+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2006src1374 started at 11:55:34 on 05-Jun-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL Test in Pbcn CELL 0.71073 19.6222 7.8609 21.3982 90.000 90.000 90.000 ZERR 4.00 0.0011 0.0003 0.0011 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, 1/2 - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, - Z SYMM - X, Y, 1/2 - Z SFAC C H O FE B UNIT 144 160 32 8 16 V = 3300.63 F(000) = 1568.0 Mu = 0.93 mm-1 Cell Wt = 3022.48 Rho = 1.521 MERG 2 OMIT -3.00 55.00 SHEL 7 0.80 FMAP 2 PLAN 10 SIZE 0.01 0.04 0.19 ACTA BOND $H WGHT 0.00000 18.24770 L.S. 10 TEMP -153.00 FVAR 0.24944 C1 1 0.595332 0.240479 0.463439 11.00000 0.04054 0.02765 = 0.02274 0.00900 -0.00078 0.00212 C2 1 0.661017 0.192588 0.439319 11.00000 0.04553 0.02422 = 0.02421 0.00368 0.00008 0.01163 AFIX 43 H2 2 0.670222 0.093311 0.415452 11.00000 -1.20000 AFIX 0 C3 1 0.709537 0.315882 0.456621 11.00000 0.03697 0.03645 = 0.04259 0.00799 -0.00394 0.00190 AFIX 43 H3 2 0.756518 0.315659 0.445897 11.00000 -1.20000 AFIX 0 C4 1 0.675608 0.439904 0.492819 11.00000 0.04885 0.03114 = 0.02277 0.00172 -0.00936 -0.00204 AFIX 43 H4 2 0.696165 0.536819 0.511477 11.00000 -1.20000 AFIX 0 C5 1 0.605529 0.395373 0.496649 11.00000 0.04716 0.03133 = 0.01757 0.00118 -0.00433 0.00196 AFIX 43 H5 2 0.571253 0.458360 0.517808 11.00000 -1.20000 AFIX 0 C6 1 0.629255 0.417445 0.310135 11.00000 0.04648 0.02683 = 0.01721 0.00240 0.00118 0.00054 C7 1 0.669215 0.559023 0.331809 11.00000 0.04917 0.03068 = 0.02108 0.00577 0.00117 -0.00690 AFIX 43 H7 2 0.716011 0.579089 0.323134 11.00000 -1.20000 AFIX 0 C8 1 0.625573 0.663793 0.368759 11.00000 0.06740 0.01961 = 0.02317 0.00321 0.00142 -0.00270 AFIX 43 H8 2 0.638627 0.766602 0.388791 11.00000 -1.20000 AFIX 0 C9 1 0.560910 0.591568 0.370798 11.00000 0.05399 0.03124 = 0.02934 0.01017 0.00858 0.01472 AFIX 43 H9 2 0.522635 0.635784 0.392599 11.00000 -1.20000 AFIX 0 C10 1 0.562074 0.441868 0.335004 11.00000 0.03747 0.04011 = 0.02034 0.00482 -0.00622 0.00011 AFIX 43 H10 2 0.524336 0.368384 0.328315 11.00000 -1.20000 AFIX 0 C11 1 0.450458 -0.023641 0.400915 11.00000 0.03835 0.02415 = 0.02684 0.00734 0.00226 -0.00473 AFIX 13 H11 2 0.429508 -0.128418 0.419171 11.00000 -1.20000 AFIX 0 C12 1 0.412200 0.134525 0.426412 11.00000 0.04193 0.02595 = 0.02242 0.00521 0.00661 0.00209 AFIX 13 H12 2 0.385387 0.100779 0.464171 11.00000 -1.20000 AFIX 0 C13 1 0.366002 0.223545 0.381317 11.00000 0.04085 0.02821 = 0.02722 -0.00018 0.01050 0.00200 AFIX 23 H13A 2 0.391516 0.248359 0.342458 11.00000 -1.20000 H13B 2 0.351446 0.333355 0.399619 11.00000 -1.20000 AFIX 0 C14 1 0.302442 0.117581 0.365114 11.00000 0.03728 0.03188 = 0.02995 0.00153 0.00602 -0.00497 AFIX 23 H14A 2 0.305768 0.006599 0.386769 11.00000 -1.20000 H14B 2 0.261752 0.176927 0.381634 11.00000 -1.20000 AFIX 0 C15 1 0.291869 0.085013 0.295534 11.00000 0.03828 0.02284 = 0.03196 0.00282 -0.00166 -0.00377 AFIX 13 H15 2 0.246960 0.027223 0.289420 11.00000 -1.20000 AFIX 0 C16 1 0.347633 -0.016817 0.260382 11.00000 0.04322 0.02524 = 0.02891 -0.00171 -0.00411 -0.00481 AFIX 13 H16 2 0.323889 -0.090261 0.229047 11.00000 -1.20000 AFIX 0 C17 1 0.396794 -0.131419 0.296765 11.00000 0.04681 0.02990 = 0.02489 -0.00108 0.00103 -0.00398 AFIX 23 H17A 2 0.370058 -0.193906 0.328584 11.00000 -1.20000 H17B 2 0.415363 -0.216863 0.267349 11.00000 -1.20000 AFIX 0 C18 1 0.456738 -0.046428 