+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 13:16:00 on 14-Dec-2001 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 01src873 in C2/c CELL 0.71073 26.7983 6.0907 12.6373 90.000 108.968 90.000 ZERR 8.00 0.0023 0.0006 0.0015 0.000 0.003 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H B FE O UNIT 76 72 8 8 32 V = 1950.66 F(000) = 1032.0 Mu = 1.53 mm-1 Cell Wt = 2030.62 Rho = 1.729 SHEL 7 0.84 ACTA TEMP -153 SIZE 0.15 0.15 0.02 OMIT -5 5 1 OMIT 2 4 1 OMIT -8 6 2 FMAP 2 PLAN 10 L.S. 4 WGHT 0.028300 3.923900 FVAR 0.47625 C1 1 0.200653 0.507916 0.071205 11.00000 0.05458 0.04356 = 0.02226 0.00245 0.00004 -0.02685 AFIX 43 H1 2 0.208093 0.586522 0.013141 11.00000 -1.20000 AFIX 0 C2 1 0.223192 0.307441 0.117471 11.00000 0.02430 0.05231 = 0.03558 -0.01026 0.00563 -0.00248 AFIX 43 H2 2 0.249047 0.227526 0.096833 11.00000 -1.20000 AFIX 0 C3 1 0.201262 0.245683 0.198609 11.00000 0.03180 0.04040 = 0.02058 -0.00045 -0.00208 -0.00548 AFIX 43 H3 2 0.209238 0.115793 0.242529 11.00000 -1.20000 AFIX 0 C4 1 0.165350 0.408452 0.204277 11.00000 0.03216 0.05233 = 0.02480 -0.01853 0.00741 -0.00288 AFIX 43 H4 2 0.144708 0.408199 0.252798 11.00000 -1.20000 AFIX 0 C5 1 0.165095 0.571371 0.126274 11.00000 0.04414 0.03112 = 0.03725 -0.01008 -0.01393 0.00793 AFIX 43 H5 2 0.144540 0.701795 0.112873 11.00000 -1.20000 AFIX 0 C6 1 0.141848 0.159441 -0.083146 11.00000 0.02685 0.02458 = 0.03050 -0.00204 0.00828 -0.00505 C7 1 0.095492 0.091476 0.062400 11.00000 0.03159 0.02795 = 0.02115 0.00247 0.00697 0.00507 C9 1 0.045362 0.754533 -0.185364 11.00000 0.03420 0.01901 = 0.02230 0.00325 0.00223 0.00082 AFIX 23 H9A 2 0.057835 0.838748 -0.238928 11.00000 -1.20000 H9B 2 0.032511 0.860592 -0.140744 11.00000 -1.20000 AFIX 0 C10 1 0.000000 0.604483 -0.250000 10.50000 0.02844 0.02320 = 0.01808 0.00000 0.00680 0.00000 C11 1 -0.014974 0.465620 -0.165674 11.00000 0.02207 0.03345 = 0.02032 0.00474 0.00390 0.00412 AFIX 23 H11A 2 -0.030618 0.560670 -0.121192 11.00000 -1.20000 H11B 2 -0.041925 0.356696 -0.205695 11.00000 -1.20000 AFIX 0 B1 3 0.079459 0.438722 -0.064556 11.00000 0.03465 0.02922 = 0.01574 -0.00357 0.01156 0.00059 FE1 4 0.141492 0.274742 0.042078 11.00000 0.02673 0.02886 = 0.02017 -0.00110 0.00567 0.00051 O1 5 0.143068 0.089186 -0.166793 11.00000 0.04095 0.04329 = 0.03066 -0.01309 0.01692 -0.01074 O2 5 0.065362 -0.028195 0.078163 11.00000 0.03999 0.03610 = 0.02619 0.00288 0.01162 -0.00049 O3 5 0.088866 0.630174 -0.111607 11.00000 0.02637 0.03040 = 0.02126 0.00315 0.00237 -0.00236 O4 5 0.030000 0.353168 -0.091879 11.00000 0.02555 0.03275 = 0.02448 0.00671 0.00598 -0.00073 HKLF 4 Covalent radii and connectivity table for 01src873 in C2/c C 0.770 H 0.320 B 0.820 FE 1.240 O 0.660 C1 - C2 C5 Fe1 C2 - C3 C1 Fe1 C3 - C2 C4 Fe1 C4 - C5 C3 Fe1 C5 - C4 C1 Fe1 C6 - O1 Fe1 C7 - O2 Fe1 C9 - O3 C10 C10 - C11_$1 C11 C9 C9_$1 C11 - O4 C10 B1 - O4 O3 Fe1 Fe1 - C6 C7 B1 C1 C5 C2 C4 C3 O1 - C6 O2 - C7 O3 - B1 C9 O4 - B1 C11 Operators for generating