+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2010src0402a started at 20:15:19 on 02-Jun-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2010src0402a CELL 0.71073 17.3279 7.3648 20.9885 90.000 90.000 90.000 ZERR 8.00 0.0002 0.0001 0.0003 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N FE UNIT 128 128 16 8 V = 2678.48 F(000) = 1216.0 Mu = 1.11 mm-1 Cell Wt = 2337.26 Rho = 1.449 MERG 2 OMIT -3.00 55.00 OMIT 0 0 4 OMIT 3 1 2 OMIT 4 0 0 OMIT 3 0 2 OMIT 2 0 2 SHEL 7 0.77 FMAP 2 PLAN 5 SIZE 0.06 0.14 0.25 ACTA BOND $H WGHT 0.01930 2.50180 L.S. 20 TEMP -153.00 FVAR 0.15098 C1 1 0.438762 -0.162884 0.177267 11.00000 0.01599 0.01381 = 0.01744 0.00202 0.00001 0.00086 C2 1 0.419313 -0.244243 0.117490 11.00000 0.01823 0.01125 = 0.02028 0.00056 -0.00131 0.00073 AFIX 43 H2 2 0.379982 -0.331969 0.110651 11.00000 -1.20000 AFIX 0 C3 1 0.469072 -0.171043 0.070029 11.00000 0.01956 0.01728 = 0.01790 -0.00033 0.00068 0.00411 AFIX 43 H3 2 0.468822 -0.201504 0.026047 11.00000 -1.20000 AFIX 0 C4 1 0.519386 -0.043897 0.100113 11.00000 0.01487 0.01930 = 0.01918 0.00176 0.00197 0.00048 AFIX 43 H4 2 0.558584 0.024726 0.079579 11.00000 -1.20000 AFIX 0 C5 1 0.500833 -0.037408 0.166132 11.00000 0.01553 0.01708 = 0.01694 0.00104 -0.00182 -0.00019 AFIX 43 H5 2 0.525145 0.036659 0.197283 11.00000 -1.20000 AFIX 0 C6 1 0.307674 0.149146 0.145343 11.00000 0.02790 0.03174 = 0.02472 0.00670 0.00899 0.01291 AFIX 43 H6 2 0.279619 0.115343 0.182378 11.00000 -1.20000 AFIX 0 C7 1 0.368196 0.278211 0.142800 11.00000 0.03708 0.02030 = 0.02404 -0.00382 -0.00304 0.01102 AFIX 43 H7 2 0.387975 0.345556 0.177781 11.00000 -1.20000 AFIX 0 C8 1 0.394120 0.289168 0.078637 11.00000 0.02449 0.01338 = 0.03116 0.00400 0.00113 0.00291 AFIX 43 H8 2 0.434318 0.365036 0.063190 11.00000 -1.20000 AFIX 0 C9 1 0.349336 0.166738 0.041738 11.00000 0.02378 0.02178 = 0.01944 0.00380 0.00009 0.00734 AFIX 43 H9 2 0.354116 0.146959 -0.002815 11.00000 -1.20000 AFIX 0 C10 1 0.296102 0.078876 0.083015 11.00000 0.01478 0.02430 = 0.03360 0.00569 -0.00145 0.00326 AFIX 43 H10 2 0.259394 -0.010699 0.071085 11.00000 -1.20000 AFIX 0 C11 1 0.414889 -0.113446 0.284378 11.00000 0.01527 0.01470 = 0.02086 0.00366 0.00042 -0.00011 AFIX 43 H11 2 0.450780 -0.016561 0.280511 11.00000 -1.20000 AFIX 0 C12 1 0.380891 -0.144245 0.346041 11.00000 0.01325 0.01669 = 0.01794 0.00210 -0.00036 0.00128 C13 1 0.394411 -0.043922 0.400983 11.00000 0.01854 0.01900 = 0.02267 -0.00184 -0.00098 -0.00034 AFIX 43 H13 2 0.428848 0.055809 0.404952 11.00000 -1.20000 AFIX 0 C14 1 0.347956 -0.116540 0.449666 11.00000 0.02145 0.02587 = 0.01683 -0.00136 -0.00049 0.00611 AFIX 43 H14 2 0.345202 -0.075198 0.492481 11.00000 -1.20000 AFIX 0 C15 1 0.307307 -0.258514 0.423653 11.00000 0.01820 0.02458 = 0.01699 0.00491 0.00347 0.00280 AFIX 43 H15 2 0.271257 -0.332486 0.445771 11.00000 -1.20000 AFIX 0 C16 1 0.293769 -0.412925 0.319146 11.00000 0.02597 0.03174 = 0.02365 -0.00336 0.00282 -0.01295 AFIX 137 H16A 2 0.254443 -0.481838 0.342411 11.00000 -1.50000 H16B 2 0.334425 -0.495611 0.304595 11.00000 -1.50000 H16C 2 0.270035 -0.353431 0.282263 11.00000 -1.50000 AFIX 0 N1 3 0.400329 -0.206985 0.234359 11.00000 0.01835 0.01689 = 0.01707 0.00330 -0.00074 -0.00097 N2 3 0.326969 -0.276445 0.360887 11.00000 0.01489 0.01802 = 0.01719 0.00135 0.00053 -0.00070 FE1 4 0.406792 0.031032 0.112368 11.00000 0.01444 0.01153 = 0.01458 0.00097 0.00040 0.00058 HKLF 4 Covalent radii and connectivity table for 2010src0402a C 0.770 H 0.320 N 0.700 FE 1.240 C1 - N1 C2 C5 Fe1 C2 - C3 C1 Fe1 C3 - C2 C4 Fe1 C4 - C5 C3 Fe1 C5 - C4 C1 Fe1 C6 - C7 C10 Fe1 C7 - C6 C8 Fe1 C8 - C9 C7 Fe1 C9 - C8 C10 Fe1 C10 - C6 C9 Fe1 C11 - N1 C12 C12 - N2 C13 C11 C13 - C12 C14 C14 - C15 C13 C15 - N2 C14 C16 - N2 N1 - C11 C1 N2 - C15 C12 C16 Fe1 - C8 C2 C3 C7 C4 C10 C5 C6 C9 C1 21774 Reflections read, of which 1917 rejected -22 =< h =< 22, -9 =< k =< 9, -27 =< l =< 24, Max. 2-theta = 54.96 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 10 3 2 1.12 0.09 9 0.54 8 1 24 2.32 0.62 2 6.67 2 Inconsistent equivalents 3063 Unique reflections, of which 0 suppressed R(int) = 0.0447 R(sigma) = 0.0423 Friedel opposites merged Maximum memory for data reduction = 2091 / 30739 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 = 2573 / 215198 wR2 = 0.0813 before cycle 1 for 3063 data and 173 / 173 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0193 * P )^2 + 2.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.15096 0.00023 -0.106 OSF Mean shift/su = 0.012 Maximum = -0.106 for OSF Max. shift = 0.000 A for C8 Max. dU = 0.000 for C12 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2573 / 215198 wR2 = 0.0813 before cycle 2 for 3063 data and 173 / 173 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0193 * P )^2 + 2.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.15095 0.00023 -0.033 OSF Mean shift/su = 0.004 Maximum = -0.033 for OSF Max. shift = 0.000 A for C8 Max. dU = 0.000 for C12 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2573 / 215198 wR2 = 0.0813 before cycle 3 for 3063 data and 173 / 173 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0193 * P )^2 + 2.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.15095 0.00023 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for U11 Fe1 Max. shift = 0.000 A for H16C Max. dU = 0.000 for C16 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2573 / 215198 wR2 = 0.0813 before cycle 4 for 3063 data and 173 / 173 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0193 * P )^2 + 2.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.15095 0.00023 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H16B Max. dU = 0.000 for C8 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2573 / 215198 wR2 = 0.0813 before cycle 5 for 3063 data and 173 / 173 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0193 * P )^2 + 2.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.15095 0.00023 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x Fe1 Max. shift = 0.000 A for H16A Max. dU = 0.000 for N1 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2573 / 215198 wR2 = 0.0813 before cycle 6 for 3063 data and 173 / 173 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0193 * P )^2 + 2.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.15095 0.00023 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H16C Max. dU = 0.000 for C16 Least-squares cycle 7 Maximum vector length = 511 Memory required = 2573 / 215198 wR2 = 0.0813 before cycle 7 for 3063 data and 173 / 173 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0193 * P )^2 + 2.