+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0216r started at 13:02:13 on 04-Mar-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0216r in P2(1)/c CELL 0.71073 6.2066 17.1960 15.1712 90.000 90.442 90.000 ZERR 4.00 0.0003 0.0008 0.0006 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N P S CL PD UNIT 56 84 12 4 4 4 4 V = 1619.15 F(000) = 880.0 Mu = 1.53 mm-1 Cell Wt = 1744.87 Rho = 1.789 MERG 2 OMIT -3.00 50.00 SHEL 7 0.84 FMAP 2 PLAN 10 SIZE 0.01 0.07 0.09 ACTA 50.00 BOND $H WGHT 0.00000 28.39930 L.S. 4 TEMP -153.00 FVAR 0.40489 MOLE 1 C1 1 0.253963 0.673844 0.183218 11.00000 0.01647 0.01489 = 0.01742 0.00090 -0.00421 0.00106 C2 1 0.203834 0.691608 0.268681 11.00000 0.03168 0.02405 = 0.01499 0.00661 -0.00439 -0.00820 AFIX 43 H2 2 0.066090 0.712308 0.282220 11.00000 -1.20000 AFIX 0 C3 1 0.354198 0.679384 0.335549 11.00000 0.04099 0.02307 = 0.02416 0.00389 -0.00358 -0.01149 AFIX 43 H3 2 0.321877 0.694603 0.394172 11.00000 -1.20000 AFIX 0 C4 1 0.547200 0.645810 0.317694 11.00000 0.05223 0.02475 = 0.03676 0.00559 -0.02573 -0.00247 AFIX 43 H4 2 0.648414 0.638810 0.364313 11.00000 -1.20000 AFIX 0 C5 1 0.600598 0.621651 0.234276 11.00000 0.02258 0.01503 = 0.06506 0.00822 -0.01419 0.00312 AFIX 43 H5 2 0.733124 0.595941 0.223182 11.00000 -1.20000 AFIX 0 C6 1 0.450627 0.636537 0.165538 11.00000 0.02584 0.01872 = 0.02616 -0.00447 -0.00023 -0.00643 C7 1 0.499290 0.612176 0.073502 11.00000 0.02828 0.01593 = 0.04086 0.00464 -0.00139 0.00226 AFIX 23 H7A 2 0.605478 0.569217 0.073372 11.00000 -1.20000 H7B 2 0.558573 0.656307 0.039514 11.00000 -1.20000 AFIX 0 C8 1 0.298879 0.590190 -0.089839 11.00000 0.04615 0.04201 = 0.00945 -0.00409 0.00363 0.00962 AFIX 137 H8A 2 0.423758 0.558148 -0.105058 11.00000 -1.50000 H8B 2 0.329827 0.644797 -0.103210 11.00000 -1.50000 H8C 2 0.173267 0.573108 -0.124252 11.00000 -1.50000 AFIX 0 C9 1 0.072679 0.867002 0.211518 11.00000 0.03571 0.01713 = 0.02115 -0.01128 -0.00859 0.00608 AFIX 23 H9A 2 0.067191 0.837377 0.267408 11.00000 -1.20000 H9B 2 0.226052 0.875435 0.196832 11.00000 -1.20000 AFIX 0 C11 1 -0.261694 0.933817 0.246560 11.00000 0.04848 0.02011 = 0.03834 0.00053 0.02955 0.01154 AFIX 23 H11A 2 -0.270177 0.900197 0.299392 11.00000 -1.20000 H11B 2 -0.320987 0.985287 0.262695 11.00000 -1.20000 AFIX 0 C13 1 -0.335625 0.819378 0.161143 11.00000 0.01736 0.02897 = 0.05751 -0.00249 -0.00231 -0.00302 AFIX 23 H13B 2 -0.434339 0.797635 0.115886 11.00000 -1.20000 H13A 2 -0.353504 0.788608 0.215753 11.00000 -1.20000 AFIX 0 C14 1 -0.061784 0.885187 0.036755 11.00000 0.05027 0.01833 = 0.01964 0.00051 -0.01078 0.00129 AFIX 23 H14A 2 0.086943 0.894724 0.016261 11.00000 -1.20000 H14B 2 -0.147895 0.866456 -0.014178 11.00000 -1.20000 AFIX 0 C16 1 -0.026121 0.989753 0.142334 11.00000 0.02183 0.01946 = 0.03917 -0.00384 0.00576 -0.01180 AFIX 23 H16A 2 -0.076341 1.043139 0.155389 11.00000 -1.20000 H16B 2 0.125806 0.993407 0.123365 11.00000 -1.20000 AFIX 0 C17 1 -0.374990 0.948016 0.098826 11.00000 0.03596 0.03118 = 0.04694 -0.00237 -0.01560 0.00664 AFIX 23 H17A 2 -0.458936 0.923136 0.050774 11.00000 -1.20000 H17B 2 -0.439420 0.999741 0.109859 11.00000 -1.20000 AFIX 0 N10 3 -0.034362 0.943684 0.223891 11.00000 0.03563 0.01749 = 0.02110 -0.00091 -0.00808 0.00529 N12 3 -0.396288 0.900799 0.178669 11.00000 0.03036 0.02052 = 0.05532 -0.00300 0.00836 0.00017 N15 3 -0.154637 0.958855 0.069255 11.00000 0.03917 0.00948 = 0.02510 0.00349 -0.00799 -0.00018 P1 4 -0.057040 0.809510 0.123039 11.00000 0.01912 0.01713 = 0.01732 0.00177 -0.00005 0.00019 S1 5 0.243380 0.580121 0.025889 11.00000 0.02914 0.02081 = 0.02240 -0.00258 0.00058 0.00354 CL1 6 -0.132899 0.711292 -0.059898 11.00000 0.02858 0.02491 = 0.01710 0.00299 -0.00435 0.00007 PD1 7 0.066060 0.693349 0.074819 11.00000 0.01934 0.01741 = 0.01575 0.00046 -0.00016 0.00096 HKLF 4 Covalent radii and connectivity table for 2009src0216r in P2(1)/c C 0.770 H 0.320 N 0.700 P 1.100 S 1.030 CL 0.990 PD 1.380 C1 - C2 C6 Pd1 C2 - C1 C3 C3 - C4 C2 C4 - C3 C5 C5 - C4 C6 C6 - C1 C5 C7 C7 - C6 S1 C8 - S1 C9 - N10 P1 C11 - N12 N10 C13 - N12 P1 C14 - N15 P1 C16 - N15 N10 C17 - N15 N12 N10 - C11 C16 C9 N12 - C11 C17 C13 N15 - C17 C16 C14 P1 - C13 C14 C9 Pd1 S1 - C8 C7 Pd1 Cl1 - Pd1 Pd1 - C1 P1 S1 Cl1 18947 Reflections read, of which 3014 rejected -7 =< h =< 7, -20 =< k =< 19, -18 =< l =< 17, Max. 2-theta = 49.99 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 0 9 6 -1.52 0.42 8 12.69 1 Inconsistent equivalents 2837 Unique reflections, of which 0 suppressed R(int) = 0.1108 R(sigma) = 0.0836 Friedel opposites merged Maximum memory for data reduction = 2238 / 28389 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 = 2807 / 239981 wR2 = 0.1527 before cycle 1 for 2837 data and 191 / 191 parameters GooF = S = 1.168; Restrained GooF = 1.168 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 28.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.40489 0.00111 0.000 OSF Mean shift/su = 0.001 Maximum = 0.012 for U13 Pd1 Max. shift = 0.000 A for C6 Max. dU = 0.000 for C2 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2807 / 239981 wR2 = 0.1527 before cycle 2 for 2837 data and 191 / 191 parameters GooF = S = 1.168; Restrained GooF = 1.168 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 28.