+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 04skc0010p-1 started at 11:09:19 on 13-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 04skc0010p-1 in P-1 CELL 0.71073 7.2670 7.3373 11.6052 106.343 101.093 93.796 ZERR 2.00 0.0045 0.0036 0.0051 0.045 0.043 0.058 LATT 1 SFAC C H N O UNIT 16 38 2 16 V = 577.92 F(000) = 276.0 Mu = 0.13 mm-1 Cell Wt = 514.48 Rho = 1.478 MERG 2 OMIT -3.00 55.00 EXTI 0.04360 SHEL 7 0.77 DFIX 0.84 0.02 O1W H1W O1W H2W DANG 1.35 0.02 H1W H2W DFIX 0.84 0.02 O2W H21W O2W H22W DANG 1.35 0.02 H21W H22W HTAB O2 O1A HTAB O3 O2W HTAB O3 O4B EQIV_$1 x, y-1, z HTAB O2 O1W_$1 EQIV_$2 x-1, y, z HTAB O4A O1B_$2 EQIV_$3 -x+1, -y, -z+1 HTAB N21 O1A_$3 EQIV_$4 -x+1, -y+1, -z+1 HTAB N21 O1B_$4 HTAB O1W O1A_$4 EQIV_$5 -x, -y+1, -z+1 HTAB O1W O2_$5 EQIV_$6 -x+1, -y+1, -z+2 HTAB O2W O3_$6 EQIV_$7 -x, -y+1, -z+2 HTAB O2W O4B_$7 FMAP 2 PLAN 5 SIZE 0.01 0.08 0.09 ACTA BOND $H WGHT 0.03710 0.39560 L.S. 4 TEMP -153.00 FVAR 1.15778 MOLE 1 C1 1 0.466331 0.403180 0.617994 11.00000 0.01944 0.02241 = 0.01330 0.00678 0.00485 0.00268 C2 1 0.258565 0.418581 0.617551 11.00000 0.01715 0.01536 = 0.02135 0.00486 0.00491 0.00070 AFIX 13 H2 2 0.211318 0.493845 0.560764 11.00000 -1.20000 AFIX 0 C3 1 0.239628 0.527798 0.745957 11.00000 0.01682 0.02372 = 0.02070 0.00787 0.00397 0.00171 AFIX 13 H3 2 0.289858 0.665201 0.763009 11.00000 -1.20000 AFIX 0 C4 1 0.034695 0.517629 0.755595 11.00000 0.02094 0.01562 = 0.01762 -0.00106 0.00528 0.00134 O1A 4 0.516916 0.240816 0.584321 11.00000 0.02057 0.01891 = 0.02521 0.00723 0.00680 0.00528 O1B 4 0.575818 0.559930 0.652985 11.00000 0.01597 0.01928 = 0.02477 0.00623 0.00478 0.00166 O2 4 0.146140 0.238178 0.575979 11.00000 0.01735 0.02015 = 0.03138 0.00332 0.00411 0.00353 AFIX 147 H2O 2 0.216070 0.151825 0.577552 11.00000 -1.50000 AFIX 0 O3 4 0.348241 0.456121 0.834164 11.00000 0.01799 0.05534 = 0.02125 0.01680 0.00721 0.00796 AFIX 147 H3O 2 0.285782 0.446560 0.886495 11.00000 -1.50000 AFIX 0 O4A 4 -0.073907 0.557602 0.664298 11.00000 0.01769 0.02935 = 0.02674 0.01077 0.00730 0.00482 AFIX 147 H4 2 -0.186859 0.546364 0.670967 11.00000 -1.50000 AFIX 0 O4B 4 -0.017683 0.481076 0.840316 11.00000 0.01910 0.03465 = 0.02422 0.01014 0.00949 0.00334 MOLE 2 C22 1 0.181651 -0.007757 0.274502 11.00000 0.01948 0.02430 = 0.02897 0.00807 0.00609 0.00159 AFIX 23 H22A 2 0.148097 -0.128467 0.292283 11.00000 -1.20000 H22B 2 0.131378 0.097628 0.328789 11.00000 -1.20000 AFIX 0 C23 1 0.105962 -0.025605 0.141053 11.00000 0.02442 0.02788 = 0.02437 0.00943 -0.00177 -0.00138 AFIX 23 H23A 2 0.094782 0.101765 0.128856 11.00000 -1.20000 H23B 2 -0.019196 -0.104642 0.109539 11.00000 -1.20000 AFIX 0 C24 1 0.254241 -0.123357 0.078173 11.00000 0.03531 0.02609 = 0.02419 0.00307 0.00312 0.00273 AFIX 23 H24A 2 0.236964 -0.262947 0.066164 11.00000 -1.20000 H24B 2 0.248298 -0.101270 -0.002708 11.00000 -1.20000 AFIX 0 C25 1 0.439330 -0.029337 0.166802 11.00000 0.03038 0.03228 = 0.02949 0.00485 0.00882 0.00500 AFIX 23 H25A 2 0.532994 -0.121537 0.165248 11.00000 -1.20000 H25B 2 0.491749 0.081540 0.145215 11.00000 -1.20000 AFIX 0 N21 3 0.392144 0.034731 0.291797 11.00000 0.02365 0.01949 = 0.02160 0.00414 -0.00022 0.00326 AFIX 23 H21A 2 0.453433 -0.029749 0.342108 11.00000 -1.20000 H21B 2 0.430132 0.163849 0.327743 11.00000 -1.20000 AFIX 0 MOLE 3 O1W 4 0.224838 0.867521 0.562191 11.00000 0.01871 0.02516 = 0.02868 0.00437 0.00413 0.00136 H1W 2 0.110341 0.823124 0.528213 11.00000 0.07853 H2W 2 0.290730 0.816424 0.513840 11.00000 0.07858 MOLE 4 O2W 4 0.299718 0.357163 1.036849 11.00000 0.02553 0.03097 = 0.03318 0.00809 0.01224 0.00552 H21W 2 0.405726 0.411572 1.081054 11.00000 0.19009 H22W 2 0.216839 0.401733 1.074185 11.00000 0.05248 HKLF 4 Covalent radii and connectivity table for 04skc0010p-1 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1A O1B C2 C2 - O2 C3 C1 C3 - O3 C4 C2 C4 - O4B O4A C3 O1A - C1 O1B - C1 O2 - C2 O3 - C3 O4A - C4 O4B - C4 C22 - N21 C23 C23 - C22 C24 C24 - C25 C23 C25 - N21 C24 N21 - C22 C25 O1W - no bonds found O2W - no bonds found Operators for generating equivalent atoms: $1 x, y-1, z $2 x-1, y, z $3 -x+1, -y, -z+1 $4 -x+1, -y+1, -z+1 $5 -x, -y+1, -z+1 $6 -x+1, -y+1, -z+2 $7 -x, -y+1, -z+2 10813 Reflections read, of which 34 rejected -9 =< h =< 9, -9 =< k =< 9, -15 =< l =< 15, Max. 2-theta = 54.97 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 5 6 1 55.58 13.99 3 80.90 -6 0 6 35.48 2.47 6 24.55 2 6 6 194.59 34.60 2 196.91 3 -2 7 55.93 2.52 4 26.09 4 Inconsistent equivalents 2635 Unique reflections, of which 0 suppressed R(int) = 0.0954 R(sigma) = 0.1253 Friedel opposites merged Maximum memory for data reduction = 2257 / 26636 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 = 2749 / 216396 wR2 = 0.1359 before cycle 1 for 2635 data and 174 / 174 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. 2. 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 0.006 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.069; Restrained GooF = 1.068 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0371 * P )^2 + 0.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.15801 0.00381 0.061 OSF 2 0.04371 0.00579 0.018 EXTI Mean shift/esd = 0.017 Maximum = 0.061 for U11 O4A Max. shift = 0.002 A for H1W Max. dU = 0.001 for H22W Least-squares cycle 2 Maximum vector length = 511 Memory required = 2749 / 216396 wR2 = 0.1359 before cycle 2 for 2635 data and 174 / 174 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. 2. 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 0.005 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.069; Restrained GooF = 1.068 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0371 * P )^2 + 0.