+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + platon started at 17:41:25 on 19-Feb-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0154 in Pbca CELL 0.71073 17.4825 7.3420 23.1152 90.000 90.000 90.000 ZERR 8.00 0.0005 0.0002 0.0007 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, - Z SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H FE N O UNIT 160 136 8 8 8 V = 2966.99 F(000) = 1424.0 Mu = 1.02 mm-1 Cell Wt = 2745.57 Rho = 1.537 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 FMAP 2 PLAN 10 SIZE 0.01 0.02 0.26 ACTA HTAB 2.00000 BOND $H WGHT 0.00000 24.75550 L.S. 6 TEMP -153.00 FVAR 0.24917 C1 1 0.323325 0.112834 0.651094 11.00000 0.02043 0.02768 = 0.01491 0.00364 -0.00088 0.00121 AFIX 137 H1A 2 0.378310 0.101210 0.658468 11.00000 -1.50000 H1B 2 0.298442 -0.005217 0.657203 11.00000 -1.50000 H1C 2 0.301415 0.202935 0.677625 11.00000 -1.50000 AFIX 0 C2 1 0.239189 0.192638 0.566793 11.00000 0.01748 0.01242 = 0.01103 -0.00157 0.00075 0.00156 C3 1 0.168220 0.157874 0.590489 11.00000 0.02548 0.01498 = 0.01530 -0.00136 0.00648 0.00263 AFIX 43 H3 2 0.163575 0.106301 0.628017 11.00000 -1.20000 AFIX 0 C4 1 0.103497 0.200422 0.557910 11.00000 0.01386 0.02327 = 0.02130 -0.00393 0.00270 0.00006 AFIX 43 H4 2 0.054156 0.174884 0.573099 11.00000 -1.20000 AFIX 0 C5 1 0.110159 0.279668 0.503528 11.00000 0.01963 0.02696 = 0.01678 -0.00353 -0.00092 -0.00118 AFIX 43 H5 2 0.065513 0.311868 0.482449 11.00000 -1.20000 AFIX 0 C6 1 0.182709 0.312185 0.479712 11.00000 0.01865 0.01588 = 0.01929 0.00172 0.00175 0.00449 AFIX 43 H6 2 0.187238 0.366830 0.442616 11.00000 -1.20000 AFIX 0 C7 1 0.247473 0.264572 0.510321 11.00000 0.01708 0.01203 = 0.01469 -0.00113 0.00073 -0.00233 C8 1 0.330281 0.286424 0.500468 11.00000 0.01711 0.01023 = 0.01355 0.00125 -0.00016 0.00232 C9 1 0.368186 0.233592 0.556148 11.00000 0.02147 0.01128 = 0.01559 -0.00108 -0.00319 0.00489 C10 1 0.374147 0.342255 0.456519 11.00000 0.01780 0.01221 = 0.01759 -0.00518 -0.00366 0.00119 AFIX 43 H10 2 0.427007 0.355616 0.465049 11.00000 -1.20000 AFIX 0 C11 1 0.352024 0.385185 0.397615 11.00000 0.01529 0.01215 = 0.01259 -0.00456 0.00745 0.00240 C12 1 0.291775 0.309636 0.363933 11.00000 0.01183 0.01602 = 0.01652 -0.00147 0.00403 0.00085 AFIX 43 H12 2 0.255959 0.221136 0.376784 11.00000 -1.20000 AFIX 0 C13 1 0.294128 0.388989 0.307626 11.00000 0.01823 0.02154 = 0.01329 -0.00034 0.00178 0.01069 AFIX 43 H13 2 0.259802 0.363153 0.276840 11.00000 -1.20000 AFIX 0 C14 1 0.356102 0.512537 0.305304 11.00000 0.02688 0.01611 = 0.01810 0.00202 0.00222 0.00685 AFIX 43 H14 2 0.370281 0.584873 0.272959 11.00000 -1.20000 AFIX 0 C15 1 0.393310 0.509366 0.359745 11.00000 0.01749 0.01609 = 0.01981 -0.00333 0.00705 -0.00054 AFIX 43 H15 2 0.437706 0.576887 0.369828 11.00000 -1.20000 AFIX 0 C16 1 0.404736 -0.021409 0.321570 11.00000 0.02339 0.00798 = 0.02039 -0.00073 0.00553 0.00203 AFIX 43 H16 2 0.370158 -0.107116 0.337821 11.00000 -1.20000 AFIX 0 C17 1 0.401225 0.051269 0.264795 11.00000 