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.40489 0.00111 -0.002 OSF Mean shift/su = 0.000 Maximum = 0.004 for U13 Pd1 Max. shift = 0.000 A for H8C Max. dU = 0.000 for C2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2807 / 239981 wR2 = 0.1527 before cycle 3 for 2837 data and 191 / 191 parameters GooF = S = 1.168; Restrained GooF = 1.168 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 28.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.40489 0.00111 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for y Pd1 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C3 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2807 / 239981 wR2 = 0.1527 before cycle 4 for 2837 data and 191 / 191 parameters GooF = S = 1.168; Restrained GooF = 1.168 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 28.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.40489 0.00111 0.000 OSF Mean shift/su = 0.000 Maximum = -0.001 for y Pd1 Max. shift = 0.000 A for H8A Max. dU = 0.000 for C11 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.0661 0.7123 0.2822 43 0.950 0.000 C2 C1 C3 H3 0.3219 0.6946 0.3942 43 0.950 0.000 C3 C4 C2 H4 0.6484 0.6388 0.3643 43 0.950 0.000 C4 C3 C5 H5 0.7331 0.5959 0.2232 43 0.950 0.000 C5 C4 C6 H7A 0.6055 0.5692 0.0734 23 0.990 0.000 C7 C6 S1 H7B 0.5586 0.6563 0.0395 23 0.990 0.000 C7 C6 S1 H8A 0.4238 0.5581 -0.1051 137 0.980 0.000 C8 S1 H8A H8B 0.3298 0.6448 -0.1032 137 0.980 0.000 C8 S1 H8A H8C 0.1733 0.5731 -0.1243 137 0.980 0.000 C8 S1 H8A H9A 0.0672 0.8374 0.2674 23 0.990 0.000 C9 N10 P1 H9B 0.2261 0.8754 0.1968 23 0.990 0.000 C9 N10 P1 H11A -0.2702 0.9002 0.2994 23 0.990 0.000 C11 N12 N10 H11B -0.3210 0.9853 0.2627 23 0.990 0.000 C11 N12 N10 H13B -0.4343 0.7976 0.1159 23 0.990 0.000 C13 N12 P1 H13A -0.3535 0.7886 0.2158 23 0.990 0.000 C13 N12 P1 H14A 0.0869 0.8947 0.0163 23 0.990 0.000 C14 N15 P1 H14B -0.1479 0.8665 -0.0142 23 0.990 0.000 C14 N15 P1 H16A -0.0763 1.0431 0.1554 23 0.990 0.000 C16 N15 N10 H16B 0.1258 0.9934 0.1234 23 0.990 0.000 C16 N15 N10 H17A -0.4589 0.9231 0.0508 23 0.990 0.000 C17 N15 N12 H17B -0.4394 0.9997 0.1099 23 0.990 0.000 C17 N15 N12 2009src0216r in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.25396 0.67384 0.18322 1.00000 0.01647 0.01489 0.01742 0.00090 -0.00421 0.00106 0.01628 0.01651 0.00150 0.00055 0.00063 0.00000 0.00490 0.00551 0.00517 0.00413 0.00419 0.00390 0.00218 C2 0.20383 0.69161 0.26868 1.00000 0.03168 0.02405 0.01499 0.00661 -0.00439 -0.00820 0.02359 0.01746 0.00168 0.00065 0.00062 0.00000 0.00568 0.00577 0.00508 0.00494 0.00440 0.00515 0.00229 H2 0.06609 0.71231 0.28222 1.00000 0.02831 0.00000 0.00000 C3 0.35420 0.67938 0.33555 1.00000 0.04099 0.02307 0.02416 0.00389 -0.00358 -0.01149 0.02942 0.01876 0.00184 0.00062 0.00074 