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.15095 0.00023 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C10 Max. dU = 0.000 for C6 Least-squares cycle 8 Maximum vector length = 511 Memory required = 2573 / 215198 wR2 = 0.0813 before cycle 8 for 3063 data and 173 / 173 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0193 * P )^2 + 2.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.15095 0.00023 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x Fe1 Max. shift = 0.000 A for H16C Max. dU = 0.000 for C4 Least-squares cycle 9 Maximum vector length = 511 Memory required = 2573 / 215198 wR2 = 0.0813 before cycle 9 for 3063 data and 173 / 173 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0193 * P )^2 + 2.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.15095 0.00023 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C11 Max. dU = 0.000 for C4 Least-squares cycle 10 Maximum vector length = 511 Memory required = 2573 / 215198 wR2 = 0.0813 before cycle 10 for 3063 data and 173 / 173 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0193 * P )^2 + 2.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.15095 0.00023 0.001 OSF Mean shift/su = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for C10 Max. dU = 0.000 for C3 Least-squares cycle 11 Maximum vector length = 511 Memory required = 2573 / 215198 wR2 = 0.0813 before cycle 11 for 3063 data and 173 / 173 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0193 * P )^2 + 2.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.15095 0.00023 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C9 Max. dU = 0.000 for C16 Least-squares cycle 12 Maximum vector length = 511 Memory required = 2573 / 215198 wR2 = 0.0813 before cycle 12 for 3063 data and 173 / 173 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0193 * P )^2 + 2.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.15095 0.00023 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H16A Max. dU = 0.000 for C14 Least-squares cycle 13 Maximum vector length = 511 Memory required = 2573 / 215198 wR2 = 0.0813 before cycle 13 for 3063 data and 173 / 173 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0193 * P )^2 + 2.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.15095 0.00023 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C10 Max. dU = 0.000 for C13 Least-squares cycle 14 Maximum vector length = 511 Memory required = 2573 / 215198 wR2 = 0.0813 before cycle 14 for 3063 data and 173 / 173 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0193 * P )^2 + 2.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.15095 0.00023 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H16A Max. dU = 0.000 for C6 Least-squares cycle 15 Maximum vector length = 511 Memory required = 2573 / 215198 wR2 = 0.0813 before cycle 15 for 3063 data and 173 / 173 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0193 * P )^2 + 2.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.15095 0.00023 -0.001 OSF Mean shift/su = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for C6 Max. dU = 0.000 for C14 Least-squares cycle 16 Maximum vector length = 511 Memory required = 2573 / 215198 wR2 = 0.0813 before cycle 16 for 3063 data and 173 / 173 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0193 * P )^2 + 2.