+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 97src139 started at 15:44:26 on 13-Sep-2006 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P2(1)/n CELL 0.71069 11.8170 5.9830 31.6890 90.000 97.340 90.000 ZERR 6.00 0.0020 0.0008 0.0100 0.000 0.038 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - 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 MERG 2 FMAP 2 PLAN 10 ACTA BOND $H CONF WGHT 0.04210 L.S. 4 FVAR 0.06398 HG1 5 0.128404 0.610332 0.183009 11.00000 0.02640 0.01936 = 0.01923 0.00007 -0.00064 0.00537 HG2 5 0.000000 0.000000 0.000000 10.50000 0.02307 0.01725 = 0.01877 0.00388 0.00242 -0.00067 S1 4 0.247231 0.337124 0.218667 11.00000 0.03962 0.02551 = 0.01914 0.00020 -0.00471 0.01303 S2 4 0.353852 -0.045174 0.176545 11.00000 0.02446 0.01744 = 0.01822 0.00374 -0.00075 0.00468 S3 4 0.013484 0.891682 0.148505 11.00000 0.02950 0.02073 = 0.01570 -0.00055 0.00090 0.00626 S4 4 -0.091273 1.268128 0.192757 11.00000 0.02610 0.01857 = 0.02256 0.00230 0.00119 0.00441 S5 4 0.081511 -0.278389 0.046706 11.00000 0.01911 0.01794 = 0.02117 0.00323 -0.00014 0.00006 S6 4 -0.031884 -0.669024 0.081327 11.00000 0.02362 0.01568 = 0.01684 0.00502 0.00022 0.00227 N1 3 0.252120 0.290047 0.133768 11.00000 0.00901 0.02141 = 0.01754 0.00488 -0.00150 -0.00009 N2 3 -0.024168 0.894651 0.231234 11.00000 0.01086 0.02880 = 0.02300 -0.00293 -0.00380 0.00263 N3 3 -0.149282 -0.342655 0.042375 11.00000 0.00962 0.02255 = 0.01522 0.00198 0.00021 -0.00010 C1 1 0.280642 0.211300 0.172826 11.00000 0.02018 0.01472 = 0.02220 0.00517 0.00572 -0.00028 C2 1 0.345334 -0.050956 0.120996 11.00000 0.01404 0.01641 = 0.01707 0.00021 0.00023 -0.00633 C3 1 0.383732 -0.211050 0.095241 11.00000 0.01383 0.02914 = 0.02139 0.00179 0.00539 0.00055 AFIX 43 H3 2 0.420911 -0.338211 0.106801 11.00000 -1.20000 AFIX 0 C4 1 0.365808 -0.178708 0.051721 11.00000 0.01482 0.02912 = 0.02890 -0.00372 0.00348 -0.00268 AFIX 43 H4 2 0.390274 -0.286550 0.033785 11.00000 -1.20000 AFIX 0 C5 1 0.311957 0.011907 0.034434 11.00000 0.02388 0.04831 = 0.01351 0.00798 0.00295 -0.00819 AFIX 43 H5 2 0.301578 0.029442 0.005032 11.00000 -1.20000 AFIX 0 C6 1 0.273120 0.177048 0.059526 11.00000 0.01514 0.02337 = 0.01839 0.00341 -0.00175 -0.00920 AFIX 43 H6 2 0.238350 0.305475 0.047478 11.00000 -1.20000 AFIX 0 C7 1 0.288206 0.143875 0.104830 11.00000 0.01507 0.02755 = 0.01571 0.00500 -0.00019 -0.00553 C8 1 -0.028033 0.998230 0.194817 11.00000 0.02321 0.01653 = 0.02441 0.00403 0.00158 0.00695 C9 1 -0.106103 1.242801 0.246475 11.00000 0.01289 0.02090 = 0.01577 -0.00340 -0.00212 0.00278 C10 1 -0.154582 1.395175 0.272260 11.00000 0.01774 0.02061 = 0.03379 -0.01133 -0.00484 -0.00055 AFIX 43 H10 2 -0.179300 1.535390 0.262314 11.00000 -1.20000 AFIX 0 C11 1 -0.164088 1.326348 0.313777 11.00000 0.02098 0.03123 = 0.02561 -0.01568 0.00491 0.00287 AFIX 43 H11 2 -0.197255 1.422707 0.331686 11.00000 -1.20000 AFIX 0 C12 1 -0.126286 1.122074 0.328993 11.00000 0.01973 0.04335 = 0.01243 -0.00138 0.00036 -0.00353 AFIX 43 H12 2 -0.134001 1.083529 0.356913 11.00000 -1.20000 AFIX 0 C13 1 -0.077053 0.972350 0.303834 11.00000 0.02178 0.02971 = 0.02425 0.00371 -0.00711 -0.00006 AFIX 43 H13 2 -0.050864 0.834510 0.314578 11.00000 -1.20000 AFIX 0 C14 1 -0.067043 1.033112 0.260905 11.00000 0.01004 0.02510 = 0.01928 -0.00389 -0.00454 -0.00508 C15 1 -0.044113 -0.413533 0.054462 11.00000 0.04276 0.01257 = 0.00999 0.00013 0.00804 0.00266 C16 1 -0.181125 -0.688399 0.075280 11.00000 0.02012 0.02212 = 0.00560 -0.00515 -0.00189 -0.00252 C17 1 -0.249626 -0.854241 0.087742 11.00000 0.03214 0.01962 = 0.00960 0.00565 0.00257 0.00332 AFIX 43 H17 2 -0.217838 -0.981212 0.101438 11.00000 -1.20000 AFIX 0 C18 1 -0.365900 -0.830072 0.079698 11.00000 0.03080 0.02933 = 0.01954 -0.00234 0.00969 -0.00752 AFIX 43 H18 2 -0.412569 -0.941683 0.088397 11.00000 -1.20000 AFIX 0 C19 1 -0.414874 -0.646461 0.059257 11.00000 0.02179 0.03625 = 0.02215 -0.01213 -0.00510 -0.00422 AFIX 43 H19 2 -0.493964 -0.636899 0.053943 11.00000 -1.20000 AFIX 0 C20 1 -0.346731 -0.468315 0.045844 11.00000 0.02648 0.02087 = 0.02353 -0.00117 0.00194 0.00878 AFIX 43 H20 2 -0.378955 -0.340651 0.032550 11.00000 -1.20000 AFIX 0 C21 1 -0.227544 -0.499065 0.054109 11.00000 0.02369 0.02297 = 0.01520 -0.00731 0.00614 -0.00142 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_$1 S5 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 - C6 C4 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 44.45 4.90 observed but should be systematically absent -2 0 17 59.22 4.92 observed but should be systematically absent -2 0 19 18.84 3.37 observed but should be systematically absent 0 5 0 27.15 3.38 observed but should be systematically absent 0 1 0 8.07 0.94 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 50.68 1.09 4 12.89 1 2 0 71.15 0.81 7 5.73 2 2 0 81.38 1.04 6 7.49 1 3 0 313.14 2.15 7 13.21 2 3 0 93.03 1.97 5 21.54 3 6 0 36.43 2.66 3 15.11 -1 0 1 973.01 3.05 3 249.19 1 1 1 98.87 0.89 5 9.93 -2 2 1 136.70 1.42 7 9.13 -1 2 1 64.84 0.90 7 16.51 0 2 1 52.18 0.94 6 5.10 1 2 1 27.44 0.95 5 9.20 2 2 1 41.85 0.81 5 5.44 -3 3 1 27.48 0.87 6 5.86 -2 3 1 170.14 1.72 7 9.20 -1 3 1 190.96 2.14 5 54.59 0 3 1 221.60 2.27 6 12.13 1 3 1 222.08 1.70 7 9.91 -2 4 1 6.19 0.37 3 7.34 1 4 1 104.57 1.21 7 6.77 3 4 1 213.62 3.45 5 23.50 4 4 1 59.08 2.28 4 23.29 -2 5 1 118.82 2.85 5 14.46 1 5 1 25.55 1.39 4 8.99 -4 0 2 444.43 5.04 2 56.48 -1 1 2 72.30 0.81 8 6.67 0 1 2 63.22 0.61 8 19.13 1 1 2 160.83 0.97 6 9.49 6 1 2 194.69 5.47 2 38.31 -1 2 2 129.98 1.29 7 13.78 0 2 2 18.78 0.55 7 3.18 -4 3 2 67.09 1.90 5 13.68 -2 3 2 89.71 1.69 6 18.15 1 3 2 165.82 1.15 3 94.10 2 3 2 90.45 1.92 5 21.61 4 3 2 83.97 1.10 7 8.99 0 4 2 180.36 2.24 6 14.87 1 4 2 42.61 1.02 4 27.27 2 4 2 172.27 2.95 5 28.16 -3 0 3 260.07 3.56 2 20.20 0 1 3 197.62 1.07 8 19.63 1 1 3 23.78 0.64 4 15.92 -2 2 3 103.81 1.40 6 16.13 -1 2 3 62.72 1.38 5 29.09 1 2 3 81.60 1.51 5 10.12 2 2 3 422.53 3.48 5 23.11 -4 3 3 204.56 3.14 5 20.17 -2 3 3 68.02 1.43 6 7.23 -1 3 3 63.91 1.56 5 8.52 1 3 3 199.18 2.60 5 20.09 ** 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 = 2809 / 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 = 3551 / 357922 wR2 = 0.0997 before cycle 1 for 3319 data and 286 / 286 parameters