+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 07skc0019p21c started at 12:43:19 on 06-May-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 07skc0019p21c in P2(1)/c CELL 0.71073 11.8885 6.2179 21.9459 90.000 104.852 90.000 ZERR 4.00 0.0005 0.0003 0.0009 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 56 116 4 16 V = 1568.08 F(000) = 608.0 Mu = 0.08 mm-1 Cell Wt = 1101.53 Rho = 1.166 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 HTAB O1A O31A HTAB N25 O31B EQIV_$1 -x+1, y+1/2, -z+1/2 HTAB N25 O31A_$1 HTAB N25 O31B_$1 EQIV_$2 x, y+1, z HTAB N25 O31A_$2 FMAP 2 PLAN 10 EQIV_$3 -x+1, -y+2, -z MPLA C31 O31A O31B MPLA C31_$3 O31A_$3 O31B_$3 SIZE 0.02 0.10 0.12 ACTA CONF BOND $H WGHT 0.00000 3.11610 L.S. 4 TEMP -153.00 FVAR 0.54804 MOLE 1 C1 1 0.203149 0.316590 0.071255 11.00000 0.02199 0.02694 = 0.01525 0.00365 0.00499 -0.00076 C2 1 0.154702 0.111461 0.037535 11.00000 0.02479 0.02363 = 0.02449 -0.00145 0.00652 -0.00057 AFIX 23 H2A 2 0.183884 -0.012163 0.065559 11.00000 -1.20000 H2B 2 0.184337 0.095820 -0.000475 11.00000 -1.20000 AFIX 0 C3 1 0.022228 0.102965 0.017778 11.00000 0.02313 0.02435 = 0.02758 -0.00354 0.00827 -0.00179 AFIX 23 H3A 2 -0.007941 0.112612 0.055754 11.00000 -1.20000 H3B 2 -0.007667 0.228263 -0.009388 11.00000 -1.20000 AFIX 0 O1A 4 0.319297 0.318277 0.086026 11.00000 0.02139 0.02934 = 0.03318 -0.00511 0.00495 -0.00262 AFIX 147 H1 2 0.343866 0.432322 0.105421 11.00000 0.05491 AFIX 0 O1B 4 0.145626 0.461625 0.083390 11.00000 0.02576 0.03196 = 0.03334 -0.01107 0.00703 -0.00063 MOLE 2 C21 1 0.939339 1.371344 0.175866 11.00000 0.02031 0.02906 = 0.02803 0.00192 0.00587 0.00110 AFIX 137 H21A 2 0.927582 1.215422 0.172096 11.00000 -1.50000 H21B 2 0.961470 1.411647 0.220525 11.00000 -1.50000 H21C 2 1.001293 1.413324 0.156180 11.00000 -1.50000 AFIX 0 C22 1 0.826877 1.485848 0.142898 11.00000 0.01903 0.01923 = 0.01708 -0.00155 0.00544 -0.00129 C23 1 0.718282 1.401788 0.162556 11.00000 0.01632 0.02140 = 0.01432 -0.00245 0.00253 -0.00005 AFIX 23 H23A 2 0.652260 1.493712 0.140679 11.00000 -1.20000 H23B 2 0.702123 1.256118 0.144188 11.00000 -1.20000 AFIX 0 C24 1 0.711662 1.384484 0.231797 11.00000 0.01798 0.01929 = 0.01701 0.00078 0.00397 -0.00283 C26 1 0.843498 1.729749 0.152602 11.00000 0.02810 0.02447 = 0.02914 0.00121 0.00953 -0.00213 AFIX 137 H26A 2 0.867879 1.761521 0.197821 11.00000 -1.50000 H26B 2 0.769914 1.803381 0.133764 11.00000 -1.50000 H26C 2 0.903297 1.779845 0.132406 11.00000 -1.50000 AFIX 0 C27 1 0.802276 1.441264 0.071833 11.00000 0.02552 0.03591 = 0.02074 -0.00138 0.00894 -0.00374 AFIX 137 H27A 2 0.868387 1.490109 0.056432 11.00000 -1.50000 H27B 2 0.731925 1.518684 0.049577 11.00000 -1.50000 H27C 2 0.790827 1.286562 0.064164 11.00000 -1.50000 AFIX 0 C28 1 0.730057 1.593702 0.269157 11.00000 0.02958 0.02133 = 0.01858 -0.00220 0.00652 -0.00250 AFIX 137 H28A 2 0.684386 1.708494 0.243726 