+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 07skc0010cc started at 15:42:14 on 02-Jul-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 07skc0010cc in Cc CELL 0.71073 13.8261 11.0607 9.6798 90.000 115.478 90.000 ZERR 4.00 0.0010 0.0010 0.0009 0.000 0.007 0.000 LATT -7 SYMM X, - Y, 1/2 + Z SFAC C H N O UNIT 48 92 4 16 V = 1336.34 F(000) = 536.0 Mu = 0.09 mm-1 Cell Wt = 981.26 Rho = 1.219 MERG 4 OMIT -3.00 55.00 SHEL 7 0.77 EQIV_$1 x-1/2, y+1/2, z-1 HTAB O1A O6A_$1 HTAB N21 O6B_$1 EQIV_$2 x-1/2, -y+3/2, z-1/2 HTAB N21 O6A_$2 FMAP 2 PLAN 10 SIZE 0.02 0.06 0.12 ACTA BOND $H WGHT 0.03020 1.07850 L.S. 4 TEMP -153.00 FVAR 0.52855 MOLE 1 C1 1 0.134469 0.854173 0.051206 11.00000 0.02565 0.02543 = 0.02166 0.00226 0.01011 0.00477 C2 1 0.210079 0.846961 0.217814 11.00000 0.02797 0.02450 = 0.02179 0.00243 0.00468 0.00224 AFIX 23 H2A 2 0.176554 0.887096 0.277765 11.00000 -1.20000 H2B 2 0.276067 0.892298 0.235197 11.00000 -1.20000 AFIX 0 C3 1 0.240942 0.718293 0.277588 11.00000 0.02436 0.02358 = 0.01843 0.00277 0.00581 0.00162 AFIX 23 H3A 2 0.271457 0.676141 0.215146 11.00000 -1.20000 H3B 2 0.175968 0.673811 0.266951 11.00000 -1.20000 AFIX 0 C4 1 0.322643 0.717379 0.445175 11.00000 0.02649 0.02203 = 0.02078 0.00319 0.00469 0.00467 AFIX 23 H4A 2 0.386423 0.764375 0.455849 11.00000 -1.20000 H4B 2 0.291102 0.757743 0.507519 11.00000 -1.20000 AFIX 0 C5 1 0.357365 0.590890 0.506494 11.00000 0.02623 0.02197 = 0.01717 -0.00049 0.00463 0.00167 AFIX 23 H5A 2 0.292756 0.542497 0.488289 11.00000 -1.20000 H5B 2 0.393070 0.552905 0.448078 11.00000 -1.20000 AFIX 0 C6 1 0.432477 0.585654 0.674950 11.00000 0.02277 0.02073 = 0.02050 0.00209 0.00999 0.00152 O1A 4 0.113149 0.967388 0.002616 11.00000 0.04194 0.02140 = 0.02175 0.00225 -0.00051 0.00559 AFIX 147 H1 2 0.068118 0.967902 -0.089540 11.00000 0.05061 AFIX 0 O1B 4 0.097224 0.767572 -0.030689 11.00000 0.04923 0.02508 = 0.02178 0.00157 -0.00010 0.00126 O6A 4 0.479758 0.485005 0.724527 11.00000 0.04270 0.02318 = 0.01861 0.00259 0.00322 0.01169 O6B 4 0.443572 0.675045 0.757362 11.00000 0.05036 0.02553 = 0.02095 -0.00085 0.00378 0.01044 MOLE 2 C22 1 -0.072152 1.287550 0.082452 11.00000 0.03102 0.02869 = 0.03227 0.00067 0.01545 -0.00146 AFIX 23 H22A 2 -0.041264 1.320917 0.187570 11.00000 -1.20000 H22B 2 -0.137515 1.241813 0.067300 11.00000 -1.20000 AFIX 0 C23 1 -0.102807 1.390954 -0.030838 11.00000 0.02777 0.02789 = 0.03387 0.00251 0.01170 0.00566 AFIX 23 H23A 2 -0.168337 1.429454 -0.033884 11.00000 -1.20000 H23B 2 -0.121031 1.357109 -0.133754 11.00000 -1.20000 AFIX 0 C24 1 -0.017982 1.488808 0.001338 11.00000 0.03779 0.02525 = 0.03662 0.00244 0.01417 0.00532 AFIX 23 H24A 2 -0.044765 1.547527 -0.084152 11.00000 -1.20000 H24B 2 -0.009020 1.532646 0.095261 11.00000 -1.20000 AFIX 0 C25 1 0.091436 1.443780 0.021709 11.00000 0.03449 0.02286 = 0.04068 0.00184 0.01654 -0.00154 AFIX 23 H25A 2 