+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXH-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 14:02:09 on 19-Jun-2003 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL s92 in P-1 CELL 0.71073 8.9162 11.0761 23.8610 80.144 87.570 77.550 ZERR 1.00 0.0002 0.0002 0.0005 0.001 0.001 0.001 LATT 1 SFAC C H N S CR UNIT 70 56 12 32 2 V = 2267.02 F(000) = 1120.0 Mu = 1.03 mm-1 Cell Wt = 2195.19 Rho = 1.608 MERG 2 OMIT -3.00 55.00 OMIT 1 -2 3 FMAP 2 PLAN 10 SIZE 0.08 0.42 0.50 ACTA BOND $H WGHT 0.05530 2.26430 L.S. 11 TEMP 27.00 FVAR 0.34425 MOLE 1 C1 1 1.295062 -0.519800 0.763327 11.00000 0.12764 0.12725 = 0.05383 -0.03298 -0.00413 0.01844 AFIX 23 H1A 2 1.201405 -0.455913 0.762689 11.00000 -1.20000 H1B 2 1.325375 -0.525688 0.724197 11.00000 -1.20000 AFIX 0 C2 1 1.262888 -0.638786 0.790610 11.00000 0.08379 0.15046 = 0.08168 -0.07069 0.00538 -0.02220 AFIX 23 H2A 2 1.357674 -0.701632 0.791921 11.00000 -1.20000 H2B 2 1.191915 -0.662093 0.766804 11.00000 -1.20000 AFIX 0 C3 1 1.261299 -0.537133 0.888075 11.00000 0.06927 0.06910 = 0.04732 -0.02505 -0.00130 -0.01448 C4 1 1.361883 -0.470170 0.865294 11.00000 0.07456 0.07709 = 0.05297 -0.02733 0.00818 -0.01384 C5 1 1.302375 -0.407004 0.963944 11.00000 0.06465 0.06060 = 0.04452 -0.01597 -0.00050 -0.01232 C6 1 1.297161 -0.354151 1.011342 11.00000 0.07079 0.06055 = 0.04256 -0.01627 0.00077 -0.01680 C7 1 1.331289 -0.214811 1.083822 11.00000 0.05944 0.05884 = 0.04755 -0.01970 0.00172 -0.01143 C8 1 1.220275 -0.273502 1.105959 11.00000 0.08214 0.05876 = 0.04488 -0.01856 0.00654 -0.02328 C9 1 1.252408 -0.202541 1.206693 11.00000 0.15120 0.21646 = 0.06478 -0.06621 0.03601 -0.12641 AFIX 23 H9A 2 1.195583 -0.166856 1.237663 11.00000 -1.20000 H9B 2 1.327133 -0.275310 1.223930 11.00000 -1.20000 AFIX 0 C10 1 1.330441 -0.119956 1.181336 11.00000 0.15510 0.15883 = 0.07208 -0.05351 0.02793 -0.09685 AFIX 23 H10A 2 1.413718 -0.124550 1.207013 11.00000 -1.20000 H10B 2 1.262813 -0.038743 1.181658 11.00000 -1.20000 AFIX 0 S1 4 1.445044 -0.470115 0.797668 11.00000 0.14484 0.13056 = 0.07459 -0.05287 0.05189 -0.06424 S2 4 1.185727 -0.645093 0.859729 11.00000 0.12870 0.10429 = 0.08678 -0.05711 0.00557 -0.04329 S3 4 1.193019 -0.515235 0.955344 11.00000 0.09729 0.08343 = 0.04919 -0.02543 0.01082 -0.04032 S4 4 1.415669 -0.369644 0.905738 11.00000 0.08311 0.09440 = 0.05705 -0.02900 0.01302 -0.03887 S5 4 1.410943 -0.249425 1.019199 11.00000 0.06940 0.08837 = 0.05463 -0.03222 0.01128 -0.02883 S6 4 1.175080 -0.382802 1.068298 11.00000 0.12064 0.08457 = 0.05286 -0.03155 0.02113 -0.05687 S7 4 1.120935 -0.258791 1.169490 11.00000 0.11725 0.13308 = 0.05767 -0.04540 0.03075 -0.07508 S8 4 1.413936 -0.111266 1.112967 11.00000 0.08848 0.08525 = 0.05770 -0.02970 0.01019 -0.04257 MOLE 2 C11 1 0.987057 -0.036209 0.980713 11.00000 0.05203 0.06459 = 0.04348 -0.01433 -0.00131 -0.01536 C12 1 0.878053 -0.178689 0.926748 11.00000 0.05773 0.05700 = 0.04509 -0.01509 -0.00302 -0.01628 C13 1 0.994457 -0.146224 0.894328 11.00000 0.05110 0.05859 = 0.04522 -0.01795 -0.00316 -0.01223 C14 1 0.927707 -0.287672 0.819259 11.00000 0.09243 0.17613 = 0.10869 -0.09721 0.01481 -0.05490 AFIX 23 H14A 2 0.922797 -0.289299 0.778869 11.00000 -1.20000 H14B 2 0.979086 -0.371042 0.836921 11.00000 -1.20000 AFIX 0 C15 1 0.775633 -0.268087 0.839921 11.00000 0.07951 0.12994 = 0.07037 -0.04329 0.00869 -0.05101 AFIX 23 H15A 2 0.728439 -0.332545 0.829875 11.00000 -1.20000 H15B 2 0.720064 -0.188152 0.820070 11.00000 -1.20000 AFIX 0 S11 4 1.095521 -0.049359 0.919744 11.00000 0.05813 0.07905 = 0.04949 -0.02391 0.00486 -0.02832 S12 4 0.844737 -0.121111 0.990675 11.00000 0.07243 0.08265 = 0.04670 -0.02247 0.00927 -0.03875 S13 4 0.749362 -0.268301 0.913823 11.00000 0.10016 0.09806 = 0.05905 -0.02849 0.01248 -0.06298 S14 4 1.049961 -0.184292 0.827397 11.00000 0.06217 0.10085 = 0.06036 -0.04107 0.01272 -0.02895 MOLE 3 C21 1 1.336561 -0.058253 0.628275 11.00000 0.04245 0.03523 = 0.06068 -0.00662 -0.01059 -0.00214 AFIX 43 H21 2 1.362419 -0.076324 0.666603 11.00000 -1.20000 AFIX 0 C22 1 1.411242 -0.140993 0.592510 11.00000 0.03840 0.03253 = 0.08206 -0.01566 -0.00445 -0.00137 C23 1 1.373427 -0.116816 0.535898 11.00000 0.04297 0.04257 = 0.06959 -0.02637 0.00773 -0.00854 C24 1 1.259832 -0.008498 0.515568 11.00000 0.03995 0.03886 = 0.05165 -0.01795 0.00549 -0.00709 C25 1 1.192812 0.068376 0.554826 11.00000 0.03422 0.03268 = 0.04192 -0.01045 0.00310 -0.00482 C26 1 1.080353 0.179899 0.536814 11.00000 0.03379 0.03369 = 0.03757 -0.00900 0.00464 -0.00604 C27 1 1.031338 0.214121 0.480175 11.00000 0.04048 0.04297 = 0.03621 -0.00884 0.00332 -0.00917 C28 1 0.917832 0.324787 0.465091 11.00000 0.04563 0.04926 = 0.03943 -0.00183 -0.00121 -0.01534 C29 1 0.861669 0.394700 0.507276 11.00000 0.03404 0.04157 = 0.04780 -0.00150 0.00213 -0.00638 C30 1 0.917882 0.353568 0.562502 11.00000 0.03931 0.03497 = 0.04494 -0.00962 0.00422 -0.00054 AFIX 43 H30 2 0.878415 0.401292 0.590347 11.00000 -1.20000 AFIX 0 C31 1 1.208982 0.028157 0.458496 11.00000 0.06329 0.05829 = 0.04493 -0.02577 0.00852 -0.00599 AFIX 43 H31 2 1.251313 -0.021882 0.431822 11.00000 -1.20000 AFIX 0 C32 1 1.101996 0.132381 0.441412 11.00000 0.06437 0.06207 = 0.03805 -0.01804 -0.00004 -0.00536 AFIX 43 H32 2 1.072875 0.152152 0.403414 11.00000 -1.20000 AFIX 0 C33 1 1.530087 -0.253829 0.619520 11.00000 0.05848 0.04287 = 0.10986 -0.02333 -0.01697 0.01008 AFIX 137 H33A 2 1.500638 -0.329422 0.614089 11.00000 -1.50000 H33B 2 1.536225 -0.252669 0.659488 11.00000 -1.50000 H33C 2 1.628444 -0.250646 0.602038 11.00000 -1.50000 