+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008src0504 started at 11:34:52 on 04-Jun-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src0504 in P2(1)/c CELL 0.71073 13.9991 18.4241 11.2873 90.000 99.134 90.000 ZERR 4.00 0.0002 0.0002 0.0001 0.000 0.001 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H O S P UNIT 108 140 41 8 4 V = 2874.31 F(000) = 1304.0 Mu = 0.30 mm-1 Cell Wt = 2474.56 Rho = 1.430 MERG 2 OMIT -3.00 55.00 OMIT 3 1 2 OMIT -1 0 2 OMIT 1 2 1 OMIT -1 2 1 OMIT -1 1 2 OMIT 2 0 0 OMIT -4 6 4 FMAP 2 PLAN 40 SIZE 0.03 0.05 0.40 ACTA BOND WGHT 0.03730 1.85570 L.S. 4 TEMP -153.00 FVAR 0.49075 0.16660 C1 1 0.330382 0.036387 0.666653 11.00000 0.01732 0.01490 = 0.01362 -0.00088 0.00145 0.00206 AFIX 23 H1A 2 0.387218 0.067687 0.662384 11.00000 -1.20000 H1B 2 0.354192 -0.011835 0.696783 11.00000 -1.20000 AFIX 0 C2 1 0.271174 0.028278 0.541304 11.00000 0.01838 0.01925 = 0.01355 -0.00252 0.00090 0.00274 AFIX 23 H2A 2 0.224889 -0.012293 0.541943 11.00000 -1.20000 H2B 2 0.233304 0.073180 0.520786 11.00000 -1.20000 AFIX 0 C3 1 0.333806 0.013961 0.445371 11.00000 0.02565 0.01755 = 0.01582 -0.00146 0.00598 -0.00053 AFIX 23 H3A 2 0.375487 0.056929 0.440583 11.00000 -1.20000 H3B 2 0.290793 0.009511 0.367146 11.00000 -1.20000 AFIX 0 C4 1 0.142315 0.030693 0.732248 11.00000 0.01839 0.01672 = 0.01261 -0.00076 0.00280 -0.00282 C5 1 0.142973 -0.045133 0.749095 11.00000 0.02802 0.01708 = 0.01401 -0.00102 0.00587 -0.00276 C6 1 0.235899 -0.148194 0.829782 11.00000 0.06344 0.01290 = 0.04049 0.00505 -0.00747 -0.00228 AFIX 137 H6A 2 0.194904 -0.156986 0.891083 11.00000 -1.50000 H6B 2 0.303100 -0.160418 0.862210 11.00000 -1.50000 H6C 2 0.213764 -0.178458 0.759370 11.00000 -1.50000 AFIX 0 C7 1 0.059167 -0.085687 0.718130 11.00000 0.03964 0.02000 = 0.02562 -0.00313 0.00835 -0.01302 AFIX 43 H7 2 0.059566 -0.136673 0.730763 11.00000 -1.20000 AFIX 0 C8 1 -0.024826 -0.050446 0.668582 11.00000 0.02984 0.03173 = 0.03023 -0.00592 0.00618 -0.01750 AFIX 43 H8 2 -0.082431 -0.077966 0.647744 11.00000 -1.20000 AFIX 0 C9 1 -0.027746 0.023385 0.648398 11.00000 0.01959 0.03388 = 0.02261 -0.00109 0.00321 -0.00735 AFIX 43 H9 2 -0.086579 0.046235 0.614396 11.00000 -1.20000 AFIX 0 C10 1 0.056371 0.064106 0.678341 11.00000 0.02061 0.02059 = 0.01441 0.00084 0.00438 -0.00424 C11 1 -0.030559 0.173647 0.623211 11.00000 0.01582 0.03251 = 0.04121 0.01446 0.00335 0.00432 AFIX 137 H11A 2 -0.060166 0.160066 0.541669 11.00000 -1.50000 H11B 2 -0.019079 0.226130 0.626845 11.00000 -1.50000 H11C 2 -0.074080 0.160396 0.679683 11.00000 -1.50000 AFIX 0 C12 1 0.246304 0.173192 0.755752 11.00000 0.01427 0.01178 = 0.01762 0.00035 -0.00096 0.00032 C13 1 0.190343 0.206415 0.833375 11.00000 0.01654 0.01731 = 0.01738 0.00023 -0.00007 0.00102 C14 1 0.078319 0.185760 0.969267 11.00000 0.02289 0.03110 = 0.02824 -0.00207 0.01026 0.00390 AFIX 137 H14A 2 0.107553 0.222828 1.025973 11.00000 -1.50000 H14B 2 0.054388 0.145675 1.013527 11.00000 -1.50000 H14C 2 0.024376 0.207106 0.914362 11.00000 -1.50000 AFIX 0 C15 1 0.180721 0.281169 0.837730 11.00000 0.02410 0.01732 = 0.02793 -0.00401 0.00399 0.00378 AFIX 43 H15 2 0.141432 0.303108 0.889044 11.00000 -1.20000 AFIX 0 C16 1 0.229954 0.323063 0.765219 11.00000 0.02799 0.01194 = 0.03579 -0.00163 0.00133 0.00039 AFIX 43 H16 2 0.224788 0.374411 0.768536 11.00000 -1.20000 AFIX 0 C17 1 0.286086 0.292766 0.688559 11.00000 0.02225 0.01631 = 0.02940 0.00350 0.00190 -0.00263 AFIX 43 H17 2 0.319426 0.322940 0.640430 11.00000 -1.20000 AFIX 0 C18 1 0.293683 0.217378 0.682026 11.00000 0.01433 0.01570 = 0.01904 0.00066 -0.00058 0.00032 C19 1 0.403009 0.226498 0.540392 11.00000 0.02181 0.02386 = 0.02846 0.00804 0.00761 -0.00233 AFIX 137 H19A 2 0.361844 0.259212 0.485963 11.00000 -1.50000 H19B 2 0.439178 0.194727 0.493781 11.00000 -1.50000 H19C 2 0.448448 0.255116 0.596881 11.00000 -1.50000 AFIX 0 C20 1 0.317795 0.061269 0.921525 11.00000 0.01945 0.01388 = 0.01306 -0.00151 0.00000 0.00471 C21 1 0.413309 0.087661 0.948660 11.00000 0.02118 0.01574 = 0.01700 -0.00395 0.00136 0.00598 C22 1 0.540358 0.154947 0.877187 11.00000 0.01690 0.02702 = 0.03001 -0.00690 0.00207 -0.00118 AFIX 137 H22A 2 0.542762 0.192239 0.939501 11.00000 -1.50000 H22B 2 0.553561 0.177213 0.802611 11.00000 -1.50000 H22C 2 0.589128 0.117670 0.903204 11.00000 -1.50000 AFIX 0 C23 1 0.467165 0.078267 1.062499 11.00000 0.02259 0.02414 = 0.02105 -0.00663 -0.00340 0.00734 