+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src1319 started at 16:14:14 on 02-Feb-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src1319 in P-1 CELL 0.71073 10.1895 11.4764 17.7626 102.487 96.931 101.360 ZERR 4.00 0.0010 0.0016 0.0026 0.005 0.008 0.008 LATT 1 SFAC C H N O UNIT 108 84 4 4 V = 1959.14 F(000) = 792.0 Mu = 0.08 mm-1 Cell Wt = 1501.79 Rho = 1.273 MERG 2 OMIT -3.00 50.00 SHEL 7 0.84 OMIT 2 1 0 FMAP 2 PLAN 20 SIZE 0.05 0.07 0.41 TEMP -153 ACTA BOND $H WGHT 0.10170 0.92090 L.S. 10 FVAR 0.19270 MOLE 1 O1 4 1.253023 -0.351377 0.611639 11.00000 0.08161 0.07697 = 0.05142 0.03122 0.01205 0.02489 N1 3 0.903332 0.297079 0.139584 11.00000 0.05767 0.03926 = 0.04342 0.01634 0.01327 0.02162 C1 1 0.860020 0.407959 0.158052 11.00000 0.04213 0.03355 = 0.03535 0.00872 0.00451 0.01063 C2 1 0.793915 0.434812 0.220870 11.00000 0.04166 0.03420 = 0.05090 0.00828 0.00104 0.00756 AFIX 43 H2 2 0.780005 0.380440 0.252650 11.00000 -1.20000 AFIX 0 C3 1 0.747913 0.542614 0.237027 11.00000 0.05327 0.05180 = 0.04579 0.00651 -0.00591 0.01739 AFIX 43 H3 2 0.706436 0.561486 0.280521 11.00000 -1.20000 AFIX 0 C4 1 0.764013 0.621375 0.188353 11.00000 0.07170 0.04992 = 0.05908 0.00571 -0.00745 0.02824 AFIX 43 H4 2 0.729760 0.691550 0.197718 11.00000 -1.20000 AFIX 0 C5 1 0.830344 0.596278 0.126322 11.00000 0.06538 0.03819 = 0.05848 0.02138 -0.01046 0.00891 AFIX 43 H5 2 0.843889 0.651106 0.094814 11.00000 -1.20000 AFIX 0 C6 1 0.877720 0.489187 0.110036 11.00000 0.05635 0.04519 = 0.04860 0.01707 -0.00071 0.01263 AFIX 43 H6 2 0.921111 0.471900 0.067177 11.00000 -1.20000 AFIX 0 C7 1 0.904208 0.237985 0.060351 11.00000 0.05109 0.03539 = 0.04295 0.01730 0.00971 0.01382 C8 1 0.791619 0.218606 0.002066 11.00000 0.05508 0.04443 = 0.04819 0.02318 0.01320 0.01580 AFIX 43 H8 2 0.714813 0.245435 0.014680 11.00000 -1.20000 AFIX 0 C9 1 0.793687 0.159513 -0.074609 11.00000 0.05474 0.05036 = 0.03680 0.01437 0.00595 0.01649 AFIX 43 H9 2 0.719200 0.148023 -0.113481 11.00000 -1.20000 AFIX 0 C10 1 0.906203 0.118234 -0.092627 11.00000 0.05877 0.04139 = 0.03786 0.01470 0.01679 0.01710 AFIX 43 H10 2 0.907280 0.077505 -0.143779 11.00000 -1.20000 AFIX 0 C11 1 1.016283 0.136347 -0.036320 11.00000 0.04753 0.04365 = 0.04452 0.01614 0.01453 0.01426 AFIX 43 H11 2 1.092054 0.107916 -0.049247 11.00000 -1.20000 AFIX 0 C12 1 1.016369 0.196485 0.039705 11.00000 0.04249 0.04175 = 0.04653 0.01896 0.00710 0.01363 AFIX 43 H12 2 1.092746 0.209287 0.077539 11.00000 -1.20000 AFIX 0 C13 1 0.933482 0.233500 0.196797 11.00000 0.04432 0.03890 = 0.04295 0.01451 0.01072 0.01891 C14 1 0.888403 0.105126 0.177599 11.00000 0.04194 0.04000 = 0.04277 0.01589 0.00832 0.01407 AFIX 43 H14 2 0.837752 0.064243 0.128549 11.00000 -1.20000 AFIX 0 C15 1 0.919137 0.039418 0.231424 11.00000 0.04463 0.03844 = 0.05048 0.01306 0.01122 0.01090 AFIX 43 H15 2 0.889544 -0.045553 0.217407 11.00000 -1.20000 AFIX 0 C16 1 0.992309 0.096035 0.305232 11.00000 0.04418 0.04622 = 0.03978 0.01732 0.01073 0.01679 C17 1 1.033139 0.224404 0.324862 11.00000 0.04350 0.04076 = 0.03945 0.00743 0.00849 0.01425 AFIX 43 H17 2 1.079978 0.265452 0.374793 11.00000 -1.20000 AFIX 0 C18 1 1.004766 0.291029 0.271003 11.00000 0.04888 0.04054 = 0.04793 0.01244 0.00935 0.01500 AFIX 43 H18 2 1.034279 0.376006 0.285109 11.00000 -1.20000 AFIX 0 C19 1 1.034382 0.027549 0.361351 11.00000 0.03724 0.04215 = 0.04505 0.01306 0.00875 0.00922 AFIX 43 H19 2 1.068980 0.072321 0.412564 11.00000 -1.20000 AFIX 0 C20 1 1.027599 -0.092401 0.345741 11.00000 0.04441 0.04609 = 0.04485 0.01769 0.01304 0.01597 AFIX 43 H20 2 0.991123 -0.136009 0.294509 11.00000 -1.20000 AFIX 0 C21 1 1.069889 -0.164267 0.398484 11.00000 0.03913 0.03932 = 0.04703 0.01549 0.01209 0.01564 C22 1 1.049626 -0.290212 0.371337 11.00000 0.05871 0.04019 = 0.04327 0.01183 0.00514 0.01390 AFIX 43 H22 2 1.011539 -0.327269 0.319277 11.00000 -1.20000 AFIX 0 C23 1 1.084969 -0.361370 0.420192 11.00000 0.04827 0.03925 = 0.05886 0.01503 0.00631 0.01322 AFIX 43 H23 2 1.068629 -0.445862 0.400762 11.00000 -1.20000 AFIX 0 C24 1 1.144313 -0.309619 0.497620 11.00000 0.04972 0.04062 = 0.03876 0.01550 0.01027 0.01576 C25 1 1.168051 -0.183325 0.525300 11.00000 0.04665 0.05004 = 0.04500 0.01551 0.00704 0.01164 AFIX 43 H25 2 1.209495 -0.146599 0.576880 11.00000 -1.20000 AFIX 0 C26 1 1.130672 -0.111577 0.476926 11.00000 0.05764 0.03840 = 0.04177 0.01601 0.01549 0.01355 AFIX 43 H26 2 1.146020 -0.027218 0.496638 11.00000 -1.20000 AFIX 0 C27 1 1.183601 -0.387723 0.547688 11.00000 0.05637 0.05266 = 0.06521 0.02669 0.02640 0.02380 AFIX 43 H27 2 1.152344 -0.472095 0.528459 11.00000 -1.20000 AFIX 0 MOLE 2 O101 4 1.297926 0.441182 0.430850 11.00000 0.08293 0.05552 = 0.07062 0.02780 0.01239 0.02858 N101 3 1.603024 -0.294769 0.863511 11.00000 0.06238 0.03553 = 0.03774 0.01067 0.00974 0.01765 C101 1 1.644628 -0.404168 0.834102 11.00000 0.04468 0.03384 = 0.04412 0.00865 0.01570 0.00642 C102 1 1.604446 -0.465088 0.756501 11.00000 0.06810 0.04493 = 0.05024 0.01512 0.01526 0.01026 AFIX 43 H102 2 1.548604 -0.434698 0.723988 11.00000 -1.20000 AFIX 0 C103 1 1.645663 -0.570819 0.725961 11.00000 0.08898 0.04148 = 0.06067 0.00262 0.02756 0.00983 AFIX 43 H103 2 1.619706 -0.609426 0.672996 11.00000 -1.20000 AFIX 0 C104 1 1.724688 -0.618805 0.773605 11.00000 0.08255 0.03427 = 0.09106 0.01220 0.04455 0.01751 AFIX 43 H104 2 1.752021 -0.690293 0.753580 11.00000 -1.20000 AFIX 0 C105 1 1.762654 -0.559496 0.851270 11.00000 0.05574 0.04788 = 0.08072 0.02636 0.02636 0.02300 AFIX 43 H105 2 1.815136 -0.592385 0.883957 11.00000 -1.20000 AFIX 0 C106 1 1.725186 -0.452218 0.882405 11.00000 0.04699 0.03818 = 0.06170 0.01745 0.01576 0.01150 AFIX 43 H106 2 