+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 15:32:42 on 04-Apr-2002 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 02SRC143 in P2(1)/c CELL 0.71073 14.7341 11.2352 19.3377 90.000 111.878 90.000 ZERR 4.00 0.0002 0.0002 0.0003 0.000 0.001 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O F P PD UNIT 116 180 4 8 12 4 4 V = 2970.62 F(000) = 1320.0 Mu = 0.72 mm-1 Cell Wt = 2536.12 Rho = 1.418 MERG 2 FMAP 2 ISOR F1 F2 F3 PLAN 10 BOND $H OMIT -3 55 OMIT 2 0 0 OMIT -2 0 2 OMIT -3 1 2 OMIT -1 4 8 TEMP -153 SIZE 0.25 0.25 0.2 ACTA WGHT 0.03440 2.11820 L.S. 4 FVAR 0.44630 C1 1 0.374504 0.492600 0.459724 11.00000 0.01639 0.05097 = 0.01497 -0.00921 -0.00288 0.00609 AFIX 137 H1A 2 0.385763 0.548453 0.499637 11.00000 -1.50000 H1B 2 0.421262 0.505659 0.436751 11.00000 -1.50000 H1C 2 0.381389 0.413032 0.479106 11.00000 -1.50000 AFIX 0 C2 1 0.203349 0.478853 0.438348 11.00000 0.02304 0.04294 = 0.01401 0.00237 0.01057 0.00810 AFIX 137 H2A 2 0.209628 0.396214 0.451943 11.00000 -1.50000 H2B 2 0.138258 0.494039 0.403481 11.00000 -1.50000 H2C 2 0.215916 0.526718 0.482067 11.00000 -1.50000 AFIX 0 C3 1 0.261915 0.634493 0.377070 11.00000 0.01825 0.02527 = 0.01944 -0.00926 0.00694 -0.00298 AFIX 23 H3A 2 0.317624 0.658718 0.365200 11.00000 -1.20000 H3B 2 0.257839 0.686679 0.415769 11.00000 -1.20000 AFIX 0 C4 1 0.170223 0.643618 0.309186 11.00000 0.01658 0.01948 = 0.01449 -0.00248 0.00805 -0.00185 C5 1 0.108896 0.742394 0.294127 11.00000 0.02878 0.01723 = 0.01978 -0.00254 0.01433 0.00117 AFIX 43 H5 2 0.126294 0.808509 0.325260 11.00000 -1.20000 AFIX 0 C6 1 0.021418 0.742114 0.232365 11.00000 0.02783 0.02059 = 0.01975 0.00512 0.01223 0.00957 AFIX 43 H6 2 -0.019077 0.808614 0.221408 11.00000 -1.20000 AFIX 0 C7 1 -0.004761 0.642275 0.187481 11.00000 0.01849 0.02482 = 0.01687 0.00550 0.00662 0.00750 AFIX 43 H7 2 -0.064410 0.640518 0.147457 11.00000 -1.20000 AFIX 0 C8 1 0.057889 0.543595 0.201801 11.00000 0.01557 0.01672 = 0.01427 0.00054 0.00558 0.00232 AFIX 43 H8 2 0.039341 0.477102 0.171070 11.00000 -1.20000 AFIX 0 C9 1 0.147695 0.543941 0.261574 11.00000 0.01355 0.01566 = 0.01324 0.00020 0.00671 0.00202 C10 1 0.335278 0.211988 0.392577 11.00000 0.02598 0.02378 = 0.01503 0.00479 0.00651 0.00817 C11 1 0.421121 0.126762 0.433082 11.00000 0.04047 0.04052 = 0.02127 0.01326 0.01427 0.02140 C12 1 0.384637 0.329020 0.209167 11.00000 0.01242 0.01441 = 0.01565 0.00147 0.00527 0.00017 AFIX 13 H12 2 0.398714 0.257527 0.240438 11.00000 -1.20000 AFIX 0 C13 1 0.455633 0.423966 0.256795 11.00000 0.01544 0.01969 = 0.02392 -0.00199 0.00497 -0.00251 AFIX 23 H13A 2 0.451962 0.494651 0.227067 11.00000 -1.20000 H13B 2 0.437570 0.445883 0.298473 11.00000 -1.20000 AFIX 0 C14 1 0.560275 0.374763 0.285749 11.00000 0.01509 0.03105 = 0.02995 0.00141 0.00211 -0.00258 AFIX 23 H14A 2 0.605002 0.435705 0.314643 11.00000 -1.20000 H14B 2 0.564568 0.307655 0.318380 11.00000 -1.20000 AFIX 0 C15 1 0.590601 0.335161 0.222151 11.00000 0.01503 0.03043 = 0.03720 0.01239 0.01080 0.00512 AFIX 23 H15A 2 0.595055 0.404124 0.193403 11.00000 -1.20000 H15B 2 0.654685 0.298302 0.242444 11.00000 -1.20000 AFIX 0 C16 1 0.517187 0.246828 0.171200 11.00000 0.02061 0.03071 = 0.02986 0.00257 0.01287 0.01018 AFIX 23 H16A 2 0.519522 0.173466 0.198257 11.00000 -1.20000 H16B 2 0.535260 0.228531 0.129004 11.00000 -1.20000 AFIX 0 C17 1 0.412711 0.296309 0.142863 11.00000 0.01687 0.02951 = 0.01917 0.00036 0.00921 0.00366 AFIX 23 H17A 2 0.367612 0.237109 0.112273 11.00000 -1.20000 H17B 2 0.408631 0.366286 0.112466 11.00000 -1.20000 AFIX 0 C18 1 0.193167 0.221094 0.147890 11.00000 0.01400 0.01130 = 0.01404 -0.00128 0.00554 -0.00105 AFIX 13 H18 2 0.217349 0.197667 0.109031 11.00000 -1.20000 AFIX 0 C19 1 0.219510 0.120837 0.206302 11.00000 0.01800 0.01407 = 0.02184 0.00428 0.00250 -0.00031 AFIX 23 H19A 2 0.290011 0.111757 0.228176 11.00000 -1.20000 H19B 2 0.196792 0.141810 0.245783 11.00000 -1.20000 AFIX 0 C20 1 0.173008 0.003292 0.170983 11.00000 0.02151 0.01182 = 0.03254 0.00212 0.00753 -0.00125 AFIX 23 H20A 2 0.200612 -0.021468 0.134909 11.00000 -1.20000 H20B 2 0.188036 -0.057517 0.209236 11.00000 -1.20000 AFIX 0 C21 1 0.062190 0.014815 0.132376 11.00000 0.01959 0.01519 = 0.02706 0.00001 0.00724 -0.00314 AFIX 23 H21A 2 0.033615 0.030877 0.169216 11.00000 -1.20000 H21B 2 0.035254 -0.059519 0.107752 11.00000 -1.20000 AFIX 0 C22 1 0.036116 0.115393 0.075071 11.00000 0.01666 0.01870 = 0.02070 -0.00065 0.00279 -0.00411 AFIX 23 H22A 2 0.059622 0.095689 0.035822 11.00000 -1.20000 H22B 2 -0.034424 0.123680 0.052732 11.00000 -1.20000 AFIX 0 C23 1 0.081299 0.233327 0.111060 11.00000 0.01381 