+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008sjc0013 started at 13:46:30 on 14-Jul-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008sjc0013 in P-1 CELL 0.71073 10.9590 11.4830 14.0360 96.445 111.731 97.318 ZERR 4.00 0.0001 0.0002 0.0002 0.001 0.001 0.001 LATT 1 SFAC C H AG F N O S UNIT 44 48 4 12 24 12 4 V = 1602.88 F(000) = 936.0 Mu = 1.45 mm-1 Cell Wt = 1892.78 Rho = 1.961 MERG 2 OMIT 2 -1 3 OMIT 1 -1 3 OMIT 1 0 4 OMIT -3 55 FMAP 2 PLAN 10 SIZE 0.08 0.10 0.10 ACTA BOND $H WGHT 0.03620 2.63610 L.S. 5 TEMP -153.00 FVAR 0.48439 C1 1 0.863567 0.536883 0.911254 11.00000 0.01553 0.01433 = 0.02292 0.00307 0.00662 0.00377 C2 1 0.747481 0.341648 0.931977 11.00000 0.02784 0.01752 = 0.04589 0.00806 0.02022 0.00427 AFIX 33 H2A 2 0.741879 0.257476 0.905955 11.00000 -1.50000 H2B 2 0.657681 0.361226 0.907617 11.00000 -1.50000 H2C 2 0.786876 0.356311 1.008282 11.00000 -1.50000 AFIX 0 C3 1 0.891935 0.374226 0.830640 11.00000 0.02074 0.01774 = 0.02425 0.00058 0.00791 0.00602 AFIX 43 H3 2 0.887823 0.293154 0.804673 11.00000 -1.20000 AFIX 0 C4 1 0.960388 0.473192 0.812779 11.00000 0.02302 0.01929 = 0.02199 0.00202 0.00938 0.00809 AFIX 43 H4 2 1.012583 0.471467 0.771794 11.00000 -1.20000 AFIX 0 C5 1 0.817261 0.617283 0.972203 11.00000 0.01477 0.01738 = 0.02302 0.00251 0.00831 0.00372 AFIX 43 H5 2 0.761910 0.587478 1.005794 11.00000 -1.20000 AFIX 0 C6 1 0.840055 0.910266 1.049140 11.00000 0.01646 0.01968 = 0.01799 0.00412 0.00722 0.00692 AFIX 43 H6 2 0.908840 0.936597 1.026445 11.00000 -1.20000 AFIX 0 C7 1 0.788856 0.997492 1.098992 11.00000 0.01677 0.01782 = 0.01809 0.00572 0.00779 0.00482 C8 1 0.582762 0.865907 1.096822 11.00000 0.02074 0.02267 = 0.03858 0.00147 0.01597 -0.00119 AFIX 33 H8A 2 0.511554 0.879327 1.120854 11.00000 -1.50000 H8B 2 0.630033 0.806508 1.132631 11.00000 -1.50000 H8C 2 0.543778 0.836885 1.021544 11.00000 -1.50000 AFIX 0 C9 1 0.662394 1.085727 1.162793 11.00000 0.02070 0.02145 = 0.02233 0.00129 0.01024 0.00877 AFIX 43 H9 2 0.593142 1.100073 1.185416 11.00000 -1.20000 AFIX 0 C10 1 0.766156 1.168420 1.166860 11.00000 0.02239 0.01631 = 0.02124 0.00324 0.00882 0.00757 AFIX 43 H10 2 0.781416 1.251194 1.193127 11.00000 -1.20000 AFIX 0 C11 1 0.236365 0.518000 0.425931 11.00000 0.01977 0.01783 = 0.01996 0.00401 0.00884 0.00569 C12 1 0.362439 0.393670 0.347069 11.00000 0.02833 0.02329 = 0.03326 0.00132 0.01754 0.01013 AFIX 33 H12A 2 0.438056 0.412311 0.326578 11.00000 -1.50000 H12B 2 0.283938 0.351721 0.286158 11.00000 -1.50000 H12C 2 0.385091 0.342884 0.400453 11.00000 -1.50000 AFIX 0 C13 1 0.401748 0.615983 0.397720 11.00000 0.02289 0.02280 = 0.02964 0.00342 0.01465 -0.00009 AFIX 43 H13 2 0.474776 0.634895 0.377704 11.00000 -1.20000 AFIX 0 C14 1 0.345149 0.694214 0.440634 11.00000 0.02808 0.02102 = 0.03219 0.00452 0.01616 -0.00011 AFIX 43 H14 2 0.372671 0.778384 0.455610 11.00000 -1.20000 AFIX 0 C15 1 0.137477 0.425458 0.430329 11.00000 0.02096 0.01676 = 0.02145 0.00337 0.01026 0.00667 AFIX 43 H15 2 0.079379 0.445974 0.463063 11.00000 -1.20000 AFIX 0 C16 1 0.021164 0.129920 0.372573 11.00000 0.01822 0.01795 = 0.01830 0.00387 0.00755 0.00617 AFIX 43 H16 2 0.082651 0.107465 0.344003 11.00000 -1.20000 AFIX 0 C17 1 -0.078384 0.041075 0.381190 11.00000 0.02081 0.01698 = 0.01818 0.00353 0.00687 0.00515 C18 1 -0.013436 -0.142205 0.307671 11.00000 0.02728 0.01907 = 0.02856 0.00197 0.01507 0.00760 AFIX 33 H18A 2 -0.049401 -0.227905 0.291823 11.00000 -1.50000 H18B 2 0.078757 -0.127225 0.359227 11.00000 -1.50000 H18C 2 -0.014991 -0.114140 0.243892 11.00000 -1.50000 AFIX 0 C19 1 -0.199842 -0.131018 0.370500 11.00000 0.01952 0.01969 = 0.02285 0.00281 0.00604 0.00095 AFIX 43 H19 2 -0.235087 -0.213806 0.357982 11.00000 -1.20000 AFIX 0 C20 1 -0.243291 -0.039858 0.413088 11.00000 0.01882 0.02197 = 0.02473 0.00296 0.00993 0.00290 AFIX 43 H20 2 -0.315753 -0.049816 0.434920 11.00000 -1.20000 AFIX 0 C21 1 0.575705 0.424873 0.171155 11.00000 0.03158 0.03743 = 0.04044 -0.00494 0.01419 0.01140 C22 1 0.377980 -0.009469 0.322044 11.00000 0.02921 0.03782 = 0.02791 0.00742 0.01171 0.01341 AG1 3 0.131589 0.714546 0.537802 11.00000 0.02627 0.01972 = 0.02658 0.00348 0.01460 0.00919 AG2 3 0.012884 0.210692 0.104775 11.00000 0.02175 0.01782 = 0.03249 0.00765 0.01524 0.00443 F1 4 0.474393 0.481512 0.142266 11.00000 0.02908 0.06845 = 0.07109 -0.01912 -0.00790 0.02226 F2 4 0.535379 0.327296 0.203646 11.00000 0.05375 