+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 06skc0060p-1 started at 14:34:03 on 10-Oct-2006 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 06skc0060p-1 in P-1 CELL 0.71073 6.5398 9.4992 10.2235 91.506 91.388 107.346 ZERR 2.00 0.0002 0.0004 0.0003 0.002 0.002 0.002 LATT 1 SFAC C H N O UNIT 20 40 4 10 V = 605.68 F(000) = 268.0 Mu = 0.11 mm-1 Cell Wt = 496.56 Rho = 1.361 MERG 2 OMIT -3.00 55.00 OMIT 0 0 3 OMIT 1 0 1 OMIT 0 0 1 OMIT 0 1 3 OMIT 1 -1 2 OMIT 1 0 0 EXTI 0.03193 DFIX 0.84 0.02 O1W H1W O1W H2W DANG 1.35 0.02 H1W H2W HTAB O1W O1A EQIV_$1 -x, -y, -z+1 HTAB N21 O1B_$1 EQIV_$2 x+1, y, z HTAB O1W O1B_$2 FMAP 2 PLAN 10 SIZE 0.21 0.28 0.39 ACTA BOND $H WGHT 0.04910 0.28060 L.S. 4 TEMP -153.00 FVAR 1.74886 MOLE 1 C1 1 0.248053 0.159998 0.338316 11.00000 0.01898 0.02021 = 0.01894 0.00013 0.00141 0.00196 C2 1 0.122076 0.098440 0.208526 11.00000 0.02175 0.02088 = 0.01929 -0.00121 0.00126 0.00424 AFIX 13 H2 2 0.051321 0.172449 0.178662 11.00000 -1.20000 AFIX 0 C3 1 0.274569 0.081907 0.102810 11.00000 0.02545 0.02496 = 0.02119 -0.00298 0.00142 0.00556 AFIX 23 H3A 2 0.349480 0.010451 0.130085 11.00000 -1.20000 H3B 2 0.192043 0.043322 0.020350 11.00000 -1.20000 AFIX 0 C4 1 0.436257 0.228491 0.080228 11.00000 0.03066 0.02328 = 0.01806 0.00021 0.00328 0.00487 C5 1 0.794441 0.351811 0.035929 11.00000 0.03059 0.03329 = 0.03804 -0.00214 0.00523 0.00158 AFIX 137 H5A 2 0.743294 0.414992 -0.022712 11.00000 -1.50000 H5B 2 0.919862 0.331204 -0.000989 11.00000 -1.50000 H5C 2 0.834096 0.402190 0.121830 11.00000 -1.50000 AFIX 0 C22 1 -0.408129 -0.159966 0.302087 11.00000 0.01759 0.02142 = 0.02239 -0.00038 -0.00096 0.00713 AFIX 23 H22A 2 -0.519955 -0.144248 0.359268 11.00000 -1.20000 H22B 2 -0.470467 -0.181906 0.211938 11.00000 -1.20000 AFIX 0 C23 1 -0.220365 -0.021211 0.303821 11.00000 0.02002 0.01925 = 0.02264 -0.00142 0.00086 0.00611 AFIX 23 H23A 2 -0.267891 0.060842 0.269593 11.00000 -1.20000 H23B 2 -0.165691 0.005752 0.395055 11.00000 -1.20000 AFIX 0 C25 1 0.023612 -0.162226 0.276736 11.00000 0.01806 0.02436 = 0.02359 -0.00198 0.00150 0.00851 AFIX 23 H25A 2 0.075696 -0.137102 0.368643 11.00000 -1.20000 H25B 2 0.143687 -0.174925 0.225369 11.00000 -1.20000 AFIX 0 C26 1 -0.160161 -0.305030 0.270679 11.00000 0.02362 0.02106 = 0.02236 -0.00307 0.00250 0.00958 AFIX 23 H26A 2 -0.208677 -0.331968 0.178425 11.00000 -1.20000 H26B 2 -0.110532 -0.385537 0.306349 11.00000 -1.20000 AFIX 0 C27 1 -0.525329 -0.425363 0.342512 11.00000 0.02527 0.02136 = 0.02753 -0.00122 -0.00102 0.00011 AFIX 137 H27A 2 -0.582200 -0.446890 0.252217 11.00000 -1.50000 H27B 2 -0.638051 -0.412795 0.398978 11.00000 -1.50000 H27C 2 -0.476436 -0.507293 0.372846 11.00000 -1.50000 AFIX 0 N21 3 -0.342179 -0.287445 0.347815 11.00000 0.01937 0.01754 = 0.01862 -0.00172 -0.00069 0.00441 AFIX 13 H21 2 -0.294484 -0.267535 0.434714 11.00000 -1.20000 AFIX 0 N24 3 -0.048363 -0.042575 0.223914 11.00000 