AFIX 43 H23 2 0.530925 0.097158 1.081163 11.00000 -1.20000 AFIX 0 C24 1 0.425875 0.040918 1.147578 11.00000 0.03268 0.02675 = 0.01356 -0.00399 -0.00388 0.01184 AFIX 43 H24 2 0.463136 0.032678 1.224348 11.00000 -1.20000 AFIX 0 C25 1 0.332141 0.015164 1.124609 11.00000 0.03558 0.02077 = 0.01307 0.00080 0.00449 0.01071 AFIX 43 H25 2 0.305803 -0.010708 1.184694 11.00000 -1.20000 AFIX 0 C26 1 0.276339 0.027397 1.012512 11.00000 0.02599 0.01397 = 0.01492 -0.00205 0.00299 0.00535 C27 1 0.138553 -0.028349 1.074490 11.00000 0.03916 0.03454 = 0.02831 0.01173 0.00844 -0.00704 AFIX 137 H27A 2 0.173953 -0.073520 1.096383 11.00000 -1.50000 H27B 2 0.071106 -0.039629 1.041767 11.00000 -1.50000 H27C 2 0.140661 0.002258 1.145868 11.00000 -1.50000 AFIX 0 O1 3 0.250728 -0.152689 0.513951 11.00000 0.02804 0.03188 = 0.02546 0.00201 0.00944 -0.00881 O2 3 0.252099 -0.125564 0.305318 11.00000 0.02858 0.02581 = 0.02166 0.00235 -0.00481 -0.00512 O3 3 0.369095 -0.210470 0.409385 11.00000 0.02433 0.01744 = 0.04854 -0.00542 0.00173 0.00115 O4 3 0.229945 -0.073218 0.795694 11.00000 0.03354 0.01178 = 0.02533 0.00172 0.00439 0.00180 O5 3 0.059632 0.136121 0.654571 11.00000 0.01413 0.02126 = 0.02887 0.00811 -0.00047 -0.00085 O6 3 0.149242 0.159037 0.902103 11.00000 0.02380 0.01836 = 0.02183 0.00050 0.00903 0.00343 O7 3 0.344004 0.183371 0.605390 11.00000 0.02427 0.01717 = 0.02504 0.00382 0.01067 -0.00123 O8 3 0.446167 0.122349 0.857059 11.00000 0.01744 0.02531 = 0.01938 -0.00097 0.00006 -0.00173 O9 3 0.181968 0.009127 0.986691 11.00000 0.02646 0.02540 = 0.01595 0.00451 0.00512 -0.00129 O10 3 0.166856 -0.281799 0.603739 11.00000 0.03976 0.03107 = 0.03381 0.00814 -0.00499 -0.01167 S1 4 0.410608 -0.065680 0.465924 11.00000 0.01535 0.01973 = 0.02808 -0.00611 0.00479 -0.00194 S2 4 0.308165 -0.148342 0.418301 11.00000 0.01607 0.01650 = 0.01917 0.00039 0.00111 -0.00167 P1 5 0.257661 0.076016 0.769567 11.00000 0.01456 0.01157 = 0.01170 0.00034 0.00094 0.00067 O11 3 0.411989 -0.180152 0.732300 10.16660 0.04163 0.05233 = 0.03391 0.00358 -0.00179 -0.00503 H10A 2 0.202445 -0.247762 0.579024 11.00000 0.05917 H10B 2 0.203840 -0.303614 0.657501 11.00000 0.06550 HKLF 4 1.0 0.00 0.00 1.00 0.00 -1.00 0.00 1.00 0.00 0.00 Covalent radii and connectivity table for 2008src0504 in P2(1)/c C 0.770 H 0.320 O 0.660 S 1.030 P 1.100 C1 - C2 P1 C2 - C3 C1 C3 - C2 S1 C4 - C10 C5 P1 C5 - O4 C7 C4 C6 - O4 C7 - C8 C5 C8 - C9 C7 C9 - C8 C10 C10 - O5 C9 C4 C11 - O5 C12 - C18 C13 P1 C13 - O6 C15 C12 C14 - O6 C15 - C13 C16 C16 - C17 C15 C17 - C16 C18 C18 - O7 C17 C12 C19 - O7 C20 - C26 C21 P1 C21 - O8 C23 C20 C22 - O8 C23 - C24 C21 C24 - C23 C25 C25 - C24 C26 C26 - O9 C25 C20 C27 - O9 O1 - S2 O2 - S2 O3 - S2 O4 - C5 C6 O5 - C10 C11 O6 - C13 C14 O7 - C18 C19 O8 - C21 C22 O9 - C26 C27 O10 - no bonds found S1 - C3 S2 S2 - O3 O1 O2 S1 P1 - C12 C20 C4 C1 O11 - no bonds found 59820 Reflections read, of which 1095 rejected -18 =< h =< 18, -23 =< k =< 23, -14 =< l =< 14, Max. 2-theta = 54.99 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -5 13 9 0.30 0.08 8 3.85 1 Inconsistent equivalents 6575 Unique reflections, of which 0 suppressed R(int) = 0.0538 R(sigma) = 0.0314 Friedel opposites merged Maximum memory for data reduction = 3387 / 64965 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. ** Cell contents from UNIT instruction and atom list do not agree ** Unit-cell contents from UNIT instruction and atom list resp. C 108.00 108.00 H 140.00 140.00 O 41.00 40.67 S 8.00 8.00 P 4.00 4.00 Least-squares cycle 1 Maximum vector length = 511 Memory required = 4453 / 492562 wR2 = 0.0894 before cycle 1 for 6575 data and 385 / 385 parameters GooF = S = 1.034; Restrained GooF = 1.034 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0373 * P )^2 + 1.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.49080 0.00058 0.079 OSF 2 0.16660 9.99999 0.000 FVAR 2 Mean shift/esd = 0.008 Maximum = 0.079 for OSF Max. shift = 0.000 A for H10A Max. dU = 0.000 for H10A Least-squares cycle 2 Maximum vector length = 511 Memory required = 4453 / 492562 wR2 = 0.0894 before cycle 2 for 6575 data and 385 / 385 parameters GooF = S = 1.034; Restrained GooF = 1.034 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0373 * P )^2 + 1.