0.03506 = 0.08343 -0.01516 0.04430 -0.01461 F3 4 0.601319 0.388201 0.087936 11.00000 0.05483 0.05542 = 0.02864 -0.00619 0.01428 0.01571 F4 4 0.427034 -0.109804 0.312566 11.00000 0.03649 0.03912 = 0.05251 0.02184 0.01726 0.02184 F5 4 0.482229 0.079635 0.367623 11.00000 0.04050 0.04966 = 0.04662 -0.01106 -0.01269 0.00952 F6 4 0.315582 -0.022937 0.387063 11.00000 0.06653 0.10947 = 0.03757 0.03275 0.03304 0.04829 N1 5 0.831261 0.416335 0.893201 11.00000 0.01906 0.01460 = 0.02570 0.00438 0.00938 0.00506 N2 5 0.941674 0.573807 0.862926 11.00000 0.02065 0.01854 = 0.02214 0.00437 0.00858 0.00561 N3 5 0.853334 0.730120 0.979443 11.00000 0.01901 0.01693 = 0.02355 0.00498 0.01050 0.00645 N4 5 0.795053 0.797785 1.034600 11.00000 0.02473 0.01489 = 0.02043 0.00303 0.01133 0.00728 N5 5 0.677261 0.978548 1.120004 11.00000 0.01913 0.01695 = 0.02331 0.00294 0.01023 0.00289 N6 5 0.845280 1.112674 1.126774 11.00000 0.01746 0.01666 = 0.02117 0.00438 0.00920 0.00578 N7 5 0.332770 0.504868 0.389119 11.00000 0.02104 0.02032 = 0.02359 0.00219 0.01149 0.00469 N8 5 0.242655 0.633345 0.458942 11.00000 0.02399 0.01711 = 0.02485 0.00172 0.01348 0.00384 N9 5 0.125853 0.316364 0.391303 11.00000 0.02206 0.01953 = 0.02470 0.00483 0.01187 0.00397 N10 5 0.024492 0.241278 0.404869 11.00000 0.01689 0.02255 = 0.01997 0.00546 0.00842 0.00178 N11 5 -0.095174 -0.078429 0.349640 11.00000 0.01918 0.01355 = 0.02190 0.00187 0.00828 0.00440 N12 5 -0.167933 0.067191 0.419749 11.00000 0.01953 0.01899 = 0.02374 0.00311 0.00848 0.00493 O1 6 0.814642 0.439813 0.306865 11.00000 0.03321 0.03954 = 0.03594 0.00393 0.00726 0.01982 O2 6 0.759994 0.607055 0.218304 11.00000 0.04680 0.02808 = 0.06472 0.01161 0.03359 0.00453 O3 6 0.669344 0.565237 0.348188 11.00000 0.03495 0.03219 = 0.03038 -0.00286 0.01451 0.00921 O4 6 0.219774 0.120792 0.223563 11.00000 0.03657 0.02958 = 0.04323 0.00043 0.00722 0.01892 O5 6 0.164751 -0.090327 0.158857 11.00000 0.02581 0.02455 = 0.04627 0.00043 0.00963 0.00148 O6 6 0.351826 0.026976 0.141179 11.00000 0.02789 0.06240 = 0.03241 0.01888 0.01874 0.01415 S1 7 0.721879 0.519458 0.274062 11.00000 0.01811 0.01962 = 0.03063 -0.00264 0.00848 0.00438 S2 7 0.266168 0.015098 0.197157 11.00000 0.01692 0.01882 = 0.02288 0.00228 0.00780 0.00540 HKLF 4 Covalent radii and connectivity table for 2008sjc0013 in P-1 C 0.770 H 0.320 AG 1.440 F 0.640 N 0.700 O 0.660 S 1.030 C1 - N2 N1 C5 C2 - N1 C3 - N1 C4 C4 - N2 C3 C5 - N3 C1 C6 - N4 C7 C7 - N6 N5 C6 C8 - N5 C9 - N5 C10 C10 - C9 N6 C11 - N8 N7 C15 C12 - N7 C13 - C14 N7 C14 - C13 N8 C15 - N9 C11 C16 - N10 C17 C17 - N12 N11 C16 C18 - N11 C19 - C20 N11 C20 - N12 C19 C21 - F1 F3 F2 S1 C22 - F5 F6 F4 S2 Ag1 - N8 N10_$1 N12_$1 Ag2 - N6_$4 N3_$3 N2_$3 F1 - C21 F2 - C21 F3 - C21 F4 - C22 F5 - C22 F6 - C22 N1 - C1 C3 C2 N2 - C1 C4 Ag2_$3 N3 - C5 N4 Ag2_$3 N4 - C6 N3 N5 - C7 C9 C8 N6 - C7 C10 Ag2_$2 N7 - C11 C13 C12 N8 - C11 C14 Ag1 N9 - C15 N10 N10 - C16 N9 Ag1_$1 N11 - C17 C19 C18 N12 - C17 C20 Ag1_$1 O1 - S1 O2 - S1 O3 - S1 O4 - S2 O5 - S2 O6 - S2 S1 - O1 O3 O2 C21 S2 - O6 O5 O4 C22 Operators for generating equivalent atoms: $1 -x, -y+1, -z+1 $2 x+1, y+1, z+1 $3 -x+1, -y+1, -z+1 $4 x-1, y-1, z-1 35984 Reflections read, of which 25 rejected -14 =< h =< 14, -14 =< k =< 14, -18 =< 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) -9 -5 4 -0.01 0.18 4 5.27 1 Inconsistent equivalents 7338 Unique reflections, of which 0 suppressed R(int) = 0.0488 R(sigma) = 0.0395 Friedel opposites merged Maximum memory for data reduction = 3838 / 73723 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 = 5024 / 589811 wR2 = 0.0878 before cycle 1 for 7338 data and 451 / 451 parameters GooF = S = 1.060; Restrained GooF = 1.060 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0362 * P )^2 + 2.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.48436 0.00054 -0.052 OSF Mean shift/esd = 0.028 Maximum = -0.139 for U12 C3 Max. shift = 0.000 A for C4 Max. dU = 0.000 for C2 Least-squares cycle 2 Maximum vector length = 511 Memory required = 5024 / 589811 wR2 = 0.0878 before cycle 2 for 7338 data and 451 / 451 parameters GooF = S = 1.061; Restrained GooF = 1.061 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0362 * P )^2 + 2.