+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 14:13:06 on 20-Oct-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src0895r in P-1 CELL 0.71073 12.1832 12.3253 16.5184 96.114 106.867 114.864 ZERR 2.00 0.0000 0.0000 0.0000 0.000 0.000 0.000 LATT 1 SFAC C H O S N MN UNIT 68 72 38 4 6 6 V = 2077.78 F(000) = 1040.0 Mu = 1.08 mm-1 Cell Wt = 2039.20 Rho = 1.630 MERG 2 OMIT -3.00 55.00 OMIT 0 -3 2 OMIT 0 -3 3 OMIT -1 1 5 OMIT 0 0 3 OMIT -2 0 1 OMIT -1 -2 3 OMIT -2 -2 4 OMIT 0 -1 3 DFIX 0.85 0.02 O19 H19b O19 H19A DFIX 0.85 0.02 O15 H15a O15 H15b DFIX 0.85 0.02 O16 H16b O16 H16a DFIX 0.85 0.02 O18 H18b O18 H18a DFIX 0.85 0.02 O20 H20a O20 H20b DFIX 0.85 0.01 O17 H17B O17 H17c DFIX 0.85 0.02 O14 H14b O14 H14a DANG 1.390 0.04 H19A H19b DANG 1.390 0.04 H15b H15a DANG 1.390 0.04 H16a H16b DANG 1.390 0.04 H18a H18b DANG 1.390 0.04 H20b H20a DANG 1.390 0.01 H17c H17B DANG 1.390 0.04 H14a H14b FMAP 2 PLAN 10 SIZE 0.06 0.14 0.20 ACTA WGHT 0.06080 2.84700 L.S. 10 TEMP -153.00 FVAR 0.50490 C1 1 0.416898 0.916937 0.310590 11.00000 0.03238 0.01733 = 0.01905 0.00750 0.01114 0.01353 C2 1 0.478670 1.046509 0.322325 11.00000 0.03524 0.01857 = 0.02165 0.00552 0.00817 0.01144 AFIX 43 H2 2 0.571109 1.091573 0.344181 11.00000 -1.20000 AFIX 0 C3 1 0.407340 1.109021 0.302654 11.00000 0.05035 0.01705 = 0.02350 0.00463 0.01094 0.01710 AFIX 43 H3 2 0.451040 1.196292 0.311281 11.00000 -1.20000 AFIX 0 C4 1 0.271933 1.044996 0.270294 11.00000 0.05340 0.02850 = 0.02879 0.01073 0.01418 0.02996 AFIX 43 H4 2 0.222915 1.087940 0.256167 11.00000 -1.20000 AFIX 0 C5 1 0.209087 0.917579 0.258839 11.00000 0.03646 0.02857 = 0.02677 0.00811 0.01007 0.02223 AFIX 43 H5 2 0.116597 0.874014 0.237320 11.00000 -1.20000 AFIX 0 C6 1 0.279022 0.851957 0.278303 11.00000 0.02833 0.01875 = 0.02022 0.00646 0.00918 0.01434 C7 1 0.204862 0.719136 0.264224 11.00000 0.01927 0.02087 = 0.02298 0.00676 0.00845 0.01055 AFIX 43 H7 2 0.112638 0.681929 0.237912 11.00000 -1.20000 AFIX 0 C8 1 -0.001873 0.200896 0.314950 11.00000 0.01569 0.01605 = 0.02315 0.00181 0.00912 0.00423 C9 1 -0.139236 0.135965 0.284386 11.00000 0.01674 0.02259 = 0.03079 0.00254 0.00790 0.00549 AFIX 43 H9 2 -0.189394 0.163630 0.245133 11.00000 -1.20000 AFIX 0 C10 1 -0.200755 0.032236 0.311519 11.00000 0.01758 0.02500 = 0.03655 0.00240 0.01216 -0.00051 AFIX 43 H10 2 -0.293215 -0.010115 0.290966 11.00000 -1.20000 AFIX 0 C11 1 -0.130794 -0.011472 0.367986 11.00000 0.02599 0.02293 = 0.04642 0.01461 0.01489 -0.00169 AFIX 43 H11 2 -0.174850 -0.082525 0.386331 11.00000 -1.20000 AFIX 0 C12 1 0.002884 0.048865 0.397219 11.00000 0.02294 0.02495 = 0.03640 0.01267 0.00761 0.00356 AFIX 43 H12 2 0.051132 0.018113 0.434938 11.00000 -1.20000 AFIX 0 C13 1 0.069285 0.155980 0.371841 11.00000 0.01596 0.01434 = 0.02250 0.00272 0.00746 0.00158 C14 1 0.209797 0.220910 0.411658 11.00000 0.01899 0.01551 = 0.01855 0.00326 0.00595 0.00699 AFIX 43 H14 2 0.251654 0.184845 0.448875 11.00000 -1.20000 AFIX 0 C15 1 0.749296 0.467751 0.420658 11.00000 0.01442 0.02319 = 0.01922 -0.00053 0.00437 0.00903 C16 1 0.803672 0.387742 0.430196 11.00000 0.02383 0.02277 = 0.03155 0.00210 0.00888 0.01338 AFIX 43 H16 2 0.770928 0.321813 0.456073 11.00000 -1.20000 AFIX 0 C17 1 0.905128 0.404025 0.402113 11.00000 0.02549 0.03600 = 0.03800 -0.00277 0.00905 0.01935 AFIX 43 H17 2 0.941932 0.349732 0.409864 11.00000 -1.20000 AFIX 0 C18 1 0.953364 0.497871 0.363105 11.00000 0.02819 0.04950 = 0.04084 0.00739 0.02101 0.02261 AFIX 43 H18 2 1.021505 0.506860 0.342986 11.00000 -1.20000 AFIX 0 C19 1 0.902273 0.578182 0.353546 11.00000 0.02748 0.04821 = 0.03827 0.01557 0.02031 0.02183 AFIX 43 H19 2 0.936757 0.643691 0.327723 11.00000 -1.20000 AFIX 0 C20 1 0.799121 0.564865 0.381552 11.00000 0.01804 0.03176 = 0.02827 0.00696 0.01127 0.01401 C21 1 0.754102 0.655490 0.372169 11.00000 0.01922 0.02673 = 0.03184 0.01323 0.01478 0.00907 AFIX 43 H21 2 0.802775 0.726436 0.355477 11.00000 -1.20000 AFIX 0 C22 1 0.355623 0.334837 0.212563 11.00000 0.02006 0.01582 = 0.01678 0.00360 0.00744 0.00848 C23 1 0.360457 0.273968 0.133524 11.00000 0.01831 0.02283 = 0.02012 0.00281 0.00633 0.01008 C24 1 0.265638 0.204982 0.052564 11.00000 0.01961 0.02514 = 0.01991 0.00160 0.00667 0.00869 C25 1 0.069969 0.136127 -0.064849 11.00000 0.02713 0.06318 = 0.02414 -0.00591 0.00095 0.01747 AFIX 23 H25A 2 0.096341 0.206696 -0.091398 11.00000 -1.20000 H25B 2 -0.024906 0.100083 -0.078455 11.00000 -1.20000 AFIX 0 C26 1 0.097878 0.041417 -0.103536 11.00000 0.02961 0.05184 = 0.03261 -0.01133 0.00323 0.01392 AFIX 23 H26A 2 0.070937 -0.029162 -0.077054 11.00000 -1.20000 H26B 2 0.045601 0.010039 -0.167252 11.00000 -1.20000 AFIX 0 C27 1 0.312951 0.160134 -0.004783 11.00000 0.02600 0.02449 = 0.01705 -0.00033 0.00657 0.00945 C28 1 0.443628 0.194925 0.031299 11.00000 0.02542 0.02855 = 0.01686 -0.00005 0.00831 0.01142 C29 1 0.523846 0.166234 -0.008432 11.00000 0.02374 0.02831 = 0.02734 0.00213 0.01148 0.01252 C30 1 0.657391 0.212518 0.027986 11.00000 0.02865 0.03533 = 0.02314 0.00285 0.00867 0.01472 C31 1 0.871702 0.347747 0.123661 11.00000 0.02357 0.04562 = 0.03560 0.00207 0.00606 0.01136 AFIX 23 H31A 2 0.922891 0.388138 0.186976 11.00000 -1.20000 H31B 2 0.897047 0.411391 0.091204 11.00000 -1.20000 AFIX 0 C32 1 0.902323 0.247323 0.095073 11.00000 0.03076 0.05073 = 0.03263 0.00544 0.00757 0.01822 AFIX 23 H32A 2 0.997573 0.282493 0.110797 11.00000 -1.20000 H32B 2 0.874457 0.182342 0.126142 11.00000 -1.20000 AFIX 0 C33 1 0.706521 0.159427 -0.023770 11.00000 0.02717 0.04021 = 0.02749 0.00900 0.01242 0.01680 C34 1 0.611667 0.074989 -0.098526 11.00000 0.03679 0.04140 = 0.02528 0.00463 0.01469 0.02081 AFIX 43 H34 2 0.626486 0.030616 -0.141163 11.00000 -1.20000 AFIX 0 O1 3 0.492217 0.863116 0.329721 11.00000 0.02040 0.01653 = 0.03284 0.01099 0.00983 0.00808 O2 3 0.168325 0.524117 0.265120 11.00000 0.01237 0.01328 = 0.02864 0.00614 0.00606 0.00384 O3 3 0.054530 0.302866 0.290094 11.00000 0.01289 0.01767 = 0.03247 0.00924 0.00641 0.00572 O4 3 0.413048 0.375114 0.451446 11.00000 0.01039 0.01415 = 0.01828 0.00334 0.00375 0.00467 O5 3 0.655325 0.451954 0.452084 11.00000 0.01561 0.02136 = 0.02157 0.00606 0.00880 0.01102 O6 3 0.627446 0.745010 