+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008src0818 started at 17:55:13 on 12-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src0818 in P-1 CELL 0.71073 8.8129 8.8960 10.3618 74.043 78.854 88.962 ZERR 2.00 0.0002 0.0002 0.0002 0.001 0.001 0.001 LATT 1 SFAC C H B N O UNIT 12 38 10 4 20 V = 765.80 F(000) = 348.0 Mu = 0.12 mm-1 Cell Wt = 666.56 Rho = 1.445 MERG 2 OMIT -3.00 55.00 OMIT 0 -1 1 OMIT 1 2 2 OMIT 1 1 1 OMIT 0 -1 2 OMIT 0 -2 1 OMIT 3 3 3 OMIT -1 1 0 OMIT 5 1 3 OMIT 0 2 2 OMIT 3 -3 1 OMIT -2 1 3 OMIT 1 3 2 OMIT 1 -2 3 EQIV $1 -X, -Y+1, -Z EQIV $2 -X, -Y, -Z+1 EQIV $3 -X+1, -Y, -Z EQIV $4 -X, -Y, -Z HTAB O7 O1_$1 HTAB O8 O3_$2 HTAB O9 O10_$3 HTAB O10 O6_$4 HTAB N12 O4 SIZE 0.28 0.23 0.18 SHEL 7 0.77 FMAP 2 PLAN 5 ACTA HTAB BOND $H WGHT 0.03790 0.24180 L.S. 8 TEMP -153.00 FVAR 1.99256 MOLE 1 B1 3 0.092877 0.191639 0.191291 11.00000 0.01418 0.01413 = 0.01193 -0.00422 -0.00176 0.00405 B2 3 -0.091830 0.406102 0.200381 11.00000 0.01808 0.01723 = 0.01451 -0.00291 -0.00089 0.00510 B3 3 -0.096750 0.195176 0.403191 11.00000 0.01475 0.01697 = 0.01317 -0.00316 -0.00193 0.00343 B4 3 0.375709 0.144032 0.137878 11.00000 0.01651 0.01593 = 0.01350 -0.00362 -0.00248 0.00314 B5 3 0.200186 -0.000260 0.066023 11.00000 0.01700 0.01544 = 0.01310 -0.00349 -0.00219 0.00380 O1 5 0.023316 0.338400 0.130327 11.00000 0.01819 0.01531 = 0.01158 -0.00236 -0.00079 0.00575 O2 5 -0.150027 0.337656 0.337998 11.00000 0.02479 0.02066 = 0.01315 0.00023 0.00217 0.01172 O3 5 0.015351 0.122957 0.334547 11.00000 0.01704 0.01485 = 0.01115 -0.00214 -0.00136 0.00515 O4 5 0.256946 0.224940 0.188781 11.00000 0.01437 0.01711 = 0.01696 -0.00769 -0.00222 0.00316 O5 5 0.346892 0.021022 0.088034 11.00000 0.01538 0.02085 = 0.02425 -0.01225 -0.00377 0.00566 O6 5 0.079275 0.082134 0.109793 11.00000 0.01523 0.01688 = 0.01411 -0.00630 -0.00333 0.00424 O7 5 -0.152383 0.543014 0.141680 11.00000 0.03493 0.02424 = 0.01511 0.00366 0.00591 0.01671 AFIX 147 H7 2 -0.109253 0.574864 0.058840 11.00000 -1.50000 AFIX 0 O8 5 -0.160801 0.135104 0.537745 11.00000 0.02243 0.02183 = 0.01290 0.00093 0.00112 0.01021 AFIX 147 H8 2 -0.115140 0.053983 0.570516 11.00000 -1.50000 AFIX 0 O9 5 0.521656 0.191507 0.136926 11.00000 0.01454 0.02282 = 0.02522 -0.01245 -0.00142 0.00352 AFIX 147 H9 2 0.585795 0.139617 0.097369 11.00000 -1.50000 AFIX 0 O10 5 0.188174 -0.105533 -0.005821 11.00000 0.01731 0.02295 = 0.02344 -0.01360 -0.00633 0.00682 AFIX 147 H10 2 0.101379 -0.099196 -0.028691 11.00000 -1.50000 AFIX 0 MOLE 2 C11 1 0.460614 0.251631 0.468159 11.00000 0.02213 0.02190 = 0.02705 -0.01058 -0.00901 0.00571 AFIX 23 H11A 2 0.414260 0.166582 0.441954 11.00000 -1.20000 H11B 2 0.556781 0.213650 0.500286 11.00000 -1.20000 AFIX 0 C12 1 0.498503 0.392671 0.345475 11.00000 0.01997 0.02794 = 0.02320 -0.01157 -0.00229 -0.00276 AFIX 23 H12A 2 0.547649 0.476816 0.370767 11.00000 -1.20000 H12B 2 0.572361 0.364532 0.271533 11.00000 -1.20000 AFIX 0 C13 1 0.237057 0.482419 0.409667 11.00000 0.02980 0.02826 = 0.02984 -0.01530 -0.01239 0.01283 AFIX 23 H13A 2 0.138615 0.511520 0.378282 11.00000 -1.20000 H13B 2 0.275360 0.571649 0.435756 11.00000 -1.20000 AFIX 0 C14 1 0.208812 0.340541 0.532374 11.00000 0.02006 0.03476 = 0.02541 -0.01350 -0.00201 0.00072 AFIX 23 H14A 2 0.134377 