+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src0866 started at 11:37:06 on 11-Jul-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src0866 in P2(1)/m CELL 0.71073 6.5148 11.4581 6.8511 90.000 111.601 90.000 ZERR 2.00 0.0003 0.0005 0.0002 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, - Z SFAC C H N FE UNIT 24 16 4 2 V = 475.50 F(000) = 240.0 Mu = 1.54 mm-1 Cell Wt = 472.11 Rho = 1.649 MERG 2 OMIT -3.00 55.00 EXTI 0.32250 SHEL 7 0.77 ACTA FMAP 2 PLAN 5 SIZE 0.07 0.13 0.20 BOND $H WGHT 0.07590 L.S. 20 TEMP -153.00 FVAR 1.69686 C1 1 0.707587 0.112598 0.787690 11.00000 0.02257 0.01754 = 0.01941 0.00302 0.01129 0.00343 C2 1 0.896696 0.186611 0.828423 11.00000 0.02013 0.01945 = 0.01355 0.00255 0.00668 0.00106 C3 1 1.120303 0.148911 0.879292 11.00000 0.02104 0.02514 = 0.01299 0.00449 0.00486 0.00541 AFIX 43 H3 2 1.169760 0.070340 0.889667 11.00000 -1.20000 AFIX 0 C4 1 1.254346 0.250000 0.911326 10.50000 0.01856 0.03697 = 0.01146 0.00000 0.00253 0.00000 AFIX 43 H4 2 1.409959 0.250000 0.948516 10.50000 -1.20000 AFIX 0 C5 1 0.814441 0.187788 0.322116 11.00000 0.02378 0.02644 = 0.01142 -0.00383 0.00331 -0.00627 AFIX 43 H5 2 0.688774 0.138919 0.292387 11.00000 -1.20000 AFIX 0 C6 1 1.037625 0.149665 0.374916 11.00000 0.03177 0.02492 = 0.01644 -0.00237 0.00964 0.00405 AFIX 43 H6 2 1.085790 0.070832 0.386154 11.00000 -1.20000 AFIX 0 C7 1 1.175138 0.250000 0.407723 10.50000 0.02289 0.03736 = 0.01614 0.00000 0.00962 0.00000 AFIX 43 H7 2 1.330742 0.250000 0.444847 10.50000 -1.20000 AFIX 0 N1 3 0.559631 0.052512 0.759105 11.00000 0.02706 0.02092 = 0.03433 0.00425 0.01348 -0.00056 FE1 4 1.011692 0.250000 0.612626 10.50000 0.01494 0.01782 = 0.01125 0.00000 0.00431 0.00000 HKLF 4 Covalent radii and connectivity table for 2007src0866 in P2(1)/m C 0.770 H 0.320 N 0.700 FE 1.240 C1 - N1 C2 C2 - C3 C1 C2_$1 Fe1 C3 - C4 C2 Fe1 C4 - C3_$1 C3 Fe1 C5 - C5_$1 C6 Fe1 C6 - C7 C5 Fe1 C7 - C6 C6_$1 Fe1 N1 - C1 Fe1 - C2_$1 C2 C6 C6_$1 C7 C3_$1 C3 C5 C5_$1 C4 Operators for generating equivalent atoms: $1 x, -y+1/2, z 6221 Reflections read, of which 22 rejected -8 =< h =< 8, -14 =< k =< 14, -8 =< l =< 8, Max. 2-theta = 54.95 0 Systematic absence violations 0 Inconsistent equivalents 1144 Unique reflections, of which 0 suppressed R(int) = 0.0382 R(sigma) = 0.0353 Friedel opposites merged Maximum memory for data reduction = 1186 / 11175 Special position constraints for C4 y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for C7 y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for Fe1 y = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof 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 = 1398 / 101546 wR2 = 0.1296 before cycle 1 for 1144 data and 74 / 74 parameters GooF = S = 1.394; Restrained GooF = 1.394 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0759 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.69653 0.01112 -0.030 OSF 2 0.32077 0.03032 -0.057 EXTI Mean shift/esd = 0.016 Maximum = -0.057 for EXTI Max. shift = 0.000 A for N1 Max. dU = 0.000 for C4 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1398 / 101546 wR2 = 0.1295 before cycle 2 for 1144 data and 74 / 74 parameters GooF = S = 1.393; Restrained GooF = 1.393 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0759 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.69656 0.01110 0.003 OSF 2 0.32062 0.03019 -0.005 EXTI Mean shift/esd = 0.005 Maximum = -0.019 for z N1 Max. shift = 0.000 A for N1 Max. dU = 0.000 for C4 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1398 / 101546 wR2 = 0.1295 before cycle 3 for 1144 data and 74 / 74 parameters GooF = S = 1.393; Restrained GooF = 1.393 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0759 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.69660 0.01110 0.003 OSF 2 0.32064 0.03018 0.001 EXTI Mean shift/esd = 0.001 Maximum = 0.004 for U33 Fe1 Max. shift = 0.000 A for N1 Max. dU = 0.000 for C4 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1398 / 101546 wR2 = 0.1295 before cycle 4 for 1144 data and 74 / 74 parameters GooF = S = 1.393; Restrained GooF = 1.393 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0759 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.69660 0.01110 0.000 OSF 2 0.32065 0.03018 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for U33 C6 Max. shift = 0.000 A for C4 Max. dU = 0.000 for C4 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1398 / 101546 wR2 = 0.1295 before cycle 5 for 1144 data and 74 / 74 parameters GooF = S = 1.393; Restrained GooF = 1.393 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0759 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.69660 0.01110 0.000 OSF 2 0.32065 0.03018 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z Fe1 Max. shift = 0.000 A for C3 Max. dU = 0.000 for C7 Least-squares cycle 6 Maximum vector length = 511 Memory required = 1398 / 101546 wR2 = 0.1295 before cycle 6 for 1144 data and 74 / 74 parameters GooF = S = 1.393; Restrained GooF = 1.393 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0759 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.69660 0.01110 0.000 OSF 2 0.32065 0.03018 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x Fe1 Max. shift = 0.000 A for N1 Max. dU = 0.000 for C7 Least-squares cycle 7 Maximum vector length = 511 Memory required = 1398 / 101546 wR2 = 0.1295 before cycle 7 for 1144 data and 74 / 74 parameters GooF = S = 1.393; Restrained GooF = 1.393 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0759 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.69660 0.01110 0.000 OSF 2 0.32065 0.03018 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x Fe1 Max. shift = 0.000 A for C3 Max. dU = 0.000 for C1 Least-squares cycle 8 Maximum vector length = 511 Memory required = 1398 / 101546 wR2 = 0.1295 before cycle 8 for 1144 data and 74 / 74 parameters GooF = S = 1.393; Restrained GooF = 1.393 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0759 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.69660 0.01110 0.000 OSF 2 0.32065 0.03018 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x Fe1 Max. shift = 0.000 A for N1 Max. dU = 