0.382711 11.00000 0.01716 0.01501 = 0.03043 0.01028 0.01128 0.00712 O7 3 0.397861 0.547317 0.367395 11.00000 0.01162 0.01110 = 0.02030 0.00425 0.00625 0.00437 O8 3 0.249822 0.336027 0.207644 11.00000 0.01861 0.02356 = 0.01976 0.00014 0.00659 0.00958 O9 3 0.457689 0.379767 0.280398 11.00000 0.01988 0.01881 = 0.01747 0.00105 0.00564 0.01034 O10 3 0.138407 0.180309 0.028971 11.00000 0.01949 0.04036 = 0.02070 -0.00263 0.00405 0.01211 O11 3 0.235130 0.089501 -0.090012 11.00000 0.02584 0.03816 = 0.01884 -0.00703 0.00367 0.01134 O12 3 0.836364 0.192670 0.001166 11.00000 0.02917 0.05426 = 0.03319 0.00738 0.01335 0.02037 O13 3 0.733750 0.297448 0.107585 11.00000 0.02485 0.04511 = 0.03267 -0.00577 0.00627 0.01210 O14 3 0.331071 0.001779 0.486943 11.00000 0.05885 0.09071 = 0.03527 0.00149 0.01274 -0.00617 O15 3 0.212441 0.467851 0.062737 11.00000 0.05635 0.04937 = 0.04682 0.02031 0.01439 0.00842 O16 3 0.673174 0.712544 0.182006 11.00000 0.06203 0.05950 = 0.05139 0.02059 0.03204 0.02201 O17 3 0.636161 0.523275 0.044029 10.50000 0.12127 0.01756 = 0.04317 0.00830 0.06320 0.01303 O18 3 0.439569 0.633631 0.208257 11.00000 0.02808 0.04483 = 0.02735 0.00297 0.01387 0.01119 O19 3 0.967748 0.407493 -0.053192 10.50000 0.05173 0.06032 = 0.06703 0.03001 0.02090 0.00794 O20 3 0.436808 0.769847 0.473331 11.00000 0.02794 0.01993 = 0.02325 0.00508 0.00981 0.01052 S1 4 0.508862 0.282967 0.138869 11.00000 0.02036 0.02713 = 0.01846 -0.00004 0.00669 0.01117 S2 4 0.461181 0.057935 -0.106822 11.00000 0.02902 0.03993 = 0.02352 -0.00217 0.00749 0.01550 N1 5 0.255544 0.648322 0.284962 11.00000 0.01686 0.01373 = 0.02134 0.00515 0.00867 0.00647 N2 5 0.281519 0.324644 0.399675 11.00000 0.01081 0.01491 = 0.01622 0.00113 0.00452 0.00362 N3 5 0.651125 0.645480 0.385230 11.00000 0.01472 0.01774 = 0.02037 0.00641 0.00760 0.00843 MN1 6 0.526081 0.497898 0.407957 11.00000 0.01063 0.01291 = 0.01654 0.00399 0.00591 0.00530 MN2 6 0.228327 0.418039 0.317567 11.00000 0.01038 0.01221 = 0.01961 0.00432 0.00630 0.00469 MN3 6 0.446240 0.701033 0.340191 11.00000 0.01342 0.01214 = 0.02106 0.00592 0.00702 0.00536 H14A 2 0.355834 0.030328 0.541961 11.00000 -1.50000 H14B 2 0.332418 -0.070950 0.489337 11.00000 -1.50000 H15A 2 0.199144 0.415333 0.095833 11.00000 -1.50000 H15B 2 0.271783 0.465799 0.045615 11.00000 -1.50000 H16A 2 0.628973 0.652736 0.128989 11.00000 -1.50000 H16B 2 0.696669 0.783596 0.164620 11.00000 -1.50000 H17B 2 0.714451 0.548304 0.077450 10.50000 -1.50000 H17C 2 0.607472 0.571214 0.052096 10.50000 -1.50000 H18A 2 0.372965 0.588609 0.164571 11.00000 -1.50000 H18B 2 0.509317 0.657517 0.199362 11.00000 -1.50000 H19A 2 0.906791 0.337060 -0.054455 10.50000 -1.50000 H19B 2 1.035878 0.396883 -0.042022 10.50000 -1.50000 H20A 2 0.421665 0.716323 0.502129 11.00000 -1.50000 H20B 2 0.509538 0.831505 0.498689 11.00000 -1.50000 HKLF 4 Covalent radii and connectivity table for 2008src0895r in P-1 C 0.770 H 0.320 O 0.660 S 1.030 N 0.700 MN 1.370 C1 - O1 C2 C6 C2 - C3 C1 C3 - C2 C4 C4 - C5 C3 C5 - C4 C6 C6 - C5 C1 C7 C7 - N1 C6 C8 - O3 C13 C9 C9 - C10 C8 C10 - C9 C11 C11 - C12 C10 C12 - C11 C13 C13 - C8 C12 C14 C14 - N2 C13 C15 - O5 C16 C20 C16 - C17 C15 C17 - C18 C16 C18 - C19 C17 C19 - C18 C20 C20 - C15 C19 C21 C21 - N3 C20 C22 - O9 O8 C23 C23 - C24 C22 S1 C24 - O10 C23 C27 C25 - O10 C26 C26 - O11 C25 C27 - C28 O11 C24 C28 - C27 C29 S1 C29 - C30 C28 S2 C30 - O13 C29 C33 C31 - O13 C32 C32 - O12 C31 C33 - C34 O12 C30 C34 - C33 S2 O1 - C1 Mn3 O2 - N1 Mn2 O3 - C8 Mn2 O4 - N2 Mn1 Mn1_$1 O5 - C15 Mn1 O6 - N3 Mn3 O7 - Mn2 Mn3 Mn1 O8 - C22 Mn2 O9 - C22 Mn1 O10 - C24 C25 O11 - C27 C26 O12 - C33 C32 O13 - C30 C31 O14 - no bonds found O15 - no bonds found O16 - no bonds found O17 - no bonds found O18 - Mn3 O19 - no bonds found O20 - Mn3 S1 - C28 C23 S2 - C34 C29 N1 - C7 O2 Mn3 N2 - C14 O4 Mn2 N3 - C21 O6 Mn1 Mn1 - O5 O7 O4 N3 O9 O4_$1 Mn2 Mn3 Mn2 - O7 O3 O2 N2 O8 Mn1 Mn3 - O1 O7 O6 N1 O18 O20 Mn1 Operators for generating equivalent atoms: $1 -x+1, -y+1, -z+1 48582 Reflections read, of which 51 rejected -15 =< h =< 15, -15 =< k =< 16, -21 =< l =< 21, Max. 2-theta = 55.00 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 9 0 8 7.96 5.52 2 28.34 1 Inconsistent equivalents 9473 Unique reflections, of which 0 suppressed R(int) = 0.0498 R(sigma) = 0.0395 Friedel opposites merged Maximum memory for data reduction = 4763 / 96465 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 = 6312 / 821364 wR2 = 0.1201 before cycle 1 for 9473 data and 601 / 601 parameters Disagreeable restraints before cycle 1 Observed Target Error Sigma Restraint 0.9248 0.8500 0.0748 0.0200 DFIX O16 H16A Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 14. 7. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.019 0.037 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.034 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.054; Restrained GooF = 1.056 for 21 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0608 * P )^2 + 2.85 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.50492 0.00069 0.023 OSF Mean shift/esd = 0.008 Maximum = 0.373 for x H17B Max. shift = 0.032 A for H17B Max. dU = 0.000 for O17 Least-squares cycle 2 Maximum vector length = 511 Memory required = 6312 / 821364 wR2 = 0.1201 before cycle 2 for 9473 data and 601 / 601 parameters Disagreeable restraints before cycle 2 Observed Target Error Sigma Restraint 0.9247 0.8500 0.0747 0.0200 DFIX O16 H16A Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 14. 7. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.019 0.037 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.034 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.054; Restrained GooF = 1.055 for 21 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0608 * P )^2 + 2.85 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.50492 0.00069 0.006 OSF Mean shift/esd = 0.009 Maximum = -0.590 for x H17B Max. shift = 0.048 A for H17B Max. dU = 0.000 for O17 Least-squares cycle 3 Maximum vector length = 511 Memory required = 6312 / 821364 wR2 = 0.1201 before cycle 3 for 9473 data and 601 / 601 parameters Disagreeable restraints before cycle 3 Observed Target Error Sigma Restraint 0.9246 0.8500 0.0746 0.0200 DFIX O16 H16A Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 14. 7. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.019 0.037 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.034 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.054; Restrained GooF = 1.056 for 21 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0608 * P )^2 + 2.85 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.50493 0.00069 0.016 OSF Mean shift/esd = 0.010 Maximum = 0.650 for x H17B Max. shift = 0.054 A for H17B Max. dU = 0.000 for O17 Least-squares cycle 4 Maximum vector length = 511 Memory required = 6312 / 821364 wR2 = 0.1201 before cycle 4 for 9473 data and 601 / 601 parameters Disagreeable restraints before cycle 4 Observed Target Error Sigma Restraint 0.9246 0.8500 0.0746 0.0200 DFIX O16 H16A Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 14. 7. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.019 0.037 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.034 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.054; Restrained GooF = 1.055 for 21 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0608 * P )^2 + 2.85 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.50492 0.00069 -0.011 OSF Mean shift/esd = 0.009 Maximum = -0.664 for x H17B Max. shift = 0.053 A for H17B Max. dU = 0.000 for O17 Least-squares cycle 5 Maximum vector length = 511 Memory required = 6312 / 821364 wR2 = 0.1201 before cycle 5 for 9473 data and 601 / 601 parameters Disagreeable restraints before cycle 5 Observed Target Error Sigma Restraint 0.9246 0.8500 0.0746 0.0200 DFIX O16 H16A Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 14. 7. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.019 0.037 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.034 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.054; Restrained GooF = 1.055 for 21 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0608 * P )^2 + 2.85 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.50493 0.00069 0.008 OSF Mean shift/esd = 0.008 Maximum = 0.513 for x H17B Max. shift = 0.046 A for H17B Max. dU = 0.000 for O17 Least-squares cycle 6 Maximum vector length = 511 Memory required = 6312 / 821364 wR2 = 0.1201 before cycle 6 for 9473 data and 601 / 601 parameters Disagreeable restraints before cycle 6 Observed Target Error Sigma Restraint 0.9246 0.8500 0.0746 0.0200 DFIX O16 H16A Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 14. 7. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.019 0.037 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.034 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.054; Restrained GooF = 1.055 for 21 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0608 * P )^2 + 2.85 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.50492 0.00069 -0.007 OSF Mean shift/esd = 0.007 Maximum = -0.519 for x H17B Max. shift = 0.039 A for H17B Max. dU = 0.000 for O17 Least-squares cycle 7 Maximum vector length = 511 Memory required = 6312 / 821364 wR2 = 0.1201 before cycle 7 for 9473 data and 601 / 601 parameters Disagreeable restraints before cycle 7 Observed Target Error Sigma Restraint 0.9246 0.8500 0.0746 0.0200 DFIX O16 H16A Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 14. 7. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.019 0.037 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.034 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.054; Restrained GooF = 1.055 for 21 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0608 * P )^2 + 2.85 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.50493 0.00069 0.007 OSF Mean shift/esd = 0.006 Maximum = 0.375 for x H17B Max. shift = 0.033 A for H17B Max. dU = 0.000 for O17 Least-squares cycle 8 Maximum vector length = 511 Memory required = 6312 / 821364 wR2 = 0.1201 before cycle 8 for 9473 data and 601 / 601 parameters Disagreeable restraints before cycle 8 Observed Target Error Sigma Restraint 0.9246 0.8500 0.0746 0.0200 DFIX O16 H16A Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 14. 7. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.019 0.037 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.034 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.054; Restrained GooF = 1.055 for 21 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0608 * P )^2 + 2.85 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.50492 0.00069 -0.007 OSF Mean shift/esd = 0.005 Maximum = -0.376 for x H17B Max. shift = 0.029 A for H17B Max. dU = 0.000 for O17 Least-squares cycle 9 Maximum vector length = 511 Memory required = 6312 / 821364 wR2 = 0.1201 before cycle 9 for 9473 data and 601 / 601 parameters Disagreeable restraints before cycle 9 Observed Target Error Sigma Restraint 0.9246 0.8500 0.0746 0.0200 DFIX O16 H16A Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 14. 7. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.019 0.037 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.034 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.054; Restrained GooF = 1.055 for 21 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0608 * P )^2 + 2.85 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.50493 0.00069 0.005 OSF Mean shift/esd = 0.004 Maximum = 0.279 for x H17B Max. shift = 0.025 A for H17B Max. dU = 0.000 for O17 Least-squares cycle 10 Maximum vector length = 511 Memory required = 6312 / 821364 wR2 = 0.1201 before cycle 10 for 9473 data and 601 / 601 parameters Disagreeable restraints before cycle 10 Observed Target Error Sigma Restraint 0.9246 0.8500 0.0746 0.0200 DFIX O16 H16A Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 14. 7. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.019 0.037 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.034 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.054; Restrained GooF = 1.055 for 21 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0608 * P )^2 + 2.85 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.50493 0.00069 -0.003 OSF Mean shift/esd = 0.004 Maximum = -0.272 for x H17B Max. shift = 0.021 A for H17B Max. dU = 0.000 for O17 Largest correlation matrix elements 0.937 y H17C / x H17C 0.678 z H20A / y H20A 0.622 z H18B / x H18B 0.859 y H19B / x H19B 0.668 U12 C4 / U22 C4 0.620 U12 C17 / U11 C17 0.743 y H14B / x H14B 0.662 U13 O17 / U11 O17 0.617 y H15B / x H15B 0.729 y H17B / x H17B 0.645 U12 C5 / U11 C5 0.617 U12 C17 / U22 C17 0.725 U13 O17 / U33 O17 0.639 z O17 / x O17 0.612 U12 C19 / U11 C19 0.724 z H15B / x H15B 0.635 U12 C5 / U22 C5 0.611 U12 C18 / U11 C18 0.696 z H15A / y H15A 0.634 U12 O17 / U23 O17 0.609 U13 C4 / U23 C4 0.684 U12 C4 / U11 C4 -0.631 x H17C / y H17B 0.608 U12 C19 / U22 C19 Idealized hydrogen atom generation before cycle 11 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.5711 1.0916 0.3442 43 0.950 0.000 C2 C3 C1 H3 0.4510 1.1963 0.3113 43 0.950 0.000 C3 C2 C4 H4 0.2229 1.0879 0.2562 43 0.950 0.000 C4 C5 C3 H5 0.1166 0.8740 0.2373 43 0.950 0.000 C5 C4 C6 H7 0.1126 0.6819 0.2379 43 0.950 0.000 C7 N1 C6 H9 -0.1894 0.1636 0.2451 43 0.950 0.000 C9 C10 C8 H10 -0.2932 -0.0101 0.2910 43 0.950 0.000 C10 C9 C11 H11 -0.1748 -0.0825 0.3863 43 0.950 0.000 C11 C12 C10 H12 0.0511 0.0181 0.4349 43 0.950 0.000 C12 C11 C13 H14 0.2517 0.1848 0.4489 43 0.950 0.000 C14 N2 C13 H16 0.7709 0.3218 0.4561 43 0.950 0.000 C16 C17 C15 H17 0.9419 0.3497 0.4099 43 0.950 0.000 C17 C18 C16 H18 1.0215 0.5069 0.3430 43 0.950 0.000 C18 C19 C17 H19 0.9368 0.6437 0.3277 43 0.950 0.000 C19 C18 C20 H21 0.8028 0.7264 0.3555 43 0.950 0.000 C21 N3 C20 H25A 0.0963 0.2067 -0.0914 23 0.990 0.000 C25 O10 C26 H25B -0.0249 0.1001 -0.0785 23 0.990 0.000 C25 O10 C26 H26A 0.0709 -0.0292 -0.0771 23 0.990 0.000 C26 O11 C25 H26B 0.0456 0.0100 -0.1673 23 0.990 0.000 C26 O11 C25 H31A 0.9229 0.3881 0.1870 23 0.990 0.000 C31 O13 C32 H31B 0.8970 0.4114 0.0912 23 0.990 0.000 C31 O13 C32 H32A 0.9976 0.2825 0.1108 23 0.990 0.000 C32 O12 C31 H32B 0.8745 0.1823 0.1261 23 0.990 0.000 C32 O12 C31 H34 0.6265 0.0306 -0.1412 43 0.950 0.000 C34 C33 S2 2008src0895r in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.41690 0.91694 0.31059 1.00000 0.03238 0.01734 0.01906 0.00751 0.01114 0.01353 0.02163 0.00745 0.00029 0.00025 0.00018 0.00000 0.00155 0.00129 0.00129 0.00104 0.00114 0.00120 0.00057 C2 0.47867 1.04651 0.32232 1.00000 0.03525 0.01857 0.02165 0.00552 0.00817 0.01144 0.02624 0.00784 0.00032 0.00026 0.00019 0.00000 0.00167 0.00136 0.00140 0.00110 0.00121 0.00127 0.00062 H2 0.57111 1.09157 0.34418 1.00000 0.03148 0.00000 0.00000 C3 0.40734 1.10902 0.30265 1.00000 0.05036 0.01706 0.02351 0.00463 0.01094 0.01710 0.03064 0.00824 0.00035 0.00027 0.00019 0.00000 0.00204 0.00136 0.00147 0.00113 0.00138 0.00141 0.00070 H3 0.45104 1.19629 0.31128 1.00000 0.03676 0.00000 0.00000 C4 0.27193 1.04500 0.27029 1.00000 0.05340 0.02850 0.02879 0.01073 0.01418 0.02996 0.03288 0.00900 0.00036 0.00030 0.00021 0.00000 0.00213 0.00161 0.00158 0.00129 0.00147 0.00162 0.00073 H4 0.22292 1.08794 0.25617 1.00000 0.03946 0.00000 0.00000 C5 0.20909 0.91758 0.25884 1.00000 0.03647 0.02857 0.02679 0.00811 0.01007 0.02224 0.02836 0.00839 0.00033 0.00029 0.00020 0.00000 0.00172 0.00156 0.00151 0.00123 0.00129 0.00142 0.00065 H5 0.11660 0.87401 0.23732 1.00000 0.03404 0.00000 0.00000 C6 0.27902 0.85196 0.27830 1.00000 0.02833 0.01877 0.02023 0.00646 0.00919 0.01435 0.02108 0.00731 0.00028 0.00025 0.00018 0.00000 0.00149 0.00131 0.00131 0.00105 0.00112 0.00119 0.00056 C7 0.20486 0.71913 0.26422 1.00000 0.01927 0.02088 0.02298 0.00676 0.00845 0.01055 0.02042 0.00724 0.00027 0.00026 0.00018 0.00000 0.00133 0.00133 0.00135 0.00107 0.00108 0.00113 0.00055 H7 0.11264 0.68193 0.23791 1.00000 0.02450 0.00000 0.00000 C8 -0.00187 0.20090 0.31495 1.00000 0.01571 0.01605 0.02316 0.00181 0.00913 0.00423 0.01938 0.00685 0.00026 0.00025 0.00018 0.00000 0.00128 0.00124 0.00134 0.00102 0.00105 0.00105 0.00054 C9 -0.13924 0.13597 0.28439 1.00000 0.01675 0.02259 0.03080 0.00254 0.00791 0.00549 0.02547 0.00738 0.00028 0.00027 0.00020 0.00000 0.00136 0.00141 0.00153 0.00117 0.00115 0.00116 0.00061 H9 -0.18939 0.16363 0.24513 1.00000 0.03056 0.00000 0.00000 C10 -0.20075 0.03224 0.31152 1.00000 0.01760 0.02499 0.03656 0.00241 0.01218 -0.00050 0.03039 0.00788 0.00030 0.00029 0.00021 0.00000 0.00141 0.00151 0.00170 0.00128 0.00125 0.00122 0.00068 H10 -0.29321 -0.01011 0.29097 1.00000 0.03647 0.00000 0.00000 C11 -0.13079 -0.01147 0.36799 1.00000 0.02600 0.02292 0.04644 0.01462 0.01490 -0.00169 0.03600 0.00852 0.00032 0.00030 0.00024 0.00000 0.00165 0.00153 0.00197 0.00140 0.00145 0.00131 0.00077 H11 -0.17485 -0.08252 0.38633 1.00000 0.04320 0.00000 0.00000 C12 0.00288 0.04886 0.39722 1.00000 0.02295 0.02496 0.03640 0.01268 0.00761 0.00357 0.03151 0.00807 0.00031 0.00029 0.00022 0.00000 0.00154 0.00153 0.00173 0.00131 0.00129 0.00127 0.00070 H12 0.05113 0.01811 0.43494 1.00000 0.03781 0.00000 0.00000 C13 0.06929 0.15598 0.37184 1.00000 0.01596 0.01434 0.02252 0.00273 0.00746 0.00158 0.01985 0.00675 0.00026 0.00024 0.00018 0.00000 0.00129 0.00122 0.00133 0.00102 0.00105 0.00105 0.00054 C14 0.20980 0.22091 0.41166 1.00000 0.01900 0.01552 0.01855 0.00326 0.00596 0.00700 0.01850 0.00672 0.00026 0.00024 0.00017 0.00000 0.00132 0.00122 0.00126 0.00099 0.00103 0.00108 0.00053 H14 0.25166 0.18485 0.44887 1.00000 0.02220 0.00000 0.00000 C15 0.74930 0.46775 0.42066 1.00000 0.01443 0.02320 0.01922 -0.00053 0.00438 0.00904 0.01991 0.00680 0.00026 0.00026 0.00017 0.00000 0.00125 0.00136 0.00128 0.00105 0.00101 0.00110 0.00055 C16 0.80367 0.38774 0.43020 1.00000 0.02384 0.02278 0.03157 0.00211 0.00890 0.01339 0.02597 0.00758 0.00029 0.00028 0.00020 0.00000 0.00147 0.00142 0.00156 0.00118 0.00121 0.00123 0.00061 H16 0.77093 0.32181 0.45607 1.00000 0.03116 0.00000 0.00000 C17 0.90513 0.40403 0.40212 1.00000 0.02550 0.03602 0.03800 -0.00277 0.00905 0.01935 0.03314 0.00826 0.00031 0.00031 0.00022 0.00000 0.00159 0.00176 0.00178 0.00140 0.00135 0.00144 0.00073 H17 0.94194 0.34974 0.40987 1.00000 0.03977 0.00000 0.00000 C18 0.95337 0.49787 0.36311 1.00000 0.02821 0.04952 0.04086 0.00740 0.02102 0.02262 0.03629 0.00931 0.00033 0.00035 0.00023 0.00000 0.00166 0.00206 0.00186 0.00157 0.00146 0.00159 0.00077 H18 1.02150 0.50686 0.34299 1.00000 0.04355 0.00000 0.00000 C19 0.90227 0.57818 0.35355 1.00000 0.02748 