GooF = S = 0.944; Restrained GooF = 0.944 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0421 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.06400 0.00013 0.124 OSF Mean shift/esd = 0.016 Maximum = -0.141 for x C6 Max. shift = 0.001 A for C6 Max. dU = 0.000 for C10 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3551 / 357922 wR2 = 0.0997 before cycle 2 for 3319 data and 286 / 286 parameters GooF = S = 0.944; Restrained GooF = 0.944 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0421 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.06400 0.00013 0.018 OSF Mean shift/esd = 0.005 Maximum = -0.042 for x C6 Max. shift = 0.000 A for C6 Max. dU = 0.000 for C21 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3551 / 357922 wR2 = 0.0996 before cycle 3 for 3319 data and 286 / 286 parameters GooF = S = 0.944; Restrained GooF = 0.944 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0421 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.06400 0.00013 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.003 for y C6 Max. shift = 0.000 A for C6 Max. dU = 0.000 for C21 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3551 / 357922 wR2 = 0.0996 before cycle 4 for 3319 data and 286 / 286 parameters GooF = S = 0.944; Restrained GooF = 0.944 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0421 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.06400 0.00013 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for U11 C6 Max. shift = 0.000 A for C19 Max. dU = 0.000 for C6 Largest correlation matrix elements 0.518 U33 Hg1 / OSF 0.511 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 C6 C4 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 -0.9417 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 0.02642 0.01936 0.01925 0.00006 -0.00063 0.00537 0.02199 0.00078 0.00004 0.00007 0.00001 0.00000 0.00029 0.00025 0.00025 0.00017 0.00019 0.00019 0.00016 Hg2 0.00000 0.00000 0.00000 0.50000 0.02308 0.01725 0.01879 0.00388 0.00242 -0.00067 0.01973 0.00000 0.00000 0.00000 0.00000 0.00000 0.00037 0.00032 0.00033 0.00024 0.00026 0.00026 0.00018 S1 0.24724 0.33713 0.21867 1.00000 0.03969 0.02551 0.01914 0.00019 -0.00471 0.01303 0.02884 0.00544 0.00027 0.00048 0.00009 0.00000 0.00190 0.00171 0.00145 0.00115 0.00135 0.00137 0.00072 S2 0.35385 -0.04517 0.17654 1.00000 0.02446 0.01745 0.01821 0.00374 -0.00075 0.00468 0.02034 0.00497 0.00024 0.00044 0.00008 0.00000 0.00163 0.00149 0.00141 0.00105 0.00122 0.00117 0.00063 S3 0.01348 0.89166 0.14850 1.00000 0.02943 0.02074 0.01570 -0.00056 0.00092 0.00627 0.02212 0.00509 0.00024 0.00047 0.00008 0.00000 0.00169 0.00147 0.00135 0.00114 0.00121 0.00130 0.00063 S4 -0.09127 1.26813 0.19276 1.00000 0.02615 0.01858 0.02255 0.00225 0.00119 0.00442 0.02259 0.00504 0.00024 0.00047 0.00008 0.00000 0.00164 0.00150 0.00143 0.00118 0.00123 0.00126 0.00063 S5 0.08151 -0.27839 0.04671 1.00000 0.01911 0.01794 0.02117 0.00323 -0.00014 0.00005 0.01964 0.00479 0.00022 0.00046 0.00008 0.00000 0.00151 0.00146 0.00139 0.00110 0.00116 0.00116 0.00060 S6 -0.03188 -0.66903 0.08133 1.00000 0.02362 0.01568 