+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 16:15:33 on 02-Aug-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 00SRC130 in P2(1)/c CELL 0.71073 9.5400 13.2477 28.5916 90.000 98.729 90.000 ZERR 4.00 0.0019 0.0026 0.0057 0.000 0.030 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H O SB UNIT 176 180 16 4 V = 3571.64 F(000) = 1568.0 Mu = 0.82 mm-1 Cell Wt = 3038.20 Rho = 1.413 L.S. 4 BOND FMAP 2 PLAN 10 TWIN SIZE 0.15 0.15 0.1 OMIT -3 55 OMIT 0 0 2 OMIT 0 1 1 OMIT -4 4 5 OMIT 4 1 5 OMIT 8 2 4 OMIT -4 1 3 OMIT 4 5 1 OMIT 7 2 2 OMIT 2 1 10 OMIT 8 2 12 OMIT -5 2 8 OMIT 7 2 10 OMIT -6 2 2 OMIT -5 4 3 WGHT 0.100000 BASF 0.62837 FVAR 0.12421 SB1 4 0.154491 0.133824 0.122833 11.00000 0.03441 0.02521 = 0.02405 -0.00138 -0.01022 0.00173 O1 3 0.170376 0.256042 0.075116 11.00000 0.03936 0.02790 = 0.02827 0.00303 -0.01711 0.00392 O2 3 0.405508 0.237665 0.056062 11.00000 0.05433 0.04831 = 0.04454 -0.00589 -0.00834 -0.00583 O3 3 0.122077 0.011158 0.169316 11.00000 0.03775 0.02759 = 0.03232 0.00389 -0.01609 0.00030 O4 3 0.350910 0.006382 0.173993 11.00000 0.04608 0.04157 = 0.03569 -0.00520 -0.02350 0.00848 C1 1 0.237883 0.037190 0.066928 11.00000 0.03663 0.02403 = 0.02750 -0.00135 -0.01040 -0.00216 C2 1 0.352472 -0.027310 0.067807 11.00000 0.03755 0.03388 = 0.03063 0.00510 -0.00983 0.00356 AFIX 43 H2 2 0.410824 -0.032197 0.096887 11.00000 -1.20000 AFIX 0 C3 1 0.396346 -0.089605 0.029636 11.00000 0.04073 0.03304 = 0.03774 0.00042 -0.00303 0.01027 AFIX 43 H3 2 0.476597 -0.130150 0.035845 11.00000 -1.20000 AFIX 0 C4 1 0.328626 -0.088003 -0.009381 11.00000 0.05642 0.03125 = 0.03396 -0.00989 -0.00296 -0.00241 AFIX 43 H4 2 0.349552 -0.125189 -0.035033 11.00000 -1.20000 AFIX 0 C5 1 0.215294 -0.022920 -0.010547 11.00000 0.05582 0.04493 = 0.02826 -0.00689 -0.01553 0.00204 AFIX 43 H5 2 0.158337 -0.017736 -0.039877 11.00000 -1.20000 AFIX 0 C6 1 0.169070 0.040212 0.027187 11.00000 0.04454 0.03618 = 0.03589 -0.00011 -0.02029 -0.00173 AFIX 43 H6 2 0.089387 0.081256 0.020757 11.00000 -1.20000 AFIX 0 C7 1 -0.067461 0.147515 0.127950 11.00000 0.03641 0.03650 = 0.02513 -0.00739 -0.01099 0.00385 C8 1 -0.155928 0.065160 0.144225 11.00000 0.03291 0.03866 = 0.04420 -0.00972 -0.01547 0.00346 AFIX 43 H8 2 -0.111622 0.004229 0.153357 11.00000 -1.20000 AFIX 0 C9 1 -0.299298 0.073571 0.146603 11.00000 0.03446 0.04422 = 0.05458 -0.01206 -0.01307 -0.00074 AFIX 43 H9 2 -0.350803 0.020055 0.156429 11.00000 -1.20000 AFIX 0 C10 1 -0.359806 0.162066 0.134125 11.00000 0.02929 0.06589 = 0.04896 -0.00552 -0.00938 0.00938 AFIX 43 H10 2 -0.455786 0.171784 0.135245 11.00000 -1.20000 AFIX 0 C11 1 -0.276906 0.241909 0.119036 11.00000 0.04207 0.05857 = 0.04589 -0.00011 -0.00874 0.01491 AFIX 43 H11 2 -0.323170 0.302570 0.110760 11.00000 -1.20000 AFIX 0 C12 1 -0.126711 0.237140 0.115411 11.00000 0.03568 0.04181 = 0.03551 0.00177 -0.01285 0.00819 AFIX 43 H12 2 -0.076532 0.291114 0.105354 11.00000 -1.20000 AFIX 0 C13 1 0.230852 0.222453 0.175101 11.00000 0.03102 0.02653 = 0.02909 -0.00014 -0.01868 0.00763 C14 1 0.176879 0.201752 0.221948 11.00000 0.06112 0.03024 = 0.03079 0.00041 -0.01892 0.00174 AFIX 43 H14 2 0.113348 0.149660 0.224767 11.00000 -1.20000 AFIX 0 C15 1 0.223637 0.260279 0.257971 11.00000 0.06953 0.03958 = 0.03288 -0.00344 -0.02028 0.01629 AFIX 43 H15 2 0.200480 0.251070 0.288126 11.00000 -1.20000 AFIX 0 C16 1 0.312076 0.338159 0.246451 11.00000 0.06274 0.03949 = 0.04726 -0.01262 -0.03745 0.01011 AFIX 43 H16 2 0.342738 0.382803 0.270979 11.00000 -1.20000 AFIX 0 C17 1 0.365886 0.361056 0.199853 11.00000 0.06058 0.03355 = 0.05302 -0.01045 -0.03040 0.00577 AFIX 43 H17 2 0.427866 0.414309 0.197393 11.00000 -1.20000 AFIX 0 C18 1 0.321440 0.302812 0.163407 11.00000 0.03076 0.03435 = 0.03601 -0.00392 -0.01883 0.00275 AFIX 43 H18 2 0.345697 0.312352 0.133418 11.00000 -1.20000 AFIX 0 C19 1 0.292827 0.273482 0.047907 11.00000 0.05544 0.02668 = 0.02538 -0.00001 -0.01637 -0.00838 C20 1 0.288797 0.340745 0.005944 11.00000 0.07787 0.04719 = 0.04418 0.00274 -0.02081 -0.01776 AFIX 13 H20 2 0.386951 0.349083 0.000330 11.00000 -1.20000 AFIX 0 C21 1 0.217838 0.289347 -0.032488 11.00000 0.05414 0.03223 = 0.02684 0.00368 -0.01325 0.00228 C22 1 0.074392 0.266662 -0.025979 11.00000 0.05330 0.03924 = 0.04785 0.00590 -0.00638 0.00294 AFIX 43 H22 2 0.030952 0.285971 -0.000381 11.00000 -1.20000 AFIX 0 C23 1 0.019722 0.217198 -0.060334 11.00000 0.05340 0.03808 = 0.07258 0.00759 -0.02798 -0.00083 AFIX 43 H23 2 -0.073789 0.196228 -0.061533 11.00000 -1.20000 AFIX 0 C24 1 0.098374 0.188565 -0.101183 11.00000 0.11945 0.03415 = 0.06775 -0.00450 -0.06522 0.00556 AFIX 43 H24 2 0.045260 0.152091 -0.125449 11.00000 -1.20000 AFIX 0 C25 1 0.244717 0.209840 -0.107926 11.00000 0.13336 0.05961 = 0.03059 -0.00569 -0.01777 0.04818 AFIX 43 H25 2 0.287621 0.189966 -0.133557 11.00000 -1.20000 AFIX 0 C26 1 0.300753 0.259041 -0.073317 11.00000 0.04197 0.05954 = 0.04247 0.01292 -0.00758 0.00966 AFIX 43 H26 2 0.395054 0.278517 -0.071599 11.00000 -1.20000 AFIX 0 C27 1 0.238120 0.442838 0.018997 11.00000 0.07482 0.03718 = 0.05771 0.00069 -0.04123 0.00982 AFIX 13 H27 2 0.141479 0.436750 