+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 17:05:40 on 04-Aug-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P2(1)/n CELL 0.71073 6.9597 26.6109 12.1011 90.000 105.145 90.000 ZERR 4.00 0.0014 0.0053 0.0024 0.000 0.030 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 88 112 16 8 V = 2163.33 F(000) = 816.0 Mu = 0.08 mm-1 Cell Wt = 1521.94 Rho = 1.168 SHEL 7 0.9 FMAP 2 PLAN 30 SIZE 0.10 0.10 0.10 DFIX 0.005 0.95 N4 H4N BOND L.S. 4 TEMP 23.00 WGHT 0.121400 EXTI 0.004755 FVAR 0.23565 C1 1 0.196258 -0.059866 0.362246 11.00000 0.07207 0.06005 = 0.08189 -0.03133 0.02449 -0.00915 AFIX 33 H1A 2 0.154428 -0.051855 0.282178 11.00000 -1.50000 H1B 2 0.097077 -0.080396 0.382326 11.00000 -1.50000 H1C 2 0.320143 -0.077807 0.378228 11.00000 -1.50000 AFIX 0 C2 1 0.279073 -0.018040 0.542095 11.00000 0.05248 0.05362 = 0.05759 -0.00372 0.01549 -0.00259 C3 1 0.295224 0.031851 0.597377 11.00000 0.05142 0.03854 = 0.04819 -0.00487 0.01525 0.00023 C4 1 0.345226 0.034883 0.715576 11.00000 0.06325 0.03836 = 0.06073 0.00732 0.01631 0.00274 AFIX 43 H4 2 0.371707 0.005614 0.758894 11.00000 -1.20000 AFIX 0 C5 1 0.356262 0.080413 0.769681 11.00000 0.05583 0.05254 = 0.04093 0.00077 0.01001 0.00231 AFIX 43 H5 2 0.389147 0.081570 0.849231 11.00000 -1.20000 AFIX 0 C6 1 0.318901 0.125156 0.707263 11.00000 0.04533 0.03852 = 0.04206 -0.00385 0.00713 -0.00138 C7 1 0.270231 0.121781 0.588560 11.00000 0.06678 0.03634 = 0.04532 -0.00075 0.00852 0.00087 AFIX 43 H7 2 0.244967 0.150980 0.544928 11.00000 -1.20000 AFIX 0 C8 1 0.258813 0.076004 0.534574 11.00000 0.06174 0.05186 = 0.03797 -0.00329 0.00895 0.00114 AFIX 43 H8 2 0.226305 0.074643 0.455046 11.00000 -1.20000 AFIX 0 C9 1 0.311987 0.174636 0.760428 11.00000 0.04791 0.04186 = 0.04354 0.00256 0.00924 -0.00101 C10 1 0.197460 0.249188 0.766561 11.00000 0.05474 0.04261 = 0.04647 0.00164 0.00120 0.00006 C11 1 0.136948 0.326921 0.824635 11.00000 0.07821 0.04409 = 0.07466 -0.00867 0.00572 0.00405 AFIX 43 H11 2 0.072273 0.357752 0.810413 11.00000 -1.20000 AFIX 0 C12 1 0.268774 0.319380 0.932785 11.00000 0.07793 0.04898 = 0.06520 -0.01927 0.00411 -0.00105 AFIX 43 H12 2 0.287133 0.344341 0.988359 11.00000 -1.20000 AFIX 0 C13 1 0.367601 0.275992 0.955093 11.00000 0.05533 0.05647 = 0.05099 -0.01245 0.00285 -0.00734 AFIX 43 H13 2 0.456171 0.270210 1.026081 11.00000 -1.20000 AFIX 0 C14 1 0.410876 0.192472 0.867138 11.00000 0.04667 0.04450 = 0.03221 -0.00149 0.00494 -0.00268 C15 1 0.775222 0.179987 0.948519 11.00000 0.04181 0.07855 = 0.06310 -0.01227 0.00685 0.00527 C16 1 0.819959 0.236868 0.945768 11.00000 0.07052 0.08568 = 0.14545 -0.02680 0.04130 -0.02327 AFIX 33 H16A 2 0.801719 0.252513 1.013790 11.00000 -1.50000 H16B 2 0.731004 0.251806 0.879718 11.00000 -1.50000 H16C 2 0.954908 0.241573 0.942091 11.00000 -1.50000 AFIX 0 C17 1 0.803843 0.156275 0.839444 11.00000 0.06426 0.10207 = 0.06509 -0.01616 0.02313 -0.00194 AFIX 33 H17A 2 0.708691 0.170124 0.774395 11.00000 -1.50000 H17B 2 0.784814 0.120601 0.841842 11.00000 -1.50000 H17C 2 0.936076 0.163148 0.833309 11.00000 -1.50000 AFIX 0 C18 1 0.916858 0.161021 1.059607 11.00000 0.07902 0.13754 = 0.06633 -0.02147 -0.00229 0.02621 AFIX 23 H18A 2 1.042424 0.177994 1.065323 11.00000 -1.20000 H18B 2 0.865809 0.174371 1.120932 11.00000 -1.20000 AFIX 0 C19 1 0.969934 0.106604 1.091146 11.00000 0.10118 0.08997 = 0.08524 0.01776 0.03793 0.02464 C20 1 1.074584 0.104127 1.214032 11.00000 0.11881 0.36704 = 0.07869 0.03817 -0.01169 0.10268 AFIX 33 H20A 2 1.107548 0.069821 1.235339 11.00000 -1.50000 H20B 2 0.989905 