+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0685a started at 15:24:17 on 22-Jul-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0685a in P2(1)2(1)2(1) CELL 0.71073 9.3572 11.0999 25.9334 90.000 90.000 90.000 ZERR 4.00 0.0001 0.0002 0.0005 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H O UNIT 96 128 60 V = 2693.55 F(000) = 1184.0 Mu = 0.12 mm-1 Cell Wt = 2241.98 Rho = 1.382 MERG 4 OMIT -3.00 55.00 SHEL 7 0.77 FMAP 2 PLAN 20 SIZE 0.10 0.12 0.20 ACTA BOND $H WGHT 0.01080 1.72760 L.S. 10 TEMP -153.00 FVAR 0.54820 MOLE 1 C1 1 0.495154 0.564338 0.355370 11.00000 0.02390 0.03561 = 0.02074 -0.00327 -0.00181 0.00231 AFIX 13 H1 2 0.414372 0.619918 0.346920 11.00000 -1.20000 AFIX 0 C2 1 0.559589 0.515688 0.305539 11.00000 0.02033 0.03321 = 0.02208 -0.00025 -0.00297 0.00111 AFIX 13 H2 2 0.483692 0.475550 0.284519 11.00000 -1.20000 AFIX 0 C3 1 0.626855 0.618048 0.274688 11.00000 0.02405 0.02970 = 0.01562 -0.00441 -0.00136 0.00399 AFIX 13 H3 2 0.549415 0.670087 0.260194 11.00000 -1.20000 AFIX 0 C4 1 0.725117 0.694408 0.307536 11.00000 0.02402 0.02751 = 0.01751 -0.00054 -0.00237 0.00359 AFIX 13 H4 2 0.814380 0.648993 0.316004 11.00000 -1.20000 AFIX 0 C5 1 0.648625 0.732428 0.356681 11.00000 0.02403 0.03454 = 0.02067 -0.00509 -0.00552 0.00155 AFIX 13 H5 2 0.566185 0.786487 0.348514 11.00000 -1.20000 AFIX 0 C6 1 0.442747 0.466927 0.391218 11.00000 0.03202 0.04181 = 0.02291 0.00168 0.00118 -0.00044 AFIX 23 H6A 2 0.517620 0.405018 0.396251 11.00000 -1.20000 H6B 2 0.417625 0.501460 0.425228 11.00000 -1.20000 AFIX 0 C7 1 0.265567 0.313885 0.389447 11.00000 0.04350 0.03259 = 0.03725 0.00209 0.01438 0.00724 C8 1 0.132377 0.272808 0.363375 11.00000 0.05374 0.03274 = 0.03922 -0.00412 0.01210 -0.00903 AFIX 137 H8A 2 0.156041 0.240111 0.329327 11.00000 -1.50000 H8B 2 0.066958 0.341132 0.359416 11.00000 -1.50000 H8C 2 0.086494 0.210154 0.384227 11.00000 -1.50000 AFIX 0 C9 1 0.678456 0.328070 0.290791 11.00000 0.02904 0.02643 = 0.03436 0.00135 0.00970 -0.00573 C10 1 0.775724 0.238811 0.315246 11.00000 0.03866 0.02753 = 0.05794 0.00506 0.00669 0.00248 AFIX 137 H10A 2 0.726036 0.161550 0.318855 11.00000 -1.50000 H10B 2 0.804539 0.267973 0.349365 11.00000 -1.50000 H10C 2 0.860685 0.228100 0.293630 11.00000 -1.50000 AFIX 0 C11 1 0.638433 0.537839 0.189862 11.00000 0.03960 0.03589 = 0.01978 -0.00680 -0.00539 0.00208 C12 1 0.731528 0.476554 0.151676 11.00000 0.04870 0.04163 = 0.02856 -0.01220 0.00466 -0.00420 AFIX 137 H12A 2 0.725606 0.389164 0.156615 11.00000 -1.50000 H12B 2 0.830569 0.502993 0.156461 11.00000 -1.50000 H12C 2 0.699885 0.497032 0.116736 11.00000 -1.50000 AFIX 0 C13 1 0.898962 0.831343 0.273656 11.00000 0.03587 0.03805 = 0.01931 -0.00817 -0.00183 -0.00242 C14 1 0.914805 0.956053 0.252977 11.00000 0.05109 0.03614 = 0.05861 -0.00051 0.00523 -0.00708 AFIX 137 H14A 2 0.911725 1.013877 0.281512 11.00000 -1.50000 H14B 2 0.836648 0.973029 0.228895 11.00000 -1.50000 H14C 2 1.006450 0.963172 0.234940 11.00000 -1.50000 AFIX 0 C15 1 0.684695 0.861537 0.428648 11.00000 0.02335 0.03223 = 0.01855 -0.00726 0.00220 0.00053 AFIX 13 H15 2 0.581874 0.839374 0.433178 11.00000 -1.20000 AFIX 0 C16 1 0.698398 0.993913 0.414843 11.00000 0.02344 0.03817 = 0.02114 0.00235 -0.00560 0.00070 AFIX 13 H16 2 0.648306 1.007161 0.381256 11.00000 -1.20000 AFIX 0 C17 1 0.937605 0.980624 0.443729 11.00000 0.02294 0.04700 = 0.02358 -0.00255 -0.00124 -0.00286 AFIX 43 H17 2 1.031105 1.013885 0.444782 11.00000 -1.20000 AFIX 0 C18 1 0.909361 0.893003 0.477116 11.00000 0.02217 0.03814 = 0.01975 -0.00278 -0.00273 0.00560 AFIX 43 H18 2 0.979917 0.870707 0.501667 11.00000 -1.20000 AFIX 0 C19 1 0.769684 0.829084 0.476882 11.00000 0.02989 0.02798 = 0.01684 -0.00195 0.00164 0.00230 AFIX 13 H19 2 0.786484 0.740134 0.477713 11.00000 -1.20000 AFIX 0 C20 1 0.636112 1.080698 0.453865 11.00000 0.02905 0.03102 = 0.02836 0.00040 -0.00264 -0.00028 AFIX 23 H20A 2 0.691930 1.078011 0.486274 11.00000 -1.20000 H20B 2 0.638939 1.163977 0.440237 11.00000 -1.20000 AFIX 0 C21 1 0.429106 1.090661 0.505896 11.00000 0.03745 0.06445 = 0.02500 -0.00839 -0.00562 0.00880 C22 1 0.278042 1.048543 0.512061 11.00000 0.03543 0.06372 = 0.03728 0.00111 0.00097 0.00438 AFIX 137 H22A 2 0.261307 1.025699 0.548060 11.00000 -1.50000 H22B 2 0.261446 0.978728 0.489717 11.00000 -1.50000 H22C 2 