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.15095 0.00023 0.001 OSF Mean shift/su = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for C10 Max. dU = 0.000 for C16 Least-squares cycle 17 Maximum vector length = 511 Memory required = 2573 / 215198 wR2 = 0.0813 before cycle 17 for 3063 data and 173 / 173 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0193 * P )^2 + 2.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.15095 0.00023 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C11 Max. dU = 0.000 for C8 Least-squares cycle 18 Maximum vector length = 511 Memory required = 2573 / 215198 wR2 = 0.0813 before cycle 18 for 3063 data and 173 / 173 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0193 * P )^2 + 2.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.15095 0.00023 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H16C Max. dU = 0.000 for C14 Least-squares cycle 19 Maximum vector length = 511 Memory required = 2573 / 215198 wR2 = 0.0813 before cycle 19 for 3063 data and 173 / 173 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0193 * P )^2 + 2.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.15095 0.00023 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H16B Max. dU = 0.000 for C2 Least-squares cycle 20 Maximum vector length = 511 Memory required = 2573 / 215198 wR2 = 0.0813 before cycle 20 for 3063 data and 173 / 173 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0193 * P )^2 + 2.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.15095 0.00023 0.001 OSF Mean shift/su = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H16A Max. dU = 0.000 for C16 Largest correlation matrix elements 0.538 U22 Fe1 / OSF 0.536 U33 Fe1 / OSF 0.534 U11 Fe1 / OSF Idealized hydrogen atom generation before cycle 21 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C2 ** H2 0.3800 -0.3320 0.1107 43 0.950 0.000 C2 C3 C1 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C3 ** H3 0.4688 -0.2015 0.0260 43 0.950 0.000 C3 C2 C4 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C4 ** H4 0.5586 0.0247 0.0796 43 0.950 0.000 C4 C5 C3 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C5 ** H5 0.5251 0.0367 0.1973 43 0.950 0.000 C5 C4 C1 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C6 ** H6 0.2796 0.1153 0.1824 43 0.950 0.000 C6 C7 C10 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C7 ** H7 0.3880 0.3456 0.1778 43 0.950 0.000 C7 C6 C8 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C8 ** H8 0.4343 0.3650 0.0632 43 0.950 0.000 C8 C9 C7 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C9 ** H9 0.3541 0.1470 -0.0028 43 0.950 0.000 C9 C8 C10 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C10 ** H10 0.2594 -0.0107 0.0711 43 0.950 0.000 C10 C6 C9 H11 0.4508 -0.0166 0.2805 43 0.950 0.000 C11 N1 C12 H13 0.4288 0.0558 0.4050 43 0.950 0.000 C13 C12 C14 H14 0.3452 -0.0752 0.4925 43 0.950 0.000 C14 C15 C13 H15 0.2713 -0.3325 0.4458 43 0.950 0.000 C15 N2 C14 H16A 0.2544 -0.4818 0.3424 137 0.980 0.000 C16 N2 H16A H16B 0.3344 -0.4956 0.3046 137 0.980 0.000 C16 N2 H16A H16C 0.2700 -0.3534 0.2823 137 0.980 0.000 C16 N2 H16A 2010src0402a ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.43876 -0.16288 0.17727 1.00000 0.01597 0.01380 0.01742 0.00202 0.00000 0.00085 0.01573 0.00292 0.00009 0.00023 0.00008 0.00000 0.00078 0.00080 0.00081 0.00066 0.00064 0.00065 0.00034 C2 0.41931 -0.24424 0.11749 1.00000 0.01821 0.01123 0.02024 0.00056 -0.00130 0.00072 0.01656 0.00311 0.00010 0.00024 0.00008 0.00000 0.00081 0.00083 0.00087 0.00065 0.00067 0.00065 0.00036 H2 0.37998 -0.33197 0.11065 1.00000 0.01987 0.00000 0.00000 C3 0.46907 -0.17104 0.07003 1.00000 0.01955 0.01726 0.01787 -0.00034 0.00068 0.00411 0.01823 0.00309 0.00010 0.00024 0.00008 0.00000 0.00083 0.00085 0.00083 0.00070 0.00066 0.00069 0.00036 H3 0.46882 -0.20150 0.02604 1.00000 0.02187 0.00000 0.00000 C4 0.51938 -0.04390 0.10011 1.00000 0.01485 0.01927 0.01918 0.00176 0.00196 0.00046 0.01777 0.00316 0.00010 0.00024 0.00009 0.00000 0.00081 0.00092 0.00083 0.00069 0.00068 0.00066 0.00036 H4 0.55858 0.02473 0.07958 1.00000 0.02132 0.00000 0.00000 C5 0.50083 -0.03741 0.16613 1.00000 0.01551 0.01705 0.01693 0.00104 -0.00181 -0.00021 0.01650 0.00302 0.00010 0.00023 0.00008 0.00000 0.00079 0.00088 0.00082 0.00066 0.00065 0.00065 0.00035 H5 0.52514 0.03665 0.19728 1.00000 0.01980 0.00000 0.00000 C6 0.30767 0.14915 0.14534 1.00000 0.02787 0.03172 0.02471 0.00670 0.00900 0.01290 0.02810 0.00388 0.00011 0.00029 0.00010 0.00000 0.00098 0.00109 0.00098 0.00085 0.00079 0.00086 0.00044 H6 0.27962 0.11534 0.18238 1.00000 0.03372 0.00000 0.00000 C7 0.36820 0.27821 0.14280 1.00000 0.03705 0.02029 0.02402 -0.00383 -0.00303 0.01101 0.02712 0.00367 0.00012 0.00026 0.00009 0.00000 0.00109 0.00095 0.00095 0.00078 0.00082 0.00083 0.00043 H7 0.38798 0.34556 0.17778 1.00000 0.03255 0.00000 0.00000 C8 0.39412 0.28916 0.07864 1.00000 0.02447 0.01337 0.03114 0.00400 0.00114 0.00290 0.02299 0.00342 0.00011 0.00025 0.00010 0.00000 0.00089 0.00087 0.00102 0.00077 0.00078 0.00070 0.00039 H8 0.43431 0.36503 0.06319 1.00000 0.02759 0.00000 0.00000 C9 0.34934 0.16674 0.04174 1.00000 0.02377 0.02176 0.01942 0.00380 0.00009 0.00734 0.02165 0.00334 0.00010 0.00026 0.00009 0.00000 0.00090 0.00093 0.00084 0.00074 0.00071 0.00074 0.00038 H9 0.35412 0.14696 -0.00281 1.00000 0.02598 0.00000 0.00000 C10 0.29610 0.07888 0.08302 1.00000 0.01476 0.02429 0.03357 0.00568 -0.00145 0.00325 0.02421 0.00356 0.00010 0.00028 0.00010 0.00000 0.00083 0.00096 0.00106 0.00085 0.00076 0.00072 0.00041 H10 0.25940 -0.01069 0.07109 1.00000 0.02905 0.00000 0.00000 C11 0.41489 -0.11345 0.28438 1.00000 0.01526 0.01469 0.02083 0.00365 0.00042 -0.00012 0.01692 0.00307 0.00009 0.00024 0.00008 0.00000 0.00077 0.00085 0.00088 0.00070 0.00065 0.00065 0.00036 H11 0.45078 -0.01657 0.28051 1.00000 0.02031 0.00000 0.00000 C12 0.38089 -0.14424 0.34604 1.00000 0.01322 0.01666 0.01792 0.00211 -0.00036 0.00127 0.01593 0.00295 0.00009 0.00023 0.00008 0.00000 0.00075 0.00084 0.00083 0.00068 0.00064 0.00065 0.00034 C13 0.39441 -0.04393 0.40098 1.00000 0.01852 0.01897 0.02266 -0.00184 -0.00098 -0.00034 0.02005 0.00325 0.00011 0.00025 0.00009 0.00000 0.00084 0.00096 0.00090 0.00073 0.00073 0.00069 0.00038 H13 0.42885 0.05580 0.40495 1.00000 0.02406 0.00000 0.00000 C14 0.34796 -0.11654 0.44967 1.00000 0.02144 0.02586 0.01680 -0.00137 -0.00050 0.00611 0.02137 0.00326 0.00010 0.00026 