+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src1151 started at 16:38:10 on 02-Nov-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src1151 in P2(1)/c CELL 0.71073 6.0028 21.5130 11.3488 90.000 93.010 90.000 ZERR 4.00 0.0002 0.0012 0.0005 0.000 0.003 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O FE UNIT 76 68 4 4 4 V = 1463.54 F(000) = 688.0 Mu = 1.03 mm-1 Cell Wt = 1324.74 Rho = 1.503 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 DFIX 1.00 N1 H1N FMAP 2 PLAN 20 SIZE 0.15 0.15 0.31 ACTA BOND $H CONF WGHT 0.05560 1.35160 L.S. 10 TEMP -153.00 FVAR 0.52707 C1 1 0.082946 0.317052 0.605034 11.00000 0.03319 0.02683 = 0.01565 -0.00059 0.00737 -0.00826 AFIX 43 H1 2 -0.035953 0.290187 0.580059 11.00000 -1.20000 AFIX 0 C2 1 0.302530 0.298631 0.641570 11.00000 0.05228 0.02998 = 0.01406 0.01168 0.01210 0.01610 AFIX 43 H2 2 0.357458 0.257221 0.644958 11.00000 -1.20000 AFIX 0 C3 1 0.426800 0.353628 0.672471 11.00000 0.02433 0.06724 = 0.01068 0.00642 -0.00020 0.00074 AFIX 43 H3 2 0.578528 0.355185 0.700675 11.00000 -1.20000 AFIX 0 C4 1 0.283681 0.405043 0.653547 11.00000 0.04121 0.03031 = 0.01130 -0.00465 0.00634 -0.01130 AFIX 43 H4 2 0.322104 0.447448 0.666185 11.00000 -1.20000 AFIX 0 C5 1 0.072684 0.382226 0.612389 11.00000 0.02620 0.02678 = 0.01410 0.00043 0.00580 0.00472 AFIX 43 H5 2 -0.055172 0.406923 0.592887 11.00000 -1.20000 AFIX 0 C6 1 0.221548 0.336121 0.326480 11.00000 0.02640 0.02413 = 0.01127 -0.00214 -0.00021 0.00173 AFIX 43 H6 2 0.087880 0.316287 0.298097 11.00000 -1.20000 AFIX 0 C7 1 0.424698 0.305597 0.362837 11.00000 0.03289 0.02459 = 0.01266 -0.00145 0.00324 0.01097 AFIX 43 H7 2 0.449744 0.261995 0.362715 11.00000 -1.20000 AFIX 0 C8 1 0.583952 0.352020 0.399470 11.00000 0.02119 0.03737 = 0.01384 0.00502 0.00341 0.00712 AFIX 43 H8 2 0.733437 0.344912 0.427936 11.00000 -1.20000 AFIX 0 C9 1 0.477434 0.410856 0.385468 11.00000 0.01915 0.03145 = 0.01104 0.00088 0.00408 -0.00321 AFIX 43 H9 2 0.544450 0.449962 0.403426 11.00000 -1.20000 AFIX 0 C10 1 0.253389 0.401590 0.340029 11.00000 0.02079 0.02353 = 0.00870 0.00162 0.00240 0.00228 C11 1 0.086866 0.452131 0.311617 11.00000 0.02420 0.02106 = 0.01010 0.00007 0.00217 -0.00014 AFIX 23 H11A 2 0.137734 0.490746 0.352141 11.00000 -1.20000 H11B 2 -0.057810 0.440254 0.343138 11.00000 -1.20000 AFIX 0 C12 1 0.050995 0.465525 0.178164 11.00000 0.02086 0.01921 = 0.01380 0.00227 -0.00058 0.00203 AFIX 13 H12 2 -0.054477 0.501334 0.167979 11.00000 -1.20000 AFIX 0 C13 1 0.265667 0.482241 0.119062 11.00000 0.02514 0.02348 = 0.01125 0.00748 -0.00311 0.00082 C14 1 0.104934 0.402075 0.012412 11.00000 0.02004 0.01795 = 0.01473 0.00634 -0.00096 0.00080 C15 1 0.067245 0.356853 -0.072873 11.00000 0.02537 0.02421 = 0.01241 0.00098 0.00427 0.00216 AFIX 43 H15 2 0.168409 0.350274 -0.133279 11.00000 -1.20000 AFIX 0 C16 1 -0.126237 0.321298 -0.066187 11.00000 0.03221 0.02210 = 0.01671 0.00003 -0.00074 -0.00287 AFIX 43 H16 2 -0.157758 0.289857 -0.123435 11.00000 -1.20000 AFIX 0 C17 1 -0.273248 0.330884 0.022149 11.00000 0.02431 0.02879 = 0.02027 0.00153 0.00033 -0.00788 AFIX 43 H17 2 -0.403878 0.306092 0.024658 11.00000 -1.20000 AFIX 0 C18 1 -0.230549 0.377043 0.108136 11.00000 0.01808 0.03157 = 0.01640 0.00303 0.00176 0.00003 AFIX 43 H18 2 -0.331264 0.383814 0.168682 11.00000 -1.20000 AFIX 0 C19 1 -0.039412 0.412275 0.102729 11.00000 0.01908 0.02012 = 0.00961 0.00392 -0.00170 0.00194 N1 3 0.284058 0.444483 0.023518 11.00000 0.02100 0.02503 = 0.01217 0.00019 0.00342 -0.00441 O1 4 0.399741 0.522967 0.151053 11.00000 0.03063 0.02975 = 0.01526 0.00197 -0.00057 -0.01078 FE1 5 0.311432 0.356407 0.499334 11.00000 0.02011 0.02184 = 0.00808 0.00112 0.00071 0.00110 H1N 2 0.399407 0.448407 -0.032151 11.00000 -1.20000 HKLF 4 Covalent radii and connectivity table for 2009src1151 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 FE 1.240 C1 - C5 C2 Fe1 C2 - C1 C3 Fe1 C3 - C4 C2 Fe1 C4 - C3 C5 Fe1 C5 - C1 C4 Fe1 C6 - C7 C10 Fe1 C7 - C6 C8 Fe1 C8 - C9 C7 Fe1 C9 - C8 C10 Fe1 C10 - C6 C9 C11 Fe1 C11 - C10 C12 C12 - C19 C13 C11 C13 - O1 N1 C12 C14 - C15 C19 N1 C15 - C14 C16 C16 - C17 C15 C17 - C16 C18 C18 - C19 C17 C19 - C18 C14 C12 N1 - C13 C14 O1 - C13 Fe1 - C2 C8 C7 C9 C3 C5 C1 C4 C6 C10 17355 Reflections read, of which 356 rejected -7 =< h =< 6, -27 =< k =< 27, -14 =< l =< 14, Max. 2-theta = 54.97 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 0 20 3 -0.11 0.14 7 2.00 1 Inconsistent equivalents 3347 Unique reflections, of