+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 10:50:15 on 23-Apr-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P-1 CELL 0.71073 6.1793 17.1497 20.2838 75.314 89.542 84.133 ZERR 2.00 0.0032 0.0071 0.0071 0.070 0.061 0.035 LATT 1 SFAC C H O CL UNIT 92 98 12 6 V = 2068.06 F(000) = 848.0 Mu = 0.27 mm-1 Cell Wt = 1608.40 Rho = 1.291 MERG 2 OMIT -3.00 55.00 OMIT 0 12 6 OMIT 0 14 7 SHEL 7 0.77 HTAB O1 O21 EQIV $1 -X, -Y+1, -Z+1 EQIV $2 -X, -Y+1, -Z EQIV $3 X+1, Y, Z EQIV $4 X-1, Y+1, Z HTAB O2 O22_$1 HTAB O21 O1_$2 HTAB O22 O42_$3 HTAB O41 O1_$4 HTAB O42 O2_$1 FMAP 2 PLAN 5 SIZE 0.03 0.10 0.18 ACTA EXTI BOND $H WGHT 0.06750 1.10000 L.S. 8 TEMP -153.00 FVAR 0.23425 MOLE 1 C1 1 -0.273878 0.537606 0.334912 11.00000 0.02733 0.02351 = 0.02808 -0.00254 0.00015 -0.00305 C2 1 -0.171935 0.609425 0.350088 11.00000 0.03253 0.02563 = 0.03229 -0.00809 0.00288 -0.00396 AFIX 137 H2A 2 -0.233442 0.620478 0.391876 11.00000 -1.50000 H2B 2 -0.203269 0.657463 0.311988 11.00000 -1.50000 H2C 2 -0.014098 0.596125 0.356077 11.00000 -1.50000 AFIX 0 C3 1 -0.519875 0.562539 0.323227 11.00000 0.02658 0.03143 = 0.03997 -0.00182 -0.00223 0.00003 AFIX 137 H3A 2 -0.591543 0.516264 0.317381 11.00000 -1.50000 H3B 2 -0.544260 0.607383 0.282203 11.00000 -1.50000 H3C 2 -0.580379 0.579838 0.362659 11.00000 -1.50000 AFIX 0 C4 1 -0.183481 0.516419 0.270372 11.00000 0.02476 0.02608 = 0.02554 -0.00077 -0.00386 -0.00216 C5 1 -0.039436 0.561205 0.227741 11.00000 0.03323 0.02736 = 0.02705 -0.00480 -0.00199 -0.00737 AFIX 43 H5 2 0.008012 0.607616 0.238417 11.00000 -1.20000 AFIX 0 C6 1 0.036350 0.539422 0.169906 11.00000 0.03623 0.03142 = 0.02496 -0.00220 0.00064 -0.00881 AFIX 43 H6 2 0.135929 0.570576 0.141446 11.00000 -1.20000 AFIX 0 C7 1 -0.031663 0.473242 0.153641 11.00000 0.03457 0.03035 = 0.02333 -0.00658 -0.00579 -0.00070 C8 1 -0.176969 0.427860 0.194561 11.00000 0.03963 0.02906 = 0.03291 -0.00747 -0.00736 -0.00944 AFIX 43 H8 2 -0.226018 0.382192 0.183030 11.00000 -1.20000 AFIX 0 C9 1 -0.249873 0.449684 0.252329 11.00000 0.03254 0.02976 = 0.02701 -0.00410 -0.00147 -0.00775 AFIX 43 H9 2 -0.348716 0.418047 0.280705 11.00000 -1.20000 AFIX 0 C10 1 -0.224368 0.464654 0.396075 11.00000 0.02461 0.02255 = 0.02706 -0.00737 0.00063 -0.00469 C11 1 -0.375402 0.437564 0.444709 11.00000 0.02342 0.02852 = 0.02839 -0.00993 0.00110 -0.00089 AFIX 43 H11 2 -0.519665 0.463695 0.439540 11.00000 -1.20000 AFIX 0 C12 1 -0.322515 0.373620 0.500565 11.00000 0.02939 0.02732 = 0.02450 -0.00823 0.00444 -0.00632 AFIX 43 H12 2 -0.429445 0.355962 0.533359 11.00000 -1.20000 AFIX 0 C13 1 -0.113167 0.335291 0.508659 11.00000 0.02986 0.02355 = 0.02108 -0.00710 -0.00413 -0.00247 C14 1 0.041163 0.360604 0.460911 11.00000 0.02060 0.03062 = 0.03098 -0.00351 0.00085 -0.00025 AFIX 43 H14 2 0.184881 0.333977 0.466120 11.00000 -1.20000 AFIX 0 C15 1 -0.014198 0.424605 0.405723 11.00000 0.02505 0.03070 = 0.02864 -0.00372 0.00394 -0.00556 AFIX 43 H15 2 0.093425 0.442180 0.373156 11.00000 -1.20000 AFIX 0 O1 3 0.044131 0.447514 0.097169 11.00000 0.04853 0.03487 = 0.02548 -0.00986 -0.00067 -0.00811 AFIX 147 H1 2 0.120094 0.481883 0.073660 11.00000 -1.50000 AFIX 0 O2 3 -0.051893 0.269982 0.562655 11.00000 0.03091 0.03014 = 0.02635 -0.00089 0.00327 -0.00341 AFIX 147 H2 2 -0.158072 0.259916 0.588433 11.00000 -1.50000 AFIX 0 MOLE 2 C21 1 0.490365 0.831245 0.068551 11.00000 0.02993 0.03329 = 0.02343 -0.00447 0.00195 -0.00971 C22 1 0.345010 0.908259 0.035109 11.00000 0.04387 0.02833 = 0.02908 -0.00256 -0.00267 -0.00734 AFIX 137 H22A 2 0.359724 0.920124 -0.014492 11.00000 -1.50000 H22B 2 0.388678 0.953569 0.051404 11.00000 -1.50000 H22C 2 0.193194 0.900588 0.046916 11.00000 -1.50000 AFIX 0 C23 1 0.722848 0.844586 0.045209 11.00000 0.03270 0.04569 = 0.03104 -0.00736 0.00392 -0.01130 AFIX 137 H23A 2 0.730660 0.850478 -0.004063 11.00000 -1.50000 H23B 2 0.822738 0.797994 0.068969 11.00000 -1.50000 H23C 2 0.764030 0.893830 0.055771 11.00000 -1.50000 AFIX 0 C24 1 0.426288 0.757083 0.047915 11.00000 0.02562 0.03078 = 0.02314 -0.00482 0.00404 -0.00226 C25 1 0.254559 0.760122 0.003571 11.00000 0.03259 0.03168 = 0.02412 -0.00520 0.00392 -0.00420 AFIX 43 H25 2 0.173592 0.810787 -0.016032 11.00000 -1.20000 AFIX 0 C26 1 0.197872 0.691388 -0.012916 11.00000 0.03653 0.04064 = 0.02185 -0.00885 0.00254 -0.00817 AFIX 43 H26 2 0.078732 0.695040 -0.043238 11.00000 -1.20000 AFIX 0 C27 1 0.313907 0.618029 0.014577 11.00000 0.04123 0.03114 = 0.02797 -0.01114 0.00639 -0.00765 C28 1 0.486998 0.612799 0.058576 11.00000 0.04466 0.03018 = 0.03496 -0.00742 0.00360 0.00370 AFIX 43 H28 2 0.569167 0.562117 0.077223 11.00000 -1.20000 AFIX 0 C29 1 0.539905 0.681869 0.075307 11.00000 0.03351 0.04278 = 0.02874 -0.01206 -0.00407 -0.00061 AFIX 43 H29 2 0.657235 0.677713 0.106402 11.00000 -1.20000 AFIX 0 C30 1 0.468231 0.816940 0.145956 11.00000 0.02450 0.02391 = 0.02569 -0.00351 0.00243 -0.00412 C31 1 0.283816 0.785291 0.177888 11.00000 0.02424 0.02862 = 0.02983 -0.00802 0.00008 -0.00476 AFIX 43 H31 2 0.176291 0.770840 0.151236 11.00000 -1.20000 AFIX 0 C32 1 0.252983 0.774394 0.246644 11.00000 0.02829 0.02779 = 0.02781 -0.00537 0.00571 -0.00726 AFIX 43 H32 2 0.125348 0.753211 0.267054 11.00000 -1.20000 AFIX 0 C33 1 0.409743 0.794598 0.285756 11.00000 0.02811 0.02130 = 0.02344 -0.00497 0.00300 -0.00309 C34 1 0.592590 0.827385 0.255838 11.00000 0.02743 0.03043 = 0.02731 -0.00929 -0.00133 -0.00601 AFIX 43 H34 2 0.698233 0.842550 0.282683 11.00000 -1.20000 AFIX 0 C35 1 0.620941 0.838014 0.186422 11.00000 0.02702 0.02916 = 0.02846 -0.00413 0.00368 -0.00851 AFIX 43 H35 2 0.747508 0.860184 0.166085 11.00000 -1.20000 AFIX 0 O21 3 0.260303 0.547033 0.002011 11.00000 0.05664 0.03399 = 0.03644 -0.01384 -0.00366 -0.00771 AFIX 147 H21 2 0.170476 0.557851 -0.030717 11.00000 -1.50000 AFIX 0 O22 3 0.375766 0.781202 0.354732 11.00000 0.03288 0.03390 = 0.02218 -0.00491 0.00047 -0.01076 AFIX 147 H22 2 0.481008 0.795273 0.373329 11.00000 -1.50000 AFIX 0 MOLE 3 C41 1 -0.277962 1.167091 0.376406 11.00000 0.02670 0.03066 = 0.03206 -0.01235 0.00043 -0.00609 C42 1 -0.046014 1.192296 0.376667 11.00000 0.03406 0.03540 = 0.04925 -0.01272 -0.00263 -0.00784 AFIX 137 H42A 2 0.038626 1.174300 0.341185 11.00000 -1.50000 H42B 2 0.023854 1.167232 0.421258 11.00000 -1.50000 H42C 2 -0.052841 1.251405 0.367724 11.00000 -1.50000 AFIX 0 C43 1 -0.403030 1.193311 0.433820 11.00000 0.03861 0.03674 = 0.03412 -0.01627 -0.00254 -0.00387 AFIX 137 H43A 2 -0.400484 1.251749 0.427744 11.00000 -1.50000 H43B 2 -0.334763 1.164150 0.477796 11.00000 -1.50000 H43C 2 -0.554039 1.180846 0.432736 11.00000 -1.50000 AFIX 0 C44 1 -0.380349 1.207334 0.306657 11.00000 0.02734 0.02401 = 0.03351 -0.00734 -0.00041 -0.00531 C45 1 -0.559041 1.265065 0.296333 11.00000 0.03419 0.02920 = 0.03594 -0.00746 0.00432 -0.00702 AFIX 43 H45 2 -0.619650 1.281607 0.334424 11.00000 -1.20000 AFIX 0 C46 1 -0.651792 1.299284 0.232787 11.00000 0.03223 0.02969 = 0.04012 -0.00187 0.00065 0.00195 AFIX 43 H46 2 -0.773508 1.339118 0.227300 11.00000 -1.20000 AFIX 0 C47 1 -0.566445 1.275234 0.176978 11.00000 0.04285 0.03223 = 0.03171 0.00076 -0.00172 -0.00912 C48 1 -0.385247 1.218998 0.185440 11.00000 0.05015 0.02953 = 0.03171 -0.00660 0.00603 -0.00648 AFIX 43 H48 2 -0.323287 1.203321 0.147141 11.00000 -1.20000 AFIX 0 C49 1 -0.295337 1.185969 0.249075 11.00000 0.03409 0.02844 = 0.03581 -0.00706 -0.00097 -0.00044 AFIX 43 H49 2 -0.171124 1.147277 0.254164 11.00000 -1.20000 AFIX 0 C50 1 -0.278019 1.075515 0.389142 11.00000 0.02728 0.03057 = 0.02210 -0.00651 -0.00004 -0.00414 C51 1 -0.468917 1.044172 0.375888 11.00000 0.02437 0.03075 = 0.03872 -0.00638 -0.00146 0.00044 AFIX 43 H51 2 -0.593509 1.080520 0.358251 11.00000 -1.20000 AFIX 0 C52 1 -0.480777 0.962056 0.387747 11.00000 0.02548 0.02804 = 0.04198 -0.00755 -0.00169 -0.00642 AFIX 43 H52 2 -0.612158 0.942107 0.378550 11.00000 -1.20000 AFIX 0 C53 1 -0.300642 0.909184 0.413031 11.00000 0.02991 0.02313 = 0.02222 -0.00376 0.00068 -0.00208 C54 1 -0.111206 0.937979 0.427776 11.00000 0.02852 0.03194 = 0.02552 -0.00421 -0.00683 -0.00021 AFIX 43 H54 2 0.012127 0.901301 0.446088 11.00000 -1.20000 AFIX 0 C55 1 -0.102130 1.020411 0.415742 11.00000 0.02697 0.03027 = 0.02722 -0.00591 -0.00513 -0.00631 AFIX 43 H55 2 0.028838 1.039822 0.426045 11.00000 -1.20000 AFIX 0 O41 3 -0.654716 1.304794 0.112835 11.00000 0.05908 0.04935 = 0.03103 -0.00113 -0.00451 0.00455 AFIX 147 H41 2 -0.744340 1.345314 0.112031 11.00000 -1.50000 AFIX 0 O42 3 -0.317903 0.827182 0.422674 11.00000 0.02894 0.02629 = 0.03189 -0.00434 -0.00449 -0.00112 AFIX 147 H42 2 -0.194814 0.801183 0.432639 11.00000 -1.50000 AFIX 0 MOLE 4 C61 1 0.153149 0.995151 0.188657 11.00000 0.03701 0.02875 = 0.03726 -0.00920 -0.00031 -0.00190 AFIX 13 H61 2 0.237907 0.944550 0.182788 11.00000 -1.20000 AFIX 0 CL61 4 0.025900 0.973045 0.268007 11.00000 0.04786 0.04318 = 0.03642 -0.00953 0.00607 0.00139 CL62 4 0.331509 1.068194 0.185021 11.00000 0.06332 0.06843 = 0.06773 -0.01248 -0.00018 -0.03494 CL63 4 -0.043987 1.027990 0.123128 11.00000 0.05263 0.04962 = 0.04055 -0.00526 -0.01288 -0.00085 HKLF 4 Covalent radii and connectivity table for s92 in P-1 C 0.770 H 0.320 O 0.660 CL 0.990 C1 - C10 C4 C2 C3 C2 - C1 C3 - C1 C4 - C5 C9 C1 C5 - C6 C4 C6 - C7 C5 C7 - C6 C8 O1 C8 - C9 C7 C9 - C8 C4 C10 - C11 C15 C1 C11 - C12 C10 C12 - C11 C13 C13 - C14 O2 C12 C14 - C15 C13 C15 - C14 C10 O1 - C7 O2 - C13 C21 - C22 C24 C23 C30 C22 - C21 C23 - C21 C24 - C25 C29 C21 C25 - C26 C24 C26 - C27 C25 C27 - C26 O21 C28 C28 - C27 C29 C29 - C28 C24 C30 - C35 C31 C21 C31 - C32 C30 C32 - C31 C33 C33 - O22 C34 C32 C34 - C33 C35 C35 - C34 C30 O21 - C27 O22 - C33 C41 - C44 C50 C43 C42 C42 - C41 C43 - C41 C44 - C45 C49 C41 C45 - C46 C44 C46 - C45 C47 C47 - O41 C48 C46 C48 - C49 C47 C49 - C48 C44 C50 - C55 C51 C41 C51 - C52 C50 C52 - C53 C51 C53 - C52 C54 O42 C54 - C53 C55 C55 - C54 C50 O41 - C47 O42 - C53 C61 - Cl62 Cl63 Cl61 Cl61 - C61 Cl62 - C61 Cl63 - C61 Operators for generating equivalent atoms: $1 -x, -y+1, -z+1 $2 -x, -y+1, -z $3 x+1, y, z $4 x-1, y+1, z 40292 Reflections read, of which 244 rejected -8 =< h =< 8, -22 =< k =< 22, -26 =< l =< 26, Max. 2-theta = 54.97 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 1 0 0 52.48 0.67 11 6.39 -1 1 0 203.80 0.95 8 53.81 1 1 0 48.14 0.62 8 4.19 -1 2 0 1125.91 27.57 2 309.52 -2 4 0 49.48 0.98 6 6.08 -3 6 0 104.57 2.08 6 11.10 -3 8 0 32.28 0.81 7 4.07 1 -2 1 370.81 0.85 7 135.27 -1 0 1 165.49 1.91 9 14.03 -1 1 1 64.36 0.91 8 5.45 1 1 1 72.05 1.02 8 8.55 -1 4 1 940.29 15.44 4 119.73 2 -3 2 110.70 1.44 6 17.51 0 -2 2 160.17 3.02 5 16.84 -5 0 2 56.50 0.88 8 5.80 -1 4 2 191.54 3.36 5 19.42 3 -5 3 89.85 1.86 6 9.61 3 -3 3 109.34 1.65 9 8.26 -1 -1 3 83.23 1.32 5 10.27 5 -1 3 85.47 0.79 9 7.50 -1 3 3 255.07 3.90 6 22.99 -2 6 3 81.63 1.38 5 10.70 -3 13 3 22.54 0.69 5 4.47 -3 2 4 53.29 0.74 8 5.65 -2 5 4 96.11 1.74 6 10.21 -1 -1 5 95.57 1.49 5 16.64 -3 12 5 30.88 0.79 5 5.25 -3 13 6 40.01 0.83 4 9.01 -3 13 7 18.72 0.72 4 4.83 -4 3 8 47.45 0.80 7 5.40 -5 3 9 42.56 0.80 7 6.21 -3 8 9 30.63 0.70 7 3.76 -3 10 9 37.39 0.80 5 5.80 -5 3 10 54.35 0.83 7 8.18 -4 6 10 112.67 0.91 8 11.76 3 9 10 79.39 1.64 7 10.14 2 7 19 10.75 1.19 4 6.47 -2 0 21 12.79 1.63 3 11.00 38 Inconsistent equivalents 9380 Unique reflections, of which 0 suppressed R(int) = 0.1387 R(sigma) = 0.1038 Friedel opposites merged Maximum memory for data reduction = 5056 / 94991 Default effective X-H distances for T = -153.