+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 15:59:04 on 13-Mar-2002 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 02SRC110 in P2(1) CELL 0.71073 9.2892 9.6862 16.7860 90.000 92.111 90.000 ZERR 2.00 0.0002 0.0002 0.0006 0.000 0.001 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N O F P S PD UNIT 56 90 2 6 6 2 2 2 V = 1509.33 F(000) = 696.0 Mu = 0.78 mm-1 Cell Wt = 1340.16 Rho = 1.474 MERG 2 OMIT -3.00 55.00 OMIT 3 -7 5 OMIT 3 -8 7 OMIT 4 -8 6 EXTI 0.00274 FMAP 2 PLAN 10 SIZE 0.02 0.05 0.28 ACTA BOND $H WGHT 0.04090 L.S. 4 TEMP -153.00 FVAR 0.27174 C1 1 1.011813 0.710098 0.762676 11.00000 0.03686 0.02839 = 0.08984 0.00032 -0.03336 -0.00143 C2 1 0.840168 0.505486 0.540978 11.00000 0.07012 0.05233 = 0.03768 0.02724 0.00154 -0.01259 AFIX 137 H2A 2 0.920899 0.549036 0.570619 11.00000 -1.50000 H2B 2 0.749303 0.544887 0.558269 11.00000 -1.50000 H2C 2 0.849405 0.522143 0.483808 11.00000 -1.50000 AFIX 0 C3 1 0.984818 0.299049 0.538857 11.00000 0.01892 0.07410 = 0.02746 -0.00938 0.01056 -0.00020 AFIX 137 H3A 2 1.004724 0.315364 0.482706 11.00000 -1.50000 H3B 2 0.985843 0.199574 0.549522 11.00000 -1.50000 H3C 2 1.058744 0.344465 0.572772 11.00000 -1.50000 AFIX 0 C4 1 0.728749 0.289892 0.503622 11.00000 0.02539 0.06151 = 0.01410 0.00021 0.00134 -0.00432 AFIX 23 H4A 2 0.761847 0.284245 0.448326 11.00000 -1.20000 H4B 2 0.638931 0.344932 0.503377 11.00000 -1.20000 AFIX 0 C5 1 0.702011 0.148175 0.535369 11.00000 0.01427 0.04669 = 0.01984 -0.00654 0.00511 0.00189 C6 1 0.671671 0.034456 0.486301 11.00000 0.02124 0.06140 = 0.01814 -0.00807 -0.00207 0.00132 AFIX 43 H6 2 0.664206 0.045569 0.430071 11.00000 -1.20000 AFIX 0 C7 1 0.652710 -0.093292 0.519666 11.00000 0.02174 0.05199 = 0.03139 -0.02226 0.00093 -0.00013 AFIX 43 H7 2 0.631895 -0.170412 0.486225 11.00000 -1.20000 AFIX 0 C8 1 0.663526 -0.111003 0.601182 11.00000 0.02474 0.03165 = 0.03612 -0.01623 0.00141 0.00210 AFIX 43 H8 2 0.651426 -0.199912 0.623872 11.00000 -1.20000 AFIX 0 C9 1 0.692543 0.003485 0.650184 11.00000 0.02260 0.02031 = 0.02363 -0.00819 -0.00238 0.00356 AFIX 43 H9 2 0.700498 -0.008872 0.706318 11.00000 -1.20000 AFIX 0 C10 1 0.709907 0.134414 0.618583 11.00000 0.01364 0.02610 = 0.01735 -0.00023 0.00013 0.00186 C11 1 0.610321 0.457054 0.820149 11.00000 0.01923 0.01853 = 0.01575 -0.00138 0.00400 -0.00557 AFIX 13 H11 2 0.707668 0.501203 0.823503 11.00000 -1.20000 AFIX 0 C12 1 0.522121 0.544112 0.759767 11.00000 0.02891 0.02578 = 0.02543 -0.00424 0.00396 0.00168 AFIX 23 H12A 2 0.422191 0.508602 0.755611 11.00000 -1.20000 H12B 2 0.564235 0.535964 0.706645 11.00000 -1.20000 AFIX 0 C13 1 0.520105 0.696251 0.784764 11.00000 0.04005 0.02488 = 0.03298 0.00249 0.00338 0.00444 AFIX 23 H13A 2 0.618754 0.734610 0.783277 11.00000 -1.20000 H13B 2 0.457715 0.749127 0.746655 11.00000 -1.20000 AFIX 0 C14 1 0.464265 0.711840 0.868375 11.00000 0.03227 0.02170 = 0.04245 -0.01200 0.00905 0.00378 AFIX 23 H14A 2 0.470371 0.809927 0.884730 11.00000 -1.20000 H14B 2 0.361818 0.683670 0.868377 11.00000 -1.20000 AFIX 0 C15 1 0.550721 0.624333 0.927326 11.00000 0.03291 0.02108 = 0.02414 -0.00848 0.00333 -0.00101 AFIX 23 H15A 2 0.510221 0.634298 0.980757 11.00000 -1.20000 H15B 2 0.651310 0.658226 0.930595 11.00000 -1.20000 AFIX 0 C16 1 0.550359 0.472772 0.904256 11.00000 0.03025 0.02024 = 0.01789 -0.00739 0.01030 -0.00171 AFIX 23 H16A 2 0.450928 0.436056 0.904661 11.00000 -1.20000 H16B 2 0.610601 0.419562 0.943243 11.00000 -1.20000 AFIX 0 C17 1 0.721398 0.191921 0.873641 11.00000 0.01756 0.01763 = 0.01267 0.00053 0.00091 -0.00006 AFIX 13 H17 2 0.654884 0.209920 0.917981 11.00000 -1.20000 AFIX 0 C18 1 0.866769 0.255462 0.899096 11.00000 0.02480 0.01782 = 0.03086 0.00914 -0.00933 -0.00275 AFIX 23 H18A 2 0.937735 0.237072 0.857816 11.00000 -1.20000 H18B 2 0.856368 0.356727 0.904430 11.00000 -1.20000 AFIX 0 C19 1 0.920709 0.194318 0.978467 11.00000 0.04239 0.01962 = 0.03531 0.00541 -0.02381 -0.00178 AFIX 23 H19A 2 1.017455 0.232169 0.992223 11.00000 -1.20000 H19B 2 0.855257 0.222877 1.020684 11.00000 -1.20000 AFIX 0 C20 1 0.929302 0.038023 0.976837 11.00000 0.02777 0.02596 = 0.02432 0.00749 -0.00990 -0.00071 AFIX 23 H20A 2 0.954729 0.003428 1.031040 11.00000 -1.20000 H20B 2 1.006140 0.009183 0.941043 11.00000 -1.20000 AFIX 0 C21 1 0.786674 -0.025006 0.947972 