+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 13:26:32 on 28-Nov-2002 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P-1 CELL 0.71073 8.6560 10.2951 25.0197 82.829 88.605 73.299 ZERR 1.00 0.0002 0.0002 0.0005 0.001 0.001 0.001 LATT 1 SFAC C H N S CR UNIT 66 48 12 32 2 V = 2118.70 F(000) = 1088.0 Mu = 1.10 mm-1 Cell Wt = 2139.08 Rho = 1.677 MERG 2 OMIT -1 -3 3 OMIT -2 0 7 OMIT -1 4 0 OMIT 0 4 6 OMIT -2 5 8 OMIT -1 5 9 OMIT 1 -5 6 OMIT 0 -4 -3 OMIT -1 -6 -3 OMIT -1 4 6 OMIT 0 -4 4 OMIT 2 8 3 OMIT 0 -6 -5 OMIT -3 -6 8 OMIT 1 -4 -3 OMIT 1 6 7 OMIT 0 6 -1 OMIT -2 6 -1 OMIT 1 3 0 OMIT -2 5 0 OMIT 0 4 0 OMIT 2 -5 5 OMIT 2 -4 1 OMIT -2 5 7 OMIT 1 5 2 OMIT 3 6 -2 ACTA SIZE 0.5 0.42 0.05 BASF 0.34855 FMAP 2 PLAN 10 BOND $H WGHT 0.10320 9.70610 L.S. 15 TEMP -153.00 FVAR 0.20622 MOLE 1 S1 4 -0.114369 0.189524 -0.238568 11.00000 0.03795 0.02701 = 0.01251 -0.00393 0.00819 -0.01503 S2 4 -0.278246 -0.087714 -0.205221 11.00000 0.03585 0.02242 = 0.01649 -0.00620 0.00169 -0.01420 S3 4 -0.264632 -0.024318 -0.094304 11.00000 0.03168 0.01894 = 0.01076 -0.00213 0.00140 -0.01197 S4 4 -0.116393 0.197537 -0.121520 11.00000 0.02264 0.01792 = 0.01146 -0.00332 0.00114 -0.00835 S5 4 -0.108717 0.238252 0.004093 11.00000 0.02715 0.01786 = 0.01300 -0.00240 -0.00066 -0.00829 S6 4 -0.278797 0.030667 0.030174 11.00000 0.03597 0.02470 = 0.01129 -0.00238 0.00399 -0.01556 S7 4 -0.312451 0.060825 0.146290 11.00000 0.05318 0.02326 = 0.01327 -0.00424 0.00988 -0.01327 S8 4 -0.107182 0.312260 0.112918 11.00000 0.03513 0.02294 = 0.01827 -0.00699 -0.00277 -0.00887 C1 1 -0.109581 0.053108 -0.277076 11.00000 0.03349 0.02804 = 0.00959 -0.00763 0.00428 -0.00956 AFIX 23 H1A 2 -0.097901 0.084611 -0.315592 11.00000 -1.20000 H1B 2 -0.013097 -0.024091 -0.266064 11.00000 -1.20000 AFIX 0 C2 1 -0.255851 0.002252 -0.271141 11.00000 0.02831 0.04844 = 0.01140 -0.00436 0.00077 -0.02104 AFIX 23 H2A 2 -0.251879 -0.059820 -0.298671 11.00000 -1.20000 H2B 2 -0.352914 0.081230 -0.278811 11.00000 -1.20000 AFIX 0 C3 1 -0.225301 0.016108 -0.162412 11.00000 0.01737 0.02432 = 0.00882 -0.00318 -0.00010 -0.00448 C4 1 -0.159949 0.118629 -0.174860 11.00000 0.02201 0.01599 = 0.01424 -0.00551 0.00233 -0.00455 C5 1 -0.189073 0.099503 -0.071411 11.00000 0.02230 0.01508 = 0.01936 -0.00131 0.00483 -0.01037 C6 1 -0.190768 0.120275 -0.018490 11.00000 0.01984 0.01861 = 0.01588 -0.00131 -0.00027 -0.00700 C7 1 -0.165520 0.208784 0.071610 11.00000 0.01854 0.01312 = 0.01146 -0.00429 0.00017 0.00720 C8 1 -0.242304 0.113765 0.083482 11.00000 0.02746 0.02246 = 0.01324 0.00173 0.00657 -0.00658 C9 1 -0.321101 0.210531 0.179053 11.00000 0.04244 0.01607 = 0.01776 -0.00809 0.00191 0.00099 AFIX 23 H9A 2 -0.404522 0.289753 0.160781 11.00000 -1.20000 H9B 2 -0.354473 0.194793 0.216866 11.00000 -1.20000 AFIX 0 C10 1 -0.166417 0.244327 0.178628 11.00000 0.03278 0.03354 = 0.01335 -0.00489 -0.00557 -0.00491 AFIX 23 H10A 2 -0.080430 0.160790 0.192174 11.00000 -1.20000 H10B 2 -0.173564 0.312251 0.204007 11.00000 -1.20000 AFIX 0 MOLE 2 S11 4 0.486172 0.583685 0.187627 11.00000 0.02220 0.02410 = 0.01174 -0.00480 0.00224 -0.00891 S12 4 0.754241 0.732684 0.112193 11.00000 0.03252 0.03055 = 0.01685 -0.00267 0.00064 -0.01859 S13 4 0.642536 0.631837 0.020606 11.00000 0.03078 0.03787 = 0.01287 -0.00546 0.00602 -0.01788 S14 4 0.414295 0.507407 0.082949 11.00000 0.02197 0.02571 = 0.01217 -0.00607 0.00357 -0.01068 C11 1 0.580208 0.707565 0.205948 11.00000 0.02585 0.02001 = 0.01779 -0.00738 -0.00118 -0.00073 AFIX 23 H11A 2 0.512264 0.800275 0.192230 11.00000 -1.20000 H11B 2 0.584414 0.701230 0.245723 11.00000 -1.20000 AFIX 0 C12 1 0.748478 0.689397 0.184561 11.00000 0.02467 0.02901 = 0.01002 -0.00637 -0.00317 -0.00680 AFIX 23 H12A 2 0.812667 0.593090 0.194198 11.00000 -1.20000 H12B 2 0.799751 0.747444 0.202330 11.00000 -1.20000 AFIX 0 C13 1 0.624302 0.649067 0.090522 11.00000 0.02158 0.01776 = 0.01220 -0.00388 0.00210 -0.00124 C14 1 0.522526 0.591915 0.118344 11.00000 0.01639 0.01534 = 0.01169 -0.00676 0.00664 -0.00418 C15 1 0.513073 0.529228 0.021735 11.00000 0.01262 0.01980 = 0.02057 -0.00664 0.00366 -0.00616 MOLE 3 CR1 5 0.376641 0.312605 0.355855 11.00000 0.01567 0.01951 = 0.00911 -0.00306 0.00335 -0.00699 S41 4 -0.016807 0.074868 0.402326 11.00000 0.02809 0.03194 = 0.02904 -0.00822 0.01170 -0.02102 S42 4 0.143519 0.463084 0.180438 11.00000 0.02849 0.02846 = 0.01301 0.00278 -0.00223 -0.01087 S43 4 0.839793 0.441741 0.304120 11.00000 0.01923 0.04751 = 0.02338 0.00253 0.00321 -0.01822 S44 4 0.708517 -0.091116 0.291531 11.00000 0.02266 0.02353 = 0.02242 -0.00937 -0.00062 0.00070 N21 3 0.231171 0.480438 0.387832 11.00000 0.01513 0.01444 = 0.01180 0.00087 0.00181 -0.00926 N22 3 0.465126 0.274915 0.434636 11.00000 0.00787 0.01306 = 0.01457 -0.00253 -0.00138 -0.00102 N41 3 0.214377 0.213899 0.380602 11.00000 0.01396 0.01664 = 0.01581 -0.00295 0.00135 -0.00971 N42 3 0.274259 0.367357 0.283646 11.00000 0.02423 0.02812 = 0.00733 -0.00356 0.00078 -0.01010 N43 3 0.540585 0.408443 0.335663 11.00000 0.01902 0.02248 = 0.01920 -0.00524 0.00656 -0.01099 N44 3 0.524714 0.139783 0.335445 11.00000 0.02313 0.02382 = 0.01622 -0.00766 0.00445 -0.00860 C21 1 0.111691 0.578742 0.363182 11.00000 0.01188 0.01423 = 0.01411 0.00141 0.00221 -0.00650 AFIX 43 H21 2 0.094213 0.580397 0.325733 11.00000 -1.20000 AFIX 0 C22 1 0.009190 