0.04823 0.03826 0.01557 0.02031 0.02184 0.03413 0.00916 0.00032 0.00034 0.00022 0.00000 0.00166 0.00204 0.00178 0.00154 0.00142 0.00157 0.00074 H19 0.93676 0.64369 0.32772 1.00000 0.04096 0.00000 0.00000 C20 0.79912 0.56486 0.38155 1.00000 0.01805 0.03177 0.02828 0.00696 0.01127 0.01401 0.02462 0.00769 0.00028 0.00029 0.00019 0.00000 0.00136 0.00156 0.00148 0.00122 0.00116 0.00124 0.00060 C21 0.75410 0.65549 0.37217 1.00000 0.01922 0.02673 0.03185 0.01324 0.01478 0.00907 0.02483 0.00776 0.00028 0.00028 0.00020 0.00000 0.00138 0.00148 0.00155 0.00123 0.00119 0.00121 0.00060 H21 0.80278 0.72644 0.35548 1.00000 0.02979 0.00000 0.00000 C22 0.35562 0.33484 0.21256 1.00000 0.02006 0.01582 0.01678 0.00360 0.00744 0.00848 0.01748 0.00672 0.00026 0.00024 0.00017 0.00000 0.00132 0.00122 0.00123 0.00098 0.00103 0.00108 0.00052 C23 0.36045 0.27397 0.13352 1.00000 0.01832 0.02284 0.02013 0.00281 0.00633 0.01008 0.02076 0.00709 0.00027 0.00026 0.00018 0.00000 0.00132 0.00136 0.00132 0.00107 0.00106 0.00114 0.00055 C24 0.26564 0.20498 0.05256 1.00000 0.01962 0.02516 0.01991 0.00159 0.00667 0.00869 0.02284 0.00726 0.00028 0.00027 0.00018 0.00000 0.00137 0.00141 0.00133 0.00109 0.00108 0.00117 0.00058 C25 0.06997 0.13613 -0.06485 1.00000 0.02714 0.06316 0.02415 -0.00591 0.00095 0.01746 0.04331 0.00897 0.00034 0.00039 0.00022 0.00000 0.00173 0.00250 0.00164 0.00157 0.00133 0.00174 0.00092 H25A 0.09634 0.20669 -0.09140 1.00000 0.05197 0.00000 0.00000 H25B -0.02491 0.10008 -0.07846 1.00000 0.05197 0.00000 0.00000 C26 0.09788 0.04141 -0.10354 1.00000 0.02962 0.05183 0.03261 -0.01131 0.00324 0.01391 0.04411 0.00888 0.00034 0.00038 0.00024 0.00000 0.00180 0.00224 0.00182 0.00159 0.00143 0.00168 0.00091 H26A 0.07094 -0.02916 -0.07705 1.00000 0.05293 0.00000 0.00000 H26B 0.04560 0.01004 -0.16725 1.00000 0.05293 0.00000 0.00000 C27 0.31295 0.16014 -0.00478 1.00000 0.02601 0.02449 0.01706 -0.00032 0.00658 0.00945 0.02434 0.00734 0.00029 0.00027 0.00018 0.00000 0.00149 0.00143 0.00131 0.00109 0.00112 0.00123 0.00060 C28 0.44363 0.19493 0.03130 1.00000 0.02544 0.02857 0.01686 -0.00005 0.00831 0.01142 0.02456 0.00746 0.00029 0.00028 0.00018 0.00000 0.00148 0.00150 0.00130 0.00111 0.00111 0.00126 0.00060 C29 0.52385 0.16623 -0.00843 1.00000 0.02375 0.02832 0.02734 0.00213 0.01149 0.01252 0.02636 0.00779 0.00029 0.00028 0.00020 0.00000 0.00149 0.00154 0.00150 0.00120 0.00121 0.00128 0.00062 C30 0.65739 0.21252 0.02799 1.00000 0.02866 0.03533 0.02315 0.00286 0.00868 0.01473 0.02987 0.00814 0.00031 0.00031 0.00020 0.00000 0.00161 0.00170 0.00147 0.00126 0.00124 0.00140 0.00067 C31 0.87170 0.34775 0.12366 1.00000 0.02357 0.04561 0.03560 0.00207 0.00606 0.01137 0.03882 0.00873 0.00032 0.00035 0.00024 0.00000 0.00164 0.00205 0.00181 0.00152 0.00137 0.00153 0.00080 H31A 0.92289 0.38814 0.18698 1.00000 0.04659 0.00000 0.00000 H31B 0.89705 0.41139 0.09120 1.00000 0.04659 0.00000 0.00000 C32 0.90232 0.24732 0.09507 1.00000 0.03077 0.05073 0.03264 0.00545 0.00758 0.01822 0.03999 0.00925 0.00035 0.00037 0.00023 0.00000 0.00180 0.00218 0.00178 0.00156 0.00142 0.00167 0.00082 H32A 0.99757 0.28249 0.11080 1.00000 0.04799 0.00000 0.00000 H32B 0.87446 0.18234 0.12614 1.00000 0.04799 0.00000 0.00000 C33 0.70652 0.15943 -0.02377 1.00000 0.02719 0.04021 0.02749 0.00900 0.01243 0.01681 0.03074 0.00854 0.00031 0.00032 0.00021 0.00000 0.00160 0.00181 0.00156 0.00134 0.00129 0.00144 0.00068 C34 0.61167 0.07499 -0.09853 1.00000 0.03680 0.04139 0.02530 0.00463 0.01470 0.02082 0.03321 0.00876 0.00033 0.00032 0.00021 0.00000 0.00180 0.00187 0.00154 0.00134 0.00135 0.00156 0.00071 H34 0.62649 0.03062 -0.14116 1.00000 0.03985 0.00000 0.00000 O1 0.49222 0.86312 0.32972 1.00000 0.02042 0.01654 0.03285 0.01099 0.00984 0.00809 0.02315 0.00511 0.00019 0.00018 0.00013 0.00000 0.00099 0.00093 0.00110 0.00082 0.00084 0.00081 0.00042 O2 0.16832 0.52412 0.26512 1.00000 0.01237 0.01329 0.02865 0.00614 0.00606 0.00384 0.01929 0.00471 0.00017 0.00017 0.00013 0.00000 0.00087 0.00087 0.00101 0.00075 0.00075 0.00073 0.00039 O3 0.05453 0.30287 0.29009 1.00000 0.01291 0.01768 0.03247 0.00924 0.00641 0.00573 0.02187 0.00492 0.00018 0.00017 0.00013 0.00000 0.00090 0.00093 0.00108 0.00081 0.00079 0.00077 0.00041 O4 0.41305 0.37511 0.45145 1.00000 0.01039 0.01415 0.01829 0.00334 0.00375 0.00467 0.01519 0.00445 0.00017 0.00016 0.00011 0.00000 0.00083 0.00084 0.00088 0.00068 0.00068 0.00070 0.00036 O5 0.65533 0.45195 0.45209 1.00000 0.01562 0.02137 0.02158 0.00606 0.00880 0.01102 0.01816 0.00480 0.00018 0.00017 0.00012 0.00000 0.00090 0.00095 0.00094 0.00075 0.00074 0.00079 0.00038 O6 0.62745 0.74501 0.38271 1.00000 0.01717 0.01501 0.03044 0.01029 0.01129 0.00713 0.02008 0.00495 0.00018 0.00017 0.00013 0.00000 0.00093 0.00089 0.00104 0.00078 0.00079 0.00077 0.00039 O7 0.39786 0.54732 0.36739 1.00000 0.01163 0.01110 0.02031 0.00426 0.00626 0.00437 0.01464 0.00444 0.00017 0.00016 0.00012 0.00000 0.00083 0.00081 0.00089 0.00068 0.00069 0.00069 0.00035 O8 0.24982 0.33603 0.20764 1.00000 0.01862 0.02357 0.01977 0.00014 0.00659 0.00958 0.02144 0.00485 0.00018 0.00018 0.00012 0.00000 0.00096 0.00099 0.00094 0.00076 0.00076 0.00083 0.00040 O9 0.45769 0.37977 0.28040 1.00000 0.01988 0.01882 0.01748 0.00105 0.00565 0.01035 0.01893 0.00474 0.00018 0.00017 0.00012 0.00000 0.00096 0.00091 0.00090 0.00072 0.00075 0.00079 0.00039 O10 0.13841 0.18031 0.02897 1.00000 0.01950 0.04036 0.02070 -0.00262 0.00405 0.01211 0.02943 0.00532 0.00020 0.00021 0.00013 0.00000 0.00102 0.00125 0.00101 0.00088 0.00081 0.00095 0.00048 O11 0.23513 0.08950 -0.09001 1.00000 0.02586 0.03816 0.01884 -0.00703 0.00367 0.01135 0.03151 0.00531 0.00021 0.00021 0.00013 0.00000 0.00112 0.00125 0.00101 0.00088 0.00085 0.00099 0.00050 O12 0.83636 0.19267 0.00117 1.00000 0.02917 0.05426 0.03319 0.00738 0.01335 0.02037 0.03857 0.00631 0.00023 0.00025 0.00015 0.00000 0.00123 0.00154 0.00124 0.00111 0.00100 0.00117 0.00056 O13 0.73375 0.29745 0.10758 1.00000 0.02486 0.04511 0.03267 -0.00577 0.00627 0.01211 0.03842 0.00579 0.00022 0.00023 0.00015 0.00000 0.00117 0.00142 0.00123 0.00104 0.00096 0.00107 0.00057 O14 0.33107 0.00179 0.48694 1.00000 0.05885 0.09069 0.03529 0.00151 