+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 10:20:55 on 31-Jul-2002 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in C2 CELL 0.71073 19.4025 8.9915 17.8551 90.000 93.313 90.000 ZERR 4.00 0.0021 0.0011 0.0024 0.000 0.004 0.000 LATT -7 SYMM - X, Y, - Z SFAC C H N O UNIT 128 160 8 32 V = 3109.75 F(000) = 1240.0 Mu = 0.09 mm-1 Cell Wt = 2322.64 Rho = 1.240 MERG 2 OMIT 2 -6 0 OMIT 3 -3 1 OMIT 9 7 1 OMIT 9 -3 0 OMIT 8 -4 1 OMIT 1 -3 0 OMIT -9 -7 2 OMIT 15 -3 0 OMIT 3 -5 3 EXTI ACTA SHEL 7 0.84 FMAP 2 PLAN 10 SIZE 0.12 0.16 0.28 BOND $H WGHT 0.15420 L.S. 10 TEMP -153.00 FVAR 0.13980 O8 4 0.440105 0.872383 0.199092 11.00000 0.01859 0.04508 = 0.07601 0.00044 0.00624 0.00139 O6 4 0.612483 1.090380 0.094448 11.00000 0.04627 0.08121 = 0.04740 0.00552 0.00567 -0.00621 O7 4 0.491626 1.096854 0.192214 11.00000 0.02573 0.03563 = 0.09447 0.00438 0.00497 -0.00218 O1 4 0.810886 0.740405 0.268951 11.00000 0.03068 0.03998 = 0.11637 0.00057 0.01300 0.00176 O5 4 0.640524 1.230128 0.194178 11.00000 0.02338 0.04681 = 0.06901 0.00874 0.00161 -0.00306 N1 3 0.732770 0.970935 0.377154 11.00000 0.02149 0.03692 = 0.06075 0.00375 0.00076 -0.00677 N2 3 0.637109 0.997004 0.291154 11.00000 0.02312 0.03955 = 0.05013 0.00369 0.00252 -0.00087 O2 4 0.866240 0.961620 0.270689 11.00000 0.02277 0.04448 = 0.10152 0.00540 0.00834 0.00858 C30 1 0.495183 0.964921 0.195165 11.00000 0.02702 0.04837 = 0.05288 -0.00043 0.00136 -0.00164 O4 4 0.664337 0.750128 0.079677 11.00000 0.03319 0.06754 = 0.06823 -0.01952 0.01321 -0.01242 C20 1 0.811142 0.874305 0.260746 11.00000 0.01763 0.04221 = 0.08211 -0.00257 0.01508 -0.01744 O3 4 0.752046 0.916938 0.080013 11.00000 0.03919 0.07846 = 0.08320 -0.00448 0.02071 -0.01676 C17 1 0.412910 0.864640 0.412382 11.00000 0.02527 0.06465 = 0.06490 -0.00517 0.00778 -0.02147 AFIX 43 H17 2 0.366838 0.860431 0.427606 11.00000 -1.20000 AFIX 0 C8 1 0.804618 1.002648 0.494634 11.00000 0.02574 0.02160 = 0.06225 0.00312 0.00288 -0.01748 C15 1 0.508238 1.004646 0.368309 11.00000 0.02548 0.06664 = 0.05618 -0.00743 0.00897 -0.01073 AFIX 43 H15 2 0.527681 1.097181 0.354884 11.00000 -1.20000 AFIX 0 C3 1 0.711671 1.031724 0.304657 11.00000 0.01348 0.04988 = 0.06279 -0.00197 0.00773 -0.01249 AFIX 13 H3 2 0.718320 1.142012 0.305402 11.00000 -1.20000 AFIX 0 C14 1 0.546568 0.875326 0.365630 11.00000 0.02448 0.05008 = 0.06225 -0.00070 -0.00240 -0.00396 C7 1 0.775325 1.073449 0.423649 11.00000 0.02478 0.03812 = 0.07623 0.00291 0.00217 -0.00760 AFIX 23 H7A 2 0.746998 1.160332 0.436555 11.00000 -1.20000 H7B 2 0.813710 1.109939 0.394397 11.00000 -1.20000 AFIX 0 C6 1 0.626085 0.963803 0.211194 11.00000 0.01291 0.04429 = 0.06281 0.00696 0.00974 0.00084 C26 1 0.625748 1.110655 0.167107 11.00000 0.01201 0.04059 = 0.06748 -0.00342 0.00904 -0.00655 C2 1 0.621547 0.881713 0.345422 11.00000 0.02588 0.04863 = 0.04498 0.00628 0.00739 0.00656 AFIX 13 H2 2 0.635576 0.782543 0.326029 11.00000 -1.20000 AFIX 0 C29 1 0.559943 0.872984 0.191166 11.00000 0.01972 0.04286 = 0.06649 -0.00851 0.00567 -0.00679 AFIX 23 H29A 2 0.562240 0.832514 0.139806 11.00000 -1.20000 H29B 2 0.557767 0.787923 0.226156 11.00000 -1.20000 AFIX 0 C13 1 0.858013 0.894256 0.490042 11.00000 0.03742 0.04921 = 0.05963 0.00448 -0.00005 -0.01321 AFIX 43 H13 2 0.872842 0.865439 0.442378 11.00000 -1.20000 AFIX 0 C4 1 0.749195 0.963395 0.237435 11.00000 0.02294 0.03657 = 0.07003 0.01089 0.00448 -0.00007 AFIX 13 H4 2 0.763654 1.046321 0.204479 11.00000 -1.20000 AFIX 0 C1 1 0.668090 0.922902 0.412148 11.00000 0.02222 0.04291 = 0.06189 0.00168 0.01078 -0.00535 AFIX 23 H1A 2 0.648238 1.005015 0.440911 11.00000 -1.20000 H1B 2 0.676775 0.836557 0.445782 11.00000 -1.20000 AFIX 0 C23 1 0.707690 0.854080 0.111560 11.00000 0.03682 0.04741 = 0.07786 -0.00740 0.01089 0.00966 C32 1 0.321321 0.832469 0.213355 11.00000 0.02154 0.06285 = 0.08379 -0.00021 0.00337 -0.01105 AFIX 137 H32A 2 0.320154 0.765066 0.170168 11.00000 -1.50000 H32B 2 0.276031 0.879527 0.216588 11.00000 -1.50000 H32C 2 0.332690 0.776030 0.259375 11.00000 -1.50000 AFIX 0 C19 1 0.519097 0.741128 0.388946 11.00000 0.02677 0.05315 = 0.06737 0.00736 0.00189 -0.00179 AFIX 43 H19 2 0.546439 0.653473 0.389075 11.00000 -1.20000 AFIX 0 C11 1 0.867271 0.862058 0.621920 11.00000 0.03996 0.03507 = 0.07501 0.01198 -0.01479 -0.01961 AFIX 43 H11 2 0.887940 0.813579 0.664837 11.00000 -1.20000 AFIX 0 C10 1 0.812571 0.970992 0.628339 11.00000 0.05757 0.07349 = 0.06251 -0.01059 0.00249 -0.05269 AFIX 43 H10 2 0.796397 0.997836 0.675699 11.00000 -1.20000 AFIX 0 C5 1 0.693331 0.872217 0.194246 11.00000 0.02492 0.05201 = 0.05601 -0.00280 0.00127 0.00410 AFIX 13 H5 2 0.690627 0.771586 0.217742 11.00000 -1.20000 AFIX 0 C22 1 0.980658 0.956492 0.226558 11.00000 0.03212 0.05986 = 