+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s93 started at 15:47:04 on 13-Oct-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL S93 in P2(1)/c CELL 0.71073 18.1092 9.6385 12.7261 90.000 102.100 90.000 ZERR 4.00 0.0014 0.0006 0.0007 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N FE O UNIT 116 108 4 4 0 V = 2171.93 F(000) = 936.0 Mu = 0.71 mm-1 Cell Wt = 1781.46 Rho = 1.362 MERG 2 TWIN 1.00 0.00 0.00 0.00 -1.00 0.00 0.00 0.00 -1.00 2 BASF 0.02510 SHEL 7 0.84 FMAP 2 PLAN 25 SIZE 0.02 0.15 0.20 ACTA BOND $H WGHT 0.06490 153.82530 L.S. 12 TEMP -153.00 FVAR 0.09197 FE01 4 0.155544 0.262288 0.459554 11.00000 0.02763 0.01881 = 0.01936 -0.00037 0.00752 0.00046 C002 1 0.355770 0.418292 0.224339 11.00000 0.02652 0.02964 = 0.00981 0.00004 0.01321 0.00049 C003 1 0.394780 0.301419 0.200911 11.00000 0.02098 0.03823 = 0.01077 -0.00185 0.00387 -0.00344 C004 1 0.428547 0.302446 0.108912 11.00000 0.02556 0.04022 = 0.02086 -0.00993 0.00465 0.00110 C005 1 0.318910 0.665885 0.192156 11.00000 0.02208 0.02504 = 0.04850 -0.00390 0.01263 -0.00403 AFIX 43 H005 2 0.301713 0.671025 0.257630 11.00000 -1.20000 AFIX 0 N006 3 0.074021 0.674913 0.317877 11.00000 0.01987 0.04632 = 0.04921 0.00184 0.01222 0.00467 C007 1 0.066477 0.745007 0.413649 11.00000 0.02893 0.04352 = 0.06516 0.00886 0.02836 0.00695 AFIX 137 H00A 2 0.024481 0.704498 0.440801 11.00000 -1.50000 H00B 2 0.056453 0.843603 0.398043 11.00000 -1.50000 H00C 2 0.113308 0.735126 0.467970 11.00000 -1.50000 AFIX 0 C008 1 0.372933 0.659842 0.001520 11.00000 0.02871 0.04524 = 0.02192 0.00226 0.00299 -0.01055 AFIX 43 H008 2 0.392646 0.659196 -0.062027 11.00000 -1.20000 AFIX 0 C009 1 0.421587 0.422787 0.046753 11.00000 0.02539 0.03960 = 0.02396 -0.00130 0.01192 -0.00324 AFIX 43 H009 2 0.444638 0.424760 -0.013763 11.00000 -1.20000 AFIX 0 C010 1 0.077867 0.522315 0.328224 11.00000 0.01923 0.02838 = 0.04351 0.01000 0.00456 0.00213 AFIX 23 H01A 2 0.084758 0.483379 0.258934 11.00000 -1.20000 H01B 2 0.028541 0.488876 0.339967 11.00000 -1.20000 AFIX 0 C011 1 0.060599 0.142966 0.406176 11.00000 0.02053 0.03362 = 0.04741 0.01534 -0.00305 -0.00243 AFIX 43 H011 2 0.010118 0.176179 0.393654 11.00000 -1.20000 AFIX 0 C012 1 0.467584 0.183158 0.082056 11.00000 0.02711 0.03881 = 0.02980 -0.01522 0.00951 -0.00113 AFIX 43 H012 2 0.491758 0.186314 0.022667 11.00000 -1.20000 AFIX 0 C013 1 0.382433 0.540799 0.068826 11.00000 0.02219 0.04868 = 0.03063 -0.00091 0.00438 -0.00010 C014 1 0.321318 0.412234 0.321986 11.00000 0.03058 0.03641 = 0.00460 0.00374 0.00398 0.00648 AFIX 43 H014 2 0.353541 0.395463 0.389916 11.00000 -1.20000 AFIX 0 C015 1 0.352617 0.540046 0.162948 11.00000 0.01427 0.02665 = 0.04349 -0.00334 -0.00066 -0.00268 C016 1 0.311912 0.777721 0.124827 11.00000 0.03097 0.04479 = 0.02974 0.00846 0.00062 0.00244 AFIX 43 H016 2 0.289933 0.860652 0.144582 11.00000 -1.20000 AFIX 0 C017 1 0.436284 0.062050 0.227425 11.00000 0.03286 0.02483 = 0.05767 -0.00618 -0.00962 0.00804 AFIX 43 H017 2 0.438511 -0.020777 0.268435 11.00000 -1.20000 AFIX 0 C018 1 0.173769 0.058217 0.492847 11.00000 0.03441 0.02805 = 0.06386 0.01305 -0.01101 0.00864 AFIX 43 H018 2 0.212994 0.025231 0.548931 11.00000 -1.20000 AFIX 0 C019 1 0.138562 0.464249 0.415742 11.00000 0.03790 0.01681 = 0.03964 0.00567 0.03143 0.00319 C020 1 0.250104 0.376541 0.518627 11.00000 0.02322 0.02662 = 0.03270 -0.00194 0.00383 -0.00780 AFIX 43 H020 2 0.300054 0.341336 0.539140 11.00000 -1.20000 AFIX 0 C021 1 0.248142 0.429183 0.317737 11.00000 0.03170 0.01377 = 0.02876 0.00050 0.00627 -0.00120 AFIX 43 H021 2 0.215611 0.445714 0.250007 11.00000 -1.20000 AFIX 0 C022 1 0.132227 0.443778 0.526855 11.00000 0.04662 0.03825 = 0.03262 -0.01622 0.01776 -0.00169 AFIX 43 H022 2 0.088257 0.464433 0.553552 11.00000 -1.20000 AFIX 0 C023 1 0.196950 0.391490 0.587673 11.00000 0.02670 0.04132 = 0.04383 -0.02164 0.00615 -0.00418 AFIX 43 H023 2 0.205537 0.368984 0.661923 11.00000 -1.20000 AFIX 0 C024 1 0.215073 0.423228 0.415465 11.00000 0.03923 0.02198 = 0.03405 -0.00964 0.01426 -0.00012 C025 1 0.102488 0.090606 0.501945 11.00000 0.03406 0.05292 = 0.02408 0.02064 0.00072 -0.00376 AFIX 43 H025 2 0.083644 0.078962 0.565659 11.00000 -1.20000 AFIX 0 C027 1 0.470293 0.063738 0.141889 11.00000 0.03649 0.03716 = 0.04582 -0.00252 0.00800 0.01310 AFIX 43 H027 2 0.495549 -0.016310 0.123692 11.00000 -1.20000 AFIX 0 C028 1 0.108803 0.136946 0.329675 11.00000 0.04050 0.02840 = 0.03985 -0.01295 0.00555 -0.00020 AFIX 43 H028 2 0.095509 0.164491 0.256462 11.00000 -1.20000 AFIX 0 C029 1 0.179556 0.082763 0.382611 11.00000 0.05100 0.03335 = 0.03997 -0.00559 0.00793 0.00309 AFIX 43 H029 2 0.222236 0.065912 0.351946 11.00000 -1.20000 AFIX 0 C030 1 0.141752 0.729342 0.281011 11.00000 0.05225 0.02492 = 0.04710 -0.00026 0.01666 -0.00289 AFIX 137 H03A 2 0.137271 0.830123 0.271606 11.00000 -1.50000 H03B 2 0.144873 0.685918 0.212447 11.00000 -1.50000 H03C 2 0.187451 0.707618 0.334847 11.00000 -1.50000 AFIX 0 C031 1 0.398362 0.175780 0.257826 11.00000 0.02203 0.02757 = 0.07085 -0.00574 -0.00535 0.01085 AFIX 43 H031 2 0.374693 0.168489 0.317530 11.00000 -1.20000 AFIX 0 C032 1 0.336743 0.773246 0.025624 11.00000 0.04920 0.04120 = 0.03137 0.02656 0.00537 0.00470 AFIX 43 H032 2 0.327792 0.849464 -0.022709 11.00000 -1.20000 AFIX 0 HKLF 4 Covalent radii and connectivity table for S93 in P2(1)/c C 0.770 H 0.320 N 0.700 FE 1.240 O 0.660 Fe01 - C018 C019 C022 C024 C025 C020 C011 C023 C029 C028 C002 - C003 C015 C014 C003 - C002 C031 C004 C004 - C009 C012 C003 C005 - C016 C015 N006 - C007 C010 C030 C007 - N006 C008 - C032 C013 C009 - C004 C013 C010 - N006 C019 C011 - C025 C028 Fe01 C012 - C027 C004 C013 - C009 C015 C008 C014 - C021 C002 C015 - C002 C013 C005 C016 - C005 C032 C017 - C027 C031 C018 - C025 C029 Fe01 C019 - C024 C022 C010 Fe01 C020 - C024 C023 Fe01 C021 - C014 C024 C022 - C023 C019 Fe01 C023 - C022 C020 Fe01 C024 - C020 C019 C021 Fe01 C025 - C018 C011 Fe01 C027 - C017 C012 C028 - C029 C011 Fe01 C029 - C028 C018 Fe01 C030 - N006 C031 - C017 C003 C032 - C008 C016 29588 Reflections read, of which 2944 rejected -21 =< h =< 21, -11 =< k =< 11, -14 =< l =< 15, Max. 2-theta = 50.05 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 1 1 1 53.68 0.83 7 6.53 -3 0 2 175.23 7.41 5 38.72 -1 0 2 9.52 0.58 4 10.02 1 0 2 113.94 3.36 6 25.40 -3 1 2 9.53 0.57 9 41.78 1 4 2 37.30 0.78 8 3.98 -3 5 2 59.39 0.97 8 10.07 -2 3 3 11.05 0.45 5 3.19 3 0 4 10.75 0.98 4 5.89 -3 4 4 35.85 0.94 7 4.76 0 4 4 6.32 0.41 7 2.65 -2 5 4 7.28 0.49 8 3.97 12 Inconsistent equivalents 3808 Unique reflections, of which 0 suppressed R(int) = 0.1982 R(sigma) = 0.1271 Friedel opposites merged Maximum memory for data reduction = 3085 / 40103 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 = 3902 / 353995 wR2 = 0.4656 before cycle 1 for 3808 data and 283 / 283 parameters GooF = S = 1.099; Restrained GooF = 1.099 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0649 * P )^2 + 153.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.09117 0.00073 -1.106 OSF 2 0.02550 0.00353 0.114 BASF 1 Mean shift/su = 0.034 Maximum = -1.106 for OSF Max. shift = 0.003 A for H00A Max. dU =-0.001 for C023 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3902 / 353995 wR2 = 0.4646 before cycle 2 for 3808 data and 283 / 283 parameters GooF = S = 1.099; Restrained GooF = 1.099 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0649 * P )^2 + 153.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.09099 0.00072 -0.246 OSF 2 0.02575 0.00354 0.068 BASF 1 Mean shift/su = 0.014 Maximum = -0.246 for OSF Max. shift = 0.001 A for H03C Max. dU = 0.000 for C023 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3902 / 353995 wR2 = 0.4644 before cycle 3 for 3808 data and 283 / 283 parameters GooF = S = 1.100; Restrained GooF = 1.100 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0649 * P )^2 + 153.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.09098 0.00072 -0.013 OSF 2 0.02585 0.00354 0.029 BASF 1 Mean shift/su = 0.003 Maximum = 0.029 for BASF 1 Max. shift = 0.001 A for H00C Max. dU = 0.000 for C023 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3902 / 353995 wR2 = 0.4644 before cycle 4 for 3808 data and 283 / 283 parameters GooF = S = 1.100; Restrained GooF = 1.100 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0649 * P )^2 + 153.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.09098 0.00072 -0.003 OSF 2 0.02589 0.00355 0.012 BASF 1 Mean shift/su = 0.002 Maximum = 0.012 for BASF 1 Max. shift = 0.000 A for H03B Max. dU = 0.000 for C018 Least-squares cycle 5 Maximum vector length = 511 Memory required = 3902 / 353995 wR2 = 0.4644 before cycle 5 for 3808 data and 283 / 283 parameters GooF = S = 1.100; Restrained GooF = 1.100 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0649 * P )^2 + 153.