0.212505 1.113639 0.502439 11.00000 -1.50000 AFIX 0 C23 1 0.706482 0.810800 0.565886 11.00000 0.03487 0.03104 = 0.02077 0.00314 -0.00143 -0.01279 C24 1 0.599072 0.846230 0.605473 11.00000 0.03935 0.04131 = 0.02184 -0.00014 0.00404 -0.01047 AFIX 137 H24A 2 0.510460 0.801031 0.599859 11.00000 -1.50000 H24B 2 0.579599 0.932735 0.602687 11.00000 -1.50000 H24C 2 0.636489 0.828233 0.639917 11.00000 -1.50000 AFIX 0 O1 3 0.601391 0.628516 0.383874 11.00000 0.02937 0.03771 = 0.01776 -0.00243 -0.00195 0.00017 O2 3 0.317822 0.414429 0.367105 11.00000 0.03627 0.03352 = 0.02612 0.00146 0.00080 -0.00499 O3 3 0.322219 0.268433 0.426427 11.00000 0.05106 0.06282 = 0.07319 0.03544 0.00298 0.00806 O4 3 0.666799 0.428514 0.320290 11.00000 0.02390 0.02991 = 0.02628 -0.00180 -0.00312 0.00229 O5 3 0.616364 0.314692 0.250599 11.00000 0.04402 0.03006 = 0.03461 -0.00696 0.00209 -0.01049 O6 3 0.712320 0.570571 0.232797 11.00000 0.02627 0.02748 = 0.01694 -0.00559 -0.00060 0.00101 O7 3 0.513431 0.556258 0.184919 11.00000 0.03864 0.07978 = 0.03102 -0.01999 -0.01434 0.01224 O8 3 0.758884 0.802958 0.279566 11.00000 0.02789 0.02727 = 0.02348 -0.00207 -0.00174 0.00095 O9 3 0.995580 0.764312 0.284118 11.00000 0.02851 0.05885 = 0.04130 0.01496 0.00095 0.00118 O10 3 0.747608 0.791722 0.387567 11.00000 0.02464 0.04563 = 0.02143 -0.01407 -0.00250 0.00061 O11 3 0.846433 1.027507 0.408239 11.00000 0.02775 0.04436 = 0.02612 0.00912 -0.00164 -0.00530 O12 3 0.490704 1.044746 0.463356 11.00000 0.02756 0.03316 = 0.02788 -0.00199 -0.00251 0.00229 O13 3 0.490262 1.156007 0.534858 11.00000 0.04908 0.14405 = 0.05977 -0.06549 -0.00083 -0.00919 O14 3 0.676998 0.863464 0.520174 11.00000 0.03082 0.03404 = 0.01645 0.00177 0.00065 0.00121 O15 3 0.807389 0.744975 0.572230 11.00000 0.04566 0.04244 = 0.02978 0.01253 -0.00190 0.00545 HKLF 4 Covalent radii and connectivity table for 2009src0685a in P2(1)2(1)2(1) C 0.770 H 0.320 O 0.660 C1 - O1 C6 C2 C2 - O4 C1 C3 C3 - O6 C4 C2 C4 - O8 C3 C5 C5 - O10 O1 C4 C6 - O2 C1 C7 - O3 O2 C8 C8 - C7 C9 - O5 O4 C10 C10 - C9 C11 - O7 O6 C12 C12 - C11 C13 - O9 O8 C14 C14 - C13 C15 - O10 C16 C19 C16 - O11 C20 C15 C17 - C18 O11 C18 - C17 C19 C19 - O14 C18 C15 C20 - O12 C16 C21 - O13 O12 C22 C22 - C21 C23 - O15 O14 C24 C24 - C23 O1 - C5 C1 O2 - C7 C6 O3 - C7 O4 - C9 C2 O5 - C9 O6 - C11 C3 O7 - C11 O8 - C13 C4 O9 - C13 O10 - C5 C15 O11 - C17 C16 O12 - C21 C20 O13 - C21 O14 - C23 C19 O15 - C23 h k l Fo^2 Sigma Why rejected 7 0 0 4.45 1.00 observed but should be systematically absent 28928 Reflections read, of which 146 rejected -12 =< h =< 12, -12 =< k =< 14, -33 =< l =< 31, Max. 2-theta = 54.96 1 Systematic absence violations 0 Inconsistent equivalents 3484 Unique reflections, of which 0 suppressed R(int) = 0.0497 R(sigma) = 0.0330 Friedel opposites merged Maximum memory for data reduction = 3418 / 34335 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 = 4436 / 452826 wR2 = 0.0901 before cycle 1 for 3484 data and 358 / 358 parameters GooF = S = 1.155; Restrained GooF = 1.155 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0108 * P )^2 + 1.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.54759 0.00075 -0.813 OSF Mean shift/su = 0.152 Maximum = -0.813 for OSF Max. shift = 0.008 A for H10A Max. dU = 0.000 for C1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4436 / 452826 wR2 = 0.0898 before cycle 2 for 3484 data and 358 / 358 parameters GooF = S = 1.152; Restrained GooF = 1.152 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0108 * P )^2 + 1.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.54732 0.00075 -0.366 OSF Mean shift/su = 0.055 Maximum = -0.366 for OSF Max. shift = 0.005 A for H10A Max. dU = 0.000 for C1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4436 / 452826 wR2 = 0.0898 before cycle 3 for 3484 data and 358 / 358 parameters GooF = S = 1.152; Restrained GooF = 1.152 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0108 * P )^2 + 1.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.54731 0.00075 -0.010 OSF Mean shift/su = 0.004 Maximum = 0.054 for tors H10A Max. shift = 0.001 A for H10B Max. dU = 0.000 for C24 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4436 / 452826 wR2 = 0.0897 before cycle 4 for 3484 data and 358 / 358 parameters GooF = S = 1.152; Restrained GooF = 1.152 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0108 * P )^2 + 1.