+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s93 started at 10:49:47 on 07-May-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s93 in P2(1)/c CELL 0.71069 14.8790 12.0240 14.6050 90.000 111.400 90.000 ZERR 4.00 0.0002 0.0002 0.0002 0.000 0.0007 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O F PT UNIT 96 88 4 16 28 4 V = 2432.76 F(000) = 1384.0 Mu = 5.85 mm-1 Cell Wt = 2866.06 Rho = 1.956 MERG 2 OMIT -3.00 55.00 OMIT 0 1 2 OMIT -1 0 4 OMIT 0 0 4 OMIT 1 0 2 SHEL 7 0.77 FMAP 2 PLAN 5 SIZE 0.03 0.09 0.13 ACTA BOND $H WGHT 0.00610 3.41910 L.S. 12 TEMP -153.00 FVAR 0.26059 PT1 6 0.067134 0.174464 0.396212 11.00000 0.01195 0.01238 = 0.01498 0.00023 0.00658 0.00099 MOLE 1 C1 1 -0.067751 0.199097 0.381445 11.00000 0.01450 0.01748 = 0.01142 0.00019 0.00467 0.00324 C2 1 -0.093042 0.312552 0.380858 11.00000 0.01844 0.01812 = 0.01443 0.00127 0.00666 0.00228 C3 1 -0.186251 0.344448 0.371107 11.00000 0.02397 0.01921 = 0.02446 -0.00110 0.00933 0.00572 AFIX 43 H3 2 -0.201764 0.420932 0.372377 11.00000 -1.20000 AFIX 0 C4 1 -0.255557 0.264300 0.359635 11.00000 0.01387 0.02702 = 0.03002 -0.00025 0.00870 0.00712 AFIX 43 H4 2 -0.319294 0.285233 0.352648 11.00000 -1.20000 AFIX 0 C5 1 -0.231786 0.151799 0.358299 11.00000 0.01487 0.02250 = 0.02008 -0.00215 0.00817 -0.00139 C6 1 -0.138341 0.119074 0.370493 11.00000 0.01512 0.01727 = 0.01630 -0.00158 0.00600 0.00243 AFIX 43 H6 2 -0.122891 0.042329 0.371323 11.00000 -1.20000 AFIX 0 C7 1 -0.013511 0.385671 0.394630 11.00000 0.01917 0.01610 = 0.01657 0.00174 0.00818 0.00378 AFIX 43 H7 2 -0.020924 0.464121 0.395058 11.00000 -1.20000 AFIX 0 C8 1 0.153153 0.407900 0.423765 11.00000 0.01823 0.01374 = 0.01666 -0.00370 0.00774 -0.00110 C9 1 0.239073 0.379523 0.499779 11.00000 0.02002 0.01791 = 0.01882 -0.00007 0.00551 0.00137 AFIX 43 H9 2 0.241548 0.315412 0.538640 11.00000 -1.20000 AFIX 0 C10 1 0.320138 0.444013 0.518620 11.00000 0.01905 0.02203 = 0.02359 -0.00265 0.00245 0.00144 AFIX 43 H10 2 0.378106 0.424913 0.571160 11.00000 -1.20000 AFIX 0 C11 1 0.317791 0.537186 0.461142 11.00000 0.01769 0.02096 = 0.02518 -0.00752 0.00795 -0.00384 C12 1 0.232609 0.565622 0.385129 11.00000 0.02215 0.01645 = 0.02253 -0.00071 0.00966 0.00001 AFIX 43 H12 2 0.230420 0.629210 0.345766 11.00000 -1.20000 AFIX 0 C13 1 0.150862 0.500965 0.366902 11.00000 0.01856 0.01869 = 0.01618 -0.00109 0.00645 0.00098 AFIX 43 H13 2 0.092641 0.520579 0.314919 11.00000 -1.20000 AFIX 0 C14 1 -0.286594 -0.036962 0.338786 11.00000 0.02024 0.02204 = 0.03779 -0.00281 0.01326 -0.00619 AFIX 137 H14A 2 -0.265764 -0.050416 0.283367 11.00000 -1.50000 H14B 2 -0.345340 -0.079754 0.329458 11.00000 -1.50000 H14C 2 -0.235474 -0.060138 0.400064 11.00000 -1.50000 AFIX 0 C15 1 0.407986 0.677819 0.418752 11.00000 0.03145 0.03642 = 0.04265 -0.00409 0.01669 -0.01542 AFIX 137 H15A 2 0.391613 0.645481 0.353063 11.00000 -1.50000 H15B 2 0.473783 0.707652 0.441158 11.00000 -1.50000 H15C 2 0.362612 0.737885 0.416192 11.00000 -1.50000 AFIX 0 N1 3 0.069523 0.340540 0.406571 11.00000 0.01785 0.01173 = 0.01628 -0.00082 0.00728 0.00028 O1 4 -0.305920 0.079270 0.343861 11.00000 0.01469 0.02412 = 0.03925 -0.00437 0.01294 -0.00295 O2 4 0.402118 0.594382 0.485202 11.00000 0.01840 0.02868 = 0.03758 -0.00212 0.00512 -0.00917 MOLE 2 C21 1 0.464390 0.132598 0.318742 11.00000 0.02006 0.04172 = 0.03030 -0.00189 0.01462 -0.00343 C22 1 0.364772 0.140780 0.327103 11.00000 0.01800 0.03460 = 0.02774 0.00363 0.00992 0.00322 C23 1 0.349958 0.070364 0.408454 11.00000 0.01540 0.01951 = 0.02350 0.00181 0.00634 0.00140 C24 1 0.244493 0.061116 0.399128 11.00000 0.01259 0.02092 = 0.01592 0.00316 0.00604 0.00368 C25 1 0.201155 -0.041768 0.384521 11.00000 0.01711 0.01733 = 0.02390 -0.00037 0.00896 0.00320 AFIX 43 H25 2 0.238500 -0.103455 0.378476 11.00000 -1.20000 AFIX 0 C26 1 0.106360 -0.062943 0.377835 11.00000 0.01698 0.01428 = 0.01369 0.00017 0.00679 0.00240 C27 1 0.070313 -0.180754 0.367727 