0.09150 0.01037 0.01101 0.01594 AFIX 137 H22A 2 0.961450 0.934050 0.175848 11.00000 -1.50000 H22B 2 1.026898 0.913040 0.233627 11.00000 -1.50000 H22C 2 0.983582 1.064527 0.233271 11.00000 -1.50000 AFIX 0 C31 1 0.373676 0.947039 0.204305 11.00000 0.02677 0.04864 = 0.07744 -0.00093 0.00513 -0.01348 AFIX 23 H31A 2 0.362402 1.005562 0.158252 11.00000 -1.20000 H31B 2 0.375465 1.015532 0.247786 11.00000 -1.20000 AFIX 0 C16 1 0.439744 0.997628 0.391266 11.00000 0.02115 0.04922 = 0.08393 -0.01237 0.00474 -0.00098 AFIX 43 H16 2 0.412450 1.085276 0.391996 11.00000 -1.20000 AFIX 0 C24 1 0.670053 0.725872 0.000842 11.00000 0.04530 0.09241 = 0.06647 -0.02485 0.01309 -0.00926 AFIX 23 H24A 2 0.711507 0.665490 -0.007839 11.00000 -1.20000 H24B 2 0.674056 0.822063 -0.025534 11.00000 -1.20000 AFIX 0 C21 1 0.935005 0.892270 0.282837 11.00000 0.02448 0.05755 = 0.09042 -0.00467 0.00844 0.01293 AFIX 23 H21A 2 0.931441 0.783137 0.276366 11.00000 -1.20000 H21B 2 0.954238 0.913204 0.334322 11.00000 -1.20000 AFIX 0 C9 1 0.785582 1.032747 0.563685 11.00000 0.03487 0.02339 = 0.06215 0.00147 0.00322 -0.01985 AFIX 43 H9 2 0.749854 1.103945 0.568005 11.00000 -1.20000 AFIX 0 C18 1 0.452448 0.734516 0.411868 11.00000 0.02932 0.07179 = 0.07088 0.01344 -0.00105 -0.01185 AFIX 43 H18 2 0.433607 0.642601 0.427137 11.00000 -1.20000 AFIX 0 C27 1 0.612757 1.217923 0.047946 11.00000 0.06012 0.10249 = 0.04771 0.01799 0.00043 -0.01406 AFIX 23 H27A 2 0.656630 1.272777 0.057480 11.00000 -1.20000 H27B 2 0.574363 1.284671 0.060012 11.00000 -1.20000 AFIX 0 C12 1 0.887392 0.832818 0.552447 11.00000 0.04950 0.03720 = 0.07196 0.01018 -0.00711 -0.02558 AFIX 43 H12 2 0.924390 0.765015 0.547412 11.00000 -1.20000 AFIX 0 C28 1 0.605233 1.175343 -0.030472 11.00000 0.11615 0.08164 = 0.07866 0.00527 0.00043 -0.00060 AFIX 137 H28A 2 0.642628 1.107315 -0.042020 11.00000 -1.50000 H28B 2 0.607301 1.264305 -0.061973 11.00000 -1.50000 H28C 2 0.560686 1.125648 -0.040396 11.00000 -1.50000 AFIX 0 C25 1 0.608092 0.647950 -0.026705 11.00000 0.05992 0.08941 = 0.08869 -0.01000 0.00000 -0.03721 AFIX 137 H25A 2 0.604835 0.552840 -0.000339 11.00000 -1.50000 H25B 2 0.610168 0.629694 -0.080639 11.00000 -1.50000 H25C 2 0.567467 0.708743 -0.017725 11.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for s92 in C2 C 0.770 H 0.320 N 0.700 O 0.660 O8 - C30 C31 O6 - C26 C27 O7 - C30 O1 - C20 O5 - C26 N1 - C3 C7 C1 N2 - C6 C2 C3 O2 - C20 C21 C30 - O7 O8 C29 O4 - C23 C24 C20 - O1 O2 C4 O3 - C23 C17 - C16 C18 C8 - C9 C13 C7 C15 - C14 C16 C3 - N1 N2 C4 C14 - C15 C19 C2 C7 - N1 C8 C6 - N2 C26 C29 C5 C26 - O5 O6 C6 C2 - N2 C1 C14 C29 - C30 C6 C13 - C12 C8 C4 - C20 C5 C3 C1 - N1 C2 C23 - O3 O4 C5 C32 - C31 C19 - C18 C14 C11 - C12 C10 C10 - C9 C11 C5 - C23 C4 C6 C22 - C21 C31 - O8 C32 C16 - C17 C15 C24 - O4 C25 C21 - O2 C22 C9 - C8 C10 C18 - C19 C17 C27 - O6 C28 C12 - C13 C11 C28 - C27 C25 - C24 Floating origin restraints generated 10383 Reflections read, of which 872 rejected -22 =< h =< 21, -10 =< k =< 10, -21 =< l =< 21, Max. 2-theta = 50.04 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 10 -6 0 12.68 0.93 2 9.76 9 -5 0 22.60 0.86 3 12.22 11 -5 0 14.25 0.89 2 6.96 12 -4 0 10.49 0.89 2 5.97 2 -2 0 34.10 2.04 2 37.79 2 2 0 35.93 1.18 4 9.77 -8 -6 1 15.53 0.94 3 12.39 -10 -4 1 31.62 1.79 2 13.94 7 -3 1 29.25 2.91 3 17.79 -8 -2 1 44.02 1.69 3 11.25 -2 -2 1 136.26 0.97 4 92.36 7 3 1 46.44 1.95 4 17.41 -6 4 1 21.95 0.90 4 14.33 2 4 1 10.31 0.68 3 5.80 6 4 1 73.96 1.87 5 15.19 8 4 1 21.04 1.68 4 25.66 10 4 1 35.84 1.76 3 8.87 0 8 1 26.45 2.80 2 25.22 -14 -4 2 38.23 2.85 2 16.05 5 -3 2 24.33 1.99 3 15.01 -9 -1 2 184.32 6.29 2 48.44 -1 -1 2 29.75 1.88 2 20.30 1 -1 2 99.69 5.63 3 35.17 4 2 2 31.45 1.40 3 26.20 6 2 2 23.19 1.38 3 8.58 -3 3 2 22.14 0.69 3 5.72 -1 3 2 14.21 0.67 3 3.51 -10 4 2 8.86 0.92 2 5.03 0 4 2 26.66 1.36 3 8.10 6 4 2 14.76 0.69 5 5.70 0 6 2 24.67 1.44 2 12.98 0 8 2 25.74 3.11 2 32.32 6 2 3 10.40 0.69 2 3.88 -9 3 3 31.77 1.96 2 21.10 -4 4 3 7.90 0.91 3 6.52 -2 4 3 10.78 0.97 2 11.40 8 4 3 10.88 0.90 4 26.81 -3 5 3 9.86 0.96 3 7.08 1 -1 4 624.13 26.78 3 180.83 2 6 4 17.34 1.04 2 7.04 6 0 16 -0.16 1.00 2 6.38 41 Inconsistent equivalents 4596 Unique reflections, of which 0 suppressed R(int) = 0.1615 R(sigma) = 0.1887 Friedel opposites not merged Maximum memory for data reduction = 3924 / 57132 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 = 5025 / 490131 wR2 = 0.2805 before cycle 1 for 4596 data and 384 / 384 parameters GooF = S = 0.992; Restrained GooF = 0.992 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1542 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.13935 0.00078 -0.580 OSF 2 0.00335 0.00109 3.083 EXTI Mean shift/esd = 0.178 Maximum = 3.083 for EXTI Max. shift = 0.045 A for