0.00000 0.00681 0.00655 0.00584 0.00498 0.00522 0.00527 0.00268 H3 0.32188 0.69460 0.39417 1.00000 0.03531 0.00000 0.00000 C4 0.54720 0.64581 0.31769 1.00000 0.05223 0.02475 0.03676 0.00559 -0.02573 -0.00247 0.03805 0.02057 0.00210 0.00068 0.00083 0.00000 0.00829 0.00681 0.00737 0.00569 0.00643 0.00596 0.00315 H4 0.64841 0.63881 0.36431 1.00000 0.04566 0.00000 0.00000 C5 0.60060 0.62165 0.23428 1.00000 0.02258 0.01503 0.06506 0.00822 -0.01419 0.00312 0.03430 0.02042 0.00179 0.00063 0.00088 0.00000 0.00582 0.00592 0.00917 0.00587 0.00597 0.00461 0.00303 H5 0.73312 0.59594 0.22318 1.00000 0.04116 0.00000 0.00000 C6 0.45063 0.63654 0.16554 1.00000 0.02584 0.01872 0.02616 -0.00447 -0.00023 -0.00643 0.02358 0.01774 0.00166 0.00060 0.00070 0.00000 0.00585 0.00579 0.00600 0.00473 0.00483 0.00456 0.00243 C7 0.49929 0.61218 0.07350 1.00000 0.02828 0.01593 0.04086 0.00464 -0.00139 0.00226 0.02836 0.01902 0.00169 0.00063 0.00075 0.00000 0.00613 0.00567 0.00702 0.00510 0.00564 0.00447 0.00267 H7A 0.60548 0.56922 0.07337 1.00000 0.03404 0.00000 0.00000 H7B 0.55857 0.65631 0.03951 1.00000 0.03404 0.00000 0.00000 C8 0.29888 0.59019 -0.08984 1.00000 0.04615 0.04201 0.00945 -0.00409 0.00363 0.00962 0.03252 0.02084 0.00195 0.00071 0.00065 0.00000 0.00727 0.00748 0.00521 0.00514 0.00507 0.00585 0.00285 H8A 0.42376 0.55815 -0.10506 1.00000 0.04878 0.00000 0.00000 H8B 0.32983 0.64480 -0.10321 1.00000 0.04878 0.00000 0.00000 H8C 0.17327 0.57311 -0.12425 1.00000 0.04878 0.00000 0.00000 C9 0.07268 0.86700 0.21152 1.00000 0.03571 0.01713 0.02115 -0.01128 -0.00859 0.00608 0.02471 0.01749 0.00178 0.00060 0.00069 0.00000 0.00626 0.00574 0.00560 0.00461 0.00490 0.00469 0.00247 H9A 0.06719 0.83738 0.26741 1.00000 0.02965 0.00000 0.00000 H9B 0.22605 0.87543 0.19683 1.00000 0.02965 0.00000 0.00000 C11 -0.26169 0.93382 0.24656 1.00000 0.04848 0.02011 0.03834 0.00053 0.02955 0.01154 0.03549 0.02285 0.00193 0.00067 0.00079 0.00000 0.00756 0.00624 0.00695 0.00543 0.00625 0.00542 0.00311 H11A -0.27018 0.90020 0.29939 1.00000 0.04259 0.00000 0.00000 H11B -0.32099 0.98529 0.26270 1.00000 0.04259 0.00000 0.00000 C13 -0.33563 0.81938 0.16114 1.00000 0.01736 0.02897 0.05751 -0.00249 -0.00231 -0.00302 0.03463 0.02045 0.00164 0.00067 0.00088 0.00000 0.00545 0.00701 0.00813 0.00607 0.00544 0.00483 0.00295 H13B -0.43434 0.79763 0.11589 1.00000 0.04155 0.00000 0.00000 H13A -0.35350 0.78861 0.21575 1.00000 0.04155 0.00000 0.00000 C14 -0.06178 0.88519 0.03676 1.00000 0.05027 0.01833 0.01964 0.00051 -0.01078 0.00129 0.02947 0.01957 0.00201 0.00061 0.00070 0.00000 0.00737 0.00593 0.00572 0.00474 0.00536 0.00521 0.00268 H14A 0.08694 0.89472 0.01626 1.00000 0.03537 0.00000 0.00000 