equivalent atoms: $1 -x, y, -z-1/2 5588 Reflections read, of which 947 rejected -31 =< h =< 30, -6 =< k =< 6, -15 =< l =< 13, Max. 2-theta = 50.03 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -2 4 2 671.07 25.67 3 129.48 1 Inconsistent equivalents 1649 Unique reflections, of which 0 suppressed R(int) = 0.0580 R(sigma) = 0.0740 Friedel opposites merged Maximum memory for data reduction = 1541 / 19420 Special position constraints for C10 x = 0.0000 z = -0.2500 U23 = 0 U12 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Default effective X-H distances for T = -153.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 1.00 0.99 0.98 0.95 0.88 0.91 1.12 0.84 0.95 0.88 0.95 Note that these distances are chosen to give the best fit to the X-ray data and so avoid the introduction of systematic error. The true internuclear distances are longer and do not vary with temperature ! The apparent variation with temperature is caused by libration. Least-squares cycle 1 Maximum vector length = 511 Memory required = 1919 / 178412 wR2 = 0.1054 before cycle 1 for 1649 data and 141 / 141 parameters GooF = S = 1.089; Restrained GooF = 1.089 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 3.92 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.47625 0.00128 0.002 OSF Mean shift/esd = 0.001 Maximum = -0.008 for z Fe1 Max. shift = 0.000 A for C7 Max. dU = 0.000 for C3 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1919 / 178412 wR2 = 0.1054 before cycle 2 for 1649 data and 141 / 141 parameters GooF = S = 1.089; Restrained GooF = 1.089 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 3.92 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.47625 0.00128 0.001 OSF Mean shift/esd = 0.000 Maximum = -0.003 for z Fe1 Max. shift = 0.000 A for C7 Max. dU = 0.000 for C3 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1919 / 178412 wR2 = 0.1054 before cycle 3 for 1649 data and 141 / 141 parameters GooF = S = 1.089; Restrained GooF = 1.089 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 3.92 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.47625 0.00128 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H4 Max. dU = 0.000 for C4 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1919 / 178412 wR2 = 0.1054 before cycle 4 for 1649 data and 141 / 141 parameters GooF = S = 1.089; Restrained GooF = 1.089 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 3.92 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.47625 0.00128 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C5 Max. dU = 0.000 for C10 Largest correlation matrix elements 0.513 U33 Fe1 / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C1 ** H1 0.2081 0.5865 0.0131 43 0.950 0.000 C1 C2 C5 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C2 ** H2 0.2490 0.2275 0.0968 43 0.950 0.000 C2 C3 C1 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C3 ** H3 0.2092 0.1158 0.2425 43 0.950 0.000 C3 C2 C4 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C4 ** H4 0.1447 0.4082 0.2528 43 0.950 0.000 C4 C5 C3 ** Bond(s) to Fe1 ignored in idealizing H-atoms attached to C5 ** H5 0.1445 0.7018 0.1129 43 0.950 0.000 C5 C4 C1 H9A 0.0578 0.8387 -0.2389 23 0.990 0.000 C9 O3 C10 H9B 0.0325 0.8606 -0.1407 23 0.990 0.000 C9 O3 C10 H11A -0.0306 0.5607 -0.1212 23 0.990 0.000 C11 O4 C10 H11B -0.0419 0.3567 -0.2057 23 0.990 0.000 C11 O4 C10 01src873 in C2/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.20065 0.50792 0.07120 1.00000 0.05458 0.04356 0.02226 0.00245 0.00004 -0.02685 0.04315 0.00872 0.00021 0.00084 0.00038 0.00000 0.00360 0.00339 0.00269 0.00217 0.00256 0.00272 0.00141 H1 0.20809 0.58652 0.01314 1.00000 0.05178 0.00000 0.00000 C2 0.22319 0.30744 0.11747 1.00000 0.02430 0.05231 0.03558 -0.01026 0.00563 -0.00248 0.03839 0.00891 0.00019 0.00085 0.00039 0.00000 0.00271 0.00338 0.00289 0.00232 0.00232 0.00234 0.00122 H2 0.24905 0.22753 0.09683 1.00000 0.04607 0.00000 0.00000 C3 0.20126 0.24568 0.19861 1.00000 0.03180 0.04041 0.02058 -0.00045 -0.00208 -0.00548 0.03350 0.00841 0.00018 0.00081 0.00035 0.00000 0.00271 0.00304 0.00232 0.00207 0.00207 0.00222 0.00114 H3 0.20924 0.11579 0.24253 1.00000 0.04020 0.00000 0.00000 C4 0.16535 0.40845 0.20428 1.00000 0.03216 0.05233 0.02480 -0.01853 0.00741 -0.00288 0.03688 0.00877 0.00019 0.00085 0.00038 0.00000 0.00296 0.00342 0.00261 0.00229 0.00226 0.00239 0.00124 H4 0.14471 0.40820 0.25280 1.00000 0.04425 0.00000 0.00000 C5 0.16510 0.57137 0.12627 1.00000 0.04414 0.03112 0.03725 -0.01008 -0.01393 0.00793 0.04408 0.00915 0.00021 0.00085 0.00041 0.00000 0.00339 0.00303 0.00304 0.00223 0.00260 0.00236 0.00141 H5 0.14454 0.70179 0.11287 1.00000 0.05290 0.00000 0.00000 C6 0.14185 0.15944 -0.08315 1.00000 0.02685 0.02458 0.03050 -0.00204 0.00828 -0.00505 0.02756 0.00860 0.00017 0.00071 0.00038 0.00000 0.00268 0.00259 0.00273 0.00193 0.00220 0.00190 0.00106 C7 0.09549 0.09148 0.06240 1.00000 0.03159 0.02795 0.02115 0.00247 0.00697 0.00507 0.02728 0.00894 0.00019 0.00073 0.00034 0.00000 0.00284 0.00272 0.00243 0.00187 0.00216 0.00212 0.00105 C9 0.04536 0.75453 -0.18536 1.00000 0.03420 0.01901 0.02230 0.00325 0.00223 0.00082 0.02685 0.00799 0.00017 0.00068 0.00032 0.00000 0.00266 0.00247 0.00233 0.00179 0.00205 0.00191 0.00102 H9A 0.05784 0.83875 -0.23893 1.00000 0.03222 0.00000 0.00000 H9B 0.03251 0.86059 -0.14074 1.00000 0.03222 0.00000 0.00000 C10 0.00000 0.60448 -0.25000 0.50000 0.02844 0.02320 0.01808 0.00000 0.00680 0.00000 0.02342 0.00584 0.00000 0.00096 0.00000 0.00000 0.00371 0.00351 0.00317 0.00000 0.00280 0.00000 0.00139 C11 -0.01497 0.46562 -0.16567 1.00000 0.02207 0.03345 0.02032 0.00474 0.00390 0.00412 0.02600 0.00865 0.00016 0.00072 0.00034 0.00000 0.00252 0.00267 0.00231 0.00184 0.00197 0.00193 0.00102 H11A -0.03062 0.56067 -0.12119 1.00000 0.03120 0.00000 0.00000 H11B -0.04193 0.35670 -0.20570 1.00000 0.03120 0.00000 0.00000 B1 0.07946 0.43872 -0.06456 1.00000 0.03465 0.02922 0.01574 -0.00357 0.01156 