+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008src0926 started at 14:25:20 on 25-Sep-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src0926 in P2(1) CELL 0.71073 10.9342 8.2762 12.6979 90.000 92.780 90.000 ZERR 4.00 0.0002 0.0003 0.0004 0.000 0.002 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N O UNIT 48 56 16 8 V = 1147.73 F(000) = 520.0 Mu = 0.10 mm-1 Cell Wt = 985.09 Rho = 1.425 MERG 4 OMIT -3.00 55.00 OMIT -2 -1 1 OMIT -2 0 2 OMIT 1 -1 0 OMIT 0 1 1 EXTI 0.11177 SHEL 7 0.77 FMAP 2 PLAN 10 SIZE 0.10 0.17 0.44 ACTA BOND $H WGHT 0.06570 L.S. 4 TEMP -153.00 FVAR 0.97197 MOLE 1 C2 1 0.040611 0.446458 0.387279 11.00000 0.02421 0.03360 = 0.02848 -0.00519 0.00164 -0.00133 AFIX 43 H2 2 -0.007962 0.351640 0.390973 11.00000 -1.20000 AFIX 0 C4 1 0.198171 0.605045 0.369324 11.00000 0.03024 0.02825 = 0.02709 -0.00228 0.00612 -0.00701 AFIX 43 H4 2 0.277848 0.645733 0.358585 11.00000 -1.20000 AFIX 0 C5 1 0.096144 0.692359 0.387825 11.00000 0.04194 0.02625 = 0.02932 -0.00219 0.00715 0.00089 AFIX 43 H5 2 0.093633 0.806872 0.392413 11.00000 -1.20000 AFIX 0 C6 1 0.238336 0.307362 0.342428 11.00000 0.01894 0.02782 = 0.02390 -0.00388 -0.00045 0.00107 AFIX 13 H6 2 0.326857 0.331209 0.358922 11.00000 -1.50000 AFIX 0 C7 1 0.216671 0.262415 0.225726 11.00000 0.01642 0.02450 = 0.02164 0.00054 0.00263 0.00073 AFIX 13 H7 2 0.196274 0.359362 0.181267 11.00000 -1.50000 AFIX 0 C9 1 0.290091 0.009008 0.173253 11.00000 0.02642 0.02694 = 0.02734 -0.00716 -0.00228 0.00462 AFIX 23 H9A 2 0.316936 -0.054804 0.236145 11.00000 -1.50000 H9B 2 0.330577 -0.034566 0.111230 11.00000 -1.50000 AFIX 0 C10 1 0.151482 0.002077 0.155843 11.00000 0.02450 0.02202 = 0.02008 -0.00140 0.00059 -0.00030 AFIX 13 H10 2 0.119348 -0.102965 0.181902 11.00000 -1.50000 AFIX 0 C11 1 0.110143 0.141941 0.225094 11.00000 0.02215 0.02316 = 0.01617 0.00256 0.00033 -0.00084 AFIX 13 H11 2 0.032086 0.191511 0.196320 11.00000 -1.50000 AFIX 0 C13 1 0.200515 0.152973 0.396933 11.00000 0.03007 0.03061 = 0.02057 -0.00096 -0.00497 0.00327 AFIX 23 H13A 2 0.269344 0.075200 0.401932 11.00000 -1.50000 H13B 2 0.174239 0.176412 0.468874 11.00000 -1.50000 AFIX 0 C15 1 -0.001309 -0.017392 0.004124 11.00000 0.02456 0.03777 = 0.02801 -0.00401 -0.00131 -0.00718 AFIX 43 H15 2 -0.059093 -0.076448 0.042278 11.00000 -1.20000 AFIX 0 C17 1 0.083739 0.109570 -0.117717 11.00000 0.02822 0.03529 = 0.02191 -0.00360 0.00452 0.00151 AFIX 43 H17 2 0.097270 0.157991 -0.183980 11.00000 -1.20000 AFIX 0 C18 1 0.166110 0.111102 -0.032756 11.00000 0.02375 0.03196 = 0.02473 -0.00255 0.00588 -0.00434 AFIX 43 H18 2 0.245074 0.159241 -0.028838 11.00000 -1.20000 AFIX 0 N1 3 -0.002214 0.593343 0.398922 11.00000 0.03046 0.03672 = 0.03012 -0.00302 0.00426 0.00470 N3 3 0.162319 0.445241 0.369336 11.00000 0.01972 0.02599 = 0.02105 -0.00339 0.00148 -0.00236 N14 3 0.110296 0.028284 0.045521 11.00000 0.02345 0.02449 = 0.01992 -0.00369 -0.00020 -0.00132 N16 3 -0.020799 0.028622 -0.093968 11.00000 0.03092 0.04369 = 0.02615 -0.00376 -0.00108 -0.00339 O8 4 0.319713 0.175985 0.188312 11.00000 0.01889 0.03334 = 0.03233 -0.01042 0.00521 -0.00129 O12 4 0.100493 0.089158 0.332215 11.00000 0.03257 0.02758 = 0.01767 0.00164 0.00213 -0.00855 MOLE 2 C22 1 0.474138 0.734003 0.982936 11.00000 0.02076 0.03537 = 0.02539 -0.00234 0.00574 -0.00144 AFIX 43 H22 2 0.514199 0.778316 0.924810 11.00000 -1.20000 AFIX 0 C24 1 0.331033 0.631844 1.077889 11.00000 0.02554 0.02908 = 0.01866 0.00096 0.00374 -0.00188 AFIX 43 H24 2 0.255311 0.591409 1.100440 11.00000 -1.20000 AFIX 0 C25 1 0.438496 0.640541 1.135536 11.00000 0.03154 0.03239 = 0.02183 0.00195 0.00184 0.00381 AFIX 43 H25 2 0.449973 0.607201 