H28C Max. dU =-0.001 for C16 Least-squares cycle 2 Maximum vector length = 511 Memory required = 5025 / 490131 wR2 = 0.2785 before cycle 2 for 4596 data and 384 / 384 parameters GooF = S = 0.981; Restrained GooF = 0.981 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1542 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.13943 0.00080 0.108 OSF 2 0.00543 0.00140 1.482 EXTI Mean shift/esd = 0.076 Maximum = 1.482 for EXTI Max. shift = 0.012 A for H28C Max. dU = 0.000 for O8 Least-squares cycle 3 Maximum vector length = 511 Memory required = 5025 / 490131 wR2 = 0.2782 before cycle 3 for 4596 data and 384 / 384 parameters GooF = S = 0.980; Restrained GooF = 0.980 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1542 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.13942 0.00081 -0.018 OSF 2 0.00547 0.00160 0.026 EXTI Mean shift/esd = 0.025 Maximum = -0.153 for U22 O4 Max. shift = 0.004 A for H32A Max. dU = 0.000 for C27 Least-squares cycle 4 Maximum vector length = 511 Memory required = 5025 / 490131 wR2 = 0.2782 before cycle 4 for 4596 data and 384 / 384 parameters GooF = S = 0.980; Restrained GooF = 0.980 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1542 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.13939 0.00081 -0.033 OSF 2 0.00547 0.00160 -0.004 EXTI Mean shift/esd = 0.012 Maximum = -0.060 for U22 C19 Max. shift = 0.001 A for H28A Max. dU = 0.000 for C27 Least-squares cycle 5 Maximum vector length = 511 Memory required = 5025 / 490131 wR2 = 0.2782 before cycle 5 for 4596 data and 384 / 384 parameters GooF = S = 0.980; Restrained GooF = 0.980 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1542 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.13939 0.00081 -0.007 OSF 2 0.00546 0.00160 -0.006 EXTI Mean shift/esd = 0.006 Maximum = -0.027 for y C23 Max. shift = 0.000 A for H25B Max. dU = 0.000 for C27 Least-squares cycle 6 Maximum vector length = 511 Memory required = 5025 / 490131 wR2 = 0.2782 before cycle 6 for 4596 data and 384 / 384 parameters GooF = S = 0.980; Restrained GooF = 0.980 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1542 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.13938 0.00081 -0.004 OSF 2 0.00545 0.00160 -0.002 EXTI Mean shift/esd = 0.003 Maximum = -0.015 for y C23 Max. shift = 0.000 A for H28C Max. dU = 0.000 for C27 Least-squares cycle 7 Maximum vector length = 511 Memory required = 5025 / 490131 wR2 = 0.2782 before cycle 7 for 4596 data and 384 / 384 parameters GooF = S = 0.980; Restrained GooF = 0.980 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1542 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.13938 0.00081 -0.002 OSF 2 0.00545 0.00160 -0.001 EXTI Mean shift/esd = 0.002 Maximum = -0.008 for y C23 Max. shift = 0.000 A for H25B Max. dU = 0.000 for C27 Least-squares cycle 8 Maximum vector length = 511 Memory required = 5025 / 490131 wR2 = 0.2782 before cycle 8 for 4596 data and 384 / 384 parameters GooF = S = 0.980; Restrained GooF = 0.980 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1542 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.13938 0.00081 -0.001 OSF 2 0.00545 0.00160 0.000 EXTI Mean shift/esd = 0.001 Maximum = -0.004 for y C23 Max. shift = 0.000 A for H28C Max. dU = 0.000 for C27 Least-squares cycle 9 Maximum vector length = 511 Memory required = 5025 / 490131 wR2 = 0.2782 before cycle 9 for 4596 data and 384 / 384 parameters GooF = S = 0.980; Restrained GooF = 0.980 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1542 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.13938 0.00081 -0.001 OSF 2 0.00545 0.00160 0.000 EXTI Mean shift/esd = 0.001 Maximum = -0.002 for y C23 Max. shift = 0.000 A for H28C Max. dU = 0.000 for C27 Least-squares cycle 10 Maximum vector length = 511 Memory required = 5025 / 490131 wR2 = 0.2782 before cycle 10 for 4596 data and 384 / 384 parameters GooF = S = 0.980; Restrained GooF = 0.980 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1542 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.13938 0.00081 0.000 OSF 2 0.00545 0.00160 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for y C23 Max. shift = 0.000 A for H28C Max. dU = 0.000 for C10 Largest correlation matrix elements 0.537 EXTI / OSF -0.526 U12 C10 / U22 C10 Idealized hydrogen atom generation before cycle 11 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H17 0.3668 0.8605 0.4277 43 0.950 0.000 C17 C16 C18 H15 0.5274 1.0968 0.3546 43 0.950 0.000 C15 C14 C16 H3 0.7182 1.1429 0.3054 13 1.000 0.000 C3 N1 N2 C4 H7A 0.7472 1.1602 0.4366 23 0.990 0.000 C7 N1 C8 H7B 0.8138 1.1092 0.3945 23 0.990 0.000 C7 N1 C8 H2 0.6354 0.7829 0.3261 13 1.000 0.000 C2 N2 C1 C14 H29A 0.5620 0.8332 0.1396 23 0.990 0.000 C29 