 AFIX 0 C29 1 0.21544 0.29307 0.32813 11.00000 0.01864 0.02204 = 0.01984 -0.00533 0.00171 -0.00394 C30 1 0.21004 0.22806 0.34674 11.00000 0.02725 0.02306 = 0.02734 0.00004 0.00071 0.00114 AFIX 43 H30 2 0.27346 0.21102 0.38659 11.00000 -1.20000 AFIX 0 C31 1 0.10919 0.18880 0.30534 11.00000 0.02815 0.02088 = 0.03447 -0.00273 0.00371 -0.00366 AFIX 43 H31 2 0.10481 0.14524 0.31758 11.00000 -1.20000 AFIX 0 C32 1 0.01487 0.21406 0.24581 11.00000 0.02701 0.03199 = 0.03255 -0.00889 0.00102 -0.00668 AFIX 43 H32 2 -0.05221 0.18747 0.21797 11.00000 -1.20000 AFIX 0 C33 1 0.02077 0.27838 0.22809 11.00000 0.03327 0.04064 = 0.02975 0.00168 -0.01174 -0.00436 AFIX 43 H33 2 -0.04336 0.29522 0.18842 11.00000 -1.20000 AFIX 0 C34 1 0.12119 0.31889 0.26853 11.00000 0.03095 0.02640 = 0.02793 0.00454 -0.00320 0.00184 AFIX 43 H34 2 0.12517 0.36238 0.25594 11.00000 -1.20000 AFIX 0 C35 1 0.55373 0.37535 0.37361 11.00000 0.02217 0.02125 = 0.02496 0.00461 0.00553 0.00292 C36 1 0.57074 0.34325 0.31110 11.00000 0.03248 0.03209 = 0.02502 -0.00092 0.00817 0.00142 AFIX 43 H36 2 0.49878 0.32072 0.28125 11.00000 -1.20000 AFIX 0 C37 1 0.69686 0.34541 0.29403 11.00000 0.04344 0.03889 = 0.03485 0.00192 0.01995 0.00714 AFIX 43 H37 2 0.71052 0.32447 0.25231 11.00000 -1.20000 AFIX 0 C38 1 0.80251 0.37905 0.33965 11.00000 0.02816 0.04073 = 0.05121 0.01110 0.02017 0.00462 AFIX 43 H38 2 0.88814 0.37942 0.32927 11.00000 -1.20000 AFIX 0 C39 1 0.78177 0.41215 0.40064 11.00000 0.02907 0.03475 = 0.04716 0.00451 0.00835 -0.00641 AFIX 43 H39 2 0.85291 0.43557 0.42995 11.00000 -1.20000 AFIX 0 C40 1 0.65642 0.41068 0.41827 11.00000 0.02831 0.02465 = 0.03250 -0.00174 0.00592 -0.00247 AFIX 43 H40 2 0.64184 0.43287 0.45903 11.00000 -1.20000 AFIX 0 C41 1 0.26421 0.37567 0.49510 11.00000 0.02374 0.02394 = 0.02187 -0.00025 0.00748 0.00284 C42 1 0.32578 0.41455 0.55356 11.00000 0.02806 0.03019 = 0.02554 -0.00529 0.00507 0.00115 AFIX 43 H42 2 0.40282 0.43888 0.55247 11.00000 -1.20000 AFIX 0 C43 1 0.26824 0.41595 0.61409 11.00000 0.05025 0.03786 = 0.02486 -0.00625 0.00899 0.00180 AFIX 43 H43 2 0.30793 0.44114 0.65473 11.00000 -1.20000 AFIX 0 C44 1 0.15295 0.38037 0.61449 11.00000 0.07323 0.04596 = 0.04092 -0.00548 0.03502 -0.00719 AFIX 43 H44 2 0.11523 0.38190 0.65528 11.00000 -1.20000 AFIX 0 C45 1 0.09296 0.34245 0.55479 11.00000 0.06514 0.05884 = 0.05713 -0.01798 0.04040 -0.02788 AFIX 43 H45 2 0.01468 0.31892 0.55540 11.00000 -1.20000 AFIX 0 C46 1 0.14904 0.33931 0.49389 11.00000 0.03774 0.04706 = 0.04041 -0.01517 0.02175 -0.01759 AFIX 43 H46 2 0.11025 0.31355 0.45359 11.00000 -1.20000 HKLF 4 Covalent radii and connectivity table for 99SRC156 in P2(1)/c C 0.770 H 0.320 O 0.660 BI 1.600 Bi1 - C35 C41 C29 O4 O1 O1 - C1 Bi1 O2 - C1 O3 - C2 O4 - C15 Bi1 O5 - C15 O6 - C16 C1 - O2 O1 C2 C2 - O3 C3 C1 C9 C3 - C4 C8 C2 C4 - C3 C5 C5 - C6 C4 C6 - C5 C7 C7 - C6 C8 C8 - C7 C3 C9 - C10 C14 C2 C10 - C9 C11 C11 - C12 C10 C12 - C11 C13 C13 - C12 C14 C14 - C13 C9 C15 - O5 O4 C16 C16 - O6 C17 C23 C15 C17 - C18 C22 C16 C18 - C17 C19 C19 - C20 C18 C20 - C19 C21 C21 - C22 C20 C22 - C21 C17 C23 - C28 C24 C16 C24 - C25 C23 C25 - C26 C24 C26 - C25 C27 C27 - C26 C28 C28 - C23 C27 C29 - C30 C34 Bi1 C30 - C31 C29 C31 - C32 C30 C32 - C33 C31 C33 - C32 C34 C34 - C29 C33 C35 - C40 C36 Bi1 C36 - C37 C35 C37 - C36 C38 C38 - C37 C39 C39 - C40 C38 C40 - C35 C39 C41 - C46 C42 Bi1 C42 - C41 C43 C43 - C44 C42 C44 - C43 C45 C45 - C44 C46 C46 - C41 C45 h k l Fo^2 Sigma Why rejected -7 0 3 2.70 0.51 observed but should be systematically absent -2 0 1 0.69 0.17 observed but should be systematically absent -2 0 3 2.35 0.54 observed but should be systematically absent -2 0 3 2.54 0.55 observed but should be systematically absent -2 0 3 2.16 0.54 observed but should be systematically absent -1 0 1 1.40 0.35 observed but should be systematically absent 0 0 3 4.75 0.73 observed but should be systematically absent 0 0 3 2.51 0.36 observed but should be systematically absent 0 0 9 8.62 1.72 observed but should be systematically absent 1 0 1 1.63 0.36 observed but should be systematically absent 1 0 1 1.69 0.37 observed but should be systematically absent 1 0 1 2.36 0.34 observed but should be systematically absent 1 0 1 3.02 0.50 observed but should