which 0 suppressed R(int) = 0.0823 R(sigma) = 0.0643 Friedel opposites merged Maximum memory for data reduction = 3885 / 32784 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 = 4453 / 251368 wR2 = 0.1253 before cycle 1 for 3347 data and 202 / 202 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.035 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.046; Restrained GooF = 1.046 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0556 * P )^2 + 1.35 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.52719 0.00124 0.099 OSF Mean shift/su = 0.038 Maximum = 0.391 for U13 N1 Max. shift = 0.013 A for H1N Max. dU = 0.000 for N1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4453 / 251368 wR2 = 0.1253 before cycle 2 for 3347 data and 202 / 202 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.043 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.046; Restrained GooF = 1.047 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0556 * P )^2 + 1.35 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.52719 0.00124 -0.001 OSF Mean shift/su = 0.014 Maximum = -0.182 for y H1N Max. shift = 0.007 A for H1N Max. dU = 0.000 for N1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4453 / 251368 wR2 = 0.1253 before cycle 3 for 3347 data and 202 / 202 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.047 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.046; Restrained GooF = 1.047 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0556 * P )^2 + 1.35 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.52719 0.00124 0.000 OSF Mean shift/su = 0.002 Maximum = 0.046 for z H1N Max. shift = 0.002 A for H1N Max. dU = 0.000 for C19 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4453 / 251368 wR2 = 0.1253 before cycle 4 for 3347 data and 202 / 202 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.047 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.046; Restrained GooF = 1.047 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0556 * P )^2 + 1.35 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.52719 0.00124 -0.001 OSF Mean shift/su = 0.001 Maximum = 0.013 for z H1N Max. shift = 0.001 A for H1N Max. dU = 0.000 for N1 Least-squares cycle 5 Maximum vector length = 511 Memory required = 4453 / 251368 wR2 = 0.1253 before cycle 5 for 3347 data and 202 / 202 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.047 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.046; Restrained GooF = 1.047 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0556 * P )^2 + 1.35 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.52719 0.00124 0.000 OSF Mean shift/su = 0.000 Maximum = 0.005 for z H1N Max. shift = 0.000 A for H1N Max. dU = 0.000 for C3 Least-squares cycle 6 Maximum vector length = 511 Memory required = 4453 / 251368 wR2 = 0.1253 before cycle 6 for 3347 data and 202 / 202 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.047 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.046; Restrained GooF = 1.047 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0556 * P )^2 + 1.35 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.52719 0.00124 0.000 OSF Mean shift/su = 0.000 Maximum = 0.002 for x H1N Max. shift = 0.000 A for H1N Max. dU = 0.000 for N1 Least-squares cycle 7 Maximum vector length = 511 Memory required = 4453 / 251368 wR2 = 0.1253 before cycle 7 for 3347 data and 202 / 202 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.047 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.046; Restrained GooF = 1.047 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0556 * P )^2 + 1.35 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.52719 0.00124 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for y Fe1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for C16 Least-squares cycle 8 Maximum vector length = 511 Memory required = 4453 / 251368 wR2 = 0.1253 before cycle 8 for 3347 data and 202 / 202 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.047 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.046; Restrained GooF = 1.047 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0556 * P )^2 + 1.35 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.52719 0.00124 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for y Fe1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for N1 Least-squares cycle 9 Maximum vector length = 511 Memory required = 4453 / 251368 wR2 = 0.1253 before cycle 