0.01507 = 0.01944 0.00142 0.00499 -0.00032 AFIX 23 H23A 2 0.054908 0.255804 0.148259 11.00000 -1.20000 H23B 2 0.064858 0.295314 0.073468 11.00000 -1.20000 AFIX 0 C24 1 0.208168 0.473535 0.114106 11.00000 0.01594 0.01085 = 0.01381 0.00107 0.00677 0.00090 AFIX 13 H24 2 0.139843 0.487040 0.107854 11.00000 -1.20000 AFIX 0 C25 1 0.258647 0.594596 0.137399 11.00000 0.02578 0.01345 = 0.01449 -0.00011 0.00610 -0.00379 AFIX 23 H25A 2 0.261221 0.615197 0.186808 11.00000 -1.20000 H25B 2 0.325156 0.590174 0.139016 11.00000 -1.20000 AFIX 0 C26 1 0.202103 0.690191 0.081693 11.00000 0.03189 0.01409 = 0.02669 0.00385 0.01083 0.00125 AFIX 23 H26A 2 0.235535 0.765951 0.095646 11.00000 -1.20000 H26B 2 0.137255 0.698632 0.083023 11.00000 -1.20000 AFIX 0 C27 1 0.193444 0.657554 0.002860 11.00000 0.02682 0.01975 = 0.01983 0.00910 0.00869 0.00241 AFIX 23 H27A 2 0.153036 0.716189 -0.031836 11.00000 -1.20000 H27B 2 0.257851 0.659572 0.000149 11.00000 -1.20000 AFIX 0 C28 1 0.148935 0.534325 -0.020034 11.00000 0.02306 0.02385 = 0.01267 0.00283 0.00385 0.00228 AFIX 23 H28A 2 0.149894 0.514423 -0.068567 11.00000 -1.20000 H28B 2 0.081279 0.535374 -0.024163 11.00000 -1.20000 AFIX 0 C29 1 0.204882 0.438927 0.036453 11.00000 0.02215 0.01635 = 0.01190 0.00025 0.00753 0.00206 AFIX 23 H29A 2 0.270899 0.431884 0.037292 11.00000 -1.20000 H29B 2 0.172673 0.362534 0.022066 11.00000 -1.20000 AFIX 0 N1 3 0.274552 0.509010 0.403785 11.00000 0.01247 0.02985 = 0.01105 -0.00419 0.00389 0.00379 O1 4 0.357502 0.286781 0.352575 11.00000 0.01804 0.02496 = 0.01407 0.00652 0.00561 0.00787 O2 4 0.260321 0.200561 0.404876 11.00000 0.03180 0.03855 = 0.03854 0.01687 0.01991 0.00834 F1 5 0.472046 0.095108 0.392208 11.00000 0.04070 0.03947 = 0.03288 0.00623 0.01807 0.02126 F2 5 0.393130 0.029304 0.455875 11.00000 0.08318 0.07178 = 0.13353 0.08177 0.07293 0.05015 F3 5 0.484208 0.180807 0.493368 11.00000 0.07814 0.09963 = 0.02886 -0.01344 -0.01784 0.05947 P1 6 0.254064 0.361930 0.188857 11.00000 0.01145 0.01058 = 0.00974 0.00004 0.00389 0.00015 PD1 7 0.248344 0.416613 0.299727 11.00000 0.01052 0.01614 = 0.00827 0.00042 0.00307 0.00200 HKLF 4 Covalent radii and connectivity table for 02SRC143 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 F 0.640 P 1.100 PD 1.380 C1 - N1 C2 - N1 C3 - N1 C4 C4 - C5 C9 C3 C5 - C4 C6 C6 - C7 C5 C7 - C6 C8 C8 - C9 C7 C9 - C8 C4 Pd1 C10 - O2 O1 C11 C11 - F2 F1 F3 C10 C12 - C17 C13 P1 C13 - C14 C12 C14 - C15 C13 C15 - C14 C16 C16 - C15 C17 C17 - C12 C16 C18 - C23 C19 P1 C19 - C20 C18 C20 - C19 C21 C21 - C20 C22 C22 - C21 C23 C23 - C22 C18 C24 - C29 C25 P1 C25 - C26 C24 C26 - C27 C25 C27 - C28 C26 C28 - C27 C29 C29 - C28 C24 N1 - C2 C1 C3 Pd1 O1 - C10 Pd1 O2 - C10 F1 - C11 F2 - C11 F3 - C11 P1 - C24 C18 C12 Pd1 Pd1 - C9 O1 N1 P1 h k l Fo^2 Sigma Why rejected -10 0 1 12.44 2.49 observed but should be systematically absent -8 0 5 8.73 1.25 observed but should be systematically absent -8 0 7 4.93 1.23 observed but should be systematically absent -8 0 11 4.89 1.22 observed but should be systematically absent -6 0 7 7.38 1.23 observed but should be systematically absent -5 0 1 11.19 1.24 observed but should be systematically absent 4 0 7 7.27 1.21 observed but should be systematically absent 2 0 9 9.69 2.42 observed but should be systematically absent 0 0 13 13.33 2.42 observed but should be systematically absent 1 0 3 6.03 1.21 observed but should be systematically absent 2 0 7 4.84 1.21 observed but should be systematically absent 2 0 9 13.32 2.42 observed but should be systematically absent -3 0 1 11.21 2.49 observed but should be systematically absent 3 0 1 44.62 2.48 observed but should be systematically absent 3 0 5 7.28 1.21 observed but should be systematically absent -4 0 1 72.16 4.98 observed but should be systematically absent 4 0 1 7.45 1.24 observed but should be systematically absent 5 0 1 4.97 1.24 observed but should be systematically absent -7 0 13 5.01 1.25 observed but should be systematically absent -9 0 7 16.04 1.23 observed but should be systematically absent -12 0 5 21.11 2.48 observed but should be systematically absent 17980 Reflections read, of which 541 rejected -19 =< h =< 19, -12 =< k =< 14, -20 =< l =< 25, Max. 2-theta = 54.96 21 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 1 3 0 3340.32 64.69 4 325.78 2 6 0 423.32 5.33 5 48.35 2 7 0 246.74 4.32 4 33.41 1 9 0 1045.03 21.10 4 107.62 1 10 0 167.73 1.88 4 29.47 -1 2 1 1643.44 21.85 5 174.95 5 3 1 44.15 1.10 3 10.59 -1 4 1 649.74 9.31 5 66.33 -1 5 1 1979.66 37.62 3 406.58 -1 7 1 550.98 11.42 3 96.44 -1 8 1 495.18 8.41 4 66.98 2 8 1 285.83 4.61 5 31.35 2 9 1 155.43 