+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 17:16:41 on 02-Aug-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 99SRC141 in P2(1)/c CELL 0.71073 10.082 20.406 18.756 90.00 103.87 90.00 ZERR 4.00 0.002 0.004 0.004 0.00 0.03 0.00 LATT 1 SYMM -X, .5+Y, .5-Z SFAC C H O SB UNIT 184 148 24 4 V = 3746.22 F(000) = 1648.0 Mu = 0.79 mm-1 Cell Wt = 3230.02 Rho = 1.432 L.S. 4 BOND FMAP 2 PLAN 10 HTAB OMIT 0 1 1 OMIT -1 1 1 OMIT 1 0 0 OMIT 2 8 0 WGHT 0.100000 FVAR 0.11650 SB1 4 0.14926 0.35544 0.10039 11.00000 0.01615 0.01097 = 0.01360 0.00018 -0.00026 -0.00049 O1 3 0.05547 0.26874 0.04608 11.00000 0.02175 0.01509 = 0.01723 -0.00219 -0.00091 -0.00192 O2 3 -0.06899 0.33721 -0.03593 11.00000 0.02372 0.01824 = 0.02086 0.00220 0.00097 0.00051 O3 3 -0.17296 0.24185 -0.12846 11.00000 0.02808 0.02847 = 0.01242 0.00331 -0.00560 -0.00015 AFIX 83 H3 2 -0.22614 0.27218 -0.12808 11.00000 -1.50000 AFIX 0 O4 3 0.23601 0.43469 0.16708 11.00000 0.02281 0.01275 = 0.02187 -0.00151 0.00030 -0.00206 O5 3 0.12187 0.50225 0.08049 11.00000 0.02619 0.01783 = 0.02047 -0.00349 -0.00064 0.00152 O6 3 0.26448 0.60533 0.15212 11.00000 0.02353 0.01457 = 0.02041 0.00425 0.00179 -0.00297 AFIX 83 H6 2 0.19249 0.61483 0.12302 11.00000 -1.50000 AFIX 0 C1 1 0.23926 0.37390 0.01235 11.00000 0.02318 0.01643 = 0.01910 -0.00061 0.00547 -0.00091 C2 1 0.17935 0.41332 -0.04695 11.00000 0.03051 0.01870 = 0.02222 0.00214 0.00329 -0.00157 AFIX 43 H2 2 0.10149 0.43761 -0.04651 11.00000 -1.20000 AFIX 0 C3 1 0.23730 0.41592 -0.10673 11.00000 0.05108 0.02806 = 0.02253 0.00510 0.01258 -0.00231 AFIX 43 H3A 2 0.19756 0.44175 -0.14705 11.00000 -1.20000 AFIX 0 C4 1 0.35406 0.38030 -0.10681 11.00000 0.06996 0.03806 = 0.04002 0.00771 0.03697 0.00490 AFIX 43 H4 2 0.39237 0.38216 -0.14720 11.00000 -1.20000 AFIX 0 C5 1 0.41363 0.34211 -0.04719 11.00000 0.05637 0.04809 = 0.05696 0.01735 0.03640 0.02441 AFIX 43 H5 2 0.49306 0.31887 -0.04702 11.00000 -1.20000 AFIX 0 C6 1 0.35592 0.33824 0.01211 11.00000 0.03739 0.03763 = 0.03600 0.01496 0.01699 0.01557 AFIX 43 H6A 2 0.39518 0.31174 0.05193 11.00000 -1.20000 AFIX 0 C7 1 -0.03786 0.37242 0.12890 11.00000 0.02074 0.01197 = 0.02084 -0.00376 0.00527 -0.00332 C8 1 -0.14402 0.40851 0.08610 11.00000 0.02455 0.02092 = 0.02549 0.00046 0.00395 0.00117 AFIX 43 H8 2 -0.13179 0.43187 0.04558 11.00000 -1.20000 AFIX 0 C9 1 -0.26841 0.40905 0.10488 11.00000 0.02607 0.02290 = 0.04308 -0.00389 0.00565 0.00394 AFIX 43 H9 2 -0.34091 0.43256 0.07624 11.00000 -1.20000 AFIX 0 C10 1 -0.28674 0.37513 0.16569 11.00000 0.02983 0.03278 = 0.04802 -0.00837 0.01971 -0.00406 AFIX 43 H10 2 -0.37172 0.37510 0.17692 11.00000 -1.20000 AFIX 0 C11 1 -0.17922 0.34136 0.20966 11.00000 0.04473 0.03079 = 0.02789 -0.00514 0.01761 -0.00776 AFIX 43 H11 2 -0.19073 0.31975 0.25141 11.00000 -1.20000 AFIX 0 C12 1 -0.05456 0.33974 0.19151 11.00000 0.03136 0.02207 = 0.02080 -0.00171 0.00514 -0.00220 AFIX 43 H12 2 0.01818 0.31693 0.22093 11.00000 -1.20000 AFIX 0 C13 1 0.28567 0.29361 0.17322 11.00000 0.01820 0.01668 = 0.01657 0.00266 0.00251 0.00144 C14 1 0.29186 0.22717 0.15674 11.00000 0.02563 0.01668 = 0.02184 0.00137 -0.00352 0.00002 AFIX 43 H14 2 0.22881 0.20925 0.11705 11.00000 -1.20000 AFIX 0 C15 1 0.39212 0.18796 0.19961 11.00000 0.03003 0.01628 = 0.03309 0.00353 0.00602 0.00364 AFIX 43 H15 2 0.39592 0.14370 0.18840 11.00000 -1.20000 AFIX 0 C16 1 0.48581 0.21353 0.25833 11.00000 0.02365 0.02569 = 0.03016 0.00709 -0.00068 0.00672 AFIX 43 H16 2 0.55286 0.18686 0.28679 11.00000 -1.20000 AFIX 0 C17 1 0.47977 0.27913 0.27484 11.00000 0.03745 0.03234 = 0.02739 -0.00173 -0.01659 0.00483 AFIX 43 H17 2 0.54326 0.29660 0.31463 11.00000 -1.20000 AFIX 0 C18 1 0.38044 0.31931 0.23295 11.00000 0.03174 0.02089 = 0.02561 -0.00534 -0.00508 0.00224 AFIX 43 H18 2 0.37713 0.36344 0.24477 11.00000 -1.20000 AFIX 0 C19 1 -0.03779 0.28152 -0.01323 11.00000 0.01599 0.01949 = 0.01544 -0.00157 0.00279 -0.00148 C20 1 -0.11254 0.22184 -0.05449 11.00000 0.02077 0.01954 = 0.01207 0.00016 -0.00380 -0.00238 C21 1 -0.00594 0.16937 -0.05835 11.00000 0.02128 0.02010 = 0.01903 -0.00773 -0.00138 -0.00358 C22 1 0.00950 0.11370 -0.01488 11.00000 0.02590 0.02571 = 0.03041 -0.00130 0.00311 -0.00066 AFIX 43 H22 2 -0.04835 0.10626 0.01615 11.00000 -1.20000 AFIX 0 C23 1 0.11281 0.06870 -0.01799 11.00000 0.03185 0.02862 = 0.04488 -0.00304 0.00085 0.00490 AFIX 43 H23 2 0.12295 0.03116 0.01094 11.00000 -1.20000 AFIX 0 C24 1 0.19873 0.07932 -0.06300 11.00000 0.02663 0.04459 = 0.05166 -0.02300 -0.00086 0.00963 AFIX 43 H24 2 0.26647 