+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 13:37:52 on 06-Apr-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P-1 CELL 0.71073 11.3216 13.2873 13.9320 110.438 98.073 115.161 ZERR 2.00 0.0003 0.0006 0.0009 0.004 0.004 0.004 LATT 1 SFAC C H N S F CL UNIT 62 34 8 12 8 6 V = 1671.26 F(000) = 828.0 Mu = 0.70 mm-1 Cell Wt = 1640.39 Rho = 1.630 MERG 2 OMIT -3.00 55.00 FMAP 2 PLAN 20 SIZE 0.08 0.12 0.16 ACTA BOND $H L.S. 6 TEMP -153.00 WGHT 0.069000 6.389800 FVAR 0.33868 0.76241 MOLE 1 C1 1 0.385239 0.625304 0.164864 11.00000 0.01667 0.02122 = 0.01824 0.00969 0.00955 0.01210 C2 1 0.413679 0.666922 0.342234 11.00000 0.01632 0.01577 = 0.01683 0.00909 0.00862 0.00946 C3 1 0.318083 0.694905 0.308946 11.00000 0.01593 0.01522 = 0.01412 0.00748 0.00713 0.00828 C4 1 0.251056 0.748458 0.373712 11.00000 0.01521 0.01542 = 0.01393 0.00731 0.00579 0.00957 C5 1 0.170303 0.701973 0.428796 11.00000 0.01646 0.01546 = 0.01486 0.00717 0.00630 0.01125 C6 1 0.201616 0.894562 0.468083 11.00000 0.01550 0.01819 = 0.01450 0.00929 0.00644 0.01029 C7 1 0.205912 0.682699 0.133139 11.00000 0.02164 0.02077 = 0.01299 0.00614 0.00540 0.01433 C8 1 0.068574 0.629574 0.127532 11.00000 0.02217 0.02447 = 0.01883 0.00705 0.00688 0.01449 C9 1 -0.024246 0.639591 0.060419 11.00000 0.02453 0.04041 = 0.02467 0.00786 0.00539 0.02213 C10 1 0.024639 0.700773 0.000486 11.00000 0.04407 0.05093 = 0.02183 0.01461 0.00536 0.03670 C11 1 0.160634 0.755493 0.005926 11.00000 0.04887 0.04164 = 0.02327 0.01981 0.01381 0.03052 C12 1 0.253515 0.746766 0.073861 11.00000 0.02909 0.02861 = 0.02051 0.01224 0.00972 0.01709 C13 1 0.545821 0.576054 0.249102 11.00000 0.01940 0.02525 = 0.01655 0.01053 0.00946 0.01642 C14 1 0.682893 0.653706 0.264405 11.00000 0.02079 0.02805 = 0.02462 0.00680 0.00921 0.01386 C15 1 0.770971 0.606115 0.254961 11.00000 0.02195 0.04972 = 0.02372 0.00861 0.00941 0.02272 C16 1 0.718159 0.483167 0.231110 11.00000 0.04347 0.06059 = 0.01967 0.01917 0.01581 0.04638 C17 1 0.583851 0.405629 0.216842 11.00000 0.05651 0.03993 = 0.03521 0.02340 0.02443 0.03914 C18 1 0.495118 0.452742 0.225821 11.00000 0.03257 0.02896 = 0.03321 0.01870 0.01755 0.02127 C19 1 0.058188 0.783048 0.556466 11.00000 0.01618 0.01525 = 0.01614 0.00747 0.00861 0.00832 C20 1 0.090914 0.757124 0.641330 11.00000 0.01667 0.01636 = 0.01938 0.00920 0.00828 0.00939 C21 1 0.011967 0.750709 0.709326 11.00000 0.02253 0.01934 = 0.01612 0.00884 0.00813 0.00973 C22 1 -0.096343 0.771293 0.690253 11.00000 0.02068 0.02147 = 0.02092 0.00900 0.01470 0.00968 C23 1 -0.130477 0.797273 0.606527 11.00000 0.01847 0.02355 = 0.02550 0.01084 0.01139 0.01302 C24 1 -0.051997 0.803124 0.538760 11.00000 0.01790 0.02031 = 0.01816 0.00884 0.00755 0.01162 C25 1 0.342160 0.942915 0.350709 11.00000 0.01883 0.01535 = 0.01455 0.00845 0.00783 0.00852 C26 1 0.277949 0.985668 0.296208 11.00000 0.02231 0.01960 = 0.01970 0.01036 0.00935 0.01328 C27 1 0.350379 1.056759 0.248668 11.00000 0.03371 0.02342 = 0.02288 0.01518 0.01216 0.01839 C28 1 0.483134 1.080052 0.256697 11.00000 0.03056 0.01799 = 0.02245 0.01305 0.01537 0.01060 C29 1 0.547445 1.037048 0.308864 11.00000 0.01947 0.01793 = 0.02142 0.00895 0.00946 0.00754 C30 1 0.476195 0.968835 0.358509 11.00000 0.01906 0.01635 = 0.01553 0.00780 0.00717 0.00996 N1 3 0.301121 0.670125 0.200683 11.00000 0.01766 0.01967 = 0.01479 0.00840 0.00826 0.01232 N2 3 0.453347 0.623710 0.253415 11.00000 0.01864 0.02189 = 0.01660 0.01003 0.00990 0.01431 N3 3 0.139721 0.792151 0.486664 11.00000 0.01636 0.01615 = 0.01743 0.00951 0.00875 0.01082 N4 3 0.266322 0.864631 0.395686 11.00000 0.01685 0.01664 = 0.01638 0.00984 0.00905 0.01092 S1 4 0.093628 0.549957 0.412024 11.00000 0.01514 0.01585 = 0.02019 0.01030 0.00798 0.00921 S2 4 0.227556 0.558800 0.536946 11.00000 0.01948 0.02418 = 0.02168 0.01526 0.01160 0.01495 S3 4 0.369913 0.531384 0.475349 11.00000 0.02028 0.02362 = 0.02493 0.01550 0.01255 0.01577 S4 4 0.495649 0.697189 0.472247 11.00000 0.01566 0.02117 = 0.01653 0.00972 0.00674 0.01023 S5 4 0.401381 0.579527 0.043101 11.00000 0.02781 0.03687 = 0.01615 0.01047 0.01198 0.02179 S6 4 0.208736 1.030642 0.526899 11.00000 0.02692 0.01877 = 0.02443 0.01242 0.01494 0.01658 F1 5 -0.067021 0.705136 -0.069640 11.00000 0.06575 0.09935 = 0.03956 0.03798 0.01201 0.06500 F2 5 0.804406 0.436728 0.220765 11.00000 0.06431 0.09253 = 0.03611 0.03043 0.02451 0.07151 F3 5 -0.172534 0.766690 0.756999 11.00000 0.03272 0.04025 = 0.03005 0.01913 0.02453 0.02192 F4 5 0.553720 1.147328 0.208883 11.00000 0.04126 0.03101 = 0.03836 0.02716 0.02447 0.01690 H8 2 0.039661 0.585437 0.167087 11.00000 0.01657 H9 2 -0.121195 0.601121 0.052602 11.00000 0.03603 H11 2 0.190209 0.797158 -0.034546 11.00000 0.04810 H12 2 0.346113 0.782491 0.080976 11.00000 0.02870 H14 2 0.713474 0.738368 0.278167 11.00000 0.03344 H15 2 0.869973 0.660533 0.266090 11.00000 0.04432 H17 2 0.551123 0.322660 0.202598 11.00000 0.05146 H18 2 0.399521 0.400320 0.217099 11.00000 0.03515 H20 2 0.165573 0.746154 0.654630 