C30 C6 H29B 0.5577 0.7879 0.2258 23 0.990 0.000 C29 C30 C6 H13 0.8725 0.8641 0.4423 43 0.950 0.000 C13 C12 C8 H4 0.7641 1.0456 0.2044 13 1.000 0.000 C4 C20 C5 C3 H1A 0.6481 1.0048 0.4409 23 0.990 0.000 C1 N1 C2 H1B 0.6765 0.8363 0.4456 23 0.990 0.000 C1 N1 C2 H32A 0.3202 0.7648 0.1703 137 0.980 0.000 C32 C31 H32A H32B 0.2762 0.8792 0.2169 137 0.980 0.000 C32 C31 H32A H32C 0.3331 0.7761 0.2595 137 0.980 0.000 C32 C31 H32A H19 0.5464 0.6541 0.3890 43 0.950 0.000 C19 C18 C14 H11 0.8876 0.8117 0.6646 43 0.950 0.000 C11 C12 C10 H10 0.7964 0.9979 0.6758 43 0.950 0.000 C10 C9 C11 H5 0.6904 0.7724 0.2180 13 1.000 0.000 C5 C23 C4 C6 H22A 0.9609 0.9383 0.1759 137 0.980 0.000 C22 C21 H22A H22B 1.0268 0.9122 0.2325 137 0.980 0.000 C22 C21 H22A H22C 0.9847 1.0651 0.2347 137 0.980 0.000 C22 C21 H22A H31A 0.3623 1.0047 0.1578 23 0.990 0.000 C31 O8 C32 H31B 0.3753 1.0160 0.2473 23 0.990 0.000 C31 O8 C32 H16 0.4125 1.0845 0.3919 43 0.950 0.000 C16 C17 C15 H24A 0.7114 0.6637 -0.0075 23 0.990 0.000 C24 O4 C25 H24B 0.6743 0.8205 -0.0256 23 0.990 0.000 C24 O4 C25 H21A 0.9314 0.7826 0.2760 23 0.990 0.000 C21 O2 C22 H21B 0.9543 0.9116 0.3346 23 0.990 0.000 C21 O2 C22 H9 0.7500 1.1053 0.5681 43 0.950 0.000 C9 C8 C10 H18 0.4337 0.6431 0.4269 43 0.950 0.000 C18 C19 C17 H27A 0.6568 1.2733 0.0575 23 0.990 0.000 C27 O6 C28 H27B 0.5746 1.2860 0.0602 23 0.990 0.000 C27 O6 C28 H12 0.9245 0.7643 0.5473 43 0.950 0.000 C12 C13 C11 H28A 0.6408 1.1035 -0.0416 137 0.980 0.000 C28 C27 H28A H28B 0.6095 1.2639 -0.0624 137 0.980 0.000 C28 C27 H28A H28C 0.5594 1.1310 -0.0410 137 0.980 0.000 C28 C27 H28A H25A 0.6042 0.5531 0.0006 137 0.980 0.000 C25 C24 H25A H25B 0.6107 0.6271 -0.0802 137 0.980 0.000 C25 C24 H25A H25C 0.5677 0.7092 -0.0185 137 0.980 0.000 C25 C24 H25A s92 in C2 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq O8 0.44018 0.87275 0.19914 1.00000 0.01808 0.03936 0.07719 0.00095 0.00620 0.00290 0.04475 0.00938 0.00025 0.00064 0.00028 0.00000 0.00312 0.00347 0.00366 0.00282 0.00237 0.00273 0.00140 O6 0.61234 1.09038 0.09437 1.00000 0.04510 0.07838 0.04822 0.00641 0.00571 -0.00527 0.05712 0.01095 0.00030 0.00077 0.00032 0.00000 0.00408 0.00482 0.00374 0.00328 0.00278 0.00333 0.00173 O7 0.49157 1.09663 0.19214 1.00000 0.02570 0.03232 0.09491 0.00451 0.00456 -0.00165 0.05094 0.01051 0.00028 0.00072 0.00034 0.00000 0.00342 0.00397 0.00439 0.00288 0.00281 0.00273 0.00151 O1 0.81100 0.74039 0.26900 1.00000 0.03021 0.04071 0.11597 0.00165 0.01281 0.00388 0.06197 0.01203 0.00030 0.00075 0.00039 0.00000 0.00349 0.00447 0.00525 0.00341 0.00314 0.00298 0.00179 O5 0.64056 1.22988 0.19421 1.00000 0.02336 0.04556 0.06900 0.00719 0.00141 -0.00302 0.04602 0.01066 0.00026 0.00070 0.00031 0.00000 0.00313 0.00394 0.00364 0.00300 0.00262 0.00285 0.00144 N1 0.73280 0.97099 0.37732 1.00000 0.02313 0.03506 0.06039 0.00356 0.00052 -0.00684 0.03960 0.01104 0.00032 0.00073 0.00035 0.00000 0.00379 0.00426 0.00412 0.00311 0.00303 0.00311 0.00167 N2 0.63718 0.99695 0.29104 1.00000 0.02209 0.04193 0.04971 0.00426 0.00245 -0.00070 0.03789 0.01084 0.00032 0.00070 0.00033 0.00000 0.00363 0.00427 0.00392 0.00295 0.00273 0.00297 0.00164 O2 0.86638 0.96199 0.27076 1.00000 0.02337 0.04380 0.10092 0.00547 0.00781 0.01029 0.05587 0.01071 0.00029 0.00065 0.00034 0.00000 0.00335 0.00386 0.00446 0.00314 0.00292 0.00290 0.00164 C30 0.49522 0.96437 0.19521 1.00000 0.02775 0.05252 0.05100 0.00009 0.00126 0.00043 0.04380 0.01516 0.00042 0.00115 0.00042 0.00000 0.00514 0.00688 0.00482 0.00408 0.00361 0.00469 0.00213 O4 0.66433 0.74960 0.07976 1.00000 0.03262 0.06646 0.06779 -0.01810 0.01244 -0.01101 0.05526 0.01046 0.00030 0.00073 0.00032 0.00000 0.00339 0.00448 0.00391 0.00326 0.00279 0.00325 0.00169 C20 0.81102 0.87371 0.26067 1.00000 0.01699 0.04166 0.08161 -0.00280 0.01439 -0.01755 0.04631 0.01469 0.00038 0.00113 0.00046 0.00000 0.00457 0.00605 0.00588 0.00469 0.00376 0.00433 0.00213 O3 0.75205 0.91749 0.08000 1.00000 0.03884 0.08094 0.08149 -0.00499 0.02009 -0.01544 0.06645 0.01167 0.00034 0.00082 0.00036 0.00000 0.00392 0.00509 0.00412 0.00343 0.00328 0.00350 0.00190 C17 0.41281 0.86468 0.41237 1.00000 0.02345 0.07204 0.06357 -0.00608 0.00853 -0.01978 0.05279 0.01447 0.00043 0.00119 0.00045 0.00000 0.00486 0.00743 0.00532 0.00496 0.00372 0.00532 0.00241 H17 0.36676 0.86046 0.42767 1.00000 0.06335 0.00000 0.00000 C8 0.80456 1.00346 0.49458 1.00000 0.02651 0.02557 0.06014 0.00452 0.00275 -0.01738 0.03740 0.01300 0.00040 0.00084 0.00044 0.00000 0.00469 0.00471 0.00520 0.00351 0.00366 0.00367 0.00195 C15 0.50815 1.00416 0.36825 1.00000 0.02559 0.06328 0.05643 -0.00629 0.00840 -0.00904 0.04820 0.01453 0.00043 0.00108 0.00045 0.00000 0.00480 0.00640 0.00497 0.00417 0.00372 0.00462 0.00227 H15 0.52737 