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.48435 0.00054 -0.031 OSF Mean shift/esd = 0.009 Maximum = -0.045 for U12 C3 Max. shift = 0.000 A for C4 Max. dU = 0.000 for C2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 5024 / 589811 wR2 = 0.0878 before cycle 3 for 7338 data and 451 / 451 parameters GooF = S = 1.061; Restrained GooF = 1.061 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0362 * P )^2 + 2.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.48435 0.00054 -0.001 OSF Mean shift/esd = 0.000 Maximum = 0.002 for y C17 Max. shift = 0.000 A for C17 Max. dU = 0.000 for C21 Least-squares cycle 4 Maximum vector length = 511 Memory required = 5024 / 589811 wR2 = 0.0878 before cycle 4 for 7338 data and 451 / 451 parameters GooF = S = 1.060; Restrained GooF = 1.060 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0362 * P )^2 + 2.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.48435 0.00054 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z Ag1 Max. shift = 0.000 A for C2 Max. dU = 0.000 for C21 Least-squares cycle 5 Maximum vector length = 511 Memory required = 5024 / 589811 wR2 = 0.0878 before cycle 5 for 7338 data and 451 / 451 parameters GooF = S = 1.060; Restrained GooF = 1.060 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0362 * P )^2 + 2.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.48435 0.00054 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for z Ag1 Max. shift = 0.000 A for C8 Max. dU = 0.000 for C10 Largest correlation matrix elements 0.631 U13 F2 / U33 F2 0.553 U13 O2 / U11 O2 0.532 U13 C8 / U33 C8 0.601 U13 F6 / U33 F6 0.553 U13 C2 / U33 C2 0.529 U13 N8 / U33 N8 0.601 U13 F2 / U11 F2 0.552 U12 F6 / U23 F6 0.527 z F2 / x F2 0.593 U13 O2 / U33 O2 0.551 U13 C12 / U33 C12 0.524 U13 Ag1 / U11 Ag1 0.592 U13 F6 / U11 F6 0.535 U13 C18 / U33 C18 0.522 U13 O6 / U11 O6 0.567 U13 Ag2 / U33 Ag2 0.535 U13 C13 / U33 C13 0.519 U13 Ag2 / U11 Ag2 0.561 U13 Ag1 / U33 Ag1 0.535 U13 C14 / U33 C14 0.519 z F6 / x F6 0.559 U13 O6 / U33 O6 0.533 U12 F2 / U23 F2 0.518 U13 N7 / U33 N7 Idealized hydrogen atom generation before cycle 6 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2A 0.7419 0.2575 0.9059 33 0.980 0.000 C2 N1 H2A H2B 0.6577 0.3612 0.9076 33 0.980 0.000 C2 N1 H2A H2C 0.7869 0.3563 1.0083 33 0.980 0.000 C2 N1 H2A H3 0.8878 0.2932 0.8047 43 0.950 0.000 C3 N1 C4 H4 1.0125 0.4714 0.7718 43 0.950 0.000 C4 N2 C3 H5 0.7619 0.5875 1.0058 43 0.950 0.000 C5 N3 C1 H6 0.9088 0.9366 1.0264 43 0.950 0.000 C6 N4 C7 H8A 0.5115 0.8793 1.1208 33 0.980 0.000 C8 N5 H8A H8B 0.6300 0.8065 1.1326 33 0.980 0.000 C8 N5 H8A H8C 0.5438 0.8369 1.0215 33 0.980 0.000 C8 N5 H8A H9 0.5931 1.1001 1.1854 43 0.950 0.000 C9 N5 C10 H10 0.7814 1.2512 1.1931 43 0.950 0.000 C10 C9 N6 H12A 0.4381 0.4123 0.3266 33 0.980 0.000 C12 N7 H12A H12B 0.2839 0.3517 0.2862 33 0.980 0.000 C12 N7 H12A H12C 0.3851 0.3429 0.4004 33 0.980 0.000 C12 N7 H12A H13 0.4748 0.6349 0.3777 43 0.950 0.000 C13 C14 N7 H14 0.3727 0.7784 0.4556 43 0.950 0.000 C14 C13 N8 H15 0.0793 0.4460 0.4630 43 0.950 0.000 C15 N9 C11 H16 0.0826 0.1075 0.3440 43 0.950 0.000 C16 N10 C17 H18A -0.0494 -0.2279 0.2918 33 0.980 0.000 C18 N11 H18A H18B 0.0787 -0.1272 0.3592 33 0.980 0.000 C18 N11 H18A H18C -0.0150 -0.1141 0.2439 33 0.980 0.000 C18 N11 H18A H19 -0.2351 -0.2138 0.3580 43 0.950 0.000 C19 C20 N11 H20 -0.3157 -0.0498 0.4349 43 0.950 0.000 C20 N12 C19 2008sjc0013 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.86357 0.53689 0.91125 1.00000 0.01557 0.01434 0.02295 0.00315 0.00666 0.00385 0.01777 0.00641 0.00027 0.00025 0.00023 0.00000 0.00127 0.00138 0.00144 0.00111 0.00110 0.00103 0.00056 C2 0.74748 0.34163 0.93197 1.00000 0.02769 0.01734 0.04575 0.00789 0.02003 0.00412 0.02837 0.00796 0.00033 0.00029 0.00029 0.00000 0.00161 0.00156 0.00202 0.00140 0.00150 0.00124 0.00071 H2A 0.74188 0.25746 0.90594 1.00000 0.04256 0.00000 0.00000 H2B 0.65767 0.36121 0.90761 1.00000 0.04256 0.00000 0.00000 H2C 0.78687 0.35630 1.00827 1.00000 0.04256 0.00000 0.00000 C3 0.89194 0.37423 0.83064 1.00000 0.02056 0.01771 0.02418 0.00046 0.00775 0.00581 0.02116 0.00676 0.00029 0.00028 0.00023 0.00000 0.00140 0.00148 0.00150 0.00117 0.00118 0.00112 0.00060 H3 0.88785 0.29316 0.80469 1.00000 0.02539 0.00000 0.00000 C4 0.96037 0.47316 0.81277 1.00000 0.02295 0.01929 0.02195 0.00199 0.00933 0.00801 0.02096 0.00680 0.00030 0.00027 0.00023 0.00000 0.00144 0.00150 0.00145 0.00117 0.00119 0.00115 0.00060 H4 1.01255 0.47142 0.77177 1.00000 0.02516 0.00000 0.00000 C5 0.81727 0.61730 0.97221 1.00000 0.01480 0.01746 0.02303 