9 for 3347 data and 202 / 202 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.047 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.046; Restrained GooF = 1.047 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0556 * P )^2 + 1.35 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.52719 0.00124 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for y Fe1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for C13 Least-squares cycle 10 Maximum vector length = 511 Memory required = 4453 / 251368 wR2 = 0.1253 before cycle 10 for 3347 data and 202 / 202 parameters Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.047 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.046; Restrained GooF = 1.047 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0556 * P )^2 + 1.35 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.52719 0.00124 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for y Fe1 Max. shift = 0.000 A for C7 Max. dU = 0.000 for C8 Largest correlation matrix elements 0.550 U11 Fe1 / OSF 0.534 U33 Fe1 / OSF 0.518 U22 Fe1 / OSF Idealized hydrogen atom generation before cycle 11 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 C1 ** H1 -0.0360 0.2902 0.5801 43 0.950 0.000 C1 C5 C2 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C2 ** H2 0.3575 0.2572 0.6450 43 0.950 0.000 C2 C1 C3 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C3 ** H3 0.5785 0.3552 0.7007 43 0.950 0.000 C3 C4 C2 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C4 ** H4 0.3221 0.4474 0.6662 43 0.950 0.000 C4 C3 C5 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C5 ** H5 -0.0552 0.4069 0.5929 43 0.950 0.000 C5 C1 C4 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C6 ** H6 0.0879 0.3163 0.2981 43 0.950 0.000 C6 C7 C10 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C7 ** H7 0.4498 0.2620 0.3627 43 0.950 0.000 C7 C6 C8 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C8 ** H8 0.7334 0.3449 0.4279 43 0.950 0.000 C8 C9 C7 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C9 ** H9 0.5445 0.4499 0.4034 43 0.950 0.000 C9 C8 C10 H11A 0.1378 0.4907 0.3521 23 0.990 0.000 C11 C10 C12 H11B -0.0578 0.4403 0.3431 23 0.990 0.000 C11 C10 C12 H12 -0.0545 0.5013 0.1680 13 1.000 0.000 C12 C19 C13 C11 H15 0.1684 0.3503 -0.1333 43 0.950 0.000 C15 C14 C16 H16 -0.1577 0.2899 -0.1234 43 0.950 0.000 C16 C17 C15 H17 -0.4039 0.3061 0.0246 43 0.950 0.000 C17 C16 C18 H18 -0.3312 0.3838 0.1687 43 0.950 0.000 C18 C19 C17 2009src1151 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.08293 0.31706 0.60503 1.00000 0.03317 0.02678 0.01563 -0.00065 0.00737 -0.00814 0.02498 0.00533 0.00051 0.00014 0.00025 0.00000 0.00168 0.00167 0.00145 0.00124 0.00119 0.00130 0.00066 H1 -0.03597 0.29020 0.58006 1.00000 0.02998 0.00000 0.00000 C2 0.30258 0.29863 0.64157 1.00000 0.05224 0.02989 0.01406 0.01162 0.01205 0.01607 0.03170 0.00655 0.00058 0.00016 0.00027 0.00000 0.00213 0.00182 0.00148 0.00129 0.00135 0.00151 0.00078 H2 0.35752 0.25722 0.64496 1.00000 0.03804 0.00000 0.00000 C3 0.42678 0.35361 0.67246 1.00000 0.02430 0.06739 0.01065 0.00633 -0.00017 0.00072 0.03415 0.00611 0.00054 0.00018 0.00027 0.00000 0.00162 0.00260 0.00147 0.00148 0.00118 0.00154 0.00084 H3 0.57851 0.35516 0.70066 1.00000 0.04098 0.00000 0.00000 C4 0.28370 0.40504 0.65356 1.00000 0.04137 0.03021 0.01121 -0.00461 0.00637 -0.01127 0.02742 0.00524 0.00053 0.00015 0.00025 0.00000 0.00185 0.00178 0.00141 0.00123 0.00123 0.00140 0.00071 H4 0.32214 0.44744 0.66622 1.00000 0.03291 0.00000 0.00000 C5 0.07269 0.38223 0.61239 1.00000 0.02610 0.02681 0.01399 0.00042 0.00585 0.00477 0.02213 0.00530 0.00049 0.00015 0.00025 0.00000 0.00151 0.00159 0.00139 0.00123 0.00109 0.00124 0.00061 H5 -0.05515 0.40693 0.59289 1.00000 0.02656 0.00000 0.00000 C6 0.22154 0.33612 0.32648 1.00000 0.02636 0.02426 0.01120 -0.00216 -0.00026 0.00173 0.02065 0.00506 0.00048 0.00014 0.00024 0.00000 0.00153 0.00152 0.00134 0.00114 0.00109 0.00118 0.00061 H6 0.08788 0.31628 0.29811 1.00000 0.02478 0.00000 0.00000 C7 0.42472 0.30560 0.36282 1.00000 0.03297 0.02458 0.01263 -0.00145 0.00318 0.01104 0.02332 0.00540 0.00049 0.00015 0.00024 0.00000 0.00166 0.00160 0.00137 0.00117 0.00115 0.00127 0.00064 H7 0.44980 0.26200 0.36268 1.00000 0.02799 0.00000 0.00000 C8 0.58391 0.35202 0.39946 1.00000 0.02122 0.03735 0.01378 0.00507 0.00342 0.00713 0.02403 0.00555 0.00050 0.00014 0.00026 0.00000 0.00146 0.00184 0.00141 0.00125 0.00110 0.00125 