11.00000 0.02817 0.01572 = 0.02488 0.00944 0.00032 0.00207 AFIX 23 H21A 2 0.712741 -0.006779 0.987648 11.00000 -1.20000 H21B 2 0.797768 -0.126276 0.943116 11.00000 -1.20000 AFIX 0 C22 1 0.736551 0.034768 0.867372 11.00000 0.02225 0.02087 = 0.02483 0.00516 -0.00566 0.00571 AFIX 23 H22A 2 0.642696 -0.006314 0.850545 11.00000 -1.20000 H22B 2 0.807230 0.011676 0.826705 11.00000 -1.20000 AFIX 0 C23 1 0.469320 0.187213 0.764874 11.00000 0.02031 0.01880 = 0.01863 -0.00393 -0.00538 -0.00178 AFIX 13 H23 2 0.496248 0.088460 0.756478 11.00000 -1.20000 AFIX 0 C24 1 0.390541 0.231304 0.687569 11.00000 0.02596 0.02854 = 0.02064 -0.00261 -0.00585 0.00022 AFIX 23 H24A 2 0.349868 0.324963 0.693922 11.00000 -1.20000 H24B 2 0.459045 0.234184 0.643794 11.00000 -1.20000 AFIX 0 C25 1 0.269965 0.129477 0.667004 11.00000 0.03102 0.03642 = 0.04842 -0.01647 -0.02211 0.01573 AFIX 23 H25A 2 0.311822 0.037435 0.656827 11.00000 -1.20000 H25B 2 0.217404 0.159972 0.617727 11.00000 -1.20000 AFIX 0 C26 1 0.164522 0.118619 0.734837 11.00000 0.01940 0.02542 = 0.07640 0.00523 -0.01691 -0.00430 AFIX 23 H26A 2 0.113544 0.207642 0.740487 11.00000 -1.20000 H26B 2 0.091762 0.046678 0.721690 11.00000 -1.20000 AFIX 0 C27 1 0.242286 0.082858 0.812634 11.00000 0.02316 0.03032 = 0.06719 0.01569 -0.00625 -0.01005 AFIX 23 H27A 2 0.282616 -0.011471 0.809198 11.00000 -1.20000 H27B 2 0.172996 0.083775 0.856052 11.00000 -1.20000 AFIX 0 C28 1 0.363973 0.185023 0.832213 11.00000 0.01834 0.03565 = 0.02475 0.00637 -0.00002 -0.00611 AFIX 23 H28A 2 0.323430 0.278503 0.839507 11.00000 -1.20000 H28B 2 0.415009 0.157616 0.882566 11.00000 -1.20000 AFIX 0 N1 3 0.841515 0.356068 0.556336 11.00000 0.02072 0.04390 = 0.02029 0.00630 0.00673 -0.00268 O1 4 0.884419 0.489852 0.724227 11.00000 0.02076 0.02759 = 0.03821 -0.00567 0.01267 -0.00660 O2 4 1.124885 0.522530 0.676183 11.00000 0.02564 0.08421 = 0.03511 -0.01071 0.01298 -0.01240 O3 4 1.095396 0.476109 0.815605 11.00000 0.04481 0.03389 = 0.04278 0.01646 -0.00423 -0.00084 F1 5 0.954550 0.775078 0.698314 11.00000 0.08560 0.03713 = 0.15959 0.03702 -0.07423 -0.00866 F2 5 0.926807 0.732612 0.822593 11.00000 0.06409 0.09574 = 0.13183 -0.08428 -0.01368 0.03369 F3 5 1.137562 0.769294 0.780144 11.00000 0.05992 0.03026 = 0.16288 0.00299 -0.05996 -0.01391 P1 6 0.642099 0.278513 0.784526 11.00000 0.01480 0.01784 = 0.01194 -0.00087 0.00117 0.00102 S1 7 1.034019 0.529635 0.742589 11.00000 0.02156 0.01765 = 0.02729 0.00041 0.00633 -0.00126 PD1 8 0.775375 0.305627 0.673881 11.00000 0.01680 0.01894 = 0.01388 0.00097 0.00337 0.00257 HKLF 4 Covalent radii and connectivity table for 02SRC110 in P2(1) C 0.770 H 0.320 N 0.700 O 0.660 F 0.640 P 1.100 S 1.030 PD 1.380 C1 - F2 F3 F1 S1 C2 - N1 C3 - N1 C4 - N1 C5 C5 - C6 C10 C4 C6 - C7 C5 C7 - C6 C8 C8 - C7 C9 C9 - C10 C8 C10 - C9 C5 Pd1 C11 - C12 C16 P1 C12 - C11 C13 C13 - C14 C12 C14 - C15 C13 C15 - C14 C16 C16 - C15 C11 C17 - C18 C22 P1 C18 - C19 C17 C19 - C20 C18 C20 - C19 C21 C21 - C20 C22 C22 - C21 C17 C23 - C28 C24 P1 C24 - C25 C23 C25 - C24 C26 C26 - C27 C25 C27 - C26 C28 C28 - C23 C27 N1 - C2 C3 C4 Pd1 O1 - S1 Pd1 O2 - S1 O3 - S1 F1 - C1 F2 - C1 F3 - C1 P1 - C17 C23 C11 Pd1 S1 - O2 O3 O1 C1 Pd1 - C10 N1 O1 P1 Floating origin restraints generated 11601 Reflections read, of which 13 rejected -12 =< h =< 10, -11 =< k =< 11, -21 =< l =< 21, 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) 1 -1 0 526.59 10.05 2 448.47 6 -8 1 11.13 0.98 2 9.17 0 -1 2 195.16 7.41 2 119.31 -1 -7 3 94.33 3.23 3 18.29 4 -7 3 13.34 0.97 2 11.77 -2 -9 5 37.69 0.99 3 21.07 -1 -8 5 112.50 4.56 3 30.25 0 -7 5 169.12 3.67 4 27.77 2 0 5 292.67 2.85 3 100.36 -1 -9 7 5.70 0.98 2 5.55 0 -8 7 12.37 0.71 3 4.53 11 Inconsistent equivalents 6436 Unique reflections, of which 0 suppressed R(int) = 0.0348 R(sigma) = 0.0702 Friedel opposites not merged Maximum memory for data reduction = 4024 / 63926 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 = 5087 / 441418 wR2 = 0.0802 before cycle 1 for 6436 data and 346 / 346 parameters GooF = S = 0.936; Restrained GooF = 0.936 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0409 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27188 0.00036 0.388 OSF 2 0.00285 0.00066 0.159 EXTI 16 0.04283 0.00307 -3.090 U22 C2 200 0.00076 0.00144 -3.064 U23 C22 243 0.03765 