1.206921 11.00000 -1.20000 AFIX 0 C26 1 0.266277 0.693086 0.888801 11.00000 0.01813 0.02952 = 0.01917 -0.00075 -0.00004 0.00446 AFIX 13 H26 2 0.180522 0.703149 0.912033 11.00000 -1.50000 AFIX 0 C27 1 0.280940 0.537933 0.824098 11.00000 0.01847 0.02744 = 0.01868 0.00182 -0.00095 0.00047 AFIX 13 H27 2 0.307653 0.444548 0.869593 11.00000 -1.50000 AFIX 0 C29 1 0.189270 0.533287 0.652146 11.00000 0.02490 0.04981 = 0.01846 -0.00271 -0.00098 0.01135 AFIX 23 H29A 2 0.158833 0.642234 0.632140 11.00000 -1.50000 H29B 2 0.145086 0.452322 0.607293 11.00000 -1.50000 AFIX 0 C30 1 0.326712 0.521677 0.638894 11.00000 0.02589 0.02579 = 0.01959 0.00162 0.00204 0.00712 AFIX 13 H30 2 0.351716 0.594561 0.580923 11.00000 -1.50000 AFIX 0 C31 1 0.377984 0.583454 0.745776 11.00000 0.02064 0.02060 = 0.02050 -0.00039 0.00222 0.00448 AFIX 13 H31 2 0.459131 0.533506 0.765631 11.00000 -1.50000 AFIX 0 C33 1 0.293287 0.824267 0.809811 11.00000 0.03227 0.02738 = 0.02140 -0.00112 0.00453 0.01056 AFIX 23 H33A 2 0.218530 0.852571 0.766638 11.00000 -1.50000 H33B 2 0.324638 0.922679 0.846296 11.00000 -1.50000 AFIX 0 C35 1 0.468600 0.316569 0.568474 11.00000 0.02440 0.02696 = 0.02872 -0.00134 0.00921 -0.00168 AFIX 43 H35 2 0.520583 0.393827 0.538045 11.00000 -1.20000 AFIX 0 C37 1 0.392806 0.094356 0.618977 11.00000 0.03653 0.02778 = 0.01894 0.00120 0.00218 -0.00403 AFIX 43 H37 2 0.380843 -0.017929 0.630117 11.00000 -1.20000 AFIX 0 C38 1 0.319421 0.212896 0.653679 11.00000 0.02790 0.03380 = 0.02400 -0.00133 0.00751 -0.01008 AFIX 43 H38 2 0.248825 0.199312 0.693534 11.00000 -1.20000 AFIX 0 N21 3 0.528878 0.704685 1.075846 11.00000 0.02501 0.04028 = 0.02611 -0.00497 0.00110 0.00079 N23 3 0.353795 0.693328 0.980275 11.00000 0.02154 0.02512 = 0.01801 -0.00108 0.00250 0.00188 N34 3 0.366847 0.356429 0.620088 11.00000 0.02146 0.02615 = 0.01924 -0.00094 0.00410 0.00064 N36 3 0.487462 0.160204 0.565103 11.00000 0.02907 0.02605 = 0.02633 -0.00133 0.00448 0.00019 O28 4 0.171195 0.502301 0.761951 11.00000 0.01830 0.04650 = 0.02137 -0.00464 -0.00016 0.00011 O32 4 0.384989 0.756367 0.744838 11.00000 0.03674 0.02248 = 0.02550 0.00226 0.01130 0.00226 HKLF 4 Covalent radii and connectivity table for 2008src0926 in P2(1) C 0.770 H 0.320 N 0.700 O 0.660 C2 - N1 N3 C4 - C5 N3 C5 - C4 N1 C6 - N3 C13 C7 C7 - O8 C11 C6 C9 - O8 C10 C10 - N14 C9 C11 C11 - O12 C7 C10 C13 - O12 C6 C15 - N16 N14 C17 - N16 C18 C18 - C17 N14 N1 - C2 C5 N3 - C2 C4 C6 N14 - C15 C18 C10 N16 - C15 C17 O8 - C9 C7 O12 - C13 C11 C22 - N21 N23 C24 - C25 N23 C25 - C24 N21 C26 - N23 C33 C27 C27 - O28 C31 C26 C29 - O28 C30 C30 - N34 C29 C31 C31 - O32 C30 C27 C33 - O32 C26 C35 - N36 N34 C37 - C38 N36 C38 - C37 N34 N21 - C22 C25 N23 - C22 C24 C26 N34 - C35 C38 C30 N36 - C35 C37 O28 - C27 C29 O32 - C31 C33 Floating origin restraints generated 15536 Reflections read, of which 27 rejected -13 =< h =< 14, -10 =< k =< 10, -16 =< l =< 16, Max. 2-theta = 54.95 0 Systematic absence violations 0 Inconsistent equivalents 2805 Unique reflections, of which 0 suppressed R(int) = 0.0539 R(sigma) = 0.0417 Friedel opposites merged Maximum memory for data reduction = 3187 / 27618 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 = 4101 / 410120 wR2 = 0.1084 before cycle 1 for 2805 data and 326 / 326 parameters GooF = S = 1.165; Restrained GooF = 1.165 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0657 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.97182 0.00287 -0.052 OSF 2 0.11132 0.00848 -0.053 EXTI Mean shift/su = 0.009 Maximum = -0.053 for EXTI Max. shift = 0.000 A for C5 Max. dU = 0.000 for C10 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4101 / 410120 wR2 = 0.1084 before cycle 2 for 2805 data and 326 / 326 parameters GooF = S = 1.165; Restrained GooF = 1.165 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0657 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.97178 0.00287 -0.013 OSF 2 0.11118 0.00845 -0.016 EXTI Mean shift/su = 0.003 Maximum = -0.016 for EXTI Max. shift = 0.000 A for C5 Max. dU = 0.000 for C10 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4101 / 410120 wR2 = 0.1083 before cycle 3 for 2805 data and 326 / 326 parameters GooF = S = 1.165; Restrained GooF = 1.165 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0657 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.97178 0.00287 0.001 OSF 2 0.11118 0.00845 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.001 for U12 C18 Max. shift = 0.000 A for N14 Max. dU = 0.000 for C22 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4101 / 410120 wR2 = 0.1083 before cycle 4 for 2805 data and 326 / 326 parameters GooF = S = 1.165; Restrained GooF = 1.165 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0657 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.97179 0.00287 0.000 OSF 2 0.11119 0.00845 0.001 EXTI Mean shift/su = 0.000 Maximum = 0.001 for EXTI Max. shift = 0.000 A for C5 Max. dU = 0.000 for C5 Largest correlation matrix elements 0.557 EXTI / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 -0.0080 0.3516 0.3910 43 0.950 0.000 C2 N1 N3 H4 0.2779 0.6457 0.3586 43 0.950 0.000 C4 C5 N3 H5 0.0936 0.8069 0.3924 43 0.950 0.000 C5 C4 N1 H6 0.3269 0.3312 0.3589 13 1.000 0.000 C6 N3 C13 C7 H7 0.1963 0.3594 0.1813 13 1.000 0.000 C7 O8 C11 C6 H9A 0.3169 -0.0548 0.2362 23 0.990 0.000 C9 O8 C10 H9B 0.3306 -0.0346 0.1112 23 0.990 0.000 C9 O8 C10 H10 0.1193 -0.1030 0.1819 13 1.000 0.000 C10 N14 C9 C11 H11 0.0321 0.1915 0.1963 13 1.000 0.000 C11 O12 C7 C10 H13A 0.2693 0.0752 0.4019 23 0.990 0.000 C13 O12 C6 H13B 0.1742 0.1764 0.4689 23 0.990 0.000 C13 O12 C6 H15 -0.0591 -0.0764 0.0423 43 0.950 0.000 C15 N16 N14 H17 0.0973 0.1580 -0.1840 43 0.950 0.000 C17 N16 C18 H18 0.2451 0.1592 -0.0288 43 0.950 0.000 C18 C17 N14 H22 0.5142 0.7783 0.9248 43 0.950 0.000 C22 N21 N23 H24 0.2553 0.5914 1.1004 43 0.950 0.000 C24 C25 N23 H25 0.4500 0.6072 1.2069 43 0.950 0.000 C25 C24 N21 H26 0.1805 0.7032 0.9120 13 1.000 0.000 C26 N23 C33 C27 H27 0.3076 0.4445 0.8696 13 1.000 0.000 C27 O28 C31 C26 H29A 0.1588 0.6422 0.6321 23 0.990 0.000 C29 O28 C30 H29B 0.1451 0.4523 0.6073 23 0.990 0.000 C29 O28 C30 H30 0.3517 0.5946 0.5809 13 1.000 0.000 C30 N34 C29 C31 H31 0.4591 0.5335 0.7656 13 1.000 0.000 C31 O32 C30 C27 H33A 0.2185 0.8526 0.7666 23 0.990 0.000 C33 O32 C26 H33B 0.3246 0.9227 0.8463 23 0.990 0.000 C33 O32 C26 H35 0.5206 0.3938 0.5380 43 0.950 0.000 C35 N36 N34 H37 0.3808 -0.0179 0.6301 43 0.950 0.000 C37 C38 N36 H38 0.2488 0.1993 0.6935 43 0.950 0.000 C38 C37 N34 2008src0926 in P2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C2 0.04061 0.44646 0.38728 1.00000 0.02424 0.03359 0.02848 -0.00518 0.00163 -0.00131 0.02876 0.00493 0.00024 0.00037 0.00022 0.00000 0.00126 0.00158 0.00153 0.00119 0.00100 0.00113 0.00061 H2 -0.00797 0.35164 0.39096 1.00000 0.03451 0.00000 0.00000 C4 0.19818 0.60505 0.36933 1.00000 0.03024 0.02825 0.02709 -0.00229 0.00612 -0.00701 0.02838 0.00484 0.00024 0.00035 0.00021 0.00000 0.00129 0.00149 0.00142 0.00115 0.00100 0.00110 0.00059 H4 0.27786 0.64574 0.35859 1.00000 0.03405 0.00000 0.00000 C5 0.09615 0.69237 0.38782 1.00000 0.04193 0.02623 0.02934 -0.00221 0.00714 0.00090 0.03232 0.00512 0.00025 0.00039 0.00021 0.00000 0.00151 0.00148 0.00152 0.00118 0.00114 0.00114 0.00064 H5 0.09363 0.80689 0.39240 1.00000 0.03879 0.00000 