+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + s92 started at 10:11:20 on 03-Aug-2004 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 00SRC426 in P-1 CELL 0.71073 10.3490 12.0808 15.0992 91.005 103.075 90.718 ZERR 4.00 0.0021 0.0024 0.0030 0.030 0.030 0.030 LATT 1 SFAC C H O S UNIT 76 64 12 12 V = 1838.28 F(000) = 808.0 Mu = 0.42 mm-1 Cell Wt = 1553.99 Rho = 1.404 FMAP 2 PLAN 20 BOND L.S. 4 OMIT -3 55 OMIT -2 4 2 OMIT -1 -1 2 OMIT -3 -2 5 OMIT 5 0 1 OMIT 3 5 1 OMIT -1 3 0 SIZE 0.2 0.1 0.1 TEMP -123 WGHT 0.0460 0.5015 EXTI 0.003229 FVAR 0.38498 C1 1 0.830875 0.357659 0.401306 11.00000 0.05030 0.02518 = 0.02572 -0.00241 0.01203 0.00013 C2 1 0.880644 0.538846 0.329024 11.00000 0.03445 0.02501 = 0.03082 0.00025 0.01172 0.00172 C3 1 0.998558 0.498025 0.365634 11.00000 0.03661 0.02458 = 0.02877 0.00182 0.01483 0.00610 C4 1 0.894808 0.645872 0.282172 11.00000 0.02627 0.02890 = 0.03541 0.00386 0.00865 0.00105 AFIX 13 H4 2 0.852317 0.637034 0.215976 11.00000 -1.20000 AFIX 0 C5 1 1.108634 0.571119 0.346006 11.00000 0.02873 0.02693 = 0.03539 0.00243 0.01070 0.00468 AFIX 13 H5 2 1.165069 0.602338 0.403927 11.00000 -1.20000 AFIX 0 C6 1 0.839109 0.745903 0.320304 11.00000 0.02742 0.02430 = 0.02873 0.00614 0.00559 0.00318 C7 1 0.918144 0.831144 0.366013 11.00000 0.02506 0.03380 = 0.03942 0.00222 0.00123 0.00102 AFIX 43 H7 2 1.011907 0.825943 0.376768 11.00000 -1.20000 AFIX 0 C8 1 0.862814 0.924252 0.396480 11.00000 0.04244 0.03165 = 0.04006 -0.00510 -0.00031 -0.00012 AFIX 43 H8 2 0.918352 0.982714 0.427248 11.00000 -1.20000 AFIX 0 C9 1 0.727232 0.931597 0.381968 11.00000 0.04444 0.03172 = 0.03419 0.00061 0.00937 0.01005 AFIX 43 H9 2 0.689277 0.995694 0.402345 11.00000 -1.20000 AFIX 0 C10 1 0.645322 0.846219 0.337819 11.00000 0.02618 0.03347 = 0.04018 0.01094 0.01048 0.00764 AFIX 43 H10 2 0.551729 0.850620 0.329223 11.00000 -1.20000 AFIX 0 C11 1 0.701751 0.754702 0.306528 11.00000 0.02589 0.02394 = 0.03078 0.00664 0.00366 -0.00039 C12 1 0.491364 0.663610 0.251026 11.00000 0.02778 0.04193 = 0.07220 0.01789 -0.00377 -0.00711 AFIX 137 H12A 2 0.470466 0.667216 0.311146 11.00000 -1.50000 H12B 2 0.454359 0.594839 0.219392 11.00000 -1.50000 H12C 2 0.452779 0.727124 0.215553 11.00000 -1.50000 AFIX 0 C13 1 1.192769 0.511103 0.291951 11.00000 0.02604 0.02380 = 0.03281 -0.00379 0.00890 -0.00139 C14 1 1.177138 0.522170 0.199704 11.00000 0.02852 0.03137 = 0.03382 0.00110 0.00747 -0.00755 AFIX 43 H14 2 1.116109 0.574252 0.168501 11.00000 -1.20000 AFIX 0 C15 1 1.249236 0.458354 0.151741 11.00000 0.04791 0.04395 = 0.03493 -0.00946 0.02232 -0.01633 AFIX 43 H15 2 1.236930 0.465889 0.087866 11.00000 -1.20000 AFIX 0 C16 1 1.338667 0.384080 0.197025 11.00000 0.05295 0.03389 = 0.06260 -0.00712 0.03952 -0.00248 AFIX 43 H16 2 1.386900 0.339453 0.163775 11.00000 -1.20000 AFIX 0 C17 1 1.359697 0.373131 0.289938 11.00000 0.04059 0.03103 = 0.06517 0.00544 0.02670 0.01019 AFIX 43 H17 2 1.423496 0.322895 0.320835 11.00000 -1.20000 AFIX 0 C18 1 1.286532 0.436368 0.337477 11.00000 0.03735 0.03243 = 0.03685 0.00239 0.01403 0.00678 C19 1 1.383117 0.351809 0.478389 11.00000 0.10446 0.10140 = 0.05867 0.03868 0.02245 0.06433 AFIX 137 H19A 2 1.356320 0.277251 0.453921 11.00000 -1.50000 H19B 2 1.380176 0.355789 0.542783 11.00000 -1.50000 H19C 2 1.473604 0.368203 0.472208 11.00000 -1.50000 AFIX 0 C20 1 0.699705 0.849370 0.080894 11.00000 0.04033 0.02903 = 0.02463 0.00327 0.00869 0.00422 C21 1 0.546527 0.993262 0.128574 11.00000 0.03091 0.02392 = 0.02447 0.00352 0.00848 0.00000 C22 1 0.667824 1.037459 0.153381 11.00000 0.03214 0.02382 = 0.02427 0.00293 0.00846 0.00198 C23 1 0.446625 1.069283 0.156110 11.00000 0.02739 0.02540 = 0.03086 0.00285 0.00866 -0.00032 AFIX 13 H23 2 0.375647 1.087078 0.101591 11.00000 -1.20000 AFIX 0 C24 1 0.664533 1.149203 0.198451 11.00000 0.03125 0.02404 = 0.02998 -0.00064 0.00967 0.00122 AFIX 13 H24 2 0.707691 1.144599 0.264567 11.00000 -1.20000 AFIX 0 C25 1 0.384937 1.022142 0.229159 11.00000 0.02513 0.02414 = 0.03001 0.00653 0.00883 0.00667 C26 1 0.417334 1.061275 0.318002 11.00000 0.02709 0.03144 = 0.03412 0.00370 0.00997 0.00697 AFIX 43 H26 2 0.477989 1.121888 0.334095 11.00000 -1.20000 AFIX 0 C27 1 0.362674 1.013410 0.383755 11.00000 0.03603 0.05323 = 0.03156 0.00838 0.01203 0.00830 AFIX 43 H27 2 0.385193 1.041007 0.444699 11.00000 -1.20000 AFIX 0 C28 1 0.275017 0.925101 0.360114 11.00000 0.03800 0.06075 = 0.04555 0.02567 0.02095 0.00900 AFIX 43 H28 2 0.239047 0.891060 0.405658 11.00000 -1.20000 AFIX 0 C29 1 0.238439 0.885109 0.271248 11.00000 0.02963 0.03564 = 0.05384 