0.00257 0.00836 0.00379 0.01814 0.00642 0.00027 0.00026 0.00023 0.00000 0.00126 0.00144 0.00144 0.00113 0.00111 0.00105 0.00057 H5 0.76191 0.58750 1.00580 1.00000 0.02177 0.00000 0.00000 C6 0.84005 0.91027 1.04914 1.00000 0.01647 0.01959 0.01800 0.00410 0.00721 0.00692 0.01746 0.00644 0.00027 0.00026 0.00022 0.00000 0.00129 0.00148 0.00135 0.00111 0.00108 0.00108 0.00056 H6 0.90883 0.93659 1.02644 1.00000 0.02095 0.00000 0.00000 C7 0.78887 0.99752 1.09900 1.00000 0.01675 0.01783 0.01811 0.00572 0.00778 0.00481 0.01690 0.00647 0.00027 0.00026 0.00022 0.00000 0.00129 0.00142 0.00133 0.00109 0.00108 0.00106 0.00055 C8 0.58274 0.86589 1.09680 1.00000 0.02065 0.02247 0.03859 0.00135 0.01590 -0.00129 0.02678 0.00723 0.00031 0.00029 0.00027 0.00000 0.00149 0.00164 0.00186 0.00137 0.00138 0.00121 0.00069 H8A 0.51153 0.87931 1.12083 1.00000 0.04018 0.00000 0.00000 H8B 0.63001 0.80648 1.13260 1.00000 0.04018 0.00000 0.00000 H8C 0.54376 0.83688 1.02152 1.00000 0.04018 0.00000 0.00000 C9 0.66240 1.08574 1.16280 1.00000 0.02067 0.02130 0.02234 0.00124 0.01020 0.00866 0.02065 0.00678 0.00029 0.00027 0.00023 0.00000 0.00139 0.00154 0.00146 0.00118 0.00117 0.00116 0.00060 H9 0.59315 1.10008 1.18542 1.00000 0.02479 0.00000 0.00000 C10 0.76615 1.16841 1.16685 1.00000 0.02240 0.01642 0.02120 0.00330 0.00884 0.00765 0.01952 0.00681 0.00029 0.00027 0.00023 0.00000 0.00141 0.00142 0.00143 0.00112 0.00116 0.00111 0.00058 H10 0.78141 1.25118 1.19312 1.00000 0.02342 0.00000 0.00000 C11 0.23638 0.51800 0.42594 1.00000 0.01978 0.01773 0.01997 0.00394 0.00886 0.00568 0.01856 0.00661 0.00028 0.00026 0.00022 0.00000 0.00138 0.00145 0.00140 0.00112 0.00113 0.00110 0.00057 C12 0.36243 0.39367 0.34706 1.00000 0.02833 0.02333 0.03327 0.00135 0.01755 0.01010 0.02646 0.00761 0.00032 0.00029 0.00026 0.00000 0.00162 0.00167 0.00175 0.00134 0.00140 0.00130 0.00068 H12A 0.43805 0.41231 0.32657 1.00000 0.03969 0.00000 0.00000 H12B 0.28393 0.35172 0.28615 1.00000 0.03969 0.00000 0.00000 H12C 0.38509 0.34288 0.40044 1.00000 0.03969 0.00000 0.00000 C13 0.40176 0.61600 0.39773 1.00000 0.02293 0.02288 0.02967 0.00350 0.01472 -0.00004 0.02434 0.00707 0.00031 0.00028 0.00025 0.00000 0.00147 0.00161 0.00166 0.00128 0.00129 0.00120 0.00064 H13 0.47480 0.63492 0.37773 1.00000 0.02920 0.00000 0.00000 C14 0.34515 0.69421 0.44063 1.00000 0.02805 0.02098 0.03220 0.00450 0.01613 -0.00008 0.02622 0.00743 0.00032 0.00030 0.00026 0.00000 0.00161 0.00161 0.00173 0.00132 0.00138 0.00125 0.00067 H14 0.37266 0.77838 0.45560 1.00000 0.03147 0.00000 0.00000 C15 0.13746 0.42544 0.43031 1.00000 0.02092 0.01692 0.02142 0.00344 0.01026 0.00668 0.01884 0.00664 0.00029 0.00026 0.00023 0.00000 0.00138 0.00145 0.00142 0.00113 0.00115 0.00111 0.00057 H15 0.07934 0.44595 0.46303 1.00000 0.02261 0.00000 0.00000 C16 0.02116 0.12992 0.37257 1.00000 0.01821 0.01796 0.01827 0.00387 0.00753 0.00617 0.01769 0.00644 0.00028 0.00026 0.00022 0.00000 0.00132 0.00145 0.00136 0.00111 0.00110 0.00109 0.00056 H16 0.08265 0.10747 0.34400 1.00000 0.02123 0.00000 0.00000 C17 -0.07838 0.04107 0.38119 1.00000 0.02086 0.01684 0.01824 0.00352 0.00690 0.00514 0.01866 0.00654 0.00029 0.00026 0.00022 0.00000 0.00137 0.00145 0.00136 0.00111 0.00111 0.00110 0.00057 C18 -0.01345 -0.14221 0.30767 1.00000 0.02734 0.01903 0.02858 0.00199 0.01511 0.00769 0.02359 0.00733 0.00031 0.00028 0.00025 0.00000 0.00154 0.00154 0.00162 0.00124 0.00131 0.00121 0.00063 H18A -0.04942 -0.22791 0.29182 1.00000 0.03539 0.00000 0.00000 H18B 0.07875 -0.12724 0.35922 1.00000 0.03539 0.00000 0.00000 H18C -0.01501 -0.11415 0.24389 1.00000 0.03539 0.00000 0.00000 C19 -0.19985 -0.13103 0.37049 1.00000 0.01953 0.01978 0.02284 0.00286 0.00605 0.00100 0.02169 0.00668 0.00029 0.00028 0.00023 0.00000 0.00140 0.00153 0.00150 0.00119 0.00118 0.00113 0.00061 H19 -0.23510 -0.21382 0.35797 1.00000 0.02603 0.00000 0.00000 C20 -0.24329 -0.03987 0.41309 1.00000 0.01885 0.02200 0.02474 0.00298 0.00995 0.00297 0.02160 0.00677 0.00029 0.00027 0.00024 0.00000 0.00138 0.00156 0.00151 0.00121 0.00118 0.00115 0.00061 H20 -0.31575 -0.04982 0.43492 1.00000 0.02592 0.00000 0.00000 C21 0.57571 0.42488 0.17116 1.00000 0.03173 0.03741 0.04047 -0.00488 0.01431 0.01156 0.03694 0.00850 0.00036 0.00035 0.00030 0.00000 0.00182 0.00211 0.00204 0.00163 0.00158 0.00156 0.00084 C22 0.37799 -0.00946 0.32205 1.00000 0.02916 0.03783 0.02787 0.00739 0.01167 