0.117211 1.258367 11.00000 -1.50000 H20C 2 1.194337 0.123737 1.228287 11.00000 -1.50000 AFIX 0 C21 1 1.109630 0.085076 1.025998 11.00000 0.14442 0.18941 = 0.13053 0.03194 0.06011 0.09441 AFIX 33 H21A 2 1.044757 0.084930 0.945566 11.00000 -1.50000 H21B 2 1.144975 0.051327 1.051327 11.00000 -1.50000 H21C 2 1.227674 0.105329 1.039822 11.00000 -1.50000 AFIX 0 C22 1 0.778412 0.075233 1.072136 11.00000 0.11676 0.16090 = 0.15564 0.06015 0.03677 0.02058 AFIX 33 H22A 2 0.707952 0.076047 0.992554 11.00000 -1.50000 H22B 2 0.695686 0.088947 1.116932 11.00000 -1.50000 H22C 2 0.812075 0.041127 1.095059 11.00000 -1.50000 AFIX 0 N1 3 0.184945 0.210238 0.699119 11.00000 0.06323 0.04286 = 0.04506 -0.00634 0.00335 0.00155 N2 3 0.098529 0.293344 0.741906 11.00000 0.07718 0.04271 = 0.06091 -0.00326 0.00253 0.00747 N3 3 0.335673 0.240479 0.871580 11.00000 0.04781 0.04521 = 0.03969 -0.00790 0.00317 -0.00106 N4 3 0.563774 0.171260 0.952460 11.00000 0.05125 0.06402 = 0.03619 0.00292 0.00636 0.00333 O1 4 0.310966 -0.057536 0.591021 11.00000 0.12251 0.04636 = 0.08245 0.00141 0.02458 -0.00034 O2 4 0.221998 -0.014086 0.428389 11.00000 0.08178 0.05014 = 0.06472 -0.01677 0.01798 -0.00189 H4N 2 0.550283 0.175120 1.012557 11.00000 0.05766 HKLF 4 Covalent radii and connectivity table for s92 in P2(1)/n C 0.770 H 0.320 N 0.700 O 0.660 C1 - O2 C2 - O1 O2 C3 C3 - C4 C8 C2 C4 - C5 C3 C5 - C4 C6 C6 - C7 C5 C9 C7 - C8 C6 C8 - C7 C3 C9 - N1 C14 C6 C10 - N1 N2 N3 C11 - N2 C12 C12 - C13 C11 C13 - C12 N3 C14 - C9 N3 N4 C15 - N4 C17 C18 C16 C16 - C15 C17 - C15 C18 - C19 C15 C19 - C20 C21 C18 C22 C20 - C19 C21 - C19 C22 - C19 N1 - C10 C9 N2 - C11 C10 N3 - C13 C14 C10 N4 - C14 C15 O1 - C2 O2 - C2 C1 h k l Fo^2 Sigma Why rejected 1 0 0 0.84 0.21 observed but should be systematically absent 15287 Reflections read, of which 2553 rejected -7 =< h =< 7, -29 =< k =< 29, -13 =< l =< 13, Max. 2-theta = 46.49 1 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 0 2 3 29.04 0.29 7 3.53 1 1 4 13.72 0.29 6 2.75 0 2 4 32.49 0.29 7 4.23 0 3 4 89.84 0.32 7 27.63 0 1 5 30.79 0.38 8 3.08 2 1 5 25.37 0.39 7 4.02 0 3 5 41.55 0.31 7 8.26 0 1 7 19.14 0.37 8 2.11 0 0 8 9.33 0.50 3 5.97 0 1 8 28.98 0.40 8 4.33 1 3 8 7.18 0.50 4 2.60 11 Inconsistent equivalents 3097 Unique reflections, of which 0 suppressed R(int) = 0.1065 R(sigma) = 0.1003 Friedel opposites merged Maximum memory for data reduction = 2558 / 30737 Default effective X-H distances for T = 23.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 0.98 0.97 0.96 0.93 0.86 0.89 1.10 0.82 0.93 0.86 0.93 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 = 3320 / 320598 wR2 = 0.2106 before cycle 1 for 3097 data and 258 / 258 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.950 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.759 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.942; Restrained GooF = 0.941 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1214 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23565 0.00111 -0.003 OSF 2 0.00475 0.00229 0.000 EXTI Mean shift/esd = 0.001 Maximum = -0.003 for OSF Max. shift = 0.000 A for H4N Max. dU = 0.000 for H4N Least-squares cycle 2 Maximum vector length = 511 Memory required = 3320 / 320598 wR2 = 0.2106 before cycle 2 for 3097 data and 258 / 258 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.950 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.759 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.941; Restrained GooF = 0.941 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1214 