0.00000 C6 0.23834 0.30737 0.34243 1.00000 0.01891 0.02781 0.02390 -0.00389 -0.00045 0.00107 0.02359 0.00445 0.00021 0.00033 0.00020 0.00000 0.00110 0.00143 0.00134 0.00106 0.00092 0.00100 0.00056 H6 0.32686 0.33121 0.35892 1.00000 0.03538 0.00000 0.00000 C7 0.21667 0.26241 0.22572 1.00000 0.01641 0.02448 0.02164 0.00056 0.00263 0.00073 0.02079 0.00438 0.00020 0.00033 0.00019 0.00000 0.00103 0.00130 0.00123 0.00104 0.00085 0.00096 0.00051 H7 0.19627 0.35936 0.18126 1.00000 0.03119 0.00000 0.00000 C9 0.29010 0.00901 0.17326 1.00000 0.02636 0.02698 0.02735 -0.00716 -0.00226 0.00461 0.02701 0.00456 0.00023 0.00034 0.00022 0.00000 0.00126 0.00143 0.00140 0.00114 0.00101 0.00108 0.00058 H9A 0.31694 -0.05480 0.23615 1.00000 0.04052 0.00000 0.00000 H9B 0.33059 -0.03457 0.11124 1.00000 0.04052 0.00000 0.00000 C10 0.15148 0.00207 0.15584 1.00000 0.02444 0.02199 0.02009 -0.00142 0.00061 -0.00032 0.02219 0.00436 0.00021 0.00032 0.00019 0.00000 0.00119 0.00131 0.00122 0.00100 0.00092 0.00099 0.00052 H10 0.11934 -0.10297 0.18190 1.00000 0.03328 0.00000 0.00000 C11 0.11014 0.14194 0.22509 1.00000 0.02213 0.02312 0.01618 0.00255 0.00031 -0.00085 0.02050 0.00421 0.00020 0.00032 0.00018 0.00000 0.00107 0.00130 0.00116 0.00096 0.00085 0.00100 0.00051 H11 0.03208 0.19151 0.19632 1.00000 0.03075 0.00000 0.00000 C13 0.20051 0.15297 0.39694 1.00000 0.03006 0.03059 0.02057 -0.00098 -0.00497 0.00327 0.02728 0.00452 0.00023 0.00034 0.00020 0.00000 0.00123 0.00151 0.00129 0.00111 0.00096 0.00115 0.00058 H13A 0.26934 0.07520 0.40194 1.00000 0.04091 0.00000 0.00000 H13B 0.17424 0.17641 0.46888 1.00000 0.04091 0.00000 0.00000 C15 -0.00131 -0.01739 0.00413 1.00000 0.02456 0.03777 0.02802 -0.00404 -0.00132 -0.00718 0.03020 0.00504 0.00026 0.00037 0.00025 0.00000 0.00114 0.00169 0.00138 0.00120 0.00094 0.00111 0.00061 H15 -0.05909 -0.07645 0.04228 1.00000 0.03624 0.00000 0.00000 C17 0.08374 0.10958 -0.11773 1.00000 0.02819 0.03527 0.02193 -0.00359 0.00452 0.00152 0.02835 0.00478 0.00022 0.00038 0.00020 0.00000 0.00125 0.00158 0.00135 0.00115 0.00096 0.00113 0.00060 H17 0.09727 0.15800 -0.18399 1.00000 0.03403 0.00000 0.00000 C18 0.16611 0.11111 -0.03275 1.00000 0.02375 0.03194 0.02473 -0.00254 0.00588 -0.00434 0.02665 0.00468 0.00022 0.00034 0.00020 0.00000 0.00118 0.00152 0.00134 0.00117 0.00095 0.00109 0.00058 H18 0.24508 0.15924 -0.02883 1.00000 0.03198 0.00000 0.00000 N1 -0.00221 0.59334 0.39892 1.00000 0.03044 0.03673 0.03015 -0.00301 0.00426 0.00468 0.03235 0.00425 0.00020 0.00031 0.00018 0.00000 0.00117 0.00143 0.00129 0.00111 0.00090 0.00103 0.00055 N3 0.16232 0.44524 0.36934 1.00000 0.01971 0.02597 0.02104 -0.00340 0.00148 -0.00236 0.02222 0.00369 0.00018 0.00027 0.00017 0.00000 0.00098 0.00119 0.00114 0.00090 0.00076 0.00085 0.00047 N14 0.11030 0.02829 0.04552 1.00000 0.02346 0.02450 0.01992 -0.00369 -0.00021 -0.00132 0.02267 0.00360 0.00018 0.00027 0.00016 0.00000 0.00101 0.00115 0.00106 0.00092 0.00078 0.00087 0.00046 N16 -0.02080 0.02862 -0.09396 1.00000 0.03090 0.04366 0.02619 -0.00374 -0.00105 -0.00337 0.03367 0.00420 0.00021 0.00034 0.00018 0.00000 0.00117 0.00152 0.00124 0.00116 0.00091 0.00108 0.00056 O8 0.31971 0.17598 0.18831 1.00000 0.01889 0.03334 0.03231 -0.01042 0.00521 -0.00128 0.02805 0.00314 0.00015 0.00024 0.00015 0.00000 0.00078 0.00111 0.00102 0.00085 0.00066 0.00075 0.00044 O12 0.10049 0.08916 0.33222 1.00000 0.03255 0.02756 0.01766 0.00162 0.00213 -0.00857 0.02589 0.00305 0.00016 0.00022 0.00013 0.00000 0.00096 0.00104 0.00091 0.00079 0.00069 0.00078 0.00043 C22 0.47414 0.73401 0.98294 1.00000 0.02075 0.03537 0.02537 -0.00236 0.00576 -0.00142 0.02702 0.00447 0.00021 0.00035 