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 1.00 0.99 0.98 0.95 0.88 0.91 1.12 0.84 0.95 0.88 0.95 Note that these distances are chosen to give the best fit to the X-ray data and so avoid the introduction of systematic error. The true internuclear distances are longer and do not vary with temperature ! The apparent variation with temperature is caused by libration. Least-squares cycle 1 Maximum vector length = 511 Memory required = 6513 / 674006 wR2 = 0.1754 before cycle 1 for 9380 data and 509 / 509 parameters GooF = S = 1.022; Restrained GooF = 1.022 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0675 * P )^2 + 1.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23521 0.00049 1.966 OSF 2 0.00370 0.00093 3.980 EXTI Mean shift/esd = 0.081 Maximum = 3.980 for EXTI Max. shift = 0.003 A for H41 Max. dU = 0.000 for C61 Least-squares cycle 2 Maximum vector length = 511 Memory required = 6513 / 674006 wR2 = 0.1752 before cycle 2 for 9380 data and 509 / 509 parameters GooF = S = 1.020; Restrained GooF = 1.020 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0675 * P )^2 + 1.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23569 0.00050 0.960 OSF 2 0.00572 0.00108 1.872 EXTI Mean shift/esd = 0.039 Maximum = 1.872 for EXTI Max. shift = 0.002 A for H41 Max. dU = 0.000 for C61 Least-squares cycle 3 Maximum vector length = 511 Memory required = 6513 / 674006 wR2 = 0.1751 before cycle 3 for 9380 data and 509 / 509 parameters GooF = S = 1.019; Restrained GooF = 1.019 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0675 * P )^2 + 1.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23573 0.00050 0.080 OSF 2 0.00588 0.00116 0.135 EXTI Mean shift/esd = 0.004 Maximum = 0.135 for EXTI Max. shift = 0.000 A for H42 Max. dU = 0.000 for C22 Least-squares cycle 4 Maximum vector length = 511 Memory required = 6513 / 674006 wR2 = 0.1751 before cycle 4 for 9380 data and 509 / 509 parameters GooF = S = 1.019; Restrained GooF = 1.019 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0675 * P )^2 + 1.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23573 0.00050 0.003 OSF 2 0.00588 0.00117 0.004 EXTI Mean shift/esd = 0.000 Maximum = 0.004 for EXTI Max. shift = 0.000 A for H42 Max. dU = 0.000 for C22 Least-squares cycle 5 Maximum vector length = 511 Memory required = 6513 / 674006 wR2 = 0.1751 before cycle 5 for 9380 data and 509 / 509 parameters GooF = S = 1.019; Restrained GooF = 1.019 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0675 * P )^2 + 1.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23573 0.00050 0.002 OSF 2 0.00588 0.00117 0.001 EXTI Mean shift/esd = 0.000 Maximum = 0.002 for OSF Max. shift = 0.000 A for H42 Max. dU = 0.000 for C22 Least-squares cycle 6 Maximum vector length = 511 Memory required = 6513 / 674006 wR2 = 0.1751 before cycle 6 for 9380 data and 509 / 509 parameters GooF = S = 1.019; Restrained GooF = 1.019 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0675 * P )^2 + 1.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23573 0.00050 0.000 OSF 2 0.00588 0.00117 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for y Cl63 Max. shift = 0.000 A for H42 Max. dU = 0.000 for C30 Least-squares cycle 7 Maximum vector length = 511 Memory required = 6513 / 674006 wR2 = 0.1751 before cycle 7 for 9380 data and 509 / 509 parameters GooF = S = 1.019; Restrained GooF = 1.019 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0675 * P )^2 + 1.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23573 0.00050 0.000 OSF 2 0.00588 0.00117 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for y Cl63 Max. shift = 0.000 A for H42 Max. dU = 0.000 for C23 Least-squares cycle 8 Maximum vector length = 511 Memory required = 6513 / 674006 wR2 = 0.1751 before cycle 8 for 9380 data and 509 / 509 parameters GooF = S = 1.019; Restrained GooF = 1.019 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0675 * P )^2 + 1.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.23573 0.00050 0.000 OSF 2 0.00588 0.00117 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for y Cl63 Max. shift = 0.000 A for H42 Max. dU = 0.000 for C8 Largest correlation matrix elements 0.523 EXTI / OSF Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2A -0.2334 0.6204 0.3919 137 0.980 0.000 C2 C1 H2A H2B -0.2034 0.6575 0.3120 137 0.980 0.000 C2 C1 H2A H2C -0.0141 0.5961 0.3560 137 0.980 0.000 C2 C1 H2A H3A -0.5915 0.5163 0.3174 137 0.980 0.000 C3 C1 H3A H3B -0.5443 0.6074 0.2822 137 0.980 0.000 C3 C1 H3A H3C -0.5804 0.5798 0.3627 137 0.980 0.000 C3 C1 H3A H5 0.0080 0.6076 0.2384 43 0.950 0.000 C5 C6 C4 H6 0.1360 0.5705 0.1415 43 0.950 0.000 C6 C7 C5 H8 -0.2260 0.3822 0.1830 43 0.950 0.000 C8 C9 C7 H9 -0.3487 0.4181 0.2807 43 0.950 0.000 C9 C8 C4 H11 -0.5197 0.4637 0.4395 43 0.950 0.000 C11 C12 C10 H12 -0.4294 0.3560 0.5334 43 0.950 0.000 C12 C11 C13 H14 0.1849 0.3340 0.4661 43 0.950 0.000 C14 C15 C13 H15 0.0934 0.4422 0.3732 43 0.950 0.000 C15 C14 C10 H1 0.1200 0.4819 0.0737 147 0.840 0.000 O1 C7 H1 H2 -0.1582 0.2599 0.5884 147 0.840 0.000 O2 C13 H2 H22A 0.3596 0.9201 -0.0145 137 0.980 0.000 C22 C21 H22A H22B 0.3887 0.9536 0.0514 137 0.980 0.000 C22 C21 H22A H22C 0.1932 0.9006 0.0469 137 0.980 0.000 C22 C21 H22A H23A 0.7307 0.8505 -0.0041 137 0.980 0.000 C23 C21 H23A H23B 0.8227 0.7980 0.0690 137 0.980 0.000 C23 C21 H23A H23C 0.7640 0.8938 0.0558 137 0.980 