0.000 for C4 Least-squares cycle 9 Maximum vector length = 511 Memory required = 1398 / 101546 wR2 = 0.1295 before cycle 9 for 1144 data and 74 / 74 parameters GooF = S = 1.393; Restrained GooF = 1.393 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0759 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.69660 0.01110 0.000 OSF 2 0.32065 0.03018 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x Fe1 Max. shift = 0.000 A for C4 Max. dU = 0.000 for C7 Least-squares cycle 10 Maximum vector length = 511 Memory required = 1398 / 101546 wR2 = 0.1295 before cycle 10 for 1144 data and 74 / 74 parameters GooF = S = 1.393; Restrained GooF = 1.393 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0759 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.69660 0.01110 0.000 OSF 2 0.32065 0.03018 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x Fe1 Max. shift = 0.000 A for C3 Max. dU = 0.000 for C7 Least-squares cycle 11 Maximum vector length = 511 Memory required = 1398 / 101546 wR2 = 0.1295 before cycle 11 for 1144 data and 74 / 74 parameters GooF = S = 1.393; Restrained GooF = 1.393 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0759 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.69660 0.01110 0.000 OSF 2 0.32065 0.03018 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x Fe1 Max. shift = 0.000 A for C2 Max. dU = 0.000 for C5 Least-squares cycle 12 Maximum vector length = 511 Memory required = 1398 / 101546 wR2 = 0.1295 before cycle 12 for 1144 data and 74 / 74 parameters GooF = S = 1.393; Restrained GooF = 1.393 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0759 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.69660 0.01110 0.000 OSF 2 0.32065 0.03018 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x Fe1 Max. shift = 0.000 A for C7 Max. dU = 0.000 for C7 Least-squares cycle 13 Maximum vector length = 511 Memory required = 1398 / 101546 wR2 = 0.1295 before cycle 13 for 1144 data and 74 / 74 parameters GooF = S = 1.393; Restrained GooF = 1.393 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0759 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.69660 0.01110 0.000 OSF 2 0.32065 0.03018 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x Fe1 Max. shift = 0.000 A for C1 Max. dU = 0.000 for C7 Least-squares cycle 14 Maximum vector length = 511 Memory required = 1398 / 101546 wR2 = 0.1295 before cycle 14 for 1144 data and 74 / 74 parameters GooF = S = 1.393; Restrained GooF = 1.393 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0759 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.69660 0.01110 0.000 OSF 2 0.32065 0.03018 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x Fe1 Max. shift = 0.000 A for C1 Max. dU = 0.000 for C7 Least-squares cycle 15 Maximum vector length = 511 Memory required = 1398 / 101546 wR2 = 0.1295 before cycle 15 for 1144 data and 74 / 74 parameters GooF = S = 1.393; Restrained GooF = 1.393 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0759 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.69660 0.01110 0.000 