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.49081 0.00058 0.029 OSF 2 0.16660 9.99999 0.000 FVAR 2 Mean shift/esd = 0.003 Maximum = 0.029 for OSF Max. shift = 0.000 A for H10A Max. dU = 0.000 for H10A Least-squares cycle 3 Maximum vector length = 511 Memory required = 4453 / 492562 wR2 = 0.0894 before cycle 3 for 6575 data and 385 / 385 parameters GooF = S = 1.034; Restrained GooF = 1.034 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0373 * P )^2 + 1.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.49081 0.00058 0.000 OSF 2 0.16660 9.99999 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = -0.001 for U11 H10A Max. shift = 0.000 A for H10A Max. dU = 0.000 for H10A Least-squares cycle 4 Maximum vector length = 511 Memory required = 4453 / 492562 wR2 = 0.0894 before cycle 4 for 6575 data and 385 / 385 parameters GooF = S = 1.034; Restrained GooF = 1.034 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0373 * P )^2 + 1.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.49081 0.00058 0.000 OSF 2 0.16660 9.99999 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for z P1 Max. shift = 0.000 A for H10A Max. dU = 0.000 for H10A No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.3872 0.0677 0.6624 23 0.990 0.000 C1 C2 P1 H1B 0.3542 -0.0118 0.6968 23 0.990 0.000 C1 C2 P1 H2A 0.2249 -0.0123 0.5419 23 0.990 0.000 C2 C3 C1 H2B 0.2333 0.0732 0.5208 23 0.990 0.000 C2 C3 C1 H3A 0.3755 0.0569 0.4406 23 0.990 0.000 C3 C2 S1 H3B 0.2908 0.0095 0.3671 23 0.990 0.000 C3 C2 S1 H6A 0.1949 -0.1570 0.8911 137 0.980 0.000 C6 O4 H6A H6B 0.3031 -0.1604 0.8622 137 0.980 0.000 C6 O4 H6A H6C 0.2138 -0.1785 0.7594 137 0.980 0.000 C6 O4 H6A H7 0.0596 -0.1367 0.7308 43 0.950 0.000 C7 C8 C5 H8 -0.0824 -0.0780 0.6477 43 0.950 0.000 C8 C9 C7 H9 -0.0866 0.0462 0.6144 43 0.950 0.000 C9 C8 C10 H11A -0.0602 0.1601 0.5417 137 0.980 0.000 C11 O5 H11A H11B -0.0191 0.2261 0.6269 137 0.980 0.000 C11 O5 H11A H11C -0.0741 0.1604 0.6797 137 0.980 0.000 C11 O5 H11A H14A 0.1076 0.2228 1.0260 137 0.980 0.000 C14 O6 H14A H14B 0.0544 0.1457 1.0135 137 0.980 0.000 C14 O6 H14A H14C 0.0244 0.2071 0.9144 137 0.980 0.000 C14 O6 H14A H15 0.1414 0.3031 0.8890 43 0.950 0.000 C15 C13 C16 H16 0.2248 0.3744 0.7685 43 0.950 0.000 C16 C17 C15 H17 0.3194 0.3229 0.6404 43 0.950 0.000 C17 C16 C18 H19A 0.3618 0.2592 0.4860 137 0.980 0.000 C19 O7 H19A H19B 0.4392 0.1947 0.4938 137 0.980 0.000 C19 O7 H19A H19C 0.4485 0.2551 0.5969 137 0.980 0.000 C19 O7 H19A H22A 0.5428 0.1922 0.9395 137 0.980 0.000 C22 O8 H22A H22B 0.5536 0.1772 0.8026 137 0.980 0.000 C22 O8 H22A H22C 0.5891 0.1177 0.9032 137 0.980 0.000 C22 O8 H22A H23 0.5309 0.0972 1.0812 43 0.950 0.000 C23 C24 C21 H24 0.4631 0.0327 1.2243 43 0.950 0.000 C24 C23 C25 H25 0.3058 -0.0107 1.1847 43 0.950 0.000 C25 C24 C26 H27A 0.1740 -0.0735 1.0964 137 0.980 0.000 C27 O9 H27A H27B 0.0711 -0.0396 1.0418 137 0.980 0.000 C27 O9 H27A H27C 0.1407 0.0023 1.1459 137 0.980 0.000 C27 O9 H27A 2008src0504 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.33038 0.03639 0.66665 1.00000 0.01732 0.01491 0.01363 -0.00087 0.00146 0.00206 0.01540 0.00271 0.00011 0.00008 0.00013 0.00000 0.00075 0.00073 0.00068 0.00055 0.00056 0.00058 0.00030 H1A 0.38722 0.06769 0.66238 1.00000 0.01848 0.00000 0.00000 H1B 0.35419 -0.01183 0.69678 1.00000 0.01848 0.00000 0.00000 C2 0.27117 0.02828 0.54131 1.00000 0.01838 0.01926 0.01357 -0.00252 0.00091 0.00274 0.01725 0.00280 0.00011 0.00009 0.00013 0.00000 0.00077 0.00077 0.00068 0.00058 0.00057 0.00060 0.00031 H2A 0.22489 -0.01229 0.54194 1.00000 0.02070 0.00000 0.00000 H2B 0.23330 0.07318 0.52079 1.00000 0.02070 0.00000 0.00000 C3 0.33381 0.01396 0.44537 1.00000 0.02566 0.01756 0.01583 -0.00146 0.00598 -0.00054 0.01939 0.00298 0.00012 0.00009 0.00014 0.00000 0.00084 0.00077 0.00072 0.00059 0.00061 0.00064 0.00032 H3A 0.37549 0.05693 0.44058 1.00000 0.02327 0.00000 0.00000 H3B 0.29079 0.00951 0.36715 1.00000 0.02327 0.00000 0.00000 C4 0.14231 0.03069 0.73225 1.00000 0.01840 0.01674 0.01261 -0.00076 0.00280 -0.00282 0.01588 0.00271 0.00011 0.00008 0.00013 0.00000 0.00076 0.00074 0.00066 0.00056 0.00056 0.00059 0.00030 C5 0.14297 -0.04513 0.74909 1.00000 0.02803 0.01710 0.01401 -0.00103 0.00588 -0.00277 0.01944 0.00291 0.00012 0.00009 0.00013 0.00000 0.00087 0.00076 0.00070 0.00058 0.00062 0.00064 0.00032 C6 0.23590 -0.14819 0.82978 1.00000 0.06345 0.01291 0.04050 0.00506 -0.00746 -0.00229 0.04066 0.00378 0.00018 0.00010 0.00019 0.00000 0.00145 0.00085 0.00112 0.00078 0.00100 0.00087 0.00052 H6A 0.19491 -0.15699 0.89108 1.00000 0.06099 0.00000 