0.01365 0.01354 -0.00173 AFIX 43 H29 2 0.176766 0.825157 0.255372 11.00000 -1.20000 AFIX 0 C30 1 0.293731 0.934426 0.206100 11.00000 0.02711 0.02818 = 0.03642 0.00624 0.00965 0.00294 C31 1 0.171327 0.817447 0.084796 11.00000 0.04955 0.06062 = 0.06491 -0.01326 0.00392 -0.02482 AFIX 137 H31A 2 0.200297 0.749741 0.117822 11.00000 -1.50000 H31B 2 0.162685 0.803864 0.019522 11.00000 -1.50000 H31C 2 0.085386 0.839297 0.095881 11.00000 -1.50000 AFIX 0 C32 1 0.726609 1.243138 0.157926 11.00000 0.02959 0.02457 = 0.03011 -0.00413 0.00830 -0.00248 C33 1 0.652514 1.324762 0.107145 11.00000 0.03092 0.03125 = 0.03416 0.00094 0.00985 -0.00300 AFIX 43 H33 2 0.558364 1.320578 0.094330 11.00000 -1.20000 AFIX 0 C34 1 0.715655 1.412609 0.074983 11.00000 0.04559 0.03269 = 0.04591 0.00927 0.01014 -0.00581 AFIX 43 H34 2 0.664936 1.469058 0.041060 11.00000 -1.20000 AFIX 0 C35 1 0.851600 1.417297 0.092520 11.00000 0.04375 0.03610 = 0.05945 0.00387 0.01465 -0.01706 AFIX 43 H35 2 0.894409 1.477986 0.071172 11.00000 -1.20000 AFIX 0 C36 1 0.927433 1.335448 0.140630 11.00000 0.03164 0.03740 = 0.05933 -0.00843 0.00931 -0.01173 AFIX 43 H36 2 1.021434 1.338337 0.150820 11.00000 -1.20000 AFIX 0 C37 1 0.863912 1.248899 0.173830 11.00000 0.03097 0.02582 = 0.04243 -0.00881 0.00437 -0.00406 C38 1 1.069337 1.160479 0.237339 11.00000 0.03109 0.05786 = 0.09471 -0.01050 -0.00385 0.00994 AFIX 137 H38A 2 1.093820 1.154338 0.178451 11.00000 -1.50000 H38B 2 1.102504 1.096397 0.274075 11.00000 -1.50000 H38C 2 1.108497 1.228525 0.269146 11.00000 -1.50000 AFIX 0 O1 3 1.036384 0.657393 0.293376 11.00000 0.02892 0.02950 = 0.06137 0.01342 0.02016 0.00775 O2 3 0.631794 0.666013 0.261193 11.00000 0.02621 0.02615 = 0.05989 0.00290 -0.00013 -0.00225 O3 3 1.294163 0.431152 0.428974 11.00000 0.05337 0.05539 = 0.03854 0.01384 0.01173 0.02442 O4 3 0.524865 1.166569 0.188262 11.00000 0.03367 0.02177 = 0.05034 0.00142 0.02061 -0.00029 O5 3 0.266830 0.903967 0.115603 11.00000 0.03754 0.04231 = 0.04167 -0.00522 0.00885 -0.01043 O6 3 0.928237 1.163652 0.223266 11.00000 0.02891 0.03611 = 0.06341 -0.00222 -0.00295 0.00410 S1 4 0.755451 0.252113 0.437910 11.00000 0.06344 0.03104 = 0.03779 0.00331 0.01345 -0.00965 S2 4 0.742772 0.464034 0.340870 11.00000 0.03507 0.02567 = 0.03785 0.00173 0.01056 -0.00223 S3 4 1.001824 0.374157 0.420937 11.00000 0.04590 0.02716 = 0.03130 0.00518 0.01353 0.00781 S4 4 0.761092 0.740537 0.038536 11.00000 0.06094 0.03380 = 0.04220 -0.00647 0.01290 0.01255 S5 4 0.797270 0.960965 0.132194 11.00000 0.03146 0.02759 = 0.03689 -0.00036 0.00927 0.00509 S6 4 0.531741 0.863985 0.076892 11.00000 0.03943 0.02647 = 0.02668 -0.00144 0.00776 -0.00293 HKLF 4 Covalent radii and connectivity table for 00SRC426 in P-1 C 0.770 H 0.320 O 0.660 S 1.030 C1 - S1 S3 S2 C2 - C3 C4 S2 C3 - C2 C5 S3 C4 - O1 C6 C2 C5 - O1 C13 C3 C6 - C7 C11 C4 C7 - C6 C8 C8 - C9 C7 C9 - C8 C10 C10 - C11 C9 C11 - O2 C10 C6 C12 - O2 C13 - C14 C18 C5 C14 - C13 C15 C15 - C16 C14 C16 - C15 C17 C17 - C16 C18 C18 - O3 C17 C13 C19 - O3 C20 - S4 S5 S6 C21 - C22 C23 S6 C22 - C21 C24 S5 C23 - O4 C25 C21 C24 - O4 C32 C22 C25 - C26 C30 C23 C26 - C25 C27 C27 - C28 C26 C28 - C27 C29 C29 - C30 C28 C30 - O5 C29 C25 C31 - O5 C32 - C37 C33 C24 C33 - C32 C34 C34 - C35 C33 C35 - C34 C36 C36 - C35 C37 C37 - O6 C32 C36 C38 - O6 O1 - C5 C4 O2 - C11 C12 O3 - C18 C19 O4 - C23 C24 O5 - C30 C31 O6 - C37 C38 S1 - C1 S2 - C2 C1 S3 - C3 C1 S4 - C20 S5 - C22 C20 S6 - C21 C20 27385 Reflections read, of which 27 rejected -13 =< h =< 13, -15 =< k =< 15, -19 =< l =< 19, Max. 2-theta = 54.97 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -7 2 0 215.44 5.22 4 28.04 3 2 0 176.31 1.28 6 20.44 5 -1 1 186.13 0.54 5 48.80 -7 2 1 57.35 1.57 4 8.18 -4 0 2 433.58 6.79 6 35.21 5 0 2 99.05 1.34 6 9.45 -5 1 2 276.93 0.54 6 95.11 -7 2 2 84.46 0.53 5 20.61 -5 -2 3 35.75 0.51 3 13.87 8 -2 3 73.69 0.91 4 18.18 -5 -1 3 15.24 0.46 4 2.34 -5 0 3 195.78 0.43 7 44.38 -6 1 3 32.74 0.47 6 4.66 7 4 3 51.54 2.46 3 14.63 -7 -4 4 42.43 0.71 4 11.61 -6 -2 4 93.30 0.54 4 40.14 -6 0 4 77.89 1.87 4 10.92 7 0 4 58.49 0.53 5 13.81 -7 1 4 46.47 0.59 5 8.89 7 1 4 210.45 5.76 4 31.31 -9 2 5 17.87 0.67 5 3.60 -10 3 5 23.98 0.90 4 6.75 -8 -1 6 94.70 0.75 4 44.37 -9 -3 7 31.42 0.92 3 16.34 -9 -1 7 19.74 0.80 4 5.81 25 Inconsistent equivalents 8248 Unique reflections, of which 0 suppressed R(int) = 0.0490 R(sigma) = 0.0542 Friedel opposites merged Maximum memory for data reduction = 3739 / 82385 Default effective X-H distances for T = -123.0 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 = 4969 / 594135 wR2 = 0.1039 before cycle 1 for 8248 data and 456 / 456 parameters GooF = S = 1.022; Restrained GooF = 1.022 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0460 * P )^2 + 0.