+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2005src0348 started at 15:33:24 on 24-May-2005 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2005src0348 in P-1 CELL 0.71073 9.2976 11.4767 11.5814 90.2293 99.1866 95.1936 ZERR 2.0 0.0021 0.0016 0.0007 0.0100 0.0080 0.0150 LATT 1 SFAC C H P CL FE UNIT 40 56 2 8 2 V = 1214.73 F(000) = 514.0 Mu = 1.13 mm-1 Cell Wt = 994.09 Rho = 1.359 MERG 2 OMIT -3.00 55.00 BASF 0.48355 EXTI 0.01234 SHEL 7 0.77 FMAP 2 PLAN 5 SIZE 0.02 0.17 0.33 ACTA BOND $H WGHT 0.09620 15.38790 L.S. 10 TEMP -153.00 FVAR 1.16604 MOLE 1 C1 1 0.050112 0.241624 0.130814 11.00000 0.02145 0.01687 = 0.01547 0.00676 -0.00198 0.00447 C2 1 0.084531 0.225084 0.019708 11.00000 0.03359 0.01433 = 0.02144 0.00213 -0.00251 0.00426 AFIX 43 H2 2 0.178992 0.204029 0.011336 11.00000 -1.20000 AFIX 0 C3 1 -0.018933 0.239352 -0.078274 11.00000 0.03782 0.02197 = 0.02107 -0.00255 -0.00194 0.00267 AFIX 43 H3 2 0.005096 0.229525 -0.154202 11.00000 -1.20000 AFIX 0 C4 1 -0.158052 0.268011 -0.066487 11.00000 0.04289 0.02367 = 0.02167 -0.00228 -0.00903 0.00978 AFIX 43 H4 2 -0.230364 0.273856 -0.134187 11.00000 -1.20000 AFIX 0 C5 1 -0.191404 0.287974 0.043119 11.00000 0.02438 0.02493 = 0.03257 -0.00160 -0.00781 0.01163 AFIX 43 H5 2 -0.285222 0.311697 0.049701 11.00000 -1.20000 AFIX 0 C6 1 -0.090121 0.274093 0.145148 11.00000 0.01962 0.02266 = 0.01988 0.00658 -0.00711 0.00263 C7 1 -0.132192 0.298531 0.261139 11.00000 0.01574 0.02994 = 0.02531 -0.00330 -0.00245 0.01003 C8 1 -0.177122 0.210023 0.329655 11.00000 0.02527 0.03079 = 0.03201 0.00763 0.00116 0.00754 AFIX 43 H8 2 -0.184750 0.131107 0.302214 11.00000 -1.20000 AFIX 0 C9 1 -0.212121 0.235067 0.440508 11.00000 0.02839 0.04403 = 0.03120 0.00502 0.00775 0.00194 AFIX 43 H9 2 -0.241099 0.173326 0.488585 11.00000 -1.20000 AFIX 0 C10 1 -0.203967 0.349778 0.478566 11.00000 0.03297 0.04725 = 0.02957 -0.01152 0.00685 0.00210 AFIX 43 H10 2 -0.228414 0.367447 0.552866 11.00000 -1.20000 AFIX 0 C11 1 -0.160685 0.438499 0.409553 11.00000 0.03527 0.03531 = 0.04897 -0.00933 0.01697 0.00114 AFIX 43 H11 2 -0.155148 0.517545 0.436206 11.00000 -1.20000 AFIX 0 C12 1 -0.124977 0.413538 0.301160 11.00000 0.03372 0.02936 = 0.03721 -0.00062 0.00740 0.00939 AFIX 43 H12 2 -0.095289 0.475644 0.253783 11.00000 -1.20000 AFIX 0 C13 1 0.338246 0.355163 0.252864 11.00000 0.02051 0.01206 = 0.02467 0.00105 -0.00461 0.00318 C14 1 0.457105 0.321449 0.185604 11.00000 0.02565 0.02486 = 0.03223 0.00180 0.00079 0.00395 AFIX 137 H14A 2 0.528792 0.389104 0.183075 11.00000 -1.50000 H14B 2 0.412342 0.296704 0.105498 11.00000 -1.50000 H14C 2 0.506481 0.256895 0.225063 11.00000 -1.50000 AFIX 0 C15 1 0.405770 0.389208 0.380654 11.00000 0.02484 0.01787 = 0.02996 -0.00255 -0.00505 -0.00201 AFIX 137 H15A 2 0.444739 0.320694 0.420642 11.00000 -1.50000 H15B 2 0.330203 0.417022 0.421117 11.00000 -1.50000 H15C 2 0.485321 0.451565 0.381491 11.00000 -1.50000 AFIX 0 C16 1 0.265834 0.460695 0.195606 11.00000 0.01735 0.01806 = 0.04990 0.00246 -0.01125 -0.00193 AFIX 137 H16A 2 0.189181 0.481483 0.238822 11.00000 -1.50000 H16B 2 0.222205 0.440516 0.114124 11.00000 -1.50000 H16C 2 0.339917 0.527418 0.197338 11.00000 -1.50000 AFIX 0 C17 1 0.246753 0.084522 0.276768 11.00000 0.03086 0.01346 = 0.02420 -0.00163 0.00397 0.00339 C18 1 0.292467 0.033304 0.168905 11.00000 0.03906 0.01997 = 0.03114 0.00078 -0.00136 0.00812 AFIX 137 H18A 2 0.323515 -0.045179 0.185919 11.00000 -1.50000 H18B 2 0.374078 0.083721 0.146941 11.00000 -1.50000 H18C 2 0.209382 0.028235 0.104073 11.00000 -1.50000 AFIX 0 C19 1 0.372264 0.083798 0.380763 11.00000 0.02967 0.02330 = 0.02435 -0.00045 -0.00321 0.00936 AFIX 137 H19A 2 0.342091 0.116430 0.450526 11.00000 -1.50000 H19B 2 0.458521 0.131330 0.362798 11.00000 -1.50000 H19C 2 0.396562 0.003171 0.395565 11.00000 -1.50000 AFIX 0 C20 1 0.111389 0.011935 0.308545 11.00000 0.03973 0.02175 = 0.02990 0.00204 0.00297 -0.00001 AFIX 137 H20A 2 0.029079 0.013226 0.243582 11.00000 -1.50000 H20B 2 0.084833 0.045543 0.379325 11.00000 -1.50000 H20C 2 0.134228 -0.069096 0.322923 11.00000 -1.50000 AFIX 0 P1 3 0.192324 0.235596 0.255423 11.00000 0.01857 0.01692 = 0.01656 -0.00075 -0.00116 0.00364 H1P 2 0.131837 0.258915 0.348173 11.00000 0.00741 MOLE 2 CL1 4 0.849039 0.778299 0.392018 11.00000 0.02938 0.04857 = 0.03199 -0.00018 -0.00446 0.00069 CL2 4 0.671279 0.933599 0.149196 11.00000 0.05498 0.02500 = 0.03528 0.00852 0.01285 0.00746 CL3 4 0.456036 0.763810 0.333816 11.00000 0.02554 0.03490 = 0.02004 0.00209 0.00138 0.00363 CL4 4 0.646488 0.622622 0.138070 11.00000 0.05331 0.02324 = 0.03464 -0.00469 0.01363 -0.00093 FE1 5 0.655917 0.775487 0.252846 11.00000 0.02825 0.02187 = 0.02050 0.00068 0.00314 0.00084 HKLF 5 Covalent radii and connectivity table for 2005src0348 in P-1 C 0.770 H 0.320 P 1.100 CL 0.990 FE 1.240 C1 - C2 C6 P1 C2 - C3 C1 C3 - C2 C4 C4 - C5 C3 C5 - C4 C6 C6 - C5 C1 C7 C7 - C8 C12 C6 C8 - C7 C9 C9 - C10 C8 C10 - C11 C9 C11 - C10 C12 C12 - C11 C7 C13 - C14 C16 C15 P1 C14 - C13 C15 - C13 C16 - C13 C17 - C18 C19 C20 P1 C18 - C17 C19 - C17 C20 - C17 P1 - C1 C13 C17 Cl1 - Fe1 Cl2 - Fe1 Cl3 - Fe1 Cl4 - Fe1 Fe1 - Cl4 Cl2 Cl3 Cl1 ** MERG code changed to 0 for compatibility with HKLF and BASF parameters ** 16921 Reflections read, of which 68 rejected -12 =< h =< 12, -14 =< k =< 14, -15 =< l =< 15, Max. 2-theta = 54.97 0 Systematic absence violations 0 Data suppressed, R(sigma) = 0.0840 Maximum memory for data reduction = 2642 / 5 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 = 3369 / 307573 wR2 = 0.2891 before cycle 1 for 16853 data and 247 / 247 parameters GooF = S = 1.131; Restrained GooF = 1.131 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0962 * P )^2 + 15.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.16445 0.00422 -0.377 OSF 2 0.48355 0.00197 0.002 BASF 1 3 0.01228 0.00362 -0.017 EXTI Mean shift/esd = 0.048 Maximum = -0.377 for OSF Max. shift = 0.003 A for H1P Max. dU = 0.001 for H1P Least-squares cycle 2 Maximum vector length = 511 Memory required = 3369 / 307573 wR2 = 0.2889 before cycle 2 for 16853 data and 247 / 247 parameters GooF = S = 1.129; Restrained GooF = 1.129 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0962 * P )^2 + 15.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.16472 0.00422 0.064 OSF 2 0.48356 0.00197 0.001 BASF 1 3 0.01225 0.00361 -0.008 EXTI Mean shift/esd = 0.017 Maximum = 0.101 for U13 Fe1 Max. shift = 0.001 A for H1P Max. dU = 0.000 for H1P Least-squares cycle 3 Maximum vector length = 511 Memory required = 3369 / 307573 wR2 = 0.2889 before cycle 3 for 16853 data and 247 / 247 parameters GooF = S = 1.129; Restrained GooF = 1.129 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0962 * P )^2 + 15.