+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 10:04:17 on 06-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P2(1) CELL 0.71073 5.5528 16.0180 11.7768 90.000 103.378 90.000 ZERR 2.00 0.0006 0.0018 0.0019 0.000 0.009 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N O UNIT 40 56 4 12 V = 1019.06 F(000) = 420.0 Mu = 0.09 mm-1 Cell Wt = 784.89 Rho = 1.279 MERG 4 OMIT -3.00 55.00 EXTI 0.04172 SHEL 7 0.77 HTAB O2 O3 HTAB O3 O4A EQIV_$1 x-1, y, z HTAB O2 O1B_$1 EQIV_$2 -x+1, y-1/2, -z+1 HTAB N19 O1B_$2 EQIV_$3 -x, y-1/2, -z+1 HTAB N19 O1A_$3 EQIV_$4 x, y, z+1 HTAB N19 O4B_$4 HTAB N29 O1A_$4 EQIV_$5 -x, y+1/2, -z+1 HTAB N29 O4A_$5 EQIV_$6 -x+1, y+1/2, -z+1 HTAB N29 O4B_$6 FMAP 2 PLAN 10 SIZE 0.02 0.15 0.50 ACTA 50.00 BOND $H WGHT 0.03910 0.23790 L.S. 4 TEMP -153.00 FVAR 0.91904 C1 1 0.435564 0.182416 0.008631 11.00000 0.02782 0.01719 = 0.02653 0.00146 0.01548 0.00095 C2 1 0.290536 0.103239 0.020507 11.00000 0.01864 0.01784 = 0.02524 0.00020 0.00594 -0.00063 AFIX 13 H2 2 0.370776 0.056359 -0.013044 11.00000 -1.20000 AFIX 0 C3 1 0.312981 0.083379 0.149499 11.00000 0.02352 0.01855 = 0.02137 -0.00123 0.00423 -0.00245 AFIX 13 H3 2 0.492154 0.080809 0.190094 11.00000 -1.20000 AFIX 0 C4 1 0.192444 -0.000461 0.162594 11.00000 0.02927 0.01917 = 0.02017 0.00326 0.00275 -0.00197 O1A 4 0.323084 0.243593 -0.046102 11.00000 0.04330 0.02089 = 0.03507 0.00932 0.02145 0.00850 O1B 4 0.662801 0.180840 0.055885 11.00000 0.02272 0.02477 = 0.04561 -0.00194 0.01257 -0.00462 O2 4 0.040651 0.105755 -0.040797 11.00000 0.02231 0.03056 = 0.02405 -0.00197 0.00474 0.00219 AFIX 147 H2O 2 -0.043906 0.129597 0.000292 11.00000 -1.50000 AFIX 0 O3 4 0.196397 0.148336 0.200318 11.00000 0.03384 0.02133 = 0.02731 -0.00456 0.01323 -0.00370 AFIX 147 H3O 2 0.075028 0.128682 0.222763 11.00000 -1.50000 AFIX 0 O4A 4 0.010429 -0.000068 0.208222 11.00000 0.04141 0.02771 = 0.04154 0.00162 0.02146 -0.00810 O4B 4 0.282697 -0.064614 0.125304 11.00000 0.03037 0.01845 = 0.03092 0.00169 0.00262 0.00053 MOLE 2 C11 1 0.035167 -0.110627 0.773272 11.00000 0.01735 0.02495 = 0.02012 -0.00188 0.00149 0.00123 C12 1 0.059267 -0.025823 0.754674 11.00000 0.02420 0.02259 = 0.02430 -0.00038 0.00595 0.00375 AFIX 43 H12 2 -0.018205 0.013356 0.795259 11.00000 -1.20000 AFIX 0 C13 1 0.196443 0.002409 0.676799 11.00000 0.02514 0.02725 = 0.02770 0.00300 0.00612 0.00197 AFIX 43 H13 2 0.212216 0.060605 0.664759 11.00000 -1.20000 AFIX 0 C14 1 0.309060 -0.054006 0.617336 11.00000 0.02724 0.03761 = 0.02574 0.00185 0.01036 0.00166 AFIX 43 H14 2 0.401187 -0.034715 0.563881 11.00000 -1.20000 AFIX 0 C15 1 0.287780 -0.138732 0.635584 11.00000 0.03088 0.03583 = 0.02898 -0.00861 0.01108 0.00466 AFIX 43 H15 2 0.365701 -0.177628 0.594782 11.00000 -1.20000 AFIX 0 C16 1 0.152362 -0.167030 0.713638 11.00000 0.02414 0.02321 = 0.02958 -0.00537 0.00535 -0.00072 AFIX 43 H16 2 0.139634 -0.225259 0.726413 11.00000 -1.20000 AFIX 0 C17 1 -0.117977 -0.143955 0.854522 11.00000 0.01888 0.01952 = 0.02533 -0.00090 0.00330 0.00122 AFIX 13 H17 2 -0.229828 -0.188368 0.811846 11.00000 -1.20000 AFIX 0 C18 1 -0.277681 -0.079927 0.898390 11.00000 0.01960 0.02228 = 0.02889 0.00029 0.00616 0.00154 AFIX 33 H18A 2 -0.389172 -0.053067 0.831689 11.00000 -1.20000 H18B 2 -0.171264 -0.037624 0.945089 