0.04895 -0.06510 11.00000 -1.20000 AFIX 0 C25 1 0.18479 0.13519 -0.10533 11.00000 0.03204 0.05938 = 0.04206 -0.00898 0.01563 0.00535 AFIX 43 H25 2 0.24414 0.14297 -0.13546 11.00000 -1.20000 AFIX 0 C26 1 0.08249 0.17971 -0.10302 11.00000 0.03288 0.04072 = 0.02885 -0.00193 0.00826 -0.00170 AFIX 43 H26 2 0.07324 0.21718 -0.13202 11.00000 -1.20000 AFIX 0 C27 1 -0.22502 0.19941 -0.01833 11.00000 0.01845 0.01620 = 0.02357 0.00182 -0.00103 0.00082 C28 1 -0.31594 0.15178 -0.05457 11.00000 0.02781 0.02349 = 0.02603 -0.00376 0.00351 -0.00432 AFIX 43 H28 2 -0.30103 0.13193 -0.09660 11.00000 -1.20000 AFIX 0 C29 1 -0.42810 0.13382 -0.02853 11.00000 0.02779 0.02651 = 0.04095 -0.00223 0.00314 -0.01153 AFIX 43 H29 2 -0.48823 0.10209 -0.05307 11.00000 -1.20000 AFIX 0 C30 1 -0.45064 0.16309 0.03399 11.00000 0.02763 0.02910 = 0.04513 0.00622 0.01349 -0.00538 AFIX 43 H30 2 -0.52739 0.15195 0.05070 11.00000 -1.20000 AFIX 0 C31 1 -0.36014 0.20842 0.07130 11.00000 0.03620 0.03187 = 0.03425 -0.00325 0.01352 -0.00468 AFIX 43 H31 2 -0.37353 0.22685 0.11438 11.00000 -1.20000 AFIX 0 C32 1 -0.24879 0.22684 0.04497 11.00000 0.03029 0.02487 = 0.02720 -0.00677 0.00731 -0.00984 AFIX 43 H32 2 -0.18872 0.25826 0.07026 11.00000 -1.20000 AFIX 0 C33 1 0.19535 0.49286 0.14135 11.00000 0.01385 0.01405 = 0.02208 -0.00159 0.00461 -0.00138 C34 1 0.24330 0.55042 0.19508 11.00000 0.01923 0.01404 = 0.01672 0.00075 0.00213 -0.00338 C35 1 0.37954 0.53500 0.24784 11.00000 0.01949 0.00954 = 0.01974 -0.00094 0.00078 -0.00258 C36 1 0.48938 0.51687 0.21866 11.00000 0.02368 0.02643 = 0.02056 -0.00697 0.00343 -0.00280 AFIX 43 H36 2 0.47832 0.51553 0.16801 11.00000 -1.20000 AFIX 0 C37 1 0.61420 0.50092 0.26437 11.00000 0.02007 0.02831 = 0.03472 -0.00600 0.00469 0.00039 AFIX 43 H37 2 0.68671 0.48901 0.24441 11.00000 -1.20000 AFIX 0 C38 1 0.63163 0.50263 0.33982 11.00000 0.02348 0.02413 = 0.03112 0.00358 -0.00576 -0.00019 AFIX 43 H38 2 0.71537 0.49128 0.37051 11.00000 -1.20000 AFIX 0 C39 1 0.52483 0.52116 0.36939 11.00000 0.02899 0.02698 = 0.02082 0.00448 -0.00024 -0.00196 AFIX 43 H39 2 0.53668 0.52265 0.42008 11.00000 -1.20000 AFIX 0 C40 1 0.39917 0.53766 0.32346 11.00000 0.02279 0.02099 = 0.02308 -0.00035 0.00379 -0.00281 AFIX 43 H40 2 0.32770 0.55059 0.34373 11.00000 -1.20000 AFIX 0 C41 1 0.13058 0.56349 0.23537 11.00000 0.01842 0.01640 = 0.01633 -0.00061 -0.00067 0.00025 C42 1 0.07081 0.51232 0.26490 11.00000 0.02083 0.02021 = 0.02440 -0.00168 0.00356 0.00038 AFIX 43 H42 2 0.09522 0.46937 0.25747 11.00000 -1.20000 AFIX 0 C43 1 -0.02480 0.52442 0.30532 11.00000 0.02235 0.03303 = 0.02290 0.00303 0.00528 -0.00394 AFIX 43 H43 2 -0.06334 0.48966 0.32533 11.00000 -1.20000 AFIX 0 C44 1 -0.06302 0.58766 0.31599 11.00000 0.02490 0.03929 = 0.02806 0.00020 0.00982 0.00643 AFIX 43 H44 2 -0.12796 0.59572 0.34274 11.00000 -1.20000 AFIX 0 C45 1 -0.00468 0.63894 0.28690 11.00000 0.04444 0.02429 = 0.04883 -0.00518 0.01986 0.00763 AFIX 43 H45 2 -0.03017 0.68176 0.29417 11.00000 -1.20000 AFIX 0 C46 1 0.09197 0.62714 0.24675 11.00000 0.03937 0.01728 = 0.03988 -0.00097 0.01750 0.00200 AFIX 43 H46 2 0.13105 0.66210 0.22738 11.00000 -1.20000 HKLF 4 Covalent radii and connectivity table for 99SRC141 in P2(1)/c C 0.770 H 0.320 O 0.660 SB 1.410 Sb1 - C1 O4 C13 C7 O1 O1 - C19 Sb1 O2 - C19 O3 - C20 O4 - C33 Sb1 O5 - C33 O6 - C34 C1 - C6 C2 Sb1 C2 - C3 C1 C3 - C4 C2 C4 - C5 C3 C5 - C6 C4 C6 - C5 C1 C7 - C8 C12 Sb1 C8 - C9 C7 C9 - C8 C10 C10 - C11 C9 C11 - C10 C12 C12 - C11 C7 C13 - C18 C14 Sb1 C14 - C15 C13 C15 - C16 C14 C16 - C15 C17 C17 - C16 C18 C18 - C17 C13 C19 - O2 O1 C20 C20 - O3 C27 C21 C19 C21 - C26 C22 C20 C22 - C21 C23 C23 - C24 C22 C24 - C23 C25 C25 - C24 C26 C26 - C21 C25 C27 - C32 C28 C20 C28 - C29 C27 C29 - C30 C28 C30 - C31 C29 C31 - C30 C32 C32 - C31 C27 C33 - O5 O4 C34 C34 - O6 C35 C41 C33 C35 - C40 C36 C34 C36 - C37 C35 C37 - C36 C38 C38 - C39 C37 C39 - C38 C40 C40 - C35 C39 C41 - C42 C46 C34 C42 - C43 C41 C43 - C44 C42 C44 - C43 C45 C45 - C44 C46 C46 - C41 C45 h k l Fo^2 Sigma Why rejected -8 0 15 50.24 11.79 observed but should be systematically absent -5 0 11 76.42 12.86 observed but should be systematically absent -4 0 11 30.18 6.20 observed but should be systematically absent 52030 Reflections read, of which 975 rejected -12 =< h =< 12, -25 =< k =< 25, -23 =< l =< 23, Max. 2-theta = 52.73 3 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 1 1 0 39.44 0.11 12 9.98 0 2 0 5.18 0.12 2 14.51 -2 2 1 56.64 0.57 9 3.85 0 2 1 81.04 1.34 9 8.50 0 0 2 35.61 0.93 4 8.61 -3 3 2 86.47 0.87 9 6.09 -5 