+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 17:09:23 on 02-Aug-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P2(1)/n CELL 0.71069 11.817 5.983 31.689 90.00 97.34 90.00 ZERR 6.00 0.002 0.0008 0.01 0 0.038 0 LATT 1 SYMM .5-X, .5+Y, .5-Z SFAC C H N S HG UNIT 84 48 12 24 6 V = 2222.09 F(000) = 1500.0 Mu = 10.94 mm-1 Cell Wt = 3198.32 Rho = 2.390 L.S. 4 CONF FMAP 2 PLAN 10 WGHT 0.042700 FVAR 0.63990 HG1 5 0.12840 0.61033 0.18301 11.00000 0.02641 0.01936 = 0.01924 0.00006 -0.00063 0.00537 HG2 5 0.00000 0.00000 0.00000 10.50000 0.02307 0.01725 = 0.01878 0.00388 0.00242 -0.00067 S1 4 0.24724 0.33713 0.21867 11.00000 0.03968 0.02552 = 0.01912 0.00018 -0.00471 0.01303 S2 4 0.35385 -0.04517 0.17654 11.00000 0.02446 0.01744 = 0.01821 0.00373 -0.00075 0.00468 S3 4 0.01348 0.89166 0.14850 11.00000 0.02942 0.02074 = 0.01570 -0.00056 0.00092 0.00627 S4 4 -0.09127 1.26813 0.19276 11.00000 0.02615 0.01857 = 0.02255 0.00225 0.00118 0.00441 S5 4 0.08151 -0.27839 0.04671 11.00000 0.01911 0.01794 = 0.02116 0.00324 -0.00012 0.00004 S6 4 -0.03189 -0.66902 0.08133 11.00000 0.02361 0.01568 = 0.01684 0.00503 0.00021 0.00227 N1 3 0.25212 0.29008 0.13377 11.00000 0.00911 0.02160 = 0.01750 0.00477 -0.00151 -0.00008 N2 3 -0.02418 0.89463 0.23123 11.00000 0.01133 0.02915 = 0.02281 -0.00293 -0.00376 0.00263 N3 3 -0.14929 -0.34265 0.04238 11.00000 0.01040 0.02273 = 0.01490 0.00180 0.00019 0.00024 C1 1 0.28065 0.21129 0.17282 11.00000 0.01996 0.01480 = 0.02220 0.00495 0.00573 -0.00032 C2 1 0.34528 -0.05084 0.12101 11.00000 0.01421 0.01662 = 0.01687 0.00014 0.00025 -0.00634 C3 1 0.38373 -0.21107 0.09524 11.00000 0.01381 0.02925 = 0.02143 0.00200 0.00520 0.00062 AFIX 43 H3 2 0.42091 -0.33823 0.10680 11.00000 -1.20000 AFIX 0 C4 1 0.36581 -0.17867 0.05171 11.00000 0.01482 0.02928 = 0.02881 -0.00351 0.00354 -0.00251 AFIX 43 H4 2 0.39032 -0.28646 0.03378 11.00000 -1.20000 AFIX 0 C5 1 0.31194 0.01180 0.03443 11.00000 0.02393 0.04779 = 0.01378 0.00779 0.00305 -0.00820 AFIX 43 H5 2 0.30160 0.02930 0.00503 11.00000 -1.20000 AFIX 0 C6 1 0.27296 0.17713 0.05952 11.00000 0.01545 0.02378 = 0.01822 0.00274 -0.00184 -0.00935 AFIX 43 H6 2 0.23806 0.30544 0.04748 11.00000 -1.20000 AFIX 0 C7 1 0.28821 0.14385 0.10483 11.00000 0.01509 0.02734 = 0.01569 0.00506 -0.00011 -0.00563 C8 1 -0.02804 0.99823 0.19482 11.00000 0.02307 0.01670 = 0.02449 0.00412 0.00176 0.00690 C9 1 -0.10610 1.24281 0.24648 11.00000 0.01283 0.02098 = 0.01638 -0.00310 -0.00208 0.00302 C10 1 -0.15463 1.39520 0.27225 11.00000 0.01767 0.02132 = 0.03390 -0.01139 -0.00480 -0.00061 AFIX 43 H10 2 -0.17939 1.53538 0.26230 11.00000 -1.20000 AFIX 0 C11 1 -0.16410 1.32632 0.31377 11.00000 0.02100 0.03136 = 0.02561 -0.01566 0.00486 0.00288 AFIX 43 H11 2 -0.19727 1.42268 0.33168 11.00000 -1.20000 AFIX 0 C12 1 -0.12630 1.12209 0.32900 11.00000 0.01977 0.04355 = 0.01235 -0.00143 0.00029 -0.00323 AFIX 43 H12 2 -0.13400 1.08360 0.35692 11.00000 -1.20000 AFIX 0 C13 1 -0.07707 0.97232 0.30384 11.00000 0.02180 0.02993 = 0.02412 0.00374 -0.00718 -0.00036 AFIX 43 H13 2 -0.05090 0.83447 0.31458 11.00000 -1.20000 AFIX 0 C14 1 -0.06705 