0.00009 0.00000 0.00089 0.00099 0.00083 0.00072 0.00069 0.00075 0.00039 H14 0.34520 -0.07519 0.49248 1.00000 0.02564 0.00000 0.00000 C15 0.30731 -0.25852 0.42365 1.00000 0.01818 0.02457 0.01697 0.00491 0.00346 0.00279 0.01990 0.00326 0.00010 0.00026 0.00008 0.00000 0.00081 0.00094 0.00084 0.00073 0.00067 0.00072 0.00037 H15 0.27126 -0.33249 0.44577 1.00000 0.02389 0.00000 0.00000 C16 0.29377 -0.41293 0.31915 1.00000 0.02595 0.03171 0.02363 -0.00336 0.00281 -0.01295 0.02710 0.00324 0.00011 0.00029 0.00009 0.00000 0.00098 0.00111 0.00097 0.00084 0.00077 0.00084 0.00044 H16A 0.25444 -0.48184 0.34241 1.00000 0.04065 0.00000 0.00000 H16B 0.33442 -0.49561 0.30460 1.00000 0.04065 0.00000 0.00000 H16C 0.27003 -0.35344 0.28226 1.00000 0.04065 0.00000 0.00000 N1 0.40033 -0.20698 0.23436 1.00000 0.01832 0.01688 0.01705 0.00329 -0.00073 -0.00097 0.01742 0.00252 0.00008 0.00021 0.00007 0.00000 0.00070 0.00075 0.00073 0.00060 0.00056 0.00057 0.00031 N2 0.32697 -0.27644 0.36089 1.00000 0.01487 0.01801 0.01716 0.00134 0.00053 -0.00071 0.01668 0.00250 0.00008 0.00020 0.00007 0.00000 0.00067 0.00074 0.00072 0.00059 0.00055 0.00056 0.00031 Fe1 0.40679 0.03103 0.11237 1.00000 0.01443 0.01152 0.01456 0.00097 0.00040 0.00059 0.01350 0.00042 0.00001 0.00003 0.00001 0.00000 0.00015 0.00016 0.00015 0.00009 0.00009 0.00009 0.00010 Final Structure Factor Calculation for 2010src0402a Total number of l.s. parameters = 173 Maximum vector length = 511 Memory required = 2400 / 22995 wR2 = 0.0813 before cycle 21 for 3063 data and 0 / 173 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0193 * P )^2 + 2.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0328 for 2709 Fo > 4sig(Fo) and 0.0386 for all 3063 data wR2 = 0.0813, GooF = S = 1.068, Restrained GooF = 1.068 for all data Occupancy sum of asymmetric unit = 19.00 for non-hydrogen and 16.00 for hydrogen atoms Principal mean square atomic displacements U 0.0184 0.0161 0.0127 C1 0.0209 0.0177 0.0111 C2 0.0227 0.0180 0.0140 C3 0.0214 0.0178 0.0141 C4 0.0187 0.0165 0.0142 C5 0.0480 0.0208 0.0155 C6 0.0435 0.0235 0.0143 C7 0.0324 0.0246 0.0120 C8 0.0308 0.0203 0.0138 C9 0.0363 0.0231 0.0132 C10 0.0225 0.0153 0.0130 C11 0.0195 0.0157 0.0126 C12 0.0235 0.0190 0.0176 C13 0.0303 0.0174 0.0165 C14 0.0286 0.0176 0.0135 C15 0.0431 0.0226 0.0156 C16 0.0208 0.0178 0.0137 N1 0.0190 0.0166 0.0144 N2 0.0152 0.0141 0.0112 Fe1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.017 0.033 0.051 0.071 0.096 0.125 0.159 0.211 0.287 1.000 Number in group 308. 326. 296. 301. 310. 302. 300. 306. 305. 309. GooF 1.082 1.039 1.142 1.174 1.125 0.967 0.966 1.017 0.987 1.155 K 1.473 0.985 0.965 0.968 0.973 0.985 1.003 1.016 1.019 0.997 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.64 inf Number in group 311. 304. 309. 301. 309. 304. 309. 308. 299. 