0.365401 0.607697 11.00000 -1.20000 H14B 2 0.162875 0.253775 0.508125 11.00000 -1.20000 AFIX 0 C15 1 0.321440 0.161089 0.702117 11.00000 0.05547 0.02718 = 0.02470 0.00011 -0.01154 -0.00841 AFIX 137 H15A 2 0.272266 0.073549 0.683326 11.00000 -1.50000 H15B 2 0.252187 0.193994 0.774664 11.00000 -1.50000 H15C 2 0.418893 0.128034 0.731612 11.00000 -1.50000 AFIX 0 C16 1 0.386946 0.587555 0.173575 11.00000 0.07136 0.02226 = 0.02770 0.00095 -0.01752 -0.00653 AFIX 137 H16A 2 0.428010 0.674836 0.198791 11.00000 -1.50000 H16B 2 0.291540 0.618018 0.139342 11.00000 -1.50000 H16C 2 0.463544 0.560701 0.102029 11.00000 -1.50000 AFIX 0 N11 4 0.352671 0.291658 0.578158 11.00000 0.02500 0.02144 = 0.01870 -0.00467 -0.00590 -0.00079 N12 4 0.353147 0.449531 0.295914 11.00000 0.03074 0.01768 = 0.01890 -0.00620 -0.00826 0.00063 AFIX 13 H12 2 0.311757 0.369548 0.269897 11.00000 -1.20000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 2008src0818 in P-1 C 0.770 H 0.320 B 0.820 N 0.700 O 0.660 B1 - O1 O3 O6 O4 B2 - O7 O1 O2 B3 - O8 O3 O2 B4 - O9 O4 O5 B5 - O6 O10 O5 O1 - B2 B1 O2 - B3 B2 O3 - B3 B1 O4 - B4 B1 O5 - B4 B5 O6 - B5 B1 O7 - B2 O8 - B3 O9 - B4 O10 - B5 C11 - N11 C12 C12 - N12 C11 C13 - N12 C14 C14 - N11 C13 C15 - N11 C16 - N12 N11 - C14 C11 C15 N12 - C16 C13 C12 Operators for generating equivalent atoms: $1 -x, -y+1, -z $2 -x, -y, -z+1 $3 -x+1, -y, -z $4 -x, -y, -z 16046 Reflections read, of which 36 rejected -11 =< h =< 11, -11 =< k =< 11, -13 =< l =< 12, Max. 2-theta = 54.96 0 Systematic absence violations 0 Inconsistent equivalents 3493 Unique reflections, of which 0 suppressed R(int) = 0.0281 R(sigma) = 0.0232 Friedel opposites merged Maximum memory for data reduction = 2394 / 34883 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 = 2959 / 266158 wR2 = 0.0843 before cycle 1 for 3493 data and 214 / 214 parameters GooF = S = 1.050; Restrained GooF = 1.050 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0379 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.99317 0.00308 0.200 OSF Mean shift/esd = 0.121 Maximum = -0.425 for U22 O1 Max. shift = 0.003 A for H8 Max. dU = 0.000 for B2 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2959 / 266158 wR2 = 0.0842 before cycle 2 for 3493 data and 214 / 214 parameters GooF = S = 1.051; Restrained GooF = 1.051 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0379 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.99256 0.00307 -0.199 OSF Mean shift/esd = 0.044 Maximum = -0.199 for OSF Max. shift = 0.002 A for H8 Max. dU = 0.000 for B2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2959 / 266158 wR2 = 0.0842 before cycle 3 for 3493 data and 214 / 214 parameters GooF = S = 1.051; Restrained GooF = 1.051 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0379 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.99255 0.00307 -0.004 OSF Mean shift/esd = 0.002 Maximum = -0.028 for tors H8 Max. shift = 0.000 A for H8 Max. dU = 0.000 for C16 Least-squares cycle 4 Maximum vector length = 511 Memory required = 2959 / 266158 wR2 = 0.0842 before cycle 4 for 3493 data and 214 / 214 parameters GooF = S = 1.051; Restrained GooF = 1.051 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0379 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.99255 