+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src0902r started at 21:58:59 on 08-Aug-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src0902r in P2(1)/c CELL 0.71073 7.3730 13.2476 30.3240 90.000 93.123 90.000 ZERR 8.00 0.0005 0.0010 0.0020 0.000 0.004 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N CL FE UNIT 144 88 16 8 8 V = 2957.48 F(000) = 1408.0 Mu = 1.20 mm-1 Cell Wt = 2772.70 Rho = 1.557 MERG 2 OMIT -3.00 55.00 SHEL 7 0.84 FMAP 2 PLAN 10 SIZE 0.01 0.14 0.27 ACTA BOND $H WGHT 0.02640 6.68580 L.S. 10 TEMP -153.00 FVAR 0.22855 MOLE 1 C1 1 0.148651 0.226327 0.609459 11.00000 0.01972 0.02132 = 0.01858 -0.00043 -0.00355 -0.00615 C2 1 0.105129 0.236493 0.562957 11.00000 0.02547 0.00889 = 0.03306 -0.00350 0.00086 -0.00515 AFIX 43 H2 2 0.023606 0.284292 0.549481 11.00000 -1.20000 AFIX 0 C3 1 0.205152 0.162676 0.540646 11.00000 0.02903 0.02236 = 0.02605 -0.00674 0.00952 -0.01307 AFIX 43 H3 2 0.204136 0.153523 0.509561 11.00000 -1.20000 AFIX 0 C4 1 0.306778 0.104949 0.572590 11.00000 0.01078 0.02767 = 0.05488 -0.01229 0.01043 -0.00621 AFIX 43 H4 2 0.384371 0.049934 0.566621 11.00000 -1.20000 AFIX 0 C5 1 0.272881 0.143325 0.615007 11.00000 0.01755 0.02154 = 0.03331 -0.00339 -0.00516 -0.00314 AFIX 43 H5 2 0.323600 0.118417 0.642352 11.00000 -1.20000 AFIX 0 C6 1 -0.236718 0.076724 0.578924 11.00000 0.01355 0.02711 = 0.05047 -0.00780 0.01053 -0.00990 AFIX 43 H6 2 -0.322990 0.129369 0.574066 11.00000 -1.20000 AFIX 0 C7 1 -0.155158 0.019801 0.545838 11.00000 0.02087 0.01691 = 0.02380 -0.00063 -0.00183 -0.00642 AFIX 43 H7 2 -0.177512 0.027212 0.514858 11.00000 -1.20000 AFIX 0 C8 1 -0.033116 -0.050865 0.567297 11.00000 0.02108 0.01560 = 0.03443 -0.00834 0.00174 -0.00662 AFIX 43 H8 2 0.039764 -0.098816 0.553111 11.00000 -1.20000 AFIX 0 C9 1 -0.040225 -0.036692 0.613250 11.00000 0.03766 0.02143 = 0.02486 0.00724 0.00081 -0.01331 AFIX 43 H9 2 0.028070 -0.073104 0.635450 11.00000 -1.20000 AFIX 0 C10 1 -0.166938 0.041316 0.620638 11.00000 0.03624 0.03916 = 0.02978 -0.01563 0.01938 -0.02325 AFIX 43 H10 2 -0.199378 0.065590 0.648616 11.00000 -1.20000 AFIX 0 C11 1 0.084264 0.287517 0.645904 11.00000 0.01380 0.02189 = 0.02322 -0.00139 -0.00315 0.00016 C12 1 0.063003 0.394040 0.643924 11.00000 0.01539 0.02176 = 0.02580 0.00015 -0.00094 -0.00123 C13 1 0.008128 0.449886 0.679186 11.00000 0.02113 0.01399 = 0.03000 -0.00460 -0.00535 0.00253 AFIX 43 H13 2 -0.006041 0.520975 0.676734 11.00000 -1.20000 AFIX 0 C14 1 -0.025970 0.401035 0.718135 11.00000 0.02105 0.02937 = 0.01872 -0.00897 0.00019 0.00228 C15 1 -0.003275 0.295336 0.721830 11.00000 0.03169 0.02291 = 0.02269 0.00184 -0.00526 -0.00752 C16 1 0.050233 0.241419 0.685922 11.00000 0.03081 0.01689 = 0.02256 -0.00357 -0.00507 0.00228 AFIX 43 H16 2 0.064417 0.170359 0.688537 11.00000 -1.20000 AFIX 0 C17 1 -0.087596 0.458661 0.755122 11.00000 0.02706 0.02317 = 0.02767 0.00139 -0.00920 -0.00817 C18 1 -0.036815 0.243989 0.762877 11.00000 0.03176 0.01962 = 0.03478 -0.00547 -0.00458 0.00075 N1 3 -0.140898 0.503954 0.784167 11.00000 0.04172 0.02976 = 0.03007 -0.01038 -0.00004 0.00187 N2 3 -0.062491 0.202925 0.795120 11.00000 0.05641 0.03627 = 0.03024 0.00301 0.00265 -0.00233 CL1 4 0.111972 0.461026 0.596482 11.00000 0.03168 0.02164 = 0.02993 0.00343 0.00140 -0.00054 FE1 5 0.038131 0.094593 0.583291 11.00000 0.01703 0.01943 = 0.02326 -0.00204 0.00176 -0.00289 MOLE 2 C101 1 0.639395 0.567329 0.601913 11.00000 0.01691 0.01567 = 0.02723 0.00004 -0.00223 0.00314 C102 1 0.754642 0.655098 0.606000 11.00000 0.01778 0.01822 = 0.02905 -0.00044 -0.00515 0.00153 AFIX 43 H102 2 0.793914 0.687428 0.632809 11.00000 -1.20000 AFIX 0 C103 1 0.798853 0.684538 0.563184 11.00000 0.01436 0.02643 = 0.04289 0.00743 0.00472 0.00210 AFIX 43 H103 2 0.874765 0.739757 0.556452 11.00000 -1.20000 AFIX 0 C104 1 0.711921 0.618566 0.531724 11.00000 0.02799 0.03371 = 0.02576 0.00468 0.01188 0.00613 AFIX 43 H104 2 0.718775 0.621688 0.500561 11.00000 -1.20000 AFIX 0 C105 1 0.612428 0.546774 0.555782 11.00000 0.02205 0.02546 = 0.03210 0.00126 0.00298 0.00164 AFIX 43 H105 2 0.539893 0.493807 0.543162 11.00000 -1.20000 AFIX 0 C106 1 0.279797 0.724528 0.592833 11.00000 0.02158 0.03433 = 0.03729 0.01573 0.01355 0.00795 AFIX 43 H106 2 0.223782 0.690288 0.616024 11.00000 -1.20000 AFIX 0 C107 1 0.398961 0.808350 0.597831 11.00000 0.02744 0.02160 = 0.03851 -0.00860 -0.00301 0.01434 AFIX 43 H107 2 0.436244 0.840736 0.624770 11.00000 -1.20000 AFIX 0 C108 1 0.452231 0.834848 0.554860 11.00000 0.02633 0.02260 = 0.04933 0.00677 0.01125 0.00581 AFIX 43 H108 2 0.533078 0.887767 0.548074 11.00000 -1.20000 AFIX 0 C109 1 0.363703 0.768592 0.524072 11.00000 0.03858 0.04303 = 0.03251 0.01218 0.00662 0.01591 AFIX 43 H109 2 0.373324 0.769639 0.492962 11.00000 -1.20000 AFIX 0 C110 1 0.258972 