+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src1055 started at 10:33:07 on 10-Aug-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src1055 in P-1 CELL 0.71073 5.3732 13.4962 15.8088 95.389 98.498 101.201 ZERR 4.00 0.0001 0.0004 0.0005 0.001 0.002 0.002 LATT 1 SFAC C H N O UNIT 56 60 4 4 V = 1103.32 F(000) = 456.0 Mu = 0.08 mm-1 Cell Wt = 853.08 Rho = 1.284 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 FMAP 2 PLAN 10 EQIV $1 -x+1, -y+1, -z+2 EQIV $2 -x, -y+2, -z+1 HTAB N1 O1_$1 HTAB N101 O101_$2 SIZE 0.06 0.08 0.85 ACTA HTAB 2.00000 BOND $H WGHT 0.00820 1.51310 L.S. 10 TEMP -153.00 FVAR 0.78364 MOLE 1 C1 1 0.871019 0.677420 0.932795 11.00000 0.02181 0.02620 = 0.01652 0.00312 0.00104 0.00424 C2 1 0.866509 0.778068 0.955490 11.00000 0.02845 0.02873 = 0.02285 0.00039 0.00340 0.00912 AFIX 43 H2 2 0.747145 0.796608 0.989524 11.00000 -1.20000 AFIX 0 C3 1 1.043380 0.851746 0.926726 11.00000 0.03458 0.02388 = 0.02195 0.00187 0.00009 0.00502 AFIX 43 H3 2 1.044055 0.921799 0.940845 11.00000 -1.20000 AFIX 0 C4 1 1.217429 0.823989 0.877976 11.00000 0.02894 0.02416 = 0.02647 0.00414 0.00278 -0.00111 AFIX 43 H4 2 1.337566 0.875162 0.859285 11.00000 -1.20000 AFIX 0 C5 1 1.218937 0.721652 0.855839 11.00000 0.02447 0.02822 = 0.02316 0.00339 0.00569 0.00142 AFIX 43 H5 2 1.342087 0.703635 0.823231 11.00000 -1.20000 AFIX 0 C6 1 1.041033 0.645889 0.881276 11.00000 0.02159 0.02605 = 0.01599 0.00248 0.00057 0.00319 C7 1 0.982997 0.533066 0.870532 11.00000 0.01934 0.02321 = 0.01545 0.00266 0.00273 0.00085 C8 1 0.773230 0.504040 0.922809 11.00000 0.02072 0.03017 = 0.01412 0.00455 0.00389 0.00492 C9 1 1.074653 0.464939 0.821958 11.00000 0.01872 0.02504 = 0.01986 0.00271 0.00332 0.00077 C10 1 1.258839 0.494956 0.761116 11.00000 0.02838 0.02898 = 0.03224 -0.00064 0.01531 0.00126 AFIX 23 H10A 2 1.418296 0.469860 0.777608 11.00000 -1.20000 H10B 2 1.305496 0.570101 0.765020 11.00000 -1.20000 AFIX 0 C11 1 1.134799 0.449848 0.668263 11.00000 0.03092 0.02831 = 0.02434 0.00502 0.00991 0.01060 AFIX 23 H11A 2 0.982746 0.479045 0.650433 11.00000 -1.20000 H11B 2 1.259374 0.468259 0.629090 11.00000 -1.20000 AFIX 0 C12 1 1.052592 0.334543 0.660753 11.00000 0.02305 0.02710 = 0.02266 0.00159 0.00423 0.00672 AFIX 23 H12A 2 1.206673 0.304749 0.672676 11.00000 -1.20000 H12B 2 0.963911 0.307507 0.601268 11.00000 -1.20000 AFIX 0 C13 1 0.872508 0.303814 0.724255 11.00000 0.02326 0.02118 = 0.02887 0.00159 0.00647 0.00444 AFIX 23 H13A 2 0.831896 0.228697 0.721442 11.00000 -1.20000 H13B 2 0.709302 0.326267 0.707611 11.00000 -1.20000 AFIX 0 C14 1 0.993634 0.351102 0.817467 11.00000 0.02653 0.02488 = 0.02331 0.00454 0.00846 0.00616 AFIX 23 H14A 2 0.867098 0.334186 0.856276 11.00000 -1.20000 H14B 2 1.145221 0.322346 0.836961 11.00000 -1.20000 AFIX 0 N1 3 0.714443 0.591992 0.955396 11.00000 0.02172 0.02665 = 0.02258 0.00187 0.00919 0.00381 AFIX 43 H1 2 0.593043 0.594729 0.986769 11.00000 -1.20000 AFIX 0 O1 4 0.662018 0.418787 0.934807 11.00000 0.02770 0.02599 = 0.02397 0.00478 0.01072 0.00263 MOLE 2 C101 1 0.343298 1.035878 0.687978 11.00000 0.01756 0.01932 = 0.02931 0.00542 0.00475 0.00144 C102 1 0.313342 1.107173 0.752207 11.00000 0.02590 0.02301 = 0.03448 0.00476 0.01200 0.00465 AFIX 43 H102 2 0.180114 1.144144 0.743672 11.00000 -1.20000 AFIX 0 C103 1 0.484181 1.123134 0.829706 11.00000 0.03546 0.02292 = 0.03031 -0.00030 0.01205 0.00271 AFIX 43 H103 2 0.466672 1.170984 0.875341 11.00000 -1.20000 AFIX 0 C104 1 0.680499 1.069560 0.840898 11.00000 0.03082 0.02775 = 0.02275 0.00397 0.00317 0.00003 AFIX 43 H104 2 0.798275 1.082362 0.893747 11.00000 -1.20000 AFIX 0 C105 