+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2005slh0248 started at 10:31:59 on 21-Jun-2006 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2005slh0248 in P-1 CELL 0.71073 8.1560 14.1030 16.3800 90.940 99.310 100.910 ZERR 2.00 0.0020 0.0040 0.0060 0.020 0.020 0.020 LATT 1 SFAC C H N BR I UNIT 36 30 12 16 10 V = 1823.52 F(000) = 1420.0 Mu = 13.05 mm-1 Cell Wt = 3178.28 Rho = 2.894 MERG 2 OMIT -3.00 55.00 OMIT 1 1 0 OMIT -1 -1 1 OMIT 1 -2 1 EXTI 0.00031 FMAP 2 PLAN 5 SIZE 0.02 0.04 0.46 ACTA BOND $H WGHT 0.04770 10.57820 L.S. 6 TEMP -153.00 FVAR 0.20741 MOLE 1 C1 1 1.084778 0.199757 0.358579 11.00000 0.01892 0.03506 = 0.02901 0.00145 0.01116 0.00634 C2 1 1.011480 0.059431 0.284196 11.00000 0.02591 0.01990 = 0.03010 0.00557 0.01193 0.00656 C3 1 0.920202 0.191769 0.232438 11.00000 0.02193 0.02273 = 0.02731 0.00390 0.01086 0.00536 C4 1 1.168704 0.254430 0.435855 11.00000 0.02289 0.02952 = 0.02479 0.00282 0.00619 0.01014 C5 1 1.243641 0.208069 0.501515 11.00000 0.03711 0.05457 = 0.02253 -0.00073 0.00392 0.02139 AFIX 43 H5 2 1.243393 0.140696 0.498949 11.00000 -1.20000 AFIX 0 C6 1 1.321406 0.268918 0.573442 11.00000 0.04116 0.14894 = 0.02701 0.01878 0.00205 0.03790 AFIX 43 H6 2 1.381652 0.242731 0.619393 11.00000 -1.20000 AFIX 0 C7 1 1.309764 0.366525 0.576896 11.00000 0.03568 0.11372 = 0.05782 -0.04310 0.00248 0.00336 AFIX 43 H7 2 1.359075 0.405876 0.625564 11.00000 -1.20000 AFIX 0 C8 1 1.231526 0.403150 0.513528 11.00000 0.07582 0.05949 = 0.06446 -0.04507 0.01110 -0.00968 AFIX 43 H8 2 1.223548 0.469423 0.516330 11.00000 -1.20000 AFIX 0 C9 1 1.002605 -0.046355 0.278008 11.00000 0.02302 0.02439 = 0.02368 -0.00339 0.00958 0.00924 C10 1 1.077943 -0.095524 0.337690 11.00000 0.02353 0.03647 = 0.03342 -0.00287 0.00204 0.00276 AFIX 43 H10 2 1.146045 -0.061722 0.385796 11.00000 -1.20000 AFIX 0 C11 1 1.057035 -0.195099 0.329581 11.00000 0.04469 0.05099 = 0.05382 0.01888 0.00622 0.02387 AFIX 43 H11 2 1.110990 -0.229877 0.371589 11.00000 -1.20000 AFIX 0 C12 1 0.954671 -0.244122 0.258195 11.00000 0.05854 0.02749 = 0.07173 0.00319 0.01580 0.01238 AFIX 43 H12 2 0.938765 -0.312437 0.251178 11.00000 -1.20000 AFIX 0 C13 1 0.879804 -0.192670 0.200124 11.00000 0.05278 0.02331 = 0.05392 -0.00294 -0.00195 0.00008 AFIX 43 H13 2 0.808914 -0.224806 0.152009 11.00000 -1.20000 AFIX 0 C14 1 0.829115 0.238509 0.166652 11.00000 0.01983 0.02206 = 0.02318 0.00224 0.00175 -0.00265 C15 1 0.756343 0.190036 0.091984 11.00000 0.02580 0.03022 = 0.02654 -0.00250 0.00430 -0.00872 AFIX 43 H15 2 0.759397 0.123777 0.082660 11.00000 -1.20000 AFIX 0 C16 1 0.675632 0.243458 0.028722 11.00000 0.01671 0.13460 = 0.02738 0.00455 0.00226 -0.02128 AFIX 43 H16 2 0.627369 0.213732 -0.024397 11.00000 -1.20000 AFIX 0 C17 1 0.669273 0.340308 0.046705 11.00000 0.03050 0.09868 = 0.09065 0.06622 0.00993 0.01512 AFIX 43 H17 2 0.616057 0.376481 0.005600 11.00000 -1.20000 AFIX 0 C18 1 0.735934 0.380468 0.119347 11.00000 0.04879 0.05680 = 0.09962 0.04947 0.02491 0.03057 AFIX 43 H18 2 0.726802 0.445348 0.130776 11.00000 -1.20000 AFIX 0 N1 3 0.997540 0.246639 0.300674 11.00000 0.02378 0.02282 = 0.02078 -0.00176 0.00175 0.00252 N2 3 1.099523 0.107202 0.351948 11.00000 0.02321 0.02733 = 0.02240 0.00027 0.00462 0.00562 N3 3 0.917985 0.097270 0.220901 11.00000 0.02417 0.02186 = 0.02733 -0.00542 0.00588 0.00110 N4 3 1.161151 0.348692 0.443580 11.00000 0.04274 0.04250 = 0.03872 -0.00374 0.01078 0.01766 AFIX 3 H4 2 1.108641 