1.03312 0.26091 11.00000 0.01003 0.02546 = 0.01936 -0.00386 -0.00452 -0.00510 C15 1 -0.04411 -0.41352 0.05447 11.00000 0.04225 0.01359 = 0.01001 -0.00005 0.00776 0.00277 C16 1 -0.18112 -0.68838 0.07528 11.00000 0.02038 0.02217 = 0.00549 -0.00514 -0.00185 -0.00231 C17 1 -0.24957 -0.85423 0.08774 11.00000 0.03208 0.01968 = 0.00972 0.00567 0.00286 0.00324 AFIX 43 H17 2 -0.21775 -0.98121 0.10143 11.00000 -1.20000 AFIX 0 C18 1 -0.36591 -0.83009 0.07972 11.00000 0.03086 0.02935 = 0.01948 -0.00230 0.00948 -0.00759 AFIX 43 H18 2 -0.41259 -0.94165 0.08844 11.00000 -1.20000 AFIX 0 C19 1 -0.41485 -0.64638 0.05925 11.00000 0.02167 0.03720 = 0.02191 -0.01218 -0.00515 -0.00398 AFIX 43 H19 2 -0.49394 -0.63683 0.05391 11.00000 -1.20000 AFIX 0 C20 1 -0.34669 -0.46822 0.04588 11.00000 0.02677 0.02086 = 0.02354 -0.00111 0.00206 0.00880 AFIX 43 H20 2 -0.37890 -0.34045 0.03262 11.00000 -1.20000 AFIX 0 C21 1 -0.22756 -0.49906 0.05411 11.00000 0.02368 0.02386 = 0.01498 -0.00719 0.00592 -0.00145 HKLF 4 Covalent radii and connectivity table for s92 in P2(1)/n C 0.770 H 0.320 N 0.700 S 1.030 HG 1.500 Hg1 - S3 S1 Hg2 - S5 S5_$1 S1 - C1 Hg1 S2 - C2 C1 S3 - C8 Hg1 S4 - C9 C8 S5 - C15 Hg2 S6 - C15 C16 N1 - C1 C7 N2 - C8 C14 N3 - C15 C21 C1 - N1 S1 S2 C2 - C3 C7 S2 C3 - C2 C4 C4 - C3 C5 C5 - C4 C6 C6 - C5 C7 C7 - N1 C2 C6 C8 - N2 S3 S4 C9 - C14 C10 S4 C10 - C9 C11 C11 - C12 C10 C12 - C11 C13 C13 - C12 C14 C14 - C9 N2 C13 C15 - N3 S5 S6 C16 - C17 C21 S6 C17 - C16 C18 C18 - C19 C17 C19 - C18 C20 C20 - C21 C19 C21 - C16 N3 C20 Operators for generating equivalent atoms: $1 -x, -y, -z h k l Fo^2 Sigma Why rejected 0 0 11 4445.00 490.00 observed but should be systematically absent -2 0 17 5922.00 492.00 observed but should be systematically absent -2 0 19 1884.00 337.00 observed but should be systematically absent 0 5 0 2715.00 338.00 observed but should be systematically absent 0 1 0 807.00 94.00 observed but should be systematically absent 8492 Reflections read, of which 218 rejected -9 =< h =< 13, -6 =< k =< 6, -35 =< l =< 34, Max. 2-theta = 49.87 5 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 0 2 0 5068.25 109.27 4 1289.15 1 2 0 7114.51 80.95 7 572.57 2 2 0 8138.09 103.53 6 748.66 1 3 0 31313.79 215.27 7 1320.65 2 3 0 9303.36 196.52 5 2153.74 3 6 0 3643.08 265.71 3 1511.11 -1 0 1 97301.26 304.85 3 24918.85 1 1 1 9887.47 89.48 5 993.04 -2 2 1 13670.03 142.30 7 912.50 -1 2 1 6483.51 90.15 7 1650.58 0 2 1 5217.73 94.03 6 509.89 1 2 1 2743.56 95.37 5 919.56 2 2 1 4184.50 80.59 5 544.35 -3 3 1 2748.04 86.75 6 586.31 -2 3 1 17013.85 172.27 7 920.12 -1 3 1 19095.90 214.19 5 5458.59 0 3 1 22160.19 227.03 6 1213.17 1 3 1 22207.89 170.30 7 990.87 -2 4 1 618.62 37.50 3 733.89 1 4 1 10456.55 121.02 7 677.19 3 4 1 21362.46 345.36 5 2350.25 4 4 1 5908.32 227.80 4 2328.98 -2 5 1 11881.72 285.12 5 1445.53 1 5 1 2554.66 138.83 4 899.27 -4 0 2 44442.88 504.04 2 5647.50 -1 1 2 7229.76 80.67 8 667.01 0 1 2 6321.71 61.35 8 1913.01 1 1 2 16082.56 97.20 6 949.23 6 1 2 19469.42 547.01 2 3831.00 -1 2 2 12997.80 129.03 7 1378.47 0 2 2 1877.87 54.67 7 317.87 -4 3 2 6709.43 189.50 5 1368.33 -2 