0.00307 0.000 OSF Mean shift/esd = 0.001 Maximum = -0.006 for tors H8 Max. shift = 0.000 A for H8 Max. dU = 0.000 for N12 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2959 / 266158 wR2 = 0.0842 before cycle 5 for 3493 data and 214 / 214 parameters GooF = S = 1.051; Restrained GooF = 1.051 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0379 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.99255 0.00307 0.001 OSF Mean shift/esd = 0.000 Maximum = -0.002 for tors H8 Max. shift = 0.000 A for H8 Max. dU = 0.000 for O8 Least-squares cycle 6 Maximum vector length = 511 Memory required = 2959 / 266158 wR2 = 0.0842 before cycle 6 for 3493 data and 214 / 214 parameters GooF = S = 1.051; Restrained GooF = 1.051 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0379 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.99255 0.00307 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H8 Max. dU = 0.000 for O3 Least-squares cycle 7 Maximum vector length = 511 Memory required = 2959 / 266158 wR2 = 0.0842 before cycle 7 for 3493 data and 214 / 214 parameters GooF = S = 1.051; Restrained GooF = 1.051 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0379 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.99255 0.00307 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O8 Max. shift = 0.000 A for H8 Max. dU = 0.000 for C15 Least-squares cycle 8 Maximum vector length = 511 Memory required = 2959 / 266158 wR2 = 0.0842 before cycle 8 for 3493 data and 214 / 214 parameters GooF = S = 1.051; Restrained GooF = 1.051 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0379 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.99255 0.00307 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O8 Max. shift = 0.000 A for H7 Max. dU = 0.000 for N12 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H7 -0.1090 0.5751 0.0589 147 0.840 0.000 O7 B2 H7 H8 -0.1156 0.0536 0.5704 147 0.840 0.000 O8 B3 H8 H9 0.5858 0.1399 0.0971 147 0.840 0.000 O9 B4 H9 H10 0.1014 -0.0991 -0.0288 147 0.840 0.000 O10 B5 H10 H11A 0.4142 0.1666 0.4419 23 0.990 0.000 C11 N11 C12 H11B 0.5568 0.2136 0.5003 23 0.990 0.000 C11 N11 C12 H12A 0.5476 0.4769 0.3708 23 0.990 0.000 C12 N12 C11 H12B 0.5724 0.3646 0.2715 23 0.990 0.000 C12 N12 C11 H13A 0.1387 0.5116 0.3783 23 0.990 0.000 C13 N12 C14 H13B 0.2755 0.5717 0.4357 23 0.990 0.000 C13 N12 C14 H14A 0.1344 0.3654 0.6077 23 0.990 0.000 C14 N11 C13 H14B 0.1629 0.2538 0.5081 23 0.990 0.000 C14 N11 C13 H15A 0.2724 0.0735 0.6833 137 0.980 0.000 C15 N11 H15A H15B 0.2521 0.1939 0.7747 137 0.980 0.000 C15 N11 H15A H15C 0.4189 0.1281 0.7317 137 0.980 0.000 C15 N11 H15A H16A 0.4284 0.6747 0.1986 137 0.980 0.000 C16 N12 H16A H16B 0.2914 0.6183 0.1396 137 0.980 0.000 C16 N12 H16A H16C 0.4632 0.5605 0.1019 137 0.980 0.000 C16 N12 H16A H12 0.3118 0.3695 0.2700 13 0.930 0.000 N12 C16 C13 C12 2008src0818 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq B1 0.09288 0.19162 0.19128 1.00000 0.01413 0.01401 0.01185 -0.00414 -0.00179 0.00403 0.01337 0.00160 0.00012 0.00012 0.00011 0.00000 0.00047 0.00048 0.00047 0.00039 0.00037 0.00037 0.00021 B2 -0.09180 0.40610 0.20037 1.00000 0.01785 0.01715 0.01448 -0.00297 -0.00085 0.00499 0.01716 0.00175 0.00013 0.00013 0.00011 0.00000 0.00051 