1 3 62.35 0.61 13 3.14 -5 1 4 59.11 0.12 10 7.82 -4 4 6 170.07 1.60 9 11.87 -4 5 6 4.26 0.18 11 2.17 -4 8 6 137.22 1.58 9 9.06 -7 11 6 5.48 0.28 10 1.97 -9 13 6 26.89 1.56 3 10.12 -4 1 7 162.40 1.73 11 8.93 -5 2 7 18.53 0.40 10 8.88 -4 2 7 284.91 3.50 9 18.85 -3 2 7 327.75 0.72 10 29.15 -6 3 7 45.09 1.16 6 8.96 -5 4 7 6.93 0.23 11 1.42 -4 4 7 87.67 1.08 9 5.56 -6 7 7 26.10 0.58 9 3.17 -4 7 7 147.06 1.53 9 9.03 -3 8 7 178.10 1.87 9 11.04 -7 9 7 6.03 0.61 6 3.13 -5 13 7 141.51 2.25 8 11.33 -8 17 7 21.69 1.70 3 9.03 -3 0 8 413.26 4.92 6 45.84 -3 1 8 78.98 0.77 13 5.22 -7 2 8 3.79 0.28 9 3.19 -7 4 8 6.15 0.40 8 3.70 -7 6 8 5.78 0.44 8 9.03 -6 7 8 1.44 0.14 12 1.24 -7 9 8 106.92 1.38 12 8.12 -5 9 8 6.42 0.32 10 2.15 -4 9 8 154.80 1.11 9 10.79 -3 9 8 204.49 1.91 9 10.47 -7 10 8 9.95 0.37 9 2.19 -4 10 8 9.56 0.40 10 4.54 -3 10 8 54.59 0.81 9 4.28 -9 14 8 42.62 2.15 3 18.44 -7 20 8 5.67 1.19 3 8.70 -6 1 9 162.84 2.02 9 12.92 -5 1 9 45.22 0.78 11 5.55 -5 3 9 72.07 1.16 10 7.31 -4 3 9 16.67 0.41 11 2.98 -6 4 9 7.35 0.25 12 3.47 -5 9 9 0.12 0.27 10 1.36 -3 11 9 84.23 0.99 9 5.83 -8 12 9 60.15 1.75 6 11.04 -4 12 9 135.27 0.91 9 11.75 ** etc. ** 93 Inconsistent equivalents 7657 Unique reflections, of which 0 suppressed R(int) = 0.0986 R(sigma) = 0.0501 Friedel opposites merged Maximum memory for data reduction = 4051 / 76317 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 = 5375 / 626948 wR2 = 0.1072 before cycle 1 for 7657 data and 478 / 478 parameters GooF = S = 0.796; Restrained GooF = 0.796 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 0.11650 0.00017 0.017 OSF Mean shift/esd = 0.007 Maximum = 0.479 for y Sb1 Max. shift = 0.000 A for C8 Max. dU = 0.000 for C41 Least-squares cycle 2 Maximum vector length = 511 Memory required = 5375 / 626948 wR2 = 0.1072 before cycle 2 for 7657 data and 478 / 478 parameters GooF = S = 0.796; Restrained GooF = 0.796 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 0.11650 0.00017 0.004 OSF Mean shift/esd = 0.002 Maximum = 0.161 for y Sb1 Max. shift = 0.000 A for C5 Max. dU = 0.000 for C24 Least-squares cycle 3 Maximum vector length = 511 Memory required = 5375 / 626948 wR2 = 0.1072 before cycle 3 for 7657 data and 478 / 478 parameters GooF = S = 0.796; Restrained GooF = 0.796 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 0.11650 0.00017 0.002 OSF Mean shift/esd = 0.000 Maximum = 0.002 for OSF Max. shift = 0.000 A for C5 Max. dU = 0.000 for C10 Least-squares cycle 4 Maximum vector length = 511 Memory required = 5375 / 626948 wR2 = 0.1072 before cycle 4 for 7657 data and 478 / 478 parameters GooF = S = 0.796; Restrained GooF = 0.796 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 0.11650 0.00017 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for U33 Sb1 Max. shift = 0.000 A for C45 Max. dU = 0.000 for C38 Largest correlation matrix elements 0.623 U11 Sb1 / OSF 0.588 U13 C4 / U33 C4 0.524 U13 C5 / U11 C5 0.613 U22 Sb1 / OSF 0.557 U13 C4 / U11 C4 0.607 U33 Sb1 / OSF 0.553 U13 C5 / U33 C5 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 -0.2261 0.2722 -0.1281 83 0.820 0.000 O3 C20 H3 H6 0.1925 0.6148 0.1230 83 0.820 0.000 O6 C34 H6 H2 0.1015 0.4376 -0.0465 43 0.930 0.000 C2 C3 C1 H3A 0.1976 0.4417 -0.1471 43 0.930 0.000 C3 C4 C2 H4 0.3924 0.3822 -0.1472 43 0.930 0.000 C4 C5 C3 H5 0.4931 0.3189 -0.0470 43 0.930 0.000 C5 C6 C4 H6A 0.3952 0.3117 0.0519 43 0.930 0.000 C6 C5 C1 H8 -0.1318 0.4319 0.0456 43 0.930 0.000 C8 C9 C7 H9 -0.3409 0.4326 0.0762 43 0.930 0.000 C9 C8 C10 H10 -0.3717 0.3751 0.1769 43 0.930 0.000 C10 C11 C9 H11 -0.1907 0.3198 0.2514 43 0.930 0.000 C11 C10 C12 H12 0.0182 0.3169 0.2209 43 0.930 0.000 C12 C11 C7 H14 0.2288 0.2092 0.1171 43 0.930 0.000 C14 C15 C13 H15 0.3959 0.1437 0.1884 43 0.930 0.000 C15 C16 C14 H16 0.5529 0.1869 0.2868 43 0.930 0.000 C16 C15 C17 H17 0.5433 0.2966 0.3146 43 0.930 0.000 C17 C16 C18 H18 0.3771 0.3634 0.2448 43 0.930 0.000 C18 C17 C13 H22 -0.0484 0.1063 0.0162 43 0.930 0.000 C22 C21 C23 H23 0.1229 0.0312 0.0109 43 0.930 0.000 C23 C24 C22 H24 0.2665 0.0490 -0.0651 43 0.930 0.000 C24 C23 C25 H25 0.2441 0.1430 -0.1355 43 0.930 0.000 C25 C24 C26 H26 0.0732 0.2172 -0.1320 43 0.930 0.000 C26 C21 C25 H28 -0.3010 0.1319 -0.0966 43 0.930 0.000 C28 C29 C27 H29 -0.4882 0.1021 -0.0531 43 0.930 0.000 C29 C30 C28 H30 -0.5274 0.1519 0.0507 43 0.930 0.000 C30 C31 C29 H31 -0.3735 0.2268 0.1144 43 0.930 0.000 C31 C30 C32 H32 -0.1887 0.2583 0.0703 43 0.930 0.000 C32 C31 C27 H36 0.4783 0.5155 0.1680 43 0.930 0.000 C36 C37 C35 H37 0.6867 0.4890 0.2444 