0.700945 0.547754 11.00000 0.01598 0.03776 = 0.04366 -0.00422 -0.00892 0.00393 AFIX 43 H110 2 0.186071 0.647964 0.535278 11.00000 -1.20000 AFIX 0 C111 1 0.572222 0.512878 0.639799 11.00000 0.01429 0.02404 = 0.02305 0.00017 -0.00286 -0.00065 C112 1 0.562014 0.408305 0.642620 11.00000 0.01391 0.01981 = 0.02203 -0.00024 -0.00300 -0.00104 C113 1 0.515122 0.359038 0.680439 11.00000 0.02192 0.01926 = 0.02428 0.00663 -0.00718 -0.00102 AFIX 43 H113 2 0.511347 0.287365 0.680841 11.00000 -1.20000 AFIX 0 C114 1 0.473755 0.412098 0.717570 11.00000 0.01866 0.02465 = 0.02115 0.00019 -0.00130 -0.00184 C115 1 0.478450 0.519257 0.715737 11.00000 0.02211 0.02380 = 0.02001 -0.00211 -0.00281 0.00496 C116 1 0.527267 0.567074 0.677487 11.00000 0.02273 0.01675 = 0.02572 0.00013 -0.00514 -0.00244 AFIX 43 H116 2 0.530412 0.638741 0.676741 11.00000 -1.20000 AFIX 0 C117 1 0.430690 0.361728 0.757563 11.00000 0.02615 0.02055 = 0.03250 -0.00036 -0.00209 -0.00261 C118 1 0.434756 0.577761 0.754269 11.00000 0.02976 0.02707 = 0.02235 0.00448 -0.00031 -0.00275 N101 3 0.396958 0.318455 0.789191 11.00000 0.04518 0.03236 = 0.03384 0.00924 0.00107 -0.00685 N102 3 0.401618 0.621859 0.785040 11.00000 0.05125 0.03535 = 0.02970 -0.00124 0.00717 -0.00186 CL11 4 0.621591 0.332135 0.598784 11.00000 0.03456 0.01980 = 0.03355 -0.00588 0.00510 -0.00051 FE11 5 0.525310 0.689515 0.568423 11.00000 0.01717 0.02032 = 0.02461 0.00239 0.00114 0.00105 HKLF 4 Covalent radii and connectivity table for 2007src0902r in P2(1)/c C 0.770 H 0.320 N 0.700 CL 0.990 FE 1.240 C1 - C5 C2 C11 Fe1 C2 - C3 C1 Fe1 C3 - C4 C2 Fe1 C4 - C3 C5 Fe1 C5 - C4 C1 Fe1 C6 - C7 C10 Fe1 C7 - C6 C8 Fe1 C8 - C9 C7 Fe1 C9 - C8 C10 Fe1 C10 - C9 C6 Fe1 C11 - C16 C12 C1 C12 - C13 C11 Cl1 C13 - C12 C14 C14 - C13 C15 C17 C15 - C16 C14 C18 C16 - C15 C11 C17 - N1 C14 C18 - N2 C15 N1 - C17 N2 - C18 Cl1 - C12 Fe1 - C4 C7 C6 C5 C3 C2 C8 C9 C10 C1 C101 - C105 C102 C111 Fe11 C102 - C103 C101 Fe11 C103 - C102 C104 Fe11 C104 - C103 C105 Fe11 C105 - C104 C101 Fe11 C106 - C110 C107 Fe11 C107 - C106 C108 Fe11 C108 - C109 C107 Fe11 C109 - C110 C108 Fe11 C110 - C106 C109 Fe11 C111 - C112 C116 C101 C112 - C113 C111 Cl11 C113 - C114 C112 C114 - C113 C115 C117 C115 - C116 C114 C118 C116 - C115 C111 C117 - N101 C114 C118 - N102 C115 N101 - C117 N102 - C118 Cl11 - C112 Fe11 - C103 C110 C108 C109 C102 C105 C104 C106 C107 C101 h k l Fo^2 Sigma Why rejected -4 0 3 19.87 4.80 observed but should be systematically absent -4 0 5 12.37 2.89 observed but should be systematically absent 28108 Reflections read, of which 4778 rejected -8 =< h =< 8, -15 =< k =< 15, -36 =< l =< 35, Max. 2-theta = 50.05 2 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 6 3 0 80.56 4.18 3 22.40 -6 2 1 105.48 5.20 2 33.71 5 2 25 181.01 16.31 4 106.79 3 Inconsistent equivalents 5192 Unique reflections, of which 0 suppressed R(int) = 0.0925 R(sigma) = 0.1035 Friedel opposites merged Maximum memory for data reduction = 3679 / 51337 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 = 4736 / 509548 wR2 = 0.1248 before cycle 1 for 5192 data and 397 / 397 parameters GooF = S = 1.066; Restrained GooF = 1.066 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0264 * P )^2 + 6.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22841 0.00038 -0.372 OSF Mean shift/esd = 0.155 Maximum = -0.747 for U12 Fe11 Max. shift = 0.003 A for C117 Max. dU =-0.001 for C10 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4736 / 509548 wR2 = 0.1245 before cycle 2 for 5192 data and 397 / 397 parameters GooF = S = 1.063; Restrained GooF = 1.063 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0264 * P )^2 + 6.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22839 0.00038 -0.052 OSF Mean shift/esd = 0.057 Maximum = 0.282 for U12 C5 Max. shift = 0.001 A for C109 Max. dU = 0.000 for C6 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4736 / 509548 wR2 = 0.1245 before cycle 3 for 5192 data and 397 / 397 parameters GooF = S = 1.063; Restrained GooF = 1.063 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0264 * P )^2 + 6.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22839 0.00038 -0.010 OSF Mean shift/esd = 0.005 Maximum = -0.050 for U22 C1 Max. shift = 0.000 A for C114 Max. dU = 0.000 for C1 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4736 / 509548 wR2 = 0.1245 before cycle 4 for 5192 data and 397 / 397 parameters GooF = S = 1.063; Restrained GooF = 1.063 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0264 * P )^2 + 6.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22839 0.00038 -0.001 OSF Mean shift/esd = 0.001 Maximum = -0.007 for U22 C101 Max. shift = 0.000 A for C105 Max. dU = 0.000 for C111 Least-squares cycle 5 Maximum vector length = 511 Memory required = 4736 / 509548 wR2 = 0.1245 before cycle 5 for 5192 data and 397 / 397 parameters GooF = S = 1.063; Restrained GooF = 1.063 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0264 * P )^2 + 6.