1.09681 0.35464 1.00000 0.05784 0.00000 0.00000 C3 0.71155 1.03264 0.30471 1.00000 0.01281 0.05167 0.06254 -0.00385 0.00755 -0.01220 0.04213 0.01364 0.00036 0.00104 0.00043 0.00000 0.00432 0.00544 0.00526 0.00412 0.00355 0.00387 0.00206 H3 0.71815 1.14294 0.30540 1.00000 0.05056 0.00000 0.00000 C14 0.54659 0.87635 0.36576 1.00000 0.02429 0.05067 0.06250 0.00032 -0.00185 -0.00509 0.04599 0.01410 0.00040 0.00105 0.00044 0.00000 0.00471 0.00588 0.00499 0.00440 0.00359 0.00465 0.00207 C7 0.77542 1.07307 0.42381 1.00000 0.02456 0.03847 0.07621 0.00283 0.00315 -0.00586 0.04640 0.01386 0.00042 0.00097 0.00047 0.00000 0.00473 0.00551 0.00569 0.00410 0.00396 0.00384 0.00216 H7A 0.74717 1.16019 0.43656 1.00000 0.05568 0.00000 0.00000 H7B 0.81384 1.10925 0.39453 1.00000 0.05568 0.00000 0.00000 C6 0.62620 0.96368 0.21115 1.00000 0.01378 0.04082 0.06222 0.00553 0.00955 0.00202 0.03866 0.01415 0.00037 0.00092 0.00043 0.00000 0.00405 0.00499 0.00514 0.00384 0.00334 0.00360 0.00193 C26 0.62563 1.11131 0.16712 1.00000 0.01097 0.04247 0.06606 -0.00282 0.00946 -0.00498 0.03955 0.01541 0.00038 0.00101 0.00049 0.00000 0.00425 0.00572 0.00606 0.00428 0.00355 0.00373 0.00200 C2 0.62155 0.88224 0.34543 1.00000 0.02640 0.04381 0.04564 0.00601 0.00698 0.00776 0.03843 0.01423 0.00039 0.00097 0.00038 0.00000 0.00452 0.00508 0.00435 0.00375 0.00328 0.00390 0.00191 H2 0.63540 0.78290 0.32610 1.00000 0.04611 0.00000 0.00000 C29 0.55981 0.87330 0.19102 1.00000 0.02052 0.04224 0.06636 -0.00830 0.00555 -0.00561 0.04292 0.01353 0.00037 0.00101 0.00045 0.00000 0.00447 0.00507 0.00506 0.00414 0.00357 0.00403 0.00198 H29A 0.56204 0.83323 0.13957 1.00000 0.05151 0.00000 0.00000 H29B 0.55766 0.78791 0.22581 1.00000 0.05151 0.00000 0.00000 C13 0.85794 0.89346 0.48998 1.00000 0.03766 0.04556 0.05937 0.00515 0.00013 -0.00962 0.04763 0.01456 0.00044 0.00098 0.00047 0.00000 0.00519 0.00586 0.00521 0.00424 0.00406 0.00459 0.00221 H13 0.87250 0.86409 0.44228 1.00000 0.05716 0.00000 0.00000 C4 0.74940 0.96296 0.23743 1.00000 0.02220 0.03816 0.06955 0.00994 0.00446 0.00140 0.04323 0.01420 0.00039 0.00094 0.00045 0.00000 0.00447 0.00515 0.00523 0.00396 0.00368 0.00389 0.00204 H4 0.76407 1.04559 0.20441 1.00000 0.05188 0.00000 0.00000 C1 0.66796 0.92285 0.41206 1.00000 0.02174 0.04185 0.06223 0.00359 0.01099 -0.00313 0.04161 0.01390 0.00039 0.00092 0.00044 0.00000 0.00447 0.00526 0.00493 0.00369 0.00377 0.00363 0.00206 H1A 0.64812 1.00483 0.44092 1.00000 0.04993 0.00000 0.00000 H1B 0.67654 0.83628 0.44557 1.00000 0.04993 0.00000 0.00000 C23 0.70772 0.85276 0.11166 1.00000 0.03523 0.05159 0.07542 -0.00838 0.01096 0.00830 0.05378 0.01690 0.00048 0.00112 0.00050 0.00000 0.00569 0.00616 0.00616 0.00486 0.00469 0.00502 0.00236 C32 0.32149 0.83233 0.21345 1.00000 0.02135 0.06354 0.08208 0.00089 0.00330 -0.00929 0.05565 0.01610 0.00043 0.00111 0.00055 0.00000 0.00485 0.00676 0.00624 0.00474 0.00413 0.00439 0.00247 H32A 0.32020 0.76477 0.17032 1.00000 0.08347 0.00000 0.00000 H32B 0.27619 0.87924 0.21686 1.00000 0.08347 0.00000 0.00000 H32C 0.33310 0.77609 0.25948 1.00000 0.08347 0.00000 0.00000 C19 0.51905 0.74174 0.38894 1.00000 0.02784 0.04872 0.06700 0.00445 0.00170 -0.00380 0.04789 0.01525 0.00043 0.00103 0.00047 0.00000 0.00527 0.00602 0.00549 0.00454 0.00411 0.00431 0.00225 H19 0.54638 0.65407 0.38900 1.00000 0.05747 0.00000 0.00000 C11 0.86722 0.86082 0.62178 1.00000 0.03736 0.03875 0.07546 0.01357 -0.01457 -0.01991 0.05121 0.01475 0.00045 0.00105 0.00054 0.00000 0.00544 0.00530 0.00642 0.00460 0.00437 0.00461 0.00230 H11 0.88765 0.81173 0.66464 1.00000 0.06146 0.00000 0.00000 C10 0.81250 0.97105 0.62834 1.00000 0.05917 0.07558 0.06157 -0.01078 0.00257 -0.05330 0.06548 0.01478 0.00055 0.00124 0.00054 0.00000 0.00687 0.00773 0.00575 0.00548 0.00479 0.00633 0.00309 H10 0.79644 0.99788 0.67575 1.00000 0.07857 0.00000 0.00000 C5 0.69326 0.87282 0.19428 1.00000 0.02539 0.05628 0.05431 -0.00243 0.00145 0.00121 0.04536 0.01413 0.00040 0.00107 0.00041 0.00000 0.00459 0.00570 0.00484 0.00421 0.00352 0.00443 0.00205 H5 0.69043 0.77242 0.21800 1.00000 0.05443 0.00000 0.00000 C22 0.98084 0.95755 0.22661 1.00000 0.03082 0.06023 0.09112 0.00797 0.01056 0.01480 0.06045 0.01829 0.00047 0.00115 0.00053 0.00000 0.00538 0.00652 0.00666 0.00527 0.00470 0.00486 0.00257 H22A 0.96090 0.93833 0.17585 1.00000 0.09068 0.00000 0.00000 H22B 1.02677 0.91222 0.23246 1.00000 0.09068 0.00000 0.00000 H22C 0.98470 1.06509 0.23472 1.00000 0.09068 0.00000 0.00000 C31 0.37362 0.94687 0.20404 1.00000 0.02789 0.04523 0.07809 -0.00321 0.00504 -0.01667 0.05033 0.01498 0.00042 0.00101 0.00051 0.00000 0.00511 0.00540 0.00579 0.00430 0.00414 0.00431 0.00224 H31A 0.36228 1.00470 0.15778 1.00000 0.06039 0.00000 0.00000 H31B 