+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 09:35:55 on 02-May-2002 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 02sot029 in Pbca CELL 0.71073 16.1973 9.3378 34.0104 90.000 90.000 90.000 ZERR 8.00 0.0005 0.0002 0.0012 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N O F P UNIT 176 240 40 32 48 8 V = 5143.98 F(000) = 2384.0 Mu = 0.19 mm-1 Cell Wt = 4587.84 Rho = 1.481 MERG 2 DFIX 0.9 0.001 O1W H1W O2W H3W O2W H4W DFIX 1.6 0.001 H3W H4W SHEL 7 0.84 EQIV $6 -x+1/2, y-1/2, z EQIV $5 x+1/2, y, -z+3/2 EQIV $4 -x+1/2, -y+1, z+1/2 EQIV $3 -x+1/2, -y, z+1/2 EQIV $2 -x+1, -y, -z+2 EQIV $1 -x+1/2, y+1/2, z HTAB N5 F3 HTAB N5 F4 HTAB O2W F5 HTAB O2W F4_$1 HTAB N3 O1_$2 HTAB N1 O2_$2 HTAB N1 F4_$3 HTAB N1 F6_$3 HTAB N1 O2W_$4 HTAB N5 O1W_$5 HTAB N5 F1_$6 HTAB N5 F3_$6 FMAP 2 PLAN 20 SIZE 0.02 0.10 0.10 ACTA BOND WGHT 0.08180 L.S. 4 TEMP -153.00 FVAR 0.07749 MOLE 1 N1 3 0.392690 0.108706 1.151283 11.00000 0.02982 0.02079 = 0.02432 -0.00292 0.00310 0.00197 N2 3 0.321014 -0.072989 1.059572 11.00000 0.01596 0.03041 = 0.02086 -0.00219 0.00156 -0.00287 AFIX 43 H2 2 0.268051 -0.088579 1.055707 11.00000 -1.20000 AFIX 0 N3 3 0.383658 -0.043276 0.956934 11.00000 0.01458 0.02158 = 0.01800 -0.00067 0.00141 0.00117 AFIX 43 H3 2 0.437954 -0.041683 0.957737 11.00000 -1.20000 AFIX 0 N4 3 0.332171 -0.030316 0.852882 11.00000 0.02555 0.04262 = 0.01978 0.00248 -0.00173 0.00425 AFIX 43 H4 2 0.278652 -0.042330 0.855875 11.00000 -1.20000 AFIX 0 N5 3 0.331767 0.123283 0.751775 11.00000 0.04073 0.04081 = 0.02465 0.00548 -0.00163 0.01021 O1 4 0.446139 -0.048232 1.032072 11.00000 0.02217 0.04599 = 0.02489 0.00366 0.00006 -0.00262 O2 4 0.456099 -0.034424 0.883564 11.00000 0.02128 0.03606 = 0.02599 -0.00106 -0.00135 0.00154 C1 1 0.347885 0.089582 1.113589 11.00000 0.02851 0.03026 = 0.02269 0.00067 -0.00466 0.00082 AFIX 23 H1D 2 0.372157 0.153456 1.093436 11.00000 -1.20000 H1E 2 0.289336 0.117102 1.117154 11.00000 -1.20000 AFIX 0 C2 1 0.352476 -0.065020 1.099362 11.00000 0.02154 0.03523 = 0.02134 -0.00309 0.00336 0.00008 AFIX 23 H2A 2 0.410413 -0.098701 1.100055 11.00000 -1.20000 H2B 2 0.319296 -0.127318 1.116828 11.00000 -1.20000 AFIX 0 C3 1 0.371328 -0.056976 1.028407 11.00000 0.02657 0.01597 = 0.02384 0.00331 -0.00294 -0.00220 C4 1 0.332981 -0.050772 0.989032 11.00000 0.02519 0.01381 = 0.01770 0.00003 0.00124 0.00281 C5 1 0.251043 -0.052036 0.975820 11.00000 0.01964 0.01502 = 0.02479 -0.00017 0.00256 -0.00228 C6 1 0.254605 -0.044293 0.934145 11.00000 0.02510 0.01220 = 0.02304 -0.00257 -0.00032 -0.00074 C7 1 0.337373 -0.038654 0.923560 11.00000 0.01825 0.01875 = 0.01299 -0.00135 -0.00202 -0.00045 C8 1 0.380031 -0.034153 0.885046 11.00000 0.02890 0.01467 = 0.02200 0.00366 -0.00308 -0.00119 C9 1 0.363837 -0.007328 0.813167 11.00000 0.02898 0.05714 = 0.01777 0.00195 0.00111 0.00389 AFIX 23 H9A 2 0.365676 -0.099200 0.798666 11.00000 -1.20000 H9B 2 0.420460 0.032374 0.814314 11.00000 -1.20000 AFIX 0 C10 1 0.307312 0.095684 0.792760 11.00000 0.05827 0.04955 = 0.02710 0.00570 0.00742 0.01541 AFIX 23 H10A 2 0.250483 0.056678 0.793117 11.00000 -1.20000 H10B 2 0.306913 0.187346 0.807387 11.00000 -1.20000 AFIX 0 C11 1 0.175472 -0.055139 1.000439 11.00000 0.02296 0.01958 = 0.01969 0.00491 -0.00532 0.00542 C12 1 0.152980 0.065769 1.022521 11.00000 0.02634 0.02133 = 0.03593 -0.00115 -0.00099 -0.00328 AFIX 43 H12 2 0.185768 0.149955 1.021055 11.00000 -1.20000 AFIX 0 C13 1 0.084032 0.064210 1.046306 11.00000 0.03185 0.02922 = 0.03868 -0.00948 0.01246 0.00169 AFIX 43 H13 2 0.069753 0.146441 1.061281 11.00000 -1.20000 AFIX 0 C14 1 0.035942 -0.057457 1.048217 11.00000 0.01890 0.03323 = 0.04167 0.00873 0.00669 0.00567 AFIX 43 H14 2 -0.011035 -0.059986 1.064927 11.00000 -1.20000 AFIX 0 C15 1 0.056116 -0.174991 1.025905 11.00000 0.02206 0.02973 = 0.04166 0.00735 0.00144 -0.00648 AFIX 43 H15 2 0.021701 -0.257329 1.026648 11.00000 -1.20000 AFIX 0 C16 1 0.125615 -0.175292 1.002426 11.00000 0.02592 0.02095 = 0.03536 -0.00274 -0.00080 -0.00144 AFIX 