0.026393 11.00000 -1.20000 AFIX 0 C28 1 0.319680 0.499343 0.054252 11.00000 0.05578 0.03228 = 0.03688 -0.00201 -0.02416 -0.00248 AFIX 23 H28A 2 0.419359 0.492450 0.051549 11.00000 -1.20000 H28B 2 0.305689 0.474617 0.085141 11.00000 -1.20000 AFIX 0 C29 1 0.276550 0.609479 0.049232 11.00000 0.04057 0.03936 = 0.04606 -0.00247 -0.01302 0.01110 AFIX 23 H29A 2 0.343171 0.653190 0.068669 11.00000 -1.20000 H29B 2 0.181720 0.620680 0.056510 11.00000 -1.20000 AFIX 0 C30 1 0.283549 0.622735 -0.004494 11.00000 0.04565 0.03996 = 0.04940 0.00395 -0.01091 0.00557 AFIX 23 H30A 2 0.218687 0.674589 -0.018555 11.00000 -1.20000 H30B 2 0.378852 0.638698 -0.010079 11.00000 -1.20000 AFIX 0 C31 1 0.238758 0.520718 -0.022539 11.00000 0.06415 0.04189 = 0.04724 -0.00365 -0.03185 0.00240 AFIX 23 H31A 2 0.302929 0.497249 -0.043473 11.00000 -1.20000 H31B 2 0.144413 0.524736 -0.040709 11.00000 -1.20000 AFIX 0 C32 1 0.230333 -0.024683 0.185797 11.00000 0.04873 0.02526 = 0.02326 -0.00207 -0.00586 0.00501 C33 1 0.192572 -0.109521 0.222454 11.00000 0.07164 0.03492 = 0.03030 0.00294 -0.00484 0.00354 AFIX 13 H33 2 0.099246 -0.134645 0.208137 11.00000 -1.20000 AFIX 0 C34 1 0.164939 -0.059924 0.270466 11.00000 0.03496 0.02582 = 0.02822 0.00399 -0.01123 0.00201 C35 1 0.028838 -0.055773 0.293934 11.00000 0.05388 0.04539 = 0.05999 0.00036 -0.01640 -0.00662 AFIX 43 H35 2 -0.047410 -0.090831 0.277352 11.00000 -1.20000 AFIX 0 C36 1 -0.002815 -0.007431 0.337068 11.00000 0.06511 0.07418 = 0.07612 -0.01342 0.02197 -0.00044 AFIX 43 H36 2 -0.089936 -0.007275 0.347902 11.00000 -1.20000 AFIX 0 C37 1 0.113269 0.035366 0.357542 11.00000 0.10036 0.03956 = 0.03787 -0.00705 -0.00683 -0.00572 AFIX 43 H37 2 0.115073 0.068981 0.386183 11.00000 -1.20000 AFIX 0 C38 1 0.243055 0.029928 0.334632 11.00000 0.07778 0.05567 = 0.04765 -0.01030 -0.03418 0.00702 AFIX 43 H38 2 0.320943 0.062484 0.351638 11.00000 -1.20000 AFIX 0 C39 1 0.272060 -0.015279 0.291740 11.00000 0.04284 0.05853 = 0.04837 0.00318 -0.02290 0.00479 AFIX 43 H39 2 0.359163 -0.012035 0.280967 11.00000 -1.20000 AFIX 0 C40 1 0.290839 -0.193911 0.216139 11.00000 0.06834 0.04199 = 0.05407 -0.00113 -0.01249 0.01191 AFIX 13 H40 2 0.387075 -0.170298 0.227924 11.00000 -1.20000 AFIX 0 C41 1 0.255976 -0.280621 0.250482 11.00000 0.11505 0.04149 = 0.04016 0.01090 0.00595 0.02115 AFIX 23 H41A 2 0.293355 -0.267136 0.283358 11.00000 -1.20000 H41B 2 0.155470 -0.295762 0.247139 11.00000 -1.20000 AFIX 0 C42 1 0.342810 -0.364044 0.227872 11.00000 0.09740 0.06461 = 0.05568 -0.00625 -0.01272 0.00347 AFIX 23 H42A 2 0.433675 -0.372176 0.247925 11.00000 -1.20000 H42B 2 0.292415 -0.427590 0.228119 11.00000 -1.20000 AFIX 0 C43 1 0.370129 -0.343803 0.177051 11.00000 0.13715 0.07588 = 0.05361 -0.00785 -0.01228 0.01758 AFIX 23 H43A 2 0.470606 -0.337676 0.175442 11.00000 -1.20000 H43B 2 0.329322 -0.396041 0.155388 11.00000 -1.20000 AFIX 0 C44 1 0.296471 -0.247629 0.167650 11.00000 0.11434 0.05220 = 0.03268 0.00040 0.01000 0.01176 AFIX 23 H44A 2 0.201096 -0.259054 0.151263 11.00000 -1.20000 H44B 2 0.346462 -0.205617 0.147815 11.00000 -1.20000 HKLF 4 Covalent radii and connectivity table for 00SRC130 in P2(1)/c C 0.770 H 0.320 O 0.660 SB 1.410 Sb1 - C13 O1 O3 C7 C1 O1 - C19 Sb1 O2 - C19 O3 - C32 Sb1 O4 - C32 C1 - C6 C2 Sb1 C2 - C1 C3 C3 - C4 C2 C4 - C3 C5 C5 - C4 C6 C6 - C1 C5 C7 - C12 C8 Sb1 C8 - C9 C7 C9 - C10 C8 C10 - C9 C11 C11 - C10 C12 C12 - C7 C11 C13 - C18 C14 Sb1 C14 - C15 C13 C15 - C14 C16 C16 - C15 C17 C17 - C18 C16 C18 - C17 C13 C19 - O2 C20 O1 C20 - C21 C19 C27 C21 - C20 C22 C26 C22 - C23 C21 C23 - C22 C24 C24 - C25 C23 C25 - C26 C24 C26 - C25 C21 C27 - C28 C20 C31 C28 - C27 C29 C29 - C28 C30 C30 - C31 C29 C31 - C30 C27 C32 - O3 O4 C33 C33 - C40 C34 C32 C34 - C39 C35 C33 C35 - C36 C34 C36 - C37 C35 C37 - C36 C38 C38 - C39 C37 C39 - C34 C38 C40 - C33 C44 C41 C41 - C42 C40 C42 - C43 C41 C43 - C44 C42 C44 - C43 C40 h k l Fo^2 Sigma Why rejected 8 0 11 3.85 0.79 observed but should be systematically absent 8 0 9 9.94 2.26 observed but should be systematically absent 8 0 9 4.52 0.90 observed but should be systematically absent 8 0 3 7.51 1.68 observed but should be systematically absent 7 0 11 5.11 0.91 observed but should be systematically absent 7 0 11 7.63 1.35 observed but should be systematically absent 7 0 7 7.80 1.34 observed but should be systematically absent -7 0 1 6.21 1.47 observed but should be systematically absent -7 0 5 6.20 1.47 observed but should be systematically absent 6 0 25 5.38 1.01 observed but should be systematically absent 6 0 17 3.54 0.80 observed but should be systematically absent 6 0 9 3.41 0.80 observed but should be systematically absent 6 0 1 2.78 0.67 observed but should be systematically absent -6 0 11 2.18 0.34 observed but should be systematically absent -6 0 11 1.82 0.34 observed but should be systematically absent 5 0 21 1.69 0.34 observed but should be systematically absent 5 0 7 4.13 0.78 observed but should be systematically absent 5 0 3 3.89 0.89 observed but should be systematically absent 5 0 3 4.62 0.90 observed but should be systematically absent 5 0 1 5.66 1.22 observed but should be