+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - DOS/WIN95/NT VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + S92 started at 11:32:51 on 04-May-2001 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 01SRC401 in Pbca CELL 0.71073 7.4181 16.6837 27.9934 90 90 90 ZERR 8 0.0001 0.0003 0.0005 0 0 0 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H O UNIT 168 128 72 V = 3464.50 F(000) = 1712.0 Mu = 0.13 mm-1 Cell Wt = 3298.70 Rho = 1.581 SHEL 7 0.84 ACTA TEMP -153 SIZE 0.1 0.1 0.02 HTAB O3 O9_$1 EQIV $1 x-1/2, y, -z+1/2 HTAB FMAP 2 PLAN 20 BOND L.S. 4 WGHT 0.037800 EXTI 0.000790 FVAR 0.09284 C1 1 -0.231312 0.060793 0.303032 11.00000 0.02962 0.02258 = 0.02785 0.00031 -0.00299 -0.00424 AFIX 23 H1A 2 -0.236761 0.019819 0.328571 11.00000 -1.20000 H1B 2 -0.312314 0.044099 0.276745 11.00000 -1.20000 AFIX 0 C2 1 -0.125593 0.177697 0.329954 11.00000 0.01615 0.01980 = 0.02120 0.00472 -0.00479 -0.00703 C3 1 0.016589 0.136683 0.308419 11.00000 0.02097 0.01445 = 0.01902 -0.00217 -0.00020 -0.00162 C4 1 0.189630 0.163920 0.309018 11.00000 0.02195 0.01807 = 0.01880 -0.00321 0.00162 0.00396 AFIX 43 H4 2 0.285962 0.134961 0.294800 11.00000 -1.20000 AFIX 0 C5 1 0.216054 0.238060 0.332192 11.00000 0.01477 0.01544 = 0.01606 0.00191 -0.00317 0.00234 C6 1 0.074486 0.278343 0.353267 11.00000 0.01658 0.01475 = 0.01254 0.00195 -0.00149 0.00062 C7 1 -0.102008 0.248902 0.353241 11.00000 0.01713 0.02127 = 0.01745 -0.00190 0.00157 0.00113 AFIX 43 H7 2 -0.198574 0.276432 0.368329 11.00000 -1.20000 AFIX 0 C8 1 0.392272 0.283845 0.337134 11.00000 0.01889 0.02037 = 0.01655 -0.00114 0.00046 0.00499 AFIX 13 H8 2 0.475335 0.258333 0.360808 11.00000 -1.20000 AFIX 0 C9 1 0.326318 0.367318 0.353920 11.00000 0.02115 0.01954 = 0.01158 0.00204 -0.00204 -0.00026 C10 1 0.131702 0.357172 0.375511 11.00000 0.01405 0.01610 = 0.01943 0.00188 -0.00105 0.00247 C11 1 0.130326 0.352598 0.429953 11.00000 0.01149 0.01601 = 0.01650 -0.00069 0.00183 -0.00238 C12 1 -0.006425 0.392275 0.455277 11.00000 0.02099 0.01388 = 0.01979 0.00076 -0.00293 0.00001 AFIX 43 H12 2 -0.096068 0.422860 0.439304 11.00000 -1.20000 AFIX 0 C13 1 -0.005057 0.384972 0.504179 11.00000 0.01305 0.01816 = 0.02154 -0.00528 0.00594 -0.00113 C14 1 0.123429 0.340958 0.528015 11.00000 0.01906 0.02046 = 0.01458 -0.00180 0.00182 -0.00286 C15 1 0.256149 0.300690 0.504443 11.00000 0.02895 0.02658 = 0.01795 0.00424 -0.00384 0.00559 AFIX 43 H15 2 0.343284 0.269568 0.521010 11.00000 -1.20000 AFIX 0 C16 1 0.257764 0.307453 0.454553 11.00000 0.01980 0.02415 = 0.02067 -0.00596 0.00228 0.00341 AFIX 43 H16 2 0.348772 0.280350 0.436970 11.00000 -1.20000 AFIX 0 C17 1 -0.054590 0.399775 0.582197 11.00000 0.04130 0.02452 = 0.02344 0.00221 0.00692 0.00887 AFIX 23 H17A 2 -0.149513 0.377770 0.603316 11.00000 -1.20000 H17B 2 -0.007668 0.449664 0.596760 11.00000 -1.20000 AFIX 0 C18 1 0.486062 0.301755 0.290052 11.00000 0.01415 0.02063 = 0.02149 -0.00138 0.00291 0.00339 AFIX 23 H18A 2 0.616473 0.311361 0.294919 11.00000 -1.20000 H18B 2 0.470296 0.257101 0.267139 11.00000 -1.20000 AFIX 0 C19 1 0.393662 0.375676 0.272910 11.00000 0.01631 0.02025 = 0.02024 -0.00187 0.00232 -0.00863 C20 1 0.462225 0.412998 0.384648 11.00000 0.01874 0.02819 = 0.01485 -0.00066 0.00543 -0.00111 C21 1 0.520539 0.531721 0.427091 11.00000 0.02414 0.03121 = 0.03639 -0.01441 -0.00277 -0.00597 AFIX 33 H21A 2 0.465699 0.583909 0.433944 11.00000 -1.50000 H21B 2 0.636499 0.539719 0.411010 11.00000 -1.50000 H21C 2 0.539722 0.502587 0.457062 11.00000 -1.50000 AFIX 0 O1 3 -0.285633 0.137750 0.321399 11.00000 0.02588 0.01881 = 0.03163 -0.00622 0.00092 -0.00155 O2 3 -0.049511 0.068999 0.285786 11.00000 0.02598 0.01948 = 0.03074 -0.00872 -0.00031 -0.00296 O3 3 0.017199 0.421082 0.362068 11.00000 0.02239 0.02052 = 0.01543 -0.00001 -0.00089 0.00459 AFIX 147 H3 2 -0.004501 0.418244 0.332665 11.00000 -1.50000 AFIX 0 O4 3 -0.127424 0.416316 0.535967 11.00000 0.02956 0.03639 = 0.01907 -0.00076 0.00390 0.01005 O5 3 0.088821 0.342417 0.576664 11.00000 0.03155 0.02874 = 0.01739 0.00126 0.00159 0.00276 O6 3 0.307615 0.412753 0.309519 11.00000 0.02217 0.02012 = 0.01884 0.00165 0.00217 0.00129 O7 3 0.604913 0.386117 0.396736 11.00000 0.02157 0.03484 = 0.04845 -0.01593 -0.01272 0.00523 O8 3 0.401596 0.485728 0.396366 11.00000 0.02357 0.02126 = 0.03261 -0.01065 -0.00136 -0.00157 O9 3 0.388616 0.403987 0.233397 11.00000 0.03448 0.02315 = 0.01746 0.00434 0.00494 0.00213 HKLF 4 Covalent radii and connectivity table for 01SRC401 in Pbca C 0.770 H 0.320 O 0.660 C1 - O2 O1 C2 - C7 O1 C3 C3 - C4 O2 C2 C4 - C3 C5 C5 - C6 C4 C8 C6 - C5 C7 C10 C7 - C2 C6 C8 - C18 C5 C9 C9 - O6 C20 C8 C10 C10 - O3 C6 C11 C9 C11 - C16 C12 C10 C12 - C13 C11 C13 - C12 O4 C14 C14 - C15 C13 O5 C15 - C14 C16 C16 - C11 C15 C17 - O4 O5 C18 - C19 C8 C19 - O9 O6 C18 C20 - O7 O8 C9 C21 - O8 O1 - C2 C1 O2 - C3 C1 O3 - C10 O4 - C13 C17 O5 - C14 C17 O6 - C19 C9 O7 - C20 O8 - C20 C21 O9 - C19 Operators for generating equivalent atoms: $1 x-1/2, y, -z+1/2 20380 Reflections read, of which 4439 rejected -8 =< h =< 8, -19 =< k =< 19, -25 =< l =< 33, Max. 2-theta = 50.05 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 0 2 5 49.18 0.93 6 4.78 1 1 6 12.25 0.11 13 0.67 0 2 6 133.69 0.11 7 128.58 1 2 6 21.36 0.11 12 1.41 1 4 9 21.45 0.19 12 1.37 0 4 10 54.00 0.83 7 4.76 2 0 14 93.01 0.47 6 23.46 3 5 15 36.15 0.51 7 4.91 3 1 21 45.03 0.68 7 7.08 9 Inconsistent equivalents 3054 Unique reflections, of which 0 suppressed R(int) = 0.1471 R(sigma) = 0.1296 Friedel opposites merged Maximum memory for data reduction = 2342 / 30391 