H14B -0.14789 0.86646 -0.01418 1.00000 0.03537 0.00000 0.00000 C16 -0.02612 0.98975 0.14233 1.00000 0.02183 0.01946 0.03917 -0.00384 0.00576 -0.01180 0.02679 0.01806 0.00171 0.00062 0.00073 0.00000 0.00567 0.00584 0.00674 0.00521 0.00507 0.00457 0.00256 H16A -0.07634 1.04314 0.15539 1.00000 0.03215 0.00000 0.00000 H16B 0.12581 0.99341 0.12337 1.00000 0.03215 0.00000 0.00000 C17 -0.37499 0.94802 0.09883 1.00000 0.03596 0.03118 0.04694 -0.00237 -0.01560 0.00664 0.03811 0.02148 0.00191 0.00071 0.00084 0.00000 0.00711 0.00728 0.00787 0.00599 0.00601 0.00546 0.00308 H17A -0.45894 0.92314 0.05077 1.00000 0.04573 0.00000 0.00000 H17B -0.43942 0.99974 0.10986 1.00000 0.04573 0.00000 0.00000 N10 -0.03436 0.94368 0.22389 1.00000 0.03563 0.01749 0.02110 -0.00091 -0.00808 0.00529 0.02478 0.01501 0.00145 0.00049 0.00055 0.00000 0.00542 0.00486 0.00476 0.00396 0.00411 0.00395 0.00208 N12 -0.39629 0.90080 0.17867 1.00000 0.03036 0.02052 0.05532 -0.00300 0.00836 0.00017 0.03536 0.01782 0.00151 0.00053 0.00072 0.00000 0.00541 0.00538 0.00692 0.00494 0.00505 0.00420 0.00249 N15 -0.15464 0.95886 0.06925 1.00000 0.03917 0.00948 0.02510 0.00349 -0.00799 -0.00018 0.02462 0.01517 0.00148 0.00047 0.00058 0.00000 0.00551 0.00440 0.00487 0.00383 0.00423 0.00389 0.00205 P1 -0.05704 0.80951 0.12304 1.00000 0.01912 0.01713 0.01732 0.00177 -0.00005 0.00019 0.01786 0.00453 0.00039 0.00016 0.00016 0.00000 0.00126 0.00137 0.00129 0.00118 0.00103 0.00115 0.00056 S1 0.24338 0.58012 0.02589 1.00000 0.02914 0.02081 0.02240 -0.00258 0.00058 0.00354 0.02412 0.00474 0.00043 0.00016 0.00017 0.00000 0.00146 0.00146 0.00141 0.00118 0.00116 0.00116 0.00062 Cl1 -0.13290 0.71129 -0.05990 1.00000 0.02858 0.02491 0.01710 0.00299 -0.00435 0.00007 0.02356 0.00439 0.00041 0.00015 0.00016 0.00000 0.00135 0.00148 0.00128 0.00107 0.00105 0.00106 0.00060 Pd1 0.06606 0.69335 0.07482 1.00000 0.01934 0.01741 0.01575 0.00046 -0.00016 0.00096 0.01750 0.00137 0.00012 0.00005 0.00005 0.00000 0.00039 0.00041 0.00039 0.00037 0.00029 0.00036 0.00023 Final Structure Factor Calculation for 2009src0216r in P2(1)/c Total number of l.s. parameters = 191 Maximum vector length = 511 Memory required = 2616 / 26061 wR2 = 0.1527 before cycle 5 for 2837 data and 0 / 191 parameters GooF = S = 1.168; Restrained GooF = 1.168 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0000 * P )^2 + 28.40 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0780 for 2098 Fo > 4sig(Fo) and 0.1154 for all 2837 data wR2 = 0.1527, GooF = S = 1.168, Restrained GooF = 1.168 for all data Occupancy sum of asymmetric unit = 21.00 for non-hydrogen and 21.00 for hydrogen atoms Principal mean square atomic displacements