0.681425 0.390825 11.00000 0.02229 0.01552 = 0.01921 -0.00096 -0.00669 -0.00224 AFIX 43 H22 2 -0.074930 0.750833 0.371691 11.00000 -1.20000 AFIX 0 C23 1 0.029866 0.682036 0.445257 11.00000 0.01761 0.01133 = 0.02309 -0.00474 0.00733 -0.01260 C24 1 0.159387 0.577217 0.472260 11.00000 0.01529 0.01570 = 0.00963 0.00072 0.00159 -0.00702 C25 1 0.253226 0.479415 0.441897 11.00000 0.01467 0.01574 = 0.01038 -0.00149 0.00223 -0.01006 C26 1 0.383313 0.367685 0.466985 11.00000 0.01721 0.01186 = 0.01232 -0.00394 0.00220 -0.00661 C27 1 0.417090 0.358308 0.522025 11.00000 0.01219 0.01881 = 0.01382 0.00216 0.00078 -0.00911 C28 1 0.543135 0.244551 0.544625 11.00000 0.01839 0.02022 = 0.01197 0.00482 -0.00400 -0.01306 C29 1 0.626457 0.152951 0.511194 11.00000 0.01607 0.01961 = 0.02461 0.00208 -0.00459 -0.00173 AFIX 43 H29 2 0.713854 0.077626 0.525063 11.00000 -1.20000 AFIX 0 C30 1 0.582535 0.170548 0.456462 11.00000 0.01498 0.01690 = 0.02442 -0.00537 0.00035 -0.00191 AFIX 43 H30 2 0.639805 0.104528 0.434291 11.00000 -1.20000 AFIX 0 C31 1 0.195563 0.565185 0.528713 11.00000 0.02505 0.01860 = 0.01506 -0.00779 0.00365 -0.01105 AFIX 43 H31 2 0.132494 0.631292 0.549828 11.00000 -1.20000 AFIX 0 C32 1 0.318448 0.460919 0.552565 11.00000 0.02440 0.02886 = 0.00489 0.00025 -0.00035 -0.01347 AFIX 43 H32 2 0.339570 0.455679 0.589976 11.00000 -1.20000 AFIX 0 C33 1 -0.083248 0.787635 0.475424 11.00000 0.02581 0.01979 = 0.01733 -0.00254 0.00976 -0.00853 AFIX 137 H33A 2 -0.168366 0.846608 0.450881 11.00000 -1.50000 H33B 2 -0.023179 0.843124 0.489945 11.00000 -1.50000 H33C 2 -0.131817 0.741900 0.505082 11.00000 -1.50000 AFIX 0 C34 1 0.585060 0.224902 0.603965 11.00000 0.02626 0.03642 = 0.00989 -0.00022 -0.00332 -0.01054 AFIX 137 H34A 2 0.495356 0.206084 0.625076 11.00000 -1.50000 H34B 2 0.604667 0.308059 0.613799 11.00000 -1.50000 H34C 2 0.682333 0.147828 0.611482 11.00000 -1.50000 AFIX 0 C41 1 0.116914 0.156990 0.388902 11.00000 0.01862 0.00970 = 0.01591 -0.00237 0.00136 0.00490 C42 1 0.220092 0.408148 0.240871 11.00000 0.01595 0.01512 = 0.02122 -0.00647 0.00812 -0.00740 C43 1 0.665798 0.421497 0.322092 11.00000 0.02992 0.01036 = 0.01404 -0.00206 -0.00497 -0.00596 C44 1 0.601339 0.043539 0.317607 11.00000 0.01467 0.02755 = 0.01081 0.00485 0.00385 -0.01046 HKLF 5 Covalent radii and connectivity table for s92 in P-1 C 0.770 H 0.320 N 0.700 S 1.030 CR 1.240 S1 - C4 C1 S2 - C3 C2 S3 - C5 C3 S4 - C5 C4 S5 - C6 C7 S6 - C6 C8 S7 - C8 C9 S8 - C7 C10 C1 - C2 S1 C2 - C1 S2 C3 - C4 S3 S2 C4 - C3 S4 S1 C5 - C6 S4 S3 C6 - C5 S5 S6 C7 - C8 S8 S5 C8 - C7 S7 S6 C9 - C10 S7 C10 - C9 S8 S11 - C14 C11 S12 - C13 C12 S13 - C15 C13 S14 - C15 C14 C11 - C12 S11 C12 - C11 S12 C13 - C14 S12 S13 C14 - C13 S11 S14 C15 - C15_$1 S13 S14 Cr1 - N43 N42 N44 N41 N21 N22 S41 - C41 S42 - C42 S43 - C43 S44 - C44 N21 - C21 C25 Cr1 N22 - C30 C26 Cr1 N41 - C41 Cr1 N42 - C42 Cr1 N43 - C43 Cr1 N44 - C44 Cr1 C21 - N21 C22 C22 - C23 C21 C23 - C22 C24 C33 C24 - C25 C23 C31 C25 - N21 C24 C26 C26 - N22 C27 C25 C27 - C26 C28 C32 C28 - C29 C27 C34 C29 - C28 C30 C30 - N22 C29 C31 - C32 C24 C32 - C31 C27 C33 - C23 C34 - C28 C41 - N41 S41 C42 - N42 S42 C43 - N43 S43 C44 - N44 S44 Operators for generating equivalent atoms: $1 -x+1, -y+1, -z ** MERG code changed to 0 for compatibility with HKLF and BASF parameters ** 19688 Reflections read, of which 120 rejected -11 =< h =< 11, -13 =< k =< 13, -32 =< l =< 32, Max. 2-theta = 55.36 0 Systematic absence violations 0 Data suppressed, R(sigma) = 0.0677 Maximum memory for data reduction = 4058 / 109 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 = 5304 / 673495 wR2 = 0.1887 before cycle 1 for 19591 data and 508 / 508 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1032 * P )^2 + 9.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20622 0.00027 0.012 OSF 2 0.34855 0.00082 -0.002 BASF 1 Mean shift/esd = 0.001 Maximum = 0.012 for OSF Max. shift = 0.000 A for H34B Max. dU = 0.000 for C29 Least-squares cycle 2 Maximum vector length = 511 Memory required = 5304 / 673495 wR2 = 0.1887 before cycle 2 for 19591 data and 508 / 508 parameters GooF = S = 1.045; Restrained GooF = 1.045 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1032 * P )^2 + 9.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20622 0.00027 0.001 OSF 2 0.34855 0.00082 -0.001 BASF 1 Mean shift/esd = 0.000 Maximum = 0.003 for U23 Cr1 Max. shift = 0.000 A for H34A Max. dU = 0.000 for C29 Least-squares cycle 3 Maximum vector length = 511 Memory required = 5304 / 673495 wR2 = 0.1887 before cycle 3 for 19591 data and 508 / 508 parameters GooF = S = 1.045; Restrained GooF = 1.045 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1032 * P )^2 + 9.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20622 0.00027 0.000 OSF 2 0.34855 0.00082 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.001 for U33 Cr1 Max. shift = 0.000 A for C43 Max. dU = 0.000 for C34 Least-squares cycle 4 Maximum vector length = 511 Memory required = 5304 / 673495 wR2 = 0.1887 before cycle 4 for 19591 data and 508 / 508 parameters GooF = S = 1.045; Restrained GooF = 1.045 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1032 * P )^2 + 9.