0.01684 0.00502 0.00022 0.00228 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 0.29007 0.13377 1.00000 0.00907 0.02158 0.01749 0.00478 -0.00150 -0.00004 0.01632 0.01495 0.00067 0.00140 0.00026 0.00000 0.00458 0.00473 0.00455 0.00405 0.00366 0.00396 0.00189 N2 -0.02419 0.89463 0.23123 1.00000 0.01130 0.02920 0.02283 -0.00292 -0.00380 0.00261 0.02163 0.01575 0.00071 0.00160 0.00027 0.00000 0.00490 0.00549 0.00504 0.00436 0.00398 0.00412 0.00210 N3 -0.14929 -0.34265 0.04238 1.00000 0.01030 0.02272 0.01492 0.00181 0.00013 0.00024 0.01611 0.01499 0.00069 0.00141 0.00026 0.00000 0.00479 0.00529 0.00451 0.00362 0.00377 0.00394 0.00200 C1 0.28065 0.21128 0.17282 1.00000 0.01996 0.01477 0.02223 0.00493 0.00573 -0.00033 0.01872 0.01912 0.00088 0.00174 0.00032 0.00000 0.00612 0.00562 0.00587 0.00454 0.00485 0.00476 0.00239 C2 0.34527 -0.05084 0.12101 1.00000 0.01417 0.01660 0.01690 0.00015 0.00020 -0.00635 0.01605 0.01809 0.00088 0.00168 0.00032 0.00000 0.00588 0.00604 0.00549 0.00426 0.00466 0.00451 0.00240 C3 0.38373 -0.21106 0.09524 1.00000 0.01379 0.02928 0.02137 0.00199 0.00520 0.00064 0.02123 0.01901 0.00085 0.00194 0.00032 0.00000 0.00595 0.00671 0.00592 0.00490 0.00479 0.00498 0.00251 H3 0.42091 -0.33821 0.10680 1.00000 0.02547 0.00000 0.00000 C4 0.36581 -0.17867 0.05172 1.00000 0.01478 0.02929 0.02891 -0.00352 0.00351 -0.00249 0.02427 0.01928 0.00087 0.00189 0.00035 0.00000 0.00627 0.00713 0.00657 0.00512 0.00516 0.00514 0.00271 H4 0.39032 -0.28646 0.03378 1.00000 0.02912 0.00000 0.00000 C5 0.31195 0.01180 0.03444 1.00000 0.02395 0.04785 0.01372 0.00783 0.00300 -0.00821 0.02845 0.02099 0.00095 0.00206 0.00035 0.00000 0.00680 0.00807 0.00568 0.00556 0.00507 0.00611 0.00285 H5 0.30161 0.02929 0.00503 1.00000 0.03414 0.00000 0.00000 C6 0.27296 0.17714 0.05952 1.00000 0.01544 0.02375 0.01821 0.00272 -0.00183 -0.00936 0.01948 0.01769 0.00086 0.00179 0.00032 0.00000 0.00600 0.00639 0.00569 0.00456 0.00472 0.00479 0.00250 H6 0.23808 0.30545 0.04747 1.00000 0.02337 0.00000 0.00000 C7 0.28821 0.14387 0.10483 1.00000 0.01506 0.02738 0.01569 0.00508 -0.00013 -0.00564 0.01956 0.01901 0.00088 0.00186 0.00032 0.00000 0.00599 0.00677 0.00561 0.00462 0.00470 0.00486 0.00251 C8 -0.02802 0.99822 0.19482 1.00000 0.02312 0.01668 0.02452 0.00411 0.00176 0.00690 0.02155 0.02063 0.00094 0.00185 0.00034 0.00000 0.00652 0.00587 0.00623 0.00491 0.00503 0.00513 0.00251 C9 -0.10609 1.24282 0.24648 1.00000 0.01284 0.02100 0.01633 -0.00311 -0.00209 0.00305 0.01707 0.01777 0.00083 0.00175 0.00030 0.00000 0.00574 0.00624 0.00530 0.00459 0.00443 0.00472 0.00234 C10 -0.15463 1.39519 0.27226 1.00000 0.01770 0.02129 0.03396 -0.01139 -0.00481 -0.00062 0.02502 0.01865 0.00092 0.00200 0.00035 0.00000 0.00623 0.00617 0.00692 0.00527 0.00521 0.00512 0.00265 H10 -0.17939 1.53537 0.26231 1.00000 0.03002 0.00000 0.00000 C11 -0.16409 1.32631 0.31377 1.00000 0.02100 0.03132 0.02562 -0.01566 0.00490 0.00287 0.02581 0.01942 0.00092 0.00198 0.00034 0.00000 0.00652 0.00753 0.00647 0.00507 0.00530 0.00520 0.00284 H11 -0.19725 1.42268 0.33168 1.00000 0.03098 0.00000 0.00000 C12 -0.12629 1.12209 