309. GooF 1.000 0.993 0.967 1.015 0.878 0.905 0.903 0.911 1.285 1.604 K 0.984 1.005 1.026 1.019 1.013 1.018 1.020 1.017 1.009 0.979 R1 0.075 0.069 0.059 0.050 0.037 0.033 0.028 0.025 0.027 0.029 Recommended weighting scheme: WGHT 0.0190 2.5203 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) 6 3 4 2286.15 1814.48 4.95 0.205 1.76 4 0 10 85.25 197.84 4.53 0.068 1.89 5 0 8 130.87 61.47 4.13 0.038 2.09 8 3 1 3959.55 4601.34 4.03 0.327 1.62 0 2 24 59.03 141.34 3.63 0.057 0.85 1 1 14 230.43 146.70 3.55 0.058 1.46 5 2 9 6374.40 5601.36 3.53 0.361 1.71 6 2 9 79.24 35.16 3.52 0.029 1.63 12 0 2 60.54 22.35 3.46 0.023 1.43 5 1 10 205.07 126.10 3.43 0.054 1.74 0 4 3 2491.34 2944.02 3.42 0.262 1.78 1 4 4 37.73 6.87 3.32 0.013 1.73 9 4 17 636.73 847.72 3.23 0.140 0.91 10 0 2 1366.23 1130.85 3.22 0.162 1.71 8 0 2 142.10 84.04 3.18 0.044 2.12 1 1 12 867.00 701.82 3.14 0.128 1.69 10 3 0 4825.28 4249.56 3.13 0.314 1.42 5 1 3 1612.48 1357.12 3.12 0.178 2.86 6 3 0 4416.70 3791.03 3.10 0.297 1.87 3 2 8 36.43 11.54 3.10 0.016 2.00 8 2 7 207.17 137.62 3.10 0.057 1.58 17 1 14 7.57 58.32 3.09 0.037 0.84 10 1 0 1792.46 1512.17 3.09 0.188 1.69 7 3 23 165.32 263.48 3.08 0.078 0.81 2 2 26 -8.69 20.09 3.06 0.022 0.79 3 0 10 5129.26 5846.25 3.05 0.369 1.97 0 0 12 265.76 371.24 3.04 0.093 1.75 3 3 6 447.10 341.65 3.02 0.089 1.90 4 3 4 596.27 738.33 3.00 0.131 1.98 9 1 22 78.76 151.98 2.99 0.059 0.85 3 2 2 119.43 67.89 2.98 0.040 2.98 17 4 4 232.88 328.78 2.90 0.087 0.88 5 4 17 264.61 369.63 2.86 0.093 0.98 3 1 11 364.86 275.09 2.85 0.080 1.76 8 4 1 141.96 89.72 2.85 0.046 1.40 7 1 2 201.83 139.39 2.83 0.057 2.29 6 1 12 45.76 18.12 2.82 0.021 1.47 8 2 1 2792.59 2468.43 2.78 0.240 1.86 1 4 11 112.26 66.99 2.77 0.039 1.32 1 1 3 14154.24 15786.51 2.75 0.606 4.87 6 6 2 19.72 1.17 2.74 0.005 1.12 3 4 18 23.19 0.20 2.73 0.002 0.97 2 7 13 109.34 180.12 2.68 0.065 0.88 2 1 8 16.00 1.77 2.66 0.006 2.38 9 4 11 -2.35 13.48 2.64 0.018 1.09 11 2 1 39.14 14.56 2.64 0.018 1.44 12 3 9 77.11 126.66 2.63 0.054 1.10 3 2 6 12498.51 13677.25 2.61 0.564 2.32 6 2 13 282.48 211.68 2.60 0.070 1.32 13 1 2 1490.26 1293.10 2.59 0.173 1.30 Bond lengths and angles C1 - Distance Angles N1 1.4089 (0.0021) C2 1.4306 (0.0024) 122.55 (0.15) C5 1.4371 (0.0023) 129.82 (0.15) 107.64 (0.15) Fe1 2.0498 (0.0017) 126.73 (0.12) 69.23 (0.10) 69.28 (0.10) C1 - N1 C2 C5 C2 - Distance Angles C3 1.4235 (0.0024) C1 1.4306 (0.0024) 108.21 (0.15) Fe1 2.0417 (0.0018) 69.60 (0.10) 69.84 (0.10) H2 0.9500 125.90 125.90 126.24 C2 - C3 C1 Fe1 C3 - Distance Angles C2 1.4235 (0.0024) C4 1.4268 (0.0025) 107.99 (0.15) Fe1 2.0419 (0.0017) 69.59 (0.10) 69.63 (0.10) H3 0.9500 126.00 126.00 126.34 C3 - C2 C4 Fe1 C4 - Distance Angles C5 1.4232 (0.0024) C3 1.4268 (0.0025) 108.35 (0.15) Fe1 2.0438 (0.0018) 69.68 (0.10) 69.49 (0.10) H4 0.9500 125.82 125.82 126.58 C4 - C5 C3 Fe1 C5 - Distance Angles C4 1.4232 (0.0024) C1 1.4371 (0.0023) 107.81 (0.15) Fe1 2.0452 (0.0017) 69.58 (0.10) 69.63 (0.10) H5 0.9500 126.10 126.10 126.27 C5 - C4 C1 Fe1 C6 - Distance Angles C7 1.4164 (0.0030) C10 1.4210 (0.0030) 108.31 (0.17) Fe1 2.0459 (0.0019) 69.57 (0.11) 69.65 (0.10) H6 0.9500 125.85 125.85 126.51 C6 - C7 C10 Fe1 C7 - Distance Angles C6 1.4164 (0.0030) C8 1.4219 (0.0028) 107.92 (0.18) Fe1 2.0419 (0.0019) 69.88 (0.11) 69.56 (0.11) H7 0.9500 126.04 126.04 126.09 C7 - C6 C8 Fe1 C8 - Distance Angles C9 1.4195 (0.0027) C7 1.4219 (0.0028) 107.94 (0.17) Fe1 2.0405 (0.0018) 69.90 (0.10) 69.67 (0.11) H8 0.9500 126.03 126.03 125.98 C8 - C9 C7 Fe1 C9 - Distance Angles C8 1.4195 (0.0027) C10 1.4213 (0.0026) 108.14 (0.17) Fe1 2.0464 (0.0018) 69.45 (0.10) 69.63 (0.10) H9 0.9500 125.93 125.93 126.57 C9 - C8 C10 Fe1 C10 - Distance Angles C6 1.4210 (0.0030) C9 1.4213 (0.0026) 