0.01829 0.01972 = 0.01999 -0.00106 0.00153 0.00464 O1A 4 0.416015 0.130045 0.364201 11.00000 0.02403 0.03811 = 0.03088 -0.00939 -0.00317 0.01433 O1B 4 0.166146 0.236376 0.411962 11.00000 0.02466 0.02461 = 0.02172 -0.00481 -0.00238 0.00913 O4A 4 0.626731 0.214979 0.050144 11.00000 0.02592 0.02676 = 0.03416 -0.00173 0.00544 0.00361 O4B 4 0.398421 0.345690 0.086131 11.00000 0.03690 0.03242 = 0.04507 0.00525 0.01308 0.01249 MOLE 2 O1W 4 0.815460 0.354328 0.390181 11.00000 0.03219 0.03065 = 0.07669 -0.00796 -0.00803 0.01471 H1W 2 0.703500 0.280901 0.382115 11.00000 0.07783 H2W 2 0.921353 0.324737 0.392090 11.00000 0.05785 HKLF 4 Covalent radii and connectivity table for 06skc0060p-1 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1A O1B C2 C2 - N24 C3 C1 C3 - C4 C2 C4 - O4B O4A C3 C5 - O4A C22 - N21 C23 C23 - N24 C22 C25 - N24 C26 C26 - N21 C25 C27 - N21 N21 - C22 C27 C26 N24 - C25 C23 C2 O1A - C1 O1B - C1 O4A - C4 C5 O4B - C4 O1W - no bonds found Operators for generating equivalent atoms: $1 -x, -y, -z+1 $2 x+1, y, z 13267 Reflections read, of which 16 rejected -8 =< h =< 8, -12 =< k =< 12, -13 =< l =< 12, Max. 2-theta = 55.00 0 Systematic absence violations 0 Inconsistent equivalents 2778 Unique reflections, of which 0 suppressed R(int) = 0.0375 R(sigma) = 0.0333 Friedel opposites merged Maximum memory for data reduction = 2025 / 27995 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 = 2496 / 205650 wR2 = 0.1151 before cycle 1 for 2778 data and 165 / 165 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 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 0.014 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.035; Restrained GooF = 1.035 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0491 * P )^2 + 0.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.74886 0.00480 0.000 OSF 2 0.03193 0.00738 0.000 EXTI Mean shift/esd = 0.002 Maximum = 0.008 for U13 O1A Max. shift = 0.000 A for H2W Max. dU = 0.000 for O1W Least-squares cycle 2 Maximum vector length = 511 Memory required = 2496 / 205650 wR2 = 0.1151 before cycle 2 for 2778 data and 165 / 165 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 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 0.014 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.035; Restrained GooF = 1.035 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0491 * P )^2 + 0.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.74886 0.00480 0.001 OSF 2 0.03193 0.00738 0.000 EXTI Mean shift/esd = 0.001 Maximum = 0.003 for U13 O1A Max. shift = 0.000 A for H2W Max. dU = 0.000 for O1W Least-squares cycle 3 Maximum vector length = 511 Memory required = 2496 / 205650 wR2 = 0.1151 before cycle 3 for 2778 data and 165 / 165 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 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 0.014 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.035; Restrained GooF = 1.035 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0491 * P )^2 + 0.