0.01191 0.02344 = 0.02075 -0.00998 0.00516 0.00118 AFIX 43 H17 2 0.364072 0.021914 0.236290 11.00000 -1.20000 AFIX 0 C18 1 0.462997 0.175863 0.257868 11.00000 0.02043 0.01826 = 0.01529 -0.00030 0.00657 0.00442 AFIX 43 H18 2 0.474145 0.244449 0.224054 11.00000 -1.20000 AFIX 0 C19 1 0.504998 0.179421 0.310485 11.00000 0.01374 0.01687 = 0.02351 -0.00427 0.00303 0.00351 AFIX 43 H19 2 0.549146 0.251090 0.317968 11.00000 -1.20000 AFIX 0 C20 1 0.469521 0.057014 0.350104 11.00000 0.01591 0.01984 = 0.01892 0.00066 -0.00241 0.00750 AFIX 43 H20 2 0.485891 0.032003 0.388480 11.00000 -1.20000 AFIX 0 FE1 3 0.393685 0.255552 0.324640 11.00000 0.01275 0.01247 = 0.01311 -0.00006 0.00184 0.00090 N1 4 0.311259 0.171119 0.592164 11.00000 0.01660 0.02131 = 0.01017 -0.00103 -0.00069 -0.00218 O9 5 0.436155 0.238080 0.568745 11.00000 0.01486 0.02622 = 0.02023 -0.00048 -0.00317 0.00756 HKLF 4 1.0 0.00 1.00 0.00 0.00 0.00 -1.00 -1.00 0.00 0.00 Covalent radii and connectivity table for 2009src0154 in Pbca C 0.770 H 0.320 FE 1.240 N 0.700 O 0.660 C1 - N1 C2 - C3 N1 C7 C3 - C2 C4 C4 - C5 C3 C5 - C4 C6 C6 - C7 C5 C7 - C6 C2 C8 C8 - C10 C7 C9 C9 - O9 N1 C8 C10 - C8 C11 C11 - C12 C10 C15 Fe1 C12 - C11 C13 Fe1 C13 - C14 C12 Fe1 C14 - C13 C15 Fe1 C15 - C14 C11 Fe1 C16 - C17 C20 Fe1 C17 - C16 C18 Fe1 C18 - C19 C17 Fe1 C19 - C18 C20 Fe1 C20 - C19 C16 Fe1 Fe1 - C15 C13 C12 C16 C17 C14 C18 C19 C20 C11 N1 - C9 C2 C1 O9 - C9 h k l Fo^2 Sigma Why rejected 1 1 0 21.61 5.15 observed but should be systematically absent 0 3 20 46.15 11.48 observed but should be systematically absent 24037 Reflections read, of which 1904 rejected -20 =< h =< 22, -9 =< k =< 9, -30 =< l =< 29, Max. 2-theta = 54.97 2 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 7 3 14 -0.72 0.16 8 2.52 1 Inconsistent equivalents 3408 Unique reflections, of which 0 suppressed R(int) = 0.1137 R(sigma) = 0.0806 Friedel opposites merged Maximum memory for data reduction = 2330 / 34165 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 = 2917 / 259978 wR2 = 0.1661 before cycle 1 for 3408 data and 209 / 209 parameters GooF = S = 1.153; Restrained GooF = 1.153 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 24.76 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24917 0.00065 -0.004 OSF Mean shift/su = 0.006 Maximum = 0.022 for U12 Fe1 Max. shift = 0.000 A for H1B Max. dU = 0.000 for C6 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2917 / 259978 wR2 = 0.1661 before cycle 2 for 3408 data and 209 / 209 parameters GooF = S = 1.153; Restrained GooF = 1.153 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 24.76 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24917 0.00065 0.005 OSF Mean shift/su = 0.002 Maximum = 0.009 for U12 Fe1 Max. shift = 0.000 A for H1B Max. dU = 0.000 for C6 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2917 / 259978 wR2 = 0.1661 before cycle 3 for 3408 data and 209 / 209 parameters GooF = S = 1.153; Restrained GooF = 1.153 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 