43 H16 2 0.139265 -0.258181 0.987591 11.00000 -1.20000 AFIX 0 C17 1 0.182135 -0.037319 0.906898 11.00000 0.01732 0.02329 = 0.01748 -0.00313 -0.00141 -0.00236 C18 1 0.134034 -0.156488 0.899206 11.00000 0.02702 0.01845 = 0.03062 -0.00523 -0.00245 0.00249 AFIX 43 H18 2 0.144704 -0.243439 0.912789 11.00000 -1.20000 AFIX 0 C19 1 0.070871 -0.150823 0.872121 11.00000 0.02571 0.03162 = 0.03384 -0.00701 0.00107 -0.01362 AFIX 43 H19 2 0.038426 -0.233741 0.867304 11.00000 -1.20000 AFIX 0 C20 1 0.054312 -0.026483 0.851999 11.00000 0.03185 0.03436 = 0.03290 -0.00025 -0.00719 0.00328 AFIX 43 H20 2 0.011282 -0.023684 0.833034 11.00000 -1.20000 AFIX 0 C21 1 0.100963 0.094808 0.859627 11.00000 0.02672 0.02070 = 0.03536 0.00482 -0.00849 0.00306 AFIX 43 H21 2 0.090283 0.181470 0.845908 11.00000 -1.20000 AFIX 0 C22 1 0.162928 0.088475 0.887278 11.00000 0.02636 0.02510 = 0.02614 -0.00334 -0.00057 0.00001 AFIX 43 H22 2 0.193416 0.172774 0.893085 11.00000 -1.20000 AFIX 0 H51 2 0.442764 0.084938 1.147316 11.00000 0.03294 H52 2 0.371609 0.050441 1.171645 11.00000 0.04492 H53 2 0.382312 0.204578 1.161392 11.00000 0.02557 H55 2 0.385982 0.192846 0.755348 11.00000 0.08933 H56 2 0.283931 0.166260 0.736280 11.00000 0.09545 H57 2 0.349371 0.050347 0.740693 11.00000 0.08859 MOLE 2 P1 6 0.130902 0.246167 0.709142 11.00000 0.03499 0.02870 = 0.03537 -0.00163 -0.00320 0.00268 F1 5 0.075210 0.390376 0.723317 11.00000 0.03333 0.03486 = 0.04203 -0.00579 -0.00618 0.01240 F2 5 0.117678 0.169784 0.753001 11.00000 0.09940 0.04063 = 0.03268 0.00508 0.00827 0.00789 F3 5 0.215698 0.326587 0.726417 11.00000 0.03086 0.03952 = 0.10474 -0.02580 -0.02068 0.00491 F4 5 0.189725 0.102333 0.695573 11.00000 0.03426 0.03143 = 0.05590 -0.00959 0.00336 0.00391 F5 5 0.145982 0.321206 0.665155 11.00000 0.12189 0.02925 = 0.03667 -0.00091 0.02441 -0.00222 F6 5 0.048064 0.165111 0.692348 11.00000 0.04531 0.03632 = 0.07659 -0.01105 -0.02726 -0.00022 MOLE 3 O1W 4 -0.074955 0.370849 0.758336 11.00000 0.06603 0.06047 = 0.06221 -0.00665 0.00932 -0.00863 H1W 2 -0.102975 0.401095 0.737042 11.00000 0.02262 MOLE 4 O2W 4 0.161234 0.612377 0.657450 11.00000 0.03732 0.03901 = 0.05695 0.00827 -0.01120 -0.00162 H3W 2 0.145338 0.552171 0.638220 11.00000 0.21167 H4W 2 0.212294 0.617494 0.667796 11.00000 0.08776 MOLE 0 HKLF 4 1.0 0.00 1.00 0.00 1.00 0.00 0.00 0.00 0.00 -1.00 Covalent radii and connectivity table for 02sot029 in Pbca C 0.770 H 0.320 N 0.700 O 0.660 F 0.640 P 1.100 N1 - C1 N2 - C3 C2 N3 - C7 C4 N4 - C8 C9 N5 - C10 O1 - C3 O2 - C8 C1 - N1 C2 C2 - N2 C1 C3 - O1 N2 C4 C4 - N3 C5 C3 C5 - C4 C6 C11 C6 - C7 C5 C17 C7 - N3 C6 C8 C8 - O2 N4 C7 C9 - N4 C10 C10 - N5 C9 C11 - C16 C12 C5 C12 - C13 C11 C13 - C14 C12 C14 - C15 C13 C15 - C14 C16 C16 - C15 C11 C17 - C18 C22 C6 C18 - C19 C17 C19 - C20 C18 C20 - C19 C21 C21 - C22 C20 C22 - C21 C17 P1 - F6 F2 F5 F3 F1 F4 F1 - P1 F2 - P1 F3 - P1 F4 - P1 F5 - P1 F6 - P1 O1W - no bonds found O2W - no bonds found Operators for generating equivalent atoms: $1 -x+1/2, y+1/2, z $2 -x+1, -y, -z+2 $3 -x+1/2, -y, z+1/2 $4 -x+1/2, -y+1, z+1/2 $5 x+1/2, y, -z+3/2 $6 -x+1/2, y-1/2, z 20398 Reflections read, of which 1694 rejected -19 =< h =< 13, -11 =< k =< 9, -40 =< l =< 39, Max. 2-theta = 50.05 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 8 0 0 39.59 0.95 3 13.25 2 5 0 204.44 3.13 4 69.67 1 4 1 187.23 1.85 8 14.51 1 6 1 97.40 1.86 6 12.22 2 3 2 370.65 2.91 8 30.80 7 3 2 73.00 0.90 8 6.18 0 6 3 36.67 1.67 3 10.89 1 1 4 90.93 1.55 9 7.80 1 2 4 55.63 0.89 6 6.08 7 2 6 86.78 1.40 10 7.26 4 1 7 51.41 0.80 9 4.29 1 3 7 33.40 0.58 9 3.62 7 0 8 54.19 1.42 4 21.87 0 2 10 46.95 0.86 4 8.70 5 2 13 109.12 1.92 7 19.15 4 1 15 146.45 1.93 9 12.37 2 3 15 82.33 1.56 9 7.84 1 3 30 28.44 1.85 3 10.89 18 Inconsistent equivalents 4519 Unique reflections, of which 0 suppressed R(int) = 0.1556 R(sigma) = 0.1655 Friedel opposites merged Maximum memory for data reduction = 3593 / 45775 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 = 4608 / 485145 wR2 = 0.1779 