+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 15:42:13 on 09-Oct-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 03src0400 in P2(1)2(1)2(1) CELL 0.71073 8.5458 9.3820 38.2811 90.000 90.000 90.000 ZERR 4.00 0.0004 0.0005 0.0020 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N F P UNIT 108 156 8 24 4 V = 3069.25 F(000) = 1136.0 Mu = 0.14 mm-1 Cell Wt = 2146.29 Rho = 1.161 MERG 2 OMIT -3.00 55.00 FMAP 2 PLAN 10 SIZE 0.08 0.35 0.60 ACTA BOND $H WGHT 0.17630 L.S. 10 TEMP -153.00 FVAR 0.56967 C17 1 0.957857 0.636156 0.610925 11.00000 0.27028 0.32043 = 0.10231 -0.01461 -0.00600 -0.04071 AFIX 137 H17A 2 1.070226 0.652116 0.614212 11.00000 -1.50000 H17B 2 0.919770 0.569663 0.628744 11.00000 -1.50000 H17C 2 0.902037 0.726978 0.613076 11.00000 -1.50000 AFIX 0 C19 1 0.452937 0.339827 0.338453 11.00000 0.39449 0.18681 = 0.10806 0.00251 0.02630 -0.20132 AFIX 43 H19 2 0.402309 0.249875 0.339906 11.00000 -1.20000 AFIX 0 C20 1 0.460523 0.398073 0.366481 11.00000 0.43462 0.15603 = 0.12714 -0.03577 0.11122 -0.16714 AFIX 43 H20 2 0.512443 0.487458 0.365212 11.00000 -1.20000 AFIX 0 C21 1 0.408820 0.364089 0.402105 11.00000 0.29312 0.30631 = 0.09613 0.04033 0.02397 -0.12668 AFIX 43 H21 2 0.319084 0.304442 0.403033 11.00000 -1.20000 AFIX 0 C22 1 0.461767 0.399617 0.432121 11.00000 0.30085 0.19630 = 0.12201 -0.01637 0.07006 -0.11211 AFIX 43 H22 2 0.553088 0.457334 0.431724 11.00000 -1.20000 AFIX 0 C23 1 0.404955 0.365985 0.465728 11.00000 0.17920 0.25987 = 0.12131 0.01321 0.01675 -0.06068 AFIX 43 H23 2 0.303950 0.323766 0.466336 11.00000 -1.20000 AFIX 0 C24 1 0.471870 0.384727 0.496384 11.00000 0.26781 0.22925 = 0.13872 -0.03714 0.03551 -0.08689 AFIX 43 H24 2 0.572218 0.428292 0.496213 11.00000 -1.20000 AFIX 0 C25 1 0.410024 0.346575 0.530220 11.00000 0.21438 0.28482 = 0.10222 -0.00480 0.00212 -0.04370 AFIX 43 H25 2 0.308746 0.304871 0.529756 11.00000 -1.20000 AFIX 0 C26 1 0.474013 0.360826 0.563058 11.00000 0.35123 0.24078 = 0.22800 -0.03652 0.04663 -0.06444 AFIX 43 H26 2 0.577482 0.397762 0.563673 11.00000 -1.20000 AFIX 0 C27 1 0.410409 0.329621 0.594794 11.00000 0.28622 0.30229 = 0.11891 0.01154 -0.01977 -0.04589 AFIX 137 H27A 2 0.409618 0.415516 0.609360 11.00000 -1.50000 H27B 2 0.472878 0.255478 0.606226 11.00000 -1.50000 H27C 2 0.302989 0.295427 0.591617 11.00000 -1.50000 AFIX 0 F5 4 0.058960 0.779239 0.231754 11.00000 0.21725 0.18118 = 0.12967 -0.00269 -0.04728 -0.08449 F6 4 -0.112094 0.595894 0.178425 11.00000 0.31693 0.21760 = 0.14492 -0.06094 0.03426 -0.17028 C1 1 0.740195 0.521312 0.307038 11.00000 0.06570 0.07423 = 0.08971 0.00361 0.01982 0.00977 AFIX 43 H1 2 0.810102 0.444321 0.311072 11.00000 -1.20000 AFIX 0 C2 1 0.647494 0.737484 0.299808 11.00000 0.05878 0.07168 = 0.06358 -0.00061 0.00961 -0.00305 C3 1 0.626048 0.883936 0.296341 11.00000 0.08538 0.06399 = 0.08054 -0.00160 -0.00272 -0.01010 AFIX 43 H3 2 0.710042 0.949360 0.299018 11.00000 -1.20000 AFIX 0 C4 1 0.476776 0.928518 0.288838 11.00000 0.08075 0.06443 = 0.09634 0.00741 0.00141 0.00912 AFIX 43 H4 2 0.456834 1.027499 0.286090 11.00000 -1.20000 AFIX 0 C5 1 0.353600 0.832010 0.285150 11.00000 0.06736 0.09455 = 0.09453 -0.00632 -0.00452 0.02352 AFIX 43 H5 2 0.251461 0.867354 0.280576 11.00000 -1.20000 AFIX 0 C6 1 0.375133 0.690990 0.287870 11.00000 0.04977 0.10257 = 0.08092 -0.01016 0.00361 -0.00352 AFIX 43 H6 2 0.291744 0.625606 0.284329 11.00000 -1.20000 AFIX 0 C7 1 0.527432 0.644176 0.296236 11.00000 0.06584 0.06385 = 0.06272 -0.00228 0.00587 0.00239 C8 1 0.938944 0.711076 0.313783 11.00000 0.04979 0.11433 = 0.09604 0.01349 -0.00047 -0.01378 AFIX 23 H8A 2 0.961089 0.791330 0.297736 11.00000 -1.20000 H8B 2 1.015824 0.634755 0.308845 11.00000 -1.20000 AFIX 0 C9 1 0.960037 0.760086 0.350095 11.00000 0.08276 0.15636 = 0.11351 0.01842 -0.01691 -0.04848 AFIX 23 H9A 2 0.890916 0.843503 0.353666 11.00000 -1.20000 H9B 2 1.069139 0.794175 0.352506 11.00000 -1.20000 AFIX 0 C10 1 0.929758 0.658040 0.378895 11.00000 0.10090 0.11903 = 0.09905 0.01484 -0.01505 -0.01605 AFIX 23 H10A 2 0.818895 0.627852 0.377642 11.00000 -1.20000 H10B 2 0.995081 0.572316 0.375053 11.00000 -1.20000 AFIX 0 C11 1 0.960842 0.712314 0.414394 11.00000 0.14715 0.16760 = 0.09622 0.01144 -0.02010 -0.04418 AFIX 23 H11A 2 0.898354 0.800229 0.417552 11.00000 -1.20000 H11B 