24.76 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24917 0.00065 0.001 OSF Mean shift/su = 0.000 Maximum = 0.002 for tors H1A Max. shift = 0.000 A for H1B Max. dU = 0.000 for C1 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2917 / 259978 wR2 = 0.1661 before cycle 4 for 3408 data and 209 / 209 parameters GooF = S = 1.153; Restrained GooF = 1.153 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 24.76 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24917 0.00065 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for tors H1A Max. shift = 0.000 A for H1B Max. dU = 0.000 for C19 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2917 / 259978 wR2 = 0.1661 before cycle 5 for 3408 data and 209 / 209 parameters GooF = S = 1.153; Restrained GooF = 1.153 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 24.76 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24917 0.00065 -0.001 OSF Mean shift/su = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for H1C Max. dU = 0.000 for C13 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2917 / 259978 wR2 = 0.1661 before cycle 6 for 3408 data and 209 / 209 parameters GooF = S = 1.153; Restrained GooF = 1.153 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 24.76 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.24917 0.00065 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for z Fe1 Max. shift = 0.000 A for H1C Max. dU = 0.000 for C9 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.3783 0.1013 0.6585 137 0.980 0.000 C1 N1 H1A H1B 0.2985 -0.0053 0.6572 137 0.980 0.000 C1 N1 H1A H1C 0.3014 0.2029 0.6776 137 0.980 0.000 C1 N1 H1A H3 0.1636 0.1063 0.6280 43 0.950 0.000 C3 C2 C4 H4 0.0542 0.1749 0.5731 43 0.950 0.000 C4 C5 C3 H5 0.0655 0.3118 0.4825 43 0.950 0.000 C5 C4 C6 H6 0.1872 0.3669 0.4426 43 0.950 0.000 C6 C7 C5 H10 0.4270 0.3556 0.4650 43 0.950 0.000 C10 C8 C11 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C12 ** H12 0.2560 0.2211 0.3768 43 0.950 0.000 C12 C11 C13 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C13 ** H13 0.2598 0.3631 0.2768 43 0.950 0.000 C13 C14 C12 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C14 ** H14 0.3703 0.5849 0.2730 43 0.950 0.000 C14 C13 C15 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C15 ** H15 0.4377 0.5769 0.3698 43 0.950 0.000 C15 C14 C11 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C16 ** H16 0.3702 -0.1071 0.3378 43 0.950 0.000 C16 C17 C20 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C17 ** H17 0.3641 0.0219 0.2363 43 0.950 0.000 C17 C16 C18 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C18 ** H18 0.4741 0.2444 0.2241 43 0.950 0.000 C18 C19 C17 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C19 ** H19 0.5491 0.2511 0.3180 43 0.950 0.000 C19 C18 C20 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C20 ** H20 0.4859 0.0320 0.3885 43 0.950 0.000 C20 C19 C16 2009src0154 in Pbca ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.32333 