0.375662 0.401670 11.00000 -1.20000 AFIX 0 N5 3 0.905219 -0.094692 0.210028 11.00000 0.03415 0.03130 = 0.03946 0.00171 0.00305 0.01147 AFIX 3 H5A 2 0.856789 -0.061972 0.171008 11.00000 -1.20000 AFIX 0 N6 3 0.816457 0.334356 0.178348 11.00000 0.03927 0.02654 = 0.05621 -0.00324 0.00811 -0.00038 AFIX 3 H6A 2 0.862887 0.365356 0.226008 11.00000 -1.20000 AFIX 0 MOLE 2 BR1 4 0.555353 0.165481 0.779341 11.00000 0.04142 0.04584 = 0.03529 0.01039 0.00565 0.01096 I1 5 0.584583 -0.015519 0.791263 11.00000 0.03121 0.05658 = 0.03207 0.00765 0.00631 0.00494 MOLE 3 BR8 4 0.783760 0.038829 0.433944 11.00000 0.02915 0.05226 = 0.04342 0.01066 0.01596 0.00993 I6 5 0.500000 0.000000 0.500000 10.50000 0.02359 0.03397 = 0.03451 0.00553 0.00466 0.00973 MOLE 4 BR2 4 0.360568 0.220083 0.191314 11.00000 0.03588 0.06741 = 0.03545 0.00912 0.00675 0.00386 BR3 4 0.738756 0.333170 0.494854 11.00000 0.05001 0.06099 = 0.03804 0.00708 0.00247 0.01079 I2 5 0.561382 0.283481 0.349704 11.00000 0.03136 0.04882 = 0.03761 0.00959 0.01139 0.00953 MOLE 5 BR5 4 -0.016841 0.511495 0.330335 11.00000 0.04456 0.03002 = 0.04009 0.00415 0.00784 0.01228 BR6 4 0.534879 0.585549 0.178430 11.00000 0.03708 0.05622 = 0.05765 0.00040 0.00814 0.00678 I4 5 0.267145 0.546165 0.253680 11.00000 0.03418 0.03119 = 0.03570 -0.00170 -0.00346 0.00738 MOLE 6 BR4 4 0.993591 0.608349 0.080229 11.00000 0.04746 0.03462 = 0.04151 0.00041 0.02047 0.00563 I3 5 0.813087 0.675152 -0.044751 11.00000 0.03543 0.04917 = 0.04587 -0.00540 0.01018 0.00118 MOLE 7 BR7 4 0.684432 0.936585 0.031192 11.00000 0.03334 0.04661 = 0.03171 0.00037 0.00424 0.00547 I5 5 1.000000 1.000000 0.000000 10.50000 0.03769 0.03387 = 0.02581 -0.00099 0.00248 0.01138 HKLF 4 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00 Covalent radii and connectivity table for 2005slh0248 in P-1 C 0.770 H 0.320 N 0.700 BR 1.140 I 1.330 C1 - N2 N1 C4 C2 - N2 N3 C9 C3 - N3 N1 C14 C4 - N4 C5 C1 C5 - C4 C6 C6 - C7 C5 C7 - C8 C6 C8 - C7 N4 C9 - C10 N5 C2 C10 - C9 C11 C11 - C10 C12 C12 - C13 C11 C13 - C12 N5 C14 - C15 N6 C3 C15 - C14 C16 C16 - C17 C15 C17 - C18 C16 C18 - C17 N6 N1 - C3 C1 N2 - C2 C1 N3 - C3 C2 N4 - C4 C8 N5 - C9 C13 N6 - C18 C14 Br1 - I1 I1 - Br1 Br8 - I6 I6 - Br8_$1 Br8 Br2 - I2 Br3 - I2 I2 - Br3 Br2 Br5 - I4 Br6 - I4 I4 - Br6 Br5 Br4 - I3 I3 - Br4 Br7 - I5 I5 - Br7_$2 Br7 Operators for generating equivalent atoms: $1 -x+1, -y, -z+1 $2 -x+2, -y+2, -z 36794 Reflections read, of which 15 rejected -10 =< h =< 10, -18 =< k =< 18, -21 =< l =< 21, Max. 2-theta = 55.00 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -8 5 1 142.18 7.88 7 103.58 -7 5 4 118.87 4.00 6 20.56 2 Inconsistent equivalents 8316 Unique reflections, of which 0 suppressed R(int) = 0.0851 R(sigma) = 0.0919 Friedel opposites merged Maximum memory for data reduction = 2670 / 83254 Special position constraints for I6 x = 0.5000 y = 0.0000 z = 0.5000 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for I5 x = 1.0000 y = 1.0000 z = 0.0000 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 = 3545 / 427420 wR2 = 0.1239 before cycle 1 for 8316 data and 338 / 338 parameters GooF = S = 1.015; Restrained GooF = 1.015 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0477 * P )^2 + 10.58 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20741 0.00035 0.012 OSF 2 0.00031 0.00008 -0.037 EXTI Mean shift/esd = 0.002 Maximum = -0.037 for EXTI Max. shift = 0.000 A for H18 Max. dU = 0.000 for C16 