U 0.0213 0.0155 0.0120 C1 0.0393 0.0200 0.0115 C2 0.0478 0.0236 0.0169 C3 0.0725 0.0253 0.0164 C4 0.0705 0.0219 0.0105 C5 0.0307 0.0265 0.0136 C6 0.0418 0.0286 0.0146 C7 0.0539 0.0353 0.0083 C8 0.0442 0.0223 0.0076 C9 0.0744 0.0234 0.0086 C11 0.0579 0.0296 0.0164 C13 0.0540 0.0186 0.0158 C14 0.0432 0.0284 0.0088 C16 0.0596 0.0321 0.0226 C17 0.0406 0.0183 0.0154 N10 0.0578 0.0281 0.0202 N12 0.0431 0.0221 0.0087 N15 0.0191 0.0190 0.0154 P1 0.0305 0.0239 0.0180 S1 0.0304 0.0255 0.0148 Cl1 0.0197 0.0172 0.0156 Pd1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.023 0.045 0.069 0.092 0.123 0.154 0.188 0.237 0.315 1.000 Number in group 292. 281. 285. 282. 289. 280. 275. 287. 280. 286. GooF 1.310 1.272 1.286 1.265 1.141 1.107 1.135 1.195 1.018 0.876 K 9.093 2.137 1.301 1.162 1.015 1.031 1.019 1.005 1.002 1.007 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.06 1.14 1.25 1.44 1.81 inf Number in group 286. 295. 273. 286. 282. 279. 283. 287. 282. 284. GooF 1.297 1.274 1.203 1.221 1.242 1.109 1.152 1.006 1.068 1.068 K 1.134 1.111 1.038 1.030 1.037 1.020 1.005 1.010 0.997 1.009 R1 0.241 0.227 0.180 0.146 0.128 0.101 0.096 0.071 0.053 0.038 Recommended weighting scheme: WGHT 0.0000 28.4158 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)/su Fc/Fc(max) Resolution(A) 3 1 4 1753.01 274.11 5.18 0.068 1.80 2 7 10 613.86 14.74 3.62 0.016 1.19 1 1 13 548.41 2.96 3.62 0.007 1.14 1 8 5 432.04 0.52 3.49 0.003 1.69 0 12 8 1613.54 2808.53 3.48 0.218 1.14 -4 7 12 660.20 2155.68 3.45 0.191 0.91 -2 16 1 620.38 0.28 3.45 0.002 1.01 -2 7 15 550.39 1487.57 3.44 0.159 0.90 3 10 8 1107.63 2343.70 3.24 0.199 1.08 -2 16 5 -71.60 691.15 3.19 0.108 0.96 -7 2 2 850.21 104.24 3.12 0.042 0.88 3 16 6 3219.69 1869.69 3.10 0.178 0.89 0 7 11 885.46 255.08 3.09 0.066 1.20 3 15 9 -6.03 1026.75 3.04 0.132 0.86 -6 7 8 2044.26 3606.34 2.99 0.247 0.85 6 1 1 1223.52 2100.95 2.93 0.189 1.03 -3 15 1 1497.38 416.36 2.93 0.084 1.00 4 7 12 1102.59 2259.20 2.89 0.195 0.91 3 1 7 367.99 1.74 2.88 0.005 1.49 -5 12 7 1218.99 427.22 2.82 0.085 0.86 3 0 14 2086.69 38.34 2.81 0.025 0.96 -3 3 11 2766.55 1717.48 2.74 0.170 1.13 3 4 10 619.03 122.78 2.72 0.046 1.17 -4 1 12 6034.68 4431.95 2.72 0.274 0.98 1 9 12 819.75 29.22 2.71 0.022 1.04 0 1 6 1420.79 436.83 2.71 0.086 2.50 -1 7 14 707.34 84.63 2.70 0.038 0.98 -5 9 1 98.73 512.46 2.69 0.093 1.04 5 5 7 5680.94 7567.59 2.67 0.358 1.02 1 13 1 660.09 140.25 2.67 0.049 1.29 2 3 15 554.23 66.84 2.65 0.034 0.95 -3 3 10 730.78 1484.10 2.65 0.158 1.20 3 2 11 544.77 98.87 2.65 0.041 1.13 2 15 4 670.27 1312.74 2.64 0.149 1.03 7 1 5 937.81 199.83 2.64 0.058 0.85 -1 5 16 612.50 73.72 2.63 0.035 0.91 -5 5 7 278.25 47.48 2.60 