3 2 8971.16 169.46 6 1815.04 1 3 2 16582.13 115.37 3 9410.44 2 3 2 9044.83 191.77 5 2160.78 4 3 2 8397.43 110.37 7 898.75 0 4 2 18035.61 224.41 6 1486.55 1 4 2 4260.56 102.14 4 2726.55 2 4 2 17227.38 295.05 5 2815.56 -3 0 3 26007.38 356.10 2 2020.50 0 1 3 19761.55 107.05 8 1962.67 1 1 3 2377.77 63.60 4 1592.04 -2 2 3 10380.86 140.20 6 1612.73 -1 2 3 6271.70 138.26 5 2908.77 1 2 3 8160.35 150.57 5 1012.10 2 2 3 42252.75 348.05 5 2310.88 -4 3 3 20456.17 314.46 5 2016.95 -2 3 3 6801.72 143.33 6 723.10 -1 3 3 6390.67 156.26 5 852.07 1 3 3 19917.91 259.84 5 2009.03 ** etc. ** 182 Inconsistent equivalents 3319 Unique reflections, of which 0 suppressed R(int) = 0.1379 R(sigma) = 0.1011 Friedel opposites merged Maximum memory for data reduction = 2342 / 33235 Special position constraints for Hg2 x = 0.0000 y = 0.0000 z = 0.0000 sof = 0.50000 Input constraints retained (at least in part) for sof Default effective X-H distances for T = 20.0 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 = 3084 / 357922 wR2 = 0.0998 before cycle 1 for 3319 data and 286 / 286 parameters GooF = S = 0.940; Restrained GooF = 0.940 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0427 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.63990 0.00126 0.000 OSF Mean shift/esd = 0.003 Maximum = 0.090 for x Hg1 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C9 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3084 / 357922 wR2 = 0.0997 before cycle 2 for 3319 data and 286 / 286 parameters GooF = S = 0.940; Restrained GooF = 0.940 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0427 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.63990 0.00126 0.003 OSF Mean shift/esd = 0.001 Maximum = 0.030 for x Hg1 Max. shift = 0.000 A for C21 Max. dU = 0.000 for C15 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3084 / 357922 wR2 = 0.0997 before cycle 3 for 3319 data and 286 / 286 parameters GooF = S = 0.940; Restrained GooF = 0.940 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0427 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.63990 0.00126 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for U12 S3 Max. shift = 0.000 A for C11 Max. dU = 0.000 for C14 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3084 / 357922 wR2 = 0.0997 before cycle 4 for 3319 data and 286 / 286 parameters GooF = S = 0.940; Restrained GooF = 0.940 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0427 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.63990 0.00126 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for C12 Max. dU = 0.000 for C9 Largest correlation matrix elements 0.518 U33 Hg1 / OSF 0.512 U11 Hg1 / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 0.4209 -0.3382 0.1068 43 0.930 0.000 C3 C2 C4 H4 0.3903 -0.2865 0.0338 43 0.930 0.000 C4 C3 C5 H5 0.3016 0.0293 0.0050 43 0.930 0.000 C5 C4 C6 H6 0.2381 0.3054 0.0475 43 0.930 0.000 C6 C5 C7 H10 -0.1794 1.5354 0.2623 43 0.930 0.000 C10 C9 C11 H11 -0.1973 1.4227 0.3317 43 0.930 0.000 C11 C12 C10 H12 -0.1340 1.0836 0.3569 43 0.930 0.000 C12 C11 C13 H13 -0.0509 0.8345 0.3146 43 0.930 0.000 C13 