0.00230 3.183 U22 C27 Mean shift/esd = 0.626 Maximum = 3.183 for U22 C27 Max. shift = 0.033 A for H2C Max. dU =-0.002 for C2 Least-squares cycle 2 Maximum vector length = 511 Memory required = 5087 / 441418 wR2 = 0.0774 before cycle 2 for 6436 data and 346 / 346 parameters GooF = S = 0.906; Restrained GooF = 0.905 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0409 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27182 0.00035 -0.158 OSF 2 0.00286 0.00064 0.019 EXTI Mean shift/esd = 0.203 Maximum = 1.155 for U22 C27 Max. shift = 0.009 A for H2C Max. dU = 0.001 for C27 Least-squares cycle 3 Maximum vector length = 511 Memory required = 5087 / 441418 wR2 = 0.0772 before cycle 3 for 6436 data and 346 / 346 parameters GooF = S = 0.903; Restrained GooF = 0.903 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0409 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27182 0.00034 -0.013 OSF 2 0.00285 0.00064 -0.004 EXTI Mean shift/esd = 0.011 Maximum = -0.076 for U11 C25 Max. shift = 0.001 A for H3A Max. dU = 0.000 for C22 Least-squares cycle 4 Maximum vector length = 511 Memory required = 5087 / 441418 wR2 = 0.0773 before cycle 4 for 6436 data and 346 / 346 parameters GooF = S = 0.903; Restrained GooF = 0.903 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0409 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.27182 0.00034 -0.005 OSF 2 0.00285 0.00064 -0.007 EXTI Mean shift/esd = 0.003 Maximum = 0.023 for U12 C27 Max. shift = 0.001 A for H3A Max. dU = 0.000 for C27 Largest correlation matrix elements 0.594 EXTI / OSF 0.558 U33 Pd1 / OSF -0.528 U13 F1 / U33 F1 -0.579 U23 F2 / U22 F2 0.548 U22 Pd1 / OSF -0.513 z F2 / y F2 0.565 U11 Pd1 / OSF -0.548 U23 F2 / U33 F2 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2A 0.9191 0.5496 0.5727 137 0.980 0.000 C2 N1 H2A H2B 0.7483 0.5450 0.5565 137 0.980 0.000 C2 N1 H2A H2C 0.8540 0.5230 0.4845 137 0.980 0.000 C2 N1 H2A H3A 1.0065 0.3174 0.4834 137 0.980 0.000 C3 N1 H3A H3B 0.9847 0.1990 0.5483 137 0.980 0.000 C3 N1 H3A H3C 1.0585 0.3422 0.5742 137 0.980 0.000 C3 N1 H3A H4A 0.7625 0.2835 0.4484 23 0.990 0.000 C4 N1 C5 H4B 0.6391 0.3444 0.5030 23 0.990 0.000 C4 N1 C5 H6 0.6653 0.0449 0.4302 43 0.950 0.000 C6 C7 C5 H7 0.6313 -0.1718 0.4863 43 0.950 0.000 C7 C6 C8 H8 0.6517 -0.1996 0.6241 43 0.950 0.000 C8 C7 C9 H9 0.7002 -0.0094 0.7063 43 0.950 0.000 C9 C10 C8 H11 0.7075 0.5013 0.8233 13 1.000 0.000 C11 C12 C16 P1 H12A 0.4221 0.5084 0.7556 23 0.990 0.000 C12 C11 C13 H12B 0.5642 0.5355 0.7065 23 0.990 0.000 C12 C11 C13 H13A 0.6196 0.7337 0.7836 23 0.990 0.000 C13 C14 C12 H13B 0.4591 0.7491 0.7466 23 0.990 0.000 C13 C14 C12 H14A 0.4707 0.8109 0.8844 23 0.990 0.000 C14 C15 C13 H14B 0.3618 0.6848 0.8683 23 0.990 0.000 C14 C15 C13 H15A 0.5104 0.6352 0.9807 23 0.990 0.000 C15 C14 C16 H15B 0.6514 0.6591 0.9305 23 0.990 0.000 C15 C14 C16 H16A 0.4508 0.4363 0.9046 23 0.990 0.000 C16 C15 C11 H16B 0.6105 0.4197 0.9431 23 0.990 0.000 C16 C15 C11 H17 0.6545 0.2099 0.9178 13 1.000 0.000 C17 C18 C22 P1 H18A 0.9377 0.2364 0.8577 23 0.990 0.000 C18 C19 C17 H18B 0.8567 0.3563 0.9043 23 0.990 0.000 C18 C19 C17 H19A 1.0175 0.2315 0.9922 23 0.990 0.000 C19 C20 C18 H19B 0.8553 0.2223 1.0207 23 0.990 0.000 C19 C20 C18 H20A 0.9544 0.0023 1.0311 23 0.990 0.000 C20 C19 C21 H20B 1.0063 0.0079 0.9412 23 0.990 0.000 C20 C19 C21 H21A 0.7125 -0.0079 0.9874 23 0.990 0.000 C21 C20 C22 H21B 0.7974 -0.1272 0.9426 23 0.990 0.000 C21 C20 C22 H22A 0.6431 -0.0069 0.8504 23 0.990 0.000 C22 C21 C17 H22B 0.8076 0.0115 0.8269 23 0.990 0.000 C22 C21 C17 H23 0.4963 0.0896 0.7566 13 1.000 0.000 C23 C28 C24 P1 H24A 0.3486 0.3248 0.6936 23 0.990 0.000 C24 C25 C23 H24B 0.4585 0.2345 0.6436 23 0.990 0.000 C24 C25 C23 H25A 0.3121 0.0360 0.6575 23 0.990 0.000 C25 C24 C26 H25B 0.2172 0.1574 0.6175 23 0.990 0.000 C25 C24 C26 H26A 0.1131 0.2068 0.7396 23 0.990 0.000 C26 C27 C25 H26B 0.0920 0.0454 0.7216 23 0.990 0.000 C26 C27 C25 H27A 0.2829 -0.0110 0.8096 23 0.990 0.000 C27 C26 C28 H27B 0.1730 0.0846 0.8559 23 0.990 0.000 C27 C26 C28 H28A 0.3234 0.2791 0.8397 23 0.990 0.000 C28 C23 C27 H28B 0.4152 0.1582 0.8826 23 0.990 0.000 C28 C23 C27 02SRC110 in P2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 1.01145 0.71147 0.76207 1.00000 0.03810 0.02437 0.09061 -0.00111 -0.03284 -0.00229 0.05189 