11.00000 -1.50000 H28B 2 0.812745 1.632160 0.279783 11.00000 -1.50000 H28C 2 0.704874 1.575049 0.307995 11.00000 -1.50000 AFIX 0 C29 1 0.785119 1.204640 0.268770 11.00000 0.02998 0.02502 = 0.02252 0.00669 0.00825 0.00321 AFIX 137 H29A 2 0.764204 1.183604 0.308745 11.00000 -1.50000 H29B 2 0.867654 1.242921 0.277274 11.00000 -1.50000 H29C 2 0.770881 1.071390 0.244140 11.00000 -1.50000 AFIX 0 N25 3 0.585621 1.321093 0.225490 11.00000 0.02303 0.01990 = 0.01813 -0.00159 0.00840 -0.00161 AFIX 137 H25A 2 0.574653 1.296333 0.264430 11.00000 0.03141 H25B 2 0.568869 1.199574 0.201785 11.00000 0.03353 H25C 2 0.537933 1.429446 0.206482 11.00000 0.02672 AFIX 0 MOLE 3 C31 1 0.478512 0.796095 0.131438 11.00000 0.01888 0.02040 = 0.01947 0.00254 0.00645 0.00568 C32 1 0.456201 0.809183 0.060054 11.00000 0.02319 0.02409 = 0.01503 0.00020 0.00399 -0.00132 AFIX 23 H32A 2 0.481677 0.672482 0.044699 11.00000 -1.20000 H32B 2 0.371304 0.822395 0.041567 11.00000 -1.20000 AFIX 0 C33 1 0.516433 0.993661 0.035834 11.00000 0.02435 0.02240 = 0.01800 0.00092 0.00469 0.00065 AFIX 23 H33A 2 0.601745 0.975326 0.051216 11.00000 -1.20000 H33B 2 0.495332 1.130615 0.053085 11.00000 -1.20000 AFIX 0 O31A 4 0.431503 0.639294 0.153435 11.00000 0.02199 0.03223 = 0.01803 0.00393 0.00599 -0.00380 O31B 4 0.539684 0.932329 0.165815 11.00000 0.03916 0.02201 = 0.01927 -0.00286 0.00255 -0.00209 HKLF 4 Covalent radii and connectivity table for 07skc0019p21c in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1B O1A C2 C2 - C1 C3 C3 - C3_$4 C2 O1A - C1 O1B - C1 C21 - C22 C22 - C21 C27 C26 C23 C23 - C24 C22 C24 - C29 N25 C28 C23 C26 - C22 C27 - C22 C28 - C24 C29 - C24 N25 - C24 C31 - O31B O31A C32 C32 - C33 C31 C33 - C32 C33_$3 O31A - C31 O31B - C31 Operators for generating equivalent atoms: $1 -x+1, y+1/2, -z+1/2 $2 x, y+1, z $3 -x+1, -y+2, -z $4 -x, -y, -z 13653 Reflections read, of which 827 rejected -15 =< h =< 15, -8 =< k =< 7, -28 =< l =< 26, Max. 2-theta = 54.96 0 Systematic absence violations 0 Inconsistent equivalents 3562 Unique reflections, of which 0 suppressed R(int) = 0.0593 R(sigma) = 0.0686 Friedel opposites merged Maximum memory for data reduction = 2741 / 36100 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 = 3326 / 227223 wR2 = 0.1536 before cycle 1 for 3562 data and 183 / 183 parameters GooF = S = 1.101; Restrained GooF = 1.101 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 3.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.54804 0.00119 0.001 OSF Mean shift/esd = 0.001 Maximum = 0.005 for U13 O31A Max. shift = 0.000 A for C32 Max. dU = 0.000 for H25A Least-squares cycle 2 Maximum vector length = 511 Memory required = 3326 / 227223 wR2 = 0.1536 before cycle 2 for 3562 data and 183 / 183 parameters GooF = S = 1.101; Restrained GooF = 1.101 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 3.