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22839 0.00038 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for U12 C1 Max. shift = 0.000 A for C1 Max. dU = 0.000 for C6 Least-squares cycle 6 Maximum vector length = 511 Memory required = 4736 / 509548 wR2 = 0.1245 before cycle 6 for 5192 data and 397 / 397 parameters GooF = S = 1.063; Restrained GooF = 1.063 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0264 * P )^2 + 6.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22839 0.00038 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z Fe1 Max. shift = 0.000 A for H108 Max. dU = 0.000 for C102 Least-squares cycle 7 Maximum vector length = 511 Memory required = 4736 / 509548 wR2 = 0.1245 before cycle 7 for 5192 data and 397 / 397 parameters GooF = S = 1.063; Restrained GooF = 1.063 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0264 * P )^2 + 6.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22839 0.00038 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z Fe1 Max. shift = 0.000 A for C11 Max. dU = 0.000 for C102 Least-squares cycle 8 Maximum vector length = 511 Memory required = 4736 / 509548 wR2 = 0.1245 before cycle 8 for 5192 data and 397 / 397 parameters GooF = S = 1.063; Restrained GooF = 1.063 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0264 * P )^2 + 6.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22839 0.00038 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z Fe1 Max. shift = 0.000 A for C4 Max. dU = 0.000 for N1 Least-squares cycle 9 Maximum vector length = 511 Memory required = 4736 / 509548 wR2 = 0.1245 before cycle 9 for 5192 data and 397 / 397 parameters GooF = S = 1.063; Restrained GooF = 1.063 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0264 * P )^2 + 6.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22839 0.00038 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z Fe1 Max. shift = 0.000 A for C115 Max. dU = 0.000 for C107 Least-squares cycle 10 Maximum vector length = 511 Memory required = 4736 / 509548 wR2 = 0.1245 before cycle 10 for 5192 data and 397 / 397 parameters GooF = S = 1.063; Restrained GooF = 1.063 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0264 * P )^2 + 6.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22839 0.00038 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z Fe1 Max. shift = 0.000 A for C4 Max. dU = 0.000 for C105 No correlation matrix elements larger than 0.500 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 C2 ** H2 0.0234 0.2840 0.5495 43 0.950 0.000 C2 C3 C1 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C3 ** H3 0.2044 0.1538 0.5096 43 0.950 0.000 C3 C4 C2 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C4 ** H4 0.3847 0.0502 0.5666 43 0.950 0.000 C4 C3 C5 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C5 ** H5 0.3236 0.1183 0.6423 43 0.950 0.000 C5 C4 C1 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C6 ** H6 -0.3229 0.1295 0.5741 43 0.950 0.000 C6 C7 C10 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C7 ** H7 -0.1780 0.0270 0.5149 43 0.950 0.000 C7 C6 C8 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C8 ** H8 0.0394 -0.0989 0.5531 43 0.950 0.000 C8 C9 C7 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C9 ** H9 0.0284 -0.0729 0.6355 43 0.950 0.000 C9 C8 C10 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C10 ** H10 -0.1999 0.0656 0.6486 43 0.950 0.000 C10 C9 C6 H13 -0.0058 0.5209 0.6767 43 0.950 0.000 C13 C12 C14 H16 0.0636 0.1704 0.6885 43 0.950 0.000 C16 C15 C11 ** Bond(s) to Fe11 ignored in idealizing H-atoms attached to C102 ** H102 0.7936 0.6878 0.6327 43 0.950 0.000 C102 C103 C101 ** Bond(s) to Fe11 ignored in idealizing H-atoms attached to C103 ** H103 0.8749 0.7395 0.5564 43 0.950 0.000 C103 C102 C104 ** Bond(s) to Fe11 ignored in idealizing H-atoms attached to C104 ** H104 0.7189 0.6216 0.5006 43 0.950 0.000 C104 C103 C105 ** Bond(s) to Fe11 ignored in idealizing H-atoms attached to C105 ** H105 0.5401 0.4940 0.5432 43 0.950 0.000 C105 C104 C101 ** Bond(s) to Fe11 ignored in idealizing H-atoms attached to C106 ** H106 0.2238 0.6903 0.6160 43 0.950 0.000 C106 C110 C107 ** Bond(s) to Fe11 ignored in idealizing H-atoms attached to C107 ** H107 0.4369 0.8406 0.6248 43 0.950 0.000 C107 C106 C108 ** Bond(s) to Fe11 ignored in idealizing H-atoms attached to C108 ** H108 0.5327 0.8879 0.5481 43 0.950 0.000 C108 C109 C107 ** Bond(s) to Fe11 ignored in idealizing H-atoms attached to C109 ** H109 0.3733 0.7700 0.4930 43 0.950 0.000 C109 C110 C108 ** Bond(s) to Fe11 ignored in idealizing H-atoms attached to C110 ** H110 0.1862 