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38491 0.00055 -0.135 OSF 2 0.00318 0.00092 -0.048 EXTI Mean shift/esd = 0.044 Maximum = -0.414 for y C31 Max. shift = 0.005 A for H31B Max. dU = 0.000 for C36 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4969 / 594135 wR2 = 0.1039 before cycle 2 for 8248 data and 456 / 456 parameters GooF = S = 1.021; Restrained GooF = 1.021 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0460 * P )^2 + 0.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38487 0.00055 -0.057 OSF 2 0.00317 0.00092 -0.019 EXTI Mean shift/esd = 0.015 Maximum = -0.142 for y C31 Max. shift = 0.002 A for H31B Max. dU = 0.000 for C36 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4969 / 594135 wR2 = 0.1038 before cycle 3 for 8248 data and 456 / 456 parameters GooF = S = 1.021; Restrained GooF = 1.021 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0460 * P )^2 + 0.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38487 0.00055 -0.002 OSF 2 0.00317 0.00092 -0.001 EXTI Mean shift/esd = 0.001 Maximum = 0.012 for tors H31A Max. shift = 0.000 A for H31B Max. dU = 0.000 for O3 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4969 / 594135 wR2 = 0.1039 before cycle 4 for 8248 data and 456 / 456 parameters GooF = S = 1.021; Restrained GooF = 1.021 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0460 * P )^2 + 0.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.38487 0.00055 0.001 OSF 2 0.00317 0.00092 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.002 for tors H31A Max. shift = 0.000 A for H31C Max. dU = 0.000 for C19 Largest correlation matrix elements 0.544 U13 C16 / U11 C16 0.522 U13 C16 / U33 C16 0.535 EXTI / OSF 0.518 U12 C19 / U11 C19 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H4 0.8523 0.6370 0.2160 13 1.000 0.000 C4 O1 C6 C2 H5 1.1650 0.6024 0.4039 13 1.000 0.000 C5 O1 C13 C3 H7 1.0119 0.8260 0.3768 43 0.950 0.000 C7 C6 C8 H8 0.9183 0.9828 0.4272 43 0.950 0.000 C8 C9 C7 H9 0.6893 0.9956 0.4024 43 0.950 0.000 C9 C8 C10 H10 0.5517 0.8507 0.3292 43 0.950 0.000 C10 C11 C9 H12A 0.4705 0.6673 0.3111 137 0.980 0.000 C12 O2 H12A H12B 0.4543 0.5948 0.2195 137 0.980 0.000 C12 O2 H12A H12C 0.4528 0.7271 0.2155 137 0.980 0.000 C12 O2 H12A H14 1.1161 0.5742 0.1685 43 0.950 0.000 C14 C13 C15 H15 1.2369 0.4658 0.0879 43 0.950 0.000 C15 C16 C14 H16 1.3869 0.3395 0.1638 43 0.950 0.000 C16 C15 C17 H17 1.4235 0.3230 0.3208 43 0.950 0.000 C17 C16 C18 H19A 1.3564 0.2774 0.4540 137 0.980 0.000 C19 O3 H19A H19B 1.3801 0.3560 0.5428 137 0.980 0.000 C19 O3 H19A H19C 1.4736 0.3684 0.4723 137 0.980 0.000 C19 O3 H19A H23 0.3756 1.0871 0.1016 13 1.000 0.000 C23 O4 C25 C21 H24 0.7077 1.1446 0.2646 13 1.000 0.000 C24 O4 C32 C22 H26 0.4780 1.1219 0.3341 43 0.950 0.000 C26 C25 C27 H27 0.3851 1.0411 0.4447 43 0.950 0.000 C27 C28 C26 H28 0.2391 0.8910 0.4057 43 0.950 0.000 C28 C27 C29 H29 0.1768 0.8251 0.2554 43 0.950 0.000 C29 C30 C28 H31A 0.2002 0.7498 0.1181 137 0.980 0.000 C31 O5 H31A H31B 0.1632 0.8034 0.0196 137 0.980 0.000 C31 O5 H31A H31C 0.0853 0.8393 0.0955 137 0.980 0.000 C31 O5 H31A H33 0.5584 1.3205 0.0943 43 0.950 0.000 C33 C32 C34 H34 0.6649 1.4691 0.0411 43 0.950 0.000 C34 C35 C33 H35 0.8945 1.4779 0.0712 43 0.950 0.000 C35 C34 C36 H36 1.0215 1.3383 0.1508 43 0.950 0.000 C36 C35 C37 H38A 1.0938 1.1539 0.1785 137 0.980 0.000 C38 O6 H38A H38B 1.1025 1.0965 0.2743 137 0.980 0.000 C38 O6 H38A H38C 1.1085 1.2286 0.2689 137 0.980 0.000 C38 O6 H38A 00SRC426 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.83090 0.35761 0.40131 1.00000 0.05030 0.02514 0.02568 -0.00240 0.01203 0.00014 0.03320 0.00385 0.00021 0.00017 0.00013 0.00000 0.00131 0.00106 0.00105 0.00083 0.00089 0.00088 0.00047 C2 0.88063 0.53889 0.32902 1.00000 0.03440 0.02497 0.03082 0.00025 0.01172 0.00172 0.02937 0.00375 0.00019 0.00016 0.00013 0.00000 0.00112 0.00103 0.00108 0.00083 0.00083 0.00081 0.00043 C3 0.99856 0.49802 0.36563 1.00000 0.03656 0.02468 0.02873 0.00182 0.01483 0.00602 0.02874 0.00381 0.00019 0.00016 0.00013 0.00000 0.00114 0.00102 0.00105 0.00081 0.00083 0.00081 0.00043 C4 0.89482 0.64585 0.28217 1.00000 0.02629 0.02878 0.03539 0.00388 0.00866 0.00111 0.02984 0.00384 0.00019 0.00016 0.00014 0.00000 0.00105 0.00107 0.00112 0.00086 0.00080 0.00079 0.00043 H4 0.85233 0.63701 0.21597 1.00000 0.03581 0.00000 0.00000 C5 1.10862 0.57114 0.34600 1.00000 0.02869 0.02698 