0.329759 11.00000 0.03660 0.02082 = 0.02329 -0.00101 0.00701 0.00856 AFIX 23 H18A 2 0.463686 0.067145 0.310808 11.00000 -1.20000 H18B 2 0.498182 -0.114379 0.321213 11.00000 -1.20000 AFIX 0 O1 3 0.519392 -0.005114 0.425339 11.00000 0.04665 0.02639 = 0.02742 -0.00152 -0.00298 0.00723 O2 3 0.466516 0.248615 0.445252 11.00000 0.03669 0.02884 = 0.02885 -0.00492 0.00053 -0.00122 O3 3 0.290936 0.247158 0.262776 11.00000 0.03758 0.03165 = 0.03035 0.00034 0.00065 0.00202 O4 3 0.385732 0.110627 0.225648 11.00000 0.04504 0.03010 = 0.02227 0.00046 0.00487 0.00209 FE1 4 0.631571 0.424795 0.405832 11.00000 0.04166 0.02286 = 0.01784 0.00099 0.00208 0.00437 B1 5 0.527148 0.159203 0.445263 11.00000 0.04117 0.03069 = 0.01401 0.00512 0.00084 0.00290 B2 5 0.348551 0.256103 0.225952 11.00000 0.03445 0.03146 = 0.02427 -0.00819 -0.00127 0.00010 HKLF 4 Covalent radii and connectivity table for Test in Pbcn C 0.770 H 0.320 O 0.660 FE 1.240 B 0.820 C1 - C5 C2 B1 Fe1 C2 - C3 C1 Fe1 C3 - C2 C4 Fe1 C4 - C3 C5 Fe1 C5 - C4 C1 Fe1 C6 - C10 C7 B2_$1 Fe1 C7 - C8 C6 Fe1 C8 - C9 C7 Fe1 C9 - C8 C10 Fe1 C10 - C9 C6 Fe1 C11 - O1 C18 C12 C12 - O2 C13 C11 C13 - C12 C14 C14 - C15 C13 C15 - O3 C14 C16 C16 - O4 C17 C15 C17 - C18 C16 C18 - C17 C11 O1 - B1 C11 O2 - B1 C12 O3 - B2 C15 O4 - B2 C16 Fe1 - C5 C1 C7 C8 C10 C2 C6 C9 C4 C3 B1 - O1 O2 C1 B2 - O4 O3 C6_$1 Operators for generating equivalent atoms: $1 -x+1, y, -z+1/2 h k l Fo^2 Sigma Why rejected 13 0 0 49.71 10.10 observed but should be systematically absent 28729 Reflections read, of which 3595 rejected -24 =< h =< 13, -8 =< k =< 9, -26 =< l =< 26, Max. 2-theta = 52.74 1 Systematic absence violations 0 Inconsistent equivalents 3366 Unique reflections, of which 0 suppressed R(int) = 0.1290 R(sigma) = 0.0793 Friedel opposites merged Maximum memory for data reduction = 2624 / 33481 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 = 3270 / 281092 wR2 = 0.1676 before cycle 1 for 3366 data and 226 / 226 parameters GooF = S = 1.219; Restrained GooF = 1.219 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 18.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24944 0.00065 -0.003 OSF Mean shift/esd = 0.001 Maximum = -0.008 for z Fe1 Max. shift = 0.000 A for B2 Max. dU = 0.000 for C4 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3270 / 281092 wR2 = 0.1676 before cycle 2 for 3366 data and 226 / 226 parameters GooF = S = 1.219; Restrained GooF = 1.219 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 18.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24944 0.00065 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.003 for z Fe1 Max. shift = 0.000 A for O1 Max. dU = 0.000 for C4 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3270 / 281092 wR2 = 0.1676 before cycle 3 for 3366 data and 226 / 226 parameters GooF = S = 1.219; Restrained GooF = 1.219 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 18.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24944 0.00065 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for B1 Max. dU = 0.000 for C4 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3270 / 281092 wR2 = 0.1676 before cycle 4 for 3366 data and 226 / 226 parameters GooF = S = 1.219; Restrained GooF = 1.219 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 18.