C12 C14 H17 -0.2177 -0.9812 0.1014 43 0.930 0.000 C17 C16 C18 H18 -0.4126 -0.9416 0.0884 43 0.930 0.000 C18 C19 C17 H19 -0.4939 -0.6368 0.0539 43 0.930 0.000 C19 C18 C20 H20 -0.3789 -0.3404 0.0326 43 0.930 0.000 C20 C21 C19 s92 in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Hg1 0.12840 0.61033 0.18301 1.00000 0.02641 0.01936 0.01924 0.00006 -0.00063 0.00537 0.02198 0.00078 0.00004 0.00007 0.00001 0.00000 0.00029 0.00025 0.00025 0.00017 0.00018 0.00019 0.00016 Hg2 0.00000 0.00000 0.00000 0.50000 0.02307 0.01725 0.01878 0.00388 0.00242 -0.00067 0.01972 0.00000 0.00000 0.00000 0.00000 0.00000 0.00037 0.00032 0.00032 0.00024 0.00026 0.00026 0.00018 S1 0.24724 0.33713 0.21867 1.00000 0.03968 0.02552 0.01912 0.00018 -0.00470 0.01303 0.02884 0.00543 0.00027 0.00048 0.00009 0.00000 0.00190 0.00171 0.00145 0.00114 0.00134 0.00137 0.00072 S2 0.35385 -0.04517 0.17654 1.00000 0.02446 0.01744 0.01821 0.00373 -0.00075 0.00468 0.02034 0.00497 0.00024 0.00044 0.00008 0.00000 0.00162 0.00149 0.00141 0.00105 0.00122 0.00117 0.00063 S3 0.01348 0.89166 0.14850 1.00000 0.02942 0.02074 0.01570 -0.00056 0.00092 0.00627 0.02212 0.00508 0.00024 0.00047 0.00008 0.00000 0.00168 0.00147 0.00135 0.00114 0.00121 0.00129 0.00063 S4 -0.09127 1.26813 0.19276 1.00000 0.02615 0.01857 0.02255 0.00225 0.00118 0.00441 0.02259 0.00503 0.00024 0.00047 0.00008 0.00000 0.00164 0.00150 0.00142 0.00118 0.00122 0.00126 0.00063 S5 0.08151 -0.27839 0.04671 1.00000 0.01911 0.01794 0.02116 0.00324 -0.00012 0.00004 0.01964 0.00479 0.00022 0.00046 0.00008 0.00000 0.00151 0.00145 0.00139 0.00110 0.00115 0.00116 0.00060 S6 -0.03189 -0.66902 0.08133 1.00000 0.02361 0.01568 0.01684 0.00503 0.00021 0.00227 0.01892 0.00484 0.00023 0.00043 0.00008 0.00000 0.00156 0.00146 0.00133 0.00103 0.00117 0.00114 0.00061 N1 0.25212 0.29008 0.13377 1.00000 0.00911 0.02161 0.01750 0.00477 -0.00151 -0.00008 0.01635 0.01494 0.00067 0.00140 0.00026 0.00000 0.00457 0.00473 0.00454 0.00404 0.00366 0.00396 0.00189 N2 -0.02418 0.89463 0.23123 1.00000 0.01133 0.02915 0.02281 -0.00293 -0.00376 0.00263 0.02161 0.01573 0.00071 0.00160 0.00027 0.00000 0.00489 0.00548 0.00503 0.00435 0.00398 0.00412 0.00209 N3 -0.14929 -0.34265 0.04238 1.00000 0.01040 0.02273 0.01490 0.00180 0.00019 0.00024 0.01613 0.01498 0.00069 0.00141 0.00026 0.00000 0.00479 0.00528 0.00450 0.00361 0.00377 0.00393 0.00200 C1 0.28065 0.21129 0.17282 1.00000 0.01996 0.01480 0.02220 0.00495 0.00573 -0.00032 0.01872 0.01911 0.00088 0.00174 0.00032 0.00000 0.00611 0.00561 0.00586 0.00454 0.00484 0.00476 0.00238 C2 0.34528 -0.05084 0.12101 1.00000 0.01421 0.01662 0.01687 0.00014 0.00025 -0.00634 0.01605 0.01808 0.00088 0.00168 0.00032 0.00000 0.00587 0.00603 0.00548 0.00425 0.00465 0.00450 0.00239 C3 0.38373 -0.21107 0.09524 1.00000 0.01381 0.02925 0.02143 0.00200 0.00520 0.00062 0.02124 0.01900 0.00085 0.00194 0.00032 0.00000 0.00594 0.00670 0.00591 0.00490 0.00478 0.00498 0.00251 H3 0.42091 -0.33823 0.10680 1.00000 0.02549 0.00000 0.00000 C4 0.36581 -0.17867 0.05171 1.00000 0.01482 0.02928 0.02881 -0.00351 0.00354 -0.00251 0.02424 0.01926 0.00087 