0.37527 1.01598 0.24728 1.00000 0.06039 0.00000 0.00000 C16 0.43975 0.99685 0.39121 1.00000 0.01915 0.04348 0.08613 -0.01170 0.00417 -0.00151 0.04954 0.01450 0.00042 0.00099 0.00050 0.00000 0.00473 0.00602 0.00595 0.00439 0.00401 0.00401 0.00227 H16 0.41247 1.08453 0.39186 1.00000 0.05945 0.00000 0.00000 C24 0.67003 0.72455 0.00099 1.00000 0.04541 0.08891 0.06704 -0.02439 0.01347 -0.00872 0.06672 0.01669 0.00051 0.00137 0.00052 0.00000 0.00614 0.00793 0.00624 0.00563 0.00476 0.00570 0.00282 H24A 0.71138 0.66369 -0.00751 1.00000 0.08007 0.00000 0.00000 H24B 0.67428 0.82048 -0.02557 1.00000 0.08007 0.00000 0.00000 C21 0.93508 0.89161 0.28302 1.00000 0.02316 0.06257 0.08934 -0.00627 0.00909 0.01207 0.05813 0.01754 0.00043 0.00115 0.00053 0.00000 0.00496 0.00688 0.00620 0.00531 0.00421 0.00466 0.00255 H21A 0.93141 0.78262 0.27601 1.00000 0.06976 0.00000 0.00000 H21B 0.95428 0.91164 0.33461 1.00000 0.06976 0.00000 0.00000 C9 0.78550 1.03373 0.56365 1.00000 0.03332 0.02143 0.06266 0.00075 0.00278 -0.01851 0.03913 0.01314 0.00042 0.00088 0.00046 0.00000 0.00487 0.00444 0.00568 0.00367 0.00410 0.00364 0.00199 H9 0.74995 1.10533 0.56805 1.00000 0.04696 0.00000 0.00000 C18 0.45252 0.73518 0.41173 1.00000 0.02930 0.07117 0.07019 0.01173 -0.00078 -0.01139 0.05703 0.01663 0.00046 0.00127 0.00049 0.00000 0.00533 0.00707 0.00594 0.00505 0.00425 0.00521 0.00253 H18 0.43374 0.64314 0.42692 1.00000 0.06844 0.00000 0.00000 C27 0.61281 1.21896 0.04802 1.00000 0.05907 0.10368 0.04710 0.01795 0.00105 -0.01152 0.07003 0.01919 0.00056 0.00139 0.00049 0.00000 0.00673 0.00895 0.00568 0.00579 0.00456 0.00630 0.00304 H27A 0.65681 1.27335 0.05748 1.00000 0.08404 0.00000 0.00000 H27B 0.57456 1.28598 0.06022 1.00000 0.08404 0.00000 0.00000 C12 0.88740 0.83188 0.55238 1.00000 0.05203 0.03675 0.07021 0.00887 -0.00708 -0.02846 0.05340 0.01431 0.00049 0.00100 0.00053 0.00000 0.00604 0.00565 0.00661 0.00450 0.00506 0.00441 0.00249 H12 0.92446 0.76427 0.54732 1.00000 0.06408 0.00000 0.00000 C28 0.60499 1.17583 -0.03069 1.00000 0.11168 0.07959 0.08030 0.00607 0.00062 -0.00087 0.09071 0.02281 0.00076 0.00145 0.00064 0.00000 0.01109 0.00907 0.00841 0.00591 0.00703 0.00762 0.00392 H28A 0.64084 1.10353 -0.04164 1.00000 0.13607 0.00000 0.00000 H28B 0.60949 1.26394 -0.06235 1.00000 0.13607 0.00000 0.00000 H28C 0.55939 1.13103 -0.04102 1.00000 0.13607 0.00000 0.00000 C25 0.60816 0.64727 -0.02652 1.00000 0.06205 0.09008 0.08626 -0.00787 -0.00067 -0.03187 0.07965 0.01831 0.00061 0.00146 0.00062 0.00000 0.00787 0.00899 0.00757 0.00606 0.00580 0.00665 0.00350 H25A 0.60424 0.55315 0.00058 1.00000 0.11948 0.00000 0.00000 H25B 0.61068 0.62712 -0.08024 1.00000 0.11948 0.00000 0.00000 H25C 0.56768 0.70923 -0.01853 1.00000 0.11948 0.00000 0.00000 Final Structure Factor Calculation for s92 in C2 Total number of l.s. parameters = 384 Maximum vector length = 511 Memory required = 4643 / 25046 wR2 = 0.2782 before cycle 11 for 4596 data and 2 / 384 parameters GooF = S = 0.980; Restrained GooF = 0.980 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1542 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0942 for 2499 Fo > 4sig(Fo) and 0.1777 for all 4596 data wR2 = 0.2782, GooF = S = 0.980, Restrained GooF = 0.980 for all data Flack x parameter = -4.0266 with esd 3.0852 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 42.00 for non-hydrogen and 40.00 for hydrogen atoms Principal mean square atomic displacements U 0.0773 0.0397 0.0173 O8 0.0804 0.0497 0.0413 O6 0.0953 0.0325 0.0251 O7 0.1165 0.0417 0.0277 O1 0.0713 0.0439 0.0229 O5 0.0613 0.0375 0.0200 N1 0.0516 0.0401 0.0220 N2 0.1016 0.0472 0.0189 O2 0.0525 0.0511 0.0277 C30 0.0883 0.0491 0.0284 O4 0.0837 0.0490 0.0062 C20 0.0944 0.0762 0.0288 O3 0.0818 0.0607 0.0158 C17 0.0611 0.0429 0.0082 C8 0.0693 0.0527 0.0226 C15 0.0650 0.0527 0.0087 C3 0.0634 0.0515 0.0231 C14 0.0765 0.0405 0.0223 C7 0.0643 0.0395 0.0122 C6 0.0671 0.0426 0.0090 C26 0.0533 0.0391 0.0230 C2 0.0691 0.0406 0.0190 C29 0.0629 0.0488 0.0311 C13 0.0724 0.0353 0.0220 C4 0.0639 0.0421 0.0188 C1 0.0784 0.0542 0.0287 C23 0.0822 0.0654 0.0193 C32 0.0683 0.0483 0.0272 C19 0.0921 0.0435 0.0181 C11 0.1218 0.0619 0.0128 C10 0.0581 0.0527 0.0253 C5 0.0943 0.0629 0.0242 C22 0.0785 0.0548 0.0177 C31 0.0891 0.0405 0.0190 C16 0.1068 0.0528 0.0406 C24 0.0908 0.0651 0.0185 C21 0.0627 0.0468 0.0079 C9 0.0851 0.0596 0.0264 C18 0.1119 0.0565 0.0417 C27 0.0872 0.0582 0.0148 C12 0.1129 0.0855 0.0738 C28 0.1112 0.0875 0.0402 C25 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.019 0.031 0.040 0.051 0.062 0.076 0.096 0.127 0.181 1.000 Number in group 476. 484. 425. 486. 448. 445. 459. 455. 461. 