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.16474 0.00422 0.006 OSF 2 0.48356 0.00197 0.002 BASF 1 3 0.01225 0.00361 0.001 EXTI Mean shift/esd = 0.002 Maximum = 0.006 for OSF Max. shift = 0.000 A for H1P Max. dU = 0.000 for C11 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3369 / 307573 wR2 = 0.2889 before cycle 4 for 16853 data and 247 / 247 parameters GooF = S = 1.128; Restrained GooF = 1.128 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0962 * P )^2 + 15.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.16474 0.00422 -0.002 OSF 2 0.48356 0.00197 -0.001 BASF 1 3 0.01225 0.00361 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.003 for z C7 Max. shift = 0.000 A for H1P Max. dU = 0.000 for H1P Least-squares cycle 5 Maximum vector length = 511 Memory required = 3369 / 307573 wR2 = 0.2889 before cycle 5 for 16853 data and 247 / 247 parameters GooF = S = 1.128; Restrained GooF = 1.128 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0962 * P )^2 + 15.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.16474 0.00422 0.001 OSF 2 0.48356 0.00197 0.000 BASF 1 3 0.01226 0.00361 0.001 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for EXTI Max. shift = 0.000 A for H20B Max. dU = 0.000 for H1P Least-squares cycle 6 Maximum vector length = 511 Memory required = 3369 / 307573 wR2 = 0.2889 before cycle 6 for 16853 data and 247 / 247 parameters GooF = S = 1.128; Restrained GooF = 1.128 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0962 * P )^2 + 15.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.16474 0.00422 0.000 OSF 2 0.48356 0.00197 0.000 BASF 1 3 0.01226 0.00361 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for EXTI Max. shift = 0.000 A for H20B Max. dU = 0.000 for C14 Least-squares cycle 7 Maximum vector length = 511 Memory required = 3369 / 307573 wR2 = 0.2889 before cycle 7 for 16853 data and 247 / 247 parameters GooF = S = 1.128; Restrained GooF = 1.128 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0962 * P )^2 + 15.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.16474 0.00422 0.000 OSF 2 0.48356 0.00197 0.000 BASF 1 3 0.01226 0.00361 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for EXTI Max. shift = 0.000 A for H20B Max. dU = 0.000 for C15 Least-squares cycle 8 Maximum vector length = 511 Memory required = 3369 / 307573 wR2 = 0.2889 before cycle 8 for 16853 data and 247 / 247 parameters GooF = S = 1.128; Restrained GooF = 1.128 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0962 * P )^2 + 15.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.16474 0.00422 0.000 OSF 2 0.48356 0.00197 0.000 BASF 1 3 0.01226 0.00361 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H20B Max. dU = 0.000 for H1P Least-squares cycle 9 Maximum vector length = 511 Memory required = 3369 / 307573 wR2 = 0.2889 before cycle 9 for 16853 data and 247 / 247 parameters GooF = S = 1.128; Restrained GooF = 1.128 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0962 * P )^2 + 15.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.16474 0.00422 0.000 OSF 2 0.48356 0.00197 0.000 BASF 1 3 0.01226 0.00361 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for x Cl1 Max. shift = 0.000 A for H1P Max. dU = 0.000 for H1P Least-squares cycle 10 Maximum vector length = 511 Memory required = 3369 / 307573 wR2 = 0.2889 before cycle 10 for 16853 data and 247 / 247 parameters GooF = S = 1.128; Restrained GooF = 1.128 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0962 * P )^2 + 15.