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.54731 0.00075 -0.001 OSF Mean shift/su = 0.001 Maximum = 0.017 for tors H10A Max. shift = 0.000 A for H10C Max. dU = 0.000 for C12 Least-squares cycle 5 Maximum vector length = 511 Memory required = 4436 / 452826 wR2 = 0.0897 before cycle 5 for 3484 data and 358 / 358 parameters GooF = S = 1.152; Restrained GooF = 1.152 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0108 * P )^2 + 1.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.54731 0.00075 0.001 OSF Mean shift/su = 0.000 Maximum = 0.006 for tors H12A Max. shift = 0.000 A for H12C Max. dU = 0.000 for C10 Least-squares cycle 6 Maximum vector length = 511 Memory required = 4436 / 452826 wR2 = 0.0897 before cycle 6 for 3484 data and 358 / 358 parameters GooF = S = 1.152; Restrained GooF = 1.152 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0108 * P )^2 + 1.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.54731 0.00075 0.000 OSF Mean shift/su = 0.000 Maximum = 0.003 for tors H12A Max. shift = 0.000 A for H12C Max. dU = 0.000 for C7 Least-squares cycle 7 Maximum vector length = 511 Memory required = 4436 / 452826 wR2 = 0.0897 before cycle 7 for 3484 data and 358 / 358 parameters GooF = S = 1.152; Restrained GooF = 1.152 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0108 * P )^2 + 1.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.54731 0.00075 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for tors H12A Max. shift = 0.000 A for H12A Max. dU = 0.000 for O3 Least-squares cycle 8 Maximum vector length = 511 Memory required = 4436 / 452826 wR2 = 0.0897 before cycle 8 for 3484 data and 358 / 358 parameters GooF = S = 1.152; Restrained GooF = 1.152 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0108 * P )^2 + 1.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.54731 0.00075 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for tors H12A Max. shift = 0.000 A for H12B Max. dU = 0.000 for C22 Least-squares cycle 9 Maximum vector length = 511 Memory required = 4436 / 452826 wR2 = 0.0897 before cycle 9 for 3484 data and 358 / 358 parameters GooF = S = 1.152; Restrained GooF = 1.152 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0108 * P )^2 + 1.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.54731 0.00075 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H12C Max. dU = 0.000 for O13 Least-squares cycle 10 Maximum vector length = 511 Memory required = 4436 / 452826 wR2 = 0.0897 before cycle 10 for 3484 data and 358 / 358 parameters GooF = S = 1.152; Restrained GooF = 1.152 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0108 * P )^2 + 1.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.54731 0.00075 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z O14 Max. shift = 0.000 A for H12C Max. dU = 0.000 for O3 Largest correlation matrix elements -0.511 U23 O13 / U22 O13 Idealized hydrogen atom generation before cycle 11 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.4144 0.6201 0.3469 13 1.000 0.000 C1 O1 C6 C2 H2 0.4837 0.4754 0.2845 13 1.000 0.000 C2 O4 C1 C3 H3 0.5494 0.6703 0.2602 13 1.000 0.000 C3 O6 C4 C2 H4 0.8146 0.6490 0.3159 13 1.000 0.000 C4 O8 C3 C5 H5 0.5660 0.7865 0.3486 13 1.000 0.000 C5 O10 O1 C4 H6A 0.5176 0.4050 0.3962 23 0.990 0.000 C6 O2 C1 H6B 0.4176 0.5014 0.4253 23 0.990 0.000 C6 O2 C1 H8A 0.1560 0.2396 0.3294 137 0.980 0.000 C8 C7 H8A H8B 0.0671 0.3410 0.3593 137 0.980 0.000 C8 C7 H8A H8C 0.0865 0.2102 0.3844 137 0.980 0.000 C8 C7 H8A H10A 0.7266 0.1612 0.3184 137 0.980 0.000 C10 C9 H10A H10B 0.8034 0.2674 0.3496 137 0.980 0.000 C10 C9 H10A H10C 0.8614 0.2290 0.2939 137 0.980 0.000 C10 C9 H10A H12A 0.7251 0.3891 0.1565 137 0.980 0.000 C12 C11 H12A H12B 0.8307 0.5025 0.1566 137 0.980 0.000 C12 C11 H12A H12C 0.7004 0.4974 0.1167 137 0.980 0.000 C12 C11 H12A H14A 0.9110 1.0141 0.2815 137 0.980 0.000 C14 C13 H14A H14B 0.8370 0.9731 0.2287 137 0.980 0.000 C14 C13 H14A H14C 1.0067 0.9636 0.2351 137 0.980 0.000 C14 C13 H14A H15 0.5819 0.8393 0.4332 13 1.000 0.000 C15 O10 C16 C19 H16 0.6483 1.0072 0.3813 13 1.000 0.000 C16 O11 C20 C15 H17 1.0312 1.0140 0.4448 43 0.950 0.000 C17 C18 O11 H18 0.9799 0.8705 0.5017 43 0.950 0.000 C18 C17 C19 H19 0.7864 0.7401 0.4777 13 