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3545 / 427420 wR2 = 0.1239 before cycle 2 for 8316 data and 338 / 338 parameters GooF = S = 1.015; Restrained GooF = 1.015 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0477 * P )^2 + 10.58 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20741 0.00035 -0.002 OSF 2 0.00031 0.00008 -0.012 EXTI Mean shift/esd = 0.001 Maximum = -0.012 for EXTI Max. shift = 0.000 A for C13 Max. dU = 0.000 for C11 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3545 / 427420 wR2 = 0.1239 before cycle 3 for 8316 data and 338 / 338 parameters GooF = S = 1.015; Restrained GooF = 1.015 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0477 * P )^2 + 10.58 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20741 0.00035 0.001 OSF 2 0.00031 0.00008 0.001 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for C15 Max. dU = 0.000 for N6 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3545 / 427420 wR2 = 0.1239 before cycle 4 for 8316 data and 338 / 338 parameters GooF = S = 1.015; Restrained GooF = 1.015 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0477 * P )^2 + 10.58 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20741 0.00035 0.001 OSF 2 0.00031 0.00008 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for C8 Max. dU = 0.000 for C3 Least-squares cycle 5 Maximum vector length = 511 Memory required = 3545 / 427420 wR2 = 0.1239 before cycle 5 for 8316 data and 338 / 338 parameters GooF = S = 1.015; Restrained GooF = 1.015 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0477 * P )^2 + 10.58 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20741 0.00035 -0.001 OSF 2 0.00031 0.00008 -0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for C17 Max. dU = 0.000 for C17 Least-squares cycle 6 Maximum vector length = 511 Memory required = 3545 / 427420 wR2 = 0.1239 before cycle 6 for 8316 data and 338 / 338 parameters GooF = S = 1.015; Restrained GooF = 1.015 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0477 * P )^2 + 10.58 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20741 0.00035 0.000 OSF 2 0.00031 0.00008 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for y I4 Max. shift = 0.000 A for H18 Max. dU = 0.000 for C11 Largest correlation matrix elements 0.572 EXTI / OSF 0.516 U23 C17 / U22 C17 Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H5 1.2434 0.1407 0.4989 43 0.950 0.000 C5 C4 C6 H6 1.3817 0.2427 0.6194 43 0.950 0.000 C6 C7 C5 H7 1.3591 0.4059 0.6256 43 0.950 0.000 C7 C8 C6 H8 1.2235 0.4694 0.5163 43 0.950 0.000 C8 C7 N4 H10 1.1460 -0.0617 0.3858 43 0.950 0.000 C10 C9 C11 H11 1.1110 -0.2299 0.3716 43 0.950 0.000 C11 C10 C12 H12 0.9388 -0.3124 0.2512 43 0.950 0.000 C12 C13 C11 H13 0.8089 -0.2248 0.1520 43 0.950 0.000 C13 C12 N5 H15 0.7594 0.1238 0.0827 43 0.950 0.000 C15 C14 C16 H16 0.6274 0.2137 -0.0244 43 0.950 0.000 C16 C17 C15 H17 0.6161 0.3765 0.0056 43 0.950 0.000 C17 C18 C16 H18 0.7268 0.4453 0.1308 43 0.950 0.000 C18 C17 N6 2005slh0248 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 1.08478 0.19976 0.35858 1.00000 0.01892 0.03506 0.02902 0.00144 0.01116 0.00634 0.02671 0.01929 0.00110 0.00072 0.00060 0.00000 0.00462 0.00604 0.00578 0.00466 0.00412 0.00417 0.00223 C2 1.01148 0.05943 0.28420 1.00000 0.02591 0.01990 0.03010 0.00557 0.01193 0.00656 0.02416 0.01943 0.00113 0.00066 0.00061 0.00000 0.00481 0.00499 0.00578 0.00433 0.00430 0.00397 0.00211 