+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 17:53:56 on 02-Aug-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P2(1)2(1)2(1) CELL 0.71069 7.5921 14.9902 15.3720 90.00 90.00 90.00 ZERR 4 0.0011 0.0009 0.002 0 0 0 LATT -1 SYMM .5-X, -Y, .5+Z SYMM -X, .5+Y, .5-Z SYMM .5+X, .5-Y, -Z SFAC C H N FE UNIT 88 72 8 4 V = 1749.44 F(000) = 760.0 Mu = 0.87 mm-1 Cell Wt = 1464.94 Rho = 1.390 TEMP -123 L.S. 4 ISOR 0.008 0.008 C6 C9 C10 FMAP 2 PLAN 10 CONF MPLA 5 C1 > C5 FE1 C11 C12 C13 C18 MPLA 5 C6 > C10 FE1 MPLA 6 N1 C13 > C17 C12 MPLA 6 N2 C18 > C22 C12 WGHT 0.025200 FVAR 2.28321 MOVE -.5 -.5 0 1 FE1 4 0.87931 0.57887 0.02633 11.00000 0.01910 0.02285 = 0.03754 -0.00141 0.00676 -0.00279 N1 3 1.07015 0.59122 0.29159 11.00000 0.02546 0.02899 = 0.01967 0.00380 -0.00186 0.00829 N2 3 0.73022 0.83678 0.28120 11.00000 0.04454 0.02571 = 0.02696 0.00352 0.00880 0.01273 C1 1 0.98813 0.68929 0.08021 11.00000 0.01267 0.01787 = 0.02597 0.00164 0.00338 0.00015 C2 1 1.11133 0.61877 0.07745 11.00000 0.02121 0.02775 = 0.02037 0.00078 0.00365 -0.00653 AFIX 43 H2 2 1.16817 0.59327 0.12657 11.00000 -1.20000 AFIX 0 C3 1 1.13708 0.59185 -0.01057 11.00000 0.01708 0.03058 = 0.02709 0.00219 0.00503 -0.00692 AFIX 43 H3 2 1.21318 0.54595 -0.03067 11.00000 -1.20000 AFIX 0 C4 1 1.02686 0.64696 -0.06241 11.00000 0.02541 0.01953 = 0.02518 -0.00252 -0.00194 -0.00185 AFIX 43 H4 2 1.01564 0.64433 -0.12391 11.00000 -1.20000 AFIX 0 C5 1 0.93676 0.70638 -0.00657 11.00000 0.01859 0.03264 = 0.02415 0.00120 -0.00366 -0.00208 AFIX 43 H5 2 0.85491 0.75066 -0.02449 11.00000 -1.20000 AFIX 0 C6 1 0.78500 0.48068 0.10028 11.00000 0.07427 0.09069 = 0.08327 0.04392 -0.01256 -0.05291 AFIX 43 H6 2 0.84195 0.46051 0.15167 11.00000 -1.20000 AFIX 0 C7 1 0.80644 0.44848 0.01708 11.00000 0.03559 0.02491 = 0.11763 0.00111 0.01234 -0.01035 AFIX 43 H7 2 0.87921 0.39950 0.00138 11.00000 -1.20000 AFIX 0 C8 1 0.70852 0.49700 -0.03873 11.00000 0.03771 0.03458 = 0.09148 -0.01843 0.01379 -0.01569 AFIX 43 H8 2 0.70349 0.48861 -0.09994 11.00000 -1.20000 AFIX 0 C9 1 0.61965 0.55882 0.00600 11.00000 0.02353 0.05682 = 0.10340 -0.00113 0.00559 -0.01538 AFIX 43 H9 2 0.54160 0.60155 -0.01843 11.00000 -1.20000 AFIX 0 C10 1 0.65895 0.55080 0.09278 11.00000 0.07084 0.07531 = 0.09479 -0.04547 0.06836 -0.05127 AFIX 43 H10 2 0.61135 0.58531 0.13897 11.00000 -1.20000 AFIX 0 C11 1 0.91051 0.73621 0.15537 11.00000 0.01845 0.02294 = 0.02456 -0.00160 -0.00076 0.00219 AFIX 43 H11 2 0.81600 0.77554 0.14235 11.00000 -1.20000 AFIX 0 C12 1 0.95526 0.73083 0.23942 11.00000 0.01966 0.01961 = 0.01806 0.00019 0.00007 0.00015 C13 1 1.10505 0.67465 0.26835 11.00000 0.02006 0.02019 = 0.01824 -0.00223 0.00404 0.00452 C14 1 1.27459 0.71005 0.27063 11.00000 0.03095 0.03219 = 0.02684 0.00055 0.00249 -0.00166 AFIX 43 H14 2 1.29533 0.77091 0.25677 11.00000 -1.20000 AFIX 0 C15 1 1.41276 0.65389 0.29375 11.00000 0.01824 0.05194 = 0.03957 -0.00378 -0.00440 0.00600 AFIX 43 H15 2 1.53022 0.67569 0.29494 11.00000 -1.20000 AFIX 0 C16 1 1.37792 0.56693 0.31476 11.00000 0.03143 0.04723 = 0.02978 -0.00056 -0.00241 0.01492 AFIX 43 H16 2 1.47072 0.52757 0.33043 11.00000 -1.20000 AFIX 0 C17 1 1.20392 0.53703 0.31280 11.00000 0.04684 0.03670 = 0.02533 0.00367 -0.00179 0.00339 AFIX 43 H17 2 1.17955 0.47657 0.32688 11.00000 -1.20000 AFIX 0 C18 1 0.85161 0.77796 0.30753 11.00000 0.01439 0.01953 = 0.02574 -0.00280 0.00400 0.00290 C19 1 0.87734 0.75856 0.39575 11.00000 0.02120 0.04322 = 0.02467 -0.00328 0.00158 0.00549 AFIX 43 H19 2 0.96257 0.71547 0.41255 11.00000 -1.20000 AFIX 0 C20 1 0.77842 0.80222 0.45872 11.00000 0.03826 0.03209 = 0.03513 -0.00048 0.00844 -0.00214 AFIX 43 H20 2 0.79616 0.79048 0.51882 11.00000 -1.20000 AFIX 0 C21 1 0.65458 0.86267 0.43179 11.00000 0.03608 0.02650 = 0.03519 -0.00040 0.01682 0.00240 AFIX 43 H21 2 0.58326 0.89373 0.47255 11.00000 -1.20000 AFIX 0 C22 1 0.63661 0.87712 0.34275 11.00000 0.03973 0.03729 = 0.03576 -0.00231 0.00841 0.01756 AFIX 43 H22 2 0.55056 0.91918 0.32455 11.00000 -1.20000 HKLF 4 Covalent radii and connectivity table for s92 in