1 0.707009 0.997222 0.775580 11.00000 0.02340 0.02403 = 0.02561 0.00436 0.00245 0.00338 AFIX 43 H105 2 0.842689 0.961419 0.783791 11.00000 -1.20000 AFIX 0 C106 1 0.534183 0.977912 0.698636 11.00000 0.01925 0.01920 = 0.02525 0.00552 0.00483 0.00177 C107 1 0.506934 0.911149 0.615969 11.00000 0.01775 0.01933 = 0.02314 0.00724 0.00303 0.00021 C108 1 0.294790 0.941103 0.556780 11.00000 0.01812 0.01709 = 0.02721 0.00663 0.00403 0.00240 C109 1 0.625125 0.834661 0.594927 11.00000 0.01973 0.01937 = 0.02304 0.00563 0.00156 0.00247 C110 1 0.803451 0.794587 0.660327 11.00000 0.02810 0.02354 = 0.02738 0.00389 -0.00407 0.00672 AFIX 23 H11C 2 0.798347 0.826213 0.718968 11.00000 -1.20000 H11D 2 0.982147 0.813734 0.649349 11.00000 -1.20000 AFIX 0 C111 1 0.725946 0.678820 0.655636 11.00000 0.03117 0.02315 = 0.02670 0.00620 0.00010 0.00755 AFIX 23 H11E 2 0.854965 0.654424 0.695240 11.00000 -1.20000 H11F 2 0.557770 0.660446 0.674957 11.00000 -1.20000 AFIX 0 C112 1 0.706080 0.626110 0.564610 11.00000 0.02815 0.02125 = 0.02979 0.00530 0.00249 0.00724 AFIX 23 H11G 2 0.649013 0.551632 0.563510 11.00000 -1.20000 H11H 2 0.877246 0.639517 0.546743 11.00000 -1.20000 AFIX 0 C113 1 0.514282 0.665291 0.501959 11.00000 0.02469 0.02390 = 0.02364 0.00291 0.00415 0.00596 AFIX 23 H11I 2 0.340319 0.646715 0.517090 11.00000 -1.20000 H11J 2 0.507917 0.632694 0.442682 11.00000 -1.20000 AFIX 0 C114 1 0.591425 0.780933 0.505124 11.00000 0.02457 0.02099 = 0.02320 0.00803 0.00408 0.00527 AFIX 23 H11K 2 0.754714 0.798510 0.482607 11.00000 -1.20000 H11L 2 0.457364 0.804940 0.467365 11.00000 -1.20000 AFIX 0 N101 3 0.202992 1.010612 0.604581 11.00000 0.01938 0.02321 = 0.03001 0.00608 0.00274 0.00718 AFIX 43 H101 2 0.070716 1.036560 0.585167 11.00000 -1.20000 AFIX 0 O101 4 0.205960 0.909272 0.480322 11.00000 0.02425 0.02615 = 0.02569 0.00515 -0.00145 0.00629 HKLF 4 Covalent radii and connectivity table for 2007src1055 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 C1 - C2 N1 C6 C2 - C1 C3 C3 - C4 C2 C4 - C3 C5 C5 - C6 C4 C6 - C5 C1 C7 C7 - C9 C6 C8 C8 - O1 N1 C7 C9 - C7 C14 C10 C10 - C9 C11 C11 - C12 C10 C12 - C11 C13 C13 - C12 C14 C14 - C9 C13 N1 - C8 C1 O1 - C8 C101 - C102 N101 C106 C102 - C101 C103 C103 - C102 C104 C104 - C103 C105 C105 - C106 C104 C106 - C105 C101 C107 C107 - C109 C106 C108 C108 - O101 N101 C107 C109 - C107 C114 C110 C110 - C109 C111 C111 - C112 C110 C112 - C111 C113 C113 - C112 C114 C114 - C109 C113 N101 - C108 C101 O101 - C108 Operators for generating equivalent atoms: $1 -x+1, -y+1, -z+2 $2 -x, -y+2, -z+1 18538 Reflections read, of which 35 rejected -6 =< h =< 6, -17 =< k =< 17, -20 =< l =< 20, Max. 2-theta = 54.97 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -5 5 7 0.22 0.12 6 0.74 -2 4 15 1.31 0.79 3 4.61 2 Inconsistent equivalents 4997 Unique reflections, of which 0 suppressed R(int) = 0.0589 R(sigma) = 0.0577 Friedel opposites merged Maximum memory for data reduction = 3125 / 49329 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 = 3978 / 360836 wR2 = 0.1362 before cycle 1 for 4997 data and 289 / 289 parameters GooF = S = 1.067; Restrained GooF = 1.067 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0082 * P )^2 + 1.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.78307 0.00134 -0.428 OSF Mean shift/esd = 0.097 Maximum = -0.428 for OSF Max. shift = 0.001 A for C12 Max. dU = 0.000 for C6 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3978 / 360836 wR2 = 0.1360 before cycle 2 for 4997 data and 289 / 289 parameters GooF = S = 1.067; Restrained GooF = 1.067 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0082 * P )^2 + 1.