0.028 1.03 -1 18 8 1673.17 411.44 2.60 0.083 0.85 -2 1 1 533.80 192.52 2.59 0.057 3.00 4 7 7 1903.06 2962.96 2.58 0.224 1.12 2 16 2 1086.46 347.06 2.58 0.077 1.01 1 2 11 822.30 364.46 2.57 0.079 1.33 -2 13 12 731.23 0.40 2.57 0.003 0.88 -7 5 1 488.90 40.51 2.55 0.026 0.86 5 10 2 2360.21 1570.08 2.53 0.163 1.00 4 1 9 347.55 3.33 2.52 0.008 1.13 -1 8 11 1351.41 615.38 2.52 0.102 1.14 1 13 11 7729.95 5659.14 2.51 0.309 0.94 4 2 13 963.40 1673.91 2.51 0.168 0.92 -5 2 11 747.86 191.10 2.50 0.057 0.92 Bond lengths and angles C1 - Distance Angles C2 1.3702 (0.0135) C6 1.4066 (0.0138) 119.07 (0.92) Pd1 2.0366 (0.0095) 126.48 (0.74) 114.43 (0.71) C1 - C2 C6 C2 - Distance Angles C1 1.3702 (0.0135) C3 1.3891 (0.0145) 120.08 (1.02) H2 0.9500 119.96 119.96 C2 - C1 C3 C3 - Distance Angles C4 1.3589 (0.0165) C2 1.3891 (0.0145) 120.46 (1.08) H3 0.9500 119.77 119.77 C3 - C4 C2 C4 - Distance Angles C3 1.3589 (0.0165) C5 1.3750 (0.0172) 122.07 (1.11) H4 0.9500 118.97 118.97 C4 - C3 C5 C5 - Distance Angles C4 1.3750 (0.0172) C6 1.4158 (0.0154) 117.49 (1.06) H5 0.9500 121.26 121.26 C5 - C4 C6 C6 - Distance Angles C1 1.4066 (0.0138) C5 1.4158 (0.0154) 120.57 (0.99) C7 1.4909 (0.0149) 119.28 (0.94) 120.15 (1.00) C6 - C1 C5 C7 - Distance Angles C6 1.4909 (0.0149) S1 1.8250 (0.0110) 105.88 (0.72) H7A 0.9900 110.56 110.56 H7B 0.9900 110.56 110.56 108.71 C7 - C6 S1 H7A C8 - Distance Angles S1 1.8002 (0.0101) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - S1 H8A H8B C9 - Distance Angles N10 1.4891 (0.0129) P1 1.8468 (0.0101) 111.92 (0.69) H9A 0.9900 109.23 109.23 H9B 0.9900 109.23 109.23 107.92 C9 - N10 P1 H9A C11 - Distance Angles N12 1.4380 (0.0159) N10 1.4647 (0.0141) 115.65 (0.87) H11A 0.9900 108.37 108.37 H11B 0.9900 108.37 108.37 107.44 C11 - N12 N10 H11A C13 - Distance Angles N12 1.4746 (0.0141) P1 1.8352 (0.0105) 112.77 (0.75) H13B 0.9900 109.04 109.04 H13A 0.9900 109.04 109.04 107.81 C13 - N12 P1 H13B C14 - Distance Angles N15 1.4780 (0.0134) P1 1.8459 (0.0107) 111.83 (0.73) H14A 0.9900 109.25 109.25 H14B 0.9900 109.25 109.25 107.93 C14 - N15 P1 H14A C16 - Distance Angles N15 1.4609 (0.0135) N10 1.4704 (0.0135) 114.86 (0.81) H16A 0.9900 108.55 108.55 H16B 0.9900 108.55 108.55 107.54 C16 - N15 N10 H16A C17 - Distance Angles N15 1.4546 (0.0149) N12 1.4651 (0.0154) 114.65 (0.92) H17A 0.9900 108.60 108.60 H17B 0.9900 108.60 108.60 107.57 C17 - N15 N12 H17A N10 - Distance Angles C11 1.4647 (0.0142) C16 1.4704 (0.0135) 107.45 (0.84) C9 1.4891 (0.0129) 111.01 (0.86) 110.64 (0.83) N10 - C11 C16 N12 - Distance Angles C11 1.4380 (0.0159) C17 1.4651 (0.0154) 108.53 (0.90) C13 1.4746 (0.0141) 110.88 (0.95) 110.63 (0.97) N12 - C11 C17 N15 - Distance