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.15809 0.00381 0.020 OSF 2 0.04374 0.00579 0.006 EXTI Mean shift/esd = 0.006 Maximum = 0.020 for OSF Max. shift = 0.001 A for H1W Max. dU = 0.000 for H22W Least-squares cycle 3 Maximum vector length = 511 Memory required = 2749 / 216396 wR2 = 0.1360 before cycle 3 for 2635 data and 174 / 174 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. 2. 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 0.005 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.069; Restrained GooF = 1.068 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0371 * P )^2 + 0.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.15809 0.00381 0.000 OSF 2 0.04374 0.00579 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.003 for U11 H2W Max. shift = 0.000 A for H3O Max. dU = 0.000 for H21W Least-squares cycle 4 Maximum vector length = 511 Memory required = 2749 / 216396 wR2 = 0.1360 before cycle 4 for 2635 data and 174 / 174 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. 2. 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 0.005 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.069; Restrained GooF = 1.068 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0371 * P )^2 + 0.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.15809 0.00381 -0.001 OSF 2 0.04374 0.00579 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for U11 H2W Max. shift = 0.000 A for H3O Max. dU = 0.000 for H2W Largest correlation matrix elements 0.705 x H22W / x H21W 0.628 z H22W / x H22W 0.553 x H2W / x H1W 0.677 z H2W / x H2W 0.623 EXTI / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.2113 0.4938 0.5608 13 1.000 0.000 C2 O2 C3 C1 H3 0.2899 0.6652 0.7630 13 1.000 0.000 C3 O3 C4 C2 H2O 0.2161 0.1518 0.5776 147 0.840 0.000 O2 C2 H2O H3O 0.2858 0.4467 0.8865 147 0.840 0.000 O3 C3 H3O H4 -0.1869 0.5464 0.6710 147 0.840 0.000 O4A C4 H4 H22A 0.1314 0.0976 0.3288 23 0.990 0.000 C22 N21 C23 H22B 0.1481 -0.1285 0.2923 23 0.990 0.000 C22 N21 C23 H23A 0.0947 0.1018 0.1289 23 0.990 0.000 C23 C22 C24 H23B -0.0192 -0.1047 0.1095 23 0.990 0.000 C23 C22 C24 H24A 0.2370 -0.2629 0.0661 23 0.990 0.000 C24 C25 C23 H24B 0.2483 -0.1012 -0.0027 23 0.990 0.000 C24 C25 C23 H25A 0.5330 -0.1215 0.1652 23 0.990 0.000 C25 N21 C24 H25B 0.4917 0.0816 0.1452 23 0.990 0.000 C25 N21 C24 H21A 0.4534 -0.0298 0.3421 23 0.920 0.000 N21 C22 C25 H21B 0.4301 0.1638 0.3278 23 0.920 0.000 N21 C22 C25 04skc0010p-1 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.46632 0.40317 0.61800 1.00000 0.01943 0.02230 0.01335 0.00671 0.00484 0.00258 0.01791 0.00607 0.00038 0.00042 0.00025 0.00000 0.00143 0.00176 0.00151 0.00129 0.00122 0.00133 0.00066 C2 0.25857 0.41858 0.61755 1.00000 0.01719 0.01543 0.02131 0.00483 0.00493 0.00071 0.01809 0.00582 0.00036 0.00040 0.00027 0.00000 0.00140 0.00157 0.00158 0.00127 0.00123 0.00116 0.00065 H2 0.21133 0.49384 0.56076 1.00000 0.02171 0.00000 0.00000 C3 0.23964 0.52782 0.74596 1.00000 0.01684 