1.753600 -0.412672 0.935095 11.00000 -1.20000 AFIX 0 C107 1 1.582563 -0.258162 0.941992 11.00000 0.04347 0.04006 = 0.04445 0.01575 0.01070 0.01694 C108 1 1.529832 -0.343736 0.981410 11.00000 0.05855 0.03474 = 0.04849 0.01654 0.01693 0.01892 AFIX 43 H108 2 1.504603 -0.426527 0.955740 11.00000 -1.20000 AFIX 0 C109 1 1.514624 -0.306939 1.058196 11.00000 0.06092 0.04709 = 0.05061 0.02649 0.02352 0.02591 AFIX 43 H109 2 1.483384 -0.365355 1.084869 11.00000 -1.20000 AFIX 0 C110 1 1.545362 -0.183930 1.096043 11.00000 0.04763 0.05776 = 0.04146 0.01595 0.01216 0.02750 AFIX 43 H110 2 1.535722 -0.158999 1.148093 11.00000 -1.20000 AFIX 0 C111 1 1.590520 -0.098875 1.055358 11.00000 0.04349 0.04265 = 0.04994 0.01485 0.00127 0.01565 AFIX 43 H111 2 1.607228 -0.015766 1.079605 11.00000 -1.20000 AFIX 0 C112 1 1.611323 -0.134349 0.979800 11.00000 0.04079 0.03849 = 0.04580 0.01572 0.01064 0.01364 AFIX 43 H112 2 1.644672 -0.075593 0.953836 11.00000 -1.20000 AFIX 0 C113 1 1.582564 -0.215827 0.813362 11.00000 0.05011 0.03234 = 0.03293 0.00634 0.00791 0.00915 C114 1 1.463093 -0.173554 0.806433 11.00000 0.04733 0.04255 = 0.03724 0.00612 0.01336 0.01291 AFIX 43 H114 2 1.396237 -0.196417 0.835170 11.00000 -1.20000 AFIX 0 C115 1 1.443798 -0.098501 0.757481 11.00000 0.04081 0.04004 = 0.04024 0.00881 0.00443 0.01491 AFIX 43 H115 2 1.362536 -0.073299 0.752461 11.00000 -1.20000 AFIX 0 C116 1 1.542427 -0.059433 0.715409 11.00000 0.04743 0.03516 = 0.04134 0.00859 0.01121 0.00850 C117 1 1.661379 -0.102323 0.723068 11.00000 0.03789 0.04806 = 0.04862 0.01891 0.01113 0.01354 AFIX 43 H117 2 1.728374 -0.078692 0.694601 11.00000 -1.20000 AFIX 0 C118 1 1.682713 -0.178073 0.771125 11.00000 0.04866 0.04528 = 0.04068 0.01262 0.01004 0.01949 AFIX 43 H118 2 1.763538 -0.204088 0.775498 11.00000 -1.20000 AFIX 0 C119 1 1.528273 0.020711 0.663350 11.00000 0.04663 0.03956 = 0.03848 0.00922 0.01186 0.01030 AFIX 43 H119 2 1.599636 0.036921 0.636254 11.00000 -1.20000 AFIX 0 C120 1 1.425436 0.074164 0.649472 11.00000 0.05122 0.04144 = 0.03871 0.01195 0.01324 0.01516 AFIX 43 H120 2 1.354952 0.061698 0.677689 11.00000 -1.20000 AFIX 0 C121 1 1.413937 0.150435 0.593907 11.00000 0.04378 0.03495 = 0.04587 0.01085 0.00445 0.00814 C122 1 1.311019 0.214802 0.593712 11.00000 0.05282 0.04308 = 0.05029 0.01489 0.01683 0.01487 AFIX 43 H122 2 1.250420 0.208075 0.628575 11.00000 -1.20000 AFIX 0 C123 1 1.298039 0.288813 0.542041 11.00000 0.05727 0.04573 = 0.04725 0.01250 0.00733 0.02293 AFIX 43 H123 2 1.228198 0.330174 0.541934 11.00000 -1.20000 AFIX 0 C124 1 1.388680 0.300922 0.490945 11.00000 0.05455 0.03444 = 0.03864 0.00584 0.00112 0.00975 C125 1 1.489430 0.236299 0.490383 11.00000 0.05617 0.04244 = 0.03220 0.00920 0.01131 0.00926 AFIX 43 H125 2 1.549399 0.242862 0.455165 11.00000 -1.20000 AFIX 0 C126 1 1.502756 0.162609 0.540774 11.00000 0.04752 0.04386 = 0.04382 0.01090 0.00350 0.01135 AFIX 43 H126 2 1.571785 0.120281 0.539505 11.00000 -1.20000 AFIX 0 C127 1 1.381098 0.381489 0.436510 11.00000 0.05784 0.04680 = 0.04971 0.01361 0.00418 0.01416 AFIX 43 H127 2 1.446139 0.386132 0.404100 11.00000 -1.20000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 2009src1319 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 O1 - C27 N1 - C13 C1 C7 C1 - C2 C6 N1 C2 - C1 C3 C3 - C4 C2 C4 - C5 C3 C5 - C4 C6 C6 - C5 C1 C7 - C12 C8 N1 C8 - C9 C7 C9 - C10 C8 C10 - C11 C9 C11 - C10 C12 C12 - C11 C7 C13 - C18 C14 N1 C14 - C15 C13 C15 - C16 C14 C16 - C15 C17 C19 C17 - C18 C16 C18 - C13 C17 C19 - C20 C16 C20 - C19 C21 C21 - C22 C26 C20 C22 - C23 C21 C23 - C22 C24 C24 - C23 C25 C27 C25 - C26 C24 C26 - C25 C21 C27 - O1 C24 O101 - C127 N101 - C101 C107 C113 C101 - C102 C106 N101 C102 - C101 C103 C103 - C104 C102 C104 - C105 C103 C105 - C104 C106 C106 - C105 C101 C107 - C108 C112 N101 C108 - C109 C107 C109 - C108 C110 C110 - C111 C109 C111 - C112 C110 C112 - C111 C107 C113 - C118 C114 N101 C114 - C115 C113 C115 - C114 C116 C116 - C115 C117 C119 C117 - C118 C116 C118 - C117 C113 C119 - C120 C116 C120 - C119 C121 C121 - C126 C122 C120 C122 - C123 C121 C123 - C124 C122 C124 - C123 C125 C127 C125 - C126 C124 C126 - C125 C121 C127 - O101 C124 35011 Reflections read, of which 4153 rejected -12 =< h =< 11, -13 =< k =< 13, -21 =< l =< 21, Max. 2-theta = 50.00 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 2 7 1 3.67 1.67 2 16.45 -3 -11 3 8.17 2.24 2 18.87 10 -6 3 -0.09 0.03 2 0.99 3 -8 4 2.99 0.52 4 5.56 -7 10 4 11.19 2.47 2 23.62 -8 -6 7 -0.03 0.01 5 0.78 6 Inconsistent equivalents 6734 Unique reflections, of which 0 suppressed R(int) = 0.1570 R(sigma) = 0.1511 Friedel opposites merged Maximum memory for data reduction = 4700 / 67756 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 = 6168 / 695573 wR2 = 0.2547 before cycle 1 for 6734 data and 523 / 523 parameters GooF = S = 1.061; Restrained GooF = 1.061 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1017 * P )^2 + 0.92 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19351 0.00067 1.213 OSF Mean shift/su = 0.066 Maximum = 1.213 for OSF Max. shift = 0.001 A for C105 Max. dU = 0.000 for C2 Least-squares cycle 2 Maximum vector length = 511 Memory required = 6168 / 695573 wR2 = 0.2550 before cycle 2 for 6734 data and 523 / 523 parameters GooF = S = 1.063; Restrained GooF = 1.063 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1017 * P )^2 + 0.92 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19374 0.00067 0.341 OSF Mean shift/su = 0.028 Maximum = 0.341 for OSF Max. shift = 0.000 A for C2 Max. dU = 0.000 for C2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 6168 / 695573 wR2 = 0.2550 before cycle 3 for 6734 data and 523 / 523 parameters