11.00000 0.01641 H21 2 0.030331 0.730443 0.763552 11.00000 0.02376 H23 2 -0.209877 0.806766 0.592570 11.00000 0.03089 H24 2 -0.074509 0.821361 0.479687 11.00000 0.01853 H26 2 0.186706 0.966414 0.293663 11.00000 0.01729 H27 2 0.309318 1.085413 0.211235 11.00000 0.02717 H29 2 0.635673 1.050354 0.310015 11.00000 0.02110 H30 2 0.516390 0.936016 0.396599 11.00000 0.01767 MOLE 2 PART 1 C311 1 0.304625 0.138954 0.935372 21.00000 0.05210 0.03597 = 0.03147 0.01427 0.01551 0.02358 AFIX 13 H311 2 0.376203 0.229415 0.965990 21.00000 -1.20000 AFIX 0 CL31 6 0.194217 0.124859 1.011538 21.00000 0.08376 0.10853 = 0.07127 0.05271 0.05695 0.07115 CL32 6 0.389497 0.058542 0.951016 21.00000 0.05093 0.06582 = 0.04481 0.03289 0.02753 0.03438 CL33 6 0.220353 0.083784 0.798234 21.00000 0.07180 0.02769 = 0.02771 0.01036 0.00520 0.02057 PART 2 SAME C311 > CL33 C411 1 0.268390 0.143652 0.936477 -21.00000 0.51111 0.10336 = 0.08328 -0.06230 0.20635 -0.16746 AFIX 13 H411 2 0.321335 0.236456 0.981814 -21.00000 -1.20000 AFIX 0 CL41 6 0.356405 0.071133 0.958714 -21.00000 0.61334 0.17609 = 0.42416 0.05947 -0.19843 0.19819 CL42 6 0.193448 0.095601 0.804539 -21.00000 0.77244 0.15515 = 0.44559 0.12608 0.32078 0.07628 CL43 6 0.125137 0.065748 0.968029 -21.00000 0.14341 0.21145 = 0.09952 0.02573 0.05471 0.08535 HKLF 4 Covalent radii and connectivity table for s92 in P-1 C 0.770 H 0.320 N 0.700 S 1.030 F 0.640 CL 0.990 C1 - N2 N1 S5 C2 - C3 N2 S4 C3 - C2 N1 C4 C4 - C5 N4 C3 C5 - C4 N3 S1 C6 - N4 N3 S6 C7 - C8 C12 N1 C8 - C7 C9 C9 - C10 C8 C10 - F1 C11 C9 C11 - C10 C12 C12 - C11 C7 C13 - C18 C14 N2 C14 - C13 C15 C15 - C16 C14 C16 - F2 C17 C15 C17 - C16 C18 C18 - C13 C17 C19 - C20 C24 N3 C20 - C19 C21 C21 - C22 C20 C22 - F3 C21 C23 C23 - C22 C24 C24 - C23 C19 C25 - C30 C26 N4 C26 - C25 C27 C27 - C28 C26 C28 - F4 C29 C27 C29 - C28 C30 C30 - C25 C29 N1 - C1 C3 C7 N2 - C1 C2 C13 N3 - C6 C5 C19 N4 - C6 C4 C25 S1 - C5 S2 S2 - S3 S1 S3 - S2 S4 S4 - C2 S3 S5 - C1 S6 - C6 F1 - C10 F2 - C16 F3 - C22 F4 - C28 C311_a - Cl33_a Cl31_a Cl32_a Cl31_a - C311_a Cl32_a - C311_a Cl33_a - C311_a C411_b - Cl42_b Cl41_b Cl43_b Cl41_b - C411_b Cl42_b - C411_b Cl43_b - C411_b 33992 Reflections read, of which 43 rejected -14 =< h =< 14, -17 =< k =< 17, -17 =< l =< 18, Max. 2-theta = 55.00 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -2 1 0 40.42 0.49 5 4.17 1 1 0 278.61 1.56 6 74.25 -4 3 0 144.88 1.57 6 19.01 -3 3 0 218.80 1.86 5 61.38 10 -7 1 326.60 2.68 6 44.16 8 -6 1 139.01 0.93 7 12.60 4 -3 1 63.34 0.74 8 4.16 1 -2 1 289.68 2.66 10 19.79 2 -2 1 981.73 6.37 5 194.60 -2 0 1 16.34 0.35 8 1.81 1 0 1 169.92 1.78 5 18.40 -2 1 1 508.05 5.60 7 35.50 0 1 1 346.94 3.01 6 28.95 -7 7 1 93.63 1.99 5 11.88 -7 9 1 70.31 1.31 5 8.20 6 -5 2 36.70 0.80 5 6.51 1 -2 2 316.35 3.17 12 16.90 -1 -1 2 174.45 1.88 6 13.60 0 -1 2 35.38 0.56 4 3.94 0 0 2 324.51 0.98 4 100.19 -10 8 2 24.23 0.73 5 3.87 -8 8 2 466.61 7.95 4 76.89 8 -6 3 180.45 2.41 7 13.43 3 -4 3 200.76 1.83 9 9.75 4 -10 6 63.53 0.82 8 5.81 7 -8 7 60.61 0.89 5 10.00 8 -8 7 58.93 0.87 6 7.55 7 -9 8 34.30 0.77 6 4.80 28 Inconsistent equivalents 7667 Unique reflections, of which 0 suppressed R(int) = 0.0487 R(sigma) = 0.0368 Friedel opposites merged Maximum memory for data reduction = 3528 / 79445 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 = 4794 / 714700 wR2 = 0.1039 before cycle 1 for 7667 data and 534 / 534 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint 0.0879 0.0200 SAME/SADI C311_a Cl32_a C411_b Cl42_b 0.2985 0.0400 SAME/SADI Cl31_a Cl33_a Cl41_b Cl43_b 0.2560 0.0400 SAME/SADI Cl32_a Cl33_a Cl42_b Cl43_b 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. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.165 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.669; Restrained GooF = 0.674 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0690 * P )^2 + 6.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33869 0.00045 0.032 OSF 2 0.76206 0.00436 -0.080 FVAR 2 Mean shift/esd = 0.011 Maximum = 0.480 for U22 Cl43_b Max. shift = 0.003 A for Cl43_b Max. dU = 0.002 for Cl43_b Least-squares cycle 2 Maximum vector length = 511 Memory required = 4794 / 714700 wR2 = 0.1039 before cycle 2 for 7667 data and 534 / 534 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint 0.0883 0.0200 SAME/SADI C311_a Cl32_a C411_b Cl42_b 0.2979 0.0400 SAME/SADI Cl31_a Cl33_a Cl41_b Cl43_b 0.2580 0.0400 SAME/SADI Cl32_a Cl33_a Cl42_b Cl43_b 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. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.165 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.669; Restrained GooF = 0.674 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0690 * P )^2 + 6.