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20622 0.00027 0.000 OSF 2 0.34855 0.00082 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H33A Max. dU = 0.000 for C12 Least-squares cycle 5 Maximum vector length = 511 Memory required = 5304 / 673495 wR2 = 0.1887 before cycle 5 for 19591 data and 508 / 508 parameters GooF = S = 1.045; Restrained GooF = 1.045 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1032 * P )^2 + 9.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20622 0.00027 0.000 OSF 2 0.34855 0.00082 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H33C Max. dU = 0.000 for C28 Least-squares cycle 6 Maximum vector length = 511 Memory required = 5304 / 673495 wR2 = 0.1887 before cycle 6 for 19591 data and 508 / 508 parameters GooF = S = 1.045; Restrained GooF = 1.045 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1032 * P )^2 + 9.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20622 0.00027 0.000 OSF 2 0.34855 0.00082 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H32 Max. dU = 0.000 for C23 Least-squares cycle 7 Maximum vector length = 511 Memory required = 5304 / 673495 wR2 = 0.1887 before cycle 7 for 19591 data and 508 / 508 parameters GooF = S = 1.045; Restrained GooF = 1.045 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1032 * P )^2 + 9.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20622 0.00027 0.000 OSF 2 0.34855 0.00082 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for z Cr1 Max. shift = 0.000 A for H34A Max. dU = 0.000 for C28 Least-squares cycle 8 Maximum vector length = 511 Memory required = 5304 / 673495 wR2 = 0.1887 before cycle 8 for 19591 data and 508 / 508 parameters GooF = S = 1.045; Restrained GooF = 1.045 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1032 * P )^2 + 9.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20622 0.00027 0.000 OSF 2 0.34855 0.00082 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for z Cr1 Max. shift = 0.000 A for H34C Max. dU = 0.000 for N44 Least-squares cycle 9 Maximum vector length = 511 Memory required = 5304 / 673495 wR2 = 0.1887 before cycle 9 for 19591 data and 508 / 508 parameters GooF = S = 1.045; Restrained GooF = 1.045 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1032 * P )^2 + 9.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20622 0.00027 0.000 OSF 2 0.34855 0.00082 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for z Cr1 Max. shift = 0.000 A for C41 Max. dU = 0.000 for C28 Least-squares cycle 10 Maximum vector length = 511 Memory required = 5304 / 673495 wR2 = 0.1887 before cycle 10 for 19591 data and 508 / 508 parameters GooF = S = 1.045; Restrained GooF = 1.045 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1032 * P )^2 + 9.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20622 0.00027 0.000 OSF 2 0.34855 0.00082 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for z Cr1 Max. shift = 0.000 A for H34C Max. dU = 0.000 for C24 Least-squares cycle 11 Maximum vector length = 511 Memory required = 5304 / 673495 wR2 = 0.1887 before cycle 11 for 19591 data and 508 / 508 parameters GooF = S = 1.045; Restrained GooF = 1.045 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1032 * P )^2 + 9.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20622 0.00027 0.000 OSF 2 0.34855 0.00082 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for z Cr1 Max. shift = 0.000 A for C41 Max. dU = 0.000 for C41 Least-squares cycle 12 Maximum vector length = 511 Memory required = 5304 / 673495 wR2 = 0.1887 before cycle 12 for 19591 data and 508 / 508 parameters GooF = S = 1.045; Restrained GooF = 1.045 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1032 * P )^2 + 9.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20622 0.00027 0.000 OSF 2 0.34855 0.00082 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H33A Max. dU = 0.000 for C29 Least-squares cycle 13 Maximum vector length = 511 Memory required = 5304 / 673495 wR2 = 0.1887 before cycle 13 for 19591 data and 508 / 508 parameters GooF = S = 1.045; Restrained GooF = 1.045 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1032 * P )^2 + 9.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20622 0.00027 0.000 OSF 2 0.34855 0.00082 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for z Cr1 Max. shift = 0.000 A for C15 Max. dU = 0.000 for C8 Least-squares cycle 14 Maximum vector length = 511 Memory required = 5304 / 673495 wR2 = 0.1887 before cycle 14 for 19591 data and 508 / 508 parameters GooF = S = 1.045; Restrained GooF = 1.045 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1032 * P )^2 + 9.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20622 0.00027 0.000 OSF 2 0.34855 0.00082 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for z Cr1 Max. shift = 0.000 A for N44 Max. dU = 0.000 for C34 Least-squares cycle 15 Maximum vector length = 511 Memory required = 5304 / 673495 wR2 = 0.1887 before cycle 15 for 19591 data and 508 / 508 parameters GooF = S = 1.045; Restrained GooF = 1.045 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1032 * P )^2 + 9.