0.00000 H6B 0.30310 -0.16042 0.86221 1.00000 0.06099 0.00000 0.00000 H6C 0.21377 -0.17846 0.75937 1.00000 0.06099 0.00000 0.00000 C7 0.05917 -0.08569 0.71813 1.00000 0.03966 0.02001 0.02562 -0.00313 0.00835 -0.01304 0.02809 0.00317 0.00014 0.00010 0.00015 0.00000 0.00106 0.00084 0.00087 0.00068 0.00076 0.00075 0.00039 H7 0.05957 -0.13667 0.73076 1.00000 0.03371 0.00000 0.00000 C8 -0.02482 -0.05045 0.66858 1.00000 0.02984 0.03175 0.03024 -0.00591 0.00619 -0.01750 0.03045 0.00321 0.00014 0.00010 0.00016 0.00000 0.00098 0.00098 0.00093 0.00077 0.00074 0.00080 0.00041 H8 -0.08243 -0.07797 0.64775 1.00000 0.03654 0.00000 0.00000 C9 -0.02775 0.02339 0.64840 1.00000 0.01960 0.03389 0.02262 -0.00108 0.00321 -0.00735 0.02538 0.00308 0.00012 0.00010 0.00015 0.00000 0.00084 0.00096 0.00081 0.00071 0.00064 0.00071 0.00036 H9 -0.08658 0.04624 0.61439 1.00000 0.03046 0.00000 0.00000 C10 0.05637 0.06410 0.67834 1.00000 0.02062 0.02060 0.01441 0.00084 0.00439 -0.00424 0.01837 0.00283 0.00011 0.00009 0.00013 0.00000 0.00080 0.00079 0.00070 0.00059 0.00058 0.00062 0.00032 C11 -0.03056 0.17365 0.62321 1.00000 0.01584 0.03253 0.04122 0.01446 0.00336 0.00432 0.02999 0.00366 0.00012 0.00010 0.00018 0.00000 0.00083 0.00099 0.00105 0.00082 0.00073 0.00071 0.00041 H11A -0.06016 0.16007 0.54166 1.00000 0.04499 0.00000 0.00000 H11B -0.01908 0.22613 0.62686 1.00000 0.04499 0.00000 0.00000 H11C -0.07408 0.16039 0.67968 1.00000 0.04499 0.00000 0.00000 C12 0.24630 0.17319 0.75575 1.00000 0.01429 0.01180 0.01763 0.00035 -0.00096 0.00032 0.01495 0.00266 0.00010 0.00008 0.00013 0.00000 0.00073 0.00069 0.00071 0.00055 0.00056 0.00055 0.00030 C13 0.19034 0.20642 0.83337 1.00000 0.01656 0.01733 0.01738 0.00022 -0.00007 0.00102 0.01739 0.00279 0.00011 0.00008 0.00013 0.00000 0.00074 0.00077 0.00073 0.00059 0.00058 0.00059 0.00031 C14 0.07832 0.18576 0.96926 1.00000 0.02290 0.03112 0.02825 -0.00207 0.01026 0.00390 0.02675 0.00342 0.00013 0.00010 0.00016 0.00000 0.00088 0.00095 0.00089 0.00073 0.00070 0.00072 0.00037 H14A 0.10755 0.22282 1.02598 1.00000 0.04012 0.00000 0.00000 H14B 0.05438 0.14567 1.01351 1.00000 0.04012 0.00000 0.00000 H14C 0.02438 0.20711 0.91436 1.00000 0.04012 0.00000 0.00000 C15 0.18072 0.28117 0.83773 1.00000 0.02411 0.01733 0.02794 -0.00402 0.00399 0.00378 0.02314 0.00307 0.00012 0.00009 0.00015 0.00000 0.00085 0.00079 0.00086 0.00065 0.00068 0.00066 0.00035 H15 0.14143 0.30311 0.88905 1.00000 0.02777 0.00000 0.00000 C16 0.22995 0.32306 0.76522 1.00000 0.02800 0.01196 0.03580 -0.00163 0.00133 0.00039 0.02566 0.00314 0.00013 0.00009 0.00016 0.00000 0.00091 0.00075 0.00096 0.00067 0.00073 0.00066 0.00037 H16 0.22479 0.37441 0.76853 1.00000 0.03079 0.00000 0.00000 C17 0.28609 0.29277 0.68856 1.00000 0.02226 0.01632 0.02941 0.00350 0.00189 -0.00264 0.02290 0.00302 0.00012 0.00009 0.00015 0.00000 0.00084 0.00080 0.00087 0.00066 0.00067 0.00064 0.00035 H17 0.31943 0.32294 0.64043 1.00000 0.02748 0.00000 0.00000 C18 0.29368 0.21738 0.68202 1.00000 0.01434 0.01571 0.01905 0.00066 -0.00059 0.00032 0.01672 0.00275 0.00011 0.00008 0.00014 0.00000 0.00073 0.00073 0.00073 0.00058 0.00058 0.00057 0.00031 C19 0.40301 0.22650 0.54039 1.00000 0.02183 0.02387 0.02846 0.00803 0.00761 -0.00233 0.02433 0.00329 0.00012 0.00009 0.00016 0.00000 0.00084 0.00086 0.00087 0.00070 0.00068 0.00068 0.00036 H19A 0.36184 0.25922 0.48598 1.00000 0.03649 0.00000 0.00000 H19B 0.43917 0.19473 0.49377 1.00000 0.03649 0.00000 0.00000 H19C 0.44846 0.25511 0.59688 1.00000 0.03649 0.00000 0.00000 C20 0.31779 0.06127 0.92153 1.00000 0.01946 0.01389 0.01306 -0.00151 0.00000 0.00472 0.01575 0.00273 0.00011 0.00008 0.00013 0.00000 0.00077 0.00072 0.00068 0.00054 0.00056 0.00057 0.00030 C21 0.41331 0.08766 0.94866 1.00000 0.02120 0.01575 0.01702 -0.00395 0.00136 0.00597 0.01817 0.00286 0.00011 0.00008 0.00014 0.00000 0.00080 0.00074 0.00072 0.00058 0.00060 0.00060 0.00032 C22 0.54036 0.15495 0.87719 1.00000 0.01691 0.02703 0.03001 -0.00691 0.00207 -0.00118 0.02483 0.00304 0.00012 0.00010 0.00016 0.00000 0.00081 0.00089 0.00089 0.00071 0.00066 0.00067 0.00036 H22A 0.54276 0.19224 0.93950 1.00000 0.03725 0.00000 0.00000 H22B 0.55356 0.17721 0.80261 1.00000 0.03725 0.00000 0.00000 H22C 0.58913 0.11767 0.90320 1.00000 0.03725 0.00000 0.00000 C23 0.46717 0.07827 1.06250 1.00000 0.02260 0.02415 0.02107 -0.00663 -0.00340 0.00734 0.02335 0.00306 0.00013 0.00009 0.00015 0.00000 