0.02381 0.02071 0.00788 0.00394 0.00167 0.02027 0.00610 0.00037 0.00043 0.00026 0.00000 0.00143 0.00171 0.00165 0.00137 0.00127 0.00122 0.00068 H3 0.28988 0.66522 0.76302 1.00000 0.02433 0.00000 0.00000 C4 0.03469 0.51764 0.75559 1.00000 0.02098 0.01567 0.01766 -0.00105 0.00535 0.00135 0.01927 0.00586 0.00038 0.00040 0.00027 0.00000 0.00150 0.00161 0.00160 0.00129 0.00133 0.00120 0.00068 O1A 0.51692 0.24082 0.58432 1.00000 0.02059 0.01896 0.02524 0.00724 0.00680 0.00526 0.02109 0.00409 0.00025 0.00028 0.00018 0.00000 0.00103 0.00119 0.00120 0.00092 0.00090 0.00085 0.00050 O1B 0.57583 0.55992 0.65299 1.00000 0.01600 0.01937 0.02481 0.00625 0.00481 0.00167 0.02012 0.00400 0.00024 0.00027 0.00018 0.00000 0.00098 0.00116 0.00117 0.00092 0.00087 0.00084 0.00049 O2 0.14614 0.23818 0.57598 1.00000 0.01739 0.02019 0.03139 0.00334 0.00414 0.00350 0.02404 0.00398 0.00025 0.00027 0.00019 0.00000 0.00099 0.00120 0.00127 0.00100 0.00095 0.00086 0.00053 H2O 0.21607 0.15183 0.57755 1.00000 0.03606 0.00000 0.00000 O3 0.34822 0.45611 0.83416 1.00000 0.01800 0.05534 0.02129 0.01676 0.00721 0.00797 0.02988 0.00459 0.00026 0.00033 0.00019 0.00000 0.00106 0.00158 0.00123 0.00114 0.00092 0.00101 0.00057 H3O 0.28582 0.44671 0.88655 1.00000 0.04482 0.00000 0.00000 O4A -0.07392 0.55760 0.66430 1.00000 0.01777 0.02932 0.02670 0.01077 0.00730 0.00485 0.02367 0.00432 0.00026 0.00029 0.00019 0.00000 0.00102 0.00127 0.00122 0.00098 0.00093 0.00091 0.00052 H4 -0.18687 0.54636 0.67098 1.00000 0.03551 0.00000 0.00000 O4B -0.01769 0.48108 0.84031 1.00000 0.01910 0.03470 0.02426 0.01012 0.00948 0.00334 0.02510 0.00422 0.00025 0.00030 0.00019 0.00000 0.00106 0.00136 0.00122 0.00103 0.00094 0.00090 0.00053 C22 0.18164 -0.00775 0.27450 1.00000 0.01955 0.02433 0.02898 0.00807 0.00611 0.00159 0.02422 0.00625 0.00038 0.00044 0.00028 0.00000 0.00151 0.00178 0.00182 0.00144 0.00134 0.00127 0.00073 H22A 0.13138 0.09764 0.32878 1.00000 0.02907 0.00000 0.00000 H22B 0.14808 -0.12846 0.29228 1.00000 0.02907 0.00000 0.00000 C23 0.10594 -0.02561 0.14105 1.00000 0.02446 0.02794 0.02436 0.00944 -0.00173 -0.00135 0.02648 0.00642 0.00041 0.00046 0.00028 0.00000 0.00157 0.00186 0.00176 0.00145 0.00137 0.00133 0.00076 H23A 0.09473 0.10175 0.12885 1.00000 0.03177 0.00000 0.00000 H23B -0.01921 -0.10466 0.10954 1.00000 0.03177 0.00000 0.00000 C24 0.25423 -0.12335 0.07816 1.00000 0.03527 0.02609 0.02426 0.00308 0.00319 0.00275 0.03001 0.00643 0.00041 0.00046 0.00029 0.00000 0.00181 0.00189 0.00180 0.00148 0.00149 0.00144 0.00079 H24A 0.23696 -0.26294 0.06614 1.00000 0.03602 0.00000 0.00000 H24B 0.24829 -0.10125 -0.00271 1.00000 0.03602 0.00000 0.00000 C25 0.43933 -0.02933 0.16680 1.00000 0.03046 0.03225 0.02947 0.00479 0.00878 0.00502 0.03131 0.00669 0.00043 0.00048 0.00029 0.00000 0.00173 0.00199 0.00191 0.00153 0.00150 0.00145 0.00080 H25A 0.53299 -0.12153 0.16524 1.00000 0.03757 