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24944 0.00065 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x Fe1 Max. shift = 0.000 A for C9 Max. dU = 0.000 for O1 Least-squares cycle 5 Maximum vector length = 511 Memory required = 3270 / 281092 wR2 = 0.1676 before cycle 5 for 3366 data and 226 / 226 parameters GooF = S = 1.219; Restrained GooF = 1.219 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 18.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24944 0.00065 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x Fe1 Max. shift = 0.000 A for C15 Max. dU = 0.000 for C17 Least-squares cycle 6 Maximum vector length = 511 Memory required = 3270 / 281092 wR2 = 0.1676 before cycle 6 for 3366 data and 226 / 226 parameters GooF = S = 1.219; Restrained GooF = 1.219 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 18.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24944 0.00065 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x Fe1 Max. shift = 0.000 A for B2 Max. dU = 0.000 for B1 Least-squares cycle 7 Maximum vector length = 511 Memory required = 3270 / 281092 wR2 = 0.1676 before cycle 7 for 3366 data and 226 / 226 parameters GooF = S = 1.219; Restrained GooF = 1.219 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 18.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24944 0.00065 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x Fe1 Max. shift = 0.000 A for C7 Max. dU = 0.000 for C8 Least-squares cycle 8 Maximum vector length = 511 Memory required = 3270 / 281092 wR2 = 0.1676 before cycle 8 for 3366 data and 226 / 226 parameters GooF = S = 1.219; Restrained GooF = 1.219 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 18.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24944 0.00065 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x Fe1 Max. shift = 0.000 A for H18A Max. dU = 0.000 for C12 Least-squares cycle 9 Maximum vector length = 511 Memory required = 3270 / 281092 wR2 = 0.1676 before cycle 9 for 3366 data and 226 / 226 parameters GooF = S = 1.219; Restrained GooF = 1.219 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 18.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24944 0.00065 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x Fe1 Max. shift = 0.000 A for C7 Max. dU = 0.000 for C3 Least-squares cycle 10 Maximum vector length = 511 Memory required = 3270 / 281092 wR2 = 0.1676 before cycle 10 for 3366 data and 226 / 226 parameters GooF = S = 1.219; Restrained GooF = 1.219 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 18.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24944 0.00065 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x Fe1 Max. shift = 0.000 A for C13 Max. dU = 0.000 for O4 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 0.6702 0.0933 0.4155 43 0.950 0.000 C2 C3 C1 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C3 ** H3 0.7565 0.3157 0.4459 43 0.950 0.000 C3 C2 C4 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C4 ** H4 0.6962 0.5368 0.5115 43 0.950 0.000 C4 C3 C5 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C5 ** H5 0.5713 0.4584 0.5178 43 0.950 0.000 C5 C4 C1 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C7 ** H7 0.7160 0.5791 0.3231 43 0.950 0.000 C7 C8 C6 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C8 ** H8 0.6386 0.7666 0.3888 43 0.950 0.000 C8 C9 C7 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C9 ** H9 0.5226 0.6358 0.3926 43 0.950 0.000 C9 C8 C10 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C10 ** H10 0.5243 0.3684 0.3283 43 0.950 0.000 C10 C9 C6 H11 0.4295 -0.1284 0.4192 13 1.000 0.000 C11 O1 C18 C12 H12 0.3854 0.1008 0.4642 13 1.000 0.000 C12 O2 C13 C11 H13A 0.3915 0.2484 0.3425 23 0.990 0.000 C13 C12 C14 H13B 0.3514 0.3334 0.3996 23 0.990 0.000 C13 C12 C14 H14A 0.3058 0.0066 0.3868 23 0.990 0.000 C14 C15 C13 H14B 0.2618 0.1769 0.3816 23 0.990 0.000 C14 C15 C13 H15 0.2470 0.0272 0.2894 13 1.000 0.000 C15 O3 C14 C16 H16 0.3239 -0.0903 0.2290 13 1.000 0.000 C16 O4 C17 C15 H17A 0.3701 -0.1939 0.3286 23 0.990 0.000 C17 C18 C16 H17B 0.4154 -0.2169 0.2673 23 0.990 0.000 C17 C18 C16 H18A 0.4637 0.0671 0.3108 23 0.990 0.000 C18 C17 C11 H18B 0.4982 -0.1144 0.3212 23 0.990 0.000 C18 C17 C11 Test in Pbcn ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.59533 0.24048 0.46344 1.00000 0.04054 0.02765 0.02274 0.00900 -0.00078 0.00212 0.03031 0.01106 0.00035 0.00077 0.00026 0.00000 0.00404 0.00333 0.00298 0.00255 0.00284 0.00309 0.00146 C2 0.66102 0.19259 0.43932 1.00000 0.04552 0.02422 0.02421 0.00368 0.00008 0.01163 0.03132 0.01131 0.00035 0.00078 0.00027 0.00000 0.00423 0.00325 0.00304 0.00251 0.00297 0.00307 0.00152 H2 0.67022 0.09331 0.41545 1.00000 0.03758 0.00000 0.00000 C3 0.70954 0.31588 0.45662 1.00000 0.03697 0.03645 0.04259 0.00800 -0.00394 0.00190 0.03867 0.01183 0.00037 0.00083 0.00030 0.00000 0.00417 0.00384 0.00391 0.00313 0.00328 0.00336 0.00167 H3 0.75652 0.31566 0.44590 1.00000 0.04641 0.00000 0.00000 C4 0.67561 0.43990 0.49282 1.00000 0.04885 0.03113 0.02277 0.00172 -0.00936 -0.00204 0.03425 0.01106 0.00035 0.00083 0.00026 0.00000 0.00436 0.00358 0.00291 0.00275 0.00291 0.00338 0.00156 H4 0.69616 0.53682 0.51148 1.00000 0.04110 0.00000 0.00000 C5 0.60553 0.39537 0.49665 1.00000 0.04716 0.03133 0.01757 0.00118 -0.00433 0.00196 0.03202 0.01054 0.00036 0.00077 0.00025 0.00000 0.00405 0.00361 0.00271 0.00250 0.00273 0.00324 0.00151 H5 0.57125 0.45836 0.51781 1.00000 0.03842 0.00000 0.00000 C6 0.62925 0.41745 0.31013 1.00000 0.04648 0.02683 0.01721 0.00240 0.00118 0.00055 0.03017 0.01060 0.00035 0.00078 0.00024 0.00000 0.00380 0.00304 0.00249 0.00240 0.00285 0.00337 0.00135 C7 0.66921 0.55902 0.33181 1.00000 0.04917 0.03068 0.02108 0.00577 0.00117 -0.00689 0.03365 0.01075 0.00036 0.00077 0.00025 0.00000 0.00410 0.00344 0.00278 0.00273 0.00291 0.00330 0.00149 H7 0.71601 0.57909 0.32313 1.00000 0.04038 0.00000 0.00000 C8 0.62557 0.66379 0.36876 1.00000 0.06741 0.01961 0.02317 0.00321 0.00142 -0.00271 0.03673 0.01166 0.00039 0.00076 0.00026 0.00000 0.00516 0.00306 0.00299 0.00239 0.00348 0.00350 0.00167 H8 0.63863 0.76660 0.38879 1.00000 0.04407 0.00000 0.00000 C9 0.56091 0.59157 0.37080 1.00000 0.05399 0.03124 0.02934 0.01017 0.00858 0.01471 0.03819 0.01250 0.00038 0.00082 0.00028 0.00000 0.00452 0.00369 0.00329 0.00288 0.00320 0.00361 0.00167 H9 0.52264 0.63578 0.39260 1.00000 0.04583 0.00000 0.00000 C10 0.56207 0.44187 0.33500 1.00000 0.03747 0.04011 0.02033 0.00482 -0.00622 0.00011 0.03264 0.01107 0.00034 0.00084 0.00026 0.00000 0.00375 0.00368 0.00275 0.00279 0.00272 0.00323 0.00146 H10 0.52434 0.36838 0.32832 1.00000 0.03916 0.00000 0.00000 C11 0.45046 -0.02364 0.40091 1.00000 0.03835 0.02415 0.02684 0.00734 0.00226 -0.00473 0.02978 0.01045 0.00032 0.00073 0.00027 0.00000 0.00372 0.00314 0.00299 0.00263 0.00295 0.00272 0.00141 H11 0.42951 -0.12842 0.41917 1.00000 0.03574 0.00000 0.00000 