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.74886 0.00480 0.000 OSF 2 0.03193 0.00738 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for EXTI Max. shift = 0.000 A for H1W Max. dU = 0.000 for H1W Least-squares cycle 4 Maximum vector length = 511 Memory required = 2496 / 205650 wR2 = 0.1151 before cycle 4 for 2778 data and 165 / 165 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 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 0.014 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.035; Restrained GooF = 1.035 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0491 * P )^2 + 0.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.74886 0.00480 0.000 OSF 2 0.03193 0.00738 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y O4B Max. shift = 0.000 A for H1W Max. dU = 0.000 for H2W Largest correlation matrix elements 0.560 EXTI / OSF 0.560 x H2W / x H1W Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.0513 0.1724 0.1787 13 1.000 0.000 C2 N24 C3 C1 H3A 0.3495 0.0105 0.1301 23 0.990 0.000 C3 C4 C2 H3B 0.1920 0.0433 0.0203 23 0.990 0.000 C3 C4 C2 H5A 0.7433 0.4150 -0.0227 137 0.980 0.000 C5 O4A H5A H5B 0.9199 0.3312 -0.0010 137 0.980 0.000 C5 O4A H5A H5C 0.8341 0.4022 0.1218 137 0.980 0.000 C5 O4A H5A H22A -0.5200 -0.1442 0.3593 23 0.990 0.000 C22 N21 C23 H22B -0.4705 -0.1819 0.2119 23 0.990 0.000 C22 N21 C23 H23A -0.2679 0.0608 0.2696 23 0.990 0.000 C23 N24 C22 H23B -0.1657 0.0058 0.3951 23 0.990 0.000 C23 N24 C22 H25A 0.0757 -0.1371 0.3686 23 0.990 0.000 C25 N24 C26 H25B 0.1437 -0.1749 0.2254 23 0.990 0.000 C25 N24 C26 H26A -0.2087 -0.3320 0.1784 23 0.990 0.000 C26 N21 C25 H26B -0.1105 -0.3855 0.3063 23 0.990 0.000 C26 N21 C25 H27A -0.5822 -0.4469 0.2522 137 0.980 0.000 C27 N21 H27A H27B -0.6381 -0.4128 0.3990 137 0.980 0.000 C27 N21 H27A H27C -0.4764 -0.5073 0.3728 137 0.980 0.000 C27 N21 H27A H21 -0.2945 -0.2675 0.4347 13 0.930 0.000 N21 C22 C27 C26 06skc0060p-1 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.24805 0.16000 0.33832 1.00000 0.01898 0.02021 0.01894 0.00013 0.00141 0.00196 0.02023 0.00277 0.00023 0.00016 0.00014 0.00000 0.00072 0.00072 0.00071 0.00055 0.00056 0.00059 0.00032 C2 0.12208 0.09844 0.20853 1.00000 0.02175 0.02088 0.01929 -0.00121 0.00126 0.00424 0.02113 0.00281 0.00023 0.00016 0.00014 0.00000 0.00074 0.00074 0.00071 0.00056 0.00057 0.00061 0.00033 H2 0.05132 0.17245 0.17866 1.00000 0.02536 0.00000 0.00000 C3 0.27457 0.08191 0.10281 1.00000 0.02546 0.02496 0.02119 -0.00298 0.00142 0.00556 0.02436 0.00299 0.00025 0.00017 0.00015 0.00000 0.00078 0.00079 0.00074 0.00059 0.00060 0.00064 0.00034 H3A 0.34948 0.01045 0.13008 1.00000 0.02923 0.00000 0.00000 H3B 0.19204 0.04332 0.02035 1.00000 0.02923 0.00000 0.00000 C4 0.43626 0.22849 0.08023 1.00000 0.03066 0.02328 0.01806 0.00021 0.00328 0.00487 0.02466 0.00306 0.00026 