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.09098 0.00072 -0.001 OSF 2 0.02591 0.00355 0.004 BASF 1 Mean shift/su = 0.001 Maximum = 0.005 for z C023 Max. shift = 0.000 A for H03A Max. dU = 0.000 for C024 Least-squares cycle 6 Maximum vector length = 511 Memory required = 3902 / 353995 wR2 = 0.4644 before cycle 6 for 3808 data and 283 / 283 parameters GooF = S = 1.100; Restrained GooF = 1.100 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0649 * P )^2 + 153.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.09098 0.00072 0.000 OSF 2 0.02591 0.00355 0.002 BASF 1 Mean shift/su = 0.000 Maximum = 0.003 for z C023 Max. shift = 0.000 A for H00C Max. dU = 0.000 for C009 Least-squares cycle 7 Maximum vector length = 511 Memory required = 3902 / 353995 wR2 = 0.4644 before cycle 7 for 3808 data and 283 / 283 parameters GooF = S = 1.100; Restrained GooF = 1.100 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0649 * P )^2 + 153.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.09098 0.00072 0.000 OSF 2 0.02591 0.00355 0.001 BASF 1 Mean shift/su = 0.000 Maximum = 0.002 for z C023 Max. shift = 0.000 A for C023 Max. dU = 0.000 for C009 Least-squares cycle 8 Maximum vector length = 511 Memory required = 3902 / 353995 wR2 = 0.4644 before cycle 8 for 3808 data and 283 / 283 parameters GooF = S = 1.100; Restrained GooF = 1.100 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0649 * P )^2 + 153.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.09098 0.00072 0.000 OSF 2 0.02592 0.00355 0.000 BASF 1 Mean shift/su = 0.000 Maximum = 0.001 for z C023 Max. shift = 0.000 A for H018 Max. dU = 0.000 for C009 Least-squares cycle 9 Maximum vector length = 511 Memory required = 3902 / 353995 wR2 = 0.4644 before cycle 9 for 3808 data and 283 / 283 parameters GooF = S = 1.100; Restrained GooF = 1.100 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0649 * P )^2 + 153.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.09098 0.00072 0.000 OSF 2 0.02592 0.00355 0.000 BASF 1 Mean shift/su = 0.000 Maximum = 0.001 for z C023 Max. shift = 0.000 A for H00C Max. dU = 0.000 for C009 Least-squares cycle 10 Maximum vector length = 511 Memory required = 3902 / 353995 wR2 = 0.4644 before cycle 10 for 3808 data and 283 / 283 parameters GooF = S = 1.100; Restrained GooF = 1.100 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0649 * P )^2 + 153.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.09098 0.00072 0.000 OSF 2 0.02592 0.00355 0.000 BASF 1 Mean shift/su = 0.000 Maximum = 0.000 for z C023 Max. shift = 0.000 A for C023 Max. dU = 0.000 for C009 Least-squares cycle 11 Maximum vector length = 511 Memory required = 3902 / 353995 wR2 = 0.4644 before cycle 11 for 3808 data and 283 / 283 parameters GooF = S = 1.100; Restrained GooF = 1.100 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0649 * P )^2 + 153.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.09098 0.00072 0.000 OSF 2 0.02592 0.00355 0.000 BASF 1 Mean shift/su = 0.000 Maximum = 0.000 for z C023 Max. shift = 0.000 A for C023 Max. dU = 0.000 for C013 Least-squares cycle 12 Maximum vector length = 511 Memory required = 3902 / 353995 wR2 = 0.4644 before cycle 12 for 3808 data and 283 / 283 parameters GooF = S = 1.100; Restrained GooF = 1.100 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0649 * P )^2 + 153.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.09098 0.00072 0.000 OSF 2 0.02592 0.00355 0.000 BASF 1 Mean shift/su = 0.000 Maximum = 0.000 for z Fe01 Max. shift = 0.000 A for H03C Max. dU = 0.000 for C017 Largest correlation matrix elements 0.523 U13 C019 / U11 C019 Idealized hydrogen atom generation before cycle 13 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H005 0.3018 0.6710 0.2579 43 0.950 0.000 C005 C016 C015 H00A 0.0245 0.7045 0.4410 137 0.980 0.000 C007 N006 H00A H00B 0.0564 0.8436 0.3983 137 0.980 0.000 C007 N006 H00A H00C 0.1133 0.7351 0.4682 137 0.980 0.000 C007 N006 H00A H008 0.3927 0.6591 -0.0621 43 0.950 0.000 C008 C032 C013 H009 0.4446 0.4248 -0.0140 43 0.950 0.000 C009 C004 C013 H01A 0.0848 0.4833 0.2589 23 0.990 0.000 C010 N006 C019 H01B 0.0285 0.4887 0.3399 23 0.990 0.000 C010 N006 C019 ** Bond(s) to Fe01 ignored in idealizing H-atoms attached to C011 ** H011 0.0100 0.1763 0.3937 43 0.950 0.000 C011 C025 C028 H012 0.4918 0.1863 0.0225 43 0.950 0.000 C012 C027 C004 H014 0.3535 0.3955 0.3900 43 0.950 0.000 C014 C021 C002 H016 0.2899 0.8608 0.1447 43 0.950 0.000 C016 C005 C032 H017 0.4385 -0.0209 0.2685 43 0.950 0.000 C017 C027 