11.00000 0.01787 0.01467 = 0.01779 0.00007 0.00766 -0.00019 AFIX 23 H27A 2 0.110386 -0.222994 0.426676 11.00000 -1.20000 H27B 2 0.079534 -0.214797 0.310058 11.00000 -1.20000 AFIX 0 C28 1 -0.034913 -0.193273 0.355728 11.00000 0.01733 0.01745 = 0.01866 0.00156 0.00869 -0.00081 AFIX 23 H28A 2 -0.076214 -0.157643 0.293474 11.00000 -1.20000 H28B 2 -0.046145 -0.154794 0.410525 11.00000 -1.20000 AFIX 0 C29 1 -0.062917 -0.315090 0.354695 11.00000 0.02804 0.01947 = 0.01854 -0.00288 0.00991 -0.00626 AFIX 137 H29A 2 -0.057665 -0.351697 0.296903 11.00000 -1.50000 H29B 2 -0.129554 -0.320467 0.352008 11.00000 -1.50000 H29C 2 -0.019569 -0.351573 0.414509 11.00000 -1.50000 AFIX 0 O21 4 0.210475 0.155825 0.408146 11.00000 0.01164 0.01759 = 0.02259 -0.00087 0.00715 0.00128 O22 4 0.045501 0.010412 0.380440 11.00000 0.01482 0.01314 = 0.02243 -0.00002 0.00892 0.00151 F21 5 0.478273 0.034612 0.286842 11.00000 0.03177 0.05892 = 0.05945 -0.02204 0.02996 -0.00354 F22 5 0.469959 0.206824 0.253722 11.00000 0.03919 0.07756 = 0.05933 0.02384 0.03529 0.00217 F23 5 0.533580 0.152897 0.403884 11.00000 0.01699 0.07392 = 0.03618 -0.01416 0.01158 -0.01273 F24 5 0.348892 0.247558 0.340553 11.00000 0.04895 0.02959 = 0.08684 0.02343 0.04966 0.01303 F25 5 0.299039 0.107184 0.240438 11.00000 0.01872 0.10193 = 0.02267 0.00691 0.00413 -0.00570 F26 5 0.389251 -0.030310 0.406376 11.00000 0.01723 0.02410 = 0.06445 0.00717 0.01872 0.00781 F27 5 0.402164 0.117074 0.496056 11.00000 0.01609 0.05328 = 0.02311 -0.00483 0.00424 -0.00660 HKLF 4 Covalent radii and connectivity table for s93 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 F 0.640 PT 1.370 Pt1 - C1 O22 N1 O21 C1 - C6 C2 Pt1 C2 - C3 C1 C7 C3 - C4 C2 C4 - C3 C5 C5 - O1 C6 C4 C6 - C1 C5 C7 - N1 C2 C8 - C13 C9 N1 C9 - C10 C8 C10 - C9 C11 C11 - O2 C12 C10 C12 - C13 C11 C13 - C12 C8 C14 - O1 C15 - O2 N1 - C7 C8 Pt1 O1 - C5 C14 O2 - C11 C15 C21 - F21 F23 F22 C22 C22 - F24 F25 C21 C23 C23 - F26 F27 C24 C22 C24 - O21 C25 C23 C25 - C24 C26 C26 - O22 C25 C27 C27 - C26 C28 C28 - C27 C29 C29 - C28 O21 - C24 Pt1 O22 - C26 Pt1 F21 - C21 F22 - C21 F23 - C21 F24 - C22 F25 - C22 F26 - C23 F27 - C23 h k l Fo^2 Sigma Why rejected 2 0 5 7.02 1.38 observed but should be systematically absent 29686 Reflections read, of which 850 rejected -19 =< h =< 19, -15 =< k =< 15, -18 =< l =< 18, Max. 2-theta = 54.96 1 Systematic absence violations 0 Inconsistent equivalents 5563 Unique reflections, of which 0 suppressed R(int) = 0.0306 R(sigma) = 0.0259 Friedel opposites merged Maximum memory for data reduction = 2988 / 55324 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 = 3889 / 427080 wR2 = 0.0391 before cycle 1 for 5563 data and 337 / 337 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0061 * P )^2 + 3.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.26057 0.00014 -0.175 OSF Mean shift/esd = 0.010 Maximum = -0.212 for U22 Pt1 Max. shift = 0.000 A for H29C Max. dU = 0.000 for O1 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3889 / 427080 wR2 = 0.0390 before cycle 2 for 5563 data and 337 / 337 parameters GooF = S = 1.041; Restrained GooF = 1.041 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0061 * P )^2 + 3.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.26056 0.00013 -0.047 OSF Mean shift/esd = 0.003 Maximum = -0.070 for U22 Pt1 Max. shift = 0.000 A for H29C Max. dU = 0.000 for O1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3889 / 427080 wR2 = 0.0391 before cycle 3 for 5563 data and 337 / 337 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0061 * P )^2 + 3.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.26056 0.00014 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for H29B Max. dU = 0.000 for C24 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3889 / 427080 wR2 = 0.0391 before cycle 4 for 5563 data and 337 / 337 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0061 * P )^2 + 3.