P2(1)2(1)2(1) C 0.770 H 0.320 N 0.700 FE 1.240 Fe1 - C6 C10 C9 C2 C5 C1 C7 C4 C8 C3 N1 - C13 C17 N2 - C22 C18 C1 - C2 C5 C11 Fe1 C2 - C1 C3 Fe1 C3 - C4 C2 Fe1 C4 - C5 C3 Fe1 C5 - C1 C4 Fe1 C6 - C7 C10 Fe1 C7 - C8 C6 Fe1 C8 - C9 C7 Fe1 C9 - C8 C10 Fe1 C10 - C9 C6 Fe1 C11 - C12 C1 C12 - C11 C13 C18 C13 - N1 C14 C12 C14 - C15 C13 C15 - C16 C14 C16 - C15 C17 C17 - N1 C16 C18 - N2 C19 C12 C19 - C20 C18 C20 - C21 C19 C21 - C20 C22 C22 - N2 C21 7656 Reflections read, of which 21 rejected -8 =< h =< 7, -17 =< k =< 17, -17 =< l =< 16, Max. 2-theta = 50.09 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 2 1 0 14341.41 152.13 7 1134.85 1 2 0 110584.45 490.64 5 4470.35 1 3 0 137862.00 808.62 3 6687.34 -1 1 1 39531.41 233.04 8 2086.40 0 1 1 10630.12 162.26 4 2477.73 2 1 1 30386.55 330.64 5 2104.46 -1 2 1 56575.95 422.57 5 2228.29 0 2 1 23494.62 200.40 4 2699.65 1 2 1 54080.43 333.14 6 2108.76 0 3 1 62530.73 359.18 4 7842.73 -1 4 1 12773.69 341.23 3 1806.97 1 4 1 14336.71 474.72 2 2483.50 2 4 1 9581.45 315.89 3 2055.19 0 0 2 51497.17 615.22 2 8641.50 4 0 2 24631.35 311.95 6 2208.24 -1 1 2 107497.28 577.15 5 6953.13 1 1 2 107936.16 566.70 5 3874.82 3 1 2 17429.51 275.35 4 1581.94 -1 2 2 55395.64 648.77 3 3706.03 -2 5 2 2229.45 184.91 3 1029.65 -1 1 3 41943.82 446.54 4 5153.28 0 1 3 54627.86 692.62 2 26916.50 3 1 3 18574.62 334.42 5 1832.36 4 3 3 32318.89 301.54 5 1753.49 0 4 3 17226.76 393.65 3 3749.26 -1 5 3 19669.56 434.74 4 2255.71 0 1 4 57293.85 824.37 2 28909.50 0 7 4 22493.81 469.95 4 2666.64 0 8 4 30216.84 543.53 4 3121.73 1 0 5 16287.72 379.96 3 3151.74 1 2 5 36599.95 545.59 3 5573.43 4 2 5 17604.57 445.26 4 2246.92 -1 3 5 14586.56 468.95 3 2756.43 -2 1 7 34954.32 658.13 4 3776.16 2 1 7 34066.36 570.77 4 2866.83 35 Inconsistent equivalents 2717 Unique reflections, of which 0 suppressed R(int) = 0.0884 R(sigma) = 0.1224 Friedel opposites not merged Maximum memory for data reduction = 3591 / 27001 Default effective X-H distances for T = -123.0 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 = 4225 / 280070 wR2 = 0.0962 before cycle 1 for 2717 data and 226 / 226 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint -0.0439 0.0080 ISOR U23 C6 0.0529 0.0080 ISOR U12 C6 0.0377 0.0080 ISOR U11 C9 -0.0421 0.0080 ISOR U33 C9 0.0455 0.0080 ISOR U23 C10 -0.0684 0.0080 ISOR U13 C10 0.0513 0.0080 ISOR U12 C10 Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 18. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.008 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.032 0.000 GooF = S = 0.887; Restrained GooF = 0.929 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0252 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.28321 0.00468 0.001 OSF Mean shift/esd = 0.002 Maximum = -0.066 for y Fe1 Max. shift = 0.000 A for C18 Max. dU = 0.000 for C6 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4225 / 280070 wR2 = 0.0962 before cycle 2 for 2717 data and 226 / 226 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint -0.0439 0.0080 ISOR U23 C6 0.0529 0.0080 ISOR U12 C6 0.0377 0.0080 ISOR U11 C9 -0.0421 0.0080 ISOR U33 C9 0.0455 0.0080 ISOR U23 C10 -0.0684 0.0080 ISOR U13 C10 0.0513 0.0080 ISOR U12 C10 Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 18. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.008 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.032 0.000 GooF = S = 0.887; Restrained GooF = 0.929 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0252 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.28322 0.00468 0.000 OSF Mean shift/esd = 0.001 Maximum = -0.021 for y Fe1 Max. shift = 0.000 A for C18 Max. dU = 0.000 for C6 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4225 / 280070 wR2 = 0.0962 before cycle 3 for 2717 data and 226 / 226 parameters Disagreeable restraints before cycle 3 Observed Target Error Sigma Restraint -0.0439 0.0080 ISOR U23 C6 0.0529 0.0080 ISOR U12 C6 0.0377 0.0080 ISOR U11 C9 -0.0421 0.0080 ISOR U33 C9 0.0455 0.0080 ISOR U23 C10 -0.0683 0.0080 ISOR U13 C10 0.0513 0.0080 ISOR U12 C10 Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 18. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.008 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.032 0.000 GooF = S = 0.887; Restrained GooF = 0.929 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0252 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.28322 0.00468 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for U23 C10 Max. shift = 0.000 A for C6 Max. dU = 0.000 for C10 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4225 / 280070 wR2 = 0.0962 before cycle 4 for 2717 data and 226 / 226 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint -0.0439 0.0080 ISOR U23 C6 0.0529 0.0080 ISOR U12 C6 0.0377 0.0080 ISOR U11 C9 -0.0421 0.0080 ISOR U33 C9 0.0455 0.0080 ISOR U23 C10 -0.0683 0.0080 ISOR U13 C10 0.0513 0.0080 ISOR U12 C10 Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 18. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.008 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.032 0.000 GooF = S = 0.887; Restrained GooF = 0.929 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0252 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.28321 0.00468 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y C10 Max. shift = 0.000 A for C10 Max. dU = 0.000 for C10 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 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 0.6682 0.0933 0.1266 43 0.950 0.000 C2 C1 C3 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C3 ** H3 0.7132 0.0460 -0.0307 43 0.950 0.000 C3 C4 C2 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C4 ** H4 0.5156 0.1443 -0.1239 43 0.950 0.000 C4 C5 C3 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C5 ** H5 0.3549 0.2507 -0.0245 43 0.950 0.000 C5 C1 C4 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C6 ** H6 0.3419 -0.0395 0.1517 43 0.950 0.000 C6 C7 C10 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C7 ** H7 0.3792 -0.1005 0.0014 43 0.950 0.000 C7 C8 C6 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C8 ** H8 0.2035 -0.0114 -0.0999 43 0.950 0.000 C8 C9 C7 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C9 ** H9 0.0416 0.1016 -0.0184 43 0.950 0.000 C9 C8 C10 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C10 ** H10 0.1113 0.0853 0.1390 43 0.950 0.000 C10 C9 C6 H11 0.3160 0.2755 0.1423 43 0.950 0.000 C11 C12 C1 H14 0.7953 0.2709 0.2568 43 0.950 0.000 C14 C15 C13 H15 1.0302 0.1757 0.2949 43 0.950 0.000 C15 C16 C14 H16 0.9707 0.0276 0.3304 43 0.950 0.000 C16 C15 C17 H17 0.6796 -0.0234 0.3269 43 0.950 0.000 C17 N1 C16 H19 0.4626 0.2155 0.4125 43 0.950 0.000 C19 C20 C18 H20 0.2962 0.2905 0.5188 43 0.950 0.000 C20 C21 C19 H21 0.0833 0.3937 0.4725 43 0.950 0.000 C21 C20 C22 H22 0.0506 0.4192 0.3246 43 0.950 0.000 C22 N2 C21 s92 in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Fe1 0.37931 0.07887 0.02633 1.00000 0.01910 0.02285 0.03754 -0.00141 0.00676 -0.00279 0.02650 0.00125 0.00008 0.00005 0.00005 0.00000 0.00035 0.00039 0.00046 0.00041 0.00036 0.00036 0.00023 N1 0.57015 0.09122 0.29159 1.00000 0.02546 0.02898 0.01967 0.00380 -0.00186 0.00829 0.02470 0.00703 0.00044 0.00032 0.00027 0.00000 0.00239 0.00295 0.00256 0.00230 0.00173 0.00209 0.00106 N2 0.23022 0.33678 0.28120 1.00000 0.04454 0.02572 0.02696 0.00352 0.00880 0.01273 0.03241 0.00817 0.00054 0.00030 0.00030 0.00000 0.00273 0.00286 0.00287 0.00224 0.00235 0.00237 0.00116 C1 0.48813 0.18929 0.08021 1.00000 0.01267 0.01787 0.02597 0.00164 0.00338 0.00015 0.01884 0.00868 0.00057 0.00032 0.00036 0.00000 0.00257 0.00308 0.00363 0.00251 0.00219 0.00227 0.00123 C2 0.61133 0.11877 0.07745 1.00000 0.02121 0.02775 0.02037 0.00078 0.00365 -0.00653 0.02311 0.00842 0.00066 0.00032 0.00033 0.00000 0.00261 0.00297 0.00307 0.00225 0.00258 0.00278 0.00118 H2 0.66817 0.09327 0.12657 1.00000 0.02773 0.00000 0.00000 C3 0.63708 0.09185 -0.01057 1.00000 0.01708 0.03058 0.02709 0.00219 0.00503 -0.00692 0.02492 0.00805 0.00059 0.00035 0.00031 0.00000 0.00233 0.00318 0.00320 0.00256 0.00235 0.00273 0.00125 H3 0.71318 0.04595 -0.03067 