0.03537 0.00241 0.01070 0.00464 0.02974 0.00391 0.00019 0.00016 0.00014 0.00000 0.00107 0.00106 0.00112 0.00085 0.00082 0.00079 0.00044 H5 1.16505 0.60237 0.40392 1.00000 0.03569 0.00000 0.00000 C6 0.83912 0.74587 0.32030 1.00000 0.02739 0.02433 0.02869 0.00613 0.00559 0.00315 0.02684 0.00362 0.00018 0.00015 0.00013 0.00000 0.00105 0.00101 0.00103 0.00080 0.00076 0.00076 0.00041 C7 0.91814 0.83117 0.36601 1.00000 0.02502 0.03389 0.03937 0.00222 0.00121 0.00093 0.03370 0.00384 0.00020 0.00017 0.00014 0.00000 0.00107 0.00117 0.00121 0.00093 0.00083 0.00083 0.00047 H7 1.01191 0.82599 0.37676 1.00000 0.04044 0.00000 0.00000 C8 0.86279 0.92429 0.39648 1.00000 0.04242 0.03151 0.04008 -0.00513 -0.00031 -0.00005 0.03962 0.00404 0.00022 0.00018 0.00015 0.00000 0.00133 0.00119 0.00128 0.00097 0.00095 0.00093 0.00052 H8 0.91831 0.98277 0.42723 1.00000 0.04754 0.00000 0.00000 C9 0.72724 0.93157 0.38197 1.00000 0.04445 0.03158 0.03420 0.00062 0.00937 0.01010 0.03659 0.00410 0.00021 0.00018 0.00014 0.00000 0.00132 0.00117 0.00117 0.00092 0.00092 0.00093 0.00049 H9 0.68928 0.99565 0.40237 1.00000 0.04391 0.00000 0.00000 C10 0.64531 0.84625 0.33782 1.00000 0.02620 0.03333 0.04019 0.01094 0.01052 0.00771 0.03258 0.00413 0.00020 0.00017 0.00014 0.00000 0.00106 0.00115 0.00119 0.00092 0.00084 0.00083 0.00046 H10 0.55171 0.85068 0.32922 1.00000 0.03910 0.00000 0.00000 C11 0.70175 0.75472 0.30653 1.00000 0.02585 0.02403 0.03072 0.00665 0.00365 -0.00045 0.02724 0.00358 0.00018 0.00015 0.00013 0.00000 0.00104 0.00101 0.00106 0.00081 0.00077 0.00076 0.00042 C12 0.49136 0.66361 0.25102 1.00000 0.02775 0.04210 0.07213 0.01792 -0.00380 -0.00721 0.04960 0.00445 0.00021 0.00020 0.00018 0.00000 0.00125 0.00138 0.00173 0.00123 0.00106 0.00096 0.00063 H12A 0.47046 0.66733 0.31114 1.00000 0.07439 0.00000 0.00000 H12B 0.45435 0.59480 0.21946 1.00000 0.07439 0.00000 0.00000 H12C 0.45277 0.72708 0.21548 1.00000 0.07439 0.00000 0.00000 C13 1.19279 0.51107 0.29196 1.00000 0.02600 0.02386 0.03278 -0.00380 0.00890 -0.00141 0.02726 0.00355 0.00018 0.00016 0.00013 0.00000 0.00102 0.00101 0.00109 0.00081 0.00078 0.00076 0.00042 C14 1.17715 0.52215 0.19970 1.00000 0.02850 0.03143 0.03377 0.00111 0.00747 -0.00759 0.03123 0.00361 0.00019 0.00017 0.00013 0.00000 0.00109 0.00112 0.00114 0.00088 0.00082 0.00082 0.00045 H14 1.11613 0.57423 0.16850 1.00000 0.03748 0.00000 0.00000 C15 1.24926 0.45830 0.15175 1.00000 0.04789 0.04374 0.03499 -0.00942 0.02232 -0.01620 0.04042 0.00410 0.00023 0.00019 0.00015 0.00000 0.00138 0.00136 0.00121 0.00102 0.00100 0.00106 0.00054 H15 1.23694 0.46580 0.08787 1.00000 0.04850 0.00000 0.00000 C16 1.33863 0.38414 0.19701 1.00000 0.05290 0.03380 0.06255 -0.00708 0.03947 -0.00244 0.04568 0.00470 0.00024 0.00019 0.00017 0.00000 0.00149 0.00126 0.00161 0.00113 0.00123 0.00106 0.00060 H16 1.38689 0.33952 0.16377 1.00000 0.05481 0.00000 0.00000 C17 1.35967 0.37319 0.28992 1.00000 0.04061 0.03099 0.06514 0.00546 0.02670 0.01018 0.04310 0.00474 0.00022 0.00018 0.00017 0.00000 0.00132 0.00120 0.00163 0.00108 0.00112 0.00094 0.00056 H17 1.42349 0.32297 0.32081 1.00000 0.05172 0.00000 0.00000 C18 1.28654 0.43636 0.33748 1.00000 0.03735 0.03229 0.03686 0.00242 0.01404 0.00681 0.03453 0.00415 0.00021 0.00017 0.00014 0.00000 0.00118 0.00116 0.00120 0.00092 0.00089 0.00089 0.00047 C19 1.38313 0.35197 0.47842 1.00000 0.10429 0.10156 0.05865 0.03866 0.02246 0.06422 0.08655 0.00767 0.00035 0.00030 0.00020 0.00000 0.00260 0.00266 0.00189 0.00182 0.00169 0.00216 0.00114 H19A 1.35644 0.27738 0.45397 1.00000 0.12983 0.00000 0.00000 H19B 1.38012 0.35597 0.54280 1.00000 0.12983 0.00000 0.00000 H19C 1.47361 0.36844 0.47227 1.00000 0.12983 0.00000 0.00000 C20 0.69969 0.84941 0.08089 1.00000 0.04033 0.02895 0.02462 0.00327 0.00868 0.00425 0.03102 0.00383 0.00020 0.00017 0.00013 0.00000 0.00120 0.00109 0.00102 0.00083 0.00083 0.00085 0.00045 C21 0.54653 0.99325 0.12857 1.00000 0.03088 0.02398 0.02443 0.00352 0.00849 -0.00004 0.02605 0.00357 0.00019 0.00015 0.00012 0.00000 0.00108 0.00100 0.00099 0.00078 0.00076 0.00078 0.00041 C22 0.66783 1.03745 0.15339 1.00000 0.03211 0.02387 0.02423 0.00291 0.00845 0.00190 0.02637 0.00360 0.00019 0.00015 0.00012 0.00000 0.00110 0.00100 0.00098 0.00077 0.00076 0.00078 0.00041 C23 0.44660 1.06932 0.15610 1.00000 0.02738 0.02537 0.03083 0.00284 0.00868 -0.00033 0.02751 0.00367 0.00019 0.00015 0.00013 0.00000 0.00104 0.00103 0.00106 0.00082 0.00078 0.00077 0.00042 H23 0.37563 1.08713 0.10158 1.00000 0.03301 0.00000 0.00000 C24 0.66452 1.14924 0.19845 1.00000 0.03123 0.02398 