2 1.072428 0.740334 0.415456 11.00000 -1.20000 AFIX 0 C12 1 0.929116 0.618218 0.444589 11.00000 0.14988 0.17172 = 0.09881 0.01590 -0.03336 -0.00959 AFIX 23 H12A 2 0.817966 0.588881 0.443393 11.00000 -1.20000 H12B 2 0.993060 0.531006 0.441729 11.00000 -1.20000 AFIX 0 C13 1 0.958616 0.675240 0.480151 11.00000 0.16930 0.16558 = 0.10684 0.00435 -0.02389 -0.03540 AFIX 23 H13A 2 1.069978 0.704194 0.480796 11.00000 -1.20000 H13B 2 0.896319 0.763797 0.482235 11.00000 -1.20000 AFIX 0 C14 1 0.930831 0.595691 0.510960 11.00000 0.17468 0.17192 = 0.10474 0.01753 -0.02127 -0.01359 AFIX 23 H14A 2 0.991960 0.506530 0.508703 11.00000 -1.20000 H14B 2 0.819111 0.567856 0.510446 11.00000 -1.20000 AFIX 0 C15 1 0.961156 0.650192 0.545659 11.00000 0.18841 0.18143 = 0.10176 -0.01076 -0.01898 -0.01741 AFIX 23 H15A 2 1.073790 0.674695 0.546377 11.00000 -1.20000 H15B 2 0.903298 0.741294 0.547519 11.00000 -1.20000 AFIX 0 C16 1 0.930072 0.575527 0.575927 11.00000 0.22588 0.25076 = 0.10270 0.00502 -0.00671 -0.03198 AFIX 23 H16A 2 0.991060 0.485966 0.574641 11.00000 -1.20000 H16B 2 0.818274 0.548129 0.575008 11.00000 -1.20000 AFIX 0 C18 1 0.502006 0.372913 0.302913 11.00000 0.10869 0.07507 = 0.09457 -0.01074 0.00290 -0.02459 AFIX 23 H18A 2 0.408541 0.378823 0.287702 11.00000 -1.20000 H18B 2 0.569116 0.294863 0.294056 11.00000 -1.20000 AFIX 0 N1 3 0.780518 0.656707 0.306654 11.00000 0.04623 0.08466 = 0.07714 0.00044 0.00783 0.00029 N2 3 0.588435 0.507657 0.301007 11.00000 0.07444 0.07030 = 0.07189 -0.00757 0.00605 -0.00488 F1 4 -0.001427 0.553778 0.227555 11.00000 0.17092 0.12797 = 0.28700 0.10119 0.00348 0.01121 F2 4 0.129410 0.674111 0.185476 11.00000 0.12533 0.20860 = 0.21258 0.02246 0.07022 0.03190 F3 4 -0.054071 0.820334 0.181532 11.00000 0.15969 0.13192 = 0.18567 0.08118 -0.03324 -0.01463 F4 4 -0.188937 0.699271 0.224510 11.00000 0.08977 0.19730 = 0.15348 0.01488 0.02362 0.02554 P1 5 -0.030234 0.687550 0.205076 11.00000 0.06893 0.06331 = 0.09369 -0.00220 0.00410 -0.00578 HKLF 4 Covalent radii and connectivity table for 03src0400 in P2(1)2(1)2(1) C 0.770 H 0.320 N 0.700 F 0.640 P 1.100 C17 - C16 C19 - C20 C18 C20 - C19 C21 C21 - C22 C20 C22 - C21 C23 C23 - C24 C22 C24 - C23 C25 C25 - C26 C24 C26 - C27 C25 C27 - C26 F5 - P1 F6 - P1 C1 - N1 N2 C2 - C7 N1 C3 C3 - C4 C2 C4 - C3 C5 C5 - C6 C4 C6 - C5 C7 C7 - C2 N2 C6 C8 - N1 C9 C9 - C8 C10 C10 - C11 C9 C11 - C10 C12 C12 - C11 C13 C13 - C14 C12 C14 - C13 C15 C15 - C16 C14 C16 - C15 C17 C18 - C19 N2 N1 - C1 C2 C8 N2 - C1 C7 C18 F1 - P1 F2 - P1 F3 - P1 F4 - P1 P1 - F6 F5 F1 F4 F3 F2 16721 Reflections read, of which 48 rejected -10 =< h =< 10, -11 =< k =< 11, -49 =< l =< 49, Max. 2-theta = 54.94 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 1 1 0 587.06 7.99 6 40.24 1 1 1 1494.34 27.75 3 155.69 -5 2 1 143.42 3.03 4 15.27 5 2 1 149.76 3.33 4 20.00 -1 1 3 1429.19 15.13 5 160.52 -3 2 3 122.43 1.46 5 18.82 2 0 4 77.78 1.32 5 8.02 0 1 4 65.55 1.05 6 5.77 2 0 5 1043.52 12.50 5 111.60 6 2 6 104.26 2.59 4 13.32 7 5 6 10.95 2.11 2 13.04 6 2 7 91.20 2.34 4 13.42 -1 3 8 95.36 0.85 6 9.55 -1 4 13 195.28 3.21 5 18.46 2 4 16 48.19 1.20 6 6.95 4 6 22 7.99 1.47 3 7.66 1 8 28 12.69 1.84 2 25.29 1 8 29 24.21 2.25 3 14.93 7 0 30 22.62 3.09 2 24.58 0 4 32 9.16 1.42 3 20.10 2 7 32 38.69 1.97 2 49.31 2 1 35 5.76 1.25 4 10.18 22 Inconsistent equivalents 6241 Unique reflections, of which 0 suppressed R(int) = 0.0811 R(sigma) = 0.0822 Friedel opposites not merged Maximum memory for data reduction = 3583 / 62329 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 = 4576 / 412493 wR2 = 0.2897 before cycle 1 for 6241 data and 327 / 327 parameters GooF = S = 1.047; Restrained GooF = 1.047 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1763 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.56958 0.00281 -0.030 OSF Mean shift/su = 0.024 Maximum = -0.096 for U22 C26 Max. shift = 0.006 A for H27C Max. dU = 0.000 for C25 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4576 / 412493 wR2 = 0.2897 before cycle 2 for 6241 data and 327 / 327 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1763 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.56960 0.00281 0.005 OSF Mean shift/su = 0.009 Maximum = 0.049 for U12 C26 Max. shift = 0.001 A for H17C Max. dU = 0.000 for C26 