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23565 0.00111 0.000 OSF 2 0.00475 0.00229 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for y N3 Max. shift = 0.000 A for H4N Max. dU = 0.000 for H4N Least-squares cycle 3 Maximum vector length = 511 Memory required = 3320 / 320598 wR2 = 0.2106 before cycle 3 for 3097 data and 258 / 258 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.950 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.759 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.941; Restrained GooF = 0.941 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1214 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23565 0.00111 0.000 OSF 2 0.00475 0.00229 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H4N Max. dU = 0.000 for H4N Least-squares cycle 4 Maximum vector length = 511 Memory required = 3320 / 320598 wR2 = 0.2106 before cycle 4 for 3097 data and 258 / 258 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.950 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.759 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.941; Restrained GooF = 0.941 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1214 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23565 0.00111 0.000 OSF 2 0.00475 0.00229 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H4N Max. dU = 0.000 for H4N Largest correlation matrix elements 0.577 U11 H4N / z N4 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.1544 -0.0519 0.2822 33 0.960 0.000 C1 O2 H1A H1B 0.0971 -0.0804 0.3823 33 0.960 0.000 C1 O2 H1A H1C 0.3201 -0.0778 0.3782 33 0.960 0.000 C1 O2 H1A H4 0.3717 0.0056 0.7589 43 0.930 0.000 C4 C5 C3 H5 0.3891 0.0816 0.8492 43 0.930 0.000 C5 C4 C6 H7 0.2450 0.1510 0.5449 43 0.930 0.000 C7 C8 C6 H8 0.2263 0.0746 0.4550 43 0.930 0.000 C8 C7 C3 H11 0.0723 0.3578 0.8104 43 0.930 0.000 C11 N2 C12 H12 0.2871 0.3443 0.9884 43 0.930 0.000 C12 C13 C11 H13 0.4562 0.2702 1.0261 43 0.930 0.000 C13 C12 N3 H16A 0.8017 0.2525 1.0138 33 0.960 0.000 C16 C15 H16A H16B 0.7310 0.2518 0.8797 33 0.960 0.000 C16 C15 H16A H16C 0.9549 0.2416 0.9421 33 0.960 0.000 C16 C15 H16A H17A 0.7087 0.1701 0.7744 33 0.960 0.000 C17 C15 H17A H17B 0.7848 0.1206 0.8418 33 0.960 0.000 C17 C15 H17A H17C 0.9361 0.1631 0.8333 33 0.960 0.000 C17 C15 H17A H18A 1.0424 0.1780 1.0653 23 0.970 0.000 C18 C19 C15 H18B 0.8658 0.1744 1.1209 23 0.970 0.000 C18 C19 C15 H20A 1.1075 0.0698 1.2353 33 0.960 0.000 C20 C19 H20A H20B 0.9899 0.1172 1.2584 33 0.960 0.000 C20 C19 H20A H20C 1.1943 0.1237 1.2283 33 0.960 0.000 C20 C19 H20A H21A 1.0448 0.0849 0.9456 33 0.960 0.000 C21 C19 H21A H21B 1.1450 0.0513 1.0513 33 0.960 0.000 C21 C19 H21A H21C 1.2277 0.1053 1.0398 33 0.960 0.000 C21 C19 H21A H22A 0.7080 0.0760 0.9926 33 0.960 0.000 C22 C19 H22A H22B 0.6957 0.0889 1.1169 33 0.960 0.000 C22 C19 H22A H22C 0.8121 0.0411 1.0951 33 0.960 0.000 C22 C19 H22A s92 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.19626 -0.05987 0.36225 1.00000 0.07207 0.06005 0.08189 -0.03133 0.02449 -0.00915 0.07052 0.00740 0.00062 0.00016 0.00036 0.00000 0.00305 0.00323 0.00309 0.00255 0.00235 0.00244 0.00134 H1A 0.15443 -0.05186 0.28218 1.00000 0.10578 0.00000 0.00000 H1B 0.09708 -0.08040 0.38233 1.00000 0.10578 0.00000 0.00000 H1C 0.32014 -0.07781 0.37823 1.00000 0.10578 0.00000 0.00000 C2 0.27907 -0.01804 0.54210 1.00000 0.05248 0.05362 0.05759 -0.00372 0.01549 -0.00259 0.05436 0.00751 0.00056 0.00017 0.00035 0.00000 0.00259 0.00315 0.00271 0.00232 0.00199 0.00220 0.00109 C3 0.29522 0.03185 0.59738 1.00000 0.05142 