1.000 0.000 C19 O14 C18 C15 H20A 0.6919 1.0783 0.4863 23 0.990 0.000 C20 O12 C16 H20B 0.6389 1.1641 0.4402 23 0.990 0.000 C20 O12 C16 H22A 0.2610 1.0258 0.5480 137 0.980 0.000 C22 C21 H22A H22B 0.2614 0.9789 0.4897 137 0.980 0.000 C22 C21 H22A H22C 0.2125 1.1138 0.5024 137 0.980 0.000 C22 C21 H22A H24A 0.5102 0.8015 0.5996 137 0.980 0.000 C24 C23 H24A H24B 0.5802 0.9328 0.6029 137 0.980 0.000 C24 C23 H24A H24C 0.6361 0.8275 0.6399 137 0.980 0.000 C24 C23 H24A 2009src0685a in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.49514 0.56448 0.35538 1.00000 0.02370 0.03482 0.02026 -0.00305 -0.00154 0.00251 0.02626 0.00494 0.00031 0.00028 0.00010 0.00000 0.00134 0.00160 0.00135 0.00127 0.00119 0.00136 0.00062 H1 0.41439 0.62008 0.34693 1.00000 0.03152 0.00000 0.00000 C2 0.55956 0.51555 0.30555 1.00000 0.02010 0.03359 0.02191 -0.00035 -0.00289 0.00117 0.02520 0.00502 0.00029 0.00027 0.00011 0.00000 0.00127 0.00158 0.00136 0.00128 0.00114 0.00126 0.00061 H2 0.48366 0.47541 0.28453 1.00000 0.03024 0.00000 0.00000 C3 0.62683 0.61819 0.27470 1.00000 0.02454 0.02974 0.01551 -0.00414 -0.00153 0.00367 0.02326 0.00471 0.00030 0.00027 0.00010 0.00000 0.00139 0.00148 0.00124 0.00115 0.00111 0.00126 0.00059 H3 0.54941 0.67026 0.26022 1.00000 0.02791 0.00000 0.00000 C4 0.72532 0.69443 0.30749 1.00000 0.02386 0.02694 0.01724 -0.00098 -0.00210 0.00331 0.02268 0.00470 0.00030 0.00025 0.00010 0.00000 0.00135 0.00140 0.00128 0.00115 0.00114 0.00121 0.00058 H4 0.81461 0.64902 0.31593 1.00000 0.02722 0.00000 0.00000 C5 0.64850 0.73243 0.35673 1.00000 0.02420 0.03394 0.02024 -0.00479 -0.00531 0.00186 0.02612 0.00478 0.00031 0.00028 0.00010 0.00000 0.00141 0.00161 0.00136 0.00125 0.00116 0.00131 0.00064 H5 0.56604 0.78647 0.34857 1.00000 0.03135 0.00000 0.00000 C6 0.44272 0.46690 0.39123 1.00000 0.03221 0.04121 0.02227 0.00220 0.00082 -0.00102 0.03189 0.00534 0.00033 0.00030 0.00011 0.00000 0.00152 0.00183 0.00142 0.00140 0.00130 0.00148 0.00070 H6A 0.51760 0.40498 0.39623 1.00000 0.03827 0.00000 0.00000 H6B 0.41762 0.50135 0.42526 1.00000 0.03827 0.00000 0.00000 C7 0.26560 0.31388 0.38940 1.00000 0.04383 0.03273 0.03622 0.00200 0.01390 0.00739 0.03759 0.00627 0.00037 0.00030 0.00013 0.00000 0.00190 0.00167 0.00178 0.00153 0.00161 0.00158 0.00078 C8 0.13243 0.27264 0.36343 1.00000 0.05395 0.03271 0.03860 -0.00445 0.01203 -0.00855 0.04175 0.00597 0.00040 0.00032 0.00013 0.00000 0.00216 0.00176 0.00183 0.00150 0.00169 0.00171 0.00085 H8A 0.15604 0.23959 0.32944 1.00000 0.06263 0.00000 0.00000 H8B 0.06707 0.34097 0.35935 1.00000 0.06263 0.00000 0.00000 H8C 0.08650 0.21023 0.38440 1.00000 0.06263 0.00000 0.00000 C9 0.67854 0.32800 0.29079 1.00000 0.02877 0.02659 0.03431 0.00117 0.01040 -0.00584 0.02989 0.00550 0.00034 0.00027 0.00012 0.00000 0.00152 0.00151 0.00167 0.00130 0.00139 0.00135 0.00067 C10 0.77576 0.23881 0.31523 1.00000 0.03862 0.02700 0.05774 0.00584 0.00718 0.00275 0.04112 0.00634 0.00037 0.00029 0.00014 0.00000 0.00182 0.00162 0.00221 0.00160 0.00173 0.00152 0.00083 H10A 0.72658 0.16120 0.31835 1.00000 0.06168 0.00000 0.00000 H10B 0.80339 0.26739 0.34957 1.00000 0.06168 0.00000 0.00000 H10C 0.86140 0.22904 0.29388 1.00000 0.06168 0.00000 0.00000 C11 0.63840 0.53787 0.18986 1.00000 0.03930 0.03584 0.01937 -0.00670 -0.00496 0.00229 0.03150 0.00520 0.00034 0.00030 0.00011 0.00000 0.00179 0.00172 0.00139 0.00132 0.00131 0.00149 0.00070 C12 0.73155 0.47648 0.15169 1.00000 0.04830 0.04155 0.02813 -0.01227 0.00450 -0.00371 0.03933 0.00562 0.00037 0.00031 0.00012 0.00000 0.00195 0.00187 0.00159 0.00146 0.00152 0.00175 0.00080 H12A 0.72507 0.38907 0.15649 1.00000 0.05899 0.00000 0.00000 H12B 0.83070 0.50247 0.15664 1.00000 0.05899 0.00000 0.00000 H12C 0.70037 0.49736 0.11674 1.00000 0.05899 0.00000 0.00000 C13 0.89902 0.83123 0.27365 1.00000 0.03565 0.03726 0.01942 -0.00748 -0.00167 -0.00290 0.03077 0.00525 0.00035 0.00030 0.00011 0.00000 0.00168 0.00177 0.00142 0.00133 0.00133 0.00151 0.00070 C14 0.91481 0.95626 0.25297 1.00000 0.05090 0.03615 0.05786 -0.00016 0.00493 -0.00665 0.04830 0.00661 0.00042 0.00032 0.00015 0.00000 0.00223 0.00194 0.00230 0.00181 0.00199 0.00183 0.00094 H14A 0.91104 1.01405 0.28151 1.00000 0.07245 0.00000 0.00000 H14B 0.83701 0.97306 0.22872 1.00000 0.07245 0.00000 0.00000 H14C 1.00674 0.96362 0.23515 1.00000 