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.26056 0.00014 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z Pt1 Max. shift = 0.000 A for H15C Max. dU = 0.000 for C11 Least-squares cycle 5 Maximum vector length = 511 Memory required = 3889 / 427080 wR2 = 0.0391 before cycle 5 for 5563 data and 337 / 337 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0061 * P )^2 + 3.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.26056 0.00014 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z Pt1 Max. shift = 0.000 A for C11 Max. dU = 0.000 for O2 Least-squares cycle 6 Maximum vector length = 511 Memory required = 3889 / 427080 wR2 = 0.0391 before cycle 6 for 5563 data and 337 / 337 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0061 * P )^2 + 3.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.26056 0.00014 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for H29C Max. dU = 0.000 for F21 Least-squares cycle 7 Maximum vector length = 511 Memory required = 3889 / 427080 wR2 = 0.0391 before cycle 7 for 5563 data and 337 / 337 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0061 * P )^2 + 3.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.26056 0.00014 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z Pt1 Max. shift = 0.000 A for C11 Max. dU = 0.000 for C28 Least-squares cycle 8 Maximum vector length = 511 Memory required = 3889 / 427080 wR2 = 0.0391 before cycle 8 for 5563 data and 337 / 337 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0061 * P )^2 + 3.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.26056 0.00014 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H29C Max. dU = 0.000 for F21 Least-squares cycle 9 Maximum vector length = 511 Memory required = 3889 / 427080 wR2 = 0.0391 before cycle 9 for 5563 data and 337 / 337 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0061 * P )^2 + 3.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.26056 0.00014 -0.001 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z Pt1 Max. shift = 0.000 A for H15B Max. dU = 0.000 for F21 Least-squares cycle 10 Maximum vector length = 511 Memory required = 3889 / 427080 wR2 = 0.0391 before cycle 10 for 5563 data and 337 / 337 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0061 * P )^2 + 3.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.26056 0.00014 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.001 for U33 Pt1 Max. shift = 0.000 A for H29A Max. dU = 0.000 for C27 Least-squares cycle 11 Maximum vector length = 511 Memory required = 3889 / 427080 wR2 = 0.0391 before cycle 11 for 5563 data and 337 / 337 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0061 * P )^2 + 3.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.26056 0.00014 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z Pt1 Max. shift = 0.000 A for H29B Max. dU = 0.000 for C23 Least-squares cycle 12 Maximum vector length = 511 Memory required = 3889 / 427080 wR2 = 0.0391 before cycle 12 for 5563 data and 337 / 337 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0061 * P )^2 + 3.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.26056 0.00014 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z Pt1 Max. shift = 0.000 A for H15A Max. dU = 0.000 for C21 Largest correlation matrix elements 0.629 U13 F24 / U33 F24 0.565 U13 F21 / U33 F21 0.530 U13 C21 / U33 C21 0.628 U13 F24 / U11 F24 0.561 U13 Pt1 / U33 Pt1 0.522 U11 Pt1 / OSF 0.597 U13 F22 / U11 F22 0.559 U33 Pt1 / OSF 0.514 U13 C21 / U11 C21 0.585 U13 F22 / U33 F22 0.558 U13 Pt1 / U11 Pt1 0.503 z F22 / x F22 0.570 U12 F24 / U23 F24 0.549 U22 Pt1 / OSF 0.566 U13 F21 / U11 F21 0.535 z F24 / x F24 Idealized hydrogen atom generation before cycle 13 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 -0.2018 0.4209 0.3724 43 0.950 0.000 C3 C4 C2 H4 -0.3193 0.2852 0.3526 43 0.950 0.000 C4 C3 C5 H6 -0.1229 0.0423 0.3713 43 0.950 0.000 C6 C1 C5 H7 -0.0209 0.4641 