+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 04skc0011p-18 started at 14:46:08 on 12-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 04skc0011p-18 in P-1 CELL 0.71073 13.9118 14.2967 16.4556 64.325 78.777 89.720 ZERR 4.00 0.0020 0.0007 0.0020 0.008 0.009 0.007 LATT 1 SFAC C H N O BR UNIT 80 200 8 32 8 V = 2881.64 F(000) = 1272.0 Mu = 2.85 mm-1 Cell Wt = 2425.76 Rho = 1.398 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 DFIX 0.84 0.02 O1W H1W O1W H2W O2W H21W O2W H22W O3W H31W O3W H32W DANG 1.35 0.02 H1W H2W H21W H22W H31W H32W DFIX 1.51 0.02 C61A C62A C61B C62B C63A C64A C63B C64B DFIX 1.51 0.02 C71A C72A C71B C72B C73A C74A C73B C74B EQIV_$1 -x+1, -y, -z+2 EQIV_$2 -x, -y, -z+2 FREE C61A C62B FREE C61A C61B FREE C61A C63A_$1 FREE C61A C63B FREE C62A C61B FREE C63A C61B FREE C63A C61A_$1 FREE C63A C64B FREE C63A C63B FREE C64A C64B FREE C64A C63B FREE C61B C63B_$1 FREE C63B C61B_$1 FREE C71A C72B FREE C71A C73A_$2 FREE C71A C73B FREE C71A C71B FREE C72A C72B FREE C72A C71B FREE C73A C71B FREE C73A C71A_$2 FREE C73A C73B FREE C73A C74B FREE C74A C74B FREE C74A C73B FREE C71B C73B_$2 FREE C73B C71B_$2 HTAB O2 BR02 HTAB O3 BR01 HTAB O4A O1W HTAB O31B O3W HTAB O32 BR03 HTAB O1W BR03 HTAB O1W BR04 HTAB O2W BR04 HTAB O2W BR03 HTAB O3W BR02 HTAB O4W BR02 EQIV_$3 x, y+1, z HTAB O1B O2W_$3 EQIV_$4 x+1, y, z HTAB O33 BR04_$4 HTAB O3W BR01_$4 HTAB O4W BR01_$4 EQIV_$5 x, y-1, z HTAB O34B O4W_$5 EADP C74A C72A EADP C74B C72B FMAP 2 PLAN 10 SIZE 0.03 0.08 0.10 ACTA BOND $H WGHT 0.03840 4.52860 L.S. 8 TEMP -153.00 FVAR 0.24739 BR01 5 0.133384 0.360504 0.742817 11.00000 0.02285 0.02227 = 0.04416 -0.01386 -0.01069 0.00276 BR02 5 0.774572 0.415543 0.731075 11.00000 0.02038 0.02498 = 0.04990 -0.01759 -0.00762 0.00181 BR03 5 0.602503 -0.075855 0.716251 11.00000 0.02291 0.02732 = 0.04581 -0.01870 -0.00951 0.00304 BR04 5 0.234288 -0.142898 0.769522 11.00000 0.02225 0.02287 = 0.05959 -0.01310 -0.00958 0.00310 MOLE 1 C1 1 0.494117 0.506359 0.764750 11.00000 0.01374 0.02041 = 0.02614 -0.00969 -0.00216 0.00028 C2 1 0.502779 0.416625 0.738871 11.00000 0.01497 0.01769 = 0.02526 -0.00893 -0.00363 0.00215 AFIX 13 H2 2 0.546918 0.441477 0.676400 11.00000 -1.20000 AFIX 0 C3 1 0.402251 0.378454 0.735081 11.00000 0.01707 0.02411 = 0.02664 -0.01602 -0.00396 0.00284 AFIX 13 H3 2 0.377550 0.436611 0.685130 11.00000 -1.20000 AFIX 0 C4 1 0.414296 0.288990 0.709588 11.00000 0.01626 0.02270 = 0.02832 -0.01248 -0.00909 0.00208 O1A 4 0.515518 0.506667 0.831670 11.00000 0.03391 0.03203 = 0.02827 -0.01700 -0.01272 0.00499 O1B 4 0.461510 0.587463 0.700563 11.00000 0.03376 0.01859 = 0.03389 -0.01333 -0.01660 0.00743 AFIX 147 H1 2 0.455982 0.636291 0.716130 11.00000 0.04398 AFIX 0 O2 4 0.542791 0.331944 0.802226 11.00000 0.01910 0.02152 = 0.03465 -0.01025 -0.00868 0.00208 AFIX 147 H2A 2 0.602842 0.347517 0.795781 11.00000 -1.50000 AFIX 0 O3 4 0.336391 0.354833 0.819545 11.00000 0.01465 0.03954 = 0.03725 -0.02516 0.00095 -0.00120 AFIX 147 H3A 2 0.278552 0.347454 0.813903 11.00000 -1.50000 AFIX 0 O4A 4 0.375593 0.198069 0.776062 11.00000 0.03623 0.02202 = 0.02956 -0.01474 -0.00599 -0.00018 AFIX 147 H4 2 0.389786 0.151356 0.758877 11.00000 0.04939 AFIX 0 O4B 4 0.455718 0.303330 0.632891 11.00000 0.03403 0.03817 = 0.02860 -0.02181 0.00149 -0.00384 MOLE 2 C21 1 0.704083 0.574326 0.912163 11.00000 0.03876 0.02739 = 0.02242 -0.00884 -0.00894 0.00133 AFIX 23 H21A 2 0.754647 0.632695 0.871062 11.00000 -1.20000 H21B 2 0.690072 0.537392 0.876328 11.00000 -1.20000 AFIX 0 C22 1 0.764925 0.550136 1.051762 11.00000 0.03435 0.02994 = 0.02516 -0.01337 -0.00714 0.00028 AFIX 23 H22A 2 0.795576 0.500245 1.101119 11.00000 -1.20000 H22B 2 0.700936 0.563328 1.081792 11.00000 -1.20000 AFIX 0 C23 1 0.840834 0.470814 0.948368 11.00000 0.02629 0.02985 = 0.04294 -0.02157 0.00822 0.00263 AFIX 23 H23A 2 0.824722 0.437030 0.910777 11.00000 -1.20000 H23B 2 0.883886 0.535329 0.906177 11.00000 -1.20000 AFIX 0 C24 1 0.675142 0.403778 1.053955 11.00000 0.02778 0.02331 = 0.02712 -0.00971 -0.00278 0.00195 AFIX 23 H24A 2 0.704748 0.358853 1.106294 11.00000 -1.20000 H24B 2 0.613907 0.426000 1.079738 11.00000 -1.20000 AFIX 0 C25 1 0.611486 0.618789 0.938948 11.00000 0.03512 0.02613 = 0.04147 -0.01389 -0.02029 0.01012 AFIX 137 H25A 2 0.559714 0.562049 0.977334 11.00000 -1.50000 H25B 2 0.590065 0.666724 0.883167 11.00000 -1.50000 H25C 2 0.624470 0.656506 0.973758 11.00000 -1.50000 AFIX 0 C26 1 0.830288 0.651485 1.001532 11.00000 0.02825 0.03413 = 0.03737 -0.02061 -0.00921 0.00043 AFIX 137 H26A 2 0.889101 0.642699 0.962597 11.00000 -1.50000 H26B 2 0.849853 0.670968 1.046614 11.00000 -1.50000 H26C 2 0.794219 0.706393 0.962872 11.00000 -1.50000 AFIX 0 C27 1 0.896988 0.398831 1.016710 11.00000 0.03197 0.03184 = 0.08224 -0.01899 -0.00764 0.00804 AFIX 137 H27A 2 0.914083 0.431774 1.053900 11.00000 -1.50000 H27B 2 0.957291 0.384507 0.983552 11.00000 -1.50000 H27C 2 0.856154 0.333345 1.057175 11.00000 -1.50000 AFIX 0 C28 1 0.648514 0.339680 1.007840 11.00000 0.03527 0.02683 = 0.04292 -0.01764 -0.00352 -0.00115 AFIX 137 H28A 2 0.614641 0.381585 0.958711 11.00000 -1.50000 H28B 2 0.605074 0.278070 1.053479 11.00000 -1.50000 H28C 2 0.708499 0.317677 0.981323 11.00000 -1.50000 AFIX 0 N21 3 0.746105 0.500209 0.991822 11.00000 0.02170 0.01701 = 0.01933 -0.00592 -0.00276 0.00301 MOLE 3 C31 1 0.866560 0.001424 0.758928 11.00000 0.02073 0.02056 = 0.02653 -0.00837 -0.01128 0.00526 C32 1 0.873772 -0.087234 0.731344 11.00000 0.01879 0.01795 = 0.02293 -0.00888 -0.00513 -0.00015 AFIX 13 H32 2 0.864590 -0.060388 0.666497 11.00000 -1.20000 AFIX 0 C33 1 0.974808 -0.129109 0.735864 11.00000 0.02149 0.01948 = 0.02631 -0.01017 -0.00870 0.00273 AFIX 13 H33 2 1.025395 -0.071788 0.689931 11.00000 -1.20000 AFIX 0 C34 1 0.979009 -0.216848 0.707749 11.00000 0.01410 0.02028 = 0.03443 -0.01357 -0.00091 0.00308 O31A 4 0.808774 0.000700 0.823533 11.00000 0.04062 0.02823 = 0.02849 -0.01498 0.00116 0.00101 O31B 4 0.931280 0.081877 0.700143 11.00000 0.02932 0.01888 = 0.04027 -0.01484 -0.00005 0.00014 AFIX 147 H31 2 0.928547 0.128418 0.718537 11.00000 0.07245 AFIX 0 O32 4 0.801693 -0.169693 0.788982 11.00000 0.01730 0.02181 = 0.04175 -0.01240 -0.00756 0.00121 AFIX 147 H32A 2 0.745857 -0.150351 0.780573 11.00000 -1.50000 AFIX 0 O33 4 0.992887 -0.156231 0.824282 11.00000 0.02201 0.03283 = 0.03944 -0.02178 -0.01392 0.00825 AFIX 147 H33A 2 1.053417 -0.160702 0.822518 11.00000 -1.50000 AFIX 0 O34A 4 0.982730 -0.200065 0.628322 11.00000 0.03550 0.03051 = 0.02923 -0.01598 -0.00340 0.00586 O34B 4 0.978788 -0.310464 0.775254 11.00000 0.03293 0.01996 = 0.03569 -0.01503 -0.00762 0.00494 AFIX 147 H34 2 0.978971 -0.355082 0.754814 11.00000 0.05261 AFIX 0 MOLE 4 C41 1 0.821186 0.869739 0.412726 11.00000 0.03340 0.01965 = 0.02527 -0.00831 -0.00243 -0.00056 AFIX 23 H41A 2 0.888921 0.871029 0.422858 11.00000 -1.20000 H41B 2 0.793858 0.934667 0.410505 11.00000 -1.20000 AFIX 0 C42 1 0.769377 0.790390 0.579171 11.00000 0.03519 0.03002 = 0.02527 -0.01392 -0.00900 0.00163 AFIX 23 H42A 2 0.839968 0.793992 0.580849 11.00000 -1.20000 H42B 2 0.744652 0.857421 0.573844 11.00000 -1.20000 AFIX 0 C43 1 0.797053 0.676695 0.498342 11.00000 0.08888 0.02131 = 0.02771 -0.01261 -0.00549 -0.00174 AFIX 23 H43A 2 0.757017 0.618499 0.553530 11.00000 -1.20000 H43B 2 0.786193 0.669722 0.443446 11.00000 -1.20000 AFIX 0 C44 1 0.653498 0.777140 0.485962 11.00000 0.03642 0.07827 = 0.04648 -0.03421 -0.00541 -0.02058 AFIX 23 H44A 2 0.616522 0.714671 0.539145 11.00000 -1.20000 H44B 2 0.650259 0.770124 0.429263 11.00000 -1.20000 AFIX 0 C45 1 0.826318 0.869370 0.320167 11.00000 0.03725 0.03729 = 0.02455 -0.01318 -0.00596 0.01170 AFIX 137 H45A 2 0.856562 0.807302 0.320206 11.00000 -1.50000 H45B 2 0.865984 0.932000 0.271367 11.00000 -1.50000 H45C 2 0.759732 0.868567 0.308983 11.00000 -1.50000 AFIX 0 C46 1 0.714837 0.704129 0.669283 11.00000 0.05920 0.02996 = 0.02418 -0.01065 -0.00482 0.00340 AFIX 137 H46A 2 0.644730 0.699733 0.668652 11.00000 -1.50000 H46B 2 0.723168 0.718938 0.720466 11.00000 -1.50000 H46C 2 0.741231 0.637756 0.677189 11.00000 -1.50000 AFIX 0 C47 1 0.903873 0.665596 0.502317 11.00000 0.08733 0.04529 = 0.04283 -0.01940 -0.01121 0.03501 AFIX 137 H47A 2 0.944699 0.720746 0.446582 11.00000 -1.50000 H47B 2 0.920846 0.597418 0.506120 11.00000 -1.50000 H47C 2 0.915643 0.671397 0.556839 11.00000 -1.50000 AFIX 0 C48 1 0.602580 0.872296 0.482861 11.00000 0.02695 0.11493 = 0.05775 -0.04526 -0.01653 0.01758 AFIX 137 H48A 2 0.601971 0.878160 0.540125 11.00000 -1.50000 H48B 2 0.534816 0.865380 0.476257 11.00000 -1.50000 H48C 2 0.638046 0.934841 0.430199 11.00000 -1.50000 AFIX 0 N41 3 0.760105 0.778386 0.493931 11.00000 0.03110 0.02537 = 0.02052 -0.01095 -0.00278 -0.00686 MOLE 5 C61A 1 0.550628 -0.093050 1.047858 10.50000 0.02451 0.01612 = 0.02038 -0.00459 -0.00758 0.00273 AFIX 23 H61A 2 0.501858 -0.142743 1.102022 10.50000 -1.20000 H61B 2 0.601636 -0.071106 1.072019 10.50000 -1.20000 AFIX 0 C62A 1 0.599068 -0.152287 0.997601 10.50000 0.04681 0.03390 = 0.04080 -0.02810 -0.03496 0.03008 AFIX 137 H62A 2 0.552010 -0.170209 0.968211 10.50000 -1.50000 H62B 2 0.621003 -0.216256 1.041377 10.50000 -1.50000 H62C 2 0.655911 -0.109186 0.950304 10.50000 -1.50000 AFIX 0 C63A 1 0.568229 0.079876 0.908675 10.50000 0.03058 0.01432 = 0.01884 -0.00418 0.00277 0.00172 AFIX 23 H63A 2 0.592412 0.045168 0.868967 10.50000 -1.20000 H63B 2 0.530207 0.137473 0.874927 10.50000 -1.20000 AFIX 0 C64A 1 0.653975 0.123101 0.928392 10.50000 0.01909 0.02629 = 0.03723 -0.01145 -0.00857 0.00458 AFIX 137 H64A 2 0.630399 0.146467 0.976064 10.50000 -1.50000 H64B 2 0.688761 0.182209 0.871916 10.50000 -1.50000 H64C 2 0.698887 0.068921 0.950103 10.50000 -1.50000 AFIX 0 C61B 1 0.543497 -0.045671 0.939403 10.50000 0.03189 0.02221 = 0.02122 -0.01089 0.00043 0.00541 AFIX 23 H61C 2 0.595633 0.005770 0.890465 10.50000 -1.20000 H61D 2 0.492090 -0.054977 0.908880 10.50000 -1.20000 AFIX 0 C62B 1 0.587192 -0.146989 0.979902 10.50000 0.02632 0.02705 = 0.03183 -0.01335 -0.01224 0.00941 AFIX 137 H62D 2 0.630997 -0.143468 1.018672 10.50000 -1.50000 H62E 2 0.624788 -0.161127 0.930148 10.50000 -1.50000 H62F 2 0.534502 -0.202947 1.017498 10.50000 -1.50000 AFIX 0 C63B 1 0.584477 0.034008 1.037808 10.50000 0.02911 0.02687 = 0.03031 -0.01104 -0.01539 0.00653 AFIX 23 H63C 2 0.553946 0.063191 1.080347 10.50000 -1.20000 H63D 2 0.615735 -0.028741 1.073735 10.50000 -1.20000 AFIX 0 C64B 1 0.663108 0.113274 0.963119 10.50000 0.02598 0.02625 = 0.06072 -0.01489 -0.01913 -0.00142 AFIX 137 H64D 2 0.693142 0.085627 0.919994 10.50000 -1.50000 H64E 2 0.713626 0.128128 0.990977 10.50000 -1.50000 H64F 2 0.633666 0.177587 0.929838 10.50000 -1.50000 AFIX 0 N61 3 0.500000 0.000000 1.000000 10.50000 0.02392 0.01624 = 0.02197 -0.00538 0.00145 -0.00127 MOLE 6 C71A 1 0.035923 -0.101469 1.073975 10.50000 0.02584 0.02281 = 0.01831 -0.00554 -0.00568 -0.00126 AFIX 23 H71A 2 0.091130 -0.079725 1.093771 10.50000 -1.20000 H71B 2 -0.018571 -0.134216 1.128856 10.50000 -1.20000 AFIX 0 C72A 1 0.069166 -0.182947 1.041254 10.50000 0.03752 0.02903 = 0.04239 -0.01295 0.00792 -0.00156 AFIX 137 H72A 2 0.014875 -0.206372 1.022510 10.50000 -1.50000 H72B 2 0.088957 -0.242441 1.091533 10.50000 -1.50000 H72C 2 0.125137 -0.152654 0.988584 10.50000 -1.50000 AFIX 0 C73A 1 0.079289 0.052868 0.919968 10.50000 0.03171 0.03734 = 0.02093 -0.00541 0.00435 -0.00170 AFIX 23 H73A 2 0.053957 0.114335 0.874923 10.50000 -1.20000 H73B 2 0.096378 0.005360 0.890993 10.50000 -1.20000 AFIX 0 C74A 1 0.172368 0.089104 0.935320 10.50000 0.03752 0.02903 = 0.04239 -0.01295 0.00792 -0.00156 AFIX 137 H74A 2 0.155963 0.121403 0.977438 10.50000 -1.50000 H74B 2 0.211728 0.140164 0.876195 10.50000 -1.50000 H74C 2 0.210141 0.029386 0.962342 10.50000 -1.50000 AFIX 0 C71B 1 0.037249 -0.059527 0.947530 10.50000 0.04017 0.02593 = 0.02384 -0.01389 -0.01071 0.00682 AFIX 23 H71C 2 0.090356 -0.016063 0.894304 10.50000 -1.20000 H71D 2 -0.016615 -0.076401 0.923299 10.50000 -1.20000 AFIX 0 C72B 1 0.076753 -0.160257 1.008192 10.50000 0.03273 0.02725 = 0.04725 -0.01986 -0.00497 0.00419 AFIX 137 H72D 2 0.129580 -0.143727 1.032800 10.50000 -1.50000 H72E 2 0.102524 -0.196919 0.971322 10.50000 -1.50000 H72F 2 0.023504 -0.204760 1.059378 10.50000 -1.50000 AFIX 0 C73B 1 0.083077 0.039253 1.029384 10.50000 0.03318 0.02790 = 0.04045 -0.02164 -0.01422 0.00112 AFIX 23 H73C 2 0.054293 0.079665 1.062642 10.50000 -1.20000 H73D 2 0.108958 -0.022144 1.073970 10.50000 -1.20000 AFIX 0 C74B 1 0.167075 0.104620 0.955829 10.50000 0.03273 0.02725 = 0.04725 -0.01986 -0.00497 0.00419 AFIX 137 H74D 2 0.192337 0.069305 0.917647 10.50000 -1.50000 H74E 2 0.219231 0.116066 0.983749 10.50000 -1.50000 H74F 2 0.145359 0.171839 0.917314 10.50000 -1.50000 AFIX 0 N71 3 0.000000 0.000000 1.000000 10.50000 0.02232 0.02865 = 0.01974 -0.01015 -0.00517 0.00029 MOLE 7 C81 1 0.649655 0.351994 0.487556 11.00000 0.03149 0.04026 = 0.03717 -0.01628 -0.00728 0.00863 AFIX 23 H81A 2 0.626695 0.370925 0.429559 11.00000 -1.20000 H81B 2 0.594387 0.310961 0.539506 11.00000 -1.20000 AFIX 0 C82 1 0.692788 0.187240 0.489682 11.00000 0.04207 0.03521 = 0.04470 -0.01966 -0.00337 -0.00488 AFIX 23 H82A 2 0.662322 0.207862 0.435482 11.00000 -1.20000 H82B 2 0.640293 0.151648 0.545862 11.00000 -1.20000 AFIX 0 C83 1 0.815972 0.340934 0.404441 11.00000 0.03000 0.03724 = 0.04183 -0.01485 -0.00292 0.00290 AFIX 23 H83A 2 0.873638 0.299505 0.409291 11.00000 -1.20000 H83B 2 0.836525 0.407842 0.403161 11.00000 -1.20000 AFIX 0 C84 1 0.777760 0.260797 0.571255 11.00000 0.04388 0.04265 = 0.04050 -0.01838 -0.01608 0.00586 AFIX 23 H84A 2 0.804628 0.327383 0.566537 11.00000 -1.20000 H84B 2 0.833144 0.217180 0.570699 11.00000 -1.20000 AFIX 0 C85 1 0.675357 0.450643 0.493987 11.00000 0.04781 0.03170 = 0.03515 -0.01759 -0.00625 0.01110 AFIX 137 H85A 2 0.696721 0.432849 0.551891 11.00000 -1.50000 H85B 2 0.617403 0.490119 0.492486 11.00000 -1.50000 H85C 2 0.728641 0.493026 0.441761 11.00000 -1.50000 AFIX 0 C86 1 0.770558 0.109970 0.486802 11.00000 0.09288 0.02663 = 0.04850 -0.01649 0.00619 0.00099 AFIX 137 H86A 2 0.816778 0.140622 0.426831 11.00000 -1.50000 H86B 2 0.737521 0.044778 0.495761 11.00000 -1.50000 H86C 2 0.806500 0.095700 0.535996 11.00000 -1.50000 AFIX 0 C87 1 0.786389 0.363458 0.313705 11.00000 0.03507 0.02845 = 0.02476 -0.00986 -0.00476 0.00272 AFIX 137 H87A 2 0.764714 0.297865 0.314546 11.00000 -1.50000 H87B 2 0.842934 0.398126 0.262371 11.00000 -1.50000 H87C 2 0.732499 0.408863 0.305866 11.00000 -1.50000 AFIX 0 C88 1 0.702399 0.204180 0.664956 11.00000 0.05007 0.02740 = 0.02262 -0.01104 -0.01172 0.00671 AFIX 137 H88A 2 0.649981 0.249232 0.668339 11.00000 -1.50000 H88B 2 0.735960 0.188619 0.715915 11.00000 -1.50000 H88C 2 0.673872 0.139091 0.669529 11.00000 -1.50000 AFIX 0 N81 3 0.735548 0.282759 0.489648 11.00000 0.02019 0.02634 = 0.02255 -0.01224 -0.00417 -0.00014 MOLE 8 O1W 4 0.400590 0.032853 0.750065 11.00000 0.02970 0.04324 = 0.12084 -0.05631 -0.02636 0.01268 H1W 2 0.454048 0.010200 0.738236 11.00000 0.03826 H2W 2 0.355573 -0.008653 0.755302 11.00000 0.06244 MOLE 9 O2W 4 0.439141 -0.242756 0.720077 11.00000 0.02637 0.03323 = 0.08426 -0.03833 -0.00204 -0.00176 H21W 2 0.385170 -0.221813 0.733557 11.00000 0.11249 H22W 2 0.483288 -0.203982 0.721506 11.00000 0.06908 MOLE 10 O3W 4 0.933490 0.244767 0.732673 11.00000 0.02585 0.04661 = 0.13489 -0.06677 -0.02420 0.01040 H31W 2 0.983315 0.270531 0.738705 11.00000 0.07232 H32W 2 0.887294 0.280850 0.738370 11.00000 0.09251 MOLE 11 O4W 4 0.974039 0.534997 0.732086 11.00000 0.02430 0.03472 = 0.07969 -0.03874 -0.01205 0.00700 H41W 2 1.008325 0.496984 0.739306 11.00000 0.04729 H42W 2 0.918881 0.506350 0.731155 11.00000 0.08963 HKLF 4 Covalent radii and connectivity table for 04skc0011p-18 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 BR 1.140 Br01 - no bonds found Br02 - no bonds found Br03 - no bonds found Br04 - no bonds found C1 - O1A O1B C2 C2 - O2 C1 C3 C3 - O3 C4 C2 C4 - O4B O4A C3 O1A - C1 O1B - C1 O2 - C2 O3 - C3 O4A - C4 O4B - C4 C21 - N21 C25 C22 - N21 C26 C23 - C27 N21 C24 - C28 N21 C25 - C21 C26 - C22 C27 - C23 C28 - C24 N21 - C22 C21 C23 C24 C31 - O31A O31B C32 C32 - O32 C31 C33 C33 - O33 C34 C32 C34 - O34A O34B C33 O31A - C31 O31B - C31 O32 - C32 O33 - C33 O34A - C34 O34B - C34 C41 - N41 C45 C42 - C46 N41 C43 - C47 N41 C44 - N41 C48 C45 - C41 C46 - C42 C47 - C43 C48 - C44 N41 - C41 C42 C44 C43 C61A - N61 C62A C62A - C61A C63A - C64A N61 C64A - C63A C61B - N61 C62B C62B - C61B C63B - C64B N61 C64B - C63B N61 - C61B_$1 C61B C61A C61A_$1 C63A C63A_$1 C63B C63B_$1 C71A - C72A N71 C72A - C71A C73A - N71 C74A C74A - C73A C71B - N71 C72B C72B - C71B C73B - C74B N71 C74B - C73B N71 - C73A_$2 C73A C71B C71B_$2 C73B C73B_$2 C71A C71A_$2 C81 - C85 N81 C82 - N81 C86 C83 - N81 C87 C84 - N81 C88 C85 - C81 C86 - C82 C87 - C83 C88 - C84 N81 - C84 C82 C83 C81 O1W - no bonds found O2W - no bonds found O3W - no bonds found O4W - no bonds found Operators for generating equivalent atoms: $1 -x+1, -y, -z+2 $2 -x, -y, -z+2 $3 x, y+1, z $4 x+1, y, z $5 x, y-1, z 65173 Reflections read, of which 243 rejected -18 =< h =< 18, -18 =< k =< 18, -21 =< l =< 21, Max. 2-theta = 54.97 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 3 12 2 1.13 0.36 6 2.99 0 -15 3 -7.52 3.58 2 27.49 1 6 4 0.58 0.22 7 1.25 -1 13 4 2.48 0.60 5 3.61 3 8 6 0.06 0.07 8 0.91 4 12 11 1.14 0.46 8 2.82 6 Inconsistent equivalents 13207 Unique reflections, of which 0 suppressed R(int) = 0.0756 R(sigma) = 0.0673 Friedel opposites merged Maximum memory for data reduction = 9099 / 133109 Special position constraints for N61 x = 0.5000 y = 0.0000 z = 1.0000 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for N71 x = 0.0000 y = 0.0000 z = 1.0000 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 = 11399 / 993073 wR2 = 0.1111 before cycle 1 for 13207 data and 704 / 704 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 14. 3. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.013 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.012; Restrained GooF = 1.012 for 17 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 4.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24738 0.00024 -0.057 OSF Mean shift/esd = 0.007 Maximum = 0.084 for tors H74A Max. shift = 0.006 A for H74A Max. dU =-0.001 for H21W Least-squares cycle 2 Maximum vector length = 511 Memory required = 11399 / 993073 wR2 = 0.1111 before cycle 2 for 13207 data and 704 / 704 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 14. 3. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.013 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.012; Restrained GooF = 1.011 for 17 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 4.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24737 0.00024 -0.014 OSF Mean shift/esd = 0.003 Maximum = 0.085 for tors H74A Max. shift = 0.006 A for H74A Max. dU = 0.000 for H21W Least-squares cycle 3 Maximum vector length = 511 Memory required = 11399 / 993073 wR2 = 0.1111 before cycle 3 for 13207 data and 704 / 704 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 14. 3. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.013 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.012; Restrained GooF = 1.011 for 17 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 4.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24737 0.00024 -0.005 OSF Mean shift/esd = 0.001 Maximum = 0.056 for tors H74A Max. shift = 0.004 A for H74A Max. dU = 0.000 for H21W Least-squares cycle 4 Maximum vector length = 511 Memory required = 11399 / 993073 wR2 = 0.1111 before cycle 4 for 13207 data and 704 / 704 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 14. 3. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.013 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.012; Restrained GooF = 1.012 for 17 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 4.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24737 0.00024 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.037 for tors H74A Max. shift = 0.002 A for H74A Max. dU = 0.000 for H21W Least-squares cycle 5 Maximum vector length = 511 Memory required = 11399 / 993073 wR2 = 0.1111 before cycle 5 for 13207 data and 704 / 704 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 14. 3. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.013 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.012; Restrained GooF = 1.012 for 17 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 4.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24737 0.00024 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.024 for tors H74A Max. shift = 0.002 A for H74B Max. dU = 0.000 for H21W Least-squares cycle 6 Maximum vector length = 511 Memory required = 11399 / 993073 wR2 = 0.1111 before cycle 6 for 13207 data and 704 / 704 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 14. 3. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.013 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.012; Restrained GooF = 1.012 for 17 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 4.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24737 0.00024 -0.001 OSF Mean shift/esd = 0.000 Maximum = 0.016 for tors H74A Max. shift = 0.001 A for H74B Max. dU = 0.000 for H21W Least-squares cycle 7 Maximum vector length = 511 Memory required = 11399 / 993073 wR2 = 0.1111 before cycle 7 for 13207 data and 704 / 704 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 14. 3. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.013 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.012; Restrained GooF = 1.012 for 17 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 4.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24737 0.00024 -0.002 OSF Mean shift/esd = 0.000 Maximum = 0.011 for tors H74A Max. shift = 0.001 A for H74B Max. dU = 0.000 for H42W Least-squares cycle 8 Maximum vector length = 511 Memory required = 11399 / 993073 wR2 = 0.1111 before cycle 8 for 13207 data and 704 / 704 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 14. 3. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.013 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.012; Restrained GooF = 1.012 for 17 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 4.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.24737 0.00024 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.007 for tors H74A Max. shift = 0.000 A for H74B Max. dU = 0.000 for C72A Largest correlation matrix elements -0.879 x C62B / x C62A -0.757 x C64B / x C64A 0.698 y C74B / z C74A -0.873 y C62B / y C62A 0.749 z C62B / U33 C62A 0.698 U13 C64B / x C64A 0.813 U23 C64B / y C64A 0.744 y H32W / x H32W -0.698 U23 O3W / U22 O3W -0.795 y C64B / y C64A -0.726 U23 O3W / U33 O3W 0.697 x H2W / x H1W -0.784 z C62B / z C62A -0.724 z C74A / y C74A -0.695 U23 C62B / y C62A -0.779 U33 C62B / z C62A -0.715 z C74B / y C74B -0.689 U23 C64B / U22 C64B 0.775 x H22W / x H21W 0.708 z C74B / y C74A -0.687 U23 O1W / U33 O1W -0.770 y C64B / U23 C64A -0.703 U23 C64B / y C64B 0.686 U13 C62B / U11 C62A Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.5469 0.4415 0.6764 13 1.000 0.000 C2 O2 C1 C3 H3 0.3776 0.4366 0.6851 13 1.000 0.000 C3 O3 C4 C2 H1 0.4560 0.6363 0.7161 147 0.840 0.000 O1B C1 H1 H2A 0.6029 0.3475 0.7957 147 0.840 0.000 O2 C2 H2A H3A 0.2785 0.3474 0.8139 147 0.840 0.000 O3 C3 H3A H4 0.3898 0.1514 0.7589 147 0.840 0.000 O4A C4 H4 H21A 0.6901 0.5374 0.8763 23 0.990 0.000 C21 N21 C25 H21B 0.7547 0.6327 0.8711 23 0.990 0.000 C21 N21 C25 H22A 0.7956 0.5002 1.1011 23 0.990 0.000 C22 N21 C26 H22B 0.7009 0.5633 1.0818 23 0.990 0.000 C22 N21 C26 H23A 0.8247 0.4370 0.9108 23 0.990 0.000 C23 C27 N21 H23B 0.8839 0.5353 0.9062 23 0.990 0.000 C23 C27 N21 H24A 0.7047 0.3589 1.1063 23 0.990 0.000 C24 C28 N21 H24B 0.6139 0.4260 1.0797 23 0.990 0.000 C24 C28 N21 H25A 0.5597 0.5621 0.9773 137 0.980 0.000 C25 C21 H25A H25B 0.5901 0.6667 0.8832 137 0.980 0.000 C25 C21 H25A H25C 0.6245 0.6565 0.9737 137 0.980 0.000 C25 C21 H25A H26A 0.8891 0.6427 0.9626 137 0.980 0.000 C26 C22 H26A H26B 0.8498 0.6710 1.0466 137 0.980 0.000 C26 C22 H26A H26C 0.7942 0.7064 0.9629 137 0.980 0.000 C26 C22 H26A H27A 0.9141 0.4318 1.0539 137 0.980 0.000 C27 C23 H27A H27B 0.9573 0.3845 0.9835 137 0.980 0.000 C27 C23 H27A H27C 0.8562 0.3333 1.0572 137 0.980 0.000 C27 C23 H27A H28A 0.6146 0.3816 0.9587 137 0.980 0.000 C28 C24 H28A H28B 0.6051 0.2781 1.0535 137 0.980 0.000 C28 C24 H28A H28C 0.7085 0.3177 0.9813 137 0.980 0.000 C28 C24 H28A H32 0.8646 -0.0604 0.6665 13 1.000 0.000 C32 O32 C31 C33 H33 1.0254 -0.0718 0.6899 13 1.000 0.000 C33 O33 C34 C32 H31 0.9285 0.1284 0.7185 147 0.840 0.000 O31B C31 H31 H32A 0.7459 -0.1504 0.7806 147 0.840 0.000 O32 C32 H32A H33A 1.0534 -0.1607 0.8225 147 0.840 0.000 O33 C33 H33A H34 0.9789 -0.3551 0.7548 147 0.840 0.000 O34B C34 H34 H41A 0.8889 0.8710 0.4229 23 0.990 0.000 C41 N41 C45 H41B 0.7939 0.9347 0.4105 23 0.990 0.000 C41 N41 C45 H42A 0.8400 0.7940 0.5809 23 0.990 0.000 C42 C46 N41 H42B 0.7446 0.8574 0.5739 23 0.990 0.000 C42 C46 N41 H43A 0.7570 0.6185 0.5535 23 0.990 0.000 C43 C47 N41 H43B 0.7862 0.6697 0.4435 23 0.990 0.000 C43 C47 N41 H44A 0.6165 0.7147 0.5392 23 0.990 0.000 C44 N41 C48 H44B 0.6502 0.7701 0.4293 23 0.990 0.000 C44 N41 C48 H45A 0.8566 0.8073 0.3202 137 0.980 0.000 C45 C41 H45A H45B 0.8660 0.9320 0.2714 137 0.980 0.000 C45 C41 H45A H45C 0.7597 0.8686 0.3090 137 0.980 0.000 C45 C41 H45A H46A 0.6447 0.6997 0.6687 137 0.980 0.000 C46 C42 H46A H46B 0.7232 0.7189 0.7205 137 0.980 0.000 C46 C42 H46A H46C 0.7412 0.6377 0.6772 137 0.980 0.000 C46 C42 H46A H47A 0.9447 0.7208 0.4466 137 0.980 0.000 C47 C43 H47A H47B 0.9209 0.5974 0.5061 137 0.980 0.000 C47 C43 H47A H47C 0.9156 0.6714 0.5568 137 0.980 0.000 C47 C43 H47A H48A 0.6019 0.8781 0.5401 137 0.980 0.000 C48 C44 H48A H48B 0.5348 0.8654 0.4762 137 0.980 0.000 C48 C44 H48A H48C 0.6381 0.9349 0.4302 137 0.980 0.000 C48 C44 H48A H61A 0.5019 -0.1427 1.1020 23 0.990 0.000 C61A N61 C62A H61B 0.6016 -0.0711 1.0720 23 0.990 0.000 C61A N61 C62A H62A 0.5521 -0.1701 0.9681 137 0.980 0.000 C62A C61A H62A H62B 0.6209 -0.2163 1.0414 137 0.980 0.000 C62A C61A H62A H62C 0.6560 -0.1092 0.9504 137 0.980 0.000 C62A C61A H62A H63A 0.5924 0.0452 0.8690 23 0.990 0.000 C63A C64A N61 H63B 0.5302 0.1375 0.8749 23 0.990 0.000 C63A C64A N61 H64A 0.6304 0.1465 0.9761 137 0.980 0.000 C64A C63A H64A H64B 0.6888 0.1822 0.8719 137 0.980 0.000 C64A C63A H64A H64C 0.6989 0.0689 0.9501 137 0.980 0.000 C64A C63A H64A H61C 0.5956 0.0058 0.8905 23 0.990 0.000 C61B N61 C62B H61D 0.4921 -0.0550 0.9089 23 0.990 0.000 C61B N61 C62B H62D 0.6310 -0.1435 1.0187 137 0.980 0.000 C62B C61B H62D H62E 0.6248 -0.1611 0.9301 137 0.980 0.000 C62B C61B H62D H62F 0.5345 -0.2030 1.0175 137 0.980 0.000 C62B C61B H62D H63C 0.5539 0.0632 1.0804 23 0.990 0.000 C63B C64B N61 H63D 0.6157 -0.0287 1.0737 23 0.990 0.000 C63B C64B N61 H64D 0.6931 0.0856 0.9200 137 0.980 0.000 C64B C63B H64D H64E 0.7136 0.1281 0.9910 137 0.980 0.000 C64B C63B H64D H64F 0.6336 0.1776 0.9298 137 0.980 0.000 C64B C63B H64D H71A 0.0912 -0.0797 1.0937 23 0.990 0.000 C71A C72A N71 H71B -0.0185 -0.1342 1.1289 23 0.990 0.000 C71A C72A N71 H72A 0.0148 -0.2063 1.0224 137 0.980 0.000 C72A C71A H72A H72B 0.0888 -0.2425 1.0915 137 0.980 0.000 C72A C71A H72A H72C 0.1251 -0.1527 0.9886 137 0.980 0.000 C72A C71A H72A H73A 0.0540 0.1144 0.8749 23 0.990 0.000 C73A N71 C74A H73B 0.0964 0.0054 0.8910 23 0.990 0.000 C73A N71 C74A H74A 0.1559 0.1199 0.9786 137 0.980 0.000 C74A C73A H74A H74B 0.2111 0.1413 0.8765 137 0.980 0.000 C74A C73A H74A H74C 0.2108 0.0296 0.9611 137 0.980 0.000 C74A C73A H74A H71C 0.0903 -0.0160 0.8943 23 0.990 0.000 C71B N71 C72B H71D -0.0166 -0.0765 0.9233 23 0.990 0.000 C71B N71 C72B H72D 0.1296 -0.1436 1.0329 137 0.980 0.000 C72B C71B H72D H72E 0.1028 -0.1968 0.9713 137 0.980 0.000 C72B C71B H72D H72F 0.0236 -0.2048 1.0593 137 0.980 0.000 C72B C71B H72D H73C 0.0543 0.0796 1.0627 23 0.990 0.000 C73B C74B N71 H73D 0.1090 -0.0222 1.0739 23 0.990 0.000 C73B C74B N71 H74D 0.1921 0.0697 0.9173 137 0.980 0.000 C74B C73B H74D H74E 0.2194 0.1158 0.9837 137 0.980 0.000 C74B C73B H74D H74F 0.1454 0.1721 0.9176 137 0.980 0.000 C74B C73B H74D H81A 0.6267 0.3709 0.4295 23 0.990 0.000 C81 C85 N81 H81B 0.5944 0.3110 0.5395 23 0.990 0.000 C81 C85 N81 H82A 0.6623 0.2079 0.4355 23 0.990 0.000 C82 N81 C86 H82B 0.6403 0.1516 0.5459 23 0.990 0.000 C82 N81 C86 H83A 0.8736 0.2995 0.4093 23 0.990 0.000 C83 N81 C87 H83B 0.8365 0.4079 0.4031 23 0.990 0.000 C83 N81 C87 H84A 0.8046 0.3274 0.5665 23 0.990 0.000 C84 N81 C88 H84B 0.8332 0.2172 0.5707 23 0.990 0.000 C84 N81 C88 H85A 0.6967 0.4328 0.5519 137 0.980 0.000 C85 C81 H85A H85B 0.6174 0.4901 0.4925 