1.16 4 32.82 -1 10 1 309.29 6.50 4 42.65 2 3 2 279.40 5.45 3 32.12 -1 4 2 272.89 4.73 4 36.25 -1 6 2 378.19 6.07 5 33.11 -1 7 2 944.31 16.43 4 125.74 -1 8 2 88.75 1.06 3 26.31 4 8 2 88.24 1.54 5 10.78 2 10 2 50.85 0.99 4 10.16 -1 8 3 3316.90 42.99 6 274.69 0 11 3 338.16 12.95 2 66.79 -3 3 4 470.99 6.93 5 47.26 3 4 4 55.74 1.58 3 21.54 -2 5 4 1125.28 16.62 4 164.95 -5 3 5 14.31 0.56 5 5.04 -3 4 5 1654.43 22.87 5 177.30 1 6 5 9.87 0.62 4 3.39 -1 9 5 31.93 1.05 3 10.82 -1 10 5 329.18 5.98 4 54.52 5 1 6 12.91 0.68 4 4.91 -3 6 6 4003.04 72.86 4 390.06 -2 7 6 187.95 3.52 5 19.09 -2 8 6 176.52 2.86 5 18.68 -4 3 7 10.58 0.83 3 6.00 -3 7 7 234.76 4.49 4 31.25 -2 3 8 86.75 2.02 3 29.76 -4 6 8 1920.78 30.80 5 178.00 4 7 8 24.84 1.57 3 10.30 -3 8 8 267.73 5.51 4 33.68 -2 9 8 381.43 8.17 4 50.12 -5 7 10 1280.70 12.35 5 161.53 -3 9 10 710.87 16.47 4 99.79 -6 7 11 814.98 14.59 4 129.74 -5 8 11 466.43 8.50 4 75.79 -4 9 11 74.40 1.87 4 14.73 -8 7 12 104.94 1.21 3 38.12 -6 8 12 57.97 1.88 4 10.94 -9 7 13 282.26 6.06 4 48.11 ** etc. ** 51 Inconsistent equivalents 6656 Unique reflections, of which 0 suppressed R(int) = 0.0349 R(sigma) = 0.0332 Friedel opposites merged Maximum memory for data reduction = 3973 / 67173 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 = 5011 / 426741 wR2 = 0.0747 before cycle 1 for 6656 data and 336 / 336 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 18. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.100 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.036 0.000 GooF = S = 1.083; Restrained GooF = 1.081 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0344 * P )^2 + 2.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.44715 0.00045 1.893 OSF Mean shift/esd = 0.203 Maximum = 1.893 for OSF Max. shift = 0.006 A for H2C Max. dU = 0.000 for C27 Least-squares cycle 2 Maximum vector length = 511 Memory required = 5011 / 426741 wR2 = 0.0745 before cycle 2 for 6656 data and 336 / 336 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 18. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.100 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.036 0.000 GooF = S = 1.079; Restrained GooF = 1.078 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0344 * P )^2 + 2.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.44741 0.00045 0.581 OSF Mean shift/esd = 0.069 Maximum = 0.581 for OSF Max. shift = 0.002 A for H2C Max. dU = 0.000 for C27 Least-squares cycle 3 Maximum vector length = 511 Memory required = 5011 / 426741 wR2 = 0.0745 before cycle 3 for 6656 data and 336 / 336 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 18. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.100 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.036 0.000 GooF = S = 1.079; Restrained GooF = 1.078 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0344 * P )^2 + 2.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.44741 0.00045 0.010 OSF Mean shift/esd = 0.002 Maximum = 0.014 for x C10 Max. shift = 0.000 A for H2B Max. dU = 0.000 for F3 Least-squares cycle 4 Maximum vector length = 511 Memory required = 5011 / 426741 wR2 = 0.0745 before cycle 4 for 6656 data and 336 / 336 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 18. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.100 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.036 0.000 GooF = S = 1.079; Restrained GooF = 1.078 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0344 * P )^2 + 2.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.44741 0.00045 -0.001 OSF Mean shift/esd = 0.001 Maximum = 0.004 for U22 C5 Max. shift = 0.000 A for H1B Max. dU = 0.000 for C11 Largest correlation matrix elements 0.688 U13 F2 / U11 F2 0.579 U12 F2 / U13 F2 0.513 U13 C6 / U33 C6 0.682 U13 F2 / U33 F2 0.563 U22 Pd1 / OSF 0.507 U13 F1 / U11 F1 0.628 U23 F2 / U22 F2 0.541 z F2 / y F2 0.507 U13 C2 / U33 C2 0.623 U12 F2 / U23 F2 0.540 U13 O2 / U33 O2 0.504 U13 C11 / U11 C11 0.621 U23 F2 / U33 F2 0.530 U13 O2 / U11 O2 0.504 U13 Pd1 / U11 Pd1 0.597 z F2 / x F2 0.528 U12 F3 / U22 F3 0.502 U13 C4 / U11 C4 0.596 U33 Pd1 / OSF 0.526 U13 C5 / U11 C5 0.502 U13 C16 / U11 C16 0.590 U11 Pd1 / OSF 0.525 U13 C5 / U33 C5 0.501 U13 Pd1 / U33 Pd1 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.3860 0.5496 0.5005 137 0.980 0.000 C1 N1 H1A H1B 0.4222 0.5062 0.4363 137 0.980 0.000 C1 N1 H1A H1C 0.3816 0.4114 0.4794 137 0.980 0.000 C1 N1 H1A H2A 0.2094 0.3943 0.4518 137 0.980 0.000 C2 N1 H2A H2B 0.1369 0.4950 0.4030 137 0.980 0.000 C2 N1 H2A H2C 0.2166 0.5272 0.4833 137 0.980 0.000 C2 N1 H2A H3A 0.3188 0.6593 0.3650 23 0.990 0.000 C3 N1 C4 H3B 