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.54804 0.00119 -0.001 OSF Mean shift/esd = 0.000 Maximum = 0.002 for U13 O31A Max. shift = 0.000 A for H28C Max. dU = 0.000 for O31A Least-squares cycle 3 Maximum vector length = 511 Memory required = 3326 / 227223 wR2 = 0.1536 before cycle 3 for 3562 data and 183 / 183 parameters GooF = S = 1.101; Restrained GooF = 1.101 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 3.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.54804 0.00119 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H1 Max. dU = 0.000 for H1 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3326 / 227223 wR2 = 0.1536 before cycle 4 for 3562 data and 183 / 183 parameters GooF = S = 1.101; Restrained GooF = 1.101 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 3.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.54804 0.00119 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x N25 Max. shift = 0.000 A for H26A Max. dU = 0.000 for H1 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2A 0.1839 -0.0122 0.0656 23 0.990 0.000 C2 C1 C3 H2B 0.1843 0.0958 -0.0005 23 0.990 0.000 C2 C1 C3 H3A -0.0079 0.1126 0.0558 23 0.990 0.000 C3 C3_$4 C2 H3B -0.0077 0.2283 -0.0094 23 0.990 0.000 C3 C3_$4 C2 H1 0.3439 0.4323 0.1054 147 0.840 0.000 O1A C1 H1 H21A 0.9276 1.2154 0.1721 137 0.980 0.000 C21 C22 H21A H21B 0.9615 1.4116 0.2205 137 0.980 0.000 C21 C22 H21A H21C 1.0013 1.4133 0.1562 137 0.980 0.000 C21 C22 H21A H23A 0.6523 1.4937 0.1407 23 0.990 0.000 C23 C24 C22 H23B 0.7021 1.2561 0.1442 23 0.990 0.000 C23 C24 C22 H26A 0.8679 1.7615 0.1978 137 0.980 0.000 C26 C22 H26A H26B 0.7699 1.8034 0.1338 137 0.980 0.000 C26 C22 H26A H26C 0.9033 1.7798 0.1324 137 0.980 0.000 C26 C22 H26A H27A 0.8684 1.4901 0.0564 137 0.980 0.000 C27 C22 H27A H27B 0.7319 1.5187 0.0496 137 0.980 0.000 C27 C22 H27A H27C 0.7908 1.2866 0.0642 137 0.980 0.000 C27 C22 H27A H28A 0.6844 1.7085 0.2437 137 0.980 0.000 C28 C24 H28A H28B 0.8127 1.6322 0.2798 137 0.980 0.000 C28 C24 H28A H28C 0.7049 1.5750 0.3080 137 0.980 0.000 C28 C24 H28A H29A 0.7642 1.1836 0.3087 137 0.980 0.000 C29 C24 H29A H29B 0.8677 1.2429 0.2773 137 0.980 0.000 C29 C24 H29A H29C 0.7709 1.0714 0.2441 137 0.980 0.000 C29 C24 H29A H25A 0.5747 1.2963 0.2644 137 0.910 0.000 N25 C24 H25A H25B 0.5689 1.1996 0.2018 137 0.910 0.000 N25 C24 H25A H25C 0.5379 1.4294 0.2065 137 0.910 0.000 N25 C24 H25A H32A 0.4817 0.6725 0.0447 23 0.990 0.000 C32 C33 C31 H32B 0.3713 0.8224 0.0416 23 0.990 0.000 C32 C33 C31 H33A 0.6017 0.9753 0.0512 23 0.990 0.000 C33 C32 C33_$3 H33B 0.4953 1.1306 0.0531 23 0.990 0.000 C33 C32 C33_$3 07skc0019p21c in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.20315 0.31659 0.07125 1.00000 0.02199 0.02694 0.01525 0.00365 0.00499 -0.00076 0.02135 0.00526 0.00023 0.00048 0.00012 0.00000 0.00136 0.00154 0.00124 0.00118 0.00105 0.00120 0.00059 C2 0.15470 0.11146 0.03754 1.00000 0.02479 0.02363 0.02449 -0.00145 0.00652 -0.00057 0.02426 0.00526 0.00024 0.00047 0.00013 0.00000 0.00146 0.00153 0.00141 0.00122 0.00116 0.00118 0.00062 H2A 0.18388 -0.01216 0.06556 1.00000 0.02912 0.00000 0.00000 H2B 0.18434 0.09582 -0.00048 1.00000 0.02912 0.00000 0.00000 C3 0.02223 0.10296 0.01778 1.00000 0.02313 0.02435 0.02758 -0.00354 0.00827 -0.00179 0.02469 0.00517 0.00024 0.00047 0.00013 0.00000 0.00145 0.00152 0.00148 0.00126 0.00117 0.00120 0.00062 H3A -0.00794 0.11261 0.05575 1.00000 0.02963 0.00000 0.00000 H3B -0.00767 0.22826 -0.00939 1.00000 0.02963 0.00000 0.00000 O1A 0.31930 0.31828 0.08603 1.00000 0.02139 0.02934 0.03318 -0.00511 0.00495 -0.00262 0.02835 0.00392 0.00016 0.00035 0.00010 0.00000 0.00102 0.00121 0.00116 0.00101 0.00086 0.00090 0.00048 H1 0.34387 0.43232 0.10542 1.00000 0.05491 0.00000 0.01233 O1B 0.14563 0.46163 0.08339 1.00000 0.02576 0.03196 0.03334 -0.01107 0.00703 -0.00063 0.03045 0.00376 0.00017 0.00034 0.00009 0.00000 0.00109 0.00122 0.00115 0.00097 0.00091 0.00093 0.00050 C21 0.93934 1.37134 0.17587 1.00000 0.02031 0.02906 0.02803 0.00192 0.00587 0.00110 0.02586 0.00553 0.00023 0.00048 0.00013 0.00000 0.00139 0.00164 0.00147 0.00128 0.00117 0.00120 0.00064 H21A 0.92758 1.21542 0.17210 1.00000 0.03879 0.00000 0.00000 H21B 0.96147 1.41165 0.22053 1.00000 0.03879 0.00000 0.00000 H21C 1.00129 1.41332 0.15618 1.00000 0.03879 0.00000 0.00000 C22 0.82688 1.48585 0.14290 1.00000 0.01903 0.01923 0.01708 -0.00155 0.00544 -0.00129 0.01830 0.00496 0.00022 0.00044 0.00012 0.00000 0.00127 0.00140 0.00124 0.00108 0.00103 0.00105 0.00055 C23 0.71828 1.40179 0.16256 1.00000 0.01632 0.02140 0.01432 -0.00245 0.00253 -0.00005 0.01760 0.00480 0.00021 0.00044 0.00011 0.00000 0.00124 0.00139 0.00118 0.00110 0.00097 0.00107 0.00054 H23A 0.65226 1.49371 0.14068 1.00000 0.02112 0.00000 0.00000 H23B 0.70212 1.25612 0.14419 1.00000 0.02112 0.00000 0.00000 C24 0.71166 1.38448 0.23180 1.00000 0.01798 0.01929 0.01701 0.00078 0.00397 -0.00283 0.01818 0.00491 0.00022 0.00043 0.00012 0.00000 0.00128 0.00138 0.00121 0.00109 0.00101 0.00106 0.00055 C26 0.84350 1.72975 0.15260 1.00000 0.02810 0.02447 0.02914 0.00121 0.00953 -0.00213 0.02684 0.00559 0.00025 0.00047 0.00014 0.00000 0.00155 0.00159 0.00154 0.00128 0.00125 0.00123 0.00065 H26A 0.86788 1.76152 0.19782 1.00000 0.04026 0.00000 0.00000 H26B 0.76991 1.80338 0.13376 1.00000 0.04026 0.00000 0.00000 H26C 0.90330 1.77985 0.13241 1.00000 0.04026 0.00000 0.00000 C27 0.80228 1.44126 0.07183 1.00000 0.02552 0.03591 0.02074 -0.00138 0.00894 -0.00374 0.02684 0.00546 0.00025 0.00052 0.00012 0.00000 0.00148 0.00177 0.00138 0.00129 0.00117 0.00129 0.00066 H27A 0.86839 1.49011 0.05643 1.00000 0.04026 0.00000 0.00000 H27B 0.73192 1.51868 0.04958 1.00000 0.04026 0.00000 0.00000 H27C 0.79083 1.28656 0.06416 1.00000 0.04026 0.00000 0.00000 C28 0.73006 1.59370 0.26916 1.00000 0.02958 0.02133 0.01858 -0.00220 0.00652 -0.00250 0.02310 0.00520 0.00025 0.00046 0.00012 0.00000 0.00152 0.00147 0.00131 0.00116 0.00115 0.00119 0.00061 H28A 0.68439 1.70849 0.24373 1.00000 0.03465 0.00000 0.00000 H28B 0.81274 1.63216 0.27978 1.00000 0.03465 0.00000 0.00000 H28C 0.70487 1.57505 0.30800 1.00000 0.03465 0.00000 0.00000 C29 0.78512 1.20464 0.26877 1.00000 0.02998 0.02502 0.02252 0.00669 0.00825 0.00321 0.02556 0.00577 0.00025 0.00047 0.00013 0.00000 0.00154 0.00155 0.00138 0.00124 0.00118 0.00125 0.00063 H29A 0.76420 1.18360 0.30875 1.00000 0.03834 0.00000 0.00000 H29B 0.86765 1.24292 0.27727 1.00000 0.03834 0.00000 0.00000 H29C 0.77088 1.07139 0.24414 1.00000 0.03834 0.00000 0.00000 N25 0.58562 1.32109 0.22549 1.00000 0.02303 0.01990 0.01813 -0.00159 0.00840 -0.00161 0.01978 0.00417 0.00018 0.00038 0.00010 0.00000 0.00119 0.00121 0.00111 0.00100 0.00093 0.00098 0.00050 H25A 0.57465 1.29633 0.26443 1.00000 0.03141 0.00000 0.00864 H25B 0.56887 1.19957 0.20179 1.00000 0.03353 0.00000 0.00900 H25C 0.53793 1.42945 0.20648 1.00000 0.02672 0.00000 0.00831 C31 0.47851 0.79610 0.13144 1.00000 0.01888 0.02040 0.01947 0.00254 0.00645 0.00568 0.01930 0.00526 0.00022 0.00044 0.00012 0.00000 0.00128 0.00143 0.00129 0.00115 0.00105 0.00111 0.00056 C32 0.45620 0.80918 0.06005 1.00000 0.02319 0.02409 0.01503 0.00020 0.00399 -0.00132 0.02094 0.00512 0.00023 0.00046 0.00012 0.00000 0.00137 0.00147 0.00123 0.00113 0.00104 0.00115 0.00058 H32A 0.48168 0.67248 0.04470 1.00000 0.02512 0.00000 0.00000 H32B 0.37130 0.82239 0.04157 1.00000 0.02512 0.00000 0.00000 C33 0.51643 0.99366 0.03583 1.00000 0.02435 0.02240 0.01800 0.00092 0.00469 0.00065 0.02172 0.00517 0.00024 0.00046 0.00012 0.00000 0.00139 0.00144 0.00131 0.00115 0.00110 0.00116 0.00059 H33A 0.60174 0.97533 0.05122 1.00000 0.02606 0.00000 0.00000 H33B 0.49533 1.13062 0.05308 1.00000 0.02606 0.00000 0.00000 O31A 0.43150 0.63929 0.15344 1.00000 0.02199 0.03223 0.01803 0.00393 0.00599 -0.00380 0.02392 0.00358 0.00016 0.00032 0.00008 0.00000 0.00099 0.00118 0.00091 0.00086 0.00078 0.00086 0.00045 O31B 0.53968 0.93233 0.16581 1.00000 0.03916 0.02201 0.01927 -0.00286 0.00255 -0.00209 0.02772 0.00366 0.00018 0.00032 0.00009 0.00000 0.00123 0.00108 0.00096 0.00086 0.00087 0.00092 0.00048 Final Structure Factor Calculation for 07skc0019p21c in P2(1)/c Total number of l.s. parameters = 183 Maximum vector length = 511 Memory required = 3143 / 22995 wR2 = 0.1536 before cycle 5 for 3562 data and 0 / 183 parameters GooF = S = 1.101; Restrained GooF = 1.101 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 3.