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33871 0.00045 0.034 OSF 2 0.76156 0.00436 -0.115 FVAR 2 Mean shift/esd = 0.013 Maximum = 0.609 for U22 Cl43_b Max. shift = 0.004 A for Cl43_b Max. dU = 0.003 for Cl43_b Least-squares cycle 3 Maximum vector length = 511 Memory required = 4794 / 714700 wR2 = 0.1038 before cycle 3 for 7667 data and 534 / 534 parameters Disagreeable restraints before cycle 3 Observed Target Error Sigma Restraint 0.0889 0.0200 SAME/SADI C311_a Cl32_a C411_b Cl42_b 0.2970 0.0400 SAME/SADI Cl31_a Cl33_a Cl41_b Cl43_b 0.2605 0.0400 SAME/SADI Cl32_a Cl33_a Cl42_b Cl43_b 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. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.166 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.669; Restrained GooF = 0.674 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0690 * P )^2 + 6.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33872 0.00045 0.030 OSF 2 0.76100 0.00437 -0.129 FVAR 2 Mean shift/esd = 0.012 Maximum = 0.574 for U22 Cl43_b Max. shift = 0.004 A for Cl43_b Max. dU = 0.003 for Cl43_b Least-squares cycle 4 Maximum vector length = 511 Memory required = 4794 / 714700 wR2 = 0.1038 before cycle 4 for 7667 data and 534 / 534 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint 0.0895 0.0200 SAME/SADI C311_a Cl32_a C411_b Cl42_b 0.2959 0.0400 SAME/SADI Cl31_a Cl33_a Cl41_b Cl43_b 0.2632 0.0400 SAME/SADI Cl32_a Cl33_a Cl42_b Cl43_b 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. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.166 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.669; Restrained GooF = 0.674 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0690 * P )^2 + 6.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33873 0.00045 0.025 OSF 2 0.76037 0.00438 -0.144 FVAR 2 Mean shift/esd = 0.012 Maximum = 0.545 for U22 Cl43_b Max. shift = 0.004 A for Cl43_b Max. dU = 0.002 for Cl43_b Least-squares cycle 5 Maximum vector length = 511 Memory required = 4794 / 714700 wR2 = 0.1038 before cycle 5 for 7667 data and 534 / 534 parameters Disagreeable restraints before cycle 5 Observed Target Error Sigma Restraint 0.0904 0.0200 SAME/SADI C311_a Cl32_a C411_b Cl42_b 0.2946 0.0400 SAME/SADI Cl31_a Cl33_a Cl41_b Cl43_b 0.2659 0.0400 SAME/SADI Cl32_a Cl33_a Cl42_b Cl43_b 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. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.167 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.669; Restrained GooF = 0.674 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0690 * P )^2 + 6.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33875 0.00045 0.028 OSF 2 0.75968 0.00438 -0.156 FVAR 2 Mean shift/esd = 0.013 Maximum = 0.523 for U22 Cl43_b Max. shift = 0.004 A for Cl43_b Max. dU =-0.003 for Cl42_b Least-squares cycle 6 Maximum vector length = 511 Memory required = 4794 / 714700 wR2 = 0.1038 before cycle 6 for 7667 data and 534 / 534 parameters Disagreeable restraints before cycle 6 Observed Target Error Sigma Restraint 0.0912 0.0200 SAME/SADI C311_a Cl32_a C411_b Cl42_b 0.2931 0.0400 SAME/SADI Cl31_a Cl33_a Cl41_b Cl43_b 0.2686 0.0400 SAME/SADI Cl32_a Cl33_a Cl42_b Cl43_b Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.167 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.669; Restrained GooF = 0.674 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0690 * P )^2 + 6.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33876 0.00045 0.023 OSF 2 0.75896 0.00440 -0.164 FVAR 2 Mean shift/esd = 0.013 Maximum = 0.503 for U22 Cl43_b Max. shift = 0.004 A for Cl43_b Max. dU =-0.003 for Cl42_b Largest correlation matrix elements 0.897 U13 C411_b / U33 C411_b 0.776 U13 Cl31_a / U23 Cl31_a 0.737 y Cl31_a / x Cl31_a 0.894 U13 C411_b / U11 C411_b 0.773 U12 C16 / U11 C16 0.735 U12 C17 / U11 C17 0.841 U12 C411_b / U23 C411_b 0.772 U13 F2 / U23 F2 0.731 U23 Cl31_a / U33 Cl31_a 0.821 U12 F2 / U22 F2 0.767 U12 F1 / U22 F1 0.730 U13 Cl31_a / U33 Cl31_a 0.815 U12 F2 / U11 F2 0.762 U12 F1 / U11 F1 0.729 U13 C16 / U23 C16 0.798 U12 Cl31_a / U22 Cl31_a 0.757 y F2 / x F2 0.729 U12 C311_a / U22 C311_a 0.796 U12 Cl31_a / U11 Cl31_a 0.739 U12 C17 / U22 C17 0.728 U12 Cl31_a / U23 Cl31_a 0.784 U12 C16 / U22 C16 0.738 U13 Cl31_a / U11 Cl31_a 0.725 U12 C10 / U22 C10 Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H311 0.3761 0.2294 0.9660 13 1.000 0.000 C311_a Cl33_a Cl31_a Cl32_a H411 0.3233 0.2365 0.9815 13 1.000 0.002 C411_b Cl42_b Cl41_b Cl43_b s92 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.38524 0.62530 0.16486 1.00000 0.01666 0.02125 0.01827 0.00970 0.00955 0.01209 0.01706 0.00602 0.00022 0.00020 0.00017 0.00000 0.00097 0.00101 0.00100 0.00085 0.00081 0.00085 0.00040 C2 0.41368 0.66693 0.34224 1.00000 0.01633 0.01580 0.01687 0.00911 0.00863 0.00948 0.01490 0.00577 0.00021 0.00019 0.00017 0.00000 0.00094 0.00092 0.00096 0.00079 0.00079 0.00080 0.00038 C3 0.31808 0.69491 0.30895 1.00000 0.01592 0.01521 0.01411 0.00745 0.00711 0.00827 0.01445 0.00565 0.00021 0.00019 0.00016 0.00000 0.00093 0.00092 0.00093 0.00077 0.00077 0.00079 0.00038 C4 0.25105 0.74845 0.37371 1.00000 0.01525 0.01546 0.01395 0.00734 0.00581 0.00959 0.01385 0.00560 0.00021 0.00018 0.00016 0.00000 0.00092 0.00092 0.00091 0.00077 0.00076 0.00079 