0.00737 0.00050 0.00043 0.00034 0.00000 0.00268 0.00223 0.00418 0.00224 0.00281 0.00182 0.00143 C2 0.84059 0.50598 0.54125 1.00000 0.07213 0.04057 0.03879 0.02436 -0.00045 -0.01098 0.05056 0.00864 0.00060 0.00044 0.00028 0.00000 0.00342 0.00262 0.00265 0.00199 0.00233 0.00224 0.00125 H2A 0.91906 0.54960 0.57272 1.00000 0.07584 0.00000 0.00000 H2B 0.74827 0.54501 0.55652 1.00000 0.07584 0.00000 0.00000 H2C 0.85399 0.52298 0.48445 1.00000 0.07584 0.00000 0.00000 C3 0.98497 0.29891 0.53907 1.00000 0.01949 0.06884 0.02754 -0.00862 0.01003 0.00053 0.03840 0.00780 0.00034 0.00065 0.00020 0.00000 0.00161 0.00252 0.00181 0.00275 0.00135 0.00266 0.00085 H3A 1.00646 0.31740 0.48336 1.00000 0.05760 0.00000 0.00000 H3B 0.98469 0.19901 0.54831 1.00000 0.05760 0.00000 0.00000 H3C 1.05855 0.34221 0.57417 1.00000 0.05760 0.00000 0.00000 C4 0.72897 0.28944 0.50361 1.00000 0.02587 0.05355 0.01508 0.00204 0.00100 -0.00088 0.03149 0.00676 0.00036 0.00053 0.00019 0.00000 0.00169 0.00253 0.00158 0.00201 0.00130 0.00208 0.00085 H4A 0.76251 0.28349 0.44841 1.00000 0.03779 0.00000 0.00000 H4B 0.63907 0.34439 0.50297 1.00000 0.03779 0.00000 0.00000 C5 0.70181 0.14841 0.53520 1.00000 0.01506 0.04226 0.01991 -0.00437 0.00441 0.00333 0.02565 0.00608 0.00037 0.00037 0.00021 0.00000 0.00178 0.00219 0.00194 0.00149 0.00147 0.00146 0.00080 C6 0.67205 0.03394 0.48649 1.00000 0.02003 0.06560 0.01863 -0.01389 -0.00146 -0.00364 0.03481 0.00650 0.00041 0.00046 0.00023 0.00000 0.00195 0.00288 0.00200 0.00189 0.00158 0.00190 0.00096 H6 0.66533 0.04488 0.43023 1.00000 0.04177 0.00000 0.00000 C7 0.65244 -0.09458 0.51960 1.00000 0.02085 0.05132 0.03227 -0.02267 0.00177 -0.00366 0.03479 0.00637 0.00040 0.00044 0.00024 0.00000 0.00194 0.00252 0.00230 0.00190 0.00170 0.00174 0.00095 H7 0.63126 -0.17179 0.48630 1.00000 0.04175 0.00000 0.00000 C8 0.66364 -0.11082 0.60121 1.00000 0.02507 0.03303 0.03456 -0.01403 0.00133 0.00356 0.03088 0.00619 0.00040 0.00039 0.00023 0.00000 0.00200 0.00215 0.00236 0.00167 0.00171 0.00154 0.00088 H8 0.65173 -0.19958 0.62412 1.00000 0.03706 0.00000 0.00000 C9 0.69244 0.00305 0.65013 1.00000 0.02311 0.02231 0.02283 -0.00761 -0.00111 0.00564 0.02280 0.00584 0.00037 0.00034 0.00021 0.00000 0.00188 0.00183 0.00192 0.00135 0.00151 0.00135 0.00076 H9 0.70025 -0.00937 0.70626 1.00000 0.02736 0.00000 0.00000 C10 0.70985 0.13357 0.61861 1.00000 0.01387 0.02601 0.01742 -0.00082 0.00024 0.00183 0.01911 0.00566 0.00035 0.00034 0.00020 0.00000 0.00163 0.00175 0.00179 0.00131 0.00137 0.00128 0.00070 C11 0.61017 0.45705 0.81999 1.00000 0.01840 0.01783 0.01725 -0.00021 0.00381 -0.00329 0.01775 0.00550 0.00036 0.00031 0.00019 0.00000 0.00169 0.00160 0.00175 0.00123 0.00136 0.00127 0.00068 H11 0.70749 0.50125 0.82329 1.00000 0.02130 0.00000 0.00000 C12 0.52215 0.54373 0.75967 1.00000 0.02999 0.02249 0.02462 -0.00037 0.00296 0.00581 0.02565 0.00632 0.00040 0.00035 0.00021 0.00000 0.00204 0.00181 0.00196 0.00143 0.00160 0.00149 0.00079 H12A 0.42215 0.50840 0.75558 1.00000 0.03078 0.00000 0.00000 H12B 0.56419 0.53551 0.70653 1.00000 0.03078 0.00000 0.00000 C13 0.52072 0.69590 0.78487 1.00000 0.04180 0.02160 0.03308 0.00601 0.00275 0.00895 0.03213 0.00728 0.00046 0.00038 0.00024 0.00000 0.00242 0.00182 0.00234 0.00159 0.00189 0.00164 0.00091 H13A 0.61964 0.73366 0.78360 1.00000 0.03855 0.00000 0.00000 H13B 0.45906 0.74909 0.74655 1.00000 0.03855 0.00000 0.00000 C14 0.46431 0.71271 0.86831 1.00000 0.03230 0.01766 0.04238 -0.00957 0.00684 0.00431 0.03065 0.00673 0.00043 0.00036 0.00024 0.00000 0.00217 0.00181 0.00249 0.00154 0.00185 0.00148 0.00090 H14A 0.47071 0.81091 0.88441 1.00000 0.03678 0.00000 0.00000 H14B 0.36179 0.68477 0.86832 1.00000 0.03678 0.00000 0.00000 C15 0.55081 0.62521 0.92730 1.00000 0.03298 0.02146 0.02495 -0.00937 0.00384 -0.00197 0.02640 0.00613 0.00042 0.00034 0.00022 0.00000 0.00212 0.00184 0.00200 0.00144 0.00164 0.00149 0.00082 H15A 0.51036 0.63522 0.98074 1.00000 0.03167 0.00000 0.00000 H15B 0.65142 0.65906 0.93053 1.00000 0.03167 0.00000 0.00000 C16 0.55031 0.47297 0.90412 1.00000 0.03024 0.01995 0.01808 -0.00565 0.01028 0.00002 0.02253 0.00610 0.00040 0.00034 0.00021 0.00000 0.00200 0.00172 0.00180 0.00131 0.00151 0.00142 0.00075 H16A 0.45084 0.43634 0.90456 1.00000 0.02703 0.00000 0.00000 H16B 0.61052 