0.01335 0.03063 0.00809 0.00034 0.00033 0.00026 0.00000 0.00169 0.00201 0.00170 0.00147 0.00140 0.00146 0.00074 Ag1 0.13159 0.71455 0.53780 1.00000 0.02626 0.01971 0.02658 0.00348 0.01460 0.00919 0.02248 0.00053 0.00002 0.00002 0.00002 0.00000 0.00013 0.00013 0.00013 0.00009 0.00010 0.00009 0.00007 Ag2 0.01288 0.21069 0.10477 1.00000 0.02174 0.01781 0.03248 0.00764 0.01523 0.00442 0.02228 0.00053 0.00002 0.00002 0.00002 0.00000 0.00012 0.00013 0.00014 0.00010 0.00010 0.00009 0.00007 F1 0.47440 0.48152 0.14227 1.00000 0.02900 0.06845 0.07109 -0.01914 -0.00794 0.02218 0.06564 0.00546 0.00023 0.00026 0.00022 0.00000 0.00117 0.00183 0.00179 0.00142 0.00115 0.00118 0.00084 F2 0.53539 0.32730 0.20365 1.00000 0.05382 0.03500 0.08348 -0.01510 0.04437 -0.01453 0.05652 0.00559 0.00025 0.00021 0.00022 0.00000 0.00146 0.00133 0.00187 0.00123 0.00140 0.00109 0.00070 F3 0.60132 0.38819 0.08794 1.00000 0.05478 0.05536 0.02865 -0.00622 0.01426 0.01565 0.04746 0.00520 0.00024 0.00022 0.00017 0.00000 0.00140 0.00152 0.00111 0.00102 0.00102 0.00116 0.00058 F4 0.42703 -0.10981 0.31256 1.00000 0.03647 0.03907 0.05252 0.02183 0.01725 0.02184 0.04013 0.00531 0.00021 0.00020 0.00018 0.00000 0.00112 0.00124 0.00133 0.00104 0.00100 0.00095 0.00051 F5 0.48223 0.07963 0.36762 1.00000 0.04051 0.04977 0.04659 -0.01103 -0.01266 0.00958 0.05588 0.00491 0.00023 0.00023 0.00019 0.00000 0.00127 0.00151 0.00139 0.00114 0.00106 0.00109 0.00069 F6 0.31558 -0.02294 0.38706 1.00000 0.06655 0.10943 0.03758 0.03276 0.03306 0.04831 0.06268 0.00709 0.00027 0.00029 0.00019 0.00000 0.00169 0.00240 0.00130 0.00144 0.00125 0.00166 0.00080 N1 0.83125 0.41633 0.89319 1.00000 0.01898 0.01455 0.02565 0.00432 0.00930 0.00495 0.01930 0.00563 0.00024 0.00022 0.00020 0.00000 0.00117 0.00122 0.00129 0.00099 0.00101 0.00093 0.00050 N2 0.94167 0.57380 0.86292 1.00000 0.02060 0.01852 0.02213 0.00434 0.00854 0.00560 0.02009 0.00565 0.00024 0.00022 0.00019 0.00000 0.00121 0.00128 0.00126 0.00100 0.00101 0.00097 0.00051 N3 0.85335 0.73013 0.97945 1.00000 0.01897 0.01690 0.02352 0.00495 0.01047 0.00643 0.01873 0.00566 0.00024 0.00022 0.00019 0.00000 0.00116 0.00125 0.00126 0.00098 0.00099 0.00094 0.00050 N4 0.79504 0.79778 1.03459 1.00000 0.02464 0.01497 0.02039 0.00301 0.01126 0.00725 0.01893 0.00564 0.00025 0.00022 0.00019 0.00000 0.00125 0.00123 0.00123 0.00096 0.00102 0.00097 0.00050 N5 0.67727 0.97856 1.12001 1.00000 0.01905 0.01684 0.02329 0.00285 0.01015 0.00281 0.01927 0.00556 0.00024 0.00022 0.00019 0.00000 0.00118 0.00125 0.00125 0.00099 0.00099 0.00095 0.00050 N6 0.84527 1.11267 1.12677 1.00000 0.01745 0.01662 0.02117 0.00436 0.00919 0.00578 0.01758 0.00547 0.00023 0.00022 0.00019 0.00000 0.00114 0.00122 0.00121 0.00096 0.00096 0.00092 0.00048 N7 0.33276 0.50485 0.38911 1.00000 0.02100 0.02029 0.02357 0.00216 0.01145 0.00462 0.02086 0.00571 0.00024 0.00023 0.00020 0.00000 0.00123 0.00132 0.00128 0.00102 0.00104 0.00099 0.00052 N8 0.24266 0.63335 0.45895 1.00000 0.02401 0.01701 0.02484 0.00170 0.01349 0.00382 0.02094 0.00575 0.00025 0.00022 0.00020 0.00000 0.00126 0.00127 0.00130 0.00101 0.00106 0.00099 0.00052 N9 0.12584 0.31636 0.39130 1.00000 0.02203 0.01938 0.02469 0.00474 0.01183 0.00389 0.02115 0.00586 0.00025 0.00023 0.00020 0.00000 0.00124 0.00131 0.00129 0.00103 0.00104 0.00099 0.00052 N10 0.02450 0.24129 0.40487 1.00000 0.01681 0.02254 0.01992 0.00542 0.00836 0.00170 0.01944 0.00556 0.00023 0.00023 0.00019 0.00000 0.00114 0.00133 0.00120 0.00100 0.00096 0.00096 0.00050 N11 -0.09518 -0.07843 0.34964 1.00000 0.01923 0.01364 0.02191 0.00195 0.00833 0.00446 0.01812 0.00547 0.00024 0.00021 0.00019 0.00000 0.00116 0.00119 0.00123 0.00095 0.00098 0.00092 0.00049 N12 -0.16794 0.06719 0.41975 1.00000 0.01949 0.01884 0.02373 0.00304 0.00844 0.00484 0.02061 0.00566 0.00024 0.00023 0.00020 0.00000 0.00119 0.00130 0.00128 0.00101 0.00101 0.00097 0.00051 O1 0.81464 0.43981 0.30686 1.00000 0.03314 0.03940 0.03592 0.00385 0.00718 0.01971 0.03699 0.00582 0.00024 0.00024 0.00020 0.00000 0.00131 0.00150 0.00137 0.00113 0.00108 0.00113 0.00059 O2 0.75999 0.60706 0.21830 1.00000 0.04679 0.02810 0.06473 0.01161 0.03361 0.00452 0.04296 0.00664 0.00028 0.00023 0.00024 0.00000 0.00156 0.00140 0.00186 0.00128 0.00143 0.00116 0.00066 O3 0.66934 0.56524 0.34819 1.00000 0.03492 0.03218 0.03036 -0.00285 0.01449 0.00922 0.03237 0.00544 0.00024 0.00022 0.00018 0.00000 