GooF = S = 1.063; Restrained GooF = 1.063 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1017 * P )^2 + 0.92 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19376 0.00067 0.028 OSF Mean shift/su = 0.004 Maximum = 0.028 for OSF Max. shift = 0.000 A for C3 Max. dU = 0.000 for C11 Least-squares cycle 4 Maximum vector length = 511 Memory required = 6168 / 695573 wR2 = 0.2550 before cycle 4 for 6734 data and 523 / 523 parameters GooF = S = 1.063; Restrained GooF = 1.063 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1017 * P )^2 + 0.92 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19376 0.00067 0.004 OSF Mean shift/su = 0.001 Maximum = -0.007 for U33 N1 Max. shift = 0.000 A for C3 Max. dU = 0.000 for C11 Least-squares cycle 5 Maximum vector length = 511 Memory required = 6168 / 695573 wR2 = 0.2550 before cycle 5 for 6734 data and 523 / 523 parameters GooF = S = 1.063; Restrained GooF = 1.063 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1017 * P )^2 + 0.92 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19376 0.00067 0.001 OSF Mean shift/su = 0.000 Maximum = 0.002 for U13 C126 Max. shift = 0.000 A for H3 Max. dU = 0.000 for C127 Least-squares cycle 6 Maximum vector length = 511 Memory required = 6168 / 695573 wR2 = 0.2550 before cycle 6 for 6734 data and 523 / 523 parameters GooF = S = 1.063; Restrained GooF = 1.063 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1017 * P )^2 + 0.92 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19376 0.00067 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for U13 C126 Max. shift = 0.000 A for H3 Max. dU = 0.000 for C127 Least-squares cycle 7 Maximum vector length = 511 Memory required = 6168 / 695573 wR2 = 0.2550 before cycle 7 for 6734 data and 523 / 523 parameters GooF = S = 1.063; Restrained GooF = 1.063 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1017 * P )^2 + 0.92 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19376 0.00067 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C110 Max. dU = 0.000 for C103 Least-squares cycle 8 Maximum vector length = 511 Memory required = 6168 / 695573 wR2 = 0.2550 before cycle 8 for 6734 data and 523 / 523 parameters GooF = S = 1.063; Restrained GooF = 1.063 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1017 * P )^2 + 0.92 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19376 0.00067 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C12 Max. dU = 0.000 for C11 Least-squares cycle 9 Maximum vector length = 511 Memory required = 6168 / 695573 wR2 = 0.2550 before cycle 9 for 6734 data and 523 / 523 parameters GooF = S = 1.063; Restrained GooF = 1.063 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1017 * P )^2 + 0.92 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19376 0.00067 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C104 Max. dU = 0.000 for C4 Least-squares cycle 10 Maximum vector length = 511 Memory required = 6168 / 695573 wR2 = 0.2550 before cycle 10 for 6734 data and 523 / 523 parameters GooF = S = 1.063; Restrained GooF = 1.063 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1017 * P )^2 + 0.92 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.19376 0.00067 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x O1 Max. shift = 0.000 A for O1 Max. dU = 0.000 for C5 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 11 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.7797 0.3792 0.2534 43 0.950 0.000 C2 C1 C3 H3 0.7055 0.5619 0.2815 43 0.950 0.000 C3 C4 C2 H4 0.7289 0.6931 0.1979 43 0.950 0.000 C4 C5 C3 H5 0.8442 0.6523 0.0942 43 0.950 0.000 C5 C4 C6 H6 0.9221 0.4715 0.0662 43 0.950 0.000 C6 C5 C1 H8 0.7132 0.2461 0.0149 43 0.950 0.000 C8 C9 C7 H9 0.7175 0.1478 -0.1143 43 0.950 0.000 C9 C10 C8 H10 0.9074 0.0766 -0.1449 43 0.950 0.000 C10 C11 C9 H11 1.0938 0.1072 -0.0495 43 0.950 0.000 C11 C10 C12 H12 1.0944 0.2094 0.0784 43 0.950 0.000 C12 C11 C7 H14 0.8368 0.0634 0.1274 43 0.950 0.000 C14 C15 C13 H15 0.8888 -0.0474 0.2170 43 0.950 0.000 C15 C16 C14 H17 1.0811 0.2663 0.3759 43 0.950 0.000 C17 C18 C16 H18 1.0348 0.3778 0.2854 43 0.950 0.000 C18 C13 C17 H19 1.0697 0.0733 0.4137 43 0.950 0.000 C19 C20 C16 H20 0.9903 -0.1370 0.2933 43 0.950 0.000 C20 C19 C21 H22 1.0107 -0.3280 0.3181 43 0.950 0.000 C22 C23 C21 H23 1.0683 -0.4477 0.4003 43 0.950 0.000 C23 C22 C24 H25 1.2104 -0.1459 0.5780 43 0.950 0.000 C25 C26 C24 H26 1.1463 -0.0254 0.4971 43 0.950 0.000 C26 C25 C21 H27 1.1517 -0.4740 0.5279 43 0.950 0.000 C27 O1 C24 H102 1.5474 -0.4340 0.7232 43 0.950 0.000 C102 C101 C103 H103 1.6193 -0.6103 0.6718 43 0.950 0.000 C103 C104 C102 H104 1.7528 -0.6918 0.7532 43 0.950 0.000 C104 C105 C103 H105 1.8162 -0.5932 0.8848 43 0.950 0.000 C105 C104 C106 H106 1.7542 -0.4118 0.9363 43 0.950 0.000 C106 C105 C101 H108 1.5041 -0.4284 0.9552 43 0.950 0.000 C108 C109 C107 H109 1.4827 -0.3667 1.0855 43 0.950 0.000 C109 C108 C110 H110 1.5355 -0.1584 1.1493 43 0.950 0.000 C110 C111 C109 H111 1.6076 -0.0139 1.0801 43 0.950 0.000 C111 C112 C110 H112 1.6453 -0.0743 0.9533 43 0.950 0.000 C112 C111 C107 H114 1.3949 -0.1969 0.8359 43 0.950 0.000 C114 C115 C113 H115 1.3608 -0.0726 0.7524 43 0.950 0.000 C115 C114 C116 H117 1.7298 -0.0783 0.6939 43 0.950 0.000 C117 C118 C116 H118 1.7653 -0.2047 0.7756 43 0.950 0.000 C118 C117 C113 H119 1.6011 0.0373 0.6356 43 0.950 0.000 C119 C120 C116 H120 1.3534 0.0614 0.6784 43 0.950 0.000 C120 C119 C121 H122 1.2490 0.2079 0.6293 43 0.950 0.000 C122 C123 C121 H123 1.2267 0.3311 0.5419 43 0.950 0.000 C123 C124 C122 H125 1.5507 0.2430 0.4544 43 0.950 0.000 C125 C126 C124 H126 1.5733 0.1193 0.5395 43 0.950 0.000 C126 C125 C121 H127 1.4475 0.3861 