0.136654 1.514256 0.025503 11.00000 -1.20000 H25B 2 0.082354 1.394545 -0.068476 11.00000 -1.20000 AFIX 0 C26 1 0.149293 1.368148 0.166106 11.00000 0.02464 0.02893 = 0.03362 -0.00154 0.00849 -0.00487 AFIX 23 H26A 2 0.227438 1.378429 0.201125 11.00000 -1.20000 H26B 2 0.131035 1.400634 0.247235 11.00000 -1.20000 AFIX 0 C27 1 0.124146 1.234148 0.149272 11.00000 0.02466 0.02664 = 0.02778 0.00277 0.00877 0.00370 AFIX 23 H27A 2 0.162152 1.196757 0.093673 11.00000 -1.20000 H27B 2 0.153120 1.197614 0.252641 11.00000 -1.20000 AFIX 0 N21 3 0.007196 1.202634 0.066954 11.00000 0.02910 0.01973 = 0.02204 -0.00015 0.00746 -0.00009 AFIX 23 H21A 2 -0.009579 1.195410 -0.035534 11.00000 0.02629 H21B 2 -0.002341 1.127735 0.100557 11.00000 0.05174 AFIX 0 HKLF 4 Covalent radii and connectivity table for 07skc0010cc in Cc C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1B O1A C2 C2 - C1 C3 C3 - C2 C4 C4 - C5 C3 C5 - C6 C4 C6 - O6B O6A C5 O1A - C1 O1B - C1 O6A - C6 O6B - C6 C22 - N21 C23 C23 - C22 C24 C24 - C25 C23 C25 - C24 C26 C26 - C27 C25 C27 - N21 C26 N21 - C22 C27 Operators for generating equivalent atoms: $1 x-1/2, y+1/2, z-1 $2 x-1/2, -y+3/2, z-1/2 Floating origin restraints generated 10419 Reflections read, of which 292 rejected -17 =< h =< 17, -14 =< k =< 14, -12 =< l =< 12, Max. 2-theta = 54.96 0 Systematic absence violations 0 Inconsistent equivalents 1536 Unique reflections, of which 0 suppressed R(int) = 0.0670 R(sigma) = 0.0398 Friedel opposites merged Maximum memory for data reduction = 2151 / 18556 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 = 2651 / 197348 wR2 = 0.0993 before cycle 1 for 1536 data and 158 / 158 parameters GooF = S = 1.108; Restrained GooF = 1.108 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0302 * P )^2 + 1.08 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.52856 0.00135 0.006 OSF Mean shift/esd = 0.003 Maximum = 0.009 for z O1B Max. shift = 0.000 A for H1 Max. dU = 0.000 for H1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2651 / 197348 wR2 = 0.0993 before cycle 2 for 1536 data and 158 / 158 parameters GooF = S = 1.108; Restrained GooF = 1.108 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0302 * P )^2 + 1.08 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.52856 0.00135 0.003 OSF Mean shift/esd = 0.001 Maximum = -0.004 for U11 H1 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2651 / 197348 wR2 = 0.0993 before cycle 3 for 1536 data and 158 / 158 parameters GooF = S = 1.108; Restrained GooF = 1.107 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0302 * P )^2 + 1.08 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.52856 0.00135 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for U11 H1 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H1 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2651 / 197348 wR2 = 0.0993 before cycle 4 for 