11.00000 -1.20000 H18C 2 -0.375422 -0.107869 0.946635 11.00000 -1.20000 AFIX 0 N19 3 0.048229 -0.183417 0.959974 11.00000 0.02193 0.02017 = 0.02377 0.00041 0.00611 0.00113 AFIX 33 H19A 2 0.146633 -0.222120 0.936620 11.00000 -1.20000 H19B 2 -0.045683 -0.208600 1.003966 11.00000 -1.20000 H19C 2 0.144273 -0.143400 1.003122 11.00000 -1.20000 AFIX 0 MOLE 3 C21 1 0.384238 0.269495 0.631694 11.00000 0.02562 0.01920 = 0.02238 0.00175 0.00916 -0.00082 C22 1 0.313604 0.226938 0.526242 11.00000 0.03018 0.02848 = 0.02575 -0.00035 0.00396 0.00328 AFIX 43 H22 2 0.164197 0.241926 0.472598 11.00000 -1.20000 AFIX 0 C23 1 0.458182 0.162855 0.498165 11.00000 0.04120 0.02805 = 0.02372 -0.00504 0.00915 0.00165 AFIX 43 H23 2 0.408293 0.134436 0.425719 11.00000 -1.20000 AFIX 0 C24 1 0.674969 0.140730 0.576288 11.00000 0.03137 0.02619 = 0.03328 -0.00206 0.01100 0.00652 AFIX 43 H24 2 0.775080 0.097252 0.557189 11.00000 -1.20000 AFIX 0 C25 1 0.746223 0.181225 0.681203 11.00000 0.02621 0.02902 = 0.03220 -0.00216 0.00414 0.00700 AFIX 43 H25 2 0.894504 0.165321 0.734968 11.00000 -1.20000 AFIX 0 C26 1 0.601314 0.245829 0.709260 11.00000 0.02749 0.02581 = 0.02636 -0.00492 0.00546 0.00283 AFIX 43 H26 2 0.651891 0.273764 0.782048 11.00000 -1.20000 AFIX 0 C27 1 0.226576 0.342187 0.652997 11.00000 0.02356 0.02103 = 0.02186 0.00016 0.00769 0.00264 AFIX 13 H27 2 0.048594 0.326643 0.623693 11.00000 -1.20000 AFIX 0 C28 1 0.277000 0.420763 0.589148 11.00000 0.03567 0.02508 = 0.02501 0.00404 0.01095 0.00192 AFIX 33 H28A 2 0.250171 0.408924 0.505513 11.00000 -1.20000 H28B 2 0.448666 0.438554 0.619640 11.00000 -1.20000 H28C 2 0.164570 0.465307 0.601259 11.00000 -1.20000 AFIX 0 N29 3 0.268636 0.363125 0.779223 11.00000 0.02577 0.01881 = 0.02463 0.00210 0.01017 0.00228 AFIX 33 H29A 2 0.240455 0.317126 0.819614 11.00000 -1.20000 H29B 2 0.163431 0.404669 0.788938 11.00000 -1.20000 H29C 2 0.427733 0.380380 0.806276 11.00000 -1.20000 AFIX 0 HKLF 4 Covalent radii and connectivity table for s92 in P2(1) C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1B O1A C2 C2 - O2 C1 C3 C3 - O3 C4 C2 C4 - O4A O4B C3 O1A - C1 O1B - C1 O2 - C2 O3 - C3 O4A - C4 O4B - C4 C11 - C12 C16 C17 C12 - C11 C13 C13 - C14 C12 C14 - C13 C15 C15 - C14 C16 C16 - C15 C11 C17 - N19 C11 C18 C18 - C17 N19 - C17 C21 - C26 C22 C27 C22 - C23 C21 C23 - C24 C22 C24 - C25 C23 C25 - C24 C26 C26 - C21 C25 C27 - N29 C21 C28 C28 - C27 N29 - C27 Operators for generating equivalent atoms: $1 x-1, y, z $2 -x+1, y-1/2, -z+1 $3 -x, y-1/2, -z+1 $4 x, y, z+1 $5 -x, y+1/2, -z+1 $6 -x+1, y+1/2, -z+1 Floating origin restraints generated 7935 Reflections read, of which 18 rejected -5 =< h =< 6, -19 =< k =< 19, -14 =< l =< 15, Max. 2-theta = 54.96 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 0 0 8 2.84 0.60 3 3.53 2 5 9 14.12 0.82 4 5.58 2 Inconsistent equivalents 2248 Unique reflections, of which 0 suppressed R(int) = 0.0499 R(sigma) = 0.0492 Friedel opposites merged Maximum memory for data reduction = 3068 / 21929 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 = 3828 / 318035 wR2 = 0.0922 before cycle 1 for 2248 data and 256 / 256 parameters GooF = S = 1.048; Restrained GooF = 1.048 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0391 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.91931 