C031 ** Bond(s) to Fe01 ignored in idealizing H-atoms attached to C018 ** H018 0.2130 0.0251 0.5492 43 0.950 0.000 C018 C025 C029 ** Bond(s) to Fe01 ignored in idealizing H-atoms attached to C020 ** H020 0.3001 0.3413 0.5392 43 0.950 0.000 C020 C024 C023 H021 0.2157 0.4457 0.2499 43 0.950 0.000 C021 C014 C024 ** Bond(s) to Fe01 ignored in idealizing H-atoms attached to C022 ** H022 0.0882 0.4646 0.5537 43 0.950 0.000 C022 C023 C019 ** Bond(s) to Fe01 ignored in idealizing H-atoms attached to C023 ** H023 0.2055 0.3688 0.6622 43 0.950 0.000 C023 C022 C020 ** Bond(s) to Fe01 ignored in idealizing H-atoms attached to C025 ** H025 0.0835 0.0791 0.5658 43 0.950 0.000 C025 C018 C011 H027 0.4956 -0.0164 0.1236 43 0.950 0.000 C027 C017 C012 ** Bond(s) to Fe01 ignored in idealizing H-atoms attached to C028 ** H028 0.0954 0.1645 0.2563 43 0.950 0.000 C028 C029 C011 ** Bond(s) to Fe01 ignored in idealizing H-atoms attached to C029 ** H029 0.2223 0.0659 0.3519 43 0.950 0.000 C029 C028 C018 H03A 0.1375 0.8301 0.2717 137 0.980 0.000 C030 N006 H03A H03B 0.1449 0.6861 0.2123 137 0.980 0.000 C030 N006 H03A H03C 0.1876 0.7074 0.3347 137 0.980 0.000 C030 N006 H03A H031 0.3747 0.1685 0.3179 43 0.950 0.000 C031 C017 C003 H032 0.3278 0.8494 -0.0229 43 0.950 0.000 C032 C008 C016 S93 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Fe01 0.15554 0.26230 0.45956 1.00000 0.02696 0.01819 0.01870 -0.00033 0.00737 0.00048 0.02090 0.00461 0.00014 0.00023 0.00019 0.00000 0.00129 0.00122 0.00119 0.00105 0.00091 0.00110 0.00068 C002 0.35574 0.41832 0.22438 1.00000 0.02591 0.02905 0.00937 0.00002 0.01310 0.00064 0.02007 0.03157 0.00093 0.00178 0.00122 0.00000 0.00892 0.00924 0.00756 0.00669 0.00657 0.00729 0.00356 C003 0.39477 0.30139 0.20099 1.00000 0.02062 0.03750 0.01015 -0.00190 0.00403 -0.00330 0.02264 0.03066 0.00093 0.00192 0.00122 0.00000 0.00868 0.01022 0.00794 0.00712 0.00665 0.00741 0.00378 C004 0.42859 0.30253 0.10878 1.00000 0.02497 0.03959 0.02019 -0.00995 0.00470 0.00098 0.02826 0.03310 0.00100 0.00204 0.00139 0.00000 0.00955 0.01089 0.00889 0.00798 0.00727 0.00805 0.00413 C005 0.31891 0.66588 0.19239 1.00000 0.02163 0.02435 0.04773 -0.00370 0.01236 -0.00396 0.03049 0.03439 0.00097 0.00185 0.00165 0.00000 0.00939 0.00967 0.01196 0.00852 0.00841 0.00750 0.00431 H005 0.30178 0.67097 0.25791 1.00000 0.03659 0.00000 0.00000 N006 0.07402 0.67483 0.31786 1.00000 0.01936 0.04506 0.04860 0.00219 0.01190 0.00469 0.03697 0.03265 0.00087 0.00183 0.00141 0.00000 0.00802 0.01025 0.01054 0.00837 0.00725 0.00726 0.00405 C007 0.06646 0.74503 0.41387 1.00000 0.02854 0.04245 0.06473 0.00870 0.02823 0.00691 0.04254 0.04346 0.00110 0.00231 0.00178 0.00000 0.01050 0.01229 0.01423 0.01118 0.00973 0.00954 0.00522 H00A 0.02446 0.70450 0.44102 1.00000 0.06381 0.00000 0.00000 H00B 0.05644 0.84363 0.39830 1.00000 0.06381 0.00000 0.00000 H00C 0.11329 0.73512 0.46819 1.00000 0.06381 0.00000 0.00000 C008 0.37296 0.65979 0.00141 1.00000 0.02820 0.04456 0.02133 0.00230 0.00300 -0.01056 0.03168 0.03356 0.00103 0.00211 0.00145 0.00000 0.01008 0.01210 0.00933 0.00833 0.00775 0.00884 0.00444 H008 0.39267 0.65912 -0.06214 1.00000 0.03802 0.00000 0.00000 C009 0.42159 0.42280 0.04660 1.00000 0.02480 0.03876 0.02304 -0.00125 0.01160 -0.00320 0.02791 0.03363 0.00098 0.00197 0.00142 0.00000 0.00933 0.01080 0.00930 0.00815 0.00746 0.00800 0.00405 H009 0.44457 0.42476 -0.01398 1.00000 0.03349 0.00000 0.00000 C010 0.07783 0.52221 0.32814 1.00000 0.01858 0.02766 0.04272 0.00995 0.00421 0.00218 0.02998 0.03623 0.00099 0.00189 0.00162 0.00000 0.00890 0.01000 0.01123 0.00852 0.00780 0.00755 0.00422 H01A 0.08476 0.48328 0.25887 1.00000 0.03597 0.00000 0.00000 H01B 0.02850 0.48875 0.33987 1.00000 0.03597 0.00000 0.00000 C011 0.06050 0.14305 0.40623 1.00000 0.02000 0.03286 0.04639 0.01516 -0.00316 -0.00227 0.03456 0.03638 0.00104 0.00202 0.00163 0.00000 0.00949 0.01078 0.01223 0.00920 0.00837 0.00810 0.00470 H011 0.01003 0.17630 0.39373 1.00000 0.04147 0.00000 0.00000 C012 0.46762 0.18315 0.08192 1.00000 0.02653 0.03821 0.02916 -0.01543 0.00934 -0.00107 0.03079 0.03331 0.00102 0.00203 0.00150 0.00000 0.00992 0.01101 0.01004 0.00849 0.00792 0.00826 0.00434 H012 0.49178 0.18630 0.02251 1.00000 0.03695 0.00000 0.00000 C013 0.38249 0.54073 0.06878 1.00000 0.02165 0.04780 0.03028 -0.00070 0.00440 -0.00002 0.03339 0.03594 0.00101 0.00220 0.00151 0.00000 0.00942 0.01217 0.01046 0.00914 0.00776 0.00872 0.00449 C014 0.32132 