0.11283 0.65109 1.00000 0.02043 0.02770 0.01491 0.00362 -0.00088 0.00120 0.02101 0.01051 0.00035 0.00085 0.00024 0.00000 0.00301 0.00332 0.00287 0.00248 0.00249 0.00263 0.00128 H1A 0.37832 0.10131 0.65847 1.00000 0.03152 0.00000 0.00000 H1B 0.29849 -0.00527 0.65719 1.00000 0.03152 0.00000 0.00000 H1C 0.30138 0.20287 0.67762 1.00000 0.03152 0.00000 0.00000 C2 0.23918 0.19264 0.56679 1.00000 0.01750 0.01242 0.01105 -0.00161 0.00069 0.00152 0.01365 0.00920 0.00031 0.00073 0.00022 0.00000 0.00271 0.00251 0.00253 0.00201 0.00224 0.00207 0.00111 C3 0.16822 0.15787 0.59049 1.00000 0.02544 0.01498 0.01532 -0.00137 0.00647 0.00262 0.01858 0.01003 0.00033 0.00076 0.00025 0.00000 0.00313 0.00293 0.00288 0.00222 0.00250 0.00239 0.00125 H3 0.16358 0.10630 0.62802 1.00000 0.02230 0.00000 0.00000 C4 0.10350 0.20042 0.55791 1.00000 0.01388 0.02331 0.02131 -0.00394 0.00272 0.00007 0.01950 0.00967 0.00033 0.00077 0.00024 0.00000 0.00263 0.00312 0.00293 0.00220 0.00245 0.00241 0.00125 H4 0.05416 0.17489 0.57310 1.00000 0.02340 0.00000 0.00000 C5 0.11016 0.27966 0.50353 1.00000 0.01963 0.02693 0.01681 -0.00356 -0.00094 -0.00115 0.02112 0.00974 0.00033 0.00081 0.00024 0.00000 0.00272 0.00342 0.00268 0.00237 0.00243 0.00268 0.00126 H5 0.06551 0.31184 0.48245 1.00000 0.02535 0.00000 0.00000 C6 0.18271 0.31220 0.47971 1.00000 0.01864 0.01584 0.01924 0.00170 0.00174 0.00450 0.01791 0.00993 0.00031 0.00075 0.00025 0.00000 0.00281 0.00274 0.00297 0.00226 0.00244 0.00228 0.00121 H6 0.18724 0.36685 0.44262 1.00000 0.02149 0.00000 0.00000 C7 0.24747 0.26458 0.51032 1.00000 0.01711 0.01202 0.01467 -0.00115 0.00069 -0.00231 0.01460 0.00909 0.00030 0.00078 0.00022 0.00000 0.00245 0.00255 0.00247 0.00232 0.00222 0.00237 0.00106 C8 0.33028 0.28643 0.50046 1.00000 0.01714 0.01023 0.01353 0.00120 -0.00014 0.00231 0.01363 0.00912 0.00031 0.00068 0.00023 0.00000 0.00256 0.00279 0.00260 0.00199 0.00220 0.00207 0.00112 C9 0.36819 0.23360 0.55615 1.00000 0.02146 0.01130 0.01564 -0.00111 -0.00316 0.00490 0.01613 0.00958 0.00031 0.00080 0.00023 0.00000 0.00267 0.00270 0.00258 0.00228 0.00216 0.00237 0.00114 C10 0.37414 0.34225 0.45652 1.00000 0.01779 0.01222 0.01760 -0.00515 -0.00366 0.00119 0.01587 0.00920 0.00032 0.00073 0.00023 0.00000 0.00280 0.00279 0.00289 0.00222 0.00236 0.00216 0.00119 H10 0.42700 0.35560 0.46505 1.00000 0.01905 0.00000 0.00000 C11 0.35203 0.38518 0.39762 1.00000 0.01527 0.01215 0.01258 -0.00457 0.00739 0.00242 0.01333 0.00939 0.00030 0.00073 0.00023 0.00000 0.00278 0.00263 0.00274 0.00210 0.00220 0.00215 0.00114 C12 0.29178 0.30964 0.36393 1.00000 0.01188 0.01603 0.01648 -0.00145 0.00398 0.00084 0.01480 0.00945 0.00030 0.00075 0.00024 0.00000 0.00258 0.00273 0.00277 0.00217 0.00228 0.00210 0.00115 H12 0.25596 0.22114 0.37678 1.00000 0.01776 0.00000 0.00000 C13 0.29413 0.38897 0.30763 1.00000 0.01816 0.02155 0.01330 -0.00035 0.00179 0.01066 0.01767 0.01045 0.00032 0.00079 0.00024 0.00000 0.00287 0.00301 0.00281 0.00229 0.00231 0.00245 0.00123 H13 0.25981 