+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXH-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 04src0551 started at 15:13:14 on 12-Jul-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 04src0551 in C2/c CELL 0.71073 24.5776 9.3330 15.2877 90.000 123.252 90.000 ZERR 4.00 0.0049 0.0019 0.0031 0.000 0.030 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H P FE UNIT 120 208 8 4 V = 2932.56 F(000) = 1152.0 Mu = 0.64 mm-1 Cell Wt = 2122.02 Rho = 1.202 MERG 2 OMIT -3.00 55.00 OMIT -3 1 1 OMIT 3 1 0 SHEL 7 0.77 FMAP 2 PLAN 5 SIZE 0.04 0.22 0.32 ACTA BOND $H WGHT 0.02680 3.54380 L.S. 5 TEMP -153.00 FVAR 0.27020 MOLE 1 C1 1 0.070797 0.213974 0.221772 11.00000 0.01621 0.01847 = 0.01639 0.00007 0.00827 -0.00054 C2 1 0.054421 0.364295 0.204483 11.00000 0.01823 0.01971 = 0.02035 0.00194 0.01110 -0.00043 C3 1 -0.012714 0.377352 0.124431 11.00000 0.02167 0.02258 = 0.02069 0.00620 0.01227 0.00377 C4 1 -0.038970 0.237315 0.091014 11.00000 0.01649 0.02763 = 0.01414 0.00129 0.00737 -0.00024 C5 1 0.011729 0.135186 0.150459 11.00000 0.01849 0.02186 = 0.01587 -0.00209 0.00912 -0.00212 C6 1 0.100093 0.488562 0.254427 11.00000 0.02443 0.01841 = 0.03521 0.00083 0.01666 -0.00122 AFIX 137 H6A 2 0.116905 0.515892 0.211628 11.00000 -1.50000 H6B 2 0.136382 0.461169 0.324486 11.00000 -1.50000 H6C 2 0.076842 0.569845 0.259810 11.00000 -1.50000 AFIX 0 C7 1 -0.048735 0.514785 0.075605 11.00000 0.02839 0.02951 = 0.03482 0.01494 0.01744 0.01023 AFIX 137 H7A 2 -0.030515 0.591161 0.128207 11.00000 -1.50000 H7B 2 -0.094871 0.501889 0.049075 11.00000 -1.50000 H7C 2 -0.044293 0.540867 0.017714 11.00000 -1.50000 AFIX 0 C8 1 -0.107677 0.207995 0.000965 11.00000 0.01901 0.04047 = 0.01688 0.00103 0.00535 -0.00061 AFIX 137 H8A 2 -0.112752 0.237713 -0.064612 11.00000 -1.50000 H8B 2 -0.138114 0.261915 0.010894 11.00000 -1.50000 H8C 2 -0.116835 0.105296 -0.001932 11.00000 -1.50000 AFIX 0 C9 1 0.004985 -0.024119 0.135469 11.00000 0.02178 0.02233 = 0.02398 -0.00595 0.01168 -0.00346 AFIX 137 H9A 2 -0.041176 -0.050235 0.096681 11.00000 -1.50000 H9B 2 0.028024 -0.071480 0.203882 11.00000 -1.50000 H9C 2 0.023699 -0.054747 0.096050 11.00000 -1.50000 AFIX 0 C10 1 0.171519 0.108729 0.201195 11.00000 0.02031 0.02574 = 0.02257 0.00338 0.01247 0.00375 AFIX 13 H10 2 0.149120 0.015262 0.170680 11.00000 -1.20000 AFIX 0 C11 1 0.244936 0.088628 0.253609 11.00000 0.02582 0.05391 = 0.03192 0.01260 0.01892 0.01314 AFIX 137 H11A 2 0.253496 0.050744 0.202486 11.00000 -1.50000 H11B 2 0.261338 0.021182 0.311973 11.00000 -1.50000 H11C 2 0.266934 0.181103 0.279894 11.00000 -1.50000 AFIX 0 C12 1 0.145363 0.220057 0.114129 11.00000 0.02519 0.03354 = 0.02287 0.00503 0.01424 0.00212 AFIX 137 H12A 2 0.164212 0.313899 0.144348 11.00000 -1.50000 H12B 2 0.097888 0.225166 0.077351 11.00000 -1.50000 H12C 2 0.157182 0.192641 0.064742 