0.41225 0.32202 1.00000 0.02995 0.03573 0.00405 0.00376 0.00421 0.00644 0.02315 0.03260 0.00097 0.00188 0.00120 0.00000 0.00965 0.01018 0.00735 0.00682 0.00652 0.00786 0.00384 H014 0.35351 0.39548 0.38997 1.00000 0.02777 0.00000 0.00000 C015 0.35262 0.54007 0.16301 1.00000 0.01372 0.02581 0.04286 -0.00306 -0.00074 -0.00253 0.02844 0.03271 0.00094 0.00189 0.00155 0.00000 0.00849 0.00950 0.01130 0.00822 0.00758 0.00724 0.00413 C016 0.31185 0.77784 0.12496 1.00000 0.03034 0.04403 0.02917 0.00839 0.00063 0.00241 0.03533 0.03668 0.00106 0.00226 0.00147 0.00000 0.01035 0.01216 0.01016 0.00904 0.00794 0.00902 0.00460 H016 0.28986 0.86077 0.14469 1.00000 0.04240 0.00000 0.00000 C017 0.43630 0.06200 0.22754 1.00000 0.03233 0.02413 0.05666 -0.00606 -0.00986 0.00811 0.04051 0.03658 0.00110 0.00208 0.00183 0.00000 0.01112 0.01032 0.01377 0.00951 0.00985 0.00860 0.00525 H017 0.43855 -0.02086 0.26852 1.00000 0.04861 0.00000 0.00000 C018 0.17378 0.05813 0.49310 1.00000 0.03344 0.02768 0.06347 0.01300 -0.01081 0.00837 0.04459 0.04086 0.00117 0.00210 0.00192 0.00000 0.01186 0.01065 0.01494 0.01006 0.01006 0.00889 0.00562 H018 0.21298 0.02510 0.54921 1.00000 0.05351 0.00000 0.00000 C019 0.13860 0.46430 0.41582 1.00000 0.03727 0.01637 0.03893 0.00552 0.03105 0.00296 0.02748 0.03711 0.00104 0.00174 0.00150 0.00000 0.01074 0.00841 0.01074 0.00745 0.00877 0.00759 0.00422 C020 0.25014 0.37653 0.51873 1.00000 0.02264 0.02599 0.03198 -0.00218 0.00349 -0.00769 0.02720 0.03226 0.00101 0.00185 0.00145 0.00000 0.00923 0.00940 0.01008 0.00791 0.00755 0.00758 0.00398 H020 0.30008 0.34131 0.53923 1.00000 0.03264 0.00000 0.00000 C021 0.24817 0.42923 0.31760 1.00000 0.03127 0.01307 0.02805 0.00051 0.00627 -0.00127 0.02412 0.03277 0.00100 0.00168 0.00143 0.00000 0.00998 0.00820 0.00961 0.00702 0.00753 0.00713 0.00381 H021 0.21565 0.44572 0.24985 1.00000 0.02895 0.00000 0.00000 C022 0.13221 0.44384 0.52703 1.00000 0.04571 0.03794 0.03183 -0.01620 0.01734 -0.00169 0.03715 0.03706 0.00120 0.00211 0.00157 0.00000 0.01234 0.01154 0.01091 0.00906 0.00932 0.00959 0.00484 H022 0.08824 0.46459 0.55369 1.00000 0.04458 0.00000 0.00000 C023 0.19693 0.39139 0.58796 1.00000 0.02606 0.03996 0.04315 -0.02091 0.00608 -0.00418 0.03656 0.03460 0.00105 0.00213 0.00172 0.00000 0.01025 0.01174 0.01193 0.00957 0.00875 0.00876 0.00484 H023 0.20550 0.36877 0.66219 1.00000 0.04387 0.00000 0.00000 C024 0.21514 0.42333 0.41545 1.00000 0.03860 0.02128 0.03309 -0.00971 0.01402 -0.00011 0.03004 0.03487 0.00108 0.00190 0.00150 0.00000 0.01117 0.00941 0.01056 0.00785 0.00861 0.00808 0.00430 C025 0.10239 0.09065 0.50211 1.00000 0.03354 0.05218 0.02354 0.02031 0.00080 -0.00351 0.03717 0.03846 0.00110 0.00227 0.00154 0.00000 0.01109 0.01317 0.00994 0.00915 0.00813 0.00956 0.00499 H025 0.08351 0.07906 0.56579 1.00000 0.04461 0.00000 0.00000 C027 0.47036 0.06366 0.14179 1.00000 0.03570 0.03683 0.04499 -0.00262 0.00755 0.01303 0.03931 0.03995 0.00115 0.00223 0.00171 0.00000 0.01139 0.01181 0.01246 0.00976 0.00945 0.00941 0.00494 H027 0.49561 -0.01639 0.12358 1.00000 0.04717 0.00000 0.00000 C028 0.10874 0.13702 0.32947 1.00000 0.03968 0.02756 0.03913 -0.01287 0.00519 -0.00029 0.03591 0.03584 0.00113 0.00200 0.00169 0.00000 0.01151 0.01021 0.01143 0.00882 0.00905 0.00887 0.00465 H028 0.09542 0.16453 0.25625 1.00000 0.04309 0.00000 0.00000 C029 0.17961 0.08276 0.38253 1.00000 0.05027 0.03249 0.03996 -0.00568 0.00790 0.00273 0.04113 0.03938 0.00129 0.00214 0.00169 0.00000 0.01323 0.01149 0.01233 0.00939 0.00997 0.00982 0.00508 H029 0.22231 0.06592 0.35189 1.00000 0.04936 0.00000 0.00000 C030 0.14189 0.72933 0.28095 1.00000 0.05176 0.02410 0.04671 -0.00024 0.01694 -0.00304 0.03989 0.03986 0.00121 0.00205 0.00170 0.00000 0.01278 0.01014 0.01207 0.00912 0.00982 0.00929 0.00481 H03A 0.13748 0.83015 0.27174 1.00000 0.05983 0.00000 0.00000 H03B 0.14493 0.68610 0.21229 1.00000 0.05983 0.00000 0.00000 H03C 0.18759 0.70737 0.33470 1.00000 0.05983 0.00000 0.00000 C031 0.39834 0.17571 0.25813 1.00000 0.02164 0.02675 0.07015 -0.00542 -0.00490 0.01068 0.04164 0.03773 0.00107 0.00204 0.00194 0.00000 0.01005 0.01044 0.01561 0.01003 0.00978 0.00815 0.00546 H031 0.37472 0.16845 0.31789 1.00000 0.04997 0.00000 0.00000 C032 0.33673 0.77321 0.02547 1.00000 0.04865 0.04062 0.03070 0.02642 0.00544 0.00438 0.04041 0.04053 0.00120 0.00217 0.00153 0.00000 0.01250 0.01155 0.01090 0.00949 0.00923 0.01032 0.00501 H032 0.32775 0.84937 -0.02292 1.00000 0.04849 0.00000 0.00000 Final Structure Factor Calculation for S93 in P2(1)/c Total number of l.s. parameters = 283 Maximum vector length = 511 Memory required = 3619 / 24017 wR2 = 0.4644 before cycle 13 for 3808 data and 0 / 283 parameters GooF = S = 1.100; Restrained GooF = 1.100 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0649 * P )^2 + 153.