OSF 2 0.32065 0.03018 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x Fe1 Max. shift = 0.000 A for C7 Max. dU = 0.000 for C7 Least-squares cycle 16 Maximum vector length = 511 Memory required = 1398 / 101546 wR2 = 0.1295 before cycle 16 for 1144 data and 74 / 74 parameters GooF = S = 1.393; Restrained GooF = 1.393 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0759 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.69660 0.01110 0.000 OSF 2 0.32065 0.03018 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x Fe1 Max. shift = 0.000 A for C1 Max. dU = 0.000 for C6 Least-squares cycle 17 Maximum vector length = 511 Memory required = 1398 / 101546 wR2 = 0.1295 before cycle 17 for 1144 data and 74 / 74 parameters GooF = S = 1.393; Restrained GooF = 1.393 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0759 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.69660 0.01110 0.000 OSF 2 0.32065 0.03018 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x Fe1 Max. shift = 0.000 A for C1 Max. dU = 0.000 for C2 Least-squares cycle 18 Maximum vector length = 511 Memory required = 1398 / 101546 wR2 = 0.1295 before cycle 18 for 1144 data and 74 / 74 parameters GooF = S = 1.393; Restrained GooF = 1.393 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0759 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.69660 0.01110 0.000 OSF 2 0.32065 0.03018 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x Fe1 Max. shift = 0.000 A for C7 Max. dU = 0.000 for C4 Least-squares cycle 19 Maximum vector length = 511 Memory required = 1398 / 101546 wR2 = 0.1295 before cycle 19 for 1144 data and 74 / 74 parameters GooF = S = 1.393; Restrained GooF = 1.393 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0759 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.69660 0.01110 0.000 OSF 2 0.32065 0.03018 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x Fe1 Max. shift = 0.000 A for C1 Max. dU = 0.000 for C6 Least-squares cycle 20 Maximum vector length = 511 Memory required = 1398 / 101546 wR2 = 0.1295 before cycle 20 for 1144 data and 74 / 74 parameters GooF = S = 1.393; Restrained GooF = 1.393 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0759 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.69660 0.01110 0.000 OSF 2 0.32065 0.03018 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x Fe1 Max. shift = 0.000 A for C1 Max. dU = 0.000 for C6 Largest correlation matrix elements 0.729 EXTI / OSF 0.562 U13 Fe1 / U33 Fe1 0.544 U13 C6 / U33 C6 0.719 U22 Fe1 / OSF 0.556 U13 C1 / U11 C1 0.517 U13 C6 / U11 C6 0.708 U33 Fe1 / OSF 0.553 U13 C2 / U11 C2 0.512 z C1 / x C1 0.701 U11 Fe1 / OSF 0.553 U13 C7 / U11 C7 0.501 U13 C1 / U33 C1 0.611 U13 Fe1 / U11 Fe1 0.549 U13 N1 / U11 N1 0.500 U13 N1 / U33 N1 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 C3 ** H3 1.1698 0.0703 0.8897 43 0.950 0.000 C3 C4 C2 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C4 ** H4 1.4100 0.2500 0.9485 43 0.950 0.000 C4 C3_$1 C3 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C5 ** H5 0.6888 0.1389 0.2924 43 