0.03854 0.04819 -0.00487 0.01525 0.00023 0.04563 0.00667 0.00052 0.00014 0.00030 0.00000 0.00241 0.00258 0.00238 0.00188 0.00180 0.00191 0.00099 C4 0.34523 0.03488 0.71558 1.00000 0.06325 0.03836 0.06073 0.00732 0.01631 0.00274 0.05409 0.00729 0.00056 0.00015 0.00033 0.00000 0.00272 0.00267 0.00271 0.00204 0.00201 0.00206 0.00110 H4 0.37171 0.00561 0.75889 1.00000 0.06491 0.00000 0.00000 C5 0.35626 0.08041 0.76968 1.00000 0.05583 0.05254 0.04093 0.00077 0.01001 0.00231 0.05025 0.00706 0.00055 0.00015 0.00031 0.00000 0.00258 0.00288 0.00213 0.00198 0.00176 0.00204 0.00107 H5 0.38915 0.08157 0.84923 1.00000 0.06031 0.00000 0.00000 C6 0.31890 0.12516 0.70726 1.00000 0.04533 0.03852 0.04206 -0.00385 0.00713 -0.00138 0.04277 0.00625 0.00050 0.00014 0.00029 0.00000 0.00228 0.00253 0.00217 0.00177 0.00166 0.00181 0.00097 C7 0.27023 0.12178 0.58856 1.00000 0.06678 0.03634 0.04532 -0.00075 0.00852 0.00087 0.05063 0.00662 0.00054 0.00014 0.00029 0.00000 0.00273 0.00255 0.00235 0.00182 0.00188 0.00201 0.00107 H7 0.24497 0.15098 0.54493 1.00000 0.06075 0.00000 0.00000 C8 0.25881 0.07600 0.53457 1.00000 0.06174 0.05186 0.03797 -0.00329 0.00895 0.00114 0.05129 0.00701 0.00056 0.00015 0.00031 0.00000 0.00261 0.00288 0.00211 0.00201 0.00180 0.00206 0.00108 H8 0.22630 0.07464 0.45505 1.00000 0.06154 0.00000 0.00000 C9 0.31199 0.17464 0.76043 1.00000 0.04791 0.04186 0.04354 0.00256 0.00924 -0.00101 0.04494 0.00652 0.00052 0.00014 0.00029 0.00000 0.00226 0.00250 0.00218 0.00189 0.00175 0.00195 0.00098 C10 0.19746 0.24919 0.76656 1.00000 0.05474 0.04261 0.04647 0.00164 0.00120 0.00006 0.05019 0.00710 0.00056 0.00016 0.00031 0.00000 0.00255 0.00265 0.00233 0.00201 0.00192 0.00204 0.00105 C11 0.13695 0.32692 0.82463 1.00000 0.07821 0.04409 0.07466 -0.00867 0.00572 0.00405 0.06832 0.00777 0.00063 0.00016 0.00037 0.00000 0.00314 0.00292 0.00300 0.00237 0.00243 0.00234 0.00129 H11 0.07227 0.35775 0.81041 1.00000 0.08198 0.00000 0.00000 C12 0.26877 0.31938 0.93279 1.00000 0.07793 0.04898 0.06520 -0.01927 0.00411 -0.00105 0.06676 0.00745 0.00064 0.00017 0.00035 0.00000 0.00311 0.00315 0.00287 0.00225 0.00231 0.00245 0.00128 H12 0.28713 0.34434 0.98836 1.00000 0.08012 0.00000 0.00000 C13 0.36760 0.27599 0.95509 1.00000 0.05533 0.05647 0.05099 -0.01245 0.00285 -0.00734 0.05633 0.00695 0.00058 0.00016 0.00033 0.00000 0.00261 0.00308 0.00239 0.00216 0.00185 0.00229 0.00114 H13 0.45617 0.27021 1.02608 1.00000 0.06759 0.00000 0.00000 C14 0.41088 0.19247 0.86714 1.00000 0.04667 0.04450 0.03221 -0.00149 0.00494 -0.00268 0.04213 0.00641 0.00052 0.00014 0.00027 0.00000 0.00224 0.00265 0.00207 0.00170 0.00171 0.00190 0.00097 C15 0.77522 0.17999 0.94852 1.00000 0.04181 0.07855 0.06310 -0.01227 0.00685 0.00527 0.06244 0.00763 0.00057 0.00018 0.00034 0.00000 0.00247 0.00354 0.00261 0.00231 0.00192 0.00223 0.00124 C16 0.81996 0.23687 0.94577 1.00000 0.07052 0.08568 0.14545 -0.02679 0.04130 -0.02327 0.09810 0.00931 0.00071 0.00020 0.00049 0.00000 0.00353 0.00447 0.00485 0.00353 0.00324 0.00299 0.00183 H16A 0.80172 0.25251 1.01379 1.00000 0.14716 0.00000 0.00000 H16B 0.73100 0.25181 0.87972 1.00000 0.14716 0.00000 0.00000 H16C 0.95491 0.24157 0.94209 1.00000 0.14716 0.00000 0.00000 C17 0.80384 0.15628 0.83944 1.00000 0.06426 0.10207 0.06509 -0.01616 0.02313 -0.00194 0.07597 0.00797 0.00060 0.00019 0.00034 0.00000 0.00286 0.00418 0.00277 0.00261 0.00220 0.00268 0.00145 H17A 0.70869 0.17012 0.77440 1.00000 0.11396 0.00000 0.00000 H17B 0.78481 0.12060 0.84184 1.00000 0.11396 0.00000 0.00000 H17C 0.93608 0.16315 