0.00020 0.00000 0.00119 0.00160 0.00137 0.00117 0.00096 0.00112 0.00059 H22 0.51420 0.77833 0.92481 1.00000 0.03242 0.00000 0.00000 C24 0.33103 0.63184 1.07789 1.00000 0.02551 0.02912 0.01865 0.00095 0.00374 -0.00189 0.02434 0.00456 0.00022 0.00034 0.00019 0.00000 0.00114 0.00140 0.00126 0.00107 0.00090 0.00107 0.00054 H24 0.25531 0.59140 1.10044 1.00000 0.02921 0.00000 0.00000 C25 0.43850 0.64054 1.13554 1.00000 0.03153 0.03238 0.02182 0.00196 0.00183 0.00381 0.02856 0.00498 0.00023 0.00036 0.00021 0.00000 0.00127 0.00154 0.00130 0.00112 0.00096 0.00118 0.00058 H25 0.44998 0.60720 1.20693 1.00000 0.03427 0.00000 0.00000 C26 0.26628 0.69309 0.88880 1.00000 0.01814 0.02947 0.01915 -0.00074 -0.00006 0.00446 0.02229 0.00430 0.00020 0.00032 0.00019 0.00000 0.00104 0.00142 0.00122 0.00105 0.00084 0.00099 0.00054 H26 0.18053 0.70316 0.91204 1.00000 0.03343 0.00000 0.00000 C27 0.28094 0.53793 0.82410 1.00000 0.01847 0.02744 0.01867 0.00181 -0.00095 0.00048 0.02159 0.00430 0.00021 0.00033 0.00019 0.00000 0.00115 0.00141 0.00122 0.00105 0.00090 0.00097 0.00053 H27 0.30765 0.44454 0.86959 1.00000 0.03238 0.00000 0.00000 C29 0.18926 0.53328 0.65214 1.00000 0.02485 0.04980 0.01848 -0.00270 -0.00098 0.01135 0.03111 0.00528 0.00023 0.00041 0.00020 0.00000 0.00127 0.00189 0.00126 0.00128 0.00095 0.00120 0.00065 H29A 0.15882 0.64222 0.63214 1.00000 0.04667 0.00000 0.00000 H29B 0.14508 0.45231 0.60729 1.00000 0.04667 0.00000 0.00000 C30 0.32671 0.52167 0.63889 1.00000 0.02587 0.02579 0.01960 0.00161 0.00204 0.00712 0.02372 0.00466 0.00022 0.00034 0.00019 0.00000 0.00124 0.00135 0.00123 0.00108 0.00093 0.00104 0.00054 H30 0.35172 0.59456 0.58092 1.00000 0.03558 0.00000 0.00000 C31 0.37798 0.58345 0.74578 1.00000 0.02062 0.02060 0.02046 -0.00040 0.00222 0.00449 0.02052 0.00437 0.00021 0.00031 0.00019 0.00000 0.00115 0.00125 0.00123 0.00100 0.00088 0.00095 0.00051 H31 0.45913 0.53350 0.76564 1.00000 0.03078 0.00000 0.00000 C33 0.29329 0.82427 0.80981 1.00000 0.03225 0.02733 0.02139 -0.00111 0.00455 0.01055 0.02689 0.00510 0.00024 0.00035 0.00021 0.00000 0.00134 0.00146 0.00133 0.00110 0.00103 0.00114 0.00059 H33A 0.21853 0.85257 0.76664 1.00000 0.04033 0.00000 0.00000 H33B 0.32464 0.92268 0.84629 1.00000 0.04033 0.00000 0.00000 C35 0.46860 0.31657 0.56847 1.00000 0.02438 0.02694 0.02873 -0.00135 0.00920 -0.00170 0.02643 0.00479 0.00023 0.00033 0.00022 0.00000 0.00118 0.00142 0.00145 0.00114 0.00101 0.00107 0.00058 H35 0.52059 0.39382 0.53804 1.00000 0.03171 0.00000 0.00000 C37 0.39281 0.09435 0.61898 1.00000 0.03652 0.02778 0.01893 0.00122 0.00221 -0.00403 0.02772 0.00474 0.00024 0.00037 0.00019 0.00000 0.00144 0.00151 0.00132 0.00108 0.00102 0.00110 0.00059 H37 0.38084 -0.01793 0.63012 1.00000 0.03326 0.00000 0.00000 C38 0.31942 0.21290 0.65368 1.00000 0.02787 0.03379 0.02401 -0.00135 0.00752 -0.01008 0.02835 0.00470 0.00023 0.00036 0.00020 0.00000 0.00124 0.00158 0.00132 0.00115 0.00098 0.00113 0.00060 H38 0.24883 0.19931 0.69353 1.00000 0.03402 0.00000 0.00000 N21 0.52888 0.70468 1.07585 1.00000 0.02499 0.04029 0.02612 -0.00497 0.00111 0.00080 0.03047 0.00405 0.00019 0.00032 0.00017 0.00000 0.00104 0.00147 0.00118 0.00105 0.00084 0.00096 0.00054 N23 0.35379 0.69333 0.98027 1.00000 0.02156 0.02511 0.01798 -0.00109 0.00248 0.00186 0.02150 0.00363 0.00018 0.00027 0.00015 0.00000 0.00093 0.00115 0.00102 0.00088 0.00074 0.00083 0.00046 N34 0.36684 0.35644 0.62009 1.00000 0.02143 0.02616 0.01924 -0.00095 0.00412 0.00066 0.02217 0.00377 0.00018 0.00027 0.00016 0.00000 0.00097 0.00121 0.00113 0.00089 0.00079 0.00089 0.00047 N36 0.48746 0.16020 0.56510 1.00000 0.02906 0.02604 0.02631 -0.00133 