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.78294 0.00133 -0.094 OSF Mean shift/esd = 0.034 Maximum = -0.137 for U33 C101 Max. shift = 0.000 A for C12 Max. dU = 0.000 for N101 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3978 / 360836 wR2 = 0.1360 before cycle 3 for 4997 data and 289 / 289 parameters GooF = S = 1.066; Restrained GooF = 1.066 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0082 * P )^2 + 1.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.78295 0.00133 0.002 OSF Mean shift/esd = 0.002 Maximum = -0.012 for U12 N1 Max. shift = 0.000 A for C110 Max. dU = 0.000 for C114 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3978 / 360836 wR2 = 0.1360 before cycle 4 for 4997 data and 289 / 289 parameters GooF = S = 1.066; Restrained GooF = 1.066 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0082 * P )^2 + 1.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.78295 0.00133 0.006 OSF Mean shift/esd = 0.000 Maximum = 0.006 for OSF Max. shift = 0.000 A for C14 Max. dU = 0.000 for C4 Least-squares cycle 5 Maximum vector length = 511 Memory required = 3978 / 360836 wR2 = 0.1360 before cycle 5 for 4997 data and 289 / 289 parameters GooF = S = 1.066; Restrained GooF = 1.066 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0082 * P )^2 + 1.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.78295 0.00133 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for C2 Max. dU = 0.000 for C2 Least-squares cycle 6 Maximum vector length = 511 Memory required = 3978 / 360836 wR2 = 0.1360 before cycle 6 for 4997 data and 289 / 289 parameters GooF = S = 1.066; Restrained GooF = 1.066 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0082 * P )^2 + 1.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.78295 0.00133 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C5 Max. dU = 0.000 for C102 Least-squares cycle 7 Maximum vector length = 511 Memory required = 3978 / 360836 wR2 = 0.1360 before cycle 7 for 4997 data and 289 / 289 parameters GooF = S = 1.066; Restrained GooF = 1.066 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0082 * P )^2 + 1.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.78295 0.00133 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y C102 Max. shift = 0.000 A for C110 Max. dU = 0.000 for C114 Least-squares cycle 8 Maximum vector length = 511 Memory required = 3978 / 360836 wR2 = 0.1360 before cycle 8 for 4997 data and 289 / 289 parameters GooF = S = 1.066; Restrained GooF = 1.066 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0082 * P )^2 + 1.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.78295 0.00133 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y C102 Max. shift = 0.000 A for C5 Max. dU = 0.000 for C110 Least-squares cycle 9 Maximum vector length = 511 Memory required = 3978 / 360836 wR2 = 0.1360 before cycle 9 for 4997 data and 289 / 289 parameters GooF = S = 1.066; Restrained GooF = 1.066 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0082 * P )^2 + 1.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.78295 0.00133 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y C102 Max. shift = 0.000 A for O101 Max. dU = 0.000 for C4 Least-squares cycle 10 Maximum vector length = 511 Memory required = 3978 / 360836 wR2 = 0.1360 before cycle 10 for 4997 data and 289 / 289 parameters GooF = S = 1.066; Restrained GooF = 1.066 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0082 * P )^2 + 1.