0.2577 0.6878 0.4166 23 0.990 0.000 C3 N1 C4 H5 0.1267 0.8098 0.3260 43 0.950 0.000 C5 C4 C6 H6 -0.0199 0.8100 0.2211 43 0.950 0.000 C6 C7 C5 H7 -0.0656 0.6406 0.1466 43 0.950 0.000 C7 C6 C8 H8 0.0389 0.4756 0.1705 43 0.950 0.000 C8 C9 C7 H12 0.3990 0.2561 0.2411 13 1.000 0.000 C12 C17 C13 P1 H13A 0.4519 0.4962 0.2265 23 0.990 0.000 C13 C14 C12 H13B 0.4372 0.4464 0.2993 23 0.990 0.000 C13 C14 C12 H14A 0.6060 0.4370 0.3152 23 0.990 0.000 C14 C15 C13 H14B 0.5648 0.3063 0.3191 23 0.990 0.000 C14 C15 C13 H15A 0.6560 0.2975 0.2429 23 0.990 0.000 C15 C14 C16 H15B 0.5952 0.4055 0.1928 23 0.990 0.000 C15 C14 C16 H16A 0.5195 0.1719 0.1988 23 0.990 0.000 C16 C15 C17 H16B 0.5356 0.2281 0.1281 23 0.990 0.000 C16 C15 C17 H17A 0.4085 0.3677 0.1118 23 0.990 0.000 C17 C12 C16 H17B 0.3667 0.2358 0.1116 23 0.990 0.000 C17 C12 C16 H18 0.2179 0.1973 0.1083 13 1.000 0.000 C18 C23 C19 P1 H19A 0.2915 0.1117 0.2286 23 0.990 0.000 C19 C20 C18 H19B 0.1963 0.1423 0.2466 23 0.990 0.000 C19 C20 C18 H20A 0.1883 -0.0588 0.2101 23 0.990 0.000 C20 C19 C21 H20B 0.2012 -0.0222 0.1342 23 0.990 0.000 C20 C19 C21 H21A 0.0331 0.0312 0.1700 23 0.990 0.000 C21 C20 C22 H21B 0.0347 -0.0610 0.1072 23 0.990 0.000 C21 C20 C22 H22A -0.0358 0.1240 0.0523 23 0.990 0.000 C22 C21 C23 H22B 0.0601 0.0954 0.0350 23 0.990 0.000 C22 C21 C23 H23A 0.0544 0.2562 0.1490 23 0.990 0.000 C23 C22 C18 H23B 0.0646 0.2965 0.0727 23 0.990 0.000 C23 C22 C18 H24 0.1384 0.4873 0.1077 13 1.000 0.000 C24 C29 C25 P1 H25A 0.2613 0.6156 0.1879 23 0.990 0.000 C25 C26 C24 H25B 0.3266 0.5901 0.1391 23 0.990 0.000 C25 C26 C24 H26A 0.1360 0.6989 0.0831 23 0.990 0.000 C26 C27 C25 H26B 0.2363 0.7675 0.0959 23 0.990 0.000 C26 C27 C25 H27A 0.1522 0.7174 -0.0325 23 0.990 0.000 C27 C28 C26 H27B 0.2592 0.6596 0.0002 23 0.990 0.000 C27 C28 C26 H28A 0.1499 0.5139 -0.0696 23 0.990 0.000 C28 C27 C29 H28B 0.0799 0.5353 -0.0243 23 0.990 0.000 C28 C27 C29 H29A 0.2723 0.4318 0.0373 23 0.990 0.000 C29 C28 C24 H29B 0.1721 0.3610 0.0218 23 0.990 0.000 C29 C28 C24 02SRC143 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.37453 0.49267 0.45971 1.00000 0.01654 0.05167 0.01508 -0.00934 -0.00291 0.00600 0.03030 0.00415 0.00014 0.00023 0.00011 0.00000 0.00091 0.00142 0.00091 0.00092 0.00075 0.00090 0.00049 H1A 0.38598 0.54959 0.50049 1.00000 0.04545 0.00000 0.00000 H1B 0.42224 0.50618 0.43625 1.00000 0.04545 0.00000 0.00000 H1C 0.38164 0.41140 0.47943 1.00000 0.04545 0.00000 0.00000 C2 0.20337 0.47881 0.43837 1.00000 0.02313 0.04239 0.01441 0.00254 0.01058 0.00786 0.02561 0.00445 0.00015 0.00021 0.00011 0.00000 0.00097 0.00126 0.00088 0.00084 0.00077 0.00087 0.00044 H2A 0.20942 0.39428 0.45184 1.00000 0.03841 0.00000 0.00000 H2B 0.13694 0.49495 0.40295 1.00000 0.03841 0.00000 0.00000 H2C 0.21658 0.52715 0.48325 1.00000 0.03841 0.00000 0.00000 C3 0.26195 0.63453 0.37711 1.00000 0.01854 0.02487 0.01981 -0.00923 0.00698 -0.00285 0.02112 0.00378 0.00014 0.00018 0.00011 0.00000 0.00088 0.00103 0.00093 0.00078 0.00076 0.00075 0.00040 H3A 0.31885 0.65928 0.36505 1.00000 0.02535 0.00000 0.00000 H3B 0.25772 0.68777 0.41659 1.00000 0.02535 0.00000 0.00000 C4 0.17029 0.64360 0.30916 1.00000 0.01669 0.01991 0.01453 -0.00197 0.00847 -0.00154 0.01628 0.00366 0.00013 0.00017 0.00010 0.00000 0.00082 0.00090 0.00082 0.00069 0.00069 0.00068 0.00035 C5 0.10895 0.74231 0.29413 1.00000 0.02907 0.01673 0.01998 -0.00261 0.01437 0.00092 0.02042 0.00402 0.00014 0.00017 0.00011 0.00000 0.00099 0.00091 0.00090 0.00073 0.00080 0.00076 0.00038 H5 0.12668 0.80982 0.32596 1.00000 0.02450 0.00000 0.00000 C6 0.02149 0.74202 0.23235 1.00000 0.02822 0.02074 0.01966 0.00534 0.01249 0.00982 0.02185 0.00429 0.00015 0.00018 0.00011 0.00000 0.00099 0.00096 0.00092 0.00076 0.00080 0.00078 0.00040 H6 -0.01986 0.80997 0.22115 1.00000 0.02621 0.00000 0.00000 C7 -0.00470 0.64230 0.18749 1.00000 0.01874 0.02564 0.01650 0.00560 0.00683 0.00752 0.02022 0.00409 0.00014 0.00018 0.00010 0.00000 0.00088 0.00103 0.00087 0.00075 0.00073 0.00075 0.00039 H7 -0.06560 0.64057 0.14657 1.00000 0.02426 0.00000 0.00000 C8 0.05787 0.54356 0.20182 1.00000 0.01608 0.01677 0.01407 0.00081 0.00599 0.00267 0.01553 0.00371 0.00013 0.00017 0.00010 0.00000 0.00082 0.00087 0.00081 0.00068 0.00068 0.00067 0.00034 H8 0.03889 0.47557 0.17049 1.00000 0.01864 0.00000 0.00000 C9 0.14773 0.54406 0.26160 1.00000 0.01365 0.01606 0.01354 0.00046 0.00714 0.00176 0.01382 0.00360 0.00012 0.00016 0.00010 0.00000 0.00078 0.00085 0.00079 0.00067 0.00066 0.00064 0.00033 C10 0.33532 0.21204 0.39249 1.00000 0.02622 0.02453 0.01499 0.00423 0.00657 0.00786 0.02223 0.00417 0.00015 0.00018 0.00010 0.00000 