+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 16:54:25 on 02-Aug-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P-1 CELL 0.71069 7.623 8.951 10.914 82.76 73.33 80.54 ZERR 2 0.001 0.001 0.002 0.01 0.006 0.02 LATT 1 SFAC C H N S BR HG UNIT 12 20 4 8 4 2 V = 701.24 F(000) = 548.0 Mu = 17.24 mm-1 Cell Wt = 1197.62 Rho = 2.836 L.S. 4 ISOR 0.005 C6 CONF FMAP 2 PLAN 10 WGHT 0.066500 FVAR 2.00391 HG1 6 0.09467 0.28390 0.26865 11.00000 0.01707 0.01451 = 0.01603 0.00106 -0.00299 -0.00423 BR1 5 0.26929 0.19519 0.03627 11.00000 0.01920 0.01052 = 0.01602 -0.00374 -0.00299 -0.00191 BR2 5 0.35075 0.29181 0.38605 11.00000 0.02062 0.01014 = 0.02143 -0.00035 -0.00968 -0.00368 S1 4 -0.10016 0.07801 0.36468 11.00000 0.02164 0.01162 = 0.01392 -0.00204 -0.00164 -0.00504 S2 4 -0.24781 0.33474 0.53755 11.00000 0.02604 0.01100 = 0.01999 -0.00546 0.00361 -0.00950 S3 4 -0.03892 0.56117 0.25510 11.00000 0.01987 0.01357 = 0.01700 0.00199 0.00121 -0.00102 S4 4 0.13637 0.82672 0.10953 11.00000 0.02350 0.00812 = 0.01915 -0.00319 -0.00649 -0.00334 N1 3 -0.37135 0.08133 0.58130 11.00000 0.01727 0.00944 = 0.01514 0.00074 -0.00364 -0.00598 AFIX 43 H1 2 -0.38487 -0.00934 0.57089 11.00000 -1.20000 AFIX 0 N2 3 0.18573 0.57386 0.01362 11.00000 0.02124 0.00774 = 0.00870 -0.00557 0.00714 -0.00521 AFIX 43 H2 2 0.17036 0.48360 0.00353 11.00000 -1.20000 AFIX 0 C1 1 -0.24589 0.15543 0.49567 11.00000 0.02163 0.00587 = 0.02238 0.00097 -0.01603 -0.00305 C2 1 -0.48310 0.15633 0.69105 11.00000 0.02679 0.03080 = 0.01510 -0.00038 0.00319 -0.01883 AFIX 23 H2A 2 -0.44650 0.11123 0.76709 11.00000 -1.20000 H2B 2 -0.61199 0.14590 0.70409 11.00000 -1.20000 AFIX 0 C3 1 -0.45710 0.32360 0.66796 11.00000 0.02634 0.01043 = 0.02694 -0.00211 -0.00032 -0.00651 AFIX 23 H3A 2 -0.44419 0.35999 0.74455 11.00000 -1.20000 H3B 2 -0.56202 0.38438 0.64447 11.00000 -1.20000 AFIX 0 C4 1 0.09841 0.63936 0.11925 11.00000 0.01239 0.01213 = 0.01639 -0.00222 -0.00615 -0.00019 C5 1 0.31007 0.66085 -0.08599 11.00000 0.01465 0.01365 = 0.01994 -0.00595 0.00092 -0.00183 AFIX 23 H5A 2 0.30174 0.64445 -0.17020 11.00000 -1.20000 H5B 2 0.43681 0.63034 -0.08257 11.00000 -1.20000 AFIX 0 C6 1 0.25004 0.82523 -0.06030 11.00000 0.01527 0.01331 = 0.02059 0.00254 -0.00606 -0.00374 AFIX 23 H6A 2 0.16562 0.87248 -0.11004 11.00000 -1.20000 H6B 2 0.35608 0.88008 -0.08291 11.00000 -1.20000 HKLF 4 Covalent radii and connectivity table for s92 in P-1 C 0.770 H 0.320 N 0.700 S 1.030 BR 1.140 HG 1.500 Hg1 - S1 S3 Br2 Br1 Br1 - Hg1 Br2 - Hg1 S1 - C1 Hg1 S2 - C1 C3 S3 - C4 Hg1 S4 - C4 C6 N1 - C1 C2 N2 - C4 C5 C1 - N1 S1 S2 C2 - N1 C3 C3 - C2 S2 C4 - N2 S3 S4 C5 - N2 C6 C6 - C5 S4 2553 Reflections read, of which 0 rejected -8 =< h =< 6, -10 =< k =< 8, -12 =< l =< 12, Max. 2-theta = 50.01 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 0 1 0 2556.09 52.99 2 1264.50 1 1 0 75995.02 501.34 2 2635.50 -1 3 0 62582.89 479.38 2 4235.50 0 3 0 18327.38 131.70 4 839.29 2 3 0 47644.17 647.86 