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 = 3071 / 338926 wR2 = 0.1049 before cycle 1 for 3054 data and 273 / 273 parameters GooF = S = 0.921; Restrained GooF = 0.921 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0378 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.09284 0.00021 -0.016 OSF 2 0.00079 0.00030 0.001 EXTI Mean shift/esd = 0.001 Maximum = -0.016 for OSF Max. shift = 0.000 A for C8 Max. dU = 0.000 for O7 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3071 / 338926 wR2 = 0.1049 before cycle 2 for 3054 data and 273 / 273 parameters GooF = S = 0.921; Restrained GooF = 0.921 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0378 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.09284 0.00021 0.001 OSF 2 0.00079 0.00030 0.001 EXTI Mean shift/esd = 0.000 Maximum = 0.002 for z O5 Max. shift = 0.000 A for C8 Max. dU = 0.000 for C3 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3071 / 338926 wR2 = 0.1049 before cycle 3 for 3054 data and 273 / 273 parameters GooF = S = 0.921; Restrained GooF = 0.921 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0378 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.09284 0.00021 0.000 OSF 2 0.00079 0.00030 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z O4 Max. shift = 0.000 A for O4 Max. dU = 0.000 for O4 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3071 / 338926 wR2 = 0.1049 before cycle 4 for 3054 data and 273 / 273 parameters GooF = S = 0.921; Restrained GooF = 0.921 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0378 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.09284 0.00021 0.000 OSF 2 0.00079 0.00030 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z O4 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C2 Largest correlation matrix elements 0.521 EXTI / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A -0.2368 0.0198 0.3286 23 0.990 0.000 C1 O2 O1 H1B -0.3123 0.0441 0.2767 23 0.990 0.000 C1 O2 O1 H4 0.2860 0.1350 0.2948 43 0.950 0.000 C4 C3 C5 H7 -0.1986 0.2764 0.3683 43 0.950 0.000 C7 C2 C6 H8 0.4753 0.2583 0.3608 13 1.000 0.000 C8 C18 C5 C9 H12 -0.0961 0.4229 0.4393 43 0.950 0.000 C12 C13 C11 H15 0.3433 0.2696 0.5210 43 0.950 0.000 C15 C14 C16 H16 0.3488 0.2803 0.4370 43 0.950 0.000 C16 C11 C15 H17A -0.1495 0.3778 0.6033 23 0.990 0.000 C17 O4 O5 H17B -0.0077 0.4497 0.5968 23 0.990 0.000 C17 O4 O5 H18A 0.6165 0.3114 0.2949 23 0.990 0.000 C18 C19 C8 H18B 0.4703 0.2571 0.2671 23 0.990 0.000 C18 C19 C8 H21A 0.4657 0.5839 0.4339 33 0.980 0.000 C21 O8 H21A H21B 0.6365 0.5397 0.4110 33 0.980 0.000 C21 O8 H21A H21C 0.5397 0.5026 0.4571 33 0.980 0.000 C21 O8 H21A H3 -0.0045 0.4182 0.3327 147 0.840 0.000 O3 C10 H3 01SRC401 in Pbca ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.23131 0.06079 0.30303 