0.00059 0.02572 0.00999 0.00021 0.00086 0.00038 0.00000 0.00337 0.00304 0.00256 0.00197 0.00241 0.00234 0.00120 Fe1 0.14149 0.27474 0.04208 1.00000 0.02673 0.02886 0.02017 -0.00110 0.00567 0.00051 0.02573 0.00119 0.00002 0.00010 0.00005 0.00000 0.00040 0.00040 0.00035 0.00028 0.00027 0.00029 0.00023 O1 0.14307 0.08919 -0.16679 1.00000 0.04095 0.04329 0.03066 -0.01309 0.01692 -0.01074 0.03702 0.00615 0.00013 0.00053 0.00026 0.00000 0.00215 0.00215 0.00185 0.00155 0.00164 0.00156 0.00083 O2 0.06536 -0.02819 0.07816 1.00000 0.03999 0.03610 0.02619 0.00288 0.01162 -0.00049 0.03389 0.00626 0.00013 0.00052 0.00024 0.00000 0.00208 0.00209 0.00177 0.00137 0.00158 0.00164 0.00079 O3 0.08887 0.63017 -0.11161 1.00000 0.02637 0.03040 0.02126 0.00315 0.00237 -0.00236 0.02731 0.00559 0.00011 0.00047 0.00023 0.00000 0.00180 0.00186 0.00160 0.00124 0.00138 0.00130 0.00073 O4 0.03000 0.35317 -0.09188 1.00000 0.02555 0.03275 0.02448 0.00671 0.00598 -0.00073 0.02812 0.00573 0.00011 0.00049 0.00023 0.00000 0.00181 0.00181 0.00172 0.00123 0.00143 0.00135 0.00073 Final Structure Factor Calculation for 01src873 in C2/c Total number of l.s. parameters = 141 Maximum vector length = 511 Memory required = 1778 / 24017 wR2 = 0.1054 before cycle 5 for 1649 data and 0 / 141 parameters GooF = S = 1.089; Restrained GooF = 1.089 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0283 * P )^2 + 3.92 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0427 for 1224 Fo > 4sig(Fo) and 0.0732 for all 1649 data wR2 = 0.1054, GooF = S = 1.089, Restrained GooF = 1.089 for all data Occupancy sum of asymmetric unit = 15.50 for non-hydrogen and 9.00 for hydrogen atoms Principal mean square atomic displacements U 0.0854 0.0245 0.0195 C1 0.0576 0.0344 0.0232 C2 0.0472 0.0368 0.0165 C3 0.0620 0.0332 0.0154 C4 0.0855 0.0274 0.0193 C5 0.0313 0.0309 0.0205 C6 0.0356 0.0261 0.0202 C7 0.0408 0.0230 0.0167 C9 0.0291 0.0232 0.0180 C10 0.0353 0.0258 0.0170 C11 0.0347 0.0301 0.0123 B1 0.0297 0.0275 0.0200 Fe1 0.0564 0.0327 0.0219 O1 0.0403 0.0368 0.0246 O2 0.0361 0.0269 0.0190 O3 0.0378 0.0258 0.0207 O4 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.017 0.031 0.046 0.061 0.076 0.095 0.121 0.151 0.213 1.000 Number in group 173. 160. 166. 162. 163. 165. 166. 167. 161. 166. GooF 0.855 0.929 1.116 0.998 1.442 1.210 1.050 0.887 1.175 1.113 K 0.979 1.029 0.850 0.957 0.941 0.986 0.986 1.003 1.015 1.004 Resolution(A) 0.84 0.88 0.91 0.95 1.00 1.07 1.15 1.26 1.45 1.82 inf Number in group 170. 160. 166. 166. 168. 162. 165. 162. 164. 166. GooF 0.918 0.995 1.216 1.119 0.927 1.002 1.144 1.015 0.976 1.461 K 0.976 0.985 1.003 0.990 1.009 1.019 1.025 1.030 0.997 0.987 R1 0.173 0.177 0.124 0.088 0.074 0.072 0.062 0.041 0.034 0.032 Recommended weighting scheme: WGHT 0.0258 3.9367 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) -6 6 5 0.00 807.98 8.91 0.075 0.94 1 3 0 2076.60 4980.69 8.44 0.187 2.02 -1 3 1 281.59 1229.42 7.96 0.093 2.00 6 6 1 300.42 1532.50 7.07 0.104 0.98 -5 