C12 0.41220 0.13452 0.42641 1.00000 0.04193 0.02595 0.02242 0.00521 0.00661 0.00209 0.03010 0.01096 0.00034 0.00075 0.00027 0.00000 0.00407 0.00323 0.00281 0.00249 0.00277 0.00298 0.00148 H12 0.38539 0.10078 0.46417 1.00000 0.03612 0.00000 0.00000 C13 0.36600 0.22354 0.38132 1.00000 0.04085 0.02821 0.02722 -0.00018 0.01050 0.00200 0.03209 0.01093 0.00035 0.00076 0.00027 0.00000 0.00388 0.00321 0.00287 0.00257 0.00302 0.00320 0.00144 H13A 0.39152 0.24836 0.34246 1.00000 0.03851 0.00000 0.00000 H13B 0.35145 0.33335 0.39962 1.00000 0.03851 0.00000 0.00000 C14 0.30244 0.11758 0.36511 1.00000 0.03728 0.03188 0.02995 0.00153 0.00602 -0.00497 0.03304 0.01057 0.00033 0.00080 0.00028 0.00000 0.00392 0.00361 0.00320 0.00272 0.00296 0.00298 0.00154 H14A 0.30577 0.00660 0.38677 1.00000 0.03964 0.00000 0.00000 H14B 0.26175 0.17693 0.38163 1.00000 0.03964 0.00000 0.00000 C15 0.29187 0.08501 0.29553 1.00000 0.03828 0.02284 0.03196 0.00283 -0.00166 -0.00377 0.03102 0.01064 0.00033 0.00075 0.00027 0.00000 0.00371 0.00312 0.00316 0.00276 0.00284 0.00308 0.00141 H15 0.24696 0.02722 0.28942 1.00000 0.03723 0.00000 0.00000 C16 0.34763 -0.01682 0.26038 1.00000 0.04322 0.02524 0.02890 -0.00171 -0.00411 -0.00481 0.03246 0.01064 0.00034 0.00075 0.00028 0.00000 0.00416 0.00320 0.00311 0.00259 0.00293 0.00293 0.00153 H16 0.32389 -0.09026 0.22905 1.00000 0.03895 0.00000 0.00000 C17 0.39679 -0.13142 0.29676 1.00000 0.04681 0.02990 0.02489 -0.00108 0.00103 -0.00398 0.03387 0.01068 0.00035 0.00078 0.00028 0.00000 0.00420 0.00338 0.00300 0.00264 0.00302 0.00309 0.00155 H17A 0.37006 -0.19391 0.32858 1.00000 0.04064 0.00000 0.00000 H17B 0.41536 -0.21686 0.26735 1.00000 0.04064 0.00000 0.00000 C18 0.45674 -0.04643 0.32976 1.00000 0.03660 0.02082 0.02329 -0.00101 0.00701 0.00856 0.02690 0.01011 0.00031 0.00071 0.00025 0.00000 0.00363 0.00298 0.00277 0.00240 0.00268 0.00274 0.00136 H18A 0.46369 0.06715 0.31081 1.00000 0.03229 0.00000 0.00000 H18B 0.49818 -0.11438 0.32121 1.00000 0.03229 0.00000 0.00000 O1 0.51939 -0.00511 0.42534 1.00000 0.04665 0.02639 0.02742 -0.00152 -0.00298 0.00723 0.03348 0.00738 0.00023 0.00052 0.00018 0.00000 0.00289 0.00218 0.00213 0.00182 0.00207 0.00214 0.00106 O2 0.46652 0.24862 0.44525 1.00000 0.03668 0.02883 0.02885 -0.00492 0.00053 -0.00122 0.03146 0.00706 0.00023 0.00051 0.00018 0.00000 0.00267 0.00226 0.00221 0.00187 0.00194 0.00213 0.00102 O3 0.29094 0.24716 0.26278 1.00000 0.03758 0.03165 0.03035 0.00034 0.00065 0.00202 0.03319 0.00720 0.00022 0.00052 0.00019 0.00000 0.00261 0.00231 0.00229 0.00188 0.00204 0.00213 0.00103 O4 0.38573 0.11063 0.22565 1.00000 0.04504 0.03010 0.02227 0.00047 0.00486 0.00209 0.03247 0.00704 0.00022 0.00050 0.00017 0.00000 0.00285 0.00236 0.00195 0.00172 0.00192 0.00205 0.00106 Fe1 0.63157 0.42479 0.40583 1.00000 0.04166 0.02286 0.01784 0.00099 0.00208 0.00437 0.02745 0.00149 0.00005 0.00010 0.00004 0.00000 0.00052 0.00042 0.00037 0.00036 0.00041 0.00045 0.00024 B1 0.52715 0.15920 0.44526 1.00000 0.04117 0.03069 0.01402 0.00512 0.00084 0.00290 0.02862 0.01281 0.00042 0.00091 0.00029 0.00000 0.00468 0.00387 0.00297 0.00278 0.00303 0.00358 0.00166 B2 0.34855 0.25610 0.22595 1.00000 0.03445 0.03146 0.02426 -0.00820 -0.00127 0.00010 0.03006 0.01192 0.00038 0.00094 0.00031 0.00000 0.00430 0.00387 0.00335 0.00295 0.00313 0.00341 0.00164 Final Structure Factor Calculation for Test in Pbcn Total number of