0.00038 C5 0.17030 0.70197 0.42879 1.00000 0.01647 0.01546 0.01487 0.00717 0.00631 0.01125 0.01412 0.00565 0.00021 0.00018 0.00016 0.00000 0.00094 0.00092 0.00093 0.00078 0.00077 0.00080 0.00038 C6 0.20162 0.89457 0.46808 1.00000 0.01551 0.01823 0.01454 0.00932 0.00646 0.01031 0.01462 0.00573 0.00021 0.00019 0.00016 0.00000 0.00093 0.00096 0.00093 0.00079 0.00077 0.00081 0.00038 C7 0.20592 0.68270 0.13313 1.00000 0.02169 0.02079 0.01301 0.00616 0.00541 0.01437 0.01762 0.00597 0.00023 0.00020 0.00017 0.00000 0.00104 0.00101 0.00093 0.00081 0.00081 0.00088 0.00041 C8 0.06857 0.62957 0.12753 1.00000 0.02219 0.02449 0.01884 0.00704 0.00690 0.01451 0.02172 0.00645 0.00024 0.00022 0.00019 0.00000 0.00109 0.00109 0.00104 0.00090 0.00088 0.00093 0.00045 C9 -0.02424 0.63959 0.06043 1.00000 0.02453 0.04033 0.02467 0.00778 0.00534 0.02208 0.03026 0.00737 0.00027 0.00026 0.00021 0.00000 0.00123 0.00144 0.00122 0.00109 0.00100 0.00115 0.00055 C10 0.02463 0.70076 0.00048 1.00000 0.04412 0.05093 0.02181 0.01460 0.00538 0.03672 0.03520 0.00819 0.00031 0.00028 0.00021 0.00000 0.00156 0.00165 0.00121 0.00118 0.00112 0.00142 0.00062 C11 0.16064 0.75550 0.00593 1.00000 0.04887 0.04162 0.02330 0.01984 0.01382 0.03049 0.03305 0.00824 0.00032 0.00027 0.00021 0.00000 0.00163 0.00149 0.00122 0.00117 0.00117 0.00136 0.00058 C12 0.25350 0.74675 0.07386 1.00000 0.02909 0.02865 0.02055 0.01228 0.00974 0.01709 0.02463 0.00702 0.00027 0.00023 0.00019 0.00000 0.00126 0.00120 0.00111 0.00097 0.00097 0.00105 0.00048 C13 0.54582 0.57606 0.24911 1.00000 0.01941 0.02522 0.01655 0.01051 0.00946 0.01640 0.01759 0.00618 0.00022 0.00021 0.00017 0.00000 0.00101 0.00107 0.00097 0.00086 0.00082 0.00090 0.00041 C14 0.68289 0.65370 0.26441 1.00000 0.02081 0.02808 0.02464 0.00681 0.00922 0.01390 0.02546 0.00682 0.00025 0.00024 0.00020 0.00000 0.00111 0.00123 0.00116 0.00098 0.00093 0.00099 0.00049 C15 0.77098 0.60613 0.25497 1.00000 0.02196 0.04970 0.02373 0.00860 0.00940 0.02271 0.03245 0.00769 0.00027 0.00028 0.00021 0.00000 0.00121 0.00162 0.00121 0.00114 0.00099 0.00121 0.00059 C16 0.71815 0.48315 0.23111 1.00000 0.04347 0.06056 0.01966 0.01914 0.01578 0.04636 0.03215 0.00828 0.00029 0.00029 0.00020 0.00000 0.00151 0.00176 0.00113 0.00118 0.00108 0.00147 0.00060 C17 0.58386 0.40564 0.21685 1.00000 0.05651 0.03995 0.03520 0.02341 0.02444 0.03915 0.03473 0.00903 0.00033 0.00028 0.00023 0.00000 0.00178 0.00150 0.00142 0.00124 0.00132 0.00145 0.00061 C18 0.49512 0.45274 0.22582 1.00000 0.03258 0.02898 0.03321 0.01868 0.01753 0.02126 0.02704 0.00761 0.00028 0.00024 0.00021 0.00000 0.00132 0.00123 0.00131 0.00108 0.00109 0.00111 0.00050 C19 0.05819 0.78305 0.55647 1.00000 0.01618 0.01528 0.01617 0.00750 0.00862 0.00834 0.01526 0.00571 0.00021 0.00019 0.00017 0.00000 0.00095 0.00093 0.00095 0.00079 0.00079 0.00080 0.00039 C20 0.09092 0.75713 0.64133 1.00000 0.01669 0.01640 0.01941 0.00924 0.00830 0.00941 0.01649 0.00594 0.00022 0.00019 0.00017 0.00000 0.00097 0.00095 0.00101 0.00082 0.00082 0.00082 0.00040 C21 0.01197 0.75071 0.70932 1.00000 0.02251 0.01931 0.01611 0.00881 0.00810 0.00971 0.01929 0.00613 0.00023 0.00020 0.00018 0.00000 0.00107 0.00102 0.00100 0.00086 0.00086 0.00088 0.00042 C22 -0.09635 0.77128 0.69025 1.00000 0.02069 0.02151 0.02097 0.00905 0.01471 0.00971 0.02076 0.00632 0.00023 0.00021 0.00018 0.00000 0.00105 0.00105 0.00106 0.00088 0.00089 0.00089 0.00044 C23 -0.13047 0.79727 0.60652 1.00000 0.01849 0.02357 0.02552 0.01085 0.01140 0.01304 0.02121 0.00649 0.00023 0.00021 0.00019 0.00000 0.00103 0.00109 0.00113 0.00092 0.00090 0.00091 0.00044 C24 -0.05199 0.80313 0.53876 1.00000 0.01792 0.02031 0.01817 0.00885 0.00755 0.01164 0.01783 0.00608 0.00022 0.00020 0.00018 0.00000 0.00099 0.00101 0.00100 0.00085 0.00083 0.00085 0.00041 C25 0.34216 0.94291 0.35071 1.00000 0.01885 0.01536 0.01456 0.00845 0.00783 0.00853 0.01554 0.00579 0.00022 0.00019 0.00016 0.00000 0.00098 0.00092 0.00093 0.00079 0.00079 0.00081 0.00039 C26 0.27795 0.98567 0.29620 1.00000 0.02231 0.01961 0.01972 0.01037 0.00934 0.01328 0.01875 0.00629 0.00024 0.00020 0.00018 0.00000 0.00109 0.00101 0.00103 0.00086 0.00087 0.00089 0.00042 C27 0.35038 1.05676 0.24867 1.00000 0.03370 0.02345 0.02288 0.01517 0.01214 0.01839 0.02329 0.00687 0.00026 0.00022 0.00019 0.00000 0.00126 0.00111 0.00112 0.00095 0.00098 0.00102 0.00046 C28 0.48313 1.08004 0.25670 1.00000 0.03057 0.01801 0.02248 0.01307 0.01538 0.01062 0.02238 0.00656 0.00025 0.00020 0.00019 0.00000 0.00120 0.00102 0.00110 0.00090 0.00096 0.00094 0.00046 C29 0.54744 1.03704 0.30886 1.00000 0.01949 0.01795 0.02144 0.00894 0.00948 0.00756 0.02016 0.00622 0.00024 0.00020 0.00018 0.00000 0.00106 0.00101 0.00107 0.00087 0.00087 0.00086 0.00043 C30 0.47619 0.96883 0.35851 1.00000 0.01907 0.01637 0.01554 0.00781 0.00718 0.00998 0.01628 0.00585 0.00022 0.00019 0.00017 0.00000 0.00100 0.00095 0.00095 0.00081 0.00081 0.00083 0.00040 N1 0.30112 0.67012 0.20068 1.00000 0.01769 0.01970 0.01479 0.00841 