0.950 0.000 C5 C5_$1 C6 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C6 ** H6 1.0858 0.0708 0.3862 43 0.950 0.000 C6 C7 C5 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C7 ** H7 1.3308 0.2500 0.4449 43 0.950 0.000 C7 C6 C6_$1 2007src0866 in P2(1)/m ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.70758 0.11260 0.78768 1.00000 0.02255 0.01753 0.01946 0.00300 0.01131 0.00340 0.01883 0.00533 0.00042 0.00022 0.00037 0.00000 0.00129 0.00118 0.00122 0.00090 0.00102 0.00099 0.00056 C2 0.89669 0.18661 0.82841 1.00000 0.02014 0.01945 0.01362 0.00256 0.00670 0.00105 0.01760 0.00505 0.00042 0.00021 0.00037 0.00000 0.00131 0.00133 0.00111 0.00092 0.00100 0.00096 0.00055 C3 1.12030 0.14891 0.87929 1.00000 0.02101 0.02517 0.01299 0.00450 0.00485 0.00538 0.02013 0.00546 0.00043 0.00025 0.00037 0.00000 0.00134 0.00134 0.00110 0.00091 0.00099 0.00098 0.00058 H3 1.16976 0.07034 0.88967 1.00000 0.02415 0.00000 0.00000 C4 1.25436 0.25000 0.91134 0.50000 0.01866 0.03698 0.01147 0.00000 0.00255 0.00000 0.02322 0.00662 0.00064 0.00000 0.00055 0.00000 0.00178 0.00213 0.00153 0.00000 0.00136 0.00000 0.00081 H4 1.40997 0.25000 0.94853 0.50000 0.02786 0.00000 0.00000 C5 0.81442 0.18779 0.32212 1.00000 0.02384 0.02641 0.01140 -0.00383 0.00331 -0.00620 0.02145 0.00512 0.00046 0.00024 0.00036 0.00000 0.00136 0.00147 0.00112 0.00097 0.00100 0.00106 0.00059 H5 0.68876 0.13892 0.29239 1.00000 0.02574 0.00000 0.00000 C6 1.03762 0.14967 0.37492 1.00000 0.03179 0.02496 0.01645 -0.00239 0.00965 0.00399 0.02418 0.00584 0.00051 0.00025 0.00040 0.00000 0.00146 0.00143 0.00121 0.00099 0.00110 0.00118 0.00061 H6 1.08579 0.07083 0.38616 1.00000 0.02902 0.00000 0.00000 C7 1.17515 0.25000 0.40773 0.50000 0.02299 0.03730 0.01611 0.00000 0.00963 0.00000 0.02478 0.00731 0.00069 0.00000 0.00059 0.00000 0.00187 0.00226 0.00167 0.00000 0.00147 0.00000 0.00084 H7 1.33075 0.25000 0.44486 0.50000 0.02973 0.00000 0.00000 N1 0.55961 0.05251 0.75908 1.00000 0.02712 0.02087 0.03434 0.00426 0.01351 -0.00055 0.02682 0.00502 0.00041 0.00019 0.00037 0.00000 0.00130 0.00114 0.00131 0.00094 0.00107 0.00096 0.00056 Fe1 1.01170 0.25000 0.61263 0.50000 0.01494 0.01781 0.01125 0.00000 0.00431 0.00000 0.01481 0.00076 0.00007 0.00000 0.00006 0.00000 0.00040 0.00039 0.00038 0.00000 0.00024 0.00000 0.00030 Final Structure Factor Calculation for 2007src0866 in P2(1)/m Total number of l.s. parameters = 74 Maximum vector length = 511 Memory required = 1324 / 22995 wR2 = 0.1295 before cycle 21 for 1144 data and 0 / 74 parameters GooF = S = 1.393; Restrained GooF = 1.393 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0759 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0470 for 1076 Fo > 4sig(Fo) and 0.0518 for all 1144 data wR2 = 0.1295, GooF = S = 1.393, Restrained GooF = 1.393 for all data Occupancy sum of asymmetric unit = 7.50 for non-hydrogen and 4.00 for hydrogen atoms Principal mean square atomic displacements U 0.0258 0.0159 0.0149 C1 0.0210 0.0195 0.0123 C2 0.0289 0.0201 0.0114 C3 0.0370 0.0215 0.0111 C4 0.0318 0.0223 0.0102 C5 0.0344 0.0240 0.0142 C6 0.0373 0.0232 0.0139 C7 0.0356 0.0262 0.0187 N1 0.0178 0.0154 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 0.034 0.064 0.089 0.115 0.136 0.160 0.190 0.223 0.283 1.000 Number in group 117. 