AFIX 0 C34 1 1.451304 -0.201758 0.495231 11.00000 0.06543 0.05455 = 0.10147 -0.04252 0.00765 0.00505 AFIX 137 H34A 2 1.552550 -0.187045 0.486374 11.00000 -1.50000 H34B 2 1.392470 -0.184556 0.460922 11.00000 -1.50000 H34C 2 1.458377 -0.287648 0.512557 11.00000 -1.50000 AFIX 0 C35 1 0.861105 0.365818 0.405010 11.00000 0.06481 0.07030 = 0.04725 -0.00402 -0.00872 -0.00442 AFIX 137 H35A 2 0.768618 0.429288 0.404280 11.00000 -1.50000 H35B 2 0.840429 0.295266 0.390632 11.00000 -1.50000 H35C 2 0.938017 0.399119 0.381726 11.00000 -1.50000 AFIX 0 C36 1 0.740263 0.514083 0.497231 11.00000 0.05386 0.05083 = 0.05994 0.00091 -0.00284 0.00316 AFIX 137 H36A 2 0.780394 0.577526 0.472361 11.00000 -1.50000 H36B 2 0.710992 0.541840 0.532863 11.00000 -1.50000 H36C 2 0.652115 0.498884 0.480072 11.00000 -1.50000 AFIX 0 C41 1 0.850535 0.029506 0.681404 11.00000 0.06370 0.05509 = 0.03939 -0.01664 0.00916 -0.02245 C42 1 0.927161 0.417477 0.697807 11.00000 0.04873 0.05195 = 0.03650 -0.01179 0.00109 -0.01072 C43 1 1.285565 0.026444 0.767818 11.00000 0.05147 0.04991 = 0.03968 -0.00641 0.00317 -0.02150 C44 1 1.397165 0.306538 0.639691 11.00000 0.04725 0.04420 = 0.04106 -0.00794 -0.00091 -0.00488 N21 3 1.231600 0.043874 0.610660 11.00000 0.03637 0.03237 = 0.04276 -0.00722 -0.00162 -0.00385 N22 3 1.024228 0.250446 0.577522 11.00000 0.03513 0.03476 = 0.03431 -0.00694 0.00287 -0.00404 N41 3 0.949103 0.083051 0.671310 11.00000 0.05087 0.04805 = 0.04713 -0.01078 0.00593 -0.01401 N42 3 0.995277 0.320110 0.690458 11.00000 0.05397 0.04790 = 0.04267 -0.01669 0.00506 -0.00944 N43 3 1.216283 0.087492 0.729348 11.00000 0.06231 0.05278 = 0.04378 -0.00362 -0.00611 -0.01299 N44 3 1.288768 0.265682 0.639778 11.00000 0.04383 0.04237 = 0.05296 -0.00677 -0.00318 -0.00846 S41 4 0.711725 -0.043392 0.694985 11.00000 0.11864 0.15172 = 0.06685 -0.04487 0.03020 -0.10107 S42 4 0.831223 0.553511 0.707352 11.00000 0.08078 0.05929 = 0.09086 -0.03304 -0.00367 0.01237 S43 4 1.380061 -0.060058 0.821436 11.00000 0.06289 0.09112 = 0.05793 0.01820 -0.01554 -0.02166 S44 4 1.545445 0.368623 0.639200 11.00000 0.05613 0.09048 = 0.09089 -0.01630 0.00139 -0.03662 CR1 5 1.116309 0.176634 0.657410 11.00000 0.04002 0.03544 = 0.03385 -0.00776 0.00107 -0.00706 HKLF 4 Covalent radii and connectivity table for s92 in P-1 C 0.770 H 0.320 N 0.700 S 1.030 CR 1.240 C1 - C2 S1 C2 - C1 S2 C3 - C4 S3 S2 C4 - C3 S4 S1 C5 - C6 S4 S3 C6 - C5 S5 S6 C7 - C8 S5 S8 C8 - C7 S7 S6 C9 - C10 S7 C10 - C9 S8 S1 - C4 C1 S2 - C3 C2 S3 - C3 C5 S4 - C5 C4 S5 - C6 C7 S6 - C6 C8 S7 - C8 C9 S8 - C7 C10 C11 - C11_$1 S12 S11 C12 - C13 S13 S12 C13 - C12 S11 S14 C14 - C15 S14 C15 - C14 S13 S11 - C11 C13 S12 - C11 C12 S13 - C12 C15 S14 - C13 C14 C21 - N21 C22 C22 - C23 C21 C33 C23 - C22 C24 C34 C24 - C25 C31 C23 C25 - N21 C24 C26 C26 - N22 C27 C25 C27 - C26 C28 C32 C28 - C29 C27 C35 C29 - C28 C30 C36 C30 - N22 C29 C31 - C32 C24 C32 - C31 C27 C33 - C22 C34 - C23 C35 - C28 C36 - C29 C41 - N41 S41 C42 - N42 S42 C43 - N43 S43 C44 - N44 S44 N21 - C21 C25 Cr1 N22 - C30 C26 Cr1 N41 - C41 Cr1 N42 - C42 Cr1 N43 - C43 Cr1 N44 - C44 Cr1 S41 - C41 S42 - C42 S43 - C43 S44 - C44 Cr1 - N43 N41 N42 N44 N21 N22 Operators for generating equivalent atoms: $1 -x+2, -y, -z+2 39367 Reflections read, of which 1 rejected -11 =< h =< 9, -14 =< k =< 13, -30 =< l =< 30, Max. 2-theta = 54.90 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 2 0 0 451.22 4.55 8 24.12 3 0 0 407.08 4.11 9 22.08 4 0 0 285.54 2.83 9 17.63 5 0 0 39.00 0.85 6 4.34 -3 1 0 175.22 1.08 9 11.03 1 2 0 844.02 11.72 5 81.41 2 3 0 1409.65 17.31 6 121.52 -5 4 0 61.03 1.11 4 15.93 -4 4 0 112.26 1.86 5 16.03 3 4 0 1779.49 16.01 6 177.19 -7 5 0 59.48 2.69 3 15.98 -5 9 0 25.69 1.94 3 10.46 5 -4 1 77.86 1.72 5 10.24 4 -3 1 426.16 1.19 8 49.61 5 -3 1 62.63 1.07 5 10.60 4 -2 1 83.14 0.95 9 5.13 -1 -1 1 442.75 5.83 6 63.54 2 -1 1 5415.77 50.06 9 329.80 -4 0 1 175.93 1.67 9 9.39 6 0 1 27.39 0.87 5 4.42 -3 1 1 977.21 9.38 9 51.06 -5 2 1 272.96 4.90 5 31.21 -4 2 1 260.03 1.14 9 17.36 1 2 1 538.84 1.15 6 173.58 -4 3 1 211.72 1.12 8 16.76 2 -9 2 228.28 5.36 3 393.16 4 -7 2 56.00 2.56 3 14.56 4 -6 2 42.08 1.42 4 8.00 5 -5 2 126.12 1.14 5 24.56 3 -3 2 376.86 1.16 10 29.06 4 -3 2 167.39 1.14 7 18.52 5 -3 2 56.15 1.07 5 10.27 -6 -1 2 202.03 2.05 5 31.38 2 -1 2 4718.28 40.12 8 515.97 7 0 2 127.38 2.96 4 19.19 -3 1 2 434.73 4.31 10 23.38 1 1 2 538.28 5.38 9 50.66 6 1 2 55.57 0.95 6 6.09 7 1 2 51.41 1.03 4 10.99 -6 3 2 108.51 2.44 5 13.83 4 -5 3 116.55 1.14 4 33.25 5 -5 3 91.37 1.82 5 13.51 3 -4 3 74.41 0.93 8 5.31 5 -4 3 27.48 0.95 5 4.81 3 -3 3 2461.59 22.10 10 137.15 3 -2 3 231.23 1.13 9 16.36 -5 -1 3 63.96 0.88 8 5.87 1 -1 3 814.16 6.52 8 94.53 2 -1 3 77.51 0.80 7 5.52 4 -1 3 174.97 1.09 8 13.34 ** etc. ** 372 Inconsistent equivalents 10319 Unique reflections, of which 0 suppressed R(int) = 0.0990 R(sigma) = 0.0659 Friedel opposites merged Maximum memory for data reduction = 4236 / 103013 Default effective X-H distances for T = 27.0 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 = 5624 / 702793 wR2 = 0.1501 before cycle 1 for 10319 data and 527 / 527 parameters GooF = S = 1.030; Restrained GooF = 1.030 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0553 * P )^2 + 2.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34424 0.00052 -0.010 OSF Mean shift/esd = 0.002 Maximum = -0.036 for tors H34A Max. shift = 0.001 A for H34B Max. dU = 0.000 for C14 Least-squares cycle 2 Maximum vector length = 511 Memory required = 5624 / 702793 wR2 = 0.1501 before cycle 2 for 10319 data and 527 / 527 parameters GooF = S = 1.030; Restrained GooF = 1.030 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0553 * P )^2 + 2.