0.00828 0.01234 0.01572 0.00496 0.00018 0.00016 0.00014 0.00000 0.00084 0.00086 0.00083 0.00071 0.00069 0.00073 0.00034 N2 0.45335 0.62370 0.25341 1.00000 0.01865 0.02189 0.01660 0.01002 0.00990 0.01431 0.01652 0.00510 0.00018 0.00017 0.00014 0.00000 0.00086 0.00088 0.00085 0.00073 0.00071 0.00075 0.00035 N3 0.13972 0.79215 0.48666 1.00000 0.01636 0.01613 0.01746 0.00952 0.00875 0.01080 0.01463 0.00487 0.00018 0.00016 0.00014 0.00000 0.00082 0.00082 0.00084 0.00070 0.00069 0.00070 0.00034 N4 0.26632 0.86463 0.39569 1.00000 0.01684 0.01661 0.01639 0.00982 0.00903 0.01090 0.01447 0.00490 0.00018 0.00016 0.00014 0.00000 0.00082 0.00082 0.00082 0.00069 0.00069 0.00070 0.00033 S1 0.09363 0.54996 0.41202 1.00000 0.01516 0.01587 0.02021 0.01031 0.00798 0.00922 0.01562 0.00143 0.00005 0.00005 0.00004 0.00000 0.00023 0.00023 0.00025 0.00020 0.00020 0.00020 0.00011 S2 0.22755 0.55880 0.53695 1.00000 0.01950 0.02419 0.02169 0.01526 0.01160 0.01496 0.01808 0.00156 0.00005 0.00005 0.00004 0.00000 0.00025 0.00026 0.00026 0.00022 0.00021 0.00022 0.00012 S3 0.36991 0.53138 0.47535 1.00000 0.02029 0.02363 0.02495 0.01551 0.01256 0.01577 0.01902 0.00159 0.00006 0.00005 0.00005 0.00000 0.00026 0.00026 0.00027 0.00022 0.00022 0.00022 0.00012 S4 0.49565 0.69719 0.47225 1.00000 0.01567 0.02119 0.01655 0.00973 0.00674 0.01023 0.01694 0.00146 0.00005 0.00005 0.00004 0.00000 0.00024 0.00025 0.00024 0.00020 0.00019 0.00021 0.00012 S5 0.40138 0.57953 0.04310 1.00000 0.02782 0.03687 0.01616 0.01048 0.01198 0.02179 0.02475 0.00172 0.00006 0.00006 0.00005 0.00000 0.00030 0.00032 0.00026 0.00024 0.00023 0.00026 0.00013 S6 0.20874 1.03064 0.52690 1.00000 0.02694 0.01879 0.02444 0.01242 0.01495 0.01659 0.01975 0.00161 0.00006 0.00005 0.00005 0.00000 0.00028 0.00025 0.00027 0.00022 0.00023 0.00022 0.00012 F1 -0.06701 0.70515 -0.06963 1.00000 0.06579 0.09937 0.03955 0.03794 0.01200 0.06503 0.05749 0.00618 0.00022 0.00022 0.00015 0.00000 0.00127 0.00163 0.00100 0.00108 0.00091 0.00128 0.00056 F2 0.80441 0.43673 0.22077 1.00000 0.06435 0.09259 0.03612 0.03043 0.02451 0.07156 0.05008 0.00587 0.00020 0.00020 0.00014 0.00000 0.00118 0.00145 0.00090 0.00096 0.00086 0.00120 0.00050 F3 -0.17253 0.76670 0.75700 1.00000 0.03272 0.04025 0.03006 0.01913 0.02453 0.02191 0.03025 0.00435 0.00015 0.00014 0.00012 0.00000 0.00077 0.00082 0.00075 0.00067 0.00065 0.00069 0.00032 F4 0.55372 1.14733 0.20888 1.00000 0.04129 0.03103 0.03839 0.02719 0.02449 0.01692 0.03246 0.00446 0.00016 0.00014 0.00013 0.00000 0.00086 0.00077 0.00084 0.00070 0.00071 0.00069 0.00034 H8 0.03955 0.58530 0.16701 1.00000 0.01637 0.07046 0.00261 0.00239 0.00209 0.00000 0.00604 H9 -0.12120 0.60119 0.05274 1.00000 0.03607 0.08783 0.00337 0.00289 0.00251 0.00000 0.00803 H11 0.18994 0.79679 -0.03459 1.00000 0.04803 0.09707 0.00361 0.00326 0.00288 0.00000 0.00947 H12 0.34593 0.78232 0.08095 1.00000 0.02940 0.08300 0.00320 0.00271 0.00234 0.00000 0.00741 H14 0.71336 0.73827 0.27799 1.00000 0.03370 0.08646 0.00312 0.00296 0.00245 0.00000 0.00782 H15 0.86994 0.66047 0.26601 1.00000 0.04427 0.09518 0.00361 0.00313 0.00270 0.00000 0.00896 H17 0.55112 0.32273 0.20248 1.00000 0.05155 0.10131 0.00369 0.00348 0.00289 0.00000 0.00990 H18 0.39947 0.40031 0.21717 1.00000 0.03542 0.08780 0.00334 0.00289 0.00248 0.00000 0.00802 H20 0.16574 0.74621 0.65474 1.00000 0.01642 0.07072 0.00269 0.00234 0.00205 0.00000 0.00602 H21 0.03027 0.73021 0.76342 1.00000 0.02374 0.07597 0.00281 0.00253 0.00228 0.00000 0.00677 H23 -0.20988 0.80677 0.59241 1.00000 0.03097 0.08277 0.00312 0.00274 0.00240 0.00000 0.00746 H24 -0.07449 0.82139 0.47981 1.00000 0.01852 0.07169 0.00264 0.00237 0.00214 0.00000 0.00621 H26 0.18671 0.96636 0.29356 1.00000 0.01738 0.07230 0.00278 0.00236 0.00208 0.00000 0.00611 H27 0.30930 1.08555 0.21131 1.00000 0.02735 0.07896 0.00295 0.00264 0.00233 0.00000 0.00711 H29 0.63561 1.05020 0.30998 1.00000 0.02115 0.07539 0.00291 0.00248 0.00215 0.00000 0.00648 H30 0.51639 0.93601 0.39661 1.00000 0.01768 0.07064 0.00262 0.00237 0.00208 0.00000 0.00613 C311_a 0.30460 0.13894 0.93536 0.75896 0.05189 0.03585 0.03161 0.01423 0.01523 0.02364 0.03954 0.01441 0.00054 0.00046 0.00040 0.00440 0.00250 0.00245 0.00254 0.00201 0.00198 0.00222 0.00106 H311_a 0.37614 0.22942 0.96603 0.75896 0.04744 0.00440 0.00000 Cl31_a 0.19412 0.12462 1.01153 0.75896 0.08467 0.11026 0.07152 0.05412 0.05773 0.07276 0.07130 0.00692 0.00022 0.00022 0.00017 0.00440 0.00122 0.00141 0.00115 0.00109 0.00102 0.00116 0.00056 Cl32_a 0.38949 0.05854 0.95101 0.75896 0.05065 0.06561 0.04458 0.03273 0.02745 0.03422 0.04785 0.00402 0.00013 0.00014 0.00010 0.00440 0.00068 0.00080 0.00066 0.00059 0.00052 0.00060 0.00040 Cl33_a 0.22038 0.08378 0.79821 0.75896 0.07151 0.02758 0.02751 0.01028 0.00510 0.02054 0.04640 0.00308 0.00014 0.00010 0.00008 0.00440 0.00081 0.00052 0.00052 0.00039 0.00046 0.00050 0.00041 C411_b 0.26958 0.14363 0.93651 0.24104 0.51610 0.10177 0.08310 -0.06245 0.20879 -0.16579 0.38852 0.06125 0.00240 