Angles C17 1.4546 (0.0149) C16 1.4609 (0.0135) 108.77 (0.86) C14 1.4780 (0.0134) 111.29 (0.89) 110.66 (0.86) N15 - C17 C16 P1 - Distance Angles C13 1.8352 (0.0106) C14 1.8459 (0.0107) 98.53 (0.57) C9 1.8468 (0.0101) 97.36 (0.54) 98.19 (0.51) Pd1 2.2622 (0.0028) 120.32 (0.39) 113.38 (0.36) 124.15 (0.35) P1 - C13 C14 C9 S1 - Distance Angles C8 1.8002 (0.0101) C7 1.8250 (0.0111) 100.63 (0.55) Pd1 2.3592 (0.0027) 108.71 (0.40) 91.88 (0.36) S1 - C8 C7 Cl1 - Distance Angles Pd1 2.3997 (0.0026) Cl1 - Pd1 - Distance Angles C1 2.0366 (0.0095) P1 2.2622 (0.0028) 94.42 (0.27) S1 2.3592 (0.0027) 81.52 (0.28) 171.90 (0.10) Cl1 2.3997 (0.0026) 175.32 (0.28) 89.37 (0.09) 94.38 (0.09) Pd1 - C1 P1 S1 FMAP and GRID set by program FMAP 2 1 16 GRID -3.846 24 -2 3.846 1 2 R1 = 0.1135 for 2837 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.85 at 0.0726 0.7459 0.5783 [ 1.05 A from PD1 ] Deepest hole -0.78 at 0.1659 0.6753 0.4633 [ 1.47 A from H3 ] Mean = 0.00, Rms deviation from mean = 0.21 e/A^3, Highest memory used = 3031 / 26857 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0726 0.7541 0.0783 1.00000 0.05 0.85 1.05 PD1 1.42 P1 2.38 C1 2.48 C14 Q2 1 0.0280 0.6051 -0.1047 1.00000 0.05 0.82 1.10 H8C 1.71 C8 1.99 H8B 2.19 CL1 Q3 1 -0.1782 0.6681 -0.0356 1.00000 0.05 0.78 0.88 CL1 2.01 H7B 2.29 PD1 2.73 H7A Q4 1 -0.4388 0.7680 0.0622 1.00000 0.05 0.76 0.96 H13B 1.85 C13 1.95 H7B 2.41 H13A Q5 1 -0.3266 0.7672 0.0380 1.00000 0.05 0.74 1.46 H13B 2.04 H7B 2.07 C13 2.14 CL1 Q6 1 -0.3756 0.8012 0.1003 1.00000 0.05 0.72 0.44 H13B 1.00 C13 1.77 H13A 2.01 P1 Q7 1 -0.1181 0.8008 -0.0670 1.00000 0.05 0.72 1.40 H14B 1.55 CL1 2.06 H4 2.17 C14 Q8 1 0.6480 0.5134 0.1848 1.00000 0.05 0.72 1.62 H5 1.78 H8A 1.96 H7A 2.03 C5 Q9 1 0.1834 0.5981 -0.0569 1.00000 0.05 0.71 0.89 C8 1.11 H8C 1.34 S1 1.40 H8B Q10 1 -0.0712 0.7002 0.0843 1.00000 0.05 0.70 0.87 PD1 1.97 P1 2.23 CL1 2.51 H7B Shortest distances between peaks (including symmetry equivalents) 4 5 0.79 4 6 0.90 5 6 1.15 2 9 1.21 1 10 1.29 2 3 1.98 3 10 2.01 5 10 2.08 5 7 2.14 3 5 2.24 3 7 2.36 1 5 2.56 3 9 2.57 6 10 2.58 4 10 2.58 1 7 2.62 1 3 2.75 3 4 2.79 4 7 2.86 7 10 2.89 1 6 2.92 8 9 2.93 Time profile in seconds ----------------------- 0.03: 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. 0.88: 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 0.02: Generate idealized H-atoms 0.64: Structure factors and derivatives 0.72: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.09: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.09: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0216r finished at 13:02:16 Total CPU time: 2.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++