0.07245 0.00000 0.00000 C15 0.68470 0.86149 0.42865 1.00000 0.02325 0.03156 0.01864 -0.00738 0.00269 0.00048 0.02448 0.00478 0.00031 0.00026 0.00010 0.00000 0.00134 0.00155 0.00128 0.00117 0.00115 0.00130 0.00060 H15 0.58188 0.83933 0.43319 1.00000 0.02938 0.00000 0.00000 C16 0.69842 0.99400 0.41488 1.00000 0.02342 0.03790 0.02106 0.00238 -0.00557 0.00078 0.02746 0.00492 0.00029 0.00028 0.00011 0.00000 0.00139 0.00168 0.00142 0.00130 0.00117 0.00137 0.00065 H16 0.64834 1.00724 0.38129 1.00000 0.03295 0.00000 0.00000 C17 0.93769 0.98070 0.44371 1.00000 0.02250 0.04681 0.02323 -0.00308 -0.00096 -0.00291 0.03085 0.00527 0.00032 0.00031 0.00011 0.00000 0.00135 0.00193 0.00145 0.00143 0.00121 0.00145 0.00070 H17 1.03116 1.01403 0.44476 1.00000 0.03702 0.00000 0.00000 C18 0.90938 0.89287 0.47714 1.00000 0.02240 0.03754 0.01964 -0.00297 -0.00264 0.00586 0.02653 0.00503 0.00030 0.00028 0.00011 0.00000 0.00136 0.00166 0.00135 0.00130 0.00120 0.00131 0.00064 H18 0.97992 0.87049 0.50168 1.00000 0.03183 0.00000 0.00000 C19 0.76966 0.82905 0.47687 1.00000 0.03008 0.02717 0.01656 -0.00224 0.00212 0.00210 0.02460 0.00489 0.00031 0.00027 0.00010 0.00000 0.00146 0.00146 0.00129 0.00114 0.00120 0.00126 0.00061 H19 0.78640 0.74010 0.47771 1.00000 0.02952 0.00000 0.00000 C20 0.63613 1.08084 0.45385 1.00000 0.02842 0.03070 0.02844 0.00042 -0.00235 -0.00075 0.02919 0.00511 0.00031 0.00028 0.00011 0.00000 0.00152 0.00161 0.00150 0.00131 0.00127 0.00135 0.00067 H20A 0.69192 1.07826 0.48626 1.00000 0.03502 0.00000 0.00000 H20B 0.63888 1.16409 0.44018 1.00000 0.03502 0.00000 0.00000 C21 0.42917 1.09074 0.50596 1.00000 0.03816 0.06415 0.02473 -0.00830 -0.00645 0.00921 0.04234 0.00629 0.00038 0.00037 0.00012 0.00000 0.00185 0.00253 0.00160 0.00170 0.00145 0.00189 0.00090 C22 0.27793 1.04867 0.51205 1.00000 0.03504 0.06390 0.03692 0.00125 0.00148 0.00455 0.04529 0.00651 0.00036 0.00038 0.00014 0.00000 0.00179 0.00248 0.00184 0.00183 0.00154 0.00184 0.00090 H22A 0.26104 1.02580 0.54803 1.00000 0.06793 0.00000 0.00000 H22B 0.26137 0.97889 0.48968 1.00000 0.06793 0.00000 0.00000 H22C 0.21249 1.11382 0.50240 1.00000 0.06793 0.00000 0.00000 C23 0.70652 0.81089 0.56586 1.00000 0.03445 0.03118 0.02041 0.00312 -0.00186 -0.01254 0.02868 0.00493 0.00034 0.00028 0.00011 0.00000 0.00165 0.00160 0.00143 0.00125 0.00127 0.00147 0.00067 C24 0.59906 0.84619 0.60543 1.00000 0.03918 0.04012 0.02189 -0.00004 0.00379 -0.01045 0.03373 0.00539 0.00034 0.00030 0.00011 0.00000 0.00173 0.00184 0.00144 0.00137 0.00139 0.00155 0.00073 H24A 0.51019 0.80152 0.59960 1.00000 0.05060 0.00000 0.00000 H24B 0.58021 0.93284 0.60289 1.00000 0.05060 0.00000 0.00000 H24C 0.63608 0.82745 0.63986 1.00000 0.05060 0.00000 0.00000 O1 0.60142 0.62851 0.38388 1.00000 0.02985 0.03791 0.01741 -0.00243 -0.00206 0.00035 0.02839 0.00339 0.00021 0.00019 0.00007 0.00000 0.00105 0.00118 0.00094 0.00091 0.00086 0.00098 0.00046 O2 0.31789 0.41451 0.36712 1.00000 0.03564 0.03347 0.02607 0.00142 0.00093 -0.00489 0.03173 0.00361 0.00024 0.00019 0.00008 0.00000 0.00113 0.00115 0.00102 0.00092 0.00093 0.00103 0.00048 O3 0.32219 0.26858 0.42648 1.00000 0.05084 0.06258 0.07298 0.03534 0.00282 0.00720 0.06213 0.00552 0.00031 0.00026 0.00011 0.00000 0.00160 0.00177 0.00185 0.00158 0.00153 0.00150 0.00080 O4 0.66685 0.42849 0.32027 1.00000 0.02352 0.02934 0.02614 -0.00188 -0.00285 0.00212 0.02634 0.00333 0.00021 0.00018 0.00007 0.00000 0.00097 0.00107 0.00100 0.00085 0.00086 0.00090 0.00044 O5 0.61634 0.31469 0.25060 1.00000 0.04426 0.02981 0.03445 -0.00658 0.00202 -0.01076 0.03617 0.00373 0.00025 0.00020 0.00008 0.00000 0.00131 0.00117 0.00120 0.00099 0.00111 0.00108 0.00053 O6 0.71231 0.57056 0.23281 1.00000 0.02554 0.02731 0.01665 -0.00572 -0.00073 0.00105 0.02317 0.00312 0.00020 0.00017 0.00007 0.00000 0.00100 0.00102 0.00088 0.00081 0.00078 0.00087 0.00043 O7 0.51346 0.55618 0.18488 1.00000 0.03862 0.07960 0.03110 -0.02023 -0.01440 0.01249 0.04977 0.00416 0.00026 0.00027 0.00009 0.00000 0.00134 0.00193 0.00124 0.00133 0.00109 0.00142 0.00071 O8 0.75881 0.80299 0.27956 1.00000 0.02754 0.02716 0.02365 -0.00192 -0.00178 0.00052 0.02612 0.00335 0.00021 0.00018 0.00007 0.00000 0.00104 0.00106 0.00102 0.00088 0.00088 0.00092 0.00045 O9 0.99561 0.76433 0.28413 1.00000 0.02837 0.05863 0.04120 0.01498 0.00050 