before cycle 1 for 4519 data and 379 / 379 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.923; Restrained GooF = 0.923 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0818 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.07757 0.00023 0.369 OSF Mean shift/esd = 0.072 Maximum = 0.369 for OSF Max. shift = 0.018 A for H57 Max. dU = 0.014 for H3W Least-squares cycle 2 Maximum vector length = 511 Memory required = 4608 / 485145 wR2 = 0.1779 before cycle 2 for 4519 data and 379 / 379 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.924; Restrained GooF = 0.924 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0818 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.07759 0.00023 0.059 OSF Mean shift/esd = 0.024 Maximum = 0.164 for x H57 Max. shift = 0.013 A for H57 Max. dU = 0.004 for H3W Least-squares cycle 3 Maximum vector length = 511 Memory required = 4608 / 485145 wR2 = 0.1779 before cycle 3 for 4519 data and 379 / 379 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.924; Restrained GooF = 0.924 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0818 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.07759 0.00023 0.018 OSF Mean shift/esd = 0.004 Maximum = 0.067 for x H57 Max. shift = 0.005 A for H57 Max. dU = 0.001 for H55 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4608 / 485145 wR2 = 0.1779 before cycle 4 for 4519 data and 379 / 379 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.924; Restrained GooF = 0.924 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0818 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.07759 0.00023 0.004 OSF Mean shift/esd = 0.002 Maximum = 0.031 for x H57 Max. shift = 0.002 A for H57 Max. dU = 0.000 for H55 Largest correlation matrix elements -0.970 z H3W / y H3W -0.752 z H1W / x H1W -0.517 U11 H57 / y N5 -0.968 z H4W / x H4W -0.526 x H4W / x H3W Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.2681 -0.0886 1.0557 43 0.880 0.000 N2 C3 C2 H3 0.4379 -0.0418 0.9577 43 0.880 0.000 N3 C7 C4 H4 0.2787 -0.0425 0.8559 43 0.880 0.000 N4 C8 C9 H1D 0.3722 0.1534 1.0934 23 0.990 0.000 C1 N1 C2 H1E 0.2893 0.1171 1.1171 23 0.990 0.000 C1 N1 C2 H2A 0.4104 -0.0987 1.1000 23 0.990 0.000 C2 N2 C1 H2B 0.3193 -0.1273 1.1168 23 0.990 0.000 C2 N2 C1 H9A 0.3656 -0.0991 0.7986 23 0.990 0.000 C9 N4 C10 H9B 0.4204 0.0324 0.8143 23 0.990 0.000 C9 N4 C10 H10A 0.2505 0.0568 0.7932 23 0.990 0.000 C10 N5 C9 H10B 0.3070 0.1874 0.8074 23 0.990 0.000 C10 N5 C9 H12 0.1858 0.1499 1.0211 43 0.950 0.000 C12 C13 C11 H13 0.0698 0.1464 1.0613 43 0.950 0.000 C13 C14 C12 H14 -0.0111 -0.0599 1.0649 43 0.950 0.000 C14 C15 C13 H15 0.0217 -0.2573 1.0267 43 0.950 0.000 C15 C14 C16 H16 0.1393 -0.2582 0.9876 43 0.950 0.000 C16 C15 C11 H18 0.1448 -0.2435 0.9128 43 0.950 0.000 C18 C19 C17 H19 0.0385 -0.2338 0.8674 43 0.950 0.000 C19 C20 C18 H20 0.0113 -0.0236 0.8330 43 0.950 0.000 C20 C19 C21 H21 0.0902 0.1816 0.8460 43 0.950 0.000 C21 C22 C20 H22 0.1935 0.1727 0.8930 43 0.950 0.000 C22 C21 C17 02sot029 in Pbca ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq N1 0.39269 0.10868 1.15130 1.00000 0.02981 0.02075 0.02459 -0.00284 0.00294 0.00190 0.02505 0.00761 0.00030 0.00054 0.00013 0.00000 0.00283 0.00301 0.00276 0.00237 0.00212 0.00234 0.00106 N2 0.32103 -0.07299 1.05958 1.00000 0.01621 0.03051 0.02039 -0.00207 0.00145 -0.00329 0.02237 0.00620 0.00021 0.00041 0.00011 0.00000 0.00198 0.00257 0.00223 0.00190 0.00174 0.00182 0.00095 H2 0.26808 -0.08863 1.05571 1.00000 0.02684 0.00000 0.00000 N3 0.38362 -0.04330 0.95693 1.00000 0.01489 0.02134 0.01791 -0.00056 0.00157 0.00118 0.01805 0.00594 0.00021 0.00038 0.00010 0.00000 0.00186 0.00228 0.00215 0.00186 0.00170 0.00172 0.00089 H3 0.43792 -0.04178 0.95772 1.00000 0.02166 0.00000 0.00000 N4 0.33220 -0.03038 0.85288 1.00000 0.02551 0.04259 0.01966 0.00216 -0.00180 0.00385 0.02925 0.00664 0.00023 0.00043 0.00011 0.00000 0.00227 0.00296 0.00232 0.00205 0.00187 0.00207 0.00106 H4 0.27869 -0.04254 0.85587 1.00000 0.03510 