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.16474 0.00422 0.000 OSF 2 0.48356 0.00197 0.000 BASF 1 3 0.01226 0.00361 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H10 Max. dU = 0.000 for C11 Largest correlation matrix elements 0.717 EXTI / OSF Idealized hydrogen atom generation before cycle 11 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.1788 0.2040 0.0110 43 0.950 0.000 C2 C3 C1 H3 0.0054 0.2295 -0.1541 43 0.950 0.000 C3 C2 C4 H4 -0.2299 0.2738 -0.1339 43 0.950 0.000 C4 C5 C3 H5 -0.2849 0.3117 0.0501 43 0.950 0.000 C5 C4 C6 H8 -0.1847 0.1312 0.3023 43 0.950 0.000 C8 C7 C9 H9 -0.2411 0.1733 0.4887 43 0.950 0.000 C9 C10 C8 H10 -0.2285 0.3673 0.5529 43 0.950 0.000 C10 C11 C9 H11 -0.1552 0.5174 0.4361 43 0.950 0.000 C11 C10 C12 H12 -0.0953 0.4756 0.2536 43 0.950 0.000 C12 C11 C7 H14A 0.5288 0.3891 0.1829 137 0.980 0.000 C14 C13 H14A H14B 0.4128 0.2967 0.1058 137 0.980 0.000 C14 C13 H14A H14C 0.5060 0.2570 0.2250 137 0.980 0.000 C14 C13 H14A H15A 0.4445 0.3208 0.4204 137 0.980 0.000 C15 C13 H15A H15B 0.3304 0.4170 0.4214 137 0.980 0.000 C15 C13 H15A H15C 0.4853 0.4516 0.3811 137 0.980 0.000 C15 C13 H15A H16A 0.1891 0.4813 0.2389 137 0.980 0.000 C16 C13 H16A H16B 0.2225 0.4404 0.1144 137 0.980 0.000 C16 C13 H16A H16C 0.3396 0.5275 0.1969 137 0.980 0.000 C16 C13 H16A H18A 0.3233 -0.0451 0.1859 137 0.980 0.000 C18 C17 H18A H18B 0.3741 0.0837 0.1466 137 0.980 0.000 C18 C17 H18A H18C 0.2098 0.0283 0.1045 137 0.980 0.000 C18 C17 H18A H19A 0.3420 0.1164 0.4504 137 0.980 0.000 C19 C17 H19A H19B 0.4585 0.1313 0.3625 137 0.980 0.000 C19 C17 H19A H19C 0.3963 0.0032 0.3955 137 0.980 0.000 C19 C17 H19A H20A 0.0296 0.0135 0.2439 137 0.980 0.000 C20 C17 H20A H20B 0.0846 0.0453 0.3794 137 0.980 0.000 C20 C17 H20A H20C 0.1340 -0.0690 0.3227 137 0.980 0.000 C20 C17 H20A 2005src0348 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.05015 0.24162 0.13082 1.00000 0.02165 0.01629 0.01573 0.00664 -0.00179 0.00449 0.01823 0.00979 0.00057 0.00049 0.00044 0.00000 0.00276 0.00299 0.00258 0.00222 0.00205 0.00239 0.00118 C2 0.08453 0.22506 0.01969 1.00000 0.03377 0.01421 0.02152 0.00185 -0.00235 0.00438 0.02378 0.01036 0.00065 0.00054 0.00047 0.00000 0.00316 0.00297 0.00278 0.00248 0.00232 0.00273 0.00125 H2 0.17876 0.20400 0.01096 1.00000 0.02853 0.00000 0.00000 C3 -0.01894 0.23934 -0.07827 1.00000 0.03805 0.02170 0.02135 -0.00285 -0.00162 0.00265 0.02775 0.01061 0.00066 0.00055 0.00052 0.00000 0.00356 0.00347 0.00297 0.00248 0.00252 0.00284 0.00143 H3 0.00540 0.22945 -0.15409 1.00000 0.03330 0.00000 0.00000 C4 -0.15804 0.26803 -0.06649 1.00000 0.04294 0.02391 0.02179 -0.00209 -0.00907 0.00966 0.03071 0.01109 0.00070 0.00057 0.00051 0.00000 0.00367 0.00353 0.00291 0.00275 0.00252 0.00315 0.00147 H4 -0.22992 0.27384 -0.13390 1.00000 0.03686 0.00000 0.00000 C5 -0.19137 0.28799 0.04313 1.00000 0.02462 0.02530 0.03278 -0.00128 -0.00743 0.01162 0.02832 0.01067 0.00064 0.00057 0.00052 0.00000 0.00303 0.00345 0.00331 0.00287 0.00246 0.00288 0.00141 H5 -0.28495 0.31171 0.05006 1.00000 0.03398 0.00000 0.00000 C6 -0.09017 0.27409 0.14511 1.00000 0.01980 0.02290 0.02005 0.00688 -0.00687 0.00296 0.02195 0.01011 0.00057 0.00055 0.00046 0.00000 0.00274 0.00325 0.00271 0.00255 0.00211 0.00263 0.00125 C7 -0.13215 0.29859 0.26117 1.00000 0.01560 0.03030 0.02570 -0.00298 -0.00213 0.01007 0.02398 0.01076 0.00059 0.00058 0.00051 0.00000 0.00276 0.00356 0.00299 0.00267 0.00221 0.00264 0.00134 C8 -0.17708 0.21001 0.32965 1.00000 0.02541 0.03033 