0.4034 43 0.950 0.000 C127 O101 C124 2009src1319 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq O1 1.25302 -0.35132 0.61165 1.00000 0.08208 0.07740 0.05231 0.03140 0.01229 0.02504 0.06714 0.00986 0.00041 0.00037 0.00026 0.00000 0.00268 0.00279 0.00295 0.00243 0.00229 0.00213 0.00112 N1 0.90338 0.29711 0.13961 1.00000 0.05794 0.03943 0.04374 0.01636 0.01323 0.02165 0.04418 0.00896 0.00038 0.00034 0.00026 0.00000 0.00238 0.00226 0.00293 0.00215 0.00201 0.00183 0.00102 C1 0.86001 0.40795 0.15804 1.00000 0.04250 0.03396 0.03589 0.00882 0.00445 0.01066 0.03734 0.00974 0.00043 0.00039 0.00029 0.00000 0.00246 0.00253 0.00315 0.00234 0.00218 0.00194 0.00112 C2 0.79387 0.43476 0.22094 1.00000 0.04188 0.03465 0.05196 0.00837 0.00109 0.00762 0.04396 0.01000 0.00043 0.00041 0.00032 0.00000 0.00257 0.00263 0.00366 0.00250 0.00240 0.00201 0.00125 H2 0.77969 0.37921 0.25340 1.00000 0.05275 0.00000 0.00000 C3 0.74786 0.54261 0.23708 1.00000 0.05330 0.05199 0.04682 0.00661 -0.00579 0.01762 0.05203 0.01069 0.00048 0.00046 0.00034 0.00000 0.00294 0.00315 0.00368 0.00288 0.00250 0.00236 0.00138 H3 0.70550 0.56189 0.28151 1.00000 0.06244 0.00000 0.00000 C4 0.76394 0.62141 0.18839 1.00000 0.07185 0.05028 0.05928 0.00572 -0.00756 0.02813 0.06131 0.01195 0.00057 0.00050 0.00038 0.00000 0.00361 0.00333 0.00437 0.00321 0.00319 0.00274 0.00159 H4 0.72892 0.69307 0.19795 1.00000 0.07357 0.00000 0.00000 C5 0.83034 0.59629 0.12633 1.00000 0.06550 0.03865 0.05933 0.02151 -0.01053 0.00901 0.05526 0.01121 0.00052 0.00045 0.00037 0.00000 0.00330 0.00295 0.00424 0.00292 0.00300 0.00243 0.00150 H5 0.84420 0.65232 0.09415 1.00000 0.06632 0.00000 0.00000 C6 0.87773 0.48916 0.11001 1.00000 0.05649 0.04509 0.04974 0.01726 -0.00025 0.01261 0.05023 0.01072 0.00048 0.00043 0.00033 0.00000 0.00296 0.00299 0.00375 0.00280 0.00253 0.00230 0.00135 H6 0.92205 0.47150 0.06623 1.00000 0.06028 0.00000 0.00000 C7 0.90419 0.23807 0.06040 1.00000 0.05149 0.03599 0.04335 0.01738 0.00984 0.01412 0.04168 0.01074 0.00046 0.00041 0.00031 0.00000 0.00284 0.00260 0.00355 0.00253 0.00246 0.00209 0.00121 C8 0.79163 0.21867 0.00207 1.00000 0.05493 0.04508 0.04867 0.02305 0.01280 0.01579 0.04679 0.01131 0.00049 0.00043 0.00033 0.00000 0.00295 0.00291 0.00384 0.00282 0.00262 0.00225 0.00130 H8 0.71319 0.24613 0.01493 1.00000 0.05615 0.00000 0.00000 C9 0.79366 0.15953 -0.07459 1.00000 0.05532 0.05068 0.03696 0.01420 0.00607 0.01659 0.04665 0.01132 0.00049 0.00044 0.00032 0.00000 0.00292 0.00300 0.00355 0.00271 0.00242 0.00233 0.00126 H9 0.71754 0.14777 -0.11428 1.00000 0.05598 0.00000 0.00000 C10 0.90625 0.11817 -0.09267 1.00000 0.05920 0.04154 0.03848 0.01427 0.01672 0.01710 0.04420 0.01112 0.00047 0.00041 0.00032 0.00000 0.00308 0.00277 0.00333 0.00250 0.00259 0.00226 0.00123 H10 0.90736 0.07658 -0.14493 1.00000 0.05304 0.00000 0.00000 C11 1.01634 0.13629 -0.03630 1.00000 0.04779 0.04409 0.04542 0.01623 0.01458 0.01423 0.04385 0.01096 0.00047 0.00042 0.00032 0.00000 0.00282 0.00287 0.00368 0.00272 0.00254 0.00215 0.00124 H11 1.09375 0.10724 -0.04949 1.00000 0.05262 0.00000 0.00000 C12 1.01639 0.19643 0.03973 1.00000 0.04337 0.04169 0.04666 0.01888 0.00747 0.01380 0.04209 0.01083 0.00044 0.00041 0.00032 0.00000 0.00262 0.00275 0.00370 0.00268 0.00233 0.00206 0.00123 H12 1.09438 0.20945 0.07838 1.00000 0.05051 0.00000 0.00000 C13 0.93341 0.23342 0.19678 1.00000 0.04462 0.03941 0.04335 0.01464 0.01082 0.01891 0.04015 0.01074 0.00044 0.00041 0.00031 0.00000 0.00254 0.00275 0.00344 0.00256 0.00235 0.00207 0.00118 C14 0.88846 0.10516 0.17756 1.00000 0.04204 0.04021 0.04351 0.01627 0.00834 0.01394 0.04025 0.01056 0.00043 0.00040 0.00030 0.00000 0.00249 0.00274 0.00336 0.00252 0.00222 0.00199 0.00118 H14 0.83681 0.06343 0.12743 1.00000 0.04830 0.00000 0.00000 C15 0.91909 0.03935 0.23136 1.00000 0.04483 0.03873 0.05063 0.01313 0.01131 0.01096 0.04393 0.01102 0.00044 0.00044 0.00032 0.00000 0.00264 0.00267 0.00371 0.00265 0.00247 0.00207 0.00124 H15 0.88883 -0.04744 0.21703 1.00000 0.05272 0.00000 0.00000 C16 0.99233 0.09607 0.30522 1.00000 0.04455 0.04638 0.04025 0.01763 0.01083 0.01678 0.04142 0.01096 0.00044 0.00043 0.00031 0.00000 0.00259 0.00294 0.00342 0.00263 0.00234 0.00213 0.00119 C17 1.03319 0.22441 0.32488 1.00000 0.04380 0.04126 0.04011 0.00759 0.00855 0.01437 0.04133 0.01059 0.00043 0.00041 0.00031 0.00000 0.00256 0.00281 0.00327 0.00248 0.00222 0.00205 0.00118 H17 1.08108 0.26634 0.37587 1.00000 0.04960 0.00000 0.00000 C18 1.00472 0.29102 0.27099 1.00000 0.04929 0.04088 0.04838 0.01278 0.00916 0.01531 0.04513 0.01114 0.00045 0.00044 0.00032 0.00000 0.00274 0.00276 0.00375 0.00271 0.00252 0.00216 0.00127 H18 1.03482 0.37783 0.28538 1.00000 0.05415 0.00000 0.00000 C19 1.03437 0.02757 0.36140 1.00000 0.03751 0.04256 0.04619 0.01332 0.00935 0.00963 0.04146 0.01069 0.00041 0.00042 0.00031 0.00000 0.00244 0.00288 0.00344 0.00251 0.00219 0.00198 0.00120 H19 1.06965 0.07326 0.41372 1.00000 0.04975 0.00000 0.00000 C20 1.02754 -0.09246 0.34568 1.00000 0.04454 0.04637 0.04536 0.01762 0.01305 0.01602 0.04317 0.01111 0.00043 0.00043 0.00032 0.00000 0.00262 0.00301 0.00348 0.00261 0.00232 0.00213 0.00123 H20 0.99027 -0.13701 0.29335 1.00000 0.05180 0.00000 0.00000 C21 1.06993 -0.16422 0.39850 1.00000 0.03951 0.03983 0.04732 0.01559 0.01215 0.01582 0.04009 0.01065 0.00043 0.00041 0.00031 0.00000 0.00246 0.00275 0.00363 0.00261 0.00231 0.00198 0.00119 C22 1.04961 -0.29021 0.37130 1.00000 0.05917 0.04047 0.04362 0.01210 0.00531 0.01426 0.04738 0.01120 0.00048 0.00043 0.00033 0.00000 0.00296 0.00290 0.00347 0.00263 0.00249 0.00223 0.00128 H22 1.01068 -0.32804 0.31812 1.00000 0.05686 0.00000 0.00000 