0.00237 0.115 OSF 2 0.04186 0.00506 0.029 EXTI Mean shift/esd = 0.015 Maximum = 0.115 for OSF Max. shift = 0.000 A for H2O Max. dU = 0.000 for C17 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3828 / 318035 wR2 = 0.0922 before cycle 2 for 2248 data and 256 / 256 parameters GooF = S = 1.048; Restrained GooF = 1.047 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0391 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.91942 0.00237 0.046 OSF 2 0.04193 0.00506 0.013 EXTI Mean shift/esd = 0.005 Maximum = 0.046 for OSF Max. shift = 0.000 A for H2O Max. dU = 0.000 for C15 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3828 / 318035 wR2 = 0.0922 before cycle 3 for 2248 data and 256 / 256 parameters GooF = S = 1.048; Restrained GooF = 1.047 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0391 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.91943 0.00237 0.002 OSF 2 0.04194 0.00506 0.003 EXTI Mean shift/esd = 0.000 Maximum = 0.003 for EXTI Max. shift = 0.000 A for H2O Max. dU = 0.000 for C12 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3828 / 318035 wR2 = 0.0922 before cycle 4 for 2248 data and 256 / 256 parameters GooF = S = 1.048; Restrained GooF = 1.047 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0391 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.91943 0.00237 0.000 OSF 2 0.04194 0.00506 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for tors H3O Max. shift = 0.000 A for H3O Max. dU = 0.000 for C12 Largest correlation matrix elements 0.599 EXTI / OSF 0.508 U13 O4A / U33 O4A Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.3708 0.0563 -0.0130 13 1.000 0.000 C2 O2 C1 C3 H3 0.4922 0.0808 0.1901 13 1.000 0.000 C3 O3 C4 C2 H2O -0.0439 0.1296 0.0003 147 0.840 0.000 O2 C2 H2O H3O 0.0751 0.1287 0.2228 147 0.840 0.000 O3 C3 H3O H12 -0.0182 0.0134 0.7953 43 0.950 0.000 C12 C11 C13 H13 0.2122 0.0606 0.6648 43 0.950 0.000 C13 C14 C12 H14 0.4013 -0.0347 0.5639 43 0.950 0.000 C14 C13 C15 H15 0.3657 -0.1776 0.5948 43 0.950 0.000 C15 C14 C16 H16 0.1397 -0.2253 0.7264 43 0.950 0.000 C16 C15 C11 H17 -0.2298 -0.1884 0.8118 13 1.000 0.000 C17 N19 C11 C18 H18A -0.3892 -0.0531 0.8317 33 0.980 0.000 C18 C17 H18A H18B -0.1713 -0.0376 0.9451 33 0.980 0.000 C18 C17 H18A H18C -0.3754 -0.1079 0.9466 33 0.980 0.000 C18 C17 H18A H19A 0.1466 -0.2221 0.9366 33 0.910 0.000 N19 C17 H19A H19B -0.0457 -0.2086 1.0040 33 0.910 0.000 N19 C17 H19A H19C 0.1443 -0.1434 1.0031 33 0.910 0.000 N19 C17 H19A H22 0.1642 0.2419 0.4726 43 0.950 0.000 C22 C23 C21 H23 0.4083 0.1344 0.4257 43 0.950 0.000 C23 C24 C22 H24 0.7751 0.0972 0.5572 43 0.950 0.000 C24 C25 C23 H25 0.8945 0.1653 0.7350 43 0.950 0.000 C25 C24 C26 H26 0.6519 0.2738 0.7821 43 0.950 0.000 C26 C21 C25 H27 0.0486 0.3266 0.6237 13 1.000 0.000 C27 N29 C21 C28 H28A 0.2502 0.4089 0.5055 33 0.980 0.000 C28 C27 H28A H28B 0.4486 0.4386 0.6196 33 0.980 0.000 C28 C27 H28A H28C 0.1645 0.4653 0.6012 33 0.980 0.000 C28 C27 H28A H29A 0.2405 0.3171 0.8196 33 0.910 0.000 N29 C27 H29A H29B 0.1634 0.4047 0.7889 33 0.910 0.000 N29 C27 H29A H29C 0.4277 0.3804 0.8063 33 0.910 0.000 N29 C27 H29A s92 in P2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.43557 0.18242 0.00863 1.00000 0.02789 0.01720 0.02660 0.00146 0.01551 