1.00000 0.02990 0.00000 0.00000 C4 0.52686 0.14696 -0.06241 1.00000 0.02541 0.01953 0.02518 -0.00252 -0.00194 -0.00185 0.02337 0.00825 0.00059 0.00033 0.00035 0.00000 0.00282 0.00330 0.00360 0.00252 0.00228 0.00235 0.00133 H4 0.51564 0.14433 -0.12391 1.00000 0.02805 0.00000 0.00000 C5 0.43676 0.20638 -0.00657 1.00000 0.01859 0.03264 0.02415 0.00120 -0.00366 -0.00209 0.02513 0.00847 0.00057 0.00036 0.00034 0.00000 0.00270 0.00344 0.00363 0.00248 0.00207 0.00224 0.00141 H5 0.35491 0.25066 -0.02449 1.00000 0.03015 0.00000 0.00000 C6 0.28500 -0.01932 0.10028 1.00000 0.07428 0.09070 0.08328 0.04392 -0.01257 -0.05292 0.08275 0.01534 0.00105 0.00068 0.00063 0.00000 0.00470 0.00548 0.00561 0.00470 0.00422 0.00428 0.00271 H6 0.34195 -0.03949 0.15168 1.00000 0.09930 0.00000 0.00000 C7 0.30644 -0.05152 0.01708 1.00000 0.03558 0.02491 0.11765 0.00112 0.01233 -0.01035 0.05938 0.01254 0.00077 0.00041 0.00061 0.00000 0.00336 0.00398 0.00759 0.00441 0.00403 0.00268 0.00224 H7 0.37921 -0.10050 0.00138 1.00000 0.07126 0.00000 0.00000 C8 0.20852 -0.00300 -0.03873 1.00000 0.03771 0.03458 0.09148 -0.01844 0.01380 -0.01570 0.05459 0.01127 0.00075 0.00044 0.00055 0.00000 0.00369 0.00416 0.00637 0.00452 0.00387 0.00321 0.00204 H8 0.20350 -0.01139 -0.09994 1.00000 0.06551 0.00000 0.00000 C9 0.11965 0.05882 0.00600 1.00000 0.02354 0.05682 0.10339 -0.00113 0.00558 -0.01538 0.06125 0.01135 0.00078 0.00044 0.00049 0.00000 0.00272 0.00428 0.00573 0.00372 0.00364 0.00324 0.00208 H9 0.04160 0.10155 -0.01843 1.00000 0.07350 0.00000 0.00000 C10 0.15895 0.05080 0.09278 1.00000 0.07084 0.07531 0.09478 -0.04546 0.06835 -0.05127 0.08031 0.01287 0.00097 0.00052 0.00058 0.00000 0.00447 0.00525 0.00544 0.00435 0.00409 0.00398 0.00269 H10 0.11135 0.08531 0.13897 1.00000 0.09637 0.00000 0.00000 C11 0.41051 0.23621 0.15537 1.00000 0.01845 0.02294 0.02456 -0.00160 -0.00076 0.00219 0.02198 0.00814 0.00060 0.00033 0.00032 0.00000 0.00278 0.00296 0.00320 0.00240 0.00224 0.00227 0.00121 H11 0.31600 0.27554 0.14235 1.00000 0.02638 0.00000 0.00000 C12 0.45526 0.23083 0.23942 1.00000 0.01966 0.01961 0.01806 0.00019 0.00007 0.00015 0.01911 0.00862 0.00057 0.00035 0.00034 0.00000 0.00274 0.00308 0.00336 0.00245 0.00209 0.00215 0.00125 C13 0.60505 0.17465 0.26835 1.00000 0.02006 0.02019 0.01824 -0.00224 0.00404 0.00452 0.01950 0.00844 0.00064 0.00033 0.00030 0.00000 0.00279 0.00293 0.00286 0.00223 0.00240 0.00250 0.00112 C14 0.77459 0.21005 0.27063 1.00000 0.03095 0.03220 0.02683 0.00055 0.00249 -0.00166 0.02999 0.00951 0.00065 0.00040 0.00036 0.00000 0.00327 0.00378 0.00360 0.00278 0.00258 0.00279 0.00144 H14 0.79533 0.27091 0.25677 1.00000 0.03599 0.00000 0.00000 C15 0.91276 0.15389 0.29375 1.00000 0.01824 0.05194 0.03957 -0.00378 -0.00440 0.00600 0.03658 0.00961 0.00064 0.00041 0.00037 0.00000 0.00315 0.00436 0.00393 0.00323 0.00251 0.00284 0.00151 H15 1.03022 0.17569 0.29494 1.00000 0.04390 0.00000 0.00000 C16 0.87792 0.06693 0.31476 1.00000 0.03143 0.04723 0.02977 -0.00056 -0.00241 0.01492 0.03614 0.00976 0.00074 0.00040 0.00031 0.00000 0.00305 0.00433 0.00335 0.00284 0.00264 0.00359 0.00140 H16 0.97072 0.02757 0.33043 1.00000 0.04337 0.00000 0.00000 C17 0.70392 0.03703 0.31280 1.00000 0.04684 0.03670 0.02533 0.00367 -0.00179 0.00339 0.03629 0.00979 0.00074 0.00041 0.00033 0.00000 0.00381 0.00393 0.00372 0.00286 0.00263 0.00307 0.00156 H17 0.67955 -0.02343 0.32688 1.00000 0.04354 0.00000 0.00000 C18 0.35161 0.27796 0.30753 1.00000 0.01439 0.01953 0.02574 -0.00280 0.00400 0.00290 0.01989 0.00808 0.00058 0.00032 0.00032 0.00000 0.00269 0.00283 0.00331 0.00232 0.00222 0.00235 0.00118 C19 0.37734 0.25856 0.39575 1.00000 0.02120 0.04322 0.02467 -0.00328 0.00157 0.00549 0.02970 0.00886 0.00070 0.00034 0.00032 0.00000 0.00261 0.00347 0.00324 0.00257 0.00254 0.00314 0.00126 H19 0.46257 0.21547 0.41255 1.00000 0.03564 0.00000 0.00000 C20 0.27842 0.30222 0.45872 1.00000 0.03826 0.03209 0.03513 -0.00048 0.00844 -0.00214 0.03516 0.00957 0.00067 0.00036 0.00040 0.00000 0.00324 0.00358 0.00404 0.00309 0.00290 0.00272 0.00148 H20 