1.00000 0.02963 0.02258 0.02785 0.00031 -0.00299 -0.00424 0.02669 0.00531 0.00045 0.00018 0.00010 0.00000 0.00242 0.00208 0.00192 0.00152 0.00151 0.00179 0.00087 H1A -0.23676 0.01982 0.32857 1.00000 0.03202 0.00000 0.00000 H1B -0.31231 0.04410 0.27675 1.00000 0.03202 0.00000 0.00000 C2 -0.12559 0.17770 0.32995 1.00000 0.01615 0.01980 0.02120 0.00472 -0.00479 -0.00703 0.01905 0.00506 0.00041 0.00018 0.00009 0.00000 0.00202 0.00196 0.00172 0.00146 0.00150 0.00171 0.00077 C3 0.01659 0.13668 0.30842 1.00000 0.02097 0.01445 0.01902 -0.00217 -0.00020 -0.00162 0.01815 0.00507 0.00043 0.00018 0.00009 0.00000 0.00217 0.00184 0.00174 0.00141 0.00146 0.00172 0.00076 C4 0.18963 0.16392 0.30902 1.00000 0.02195 0.01807 0.01880 -0.00321 0.00162 0.00396 0.01961 0.00505 0.00042 0.00017 0.00009 0.00000 0.00210 0.00193 0.00167 0.00142 0.00144 0.00165 0.00077 H4 0.28596 0.13496 0.29480 1.00000 0.02353 0.00000 0.00000 C5 0.21605 0.23806 0.33219 1.00000 0.01477 0.01544 0.01606 0.00191 -0.00317 0.00234 0.01542 0.00482 0.00039 0.00017 0.00009 0.00000 0.00191 0.00186 0.00159 0.00137 0.00138 0.00154 0.00073 C6 0.07449 0.27834 0.35327 1.00000 0.01658 0.01475 0.01254 0.00195 -0.00149 0.00062 0.01462 0.00473 0.00040 0.00017 0.00009 0.00000 0.00199 0.00180 0.00161 0.00133 0.00136 0.00152 0.00073 C7 -0.10201 0.24890 0.35324 1.00000 0.01713 0.02127 0.01745 -0.00190 0.00157 0.00113 0.01862 0.00486 0.00039 0.00018 0.00009 0.00000 0.00200 0.00193 0.00169 0.00140 0.00146 0.00164 0.00075 H7 -0.19857 0.27643 0.36833 1.00000 0.02234 0.00000 0.00000 C8 0.39227 0.28384 0.33713 1.00000 0.01889 0.02037 0.01655 -0.00114 0.00046 0.00499 0.01860 0.00491 0.00040 0.00017 0.00009 0.00000 0.00199 0.00190 0.00164 0.00135 0.00143 0.00158 0.00076 H8 0.47534 0.25833 0.36081 1.00000 0.02233 0.00000 0.00000 C9 0.32632 0.36732 0.35392 1.00000 0.02115 0.01954 0.01158 0.00204 -0.00204 -0.00026 0.01742 0.00484 0.00040 0.00017 0.00009 0.00000 0.00204 0.00184 0.00157 0.00140 0.00137 0.00156 0.00075 C10 0.13170 0.35717 0.37551 1.00000 0.01405 0.01610 0.01943 0.00188 -0.00105 0.00247 0.01653 0.00475 0.00039 0.00017 0.00009 0.00000 0.00188 0.00184 0.00167 0.00140 0.00137 0.00157 0.00073 C11 0.13033 0.35260 0.42995 1.00000 0.01149 0.01601 0.01650 -0.00069 0.00183 -0.00238 0.01467 0.00462 0.00039 0.00017 0.00009 0.00000 0.00185 0.00179 0.00159 0.00138 0.00136 0.00153 0.00072 C12 -0.00642 0.39227 0.45528 1.00000 0.02099 0.01388 0.01979 0.00076 -0.00293 0.00001 0.01822 0.00467 0.00039 0.00016 0.00010 0.00000 0.00202 0.00173 0.00177 0.00134 0.00146 0.00153 0.00075 H12 -0.09607 0.42286 0.43930 1.00000 0.02186 0.00000 0.00000 C13 -0.00506 0.38497 0.50418 1.00000 0.01305 0.01816 0.02154 -0.00528 0.00594 -0.00113 0.01758 0.00492 0.00041 0.00017 0.00010 0.00000 0.00196 0.00193 0.00184 0.00143 