0.00017 0.00014 0.00000 0.00084 0.00078 0.00071 0.00057 0.00060 0.00066 0.00034 C5 0.79444 0.35181 0.03593 1.00000 0.03059 0.03329 0.03804 -0.00214 0.00523 0.00158 0.03571 0.00348 0.00029 0.00020 0.00018 0.00000 0.00090 0.00095 0.00096 0.00074 0.00074 0.00075 0.00042 H5A 0.74329 0.41499 -0.02271 1.00000 0.05356 0.00000 0.00000 H5B 0.91986 0.33120 -0.00099 1.00000 0.05356 0.00000 0.00000 H5C 0.83410 0.40219 0.12183 1.00000 0.05356 0.00000 0.00000 C22 -0.40813 -0.15997 0.30209 1.00000 0.01759 0.02142 0.02239 -0.00038 -0.00096 0.00713 0.02023 0.00284 0.00023 0.00016 0.00014 0.00000 0.00070 0.00074 0.00072 0.00056 0.00055 0.00058 0.00032 H22A -0.51996 -0.14425 0.35927 1.00000 0.02428 0.00000 0.00000 H22B -0.47047 -0.18191 0.21194 1.00000 0.02428 0.00000 0.00000 C23 -0.22036 -0.02121 0.30382 1.00000 0.02002 0.01925 0.02264 -0.00142 0.00086 0.00611 0.02062 0.00284 0.00023 0.00016 0.00014 0.00000 0.00073 0.00072 0.00072 0.00056 0.00057 0.00059 0.00032 H23A -0.26789 0.06084 0.26959 1.00000 0.02474 0.00000 0.00000 H23B -0.16569 0.00575 0.39505 1.00000 0.02474 0.00000 0.00000 C25 0.02361 -0.16223 0.27674 1.00000 0.01805 0.02436 0.02359 -0.00198 0.00150 0.00851 0.02156 0.00289 0.00023 0.00016 0.00015 0.00000 0.00071 0.00077 0.00073 0.00058 0.00057 0.00060 0.00032 H25A 0.07570 -0.13710 0.36864 1.00000 0.02588 0.00000 0.00000 H25B 0.14369 -0.17493 0.22537 1.00000 0.02588 0.00000 0.00000 C26 -0.16016 -0.30503 0.27068 1.00000 0.02362 0.02106 0.02236 -0.00307 0.00250 0.00958 0.02176 0.00294 0.00024 0.00016 0.00015 0.00000 0.00075 0.00073 0.00072 0.00057 0.00058 0.00061 0.00032 H26A -0.20868 -0.33197 0.17843 1.00000 0.02611 0.00000 0.00000 H26B -0.11053 -0.38554 0.30635 1.00000 0.02611 0.00000 0.00000 C27 -0.52533 -0.42536 0.34251 1.00000 0.02527 0.02136 0.02753 -0.00122 -0.00102 0.00011 0.02629 0.00296 0.00025 0.00017 0.00016 0.00000 0.00079 0.00077 0.00080 0.00060 0.00063 0.00063 0.00035 H27A -0.58220 -0.44689 0.25222 1.00000 0.03943 0.00000 0.00000 H27B -0.63805 -0.41279 0.39898 1.00000 0.03943 0.00000 0.00000 H27C -0.47644 -0.50729 0.37285 1.00000 0.03943 0.00000 0.00000 N21 -0.34218 -0.28744 0.34781 1.00000 0.01937 0.01754 0.01862 -0.00172 -0.00069 0.00441 0.01881 0.00230 0.00019 0.00013 0.00012 0.00000 0.00061 0.00061 0.00059 0.00045 0.00046 0.00049 0.00028 H21 -0.29448 -0.26753 0.43471 1.00000 0.02258 0.00000 0.00000 N24 -0.04836 -0.04257 0.22391 1.00000 0.01829 0.01972 0.01999 -0.00106 0.00153 0.00464 0.01958 0.00232 0.00019 0.00013 0.00011 0.00000 0.00060 0.00062 0.00061 0.00047 0.00047 0.00049 0.00028 O1A 0.41601 0.13004 0.36420 1.00000 0.02403 0.03811 0.03088 -0.00939 -0.00317 0.01433 0.03017 0.00217 0.00017 0.00013 0.00011 0.00000 0.00059 0.00067 0.00062 0.00049 0.00046 0.00051 0.00029 O1B 0.16615 0.23638 0.41196 1.00000 0.02466 0.02461 0.02172 -0.00481 -0.00238 0.00913 0.02344 0.00199 0.00016 0.00011 0.00010 0.00000 0.00056 0.00056 0.00054 0.00042 0.00042 