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34425 0.00052 0.002 OSF Mean shift/esd = 0.001 Maximum = -0.044 for tors H34A Max. shift = 0.001 A for H34A Max. dU = 0.000 for C14 Least-squares cycle 3 Maximum vector length = 511 Memory required = 5624 / 702793 wR2 = 0.1501 before cycle 3 for 10319 data and 527 / 527 parameters GooF = S = 1.030; Restrained GooF = 1.030 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0553 * P )^2 + 2.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34425 0.00052 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.039 for tors H34A Max. shift = 0.001 A for H34A Max. dU = 0.000 for C10 Least-squares cycle 4 Maximum vector length = 511 Memory required = 5624 / 702793 wR2 = 0.1501 before cycle 4 for 10319 data and 527 / 527 parameters GooF = S = 1.030; Restrained GooF = 1.030 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0553 * P )^2 + 2.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34425 0.00052 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.034 for tors H34A Max. shift = 0.001 A for H34A Max. dU = 0.000 for C10 Least-squares cycle 5 Maximum vector length = 511 Memory required = 5624 / 702793 wR2 = 0.1501 before cycle 5 for 10319 data and 527 / 527 parameters GooF = S = 1.030; Restrained GooF = 1.030 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0553 * P )^2 + 2.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34425 0.00052 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.030 for tors H34A Max. shift = 0.001 A for H34A Max. dU = 0.000 for C9 Least-squares cycle 6 Maximum vector length = 511 Memory required = 5624 / 702793 wR2 = 0.1501 before cycle 6 for 10319 data and 527 / 527 parameters GooF = S = 1.030; Restrained GooF = 1.030 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0553 * P )^2 + 2.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34425 0.00052 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.027 for tors H34A Max. shift = 0.001 A for H34A Max. dU = 0.000 for C9 Least-squares cycle 7 Maximum vector length = 511 Memory required = 5624 / 702793 wR2 = 0.1501 before cycle 7 for 10319 data and 527 / 527 parameters GooF = S = 1.030; Restrained GooF = 1.030 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0553 * P )^2 + 2.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34424 0.00052 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.023 for tors H34A Max. shift = 0.001 A for H34A Max. dU = 0.000 for C9 Least-squares cycle 8 Maximum vector length = 511 Memory required = 5624 / 702793 wR2 = 0.1501 before cycle 8 for 10319 data and 527 / 527 parameters GooF = S = 1.030; Restrained GooF = 1.030 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0553 * P )^2 + 2.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34424 0.00052 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.021 for tors H34A Max. shift = 0.001 A for H34A Max. dU = 0.000 for C9 Least-squares cycle 9 Maximum vector length = 511 Memory required = 5624 / 702793 wR2 = 0.1501 before cycle 9 for 10319 data and 527 / 527 parameters GooF = S = 1.030; Restrained GooF = 1.030 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0553 * P )^2 + 2.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34424 0.00052 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.018 for tors H34A Max. shift = 0.001 A for H34A Max. dU = 0.000 for C9 Least-squares cycle 10 Maximum vector length = 511 Memory required = 5624 / 702793 wR2 = 0.1501 before cycle 10 for 10319 data and 527 / 527 parameters GooF = S = 1.030; Restrained GooF = 1.030 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0553 * P )^2 + 2.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34424 0.00052 0.001 OSF Mean shift/esd = 0.000 Maximum = -0.016 for tors H34A Max. shift = 0.001 A for H34A Max. dU = 0.000 for C10 Least-squares cycle 11 Maximum vector length = 511 Memory required = 5624 / 702793 wR2 = 0.1501 before cycle 11 for 10319 data and 527 / 527 parameters GooF = S = 1.030; Restrained GooF = 1.030 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0553 * P )^2 + 2.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.34424 0.00052 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.014 for tors H34A Max. shift = 0.000 A for H34A Max. dU = 0.000 for C9 Largest correlation matrix elements -0.731 U12 S41 / U22 S41 -0.630 U12 S13 / U11 S13 -0.598 y C9 / x C9 -0.731 U12 S41 / U11 S41 -0.625 U12 S7 / U11 S7 -0.588 U23 C2 / U33 C2 -0.688 U12 C9 / U11 C9 -0.623 U12 S7 / U22 S7 -0.588 U23 S2 / U22 S2 -0.680 U12 C9 / U22 C9 -0.620 U12 S13 / U22 S13 -0.579 U12 S6 / U11 S6 -0.669 U23 C14 / U22 C14 -0.617 U12 C10 / U11 C10 -0.569 U12 C14 / U13 C14 -0.656 U23 C14 / U33 C14 -0.616 U23 C2 / U22 C2 -0.565 U23 S1 / U22 S1 -0.655 U13 S41 / U23 S41 -0.611 U12 C10 / U22 C10 -0.559 z C14 / y C14 -0.647 y S41 / x S41 -0.607 U13 C9 / U23 C9 -0.557 U12 S6 / U22 S6 Idealized hydrogen atom generation before cycle 12 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 1.2014 -0.4559 0.7627 23 0.970 0.000 C1 C2 S1 H1B 1.3254 -0.5257 0.7242 23 0.970 0.000 C1 C2 S1 H2A 1.3577 -0.7016 0.7919 23 0.970 0.000 C2 C1 S2 H2B 1.1919 -0.6621 0.7668 23 0.970 0.000 C2 C1 S2 H9A 1.1956 -0.1669 1.2377 23 0.970 0.000 C9 C10 S7 H9B 1.3271 -0.2753 1.2239 23 0.970 0.000 C9 C10 S7 H10A 1.4137 -0.1246 1.2070 23 0.970 0.000 C10 C9 S8 H10B 1.2628 -0.0387 1.1817 23 0.970 0.000 C10 C9 S8 H14A 0.9228 -0.2893 0.7789 23 0.970 0.000 C14 C15 S14 H14B 0.9791 -0.3710 0.8369 23 0.970 0.000 C14 C15 S14 H15A 0.7284 -0.3326 0.8299 23 0.970 0.000 C15 C14 S13 H15B 0.7201 -0.1882 0.8201 23 0.970 0.000 C15 C14 S13 H21 1.3624 -0.0763 0.6666 43 0.930 0.000 C21 N21 C22 H30 0.8784 0.4013 0.5903 43 0.930 0.000 C30 N22 C29 H31 1.2513 -0.0219 0.4318 43 0.930 0.000 C31 C32 C24 H32 1.0729 0.1522 0.4034 43 0.930 0.000 C32 C31 C27 H33A 1.5006 -0.3294 0.6141 137 0.960 0.000 C33 C22 H33A H33B 1.5362 -0.2527 0.6595 137 0.960 0.000 C33 C22 H33A H33C 1.6284 -0.2506 0.6020 137 0.960 0.000 C33 C22 H33A H34A 1.5521 -0.1864 0.4860 137 0.960 0.000 C34 C23 H34A H34B 1.3918 -0.1852 0.4611 137 0.960 0.000 C34 C23 H34A H34C 1.4594 -0.2877 0.5127 137 0.960 0.000 C34 C23 H34A H35A 0.7686 0.4293 0.4043 137 0.960 0.000 C35 C28 H35A H35B 0.8404 0.2953 0.3906 137 0.960 0.000 C35 C28 H35A H35C 0.9380 0.3991 0.3817 137 0.960 0.000 C35 C28 H35A H36A 0.7804 0.5775 0.4724 137 0.960 0.000 C36 C29 H36A H36B 0.7109 0.5418 0.5329 137 0.960 0.000 C36 C29 H36A H36C 0.6522 0.4989 0.4800 137 0.960 0.000 C36 C29 H36A s92 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 1.29506 -0.51980 0.76333 1.00000 0.12768 0.12723 0.05384 -0.03297 -0.00411 0.01842 0.10759 0.01006 0.00078 0.00066 0.00022 0.00000 0.00516 0.00530 0.00295 0.00339 0.00305 0.00433 0.00214 H1A 1.20141 -0.45591 0.76269 1.00000 0.12911 0.00000 0.00000 H1B 1.32537 -0.52569 0.72420 1.00000 0.12911 0.00000 0.00000 C2 1.26289 -0.63878 0.79061 1.00000 0.08380 0.15050 0.08170 -0.07072 0.00540 -0.02221 0.09971 0.00804 0.00066 0.00070 0.00025 0.00000 0.00369 0.00582 0.00369 0.00408 0.00286 0.00375 0.00195 H2A 1.35767 -0.70162 0.79192 1.00000 0.11966 0.00000 0.00000 H2B 1.19191 -0.66208 0.76680 1.00000 0.11966 0.00000 0.00000 C3 1.26130 -0.53713 0.88808 1.00000 0.06928 0.06910 0.04732 -0.02504 -0.00130 -0.01449 0.06004 0.00587 0.00050 0.00041 0.00017 0.00000 0.00266 0.00270 0.00214 0.00201 0.00188 0.00220 0.00103 C4 1.36188 -0.47017 0.86529 1.00000 0.07456 0.07709 0.05298 -0.02734 0.00819 -0.01383 0.06681 0.00667 0.00053 0.00044 0.00018 0.00000 0.00291 0.00299 0.00237 0.00224 0.00207 0.00242 0.00115 C5 1.30238 -0.40700 0.96394 1.00000 0.06465 0.06059 0.04452 -0.01597 -0.00052 -0.01231 0.05586 0.00574 0.00047 0.00038 0.00016 0.00000 0.00249 0.00244 0.00203 0.00186 0.00175 0.00198 0.00096 C6 1.29716 -0.35415 1.01134 1.00000 0.07081 0.06055 0.04254 -0.01625 0.00077 -0.01680 0.05663 0.00577 0.00049 0.00038 0.00016 0.00000 0.00260 0.00245 0.00200 0.00184 0.00178 0.00205 0.00097 C7 1.33129 -0.21481 1.08382 1.00000 0.05944 0.05884 0.04756 -0.01971 0.00172 -0.01143 0.05420 0.00565 0.00046 0.00037 0.00016 0.00000 0.00236 0.00238 0.00206 0.00185 0.00173 0.00193 0.00093 C8 1.22027 -0.27350 1.10596 1.00000 0.08215 0.05874 0.04488 -0.01854 0.00654 -0.02328 0.05965 0.00592 0.00052 0.00038 0.00016 0.00000 0.00292 0.00247 0.00207 0.00188 0.00193 0.00219 0.00103 C9 1.25240 -0.20254 1.20669 1.00000 0.15118 0.21643 0.06477 -0.06619 0.03599 -0.12638 0.12668 0.00753 0.00081 0.00075 0.00023 0.00000 0.00571 0.00770 0.00326 0.00432 0.00347 0.00586 0.00280 H9A 1.19558 -0.16685 1.23766 1.00000 0.15201 0.00000 0.00000 H9B 1.32713 -0.27531 1.22393 1.00000 0.15201 0.00000 0.00000 C10 1.33044 -0.11996 1.18134 1.00000 0.15516 0.15886 0.07208 -0.05352 0.02797 -0.09693 0.11567 0.00827 0.00084 0.00067 0.00023 0.00000 0.00587 0.00601 0.00347 0.00391 0.00361 0.00516 0.00236 H10A 1.41372 -0.12455 1.20701 1.00000 0.13881 0.00000 0.00000 H10B 1.26281 -0.03874 1.18166 1.00000 0.13881 0.00000 0.00000 S1 1.44504 -0.47012 0.79767 1.00000 0.14484 0.13056 0.07458 -0.05287 0.05189 -0.06424 0.10853 0.00247 0.00022 0.00017 0.00006 0.00000 0.00142 0.00132 0.00088 0.00092 0.00091 0.00114 0.00057 S2 1.18573 -0.64509 0.85973 1.00000 0.12871 0.10429 0.08677 -0.05710 0.00557 -0.04330 0.09896 0.00198 0.00020 0.00015 0.00006 0.00000 0.00125 0.00108 0.00095 0.00087 0.00085 0.00095 0.00049 S3 1.19302 -0.51523 0.95534 1.00000 0.09729 0.08343 0.04919 -0.02543 0.01082 -0.04032 0.07199 0.00166 0.00015 0.00012 0.00005 0.00000 0.00088 0.00081 0.00058 0.00057 0.00055 0.00070 0.00034 S4 1.41567 -0.36964 0.90574 1.00000 0.08312 0.09441 0.05705 -0.02901 0.01303 -0.03887 0.07354 0.00170 0.00015 0.00013 0.00005 0.00000 0.00080 0.00090 0.00064 0.00063 0.00056 0.00070 0.00034 S5 1.41094 -0.24943 1.01920 1.00000 0.06940 0.08837 0.05463 -0.03222 0.01128 -0.02883 0.06684 0.00159 0.00013 0.00012 0.00005 0.00000 0.00069 0.00082 0.00059 0.00058 0.00050 0.00061 0.00031 S6 1.17508 -0.38280 1.06830 1.00000 0.12063 0.08457 0.05286 -0.03155 0.02113 -0.05687 0.07886 0.00171 0.00017 0.00012 0.00005 0.00000 0.00106 0.00084 0.00062 0.00060 0.00063 0.00079 0.00039 S7 1.12094 -0.25879 1.16949 1.00000 0.11726 0.13308 0.05767 -0.04540 0.03076 -0.07508 0.09261 0.00186 0.00018 0.00015 0.00005 0.00000 0.00109 0.00123 0.00069 0.00078 0.00068 0.00099 0.00048 S8 1.41394 -0.11127 1.11297 1.00000 0.08848 0.08526 0.05770 -0.02971 0.01019 -0.04257 0.07162 0.00160 0.00015 0.00012 0.00005 0.00000 0.00082 0.00082 0.00063 0.00060 0.00056 0.00068 0.00033 C11 0.98706 -0.03621 0.98071 1.00000 0.05203 0.06460 0.04348 -0.01434 -0.00131 -0.01536 0.05223 0.00535 0.00043 0.00037 0.00015 0.00000 0.00218 0.00250 0.00198 0.00185 0.00162 0.00189 0.00092 C12 0.87805 -0.17869 0.92675 1.00000 0.05772 0.05701 0.04509 -0.01508 -0.00303 -0.01627 0.05176 0.00532 0.00045 0.00037 0.00016 0.00000 0.00227 0.00229 0.00199 0.00177 0.00167 0.00184 0.00089 C13 0.99446 -0.14623 0.89433 1.00000 0.05109 0.05860 0.04521 -0.01795 -0.00317 -0.01222 