0.00447 0.00021 0.02703 0.00396 0.00019 0.00029 0.00017 0.00000 0.00104 0.00122 0.00119 0.00097 0.00085 0.00095 0.00050 O28 0.17120 0.50230 0.76195 1.00000 0.01829 0.04648 0.02137 -0.00465 -0.00016 0.00011 0.02875 0.00312 0.00015 0.00026 0.00013 0.00000 0.00082 0.00123 0.00097 0.00086 0.00066 0.00080 0.00045 O32 0.38499 0.75637 0.74484 1.00000 0.03673 0.02247 0.02551 0.00227 0.01131 0.00226 0.02792 0.00354 0.00017 0.00024 0.00014 0.00000 0.00100 0.00093 0.00095 0.00079 0.00074 0.00079 0.00043 Final Structure Factor Calculation for 2008src0926 in P2(1) Total number of l.s. parameters = 326 Maximum vector length = 511 Memory required = 3777 / 25046 wR2 = 0.1083 before cycle 5 for 2805 data and 2 / 326 parameters GooF = S = 1.165; Restrained GooF = 1.165 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0657 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0454 for 2424 Fo > 4sig(Fo) and 0.0560 for all 2805 data wR2 = 0.1083, GooF = S = 1.165, Restrained GooF = 1.165 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 36.00 for non-hydrogen and 28.00 for hydrogen atoms Principal mean square atomic displacements U 0.0369 0.0254 0.0240 C2 0.0383 0.0253 0.0215 C4 0.0437 0.0291 0.0242 C5 0.0305 0.0217 0.0186 C6 0.0247 0.0219 0.0158 C7 0.0377 0.0236 0.0198 C9 0.0245 0.0227 0.0193 C10 0.0245 0.0217 0.0153 C11 0.0357 0.0283 0.0178 C13 0.0414 0.0295 0.0197 C15 0.0363 0.0295 0.0193 C17 0.0354 0.0255 0.0190 C18 0.0395 0.0328 0.0247 N1 0.0283 0.0198 0.0186 N3 0.0266 0.0239 0.0175 N14 0.0450 0.0319 0.0241 N16 0.0436 0.0232 0.0173 O8 0.0390 0.0220 0.0167 O12 0.0363 0.0271 0.0176 C22 0.0299 0.0257 0.0174 C24 0.0360 0.0283 0.0215 C25 0.0311 0.0192 0.0165 C26 0.0278 0.0204 0.0166 C27 0.0546 0.0208 0.0180 C29 0.0331 0.0195 0.0186 C30 0.0251 0.0207 0.0158 C31 0.0407 0.0233 0.0167 C33 0.0349 0.0264 0.0179 C35 0.0381 0.0265 0.0186 C37 0.0424 0.0258 0.0169 C38 0.0419 0.0250 0.0245 N21 0.0259 0.0216 0.0170 N23 0.0263 0.0235 0.0167 N34 0.0310 0.0266 0.0235 N36 0.0473 0.0210 0.0179 O28 0.0424 0.0222 0.0191 O32 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 0.038 0.048 0.057 0.069 0.086 0.108 0.150 1.000 Number in group 301. 289. 280. 276. 260. 280. 289. 267. 280. 283. GooF 0.956 1.143 1.123 1.149 1.174 1.152 1.006 0.906 0.863 1.867 K 1.054 0.927 1.010 1.010 1.010 1.003 1.015 1.007 0.999 1.054 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.98 1.05 1.16 1.33 1.67 inf Number in group 290. 274. 281. 279. 278. 280. 280. 280. 281. 282. GooF 0.972 1.032 1.088 1.139 1.099 0.940 0.961 0.998 1.043 1.994 K 1.066 1.032 1.025 1.021 1.000 1.009 1.009 1.006 1.023 1.057 R1 0.115 0.134 0.095 0.069 0.049 0.034 0.030 0.028 0.027 0.064 Recommended weighting scheme: WGHT 0.0661 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)/su Fc/Fc(max) Resolution(A) -2 1 1 642.63 16669.63 19.05 1.000 4.35 0 1 3 18829.40 10976.15 7.28 0.811 3.76 1 2 0 12090.21 8110.47 5.56 0.698 3.87 1 1 0 465.43 962.75 5.52 0.240 6.60 0 0 5 9814.82 7069.78 4.24 0.651 2.54 -2 0 1 9670.93 7052.02 3.84 0.650 5.11 7 4 9 25.23 39.53 3.66 0.049 0.92 2 1 4 8060.39 6179.34 3.62 0.609 2.55 -4 0 4 5.46 9.74 3.37 0.024 2.12 -2 2 7 66.46 51.27 3.37 0.055 1.61 1 1 3 5676.46 4453.98 3.33 0.517 3.51 0 0 4 7322.02 5702.16 3.26 0.585 3.17 2 0 1 8411.33 6262.21 3.15 0.613 4.93 2 1 10 44.63 60.93 3.10 0.060 1.21 2 0 6 6826.75 5391.02 3.03 0.569 1.94 -6 5 10 35.52 49.22 2.99 0.054 0.90 -11 0 2 44.98 64.03 2.85 0.062 0.99 -6 4 11 31.38 43.29 2.80 0.051 0.90 5 8 6 54.76 33.09 2.79 0.045 0.85 -7 8 2 1.75 10.27 2.78 0.025 0.86 11 2 4 8.69 13.94 2.77 0.029 0.91 11 3 2 31.50 40.83 2.75 0.049 0.92 4 1 8 65.37 51.71 2.71 0.056 1.33 2 1 6 78.46 63.17 2.70 