43 0.930 0.000 C37 C36 C38 H38 0.7154 0.4913 0.3705 43 0.930 0.000 C38 C39 C37 H39 0.5367 0.5227 0.4201 43 0.930 0.000 C39 C38 C40 H40 0.3277 0.5506 0.3437 43 0.930 0.000 C40 C35 C39 H42 0.0952 0.4694 0.2575 43 0.930 0.000 C42 C43 C41 H43 -0.0633 0.4897 0.3253 43 0.930 0.000 C43 C44 C42 H44 -0.1280 0.5957 0.3427 43 0.930 0.000 C44 C43 C45 H45 -0.0302 0.6818 0.2942 43 0.930 0.000 C45 C44 C46 H46 0.1311 0.6621 0.2274 43 0.930 0.000 C46 C41 C45 99SRC141 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq Sb1 0.14926 0.35544 0.10039 1.00000 0.01615 0.01097 0.01360 0.00018 -0.00026 -0.00049 0.01422 0.00028 0.00001 0.00001 0.00001 0.00000 0.00012 0.00012 0.00012 0.00006 0.00008 0.00005 0.00008 O1 0.05547 0.26874 0.04608 1.00000 0.02175 0.01509 0.01723 -0.00219 -0.00091 -0.00192 0.01897 0.00311 0.00017 0.00008 0.00009 0.00000 0.00087 0.00094 0.00092 0.00073 0.00072 0.00069 0.00038 O2 -0.06899 0.33721 -0.03593 1.00000 0.02372 0.01824 0.02086 0.00220 0.00097 0.00051 0.02168 0.00350 0.00018 0.00009 0.00010 0.00000 0.00092 0.00096 0.00100 0.00080 0.00076 0.00077 0.00040 O3 -0.17296 0.24185 -0.12846 1.00000 0.02808 0.02847 0.01242 0.00331 -0.00560 -0.00015 0.02476 0.00342 0.00018 0.00010 0.00010 0.00000 0.00094 0.00112 0.00092 0.00082 0.00074 0.00081 0.00042 H3 -0.22614 0.27218 -0.12808 1.00000 0.03714 0.00000 0.00000 O4 0.23601 0.43469 0.16708 1.00000 0.02281 0.01275 0.02187 -0.00151 0.00030 -0.00206 0.02000 0.00313 0.00017 0.00008 0.00009 0.00000 0.00087 0.00091 0.00096 0.00076 0.00072 0.00071 0.00038 O5 0.12187 0.50225 0.08049 1.00000 0.02619 0.01783 0.02047 -0.00350 -0.00064 0.00152 0.02255 0.00348 0.00018 0.00009 0.00010 0.00000 0.00091 0.00099 0.00097 0.00081 0.00078 0.00076 0.00041 O6 0.26448 0.60533 0.15212 1.00000 0.02353 0.01457 0.02041 0.00425 0.00179 -0.00297 0.02009 0.00324 0.00017 0.00008 0.00010 0.00000 0.00086 0.00095 0.00095 0.00075 0.00073 0.00070 0.00038 H6 0.19248 0.61483 0.12302 1.00000 0.03014 0.00000 0.00000 C1 0.23926 0.37390 0.01235 1.00000 0.02318 0.01643 0.01910 -0.00061 0.00547 -0.00091 0.01950 0.00491 0.00026 0.00013 0.00014 0.00000 0.00127 0.00129 0.00136 0.00109 0.00104 0.00104 0.00053 C2 0.17935 0.41332 -0.04695 1.00000 0.03051 0.01870 0.02222 0.00214 0.00329 -0.00157 0.02433 0.00505 0.00027 0.00013 0.00015 0.00000 0.00137 0.00140 0.00142 0.00112 0.00114 0.00109 0.00058 H2 0.10149 0.43761 -0.04651 1.00000 0.02919 0.00000 0.00000 C3 0.23730 0.41592 -0.10673 1.00000 0.05108 0.02806 0.02253 0.00510 0.01258 -0.00231 0.03325 0.00583 0.00032 0.00015 0.00016 0.00000 0.00183 0.00166 0.00153 0.00127 0.00135 0.00137 0.00069 H3A 0.19756 0.44175 -0.14705 1.00000 0.03991 0.00000 0.00000 C4 0.35406 0.38030 -0.10681 1.00000 0.06996 0.03806 0.04002 0.00771 0.03697 0.00490 0.04531 0.00732 0.00035 0.00019 0.00018 0.00000 0.00261 0.00212 0.00211 0.00156 0.00196 0.00165 0.00094 H4 0.39237 0.38216 -0.14720 1.00000 0.05438 0.00000 0.00000 C5 0.41363 0.34211 -0.04719 1.00000 0.05637 0.04809 0.05696 0.01735 0.03640 0.02441 0.04994 0.00862 0.00040 0.00019 0.00022 0.00000 0.00225 0.00215 0.00249 0.00187 0.00198 0.00177 0.00099 H5 0.49306 0.31887 -0.04702 1.00000 0.05993 0.00000 0.00000 C6 0.35592 0.33824 0.01211 1.00000 0.03739 0.03763 0.03600 0.01496 0.01699 0.01557 0.03562 0.00695 0.00032 0.00017 0.00018 0.00000 0.00173 0.00178 0.00185 0.00151 0.00145 0.00145 0.00075 H6A 0.39518 0.31174 0.05193 1.00000 0.04274 0.00000 0.00000 C7 -0.03786 0.37242 0.12890 1.00000 0.02074 0.01197 0.02084 -0.00376 0.00527 -0.00332 0.01780 0.00472 0.00025 0.00012 0.00014 0.00000 0.00123 0.00121 0.00137 0.00104 0.00103 0.00097 0.00052 C8 -0.14402 0.40851 0.08610 1.00000 0.02455 0.02093 0.02549 0.00046 0.00395 0.00117 0.02400 0.00508 0.00026 0.00014 0.00015 0.00000 0.00130 0.00143 0.00149 0.00117 0.00112 0.00109 0.00058 H8 -0.13179 0.43187 0.04558 1.00000 0.02880 0.00000 0.00000 C9 -0.26841 0.40905 0.10488 1.00000 0.02607 0.02290 0.04308 -0.00389 0.00565 0.00394 0.03113 0.00553 0.00028 0.00014 0.00017 0.00000 0.00139 0.00151 0.00184 0.00137 0.00130 0.00116 0.00067 H9 -0.34091 0.43256 0.07624 1.00000 0.03736 0.00000 0.00000 C10 -0.28674 0.37513 0.16569 1.00000 0.02983 0.03278 0.04802 -0.00837 0.01971 -0.00406 0.03512 0.00607 0.00031 0.00016 0.00019 0.00000 0.00154 0.00168 0.00204 0.00154 0.00145 0.00133 0.00073 H10 -0.37172 0.37510 0.17692 1.00000 0.04214 0.00000 0.00000 C11 -0.17922 0.34136 0.20966 1.00000 0.04473 0.03079 0.02789 -0.00514 0.01761 -0.00776 0.03296 0.00590 0.00032 0.00016 0.00017 0.00000 0.00183 0.00164 0.00168 0.00134 0.00143 0.00140 