systematically absent 5 0 1 4.87 0.79 observed but should be systematically absent -5 0 1 4.88 0.78 observed but should be systematically absent -5 0 1 3.17 0.79 observed but should be systematically absent 4 0 19 2.58 0.22 observed but should be systematically absent 4 0 19 1.80 0.22 observed but should be systematically absent 4 0 11 5.27 0.80 observed but should be systematically absent 4 0 11 4.57 0.69 observed but should be systematically absent 4 0 11 5.78 0.68 observed but should be systematically absent 4 0 11 6.06 0.88 observed but should be systematically absent 4 0 7 5.35 0.66 observed but should be systematically absent 4 0 7 5.82 1.03 observed but should be systematically absent 4 0 7 5.91 0.91 observed but should be systematically absent 4 0 7 4.90 0.68 observed but should be systematically absent 4 0 3 12.87 1.24 observed but should be systematically absent 4 0 3 13.00 0.87 observed but should be systematically absent 4 0 3 13.98 1.02 observed but should be systematically absent -4 0 1 5.33 0.68 observed but should be systematically absent -4 0 1 7.87 1.00 observed but should be systematically absent -4 0 5 2.78 0.67 observed but should be systematically absent -4 0 5 3.68 0.89 observed but should be systematically absent -4 0 5 3.50 0.79 observed but should be systematically absent -4 0 5 2.53 0.23 observed but should be systematically absent -4 0 5 2.82 0.23 observed but should be systematically absent -4 0 9 2.21 0.44 observed but should be systematically absent -4 0 13 3.89 0.67 observed but should be systematically absent 3 0 9 2.94 0.45 observed but should be systematically absent 3 0 9 3.10 0.57 observed but should be systematically absent 3 0 9 4.00 0.57 observed but should be systematically absent 3 0 9 3.20 0.55 observed but should be systematically absent 3 0 5 2.16 0.46 observed but should be systematically absent ** etc. ** 62283 Reflections read, of which 4366 rejected -12 =< h =< 10, -17 =< k =< 17, -34 =< l =< 36, Max. 2-theta = 55.00 115 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 1 0 0 11.91 0.06 6 73.08 1 1 0 314.28 4.11 14 23.68 -2 1 1 230.70 0.78 14 20.74 1 0 2 99.39 0.55 6 153.30 0 1 2 9.09 0.05 11 57.62 0 1 3 75.80 0.11 11 38.85 3 3 4 21.24 0.11 13 1.66 -1 4 5 8.56 0.10 14 0.51 5 6 7 52.80 0.23 14 5.74 -2 7 8 33.09 0.11 15 2.56 1 2 10 9.21 0.10 11 0.79 1 3 11 139.96 0.11 15 49.36 1 1 12 17.35 0.20 13 1.13 13 Inconsistent equivalents 7391 Unique reflections, of which 0 suppressed R(int) = 0.0723 R(sigma) = 0.0470 Friedel opposites merged Maximum memory for data reduction = 4158 / 75416 Default effective X-H distances for T = 20.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 0.98 0.97 0.96 0.93 0.86 0.89 1.10 0.82 0.93 0.86 0.93 Note that these distances are chosen to give the best fit to the X-ray data and so avoid the introduction of systematic error. The true internuclear distances are longer and do not vary with temperature ! The apparent variation with temperature is caused by libration. Least-squares cycle 1 Maximum vector length = 511 Memory required = 5417 / 574973 wR2 = 0.1945 before cycle 1 for 7391 data and 443 / 443 parameters GooF = S = 1.430; Restrained GooF = 1.430 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.12421 0.00033 -0.004 OSF 2 0.62837 9.99999 0.000 BASF 1 Mean shift/esd = 0.001 Maximum = -0.028 for U23 Sb1 Max. shift = 0.000 A for C20 Max. dU = 0.000 for C43 Least-squares cycle 2 Maximum vector length = 511 Memory required = 5417 / 574973 wR2 = 0.1945 before cycle 2 for 7391 data and 443 / 443 parameters GooF = S = 1.430; Restrained GooF = 1.430 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.12421 0.00033 -0.005 OSF 2 0.62837 9.99999 0.000 BASF 1 Mean shift/esd = 0.001 Maximum = -0.011 for U23 Sb1 Max. shift = 0.000 A for C20 Max. dU = 0.000 for C43 Least-squares cycle 3 Maximum vector length = 511 Memory required = 5417 / 574973 wR2 = 0.1945 before cycle 3 for 7391 data and 443 / 443 parameters GooF = S = 1.430; Restrained GooF = 1.430 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.12421 0.00033 -0.001 OSF 2 0.62837 9.99999 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.002 for U11 C20 Max. shift = 0.000 A for C20 Max. dU = 0.000 for C43 Least-squares cycle 4 Maximum vector length = 511 Memory required = 5417 / 574973 wR2 = 0.1945 before cycle 4 for 7391 data and 443 / 443 parameters GooF = S = 1.430; Restrained GooF = 1.430 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.12421 0.00033 0.000 OSF 2 0.62837 9.99999 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = -0.002 for x C20 Max. shift = 0.000 A for C20 Max. dU = 0.000 for C20 Largest correlation matrix elements 0.620 U33 Sb1 / OSF 0.605 U22 Sb1 / OSF -0.508 U13 C24 / U33 C24 0.611 U11 Sb1 / OSF -0.508 U13 C24 / U11 C24 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.4108 -0.0322 0.0969 43 0.930 0.000 C2 C1 C3 H3 0.4766 -0.1301 0.0358 43 0.930 0.000 C3 C4 C2 H4 0.3496 -0.1252 -0.0350 43 0.930 0.000 C4 C3 C5 H5 0.1583 -0.0177 -0.0399 43 0.930 0.000 C5 C4 C6 H6 0.0894 0.0813 0.0208 43 0.930 0.000 C6 C1 C5 H8 -0.1116 0.0042 0.1534 