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.1849 for 2456 Fo > 4sig(Fo) and 0.2344 for all 3808 data wR2 = 0.4644, GooF = S = 1.100, Restrained GooF = 1.100 for all data Occupancy sum of asymmetric unit = 31.00 for non-hydrogen and 27.00 for hydrogen atoms Principal mean square atomic displacements U 0.0273 0.0184 0.0170 Fe01 0.0294 0.0282 0.0026 C002 0.0382 0.0200 0.0097 C003 0.0442 0.0249 0.0157 C004 0.0486 0.0251 0.0178 C005 0.0500 0.0443 0.0165 N006 0.0726 0.0395 0.0156 C007 0.0508 0.0232 0.0210 C008 0.0397 0.0286 0.0155 C009 0.0483 0.0237 0.0179 C010 0.0616 0.0241 0.0180 C011 0.0498 0.0267 0.0159 C012 0.0478 0.0307 0.0216 C013 0.0399 0.0262 0.0033 C014 0.0465 0.0262 0.0127 C015 0.0480 0.0354 0.0225 C016 0.0745 0.0280 0.0190 C017 0.0810 0.0383 0.0145 C018 0.0579 0.0162 0.0084 C019 0.0332 0.0321 0.0163 C020 0.0314 0.0280 0.0129 C021 0.0544 0.0421 0.0149 C022 0.0627 0.0270 0.0200 C023 0.0431 0.0326 0.0144 C024 0.0654 0.0331 0.0130 C025 0.0519 0.0435 0.0226 C027 0.0493 0.0392 0.0192 C028 0.0520 0.0424 0.0289 C029 0.0554 0.0406 0.0237 C030 0.0799 0.0319 0.0131 C031 0.0627 0.0497 0.0088 C032 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.014 0.024 0.033 0.042 0.053 0.066 0.081 0.102 0.142 1.000 Number in group 382. 412. 375. 363. 371. 382. 378. 387. 379. 379. GooF 1.005 1.189 1.155 1.265 1.194 0.975 1.069 1.037 0.910 1.154 K 8.016 3.976 2.394 2.030 1.584 1.202 1.179 1.106 1.037 0.998 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.06 1.14 1.26 1.44 1.79 inf Number in group 390. 371. 386. 383. 377. 379. 384. 380. 374. 384. GooF 0.745 0.769 0.901 0.837 1.083 1.083 1.306 1.107 1.415 1.474 K 1.029 1.011 1.125 1.121 1.197 1.165 1.190 1.135 1.130 1.029 R1 0.374 0.306 0.273 0.239 0.243 0.233 0.219 0.189 0.179 0.166 Recommended weighting scheme: WGHT 0.0683 154.5033 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)/su Fc/Fc(max) Resolution(A) -4 3 10 3576.28 135.67 6.83 0.039 1.18 -5 4 2 4209.77 214.38 6.44 0.049 1.97 -2 0 10 3820.62 350.28 6.19 0.063 1.27 -6 5 2 5447.67 507.43 6.10 0.076 1.61 1 0 10 3704.94 454.47 5.91 0.072 1.22 1 1 5 2674.60 178.04 5.82 0.045 2.33 -1 6 2 2999.31 311.81 5.69 0.059 1.56 -12 2 10 2287.83 66.01 5.69 0.027 1.04 0 0 12 3258.91 142.43 5.63 0.040 1.04 -4 6 2 3218.96 451.66 5.34 0.071 1.49 -2 6 2 4148.28 847.08 5.32 0.098 1.55 5 4 2 4438.36 611.38 5.20 0.083 1.84 1 2 2 1955.01 26.38 5.05 0.017 3.63 7 5 2 2654.25 95.89 5.01 0.033 1.45 3 1 2 5925.62 896.84 4.95 0.100 3.61 -5 2 10 2809.25 452.37 4.89 0.071 1.22 -3 5 2 7175.45 138.00 4.84 0.039 1.79 3 1 10 1900.56 141.72 4.75 0.040 1.16 -2 3 8 4364.15 931.95 4.74 0.102 1.42 -5 6 2 3844.87 935.10 4.74 0.103 1.45 -6 3 10 3371.69 785.82 4.64 0.094 1.16 0 2 5 1927.55 210.74 4.58 0.049 2.21 10 1 2 2741.65 46.23 4.56 0.023 1.59 -8 2 10 3516.69 876.22 4.55 0.099 1.16 -1 1 10 1666.90 127.71 4.45 0.038 1.25 -7 2 5 1291.60 36.13 4.42 0.020 1.84 2 4 3 2512.76 457.02 4.32 0.072 1.98 4 6 10 1556.18 39.78 4.25 0.021 0.93 -2 2 10 1540.55 145.53 4.20 0.040 1.23 6 5 10 1265.44 30.25 4.08 0.018 0.93 -7 1 2 19724.41 9554.06 3.99 0.328 2.45 6 5 7 1413.35 79.79 3.99 0.030 1.13 2 1 10 2770.26 736.91 3.86 0.091 1.19 -1 0 12 1512.04 122.13 3.85 0.037 1.05 4 1 0 63137.83 44344.78 3.85 0.707 4.02 -9 2 10 1652.69 211.99 3.84 0.049 1.14 0 1 10 1673.88 272.84 3.83 0.055 1.23 5 5 8 1444.06 6.78 3.81 0.009 1.09 -3 1 7 2285.86 458.94 3.80 0.072 1.78 -11 0 10 918.11 9.76 3.77 0.010 1.10 -1 0 10 1165.84 36.76 3.77 0.020 1.26 6 1 10 1447.00 174.24 3.76 0.044 1.06 0 4 7 1196.66 80.97 3.76 0.030 1.43 -9 7 2 1370.66 92.61 3.70 0.032 1.13 -2 4 5 1424.96 214.75 3.63 0.049 1.75 3 1 5 1590.53 300.41 3.57 0.058 2.09 0 0 10 817.22 7.77 3.53 0.009 1.24 11 0 10 1346.27 139.19 3.51 0.040 0.90 2 8 2 1250.48 155.81 3.49 0.042 1.17 3 5 2 6490.67 3218.83 3.47 0.190 1.73 Bond lengths and angles Fe01 - Distance Angles C018 2.0260 (0.0199) C019 2.0305 (0.0170) 176.10 (0.89) C022 2.0322 (0.0192) 141.85 (0.92) 42.04 (0.75) C024 2.0353 (0.0192) 136.58 (0.83) 41.55 (0.71) 68.23 (0.76) C025 2.0434 (0.0201) 38.99 (0.86) 142.79 (0.77) 115.72 (0.85) 175.52 (0.83) C020 2.0428 (0.0173) 111.03 (0.79) 69.58 (0.77) 67.21 (0.80) 40.41 (0.74) 138.07 (0.74) C011 2.0625 (0.0187) 67.42 (0.79) 112.11 (0.77) 112.69 (0.84) 142.03 (0.77) 39.56 (0.73) 177.54 (0.78) C023 2.0656 (0.0189) 113.72 (0.92) 69.40 (0.84) 38.75 (0.80) 68.49 (0.80) 113.02 (0.85) 41.11 (0.73) 137.34 (0.83) C029 2.0795 (0.0208) 41.41 (0.90) 134.69 (0.78) 176.73 (0.85) 109.20 (0.79) 66.93 (0.88) 112.32 (0.83) 67.92 (0.86) C028 2.0805 (0.0192) 67.99 (0.88) 108.99 (0.82) 138.58 (0.83) 111.98 (0.79) 66.73 (0.84) 140.93 (0.78) 40.72 (0.81) Fe01 - C018 C019 C022 C024 C025 C020 C011 C002 - Distance Angles C003 1.3951 (0.0241) C015 1.4042 (0.0247) 121.30 (1.43) C014 1.5036 (0.0207) 117.47 (1.50) 121.12 (1.53) C002 - C003 C015 C003 - Distance Angles C002 1.3951 (0.0241) C031 1.4074 (0.0277) 123.74 (1.57) C004 1.4329 (0.0234) 119.42 (1.61) 116.65 (1.74) C003 - C002 C031 C004 - Distance Angles C009 1.3943 (0.0265) C012 1.4289 (0.0252) 121.62 (1.61) C003 1.4329 (0.0234) 117.87 (1.65) 120.50 (1.77) C004 - C009 C012 C005 - Distance Angles C016 1.3679 (0.0267) C015 1.4417 (0.0250) 119.33 (1.80) H005 0.9500 120.34 120.34 C005 - C016 C015 N006 - Distance Angles C007 1.4281 (0.0264) C010 1.4771 (0.0247) 114.02 (1.69) C030 1.4998 (0.0246) 109.50 (1.59) 110.51 (1.50) N006 - C007 C010 C007 - Distance Angles N006 1.4281 (0.0264) H00A 0.9800 109.47 H00B 0.9800 109.47 109.47 H00C 0.9800 109.47 109.47 109.47 C007 - N006 H00A H00B C008 - Distance Angles C032 1.3429 (0.0287) C013 1.4212 (0.0274) 121.54 (1.72) H008 0.9500 119.23 119.23 C008 - C032 C013 C009 - Distance Angles C004 1.3943 (0.0265) C013 1.3989 (0.0268) 123.41 (1.62) H009 0.9500 118.29 118.29 C009 - C004 C013 C010 - Distance Angles N006 1.4771 (0.0247) C019 1.5010 (0.0256) 116.72 (1.61) H01A 0.9900 108.11 108.11 H01B 0.9900 108.11 108.11 107.31 C010 - N006 C019 H01A C011 - Distance Angles C025 1.3897 (0.0257) C028 1.4417 (0.0286) 106.47 (1.72) Fe01 2.0625 (0.0187) 69.47 (1.13) 70.31 (1.06) H011 0.9500 126.77 126.77 125.06 C011 - C025 C028 Fe01 C012 - Distance Angles C027 1.3761 (0.0287) C004 1.4289 (0.0252) 120.25 (1.71) H012 0.9500 119.88 119.88 C012 - C027 C004 C013 - Distance Angles C009 1.3989 (0.0268) C015 1.4151 (0.0265) 117.83 (1.80) C008 1.4212 (0.0274) 122.48 (1.71) 119.68 (1.81) C013 - C009 C015 C014 - Distance Angles C021 1.3242 (0.0242) C002 1.5036 (0.0207) 122.99 (1.52) H014 0.9500 118.51 118.51 C014 - C021 C002 C015 - Distance Angles C002 1.4042 (0.0246) C013 1.4151 (0.0265) 119.81 (1.69) C005 1.4417 (0.0250) 121.91 (1.67) 118.28 (1.77) C015 - C002 C013 C016 - Distance Angles C005 1.3679 (0.0267) C032 1.4308 (0.0274) 121.68 (1.93) H016 0.9500 119.16 119.16 C016 - C005 C032 C017 - Distance Angles C027 1.3616 (0.0309) C031 1.3919 (0.0274) 123.24 (2.16) H017 0.9500 118.38 118.38 C017 - C027 C031 C018 - Distance Angles C025 1.3583 (0.0294) C029 1.4525 (0.0315) 107.93 (1.78) Fe01 2.0260 (0.0199) 71.19 (1.23) 71.27 (1.18) H018 0.9500 126.04 126.04 123.16 C018 - C025 C029 Fe01 C019 - Distance Angles C024 1.4421 (0.0253) C022 1.4574 (0.0258) 103.77 (1.68) C010 1.5010 (0.0256) 130.91 (1.59) 125.25 (1.64) Fe01 2.0305 (0.0169) 69.40 (1.02) 69.04 (1.05) 127.27 (1.34) C019 - C024 C022 C010 C020 - Distance Angles C024 1.4084 (0.0263) C023 1.4425 (0.0263) 108.10 (1.65) Fe01 2.0428 (0.0172) 69.51 (1.05) 70.30 (1.01) H020 0.9500 125.95 125.95 125.82 C020 - C024 C023 Fe01 C021 - Distance Angles C014 1.3242 (0.0242) C024 1.4913 (0.0251) 122.19 (1.64) H021 0.9500 118.91 118.91 C021 - C014 C024 C022 - Distance Angles C023 1.3600 (0.0291) C019 1.4574 (0.0258) 111.69 (1.80) Fe01 2.0322 (0.0192) 71.95 (1.16) 68.92 (0.99) H022 0.9500 124.15 124.15 126.61 C022 - C023 C019 Fe01 C023 - Distance Angles C022 1.3600 (0.0290) C020 1.4425 (0.0263) 107.15 (1.86) Fe01 2.0656 (0.0188) 69.29 (1.12) 68.60 (1.02) H023 0.9500 126.43 126.43 127.23 C023 - C022 C020 Fe01 C024 - Distance Angles C020 1.4084 (0.0263) C019 1.4421 (0.0253) 109.24 (1.58) C021 1.4913 (0.0251) 127.63 (1.69) 123.12 (1.69) Fe01 2.0353 (0.0191) 70.08 (1.04) 69.05 (1.01) 126.02 (1.23) C024 - C020 C019 C021 C025 - Distance Angles C018 1.3583 (0.0294) C011 1.3897 (0.0257) 111.34 (1.87) Fe01 2.0434 (0.0201) 69.81 (1.20) 70.96 (1.11) H025 0.9500 124.33 124.33 126.52 C025 - C018 C011 Fe01 C027 - Distance Angles C017 1.3616 (0.0309) C012 1.3761 (0.0287) 118.93 (1.88) H027 0.9500 120.53 120.53 C027 - C017 C012 C028 - Distance Angles C029 1.4190 (0.0293) C011 1.4417 (0.0286) 