0.83331 1.00000 0.11396 0.00000 0.00000 C18 0.91686 0.16102 1.05961 1.00000 0.07902 0.13754 0.06633 -0.02147 -0.00229 0.02621 0.09827 0.00904 0.00070 0.00023 0.00038 0.00000 0.00350 0.00576 0.00305 0.00307 0.00254 0.00343 0.00192 H18A 1.04242 0.17799 1.06532 1.00000 0.11793 0.00000 0.00000 H18B 0.86581 0.17437 1.12093 1.00000 0.11793 0.00000 0.00000 C19 0.96993 0.10660 1.09115 1.00000 0.10118 0.08997 0.08524 0.01776 0.03793 0.02464 0.08959 0.01152 0.00086 0.00022 0.00041 0.00000 0.00423 0.00452 0.00365 0.00309 0.00319 0.00366 0.00165 C20 1.07458 0.10413 1.21403 1.00000 0.11881 0.36704 0.07869 0.03817 -0.01169 0.10268 0.19519 0.01453 0.00100 0.00034 0.00050 0.00000 0.00534 0.01316 0.00444 0.00578 0.00372 0.00681 0.00437 H20A 1.10755 0.06982 1.23534 1.00000 0.29278 0.00000 0.00000 H20B 0.98991 0.11721 1.25837 1.00000 0.29278 0.00000 0.00000 H20C 1.19434 0.12374 1.22829 1.00000 0.29278 0.00000 0.00000 C21 1.10963 0.08508 1.02600 1.00000 0.14441 0.18941 0.13053 0.03194 0.06011 0.09441 0.15026 0.01433 0.00096 0.00027 0.00056 0.00000 0.00613 0.00784 0.00534 0.00487 0.00466 0.00547 0.00304 H21A 1.04476 0.08493 0.94557 1.00000 0.22539 0.00000 0.00000 H21B 1.14497 0.05133 1.05133 1.00000 0.22539 0.00000 0.00000 H21C 1.22767 0.10533 1.03982 1.00000 0.22539 0.00000 0.00000 C22 0.77841 0.07523 1.07214 1.00000 0.11676 0.16090 0.15564 0.06015 0.03677 0.02058 0.14421 0.01420 0.00095 0.00027 0.00059 0.00000 0.00562 0.00702 0.00647 0.00515 0.00440 0.00505 0.00271 H22A 0.70795 0.07605 0.99255 1.00000 0.21632 0.00000 0.00000 H22B 0.69569 0.08895 1.11693 1.00000 0.21632 0.00000 0.00000 H22C 0.81208 0.04113 1.09506 1.00000 0.21632 0.00000 0.00000 N1 0.18494 0.21024 0.69912 1.00000 0.06323 0.04286 0.04506 -0.00634 0.00335 0.00155 0.05240 0.00546 0.00046 0.00012 0.00024 0.00000 0.00218 0.00221 0.00187 0.00165 0.00158 0.00170 0.00092 N2 0.09853 0.29334 0.74191 1.00000 0.07718 0.04271 0.06091 -0.00326 0.00253 0.00747 0.06317 0.00627 0.00052 0.00013 0.00028 0.00000 0.00247 0.00232 0.00215 0.00179 0.00178 0.00193 0.00102 N3 0.33567 0.24048 0.87158 1.00000 0.04781 0.04521 0.03969 -0.00790 0.00317 -0.00106 0.04578 0.00526 0.00043 0.00012 0.00023 0.00000 0.00193 0.00222 0.00176 0.00156 0.00141 0.00159 0.00085 N4 0.56377 0.17126 0.95246 1.00000 0.05125 0.06402 0.03619 0.00291 0.00636 0.00333 0.05143 0.00641 0.00047 0.00013 0.00031 0.00000 0.00224 0.00258 0.00202 0.00172 0.00168 0.00171 0.00100 O1 0.31097 -0.05754 0.59102 1.00000 0.12251 0.04636 0.08245 0.00141 0.02458 -0.00034 0.08418 0.00585 0.00051 0.00012 0.00026 0.00000 0.00289 0.00221 0.00220 0.00179 0.00192 0.00200 0.00105 O2 0.22200 -0.01409 0.42839 1.00000 0.08177 0.05014 0.06472 -0.01677 0.01798 -0.00189 0.06576 0.00497 0.00040 0.00010 0.00023 0.00000 0.00210 0.00198 0.00194 0.00147 0.00146 0.00156 0.00087 H4N 0.55028 0.17512 1.01256 1.00000 0.05765 0.07345 0.00578 0.00146 0.00344 0.00000 0.01465 Final Structure Factor Calculation for s92 in P2(1)/n Total number of l.s. parameters = 258 Maximum vector length = 511 Memory required = 3062 / 22995 wR2 = 0.2106 before cycle 5 for 3097 data and 0 / 258 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 1. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.950 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.759 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.941; Restrained GooF = 0.941 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1214 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0650 for 1640 Fo > 4sig(Fo) and 0.1413 for all 3097 data wR2 = 0.2106, GooF = S = 0.941, Restrained GooF = 0.941 for all data Occupancy sum of asymmetric unit = 28.00 for non-hydrogen and 28.00 for hydrogen atoms Principal mean square atomic displacements U 0.1044 0.0694 0.0378 C1 0.0600 0.0527 0.0503 C2 0.0523 0.0485 0.0361 C3 0.0638 0.0624 0.0362 C4 0.0582 0.0518 0.0408 C5 0.0500 0.0428 0.0355 C6 0.0707 0.0449 0.0363 C7 0.0645 0.0522 0.0372 C8 0.0509 0.0440 0.0400 C9 0.0676 0.0431 0.0398 C10 0.0978 0.0655 0.0416 C11 0.0963 0.0682 0.0358 C12 0.0697 0.0633 0.0361 C13 0.0510 0.0441 0.0312 C14 0.0890 0.0575 0.0408 C15 0.1566 0.0847 0.0530 C16 0.1081 0.0667 0.0531 C17 0.1630 0.0770 0.0548 C18 0.1265 0.0730 0.0693 C19 0.4041 0.1372 0.0443 C20 may be split into 1.0871 0.1133 1.2137 and 1.0621 0.0950 1.2143 0.2667 0.1179 0.0661 C21 0.2185 0.1181 0.0960 C22 0.0730 0.0471 0.0372 N1 0.0937 0.0548 0.0410 N2 0.0576 0.0473 0.0325 N3 0.0648 0.0542 0.0352 N4 0.1240 0.0823 0.0463 O1 0.0826 0.0757 0.0390 O2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.006 0.011 0.017 0.023 0.030 0.038 0.050 0.067 0.103 1.000 Number in group 321. 329. 313. 286. 309. 312. 300. 309. 312. 306. GooF 0.798 0.875 0.952 0.939 1.042 1.014 1.015 0.930 0.955 0.880 K 4.403 1.134 0.860 0.926 0.930 1.009 1.005 1.014 1.016 1.019 Resolution(A) 0.90 0.93 0.97 1.01 1.07 1.13 1.22 1.34 1.53 1.93 inf Number in group 310. 318. 309. 308. 308. 305. 308. 314. 307. 310. GooF 0.833 0.876 0.878 0.905 0.921 1.002 0.901 0.951 0.996 1.121 K 0.957 0.974 0.999 0.986 1.012 1.035 1.024 1.032 1.062 1.007 R1 0.424 0.355 0.238 0.175 0.146 0.134 0.111 0.092 0.066 0.051 Recommended weighting scheme: WGHT 0.1049 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)/esd Fc/Fc(max) Resolution(A) 0 22 3 142.61 54.26 4.14 0.037 1.16 1 2 0 292.65 481.88 4.04 0.111 6.00 2 3 7 3.03 29.02 3.91 0.027 1.34 0 14 3 71.51 22.37 3.83 0.024 1.71 -2 5 2 23.46 49.56 3.55 0.035 2.81 1 1 2 194.33 135.61 3.31 0.059 3.89 1 1 1 3.88 9.34 3.25 0.015 5.16 4 17 2 121.01 63.69 3.25 0.040 1.09 3 14 4 149.83 92.82 3.23 0.049 1.22 -2 6 1 84.64 53.81 3.21 0.037 2.74 0 6 7 18.99 3.70 3.17 0.010 1.56 -5 16 1 50.44 0.08 3.10 0.001 1.06 5 4 3 33.53 7.67 3.02 0.014 1.16 0 2 3 524.90 818.81 3.01 0.144 3.74 0 7 4 574.67 412.75 3.01 0.102 2.32 1 20 3 -16.74 28.43 2.97 0.027 1.22 -3 1 5 119.20 81.75 2.94 0.046 1.88 2 4 8 -6.30 13.06 2.92 0.018 1.21 0 2 8 80.36 54.83 2.91 0.037 1.45 1 4 1 66.37 95.83 2.90 0.049 4.13 0 8 2 60.45 92.68 2.88 0.049 2.89 0 18 2 105.04 162.44 2.87 0.064 1.43 3 6 5 46.67 21.06 2.84 0.023 1.37 -5 2 6 153.41 225.33 2.81 0.076 1.27 1 5 4 11.10 2.98 2.81 0.009 2.23 -2 22 2 59.71 6.13 2.79 0.012 1.14 3 2 2 26.92 14.26 2.79 0.019 1.91 -4 5 7 72.73 39.66 2.79 0.032 1.33 1 23 5 63.43 19.78 2.79 0.022 1.01 2 1 2 549.59 406.02 2.78 0.102 2.62 -3 16 7 221.75 150.77 2.74 0.062 1.13 1 1 0 37.55 26.80 2.73 0.026 6.51 2 6 0 14.31 28.52 2.73 0.027 2.68 -2 2 4 -4.01 5.79 2.69 0.012 2.51 0 1 3 155.51 219.55 2.68 0.075 3.85 1 19 0 278.82 191.94 2.65 0.070 1.37 -4 5 3 164.41 114.72 2.61 0.054 1.63 -2 2 13 9.19 52.84 2.60 0.037 0.93 0 3 4 1634.11 3005.35 2.58 0.276 2.77 0 0 2 1423.06 1931.76 2.58 0.222 5.84 2 12 5 55.73 32.43 2.57 0.029 1.36 2 14 5 24.88 47.51 2.57 0.035 1.27 -4 15 4 36.09 65.95 2.57 0.041 1.21 -3 19 7 -15.89 20.93 2.56 0.023 1.04 1 10 3 14.92 39.62 2.56 0.032 2.00 -1 8 2 101.13 141.58 2.55 0.060 2.79 2 7 1 378.48 513.75 2.54 0.114 2.37 -4 4 7 -1.36 17.06 2.53 0.021 1.35 2 2 3 144.48 195.96 2.53 0.071 2.23 0 11 5 177.01 123.16 2.44 0.056 1.68 Bond lengths and angles C1 - Distance Angles O2 1.4429 (0.0045) C1 - C2 - Distance