0.00098 0.00101 0.00087 0.00075 0.00076 0.00078 0.00040 C11 0.42100 0.12681 0.43305 1.00000 0.04036 0.04023 0.02165 0.01285 0.01439 0.02097 0.03326 0.00540 0.00018 0.00023 0.00012 0.00000 0.00127 0.00134 0.00104 0.00096 0.00097 0.00106 0.00053 C12 0.38463 0.32899 0.20916 1.00000 0.01243 0.01461 0.01563 0.00138 0.00520 0.00029 0.01423 0.00350 0.00012 0.00016 0.00010 0.00000 0.00077 0.00084 0.00081 0.00065 0.00065 0.00063 0.00033 H12 0.39900 0.25605 0.24108 1.00000 0.01708 0.00000 0.00000 C13 0.45563 0.42403 0.25680 1.00000 0.01548 0.01991 0.02411 -0.00184 0.00496 -0.00276 0.02053 0.00386 0.00014 0.00017 0.00012 0.00000 0.00088 0.00097 0.00100 0.00074 0.00077 0.00068 0.00040 H13A 0.45188 0.49616 0.22645 1.00000 0.02464 0.00000 0.00000 H13B 0.43719 0.44641 0.29934 1.00000 0.02464 0.00000 0.00000 C14 0.56035 0.37479 0.28579 1.00000 0.01545 0.03110 0.03050 0.00147 0.00222 -0.00256 0.02751 0.00426 0.00014 0.00021 0.00012 0.00000 0.00090 0.00113 0.00111 0.00091 0.00081 0.00081 0.00045 H14A 0.60601 0.43701 0.31525 1.00000 0.03301 0.00000 0.00000 H14B 0.56475 0.30633 0.31912 1.00000 0.03301 0.00000 0.00000 C15 0.59062 0.33512 0.22216 1.00000 0.01543 0.03047 0.03737 0.01263 0.01064 0.00545 0.02752 0.00457 0.00014 0.00020 0.00013 0.00000 0.00088 0.00113 0.00119 0.00093 0.00085 0.00078 0.00046 H15A 0.65601 0.29746 0.24286 1.00000 0.03303 0.00000 0.00000 H15B 0.59520 0.40550 0.19282 1.00000 0.03303 0.00000 0.00000 C16 0.51714 0.24681 0.17118 1.00000 0.02027 0.03101 0.03012 0.00260 0.01259 0.01010 0.02621 0.00446 0.00014 0.00020 0.00012 0.00000 0.00094 0.00112 0.00108 0.00091 0.00084 0.00082 0.00044 H16A 0.51950 0.17194 0.19880 1.00000 0.03145 0.00000 0.00000 H16B 0.53560 0.22812 0.12812 1.00000 0.03145 0.00000 0.00000 C17 0.41271 0.29625 0.14283 1.00000 0.01724 0.02959 0.01936 0.00039 0.00941 0.00401 0.02131 0.00413 0.00013 0.00019 0.00011 0.00000 0.00086 0.00106 0.00090 0.00078 0.00073 0.00075 0.00039 H17A 0.40855 0.36767 0.11180 1.00000 0.02557 0.00000 0.00000 H17B 0.36669 0.23582 0.11161 1.00000 0.02557 0.00000 0.00000 C18 0.19316 0.22118 0.14791 1.00000 0.01370 0.01183 0.01404 -0.00133 0.00563 -0.00097 0.01306 0.00342 0.00012 0.00015 0.00010 0.00000 0.00078 0.00080 0.00079 0.00063 0.00065 0.00061 0.00033 H18 0.21786 0.19728 0.10827 1.00000 0.01567 0.00000 0.00000 C19 0.21949 0.12093 0.20627 1.00000 0.01769 0.01453 0.02197 0.00413 0.00242 -0.00028 0.01950 0.00386 0.00014 0.00017 0.00011 0.00000 0.00086 0.00088 0.00094 0.00075 0.00073 0.00071 0.00038 H19A 0.29145 0.11171 0.22860 1.00000 0.02339 0.00000 0.00000 H19B 0.19631 0.14234 0.24657 1.00000 0.02339 0.00000 0.00000 C20 0.17304 0.00320 0.17102 1.00000 0.02161 0.01222 0.03279 0.00214 0.00728 -0.00104 0.02303 0.00403 0.00014 0.00017 0.00012 0.00000 0.00093 0.00088 0.00108 0.00078 0.00083 0.00072 0.00041 H20A 0.18835 -0.05879 0.21010 1.00000 0.02764 0.00000 0.00000 H20B 0.20124 -0.02216 0.13423 1.00000 0.02764 0.00000 0.00000 C21 0.06223 0.01482 0.13238 1.00000 0.01913 0.01559 0.02726 -0.00010 0.00719 -0.00320 0.02108 0.00394 0.00014 0.00017 0.00011 0.00000 0.00090 0.00089 0.00100 0.00076 0.00078 0.00070 0.00039 H21A 0.03306 0.03119 0.16998 1.00000 0.02529 0.00000 0.00000 H21B 0.03472 -0.06102 0.10723 1.00000 0.02529 0.00000 0.00000 C22 0.03616 0.11546 0.07509 1.00000 0.01647 0.01903 0.02073 -0.00070 0.00262 -0.00408 0.01999 0.00379 0.00014 0.00018 0.00011 0.00000 0.00085 0.00092 0.00092 0.00077 0.00073 0.00072 0.00038 H22A -0.03583 0.12397 0.05231 1.00000 0.02398 0.00000 0.00000 H22B 0.06011 0.09536 0.03501 1.00000 0.02398 0.00000 0.00000 C23 0.08136 0.23324 0.11106 1.00000 0.01360 0.01518 0.01933 0.00134 0.00509 -0.00047 0.01634 0.00361 0.00013 0.00016 0.00010 0.00000 0.00079 0.00085 0.00087 0.00069 0.00069 0.00064 0.00035 H23A 0.05441 0.25619 0.14902 1.00000 0.01960 0.00000 0.00000 H23B 0.06458 0.29651 0.07270 1.00000 0.01960 0.00000 0.00000 C24 0.20815 0.47353 0.11408 1.00000 0.01586 0.01111 0.01366 0.00121 0.00624 0.00098 0.01333 0.00352 0.00013 0.00015 0.00009 0.00000 0.00079 0.00080 0.00079 0.00064 0.00065 0.00062 0.00033 H24 0.13843 0.48731 0.10770 1.00000 0.01600 0.00000 0.00000 C25 0.25869 0.59462 0.13745 1.00000 0.02594 0.01376 0.01424 -0.00018 0.00581 -0.00388 0.01846 0.00383 0.00015 0.00016 0.00011 0.00000 0.00096 0.00089 0.00087 0.00066 0.00075 0.00070 0.00038 H25A 0.26127 0.61563 0.18787 1.00000 0.02216 0.00000 0.00000 H25B 0.32658 0.59010 0.13913 1.00000 0.02216 0.00000 0.00000 C26 0.20217 0.69023 0.08172 1.00000 0.03206 0.01433 0.02675 0.00391 0.01108 0.00101 0.02434 0.00431 0.00016 0.00018 0.00011 0.00000 0.00106 0.00091 0.00102 0.00078 0.00086 0.00078 0.00041 