0.000 C23 C21 H23A H25 0.1736 0.8108 -0.0160 43 0.950 0.000 C25 C26 C24 H26 0.0787 0.6951 -0.0432 43 0.950 0.000 C26 C27 C25 H28 0.5691 0.5621 0.0772 43 0.950 0.000 C28 C27 C29 H29 0.6572 0.6777 0.1064 43 0.950 0.000 C29 C28 C24 H31 0.1763 0.7708 0.1512 43 0.950 0.000 C31 C32 C30 H32 0.1253 0.7532 0.2670 43 0.950 0.000 C32 C31 C33 H34 0.6982 0.8426 0.2827 43 0.950 0.000 C34 C33 C35 H35 0.7475 0.8602 0.1661 43 0.950 0.000 C35 C34 C30 H21 0.1703 0.5579 -0.0307 147 0.840 0.000 O21 C27 H21 H22 0.4809 0.7954 0.3733 147 0.840 0.000 O22 C33 H22 H42A 0.0384 1.1744 0.3411 137 0.980 0.000 C42 C41 H42A H42B 0.0239 1.1671 0.4212 137 0.980 0.000 C42 C41 H42A H42C -0.0529 1.2514 0.3678 137 0.980 0.000 C42 C41 H42A H43A -0.4005 1.2517 0.4277 137 0.980 0.000 C43 C41 H43A H43B -0.3347 1.1642 0.4778 137 0.980 0.000 C43 C41 H43A H43C -0.5540 1.1808 0.4327 137 0.980 0.000 C43 C41 H43A H45 -0.6197 1.2816 0.3344 43 0.950 0.000 C45 C46 C44 H46 -0.7735 1.3391 0.2273 43 0.950 0.000 C46 C45 C47 H48 -0.3233 1.2033 0.1472 43 0.950 0.000 C48 C49 C47 H49 -0.1712 1.1473 0.2542 43 0.950 0.000 C49 C48 C44 H51 -0.5935 1.0805 0.3583 43 0.950 0.000 C51 C52 C50 H52 -0.6121 0.9421 0.3785 43 0.950 0.000 C52 C53 C51 H54 0.0121 0.9013 0.4461 43 0.950 0.000 C54 C53 C55 H55 0.0288 1.0398 0.4260 43 0.950 0.000 C55 C54 C50 H41 -0.7437 1.3455 0.1120 147 0.840 0.000 O41 C47 H41 H42 -0.1949 0.8012 0.4328 147 0.840 0.000 O42 C53 H42 H61 0.2379 0.9446 0.1828 13 1.000 0.000 C61 Cl62 Cl63 Cl61 s92 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.27389 0.53761 0.33491 1.00000 0.02765 0.02388 0.02845 -0.00262 0.00015 -0.00310 0.02736 0.00441 0.00045 0.00018 0.00014 0.00000 0.00147 0.00161 0.00153 0.00124 0.00119 0.00123 0.00064 C2 -0.17197 0.60941 0.35009 1.00000 0.03288 0.02595 0.03266 -0.00819 0.00293 -0.00394 0.03031 0.00446 0.00048 0.00018 0.00015 0.00000 0.00158 0.00168 0.00164 0.00133 0.00128 0.00130 0.00067 H2A -0.23339 0.62043 0.39190 1.00000 0.04547 0.00000 0.00000 H2B -0.20339 0.65746 0.31201 1.00000 0.04547 0.00000 0.00000 H2C -0.01412 0.59613 0.35604 1.00000 0.04547 0.00000 0.00000 C3 -0.51986 0.56255 0.32324 1.00000 0.02692 0.03171 0.04033 -0.00188 -0.00220 -0.00003 0.03450 0.00488 0.00046 0.00020 0.00016 0.00000 0.00154 0.00183 0.00184 0.00144 0.00132 0.00133 0.00073 H3A -0.59153 0.51628 0.31737 1.00000 0.05176 0.00000 0.00000 H3B -0.54426 0.60741 0.28223 1.00000 0.05176 0.00000 0.00000 H3C -0.58035 0.57982 0.36268 1.00000 0.05176 0.00000 0.00000 C4 -0.18347 0.51641 0.27037 1.00000 0.02507 0.02641 0.02589 -0.00079 -0.00392 -0.00219 0.02686 0.00437 0.00044 0.00018 0.00014 0.00000 0.00142 0.00166 0.00150 0.00123 0.00116 0.00122 0.00064 C5 -0.03942 0.56119 0.22774 1.00000 0.03351 0.02770 0.02738 -0.00484 -0.00204 -0.00738 0.02961 0.00453 0.00047 0.00019 0.00014 0.00000 0.00159 0.00170 0.00155 0.00129 0.00125 0.00132 0.00067 H5 0.00801 0.60761 0.23841 1.00000 0.03553 0.00000 0.00000 C6 0.03638 0.53940 0.16992 1.00000 0.03657 0.03167 0.02533 -0.00219 0.00063 -0.00888 0.03173 0.00457 0.00049 0.00019 0.00015 0.00000 0.00166 0.00180 0.00155 0.00132 0.00127 0.00138 0.00070 H6 0.13601 0.57054 0.14147 1.00000 0.03807 0.00000 0.00000 C7 -0.03165 0.47325 0.15363 1.00000 0.03487 0.03068 0.02370 -0.00667 -0.00583 -0.00068 0.02995 0.00445 0.00048 0.00019 0.00014 0.00000 0.00160 0.00177 0.00151 0.00130 0.00124 0.00136 0.00068 C8 -0.17696 0.42786 0.19456 1.00000 0.03997 0.02933 0.03332 -0.00750 -0.00739 -0.00949 0.03382 0.00459 0.00050 0.00020 0.00016 0.00000 0.00175 0.00177 0.00170 0.00138 0.00137 0.00142 0.00072 H8 -0.22601 0.38219 0.18304 1.00000 0.04059 0.00000 0.00000 C9 -0.24984 0.44970 0.25233 1.00000 0.03280 0.03014 0.02734 -0.00414 -0.00148 -0.00779 0.03033 0.00444 0.00048 0.00019 0.00015 0.00000 0.00157 0.00177 0.00155 0.00131 0.00124 0.00134 0.00068 H9 -0.34869 0.41806 0.28070 1.00000 0.03639 0.00000 0.00000 C10 -0.22438 0.46465 0.39608 1.00000 0.02501 0.02285 0.02736 -0.00747 0.00064 -0.00476 0.02471 0.00414 0.00043 0.00017 0.00014 0.00000 0.00142 0.00158 0.00151 0.00122 0.00116 0.00119 0.00062 C11 -0.37540 0.43756 0.44470 1.00000 0.02370 0.02888 0.02872 -0.01006 0.00107 -0.00089 0.02673 0.00427 0.00045 0.00018 0.00014 0.00000 0.00142 0.00169 0.00155 0.00130 0.00117 0.00123 0.00064 H11 -0.51967 0.46367 0.43953 1.00000 0.03208 0.00000 0.00000 C12 -0.32247 0.37362 0.50056 1.00000 0.02968 0.02768 0.02485 -0.00833 0.00446 -0.00644 0.02688 0.00421 0.00045 0.00018 0.00014 0.00000 0.00153 0.00166 0.00149 0.00126 0.00118 0.00128 0.00064 H12 -0.42940 0.35597 0.53336 1.00000 0.03225 0.00000 0.00000 C13 -0.11315 0.33528 0.50866 1.00000 0.03020 0.02385 0.02141 -0.00721 -0.00415 -0.00253 0.02488 0.00414 0.00045 0.00017 0.00014 0.00000 0.00150 0.00159 0.00141 0.00121 0.00115 0.00123 0.00062 C14 0.04115 0.36060 0.46091 1.00000 0.02095 0.03094 0.03131 -0.00363 0.00084 -0.00022 0.02869 0.00449 0.00045 0.00019 0.00015 0.00000 0.00139 0.00173 0.00160 0.00133 0.00118 0.00123 0.00066 H14 0.18487 0.33398 0.46612 1.00000 0.03443 0.00000 0.00000 C15 -0.01422 0.42461 0.40573 1.00000 0.02538 0.03112 0.02891 -0.00376 0.00397 -0.00559 0.02900 0.00443 0.00045 0.00018 0.00015 0.00000 0.00147 0.00176 0.00157 0.00132 0.00120 0.00129 0.00067 H15 0.09341 0.44219 0.37317 1.00000 0.03480 0.00000 0.00000 O1 0.04414 0.44753 0.09717 1.00000 0.04898 0.03521 0.02585 -0.00993 -0.00067 -0.00817 0.03601 0.00313 0.00036 0.00013 0.00010 0.00000 0.00137 0.00133 0.00113 0.00099 0.00095 0.00104 0.00052 H1 0.12005 0.48191 0.07365 1.00000 0.05401 0.00000 0.00000 O2 -0.05191 0.27000 0.56265 1.00000 0.03129 0.03051 0.02668 -0.00096 0.00326 -0.00345 0.03063 0.00315 0.00032 