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0791 for 2499 Fo > 4sig(Fo) and 0.1189 for all 3562 data wR2 = 0.1536, GooF = S = 1.101, Restrained GooF = 1.101 for all data Occupancy sum of asymmetric unit = 19.00 for non-hydrogen and 29.00 for hydrogen atoms Principal mean square atomic displacements U 0.0283 0.0219 0.0139 C1 0.0257 0.0246 0.0225 C2 0.0302 0.0221 0.0218 C3 0.0371 0.0276 0.0203 O1A 0.0442 0.0257 0.0215 O1B 0.0305 0.0269 0.0201 C21 0.0208 0.0179 0.0161 C22 0.0223 0.0172 0.0133 C23 0.0221 0.0169 0.0156 C24 0.0304 0.0279 0.0222 C26 0.0372 0.0251 0.0182 C27 0.0303 0.0217 0.0173 C28 0.0328 0.0270 0.0169 C29 0.0247 0.0192 0.0154 N25 0.0259 0.0182 0.0138 C31 0.0253 0.0225 0.0150 C32 0.0248 0.0225 0.0178 C33 0.0348 0.0214 0.0156 O31A 0.0422 0.0238 0.0171 O31B Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.007 0.015 0.022 0.031 0.040 0.051 0.065 0.085 0.126 1.000 Number in group 362. 390. 340. 357. 337. 362. 343. 358. 355. 358. GooF 1.183 1.140 1.131 1.183 1.100 1.116 1.165 1.035 0.974 0.953 K 11.891 2.044 1.264 1.118 1.164 1.032 1.019 0.989 1.004 1.006 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.66 inf Number in group 356. 369. 343. 358. 362. 348. 359. 355. 356. 356. GooF 1.250 1.234 1.136 1.172 1.119 1.198 1.025 0.887 0.842 1.064 K 1.165 1.154 1.100 1.043 1.047 1.027 0.984 0.975 1.008 1.008 R1 0.258 0.250 0.225 0.196 0.168 0.148 0.085 0.066 0.049 0.033 Recommended weighting scheme: WGHT 0.0000 3.1162 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) -10 5 8 146.22 50.88 3.74 0.040 0.85 -4 3 22 154.29 327.86 3.47 0.102 0.90 -11 5 12 97.20 26.15 3.44 0.029 0.79 3 3 3 25.76 1.01 3.37 0.006 1.72 -2 4 17 3.64 63.53 3.33 0.045 0.99 2 0 26 806.92 544.07 3.23 0.131 0.78 2 1 20 49.73 9.79 3.20 0.018 0.99 -5 7 2 35.13 120.88 3.15 0.062 0.83 6 3 17 88.30 24.10 3.14 0.028 0.86 6 0 4 12.84 63.44 3.08 0.045 1.67 1 3 25 137.77 19.45 3.07 0.025 0.77 -6 3 21 187.18 65.33 3.07 0.045 0.91 3 3 6 72.20 29.51 2.97 0.031 1.55 6 0 10 45.25 104.18 2.96 0.057 1.27 -7 4 17 117.16 13.38 2.95 0.021 0.92 -11 5 1 61.18 3.57 2.94 0.011 0.81 8 3 13 68.15 20.95 2.90 0.026 0.87 -15 1 6 91.68 36.49 2.90 0.034 0.79 -2 1 22 39.87 97.03 2.88 0.055 0.98 2 4 18 48.01 3.09 2.86 0.010 0.90 -1 1 26 59.43 0.86 2.85 0.005 0.82 3 5 18 35.88 0.88 2.83 0.005 0.80 -15 0 6 164.08 274.79 2.83 0.093 0.79 -3 2 25 105.71 41.20 2.80 0.036 0.84 -14 1 16 57.61 0.50 2.79 0.004 0.79 -5 6 4 -5.24 26.90 2.79 0.029 0.95 8 2 10 56.93 2.83 2.79 0.009 1.01 1 6 13 16.95 72.91 2.78 0.048 0.86 7 1 12 48.09 112.50 2.69 0.060 1.06 -4 0 20 249.97 351.58 2.67 0.105 1.09 -7 4 15 163.45 84.00 2.67 0.052 0.97 -1 1 4 2581.10 2894.78 2.65 0.303 4.06 -7 1 22 40.29 4.51 2.64 0.012 0.93 -8 0 20 38.27 0.13 2.64 0.002 0.98 -14 2 1 40.85 7.87 2.62 0.016 0.80 1 0 4 4597.32 5123.89 2.61 0.403 4.40 -5 4 24 51.20 0.77 2.61 0.005 0.78 7 0 14 67.72 149.34 2.60 0.069 0.99 -4 4 24 65.02 0.00 2.59 0.000 0.79 -2 6 18 79.95 155.61 2.56 0.070 0.79 -5 1 20 246.21 169.12 2.55 0.073 1.06 -4 3 20 116.95 45.21 2.55 0.038 0.96 -13 4 8 41.92 2.27 2.53 0.008 0.79 -9 5 5 177.94 108.25 2.53 0.059 0.91 6 6 2 67.55 124.75 2.51 0.063 0.90 -13 1 16 187.79 110.21 2.48 0.059 0.83 -1 3 5 467.38 367.47 2.48 0.108 1.87 -5 