43 0.930 0.000 C8 C9 C7 H9 -0.3508 0.0201 0.1564 43 0.930 0.000 C9 C10 C8 H10 -0.4558 0.1718 0.1352 43 0.930 0.000 C10 C9 C11 H11 -0.3232 0.3026 0.1108 43 0.930 0.000 C11 C10 C12 H12 -0.0765 0.2911 0.1054 43 0.930 0.000 C12 C7 C11 H14 0.1133 0.1497 0.2248 43 0.930 0.000 C14 C15 C13 H15 0.2005 0.2511 0.2881 43 0.930 0.000 C15 C14 C16 H16 0.3427 0.3828 0.2710 43 0.930 0.000 C16 C15 C17 H17 0.4279 0.4143 0.1974 43 0.930 0.000 C17 C18 C16 H18 0.3457 0.3124 0.1334 43 0.930 0.000 C18 C17 C13 H20 0.3869 0.3491 0.0003 13 0.980 0.000 C20 C21 C19 C27 H22 0.0309 0.2860 -0.0004 43 0.930 0.000 C22 C23 C21 H23 -0.0738 0.1962 -0.0615 43 0.930 0.000 C23 C22 C24 H24 0.0453 0.1521 -0.1254 43 0.930 0.000 C24 C25 C23 H25 0.2876 0.1900 -0.1336 43 0.930 0.000 C25 C26 C24 H26 0.3950 0.2785 -0.0716 43 0.930 0.000 C26 C25 C21 H27 0.1415 0.4368 0.0264 13 0.980 0.000 C27 C28 C20 C31 H28A 0.4194 0.4924 0.0516 23 0.970 0.000 C28 C27 C29 H28B 0.3057 0.4746 0.0851 23 0.970 0.000 C28 C27 C29 H29A 0.3432 0.6532 0.0687 23 0.970 0.000 C29 C28 C30 H29B 0.1817 0.6207 0.0565 23 0.970 0.000 C29 C28 C30 H30A 0.2187 0.6746 -0.0186 23 0.970 0.000 C30 C31 C29 H30B 0.3789 0.6387 -0.0101 23 0.970 0.000 C30 C31 C29 H31A 0.3029 0.4972 -0.0435 23 0.970 0.000 C31 C30 C27 H31B 0.1444 0.5247 -0.0407 23 0.970 0.000 C31 C30 C27 H33 0.0992 -0.1346 0.2081 13 0.980 0.000 C33 C40 C34 C32 H35 -0.0474 -0.0908 0.2774 43 0.930 0.000 C35 C36 C34 H36 -0.0899 -0.0073 0.3479 43 0.930 0.000 C36 C37 C35 H37 0.1151 0.0690 0.3862 43 0.930 0.000 C37 C36 C38 H38 0.3209 0.0625 0.3516 43 0.930 0.000 C38 C39 C37 H39 0.3592 -0.0120 0.2810 43 0.930 0.000 C39 C34 C38 H40 0.3871 -0.1703 0.2279 13 0.980 0.000 C40 C33 C44 C41 H41A 0.2934 -0.2671 0.2834 23 0.970 0.000 C41 C42 C40 H41B 0.1555 -0.2958 0.2471 23 0.970 0.000 C41 C42 C40 H42A 0.4337 -0.3722 0.2479 23 0.970 0.000 C42 C43 C41 H42B 0.2924 -0.4276 0.2281 23 0.970 0.000 C42 C43 C41 H43A 0.4706 -0.3377 0.1754 23 0.970 0.000 C43 C44 C42 H43B 0.3293 -0.3960 0.1554 23 0.970 0.000 C43 C44 C42 H44A 0.2011 -0.2591 0.1513 23 0.970 0.000 C44 C43 C40 H44B 0.3465 -0.2056 0.1478 23 0.970 0.000 C44 C43 C40 00SRC130 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Sb1 0.15449 0.13382 0.12283 1.00000 0.03441 0.02521 0.02405 -0.00138 -0.01022 0.00173 0.02940 0.00050 0.00003 0.00002 0.00001 0.00000 0.00025 0.00022 0.00023 0.00011 0.00015 0.00013 0.00017 O1 0.17038 0.25604 0.07512 1.00000 0.03935 0.02790 0.02827 0.00303 -0.01711 0.00392 0.03414 0.00549 0.00036 0.00024 0.00011 0.00000 0.00200 0.00174 0.00170 0.00136 0.00146 0.00147 0.00084 O2 0.40551 0.23767 0.05606 1.00000 0.05435 0.04830 0.04454 -0.00589 -0.00834 -0.00582 0.05070 0.00679 0.00045 0.00031 0.00014 0.00000 0.00265 0.00243 0.00231 0.00185 0.00194 0.00204 0.00105 O3 0.12208 0.01116 0.16932 1.00000 0.03775 0.02759 0.03231 0.00389 -0.01609 0.00029 0.03477 0.00563 0.00036 0.00024 0.00011 0.00000 0.00198 0.00176 0.00183 0.00140 0.00149 0.00147 0.00084 O4 0.35091 0.00638 0.17399 1.00000 0.04607 0.04157 0.03569 -0.00520 -0.02350 0.00848 0.04419 0.00606 0.00041 0.00028 0.00013 0.00000 0.00234 0.00214 0.00197 0.00164 0.00167 0.00180 0.00100 C1 0.23788 0.03719 0.06693 1.00000 0.03662 0.02404 0.02750 -0.00135 -0.01040 -0.00216 0.03097 0.00795 0.00052 0.00035 0.00016 0.00000 0.00274 0.00238 0.00248 0.00188 0.00199 0.00204 0.00112 C2 0.35247 -0.02731 0.06781 1.00000 0.03755 0.03388 0.03063 0.00511 -0.00983 0.00356 0.03558 0.00873 0.00054 0.00037 0.00017 0.00000 0.00285 0.00268 0.00261 0.00211 0.00211 0.00225 0.00121 H2 0.41083 -0.03219 0.09689 1.00000 0.04269 0.00000 0.00000 C3 0.39635 -0.08960 0.02964 1.00000 0.04072 0.03303 0.03775 0.00042 -0.00303 0.01028 0.03810 0.00946 0.00057 0.00040 0.00018 0.00000 0.00306 0.00283 0.00291 0.00232 0.00230 0.00242 0.00124 H3 0.47660 -0.13015 0.03585 1.00000 0.04571 0.00000 0.00000 C4 0.32863 -0.08800 -0.00938 1.00000 0.05642 0.03125 0.03396 -0.00989 -0.00296 -0.00241 0.04156 0.00920 0.00062 0.00040 0.00019 0.00000 0.00358 0.00290 0.00288 0.00228 0.00248 0.00261 0.00133 H4 0.34955 -0.12519 -0.03503 1.00000 0.04987 0.00000 0.00000 C5 0.21529 -0.02292 -0.01055 1.00000 0.05581 0.04492 0.02826 -0.00688 -0.01553 0.00203 0.04527 0.00918 0.00062 0.00042 0.00018 0.00000 0.00357 0.00324 0.00273 0.00232 0.00241 0.00270 0.00144 H5 0.15834 -0.01773 -0.03988 1.00000 0.05432 0.00000 0.00000 C6 0.16907 0.04021 0.02719 1.00000 0.04454 0.03619 0.03589 -0.00010 -0.02030 -0.00174 0.04160 0.00848 0.00058 0.00040 0.00018 0.00000 0.00315 0.00288 0.00285 0.00223 0.00234 0.00238 0.00137 H6 0.08938 0.08125 0.02076 1.00000 0.04992 0.00000 0.00000 C7 -0.06746 0.14751 0.12795 1.00000 0.03642 0.03651 0.02513 -0.00739 -0.01100 0.00385 0.03431 0.00837 0.00056 0.00037 0.00017 0.00000 0.00289 0.00284 0.00253 0.00202 0.00210 0.00217 0.00123 C8 -0.15593 0.06516 0.14422 1.00000 0.03291 0.03866 0.04420 -0.00972 -0.01547 0.00347 0.04080 0.00847 0.00054 0.00041 0.00019 0.00000 0.00289 0.00294 0.00306 0.00236 0.00228 0.00228 0.00135 H8 -0.11162 0.00423 0.15336 1.00000 0.04896 0.00000 0.00000 C9 -0.29930 0.07357 0.14660 1.00000 0.03445 0.04423 0.05458 -0.01205 -0.01307 -0.00074 0.04647 0.00914 