0.00094 0.04273 0.00432 0.00024 0.00024 0.00009 0.00000 0.00113 0.00158 0.00132 0.00126 0.00107 0.00124 0.00060 O10 0.74756 0.79170 0.38757 1.00000 0.02463 0.04550 0.02088 -0.01403 -0.00210 0.00052 0.03034 0.00329 0.00021 0.00020 0.00007 0.00000 0.00100 0.00127 0.00098 0.00096 0.00086 0.00097 0.00049 O11 0.84632 1.02749 0.40824 1.00000 0.02701 0.04443 0.02589 0.00856 -0.00132 -0.00513 0.03244 0.00360 0.00021 0.00020 0.00008 0.00000 0.00105 0.00130 0.00104 0.00099 0.00089 0.00103 0.00051 O12 0.49057 1.04471 0.46333 1.00000 0.02695 0.03265 0.02791 -0.00224 -0.00242 0.00254 0.02917 0.00349 0.00022 0.00019 0.00008 0.00000 0.00102 0.00115 0.00105 0.00094 0.00089 0.00097 0.00047 O13 0.49013 1.15617 0.53487 1.00000 0.04971 0.14339 0.05883 -0.06498 -0.00093 -0.00891 0.08398 0.00491 0.00032 0.00036 0.00011 0.00000 0.00163 0.00330 0.00180 0.00213 0.00147 0.00205 0.00121 O14 0.67704 0.86348 0.52019 1.00000 0.03079 0.03387 0.01627 0.00173 0.00046 0.00097 0.02697 0.00337 0.00022 0.00018 0.00007 0.00000 0.00104 0.00112 0.00090 0.00085 0.00086 0.00097 0.00045 O15 0.80739 0.74502 0.57225 1.00000 0.04526 0.04282 0.02941 0.01259 -0.00198 0.00533 0.03916 0.00421 0.00027 0.00021 0.00008 0.00000 0.00136 0.00135 0.00113 0.00104 0.00107 0.00121 0.00056 Final Structure Factor Calculation for 2009src0685a in P2(1)2(1)2(1) Total number of l.s. parameters = 358 Maximum vector length = 511 Memory required = 4080 / 24024 wR2 = 0.0897 before cycle 11 for 3484 data and 2 / 358 parameters GooF = S = 1.152; Restrained GooF = 1.152 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0108 * P )^2 + 1.73 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0467 for 3005 Fo > 4sig(Fo) and 0.0588 for all 3484 data wR2 = 0.0897, GooF = S = 1.152, Restrained GooF = 1.152 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 39.00 for non-hydrogen and 32.00 for hydrogen atoms Principal mean square atomic displacements U 0.0361 0.0234 0.0194 C1 0.0337 0.0239 0.0179 C2 0.0327 0.0227 0.0144 C3 0.0294 0.0220 0.0166 C4 0.0365 0.0259 0.0160 C5 0.0416 0.0322 0.0219 C6 0.0566 0.0319 0.0244 C7 0.0636 0.0320 0.0297 C8 0.0428 0.0294 0.0175 C9 0.0613 0.0363 0.0258 C10 0.0430 0.0352 0.0163 C11 0.0541 0.0432 0.0207 C12 0.0409 0.0351 0.0164 C13 0.0609 0.0506 0.0335 C14 0.0349 0.0240 0.0145 C15 0.0382 0.0279 0.0163 C16 0.0475 0.0239 0.0212 C17 0.0402 0.0214 0.0180 C18 0.0312 0.0269 0.0157 C19 0.0316 0.0299 0.0261 C20 0.0693 0.0361 0.0216 C21 0.0647 0.0374 0.0338 C22 0.0459 0.0212 0.0189 C23 0.0504 0.0301 0.0208 C24 0.0382 0.0301 0.0168 O1 0.0396 0.0302 0.0254 O2 0.1044 0.0507 0.0314 O3 0.0315 0.0259 0.0216 O4 0.0515 0.0350 0.0220 O5 0.0301 0.0252 0.0142 O6 0.0922 0.0387 0.0184 O7 0.0291 0.0268 0.0224 O8 0.0673 0.0326 0.0283 O9 0.0519 0.0248 0.0142 O10 0.0490 0.0259 0.0224 O11 0.0349 0.0277 0.0249 O12 0.1791 0.0502 0.0226 O13 0.0343 0.0305 0.0161 O14 0.0523 0.0441 0.0210 O15 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.017 0.027 0.036 0.045 0.056 0.070 0.086 0.114 0.165 1.000 Number in group 361. 355. 342. 339. 344. 369. 335. 342. 349. 348. GooF 1.273 1.175 1.211 1.178 1.188 1.143 1.110 1.054 0.961 1.192 K 1.962 1.114 1.060 1.019 1.009 1.011 0.988 0.995 1.002 0.999 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.98 1.06 1.17 1.34 1.72 inf Number in group 365. 344. 341. 345. 360. 336. 351. 345. 347. 350. GooF 1.338 1.288 1.097 1.189 1.152 1.101 0.983 0.922 1.045 1.313 K 1.108 1.053 1.047 1.033 1.006 0.988 0.982 0.997 1.016 0.996 R1 0.211 0.166 0.120 0.103 0.076 0.054 0.037 0.030 0.029 0.021 Recommended weighting scheme: WGHT 0.0101 1.9838 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)/su Fc/Fc(max) Resolution(A) 3 6 12 35.51 1.06 5.18 0.006 1.28 0 2 0 6.14 43.06 4.17 0.036 5.55 0 7 28 249.92 121.87 3.88 0.060 0.80 1 4 31 -14.82 80.64 3.80 0.049 0.80 9 8 1 99.98 44.24 3.58 0.036 0.83 7 11 7 150.59 80.35 3.56 0.049 0.79 10 1 16 69.36 13.49 3.49 0.020 0.81 1 14 1 140.90 60.45 3.44 0.043 0.79 4 3 31 55.14 131.75 3.31 0.063 0.77 6 3 27 44.49 0.61 3.29 0.004 0.80 3 3 8 5176.11 4724.19 3.27 0.376 1.92 3 10 14 38.02 7.80 3.23 0.015 0.91 4 10 10 149.66 227.69 3.20 0.083 0.94 1 7 23 44.49 8.74 3.08 0.016 0.91 3 7 15 98.91 157.74 3.05 0.069 1.09 0 11 15 37.64 0.01 3.04 0.000 0.87 7 5 13 29.98 71.02 3.04 0.046 0.99 7 2 18 53.81 101.40 3.03 0.055 0.96 2 0 5 63.66 