0.00045 0.00027 O4A 0.62673 0.21498 0.05014 1.00000 0.02592 0.02676 0.03416 -0.00173 0.00544 0.00361 0.02986 0.00222 0.00018 0.00012 0.00011 0.00000 0.00059 0.00060 0.00064 0.00047 0.00047 0.00047 0.00029 O4B 0.39842 0.34569 0.08613 1.00000 0.03690 0.03242 0.04507 0.00525 0.01308 0.01249 0.03740 0.00262 0.00020 0.00014 0.00013 0.00000 0.00070 0.00068 0.00075 0.00054 0.00057 0.00055 0.00032 O1W 0.81546 0.35433 0.39018 1.00000 0.03220 0.03066 0.07669 -0.00796 -0.00803 0.01471 0.04570 0.00279 0.00023 0.00015 0.00016 0.00000 0.00076 0.00073 0.00106 0.00067 0.00071 0.00064 0.00039 H1W 0.70350 0.28090 0.38211 1.00000 0.07783 0.03929 0.00288 0.00241 0.00283 0.00000 0.00885 H2W 0.92135 0.32474 0.39209 1.00000 0.05785 0.04366 0.00275 0.00247 0.00239 0.00000 0.00720 Final Structure Factor Calculation for 06skc0060p-1 in P-1 Total number of l.s. parameters = 165 Maximum vector length = 511 Memory required = 2331 / 22995 wR2 = 0.1151 before cycle 5 for 2778 data and 0 / 165 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 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 0.014 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.035; Restrained GooF = 1.035 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0491 * P )^2 + 0.28 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0441 for 2117 Fo > 4sig(Fo) and 0.0653 for all 2778 data wR2 = 0.1151, GooF = S = 1.035, Restrained GooF = 1.035 for all data Occupancy sum of asymmetric unit = 17.00 for non-hydrogen and 20.00 for hydrogen atoms Principal mean square atomic displacements U 0.0254 0.0188 0.0165 C1 0.0251 0.0202 0.0181 C2 0.0298 0.0244 0.0189 C3 0.0337 0.0228 0.0175 C4 0.0476 0.0340 0.0255 C5 0.0236 0.0207 0.0164 C22 0.0238 0.0200 0.0180 C23 0.0269 0.0220 0.0158 C25 0.0257 0.0247 0.0148 C26 0.0334 0.0282 0.0173 C27 0.0206 0.0203 0.0155 N21 0.0227 0.0182 0.0179 N24 0.0465 0.0239 0.0201 O1A 0.0302 0.0226 0.0176 O1B 0.0395 0.0274 0.0227 O4A 0.0530 0.0312 0.0279 O4B 0.0806 0.0327 0.0238 O1W Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.013 0.026 0.038 0.053 0.069 0.088 0.117 0.153 0.234 1.000 Number in group 292. 279. 278. 275. 273. 271. 281. 273. 277. 279. GooF 0.945 0.990 1.032 1.173 0.992 1.049 1.092 0.994 1.075 0.994 K 1.755 0.914 0.934 0.941 0.933 0.981 0.997 1.008 1.015 1.014 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.63 inf Number in group 281. 285. 272. 277. 273. 283. 274. 279. 275. 279. GooF 0.971 0.919 0.914 0.972 0.900 0.977 1.030 1.054 1.070 1.435 K 0.997 1.024 1.031 1.007 1.003 1.012 1.012 1.016 1.025 1.002 R1 0.177 0.129 0.131 0.092 0.073 0.058 0.048 0.041 0.035 0.033 Recommended weighting scheme: WGHT 0.0491 0.2806 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) -1 1 1 6.59 1.15 5.03 0.018 5.23 1 -2 1 16.84 8.30 4.30 0.048 4.00 -3 -7 1 13.53 26.25 3.90 0.085 0.98 -7 5 3 23.85 39.47 3.77 0.105 0.89 -1 2 3 454.33 563.11 3.74 0.395 2.66 3 -4 2 3.30 0.59 3.68 0.013 