5 3 0.00 581.39 6.23 0.064 1.16 9 5 0 159.24 457.08 3.25 0.057 1.12 -18 4 10 141.82 564.16 3.12 0.063 0.89 0 4 7 1585.06 1190.37 3.04 0.091 1.14 -22 4 3 287.85 631.30 3.02 0.067 0.95 7 5 5 8004.52 6482.91 2.96 0.213 1.00 5 1 0 17789.24 20713.30 2.92 0.381 3.90 12 4 1 41.31 181.20 2.83 0.036 1.21 -22 4 9 392.64 821.30 2.80 0.076 0.87 -8 2 6 0.00 142.25 2.76 0.032 1.67 12 2 7 35.93 336.84 2.69 0.049 1.08 -26 2 9 -35.95 257.94 2.69 0.043 0.90 16 0 2 1051.02 1593.84 2.68 0.106 1.42 4 0 0 34961.70 41088.85 2.63 0.537 6.34 18 2 1 0.00 154.80 2.52 0.033 1.23 -5 3 5 1468.66 1205.46 2.40 0.092 1.58 -27 1 2 -149.06 221.37 2.35 0.039 0.96 -3 5 2 1221.86 958.44 2.33 0.082 1.19 -12 4 3 1219.26 982.20 2.32 0.083 1.25 12 0 6 633.86 957.12 2.31 0.082 1.26 -7 3 13 -70.47 223.72 2.27 0.040 0.87 -21 5 1 413.77 715.17 2.26 0.071 0.87 -10 4 1 1717.06 1456.10 2.26 0.101 1.32 10 6 3 -143.20 197.77 2.26 0.037 0.89 -19 5 2 256.17 425.00 2.21 0.055 0.92 -27 3 5 719.50 1095.33 2.18 0.088 0.89 16 4 0 894.59 1230.72 2.13 0.093 1.10 -13 1 2 3064.44 2672.35 2.12 0.137 1.95 11 1 1 421.00 630.60 2.11 0.067 2.02 10 4 6 250.45 452.01 2.11 0.056 1.02 -6 0 2 423.17 192.78 2.10 0.037 4.14 -17 5 7 406.43 232.23 2.08 0.040 0.91 22 2 2 1360.21 932.81 2.08 0.081 1.01 15 1 4 3300.30 3776.22 2.08 0.163 1.27 13 1 2 236.83 96.38 2.06 0.026 1.64 -20 4 5 1278.98 1568.55 2.06 0.105 0.99 -9 3 10 567.95 801.07 2.06 0.075 1.07 -21 3 10 1018.64 698.62 2.06 0.070 0.92 3 1 1 253.28 91.31 2.06 0.025 4.29 -9 5 2 240.77 62.62 2.05 0.021 1.13 11 5 1 2259.69 2843.69 2.04 0.141 1.06 -5 3 4 1225.71 1466.34 2.03 0.101 1.69 -17 3 5 7961.24 7029.64 2.02 0.222 1.21 -19 1 9 13485.35 12142.88 2.01 0.292 1.13 -8 6 3 -73.32 83.16 2.01 0.024 0.96 6 0 2 3968.86 3273.36 1.99 0.152 3.02 Bond lengths and angles C1 - Distance Angles C2 1.4029 (0.0070) C5 1.4045 (0.0073) 107.61 (0.43) Fe1 2.0704 (0.0046) 71.22 (0.27) 70.93 (0.28) C1 - C2 C5 C2 - Distance Angles C3 1.3892 (0.0066) C1 1.4029 (0.0070) 108.37 (0.46) Fe1 2.0940 (0.0047) 71.31 (0.27) 69.41 (0.27) C2 - C3 C1 C3 - Distance Angles C2 1.3892 (0.0066) C4 1.3996 (0.0067) 107.99 (0.44) Fe1 2.1095 (0.0043) 70.10 (0.26) 70.33 (0.25) C3 - C2 C4 C4 - Distance Angles C5 1.3971 (0.0072) C3 1.3996 (0.0067) 108.22 (0.44) Fe1 2.1028 (0.0043) 69.95 (0.26) 70.86 (0.25) C4 - C5 C3 C5 - Distance Angles C4 1.3971 (0.0072) C1 1.4045 (0.0073) 107.80 (0.45) Fe1 2.0878 (0.0049) 71.10 (0.28) 69.59 (0.27) C5 - C4 C1 C6 - Distance Angles O1 1.1507 (0.0049) Fe1 1.7342 (0.0046) 177.60 (0.41) C6 - O1 C7 - Distance Angles O2 1.1522 (0.0051) Fe1 1.7428 (0.0050) 178.54 (0.38) C7 - O2 C9 - Distance Angles O3 1.4475 (0.0049) C10 1.5280 (0.0054) 111.44 (0.35) C9 - O3 C10 - Distance Angles C11_$1 1.5133 (0.0052) C11 1.5133 (0.0052) 112.04 (0.52) C9 1.5280 (0.0054) 111.33 (0.23) 107.75 (0.22) C9_$1 1.5280 (0.0054) 107.75 (0.22) 111.33 (0.23) 106.53 (0.48) C10 - C11_$1 C11 C9 C11 - Distance Angles O4 1.4355 (0.0048) C10 1.5133 (0.0052) 111.43 (0.31) C11 - O4 B1 - Distance