1 26 -5.56 23.22 2.48 0.027 0.83 1 7 4 -7.13 16.83 2.47 0.023 0.87 14 2 1 31.62 1.84 2.46 0.008 0.79 Bond lengths and angles C1 - Distance Angles O1B 1.2022 (0.0034) O1A 1.3351 (0.0031) 123.50 (0.27) C2 1.5125 (0.0039) 125.03 (0.25) 111.46 (0.24) C1 - O1B O1A C2 - Distance Angles C1 1.5125 (0.0039) C3 1.5235 (0.0037) 113.87 (0.24) H2A 0.9900 108.78 108.78 H2B 0.9900 108.78 108.78 107.66 C2 - C1 C3 H2A C3 - Distance Angles C3_$4 1.5219 (0.0055) C2 1.5235 (0.0037) 111.89 (0.29) H3A 0.9900 109.24 109.24 H3B 0.9900 109.24 109.24 107.92 C3 - C3_$4 C2 H3A O1A - Distance Angles C1 1.3351 (0.0031) H1 0.8400 109.47 O1A - C1 O1B - Distance Angles C1 1.2022 (0.0034) O1B - C21 - Distance Angles C22 1.5238 (0.0036) H21A 0.9800 109.47 H21B 0.9800 109.47 109.47 H21C 0.9800 109.47 109.47 109.47 C21 - C22 H21A H21B C22 - Distance Angles C21 1.5238 (0.0037) C27 1.5365 (0.0036) 108.25 (0.22) C26 1.5371 (0.0039) 109.22 (0.23) 107.63 (0.23) C23 1.5529 (0.0035) 113.68 (0.22) 105.41 (0.21) 112.34 (0.23) C22 - C21 C27 C26 C23 - Distance Angles C24 1.5454 (0.0034) C22 1.5529 (0.0035) 123.51 (0.21) H23A 0.9900 106.45 106.45 H23B 0.9900 106.45 106.45 106.49 C23 - C24 C22 H23A C24 - Distance Angles C29 1.5193 (0.0037) N25 1.5210 (0.0032) 106.01 (0.21) C28 1.5233 (0.0037) 110.95 (0.22) 105.81 (0.21) C23 1.5454 (0.0034) 114.16 (0.22) 103.05 (0.19) 115.68 (0.22) C24 - C29 N25 C28 C26 - Distance Angles C22 1.5371 (0.0039) H26A 0.9800 109.47 H26B 0.9800 109.47 109.47 H26C 0.9800 109.47 109.47 109.47 C26 - C22 H26A H26B C27 - Distance Angles C22 1.5365 (0.0036) H27A 0.9800 109.47 H27B 0.9800 109.47 109.47 H27C 0.9800 109.47 109.47 109.47 C27 - C22 H27A H27B C28 - Distance Angles C24 1.5233 (0.0037) H28A 0.9800 109.47 H28B 0.9800 109.47 109.47 H28C 0.9800 109.47 109.47 109.47 C28 - C24 H28A H28B C29 - Distance Angles C24 1.5193 (0.0037) H29A 0.9800 109.47 H29B 0.9800 109.47 109.47 H29C 0.9800 109.47 109.47 109.47 C29 - C24 H29A H29B N25 - Distance Angles C24 1.5210 (0.0032) H25A 0.9100 109.47 H25B 0.9100 109.47 109.47 H25C 0.9100 109.47 109.47 109.47 N25 - C24 H25A H25B C31 - Distance Angles O31B 1.2387 (0.0032) O31A 1.2784 (0.0032) 122.47 (0.24) C32 1.5225 (0.0035) 120.69 (0.24) 116.85 (0.24) C31 - O31B O31A C32 - Distance Angles C33 1.5186 (0.0038) C31 1.5225 (0.0035) 115.28 (0.23) H32A 0.9900 108.45 108.45 H32B 0.9900 108.45 108.45 107.49 C32 - C33 C31 H32A C33 - Distance Angles C32 1.5186 (0.0038) C33_$3 1.5224 (0.0049) 112.43 (0.29) H33A 0.9900 109.11 109.11 H33B 0.9900 109.11 109.11 107.85 C33 - C32 C33_$3 H33A O31A - Distance Angles C31 1.2784 (0.0032) O31A - O31B - Distance Angles C31 1.2387 (0.0032) O31B - Selected torsion angles 1.40 ( 0.41) O1B - C1 - C2 - C3 -178.35 ( 0.23) O1A - C1 - C2 - C3 178.15 ( 0.28) C1 - C2 - C3 - C3_$4 52.82 ( 0.34) C21 - C22 - C23 - C24 171.22 ( 0.25) C27 - C22 - C23 - C24 -71.85 ( 0.32) C26 - C22 - C23 - C24 -72.02 ( 