114. 115. 120. 108. 119. 115. 107. 114. 115. GooF 1.469 1.150 1.114 1.066 0.797 0.718 0.767 0.686 0.812 3.247 K 2.073 1.003 0.958 0.979 0.988 1.004 1.001 1.001 1.033 1.059 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.16 1.32 1.67 inf Number in group 118. 115. 111. 120. 108. 115. 113. 115. 114. 115. GooF 1.002 0.999 0.774 0.915 1.019 0.841 0.832 0.942 1.192 3.340 K 0.994 1.048 1.016 1.005 1.048 1.020 1.032 1.030 1.076 1.022 R1 0.058 0.061 0.040 0.032 0.044 0.028 0.026 0.029 0.041 0.108 Recommended weighting scheme: WGHT 0.0759 0.0000 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 0 0 1 -0.94 932.89 14.69 0.348 6.37 0 2 0 136.28 7700.67 14.28 1.000 5.73 1 2 0 4056.42 7627.11 4.46 0.995 4.16 0 3 1 12.47 6.71 4.17 0.030 3.28 -2 0 1 6059.02 3985.69 3.73 0.719 3.24 -1 2 1 3900.26 2716.28 3.49 0.594 3.98 1 6 0 48.78 71.80 3.35 0.097 1.82 -7 0 3 0.45 5.15 3.20 0.026 0.93 1 0 1 3175.79 2295.37 2.98 0.546 3.75 -1 0 3 3.79 6.47 2.90 0.029 2.28 -1 5 2 3262.14 2505.87 2.60 0.570 1.90 -3 4 1 43.81 60.38 2.56 0.089 1.73 -2 2 3 14.18 20.82 2.55 0.052 2.01 2 3 2 3491.03 2728.00 2.43 0.595 1.68 -8 1 5 5.09 0.13 2.41 0.004 0.79 -2 5 2 3261.28 2555.47 2.38 0.576 1.76 -1 3 1 2770.42 2175.74 2.36 0.532 3.14 0 0 2 1873.45 1458.09 2.35 0.435 3.18 0 2 4 2945.56 2325.55 2.35 0.550 1.53 -1 3 3 112.32 144.59 2.31 0.137 1.96 7 3 1 36.98 58.80 2.14 0.087 0.80 0 5 2 2904.12 2333.42 2.13 0.550 1.86 0 1 2 1303.93 1052.71 2.10 0.370 3.07 0 0 4 2420.09 1962.92 2.05 0.505 1.59 -1 10 2 1.23 3.85 2.00 0.022 1.09 -3 3 2 2413.20 1967.18 1.99 0.505 1.83 -1 1 2 1291.28 1049.89 1.99 0.369 3.24 -3 1 2 2384.07 1940.02 1.97 0.502 2.05 1 3 1 2369.72 1938.50 1.96 0.502 2.68 3 12 2 252.20 4.96 1.95 0.025 0.80 0 0 3 108.38 134.22 1.91 0.132 2.12 0 2 1 1581.55 1300.68 1.91 0.411 4.26 1 5 2 2819.31 2323.93 1.90 0.549 1.68 0 3 4 -0.01 1.54 1.87 0.014 1.47 -1 14 3 12.35 4.77 1.84 0.025 0.77 0 3 3 2453.41 2037.18 1.83 0.514 1.86 2 1 2 2247.19 1864.73 1.83 0.492 1.85 2 9 4 4.91 1.98 1.83 0.016 0.89 5 1 3 17.85 10.82 1.79 0.037 0.91 -1 5 1 10.47 13.39 1.78 0.042 2.12 -1 3 2 2311.62 1921.26 1.78 0.499 2.53 2 10 2 5.79 9.87 1.77 0.036 0.98 0 6 7 23.83 32.82 1.77 0.065 0.82 -1 8 2 33.60 41.79 1.75 0.074 1.32 -1 0 1 1396.11 1140.66 1.73 0.385 5.52 2 1 4 3.30 0.68 1.73 0.009 1.23 -4 12 3 0.75 7.18 1.72 0.031 0.81 5 0 2 -0.79 2.74 1.71 0.019 1.01 -1 2 4 2242.56 1887.03 1.71 0.495 1.63 -4 2 1 182.12 219.62 1.70 0.169 1.55 Bond lengths and angles C1 - Distance Angles N1 1.1413 (0.0035) C2 1.4359 (0.0035) 178.57 (0.28) C1 - N1 C2 - Distance Angles C3 1.4341 (0.0035) C1 1.4359 (0.0035) 126.26 (0.23) C2_$1 1.4526 (0.0049) 107.53 (0.15) 126.20 (0.14) Fe1 2.0224 (0.0024) 70.69 (0.14) 126.32 (0.18) 68.95 (0.07) C2 - C3 C1 C2_$1 C3 - Distance Angles C4 1.4183 (0.0036) C2 1.4341 (0.0035) 107.71 (0.24) Fe1 2.0563 (0.0025) 70.63 (0.18) 68.15 (0.14) H3 0.9500 126.15 