be systematically absent 1 0 1 2.46 0.57 observed but should be systematically absent 1 0 1 1.87 0.37 observed but should be systematically absent 1 0 5 3.10 0.58 observed but should be systematically absent 2 0 5 5.96 1.23 observed but should be systematically absent 2 0 7 3.49 0.58 observed but should be systematically absent 8 0 5 2.16 0.54 observed but should be systematically absent 116458 Reflections read, of which 1851 rejected -13 =< h =< 13, -26 =< k =< 26, -24 =< l =< 24, Max. 2-theta = 55.00 19 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 1 0 0 1117.67 26.38 4 218.59 1 1 0 292.02 3.50 13 23.16 0 9 17 0.68 0.47 11 2.95 3 Inconsistent equivalents 8684 Unique reflections, of which 0 suppressed R(int) = 0.0766 R(sigma) = 0.0254 Friedel opposites merged Maximum memory for data reduction = 4048 / 86435 Default effective X-H distances for T = 20.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 0.98 0.97 0.96 0.93 0.86 0.89 1.10 0.82 0.93 0.86 0.93 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. Difference electron density (eA^-3x100) at 15 degree intervals for AFIX 147 group attached to O3 The center of the range is eclipsed (cis) to C3 and rotation is clockwise looking down C2 to O3 -19 -16 -11 -4 1 3 1 6 24 42 43 27 8 0 2 4 -5 -20 -24 -14 -1 1 -9 -18 Difference electron density (eA^-3x100) at 15 degree intervals for AFIX 147 group attached to O6 The center of the range is eclipsed (cis) to C17 and rotation is clockwise looking down C16 to O6 4 -3 -9 -9 -7 -6 -4 0 1 0 6 20 35 41 41 37 25 8 -3 -1 11 24 25 15 Least-squares cycle 1 Maximum vector length = 511 Memory required = 5377 / 629955 wR2 = 0.0887 before cycle 1 for 8684 data and 480 / 480 parameters GooF = S = 0.759; Restrained GooF = 0.759 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.14323 0.00017 -0.612 OSF 30 0.24231 0.00010 -3.450 y O3 64 0.00303 0.00072 -3.171 U13 O6 Mean shift/esd = 0.259 Maximum = -3.450 for y O3 Max. shift = 0.021 A for H6 Max. dU = 0.000 for C26 Least-squares cycle 2 Maximum vector length = 511 Memory required = 5377 / 629955 wR2 = 0.0878 before cycle 2 for 8684 data and 480 / 480 parameters GooF = S = 0.751; Restrained GooF = 0.751 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.14320 0.00016 -0.170 OSF Mean shift/esd = 0.089 Maximum = -1.099 for U13 O6 Max. shift = 0.011 A for H3 Max. dU = 0.000 for C26 Least-squares cycle 3 Maximum vector length = 511 Memory required = 5377 / 629955 wR2 = 0.0877 before cycle 3 for 8684 data and 480 / 480 parameters GooF = S = 0.751; Restrained GooF = 0.751 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.14320 0.00016 -0.005 OSF Mean shift/esd = 0.006 Maximum = -0.108 for tors H3 Max. shift = 0.004 A for H3 Max. dU = 0.000 for C45 Least-squares cycle 4 Maximum vector length = 511 Memory required = 5377 / 629955 wR2 = 0.0878 before cycle 4 for 8684 data and 480 / 480 parameters GooF = S = 0.751; Restrained GooF = 0.751 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.14320 0.00016 0.000 OSF Mean shift/esd = 0.002 Maximum = -0.037 for tors H3 Max. shift = 0.001 A for H3 Max. dU = 0.000 for C5 Largest correlation matrix elements 0.647 U33 Bi1 / OSF 0.590 U13 C45 / U33 C45 0.516 U13 C44 / U33 C44 0.643 U11 Bi1 / OSF 0.570 U13 C45 / U11 C45 0.506 U13 C44 / U11 C44 0.642 U22 Bi1 / OSF 0.518 U12 C45 / U23 C45 0.502 U13 C27 / U33 C27 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 0.6983 0.2811 0.6333 147 0.820 0.000 O3 C2 H3 H6 0.2949 0.6085 0.3824 147 0.820 0.000 O6 C16 H6 H4 0.5573 0.1076 0.4881 43 0.930 0.000 C4 C3 C5 H5 0.3852 0.0341 0.4907 43 0.930 0.000 C5 C6 C4 H6 0.2415 0.0501 0.5680 43 0.930 0.000 C6 C5 C7 H7 0.2684 0.1413 0.6424 43 0.930 0.000 C7 C6 C8 H8 0.4392 0.2151 0.6398 43 0.930 0.000 C8 C7 C3 H10 0.7033 0.2595 0.4370 43 0.930 0.000 C10 C9 C11 H11 0.8912 0.2298 0.3939 43 0.930 0.000 C11 C12 C10 H12 1.0415 0.1530 0.4564 43 0.930 0.000 C12 C11 C13 H13 0.9981 0.1028 0.5586 43 0.930 0.000 C13 C12 C14 H14 0.8084 0.1310 0.6008 43 0.930 0.000 C14 C13 C9 H18 0.1730 0.5542 0.1516 43 0.930 0.000 C18 C17 C19 H19 -0.0347 0.5260 0.0750 43 0.930 0.000 C19 C20 C18 H20 -0.2123 0.4935 0.1246 43 0.930 0.000 C20 C19 C21 H21 -0.1845 0.4911 0.2512 43 0.930 0.000 C21 C22 C20 H22 