C3 0.92020 0.19177 0.23244 1.00000 0.02193 0.02273 0.02731 0.00390 0.01086 0.00536 0.02306 0.01866 0.00109 0.00066 0.00058 0.00000 0.00463 0.00523 0.00562 0.00431 0.00407 0.00388 0.00209 C4 1.16870 0.25443 0.43586 1.00000 0.02289 0.02952 0.02479 0.00282 0.00619 0.01014 0.02480 0.01887 0.00110 0.00070 0.00059 0.00000 0.00475 0.00568 0.00553 0.00440 0.00408 0.00408 0.00214 C5 1.24364 0.20807 0.50151 1.00000 0.03711 0.05457 0.02253 -0.00073 0.00392 0.02139 0.03657 0.02182 0.00125 0.00087 0.00062 0.00000 0.00584 0.00735 0.00590 0.00523 0.00462 0.00530 0.00261 H5 1.24339 0.14070 0.49895 1.00000 0.04388 0.00000 0.00000 C6 1.32141 0.26892 0.57344 1.00000 0.04116 0.14894 0.02701 0.01878 0.00205 0.03790 0.07004 0.03169 0.00154 0.00142 0.00078 0.00000 0.00736 0.01654 0.00743 0.00882 0.00570 0.00879 0.00483 H6 1.38165 0.24273 0.61939 1.00000 0.08405 0.00000 0.00000 C7 1.30976 0.36653 0.57690 1.00000 0.03568 0.11372 0.05782 -0.04310 0.00248 0.00336 0.07170 0.02734 0.00161 0.00137 0.00101 0.00000 0.00722 0.01467 0.01039 0.00990 0.00672 0.00804 0.00486 H7 1.35908 0.40588 0.62556 1.00000 0.08604 0.00000 0.00000 C8 1.23153 0.40315 0.51353 1.00000 0.07582 0.05949 0.06446 -0.04507 0.01110 -0.00967 0.07025 0.02597 0.00188 0.00111 0.00098 0.00000 0.00981 0.00945 0.01060 0.00854 0.00845 0.00782 0.00448 H8 1.22355 0.46942 0.51633 1.00000 0.08430 0.00000 0.00000 C9 1.00261 -0.04635 0.27801 1.00000 0.02302 0.02439 0.02368 -0.00339 0.00958 0.00924 0.02249 0.01840 0.00109 0.00066 0.00058 0.00000 0.00470 0.00516 0.00535 0.00426 0.00407 0.00400 0.00206 C10 1.07794 -0.09552 0.33769 1.00000 0.02353 0.03647 0.03342 -0.00287 0.00204 0.00276 0.03191 0.02008 0.00116 0.00076 0.00066 0.00000 0.00501 0.00638 0.00625 0.00502 0.00440 0.00446 0.00241 H10 1.14604 -0.06172 0.38580 1.00000 0.03829 0.00000 0.00000 C11 1.05703 -0.19510 0.32958 1.00000 0.04469 0.05099 0.05381 0.01888 0.00622 0.02387 0.04794 0.02571 0.00143 0.00089 0.00079 0.00000 0.00672 0.00809 0.00841 0.00660 0.00602 0.00596 0.00315 H11 1.11099 -0.22988 0.37159 1.00000 0.05753 0.00000 0.00000 C12 0.95467 -0.24412 0.25820 1.00000 0.05854 0.02749 0.07173 0.00319 0.01580 0.01238 0.05149 0.02615 0.00155 0.00086 0.00086 0.00000 0.00771 0.00645 0.00973 0.00648 0.00707 0.00578 0.00329 H12 0.93877 -0.31244 0.25118 1.00000 0.06179 0.00000 0.00000 C13 0.87980 -0.19267 0.20012 1.00000 0.05278 0.02332 0.05392 -0.00294 -0.00195 0.00008 0.04560 0.02272 0.00145 0.00078 0.00079 0.00000 0.00707 0.00611 0.00808 0.00559 0.00598 0.00523 0.00298 H13 0.80891 -0.22481 0.15201 1.00000 0.05472 0.00000 0.00000 C14 0.82912 0.23851 0.16665 1.00000 0.01983 0.02206 0.02319 0.00224 0.00175 -0.00265 0.02278 0.01750 0.00107 0.00066 0.00057 0.00000 0.00454 0.00519 0.00535 0.00412 0.00385 0.00379 0.00206 C15 0.75634 0.19004 0.09198 1.00000 0.02580 0.03022 0.02654 -0.00250 0.00430 -0.00872 0.02946 0.01838 0.00114 0.00074 0.00061 0.00000 0.00500 0.00577 0.00586 0.00461 0.00431 0.00422 0.00232 H15 0.75940 0.12378 0.08266 1.00000 0.03535 0.00000 0.00000 C16 0.67563 0.24346 0.02872 1.00000 0.01671 0.13461 0.02738 0.00455 0.00226 -0.02128 0.06451 0.02580 0.00130 0.00135 0.00075 0.00000 0.00556 0.01503 0.00697 0.00817 0.00475 0.00715 0.00470 H16 0.62737 0.21373 -0.02440 1.00000 0.07741 0.00000 0.00000 C17 0.66927 0.34031 0.04671 1.00000 0.03050 0.09868 0.09065 0.06622 0.00993 0.01512 0.07227 0.03882 0.00156 0.00135 0.00116 0.00000 0.00695 0.01376 0.01328 0.01135 0.00760 0.00773 