1536 data and 158 / 158 parameters GooF = S = 1.108; Restrained GooF = 1.107 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0302 * P )^2 + 1.08 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.52856 0.00135 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y C23 Max. shift = 0.000 A for H1 Max. dU = 0.000 for H1 Largest correlation matrix elements 0.554 U13 C1 / U33 C1 0.520 U13 C25 / U11 C25 0.518 U13 C6 / U33 C6 0.543 U13 C22 / U33 C22 0.519 U13 C22 / U11 C22 0.511 U13 C23 / U11 C23 0.524 U13 C6 / U11 C6 0.518 U13 C25 / U33 C25 0.504 U13 C1 / U11 C1 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2A 0.1766 0.8871 0.2778 23 0.990 0.000 C2 C1 C3 H2B 0.2761 0.8923 0.2352 23 0.990 0.000 C2 C1 C3 H3A 0.2715 0.6761 0.2151 23 0.990 0.000 C3 C2 C4 H3B 0.1760 0.6738 0.2669 23 0.990 0.000 C3 C2 C4 H4A 0.3864 0.7644 0.4558 23 0.990 0.000 C4 C5 C3 H4B 0.2911 0.7577 0.5075 23 0.990 0.000 C4 C5 C3 H5A 0.2928 0.5425 0.4883 23 0.990 0.000 C5 C6 C4 H5B 0.3931 0.5529 0.4481 23 0.990 0.000 C5 C6 C4 H1 0.0681 0.9679 -0.0895 147 0.840 0.000 O1A C1 H1 H22A -0.0413 1.3209 0.1876 23 0.990 0.000 C22 N21 C23 H22B -0.1375 1.2418 0.0673 23 0.990 0.000 C22 N21 C23 H23A -0.1683 1.4295 -0.0339 23 0.990 0.000 C23 C22 C24 H23B -0.1210 1.3571 -0.1338 23 0.990 0.000 C23 C22 C24 H24A -0.0448 1.5475 -0.0842 23 0.990 0.000 C24 C25 C23 H24B -0.0090 1.5326 0.0953 23 0.990 0.000 C24 C25 C23 H25A 0.1367 1.5143 0.0255 23 0.990 0.000 C25 C24 C26 H25B 0.0824 1.3945 -0.0685 23 0.990 0.000 C25 C24 C26 H26A 0.2274 1.3784 0.2011 23 0.990 0.000 C26 C27 C25 H26B 0.1310 1.4006 0.2472 23 0.990 0.000 C26 C27 C25 H27A 0.1622 1.1968 0.0937 23 0.990 0.000 C27 N21 C26 H27B 0.1531 1.1976 0.2526 23 0.990 0.000 C27 N21 C26 H21A -0.0096 1.1954 -0.0355 23 0.920 0.000 N21 C22 C27 H21B -0.0023 1.1277 0.1006 23 0.920 0.000 N21 C22 C27 07skc0010cc in Cc ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.13447 0.85417 0.05121 1.00000 0.02566 0.02543 0.02165 0.00225 0.01011 0.00477 0.02427 0.00596 0.00023 0.00026 0.00030 0.00000 0.00149 0.00151 0.00144 0.00113 0.00124 0.00118 0.00062 C2 0.21008 0.84696 0.21781 1.00000 0.02797 0.02450 0.02179 0.00244 0.00469 0.00223 0.02687 0.00642 0.00025 0.00028 0.00033 0.00000 0.00155 0.00153 0.00138 0.00110 0.00117 0.00116 0.00064 H2A 0.17656 0.88710 0.27777 1.00000 0.03225 0.00000 0.00000 H2B 0.27607 0.89230 0.23520 1.00000 0.03225 0.00000 0.00000 C3 0.24094 0.71829 0.27759 1.00000 0.02437 0.02358 0.01844 0.00278 0.00581 0.00162 0.02332 0.00583 0.00023 0.00025 0.00031 0.00000 0.00146 0.00143 0.00130 0.00109 0.00112 0.00108 0.00060 H3A 0.27146 0.67614 0.21514 1.00000 0.02799 0.00000 0.00000 H3B 0.17597 0.67381 0.26695 1.00000 0.02799 0.00000 0.00000 C4 0.32264 0.71738 0.44518 1.00000 0.02649 0.02203 0.02079 0.00318 0.00469 0.00467 0.02503 0.00606 0.00023 0.00026 0.00031 0.00000 0.00149 0.00142 0.00135 0.00110 0.00114 0.00119 