11.00000 -1.50000 AFIX 0 C13 1 0.164858 -0.007083 0.372862 11.00000 0.01967 0.02143 = 0.02162 0.00206 0.01112 0.00028 AFIX 13 H13 2 0.128586 -0.009490 0.384458 11.00000 -1.20000 AFIX 0 C14 1 0.228795 0.000954 0.481654 11.00000 0.02299 0.03279 = 0.02154 0.00651 0.00841 0.00489 AFIX 137 H14A 2 0.232324 -0.083124 0.522872 11.00000 -1.50000 H14B 2 0.228968 0.088143 0.517528 11.00000 -1.50000 H14C 2 0.265750 0.002953 0.473743 11.00000 -1.50000 AFIX 0 C15 1 0.163178 -0.149485 0.322417 11.00000 0.03145 0.01811 = 0.03341 0.00270 0.01454 0.00141 AFIX 137 H15A 2 0.202082 -0.158042 0.320020 11.00000 -1.50000 H15B 2 0.124249 -0.153361 0.251162 11.00000 -1.50000 H15C 2 0.162124 -0.228521 0.363669 11.00000 -1.50000 AFIX 0 P1 3 0.156647 0.165103 0.303333 11.00000 0.01486 0.01670 = 0.01771 -0.00014 0.00722 -0.00027 FE1 4 0.000000 0.261909 0.250000 10.50000 0.01384 0.01559 = 0.01519 0.00000 0.00662 0.00000 HKLF 4 Covalent radii and connectivity table for 04src0551 in C2/c C 0.770 H 0.320 P 1.100 FE 1.240 C1 - C2 C5 P1 Fe1 C2 - C3 C1 C6 Fe1 C3 - C2 C4 C7 Fe1 C4 - C3 C5 C8 Fe1 C5 - C4 C1 C9 Fe1 C6 - C2 C7 - C3 C8 - C4 C9 - C5 C10 - C12 C11 P1 C11 - C10 C12 - C10 C13 - C15 C14 P1 C14 - C13 C15 - C13 P1 - C1 C10 C13 Fe1 - C2_$1 C2 C1_$1 C1 C5 C5_$1 C3_$1 C3 C4 C4_$1 Operators for generating equivalent atoms: $1 -x, y, -z+1/2 26433 Reflections read, of which 961 rejected -31 =< h =< 31, -12 =< k =< 11, -18 =< l =< 19, Max. 2-theta = 54.96 0 Systematic absence violations 0 Inconsistent equivalents 3356 Unique reflections, of which 0 suppressed R(int) = 0.0614 R(sigma) = 0.0407 Friedel opposites merged Maximum memory for data reduction = 2428 / 41367 Special position constraints for Fe1 x = 0.0000 z = 0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Default effective X-H distances for T = -153.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 1.00 0.99 0.98 0.95 0.88 0.91 1.12 0.84 0.95 0.88 0.95 Note that these distances are chosen to give the best fit to the X-ray data and so avoid the introduction of systematic error. The true internuclear distances are longer and do not vary with temperature ! The apparent variation with temperature is caused by libration. Least-squares cycle 1 Maximum vector length = 511 Memory required = 2940 / 197348 wR2 = 0.0771 before cycle 1 for 3356 data and 158 / 158 parameters GooF = S = 1.039; Restrained GooF = 1.039 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0268 * P )^2 + 3.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27021 0.00036 0.020 OSF Mean shift/esd = 0.010 Maximum = -0.050 for U11 Fe1 Max. shift = 0.000 A for H6B Max. dU = 0.000 for C3 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2940 / 197348 wR2 = 0.0770 before cycle 2 for 3356 data and 158 / 158 parameters GooF = S = 1.039; Restrained GooF = 1.039 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0268 * P )^2 + 3.