0.32900 1.00000 0.01975 0.04354 0.01229 -0.00145 0.00028 -0.00324 0.02535 0.01968 0.00090 0.00207 0.00033 0.00000 0.00641 0.00794 0.00553 0.00522 0.00491 0.00575 0.00275 H12 -0.13399 1.08359 0.35693 1.00000 0.03042 0.00000 0.00000 C13 -0.07707 0.97235 0.30384 1.00000 0.02177 0.02989 0.02420 0.00375 -0.00720 -0.00038 0.02616 0.01981 0.00094 0.00199 0.00034 0.00000 0.00666 0.00702 0.00633 0.00514 0.00521 0.00538 0.00275 H13 -0.05089 0.83450 0.31458 1.00000 0.03140 0.00000 0.00000 C14 -0.06705 1.03312 0.26090 1.00000 0.01005 0.02544 0.01933 -0.00387 -0.00456 -0.00512 0.01883 0.01800 0.00087 0.00182 0.00032 0.00000 0.00576 0.00664 0.00586 0.00462 0.00468 0.00470 0.00251 C15 -0.04411 -0.41353 0.05447 1.00000 0.04251 0.01353 0.00996 -0.00005 0.00783 0.00277 0.02161 0.01999 0.00102 0.00174 0.00031 0.00000 0.00792 0.00575 0.00519 0.00435 0.00517 0.00528 0.00261 C16 -0.18113 -0.68837 0.07528 1.00000 0.02035 0.02216 0.00547 -0.00515 -0.00186 -0.00231 0.01630 0.01734 0.00087 0.00174 0.00029 0.00000 0.00606 0.00613 0.00488 0.00418 0.00448 0.00486 0.00238 C17 -0.24957 -0.85423 0.08774 1.00000 0.03209 0.01972 0.00969 0.00569 0.00288 0.00327 0.02048 0.01918 0.00095 0.00180 0.00031 0.00000 0.00723 0.00645 0.00520 0.00426 0.00486 0.00514 0.00258 H17 -0.21775 -0.98122 0.10142 1.00000 0.02458 0.00000 0.00000 C18 -0.36590 -0.83009 0.07972 1.00000 0.03087 0.02934 0.01950 -0.00232 0.00949 -0.00760 0.02603 0.02005 0.00099 0.00195 0.00033 0.00000 0.00742 0.00723 0.00590 0.00490 0.00538 0.00556 0.00277 H18 -0.41257 -0.94165 0.08844 1.00000 0.03123 0.00000 0.00000 C19 -0.41486 -0.64639 0.05926 1.00000 0.02169 0.03718 0.02191 -0.01219 -0.00515 -0.00401 0.02762 0.01951 0.00099 0.00204 0.00034 0.00000 0.00660 0.00788 0.00614 0.00540 0.00514 0.00561 0.00287 H19 -0.49395 -0.63685 0.05391 1.00000 0.03314 0.00000 0.00000 C20 -0.34668 -0.46821 0.04587 1.00000 0.02677 0.02087 0.02351 -0.00113 0.00204 0.00880 0.02382 0.01996 0.00094 0.00189 0.00034 0.00000 0.00712 0.00652 0.00616 0.00467 0.00532 0.00515 0.00270 H20 -0.37889 -0.34044 0.03261 1.00000 0.02858 0.00000 0.00000 C21 -0.22755 -0.49908 0.05411 1.00000 0.02374 0.02384 0.01498 -0.00723 0.00596 -0.00144 0.02055 0.01912 0.00092 0.00184 0.00032 0.00000 0.00670 0.00629 0.00547 0.00482 0.00487 0.00542 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 = 3265 / 24017 wR2 = 0.0996 before cycle 5 for 3319 data and 0 / 286 parameters GooF = S = 0.944; Restrained GooF = 0.944 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0421 * 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 = 0.0996, GooF = S = 0.944, Restrained GooF = 0.944 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 0.0217 0.0145 S1 0.0275 0.0216 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 0.0155 0.0082 N1 0.0320 0.0235 0.0093 N2 0.0231 0.0152 0.0100 N3 0.0255 0.0190 0.0117 C1 0.0225 0.0168 0.0089 C2 0.0298 0.0215 0.0123 C3 0.0327 0.0258 0.0143 C4 0.0523 0.0220 0.0111 C5 0.0321 0.0171 0.0092 C6 0.0320 0.0138 0.0128 C7 0.0278 0.0255 0.0114 C8 0.0249 0.0157 0.0106 C9 0.0437 0.0196 0.0118 C10 0.0447 0.0222 0.0106 C11 0.0440 0.0201 0.0120 C12 0.0364 0.0285 0.0137 C13 0.0275 0.0234 0.0057 C14 0.0429 0.0134 0.0085 C15 0.0240 0.0214 0.0035 C16 0.0329 0.0214 0.0071 C17 0.0390 0.0235 0.0156 C18 0.0441 0.0286 0.0102 C19 0.0337 0.0233 0.0144 C20 0.0290 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 345. 