C23 1.08497 -0.36138 0.42017 1.00000 0.04850 0.03977 0.05919 0.01504 0.00643 0.01315 0.04852 0.01142 0.00046 0.00044 0.00034 0.00000 0.00280 0.00279 0.00415 0.00287 0.00262 0.00217 0.00135 H23 1.06829 -0.44769 0.40034 1.00000 0.05822 0.00000 0.00000 C24 1.14433 -0.30956 0.49762 1.00000 0.05000 0.04077 0.03963 0.01548 0.01034 0.01589 0.04158 0.01094 0.00045 0.00042 0.00031 0.00000 0.00269 0.00286 0.00350 0.00258 0.00238 0.00211 0.00119 C25 1.16808 -0.18338 0.52533 1.00000 0.04717 0.05054 0.04564 0.01585 0.00745 0.01185 0.04711 0.01121 0.00045 0.00044 0.00033 0.00000 0.00276 0.00317 0.00356 0.00275 0.00237 0.00222 0.00129 H25 1.21043 -0.14589 0.57802 1.00000 0.05653 0.00000 0.00000 C26 1.13064 -0.11152 0.47692 1.00000 0.05760 0.03917 0.04227 0.01620 0.01531 0.01355 0.04444 0.01118 0.00046 0.00044 0.00031 0.00000 0.00291 0.00270 0.00363 0.00266 0.00256 0.00221 0.00125 H26 1.14626 -0.02536 0.49707 1.00000 0.05333 0.00000 0.00000 C27 1.18357 -0.38783 0.54761 1.00000 0.05651 0.05347 0.06567 0.02725 0.02617 0.02371 0.05363 0.01431 0.00053 0.00051 0.00039 0.00000 0.00319 0.00325 0.00461 0.00329 0.00310 0.00253 0.00144 H27 1.15173 -0.47402 0.52794 1.00000 0.06435 0.00000 0.00000 O101 1.29789 0.44122 0.43085 1.00000 0.08302 0.05623 0.07153 0.02786 0.01283 0.02875 0.06656 0.00879 0.00039 0.00033 0.00025 0.00000 0.00256 0.00232 0.00308 0.00221 0.00217 0.00201 0.00111 N101 1.60300 -0.29475 0.86350 1.00000 0.06241 0.03586 0.03838 0.01101 0.01006 0.01778 0.04421 0.00868 0.00038 0.00033 0.00025 0.00000 0.00246 0.00222 0.00279 0.00205 0.00202 0.00183 0.00102 C101 1.64462 -0.40421 0.83407 1.00000 0.04495 0.03412 0.04505 0.00889 0.01575 0.00643 0.04119 0.01062 0.00044 0.00041 0.00032 0.00000 0.00258 0.00259 0.00361 0.00256 0.00236 0.00202 0.00120 C102 1.60447 -0.46509 0.75646 1.00000 0.06853 0.04482 0.05076 0.01483 0.01547 0.01019 0.05418 0.01196 0.00052 0.00046 0.00035 0.00000 0.00335 0.00311 0.00409 0.00300 0.00289 0.00251 0.00141 H102 1.54743 -0.43404 0.72325 1.00000 0.06501 0.00000 0.00000 C103 1.64574 -0.57084 0.72591 1.00000 0.08920 0.04149 0.06146 0.00283 0.02783 0.00982 0.06505 0.01312 0.00059 0.00048 0.00040 0.00000 0.00412 0.00320 0.00443 0.00310 0.00345 0.00289 0.00163 H103 1.61930 -0.61028 0.67181 1.00000 0.07806 0.00000 0.00000 C104 1.72479 -0.61879 0.77366 1.00000 0.08272 0.03503 0.09156 0.01274 0.04459 0.01780 0.06704 0.01497 0.00061 0.00049 0.00046 0.00000 0.00399 0.00304 0.00581 0.00360 0.00389 0.00278 0.00180 H104 1.75277 -0.69179 0.75322 1.00000 0.08045 0.00000 0.00000 C105 1.76268 -0.55954 0.85134 1.00000 0.05626 0.04819 0.08078 0.02642 0.02655 0.02309 0.05721 0.01393 0.00051 0.00049 0.00042 0.00000 0.00310 0.00324 0.00514 0.00348 0.00311 0.00250 0.00156 H105 1.81620 -0.59318 0.88475 1.00000 0.06866 0.00000 0.00000 C106 1.72519 -0.45224 0.88245 1.00000 0.04731 0.03820 0.06224 0.01761 0.01565 0.01166 0.04762 0.01151 0.00045 0.00042 0.00035 0.00000 0.00274 0.00278 0.00397 0.00275 0.00256 0.00215 0.00133 H106 1.75417 -0.41182 0.93627 1.00000 0.05714 0.00000 0.00000 C107 1.58249 -0.25818 0.94191 1.00000 0.04390 0.04050 0.04486 0.01595 0.01106 0.01708 0.04088 0.01066 0.00043 0.00042 0.00031 0.00000 0.00259 0.00286 0.00351 0.00261 0.00229 0.00206 0.00120 C108 1.52981 -0.34378 0.98141 1.00000 0.05872 0.03516 0.04928 0.01677 0.01724 0.01906 0.04484 0.01133 0.00046 0.00043 0.00032 0.00000 0.00292 0.00264 0.00378 0.00263 0.00256 0.00216 0.00127 H108 1.50409 -0.42836 0.95520 1.00000 0.05381 0.00000 0.00000 C109 1.51457 -0.30700 1.05822 1.00000 0.06129 0.04782 0.05116 0.02666 0.02374 0.02635 0.04794 0.01194 0.00048 0.00045 0.00033 0.00000 0.00302 0.00319 0.00385 0.00288 0.00264 0.00239 0.00133 H109 1.48265 -0.36668 1.08546 1.00000 0.05753 0.00000 0.00000 C110 1.54533 -0.18387 1.09610 1.00000 0.04833 0.05792 0.04218 0.01619 0.01192 0.02764 0.04630 0.01134 0.00044 0.00046 0.00032 0.00000 0.00274 0.00338 0.00343 0.00284 0.00237 0.00235 0.00129 H110 1.53550 -0.15837 1.14927 1.00000 0.05556 0.00000 0.00000 C111 1.59048 -0.09883 1.05535 1.00000 0.04413 0.04276 0.04969 0.01481 0.00166 0.01563 0.04473 0.01087 0.00044 0.00045 0.00033 0.00000 0.00260 0.00283 0.00379 0.00275 0.00239 0.00211 0.00127 H111 1.60756 -0.01393 1.08010 1.00000 0.05368 0.00000 0.00000 C112 1.61126 -0.13432 0.97980 1.00000 0.04130 0.03880 0.04650 0.01573 0.01058 0.01376 0.04046 0.01041 0.00042 0.00042 0.00031 0.00000 0.00250 0.00282 0.00363 0.00259 0.00228 0.00198 0.00120 H112 1.64534 -0.07428 0.95330 1.00000 0.04855 0.00000 0.00000 C113 1.58260 -0.21584 0.81336 1.00000 0.05073 0.03273 0.03352 0.00656 0.00801 0.00918 0.03924 0.00985 0.00045 0.00039 0.00029 0.00000 0.00271 0.00252 0.00312 0.00231 0.00226 0.00202 0.00115 C114 1.46312 -0.17355 0.80648 1.00000 0.04754 0.04265 0.03786 0.00648 0.01315 0.01323 0.04231 0.01023 0.00045 0.00041 0.00030 0.00000 0.00273 0.00274 0.00324 0.00247 0.00225 0.00213 0.00119 H114 1.39487 -0.19690 0.83586 1.00000 0.05078 0.00000 0.00000 C115 1.44375 -0.09844 0.75751 1.00000 0.04135 0.04037 0.04034 0.00874 0.00454 0.01498 0.04029 0.00999 0.00044 0.00040 0.00029 0.00000 0.00255 0.00265 0.00325 0.00246 0.00221 0.00201 0.00117 H115 1.36077 -0.07265 0.75241 1.00000 0.04835 0.00000 0.00000 C116 1.54244 -0.05943 0.71539 1.00000 0.04760 0.03581 0.04194 0.00903 0.01120 0.00878 0.04168 0.01016 0.00044 0.00040 0.00030 0.00000 0.00270 0.00259 0.00336 0.00246 0.00231 0.00205 0.00119 C117 1.66139 -0.10238 0.72300 1.00000 0.03857 0.04826 0.04902 0.01907 0.01132 0.01355 0.04333 0.01043 0.00043 0.00042 0.00031 0.00000 0.00251 0.00288 0.00355 0.00270 0.00228 0.00208 0.00125 H117 1.72979 -0.07833 0.69387 1.00000 0.05199 0.00000 0.00000 C118 1.68271 -0.17816 0.77115 1.00000 