0.02997 -0.00062 0.00967 0.00123 0.02797 0.00369 0.00019 0.00016 0.00013 0.00000 0.00108 0.00101 0.00106 0.00080 0.00079 0.00078 0.00042 H24 0.70767 1.14465 0.26457 1.00000 0.03356 0.00000 0.00000 C25 0.38491 1.02218 0.22915 1.00000 0.02511 0.02414 0.03000 0.00655 0.00884 0.00668 0.02588 0.00366 0.00018 0.00015 0.00013 0.00000 0.00101 0.00100 0.00105 0.00080 0.00076 0.00075 0.00041 C26 0.41732 1.06133 0.31800 1.00000 0.02711 0.03137 0.03410 0.00371 0.00995 0.00699 0.03029 0.00395 0.00019 0.00017 0.00013 0.00000 0.00106 0.00111 0.00113 0.00087 0.00081 0.00080 0.00044 H26 0.47798 1.12193 0.33409 1.00000 0.03634 0.00000 0.00000 C27 0.36264 1.01348 0.38375 1.00000 0.03599 0.05328 0.03152 0.00837 0.01202 0.00829 0.03941 0.00456 0.00021 0.00020 0.00015 0.00000 0.00123 0.00145 0.00116 0.00101 0.00090 0.00102 0.00052 H27 0.38511 1.04111 0.44469 1.00000 0.04730 0.00000 0.00000 C28 0.27502 0.92510 0.36012 1.00000 0.03791 0.06095 0.04552 0.02567 0.02095 0.00889 0.04594 0.00499 0.00022 0.00021 0.00016 0.00000 0.00132 0.00162 0.00140 0.00120 0.00102 0.00110 0.00060 H28 0.23908 0.89104 0.40567 1.00000 0.05512 0.00000 0.00000 C29 0.23845 0.88508 0.27125 1.00000 0.02959 0.03580 0.05374 0.01365 0.01353 -0.00181 0.03893 0.00443 0.00021 0.00018 0.00016 0.00000 0.00117 0.00125 0.00146 0.00105 0.00096 0.00089 0.00052 H29 0.17682 0.82510 0.25538 1.00000 0.04671 0.00000 0.00000 C30 0.29373 0.93444 0.20610 1.00000 0.02708 0.02831 0.03637 0.00623 0.00962 0.00285 0.03011 0.00385 0.00019 0.00016 0.00014 0.00000 0.00107 0.00108 0.00115 0.00087 0.00082 0.00079 0.00044 C31 0.17141 0.81732 0.08481 1.00000 0.04949 0.06067 0.06491 -0.01330 0.00398 -0.02487 0.06018 0.00438 0.00026 0.00023 0.00019 0.00000 0.00162 0.00177 0.00178 0.00139 0.00123 0.00128 0.00074 H31A 0.20018 0.74977 0.11813 1.00000 0.09027 0.00000 0.00000 H31B 0.16319 0.80340 0.01962 1.00000 0.09027 0.00000 0.00000 H31C 0.08531 0.83929 0.09554 1.00000 0.09027 0.00000 0.00000 C32 0.72661 1.24314 0.15792 1.00000 0.02958 0.02440 0.03012 -0.00410 0.00829 -0.00243 0.02787 0.00350 0.00019 0.00016 0.00013 0.00000 0.00109 0.00102 0.00106 0.00081 0.00079 0.00078 0.00042 C33 0.65255 1.32471 0.10715 1.00000 0.03089 0.03133 0.03410 0.00092 0.00985 -0.00306 0.03174 0.00384 0.00020 0.00017 0.00013 0.00000 0.00110 0.00112 0.00112 0.00089 0.00084 0.00084 0.00045 H33 0.55840 1.32048 0.09431 1.00000 0.03809 0.00000 0.00000 C34 0.71564 1.41264 0.07498 1.00000 0.04554 0.03281 0.04587 0.00929 0.01014 -0.00588 0.04139 0.00421 0.00023 0.00018 0.00015 0.00000 0.00141 0.00123 0.00135 0.00101 0.00100 0.00097 0.00053 H34 0.66492 1.46911 0.04109 1.00000 0.04967 0.00000 0.00000 C35 0.85163 1.41726 0.09252 1.00000 0.04374 0.03630 0.05938 0.00379 0.01466 -0.01722 0.04612 0.00436 0.00023 0.00019 0.00017 0.00000 0.00144 0.00131 0.00155 0.00113 0.00110 0.00103 0.00058 H35 0.89445 1.47793 0.07116 1.00000 0.05534 0.00000 0.00000 C36 0.92746 1.33542 0.14064 1.00000 0.03160 0.03718 0.05935 -0.00832 0.00926 -0.01160 0.04309 0.00408 0.00022 0.00019 0.00016 0.00000 0.00124 0.00130 0.00153 0.00112 0.00101 0.00096 0.00056 H36 1.02146 1.33829 0.15083 1.00000 0.05171 0.00000 0.00000 C37 0.86390 1.24893 0.17382 1.00000 0.03095 0.02571 0.04244 -0.00877 0.00437 -0.00398 0.03382 0.00366 0.00020 0.00017 0.00014 0.00000 0.00115 0.00108 0.00124 0.00091 0.00087 0.00084 0.00047 C38 1.06936 1.16041 0.23735 1.00000 0.03100 0.05803 0.09462 -0.01054 -0.00387 0.00987 0.06416 0.00500 0.00023 0.00024 0.00021 0.00000 0.00138 0.00175 0.00222 0.00155 0.00126 0.00115 0.00080 H38A 1.09382 1.15393 0.17847 1.00000 0.09624 0.00000 0.00000 H38B 1.10250 1.09649 0.27429 1.00000 0.09624 0.00000 0.00000 H38C 1.10855 1.22858 0.26893 1.00000 0.09624 0.00000 0.00000 O1 1.03638 0.65740 0.29338 1.00000 0.02891 0.02939 0.06136 0.01345 0.02014 0.00779 0.03810 0.00292 0.00013 0.00011 0.00010 0.00000 0.00079 0.00079 0.00100 0.00070 0.00067 0.00058 0.00036 O2 0.63181 0.66599 0.26119 1.00000 0.02619 0.02620 0.05983 0.00290 -0.00014 -0.00230 0.03898 0.00260 0.00013 0.00011 0.00011 0.00000 0.00079 0.00077 0.00101 0.00069 0.00064 0.00058 0.00036 O3 1.29416 0.43115 0.42897 1.00000 0.05340 0.05520 0.03851 0.01383 0.01173 0.02449 0.04847 0.00330 0.00016 0.00014 0.00010 0.00000 0.00101 0.00106 0.00090 0.00077 0.00072 0.00079 0.00042 O4 0.52486 1.16657 0.18826 1.00000 0.03364 0.02164 0.05034 0.00143 0.02060 -0.00025 0.03344 0.00267 0.00013 0.00011 0.00010 0.00000 0.00080 0.00072 0.00089 0.00062 0.00064 0.00056 0.00033 O5 0.26685 0.90395 0.11560 1.00000 0.03752 0.04243 0.04160 -0.00525 0.00884 -0.01052 0.04071 0.00264 