0.062 1.89 0 7 12 142.28 99.37 2.69 0.077 0.79 -9 0 4 13.49 2.59 2.67 0.012 1.15 -11 0 9 2.65 7.04 2.67 0.021 0.83 -9 2 4 68.66 86.17 2.61 0.072 1.11 3 9 3 6.28 1.86 2.58 0.011 0.87 2 0 0 595.60 740.94 2.57 0.211 5.46 5 8 7 32.72 17.02 2.57 0.032 0.82 10 1 11 -18.48 26.90 2.52 0.040 0.77 9 0 9 36.83 57.06 2.50 0.059 0.90 -2 0 7 461.37 383.79 2.49 0.152 1.75 -1 1 2 117.46 141.83 2.47 0.092 4.64 0 3 13 5.08 15.89 2.47 0.031 0.92 8 4 4 8.14 4.18 2.47 0.016 1.06 3 0 0 22.29 27.38 2.43 0.041 3.64 9 0 8 17.16 28.42 2.43 0.041 0.94 6 3 12 5.15 11.97 2.43 0.027 0.85 4 1 13 144.64 109.44 2.42 0.081 0.90 -4 2 6 66.12 54.62 2.40 0.057 1.58 6 0 13 72.07 42.23 2.38 0.050 0.84 8 6 5 51.08 39.73 2.36 0.049 0.90 1 8 1 21.15 28.59 2.35 0.041 1.03 -4 5 1 23.64 18.81 2.35 0.034 1.41 -7 5 12 49.90 34.13 2.34 0.045 0.79 -6 1 14 19.94 34.79 2.33 0.046 0.82 8 2 0 29.54 36.37 2.32 0.047 1.30 7 4 5 3.07 0.47 2.32 0.005 1.10 Bond lengths and angles C2 - Distance Angles N1 1.3136 (0.0039) N3 1.3611 (0.0033) 112.48 (0.25) H2 0.9500 123.76 123.76 C2 - N1 N3 C4 - Distance Angles C5 1.3592 (0.0039) N3 1.3795 (0.0035) 105.91 (0.23) H4 0.9500 127.05 127.05 C4 - C5 N3 C5 - Distance Angles C4 1.3592 (0.0039) N1 1.3649 (0.0037) 110.85 (0.27) H5 0.9500 124.57 124.57 C5 - C4 N1 C6 - Distance Angles N3 1.4619 (0.0033) C13 1.5201 (0.0038) 112.29 (0.20) C7 1.5351 (0.0035) 110.60 (0.21) 101.72 (0.21) H6 1.0000 110.64 110.64 110.64 C6 - N3 C13 C7 C7 - Distance Angles O8 1.4348 (0.0029) C11 1.5330 (0.0033) 106.42 (0.21) C6 1.5351 (0.0035) 110.70 (0.19) 104.14 (0.19) H7 1.0000 111.73 111.73 111.73 C7 - O8 C11 C6 C9 - Distance Angles O8 1.4300 (0.0035) C10 1.5222 (0.0034) 105.86 (0.20) H9A 0.9900 110.56 110.56 H9B 0.9900 110.56 110.56 108.72 C9 - O8 C10 H9A C10 - Distance Angles N14 1.4666 (0.0032) C9 1.5222 (0.0034) 112.99 (0.20) C11 1.5350 (0.0034) 110.50 (0.20) 101.95 (0.20) H10 1.0000 110.37 110.37 110.37 C10 - N14 C9 C11 C11 - Distance Angles O12 1.4374 (0.0028) C7 1.5330 (0.0033) 106.46 (0.19) C10 1.5350 (0.0034) 110.49 (0.21) 104.40 (0.19) H11 1.0000 111.71 111.71 111.71 C11 - O12 C7 C10 C13 - Distance Angles O12 1.4364 (0.0030) C6 1.5201 (0.0038) 105.37 (0.20) H13A 0.9900 110.67 110.67 H13B 0.9900 110.67 110.67 108.78 C13 - O12 C6 H13A C15 - Distance Angles N16 1.3099 (0.0040) N14 1.3588 (0.0035) 112.87 (0.25) H15 0.9500 123.57 123.57 C15 - N16 N14 C17 - Distance Angles N16 1.3711 (0.0035) C18 1.3716 (0.0037) 110.73 (0.24) H17 0.9500 124.63 124.63 C17 - N16 C18 C18 - Distance Angles C17 1.3716 (0.0037) N14 1.3744 (0.0032) 105.46 (0.22) H18 0.9500 127.27 127.27 C18 - C17 N14 N1 - Distance Angles C2 1.3136 (0.0039) C5 1.3649 (0.0038) 104.90 (0.23) N1 - C2 N3 - Distance Angles C2 1.3611 (0.0033) C4 1.3795 (0.0035) 105.85 (0.22) C6 1.4619 (0.0033) 128.06 (0.23) 125.70 (0.21) N3 - C2 C4 N14 - Distance Angles C15 1.3588 (0.0035) C18 1.3744 (0.0032) 106.32 (0.22) C10 1.4666 (0.0032) 123.83 (0.22) 129.64 (0.21) N14 - C15 C18 N16 - Distance Angles C15 1.3099 (0.0040) C17 1.3711 (0.0035) 104.62 (0.23) N16 - C15 O8 - Distance Angles C9 1.4300 (0.0035) C7 1.4348 (0.0029) 110.47 (0.19) O8 - C9 O12 - Distance Angles C13 1.4364 (0.0030) C11 1.4374 (0.0028) 109.93 (0.18) O12 - C13 C22 - Distance Angles N21 1.3193 (0.0035) N23 1.3571 (0.0032) 111.96 (0.23) H22 0.9500 124.02 124.02 C22 - N21 N23 C24 - Distance Angles C25 1.3559 (0.0036) N23 1.3738 (0.0032) 106.10 (0.22) H24 0.9500 126.95 126.95 C24 - C25 N23 C25 - Distance Angles C24 1.3559 (0.0036) N21 1.3804 (0.0034) 110.41 (0.24) H25 0.9500 124.80 124.80 C25 - C24 N21 C26 - Distance Angles N23 1.4686 (0.0030) C33 1.5168 (0.0037) 112.44 (0.21) C27 1.5371 (0.0036) 110.06 (0.19) 