0.00523 H17 0.61606 0.37648 0.00560 1.00000 0.08672 0.00000 0.00000 C18 0.73593 0.38047 0.11935 1.00000 0.04879 0.05680 0.09962 0.04947 0.02491 0.03057 0.06378 0.03588 0.00164 0.00106 0.00111 0.00000 0.00783 0.00899 0.01291 0.00931 0.00834 0.00699 0.00430 H18 0.72680 0.44535 0.13078 1.00000 0.07654 0.00000 0.00000 N1 0.99754 0.24664 0.30067 1.00000 0.02378 0.02282 0.02079 -0.00176 0.00175 0.00252 0.02299 0.01454 0.00090 0.00054 0.00047 0.00000 0.00395 0.00432 0.00438 0.00352 0.00331 0.00331 0.00172 N2 1.09952 0.10720 0.35195 1.00000 0.02321 0.02733 0.02241 0.00027 0.00462 0.00562 0.02414 0.01517 0.00090 0.00056 0.00048 0.00000 0.00399 0.00467 0.00457 0.00369 0.00337 0.00343 0.00177 N3 0.91799 0.09727 0.22090 1.00000 0.02417 0.02186 0.02733 -0.00542 0.00588 0.00110 0.02480 0.01468 0.00091 0.00055 0.00049 0.00000 0.00403 0.00440 0.00469 0.00357 0.00346 0.00332 0.00178 N4 1.16115 0.34869 0.44358 1.00000 0.04274 0.04250 0.03872 -0.00374 0.01078 0.01766 0.03969 0.01813 0.00109 0.00066 0.00058 0.00000 0.00524 0.00577 0.00576 0.00460 0.00434 0.00439 0.00225 H4 1.10864 0.37566 0.40167 1.00000 0.04763 0.00000 0.00000 N5 0.90522 -0.09469 0.21003 1.00000 0.03415 0.03130 0.03946 0.00171 0.00304 0.01147 0.03465 0.01684 0.00100 0.00061 0.00055 0.00000 0.00473 0.00513 0.00564 0.00423 0.00410 0.00388 0.00209 H5A 0.85679 -0.06197 0.17101 1.00000 0.04158 0.00000 0.00000 N6 0.81646 0.33436 0.17835 1.00000 0.03927 0.02654 0.05621 -0.00324 0.00811 -0.00038 0.04163 0.01814 0.00109 0.00062 0.00063 0.00000 0.00508 0.00512 0.00659 0.00463 0.00462 0.00411 0.00234 H6A 0.86289 0.36536 0.22601 1.00000 0.04995 0.00000 0.00000 Br1 0.55535 0.16548 0.77934 1.00000 0.04142 0.04584 0.03529 0.01039 0.00565 0.01096 0.04052 0.00232 0.00014 0.00008 0.00007 0.00000 0.00061 0.00069 0.00065 0.00053 0.00049 0.00051 0.00028 I1 0.58458 -0.01552 0.79126 1.00000 0.03121 0.05658 0.03207 0.00765 0.00631 0.00495 0.04026 0.00146 0.00008 0.00006 0.00004 0.00000 0.00037 0.00050 0.00042 0.00035 0.00030 0.00033 0.00020 Br8 0.78376 0.03883 0.43394 1.00000 0.02915 0.05226 0.04342 0.01066 0.01596 0.00993 0.04013 0.00235 0.00013 0.00009 0.00007 0.00000 0.00054 0.00071 0.00069 0.00055 0.00048 0.00049 0.00028 I6 0.50000 0.00000 0.50000 0.50000 0.02359 0.03397 0.03451 0.00553 0.00466 0.00973 0.03012 0.00000 0.00000 0.00000 0.00000 0.00000 0.00044 0.00054 0.00056 0.00043 0.00038 0.00038 0.00023 Br2 0.36057 0.22008 0.19131 1.00000 0.03588 0.06741 0.03545 0.00912 0.00675 0.00386 0.04691 0.00240 0.00014 0.00010 0.00007 0.00000 0.00060 0.00085 0.00068 0.00059 0.00049 0.00056 0.00031 Br3 0.73876 0.33317 0.49485 1.00000 0.05001 0.06099 0.03804 0.00708 0.00247 0.01079 0.05019 0.00252 0.00015 0.00010 0.00008 0.00000 0.00070 0.00084 0.00071 0.00061 0.00055 0.00060 0.00033 I2 0.56138 0.28348 0.34970 1.00000 0.03136 0.04882 0.03761 0.00959 0.01139 0.00953 0.03831 0.00148 0.00008 0.00005 0.00005 0.00000 0.00036 0.00047 0.00043 0.00034 0.00030 0.00031 0.00020 Br5 -0.01684 0.51149 0.33033 1.00000 0.04456 0.03003 0.04009 0.00415 0.00784 0.01228 0.03745 0.00222 0.00013 0.00008 0.00007 0.00000 0.00062 0.00059 0.00066 0.00049 0.00050 0.00048 0.00027 Br6 0.53488 0.58555 0.17843 1.00000 0.03708 0.05622 0.05765 0.00040 0.00814 0.00678 0.05063 0.00250 0.00014 0.00010 0.00008 0.00000 0.00062 0.00081 0.00083 0.00064 0.00056 0.00055 0.00033 I4 0.26714 0.54617 0.25368 1.00000 0.03418 0.03119 0.03570 -0.00170 -0.00346 0.00738 0.03465 0.00132 