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.20622 0.00027 0.000 OSF 2 0.34855 0.00082 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for z Cr1 Max. shift = 0.000 A for C32 Max. dU = 0.000 for C28 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 16 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A -0.0979 0.0846 -0.3156 23 0.990 0.000 C1 C2 S1 H1B -0.0131 -0.0241 -0.2661 23 0.990 0.000 C1 C2 S1 H2A -0.2519 -0.0598 -0.2987 23 0.990 0.000 C2 C1 S2 H2B -0.3529 0.0812 -0.2788 23 0.990 0.000 C2 C1 S2 H9A -0.4045 0.2898 0.1608 23 0.990 0.000 C9 C10 S7 H9B -0.3545 0.1948 0.2169 23 0.990 0.000 C9 C10 S7 H10A -0.0804 0.1608 0.1922 23 0.990 0.000 C10 C9 S8 H10B -0.1736 0.3123 0.2040 23 0.990 0.000 C10 C9 S8 H11A 0.5123 0.8003 0.1922 23 0.990 0.000 C11 C12 S11 H11B 0.5844 0.7012 0.2457 23 0.990 0.000 C11 C12 S11 H12A 0.8127 0.5931 0.1942 23 0.990 0.000 C12 C11 S12 H12B 0.7998 0.7474 0.2023 23 0.990 0.000 C12 C11 S12 H21 0.0942 0.5804 0.3257 43 0.950 0.000 C21 N21 C22 H22 -0.0749 0.7508 0.3717 43 0.950 0.000 C22 C23 C21 H29 0.7139 0.0776 0.5251 43 0.950 0.000 C29 C28 C30 H30 0.6398 0.1045 0.4343 43 0.950 0.000 C30 N22 C29 H31 0.1325 0.6313 0.5498 43 0.950 0.000 C31 C32 C24 H32 0.3396 0.4557 0.5900 43 0.950 0.000 C32 C31 C27 H33A -0.1684 0.8466 0.4509 137 0.980 0.000 C33 C23 H33A H33B -0.0232 0.8431 0.4899 137 0.980 0.000 C33 C23 H33A H33C -0.1318 0.7419 0.5051 137 0.980 0.000 C33 C23 H33A H34A 0.4954 0.2061 0.6251 137 0.980 0.000 C34 C28 H34A H34B 0.6047 0.3081 0.6138 137 0.980 0.000 C34 C28 H34A H34C 0.6823 0.1478 0.6115 137 0.980 0.000 C34 C28 H34A s92 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq S1 -0.11437 0.18952 -0.23857 1.00000 0.03795 0.02701 0.01251 -0.00393 0.00819 -0.01503 0.02462 0.00242 0.00021 0.00015 0.00005 0.00000 0.00104 0.00090 0.00065 0.00058 0.00072 0.00075 0.00038 S2 -0.27825 -0.08771 -0.20522 1.00000 0.03585 0.02242 0.01649 -0.00620 0.00169 -0.01420 0.02338 0.00235 0.00020 0.00015 0.00006 0.00000 0.00102 0.00088 0.00070 0.00058 0.00072 0.00074 0.00037 S3 -0.26463 -0.02432 -0.09430 1.00000 0.03168 0.01894 0.01076 -0.00213 0.00140 -0.01197 0.01946 0.00222 0.00019 0.00014 0.00005 0.00000 0.00097 0.00083 0.00064 0.00054 0.00066 0.00069 0.00035 S4 -0.11639 0.19754 -0.12152 1.00000 0.02264 0.01792 0.01146 -0.00333 0.00114 -0.00835 0.01669 0.00217 0.00018 0.00014 0.00005 0.00000 0.00086 0.00079 0.00062 0.00053 0.00063 0.00065 0.00033 S5 -0.10872 0.23825 0.00409 1.00000 0.02715 0.01786 0.01300 -0.00240 -0.00066 -0.00829 0.01889 0.00222 0.00019 0.00014 0.00005 0.00000 0.00092 0.00082 0.00065 0.00054 0.00065 0.00068 0.00034 S6 -0.27880 0.03067 0.03017 1.00000 0.03597 0.02470 0.01130 -0.00239 0.00399 -0.01556 0.02259 0.00233 0.00020 0.00015 0.00006 0.00000 0.00103 0.00089 0.00065 0.00056 0.00070 0.00074 0.00037 S7 -0.31245 0.06082 0.14629 1.00000 0.05318 0.02327 0.01327 -0.00424 0.00988 -0.01327 0.02940 0.00257 0.00022 0.00015 0.00006 0.00000 0.00122 0.00092 0.00069 0.00059 0.00078 0.00079 0.00043 S8 -0.10718 0.31226 0.11292 1.00000 0.03513 0.02294 0.01827 -0.00699 -0.00277 -0.00887 0.02488 0.00237 0.00020 0.00015 0.00006 0.00000 0.00104 0.00090 0.00072 0.00060 0.00073 0.00074 0.00038 C1 -0.10958 0.05311 -0.27708 1.00000 0.03349 0.02804 0.00958 -0.00763 0.00428 -0.00956 0.02315 0.00865 0.00075 0.00057 0.00021 0.00000 0.00399 0.00355 0.00262 0.00231 0.00270 0.00296 0.00146 H1A -0.09790 0.08461 -0.31559 1.00000 0.02778 0.00000 0.00000 H1B -0.01310 -0.02409 -0.26606 1.00000 0.02778 0.00000 0.00000 C2 -0.25585 0.00225 -0.27114 1.00000 0.02831 0.04844 0.01140 -0.00436 0.00077 -0.02104 0.02722 0.00926 0.00077 0.00065 0.00022 0.00000 0.00395 0.00420 0.00276 0.00263 0.00283 0.00322 0.00152 H2A -0.25188 -0.05982 -0.29867 1.00000 0.03266 0.00000 0.00000 H2B -0.35292 0.08123 -0.27881 1.00000 0.03266 0.00000 0.00000 C3 -0.22530 0.01611 -0.16241 1.00000 0.01736 0.02432 0.00882 -0.00318 -0.00010 -0.00448 0.01704 0.00857 0.00069 0.00056 0.00020 0.00000 0.00330 0.00347 0.00247 0.00217 0.00245 0.00262 0.00129 C4 -0.15995 0.11863 -0.17486 1.00000 0.02201 0.01599 0.01424 -0.00551 0.00233 -0.00455 0.01732 0.00867 0.00070 0.00054 0.00021 0.00000 0.00353 0.00323 0.00269 0.00218 0.00260 0.00267 0.00133 C5 -0.18907 0.09950 -0.07141 1.00000 0.02230 0.01508 0.01936 -0.00131 0.00483 -0.01037 0.01801 0.00884 0.00070 0.00053 0.00022 0.00000 0.00346 0.00320 0.00283 0.00227 0.00272 0.00262 0.00131 C6 -0.19077 0.12028 -0.01849 1.00000 0.01984 0.01861 0.01588 -0.00131 -0.00027 -0.00700 0.01786 0.00860 0.00069 0.00053 0.00022 0.00000 0.00343 0.00325 0.00276 0.00220 0.00260 0.00264 0.00132 C7 -0.16552 0.20878 0.07161 1.00000 0.01854 0.01311 0.01146 -0.00429 0.00017 0.00721 0.01660 0.00882 0.00068 0.00053 0.00021 0.00000 0.00331 0.00316 0.00250 0.00208 0.00247 0.00254 0.00132 C8 -0.24230 0.11377 0.08348 1.00000 0.02746 0.02247 0.01323 0.00173 0.00656 -0.00658 0.02163 0.00931 0.00073 0.00056 0.00021 0.00000 0.00377 0.00350 0.00270 0.00229 0.00278 0.00288 0.00142 C9 -0.32110 0.21053 0.17905 1.00000 0.04244 0.01607 0.01776 -0.00809 0.00191 0.00099 0.02690 0.00935 0.00080 0.00055 0.00023 0.00000 0.00438 0.00340 0.00291 0.00237 0.00306 0.00294 0.00158 H9A -0.40452 0.28975 0.16078 1.00000 0.03227 0.00000 0.00000 H9B -0.35447 0.19479 0.21687 1.00000 0.03227 0.00000 0.00000 C10 -0.16642 0.24433 0.17863 1.00000 0.03278 0.03353 0.01335 -0.00489 -0.00557 -0.00491 0.02725 0.00949 0.00078 0.00061 0.00022 0.00000 0.00402 0.00386 0.00280 0.00251 0.00292 0.00316 0.00154 H10A -0.08043 0.16079 0.19217 1.00000 0.03269 0.00000 0.00000 H10B -0.17356 0.31225 0.20401 1.00000 0.03269 0.00000 0.00000 S11 0.48617 0.58369 0.18763 1.00000 0.02220 0.02410 0.01174 -0.00480 0.00224 -0.00891 0.01868 0.00226 