0.36313 0.27684 1.00000 0.02120 0.00000 0.00000 C14 0.35610 0.51253 0.30530 1.00000 0.02689 0.01610 0.01810 0.00206 0.00223 0.00682 0.02036 0.01050 0.00035 0.00079 0.00025 0.00000 0.00321 0.00294 0.00298 0.00233 0.00257 0.00251 0.00128 H14 0.37028 0.58486 0.27296 1.00000 0.02444 0.00000 0.00000 C15 0.39331 0.50937 0.35975 1.00000 0.01748 0.01610 0.01985 -0.00332 0.00706 -0.00056 0.01781 0.01006 0.00034 0.00075 0.00024 0.00000 0.00272 0.00273 0.00298 0.00223 0.00260 0.00243 0.00117 H15 0.43771 0.57689 0.36983 1.00000 0.02137 0.00000 0.00000 C16 0.40474 -0.02141 0.32157 1.00000 0.02339 0.00800 0.02041 -0.00075 0.00553 0.00203 0.01727 0.00973 0.00032 0.00069 0.00025 0.00000 0.00307 0.00239 0.00293 0.00225 0.00256 0.00218 0.00118 H16 0.37016 -0.10713 0.33781 1.00000 0.02072 0.00000 0.00000 C17 0.40122 0.05128 0.26480 1.00000 0.01189 0.02344 0.02073 -0.00995 0.00515 0.00121 0.01869 0.00992 0.00032 0.00078 0.00025 0.00000 0.00271 0.00297 0.00300 0.00238 0.00241 0.00241 0.00123 H17 0.36407 0.02195 0.23629 1.00000 0.02242 0.00000 0.00000 C18 0.46299 0.17585 0.25787 1.00000 0.02042 0.01826 0.01536 -0.00032 0.00656 0.00443 0.01801 0.01004 0.00031 0.00079 0.00025 0.00000 0.00297 0.00281 0.00288 0.00233 0.00241 0.00238 0.00122 H18 0.47414 0.24445 0.22406 1.00000 0.02162 0.00000 0.00000 C19 0.50500 0.17941 0.31048 1.00000 0.01372 0.01686 0.02346 -0.00429 0.00303 0.00354 0.01801 0.01002 0.00032 0.00078 0.00024 0.00000 0.00276 0.00270 0.00318 0.00232 0.00236 0.00226 0.00124 H19 0.54915 0.25106 0.31796 1.00000 0.02162 0.00000 0.00000 C20 0.46952 0.05700 0.35010 1.00000 0.01590 0.01983 0.01893 0.00065 -0.00237 0.00748 0.01822 0.01018 0.00031 0.00079 0.00026 0.00000 0.00285 0.00300 0.00298 0.00240 0.00241 0.00241 0.00124 H20 0.48588 0.03199 0.38848 1.00000 0.02186 0.00000 0.00000 Fe1 0.39369 0.25555 0.32464 1.00000 0.01276 0.01247 0.01312 -0.00007 0.00185 0.00091 0.01278 0.00131 0.00004 0.00011 0.00003 0.00000 0.00034 0.00034 0.00035 0.00034 0.00033 0.00036 0.00019 N1 0.31126 0.17113 0.59216 1.00000 0.01659 0.02131 0.01017 -0.00101 -0.00068 -0.00219 0.01602 0.00787 0.00026 0.00066 0.00019 0.00000 0.00239 0.00251 0.00224 0.00189 0.00192 0.00200 0.00101 O9 0.43616 0.23809 0.56874 1.00000 0.01485 0.02625 0.02023 -0.00045 -0.00320 0.00755 0.02044 0.00702 0.00020 0.00063 0.00017 0.00000 0.00183 0.00219 0.00200 0.00193 0.00163 0.00192 0.00085 Final Structure Factor Calculation for 2009src0154 in Pbca Total number of l.s. parameters = 209 Maximum vector length = 511 Memory required = 2708 / 24017 wR2 = 0.1661 before cycle 7 for 3408 data and 0 / 209 parameters GooF = S = 1.153; Restrained GooF = 1.153 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 24.76 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0871 for 2262 Fo > 4sig(Fo) and 0.1399 for all 3408 data wR2 = 0.1661, GooF = S = 1.153, Restrained GooF = 1.153 for all data Occupancy sum of asymmetric unit = 23.00 for non-hydrogen and 17.00 for hydrogen atoms Principal mean square atomic