0.01275 -0.00615 0.07993 0.00848 0.00035 0.00038 0.00021 0.00000 0.00208 0.00265 0.00162 0.00175 0.00148 0.00207 0.00122 O15 0.21244 0.46785 0.06273 1.00000 0.05626 0.04938 0.04686 0.02030 0.01433 0.00842 0.05768 0.00785 0.00031 0.00029 0.00020 0.00000 0.00194 0.00172 0.00168 0.00136 0.00141 0.00152 0.00080 O16 0.67317 0.71254 0.18201 1.00000 0.06201 0.05949 0.05138 0.02058 0.03202 0.02201 0.05696 0.00862 0.00032 0.00031 0.00020 0.00000 0.00198 0.00193 0.00173 0.00149 0.00154 0.00166 0.00077 O17 0.63616 0.52329 0.04402 0.50000 0.12128 0.01758 0.04323 0.00827 0.06327 0.01300 0.06011 0.01604 0.00077 0.00043 0.00036 0.00000 0.00548 0.00229 0.00324 0.00212 0.00366 0.00295 0.00195 O18 0.43957 0.63363 0.20826 1.00000 0.02808 0.04484 0.02736 0.00298 0.01388 0.01119 0.03543 0.00628 0.00024 0.00024 0.00015 0.00000 0.00122 0.00142 0.00118 0.00101 0.00097 0.00111 0.00054 O19 0.96774 0.40748 -0.05321 0.50000 0.05162 0.06032 0.06694 0.02998 0.02072 0.00777 0.06592 0.01760 0.00066 0.00064 0.00046 0.00000 0.00375 0.00396 0.00408 0.00333 0.00336 0.00324 0.00181 O20 0.43681 0.76985 0.47333 1.00000 0.02795 0.01994 0.02326 0.00508 0.00981 0.01053 0.02401 0.00539 0.00021 0.00019 0.00013 0.00000 0.00111 0.00100 0.00103 0.00081 0.00086 0.00089 0.00042 S1 0.50886 0.28297 0.13887 1.00000 0.02037 0.02713 0.01847 -0.00004 0.00669 0.01117 0.02269 0.00178 0.00007 0.00007 0.00004 0.00000 0.00034 0.00036 0.00032 0.00027 0.00026 0.00029 0.00015 S2 0.46118 0.05793 -0.10682 1.00000 0.02902 0.03993 0.02352 -0.00216 0.00749 0.01550 0.03263 0.00205 0.00008 0.00008 0.00005 0.00000 0.00041 0.00045 0.00037 0.00032 0.00031 0.00036 0.00019 N1 0.25554 0.64832 0.28496 1.00000 0.01686 0.01374 0.02134 0.00515 0.00867 0.00647 0.01717 0.00568 0.00021 0.00020 0.00014 0.00000 0.00110 0.00103 0.00111 0.00085 0.00089 0.00090 0.00045 N2 0.28152 0.32465 0.39968 1.00000 0.01083 0.01492 0.01622 0.00113 0.00452 0.00363 0.01532 0.00535 0.00020 0.00020 0.00014 0.00000 0.00100 0.00103 0.00102 0.00081 0.00081 0.00085 0.00043 N3 0.65112 0.64548 0.38523 1.00000 0.01473 0.01775 0.02039 0.00642 0.00760 0.00843 0.01695 0.00568 0.00021 0.00020 0.00014 0.00000 0.00106 0.00107 0.00110 0.00087 0.00087 0.00090 0.00044 Mn1 0.52608 0.49790 0.40796 1.00000 0.01064 0.01292 0.01654 0.00399 0.00591 0.00530 0.01325 0.00095 0.00004 0.00003 0.00002 0.00000 0.00019 0.00019 0.00019 0.00014 0.00015 0.00015 0.00010 Mn2 0.22833 0.41804 0.31757 1.00000 0.01038 0.01222 0.01961 0.00432 0.00630 0.00469 0.01413 0.00097 0.00004 0.00003 0.00002 0.00000 0.00019 0.00019 0.00020 0.00015 0.00015 0.00015 0.00010 Mn3 0.44624 0.70103 0.34019 1.00000 0.01342 0.01214 0.02107 0.00592 0.00702 0.00537 0.01552 0.00099 0.00004 0.00003 0.00003 0.00000 0.00020 0.00019 0.00021 0.00015 0.00015 0.00016 0.00010 H14A 0.35583 0.03033 0.54196 1.00000 0.02328 0.06800 0.00315 0.00268 0.00126 0.00000 0.00000 H14B 0.33242 -0.07093 0.48934 1.00000 0.02328 0.08688 0.00364 0.00223 0.00217 0.00000 0.00000 H15A 0.19899 0.41538 0.09588 1.00000 0.02328 0.08539 0.00309 0.00260 0.00189 0.00000 0.00000 H15B 0.27205 0.46570 0.04597 1.00000 0.02328 0.09100 0.00274 0.00319 0.00217 0.00000 0.00000 H16A 0.62907 0.65277 0.12900 1.00000 0.02328 0.05555 0.00293 0.00224 0.00152 0.00000 0.00000 H16B 0.69663 0.78359 0.16461 1.00000 0.02328 0.07618 0.00315 0.00195 0.00200 0.00000 0.00000 H17B 0.71447 0.54831 0.07739 0.50000 0.02328 0.09283 0.00252 0.00529 0.00378 0.00000 0.00000 H17C 0.60735 0.57100 0.05249 0.50000 0.02328 0.13305 0.00470 0.00436 0.00397 0.00000 0.00000 H18A 0.37297 0.58857 0.16459 1.00000 0.02328 0.04952 0.00214 0.00270 0.00163 0.00000 0.00000 H18B 0.50935 0.65750 0.19942 1.00000 0.02328 0.07342 0.00205 0.00293 0.00205 0.00000 0.00000 H19A 0.90704 0.33689 -0.05447 0.50000 0.02328 0.12169 0.00395 0.00334 0.00432 0.00000 0.00000 H19B 1.03639 0.39770 -0.04134 0.50000 0.02328 0.15388 0.00360 0.00553 0.00453 0.00000 0.00000 H20A 0.42166 0.71633 0.50213 1.00000 0.02328 0.08056 0.00306 0.00237 0.00193 0.00000 0.00000 H20B 0.50955 0.83152 0.49871 1.00000 0.02328 0.05242 0.00213 0.00218 0.00198 0.00000 0.00000 Final Structure Factor Calculation for 2008src0895r in P-1 Total number of l.s. parameters = 601 Maximum vector length = 511 Memory required = 5711 / 25039 wR2 = 0.1201 before cycle 11 for 9473 data and 0 / 601 parameters Disagreeable restraints before cycle 11 Observed Target Error Sigma Restraint 0.9246 0.8500 0.0746 0.0200 DFIX O16 H16A Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 14. 7. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.019 0.037 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.034 0.034 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.054; Restrained GooF = 1.055 for 21 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0608 * P )^2 + 2.85 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0426 for 7810 Fo > 4sig(Fo) and 0.0568 for all 9473 data wR2 = 0.1201, GooF = S = 1.054, Restrained GooF = 1.055 for all data Occupancy sum of asymmetric unit = 61.00 for non-hydrogen and 36.00 for hydrogen atoms Principal mean square atomic displacements U 0.0327 0.0183 0.0139 C1 0.0390 0.0217 0.0180 C2 0.0540 0.0239 0.0140 C3 0.0557 0.0283 0.0146 C4 0.0398 0.0269 0.0184 C5 0.0287 0.0199 0.0147 C6 0.0232 0.0203 0.0178 C7 0.0276 0.0173 0.0132 C8 0.0345 0.0259 0.0160 C9 0.0464 0.0325 0.0123 C10 0.0540 0.0436 0.0104 C11 0.0480 0.0295 0.0171 C12 0.0267 0.0218 0.0110 C13 0.0208 0.0194 0.0153 C14 0.0298 0.0162 0.0137 C15 0.0362 0.0245 0.0172 C16 0.0548 0.0288 0.0159 C17 0.0535 0.0421 0.0133 C18 0.0489 0.0369 0.0165 C19 0.0325 0.0283 0.0131 C20 0.0345 0.0267 0.0133 C21 0.0204 0.0172 0.0148 C22 0.0257 0.0189 0.0177 C23 0.0300 0.0202 0.0184 C24 0.0769 0.0340 0.0190 C25 0.0750 0.0355 0.0218 C26 0.0312 0.0270 0.0148 C27 0.0341 0.0256 0.0140 C28 0.0354 0.0253 0.0183 C29 0.0389 0.0286 0.0221 C30 0.0550 0.0384 0.0231 C31 0.0548 0.0370 0.0283 C32 0.0408 0.0283 0.0231 C33 0.0440 0.0357 0.0199 C34 0.0345 0.0213 0.0137 O1 0.0303 0.0168 0.0107 O2 0.0353 0.0177 0.0126 O3 0.0196 0.0155 0.0104 O4 0.0219 0.0209 0.0116 O5 0.0309 0.0176 0.0118 O6 0.0205 0.0133 0.0101 O7 0.0296 0.0186 0.0161 O8 0.0240 0.0187 0.0140 O9 0.0494 0.0215 0.0174 O10 0.0518 0.0287 0.0140 O11 0.0575 0.0334 0.0249 O12 0.0625 0.0293 0.0235 O13 0.1570 0.0489 0.0339 O14 0.0915 0.0467 0.0349 O15 0.0744 0.0610 0.0355 O16 0.1515 0.0176 0.0113 O17 0.0556 0.0292 0.0215 O18 0.1027 0.0605 0.0345 O19 0.0291 0.0232 0.0197 O20 0.0325 0.0200 0.0156 S1 0.0490 0.0289 0.0200 S2 0.0216 0.0167 0.0132 N1 0.0204 0.0151 0.0104 N2 0.0207 0.0167 0.0134 N3 0.0166 0.0133 0.0099 Mn1 0.0198 0.0131 0.0096 Mn2 0.0213 0.0144 0.0109 Mn3 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.017 0.033 0.051 0.069 0.089 0.112 0.138 0.177 0.242 1.000 Number in group 951. 