0.00095 0.02240 0.00541 0.00050 0.00017 0.00023 0.00000 0.00153 0.00121 0.00139 0.00106 0.00114 0.00111 0.00056 C2 0.29052 0.10323 0.02051 1.00000 0.01874 0.01786 0.02525 0.00021 0.00597 -0.00065 0.02047 0.00505 0.00049 0.00016 0.00023 0.00000 0.00136 0.00123 0.00143 0.00099 0.00105 0.00099 0.00055 H2 0.37075 0.05635 -0.01304 1.00000 0.02457 0.00000 0.00000 C3 0.31298 0.08339 0.14951 1.00000 0.02356 0.01859 0.02137 -0.00121 0.00420 -0.00247 0.02134 0.00506 0.00052 0.00016 0.00023 0.00000 0.00139 0.00126 0.00136 0.00099 0.00105 0.00104 0.00055 H3 0.49216 0.08082 0.19010 1.00000 0.02561 0.00000 0.00000 C4 0.19244 -0.00046 0.16259 1.00000 0.02929 0.01919 0.02022 0.00326 0.00279 -0.00196 0.02338 0.00520 0.00052 0.00017 0.00023 0.00000 0.00147 0.00127 0.00140 0.00106 0.00111 0.00114 0.00057 O1A 0.32310 0.24359 -0.04610 1.00000 0.04331 0.02092 0.03510 0.00933 0.02145 0.00849 0.03109 0.00431 0.00040 0.00012 0.00018 0.00000 0.00128 0.00099 0.00119 0.00082 0.00099 0.00089 0.00050 O1B 0.66281 0.18083 0.05589 1.00000 0.02275 0.02482 0.04566 -0.00195 0.01258 -0.00462 0.03031 0.00382 0.00036 0.00012 0.00018 0.00000 0.00106 0.00098 0.00126 0.00090 0.00092 0.00084 0.00046 O2 0.04065 0.10575 -0.04080 1.00000 0.02233 0.03061 0.02408 -0.00194 0.00476 0.00219 0.02577 0.00366 0.00036 0.00012 0.00017 0.00000 0.00106 0.00105 0.00103 0.00078 0.00077 0.00081 0.00044 H2O -0.04388 0.12964 0.00026 1.00000 0.03866 0.00000 0.00000 O3 0.19640 0.14834 0.20033 1.00000 0.03387 0.02138 0.02730 -0.00454 0.01320 -0.00372 0.02652 0.00375 0.00038 0.00012 0.00017 0.00000 0.00120 0.00093 0.00107 0.00077 0.00088 0.00083 0.00045 H3O 0.07505 0.12868 0.22278 1.00000 0.03978 0.00000 0.00000 O4A 0.01042 -0.00007 0.20822 1.00000 0.04147 0.02778 0.04154 0.00161 0.02144 -0.00812 0.03500 0.00436 0.00042 0.00013 0.00020 0.00000 0.00128 0.00104 0.00127 0.00091 0.00104 0.00096 0.00052 O4B 0.28268 -0.06461 0.12530 1.00000 0.03039 0.01848 0.03093 0.00171 0.00261 0.00052 0.02733 0.00360 0.00037 0.00011 0.00017 0.00000 0.00109 0.00090 0.00110 0.00078 0.00085 0.00080 0.00045 C11 0.03517 -0.11062 0.77327 1.00000 0.01740 0.02500 0.02017 -0.00189 0.00150 0.00123 0.02132 0.00498 0.00048 0.00016 0.00023 0.00000 0.00133 0.00134 0.00134 0.00100 0.00102 0.00102 0.00056 C12 0.05926 -0.02582 0.75467 1.00000 0.02425 0.02262 0.02430 -0.00039 0.00593 0.00374 0.02367 0.00539 0.00052 0.00017 0.00024 0.00000 0.00138 0.00135 0.00144 0.00103 0.00106 0.00106 0.00057 H12 -0.01822 0.01336 0.79526 1.00000 0.02841 0.00000 0.00000 C13 0.19644 0.00240 0.67680 1.00000 0.02519 0.02726 0.02774 0.00296 0.00614 0.00196 0.02673 0.00562 0.00052 0.00019 0.00025 0.00000 0.00144 0.00140 0.00149 0.00117 0.00114 0.00119 0.00060 H13 0.21219 0.06060 0.66476 1.00000 0.03207 0.00000 0.00000 C14 0.30910 -0.05400 0.61734 1.00000 0.02725 0.03763 0.02577 0.00183 0.01034 0.00166 0.02953 0.00566 0.00054 0.00019 0.00025 0.00000 0.00150 0.00177 0.00149 0.00121 0.00118 0.00124 0.00065 H14 0.40126 -0.03471 0.56390 1.00000 0.03544 0.00000 0.00000 C15 0.28777 -0.13873 0.63559 1.00000 0.03095 0.03585 0.02906 -0.00861 0.01114 0.00463 0.03127 0.00578 0.00055 0.00019 0.00026 0.00000 0.00156 0.00167 0.00158 0.00125 0.00123 0.00132 0.00066 H15 0.36566 -0.17763 0.59478 1.00000 0.03752 0.00000 0.00000 C16 0.15237 -0.16703 0.71364 1.00000 0.02418 0.02323 0.02963 -0.00537 0.00535 -0.00072 0.02582 0.00521 0.00051 0.00017 0.00025 0.00000 0.00140 0.00138 0.00152 0.00109 0.00114 0.00109 0.00060 H16 0.13965 -0.22526 0.72643 1.00000 0.03098 0.00000 0.00000 C17 -0.11798 -0.14396 0.85452 1.00000 0.01894 0.01957 0.02538 -0.00089 0.00332 0.00122 0.02159 0.00503 0.00047 0.00016 0.00023 0.00000 0.00126 0.00124 0.00140 0.00106 0.00102 0.00104 0.00054 H17 -0.22983 -0.18837 0.81184 1.00000 0.02591 0.00000 0.00000 C18 -0.27768 -0.07993 0.89839 1.00000 0.01965 0.02226 0.02895 0.00033 0.00616 0.00155 0.02353 0.00528 0.00051 0.00017 0.00024 0.00000 0.00132 0.00135 0.00148 0.00108 0.00105 0.00107 0.00057 H18A -0.38917 -0.05307 0.83169 1.00000 0.02824 0.00000 0.00000 H18B -0.17126 -0.03763 0.94509 1.00000 0.02824 0.00000 0.00000 H18C -0.37542 -0.10787 0.94663 1.00000 0.02824 0.00000 0.00000 N19 0.04823 -0.18342 0.95997 1.00000 0.02195 0.02022 0.02380 0.00041 0.00610 0.00113 0.02186 0.00415 0.00040 0.00013 0.00018 0.00000 0.00119 0.00111 0.00122 0.00090 0.00093 0.00092 0.00049 H19A 0.14663 -0.22212 0.93662 1.00000 0.02623 0.00000 0.00000 H19B -0.04568 -0.20860 1.00397 1.00000 0.02623 0.00000 0.00000 H19C 0.14427 -0.14340 1.00312 1.00000 0.02623 0.00000 0.00000 C21 0.38424 0.26950 0.63169 1.00000 0.02569 0.01923 0.02243 0.00176 0.00918 -0.00083 0.02186 0.00533 0.00053 0.00016 0.00024 0.00000 0.00141 0.00125 0.00142 0.00098 0.00111 0.00104 0.00056 C22 0.31360 0.22694 0.52624 1.00000 0.03021 0.02853 0.02576 -0.00036 0.00395 0.00328 0.02858 0.00574 0.00056 0.00018 0.00026 0.00000 0.00160 0.00150 0.00154 0.00115 0.00122 0.00119 0.00064 H22 0.16420 0.24193 0.47259 1.00000 0.03429 0.00000 0.00000 C23 0.45819 0.16286 0.49817 1.00000 0.04127 0.02811 0.02375 -0.00504 0.00919 0.00162 0.03077 0.00593 0.00060 0.00018 0.00026 0.00000 0.00179 0.00165 0.00148 0.00112 0.00129 0.00124 0.00068 H23 0.40831 0.13444 0.42573 1.00000 0.03692 0.00000 0.00000 C24 0.67496 0.14073 0.57629 1.00000 0.03142 0.02621 0.03331 -0.00205 0.01103 0.00653 0.02974 0.00583 0.00056 0.00019 0.00026 0.00000 0.00164 0.00144 0.00167 0.00123 0.00129 0.00125 0.00065 H24 0.77506 0.09724 0.55719 1.00000 0.03568 0.00000 0.00000 C25 0.74622 0.18122 0.68120 1.00000 0.02628 0.02909 0.03223 -0.00215 0.00418 0.00703 0.02962 0.00572 0.00055 0.00018 0.00026 0.00000 0.00147 0.00145 0.00158 0.00129 0.00117 0.00127 0.00062 H25 0.89451 0.16532 0.73496 1.00000 0.03554 0.00000 0.00000 C26 0.60131 0.24583 0.70927 1.00000 0.02752 0.02584 0.02641 -0.00490 0.00549 0.00284 0.02671 0.00558 0.00053 0.00018 0.00025 0.00000 0.00154 0.00139 0.00149 0.00112 0.00116 0.00115 0.00060 H26 0.65188 0.27376 0.78206 1.00000 0.03205 0.00000 0.00000 C27 0.22659 0.34218 0.65300 1.00000 0.02359 0.02107 0.02193 0.00014 0.00772 0.00262 0.02180 0.00527 0.00051 0.00016 0.00023 0.00000 0.00135 0.00128 0.00141 0.00100 0.00108 0.00103 0.00056 H27 0.04861 0.32663 0.62370 1.00000 0.02616 0.00000 0.00000 C28 0.27699 0.42077 0.58914 1.00000 0.03569 0.02510 0.02504 0.00404 0.01093 0.00192 0.02797 0.00594 0.00058 0.00017 0.00025 0.00000 0.00162 0.00142 0.00147 0.00111 0.00117 0.00122 0.00061 H28A 0.25016 0.40893 0.50550 1.00000 0.03357 0.00000 0.00000 H28B 0.44865 0.43857 0.61963 1.00000 0.03357 0.00000 0.00000 H28C 0.16454 0.46531 