107.97 (1.83) Fe01 2.0805 (0.0191) 70.02 (1.15) 68.97 (1.09) H028 0.9500 126.02 126.01 126.57 C028 - C029 C011 Fe01 C029 - Distance Angles C028 1.4190 (0.0292) C018 1.4525 (0.0315) 106.20 (1.90) Fe01 2.0795 (0.0208) 70.09 (1.14) 67.32 (1.15) H029 0.9500 126.90 126.90 127.21 C029 - C028 C018 Fe01 C030 - Distance Angles N006 1.4998 (0.0246) H03A 0.9800 109.47 H03B 0.9800 109.47 109.47 H03C 0.9800 109.47 109.47 109.47 C030 - N006 H03A H03B C031 - Distance Angles C017 1.3919 (0.0274) C003 1.4074 (0.0278) 120.34 (2.16) H031 0.9500 119.83 119.83 C031 - C017 C003 C032 - Distance Angles C008 1.3429 (0.0288) C016 1.4308 (0.0273) 119.12 (1.72) H032 0.9500 120.44 120.44 C032 - C008 C016 FMAP and GRID set by program FMAP 2 2 23 GRID 22.500 -2 -1 2.500 2 1 R1 = 0.2181 for 3808 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 3.53 at 0.1562 0.2392 0.5586 [ 1.28 A from FE01 ] Deepest hole -1.60 at 0.4660 0.7427 0.3796 [ 1.33 A from C012 ] Mean = 0.00, Rms deviation from mean = 0.24 e/A^3, Highest memory used = 3786 / 31509 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1562 0.2392 0.5586 1.00000 0.05 3.53 1.28 FE01 1.65 C023 1.79 C025 1.90 H023 Q2 1 0.1570 0.2394 0.3577 1.00000 0.05 3.23 1.32 C028 1.32 FE01 1.58 C029 1.68 H028 Q3 1 0.4681 -0.2499 0.2248 1.00000 0.05 2.21 2.37 H017 2.49 C031 2.49 C017 2.51 C003 Q4 1 0.4689 0.7452 0.1271 1.00000 0.05 1.57 2.26 C008 2.27 H012 2.35 H027 2.49 C032 Q5 1 0.1592 0.2487 0.7016 1.00000 0.05 1.42 1.57 H023 1.69 H028 2.16 H021 2.21 C023 Q6 1 0.3300 0.7470 -0.0953 1.00000 0.05 1.03 1.36 H032 1.41 H008 1.54 C032 1.56 C008 Q7 1 0.3380 0.4047 0.0275 1.00000 0.05 0.88 1.49 C009 1.57 C013 2.00 C004 2.11 H009 Q8 1 0.3571 0.0744 0.3139 1.00000 0.05 0.81 0.96 H031 1.50 C031 1.93 H017 1.99 C017 Q9 1 0.2613 0.4225 0.6883 1.00000 0.05 0.81 1.12 H023 1.57 C023 2.17 C020 2.25 H016 Q10 1 0.3489 0.7565 0.3262 1.00000 0.05 0.80 1.36 H005 1.68 H008 1.89 C005 2.28 H032 Q11 1 0.1979 0.4254 0.2672 1.00000 0.05 0.77 0.47 H021 1.00 C021 1.85 C024 2.10 H01A Q12 1 0.3097 0.7952 0.2479 1.00000 0.05 0.77 1.22 H005 1.43 H016 1.46 C005 1.58 C016 Q13 1 0.3528 0.4276 0.6300 1.00000 0.05 0.76 1.57 H020 1.75 C017 1.94 C031 2.10 C027 Q14 1 0.5267 -0.0781 0.3005 1.00000 0.05 0.75 1.66 H017 1.71 C004 1.84 C003 1.98 C009 Q15 1 0.0608 0.7681 0.3048 1.00000 0.05 0.73 0.94 N006 1.39 C007 1.41 H00B 1.60 C030 Q16 1 0.2300 0.0800 0.5592 1.00000 0.05 0.70 0.61 H018 1.20 C018 2.24 C029 2.27 C025 Q17 1 0.3296 0.0829 0.4140 1.00000 0.05 0.70 1.81 H031 1.95 H029 2.09 H009 2.11 C009 Q18 1 0.3803 0.9772 -0.0170 1.00000 0.05 0.69 1.55 H032 1.70 H014 2.23 C032 2.36 C014 Q19 1 0.4736 0.3200 -0.0086 1.00000 0.05 0.67 1.13 H009 1.37 H012 1.62 C009 1.77 C012 Q20 1 0.2393 0.8537 0.4417 1.00000 0.05 0.66 2.05 H03C 2.23 C032 2.26 H018 2.33 H029 Q21 1 0.4922 -0.0983 0.1149 1.00000 0.05 0.66 0.80 H027 1.66 C027 2.02 H012 2.46 C017 Q22 1 0.1317 0.4468 0.4632 1.00000 0.05 0.66 0.66 C019 0.81 C022 1.53 H022 1.76 C024 Q23 1 0.3602 0.5314 -0.1236 1.00000 0.05 0.65 1.51 H008 1.99 C008 2.10 H031 2.11 H009 Q24 1 0.4528 -0.2001 0.3225 1.00000 0.05 0.65 1.86 H017 2.02 C012 2.04 H008 2.14 C004 Q25 1 0.0890 0.6834 0.5421 1.00000 0.05 0.65 1.22 H00C 1.56 H00A 1.70 C007 2.11 H022 Shortest distances between peaks (including symmetry equivalents) 6 10 1.12 10 12 1.16 3 4 1.25 8 23 1.29 17 23 1.36 3 24 1.41 7 17 1.43 8 17 1.46 4 21 1.58 1 5 1.81 14 24 1.85 10 24 1.94 5 11 1.94 9 13 1.95 6 12 1.99 2 5 2.00 1 16 2.03 6 20 2.04 7 16 2.08 3 14 2.09 8 9 2.10 4 19 2.10 3 21 2.13 10 23 2.14 6 23 2.20 13 18 2.23 14 21 2.32 8 13 2.33 2 11 2.33 1 22 2.33 12 23 2.38 7 23 2.38 18 21 2.45 19 24 2.47 2 22 2.50 6 18 2.52 5 9 2.53 23 24 2.53 1 2 2.56 12 24 2.57 4 24 2.62 16 20 2.67 22 25 2.67 19 21 2.67 6 24 2.69 7 19 2.72 20 23 2.73 3 10 2.74 17 19 2.75 4 14 2.81 17 20 2.81 7 8 2.82 14 19 2.83 11 16 2.83 16 17 2.84 1 9 2.86 10 20 2.86 9 23 2.87 9 17 2.88 8 12 2.89 9 12 2.91 5 16 2.92 7 14 2.93 8 19 2.93 3 12 2.98 10 18 2.98 11 22 2.99 7 20 3.00 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 0.00: Analyse other restraints etc. 1.19: 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 4.56: Structure factors and derivatives 3.91: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.58: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.11: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s93 finished at 15:47:16 Total CPU time: 10.5 secs + 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