0.41973 0.94310 1.00000 0.02703 0.00000 0.00000 C17 0.72095 0.19180 0.87344 1.00000 0.01751 0.01759 0.01223 -0.00162 0.00081 -0.00245 0.01577 0.00536 0.00035 0.00032 0.00019 0.00000 0.00163 0.00153 0.00167 0.00120 0.00129 0.00126 0.00065 H17 0.65446 0.20986 0.91778 1.00000 0.01892 0.00000 0.00000 C18 0.86678 0.25500 0.89900 1.00000 0.02434 0.02012 0.03121 0.00806 -0.00891 -0.00497 0.02547 0.00576 0.00037 0.00035 0.00021 0.00000 0.00189 0.00164 0.00214 0.00133 0.00161 0.00130 0.00082 H18A 0.93768 0.23645 0.85771 1.00000 0.03056 0.00000 0.00000 H18B 0.85668 0.35630 0.90434 1.00000 0.03056 0.00000 0.00000 C19 0.92076 0.19369 0.97847 1.00000 0.04054 0.02487 0.03384 0.00421 -0.02150 -0.00428 0.03364 0.00629 0.00045 0.00039 0.00023 0.00000 0.00238 0.00186 0.00231 0.00157 0.00191 0.00159 0.00095 H19A 1.01753 0.23148 0.99222 1.00000 0.04037 0.00000 0.00000 H19B 0.85533 0.22230 1.02069 1.00000 0.04037 0.00000 0.00000 C20 0.92929 0.03687 0.97689 1.00000 0.02795 0.02561 0.02446 0.00767 -0.00940 -0.00046 0.02626 0.00580 0.00038 0.00035 0.00021 0.00000 0.00201 0.00180 0.00190 0.00141 0.00159 0.00148 0.00080 H20A 0.95437 0.00226 1.03114 1.00000 0.03151 0.00000 0.00000 H20B 1.00628 0.00791 0.94122 1.00000 0.03151 0.00000 0.00000 C21 0.78645 -0.02591 0.94775 1.00000 0.02800 0.01692 0.02396 0.00638 0.00090 -0.00132 0.02296 0.00592 0.00039 0.00034 0.00021 0.00000 0.00193 0.00165 0.00196 0.00134 0.00153 0.00138 0.00075 H21A 0.71245 -0.00791 0.98743 1.00000 0.02756 0.00000 0.00000 H21B 0.79743 -0.12715 0.94264 1.00000 0.02756 0.00000 0.00000 C22 0.73673 0.03441 0.86747 1.00000 0.02250 0.02076 0.02474 -0.00068 -0.00583 0.00119 0.02283 0.00582 0.00038 0.00034 0.00021 0.00000 0.00182 0.00167 0.00194 0.00138 0.00148 0.00138 0.00074 H22A 0.64307 -0.00686 0.85044 1.00000 0.02740 0.00000 0.00000 H22B 0.80764 0.01153 0.82689 1.00000 0.02740 0.00000 0.00000 C23 0.46942 0.18835 0.76490 1.00000 0.02050 0.01823 0.01901 -0.00422 -0.00532 -0.00116 0.01940 0.00544 0.00036 0.00034 0.00020 0.00000 0.00178 0.00160 0.00183 0.00128 0.00143 0.00129 0.00071 H23 0.49631 0.08956 0.75662 1.00000 0.02328 0.00000 0.00000 C24 0.39006 0.23139 0.68745 1.00000 0.02409 0.03484 0.01973 -0.00247 -0.00363 0.00111 0.02633 0.00595 0.00039 0.00037 0.00021 0.00000 0.00194 0.00199 0.00193 0.00147 0.00154 0.00150 0.00080 H24A 0.34862 0.32478 0.69362 1.00000 0.03159 0.00000 0.00000 H24B 0.45847 0.23452 0.64364 1.00000 0.03159 0.00000 0.00000 C25 0.26964 0.12798 0.66705 1.00000 0.03097 0.03702 0.04885 -0.01946 -0.02236 0.01197 0.03953 0.00648 0.00042 0.00045 0.00025 0.00000 0.00237 0.00240 0.00285 0.00183 0.00216 0.00166 0.00115 H25A 0.31214 0.03600 0.65747 1.00000 0.04744 0.00000 0.00000 H25B 0.21718 0.15739 0.61751 1.00000 0.04744 0.00000 0.00000 C26 0.16445 0.11782 0.73443 1.00000 0.01980 0.02456 0.07524 0.00081 -0.01565 -0.00690 0.04030 0.00672 0.00042 0.00039 0.00029 0.00000 0.00205 0.00204 0.00338 0.00197 0.00216 0.00156 0.00111 H26A 0.11311 0.20675 0.73961 1.00000 0.04835 0.00000 0.00000 H26B 0.09202 0.04544 0.72157 1.00000 0.04835 0.00000 0.00000 C27 0.24245 0.08335 0.81261 1.00000 0.02204 0.04046 0.06625 0.01655 -0.00302 -0.01160 0.04303 0.00741 0.00042 0.00050 0.00028 0.00000 0.00212 0.00250 0.00316 0.00212 0.00207 0.00173 0.00112 H27A 0.28294 -0.01097 0.80959 1.00000 0.05164 0.00000 0.00000 H27B 0.17296 0.08459 0.85593 1.00000 0.05164 0.00000 0.00000 C28 0.36408 0.18569 0.83227 1.00000 0.01827 0.03506 0.02392 0.00507 -0.00025 -0.00655 0.02578 0.00617 0.00037 0.00039 0.00022 0.00000 0.00180 0.00200 0.00203 0.00153 0.00153 0.00149 0.00079 H28A 0.32339 0.27908 0.83969 1.00000 0.03093 0.00000 0.00000 H28B 0.41521 0.15818 0.88257 1.00000 0.03093 0.00000 0.00000 N1 0.84131 0.35666 0.55633 1.00000 0.02095 0.03802 0.02071 0.00575 0.00533 -0.00230 0.02645 0.00518 0.00032 0.00031 0.00017 0.00000 0.00157 0.00173 0.00159 0.00116 0.00127 0.00118 0.00069 O1 0.88427 0.49041 0.72417 1.00000 0.02150 0.02456 0.03824 -0.00652 0.01147 -0.00740 0.02785 0.00422 0.00026 0.00025 0.00016 0.00000 0.00133 0.00130 0.00157 0.00107 0.00111 0.00100 0.00057 O2 1.12490 0.52330 0.67624 1.00000 0.02489 0.08925 0.03432 -0.01081 0.01372 -0.01315 0.04918 0.00510 0.00030 0.00036 0.00017 0.00000 0.00155 0.00245 0.00172 0.00161 0.00133 0.00151 0.00082 O3 1.09529 0.47645 0.81559 1.00000 