displacements U 0.0288 0.0205 0.0138 C1 0.0179 0.0133 0.0097 C2 0.0288 0.0162 0.0108 C3 0.0266 0.0191 0.0128 C4 0.0281 0.0199 0.0153 C5 0.0234 0.0179 0.0125 C6 0.0183 0.0145 0.0109 C7 0.0179 0.0138 0.0092 C8 0.0247 0.0144 0.0093 C9 0.0233 0.0153 0.0090 C10 0.0216 0.0150 0.0035 C11 0.0190 0.0161 0.0093 C12 0.0307 0.0138 0.0085 C13 0.0308 0.0176 0.0126 C14 0.0266 0.0159 0.0109 C15 0.0277 0.0166 0.0075 C16 0.0324 0.0165 0.0072 C17 0.0265 0.0177 0.0099 C18 0.0257 0.0187 0.0096 C19 0.0257 0.0194 0.0096 C20 0.0149 0.0127 0.0108 Fe1 0.0222 0.0159 0.0100 N1 0.0304 0.0206 0.0104 O9 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 0.063 0.084 0.112 0.160 1.000 Number in group 366. 332. 341. 352. 332. 325. 345. 336. 337. 342. GooF 1.272 1.315 1.172 1.287 1.140 1.156 1.122 1.049 1.044 0.902 K 15.735 3.499 1.414 1.214 1.131 1.044 1.012 1.012 1.012 1.001 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.66 inf Number in group 343. 347. 340. 335. 348. 338. 340. 333. 343. 341. GooF 1.350 1.234 1.269 1.267 1.181 1.131 1.067 0.984 0.988 0.986 K 1.136 1.120 1.057 1.065 1.040 1.018 1.005 1.000 1.004 1.004 R1 0.322 0.278 0.223 0.192 0.171 0.133 0.100 0.083 0.060 0.037 Recommended weighting scheme: WGHT 0.0000 24.7192 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) 12 6 17 1050.61 27.85 3.89 0.013 0.77 6 1 26 1074.81 2183.57 3.58 0.118 0.84 14 0 18 1313.88 2706.60 3.53 0.132 0.90 5 1 29 644.68 71.55 3.51 0.021 0.77 6 6 0 4024.87 7035.19 3.46 0.212 1.13 8 2 27 1260.89 242.88 3.40 0.039 0.78 7 8 9 635.60 1.25 3.37 0.003 0.82 6 8 7 841.73 149.87 3.30 0.031 0.85 4 4 22 1264.28 2232.60 3.28 0.120 0.89 9 6 20 959.03 134.16 3.12 0.029 0.77 3 6 22 2067.01 1169.54 3.01 0.087 0.79 2 9 3 639.81 4.48 2.96 0.005 0.81 18 1 10 977.32 269.48 2.94 0.042 0.89 0 2 28 3314.45 1920.47 2.88 0.111 0.81 11 7 4 356.48 8.92 2.87 0.008 0.87 7 5 13 366.26 0.36 2.87 0.002 1.03 5 3 21 390.01 14.40 2.87 0.010 0.96 13 5 18 88.60 817.92 2.87 0.072 0.78 8 4 20 660.52 131.45 2.85 0.029 0.89 3 9 1 449.57 7.90 2.82 0.007 0.81 4 3 24 710.24 237.23 2.81 0.039 0.88 12 6 11 447.83 44.48 2.79 0.017 0.86 17 6 5 704.44 23.44 2.77 0.012 0.78 11 8 2 403.99 999.87 2.70 0.080 0.79 0 6 23 1072.86 116.73 2.69 0.027 0.78 7 3 23 86.20 478.60 2.67 0.055 0.87 7 1 23 501.09 15.89 2.66 0.010 0.92 1 3 21 -53.15 122.36 2.64 0.028 1.00 12 6 9 593.67 118.44 2.60 0.028 0.88 18 1 12 260.21 758.27 2.59 0.070 0.86 11 7 1 1078.73 486.67 2.56 0.056 0.87 5 5 11 583.02 147.03 2.56 0.031 1.14 15 1 4 285.23 41.51 2.54 0.016 1.13 0 4 17 834.99 59.90 2.54 0.020 1.09 11 1 19 532.82 120.24 2.54 0.028 0.96 20 1 10 763.53 6.40 2.54 0.006 0.81 6 8 8 853.02 353.46 2.54 0.048 0.84 9 6 11 336.28 5.43 2.52 0.006 0.93 5 6 12 1138.06 407.92 2.52 0.051 0.99 4 8 15 453.99 0.87 2.52 0.002 0.78 4 7 14 565.92 174.93 2.52 0.033 0.87 20 3 9 630.62 22.81 2.51 0.012 0.78 3 6 7 199.96 0.96 2.51 0.002 1.13 4 0 26 4731.35 3263.27 2.50 0.144 0.87 12 0 24 978.47 21.77 2.50 0.012 0.80 4 7 9 953.59 439.99 2.49 0.053 0.95 11 6 5 -110.80 131.97 