0.6479 0.5353 43 0.950 0.000 C110 C106 C109 H113 0.5113 0.2875 0.6809 43 0.950 0.000 C113 C114 C112 H116 0.5304 0.6385 0.6768 43 0.950 0.000 C116 C115 C111 2007src0902r in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.14877 0.22657 0.60944 1.00000 0.01966 0.02120 0.01857 -0.00049 -0.00355 -0.00847 0.01998 0.00827 0.00063 0.00037 0.00016 0.00000 0.00275 0.00287 0.00310 0.00229 0.00220 0.00233 0.00119 C2 0.10528 0.23637 0.56295 1.00000 0.02545 0.00969 0.03281 -0.00339 0.00149 -0.00459 0.02265 0.00840 0.00066 0.00036 0.00017 0.00000 0.00290 0.00263 0.00347 0.00241 0.00246 0.00234 0.00124 H2 0.02344 0.28398 0.54946 1.00000 0.02718 0.00000 0.00000 C3 0.20533 0.16287 0.54065 1.00000 0.02875 0.02068 0.02649 -0.00640 0.00882 -0.01246 0.02504 0.00876 0.00066 0.00037 0.00018 0.00000 0.00304 0.00305 0.00325 0.00249 0.00248 0.00256 0.00128 H3 0.20441 0.15382 0.50956 1.00000 0.03005 0.00000 0.00000 C4 0.30698 0.10513 0.57256 1.00000 0.01054 0.02726 0.05595 -0.01319 0.01110 -0.00785 0.03091 0.00905 0.00064 0.00041 0.00020 0.00000 0.00275 0.00328 0.00429 0.00306 0.00260 0.00248 0.00143 H4 0.38467 0.05017 0.56657 1.00000 0.03709 0.00000 0.00000 C5 0.27302 0.14334 0.61496 1.00000 0.01773 0.02118 0.03335 -0.00249 -0.00530 -0.00066 0.02433 0.00872 0.00064 0.00038 0.00018 0.00000 0.00275 0.00297 0.00354 0.00261 0.00237 0.00240 0.00126 H5 0.32358 0.11830 0.64230 1.00000 0.02920 0.00000 0.00000 C6 -0.23683 0.07679 0.57894 1.00000 0.01265 0.02451 0.05150 -0.00723 0.00991 -0.00925 0.02925 0.00912 0.00066 0.00041 0.00019 0.00000 0.00268 0.00315 0.00419 0.00291 0.00261 0.00243 0.00140 H6 -0.32288 0.12954 0.57407 1.00000 0.03510 0.00000 0.00000 C7 -0.15545 0.01968 0.54585 1.00000 0.02048 0.01607 0.02424 0.00004 -0.00201 -0.00477 0.02038 0.00838 0.00062 0.00036 0.00017 0.00000 0.00268 0.00278 0.00316 0.00237 0.00224 0.00232 0.00119 H7 -0.17800 0.02700 0.51487 1.00000 0.02446 0.00000 0.00000 C8 -0.03338 -0.05092 0.56728 1.00000 0.02144 0.01648 0.03418 -0.00926 0.00218 -0.00772 0.02401 0.00835 0.00066 0.00037 0.00018 0.00000 0.00281 0.00284 0.00353 0.00253 0.00241 0.00238 0.00126 H8 0.03936 -0.09892 0.55308 1.00000 0.02881 0.00000 0.00000 C9 -0.04016 -0.03663 0.61330 1.00000 0.03802 0.02203 0.02456 0.00703 0.00048 -0.01506 0.02825 0.00897 0.00072 0.00039 0.00018 0.00000 0.00333 0.00311 0.00341 0.00253 0.00255 0.00274 0.00135 H9 0.02839 -0.07288 0.63550 1.00000 0.03390 0.00000 0.00000 C10 -0.16724 0.04136 0.62063 1.00000 0.03461 0.03746 0.03052 -0.01554 0.01891 -0.02315 0.03357 0.00928 0.00072 0.00043 0.00019 0.00000 0.00341 0.00366 0.00377 0.00292 0.00274 0.00293 0.00152 H10 -0.19994 0.06557 0.64860 1.00000 0.04029 0.00000 0.00000 C11 0.08446 0.28756 0.64589 1.00000 0.01411 0.02376 0.02206 -0.00145 -0.00264 0.00052 0.02011 0.00840 0.00062 0.00037 0.00017 0.00000 0.00261 0.00303 0.00314 0.00242 0.00215 0.00227 0.00119 C12 0.06296 0.39424 0.64390 1.00000 0.01526 0.02218 0.02547 0.00036 -0.00074 -0.00071 0.02104 0.00855 0.00061 0.00038 0.00016 0.00000 0.00260 0.00301 0.00317 0.00246 0.00218 0.00233 0.00120 C13 0.00825 0.44982 0.67915 1.00000 0.02164 0.01524 0.02911 -0.00438 -0.00458 0.00242 0.02221 0.00837 0.00061 0.00038 0.00017 0.00000 0.00286 0.00274 0.00337 0.00248 0.00235 0.00231 0.00123 H13 -0.00583 0.52092 0.67671 1.00000 0.02666 0.00000 0.00000 C14 -0.02597 0.40113 0.71811 1.00000 0.02073 0.02869 0.01926 -0.00979 -0.00006 0.00031 0.02294 0.00846 0.00064 0.00040 0.00017 0.00000 0.00280 0.00321 0.00310 0.00257 0.00223 0.00249 0.00123 C15 -0.00289 0.29535 0.72185 1.00000 0.03139 0.02234 0.02263 0.00122 -0.00527 -0.00833 0.02570 0.00873 0.00069 0.00039 0.00017 0.00000 0.00315 0.00314 0.00331 0.00256 0.00242 0.00255 0.00129 C16 0.05006 0.24153 0.68590 1.00000 0.03008 0.01666 0.02274 -0.00446 -0.00546 0.00061 0.02341 0.00854 0.00066 0.00039 0.00017 0.00000 0.00301 0.00283 0.00331 0.00247 0.00243 0.00243 0.00124 H16 0.06364 0.17043 0.68846 1.00000 0.02809 0.00000 0.00000 C17 -0.08735 0.45858 0.75509 1.00000 0.02840 0.02436 0.02638 0.00100 -0.00825 -0.00762 0.02674 0.00906 0.00070 0.00041 0.00018 0.00000 0.00314 0.00324 0.00354 0.00276 0.00256 0.00262 0.00131 C18 -0.03688 0.24386 0.76284 1.00000 0.03271 0.02145 0.03351 -0.00554 -0.00361 0.00067 0.02942 0.00954 0.00073 0.00041 0.00020 0.00000 0.00333 0.00322 0.00394 0.00289 0.00276 0.00265 0.00136 N1 -0.14087 0.50380 0.78412 1.00000 0.04049 0.02859 0.03059 -0.00934 -0.00065 0.00190 0.03332 0.00799 0.00061 0.00035 0.00016 0.00000 0.00289 0.00287 0.00310 0.00237 0.00229 0.00239 0.00118 N2 -0.06243 0.20298 0.79510 1.00000 0.05542 0.03525 0.03038 0.00213 0.00237 -0.00242 0.04035 0.00868 0.00067 0.00037 0.00017 0.00000 0.00342 0.00315 0.00325 0.00259 0.00252 0.00261 0.00129 Cl1 0.11190 0.46105 0.59648 1.00000 0.03178 0.02163 0.02982 0.00341 0.00153 -0.00036 