0.04441 0.03478 0.04266 0.01592 -0.00453 -0.00311 0.04077 0.00499 0.00031 0.00028 0.00017 0.00000 0.00177 0.00150 0.00181 0.00126 0.00141 0.00130 0.00071 F1 0.95418 0.77570 0.69821 1.00000 0.08728 0.03137 0.16244 0.03677 -0.07725 -0.00894 0.09571 0.00500 0.00035 0.00026 0.00024 0.00000 0.00215 0.00182 0.00328 0.00172 0.00229 0.00139 0.00132 F2 0.92675 0.73247 0.82258 1.00000 0.06517 0.08935 0.12974 -0.08185 -0.01618 0.03322 0.09524 0.00522 0.00037 0.00036 0.00025 0.00000 0.00216 0.00247 0.00327 0.00231 0.00217 0.00176 0.00138 F3 1.13742 0.77019 0.77991 1.00000 0.06155 0.02823 0.16360 0.00367 -0.06216 -0.01456 0.08609 0.00438 0.00031 0.00024 0.00023 0.00000 0.00179 0.00162 0.00328 0.00149 0.00205 0.00116 0.00121 P1 0.64208 0.27851 0.78451 1.00000 0.01480 0.01706 0.01204 -0.00106 0.00094 0.00058 0.01462 0.00132 0.00008 0.00008 0.00005 0.00000 0.00037 0.00051 0.00037 0.00029 0.00030 0.00029 0.00019 S1 1.03402 0.52978 0.74259 1.00000 0.02146 0.01886 0.02727 -0.00041 0.00656 -0.00204 0.02239 0.00146 0.00009 0.00008 0.00005 0.00000 0.00045 0.00041 0.00049 0.00033 0.00037 0.00033 0.00019 Pd1 0.77537 0.30560 0.67388 1.00000 0.01684 0.01858 0.01394 0.00088 0.00326 0.00250 0.01639 0.00036 0.00002 0.00002 0.00001 0.00000 0.00012 0.00012 0.00012 0.00011 0.00008 0.00011 0.00008 Final Structure Factor Calculation for 02SRC110 in P2(1) Total number of l.s. parameters = 346 Maximum vector length = 511 Memory required = 4743 / 29134 wR2 = 0.0772 before cycle 5 for 6436 data and 2 / 346 parameters GooF = S = 0.903; Restrained GooF = 0.903 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0409 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0341 for 5824 Fo > 4sig(Fo) and 0.0420 for all 6436 data wR2 = 0.0772, GooF = S = 0.903, Restrained GooF = 0.903 for all data Flack x parameter = 0.0042 with esd 0.0206 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Occupancy sum of asymmetric unit = 38.00 for non-hydrogen and 45.00 for hydrogen atoms Principal mean square atomic displacements U 0.1096 0.0259 0.0202 C1 0.0794 0.0578 0.0144 C2 0.0706 0.0320 0.0126 C3 0.0537 0.0258 0.0149 C4 0.0434 0.0216 0.0120 C5 0.0695 0.0214 0.0135 C6 0.0665 0.0209 0.0169 C7 0.0482 0.0261 0.0183 C8 0.0334 0.0212 0.0138 C9 0.0264 0.0174 0.0136 C10 0.0225 0.0173 0.0134 C11 0.0334 0.0246 0.0190 C12 0.0460 0.0337 0.0167 C13 0.0466 0.0330 0.0124 C14 0.0361 0.0295 0.0136 C15 0.0355 0.0221 0.0100 C16 0.0202 0.0154 0.0118 C17 0.0428 0.0178 0.0159 C18 0.0622 0.0239 0.0149 C19 0.0394 0.0260 0.0133 C20 0.0287 0.0271 0.0130 C21 0.0308 0.0206 0.0170 C22 0.0266 0.0200 0.0115 C23 0.0356 0.0264 0.0170 C24 0.0791 0.0243 0.0152 C25 0.0811 0.0277 0.0121 C26 0.0764 0.0367 0.0161 C27 0.0392 0.0222 0.0159 C28 0.0398 0.0249 0.0146 N1 0.0465 0.0228 0.0142 O1 0.0945 0.0377 0.0153 O2 0.0587 0.0413 0.0223 O3 0.2249 0.0445 0.0177 F1 may be split into 0.9433 0.7798 0.7089 and 0.9650 0.7716 0.6875 0.2049 0.0618 0.0190 F2 may be split into 0.9223 0.7205 0.8311 and 0.9312 0.7444 0.8141 0.1994 0.0410 0.0179 F3 0.0174 0.0148 0.0117 P1 0.0307 0.0198 0.0166 S1 0.0210 0.0159 0.0122 Pd1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.048 0.072 0.091 0.111 0.129 0.149 0.172 0.205 0.265 1.000 Number in group 654. 650. 632. 644. 647. 650. 637. 637. 641. 644. GooF 0.867 1.005 0.946 0.948 0.925 0.871 0.858 0.837 0.859 0.904 K 1.002 0.944 0.967 0.966 0.977 0.989 1.008 1.019 1.028 1.004 Resolution(A) 0.77 0.81 0.84 0.88 0.93 0.99 1.07 1.17 1.34 1.68 inf Number in group 645. 645. 658. 633. 646. 647. 639. 632. 643. 648. GooF 0.888 0.858 0.870 0.876 0.870 0.929 0.922 0.886 0.884 1.037 K 0.962 0.988 0.986 0.998 1.023 1.028 1.031 1.029 1.013 0.986 R1 0.107 0.083 0.065 0.052 0.043 0.038 0.031 0.026 0.021 0.022 Recommended weighting scheme: WGHT 0.0205 0.0000 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 -1 1 1783.24 2583.66 5.05 0.277 6.28 3 0 6 435.73 539.17 4.14 0.126 2.04 2 8 4 147.06 193.88 3.85 0.076 1.13 -3 4 15 97.06 191.74 3.78 0.075 0.97 -10 4 9 235.83 375.65 3.64 0.106 0.80 0 -5 4 302.96 364.15 3.51 0.104 1.76 -7 6 10 27.61 156.65 3.51 0.068 0.89 -1 0 9 177.67 246.96 3.44 0.086 1.84 2 -2 6 504.68 430.61 3.43 0.113 2.12 1 -5 3 402.08 507.99 3.42 0.123 1.79 0 2 4 684.55 809.14 3.28 0.155 3.17 -1 -3 1 739.84 625.55 3.25 0.136 3.01 -8 6 6 290.67 416.27 3.23 0.111 