0.05033 0.00520 0.00043 0.00036 0.00015 0.00000 0.00212 0.00231 0.00198 0.00177 0.00161 0.00178 0.00087 C14 0.92771 -0.28767 0.81926 1.00000 0.09245 0.17617 0.10869 -0.09722 0.01482 -0.05491 0.11332 0.00722 0.00067 0.00068 0.00027 0.00000 0.00402 0.00634 0.00450 0.00467 0.00333 0.00412 0.00231 H14A 0.92280 -0.28930 0.77887 1.00000 0.13599 0.00000 0.00000 H14B 0.97909 -0.37104 0.83692 1.00000 0.13599 0.00000 0.00000 C15 0.77564 -0.26809 0.83992 1.00000 0.07952 0.12999 0.07040 -0.04333 0.00872 -0.05105 0.08595 0.00672 0.00058 0.00058 0.00021 0.00000 0.00337 0.00462 0.00301 0.00314 0.00250 0.00325 0.00159 H15A 0.72845 -0.33255 0.82988 1.00000 0.10314 0.00000 0.00000 H15B 0.72007 -0.18816 0.82007 1.00000 0.10314 0.00000 0.00000 S11 1.09552 -0.04936 0.91974 1.00000 0.05813 0.07905 0.04949 -0.02391 0.00486 -0.02832 0.05867 0.00140 0.00012 0.00011 0.00004 0.00000 0.00060 0.00072 0.00054 0.00051 0.00043 0.00053 0.00027 S12 0.84474 -0.12111 0.99067 1.00000 0.07243 0.08265 0.04670 -0.02247 0.00927 -0.03874 0.06272 0.00146 0.00013 0.00011 0.00004 0.00000 0.00069 0.00076 0.00053 0.00052 0.00047 0.00059 0.00029 S13 0.74936 -0.26830 0.91382 1.00000 0.10015 0.09806 0.05906 -0.02849 0.01248 -0.06297 0.07786 0.00160 0.00016 0.00013 0.00005 0.00000 0.00092 0.00092 0.00065 0.00064 0.00060 0.00078 0.00038 S14 1.04996 -0.18429 0.82740 1.00000 0.06218 0.10085 0.06036 -0.04107 0.01272 -0.02895 0.06973 0.00157 0.00013 0.00013 0.00005 0.00000 0.00066 0.00091 0.00064 0.00064 0.00050 0.00062 0.00033 C21 1.33656 -0.05825 0.62828 1.00000 0.04245 0.03522 0.06068 -0.00661 -0.01058 -0.00214 0.04690 0.00523 0.00039 0.00031 0.00017 0.00000 0.00190 0.00182 0.00221 0.00165 0.00162 0.00150 0.00083 H21 1.36242 -0.07632 0.66660 1.00000 0.05628 0.00000 0.00000 C22 1.41125 -0.14100 0.59251 1.00000 0.03840 0.03253 0.08207 -0.01566 -0.00445 -0.00137 0.05108 0.00554 0.00040 0.00032 0.00019 0.00000 0.00186 0.00181 0.00280 0.00184 0.00177 0.00146 0.00092 C23 1.37342 -0.11681 0.53590 1.00000 0.04297 0.04258 0.06958 -0.02638 0.00773 -0.00855 0.04997 0.00537 0.00040 0.00034 0.00017 0.00000 0.00194 0.00200 0.00251 0.00187 0.00172 0.00158 0.00089 C24 1.25983 -0.00850 0.51557 1.00000 0.03995 0.03885 0.05164 -0.01795 0.00548 -0.00709 0.04259 0.00491 0.00038 0.00031 0.00015 0.00000 0.00179 0.00183 0.00200 0.00159 0.00147 0.00147 0.00077 C25 1.19281 0.06837 0.55483 1.00000 0.03422 0.03268 0.04191 -0.01044 0.00310 -0.00483 0.03620 0.00465 0.00035 0.00029 0.00014 0.00000 0.00162 0.00163 0.00174 0.00138 0.00130 0.00131 0.00068 C26 1.08035 0.17990 0.53681 1.00000 0.03378 0.03368 0.03758 -0.00899 0.00464 -0.00603 0.03495 0.00456 0.00034 0.00029 0.00013 0.00000 0.00160 0.00164 0.00163 0.00135 0.00125 0.00130 0.00067 C27 1.03134 0.21412 0.48018 1.00000 0.04048 0.04296 0.03621 -0.00884 0.00333 -0.00916 0.03966 0.00482 0.00037 0.00031 0.00013 0.00000 0.00177 0.00187 0.00166 0.00145 0.00133 0.00148 0.00072 C28 0.91783 0.32478 0.46509 1.00000 0.04563 0.04925 0.03944 -0.00183 -0.00122 -0.01534 0.04460 0.00509 0.00040 0.00034 0.00014 0.00000 0.00193 0.00205 0.00178 0.00157 0.00144 0.00163 0.00079 C29 0.86167 0.39470 0.50728 1.00000 0.03404 0.04158 0.04778 -0.00150 0.00213 -0.00638 0.04216 0.00522 0.00037 0.00032 0.00015 0.00000 0.00169 0.00186 0.00191 0.00155 0.00139 0.00143 0.00075 C30 0.91788 0.35357 0.56250 1.00000 0.03930 0.03496 0.04494 -0.00961 0.00421 -0.00054 0.04062 0.00501 0.00037 0.00030 0.00014 0.00000 0.00177 0.00175 0.00184 0.00148 0.00140 0.00142 0.00074 H30 0.87842 0.40129 0.59035 1.00000 0.04875 0.00000 0.00000 C31 1.20898 0.02816 0.45850 1.00000 0.06329 0.05828 0.04494 -0.02577 0.00852 -0.00601 0.05474 0.00576 0.00046 0.00037 0.00016 0.00000 0.00242 0.00241 0.00205 0.00186 0.00174 0.00197 0.00096 H31 1.25131 -0.02188 0.43182 1.00000 0.06569 0.00000 0.00000 C32 1.10199 0.13238 0.44141 1.00000 0.06437 0.06206 0.03804 -0.01804 -0.00004 -0.00535 0.05489 0.00573 0.00046 0.00037 0.00015 0.00000 0.00247 0.00248 0.00188 0.00179 0.00167 0.00202 0.00095 H32 1.07287 0.15215 0.40341 1.00000 0.06587 0.00000 0.00000 C33 1.53009 -0.25383 0.61952 1.00000 0.05848 0.04288 0.10987 -0.02334 -0.01696 0.01007 0.07182 0.00671 0.00049 0.00036 0.00022 0.00000 0.00257 0.00225 0.00379 0.00242 0.00245 0.00193 0.00129 H33A 1.50064 -0.32942 0.61409 1.00000 0.10773 0.00000 0.00000 H33B 1.53622 -0.25267 0.65949 1.00000 0.10773 0.00000 0.00000 H33C 1.62845 -0.25064 0.60204 1.00000 0.10773 0.00000 0.00000 C34 1.45129 -0.20176 0.49523 1.00000 0.06542 0.05454 0.10150 -0.04252 0.00765 0.00506 0.07322 0.00694 0.00052 0.00040 0.00022 0.00000 0.00273 0.00253 0.00361 0.00257 0.00246 0.00210 0.00131 H34A 1.55211 -0.18637 0.48603 1.00000 0.10983 0.00000 0.00000 H34B 1.39185 -0.18521 0.46109 1.00000 0.10983 0.00000 0.00000 H34C 1.45941 -0.28766 0.51272 1.00000 0.10983 0.00000 0.00000 C35 0.86110 0.36582 0.40501 1.00000 0.06480 0.07029 0.04725 -0.00403 -0.00872 -0.00441 0.06274 0.00642 0.00050 0.00042 0.00016 0.00000 0.00259 0.00277 0.00217 0.00201 0.00185 0.00216 0.00106 H35A 0.76861 0.42929 0.40428 1.00000 0.09411 0.00000 0.00000 H35B 0.84042 0.29527 0.39063 1.00000 0.09411 0.00000 0.00000 H35C 0.93801 0.39912 0.38173 1.00000 0.09411 0.00000 0.00000 C36 0.74026 0.51408 0.49723 1.00000 0.05386 0.05082 0.05993 0.00091 -0.00283 0.00315 0.05819 0.00647 0.00045 0.00036 0.00018 0.00000 0.00229 0.00226 0.00236 0.00190 0.00183 0.00184 0.00099 H36A 0.78043 0.57755 0.47239 1.00000 0.08728 0.00000 0.00000 H36B 0.71092 0.54180 0.53287 1.00000 0.08728 0.00000 0.00000 H36C 0.65215 0.49891 0.48004 1.00000 0.08728 0.00000 