0.00008 0.00005 0.00004 0.00000 0.00036 0.00039 0.00042 0.00031 0.00030 0.00029 0.00019 Br4 0.99359 0.60835 0.08023 1.00000 0.04746 0.03462 0.04151 0.00041 0.02047 0.00563 0.04006 0.00231 0.00014 0.00008 0.00007 0.00000 0.00064 0.00062 0.00068 0.00051 0.00052 0.00050 0.00028 I3 0.81309 0.67515 -0.04475 1.00000 0.03543 0.04917 0.04587 -0.00540 0.01018 0.00118 0.04413 0.00148 0.00009 0.00006 0.00005 0.00000 0.00039 0.00049 0.00049 0.00038 0.00033 0.00033 0.00022 Br7 0.68443 0.93658 0.03119 1.00000 0.03334 0.04661 0.03171 0.00037 0.00424 0.00547 0.03768 0.00213 0.00013 0.00008 0.00007 0.00000 0.00056 0.00069 0.00062 0.00051 0.00046 0.00048 0.00027 I5 1.00000 1.00000 0.00000 0.50000 0.03769 0.03387 0.02581 -0.00099 0.00248 0.01138 0.03222 0.00000 0.00000 0.00000 0.00000 0.00000 0.00052 0.00055 0.00053 0.00042 0.00040 0.00042 0.00023 Final Structure Factor Calculation for 2005slh0248 in P-1 Total number of l.s. parameters = 338 Maximum vector length = 511 Memory required = 3207 / 24017 wR2 = 0.1239 before cycle 7 for 8316 data and 0 / 338 parameters GooF = S = 1.015; Restrained GooF = 1.015 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0477 * P )^2 + 10.58 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0517 for 4961 Fo > 4sig(Fo) and 0.1154 for all 8316 data wR2 = 0.1239, GooF = S = 1.015, Restrained GooF = 1.015 for all data Occupancy sum of asymmetric unit = 37.00 for non-hydrogen and 15.00 for hydrogen atoms Principal mean square atomic displacements U 0.0351 0.0317 0.0133 C1 0.0350 0.0195 0.0180 C2 0.0312 0.0220 0.0160 C3 0.0317 0.0243 0.0184 C4 0.0598 0.0276 0.0222 C5 0.1504 0.0386 0.0211 C6 0.1442 0.0403 0.0306 C7 0.1202 0.0746 0.0159 C8 0.0290 0.0276 0.0109 C9 0.0401 0.0328 0.0228 C10 0.0685 0.0508 0.0245 C11 0.0727 0.0560 0.0258 C12 0.0671 0.0477 0.0220 C13 0.0307 0.0224 0.0152 C14 0.0459 0.0266 0.0159 C15 0.1540 0.0274 0.0121 C16 0.1574 0.0326 0.0268 C17 0.1270 0.0449 0.0195 C18 0.0259 0.0247 0.0184 N1 0.0276 0.0235 0.0213 N2 0.0335 0.0232 0.0177 N3 0.0511 0.0430 0.0250 N4 0.0420 0.0359 0.0261 N5 0.0574 0.0430 0.0245 N6 0.0501 0.0416 0.0298 Br1 0.0593 0.0321 0.0293 I1 0.0571 0.0412 0.0221 Br8 0.0379 0.0313 0.0211 I6 0.0717 0.0363 0.0327 Br2 0.0624 0.0526 0.0356 Br3 0.0522 0.0358 0.0269 I2 0.0454 0.0399 0.0270 Br5 0.0596 0.0553 0.0369 Br6 0.0464 0.0306 0.0269 I4 0.0572 0.0345 0.0284 Br4 0.0590 0.0402 0.0332 I3 0.0477 0.0342 0.0311 Br7 0.0415 0.0300 0.0252 I5 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.013 0.026 0.039 0.054 0.070 0.090 0.118 0.157 0.229 1.000 Number in group 837. 837. 820. 867. 795. 838. 836. 822. 827. 837. GooF 0.903 0.917 0.979 0.989 1.029 1.115 1.086 1.109 1.007 0.992 K 3.480 1.435 0.983 1.069 0.986 0.957 0.974 0.997 1.012 1.010 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.64 inf Number in group 865. 819. 830. 816. 828. 835. 830. 835. 827. 831. GooF 0.950 0.931 0.995 0.938 0.969 0.981 0.907 0.848 0.891 1.556 K 1.035 0.980 0.997 0.972 0.988 1.043 1.023 1.027 1.017 0.995 R1 0.365 0.295 0.233 0.181 0.140 0.104 0.068 0.044 0.034 0.037 Recommended weighting scheme: WGHT 0.0477 10.5795 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) 0 -2 3 2732.62 4916.41 7.05 0.146 4.35 -1 -2 5 3029.00 1478.79 6.83 0.080 2.86 -1 -3 3 9780.57 6465.49 6.66 0.167 3.22 1 -1 1 11858.77 18533.36 6.26 0.283 6.49 1 -1 3 5452.87 8389.87 6.15 0.190 4.12 2 -1 1 1006.27 1894.25 5.62 0.090 3.75 2 -2 3 617.94 183.56 5.46 0.028 2.90 -3 2 