0.00012 0.00010 0.00000 0.00109 0.00121 0.00109 0.00090 0.00086 0.00092 0.00048 H2 -0.15816 0.25988 0.58838 1.00000 0.04595 0.00000 0.00000 C21 0.49034 0.83124 0.06855 1.00000 0.03027 0.03370 0.02377 -0.00452 0.00194 -0.00976 0.02930 0.00444 0.00047 0.00019 0.00014 0.00000 0.00152 0.00179 0.00148 0.00129 0.00118 0.00133 0.00067 C22 0.34500 0.90826 0.03511 1.00000 0.04418 0.02874 0.02941 -0.00266 -0.00265 -0.00743 0.03469 0.00486 0.00052 0.00019 0.00015 0.00000 0.00182 0.00179 0.00164 0.00135 0.00137 0.00144 0.00073 H22A 0.35964 0.92010 -0.01449 1.00000 0.05203 0.00000 0.00000 H22B 0.38875 0.95357 0.05138 1.00000 0.05203 0.00000 0.00000 H22C 0.19319 0.90061 0.04694 1.00000 0.05203 0.00000 0.00000 C23 0.72284 0.84459 0.04521 1.00000 0.03305 0.04615 0.03133 -0.00746 0.00391 -0.01138 0.03677 0.00491 0.00048 0.00022 0.00016 0.00000 0.00168 0.00211 0.00169 0.00150 0.00134 0.00150 0.00076 H23A 0.73066 0.85047 -0.00406 1.00000 0.05516 0.00000 0.00000 H23B 0.82275 0.79801 0.06898 1.00000 0.05516 0.00000 0.00000 H23C 0.76399 0.89385 0.05575 1.00000 0.05516 0.00000 0.00000 C24 0.42628 0.75708 0.04792 1.00000 0.02596 0.03113 0.02340 -0.00481 0.00405 -0.00230 0.02728 0.00447 0.00045 0.00019 0.00014 0.00000 0.00144 0.00173 0.00144 0.00125 0.00115 0.00127 0.00065 C25 0.25458 0.76011 0.00358 1.00000 0.03291 0.03203 0.02444 -0.00528 0.00391 -0.00423 0.03009 0.00452 0.00047 0.00019 0.00014 0.00000 0.00160 0.00179 0.00151 0.00131 0.00124 0.00134 0.00068 H25 0.17363 0.81078 -0.01603 1.00000 0.03611 0.00000 0.00000 C26 0.19786 0.69140 -0.01291 1.00000 0.03696 0.04097 0.02214 -0.00892 0.00258 -0.00821 0.03291 0.00474 0.00050 0.00020 0.00015 0.00000 0.00168 0.00201 0.00149 0.00138 0.00126 0.00147 0.00072 H26 0.07871 0.69506 -0.04323 1.00000 0.03949 0.00000 0.00000 C27 0.31393 0.61803 0.01457 1.00000 0.04159 0.03151 0.02830 -0.01125 0.00639 -0.00765 0.03289 0.00469 0.00051 0.00019 0.00015 0.00000 0.00178 0.00185 0.00160 0.00138 0.00136 0.00146 0.00072 C28 0.48699 0.61281 0.05858 1.00000 0.04505 0.03048 0.03531 -0.00754 0.00362 0.00370 0.03765 0.00509 0.00053 0.00020 0.00016 0.00000 0.00188 0.00187 0.00178 0.00146 0.00146 0.00149 0.00077 H28 0.56915 0.56212 0.07723 1.00000 0.04518 0.00000 0.00000 C29 0.53989 0.68186 0.07530 1.00000 0.03380 0.04321 0.02906 -0.01213 -0.00404 -0.00068 0.03503 0.00484 0.00050 0.00020 0.00015 0.00000 0.00166 0.00206 0.00164 0.00147 0.00130 0.00147 0.00074 H29 0.65723 0.67770 0.10640 1.00000 0.04204 0.00000 0.00000 C30 0.46824 0.81694 0.14596 1.00000 0.02485 0.02416 0.02612 -0.00360 0.00239 -0.00416 0.02544 0.00431 0.00044 0.00018 0.00014 0.00000 0.00140 0.00157 0.00148 0.00121 0.00115 0.00119 0.00062 C31 0.28382 0.78529 0.17790 1.00000 0.02455 0.02898 0.03016 -0.00809 0.00006 -0.00475 0.02765 0.00444 0.00045 0.00018 0.00015 0.00000 0.00143 0.00171 0.00159 0.00130 0.00119 0.00124 0.00065 H31 0.17629 0.77084 0.15125 1.00000 0.03318 0.00000 0.00000 C32 0.25299 0.77440 0.24663 1.00000 0.02855 0.02814 0.02816 -0.00544 0.00576 -0.00728 0.02831 0.00445 0.00046 0.00018 0.00015 0.00000 0.00149 0.00170 0.00156 0.00128 0.00122 0.00128 0.00066 H32 0.12534 0.75322 0.26703 1.00000 0.03397 0.00000 0.00000 C33 0.40976 0.79460 0.28576 1.00000 0.02851 0.02156 0.02379 -0.00505 0.00295 -0.00315 0.02472 0.00425 0.00045 0.00017 0.00014 0.00000 0.00145 0.00155 0.00145 0.00118 0.00115 0.00120 0.00061 C34 0.59255 0.82738 0.25584 1.00000 0.02767 0.03077 0.02768 -0.00942 -0.00136 -0.00597 0.02813 0.00440 0.00046 0.00018 0.00015 0.00000 0.00148 0.00174 0.00154 0.00130 0.00120 0.00127 0.00065 H34 0.69817 0.84256 0.28268 1.00000 0.03375 0.00000 0.00000 C35 0.62093 0.83800 0.18643 1.00000 0.02738 0.02949 0.02880 -0.00417 0.00371 -0.00853 0.02876 0.00441 0.00046 0.00018 0.00015 0.00000 0.00147 0.00172 0.00157 0.00129 0.00121 0.00127 0.00066 H35 0.74752 0.86016 0.16610 1.00000 0.03451 0.00000 0.00000 O21 0.26032 0.54704 0.00201 1.00000 0.05705 0.03432 0.03680 -0.01392 -0.00368 -0.00773 0.04160 0.00332 0.00039 0.00014 0.00011 0.00000 0.00152 0.00135 0.00132 0.00105 0.00107 0.00111 0.00057 H21 0.17026 0.55786 -0.03066 1.00000 0.06240 0.00000 0.00000 O22 0.37576 0.78120 0.35473 1.00000 0.03324 0.03424 0.02253 -0.00499 0.00045 -0.01080 0.02988 0.00298 0.00032 0.00013 0.00009 0.00000 0.00111 0.00126 0.00104 0.00089 0.00084 0.00094 0.00048 H22 0.48088 0.79536 0.37331 1.00000 0.04483 0.00000 0.00000 C41 -0.27794 1.16709 0.37641 1.00000 0.02710 0.03099 0.03243 -0.01243 0.00044 -0.00612 0.02916 0.00430 0.00045 0.00019 0.00015 0.00000 0.00149 0.00176 0.00162 0.00135 0.00122 0.00129 0.00067 C42 -0.04608 1.19230 0.37666 1.00000 0.03443 0.03575 0.04954 -0.01284 -0.00259 -0.00790 0.03922 0.00480 0.00049 0.00021 0.00018 0.00000 0.00174 0.00195 0.00205 0.00159 0.00149 0.00147 0.00079 H42A 0.03843 1.17443 0.34110 1.00000 0.05883 0.00000 0.00000 H42B 0.02394 1.16712 0.42121 1.00000 0.05883 0.00000 0.00000 H42C -0.05295 1.25139 0.36783 1.00000 0.05883 0.00000 0.00000 C43 -0.40299 1.19330 0.43381 1.00000 0.03900 0.03700 0.03444 -0.01632 -0.00259 -0.00394 0.03548 0.00468 0.00051 0.00020 0.00016 0.00000 0.00175 0.00193 0.00174 0.00149 0.00137 0.00146 0.00074 H43A -0.40053 1.25175 0.42772 1.00000 0.05322 0.00000 0.00000 H43B -0.33467 1.16417 0.47779 1.00000 0.05322 0.00000 0.00000 H43C -0.55397 1.18080 0.43274 1.00000 0.05322 0.00000 0.00000 C44 -0.38037 1.20734 0.30665 1.00000 0.02767 0.02435 0.03387 -0.00745 -0.00040 -0.00536 0.02843 0.00435 0.00046 0.00018 0.00015 0.00000 0.00149 0.00164 0.00165 0.00131 0.00124 0.00125 0.00066 C45 -0.55902 1.26504 0.29632 1.00000 0.03456 0.02956 0.03624 -0.00756 0.00436 -0.00714 0.03335 