0.0217 0.5181 0.3274 43 0.930 0.000 C22 C21 C17 H24 0.4066 0.4735 0.2387 43 0.930 0.000 C24 C25 C23 H25 0.5675 0.4946 0.1723 43 0.930 0.000 C25 C26 C24 H26 0.6284 0.5997 0.1530 43 0.930 0.000 C26 C25 C27 H27 0.5268 0.6847 0.2004 43 0.930 0.000 C27 C26 C28 H28 0.3640 0.6647 0.2665 43 0.930 0.000 C28 C23 C27 H30 0.2730 0.2112 0.3866 43 0.930 0.000 C30 C31 C29 H31 0.1049 0.1453 0.3177 43 0.930 0.000 C31 C32 C30 H32 -0.0523 0.1874 0.2181 43 0.930 0.000 C32 C33 C31 H33 -0.0430 0.2951 0.1881 43 0.930 0.000 C33 C32 C34 H34 0.1248 0.3625 0.2563 43 0.930 0.000 C34 C29 C33 H36 0.4988 0.3207 0.2813 43 0.930 0.000 C36 C37 C35 H37 0.7109 0.3244 0.2525 43 0.930 0.000 C37 C36 C38 H38 0.8881 0.3794 0.3295 43 0.930 0.000 C38 C37 C39 H39 0.8529 0.4355 0.4299 43 0.930 0.000 C39 C40 C38 H40 0.6418 0.4330 0.4590 43 0.930 0.000 C40 C35 C39 H42 0.4028 0.4388 0.5526 43 0.930 0.000 C42 C41 C43 H43 0.3076 0.4413 0.6545 43 0.930 0.000 C43 C44 C42 H44 0.1154 0.3817 0.6554 43 0.930 0.000 C44 C43 C45 H45 0.0145 0.3191 0.5554 43 0.930 0.000 C45 C44 C46 H46 0.1101 0.3136 0.4536 43 0.930 0.000 C46 C41 C45 99SRC156 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Bi1 0.35841 0.35812 0.40245 1.00000 0.01686 0.01493 0.01666 0.00037 0.00056 0.00055 0.01671 0.00015 0.00001 0.00000 0.00000 0.00000 0.00008 0.00008 0.00008 0.00003 0.00005 0.00003 0.00006 O1 0.45730 0.26484 0.45699 1.00000 0.02466 0.02064 0.01954 0.00056 -0.00173 0.00092 0.02276 0.00336 0.00019 0.00009 0.00009 0.00000 0.00092 0.00087 0.00085 0.00069 0.00069 0.00072 0.00037 O2 0.57258 0.33505 0.53858 1.00000 0.02601 0.02010 0.02824 -0.00254 0.00083 -0.00201 0.02570 0.00354 0.00020 0.00009 0.00011 0.00000 0.00101 0.00091 0.00099 0.00078 0.00078 0.00079 0.00040 O3 0.68142 0.24221 0.63313 1.00000 0.03260 0.02852 0.01491 -0.00260 -0.00446 0.00357 0.02701 0.00351 0.00021 0.00010 0.00009 0.00000 0.00107 0.00103 0.00090 0.00075 0.00075 0.00087 0.00043 H3 0.69830 0.28113 0.63325 1.00000 0.04051 0.00000 0.00000 O4 0.26565 0.43878 0.32597 1.00000 0.02691 0.01770 0.02468 0.00062 -0.00110 0.00124 0.02428 0.00341 0.00019 0.00009 0.00010 0.00000 0.00099 0.00087 0.00094 0.00070 0.00075 0.00072 0.00040 O5 0.37152 0.50402 0.41565 1.00000 0.02654 0.02407 0.02103 0.00453 0.00002 0.00108 0.02480 0.00377 0.00019 0.00010 0.00010 0.00000 0.00104 0.00102 0.00090 0.00077 0.00076 0.00073 0.00043 O6 0.23493 0.60763 0.34433 1.00000 0.02443 0.01974 0.02303 -0.00313 0.00225 0.00230 0.02295 0.00329 0.00018 0.00008 0.00010 0.00000 0.00094 0.00090 0.00090 0.00070 0.00070 0.00071 0.00037 H6 0.29495 0.60848 0.38242 1.00000 0.03443 0.00000 0.00000 C1 0.54616 0.27936 0.51662 1.00000 0.02007 0.02257 0.01812 -0.00031 0.00364 0.00289 0.02039 0.00463 0.00025 0.00012 0.00013 0.00000 0.00123 0.00125 0.00117 0.00095 0.00094 0.00097 0.00050 C2 0.62123 0.22167 0.55964 1.00000 0.02012 0.02334 0.01334 -0.00123 -0.00047 0.00160 0.01966 0.00478 0.00027 0.00013 0.00013 0.00000 0.00124 0.00130 0.00117 0.00092 0.00093 0.00097 0.00053 C3 0.51736 0.16892 0.56387 1.00000 0.02220 0.02768 0.01928 0.00666 0.00015 0.00199 0.02383 0.00500 0.00026 0.00013 0.00014 0.00000 0.00129 0.00138 0.00122 0.00102 0.00098 0.00104 0.00053 C4 0.49964 0.11469 0.51942 1.00000 0.02886 0.02988 0.03515 0.00302 0.00435 -0.00004 0.03182 0.00558 0.00030 0.00014 0.00016 0.00000 0.00150 0.00154 0.00158 0.00122 0.00119 0.00118 0.00062 H4 0.55733 0.10759 0.48809 1.00000 0.03818 0.00000 0.00000 C5 0.39602 0.07042 0.52104 1.00000 0.03349 0.03427 0.04681 0.00403 -0.00284 -0.00791 0.04023 0.00596 0.00033 0.00015 0.00019 0.00000 0.00167 0.00163 0.00184 0.00136 0.00137 0.00127 0.00074 H5 0.38517 0.03410 0.49072 1.00000 0.04827 0.00000 0.00000 C6 0.31006 0.07989 0.56680 1.00000 0.02827 0.04442 0.05012 0.01870 0.00245 -0.00583 0.04206 0.00665 0.00032 0.00017 0.00019 0.00000 0.00158 0.00189 0.00194 0.00154 0.00136 0.00135 0.00078 H6 0.24146 0.05010 0.56798 1.00000 0.05047 0.00000 0.00000 C7 0.32656 0.13437 0.61128 1.00000 0.03128 0.07039 0.04327 0.01000 0.01518 -0.00407 0.04725 0.00804 0.00041 0.00019 0.00023 0.00000 0.00195 0.00264 0.00222 0.00165 0.00166 0.00152 0.00095 H7 0.26837 0.14135 0.64236 1.00000 0.05670 0.00000 0.00000 C8 0.42923 0.17857 0.60979 1.00000 0.03425 0.04354 0.03193 -0.00081 0.00965 -0.00249 0.03626 0.00607 0.00032 0.00016 0.00017 0.00000 0.00165 0.00183 0.00156 0.00131 0.00125 0.00134 0.00068 H8 0.43924 0.21506 0.63984 1.00000 0.04351 0.00000 0.00000 C9 0.73641 0.19937 0.52397 1.00000 0.01901 0.02153 0.02456 -0.00299 0.00261 -0.00015 0.02211 0.00470 0.00026 0.00012 0.00014 0.00000 0.00122 0.00125 0.00126 0.00096 0.00096 0.00094 0.00051 C10 0.76242 0.22800 0.46184 1.00000 0.03151 0.03077 0.02771 0.00367 0.00742 0.00653 0.02992 0.00554 0.00030 0.00014 0.00015 0.00000 0.00148 0.00145 0.00138 0.00111 0.00112 0.00114 0.00059 H10 0.70332 0.25954 0.43696 1.00000 0.03591 0.00000 0.00000 C11 0.87555 0.21036 0.43599 1.00000 0.03966 0.03353 0.03647 0.00249 0.01428 0.00427 0.03567 0.00618 0.00032 0.00015 0.00017 0.00000 0.00171 0.00154 0.00167 0.00128 0.00129 0.00129 0.00066 H11 0.89123 0.22975 0.39385 1.00000 0.04280 0.00000 0.00000 C12 0.96449 0.16410 0.47285 1.00000 0.02778 0.03485 0.04897 -0.00634 0.01141 0.00508 0.03681 0.00610 0.00031 0.00016 0.00018 0.00000 0.00155 0.00156 0.00189 0.00144 0.00135 0.00129 0.00067 H12 1.04145 0.15297 0.45637 1.00000 0.04417 0.00000 0.00000 C13 0.93893 0.13450 0.53408 1.00000 0.02599 0.02860 0.04597 0.00061 0.00568 0.01113 0.03398 0.00662 0.00034 0.00014 0.00021 0.00000 0.00164 0.00148 0.00199 0.00123 0.00143 0.00111 0.00072 H13 0.99812 0.10281 0.55856 1.00000 0.04078 0.00000 0.00000 C14 0.82527 0.15162 0.55960 1.00000 0.02593 0.02942 0.02623 0.00417 0.00260 0.00409 0.02778 0.00590 0.00031 0.00014 0.00017 0.00000 0.00154 0.00138 0.00151 0.00109 0.00118 0.00109 0.00061 H14 0.80839 0.13102 0.60080 1.00000 0.03333 0.00000 0.00000 C15 0.30279 0.49542 0.35360 1.00000 0.01657 0.02140 0.02547 0.00449 0.00556 0.00243 0.02104 0.00518 0.00026 0.00012 0.00015 0.00000 0.00121 0.00125 0.00134 0.00101 0.00102 0.00096 0.00052 C16 0.25598 0.55345 0.30082 1.00000 0.02165 0.01634 0.01955 0.00091 0.00303 0.00339 0.01948 0.00461 0.00025 0.00012 0.00013 0.00000 0.00123 0.00108 0.00117 0.00091 0.00094 0.00092 0.00048 C17 0.12097 0.53855 0.24793 1.00000 0.02222 0.01472 0.02234 -0.00024 0.00193 0.00393 0.02031 0.00460 0.00025 0.00011 0.00013 0.00000 0.00125 0.00112 0.00121 0.00091 0.00096 0.00091 0.00049 C18 0.10170 0.54109 0.17194 1.00000 0.02348 0.02720 0.02326 0.00069 0.00438 0.00226 0.02483 0.00495 0.00027 0.00013 0.00014 0.00000 0.00129 0.00135 0.00128 0.00101 0.00102 0.00103 0.00053 H18 0.17300 0.55416 0.15160 1.00000 0.02980 0.00000 0.00000 C19 -0.02324 0.52429 0.12576 1.00000 0.03292 0.03091 0.02171 -0.00386 -0.00206 0.00309 0.02992 0.00520 0.00029 0.00014 0.00015 0.00000 0.00153 0.00143 0.00130 0.00109 0.00109 0.00118 0.00060 H19 -0.03470 0.52604 0.07499 1.00000 0.03590 0.00000 0.00000 C20 -0.12931 0.50517 0.15528 1.00000 0.02392 0.02628 0.03618 -0.00263 -0.00408 -0.00083 0.03064 0.00511 0.00029 0.00013 0.00016 0.00000 0.00140 0.00134 0.00152 0.00113 0.00113 0.00108 0.00061 H20 -0.21230 0.49346 0.12456 1.00000 0.03677 0.00000 0.00000 C21 -0.11230 0.50337 0.23111 1.00000 0.02073 0.03427 0.03912 0.00868 0.00519 -0.00195 0.03168 0.00557 0.00028 0.00014 0.00016 0.00000 0.00137 0.00154 0.00160 0.00124 0.00115 0.00111 0.00062 H21 -0.18452 0.49113 0.25115 1.00000 0.03802 0.00000 0.00000 C22 0.01122 0.51967 0.27673 1.00000 0.02373 0.03306 0.02448 0.00491 0.00596 0.00463 0.02704 0.00555 0.00028 0.00014 0.00015 0.00000 0.00138 0.00146 0.00132 0.00111 0.00107 0.00112 0.00058 H22 0.02170 0.51808 0.32745 1.00000 0.03245 0.00000 0.00000 C23 0.36914 0.56714 0.26071 1.00000 0.02010 0.02058 0.02005 0.00117 0.00035 0.00063 0.02097 0.00460 0.00026 0.00012 0.00013 0.00000 0.00121 0.00121 0.00119 0.00093 0.00094 0.00093 0.00050 C24 0.43056 0.51613 0.23137 1.00000 0.02165 0.02339 0.02836 -0.00060 0.00585 -0.00103 0.02447 0.00488 0.00026 0.00013 0.00014 0.00000 0.00129 0.00125 0.00132 0.00102 0.00103 0.00098 0.00053 H24 0.40664 0.47348 0.23867 1.00000 0.02936 0.00000 0.00000 C25 0.52691 0.52888 0.19145 1.00000 0.02605 0.03575 0.03069 -0.00573 0.00782 0.00213 0.03064 0.00535 0.00029 0.00014 0.00015 0.00000 0.00139 0.00152 0.00143 0.00117 0.00112 0.00117 0.00059 H25 0.56752 0.49460 0.17230 1.00000 0.03677 0.00000 0.00000 C26 0.56337 0.59152 0.17974 1.00000 0.03153 0.04260 0.03146 -0.00159 0.01535 -0.00735 0.03388 0.00578 0.00031 0.00016 