Angles O4 1.3601 (0.0058) O3 1.3690 (0.0058) 121.19 (0.42) Fe1 2.0299 (0.0052) 120.01 (0.34) 118.73 (0.34) B1 - O4 O3 Fe1 - Distance Angles C6 1.7342 (0.0046) C7 1.7428 (0.0050) 95.11 (0.20) B1 2.0299 (0.0052) 80.77 (0.19) 86.97 (0.20) C1 2.0704 (0.0046) 102.06 (0.20) 161.91 (0.19) 101.25 (0.21) C5 2.0878 (0.0049) 136.46 (0.22) 126.21 (0.22) 87.69 (0.20) 39.48 (0.21) C2 2.0940 (0.0047) 97.97 (0.20) 132.76 (0.20) 139.89 (0.21) 39.37 (0.20) 65.61 (0.20) C4 2.1028 (0.0043) 162.99 (0.20) 96.31 (0.20) 112.36 (0.19) 65.69 (0.20) 38.95 (0.20) 65.04 (0.19) C3 2.1095 (0.0043) 126.44 (0.20) 99.55 (0.19) 150.71 (0.19) 65.59 (0.19) 65.34 (0.19) 38.60 (0.18) 38.81 (0.18) Fe1 - C6 C7 B1 C1 C5 C2 C4 O1 - Distance Angles C6 1.1507 (0.0049) O1 - O2 - Distance Angles C7 1.1522 (0.0051) O2 - O3 - Distance Angles B1 1.3690 (0.0058) C9 1.4475 (0.0049) 120.13 (0.35) O3 - B1 O4 - Distance Angles B1 1.3601 (0.0058) C11 1.4355 (0.0048) 121.68 (0.35) O4 - B1 FMAP and GRID set by program FMAP 2 2 10 GRID -3.571 -2 -1 3.571 2 1 R1 = 0.0716 for 1649 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.47 at 0.0788 0.2251 0.3758 [ 0.92 A from O3 ] Deepest hole -0.41 at 0.3591 0.2190 0.0226 [ 0.81 A from FE1 ] Mean = 0.00, Rms deviation from mean = 0.10 e/A^3, Highest memory used = 2480 / 22342 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0788 0.7749 -0.1242 1.00000 0.05 0.47 0.92 O3 0.98 C9 1.30 H9B 1.43 H9A Q2 1 0.2312 0.7771 0.0387 1.00000 0.05 0.39 1.31 H1 1.94 C1 2.11 H1 2.68 C5 Q3 1 0.1036 0.3611 -0.0286 1.00000 0.05 0.37 0.81 B1 1.23 FE1 1.87 C6 1.87 O4 Q4 1 0.1012 0.4308 0.0643 1.00000 0.05 0.34 1.53 FE1 1.54 B1 1.85 C5 2.00 H5 Q5 1 0.0573 0.8751 -0.2911 1.00000 0.05 0.34 0.69 H9A 1.64 C9 1.97 O2 2.21 H9B Q6 1 0.2278 0.7901 -0.0315 1.00000 0.05 0.33 1.53 H1 1.82 H1 2.40 C1 2.46 C1 Q7 1 0.2541 0.3721 0.1710 1.00000 0.05 0.33 0.97 C2 1.26 H2 1.74 C3 1.77 C1 Q8 1 0.2210 0.8210 -0.0630 1.00000 0.05 0.31 1.82 H1 1.88 H1 2.38 C1 2.40 H3 Q9 1 0.1561 0.5083 0.3423 1.00000 0.05 0.30 1.23 H4 1.94 C4 2.23 O3 2.23 H1 Q10 1 -0.0015 0.8487 -0.1025 1.00000 0.05 0.30 1.17 H9B 1.90 H11A 1.96 C9 2.08 H9A Shortest distances between peaks (including symmetry equivalents) 6 8 0.42 2 6 0.86 2 6 1.20 2 8 1.25 3 4 1.27 6 6 1.29 2 8 1.36 6 8 1.64 2 2 1.65 5 10 1.66 8 8 2.02 1 5 2.09 1 10 2.30 7 8 2.53 3 9 2.60 8 9 2.67 6 9 2.75 1 3 2.78 1 9 2.83 6 7 2.85 2 7 2.93 Time profile in seconds ----------------------- 0.11: 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. 0.11: 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 0.00: Generate idealized H-atoms 0.22: Structure factors and derivatives 0.27: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.11: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.11: Analysis of variance 0.00: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.00: Peaksearch 0.05: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 13:16:01 Total elapsed time: 1.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++