0.3951 43 0.950 0.000 C7 N1 C2 H9 0.2415 0.3154 0.5386 43 0.950 0.000 C9 C10 C8 H10 0.3781 0.4249 0.5712 43 0.950 0.000 C10 C9 C11 H12 0.2304 0.6292 0.3458 43 0.950 0.000 C12 C13 C11 H13 0.0926 0.5206 0.3149 43 0.950 0.000 C13 C12 C8 H14A -0.2658 -0.0504 0.2834 137 0.980 0.000 C14 O1 H14A H14B -0.3453 -0.0797 0.3294 137 0.980 0.000 C14 O1 H14A H14C -0.2355 -0.0601 0.4001 137 0.980 0.000 C14 O1 H14A H15A 0.3916 0.6455 0.3531 137 0.980 0.000 C15 O2 H15A H15B 0.4738 0.7076 0.4412 137 0.980 0.000 C15 O2 H15A H15C 0.3626 0.7379 0.4162 137 0.980 0.000 C15 O2 H15A H25 0.2385 -0.1035 0.3785 43 0.950 0.000 C25 C24 C26 H27A 0.1104 -0.2230 0.4267 23 0.990 0.000 C27 C26 C28 H27B 0.0795 -0.2148 0.3101 23 0.990 0.000 C27 C26 C28 H28A -0.0762 -0.1576 0.2935 23 0.990 0.000 C28 C27 C29 H28B -0.0461 -0.1548 0.4105 23 0.990 0.000 C28 C27 C29 H29A -0.0576 -0.3517 0.2969 137 0.980 0.000 C29 C28 H29A H29B -0.1296 -0.3205 0.3520 137 0.980 0.000 C29 C28 H29A H29C -0.0196 -0.3516 0.4145 137 0.980 0.000 C29 C28 H29A s93 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Pt1 0.06713 0.17446 0.39621 1.00000 0.01195 0.01237 0.01497 0.00023 0.00657 0.00099 0.01263 0.00017 0.00001 0.00001 0.00001 0.00000 0.00005 0.00005 0.00005 0.00003 0.00004 0.00003 0.00003 C1 -0.06775 0.19909 0.38144 1.00000 0.01450 0.01746 0.01139 0.00020 0.00466 0.00324 0.01447 0.00482 0.00017 0.00019 0.00017 0.00000 0.00122 0.00111 0.00111 0.00088 0.00095 0.00092 0.00047 C2 -0.09304 0.31255 0.38086 1.00000 0.01842 0.01809 0.01442 0.00127 0.00665 0.00229 0.01679 0.00497 0.00018 0.00019 0.00017 0.00000 0.00131 0.00116 0.00117 0.00091 0.00102 0.00095 0.00050 C3 -0.18625 0.34445 0.37112 1.00000 0.02398 0.01920 0.02439 -0.00111 0.00930 0.00571 0.02239 0.00539 0.00020 0.00021 0.00019 0.00000 0.00144 0.00123 0.00138 0.00101 0.00116 0.00103 0.00055 H3 -0.20176 0.42093 0.37240 1.00000 0.02687 0.00000 0.00000 C4 -0.25556 0.26430 0.35963 1.00000 0.01388 0.02700 0.03001 -0.00023 0.00872 0.00710 0.02343 0.00538 0.00019 0.00021 0.00019 0.00000 0.00129 0.00135 0.00145 0.00111 0.00112 0.00104 0.00056 H4 -0.31930 0.28523 0.35264 1.00000 0.02811 0.00000 0.00000 C5 -0.23179 0.15180 0.35830 1.00000 0.01486 0.02250 0.02008 -0.00217 0.00817 -0.00139 0.01864 0.00502 0.00018 0.00020 0.00018 0.00000 0.00126 0.00122 0.00128 0.00098 0.00104 0.00098 0.00051 C6 -0.13834 0.11908 0.37050 1.00000 0.01510 0.01728 0.01626 -0.00159 0.00597 0.00244 0.01614 0.00476 0.00017 0.00020 0.00017 0.00000 0.00122 0.00114 0.00118 0.00092 0.00098 0.00094 0.00048 H6 -0.12288 0.04233 0.37133 1.00000 0.01937 0.00000 0.00000 C7 -0.01352 0.38567 0.39463 1.00000 0.01914 0.01609 0.01655 0.00173 0.00815 0.00378 0.01680 0.00493 0.00018 0.00020 0.00017 0.00000 0.00128 0.00114 0.00120 0.00092 0.00101 0.00095 0.00049 H7 -0.02093 0.46412 0.39505 1.00000 0.02016 0.00000 0.00000 C8 0.15316 0.40790 0.42377 1.00000 0.01819 0.01373 0.01663 -0.00369 0.00772 -0.00110 0.01580 0.00475 0.00018 0.00019 0.00017 0.00000 0.00127 0.00108 0.00118 0.00089 0.00100 0.00093 0.00048 C9 0.23907 0.37953 0.49978 1.00000 0.02003 0.01788 0.01882 -0.00007 0.00551 0.00137 0.01935 0.00494 0.00018 0.00020 0.00018 0.00000 0.00133 0.00117 0.00125 0.00097 0.00105 0.00100 0.00051 H9 0.24154 0.31542 0.53864 1.00000 0.02322 0.00000 0.00000 C10 0.32014 0.44401 0.51862 1.00000 0.01906 0.02201 0.02358 -0.00264 0.00245 0.00145 0.02304 0.00521 0.00019 0.00021 0.00019 0.00000 0.00136 0.00127 0.00136 0.00103 0.00110 0.00103 0.00056 H10 0.37811 0.42491 0.57115 1.00000 0.02765 0.00000 0.00000 C11 0.31779 0.53719 0.46114 1.00000 0.01768 0.02095 0.02519 -0.00752 0.00796 -0.00385 0.02123 0.00497 0.00018 0.00021 0.00019 0.00000 0.00131 0.00124 0.00134 0.00103 0.00109 0.00101 0.00053 C12 0.23261 0.56562 0.38513 1.00000 0.02216 0.01643 0.02252 -0.00071 0.00967 0.00002 0.01994 0.00504 0.00019 0.00020 0.00018 0.00000 0.00139 0.00114 0.00130 0.00098 0.00110 0.00100 0.00052 H12 0.23042 0.62921 0.34576 1.00000 