0.00473 0.00049 0.00019 0.00016 0.00000 0.00166 0.00178 0.00174 0.00141 0.00134 0.00138 0.00071 H45 -0.61965 1.28158 0.33441 1.00000 0.04002 0.00000 0.00000 C46 -0.65178 1.29927 0.23278 1.00000 0.03251 0.02999 0.04047 -0.00197 0.00068 0.00189 0.03595 0.00503 0.00051 0.00020 0.00016 0.00000 0.00163 0.00183 0.00186 0.00145 0.00138 0.00138 0.00074 H46 -0.77352 1.33909 0.22730 1.00000 0.04314 0.00000 0.00000 C47 -0.56643 1.27525 0.17698 1.00000 0.04325 0.03258 0.03202 0.00067 -0.00171 -0.00930 0.03717 0.00497 0.00053 0.00020 0.00016 0.00000 0.00186 0.00188 0.00173 0.00142 0.00141 0.00152 0.00076 C48 -0.38525 1.21901 0.18545 1.00000 0.05046 0.02978 0.03204 -0.00665 0.00599 -0.00652 0.03751 0.00505 0.00054 0.00019 0.00016 0.00000 0.00200 0.00186 0.00174 0.00142 0.00147 0.00156 0.00077 H48 -0.32328 1.20332 0.14715 1.00000 0.04501 0.00000 0.00000 C49 -0.29541 1.18599 0.24908 1.00000 0.03443 0.02876 0.03619 -0.00715 -0.00096 -0.00050 0.03352 0.00470 0.00050 0.00019 0.00015 0.00000 0.00164 0.00176 0.00177 0.00140 0.00135 0.00135 0.00071 H49 -0.17120 1.14730 0.25417 1.00000 0.04022 0.00000 0.00000 C50 -0.27802 1.07551 0.38914 1.00000 0.02764 0.03095 0.02245 -0.00661 0.00000 -0.00422 0.02696 0.00429 0.00045 0.00018 0.00014 0.00000 0.00148 0.00173 0.00145 0.00126 0.00116 0.00127 0.00065 C51 -0.46889 1.04417 0.37589 1.00000 0.02469 0.03111 0.03902 -0.00647 -0.00140 0.00043 0.03227 0.00464 0.00047 0.00019 0.00016 0.00000 0.00148 0.00185 0.00178 0.00142 0.00127 0.00130 0.00071 H51 -0.59349 1.08051 0.35825 1.00000 0.03873 0.00000 0.00000 C52 -0.48075 0.96205 0.38774 1.00000 0.02580 0.02843 0.04231 -0.00767 -0.00161 -0.00653 0.03214 0.00463 0.00047 0.00019 0.00016 0.00000 0.00151 0.00179 0.00183 0.00141 0.00131 0.00130 0.00070 H52 -0.61211 0.94210 0.37853 1.00000 0.03856 0.00000 0.00000 C53 -0.30062 0.90919 0.41304 1.00000 0.03019 0.02343 0.02249 -0.00382 0.00071 -0.00208 0.02578 0.00432 0.00045 0.00018 0.00014 0.00000 0.00152 0.00162 0.00144 0.00119 0.00116 0.00123 0.00063 C54 -0.11126 0.93799 0.42777 1.00000 0.02890 0.03226 0.02584 -0.00425 -0.00684 -0.00023 0.02974 0.00442 0.00047 0.00019 0.00014 0.00000 0.00153 0.00182 0.00153 0.00130 0.00121 0.00130 0.00068 H54 0.01208 0.90132 0.44609 1.00000 0.03569 0.00000 0.00000 C55 -0.10216 1.02040 0.41574 1.00000 0.02726 0.03065 0.02753 -0.00599 -0.00515 -0.00642 0.02846 0.00439 0.00046 0.00018 0.00014 0.00000 0.00148 0.00178 0.00155 0.00130 0.00119 0.00128 0.00066 H55 0.02882 1.03981 0.42604 1.00000 0.03415 0.00000 0.00000 O41 -0.65471 1.30480 0.11285 1.00000 0.05946 0.04970 0.03140 -0.00118 -0.00452 0.00449 0.04921 0.00399 0.00042 0.00016 0.00011 0.00000 0.00163 0.00166 0.00125 0.00112 0.00110 0.00124 0.00063 H41 -0.74372 1.34551 0.11198 1.00000 0.07381 0.00000 0.00000 O42 -0.31790 0.82719 0.42267 1.00000 0.02927 0.02666 0.03223 -0.00441 -0.00451 -0.00119 0.03004 0.00297 0.00031 0.00012 0.00010 0.00000 0.00107 0.00119 0.00113 0.00091 0.00089 0.00088 0.00047 H42 -0.19489 0.80117 0.43277 1.00000 0.04506 0.00000 0.00000 C61 0.15315 0.99515 0.18866 1.00000 0.03745 0.02909 0.03769 -0.00937 -0.00030 -0.00192 0.03469 0.00477 0.00051 0.00020 0.00016 0.00000 0.00168 0.00180 0.00177 0.00142 0.00138 0.00139 0.00072 H61 0.23791 0.94455 0.18279 1.00000 0.04163 0.00000 0.00000 Cl61 0.02590 0.97305 0.26801 1.00000 0.04823 0.04356 0.03678 -0.00962 0.00608 0.00136 0.04343 0.00137 0.00014 0.00005 0.00004 0.00000 0.00049 0.00052 0.00046 0.00038 0.00036 0.00039 0.00024 Cl62 0.33150 1.06819 0.18502 1.00000 0.06371 0.06883 0.06811 -0.01255 -0.00019 -0.03501 0.06575 0.00152 0.00017 0.00007 0.00006 0.00000 0.00064 0.00075 0.00068 0.00055 0.00051 0.00056 0.00032 Cl63 -0.04398 1.02799 0.12313 1.00000 0.05301 0.04998 0.04090 -0.00534 -0.01289 -0.00089 0.04933 0.00138 0.00015 0.00006 0.00004 0.00000 0.00053 0.00058 0.00049 0.00041 0.00039 0.00043 0.00026 Final Structure Factor Calculation for s92 in P-1 Total number of l.s. parameters = 509 Maximum vector length = 511 Memory required = 6004 / 22995 wR2 = 0.1751 before cycle 9 for 9380 data and 0 / 509 parameters GooF = S = 1.019; Restrained GooF = 1.019 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0675 * P )^2 + 1.10 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0671 for 5546 Fo > 4sig(Fo) and 0.1275 for all 9380 data wR2 = 0.1751, GooF = S = 1.019, Restrained GooF = 1.019 for all data Occupancy sum of asymmetric unit = 55.00 for non-hydrogen and 49.00 for hydrogen atoms Principal mean square atomic displacements U 0.0322 0.0276 0.0223 C1 0.0351 0.0304 0.0255 C2 0.0470 0.0319 0.0246 C3 0.0347 0.0260 0.0198 C4 0.0373 0.0265 0.0250 C5 0.0410 0.0313 0.0229 C6 0.0383 0.0306 0.0209 C7 0.0478 0.0309 0.0228 C8 0.0381 0.0273 0.0256 C9 0.0275 0.0260 0.0206 C10 0.0312 0.0265 0.0225 C11 0.0331 0.0250 0.0225 C12 0.0323 0.0241 0.0183 C13 0.0375 0.0280 0.0206 C14 0.0354 0.0299 0.0217 C15 0.0498 0.0341 0.0241 O1 0.0381 0.0313 0.0225 O2 0.0389 0.0269 0.0221 C21 0.0465 0.0324 0.0252 C22 0.0494 0.0339 0.0270 C23 0.0334 0.0277 0.0208 C24 0.0342 0.0330 0.0230 C25 0.0432 0.0341 0.0214 C26 0.0443 0.0301 0.0243 C27 0.0508 0.0345 0.0276 C28 0.0450 0.0346 0.0254 C29 0.0292 0.0260 0.0211 C30 0.0303 0.0293 0.0233 C31 0.0336 0.0303 0.0210 C32 0.0296 0.0234 0.0212 C33 0.0323 0.0295 0.0226 C34 0.0344 0.0313 0.0207 C35 0.0583 0.0395 0.0270 O21 0.0413 0.0259 0.0224 O22 0.0354 0.0290 0.0230 C41 0.0503 0.0390 0.0283 C42 0.0430 0.0385 0.0249 C43 0.0343 0.0288 0.0222 C44 0.0391 0.0341 0.0268 C45 0.0474 0.0348 0.0257 C46 0.0494 0.0374 0.0247 C47 0.0518 0.0324 0.0283 C48 0.0372 0.0355 0.0279 C49 0.0315 0.0272 0.0223 C50 0.0406 0.0328 0.0234 C51 0.0435 0.0306 0.0223 C52 0.0304 0.0256 0.0213 C53 0.0352 0.0343 0.0198 C54 0.0363 0.0286 0.0205 C55 0.0677 0.0519 0.0280 O41 0.0369 0.0293 0.0240 O42 0.0387 0.0368 0.0285 C61 0.0558 0.0407 0.0337 Cl61 0.0953 0.0675 0.0344 Cl62 0.0624 0.0541 0.0315 Cl63 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.009 0.017 0.026 0.036 0.047 0.061 0.077 0.101 0.155 1.000 Number in group 1012. 