0.00000 0.00000 N5 0.33175 0.12329 0.75174 1.00000 0.04079 0.04122 0.02459 0.00583 -0.00128 0.01068 0.03553 0.00939 0.00031 0.00063 0.00013 0.00000 0.00297 0.00333 0.00281 0.00251 0.00227 0.00276 0.00119 O1 0.44614 -0.04822 1.03208 1.00000 0.02199 0.04630 0.02500 0.00366 -0.00002 -0.00283 0.03110 0.00547 0.00019 0.00036 0.00009 0.00000 0.00191 0.00237 0.00200 0.00165 0.00147 0.00171 0.00087 O2 0.45611 -0.03444 0.88355 1.00000 0.02152 0.03619 0.02598 -0.00112 -0.00115 0.00153 0.02790 0.00518 0.00018 0.00034 0.00009 0.00000 0.00192 0.00220 0.00191 0.00163 0.00146 0.00161 0.00082 C1 0.34788 0.08953 1.11357 1.00000 0.02908 0.03028 0.02259 0.00055 -0.00445 0.00092 0.02732 0.00791 0.00028 0.00053 0.00013 0.00000 0.00265 0.00322 0.00279 0.00248 0.00228 0.00238 0.00120 H1D 0.37216 0.15341 1.09342 1.00000 0.03278 0.00000 0.00000 H1E 0.28932 0.11706 1.11712 1.00000 0.03278 0.00000 0.00000 C2 0.35247 -0.06498 1.09934 1.00000 0.02138 0.03513 0.02149 -0.00314 0.00354 -0.00005 0.02600 0.00775 0.00028 0.00053 0.00013 0.00000 0.00247 0.00346 0.00284 0.00246 0.00216 0.00233 0.00123 H2A 0.41040 -0.09865 1.10004 1.00000 0.03120 0.00000 0.00000 H2B 0.31929 -0.12728 1.11681 1.00000 0.03120 0.00000 0.00000 C3 0.37137 -0.05695 1.02844 1.00000 0.02680 0.01557 0.02401 0.00331 -0.00302 -0.00248 0.02213 0.00773 0.00028 0.00049 0.00013 0.00000 0.00295 0.00287 0.00289 0.00226 0.00232 0.00228 0.00115 C4 0.33297 -0.05072 0.98903 1.00000 0.02532 0.01371 0.01778 0.00012 0.00126 0.00302 0.01894 0.00729 0.00025 0.00045 0.00013 0.00000 0.00268 0.00272 0.00263 0.00216 0.00215 0.00218 0.00109 C5 0.25105 -0.05201 0.97580 1.00000 0.01942 0.01473 0.02470 0.00022 0.00259 -0.00240 0.01962 0.00738 0.00026 0.00045 0.00013 0.00000 0.00242 0.00259 0.00283 0.00226 0.00215 0.00217 0.00106 C6 0.25462 -0.04427 0.93414 1.00000 0.02469 0.01198 0.02337 -0.00262 -0.00024 -0.00058 0.02002 0.00740 0.00027 0.00044 0.00013 0.00000 0.00262 0.00265 0.00284 0.00224 0.00214 0.00225 0.00109 C7 0.33731 -0.03865 0.92356 1.00000 0.01790 0.01862 0.01308 -0.00176 -0.00198 -0.00060 0.01653 0.00705 0.00024 0.00047 0.00012 0.00000 0.00246 0.00287 0.00251 0.00210 0.00202 0.00216 0.00107 C8 0.38000 -0.03415 0.88504 1.00000 0.02835 0.01492 0.02186 0.00340 -0.00319 -0.00107 0.02171 0.00783 0.00028 0.00049 0.00013 0.00000 0.00292 0.00280 0.00287 0.00231 0.00227 0.00227 0.00113 C9 0.36382 -0.00727 0.81316 1.00000 0.02873 0.05729 0.01729 0.00223 0.00099 0.00370 0.03444 0.00899 0.00028 0.00062 0.00013 0.00000 0.00284 0.00396 0.00282 0.00267 0.00232 0.00270 0.00137 H9A 0.36565 -0.09910 0.79864 1.00000 0.04132 0.00000 0.00000 H9B 0.42045 0.03243 0.81431 1.00000 0.04132 0.00000 0.00000 C10 0.30732 0.09572 0.79280 1.00000 0.05875 0.04996 0.02619 0.00561 0.00777 0.01513 0.04497 0.01037 0.00035 0.00063 0.00014 0.00000 0.00366 0.00387 0.00328 0.00292 0.00276 0.00314 0.00153 H10A 0.25048 0.05677 0.79319 1.00000 0.05396 0.00000 0.00000 H10B 0.30699 0.18739 0.80743 1.00000 0.05396 0.00000 0.00000 C11 0.17546 -0.05512 1.00045 1.00000 0.02261 0.01949 0.01982 0.00481 -0.00555 0.00551 0.02064 0.00775 0.00025 0.00050 0.00013 0.00000 0.00260 0.00298 0.00271 0.00231 0.00199 0.00238 0.00114 C12 0.15296 0.06574 1.02254 1.00000 0.02692 0.02122 0.03603 -0.00122 -0.00096 -0.00302 0.02805 0.00818 0.00028 0.00052 0.00014 0.00000 0.00267 0.00315 0.00312 0.00263 0.00240 0.00239 0.00122 H12 0.18576 0.14992 1.02108 1.00000 0.03367 0.00000 0.00000 C13 0.08403 0.06421 1.04632 1.00000 0.03149 0.02916 0.03837 -0.00948 0.01263 0.00169 0.03301 0.00877 0.00030 0.00055 0.00014 0.00000 0.00284 0.00336 0.00333 0.00268 0.00250 0.00264 0.00132 H13 0.06977 0.14642 1.06131 1.00000 0.03961 0.00000 0.00000 C14 0.03592 -0.05743 1.04821 1.00000 0.01853 0.03326 0.04148 0.00914 0.00714 0.00591 0.03109 0.00907 0.00028 0.00056 0.00015 0.00000 0.00259 0.00351 0.00337 0.00285 0.00231 0.00260 0.00130 H14 -0.01110 -0.05991 1.06490 1.00000 0.03731 0.00000 0.00000 C15 0.05610 -0.17498 1.02592 1.00000 0.02190 0.02971 0.04245 0.00744 0.00153 -0.00673 0.03135 0.00856 0.00027 0.00057 0.00014 0.00000 0.00263 0.00337 0.00334 0.00283 0.00246 0.00241 0.00129 H15 0.02169 -0.25733 1.02667 1.00000 0.03763 0.00000 0.00000 C16 0.12562 -0.17527 1.00244 1.00000 0.02583 0.02028 0.03544 -0.00278 -0.00087 -0.00140 0.02718 0.00803 0.00027 0.00053 0.00013 0.00000 0.00269 0.00310 0.00317 0.00251 0.00224 0.00237 0.00124 H16 0.13929 -0.25817 0.98762 1.00000 0.03262 0.00000 0.00000 C17 0.18213 -0.03730 0.90691 1.00000 0.01717 0.02313 0.01720 -0.00301 -0.00138 -0.00227 0.01916 0.00742 0.00025 0.00051 0.00012 0.00000 0.00235 0.00308 0.00259 0.00232 0.00192 0.00233 0.00111 C18 0.13404 -0.15656 0.89920 1.00000 0.02673 0.01871 0.03045 -0.00486 -0.00253 0.00256 0.02530 0.00791 0.00027 0.00053 0.00014 0.00000 0.00269 0.00299 0.00300 0.00241 0.00233 0.00234 0.00121 H18 0.14476 -0.24354 0.91276 1.00000 0.03036 0.00000 0.00000 C19 0.07093 -0.15092 0.87217 1.00000 0.02546 0.03149 0.03435 -0.00759 0.00094 -0.01339 0.03043 0.00797 0.00027 0.00056 0.00014 0.00000 0.00277 0.00341 0.00320 0.00270 0.00241 0.00253 0.00130 H19 0.03847 -0.23383 0.86737 1.00000 0.03652 0.00000 0.00000 C20 0.05433 -0.02641 0.85202 1.00000 0.03167 0.03474 0.03316 -0.00015 -0.00732 0.00367 0.03319 0.00898 0.00030 0.00058 0.00015 0.00000 0.00291 0.00358 0.00314 0.00283 0.00244 0.00283 0.00132 H20 0.01132 -0.02364 0.83305 1.00000 0.03983 0.00000 0.00000 C21 0.10093 0.09487 0.85966 1.00000 0.02673 0.02003 0.03514 0.00471 -0.00833 0.00260 0.02730 0.00826 0.00027 0.00054 0.00014 0.00000 0.00279 0.00305 0.00324 0.00248 0.00237 0.00249 0.00124 H21 0.09020 0.18158 0.84597 1.00000 0.03276 0.00000 0.00000 C22 0.16292 0.08846 0.88726 1.00000 0.02634 0.02449 0.02693 -0.00375 -0.00087 -0.00002 0.02592 0.00814 0.00027 0.00053 0.00013 0.00000 0.00265 0.00313 0.00288 0.00252 0.00231 0.00237 0.00117 H22 0.19346 0.17273 0.89304 1.00000 0.03110 0.00000 0.00000 H51 0.44257 0.08556 1.14717 1.00000 0.03861 0.08405 0.00323 0.00547 0.00144 0.00000 0.01697 H52 0.37148 0.04915 1.17173 1.00000 0.04736 0.08539 0.00300 0.00577 0.00156 0.00000 0.01727 H53 0.38216 0.20549 1.16144 1.00000 0.02793 0.08077 0.00250 0.00565 0.00125 0.00000 0.01385 H55 0.38729 0.19157 0.75548 1.00000 0.09465 0.11920 0.00409 0.00736 0.00177 0.00000 0.02237 H56 0.28343 0.16581 0.73623 1.00000 0.09280 0.11032 0.00405 0.00678 0.00186 0.00000 0.02252 H57 0.35154 0.04882 0.74069 1.00000 0.09549 0.12476 0.00437 0.00840 0.00204 0.00000 0.02987 P1 0.13090 0.24618 0.70914 1.00000 0.03518 0.02890 0.03561 -0.00176 -0.00323 0.00274 0.03323 0.00234 0.00008 0.00015 0.00004 0.00000 0.00078 0.00087 0.00085 0.00073 0.00063 0.00067 0.00041 F1 0.07520 0.39039 0.72332 1.00000 0.03353 0.03471 0.04207 -0.00586 -0.00611 0.01261 0.03677 0.00455 0.00015 0.00029 0.00008 0.00000 0.00153 0.00179 0.00181 0.00145 0.00135 0.00134 0.00075 F2 0.11763 0.16979 0.75300 1.00000 0.10045 0.04034 0.03251 0.00534 0.00855 0.00812 0.05777 0.00563 0.00021 0.00034 0.00008 0.00000 0.00252 0.00209 0.00190 0.00158 0.00171 0.00174 0.00095 F3 0.21570 0.32654 0.72643 1.00000 0.03097 0.03958 0.10561 -0.02633 -0.02113 0.00461 0.05872 0.00472 0.00016 0.00032 0.00010 0.00000 0.00161 0.00197 0.00281 0.00190 0.00172 0.00149 0.00101 F4 0.18973 0.10230 0.69558 1.00000 0.03442 0.03119 0.05608 -0.01002 0.00350 0.00407 0.04056 0.00466 0.00016 0.00030 0.00008 0.00000 0.00156 0.00180 0.00198 0.00152 0.00142 0.00138 0.00079 F5 0.14606 0.32124 0.66516 1.00000 0.12139 0.02944 0.03654 -0.00053 0.02433 -0.00224 0.06246 0.00580 0.00022 0.00032 0.00008 0.00000 0.00289 0.00193 0.00200 0.00157 0.00187 0.00186 0.00102 F6 0.04805 0.16517 0.69234 1.00000 0.04513 0.03638 0.07654 -0.01108 -0.02749 -0.00032 0.05268 0.00464 0.00017 0.00031 0.00009 0.00000 0.00183 0.00194 0.00235 0.00170 0.00169 0.00150 0.00092 O1W -0.07494 0.37086 0.75835 1.00000 0.06638 0.06175 0.06257 -0.00750 0.00909 -0.00939 0.06357 0.00752 0.00026 0.00047 0.00013 0.00000 0.00289 0.00321 0.00332 0.00261 0.00259 0.00244 0.00124 H1W -0.10332 0.40062 0.73711 1.00000 0.02490 