0.00014 0.00012 0.00010 0.00000 0.00087 0.00092 0.00089 0.00071 0.00065 0.00067 0.00037 O6 0.92823 1.16367 0.22326 1.00000 0.02886 0.03616 0.06337 -0.00221 -0.00295 0.00405 0.04493 0.00276 0.00014 0.00013 0.00011 0.00000 0.00083 0.00088 0.00107 0.00076 0.00068 0.00064 0.00040 S1 0.75545 0.25211 0.43791 1.00000 0.06342 0.03099 0.03777 0.00330 0.01344 -0.00963 0.04380 0.00110 0.00006 0.00005 0.00004 0.00000 0.00040 0.00031 0.00032 0.00024 0.00027 0.00026 0.00016 S2 0.74277 0.46404 0.34087 1.00000 0.03504 0.02567 0.03782 0.00173 0.01054 -0.00225 0.03249 0.00097 0.00005 0.00004 0.00004 0.00000 0.00029 0.00027 0.00030 0.00021 0.00021 0.00020 0.00013 S3 1.00183 0.37415 0.42094 1.00000 0.04588 0.02713 0.03128 0.00518 0.01353 0.00781 0.03389 0.00104 0.00005 0.00004 0.00003 0.00000 0.00032 0.00028 0.00028 0.00021 0.00022 0.00022 0.00014 S4 0.76109 0.74054 0.03854 1.00000 0.06090 0.03381 0.04217 -0.00648 0.01289 0.01254 0.04542 0.00117 0.00006 0.00005 0.00004 0.00000 0.00040 0.00032 0.00034 0.00025 0.00027 0.00026 0.00016 S5 0.79727 0.96096 0.13219 1.00000 0.03144 0.02756 0.03688 -0.00036 0.00927 0.00510 0.03169 0.00098 0.00005 0.00004 0.00004 0.00000 0.00028 0.00028 0.00030 0.00021 0.00021 0.00020 0.00013 S6 0.53174 0.86398 0.07689 1.00000 0.03941 0.02644 0.02666 -0.00144 0.00775 -0.00292 0.03085 0.00092 0.00005 0.00004 0.00003 0.00000 0.00030 0.00027 0.00027 0.00020 0.00020 0.00020 0.00013 Final Structure Factor Calculation for 00SRC426 in P-1 Total number of l.s. parameters = 456 Maximum vector length = 511 Memory required = 4513 / 22995 wR2 = 0.1038 before cycle 5 for 8248 data and 0 / 456 parameters GooF = S = 1.021; Restrained GooF = 1.021 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0460 * P )^2 + 0.50 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0412 for 6108 Fo > 4sig(Fo) and 0.0651 for all 8248 data wR2 = 0.1038, GooF = S = 1.021, Restrained GooF = 1.021 for all data Occupancy sum of asymmetric unit = 50.00 for non-hydrogen and 32.00 for hydrogen atoms Principal mean square atomic displacements U 0.0503 0.0276 0.0217 C1 0.0365 0.0272 0.0244 C2 0.0411 0.0249 0.0203 C3 0.0367 0.0275 0.0254 C4 0.0370 0.0292 0.0231 C5 0.0324 0.0281 0.0200 C6 0.0436 0.0338 0.0238 C7 0.0545 0.0366 0.0277 C8 0.0495 0.0342 0.0261 C9 0.0480 0.0282 0.0215 C10 0.0361 0.0253 0.0203 C11 0.0897 0.0347 0.0244 C12 0.0350 0.0246 0.0221 C13 0.0386 0.0337 0.0214 C14 0.0680 0.0303 0.0230 C15 0.0812 0.0337 0.0222 C16 0.0704 0.0361 0.0228 C17 0.0439 0.0331 0.0266 C18 0.1663 0.0662 0.0272 C19 0.0413 0.0286 0.0231 C20 0.0312 0.0267 0.0202 C21 0.0326 0.0252 0.0214 C22 0.0319 0.0273 0.0233 C23 0.0329 0.0277 0.0233 C24 0.0353 0.0243 0.0180 C25 0.0383 0.0308 0.0218 C26 0.0575 0.0334 0.0273 C27 0.0799 0.0363 0.0216 C28 0.0601 0.0338 0.0228 C29 0.0393 0.0259 0.0251 C30 0.0825 0.0717 0.0263 C31 0.0339 0.0279 0.0218 C32 0.0357 0.0333 0.0263 C33 0.0531 0.0455 0.0255 C34 0.0600 0.0584 0.0200 C35 0.0630 0.0444 0.0220 C36 0.0479 0.0334 0.0201 C37 0.1100 0.0551 0.0274 C38 0.0667 0.0262 0.0214 O1 0.0657 0.0278 0.0233 O2 0.0781 0.0404 0.0270 O3 0.0538 0.0252 0.0213 O4 0.0526 0.0411 0.0284 O5 0.0727 0.0362 0.0259 O6 0.0668 0.0386 0.0260 S1 0.0387 0.0343 0.0244 S2 0.0490 0.0289 0.0238 S3 0.0660 0.0459 0.0243 S4 0.0370 0.0343 0.0238 S5 0.0404 0.0276 0.0245 S6 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.022 0.034 0.046 0.060 0.077 0.100 0.129 0.187 1.000 Number in group 825. 841. 873. 818. 776. 814. 842. 810. 823. 826. GooF 0.976 0.986 0.984 1.013 1.036 1.083 1.074 1.055 1.019 0.988 K 2.324 1.155 1.023 0.968 0.994 0.986 0.991 0.993 1.017 1.010 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.98 1.05 1.15 1.32 1.66 inf Number in group 833. 825. 823. 836. 814. 834. 810. 826. 817. 830. GooF 0.821 0.889 0.870 0.886 0.917 0.963 0.970 0.927 1.160 1.586 K 1.016 1.020 1.012 1.013 1.014 1.013 1.018 1.021 1.013 0.997 R1 0.180 0.175 0.127 0.087 0.072 0.064 0.045 0.033 0.033 0.032 Recommended weighting scheme: WGHT 0.0460 0.4967 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 -2 4 21.81 1.96 5.71 0.008 1.87 -4 7 4 54.80 14.85 5.69 0.023 1.39 -2 2 0 348.51 234.45 5.66 0.093 3.90 5 0 0 741.83 521.76 5.26 0.138 2.02 5 3 1 621.08 458.08 5.22 0.130 1.73 2 1 3 94.06 150.23 5.20 0.074 3.05 -3 2 3 11.32 0.03 5.08 0.001 2.77 -2 3 0 37.48 12.33 4.98 0.021 3.17 -2 6 1 247.50 172.84 4.76 0.080 1.88 -5 -1 4 248.44 179.02 4.53 0.081 1.94 4 2 3 108.48 71.58 4.48 0.051 1.94 -1 1 8 26.92 5.71 4.46 0.014 1.86 -6 -2 5 216.02 134.54 4.45 0.070 1.57 -2 -5 3 92.23 56.83 4.41 0.046 2.07 -3 3 2 34.61 15.80 4.38 0.024 2.59 