137 0.980 0.000 C85 C81 H85A H85C 0.7286 0.4930 0.4418 137 0.980 0.000 C85 C81 H85A H86A 0.8168 0.1406 0.4268 137 0.980 0.000 C86 C82 H86A H86B 0.7375 0.0448 0.4958 137 0.980 0.000 C86 C82 H86A H86C 0.8065 0.0957 0.5360 137 0.980 0.000 C86 C82 H86A H87A 0.7648 0.2979 0.3145 137 0.980 0.000 C87 C83 H87A H87B 0.8429 0.3982 0.2624 137 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0.00555 0.00470 H62A 0.55209 -0.17009 0.96813 0.50000 0.04855 0.00000 0.00000 H62B 0.62091 -0.21631 1.04144 0.50000 0.04855 0.00000 0.00000 H62C 0.65602 -0.10922 0.95042 0.50000 0.04855 0.00000 0.00000 C63A 0.56823 0.07988 0.90868 0.50000 0.03059 0.01433 0.01883 -0.00420 0.00277 0.00172 0.02360 0.01004 0.00051 0.00051 0.00047 0.00000 0.00408 0.00332 0.00366 0.00286 0.00303 0.00283 0.00155 H63A 0.59240 0.04517 0.86897 0.50000 0.02832 0.00000 0.00000 H63B 0.53020 0.13747 0.87494 0.50000 0.02832 0.00000 0.00000 C64A 0.65398 0.12311 0.92838 0.50000 0.01911 0.02627 0.03717 -0.01144 -0.00857 0.00460 0.02807 0.01654 0.00101 0.00128 0.00090 0.00000 0.00541 0.00517 0.00725 0.00592 0.00498 0.00398 0.00285 H64A 0.63042 0.14647 0.97605 0.50000 0.04211 0.00000 0.00000 H64B 0.68876 0.18221 0.87190 0.50000 0.04211 0.00000 0.00000 H64C 0.69890 0.06893 0.95009 0.50000 0.04211 0.00000 0.00000 C61B 0.54349 -0.04567 0.93940 0.50000 0.03189 0.02222 0.02115 -0.01085 0.00041 0.00544 0.02554 0.01102 0.00055 0.00053 0.00048 0.00000 0.00418 0.00368 0.00382 0.00311 0.00314 0.00302 0.00159 H61C 0.59563 0.00577 0.89047 0.50000 0.03065 0.00000 0.00000 H61D 0.49208 -0.05495 0.90887 0.50000 0.03065 0.00000 0.00000 C62B 0.58717 -0.14701 0.97988 0.50000 0.02635 0.02706 0.03167 -0.01341 -0.01246 0.00950 0.02727 0.03325 0.00158 0.00133 0.00136 0.00000 0.00646 0.00663 0.00768 0.00597 0.00743 0.00488 0.00415 H62D 0.63098 -0.14351 1.01866 0.50000 0.04091 0.00000 0.00000 H62E 0.62476 -0.16113 0.93011 0.50000 0.04091 0.00000 0.00000 H62F 0.53448 -0.20296 1.01746 0.50000 0.04091 0.00000 0.00000 C63B 0.58447 0.03400 1.03781 0.50000 0.02907 0.02689 0.03024 -0.01104 -0.01532 0.00651 0.02796 0.01019 0.00053 0.00056 0.00051 0.00000 0.00414 0.00392 0.00425 0.00337 0.00335 0.00310 0.00166 H63C 0.55393 0.06318 1.08036 0.50000 0.03355 0.00000 0.00000 H63D 0.61573 -0.02875 1.07374 0.50000 0.03355 0.00000 0.00000 C64B 0.66310 0.11327 0.96313 0.50000 0.02601 0.02627 0.06050 -0.01483 -0.01906 -0.00145 0.03766 0.01954 0.00111 0.00127 0.00085 0.00000 0.00542 0.00642 0.01047 0.00777 0.00712 0.00424 0.00365 H64D 0.69315 0.08562 0.92001 0.50000 0.05649 0.00000 0.00000 H64E 0.71360 0.12815 0.99099 0.50000 0.05649 0.00000 0.00000 H64F 0.63365 0.17758 0.92983 0.50000 0.05649 0.00000 0.00000 N61 0.50000 0.00000 1.00000 0.50000 0.02390 0.01620 0.02197 -0.00537 0.00145 -0.00126 0.02275 0.00000 0.00000 0.00000 0.00000 0.00000 0.00226 0.00203 0.00226 0.00176 0.00177 0.00165 0.00091 C71A 0.03592 -0.10147 1.07398 0.50000 0.02586 0.02280 0.01826 -0.00550 -0.00567 -0.00126 0.02345 0.01001 0.00053 0.00052 0.00047 0.00000 0.00387 0.00365 0.00363 0.00298 0.00295 0.00289 0.00153 H71A 0.09118 -0.07974 1.09373 0.50000 0.02814 0.00000 0.00000 H71B -0.01855 -0.13419 1.12889 0.50000 0.02814 0.00000 0.00000 C72A 0.06906 -0.18296 1.04122 0.50000 0.03735 0.02881 0.04270 -0.01304 0.00822 -0.00177 0.03979 0.02074 0.00089 0.00085 0.00080 0.00000 0.00455 0.00409 0.00558 0.00302 0.00350 0.00297 0.00235 H72A 0.01475 -0.20627 1.02242 0.50000 0.05968 0.00000 0.00000 H72B 0.08877 -0.24253 1.09150 0.50000 0.05968 0.00000 0.00000 H72C 0.12507 -0.15272 0.98858 0.50000 0.05968 0.00000 0.00000 C73A 0.07928 0.05287 0.91996 0.50000 0.03172 0.03728 0.02089 -0.00540 0.00440 -0.00172 0.03417 0.01160 0.00055 0.00064 0.00052 0.00000 0.00447 0.00452 0.00406 0.00350 0.00333 0.00347 0.00186 H73A 0.05397 0.11435 0.87491 0.50000 0.04100 0.00000 0.00000 H73B 0.09639 0.00538 0.89097 0.50000 0.04100 0.00000 0.00000 C74A 0.17236 0.08908 0.93541 0.50000 0.03735 0.02881 0.04270 -0.01304 0.00822 -0.00177 0.03979 0.01577 0.00085 0.00105 0.00104 0.00000 0.00455 0.00409 0.00558 0.00302 0.00350 0.00297 0.00235 H74A 0.15589 0.11992 0.97865 0.50000 0.05968 0.00000 0.00000 H74B 0.21106 0.14132 0.87653 0.50000 0.05968 0.00000 0.00000 H74C 0.21082 0.02960 0.96114 0.50000 0.05968 0.00000 0.00000 C71B 0.03726 -0.05953 0.94752 0.50000 0.04022 0.02589 0.02381 -0.01387 -0.01069 0.00681 0.02834 0.01088 0.00059 0.00055 0.00050 0.00000 0.00461 0.00390 0.00400 0.00329 0.00339 0.00324 0.00167 H71C 0.09032 -0.01604 0.89426 0.50000 0.03401 0.00000 0.00000 H71D -0.01662 -0.07647 0.92335 0.50000 0.03401 0.00000 0.00000 C72B 0.07686 -0.16022 1.00821 0.50000 0.03269 0.02730 0.04723 -0.01979 -0.00480 0.00411 0.03508 0.01963 0.00082 0.00079 0.00079 0.00000 0.00434 0.00386 0.00569 0.00303 0.00347 0.00276 0.00205 H72D 0.12956 -0.14363 1.03292 0.50000 0.05262 0.00000 0.00000 H72E 0.10283 -0.19680 0.97131 0.50000 0.05262 0.00000 0.00000 H72F 0.02361 -0.20484 1.05932 0.50000 0.05262 0.00000 0.00000 C73B 0.08308 0.03924 1.02939 0.50000 0.03318 0.02792 0.04045 -0.02167 -0.01422 0.00110 0.03047 0.00989 0.00054 0.00058 0.00054 0.00000 0.00439 0.00403 0.00474 0.00368 0.00363 0.00323 0.00176 H73C 0.05428 0.07958 1.06271 0.50000 0.03657 0.00000 0.00000 H73D 0.10901 -0.02216 1.07392 0.50000 0.03657 0.00000 0.00000 C74B 0.16707 0.10474 0.95577 0.50000 0.03269 0.02730 0.04723 -0.01979 -0.00480 0.00411 0.03508 0.01647 0.00083 0.00100 0.00101 0.00000 0.00434 0.00386 0.00569 0.00303 0.00347 0.00276 0.00205 H74D 0.19206 0.06970 0.91729 0.50000 0.05262 0.00000 0.00000 H74E 0.21941 0.11582 0.98367 0.50000 0.05262 0.00000 0.00000 H74F 0.14540 0.17213 0.91756 0.50000 0.05262 0.00000 0.00000 N71 0.00000 0.00000 1.00000 0.50000 0.02232 0.02862 0.01978 -0.01017 -0.00516 0.00029 0.02364 0.00000 0.00000 0.00000 0.00000 0.00000 0.00224 0.00233 0.00223 0.00187 0.00177 0.00176 0.00092 C81 0.64966 0.35200 0.48754 1.00000 0.03147 0.04022 0.03715 -0.01627 -0.00728 0.00863 0.03659 0.00615 0.00030 0.00032 0.00030 0.00000 0.00227 0.00238 0.00241 0.00197 0.00184 0.00179 0.00096 H81A 0.62672 0.37094 0.42954 1.00000 0.04391 0.00000 0.00000 H81B 0.59439 0.31097 0.53949 1.00000 0.04391 0.00000 0.00000 C82 0.69279 0.18724 0.48968 1.00000 0.04202 0.03522 0.04462 -0.01964 -0.00334 -0.00493 0.04073 0.00610 0.00032 0.00032 0.00032 0.00000 0.00258 0.00234 0.00266 0.00207 0.00205 0.00190 0.00104 H82A 0.66233 0.20786 0.43547 1.00000 0.04888 0.00000 0.00000 H82B 0.64029 0.15165 0.54585 1.00000 0.04888 0.00000 0.00000 C83 0.81598 0.34094 0.40443 1.00000 0.02997 0.03718 0.04175 -0.01481 -0.00289 0.00286 0.03796 0.00619 0.00030 0.00033 0.00029 0.00000 0.00226 0.00234 0.00255 0.00200 0.00188 0.00176 0.00099 H83A 0.87364 0.29951 0.40928 1.00000 0.04555 0.00000 0.00000 H83B 0.83653 0.40785 0.40315 1.00000 0.04555 0.00000 0.00000 C84 0.77777 0.26081 0.57126 1.00000 0.04387 0.04261 0.04045 -0.01839 -0.01606 0.00585 0.04123 0.00621 0.00033 0.00035 0.00029 0.00000 0.00262 0.00251 0.00258 0.00210 0.00206 0.00198 0.00103 H84A 0.80463 0.32739 0.56654 1.00000 0.04947 0.00000 0.00000 H84B 0.83316 0.21720 0.57070 1.00000 0.04947 0.00000 0.00000 C85 0.67536 0.45065 0.49398 1.00000 0.04782 0.03169 0.03514 -0.01758 -0.00624 0.01110 0.03760 