0.00213 0.00168 0.00440 0.08996 0.02432 0.02143 0.01764 0.04112 0.03816 0.06344 H411_b 0.32329 0.23650 0.98145 0.24104 0.46623 0.00440 0.00000 Cl41_b 0.35667 0.07068 0.95885 0.24104 0.61708 0.17529 0.41542 0.06035 -0.19707 0.19518 0.47661 0.06240 0.00293 0.00191 0.00213 0.00440 0.05028 0.01571 0.03443 0.01825 0.03327 0.02408 0.02874 Cl42_b 0.19375 0.09534 0.80501 0.24104 0.76344 0.14804 0.42603 0.11592 0.32306 0.07225 0.50218 0.06446 0.00338 0.00194 0.00171 0.00440 0.07126 0.01635 0.04134 0.02103 0.04699 0.02614 0.03139 Cl43_b 0.12579 0.06772 0.96817 0.24104 0.15607 0.25736 0.10005 0.03639 0.05865 0.11263 0.18121 0.04200 0.00152 0.00153 0.00096 0.00440 0.01073 0.01541 0.00739 0.00823 0.00723 0.01072 0.00612 Final Structure Factor Calculation for s92 in P-1 Total number of l.s. parameters = 534 Maximum vector length = 511 Memory required = 4260 / 25039 wR2 = 0.1038 before cycle 7 for 7667 data and 0 / 534 parameters Disagreeable restraints before cycle 7 Observed Target Error Sigma Restraint 0.0920 0.0200 SAME/SADI C311_a Cl32_a C411_b Cl42_b 0.2914 0.0400 SAME/SADI Cl31_a Cl33_a Cl41_b Cl43_b 0.2714 0.0400 SAME/SADI Cl32_a Cl33_a Cl42_b Cl43_b Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.167 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.669; Restrained GooF = 0.674 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0690 * P )^2 + 6.39 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0382 for 6356 Fo > 4sig(Fo) and 0.0493 for all 7667 data wR2 = 0.1038, GooF = S = 0.669, Restrained GooF = 0.674 for all data Occupancy sum of asymmetric unit = 48.00 for non-hydrogen and 17.00 for hydrogen atoms Principal mean square atomic displacements U 0.0215 0.0186 0.0110 C1 0.0189 0.0138 0.0121 C2 0.0168 0.0149 0.0117 C3 0.0165 0.0133 0.0118 C4 0.0181 0.0146 0.0096 C5 0.0186 0.0131 0.0121 C6 0.0256 0.0146 0.0126 C7 0.0287 0.0201 0.0164 C8 0.0498 0.0242 0.0168 C9 0.0634 0.0279 0.0143 C10 0.0516 0.0308 0.0168 C11 0.0306 0.0241 0.0192 C12 0.0265 0.0157 0.0105 C13 0.0366 0.0235 0.0163 C14 0.0594 0.0242 0.0137 C15 0.0701 0.0166 0.0097 C16 0.0602 0.0280 0.0160 C17 0.0380 0.0240 0.0191 C18 0.0192 0.0151 0.0114 C19 0.0201 0.0151 0.0143 C20 0.0241 0.0193 0.0145 C21 0.0317 0.0213 0.0093 C22 0.0269 0.0236 0.0131 C23 0.0208 0.0182 0.0145 C24 0.0197 0.0155 0.0114 C25 0.0233 0.0176 0.0154 C26 0.0338 0.0225 0.0135 C27 0.0355 0.0205 0.0111 C28 0.0258 0.0195 0.0153 C29 0.0192 0.0152 0.0144 C30 0.0207 0.0154 0.0110 N1 0.0232 0.0160 0.0103 N2 0.0194 0.0134 0.0111 N3 0.0196 0.0124 0.0114 N4 0.0205 0.0136 0.0128 S1 0.0269 0.0140 0.0133 S2 0.0282 0.0164 0.0124 S3 0.0213 0.0155 0.0141 S4 0.0397 0.0231 0.0115 S5 0.0304 0.0175 0.0113 S6 0.1073 0.0522 0.0129 F1 0.1071 0.0320 0.0111 F2 0.0419 0.0386 0.0103 F3 0.0486 0.0378 0.0110 F4 0.0525 0.0362 0.0298 C311_a 0.1171 0.0692 0.0276 Cl31_a 0.0660 0.0479 0.0296 Cl32_a 0.0840 0.0294 0.0258 Cl33_a 1.1347 0.0330 -0.0021 C411_b ** NON POSITIVE DEFINITE ** 1.0953 0.2260 0.1086 Cl41_b may be split into 0.3454 0.0944 0.9853 and 0.3679 0.0470 0.9324 1.0514 0.3240 0.1312 Cl42_b may be split into 0.2210 0.0839 0.8153 and 0.1665 0.1068 0.7947 0.3148 0.1497 0.0791 Cl43_b Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.012 0.023 0.034 0.048 0.061 0.076 0.096 0.122 0.166 1.000 Number in group 831. 750. 738. 804. 733. 750. 761. 777. 752. 771. GooF 0.763 0.728 0.692 0.646 0.641 0.662 0.638 0.646 0.615 0.635 K 1.260 0.958 0.946 0.976 0.972 0.984 1.003 1.009 1.019 0.994 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.65 inf Number in group 770. 765. 780. 749. 790. 761. 750. 773. 767. 762. GooF 0.696 0.648 0.639 0.629 0.597 0.609 0.576 0.589 0.694 0.938 K 0.974 1.004 1.028 1.019 1.026 1.003 1.005 1.010 1.012 0.978 R1 0.102 0.087 0.070 0.058 0.052 0.046 0.036 0.032 0.034 0.037 Recommended weighting scheme: WGHT 0.0429 1.7293 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) -6 3 3 56.40 2.70 6.92 0.007 1.81 -4 1 6 748.37 508.52 4.98 0.096 1.88 1 -2 4 447.44 284.51 4.79 0.072 3.17 0 -1 3 34.73 3.66 4.59 0.008 4.58 -4 2 6 118.26 215.21 4.09 0.063 1.79 -2 -8 10 105.28 48.26 4.01 0.030 1.15 -3 -4 6 498.30 347.81 3.99 0.080 1.76 -5 1 6 178.64 102.13 3.92 0.043 1.72 -4 0 7 428.89 296.69 3.80 0.073 1.72 3 8 2 -8.81 15.61 3.59 0.017 0.97 -6 1 2 111.00 58.91 3.51 0.033 1.80 -3 -2 2 39.59 12.12 3.47 0.015 2.54 1 -6 6 122.73 68.26 3.46 0.035 1.86 -3 -3 6 316.50 218.00 3.46 0.063 1.91 -7 4 3 61.61 25.57 3.46 0.022 1.56 -5 1 4 1572.89 1266.70 3.45 0.152 2.01 0 -1 4 530.71 390.37 3.45 0.084 3.39 -6 2 4 81.09 147.48 3.45 0.052 1.75 6 -4 2 208.90 311.99 3.43 0.075 1.74 1 -2 3 598.50 450.12 3.41 0.091 4.04 -13 1 10 -26.14 15.81 3.37 0.017 0.77 0 1 1 3023.26 3847.12 3.33 0.265 6.69 -2 2 3 690.83 890.00 3.32 0.127 3.08 -9 13 6 -16.90 11.23 3.30 0.014 0.78 13 -11 4 27.23 75.65 3.29 0.037 0.80 -4 1 4 35.05 10.41 3.27 0.014 2.34 -4 2 15 45.66 10.75 3.22 0.014 0.82 -6 1 5 496.79 652.60 3.21 0.109 1.66 2 5 0 757.94 594.80 3.18 0.104 1.67 1 4 0 475.83 624.75 3.17 0.107 2.29 