2.49 0.029 0.95 5 8 5 480.51 40.11 2.49 0.016 0.87 12 3 18 1935.13 1244.49 2.49 0.089 0.90 10 6 12 2948.44 2051.50 2.48 0.115 0.89 Bond lengths and angles C1 - Distance Angles N1 1.4433 (0.0068) H1A 0.9800 109.47 H1B 0.9800 109.47 109.47 H1C 0.9800 109.47 109.47 109.47 C1 - N1 H1A H1B C2 - Distance Angles C3 1.3800 (0.0077) N1 1.3988 (0.0069) 128.50 (0.48) C7 1.4155 (0.0072) 121.81 (0.51) 109.67 (0.46) C2 - C3 N1 C3 - Distance Angles C2 1.3800 (0.0077) C4 1.3946 (0.0080) 118.27 (0.52) H3 0.9500 120.87 120.87 C3 - C2 C4 C4 - Distance Angles C5 1.3900 (0.0078) C3 1.3946 (0.0080) 120.94 (0.54) H4 0.9500 119.53 119.53 C4 - C5 C3 C5 - Distance Angles C4 1.3900 (0.0078) C6 1.4032 (0.0078) 120.12 (0.54) H5 0.9500 119.94 119.94 C5 - C4 C6 C6 - Distance Angles C7 1.3802 (0.0075) C5 1.4032 (0.0078) 119.82 (0.52) H6 0.9500 120.09 120.09 C6 - C7 C5 C7 - Distance Angles C6 1.3802 (0.0075) C2 1.4155 (0.0072) 118.90 (0.50) C8 1.4743 (0.0073) 134.33 (0.50) 106.48 (0.46) C7 - C6 C2 C8 - Distance Angles C10 1.3371 (0.0076) C7 1.4743 (0.0073) 135.55 (0.51) C9 1.4988 (0.0072) 118.57 (0.48) 105.86 (0.44) C8 - C10 C7 C9 - Distance Angles O9 1.2239 (0.0062) N1 1.3762 (0.0070) 124.56 (0.51) C8 1.4988 (0.0072) 128.79 (0.52) 106.62 (0.44) C9 - O9 N1 C10 - Distance Angles C8 1.3371 (0.0076) C11 1.4500 (0.0076) 128.84 (0.52) H10 0.9500 115.58 115.58 C10 - C8 C11 C11 - Distance Angles C12 1.4225 (0.0075) C10 1.4500 (0.0076) 128.81 (0.51) C15 1.4555 (0.0075) 106.39 (0.48) 124.66 (0.51) Fe1 2.0693 (0.0051) 68.59 (0.29) 124.86 (0.38) 67.87 (0.29) C11 - C12 C10 C15 C12 - Distance Angles C11 1.4225 (0.0075) C13 1.4264 (0.0077) 108.59 (0.49) Fe1 2.0388 (0.0053) 70.90 (0.30) 69.38 (0.31) H12 0.9500 125.70 125.70 125.59 C12 - C11 C13 Fe1 C13 - Distance Angles C14 1.4141 (0.0083) C12 1.4264 (0.0077) 108.59 (0.51) Fe1 2.0355 (0.0054) 70.18 (0.32) 69.63 (0.31) H13 0.9500 125.71 125.71 126.06 C13 - C14 C12 Fe1 C14 - Distance Angles C13 1.4141 (0.0083) C15 1.4168 (0.0082) 107.91 (0.52) Fe1 2.0472 (0.0057) 69.29 (0.32) 69.12 (0.32) H14 0.9500 126.05 126.05 127.11 C14 - C13 C15 Fe1 C15 - Distance Angles C14 1.4168 (0.0082) C11 1.4555 (0.0075) 108.47 (0.51) Fe1 2.0326 (0.0055) 70.24 (0.33) 70.57 (0.30) H15 0.9500 125.77 125.77 125.02 C15 - C14 C11 Fe1 C16 - Distance Angles C17 1.4179 (0.0080) C20 1.4315 (0.0079) 108.02 (0.50) Fe1 2.0439 (0.0051) 69.73 (0.31) 70.04 (0.31) H16 0.9500 125.99 125.99 125.82 C16 - C17 C20 Fe1 C17 - Distance Angles C16 1.4179 (0.0080) C18 1.4242 (0.0078) 108.23 (0.51) Fe1 2.0445 (0.0055) 69.68 (0.30) 69.75 (0.32) H17 0.9500 125.88 125.88 126.26 C17 - C16 C18 Fe1 C18 - Distance Angles C19 1.4208 (0.0081) C17 1.4242 (0.0078) 107.91 (0.52) Fe1 2.0475 (0.0055) 69.85 (0.32) 69.52 (0.31) H18 0.9500 126.05 126.05 126.16 C18 - C19 C17 Fe1 C19 - Distance Angles C18 1.4208 (0.0080) C20 1.4252 (0.0080) 108.27 (0.50) Fe1 2.0510 (0.0055) 69.58 (0.31) 69.90 (0.31) H19 0.9500 125.87 125.87 126.22 C19 - C18 C20 Fe1 C20 - Distance Angles C19 1.4252 (0.0081) C16 1.4315 (0.0079) 107.57 (0.50) Fe1 2.0565 (0.0055) 69.49 (0.32) 69.09 (0.30) H20 0.9500 126.22 126.22 126.76 C20 - C19 C16 Fe1 Fe1 - Distance Angles C15 2.0326 (0.0055) C13 2.0355 (0.0054) 68.48 (0.24) C12 2.0388 (0.0053) 68.95 (0.22) 40.99 (0.22) C16 2.0439 (0.0051) 157.87 (0.24) 123.57 (0.24) 106.97 (0.23) C17 2.0445 (0.0055) 160.54 (0.23) 106.11 (0.24) 120.04 (0.22) 40.59 (0.23) C14 2.0472 (0.0057) 40.64 (0.23) 40.53 (0.23) 68.73 (0.23) 159.99 (0.25) 123.30 (0.24) C18 2.0475 (0.0055) 124.39 (0.23) 119.86 (0.23) 155.31 (0.23) 68.50 (0.23) 40.73 (0.22) 106.78 (0.23) C19 2.0510 (0.0055) 108.46 (0.24) 155.73 (0.23) 162.42 (0.23) 68.50 (0.23) 68.34 (0.23) 121.39 (0.24) 40.57 (0.22) C20 2.0565 (0.0055) 122.53 (0.24) 161.38 (0.24) 125.02 (0.23) 40.87 (0.22) 68.41 (0.24) 157.32 (0.24) 68.39 (0.23) C11 2.0693 (0.0051) 41.56 (0.21) 68.60 (0.22) 40.51 (0.21) 121.28 (0.23) 155.73 (0.22) 68.97 (0.22) 162.59 (0.22) Fe1 - C15 C13 C12 C16 C17 C14 C18 N1 - Distance Angles C9 1.3762 (0.0070) C2 1.3988 (0.0069) 111.11 (0.43) C1 1.4433 (0.0068) 124.33 (0.47) 124.12 (0.46) N1 - C9 C2 O9 - Distance Angles C9 1.2239 (0.0063) O9 - FMAP and GRID set by program FMAP 2 1 22 GRID -1.316 -2 -1 1.316 2 1 R1 = 0.1375 for 3408 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.60 at 0.2014 0.2596 0.0835 [ 0.84 A from C2 ] Deepest hole -0.60 at 0.2138 0.2441 0.3704 [ 0.77 A from H12 ] Mean = 0.00, Rms deviation from mean = 0.13 e/A^3, Highest memory used = 2944 / 27775 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2014 0.2404 0.5835 1.00000 0.05 0.60 0.84 C2 0.85 C3 1.57 H3 1.83 C4 Q2 1 0.3444 0.2627 0.5301 1.00000 0.05 0.59 0.75 C8 0.76 C9 1.69 N1 1.76 C7 Q3 1 0.4597 0.5522 0.3804 1.00000 0.05 0.55 0.49 H15 1.29 C15 2.28 C11 2.50 H10 Q4 1 0.0620 0.0461 0.6221 1.00000 0.05 0.54 1.48 H4 1.84 H3 2.00 C4 2.05 H19 Q5 1 0.6164 0.0983 0.3076 1.00000 0.05 0.50 1.64 H19 1.66 H1A 1.83 H1B 1.88 H14 Q6 1 0.2528 0.3234 0.2527 1.00000 0.05 0.49 0.64 H13 1.54 C13 1.94 H1C 2.54 H17 Q7 1 0.0558 -0.0128 0.5816 1.00000 0.05 0.49 1.39 H4 1.86 C4 1.86 O9 2.34 H3 Q8 1 0.4299 0.1935 0.4807 1.00000 0.05 0.49 1.24 H10 1.57 C10 1.93 C8 2.06 O9 Q9 1 0.4371 0.1124 0.3310 1.00000 0.05 0.48 0.83 C20 1.15 C16 1.30 FE1 1.37 C19 Q10 1 0.2013 0.4550 0.4898 1.00000 0.05 0.48 1.12 C6 1.29 H6 1.68 C7 2.07 C5 Shortest distances between peaks (including symmetry equivalents) 4 7 1.04 3 7 1.92 3 4 1.93 2 8 1.95 2 10 2.57 1 10 2.68 2 7 2.68 1 2 2.79 8 10 2.89 1 4 2.96 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 0.02: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 1.08: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.64: Structure factors and derivatives 1.53: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.19: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.14: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.06: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + platon finished at 17:41:30 Total CPU time: 4.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++