0.60125 1.00000 0.03357 0.00000 0.00000 N29 0.26864 0.36312 0.77922 1.00000 0.02578 0.01885 0.02465 0.00212 0.01014 0.00226 0.02239 0.00437 0.00042 0.00013 0.00019 0.00000 0.00118 0.00108 0.00123 0.00089 0.00093 0.00093 0.00048 H29A 0.24046 0.31713 0.81961 1.00000 0.02686 0.00000 0.00000 H29B 0.16343 0.40467 0.78893 1.00000 0.02686 0.00000 0.00000 H29C 0.42774 0.38038 0.80627 1.00000 0.02686 0.00000 0.00000 Final Structure Factor Calculation for s92 in P2(1) Total number of l.s. parameters = 256 Maximum vector length = 511 Memory required = 3574 / 25046 wR2 = 0.0922 before cycle 5 for 2248 data and 2 / 256 parameters GooF = S = 1.048; Restrained GooF = 1.047 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0391 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0398 for 1972 Fo > 4sig(Fo) and 0.0520 for all 2248 data wR2 = 0.0922, GooF = S = 1.048, Restrained GooF = 1.047 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 28.00 for non-hydrogen and 28.00 for hydrogen atoms Principal mean square atomic displacements U 0.0349 0.0172 0.0151 C1 0.0253 0.0188 0.0173 C2 0.0249 0.0218 0.0173 C3 0.0320 0.0218 0.0163 C4 0.0537 0.0233 0.0163 O1A 0.0461 0.0270 0.0178 O1B 0.0320 0.0236 0.0218 O2 0.0379 0.0229 0.0188 O3 0.0519 0.0343 0.0188 O4A 0.0366 0.0272 0.0182 O4B 0.0267 0.0211 0.0162 C11 0.0274 0.0244 0.0193 C12 0.0306 0.0260 0.0236 C13 0.0382 0.0294 0.0210 C14 0.0426 0.0334 0.0178 C15 0.0330 0.0243 0.0202 C16 0.0267 0.0201 0.0180 C17 0.0290 0.0229 0.0187 C18 0.0241 0.0219 0.0196 N19 0.0273 0.0213 0.0169 C21 0.0342 0.0267 0.0248 C22 0.0415 0.0314 0.0194 C23 0.0363 0.0334 0.0195 C24 0.0385 0.0299 0.0204 C25 0.0332 0.0266 0.0202 C26 0.0259 0.0214 0.0182 C27 0.0369 0.0268 0.0202 C28 0.0295 0.0196 0.0181 N29 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.021 0.033 0.043 0.051 0.062 0.076 0.092 0.117 0.159 1.000 Number in group 230. 237. 231. 206. 225. 227. 225. 216. 225. 226. GooF 1.021 1.087 1.096 0.978 1.159 1.043 0.980 0.996 1.040 1.051 K 1.138 1.030 0.976 0.959 0.956 0.974 1.016 1.020 1.019 1.018 Resolution(A) 0.77 0.82 0.85 0.89 0.93 1.00 1.07 1.18 1.35 1.70 inf Number in group 227. 231. 219. 223. 225. 227. 227. 220. 224. 225. GooF 1.190 1.069 1.051 1.014 1.031 0.983 0.993 0.919 0.991 1.196 K 0.887 0.968 1.020 1.027 1.031 1.007 1.027 1.011 1.016 1.016 R1 0.189 0.119 0.082 0.062 0.053 0.043 0.034 0.029 0.027 0.027 Recommended weighting scheme: WGHT 0.0401 0.2297 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 0 2 16425.74 12777.48 4.88 1.000 3.54 3 0 6 254.01 124.47 4.27 0.099 1.18 5 1 2 26.65 47.47 3.62 0.061 1.02 -4 1 2 15.06 25.86 3.43 0.045 1.38 6 8 0 -0.84 8.30 3.40 0.025 0.82 0 3 3 205.18 246.85 3.32 0.139 3.11 5 0 8 -14.67 33.28 3.15 0.051 0.78 0 4 1 331.96 392.91 3.14 0.175 3.78 -3 3 3 116.81 91.96 3.14 0.085 1.70 -6 8 8 12.14 32.45 3.00 0.050 0.79 -2 14 11 31.94 53.58 2.91 0.065 0.78 1 6 5 61.78 46.86 2.87 0.061 1.58 -1 0 2 558.32 641.62 2.86 0.224 4.48 0 0 14 -9.74 19.13 2.86 0.039 0.82 -3 14 3 40.54 54.68 2.82 0.065 0.97 -5 7 6 25.87 40.95 2.78 0.057 0.95 -6 6 4 45.36 63.05 2.77 0.070 0.87 5 11 1 37.25 60.54 2.76 0.069 0.85 3 15 1 2.37 10.85 2.65 0.029 0.91 -3 14 7 55.06 41.06 2.64 0.057 0.88 -5 13 1 194.80 155.67 2.61 0.110 0.82 -2 0 2 98.57 119.76 2.60 0.097 2.70 2 10 9 