0.00084 0.00086 0.00079 0.00066 0.00064 0.00067 0.00035 H23 0.53093 0.09716 1.08116 1.00000 0.02802 0.00000 0.00000 C24 0.42587 0.04092 1.14758 1.00000 0.03269 0.02675 0.01357 -0.00399 -0.00388 0.01183 0.02516 0.00315 0.00013 0.00010 0.00014 0.00000 0.00097 0.00090 0.00072 0.00064 0.00065 0.00073 0.00037 H24 0.46313 0.03268 1.22435 1.00000 0.03019 0.00000 0.00000 C25 0.33214 0.01516 1.12461 1.00000 0.03559 0.02079 0.01308 0.00081 0.00450 0.01071 0.02309 0.00317 0.00013 0.00009 0.00014 0.00000 0.00099 0.00082 0.00072 0.00061 0.00066 0.00070 0.00036 H25 0.30580 -0.01071 1.18469 1.00000 0.02770 0.00000 0.00000 C26 0.27634 0.02740 1.01251 1.00000 0.02600 0.01398 0.01494 -0.00205 0.00298 0.00535 0.01833 0.00290 0.00012 0.00008 0.00013 0.00000 0.00085 0.00072 0.00070 0.00058 0.00060 0.00062 0.00032 C27 0.13856 -0.02835 1.07449 1.00000 0.03918 0.03454 0.02833 0.01172 0.00844 -0.00704 0.03368 0.00375 0.00015 0.00011 0.00017 0.00000 0.00111 0.00105 0.00093 0.00080 0.00080 0.00085 0.00044 H27A 0.17396 -0.07352 1.09639 1.00000 0.05052 0.00000 0.00000 H27B 0.07111 -0.03964 1.04176 1.00000 0.05052 0.00000 0.00000 H27C 0.14065 0.00226 1.14586 1.00000 0.05052 0.00000 0.00000 O1 0.25073 -0.15269 0.51395 1.00000 0.02805 0.03189 0.02547 0.00201 0.00944 -0.00881 0.02790 0.00225 0.00009 0.00007 0.00011 0.00000 0.00067 0.00069 0.00062 0.00052 0.00051 0.00053 0.00028 O2 0.25210 -0.12556 0.30532 1.00000 0.02859 0.02582 0.02167 0.00235 -0.00481 -0.00512 0.02631 0.00212 0.00009 0.00007 0.00010 0.00000 0.00067 0.00063 0.00059 0.00049 0.00049 0.00051 0.00027 O3 0.36910 -0.21047 0.40939 1.00000 0.02434 0.01745 0.04856 -0.00543 0.00174 0.00114 0.03056 0.00228 0.00009 0.00007 0.00012 0.00000 0.00065 0.00060 0.00080 0.00055 0.00056 0.00049 0.00029 O4 0.22994 -0.07322 0.79569 1.00000 0.03355 0.01179 0.02534 0.00173 0.00440 0.00180 0.02359 0.00216 0.00009 0.00006 0.00010 0.00000 0.00067 0.00054 0.00060 0.00044 0.00050 0.00047 0.00026 O5 0.05963 0.13612 0.65457 1.00000 0.01414 0.02127 0.02888 0.00811 -0.00047 -0.00085 0.02185 0.00210 0.00008 0.00006 0.00010 0.00000 0.00055 0.00059 0.00061 0.00047 0.00045 0.00044 0.00025 O6 0.14924 0.15904 0.90210 1.00000 0.02381 0.01837 0.02184 0.00050 0.00903 0.00343 0.02075 0.00212 0.00008 0.00006 0.00010 0.00000 0.00060 0.00056 0.00056 0.00044 0.00046 0.00046 0.00024 O7 0.34401 0.18337 0.60539 1.00000 0.02428 0.01719 0.02505 0.00382 0.01067 -0.00123 0.02144 0.00213 0.00008 0.00006 0.00010 0.00000 0.00061 0.00056 0.00059 0.00046 0.00047 0.00046 0.00025 O8 0.44617 0.12235 0.85706 1.00000 0.01746 0.02532 0.01940 -0.00097 0.00006 -0.00173 0.02104 0.00201 0.00008 0.00006 0.00010 0.00000 0.00057 0.00061 0.00055 0.00046 0.00043 0.00046 0.00024 O9 0.18197 0.00913 0.98669 1.00000 0.02647 0.02542 0.01596 0.00451 0.00512 -0.00129 0.02243 0.00212 0.00008 0.00006 0.00010 0.00000 0.00063 0.00062 0.00054 0.00046 0.00045 0.00049 0.00025 O10 0.16686 -0.28180 0.60374 1.00000 0.03977 0.03107 0.03382 0.00814 -0.00498 -0.01167 0.03606 0.00254 0.00011 0.00008 0.00013 0.00000 0.00082 0.00076 0.00075 0.00061 0.00064 0.00065 0.00033 S1 0.41061 -0.06568 0.46592 1.00000 0.01536 0.01974 0.02808 -0.00611 0.00479 -0.00194 0.02092 0.00072 0.00003 0.00002 0.00004 0.00000 0.00019 0.00020 0.00021 0.00016 0.00015 0.00015 0.00010 S2 0.30817 -0.14834 0.41830 1.00000 0.01608 0.01651 0.01918 0.00039 0.00111 -0.00167 0.01744 0.00069 0.00003 0.00002 0.00003 0.00000 0.00019 0.00019 0.00019 0.00014 0.00014 0.00014 0.00010 P1 0.25766 0.07602 0.76957 1.00000 0.01457 0.01157 0.01170 0.00034 0.00094 0.00067 0.01274 0.00068 0.00003 0.00002 0.00003 0.00000 0.00019 0.00018 0.00018 0.00013 0.00014 0.00014 0.00009 O11 0.41198 -0.18016 0.73229 0.16660 0.04162 0.05232 0.03391 0.00356 -0.00178 -0.00500 0.04346 0.01615 0.00065 0.00053 0.00077 0.00000 0.00510 0.00568 0.00455 0.00403 0.00375 0.00424 0.00213 H10A 0.20243 -0.24774 0.57904 1.00000 0.05907 0.04909 0.00191 0.00157 0.00235 0.00000 0.00804 H10B 0.20384 -0.30363 0.65752 1.00000 0.06556 0.05177 0.00204 0.00163 0.00260 0.00000 0.00887 Final Structure Factor Calculation for 2008src0504 in P2(1)/c Total number of l.s. parameters = 385 Maximum vector length = 511 Memory required = 4068 / 24017 wR2 = 0.0894 before cycle 5 for 6575 data and 0 / 385 parameters GooF = S = 1.034; Restrained GooF = 1.034 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0373 * P )^2 + 1.86 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0358 