107.15 3.03 0.057 3.47 8 0 24 145.72 16.87 3.02 0.022 0.79 3 2 25 35.50 79.56 2.95 0.049 0.97 11 2 8 31.72 73.50 2.94 0.047 0.81 0 2 2 1471.06 1662.58 2.90 0.223 5.10 6 7 1 309.20 395.48 2.89 0.109 1.11 5 0 26 69.71 23.12 2.88 0.026 0.88 2 2 10 10065.04 9378.52 2.86 0.530 2.10 5 7 19 76.55 38.34 2.85 0.034 0.91 1 7 6 77.77 45.81 2.76 0.037 1.47 1 2 1 9892.57 10504.26 2.71 0.561 4.69 1 1 1 6548.43 6991.97 2.69 0.458 6.90 2 5 31 77.01 27.59 2.67 0.029 0.77 9 6 5 259.27 193.23 2.66 0.076 0.89 2 3 30 36.63 83.71 2.66 0.050 0.83 2 10 20 202.65 135.82 2.65 0.064 0.83 0 4 13 268.93 197.91 2.65 0.077 1.62 0 4 32 -12.69 62.71 2.63 0.043 0.78 6 2 0 391.99 316.51 2.62 0.097 1.50 5 4 23 131.42 206.62 2.62 0.079 0.91 1 1 2 14540.16 15381.62 2.60 0.679 6.26 8 9 7 245.01 162.07 2.59 0.070 0.83 0 9 23 -12.72 16.57 2.58 0.022 0.83 0 10 18 60.95 104.75 2.57 0.056 0.88 5 2 6 21.38 7.21 2.57 0.015 1.64 9 3 15 67.39 34.16 2.55 0.032 0.87 3 10 18 31.66 6.56 2.55 0.014 0.85 9 7 5 23.93 1.35 2.53 0.006 0.86 10 0 3 13.55 37.49 2.52 0.034 0.93 3 10 3 161.59 221.01 2.52 0.081 1.04 0 9 18 136.71 195.34 2.52 0.076 0.94 0 9 9 16.14 0.32 2.51 0.003 1.13 Bond lengths and angles C1 - Distance Angles O1 1.4284 (0.0034) C6 1.5093 (0.0041) 105.35 (0.22) C2 1.5260 (0.0037) 109.89 (0.23) 113.25 (0.25) H1 1.0000 109.42 109.42 109.42 C1 - O1 C6 C2 C2 - Distance Angles O4 1.4447 (0.0033) C1 1.5260 (0.0037) 106.78 (0.22) C3 1.5277 (0.0040) 110.54 (0.22) 109.93 (0.24) H2 1.0000 109.85 109.85 109.85 C2 - O4 C1 C3 C3 - Distance Angles O6 1.4491 (0.0031) C4 1.5128 (0.0038) 106.82 (0.22) C2 1.5277 (0.0040) 110.36 (0.23) 111.96 (0.22) H3 1.0000 109.22 109.22 109.22 C3 - O6 C4 C2 C4 - Distance Angles O8 1.4404 (0.0033) C3 1.5128 (0.0038) 108.53 (0.21) C5 1.5248 (0.0037) 106.99 (0.22) 109.77 (0.23) H4 1.0000 110.49 110.49 110.49 C4 - O8 C3 C5 C5 - Distance Angles O10 1.3898 (0.0033) O1 1.4213 (0.0035) 107.81 (0.22) C4 1.5248 (0.0037) 107.36 (0.23) 109.66 (0.23) H5 1.0000 110.64 110.64 110.64 C5 - O10 O1 C4 C6 - Distance Angles O2 1.4469 (0.0036) C1 1.5093 (0.0041) 106.53 (0.23) H6A 0.9900 110.42 110.42 H6B 0.9900 110.42 110.42 108.63 C6 - O2 C1 H6A C7 - Distance Angles O3 1.2074 (0.0041) O2 1.3494 (0.0038) 121.79 (0.35) C8 1.4887 (0.0049) 126.83 (0.33) 111.36 (0.29) C7 - O3 O2 C8 - Distance Angles C7 1.4887 (0.0049) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - C7 H8A H8B C9 - Distance Angles O5 1.2030 (0.0037) O4 1.3567 (0.0035) 123.38 (0.29) C10 1.4864 (0.0045) 125.72 (0.30) 110.90 (0.27) C9 - O5 O4 C10 - Distance Angles C9 1.4864 (0.0045) H10A 0.9800 109.47 H10B 0.9800 109.47 109.47 H10C 0.9800 109.47 109.47 109.47 C10 - C9 H10A H10B C11 - Distance Angles O7 1.1937 (0.0038) O6 1.3602 (0.0033) 122.76 (0.28) C12 1.4847 (0.0042) 125.52 (0.29) 111.71 (0.26) C11 - O7 O6 C12 - Distance Angles C11 1.4847 (0.0042) H12A 0.9800 109.47 H12B 0.9800 109.47 109.47 H12C 0.9800 109.47 109.47 109.47 C12 - C11 H12A H12B C13 - Distance Angles O9 1.2010 (0.0039) O8 1.3576 (0.0037) 123.99 (0.30) C14 1.4951 (0.0047) 125.50 (0.32) 110.51 (0.29) C13 - O9 O8 C14 - Distance Angles C13 1.4951 (0.0047) H14A 0.9800 109.47 H14B 0.9800 109.47 109.47 H14C 0.9800 109.47 109.47 109.47 C14 - C13 H14A H14B C15 - Distance Angles O10 1.4426 (0.0031) C16 1.5190 (0.0042) 108.17 (0.23) C19 1.5249 (0.0038) 105.45 (0.22) 112.17 (0.24) H15 1.0000 110.31 110.31 110.31 C15 - O10 C16 C19 C16 - Distance Angles O11 1.4433 (0.0034) C20 1.5133 (0.0040) 106.56 (0.24) C15 1.5190 (0.0042) 111.01 (0.24) 115.29 (0.24) H16 1.0000 107.91 107.91 107.91 C16 - O11 C20 C15 C17 - Distance Angles C18 1.3312 (0.0043) O11 1.3591 (0.0035) 126.55 (0.28) H17 0.9500 116.73 116.73 C17 - C18 O11 C18 - Distance Angles C17 1.3312 (0.0043) C19 1.4870 (0.0041) 121.38 (0.27) H18 0.9500 119.31 119.31 C18 - C17 C19 C19 - Distance Angles O14 1.4695 (0.0032) C18 1.4870 (0.0041) 113.02 (0.22) C15 1.5249 (0.0038) 104.96 (0.22) 110.47 (0.24) H19 1.0000 109.43 109.43 109.43 C19 - O14 C18 C15 C20 - Distance Angles O12 1.4410 (0.0035) C16 1.5133 (0.0040) 107.50 (0.24) H20A 0.9900 110.21 110.21 H20B 0.9900 110.21 110.21 108.50 C20 - O12 C16 H20A C21 - Distance Angles O13 1.1894 (0.0043) O12 1.3467 (0.0037) 122.99 (0.34) C22 1.4985 (0.0050) 125.23 (0.34) 111.78 (0.31) C21 - O13 O12 C22 - Distance Angles C21 1.4985 (0.0050) H22A 0.9800 109.47 