457. GooF 0.835 0.908 0.944 1.009 0.945 1.074 1.043 1.046 1.009 0.973 K 2.697 1.134 1.247 1.102 1.018 1.082 1.039 1.069 1.047 1.034 Resolution(A) 0.84 0.88 0.93 0.97 1.03 1.10 1.19 1.32 1.50 1.89 inf Number in group 480. 439. 463. 462. 459. 465. 451. 460. 462. 455. GooF 0.787 0.887 1.006 0.912 1.021 1.073 1.060 0.927 1.022 1.070 K 1.233 1.074 1.078 1.032 0.987 1.097 1.068 1.048 1.072 1.030 R1 0.498 0.417 0.365 0.249 0.182 0.143 0.128 0.102 0.087 0.082 Recommended weighting scheme: WGHT 0.1467 0.0000 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 -4 0 2747.59 763.35 5.08 0.124 2.04 5 -5 1 307.34 52.44 4.88 0.032 1.62 -13 -5 2 254.74 32.93 4.87 0.026 1.14 14 -4 2 843.28 83.77 4.84 0.041 1.16 1 -7 5 -51.49 191.80 4.70 0.062 1.20 17 1 6 -204.13 941.73 4.47 0.138 1.04 13 -7 1 714.70 219.89 4.44 0.066 0.97 0 6 0 2110.50 1043.32 4.24 0.145 1.50 -8 0 2 2221.27 1075.25 4.23 0.147 2.37 14 4 2 518.43 83.55 4.22 0.041 1.16 11 7 1 951.63 257.75 4.20 0.072 1.03 10 -8 0 393.79 6.06 4.11 0.011 0.97 7 7 2 975.70 151.00 4.07 0.055 1.15 14 -4 0 1210.69 498.32 3.88 0.100 1.18 -3 7 2 1516.92 741.46 3.82 0.122 1.25 3 7 1 691.95 100.41 3.79 0.045 1.26 7 -7 4 484.97 90.87 3.70 0.043 1.12 -4 0 1 39839.66 23756.45 3.64 0.691 4.74 9 3 0 1590.13 797.47 3.58 0.127 1.75 -11 5 5 106.84 290.51 3.49 0.076 1.20 -16 0 4 961.67 385.74 3.48 0.088 1.19 8 6 2 5058.21 3007.43 3.44 0.246 1.26 8 8 1 616.77 110.55 3.36 0.047 1.02 16 -4 0 207.64 609.26 3.36 0.111 1.07 2 -4 1 307.33 60.65 3.32 0.035 2.17 13 7 1 743.02 218.54 3.27 0.066 0.97 17 5 6 -102.47 219.36 3.27 0.066 0.90 8 6 1 2526.58 1165.74 3.25 0.153 1.27 12 0 0 3621.67 2208.15 3.25 0.211 1.61 3 7 2 854.96 313.23 3.25 0.079 1.25 -6 -4 1 3226.78 1592.79 3.24 0.179 1.84 12 -6 7 383.00 41.97 3.24 0.029 0.99 13 3 2 206.95 46.47 3.15 0.031 1.31 4 0 1 149.28 0.03 3.15 0.001 4.61 -2 8 1 343.11 8.71 3.14 0.013 1.11 -3 3 3 382.64 652.49 3.13 0.114 2.50 -10 0 1 10200.44 6365.79 3.13 0.358 1.94 -8 6 1 1178.41 584.73 3.11 0.108 1.27 18 -4 1 359.84 52.06 3.10 0.032 0.97 -9 1 1 19887.24 12681.44 3.09 0.505 2.09 6 4 6 0.00 91.51 3.09 0.043 1.54 18 -4 3 362.41 54.29 3.08 0.033 0.95 14 2 9 51.00 515.37 3.05 0.102 1.07 -1 7 3 106.67 601.64 3.03 0.110 1.25 -8 -4 1 2018.56 1287.34 3.03 0.161 1.65 -9 -1 1 19636.37 12686.84 3.03 0.505 2.09 1 -5 0 864.41 541.73 3.01 0.104 1.79 16 -6 2 309.89 14.23 3.00 0.017 0.93 -12 4 5 54.60 381.61 2.99 0.088 1.25 -5 -3 1 584.38 269.21 2.98 0.074 2.36 Bond lengths and angles O8 - Distance Angles C30 1.3537 (0.0102) C31 1.4604 (0.0100) 115.36 (0.63) O8 - C30 O6 - Distance Angles C26 1.3231 (0.0099) C27 1.4222 (0.0124) 116.63 (0.74) O6 - C26 O7 - Distance Angles C30 1.1924 (0.0104) O7 - O1 - Distance Angles C20 1.2079 (0.0106) O1 - O5 - Distance Angles C26 1.1993 (0.0099) O5 - N1 - Distance Angles C3 1.4479 (0.0105) C7 1.4614 (0.0102) 113.00 (0.64) C1 1.4984 (0.0099) 106.18 (0.57) 114.04 (0.60) N1 - C3 C7 N2 - Distance Angles C6 1.4611 (0.0100) C2 1.4603 (0.0098) 118.72 (0.61) C3 1.4846 (0.0096) 106.87 (0.54) 106.29 (0.58) N2 - C6 C2 O2 - Distance Angles C20 1.3393 (0.0097) C21 1.4805 (0.0101) 118.34 (0.71) O2 - C20 C30 - Distance Angles O7 1.1924 (0.0104) O8 1.3537 (0.0102) 124.35 (0.77) C29 1.5024 (0.0120) 126.07 (0.78) 109.49 (0.77) C30 - O7 O8 O4 - Distance Angles C23 1.3558 (0.0110) C24 1.4350 (0.0106) 115.98 (0.71) O4 - C23 C20 - Distance Angles O1 1.2079 (0.0106) O2 1.3393 (0.0096) 125.29 (0.79) C4 1.4794 (0.0120) 124.53 (0.70) 110.19 (0.77) C20 - O1 O2 O3 - Distance Angles C23 1.2061 (0.0105) O3 - C17 - Distance Angles C16 1.3606 (0.0131) C18 1.3966 (0.0140) 120.33 (0.80) H17 0.9500 119.84 119.83 C17 - C16 C18 C8 - Distance Angles C9 1.3357 (0.0107) C13 1.4379 (0.0123) 115.58 (0.71) C7 1.4919 (0.0116) 125.80 (0.79) 118.63 (0.74) C8 - C9 C13 C15 - Distance Angles C14 1.3722 (0.0124) C16 1.4131 (0.0121) 119.46 (0.82) H15 0.9500 120.27 120.27 C15 - C14 C16 C3 - Distance Angles N1 1.4479 (0.0105) N2 1.4846 (0.0096) 106.76 (0.60) C4 1.5738 (0.0115) 114.19 (0.69) 106.29 (0.59) H3 1.0000 109.82 109.82 109.82 C3 - N1 N2 C4 C14 - Distance Angles C15 1.3722 (0.0124) C19 1.3954 (0.0121) 119.91 (0.75) C2 1.5201 (0.0113) 120.52 (0.79) 119.29 (0.79) C14 - C15 C19 C7 - Distance Angles N1 1.4614 (0.0102) C8 1.4919 (0.0116) 113.07 (0.68) H7A 0.9900 108.97 108.97 H7B 0.9900 108.97 108.97 107.77 C7 - N1 C8 H7A C6 - Distance Angles N2 1.4611 (0.0100) C26 1.5424 (0.0118) 108.53 (0.66) C29 1.5478 (0.0108) 113.99 (0.59) 110.62 (0.63) C5 1.5801 (0.0111) 102.52 (0.57) 109.24 (0.61) 111.58 (0.65) C6 - N2 C26 C29 C26 - Distance Angles O5 1.1993 (0.0099) O6 1.3231 (0.0099) 123.46 (0.78) C6 1.5424 (0.0118) 124.40 (0.76) 111.92 (0.73) C26 - O5 O6 C2 - Distance Angles N2 1.4603 (0.0099) C1 1.4952 (0.0112) 102.59 (0.65) C14 1.5201 (0.0113) 114.94 (0.65) 111.04 (0.60) H2 1.0000 109.34 109.34 109.34 C2 - N2 C1 