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4576 / 412493 wR2 = 0.2896 before cycle 3 for 6241 data and 327 / 327 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1763 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.56962 0.00281 0.009 OSF Mean shift/su = 0.003 Maximum = -0.019 for U33 F2 Max. shift = 0.001 A for H17C Max. dU = 0.000 for C26 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4576 / 412493 wR2 = 0.2897 before cycle 4 for 6241 data and 327 / 327 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1763 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.56962 0.00281 0.000 OSF Mean shift/su = 0.002 Maximum = -0.007 for y F2 Max. shift = 0.000 A for H17B Max. dU = 0.000 for C26 Least-squares cycle 5 Maximum vector length = 511 Memory required = 4576 / 412493 wR2 = 0.2897 before cycle 5 for 6241 data and 327 / 327 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1763 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.56962 0.00281 0.000 OSF Mean shift/su = 0.001 Maximum = -0.003 for U11 C26 Max. shift = 0.000 A for H27A Max. dU = 0.000 for C26 Least-squares cycle 6 Maximum vector length = 511 Memory required = 4576 / 412493 wR2 = 0.2897 before cycle 6 for 6241 data and 327 / 327 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1763 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.56962 0.00281 0.000 OSF Mean shift/su = 0.000 Maximum = 0.002 for U11 F1 Max. shift = 0.000 A for H17C Max. dU = 0.000 for C26 Least-squares cycle 7 Maximum vector length = 511 Memory required = 4576 / 412493 wR2 = 0.2897 before cycle 7 for 6241 data and 327 / 327 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1763 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.56962 0.00281 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for x C6 Max. shift = 0.000 A for H17C Max. dU = 0.000 for C26 Least-squares cycle 8 Maximum vector length = 511 Memory required = 4576 / 412493 wR2 = 0.2897 before cycle 8 for 6241 data and 327 / 327 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1763 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.56962 0.00281 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for x C6 Max. shift = 0.000 A for H17B Max. dU = 0.000 for C17 Least-squares cycle 9 Maximum vector length = 511 Memory required = 4576 / 412493 wR2 = 0.2897 before cycle 9 for 6241 data and 327 / 327 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1763 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.56962 0.00281 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for U11 F1 Max. shift = 0.000 A for H17C Max. dU = 0.000 for C16 Least-squares cycle 10 Maximum vector length = 511 Memory required = 4576 / 412493 wR2 = 0.2897 before cycle 10 for 6241 data and 327 / 327 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1763 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.56962 0.00281 0.000 OSF Mean shift/su = 0.000 Maximum = 0.000 for x C6 Max. shift = 0.000 A for H17C Max. dU = 0.000 for C17 Largest correlation matrix elements -0.736 U12 C19 / U11 C19 -0.616 y C19 / x C19 0.529 U23 F3 / U33 F3 -0.726 U12 C19 / U22 C19 -0.566 U13 C19 / U23 C19 0.520 U23 F1 / U22 F1 -0.696 U12 F6 / U11 F6 0.565 U23 F1 / U33 F1 -0.508 U12 C22 / U11 C22 -0.679 U12 C20 / U11 C20 0.557 U23 F3 / U22 F3 -0.505 U12 C22 / U22 C22 -0.674 U12 F6 / U22 F6 -0.548 U13 F6 / U23 F6 -0.642 U12 C20 / U22 C20 -0.543 y F6 / x F6 Idealized hydrogen atom generation before cycle 11 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H17A 1.0701 0.6521 0.6143 137 0.980 0.000 C17 C16 H17A H17B 0.9195 0.5697 0.6287 137 0.980 0.000 C17 C16 H17A H17C 0.9020 0.7270 0.6131 137 0.980 0.000 C17 C16 H17A H19 0.4024 0.2498 0.3399 43 0.950 0.000 C19 C20 C18 H20 0.5122 0.4875 0.3652 43 0.950 0.000 C20 C19 C21 H21 0.3195 0.3040 0.4031 43 0.950 0.000 C21 C22 C20 H22 0.5529 0.4576 0.4317 43 0.950 0.000 C22 C21 C23 H23 0.3040 0.3239 0.4663 43 0.950 0.000 C23 C24 C22 H24 0.5723 0.4282 0.4962 43 0.950 0.000 C24 C23 C25 H25 0.3087 0.3051 0.5297 43 0.950 0.000 C25 C26 C24 H26 0.5778 0.3973 0.5637 43 0.950 0.000 C26 C27 C25 H27A 0.4100 0.4154 0.6094 137 0.980 0.000 C27 C26 H27A H27B 0.4720 0.2550 0.6062 137 0.980 0.000 C27 C26 H27A H27C 0.3026 0.2962 0.5916 137 0.980 0.000 C27 C26 H27A H1 0.8101 0.4443 0.3111 43 