323. 337. 340. 322. 326. 336. 325. 333. 332. GooF 0.803 0.524 0.545 0.670 0.775 0.916 0.939 1.061 1.058 1.639 K 5.138 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 0.734 0.762 0.816 0.674 0.727 0.798 0.870 0.912 1.132 1.628 K 1.004 1.004 1.013 1.027 1.040 1.041 1.038 1.049 1.027 1.055 R1 0.081 0.069 0.075 0.053 0.050 0.064 0.055 0.065 0.059 0.070 Recommended weighting scheme: WGHT 0.0421 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 8350.12 131.79 7.38 0.021 0.93 1 0 5 337496.13 258222.75 7.18 0.951 5.27 -1 0 7 102164.41 76861.52 7.03 0.519 4.38 3 0 3 14402.73 21380.33 6.81 0.274 3.52 5 0 3 25379.96 35329.23 5.91 0.352 2.23 2 0 10 84306.88 66797.66 5.41 0.484 2.63 -3 0 5 15584.44 21186.40 5.03 0.272 3.53 2 0 4 203530.44 168816.11 4.87 0.769 4.43 -2 0 8 59193.05 47488.12 4.84 0.408 3.47 6 0 6 76113.02 94701.66 4.68 0.576 1.76 -1 1 13 5283.42 6627.02 4.58 0.152 2.25 -3 6 7 2839.53 102.37 4.54 0.019 0.95 4 0 2 49443.93 60731.31 4.31 0.461 2.82 2 6 7 2678.39 39.10 4.30 0.012 0.96 7 0 5 33832.63 43322.74 4.28 0.389 1.57 1 0 21 164580.33 137567.73 4.15 0.694 1.46 -4 0 14 226966.92 192059.70 4.09 0.820 1.90 0 3 2 65548.09 55489.50 3.78 0.441 1.98 1 0 15 124863.55 106925.28 3.66 0.612 2.02 2 6 4 2747.57 403.93 3.58 0.038 0.97 -1 0 3 11755.02 9372.57 3.54 0.181 8.36 1 3 1 54221.79 44211.16 3.53 0.393 1.96 -3 0 13 192196.75 166490.86 3.50 0.763 2.18 1 0 1 5637.07 6979.40 3.49 0.156 10.55 4 0 14 238669.31 207573.31 3.45 0.852 1.68 1 3 4 68190.34 58494.46 3.45 0.453 1.90 -2 0 6 107811.73 93878.92 3.41 0.573 4.18 -1 6 15 15345.17 10105.86 3.37 0.188 0.90 3 1 12 85797.68 74507.81 3.36 0.511 1.95 -8 1 19 22569.49 17873.86 3.35 0.250 1.15 -4 1 6 14464.89 17160.91 3.33 0.245 2.47 0 3 1 54105.32 43392.82 3.33 0.390 1.99 1 1 6 14714.04 11727.22 3.31 0.203 3.63 6 0 2 71500.93 83679.03 3.29 0.541 1.91 4 2 7 61216.42 52659.91 3.29 0.429 1.83 -4 1 21 27577.81 32111.64 3.23 0.335 1.37 5 3 12 51582.90 42464.81 3.14 0.386 1.27 -1 2 17 40324.72 33937.09 3.10 0.345 1.58 2 1 7 219077.52 182186.48 3.09 0.799 2.93 4 3 4 33264.44 27896.77 3.08 0.313 1.59 1 0 27 134300.64 103216.38 3.05 0.601 1.14 -8 0 22 92278.56 77436.98 3.03 0.521 1.10 3 4 12 1523.31 12.95 3.00 0.007 1.21 -1 0 5 18480.13 15784.81 2.99 0.235 5.86 1 2 8 13936.58 11978.44 2.98 0.205 2.30 2 4 6 25369.97 31334.67 2.95 0.331 1.39 3 3 2 13629.62 17787.04 2.94 0.250 1.75 5 1 5 13127.12 15566.74 2.92 0.233 1.99 3 4 17 94796.15 82430.52 2.90 0.537 1.09 -4 1 24 28593.09 33457.25 2.88 0.342 1.23 Bond lengths and angles Hg1 - Distance Angles S3 2.3439 (0.0028) S1 2.3484 (0.0028) 178.21 (0.11) Hg1 - S3 Hg2 - Distance Angles S5_$1 2.3513 (0.0027) S5 2.3513 (0.0027) 180.00 (0.19) Hg2 - S5_$1 S1 - Distance Angles C1 1.7263 (0.0105) Hg1 2.3484 (0.0028) 94.91 (0.36) S1 - C1 S2 - Distance Angles C2 1.7503 (0.0103) C1 1.7579 (0.0107) 89.12 (0.49) S2 - C2 S3 - Distance Angles C8 1.7277 (0.0110) Hg1 2.3439 (0.0028) 94.54 (0.37) S3 - C8 S4 - Distance Angles C9 1.7400 (0.0100) C8 1.7772 (0.0111) 88.82 (0.50) S4 - C9 S5 - Distance Angles C15 1.7353 (0.0118) Hg2 2.3513 (0.0027) 97.48 (0.37) S5 - C15 S6 - Distance Angles C15 1.7466 (0.0104) C16 1.7534 (0.0106) 89.15 (0.53) S6 - C15 N1 - Distance Angles C1 1.3270 (0.0127) C7 1.3740 (0.0136) 109.43 (0.85) N1 - C1 N2 - Distance Angles C8 1.3055 (0.0139) C14 1.3960 (0.0137) 109.81 (0.93) N2 - C8 N3 - Distance Angles C15 1.3228 (0.0136) C21 1.3990 (0.0136) 109.70 (0.88) N3 - C15 C1 - Distance Angles N1 1.3270 (0.0127) S1 1.7263 (0.0105) 124.87 (0.81) S2 1.7579 (0.0107) 115.91 (0.76) 119.19 (0.58) C1 - N1 S1 C2 - Distance Angles C3 1.3735 (0.0149) C7 1.4093 (0.0153) 122.68 (0.96) S2 1.7503 (0.0103) 129.06 (0.85) 108.25 (0.76) C2 - C3 C7 C3 - Distance Angles C2 1.3735 (0.0149) C4 1.3821 (0.0152) 118.37 (1.06) H3 0.9300 120.81 120.81 C3 - C2 C4 C4 - Distance Angles C3 1.3821 (0.0152) C5 1.3837 (0.0163) 120.96 (1.08) H4 0.9300 119.52 119.52 C4 - C3 C5 C5 - Distance Angles C6 1.3842 (0.0160) C4 1.3837 (0.0163) 122.09 (1.03) H5 0.9300 118.95 118.95 C5 - C6 C4 C6 - Distance Angles C5 1.3842 (0.0160) C7 1.4380 (0.0145) 117.78 (1.03) H6 0.9300 121.11 121.11 C6 - C5 C7 C7 - Distance Angles N1 1.3740 (0.0136) C2 1.4093 (0.0152) 117.28 (0.88) C6 1.4380 (0.0145) 124.63 (0.97) 118.08 (0.99) C7 - N1 C2 C8 - Distance Angles N2 1.3055 (0.0139) S3 1.7277 (0.0110) 126.45 (0.85) S4 1.7772 (0.0111) 115.52 (0.81) 117.89 (0.61) C8 - N2 S3 C9 - Distance Angles C14 1.3936 (0.0151) C10 1.3954 (0.0148) 122.67 (0.99) S4 1.7400 (0.0100) 109.20 (0.75) 128.03 (0.88) C9 - C14 C10 C10 - Distance Angles C9 1.3954 (0.0148) C11 1.3967 (0.0162) 116.55 (1.09) H10 0.9300 121.72 121.72 C10 - C9 C11 C11 - Distance Angles C12 1.3676 (0.0166) C10 1.3967 (0.0162) 122.29 (1.01) H11 0.9300 118.85 118.85 C11 - C12 C10 C12 - Distance Angles C11 1.3676 (0.0166) C13 1.3767 (0.0159) 121.34 (1.02) H12 0.9300 119.33 119.33 C12 - C11 C13 C13 - Distance Angles C12 1.3767 (0.0159) C14 1.4278 (0.0148) 118.61 (1.07) H13 0.9300 120.70 120.70 C13 - C12 C14 C14 - Distance Angles C9 1.3936 (0.0151) N2 1.3960 (0.0137) 116.54 (0.92) C13 1.4278 (0.0148) 118.53 (0.98) 124.90 (1.03) C14 - C9 N2 C15 - Distance Angles N3 1.3228 (0.0136) S5 1.7353 (0.0118) 126.78 (0.79) S6 1.7466 (0.0104) 115.97 (0.81) 117.25 (0.67) C15 - N3 S5 C16 - Distance Angles C17 1.3697 (0.0147) C21 1.3927 (0.0153) 121.15 (0.99) S6 1.7534 (0.0106) 129.72 (0.86) 109.13 (0.79) C16 - C17 C21 C17 - Distance Angles C16 1.3697 (0.0147) C18 1.3733 (0.0151) 118.97 (1.01) H17 0.9300 120.51 120.51 C17 - C16 C18 C18 - Distance Angles C19 1.3665 (0.0172) C17 1.3733 (0.0151) 121.70 (1.10) H18 0.9300 119.15 119.15 C18 - C19 C17 C19 - Distance Angles C18 1.3665 (0.0172) C20 1.4327 (0.0167) 121.26 (1.10) H19 0.9300 119.37 119.37 C19 - C18 C20 C20 - Distance Angles C21 1.4107 (0.0150) C19 1.4327 (0.0167) 115.69 (1.04) H20 0.9300 122.16 122.16 C20 - C21 C19 C21 - Distance Angles C16 1.3927 (0.0153) N3 1.3990 (0.0136) 116.04 (0.95) C20 1.4107 (0.0150) 121.19 (1.00) 122.76 (1.02) C21 - C16 N3 Selected torsion angles -121.36 ( 3.16) S3 - Hg1 - S1 - C1 -63.67 ( 3.25) S1 - Hg1 - S3 - C8 70.62 (41.07) S5_$1 - Hg2 - S5 - C15 -177.56 ( 0.77) C7 - N1 - C1 - S1 0.32 ( 1.14) C7 - N1 - C1 - S2 7.70 ( 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 0.43 ( 0.79) C1 - S2 - C2 - C7 0.22 ( 1.61) C7 - C2 - C3 - C4 179.38 ( 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 178.94 ( 0.95) C3 - C2 - C7 - N1 -0.37 ( 1.19) S2 - C2 - C7 - N1 -1.76 ( 1.57) C3 - C2 - C7 - C6 178.93 ( 0.76) S2 - C2 - C7 - C6 -178.61 ( 0.98) C5 - C6 - C7 - N1 2.15 ( 1.48) C5 - C6 - C7 - C2 -178.79 ( 0.85) C14 - N2 - C8 - S3 -3.22 ( 1.18) C14 - N2 - C8 - S4 -20.13 ( 1.06) Hg1 - S3 - C8 - N2 164.40 ( 0.60) Hg1 - S3 - C8 - S4 3.35 ( 0.91) C9 - S4 - C8 - N2 179.32 ( 0.72) C9 - S4 - C8 - S3 -2.32 ( 0.81) C8 - S4 - C9 - C14 -178.71 ( 1.05) C8 - S4 - C9 - C10 -0.87 ( 1.57) C14 - C9 - C10 - C11 175.08 ( 0.83) S4 - C9 - C10 - C11 1.10 ( 1.61) C9 - C10 - C11 - C12 -0.34 ( 1.76) C10 - C11 - C12 - C13 -0.69 ( 1.67) C11 - C12 - C13 - C14 177.77 ( 0.95) C10 - C9 - C14 - N2 1.14 ( 1.18) S4 - C9 - C14 - N2 -0.10 ( 1.58) C10 - C9 - C14 - C13 -176.73 ( 0.78) S4 - C9 - C14 - C13 1.32 ( 1.32) C8 - N2 - C14 - C9 179.03 ( 1.03) C8 - N2 - C14 - C13 0.89 ( 1.54) C12 - C13 - C14 - C9 -176.78 ( 1.02) C12 - C13 - C14 - N2 179.50 ( 0.75) C21 - N3 - C15 - S5 -0.97 ( 1.10) C21 - N3 - C15 - S6 -10.19 ( 0.95) Hg2 - S5 - C15 - N3 170.29 ( 0.50) Hg2 - S5 - C15 - S6 1.12 ( 0.82) C16 - S6 - C15 - N3 -179.31 ( 0.62) C16 - S6 - C15 - S5 178.69 ( 1.01) C15 - S6 - C16 - C17 -0.89 ( 0.74) C15 - S6 - C16 - C21 -1.14 ( 1.52) C21 - C16 - C17 - C18 179.33 ( 0.81) S6 - C16 - C17 - C18 0.74 ( 1.60) C16 - C17 - C18 - C19 -1.12 ( 1.68) C17 - C18 - C19 - C20 1.79 ( 1.58) C18 - C19 - C20 - C21 -179.04 ( 0.90) C17 - C16 - C21 - N3 0.57 ( 1.10) S6 - C16 - C21 - N3 1.94 ( 1.53) C17 - C16 - C21 - C20 -178.45 ( 0.81) S6 - C16 - C21 - C20 0.23 ( 1.24) C15 - N3 - C21 - C16 179.23 ( 0.95) C15 - N3 - C21 - C20 -2.17 ( 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 0.2201 [ 1.18 A from HG1 ] Mean = 0.00, Rms deviation from mean = 0.27 e/A^3, Highest memory used = 3019 / 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 1.05 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 0.0534 0.5689 0.1914 1.00000 0.05 1.32 0.99 HG1 2.37 S3 2.49 S4 2.56 N2 Q5 1 0.2143 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 0.2557 -0.2929 0.1399 1.00000 0.05 1.10 1.93 C2 2.13 S2 2.23 HG1 2.25 C3 Shortest distances between peaks (including symmetry equivalents) 6 7 0.37 6 8 0.54 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 2.07 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 ----------------------- 0.03: 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 0.00: Analyse other restraints etc. 0.38: 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 0.80: Structure factors and derivatives 1.59: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.22: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 97src139 finished at 15:44:29 Total CPU time: 3.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++