0.00066 H8 0.73338 0.34491 0.42794 1.00000 0.02884 0.00000 0.00000 C9 0.47748 0.41084 0.38544 1.00000 0.01922 0.03157 0.01093 0.00092 0.00405 -0.00320 0.02046 0.00504 0.00044 0.00014 0.00024 0.00000 0.00142 0.00169 0.00132 0.00116 0.00104 0.00116 0.00062 H9 0.54455 0.44994 0.40337 1.00000 0.02455 0.00000 0.00000 C10 0.25337 0.40159 0.34004 1.00000 0.02072 0.02360 0.00872 0.00163 0.00240 0.00231 0.01762 0.00485 0.00045 0.00013 0.00023 0.00000 0.00139 0.00151 0.00126 0.00109 0.00099 0.00111 0.00058 C11 0.08687 0.45213 0.31162 1.00000 0.02426 0.02111 0.01009 0.00009 0.00210 -0.00009 0.01844 0.00485 0.00045 0.00013 0.00023 0.00000 0.00145 0.00146 0.00128 0.00109 0.00105 0.00111 0.00058 H11A 0.13776 0.49075 0.35214 1.00000 0.02213 0.00000 0.00000 H11B -0.05780 0.44026 0.34315 1.00000 0.02213 0.00000 0.00000 C12 0.05097 0.46553 0.17818 1.00000 0.02089 0.01922 0.01372 0.00225 -0.00064 0.00206 0.01800 0.00473 0.00045 0.00013 0.00024 0.00000 0.00140 0.00144 0.00133 0.00110 0.00104 0.00110 0.00058 H12 -0.05451 0.50134 0.16801 1.00000 0.02160 0.00000 0.00000 C13 0.26566 0.48225 0.11907 1.00000 0.02516 0.02342 0.01123 0.00751 -0.00301 0.00082 0.02007 0.00495 0.00046 0.00014 0.00024 0.00000 0.00149 0.00151 0.00132 0.00114 0.00106 0.00118 0.00060 C14 0.10497 0.40207 0.01243 1.00000 0.02011 0.01797 0.01464 0.00637 -0.00094 0.00082 0.01764 0.00483 0.00045 0.00013 0.00024 0.00000 0.00136 0.00141 0.00131 0.00108 0.00102 0.00107 0.00057 C15 0.06723 0.35685 -0.07287 1.00000 0.02549 0.02418 0.01229 0.00099 0.00424 0.00208 0.02054 0.00506 0.00048 0.00013 0.00025 0.00000 0.00149 0.00152 0.00137 0.00114 0.00110 0.00117 0.00061 H15 0.16835 0.35027 -0.13330 1.00000 0.02465 0.00000 0.00000 C16 -0.12623 0.32130 -0.06616 1.00000 0.03228 0.02220 0.01671 0.00000 -0.00083 -0.00281 0.02380 0.00516 0.00050 0.00014 0.00025 0.00000 0.00162 0.00160 0.00144 0.00121 0.00118 0.00125 0.00064 H16 -0.15773 0.28985 -0.12340 1.00000 0.02856 0.00000 0.00000 C17 -0.27326 0.33088 0.02214 1.00000 0.02430 0.02884 0.02021 0.00150 0.00031 -0.00793 0.02448 0.00521 0.00050 0.00015 0.00026 0.00000 0.00153 0.00164 0.00150 0.00129 0.00116 0.00125 0.00065 H17 -0.40391 0.30609 0.02463 1.00000 0.02937 0.00000 0.00000 C18 -0.23053 0.37703 0.10815 1.00000 0.01815 0.03152 0.01631 0.00306 0.00172 0.00005 0.02197 0.00512 0.00045 0.00015 0.00025 0.00000 0.00139 0.00165 0.00142 0.00124 0.00107 0.00120 0.00062 H18 -0.33120 0.38379 0.16872 1.00000 0.02636 0.00000 0.00000 C19 -0.03941 0.41228 0.10271 1.00000 0.01915 0.02015 0.00965 0.00387 -0.00174 0.00192 0.01641 0.00468 0.00044 0.00013 0.00023 0.00000 0.00135 0.00142 0.00125 0.00107 0.00098 0.00107 0.00056 N1 0.28389 0.44449 0.02354 1.00000 0.02049 0.02535 0.01203 0.00022 0.00391 -0.00437 0.01918 0.00403 0.00038 0.00012 0.00020 0.00000 0.00120 0.00134 0.00115 0.00096 0.00091 0.00098 0.00051 O1 0.39974 0.52297 0.15104 1.00000 0.03062 0.02978 0.01522 0.00199 -0.00057 -0.01086 0.02527 0.00346 0.00034 0.00010 0.00017 0.00000 0.00112 0.00120 0.00101 0.00089 0.00082 0.00093 0.00048 Fe1 0.31143 0.35641 0.49933 1.00000 0.02014 0.02183 0.00807 0.00111 0.00071 0.00111 0.01668 0.00067 0.00006 0.00002 0.00003 0.00000 0.00024 0.00024 0.00022 0.00016 0.00014 0.00016 0.00015 H1N 0.39865 0.44761 -0.03104 1.00000 0.02002 0.05172 0.00387 0.00143 0.00220 0.00000 0.00000 Final Structure Factor Calculation for 2009src1151 in P2(1)/c Total number of l.s. parameters = 202 Maximum vector length = 511 Memory required = 4251 / 24017 wR2 = 0.1253 before cycle 11 for 3347 data and 0 / 202 parameters Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.047 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.046; Restrained GooF = 1.047 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0556 * P )^2 + 1.35 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0505 for 2562 Fo > 4sig(Fo) and 0.0713 for all 3347 data wR2 = 0.1253, GooF = S = 1.046, Restrained GooF = 1.047 for all data Occupancy sum of asymmetric unit = 22.00 for non-hydrogen and 17.00 for hydrogen atoms Principal mean square atomic displacements U 0.0397 0.0223 0.0130 C1 0.0641 0.0233 0.0077 C2 0.0681 0.0245 0.0099 C3 0.0492 0.0233 0.0097 C4 0.0318 0.0226 0.0119 C5 0.0277 0.0234 0.0108 C6 0.0406 0.0181 0.0113 C7 0.0410 0.0186 0.0125 C8 0.0324 0.0196 0.0094 C9 0.0251 0.0195 0.0083 C10 0.0243 0.0211 0.0099 C11 0.0223 0.0192 0.0125 C12 0.0278 0.0254 0.0070 C13 0.0231 0.0204 0.0095 C14 0.0275 0.0227 0.0113 C15 0.0334 0.0215 0.0165 C16 0.0351 0.0201 0.0182 C17 0.0321 0.0183 0.0154 C18 0.0219 0.0196 0.0078 C19 0.0280 0.0189 0.0107 N1 0.0415 0.0194 0.0150 O1 0.0224 0.0196 0.0080 Fe1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.015 0.027 0.041 0.057 0.074 0.095 0.116 0.148 0.201 1.000 Number in group 366. 