0.950 0.000 C1 N1 N2 H3 0.7100 0.9494 0.2990 43 0.950 0.000 C3 C4 C2 H4 0.4569 1.0275 0.2861 43 0.950 0.000 C4 C3 C5 H5 0.2514 0.8673 0.2806 43 0.950 0.000 C5 C6 C4 H6 0.2918 0.6256 0.2843 43 0.950 0.000 C6 C5 C7 H8A 0.9611 0.7913 0.2977 23 0.990 0.000 C8 N1 C9 H8B 1.0158 0.6347 0.3089 23 0.990 0.000 C8 N1 C9 H9A 0.8910 0.8435 0.3537 23 0.990 0.000 C9 C8 C10 H9B 1.0692 0.7941 0.3525 23 0.990 0.000 C9 C8 C10 H10A 0.8189 0.6279 0.3776 23 0.990 0.000 C10 C11 C9 H10B 0.9950 0.5723 0.3751 23 0.990 0.000 C10 C11 C9 H11A 0.8984 0.8003 0.4175 23 0.990 0.000 C11 C10 C12 H11B 1.0724 0.7404 0.4155 23 0.990 0.000 C11 C10 C12 H12A 0.9929 0.5310 0.4417 23 0.990 0.000 C12 C11 C13 H12B 0.8179 0.5889 0.4434 23 0.990 0.000 C12 C11 C13 H13A 1.0700 0.7042 0.4808 23 0.990 0.000 C13 C14 C12 H13B 0.8963 0.7639 0.4822 23 0.990 0.000 C13 C14 C12 H14A 0.9918 0.5065 0.5087 23 0.990 0.000 C14 C13 C15 H14B 0.8191 0.5680 0.5105 23 0.990 0.000 C14 C13 C15 H15A 1.0739 0.6745 0.5464 23 0.990 0.000 C15 C16 C14 H15B 0.9035 0.7413 0.5475 23 0.990 0.000 C15 C16 C14 H16A 0.9912 0.4860 0.5746 23 0.990 0.000 C16 C15 C17 H16B 0.8184 0.5480 0.5750 23 0.990 0.000 C16 C15 C17 H18A 0.4085 0.3788 0.2877 23 0.990 0.000 C18 C19 N2 H18B 0.5691 0.2949 0.2940 23 0.990 0.000 C18 C19 N2 03src0400 in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C17 0.95776 0.63619 0.61093 1.00000 0.27026 0.32050 0.10232 -0.01523 -0.00587 -0.04077 0.23103 0.02159 0.00181 0.00161 0.00023 0.00000 0.01486 0.01616 0.00604 0.00796 0.00767 0.01449 0.00635 H17A 1.07011 0.65212 0.61425 1.00000 0.34654 0.00000 0.00000 H17B 0.91953 0.56974 0.62875 1.00000 0.34654 0.00000 0.00000 H17C 0.90197 0.72704 0.61306 1.00000 0.34654 0.00000 0.00000 C19 0.45297 0.33980 0.33844 1.00000 0.39625 0.18677 0.10760 0.00267 0.02644 -0.20172 0.23021 0.01544 0.00165 0.00107 0.00023 0.00000 0.01829 0.00910 0.00563 0.00578 0.00826 0.01125 0.00710 H19 0.40243 0.24981 0.33990 1.00000 0.27625 0.00000 0.00000 C20 0.46050 0.39804 0.36647 1.00000 0.43417 0.15561 0.12750 -0.03575 0.11164 -0.16695 0.23909 0.02054 0.00192 0.00101 0.00026 0.00000 0.02128 0.00758 0.00655 0.00571 0.00990 0.01114 0.00787 H20 0.51222 0.48753 0.36520 1.00000 0.28691 0.00000 0.00000 C21 0.40895 0.36393 0.40213 1.00000 0.29202 0.30633 0.09632 0.04050 0.02367 -0.12542 0.23156 0.02419 0.00186 0.00159 0.00026 0.00000 0.01546 0.01574 0.00556 0.00779 0.00788 0.01414 0.00690 H21 0.31947 0.30396 0.40306 1.00000 0.27787 0.00000 0.00000 C22 0.46171 0.39969 0.43213 1.00000 0.30028 0.19665 0.12141 -0.01645 0.06956 -0.11185 0.20611 0.02169 0.00184 0.00112 0.00027 0.00000 0.01631 0.00998 0.00650 0.00640 0.00863 0.01046 0.00603 H22 0.55287 0.45762 0.43173 1.00000 0.24734 0.00000 0.00000 C23 0.40502 0.36609 0.46571 1.00000 0.17853 0.25968 0.12141 0.01280 0.01671 -0.06061 0.18654 0.02129 0.00139 0.00138 0.00027 0.00000 0.00978 0.01308 0.00666 0.00726 0.00675 0.00921 0.00472 H23 0.30398 0.32393 0.46632 1.00000 0.22385 0.00000 0.00000 C24 0.47190 0.38472 0.49637 1.00000 0.26742 0.22950 0.13861 -0.03704 0.03564 -0.08688 0.21184 0.02269 0.00200 0.00127 0.00030 0.00000 0.01555 0.01147 0.00854 0.00807 0.00961 0.01165 0.00598 H24 0.57230 0.42818 0.49621 1.00000 0.25421 0.00000 0.00000 C25 0.41002 0.34661 0.53020 1.00000 0.21566 0.28529 0.10219 -0.00502 0.00215 -0.04418 0.20104 0.02228 0.00161 0.00158 0.00026 0.00000 0.01204 0.01523 0.00617 0.00745 0.00681 0.01140 0.00545 H25 0.30866 0.30507 0.52974 1.00000 0.24125 0.00000 0.00000 C26 0.47423 0.36073 0.56311 1.00000 0.34998 0.23837 0.22974 -0.03614 0.04665 -0.06185 0.27270 0.03371 0.00277 0.00174 0.00051 0.00000 0.02599 0.01601 0.01653 0.01322 0.01821 0.01653 0.00886 H26 0.57785 0.39733 0.56375 1.00000 0.32724 0.00000 0.00000 C27 0.41022 0.32968 0.59480 1.00000 0.28620 0.30442 0.11815 0.01225 -0.01948 -0.04677 0.23626 0.02449 0.00195 0.00179 0.00030 0.00000 0.01716 0.01638 0.00690 0.00900 0.00906 0.01603 0.00667 H27A 0.41004 0.41545 0.60941 1.00000 0.35438 0.00000 0.00000 H27B 0.47204 0.25502 0.60621 1.00000 0.35438 0.00000 0.00000 H27C 0.30255 0.29622 0.59158 1.00000 0.35438 0.00000 0.00000 F5 0.05896 0.77924 0.23175 1.00000 0.21735 0.18121 0.12987 -0.00253 -0.04736 -0.08439 0.17615 0.00741 0.00074 0.00058 0.00013 0.00000 0.00558 0.00428 0.00300 0.00299 0.00335 0.00417 0.00228 F6 -0.11211 0.59588 