2 5 0 24.09 1.72 4.38 0.008 2.16 2 -1 8 49.04 25.26 4.25 0.030 1.60 -1 1 2 1089.96 1374.06 4.24 0.224 5.84 -4 7 5 25.55 1.27 4.23 0.007 1.35 -2 1 1 21.59 9.49 4.17 0.019 4.74 -3 -10 3 40.54 9.08 4.03 0.018 1.13 -1 4 5 216.92 290.18 3.99 0.103 2.12 -3 6 0 24.63 5.03 3.97 0.014 1.74 -5 0 4 128.51 91.54 3.96 0.058 1.97 2 2 5 180.06 239.24 3.93 0.094 2.15 3 4 5 190.36 256.49 3.92 0.097 1.65 5 1 3 32.06 56.35 3.92 0.045 1.71 1 -5 1 13.31 0.81 3.90 0.005 2.32 -2 1 5 278.32 358.02 3.89 0.115 2.75 -6 -4 3 19.02 4.01 3.88 0.012 1.48 -1 2 2 386.59 302.08 3.83 0.105 4.47 -6 -3 7 20.13 5.51 3.81 0.014 1.39 1 2 3 45.94 27.87 3.75 0.032 3.33 1 5 1 357.37 278.82 3.74 0.101 2.29 2 5 3 36.38 18.11 3.70 0.026 1.90 0 -4 4 16.19 2.64 3.63 0.010 2.36 -2 4 6 460.40 366.95 3.61 0.116 1.88 -3 6 5 116.60 79.03 3.59 0.054 1.57 0 3 2 911.54 1110.83 3.52 0.202 3.50 3 4 3 26.45 46.09 3.52 0.041 1.91 -4 -2 2 37.11 58.54 3.49 0.046 2.36 1 1 1 6.56 1.59 3.46 0.008 6.34 -3 1 0 33.68 6.89 3.43 0.016 3.25 -6 1 1 406.91 315.93 3.41 0.108 1.70 -9 3 10 77.17 116.03 3.40 0.065 0.98 -3 2 6 104.46 74.12 3.39 0.052 2.09 -2 2 3 11.51 3.23 3.38 0.011 3.33 4 -1 5 452.80 367.26 3.37 0.116 1.72 -2 0 8 31.50 55.45 3.36 0.045 1.87 -4 3 9 12.12 0.03 3.36 0.001 1.43 Bond lengths and angles C1 - Distance Angles S1 1.6536 (0.0021) S3 1.7346 (0.0023) 124.05 (0.13) S2 1.7355 (0.0022) 121.82 (0.13) 114.12 (0.12) C1 - S1 S3 C2 - Distance Angles C3 1.3261 (0.0027) C4 1.5053 (0.0028) 110.85 (0.17) S2 1.7245 (0.0021) 117.38 (0.16) 131.77 (0.15) C2 - C3 C4 C3 - Distance Angles C2 1.3261 (0.0027) C5 1.5173 (0.0027) 110.72 (0.17) S3 1.7234 (0.0020) 117.40 (0.16) 131.82 (0.15) C3 - C2 C5 C4 - Distance Angles O1 1.4409 (0.0023) C6 1.5057 (0.0027) 110.88 (0.16) C2 1.5053 (0.0028) 102.74 (0.15) 115.25 (0.16) C4 - O1 C6 C5 - Distance Angles O1 1.4339 (0.0024) C13 1.5059 (0.0026) 110.44 (0.16) C3 1.5173 (0.0027) 102.48 (0.15) 112.41 (0.16) C5 - O1 C13 C6 - Distance Angles C7 1.3804 (0.0028) C11 1.3952 (0.0027) 118.40 (0.18) C4 1.5057 (0.0027) 122.76 (0.18) 118.81 (0.17) C6 - C7 C11 C7 - Distance Angles C6 1.3804 (0.0028) C8 1.3865 (0.0030) 121.03 (0.19) C7 - C6 C8 - Distance Angles C9 1.3742 (0.0031) C7 1.3865 (0.0030) 119.67 (0.20) C8 - C9 C9 - Distance Angles C8 1.3742 (0.0031) C10 1.3870 (0.0030) 120.64 (0.20) C9 - C8 C10 - Distance Angles C11 1.3821 (0.0028) C9 1.3870 (0.0030) 119.06 (0.19) C10 - C11 C11 - Distance Angles O2 1.3682 (0.0023) C10 1.3821 (0.0028) 124.64 (0.18) C6 1.3952 (0.0027) 114.18 (0.17) 121.18 (0.18) C11 - O2 C10 C12 - Distance Angles O2 1.4265 (0.0026) C12 - C13 - Distance Angles C14 1.3746 (0.0027) C18 1.4036 (0.0028) 118.86 (0.18) C5 1.5059 (0.0026) 122.90 (0.18) 118.16 (0.17) C13 - C14 C18 C14 - Distance Angles C13 1.3746 (0.0027) C15 1.3840 (0.0029) 120.77 (0.20) C14 - C13 C15 - Distance Angles C16 1.3716 (0.0035) C14 1.3840 (0.0029) 119.60 (0.21) C15 - C16 C16 - Distance Angles C15 1.3716 (0.0035) C17 1.3792 (0.0034) 121.16 (0.20) C16 - C15 C17 - Distance Angles C16 1.3792 (0.0034) C18 1.3827 (0.0028) 119.05 (0.21) C17 - C16 C18 - Distance Angles O3 1.3684 (0.0025) C17 1.3827 (0.0028) 125.14 (0.20) C13 1.4036 (0.0028) 114.34 (0.17) 120.50 (0.20) C18 - O3 C17 C19 - Distance Angles O3 1.4340 (0.0030) C19 - C20 - Distance Angles S4 1.6486 (0.0021) S5 1.7353 (0.0022) 122.87 (0.13) S6 1.7367 (0.0021) 123.25 (0.13) 113.88 (0.11) C20 - S4 S5 C21 - Distance Angles C22 1.3284 (0.0027) C23 1.5139 (0.0026) 110.36 (0.17) S6 1.7229 (0.0020) 117.04 (0.15) 132.56 (0.15) C21 - C22 C23 C22 - Distance Angles C21 1.3284 (0.0027) C24 1.5058 (0.0026) 110.68 (0.17) S5 1.7221 (0.0020) 117.61 (0.15) 131.69 (0.14) C22 - C21 C24 C23 - Distance Angles O4 1.4318 (0.0023) C25 1.5100 (0.0026) 111.30 (0.16) C21 1.5139 (0.0026) 102.54 (0.15) 113.18 (0.16) C23 - O4 C25 C24 - Distance Angles O4 1.4368 (0.0023) C32 1.5027 (0.0027) 110.34 (0.16) C22 1.5058 (0.0026) 102.67 (0.15) 115.68 (0.16) C24 - O4 C32 C25 - Distance Angles C26 1.3806 (0.0027) C30 1.3959 (0.0027) 118.99 (0.18) C23 1.5100 (0.0026) 122.39 (0.18) 118.61 (0.17) C25 - C26 C30 C26 - Distance Angles C25 1.3806 (0.0027) C27 1.3807 (0.0029) 120.81 (0.20) C26 - C25 C27 - Distance Angles C28 1.3804 (0.0034) C26 1.3807 (0.0029) 119.37 (0.21) C27 - C28 C28 - Distance Angles C27 1.3804 (0.0034) C29 1.3858 (0.0033) 121.30 (0.20) C28 - C27 C29 - Distance Angles C30 1.3846 (0.0029) C28 1.3858 (0.0033) 118.54 (0.21) C29 - C30 C30 - Distance Angles O5 1.3740 (0.0024) C29 1.3846 (0.0029) 125.07 (0.19) C25 1.3959 (0.0027) 113.97 (0.17) 120.97 (0.19) C30 - O5 C29 C31 - Distance Angles