0.00000 C41 0.85053 0.02951 0.68140 1.00000 0.06369 0.05509 0.03939 -0.01664 0.00916 -0.02244 0.05043 0.00544 0.00046 0.00036 0.00015 0.00000 0.00238 0.00223 0.00187 0.00169 0.00166 0.00195 0.00088 C42 0.92716 0.41748 0.69781 1.00000 0.04874 0.05196 0.03650 -0.01179 0.00109 -0.01073 0.04522 0.00514 0.00041 0.00035 0.00014 0.00000 0.00201 0.00221 0.00175 0.00161 0.00145 0.00172 0.00080 C43 1.28557 0.02644 0.76782 1.00000 0.05146 0.04991 0.03969 -0.00642 0.00318 -0.02150 0.04559 0.00511 0.00041 0.00034 0.00015 0.00000 0.00208 0.00211 0.00186 0.00167 0.00158 0.00173 0.00081 C44 1.39716 0.30654 0.63969 1.00000 0.04724 0.04419 0.04105 -0.00793 -0.00092 -0.00487 0.04477 0.00536 0.00041 0.00033 0.00014 0.00000 0.00205 0.00197 0.00184 0.00156 0.00149 0.00164 0.00079 N21 1.23160 0.04387 0.61066 1.00000 0.03637 0.03237 0.04277 -0.00722 -0.00162 -0.00385 0.03753 0.00386 0.00029 0.00024 0.00011 0.00000 0.00141 0.00141 0.00149 0.00118 0.00113 0.00114 0.00059 N22 1.02423 0.25045 0.57752 1.00000 0.03513 0.03476 0.03431 -0.00693 0.00288 -0.00405 0.03519 0.00378 0.00029 0.00024 0.00011 0.00000 0.00136 0.00141 0.00133 0.00113 0.00105 0.00113 0.00056 N41 0.94910 0.08305 0.67131 1.00000 0.05087 0.04804 0.04713 -0.01078 0.00593 -0.01401 0.04798 0.00447 0.00035 0.00028 0.00012 0.00000 0.00177 0.00174 0.00168 0.00140 0.00134 0.00146 0.00070 N42 0.99528 0.32011 0.69046 1.00000 0.05397 0.04789 0.04268 -0.01669 0.00507 -0.00944 0.04744 0.00435 0.00035 0.00029 0.00012 0.00000 0.00180 0.00176 0.00160 0.00140 0.00132 0.00146 0.00069 N43 1.21628 0.08749 0.72935 1.00000 0.06231 0.05278 0.04378 -0.00361 -0.00611 -0.01300 0.05319 0.00466 0.00038 0.00030 0.00013 0.00000 0.00202 0.00189 0.00172 0.00150 0.00148 0.00158 0.00076 N44 1.28877 0.26568 0.63978 1.00000 0.04383 0.04236 0.05296 -0.00676 -0.00318 -0.00845 0.04654 0.00438 0.00034 0.00027 0.00013 0.00000 0.00166 0.00166 0.00176 0.00138 0.00132 0.00137 0.00068 S41 0.71172 -0.04339 0.69498 1.00000 0.11863 0.15171 0.06685 -0.04487 0.03019 -0.10106 0.09901 0.00175 0.00018 0.00016 0.00006 0.00000 0.00112 0.00136 0.00075 0.00085 0.00072 0.00109 0.00054 S42 0.83122 0.55351 0.70735 1.00000 0.08078 0.05929 0.09086 -0.03304 -0.00367 0.01237 0.07857 0.00198 0.00015 0.00011 0.00006 0.00000 0.00082 0.00069 0.00088 0.00066 0.00066 0.00060 0.00037 S43 1.38006 -0.06006 0.82144 1.00000 0.06289 0.09112 0.05793 0.01821 -0.01554 -0.02166 0.07306 0.00187 0.00013 0.00013 0.00005 0.00000 0.00068 0.00086 0.00063 0.00060 0.00051 0.00062 0.00034 S44 1.54544 0.36862 0.63920 1.00000 0.05613 0.09048 0.09090 -0.01630 0.00139 -0.03662 0.07585 0.00175 0.00013 0.00013 0.00006 0.00000 0.00065 0.00088 0.00087 0.00071 0.00058 0.00063 0.00035 Cr1 1.11631 0.17663 0.65741 1.00000 0.04002 0.03544 0.03385 -0.00776 0.00107 -0.00706 0.03637 0.00074 0.00006 0.00005 0.00002 0.00000 0.00029 0.00028 0.00027 0.00022 0.00021 0.00022 0.00014 Final Structure Factor Calculation for s92 in P-1 Total number of l.s. parameters = 527 Maximum vector length = 511 Memory required = 5097 / 24017 wR2 = 0.1501 before cycle 12 for 10319 data and 0 / 527 parameters GooF = S = 1.030; Restrained GooF = 1.030 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0553 * P )^2 + 2.26 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0564 for 6861 Fo > 4sig(Fo) and 0.0934 for all 10319 data wR2 = 0.1501, GooF = S = 1.030, Restrained GooF = 1.030 for all data Occupancy sum of asymmetric unit = 58.00 for non-hydrogen and 28.00 for hydrogen atoms Principal mean square atomic displacements U 0.1852 0.0920 0.0456 C1 0.1717 0.0836 0.0439 C2 0.0753 0.0693 0.0356 C3 0.0832 0.0768 0.0405 C4 0.0653 0.0621 0.0401 C5 0.0712 0.0608 0.0379 C6 0.0640 0.0598 0.0388 C7 0.0848 0.0565 0.0376 C8 0.2681 0.0678 0.0441 C9 may be split into 1.2321 -0.1865 1.2051 and 1.2727 -0.2185 1.2083 0.2159 0.0796 0.0515 C10 may be split into 1.3488 -0.1314 1.1829 and 1.3121 -0.1085 1.1798 0.1899 0.0931 0.0426 S1 0.1435 0.1130 0.0403 S2 0.1114 0.0638 0.0408 S3 0.1105 0.0626 0.0475 S4 0.0993 0.0603 0.0410 S5 0.1412 0.0571 0.0383 S6 0.1738 0.0629 0.0411 S7 0.1107 0.0613 0.0428 S8 0.0653 0.0514 0.0400 C11 0.0609 0.0561 0.0383 C12 0.0624 0.0519 0.0367 C13 0.2148 0.0841 0.0411 C14 may be split into 0.9183 -0.2723 0.8157 and 0.9372 -0.3030 0.8228 0.1437 0.0659 0.0483 C15 0.0863 0.0496 0.0401 S11 0.0984 0.0492 0.0405 S12 0.1358 0.0563 0.0415 S13 0.1128 0.0557 0.0407 S14 0.0653 0.0431 0.0323 C21 0.0827 0.0418 0.0287 C22 0.0760 0.0434 0.0305 C23 0.0566 0.0410 0.0302 C24 0.0434 0.0364 0.0287 C25 0.0409 0.0350 0.0289 C26 0.0436 0.0415 0.0338 C27 0.0547 0.0420 0.0371 C28 0.0540 0.0389 0.0337 C29 0.0491 0.0441 0.0286 C30 0.0702 0.0660 0.0281 C31 0.0739 0.0581 0.0326 C32 0.1177 0.0662 0.0316 C33 0.1119 0.0792 0.0286 C34 0.0807 0.0645 0.0430 C35 0.0759 0.0602 0.0385 C36 0.0714 0.0463 0.0336 C41 0.0525 0.0487 0.0344 C42 0.0596 0.0415 0.0357 C43 0.0520 0.0417 0.0406 C44 0.0432 0.0385 0.0309 N21 0.0402 0.0355 0.0298 N22 0.0563 0.0451 0.0426 N41 0.0562 0.0527 0.0335 N42 0.0642 0.0538 0.0417 N43 0.0539 0.0436 0.0421 N44 0.2017 0.0540 0.0413 S41 may be split into 0.6935 -0.0304 0.6935 and 0.7299 -0.0563 0.6965 0.1135 0.0845 0.0377 S42 0.1162 0.0619 0.0411 S43 0.0970 0.0904 0.0401 S44 0.0406 0.0365 0.0320 Cr1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.015 0.022 0.030 0.038 0.050 0.066 0.091 0.141 1.000 Number in group 1192. 1014. 1029. 1011. 915. 1055. 1017. 1020. 1037. 1029. GooF 0.901 0.956 1.045 0.999 1.052 1.133 1.040 1.050 1.131 0.985 K 2.389 1.088 1.052 0.997 0.977 0.983 1.000 1.007 1.003 1.007 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.66 inf Number in group 1034. 