0.00000 0.00000 H25B 0.49174 0.08155 0.14522 1.00000 0.03757 0.00000 0.00000 N21 0.39215 0.03472 0.29180 1.00000 0.02366 0.01952 0.02161 0.00413 -0.00023 0.00323 0.02274 0.00497 0.00031 0.00035 0.00022 0.00000 0.00130 0.00142 0.00138 0.00111 0.00111 0.00105 0.00061 H21A 0.45343 -0.02978 0.34210 1.00000 0.02729 0.00000 0.00000 H21B 0.43015 0.16384 0.32775 1.00000 0.02729 0.00000 0.00000 O1W 0.22483 0.86752 0.56218 1.00000 0.01876 0.02515 0.02872 0.00439 0.00415 0.00139 0.02521 0.00434 0.00030 0.00031 0.00020 0.00000 0.00114 0.00128 0.00131 0.00100 0.00106 0.00095 0.00053 H1W 0.11040 0.82283 0.52824 1.00000 0.07906 0.06069 0.00266 0.00575 0.00347 0.00000 0.01534 H2W 0.29078 0.81653 0.51382 1.00000 0.07819 0.08052 0.00427 0.00567 0.00317 0.00000 0.01636 O2W 0.29971 0.35717 1.03686 1.00000 0.02557 0.03099 0.03324 0.00813 0.01222 0.00554 0.02935 0.00492 0.00032 0.00032 0.00021 0.00000 0.00122 0.00138 0.00139 0.00107 0.00115 0.00104 0.00057 H21W 0.40575 0.41144 1.08103 1.00000 0.18975 0.06711 0.00334 0.00893 0.00474 0.00000 0.03332 H22W 0.21690 0.40172 1.07428 1.00000 0.05332 0.07635 0.00381 0.00503 0.00305 0.00000 0.01270 Final Structure Factor Calculation for 04skc0010p-1 in P-1 Total number of l.s. parameters = 174 Maximum vector length = 511 Memory required = 2575 / 22995 wR2 = 0.1360 before cycle 5 for 2635 data and 0 / 174 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. 2. 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 0.005 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.069; Restrained GooF = 1.068 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0371 * P )^2 + 0.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0808 for 1472 Fo > 4sig(Fo) and 0.1574 for all 2635 data wR2 = 0.1360, GooF = S = 1.069, Restrained GooF = 1.068 for all data Occupancy sum of asymmetric unit = 17.00 for non-hydrogen and 19.00 for hydrogen atoms Principal mean square atomic displacements U 0.0223 0.0195 0.0119 C1 0.0219 0.0177 0.0146 C2 0.0243 0.0198 0.0167 C3 0.0257 0.0204 0.0117 C4 0.0255 0.0212 0.0165 O1A 0.0251 0.0196 0.0157 O1B 0.0354 0.0199 0.0168 O2 0.0554 0.0189 0.0153 O3 0.0303 0.0244 0.0164 O4A 0.0348 0.0258 0.0147 O4B 0.0291 0.0248 0.0188 C22 0.0357 0.0252 0.0186 C23 0.0374 0.0311 0.0215 C24 0.0375 0.0313 0.0252 C25 0.0304 0.0197 0.0181 N21 0.0327 0.0243 0.0186 O1W 0.0361 0.0314 0.0206 O2W Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.022 0.031 0.042 0.054 0.070 0.089 0.121 0.173 1.000 Number in group 271. 278. 248. 262. 265. 261. 259. 263. 264. 264. GooF 0.977 1.013 1.101 0.950 1.175 1.128 1.190 1.089 0.974 1.072 K 16.080 3.034 3.165 1.654 1.448 1.165 1.190 1.068 1.005 1.017 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.32 1.66 inf Number in group 271. 263. 266. 254. 264. 263. 265. 263. 261. 