0.17843 1.00000 0.31712 0.21769 0.14506 -0.06095 0.03428 -0.17011 0.22662 0.00847 0.00093 0.00065 0.00014 0.00000 0.00864 0.00572 0.00369 0.00378 0.00468 0.00644 0.00373 C1 0.74020 0.52132 0.30703 1.00000 0.06569 0.07412 0.08981 0.00378 0.01992 0.00986 0.07654 0.00971 0.00060 0.00057 0.00013 0.00000 0.00305 0.00308 0.00320 0.00245 0.00251 0.00234 0.00130 H1 0.81010 0.44433 0.31107 1.00000 0.09185 0.00000 0.00000 C2 0.64750 0.73746 0.29980 1.00000 0.05884 0.07169 0.06373 -0.00056 0.00966 -0.00309 0.06475 0.00772 0.00050 0.00047 0.00011 0.00000 0.00247 0.00276 0.00246 0.00202 0.00204 0.00213 0.00110 C3 0.62603 0.88394 0.29635 1.00000 0.08543 0.06390 0.08064 -0.00160 -0.00280 -0.01003 0.07666 0.00877 0.00066 0.00047 0.00014 0.00000 0.00360 0.00287 0.00290 0.00241 0.00304 0.00239 0.00131 H3 0.71001 0.94937 0.29904 1.00000 0.09199 0.00000 0.00000 C4 0.47679 0.92851 0.28883 1.00000 0.08052 0.06433 0.09662 0.00760 0.00137 0.00904 0.08049 0.00970 0.00067 0.00054 0.00014 0.00000 0.00344 0.00254 0.00346 0.00231 0.00288 0.00258 0.00136 H4 0.45687 1.02749 0.28607 1.00000 0.09659 0.00000 0.00000 C5 0.35358 0.83200 0.28515 1.00000 0.06737 0.09468 0.09441 -0.00645 -0.00462 0.02359 0.08549 0.00980 0.00063 0.00063 0.00014 0.00000 0.00295 0.00407 0.00343 0.00283 0.00249 0.00287 0.00149 H5 0.25143 0.86734 0.28057 1.00000 0.10259 0.00000 0.00000 C6 0.37516 0.69101 0.28787 1.00000 0.04972 0.10254 0.08097 -0.01014 0.00365 -0.00347 0.07775 0.00856 0.00051 0.00065 0.00012 0.00000 0.00239 0.00358 0.00292 0.00295 0.00208 0.00263 0.00128 H6 0.29178 0.62562 0.28434 1.00000 0.09329 0.00000 0.00000 C7 0.52745 0.64418 0.29623 1.00000 0.06600 0.06377 0.06275 -0.00233 0.00597 0.00250 0.06417 0.00779 0.00054 0.00044 0.00011 0.00000 0.00254 0.00232 0.00222 0.00186 0.00223 0.00215 0.00102 C8 0.93896 0.71105 0.31379 1.00000 0.04970 0.11414 0.09617 0.01340 -0.00051 -0.01388 0.08667 0.00930 0.00053 0.00070 0.00014 0.00000 0.00257 0.00397 0.00348 0.00305 0.00227 0.00258 0.00151 H8A 0.96112 0.79130 0.29775 1.00000 0.10400 0.00000 0.00000 H8B 1.01584 0.63472 0.30885 1.00000 0.10400 0.00000 0.00000 C9 0.96005 0.76004 0.35010 1.00000 0.08236 0.15660 0.11350 0.01834 -0.01698 -0.04833 0.11749 0.01072 0.00077 0.00081 0.00017 0.00000 0.00376 0.00582 0.00435 0.00409 0.00331 0.00393 0.00223 H9A 0.89095 0.84347 0.35367 1.00000 0.14099 0.00000 0.00000 H9B 1.06916 0.79410 0.35251 1.00000 0.14099 0.00000 0.00000 C10 0.92973 0.65804 0.37889 1.00000 0.10060 0.11908 0.09903 0.01471 -0.01510 -0.01593 0.10624 0.01106 0.00080 0.00072 0.00016 0.00000 0.00429 0.00467 0.00389 0.00357 0.00337 0.00358 0.00191 H10A 0.81886 0.62788 0.37763 1.00000 0.12749 0.00000 0.00000 H10B 0.99503 0.57229 0.37505 1.00000 0.12749 0.00000 0.00000 C11 0.96084 0.71239 0.41439 1.00000 0.14714 0.16782 0.09613 0.01151 -0.01996 -0.04411 0.13703 0.01239 0.00109 0.00094 0.00018 0.00000 0.00641 0.00663 0.00429 0.00444 0.00436 0.00590 0.00269 H11A 0.89837 0.80031 0.41755 1.00000 0.16444 0.00000 0.00000 H11B 1.07244 0.74037 0.41546 1.00000 0.16444 0.00000 0.00000 C12 0.92903 0.61823 0.44459 1.00000 0.14972 0.17206 0.09883 0.01587 -0.03334 -0.00958 0.14020 0.01440 0.00117 0.00094 0.00018 0.00000 0.00682 0.00697 0.00457 0.00469 0.00468 0.00564 0.00283 H12A 0.99294 0.53099 0.44173 1.00000 0.16824 0.00000 0.00000 H12B 0.81787 0.58894 0.44339 1.00000 0.16824 0.00000 0.00000 C13 0.95859 0.67529 0.48015 1.00000 0.16960 0.16575 0.10680 0.00423 -0.02362 -0.03554 0.14738 0.01435 0.00121 0.00102 0.00020 0.00000 0.00768 0.00694 0.00488 0.00484 0.00521 0.00673 0.00299 H13A 1.06996 0.70422 0.48079 1.00000 0.17686 0.00000 0.00000 H13B 0.89631 0.76386 0.48224 1.00000 0.17686 0.00000 0.00000 C14 0.93081 0.59576 0.51096 1.00000 0.17467 0.17187 0.10478 0.01769 -0.02146 -0.01346 0.15044 0.01587 0.00132 0.00102 0.00019 0.00000 0.00864 0.00764 0.00513 0.00519 0.00534 0.00658 0.00325 H14A 0.99184 0.50655 0.50869 1.00000 0.18053 0.00000 0.00000 H14B 0.81906 0.56803 0.51046 1.00000 0.18053 0.00000 0.00000 C15 0.96126 0.65013 0.54565 1.00000 0.18876 0.18101 0.10185 -0.01089 -0.01905 -0.01757 0.15721 0.01548 0.00132 0.00102 0.00021 0.00000 0.00901 0.00785 0.00521 0.00520 0.00580 0.00714 0.00336 H15A 1.07393 0.67451 0.54636 1.00000 0.18865 0.00000 0.00000 H15B 0.90353 0.74130 0.54753 1.00000 0.18865 0.00000 0.00000 