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.78295 0.00133 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y C102 Max. shift = 0.000 A for C5 Max. dU = 0.000 for C3 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 0.7470 0.7966 0.9895 43 0.950 0.000 C2 C1 C3 H3 1.0441 0.9218 0.9408 43 0.950 0.000 C3 C4 C2 H4 1.3377 0.8751 0.8593 43 0.950 0.000 C4 C3 C5 H5 1.3419 0.7036 0.8231 43 0.950 0.000 C5 C6 C4 H10A 1.4183 0.4699 0.7776 23 0.990 0.000 C10 C9 C11 H10B 1.3053 0.5701 0.7650 23 0.990 0.000 C10 C9 C11 H11A 0.9827 0.4790 0.6504 23 0.990 0.000 C11 C12 C10 H11B 1.2594 0.4682 0.6291 23 0.990 0.000 C11 C12 C10 H12A 1.2067 0.3047 0.6728 23 0.990 0.000 C12 C11 C13 H12B 0.9640 0.3074 0.6013 23 0.990 0.000 C12 C11 C13 H13A 0.8319 0.2287 0.7215 23 0.990 0.000 C13 C12 C14 H13B 0.7093 0.3262 0.7076 23 0.990 0.000 C13 C12 C14 H14A 0.8671 0.3342 0.8562 23 0.990 0.000 C14 C9 C13 H14B 1.1452 0.3224 0.8369 23 0.990 0.000 C14 C9 C13 H1 0.5931 0.5947 0.9868 43 0.880 0.000 N1 C8 C1 H102 0.1802 1.1441 0.7436 43 0.950 0.000 C102 C101 C103 H103 0.4669 1.1710 0.8753 43 0.950 0.000 C103 C102 C104 H104 0.7982 1.0823 0.8937 43 0.950 0.000 C104 C103 C105 H105 0.8425 0.9614 0.7838 43 0.950 0.000 C105 C106 C104 H11C 0.7984 0.8262 0.7190 23 0.990 0.000 C110 C109 C111 H11D 0.9821 0.8138 0.6493 23 0.990 0.000 C110 C109 C111 H11E 0.8552 0.6544 0.6952 23 0.990 0.000 C111 C112 C110 H11F 0.5579 0.6604 0.6750 23 0.990 0.000 C111 C112 C110 H11G 0.6492 0.5516 0.5635 23 0.990 0.000 C112 C111 C113 H11H 0.8774 0.6395 0.5468 23 0.990 0.000 C112 C111 C113 H11I 0.3404 0.6466 0.5171 23 0.990 0.000 C113 C112 C114 H11J 0.5082 0.6327 0.4427 23 0.990 0.000 C113 C112 C114 H11K 0.7546 0.7986 0.4826 23 0.990 0.000 C114 C109 C113 H11L 0.4572 0.8049 0.4674 23 0.990 0.000 C114 C109 C113 H101 0.0707 1.0365 0.5852 43 0.880 0.000 N101 C108 C101 2007src1055 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.87106 0.67744 0.93277 1.00000 0.02172 0.02616 0.01667 0.00320 0.00098 0.00400 0.02187 0.00448 0.00041 0.00017 0.00014 0.00000 0.00109 0.00120 0.00108 0.00090 0.00084 0.00089 0.00047 C2 0.86648 0.77804 0.95546 1.00000 0.02832 0.02879 0.02266 0.00019 0.00334 0.00903 0.02648 0.00477 0.00045 0.00018 0.00015 0.00000 0.00122 0.00129 0.00119 0.00098 0.00094 0.00099 0.00051 H2 0.74704 0.79655 0.98947 1.00000 0.03178 0.00000 0.00000 C3 1.04342 0.85178 0.92673 1.00000 0.03448 0.02355 0.02170 0.00169 -0.00024 0.00504 0.02733 0.00479 0.00046 0.00018 0.00015 0.00000 0.00131 0.00122 0.00119 0.00095 0.00097 0.00098 0.00052 H3 1.04414 0.92183 0.94084 1.00000 0.03279 0.00000 0.00000 C4 1.21744 0.82392 0.87799 1.00000 0.02880 0.02404 0.02626 0.00421 0.00268 -0.00120 0.02744 0.00476 0.00046 0.00018 0.00015 0.00000 0.00123 0.00123 0.00124 0.00098 0.00096 0.00095 0.00052 H4 1.33772 0.87508 0.85935 1.00000 0.03293 0.00000 0.00000 C5 1.21888 0.72166 0.85580 1.00000 0.02435 0.02855 0.02290 0.00333 0.00560 0.00161 0.02565 0.00469 0.00044 0.00018 0.00015 0.00000 0.00116 0.00127 0.00118 0.00097 0.00091 0.00094 0.00050 H5 1.34186 0.70365 0.82311 1.00000 0.03077 0.00000 0.00000 C6 1.04104 0.64590 0.88130 1.00000 0.02134 0.02590 0.01572 0.00242 0.00051 0.00310 0.02153 0.00442 0.00041 0.00017 0.00014 0.00000 0.00109 0.00119 0.00105 0.00088 0.00083 0.00088 0.00046 C7 0.98296 0.53302 0.87054 1.00000 0.01918 0.02329 0.01527 0.00271 0.00255 0.00107 0.01974 0.00434 0.00040 0.00017 0.00013 0.00000 0.00103 0.00113 0.00102 0.00085 0.00080 0.00084 0.00044 C8 0.77327 0.50402 0.92281 1.00000 0.02068 0.02995 0.01413 0.00438 0.00365 0.00495 0.02146 0.00453 0.00041 0.00018 0.00013 0.00000 0.00107 0.00126 0.00103 0.00090 0.00082 0.00091 0.00047 C9 1.07460 0.46493 0.82191 1.00000 0.01867 0.02531 0.01977 0.00270 0.00297 0.00078 0.02183 0.00446 0.00041 