0.02393 0.00000 0.00000 C13 0.15086 0.50096 0.36690 1.00000 0.01852 0.01868 0.01617 -0.00107 0.00645 0.00098 0.01775 0.00494 0.00018 0.00019 0.00017 0.00000 0.00127 0.00120 0.00118 0.00092 0.00101 0.00094 0.00050 H13 0.09264 0.52058 0.31492 1.00000 0.02130 0.00000 0.00000 C14 -0.28660 -0.03696 0.33878 1.00000 0.02025 0.02202 0.03778 -0.00280 0.01326 -0.00617 0.02594 0.00549 0.00020 0.00021 0.00021 0.00000 0.00138 0.00130 0.00158 0.00115 0.00122 0.00108 0.00058 H14A -0.26577 -0.05041 0.28336 1.00000 0.03891 0.00000 0.00000 H14B -0.34535 -0.07975 0.32945 1.00000 0.03891 0.00000 0.00000 H14C -0.23548 -0.06014 0.40006 1.00000 0.03891 0.00000 0.00000 C15 0.40799 0.67782 0.41876 1.00000 0.03148 0.03640 0.04264 -0.00409 0.01669 -0.01543 0.03595 0.00624 0.00023 0.00025 0.00024 0.00000 0.00175 0.00166 0.00185 0.00135 0.00148 0.00134 0.00073 H15A 0.39160 0.64549 0.35306 1.00000 0.05392 0.00000 0.00000 H15B 0.47379 0.70764 0.44115 1.00000 0.05392 0.00000 0.00000 H15C 0.36263 0.73790 0.41621 1.00000 0.05392 0.00000 0.00000 N1 0.06952 0.34054 0.40657 1.00000 0.01782 0.01172 0.01626 -0.00081 0.00726 0.00027 0.01497 0.00397 0.00014 0.00016 0.00014 0.00000 0.00113 0.00091 0.00103 0.00074 0.00089 0.00076 0.00042 O1 -0.30592 0.07927 0.34386 1.00000 0.01467 0.02410 0.03922 -0.00436 0.01293 -0.00295 0.02513 0.00365 0.00013 0.00015 0.00014 0.00000 0.00094 0.00093 0.00111 0.00081 0.00084 0.00074 0.00041 O2 0.40212 0.59438 0.48520 1.00000 0.01839 0.02867 0.03756 -0.00211 0.00511 -0.00916 0.02964 0.00366 0.00013 0.00016 0.00014 0.00000 0.00100 0.00101 0.00113 0.00085 0.00086 0.00080 0.00044 C21 0.46439 0.13260 0.31874 1.00000 0.02006 0.04171 0.03029 -0.00188 0.01463 -0.00343 0.02916 0.00588 0.00020 0.00025 0.00021 0.00000 0.00146 0.00165 0.00155 0.00129 0.00125 0.00124 0.00063 C22 0.36477 0.14078 0.32710 1.00000 0.01800 0.03458 0.02771 0.00363 0.00992 0.00320 0.02632 0.00576 0.00020 0.00024 0.00020 0.00000 0.00137 0.00149 0.00147 0.00118 0.00118 0.00115 0.00059 C23 0.34996 0.07037 0.40845 1.00000 0.01539 0.01950 0.02348 0.00180 0.00633 0.00140 0.01967 0.00512 0.00018 0.00020 0.00018 0.00000 0.00129 0.00118 0.00133 0.00100 0.00106 0.00098 0.00052 C24 0.24449 0.06112 0.39913 1.00000 0.01258 0.02092 0.01590 0.00317 0.00604 0.00369 0.01623 0.00492 0.00017 0.00020 0.00017 0.00000 0.00120 0.00117 0.00118 0.00093 0.00098 0.00093 0.00049 C25 0.20116 -0.04177 0.38452 1.00000 0.01709 0.01733 0.02389 -0.00038 0.00895 0.00319 0.01902 0.00500 0.00018 0.00020 0.00018 0.00000 0.00128 0.00118 0.00130 0.00097 0.00106 0.00096 0.00051 H25 0.23850 -0.10345 0.37848 1.00000 0.02283 0.00000 0.00000 C26 0.10636 -0.06294 0.37784 1.00000 0.01698 0.01428 0.01368 0.00017 0.00678 0.00240 0.01464 0.00479 0.00018 0.00019 0.00017 0.00000 0.00125 0.00107 0.00114 0.00088 0.00098 0.00091 0.00047 C27 0.07031 -0.18075 0.36773 1.00000 0.01784 0.01465 0.01776 0.00006 0.00764 -0.00019 0.01643 0.00490 0.00018 0.00018 0.00018 0.00000 0.00130 0.00112 0.00120 0.00090 0.00102 0.00093 0.00049 H27A 0.11038 -0.22299 0.42668 1.00000 0.01972 0.00000 0.00000 H27B 0.07953 -0.21480 0.31006 1.00000 0.01972 0.00000 0.00000 C28 -0.03491 -0.19327 0.35573 1.00000 0.01733 0.01743 0.01866 0.00157 0.00869 -0.00080 0.01721 0.00500 0.00018 0.00019 0.00018 0.00000 0.00129 0.00115 0.00124 0.00093 0.00104 0.00095 0.00050 H28A -0.07621 -0.15764 0.29347 1.00000 0.02066 0.00000 0.00000 H28B -0.04615 -0.15479 0.41052 1.00000 0.02066 0.00000 0.00000 C29 -0.06292 -0.31509 0.35470 1.00000 0.02801 0.01946 0.01854 -0.00288 0.00990 -0.00625 0.02161 0.00516 0.00020 0.00020 0.00019 0.00000 0.00152 0.00124 0.00129 0.00097 0.00115 0.00105 0.00055 H29A -0.05763 -0.35171 0.29692 1.00000 0.03242 0.00000 0.00000 H29B -0.12957 -0.32046 0.35198 1.00000 0.03242 0.00000 0.00000 H29C -0.01959 -0.35156 0.41453 1.00000 0.03242 0.00000 0.00000 O21 0.21048 0.15582 0.40815 1.00000 0.01164 0.01758 0.02257 -0.00087 0.00714 0.00127 0.01701 0.00337 0.00012 0.00013 