0.00057 0.00044 0.00021 0.00000 0.00305 0.00335 0.00355 0.00267 0.00252 0.00244 0.00146 H9 -0.35081 0.02006 0.15643 1.00000 0.05577 0.00000 0.00000 C10 -0.35981 0.16207 0.13412 1.00000 0.02930 0.06590 0.04896 -0.00552 -0.00938 0.00938 0.04964 0.01091 0.00060 0.00054 0.00021 0.00000 0.00307 0.00406 0.00338 0.00312 0.00249 0.00275 0.00154 H10 -0.45579 0.17178 0.13524 1.00000 0.05957 0.00000 0.00000 C11 -0.27691 0.24191 0.11904 1.00000 0.04208 0.05859 0.04589 -0.00010 -0.00874 0.01490 0.05045 0.01065 0.00062 0.00049 0.00020 0.00000 0.00350 0.00390 0.00332 0.00285 0.00255 0.00300 0.00156 H11 -0.32317 0.30257 0.11076 1.00000 0.06054 0.00000 0.00000 C12 -0.12671 0.23714 0.11541 1.00000 0.03568 0.04180 0.03551 0.00177 -0.01285 0.00819 0.03955 0.00892 0.00055 0.00041 0.00018 0.00000 0.00296 0.00306 0.00273 0.00226 0.00220 0.00235 0.00129 H12 -0.07653 0.29112 0.10535 1.00000 0.04746 0.00000 0.00000 C13 0.23085 0.22245 0.17510 1.00000 0.03101 0.02654 0.02908 -0.00015 -0.01868 0.00764 0.03128 0.00775 0.00050 0.00034 0.00016 0.00000 0.00261 0.00246 0.00244 0.00190 0.00196 0.00201 0.00116 C14 0.17688 0.20175 0.22195 1.00000 0.06111 0.03024 0.03079 0.00041 -0.01892 0.00173 0.04340 0.00917 0.00063 0.00039 0.00018 0.00000 0.00364 0.00268 0.00269 0.00213 0.00241 0.00251 0.00141 H14 0.11335 0.14966 0.22477 1.00000 0.05207 0.00000 0.00000 C15 0.22364 0.26028 0.25797 1.00000 0.06952 0.03959 0.03288 -0.00344 -0.02027 0.01630 0.05023 0.01020 0.00069 0.00043 0.00020 0.00000 0.00408 0.00323 0.00289 0.00237 0.00265 0.00295 0.00162 H15 0.20048 0.25107 0.28813 1.00000 0.06028 0.00000 0.00000 C16 0.31208 0.33816 0.24645 1.00000 0.06274 0.03949 0.04725 -0.01262 -0.03744 0.01011 0.05457 0.00952 0.00067 0.00045 0.00021 0.00000 0.00400 0.00314 0.00355 0.00270 0.00296 0.00288 0.00182 H16 0.34274 0.38280 0.27098 1.00000 0.06548 0.00000 0.00000 C17 0.36589 0.36106 0.19985 1.00000 0.06058 0.03355 0.05303 -0.01046 -0.03041 0.00578 0.05309 0.00964 0.00071 0.00040 0.00023 0.00000 0.00405 0.00314 0.00385 0.00243 0.00308 0.00255 0.00182 H17 0.42786 0.41431 0.19739 1.00000 0.06371 0.00000 0.00000 C18 0.32144 0.30281 0.16341 1.00000 0.03077 0.03435 0.03601 -0.00392 -0.01882 0.00275 0.03619 0.00803 0.00051 0.00037 0.00018 0.00000 0.00266 0.00273 0.00272 0.00213 0.00210 0.00214 0.00125 H18 0.34570 0.31235 0.13342 1.00000 0.04342 0.00000 0.00000 C19 0.29283 0.27348 0.04791 1.00000 0.05544 0.02668 0.02537 -0.00001 -0.01637 -0.00839 0.03816 0.00829 0.00063 0.00037 0.00017 0.00000 0.00363 0.00262 0.00252 0.00199 0.00239 0.00245 0.00135 C20 0.28879 0.34075 0.00594 1.00000 0.07793 0.04718 0.04417 0.00275 -0.02083 -0.01778 0.05954 0.01058 0.00082 0.00048 0.00022 0.00000 0.00476 0.00356 0.00358 0.00283 0.00318 0.00328 0.00187 H20 0.38694 0.34909 0.00033 1.00000 0.07145 0.00000 0.00000 C21 0.21784 0.28935 -0.03249 1.00000 0.05415 0.03223 0.02684 0.00368 -0.01325 0.00227 0.03975 0.00910 0.00061 0.00039 0.00017 0.00000 0.00346 0.00274 0.00255 0.00206 0.00229 0.00242 0.00132 C22 0.07439 0.26666 -0.02598 1.00000 0.05330 0.03924 0.04785 0.00590 -0.00639 0.00294 0.04826 0.01059 0.00064 0.00043 0.00022 0.00000 0.00376 0.00316 0.00339 0.00260 0.00276 0.00271 0.00149 H22 0.03095 0.28597 -0.00038 1.00000 0.05791 0.00000 0.00000 C23 0.01972 0.21720 -0.06033 1.00000 0.05342 0.03807 0.07258 0.00760 -0.02798 -0.00084 0.05858 0.01089 0.00070 0.00045 0.00025 0.00000 0.00381 0.00333 0.00460 0.00313 0.00331 0.00282 0.00186 H23 -0.07379 0.19623 -0.06153 1.00000 0.07030 0.00000 0.00000 C24 0.09837 0.18857 -0.10118 1.00000 0.11947 0.03416 0.06775 -0.00450 -0.06522 0.00557 0.08202 0.01126 0.00102 0.00046 0.00027 0.00000 0.00688 0.00352 0.00470 0.00314 0.00467 0.00388 0.00286 H24 0.04525 0.15209 -0.12545 1.00000 0.09842 0.00000 0.00000 C25 0.24472 0.20984 -0.10793 1.00000 0.13335 0.05960 0.03059 -0.00568 -0.01776 0.04815 0.07764 0.01487 0.00104 0.00054 0.00022 0.00000 0.00765 0.00433 0.00327 0.00299 0.00396 0.00481 0.00266 H25 0.28762 0.18996 -0.13356 1.00000 0.09317 0.00000 0.00000 C26 0.30075 0.25904 -0.07332 1.00000 0.04198 0.05956 0.04247 0.01292 -0.00759 0.00966 0.04945 0.01099 0.00062 0.00047 0.00020 0.00000 0.00328 0.00380 0.00331 0.00279 0.00256 0.00280 0.00151 H26 0.39505 0.27852 -0.07160 1.00000 0.05934 0.00000 0.00000 C27 0.23812 0.44284 0.01900 1.00000 0.07485 0.03719 0.05771 0.00069 -0.04125 0.00982 0.06190 0.01018 0.00074 0.00044 0.00022 0.00000 0.00452 0.00322 0.00387 0.00275 0.00333 0.00300 0.00201 H27 0.14148 0.43675 0.02639 1.00000 0.07427 0.00000 0.00000 C28 0.31968 0.49934 0.05425 1.00000 0.05578 0.03228 0.03688 -0.00201 -0.02415 -0.00248 0.04487 0.00859 0.00065 0.00039 0.00019 0.00000 0.00354 0.00283 0.00294 0.00227 0.00251 0.00248 0.00148 H28A 0.41936 0.49245 0.05155 1.00000 0.05385 0.00000 0.00000 H28B 0.30568 0.47462 0.08514 1.00000 0.05385 0.00000 0.00000 C29 0.27655 0.60948 0.04923 1.00000 0.04057 0.03936 0.04606 -0.00247 -0.01302 0.01110 0.04403 0.01014 0.00061 0.00042 0.00020 0.00000 0.00318 0.00294 0.00328 0.00248 0.00249 0.00246 0.00142 H29A 0.34317 0.65319 0.06867 1.00000 0.05283 0.00000 0.00000 H29B 0.18172 0.62068 0.05651 1.00000 0.05283 0.00000 0.00000 