0.00018 0.00014 0.00005 0.00000 0.00085 0.00085 0.00065 0.00056 0.00064 0.00067 0.00034 S12 0.75424 0.73268 0.11219 1.00000 0.03252 0.03055 0.01685 -0.00267 0.00064 -0.01859 0.02466 0.00238 0.00020 0.00015 0.00006 0.00000 0.00100 0.00094 0.00072 0.00061 0.00073 0.00075 0.00037 S13 0.64254 0.63184 0.02061 1.00000 0.03078 0.03787 0.01287 -0.00546 0.00602 -0.01788 0.02537 0.00245 0.00020 0.00016 0.00006 0.00000 0.00100 0.00101 0.00068 0.00061 0.00069 0.00079 0.00039 S14 0.41429 0.50741 0.08295 1.00000 0.02197 0.02572 0.01217 -0.00607 0.00357 -0.01068 0.01887 0.00221 0.00018 0.00014 0.00005 0.00000 0.00085 0.00088 0.00063 0.00056 0.00064 0.00067 0.00034 C11 0.58021 0.70756 0.20595 1.00000 0.02586 0.02001 0.01779 -0.00738 -0.00118 -0.00073 0.02198 0.00864 0.00069 0.00054 0.00022 0.00000 0.00373 0.00344 0.00280 0.00234 0.00278 0.00279 0.00144 H11A 0.51226 0.80027 0.19223 1.00000 0.02638 0.00000 0.00000 H11B 0.58441 0.70123 0.24572 1.00000 0.02638 0.00000 0.00000 C12 0.74848 0.68940 0.18456 1.00000 0.02466 0.02901 0.01002 -0.00637 -0.00317 -0.00679 0.02101 0.00881 0.00070 0.00058 0.00020 0.00000 0.00363 0.00362 0.00255 0.00235 0.00266 0.00280 0.00139 H12A 0.81267 0.59309 0.19420 1.00000 0.02522 0.00000 0.00000 H12B 0.79975 0.74744 0.20233 1.00000 0.02522 0.00000 0.00000 C13 0.62430 0.64907 0.09052 1.00000 0.02158 0.01776 0.01220 -0.00388 0.00210 -0.00124 0.01796 0.00858 0.00068 0.00052 0.00020 0.00000 0.00351 0.00327 0.00260 0.00220 0.00260 0.00262 0.00133 C14 0.52253 0.59192 0.11834 1.00000 0.01639 0.01534 0.01168 -0.00676 0.00664 -0.00418 0.01421 0.00836 0.00066 0.00050 0.00020 0.00000 0.00328 0.00315 0.00252 0.00211 0.00242 0.00250 0.00124 C15 0.51307 0.52923 0.02174 1.00000 0.01262 0.01980 0.02057 -0.00664 0.00366 -0.00616 0.01703 0.00798 0.00067 0.00053 0.00022 0.00000 0.00311 0.00327 0.00288 0.00233 0.00265 0.00255 0.00130 Cr1 0.37664 0.31261 0.35585 1.00000 0.01567 0.01951 0.00911 -0.00306 0.00335 -0.00699 0.01429 0.00137 0.00011 0.00008 0.00003 0.00000 0.00051 0.00051 0.00040 0.00035 0.00040 0.00039 0.00021 S41 -0.01681 0.07487 0.40233 1.00000 0.02809 0.03194 0.02904 -0.00822 0.01170 -0.02102 0.02688 0.00247 0.00020 0.00016 0.00006 0.00000 0.00096 0.00097 0.00085 0.00066 0.00078 0.00077 0.00039 S42 0.14352 0.46308 0.18044 1.00000 0.02849 0.02845 0.01301 0.00278 -0.00223 -0.01087 0.02318 0.00243 0.00020 0.00015 0.00006 0.00000 0.00097 0.00090 0.00067 0.00059 0.00069 0.00074 0.00037 S43 0.83979 0.44174 0.30412 1.00000 0.01923 0.04751 0.02338 0.00253 0.00321 -0.01822 0.02888 0.00260 0.00020 0.00016 0.00006 0.00000 0.00091 0.00109 0.00079 0.00070 0.00072 0.00078 0.00040 S44 0.70852 -0.09112 0.29153 1.00000 0.02266 0.02353 0.02242 -0.00937 -0.00062 0.00070 0.02382 0.00242 0.00019 0.00015 0.00006 0.00000 0.00091 0.00090 0.00074 0.00061 0.00070 0.00069 0.00037 N21 0.23117 0.48044 0.38783 1.00000 0.01513 0.01444 0.01180 0.00087 0.00181 -0.00926 0.01298 0.00687 0.00054 0.00042 0.00017 0.00000 0.00274 0.00261 0.00212 0.00176 0.00206 0.00211 0.00103 N22 0.46513 0.27491 0.43464 1.00000 0.00787 0.01306 0.01458 -0.00253 -0.00138 -0.00102 0.01215 0.00663 0.00051 0.00041 0.00017 0.00000 0.00244 0.00256 0.00220 0.00176 0.00200 0.00197 0.00100 N41 0.21438 0.21390 0.38060 1.00000 0.01396 0.01663 0.01581 -0.00295 0.00135 -0.00971 0.01428 0.00700 0.00055 0.00043 0.00017 0.00000 0.00272 0.00269 0.00232 0.00184 0.00211 0.00220 0.00103 N42 0.27426 0.36736 0.28365 1.00000 0.02424 0.02812 0.00733 -0.00356 0.00078 -0.01010 0.01924 0.00716 0.00059 0.00046 0.00017 0.00000 0.00309 0.00290 0.00220 0.00187 0.00217 0.00228 0.00116 N43 0.54059 0.40844 0.33566 1.00000 0.01902 0.02248 0.01920 -0.00524 0.00656 -0.01099 0.01904 0.00720 0.00059 0.00045 0.00018 0.00000 0.00295 0.00285 0.00253 0.00196 0.00232 0.00226 0.00113 N44 0.52471 0.13978 0.33544 1.00000 0.02313 0.02382 0.01622 -0.00766 0.00445 -0.00860 0.02027 0.00716 0.00058 0.00047 0.00018 0.00000 0.00295 0.00300 0.00240 0.00203 0.00226 0.00234 0.00115 C21 0.11169 0.57874 0.36318 1.00000 0.01188 0.01423 0.01411 0.00141 0.00221 -0.00650 0.01314 0.00831 0.00062 0.00050 0.00021 0.00000 0.00307 0.00307 0.00256 0.00211 0.00244 0.00240 0.00121 H21 0.09421 0.58040 0.32573 1.00000 0.01577 0.00000 0.00000 C22 0.00919 0.68143 0.39083 1.00000 0.02229 0.01552 0.01920 -0.00096 -0.00669 -0.00224 0.01966 0.00870 0.00072 0.00054 0.00022 0.00000 0.00355 0.00331 0.00288 0.00228 0.00272 0.00266 0.00138 H22 -0.07493 0.75083 0.37169 1.00000 0.02359 0.00000 0.00000 C23 0.02987 0.68204 0.44526 1.00000 0.01761 0.01133 0.02309 -0.00474 0.00733 -0.01260 0.01545 0.00849 0.00069 0.00051 0.00022 0.00000 0.00330 0.00312 0.00295 0.00222 0.00266 0.00250 0.00128 C24 0.15939 0.57722 0.47226 1.00000 0.01529 0.01570 0.00963 0.00072 0.00159 -0.00702 0.01322 0.00838 0.00066 0.00052 0.00020 0.00000 0.00320 0.00315 0.00252 0.00206 0.00242 0.00250 0.00124 C25 0.25323 0.47942 0.44190 1.00000 0.01468 0.01574 0.01038 -0.00149 0.00223 -0.01006 0.01245 0.00831 0.00067 0.00052 0.00020 0.00000 0.00314 0.00308 0.00250 0.00201 0.00237 0.00245 0.00121 C26 0.38331 0.36768 0.46699 1.00000 0.01721 0.01187 0.01232 -0.00394 0.00220 -0.00661 0.01310 0.00826 0.00068 0.00051 0.00020 0.00000 0.00336 0.00311 0.00253 0.00206 0.00245 0.00251 0.00127 C27 0.41709 0.35831 0.52202 1.00000 0.01219 0.01881 0.01382 0.00216 0.00079 -0.00911 0.01434 