0.02775 0.00232 0.00017 0.00009 0.00004 0.00000 0.00076 0.00072 0.00083 0.00061 0.00060 0.00060 0.00033 Fe1 0.03810 0.09460 0.58329 1.00000 0.01706 0.01945 0.02313 -0.00198 0.00178 -0.00264 0.01986 0.00122 0.00009 0.00005 0.00002 0.00000 0.00039 0.00042 0.00045 0.00034 0.00030 0.00033 0.00021 C101 0.63954 0.56719 0.60189 1.00000 0.01737 0.01602 0.02652 0.00022 -0.00229 0.00394 0.02010 0.00859 0.00062 0.00036 0.00017 0.00000 0.00270 0.00275 0.00329 0.00237 0.00226 0.00225 0.00119 C102 0.75461 0.65524 0.60596 1.00000 0.01745 0.01673 0.02923 -0.00119 -0.00533 0.00037 0.02138 0.00874 0.00062 0.00036 0.00017 0.00000 0.00271 0.00285 0.00339 0.00238 0.00228 0.00229 0.00122 H102 0.79359 0.68777 0.63274 1.00000 0.02565 0.00000 0.00000 C103 0.79886 0.68439 0.56315 1.00000 0.01451 0.02574 0.04272 0.00739 0.00463 0.00216 0.02754 0.00970 0.00064 0.00041 0.00018 0.00000 0.00281 0.00317 0.00383 0.00289 0.00243 0.00247 0.00132 H103 0.87495 0.73952 0.55641 1.00000 0.03305 0.00000 0.00000 C104 0.71206 0.61855 0.53172 1.00000 0.02764 0.03253 0.02610 0.00519 0.01202 0.00696 0.02837 0.00997 0.00067 0.00040 0.00018 0.00000 0.00309 0.00341 0.00337 0.00269 0.00251 0.00268 0.00135 H104 0.71889 0.62165 0.50055 1.00000 0.03405 0.00000 0.00000 C105 0.61270 0.54691 0.55580 1.00000 0.02288 0.02721 0.03145 0.00150 0.00361 0.00163 0.02710 0.00965 0.00067 0.00040 0.00017 0.00000 0.00294 0.00321 0.00362 0.00264 0.00247 0.00251 0.00133 H105 0.54006 0.49401 0.54317 1.00000 0.03252 0.00000 0.00000 C106 0.27986 0.72450 0.59284 1.00000 0.02144 0.03414 0.03768 0.01669 0.01386 0.01032 0.03064 0.01070 0.00069 0.00042 0.00019 0.00000 0.00294 0.00350 0.00393 0.00286 0.00257 0.00266 0.00143 H106 0.22379 0.69030 0.61603 1.00000 0.03676 0.00000 0.00000 C107 0.39929 0.80835 0.59784 1.00000 0.02685 0.02159 0.03865 -0.00959 -0.00325 0.01186 0.02921 0.00965 0.00068 0.00039 0.00019 0.00000 0.00305 0.00308 0.00372 0.00279 0.00257 0.00267 0.00135 H107 0.43689 0.84063 0.62478 1.00000 0.03505 0.00000 0.00000 C108 0.45209 0.83493 0.55485 1.00000 0.02548 0.02164 0.04971 0.00673 0.01125 0.00678 0.03194 0.01053 0.00071 0.00040 0.00020 0.00000 0.00309 0.00321 0.00421 0.00291 0.00281 0.00261 0.00143 H108 0.53275 0.88794 0.54806 1.00000 0.03833 0.00000 0.00000 C109 0.36376 0.76885 0.52406 1.00000 0.03818 0.04358 0.03239 0.01227 0.00684 0.01590 0.03787 0.01151 0.00076 0.00045 0.00020 0.00000 0.00354 0.00389 0.00383 0.00315 0.00291 0.00316 0.00155 H109 0.37335 0.77003 0.49295 1.00000 0.04545 0.00000 0.00000 C110 0.25897 0.70091 0.54774 1.00000 0.01623 0.03902 0.04324 -0.00378 -0.00875 0.00586 0.03320 0.01002 0.00068 0.00043 0.00020 0.00000 0.00282 0.00369 0.00407 0.00310 0.00256 0.00270 0.00145 H110 0.18620 0.64789 0.53525 1.00000 0.03985 0.00000 0.00000 C111 0.57218 0.51308 0.63981 1.00000 0.01450 0.02486 0.02225 -0.00003 -0.00253 -0.00028 0.02067 0.00847 0.00061 0.00039 0.00017 0.00000 0.00255 0.00306 0.00314 0.00246 0.00212 0.00236 0.00119 C112 0.56191 0.40814 0.64261 1.00000 0.01482 0.02099 0.02124 -0.00026 -0.00262 -0.00126 0.01915 0.00826 0.00060 0.00037 0.00016 0.00000 0.00254 0.00293 0.00303 0.00240 0.00210 0.00230 0.00115 C113 0.51508 0.35920 0.68045 1.00000 0.02122 0.01858 0.02452 0.00656 -0.00757 -0.00170 0.02176 0.00859 0.00062 0.00039 0.00016 0.00000 0.00279 0.00280 0.00327 0.00251 0.00229 0.00235 0.00121 H113 0.51128 0.28753 0.68087 1.00000 0.02611 0.00000 0.00000 C114 0.47374 0.41211 0.71761 1.00000 0.01951 0.02594 0.02057 0.00029 -0.00063 -0.00128 0.02207 0.00874 0.00063 0.00039 0.00017 0.00000 0.00275 0.00309 0.00311 0.00255 0.00223 0.00246 0.00120 C115 0.47829 0.51938 0.71575 1.00000 0.02201 0.02352 0.02007 -0.00243 -0.00266 0.00363 0.02200 0.00863 0.00064 0.00039 0.00017 0.00000 0.00279 0.00300 0.00316 0.00246 0.00224 0.00242 0.00121 C116 0.52721 0.56687 0.67751 1.00000 0.02288 0.01700 0.02563 0.00036 -0.00503 -0.00160 0.02207 0.00843 0.00062 0.00038 0.00017 0.00000 0.00282 0.00282 0.00325 0.00242 0.00233 0.00234 0.00122 H116 0.53043 0.63854 0.67679 1.00000 0.02648 0.00000 0.00000 C117 0.43021 0.36181 0.75754 1.00000 0.02565 0.02013 0.03227 -0.00124 -0.00213 -0.00490 0.02616 0.00905 0.00068 0.00040 0.00019 0.00000 0.00306 0.00308 0.00370 0.00278 0.00256 0.00251 0.00130 C118 0.43499 0.57768 0.75433 1.00000 0.02988 0.02820 0.02195 0.00558 -0.00011 -0.00116 0.02673 0.00978 0.00069 0.00042 0.00019 0.00000 0.00319 0.00335 0.00342 0.00274 0.00254 0.00268 0.00131 N101 0.39692 0.31859 0.78919 1.00000 0.04502 0.03150 0.03439 0.00969 0.00125 -0.00490 0.03700 0.00836 0.00063 0.00036 0.00016 0.00000 0.00310 0.00296 0.00321 0.00255 0.00240 0.00247 0.00123 N102 0.40140 0.62186 0.78502 1.00000 0.05156 0.03584 0.02930 -0.00117 0.00757 -0.00225 0.03871 0.00875 0.00065 0.00037 0.00016 0.00000 0.00333 0.00316 0.00318 0.00251 0.00252 