0.03236 0.00744 0.00133 0.00749 0.02941 0.01203 0.00063 0.00065 0.00053 0.00000 0.00313 0.00376 0.00334 0.00311 0.00249 0.00300 0.00142 H8 -0.18471 0.13119 0.30230 1.00000 0.03529 0.00000 0.00000 C9 -0.21209 0.23507 0.44050 1.00000 0.02888 0.04391 0.03154 0.00473 0.00821 0.00178 0.03450 0.01246 0.00068 0.00067 0.00058 0.00000 0.00346 0.00459 0.00354 0.00308 0.00270 0.00313 0.00165 H9 -0.24108 0.17334 0.48868 1.00000 0.04140 0.00000 0.00000 C10 -0.20401 0.34977 0.47856 1.00000 0.03287 0.04752 0.02986 -0.01134 0.00720 0.00212 0.03664 0.01249 0.00072 0.00071 0.00060 0.00000 0.00366 0.00473 0.00352 0.00354 0.00277 0.00352 0.00170 H10 -0.22852 0.36729 0.55287 1.00000 0.04397 0.00000 0.00000 C11 -0.16073 0.43846 0.40953 1.00000 0.03510 0.03556 0.04930 -0.00922 0.01709 0.00080 0.03904 0.01367 0.00076 0.00069 0.00067 0.00000 0.00404 0.00439 0.00465 0.00364 0.00335 0.00341 0.00180 H11 -0.15520 0.51741 0.43607 1.00000 0.04684 0.00000 0.00000 C12 -0.12498 0.41351 0.30112 1.00000 0.03404 0.02959 0.03772 -0.00083 0.00779 0.00933 0.03317 0.01252 0.00072 0.00063 0.00060 0.00000 0.00382 0.00392 0.00403 0.00304 0.00300 0.00314 0.00162 H12 -0.09527 0.47559 0.25363 1.00000 0.03981 0.00000 0.00000 C13 0.33825 0.35518 0.25286 1.00000 0.02068 0.01213 0.02460 0.00120 -0.00479 0.00346 0.01994 0.01002 0.00061 0.00048 0.00050 0.00000 0.00288 0.00287 0.00291 0.00227 0.00224 0.00239 0.00123 C14 0.45710 0.32149 0.18563 1.00000 0.02593 0.02498 0.03228 0.00191 0.00077 0.00385 0.02806 0.01154 0.00063 0.00060 0.00052 0.00000 0.00311 0.00352 0.00328 0.00286 0.00246 0.00287 0.00138 H14A 0.52881 0.38906 0.18288 1.00000 0.04209 0.00000 0.00000 H14B 0.41280 0.29674 0.10579 1.00000 0.04209 0.00000 0.00000 H14C 0.50605 0.25700 0.22503 1.00000 0.04209 0.00000 0.00000 C15 0.40579 0.38923 0.38067 1.00000 0.02517 0.01765 0.03000 -0.00283 -0.00481 -0.00209 0.02555 0.01045 0.00067 0.00057 0.00054 0.00000 0.00330 0.00324 0.00351 0.00265 0.00258 0.00269 0.00141 H15A 0.44453 0.32076 0.42043 1.00000 0.03832 0.00000 0.00000 H15B 0.33039 0.41696 0.42143 1.00000 0.03832 0.00000 0.00000 H15C 0.48525 0.45155 0.38114 1.00000 0.03832 0.00000 0.00000 C16 0.26579 0.46066 0.19557 1.00000 0.01747 0.01786 0.05049 0.00256 -0.01109 -0.00212 0.03065 0.01166 0.00068 0.00056 0.00064 0.00000 0.00322 0.00337 0.00441 0.00291 0.00288 0.00261 0.00162 H16A 0.18910 0.48127 0.23892 1.00000 0.04597 0.00000 0.00000 H16B 0.22254 0.44038 0.11439 1.00000 0.04597 0.00000 0.00000 H16C 0.33963 0.52746 0.19694 1.00000 0.04597 0.00000 0.00000 C17 0.24678 0.08454 0.27676 1.00000 0.03120 0.01318 0.02456 -0.00176 0.00415 0.00338 0.02294 0.01094 0.00067 0.00053 0.00052 0.00000 0.00347 0.00300 0.00319 0.00241 0.00257 0.00257 0.00134 C18 0.29252 0.03334 0.16893 1.00000 0.03859 0.01998 0.03139 0.00074 -0.00163 0.00791 0.03046 0.01229 0.00075 0.00057 0.00057 0.00000 0.00406 0.00341 0.00366 0.00272 0.00300 0.00291 0.00157 H18A 0.32325 -0.04509 0.18587 1.00000 0.04570 0.00000 0.00000 H18B 0.37414 0.08366 0.14665 1.00000 0.04570 0.00000 0.00000 H18C 0.20976 0.02832 0.10450 1.00000 0.04570 0.00000 0.00000 C19 0.37227 0.08379 0.38072 1.00000 0.03003 0.02340 0.02468 -0.00046 -0.00282 0.00941 0.02640 0.01115 0.00067 0.00057 0.00054 0.00000 0.00353 0.00346 0.00334 0.00265 0.00264 0.00290 0.00145 H19A 0.34195 0.11635 0.45044 1.00000 0.03960 0.00000 0.00000 H19B 0.45851 0.13129 0.36251 1.00000 0.03960 0.00000 0.00000 H19C 0.39634 0.00324 0.39548 1.00000 