0.90 6 3 13 236.25 398.30 3.21 0.109 0.93 -6 -7 14 1477.21 1065.39 3.20 0.178 0.79 -11 4 5 138.76 333.91 3.16 0.100 0.78 1 -2 6 540.50 621.19 3.16 0.136 2.32 7 4 11 207.94 327.69 3.15 0.099 0.91 -3 0 6 1729.69 1442.71 3.15 0.207 2.11 6 4 12 250.14 133.47 3.14 0.063 0.94 -5 9 8 124.94 203.32 3.11 0.078 0.86 8 7 4 124.74 207.29 3.10 0.078 0.86 -6 0 1 221.43 281.68 3.08 0.091 1.55 7 5 13 13.94 88.66 3.05 0.051 0.82 -1 -6 1 955.73 1145.04 3.04 0.184 1.58 1 -4 1 3856.77 4559.39 3.04 0.368 2.32 -7 9 2 55.77 130.48 3.01 0.062 0.83 -2 -3 2 2140.16 2442.87 2.96 0.269 2.54 -7 -1 5 331.40 403.30 2.95 0.109 1.24 -2 10 4 415.31 233.99 2.94 0.083 0.93 0 -3 9 692.49 803.91 2.94 0.154 1.61 -3 -3 7 897.36 760.94 2.93 0.150 1.66 6 10 3 249.23 396.11 2.92 0.108 0.81 5 -5 8 2285.34 1920.26 2.92 0.239 1.12 -3 -7 14 -41.42 28.77 2.89 0.029 0.88 3 9 11 400.78 583.67 2.88 0.132 0.84 6 4 17 348.91 566.07 2.87 0.130 0.78 -2 3 6 79.07 101.26 2.85 0.055 1.94 0 1 2 4296.71 4924.66 2.85 0.382 6.34 -6 -8 10 1017.50 759.03 2.84 0.150 0.84 -8 -7 6 906.54 654.77 2.80 0.139 0.85 0 2 0 4243.97 4871.16 2.80 0.380 4.84 2 1 11 278.70 217.03 2.79 0.080 1.42 6 9 0 355.26 452.70 2.79 0.116 0.88 8 -2 6 126.95 163.40 2.78 0.070 1.03 -3 -10 6 110.72 75.87 2.78 0.047 0.88 -3 -2 9 83.00 114.94 2.78 0.058 1.54 -1 -3 16 404.87 520.64 2.77 0.124 1.00 2 0 10 463.93 394.43 2.75 0.108 1.56 -5 1 13 580.26 703.47 2.74 0.144 1.07 Bond lengths and angles C1 - Distance Angles F2 1.3232 (0.0068) F3 1.3254 (0.0049) 107.79 (0.42) F1 1.3330 (0.0055) 108.33 (0.42) 107.72 (0.41) S1 1.8037 (0.0044) 111.44 (0.36) 110.62 (0.31) 110.80 (0.35) C1 - F2 F3 F1 C2 - Distance Angles N1 1.4683 (0.0051) H2A 0.9800 109.47 H2B 0.9800 109.47 109.47 H2C 0.9800 109.47 109.47 109.47 C2 - N1 H2A H2B C3 - Distance Angles N1 1.4854 (0.0046) H3A 0.9800 109.47 H3B 0.9800 109.47 109.47 H3C 0.9800 109.47 109.47 109.47 C3 - N1 H3A H3B C4 - Distance Angles N1 1.4926 (0.0046) C5 1.4902 (0.0060) 108.22 (0.28) H4A 0.9900 110.05 110.05 H4B 0.9900 110.06 110.06 108.40 C4 - N1 C5 H4A C5 - Distance Angles C6 1.3992 (0.0052) C10 1.4067 (0.0048) 120.18 (0.34) C4 1.4902 (0.0060) 123.42 (0.33) 116.39 (0.30) C5 - C6 C10 C6 - Distance Angles C7 1.3782 (0.0061) C5 1.3992 (0.0052) 120.42 (0.35) H6 0.9500 119.79 119.79 C6 - C7 C5 C7 - Distance Angles C6 1.3782 (0.0061) C8 1.3789 (0.0057) 119.83 (0.34) H7 0.9500 120.09 120.09 C7 - C6 C8 C8 - Distance Angles C7 1.3789 (0.0057) C9 1.3951 (0.0048) 120.03 (0.37) H8 0.9500 119.99 119.99 C8 - C7 C9 C9 - Distance Angles C10 1.3822 (0.0047) C8 1.3951 (0.0048) 121.36 (0.33) H9 0.9500 119.32 119.32 C9 - C10 C8 C10 - Distance Angles C9 1.3822 (0.0047) C5 1.4067 (0.0048) 118.15 (0.30) Pd1 1.9915 (0.0033) 128.69 (0.25) 112.47 (0.24) C10 - C9 C5 C11 - Distance Angles C12 1.5290 (0.0045) C16 1.5443 (0.0048) 110.43 (0.28) P1 1.8564 (0.0032) 112.76 (0.22) 116.97 (0.21) H11 1.0000 105.18 105.18 105.18 C11 - C12 C16 P1 C12 - Distance Angles C11 1.5290 (0.0045) C13 1.5337 (0.0050) 110.78 (0.29) H12A 0.9900 109.49 109.49 H12B 0.9900 109.49 109.49 108.06 C12 - C11 C13 H12A C13 - Distance Angles C14 1.5222 (0.0054) C12 1.5337 (0.0050) 111.31 (0.31) H13A 0.9900 109.37 109.37 H13B 0.9900 109.37 109.37 107.99 C13 - C14 C12 H13A C14 - Distance Angles C15 1.5118 (0.0053) C13 1.5222 (0.0054) 110.48 (0.30) H14A 0.9900 109.55 109.55 H14B 0.9900 109.55 109.55 108.10 C14 - C15 C13 H14A C15 - Distance Angles C14 1.5118 (0.0053) C16 1.5251 (0.0045) 112.24 (0.30) H15A 0.9900 109.16 109.16 H15B 0.9900 109.16 109.16 107.88 C15 - C14 C16 H15A C16 - Distance Angles C15 1.5251 (0.0045) C11 1.5443 (0.0048) 109.39 (0.27) H16A 0.9900 109.80 109.80 H16B 0.9900 109.80 109.80 108.25 C16 - C15 C11 H16A C17 - Distance Angles C18 1.5334 (0.0044) C22 1.5351 (0.0044) 109.22 (0.27) P1 1.8412 (0.0032) 111.45 (0.22) 115.86 (0.23) H17 1.0000 106.59 106.59 106.59 C17 - C18 C22 P1 C18 - Distance Angles C19 1.5279 (0.0047) C17 1.5334 (0.0044) 110.31 (0.28) H18A 0.9900 109.59 109.59 H18B 0.9900 109.59 109.59 108.12 C18 - C19 C17 H18A C19 - Distance Angles C20 1.5213 (0.0051) C18 1.5279 (0.0047) 112.86 (0.30) H19A 0.9900 109.01 109.01 H19B 0.9900 109.01 109.01 107.79 C19 - C20 C18 H19A C20 - Distance Angles C19 1.5213 (0.0051) C21 1.5237 (0.0047) 111.02 (0.29) H20A 0.9900 109.43 109.43 H20B 0.9900 109.43 109.43 