0.00012 0.00000 0.00086 0.00082 0.00091 0.00067 0.00073 0.00065 0.00035 O22 0.04550 0.01041 0.38044 1.00000 0.01481 0.01312 0.02241 -0.00002 0.00891 0.00152 0.01619 0.00333 0.00012 0.00013 0.00012 0.00000 0.00085 0.00078 0.00088 0.00065 0.00071 0.00065 0.00034 F21 0.47827 0.03462 0.28684 1.00000 0.03176 0.05890 0.05942 -0.02203 0.02994 -0.00352 0.04629 0.00371 0.00013 0.00016 0.00014 0.00000 0.00103 0.00121 0.00121 0.00099 0.00094 0.00090 0.00048 F22 0.46996 0.20682 0.25372 1.00000 0.03920 0.07754 0.05932 0.02385 0.03529 0.00217 0.05383 0.00459 0.00014 0.00019 0.00015 0.00000 0.00118 0.00142 0.00129 0.00111 0.00104 0.00105 0.00054 F23 0.53358 0.15289 0.40389 1.00000 0.01699 0.07391 0.03617 -0.01415 0.01159 -0.01273 0.04183 0.00339 0.00012 0.00017 0.00013 0.00000 0.00087 0.00132 0.00101 0.00089 0.00077 0.00085 0.00046 F24 0.34889 0.24756 0.34056 1.00000 0.04892 0.02958 0.08681 0.02344 0.04964 0.01303 0.04812 0.00446 0.00014 0.00014 0.00016 0.00000 0.00120 0.00092 0.00149 0.00094 0.00114 0.00084 0.00052 F25 0.29904 0.10718 0.24044 1.00000 0.01870 0.10194 0.02267 0.00693 0.00412 -0.00571 0.04874 0.00369 0.00012 0.00019 0.00012 0.00000 0.00091 0.00166 0.00089 0.00096 0.00073 0.00098 0.00053 F26 0.38925 -0.03031 0.40638 1.00000 0.01722 0.02408 0.06445 0.00716 0.01872 0.00781 0.03418 0.00348 0.00011 0.00013 0.00013 0.00000 0.00081 0.00080 0.00117 0.00079 0.00081 0.00066 0.00040 F27 0.40217 0.11708 0.49606 1.00000 0.01609 0.05326 0.02310 -0.00483 0.00424 -0.00660 0.03163 0.00304 0.00011 0.00014 0.00011 0.00000 0.00080 0.00106 0.00081 0.00074 0.00066 0.00074 0.00038 Final Structure Factor Calculation for s93 in P2(1)/c Total number of l.s. parameters = 337 Maximum vector length = 511 Memory required = 3552 / 25039 wR2 = 0.0391 before cycle 13 for 5563 data and 0 / 337 parameters GooF = S = 1.043; Restrained GooF = 1.043 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0061 * P )^2 + 3.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0186 for 5123 Fo > 4sig(Fo) and 0.0218 for all 5563 data wR2 = 0.0391, GooF = S = 1.043, Restrained GooF = 1.043 for all data Occupancy sum of asymmetric unit = 37.00 for non-hydrogen and 22.00 for hydrogen atoms Principal mean square atomic displacements U 0.0153 0.0126 0.0099 Pt1 0.0197 0.0124 0.0113 C1 0.0206 0.0160 0.0138 C2 0.0283 0.0245 0.0143 C3 0.0315 0.0292 0.0096 C4 0.0239 0.0188 0.0132 C5 0.0200 0.0161 0.0124 C6 0.0219 0.0150 0.0134 C7 0.0198 0.0166 0.0110 C8 0.0225 0.0184 0.0172 C9 0.0316 0.0206 0.0170 C10 0.0309 0.0185 0.0143 C11 0.0235 0.0200 0.0163 C12 0.0201 0.0178 0.0154 C13 0.0383 0.0256 0.0139 C14 0.0502 0.0406 0.0171 C15 0.0181 0.0154 0.0114 N1 0.0404 0.0232 0.0117 O1 0.0424 0.0335 0.0130 O2 0.0425 0.0307 0.0143 C21 0.0363 0.0263 0.0164 C22 0.0246 0.0194 0.0150 C23 0.0230 0.0146 0.0110 C24 0.0239 0.0202 0.0129 C25 0.0184 0.0137 0.0118 C26 0.0186 0.0160 0.0146 C27 0.0200 0.0182 0.0135 C28 0.0313 0.0177 0.0158 C29 0.0229 0.0177 0.0104 O21 0.0225 0.0147 0.0114 O22 0.0813 0.0416 0.0160 F21 0.0941 0.0522 0.0152 F22 0.0794 0.0324 0.0136 F23 0.1006 0.0239 0.0199 F24 0.1036 0.0250 0.0176 F25 0.0660 0.0261 0.0104 F26 0.0546 0.0258 0.0145 F27 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.026 0.050 0.079 0.110 0.144 0.183 0.225 0.276 0.345 1.000 Number in group 571. 543. 569. 543. 556. 557. 552. 566. 545. 561. GooF 1.098 1.050 1.051 1.010 1.023 1.066 1.054 0.948 0.997 1.115 K 1.207 1.001 0.982 0.985 0.987 0.995 1.000 1.003 1.007 0.996 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.32 1.65 inf Number in group 561. 558. 551. 563. 558. 555. 545. 567. 550. 