265. GooF 1.230 1.177 0.962 1.081 1.038 1.081 0.912 1.014 0.938 1.202 K 1.488 1.391 1.163 1.162 1.252 1.170 1.025 1.114 1.016 1.005 R1 0.441 0.392 0.274 0.262 0.224 0.172 0.085 0.093 0.046 0.034 Recommended weighting scheme: WGHT 0.0372 0.4040 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) -9 1 1 601.34 7.31 5.90 0.030 0.80 9 -2 1 22.25 117.41 4.72 0.120 0.78 -6 1 9 227.05 27.80 4.57 0.058 0.93 5 -3 11 637.14 6.33 4.42 0.028 0.77 3 -2 13 -7.18 21.86 4.40 0.052 0.77 4 -2 12 -2.12 28.04 4.11 0.058 0.77 -2 -9 4 1114.28 45.21 4.08 0.074 0.78 5 -5 7 81.35 171.82 4.05 0.145 0.90 5 -6 3 24.41 62.90 4.05 0.088 0.95 7 4 1 410.60 19.04 3.90 0.048 0.81 -8 4 3 208.08 125.72 3.89 0.124 0.82 -5 -6 11 18.97 52.62 3.40 0.080 0.80 6 -3 5 1346.46 55.03 3.37 0.082 0.96 6 -5 7 0.86 43.82 3.37 0.073 0.83 3 3 10 594.49 84.01 3.28 0.101 0.77 2 -3 9 278.69 1.51 3.26 0.014 1.11 -1 1 1 617.57 730.37 3.18 0.298 4.66 0 -1 1 0.96 20.83 3.17 0.050 6.89 2 -1 10 982.56 15.40 3.12 0.043 1.01 3 -3 12 659.40 6.24 2.94 0.028 0.83 -9 -2 4 243.41 147.65 2.94 0.134 0.78 6 -5 6 -4.15 24.37 2.94 0.054 0.86 4 2 6 554.99 20.96 2.91 0.051 1.01 -8 2 3 6.36 25.09 2.90 0.055 0.89 -1 -1 1 1633.30 1866.91 2.85 0.477 4.97 2 -4 7 1649.23 118.10 2.81 0.120 1.25 4 -2 8 68.99 104.81 2.74 0.113 1.02 -6 -5 1 13.55 38.37 2.74 0.068 0.87 -4 3 2 29.85 17.15 2.67 0.046 1.45 0 -4 7 383.73 325.98 2.63 0.199 1.38 3 -2 7 41.76 97.20 2.62 0.109 1.23 3 -5 10 61.33 36.38 2.62 0.067 0.90 0 0 2 528.85 609.86 2.60 0.273 5.43 5 -7 3 73.16 27.17 2.60 0.058 0.87 6 1 3 911.49 794.48 2.56 0.311 1.01 -4 1 0 109.00 87.93 2.54 0.104 1.77 -9 2 0 5.73 23.67 2.54 0.054 0.79 8 -4 4 -8.83 12.64 2.54 0.039 0.78 8 -2 1 13.16 0.02 2.53 0.001 0.87 -8 -4 7 3.37 38.96 2.52 0.069 0.78 -2 3 9 143.62 103.95 2.46 0.113 0.99 0 -5 10 41.41 15.19 2.46 0.043 1.02 2 0 11 -19.24 22.46 2.46 0.052 0.90 -7 1 2 86.34 110.59 2.45 0.116 1.04 -4 -2 7 23.56 40.90 2.45 0.071 1.31 -7 -2 7 64.71 14.82 2.45 0.042 0.93 2 2 7 16.66 2.65 2.44 0.018 1.13 -4 2 0 12.71 5.18 2.44 0.025 1.67 -4 7 3 40.83 1.41 2.44 0.013 0.86 -6 -6 1 -13.55 14.26 2.43 0.042 0.80 Bond lengths and angles C1 - Distance Angles O1A 1.2483 (0.0033) O1B 1.2699 (0.0034) 124.93 (0.25) C2 1.5205 (0.0039) 118.72 (0.25) 116.35 (0.25) C1 - O1A O1B C2 - Distance Angles O2 1.4135 (0.0033) C3 1.5177 (0.0040) 110.48 (0.23) C1 1.5205 (0.0039) 112.79 (0.23) 109.18 (0.22) H2 1.0000 108.08 108.08 108.08 C2 - O2 C3 C1 C3 - Distance Angles O3 1.4123 (0.0034) C4 1.5134 (0.0039) 110.69 (0.24) C2 1.5177 (0.0040) 110.17 (0.24) 111.08 (0.23) H3 1.0000 108.27 108.27 108.27 C3 - O3 C4 C2 C4 - Distance Angles O4B 1.2094 (0.0034) O4A 1.3095 (0.0034) 125.33 (0.26) C3 1.5134 (0.0039) 122.66 (0.26) 111.99 (0.25) C4 - O4B O4A O1A - Distance Angles C1 1.2483 (0.0033) O1A - O1B - Distance Angles C1 1.2699 (0.0034) O1B - O2 - Distance Angles C2 1.4135 (0.0033) H2O 0.8400 109.47 O2 - C2 O3 - Distance Angles C3 1.4123 (0.0034) H3O 0.8400 109.47 O3 - C3 O4A - Distance Angles C4 1.3095 (0.0034) H4 