0.00016 0.00000 0.00156 0.00168 0.00152 0.00127 0.00123 0.00128 0.00064 H26 0.62839 0.59967 0.15297 1.00000 0.04066 0.00000 0.00000 C27 0.50255 0.64221 0.20811 1.00000 0.05161 0.02722 0.05744 0.00650 0.02886 -0.00802 0.04276 0.00783 0.00043 0.00013 0.00023 0.00000 0.00242 0.00177 0.00244 0.00123 0.00199 0.00123 0.00093 H27 0.52683 0.68472 0.20043 1.00000 0.05131 0.00000 0.00000 C28 0.40515 0.63018 0.24812 1.00000 0.03821 0.02310 0.04248 0.00070 0.01852 -0.00024 0.03310 0.00651 0.00034 0.00015 0.00019 0.00000 0.00176 0.00127 0.00182 0.00124 0.00144 0.00122 0.00067 H28 0.36398 0.66470 0.26652 1.00000 0.03972 0.00000 0.00000 C29 0.21525 0.29307 0.32795 1.00000 0.01800 0.02253 0.01908 -0.00518 0.00075 -0.00390 0.02047 0.00454 0.00025 0.00013 0.00014 0.00000 0.00121 0.00123 0.00118 0.00096 0.00093 0.00096 0.00050 C30 0.20968 0.22819 0.34666 1.00000 0.02700 0.02292 0.02772 0.00005 0.00053 0.00134 0.02685 0.00507 0.00028 0.00013 0.00015 0.00000 0.00138 0.00129 0.00134 0.00103 0.00107 0.00105 0.00055 H30 0.27300 0.21125 0.38661 1.00000 0.03222 0.00000 0.00000 C31 0.10915 0.18882 0.30542 1.00000 0.02834 0.02111 0.03445 -0.00291 0.00381 -0.00404 0.02856 0.00505 0.00028 0.00013 0.00015 0.00000 0.00144 0.00125 0.00149 0.00109 0.00113 0.00107 0.00057 H31 0.10488 0.14527 0.31773 1.00000 0.03427 0.00000 0.00000 C32 0.01489 0.21405 0.24589 1.00000 0.02666 0.03224 0.03199 -0.00863 0.00040 -0.00629 0.03137 0.00521 0.00030 0.00014 0.00016 0.00000 0.00145 0.00149 0.00150 0.00120 0.00116 0.00119 0.00062 H32 -0.05226 0.18745 0.21813 1.00000 0.03765 0.00000 0.00000 C33 0.02079 0.27833 0.22799 1.00000 0.03245 0.03956 0.03083 0.00148 -0.01240 -0.00470 0.03757 0.00551 0.00033 0.00016 0.00017 0.00000 0.00160 0.00173 0.00152 0.00127 0.00122 0.00130 0.00072 H33 -0.04305 0.29508 0.18814 1.00000 0.04508 0.00000 0.00000 C34 0.12109 0.31895 0.26866 1.00000 0.03130 0.02635 0.02797 0.00417 -0.00309 0.00216 0.03021 0.00557 0.00031 0.00015 0.00016 0.00000 0.00154 0.00140 0.00144 0.00112 0.00116 0.00115 0.00062 H34 0.12478 0.36250 0.25629 1.00000 0.03625 0.00000 0.00000 C35 0.55368 0.37524 0.37357 1.00000 0.02216 0.02126 0.02471 0.00456 0.00550 0.00303 0.02271 0.00532 0.00027 0.00013 0.00015 0.00000 0.00130 0.00114 0.00132 0.00107 0.00103 0.00105 0.00051 C36 0.57070 0.34320 0.31119 1.00000 0.03278 0.03191 0.02506 -0.00129 0.00859 0.00145 0.02962 0.00655 0.00035 0.00017 0.00017 0.00000 0.00170 0.00138 0.00151 0.00126 0.00125 0.00134 0.00063 H36 0.49876 0.32067 0.28133 1.00000 0.03554 0.00000 0.00000 C37 0.69710 0.34536 0.29415 1.00000 0.04315 0.03847 0.03546 0.00200 0.02037 0.00679 0.03718 0.00716 0.00037 0.00016 0.00019 0.00000 0.00195 0.00156 0.00174 0.00137 0.00148 0.00147 0.00072 H37 0.71089 0.32441 0.25246 1.00000 0.04462 0.00000 0.00000 C38 0.80245 0.37900 0.33978 1.00000 0.02805 0.04117 0.05065 0.01136 0.01985 0.00452 0.03820 0.00700 0.00032 0.00017 0.00019 0.00000 0.00159 0.00169 0.00196 0.00154 0.00143 0.00136 0.00070 H38 0.88812 0.37939 0.32945 1.00000 0.04584 0.00000 0.00000 C39 0.78170 0.41207 0.40060 1.00000 0.02854 0.03476 0.04770 0.00453 0.00862 -0.00637 0.03706 0.00619 0.00032 0.00015 0.00019 0.00000 0.00155 0.00159 0.00183 0.00134 0.00133 0.00124 0.00068 H39 0.85290 0.43547 0.42989 1.00000 0.04447 0.00000 0.00000 C40 0.65640 0.41075 0.41833 1.00000 0.02844 0.02490 0.03206 -0.00126 0.00559 -0.00249 0.02872 0.00546 0.00029 0.00014 0.00016 0.00000 0.00144 0.00137 0.00150 0.00112 0.00114 0.00110 0.00058 H40 0.64181 0.43301 0.45904 1.00000 0.03446 0.00000 0.00000 C41 0.26428 0.37577 0.49511 1.00000 0.02386 0.02349 0.02194 -0.00032 0.00735 0.00299 0.02277 0.00519 0.00027 0.00014 0.00014 0.00000 0.00134 0.00119 0.00128 0.00104 0.00102 0.00107 0.00051 C42 0.32566 0.41452 0.55356 1.00000 0.02780 0.02998 0.02539 -0.00472 0.00485 0.00131 0.02795 0.00520 0.00028 0.00013 0.00015 0.00000 0.00141 0.00139 0.00134 0.00106 0.00107 0.00110 0.00057 H42 0.40284 0.43877 0.55256 1.00000 0.03355 0.00000 0.00000 C43 0.26807 0.41599 0.61395 1.00000 0.05026 0.03760 0.02499 -0.00594 0.00867 0.00199 0.03765 0.00600 0.00035 0.00015 0.00016 0.00000 0.00195 0.00166 0.00146 0.00120 0.00132 0.00140 0.00070 H43 0.30758 0.44133 0.65450 1.00000 0.04518 0.00000 0.00000 C44 0.15289 0.38031 0.61450 