0.29616 0.29048 0.51882 1.00000 0.04219 0.00000 0.00000 C21 0.15458 0.36267 0.43179 1.00000 0.03608 0.02650 0.03519 -0.00040 0.01682 0.00240 0.03259 0.00942 0.00066 0.00035 0.00036 0.00000 0.00351 0.00332 0.00380 0.00269 0.00265 0.00273 0.00146 H21 0.08326 0.39373 0.47255 1.00000 0.03911 0.00000 0.00000 C22 0.13661 0.37712 0.34275 1.00000 0.03973 0.03729 0.03575 -0.00232 0.00841 0.01756 0.03759 0.01014 0.00073 0.00038 0.00037 0.00000 0.00324 0.00347 0.00383 0.00283 0.00309 0.00309 0.00143 H22 0.05056 0.41918 0.32455 1.00000 0.04511 0.00000 0.00000 Final Structure Factor Calculation for s92 in P2(1)2(1)2(1) Total number of l.s. parameters = 226 Maximum vector length = 511 Memory required = 4001 / 25046 wR2 = 0.0962 before cycle 5 for 2717 data and 2 / 226 parameters Disagreeable restraints before cycle 5 Observed Target Error Sigma Restraint -0.0439 0.0080 ISOR U23 C6 0.0529 0.0080 ISOR U12 C6 0.0377 0.0080 ISOR U11 C9 -0.0421 0.0080 ISOR U33 C9 0.0455 0.0080 ISOR U23 C10 -0.0683 0.0080 ISOR U13 C10 0.0513 0.0080 ISOR U12 C10 Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 18. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.008 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.032 0.000 GooF = S = 0.887; Restrained GooF = 0.929 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0252 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0422 for 2100 Fo > 4sig(Fo) and 0.0541 for all 2717 data wR2 = 0.0962, GooF = S = 0.887, Restrained GooF = 0.929 for all data Flack x parameter = -0.0095 with esd 0.0316 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Occupancy sum of asymmetric unit = 25.00 for non-hydrogen and 18.00 for hydrogen atoms Principal mean square atomic displacements U 0.0400 0.0233 0.0161 Fe1 0.0359 0.0229 0.0153 N1 0.0542 0.0238 0.0192 N2 0.0271 0.0176 0.0118 C1 0.0319 0.0225 0.0149 C2 0.0335 0.0291 0.0121 C3 0.0273 0.0251 0.0178 C4 0.0333 0.0254 0.0167 C5 0.1595 0.0675 0.0212 C6 0.1195 0.0406 0.0180 C7 0.1019 0.0418 0.0200 C8 0.1039 0.0626 0.0173 C9 0.1918 0.0388 0.0103 C10 0.0260 0.0224 0.0176 C11 0.0198 0.0195 0.0180 C12 0.0250 0.0213 0.0122 C13 0.0335 0.0310 0.0254 C14 0.0544 0.0388 0.0166 C15 0.0563 0.0301 0.0220 C16 0.0479 0.0370 0.0239 C17 0.0275 0.0207 0.0115 C18 0.0449 0.0252 0.0189 C19 0.0456 0.0321 0.0279 C20 0.0525 0.0269 0.0183 C21 0.0572 0.0379 0.0178 C22 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.044 0.064 0.080 0.096 0.115 0.134 0.161 0.196 0.262 1.000 Number in group 272. 275. 278. 265. 275. 269. 270. 272. 270. 271. GooF 0.349 0.472 0.643 0.607 0.631 0.864 0.798 0.651 0.995 1.887 K 1.491 1.017 0.993 0.994 0.990 1.007 1.005 1.004 1.002 1.033 Resolution(A) 0.84 0.90 0.94 0.99 1.04 1.10 1.19 1.31 1.50 1.87 inf Number in group 276. 275. 266. 276. 266. 278. 265. 270. 271. 274. GooF 0.483 0.478 0.507 0.554 0.589 0.594 0.608 0.776 1.124 1.970 K 0.956 1.007 1.010 1.028 1.023 1.031 1.009 1.002 1.037 1.022 R1 0.102 0.080 0.062 0.064 0.060 0.049 0.038 0.034 0.037 0.055 Recommended weighting scheme: WGHT 0.0255 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 1 2 1772.61 3164.91 14.40 0.366 6.84 0 6 0 4852.04 7756.74 12.61 0.574 2.50 1 1 0 602.05 382.70 8.61 0.127 6.77 0 4 7 5152.63 7211.85 7.84 0.553 1.89 4 6 0 12282.27 10669.00 5.72 0.673 1.51 -3 7 1 5818.84 4385.18 5.50 0.431 1.63 1 3 2 812.00 1030.05 5.26 0.209 3.67 -2 1 1 6298.57 5462.17 5.17 0.481 3.58 0 9 1 4405.30 5381.97 5.10 0.478 1.66 -1 5 4 2454.14 2932.97 5.06 0.353 2.26 -1 7 1 3195.00 3875.60 5.06 0.406 2.04 1 7 1 4827.15 4022.12 4.99 0.413 2.04 3 6 0 4623.50 3552.42 4.87 0.388 1.78 -1 2 5 8072.82 6653.27 4.66 0.531 2.66 1 1 3 9222.09 8066.94 4.56 0.585 4.09 -1 3 2 782.60 981.34 4.55 0.204 3.67 1 4 3 255.27 407.25 4.09 0.131 2.81 4 3 1 7984.09 6429.81 4.05 0.522 1.76 1 3 1 4168.77 3543.39 3.98 0.388 4.03 0 6 2 5607.08 4777.73 3.95 0.450 2.38 0 0 6 876.07 1245.64 3.89 0.230 2.56 4 0 0 12435.08 10853.50 3.77 0.679 1.90 0 2 6 5415.35 4410.41 3.57 0.433 2.42 3 5 2 3643.25 3138.34 3.57 0.365 1.88 3 7 0 7855.91 6922.37 3.55 0.542 1.63 2 2 0 4306.40 3697.68 3.52 