0.06606 0.00234 0.00476 0.00079 0.00000 0.01493 O2W 0.16125 0.61223 0.65745 1.00000 0.03702 0.03923 0.05690 0.00805 -0.01069 -0.00114 0.04439 0.00727 0.00022 0.00041 0.00012 0.00000 0.00230 0.00256 0.00273 0.00214 0.00202 0.00194 0.00100 H3W 0.14573 0.55253 0.63803 1.00000 0.22896 0.03024 0.00256 0.00870 0.00213 0.00000 0.05768 H4W 0.21221 0.61760 0.66790 1.00000 0.08887 0.04836 0.00133 0.00576 0.00149 0.00000 0.02331 Final Structure Factor Calculation for 02sot029 in Pbca Total number of l.s. parameters = 379 Maximum vector length = 511 Memory required = 4229 / 25039 wR2 = 0.1779 before cycle 5 for 4519 data and 0 / 379 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.001 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.924; Restrained GooF = 0.924 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0818 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0656 for 2080 Fo > 4sig(Fo) and 0.1736 for all 4519 data wR2 = 0.1779, GooF = S = 0.924, Restrained GooF = 0.924 for all data Occupancy sum of asymmetric unit = 38.00 for non-hydrogen and 30.00 for hydrogen atoms Principal mean square atomic displacements U 0.0312 0.0256 0.0184 N1 0.0317 0.0201 0.0153 N2 0.0216 0.0186 0.0140 N3 0.0435 0.0255 0.0187 N4 0.0521 0.0331 0.0214 N5 0.0472 0.0245 0.0216 O1 0.0365 0.0261 0.0211 O2 0.0316 0.0301 0.0202 C1 0.0359 0.0245 0.0176 C2 0.0298 0.0223 0.0143 C3 0.0262 0.0176 0.0130 C4 0.0258 0.0195 0.0136 C5 0.0247 0.0239 0.0114 C6 0.0191 0.0186 0.0119 C7 0.0300 0.0216 0.0135 C8 0.0579 0.0283 0.0171 C9 0.0721 0.0386 0.0242 C10 0.0275 0.0245 0.0100 C11 0.0362 0.0282 0.0198 C12 0.0502 0.0317 0.0171 C13 0.0501 0.0274 0.0157 C14 0.0460 0.0311 0.0169 C15 0.0360 0.0262 0.0194 C16 0.0247 0.0185 0.0142 C17 0.0337 0.0254 0.0167 C18 0.0460 0.0314 0.0139 C19 0.0409 0.0343 0.0244 C20 0.0406 0.0254 0.0159 C21 0.0298 0.0263 0.0217 C22 0.0396 0.0323 0.0278 P1 0.0532 0.0356 0.0215 F1 0.1027 0.0410 0.0295 F2 0.1200 0.0315 0.0246 F3 0.0598 0.0369 0.0250 F4 0.1279 0.0301 0.0294 F5 0.0940 0.0384 0.0256 F6 0.0812 0.0552 0.0543 O1W 0.0640 0.0376 0.0315 O2W Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.005 0.010 0.015 0.021 0.028 0.036 0.046 0.061 0.091 1.000 Number in group 496. 434. 436. 456. 485. 443. 445. 439. 430. 455. GooF 0.753 0.760 0.878 0.868 0.910 0.911 1.012 1.022 1.054 1.032 K 1.753 0.988 1.034 1.218 0.971 1.001 0.996 1.004 1.013 1.005 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.06 1.14 1.26 1.44 1.80 inf Number in group 454. 469. 445. 447. 443. 451. 466. 443. 451. 450. GooF 0.809 0.852 0.802 0.869 0.852 0.848 0.919 0.946 0.912 1.321 K 1.214 1.118 1.010 1.019 1.014 0.999 1.003 1.019 1.017 0.991 R1 0.452 0.432 0.341 0.283 0.223 0.141 0.112 0.089 0.061 0.058 Recommended weighting scheme: WGHT 0.0803 0.0000 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 10 1040.77 1697.28 5.33 0.068 2.97 8 2 5 220.67 506.54 4.68 0.037 1.79 4 2 2 4673.66 7316.20 4.59 0.141 3.01 3 0 4 1636.13 1158.89 4.01 0.056 4.56 2 2 14 4565.85 3368.34 4.01 0.096 2.08 0 4 24 1302.47 727.62 3.91 0.044 1.21 1 3 10 282.96 46.88 3.88 0.011 2.27 1 5 4 309.71 72.21 3.87 0.014 1.81 1 0 16 6808.29 5158.95 3.61 0.118 2.11 6 2 4 1042.47 757.45 3.50 0.045 2.25 5 2 10 932.15 673.25 3.39 0.043 2.10 1 0 8 2232.76 1567.71 3.28 0.065 4.11 1 3 6 18986.08 15035.41 3.26 0.202 2.69 5 0 18 400.25 951.81 3.26 0.051 1.63 2 1 17 444.50 737.26 3.21 0.045 1.90 9 5 5 73.01 308.11 3.19 0.029 1.27 4 0 4 1474.26 1122.66 3.17 0.055 3.66 7 5 30 -158.85 492.53 3.15 0.037 0.89 12 2 12 662.66 1267.89 3.13 0.059 1.18 4 4 0 1458.67 1087.22 3.13 0.054 2.02 6 8 20 1958.25 0.44 3.10 0.001 0.91 13 1 10 852.90 496.93 3.09 0.037 1.16 2 3 0 12542.38 9962.45 3.07 0.164 2.91 7 2 4 1490.01 1151.96 3.07 0.056 2.01 6 1 18 975.11 1307.91 3.07 0.060 1.53 2 2 0 6571.42 5187.99 3.05 0.119 4.04 10 1 12 690.51 998.57 3.05 0.052 1.39 10 0 8 504.38 175.09 3.04 0.022 1.51 4 4 14 1839.57 2377.32 3.02 0.080 1.55 0 0 6 2115.01 2769.38 3.01 0.087 5.67 0 4 36 3524.72 1922.14 2.99 0.072 0.88 4 2 13 