0.00189 0.00035 0.00000 0.00626 0.00712 0.00656 0.00511 0.00515 0.00513 0.00271 H4 0.39032 -0.28646 0.03378 1.00000 0.02908 0.00000 0.00000 C5 0.31194 0.01180 0.03443 1.00000 0.02393 0.04779 0.01378 0.00779 0.00305 -0.00820 0.02845 0.02098 0.00095 0.00206 0.00035 0.00000 0.00679 0.00806 0.00567 0.00555 0.00506 0.00610 0.00284 H5 0.30160 0.02930 0.00503 1.00000 0.03413 0.00000 0.00000 C6 0.27296 0.17713 0.05952 1.00000 0.01545 0.02378 0.01822 0.00274 -0.00184 -0.00936 0.01950 0.01768 0.00086 0.00179 0.00032 0.00000 0.00600 0.00638 0.00568 0.00456 0.00471 0.00479 0.00249 H6 0.23806 0.30544 0.04748 1.00000 0.02340 0.00000 0.00000 C7 0.28821 0.14385 0.10483 1.00000 0.01509 0.02734 0.01569 0.00506 -0.00011 -0.00563 0.01956 0.01899 0.00088 0.00186 0.00032 0.00000 0.00599 0.00676 0.00560 0.00462 0.00470 0.00485 0.00251 C8 -0.02804 0.99823 0.19482 1.00000 0.02307 0.01670 0.02449 0.00412 0.00176 0.00690 0.02153 0.02061 0.00094 0.00185 0.00034 0.00000 0.00651 0.00587 0.00622 0.00490 0.00502 0.00512 0.00251 C9 -0.10610 1.24281 0.24648 1.00000 0.01283 0.02098 0.01638 -0.00310 -0.00208 0.00302 0.01708 0.01775 0.00083 0.00175 0.00030 0.00000 0.00573 0.00622 0.00529 0.00459 0.00442 0.00471 0.00233 C10 -0.15463 1.39520 0.27225 1.00000 0.01767 0.02132 0.03390 -0.01139 -0.00480 -0.00061 0.02500 0.01864 0.00092 0.00199 0.00035 0.00000 0.00622 0.00616 0.00691 0.00526 0.00521 0.00511 0.00264 H10 -0.17939 1.53538 0.26230 1.00000 0.03000 0.00000 0.00000 C11 -0.16410 1.32632 0.31377 1.00000 0.02100 0.03136 0.02561 -0.01566 0.00486 0.00288 0.02582 0.01941 0.00092 0.00198 0.00034 0.00000 0.00651 0.00752 0.00646 0.00506 0.00529 0.00520 0.00283 H11 -0.19727 1.42268 0.33168 1.00000 0.03099 0.00000 0.00000 C12 -0.12630 1.12209 0.32900 1.00000 0.01977 0.04355 0.01235 -0.00143 0.00029 -0.00323 0.02538 0.01967 0.00090 0.00207 0.00033 0.00000 0.00641 0.00793 0.00553 0.00522 0.00491 0.00574 0.00275 H12 -0.13400 1.08360 0.35692 1.00000 0.03045 0.00000 0.00000 C13 -0.07707 0.97232 0.30384 1.00000 0.02180 0.02993 0.02412 0.00374 -0.00718 -0.00036 0.02616 0.01979 0.00094 0.00199 0.00034 0.00000 0.00665 0.00701 0.00632 0.00513 0.00520 0.00537 0.00275 H13 -0.05090 0.83447 0.31458 1.00000 0.03139 0.00000 0.00000 C14 -0.06705 1.03312 0.26091 1.00000 0.01003 0.02546 0.01936 -0.00386 -0.00452 -0.00510 0.01884 0.01799 0.00087 0.00182 0.00032 0.00000 0.00575 0.00663 0.00585 0.00462 0.00467 0.00469 0.00251 C15 -0.04411 -0.41352 0.05447 1.00000 0.04225 0.01359 0.01001 -0.00005 0.00776 0.00277 0.02157 0.01996 0.00102 0.00173 0.00031 0.00000 0.00789 0.00575 0.00519 0.00435 0.00516 0.00527 0.00260 C16 -0.18112 -0.68838 0.07528 1.00000 0.02038 0.02217 0.00549 -0.00514 -0.00185 -0.00231 0.01632 0.01733 0.00087 0.00173 0.00029 0.00000 0.00605 0.00612 0.00488 0.00418 0.00447 0.00485 0.00238 C17 -0.24957 -0.85423 0.08774 1.00000 0.03208 0.01968 0.00972 0.00567 0.00286 0.00324 0.02048 0.01916 0.00095 0.00180 0.00031 0.00000 0.00722 0.00644 0.00519 0.00426 0.00485 0.00513 0.00257 H17 -0.21775 -0.98121 0.10143 1.00000 0.02458 0.00000 0.00000 C18 -0.36591 -0.83009 0.07972 1.00000 0.03086 0.02935 0.01948 -0.00230 0.00948 -0.00759 0.02602 0.02003 0.00099 0.00194 0.00033 0.00000 0.00741 0.00721 0.00589 0.00489 0.00537 0.00555 0.00277 H18 -0.41259 -0.94165 0.08844 1.00000 0.03123 0.00000 0.00000 C19 -0.41485 -0.64638 0.05925 1.00000 0.02167 0.03720 0.02191 -0.01218 -0.00515 -0.00398 0.02761 0.01950 0.00099 0.00203 0.00034 0.00000 0.00659 0.00786 0.00613 0.00539 0.00513 0.00560 0.00287 H19 -0.49394 -0.63683 0.05391 1.00000 0.03313 0.00000 0.00000 C20 -0.34669 -0.46822 0.04588 1.00000 0.02677 0.02086 0.02354 -0.00111 0.00206 0.00880 0.02382 0.01995 0.00094 0.00189 0.00034 0.00000 0.00711 0.00651 0.00615 0.00466 0.00531 0.00514 0.00269 H20 -0.37890 -0.34045 0.03262 1.00000 0.02859 0.00000 0.00000 C21 -0.22756 -0.49906 0.05411 1.00000 0.02368 0.02386 0.01498 -0.00719 0.00592 -0.00145 0.02054 0.01910 0.00092 0.00183 0.00032 0.00000 0.00668 0.00628 0.00547 0.00481 0.00487 0.00541 0.00251 Final Structure Factor Calculation for s92 in P2(1)/n Total number of l.s. parameters = 286 Maximum vector length = 511 Memory required = 2798 / 24017 wR2 = 0.0997 before cycle 5 for 3319 data and 0 / 286 parameters GooF = S = 0.940; Restrained GooF = 0.940 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0427 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0459 for 2601 Fo > 4sig(Fo) and 0.0638 for all 3319 data wR2 = 0.0997, GooF = S = 0.940, Restrained GooF = 0.940 for all data Occupancy sum of asymmetric unit = 31.50 for non-hydrogen and 12.00 for hydrogen atoms Principal mean square atomic displacements U 0.0307 0.0193 0.0159 Hg1 0.0236 0.0216 0.0140 Hg2 0.0504 0.0216 0.0145 S1 0.0275 0.0215 0.0120 S2 0.0333 0.0175 0.0156 S3 0.0285 0.0236 0.0157 S4 0.0246 0.0188 0.0155 S5 0.0247 0.0213 0.0107 S6 0.0252 0.0156 0.0083 N1 0.0320 0.0235 0.0094 N2 0.0231 0.0152 0.0101 N3 0.0255 0.0190 0.0117 C1 0.0225 0.0168 0.0089 C2 0.0298 0.0216 0.0124 C3 0.0327 0.0257 0.0143 C4 0.0522 0.0220 0.0111 C5 0.0321 0.0171 0.0092 C6 0.0320 0.0138 0.0129 C7 0.0277 0.0254 0.0114 C8 0.0249 0.0157 0.0106 C9 0.0436 0.0196 0.0118 C10 0.0447 0.0222 0.0106 C11 0.0440 0.0201 0.0120 C12 0.0363 0.0285 0.0137 C13 0.0275 0.0233 0.0057 C14 0.0427 0.0134 0.0086 C15 0.0240 0.0214 0.0036 C16 0.0329 0.0214 0.0071 C17 0.0390 0.0235 0.0156 C18 0.0441 0.0286 0.0102 C19 0.0337 0.0234 0.0144 C20 0.0289 0.0226 0.0101 C21 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.032 0.054 0.078 0.105 0.132 0.164 0.200 0.256 0.329 1.000 Number in group 346. 322. 337. 340. 322. 326. 335. 326. 333. 332. GooF 0.802 0.524 0.544 0.669 0.773 0.913 0.937 1.055 1.053 1.628 K 5.114 1.521 0.995 1.046 1.045 1.032 1.039 1.026 1.011 1.039 Resolution(A) 0.84 0.91 0.95 0.99 1.05 1.12 1.20 1.32 1.51 1.89 inf Number in group 342. 327. 330. 341. 330. 327. 332. 327. 331. 