for 5500 Fo > 4sig(Fo) and 0.0467 for all 6575 data wR2 = 0.0894, GooF = S = 1.034, Restrained GooF = 1.034 for all data Occupancy sum of asymmetric unit = 40.17 for non-hydrogen and 35.00 for hydrogen atoms Principal mean square atomic displacements U 0.0191 0.0140 0.0131 C1 0.0230 0.0161 0.0126 C2 0.0261 0.0180 0.0141 C3 0.0205 0.0147 0.0125 C4 0.0288 0.0165 0.0130 C5 0.0748 0.0352 0.0120 C6 0.0464 0.0243 0.0135 C7 0.0489 0.0293 0.0132 C8 0.0370 0.0227 0.0165 C9 0.0249 0.0174 0.0129 C10 0.0520 0.0235 0.0144 C11 0.0205 0.0128 0.0116 C12 0.0204 0.0175 0.0143 C13 0.0327 0.0314 0.0161 C14 0.0300 0.0252 0.0142 C15 0.0381 0.0270 0.0118 C16 0.0318 0.0223 0.0146 C17 0.0213 0.0158 0.0130 C18 0.0345 0.0242 0.0142 C19 0.0237 0.0125 0.0111 C20 0.0272 0.0170 0.0103 C21 0.0358 0.0221 0.0166 C22 0.0383 0.0160 0.0158 C23 0.0459 0.0177 0.0119 C24 0.0413 0.0152 0.0128 C25 0.0284 0.0160 0.0106 C26 0.0471 0.0381 0.0158 C27 0.0390 0.0286 0.0161 O1 0.0390 0.0232 0.0168 O2 0.0510 0.0242 0.0164 O3 0.0338 0.0255 0.0115 O4 0.0355 0.0164 0.0136 O5 0.0284 0.0190 0.0149 O6 0.0308 0.0206 0.0130 O7 0.0257 0.0220 0.0155 O8 0.0279 0.0261 0.0133 O9 0.0587 0.0271 0.0224 O10 0.0313 0.0168 0.0146 S1 0.0206 0.0172 0.0145 S2 0.0153 0.0120 0.0110 P1 0.0571 0.0431 0.0301 O11 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.015 0.029 0.043 0.059 0.076 0.098 0.122 0.157 0.214 1.000 Number in group 708. 634. 651. 648. 655. 669. 634. 672. 648. 656. GooF 0.894 1.045 1.053 1.138 1.087 1.045 1.037 0.999 0.987 1.052 K 1.211 0.958 0.902 0.953 0.979 0.979 0.998 1.008 1.020 0.997 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.64 inf Number in group 665. 649. 683. 649. 639. 665. 648. 663. 657. 657. GooF 0.949 0.938 0.969 1.002 0.934 0.904 0.970 0.907 1.092 1.526 K 0.982 0.996 1.005 1.010 1.015 1.015 1.024 1.012 1.009 0.980 R1 0.109 0.084 0.072 0.060 0.046 0.039 0.036 0.027 0.028 0.033 Recommended weighting scheme: WGHT 0.0374 1.8522 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) -3 5 2 64.66 21.57 4.80 0.023 2.67 -4 3 4 408.40 278.59 4.53 0.083 2.20 -4 4 4 162.77 91.27 4.42 0.047 2.10 -5 5 2 550.17 736.52 4.16 0.134 2.15 4 8 4 175.95 106.62 3.95 0.051 1.52 0 8 1 320.34 222.34 3.94 0.074 2.26 -2 0 4 145.40 83.70 3.89 0.045 2.74 2 8 1 32.12 5.75 3.80 0.012 2.12 -3 8 5 239.48 160.99 3.72 0.063 1.57 6 4 1 1783.53 2152.90 3.69 0.230 1.98 7 4 0 405.34 297.36 3.67 0.085 1.81 1 17 2 336.92 466.40 3.61 0.107 1.06 -8 1 1 51.80 20.02 3.59 0.022 1.74 9 5 0 28.63 3.99 3.59 0.010 1.42 -8 6 9 94.10 161.73 3.56 0.063 1.03 -4 7 4 597.87 463.97 3.55 0.107 1.76 6 6 1 207.25 298.81 3.51 0.086 1.78 3 6 3 70.36 123.97 3.47 0.055 2.02 -3 5 4 161.86 104.16 3.42 0.051 2.11 -8 8 8 102.65 165.90 3.41 0.064 1.05 -4 11 1 214.67 146.48 3.39 0.060 1.51 -7 3 3 -2.00 13.18 3.34 0.018 1.79 -4 3 5 1522.54 1278.11 3.25 0.177 1.92 0 8 3 857.53 1044.42 3.24 0.160 1.96 -5 4 3 448.43 571.66 3.23 0.118 2.13 -16 9 5 78.10 182.67 3.20 0.067 0.79 3 3 0 469.13 364.36 3.19 0.094 3.69 -9 2 7 59.76 26.85 3.17 0.026 1.19 6 2 0 609.18 756.26 3.16 0.136 2.23 -8 6 2 887.44 723.45 3.15 0.133 1.51 -4 0 2 12032.94 13817.87 3.11 0.582 3.17 -2 4 3 48.28 22.56 3.11 0.024 2.79 6 7 2 189.48 130.68 3.11 0.057 1.60 1 15 0 62.22 27.92 3.10 0.026 1.22 8 0 0 3061.47 2625.96 3.08 0.254 1.73 12 11 3 71.25 129.18 3.07 0.056 0.89 2 6 3 55.02 26.01 3.05 0.025 2.17 3 11 0 24.35 4.73 3.04 0.011 1.57 -2 8 3 329.41 425.28 3.02 0.102 1.93 -1 13 2 511.79 405.06 3.01 0.100 1.37 -3 7 5 78.96 125.53 3.00 0.055 1.66 1 4 5 741.51 897.84 2.99 0.148 1.95 8 6 9 60.20 110.99 2.98 0.052 0.90 -2 1 2 2078.37 2441.29 2.98 0.245 4.57 -8 1 9 21.92 4.45 2.96 0.010 1.09 0 10 1 418.41 328.15 2.94 0.090 1.82 -1 6 5 130.35 86.86 2.93 0.046 1.82 8 11 1 -1.32 17.61 2.93 0.021 1.18 2 15 2 33.81 10.33 2.93 0.016 1.18 1 5 6 846.15 703.41 2.90 0.131 1.62 Bond lengths and angles C1 - Distance Angles C2 1.5293 (0.0020) P1 1.8150 (0.0015) 110.78 (0.10) C1 - C2 C2 - Distance Angles C3 1.5206 (0.0020) C1 1.5293 (0.0020) 112.75 (0.13) C2 - C3 C3 - Distance Angles C2 1.5206 (0.0020) S1 1.8121 (0.0016) 116.54 (0.11) C3 - C2 C4 - Distance Angles C10 1.4015 (0.0022) C5 1.4097 (0.0022) 118.73 (0.14) P1 1.8073 (0.0015) 124.88 (0.12) 116.10 (0.12) C4 - C10 C5 C5 - Distance Angles O4 1.3503 (0.0021) C7 1.3880 (0.0024) 124.44 (0.15) C4 1.4097 (0.0022) 114.74 (0.14) 120.82 (0.16) C5 - O4 C7 C6 - Distance Angles O4 1.4328 (0.0020) C6 - C7 - Distance Angles C8 1.3814 (0.0028) C5 1.3880 (0.0024) 118.69 (0.16) C7 - C8 C8 - Distance Angles C9 1.3788 (0.0026) C7 1.3814 (0.0028) 122.12 (0.16) C8 - C9 C9 - Distance Angles C8 1.3788 (0.0026) C10 1.3919 (0.0023) 119.33 (0.17) C9 - C8 C10 - Distance Angles O5 1.3559 (0.0019) C9 1.3919 (0.0023) 122.22 (0.15) C4 1.4015 (0.0022) 117.53 (0.14) 120.24 (0.15) C10 - O5 C9 C11 - Distance Angles O5 1.4337 (0.0020) C11 - C12 - Distance Angles C18 1.4037 (0.0021) C13 1.4050 (0.0021) 118.67 (0.14) P1 1.8020 (0.0015) 125.73 (0.12) 115.42 (0.11) C12 - C18 C13 C13 - Distance Angles O6 1.3552 (0.0019) C15 1.3854 (0.0023) 124.58 (0.15) C12 1.4050 (0.0021) 113.94 (0.13) 121.48 (0.15) C13 - O6 C15 C14 - Distance Angles O6 1.4289 (0.0019) C14 - C15 - Distance Angles C13 1.3854 (0.0023) C16 1.3856 (0.0025) 118.20 (0.15) C15 - C13 C16 - Distance Angles C17 1.3761 (0.0025) C15 1.3856 (0.0025) 122.19 (0.16) C16 - C17 C17 - Distance Angles C16 1.3761 (0.0025) C18 1.3959 (0.0023) 119.52 (0.15) C17 - C16 C18 - Distance Angles O7 1.3530 (0.0019) C17 1.3959 (0.0023) 123.12 (0.14) C12 1.4037 (0.0021) 116.96 (0.14) 119.91 (0.14) C18 - O7 C17 C19 - Distance Angles O7 1.4298 (0.0019) C19 - C20 - Distance Angles C26 1.4036 (0.0022) C21 1.4100 (0.0022) 118.84 (0.14) P1 1.8072 (0.0015) 125.23 (0.12) 115.92 (0.11) C20 - C26 C21 C21 - Distance Angles O8 1.3565 (0.0019) C23 1.3935 (0.0022) 124.20 (0.15) C20 1.4100 (0.0022) 114.93 (0.13) 120.87 (0.15) C21 - O8 C23 C22 - Distance Angles O8 1.4338 (0.0020) C22 - C23 - Distance Angles C24 1.3806 (0.0026) C21 1.3935 (0.0022) 118.57 (0.16) C23 - C24 C24 - Distance Angles C23 1.3806 (0.0026) C25 1.3806 (0.0026) 122.08 (0.15) C24 - C23 C25 - Distance Angles C24 1.3806 (0.0026) C26 1.3957 (0.0022) 119.55 (0.15) C25 - C24 C26 - Distance Angles O9 1.3496 (0.0020) C25 1.3957 (0.0022) 122.91 (0.14) C20 1.4036 (0.0022) 117.20 (0.13) 119.88 (0.15) C26 - O9 C25 C27 - Distance Angles O9 1.4210 (0.0020) C27 - O1 - Distance Angles S2 1.4471 (0.0012) O1 - O2 - Distance Angles S2 1.4494 (0.0012) O2 - O3 - Distance Angles S2 1.4405 (0.0013) O3 - O4 - Distance Angles C5 1.3503 (0.0021) C6 1.4328 (0.0020) 118.98 (0.14) O4 - C5 O5 - Distance Angles C10 1.3559 (0.0019) C11 1.4337 (0.0020) 117.69 (0.13) O5 - C10 O6 - Distance Angles C13 1.3552 (0.0019) C14 1.4289 (0.0019) 118.40 (0.13) O6 - C13 O7 - Distance Angles C18 1.3530 (0.0019) C19 1.4298 (0.0019) 118.20 (0.13) O7 - C18 O8 - Distance Angles C21 1.3565 (0.0019) C22 1.4338 (0.0020) 119.42 (0.13) O8 - C21 O9 - Distance Angles C26 1.3496 (0.0020) C27 1.4210 (0.0020) 118.88 (0.13) O9 - C26 S1 - Distance Angles C3 1.8121 (0.0016) S2 2.1025 (0.0005) 100.78 (0.06) S1 - C3 S2 - Distance Angles O3 1.4405 (0.0013) O1 1.4471 (0.0012) 114.42 (0.08) O2 1.4494 (0.0012) 114.37 (0.08) 112.65 (0.08) S1 2.1025 (0.0005) 101.89 (0.05) 106.65 (0.05) 105.51 (0.05) S2 - O3 O1 O2 P1 - Distance Angles C12 1.8020 (0.0015) C20 1.8072 (0.0015) 104.65 (0.07) C4 1.8073 (0.0016) 112.06 (0.07) 114.59 (0.07) C1 1.8150 (0.0015) 113.27 (0.07) 108.84 (0.07) 103.66 (0.07) P1 - C12 C20 C4 FMAP and GRID set by program FMAP 2 2 23 GRID -1.250 -2 -2 1.250 2 2 R1 = 0.0464 for 6575 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.29 at 0.1846 0.0476 0.7614 [ 0.70 A from C4 ] Deepest hole -0.42 at 0.7243 0.1207 0.5735 [ 0.70 A from S2 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 3937 / 27653 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1846 0.0476 0.7614 1.00000 0.05 0.29 0.70 C4 1.14 P1 1.80 C5 1.91 C10 Q2 1 0.2420 0.1287 0.7496 1.00000 0.05 0.27 0.82 C12 1.01 P1 1.92 C13 1.99 C18 Q3 1 0.1396 -0.0051 0.7292 1.00000 0.05 0.27 0.66 C4 0.77 C5 1.76 C10 1.85 O4 Q4 1 0.3550 0.0848 0.9471 1.00000 0.05 0.25 0.70 C20 0.81 C21 1.77 C26 1.88 C23 Q5 1 0.2371 0.1878 0.8007 1.00000 0.05 0.25 0.61 C12 0.87 C13 1.75 C18 1.88 O6 Q6 1 0.2770 0.1960 0.7265 1.00000 0.05 0.24 0.71 C18 0.72 C12 1.79 O7 1.84 C17 Q7 1 0.3011 0.0528 0.7031 1.00000 0.05 0.23 0.70 C1 1.12 P1 1.38 H1A 1.41 H1B Q8 1 0.3044 0.0301 1.0707 1.00000 0.05 0.23 0.71 C26 0.72 C25 1.49 H25 1.79 C24 Q9 1 0.2854 0.0684 0.8541 1.00000 0.05 0.22 0.83 C20 0.98 P1 1.96 C26 1.97 C21 Q10 1 0.3044 0.0335 0.6056 1.00000 0.05 0.22 0.73 C1 0.80 C2 1.38 H1A 1.42 H1B Q11 1 0.0833 -0.0666 0.9905 1.00000 0.05 0.21 0.80 H27B 1.33 C27 1.61 H27A 1.97 O9 Q12 1 0.2986 0.2538 0.7000 1.00000 0.05 0.21 0.70 C18 0.75 C17 1.49 H17 1.81 C12 Q13 1 0.3051 0.0128 