0.00619 0.00032 0.00031 0.00029 0.00000 0.00264 0.00220 0.00240 0.00190 0.00196 0.00187 0.00098 H85A 0.69673 0.43285 0.55189 1.00000 0.05639 0.00000 0.00000 H85B 0.61740 0.49011 0.49249 1.00000 0.05639 0.00000 0.00000 H85C 0.72864 0.49304 0.44176 1.00000 0.05639 0.00000 0.00000 C86 0.77055 0.10997 0.48681 1.00000 0.09287 0.02666 0.04849 -0.01650 0.00619 0.00102 0.05922 0.00822 0.00042 0.00034 0.00035 0.00000 0.00417 0.00237 0.00304 0.00222 0.00276 0.00242 0.00146 H86A 0.81677 0.14062 0.42684 1.00000 0.08883 0.00000 0.00000 H86B 0.73752 0.04478 0.49578 1.00000 0.08883 0.00000 0.00000 H86C 0.80650 0.09572 0.53600 1.00000 0.08883 0.00000 0.00000 C87 0.78639 0.36346 0.31371 1.00000 0.03509 0.02840 0.02476 -0.00986 -0.00475 0.00273 0.03034 0.00557 0.00029 0.00030 0.00025 0.00000 0.00223 0.00203 0.00204 0.00167 0.00168 0.00164 0.00086 H87A 0.76475 0.29786 0.31454 1.00000 0.04552 0.00000 0.00000 H87B 0.84292 0.39816 0.26237 1.00000 0.04552 0.00000 0.00000 H87C 0.73247 0.40883 0.30589 1.00000 0.04552 0.00000 0.00000 C88 0.70240 0.20418 0.66495 1.00000 0.05007 0.02742 0.02262 -0.01105 -0.01173 0.00669 0.03278 0.00578 0.00031 0.00030 0.00025 0.00000 0.00259 0.00204 0.00205 0.00169 0.00181 0.00176 0.00091 H88A 0.64999 0.24923 0.66834 1.00000 0.04917 0.00000 0.00000 H88B 0.73596 0.18861 0.71592 1.00000 0.04917 0.00000 0.00000 H88C 0.67388 0.13910 0.66952 1.00000 0.04917 0.00000 0.00000 N81 0.73554 0.28276 0.48965 1.00000 0.02019 0.02636 0.02255 -0.01225 -0.00418 -0.00012 0.02255 0.00400 0.00021 0.00022 0.00020 0.00000 0.00150 0.00159 0.00158 0.00131 0.00122 0.00119 0.00063 O1W 0.40059 0.03285 0.75006 1.00000 0.02972 0.04322 0.12087 -0.05629 -0.02636 0.01267 0.05573 0.00445 0.00024 0.00025 0.00029 0.00000 0.00177 0.00189 0.00321 0.00211 0.00196 0.00150 0.00097 H1W 0.45405 0.01019 0.73822 1.00000 0.03844 0.05403 0.00161 0.00296 0.00292 0.00000 0.01268 H2W 0.35557 -0.00873 0.75541 1.00000 0.06239 0.03944 0.00206 0.00305 0.00351 0.00000 0.01608 O2W 0.43914 -0.24275 0.72008 1.00000 0.02635 0.03324 0.08428 -0.03837 -0.00203 -0.00174 0.04486 0.00435 0.00023 0.00023 0.00025 0.00000 0.00163 0.00163 0.00249 0.00170 0.00163 0.00132 0.00080 H21W 0.38518 -0.22182 0.73360 1.00000 0.11107 0.07730 0.00197 0.00455 0.00469 0.00000 0.02617 H22W 0.48330 -0.20398 0.72150 1.00000 0.06923 0.03482 0.00253 0.00344 0.00365 0.00000 0.01715 O3W 0.93349 0.24476 0.73268 1.00000 0.02584 0.04661 0.13489 -0.06677 -0.02421 0.01040 0.05829 0.00435 0.00023 0.00026 0.00031 0.00000 0.00167 0.00193 0.00345 0.00224 0.00197 0.00148 0.00103 H31W 0.98333 0.27057 0.73866 1.00000 0.07211 0.03732 0.00219 0.00373 0.00374 0.00000 0.01767 H32W 0.88730 0.28087 0.73831 1.00000 0.09273 0.07395 0.00253 0.00387 0.00429 0.00000 0.02187 O4W 0.97404 0.53499 0.73209 1.00000 0.02429 0.03470 0.07965 -0.03873 -0.01203 0.00697 0.04115 0.00460 0.00025 0.00025 0.00025 0.00000 0.00165 0.00173 0.00250 0.00174 0.00159 0.00142 0.00081 H41W 1.00837 0.49685 0.73931 1.00000 0.04764 0.07370 0.00385 0.00393 0.00349 0.00000 0.01688 H42W 0.91892 0.50634 0.73115 1.00000 0.08896 0.09508 0.00481 0.00467 0.00412 0.00000 0.02074 Final Structure Factor Calculation for 04skc0011p-18 in P-1 Total number of l.s. parameters = 704 Maximum vector length = 511 Memory required = 10695 / 24017 wR2 = 0.1111 before cycle 9 for 13207 data and 0 / 704 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 14. 3. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.013 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.012; Restrained GooF = 1.012 for 17 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0384 * P )^2 + 4.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0488 for 9166 Fo > 4sig(Fo) and 0.0859 for all 13207 data wR2 = 0.1111, GooF = S = 1.012, Restrained GooF = 1.012 for all data Occupancy sum of asymmetric unit = 64.00 for non-hydrogen and 100.00 for hydrogen atoms Principal mean square atomic displacements U 0.0459 0.0217 0.0209 Br01 0.0511 0.0233 0.0196 Br02 0.0459 0.0246 0.0217 Br03 0.0657 0.0230 0.0212 Br04 0.0277 0.0206 0.0136 C1 0.0264 0.0176 0.0147 C2 0.0291 0.0179 0.0158 C3 0.0290 0.0218 0.0131 C4 0.0372 0.0306 0.0196 O1A 0.0416 0.0223 0.0162 O1B 0.0371 0.0215 0.0177 O2 0.0470 0.0244 0.0139 O3 0.0374 0.0298 0.0174 O4A 0.0483 0.0294 0.0190 O4B 0.0395 0.0290 0.0213 C21 0.0359 0.0291 0.0227 C22 0.0566 0.0290 0.0144 C23 0.0324 0.0256 0.0232 C24 0.0491 0.0298 0.0195 C25 0.0394 0.0320 0.0219 C26 0.0924 0.0366 0.0259 C27 0.0466 0.0346 0.0235 C28 0.0253 0.0195 0.0162 N21 0.0304 0.0227 0.0141 C31 0.0235 0.0202 0.0158 C32 0.0279 0.0191 0.0185 C33 0.0370 0.0196 0.0125 C34 0.0473 0.0285 0.0226 O31A 0.0464 0.0270 0.0165 O31B 0.0440 0.0217 0.0164 O32 0.0425 0.0248 0.0173 O33 0.0390 0.0319 0.0229 O34A 0.0357 0.0331 0.0166 O34B 0.0359 0.0265 0.0193 C41 0.0359 0.0301 0.0214 C42 0.0923 0.0277 0.0190 C43 0.0932 0.0419 0.0201 C44 0.0479 0.0282 0.0239 C45 0.0612 0.0313 0.0242 C46 0.1079 0.0428 0.0264 C47 0.1161 0.0493 0.0228 C48 0.0390 0.0205 0.0177 N41 0.0266 0.0226 0.0144 C61A 0.0714 0.0163 0.0094 C62A 0.0386 0.0187 0.0136 C63A 0.0400 0.0269 0.0174 C64A 0.0380 0.0227 0.0159 C61B 0.0351 0.0287 0.0180 C62B 0.0374 0.0285 0.0179 C63B 0.0672 0.0290 0.0167 C64B 0.0319 0.0218 0.0145 N61 0.0305 0.0225 0.0173 C71A 0.0632 0.0311 0.0251 C72A 0.0471 0.0391 0.0163 C73A 0.0632 0.0311 0.0251 C74A 0.0409 0.0250 0.0191 C71B 0.0494 0.0329 0.0230 C72B 0.0431 0.0328 0.0155 C73B 0.0494 0.0329 0.0230 C74B 0.0301 0.0220 0.0188 N71 0.0443 0.0372 0.0283 C81 0.0524 0.0408 0.0290 C82 0.0478 0.0370 0.0290 C83 0.0482 0.0427 0.0328 C84 0.0526 0.0358 0.0244 C85 0.1079 0.0443 0.0254 C86 0.0361 0.0304 0.0245 C87 0.0503 0.0273 0.0207 C88 0.0274 0.0213 0.0190 N81 0.1210 0.0252 0.0210 O1W 0.0889 0.0271 0.0185 O2W 0.1357 0.0229 0.0163 O3W 0.0804 0.0239 0.0191 O4W Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.009 0.017 0.026 0.035 0.046 0.059 0.075 0.098 0.138 1.000 Number in group 1386. 1334. 1363. 1275. 1312. 1310. 1261. 1341. 1304. 1321. GooF 0.903 0.963 1.037 1.019 1.062 1.046 1.093 0.997 1.002 0.997 K 4.131 1.540 1.126 1.020 0.995 0.997 0.996 1.002 1.010 0.996 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 1377. 1273. 1333. 1297. 1318. 1340. 1301. 1323. 1318. 