102.46 (0.19) H26 1.0000 110.54 110.54 110.54 C26 - N23 C33 C27 C27 - Distance Angles O28 1.4345 (0.0029) C31 1.5360 (0.0032) 106.26 (0.19) C26 1.5371 (0.0036) 111.08 (0.19) 103.55 (0.21) H27 1.0000 111.84 111.84 111.84 C27 - O28 C31 C26 C29 - Distance Angles O28 1.4407 (0.0030) C30 1.5234 (0.0034) 106.14 (0.20) H29A 0.9900 110.50 110.50 H29B 0.9900 110.50 110.50 108.68 C29 - O28 C30 H29A C30 - Distance Angles N34 1.4594 (0.0034) C29 1.5234 (0.0034) 112.53 (0.24) C31 1.5310 (0.0036) 110.97 (0.20) 101.64 (0.19) H30 1.0000 110.47 110.47 110.47 C30 - N34 C29 C31 C31 - Distance Angles O32 1.4333 (0.0032) C30 1.5310 (0.0036) 110.09 (0.21) C27 1.5360 (0.0032) 106.81 (0.20) 104.91 (0.20) H31 1.0000 111.58 111.58 111.58 C31 - O32 C30 C27 C33 - Distance Angles O32 1.4430 (0.0030) C26 1.5168 (0.0037) 105.21 (0.20) H33A 0.9900 110.70 110.70 H33B 0.9900 110.70 110.70 108.80 C33 - O32 C26 H33A C35 - Distance Angles N36 1.3115 (0.0036) N34 1.3591 (0.0031) 112.89 (0.23) H35 0.9500 123.55 123.55 C35 - N36 N34 C37 - Distance Angles C38 1.3545 (0.0040) N36 1.3802 (0.0033) 110.22 (0.25) H37 0.9500 124.89 124.89 C37 - C38 N36 C38 - Distance Angles C37 1.3545 (0.0040) N34 1.3724 (0.0035) 106.69 (0.21) H38 0.9500 126.66 126.66 C38 - C37 N34 N21 - Distance Angles C22 1.3193 (0.0035) C25 1.3804 (0.0034) 104.83 (0.21) N21 - C22 N23 - Distance Angles C22 1.3571 (0.0032) C24 1.3738 (0.0032) 106.69 (0.21) C26 1.4686 (0.0030) 127.87 (0.21) 124.99 (0.21) N23 - C22 C24 N34 - Distance Angles C35 1.3591 (0.0031) C38 1.3724 (0.0035) 105.68 (0.22) C30 1.4594 (0.0034) 124.48 (0.22) 129.73 (0.20) N34 - C35 C38 N36 - Distance Angles C35 1.3115 (0.0036) C37 1.3802 (0.0033) 104.51 (0.23) N36 - C35 O28 - Distance Angles C27 1.4345 (0.0029) C29 1.4407 (0.0030) 110.21 (0.19) O28 - C27 O32 - Distance Angles C31 1.4333 (0.0032) C33 1.4430 (0.0030) 110.19 (0.20) O32 - C31 FMAP and GRID set by program FMAP 2 2 21 GRID -2.778 -2 -2 2.778 2 2 R1 = 0.0560 for 2805 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.61 at 0.0156 0.1173 0.2195 [ 0.71 A from H11 ] Deepest hole -0.60 at 0.6683 0.0882 0.0967 [ 1.13 A from C26 ] Mean = 0.00, Rms deviation from mean = 0.20 e/A^3, Highest memory used = 3688 / 24201 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0156 0.1173 0.2195 1.00000 0.05 0.61 0.71 H11 1.05 C11 1.68 O12 1.97 C10 Q2 1 0.4770 0.6831 0.7486 1.00000 0.05 0.56 1.17 O32 1.27 H31 1.36 C31 2.33 O8 Q3 1 0.3640 0.6615 0.4376 1.00000 0.05 0.56 1.35 H4 1.63 N36 1.91 H30 2.03 C4 Q4 1 0.0210 0.1353 0.2805 1.00000 0.05 0.55 1.13 O12 1.18 H11 1.23 C11 2.30 H29A Q5 1 0.3210 0.1615 -0.0952 1.00000 0.05 0.55 1.21 H18 1.69 N21 1.95 C18 2.11 H33B Q6 1 0.1433 0.6668 1.0784 1.00000 0.05 0.54 1.39 H24 1.78 N16 2.07 C24 2.19 H26 Q7 1 0.6243 0.6101 1.0589 1.00000 0.05 0.53 1.33 N21 1.55 H18 2.02 H33B 2.13 C22 Q8 1 0.2843 0.6020 0.3681 1.00000 0.05 0.53 0.39 H4 0.94 C4 1.86 N3 2.21 C5 Q9 1 0.4673 0.5882 0.7501 1.00000 0.05 0.53 0.50 H31 0.98 C31 1.66 O32 2.11 C30 Q10 1 0.1422 0.5571 1.0532 1.00000 0.05 0.53 1.38 H24 1.47 N16 1.78 C15 1.85 H15 Shortest distances between peaks (including symmetry equivalents) 1 4 0.79 2 9 0.79 5 7 0.85 6 10 0.96 3 8 1.31 Time profile in seconds ----------------------- 0.03: 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. 0.73: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.97: Structure factors and derivatives 1.86: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.34: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.08: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008src0926 finished at 14:25:24 Total CPU time: 4.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++