0.00071 H11 -0.19073 0.31975 0.25141 1.00000 0.03955 0.00000 0.00000 C12 -0.05456 0.33974 0.19151 1.00000 0.03136 0.02207 0.02080 -0.00171 0.00514 -0.00220 0.02493 0.00541 0.00030 0.00014 0.00016 0.00000 0.00150 0.00142 0.00148 0.00118 0.00119 0.00119 0.00060 H12 0.01818 0.31693 0.22093 1.00000 0.02992 0.00000 0.00000 C13 0.28567 0.29361 0.17322 1.00000 0.01820 0.01668 0.01657 0.00266 0.00251 0.00144 0.01743 0.00474 0.00024 0.00013 0.00014 0.00000 0.00118 0.00129 0.00129 0.00103 0.00098 0.00097 0.00052 C14 0.29186 0.22717 0.15674 1.00000 0.02563 0.01668 0.02184 0.00137 -0.00352 0.00002 0.02294 0.00502 0.00026 0.00013 0.00015 0.00000 0.00132 0.00138 0.00139 0.00112 0.00108 0.00106 0.00057 H14 0.22881 0.20925 0.11705 1.00000 0.02753 0.00000 0.00000 C15 0.39212 0.18796 0.19961 1.00000 0.03003 0.01628 0.03309 0.00353 0.00602 0.00364 0.02673 0.00541 0.00027 0.00014 0.00016 0.00000 0.00141 0.00141 0.00163 0.00122 0.00123 0.00111 0.00062 H15 0.39592 0.14370 0.18840 1.00000 0.03207 0.00000 0.00000 C16 0.48581 0.21353 0.25833 1.00000 0.02365 0.02569 0.03016 0.00709 -0.00068 0.00672 0.02771 0.00544 0.00027 0.00014 0.00016 0.00000 0.00133 0.00155 0.00158 0.00127 0.00116 0.00115 0.00062 H16 0.55286 0.18686 0.28679 1.00000 0.03325 0.00000 0.00000 C17 0.47977 0.27913 0.27484 1.00000 0.03745 0.03234 0.02739 -0.00173 -0.01659 0.00483 0.03652 0.00567 0.00031 0.00016 0.00017 0.00000 0.00161 0.00179 0.00163 0.00137 0.00130 0.00134 0.00075 H17 0.54326 0.29660 0.31463 1.00000 0.04383 0.00000 0.00000 C18 0.38044 0.31931 0.23295 1.00000 0.03174 0.02089 0.02561 -0.00534 -0.00508 0.00224 0.02810 0.00523 0.00028 0.00014 0.00016 0.00000 0.00147 0.00154 0.00155 0.00122 0.00120 0.00116 0.00065 H18 0.37713 0.36344 0.24477 1.00000 0.03373 0.00000 0.00000 C19 -0.03779 0.28152 -0.01323 1.00000 0.01599 0.01949 0.01544 -0.00157 0.00279 -0.00148 0.01714 0.00455 0.00023 0.00013 0.00013 0.00000 0.00115 0.00136 0.00126 0.00106 0.00096 0.00100 0.00052 C20 -0.11254 0.22184 -0.05449 1.00000 0.02077 0.01954 0.01207 0.00016 -0.00380 -0.00238 0.01878 0.00464 0.00025 0.00013 0.00014 0.00000 0.00121 0.00140 0.00122 0.00104 0.00098 0.00104 0.00054 C21 -0.00594 0.16937 -0.05835 1.00000 0.02128 0.02010 0.01903 -0.00773 -0.00138 -0.00358 0.02119 0.00466 0.00025 0.00013 0.00014 0.00000 0.00125 0.00141 0.00137 0.00112 0.00104 0.00106 0.00056 C22 0.00950 0.11370 -0.01488 1.00000 0.02590 0.02571 0.03041 -0.00131 0.00311 -0.00066 0.02796 0.00535 0.00028 0.00014 0.00016 0.00000 0.00135 0.00159 0.00162 0.00130 0.00118 0.00117 0.00062 H22 -0.04835 0.10626 0.01615 1.00000 0.03355 0.00000 0.00000 C23 0.11281 0.06870 -0.01799 1.00000 0.03185 0.02862 0.04488 -0.00304 0.00085 0.00490 0.03653 0.00563 0.00029 0.00016 0.00018 0.00000 0.00154 0.00172 0.00193 0.00148 0.00138 0.00129 0.00073 H23 0.12295 0.03116 0.01094 1.00000 0.04384 0.00000 0.00000 C24 0.19873 0.07932 -0.06300 1.00000 0.02663 0.04459 0.05166 -0.02300 -0.00086 0.00963 0.04269 0.00579 0.00030 0.00018 0.00019 0.00000 0.00151 0.00214 0.00214 0.00175 0.00144 0.00138 0.00087 H24 0.26647 0.04895 -0.06510 1.00000 0.05123 0.00000 0.00000 C25 0.18479 0.13519 -0.10533 1.00000 0.03204 0.05938 0.04206 -0.00898 0.01563 0.00535 0.04335 0.00682 0.00034 0.00018 0.00021 0.00000 0.00174 0.00252 0.00212 0.00171 0.00155 0.00151 0.00089 H25 0.24414 0.14297 -0.13546 1.00000 0.05202 0.00000 0.00000 C26 0.08249 0.17971 -0.10302 1.00000 0.03288 0.04072 0.02885 -0.00193 0.00826 -0.00170 0.03400 0.00569 0.00029 0.00017 0.00016 0.00000 0.00153 0.00196 0.00165 0.00142 0.00129 0.00136 0.00070 H26 0.07324 0.21718 -0.13202 1.00000 0.04080 0.00000 0.00000 C27 -0.22502 0.19941 -0.01833 1.00000 0.01845 0.01620 0.02357 0.00182 -0.00103 0.00082 0.02044 0.00478 0.00024 0.00013 0.00014 0.00000 0.00119 0.00133 0.00141 0.00109 0.00103 0.00099 0.00055 C28 -0.31594 0.15178 -0.05457 1.00000 0.02781 0.02349 0.02603 -0.00376 0.00351 -0.00432 0.02628 0.00540 0.00029 0.00013 0.00017 0.00000 0.00146 0.00153 0.00157 0.00116 0.00122 0.00109 0.00063 H28 -0.30103 0.13193 -0.09660 1.00000 0.03153 0.00000 0.00000 C29 -0.42810 0.13382 -0.02853 1.00000 0.02779 0.02651 0.04095 -0.00223 0.00314 -0.01153 0.03261 0.00577 0.00030 0.00014 0.00018 0.00000 0.00151 0.00164 0.00193 0.00136 0.00137 0.00118 0.00072 H29 -0.48823 0.10209 -0.05307 1.00000 0.03914 0.00000 0.00000 C30 -0.45064 0.16309 0.03399 1.00000 0.02763 0.02910 0.04513 0.00622 0.01349 -0.00538 0.03314 0.00598 0.00029 0.00016 0.00018 0.00000 0.00150 0.00162 0.00197 0.00146 0.00139 0.00127 0.00070 H30 -0.52739 0.15195 0.05070 1.00000 0.03977 