0.00852 0.00066 0.00053 0.00021 0.00000 0.00314 0.00327 0.00263 0.00217 0.00246 0.00252 0.00125 C28 0.54313 0.24455 0.54462 1.00000 0.01839 0.02022 0.01197 0.00482 -0.00400 -0.01306 0.01581 0.00868 0.00071 0.00055 0.00021 0.00000 0.00339 0.00332 0.00259 0.00219 0.00257 0.00265 0.00130 C29 0.62646 0.15295 0.51119 1.00000 0.01607 0.01960 0.02461 0.00208 -0.00459 -0.00173 0.02114 0.00887 0.00071 0.00056 0.00023 0.00000 0.00344 0.00343 0.00311 0.00241 0.00282 0.00267 0.00140 H29 0.71385 0.07763 0.52506 1.00000 0.02537 0.00000 0.00000 C30 0.58254 0.17055 0.45646 1.00000 0.01498 0.01690 0.02442 -0.00537 0.00035 -0.00191 0.01908 0.00894 0.00069 0.00054 0.00023 0.00000 0.00344 0.00350 0.00306 0.00245 0.00281 0.00271 0.00142 H30 0.63980 0.10453 0.43429 1.00000 0.02289 0.00000 0.00000 C31 0.19556 0.56519 0.52871 1.00000 0.02504 0.01860 0.01506 -0.00779 0.00365 -0.01105 0.01811 0.00850 0.00072 0.00056 0.00021 0.00000 0.00360 0.00330 0.00271 0.00226 0.00272 0.00271 0.00134 H31 0.13249 0.63129 0.54983 1.00000 0.02174 0.00000 0.00000 C32 0.31845 0.46092 0.55257 1.00000 0.02440 0.02886 0.00489 0.00025 -0.00036 -0.01347 0.01835 0.00850 0.00069 0.00054 0.00020 0.00000 0.00362 0.00357 0.00243 0.00217 0.00244 0.00281 0.00135 H32 0.33957 0.45568 0.58998 1.00000 0.02202 0.00000 0.00000 C33 -0.08325 0.78764 0.47542 1.00000 0.02581 0.01979 0.01733 -0.00254 0.00976 -0.00853 0.02070 0.00912 0.00070 0.00052 0.00021 0.00000 0.00369 0.00345 0.00280 0.00230 0.00276 0.00280 0.00142 H33A -0.16837 0.84661 0.45088 1.00000 0.03105 0.00000 0.00000 H33B -0.02318 0.84312 0.48994 1.00000 0.03105 0.00000 0.00000 H33C -0.13182 0.74190 0.50508 1.00000 0.03105 0.00000 0.00000 C34 0.58506 0.22490 0.60396 1.00000 0.02625 0.03642 0.00989 -0.00022 -0.00332 -0.01054 0.02403 0.00887 0.00072 0.00058 0.00020 0.00000 0.00388 0.00384 0.00264 0.00240 0.00267 0.00302 0.00149 H34A 0.49535 0.20609 0.62508 1.00000 0.03605 0.00000 0.00000 H34B 0.60467 0.30806 0.61380 1.00000 0.03605 0.00000 0.00000 H34C 0.68233 0.14783 0.61148 1.00000 0.03605 0.00000 0.00000 C41 0.11691 0.15699 0.38890 1.00000 0.01863 0.00970 0.01591 -0.00237 0.00136 0.00490 0.01658 0.00927 0.00072 0.00052 0.00021 0.00000 0.00346 0.00313 0.00266 0.00217 0.00262 0.00263 0.00132 C42 0.22009 0.40815 0.24087 1.00000 0.01595 0.01512 0.02122 -0.00647 0.00812 -0.00740 0.01657 0.00882 0.00068 0.00052 0.00022 0.00000 0.00333 0.00314 0.00295 0.00229 0.00272 0.00255 0.00130 C43 0.66580 0.42150 0.32209 1.00000 0.02992 0.01037 0.01404 -0.00206 -0.00497 -0.00596 0.01793 0.00869 0.00076 0.00052 0.00021 0.00000 0.00398 0.00316 0.00269 0.00214 0.00282 0.00279 0.00138 C44 0.60134 0.04354 0.31761 1.00000 0.01467 0.02755 0.01081 0.00485 0.00385 -0.01046 0.01745 0.00890 0.00067 0.00058 0.00021 0.00000 0.00340 0.00368 0.00255 0.00230 0.00254 0.00278 0.00134 Final Structure Factor Calculation for s92 in P-1 Total number of l.s. parameters = 508 Maximum vector length = 511 Memory required = 4796 / 24017 wR2 = 0.1887 before cycle 16 for 19591 data and 0 / 508 parameters GooF = S = 1.045; Restrained GooF = 1.045 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1032 * P )^2 + 9.71 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0684 for 15040 Fo > 4sig(Fo) and 0.0992 for all 19591 data wR2 = 0.1887, GooF = S = 1.045, Restrained GooF = 1.045 for all data Occupancy sum of asymmetric unit = 56.00 for non-hydrogen and 24.00 for hydrogen atoms Principal mean square atomic displacements U 0.0407 0.0230 0.0101 S1 0.0369 0.0202 0.0131 S2 0.0323 0.0155 0.0107 S3 0.0233 0.0159 0.0109 S4 0.0273 0.0168 0.0126 S5 0.0379 0.0192 0.0106 S6 0.0555 0.0217 0.0110 S7 0.0360 0.0251 0.0135 S8 0.0341 0.0281 0.0073 C1 0.0505 0.0201 0.0111 C2 0.0253 0.0173 0.0085 C3 0.0228 0.0184 0.0108 C4 0.0258 0.0187 0.0096 C5 0.0207 0.0171 0.0157 C6 0.0326 0.0120 0.0052 C7 0.0320 0.0234 0.0094 C8 0.0493 0.0219 0.0095 C9 0.0405 0.0301 0.0111 C10 0.0255 0.0198 0.0108 S11 0.0391 0.0181 0.0168 S12 0.0416 0.0234 0.0111 S13 0.0280 0.0181 0.0105 S14 0.0328 0.0202 0.0129 C11 0.0304 0.0252 0.0074 C12 0.0263 0.0169 0.0106 C13 0.0210 0.0161 0.0055 C14 0.0242 0.0157 0.0111 C15 0.0201 0.0150 0.0078 Cr1 0.0446 0.0252 0.0108 S41 0.0325 0.0251 0.0119 S42 0.0506 0.0249 0.0112 S43 0.0354 0.0217 0.0144 S44 0.0188 0.0138 0.0063 N21 0.0160 0.0130 0.0075 N22 0.0198 0.0154 0.0076 N41 0.0288 0.0219 0.0070 N42 0.0277 0.0180 0.0115 N43 0.0274 0.0208 0.0126 N44 0.0178 0.0145 0.0071 C21 0.0288 0.0172 0.0129 C22 0.0286 0.0158 0.0020 C23 0.0177 0.0141 0.0079 C24 0.0197 0.0109 0.0067 C25 0.0184 0.0121 0.0088 C26 0.0222 0.0139 0.0069 C27 0.0292 0.0102 0.0080 C28 0.0283 0.0227 0.0125 C29 0.0253 0.0186 0.0133 C30 0.0280 0.0168 0.0095 C31 0.0320 0.0181 0.0049 C32 0.0320 0.0195 0.0106 C33 0.0371 0.0258 0.0092 C34 0.0280 0.0159 0.0058 C41 0.0273 0.0125 0.0100 C42 0.0318 0.0129 0.0090 C43 0.0312 0.0168 0.0043 C44 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.026 0.041 0.055 0.071 0.088 0.108 0.133 0.165 0.223 1.000 Number in group 2021. 1910. 2004. 1982. 1924. 1936. 1949. 1950. 1953. 1962. GooF 1.088 1.022 1.027 1.026 1.012 0.988 1.066 1.062 0.967 1.178 K 1.920 1.097 1.000 0.993 1.006 1.008 1.009 1.012 1.014 1.013 Resolution(A) 0.77 0.82 0.88 0.95 1.04 1.16 1.31 1.50 1.80 2.35 inf Number in group 1967. 1984. 1927. 1952. 2005. 1946. 1919. 1970. 1957. 