0.00017 0.00014 0.00000 0.00105 0.00118 0.00110 0.00091 0.00083 0.00087 0.00047 C10 1.25875 0.49496 0.76111 1.00000 0.02810 0.02898 0.03181 -0.00069 0.01499 0.00113 0.02958 0.00505 0.00046 0.00019 0.00016 0.00000 0.00125 0.00130 0.00135 0.00104 0.00103 0.00100 0.00054 H10A 1.41825 0.46991 0.77762 1.00000 0.03549 0.00000 0.00000 H10B 1.30531 0.57011 0.76499 1.00000 0.03549 0.00000 0.00000 C11 1.13477 0.44981 0.66825 1.00000 0.03077 0.02816 0.02405 0.00503 0.00988 0.01048 0.02642 0.00496 0.00046 0.00018 0.00015 0.00000 0.00126 0.00127 0.00120 0.00099 0.00096 0.00100 0.00051 H11A 0.98272 0.47900 0.65038 1.00000 0.03170 0.00000 0.00000 H11B 1.25938 0.46819 0.62908 1.00000 0.03170 0.00000 0.00000 C12 1.05258 0.33451 0.66081 1.00000 0.02314 0.02724 0.02241 0.00143 0.00401 0.00660 0.02419 0.00474 0.00043 0.00017 0.00015 0.00000 0.00113 0.00123 0.00115 0.00094 0.00088 0.00093 0.00048 H12A 1.20668 0.30474 0.67279 1.00000 0.02902 0.00000 0.00000 H12B 0.96400 0.30743 0.60132 1.00000 0.02902 0.00000 0.00000 C13 0.87245 0.30380 0.72426 1.00000 0.02310 0.02124 0.02876 0.00172 0.00644 0.00452 0.02427 0.00468 0.00043 0.00017 0.00015 0.00000 0.00114 0.00116 0.00125 0.00095 0.00093 0.00089 0.00049 H13A 0.83186 0.22869 0.72147 1.00000 0.02913 0.00000 0.00000 H13B 0.70925 0.32625 0.70759 1.00000 0.02913 0.00000 0.00000 C14 0.99362 0.35115 0.81742 1.00000 0.02621 0.02489 0.02319 0.00459 0.00823 0.00621 0.02413 0.00472 0.00044 0.00017 0.00015 0.00000 0.00118 0.00120 0.00117 0.00094 0.00092 0.00093 0.00048 H14A 0.86712 0.33424 0.85624 1.00000 0.02896 0.00000 0.00000 H14B 1.14522 0.32240 0.83691 1.00000 0.02896 0.00000 0.00000 N1 0.71446 0.59196 0.95540 1.00000 0.02169 0.02678 0.02258 0.00191 0.00934 0.00381 0.02336 0.00384 0.00035 0.00014 0.00012 0.00000 0.00096 0.00104 0.00099 0.00080 0.00076 0.00077 0.00041 H1 0.59309 0.59469 0.98679 1.00000 0.02804 0.00000 0.00000 O1 0.66209 0.41878 0.93482 1.00000 0.02743 0.02599 0.02421 0.00488 0.01089 0.00265 0.02550 0.00329 0.00030 0.00012 0.00010 0.00000 0.00085 0.00088 0.00085 0.00068 0.00066 0.00067 0.00036 C101 0.34334 1.03585 0.68803 1.00000 0.01768 0.01932 0.02868 0.00548 0.00472 0.00132 0.02201 0.00453 0.00040 0.00017 0.00015 0.00000 0.00105 0.00111 0.00121 0.00092 0.00088 0.00084 0.00047 C102 0.31338 1.10715 0.75219 1.00000 0.02568 0.02322 0.03469 0.00491 0.01196 0.00477 0.02713 0.00498 0.00045 0.00018 0.00016 0.00000 0.00120 0.00121 0.00136 0.00102 0.00100 0.00094 0.00052 H102 0.18016 1.14413 0.74364 1.00000 0.03255 0.00000 0.00000 C103 0.48428 1.12313 0.82969 1.00000 0.03526 0.02280 0.03038 -0.00023 0.01210 0.00256 0.02953 0.00510 0.00047 0.00018 0.00016 0.00000 0.00136 0.00122 0.00133 0.00101 0.00106 0.00101 0.00054 H103 0.46687 1.17102 0.87532 1.00000 0.03544 0.00000 0.00000 C104 0.68044 1.06953 0.84088 1.00000 0.03086 0.02775 0.02273 0.00396 0.00307 0.00006 0.02806 0.00493 0.00047 0.00018 0.00015 0.00000 0.00127 0.00127 0.00119 0.00098 0.00096 0.00099 0.00052 H104 0.79820 1.08231 0.89374 1.00000 0.03368 0.00000 0.00000 C105 0.70689 0.99718 0.77556 1.00000 0.02326 0.02389 0.02577 0.00438 0.00253 0.00336 0.02462 0.00463 0.00043 0.00017 0.00015 0.00000 0.00115 0.00118 0.00121 0.00096 0.00091 0.00091 0.00049 H105 0.84253 0.96136 0.78380 1.00000 0.02954 0.00000 0.00000 C106 0.53423 0.97786 0.69860 1.00000 0.01903 0.01901 0.02516 0.00552 0.00490 0.00166 0.02109 0.00448 0.00040 0.00016 0.00014 0.00000 0.00105 0.00110 0.00117 0.00090 0.00087 0.00084 0.00046 C107 0.50698 0.91114 0.61599 1.00000 0.01770 0.01915 0.02319 0.00729 0.00301 0.00025 0.02026 0.00440 0.00040 0.00016 0.00014 0.00000 0.00103 0.00108 0.00114 