0.03960 0.00000 0.00000 C20 0.11144 0.01199 0.30859 1.00000 0.04000 0.02178 0.02977 0.00216 0.00324 -0.00003 0.03095 0.01216 0.00074 0.00058 0.00058 0.00000 0.00401 0.00351 0.00355 0.00275 0.00292 0.00298 0.00152 H20A 0.02963 0.01347 0.24392 1.00000 0.04642 0.00000 0.00000 H20B 0.08464 0.04534 0.37936 1.00000 0.04642 0.00000 0.00000 H20C 0.13398 -0.06901 0.32274 1.00000 0.04642 0.00000 0.00000 P1 0.19233 0.23558 0.25542 1.00000 0.01868 0.01690 0.01662 -0.00073 -0.00107 0.00366 0.01771 0.00257 0.00015 0.00014 0.00012 0.00000 0.00071 0.00077 0.00066 0.00060 0.00051 0.00064 0.00033 H1P 0.13203 0.25868 0.34840 1.00000 0.00809 0.08591 0.00495 0.00454 0.00418 0.00000 0.01301 Cl1 0.84905 0.77830 0.39202 1.00000 0.02953 0.04861 0.03218 -0.00019 -0.00435 0.00067 0.03798 0.00301 0.00017 0.00018 0.00014 0.00000 0.00082 0.00112 0.00083 0.00083 0.00062 0.00084 0.00044 Cl2 0.67129 0.93360 0.14920 1.00000 0.05523 0.02501 0.03539 0.00853 0.01304 0.00742 0.03766 0.00354 0.00022 0.00015 0.00016 0.00000 0.00113 0.00090 0.00096 0.00071 0.00079 0.00081 0.00045 Cl3 0.45604 0.76380 0.33382 1.00000 0.02559 0.03495 0.02018 0.00210 0.00151 0.00359 0.02709 0.00268 0.00015 0.00015 0.00012 0.00000 0.00073 0.00091 0.00067 0.00065 0.00053 0.00069 0.00037 Cl4 0.64650 0.62261 0.13807 1.00000 0.05349 0.02328 0.03481 -0.00464 0.01374 -0.00091 0.03675 0.00321 0.00020 0.00015 0.00015 0.00000 0.00111 0.00087 0.00094 0.00070 0.00078 0.00079 0.00044 Fe1 0.65592 0.77549 0.25284 1.00000 0.02838 0.02189 0.02059 0.00070 0.00326 0.00081 0.02379 0.00158 0.00009 0.00008 0.00007 0.00000 0.00048 0.00049 0.00043 0.00036 0.00032 0.00039 0.00026 Final Structure Factor Calculation for 2005src0348 in P-1 Total number of l.s. parameters = 247 Maximum vector length = 511 Memory required = 3122 / 24017 wR2 = 0.2889 before cycle 11 for 16853 data and 0 / 247 parameters GooF = S = 1.128; Restrained GooF = 1.128 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0962 * P )^2 + 15.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1092 for 11859 Fo > 4sig(Fo) and 0.1614 for all 16853 data wR2 = 0.2889, GooF = S = 1.128, Restrained GooF = 1.128 for all data Occupancy sum of asymmetric unit = 26.00 for non-hydrogen and 28.00 for hydrogen atoms Principal mean square atomic displacements U 0.0256 0.0212 0.0078 C1 0.0381 0.0202 0.0130 C2 0.0415 0.0238 0.0180 C3 0.0541 0.0217 0.0164 C4 0.0460 0.0264 0.0126 C5 0.0343 0.0228 0.0088 C6 0.0370 0.0240 0.0110 C7 0.0383 0.0308 0.0192 C8 0.0453 0.0328 0.0254 C9 0.0540 0.0329 0.0230 C10 0.0583 0.0332 0.0256 C11 0.0385 0.0375 0.0235 C12 0.0329 0.0161 0.0108 C13 0.0350 0.0265 0.0227 C14 0.0389 0.0236 0.0141 C15 0.0611 0.0188 0.0120 C16 0.0314 0.0250 0.0125 C17 0.0450 0.0286 0.0178 C18 0.0387 0.0233 0.0172 C19 0.0419 0.0297 0.0212 C20 0.0231 0.0160 0.0140 P1 0.0495 0.0417 0.0227 Cl1 0.0564 0.0360 0.0205 Cl2 0.0351 0.0267 0.0194 Cl3 0.0562 0.0327 0.0213 Cl4 0.0291 0.0217 0.0205 Fe1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.033 0.058 0.083 0.110 0.140 0.174 0.213 0.274 0.380 1.000 Number in group 1709. 1681. 1688. 1657. 1703. 1698. 1670. 1684. 1668. 1695. GooF 1.392 1.202 1.206 1.213 1.092 1.003 0.983 0.920 1.002 1.187 K 6.158 1.643 1.199 1.073 1.055 1.032 1.038 1.009 1.024 1.014 Resolution(A) 0.77 0.81 0.85 0.90 0.96 1.04 1.13 1.25 1.46 1.81 inf Number in group 1725. 1647. 1683. 1695. 1669. 1701. 1670. 1684. 1683. 