0.00000 0.00000 C31 -0.36014 0.20842 0.07130 1.00000 0.03620 0.03187 0.03425 -0.00324 0.01352 -0.00468 0.03325 0.00577 0.00028 0.00016 0.00017 0.00000 0.00160 0.00175 0.00173 0.00141 0.00130 0.00129 0.00068 H31 -0.37353 0.22685 0.11438 1.00000 0.03990 0.00000 0.00000 C32 -0.24879 0.22684 0.04497 1.00000 0.03029 0.02487 0.02720 -0.00677 0.00731 -0.00984 0.02738 0.00522 0.00027 0.00014 0.00015 0.00000 0.00142 0.00155 0.00151 0.00124 0.00119 0.00116 0.00062 H32 -0.18872 0.25826 0.07026 1.00000 0.03286 0.00000 0.00000 C33 0.19535 0.49286 0.14135 1.00000 0.01385 0.01405 0.02208 -0.00159 0.00461 -0.00138 0.01661 0.00465 0.00023 0.00012 0.00014 0.00000 0.00112 0.00129 0.00138 0.00107 0.00101 0.00095 0.00052 C34 0.24330 0.55042 0.19508 1.00000 0.01923 0.01404 0.01672 0.00075 0.00213 -0.00338 0.01703 0.00453 0.00024 0.00012 0.00013 0.00000 0.00116 0.00127 0.00126 0.00100 0.00098 0.00095 0.00051 C35 0.37954 0.53500 0.24784 1.00000 0.01949 0.00954 0.01974 -0.00094 0.00078 -0.00258 0.01692 0.00447 0.00024 0.00012 0.00014 0.00000 0.00117 0.00120 0.00132 0.00101 0.00101 0.00094 0.00051 C36 0.48938 0.51687 0.21866 1.00000 0.02368 0.02643 0.02056 -0.00697 0.00343 -0.00280 0.02388 0.00492 0.00025 0.00014 0.00015 0.00000 0.00129 0.00155 0.00139 0.00116 0.00109 0.00110 0.00059 H36 0.47832 0.51553 0.16801 1.00000 0.02865 0.00000 0.00000 C37 0.61420 0.50092 0.26437 1.00000 0.02007 0.02831 0.03472 -0.00600 0.00469 0.00039 0.02802 0.00519 0.00026 0.00014 0.00016 0.00000 0.00128 0.00160 0.00169 0.00130 0.00120 0.00112 0.00064 H37 0.68671 0.48901 0.24441 1.00000 0.03362 0.00000 0.00000 C38 0.63163 0.50263 0.33982 1.00000 0.02348 0.02413 0.03112 0.00358 -0.00576 -0.00019 0.02833 0.00518 0.00027 0.00014 0.00016 0.00000 0.00131 0.00151 0.00162 0.00126 0.00117 0.00113 0.00063 H38 0.71537 0.49128 0.37051 1.00000 0.03399 0.00000 0.00000 C39 0.52483 0.52116 0.36939 1.00000 0.02899 0.02698 0.02082 0.00448 -0.00024 -0.00196 0.02665 0.00518 0.00026 0.00014 0.00016 0.00000 0.00140 0.00158 0.00142 0.00120 0.00114 0.00117 0.00061 H39 0.53668 0.52265 0.42008 1.00000 0.03198 0.00000 0.00000 C40 0.39917 0.53766 0.32346 1.00000 0.02279 0.02099 0.02308 -0.00035 0.00379 -0.00281 0.02258 0.00483 0.00026 0.00013 0.00014 0.00000 0.00125 0.00142 0.00142 0.00113 0.00108 0.00107 0.00057 H40 0.32770 0.55059 0.34373 1.00000 0.02709 0.00000 0.00000 C41 0.13058 0.56349 0.23537 1.00000 0.01842 0.01640 0.01633 -0.00061 -0.00067 0.00025 0.01787 0.00451 0.00024 0.00012 0.00013 0.00000 0.00115 0.00130 0.00126 0.00105 0.00096 0.00099 0.00051 C42 0.07081 0.51232 0.26490 1.00000 0.02083 0.02021 0.02440 -0.00168 0.00356 0.00038 0.02213 0.00472 0.00024 0.00013 0.00014 0.00000 0.00125 0.00142 0.00145 0.00113 0.00108 0.00104 0.00057 H42 0.09522 0.46936 0.25747 1.00000 0.02656 0.00000 0.00000 C43 -0.02480 0.52442 0.30532 1.00000 0.02235 0.03303 0.02290 0.00303 0.00528 -0.00394 0.02612 0.00509 0.00025 0.00015 0.00015 0.00000 0.00128 0.00166 0.00145 0.00122 0.00112 0.00115 0.00061 H43 -0.06334 0.48966 0.32533 1.00000 0.03134 0.00000 0.00000 C44 -0.06302 0.58766 0.31599 1.00000 0.02490 0.03929 0.02806 0.00020 0.00982 0.00643 0.03016 0.00567 0.00027 0.00016 0.00016 0.00000 0.00136 0.00180 0.00159 0.00133 0.00121 0.00123 0.00066 H44 -0.12796 0.59572 0.34274 1.00000 0.03619 0.00000 0.00000 C45 -0.00468 0.63894 0.28690 1.00000 0.04444 0.02429 0.04883 -0.00518 0.01986 0.00763 0.03771 0.00668 0.00035 0.00015 0.00020 0.00000 0.00189 0.00173 0.00219 0.00140 0.00166 0.00127 0.00080 H45 -0.03017 0.68176 0.29417 1.00000 0.04526 0.00000 0.00000 C46 0.09197 0.62714 0.24675 1.00000 0.03937 0.01728 0.03988 -0.00097 0.01750 0.00200 0.03082 0.00603 0.00031 0.00015 0.00018 0.00000 0.00165 0.00141 0.00183 0.00133 0.00141 0.00123 0.00067 H46 0.13105 0.66210 0.22738 1.00000 0.03698 0.00000 0.00000 Final Structure Factor Calculation for 99SRC141 in P2(1)/c Total number of l.s. parameters = 478 Maximum vector length = 511 Memory required = 4897 / 22995 wR2 = 0.1072 before cycle 5 for 7657 data and 0 / 478 parameters GooF = S = 0.796; Restrained GooF = 0.796 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 = 0.0348 for 6257 Fo > 4sig(Fo) and 0.0474 for all 7657 data wR2 = 0.1072, GooF = S = 0.796, Restrained GooF = 0.796 for all data Occupancy sum of asymmetric unit = 53.00 for non-hydrogen and 37.00 for hydrogen atoms Principal mean square atomic displacements U 0.0202 0.0116 0.0109 Sb1 0.0273 0.0174 0.0122 O1 0.0284 0.0202 0.0164 O2 0.0371 0.0284 0.0088 O3 0.0290 0.0190 0.0119 O4 0.0331 0.0193 0.0152 O5 0.0291 