O5 1.4270 (0.0027) C31 - C32 - Distance Angles C37 1.3870 (0.0028) C33 1.3877 (0.0028) 119.10 (0.18) C24 1.5027 (0.0027) 118.12 (0.18) 122.77 (0.18) C32 - C37 C33 C33 - Distance Angles C32 1.3877 (0.0028) C34 1.3910 (0.0029) 120.25 (0.20) C33 - C32 C34 - Distance Angles C35 1.3721 (0.0032) C33 1.3910 (0.0029) 119.56 (0.22) C34 - C35 C35 - Distance Angles C34 1.3721 (0.0032) C36 1.3813 (0.0034) 121.28 (0.21) C35 - C34 C36 - Distance Angles C35 1.3813 (0.0034) C37 1.3878 (0.0031) 118.82 (0.21) C36 - C35 C37 - Distance Angles O6 1.3713 (0.0026) C32 1.3870 (0.0028) 114.81 (0.18) C36 1.3878 (0.0031) 124.24 (0.19) 120.94 (0.20) C37 - O6 C32 C38 - Distance Angles O6 1.4287 (0.0028) C38 - O1 - Distance Angles C5 1.4339 (0.0024) C4 1.4409 (0.0023) 113.13 (0.15) O1 - C5 O2 - Distance Angles C11 1.3682 (0.0023) C12 1.4265 (0.0026) 117.95 (0.17) O2 - C11 O3 - Distance Angles C18 1.3684 (0.0025) C19 1.4340 (0.0030) 116.93 (0.19) O3 - C18 O4 - Distance Angles C23 1.4318 (0.0023) C24 1.4368 (0.0023) 112.64 (0.14) O4 - C23 O5 - Distance Angles C30 1.3740 (0.0024) C31 1.4270 (0.0027) 118.14 (0.18) O5 - C30 O6 - Distance Angles C37 1.3713 (0.0026) C38 1.4287 (0.0028) 117.89 (0.19) O6 - C37 S1 - Distance Angles C1 1.6536 (0.0022) S1 - S2 - Distance Angles C2 1.7245 (0.0021) C1 1.7355 (0.0022) 95.53 (0.10) S2 - C2 S3 - Distance Angles C3 1.7234 (0.0020) C1 1.7346 (0.0023) 95.57 (0.10) S3 - C3 S4 - Distance Angles C20 1.6486 (0.0021) S4 - S5 - Distance Angles C22 1.7221 (0.0020) C20 1.7353 (0.0022) 95.62 (0.10) S5 - C22 S6 - Distance Angles C21 1.7229 (0.0020) C20 1.7367 (0.0021) 95.83 (0.10) S6 - C21 FMAP and GRID set by program FMAP 2 3 36 GRID -1.515 -2 -2 1.515 2 2 R1 = 0.0647 for 8248 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.32 at 0.5619 0.4047 0.0141 [ 1.30 A from H34 ] Deepest hole -0.35 at 0.7176 0.5206 0.3179 [ 0.79 A from S2 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 4174 / 32361 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5619 1.4047 0.0141 1.00000 0.05 0.32 1.30 H34 1.60 H33 1.65 C34 1.81 C33 Q2 1 0.9520 0.3382 0.3692 1.00000 0.05 0.26 0.93 S3 1.46 C1 1.99 C3 2.59 C2 Q3 1 1.0966 1.1628 0.1288 1.00000 0.05 0.25 0.77 H38A 1.73 C38 2.22 H38C 2.31 H36 Q4 1 0.6923 1.2534 0.1278 1.00000 0.05 0.24 0.53 C32 0.98 C33 1.60 H33 1.73 C24 Q5 1 0.4890 1.0217 0.1270 1.00000 0.05 0.24 0.69 C21 0.89 C23 1.41 H23 1.81 C22 Q6 1 0.8705 0.8892 0.4752 1.00000 0.05 0.24 1.25 C8 1.49 H8 1.88 C9 1.95 C7 Q7 1 0.6723 1.0955 0.1718 1.00000 0.05 0.24 0.75 C22 0.77 C24 1.48 H24 1.79 C21 Q8 1 0.9382 0.5312 0.3621 1.00000 0.05 0.24 0.69 C2 0.74 C3 1.84 C4 1.89 C5 Q9 1 0.3098 0.9421 0.0994 1.00000 0.05 0.23 0.72 O5 1.66 C30 1.87 H23 2.04 C31 Q10 1 0.6901 0.8786 0.3879 1.00000 0.05 0.22 0.76 C9 0.88 C10 1.43 H9 1.53 H10 Q11 1 0.8681 0.9539 0.4039 1.00000 0.05 0.22 0.37 C8 0.65 H8 1.44 C9 1.71 C7 Q12 1 1.2797 0.2658 0.4266 1.00000 0.05 0.22 0.82 H19A 1.55 C19 2.00 O3 2.10 H19B Q13 1 0.3592 0.9603 0.2240 1.00000 0.05 0.21 0.73 C30 0.79 C25 1.81 O5 1.82 C29 Q14 1 0.6189 0.9772 0.3795 1.00000 0.05 0.21 0.76 H9 1.25 C9 1.74 C10 1.76 H10 Q15 1 0.9375 0.4930 0.3194 1.00000 0.05 0.21 0.83 C3 0.85 C2 1.95 C5 1.97 C4 Q16 1 0.6926 1.2008 0.1690 1.00000 0.05 0.21 0.66 C32 0.86 C24 1.58 H24 1.78 C33 Q17 1 0.8596 0.7044 0.2887 1.00000 0.05 0.21 0.75 C6 0.81 C4 1.34 H4 1.82 C11 Q18 1 0.7956 1.4316 0.1065 1.00000 0.05 0.20 0.68 C35 0.88 C34 1.37 H35 1.56 H34 Q19 1 0.9384 1.1397 0.1679 1.00000 0.05 0.20 0.91 O6 1.53 C38 1.55 C37 1.59 H38A Q20 1 0.6802 0.5608 0.2093 1.00000 0.05 0.20 1.62 O2 1.98 H4 2.29 S2 2.42 H12B Shortest distances between peaks (including symmetry equivalents) 8 15 0.78 4 16 0.90 7 16 1.29 6 11 1.34 10 14 1.40 9 13 1.84 3 19 1.88 10 11 2.01 2 15 2.02 6 10 2.03 5 9 2.03 5 7 2.05 4 7 2.05 5 13 2.32 2 8 2.34 8 17 2.45 4 18 2.45 1 18 2.52 11 14 2.54 17 20 2.59 1 1 2.64 18 20 2.66 16 19 2.66 1 4 2.69 15 17 2.70 7 19 2.81 4 19 2.86 6 14 2.90 15 20 2.94 5 16 2.96 Time profile in seconds ----------------------- 0.19: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.02: 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. 3.80: 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 4.30: Structure factors and derivatives 12.00: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 1.34: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.20: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.14: Fourier summations 0.08: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + s92 finished at 10:11:44 Total CPU time: 22.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++