0.00255 0.00128 Cl11 0.62153 0.33211 0.59878 1.00000 0.03470 0.02000 0.03341 -0.00589 0.00528 -0.00055 0.02924 0.00230 0.00017 0.00010 0.00005 0.00000 0.00079 0.00072 0.00085 0.00061 0.00062 0.00062 0.00034 Fe11 0.52530 0.68954 0.56842 1.00000 0.01706 0.02029 0.02459 0.00232 0.00109 0.00071 0.02065 0.00127 0.00009 0.00005 0.00002 0.00000 0.00039 0.00043 0.00045 0.00035 0.00031 0.00033 0.00021 Final Structure Factor Calculation for 2007src0902r in P2(1)/c Total number of l.s. parameters = 397 Maximum vector length = 511 Memory required = 4339 / 24017 wR2 = 0.1245 before cycle 11 for 5192 data and 0 / 397 parameters GooF = S = 1.063; Restrained GooF = 1.063 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0264 * P )^2 + 6.69 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0617 for 3460 Fo > 4sig(Fo) and 0.1121 for all 5192 data wR2 = 0.1245, GooF = S = 1.063, Restrained GooF = 1.063 for all data Occupancy sum of asymmetric unit = 44.00 for non-hydrogen and 22.00 for hydrogen atoms Principal mean square atomic displacements U 0.0299 0.0196 0.0105 C1 0.0333 0.0266 0.0081 C2 0.0428 0.0207 0.0116 C3 0.0630 0.0230 0.0067 C4 0.0365 0.0212 0.0153 C5 0.0553 0.0255 0.0070 C6 0.0270 0.0213 0.0128 C7 0.0388 0.0243 0.0090 C8 0.0484 0.0260 0.0104 C9 0.0708 0.0181 0.0118 C10 0.0253 0.0221 0.0129 C11 0.0260 0.0222 0.0150 C12 0.0341 0.0186 0.0139 C13 0.0350 0.0208 0.0131 C14 0.0393 0.0214 0.0164 C15 0.0351 0.0212 0.0139 C16 0.0405 0.0242 0.0155 C17 0.0401 0.0290 0.0192 C18 0.0433 0.0364 0.0202 N1 0.0557 0.0358 0.0295 N2 0.0319 0.0310 0.0204 Cl1 0.0243 0.0199 0.0153 Fe1 0.0280 0.0199 0.0124 C101 0.0327 0.0166 0.0148 C102 0.0457 0.0230 0.0138 C103 0.0434 0.0261 0.0156 C104 0.0325 0.0269 0.0220 C105 0.0586 0.0193 0.0140 C106 0.0484 0.0282 0.0110 C107 0.0545 0.0249 0.0165 C108 0.0617 0.0296 0.0223 C109 0.0503 0.0368 0.0125 C110 0.0249 0.0238 0.0133 C111 0.0231 0.0211 0.0132 C112 0.0348 0.0180 0.0125 C113 0.0263 0.0217 0.0182 C114 0.0289 0.0198 0.0173 C115 0.0312 0.0186 0.0163 C116 0.0342 0.0274 0.0168 C117 0.0328 0.0287 0.0187 C118 0.0485 0.0400 0.0225 N101 0.0529 0.0355 0.0277 N102 0.0384 0.0316 0.0177 Cl11 0.0256 0.0194 0.0169 Fe11 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.010 0.019 0.029 0.040 0.052 0.065 0.081 0.102 0.139 1.000 Number in group 567. 496. 519. 514. 532. 496. 519. 511. 524. 514. GooF 1.044 0.975 1.009 1.048 1.010 0.990 1.136 1.156 1.023 1.212 K 8.094 2.012 1.344 1.117 1.058 0.988 1.017 1.042 0.998 1.004 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.06 1.14 1.26 1.44 1.81 inf Number in group 520. 531. 522. 509. 516. 528. 515. 516. 518. 517. GooF 1.072 0.994 1.049 1.019 1.037 1.026 1.104 0.958 1.057 1.282 K 1.047 1.169 1.124 1.023 1.019 0.995 0.997 1.003 1.010 1.000 R1 0.250 0.225 0.198 0.154 0.126 0.121 0.086 0.059 0.043 0.032 Recommended weighting scheme: WGHT 0.0416 6.0890 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) -1 1 1 12957.55 33631.14 14.71 0.416 6.36 5 12 8 42.50 1438.01 10.27 0.086 0.85 -2 8 15 77.89 1044.32 8.99 0.073 1.22 1 1 0 1558.43 3430.56 7.73 0.133 6.44 -3 6 15 562.39 1505.28 4.52 0.088 1.30 4 7 10 3713.21 4919.47 3.95 0.159 1.19 -8 0 12 923.20 5.05 3.44 0.005 0.88 1 11 0 445.87 88.66 3.44 0.021 1.19 5 12 4 1160.06 2496.96 3.38 0.113 0.87 -8 1 3 1367.52 202.62 3.34 0.032 0.92 -6 5 3 362.91 1106.63 3.27 0.075 1.11 -3 11 15 3275.36 4965.82 3.26 0.160 0.96 0 10 8 2328.65 3086.08 3.21 0.126 1.25 2 0 10 78.22 295.43 3.18 0.039 2.28 4 3 10 513.23 882.09 3.15 0.067 1.45 -7 4 4 2415.91 5883.47 3.15 0.174 1.00 1 14 2 775.80 234.02 3.11 0.035 0.94 0 0 12 1688.90 2219.19 3.10 0.107 2.52 4 9 15 597.59 1141.12 3.03 0.077 0.98 -7 1 4 286.10 883.94 2.95 0.067 1.05 -1 8 1 166.33 17.78 2.95 0.010 1.61 -5 9 11 960.82 18.68 2.91 0.010 0.99 0 13 1 3516.10 2767.42 2.91 0.119 1.02 1 13 6 495.17 907.92 2.88 0.068 0.99 3 5 1 426.45 253.84 2.86 0.036 1.79 -3 11 8 811.28 1205.41 2.82 0.079 1.05 0 12 17 2138.08 3863.91 2.82 0.141 0.94 -2 15 3 1158.09 167.85 2.80 0.029 0.86 1 2 14 2378.96 1897.43 2.77 0.099 1.95 3 2 2 4846.80 4192.05 2.76 0.147 2.26 -3 9 24 15068.33 1527.68 2.76 0.089 0.91 3 10 9 2205.32 2964.09 2.76 0.124 1.09 -2 1 27 268.69 5.07 2.75 0.005 1.09 1 12 4 912.32 1315.94 2.74 0.082 1.08 0 2 1 370.71 233.08 2.74 0.035 6.47 7 4 0 499.32 77.06 2.73 0.020 1.00 4 5 22 318.75 0.38 2.71 0.001 1.00 -3 4 17 356.27 153.56 2.70 0.028 1.35 -3 7 2 151.04 11.48 2.68 0.008 1.50 -1 14 4 347.00 9.23 2.66 0.007 0.93 3 7 0 174.18 5.49 2.65 0.005 1.50 7 4 2 1605.78 2692.95 2.64 0.118 1.00 -4 2 4 270.56 106.46 2.64 0.023 1.75 7 5 13 2216.98 1529.06 2.63 0.089 0.89 3 1 29 424.14 45.56 2.63 0.015 0.94 0 7 21 -98.70 136.42 2.60 0.026 1.15 6 10 6 173.52 409.39 2.59 0.046 0.88 3 4 2 2397.68 1997.24 2.57 0.101 1.94 -5 7 1 1514.48 1025.62 2.57 0.073 1.16 -3 4 7 