0.0193 0.0119 O6 0.0233 0.0190 0.0162 C1 0.0329 0.0224 0.0176 C2 0.0513 0.0311 0.0174 C3 0.0797 0.0379 0.0183 C4 0.0915 0.0349 0.0235 C5 0.0601 0.0259 0.0209 C6 0.0229 0.0204 0.0101 C7 0.0278 0.0237 0.0205 C8 0.0456 0.0281 0.0196 C9 0.0542 0.0294 0.0218 C10 0.0505 0.0273 0.0211 C11 0.0323 0.0230 0.0195 C12 0.0199 0.0190 0.0135 C13 0.0361 0.0174 0.0154 C14 0.0344 0.0309 0.0149 C15 0.0376 0.0315 0.0141 C16 0.0659 0.0315 0.0122 C17 0.0462 0.0218 0.0164 C18 0.0202 0.0170 0.0142 C19 0.0284 0.0190 0.0090 C20 0.0297 0.0243 0.0096 C21 0.0337 0.0263 0.0239 C22 0.0530 0.0316 0.0251 C23 0.0801 0.0268 0.0211 C24 0.0639 0.0427 0.0234 C25 0.0413 0.0325 0.0282 C26 0.0296 0.0174 0.0143 C27 0.0313 0.0287 0.0189 C28 0.0451 0.0373 0.0154 C29 0.0473 0.0337 0.0185 C30 0.0420 0.0296 0.0281 C31 0.0385 0.0275 0.0161 C32 0.0224 0.0148 0.0126 C33 0.0227 0.0160 0.0124 C34 0.0249 0.0171 0.0088 C35 0.0311 0.0250 0.0155 C36 0.0393 0.0247 0.0201 C37 0.0446 0.0240 0.0164 C38 0.0366 0.0258 0.0176 C39 0.0261 0.0228 0.0188 C40 0.0239 0.0164 0.0133 C41 0.0264 0.0204 0.0196 C42 0.0356 0.0226 0.0202 C43 0.0417 0.0290 0.0198 C44 0.0539 0.0414 0.0178 C45 0.0461 0.0296 0.0168 C46 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.015 0.029 0.045 0.062 0.082 0.105 0.128 0.160 0.207 1.000 Number in group 802. 756. 772. 756. 749. 783. 739. 771. 759. 770. GooF 0.847 0.969 0.917 0.911 0.836 0.775 0.717 0.651 0.663 0.573 K 0.839 1.002 0.968 0.998 0.980 0.990 0.999 1.009 1.026 1.006 Resolution(A) 0.80 0.83 0.86 0.90 0.95 1.01 1.09 1.20 1.37 1.72 inf Number in group 771. 759. 765. 768. 773. 765. 771. 753. 767. 765. GooF 0.848 0.792 0.770 0.816 0.783 0.760 0.706 0.673 0.807 0.966 K 1.002 1.008 1.011 1.009 1.023 1.025 1.034 1.029 1.025 0.975 R1 0.107 0.078 0.065 0.060 0.051 0.043 0.035 0.029 0.029 0.030 Recommended weighting scheme: WGHT 0.0521 0.0854 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 1 5 8 191.51 82.04 5.73 0.023 1.87 -1 4 8 47.64 103.77 4.87 0.026 2.13 -1 11 5 70.46 163.39 4.81 0.032 1.66 1 0 8 214.36 373.38 4.78 0.048 2.11 1 1 0 2905.50 6112.59 4.67 0.196 8.83 -4 4 3 53.73 28.00 4.67 0.013 2.23 -1 3 6 180.47 113.55 4.52 0.027 2.83 3 8 5 203.23 118.45 4.27 0.027 1.66 2 6 8 267.90 391.68 4.18 0.050 1.66 -2 3 6 87.80 46.31 4.13 0.017 2.68 -2 1 8 71.04 118.12 4.05 0.027 2.27 -10 10 15 5.84 239.19 4.04 0.039 0.80 -1 2 4 43.34 16.68 3.86 0.010 4.17 -2 9 2 214.94 310.43 3.81 0.044 2.05 -4 9 5 157.11 99.90 3.71 0.025 1.62 -9 14 10 510.66 983.58 3.70 0.079 0.85 0 4 21 177.02 552.05 3.67 0.059 0.85 -5 5 7 179.51 127.07 3.66 0.028 1.63 -4 2 5 391.48 540.39 3.66 0.058 2.25 -3 4 4 1158.93 1562.46 3.59 0.099 2.60 -4 8 18 -40.17 71.16 3.57 0.021 0.95 2 9 13 -32.66 90.83 3.56 0.024 1.11 3 5 6 322.69 233.76 3.54 0.038 1.79 -12 1 9 267.57 649.09 3.53 0.064 0.83 1 10 11 141.69 237.17 3.48 0.039 1.25 1 2 2 57.85 36.14 3.47 0.015 5.16 -3 8 8 170.92 254.44 3.44 0.040 1.63 9 2 8 47.06 161.61 3.43 0.032 0.90 -6 2 19 177.38 342.71 3.41 0.046 0.93 -4 5 5 129.93 91.76 3.41 0.024 2.01 -2 1 11 201.41 134.06 3.41 0.029 1.69 -1 0 2 76935.17 113763.64 3.38 0.845 7.64 -6 5 1 120.19 80.22 3.34 0.022 1.54 -5 1 4 4354.56 6419.57 3.30 0.201 1.97 0 2 19 108.57 6.86 3.26 0.007 0.95 -2 5 19 193.11 64.19 3.25 0.020 0.96 2 1 8 183.98 252.22 3.22 0.040 1.89 3 0 4 951.62 1246.83 3.21 0.088 2.39 2 11 1 195.64 279.42 3.20 0.042 1.71 5 18 0 312.55 451.70 3.19 0.053 0.98 -2 2 7 352.19 477.47 3.16 0.055 2.49 0 7 10 258.97 366.64 3.11 0.048 1.54 4 8 10 361.53 240.11 3.11 0.039 1.17 4 10 7 362.38 488.64 3.10 0.055 1.26 -8 7 12 146.59 206.19 3.09 0.036 1.02 -8 4 20 822.39 517.33 3.07 0.057 0.82 3 21 2 114.76 260.25 3.06 0.040 0.92 -3 8 5 -14.40 28.14 3.06 0.013 1.88 3 5 1 32.66 10.42 3.04 0.008 2.46 0 2 0 381.46 2928.38 3.04 0.135 10.20 Bond lengths and angles Sb1 - Distance Angles C1 2.1001 (0.0026) O4 2.1024 (0.0017) 97.66 (0.09) C13 2.1091 (0.0025) 106.19 (0.10) 87.77 (0.09) C7 2.1091 (0.0025) 138.70 (0.10) 89.58 (0.08) 114.71 (0.10) O1 2.1449 (0.0017) 89.93 (0.09) 171.98 (0.07) 87.64 (0.08) 86.37 (0.08) Sb1 - C1 O4 C13 C7 O1 - Distance Angles C19 1.2993 (0.0029) Sb1 2.1449 (0.0017) 112.77 (0.15) O1 - C19 O2 - Distance Angles C19 1.2277 (0.0032) O2 - O3 - Distance Angles C20 1.4345 (0.0031) O3 - O4 - Distance Angles C33 1.3096 (0.0030) Sb1 2.1024 (0.0017) 115.41 (0.15) O4 - C33 O5 - Distance Angles C33 1.2179 (0.0031) O5 - O6 - Distance Angles C34 1.4258 (0.0029) O6 - C1 - Distance Angles C6 1.3839 (0.0040) C2 1.3882 (0.0037) 120.60 (0.26) Sb1 2.1001 (0.0026) 115.85 (0.21) 123.15 (0.19) C1 - C6 C2 C2 - Distance