0.8400 109.47 O4A - C4 O4B - Distance Angles C4 1.2094 (0.0034) O4B - C22 - Distance Angles N21 1.5037 (0.0036) C23 1.5055 (0.0041) 104.02 (0.24) H22A 0.9900 110.95 110.95 H22B 0.9900 110.95 110.95 108.96 C22 - N21 C23 H22A C23 - Distance Angles C22 1.5055 (0.0041) C24 1.5227 (0.0045) 103.08 (0.24) H23A 0.9900 111.15 111.15 H23B 0.9900 111.15 111.15 109.09 C23 - C22 C24 H23A C24 - Distance Angles C25 1.5128 (0.0043) C23 1.5227 (0.0045) 103.65 (0.25) H24A 0.9900 111.03 111.03 H24B 0.9900 111.03 111.03 109.01 C24 - C25 C23 H24A C25 - Distance Angles N21 1.5072 (0.0040) C24 1.5128 (0.0043) 105.36 (0.25) H25A 0.9900 110.67 110.67 H25B 0.9900 110.67 110.67 108.78 C25 - N21 C24 H25A N21 - Distance Angles C22 1.5037 (0.0036) C25 1.5072 (0.0040) 107.85 (0.22) H21A 0.9200 110.14 110.14 H21B 0.9200 110.14 110.14 108.45 N21 - C22 C25 H21A O1W - Distance Angles H1W 0.8481 (0.0180) H2W 0.8329 (0.0181) 107.44 (2.62) O1W - H1W O2W - Distance Angles H21W 0.8412 (0.0197) H22W 0.8393 (0.0179) 107.52 (2.93) O2W - H21W Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 2.22 2.676(3) 114.2 O2-H2O...O1A 0.84 2.02 2.726(3) 141.6 O3-H3O...O2W 0.84 2.22 2.691(3) 115.9 O3-H3O...O4B 0.84 2.05 2.783(3) 145.6 O2-H2O...O1W_$1 0.84 1.71 2.525(3) 162.9 O4A-H4...O1B_$2 0.92 1.97 2.835(3) 155.4 N21-H21A...O1A_$3 0.92 1.98 2.844(3) 155.8 N21-H21B...O1B_$4 0.833(18) 1.962(19) 2.777(3) 166(4) O1W-H2W...O1A_$4 0.848(18) 1.96(2) 2.793(3) 165(4) O1W-H1W...O2_$5 0.84(2) 1.91(2) 2.752(4) 173(7) O2W-H21W...O3_$6 0.839(18) 2.014(19) 2.852(3) 177(4) O2W-H22W...O4B_$7 FMAP and GRID set by program FMAP 2 1 20 GRID -2.941 -2 -2 2.941 2 2 R1 = 0.1573 for 2635 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.30 at 0.1493 0.3619 0.1422 [ 1.10 A from H22W ] Deepest hole -0.29 at 0.5013 0.7591 0.7020 [ 0.91 A from H21B ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 2586 / 17215 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1493 0.3619 1.1422 1.00000 0.05 0.30 1.10 H22W 1.54 O4B 1.78 O2W 1.88 H23A Q2 1 -0.1551 0.5188 0.7724 1.00000 0.05 0.28 1.23 H4 1.25 O4B 1.43 C4 1.57 O4A Q3 1 0.0142 -0.2074 0.0034 1.00000 0.05 0.28 1.33 H23B 1.75 C23 1.77 H24A 1.77 C24 Q4 1 0.3259 0.6320 0.9572 1.00000 0.05 0.27 1.35 H3O 1.56 H24A 1.68 O3 2.02 H24B Q5 1 0.6248 0.5137 0.7635 1.00000 0.05 0.26 1.40 O1B 1.79 C1 1.79 H21W 1.92 H22W Shortest distances between peaks (including symmetry equivalents) 1 2 1.11 2 5 1.58 1 5 1.81 1 3 1.88 3 4 2.70 2 3 2.85 Time profile in seconds ----------------------- 0.06: 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 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.44: Structure factors and derivatives 0.48: 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 0.03: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 04skc0010p-1 finished at 11:09:21 Total CPU time: 1.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++