332. GooF 0.733 0.761 0.814 0.672 0.724 0.796 0.867 0.908 1.127 1.618 K 1.003 1.004 1.013 1.027 1.041 1.041 1.038 1.049 1.027 1.055 R1 0.081 0.069 0.074 0.053 0.050 0.064 0.055 0.065 0.059 0.070 Recommended weighting scheme: WGHT 0.0422 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) -8 5 6 8352.15 131.87 7.41 0.021 0.93 1 0 5 337578.38 258221.50 7.11 0.951 5.27 -1 0 7 102189.31 76858.53 6.99 0.519 4.38 3 0 3 14406.24 21388.80 6.79 0.274 3.52 5 0 3 25386.15 35343.47 5.89 0.352 2.23 2 0 10 84327.43 66793.23 5.38 0.484 2.63 -3 0 5 15588.24 21192.35 5.02 0.272 3.53 2 0 4 203580.03 168806.08 4.84 0.769 4.43 -2 0 8 59207.48 47484.91 4.82 0.408 3.47 6 0 6 76131.58 94736.65 4.65 0.576 1.76 -1 1 13 5284.71 6633.51 4.57 0.152 2.25 -3 6 7 2840.22 102.42 4.56 0.019 0.95 2 6 7 2679.04 39.09 4.32 0.012 0.96 4 0 2 49455.98 60752.73 4.29 0.461 2.82 7 0 5 33840.87 43325.59 4.26 0.389 1.57 1 0 21 164620.44 137573.73 4.13 0.694 1.46 -4 0 14 227022.25 192075.03 4.06 0.820 1.90 0 3 2 65564.05 55484.87 3.77 0.441 1.98 1 0 15 124893.99 106914.67 3.64 0.612 2.02 2 6 4 2748.24 403.87 3.59 0.038 0.97 -1 0 3 11757.88 9371.46 3.54 0.181 8.36 1 3 1 54235.00 44210.88 3.53 0.393 1.96 -3 0 13 192243.59 166506.38 3.48 0.763 2.18 1 0 1 5638.44 6981.12 3.48 0.156 10.55 4 0 14 238727.47 207541.63 3.43 0.852 1.68 1 3 4 68206.95 58489.57 3.43 0.452 1.90 -2 0 6 107838.01 93877.58 3.39 0.573 4.18 -1 6 15 15348.91 10109.52 3.38 0.188 0.90 -8 1 19 22575.00 17880.58 3.35 0.250 1.15 3 1 12 85818.59 74518.48 3.34 0.511 1.95 0 3 1 54118.51 43393.73 3.34 0.390 1.99 1 1 6 14717.62 11726.99 3.32 0.203 3.63 -4 1 6 14468.42 17161.76 3.32 0.245 2.47 4 2 7 61231.34 52657.39 3.28 0.429 1.83 6 0 2 71518.36 83684.34 3.27 0.541 1.91 -4 1 21 27584.54 32122.03 3.21 0.335 1.37 5 3 12 51595.48 42462.93 3.14 0.386 1.27 -1 2 17 40334.55 33937.70 3.10 0.345 1.58 2 1 7 219130.89 182195.14 3.09 0.799 2.93 4 3 4 33272.55 27901.65 3.07 0.313 1.59 1 0 27 134333.36 103239.05 3.06 0.601 1.14 -8 0 22 92301.05 77444.43 3.03 0.521 1.10 3 4 12 1523.68 12.95 3.02 0.007 1.21 -1 0 5 18484.63 15784.47 2.99 0.235 5.86 1 2 8 13939.97 11977.99 2.97 0.205 2.30 2 4 6 25376.15 31338.73 2.95 0.331 1.39 3 3 2 13632.94 17791.73 2.94 0.250 1.75 5 1 5 13130.31 15567.35 2.91 0.233 1.99 3 4 17 94819.27 82432.71 2.89 0.537 1.09 -4 1 24 28600.06 33465.21 2.87 0.342 1.23 Selected torsion angles -121.33 ( 3.16) S3 - Hg1 - S1 - C1 -63.70 ( 3.24) S1 - Hg1 - S3 - C8 -27.48 (99.99) S5_$1 - Hg2 - S5 - C15 -177.57 ( 0.77) C7 - N1 - C1 - S1 0.32 ( 1.14) C7 - N1 - C1 - S2 7.71 ( 0.96) Hg1 - S1 - C1 - N1 -170.11 ( 0.56) Hg1 - S1 - C1 - S2 -0.45 ( 0.86) C2 - S2 - C1 - N1 177.56 ( 0.69) C2 - S2 - C1 - S1 -178.82 ( 1.06) C1 - S2 - C2 - C3 0.42 ( 0.79) C1 - S2 - C2 - C7 0.23 ( 1.61) C7 - C2 - C3 - C4 179.37 ( 0.82) S2 - C2 - C3 - C4 0.91 ( 1.61) C2 - C3 - C4 - C5 -0.45 ( 1.72) C3 - C4 - C5 - C6 -1.11 ( 1.62) C4 - C5 - C6 - C7 0.04 ( 1.31) C1 - N1 - C7 - C2 -179.21 ( 0.97) C1 - N1 - C7 - C6 178.93 ( 0.95) C3 - C2 - C7 - N1 -0.36 ( 1.19) S2 - C2 - C7 - N1 -1.76 ( 1.57) C3 - C2 - C7 - C6 178.94 ( 0.76) S2 - C2 - C7 - C6 -178.61 ( 0.98) C5 - C6 - C7 - N1 2.14 ( 1.48) C5 - C6 - C7 - C2 -178.81 ( 0.84) C14 - N2 - C8 - S3 -3.20 ( 1.18) C14 - N2 - C8 - S4 -20.10 ( 1.06) Hg1 - S3 - C8 - N2 164.38 ( 0.60) Hg1 - S3 - C8 - S4 3.33 ( 0.91) C9 - S4 - C8 - N2 179.33 ( 0.72) C9 - S4 - C8 - S3 -2.31 ( 0.81) C8 - S4 - C9 - C14 -178.71 ( 1.05) C8 - S4 - C9 - C10 -0.88 ( 1.57) C14 - C9 - C10 - C11 175.08 ( 0.83) S4 - C9 - C10 - C11 1.11 ( 1.61) C9 - C10 - C11 - C12 -0.34 ( 1.76) C10 - C11 - C12 - C13 -0.68 ( 1.67) C11 - C12 - C13 - C14 177.77 ( 0.95) C10 - C9 - C14 - N2 1.13 ( 1.18) S4 - C9 - C14 - N2 -0.09 ( 1.58) C10 - C9 - C14 - C13 -176.72 ( 0.78) S4 - C9 - C14 - C13 1.31 ( 1.32) C8 - N2 - C14 - C9 179.02 ( 1.03) C8 - N2 - C14 - C13 0.88 ( 1.54) C12 - C13 - C14 - C9 -176.78 ( 1.02) C12 - C13 - C14 - N2 179.50 ( 0.75) C21 - N3 - C15 - S5 -0.96 ( 1.10) C21 - N3 - C15 - S6 -10.18 ( 0.95) Hg2 - S5 - C15 - N3 170.29 ( 0.50) Hg2 - S5 - C15 - S6 1.11 ( 0.82) C16 - S6 - C15 - N3 -179.30 ( 0.62) C16 - S6 - C15 - S5 178.71 ( 1.01) C15 - S6 - C16 - C17 -0.89 ( 0.74) C15 - S6 - C16 - C21 -1.11 ( 1.52) C21 - C16 - C17 - C18 179.33 ( 0.81) S6 - C16 - C17 - C18 0.73 ( 1.60) C16 - C17 - C18 - C19 -1.13 ( 1.68) C17 - C18 - C19 - C20 1.80 ( 1.57) C18 - C19 - C20 - C21 -179.05 ( 0.90) C17 - C16 - C21 - N3 0.58 ( 1.10) S6 - C16 - C21 - N3 1.92 ( 1.53) C17 - C16 - C21 - C20 -178.44 ( 0.81) S6 - C16 - C21 - C20 0.22 ( 1.24) C15 - N3 - C21 - C16 179.22 ( 0.95) C15 - N3 - C21 - C20 -2.18 ( 1.50) C19 - C20 - C21 - C16 178.87 ( 0.91) C19 - C20 - C21 - N3 FMAP and GRID set by program FMAP 2 3 34 GRID -0.806 -2 -2 0.806 2 2 R1 = 0.0617 for 3319 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 2.08 at 0.2477 0.5033 0.1365 [ 1.28 A from N1 ] Deepest hole -1.57 at 0.1545 0.6114 0.2202 [ 1.18 A from HG1 ] Mean = 0.00, Rms deviation from mean = 0.27 e/A^3, Highest memory used = 2552 / 18351 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2477 0.5033 0.1365 1.00000 0.05 2.08 1.28 N1 2.10 C1 2.26 HG1 2.45 C7 Q2 1 -0.0822 0.0129 0.0086 1.00000 0.05 1.75 1.04 HG2 2.37 S5 2.55 N3 2.59 H5 Q3 1 0.4570 -0.3961 0.0417 1.00000 0.05 1.54 1.03 H4 1.58 H19 1.74 C4 2.02 H20 Q4 1 0.0535 0.5690 0.1914 1.00000 0.05 1.33 0.99 HG1 2.37 S3 2.49 S4 2.56 N2 Q5 1 0.2142 0.6091 0.1752 1.00000 0.05 1.31 1.07 HG1 2.13 S1 2.39 N1 2.51 C1 Q6 1 0.0838 -0.0676 0.0322 1.00000 0.05 1.17 1.34 S5 1.39 HG2 2.71 C15 2.72 C6 Q7 1 0.0600 -0.0954 0.0254 1.00000 0.05 1.14 1.15 HG2 1.29 S5 2.50 C15 2.99 N3 Q8 1 0.1109 -0.0077 0.0418 1.00000 0.05 1.14 1.67 S5 1.74 HG2 2.22 C6 2.39 H6 Q9 1 0.0653 0.0961 0.0291 1.00000 0.05 1.13 1.26 HG2 2.31 S5 2.40 H6 2.55 S6 Q10 1 0.2558 -0.2929 0.1399 1.00000 0.05 1.10 1.93 C2 2.13 S2 2.24 HG1 2.25 C3 Shortest distances between peaks (including symmetry equivalents) 6 7 0.37 6 8 0.55 8 9 0.88 7 8 0.91 6 9 1.00 7 9 1.15 1 10 1.23 2 7 1.24 2 6 1.33 2 9 1.40 5 10 1.41 1 5 1.48 2 8 1.59 2 7 1.82 2 9 1.85 4 5 2.04 2 6 2.06 2 2 2.09 7 9 2.13 7 7 2.31 2 8 2.39 6 9 2.46 9 9 2.52 6 7 2.53 6 6 2.78 7 8 2.81 8 9 2.91 Time profile in seconds ----------------------- 0.17: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.02: Analyse other restraints etc. 1.16: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.38: Structure factors and derivatives 2.47: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.56: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.13: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 17:09:30 Total CPU time: 6.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++