l.s. parameters = 226 Maximum vector length = 511 Memory required = 3044 / 24017 wR2 = 0.1676 before cycle 11 for 3366 data and 0 / 226 parameters GooF = S = 1.219; Restrained GooF = 1.219 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 18.25 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0905 for 2254 Fo > 4sig(Fo) and 0.1451 for all 3366 data wR2 = 0.1676, GooF = S = 1.219, Restrained GooF = 1.219 for all data Occupancy sum of asymmetric unit = 25.00 for non-hydrogen and 20.00 for hydrogen atoms Principal mean square atomic displacements U 0.0409 0.0343 0.0157 C1 0.0507 0.0258 0.0174 C2 0.0485 0.0384 0.0291 C3 0.0521 0.0309 0.0197 C4 0.0480 0.0313 0.0168 C5 0.0466 0.0274 0.0166 C6 0.0515 0.0316 0.0178 C7 0.0676 0.0251 0.0175 C8 0.0654 0.0297 0.0195 C9 0.0418 0.0387 0.0174 C10 0.0398 0.0327 0.0168 C11 0.0446 0.0278 0.0179 C12 0.0467 0.0282 0.0213 C13 0.0421 0.0326 0.0244 C14 0.0398 0.0318 0.0214 C15 0.0452 0.0294 0.0228 C16 0.0478 0.0292 0.0247 C17 0.0423 0.0234 0.0150 C18 0.0495 0.0270 0.0240 O1 0.0372 0.0333 0.0239 O2 0.0383 0.0311 0.0303 O3 0.0463 0.0298 0.0213 O4 0.0428 0.0220 0.0176 Fe1 0.0421 0.0312 0.0126 B1 0.0371 0.0343 0.0188 B2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.009 0.016 0.026 0.035 0.047 0.060 0.079 0.106 0.153 1.000 Number in group 374. 309. 354. 321. 340. 323. 339. 336. 332. 338. GooF 1.447 1.341 1.239 1.399 1.350 1.161 1.181 1.075 0.921 0.935 K 19.066 3.470 1.728 1.401 1.137 1.022 1.000 1.003 0.999 1.009 Resolution(A) 0.80 0.83 0.86 0.90 0.95 1.01 1.09 1.20 1.37 1.72 inf Number in group 348. 328. 338. 340. 328. 341. 338. 330. 338. 337. GooF 1.330 1.387 1.344 1.351 1.231 1.192 1.103 1.078 1.040 1.068 K 1.229 1.295 1.055 1.063 1.034 1.017 1.028 0.995 1.000 1.014 R1 0.339 0.340 0.244 0.225 0.181 0.132 0.109 0.091 0.055 0.037 Recommended weighting scheme: WGHT 0.0000 18.2477 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) 7 2 10 369.48 0.45 4.07 0.002 1.56 15 3 11 415.33 7.06 3.81 0.007 1.00 11 1 19 918.82 251.52 3.72 0.043 0.95 8 3 14 429.02 23.99 3.49 0.013 1.16 5 1 23 409.45 17.29 3.39 0.011 0.90 16 3 6 312.23 6.93 3.34 0.007 1.06 2 8 9 503.05 6.82 3.24 0.007 0.90 1 1 2 3707.24 5625.92 3.22 0.205 6.03 14 1 1 270.02 8.80 3.21 0.008 1.38 18 4 0 867.76 32.55 3.20 0.016 0.95 16 1 6 615.44 32.26 3.18 0.015 1.15 22 3 4 323.26 15.68 3.17 0.011 0.83 19 1 13 636.38 133.70 3.15 0.032 0.87 13 1 13 557.34 3.60 3.12 0.005 1.10 18 3 8 283.34 22.29 3.09 0.013 0.94 2 5 20 695.76 244.29 3.07 0.043 0.88 18 2 1 521.31 162.99 3.05 0.035 1.05 20 2 0 922.60 254.36 3.03 0.044 0.95 12 7 6 -96.88 210.22 3.03 0.040 0.90 16 1 12 288.97 8.34 3.02 0.008 1.00 24 0 2 406.61 2.23 3.01 0.004 0.82 9 1 3 273.76 22.86 3.00 0.013 2.02 13 5 17 813.31 219.07 2.99 0.040 0.82 17 3 17 -92.52 349.09 2.98 0.051 0.81 18 2 16 632.11 162.69 2.96 0.035 0.83 5 1 25 693.61 287.96 2.88 0.046 0.83 10 4 14 245.08 709.71 2.87 0.073 1.03 21 1 6 -70.88 247.81 2.85 0.043 0.90 20 2 5 351.79 6.83 2.84 0.007 0.93 5 7 17 707.85 120.57 2.83 0.030 0.82 5 2 25 940.34 439.09 2.82 0.057 0.82 12 5 14 677.73 101.30 2.82 0.027 0.91 19 2 10 475.68 2.67 2.80 0.004 0.91 23 3 0 360.14 4.68 2.78 0.006 0.81 3 3 24 298.01 2.65 2.74 0.004 0.84 10 0 20 421.25 31.89 2.73 0.015 0.94 10 3 23 506.96 192.37 2.69 0.038 0.80 6 4 23 212.80 676.09 2.68 0.071 0.81 12 4 4 177.97 7.34 2.68 0.007 1.22 5 3 21 399.91 110.26 2.68 0.029 0.92 2 3 25 743.45 306.21 2.67 0.048 