Angles O1 1.1982 (0.0047) O2 1.3329 (0.0045) 123.10 (0.40) C3 1.4777 (0.0053) 125.59 (0.38) 111.31 (0.37) C2 - O1 O2 C3 - Distance Angles C4 1.3833 (0.0049) C8 1.3862 (0.0051) 118.56 (0.35) C2 1.4777 (0.0053) 119.30 (0.36) 122.14 (0.35) C3 - C4 C8 C4 - Distance Angles C5 1.3697 (0.0050) C3 1.3833 (0.0049) 120.89 (0.36) C4 - C5 C5 - Distance Angles C4 1.3697 (0.0050) C6 1.3976 (0.0049) 121.06 (0.34) C5 - C4 C6 - Distance Angles C7 1.3899 (0.0047) C5 1.3976 (0.0049) 117.66 (0.34) C9 1.4718 (0.0049) 118.85 (0.32) 123.28 (0.32) C6 - C7 C5 C7 - Distance Angles C8 1.3747 (0.0049) C6 1.3899 (0.0047) 121.10 (0.35) C7 - C8 C8 - Distance Angles C7 1.3747 (0.0049) C3 1.3862 (0.0051) 120.73 (0.34) C8 - C7 C9 - Distance Angles N1 1.3737 (0.0043) C14 1.3791 (0.0046) 111.20 (0.33) C6 1.4718 (0.0049) 118.09 (0.30) 130.68 (0.33) C9 - N1 C14 C10 - Distance Angles N1 1.3080 (0.0046) N2 1.3552 (0.0049) 127.05 (0.33) N3 1.3983 (0.0045) 110.71 (0.34) 122.22 (0.35) C10 - N1 N2 C11 - Distance Angles N2 1.3161 (0.0049) C12 1.4026 (0.0056) 124.47 (0.41) C11 - N2 C12 - Distance Angles C13 1.3349 (0.0053) C11 1.4026 (0.0056) 119.29 (0.39) C12 - C13 C13 - Distance Angles C12 1.3349 (0.0053) N3 1.3588 (0.0045) 118.40 (0.36) C13 - C12 C14 - Distance Angles C9 1.3791 (0.0046) N3 1.3869 (0.0045) 104.61 (0.29) N4 1.3939 (0.0046) 130.68 (0.37) 124.55 (0.31) C14 - C9 N3 C15 - Distance Angles N4 1.5028 (0.0051) C17 1.5223 (0.0056) 108.33 (0.32) C18 1.5301 (0.0058) 109.43 (0.38) 115.14 (0.38) C16 1.5475 (0.0064) 110.86 (0.34) 108.31 (0.39) 104.74 (0.39) C15 - N4 C17 C18 C16 - Distance Angles C15 1.5475 (0.0064) C16 - C17 - Distance Angles C15 1.5223 (0.0056) C17 - C18 - Distance Angles C19 1.5184 (0.0067) C15 1.5301 (0.0058) 126.44 (0.45) C18 - C19 C19 - Distance Angles C20 1.4766 (0.0070) C21 1.5151 (0.0075) 107.00 (0.49) C18 1.5184 (0.0067) 108.62 (0.54) 112.14 (0.49) C22 1.5383 (0.0078) 107.85 (0.53) 111.45 (0.59) 109.61 (0.47) C19 - C20 C21 C18 C20 - Distance Angles C19 1.4766 (0.0070) C20 - C21 - Distance Angles C19 1.5151 (0.0075) C21 - C22 - Distance Angles C19 1.5383 (0.0077) C22 - N1 - Distance Angles C10 1.3080 (0.0046) C9 1.3737 (0.0043) 106.32 (0.30) N1 - C10 N2 - Distance Angles C11 1.3161 (0.0049) C10 1.3552 (0.0049) 115.51 (0.34) N2 - C11 N3 - Distance Angles C13 1.3588 (0.0046) C14 1.3869 (0.0045) 132.80 (0.31) C10 1.3983 (0.0045) 120.04 (0.34) 107.12 (0.29) N3 - C13 C14 N4 - Distance Angles C14 1.3939 (0.0046) C15 1.5028 (0.0051) 118.57 (0.33) N4 - C14 O1 - Distance Angles C2 1.1982 (0.0047) O1 - O2 - Distance Angles C2 1.3329 (0.0045) C1 1.4429 (0.0045) 117.80 (0.34) O2 - C2 FMAP and GRID set by program FMAP 2 2 29 GRID -0.962 -2 -2 0.962 2 2 R1 = 0.1413 for 3097 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.32 at 0.8035 0.1245 0.0554 [ 1.22 A from C19 ] Deepest hole -0.25 at 0.8996 0.1457 0.0864 [ 0.55 A from C18 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 2795 / 17701 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.8035 0.1245 1.0554 1.00000 0.05 0.32 1.22 C19 1.24 C18 1.34 C22 1.52 H22B Q2 1 0.8559 0.2101 1.0293 1.00000 0.05 0.26 1.19 H16A 1.21 C16 1.28 C15 1.39 C18 Q3 1 1.1251 0.1598 1.2237 1.00000 0.05 0.22 1.07 H20C 1.52 C20 1.60 H20B 1.91 H18A Q4 1 1.0046 0.0993 1.2162 1.00000 0.05 0.19 0.51 C20 0.73 H20B 1.05 H20A 1.44 H20C Q5 1 1.1163 0.0523 1.2154 1.00000 0.05 0.18 0.54 H20A 1.41 C20 1.97 H20C 2.05 H21B Q6 1 1.2506 0.1446 1.1220 1.00000 0.05 0.15 1.42 H21C 1.54 H20C 1.69 H18A 2.05 C21 Q7 1 0.3286 0.1058 0.7371 1.00000 0.05 0.15 0.62 C6 0.78 C5 1.46 