0.00061 H4A 0.38642 0.76437 0.45585 1.00000 0.03004 0.00000 0.00000 H4B 0.29110 0.75774 0.50752 1.00000 0.03004 0.00000 0.00000 C5 0.35736 0.59089 0.50649 1.00000 0.02624 0.02197 0.01718 -0.00049 0.00463 0.00167 0.02345 0.00588 0.00023 0.00025 0.00031 0.00000 0.00148 0.00144 0.00123 0.00109 0.00110 0.00114 0.00060 H5A 0.29275 0.54250 0.48829 1.00000 0.02814 0.00000 0.00000 H5B 0.39307 0.55290 0.44808 1.00000 0.02814 0.00000 0.00000 C6 0.43248 0.58565 0.67495 1.00000 0.02277 0.02072 0.02049 0.00209 0.00998 0.00152 0.02109 0.00583 0.00022 0.00025 0.00030 0.00000 0.00140 0.00139 0.00129 0.00110 0.00111 0.00110 0.00057 O1A 0.11315 0.96739 0.00262 1.00000 0.04194 0.02141 0.02175 0.00224 -0.00051 0.00559 0.03336 0.00424 0.00018 0.00017 0.00023 0.00000 0.00138 0.00109 0.00111 0.00085 0.00097 0.00092 0.00055 H1 0.06810 0.96790 -0.08953 1.00000 0.05046 0.00000 0.01190 O1B 0.09722 0.76757 -0.03069 1.00000 0.04923 0.02509 0.02178 0.00157 -0.00009 0.00126 0.03744 0.00439 0.00019 0.00019 0.00024 0.00000 0.00146 0.00112 0.00109 0.00088 0.00096 0.00099 0.00058 O6A 0.47976 0.48500 0.72453 1.00000 0.04271 0.02318 0.01861 0.00259 0.00322 0.01169 0.03167 0.00439 0.00018 0.00019 0.00021 0.00000 0.00126 0.00107 0.00100 0.00079 0.00092 0.00093 0.00052 O6B 0.44357 0.67504 0.75736 1.00000 0.05037 0.02553 0.02095 -0.00085 0.00378 0.01044 0.03635 0.00449 0.00019 0.00019 0.00023 0.00000 0.00144 0.00112 0.00106 0.00089 0.00097 0.00101 0.00057 C22 -0.07215 1.28755 0.08245 1.00000 0.03103 0.02869 0.03227 0.00068 0.01544 -0.00146 0.03002 0.00679 0.00025 0.00029 0.00036 0.00000 0.00161 0.00163 0.00163 0.00128 0.00132 0.00125 0.00067 H22A -0.04127 1.32092 0.18757 1.00000 0.03603 0.00000 0.00000 H22B -0.13752 1.24181 0.06729 1.00000 0.03603 0.00000 0.00000 C23 -0.10281 1.39095 -0.03083 1.00000 0.02777 0.02789 0.03387 0.00251 0.01170 0.00566 0.03039 0.00663 0.00025 0.00027 0.00036 0.00000 0.00156 0.00160 0.00163 0.00128 0.00133 0.00122 0.00067 H23A -0.16834 1.42945 -0.03388 1.00000 0.03647 0.00000 0.00000 H23B -0.12103 1.35711 -0.13375 1.00000 0.03647 0.00000 0.00000 C24 -0.01798 1.48881 0.00134 1.00000 0.03779 0.02526 0.03662 0.00243 0.01417 0.00532 0.03387 0.00697 0.00026 0.00029 0.00038 0.00000 0.00176 0.00160 0.00171 0.00121 0.00145 0.00123 0.00073 H24A -0.04477 1.54753 -0.08415 1.00000 0.04064 0.00000 0.00000 H24B -0.00902 1.53265 0.09526 1.00000 0.04064 0.00000 0.00000 C25 0.09144 1.44378 0.02171 1.00000 0.03450 0.02287 0.04069 0.00184 0.01654 -0.00154 0.03255 0.00695 0.00026 0.00028 0.00038 0.00000 0.00166 0.00147 0.00173 0.00128 0.00139 0.00122 0.00068 H25A 0.13665 1.51426 0.02550 1.00000 0.03906 0.00000 0.00000 H25B 0.08235 1.39455 -0.06848 1.00000 0.03906 0.00000 0.00000 C26 0.14929 1.36815 0.16610 1.00000 0.02464 0.02893 0.03362 -0.00154 0.00849 -0.00487 0.03048 0.00639 0.00024 0.00029 0.00036 0.00000 0.00150 0.00162 0.00164 0.00127 0.00128 