0.81 12 5 5 280.63 26.69 2.67 0.014 1.10 12 2 21 317.79 0.60 2.67 0.002 0.84 1 6 20 881.06 470.14 2.65 0.059 0.83 4 5 7 241.01 58.85 2.64 0.021 1.34 16 4 3 1404.63 848.38 2.64 0.079 1.03 14 3 17 641.35 175.96 2.64 0.036 0.88 4 0 0 139341.41 123367.66 2.62 0.958 4.91 9 7 14 431.04 0.93 2.62 0.003 0.84 10 0 8 459.43 138.38 2.60 0.032 1.58 Bond lengths and angles C1 - Distance Angles C5 1.4239 (0.0083) C2 1.4385 (0.0087) 106.08 (0.58) B1 1.5328 (0.0099) 127.28 (0.61) 125.59 (0.56) Fe1 2.0309 (0.0059) 69.12 (0.34) 69.83 (0.34) 116.68 (0.40) C1 - C5 C2 B1 C2 - Distance Angles C3 1.4081 (0.0091) C1 1.4385 (0.0087) 109.35 (0.56) Fe1 2.0443 (0.0059) 70.65 (0.36) 68.83 (0.33) H2 0.9500 125.33 125.33 126.78 C2 - C3 C1 Fe1 C3 - Distance Angles C2 1.4081 (0.0091) C4 1.4120 (0.0089) 107.50 (0.63) Fe1 2.0627 (0.0067) 69.25 (0.37) 69.68 (0.37) H3 0.9500 126.25 126.25 126.39 C3 - C2 C4 Fe1 C4 - Distance Angles C3 1.4120 (0.0089) C5 1.4213 (0.0090) 108.53 (0.59) Fe1 2.0556 (0.0058) 70.22 (0.36) 68.36 (0.33) H4 0.9500 125.74 125.74 127.26 C4 - C3 C5 Fe1 C5 - Distance Angles C4 1.4213 (0.0090) C1 1.4239 (0.0083) 108.53 (0.59) Fe1 2.0227 (0.0057) 70.85 (0.35) 69.74 (0.32) H5 0.9500 125.74 125.74 125.25 C5 - C4 C1 Fe1 C6 - Distance Angles C10 1.4345 (0.0087) C7 1.4382 (0.0086) 106.13 (0.54) B2_$1 1.5474 (0.0093) 123.60 (0.59) 129.92 (0.62) Fe1 2.0491 (0.0052) 69.26 (0.31) 69.13 (0.31) 121.04 (0.41) C6 - C10 C7 B2_$1 C7 - Distance Angles C8 1.4271 (0.0089) C6 1.4382 (0.0086) 107.34 (0.60) Fe1 2.0415 (0.0057) 69.59 (0.33) 69.70 (0.32) H7 0.9500 126.33 126.33 125.95 C7 - C8 C6 Fe1 C8 - Distance Angles C9 1.3908 (0.0094) C7 1.4271 (0.0089) 109.22 (0.57) Fe1 2.0428 (0.0058) 70.42 (0.36) 69.50 (0.33) H8 0.9500 125.39 125.39 126.27 C8 - C9 C7 Fe1 C9 - Distance Angles C8 1.3908 (0.0094) C10 1.4043 (0.0088) 108.07 (0.60) Fe1 2.0502 (0.0065) 69.85 (0.38) 69.67 (0.36) H9 0.9500 125.97 125.97 126.09 C9 - C8 C10 Fe1 C10 - Distance Angles C9 1.4043 (0.0088) C6 1.4345 (0.0088) 109.23 (0.61) Fe1 2.0432 (0.0059) 70.20 (0.37) 69.70 (0.33) H10 0.9500 125.38 125.38 126.30 C10 - C9 C6 Fe1 C11 - Distance Angles O1 1.4574 (0.0073) C18 1.5381 (0.0073) 107.00 (0.48) C12 1.5515 (0.0082) 104.06 (0.47) 118.70 (0.48) H11 1.0000 108.89 108.89 108.89 C11 - O1 C18 C12 C12 - Distance Angles O2 1.4501 (0.0074) C13 1.4975 (0.0084) 109.58 (0.48) C11 1.5515 (0.0082) 103.75 (0.49) 116.15 (0.49) H12 1.0000 109.03 109.03 109.03 C12 - O2 C13 C11 C13 - Distance Angles C12 1.4975 (0.0084) C14 1.5393 (0.0086) 112.50 (0.51) H13A 0.9900 109.10 109.10 H13B 0.9900 109.10 109.10 107.84 C13 - C12 C14 H13A C14 - Distance Angles C15 1.5249 (0.0079) C13 1.5393 (0.0086) 114.90 (0.50) H14A 0.9900 108.54 108.54 H14B 0.9900 108.54 108.54 107.53 C14 - C15 C13 H14A C15 - Distance Angles O3 1.4548 (0.0069) C14 1.5249 (0.0079) 108.97 (0.47) C16 1.5504 (0.0085) 103.15 (0.45) 117.67 (0.53) H15 1.0000 108.90 108.90 108.90 C15 - O3 C14 C16 C16 - Distance Angles O4 1.4543 (0.0070) C17 1.5324 (0.0086) 109.94 (0.51) C15 1.5504 (0.0085) 104.78 (0.45) 120.09 (0.50) H16 1.0000 107.13 107.13 107.13 C16 - O4 C17 C15 C17 - Distance Angles C18 1.5259 (0.0084) C16 1.5324 (0.0086) 117.58 (0.51) H17A 0.9900 107.91 107.91 H17B 0.9900 107.91 107.91 107.20 C17 - C18 C16 H17A C18 - Distance Angles C17 1.5259 (0.0084) C11 1.5381 (0.0073) 116.57 (0.51) H18A 0.9900 108.15 108.15 H18B 0.9900 108.15 108.15 107.32 C18 - C17 C11 H18A O1 - Distance Angles B1 1.3687 (0.0081) C11 1.4574 (0.0073) 108.01 (0.50) O1 - B1 O2 - Distance Angles B1 1.3818 (0.0086) C12 1.4501 (0.0074) 108.56 (0.47) O2 - B1 O3 - Distance Angles B2 1.3798 (0.0080) C15 1.4548 (0.0069) 108.03 (0.49) O3 - B2 O4 - Distance Angles B2 1.3565 (0.0082) C16 1.4543 (0.0070) 107.57 (0.49) O4 - B2 Fe1 - Distance Angles C5 2.0227 (0.0057) C1 2.0309 (0.0059) 41.13 (0.24) C7 2.0415 (0.0058) 153.63 (0.25) 165.09 (0.25) C8 2.0428 (0.0058) 117.63 (0.25) 150.66 (0.28) 40.90 (0.25) C10 2.0432 (0.0059) 123.47 (0.27) 105.27 (0.26) 68.41 (0.26) 67.24 (0.27) C2 2.0443 (0.0059) 68.44 (0.24) 41.34 (0.25) 129.14 (0.26) 166.81 (0.29) 120.48 (0.26) C6 2.0491 (0.0052) 162.05 (0.28) 125.36 (0.25) 41.17 (0.24) 68.69 (0.24) 41.04 (0.25) 109.35 (0.24) C9 2.0502 (0.0065) 104.69 (0.26) 116.19 (0.28) 68.32 (0.27) 39.73 (0.27) 40.13 (0.25) 152.91 (0.29) 68.75 (0.25) C4 2.0556 (0.0058) 40.78 (0.25) 68.83 (0.25) 121.37 (0.26) 108.83 (0.26) 161.52 (0.26) 67.38 (0.25) 156.33 (0.27) C3 2.0627 (0.0067) 68.51 (0.27) 69.13 (0.27) 110.79 (0.28) 128.98 (0.29) 155.94 (0.26) 40.10 (0.25) 122.09 (0.27) Fe1 - C5 C1 C7 C8 C10 C2 C6 B1 - Distance Angles O1 1.3687 (0.0081) O2 1.3818 (0.0085) 112.60 (0.61) C1 1.5328 (0.0099) 124.71 (0.64) 122.65 (0.57) B1 - O1 O2 B2 - Distance Angles O4 1.3565 (0.0082) O3 1.3798 (0.0080) 113.61 (0.59) C6_$1 1.5474 (0.0093) 122.49 (0.58) 123.87 (0.60) B2 - O4 O3 FMAP and GRID set by program FMAP 2 1 23 GRID -1.250 -2 -1 1.250 2 1 R1 = 0.1419 for 3366 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.55 at 0.0883 0.8692 0.1077 [ 1.00 A from FE1 ] Deepest hole -0.48 at 0.2399 0.0661 0.3605 [ 1.07 A from H14B ] Mean = 0.00, Rms deviation from mean = 0.11 e/A^3, Highest memory used = 3162 / 26916 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5883 0.3692 0.3923 1.00000 0.05 0.55 1.00 FE1 1.45 C10 1.83 C1 1.86 H10 Q2 1 0.7003 0.2965 0.4961 1.00000 0.05 0.52 0.88 C3 1.23 C4 1.55 H3 1.65 C2 Q3 1 0.3958 -0.0552 0.4019 1.00000 0.05 0.45 0.95 H11 1.10 C11 1.61 C12 1.82 H12 Q4 1 0.6036 0.2776 0.3595 1.00000 0.05 0.42 1.61 C6 1.61 C10 1.62 FE1 1.84 H10 Q5 1 0.3647 0.4522 0.3386 1.00000 0.05 0.40 1.63 H13B 1.69 H13A 2.02 C13 2.50 H15 Q6 1 0.4449 -0.1625 0.4790 1.00000 0.05 0.40 1.34 H11 1.59 C1 1.71 B1 2.00 C11 Q7 1 0.6375 0.6721 0.3360 1.00000 0.05 0.39 0.74 C8 1.09 C7 1.35 H8 1.73 H7 Q8 1 0.3298 -0.0849 0.4087 1.00000 0.05 0.39 0.98 H14A 1.92 C14 2.00 H11 2.07 H17A Q9 1 0.2979 0.1461 0.3277 1.00000 0.05 0.38 0.84 C14 0.85 C15 1.38 H14B 1.60 H15 Q10 1 0.5788 0.1610 0.4798 1.00000 0.05 0.37 0.79 C1 1.25 B1 1.85 C2 1.95 C5 Shortest distances between peaks (including symmetry equivalents) 6 10 1.00 1 4 1.05 3 8 1.32 3 6 2.09 1 10 2.49 8 9 2.59 2 10 2.63 2 8 2.70 3 10 2.71 5 9 2.75 4 10 2.78 6 8 2.78 1 7 2.84 3 9 2.95 Time profile in seconds ----------------------- 0.06: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 1.52: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.02: Generate idealized H-atoms 2.92: Structure factors and derivatives 2.83: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.41: Solve l.s. equations 0.00: Generate HTAB table 0.06: Other dependent quantities, CIF, tables 0.09: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.06: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2006src1374 finished at 11:55:42 Total CPU time: 8.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++