0.04898 0.04555 0.04083 0.01290 0.01017 0.01932 0.04334 0.01062 0.00046 0.00042 0.00030 0.00000 0.00273 0.00283 0.00332 0.00258 0.00233 0.00216 0.00121 H118 1.76527 -0.20474 0.77565 1.00000 0.05201 0.00000 0.00000 C119 1.52828 0.02072 0.66330 1.00000 0.04724 0.03967 0.03887 0.00925 0.01165 0.01054 0.04155 0.01001 0.00046 0.00040 0.00029 0.00000 0.00264 0.00267 0.00325 0.00246 0.00225 0.00210 0.00118 H119 1.60112 0.03726 0.63558 1.00000 0.04986 0.00000 0.00000 C120 1.42540 0.07416 0.64951 1.00000 0.05164 0.04142 0.03911 0.01183 0.01321 0.01505 0.04266 0.01031 0.00046 0.00041 0.00030 0.00000 0.00277 0.00269 0.00329 0.00249 0.00231 0.00216 0.00119 H120 1.35343 0.06144 0.67836 1.00000 0.05120 0.00000 0.00000 C121 1.41400 0.15046 0.59390 1.00000 0.04448 0.03532 0.04631 0.01100 0.00451 0.00830 0.04229 0.01008 0.00044 0.00040 0.00031 0.00000 0.00264 0.00262 0.00347 0.00251 0.00235 0.00201 0.00122 C122 1.31097 0.21482 0.59371 1.00000 0.05325 0.04317 0.05061 0.01481 0.01673 0.01515 0.04724 0.01089 0.00047 0.00042 0.00032 0.00000 0.00286 0.00281 0.00365 0.00271 0.00250 0.00222 0.00129 H122 1.24904 0.20791 0.62930 1.00000 0.05669 0.00000 0.00000 C123 1.29802 0.28885 0.54204 1.00000 0.05736 0.04593 0.04781 0.01260 0.00747 0.02256 0.04880 0.01103 0.00050 0.00044 0.00032 0.00000 0.00303 0.00298 0.00364 0.00276 0.00260 0.00233 0.00132 H123 1.22670 0.33113 0.54194 1.00000 0.05856 0.00000 0.00000 C124 1.38872 0.30095 0.49089 1.00000 0.05519 0.03473 0.03869 0.00590 0.00126 0.00997 0.04401 0.01017 0.00048 0.00041 0.00031 0.00000 0.00290 0.00262 0.00333 0.00242 0.00246 0.00215 0.00123 C125 1.48946 0.23629 0.49035 1.00000 0.05606 0.04255 0.03292 0.00929 0.01111 0.00939 0.04382 0.01020 0.00046 0.00042 0.00030 0.00000 0.00290 0.00276 0.00315 0.00249 0.00234 0.00223 0.00121 H125 1.55072 0.24297 0.45437 1.00000 0.05258 0.00000 0.00000 C126 1.50282 0.16258 0.54078 1.00000 0.04812 0.04392 0.04417 0.01117 0.00410 0.01137 0.04557 0.01026 0.00046 0.00043 0.00031 0.00000 0.00277 0.00283 0.00354 0.00266 0.00244 0.00215 0.00127 H126 1.57333 0.11934 0.53950 1.00000 0.05468 0.00000 0.00000 C127 1.38111 0.38141 0.43651 1.00000 0.05821 0.04669 0.05067 0.01378 0.00430 0.01398 0.05174 0.01094 0.00052 0.00045 0.00033 0.00000 0.00308 0.00306 0.00386 0.00285 0.00263 0.00248 0.00137 H127 1.44751 0.38611 0.40337 1.00000 0.06209 0.00000 0.00000 Final Structure Factor Calculation for 2009src1319 in P-1 Total number of l.s. parameters = 523 Maximum vector length = 511 Memory required = 5645 / 22995 wR2 = 0.2550 before cycle 11 for 6734 data and 0 / 523 parameters GooF = S = 1.063; Restrained GooF = 1.063 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1017 * P )^2 + 0.92 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1077 for 3732 Fo > 4sig(Fo) and 0.1912 for all 6734 data wR2 = 0.2550, GooF = S = 1.063, Restrained GooF = 1.063 for all data Occupancy sum of asymmetric unit = 58.00 for non-hydrogen and 42.00 for hydrogen atoms Principal mean square atomic displacements U 0.0860 0.0759 0.0396 O1 0.0612 0.0417 0.0297 N1 0.0438 0.0356 0.0325 C1 0.0572 0.0401 0.0346 C2 0.0718 0.0477 0.0365 C3 0.0960 0.0500 0.0379 C4 0.0898 0.0473 0.0286 C5 0.0653 0.0493 0.0361 C6 0.0521 0.0449 0.0280 C7 0.0588 0.0502 0.0313 C8 0.0576 0.0479 0.0345 C9 0.0613 0.0384 0.0329 C10 0.0535 0.0409 0.0372 C11 0.0510 0.0439 0.0314 C12 0.0509 0.0405 0.0291 C13 0.0475 0.0413 0.0320 C14 0.0516 0.0428 0.0374 C15 0.0523 0.0388 0.0331 C16 0.0470 0.0421 0.0349 C17 0.0508 0.0479 0.0367 C18 0.0470 0.0409 0.0365 C19 0.0535 0.0385 0.0374 C20 0.0506 0.0388 0.0309 C21 0.0607 0.0440 0.0374 C22 0.0605 0.0488 0.0363 C23 0.0519 0.0406 0.0322 C24 0.0521 0.0474 0.0419 C25 0.0592 0.0419 0.0322 C26 0.0785 0.0419 0.0405 C27 0.0858 0.0741 0.0398 O101 0.0629 0.0379 0.0319 N101 0.0543 0.0362 0.0331 C101 0.0708 0.0499 0.0418 C102 0.1002 0.0569 0.0381 C103 0.1163 0.0523 0.0325 C104 0.0865 0.0482 0.0370 C105 0.0637 0.0439 0.0352 C106 0.0507 0.0405 0.0315 C107 0.0628 0.0430 0.0286 C108 0.0742 0.0397 0.0299 C109 0.0664 0.0401 0.0324 C110 0.0552 0.0472 0.0318 C111 0.0491 0.0395 0.0328 C112 0.0511 0.0353 0.0314 C113 0.0495 0.0455 0.0319 C114 0.0479 0.0397 0.0333 C115 0.0497 0.0396 0.0358 C116 0.0546 0.0392 0.0362 C117 0.0543 0.0396 0.0361 C118 0.0487 0.0399 0.0360 C119 0.0533 0.0388 0.0359 C120 0.0495 0.0426 0.0348 C121 0.0589 0.0424 0.0405 C122 0.0628 0.0479 0.0357 C123 0.0590 0.0394 0.0336 C124 0.0573 0.0426 0.0315 C125 0.0512 0.0442 0.0413 C126 0.0617 0.0502 0.0433 C127 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.006 0.013 0.019 0.027 0.035 0.045 0.059 0.079 0.117 1.000 Number in group 679. 734. 606. 717. 664. 640. 671. 678. 667. 678. GooF 1.147 1.221 1.126 1.071 0.997 1.064 0.979 1.047 0.954 0.981 K 52.865 9.284 5.373 2.074 1.506 1.355 1.072 1.038 0.995 0.981 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.07 1.15 1.26 1.44 1.81 inf Number in group 695. 673. 654. 679. 664. 681. 682. 654. 675. 