C16 0.93014 0.57548 0.57591 1.00000 0.22593 0.25017 0.10269 0.00489 -0.00666 -0.03193 0.19293 0.01950 0.00170 0.00135 0.00023 0.00000 0.01258 0.01223 0.00584 0.00680 0.00687 0.01072 0.00484 H16A 0.99122 0.48597 0.57463 1.00000 0.23152 0.00000 0.00000 H16B 0.81838 0.54799 0.57497 1.00000 0.23152 0.00000 0.00000 C18 0.50199 0.37290 0.30291 1.00000 0.10842 0.07507 0.09462 -0.01085 0.00280 -0.02445 0.09270 0.00907 0.00077 0.00055 0.00014 0.00000 0.00434 0.00297 0.00342 0.00257 0.00322 0.00296 0.00163 H18A 0.40851 0.37882 0.28770 1.00000 0.11125 0.00000 0.00000 H18B 0.56909 0.29486 0.29404 1.00000 0.11125 0.00000 0.00000 N1 0.78052 0.65668 0.30665 1.00000 0.04620 0.08473 0.07718 0.00043 0.00785 0.00032 0.06937 0.00650 0.00039 0.00043 0.00010 0.00000 0.00200 0.00283 0.00224 0.00187 0.00161 0.00177 0.00103 N2 0.58844 0.50768 0.30100 1.00000 0.07437 0.07044 0.07178 -0.00761 0.00600 -0.00489 0.07220 0.00654 0.00049 0.00039 0.00010 0.00000 0.00265 0.00237 0.00224 0.00189 0.00187 0.00189 0.00105 F1 -0.00151 0.55376 0.22757 1.00000 0.17096 0.12801 0.28633 0.10084 0.00298 0.01077 0.19510 0.01234 0.00068 0.00050 0.00020 0.00000 0.00498 0.00335 0.00722 0.00421 0.00461 0.00326 0.00274 F2 0.12935 0.67405 0.18546 1.00000 0.12561 0.20881 0.21235 0.02243 0.07010 0.03206 0.18226 0.01233 0.00060 0.00069 0.00016 0.00000 0.00347 0.00517 0.00501 0.00442 0.00361 0.00378 0.00223 F3 -0.05410 0.82033 0.18153 1.00000 0.15980 0.13223 0.18544 0.08122 -0.03293 -0.01456 0.15916 0.00894 0.00058 0.00049 0.00014 0.00000 0.00385 0.00314 0.00420 0.00328 0.00323 0.00308 0.00192 F4 -0.18897 0.69930 0.22452 1.00000 0.08974 0.19710 0.15349 0.01506 0.02337 0.02558 0.14678 0.00908 0.00042 0.00062 0.00012 0.00000 0.00247 0.00425 0.00341 0.00340 0.00220 0.00278 0.00162 P1 -0.03023 0.68755 0.20508 1.00000 0.06894 0.06330 0.09365 -0.00218 0.00412 -0.00581 0.07530 0.00223 0.00015 0.00014 0.00004 0.00000 0.00074 0.00066 0.00085 0.00064 0.00064 0.00059 0.00044 Final Structure Factor Calculation for 03src0400 in P2(1)2(1)2(1) Total number of l.s. parameters = 327 Maximum vector length = 511 Memory required = 4251 / 26068 wR2 = 0.2897 before cycle 11 for 6241 data and 2 / 327 parameters GooF = S = 1.046; Restrained GooF = 1.046 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1763 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0910 for 3316 Fo > 4sig(Fo) and 0.1560 for all 6241 data wR2 = 0.2897, GooF = S = 1.046, Restrained GooF = 1.046 for all data Flack x parameter = 0.3305 with su 0.2128 Expected values are 0 (within 3 su's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 36.00 for non-hydrogen and 39.00 for hydrogen atoms Principal mean square atomic displacements U 0.3437 0.2486 0.1008 C17 0.5199 0.1119 0.0589 C19 may be split into 0.4849 0.3222 0.3389 and 0.4210 0.3574 0.3380 0.5447 0.1032 0.0694 C20 may be split into 0.4946 0.3839 0.3688 and 0.4264 0.4122 0.3641 0.4253 0.1941 0.0752 C21 0.3889 0.1398 0.0896 C22 may be split into 0.4859 0.3863 0.4337 and 0.4375 0.4131 0.4305 0.2921 0.1579 0.1096 C23 0.3497 0.1607 0.1251 C24 0.3069 0.1942 0.1020 C25 0.3972 0.2237 0.1971 C26 0.3451 0.2480 0.1157 C27 0.2934 0.1489 0.0861 F5 0.4578 0.1457 0.0764 F6 may be split into -0.0868 0.5780 0.1799 and -0.1374 0.6137 0.1770 0.1034 0.0740 0.0523 C1 0.0739 0.0692 0.0511 C2 0.0898 0.0805 0.0596 C3 0.0990 0.0833 0.0592 C4 0.1119 0.0909 0.0538 C5 0.1069 0.0771 0.0492 C6 0.0706 0.0653 0.0566 C7 0.1234 0.0898 0.0467 C8 0.1882 0.1068 0.0576 C9 0.1388 0.0952 0.0847 C10 0.2070 0.1151 0.0890 C11 0.1856 0.1538 0.0812 C12 0.2074 0.1369 0.0979 C13 0.1953 0.1598 0.0962 C14 0.2036 0.1726 0.0954 C15 0.2726 0.2040 0.1023 C16 0.1234 0.0946 0.0601 C18 0.0848 0.0790 0.0443 N1 0.0846 0.0686 0.0634 N2 0.3357 0.1714 0.0782 F1 0.2716 0.1911 0.0841 F2 0.2571 0.1477 0.0727 F3 0.2102 0.1515 0.0787 F4 0.0946 0.0716 0.0597 P1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.012 0.016 0.020 0.026 0.036 0.052 0.075 0.117 1.000 Number in group 731. 684. 606. 506. 608. 632. 615. 626. 604. 629. GooF 0.946 0.968 0.997 0.951 0.977 1.193 1.201 1.098 1.126 0.969 K 4.412 1.748 1.339 1.078 1.079 1.062 1.054 1.044 1.049 0.999 Resolution(A) 0.77 0.82 0.86 0.90 0.95 1.01 1.08 1.19 1.36 1.71 inf Number in group 624. 645. 624. 613. 626. 619. 617. 621. 627. 