1.00000 0.07267 0.04617 0.04106 -0.00541 0.03506 -0.00710 0.04970 0.00816 0.00042 0.00022 0.00022 0.00000 0.00279 0.00212 0.00180 0.00182 0.00177 0.00184 0.00093 H44 0.11543 0.38170 0.65538 1.00000 0.05964 0.00000 0.00000 C45 0.09290 0.34256 0.55480 1.00000 0.06508 0.05865 0.05710 -0.01830 0.04025 -0.02762 0.05598 0.00823 0.00048 0.00022 0.00024 0.00000 0.00277 0.00216 0.00259 0.00209 0.00222 0.00214 0.00111 H45 0.01449 0.31912 0.55536 1.00000 0.06718 0.00000 0.00000 C46 0.14892 0.33938 0.49387 1.00000 0.03727 0.04710 0.04058 -0.01458 0.02180 -0.01727 0.03955 0.00669 0.00037 0.00020 0.00020 0.00000 0.00192 0.00179 0.00190 0.00167 0.00153 0.00166 0.00077 H46 0.11011 0.31361 0.45357 1.00000 0.04746 0.00000 0.00000 Final Structure Factor Calculation for 99SRC156 in P2(1)/c Total number of l.s. parameters = 480 Maximum vector length = 511 Memory required = 4897 / 22995 wR2 = 0.0878 before cycle 5 for 8684 data and 0 / 480 parameters GooF = S = 0.751; Restrained GooF = 0.751 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0267 for 7696 Fo > 4sig(Fo) and 0.0319 for all 8684 data wR2 = 0.0878, GooF = S = 0.751, Restrained GooF = 0.751 for all data Occupancy sum of asymmetric unit = 53.00 for non-hydrogen and 37.00 for hydrogen atoms Principal mean square atomic displacements U 0.0212 0.0152 0.0137 Bi1 0.0316 0.0208 0.0159 O1 0.0345 0.0244 0.0182 O2 0.0420 0.0268 0.0122 O3 0.0353 0.0204 0.0172 O4 0.0322 0.0258 0.0164 O5 0.0300 0.0212 0.0177 O6 0.0248 0.0185 0.0178 C1 0.0258 0.0212 0.0120 C2 0.0319 0.0257 0.0139 C3 0.0385 0.0293 0.0276 C4 0.0609 0.0346 0.0252 C5 0.0712 0.0293 0.0256 C6 0.0742 0.0431 0.0245 C7 0.0442 0.0343 0.0303 C8 0.0277 0.0205 0.0182 C9 0.0379 0.0280 0.0239 C10 0.0445 0.0322 0.0304 C11 0.0517 0.0363 0.0224 C12 0.0478 0.0381 0.0160 C13 0.0324 0.0307 0.0202 C14 0.0284 0.0192 0.0156 C15 0.0242 0.0197 0.0145 C16 0.0275 0.0204 0.0130 C17 0.0283 0.0244 0.0218 C18 0.0425 0.0289 0.0184 C19 0.0464 0.0265 0.0190 C20 0.0470 0.0278 0.0203 C21 0.0362 0.0237 0.0212 C22 0.0258 0.0208 0.0162 C23 0.0285 0.0238 0.0211 C24 0.0400 0.0286 0.0233 C25 0.0470 0.0346 0.0201 C26 0.0678 0.0424 0.0181 C27 0.0479 0.0284 0.0230 C28 0.0263 0.0228 0.0123 C29 0.0352 0.0236 0.0218 C30 0.0372 0.0297 0.0188 C31 0.0413 0.0351 0.0177 C32 0.0589 0.0384 0.0154 C33 0.0430 0.0286 0.0190 C34 0.0280 0.0227 0.0174 C35 0.0339 0.0313 0.0237 C36 0.0519 0.0362 0.0235 C37 0.0599 0.0342 0.0205 C38 0.0504 0.0373 0.0235 C39 0.0331 0.0296 0.0235 C40 0.0267 0.0228 0.0188 C41 0.0342 0.0272 0.0224 C42 0.0513 0.0396 0.0221 C43 0.0814 0.0444 0.0233 C44 0.1026 0.0400 0.0253 C45 0.0684 0.0290 0.0212 C46 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.018 0.036 0.056 0.079 0.107 0.137 0.169 0.209 0.270 1.000 Number in group 869. 873. 867. 874. 866. 876. 851. 865. 870. 873. GooF 0.932 1.082 0.942 0.834 0.648 0.537 0.536 0.585 0.626 0.527 K 0.866 0.904 0.956 0.965 0.974 0.994 1.019 1.039 1.044 1.001 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.65 inf Number in group 872. 897. 857. 866. 856. 874. 854. 869. 864. 875. GooF 0.830 0.809 0.830 0.759 0.759 0.735 0.702 0.613 0.594 0.827 K 1.012 1.023 1.035 1.040 1.049 1.043 1.042 1.036 1.013 0.969 R1 0.058 0.051 0.046 0.039 0.035 0.030 0.027 0.022 0.015 0.023 Recommended weighting scheme: WGHT 0.0436 1.3457 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) -4 9 5 206.61 117.76 5.35 0.023 1.62 -2 3 2 200.83 132.92 5.25 0.024 3.95 2 8 0 38.61 88.07 5.20 0.020 2.28 3 2 0 243.75 161.58 5.05 0.027 3.12 -4 2 1 537.38 379.70 4.71 0.041 2.44 0 12 2 963.28 708.58 4.18 0.057 1.69 -5 8 20 385.01 200.07 4.04 0.030 0.86 6 17 2 4.78 107.88 3.97 0.022 0.95 0 9 5 1501.72 1125.24 3.97 0.071 1.94 9 17 2 -16.29 183.63 3.96 0.029 0.80 -4 9 19 350.24 538.78 3.95 0.049 0.89 -9 0 20 206.41 447.42 3.91 0.045 0.80 9 8 10 41.44 285.36 3.89 0.036 0.81 -4 24 8 27.70 213.63 3.88 0.031 0.78 4 3 20 11.04 262.46 3.86 0.034 0.79 -4 17 16 -52.48 94.41 3.81 0.021 0.83 1 2 10 163.56 110.99 3.72 0.022 1.69 2 11 2 144.15 208.27 3.64 0.031 1.69 4 11 0 224.55 316.92 3.64 0.038 1.49 3 9 16 81.36 11.73 3.64 0.007 0.92 2 2 1 963.83 743.44 3.62 0.058 4.11 1 7 0 148.22 204.04 3.55 0.030 2.82 -11 0 14 416.28 731.55 3.55 0.057 0.83 0 18 5 -6.63 53.28 3.54 0.016 1.09 -9 16 