1 -2 2 2756.74 3364.61 3.15 0.247 5.26 -6 -1 5 327.39 233.75 3.15 0.065 1.55 -10 7 6 26.23 68.45 3.13 0.035 1.00 -8 -7 1 -24.53 11.32 3.13 0.014 0.79 -11 1 0 3.49 29.41 3.09 0.023 0.91 -1 -6 5 749.73 591.91 3.08 0.104 1.79 -8 -4 12 -4.45 18.54 3.08 0.018 0.91 0 4 3 49.90 21.11 3.08 0.020 1.88 -6 4 5 200.73 133.93 3.04 0.049 1.54 -5 1 3 542.15 418.21 3.03 0.087 2.12 0 -6 6 28.19 8.09 3.03 0.012 1.82 -2 -4 6 320.33 433.74 3.01 0.089 1.94 -8 3 6 568.71 440.72 3.01 0.090 1.27 -1 2 0 459.60 596.79 3.00 0.104 6.22 -3 4 0 411.19 539.96 3.00 0.099 2.91 -5 -9 15 68.52 24.18 3.00 0.021 0.80 -4 -2 5 2691.12 2281.88 2.99 0.204 1.93 -4 4 0 1048.42 1294.33 2.98 0.153 2.55 4 1 3 309.60 224.72 2.96 0.064 1.64 2 -1 8 65.88 32.70 2.96 0.024 1.42 Bond lengths and angles C1 - Distance Angles N2 1.3719 (0.0027) N1 1.3852 (0.0026) 104.54 (0.17) S5 1.6559 (0.0021) 126.03 (0.16) 129.42 (0.16) C1 - N2 N1 C2 - Distance Angles C3 1.3589 (0.0028) N2 1.3936 (0.0026) 106.95 (0.18) S4 1.7336 (0.0021) 129.26 (0.16) 123.17 (0.15) C2 - C3 N2 C3 - Distance Angles C2 1.3589 (0.0028) N1 1.3923 (0.0026) 107.36 (0.17) C4 1.4488 (0.0027) 127.58 (0.19) 124.95 (0.18) C3 - C2 N1 C4 - Distance Angles C5 1.3616 (0.0028) N4 1.3910 (0.0025) 107.13 (0.17) C3 1.4488 (0.0027) 128.41 (0.18) 124.36 (0.18) C4 - C5 N4 C5 - Distance Angles C4 1.3616 (0.0028) N3 1.4007 (0.0025) 107.19 (0.17) S1 1.7351 (0.0020) 126.43 (0.15) 125.45 (0.15) C5 - C4 N3 C6 - Distance Angles N4 1.3737 (0.0026) N3 1.3770 (0.0026) 105.24 (0.17) S6 1.6643 (0.0021) 126.45 (0.15) 128.16 (0.16) C6 - N4 N3 C7 - Distance Angles C8 1.3844 (0.0032) C12 1.3866 (0.0032) 121.56 (0.21) N1 1.4330 (0.0026) 119.40 (0.19) 119.04 (0.20) C7 - C8 C12 C8 - Distance Angles C7 1.3844 (0.0032) C9 1.3878 (0.0033) 119.40 (0.23) H8 0.9321 (0.0263) 119.31 (1.57) 121.25 (1.58) C8 - C7 C9 C9 - Distance Angles C10 1.3733 (0.0041) C8 1.3878 (0.0033) 117.95 (0.24) H9 0.9641 (0.0321) 120.51 (1.88) 121.47 (1.89) C9 - C10 C8 C10 - Distance Angles F1 1.3566 (0.0028) C11 1.3719 (0.0043) 118.15 (0.26) C9 1.3733 (0.0041) 118.27 (0.26) 123.57 (0.23) C10 - F1 C11 C11 - Distance Angles C10 1.3719 (0.0043) C12 1.3840 (0.0035) 118.44 (0.25) H11 0.9187 (0.0359) 121.18 (2.21) 120.39 (2.23) C11 - C10 C12 C12 - Distance Angles C11 1.3840 (0.0035) C7 1.3866 (0.0032) 119.06 (0.24) H12 0.9197 (0.0303) 121.94 (1.83) 119.00 (1.83) C12 - C11 C7 C13 - Distance Angles C18 1.3770 (0.0033) C14 1.3821 (0.0032) 121.37 (0.21) N2 1.4336 (0.0026) 119.34 (0.20) 119.24 (0.20) C13 - C18 C14 C14 - Distance Angles C13 1.3821 (0.0032) C15 1.3879 (0.0034) 119.36 (0.24) H14 0.9598 (0.0312) 118.79 (1.82) 121.79 (1.84) C14 - C13 C15 C15 - Distance Angles C16 1.3682 (0.0042) C14 1.3879 (0.0034) 118.27 (0.24) H15 0.9932 (0.0347) 121.12 (1.96) 120.61 (1.98) C15 - C16 C14 C16 - Distance Angles F2 1.3582 (0.0026) C17 1.3611 (0.0043) 118.78 (0.26) C15 1.3682 (0.0042) 118.02 (0.26) 123.20 (0.22) C16 - F2 C17 C17 - Distance Angles C16 1.3611 (0.0043) C18 1.3900 (0.0034) 118.74 (0.25) H17 0.9321 (0.0369) 121.46 (2.24) 119.80 (2.26) C17 - C16 C18 C18 - Distance Angles C13 1.3770 (0.0032) C17 1.3900 (0.0034) 119.06 (0.25) H18 0.9674 (0.0320) 120.24 (1.83) 120.68 (1.84) C18 - C13 C17 C19 - Distance Angles C20 1.3870 (0.0029) C24 1.3895 (0.0029) 120.92 (0.19) N3 1.4324 (0.0025) 120.32 (0.18) 118.75 (0.18) C19 - C20 C24 C20 - Distance Angles C19 1.3870 (0.0029) C21 1.3902 (0.0030) 119.48 (0.20) H20 0.9233 (0.0264) 121.21 (1.59) 119.29 (1.58) C20 - C19 C21 C21 - Distance Angles C22 1.3760 (0.0032) C20 1.3902 (0.0030) 118.47 (0.20) H21 0.9125 (0.0284) 121.42 (1.75) 120.07 (1.75) C21 - C22 C20 C22 - Distance Angles F3 1.3537 (0.0024) C21 1.3760 (0.0032) 118.75 (0.20) C23 1.3775 (0.0033) 118.29 (0.20) 122.96 (0.20) C22 - F3 C21 C23 - Distance Angles C22 1.3775 (0.0033) C24 1.3837 (0.0030) 118.41 (0.21) H23 0.9628 (0.0304) 121.36 (1.78) 120.14 (1.77) C23 - C22 C24 C24 - Distance Angles C23 1.3837 (0.0030) C19 1.3895 (0.0029) 119.76 (0.20) H24 0.9650 (0.0265) 119.41 (1.55) 120.84 (1.55) C24 - C23 C19 C25 - Distance Angles C30 1.3843 (0.0029) C26 1.3875 (0.0029) 121.63 (0.19) N4 1.4348 (0.0025) 118.66 (0.18) 119.63 (0.19) C25 - C30 C26 C26 - Distance Angles C25 1.3875 (0.0029) C27 1.3907 (0.0031) 119.12 (0.21) H26 0.9443 (0.0268) 118.67 (1.57) 122.20 (1.56) C26 - C25 C27 C27 - Distance Angles C28 1.3785 (0.0034) C26 1.3907 (0.0031) 118.02 (0.21) H27 0.9252 (0.0295) 121.35 (1.80) 120.61 (1.81) C27 - C28 C26 C28 - Distance Angles F4 1.3564 (0.0024) C29 1.3711 (0.0033) 117.85 (0.21) C27 1.3785 (0.0034) 118.49 (0.21) 123.64 (0.20) C28 - F4 C29 C29 - Distance Angles C28 1.3711 (0.0033) C30 1.3869 (0.0030) 118.16 (0.21) H29 0.9342 (0.0280) 122.17 (1.66) 119.64 (1.65) C29 - C28 C30 C30 - Distance Angles C25 1.3843 (0.0029) C29 1.3869 (0.0030) 119.39 (0.20) H30 0.9704 (0.0262) 118.72 (1.53) 121.86 (1.54) C30 - C25 C29 N1 - Distance Angles C1 1.3852 (0.0026) C3 1.3923 (0.0026) 110.27 (0.17) C7 1.4330 (0.0026) 124.11 (0.17) 125.56 (0.17) N1 - C1 C3 N2 - Distance Angles C1 1.3719 (0.0027) C2 1.3936 (0.0026) 110.88 (0.17) C13 1.4336 (0.0026) 122.65 (0.17) 126.37 (0.17) N2 - C1 C2 N3 - Distance Angles C6 1.3770 (0.0026) C5 1.4007 (0.0025) 109.88 (0.16) C19 1.4324 (0.0025) 123.74 (0.17) 126.38 (0.17) N3 - C6 C5 N4 - Distance Angles C6 1.3737 (0.0026) C4 1.3910 (0.0025) 110.48 (0.16) C25 1.4348 (0.0026) 125.12 (0.17) 124.38 (0.17) N4 - C6 C4 S1 - Distance Angles C5 1.7351 (0.0020) S2 2.0752 (0.0007) 104.22 (0.07) S1 - C5 S2 - Distance Angles S3 2.0338 (0.0007) S1 2.0752 (0.0007) 105.21 (0.03) S2 - S3 S3 - Distance Angles S2 2.0338 (0.0007) S4 2.0734 (0.0008) 104.78 (0.03) S3 - S2 S4 - Distance Angles C2 1.7336 (0.0021) S3 2.0734 (0.0008) 101.68 (0.07) S4 - C2 S5 - Distance Angles C1 1.6559 (0.0021) S5 - S6 - Distance Angles C6 1.6643 (0.0021) S6 - F1 - Distance Angles C10 1.3566 (0.0028) F1 - F2 - Distance Angles C16 1.3582 (0.0026) F2 - F3 - Distance Angles C22 1.3537 (0.0024) F3 - F4 - Distance Angles C28 1.3564 (0.0025) F4 - C311_a - Distance Angles Cl33_a 1.7360 (0.0048) Cl31_a 1.7430 (0.0054) 113.60 (0.29) Cl32_a 1.7576 (0.0044) 110.20 (0.27) 108.11 (0.25) H311_a 1.0000 108.26 108.27 108.26 C311_a - Cl33_a Cl31_a Cl32_a Cl31_a - Distance Angles C311_a 1.7430 (0.0055) Cl31_a - Cl32_a - Distance Angles C311_a 1.7576 (0.0044) Cl32_a - Cl33_a - Distance Angles C311_a 1.7360 (0.0048) Cl33_a - C411_b - Distance Angles Cl42_b 1.6656 (0.0182) Cl41_b 1.7164 (0.0202) 113.48 (1.79) Cl43_b 1.7258 (0.0176) 99.77 (1.44) 99.12 (1.66) H411_b 1.0000 114.25 114.27 114.09 C411_b - Cl42_b Cl41_b Cl43_b Cl41_b - Distance Angles C411_b 1.7164 (0.0203) Cl41_b - Cl42_b - Distance Angles C411_b 1.6656 (0.0182) Cl42_b - Cl43_b - Distance Angles C411_b 1.7258 (0.0177) Cl43_b - FMAP and GRID set by program FMAP 2 2 70 GRID -1.493 -1 -2 1.493 1 2 R1 = 0.0491 for 7667 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.81 at 0.2596 0.0550 0.0045 [ 1.32 A from CL41 ] Deepest hole -0.78 at 0.2531 0.1943 0.0476 [ 0.78 A from CL31 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 4099 / 66457 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2596 0.0550 1.0045 1.00000 0.05 0.81 1.32 CL41 1.40 CL31 1.63 CL43 1.68 C311 Q2 1 0.2916 0.1070 0.8579 1.00000 0.05 0.76 0.93 CL33 0.97 C311 1.14 C411 1.16 CL42 Q3 1 0.3359 0.0627 0.9096 1.00000 0.05 0.51 0.65 CL41 0.81 CL32 1.17 C311 1.53 C411 Q4 1 0.1951 0.1548 0.9032 1.00000 0.05 0.47 1.00 C411 1.31 CL42 1.37 H411 1.38 C311 Q5 1 0.1996 0.1760 0.9927 1.00000 0.05 0.34 0.80 CL31 1.20 CL43 1.29 C411 1.35 H411 Q6 1 0.2965 0.7289 0.3600 1.00000 0.05 0.29 0.69 C4 0.83 C3 1.81 C5 1.84 C2 Q7 1 0.3090 0.6827 0.2566 1.00000 0.05 0.29 0.67 C3 0.72 N1 1.69 C2 1.77 C1 Q8 1 0.2113 0.7203 0.4046 1.00000 0.05 0.28 0.63 C5 0.74 C4 1.74 N3 1.80 N4 Q9 1 0.3582 0.6761 0.3310 1.00000 0.05 0.28 0.69 C3 0.70 C2 1.80 N1 1.80 N2 Q10 1 0.5074 1.0439 0.2679 1.00000 0.05 0.27 0.69 C28 0.73 C29 1.44 H29 1.77 F4 Q11 1 -0.1168 0.7708 0.6403 1.00000 0.05 0.27 0.70 C22 0.71 C23 1.50 H23 1.78 C24 Q12 1 0.2971 0.8997 0.3740 1.00000 0.05 0.27 0.65 N4 0.79 C25 1.81 C6 1.85 C4 Q13 1 0.2568 0.6780 0.1678 1.00000 0.05 0.26 0.70 N1 0.74 C7 1.84 C12 1.86 C1 Q14 1 0.4462 0.6532 0.3084 1.00000 0.05 0.25 0.66 C2 0.76 N2 1.76 C3 1.87 C1 Q15 1 0.0383 0.7505 0.6676 1.00000 0.05 0.25 0.69 C21 0.73 C20 1.46 H21 1.50 H20 Q16 1 0.3057 0.9360 0.2893 1.00000 0.05 0.25 0.83 C26 0.85 C25 1.57 H26 1.78 C27 Q17 1 0.2639 0.8023 0.3796 1.00000 0.05 0.25 0.64 C4 0.77 N4 1.74 C5 1.82 C3 Q18 1 0.4196 0.9712 0.3681 1.00000 0.05 0.25 0.68 C30 0.75 C25 1.42 H30 1.82 C29 Q19 1 0.5081 0.5964 0.2466 1.00000 0.05 0.25 0.60 C13 0.84 N2 1.73 C14 1.76 C18 Q20 1 0.3270 1.0235 0.2829 1.00000 0.05 0.25 0.67 C26 0.76 C27 1.50 H26 1.54 H27 Shortest distances between peaks (including symmetry equivalents) 16 20 1.12 6 17 1.14 7 9 1.16 4 5 1.17 8 17 1.20 6 9 1.20 6 8 1.21 9 14 1.21 12 17 1.22 2 3 1.25 7 13 1.26 12 18 1.34 16 18 1.35 14 19 1.40 6 7 1.41 12 16 1.42 2 4 1.58 1 3 1.69 7 14 1.87 11 15 1.89 18 20 1.96 10 20 1.99 1 5 2.04 10 18 2.09 7 17 2.18 6 12 2.21 8 9 2.25 10 16 2.25 17 18 2.26 9 17 2.31 12 20 2.35 2 5 2.37 8 12 2.38 6 14 2.39 3 4 2.40 1 2 2.40 9 13 2.41 6 13 2.44 16 17 2.44 7 8 2.47 1 4 2.48 9 19 2.57 3 5 2.69 13 17 2.80 7 12 2.85 6 18 2.86 13 14 2.90 7 19 2.93 13 16 3.00 Time profile in seconds ----------------------- 0.09: Read and process instructions 0.00: Fit rigid groups 0.02: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.02: Analyse other restraints etc. 4.83: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.00: Generate idealized H-atoms 5.08: Structure factors and derivatives 21.23: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.05: Apply other restraints 2.84: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.19: Analysis of variance 0.08: Merge reflections for Fourier and .fcf 0.28: Fourier summations 0.06: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 13:38:27 Total CPU time: 34.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++