161.02 132.80 2.60 0.102 0.88 -5 3 6 31.24 43.40 2.59 0.058 1.03 -5 11 4 207.09 165.03 2.59 0.114 0.88 3 15 0 49.42 62.88 2.55 0.070 0.92 -4 11 11 46.61 65.76 2.53 0.072 0.79 -6 4 4 -3.69 2.75 2.53 0.015 0.90 6 5 4 6.08 20.54 2.51 0.040 0.78 2 0 3 308.86 249.56 2.49 0.140 2.00 -3 11 6 4.93 0.32 2.49 0.005 1.04 0 7 2 315.91 357.64 2.48 0.167 2.13 4 5 7 24.99 36.16 2.47 0.053 0.90 -5 5 10 9.88 2.28 2.47 0.013 0.86 2 11 9 288.14 236.38 2.45 0.136 0.86 -3 12 1 233.22 200.58 2.44 0.125 1.08 6 0 0 17.92 5.95 2.43 0.022 0.90 -4 13 5 25.58 39.44 2.42 0.056 0.90 0 0 4 251.52 288.37 2.42 0.150 2.86 3 3 3 105.35 85.43 2.40 0.082 1.44 -1 10 3 177.53 204.04 2.40 0.126 1.46 0 18 0 8.07 2.57 2.40 0.014 0.89 4 11 5 22.41 14.42 2.39 0.034 0.86 2 9 8 12.33 6.81 2.38 0.023 0.97 2 3 0 171.15 196.89 2.38 0.124 2.41 1 0 11 37.45 65.89 2.37 0.072 0.98 1 3 0 1317.59 1468.56 2.36 0.339 3.80 -5 8 1 130.58 104.60 2.35 0.090 0.96 -2 18 6 35.74 51.14 2.34 0.063 0.79 -4 9 3 8.67 17.22 2.34 0.037 1.09 Bond lengths and angles C1 - Distance Angles O1B 1.2560 (0.0034) O1A 1.2568 (0.0034) 124.89 (0.25) C2 1.5262 (0.0036) 116.10 (0.23) 119.00 (0.25) C1 - O1B O1A C2 - Distance Angles O2 1.4087 (0.0033) C1 1.5262 (0.0036) 114.04 (0.22) C3 1.5287 (0.0036) 111.07 (0.21) 109.91 (0.22) H2 1.0000 107.16 107.16 107.16 C2 - O2 C1 C3 C3 - Distance Angles O3 1.4279 (0.0031) C4 1.5243 (0.0036) 110.33 (0.21) C2 1.5287 (0.0036) 108.93 (0.21) 110.30 (0.21) H3 1.0000 109.09 109.09 109.09 C3 - O3 C4 C2 C4 - Distance Angles O4A 1.2497 (0.0034) O4B 1.2656 (0.0032) 125.30 (0.25) C3 1.5243 (0.0036) 117.18 (0.24) 117.52 (0.22) C4 - O4A O4B O1A - Distance Angles C1 1.2568 (0.0034) O1A - O1B - Distance Angles C1 1.2560 (0.0034) O1B - O2 - Distance Angles C2 1.4087 (0.0033) H2O 0.8400 109.47 O2 - C2 O3 - Distance Angles C3 1.4279 (0.0031) H3O 0.8400 109.47 O3 - C3 O4A - Distance Angles C4 1.2497 (0.0034) O4A - O4B - Distance Angles C4 1.2656 (0.0032) O4B - C11 - Distance Angles C12 1.3873 (0.0038) C16 1.3944 (0.0037) 118.80 (0.25) C17 1.5167 (0.0037) 122.20 (0.23) 118.99 (0.24) C11 - C12 C16 C12 - Distance Angles C11 1.3873 (0.0038) C13 1.3960 (0.0038) 120.53 (0.25) H12 0.9500 119.74 119.74 C12 - C11 C13 C13 - Distance Angles C14 1.3787 (0.0039) C12 1.3960 (0.0037) 120.14 (0.27) H13 0.9500 119.93 119.93 C13 - C14 C12 C14 - Distance Angles C13 1.3787 (0.0039) C15 1.3835 (0.0044) 119.92 (0.26) H14 0.9500 120.04 120.04 C14 - C13 C15 C15 - Distance Angles C14 1.3835 (0.0044) C16 1.3913 (0.0040) 120.07 (0.26) H15 0.9500 119.97 119.97 C15 - C14 C16 C16 - Distance Angles C15 1.3913 (0.0040) C11 1.3944 (0.0037) 120.54 (0.26) H16 0.9500 119.73 119.73 C16 - C15 C11 C17 - Distance Angles N19 1.5044 (0.0033) C11 1.5167 (0.0037) 110.01 (0.20) C18 1.5222 (0.0036) 107.29 (0.21) 115.64 (0.22) H17 1.0000 107.88 107.88 107.88 C17 - N19 C11 C18 C18 - Distance Angles C17 1.5222 (0.0036) H18A 0.9800 109.47 H18B 0.9800 109.47 109.47 H18C 0.9800 109.47 109.47 109.47 C18 - C17 H18A H18B N19 - Distance Angles C17 1.5044 (0.0033) H19A 0.9100 109.47 H19B 0.9100 109.47 109.47 H19C 0.9100 109.47 109.47 109.47 N19 - C17 H19A H19B C21 - Distance Angles C26 1.3862 (0.0041) C22 1.3912 (0.0040) 118.48 (0.25) C27 1.5121 (0.0036) 123.35 (0.24) 118.09 (0.26) C21 - C26 C22 C22 - Distance Angles