555. GooF 1.258 1.033 0.930 0.998 0.933 0.960 0.880 0.874 1.015 1.412 K 0.949 0.980 1.006 1.009 1.013 1.014 1.014 1.008 0.996 0.990 R1 0.055 0.038 0.029 0.027 0.021 0.019 0.015 0.013 0.012 0.013 Recommended weighting scheme: WGHT 0.0059 3.4253 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) -4 3 2 7.18 91.49 5.20 0.025 2.71 3 0 2 126815.90 135054.98 4.81 0.973 3.30 5 4 1 13523.62 14798.64 4.27 0.322 1.94 -1 3 2 -3.99 40.37 4.18 0.017 3.51 -5 4 3 8653.38 9581.56 4.07 0.259 2.08 4 3 0 25.28 91.26 3.79 0.025 2.62 -4 4 5 15149.92 16277.25 3.61 0.338 1.99 5 4 0 234.34 136.87 3.42 0.031 2.04 -10 10 13 503.50 741.62 3.36 0.072 0.78 1 1 2 28927.02 31190.26 3.35 0.467 4.91 1 3 0 -4.58 20.79 3.33 0.012 3.85 -6 3 1 24074.71 25507.57 3.29 0.423 2.08 4 6 3 588.96 438.16 3.26 0.055 1.53 6 4 1 36202.86 38184.24 3.25 0.517 1.75 7 3 1 15618.68 16696.26 3.21 0.342 1.69 -13 11 8 3081.30 3694.10 3.12 0.161 0.78 -5 13 3 8.96 94.36 3.11 0.026 0.88 -6 4 3 38093.66 40513.81 3.10 0.533 1.90 -5 5 1 15640.17 16642.90 3.08 0.341 1.86 -19 0 10 1796.84 2628.30 3.07 0.136 0.77 5 1 5 701.52 552.67 3.06 0.062 1.65 -2 7 15 -70.43 96.09 3.01 0.026 0.83 8 11 6 892.05 1175.93 2.95 0.091 0.80 -18 5 4 447.08 670.07 2.94 0.069 0.77 -12 6 7 102.90 4.67 2.93 0.006 1.03 -18 3 1 1694.48 2131.82 2.91 0.122 0.77 8 3 1 37257.27 39155.75 2.89 0.524 1.52 5 10 1 18149.06 16976.00 2.87 0.345 1.09 7 7 6 15359.35 14212.26 2.87 0.316 1.03 -3 3 6 121.43 64.55 2.86 0.021 2.07 -3 0 2 75609.11 80814.93 2.85 0.752 4.70 -3 1 8 3081.81 3411.07 2.85 0.155 1.80 7 13 4 616.48 895.93 2.82 0.079 0.79 -4 0 2 79215.36 85832.71 2.82 0.775 3.68 -15 9 9 6910.51 7983.61 2.81 0.236 0.78 3 4 12 1832.22 2146.58 2.79 0.123 0.96 9 7 10 828.66 1132.84 2.78 0.089 0.78 8 1 13 194.03 398.72 2.78 0.053 0.78 -15 6 1 823.30 1072.37 2.77 0.087 0.85 -2 6 6 -2.03 33.06 2.77 0.015 1.55 -2 2 18 4038.56 5152.05 2.77 0.190 0.78 3 1 0 55792.93 58312.07 2.77 0.639 4.31 5 3 12 289.84 444.76 2.76 0.056 0.91 -3 2 5 2332.28 2603.90 2.75 0.135 2.57 0 3 17 231.55 13.24 2.74 0.010 0.78 -1 1 2 49635.32 52018.87 2.74 0.604 6.20 12 3 9 2573.22 3294.40 2.74 0.152 0.77 5 2 13 110.09 230.08 2.73 0.040 0.87 3 5 12 246.23 376.87 2.73 0.051 0.94 2 1 6 6935.05 6467.35 2.72 0.213 1.93 Bond lengths and angles Pt1 - Distance Angles C1 1.9612 (0.0024) O22 1.9984 (0.0016) 91.21 (0.08) N1 2.0020 (0.0019) 81.20 (0.09) 172.29 (0.07) O21 2.0876 (0.0017) 177.09 (0.08) 91.16 (0.06) 96.39 (0.07) Pt1 - C1 O22 N1 C1 - Distance Angles C6 1.3898 (0.0033) C2 1.4144 (0.0032) 118.61 (0.22) Pt1 1.9612 (0.0024) 127.45 (0.18) 113.93 (0.18) C1 - C6 C2 C2 - Distance Angles C3 1.3952 (0.0035) C1 1.4144 (0.0032) 121.20 (0.23) C7 1.4282 (0.0034) 125.93 (0.22) 112.83 (0.22) C2 - C3 C1 C3 - Distance Angles C4 1.3763 (0.0037) C2 1.3952 (0.0035) 119.52 (0.23) H3 0.9500 120.24 120.24 C3 - C4 C2 C4 - Distance Angles C3 1.3763 (0.0037) C5 1.4001 (0.0034) 119.76 (0.24) H4 0.9500 120.12 120.12 C4 - C3 C5 C5 - Distance Angles O1 1.3609 (0.0029) C6 1.3925 (0.0033) 123.63 (0.22) C4 1.4001 (0.0034) 115.26 (0.22) 121.11 (0.23) C5 - O1 C6 C6 - Distance Angles C1 1.3898 (0.0033) C5 1.3925 (0.0033) 119.76 (0.22) H6 0.9500 120.12 120.12 C6 - C1 C5 C7 - Distance Angles N1 1.3016 (0.0030) C2 1.4282 (0.0034) 117.35 (0.21) H7 0.9500 121.32 121.32 C7 - N1 C2 C8 - Distance Angles C13 1.3865 (0.0032) C9 1.3955 (0.0034) 119.27 (0.23) N1 1.4281 (0.0030) 121.53 (0.22) 119.20 (0.21) C8 - C13 C9 C9 - Distance Angles C10 1.3746 (0.0036) C8 1.3955 (0.0034) 120.24 (0.23) H9 0.9500 119.88 119.88 C9 - C10 C8 C10 - Distance Angles C9 1.3746 (0.0036) C11 1.3927 (0.0036) 120.39 (0.24) H10 0.9500 119.80 119.80 C10 - C9 C11 C11 - Distance Angles O2 1.3598 (0.0030) C12 1.3889 (0.0036) 124.68 (0.23) C10 1.3927 (0.0036) 115.67 (0.23) 119.65 (0.24) C11 - O2 C12 C12 - Distance Angles C13 1.3851 (0.0034) C11 1.3889 (0.0036) 119.78 (0.23) H12 0.9500 120.11 120.11 C12 - C13 C11 C13 - Distance Angles C12 1.3851 (0.0034) C8 1.3865 (0.0032) 120.66 (0.23) H13 0.9500 119.67 119.67 C13 - C12 C8 C14 - Distance Angles O1 1.4342 (0.0030) H14A 0.9800 109.47 H14B 0.9800 109.47 109.47 H14C 0.9800 109.47 109.47 109.47 C14 - O1 H14A H14B C15 - Distance Angles O2 1.4204 (0.0034) H15A 0.9800 109.47 H15B 0.9800 109.47 109.47 H15C 0.9800 109.47 109.47 109.47 C15 - O2 