0.4970 1.00000 0.05 0.20 0.76 C3 0.80 C2 1.38 H2A 1.45 H3B Q14 1 0.1054 0.0470 0.7081 1.00000 0.05 0.20 0.62 C4 0.78 C10 1.81 C5 1.83 O5 Q15 1 0.2797 0.3074 0.7595 1.00000 0.05 0.20 0.76 C16 0.86 C17 1.47 H16 1.56 H17 Q16 1 0.2047 -0.1227 0.3818 1.00000 0.05 0.20 1.17 O2 1.52 S2 1.63 O1 1.98 H11C Q17 1 0.4409 0.0747 1.0000 1.00000 0.05 0.20 0.69 C21 0.74 C23 1.49 H23 1.82 C24 Q18 1 0.1876 -0.1507 0.8586 1.00000 0.05 0.19 0.38 H6A 0.80 C6 1.33 H6C 1.62 H6B Q19 1 0.0878 -0.0641 0.7183 1.00000 0.05 0.19 0.56 C7 0.87 C5 1.41 H7 1.61 C8 Q20 1 0.1585 0.1539 0.7196 1.00000 0.05 0.19 1.28 C12 1.50 O5 1.61 C13 2.01 P1 Q21 1 0.0558 0.0954 0.6728 1.00000 0.05 0.19 0.58 C10 0.78 O5 1.76 C4 1.76 C9 Q22 1 0.3069 -0.1501 0.9513 1.00000 0.05 0.18 1.02 H6B 1.56 C6 1.61 H6A 2.10 H22C Q23 1 0.3758 0.0393 1.1386 1.00000 0.05 0.18 0.69 C24 0.75 C25 1.44 H24 1.50 H25 Q24 1 0.4353 0.0762 1.1108 1.00000 0.05 0.18 0.76 C23 0.79 C24 1.48 H23 1.51 H24 Q25 1 0.1985 0.2914 0.7872 1.00000 0.05 0.18 0.68 C15 0.79 C16 1.52 H15 1.59 H16 Q26 1 0.0779 -0.1522 0.7523 1.00000 0.05 0.18 0.43 H7 1.30 C7 1.95 H6C 2.08 H6A Q27 1 -0.1008 0.0776 0.7182 1.00000 0.05 0.18 1.35 H9 1.65 H11C 1.71 C9 2.26 H27C Q28 1 0.4070 0.0381 0.4466 1.00000 0.05 0.18 0.56 H3A 1.12 C3 1.81 H3B 1.92 S1 Q29 1 0.0084 0.0465 0.6795 1.00000 0.05 0.18 0.71 C9 0.75 C10 1.41 H9 1.84 O5 Q30 1 0.3818 0.0567 0.9190 1.00000 0.05 0.18 0.76 C21 0.90 C20 1.72 O8 1.90 C23 Q31 1 0.1903 -0.1878 0.5153 1.00000 0.05 0.18 1.07 O1 1.31 H10A 1.90 H11A 2.05 O10 Q32 1 0.2359 -0.2206 0.4671 1.00000 0.05 0.17 1.36 O1 1.50 H10A 1.81 S2 2.08 O3 Q33 1 -0.0216 -0.0016 0.6756 1.00000 0.05 0.17 0.55 C9 0.90 C8 1.37 H9 1.63 C10 Q34 1 0.5379 0.1600 0.8066 1.00000 0.05 0.17 0.39 H22B 0.80 C22 1.44 H22C 1.60 H22A Q35 1 0.1917 -0.3473 0.5363 1.00000 0.05 0.17 1.50 O10 1.57 H10B 1.64 H27A 1.65 H6A Q36 1 0.4534 0.0273 0.8612 1.00000 0.05 0.17 1.64 C21 1.76 O8 1.97 H24 2.12 C24 Q37 1 0.1600 -0.1543 0.6449 1.00000 0.05 0.17 1.46 H6C 1.86 H7 2.00 H10A 2.10 O1 Q38 1 0.1758 0.0656 0.4561 1.00000 0.05 0.17 1.01 H2B 1.63 H8 1.67 C2 1.81 H2A Q39 1 0.4645 -0.0019 0.5748 1.00000 0.05 0.17 1.78 S1 2.03 H1A 2.10 H3A 2.17 C3 Q40 1 0.1703 0.2397 0.8161 1.00000 0.05 0.17 0.69 C13 0.81 C15 1.52 H15 1.82 C12 Shortest distances between peaks (including symmetry equivalents) 4 30 0.74 29 33 0.98 3 14 1.08 31 32 1.09 5 6 1.09 25 40 1.10 21 29 1.13 23 24 1.16 6 12 1.16 14 21 1.16 7 10 1.16 8 23 1.17 1 14 1.17 17 30 1.18 1 3 1.18 2 5 1.24 12 15 1.25 2 20 1.25 15 25 1.26 17 24 1.27 4 17 1.27 10 13 1.29 3 19 1.30 14 29 1.34 4 9 1.35 5 40 1.37 2 6 1.37 30 36 1.39 9 30 1.45 5 20 1.46 1 9 1.66 2 9 1.66 19 26 1.68 13 28 1.68 31 37 1.70 28 39 1.71 1 2 1.71 2 7 1.75 27 29 1.75 7 9 1.78 18 26 1.79 26 37 1.80 20 21 1.81 6 20 1.82 18 22 1.83 17 36 1.83 1 7 1.85 16 27 1.89 20 40 1.91 19 33 1.92 27 33 1.94 4 8 1.94 5 12 1.95 16 31 1.96 12 25 1.96 28 39 1.97 14 33 1.97 5 25 1.98 18 35 2.00 22 35 2.00 8 24 2.01 4 24 2.01 1 20 2.04 17 23 2.04 13 38 2.04 16 32 2.06 3 29 2.06 14 19 2.07 6 15 2.09 39 39 2.09 6 40 2.09 21 33 2.09 4 36 2.09 14 20 2.10 1 21 2.11 15 40 2.15 19 37 2.18 11 35 2.20 24 30 2.21 8 30 2.22 3 21 2.23 6 25 2.24 3 33 2.24 13 39 2.28 4 23 2.29 19 29 2.33 8 17 2.33 10 38 2.34 5 15 2.35 5 9 2.35 21 27 2.35 18 37 2.38 12 40 2.40 10 39 2.41 2 14 2.42 2 40 2.45 7 13 2.45 24 36 2.45 9 36 2.46 1 19 2.47 10 28 2.47 1 29 2.49 18 19 2.51 23 30 2.51 9 17 2.52 8 9 2.52 7 30 2.52 2 12 2.53 3 7 2.56 32 35 2.57 7 36 2.60 22 32 2.60 1 10 2.63 2 10 2.63 2 4 2.65 3 9 2.66 9 20 2.66 6 7 2.68 20 25 2.68 2 21 2.68 23 36 2.69 33 38 2.69 1 5 2.70 18 32 2.70 32 37 2.70 12 20 2.72 17 36 2.73 11 18 2.73 6 9 2.75 7 14 2.75 7 20 2.76 4 7 2.80 9 14 2.81 34 36 2.83 2 30 2.84 2 3 2.84 4 5 2.86 3 26 2.87 20 29 2.87 5 7 2.92 9 10 2.93 3 37 2.94 3 20 2.95 31 35 2.95 14 27 2.96 3 10 2.97 1 4 2.99 Time profile in seconds ----------------------- 0.06: 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 0.02: Analyse other restraints etc. 9.56: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 2.25: Structure factors and derivatives 4.69: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.75: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.08: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.11: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008src0504 finished at 11:35:09 Total CPU time: 17.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++