1696. GooF 1.331 1.262 1.160 1.134 1.116 1.033 1.027 1.030 1.008 1.135 K 1.112 1.069 1.074 1.076 1.067 1.035 1.022 0.998 1.026 1.011 R1 0.386 0.331 0.236 0.204 0.170 0.135 0.112 0.095 0.073 0.076 Recommended weighting scheme: WGHT 0.0965 15.3094 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) 2 -6 0 775.24 2.10 9.51 0.017 1.82 -2 6 0 728.27 2.10 9.50 0.017 1.82 -2 6 0 762.22 2.10 9.39 0.017 1.82 -2 6 -1 921.99 87.66 8.67 0.107 1.78 2 -6 1 763.80 87.66 7.62 0.107 1.78 0 -7 -2 -12.56 938.96 7.36 0.352 1.56 -1 -6 -5 266.41 0.67 5.88 0.009 1.40 -2 0 -2 2883.44 6791.06 5.63 0.946 3.32 -4 -6 1 816.52 2378.52 5.58 0.560 1.41 1 6 5 243.79 0.67 5.57 0.009 1.40 -2 0 9 1848.41 4677.92 5.29 0.785 1.28 3 -1 -9 692.71 198.77 5.14 0.162 1.24 2 -6 8 568.13 125.60 5.07 0.129 1.10 -3 8 -4 304.94 32.09 4.93 0.065 1.19 3 -6 -13 493.78 33.72 4.73 0.067 0.80 2 8 -3 177.62 1.87 4.51 0.016 1.28 2 -4 -11 371.21 41.97 4.45 0.074 0.99 -11 6 2 474.96 87.31 4.41 0.107 0.80 -2 -6 -5 3.68 299.50 4.41 0.199 1.32 0 8 4 189.93 1.87 4.36 0.016 1.27 -4 -5 0 646.55 1508.59 4.22 0.446 1.55 -4 -6 6 1095.05 2458.67 4.21 0.569 1.19 4 0 2 1041.36 2206.94 4.16 0.539 2.01 3 0 1 3627.25 6603.75 4.09 0.932 2.83 3 12 -3 967.18 177.17 4.06 0.153 0.88 -4 -6 0 1283.71 2542.87 4.05 0.579 1.40 -2 -6 6 210.55 24.33 4.02 0.057 1.32 -2 -8 -10 379.89 65.83 3.93 0.093 0.84 -2 -6 -1 882.53 395.95 3.92 0.228 1.67 4 -7 -9 725.67 263.59 3.91 0.186 0.98 4 6 0 1339.10 2542.87 3.87 0.579 1.40 -2 -8 3 136.68 1.87 3.85 0.016 1.28 -3 8 -4 240.82 32.09 3.80 0.065 1.19 -2 8 4 120.73 0.40 3.76 0.007 1.27 2 3 -13 214.13 0.10 3.74 0.004 0.87 -8 1 10 -46.01 214.93 3.71 0.168 0.88 2 8 9 230.31 24.90 3.67 0.057 0.89 3 0 1 3984.81 6603.75 3.67 0.932 2.83 3 12 0 41.21 363.33 3.67 0.219 0.89 -5 13 5 -68.18 251.66 3.66 0.182 0.79 -7 -2 5 -62.65 191.93 3.66 0.159 1.18 -3 0 -1 4043.70 6603.75 3.60 0.932 2.83 3 -6 4 163.49 15.58 3.60 0.045 1.41 -2 13 5 280.11 15.48 3.59 0.045 0.82 -4 8 -2 355.06 51.63 3.57 0.082 1.22 -8 6 -8 355.84 44.54 3.55 0.077 0.78 0 7 -13 381.64 51.01 3.55 0.082 0.78 1 7 -13 322.93 19.59 3.54 0.051 0.78 6 11 -4 271.75 22.90 3.50 0.055 0.81 -4 5 12 228.53 0.00 3.46 0.001 0.87 Bond lengths and angles C1 - Distance Angles C2 1.3911 (0.0075) C6 1.4230 (0.0075) 120.63 (0.47) P1 1.8008 (0.0051) 118.57 (0.41) 120.51 (0.40) C1 - C2 C6 C2 - Distance Angles C3 1.3861 (0.0075) C1 1.3911 (0.0075) 119.87 (0.55) H2 0.9500 120.06 120.06 C2 - C3 C1 C3 - Distance Angles C2 1.3861 (0.0075) C4 1.3901 (0.0085) 120.55 (0.58) H3 0.9500 119.72 119.72 C3 - C2 C4 C4 - Distance Angles C5 1.3772 (0.0084) C3 1.3901 (0.0085) 119.84 (0.53) H4 0.9500 120.08 120.08 C4 - C5 C3 C5 - Distance Angles C4 1.3772 (0.0084) C6 1.4070 (0.0071) 121.58 (0.54) H5 0.9500 119.21 119.21 C5 - C4 C6 C6 - Distance Angles C5 1.4070 (0.0071) C1 1.4230 (0.0075) 117.44 (0.51) C7 1.4908 (0.0078) 119.00 (0.49) 123.50 (0.45) C6 - C5 C1 C7 - Distance Angles C8 1.3684 (0.0096) C12 1.3882 (0.0090) 119.16 (0.61) C6 1.4908 (0.0078) 121.36 (0.59) 119.48 (0.60) C7 - C8 C12 C8 - Distance Angles C7 1.3684 (0.0097) C9 1.4085 (0.0087) 120.35 (0.67) H8 0.9500 119.83 119.83 C8 - C7 C9 C9 - Distance Angles C10 1.3783 (0.0100) C8 1.4085 (0.0087) 119.54 (0.68) H9 0.9500 120.23 120.23 C9 - C10 C8 C10 - Distance Angles C11 1.3683 (0.0109) C9 1.3783 (0.0100) 120.12 (0.65) H10 0.9500 119.94 119.94 C10 - C11 C9 C11 - Distance Angles C10 1.3683 (0.0109) C12 1.3843 (0.0093) 120.21 (0.70) H11 0.9500 119.90 119.90 C11 - C10 C12 C12 - Distance