H15A H15B N1 - Distance Angles C7 1.3016 (0.0030) C8 1.4281 (0.0030) 120.72 (0.20) Pt1 2.0020 (0.0019) 114.57 (0.16) 124.70 (0.15) N1 - C7 C8 O1 - Distance Angles C5 1.3609 (0.0029) C14 1.4342 (0.0030) 117.78 (0.20) O1 - C5 O2 - Distance Angles C11 1.3598 (0.0030) C15 1.4204 (0.0034) 117.49 (0.22) O2 - C11 C21 - Distance Angles F21 1.3107 (0.0034) F23 1.3159 (0.0032) 109.40 (0.25) F22 1.3276 (0.0033) 106.91 (0.24) 108.65 (0.24) C22 1.5342 (0.0037) 111.60 (0.23) 111.00 (0.23) 109.15 (0.24) C21 - F21 F23 F22 C22 - Distance Angles F24 1.3329 (0.0032) F25 1.3485 (0.0032) 108.67 (0.23) C21 1.5342 (0.0037) 107.57 (0.23) 107.27 (0.22) C23 1.5388 (0.0036) 109.46 (0.22) 107.50 (0.22) 116.16 (0.23) C22 - F24 F25 C21 C23 - Distance Angles F26 1.3495 (0.0028) F27 1.3530 (0.0029) 106.84 (0.20) C24 1.5289 (0.0034) 111.82 (0.20) 109.32 (0.20) C22 1.5388 (0.0036) 106.91 (0.21) 107.89 (0.21) 113.75 (0.20) C23 - F26 F27 C24 C24 - Distance Angles O21 1.2723 (0.0028) C25 1.3753 (0.0033) 129.75 (0.23) C23 1.5289 (0.0034) 111.09 (0.20) 119.15 (0.21) C24 - O21 C25 C25 - Distance Angles C24 1.3753 (0.0033) C26 1.4012 (0.0034) 125.26 (0.22) H25 0.9500 117.37 117.37 C25 - C24 C26 C26 - Distance Angles O22 1.2745 (0.0027) C25 1.4012 (0.0034) 125.47 (0.22) C27 1.5028 (0.0031) 115.04 (0.21) 119.49 (0.21) C26 - O22 C25 C27 - Distance Angles C26 1.5028 (0.0031) C28 1.5180 (0.0033) 114.89 (0.20) H27A 0.9900 108.54 108.55 H27B 0.9900 108.55 108.54 107.54 C27 - C26 C28 H27A C28 - Distance Angles C27 1.5180 (0.0033) C29 1.5214 (0.0032) 111.33 (0.20) H28A 0.9900 109.36 109.36 H28B 0.9900 109.36 109.36 107.99 C28 - C27 C29 H28A C29 - Distance Angles C28 1.5214 (0.0032) H29A 0.9800 109.47 H29B 0.9800 109.47 109.47 H29C 0.9800 109.47 109.47 109.47 C29 - C28 H29A H29B O21 - Distance Angles C24 1.2723 (0.0028) Pt1 2.0876 (0.0017) 121.36 (0.15) O21 - C24 O22 - Distance Angles C26 1.2745 (0.0027) Pt1 1.9984 (0.0016) 126.89 (0.15) O22 - C26 F21 - Distance Angles C21 1.3107 (0.0034) F21 - F22 - Distance Angles C21 1.3276 (0.0033) F22 - F23 - Distance Angles C21 1.3159 (0.0032) F23 - F24 - Distance Angles C22 1.3329 (0.0032) F24 - F25 - Distance Angles C22 1.3485 (0.0032) F25 - F26 - Distance Angles C23 1.3495 (0.0028) F26 - F27 - Distance Angles C23 1.3530 (0.0029) F27 - FMAP and GRID set by program FMAP 2 3 38 GRID -1.429 -1 -2 1.429 1 2 R1 = 0.0211 for 5563 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.58 at 0.0267 0.6881 0.1425 [ 0.82 A from C1 ] Deepest hole -0.72 at 0.0763 0.2406 0.4019 [ 0.81 A from PT1 ] Mean = 0.00, Rms deviation from mean = 0.09 e/A^3, Highest memory used = 3615 / 44552 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.0267 0.1881 0.3575 1.00000 0.05 0.58 0.82 C1 1.31 PT1 1.89 C2 1.93 C6 Q2 1 0.1660 0.1756 0.4335 1.00000 0.05 0.48 0.90 O21 1.37 PT1 1.98 C24 2.28 H9 Q3 1 -0.0042 0.1785 0.4295 1.00000 0.05 0.47 0.98 C1 1.32 PT1 2.00 C6 2.04 C2 Q4 1 0.0679 0.1935 0.4832 1.00000 0.05 0.43 1.29 PT1 1.76 H28B 2.02 C1 2.10 N1 Q5 1 0.0953 -0.1210 0.3757 1.00000 0.05 0.43 0.72 C26 0.80 C27 1.41 H27A 1.44 H27B Shortest distances between peaks (including symmetry equivalents) 1 3 0.99 3 4 1.09 1 4 1.86 2 4 1.87 2 3 2.51 1 2 2.67 Time profile in seconds ----------------------- 0.14: 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 0.02: Analyse other restraints etc. 2.30: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.08: Set up l.s. refinement 0.00: Generate idealized H-atoms 9.27: Structure factors and derivatives 19.39: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.05: Apply other restraints 1.95: Solve l.s. equations 0.00: Generate HTAB table 0.08: Other dependent quantities, CIF, tables 0.17: Analysis of variance 0.06: Merge reflections for Fourier and .fcf 0.14: Fourier summations 0.13: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s93 finished at 10:50:21 Total CPU time: 33.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++