0.00148 0.00158 0.00077 C14 0.12343 0.34096 0.52802 1.00000 0.01906 0.02046 0.01458 -0.00180 0.00182 -0.00286 0.01803 0.00485 0.00042 0.00017 0.00009 0.00000 0.00201 0.00193 0.00170 0.00140 0.00144 0.00163 0.00075 C15 0.25615 0.30069 0.50444 1.00000 0.02895 0.02658 0.01795 0.00424 -0.00384 0.00559 0.02449 0.00512 0.00045 0.00019 0.00010 0.00000 0.00221 0.00207 0.00187 0.00150 0.00151 0.00171 0.00083 H15 0.34328 0.26957 0.52101 1.00000 0.02939 0.00000 0.00000 C16 0.25776 0.30745 0.45455 1.00000 0.01980 0.02415 0.02067 -0.00596 0.00228 0.00341 0.02154 0.00483 0.00041 0.00017 0.00010 0.00000 0.00199 0.00192 0.00184 0.00152 0.00147 0.00164 0.00077 H16 0.34877 0.28035 0.43697 1.00000 0.02585 0.00000 0.00000 C17 -0.05459 0.39978 0.58220 1.00000 0.04130 0.02452 0.02344 0.00221 0.00692 0.00887 0.02976 0.00566 0.00046 0.00019 0.00010 0.00000 0.00248 0.00203 0.00196 0.00152 0.00160 0.00186 0.00089 H17A -0.14951 0.37777 0.60332 1.00000 0.03571 0.00000 0.00000 H17B -0.00767 0.44966 0.59676 1.00000 0.03571 0.00000 0.00000 C18 0.48606 0.30175 0.29005 1.00000 0.01415 0.02063 0.02149 -0.00138 0.00291 0.00339 0.01876 0.00507 0.00038 0.00017 0.00009 0.00000 0.00192 0.00188 0.00173 0.00140 0.00141 0.00158 0.00076 H18A 0.61647 0.31136 0.29492 1.00000 0.02251 0.00000 0.00000 H18B 0.47030 0.25710 0.26714 1.00000 0.02251 0.00000 0.00000 C19 0.39366 0.37568 0.27291 1.00000 0.01631 0.02025 0.02024 -0.00187 0.00232 -0.00863 0.01893 0.00486 0.00040 0.00018 0.00011 0.00000 0.00196 0.00194 0.00185 0.00155 0.00156 0.00160 0.00076 C20 0.46222 0.41300 0.38465 1.00000 0.01874 0.02819 0.01485 -0.00066 0.00543 -0.00111 0.02059 0.00533 0.00045 0.00020 0.00010 0.00000 0.00212 0.00220 0.00169 0.00156 0.00141 0.00180 0.00077 C21 0.52054 0.53172 0.42709 1.00000 0.02414 0.03121 0.03640 -0.01441 -0.00277 -0.00597 0.03058 0.00485 0.00042 0.00019 0.00011 0.00000 0.00220 0.00208 0.00196 0.00167 0.00157 0.00175 0.00086 H21A 0.46570 0.58391 0.43394 1.00000 0.04587 0.00000 0.00000 H21B 0.63650 0.53972 0.41101 1.00000 0.04587 0.00000 0.00000 H21C 0.53972 0.50259 0.45706 1.00000 0.04587 0.00000 0.00000 O1 -0.28563 0.13775 0.32140 1.00000 0.02588 0.01881 0.03163 -0.00622 0.00092 -0.00155 0.02544 0.00336 0.00028 0.00012 0.00006 0.00000 0.00146 0.00129 0.00124 0.00100 0.00103 0.00112 0.00056 O2 -0.04951 0.06900 0.28579 1.00000 0.02598 0.01948 0.03074 -0.00872 -0.00031 -0.00296 0.02540 0.00329 0.00028 0.00011 0.00007 0.00000 0.00145 0.00129 0.00122 0.00099 0.00102 0.00110 0.00056 O3 0.01720 0.42108 0.36207 1.00000 0.02239 0.02052 0.01543 -0.00001 -0.00089 0.00459 0.01945 0.00319 0.00026 0.00011 0.00006 0.00000 0.00135 0.00125 0.00109 0.00095 0.00096 0.00107 0.00052 H3 -0.00450 0.41824 0.33267 1.00000 0.02917 0.00000 0.00000 O4 -0.12742 0.41632 0.53597 1.00000 0.02956 0.03639 