C30 0.28355 0.62273 -0.00449 1.00000 0.04565 0.03996 0.04940 0.00395 -0.01091 0.00556 0.04688 0.01036 0.00067 0.00040 0.00022 0.00000 0.00346 0.00323 0.00352 0.00242 0.00269 0.00248 0.00151 H30A 0.21869 0.67459 -0.01856 1.00000 0.05626 0.00000 0.00000 H30B 0.37885 0.63870 -0.01008 1.00000 0.05626 0.00000 0.00000 C31 0.23876 0.52072 -0.02254 1.00000 0.06414 0.04189 0.04724 -0.00366 -0.03185 0.00241 0.05526 0.00936 0.00067 0.00043 0.00021 0.00000 0.00398 0.00328 0.00340 0.00261 0.00288 0.00281 0.00174 H31A 0.30293 0.49725 -0.04347 1.00000 0.06631 0.00000 0.00000 H31B 0.14441 0.52474 -0.04071 1.00000 0.06631 0.00000 0.00000 C32 0.23033 -0.02468 0.18580 1.00000 0.04874 0.02526 0.02326 -0.00207 -0.00586 0.00500 0.03359 0.00874 0.00060 0.00036 0.00016 0.00000 0.00341 0.00245 0.00242 0.00194 0.00220 0.00236 0.00121 C33 0.19257 -0.10952 0.22245 1.00000 0.07164 0.03492 0.03030 0.00295 -0.00484 0.00353 0.04692 0.01088 0.00072 0.00043 0.00019 0.00000 0.00426 0.00287 0.00286 0.00227 0.00267 0.00283 0.00149 H33 0.09925 -0.13465 0.20814 1.00000 0.05631 0.00000 0.00000 C34 0.16494 -0.05992 0.27047 1.00000 0.03495 0.02583 0.02822 0.00399 -0.01123 0.00200 0.03132 0.00820 0.00052 0.00035 0.00017 0.00000 0.00277 0.00241 0.00244 0.00192 0.00204 0.00202 0.00114 C35 0.02883 -0.05577 0.29393 1.00000 0.05390 0.04539 0.06000 0.00036 -0.01640 -0.00661 0.05569 0.01091 0.00069 0.00046 0.00023 0.00000 0.00388 0.00346 0.00395 0.00292 0.00303 0.00289 0.00170 H35 -0.04741 -0.09083 0.27735 1.00000 0.06683 0.00000 0.00000 C36 -0.00282 -0.00743 0.33707 1.00000 0.06513 0.07421 0.07611 -0.01342 0.02197 -0.00044 0.07065 0.01396 0.00083 0.00058 0.00027 0.00000 0.00477 0.00510 0.00513 0.00403 0.00398 0.00396 0.00205 H36 -0.08994 -0.00728 0.34790 1.00000 0.08478 0.00000 0.00000 C37 0.11327 0.03537 0.35754 1.00000 0.10038 0.03956 0.03787 -0.00705 -0.00683 -0.00574 0.06106 0.01151 0.00086 0.00046 0.00022 0.00000 0.00583 0.00342 0.00333 0.00264 0.00350 0.00358 0.00193 H37 0.11507 0.06899 0.38618 1.00000 0.07327 0.00000 0.00000 C38 0.24305 0.02993 0.33463 1.00000 0.07776 0.05567 0.04765 -0.01030 -0.03418 0.00702 0.06488 0.01090 0.00079 0.00049 0.00023 0.00000 0.00491 0.00398 0.00373 0.00305 0.00347 0.00344 0.00206 H38 0.32094 0.06248 0.35164 1.00000 0.07786 0.00000 0.00000 C39 0.27206 -0.01528 0.29174 1.00000 0.04283 0.05853 0.04838 0.00318 -0.02290 0.00479 0.05300 0.00994 0.00063 0.00046 0.00021 0.00000 0.00332 0.00378 0.00346 0.00287 0.00264 0.00279 0.00162 H39 0.35916 -0.01204 0.28097 1.00000 0.06360 0.00000 0.00000 C40 0.29084 -0.19391 0.21614 1.00000 0.06838 0.04197 0.05407 -0.00113 -0.01248 0.01190 0.05706 0.01165 0.00074 0.00046 0.00022 0.00000 0.00431 0.00350 0.00378 0.00279 0.00312 0.00307 0.00172 H40 0.38707 -0.17029 0.22792 1.00000 0.06847 0.00000 0.00000 C41 0.25598 -0.28062 0.25048 1.00000 0.11504 0.04149 0.04016 0.01091 0.00596 0.02114 0.06617 0.01399 0.00091 0.00046 0.00021 0.00000 0.00605 0.00360 0.00350 0.00273 0.00361 0.00380 0.00202 H41A 0.29336 -0.26714 0.28336 1.00000 0.07940 0.00000 0.00000 H41B 0.15547 -0.29576 0.24714 1.00000 0.07940 0.00000 0.00000 C42 0.34281 -0.36404 0.22787 1.00000 0.09740 0.06460 0.05569 -0.00625 -0.01272 0.00345 0.07508 0.01451 0.00101 0.00053 0.00028 0.00000 0.00646 0.00507 0.00461 0.00326 0.00421 0.00387 0.00241 H42A 0.43367 -0.37217 0.24792 1.00000 0.09010 0.00000 0.00000 H42B 0.29241 -0.42759 0.22812 1.00000 0.09010 0.00000 0.00000 C43 0.37012 -0.34380 0.17705 1.00000 0.13721 0.07587 0.05361 -0.00785 -0.01230 0.01757 0.09167 0.01678 0.00118 0.00063 0.00028 0.00000 0.00850 0.00534 0.00462 0.00405 0.00483 0.00533 0.00292 H43A 0.47060 -0.33768 0.17544 1.00000 0.11000 0.00000 0.00000 H43B 0.32931 -0.39604 0.15539 1.00000 0.11000 0.00000 0.00000 C44 0.29647 -0.24763 0.16765 1.00000 0.11432 0.05220 0.03268 0.00040 0.01000 0.01176 0.06652 0.01385 0.00093 0.00050 0.00022 0.00000 0.00628 0.00400 0.00321 0.00282 0.00349 0.00397 0.00205 H44A 0.20110 -0.25905 0.15126 1.00000 0.07982 0.00000 0.00000 H44B 0.34647 -0.20562 0.14782 1.00000 0.07982 0.00000 0.00000 Final Structure Factor Calculation for 00SRC130 in P2(1)/c Total number of l.s. parameters = 443 Maximum vector length = 511 Memory required = 4974 / 22995 wR2 = 0.1945 before cycle 5 for 7391 data and 0 / 443 parameters GooF = S = 1.430; Restrained GooF = 1.430 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.1000 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0577 for 6026 Fo > 4sig(Fo) and 0.0778 for all 7391 data wR2 = 0.1945, GooF = S = 1.430, Restrained GooF = 1.430 for all data Occupancy sum of asymmetric unit = 49.00 for non-hydrogen and 45.00 for hydrogen atoms Principal mean square atomic displacements U 0.0476 0.0250 0.0156 Sb1 0.0608 0.0292 0.0125 O1 0.0689 0.0517 0.0315 O2 0.0606 0.0281 0.0156 O3 0.0794 0.0386 0.0146 O4 0.0508 0.0247 0.0174 C1 0.0522 0.0361 0.0185 C2 0.0535 0.0363 0.0245 C3 0.0620 0.0411 0.0216 C4 0.0730 0.0447 0.0181 C5 0.0717 0.0362 0.0169 C6 0.0541 0.0334 0.0154 C7 0.0682 0.0353 0.0189 C8 0.0740 0.0425 0.0229 C9 0.0741 0.0527 0.0222 C10 0.0726 0.0520 0.0267 C11 0.0587 0.0421 0.0179 C12 0.0586 0.0267 0.0085 C13 