0.396 3.39 0 0 4 25658.22 23562.70 3.45 1.000 3.84 4 3 3 6199.59 5141.22 3.43 0.467 1.68 -4 3 3 6241.19 5311.79 3.30 0.475 1.68 2 0 1 2898.43 2564.27 3.30 0.330 3.69 -1 2 6 1068.62 1307.99 3.29 0.236 2.31 1 0 2 1165.03 1037.68 3.27 0.210 5.40 0 3 7 230.56 372.82 3.20 0.126 2.01 -1 4 3 243.58 327.21 3.15 0.118 2.81 0 2 0 170.51 103.96 3.11 0.066 7.50 1 5 9 721.85 590.81 3.03 0.158 1.46 -4 2 2 2397.25 2060.61 2.97 0.296 1.79 0 4 4 967.09 1157.64 2.97 0.222 2.68 -3 1 2 3297.63 2782.24 2.95 0.344 2.37 5 2 9 603.24 470.25 2.93 0.141 1.12 1 1 1 7994.67 7245.01 2.90 0.555 6.20 0 4 2 1744.10 1338.01 2.86 0.238 3.37 3 3 1 2128.30 1803.47 2.84 0.277 2.23 2 3 0 8100.84 7025.70 2.83 0.546 3.02 0 9 5 482.55 590.94 2.77 0.158 1.46 -2 4 4 925.10 1078.70 2.76 0.214 2.19 0 7 6 2138.46 2384.57 2.75 0.318 1.64 3 1 5 1537.85 1699.54 2.74 0.269 1.94 0 14 4 1031.09 782.01 2.73 0.182 1.03 3 7 1 5054.14 4266.85 2.73 0.426 1.63 Selected torsion angles 81.74 ( 0.43) C6 - Fe1 - C1 - C2 125.55 ( 0.42) C10 - Fe1 - C1 - C2 165.84 ( 0.35) C9 - Fe1 - C1 - C2 -118.19 ( 0.41) C5 - Fe1 - C1 - C2 53.45 ( 0.68) C7 - Fe1 - C1 - C2 -81.01 ( 0.30) C4 - Fe1 - C1 - C2 -167.32 ( 0.77) C8 - Fe1 - C1 - C2 -37.32 ( 0.28) C3 - Fe1 - C1 - C2 -160.07 ( 0.41) C6 - Fe1 - C1 - C5 -116.26 ( 0.41) C10 - Fe1 - C1 - C5 -75.97 ( 0.39) C9 - Fe1 - C1 - C5 118.19 ( 0.41) C2 - Fe1 - C1 - C5 171.64 ( 0.55) C7 - Fe1 - C1 - C5 37.18 ( 0.26) C4 - Fe1 - C1 - C5 -49.13 ( 0.92) C8 - Fe1 - C1 - C5 80.87 ( 0.30) C3 - Fe1 - C1 - C5 -43.47 ( 0.55) C6 - Fe1 - C1 - C11 0.34 ( 0.55) C10 - Fe1 - C1 - C11 40.63 ( 0.54) C9 - Fe1 - C1 - C11 -125.21 ( 0.55) C2 - Fe1 - C1 - C11 116.60 ( 0.49) C5 - Fe1 - C1 - C11 -71.77 ( 0.72) C7 - Fe1 - C1 - C11 153.78 ( 0.45) C4 - Fe1 - C1 - C11 67.47 ( 1.00) C8 - Fe1 - C1 - C11 -162.53 ( 0.46) C3 - Fe1 - C1 - C11 0.02 ( 0.54) C5 - C1 - C2 - C3 176.09 ( 0.47) C11 - C1 - C2 - C3 59.64 ( 0.34) Fe1 - C1 - C2 - C3 -59.62 ( 0.33) C5 - C1 - C2 - Fe1 116.45 ( 0.50) C11 - C1 - C2 - Fe1 -116.95 ( 0.45) C6 - Fe1 - C2 - C1 -74.11 ( 0.45) C10 - Fe1 - C2 - C1 -42.80 ( 0.93) C9 - Fe1 - C2 - C1 38.34 ( 0.29) C5 - Fe1 - C2 - C1 -158.32 ( 0.37) C7 - Fe1 - C2 - C1 82.29 ( 0.32) C4 - Fe1 - C2 - C1 169.67 ( 0.66) C8 - Fe1 - C2 - C1 120.27 ( 0.42) C3 - Fe1 - C2 - C1 122.77 ( 0.46) C6 - Fe1 - C2 - C3 165.62 ( 0.40) C10 - Fe1 - C2 - C3 -163.07 ( 0.78) C9 - Fe1 - C2 - C3 -81.93 ( 0.31) C5 - Fe1 - C2 - C3 -120.27 ( 0.42) C1 - Fe1 - C2 - C3 81.41 ( 0.42) C7 - Fe1 - C2 - C3 -37.98 ( 0.29) C4 - Fe1 - C2 - C3 49.40 ( 0.78) C8 - Fe1 - C2 - C3 -0.17 ( 0.54) C1 - C2 - C3 - C4 59.07 ( 0.31) Fe1 - C2 - C3 - C4 -59.24 ( 0.33) C1 - C2 - C3 - Fe1 164.41 ( 0.45) C6 - Fe1 - C3 - C4 -163.56 ( 0.84) C10 - Fe1 - C3 - C4 49.86 ( 0.66) C9 - Fe1 - C3 - C4 -118.59 ( 0.42) C2 - Fe1 - C3 - C4 -37.54 ( 0.30) C5 - Fe1 - C3 - C4 -81.43 ( 0.33) C1 - Fe1 - C3 - C4 122.62 ( 0.38) C7 - Fe1 - C3 - C4 81.84 ( 0.41) C8 - Fe1 - C3 - C4 -77.00 ( 0.49) C6 - Fe1 - C3 - C2 -44.98 ( 1.00) C10 - Fe1 - C3 - C2 168.45 ( 0.53) C9 - Fe1 - C3 - C2 81.05 ( 0.31) C5 - Fe1 - C3 - C2 37.16 ( 0.28) C1 - Fe1 - C3 - C2 -118.79 ( 0.38) C7 - Fe1 - C3 - C2 118.59 ( 0.42) C4 - Fe1 - C3 - C2 -159.57 ( 0.35) C8 - Fe1 - C3 - C2 0.25 ( 0.54) C2 - C3 - C4 - C5 58.75 ( 0.33) Fe1 - C3 - C4 - C5 -58.50 ( 0.33) C2 - C3 - C4 - Fe1 -163.82 ( 0.86) C6 - Fe1 - C4 - C5 49.60 ( 0.70) C10 - Fe1 - C4 - C5 82.59 ( 0.37) C9 - Fe1 - C4 - C5 -81.28 ( 0.31) C2 - Fe1 - C4 - C5 -37.28 ( 0.27) C1 - Fe1 - C4 - C5 162.46 ( 0.35) C7 - Fe1 - C4 - C5 123.06 ( 0.33) C8 - Fe1 - C4 - C5 -119.58 ( 0.42) C3 - Fe1 - C4 - C5 -44.24 ( 1.00) C6 - Fe1 - C4 - C3 169.17 ( 0.58) C10 - Fe1 - C4 - C3 -157.83 ( 0.33) C9 - Fe1 - C4 - C3 38.30 ( 0.27) C2 - Fe1 - C4 - C3 119.58 ( 0.42) C5 - Fe1 - C4 - C3 82.29 ( 0.31) C1 - Fe1 - C4 - C3 -77.96 ( 0.39) C7 - Fe1 - C4 - C3 -117.36 ( 0.34) C8 - Fe1 - C4 - C3 0.14 ( 0.54) C2 - C1 - C5 - C4 -176.29 ( 0.41) C11 - C1 - C5 - C4 -59.35 ( 0.34) Fe1 - C1 - C5 - C4 59.48 ( 0.32) C2 - C1 - C5 - Fe1 -116.94 ( 0.45) C11 - C1 - C5 - Fe1 -0.24 ( 0.55) C3 - C4 - C5 - C1 59.03 ( 0.35) Fe1 - C4 - C5 - C1 -59.27 ( 0.33) C3 - C4 - C5 - Fe1 47.08 ( 0.77) C6 - Fe1 - C5 - C1 81.96 ( 0.42) C10 - Fe1 - C5 - C1 123.92 ( 0.33) C9 - Fe1 - C5 - C1 -38.36 ( 0.26) C2 - Fe1 - C5 - C1 -169.95 ( 0.64) C7 - Fe1 - C5 - C1 -120.16 ( 0.39) C4 - Fe1 - C5 - C1 162.76 ( 0.31) C8 - Fe1 - C5 - C1 -82.64 ( 0.29) C3 - Fe1 - C5 - C1 167.24 ( 0.66) C6 - Fe1 - C5 - C4 -157.88 ( 0.39) C10 - Fe1 - C5 - C4 -115.92 ( 0.33) C9 - Fe1 - C5 - C4 81.80 ( 0.30) C2 - Fe1 - C5 - C4 120.16 ( 0.39) C1 - Fe1 - C5 - C4 -49.79 ( 0.77) C7 - Fe1 - C5 - C4 -77.08 ( 0.37) C8 - Fe1 - C5 - C4 37.52 ( 0.27) C3 - Fe1 - C5 - C4 114.73 ( 0.65) C10 - Fe1 - C6 - C7 77.06 ( 0.45) C9 - Fe1 - C6 - C7 -120.59 ( 0.42) C2 - Fe1 - C6 - C7 162.50 ( 0.54) C5 - Fe1 - C6 - C7 -163.51 ( 0.38) C1 - Fe1 - C6 - C7 -44.63 ( 1.08) C4 - Fe1 - C6 - C7 35.40 ( 0.39) C8 - Fe1 - C6 - C7 -78.30 ( 0.49) C3 - Fe1 - C6 - C7 -37.67 ( 0.45) C9 - Fe1 - C6 - C10 124.68 ( 0.48) C2 - Fe1 - C6 - C10 47.77 ( 0.90) C5 - Fe1 - C6 - C10 81.77 ( 0.51) C1 - Fe1 - C6 - C10 -114.73 ( 0.65) C7 - Fe1 - C6 - C10 -159.35 ( 0.75) C4 - Fe1 - C6 - C10 -79.33 ( 0.49) C8 - Fe1 - C6 - C10 166.97 ( 0.42) C3 - Fe1 - C6 - C10 2.68 ( 0.69) C10 - C6 - C7 - C8 -59.21 ( 0.44) Fe1 - C6 - C7 - C8 61.89 ( 0.43) C10 - C6 - C7 - Fe1 121.26 ( 0.64) C6 - Fe1 - C7 - C8 80.09 ( 0.48) C10 - Fe1 - C7 - C8 36.30 ( 0.41) C9 - Fe1 - C7 - C8 -160.60 ( 0.38) C2 - Fe1 - C7 - C8 -36.78 ( 0.90) C5 - Fe1 - C7 - C8 160.47 ( 0.52) C1 - Fe1 - C7 - C8 -74.60 ( 0.47) C4 - Fe1 - C7 - C8 -117.12 ( 0.41) C3 - Fe1 - C7 - C8 -41.17 ( 0.46) C10 - Fe1 - C7 - C6 -84.95 ( 0.49) C9 - Fe1 - C7 - C6 78.14 ( 0.51) C2 - Fe1 - C7 - C6 -158.04 ( 0.68) C5 - Fe1 - C7 - C6 39.21 ( 0.82) C1 - Fe1 - C7 - C6 164.14 ( 0.45) C4 - Fe1 - C7 - C6 -121.26 ( 0.64) C8 - Fe1 - C7 - C6 121.62 ( 0.47) C3 - Fe1 - C7 - C6 -1.60 ( 0.68) C6 - C7 - C8 - C9 -59.14 ( 0.41) Fe1 - C7 - C8 - C9 57.54 ( 0.45) C6 - C7 - C8 - Fe1 83.42 ( 0.51) C6 - Fe1 - C8 - C9 37.65 ( 0.45) C10 - Fe1 - C8 - C9 165.35 ( 0.56) C2 - Fe1 - C8 - C9 -73.60 ( 0.51) C5 - Fe1 - C8 - C9 -36.21 ( 1.08) C1 - Fe1 - C8 - C9 120.04 ( 0.67) C7 - Fe1 - C8 - C9 -115.77 ( 0.45) C4 - Fe1 - C8 - C9 -158.73 ( 0.41) C3 - Fe1 - C8 - C9 -36.62 ( 0.48) C6 - Fe1 - C8 - C7 -82.39 ( 0.50) C10 - Fe1 - C8 - C7 -120.04 ( 0.67) C9 - Fe1 - C8 - C7 45.31 ( 0.90) C2 - Fe1 - C8 - C7 166.36 ( 0.41) C5 - Fe1 - C8 - C7 -156.25 ( 0.71) C1 - Fe1 - C8 - C7 124.20 ( 0.44) C4 - Fe1 - C8 - C7 81.24 ( 0.51) C3 - Fe1 - C8 - C7 -0.23 ( 0.68) C7 - C8 - C9 - C10 -59.76 ( 0.44) Fe1 - C8 - C9 - C10 59.53 ( 0.40) C7 - C8 - C9 - Fe1 -80.03 ( 0.53) C6 - Fe1 - C9 - C8 -119.46 ( 0.66) C10 - Fe1 - C9 - C8 -160.26 ( 0.75) C2 - Fe1 - C9 - C8 124.69 ( 0.45) C5 - Fe1 - C9 - C8 166.58 ( 0.44) C1 - Fe1 - C9 - C8 -36.47 ( 0.47) C7 - Fe1 - C9 - C8 81.79 ( 0.50) C4 - Fe1 - C9 - C8 46.45 ( 0.79) C3 - Fe1 - C9 - C8 39.43 ( 0.45) C6 - Fe1 - C9 - C10 -40.80 ( 1.02) C2 - Fe1 - C9 - C10 -115.84 ( 0.45) C5 - Fe1 - C9 - C10 -73.95 ( 0.51) C1 - Fe1 - C9 - C10 82.99 ( 0.49) C7 - Fe1 - C9 - C10 -158.75 ( 0.42) C4 - Fe1 - C9 - C10 119.46 ( 0.66) C8 - Fe1 - C9 - C10 165.91 ( 0.55) C3 - Fe1 - C9 - C10 1.89 ( 0.71) C8 - C9 - C10 - C6 -59.36 ( 0.42) Fe1 - C9 - C10 - C6 61.25 ( 0.43) C8 - C9 - C10 - Fe1 -2.75 ( 0.71) C7 - C6 - C10 - C9 60.62 ( 0.44) Fe1 - C6 - C10 - C9 -63.37 ( 0.44) C7 - C6 - C10 - Fe1 -117.82 ( 0.66) C6 - Fe1 - C10 - C9 166.28 ( 0.37) C2 - Fe1 - C10 - C9 82.17 ( 0.46) C5 - Fe1 - C10 - C9 124.97 ( 0.42) C1 - Fe1 - C10 - C9 -78.48 ( 0.47) C7 - Fe1 - C10 - C9 47.04 ( 0.78) C4 - Fe1 - C10 - C9 -36.26 ( 0.42) C8 - Fe1 - C10 - C9 -158.57 ( 0.76) C3 - Fe1 - C10 - C9 117.82 ( 0.66) C9 - Fe1 - C10 - C6 -75.89 ( 0.55) C2 - Fe1 - C10 - C6 -160.00 ( 0.48) C5 - Fe1 - C10 - C6 -117.21 ( 0.52) C1 - Fe1 - C10 - C6 39.35 ( 0.47) C7 - Fe1 - C10 - C6 164.86 ( 0.60) C4 - Fe1 - C10 - C6 81.56 ( 0.51) C8 - Fe1 - C10 - C6 -40.75 ( 1.10) C3 - Fe1 - C10 - C6 9.51 ( 0.83) C2 - C1 - C11 - C12 -174.97 ( 0.50) C5 - C1 - C11 - C12 99.41 ( 0.55) Fe1 - C1 - C11 - C12 2.42 ( 0.79) C1 - C11 - C12 - C13 -174.93 ( 0.45) C1 - C11 - C12 - C18 -4.36 ( 0.75) C17 - N1 - C13 - C14 175.83 ( 0.45) C17 - N1 - C13 - C12 -91.98 ( 0.57) C11 - C12 - C13 - N1 85.46 ( 0.57) C18 - C12 - C13 - N1 88.21 ( 0.62) C11 - C12 - C13 - C14 -94.36 ( 0.58) C18 - C12 - C13 - C14 3.52 ( 0.78) N1 - C13 - C14 - C15 -176.67 ( 0.49) C12 - C13 - C14 - C15 -1.10 ( 0.80) C13 - C14 - C15 - C16 -0.31 ( 0.80) C14 - C15 - C16 - C17 2.83 ( 0.75) C13 - N1 - C17 - C16 -0.52 ( 0.78) C15 - C16 - C17 - N1 0.98 ( 0.74) C22 - N2 - C18 - C19 178.83 ( 0.46) C22 - N2 - C18 - C12 -10.33 ( 0.70) C11 - C12 - C18 - N2 172.23 ( 0.45) C13 - C12 - C18 - N2 167.54 ( 0.48) C11 - C12 - C18 - C19 -9.90 ( 0.69) C13 - C12 - C18 - C19 -1.47 ( 0.78) N2 - C18 - C19 - C20 -179.26 ( 0.46) C12 - C18 - C19 - C20 1.19 ( 0.75) C18 - C19 - C20 - C21 -0.52 ( 0.76) C19 - C20 - C21 - C22 -0.29 ( 0.84) C18 - N2 - C22 - C21 0.06 ( 0.88) C20 - C21 - C22 - N2 Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 5.6473 (0.0114) x + 9.9248 (0.0251) y - 1.4047 (0.0395) z = 4.5229 (0.0036) * -0.0003 (0.0030) C1 * -0.0006 (0.0030) C2 * 0.0012 (0.0030) C3 * -0.0014 (0.0030) C4 * 0.0011 (0.0030) C5 -1.6351 (0.0021) Fe1 -0.0786 (0.0082) C11 0.0027 (0.0106) C12 0.2504 (0.0114) C13 -0.2106 (0.0134) C18 Rms deviation of fitted atoms = 0.0010 5.7234 (0.0140) x + 9.6677 (0.0311) y - 1.9287 (0.0494) z = 1.2353 (0.0042) Angle to previous plane (with approximate esd) = 2.26 ( 0.36 ) * 0.0156 (0.0038) C6 * -0.0125 (0.0037) C7 * 0.0038 (0.0035) C8 * 0.0065 (0.0037) C9 * -0.0135 (0.0039) C10 1.6473 (0.0026) Fe1 Rms deviation of fitted atoms = 0.0113 - 0.8664 (0.0156) x + 4.0138 (0.0328) y + 14.7064 (0.0102) z = 4.1431 (0.0126) Angle to previous plane (with approximate esd) = 88.09 ( 0.22 ) * 0.0174 (0.0033) N1 * -0.0198 (0.0034) C13 * 0.0089 (0.0037) C14 * 0.0038 (0.0038) C15 * -0.0061 (0.0036) C16 * -0.0042 (0.0035) C17 -0.0901 (0.0082) C12 Rms deviation of fitted atoms = 0.0118 5.1906 (0.0120) x + 10.9153 (0.0223) y + 0.7455 (0.0312) z = 5.0825 (0.0117) Angle to previous plane (with approximate esd) = 80.60 ( 0.17 ) * -0.0018 (0.0034) N2 * 0.0058 (0.0035) C18 * -0.0066 (0.0036) C19 * 0.0035 (0.0035) C20 * 0.0005 (0.0038) C21 * -0.0014 (0.0039) C22 -0.0214 (0.0079) C12 Rms deviation of fitted atoms = 0.0040 FMAP and GRID set by program FMAP 2 1 11 GRID -3.125 -2 -2 3.125 2 2 R1 = 0.0540 for 1631 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.57 at 0.2235 0.0250 0.1421 [ 0.98 A from C10 ] Deepest hole -0.32 at 0.2599 0.9093 0.5387 [ 1.09 A from FE1 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 4238 / 19094 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2235 0.0250 0.1421 1.00000 0.05 0.57 0.98 C10 1.04 C6 1.24 H10 1.33 H6 Q2 1 0.2171 0.0373 -0.2035 1.00000 0.05 0.47 1.75 H8 2.27 H6 2.60 C8 2.61 H16 Q3 1 0.3848 0.0771 -0.0733 1.00000 0.05 0.34 1.51 C4 1.53 FE1 1.61 H4 1.88 C8 Q4 1 0.1089 0.0812 0.0942 1.00000 0.05 0.29 0.59 C10 0.69 H10 1.40 C9 1.83 H9 Q5 1 0.1117 0.0764 -0.0225 1.00000 0.05 0.29 0.52 C9 0.66 H9 1.42 C8 1.85 C10 Q6 1 0.3815 0.2249 0.4761 1.00000 0.05 0.28 1.16 H19 1.34 C19 1.35 H20 1.42 C20 Q7 1 0.5107 0.1664 0.2159 1.00000 0.05 0.27 1.09 C13 1.11 C12 1.59 C11 1.68 N1 Q8 1 0.3444 -0.0439 0.1124 1.00000 0.05 0.26 0.61 H6 0.61 C6 1.50 C7 1.92 H7 Q9 1 0.1332 0.2230 0.4366 1.00000 0.05 0.26 1.66 C20 2.03 C19 2.04 H20 2.09 H7 Q10 1 0.3649 -0.0649 0.0167 1.00000 0.05 0.25 0.49 C7 0.59 H7 1.58 C6 1.73 C8 Shortest distances between peaks (including symmetry equivalents) 1 4 1.42 1 8 1.46 8 10 1.51 4 5 1.80 6 9 1.98 3 5 2.22 2 3 2.45 6 9 2.46 3 10 2.54 1 10 2.59 1 2 2.59 4 8 2.61 9 10 2.67 1 5 2.78 2 8 2.87 5 10 2.92 2 5 2.95 Time profile in seconds ----------------------- 0.20: Read and process instructions 0.00: Fit rigid groups 0.02: Interpret restraints etc. 0.02: 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. 1.14: 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 1.38: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.16: Apply other restraints 0.34: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 17:54:02 Total CPU time: 5.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++