1.72 -2 2 1 1.92 6.51 3.62 0.042 2.91 0 3 2 13.28 22.40 3.56 0.079 2.56 -4 2 3 4.56 0.84 3.55 0.015 1.49 8 -4 1 14.62 29.02 3.44 0.090 0.81 2 -5 4 13.43 6.81 3.42 0.043 1.49 2 -3 1 441.71 365.38 3.40 0.318 2.51 3 -1 1 33.65 23.24 3.35 0.080 2.11 3 -7 3 -0.08 4.28 3.35 0.034 1.21 0 1 1 54.38 40.14 3.30 0.105 6.66 -1 -4 2 2.44 0.19 3.30 0.007 1.85 1 -1 1 1236.39 1473.85 3.27 0.639 5.19 3 -8 1 17.99 27.85 3.26 0.088 1.14 -3 -6 3 47.59 64.66 3.20 0.134 1.04 2 0 5 16.17 24.89 3.17 0.083 1.68 -3 -2 12 -8.31 13.65 3.15 0.062 0.77 2 0 11 0.01 7.86 3.06 0.047 0.88 2 -8 2 0.96 5.51 3.06 0.039 1.16 -2 -10 2 121.64 93.26 2.98 0.161 0.80 -4 -2 4 3.49 0.75 2.97 0.014 1.22 1 -1 8 9.77 3.35 2.94 0.030 1.25 1 4 10 7.08 13.28 2.93 0.061 0.89 4 -4 6 2.83 0.11 2.93 0.005 1.13 0 1 4 71.73 56.40 2.92 0.125 2.44 1 4 1 7.58 13.52 2.92 0.061 1.90 -3 7 0 12.32 7.10 2.89 0.044 1.28 -5 0 2 6.11 2.33 2.86 0.025 1.22 -1 -11 2 189.10 148.95 2.83 0.203 0.78 -1 2 5 1.38 0.03 2.81 0.003 1.84 -5 3 5 91.92 73.13 2.81 0.142 1.11 1 -4 4 194.74 163.04 2.77 0.213 1.76 0 4 6 5.98 2.73 2.77 0.027 1.34 2 -5 2 180.29 150.85 2.75 0.204 1.72 -5 3 7 9.47 4.61 2.70 0.036 0.98 4 -12 1 130.77 97.86 2.68 0.165 0.78 0 0 2 712.90 828.41 2.67 0.479 5.11 -1 0 1 408.00 484.93 2.65 0.367 5.41 2 3 0 223.51 189.75 2.65 0.229 1.90 0 1 7 11.02 6.66 2.64 0.043 1.43 -3 1 6 17.94 11.78 2.63 0.057 1.36 -4 2 7 8.45 4.07 2.62 0.034 1.10 -7 -1 2 3.41 9.69 2.61 0.052 0.86 -4 -4 2 17.49 25.07 2.61 0.083 1.12 5 0 8 0.43 3.58 2.61 0.032 0.88 -3 5 11 19.58 11.81 2.61 0.057 0.80 Bond lengths and angles C1 - Distance Angles O1A 1.2385 (0.0018) O1B 1.2660 (0.0018) 124.79 (0.13) C2 1.5493 (0.0020) 119.11 (0.13) 116.09 (0.13) C1 - O1A O1B C2 - Distance Angles N24 1.4801 (0.0018) C3 1.5245 (0.0020) 110.65 (0.11) C1 1.5493 (0.0020) 112.91 (0.11) 110.52 (0.12) H2 1.0000 107.51 107.51 107.51 C2 - N24 C3 C1 C3 - Distance Angles C4 1.5037 (0.0021) C2 1.5245 (0.0020) 110.23 (0.12) H3A 0.9900 109.61 109.61 H3B 0.9900 109.61 109.61 108.14 C3 - C4 C2 H3A C4 - Distance Angles O4B 1.2107 (0.0020) O4A 1.3321 (0.0020) 123.37 (0.14) C3 1.5037 (0.0021) 124.38 (0.15) 112.24 (0.13) C4 - O4B O4A C5 - Distance Angles O4A 1.4426 (0.0020) H5A 0.9800 109.47 H5B 0.9800 109.47 109.47 H5C 0.9800 109.47 109.47 109.47 C5 - O4A H5A H5B C22 - Distance Angles N21 1.4840 (0.0018) C23 1.5093 (0.0020) 111.31 (0.11) H22A 0.9900 109.37 109.37 H22B 0.9900 109.37 109.37 107.99 C22 - N21 C23 H22A C23 - Distance Angles N24 1.4648 (0.0018) C22 1.5093 (0.0020) 110.76 (0.11) H23A 0.9900 109.49 109.49 H23B 0.9900 109.49 109.49 108.07 C23 - N24 C22 H23A C25 - Distance Angles N24 1.4642 (0.0019) C26 1.5193 (0.0020) 109.97 (0.12) H25A 0.9900 109.67 109.67 H25B 0.9900 109.67 109.67 108.17 C25 - N24 C26 H25A C26 - Distance Angles N21 1.4913 (0.0019) C25 1.5193 (0.0020) 110.22 (0.11) H26A 0.9900 109.61 109.61 H26B 0.9900 109.61 109.61 108.14 C26 - N21 C25 H26A C27 - Distance