1065. 1010. 1022. 1050. 1006. 1036. 1035. 1022. 1039. GooF 0.937 0.878 0.879 0.963 0.967 0.952 0.993 1.002 1.117 1.473 K 0.994 1.020 1.055 1.023 1.018 1.020 1.003 0.982 0.986 1.015 R1 0.329 0.241 0.174 0.148 0.118 0.095 0.078 0.056 0.045 0.041 Recommended weighting scheme: WGHT 0.0550 2.2955 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) 4 -2 2 119.70 9.91 7.54 0.014 1.84 6 6 0 129.67 14.66 6.28 0.017 1.26 4 6 2 249.51 94.65 6.27 0.042 1.56 4 -1 1 542.08 295.00 5.90 0.074 2.04 0 -1 8 44.28 132.79 5.28 0.050 2.72 -2 3 12 66.96 14.64 4.93 0.017 1.64 0 -2 2 308.19 176.29 4.86 0.057 4.58 -1 -1 4 180.31 91.68 4.79 0.041 4.39 5 5 1 330.41 90.69 4.65 0.041 1.52 0 4 5 18.18 73.71 4.55 0.037 2.50 -2 7 3 92.46 27.07 4.55 0.022 1.37 4 7 3 323.36 1.45 4.51 0.005 1.41 0 5 2 201.64 102.95 4.48 0.044 2.16 -2 3 9 683.95 463.97 4.45 0.093 1.92 2 -4 1 63.57 18.87 4.44 0.019 2.05 2 4 1 493.24 737.95 4.44 0.117 2.55 4 6 4 1248.27 812.26 4.43 0.123 1.55 1 5 5 2790.96 2063.57 4.31 0.196 2.12 2 1 13 177.35 96.01 4.31 0.042 1.72 3 4 1 321.46 193.34 4.28 0.060 2.23 -2 4 4 59.76 14.80 4.15 0.017 2.05 3 4 6 1020.04 749.21 4.11 0.118 2.05 -6 -9 10 15.65 112.48 4.06 0.046 0.90 6 2 1 93.13 20.81 3.86 0.020 1.48 -2 1 1 1890.19 1458.47 3.83 0.165 3.75 -3 6 2 1705.79 1305.51 3.74 0.156 1.40 -2 2 0 18.35 0.24 3.69 0.002 3.07 4 -4 2 36.01 92.07 3.68 0.041 1.50 0 -5 3 58.96 21.59 3.64 0.020 1.98 -2 7 1 192.46 115.22 3.63 0.046 1.36 4 4 1 201.95 114.36 3.63 0.046 1.91 5 -7 7 121.77 265.01 3.61 0.070 0.97 0 -1 12 701.47 1005.26 3.60 0.137 1.87 2 -4 2 205.47 128.73 3.59 0.049 2.01 -3 3 3 29.52 2.43 3.54 0.007 2.03 3 0 7 573.68 792.63 3.53 0.122 2.20 1 -5 2 28.07 5.76 3.53 0.010 1.90 -1 -10 8 435.07 284.04 3.50 0.073 0.97 -3 4 28 163.86 62.31 3.48 0.034 0.79 4 9 26 -57.55 115.88 3.46 0.046 0.77 -2 2 7 67.66 126.10 3.43 0.048 2.38 2 5 2 28.75 5.14 3.42 0.010 2.13 0 -3 6 187.02 298.50 3.40 0.075 2.44 2 -9 6 0.00 49.33 3.38 0.030 1.01 -3 -4 5 315.48 444.03 3.36 0.091 1.90 -2 1 10 1141.21 891.26 3.36 0.129 2.04 1 -4 3 48.80 98.46 3.36 0.043 2.21 -3 7 4 262.95 172.49 3.35 0.057 1.25 -1 -8 18 23.88 106.84 3.35 0.045 0.87 -3 2 2 751.82 570.86 3.32 0.103 2.33 Bond lengths and angles C1 - Distance Angles C2 1.4478 (0.0082) S1 1.8240 (0.0070) 114.28 (0.42) H1A 0.9700 108.69 108.69 H1B 0.9700 108.69 108.69 107.61 C1 - C2 S1 H1A C2 - Distance Angles C1 1.4478 (0.0083) S2 1.7560 (0.0057) 116.74 (0.40) H2A 0.9700 108.11 108.11 H2B 0.9700 108.11 108.11 107.30 C2 - C1 S2 H2A C3 - Distance Angles C4 1.3256 (0.0061) S3 1.7299 (0.0040) 116.77 (0.30) S2 1.7333 (0.0041) 129.04 (0.32) 114.19 (0.26) C3 - C4 S3 C4 - Distance Angles C3 1.3256 (0.0061) S4 1.7431 (0.0043) 117.53 (0.31) S1 1.7470 (0.0043) 126.51 (0.33) 115.96 (0.27) C4 - C3 S4 C5 - Distance Angles C6 1.3544 (0.0051) S4 1.7277 (0.0041) 122.58 (0.33) S3 1.7421 (0.0041) 123.39 (0.33) 114.02 (0.21) C5 - C6 S4 C6 - Distance Angles C5 1.3544 (0.0051) S5 1.7343 (0.0041) 122.21 (0.33) S6 1.7345 (0.0041) 123.24 (0.33) 114.55 (0.21) C6 - C5 S5 C7 - Distance Angles C8 1.3405 (0.0056) S5 1.7381 (0.0038) 117.30 (0.29) S8 1.7386 (0.0038) 128.22 (0.30) 114.42 (0.23) C7 - C8 S5 C8 - Distance Angles C7 1.3405 (0.0056) S7 1.7371 (0.0040) 127.69 (0.30) S6 1.7461 (0.0038) 116.52 (0.30) 115.73 (0.24) C8 - C7 S7 C9 - Distance Angles C10 1.3176 (0.0073) S7 1.7728 (0.0052) 122.17 (0.49) H9A 0.9700 106.79 106.79 H9B 0.9700 106.79 106.79 106.64 C9 - C10 S7 H9A C10 - Distance Angles C9 1.3176 (0.0073) S8 1.7604 (0.0054) 127.80 (0.44) H10A 0.9700 105.35 105.35 H10B 0.9700 105.35 105.35 106.00 C10 - C9 S8 H10A S1 - Distance Angles C4 1.7470 (0.0043) C1 1.8240 (0.0071) 98.30 (0.25) S1 - C4 S2 - Distance Angles C3 1.7333 (0.0041) C2 1.7560 (0.0057) 104.03 (0.26) S2 - C3 S3 - Distance Angles C3 1.7299 (0.0040) C5 1.7421 (0.0041) 96.08 (0.20) S3 - C3 S4 - Distance Angles C5 1.7277 (0.0041) C4 1.7431 (0.0044) 95.58 (0.20) S4 - C5 S5 - Distance Angles C6 1.7343 (0.0041) C7 1.7381 (0.0038) 95.69 (0.19) S5 - C6 S6 - Distance Angles C6 1.7345 (0.0041) C8 1.7461 (0.0039) 95.71 (0.19) S6 - C6 S7 - Distance Angles C8 1.7371 (0.0040) C9 1.7728 (0.0053) 100.47 (0.24) S7 - C8 S8 - Distance Angles C7 1.7386 (0.0039) C10 1.7604 (0.0054) 101.57 (0.23) S8 - C7 C11 - Distance Angles C11_$1 1.3764 (0.0070) S12 1.7215 (0.0038) 122.05 (0.39) S11 1.7220 (0.0038) 122.45 (0.40) 115.49 (0.20) C11 - C11_$1 S12 C12 - Distance Angles C13 1.3426 (0.0053) S13 1.7386 (0.0037) 129.47 (0.29) S12 1.7420 (0.0037) 116.76 (0.28) 113.75 (0.22) C12 - C13 S13 C13 - Distance Angles C12 1.3426 (0.0053) S11 1.7369 (0.0036) 116.88 (0.27) S14 1.7455 (0.0036) 127.07 (0.28) 115.97 (0.22) C13 - C12 S11 C14 - Distance Angles C15 1.4077 (0.0070) S14 1.7802 (0.0054) 121.31 (0.42) H14A 0.9700 107.00 107.00 H14B 0.9700 107.00 107.00 106.75 C14 - C15 S14 H14A C15 - Distance Angles C14 1.4077 (0.0070) S13 1.7686 (0.0047) 117.13 (0.40) H15A 0.9700 108.02 108.02 H15B 0.9700 108.02 108.02 107.25 C15 - C14 S13 H15A S11 - Distance Angles C11 1.7220 (0.0038) C13 1.7369 (0.0036) 95.46 (0.18) S11 - C11 S12 - Distance Angles C11 1.7215 (0.0039) C12 1.7420 (0.0037) 95.34 (0.18) S12 - C11 S13 - Distance Angles C12 1.7386 (0.0038) C15 1.7686 (0.0047) 101.33 (0.20) S13 - C12 S14 - Distance Angles C13 1.7455 (0.0036) C14 1.7802 (0.0055) 101.64 (0.23) S14 - C13 C21 - Distance Angles N21 1.3214 (0.0041) C22 1.4029 (0.0050) 123.80 (0.35) H21 0.9300 118.10 118.10 C21 - N21 C22 C22 - Distance Angles C23 1.3734 (0.0057) C21 1.4029 (0.0050) 119.02 (0.33) C33 1.5203 (0.0051) 123.82 (0.35) 117.16 (0.37) C22 - C23 C21 C23 - Distance Angles C22 1.3734 (0.0057) C24 1.4208 (0.0050) 118.72 (0.31) C34 1.5109 (0.0049) 121.38 (0.36) 119.90 (0.37) C23 - C22 C24 C24 - Distance Angles C25 1.4020 (0.0043) C31 1.4173 (0.0052) 117.30 (0.31) C23 1.4208 (0.0050) 117.69 (0.32) 125.01 (0.31) C24 - C25 C31 C25 - Distance Angles N21 1.3575 (0.0042) C24 1.4020 (0.0043) 123.10 (0.30) C26 1.4272 (0.0044) 116.52 (0.27) 120.37 (0.30) C25 - N21 C24 C26 - Distance Angles N22 1.3618 (0.0037) C27 1.4016 (0.0045) 122.28 (0.29) C25 1.4272 (0.0044) 116.36 (0.27) 121.35 (0.28) C26 - N22 C27 C27 - Distance Angles C26 1.4016 (0.0045) C28 1.4146 (0.0048) 118.72 (0.29) C32 1.4365 (0.0046) 116.51 (0.31) 124.76 (0.31) C27 - C26 C28 C28 - Distance Angles C29 1.3858 (0.0048) C27 1.4146 (0.0048) 118.00 (0.30) C35 1.5023 (0.0049) 121.06 (0.34) 120.94 (0.32) C28 - C29 C27 C29 - Distance Angles C28 1.3858 (0.0048) C30 1.3954 (0.0047) 119.26 (0.31) C36 1.5080 (0.0048) 123.59 (0.32) 117.15 (0.31) C29 - C28 C30 C30 - Distance Angles N22 1.3243 (0.0040) C29 1.3954 (0.0047) 123.74 (0.30) H30 0.9300 118.13 118.13 C30 - N22 C29 C31 - Distance Angles C32 1.3438 (0.0053) C24 1.4173 (0.0052) 122.58 (0.32) H31 0.9300 118.71 118.71 C31 - C32 C24 C32 - Distance Angles C31 1.3438 (0.0053) C27 1.4365 (0.0046) 121.87 (0.33) H32 0.9300 119.07 119.07 C32 - C31 C27 C33 - Distance Angles C22 1.5203 (0.0051) H33A 0.9600 109.47 H33B 0.9600 109.47 109.47 H33C 0.9600 109.47 109.47 109.47 C33 - C22 H33A H33B C34 - Distance Angles C23 1.5109 (0.0049) H34A 0.9600 109.47 H34B 0.9600 109.47 109.47 H34C 0.9600 109.47 109.47 109.47 C34 - C23 H34A H34B C35 - Distance Angles C28 1.5023 (0.0049) H35A 0.9600 109.47 H35B 0.9600 109.47 109.47 H35C 0.9600 109.47 109.47 109.47 C35 - C28 H35A H35B C36 - Distance Angles C29 1.5080 (0.0048) H36A 0.9600 109.47 H36B 0.9600 109.47 109.47 H36C 0.9600 109.47 109.47 109.47 C36 - C29 H36A H36B C41 - Distance Angles N41 1.1576 (0.0044) S41 1.6112 (0.0039) 179.21 (0.44) C41 - N41 C42 - Distance Angles N42 1.1558 (0.0044) S42 1.6122 (0.0038) 179.34 (0.35) C42 - N42 C43 - Distance Angles N43 1.1562 (0.0045) S43 1.6088 (0.0038) 179.06 (0.33) C43 - N43 C44 - Distance Angles N44 1.1519 (0.0043) S44 1.6152 (0.0038) 178.02 (0.35) C44 - N44 N21 - Distance Angles C21 1.3214 (0.0041) C25 1.3575 (0.0042) 117.67 (0.28) Cr1 2.0678 (0.0026) 128.30 (0.24) 114.03 (0.20) N21 - C21 C25 N22 - Distance Angles C30 1.3243 (0.0040) C26 1.3618 (0.0037) 117.99 (0.27) Cr1 2.0702 (0.0026) 128.12 (0.21) 113.87 (0.20) N22 - C30 C26 N41 - Distance Angles C41 1.1576 (0.0044) Cr1 1.9783 (0.0030) 177.49 (0.29) N41 - C41 N42 - Distance Angles C42 1.1558 (0.0044) Cr1 1.9822 (0.0029) 165.04 (0.30) N42 - C42 N43 - Distance Angles C43 1.1562 (0.0045) Cr1 1.9713 (0.0032) 172.22 (0.32) N43 - C43 N44 - Distance Angles C44 1.1519 (0.0043) Cr1 1.9928 (0.0030) 167.20 (0.29) N44 - C44 S41 - Distance Angles C41 1.6112 (0.0039) S41 - S42 - Distance Angles C42 1.6122 (0.0038) S42 - S43 - Distance Angles C43 1.6088 (0.0038) S43 - S44 - Distance Angles C44 1.6152 (0.0038) S44 - Cr1 - Distance Angles N43 1.9713 (0.0032) N41 1.9783 (0.0030) 91.10 (0.13) N42 1.9822 (0.0029) 95.25 (0.13) 92.36 (0.12) N44 1.9928 (0.0030) 90.09 (0.13) 176.76 (0.12) 90.54 (0.12) N21 2.0678 (0.0026) 93.64 (0.12) 89.10 (0.11) 170.96 (0.12) 87.81 (0.11) N22 2.0702 (0.0026) 172.78 (0.12) 87.78 (0.11) 91.93 (0.11) 90.67 (0.11) 79.21 (0.10) Cr1 - N43 N41 N42 N44 N21 FMAP and GRID set by program FMAP 2 1 42 GRID -2.564 -2 -1 2.564 2 1 R1 = 0.0919 for 10319 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.95 at 0.6052 0.3752 0.2135 [ 1.04 A from S1 ] Deepest hole -0.52 at 0.4990 0.5404 0.1954 [ 0.82 A from S1 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 5152 / 66477 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 1.3948 -0.3752 0.7865 1.00000 0.05 0.95 1.04 S1 2.03 C4 2.15 C1 2.24 H1A Q2 1 0.8448 -0.2101 0.8077 1.00000 0.05 0.55 1.01 C14 1.12 H15B 1.16 C15 1.28 H14A Q3 1 1.0770 0.1931 0.6101 1.00000 0.05 0.52 0.98 N22 1.17 CR1 1.78 C26 1.91 N21 Q4 1 1.2229 -0.5999 0.8293 1.00000 0.05 0.47 0.90 S2 1.10 C2 1.74 C3 1.78 H2A Q5 1 1.2317 -0.3271 1.1800 1.00000 0.05 0.46 1.12 S7 1.63 H9B 1.66 C9 1.76 C8 Q6 1 0.7930 -0.0802 0.6975 1.00000 0.05 0.45 0.75 S41 1.41 C41 2.49 N41 2.81 H32 Q7 1 1.1691 0.1627 0.7014 1.00000 0.05 0.44 1.00 N43 1.14 CR1 2.05 N42 2.10 N44 Q8 1 0.8582 -0.3454 0.8505 1.00000 0.05 0.42 1.00 C15 1.10 H14B 1.15 C14 1.25 H15A Q9 1 0.7945 -0.2799 0.8815 1.00000 0.05 0.39 0.87 S13 1.00 C15 1.63 H15A 1.70 H15B Q10 1 0.6825 0.0199 0.6739 1.00000 0.05 0.37 0.79 S41 1.54 C41 2.56 H31 2.61 N41 Shortest distances between peaks (including symmetry equivalents) 8 9 1.17 6 10 1.37 2 8 1.65 2 9 1.88 3 7 2.30 2 6 2.78 Time profile in seconds ----------------------- 0.20: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: 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. 3.22: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.05: Set up l.s. refinement 0.00: Generate idealized H-atoms 15.47: Structure factors and derivatives 65.94: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.11: Apply other restraints 6.22: Solve l.s. equations 0.00: Generate HTAB table 0.17: Other dependent quantities, CIF, tables 0.22: Analysis of variance 0.11: Merge reflections for Fourier and .fcf 0.23: Fourier summations 0.09: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 14:03:41 Total CPU time: 92.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++