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27020 0.00036 -0.026 OSF Mean shift/esd = 0.003 Maximum = -0.026 for OSF Max. shift = 0.000 A for H6B Max. dU = 0.000 for C3 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2940 / 197348 wR2 = 0.0770 before cycle 3 for 3356 data and 158 / 158 parameters GooF = S = 1.039; Restrained GooF = 1.039 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0268 * P )^2 + 3.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27020 0.00036 0.001 OSF Mean shift/esd = 0.000 Maximum = -0.001 for tors H6A Max. shift = 0.000 A for H6A Max. dU = 0.000 for C11 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2940 / 197348 wR2 = 0.0770 before cycle 4 for 3356 data and 158 / 158 parameters GooF = S = 1.039; Restrained GooF = 1.039 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0268 * P )^2 + 3.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27020 0.00036 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for U11 Fe1 Max. shift = 0.000 A for H7B Max. dU = 0.000 for C13 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2940 / 197348 wR2 = 0.0770 before cycle 5 for 3356 data and 158 / 158 parameters GooF = S = 1.039; Restrained GooF = 1.039 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0268 * P )^2 + 3.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27020 0.00036 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H7B Max. dU = 0.000 for C14 Largest correlation matrix elements 0.668 U13 C11 / U11 C11 0.646 U13 C5 / U11 C5 0.636 U13 C13 / U11 C13 0.659 U13 Fe1 / U11 Fe1 0.645 U13 C6 / U11 C6 0.636 U13 C13 / U33 C13 0.658 U13 C11 / U33 C11 0.642 U13 C7 / U11 C7 0.635 U13 C9 / U11 C9 0.653 U13 C10 / U11 C10 0.639 U13 C6 / U33 C6 0.633 U13 C3 / U33 C3 0.651 U13 C2 / U11 C2 0.639 U13 C2 / U33 C2 0.633 U13 C12 / U33 C12 0.648 U13 C3 / U11 C3 0.639 U13 C10 / U33 C10 0.630 U13 C1 / U11 C1 0.648 U13 C12 / U11 C12 0.637 U13 P1 / U11 P1 0.628 U13 C4 / U11 C4 0.647 U13 Fe1 / U33 Fe1 0.637 U13 C7 / U33 C7 0.626 U13 P1 / U33 P1 Idealized hydrogen atom generation before cycle 6 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H6A 0.1169 0.5159 0.2116 137 0.980 0.000 C6 C2 H6A H6B 0.1364 0.4612 0.3245 137 0.980 0.000 C6 C2 H6A H6C 0.0768 0.5699 0.2598 137 0.980 0.000 C6 C2 H6A H7A -0.0305 0.5912 0.1282 137 0.980 0.000 C7 C3 H7A H7B -0.0949 0.5019 0.0491 137 0.980 0.000 C7 C3 H7A H7C -0.0443 0.5409 0.0177 137 0.980 0.000 C7 C3 H7A H8A -0.1128 0.2377 -0.0646 137 0.980 0.000 C8 C4 H8A H8B -0.1381 0.2619 0.0109 137 0.980 0.000 C8 C4 H8A H8C -0.1168 0.1053 -0.0019 137 0.980 0.000 C8 C4 H8A H9A -0.0412 -0.0502 0.0967 137 0.980 0.000 C9 C5 H9A H9B 0.0280 -0.0715 0.2039 137 0.980 0.000 C9 C5 H9A H9C 0.0237 -0.0547 0.0960 137 0.980 0.000 C9 C5 H9A H10 0.1491 0.0153 0.1707 13 1.000 