952. 981. 915. 957. 954. 931. 932. 945. 955. GooF 0.947 1.052 1.090 1.193 1.067 1.089 0.954 1.006 1.043 1.077 K 1.665 1.062 0.938 0.937 0.964 0.983 0.992 1.015 1.024 1.001 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.64 inf Number in group 960. 956. 945. 929. 955. 942. 943. 958. 930. 955. GooF 0.933 0.939 0.943 0.927 0.879 0.841 0.815 0.813 0.987 1.951 K 0.971 1.015 0.995 1.007 1.015 1.026 1.024 1.028 1.017 0.975 R1 0.124 0.103 0.089 0.068 0.051 0.043 0.039 0.031 0.030 0.051 Recommended weighting scheme: WGHT 0.0610 2.8411 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 2 0 232.84 18.17 11.76 0.021 5.39 -1 3 1 417.82 107.56 10.36 0.051 3.77 -1 -1 2 5104.59 11151.33 7.80 0.521 5.98 -1 -2 1 361.36 142.33 7.39 0.059 4.30 0 -2 3 543.21 1100.10 7.11 0.164 4.31 1 -6 1 199.66 54.17 7.01 0.036 1.97 -1 -2 2 1973.04 1170.32 6.81 0.169 4.23 0 3 0 191.47 471.50 6.75 0.107 3.60 -7 -10 9 5.03 1590.68 6.34 0.197 0.77 -1 -2 4 510.02 960.69 6.32 0.153 3.43 1 -2 2 102.45 17.81 6.23 0.021 4.96 -1 -1 4 155.54 364.54 5.95 0.094 3.96 -1 -2 5 111.55 285.98 5.80 0.084 2.98 0 -2 2 3489.73 5328.59 5.61 0.360 5.08 -2 0 3 290.56 568.98 5.60 0.118 4.55 6 -5 1 145.59 44.71 5.38 0.033 1.78 -1 3 0 99.20 25.26 5.31 0.025 4.05 -1 1 3 1488.20 955.28 5.27 0.153 4.79 0 -3 1 2204.20 1479.89 5.24 0.190 3.73 -1 2 0 371.61 195.62 5.24 0.069 6.12 1 -2 3 580.46 349.73 4.98 0.092 4.07 -5 4 5 44.21 0.29 4.82 0.003 1.98 0 -6 1 720.45 461.45 4.74 0.106 1.84 -1 2 1 679.63 1033.52 4.50 0.159 5.53 -2 4 1 239.95 126.94 4.35 0.056 2.96 3 2 2 908.82 622.83 4.28 0.123 2.09 8 -12 8 229.30 482.41 4.27 0.108 0.88 -2 3 3 2827.42 2082.60 4.25 0.225 3.12 -1 -1 3 2181.59 1588.38 4.24 0.197 4.91 -1 -5 1 3679.22 2773.61 4.12 0.260 2.00 4 0 6 75.47 21.59 4.07 0.023 1.54 2 -3 2 2839.00 3837.48 4.06 0.306 3.52 -4 2 2 305.26 484.51 3.96 0.109 3.02 -3 0 2 551.35 367.77 3.96 0.095 3.67 1 4 4 614.41 420.26 3.89 0.101 1.77 2 2 0 1008.35 725.73 3.87 0.133 3.06 -5 1 5 12.82 66.11 3.81 0.040 2.19 -6 6 2 497.04 331.73 3.78 0.090 1.71 0 1 3 2018.93 2714.82 3.77 0.257 4.19 -8 5 2 201.78 106.64 3.77 0.051 1.49 1 -4 1 4597.50 6017.02 3.77 0.383 3.03 -2 -1 6 417.49 274.05 3.73 0.082 2.65 -4 5 3 125.60 230.32 3.71 0.075 2.11 0 -5 6 1016.92 1390.31 3.65 0.184 1.91 4 -1 3 413.60 274.90 3.63 0.082 2.17 9 -3 11 -14.89 98.30 3.60 0.049 0.82 -1 3 2 1126.64 1520.91 3.60 0.193 3.37 -3 1 1 85.29 33.46 3.60 0.029 4.03 5 -1 1 102.65 196.28 3.58 0.069 2.09 0 -5 3 64.69 137.36 3.56 0.058 2.21 Bond lengths and angles C1 - Distance Angles O1 1.3305 (0.0035) C2 1.4118 (0.0039) 117.75 (0.27) C6 1.4161 (0.0042) 123.97 (0.24) 118.27 (0.26) C1 - O1 C2 C2 - Distance Angles C3 1.3809 (0.0044) C1 1.4118 (0.0039) 121.29 (0.30) C2 - C3 C3 - Distance Angles C2 1.3809 (0.0044) C4 1.3905 (0.0051) 120.40 (0.28) C3 - C2 C4 - Distance Angles C5 1.3892 (0.0045) C3 1.3905 (0.0051) 119.31 (0.29) C4 - C5 C5 - Distance Angles C4 1.3892 (0.0045) C6 1.3998 (0.0040) 121.46 (0.31) C5 - C4 C6 - Distance Angles C5 1.3998 (0.0040) C1 1.4161 (0.0042) 119.27 (0.26) C7 1.4504 (0.0038) 117.47 (0.27) 123.26 (0.25) C6 - C5 C1 C7 - Distance Angles N1 1.2863 (0.0035) C6 1.4504 (0.0038) 124.41 (0.26) C7 - N1 C8 - Distance Angles O3 1.3295 (0.0033) C13 1.4081 (0.0040) 122.94 (0.24) C9 1.4119 (0.0039) 118.62 (0.26) 118.43 (0.25) C8 - O3 C13 C9 - Distance Angles C10 1.3815 (0.0043) C8 1.4119 (0.0039) 120.05 (0.29) C9 - C10 C10 - Distance Angles C9 1.3815 (0.0043) C11 1.3851 (0.0050) 121.55 (0.29) C10 - C9 C11 - Distance Angles C12 1.3737 (0.0045) C10 1.3851 (0.0050) 119.40 (0.29) C11 - C12 C12 - Distance Angles C11 1.3737 (0.0045) C13 1.4106 (0.0040) 120.72 (0.30) C12 - C11 C13 - Distance Angles C8 1.4081 (0.0040) C12 1.4106 (0.0040) 119.84 (0.26) C14 1.4443 (0.0037) 122.49 (0.24) 117.49 (0.26) C13 - C8 C12 C14 - Distance Angles N2 1.2854 (0.0035) C13 1.4443 (0.0037) 123.82 (0.25) C14 - N2 C15 - Distance Angles O5 1.3405 (0.0032) C16 1.3993 (0.0040) 118.49 (0.26) C20 1.4141 (0.0042) 122.66 (0.24) 118.80 (0.26) C15 - O5 C16 C16 - Distance Angles C17 1.3883 (0.0043) C15 1.3993 (0.0040) 120.47 (0.30) C16 - C17 C17 - Distance Angles C18 1.3803 (0.0051) C16 1.3883 (0.0043) 121.03 (0.30) C17 - C18 C18 - Distance Angles C19 1.3736 (0.0048) C17 1.3803 (0.0051) 119.62 (0.29) C18 - C19 C19 - Distance Angles C18 1.3736 (0.0048) C20 1.4144 (0.0040) 121.02 (0.32) C19 - C18 C20 - Distance Angles C15 1.4141 (0.0042) C19 1.4144 (0.0040) 119.05 (0.28) C21 1.4406 (0.0042) 123.23 (0.25) 117.66 (0.28) C20 - C15 C19 C21 - Distance Angles N3 1.2916 (0.0035) C20 1.4406 (0.0042) 123.53 (0.26) C21 - N3 C22 - Distance Angles O9 1.2604 (0.0032) O8 1.2743 (0.0033) 125.90 (0.24) C23 1.4642 (0.0036) 115.97 (0.24) 118.11 (0.23) C22 - O9 O8 C23 - Distance Angles C24 1.3716 (0.0038) C22 1.4642 (0.0036) 131.58 (0.26) S1 1.7395 (0.0028) 110.76 (0.21) 117.64 (0.20) C23 - C24 C22 C24 - Distance Angles O10 1.3692 (0.0035) C23 1.3716 (0.0039) 124.28 (0.25) C27 1.4172 (0.0040) 123.01 (0.25) 112.70 (0.26) C24 - O10 C23 C25 - Distance Angles O10 1.4429 (0.0038) C26 1.4791 (0.0053) 111.43 (0.31) C25 - O10 C26 - Distance Angles O11 1.4556 (0.0041) C25 1.4791 (0.0053) 112.56 (0.30) C26 - O11 C27 - Distance Angles C28 1.3765 (0.0042) O11 1.3817 (0.0033) 122.94 (0.26) C24 1.4172 (0.0040) 114.16 (0.25) 122.88 (0.26) C27 - C28 O11 C28 - Distance Angles C27 1.3765 (0.0042) C29 1.4575 (0.0040) 128.92 (0.26) S1 1.7352 (0.0028) 109.87 (0.21) 121.21 (0.23) C28 - C27 C29 C29 - Distance Angles C30 1.3830 (0.0044) C28 1.4575 (0.0040) 126.63 (0.28) S2 1.7225 (0.0030) 109.63 (0.22) 123.58 (0.23) C29 - C30 C28 C30 - Distance Angles O13 1.3668 (0.0037) C29 1.3830 (0.0044) 123.10 (0.28) C33 1.4229 (0.0044) 123.39 (0.28) 113.46 (0.28) C30 - O13 C29 C31 - Distance Angles O13 1.4523 (0.0039) C32 1.5034 (0.0052) 110.92 (0.29) C31 - O13 C32 - Distance Angles O12 1.4507 (0.0041) C31 1.5034 (0.0052) 110.77 (0.29) C32 - O12 C33 - Distance Angles C34 1.3529 (0.0046) O12 1.3714 (0.0039) 125.12 (0.29) C30 1.4229 (0.0044) 112.48 (0.29) 122.40 (0.29) C33 - C34 O12 C34 - Distance Angles C33 1.3529 (0.0046) S2 1.7171 (0.0034) 111.64 (0.24) C34 - C33 O1 - Distance Angles C1 1.3305 (0.0035) Mn3 1.8771 (0.0019) 128.81 (0.18) O1 - C1 O2 - Distance Angles N1 1.3796 (0.0028) Mn2 1.9162 (0.0019) 118.45 (0.15) O2 - N1 O3 - Distance Angles C8 1.3295 (0.0033) Mn2 1.8660 (0.0019) 132.84 (0.18) O3 - C8 O4 - Distance Angles N2 1.3926 (0.0027) Mn1 1.9380 (0.0018) 113.04 (0.14) Mn1_$1 2.3756 (0.0018) 113.88 (0.13) 98.55 (0.07) O4 - N2 Mn1 O5 - Distance Angles C15 1.3405 (0.0032) Mn1 1.8717 (0.0018) 124.09 (0.17) O5 - C15 O6 - Distance Angles N3 1.3753 (0.0028) Mn3 1.9167 (0.0019) 114.14 (0.15) O6 - N3 O7 - Distance Angles Mn2 1.8571 (0.0017) Mn3 1.8801 (0.0018) 122.28 (0.10) Mn1 1.8815 (0.0018) 114.61 (0.09) 118.78 (0.09) O7 - Mn2 Mn3 O8 - Distance Angles C22 1.2743 (0.0033) Mn2 2.1201 (0.0019) 122.04 (0.17) O8 - C22 O9 - Distance Angles C22 1.2604 (0.0032) Mn1 2.1357 (0.0018) 135.47 (0.17) O9 - C22 O10 - Distance Angles C24 1.3692 (0.0035) C25 1.4429 (0.0038) 111.88 (0.23) O10 - C24 O11 - Distance Angles C27 1.3817 (0.0033) C26 1.4556 (0.0041) 110.78 (0.23) O11 - C27 O12 - Distance Angles C33 1.3714 (0.0039) C32 1.4507 (0.0041) 110.43 (0.25) O12 - C33 O13 - Distance Angles C30 1.3668 (0.0037) C31 1.4523 (0.0039) 112.20 (0.25) O13 - C30 O18 - Distance Angles Mn3 2.2138 (0.0022) O18 - O20 - Distance Angles Mn3 2.3239 (0.0021) O20 - S1 - Distance Angles C28 1.7352 (0.0028) C23 1.7395 (0.0028) 92.50 (0.14) S1 - C28 S2 - Distance Angles C34 1.7171 (0.0034) C29 1.7225 (0.0030) 92.79 (0.15) S2 - C34 N1 - Distance Angles C7 1.2863 (0.0035) O2 1.3796 (0.0028) 115.54 (0.22) Mn3 2.0066 (0.0023) 126.37 (0.19) 118.08 (0.16) N1 - C7 O2 N2 - Distance Angles C14 1.2854 (0.0035) O4 1.3926 (0.0027) 113.30 (0.21) Mn2 2.0086 (0.0022) 128.72 (0.18) 117.97 (0.15) N2 - C14 O4 N3 - Distance Angles C21 1.2916 (0.0035) O6 1.3753 (0.0028) 117.05 (0.22) Mn1 1.9793 (0.0022) 124.74 (0.20) 118.20 (0.15) N3 - C21 O6 Mn1 - Distance Angles O5 1.8717 (0.0018) O7 1.8815 (0.0018) 178.08 (0.08) O4 1.9380 (0.0018) 89.84 (0.08) 89.84 (0.08) N3 1.9793 (0.0022) 90.94 (0.09) 89.01 (0.08) 168.97 (0.08) O9 2.1357 (0.0018) 91.91 (0.08) 90.01 (0.07) 96.00 (0.08) 94.97 (0.08) O4_$1 2.3756 (0.0018) 91.09 (0.07) 86.99 (0.07) 81.45 (0.07) 87.54 (0.08) 176.06 (0.07) Mn2 3.1462 (0.0005) 148.47 (0.06) 32.46 (0.05) 65.50 (0.05) 117.10 (0.06) 72.64 (0.05) 103.51 (0.04) Mn3 3.2374 (0.0005) 149.10 (0.06) 30.60 (0.05) 118.97 (0.05) 58.60 (0.06) 95.57 (0.05) 83.12 (0.04) 61.67 (0.01) Mn1 - O5 O7 O4 N3 O9 O4_$1 Mn2 Mn2 - Distance Angles O7 1.8571 (0.0018) O3 1.8660 (0.0019) 167.13 (0.09) O2 1.9162 (0.0019) 90.95 (0.08) 88.13 (0.08) N2 2.0086 (0.0022) 88.63 (0.08) 88.83 (0.08) 164.47 (0.09) O8 2.1201 (0.0019) 96.41 (0.08) 96.44 (0.08) 97.84 (0.08) 97.63 (0.08) Mn1 3.1462 (0.0005) 32.94 (0.05) 149.26 (0.06) 122.49 (0.06) 61.01 (0.06) 82.89 (0.05) Mn2 - O7 O3 O2 N2 O8 Mn3 - Distance Angles O1 1.8771 (0.0019) O7 1.8801 (0.0018) 170.89 (0.09) O6 1.9167 (0.0019) 88.84 (0.08) 92.73 (0.08) N1 2.0066 (0.0023) 91.87 (0.09) 87.38 (0.08) 174.81 (0.09) O18 2.2138 (0.0022) 93.67 (0.09) 95.38 (0.09) 86.90 (0.09) 87.92 (0.09) O20 2.3239 (0.0021) 85.65 (0.08) 85.25 (0.08) 97.56 (0.08) 87.62 (0.08) 175.47 (0.09) Mn1 3.2374 (0.0005) 150.62 (0.06) 30.62 (0.05) 62.28 (0.06) 117.39 (0.06) 90.20 (0.07) 92.59 (0.05) Mn3 - O1 O7 O6 N1 O18 O20 FMAP and GRID set by program FMAP 2 2 65 GRID -1.613 -1 -2 1.613 1 2 R1 = 0.0557 for 9473 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.43 at 0.7732 0.5648 0.1019 [ 0.64 A from H17B ] Deepest hole -0.77 at 0.5794 0.9669 0.1000 [ 0.51 A from S2 ] Mean = 0.00, Rms deviation from mean = 0.10 e/A^3, Highest memory used = 5440 / 75027 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.7732 0.5648 0.1019 1.00000 0.05 1.43 0.64 H17B 1.49 O17 1.99 H17C 2.29 H15B Q2 1 0.6003 0.5313 0.0119 1.00000 0.05 0.71 0.63 O17 0.75 H17C 1.41 H17B 2.04 H15B Q3 1 0.6745 0.5203 0.0334 1.00000 0.05 0.65 0.56 O17 0.70 H17B 1.30 H17C 1.62 H15B Q4 1 0.0610 0.0605 -0.0532 1.00000 0.05 0.65 0.94 C25 1.10 C26 1.20 H26A 1.31 H25B Q5 1 0.6418 0.4819 0.0589 1.00000 0.05 0.63 0.61 O17 0.85 H17B 1.33 H17C 2.29 H15B Q6 1 0.4833 0.1501 -0.0604 1.00000 0.05 0.59 0.81 C29 1.18 S2 1.82 C28 1.95 C30 Q7 1 0.1368 0.1131 -0.1282 1.00000 0.05 0.44 1.00 C26 1.22 H26B 1.35 O11 1.56 H25A Q8 1 0.5401 0.6006 0.0962 1.00000 0.05 0.43 0.94 H16A 1.37 H17C 1.71 O16 1.97 H18B Q9 1 0.7012 -0.0003 -0.1228 1.00000 0.05 0.38 1.10 H34 1.80 C34 2.39 C33 2.50 O12 Q10 1 0.5152 0.1476 -0.1310 1.00000 0.05 0.37 1.20 S2 1.76 C34 1.98 C29 2.38 H34 Shortest distances between peaks (including symmetry equivalents) 3 5 0.74 2 3 0.94 2 5 1.17 1 3 1.25 6 10 1.33 1 5 1.39 4 7 1.77 2 8 2.01 2 8 2.02 1 2 2.03 2 2 2.12 5 8 2.41 3 8 2.54 5 8 2.60 3 8 2.62 2 5 2.77 4 4 2.78 2 3 2.97 Time profile in seconds ----------------------- 0.36: Read and process instructions 0.00: Fit rigid groups 0.03: Interpret restraints etc. 0.11: Generate connectivity array 0.09: 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 0.02: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.11: Analyse other restraints etc. 65.06: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.03: OSF, H-atoms from difference map 0.05: Set up l.s. refinement 0.00: Generate idealized H-atoms 31.75: Structure factors and derivatives 51.47: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.94: Apply other restraints 17.97: Solve l.s. equations 0.00: Generate HTAB table 0.14: Other dependent quantities, CIF, tables 0.25: Analysis of variance 0.16: Merge reflections for Fourier and .fcf 1.39: Fourier summations 0.16: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + shelxl finished at 14:15:56 Total CPU time: 170.1 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++