315. 324. 340. 327. 347. 327. 338. 326. 337. GooF 0.990 0.954 1.003 1.150 1.116 1.125 1.049 0.978 0.996 1.072 K 3.345 1.258 0.991 1.000 0.995 1.013 1.021 1.003 1.008 1.017 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.66 inf Number in group 338. 341. 332. 336. 326. 339. 333. 332. 335. 335. GooF 1.085 1.049 1.117 0.950 0.922 0.973 0.949 0.826 1.096 1.386 K 1.011 1.062 1.017 1.025 1.028 1.015 1.020 1.015 1.027 1.001 R1 0.171 0.151 0.123 0.081 0.069 0.058 0.050 0.040 0.039 0.041 Recommended weighting scheme: WGHT 0.0552 1.4130 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) -7 3 3 351.89 1.89 5.24 0.007 0.84 -6 2 3 552.41 263.62 4.83 0.084 0.97 -7 1 6 179.76 2.68 4.28 0.008 0.80 -3 5 2 166.76 89.96 4.19 0.049 1.75 -2 1 14 482.97 892.66 3.94 0.154 0.79 -7 6 2 254.39 60.54 3.93 0.040 0.83 3 0 2 862.70 1143.11 3.64 0.175 1.85 1 7 14 -22.15 95.40 3.63 0.051 0.77 -6 2 8 168.44 1.37 3.54 0.006 0.83 2 11 1 85.90 145.70 3.49 0.062 1.61 -2 1 3 355.92 260.36 3.42 0.083 2.40 -7 2 4 103.50 8.63 3.42 0.015 0.83 -3 19 4 71.12 2.32 3.31 0.008 0.94 3 6 2 66.31 117.04 3.26 0.056 1.65 -2 1 13 1320.40 2099.91 3.25 0.237 0.85 -5 2 7 384.37 232.31 3.22 0.079 0.98 2 8 3 117.63 72.22 3.17 0.044 1.74 0 3 4 446.97 336.41 3.14 0.095 2.64 -1 2 6 1025.64 817.64 3.10 0.148 1.80 3 5 2 37.00 74.50 3.10 0.045 1.70 6 14 1 139.15 39.18 3.10 0.032 0.83 3 1 1 461.14 594.71 3.09 0.126 1.94 5 3 10 107.54 196.41 3.09 0.072 0.80 -7 0 4 162.74 6.16 3.08 0.013 0.83 0 19 10 127.06 248.07 3.07 0.081 0.80 0 14 0 333.15 462.41 3.02 0.111 1.54 -1 6 14 47.15 210.97 3.02 0.075 0.79 -2 18 9 -8.86 73.01 3.00 0.044 0.84 0 0 4 6547.64 5347.50 2.99 0.378 2.83 1 1 0 13694.84 16974.83 2.98 0.674 5.77 -6 5 6 447.43 303.81 2.98 0.090 0.88 0 3 3 2929.62 2392.19 2.91 0.253 3.34 1 16 6 134.67 223.45 2.90 0.077 1.07 4 2 3 390.05 505.04 2.89 0.116 1.36 5 6 10 225.16 361.12 2.88 0.098 0.78 0 8 6 332.23 437.97 2.88 0.108 1.55 0 2 3 228.54 165.98 2.88 0.067 3.56 -1 1 7 1374.28 1123.99 2.85 0.173 1.58 6 3 1 144.27 61.86 2.83 0.041 0.98 1 4 6 2484.82 2057.99 2.81 0.235 1.69 7 1 2 560.73 274.85 2.80 0.086 0.84 -7 7 4 102.85 8.88 2.80 0.015 0.80 0 10 1 215.43 152.50 2.78 0.064 2.11 -6 3 7 134.00 3.89 2.73 0.010 0.86 3 5 0 65.46 40.19 2.68 0.033 1.81 1 12 1 356.45 462.41 2.68 0.111 1.69 4 2 1 505.38 642.64 2.68 0.131 1.46 -2 9 2 1552.12 1890.78 2.67 0.225 1.79 -4 3 7 60.70 5.62 2.66 0.012 1.12 1 1 7 455.19 354.98 2.66 0.097 1.54 Bond lengths and angles C1 - Distance Angles C5 1.4059 (0.0045) C2 1.4178 (0.0046) 107.72 (0.27) Fe1 2.0517 (0.0029) 69.88 (0.16) 69.29 (0.17) H1 0.9500 126.14 126.14 126.26 C1 - C5 C2 Fe1 C2 - Distance Angles C1 1.4178 (0.0046) C3 1.4318 (0.0050) 107.75 (0.28) Fe1 2.0402 (0.0030) 70.16 (0.17) 69.86 (0.18) H2 0.9500 126.12 126.12 125.44 C2 - C1 C3 Fe1 C3 - Distance Angles C4 1.4101 (0.0047) C2 1.4318 (0.0050) 107.80 (0.27) Fe1 2.0495 (0.0030) 70.05 (0.17) 69.16 (0.17) H3 0.9500 126.10 126.10 126.27 C3 - C4 C2 Fe1 C4 - Distance Angles C3 1.4101 (0.0047) C5 1.4147 (0.0043) 107.80 (0.28) Fe1 2.0534 (0.0029) 69.75 (0.18) 69.70 (0.17) H4 0.9500 126.10 126.10 126.03 C4 - C3 C5 Fe1 C5 - Distance Angles C1 1.4059 (0.0045) C4 1.4147 (0.0043) 108.93 (0.27) Fe1 2.0498 (0.0028) 70.03 (0.16) 69.97 (0.17) H5 0.9500 125.54 125.54 126.05 C5 - C1 C4 Fe1 C6 - Distance Angles C7 1.4268 (0.0040) C10 1.4286 (0.0041) 108.36 (0.25) Fe1 2.0539 (0.0027) 69.15 (0.16) 70.16 (0.15) H6 0.9500 125.82 125.82 126.44 C6 - C7 C10 Fe1 C7 - Distance Angles C6 1.4268 (0.0040) C8 1.4287 (0.0044) 108.13 (0.27) Fe1 2.0416 (0.0028) 70.08 (0.16) 69.47 (0.17) H7 0.9500 125.94 125.94 126.09 C7 - C6 C8 Fe1 C8 - Distance Angles C9 1.4228 (0.0041) C7 1.4287 (0.0044) 107.43 (0.25) Fe1 2.0405 (0.0029) 69.67 (0.16) 69.55 (0.16) H8 0.9500 126.28 126.29 126.07 C8 - C9 C7 Fe1 C9 - Distance Angles C8 1.4228 (0.0041) C10 1.4291 (0.0038) 108.97 (0.26) Fe1 2.0423 (0.0028) 69.54 (0.17) 70.54 (0.16) H9 0.9500 125.52 125.52 125.99 C9 - C8 C10 Fe1 C10 - Distance Angles C6 1.4286 (0.0041) C9 1.4291 (0.0038) 107.11 (0.24) C11 1.5005 (0.0038) 127.41 (0.25) 125.47 (0.26) Fe1 2.0659 (0.0027) 69.26 (0.15) 68.76 (0.15) 127.51 (0.19) C10 - C6 C9 C11 C11 - Distance Angles C10 1.5005 (0.0038) C12 1.5455 (0.0036) 