H5 1.79 C7 Q8 1 0.4008 0.1388 0.9368 1.00000 0.05 0.15 1.40 N4 1.54 H4N 1.67 C14 1.85 H5 Q9 1 0.2697 -0.0567 0.3043 1.00000 0.05 0.15 0.79 H1A 0.97 C1 1.04 H1C 1.82 H1B Q10 1 0.9529 0.0538 1.1751 1.00000 0.05 0.15 1.21 H20A 1.23 H22C 1.59 C20 1.60 C22 Q11 1 0.5876 0.2096 1.0235 1.00000 0.05 0.15 0.95 H4N 1.32 N4 1.86 H13 1.91 H16A Q12 1 0.7687 0.1903 0.7666 1.00000 0.05 0.14 0.70 H17A 1.24 C17 1.43 H17C 2.06 H17B Q13 1 0.2438 0.1675 0.7559 1.00000 0.05 0.14 0.50 C9 1.34 N1 1.43 C6 1.67 C14 Q14 1 0.1878 0.2747 0.7504 1.00000 0.05 0.14 0.71 C10 0.78 N2 1.74 C11 1.80 N3 Q15 1 1.2029 0.0803 1.2442 1.00000 0.05 0.14 0.70 H20A 1.08 C20 1.17 H20C 1.82 H20B Q16 1 0.3939 0.0218 0.7289 1.00000 0.05 0.13 0.48 C4 0.61 H4 1.58 C3 1.68 C5 Q17 1 0.3013 0.1915 0.7195 1.00000 0.05 0.13 0.66 C9 0.93 N1 1.75 C14 1.78 C6 Q18 1 0.1223 0.1773 0.6224 1.00000 0.05 0.13 1.27 N1 1.59 H7 1.84 C9 1.90 C7 Q19 1 1.1551 0.1676 1.0070 1.00000 0.05 0.13 1.22 H18A 1.75 H21C 1.93 C18 2.24 C21 Q20 1 0.2291 0.1928 0.5900 1.00000 0.05 0.13 1.26 H7 1.51 N1 1.86 H16A 1.91 C7 Q21 1 0.2766 -0.1037 0.4424 1.00000 0.05 0.13 1.14 H1C 1.41 H1B 1.53 C1 1.73 H12 Q22 1 0.3600 0.1517 0.7600 1.00000 0.05 0.13 0.70 C9 0.95 C6 1.66 C14 1.90 C5 Q23 1 0.3441 -0.0558 0.7520 1.00000 0.05 0.13 1.65 H4 1.90 H22B 1.90 O1 2.41 H22C Q24 1 0.2633 0.1257 0.7018 1.00000 0.05 0.13 0.38 C6 1.39 C7 1.48 C9 1.51 C5 Q25 1 0.4807 0.2483 1.0362 1.00000 0.05 0.12 0.61 H13 1.31 C13 1.99 N3 2.04 H4N Q26 1 0.3494 0.0715 0.8836 1.00000 0.05 0.12 0.62 H5 1.41 C5 2.25 C4 2.35 H4 Q27 1 1.1336 0.1939 1.1554 1.00000 0.05 0.12 1.19 H18A 1.86 C18 1.87 H18B 2.06 H20C Q28 1 0.3476 -0.0455 0.5838 1.00000 0.05 0.12 0.43 O1 0.94 C2 2.04 O2 2.10 C3 Q29 1 0.9622 0.0743 0.9426 1.00000 0.05 0.12 0.63 H21A 1.27 C21 1.69 H21B 1.93 H17B Q30 1 0.8465 0.2719 0.7794 1.00000 0.05 0.12 1.71 H16B 2.01 N2 2.08 H16C 2.27 C16 Shortest distances between peaks (including symmetry equivalents) 7 24 0.75 13 22 0.90 13 17 0.92 5 15 0.96 18 20 1.01 22 24 1.09 5 10 1.11 17 22 1.19 3 27 1.24 7 22 1.26 11 25 1.30 13 24 1.31 4 10 1.32 4 15 1.42 4 5 1.47 6 19 1.51 17 20 1.52 17 18 1.52 13 18 1.64 6 27 1.65 3 6 1.73 17 24 1.78 7 13 1.78 3 4 1.81 18 24 1.81 2 11 1.85 10 15 1.86 8 26 1.91 7 26 1.96 19 27 1.97 27 30 2.03 23 28 2.06 9 21 2.08 13 20 2.09 8 22 2.11 16 23 2.12 18 22 2.13 2 27 2.17 3 15 2.18 1 4 2.18 20 24 2.22 12 30 2.23 8 19 2.23 21 28 2.26 7 16 2.29 7 17 2.30 20 25 2.30 20 22 2.30 8 13 2.31 18 25 2.33 6 15 2.34 1 2 2.34 3 30 2.36 8 11 2.37 1 29 2.38 16 26 2.38 14 17 2.41 1 10 2.43 2 19 2.45 10 23 2.45 16 28 2.47 14 30 2.49 7 8 2.50 7 18 2.56 24 26 2.57 4 6 2.59 22 26 2.62 9 16 2.65 11 14 2.68 14 25 2.69 1 11 2.69 3 19 2.69 6 8 2.71 1 3 2.77 8 24 2.78 4 23 2.80 11 20 2.82 1 8 2.82 2 25 2.82 19 29 2.83 4 27 2.83 3 5 2.86 13 14 2.88 10 29 2.88 2 20 2.89 6 30 2.89 7 20 2.89 1 19 2.90 8 17 2.90 16 24 2.90 2 3 2.92 1 27 2.95 5 6 2.96 26 29 2.96 13 26 2.98 14 20 2.98 14 18 2.99 Time profile in seconds ----------------------- 0.20: Read and process instructions 0.00: Fit rigid groups 0.02: 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. 2.16: 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 1.58: Structure factors and derivatives 1.88: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.36: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.08: Analysis of variance 0.00: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.08: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 17:05:50 Total CPU time: 6.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++