677. GooF 1.043 1.110 1.150 1.085 1.038 1.032 1.025 0.898 0.992 1.221 K 1.718 1.521 2.350 1.131 1.038 1.029 1.023 1.103 1.060 0.968 R1 0.467 0.447 0.414 0.263 0.203 0.153 0.125 0.138 0.089 0.067 Recommended weighting scheme: WGHT 0.0885 1.0719 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 0 2 2036.85 7665.86 7.60 0.535 4.62 2 0 0 1976.26 5420.21 6.12 0.450 4.92 -2 1 0 758.59 1814.36 6.11 0.260 4.93 1 2 0 80.26 2.34 5.75 0.009 4.36 -9 7 6 43.68 181.30 4.73 0.082 0.95 -1 -1 2 310.04 792.32 4.45 0.172 6.04 -11 0 9 40.44 137.76 4.00 0.072 0.87 -2 0 1 2899.04 5339.29 3.96 0.447 4.96 5 0 3 50.30 9.80 3.87 0.019 1.77 0 -8 15 115.81 326.32 3.79 0.110 1.00 11 -4 4 4.53 109.84 3.66 0.064 0.88 11 -5 3 -32.23 105.28 3.64 0.063 0.88 -1 2 0 32.38 3.51 3.57 0.011 5.32 -10 -3 2 34.37 101.73 3.56 0.062 0.92 -5 3 4 34.60 0.68 3.48 0.005 1.78 -1 2 2 114.06 43.64 3.47 0.040 4.24 3 -12 13 163.19 41.00 3.42 0.039 0.85 5 -10 10 92.68 7.03 3.39 0.016 0.97 -3 6 16 180.17 0.99 3.34 0.006 0.86 9 -8 8 56.62 2.17 3.21 0.009 0.89 -6 -5 2 40.07 7.18 3.19 0.016 1.22 0 -8 12 35.36 0.14 3.19 0.002 1.13 2 -9 18 114.71 11.69 3.19 0.021 0.85 1 -2 2 139.25 61.66 3.16 0.048 4.85 -5 1 16 80.74 0.60 3.12 0.005 1.00 4 1 10 48.58 0.50 3.10 0.004 1.25 6 -9 13 86.80 11.96 3.10 0.021 0.89 5 9 0 64.58 2.31 3.05 0.009 0.94 -10 3 8 114.64 208.30 3.03 0.088 0.95 7 -4 6 33.50 1.09 3.00 0.006 1.23 -1 1 2 30.95 4.47 2.98 0.013 5.83 -8 6 11 268.30 131.28 2.96 0.070 0.93 -6 -6 4 181.91 296.51 2.96 0.105 1.14 -3 2 12 203.23 107.54 2.95 0.063 1.31 1 -7 18 261.30 41.29 2.94 0.039 0.91 1 -2 3 58.17 4.03 2.90 0.012 4.21 -1 2 1 43.11 2.67 2.90 0.010 4.88 8 1 2 48.84 103.14 2.89 0.062 1.15 4 -9 2 29.03 0.27 2.86 0.003 1.22 -5 -10 6 225.42 117.04 2.84 0.066 0.91 4 -1 14 67.40 4.09 2.81 0.012 1.05 10 -7 2 35.14 1.10 2.77 0.006 0.93 9 -8 6 3561.48 8.32 2.76 0.018 0.92 10 -7 5 67.42 3.64 2.76 0.012 0.90 0 -1 4 96.28 31.82 2.73 0.034 4.36 2 -1 18 2910.77 9.47 2.73 0.019 0.92 6 -2 15 125.35 41.73 2.73 0.039 0.90 8 -5 3 76.61 35.99 2.72 0.037 1.16 3 -13 6 143.30 8.75 2.72 0.018 0.88 -1 3 0 -11.88 11.30 2.71 0.021 3.70 Bond lengths and angles O1 - Distance Angles C27 1.2054 (0.0067) O1 - N1 - Distance Angles C13 1.4119 (0.0059) C1 1.4131 (0.0056) 122.03 (0.43) C7 1.4253 (0.0065) 116.94 (0.37) 120.68 (0.39) N1 - C13 C1 C1 - Distance Angles C2 1.3826 (0.0069) C6 1.3942 (0.0065) 119.10 (0.43) N1 1.4131 (0.0056) 121.05 (0.42) 119.77 (0.46) C1 - C2 C6 C2 - Distance Angles C1 1.3826 (0.0069) C3 1.3934 (0.0065) 120.52 (0.48) H2 0.9500 119.74 119.74 C2 - C1 C3 C3 - Distance Angles C4 1.3809 (0.0075) C2 1.3934 (0.0065) 119.89 (0.55) H3 0.9500 120.06 120.06 C3 - C4 C2 C4 - Distance Angles C5 1.3695 (0.0082) C3 1.3809 (0.0075) 120.03 (0.50) H4 0.9500 119.98 119.98 C4 - C5 C3 C5 - Distance Angles C4 1.3695 (0.0081) C6 1.3937 (0.0068) 120.49 (0.51) H5 0.9500 119.75 119.75 C5 - C4 C6 C6 - Distance Angles C5 1.3937 (0.0068) C1 1.3942 (0.0065) 119.91 (0.53) H6 0.9500 120.05 120.05 C6 - C5 C1 C7 - Distance Angles C12 1.3824 (0.0063) C8 1.3969 (0.0067) 118.28 (0.50) N1 1.4253 (0.0065) 120.45 (0.44) 121.26 (0.42) C7 - C12 C8 C8 - Distance Angles C9 1.3885 (0.0072) C7 1.3969 (0.0067) 120.42 (0.45) H8 0.9500 119.79 119.79 C8 - C9 C7 C9 - Distance Angles C10 1.3720 (0.0065) C8 1.3885 (0.0072) 119.60 (0.47) H9 0.9500 120.20 120.20 C9 - C10 C8 C10 - Distance Angles C11 1.3606 (0.0067) C9 1.3720 (0.0065) 120.47 (0.50) H10 0.9500 119.77 119.77 C10 - C11 C9 C11 - Distance Angles C10 1.3606 (0.0067) C12 1.3773 (0.0070) 120.49 (0.44) H11 0.9500 119.75 119.75 C11 - C10 C12 C12 - Distance Angles C11 1.3773 (0.0070) C7 1.3824 (0.0063) 120.71 (0.46) H12 0.9500 119.64 119.64 C12 - C11 C7 C13 - Distance Angles C18 1.3803 (0.0069) C14 1.4045 (0.0062) 118.14 (0.44) N1 1.4119 (0.0059) 123.23 (0.42) 118.62 (0.46) C13 - C18 C14 C14 - Distance Angles C15 1.3834 (0.0063) C13 1.4045 (0.0062) 120.26 (0.48) H14 0.9500 119.87 119.87 C14 - C15 C13 C15 - Distance Angles C16 1.3802 (0.0070) C14 1.3834 (0.0063) 121.95 (0.45) H15 0.9500 119.03 119.03 C15 - C16 C14 C16 - Distance Angles C15 1.3802 (0.0070) C17 1.4021 (0.0063) 117.49 (0.43) C19 1.4716 (0.0064) 122.88 (0.43) 119.55 (0.46) C16 - C15 C17 C17 - Distance Angles C18 1.3861 (0.0065) C16 1.4021 (0.0063) 120.97 (0.49) H17 0.9500 119.52 119.52 C17 - C18 C16 C18 - Distance Angles C13 1.3803 (0.0069) C17 1.3861 (0.0065) 121.15 (0.45) H18 0.9500 119.42 119.42 C18 - C13 C17 C19 - Distance Angles C20 1.3311 (0.0061) C16 1.4716 (0.0064) 126.05 (0.50) H19 0.9500 116.98 116.98 C19 - C20 C16 C20 - Distance Angles C19 1.3311 (0.0061) C21 1.4564 (0.0063) 128.27 (0.51) H20 0.9500 115.87 115.87 C20 - C19 C21 C21 - Distance Angles C22 1.3866 (0.0064) C26 1.4033 (0.0070) 117.72 (0.43) C20 1.4564 (0.0063) 119.46 (0.49) 122.81 (0.43) C21 - C22 C26 C22 - Distance Angles C23 1.3776 (0.0065) C21 1.3866 (0.0064) 121.04 (0.52) H22 0.9500 119.48 119.48 C22 - C23 C21 C23 - Distance Angles C22 1.3776 (0.0065) C24 1.3841 (0.0071) 121.28 (0.47) H23 0.9500 119.36 119.36 C23 - C22 C24 C24 - Distance Angles C23 1.3841 (0.0071) C25 1.3867 (0.0065) 118.42 (0.44) C27 1.4683 (0.0069) 119.84 (0.48) 121.71 (0.51) C24 - C23 C25 C25 - Distance Angles C26 1.3843 (0.0064) C24 1.3867 (0.0065) 120.61 (0.51) H25 0.9500 119.70 119.70 C25 - C26 C24 C26 - Distance Angles C25 1.3843 (0.0064) C21 1.4033 (0.0070) 120.91 (0.46) H26 0.9500 119.55 119.55 C26 - C25 C21 C27 - Distance Angles O1 1.2054 (0.0067) C24 1.4683 (0.0069) 125.13 (0.54) H27 0.9500 117.43 117.43 C27 - O1 C24 O101 - Distance Angles C127 1.1995 (0.0054) O101 - N101 - Distance Angles C101 1.4180 (0.0059) C107 1.4184 (0.0064) 122.80 (0.39) C113 1.4264 (0.0058) 119.45 (0.43) 117.75 (0.37) N101 - C101 C107 C101 - Distance Angles C102 1.3750 (0.0073) C106 1.3889 (0.0066) 118.88 (0.47) N101 1.4180 (0.0059) 119.94 (0.46) 121.17 (0.49) C101 - C102 C106 C102 - Distance Angles C101 1.3750 (0.0073) C103 1.3841 (0.0073) 121.11 (0.54) H102 0.9500 119.45 119.45 C102 - C101 C103 C103 - Distance Angles C104 1.3721 (0.0083) C102 1.3841 (0.0073) 120.10 (0.62) H103 0.9500 119.95 119.95 C103 - C104 C102 C104 - Distance Angles C105 1.3703 (0.0086) C103 1.3721 (0.0083) 118.84 (0.53) H104 0.9500 120.58 120.58 C104 - C105 C103 C105 - Distance Angles C104 1.3703 (0.0086) C106 1.3819 (0.0071) 121.84 (0.56) H105 0.9500 119.08 119.08 C105 - C104 C106 C106 - Distance Angles C105 1.3819 (0.0071) C101 1.3889 (0.0066) 