2 4603.50 -1 4 0 20696.93 270.07 2 1638.50 -1 -4 1 151782.23 1029.18 2 5406.00 -5 -3 1 52909.68 799.76 2 7189.50 -4 -3 1 22557.54 525.01 2 3431.00 -4 -2 1 46555.04 635.24 2 3736.00 -3 -2 1 55485.72 648.29 2 7698.00 0 -2 1 10308.52 143.88 3 5216.92 1 -2 1 115150.00 424.80 3 6274.16 -5 -1 1 111902.55 863.41 2 7431.50 -4 -1 1 26136.42 399.70 2 5986.50 -3 -1 1 35770.76 412.63 2 2179.00 0 -1 1 102455.37 561.87 2 15340.50 1 -1 1 63604.89 350.67 3 2614.44 -1 1 1 58247.05 400.40 3 2301.41 0 1 1 83798.73 469.13 3 4387.77 1 1 1 36405.01 374.69 2 1916.50 -1 4 1 20169.38 498.90 2 2566.00 1 4 1 67677.95 598.29 3 4436.87 0 6 1 72349.43 550.11 3 5013.72 3 7 1 44419.54 842.24 2 6432.50 -5 -4 2 76910.68 1084.60 2 7879.50 0 -4 2 95212.85 500.75 2 4634.50 1 -4 2 63001.31 354.18 3 4248.61 1 -2 2 29717.68 291.89 3 1959.23 1 -1 2 58508.49 495.57 2 5887.50 1 0 2 60042.71 361.47 2 12921.50 -3 1 2 27397.54 366.56 2 2441.50 -2 1 2 24096.42 379.91 2 6066.50 -1 1 2 15595.33 290.99 2 3339.50 1 1 2 57301.68 323.85 2 4667.50 0 3 2 72503.05 837.27 2 4425.00 0 5 2 105070.30 1034.50 2 10557.00 0 7 2 57399.95 671.44 2 3932.50 2 -5 3 126806.57 905.80 2 6461.00 -2 2 3 56368.72 748.27 2 4289.00 2 4 3 31483.95 486.99 3 3769.36 2 5 3 113525.23 925.19 3 6032.15 1 6 3 83034.88 871.16 3 5830.59 3 6 3 41893.04 838.46 2 9403.50 3 -5 4 67641.63 877.01 2 5734.00 2 -1 4 49997.94 590.33 2 8318.50 3 0 4 13477.88 414.01 2 2467.00 -2 1 4 80035.26 746.01 2 11527.50 3 4 4 33636.55 667.00 2 10570.50 1 5 4 88613.56 1158.57 2 14049.00 ** etc. ** 58 Inconsistent equivalents 1907 Unique reflections, of which 0 suppressed R(int) = 0.0541 R(sigma) = 0.0487 Friedel opposites merged Maximum memory for data reduction = 1369 / 19267 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 = 1745 / 173619 wR2 = 0.1008 before cycle 1 for 1907 data and 136 / 136 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 6. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.005 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.003 0.000 GooF = S = 1.036; Restrained GooF = 1.034 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0665 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.00391 0.00524 0.000 OSF Mean shift/esd = 0.003 Maximum = -0.022 for y Br1 Max. shift = 0.000 A for C4 Max. dU = 0.000 for C6 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1745 / 173619 wR2 = 0.1008 before cycle 2 for 1907 data and 136 / 136 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 6. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.005 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.003 0.000 GooF = S = 1.035; Restrained GooF = 1.034 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0665 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.00391 0.00524 0.001 OSF Mean shift/esd = 0.001 Maximum = -0.008 for y Br1 Max. shift = 0.000 A for S2 Max. dU = 0.000 for C6 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1745 / 173619 wR2 = 0.1008 before cycle 3 for 1907 data and 136 / 136 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 6. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.005 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.003 0.000 GooF = S = 1.035; Restrained GooF = 1.034 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0665 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.00391 0.00524 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for U22 Hg1 Max. shift = 0.000 A for C1 Max. dU = 0.000 for C4 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1745 / 173619 wR2 = 0.1008 before cycle 4 for 1907 data and 136 / 136 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 6. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.005 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.003 0.000 GooF = S = 1.035; Restrained GooF = 1.034 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0665 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 2.00391 0.00524 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C1 Max. dU = 0.000 for C5 Largest correlation matrix elements 0.577 U33 Hg1 / OSF 0.547 U22 Hg1 / OSF -0.508 U13 C1 / U11 C1 0.565 U11 Hg1 / OSF -0.508 U13 C1 / U33 C1 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 -0.3849 -0.0093 0.5709 43 0.860 0.000 N1 C1 C2 H2 0.1704 0.4836 0.0035 43 0.860 0.000 N2 C4 C5 H2A -0.4465 0.1112 0.7671 23 0.970 0.000 C2 N1 C3 H2B -0.6120 0.1459 0.7041 23 0.970 0.000 C2 N1 C3 H3A -0.4442 0.3600 0.7446 23 0.970 0.000 C3 C2 S2 H3B -0.5620 0.3844 0.6445 23 0.970 0.000 C3 C2 S2 H5A 0.3017 0.6444 -0.1702 23 0.970 0.000 C5 N2 C6 H5B 0.4368 0.6303 -0.0826 23 0.970 0.000 C5 N2 C6 H6A 0.1656 0.8725 -0.1100 23 0.970 0.000 C6 C5 S4 H6B 0.3561 0.8801 -0.0829 23 0.970 0.000 C6 C5 S4 s92 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Hg1 0.09467 0.28390 0.26865 1.00000 0.01707 0.01451 0.01603 0.00106 -0.00299 -0.00423 0.01615 0.00055 0.00006 0.00004 0.00004 0.00000 0.00027 0.00032 0.00028 0.00019 0.00018 0.00018 0.00019 Br1 0.26929 0.19519 0.03627 1.00000 0.01920 0.01052 0.01602 -0.00374 -0.00299 -0.00191 0.01540 0.00138 0.00014 0.00011 0.00010 0.00000 0.00060 0.00063 0.00060 0.00045 0.00045 0.00043 0.00028 Br2 0.35075 0.29181 0.38605 1.00000 0.02062 0.01014 0.02143 -0.00035 -0.00968 -0.00368 0.01646 0.00137 0.00015 0.00011 0.00010 0.00000 0.00061 0.00063 0.00062 0.00045 0.00048 0.00043 0.00028 S1 -0.10016 0.07801 0.36468 1.00000 0.02164 0.01162 0.01392 -0.00204 -0.00164 -0.00504 0.01599 0.00363 0.00038 0.00030 0.00026 0.00000 0.00154 0.00160 0.00143 0.00112 0.00116 0.00110 0.00060 S2 -0.24781 0.33474 0.53755 1.00000 0.02604 0.01100 0.01999 -0.00546 0.00361 -0.00950 0.01990 0.00382 0.00040 0.00030 0.00028 0.00000 0.00166 0.00165 0.00157 0.00121 0.00124 0.00115 0.00066 S3 -0.03892 0.56117 0.25510 1.00000 0.01987 0.01357 0.01700 0.00199 0.00121 -0.00102 0.01856 0.00398 0.00039 0.00031 0.00027 0.00000 0.00150 0.00168 0.00153 0.00118 0.00118 0.00112 0.00063 S4 