0.00115 0.00068 H26A 0.22744 1.37843 0.20112 1.00000 0.03658 0.00000 0.00000 H26B 0.13104 1.40063 0.24724 1.00000 0.03658 0.00000 0.00000 C27 0.12415 1.23415 0.14927 1.00000 0.02466 0.02663 0.02778 0.00277 0.00877 0.00371 0.02724 0.00621 0.00023 0.00027 0.00034 0.00000 0.00146 0.00153 0.00149 0.00120 0.00120 0.00119 0.00063 H27A 0.16215 1.19676 0.09368 1.00000 0.03269 0.00000 0.00000 H27B 0.15312 1.19762 0.25264 1.00000 0.03269 0.00000 0.00000 N21 0.00720 1.20264 0.06695 1.00000 0.02911 0.01973 0.02204 -0.00016 0.00747 -0.00009 0.02487 0.00491 0.00019 0.00021 0.00027 0.00000 0.00128 0.00119 0.00114 0.00100 0.00098 0.00099 0.00052 H21A -0.00958 1.19541 -0.03554 1.00000 0.02623 0.00000 0.00836 H21B -0.00234 1.12774 0.10055 1.00000 0.05166 0.00000 0.01183 Final Structure Factor Calculation for 07skc0010cc in Cc Total number of l.s. parameters = 158 Maximum vector length = 511 Memory required = 2495 / 25046 wR2 = 0.0993 before cycle 5 for 1536 data and 2 / 158 parameters GooF = S = 1.108; Restrained GooF = 1.107 for 2 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0302 * P )^2 + 1.08 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0438 for 1348 Fo > 4sig(Fo) and 0.0541 for all 1536 data wR2 = 0.0993, GooF = S = 1.108, Restrained GooF = 1.107 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 17.00 for non-hydrogen and 23.00 for hydrogen atoms Principal mean square atomic displacements U 0.0304 0.0222 0.0202 C1 0.0362 0.0258 0.0186 C2 0.0285 0.0247 0.0167 C3 0.0345 0.0246 0.0160 C4 0.0323 0.0215 0.0165 C5 0.0238 0.0210 0.0184 C6 0.0605 0.0235 0.0161 O1A 0.0678 0.0255 0.0189 O1B 0.0577 0.0228 0.0145 O6A 0.0668 0.0223 0.0199 O6B 0.0330 0.0306 0.0265 C22 0.0355 0.0335 0.0222 C23 0.0414 0.0370 0.0232 C24 0.0411 0.0344 0.0222 C25 0.0385 0.0316 0.0213 C26 0.0311 0.0295 0.0212 C27 0.0333 0.0216 0.0197 N21 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.019 0.029 0.037 0.045 0.054 0.065 0.080 0.101 0.143 1.000 Number in group 162. 156. 158. 152. 146. 156. 150. 148. 155. 153. GooF 1.173 1.195 1.222 1.104 1.056 1.045 1.155 0.907 1.021 1.153 K 1.380 1.062 1.050 1.008 1.008 0.997 1.002 1.004 1.009 0.993 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.65 inf Number in group 157. 154. 152. 155. 150. 153. 154. 153. 154. 154. GooF 1.199 1.228 1.162 1.075 1.183 1.075 1.036 0.944 0.959 1.179 K 1.037 1.069 1.066 1.019 1.017 0.983 1.000 0.997 1.012 0.990 R1 0.146 0.142 0.097 0.086 0.081 0.052 0.041 0.029 0.025 0.022 Recommended weighting scheme: WGHT 0.0302 1.0785 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) -2 0 2 6588.16 7908.89 4.31 0.473 4.64 -12 6 3 53.58 11.90 3.74 0.018 0.97 -4 2 9 79.36 158.21 3.62 0.067 1.05 1 1 1 1026.69 1219.71 3.48 0.186 5.30 -13 7 5 -3.20 27.96 3.45 0.028 0.88 -6 10 9 34.00 83.04 3.30 0.048 0.77 14 2 2 99.81 55.18 3.20 0.040 0.80 -7 11 7 39.35 4.11 3.11 0.011 0.80 -3 13 4 