108.03 C20 - C19 C21 H20A C21 - Distance Angles C20 1.5237 (0.0047) C22 1.5248 (0.0046) 111.26 (0.28) H21A 0.9900 109.38 109.38 H21B 0.9900 109.38 109.38 108.00 C21 - C20 C22 H21A C22 - Distance Angles C21 1.5248 (0.0046) C17 1.5351 (0.0044) 110.45 (0.28) H22A 0.9900 109.56 109.56 H22B 0.9900 109.56 109.56 108.11 C22 - C21 C17 H22A C23 - Distance Angles C28 1.5226 (0.0049) C24 1.5287 (0.0045) 109.47 (0.28) P1 1.8452 (0.0033) 116.98 (0.23) 114.29 (0.24) H23 1.0000 104.94 104.94 104.94 C23 - C28 C24 P1 C24 - Distance Angles C25 1.5310 (0.0054) C23 1.5287 (0.0045) 109.72 (0.30) H24A 0.9900 109.72 109.72 H24B 0.9900 109.73 109.72 108.20 C24 - C25 C23 H24A C25 - Distance Angles C24 1.5310 (0.0054) C26 1.5249 (0.0063) 111.05 (0.31) H25A 0.9900 109.43 109.43 H25B 0.9900 109.43 109.43 108.03 C25 - C24 C26 H25A C26 - Distance Angles C27 1.5128 (0.0058) C25 1.5249 (0.0063) 110.99 (0.32) H26A 0.9900 109.44 109.44 H26B 0.9900 109.44 109.44 108.04 C26 - C27 C25 H26A C27 - Distance Angles C26 1.5128 (0.0058) C28 1.5299 (0.0051) 111.74 (0.33) H27A 0.9900 109.27 109.27 H27B 0.9900 109.27 109.27 107.94 C27 - C26 C28 H27A C28 - Distance Angles C23 1.5226 (0.0049) C27 1.5299 (0.0051) 109.91 (0.32) H28A 0.9900 109.68 109.68 H28B 0.9900 109.68 109.68 108.18 C28 - C23 C27 H28A N1 - Distance Angles C2 1.4683 (0.0052) C3 1.4854 (0.0046) 109.62 (0.38) C4 1.4926 (0.0047) 109.20 (0.33) 109.49 (0.31) Pd1 2.1454 (0.0029) 112.70 (0.26) 112.43 (0.23) 103.16 (0.21) N1 - C2 C3 C4 O1 - Distance Angles S1 1.4644 (0.0025) Pd1 2.2085 (0.0023) 135.23 (0.15) O1 - S1 O2 - Distance Angles S1 1.4235 (0.0029) O2 - O3 - Distance Angles S1 1.4287 (0.0027) O3 - F1 - Distance Angles C1 1.3330 (0.0055) F1 - F2 - Distance Angles C1 1.3232 (0.0068) F2 - F3 - Distance Angles C1 1.3254 (0.0049) F3 - P1 - Distance Angles C17 1.8412 (0.0032) C23 1.8452 (0.0033) 104.24 (0.15) C11 1.8564 (0.0032) 103.20 (0.14) 110.49 (0.15) Pd1 2.2847 (0.0008) 120.00 (0.11) 113.76 (0.11) 104.57 (0.11) P1 - C17 C23 C11 S1 - Distance Angles O2 1.4235 (0.0029) O3 1.4287 (0.0027) 115.22 (0.19) O1 1.4644 (0.0025) 114.17 (0.16) 115.61 (0.17) C1 1.8037 (0.0044) 105.14 (0.25) 104.04 (0.21) 100.17 (0.18) S1 - O2 O3 O1 Pd1 - Distance Angles C10 1.9915 (0.0033) N1 2.1454 (0.0029) 81.79 (0.13) O1 2.2085 (0.0024) 169.76 (0.12) 91.29 (0.10) P1 2.2847 (0.0008) 96.72 (0.10) 162.89 (0.08) 92.10 (0.07) Pd1 - C10 N1 O1 FMAP and GRID set by program FMAP 2 3 38 GRID -1.429 -2 -2 1.429 2 2 R1 = 0.0358 for 3616 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.80 at 0.3262 0.8081 0.0218 [ 1.36 A from H16B ] Deepest hole -0.76 at 0.1381 0.8058 0.3392 [ 0.84 A from PD1 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 4337 / 26460 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.6738 0.3081 0.9782 1.00000 0.05 0.80 1.36 H16B 1.40 H17 1.99 H19B 2.15 C17 Q2 1 0.7767 -0.0964 0.6769 1.00000 0.05 0.69 1.22 H9 1.31 C9 1.62 C8 1.75 H8 Q3 1 0.4901 0.0315 0.3977 1.00000 0.05 0.48 1.70 H6 1.80 H12B 2.21 C6 2.37 H2B Q4 1 0.7801 -0.2856 0.6788 1.00000 0.05 0.41 1.70 H8 1.74 F1 2.35 H13A 2.37 C8 Q5 1 0.8766 0.3045 0.6167 1.00000 0.05 0.37 1.17 N1 1.37 PD1 1.68 C3 1.86 H3B Q6 1 0.6861 0.2027 0.6479 1.00000 0.05 0.37 0.86 C10 1.36 PD1 1.93 C9 1.97 C5 Q7 1 0.6654 0.3049 0.7276 1.00000 0.05 0.36 1.02 P1 1.39 PD1 2.21 C11 2.25 C23 Q8 1 1.0513 0.6645 0.7468 1.00000 0.05 0.36 0.65 C1 1.32 S1 1.40 F3 1.61 F1 Q9 1 0.4021 0.5224 0.9129 1.00000 0.05 0.35 0.96 H16A 1.47 C16 1.71 C15 1.78 H14B Q10 1 0.9068 0.2857 0.5612 1.00000 0.05 0.35 0.84 C3 0.92 N1 1.13 H3B 1.52 H3C Shortest distances between peaks (including symmetry equivalents) 5 10 1.00 6 7 1.68 2 4 1.83 5 6 2.11 6 10 2.68 5 7 2.75 4 8 2.77 Time profile in seconds ----------------------- 0.11: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.28: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 3.48: Structure factors and derivatives 5.58: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.09: Apply other restraints 0.28: Solve l.s. equations 0.00: Generate HTAB table 0.06: Other dependent quantities, CIF, tables 0.16: Analysis of variance 0.11: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.06: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 15:59:15 Total elapsed time: 10.3 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++