H22B 0.9800 109.47 109.47 H22C 0.9800 109.47 109.47 109.47 C22 - C21 H22A H22B C23 - Distance Angles O15 1.2053 (0.0038) O14 1.3489 (0.0033) 122.92 (0.28) C24 1.4893 (0.0042) 126.41 (0.27) 110.68 (0.27) C23 - O15 O14 C24 - Distance Angles C23 1.4893 (0.0042) H24A 0.9800 109.47 H24B 0.9800 109.47 109.47 H24C 0.9800 109.47 109.47 109.47 C24 - C23 H24A H24B O1 - Distance Angles C5 1.4213 (0.0036) C1 1.4284 (0.0034) 111.31 (0.20) O1 - C5 O2 - Distance Angles C7 1.3494 (0.0038) C6 1.4469 (0.0036) 116.12 (0.25) O2 - C7 O3 - Distance Angles C7 1.2074 (0.0041) O3 - O4 - Distance Angles C9 1.3567 (0.0035) C2 1.4447 (0.0033) 117.20 (0.23) O4 - C9 O5 - Distance Angles C9 1.2030 (0.0037) O5 - O6 - Distance Angles C11 1.3602 (0.0033) C3 1.4491 (0.0031) 115.51 (0.21) O6 - C11 O7 - Distance Angles C11 1.1937 (0.0038) O7 - O8 - Distance Angles C13 1.3576 (0.0037) C4 1.4404 (0.0033) 117.40 (0.23) O8 - C13 O9 - Distance Angles C13 1.2010 (0.0039) O9 - O10 - Distance Angles C5 1.3898 (0.0033) C15 1.4426 (0.0031) 114.03 (0.22) O10 - C5 O11 - Distance Angles C17 1.3591 (0.0035) C16 1.4433 (0.0034) 115.09 (0.22) O11 - C17 O12 - Distance Angles C21 1.3467 (0.0037) C20 1.4410 (0.0035) 115.96 (0.25) O12 - C21 O13 - Distance Angles C21 1.1894 (0.0043) O13 - O14 - Distance Angles C23 1.3489 (0.0033) C19 1.4695 (0.0032) 115.98 (0.23) O14 - C23 O15 - Distance Angles C23 1.2053 (0.0038) O15 - FMAP and GRID set by program FMAP 2 3 30 GRID -0.926 -2 -2 0.926 2 2 R1 = 0.0588 for 3484 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.25 at 0.3120 0.2164 0.1694 [ 0.74 A from C4 ] Deepest hole -0.22 at 0.8800 0.7022 0.0642 [ 1.37 A from H8C ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 3815 / 25260 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.6880 0.7164 0.3306 1.00000 0.05 0.25 0.74 C4 0.79 C5 1.45 H4 1.46 H5 Q2 1 0.9976 0.9003 0.1876 1.00000 0.05 0.22 1.42 H14C 1.51 H8B 1.96 C14 2.01 H14B Q3 1 0.7144 0.9373 0.6138 1.00000 0.05 0.21 1.29 H24B 1.49 C24 1.58 H24C 1.88 C23 Q4 1 0.6013 0.5677 0.2875 1.00000 0.05 0.20 0.69 C3 0.84 C2 1.43 H3 1.51 H2 Q5 1 0.8164 0.4327 0.1656 1.00000 0.05 0.20 0.82 H12B 1.00 C12 1.01 H12A 1.82 H12C Q6 1 0.4362 0.4980 0.2507 1.00000 0.05 0.19 1.02 H2 1.84 C2 1.96 O7 2.20 H3 Q7 1 0.3039 0.4167 0.3258 1.00000 0.05 0.19 1.08 O2 2.03 H14B 2.04 C7 2.10 H2 Q8 1 0.5949 1.1552 0.4388 1.00000 0.05 0.18 0.42 H20B 0.99 C20 1.69 O12 1.75 H20A Q9 1 0.9748 1.0325 0.1780 1.00000 0.05 0.18 1.69 H14C 1.96 H14B 2.05 H24B 2.11 H24C Q10 1 0.9823 0.8267 0.4784 1.00000 0.05 0.18 0.77 H18 1.00 C18 1.98 C17 1.99 C19 Q11 1 0.1046 0.3803 0.3132 1.00000 0.05 0.18 1.32 H8B 1.59 H14B 1.69 H8A 1.79 C8 Q12 1 0.5052 0.3604 0.3978 1.00000 0.05 0.17 0.51 H6A 1.33 C6 1.90 H6B 2.02 O2 Q13 1 0.7074 0.5020 0.1746 1.00000 0.05 0.17 0.69 C12 0.86 C11 1.24 H12B 1.35 H12A Q14 1 0.6511 0.6530 0.4615 1.00000 0.05 0.17 1.65 H19 1.88 H18 2.08 O1 2.19 H22B Q15 1 0.4664 0.3926 0.4624 1.00000 0.05 0.17 1.61 H6B 1.79 H6A 2.03 C6 2.14 O3 Q16 1 0.5127 0.8680 0.6240 1.00000 0.05 0.17 0.97 C24 0.97 H24A 1.10 H24B 1.31 H24C Q17 1 0.4071 0.1258 0.4072 1.00000 0.05 0.17 1.84 O3 1.85 H12C 1.88 O12 2.37 H20B Q18 1 1.0518 1.0758 0.2693 1.00000 0.05 0.17 1.52 H14A 1.59 H14C 1.89 C14 2.21 O6 Q19 1 0.3636 0.2465 0.3899 1.00000 0.05 0.17 1.05 O3 1.18 C7 2.00 O2 2.28 H6A Q20 1 0.8153 0.0498 0.3319 1.00000 0.05 0.17 1.53 H10A 1.63 H14A 2.02 O11 2.07 H16 Shortest distances between peaks (including symmetry equivalents) 2 11 0.98 5 13 1.30 17 19 1.47 2 9 1.50 12 15 1.75 9 16 1.79 12 19 1.84 9 11 1.86 7 11 1.94 8 17 1.97 4 6 1.97 3 16 2.05 1 4 2.15 10 14 2.23 3 7 2.40 3 9 2.45 6 7 2.48 9 18 2.52 7 19 2.58 5 18 2.63 8 12 2.65 15 19 2.66 8 19 2.71 7 12 2.72 13 17 2.75 18 20 2.76 12 17 2.77 13 18 2.81 2 7 2.85 7 9 2.91 2 18 2.92 3 11 2.96 8 15 2.96 Time profile in seconds ----------------------- 0.06: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 1.16: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 3.00: Structure factors and derivatives 4.77: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.70: Solve l.s. equations 0.00: Generate HTAB table 0.06: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.03: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0685a finished at 15:24:28 Total CPU time: 9.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++