0.000 C10 C12 C11 P1 H11A 0.2535 0.0508 0.2025 137 0.980 0.000 C11 C10 H11A H11B 0.2613 0.0212 0.3120 137 0.980 0.000 C11 C10 H11A H11C 0.2669 0.1811 0.2799 137 0.980 0.000 C11 C10 H11A H12A 0.1642 0.3139 0.1444 137 0.980 0.000 C12 C10 H12A H12B 0.0979 0.2251 0.0773 137 0.980 0.000 C12 C10 H12A H12C 0.1572 0.1927 0.0648 137 0.980 0.000 C12 C10 H12A H13 0.1286 -0.0095 0.3845 13 1.000 0.000 C13 C15 C14 P1 H14A 0.2323 -0.0831 0.5229 137 0.980 0.000 C14 C13 H14A H14B 0.2290 0.0881 0.5175 137 0.980 0.000 C14 C13 H14A H14C 0.2657 0.0030 0.4737 137 0.980 0.000 C14 C13 H14A H15A 0.2021 -0.1580 0.3200 137 0.980 0.000 C15 C13 H15A H15B 0.1242 -0.1534 0.2512 137 0.980 0.000 C15 C13 H15A H15C 0.1621 -0.2285 0.3637 137 0.980 0.000 C15 C13 H15A 04src0551 in C2/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.07080 0.21397 0.22177 1.00000 0.01620 0.01848 0.01637 0.00007 0.00826 -0.00054 0.01737 0.00377 0.00008 0.00018 0.00013 0.00000 0.00081 0.00091 0.00079 0.00066 0.00069 0.00066 0.00035 C2 0.05442 0.36429 0.20448 1.00000 0.01823 0.01969 0.02035 0.00195 0.01110 -0.00042 0.01915 0.00396 0.00008 0.00019 0.00013 0.00000 0.00084 0.00092 0.00085 0.00070 0.00073 0.00070 0.00036 C3 -0.01271 0.37735 0.12443 1.00000 0.02165 0.02256 0.02067 0.00619 0.01226 0.00376 0.02129 0.00416 0.00008 0.00020 0.00013 0.00000 0.00090 0.00097 0.00086 0.00072 0.00075 0.00074 0.00038 C4 -0.03897 0.23732 0.09101 1.00000 0.01648 0.02761 0.01413 0.00128 0.00737 -0.00025 0.01994 0.00388 0.00008 0.00020 0.00013 0.00000 0.00082 0.00101 0.00078 0.00070 0.00068 0.00072 0.00037 C5 0.01173 0.13519 0.15046 1.00000 0.01849 0.02183 0.01587 -0.00208 0.00913 -0.00211 0.01888 0.00385 0.00008 0.00019 0.00013 0.00000 0.00084 0.00094 0.00080 0.00067 0.00070 0.00070 0.00036 C6 0.10009 0.48856 0.25443 1.00000 0.02442 0.01841 0.03519 0.00083 0.01666 -0.00122 0.02585 0.00427 0.00009 0.00019 0.00015 0.00000 0.00094 0.00097 0.00106 0.00078 0.00086 0.00075 0.00041 H6A 0.11692 0.51586 0.21165 1.00000 0.03877 0.00000 0.00000 H6B 0.13637 0.46118 0.32450 1.00000 0.03877 0.00000 0.00000 H6C 0.07683 0.56986 0.25978 1.00000 0.03877 0.00000 0.00000 C7 -0.04873 0.51478 0.07560 1.00000 0.02836 0.02952 0.03479 0.01494 0.01742 0.01023 0.03084 0.00494 0.00009 0.00021 0.00016 0.00000 0.00103 0.00112 0.00110 0.00087 0.00091 0.00085 0.00046 H7A -0.03051 0.59116 0.12820 1.00000 0.04626 0.00000 0.00000 H7B -0.09487 0.50189 0.04909 1.00000 0.04626 0.00000 0.00000 H7C -0.04430 0.54085 0.01770 1.00000 0.04626 0.00000 0.00000 C8 -0.10768 0.20799 0.00096 1.00000 0.01901 0.04046 0.01686 0.00103 0.00535 -0.00060 0.02779 0.00415 0.00009 0.00023 0.00014 0.00000 0.00090 0.00122 0.00087 0.00079 0.00075 0.00082 0.00043 H8A -0.11276 0.23772 -0.06461 1.00000 0.04168 0.00000 0.00000 H8B -0.13812 0.26190 0.01090 1.00000 0.04168 0.00000 0.00000 H8C -0.11683 0.10529 -0.00194 1.00000 0.04168 0.00000 0.00000 C9 0.00499 -0.02412 0.13547 1.00000 0.02177 0.02233 0.02397 -0.00596 0.01168 -0.00347 0.02314 0.00402 0.00009 0.00019 0.00014 0.00000 0.00089 0.00099 0.00091 0.00073 0.00077 0.00074 0.00039 H9A -0.04117 -0.05024 0.09669 1.00000 0.03471 0.00000 0.00000 H9B 0.02803 -0.07148 0.20388 1.00000 0.03471 0.00000 0.00000 H9C 0.02370 -0.05474 0.09605 1.00000 0.03471 0.00000 0.00000 C10 0.17152 0.10873 0.20119 1.00000 0.02028 0.02573 0.02257 0.00339 0.01245 0.00376 0.02249 0.00424 0.00008 0.00020 0.00013 0.00000 0.00089 0.00100 0.00090 0.00075 0.00077 0.00075 0.00039 H10 0.14912 0.01526 0.17068 1.00000 0.02699 0.00000 0.00000 C11 0.24494 0.08863 0.25361 1.00000 0.02580 0.05392 0.03193 0.01262 0.01892 0.01314 0.03560 0.00519 0.00009 0.00026 0.00016 0.00000 0.00103 0.00148 0.00108 0.00098 0.00090 0.00096 0.00051 H11A 0.25350 0.05075 0.20248 1.00000 0.05340 0.00000 0.00000 H11B 0.26134 0.02119 0.31197 1.00000 0.05340 0.00000 0.00000 H11C 0.26693 0.18111 0.27989 1.00000 0.05340 0.00000 0.00000 C12 0.14536 0.22006 0.11413 1.00000 0.02518 0.03355 0.02286 0.00505 0.01424 0.00213 0.02664 0.00450 0.00009 0.00021 0.00014 0.00000 0.00095 0.00116 0.00092 0.00079 0.00080 0.00082 0.00042 H12A 0.16420 0.31391 0.14435 1.00000 0.03996 0.00000 0.00000 H12B 0.09789 0.22515 0.07734 1.00000 0.03996 0.00000 0.00000 H12C 0.15719 0.19266 0.06475 1.00000 0.03996 0.00000 0.00000 C13 0.16486 -0.00708 0.37286 1.00000 0.01966 0.02142 0.02160 0.00206 0.01110 0.00029 0.02100 0.00400 0.00008 0.00019 0.00013 0.00000 0.00086 0.00097 0.00088 0.00071 0.00075 0.00071 0.00038 H13 0.12859 -0.00948 0.38446 1.00000 0.02520 0.00000 0.00000 C14 0.22879 0.00095 0.48165 1.00000 0.02297 0.03277 0.02153 0.00651 0.00840 0.00489 0.02774 0.00431 0.00009 0.00022 0.00014 0.00000 0.00093 0.00113 0.00092 0.00080 0.00080 0.00081 0.00043 H14A 0.23233 -0.08314 0.52286 1.00000 0.04162 0.00000 0.00000 H14B 0.22896 0.08812 0.51754 1.00000 0.04162 0.00000 0.00000 H14C 0.26575 0.00298 0.47374 1.00000 0.04162 0.00000 0.00000 C15 0.16318 -0.14949 0.32242 1.00000 0.03143 0.01810 0.03341 0.00269 0.01454 0.00140 0.02934 0.00457 0.00010 0.00020 0.00015 0.00000 0.00107 0.00101 0.00106 0.00079 0.00091 0.00079 0.00044 H15A 0.20208 -0.15804 0.32000 1.00000 0.04401 0.00000 0.00000 H15B 0.12424 -0.15338 0.25117 1.00000 0.04401 0.00000 0.00000 H15C 0.16213 -0.22852 0.36368 1.00000 0.04401 0.00000 0.00000 P1 0.15665 0.16510 0.30333 1.00000 0.01485 0.01670 0.01771 -0.00014 0.00722 -0.00027 0.01731 0.00099 0.00002 0.00005 0.00003 0.00000 0.00022 0.00025 0.00022 0.00017 0.00018 0.00017 0.00011 Fe1 0.00000 0.26191 0.25000 0.50000 0.01383 0.01558 0.01518 0.00000 0.00662 0.00000 0.01556 0.00034 0.00000 0.00004 0.00000 0.00000 0.00017 0.00019 0.00017 0.00000 0.00014 0.00000 0.00010 Final Structure Factor Calculation for 04src0551 