113.76 (0.23) H11A 0.9900 108.81 108.81 H11B 0.9900 108.81 108.81 107.68 C11 - C10 C12 H11A C12 - Distance Angles C19 1.5138 (0.0038) C13 1.5268 (0.0040) 102.44 (0.22) C11 1.5455 (0.0036) 116.14 (0.23) 113.39 (0.22) H12 1.0000 108.16 108.16 108.16 C12 - C19 C13 C11 C13 - Distance Angles O1 1.2313 (0.0034) N1 1.3639 (0.0037) 125.42 (0.27) C12 1.5268 (0.0040) 126.30 (0.27) 108.28 (0.24) C13 - O1 N1 C14 - Distance Angles C15 1.3828 (0.0040) C19 1.3937 (0.0039) 122.70 (0.26) N1 1.4099 (0.0036) 127.88 (0.26) 109.42 (0.24) C14 - C15 C19 C15 - Distance Angles C14 1.3828 (0.0040) C16 1.3959 (0.0041) 116.97 (0.26) H15 0.9500 121.52 121.52 C15 - C14 C16 C16 - Distance Angles C17 1.3852 (0.0043) C15 1.3959 (0.0041) 121.43 (0.27) H16 0.9500 119.28 119.28 C16 - C17 C15 C17 - Distance Angles C16 1.3852 (0.0043) C18 1.4064 (0.0043) 120.48 (0.27) H17 0.9500 119.76 119.76 C17 - C16 C18 C18 - Distance Angles C19 1.3792 (0.0039) C17 1.4064 (0.0043) 118.61 (0.27) H18 0.9500 120.70 120.70 C18 - C19 C17 C19 - Distance Angles C18 1.3792 (0.0039) C14 1.3937 (0.0039) 119.81 (0.26) C12 1.5138 (0.0038) 131.68 (0.25) 108.48 (0.23) C19 - C18 C14 N1 - Distance Angles C13 1.3639 (0.0037) C14 1.4099 (0.0036) 111.35 (0.23) H1N 0.9527 (0.0174) 124.45 (1.85) 124.13 (1.83) N1 - C13 C14 O1 - Distance Angles C13 1.2313 (0.0034) O1 - Fe1 - Distance Angles C2 2.0402 (0.0030) C8 2.0405 (0.0030) 117.79 (0.12) C7 2.0416 (0.0028) 107.33 (0.13) 40.97 (0.12) C9 2.0423 (0.0028) 152.12 (0.13) 40.79 (0.12) 68.51 (0.12) C3 2.0495 (0.0031) 40.99 (0.14) 106.91 (0.12) 127.05 (0.13) 118.16 (0.13) C5 2.0498 (0.0028) 67.77 (0.12) 165.33 (0.13) 153.10 (0.13) 128.41 (0.12) 67.67 (0.12) C1 2.0517 (0.0029) 40.55 (0.13) 152.33 (0.12) 118.84 (0.13) 165.95 (0.12) 68.28 (0.13) 40.09 (0.12) C4 2.0534 (0.0029) 68.24 (0.14) 126.89 (0.12) 164.75 (0.12) 108.15 (0.12) 40.20 (0.13) 40.34 (0.12) 67.99 (0.12) C6 2.0539 (0.0027) 127.57 (0.13) 68.76 (0.12) 40.77 (0.11) 68.28 (0.12) 165.45 (0.14) 119.88 (0.12) 108.70 (0.12) C10 2.0659 (0.0027) 165.64 (0.13) 68.84 (0.11) 68.62 (0.11) 40.71 (0.11) 152.33 (0.13) 109.20 (0.11) 128.20 (0.11) Fe1 - C2 C8 C7 C9 C3 C5 C1 Selected torsion angles 0.46 ( 0.32) C5 - C1 - C2 - C3 60.01 ( 0.21) Fe1 - C1 - C2 - C3 -59.55 ( 0.19) C5 - C1 - C2 - Fe1 -0.59 ( 0.34) C1 - C2 - C3 - C4 59.62 ( 0.21) Fe1 - C2 - C3 - C4 -60.20 ( 0.20) C1 - C2 - C3 - Fe1 0.48 ( 0.34) C2 - C3 - C4 - C5 59.54 ( 0.20) Fe1 - C3 - C4 - C5 -59.06 ( 0.21) C2 - C3 - C4 - Fe1 -0.17 ( 0.31) C2 - C1 - C5 - C4 -59.34 ( 0.20) Fe1 - C1 - C5 - C4 59.18 ( 0.20) C2 - C1 - C5 - Fe1 -0.20 ( 0.32) C3 - C4 - C5 - C1 59.38 ( 0.19) Fe1 - C4 - C5 - C1 -59.58 ( 0.21) C3 - C4 - C5 - Fe1 0.13 ( 0.32) C10 - C6 - C7 - C8 -59.27 ( 0.20) Fe1 - C6 - C7 - C8 59.40 ( 0.19) C10 - C6 - C7 - Fe1 0.02 ( 0.32) C6 - C7 - C8 - C9 -59.62 ( 0.20) Fe1 - C7 - C8 - C9 59.64 ( 0.20) C6 - C7 - C8 - Fe1 -0.17 ( 0.32) C7 - C8 - C9 - C10 -59.72 ( 0.19) Fe1 - C8 - C9 - C10 59.55 ( 0.20) C7 - C8 - C9 - Fe1 -0.24 ( 0.30) C7 - C6 - C10 - C9 58.54 ( 0.19) Fe1 - C6 - C10 - C9 179.22 ( 0.26) C7 - C6 - C10 - C11 -122.01 ( 0.27) Fe1 - C6 - C10 - C11 -58.77 ( 0.19) C7 - C6 - C10 - Fe1 0.25 ( 0.31) C8 - C9 - C10 - C6 -58.85 ( 0.19) Fe1 - C9 - C10 - C6 -179.22 ( 0.25) C8 - C9 - C10 - C11 121.68 ( 0.27) Fe1 - C9 - C10 - C11 59.10 ( 0.20) C8 - C9 - C10 - Fe1 -75.88 ( 0.35) C6 - C10 - C11 - C12 103.48 ( 0.31) C9 - C10 - C11 - C12 -167.32 ( 0.19) Fe1 - C10 - C11 - C12 61.71 ( 0.31) C10 - C11 - C12 - C19 -56.57 ( 0.32) C10 - C11 - C12 - C13 -178.83 ( 0.26) C19 - C12 - C13 - O1 -52.88 ( 0.38) C11 - C12 - C13 - O1 1.54 ( 0.28) C19 - C12 - C13 - N1 127.49 ( 0.24) C11 - C12 - C13 - N1 0.66 ( 0.41) C19 - C14 - C15 - C16 -178.62 ( 0.26) N1 - C14 - C15 - C16 -0.12 ( 0.43) C14 - C15 - C16 - C17 -0.12 ( 0.46) C15 - C16 - C17 - C18 -0.15 ( 0.44) C16 - C17 - C18 - C19 0.67 ( 0.41) C17 - C18 - C19 - C14 178.30 ( 0.27) C17 - C18 - C19 - C12 -0.95 ( 0.41) C15 - C14 - C19 - C18 178.44 ( 0.24) N1 - C14 - C19 - C18 -179.09 ( 0.24) C15 - C14 - C19 - C12 0.31 ( 0.30) N1 - C14 - C19 - C12 -178.93 ( 0.28) C13 - C12 - C19 - C18 56.93 ( 0.39) C11 - C12 - C19 - C18 -1.10 ( 0.27) C13 - C12 - C19 - C14 -125.23 ( 0.25) C11 - C12 - C19 - C14 178.90 ( 0.26) O1 - C13 - N1 - C14 -1.47 ( 0.30) C12 - C13 - N1 - C14 -179.89 ( 0.27) C15 - C14 - N1 - C13 0.75 ( 0.31) C19 - C14 - N1 - C13 -157.52 ( 0.18) C1 - C2 - Fe1 - C8 83.96 ( 0.21) C3 - C2 - Fe1 - C8 -114.37 ( 0.19) C1 - C2 - Fe1 - C7 127.10 ( 0.19) C3 - C2 - Fe1 - C7 168.99 ( 0.23) C1 - C2 - Fe1 - C9 50.46 ( 0.34) C3 - C2 - Fe1 - C9 118.53 ( 0.27) C1 - C2 - Fe1 - C3 37.48 ( 0.18) C1 - C2 - Fe1 - C5 -81.05 ( 0.20) C3 - C2 - Fe1 - C5 -118.53 ( 0.27) C3 - C2 - Fe1 - C1 81.13 ( 0.20) C1 - C2 - Fe1 - C4 -37.40 ( 0.19) C3 - C2 - Fe1 - C4 -73.91 ( 0.22) C1 - C2 - Fe1 - C6 167.57 ( 0.18) C3 - C2 - Fe1 - C6 -43.10 ( 0.55) C1 - C2 - Fe1 - C10 -161.63 ( 0.43) C3 - C2 - Fe1 - C10 -156.73 ( 0.18) C9 - C8 - Fe1 - C2 84.64 ( 0.20) C7 - C8 - Fe1 - C2 118.62 ( 0.24) C9 - C8 - Fe1 - C7 -118.62 ( 0.24) C7 - C8 - Fe1 - C9 -113.76 ( 0.19) C9 - C8 - Fe1 - C3 127.62 ( 0.19) C7 - C8 - Fe1 - C3 -47.78 ( 0.51) C9 - C8 - Fe1 - C5 -166.40 ( 0.41) C7 - C8 - Fe1 - C5 170.90 ( 0.23) C9 - C8 - Fe1 - C1 52.28 ( 0.32) C7 - C8 - Fe1 - C1 -74.11 ( 0.21) C9 - C8 - Fe1 - C4 167.27 ( 0.17) C7 - C8 - Fe1 - C4 80.95 ( 0.18) C9 - C8 - Fe1 - C6 -37.68 ( 0.17) C7 - C8 - Fe1 - C6 37.28 ( 0.16) C9 - C8 - Fe1 - C10 -81.34 ( 0.18) C7 - C8 - Fe1 - C10 128.04 ( 0.19) C6 - C7 - Fe1 - C2 -112.68 ( 0.19) C8 - C7 - Fe1 - C2 -119.28 ( 0.25) C6 - C7 - Fe1 - C8 -81.23 ( 0.19) C6 - C7 - Fe1 - C9 38.05 ( 0.16) C8 - C7 - Fe1 - C9 169.00 ( 0.18) C6 - C7 - Fe1 - C3 -71.73 ( 0.22) C8 - C7 - Fe1 - C3 53.16 ( 0.33) C6 - C7 - Fe1 - C5 172.44 ( 0.24) C8 - C7 - Fe1 - C5 85.51 ( 0.20) C6 - C7 - Fe1 - C1 -155.21 ( 0.17) C8 - C7 - Fe1 - C1 -161.33 ( 0.43) C6 - C7 - Fe1 - C4 -42.06 ( 0.54) C8 - C7 - Fe1 - C4 119.28 ( 0.25) C8 - C7 - Fe1 - C6 -37.35 ( 0.17) C6 - C7 - Fe1 - C10 81.93 ( 0.18) C8 - C7 - Fe1 - C10 48.36 ( 0.33) C8 - C9 - Fe1 - C2 168.35 ( 0.25) C10 - C9 - Fe1 - C2 119.99 ( 0.24) C10 - C9 - Fe1 - C8 -38.21 ( 0.17) C8 - C9 - Fe1 - C7 81.77 ( 0.18) C10 - C9 - Fe1 - C7 83.37 ( 0.21) C8 - C9 - Fe1 - C3 -156.64 ( 0.17) C10 - C9 - Fe1 - C3 166.15 ( 0.17) C8 - C9 - Fe1 - C5 -73.86 ( 0.20) C10 - C9 - Fe1 - C5 -162.40 ( 0.44) C8 - C9 - Fe1 - C1 -42.41 ( 0.54) C10 - C9 - Fe1 - C1 125.96 ( 0.18) C8 - C9 - Fe1 - C4 -114.05 ( 0.18) C10 - C9 - Fe1 - C4 -82.22 ( 0.18) C8 - C9 - Fe1 - C6 37.76 ( 0.16) C10 - C9 - Fe1 - C6 -119.99 ( 0.24) C8 - C9 - Fe1 - C10 -119.09 ( 0.26) C4 - C3 - Fe1 - C2 127.76 ( 0.18) C4 - C3 - Fe1 - C8 -113.15 ( 0.19) C2 - C3 - Fe1 - C8 168.36 ( 0.18) C4 - C3 - Fe1 - C7 -72.55 ( 0.23) C2 - C3 - Fe1 - C7 85.05 ( 0.20) C4 - C3 - Fe1 - C9 -155.85 ( 0.18) C2 - C3 - Fe1 - C9 -37.76 ( 0.18) C4 - C3 - Fe1 - C5 81.33 ( 0.20) C2 - C3 - Fe1 - C5 -81.16 ( 0.19) C4 - C3 - Fe1 - C1 37.93 ( 0.18) C2 - C3 - Fe1 - C1 119.09 ( 0.26) C2 - C3 - Fe1 - C4 -161.89 ( 0.43) C4 - C3 - Fe1 - C6 -42.79 ( 0.55) C2 - C3 - Fe1 - C6 51.21 ( 0.33) C4 - C3 - Fe1 - C10 170.31 ( 0.22) C2 - C3 - Fe1 - C10 -37.89 ( 0.19) C1 - C5 - Fe1 - C2 82.10 ( 0.21) C4 - C5 - Fe1 - C2 -153.22 ( 0.42) C1 - C5 - Fe1 - C8 -33.23 ( 0.53) C4 - C5 - Fe1 - C8 46.70 ( 0.33) C1 - C5 - Fe1 - C7 166.69 ( 0.24) C4 - C5 - Fe1 - C7 168.66 ( 0.17) C1 - C5 - Fe1 - C9 -71.36 ( 0.22) C4 - C5 - Fe1 - C9 -82.35 ( 0.20) C1 - C5 - Fe1 - C3 37.64 ( 0.19) C4 - C5 - Fe1 - C3 119.99 ( 0.25) C4 - C5 - Fe1 - C1 -119.99 ( 0.25) C1 - C5 - Fe1 - C4 83.77 ( 0.20) C1 - C5 - Fe1 - C6 -156.24 ( 0.18) C4 - C5 - Fe1 - C6 127.10 ( 0.17) C1 - C5 - Fe1 - C10 -112.91 ( 0.19) C4 - C5 - Fe1 - C10 119.01 ( 0.26) C5 - C1 - Fe1 - C2 165.78 ( 0.23) C5 - C1 - Fe1 - C8 46.76 ( 0.33) C2 - C1 - Fe1 - C8 -157.92 ( 0.17) C5 - C1 - Fe1 - C7 83.07 ( 0.21) C2 - C1 - Fe1 - C7 -39.40 ( 0.54) C5 - C1 - Fe1 - C9 -158.42 ( 0.44) C2 - C1 - Fe1 - C9 80.68 ( 0.19) C5 - C1 - Fe1 - C3 -38.34 ( 0.20) C2 - C1 - Fe1 - C3 -119.01 ( 0.26) C2 - C1 - Fe1 - C5 37.21 ( 0.17) C5 - C1 - Fe1 - C4 -81.81 ( 0.21) C2 - C1 - Fe1 - C4 -114.50 ( 0.17) C5 - C1 - Fe1 - C6 126.49 ( 0.19) C2 - C1 - Fe1 - C6 -73.44 ( 0.21) C5 - C1 - Fe1 - C10 167.55 ( 0.19) C2 - C1 - Fe1 - C10 38.10 ( 0.19) C3 - C4 - Fe1 - C2 -80.84 ( 0.20) C5 - C4 - Fe1 - C2 -71.05 ( 0.23) C3 - C4 - Fe1 - C8 170.01 ( 0.17) C5 - C4 - Fe1 - C8 -37.74 ( 0.54) C3 - C4 - Fe1 - C7 -156.68 ( 0.43) C5 - C4 - Fe1 - C7 -112.44 ( 0.19) C3 - C4 - Fe1 - C9 128.62 ( 0.18) C5 - C4 - Fe1 - C9 -118.94 ( 0.27) C5 - C4 - Fe1 - C3 118.94 ( 0.27) C3 - C4 - Fe1 - C5 81.95 ( 0.20) C3 - C4 - Fe1 - C1 -36.99 ( 0.18) C5 - C4 - Fe1 - C1 169.99 ( 0.25) C3 - C4 - Fe1 - C6 51.05 ( 0.35) C5 - C4 - Fe1 - C6 -155.49 ( 0.18) C3 - C4 - Fe1 - C10 85.57 ( 0.20) C5 - C4 - Fe1 - C10 -71.54 ( 0.22) C7 - C6 - Fe1 - C2 168.74 ( 0.17) C10 - C6 - Fe1 - C2 37.86 ( 0.18) C7 - C6 - Fe1 - C8 -81.87 ( 0.18) C10 - C6 - Fe1 - C8 -119.72 ( 0.25) C10 - C6 - Fe1 - C7 81.84 ( 0.19) C7 - C6 - Fe1 - C9 -37.88 ( 