704.76 497.96 2.96 0.037 1.99 2 2 5 3600.48 2862.82 2.95 0.088 3.48 12 7 10 -171.48 276.34 2.94 0.027 0.91 7 2 8 513.02 328.73 2.92 0.030 1.86 3 3 8 2559.57 2028.82 2.92 0.074 2.28 9 0 16 6303.18 4800.26 2.92 0.114 1.37 16 2 7 547.46 923.89 2.92 0.050 0.97 2 5 18 406.17 153.75 2.90 0.020 1.31 2 1 5 4894.47 6144.03 2.87 0.129 4.55 8 1 2 216.22 69.45 2.87 0.014 1.97 12 2 21 82.96 589.81 2.87 0.040 1.01 17 1 13 -302.65 519.50 2.85 0.038 0.89 4 6 1 211.22 25.42 2.83 0.008 1.45 10 6 19 3029.56 1209.69 2.83 0.057 0.95 13 1 25 72.75 551.29 2.83 0.039 0.91 10 1 31 622.16 135.40 2.82 0.019 0.90 5 0 14 662.58 269.21 2.81 0.027 1.94 0 0 30 2743.87 1346.15 2.78 0.060 1.13 0 2 38 2612.72 1299.26 2.77 0.059 0.88 Bond lengths and angles N1 - Distance Angles C1 1.4851 (0.0059) N1 - N2 - Distance Angles C3 1.3451 (0.0054) C2 1.4468 (0.0053) 121.13 (0.36) N2 - C3 N3 - Distance Angles C7 1.3611 (0.0049) C4 1.3676 (0.0051) 109.68 (0.33) N3 - C7 N4 - Distance Angles C8 1.3406 (0.0054) C9 1.4608 (0.0054) 123.77 (0.38) N4 - C8 N5 - Distance Angles C10 1.4742 (0.0063) N5 - O1 - Distance Angles C3 1.2200 (0.0048) O1 - O2 - Distance Angles C8 1.2339 (0.0049) O2 - C1 - Distance Angles N1 1.4851 (0.0059) C2 1.5235 (0.0067) 111.37 (0.40) C1 - N1 C2 - Distance Angles N2 1.4468 (0.0053) C1 1.5235 (0.0067) 109.18 (0.38) C2 - N2 C3 - Distance Angles O1 1.2200 (0.0048) N2 1.3451 (0.0054) 121.96 (0.41) C4 1.4787 (0.0060) 120.45 (0.40) 117.59 (0.38) C3 - O1 N2 C4 - Distance Angles N3 1.3676 (0.0051) C5 1.4012 (0.0057) 108.18 (0.36) C3 1.4787 (0.0060) 118.25 (0.36) 133.57 (0.40) C4 - N3 C5 C5 - Distance Angles C4 1.4012 (0.0057) C6 1.4196 (0.0060) 106.36 (0.37) C11 1.4843 (0.0058) 126.86 (0.39) 126.75 (0.38) C5 - C4 C6 C6 - Distance Angles C7 1.3879 (0.0059) C5 1.4196 (0.0060) 107.46 (0.38) C17 1.4970 (0.0059) 126.50 (0.40) 125.99 (0.39) C6 - C7 C5 C7 - Distance Angles N3 1.3611 (0.0049) C6 1.3879 (0.0059) 108.33 (0.36) C8 1.4819 (0.0058) 118.74 (0.36) 132.89 (0.39) C7 - N3 C6 C8 - Distance Angles O2 1.2339 (0.0048) N4 1.3406 (0.0053) 122.93 (0.41) C7 1.4819 (0.0058) 120.17 (0.39) 116.90 (0.38) C8 - O2 N4 C9 - Distance Angles N4 1.4608 (0.0054) C10 1.4972 (0.0069) 107.95 (0.38) C9 - N4 C10 - Distance Angles N5 1.4742 (0.0063) C9 1.4972 (0.0069) 112.72 (0.43) C10 - N5 C11 - Distance Angles C16 1.3839 (0.0062) C12 1.4039 (0.0061) 118.30 (0.42) C5 1.4843 (0.0058) 121.65 (0.41) 120.05 (0.40) C11 - C16 C12 C12 - Distance Angles C13 1.3788 (0.0064) C11 1.4039 (0.0061) 121.05 (0.44) C12 - C13 C13 - Distance Angles C14 1.3789 (0.0068) C12 1.3788 (0.0064) 119.57 (0.46) C13 - C14 C14 - Distance Angles C15 1.3735 (0.0067) C13 1.3789 (0.0068) 119.87 (0.44) C14 - C15 C15 - Distance Angles C14 1.3735 (0.0068) C16 1.3805 (0.0061) 121.00 (0.46) C15 - C14 C16 - Distance Angles C15 1.3805 (0.0061) C11 1.3839 (0.0062) 120.17 (0.46) C16 - C15 C17 - Distance Angles C18 1.3841 (0.0062) C22 1.3865 (0.0063) 117.63 (0.41) C6 1.4970 (0.0059) 121.59 (0.42) 120.73 (0.40) C17 - C18 C22 C18 - Distance Angles C19 1.3757 (0.0062) C17 1.3841 (0.0062) 120.93 (0.46) C18 - C19 C19 - Distance Angles C20 1.3761 (0.0067) C18 1.3757 (0.0062) 120.68 (0.46) C19 - C20 C20 - Distance Angles C19 1.3761 (0.0066) C21 1.3855 (0.0067) 119.39 (0.45) C20 - C19 C21 - Distance Angles C22 1.3759 (0.0061) C20 1.3855 (0.0067) 119.33 (0.46) C21 - C22 C22 - Distance Angles C21 1.3759 (0.0061) C17 1.3865 (0.0063) 121.97 (0.44) C22 - C21 P1 - Distance Angles F6 1.6430 (0.0030) F2 1.6672 (0.0031) 90.50 (0.18) F5 1.6700 (0.0031) 90.11 (0.18) 178.86 (0.20) F3 1.6719 (0.0030) 179.25 (0.19) 89.04 (0.18) 90.34 (0.19) F1 1.6912 (0.0028) 91.72 (0.15) 90.95 (0.16) 89.98 (0.16) 88.89 (0.14) F4 1.7105 (0.0030) 89.98 (0.15) 88.69 (0.16) 90.36 (0.16) 89.41 (0.15) 178.27 (0.16) P1 - F6 F2 F5 F3 F1 F1 - Distance Angles P1 1.6912 (0.0028) F1 - F2 - Distance Angles P1 1.6672 (0.0031) F2 - F3 - Distance Angles P1 1.6719 (0.0029) F3 - F4 - Distance Angles P1 1.7105 (0.0030) F4 - F5 - Distance Angles P1 1.6700 (0.0031) F5 - F6 - Distance Angles P1 1.6430 (0.0030) F6 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 1.02(7) 1.89(7) 2.806(6) 147(5) N5-H56...F3 1.02(7) 2.14(7) 2.997(6) 140(5) N5-H56...F4 0.9000(11) 2.35(10) 2.741(5) 106(8) O2W-H3W...F5 0.9000(12) 1.852(13) 2.742(5) 169(6) O2W-H4W...F4_$1 0.88 2.09 2.911(5) 155.7 N3-H3...O1_$2 0.85(5) 2.00(5) 2.808(6) 158(5) N1-H51...O2_$2 0.95(6) 1.91(6) 2.816(6) 158(4) N1-H52...F4_$3 0.95(6) 2.49(5) 3.067(6) 119(4) N1-H52...F6_$3 0.98(5) 1.85(5) 2.757(6) 153(4) N1-H53...O2W_$4 1.11(7) 1.84(7) 2.783(7) 140(5) N5-H55...O1W_$5 0.85(8) 1.99(8) 2.817(6) 164(7) N5-H57...F1_$6 0.85(8) 2.39(8) 3.002(7) 129(6) N5-H57...F3_$6 FMAP and GRID set by program FMAP 2 2 13 GRID -2.500 24 -2 2.500 1 2 R1 = 0.1729 for 4519 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.69 at 0.4719 0.2348 0.7134 [ 1.76 A from O1W ] Deepest hole -0.52 at 0.6033 0.2311 0.2809 [ 0.60 A from P1 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 5207 / 40091 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.0281 0.2348 0.7866 1.00000 0.05 0.69 1.76 O1W 2.02 H55 2.36 H53 2.59 H1W Q2 1 -0.1081 0.4841 0.7509 1.00000 0.05 0.37 0.91 H1W 1.21 O1W 1.75 F2 2.51 F4 Q3 1 -0.1586 0.4599 0.7165 1.00000 0.05 0.32 1.26 H1W 1.77 H10A 2.13 O1W 2.31 F2 Q4 1 0.1359 0.3509 0.6579 1.00000 0.05 0.31 0.41 F5 2.00 P1 2.01 H3W 2.46 F1 Q5 1 0.1237 0.5268 0.6696 1.00000 0.05 0.29 1.09 O2W 1.16 H3W 1.67 H4W 1.96 F5 Q6 1 0.3628 0.1170 0.8039 1.00000 0.05 0.29 0.99 C10 1.12 H10B 1.20 C9 1.27 H9B Q7 1 -0.0147 0.3545 0.7393 1.00000 0.05 0.27 1.18 O1W 1.50 H1W 1.59 F1 2.21 H55 Q8 1 0.1976 0.3058 0.6777 1.00000 0.05 0.27 0.95 F5 1.62 P1 1.69 F3 2.00 F4 Q9 1 -0.1611 0.4121 0.7474 1.00000 0.05 0.26 1.01 H1W 1.50 O1W 2.21 H55 2.33 F3 Q10 1 0.0595 0.1035 0.7273 1.00000 0.05 0.26 1.33 F6 1.43 F2 1.87 P1 2.24 O1W Q11 1 0.5190 -0.0657 1.0186 1.00000 0.05 0.25 1.28 O1 1.46 H3 2.05 N3 2.10 O1 Q12 1 -0.0033 0.3668 0.7474 1.00000 0.05 0.25 1.22 O1W 1.53 F1 1.69 H1W 2.41 H55 Q13 1 0.2164 0.3911 0.6841 1.00000 0.05 0.24 1.46 F5 1.56 F3 2.12 P1 2.19 H4W Q14 1 0.2456 -0.0008 0.7108 1.00000 0.05 0.24 1.42 F4 1.81 F3 1.88 H56 1.95 H4W Q15 1 0.1372 0.1753 0.9203 1.00000 0.05 0.24 1.30 H22 1.45 C22 2.16 C17 2.27 C21 Q16 1 0.2465 -0.0114 0.9529 1.00000 0.05 0.24 0.72 C6 0.87 C5 1.80 C7 1.90 C17 Q17 1 0.0388 -0.2813 1.0456 1.00000 0.05 0.23 0.74 H15 1.23 C15 2.09 C14 2.26 H1D Q18 1 0.5210 -0.0535 0.8893 1.00000 0.05 0.23 1.08 O2 1.41 H51 1.84 H2A 2.03 N1 Q19 1 0.4169 0.0074 0.9582 1.00000 0.05 0.23 0.57 H3 0.72 N3 1.80 C7 1.80 C4 Q20 1 0.4980 0.0525 0.8719 1.00000 0.05 0.23 1.13 O2 1.73 H51 1.82 H2A 2.09 H19 Shortest distances between peaks (including symmetry equivalents) 7 12 0.35 8 13 0.88 2 9 1.10 3 9 1.14 18 20 1.21 4 8 1.28 11 19 1.41 2 3 1.45 13 14 1.49 2 10 1.55 4 13 1.62 4 5 1.70 1 12 1.86 11 11 1.87 1 7 1.97 2 7 1.98 2 12 2.02 5 13 2.02 9 14 2.13 8 14 2.32 5 8 2.40 7 9 2.45 10 12 2.54 5 14 2.55 9 10 2.58 2 14 2.58 9 12 2.59 11 17 2.63 3 7 2.65 7 10 2.66 7 10 2.69 17 18 2.71 15 16 2.72 11 19 2.72 10 12 2.75 1 10 2.75 16 19 2.77 3 10 2.83 3 12 2.86 3 14 2.87 17 19 2.89 1 5 2.90 1 2 2.93 18 19 2.94 11 17 2.96 4 14 2.97 Time profile in seconds ----------------------- 0.11: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.05: 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 0.06: Generate ISOR restraints 0.00: Generate NCSY restraints 0.05: Analyse other restraints etc. 0.55: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.05: OSF, H-atoms from difference map 0.06: Set up l.s. refinement 0.00: Generate idealized H-atoms 3.88: Structure factors and derivatives 7.19: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.44: Solve l.s. equations 0.00: Generate HTAB table 0.13: Other dependent quantities, CIF, tables 0.22: Analysis of variance 0.11: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.22: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 09:36:08 Total elapsed time: 13.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++