0.00088 0.00084 0.00083 0.00045 C108 0.29484 0.94109 0.55680 1.00000 0.01825 0.01710 0.02732 0.00671 0.00419 0.00225 0.02081 0.00453 0.00040 0.00016 0.00015 0.00000 0.00104 0.00106 0.00121 0.00090 0.00088 0.00082 0.00046 C109 0.62509 0.83466 0.59497 1.00000 0.01956 0.01955 0.02329 0.00578 0.00150 0.00212 0.02110 0.00443 0.00041 0.00016 0.00014 0.00000 0.00107 0.00110 0.00115 0.00090 0.00086 0.00084 0.00046 C110 0.80344 0.79459 0.66032 1.00000 0.02785 0.02331 0.02742 0.00376 -0.00381 0.00661 0.02687 0.00475 0.00045 0.00017 0.00016 0.00000 0.00123 0.00120 0.00127 0.00098 0.00097 0.00095 0.00052 H11C 0.79836 0.82620 0.71897 1.00000 0.03225 0.00000 0.00000 H11D 0.98212 0.81377 0.64932 1.00000 0.03225 0.00000 0.00000 C111 0.72607 0.67880 0.65562 1.00000 0.03096 0.02300 0.02686 0.00632 0.00032 0.00753 0.02696 0.00485 0.00047 0.00017 0.00015 0.00000 0.00126 0.00120 0.00125 0.00097 0.00097 0.00096 0.00051 H11E 0.85515 0.65443 0.69521 1.00000 0.03235 0.00000 0.00000 H11F 0.55792 0.66040 0.67495 1.00000 0.03235 0.00000 0.00000 C112 0.70621 0.62613 0.56464 1.00000 0.02809 0.02125 0.02995 0.00551 0.00245 0.00711 0.02628 0.00482 0.00045 0.00017 0.00015 0.00000 0.00123 0.00119 0.00130 0.00098 0.00098 0.00095 0.00051 H11G 0.64919 0.55165 0.56354 1.00000 0.03153 0.00000 0.00000 H11H 0.87737 0.63955 0.54677 1.00000 0.03153 0.00000 0.00000 C113 0.51440 0.66527 0.50198 1.00000 0.02454 0.02403 0.02365 0.00290 0.00427 0.00600 0.02394 0.00473 0.00044 0.00017 0.00015 0.00000 0.00115 0.00119 0.00117 0.00093 0.00090 0.00091 0.00048 H11I 0.34042 0.64663 0.51708 1.00000 0.02873 0.00000 0.00000 H11J 0.50817 0.63270 0.44270 1.00000 0.02873 0.00000 0.00000 C114 0.59136 0.78096 0.50518 1.00000 0.02448 0.02101 0.02323 0.00770 0.00409 0.00525 0.02252 0.00462 0.00043 0.00017 0.00014 0.00000 0.00113 0.00113 0.00117 0.00091 0.00089 0.00088 0.00047 H11K 0.75459 0.79860 0.48264 1.00000 0.02702 0.00000 0.00000 H11L 0.45718 0.80494 0.46745 1.00000 0.02702 0.00000 0.00000 N101 0.20297 1.01058 0.60457 1.00000 0.01899 0.02320 0.02972 0.00592 0.00246 0.00723 0.02359 0.00387 0.00035 0.00014 0.00012 0.00000 0.00092 0.00100 0.00107 0.00082 0.00077 0.00076 0.00042 H101 0.07069 1.03652 0.58515 1.00000 0.02831 0.00000 0.00000 O101 0.20589 0.90924 0.48031 1.00000 0.02409 0.02607 0.02549 0.00502 -0.00138 0.00626 0.02555 0.00320 0.00029 0.00012 0.00010 0.00000 0.00083 0.00087 0.00088 0.00069 0.00065 0.00066 0.00036 Final Structure Factor Calculation for 2007src1055 in P-1 Total number of l.s. parameters = 289 Maximum vector length = 511 Memory required = 3689 / 22995 wR2 = 0.1360 before cycle 11 for 4997 data and 0 / 289 parameters GooF = S = 1.066; Restrained GooF = 1.066 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0082 * P )^2 + 1.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0660 for 3778 Fo > 4sig(Fo) and 0.0940 for all 4997 data wR2 = 0.1360, GooF = S = 1.066, Restrained GooF = 1.066 for all data Occupancy sum of asymmetric unit = 32.00 for non-hydrogen and 30.00 for hydrogen atoms Principal mean square atomic displacements U 0.0268 0.0228 0.0160 C1 0.0327 0.0253 0.0214 C2 0.0374 0.0240 0.0205 C3 0.0363 0.0258 0.0203 C4 0.0321 0.0241 0.0208 C5 0.0272 0.0224 0.0150 C6 0.0262 0.0179 0.0152 C7 0.0302 0.0206 0.0135 C8 0.0281 0.0198 0.0175 C9 0.0443 0.0265 0.0179 C10 0.0343 0.0251 0.0199 C11 0.0282 0.0229 0.0214 C12 0.0298 0.0221 0.0210 C13 0.0285 0.0243 0.0195 C14 0.0296 0.0251 0.0154 N1 0.0329 0.0268 0.0168 O1 0.0291 0.0216 0.0153 C101 0.0375 0.0236 0.0203 C102 0.0420 0.0250 0.0217 C103 0.0377 0.0241 0.0225 C104 0.0282 0.0235 0.0222 C105 0.0260 0.0217 0.0156 C106 0.0277 0.0195 0.0136 C107 0.0285 0.0193 0.0146 C108 0.0271 0.0190 0.0172 C109 0.0379 0.0239 0.0188 C110 0.0350 0.0271 0.0188 C111 0.0323 0.0274 0.0192 C112 0.0251 0.0237 0.0230 C113 0.0267 0.0245 0.0163 C114 0.0308 0.0236 0.0164 N101 0.0318 0.0263 0.0186 O101 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.009 0.017 0.026 0.036 0.047 0.059 0.075 0.097 0.139 1.000 Number in group 526. 