H26A 0.13599 0.69891 0.08309 1.00000 0.02921 0.00000 0.00000 H26B 0.23633 0.76753 0.09594 1.00000 0.02921 0.00000 0.00000 C27 0.19347 0.65755 0.00293 1.00000 0.02700 0.02046 0.01989 0.00914 0.00845 0.00238 0.02253 0.00421 0.00015 0.00018 0.00011 0.00000 0.00099 0.00097 0.00093 0.00076 0.00080 0.00077 0.00040 H27A 0.15224 0.71741 -0.03248 1.00000 0.02704 0.00000 0.00000 H27B 0.25920 0.65961 0.00015 1.00000 0.02704 0.00000 0.00000 C28 0.14892 0.53426 -0.02004 1.00000 0.02324 0.02423 0.01258 0.00302 0.00396 0.00230 0.02080 0.00394 0.00014 0.00018 0.00010 0.00000 0.00093 0.00101 0.00083 0.00074 0.00072 0.00077 0.00039 H28A 0.14994 0.51395 -0.06956 1.00000 0.02496 0.00000 0.00000 H28B 0.07986 0.53530 -0.02428 1.00000 0.02496 0.00000 0.00000 C29 0.20489 0.43896 0.03648 1.00000 0.02221 0.01653 0.01186 0.00029 0.00757 0.00185 0.01651 0.00381 0.00014 0.00017 0.00010 0.00000 0.00090 0.00085 0.00081 0.00068 0.00071 0.00070 0.00035 H29A 0.27228 0.43182 0.03735 1.00000 0.01982 0.00000 0.00000 H29B 0.17207 0.36096 0.02181 1.00000 0.01982 0.00000 0.00000 N1 0.27453 0.50902 0.40378 1.00000 0.01254 0.03041 0.01142 -0.00412 0.00395 0.00381 0.01827 0.00313 0.00011 0.00015 0.00008 0.00000 0.00070 0.00090 0.00071 0.00063 0.00059 0.00062 0.00033 O1 0.35744 0.28671 0.35261 1.00000 0.01820 0.02509 0.01427 0.00648 0.00576 0.00762 0.01927 0.00275 0.00009 0.00012 0.00007 0.00000 0.00063 0.00070 0.00061 0.00053 0.00051 0.00052 0.00028 O2 0.26034 0.20055 0.40488 1.00000 0.03167 0.03885 0.03884 0.01720 0.02010 0.00855 0.03444 0.00368 0.00011 0.00015 0.00009 0.00000 0.00082 0.00094 0.00091 0.00074 0.00073 0.00069 0.00038 F1 0.47201 0.09510 0.39226 1.00000 0.04081 0.03975 0.03325 0.00646 0.01816 0.02127 0.03668 0.00315 0.00011 0.00012 0.00008 0.00000 0.00078 0.00080 0.00074 0.00058 0.00064 0.00060 0.00033 F2 0.39316 0.02941 0.45591 1.00000 0.08285 0.07184 0.13408 0.08134 0.07322 0.04974 0.08679 0.00589 0.00015 0.00019 0.00014 0.00000 0.00141 0.00135 0.00197 0.00142 0.00146 0.00114 0.00082 F3 0.48420 0.18079 0.49336 1.00000 0.07827 0.09946 0.02895 -0.01347 -0.01847 0.05977 0.07998 0.00403 0.00015 0.00020 0.00009 0.00000 0.00129 0.00158 0.00082 0.00090 0.00081 0.00119 0.00072 P1 0.25406 0.36192 0.18886 1.00000 0.01150 0.01078 0.00993 0.00007 0.00388 0.00009 0.01077 0.00086 0.00003 0.00004 0.00002 0.00000 0.00020 0.00021 0.00020 0.00015 0.00016 0.00015 0.00009 Pd1 0.24835 0.41661 0.29973 1.00000 0.01066 0.01632 0.00835 0.00042 0.00308 0.00203 0.01191 0.00025 0.00001 0.00001 0.00001 0.00000 0.00008 0.00009 0.00008 0.00004 0.00005 0.00004 0.00006 Final Structure Factor Calculation for 02SRC143 in P2(1)/c Total number of l.s. parameters = 336 Maximum vector length = 511 Memory required = 4675 / 26061 wR2 = 0.0745 before cycle 5 for 6656 data and 0 / 336 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 18. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.100 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.036 0.000 GooF = S = 1.079; Restrained GooF = 1.078 for 18 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0344 * P )^2 + 2.12 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0284 for 6085 Fo > 4sig(Fo) and 0.0322 for all 6656 data wR2 = 0.0745, GooF = S = 1.079, Restrained GooF = 1.078 for all data Occupancy sum of asymmetric unit = 37.00 for non-hydrogen and 45.00 for hydrogen atoms Principal mean square atomic displacements U 0.0583 0.0234 0.0092 C1 0.0452 0.0208 0.0108 C2 0.0320 0.0186 0.0128 C3 0.0212 0.0166 0.0111 C4 0.0301 0.0191 0.0121 C5 0.0354 0.0162 0.0139 C6 0.0309 0.0169 0.0129 C7 0.0191 0.0139 0.0136 C8 0.0172 0.0143 0.0100 C9 0.0334 0.0201 0.0132 C10 0.0615 0.0235 0.0148 C11 0.0167 0.0137 0.0123 C12 0.0264 0.0212 0.0140 C13 0.0380 0.0300 0.0145 C14 0.0472 0.0219 0.0135 C15 0.0374 0.0289 0.0123 C16 0.0308 0.0200 0.0131 C17 0.0149 0.0131 0.0112 C18 0.0294 0.0164 0.0126 C19 0.0356 0.0216 0.0118 C20 0.0286 0.0210 0.0136 C21 0.0268 0.0203 0.0129 C22 0.0207 0.0149 0.0134 C23 0.0162 0.0132 0.0106 C24 0.0286 0.0142 0.0126 C25 0.0322 0.0276 0.0132 C26 0.0293 0.0274 0.0109 C27 0.0264 0.0242 0.0118 C28 0.0228 0.0160 0.0107 C29 0.0329 0.0119 0.0100 N1 0.0305 0.0167 0.0106 O1 0.0572 0.0261 0.0201 O2 0.0616 0.0304 0.0180 F1 0.1974 0.0473 0.0156 F2 0.1824 0.0417 0.0158 F3 0.0116 0.0108 0.0099 P1 0.0170 0.0104 0.0083 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 0.044 0.068 0.093 0.120 0.151 0.184 0.228 0.301 1.000 Number in group 678. 678. 652. 677. 641. 679. 661. 668. 659. 663. GooF 1.127 1.146 1.177 1.204 1.070 0.967 0.935 0.948 0.977 1.189 K 1.069 0.958 0.947 0.950 0.973 0.995 1.008 1.022 1.024 0.988 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.16 1.32 1.66 inf Number in group 669. 