35.50 7.46 3.01 0.015 0.80 -13 7 8 153.40 98.98 2.98 0.053 0.82 -5 1 10 49.99 14.71 2.76 0.020 0.96 -2 2 2 2639.06 2965.56 2.74 0.290 3.55 -10 10 2 45.97 2.43 2.70 0.008 0.86 -11 7 6 138.74 189.68 2.67 0.073 0.94 6 0 6 23.70 62.72 2.66 0.042 1.01 -5 13 1 308.28 203.76 2.65 0.076 0.81 12 4 4 3.63 31.28 2.62 0.030 0.78 -6 6 6 35.92 17.55 2.61 0.022 1.18 3 5 9 167.65 120.11 2.60 0.058 0.81 9 9 0 78.02 114.14 2.59 0.057 0.92 0 4 3 1824.17 1623.79 2.58 0.214 2.01 -12 6 9 35.46 7.44 2.57 0.015 0.84 -3 3 1 627.36 541.88 2.55 0.124 2.88 -15 1 3 46.13 14.09 2.53 0.020 0.91 -17 1 8 -0.32 26.22 2.50 0.027 0.78 3 5 8 9.74 30.17 2.48 0.029 0.88 -11 3 9 11.56 36.54 2.47 0.032 0.94 -4 2 6 86.86 62.18 2.45 0.042 1.55 -15 5 5 75.50 40.86 2.43 0.034 0.85 -12 10 2 135.23 92.52 2.43 0.051 0.79 7 1 3 15.53 32.91 2.42 0.031 1.28 -4 10 7 44.36 77.40 2.41 0.047 0.86 3 7 8 9.07 28.92 2.40 0.029 0.82 -17 3 6 45.37 17.63 2.40 0.022 0.79 13 3 3 29.50 9.99 2.38 0.017 0.79 -14 2 11 6.51 30.10 2.36 0.029 0.78 -13 3 1 35.46 64.25 2.36 0.043 0.97 4 4 1 1101.62 981.47 2.35 0.167 1.90 0 0 6 58.90 36.56 2.34 0.032 1.46 -6 0 4 596.65 694.21 2.33 0.140 1.99 3 11 6 281.32 205.95 2.32 0.076 0.78 -7 3 2 3690.49 3345.47 2.29 0.308 1.74 -15 1 7 114.09 152.62 2.28 0.066 0.89 11 5 4 47.05 14.52 2.26 0.020 0.81 8 4 6 62.52 39.11 2.24 0.033 0.85 7 9 0 201.46 246.17 2.24 0.083 1.01 13 1 0 2.63 13.60 2.21 0.020 0.96 -4 2 3 2866.70 3148.92 2.20 0.298 2.51 10 10 1 43.01 69.09 2.18 0.044 0.80 -8 2 11 194.30 150.60 2.17 0.065 0.87 Bond lengths and angles C1 - Distance Angles O1B 1.2083 (0.0035) O1A 1.3255 (0.0034) 123.31 (0.25) C2 1.4999 (0.0039) 124.51 (0.25) 112.18 (0.24) C1 - O1B O1A C2 - Distance Angles C1 1.4999 (0.0039) C3 1.5264 (0.0039) 114.15 (0.24) H2A 0.9900 108.72 108.72 H2B 0.9900 108.72 108.72 107.63 C2 - C1 C3 H2A C3 - Distance Angles C2 1.5264 (0.0039) C4 1.5268 (0.0035) 111.55 (0.22) H3A 0.9900 109.31 109.31 H3B 0.9900 109.31 109.31 107.96 C3 - C2 C4 H3A C4 - Distance Angles C5 1.5149 (0.0038) C3 1.5268 (0.0035) 112.79 (0.22) H4A 0.9900 109.03 109.03 H4B 0.9900 109.03 109.03 107.80 C4 - C5 C3 H4A C5 - Distance Angles C6 1.5113 (0.0038) C4 1.5149 (0.0038) 114.39 (0.23) H5A 0.9900 108.66 108.66 H5B 0.9900 108.66 108.66 107.60 C5 - C6 C4 H5A C6 - Distance Angles O6B 1.2378 (0.0033) O6A 1.2756 (0.0034) 123.59 (0.26) C5 1.5113 (0.0038) 120.13 (0.24) 116.26 (0.24) C6 - O6B O6A O1A - Distance Angles C1 1.3255 (0.0034) H1 0.8400 109.47 O1A - C1 O1B - Distance Angles C1 1.2083 (0.0035) O1B - O6A - Distance Angles C6 1.2756 (0.0034) O6A - O6B - Distance Angles C6 1.2378 (0.0033) O6B - C22 - Distance Angles N21 1.4999 (0.0038) C23 1.5134 (0.0043) 112.93 (0.25) H22A 0.9900 109.00 109.00 H22B 0.9900 109.00 109.00 107.78 C22 - N21 C23 H22A C23 - Distance Angles C22 1.5134 (0.0043) C24 1.5263 (0.0044) 115.91 (0.26) H23A 0.9900 108.31 108.31 H23B 0.9900 108.31 108.31 