500. 495. 504. 502. 479. 502. 494. 492. 503. GooF 1.097 1.163 1.132 1.107 1.056 1.043 1.044 0.996 0.940 1.064 K 5.908 1.645 1.211 1.137 1.063 0.984 1.016 1.006 0.999 0.999 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.16 1.32 1.66 inf Number in group 506. 499. 494. 498. 502. 504. 499. 498. 495. 502. GooF 1.175 1.134 1.159 1.101 1.017 1.023 0.990 0.901 0.990 1.139 K 1.092 1.082 1.085 1.065 1.009 0.999 0.983 0.991 1.013 0.999 R1 0.219 0.212 0.187 0.159 0.110 0.092 0.064 0.049 0.049 0.033 Recommended weighting scheme: WGHT 0.0002 1.4931 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) 3 3 0 38.87 7.42 4.31 0.021 1.50 -3 -3 6 39.26 10.18 4.31 0.025 1.42 0 3 3 67.89 29.43 3.79 0.043 3.15 5 0 3 30.13 3.57 3.79 0.015 0.99 1 -9 15 68.49 26.00 3.73 0.040 0.88 -1 2 1 3489.29 3969.80 3.65 0.494 4.46 -3 6 3 11.99 0.08 3.57 0.002 1.49 -5 13 6 71.62 27.13 3.33 0.041 0.78 -2 10 15 141.97 67.27 3.30 0.064 0.79 -3 -8 15 39.04 7.26 3.30 0.021 0.83 -4 -6 14 36.34 86.24 3.29 0.073 0.84 -3 14 5 91.87 38.86 3.27 0.049 0.86 0 3 7 1326.95 1144.76 3.25 0.265 1.88 2 8 11 237.03 161.12 3.24 0.099 0.87 -3 -11 12 1.61 22.85 3.21 0.037 0.81 0 -2 2 2957.46 3338.19 3.21 0.453 5.36 0 4 14 13.16 38.82 3.16 0.049 1.01 -3 6 10 5.28 24.04 3.12 0.038 1.12 0 5 10 20.37 45.12 3.07 0.053 1.27 2 -3 14 27.18 1.47 3.05 0.009 0.98 3 -13 10 51.76 20.10 3.05 0.035 0.83 0 -8 3 774.24 655.07 3.04 0.201 1.62 1 2 7 941.74 812.88 2.99 0.223 1.76 1 -13 2 12.89 0.65 2.97 0.006 1.04 5 6 2 19.98 1.05 2.97 0.008 0.85 -4 -9 13 16.17 46.91 2.97 0.054 0.78 3 -12 7 18.22 0.72 2.95 0.007 0.94 -4 -10 10 32.05 67.85 2.88 0.065 0.80 4 -1 1 13.33 0.71 2.85 0.007 1.30 5 -12 7 53.61 23.17 2.85 0.038 0.78 1 0 4 4097.70 4482.81 2.84 0.525 2.88 4 -10 12 -7.25 9.16 2.78 0.024 0.80 -6 -4 8 -1.45 19.18 2.74 0.034 0.79 -4 2 10 163.97 221.87 2.72 0.117 1.09 2 -8 11 16.72 1.83 2.71 0.011 1.05 -5 4 13 42.76 16.90 2.70 0.032 0.85 -1 -14 2 4.29 22.75 2.69 0.037 0.90 1 -2 2 4361.02 4731.79 2.68 0.539 3.84 -6 3 12 68.06 24.28 2.67 0.039 0.79 -3 1 4 813.58 702.67 2.66 0.208 1.71 0 -6 15 30.91 2.30 2.65 0.012 0.98 1 2 15 76.09 120.44 2.64 0.086 0.95 1 0 1 2299.66 2547.70 2.63 0.395 4.69 1 10 11 175.10 116.98 2.63 0.085 0.86 -4 -10 6 28.56 3.68 2.63 0.015 0.85 3 -1 11 -0.69 9.45 2.63 0.024 1.03 0 -3 9 37.79 18.26 2.63 0.033 1.68 -1 9 1 12.14 0.05 2.63 0.002 1.47 -3 -5 14 9.83 27.14 2.59 0.041 0.94 -6 5 8 42.15 80.31 2.59 0.070 0.84 Bond lengths and angles C1 - Distance Angles C2 1.3772 (0.0032) N1 1.3986 (0.0028) 127.10 (0.21) C6 1.4082 (0.0031) 123.42 (0.21) 109.48 (0.19) C1 - C2 N1 C2 - Distance Angles C1 1.3772 (0.0032) C3 1.3948 (0.0034) 117.64 (0.22) H2 0.9500 121.18 121.18 C2 - C1 C3 C3 - Distance Angles C4 1.3799 (0.0034) C2 1.3948 (0.0034) 120.62 (0.23) H3 0.9500 119.69 119.69 C3 - C4 C2 C4 - Distance Angles C3 1.3799 (0.0034) C5 1.3935 (0.0033) 120.81 (0.22) H4 0.9500 119.60 119.60 C4 - C3 C5 C5 - Distance Angles C6 1.3903 (0.0031) C4 1.3935 (0.0033) 120.25 (0.22) H5 0.9500 119.87 119.87 C5 - C6 C4 C6 - Distance Angles C5 1.3903 (0.0031) C1 1.4082 (0.0031) 117.19 (0.21) C7 1.4826 (0.0031) 135.83 (0.21) 106.94 (0.19) C6 - C5 C1 C7 - Distance Angles C9 1.3538 (0.0031) C6 1.4826 (0.0031) 131.10 (0.20) C8 1.5068 (0.0029) 123.95 (0.20) 104.83 (0.18) C7 - C9 C6 C8 - Distance Angles O1 1.2345 (0.0026) N1 1.3611 (0.0029) 123.31 (0.20) C7 1.5068 (0.0029) 129.53 (0.21) 107.13 (0.19) C8 - O1 N1 C9 - Distance Angles C7 1.3538 (0.0031) C14 1.5045 (0.0031) 124.70 (0.20) C10 1.5052 (0.0030) 123.35 (0.21) 111.85 (0.19) C9 - C7 C14 C10 - Distance Angles C9 1.5052 (0.0030) C11 1.5347 (0.0033) 110.14 (0.19) H10A 0.9900 109.63 109.63 H10B 0.9900 109.63 109.63 108.15 C10 - C9 C11 H10A C11 - Distance Angles C12 1.5211 (0.0032) C10 1.5347 (0.0033) 110.90 (0.19) H11A 0.9900 109.46 109.46 H11B 0.9900 109.46 109.46 108.05 C11 - C12 C10 H11A C12 - Distance Angles C11 1.5211 (0.0032) C13 1.5243 (0.0031) 110.63 (0.19) H12A 0.9900 109.52 109.52 H12B 0.9900 109.52 109.52 108.08 C12 - C11 C13 H12A C13 - Distance Angles C12 1.5243 (0.0031) C14 1.5426 (0.0032) 111.61 (0.19) H13A 0.9900 109.30 109.30 H13B 0.9900 109.30 109.30 107.96 C13 - C12 C14 H13A C14 - Distance Angles C9 1.5045 (0.0031) C13 1.5426 (0.0032) 110.24 (0.18) H14A 0.9900 109.61 109.61 H14B 0.9900 109.61 109.61 108.14 C14 - C9 C13 H14A N1 - Distance Angles C8 1.3611 (0.0029) C1 1.3986 (0.0028) 111.54 (0.18) H1 0.8800 124.23 124.23 N1 - C8 C1 O1 - Distance Angles C8 1.2345 (0.0027) O1 - C101 - Distance Angles C102 1.3806 (0.0033) N101 1.3955 (0.0029) 127.82 (0.21) C106 1.4065 (0.0030) 122.92 (0.22) 109.25 (0.20) C101 - C102 N101 C102 - Distance Angles C101 1.3806 (0.0033) C103 1.3899 (0.0035) 117.89 (0.22) H102 0.9500 121.05 121.05 C102 - C101 C103 C103 - Distance Angles C102 1.3899 (0.0035) C104 1.3895 (0.0035) 120.44 (0.23) H103 0.9500 119.78 119.78 C103 - C102 C104 C104 - Distance Angles C103 1.3895 (0.0035) C105 1.3957 (0.0033) 120.92 (0.23) H104 0.9500 119.54 119.54 C104 - C103 C105 C105 - Distance Angles C106 1.3862 (0.0031) C104 1.3957 (0.0034) 119.66 (0.22) H105 0.9500 120.17 120.17 C105 - C106 C104 C106 - Distance Angles C105 1.3862 (0.0031) C101 1.4065 (0.0030) 118.08 (0.21) C107 1.4864 (0.0032) 134.72 (0.21) 107.05 (0.19) C106 - C105 C101 C107 - Distance Angles C109 1.3532 (0.0031) C106 1.4864 (0.0032) 130.74 (0.20) C108 1.5076 (0.0029) 124.46 (0.20) 104.66 (0.18) C107 - C109 C106 C108 - Distance Angles O101 1.2358 (0.0027) N101 1.3603 (0.0029) 123.69 (0.20) C107 1.5076 (0.0029) 129.42 (0.21) 106.85 (0.19) C108 - O101 N101 C109 - Distance Angles C107 1.3532 (0.0031) C114 1.5008 (0.0031) 123.53 (0.20) C110 1.5139 (0.0030) 122.99 (0.21) 113.48 (0.19) C109 - C107 C114 C110 - Distance Angles C109 1.5139 (0.0030) C111 1.5287 (0.0032) 111.26 (0.19) H11C 0.9900 109.38 109.38 H11D 0.9900 109.38 109.38 108.00 C110 - C109 C111 H11C C111 - Distance Angles C112 1.5227 (0.0033) C110 1.5287 (0.0032) 111.86 (0.19) H11E 0.9900 109.24 109.24 H11F 0.9900 109.24 109.24 107.92 C111 - C112 C110 H11E C112 - Distance Angles C111 1.5227 (0.0033) C113 1.5266 (0.0031) 110.08 (0.19) H11G 0.9900 109.64 109.64 H11H 0.9900 109.64 109.64 108.15 C112 - C111 C113 H11G C113 - Distance Angles C112 1.5266 (0.0031) C114 1.5296 (0.0030) 110.81 (0.19) H11I 0.9900 109.48 109.48 H11J 0.9900 109.48 109.48 108.06 C113 - C112 C114 H11I C114 - Distance Angles C109 1.5008 (0.0031) C113 1.5296 (0.0030) 112.15 (0.18) H11K 0.9900 109.18 109.18 H11L 0.9900 109.18 109.18 107.89 C114 - C109 C113 H11K N101 - Distance Angles C108 1.3603 (0.0029) C101 1.3955 (0.0029) 111.99 (0.18) H101 0.8800 124.00 124.00 N101 - C108 C101 O101 - Distance Angles C108 1.2358 (0.0027) O101 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 1.97 2.846(2) 170.5 N1-H1...O1_$1 0.88 1.98 2.850(2) 169.0 N101-H101...O101_$2 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)