C14 C29 - Distance Angles C30 1.5024 (0.0120) C6 1.5478 (0.0108) 112.81 (0.69) H29A 0.9900 109.03 109.03 H29B 0.9900 109.03 109.03 107.80 C29 - C30 C6 H29A C13 - Distance Angles C12 1.3421 (0.0118) C8 1.4379 (0.0123) 120.65 (0.85) H13 0.9500 119.67 119.67 C13 - C12 C8 C4 - Distance Angles C20 1.4794 (0.0120) C5 1.5296 (0.0114) 113.22 (0.70) C3 1.5738 (0.0115) 114.02 (0.65) 104.20 (0.59) H4 1.0000 108.39 108.39 108.39 C4 - C20 C5 C3 C1 - Distance Angles N1 1.4984 (0.0099) C2 1.4952 (0.0112) 102.86 (0.58) H1A 0.9900 111.19 111.19 H1B 0.9900 111.19 111.19 109.12 C1 - N1 C2 H1A C23 - Distance Angles O3 1.2061 (0.0105) O4 1.3558 (0.0110) 125.14 (0.81) C5 1.5281 (0.0114) 124.84 (0.86) 110.01 (0.78) C23 - O3 O4 C32 - Distance Angles C31 1.4601 (0.0119) H32A 0.9800 109.47 H32B 0.9800 109.47 109.47 H32C 0.9800 109.47 109.47 109.47 C32 - C31 H32A H32B C19 - Distance Angles C18 1.3771 (0.0122) C14 1.3954 (0.0121) 120.43 (0.87) H19 0.9500 119.79 119.79 C19 - C18 C14 C11 - Distance Angles C12 1.3463 (0.0122) C10 1.4620 (0.0143) 117.12 (0.84) H11 0.9500 121.44 121.44 C11 - C12 C10 C10 - Distance Angles C9 1.3625 (0.0133) C11 1.4620 (0.0143) 117.26 (0.88) H10 0.9500 121.37 121.37 C10 - C9 C11 C5 - Distance Angles C23 1.5281 (0.0114) C4 1.5296 (0.0114) 112.56 (0.69) C6 1.5801 (0.0111) 116.37 (0.65) 101.55 (0.63) H5 1.0000 108.66 108.66 108.66 C5 - C23 C4 C6 C22 - Distance Angles C21 1.5025 (0.0124) 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 C31 - Distance Angles O8 1.4604 (0.0100) C32 1.4601 (0.0119) 107.81 (0.72) H31A 0.9900 110.14 110.14 H31B 0.9900 110.14 110.14 108.46 C31 - O8 C32 H31A C16 - Distance Angles C17 1.3606 (0.0131) C15 1.4131 (0.0121) 120.24 (0.83) H16 0.9500 119.88 119.88 C16 - C17 C15 C24 - Distance Angles O4 1.4350 (0.0106) C25 1.4482 (0.0141) 107.36 (0.77) H24A 0.9900 110.24 110.24 H24B 0.9900 110.24 110.24 108.52 C24 - O4 C25 H24A C21 - Distance Angles O2 1.4805 (0.0101) C22 1.5025 (0.0124) 107.10 (0.74) H21A 0.9900 110.30 110.30 H21B 0.9900 110.30 110.30 108.55 C21 - O2 C22 H21A C9 - Distance Angles C8 1.3357 (0.0107) C10 1.3625 (0.0133) 125.80 (0.93) H9 0.9500 117.10 117.10 C9 - C8 C10 C18 - Distance Angles C19 1.3771 (0.0122) C17 1.3966 (0.0140) 119.59 (0.88) H18 0.9500 120.21 120.21 C18 - C19 C17 C27 - Distance Angles O6 1.4222 (0.0123) C28 1.4573 (0.0147) 109.94 (0.97) H27A 0.9900 109.68 109.67 H27B 0.9900 109.67 109.67 108.17 C27 - O6 C28 H27A C12 - Distance Angles C13 1.3421 (0.0118) C11 1.3463 (0.0122) 123.50 (1.01) H12 0.9500 118.25 118.25 C12 - C13 C11 C28 - Distance Angles C27 1.4573 (0.0147) H28A 0.9800 109.47 H28B 0.9800 109.47 109.47 H28C 0.9800 109.47 109.47 109.47 C28 - C27 H28A H28B C25 - Distance Angles C24 1.4482 (0.0141) H25A 0.9800 109.47 H25B 0.9800 109.47 109.47 H25C 0.9800 109.47 109.47 109.47 C25 - C24 H25A H25B FMAP and GRID set by program FMAP 2 3 37 GRID -1.471 -1 -2 1.471 1 2 R1 = 0.1594 for 2772 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.38 at 0.1208 0.4598 0.1304 [ 1.35 A from O6 ] Deepest hole -0.37 at 0.1827 0.4508 0.2477 [ 1.21 A from C5 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 4404 / 22807 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.6208 0.9598 0.1304 1.00000 0.05 0.38 1.35 O6 1.44 C6 1.51 C26 1.63 H29A Q2 1 0.6675 0.7423 0.1497 1.00000 0.05 0.34 1.25 O4 1.30 H5 1.46 C23 1.49 C5 Q3 1 0.6262 1.0753 0.1937 1.00000 0.05 0.29 0.57 C26 1.05 C6 1.42 O5 1.78 O6 Q4 1 0.6337 0.8971 0.2850 1.00000 0.05 0.28 0.91 N2 1.13 C2 1.26 H2 1.45 C6 Q5 1 0.7735 1.0652 0.4923 1.00000 0.05 0.28 0.82 C8 1.23 C7 1.31 C9 1.39 H7A Q6 1 0.4515 1.0904 0.4016 1.00000 0.05 0.27 0.77 H16 0.89 C16 1.50 C15 1.74 H15 Q7 1 0.7906 0.7541 0.1470 1.00000 0.05 0.27 1.91 C23 2.01 O3 2.19 O1 2.31 C20 Q8 1 0.7202 1.2924 0.3256 1.00000 0.05 0.26 1.39 H3 1.88 H10 1.93 C10 2.08 C11 Q9 1 0.7324 1.2557 0.4638 1.00000 0.05 0.26 1.04 H7A 1.99 C7 2.31 H9 2.34 C13 Q10 1 0.6177 1.1200 0.0228 1.00000 0.05 0.26 1.00 C27 1.09 C28 1.27 H28A 1.32 O6 Shortest distances between peaks (including symmetry equivalents) 1 3 1.53 5 9 1.94 1 2 2.17 3 4 2.28 2 7 2.39 1 10 2.40 8 9 2.49 1 4 2.81 2 4 2.89 5 9 2.90 Time profile in seconds ----------------------- 0.05: 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. 1.21: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.05: Set up l.s. refinement 0.00: Generate idealized H-atoms 8.52: Structure factors and derivatives 16.00: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.20: Apply other restraints 2.52: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.11: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.17: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 10:21:24 Total CPU time: 29.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++