107.41 C23 - C22 C24 H23A C24 - Distance Angles C25 1.5228 (0.0046) C23 1.5263 (0.0044) 115.33 (0.26) H24A 0.9900 108.44 108.44 H24B 0.9900 108.44 108.44 107.48 C24 - C25 C23 H24A C25 - Distance Angles C24 1.5228 (0.0046) C26 1.5269 (0.0045) 113.44 (0.27) H25A 0.9900 108.88 108.88 H25B 0.9900 108.88 108.88 107.72 C25 - C24 C26 H25A C26 - Distance Angles C27 1.5151 (0.0042) C25 1.5269 (0.0045) 115.59 (0.26) H26A 0.9900 108.38 108.38 H26B 0.9900 108.38 108.38 107.45 C26 - C27 C25 H26A C27 - Distance Angles N21 1.5042 (0.0037) C26 1.5151 (0.0042) 115.36 (0.24) H27A 0.9900 108.43 108.43 H27B 0.9900 108.43 108.43 107.48 C27 - N21 C26 H27A N21 - Distance Angles C22 1.4999 (0.0038) C27 1.5042 (0.0037) 117.89 (0.23) H21A 0.9200 107.83 107.83 H21B 0.9200 107.83 107.83 107.16 N21 - C22 C27 H21A Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.70 2.533(3) 173.9 O1A-H1...O6A_$1 0.92 1.84 2.753(3) 174.1 N21-H21A...O6B_$1 0.92 1.82 2.697(3) 158.6 N21-H21B...O6A_$2 FMAP and GRID set by program FMAP 2 2 32 GRID -1.724 -2 -1 1.724 2 1 R1 = 0.0541 for 1536 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.16 at 0.4684 0.1054 0.8573 [ 0.92 A from H24A ] Deepest hole -0.20 at 0.3488 0.2284 0.9020 [ 0.56 A from H4A ] Mean = 0.00, Rms deviation from mean = 0.04 e/A^3, Highest memory used = 2623 / 28899 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.0316 1.6054 -0.1427 1.00000 0.05 0.16 0.92 H24A 1.79 H22A 1.85 C24 2.28 H4A Q2 1 -0.0295 1.2564 -0.1394 1.00000 0.05 0.16 1.14 H21A 1.28 O6B 1.70 H23B 1.93 N21 Q3 1 0.0433 1.5465 0.2160 1.00000 0.05 0.15 1.09 H24B 1.96 H26B 1.98 C24 2.02 H25B Q4 1 -0.0249 1.4966 -0.1389 1.00000 0.05 0.15 0.89 H24A 1.32 C24 1.75 H25B 1.79 C25 Q5 1 0.3373 0.5898 0.1431 1.00000 0.05 0.15 1.67 H3A 1.93 H22B 1.96 O6A 1.99 H5A Q6 1 0.0843 0.8095 -0.1371 1.00000 0.05 0.15 1.07 O1B 1.71 H27B 1.72 C1 1.85 H1 Q7 1 0.3400 0.5403 0.3823 1.00000 0.05 0.15 0.75 H5B 1.25 C5 1.43 H5A 2.10 C4 Q8 1 -0.0186 1.3550 0.2555 1.00000 0.05 0.14 0.70 H22A 1.69 C22 2.05 H24A 2.16 H26B Q9 1 0.4877 0.4820 0.6573 1.00000 0.05 0.14 0.71 O6A 1.36 H21B 1.43 C6 2.04 H5B Q10 1 0.3817 0.5882 0.5848 1.00000 0.05 0.14 0.69 C5 0.85 C6 1.29 H5A 1.45 H5B Shortest distances between peaks (including symmetry equivalents) 1 8 1.16 1 4 1.21 9 10 1.77 7 10 1.87 4 8 1.95 3 4 2.06 5 9 2.17 5 10 2.21 6 8 2.27 5 7 2.36 3 8 2.38 1 3 2.64 7 9 2.64 2 4 2.66 6 9 2.66 1 6 2.75 5 7 2.92 2 3 2.99 Time profile in seconds ----------------------- 0.08: 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 0.02: Analyse other restraints etc. 0.47: 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 0.34: Structure factors and derivatives 0.25: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.08: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 07skc0010cc finished at 15:42:15 Total CPU time: 1.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++