0.00129 0.00135 0.00124 0.00102 0.00104 0.00104 0.00054 O4 0.21978 0.12080 0.22357 1.00000 0.03662 0.02946 0.04325 0.00041 0.00722 0.01894 0.03818 0.00581 0.00025 0.00023 0.00021 0.00000 0.00135 0.00138 0.00149 0.00112 0.00114 0.00109 0.00061 O5 0.16474 -0.09034 0.15885 1.00000 0.02583 0.02453 0.04627 0.00043 0.00966 0.00151 0.03428 0.00537 0.00023 0.00022 0.00020 0.00000 0.00117 0.00126 0.00149 0.00108 0.00108 0.00095 0.00056 O6 0.35183 0.02698 0.14118 1.00000 0.02791 0.06247 0.03241 0.01891 0.01876 0.01419 0.03741 0.00617 0.00024 0.00026 0.00019 0.00000 0.00123 0.00184 0.00131 0.00125 0.00106 0.00119 0.00061 S1 0.72188 0.51946 0.27406 1.00000 0.01809 0.01959 0.03063 -0.00266 0.00846 0.00436 0.02357 0.00171 0.00007 0.00007 0.00006 0.00000 0.00034 0.00038 0.00040 0.00031 0.00030 0.00028 0.00017 S2 0.26617 0.01509 0.19715 1.00000 0.01690 0.01879 0.02286 0.00226 0.00778 0.00537 0.01942 0.00163 0.00007 0.00007 0.00006 0.00000 0.00033 0.00037 0.00036 0.00028 0.00028 0.00027 0.00015 Final Structure Factor Calculation for 2008sjc0013 in P-1 Total number of l.s. parameters = 451 Maximum vector length = 511 Memory required = 4573 / 26061 wR2 = 0.0878 before cycle 6 for 7338 data and 0 / 451 parameters GooF = S = 1.060; Restrained GooF = 1.060 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0362 * P )^2 + 2.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0352 for 6364 Fo > 4sig(Fo) and 0.0434 for all 7338 data wR2 = 0.0878, GooF = S = 1.060, Restrained GooF = 1.060 for all data Occupancy sum of asymmetric unit = 50.00 for non-hydrogen and 24.00 for hydrogen atoms Principal mean square atomic displacements U 0.0239 0.0160 0.0134 C1 0.0460 0.0229 0.0162 C2 0.0277 0.0209 0.0149 C3 0.0259 0.0225 0.0145 C4 0.0235 0.0176 0.0134 C5 0.0214 0.0178 0.0132 C6 0.0203 0.0156 0.0148 C7 0.0408 0.0248 0.0148 C8 0.0266 0.0230 0.0124 C9 0.0241 0.0212 0.0132 C10 0.0212 0.0189 0.0157 C11 0.0359 0.0298 0.0137 C12 0.0323 0.0248 0.0160 C13 0.0350 0.0265 0.0172 C14 0.0229 0.0199 0.0138 C15 0.0205 0.0180 0.0145 C16 0.0219 0.0183 0.0157 C17 0.0312 0.0251 0.0145 C18 0.0256 0.0221 0.0174 C19 0.0254 0.0219 0.0175 C20 0.0552 0.0344 0.0212 C21 0.0410 0.0275 0.0234 C22 0.0297 0.0240 0.0137 Ag1 0.0331 0.0183 0.0155 Ag2 0.1317 0.0446 0.0206 F1 0.1078 0.0385 0.0232 F2 0.0701 0.0496 0.0226 F3 0.0592 0.0432 0.0180 F4 0.1002 0.0462 0.0212 F5 0.1219 0.0422 0.0239 F6 0.0257 0.0187 0.0134 N1 0.0222 0.0212 0.0168 N2 0.0240 0.0185 0.0137 N3 0.0255 0.0190 0.0123 N4 0.0238 0.0173 0.0167 N5 0.0216 0.0177 0.0135 N6 0.0252 0.0211 0.0163 N7 0.0280 0.0192 0.0156 N8 0.0256 0.0196 0.0182 N9 0.0242 0.0196 0.0146 N10 0.0224 0.0193 0.0127 N11 0.0242 0.0203 0.0173 N12 0.0562 0.0349 0.0199 O1 0.0675 0.0370 0.0244 O2 0.0423 0.0350 0.0198 O3 0.0623 0.0357 0.0165 O4 0.0517 0.0289 0.0223 O5 0.0644 0.0296 0.0182 O6 0.0365 0.0189 0.0153 S1 0.0241 0.0196 0.0146 S2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.021 0.042 0.063 0.086 0.113 0.144 0.179 0.222 0.304 1.000 Number in group 756. 729. 717. 744. 727. 738. 727. 737. 724. 739. GooF 1.004 1.050 1.141 1.112 1.048 1.030 1.018 0.928 1.029 1.220 K 1.846 1.000 0.987 0.961 0.978 0.989 1.003 1.010 1.017 0.997 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.64 inf Number in group 751. 758. 717. 721. 726. 732. 739. 723. 733. 738. GooF 1.028 0.966 0.990 0.988 0.942 0.868 0.868 1.003 1.161 1.596 K 0.977 0.999 0.993 1.002 1.015 1.019 1.023 1.027 1.014 0.976 R1 0.095 0.074 0.068 0.056 0.044 0.034 0.028 0.029 0.027 0.034 Recommended weighting scheme: WGHT 0.0356 2.7481 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) -3 4 2 277.86 122.67 6.09 0.053 2.33 1 -1 1 7164.08 10557.73 4.58 0.494 6.40 -3 -2 6 312.23 484.02 4.40 0.106 2.13 1 2 1 757.31 1051.36 4.32 0.156 3.92 3 1 0 4212.53 5211.91 4.28 0.347 3.05 -13 -3 3 -138.64 276.75 4.24 0.080 0.77 -6 -2 5 1497.89 1132.90 4.22 0.162 1.63 -2 -7 3 2730.18 2155.91 4.15 0.223 1.50 -11 -4 1 428.64 632.02 4.13 0.121 0.84 -1 -10 14 -89.36 169.61 4.06 0.063 0.79 -2 6 2 1136.47 859.42 3.97 0.141 1.78 -5 -3 4 71.93 25.95 3.82 0.024 1.78 1 3 2 3204.03 4034.92 3.78 0.305 2.65 0 2 3 2696.56 3312.73 3.73 0.277 3.15 -4 -3 4 288.15 425.30 3.70 0.099 2.04 1 -2 8 1175.42 905.61 3.69 0.145 1.52 5 1 0 1371.05 1715.00 3.68 0.199 1.91 -4 3 6 188.75 300.68 3.60 0.083 1.80 -8 4 1 239.20 146.54 3.60 0.058 1.26 0 -2 1 300.82 183.65 3.60 0.065 5.50 3 6 0 399.25 266.15 3.59 0.078 