885. 935. 973. 890. 993. 889. 921. 943. 939. GooF 0.947 0.986 0.949 1.006 1.039 1.034 1.122 1.051 1.070 0.983 K 7.036 1.774 1.131 1.010 1.002 1.001 1.000 1.020 1.020 1.001 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.66 inf Number in group 962. 946. 911. 947. 950. 927. 928. 928. 938. 943. GooF 0.910 0.969 0.974 1.024 1.012 1.007 1.008 0.975 1.049 1.231 K 0.976 1.058 1.087 1.088 1.027 1.027 1.018 1.019 1.025 0.991 R1 0.366 0.309 0.269 0.218 0.154 0.123 0.086 0.064 0.058 0.045 Recommended weighting scheme: WGHT 0.0667 1.1039 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 9 0 65.48 2.53 6.13 0.009 1.83 0 3 6 70.69 24.47 5.10 0.029 3.19 -3 0 6 198.58 38.61 4.58 0.037 1.75 2 -2 5 38.29 3.34 4.46 0.011 2.17 0 -6 3 107.37 51.69 4.44 0.043 2.33 -3 -6 6 60.69 3.95 4.12 0.012 1.45 3 9 3 106.02 0.20 4.10 0.003 1.47 0 -3 9 141.34 72.01 4.05 0.050 1.87 0 -3 6 55.34 11.78 3.99 0.020 2.54 -3 -1 3 225.23 139.39 3.95 0.070 1.96 -1 1 0 3910.57 8250.42 3.86 0.538 5.57 -3 0 9 711.40 500.71 3.86 0.132 1.51 0 13 0 387.26 245.44 3.75 0.093 1.27 -4 1 0 265.79 159.96 3.73 0.075 1.52 1 1 0 876.25 1296.48 3.69 0.213 5.96 -2 10 17 26.49 71.75 3.68 0.050 1.01 0 7 0 55.11 12.57 3.68 0.021 2.36 4 13 3 191.14 312.25 3.64 0.105 1.05 3 -2 14 6.53 43.65 3.64 0.039 1.10 0 -7 8 62.44 112.89 3.56 0.063 1.52 -3 3 12 339.14 232.81 3.51 0.090 1.30 -1 5 7 332.31 222.62 3.49 0.088 2.24 6 -7 5 115.66 5.55 3.49 0.014 0.86 3 -3 9 53.21 0.04 3.48 0.001 1.35 -4 7 1 90.65 162.67 3.47 0.076 1.24 3 4 21 225.13 111.19 3.44 0.062 0.88 -2 14 20 582.42 324.99 3.44 0.107 0.82 -1 19 8 209.86 106.54 3.35 0.061 0.87 -4 16 3 62.70 182.12 3.30 0.080 0.83 2 15 5 76.80 12.62 3.30 0.021 1.10 -1 9 22 -11.22 37.85 3.30 0.036 0.88 -4 14 6 37.44 168.31 3.29 0.077 0.91 0 12 1 117.04 65.09 3.26 0.048 1.40 -6 4 7 54.81 116.48 3.22 0.064 0.94 5 13 7 245.98 113.87 3.22 0.063 0.93 7 3 10 -5.36 43.73 3.18 0.039 0.81 3 -3 17 87.83 156.03 3.18 0.074 0.94 -2 1 23 133.65 246.26 3.16 0.093 0.83 -5 8 14 54.74 126.92 3.16 0.067 0.88 -3 3 0 121.86 35.81 3.15 0.035 1.86 -4 8 6 44.08 3.64 3.13 0.011 1.17 6 5 0 591.64 441.45 3.13 0.124 1.01 -5 -4 1 21.92 0.15 3.13 0.002 1.21 -3 3 9 560.69 388.91 3.09 0.117 1.49 6 12 0 96.69 28.75 3.07 0.032 0.87 -3 -6 2 414.57 296.67 3.06 0.102 1.66 5 7 2 83.68 31.44 3.06 0.033 1.15 2 14 15 9.82 57.19 3.06 0.045 0.98 1 16 10 42.76 104.42 3.05 0.060 1.03 5 9 3 96.31 151.35 3.03 0.073 1.08 Bond lengths and angles C1 - Distance Angles C10 1.5295 (0.0042) C4 1.5318 (0.0041) 109.39 (0.24) C2 1.5367 (0.0041) 107.62 (0.23) 112.33 (0.24) C3 1.5397 (0.0040) 112.26 (0.25) 107.75 (0.24) 107.54 (0.25) C1 - C10 C4 C2 C2 - Distance Angles C1 1.5367 (0.0041) H2A 0.9800 109.47 H2B 0.9800 109.47 109.47 H2C 0.9800 109.47 109.47 109.47 C2 - C1 H2A H2B C3 - Distance Angles C1 1.5397 (0.0040) H3A 0.9800 109.47 H3B 0.9800 109.47 109.47 H3C 0.9800 109.47 109.47 109.47 C3 - C1 H3A H3B C4 - Distance Angles C5 1.3858 (0.0042) C9 1.3862 (0.0042) 117.39 (0.27) C1 1.5318 (0.0041) 123.52 (0.27) 119.08 (0.26) C4 - C5 C9 C5 - Distance Angles C6 1.3829 (0.0042) C4 1.3858 (0.0042) 121.06 (0.29) H5 0.9500 119.47 119.47 C5 - C6 C4 C6 - Distance Angles C7 1.3648 (0.0043) C5 1.3829 (0.0042) 120.14 (0.29) H6 0.9500 119.93 119.93 C6 - C7 C5 C7 - Distance Angles C6 1.3648 (0.0043) C8 1.3801 (0.0045) 120.28 (0.28) O1 1.3896 (0.0036) 122.37 (0.28) 117.33 (0.27) C7 - C6 C8 C8 - Distance Angles C9 1.3767 (0.0043) C7 1.3801 (0.0045) 119.08 (0.29) H8 0.9500 120.46 120.46 C8 - C9 C7 C9 - Distance Angles C8 1.3767 (0.0043) C4 1.3862 (0.0042) 122.05 (0.29) H9 0.9500 118.98 118.98 C9 - C8 C4 C10 - Distance Angles C11 1.3788 (0.0041) C15 1.3964 (0.0040) 117.26 (0.27) C1 1.5295 (0.0042) 123.33 (0.26) 119.36 (0.26) C10 - C11 C15 C11 - Distance Angles C12 1.3768 (0.0043) C10 1.3788 (0.0041) 121.70 (0.27) H11 0.9500 119.15 119.15 C11 - C12 C10 C12 - Distance Angles C11 1.3768 (0.0043) C13 1.3809 (0.0041) 119.65 (0.27) H12 0.9500 120.17 120.17 C12 - C11 C13 C13 - Distance Angles C14 1.3756 (0.0042) O2 1.3763 (0.0036) 117.60 (0.26) C12 1.3809 (0.0040) 120.10 (0.27) 122.27 (0.26) C13 - C14 O2 C14 - Distance Angles C15 1.3715 (0.0043) C13 1.3756 (0.0042) 119.45 (0.27) H14 0.9500 120.28 120.28 C14 - C15 C13 C15 - Distance Angles C14 1.3715 (0.0043) C10 1.3964 (0.0040) 121.84 (0.27) H15 0.9500 119.08 119.08 C15 - C14 C10 O1 - Distance Angles C7 1.3896 (0.0036) H1 0.8400 109.47 O1 - C7 O2 - Distance Angles C13 1.3763 (0.0036) H2 0.8400 109.47 O2 - C13 C21 - Distance Angles C22 1.5246 (0.0045) C24 1.5246 (0.0043) 112.60 (0.24) C23 1.5304 (0.0042) 107.36 (0.26) 108.30 (0.25) C30 1.5338 (0.0040) 107.54 (0.25) 108.66 (0.24) 112.44 (0.24) C21 - C22 C24 C23 C22 - Distance Angles C21 1.5246 (0.0045) H22A 0.9800 109.47 H22B 0.9800 109.47 109.47 H22C 0.9800 109.47 109.47 109.47 C22 - C21 H22A H22B C23 - Distance Angles C21 1.5304 (0.0042) H23A 0.9800 109.47 H23B 0.9800 109.47 109.47 H23C 0.9800 109.47 109.47 109.47 C23 - C21 H23A H23B C24 - Distance Angles C25 1.3848 (0.0041) C29 1.3869 (0.0045) 117.14 (0.29) C21 1.5246 (0.0043) 123.23 (0.28) 119.62 (0.26) C24 - C25 C29 C25 - Distance Angles C26 1.3819 (0.0044) C24 1.3848 (0.0041) 121.75 (0.30) H25 0.9500 119.12 119.12 C25 - C26 C24 C26 - Distance Angles C27 