126.15 126.63 C3 - C4 C2 Fe1 C4 - Distance Angles C3_$1 1.4183 (0.0036) C3 1.4183 (0.0036) 109.51 (0.34) Fe1 2.0749 (0.0037) 69.22 (0.17) 69.22 (0.17) H4 0.9500 125.24 125.24 127.95 C4 - C3_$1 C3 Fe1 C5 - Distance Angles C5_$1 1.4257 (0.0054) C6 1.4314 (0.0039) 107.77 (0.16) Fe1 2.0586 (0.0024) 69.74 (0.08) 69.31 (0.14) H5 0.9500 126.12 126.12 126.40 C5 - C5_$1 C6 Fe1 C6 - Distance Angles C7 1.4236 (0.0039) C5 1.4314 (0.0039) 108.37 (0.26) Fe1 2.0506 (0.0026) 69.69 (0.18) 69.92 (0.15) H6 0.9500 125.81 125.81 126.16 C6 - C7 C5 Fe1 C7 - Distance Angles C6 1.4236 (0.0039) C6_$1 1.4236 (0.0039) 107.72 (0.36) Fe1 2.0506 (0.0037) 69.69 (0.18) 69.69 (0.18) H7 0.9500 126.14 126.14 126.06 C7 - C6 C6_$1 Fe1 N1 - Distance Angles C1 1.1413 (0.0036) N1 - Fe1 - Distance Angles C2_$1 2.0224 (0.0024) C2 2.0224 (0.0024) 42.09 (0.14) C6 2.0506 (0.0026) 160.54 (0.12) 122.70 (0.11) C6_$1 2.0506 (0.0026) 122.70 (0.11) 160.54 (0.12) 68.20 (0.16) C7 2.0506 (0.0037) 157.81 (0.08) 157.81 (0.08) 40.62 (0.11) 40.62 (0.11) C3_$1 2.0563 (0.0025) 41.16 (0.10) 69.62 (0.10) 156.84 (0.12) 106.73 (0.11) 120.84 (0.11) C3 2.0563 (0.0025) 69.62 (0.10) 41.16 (0.10) 106.73 (0.11) 156.84 (0.12) 120.84 (0.11) 68.57 (0.15) C5 2.0586 (0.0024) 124.31 (0.11) 108.36 (0.10) 40.77 (0.11) 68.34 (0.10) 68.58 (0.13) 160.42 (0.12) 123.51 (0.11) C5_$1 2.0586 (0.0024) 108.36 (0.10) 124.31 (0.11) 68.34 (0.10) 40.77 (0.11) 68.58 (0.13) 123.51 (0.11) 160.42 (0.12) C4 2.0749 (0.0037) 68.40 (0.12) 68.40 (0.12) 121.85 (0.11) 121.85 (0.11) 106.02 (0.16) 40.15 (0.09) 40.15 (0.09) Fe1 - C2_$1 C2 C6 C6_$1 C7 C3_$1 C3 FMAP and GRID set by program FMAP 2 2 17 GRID -1.786 -2 -2 1.786 2 2 R1 = 0.0515 for 1144 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.05 at 0.0132 0.2500 0.6230 [ 0.07 A from FE1 ] Deepest hole -1.15 at 0.9655 0.2500 0.3555 [ 1.17 A from C5 ] Mean = 0.00, Rms deviation from mean = 0.31 e/A^3, Highest memory used = 1365 / 12175 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 1.0542 0.0139 1.0293 1.00000 0.05 0.81 1.56 H3 1.99 C3 1.99 H3 2.16 C1 Q2 1 1.1033 -0.0010 0.7709 1.00000 0.05 0.74 1.12 H3 1.53 H6 1.86 C3 2.02 C6 Q3 1 1.2379 0.0014 1.0710 1.00000 0.05 0.67 1.40 H3 1.53 N1 1.59 C1 2.10 C3 Q4 1 0.6851 0.0312 0.7782 1.00000 0.05 0.64 0.82 N1 0.94 C1 2.20 C2 2.42 H3 Q5 1 1.0654 0.0490 0.2206 1.00000 0.05 0.62 1.12 H6 1.62 C6 1.98 H3 2.38 C1 Shortest distances between peaks (including symmetry equivalents) 1 1 0.74 3 4 1.04 1 3 1.13 2 5 1.25 1 5 1.35 1 5 1.75 1 3 1.78 1 4 1.80 3 5 1.86 4 5 1.86 2 3 1.92 1 2 1.92 1 2 2.00 3 5 2.31 1 4 2.39 2 4 2.77 2 3 2.81 3 3 2.89 2 4 2.90 Time profile in seconds ----------------------- 0.09: 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. 1.19: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.05: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.69: Structure factors and derivatives 0.84: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.34: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src0866 finished at 11:37:15 Total CPU time: 3.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++