0.13637 0.82672 0.10953 1.00000 0.02350 0.00812 0.01915 -0.00319 -0.00649 -0.00334 0.01645 0.00357 0.00038 0.00029 0.00027 0.00000 0.00158 0.00157 0.00154 0.00116 0.00122 0.00112 0.00062 N1 -0.37135 0.08133 0.58130 1.00000 0.01728 0.00944 0.01514 0.00074 -0.00364 -0.00598 0.01378 0.01187 0.00118 0.00096 0.00082 0.00000 0.00502 0.00516 0.00497 0.00381 0.00403 0.00366 0.00195 H1 -0.38487 -0.00934 0.57089 1.00000 0.01654 0.00000 0.00000 N2 0.18573 0.57387 0.01362 1.00000 0.02124 0.00775 0.00870 -0.00557 0.00714 -0.00521 0.01411 0.01202 0.00120 0.00094 0.00079 0.00000 0.00518 0.00499 0.00477 0.00367 0.00386 0.00369 0.00200 H2 0.17036 0.48360 0.00353 1.00000 0.01693 0.00000 0.00000 C1 -0.24589 0.15543 0.49567 1.00000 0.02163 0.00587 0.02238 0.00097 -0.01603 -0.00305 0.01456 0.01371 0.00148 0.00113 0.00106 0.00000 0.00632 0.00619 0.00635 0.00469 0.00521 0.00449 0.00243 C2 -0.48310 0.15633 0.69105 1.00000 0.02679 0.03080 0.01509 -0.00038 0.00319 -0.01883 0.02449 0.01593 0.00167 0.00129 0.00109 0.00000 0.00704 0.00798 0.00639 0.00533 0.00525 0.00550 0.00285 H2A -0.44650 0.11123 0.76709 1.00000 0.02938 0.00000 0.00000 H2B -0.61199 0.14590 0.70409 1.00000 0.02938 0.00000 0.00000 C3 -0.45709 0.32360 0.66796 1.00000 0.02634 0.01043 0.02694 -0.00211 -0.00032 -0.00651 0.02218 0.01633 0.00164 0.00120 0.00114 0.00000 0.00681 0.00660 0.00706 0.00516 0.00543 0.00483 0.00271 H3A -0.44419 0.35999 0.74455 1.00000 0.02661 0.00000 0.00000 H3B -0.56202 0.38438 0.64447 1.00000 0.02661 0.00000 0.00000 C4 0.09840 0.63936 0.11925 1.00000 0.01239 0.01213 0.01639 -0.00222 -0.00615 -0.00019 0.01324 0.01394 0.00141 0.00114 0.00102 0.00000 0.00563 0.00624 0.00603 0.00460 0.00466 0.00424 0.00232 C5 0.31007 0.66085 -0.08599 1.00000 0.01465 0.01365 0.01994 -0.00595 0.00092 -0.00183 0.01687 0.01511 0.00149 0.00115 0.00108 0.00000 0.00587 0.00664 0.00628 0.00483 0.00480 0.00441 0.00245 H5A 0.30174 0.64445 -0.17020 1.00000 0.02024 0.00000 0.00000 H5B 0.43681 0.63034 -0.08257 1.00000 0.02024 0.00000 0.00000 C6 0.25004 0.82522 -0.06030 1.00000 0.01527 0.01331 0.02060 0.00254 -0.00606 -0.00374 0.01628 0.01466 0.00148 0.00115 0.00104 0.00000 0.00406 0.00435 0.00431 0.00345 0.00344 0.00330 0.00242 H6A 0.16562 0.87248 -0.11005 1.00000 0.01954 0.00000 0.00000 H6B 0.35608 0.88008 -0.08291 1.00000 0.01954 0.00000 0.00000 Final Structure Factor Calculation for s92 in P-1 Total number of l.s. parameters = 136 Maximum vector length = 511 Memory required = 1609 / 25039 wR2 = 0.1008 before cycle 5 for 1907 data and 0 / 136 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 0. 0. 0. 0. 0. 0. 6. 