0.33) C22 - C23 - C24 - C29 173.50 ( 0.23) C22 - C23 - C24 - N25 58.55 ( 0.34) C22 - C23 - C24 - C28 1.69 ( 0.38) O31B - C31 - C32 - C33 -178.23 ( 0.23) O31A - C31 - C32 - C33 -175.96 ( 0.28) C31 - C32 - C33 - C33_$3 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.81 2.634(3) 165.2 O1A-H1...O31A 0.91 1.83 2.737(3) 171.0 N25-H25B...O31B 0.91 2.07 2.942(3) 160.8 N25-H25A...O31A_$1 0.91 2.44 3.195(3) 140.0 N25-H25A...O31B_$1 0.91 1.98 2.879(3) 171.4 N25-H25C...O31A_$2 Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 9.8439 (0.0098) x - 3.4760 (0.0067) y - 3.7413 (0.1041) z = 1.4514 (0.0148) * 0.0000 (0.0000) C31 * 0.0000 (0.0000) O31A * 0.0000 (0.0000) O31B Rms deviation of fitted atoms = 0.0000 9.8439 (0.0098) x - 3.4760 (0.0067) y - 3.7412 (0.1041) z = 1.4404 (0.0243) Angle to previous plane (with approximate esd) = 0.00 ( 0.19 ) * 0.0000 (0.0000) C31_$3 * 0.0000 (0.0000) O31A_$3 * 0.0000 (0.0000) O31B_$3 Rms deviation of fitted atoms = 0.0000 FMAP and GRID set by program FMAP 2 3 28 GRID -1.000 -2 -2 1.000 2 2 R1 = 0.1187 for 3562 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.30 at 0.7885 0.4310 0.1573 [ 0.71 A from C22 ] Deepest hole -0.29 at 0.7133 0.9089 0.2208 [ 1.25 A from H29C ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 3039 / 19659 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.7885 1.4310 0.1573 1.00000 0.05 0.30 0.71 C22 0.89 C23 1.47 H23B 1.61 H23A Q2 1 0.7578 1.3164 0.2492 1.00000 0.05 0.30 0.72 C24 0.84 C29 1.37 H29B 1.53 H29A Q3 1 0.5148 0.6379 0.1970 1.00000 0.05 0.27 1.19 O31A 1.33 H25C 1.70 C31 1.81 H25A Q4 1 0.6400 1.4173 0.1243 1.00000 0.05 0.26 0.59 H23A 1.09 C23 1.26 H23B 2.20 C22 Q5 1 0.5957 1.6141 0.3380 1.00000 0.05 0.25 1.62 H28C 1.95 O31B 2.00 H25B 2.13 O1A Q6 1 0.9048 1.6774 0.2928 1.00000 0.05 0.24 1.09 H28B 1.96 H21A 2.00 H21C 2.07 C28 Q7 1 0.6020 0.8437 -0.0008 1.00000 0.05 0.24 1.41 H33A 1.41 H33B 1.72 C33 1.74 C33 Q8 1 0.0966 0.0918 0.0396 1.00000 0.05 0.23 0.71 C2 0.89 C3 1.23 H2A 1.38 H3A Q9 1 0.8431 1.3394 0.3246 1.00000 0.05 0.23 1.30 H29B 1.33 H29A 1.50 C29 2.06 H28B Q10 1 0.7213 1.4065 0.2016 1.00000 0.05 0.22 0.71 C24 0.85 C23 1.48 H23A 1.54 H23B Shortest distances between peaks (including symmetry equivalents) 2 10 1.17 1 10 1.42 2 9 1.71 4 10 1.72 1 4 1.73 1 2 2.26 6 9 2.39 9 10 2.75 8 8 2.75 3 4 2.80 2 4 2.81 3 10 2.82 2 6 2.86 Time profile in seconds ----------------------- 0.09: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.02: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.61: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.81: Structure factors and derivatives 0.88: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.09: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.13: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 07skc0019p21c finished at 12:43:22 Total CPU time: 2.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++