0.01907 -0.00076 0.00390 0.01005 0.02834 0.00349 0.00028 0.00012 0.00006 0.00000 0.00146 0.00145 0.00116 0.00101 0.00103 0.00118 0.00058 O5 0.08882 0.34242 0.57666 1.00000 0.03155 0.02874 0.01739 0.00126 0.00159 0.00276 0.02589 0.00339 0.00028 0.00012 0.00006 0.00000 0.00150 0.00135 0.00120 0.00095 0.00100 0.00118 0.00057 O6 0.30761 0.41275 0.30952 1.00000 0.02217 0.02012 0.01884 0.00165 0.00217 0.00129 0.02038 0.00315 0.00026 0.00011 0.00006 0.00000 0.00138 0.00125 0.00111 0.00099 0.00095 0.00107 0.00054 O7 0.60491 0.38612 0.39674 1.00000 0.02157 0.03484 0.04845 -0.01593 -0.01272 0.00523 0.03495 0.00352 0.00031 0.00013 0.00007 0.00000 0.00150 0.00154 0.00147 0.00112 0.00120 0.00125 0.00063 O8 0.40160 0.48573 0.39637 1.00000 0.02357 0.02126 0.03261 -0.01065 -0.00136 -0.00157 0.02581 0.00330 0.00027 0.00012 0.00006 0.00000 0.00141 0.00136 0.00122 0.00102 0.00104 0.00112 0.00056 O9 0.38862 0.40399 0.23340 1.00000 0.03448 0.02315 0.01746 0.00434 0.00494 0.00213 0.02503 0.00331 0.00027 0.00011 0.00007 0.00000 0.00151 0.00132 0.00117 0.00099 0.00104 0.00110 0.00056 Final Structure Factor Calculation for 01SRC401 in Pbca Total number of l.s. parameters = 273 Maximum vector length = 511 Memory required = 2798 / 21973 wR2 = 0.1049 before cycle 5 for 3054 data and 0 / 273 parameters GooF = S = 0.921; Restrained GooF = 0.921 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0378 * P )^2 + 0.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0501 for 1651 Fo > 4sig(Fo) and 0.1285 for all 3054 data wR2 = 0.1049, GooF = S = 0.921, Restrained GooF = 0.921 for all data Occupancy sum of asymmetric unit = 30.00 for non-hydrogen and 16.00 for hydrogen atoms Principal mean square atomic displacements U 0.0332 0.0265 0.0204 C1 0.0302 0.0163 0.0106 C2 0.0214 0.0198 0.0133 C3 0.0244 0.0211 0.0133 C4 0.0187 0.0172 0.0104 C5 0.0171 0.0158 0.0109 C6 0.0221 0.0188 0.0150 C7 0.0247 0.0170 0.0141 C8 0.0218 0.0197 0.0107 C9 0.0203 0.0174 0.0119 C10 0.0183 0.0156 0.0101 C11 0.0234 0.0175 0.0138 C12 0.0275 0.0155 0.0097 C13 0.0234 0.0168 0.0138 C14 0.0335 0.0261 0.0139 C15 0.0289 0.0221 0.0137 C16 0.0473 0.0217 0.0202 C17 0.0226 0.0220 0.0116 C18 0.0282 0.0192 0.0094 C19 0.0285 0.0223 0.0110 C20 0.0486 0.0284 0.0148 C21 0.0344 0.0258 0.0162 O1 0.0356 0.0265 0.0141 O2 0.0262 0.0170 0.0152 O3 0.0437 0.0246 0.0167 O4 0.0335 0.0271 0.0171 O5 0.0242 0.0196 0.0174 O6 0.0633 0.0251 0.0164 O7 0.0390 0.0240 0.0144 O8 0.0366 0.0240 0.0145 O9 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.009 0.016 0.023 0.032 0.042 0.054 0.069 0.091 0.133 1.000 Number in group 326. 300. 293. 307. 301. 318. 295. 301. 306. 307. GooF 0.746 0.815 0.798 0.832 0.918 0.910 0.970 0.979 1.011 1.163 K -0.620 1.187 1.013 0.980 0.979 0.992 0.965 1.015 0.997 0.991 Resolution(A) 0.84 0.87 0.91 0.95 1.00 1.06 1.14 1.25 1.43 1.80 inf Number in group 313. 