Angles C3 1.3840 (0.0039) C1 1.3882 (0.0037) 118.96 (0.26) C2 - C3 C3 - Distance Angles C4 1.3838 (0.0046) C2 1.3840 (0.0039) 120.35 (0.29) C3 - C4 C4 - Distance Angles C5 1.3773 (0.0050) C3 1.3838 (0.0045) 120.12 (0.29) C4 - C5 C5 - Distance Angles C6 1.3755 (0.0045) C4 1.3773 (0.0050) 120.16 (0.31) C5 - C6 C6 - Distance Angles C5 1.3755 (0.0045) C1 1.3839 (0.0040) 119.80 (0.30) C6 - C5 C7 - Distance Angles C8 1.3858 (0.0037) C12 1.3953 (0.0038) 120.62 (0.24) Sb1 2.1091 (0.0025) 123.63 (0.19) 115.51 (0.19) C7 - C8 C12 C8 - Distance Angles C9 1.3817 (0.0038) C7 1.3858 (0.0037) 118.60 (0.26) C8 - C9 C9 - Distance Angles C8 1.3817 (0.0038) C10 1.3838 (0.0044) 120.99 (0.28) C9 - C8 C10 - Distance Angles C11 1.3789 (0.0046) C9 1.3838 (0.0044) 120.12 (0.27) C10 - C11 C11 - Distance Angles C10 1.3789 (0.0046) C12 1.3790 (0.0042) 119.78 (0.29) C11 - C10 C12 - Distance Angles C11 1.3790 (0.0041) C7 1.3953 (0.0038) 119.82 (0.28) C12 - C11 C13 - Distance Angles C18 1.3892 (0.0037) C14 1.3953 (0.0036) 119.13 (0.23) Sb1 2.1091 (0.0025) 120.80 (0.20) 119.65 (0.18) C13 - C18 C14 C14 - Distance Angles C15 1.3853 (0.0037) C13 1.3953 (0.0036) 119.86 (0.25) C14 - C15 C15 - Distance Angles C16 1.3708 (0.0040) C14 1.3853 (0.0037) 120.86 (0.27) C15 - C16 C16 - Distance Angles C15 1.3708 (0.0040) C17 1.3786 (0.0042) 119.41 (0.25) C16 - C15 C17 - Distance Angles C16 1.3786 (0.0042) C18 1.3839 (0.0040) 120.85 (0.26) C17 - C16 C18 - Distance Angles C17 1.3839 (0.0040) C13 1.3892 (0.0037) 119.90 (0.27) C18 - C17 C19 - Distance Angles O2 1.2277 (0.0032) O1 1.2993 (0.0029) 123.75 (0.23) C20 1.5397 (0.0035) 120.26 (0.22) 115.98 (0.22) C19 - O2 O1 C20 - Distance Angles O3 1.4345 (0.0031) C27 1.5245 (0.0035) 109.09 (0.20) C21 1.5310 (0.0037) 107.07 (0.21) 114.62 (0.22) C19 1.5397 (0.0035) 107.71 (0.21) 109.91 (0.20) 108.20 (0.20) C20 - O3 C27 C21 C21 - Distance Angles C26 1.3781 (0.0039) C22 1.3851 (0.0041) 119.06 (0.26) C20 1.5310 (0.0037) 119.04 (0.26) 121.79 (0.24) C21 - C26 C22 C22 - Distance Angles C21 1.3851 (0.0041) C23 1.4002 (0.0040) 119.55 (0.28) C22 - C21 C23 - Distance Angles C24 1.3642 (0.0045) C22 1.4002 (0.0040) 120.70 (0.31) C23 - C24 C24 - Distance Angles C23 1.3642 (0.0045) C25 1.3769 (0.0052) 119.75 (0.29) C24 - C23 C25 - Distance Angles C24 1.3769 (0.0052) C26 1.3830 (0.0046) 119.98 (0.32) C25 - C24 C26 - Distance Angles C21 1.3781 (0.0039) C25 1.3830 (0.0046) 120.95 (0.32) C26 - C21 C27 - Distance Angles C32 1.3846 (0.0037) C28 1.3958 (0.0037) 118.08 (0.25) C20 1.5245 (0.0035) 124.07 (0.23) 117.65 (0.24) C27 - C32 C28 C28 - Distance Angles C29 1.3843 (0.0042) C27 1.3958 (0.0037) 120.60 (0.28) C28 - C29 C29 - Distance Angles C30 1.3824 (0.0045) C28 1.3843 (0.0042) 119.95 (0.27) C29 - C30 C30 - Distance Angles C31 1.3682 (0.0043) C29 1.3824 (0.0045) 120.05 (0.27) C30 - C31 C31 - Distance Angles C30 1.3682 (0.0043) C32 1.3824 (0.0038) 120.02 (0.28) C31 - C30 C32 - Distance Angles C31 1.3824 (0.0038) C27 1.3846 (0.0037) 121.24 (0.26) C32 - C31 C33 - Distance Angles O5 1.2179 (0.0031) O4 1.3096 (0.0030) 123.66 (0.22) C34 1.5476 (0.0035) 121.05 (0.22) 115.26 (0.21) C33 - O5 O4 C34 - Distance Angles O6 1.4258 (0.0029) C35 1.5210 (0.0033) 107.22 (0.19) C41 1.5315 (0.0033) 111.80 (0.20) 112.09 (0.20) C33 1.5476 (0.0035) 107.12 (0.19) 111.04 (0.20) 107.49 (0.19) C34 - O6 C35 C41 C35 - Distance Angles C40 1.3853 (0.0035) C36 1.3976 (0.0036) 118.62 (0.23) C34 1.5210 (0.0033) 122.90 (0.22) 118.47 (0.23) C35 - C40 C36 C36 - Distance Angles C37 1.3811 (0.0037) C35 1.3976 (0.0036) 120.59 (0.25) C36 - C37 C37 - Distance Angles C36 1.3811 (0.0037) C38 1.3839 (0.0040) 120.15 (0.26) C37 - C36 C38 - Distance Angles C39 1.3770 (0.0039) C37 1.3839 (0.0040) 119.92 (0.25) C38 - C39 C39 - Distance Angles C38 1.3770 (0.0039) C40 1.3918 (0.0036) 120.05 (0.26) C39 - C38 C40 - Distance Angles C35 1.3853 (0.0035) C39 1.3918 (0.0036) 120.64 (0.25) C40 - C35 C41 - Distance Angles C42 1.3856 (0.0035) C46 1.3872 (0.0037) 118.63 (0.24) C34 1.5315 (0.0033) 120.75 (0.22) 120.52 (0.23) C41 - C42 C46 C42 - Distance Angles C43 1.3839 (0.0035) C41 1.3856 (0.0036) 120.75 (0.25) C42 - C43 C43 - Distance Angles C44 1.3750 (0.0042) C42 1.3839 (0.0035) 120.23 (0.26) C43 - C44 C44 - Distance Angles C43 1.3750 (0.0042) C45 1.3757 (0.0044) 119.65 (0.26) C44 - C43 C45 - Distance Angles C44 1.3757 (0.0044) C46 1.3878 (0.0043) 120.39 (0.28) C45 - C44 C46 - Distance Angles C41 1.3872 (0.0037) C45 1.3878 (0.0043) 120.35 (0.27) C46 - C41 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)