625. GooF 0.911 0.907 0.840 0.928 0.961 1.057 1.016 1.207 1.319 1.209 K 1.213 1.201 1.125 1.025 1.056 1.082 1.071 1.094 1.017 0.992 R1 0.615 0.502 0.408 0.341 0.218 0.146 0.097 0.091 0.081 0.074 Recommended weighting scheme: WGHT 0.1775 0.0000 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/su Fc/Fc(max) Resolution(A) -2 1 22 27.50 2.45 6.16 0.012 1.59 6 0 15 50.18 3.20 5.54 0.013 1.24 1 8 31 1.30 24.44 5.26 0.037 0.85 1 0 5 36.22 14.52 5.18 0.028 5.70 6 5 0 28.18 2.79 5.07 0.012 1.13 -1 6 26 359.11 0.52 5.00 0.005 1.06 -6 2 1 22.04 0.94 4.77 0.007 1.36 -8 2 23 165.01 13.14 4.72 0.027 0.88 0 6 4 75.11 34.47 4.39 0.044 1.54 -9 3 22 0.00 14.57 4.18 0.028 0.81 5 0 8 11.80 2.37 4.08 0.011 1.61 -7 2 16 -3.87 20.69 4.05 0.034 1.06 6 2 1 15.53 1.06 3.94 0.008 1.36 4 0 26 38.64 16.37 3.93 0.030 1.21 0 1 16 962.29 498.48 3.91 0.166 2.32 -1 1 23 98.41 50.25 3.88 0.053 1.61 3 0 18 89.41 45.01 3.85 0.050 1.70 0 2 26 13.83 4.16 3.81 0.015 1.40 2 9 27 0.00 15.56 3.81 0.029 0.82 7 2 0 23.44 0.10 3.67 0.002 1.18 1 1 23 106.81 49.52 3.60 0.052 1.61 5 7 0 19.73 0.73 3.56 0.006 1.05 -6 1 11 15.66 1.39 3.56 0.009 1.31 4 7 5 42.88 20.89 3.49 0.034 1.12 -5 5 7 16.64 3.45 3.49 0.014 1.23 3 4 8 47.68 99.02 3.46 0.074 1.69 0 1 11 54.04 119.01 3.44 0.081 3.26 1 8 0 39.46 6.62 3.40 0.019 1.16 3 0 20 102.74 56.62 3.39 0.056 1.59 5 0 18 183.40 100.94 3.38 0.075 1.33 4 0 16 99.83 54.75 3.36 0.055 1.59 5 1 15 67.61 35.46 3.34 0.044 1.40 0 3 2 140.25 79.98 3.31 0.067 3.09 1 8 33 1.61 13.53 3.31 0.027 0.82 -7 1 5 19.77 1.04 3.26 0.008 1.20 1 0 7 347.65 200.71 3.23 0.105 4.61 1 0 32 12.38 30.46 3.23 0.041 1.18 -6 1 12 217.40 117.81 3.20 0.081 1.29 0 7 9 38.30 19.07 3.19 0.033 1.28 0 1 23 102.58 58.73 3.19 0.057 1.64 4 0 18 83.33 47.92 3.13 0.052 1.51 -3 5 11 24.75 10.15 3.12 0.024 1.43 -5 7 10 43.16 19.32 3.11 0.033 1.02 1 1 25 104.22 60.78 3.06 0.058 1.49 -5 4 6 38.35 19.53 3.03 0.033 1.35 4 4 0 38.13 20.32 3.02 0.034 1.58 5 0 9 147.86 86.52 3.01 0.069 1.59 2 4 8 145.39 267.79 2.98 0.122 1.89 0 6 7 110.55 65.93 2.98 0.060 1.50 7 1 17 30.44 13.86 2.97 0.028 1.07 Bond lengths and angles C17 - Distance Angles C16 1.4759 (0.0130) H17A 0.9800 109.47 H17B 0.9800 109.47 109.47 H17C 0.9800 109.47 109.47 109.47 C17 - C16 H17A H17B C19 - Distance Angles C20 1.2057 (0.0111) C18 1.4569 (0.0099) 135.97 (0.73) H19 0.9500 112.02 112.02 C19 - C20 C18 C20 - Distance Angles C19 1.2057 (0.0111) C21 1.4696 (0.0124) 135.38 (0.97) H20 0.9500 112.31 112.31 C20 - C19 C21 C21 - Distance Angles C22 1.2788 (0.0154) C20 1.4696 (0.0124) 132.18 (1.27) H21 0.9500 113.91 113.91 C21 - C22 C20 C22 - Distance Angles C21 1.2788 (0.0154) C23 1.4094 (0.0125) 129.74 (1.26) H22 0.9500 115.13 115.13 C22 - C21 C23 C23 - Distance Angles C24 1.3172 (0.0142) C22 1.4094 (0.0125) 129.34 (1.25) H23 0.9500 115.33 115.33 C23 - C24 C22 C24 - Distance Angles C23 1.3172 (0.0142) C25 1.4438 (0.0146) 127.41 (1.34) H24 0.9500 116.29 116.29 C24 - C23 C25 C25 - Distance Angles C26 1.3803 (0.0200) C24 1.4438 (0.0146) 130.48 (1.52) H25 0.9500 114.76 114.76 C25 - C26 C24 C26 - Distance Angles C27 1.3624 (0.0194) C25 1.3803 (0.0200) 129.24 (1.90) H26 0.9500 115.38 115.38 C26 - C27 C25 C27 - Distance Angles C26 1.3624 (0.0194) H27A 0.9800 109.47 H27B 0.9800 109.47 109.47 H27C 0.9800 109.47 109.47 109.47 C27 - C26 H27A H27B F5 - Distance Angles P1 1.5373 (0.0045) F5 - F6 - Distance Angles P1 1.5066 (0.0049) F6 - C1 - Distance Angles N1 1.3160 (0.0064) N2 1.3235 (0.0065) 110.37 (0.44) H1 0.9500 124.82 124.82 C1 - N1 N2 C2 - Distance Angles C7 1.3553 (0.0064) N1 1.3912 (0.0056) 106.60 (0.38) C3 1.3928 (0.0060) 121.86 (0.44) 131.53 (0.43) C2 - C7 N1 C3 - Distance Angles C4 1.3727 (0.0075) C2 1.3928 (0.0060) 116.29 (0.46) H3 0.9500 121.86 121.86 C3 - C4 C2 C4 - Distance Angles C3 1.3727 (0.0075) C5 1.3959 (0.0079) 121.63 (0.46) H4 0.9500 119.18 119.18 C4 - C3 C5 C5 - Distance Angles C6 1.3397 (0.0081) C4 1.3959 (0.0079) 121.92 (0.48) H5 0.9500 119.04 119.04 C5 - C6 C4 C6 - Distance Angles C5 1.3397 (0.0081) C7 1.4104 (0.0065) 116.89 (0.47) H6 0.9500 121.55 121.55 C6 - C5 C7 C7 - Distance Angles C2 1.3553 (0.0064) N2 1.3947 (0.0056) 107.27 (0.40) C6 1.4104 (0.0065) 121.35 (0.41) 131.34 (0.45) C7 - C2 N2 C8 - Distance Angles N1 1.4725 (0.0058) C9 1.4750 (0.0087) 113.27 (0.43) H8A 0.9900 108.92 108.92 H8B 0.9900 