666. 676. 649. 673. 658. 673. 670. 653. 669. GooF 1.009 0.928 0.906 0.959 0.993 0.984 1.057 1.043 1.054 1.656 K 0.984 1.005 1.015 1.019 1.024 1.019 1.023 1.028 1.013 0.957 R1 0.049 0.043 0.037 0.035 0.033 0.028 0.028 0.025 0.022 0.034 Recommended weighting scheme: WGHT 0.0296 2.4501 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 4 0 0 48647.71 62934.48 5.15 1.000 3.42 6 0 2 1597.16 2120.34 4.85 0.184 2.04 -6 0 2 47679.21 58421.18 4.56 0.963 2.44 -7 0 4 90.33 183.90 4.48 0.054 2.10 1 5 4 397.78 262.14 4.34 0.065 1.94 3 4 1 101.08 43.49 4.33 0.026 2.31 3 1 7 416.43 613.35 4.22 0.099 1.92 2 2 1 32904.79 40080.24 4.11 0.798 4.01 7 0 12 42.96 125.38 4.08 0.045 1.02 2 4 3 503.77 358.97 4.02 0.076 2.27 2 0 6 42.26 5.83 4.00 0.010 2.43 -8 1 3 448.41 619.62 3.94 0.099 1.81 -6 0 8 3390.12 4106.29 3.85 0.255 2.02 -5 0 2 237.16 359.14 3.76 0.076 2.94 -5 0 6 2163.86 2658.95 3.75 0.206 2.54 1 5 2 1456.51 1180.93 3.66 0.137 2.12 -3 0 4 29221.41 34369.33 3.61 0.739 4.04 2 1 6 133.15 77.09 3.55 0.035 2.37 -8 1 7 395.90 531.74 3.51 0.092 1.73 -4 0 2 18373.14 21495.79 3.49 0.584 3.68 -3 1 4 31168.62 35961.92 3.46 0.756 3.80 -5 3 9 151.50 91.53 3.41 0.038 1.77 -7 3 19 13.59 59.47 3.41 0.031 0.98 -6 1 7 386.55 517.90 3.40 0.091 2.11 3 7 1 202.83 299.14 3.39 0.069 1.49 5 0 2 9.25 42.08 3.36 0.026 2.38 4 0 6 95.34 43.97 3.36 0.026 1.92 -5 1 12 241.11 341.22 3.35 0.074 1.57 1 0 4 567.25 734.77 3.31 0.108 3.86 -6 1 3 290.59 397.80 3.27 0.080 2.40 -1 5 4 312.69 224.06 3.23 0.060 2.04 -1 4 6 3288.51 2811.46 3.22 0.211 2.11 4 8 5 517.63 680.65 3.20 0.104 1.17 7 10 1 776.21 973.20 3.19 0.124 0.96 7 6 7 91.97 22.61 3.15 0.019 1.09 -6 7 12 129.80 201.51 3.15 0.057 1.11 2 0 2 3870.10 3214.74 3.15 0.226 4.66 -5 2 2 189.49 123.62 3.13 0.044 2.60 -15 8 9 1.78 58.71 3.09 0.031 0.80 -2 1 5 32337.47 36743.52 3.08 0.764 3.61 6 3 1 979.95 800.13 3.06 0.113 1.87 0 6 5 124.20 72.11 3.03 0.034 1.66 0 5 18 159.01 241.59 3.02 0.062 0.91 3 5 2 644.59 512.44 3.02 0.090 1.90 -5 0 20 1956.23 1589.00 3.02 0.159 0.97 0 2 3 41575.48 48482.95 2.99 0.878 4.09 0 1 3 22059.40 25020.38 2.99 0.631 5.28 3 3 5 154.22 81.16 2.96 0.036 2.03 -8 2 10 31.18 3.09 2.95 0.007 1.50 -6 3 17 225.30 313.53 2.95 0.071 1.08 Bond lengths and angles C1 - Distance Angles N1 1.4788 (0.0023) H1A 0.9800 109.47 H1B 0.9800 109.47 109.47 H1C 0.9800 109.47 109.47 109.47 C1 - N1 H1A H1B C2 - Distance Angles N1 1.4780 (0.0024) 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 1.4891 (0.0027) C4 1.4961 (0.0025) 108.89 (0.15) H3A 0.9900 109.91 109.91 H3B 0.9900 109.91 109.91 108.31 C3 - N1 C4 H3A C4 - Distance Angles C5 1.3912 (0.0026) C9 1.4069 (0.0025) 121.35 (0.17) C3 1.4961 (0.0025) 122.77 (0.17) 115.86 (0.16) C4 - C5 C9 C5 - Distance Angles C4 1.3912 (0.0026) C6 1.3931 (0.0028) 119.91 (0.18) H5 0.9500 120.04 120.04 C5 - C4 C6 C6 - Distance Angles C7 1.3810 (0.0029) C5 1.3931 (0.0028) 119.55 (0.17) H6 0.9500 120.22 120.22 C6 - C7 C5 C7 - Distance Angles C6 1.3810 (0.0029) C8 1.4025 (0.0026) 120.55 (0.17) H7 0.9500 119.72 119.72 C7 - C6 C8 C8 - Distance Angles C9 1.3959 (0.0024) C7 1.4025 (0.0026) 120.75 (0.17) H8 0.9500 119.63 119.63 C8 - C9 C7 C9 - Distance Angles C8 1.3959 (0.0024) C4 1.4069 (0.0025) 117.69 (0.16) Pd1 1.9943 (0.0017) 130.41 (0.14) 111.53 (0.12) C9 - C8 C4 C10 - Distance Angles O2 1.2214 (0.0025) O1 1.2618 (0.0024) 130.45 (0.19) C11 1.5454 (0.0028) 117.55 (0.18) 111.96 (0.17) C10 - O2 O1 C11 - Distance Angles F2 1.3025 (0.0032) F1 1.3250 (0.0026) 107.25 (0.21) F3 1.3364 (0.0031) 106.87 (0.22) 106.04 (0.21) C10 1.5454 (0.0028) 113.07 (0.20) 113.69 (0.17) 109.48 (0.20) C11 - F2 F1 F3 C12 - Distance Angles C17 1.5322 (0.0025) C13 1.5379 (0.0025) 109.42 (0.15) P1 1.8518 (0.0017) 116.99 (0.12) 114.17 (0.12) H12 1.0000 105.01 105.01 105.01 C12 - C17 C13 P1 C13 - Distance Angles C14 1.5351 (0.0026) C12 1.5379 (0.0025) 109.60 (0.16) H13A 0.9900 109.75 109.75 H13B 0.9900 109.75 109.75 108.22 C13 - C14 C12 H13A C14 - Distance Angles C15 1.5233 (0.0031) C13 1.5351 (0.0026) 111.56 (0.17) H14A 0.9900 109.31 109.31 H14B 0.9900 109.31 109.31 107.96 C14 - C15 C13 H14A C15 - Distance Angles C14 1.5233 (0.0031) C16 1.5274 (0.0031) 111.16 (0.16) H15A 0.9900 109.40 109.40 H15B 0.9900 109.40 109.40 108.01 C15 - C14 C16 H15A C16 - Distance Angles C15 1.5274 (0.0031) C17 1.5324 (0.0025) 111.79 (0.17) H16A 0.9900 109.26 109.26 H16B 0.9900 109.26 109.26 107.93 C16 - C15 C17 H16A C17 - Distance Angles C12 1.5322 (0.0025) C16 1.5324 (0.0025) 109.62 (0.16) H17A 0.9900 109.75 109.75 H17B 0.9900 109.75 109.75 108.22 C17 - C12 