119.20 (0.57) H106 0.9500 120.40 120.40 C106 - C105 C101 C107 - Distance Angles C108 1.3880 (0.0064) C112 1.3907 (0.0065) 118.75 (0.49) N101 1.4184 (0.0064) 121.24 (0.44) 119.97 (0.42) C107 - C108 C112 C108 - Distance Angles C109 1.3754 (0.0071) C107 1.3880 (0.0064) 120.46 (0.48) H108 0.9500 119.77 119.77 C108 - C109 C107 C109 - Distance Angles C108 1.3754 (0.0071) C110 1.3825 (0.0069) 120.52 (0.46) H109 0.9500 119.74 119.74 C109 - C108 C110 C110 - Distance Angles C111 1.3772 (0.0067) C109 1.3825 (0.0069) 118.80 (0.51) H110 0.9500 120.60 120.60 C110 - C111 C109 C111 - Distance Angles C112 1.3703 (0.0070) C110 1.3772 (0.0067) 121.28 (0.48) H111 0.9500 119.36 119.36 C111 - C112 C110 C112 - Distance Angles C111 1.3703 (0.0070) C107 1.3907 (0.0065) 120.03 (0.46) H112 0.9500 119.98 119.98 C112 - C111 C107 C113 - Distance Angles C118 1.3931 (0.0064) C114 1.3983 (0.0061) 118.82 (0.42) N101 1.4264 (0.0058) 120.34 (0.39) 120.82 (0.41) C113 - C118 C114 C114 - Distance Angles C115 1.3743 (0.0064) C113 1.3983 (0.0061) 120.45 (0.43) H114 0.9500 119.77 119.77 C114 - C115 C113 C115 - Distance Angles C114 1.3743 (0.0064) C116 1.3858 (0.0064) 121.54 (0.41) H115 0.9500 119.23 119.23 C115 - C114 C116 C116 - Distance Angles C115 1.3858 (0.0064) C117 1.3982 (0.0060) 117.28 (0.42) C119 1.4529 (0.0065) 124.03 (0.41) 118.68 (0.42) C116 - C115 C117 C117 - Distance Angles C118 1.3734 (0.0063) C116 1.3982 (0.0060) 122.23 (0.44) H117 0.9500 118.88 118.88 C117 - C118 C116 C118 - Distance Angles C117 1.3734 (0.0063) C113 1.3931 (0.0064) 119.64 (0.41) H118 0.9500 120.18 120.18 C118 - C117 C113 C119 - Distance Angles C120 1.3384 (0.0060) C116 1.4529 (0.0065) 128.09 (0.45) H119 0.9500 115.96 115.96 C119 - C120 C116 C120 - Distance Angles C119 1.3384 (0.0060) C121 1.4637 (0.0065) 125.75 (0.45) H120 0.9500 117.12 117.12 C120 - C119 C121 C121 - Distance Angles C126 1.3936 (0.0068) C122 1.3976 (0.0062) 118.03 (0.44) C120 1.4637 (0.0065) 122.59 (0.41) 119.37 (0.45) C121 - C126 C122 C122 - Distance Angles C123 1.3906 (0.0068) C121 1.3976 (0.0062) 120.80 (0.47) H122 0.9500 119.60 119.60 C122 - C123 C121 C123 - Distance Angles C124 1.3804 (0.0070) C122 1.3906 (0.0068) 120.04 (0.43) H123 0.9500 119.98 119.98 C123 - C124 C122 C124 - Distance Angles C123 1.3804 (0.0070) C125 1.3798 (0.0063) 119.22 (0.45) C127 1.4791 (0.0069) 121.86 (0.43) 118.93 (0.47) C124 - C123 C125 C125 - Distance Angles C126 1.3712 (0.0065) C124 1.3798 (0.0063) 121.23 (0.47) H125 0.9500 119.39 119.39 C125 - C126 C124 C126 - Distance Angles C125 1.3712 (0.0065) C121 1.3936 (0.0068) 120.67 (0.44) H126 0.9500 119.67 119.67 C126 - C125 C121 C127 - Distance Angles O101 1.1995 (0.0054) C124 1.4791 (0.0069) 125.29 (0.52) H127 0.9500 117.35 117.35 C127 - O101 C124 FMAP and GRID set by program FMAP 2 3 39 GRID -1.389 -2 -2 1.389 2 2 R1 = 0.1911 for 6734 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.26 at 0.7063 0.5120 0.2840 [ 0.59 A from H3 ] Deepest hole -0.28 at 0.4703 0.1623 0.2798 [ 1.19 A from C116 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 5069 / 28617 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.7063 0.5120 0.2840 1.00000 0.05 0.26 0.59 H3 1.07 C3 1.72 C2 1.83 H2 Q2 1 1.9232 -0.3762 0.9653 1.00000 0.05 0.25 1.68 H106 2.06 C12 2.15 H6 2.24 C106 Q3 1 1.7870 -0.4380 0.7813 1.00000 0.05 0.24 1.81 C102 1.87 C103 1.88 C101 2.00 C106 Q4 1 1.2370 -0.2015 0.6928 1.00000 0.05 0.23 1.78 H115 2.04 O1 2.24 C115 2.27 H25 Q5 1 1.4422 -0.1252 0.9535 1.00000 0.05 0.23 1.76 C112 1.95 H111 2.03 H114 2.04 H112 Q6 1 0.7434 -0.0598 0.2041 1.00000 0.05 0.22 1.45 H15 1.87 C15 2.09 H115 2.19 H110 Q7 1 1.5939 -0.4644 0.9751 1.00000 0.05 0.21 1.13 H108 1.63 C108 1.89 H106 1.96 H109 Q8 1 1.0988 0.0546 0.0688 1.00000 0.05 0.21 1.76 H12 2.10 C12 2.11 C10 2.19 C11 Q9 1 1.8208 -0.3613 0.8036 1.00000 0.05 0.21 1.94 C101 2.12 H118 2.14 C106 2.25 C102 Q10 1 1.3127 -0.1983 0.7986 1.00000 0.05 0.21 1.00 H114 1.49 C114 1.82 H115 1.90 C115 Q11 1 1.8517 -0.5023 0.7698 1.00000 0.05 0.21 1.69 C104 1.96 C105 2.08 C103 2.14 H18 Q12 1 1.0171 0.0576 0.0806 1.00000 0.05 0.21 1.78 H12 1.89 C12 1.93 H11 2.11 H14 Q13 1 1.3079 -0.2831 0.7908 1.00000 0.05 0.21 1.24 H114 1.30 H2 1.77 C114 1.80 C2 Q14 1 0.7824 0.5266 0.3609 1.00000 0.05 0.21 1.69 H3 2.13 H123 2.14 O1 2.24 C3 Q15 1 1.7834 -0.4996 0.7088 1.00000 0.05 0.20 1.58 C103 1.84 H103 2.02 C104 2.07 H18 Q16 1 1.7409 -0.0074 0.6297 1.00000 0.05 0.20 1.54 H117 1.61 H119 2.31 C117 2.34 C19 Q17 1 0.7522 0.8185 0.1728 1.00000 0.05 0.20 1.58 H4 1.81 H15 2.28 H110 2.36 C110 Q18 1 1.7056 -0.0494 0.6695 1.00000 0.05 0.20 0.65 H117 1.31 C117 1.73 H119 1.93 C116 Q19 1 1.1631 0.4052 0.2571 1.00000 0.05 0.19 1.46 H18 1.94 C18 2.38 C103 2.39 C102 Q20 1 0.5970 0.5185 0.1446 1.00000 0.05 0.19 1.84 C4 1.90 H108 2.04 C3 2.13 H4 Shortest distances between peaks (including symmetry equivalents) 3 9 0.86 8 12 0.89 10 13 0.94 3 19 0.99 16 18 1.00 3 11 1.09 15 19 1.11 9 19 1.13 11 15 1.22 3 15 1.32 11 19 1.33 6 17 1.41 1 14 1.45 9 11 1.70 4 10 1.93 9 15 1.99 4 13 2.26 7 7 2.28 7 20 2.58 1 20 2.61 1 13 2.64 8 12 2.69 5 10 2.78 12 12 2.83 8 8 2.84 5 5 2.92 2 9 2.99 Time profile in seconds ----------------------- 0.03: Read and process instructions 0.00: Fit rigid groups 0.02: 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. 1.34: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 3.48: Structure factors and derivatives 18.36: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 1.72: Solve l.s. equations 0.00: Generate HTAB table 0.06: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src1319 finished at 16:14:40 Total CPU time: 25.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++