0. rms sigma 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.005 0.000 rms deviation 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.003 0.000 GooF = S = 1.035; Restrained GooF = 1.034 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0665 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0372 for 1734 Fo > 4sig(Fo) and 0.0396 for all 1907 data wR2 = 0.1008, GooF = S = 1.035, Restrained GooF = 1.034 for all data Occupancy sum of asymmetric unit = 15.00 for non-hydrogen and 10.00 for hydrogen atoms Principal mean square atomic displacements U 0.0188 0.0177 0.0120 Hg1 0.0207 0.0164 0.0092 Br1 0.0243 0.0156 0.0095 Br2 0.0243 0.0134 0.0103 S1 0.0382 0.0149 0.0067 S2 0.0294 0.0148 0.0114 S3 0.0235 0.0191 0.0068 S4 0.0187 0.0157 0.0069 N1 0.0323 0.0074 0.0026 N2 0.0300 0.0082 0.0054 C1 0.0442 0.0210 0.0082 C2 0.0362 0.0216 0.0088 C3 0.0173 0.0120 0.0104 C4 0.0261 0.0143 0.0102 C5 0.0227 0.0146 0.0116 C6 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.044 0.078 0.116 0.148 0.185 0.225 0.269 0.329 0.416 1.000 Number in group 192. 191. 194. 188. 191. 188. 193. 189. 189. 192. GooF 0.711 0.702 0.570 0.710 0.835 1.012 1.215 1.266 1.527 1.333 K 1.261 1.025 0.991 0.996 0.994 0.999 1.003 1.005 1.026 1.016 Resolution(A) 0.84 0.92 0.96 1.01 1.07 1.14 1.24 1.36 1.56 1.99 inf Number in group 198. 190. 191. 186. 192. 192. 185. 191. 191. 191. GooF 0.619 0.645 0.681 0.816 0.738 0.875 0.909 1.219 1.530 1.684 K 1.003 1.009 1.010 1.006 1.016 1.018 1.022 1.005 1.020 1.010 R1 0.034 0.041 0.036 0.036 0.032 0.036 0.036 0.042 0.044 0.049 Recommended weighting scheme: WGHT 0.0607 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) 1 1 5 5735.54 11877.52 8.80 0.388 2.17 0 5 0 5449.16 9562.00 7.04 0.348 1.76 -2 3 4 333.94 19.48 5.71 0.016 1.58 0 0 6 7058.36 11029.66 5.51 0.373 1.74 0 2 3 9389.98 13832.12 5.16 0.418 2.84 5 1 3 5644.90 8252.93 4.75 0.323 1.51 5 0 4 6045.08 8681.38 4.57 0.331 1.44 1 0 7 4336.52 6366.44 4.56 0.284 1.54 4 1 2 3276.92 4710.07 4.43 0.244 1.90 2 1 3 1916.00 2705.17 4.42 0.185 2.95 0 0 1 482.11 291.61 4.38 0.061 10.42 3 1 6 3895.50 5571.07 4.32 0.265 1.66 3 2 5 2545.11 3504.32 4.09 0.210 1.82 0 2 4 3749.57 5251.64 4.07 0.258 2.33 -3 -1 4 6122.03 8413.50 3.97 0.326 1.56 0 3 3 3084.43 4278.15 3.89 0.233 2.34 3 2 3 2642.15 3606.06 3.78 0.214 2.21 1 2 4 2642.40 3629.07 3.77 0.214 2.45 -4 2 1 14714.39 19346.52 3.75 0.495 1.53 -3 -2 3 5094.80 6900.53 3.66 0.295 1.67 0 7 0 6326.98 8481.18 3.61 0.327 1.26 0 -1 7 6042.59 8075.79 3.58 0.320 1.45 2 3 5 12162.63 15674.76 3.47 0.445 1.83 -2 0 4 4299.67 5714.20 3.35 0.269 1.88 4 -6 5 7381.10 5613.92 3.35 0.266 0.99 2 0 7 4321.58 5690.59 3.34 0.268 1.53 0 -4 1 13528.28 17020.09 3.19 0.464 2.12 1 0 1 8689.48 10838.56 3.14 0.370 6.88 -1 -2 3 2596.58 3361.59 3.12 0.206 2.37 4 -5 6 11521.64 9244.64 2.97 0.342 1.04 -1 4 5 8153.50 10038.44 2.86 0.356 1.45 4 1 0 11837.40 14561.93 2.85 0.429 1.82 -2 -1 3 7950.74 6361.45 2.83 0.284 2.17 2 2 5 12959.26 15859.85 2.80 0.448 2.00 4 -1 1 5537.07 4462.99 2.79 0.238 1.77 5 2 2 9755.30 7954.36 2.79 0.317 1.50 -3 1 3 4158.22 5244.27 2.77 0.257 1.72 1 1 6 16257.84 19817.86 2.73 0.501 1.81 2 -4 7 15462.21 12827.93 2.71 0.403 1.18 1 0 5 27694.07 33450.48 2.69 0.650 2.17 3 2 7 3395.95 4288.66 2.68 0.233 1.45 -5 -3 2 6554.59 8129.49 2.66 0.321 1.24 -1 6 1 20385.68 