108.92 108.92 107.74 C8 - N1 C9 H8A C9 - Distance Angles C8 1.4750 (0.0087) C10 1.4824 (0.0085) 118.56 (0.58) H9A 0.9900 107.67 107.67 H9B 0.9900 107.67 107.67 107.08 C9 - C8 C10 H9A C10 - Distance Angles C11 1.4758 (0.0090) C9 1.4824 (0.0085) 115.47 (0.58) H10A 0.9900 108.41 108.41 H10B 0.9900 108.41 108.41 107.46 C10 - C11 C9 H10A C11 - Distance Angles C10 1.4758 (0.0090) C12 1.4800 (0.0100) 118.68 (0.63) H11A 0.9900 107.64 107.64 H11B 0.9900 107.64 107.64 107.06 C11 - C10 C12 H11A C12 - Distance Angles C11 1.4800 (0.0100) C13 1.4846 (0.0100) 118.02 (0.74) H12A 0.9900 107.80 107.80 H12B 0.9900 107.80 107.80 107.14 C12 - C11 C13 H12A C13 - Distance Angles C14 1.4156 (0.0107) C12 1.4846 (0.0100) 123.06 (0.82) H13A 0.9900 106.57 106.57 H13B 0.9900 106.57 106.57 106.54 C13 - C14 C12 H13A C14 - Distance Angles C13 1.4156 (0.0108) C15 1.4462 (0.0109) 123.29 (0.86) H14A 0.9900 106.51 106.51 H14B 0.9900 106.51 106.51 106.51 C14 - C13 C15 H14A C15 - Distance Angles C16 1.3793 (0.0117) C14 1.4462 (0.0109) 123.86 (0.91) H15A 0.9900 106.36 106.36 H15B 0.9900 106.36 106.36 106.45 C15 - C16 C14 H15A C16 - Distance Angles C15 1.3793 (0.0117) C17 1.4759 (0.0130) 122.41 (1.12) H16A 0.9900 106.73 106.73 H16B 0.9900 106.73 106.73 106.61 C16 - C15 C17 H16A C18 - Distance Angles C19 1.4569 (0.0099) N2 1.4663 (0.0062) 112.03 (0.48) H18A 0.9900 109.21 109.21 H18B 0.9900 109.21 109.21 107.90 C18 - C19 N2 H18A N1 - Distance Angles C1 1.3160 (0.0064) C2 1.3912 (0.0056) 108.29 (0.37) C8 1.4725 (0.0058) 124.96 (0.45) 126.70 (0.43) N1 - C1 C2 N2 - Distance Angles C1 1.3235 (0.0065) C7 1.3947 (0.0056) 107.47 (0.40) C18 1.4663 (0.0062) 124.64 (0.46) 127.60 (0.43) N2 - C1 C7 F1 - Distance Angles P1 1.5418 (0.0044) F1 - F2 - Distance Angles P1 1.5620 (0.0045) F2 - F3 - Distance Angles P1 1.5511 (0.0039) F3 - F4 - Distance Angles P1 1.5511 (0.0039) F4 - P1 - Distance Angles F6 1.5066 (0.0049) F5 1.5373 (0.0045) 177.95 (0.43) F1 1.5418 (0.0044) 89.27 (0.39) 90.33 (0.36) F4 1.5511 (0.0039) 87.66 (0.35) 94.31 (0.34) 85.94 (0.31) F3 1.5511 (0.0039) 90.22 (0.33) 90.10 (0.29) 177.85 (0.34) 96.13 (0.29) F2 1.5620 (0.0045) 91.93 (0.39) 86.09 (0.36) 93.64 (0.33) 179.42 (0.38) 84.29 (0.31) P1 - F6 F5 F1 F4 F3 FMAP and GRID set by program FMAP 2 3 43 GRID -0.625 -2 -2 0.625 2 2 R1 = 0.1444 for 3713 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.40 at 0.9330 0.8331 0.2197 [ 1.28 A from F5 ] Deepest hole -0.29 at 0.9881 0.7416 0.2233 [ 0.77 A from F5 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 3859 / 26196 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.0670 0.8331 0.2197 1.00000 0.05 0.40 1.28 F5 1.47 F3 1.51 P1 1.64 F4 Q2 1 0.0325 0.5606 0.1884 1.00000 0.05 0.38 1.33 F6 1.35 F2 1.45 P1 1.53 F1 Q3 1 0.0032 0.5477 0.1934 1.00000 0.05 0.37 1.23 F6 1.31 F1 1.41 P1 1.63 F2 Q4 1 -0.1210 0.6186 0.2348 1.00000 0.05 0.33 1.03 F4 1.22 F1 1.52 P1 2.16 F5 Q5 1 -0.1357 0.7270 0.1750 1.00000 0.05 0.30 1.15 F3 1.25 F6 1.51 P1 1.97 F4 Q6 1 -0.1401 0.6092 0.1729 1.00000 0.05 0.27 0.34 F6 1.71 P1 2.14 F3 2.19 F4 Q7 1 -0.2096 0.6826 0.1926 1.00000 0.05 0.27 1.25 F4 1.28 F6 1.61 P1 1.90 F3 Q8 1 0.0479 0.6479 0.2388 1.00000 0.05 0.26 1.07 F1 1.26 F5 1.50 P1 2.15 F4 Q9 1 1.0482 0.6500 0.3502 1.00000 0.05 0.25 1.28 C9 1.28 H10B 1.37 H9B 1.50 C10 Q10 1 0.0703 0.7613 0.1749 1.00000 0.05 0.25 1.04 F2 1.23 F3 1.60 P1 2.07 H1 Shortest distances between peaks (including symmetry equivalents) 2 3 0.34 5 7 1.01 5 6 1.11 6 7 1.18 4 8 1.48 3 6 1.57 2 6 1.65 5 10 1.79 4 7 1.89 2 10 1.98 3 8 2.01 3 4 2.02 1 5 2.06 2 8 2.10 1 8 2.13 1 7 2.13 1 4 2.15 3 5 2.18 2 5 2.18 1 10 2.18 3 10 2.20 3 7 2.22 2 4 2.28 6 10 2.30 2 7 2.37 4 6 2.38 4 5 2.51 7 10 2.59 8 10 2.68 1 6 2.83 7 8 2.84 1 3 2.92 1 2 2.95 5 8 3.00 Time profile in seconds ----------------------- 0.02: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: 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 0.00: Analyse other restraints etc. 0.77: 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 7.47: Structure factors and derivatives 9.02: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.72: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.09: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 15:42:30 Total CPU time: 18.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++