C23 1.3894 (0.0040) C21 1.3912 (0.0040) 121.01 (0.28) H22 0.9500 119.49 119.49 C22 - C23 C21 C23 - Distance Angles C24 1.3815 (0.0044) C22 1.3894 (0.0040) 119.58 (0.27) H23 0.9500 120.21 120.21 C23 - C24 C22 C24 - Distance Angles C25 1.3703 (0.0042) C23 1.3815 (0.0044) 120.29 (0.27) H24 0.9500 119.86 119.86 C24 - C25 C23 C25 - Distance Angles C24 1.3703 (0.0042) C26 1.3967 (0.0039) 120.14 (0.27) H25 0.9500 119.93 119.93 C25 - C24 C26 C26 - Distance Angles C21 1.3862 (0.0041) C25 1.3967 (0.0039) 120.49 (0.26) H26 0.9500 119.75 119.75 C26 - C21 C25 C27 - Distance Angles N29 1.4886 (0.0035) C21 1.5121 (0.0036) 112.09 (0.22) C28 1.5251 (0.0037) 107.59 (0.22) 111.98 (0.21) H27 1.0000 108.35 108.35 108.35 C27 - N29 C21 C28 C28 - Distance Angles C27 1.5251 (0.0037) H28A 0.9800 109.47 H28B 0.9800 109.47 109.47 H28C 0.9800 109.47 109.47 109.47 C28 - C27 H28A H28B N29 - Distance Angles C27 1.4886 (0.0035) H29A 0.9100 109.47 H29B 0.9100 109.47 109.47 H29C 0.9100 109.47 109.47 109.47 N29 - C27 H29A H29B Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 2.44 2.853(3) 111.0 O2-H2O...O3 0.84 2.09 2.602(3) 118.6 O3-H3O...O4A 0.84 2.06 2.872(3) 162.2 O2-H2O...O1B_$1 0.91 1.87 2.734(3) 157.6 N19-H19A...O1B_$2 0.91 1.89 2.760(3) 160.0 N19-H19B...O1A_$3 0.91 1.93 2.817(3) 162.8 N19-H19C...O4B_$4 0.91 1.94 2.775(3) 151.8 N29-H29A...O1A_$4 0.91 1.81 2.708(3) 168.4 N29-H29B...O4A_$5 0.91 1.85 2.741(3) 167.0 N29-H29C...O4B_$6 FMAP and GRID set by program FMAP 2 1 28 GRID -4.000 -1 -2 4.000 1 2 R1 = 0.0520 for 2248 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.21 at 0.3884 0.1382 0.0208 [ 0.78 A from C2 ] Deepest hole -0.28 at 0.8472 0.3525 0.0598 [ 0.76 A from H19C ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 3707 / 35755 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3884 0.1382 0.0208 1.00000 0.05 0.21 0.78 C2 0.78 C1 1.37 H2 1.63 O1B Q2 1 0.2941 0.2507 0.0358 1.00000 0.05 0.20 1.02 O1A 1.43 C1 1.50 H19B 2.14 H17 Q3 1 -0.0292 0.3989 0.7576 1.00000 0.05 0.20 1.05 H29B 1.67 O4A 1.71 N29 2.00 H29A Q4 1 -0.0069 0.0342 0.8188 1.00000 0.05 0.19 0.43 H12 1.33 C12 1.98 O2 2.24 H18B Q5 1 0.3647 0.1016 0.5746 1.00000 0.05 0.19 1.50 C23 1.64 H13 1.83 C24 1.90 H23 Q6 1 0.1217 -0.1382 0.1853 1.00000 0.05 0.18 1.73 O4B 1.81 H29B 1.87 H26 2.12 H29A Q7 1 -0.2547 0.0491 1.0045 1.00000 0.05 0.18 1.67 H18B 1.75 H2O 2.05 H2 2.05 O2 Q8 1 0.3106 0.0789 0.6464 1.00000 0.05 0.18 0.70 H13 1.46 C13 2.16 C14 2.18 H14 Q9 1 -0.1587 0.3598 0.6649 1.00000 0.05 0.17 1.45 H27 2.15 H29B 2.19 C27 2.36 H26 Q10 1 0.0114 -0.0713 0.7391 1.00000 0.05 0.16 0.74 C11 0.78 C12 1.53 H12 1.78 C16 Shortest distances between peaks (including symmetry equivalents) 5 8 1.03 3 6 1.11 3 9 1.32 6 9 1.73 1 2 1.90 4 10 1.95 1 7 2.48 4 7 2.85 Time profile in seconds ----------------------- 0.08: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: 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. 0.38: 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 0.72: Structure factors and derivatives 0.92: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.20: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.08: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 10:04:20 Total CPU time: 2.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++