1 2979.04 4667.31 5.45 0.142 2.67 -2 -2 5 3373.29 2113.90 5.28 0.096 2.47 -1 0 4 1812.94 995.67 5.24 0.066 3.87 -4 2 2 1650.72 2606.62 4.82 0.106 2.02 0 2 5 2315.81 3428.30 4.50 0.122 2.87 -2 7 3 79.53 740.68 4.49 0.057 1.83 -1 -3 2 1751.36 2656.51 4.42 0.107 3.51 -1 0 2 34928.25 55749.61 4.31 0.491 6.19 0 -5 2 5372.97 7289.14 4.22 0.177 2.66 1 -4 2 16883.29 13227.31 4.16 0.239 3.12 -1 -2 1 12339.48 9666.38 4.14 0.204 4.75 -1 -2 4 2714.31 3846.66 4.12 0.129 3.31 -1 0 5 10271.19 7949.52 4.11 0.185 3.18 -7 -3 11 3600.91 5296.24 4.02 0.151 0.93 3 -3 1 1145.69 1801.17 4.00 0.088 2.43 3 0 0 2247.13 1497.33 3.98 0.080 2.63 1 -1 4 5276.18 3936.04 3.87 0.130 3.37 -3 4 1 4845.96 6369.55 3.80 0.166 2.34 1 2 2 9010.33 11426.42 3.79 0.222 3.88 -2 -3 4 10848.96 13643.91 3.73 0.243 2.44 -3 2 0 632.01 1086.74 3.69 0.069 2.64 -1 -1 3 5680.64 4364.57 3.69 0.137 4.47 -1 -4 4 4638.97 6077.89 3.68 0.162 2.52 -5 2 1 156.39 519.97 3.62 0.047 1.63 1 3 0 91.46 385.13 3.56 0.041 3.68 7 10 2 2729.96 298.02 3.54 0.036 0.79 1 2 0 237.30 11.70 3.51 0.007 4.76 2 2 15 17.81 2064.03 3.50 0.094 0.97 3 -1 6 1112.08 1750.30 3.48 0.087 1.76 -2 4 0 12882.81 15868.15 3.46 0.262 2.90 0 1 16 -275.91 373.56 3.42 0.040 1.00 -2 3 1 30134.39 24906.38 3.40 0.328 3.34 -4 -8 9 3965.92 2559.71 3.39 0.105 1.06 -2 3 2 16528.58 20097.20 3.36 0.295 3.21 -4 -2 17 786.22 1955.50 3.32 0.092 0.91 2 -4 1 2306.89 3389.36 3.29 0.121 2.81 2 3 3 20631.76 17208.52 3.26 0.273 2.31 -5 5 5 406.51 28.92 3.26 0.011 1.44 0 1 6 292.72 642.17 3.24 0.053 2.62 -2 8 5 2314.59 1512.02 3.23 0.081 1.53 -1 1 3 11403.86 9380.78 3.21 0.201 4.68 1 -13 11 3345.77 5168.80 3.19 0.149 0.88 5 8 3 1966.14 3115.61 3.14 0.116 1.02 Bond lengths and angles C1 - Distance Angles N2 1.3376 (0.0121) N1 1.3503 (0.0121) 125.53 (0.88) C4 1.4674 (0.0134) 117.10 (0.85) 117.36 (0.84) C1 - N2 N1 C2 - Distance Angles N2 1.3174 (0.0120) N3 1.3629 (0.0122) 125.98 (0.84) C9 1.4809 (0.0128) 117.62 (0.84) 116.26 (0.84) C2 - N2 N3 C3 - Distance Angles N3 1.3393 (0.0116) N1 1.3434 (0.0117) 125.42 (0.85) C14 1.4482 (0.0130) 117.44 (0.84) 117.12 (0.80) C3 - N3 N1 C4 - Distance Angles N4 1.3472 (0.0127) C5 1.3854 (0.0136) 120.81 (0.94) C1 1.4674 (0.0134) 118.69 (0.87) 120.34 (0.91) C4 - N4 C5 C5 - Distance Angles C4 1.3854 (0.0136) C6 1.4303 (0.0183) 115.19 (1.13) H5 0.9500 122.40 122.40 C5 - C4 C6 C6 - Distance Angles C7 1.3985 (0.0219) C5 1.4303 (0.0182) 120.75 (1.20) H6 0.9500 119.62 119.62 C6 - C7 C5 C7 - Distance Angles C8 1.2959 (0.0217) C6 1.3985 (0.0219) 119.82 (1.34) H7 0.9500 120.09 120.09 C7 - C8 C6 C8 - Distance Angles C7 1.2959 (0.0217) N4 1.3504 (0.0153) 121.11 (1.48) H8 0.9500 119.45 119.45 C8 - C7 N4 C9 - Distance Angles C10 1.3429 (0.0136) N5 1.3489 (0.0121) 119.59 (0.88) C2 1.4809 (0.0128) 123.56 (0.89) 116.76 (0.84) C9 - C10 N5 C10 - Distance Angles C9 1.3429 (0.0136) C11 1.3837 (0.0153) 120.44 (1.00) H10 0.9500 119.78 119.78 C10 - C9 C11 C11 - Distance Angles C10 1.3837 (0.0153) C12 1.4076 (0.0170) 119.05 (1.05) H11 0.9500 120.48 120.48 C11 - C10 C12 C12 - Distance Angles C13 1.3441 (0.0165) C11 1.4076 (0.0170) 118.90 (1.09) H12 0.9500 120.55 120.55 C12 - C13 C11 C13 - Distance Angles C12 1.3441 (0.0165) N5 1.3609 (0.0132) 120.22 (1.11) H13 0.9500 119.89 119.89 C13 - C12 N5 C14 - Distance Angles C15 1.3783 (0.0131) N6 1.3875 (0.0124) 119.14 (0.90) C3 1.4482 (0.0130) 121.30 (0.88) 119.55 (0.85) C14 - C15 N6 C15 - Distance Angles C14 1.3783 (0.0131) C16 