308. 303. 302. 309. 297. 310. 302. 305. 305. GooF 0.768 0.896 0.803 0.878 0.837 0.882 0.916 0.917 0.985 1.245 K 1.037 1.060 1.031 1.000 1.010 0.983 0.980 0.979 1.013 0.983 R1 0.356 0.319 0.233 0.202 0.135 0.103 0.079 0.066 0.049 0.038 Recommended weighting scheme: WGHT 0.0377 0.0000 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 1 6 1423.21 1796.30 4.24 0.116 3.84 1 2 2 847.46 987.77 3.79 0.086 5.15 3 4 3 3830.71 3280.28 3.73 0.156 2.07 2 6 5 6032.81 5277.02 3.64 0.198 2.07 3 1 9 202.71 105.75 3.47 0.028 1.92 7 6 2 1554.85 954.08 3.47 0.084 0.99 3 6 3 13099.25 11495.25 3.45 0.292 1.81 5 1 25 1876.34 1387.40 3.41 0.102 0.89 1 2 6 2483.75 3062.24 3.35 0.151 3.57 2 8 15 520.66 689.00 3.26 0.072 1.30 1 8 11 588.51 459.03 3.21 0.058 1.58 1 5 5 1473.42 1286.83 3.21 0.098 2.67 5 4 12 227.18 414.26 3.20 0.055 1.20 1 0 2 13227.84 15490.35 3.15 0.339 6.55 0 2 6 16249.95 59667.08 3.14 0.666 4.07 5 5 23 1754.33 1290.79 3.12 0.098 0.91 0 8 7 5043.83 4414.49 3.07 0.181 1.85 5 13 4 909.01 1348.46 3.02 0.100 0.96 2 3 19 153.13 276.52 2.97 0.045 1.33 1 0 6 366.75 432.22 2.93 0.057 3.95 2 11 0 3781.18 3267.20 2.89 0.156 1.40 1 12 23 127.87 534.25 2.86 0.063 0.91 4 3 12 -37.71 56.67 2.85 0.021 1.40 6 3 22 2033.42 1644.22 2.83 0.111 0.88 3 8 2 115.98 246.59 2.82 0.043 1.58 4 5 5 160.10 238.11 2.81 0.042 1.56 2 6 8 6590.11 5937.30 2.81 0.210 1.88 3 13 2 347.26 463.89 2.80 0.059 1.14 2 8 16 1413.64 1746.62 2.76 0.114 1.26 4 0 12 823.88 1053.80 2.75 0.089 1.45 2 3 11 701.99 826.25 2.74 0.078 1.96 2 12 11 1158.91 1385.52 2.71 0.101 1.16 3 13 17 720.59 379.18 2.69 0.053 0.94 0 8 10 440.55 305.30 2.66 0.048 1.67 3 12 17 293.12 34.69 2.66 0.016 0.98 5 6 12 578.92 794.16 2.64 0.077 1.14 0 6 5 4889.50 4341.47 2.63 0.180 2.49 0 4 14 1070.58 1256.54 2.62 0.097 1.80 1 4 22 353.73 473.36 2.62 0.059 1.20 4 3 5 4885.31 4365.24 2.61 0.180 1.68 1 6 8 10316.30 9389.67 2.61 0.264 2.09 6 9 19 -152.74 196.86 2.60 0.038 0.84 5 3 18 3854.66 3355.15 2.59 0.158 1.05 5 9 2 293.62 22.26 2.55 0.013 1.15 2 0 30 595.32 218.57 2.55 0.040 0.90 1 11 17 457.56 630.62 2.54 0.068 1.10 2 1 0 1919.81 2176.22 2.51 0.127 3.62 1 6 14 1008.73 1136.02 2.46 0.092 1.59 3 8 7 7462.54 6763.44 2.46 0.224 1.48 2 2 4 140.81 198.25 2.46 0.038 3.05 Bond lengths and angles C1 - Distance Angles O2 1.4389 (0.0035) O1 1.4406 (0.0033) 107.28 (0.23) C1 - O2 C2 - Distance Angles C7 1.3663 (0.0037) O1 1.3824 (0.0032) 127.72 (0.28) C3 1.3943 (0.0039) 122.42 (0.28) 109.76 (0.26) C2 - C7 O1 C3 - Distance Angles C4 1.3618 (0.0038) O2 1.3846 (0.0032) 127.71 (0.28) C2 1.3943 (0.0039) 122.95 (0.28) 109.28 (0.26) C3 - C4 O2 C4 - Distance Angles C3 1.3618 (0.0038) C5 1.4104 (0.0037) 115.42 (0.27) C4 - C3 C5 - Distance Angles C6 1.3793 (0.0037) C4 1.4104 (0.0037) 121.21 (0.27) C8 1.5203 (0.0038) 111.77 (0.25) 127.01 (0.27) C5 - C6 C4 C6 - Distance Angles C5 1.3793 (0.0037) C7 1.3984 (0.0036) 122.78 (0.26) C10 1.5158 (0.0038) 112.66 (0.26) 124.55 (0.26) C6 - C5 C7 C7 - Distance Angles C2 1.3663 (0.0037) C6 1.3984 (0.0036) 115.19 (0.27) C7 - C2 C8 - Distance Angles C18 1.5200 (0.0035) C5 1.5203 (0.0038) 114.42 (0.23) C9 1.5491 (0.0037) 103.35 (0.22) 101.99 (0.23) C8 - C18 C5 C9 - Distance Angles O6 1.4624 (0.0030) C20 1.5288 (0.0039) 106.40 (0.22) C8 1.5491 (0.0037) 103.78 (0.19) 114.24 (0.25) C10 1.5742 (0.0038) 107.16 (0.21) 116.25 (0.22) 108.03 (0.23) C9 - O6 C20 C8 C10 - Distance Angles O3 1.4142 (0.0031) C6 1.5158 (0.0038) 112.13 (0.22) C11 1.5260 (0.0036) 107.42 (0.22) 111.41 (0.23) C9 1.5742 (0.0038) 111.57 (0.22) 101.09 (0.22) 113.26 (0.22) C10 - O3 C6 C11 C11 - Distance Angles C16 1.3911 (0.0037) C12 1.4035 (0.0037) 119.77 (0.25) C10 1.5260 (0.0036) 121.13 (0.25) 119.06 (0.26) C11 - C16 C12 C12 - Distance Angles C13 1.3744 (0.0037) C11 1.4035 (0.0037) 117.13 (0.27) C12 - C13 C13 - Distance Angles C12 1.3744 (0.0037) O4 1.3745 (0.0032) 127.32 (0.27) C14 1.3758 (0.0039) 122.38 (0.27) 110.28 (0.25) C13 - C12 O4 C14 - Distance Angles C15 1.3624 (0.0039) C13 1.3758 (0.0039) 121.93 (0.26) O5 1.3861 (0.0031) 128.20 (0.27) 109.81 (0.26) C14 - C15 C13 C15 - Distance Angles C14 1.3624 (0.0039) C16 1.4012 (0.0035) 116.69 (0.28) C15 - C14 C16 - Distance Angles C11 1.3911 (0.0037) C15 1.4012 (0.0035) 122.09 (0.27) C16 - C11 C17 - Distance Angles O4 1.4293 (0.0033) O5 1.4393 (0.0034) 108.08 (0.22) C17 - O4 C18 - Distance Angles C19 1.4903 (0.0039) C8 1.5200 (0.0035) 103.38 (0.23) C18 - C19 C19 - Distance Angles O9 1.2033 (0.0030) O6 1.3566 (0.0031) 120.05 (0.28) C18 1.4903 (0.0039) 129.43 (0.27) 110.52 (0.24) C19 - O9 O6 C20 - Distance Angles O7 1.1983 (0.0033) O8 1.3350 (0.0035) 124.63 (0.29) C9 1.5288 (0.0039) 123.70 (0.30) 111.67 (0.27) C20 - O7 O8 C21 - Distance Angles O8 1.4516 (0.0032) C21 - O1 - Distance Angles C2 1.3824 (0.0032) C1 1.4406 (0.0033) 104.55 (0.23) O1 - C2 O2 - Distance Angles C3 1.3846 (0.0032) C1 1.4389 (0.0035) 104.83 (0.22) O2 - C3 O3 - Distance Angles C10 1.4142 (0.0031) O3 - O4 - Distance Angles C13 1.3745 (0.0032) C17 1.4293 (0.0033) 105.25 (0.23) O4 - C13 O5 - Distance Angles C14 1.3861 (0.0031) C17 1.4393 (0.0034) 104.73 (0.21) O5 - C14 O6 - Distance Angles C19 1.3566 (0.0031) C9 1.4624 (0.0030) 111.17 (0.21) O6 - C19 O7 - Distance Angles C20 1.1983 (0.0034) O7 - O8 - Distance Angles C20 1.3350 (0.0035) C21 1.4516 (0.0032) 114.92 (0.24) O8 - C20 O9 - Distance Angles C19 1.2033 (0.0030) O9 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 2.03 2.852(3) 167.4 O3-H3...O9_$1 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)