2236.57 1872.52 2.56 0.098 1.82 Bond lengths and angles C1 - Distance Angles C5 1.4374 (0.0068) C2 1.4345 (0.0067) 106.91 (0.44) C11 1.4684 (0.0067) 124.35 (0.45) 128.74 (0.45) Fe1 2.0690 (0.0048) 68.41 (0.28) 68.74 (0.26) 128.08 (0.33) C1 - C5 C2 C11 C2 - Distance Angles C3 1.4156 (0.0068) C1 1.4345 (0.0067) 108.23 (0.46) Fe1 2.0460 (0.0048) 69.73 (0.28) 70.46 (0.28) H2 0.9500 125.89 125.89 125.51 C2 - C3 C1 Fe1 C3 - Distance Angles C4 1.4156 (0.0074) C2 1.4156 (0.0068) 108.39 (0.48) Fe1 2.0453 (0.0050) 69.15 (0.29) 69.78 (0.28) H3 0.9500 125.81 125.81 126.84 C3 - C4 C2 Fe1 C4 - Distance Angles C3 1.4156 (0.0074) C5 1.4169 (0.0070) 108.30 (0.47) Fe1 2.0312 (0.0047) 70.22 (0.28) 69.93 (0.28) H4 0.9500 125.85 125.85 125.59 C4 - C3 C5 Fe1 C5 - Distance Angles C4 1.4169 (0.0070) C1 1.4374 (0.0068) 108.14 (0.47) Fe1 2.0392 (0.0048) 69.33 (0.28) 70.63 (0.27) H5 0.9500 125.93 125.93 125.69 C5 - C4 C1 Fe1 C6 - Distance Angles C7 1.4158 (0.0068) C10 1.4182 (0.0076) 107.95 (0.48) Fe1 2.0379 (0.0048) 69.47 (0.27) 70.75 (0.30) H6 0.9500 126.02 126.02 125.34 C6 - C7 C10 Fe1 C7 - Distance Angles C6 1.4158 (0.0068) C8 1.4294 (0.0068) 107.95 (0.47) Fe1 2.0332 (0.0048) 69.83 (0.28) 70.14 (0.27) H7 0.9500 126.03 126.03 125.59 C7 - C6 C8 Fe1 C8 - Distance Angles C9 1.4118 (0.0069) C7 1.4294 (0.0068) 107.83 (0.46) Fe1 2.0499 (0.0047) 70.26 (0.28) 68.88 (0.27) H8 0.9500 126.08 126.08 126.34 C8 - C9 C7 Fe1 C9 - Distance Angles C8 1.4118 (0.0069) C10 1.4203 (0.0076) 108.15 (0.49) Fe1 2.0593 (0.0050) 69.55 (0.28) 70.02 (0.30) H9 0.9500 125.93 125.93 126.09 C9 - C8 C10 Fe1 C10 - Distance Angles C9 1.4203 (0.0076) C6 1.4182 (0.0076) 108.11 (0.47) Fe1 2.0637 (0.0050) 69.68 (0.28) 68.80 (0.28) H10 0.9500 125.95 125.95 127.15 C10 - C9 C6 Fe1 C11 - Distance Angles C16 1.3933 (0.0067) C12 1.4231 (0.0068) 116.51 (0.45) C1 1.4684 (0.0067) 119.74 (0.45) 123.67 (0.45) C11 - C16 C12 C12 - Distance Angles C13 1.3763 (0.0066) C11 1.4231 (0.0068) 122.35 (0.46) Cl1 1.7431 (0.0050) 116.85 (0.39) 120.77 (0.38) C12 - C13 C11 C13 - Distance Angles C12 1.3763 (0.0066) C14 1.3814 (0.0068) 119.29 (0.46) H13 0.9500 120.35 120.35 C13 - C12 C14 C14 - Distance Angles C13 1.3814 (0.0068) C15 1.4155 (0.0070) 120.27 (0.46) C17 1.4480 (0.0073) 119.75 (0.48) 119.97 (0.48) C14 - C13 C15 C15 - Distance Angles C16 1.3770 (0.0068) C14 1.4155 (0.0070) 119.15 (0.48) C18 1.4515 (0.0076) 120.29 (0.48) 120.55 (0.48) C15 - C16 C14 C16 - Distance Angles C15 1.3770 (0.0068) C11 1.3933 (0.0067) 122.40 (0.48) H16 0.9500 118.80 118.80 C16 - C15 C11 C17 - Distance Angles N1 1.1520 (0.0064) C14 1.4480 (0.0073) 178.18 (0.56) C17 - N1 C18 - Distance Angles N2 1.1427 (0.0066) C15 1.4515 (0.0076) 179.50 (0.64) C18 - N2 N1 - Distance Angles C17 1.1520 (0.0064) N1 - N2 - Distance Angles C18 1.1427 (0.0066) N2 - Cl1 - Distance Angles C12 1.7431 (0.0051) Cl1 - Fe1 - Distance Angles C4 2.0312 (0.0047) C7 2.0332 (0.0048) 127.27 (0.21) C6 2.0379 (0.0048) 166.82 (0.23) 40.70 (0.19) C5 2.0392 (0.0049) 40.74 (0.20) 165.90 (0.20) 152.07 (0.22) C3 2.0453 (0.0050) 40.64 (0.21) 106.97 (0.21) 129.95 (0.23) 68.40 (0.21) C2 2.0460 (0.0048) 68.55 (0.21) 117.00 (0.20) 110.07 (0.22) 68.78 (0.21) 40.49 (0.19) C8 2.0499 (0.0048) 105.50 (0.21) 40.98 (0.19) 68.52 (0.20) 127.60 (0.20) 114.97 (0.21) 148.79 (0.21) C9 2.0593 (0.0050) 115.35 (0.23) 68.26 (0.21) 68.23 (0.22) 108.08 (0.22) 147.74 (0.22) 170.54 (0.21) 40.19 (0.20) C10 2.0637 (0.0050) 149.65 (0.25) 68.03 (0.21) 40.45 (0.21) 118.65 (0.23) 169.59 (0.24) 132.53 (0.22) 67.77 (0.21) C1 2.0690 (0.0048) 68.62 (0.20) 151.25 (0.20) 119.53 (0.20) 40.95 (0.19) 68.28 (0.20) 40.80 (0.19) 167.52 (0.20) Fe1 - C4 C7 C6 C5 C3 C2 C8 C101 - Distance Angles C105 1.4263 (0.0068) C102 1.4437 (0.0067) 106.58 (0.44) C111 1.4645 (0.0068) 129.96 (0.46) 123.45 (0.46) Fe11 2.0672 (0.0048) 68.63 (0.28) 68.30 (0.27) 128.51 (0.34) C101 - C105 C102 C111 C102 - Distance Angles C103 1.4095 (0.0069) C101 1.4437 (0.0067) 107.88 (0.46) Fe11 2.0373 (0.0047) 69.58 (0.28) 70.52 (0.27) H102 0.9500 126.06 126.06 125.43 C102 - C103 C101 Fe11 C103 - Distance Angles C102 1.4095 (0.0069) C104 1.4187 (0.0073) 109.38 (0.47) Fe11 2.0331 (0.0047) 69.90 (0.27) 70.14 (0.29) H103 0.9500 125.31 125.31 126.24 C103 - C102 C104 Fe11 C104 - Distance Angles C103 1.4187 (0.0074) C105 1.4244 (0.0071) 106.91 (0.48) Fe11 2.0461 (0.0050) 69.16 (0.29) 69.34 (0.29) H104 0.9500 126.55 126.55 126.52 C104 - C103 C105 Fe11 C105 - Distance Angles C104 1.4244 (0.0071) C101 1.4263 (0.0068) 109.22 (0.47) Fe11 2.0393 (0.0052) 69.85 (0.30) 70.73 (0.29) H105 0.9500 125.39 125.39 125.61 C105 - C104 C101 Fe11 C106 - Distance Angles C110 1.4030 (0.0074) C107 1.4204 (0.0075) 108.23 (0.48) Fe11 2.0453 (0.0050) 69.46 (0.29) 70.13 (0.28) H106 0.9500 125.89 125.89 126.10 C106 - C110 C107 Fe11 