in C2/c Total number of l.s. parameters = 158 Maximum vector length = 511 Memory required = 2782 / 22995 wR2 = 0.0770 before cycle 6 for 3356 data and 0 / 158 parameters GooF = S = 1.039; Restrained GooF = 1.039 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0268 * P )^2 + 3.54 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0341 for 2689 Fo > 4sig(Fo) and 0.0524 for all 3356 data wR2 = 0.0770, GooF = S = 1.039, Restrained GooF = 1.039 for all data Occupancy sum of asymmetric unit = 16.50 for non-hydrogen and 26.00 for hydrogen atoms Principal mean square atomic displacements U 0.0189 0.0174 0.0158 C1 0.0223 0.0189 0.0162 C2 0.0280 0.0205 0.0153 C3 0.0279 0.0180 0.0140 C4 0.0229 0.0186 0.0152 C5 0.0361 0.0237 0.0178 C6 0.0473 0.0290 0.0162 C7 0.0407 0.0278 0.0149 C8 0.0294 0.0232 0.0168 C9 0.0283 0.0210 0.0182 C10 0.0611 0.0265 0.0192 C11 0.0356 0.0247 0.0196 C12 0.0240 0.0196 0.0194 C13 0.0358 0.0305 0.0170 C14 0.0399 0.0305 0.0176 C15 0.0206 0.0167 0.0146 P1 0.0176 0.0156 0.0135 Fe1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.014 0.028 0.041 0.055 0.070 0.087 0.107 0.137 0.186 1.000 Number in group 340. 332. 351. 329. 340. 341. 318. 337. 335. 333. GooF 0.917 1.013 1.061 1.118 1.073 0.988 1.132 1.019 0.979 1.076 K 1.553 0.833 0.990 0.985 0.980 0.980 0.981 1.003 1.014 1.006 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.31 1.64 inf Number in group 340. 336. 340. 329. 334. 339. 333. 336. 334. 335. GooF 0.981 0.923 0.990 0.995 0.836 0.926 0.977 0.983 1.031 1.572 K 0.996 1.020 0.989 0.990 1.003 1.016 1.015 1.008 1.012 0.992 R1 0.150 0.098 0.093 0.063 0.047 0.042 0.036 0.030 0.024 0.027 Recommended weighting scheme: WGHT 0.0266 3.5635 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) 4 4 0 1079.23 1563.62 5.51 0.106 2.12 8 0 2 1810.53 1318.81 5.06 0.097 2.03 9 1 1 448.27 252.18 5.04 0.043 2.01 7 3 1 1288.25 1663.09 4.20 0.109 1.98 0 4 2 3290.88 2720.52 4.06 0.140 2.19 1 5 0 1845.49 1467.29 3.90 0.103 1.86 6 2 2 5083.71 5928.13 3.87 0.207 2.20 -14 2 3 415.64 257.06 3.79 0.043 1.60 -11 3 4 374.24 549.93 3.71 0.063 1.81 6 4 0 800.41 591.44 3.65 0.065 1.93 8 2 0 858.82 1107.91 3.51 0.089 2.25 5 3 1 184.37 304.14 3.51 0.047 2.30 2 4 2 8034.35 9095.79 3.43 0.256 2.07 5 7 6 61.16 217.83 3.40 0.040 1.02 2 0 2 61.31 143.56 3.31 0.032 4.44 2 4 0 7617.71 8570.81 3.21 0.248 2.28 6 4 2 864.65 670.81 3.20 0.070 1.71 1 5 1 92.73 194.47 3.17 0.037 1.83 1 3 4 1239.08 1511.44 3.16 0.104 2.13 -4 2 4 45.43 9.98 3.12 0.008 2.95 1 9 7 159.21 348.48 3.09 0.050 0.89 0 2 0 2851.80 2443.42 3.08 0.133 4.67 -7 1 5 2545.59 2190.33 3.03 0.126 2.73 -18 0 6 6104.30 5358.43 3.02 0.196 1.37 -29 1 15 2782.47 128.32 2.99 0.030 0.80 3 1 1 1102.51 901.70 2.99 0.081 4.41 5 1 3 4881.90 5502.67 2.98 0.199 2.30 -9 5 10 23.96 89.75 2.88 0.025 1.18 -21 5 2 140.38 286.25 2.85 0.045 0.92 