C16 H17A C18 - Distance Angles C23 1.5377 (0.0023) C19 1.5384 (0.0024) 109.77 (0.14) P1 1.8447 (0.0017) 112.90 (0.12) 111.30 (0.12) H18 1.0000 107.55 107.55 107.55 C18 - C23 C19 P1 C19 - Distance Angles C20 1.5281 (0.0026) C18 1.5384 (0.0024) 110.97 (0.15) H19A 0.9900 109.45 109.44 H19B 0.9900 109.45 109.45 108.04 C19 - C20 C18 H19A C20 - Distance Angles C19 1.5281 (0.0026) C21 1.5270 (0.0026) 111.33 (0.16) H20A 0.9900 109.36 109.36 H20B 0.9900 109.36 109.36 107.99 C20 - C19 C21 H20A C21 - Distance Angles C20 1.5270 (0.0026) C22 1.5286 (0.0027) 110.61 (0.15) H21A 0.9900 109.53 109.53 H21B 0.9900 109.53 109.53 108.09 C21 - C20 C22 H21A C22 - Distance Angles C21 1.5286 (0.0027) C23 1.5276 (0.0025) 111.19 (0.16) H22A 0.9900 109.39 109.39 H22B 0.9900 109.39 109.39 108.01 C22 - C21 C23 H22A C23 - Distance Angles C22 1.5276 (0.0025) C18 1.5377 (0.0023) 110.16 (0.15) H23A 0.9900 109.63 109.63 H23B 0.9900 109.63 109.63 108.14 C23 - C22 C18 H23A C24 - Distance Angles C29 1.5334 (0.0024) C25 1.5359 (0.0024) 110.32 (0.15) P1 1.8417 (0.0017) 117.67 (0.12) 112.10 (0.12) H24 1.0000 105.20 105.20 105.20 C24 - C29 C25 P1 C25 - Distance Angles C26 1.5297 (0.0026) C24 1.5359 (0.0024) 109.74 (0.15) H25A 0.9900 109.72 109.72 H25B 0.9900 109.72 109.72 108.20 C25 - C26 C24 H25A C26 - Distance Angles C27 1.5255 (0.0029) C25 1.5297 (0.0026) 110.84 (0.16) H26A 0.9900 109.47 109.47 H26B 0.9900 109.47 109.47 108.06 C26 - C27 C25 H26A C27 - Distance Angles C28 1.5264 (0.0028) C26 1.5255 (0.0028) 112.08 (0.16) H27A 0.9900 109.19 109.19 H27B 0.9900 109.19 109.19 107.89 C27 - C28 C26 H27A C28 - Distance Angles C27 1.5264 (0.0028) C29 1.5327 (0.0025) 111.57 (0.15) H28A 0.9900 109.31 109.31 H28B 0.9900 109.31 109.31 107.96 C28 - C27 C29 H28A C29 - Distance Angles C28 1.5327 (0.0025) C24 1.5334 (0.0024) 109.46 (0.15) H29A 0.9900 109.78 109.78 H29B 0.9900 109.78 109.78 108.24 C29 - C28 C24 H29A N1 - Distance Angles C2 1.4780 (0.0024) C1 1.4788 (0.0023) 108.78 (0.15) C3 1.4891 (0.0027) 110.89 (0.15) 109.41 (0.16) Pd1 2.1672 (0.0015) 113.53 (0.12) 113.80 (0.12) 100.14 (0.11) N1 - C2 C1 C3 O1 - Distance Angles C10 1.2618 (0.0024) Pd1 2.1295 (0.0012) 115.37 (0.12) O1 - C10 O2 - Distance Angles C10 1.2214 (0.0025) O2 - F1 - Distance Angles C11 1.3250 (0.0026) F1 - F2 - Distance Angles C11 1.3025 (0.0032) F2 - F3 - Distance Angles C11 1.3364 (0.0031) F3 - P1 - Distance Angles C24 1.8417 (0.0017) C18 1.8447 (0.0017) 105.60 (0.08) C12 1.8518 (0.0017) 110.55 (0.08) 102.74 (0.08) Pd1 2.2618 (0.0004) 115.26 (0.06) 117.12 (0.06) 104.83 (0.06) P1 - C24 C18 C12 Pd1 - Distance Angles C9 1.9943 (0.0017) O1 2.1295 (0.0013) 173.60 (0.06) N1 2.1672 (0.0015) 81.37 (0.07) 92.36 (0.05) P1 2.2618 (0.0004) 97.46 (0.05) 88.91 (0.04) 162.47 (0.05) Pd1 - C9 O1 N1 FMAP and GRID set by program FMAP 2 1 39 GRID -1.389 -2 -1 1.389 2 1 R1 = 0.0319 for 6656 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.51 at 0.2531 0.4207 0.1002 [ 1.00 A from C24 ] Deepest hole -1.10 at 0.2532 0.4210 0.3399 [ 0.76 A from PD1 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 4735 / 52743 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2531 0.4207 0.1002 1.00000 0.05 0.51 1.00 C24 1.19 C29 1.35 H29A 1.68 H29B Q2 1 0.4375 0.1117 0.4933 1.00000 0.05 0.50 1.04 F3 1.11 C11 1.20 F2 2.20 F1 Q3 1 0.3457 0.0024 0.4081 1.00000 0.05 0.50 0.98 F2 1.74 C11 2.25 F1 2.37 C10 Q4 1 0.2476 0.7520 0.3004 1.00000 0.05 0.47 1.66 H3A 1.72 C4 1.94 C3 1.97 H15A Q5 1 0.3750 0.1693 0.4075 1.00000 0.05 0.40 0.73 C10 0.83 C11 1.65 O1 1.71 O2 Q6 1 0.1403 0.2324 0.1298 1.00000 0.05 0.34 0.74 C18 0.81 C23 1.41 H18 1.44 H23B Q7 1 0.3248 0.3436 0.1945 1.00000 0.05 0.34 0.84 C12 1.03 P1 1.50 H12 1.98 C17 Q8 1 0.1857 0.4984 0.2538 1.00000 0.05 0.34 0.81 C9 1.37 PD1 1.85 C8 2.01 C4 Q9 1 0.2184 0.4232 0.1432 1.00000 0.05 0.32 0.77 C24 1.09 P1 1.33 H24 2.01 C29 Q10 1 0.2122 0.2808 0.1679 1.00000 0.05 0.32 0.77 C18 1.09 P1 1.51 H18 1.91 C23 Shortest distances between peaks (including symmetry equivalents) 1 9 1.13 6 10 1.17 9 10 1.68 2 5 1.70 7 10 1.70 7 9 1.76 3 5 1.93 1 7 1.94 2 3 2.09 1 10 2.27 6 9 2.40 8 9 2.51 6 7 2.83 1 6 2.88 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. 0.39: 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 3.38: Structure factors and derivatives 4.66: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.38: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.27: Analysis of variance 0.11: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.22: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 15:32:51 Total elapsed time: 9.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++