1327. GooF 0.968 0.944 0.970 1.010 0.948 0.934 0.922 0.877 0.932 1.481 K 0.995 1.040 1.039 1.027 1.008 1.011 1.012 1.012 1.014 0.984 R1 0.255 0.193 0.171 0.143 0.096 0.070 0.053 0.039 0.032 0.035 Recommended weighting scheme: WGHT 0.0383 4.5334 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 2 1 4 653.96 328.08 5.75 0.042 3.79 -4 3 1 348.43 119.06 5.24 0.025 2.79 3 2 7 810.90 469.98 5.14 0.050 2.23 -4 4 1 2820.09 2116.69 4.70 0.107 2.49 2 6 3 1098.43 678.63 4.69 0.060 2.25 2 -4 2 409.04 210.75 4.65 0.034 2.51 -1 -2 4 175.19 55.21 4.54 0.017 2.54 3 2 6 214.12 442.28 4.49 0.049 2.54 -6 4 3 489.15 242.36 4.49 0.036 1.85 -2 -1 5 4019.61 3131.12 4.47 0.130 2.27 2 3 2 900.73 1285.59 4.43 0.083 3.94 -11 14 0 -283.37 936.63 4.36 0.071 0.77 -3 0 5 749.01 1129.21 4.35 0.078 2.23 1 4 3 3095.11 3944.00 4.26 0.146 3.41 2 6 4 402.41 695.60 4.25 0.061 2.25 -3 0 4 1272.02 913.44 4.24 0.070 2.57 -2 -1 2 2725.62 2116.60 4.17 0.107 3.86 -4 3 2 416.19 226.81 4.12 0.035 2.70 2 1 5 4367.01 3524.29 4.02 0.138 3.11 -2 -1 4 32.29 134.65 4.01 0.027 2.65 1 0 6 275.54 110.60 3.97 0.024 2.47 6 16 3 834.74 1751.43 3.90 0.097 0.78 2 0 5 186.67 65.63 3.90 0.019 2.90 0 0 10 209.37 41.15 3.89 0.015 1.45 0 -6 3 1386.87 972.96 3.88 0.072 1.70 3 0 7 3938.76 4891.92 3.88 0.162 2.06 0 2 3 105750.62 124691.04 3.86 0.819 5.08 0 0 12 2334.97 1681.35 3.85 0.095 1.21 -8 15 1 25.66 433.89 3.76 0.048 0.81 1 1 3 4054.05 3294.34 3.72 0.133 5.37 4 -3 1 1301.21 971.53 3.71 0.072 2.68 -3 -2 2 1195.57 1568.02 3.69 0.092 2.77 3 -2 4 179.10 328.65 3.66 0.042 2.54 -4 1 3 214.46 95.80 3.63 0.023 2.64 1 5 5 237.06 120.96 3.62 0.025 2.56 -1 1 2 191.96 334.30 3.59 0.042 6.41 0 0 4 159580.59 186092.67 3.59 1.000 3.62 4 1 8 4919.40 5953.62 3.58 0.179 1.84 -3 -2 3 9196.38 10861.70 3.57 0.242 2.43 -3 5 0 3139.67 2547.34 3.55 0.117 2.32 7 14 1 452.47 108.90 3.54 0.024 0.82 -3 3 4 4272.37 3538.20 3.52 0.138 2.68 3 4 2 5523.88 6595.51 3.52 0.188 2.81 5 2 9 263.84 118.08 3.51 0.025 1.64 3 -2 6 171.91 60.89 3.49 0.018 1.98 -2 -1 1 3130.01 3833.51 3.48 0.144 4.79 0 4 1 938.55 646.02 3.47 0.059 3.47 0 7 16 22.75 222.16 3.47 0.035 1.01 0 0 14 840.53 544.60 3.44 0.054 1.03 1 2 2 636.74 870.87 3.43 0.068 6.03 Bond lengths and angles C1 - Distance Angles O1A 1.1972 (0.0041) O1B 1.3364 (0.0041) 124.17 (0.32) C2 1.5145 (0.0047) 125.48 (0.32) 110.32 (0.29) C1 - O1A O1B C2 - Distance Angles O2 1.4100 (0.0040) C1 1.5145 (0.0047) 111.83 (0.28) C3 1.5259 (0.0044) 108.44 (0.26) 110.68 (0.27) H2 1.0000 108.60 108.60 108.60 C2 - O2 C1 C3 C3 - Distance Angles O3 1.4093 (0.0041) C4 1.5085 (0.0046) 114.69 (0.28) C2 1.5259 (0.0044) 108.91 (0.27) 108.86 (0.27) H3 1.0000 108.06 108.06 108.06 C3 - O3 C4 C2 C4 - Distance Angles O4B 1.2087 (0.0042) O4A 1.3121 (0.0041) 124.52 (0.32) C3 1.5085 (0.0046) 120.83 (0.31) 114.65 (0.31) C4 - O4B O4A O1A - Distance Angles C1 1.1972 (0.0041) O1A - O1B - Distance Angles C1 1.3364 (0.0041) H1 0.8400 109.47 O1B - C1 O2 - Distance Angles C2 1.4100 (0.0040) H2A 0.8400 109.47 O2 - C2 O3 - Distance Angles C3 1.4093 (0.0041) H3A 0.8400 109.47 O3 - C3 O4A - Distance Angles C4 1.3121 (0.0042) H4 0.8400 109.47 O4A - C4 O4B - Distance Angles C4 1.2087 (0.0042) O4B - C21 - Distance Angles N21 1.5071 (0.0046) C25 1.5072 (0.0055) 115.01 (0.31) H21A 0.9900 108.52 108.52 H21B 0.9900 108.52 108.52 107.52 C21 - N21 C25 H21A C22 - Distance Angles N21 1.5045 (0.0044) C26 1.5139 (0.0051) 114.88 (0.30) H22A 0.9900 108.55 108.55 H22B 0.9900 108.55 108.55 107.54 C22 - N21 C26 H22A C23 - Distance Angles C27 1.5051 (0.0061) N21 1.5207 (0.0045) 114.35 (0.34) H23A 0.9900 108.67 108.67 H23B 0.9900 108.67 108.67 107.60 C23 - C27 N21 H23A C24 - Distance Angles C28 1.5061 (0.0051) N21 1.5231 (0.0043) 115.28 (0.30) H24A 0.9900 108.45 108.45 H24B 0.9900 108.45 108.45 107.49 C24 - C28 N21 H24A C25 - Distance Angles C21 1.5072 (0.0055) H25A 0.9800 109.47 H25B 0.9800 109.47 109.47 H25C 0.9800 109.47 109.47 109.47 C25 - C21 H25A H25B C26 - Distance Angles C22 1.5139 (0.0051) H26A 0.9800 109.47 H26B 0.9800 109.47 109.47 H26C 0.9800 109.47 109.47 109.47 C26 - C22 H26A H26B C27 - Distance Angles C23 1.5051 (0.0061) H27A 0.9800 109.47 H27B 0.9800 109.47 109.47 H27C 0.9800 109.47 109.47 109.47 C27 - C23 H27A H27B C28 - Distance Angles C24 1.5061 (0.0051) H28A 0.9800 109.47 H28B 0.9800 109.47 109.47 H28C 0.9800 109.47 109.47 109.47 C28 - C24 H28A H28B N21 - Distance Angles C22 1.5045 (0.0044) C21 1.5071 (0.0046) 111.25 (0.27) C23 1.5207 (0.0045) 111.55 (0.28) 105.56 (0.28) C24 1.5231 (0.0043) 106.47 (0.26) 111.39 (0.27) 110.71 (0.27) N21 - C22 C21 C23 C31 - Distance Angles O31A 1.1977 (0.0043) O31B 1.3328 (0.0042) 124.18 (0.32) C32 1.5173 (0.0048) 124.73 (0.31) 111.07 (0.30) C31 - O31A O31B C32 - Distance Angles O32 1.4026 (0.0039) C31 1.5173 (0.0048) 111.70 (0.28) C33 1.5276 (0.0048) 108.43 (0.27) 110.49 (0.27) H32 1.0000 108.72 108.72 108.72 C32 - O32 C31 C33 C33 - Distance Angles O33 1.4083 (0.0042) C34 1.5108 (0.0047) 114.81 (0.29) C32 1.5276 (0.0048) 109.06 (0.28) 108.80 (0.27) H33 1.0000 107.99 107.99 107.99 C33 - O33 C34 C32 C34 - Distance Angles O34A 1.2127 (0.0044) O34B 1.3174 (0.0043) 123.77 (0.32) C33 1.5108 (0.0047) 121.20 (0.32) 115.02 (0.32) C34 - O34A O34B O31A - Distance Angles C31 1.1977 (0.0043) O31A - O31B - Distance Angles C31 1.3328 (0.0042) H31 0.8400 109.47 O31B - C31 O32 - Distance Angles C32 1.4026 (0.0039) H32A 0.8400 109.47 O32 - C32 O33 - Distance Angles C33 1.4083 (0.0042) H33A 0.8400 109.47 O33 - C33 O34A - Distance Angles C34 1.2127 (0.0044) O34A - O34B - Distance Angles C34 1.3174 (0.0043) H34 0.8400 109.47 O34B - C34 C41 - Distance Angles N41 1.5066 (0.0043) C45 1.5133 (0.0051) 114.91 (0.30) H41A 0.9900 108.54 108.54 H41B 0.9900 108.54 108.54 107.53 C41 - N41 C45 H41A C42 - Distance Angles C46 1.5106 (0.0053) N41 1.5143 (0.0045) 114.81 (0.31) H42A 0.9900 108.56 108.56 H42B 0.9900 108.56 108.56 107.55 C42 - C46 N41 H42A C43 - Distance Angles C47 1.5048 (0.0072) N41 1.5163 (0.0051) 115.14 (0.36) H43A 0.9900 108.49 108.49 H43B 0.9900 108.49 108.49 107.50 C43 - C47 N41 H43A C44 - Distance Angles N41 1.5151 (0.0053) C48 1.5166 (0.0073) 115.22 (0.36) H44A 0.9900 108.47 108.47 H44B 0.9900 108.47 108.47 107.49 C44 - N41 C48 H44A C45 - Distance Angles C41 1.5133 (0.0051) H45A 0.9800 109.47 H45B 0.9800 109.47 109.47 H45C 0.9800 109.47 109.47 109.47 C45 - C41 H45A H45B C46 - Distance Angles C42 1.5106 (0.0053) H46A 0.9800 109.47 H46B 0.9800 109.47 109.47 H46C 0.9800 109.47 109.47 109.47 C46 - C42 H46A H46B C47 - Distance Angles C43 1.5048 (0.0072) H47A 0.9800 109.47 H47B 0.9800 109.47 109.47 H47C 0.9800 109.47 109.47 109.47 C47 - C43 H47A H47B C48 - Distance Angles C44 1.5166 (0.0073) H48A 0.9800 109.47 H48B 0.9800 109.47 109.47 H48C 0.9800 109.47 109.47 109.47 C48 - C44 H48A H48B N41 - Distance Angles C41 1.5066 (0.0044) C42 1.5143 (0.0045) 106.46 (0.26) C44 1.5151 (0.0053) 110.99 (0.31) 110.63 (0.30) C43 1.5163 (0.0051) 110.52 (0.30) 110.87 (0.30) 107.41 (0.33) N41 - C41 C42 C44 C61A - Distance Angles N61 1.4782 (0.0065) C62A 1.4963 (0.0156) 120.43 (0.87) H61A 0.9900 107.22 107.22 H61B 0.9900 107.22 107.22 106.85 C61A - N61 C62A H61A C62A - Distance Angles C61A 1.4963 (0.0156) H62A 0.9800 109.47 H62B 0.9800 109.47 109.47 H62C 0.9800 109.47 109.47 109.47 C62A - C61A H62A H62B C63A - Distance Angles C64A 1.4973 (0.0116) N61 1.5593 (0.0065) 110.81 (0.69) H63A 0.9900 109.48 109.48 H63B 0.9900 109.48 109.48 108.06 C63A - C64A N61 H63A C64A - Distance Angles C63A 1.4973 (0.0116) H64A 0.9800 109.47 H64B 0.9800 109.47 109.47 H64C 0.9800 109.47 109.47 109.47 C64A - C63A H64A H64B C61B - Distance Angles N61 1.4534 (0.0066) C62B 1.4916 (0.0150) 118.70 (0.90) H61C 0.9900 107.64 107.64 H61D 0.9900 107.64 107.64 107.06 C61B - N61 C62B H61C C62B - Distance Angles C61B 1.4916 (0.0150) H62D 0.9800 109.47 H62E 0.9800 109.47 109.47 H62F 0.9800 109.47 109.47 109.47 C62B - C61B H62D H62E C63B - Distance Angles C64B 1.5077 (0.0135) N61 1.5990 (0.0069) 113.95 (0.65) H63C 0.9900 108.76 108.76 H63D 0.9900 108.76 108.76 107.65 C63B - C64B N61 H63C C64B - Distance Angles C63B 1.5077 (0.0134) H64D 0.9800 109.47 H64E 0.9800 109.47 109.47 H64F 0.9800 109.47 109.47 109.47 