1.4378 (0.0177) 117.54 (1.06) H15 0.9500 121.23 121.23 C15 - C14 C16 C16 - Distance Angles C17 1.4049 (0.0213) C15 1.4378 (0.0177) 118.95 (1.18) H16 0.9500 120.52 120.52 C16 - C17 C15 C17 - Distance Angles C18 1.2978 (0.0213) C16 1.4049 (0.0213) 120.14 (1.31) H17 0.9500 119.93 119.93 C17 - C18 C16 C18 - Distance Angles C17 1.2978 (0.0213) N6 1.3286 (0.0159) 122.54 (1.42) H18 0.9500 118.73 118.73 C18 - C17 N6 N1 - Distance Angles C3 1.3434 (0.0117) C1 1.3503 (0.0121) 114.31 (0.78) N1 - C3 N2 - Distance Angles C2 1.3174 (0.0120) C1 1.3376 (0.0121) 114.67 (0.81) N2 - C2 N3 - Distance Angles C3 1.3393 (0.0116) C2 1.3629 (0.0122) 113.90 (0.79) N3 - C3 N4 - Distance Angles C4 1.3472 (0.0127) C8 1.3504 (0.0153) 122.15 (1.16) H4 0.8800 118.93 118.92 N4 - C4 C8 N5 - Distance Angles C9 1.3489 (0.0121) C13 1.3609 (0.0132) 121.81 (0.92) H5A 0.8800 119.10 119.09 N5 - C9 C13 N6 - Distance Angles C18 1.3286 (0.0159) C14 1.3875 (0.0124) 121.60 (1.13) H6A 0.8800 119.20 119.20 N6 - C18 C14 Br1 - Distance Angles I1 2.6158 (0.0016) Br1 - I1 - Distance Angles Br1 2.6158 (0.0016) I1 - Br8 - Distance Angles I6 2.6789 (0.0012) Br8 - I6 - Distance Angles Br8_$1 2.6789 (0.0012) Br8 2.6789 (0.0012) 180.00 I6 - Br8_$1 Br2 - Distance Angles I2 2.8649 (0.0017) Br2 - Br3 - Distance Angles I2 2.5856 (0.0017) Br3 - I2 - Distance Angles Br3 2.5856 (0.0017) Br2 2.8649 (0.0017) 177.49 (0.05) I2 - Br3 Br5 - Distance Angles I4 2.7772 (0.0015) Br5 - Br6 - Distance Angles I4 2.6515 (0.0015) Br6 - I4 - Distance Angles Br6 2.6515 (0.0015) Br5 2.7772 (0.0015) 177.79 (0.05) I4 - Br6 Br4 - Distance Angles I3 2.6190 (0.0016) Br4 - I3 - Distance Angles Br4 2.6190 (0.0016) I3 - Br7 - Distance Angles I5 2.6934 (0.0012) Br7 - I5 - Distance Angles Br7_$2 2.6934 (0.0012) Br7 2.6934 (0.0012) 180.00 I5 - Br7_$2 FMAP and GRID set by program FMAP 2 1 38 GRID -2.857 -2 -1 2.857 2 1 R1 = 0.1125 for 8316 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 2.02 at 0.9312 0.5991 0.0437 [ 0.71 A from BR4 ] Deepest hole -2.05 at 0.1430 0.3544 0.0226 [ 0.67 A from I3 ] Mean = 0.00, Rms deviation from mean = 0.24 e/A^3, Highest memory used = 3491 / 55022 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.9312 0.5991 0.0437 1.00000 0.05 2.02 0.71 BR4 2.04 I3 3.00 H18 3.42 H13 Q2 1 0.4746 0.0546 0.7180 1.00000 0.05 2.01 1.80 BR1 1.80 I1 3.09 BR8 3.28 H6 Q3 1 0.5169 0.1400 0.7491 1.00000 0.05 1.81 0.61 BR1 2.44 I1 2.79 H6 3.50 H5A Q4 1 1.0222 0.5964 0.1012 1.00000 0.05 1.68 0.44 BR4 2.99 H12 3.01 H18 3.06 I3 Q5 1 0.5901 0.1481 0.8009 1.00000 0.05 1.67 0.51 BR1 2.30 I1 2.94 H16 3.59 H6 Shortest distances between peaks (including symmetry equivalents) 3 5 0.95 1 4 1.11 2 3 1.26 2 5 1.88 Time profile in seconds ----------------------- 0.03: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: 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 0.01: Analyse other restraints etc. 1.86: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.01: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 3.30: Structure factors and derivatives 10.93: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.56: Solve l.s. equations 0.00: Generate HTAB table 0.04: Other dependent quantities, CIF, tables 0.33: Analysis of variance 0.08: Merge reflections for Fourier and .fcf 0.13: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2005slh0248 finished at 10:32:17 Total CPU time: 17.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++