1964. GooF 1.098 1.057 1.021 1.037 0.977 0.976 1.040 1.003 1.144 1.090 K 1.021 1.019 1.019 1.031 1.018 1.013 1.003 1.010 1.034 1.000 R1 0.239 0.182 0.148 0.115 0.091 0.067 0.066 0.061 0.060 0.056 Recommended weighting scheme: WGHT 0.1031 9.7212 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 3 4 404.20 11405.23 12.62 0.382 2.64 1 5 4 12.93 4828.05 12.38 0.249 2.01 0 5 -1 441.59 4352.55 10.54 0.236 1.93 -1 3 3 826.27 6368.07 10.49 0.286 2.72 -1 3 1 -6.58 1087.48 9.40 0.118 2.79 -1 6 -2 1259.87 6229.93 9.28 0.283 1.49 1 7 11 325.90 1762.90 7.91 0.150 1.29 2 8 5 513.78 1985.73 7.17 0.160 1.28 -2 4 4 583.38 2065.32 6.99 0.163 1.85 2 -4 0 447.47 1658.34 6.84 0.146 1.88 2 -4 25 887.41 50.31 6.68 0.025 0.84 -8 -2 -9 679.08 8.43 6.61 0.010 1.01 0 -1 -12 477.09 58.55 6.42 0.027 2.08 2 8 -1 207.63 1262.33 6.40 0.127 1.27 0 -2 -7 329.19 37.86 6.29 0.022 3.06 -2 -8 -2 1230.01 440.85 6.28 0.075 1.29 1 3 7 430.77 14.05 6.02 0.013 2.61 1 7 10 258.42 1073.97 6.01 0.117 1.33 -1 -1 18 741.39 2282.70 5.95 0.171 1.34 3 0 8 748.91 226.23 5.88 0.054 2.05 0 6 10 293.69 994.16 5.75 0.113 1.45 -5 -5 5 337.89 24.62 5.71 0.018 1.40 1 -1 9 724.69 232.84 5.71 0.055 2.40 -1 -7 -4 62.78 446.29 5.44 0.076 1.45 0 -4 3 323.08 980.97 5.43 0.112 2.27 0 5 8 11.52 290.05 5.38 0.061 1.76 1 5 5 1.65 252.75 5.28 0.057 1.98 1 -2 7 1056.71 441.34 5.26 0.075 2.46 -3 8 7 -17.17 740.41 5.21 0.097 1.01 -1 -1 10 356.00 63.81 5.18 0.029 2.30 -2 4 3 129.56 537.88 5.10 0.083 1.88 6 5 -10 769.37 209.83 5.06 0.052 1.13 -2 -4 -17 310.85 2.05 5.04 0.005 1.32 -2 -4 5 238.90 14.35 4.97 0.014 2.09 4 10 23 -93.82 995.35 4.95 0.113 0.78 -1 2 14 272.05 2.62 4.90 0.006 1.67 -2 -3 -9 464.63 134.69 4.88 0.042 2.15 2 7 3 680.02 1616.17 4.86 0.144 1.47 1 -4 4 35.04 291.43 4.83 0.061 1.99 4 9 18 47.97 686.50 4.80 0.094 0.91 6 1 3 396.44 71.86 4.76 0.030 1.41 0 1 12 407.73 109.43 4.75 0.037 2.08 6 2 25 511.42 1675.43 4.70 0.147 0.83 0 2 9 2318.22 1256.88 4.64 0.127 2.54 2 1 -16 392.44 50.62 4.64 0.025 1.44 -3 5 -22 36.68 858.87 4.64 0.105 0.84 6 -5 2 346.59 1.05 4.64 0.004 0.99 4 5 9 -14.34 499.26 4.63 0.080 1.50 -1 5 8 419.96 1003.62 4.55 0.113 1.64 -2 -1 16 361.64 50.62 4.53 0.025 1.44 Bond lengths and angles S1 - Distance Angles C4 1.7531 (0.0055) C1 1.7902 (0.0053) 100.23 (0.26) S1 - C4 S2 - Distance Angles C3 1.7581 (0.0056) C2 1.8226 (0.0057) 101.08 (0.27) S2 - C3 S3 - Distance Angles C5 1.7494 (0.0057) C3 1.7518 (0.0052) 95.31 (0.27) S3 - C5 S4 - Distance Angles C5 1.7311 (0.0055) C4 1.7476 (0.0054) 95.88 (0.27) S4 - C5 S5 - Distance Angles C6 1.7279 (0.0057) C7 1.7620 (0.0053) 94.91 (0.28) S5 - C6 S6 - Distance Angles C6 1.7299 (0.0056) C8 1.7525 (0.0058) 95.38 (0.26) S6 - C6 S7 - Distance Angles C8 1.7507 (0.0055) C9 1.8163 (0.0054) 98.46 (0.28) S7 - C8 S8 - Distance Angles C7 1.7514 (0.0057) C10 1.8256 (0.0059) 100.31 (0.28) S8 - C7 C1 - Distance Angles C2 1.5006 (0.0079) S1 1.7902 (0.0053) 114.44 (0.40) H1A 0.9900 108.65 108.65 H1B 0.9900 108.65 108.65 107.59 C1 - C2 S1 H1A C2 - Distance Angles C1 1.5006 (0.0079) S2 1.8226 (0.0057) 115.21 (0.41) H2A 0.9900 108.47 108.47 H2B 0.9900 108.47 108.47 107.49 C2 - C1 S2 H2A C3 - Distance Angles C4 1.3355 (0.0076) S3 1.7518 (0.0052) 117.13 (0.41) S2 1.7581 (0.0056) 128.99 (0.42) 113.88 (0.33) C3 - C4 S3 C4 - Distance Angles C3 1.3355 (0.0076) S4 1.7476 (0.0054) 117.05 (0.41) S1 1.7531 (0.0054) 128.73 (0.43) 114.21 (0.32) C4 - C3 S4 C5 - Distance Angles C6 1.3664 (0.0072) S4 1.7311 (0.0055) 122.33 (0.45) S3 1.7494 (0.0057) 123.03 (0.45) 114.62 (0.31) C5 - C6 S4 C6 - Distance Angles C5 1.3664 (0.0072) S5 1.7279 (0.0057) 122.67 (0.46) S6 1.7299 (0.0056) 121.59 (0.46) 115.73 (0.31) C6 - C5 S5 C7 - Distance Angles C8 1.3336 (0.0076) S8 1.7514 (0.0057) 130.47 (0.44) S5 1.7620 (0.0053) 117.17 (0.42) 112.35 (0.34) C7 - C8 S8 C8 - Distance Angles C7 1.3336 (0.0076) S7 1.7507 (0.0055) 127.97 (0.45) S6 1.7525 (0.0058) 116.79 (0.42) 115.24 (0.34) C8 - C7 S7 C9 - Distance Angles C10 1.4765 (0.0083) S7 1.8163 (0.0054) 113.59 (0.41) H9A 0.9900 108.85 108.85 H9B 0.9900 108.85 108.85 107.70 C9 - C10 S7 H9A C10 - Distance Angles C9 1.4765 (0.0083) S8 1.8256 (0.0059) 115.06 (0.42) H10A 0.9900 108.51 108.51 H10B 0.9900 108.51 108.51 107.51 C10 - C9 S8 H10A S11 - Distance Angles C14 1.7502 (0.0051) C11 1.8055 (0.0058) 100.89 (0.27) S11 - C14 S12 - Distance Angles C13 1.7329 (0.0060) C12 1.8128 (0.0052) 100.99 (0.28) S12 - C13 S13 - Distance Angles C15 1.7447 (0.0055) C13 1.7788 (0.0051) 94.59 (0.27) S13 - C15 S14 - Distance Angles C15 1.7572 (0.0055) C14 1.7664 (0.0056) 94.50 (0.25) S14 - C15 C11 - Distance Angles C12 1.5078 (0.0075) S11 1.8055 (0.0058) 113.87 (0.37) H11A 0.9900 108.78 108.78 H11B 0.9900 108.78 108.78 107.67 C11 - C12 S11 H11A C12 - Distance Angles C11 1.5078 (0.0075) S12 1.8128 (0.0052) 113.49 (0.39) H12A 0.9900 108.87 108.87 H12B 0.9900 108.87 108.87 107.71 C12 - C11 S12 H12A C13 - Distance Angles C14 1.3314 (0.0074) S12 1.7329 (0.0060) 130.09 (0.42) S13 1.7788 (0.0051) 117.15 (0.43) 112.66 (0.32) C13 - C14 S12 C14 - Distance Angles C13 1.3314 (0.0074) S11 1.7502 (0.0051) 127.89 (0.44) S14 1.7664 (0.0056) 117.67 (0.40) 114.39 (0.31) C14 - C13 S11 C15 - Distance Angles C15_$1 1.3602 (0.0101) S13 1.7447 (0.0055) 122.99 (0.59) S14 1.7572 (0.0055) 121.39 (0.59) 115.62 (0.29) C15 - C15_$1 S13 Cr1 - Distance Angles N43 1.9718 (0.0050) N42 1.9758 (0.0045) 91.76 (0.20) N44 1.9883 (0.0045) 90.36 (0.20) 93.44 (0.19) N41 2.0024 (0.0048) 176.82 (0.19) 91.36 (0.19) 90.01 (0.18) N21 2.0632 (0.0042) 91.49 (0.18) 94.15 (0.18) 172.13 (0.18) 87.72 (0.18) N22 2.0818 (0.0043) 88.70 (0.18) 173.36 (0.18) 93.19 (0.17) 88.13 (0.18) 79.22 (0.17) Cr1 - N43 N42 N44 N41 N21 S41 - Distance Angles C41 1.6248 (0.0065) S41 - S42 - Distance Angles C42 1.6326 (0.0058) S42 - S43 - Distance Angles C43 1.6242 (0.0066) S43 - S44 - Distance Angles C44 1.6326 (0.0057) S44 - N21 - Distance Angles C21 1.3221 (0.0060) C25 1.3690 (0.0063) 117.97 (0.45) Cr1 2.0632 (0.0042) 127.08 (0.36) 114.59 (0.34) N21 - C21 C25 N22 - Distance Angles C30 1.3185 (0.0063) C26 1.3583 (0.0060) 117.94 (0.46) Cr1 2.0818 (0.0043) 128.00 (0.36) 113.96 (0.33) N22 - C30 C26 N41 - Distance Angles C41 1.1590 (0.0069) Cr1 2.0024 (0.0048) 172.37 (0.45) N41 - C41 N42 - Distance Angles C42 1.1579 (0.0069) Cr1 1.9758 (0.0045) 174.35 (0.51) N42 - C42 N43 - Distance Angles C43 1.1672 (0.0070) Cr1 1.9718 (0.0050) 157.67 (0.42) N43 - C43 N44 - Distance Angles C44 1.1572 (0.0060) Cr1 1.9883 (0.0045) 171.73 (0.44) N44 - C44 C21 - Distance Angles N21 1.3221 (0.0060) C22 1.4130 (0.0068) 122.02 (0.48) H21 0.9500 118.99 118.99 C21 - N21 C22 C22 - Distance Angles C23 1.3789 (0.0072) C21 1.4130 (0.0068) 120.76 (0.51) H22 0.9500 119.62 119.62 C22 - C23 C21 C23 - Distance Angles C22 1.3789 (0.0072) C24 1.4274 (0.0072) 117.79 (0.48) C33 1.5058 (0.0067) 121.02 (0.51) 121.17 (0.48) C23 - C22 C24 C24 - Distance Angles C25 1.3934 (0.0067) C23 1.4274 (0.0072) 117.48 (0.47) C31 1.4366 (0.0066) 118.56 (0.48) 123.94 (0.48) C24 - C25 C23 C25 - Distance Angles N21 1.3690 (0.0063) C24 1.3934 (0.0067) 123.95 (0.48) C26 1.4473 (0.0071) 115.55 (0.44) 120.50 (0.47) C25 - N21 C24 C26 - Distance Angles N22 1.3583 (0.0060) C27 1.4005 (0.0068) 123.56 (0.47) C25 1.4473 (0.0071) 116.42 (0.46) 120.01 (0.45) C26 - N22 C27 C27 - Distance Angles C26 1.4005 (0.0068) C28 1.4184 (0.0072) 117.41 (0.47) C32 1.4423 (0.0070) 118.45 (0.46) 124.09 (0.48) C27 - C26 C28 C28 - Distance Angles C29 1.3732 (0.0072) C27 1.4184 (0.0072) 118.30 (0.49) C34 1.5119 (0.0067) 120.85 (0.49) 120.85 (0.49) C28 - C29 C27 C29 - Distance Angles C28 1.3732 (0.0072) C30 1.4058 (0.0074) 120.06 (0.50) H29 0.9500 119.97 119.97 C29 - C28 C30 C30 - Distance Angles N22 1.3185 (0.0063) C29 1.4058 (0.0074) 122.70 (0.50) H30 0.9500 118.65 118.65 C30 - N22 C29 C31 - Distance Angles C32 1.3618 (0.0073) C24 1.4366 (0.0066) 121.32 (0.50) H31 0.9500 119.34 119.34 C31 - C32 C24 C32 - Distance Angles C31 1.3618 (0.0073) C27 1.4423 (0.0070) 121.16 (0.48) H32 0.9500 119.42 119.42 C32 - C31 C27 C33 - Distance Angles C23 1.5058 (0.0067) H33A 0.9800 109.47 H33B 0.9800 109.47 109.47 H33C 0.9800 109.47 109.47 109.47 C33 - C23 H33A H33B C34 - Distance Angles C28 1.5119 (0.0067) H34A 0.9800 109.47 H34B 0.9800 109.47 109.47 H34C 0.9800 109.47 109.47 109.47 C34 - C28 H34A H34B C41 - Distance Angles N41 1.1590 (0.0069) S41 1.6248 (0.0065) 178.18 (0.54) C41 - N41 C42 - Distance Angles N42 1.1579 (0.0069) S42 1.6326 (0.0057) 179.03 (0.55) C42 - N42 C43 - Distance Angles N43 1.1672 (0.0070) S43 1.6242 (0.0066) 178.84 (0.52) C43 - N43 C44 - Distance Angles N44 1.1572 (0.0060) S44 1.6326 (0.0057) 179.13 (0.51) C44 - N44 FMAP and GRID set by program FMAP 2 1 43 GRID -2.500 -2 -1 2.500 2 1 R1 = 0.0930 for 7758 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.65 at 0.3656 0.4014 0.1113 [ 1.39 A from S14 ] Deepest hole -0.81 at 0.7051 -0.0017 0.0792 [ 1.24 A from S6 ] Mean = 0.00, Rms deviation from mean = 0.15 e/A^3, Highest memory used = 4892 / 66717 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3656 0.4014 0.1113 1.00000 0.05 0.65 1.39 S14 2.29 H9A 2.55 S42 2.71 C14 Q2 1 0.8747 0.4408 0.3173 1.00000 0.05 0.62 0.45 S43 1.88 C43 2.72 H21 3.02 N43 Q3 1 -0.4237 -0.0196 0.0294 1.00000 0.05 0.60 1.49 S6 2.83 C8 2.95 C6 3.04 S6 Q4 1 0.4077 0.3962 0.3656 1.00000 0.05 0.60 1.03 CR1 1.39 N43 1.65 N21 1.98 N22 Q5 1 -0.4289 0.0620 0.0318 1.00000 0.05 0.59 1.25 S6 2.31 C8 2.57 C6 3.06 S7 Q6 1 0.6652 0.0604 0.6327 1.00000 0.05 0.58 1.03 H34C 1.71 C34 1.77 H34A 2.00 H2A Q7 1 0.5034 0.3159 0.3609 1.00000 0.05 0.58 1.12 CR1 1.19 N43 1.88 N22 1.95 N44 Q8 1 -0.0951 -0.1818 -0.2272 1.00000 0.05 0.57 1.72 S2 1.85 H10A 2.08 H1B 2.18 C2 Q9 1 0.6786 0.6395 0.0396 1.00000 0.05 0.57 0.60 S13 1.35 C13 2.15 C15 2.35 S12 Q10 1 -0.3298 0.0150 0.0100 1.00000 0.05 0.57 0.74 S6 1.91 C6 2.44 C8 2.54 C5 Shortest distances between peaks (including symmetry equivalents) 3 5 0.84 4 7 1.01 5 10 1.04 3 10 1.06 3 3 1.92 3 5 2.18 3 10 2.36 5 5 2.68 5 10 2.71 Time profile in seconds ----------------------- 0.19: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.02: 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. 3.25: 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 0.03: Generate idealized H-atoms 73.81: Structure factors and derivatives 163.47: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.05: Apply other restraints 7.58: Solve l.s. equations 0.00: Generate HTAB table 0.08: Other dependent quantities, CIF, tables 0.56: Analysis of variance 0.22: Merge reflections for Fourier and .fcf 0.30: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 13:30:42 Total CPU time: 249.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++