17121.32 2.65 0.465 1.39 5 -5 1 6649.96 8103.18 2.55 0.320 1.06 7 3 0 14253.69 17270.20 2.53 0.467 1.02 0 5 1 3958.00 3333.70 2.51 0.205 1.76 -4 -3 2 4045.16 4979.98 2.50 0.251 1.45 1 2 2 65.85 27.61 2.50 0.019 3.59 -1 8 1 16214.27 13536.97 2.49 0.414 1.07 -2 1 7 6793.40 8346.55 2.47 0.325 1.25 Selected torsion angles -42.25 ( 0.38) S3 - Hg1 - S1 - C1 78.69 ( 0.36) Br2 - Hg1 - S1 - C1 -166.93 ( 0.36) Br1 - Hg1 - S1 - C1 -147.85 ( 0.35) S1 - Hg1 - S3 - C4 85.85 ( 0.36) Br2 - Hg1 - S3 - C4 -27.02 ( 0.37) Br1 - Hg1 - S3 - C4 177.81 ( 0.81) C2 - N1 - C1 - S1 -0.61 ( 1.21) C2 - N1 - C1 - S2 -176.51 ( 0.80) Hg1 - S1 - C1 - N1 1.70 ( 0.73) Hg1 - S1 - C1 - S2 -8.95 ( 0.83) C3 - S2 - C1 - N1 172.67 ( 0.76) C3 - S2 - C1 - S1 12.26 ( 1.36) C1 - N1 - C2 - C3 -17.06 ( 1.12) N1 - C2 - C3 - S2 14.86 ( 0.85) C1 - S2 - C3 - C2 -174.25 ( 0.79) C5 - N2 - C4 - S3 5.71 ( 1.21) C5 - N2 - C4 - S4 31.86 ( 1.03) Hg1 - S3 - C4 - N2 -148.10 ( 0.52) Hg1 - S3 - C4 - S4 9.29 ( 0.83) C6 - S4 - C4 - N2 -170.74 ( 0.67) C6 - S4 - C4 - S3 -21.24 ( 1.28) C4 - N2 - C5 - C6 25.57 ( 0.99) N2 - C5 - C6 - S4 -20.32 ( 0.76) C4 - S4 - C6 - C5 FMAP and GRID set by program FMAP 2 1 19 GRID -3.125 -2 -2 3.125 2 2 R1 = 0.0390 for 1907 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.70 at 0.0419 0.3071 0.3621 [ 1.02 A from HG1 ] Deepest hole -1.27 at 0.4989 0.2853 0.3660 [ 1.08 A from BR2 ] Mean = 0.00, Rms deviation from mean = 0.30 e/A^3, Highest memory used = 1666 / 15608 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0419 0.3071 0.3621 1.00000 0.05 1.70 1.02 HG1 2.42 BR2 2.46 S1 2.47 S2 Q2 1 0.1529 0.2742 0.1768 1.00000 0.05 1.65 0.98 HG1 1.71 BR1 2.48 H2 2.84 S3 Q3 1 0.1833 0.2004 0.1367 1.00000 0.05 1.16 1.11 BR1 1.62 HG1 2.76 H2 2.94 H6A Q4 1 0.3051 0.3073 0.4815 1.00000 0.05 1.09 1.02 BR2 2.50 H3B 2.73 H1 2.84 H2B Q5 1 -0.0053 0.9562 0.0039 1.00000 0.05 1.06 1.67 H6A 1.95 S4 2.05 H6A 2.08 C6 Q6 1 0.2228 0.0483 -0.0179 1.00000 0.05 1.03 1.63 BR1 1.78 H6B 2.07 C6 2.13 H6A Q7 1 0.1917 0.8255 0.0141 1.00000 0.05 0.95 0.81 C6 1.01 S4 1.43 H6A 1.50 H6B Q8 1 -0.8041 0.2442 0.7774 1.00000 0.05 0.94 1.63 H2B 2.00 S3 2.34 C4 2.39 C2 Q9 1 -0.5458 0.5269 0.6797 1.00000 0.05 0.88 1.41 H3B 1.73 H3A 1.84 C3 2.02 H5A Q10 1 0.1426 0.0472 0.3540 1.00000 0.05 0.87 1.80 S1 2.17 N1 2.19 H1 2.22 HG1 Shortest distances between peaks (including symmetry equivalents) 5 5 0.79 2 3 0.80 5 6 1.63 5 7 1.77 5 6 1.99 1 2 1.99 6 7 2.02 3 6 2.22 5 7 2.24 1 10 2.33 3 10 2.55 2 10 2.62 1 3 2.62 4 9 2.66 1 4 2.69 6 8 2.69 3 5 2.92 5 8 2.97 2 6 2.99 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 0.02: 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. 0.38: 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 0.31: Structure factors and derivatives 0.36: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.17: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 16:54:26 Total CPU time: 1.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++