0.0806 0.0303 0.0192 C14 0.0949 0.0354 0.0204 C15 0.1136 0.0359 0.0142 C16 0.1051 0.0327 0.0214 C17 0.0626 0.0334 0.0125 C18 0.0728 0.0265 0.0152 C19 0.1063 0.0440 0.0283 C20 0.0677 0.0334 0.0181 C21 0.0675 0.0446 0.0326 C22 0.1092 0.0387 0.0278 C23 0.1917 0.0338 0.0205 C24 0.1697 0.0382 0.0251 C25 0.0665 0.0580 0.0239 C26 0.1281 0.0388 0.0188 C27 0.0845 0.0328 0.0173 C28 0.0700 0.0389 0.0232 C29 0.0690 0.0434 0.0283 C30 0.1044 0.0416 0.0197 C31 0.0562 0.0242 0.0204 C32 0.0776 0.0363 0.0268 C33 0.0509 0.0274 0.0157 C34 0.0873 0.0465 0.0333 C35 0.0903 0.0690 0.0527 C36 0.1082 0.0455 0.0295 C37 0.1193 0.0537 0.0217 C38 0.0809 0.0592 0.0189 C39 0.0906 0.0457 0.0349 C40 0.1218 0.0491 0.0276 C41 0.1138 0.0648 0.0466 C42 0.1551 0.0713 0.0486 C43 0.1171 0.0501 0.0324 C44 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.010 0.019 0.029 0.040 0.053 0.066 0.082 0.105 0.142 1.000 Number in group 806. 703. 749. 707. 774. 720. 736. 712. 739. 745. GooF 2.108 1.885 1.789 1.430 1.317 1.171 1.175 0.960 0.878 0.910 K 5.210 1.538 1.153 1.035 1.021 1.008 0.987 0.993 1.003 0.960 Resolution(A) 0.77 0.81 0.85 0.90 0.94 1.00 1.08 1.19 1.36 1.71 inf Number in group 742. 736. 756. 727. 743. 734. 739. 742. 729. 743. GooF 1.011 1.039 1.101 1.161 1.169 1.448 1.487 1.657 1.870 1.971 K 0.987 0.995 1.003 1.021 1.020 1.027 1.032 1.019 1.005 0.931 R1 0.159 0.138 0.128 0.101 0.074 0.069 0.058 0.048 0.045 0.061 Recommended weighting scheme: WGHT 0.0607 11.4040 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) -5 6 4 253.45 38.61 6.85 0.013 1.44 -3 6 6 143.94 3.76 6.67 0.004 1.74 -7 4 1 204.59 13.86 6.59 0.008 1.25 9 1 3 318.10 16.55 6.38 0.008 1.02 7 2 14 211.96 20.89 6.34 0.010 1.04 -6 2 10 236.77 26.89 6.19 0.011 1.44 -4 3 7 137.27 28.28 6.09 0.011 1.96 5 6 12 170.75 0.78 6.09 0.002 1.17 0 1 2 589.24 38870.41 6.06 0.411 9.66 6 2 6 239.45 80.21 5.88 0.019 1.40 5 2 20 306.69 113.14 5.67 0.022 1.04 5 7 2 336.05 108.53 5.67 0.022 1.32 -5 3 2 172.96 54.94 5.66 0.015 1.75 4 4 15 443.14 185.90 5.60 0.028 1.27 -6 4 3 300.98 101.08 5.45 0.021 1.43 7 2 6 154.19 15.70 5.40 0.008 1.22 6 1 0 245.95 93.53 5.34 0.020 1.56 -4 6 8 127.66 1.07 5.28 0.002 1.53 6 2 2 198.50 70.09 5.28 0.017 1.50 5 0 0 124.50 5.88 5.23 0.005 1.89 -2 2 3 222.05 92.51 5.20 0.020 3.72 -5 3 6 226.78 63.05 5.17 0.017 1.71 2 2 8 64.11 11.88 5.13 0.007 2.45 8 1 10 330.76 100.67 5.12 0.021 1.03 8 1 5 172.90 13.13 5.09 0.008 1.12 6 1 11 178.39 32.37 4.91 0.012 1.25 7 2 12 117.66 1.44 4.89 0.002 1.08 -5 1 2 117.92 17.35 4.84 0.009 1.89 3 4 17 132.89 39.00 4.83 0.013 1.28 5 4 9 129.57 13.29 4.78 0.008 1.38 2 6 0 79.84 0.80 4.74 0.002 2.00 -6 4 7 837.77 415.47 4.71 0.042 1.40 4 2 3 120.69 31.46 4.71 0.012 2.10 4 8 3 142.49 0.12 4.70 0.001 1.33 5 4 7 270.44 89.61 4.70 0.020 1.45 5 3 18 235.64 88.92 4.67 0.020 1.09 -6 1 12 97.80 18.43 4.61 0.009 1.40 3 6 14 105.92 0.48 4.60 0.001 1.29 -3 2 2 105.59 35.00 4.59 0.012 2.86 3 4 13 72.04 0.34 4.50 0.001 1.49 9 4 1 280.96 29.39 4.45 0.011 0.99 1 6 4 86.93 13.05 4.44 0.008 2.04 8 6 4 200.25 8.07 4.39 0.006 1.01 4 5 13 279.53 129.09 4.38 0.024 1.30 -8 3 2 350.10 50.34 4.36 0.015 1.15 8 5 7 341.51 109.51 4.35 0.022 1.01 -2 3 13 172.43 65.83 4.32 0.017 1.90 4 2 0 143.40 61.17 4.31 0.016 2.22 4 1 13 429.80 232.23 4.31 0.032 1.48 6 5 3 221.21 67.17 4.27 0.017 1.31 Bond lengths and angles Sb1 - Distance Angles C13 1.9525 (0.0044) O1 2.1374 (0.0033) 88.78 (0.16) O3 2.1511 (0.0033) 93.06 (0.17) 175.84 (0.12) C7 2.1521 (0.0055) 98.86 (0.20) 98.36 (0.16) 77.67 (0.17) C1 2.2831 (0.0051) 138.06 (0.19) 84.94 (0.15) 96.14 (0.15) 123.08 (0.17) Sb1 - C13 O1 O3 C7 O1 - Distance Angles C19 1.5163 (0.0072) Sb1 2.1374 (0.0033) 125.29 (0.27) O1 - C19 O2 - Distance Angles C19 1.1658 (0.0065) O2 - O3 - Distance Angles C32 1.1689 (0.0059) Sb1 2.1511 (0.0033) 110.79 (0.36) O3 - C32 O4 - Distance Angles C32 1.3131 (0.0068) O4 - C1 - Distance Angles C6 1.2236 (0.0063) C2 1.3847 (0.0070) 110.36 (0.50) Sb1 2.2831 (0.0051) 115.91 (0.42) 133.73 (0.34) C1 - C6 C2 C2 - Distance Angles C1 1.3847 (0.0070) C3 1.4785 (0.0076) 129.95 (0.43) C2 - C1 C3 - Distance Angles C4 1.2015 (0.0072) C2 1.4785 (0.0076) 120.19 (0.52) C3 - C4 C4 - Distance Angles C3 1.2015 (0.0072) C5 1.3793 (0.0080) 110.03 (0.53) C4 - C3 C5 - Distance Angles C4 1.3793 (0.0080) C6 1.4840 (0.0080) 130.77 (0.45) C5 - C4 C6 - Distance Angles C1 1.2236 (0.0063) C5 1.4840 (0.0080) 118.68 (0.51) C6 - C1 C7 - Distance Angles C12 1.3403 (0.0069) C8 1.4961 (0.0078) 119.62 (0.50) Sb1 2.1521 (0.0055) 115.84 (0.42) 124.54 (0.34) C7 - C12 C8 C8 - Distance Angles C9 1.3842 (0.0077) C7 1.4961 (0.0078) 124.39 (0.50) C8 - C9 C9 - Distance Angles C10 1.3313 (0.0086) C8 1.3842 (0.0077) 116.69 (0.59) C9 - C10 C10 - Distance Angles C9 1.3313 (0.0086) C11 1.4261 (0.0093) 119.76 (0.56) C10 - C9 C11 - Distance Angles C10 1.4261 (0.0093) C12 1.4536 (0.0082) 125.96 (0.54) C11 - C10 C12 - Distance Angles C7 1.3403 (0.0069) C11 1.4536 (0.0082) 113.56 (0.54) C12 - C7 C13 - Distance Angles C18 1.4421 (0.0073) C14 1.5309 (0.0078) 128.91 (0.42) Sb1 1.9525 (0.0044) 115.69 (0.36) 115.21 (0.34) C13 - C18 C14 C14 - Distance Angles C15 1.3121 (0.0072) C13 1.5309 (0.0078) 117.49 (0.55) C14 - C15 C15 - Distance Angles C14 1.3121 (0.0072) C16 1.4033 (0.0092) 113.27 (0.60) C15 - C14 C16 - Distance Angles C15 1.4033 (0.0092) C17 1.5291 (0.0098) 130.07 (0.49) C16 - C15 C17 - Distance Angles C18 1.3141 (0.0070) C16 1.5291 (0.0098) 117.64 (0.57) C17 - C18 C18 - Distance Angles C17 1.3141 (0.0070) C13 1.4421 (0.0073) 112.47 (0.55) C18 - C17 C19 - Distance Angles O2 1.1658 (0.0065) C20 1.4903 (0.0078) 108.35 (0.59) O1 1.5163 (0.0072) 126.46 (0.46) 125.19 (0.51) C19 - O2 C20 C20 - Distance Angles C21 1.3797 (0.0073) C19 1.4903 (0.0078) 107.20 (0.49) C27 1.5023 (0.0092) 120.31 (0.56) 107.96 (0.57) C20 - C21 C19 C21 - Distance Angles C20 1.3797 (0.0073) C22 1.4405 (0.0085) 111.16 (0.58) C26 1.5588 (0.0086) 118.70 (0.58) 130.02 (0.48) C21 - C20 C22 C22 - Distance Angles C23 1.2292 (0.0083) C21 1.4405 (0.0085) 107.71 (0.64) C22 - C23 C23 - Distance Angles C22 1.2292 (0.0083) C24 1.5287 (0.0120) 123.02 (0.67) C23 - C22 C24 - Distance Angles C25 1.4654 (0.0125) C23 1.5287 (0.0120) 129.84 (0.54) C24 - C25 C25 - Distance Angles C26 1.2367 (0.0088) C24 1.4654 (0.0125) 107.51 (0.70) C25 - C26 C26 - Distance Angles C25 1.2367 (0.0088) C21 1.5588 (0.0086) 121.88 (0.69) C26 - C25 C27 - Distance Angles C28 1.3942 (0.0070) C20 1.5023 (0.0092) 119.85 (0.51) C31 1.5738 (0.0088) 97.35 (0.48) 111.38 (0.60) C27 - C28 C20 C28 - Distance Angles C27 1.3942 (0.0070) C29 1.5168 (0.0073) 109.54 (0.44) C28 - C27 C29 - Distance Angles C28 1.5168 (0.0073) C30 1.5576 (0.0086) 98.63 (0.45) C29 - C28 C30 - Distance Angles C31 1.4860 (0.0076) C29 1.5576 (0.0086) 100.76 (0.48) C30 - C31 C31 - Distance Angles C30 1.4860 (0.0076) C27 1.5738 (0.0088) 111.60 (0.47) C31 - C30 C32 - Distance Angles O3 1.1689 (0.0059) O4 1.3131 (0.0068) 121.60 (0.46) C33 1.6143 (0.0078) 105.90 (0.50) 132.50 (0.46) C32 - O3 O4 C33 - Distance Angles C40 1.4875 (0.0086) C34 1.5797 (0.0076) 127.55 (0.45) C32 1.6143 (0.0078) 103.75 (0.51) 110.96 (0.42) C33 - C40 C34 C34 - Distance Angles C39 1.2552 (0.0070) C35 1.5503 (0.0087) 116.57 (0.53) C33 1.5797 (0.0076) 112.71 (0.55) 130.69 (0.45) C34 - C39 C35 C35 - Distance Angles C36 1.4613 (0.0098) C34 1.5503 (0.0087) 132.43 (0.55) C35 - C36 C36 - Distance Angles C37 1.3015 (0.0097) C35 1.4613 (0.0098) 107.45 (0.65) C36 - C37 C37 - Distance Angles C36 1.3015 (0.0097) C38 1.4878 (0.0106) 119.28 (0.61) C37 - C36 C38 - Distance Angles C39 1.4291 (0.0096) C37 1.4878 (0.0105) 132.89 (0.57) C38 - C39 C39 - Distance Angles C34 1.2552 (0.0070) C38 1.4291 (0.0096) 111.34 (0.63) C39 - C34 C40 - Distance Angles C33 1.4875 (0.0086) C44 1.5665 (0.0085) 123.76 (0.52) C41 1.5791 (0.0091) 105.97 (0.57) 104.99 (0.49) C40 - C33 C44 C41 - Distance Angles C42 1.5773 (0.0101) C40 1.5791 (0.0091) 94.68 (0.56) C41 - C42 C42 - Distance Angles C43 1.5382 (0.0120) C41 1.5773 (0.0101) 116.09 (0.61) C42 - C43 C43 - Distance Angles C44 1.4601 (0.0099) C42 1.5382 (0.0120) 100.38 (0.67) C43 - C44 C44 - Distance Angles C43 1.4601 (0.0099) C40 1.5665 (0.0085) 108.28 (0.56) C44 - C43 FMAP and GRID set by program FMAP 2 1 24 GRID -2.381 -2 -1 2.381 2 1 R1 = 0.0768 for 7391 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.43 at 0.1743 0.7990 0.2097 [ 1.10 A from C40 ] Deepest hole -1.48 at 0.1035 0.1599 0.1079 [ 0.69 A from SB1 ] Mean = 0.00, Rms deviation from mean = 0.17 e/A^3, Highest memory used = 5428 / 55653 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.1743 -0.2010 0.2097 1.00000 0.05 1.43 1.10 C40 1.13 H33 1.27 C33 1.67 C41 Q2 1 0.1974 0.3611 0.0151 1.00000 0.05 1.14 0.99 C20 1.15 C27 1.20 H27 1.67 C19 Q3 1 0.5320 -0.1008 0.1298 1.00000 0.05 0.95 1.65 H2 2.03 H9 2.08 H25 2.37 H44B Q4 1 0.3337 0.4520 0.0019 1.00000 0.05 0.83 1.10 C27 1.39 C31 1.42 H31A 1.46 H20 Q5 1 0.3422 0.2020 -0.1332 1.00000 0.05 0.66 0.54 H25 1.26 C25 1.97 C26 2.03 H26 Q6 1 0.4330 0.2379 -0.0867 1.00000 0.05 0.66 0.81 H26 1.40 C26 1.84 C25 1.89 H25 Q7 1 0.2892 -0.1019 0.2239 1.00000 0.05 0.64 0.92 C33 1.24 C40 1.29 H40 1.54 C32 Q8 1 0.4050 -0.3470 0.1781 1.00000 0.05 0.63 0.33 C43 0.65 H43A 1.10 H43B 1.64 C42 Q9 1 0.5073 -0.3223 0.1510 1.00000 0.05 0.58 0.85 H43A 1.63 C43 1.98 H43B 2.17 H44B Q10 1 0.4427 -0.2558 0.1611 1.00000 0.05 0.56 1.15 H44B 1.18 H43A 1.44 C44 1.46 C43 Shortest distances between peaks (including symmetry equivalents) 9 10 1.14 8 10 1.37 8 9 1.37 5 6 1.55 1 7 1.72 3 5 1.79 2 4 1.85 3 6 2.25 5 9 2.26 6 9 2.30 5 10 2.42 3 10 2.44 6 10 2.60 Time profile in seconds ----------------------- 0.22: Read and process instructions 0.00: Fit rigid groups 0.02: Interpret restraints etc. 0.00: Generate connectivity array 0.02: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 8.47: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 15.81: Structure factors and derivatives 10.27: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 1.20: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.17: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.19: Fourier summations 0.09: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 16:16:12 Total CPU time: 36.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++