13 -65.37 103.09 3.51 0.022 0.78 -4 4 3 631.74 840.68 3.51 0.062 2.24 -7 9 20 331.54 509.14 3.47 0.048 0.81 4 2 0 87.14 56.18 3.47 0.016 2.39 1 0 0 54504.08 87709.16 3.47 0.629 9.82 3 20 8 576.20 795.55 3.45 0.060 0.88 -2 5 3 136.58 98.22 3.45 0.021 2.99 -1 19 5 -14.78 48.62 3.45 0.015 1.04 -3 12 12 50.36 4.47 3.45 0.004 1.14 -8 3 19 155.02 44.08 3.42 0.014 0.85 -9 2 10 37.62 108.40 3.41 0.022 1.05 -4 18 5 72.92 151.94 3.37 0.026 1.03 0 17 13 63.59 137.31 3.36 0.025 0.92 -3 3 20 40.07 132.96 3.33 0.024 0.93 4 5 11 96.10 51.94 3.32 0.015 1.19 8 5 13 -22.54 109.65 3.32 0.022 0.81 -6 14 1 118.35 189.57 3.31 0.029 1.10 8 5 4 -26.76 38.14 3.31 0.013 1.08 -5 22 7 198.93 68.83 3.28 0.018 0.83 3 3 0 205.04 268.91 3.23 0.035 2.95 0 14 15 45.65 120.43 3.22 0.023 0.94 11 2 2 54.23 207.10 3.22 0.031 0.87 -12 5 13 617.83 326.60 3.21 0.038 0.78 8 15 7 59.31 203.86 3.20 0.030 0.82 4 18 5 8.86 98.14 3.17 0.021 0.97 -4 13 9 24.12 74.32 3.16 0.018 1.18 Bond lengths and angles Bi1 - Distance Angles C35 2.1928 (0.0027) C41 2.1943 (0.0026) 138.58 (0.10) C29 2.2101 (0.0025) 115.82 (0.10) 104.94 (0.10) O4 2.2490 (0.0018) 89.36 (0.09) 100.77 (0.09) 86.22 (0.09) O1 2.2925 (0.0018) 85.49 (0.08) 90.68 (0.09) 85.64 (0.08) 167.36 (0.07) Bi1 - C35 C41 C29 O4 O1 - Distance Angles C1 1.2919 (0.0030) Bi1 2.2925 (0.0018) 109.37 (0.15) O1 - C1 O2 - Distance Angles C1 1.2270 (0.0032) O2 - O3 - Distance Angles C2 1.4304 (0.0032) O3 - O4 - Distance Angles C15 1.2958 (0.0032) Bi1 2.2490 (0.0018) 111.95 (0.16) O4 - C15 O5 - Distance Angles C15 1.2173 (0.0030) O5 - O6 - Distance Angles C16 1.4270 (0.0029) O6 - C1 - Distance Angles O2 1.2270 (0.0032) O1 1.2919 (0.0030) 123.92 (0.23) C2 1.5328 (0.0035) 120.53 (0.22) 115.55 (0.21) C1 - O2 O1 C2 - Distance Angles O3 1.4304 (0.0032) C3 1.5258 (0.0037) 107.65 (0.21) C1 1.5328 (0.0035) 108.73 (0.20) 108.57 (0.21) C9 1.5412 (0.0036) 108.10 (0.22) 114.11 (0.21) 109.56 (0.21) C2 - O3 C3 C1 C3 - Distance Angles C4 1.3794 (0.0042) C8 1.3891 (0.0040) 118.53 (0.27) C2 1.5258 (0.0037) 122.64 (0.24) 118.59 (0.25) C3 - C4 C8 C4 - Distance Angles C3 1.3794 (0.0042) C5 1.3943 (0.0041) 120.58 (0.29) C4 - C3 C5 - Distance Angles C6 1.3690 (0.0050) C4 1.3943 (0.0041) 120.67 (0.31) C5 - C6 C6 - Distance Angles C5 1.3690 (0.0050) C7 1.3839 (0.0054) 119.15 (0.31) C6 - C5 C7 - Distance Angles C6 1.3839 (0.0054) C8 1.3857 (0.0048) 120.41 (0.35) C7 - C6 C8 - Distance Angles C7 1.3857 (0.0048) C3 1.3891 (0.0040) 120.65 (0.32) C8 - C7 C9 - Distance Angles C10 1.3824 (0.0038) C14 1.3920 (0.0038) 118.41 (0.26) C2 1.5412 (0.0036) 123.28 (0.23) 118.10 (0.24) C9 - C10 C14 C10 - Distance Angles C9 1.3824 (0.0038) C11 1.3898 (0.0040) 121.00 (0.27) C10 - C9 C11 - Distance Angles C12 1.3786 (0.0045) C10 1.3898 (0.0040) 119.96 (0.29) C11 - C12 C12 - Distance Angles C11 1.3786 (0.0045) C13 1.3746 (0.0050) 119.72 (0.28) C12 - C11 C13 - Distance Angles C12 1.3746 (0.0050) C14 1.3887 (0.0045) 120.40 (0.28) C13 - C12 C14 - Distance Angles C13 1.3887 (0.0045) C9 1.3920 (0.0038) 120.48 (0.28) C14 - C13 C15 - Distance Angles O5 1.2173 (0.0030) O4 1.2958 (0.0032) 123.93 (0.23) C16 1.5522 (0.0034) 120.97 (0.24) 115.08 (0.22) C15 - O5 O4 C16 - Distance Angles O6 1.4270 (0.0029) C17 1.5163 (0.0034) 107.39 (0.19) C23 1.5337 (0.0035) 111.29 (0.20) 112.19 (0.20) C15 1.5522 (0.0034) 107.70 (0.19) 110.60 (0.20) 107.59 (0.20) C16 - O6 C17 C23 C17 - Distance Angles C18 1.3897 (0.0036) C22 1.3970 (0.0038) 118.16 (0.24) C16 1.5163 (0.0034) 123.24 (0.23) 118.58 (0.22) C17 - C18 C22 C18 - Distance Angles C17 1.3897 (0.0036) C19 1.3952 (0.0037) 120.85 (0.25) C18 - C17 C19 - Distance Angles C20 1.3734 (0.0042) C18 1.3952 (0.0037) 120.00 (0.26) C19 - C20 C20 - Distance Angles C19 1.3734 (0.0042) C21 1.3887 (0.0042) 119.83 (0.26) C20 - C19 C21 - Distance Angles C22 1.3776 (0.0039) C20 1.3887 (0.0042) 120.19 (0.27) C21 - C22 C22 - Distance Angles C21 1.3776 (0.0039) C17 1.3970 (0.0038) 120.96 (0.25) C22 - C21 C23 - Distance Angles C28 1.3841 (0.0037) C24 1.3970 (0.0036) 118.73 (0.25) C16 1.5337 (0.0035) 120.78 (0.23) 120.31 (0.22) C23 - C28 C24 C24 - Distance Angles C25 1.3840 (0.0038) C23 1.3970 (0.0036) 120.17 (0.25) C24 - C25 C25 - Distance Angles C26 1.3740 (0.0043) C24 1.3840 (0.0038) 120.88 (0.27) C25 - C26 C26 - Distance Angles C25 1.3740 (0.0043) C27 1.3797 (0.0046) 119.33 (0.27) C26 - C25 C27 - Distance Angles C26 1.3797 (0.0046) C28 1.3914 (0.0047) 120.46 (0.27) C27 - C26 C28 - Distance Angles C23 1.3841 (0.0037) C27 1.3914 (0.0048) 120.41 (0.28) C28 - C23 C29 - Distance Angles C30 1.3866 (0.0036) C34 1.3868 (0.0037) 120.78 (0.24) Bi1 2.2101 (0.0025) 119.02 (0.18) 119.68 (0.20) C29 - C30 C34 C30 - Distance Angles C31 1.3844 (0.0038) C29 1.3866 (0.0036) 119.51 (0.25) C30 - C31 C31 - Distance Angles C32 1.3852 (0.0041) C30 1.3844 (0.0038) 120.24 (0.26) C31 - C32 C32 - Distance Angles C33 1.3711 (0.0044) C31 1.3852 (0.0041) 119.86 (0.26) C32 - C33 C33 - Distance Angles C32 1.3711 (0.0044) C34 1.3942 (0.0042) 120.97 (0.27) C33 - C32 C34 - Distance Angles C29 1.3868 (0.0037) C33 1.3942 (0.0042) 118.64 (0.28) C34 - C29 C35 - Distance Angles C40 1.3802 (0.0040) C36 1.3862 (0.0042) 122.61 (0.27) Bi1 2.1928 (0.0027) 121.83 (0.21) 115.31 (0.22) C35 - C40 C36 C36 - Distance Angles C37 1.3876 (0.0047) C35 1.3862 (0.0042) 118.74 (0.31) C36 - C37 C37 - Distance Angles C36 1.3876 (0.0047) C38 1.3837 (0.0051) 119.36 (0.31) C37 - C36 C38 - Distance Angles C37 1.3837 (0.0051) C39 1.3839 (0.0048) 120.71 (0.29) C38 - C37 C39 - Distance Angles C40 1.3820 (0.0043) C38 1.3839 (0.0048) 120.78 (0.30) C39 - C40 C40 - Distance Angles C35 1.3802 (0.0040) C39 1.3820 (0.0043) 117.73 (0.28) C40 - C35 C41 - Distance Angles C46 1.3815 (0.0043) C42 1.3780 (0.0038) 123.26 (0.27) Bi1 2.1943 (0.0026) 114.65 (0.21) 121.67 (0.20) C41 - C46 C42 C42 - Distance Angles C41 1.3780 (0.0038) C43 1.3873 (0.0040) 117.53 (0.27) C42 - C41 C43 - Distance Angles C44 1.3785 (0.0049) C42 1.3873 (0.0040) 120.70 (0.29) C43 - C44 C44 - Distance Angles C43 1.3785 (0.0049) C45 1.3790 (0.0060) 120.40 (0.33) C44 - C43 C45 - Distance Angles C44 1.3790 (0.0060) C46 1.3881 (0.0049) 120.35 (0.36) C45 - C44 C46 - Distance Angles C41 1.3815 (0.0043) C45 1.3881 (0.0049) 117.75 (0.32) C46 - C41 FMAP and GRID set by program FMAP 2 3 84 GRID -1.235 -1 24 1.235 1 1 R1 = 0.0310 for 8684 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 3.00 at 0.3603 0.3591 0.4022 [ 0.03 A from BI1 ] Deepest hole -1.99 at 0.3309 0.3312 0.3881 [ 0.65 A from BI1 ] Mean = 0.00, Rms deviation from mean = 0.11 e/A^3, Highest memory used = 4789 /101433 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.0767 0.1429 0.2921 1.00000 0.05 2.16 1.73 H32 1.78 H31 2.03 C32 2.06 C31 Q2 1 0.6417 0.0754 0.5980 1.00000 0.05 1.96 1.97 C4 2.02 H20 2.03 H14 2.14 H4 Q3 1 0.3756 0.3895 0.4612 1.00000 0.05 0.60 1.25 BI1 1.44 C41 1.95 H42 1.98 C42 Q4 1 0.4800 0.3586 0.3951 1.00000 0.05 0.59 0.99 C35 1.27 BI1 2.02 C36 2.04 C40 Q5 1 0.3960 0.3318 0.4662 1.00000 0.05 0.53 1.28 BI1 1.54 O1 1.80 C41 1.92 C1 Q6 1 0.3167 0.3285 0.3410 1.00000 0.05 0.52 1.24 C29 1.28 BI1 2.13 C34 2.31 H34 Q7 1 0.3541 0.3910 0.3426 1.00000 0.05 0.49 1.30 BI1 1.32 O4 1.99 C35 2.23 C15 Q8 1 0.3211 0.3880 0.4435 1.00000 0.05 0.49 1.12 BI1 1.26 C41 2.12 C42 2.27 H42 Q9 1 0.2357 0.3577 0.4064 1.00000 0.05 0.46 1.26 BI1 1.66 C41 1.93 H46 1.96 C29 Q10 1 0.3069 0.3291 0.4480 1.00000 0.05 0.42 1.25 BI1 1.44 C41 1.99 C46 1.99 O1 Shortest distances between peaks (including symmetry equivalents) 3 8 0.57 5 10 0.89 9 10 1.10 8 9 1.15 3 5 1.21 8 10 1.23 6 7 1.34 5 8 1.39 3 10 1.42 4 7 1.56 3 9 1.67 6 9 1.73 5 9 1.82 4 5 1.82 4 6 1.83 3 4 1.91 7 8 1.99 7 9 2.00 6 10 2.03 4 8 2.11 3 7 2.18 6 8 2.27 4 10 2.28 5 6 2.29 7 10 2.49 3 6 2.52 4 9 2.53 5 7 2.56 Time profile in seconds ----------------------- 0.20: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.03: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 16.22: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.77: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 6.31: Structure factors and derivatives 13.25: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.05: Apply other restraints 1.39: Solve l.s. equations 0.00: Generate HTAB table 0.06: Other dependent quantities, CIF, tables 0.20: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.47: Fourier summations 0.22: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 17:28:13 Total CPU time: 39.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++