C64B - C63B H64D H64E N61 - Distance Angles C61B_$1 1.4534 (0.0066) C61B 1.4534 (0.0066) 180.00 (0.38) C61A 1.4782 (0.0065) 112.18 (0.38) 67.82 (0.38) C61A_$1 1.4782 (0.0065) 67.82 (0.38) 112.18 (0.38) 180.00 (0.58) C63A 1.5593 (0.0065) 113.34 (0.37) 66.66 (0.37) 111.40 (0.38) 68.60 (0.37) C63A_$1 1.5593 (0.0065) 66.66 (0.37) 113.34 (0.37) 68.60 (0.37) 111.40 (0.38) 180.00 (0.00) C63B 1.5990 (0.0069) 70.65 (0.41) 109.35 (0.41) 71.81 (0.37) 108.19 (0.37) 78.27 (0.37) 101.73 (0.36) C63B_$1 1.5990 (0.0069) 109.35 (0.41) 70.65 (0.41) 108.19 (0.37) 71.81 (0.37) 101.73 (0.36) 78.27 (0.37) 180.00 (0.51) N61 - C61B_$1 C61B C61A C61A_$1 C63A C63A_$1 C63B C71A - Distance Angles C72A 1.5176 (0.0132) N71 1.5923 (0.0068) 115.47 (0.63) H71A 0.9900 108.41 108.41 H71B 0.9900 108.41 108.41 107.46 C71A - C72A N71 H71A C72A - Distance Angles C71A 1.5176 (0.0132) H72A 0.9800 109.47 H72B 0.9800 109.47 109.47 H72C 0.9800 109.47 109.47 109.47 C72A - C71A H72A H72B C73A - Distance Angles N71 1.4501 (0.0071) C74A 1.5026 (0.0123) 117.40 (0.75) H73A 0.9900 107.95 107.95 H73B 0.9900 107.95 107.95 107.22 C73A - N71 C74A H73A C74A - Distance Angles C73A 1.5026 (0.0123) H74A 0.9800 109.47 H74B 0.9800 109.47 109.47 H74C 0.9800 109.47 109.47 109.47 C74A - C73A H74A H74B C71B - Distance Angles N71 1.4822 (0.0070) C72B 1.5278 (0.0108) 111.26 (0.69) H71C 0.9900 109.38 109.38 H71D 0.9900 109.38 109.38 108.00 C71B - N71 C72B H71C C72B - Distance Angles C71B 1.5278 (0.0109) H72D 0.9800 109.47 H72E 0.9800 109.47 109.47 H72F 0.9800 109.47 109.47 109.47 C72B - C71B H72D H72E C73B - Distance Angles C74B 1.4787 (0.0129) N71 1.5308 (0.0068) 117.28 (0.72) H73C 0.9900 107.98 107.98 H73D 0.9900 107.98 107.98 107.24 C73B - C74B N71 H73C C74B - Distance Angles C73B 1.4787 (0.0128) H74D 0.9800 109.47 H74E 0.9800 109.47 109.47 H74F 0.9800 109.47 109.47 109.47 C74B - C73B H74D H74E N71 - Distance Angles C73A_$2 1.4501 (0.0071) C73A 1.4501 (0.0071) 180.00 (0.00) C71B 1.4822 (0.0070) 116.16 (0.44) 63.84 (0.44) C71B_$2 1.4822 (0.0070) 63.84 (0.44) 116.16 (0.44) 180.00 (0.41) C73B 1.5308 (0.0068) 108.79 (0.42) 71.21 (0.42) 111.54 (0.42) 68.46 (0.42) C73B_$2 1.5308 (0.0068) 71.21 (0.42) 108.79 (0.42) 68.46 (0.42) 111.54 (0.42) 180.00 (0.54) C71A 1.5923 (0.0068) 69.86 (0.42) 110.14 (0.42) 76.05 (0.36) 103.95 (0.36) 74.33 (0.38) 105.67 (0.38) C71A_$2 1.5923 (0.0068) 110.14 (0.42) 69.86 (0.42) 103.95 (0.36) 76.05 (0.36) 105.67 (0.38) 74.33 (0.38) 180.00 (0.50) N71 - C73A_$2 C73A C71B C71B_$2 C73B C73B_$2 C71A C81 - Distance Angles C85 1.5090 (0.0056) N81 1.5438 (0.0049) 114.23 (0.33) H81A 0.9900 108.70 108.70 H81B 0.9900 108.70 108.70 107.62 C81 - C85 N81 H81A C82 - Distance Angles N81 1.4920 (0.0048) C86 1.5513 (0.0065) 112.73 (0.36) H82A 0.9900 109.05 109.05 H82B 0.9900 109.05 109.05 107.81 C82 - N81 C86 H82A C83 - Distance Angles N81 1.5159 (0.0048) C87 1.5243 (0.0056) 114.40 (0.32) H83A 0.9900 108.66 108.66 H83B 0.9900 108.66 108.66 107.60 C83 - N81 C87 H83A C84 - Distance Angles N81 1.4788 (0.0049) C88 1.5586 (0.0057) 113.79 (0.33) H84A 0.9900 108.80 108.80 H84B 0.9900 108.80 108.80 107.68 C84 - N81 C88 H84A C85 - Distance Angles C81 1.5090 (0.0056) H85A 0.9800 109.47 H85B 0.9800 109.47 109.47 H85C 0.9800 109.47 109.47 109.47 C85 - C81 H85A H85B C86 - Distance Angles C82 1.5513 (0.0065) H86A 0.9800 109.47 H86B 0.9800 109.47 109.47 H86C 0.9800 109.47 109.47 109.47 C86 - C82 H86A H86B C87 - Distance Angles C83 1.5243 (0.0056) H87A 0.9800 109.47 H87B 0.9800 109.47 109.47 H87C 0.9800 109.47 109.47 109.47 C87 - C83 H87A H87B C88 - Distance Angles C84 1.5586 (0.0057) H88A 0.9800 109.47 H88B 0.9800 109.47 109.47 H88C 0.9800 109.47 109.47 109.47 C88 - C84 H88A H88B N81 - Distance Angles C84 1.4788 (0.0049) C82 1.4920 (0.0048) 113.31 (0.31) C83 1.5159 (0.0048) 107.64 (0.29) 111.25 (0.30) C81 1.5438 (0.0049) 110.24 (0.30) 105.40 (0.29) 108.94 (0.29) N81 - C84 C82 C83 O1W - Distance Angles H1W 0.8319 (0.0180) H2W 0.8309 (0.0182) 108.31 (2.77) O1W - H1W O2W - Distance Angles H21W 0.8325 (0.0190) H22W 0.8398 (0.0186) 107.61 (2.96) O2W - H21W O3W - Distance Angles H31W 0.8290 (0.0187) H32W 0.8384 (0.0188) 107.45 (2.93) O3W - H31W O4W - Distance Angles H41W 0.7092 (0.0518) H42W 0.8770 (0.0650) 106.84 (5.42) O4W - H41W Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 2.43 3.248(2) 163.7 O2-H2A...Br02 0.84 2.49 3.298(3) 161.1 O3-H3A...Br01 0.84 1.77 2.587(4) 165.5 O4A-H4...O1W 0.84 1.78 2.607(4) 167.9 O31B-H31...O3W 0.84 2.46 3.282(2) 166.1 O32-H32A...Br03 0.832(18) 2.45(2) 3.273(3) 174(4) O1W-H1W...Br03 0.831(18) 2.46(2) 3.292(3) 175(4) O1W-H2W...Br04 0.833(19) 2.47(2) 3.299(3) 174(5) O2W-H21W...Br04 0.840(19) 2.44(2) 3.276(3) 174(5) O2W-H22W...Br03 0.838(19) 2.45(2) 3.281(3) 169(5) O3W-H32W...Br02 0.88(7) 2.40(7) 3.272(3) 175(5) O4W-H42W...Br02 0.84 1.77 2.593(4) 165.3 O1B-H1...O2W_$3 0.84 2.47 3.287(3) 163.5 O33-H33A...Br04_$4 0.829(19) 2.48(2) 3.311(3) 175(5) O3W-H31W...Br01_$4 0.71(5) 2.60(5) 3.299(3) 172(5) O4W-H41W...Br01_$4 0.84 1.77 2.602(4) 170.1 O34B-H34...O4W_$5 FMAP and GRID set by program FMAP 2 2 75 GRID -1.389 -1 -2 1.389 1 2 R1 = 0.0828 for 13207 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.25 at 0.6978 0.2852 0.4055 [ 1.07 A from H82A ] Deepest hole -0.78 at 0.7736 0.1532 0.2709 [ 0.77 A from BR04 ] Mean = 0.00, Rms deviation from mean = 0.10 e/A^3, Highest memory used = 9929 / 98556 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.6978 0.2852 0.4055 1.00000 0.05 1.25 1.07 H82A 1.47 C82 1.54 H87A 1.56 N81 Q2 1 0.9595 0.9863 0.4894 1.00000 0.05 1.23 2.62 H41A 2.62 H33 2.73 O34A 2.74 H32 Q3 1 0.6536 0.2097 0.5782 1.00000 0.05 1.22 1.20 H82B 1.48 H88C 1.60 N81 1.60 H81B Q4 1 0.8281 0.2088 0.5034 1.00000 0.05 1.08 1.18 H84B 1.48 H86C 1.54 H83A 1.64 C84 Q5 1 0.7733 0.3778 0.4940 1.00000 0.05 1.02 1.26 H84A 1.46 H83B 1.49 N81 1.61 C84 Q6 1 0.2394 -0.1282 0.8101 1.00000 0.05 0.59 0.80 BR04 2.11 H2W 2.58 H33A 2.72 H72E Q7 1 0.2388 -0.0273 0.6960 1.00000 0.05 0.51 1.56 BR04 1.82 H41B 2.12 H2W 2.14 H45B Q8 1 0.7654 0.3765 0.7808 1.00000 0.05 0.39 0.75 BR02 2.25 H2A 2.36 H32W 2.59 H42W Q9 1 0.5985 -0.1674 0.7019 1.00000 0.05 0.37 1.43 BR03 1.61 H22W 2.25 H46A 2.34 H46B Q10 1 0.7870 0.4448 1.0770 1.00000 0.05 0.37 1.05 H22A 1.43 C22 1.50 N21 1.53 H24A Shortest distances between peaks (including symmetry equivalents) 2 2 1.35 6 7 1.81 4 5 2.48 3 4 2.50 1 3 2.51 1 4 2.58 3 5 2.59 1 5 2.69 Time profile in seconds ----------------------- 0.08: Read and process instructions 0.00: Fit rigid groups 0.05: 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 0.02: Analyse other restraints etc. 2.97: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.00: Generate idealized H-atoms 15.67: Structure factors and derivatives 82.41: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.05: Apply other restraints 5.00: Solve l.s. equations 0.00: Generate HTAB table 0.08: Other dependent quantities, CIF, tables 0.28: Analysis of variance 0.08: Merge reflections for Fourier and .fcf 0.17: Fourier summations 0.19: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 04skc0011p-18 finished at 14:47:56 Total CPU time: 107.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++