C107 - Distance Angles C106 1.4204 (0.0075) C108 1.4250 (0.0074) 107.11 (0.50) Fe11 2.0558 (0.0050) 69.34 (0.29) 68.89 (0.30) H107 0.9500 126.44 126.44 126.88 C107 - C106 C108 Fe11 C108 - Distance Angles C109 1.4126 (0.0079) C107 1.4250 (0.0074) 108.20 (0.50) Fe11 2.0363 (0.0052) 69.82 (0.31) 70.36 (0.29) H108 0.9500 125.90 125.90 125.51 C108 - C109 C107 Fe11 C109 - Distance Angles C110 1.4083 (0.0076) C108 1.4126 (0.0079) 107.77 (0.52) Fe11 2.0389 (0.0056) 69.59 (0.31) 69.62 (0.32) H109 0.9500 126.12 126.12 126.25 C109 - C110 C108 Fe11 C110 - Distance Angles C106 1.4030 (0.0074) C109 1.4083 (0.0076) 108.69 (0.52) Fe11 2.0342 (0.0050) 70.31 (0.29) 69.96 (0.31) H110 0.9500 125.66 125.66 125.66 C110 - C106 C109 Fe11 C111 - Distance Angles C112 1.3952 (0.0068) C116 1.4022 (0.0067) 116.15 (0.46) C101 1.4645 (0.0068) 123.87 (0.46) 119.79 (0.45) C111 - C112 C116 C112 - Distance Angles C113 1.3781 (0.0065) C111 1.3952 (0.0068) 122.43 (0.47) Cl11 1.7430 (0.0050) 116.62 (0.39) 120.84 (0.38) C112 - C113 C111 C113 - Distance Angles C114 1.3752 (0.0067) C112 1.3781 (0.0065) 121.28 (0.47) H113 0.9500 119.36 119.36 C113 - C114 C112 C114 - Distance Angles C113 1.3752 (0.0067) C115 1.4227 (0.0069) 118.03 (0.46) C117 1.4338 (0.0073) 121.67 (0.48) 120.30 (0.47) C114 - C113 C115 C115 - Distance Angles C116 1.3842 (0.0067) C114 1.4227 (0.0069) 119.67 (0.46) C118 1.4518 (0.0074) 120.80 (0.47) 119.52 (0.46) C115 - C116 C114 C116 - Distance Angles C115 1.3842 (0.0067) C111 1.4022 (0.0067) 122.41 (0.47) H116 0.9500 118.79 118.79 C116 - C115 C111 C117 - Distance Angles N101 1.1553 (0.0063) C114 1.4338 (0.0073) 177.94 (0.58) C117 - N101 C118 - Distance Angles N102 1.1380 (0.0063) C115 1.4518 (0.0073) 178.78 (0.59) C118 - N102 N101 - Distance Angles C117 1.1553 (0.0064) N101 - N102 - Distance Angles C118 1.1380 (0.0063) N102 - Cl11 - Distance Angles C112 1.7430 (0.0050) Cl11 - Fe11 - Distance Angles C103 2.0331 (0.0048) C110 2.0342 (0.0050) 157.43 (0.23) C108 2.0363 (0.0052) 105.61 (0.22) 68.09 (0.23) C109 2.0389 (0.0056) 120.78 (0.22) 40.45 (0.22) 40.56 (0.22) C102 2.0373 (0.0048) 40.52 (0.20) 161.18 (0.22) 121.78 (0.22) 157.02 (0.23) C105 2.0393 (0.0052) 68.23 (0.21) 108.68 (0.22) 157.14 (0.22) 122.20 (0.23) 68.72 (0.20) C104 2.0461 (0.0050) 40.70 (0.21) 122.23 (0.23) 120.24 (0.22) 105.32 (0.22) 68.83 (0.21) 40.81 (0.20) C106 2.0453 (0.0050) 159.58 (0.24) 40.23 (0.21) 68.22 (0.21) 68.01 (0.22) 124.89 (0.22) 124.93 (0.22) 159.38 (0.24) C107 2.0558 (0.0050) 122.24 (0.22) 68.01 (0.22) 40.75 (0.21) 68.29 (0.23) 108.01 (0.21) 161.03 (0.22) 157.13 (0.22) C101 2.0672 (0.0048) 68.46 (0.20) 124.75 (0.22) 159.61 (0.22) 159.33 (0.23) 41.18 (0.19) 40.64 (0.19) 68.80 (0.20) Fe11 - C103 C110 C108 C109 C102 C105 C104 FMAP and GRID set by program FMAP 2 1 18 GRID -3.333 -2 -1 3.333 2 1 R1 = 0.1092 for 5192 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.47 at -0.0029 0.9006 0.3778 [ 1.22 A from FE1 ] Deepest hole -0.51 at 0.0661 0.4574 0.1320 [ 1.41 A from C9 ] Mean = 0.00, Rms deviation from mean = 0.12 e/A^3, Highest memory used = 4845 / 40089 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0029 0.0994 0.6222 1.00000 0.05 0.47 1.22 FE1 1.47 C10 1.79 H10 1.85 C9 Q2 1 0.4303 0.0731 0.5422 1.00000 0.05 0.45 0.88 H4 1.40 C4 2.04 C3 2.15 H6 Q3 1 0.0937 0.2536 0.6303 1.00000 0.05 0.44 0.66 C11 0.85 C1 1.74 C16 1.92 C12 Q4 1 0.5287 0.6931 0.5273 1.00000 0.05 0.43 1.25 FE11 1.58 C109 1.67 C104 1.82 H109 Q5 1 0.4816 0.0380 0.5807 1.00000 0.05 0.42 0.83 H4 1.57 C4 1.90 H6 2.14 C6 Q6 1 0.3601 0.6415 0.7568 1.00000 0.05 0.40 0.93 N102 1.01 C118 2.25 C115 2.75 N2 Q7 1 0.1685 0.6183 0.6604 1.00000 0.05 0.39 1.72 H106 1.90 H13 1.95 N2 2.60 C13 Q8 1 -0.3850 0.1330 0.6271 1.00000 0.05 0.38 1.70 H6 1.73 H10 2.01 C6 2.03 C10 Q9 1 -0.0092 0.0901 0.5473 1.00000 0.05 0.38 1.13 FE1 1.42 C7 1.76 H7 1.87 C3 Q10 1 0.5385 0.6843 0.6048 1.00000 0.05 0.38 1.10 FE11 1.64 C102 1.73 C101 1.94 C107 Shortest distances between peaks (including symmetry equivalents) 2 5 1.29 5 8 2.09 1 3 2.16 1 9 2.27 4 10 2.35 1 8 2.91 2 8 2.96 Time profile in seconds ----------------------- 0.09: Read and process instructions 0.00: Fit rigid groups 0.00: 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 0.02: Analyse other restraints etc. 3.81: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.03: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 5.03: Structure factors and derivatives 12.73: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.06: Apply other restraints 1.97: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.14: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.17: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src0902r finished at 21:59:28 Total CPU time: 24.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++