0.16) C10 - C6 - Fe1 - C9 -37.33 ( 0.55) C7 - C6 - Fe1 - C3 -157.05 ( 0.45) C10 - C6 - Fe1 - C3 -155.32 ( 0.18) C7 - C6 - Fe1 - C5 84.96 ( 0.19) C10 - C6 - Fe1 - C5 -112.79 ( 0.19) C7 - C6 - Fe1 - C1 127.49 ( 0.17) C10 - C6 - Fe1 - C1 169.20 ( 0.25) C7 - C6 - Fe1 - C4 49.48 ( 0.33) C10 - C6 - Fe1 - C4 119.72 ( 0.25) C7 - C6 - Fe1 - C10 -38.61 ( 0.53) C6 - C10 - Fe1 - C2 -157.61 ( 0.44) C9 - C10 - Fe1 - C2 83.28 ( 0.54) C11 - C10 - Fe1 - C2 81.64 ( 0.18) C6 - C10 - Fe1 - C8 -37.35 ( 0.17) C9 - C10 - Fe1 - C8 -156.47 ( 0.28) C11 - C10 - Fe1 - C8 37.52 ( 0.17) C6 - C10 - Fe1 - C7 -81.47 ( 0.19) C9 - C10 - Fe1 - C7 159.41 ( 0.28) C11 - C10 - Fe1 - C7 119.00 ( 0.23) C6 - C10 - Fe1 - C9 -119.11 ( 0.32) C11 - C10 - Fe1 - C9 167.82 ( 0.24) C6 - C10 - Fe1 - C3 48.83 ( 0.32) C9 - C10 - Fe1 - C3 -70.29 ( 0.37) C11 - C10 - Fe1 - C3 -113.85 ( 0.18) C6 - C10 - Fe1 - C5 127.15 ( 0.18) C9 - C10 - Fe1 - C5 8.04 ( 0.28) C11 - C10 - Fe1 - C5 -73.03 ( 0.20) C6 - C10 - Fe1 - C1 167.97 ( 0.17) C9 - C10 - Fe1 - C1 48.86 ( 0.30) C11 - C10 - Fe1 - C1 -156.96 ( 0.17) C6 - C10 - Fe1 - C4 84.05 ( 0.19) C9 - C10 - Fe1 - C4 -35.07 ( 0.29) C11 - C10 - Fe1 - C4 -119.00 ( 0.23) C9 - C10 - Fe1 - C6 121.89 ( 0.31) C11 - C10 - Fe1 - C6 FMAP and GRID set by program FMAP 2 1 16 GRID -3.846 24 -2 3.846 1 2 R1 = 0.0698 for 3347 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.62 at 0.4635 0.3678 0.4979 [ 0.95 A from FE1 ] Deepest hole -0.74 at 0.3427 0.3319 0.5549 [ 0.84 A from FE1 ] Mean = 0.00, Rms deviation from mean = 0.10 e/A^3, Highest memory used = 4717 / 28992 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4635 0.3678 0.4979 1.00000 0.05 0.62 0.95 FE1 1.40 C8 1.58 C9 1.91 H8 Q2 1 0.3154 0.3117 0.5017 1.00000 0.05 0.62 0.96 FE1 1.62 C2 1.74 C7 1.87 C1 Q3 1 0.1311 0.3571 0.5047 1.00000 0.05 0.57 1.09 FE1 1.40 C5 1.47 C1 1.87 H5 Q4 1 -0.3108 0.4304 -0.0030 1.00000 0.05 0.38 1.75 C18 1.80 H1N 2.01 O1 2.01 C19 Q5 1 -0.1371 0.4104 0.0975 1.00000 0.05 0.36 0.59 C19 0.92 C18 1.56 H18 1.79 C14 Q6 1 0.3560 0.4412 0.0026 1.00000 0.05 0.35 0.49 H1N 0.51 N1 1.70 C13 1.74 C14 Q7 1 0.1978 0.4222 0.0181 1.00000 0.05 0.34 0.70 N1 0.71 C14 1.46 H1N 1.76 C13 Q8 1 -0.0189 0.3294 -0.0731 1.00000 0.05 0.33 0.68 C16 0.79 C15 1.30 H16 1.42 H15 Q9 1 0.1585 0.3840 0.6735 1.00000 0.05 0.33 0.84 C5 0.92 C4 1.61 H5 1.69 H4 Q10 1 0.2620 0.4093 0.0189 1.00000 0.05 0.33 0.77 N1 0.95 C14 1.31 H1N 1.90 C15 Q11 1 -0.1772 0.3493 0.6166 1.00000 0.05 0.32 1.47 H5 1.60 H1 1.66 C5 1.72 C1 Q12 1 0.1497 0.4778 0.1648 1.00000 0.05 0.31 0.67 C12 0.90 C13 1.33 H12 1.80 O1 Q13 1 0.6957 0.3817 0.6608 1.00000 0.05 0.31 1.03 H3 1.74 C3 1.80 H5 2.36 C5 Q14 1 0.4734 0.4970 0.1760 1.00000 0.05 0.31 0.76 O1 1.41 C13 2.20 H1N 2.31 N1 Q15 1 0.2225 0.3740 0.3232 1.00000 0.05 0.30 0.65 C10 0.82 C6 1.50 H6 1.83 C9 Q16 1 0.0072 0.4137 0.0393 1.00000 0.05 0.30 0.72 C14 0.79 C19 1.81 N1 1.82 C15 Q17 1 -0.0393 0.4834 0.1757 1.00000 0.05 0.30 0.40 H12 0.66 C12 1.74 C19 1.81 C11 Q18 1 0.0739 0.3614 -0.1021 1.00000 0.05 0.30 0.35 C15 0.72 H15 1.55 C16 1.57 C14 Q19 1 -0.5733 0.3190 0.0012 1.00000 0.05 0.29 1.07 H17 1.82 C17 2.22 H15 2.36 H7 Q20 1 0.0744 0.4328 0.6670 1.00000 0.05 0.29 1.25 H5 1.25 C5 1.41 C4 1.52 H4 Shortest distances between peaks (including symmetry equivalents) 7 10 0.47 6 10 0.91 8 18 0.95 6 7 1.06 5 16 1.12 12 17 1.15 9 20 1.17 11 13 1.17 7 16 1.19 2 3 1.48 1 2 1.50 10 16 1.56 4 5 1.56 5 17 1.88 4 16 1.98 12 14 1.98 3 9 2.00 7 18 2.01 1 3 2.01 10 18 2.01 4 6 2.02 16 18 2.02 7 12 2.08 12 16 2.13 16 17 2.18 3 15 2.19 10 19 2.19 9 11 2.21 8 16 2.22 6 16 2.24 5 7 2.26 1 13 2.28 3 11 2.30 10 12 2.34 5 12 2.35 6 14 2.38 1 15 2.40 11 20 2.40 6 12 2.40 2 15 2.47 3 20 2.49 1 11 2.51 13 20 2.52 18 19 2.54 17 20 2.55 7 8 2.57 8 10 2.59 5 10 2.60 7 19 2.62 4 10 2.63 6 18 2.65 4 14 2.65 6 19 2.66 9 18 2.67 6 14 2.67 7 17 2.69 2 9 2.70 5 8 2.73 8 19 2.77 9 13 2.77 4 6 2.78 4 17 2.78 1 9 2.80 10 14 2.85 4 14 2.85 5 18 2.85 7 14 2.87 4 19 2.87 12 15 2.88 2 19 2.89 4 12 2.90 4 8 2.93 14 17 2.94 4 7 2.98 Time profile in seconds ----------------------- 0.00: 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. 0.67: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.00: Structure factors and derivatives 1.55: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.14: Apply other restraints 0.27: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src1151 finished at 16:38:14 Total CPU time: 3.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++