Angles C11 1.3843 (0.0093) C7 1.3882 (0.0090) 120.61 (0.70) H12 0.9500 119.70 119.70 C12 - C11 C7 C13 - Distance Angles C14 1.5253 (0.0080) C16 1.5398 (0.0081) 110.04 (0.53) C15 1.5467 (0.0080) 109.99 (0.46) 108.54 (0.49) P1 1.8443 (0.0060) 112.57 (0.39) 107.34 (0.38) 108.23 (0.42) C13 - C14 C16 C15 C14 - Distance Angles C13 1.5253 (0.0080) 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 1.5467 (0.0080) 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 C16 - Distance Angles C13 1.5398 (0.0081) H16A 0.9800 109.47 H16B 0.9800 109.47 109.47 H16C 0.9800 109.47 109.47 109.47 C16 - C13 H16A H16B C17 - Distance Angles C18 1.5148 (0.0083) C19 1.5377 (0.0081) 109.73 (0.51) C20 1.5406 (0.0089) 110.58 (0.51) 108.53 (0.53) P1 1.8560 (0.0063) 112.92 (0.44) 109.48 (0.40) 105.44 (0.42) C17 - C18 C19 C20 C18 - Distance Angles C17 1.5148 (0.0083) H18A 0.9800 109.47 H18B 0.9800 109.47 109.47 H18C 0.9800 109.47 109.47 109.47 C18 - C17 H18A H18B C19 - Distance Angles C17 1.5377 (0.0081) H19A 0.9800 109.47 H19B 0.9800 109.47 109.47 H19C 0.9800 109.47 109.47 109.47 C19 - C17 H19A H19B C20 - Distance Angles C17 1.5406 (0.0089) H20A 0.9800 109.47 H20B 0.9800 109.47 109.47 H20C 0.9800 109.47 109.47 109.47 C20 - C17 H20A H20B P1 - Distance Angles C1 1.8008 (0.0051) C13 1.8443 (0.0060) 110.91 (0.26) C17 1.8560 (0.0063) 111.00 (0.26) 117.91 (0.27) H1P 1.3272 (0.0472) 106.02 (2.00) 105.00 (2.10) 104.94 (2.31) P1 - C1 C13 C17 Cl1 - Distance Angles Fe1 2.2110 (0.0017) Cl1 - Cl2 - Distance Angles Fe1 2.1861 (0.0020) Cl2 - Cl3 - Distance Angles Fe1 2.2053 (0.0017) Cl3 - Cl4 - Distance Angles Fe1 2.1839 (0.0018) Cl4 - Fe1 - Distance Angles Cl4 2.1839 (0.0018) Cl2 2.1861 (0.0020) 108.93 (0.07) Cl3 2.2053 (0.0017) 108.40 (0.08) 110.81 (0.08) Cl1 2.2110 (0.0017) 110.05 (0.08) 109.57 (0.08) 109.06 (0.07) Fe1 - Cl4 Cl2 Cl3 FMAP and GRID set by program FMAP 2 1 23 GRID -2.500 -2 -2 2.500 2 2 R1 = 0.1642 for 4912 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.04 at 0.2013 0.6590 0.6809 [ 1.09 A from C12 ] Deepest hole -0.84 at 0.1756 0.6192 0.7272 [ 0.62 A from C12 ] Mean = 0.00, Rms deviation from mean = 0.21 e/A^3, Highest memory used = 3126 / 24827 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.2013 0.3410 0.3191 1.00000 0.05 1.04 1.09 C12 1.14 C7 1.51 C11 1.54 C8 Q2 1 0.6401 0.9194 0.2472 1.00000 0.05 0.94 1.22 CL2 1.67 FE1 2.67 CL3 2.81 H8 Q3 1 0.6718 0.6434 0.2580 1.00000 0.05 0.85 1.39 CL4 1.54 FE1 2.49 CL1 2.79 CL3 Q4 1 0.5735 0.7648 0.1993 1.00000 0.05 0.84 0.90 FE1 1.99 CL4 2.04 CL3 2.19 CL2 Q5 1 0.0263 -0.0966 0.3411 1.00000 0.05 0.82 1.08 H20C 1.50 C20 1.70 H20A 1.70 H20B Shortest distances between peaks (including symmetry equivalents) 3 4 1.81 2 4 1.88 Time profile in seconds ----------------------- 0.06: Read and process instructions 0.00: Fit rigid groups 0.01: 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. 0.86: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.01: Set up l.s. refinement 0.00: Generate idealized H-atoms 13.19: Structure factors and derivatives 16.05: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.36: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.36: Analysis of variance 0.10: Merge reflections for Fourier and .fcf 0.04: Fourier summations 0.00: Peaksearch 0.01: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2005src0348 finished at 15:33:56 Total CPU time: 29.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++