1.52 -3 -1 1 2564.04 3108.24 3.56 0.268 3.28 2 -9 14 325.49 558.69 3.55 0.114 0.77 -2 -1 2 10122.03 12091.53 3.53 0.529 4.49 -1 -6 8 32.99 1.45 3.48 0.006 1.36 -5 -10 14 -40.24 61.49 3.44 0.038 0.78 -2 6 4 700.61 511.55 3.41 0.109 1.60 2 2 1 3762.94 4491.84 3.40 0.322 3.05 -3 -3 4 5235.15 6188.79 3.35 0.378 2.32 -1 -2 3 9349.05 10911.65 3.31 0.502 3.77 -5 -2 12 31.54 0.91 3.31 0.005 1.14 -8 5 3 674.21 512.17 3.29 0.109 1.24 -1 3 3 1107.20 874.05 3.28 0.142 2.78 1 -1 4 2890.26 2421.04 3.28 0.236 2.81 -1 4 6 862.12 1091.68 3.27 0.159 1.66 -5 -2 6 8475.57 9844.61 3.25 0.477 1.76 -5 -9 6 142.63 235.36 3.24 0.074 1.03 3 -6 4 401.16 275.35 3.23 0.080 1.53 -3 -4 7 381.82 273.89 3.23 0.080 1.67 1 0 5 162.93 93.50 3.21 0.046 2.28 -12 -3 12 97.25 226.59 3.20 0.072 0.81 -4 0 2 3080.13 3851.07 3.19 0.298 2.72 -3 -3 6 212.18 309.24 3.15 0.085 1.97 3 -2 6 11031.33 9598.20 3.15 0.471 1.58 2 2 3 4716.47 5553.25 3.14 0.358 2.29 11 -2 3 79.86 191.95 3.11 0.067 0.84 -4 0 8 94.64 47.36 3.09 0.033 1.68 -12 3 4 676.53 1156.99 3.03 0.163 0.90 4 1 0 314.03 424.93 2.99 0.099 2.35 -6 3 4 727.13 573.94 2.99 0.115 1.68 Bond lengths and angles C1 - Distance Angles N2 1.3321 (0.0038) N1 1.3550 (0.0037) 111.11 (0.26) C5 1.4511 (0.0040) 123.45 (0.27) 125.42 (0.26) C1 - N2 N1 C2 - Distance Angles N1 1.4659 (0.0039) 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 1.3660 (0.0039) C4 1.3792 (0.0043) 106.14 (0.26) H3 0.9500 126.93 126.93 C3 - N1 C4 C4 - Distance Angles N2 1.3629 (0.0039) C3 1.3792 (0.0043) 109.59 (0.27) H4 0.9500 125.21 125.21 C4 - N2 C3 C5 - Distance Angles N3 1.2867 (0.0038) C1 1.4511 (0.0040) 118.08 (0.26) H5 0.9500 120.96 120.96 C5 - N3 C1 C6 - Distance Angles N4 1.2874 (0.0038) C7 1.4438 (0.0039) 121.82 (0.27) H6 0.9500 119.09 119.09 C6 - N4 C7 C7 - Distance Angles N6 1.3342 (0.0038) N5 1.3578 (0.0037) 110.38 (0.25) C6 1.4438 (0.0039) 122.66 (0.26) 126.89 (0.27) C7 - N6 N5 C8 - Distance Angles N5 1.4721 (0.0038) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - N5 H8A H8B C9 - Distance Angles N5 1.3637 (0.0038) C10 1.3646 (0.0043) 106.78 (0.25) H9 0.9500 126.61 126.61 C9 - N5 C10 C10 - Distance Angles C9 1.3646 (0.0043) N6 1.3784 (0.0037) 109.14 (0.26) H10 0.9500 125.43 125.43 C10 - C9 N6 C11 - Distance Angles N8 1.3376 (0.0038) N7 1.3540 (0.0037) 110.25 (0.25) C15 1.4419 (0.0041) 122.33 (0.26) 127.42 (0.27) C11 - N8 N7 C12 - Distance Angles N7 1.4707 (0.0038) H12A 0.9800 109.47 H12B 0.9800 109.47 109.47 H12C 0.9800 109.47 109.47 109.47 C12 - N7 H12A H12B C13 - Distance Angles C14 1.3606 (0.0046) N7 1.3665 (0.0040) 106.40 (0.27) H13 0.9500 126.80 126.80 C13 - C14 N7 C14 - Distance Angles C13 1.3606 (0.0046) N8 1.3676 (0.0040) 109.73 (0.28) H14 0.9500 125.13 125.13 C14 - C13 N8 C15 - Distance Angles N9 1.2802 (0.0039) C11 1.4419 (0.0041) 121.77 (0.27) H15 0.9500 119.11 119.11 C15 - N9 C11 C16 - Distance Angles N10 1.2992 (0.0039) C17 1.4448 (0.0040) 118.35 (0.26) H16 0.9500 120.82 120.82 C16 - N10 C17 C17 - Distance Angles N12 1.3334 (0.0038) N11 1.3609 (0.0038) 111.35 (0.25) C16 1.4448 (0.0040) 123.55 (0.27) 125.08 (0.26) C17 - N12 N11 C18 - Distance Angles N11 1.4652 (0.0037) H18A 0.9800 109.47 H18B 0.9800 109.47 109.47 H18C 0.9800 109.47 109.47 109.47 C18 - N11 H18A H18B C19 - Distance Angles C20 1.3701 (0.0043) N11 1.3705 (0.0039) 105.97 (0.27) H19 0.9500 127.01 127.01 C19 - C20 N11 C20 - Distance Angles N12 1.3639 (0.0039) C19 1.3701 (0.0043) 110.50 (0.26) H20 0.9500 124.75 124.75 C20 - N12 C19 C21 - Distance Angles F1 1.3152 (0.0042) F3 1.3353 (0.0042) 108.83 (0.33) F2 1.3404 (0.0048) 106.75 (0.33) 107.30 (0.30) S1 1.8230 (0.0038) 110.99 (0.26) 111.56 (0.26) 111.22 (0.28) C21 - F1 F3 F2 C22 - Distance Angles F5 1.3323 (0.0043) F6 1.3384 (0.0040) 108.37 (0.31) F4 1.3457 (0.0040) 107.04 (0.27) 106.12 (0.29) S2 1.8063 (0.0034) 112.00 (0.25) 111.70 (0.23) 111.31 (0.24) C22 - F5 F6 F4 Ag1 - Distance Angles N8 2.1520 (0.0025) N10_$1 2.2315 (0.0024) 165.25 (0.10) N12_$1 2.4556 (0.0026) 119.28 (0.09) 73.16 (0.09) Ag1 - N8 N10_$1 Ag2 - Distance Angles N6_$4 2.1697 (0.0024) N3_$3 2.2843 (0.0024) 158.08 (0.09) N2_$3 2.4176 (0.0025) 120.81 (0.09) 72.77 (0.09) Ag2 - N6_$4 N3_$3 F1 - Distance Angles C21 1.3152 (0.0042) F1 - F2 - Distance Angles C21 1.3404 (0.0048) F2 - F3 - Distance Angles C21 1.3353 (0.0042) F3 - F4 - Distance Angles C22 1.3457 (0.0040) F4 - F5 - Distance Angles C22 1.3323 (0.0043) F5 - F6 - Distance Angles C22 1.3384 (0.0041) F6 - N1 - Distance Angles C1 1.3550 (0.0037) C3 1.3660 (0.0039) 107.24 (0.25) C2 1.4659 (0.0039) 127.87 (0.26) 124.88 (0.26) N1 - C1 C3 N2 - Distance Angles C1 1.3321 (0.0038) C4 1.3629 (0.0039) 105.92 (0.25) Ag2_$3 2.4176 (0.0025) 108.45 (0.19) 145.59 (0.21) N2 - C1 C4 N3 - Distance Angles C5 1.2867 (0.0038) N4 1.4030 (0.0033) 112.40 (0.24) Ag2_$3 2.2844 (0.0024) 117.25 (0.20) 130.21 (0.18) N3 - C5 N4 N4 - Distance Angles C6 1.2874 (0.0038) N3 1.4030 (0.0034) 112.10 (0.24) N4 - C6 N5 - Distance Angles C7 1.3578 (0.0037) C9 1.3637 (0.0038) 107.59 (0.24) C8 1.4721 (0.0038) 127.71 (0.25) 124.62 (0.25) N5 - C7 C9 N6 - Distance Angles C7 1.3342 (0.0038) C10 1.3784 (0.0037) 106.11 (0.24) Ag2_$2 2.1697 (0.0024) 131.22 (0.19) 122.39 (0.20) N6 - C7 C10 N7 - Distance Angles C11 1.3540 (0.0037) C13 1.3665 (0.0040) 107.62 (0.25) C12 1.4707 (0.0038) 128.09 (0.26) 124.29 (0.25) N7 - C11 C13 N8 - Distance Angles C11 1.3376 (0.0038) C14 1.3676 (0.0040) 105.99 (0.25) Ag1 2.1520 (0.0024) 129.44 (0.20) 124.37 (0.21) N8 - C11 C14 N9 - Distance Angles C15 1.2802 (0.0039) N10 1.4008 (0.0034) 112.39 (0.25) N9 - C15 N10 - Distance Angles C16 1.2992 (0.0039) N9 1.4008 (0.0034) 111.65 (0.24) Ag1_$1 2.2315 (0.0024) 118.02 (0.19) 130.22 (0.19) N10 - C16 N9 N11 - Distance Angles C17 1.3609 (0.0038) C19 1.3705 (0.0039) 106.92 (0.24) C18 1.4652 (0.0037) 127.72 (0.25) 125.25 (0.25) N11 - C17 C19 N12 - Distance Angles C17 1.3334 (0.0038) C20 1.3639 (0.0039) 105.25 (0.25) Ag1_$1 2.4556 (0.0025) 106.78 (0.19) 147.84 (0.20) N12 - C17 C20 O1 - Distance Angles S1 1.4376 (0.0024) O1 - O2 - Distance Angles S1 1.4528 (0.0027) O2 - O3 - Distance Angles S1 1.4451 (0.0024) O3 - O4 - Distance Angles S2 1.4370 (0.0024) O4 - O5 - Distance Angles S2 1.4348 (0.0024) O5 - O6 - Distance Angles S2 1.4335 (0.0024) O6 - S1 - Distance Angles O1 1.4376 (0.0024) O3 1.4451 (0.0024) 116.78 (0.15) O2 1.4528 (0.0027) 113.90 (0.16) 114.76 (0.16) C21 1.8230 (0.0038) 103.72 (0.16) 103.22 (0.16) 101.79 (0.19) S1 - O1 O3 O2 S2 - Distance Angles O6 1.4335 (0.0024) O5 1.4348 (0.0024) 114.63 (0.16) O4 1.4370 (0.0024) 116.36 (0.17) 113.90 (0.15) C22 1.8063 (0.0034) 102.43 (0.15) 104.02 (0.16) 103.10 (0.16) S2 - O6 O5 O4 FMAP and GRID set by program FMAP 2 3 37 GRID -1.471 -2 -2 1.471 2 2 R1 = 0.0428 for 7338 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.73 at 0.6960 0.3830 0.3078 [ 1.38 A from O1 ] Deepest hole -0.87 at 0.7960 0.3051 0.4278 [ 0.84 A from AG1 ] Mean = 0.00, Rms deviation from mean = 0.11 e/A^3, Highest memory used = 4284 / 33069 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.6960 0.3830 0.3078 1.00000 0.05 0.73 1.38 O1 1.71 S1 1.80 F2 2.04 C21 Q2 1 0.6788 0.4463 0.1080 1.00000 0.05 0.73 0.94 F3 1.69 C21 2.13 O2 2.24 S1 Q3 1 0.8639 0.5602 0.3171 1.00000 0.05 0.70 1.39 O1 1.44 S1 1.63 O2 2.19 H4 Q4 1 0.7045 0.4786 0.3100 1.00000 0.05 0.68 0.78 S1 1.25 O3 1.35 O1 1.91 C21 Q5 1 0.6135 0.5962 0.1383 1.00000 0.05 0.66 1.56 O2 1.90 F1 2.10 C21 2.19 S1 Q6 1 0.0015 0.3029 0.4127 1.00000 0.05 0.57 0.79 N10 1.49 N9 1.69 H15 1.83 AG1 Q7 1 0.0374 -0.0858 0.2819 1.00000 0.05 0.56 0.64 H18C 0.99 C18 1.19 H18B 1.83 H18A Q8 1 0.6193 0.4991 0.1680 1.00000 0.05 0.54 0.94 C21 1.47 S1 1.47 F1 1.54 F3 Q9 1 0.4840 0.3827 0.1598 1.00000 0.05 0.53 1.01 C21 1.01 F2 1.20 F1 1.91 F3 Q10 1 0.1935 0.7845 0.5481 1.00000 0.05 0.51 0.94 AG1 1.80 N12 2.26 N8 2.69 N10 Shortest distances between peaks (including symmetry equivalents) 1 4 1.09 5 8 1.23 2 8 1.38 8 9 1.83 3 4 1.84 4 8 1.92 2 5 2.01 1 8 2.45 1 9 2.48 6 10 2.52 1 3 2.52 2 9 2.55 4 9 2.55 3 8 2.66 2 4 2.72 5 9 2.78 4 5 2.81 2 3 2.91 1 2 2.92 1 10 2.99 Time profile in seconds ----------------------- 0.13: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: Generate connectivity array 0.02: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.02: Analyse other restraints etc. 6.45: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 2.59: Structure factors and derivatives 8.75: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.06: Apply other restraints 1.23: Solve l.s. equations 0.00: Generate HTAB table 0.06: Other dependent quantities, CIF, tables 0.08: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.13: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008sjc0013 finished at 13:46:50 Total CPU time: 19.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++