107.69 (0.18) Fe1 2.0451 (0.0018) 69.70 (0.11) 69.72 (0.10) H10 0.9500 126.16 126.16 125.99 C10 - C6 C9 Fe1 C11 - Distance Angles N1 1.2808 (0.0023) C12 1.4399 (0.0024) 124.85 (0.16) H11 0.9500 117.57 117.57 C11 - N1 C12 C12 - Distance Angles N2 1.3850 (0.0022) C13 1.3894 (0.0025) 107.51 (0.15) C11 1.4399 (0.0024) 126.08 (0.16) 126.39 (0.16) C12 - N2 C13 C13 - Distance Angles C12 1.3894 (0.0025) C14 1.4064 (0.0027) 107.72 (0.16) H13 0.9500 126.14 126.14 C13 - C12 C14 C14 - Distance Angles C15 1.3739 (0.0027) C13 1.4064 (0.0027) 107.10 (0.16) H14 0.9500 126.45 126.45 C14 - C15 C13 C15 - Distance Angles N2 1.3671 (0.0022) C14 1.3739 (0.0027) 109.19 (0.16) H15 0.9500 125.41 125.41 C15 - N2 C14 C16 - Distance Angles N2 1.4522 (0.0024) H16A 0.9800 109.47 H16B 0.9800 109.47 109.47 H16C 0.9800 109.47 109.47 109.47 C16 - N2 H16A H16B N1 - Distance Angles C11 1.2808 (0.0023) C1 1.4089 (0.0021) 118.69 (0.15) N1 - C11 N2 - Distance Angles C15 1.3671 (0.0022) C12 1.3850 (0.0022) 108.48 (0.14) C16 1.4522 (0.0024) 123.33 (0.15) 128.18 (0.15) N2 - C15 C12 Fe1 - Distance Angles C8 2.0405 (0.0018) C2 2.0417 (0.0018) 162.71 (0.08) C3 2.0419 (0.0017) 125.80 (0.08) 40.80 (0.07) C7 2.0419 (0.0019) 40.77 (0.08) 154.64 (0.08) 163.55 (0.08) C4 2.0438 (0.0018) 108.10 (0.07) 68.72 (0.07) 40.88 (0.07) 126.35 (0.08) C10 2.0451 (0.0018) 68.53 (0.08) 106.66 (0.08) 119.35 (0.08) 68.50 (0.08) 154.67 (0.08) C5 2.0452 (0.0017) 120.45 (0.07) 68.99 (0.07) 68.86 (0.07) 107.95 (0.08) 40.74 (0.07) 162.92 (0.08) C6 2.0459 (0.0019) 68.34 (0.08) 119.58 (0.08) 154.27 (0.08) 40.55 (0.09) 163.49 (0.08) 40.65 (0.08) 125.95 (0.08) C9 2.0464 (0.0018) 40.65 (0.08) 125.09 (0.07) 107.33 (0.07) 68.40 (0.08) 120.34 (0.07) 40.65 (0.07) 155.19 (0.07) C1 2.0498 (0.0017) 155.33 (0.08) 40.93 (0.07) 68.81 (0.07) 120.12 (0.07) 68.75 (0.07) 125.01 (0.07) 41.09 (0.07) Fe1 - C8 C2 C3 C7 C4 C10 C5 FMAP and GRID set by program FMAP 2 1 22 GRID -1.316 -2 -1 1.316 2 1 R1 = 0.0377 for 3063 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.31 at 0.1206 0.7816 0.1115 [ 0.69 A from C7 ] Deepest hole -0.49 at 0.0811 0.4642 0.0925 [ 0.68 A from FE1 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 2633 / 26000 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3794 0.2816 0.1115 1.00000 0.05 0.31 0.69 C7 0.74 C8 1.48 H7 1.52 H8 Q2 1 0.4764 -0.1495 0.1723 1.00000 0.05 0.31 0.67 C1 0.94 C5 1.67 C2 1.69 H5 Q3 1 0.5048 -0.1400 0.0877 1.00000 0.05 0.31 0.76 C3 0.80 C4 1.51 H3 1.54 H4 Q4 1 0.4289 -0.2063 0.1483 1.00000 0.05 0.30 0.71 C1 0.72 C2 1.48 H2 1.80 C5 Q5 1 0.4069 -0.0997 0.1125 1.00000 0.05 0.30 0.96 FE1 1.09 C2 1.49 C3 1.54 C1 Shortest distances between peaks (including symmetry equivalents) 2 4 1.05 4 5 1.15 2 5 1.78 3 5 1.80 2 3 1.84 3 4 1.89 1 5 2.85 Time profile in seconds ----------------------- 0.02: 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. 0.77: 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 0.02: Generate idealized H-atoms 2.55: Structure factors and derivatives 2.02: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.36: Solve l.s. equations 0.00: Generate HTAB table 0.09: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2010src0402a finished at 20:15:26 Total CPU time: 6.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++