Angles N21 1.4871 (0.0018) H27A 0.9800 109.47 H27B 0.9800 109.47 109.47 H27C 0.9800 109.47 109.47 109.47 C27 - N21 H27A H27B N21 - Distance Angles C22 1.4840 (0.0019) C27 1.4871 (0.0018) 111.51 (0.11) C26 1.4913 (0.0019) 110.36 (0.11) 111.36 (0.11) H21 0.9300 107.82 107.82 107.82 N21 - C22 C27 C26 N24 - Distance Angles C25 1.4642 (0.0019) C23 1.4648 (0.0018) 109.10 (0.11) C2 1.4801 (0.0018) 115.40 (0.11) 111.17 (0.11) N24 - C25 C23 O1A - Distance Angles C1 1.2385 (0.0018) O1A - O1B - Distance Angles C1 1.2660 (0.0018) O1B - O4A - Distance Angles C4 1.3321 (0.0020) C5 1.4426 (0.0020) 115.45 (0.13) O4A - C4 O4B - Distance Angles C4 1.2107 (0.0020) O4B - O1W - Distance Angles H1W 0.8479 (0.0161) H2W 0.8214 (0.0155) 109.15 (2.00) O1W - H1W Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.848(16) 1.996(16) 2.8376(19) 171(2) O1W-H1W...O1A 0.93 1.74 2.6570(15) 170.2 N21-H21...O1B_$1 0.821(16) 2.026(16) 2.8435(17) 174(2) O1W-H2W...O1B_$2 FMAP and GRID set by program FMAP 2 1 19 GRID -3.125 -2 -2 3.125 2 2 R1 = 0.0653 for 2778 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.35 at 0.1672 0.1560 0.1138 [ 1.06 A from H2 ] Deepest hole -0.24 at 0.3503 0.1372 0.3019 [ 0.78 A from O1A ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 2379 / 18380 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1672 0.1560 0.1138 1.00000 0.05 0.35 1.06 H2 1.13 C2 1.14 C3 1.46 H3B Q2 1 0.1979 0.0406 0.2040 1.00000 0.05 0.29 0.84 C2 1.18 C3 1.35 H3A 1.59 N24 Q3 1 0.1811 0.1349 0.2772 1.00000 0.05 0.27 0.75 C1 0.81 C2 1.42 H2 1.68 O1B Q4 1 0.3821 0.4354 0.0657 1.00000 0.05 0.26 0.92 O4B 1.90 H5A 2.11 C4 2.16 H27A Q5 1 0.4437 0.0788 0.4196 1.00000 0.05 0.25 0.81 O1A 1.87 C1 2.20 H1W 2.27 H22A Q6 1 0.9563 0.4070 0.1199 1.00000 0.05 0.24 0.79 H5C 1.32 C5 1.39 H5B 2.01 H5A Q7 1 -0.2975 -0.1023 0.2942 1.00000 0.05 0.23 0.77 C22 0.79 C23 1.40 H22B 1.49 H23B Q8 1 -0.0144 -0.1013 0.2395 1.00000 0.05 0.19 0.68 N24 0.80 C25 1.42 H25B 1.52 H25A Q9 1 -0.1069 -0.0238 0.2770 1.00000 0.05 0.19 0.72 N24 0.80 C23 1.32 H23B 1.51 H23A Q10 1 0.1606 0.0838 0.0124 1.00000 0.05 0.19 0.49 H3B 1.18 C3 1.99 H3A 2.01 C4 Shortest distances between peaks (including symmetry equivalents) 8 9 1.15 2 3 1.18 1 10 1.22 7 9 1.27 1 2 1.51 2 8 1.68 1 3 1.69 7 8 1.94 3 9 2.03 2 10 2.04 2 9 2.07 4 4 2.18 10 10 2.23 3 8 2.24 3 5 2.41 5 5 2.49 2 5 2.65 1 4 2.67 1 9 2.72 3 10 2.73 1 8 2.75 8 10 2.75 4 6 2.79 1 10 2.87 8 10 2.99 9 10 2.99 Time profile in seconds ----------------------- 0.05: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.52: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.01: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.41: Structure factors and derivatives 0.55: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.09: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 06skc0060p-1 finished at 14:34:05 Total CPU time: 1.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++