3 5 2 371.07 254.08 2.85 0.043 1.67 3 1 6 173.24 276.07 2.84 0.045 1.75 3 5 1 2242.15 2600.12 2.84 0.137 1.75 -18 8 14 318.66 32.30 2.82 0.015 0.78 1 7 2 46.55 142.29 2.82 0.032 1.29 3 3 5 9214.37 8340.44 2.78 0.245 1.71 8 6 1 2489.88 2865.58 2.75 0.144 1.29 -7 1 6 302.24 212.82 2.71 0.039 2.41 5 5 4 -17.33 28.75 2.71 0.014 1.38 -2 4 4 2839.75 2473.17 2.69 0.133 1.97 1 7 4 1084.32 1302.98 2.68 0.097 1.21 7 11 1 1188.93 536.20 2.68 0.062 0.81 5 11 0 589.14 924.25 2.65 0.082 0.83 6 4 13 -67.77 107.18 2.64 0.028 0.78 -24 2 11 83.33 0.14 2.63 0.001 0.98 -28 0 10 828.46 1150.55 2.62 0.091 0.88 11 1 2 4003.25 3574.24 2.62 0.160 1.55 -3 1 16 630.25 814.21 2.61 0.077 0.85 -1 1 6 4669.30 4194.07 2.56 0.174 2.19 -8 2 2 492.95 623.90 2.56 0.067 2.54 -14 6 8 1124.42 1345.54 2.56 0.098 1.12 Bond lengths and angles C1 - Distance Angles C2 1.4434 (0.0024) C5 1.4496 (0.0024) 106.95 (0.14) P1 1.8247 (0.0018) 118.03 (0.12) 133.88 (0.13) Fe1 2.0585 (0.0017) 69.16 (0.09) 69.81 (0.09) 134.81 (0.09) C1 - C2 C5 P1 C2 - Distance Angles C3 1.4215 (0.0025) C1 1.4434 (0.0024) 108.45 (0.15) C6 1.4994 (0.0025) 124.30 (0.16) 127.08 (0.15) Fe1 2.0511 (0.0017) 70.55 (0.10) 69.71 (0.09) 129.27 (0.13) C2 - C3 C1 C6 C3 - Distance Angles C2 1.4215 (0.0025) C4 1.4227 (0.0026) 108.32 (0.15) C7 1.5038 (0.0025) 126.16 (0.17) 125.28 (0.16) Fe1 2.0702 (0.0017) 69.10 (0.10) 70.30 (0.10) 130.74 (0.13) C3 - C2 C4 C7 C4 - Distance Angles C3 1.4227 (0.0026) C5 1.4301 (0.0025) 108.57 (0.15) C8 1.5074 (0.0024) 123.72 (0.16) 127.50 (0.17) Fe1 2.0796 (0.0017) 69.60 (0.10) 69.42 (0.10) 130.91 (0.13) C4 - C3 C5 C8 C5 - Distance Angles C4 1.4301 (0.0025) C1 1.4496 (0.0024) 107.71 (0.15) C9 1.4996 (0.0025) 125.38 (0.15) 126.80 (0.15) Fe1 2.0685 (0.0017) 70.25 (0.10) 69.07 (0.09) 129.12 (0.12) C5 - C4 C1 C9 C6 - Distance Angles C2 1.4994 (0.0025) H6A 0.9800 109.47 H6B 0.9800 109.47 109.47 H6C 0.9800 109.47 109.47 109.47 C6 - C2 H6A H6B C7 - Distance Angles C3 1.5038 (0.0025) H7A 0.9800 109.47 H7B 0.9800 109.47 109.47 H7C 0.9800 109.47 109.47 109.47 C7 - C3 H7A H7B C8 - Distance Angles C4 1.5074 (0.0024) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - C4 H8A H8B C9 - Distance Angles C5 1.4996 (0.0025) H9A 0.9800 109.47 H9B 0.9800 109.47 109.47 H9C 0.9800 109.47 109.47 109.47 C9 - C5 H9A H9B C10 - Distance Angles C12 1.5252 (0.0025) C11 1.5322 (0.0025) 110.59 (0.16) P1 1.8640 (0.0018) 110.87 (0.13) 108.19 (0.13) H10 1.0000 109.05 109.05 109.05 C10 - C12 C11 P1 C11 - Distance Angles C10 1.5322 (0.0025) H11A 0.9800 109.47 H11B 0.9800 109.47 109.47 H11C 0.9800 109.47 109.47 109.47 C11 - C10 H11A H11B C12 - Distance Angles C10 1.5252 (0.0025) H12A 0.9800 109.47 H12B 0.9800 109.47 109.47 H12C 0.9800 109.47 109.47 109.47 C12 - C10 H12A H12B C13 - Distance Angles C15 1.5258 (0.0026) C14 1.5411 (0.0025) 108.47 (0.15) P1 1.8755 (0.0018) 119.69 (0.13) 107.41 (0.12) H13 1.0000 106.88 106.88 106.88 C13 - C15 C14 P1 C14 - Distance Angles C13 1.5411 (0.0025) H14A 0.9800 109.47 H14B 0.9800 109.47 109.47 H14C 0.9800 109.47 109.47 109.47 C14 - C13 H14A H14B C15 - Distance Angles C13 1.5258 (0.0026) H15A 0.9800 109.47 H15B 0.9800 109.47 109.47 H15C 0.9800 109.47 109.47 109.47 C15 - C13 H15A H15B P1 - Distance Angles C1 1.8247 (0.0018) C10 1.8640 (0.0018) 100.52 (0.08) C13 1.8755 (0.0018) 109.04 (0.08) 102.90 (0.08) P1 - C1 C10 Fe1 - Distance Angles C2_$1 2.0511 (0.0017) C2 2.0511 (0.0017) 124.47 (0.10) C1_$1 2.0585 (0.0017) 41.12 (0.07) 162.90 (0.07) C1 2.0585 (0.0017) 162.90 (0.07) 41.12 (0.07) 154.90 (0.10) C5 2.0685 (0.0017) 153.61 (0.07) 68.71 (0.07) 120.31 (0.07) 41.13 (0.07) C5_$1 2.0685 (0.0017) 68.71 (0.07) 153.61 (0.07) 41.13 (0.07) 120.31 (0.07) 110.25 (0.10) C3_$1 2.0702 (0.0017) 40.35 (0.07) 106.09 (0.07) 68.52 (0.07) 126.32 (0.07) 165.63 (0.07) 68.07 (0.07) C3 2.0702 (0.0017) 106.09 (0.07) 40.35 (0.07) 126.32 (0.07) 68.52 (0.07) 68.07 (0.07) 165.63 (0.07) 117.28 (0.10) C4 2.0796 (0.0017) 118.67 (0.07) 67.85 (0.07) 108.69 (0.07) 68.38 (0.07) 40.33 (0.07) 129.50 (0.07) 151.62 (0.07) C4_$1 2.0796 (0.0017) 67.85 (0.07) 118.67 (0.07) 68.38 (0.07) 108.69 (0.07) 129.50 (0.07) 40.33 (0.07) 40.10 (0.07) Fe1 - C2_$1 C2 C1_$1 C1 C5 C5_$1 C3_$1 FMAP and GRID set by program FMAP 2 1 40 GRID -0.676 -2 -1 0.676 2 1 R1 = 0.0504 for 3356 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.36 at 0.1547 0.3310 0.3037 [ 1.39 A from H6B ] Deepest hole -0.30 at 0.0341 0.2680 0.2570 [ 0.79 A from FE1 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 2944 / 38156 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1547 0.3310 0.3037 1.00000 0.05 0.36 1.39 H6B 1.55 P1 1.85 C6 2.04 C1 Q2 1 0.0458 0.1598 0.1997 1.00000 0.05 0.30 0.72 C1 0.79 C5 1.92 C2 1.93 FE1 Q3 1 0.0653 0.2957 0.2083 1.00000 0.05 0.30 0.68 C2 0.78 C1 1.79 C3 1.87 C5 Q4 1 0.0210 0.3766 0.1612 1.00000 0.05 0.29 0.70 C3 0.73 C2 1.81 C4 1.85 C1 Q5 1 -0.0317 0.3173 0.0917 1.00000 0.05 0.27 0.73 C3 0.77 C4 1.88 C7 1.90 C8 Shortest distances between peaks (including symmetry equivalents) 3 4 1.19 4 5 1.27 2 3 1.34 1 3 1.88 3 5 2.06 2 4 2.10 2 5 2.25 1 2 2.75 1 4 2.80 Time profile in seconds ----------------------- 0.03: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.02: 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. 0.11: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.63: Structure factors and derivatives 0.77: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.08: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.13: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.11: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 04src0551 finished at 15:13:31 Total CPU time: 3.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++