1.3692 (0.0046) C25 1.3819 (0.0044) 119.80 (0.29) H26 0.9500 120.10 120.10 C26 - C27 C25 C27 - Distance Angles C26 1.3692 (0.0046) O21 1.3777 (0.0037) 122.44 (0.28) C28 1.3796 (0.0045) 120.04 (0.30) 117.48 (0.30) C27 - C26 O21 C28 - Distance Angles C27 1.3796 (0.0045) C29 1.3817 (0.0046) 119.49 (0.31) H28 0.9500 120.26 120.26 C28 - C27 C29 C29 - Distance Angles C28 1.3817 (0.0046) C24 1.3869 (0.0045) 121.77 (0.29) H29 0.9500 119.12 119.12 C29 - C28 C24 C30 - Distance Angles C35 1.3881 (0.0040) C31 1.3962 (0.0040) 117.34 (0.26) C21 1.5338 (0.0040) 122.58 (0.25) 120.00 (0.25) C30 - C35 C31 C31 - Distance Angles C32 1.3732 (0.0040) C30 1.3962 (0.0040) 122.06 (0.27) H31 0.9500 118.97 118.97 C31 - C32 C30 C32 - Distance Angles C31 1.3732 (0.0040) C33 1.3816 (0.0040) 119.23 (0.27) H32 0.9500 120.38 120.38 C32 - C31 C33 C33 - Distance Angles O22 1.3769 (0.0033) C34 1.3806 (0.0041) 121.94 (0.25) C32 1.3816 (0.0040) 117.66 (0.25) 120.39 (0.26) C33 - O22 C34 C34 - Distance Angles C33 1.3806 (0.0041) C35 1.3852 (0.0041) 119.58 (0.26) H34 0.9500 120.21 120.21 C34 - C33 C35 C35 - Distance Angles C34 1.3852 (0.0041) C30 1.3881 (0.0040) 121.36 (0.27) H35 0.9500 119.32 119.32 C35 - C34 C30 O21 - Distance Angles C27 1.3777 (0.0037) H21 0.8400 109.47 O21 - C27 O22 - Distance Angles C33 1.3769 (0.0033) H22 0.8400 109.47 O22 - C33 C41 - Distance Angles C44 1.5195 (0.0043) C50 1.5258 (0.0043) 108.62 (0.24) C43 1.5280 (0.0042) 112.44 (0.25) 107.91 (0.25) C42 1.5386 (0.0041) 107.75 (0.26) 111.99 (0.26) 108.19 (0.25) C41 - C44 C50 C43 C42 - Distance Angles C41 1.5386 (0.0041) H42A 0.9800 109.47 H42B 0.9800 109.47 109.47 H42C 0.9800 109.47 109.47 109.47 C42 - C41 H42A H42B C43 - Distance Angles C41 1.5280 (0.0042) H43A 0.9800 109.47 H43B 0.9800 109.47 109.47 H43C 0.9800 109.47 109.47 109.47 C43 - C41 H43A H43B C44 - Distance Angles C45 1.3846 (0.0043) C49 1.3933 (0.0043) 116.70 (0.28) C41 1.5195 (0.0043) 123.40 (0.28) 119.89 (0.27) C44 - C45 C49 C45 - Distance Angles C46 1.3761 (0.0045) C44 1.3846 (0.0043) 122.27 (0.30) H45 0.9500 118.86 118.86 C45 - C46 C44 C46 - Distance Angles C45 1.3761 (0.0045) C47 1.3826 (0.0046) 119.48 (0.30) H46 0.9500 120.26 120.26 C46 - C45 C47 C47 - Distance Angles O41 1.3665 (0.0039) C48 1.3826 (0.0047) 117.88 (0.30) C46 1.3826 (0.0046) 122.54 (0.31) 119.58 (0.30) C47 - O41 C48 C48 - Distance Angles C49 1.3679 (0.0044) C47 1.3826 (0.0047) 119.87 (0.31) H48 0.9500 120.07 120.07 C48 - C49 C47 C49 - Distance Angles C48 1.3679 (0.0044) C44 1.3933 (0.0043) 122.06 (0.30) H49 0.9500 118.97 118.97 C49 - C48 C44 C50 - Distance Angles C55 1.3806 (0.0042) C51 1.4001 (0.0041) 117.12 (0.28) C41 1.5258 (0.0043) 123.88 (0.25) 118.96 (0.26) C50 - C55 C51 C51 - Distance Angles C52 1.3767 (0.0044) C50 1.4001 (0.0041) 121.73 (0.29) H51 0.9500 119.14 119.14 C51 - C52 C50 C52 - Distance Angles C53 1.3752 (0.0042) C51 1.3767 (0.0044) 119.37 (0.27) H52 0.9500 120.32 120.32 C52 - C53 C51 C53 - Distance Angles C52 1.3752 (0.0042) C54 1.3788 (0.0041) 120.38 (0.28) O42 1.3850 (0.0035) 117.51 (0.25) 122.11 (0.27) C53 - C52 C54 C54 - Distance Angles C53 1.3788 (0.0040) C55 1.3789 (0.0043) 119.53 (0.28) H54 0.9500 120.23 120.23 C54 - C53 C55 C55 - Distance Angles C54 1.3789 (0.0043) C50 1.3806 (0.0042) 121.86 (0.27) H55 0.9500 119.07 119.07 C55 - C54 C50 O41 - Distance Angles C47 1.3665 (0.0039) H41 0.8400 109.47 O41 - C47 O42 - Distance Angles C53 1.3850 (0.0035) H42 0.8400 109.47 O42 - C53 C61 - Distance Angles Cl62 1.7387 (0.0034) Cl63 1.7533 (0.0034) 110.65 (0.19) Cl61 1.7560 (0.0034) 110.53 (0.18) 109.80 (0.18) H61 1.0000 108.60 108.60 108.60 C61 - Cl62 Cl63 Cl61 Cl61 - Distance Angles C61 1.7560 (0.0034) Cl61 - Cl62 - Distance Angles C61 1.7387 (0.0034) Cl62 - Cl63 - Distance Angles C61 1.7533 (0.0035) Cl63 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.86 2.679(4) 164.0 O1-H1...O21 0.84 1.84 2.673(3) 169.8 O2-H2...O22_$1 0.84 1.92 2.743(3) 164.8 O21-H21...O1_$2 0.84 1.81 2.646(3) 172.1 O22-H22...O42_$3 0.84 2.03 2.870(4) 172.9 O41-H41...O1_$4 0.84 1.84 2.659(3) 164.2 O42-H42...O2_$1 FMAP and GRID set by program FMAP 2 2 78 GRID -1.333 -1 -2 1.333 1 2 R1 = 0.1268 for 9380 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.36 at 0.3870 0.5366 0.0250 [ 0.89 A from O21 ] Deepest hole -0.39 at 0.0809 0.0097 0.1160 [ 0.83 A from CL63 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 5535 / 60375 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.3870 0.5366 0.0250 1.00000 0.05 0.36 0.89 O21 1.39 C27 1.71 H21 1.71 H28 Q2 1 -0.1445 0.9357 0.3137 1.00000 0.05 0.34 1.48 CL61 2.17 H34 2.19 C53 2.33 C54 Q3 1 -0.0844 0.9835 0.2294 1.00000 0.05 0.31 1.01 CL61 1.68 C61 2.12 CL63 2.31 H61 Q4 1 0.0734 1.0089 0.1556 1.00000 0.05 0.29 0.81 C61 0.96 CL63 1.42 H61 2.14 CL62 Q5 1 -0.3364 0.6694 0.2806 1.00000 0.05 0.28 1.02 H2B 1.74 H3B 1.78 C2 2.24 C3 Shortest distances between peaks (including symmetry equivalents) 2 3 1.75 3 4 1.76 1 1 2.19 Time profile in seconds ----------------------- 0.14: 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. 3.02: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.09: Set up l.s. refinement 0.00: Generate idealized H-atoms 12.67: Structure factors and derivatives 43.88: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 4.28: Solve l.s. equations 0.00: Generate HTAB table 0.11: Other dependent quantities, CIF, tables 0.36: Analysis of variance 0.11: Merge reflections for Fourier and .fcf 0.19: Fourier summations 0.11: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 10:51:23 Total CPU time: 65.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++