0.00051 0.00050 0.00041 0.00040 0.00040 0.00022 B3 -0.09675 0.19512 0.40321 1.00000 0.01463 0.01691 0.01313 -0.00318 -0.00191 0.00335 0.01523 0.00165 0.00012 0.00013 0.00011 0.00000 0.00048 0.00051 0.00048 0.00040 0.00038 0.00039 0.00021 B4 0.37574 0.14403 0.13785 1.00000 0.01643 0.01582 0.01342 -0.00350 -0.00243 0.00312 0.01544 0.00167 0.00013 0.00013 0.00011 0.00000 0.00049 0.00050 0.00047 0.00040 0.00038 0.00039 0.00021 B5 0.20020 -0.00021 0.06597 1.00000 0.01697 0.01536 0.01300 -0.00347 -0.00225 0.00383 0.01534 0.00168 0.00013 0.00013 0.00011 0.00000 0.00050 0.00049 0.00047 0.00040 0.00038 0.00039 0.00021 O1 0.02331 0.33840 0.13034 1.00000 0.01807 0.01512 0.01149 -0.00222 -0.00074 0.00574 0.01556 0.00105 0.00008 0.00008 0.00007 0.00000 0.00034 0.00034 0.00032 0.00026 0.00026 0.00026 0.00015 O2 -0.15004 0.33765 0.33798 1.00000 0.02463 0.02063 0.01309 0.00030 0.00224 0.01175 0.02142 0.00122 0.00009 0.00008 0.00007 0.00000 0.00038 0.00037 0.00034 0.00029 0.00028 0.00030 0.00017 O3 0.01534 0.12295 0.33455 1.00000 0.01694 0.01472 0.01101 -0.00207 -0.00135 0.00513 0.01478 0.00103 0.00008 0.00008 0.00007 0.00000 0.00033 0.00033 0.00032 0.00026 0.00025 0.00026 0.00015 O4 0.25695 0.22491 0.18879 1.00000 0.01427 0.01708 0.01688 -0.00768 -0.00224 0.00318 0.01562 0.00101 0.00008 0.00008 0.00007 0.00000 0.00033 0.00034 0.00033 0.00027 0.00026 0.00026 0.00015 O5 0.34688 0.02105 0.08803 1.00000 0.01528 0.02075 0.02419 -0.01222 -0.00379 0.00570 0.01893 0.00106 0.00008 0.00008 0.00007 0.00000 0.00034 0.00036 0.00037 0.00030 0.00028 0.00027 0.00016 O6 0.07928 0.08214 0.10982 1.00000 0.01519 0.01684 0.01404 -0.00634 -0.00335 0.00424 0.01492 0.00101 0.00008 0.00008 0.00007 0.00000 0.00032 0.00033 0.00032 0.00026 0.00025 0.00025 0.00015 O7 -0.15238 0.54300 0.14167 1.00000 0.03486 0.02418 0.01504 0.00370 0.00601 0.01670 0.02826 0.00145 0.00010 0.00009 0.00008 0.00000 0.00045 0.00040 0.00036 0.00030 0.00032 0.00034 0.00020 H7 -0.10895 0.57507 0.05892 1.00000 0.04239 0.00000 0.00000 O8 -0.16079 0.13511 0.53772 1.00000 0.02234 0.02181 0.01296 0.00094 0.00108 0.01032 0.02095 0.00122 0.00009 0.00009 0.00007 0.00000 0.00037 0.00037 0.00034 0.00028 0.00027 0.00029 0.00017 H8 -0.11557 0.05363 0.57037 1.00000 0.03143 0.00000 0.00000 O9 0.52167 0.19152 0.13694 1.00000 0.01450 0.02283 0.02516 -0.01254 -0.00140 0.00359 0.02002 0.00108 0.00008 0.00009 0.00008 0.00000 0.00034 0.00038 0.00038 0.00031 0.00028 0.00027 0.00017 H9 0.58584 0.13990 0.09710 1.00000 0.03003 0.00000 0.00000 O10 0.18817 -0.10555 -0.00581 1.00000 0.01723 0.02280 0.02335 -0.01352 -0.00634 0.00679 0.01943 0.00106 0.00008 0.00009 0.00008 0.00000 0.00035 0.00037 0.00037 0.00031 0.00028 0.00028 0.00016 H10 0.10144 -0.09912 -0.02880 1.00000 0.02914 0.00000 0.00000 C11 0.46062 0.25161 0.46816 1.00000 0.02200 0.02188 0.02711 -0.01065 -0.00905 0.00560 0.02235 0.00160 0.00012 0.00012 0.00011 0.00000 0.00051 0.00051 0.00055 0.00044 0.00042 0.00040 0.00022 H11A 0.41423 0.16659 0.44195 1.00000 0.02682 0.00000 0.00000 H11B 0.55677 0.21360 0.50029 1.00000 0.02682 0.00000 0.00000 C12 0.49852 0.39270 0.34548 1.00000 0.01979 0.02784 0.02323 -0.01164 -0.00230 -0.00267 0.02291 0.00159 0.00012 0.00013 0.00011 0.00000 0.00050 0.00055 0.00053 0.00045 0.00040 0.00041 0.00023 H12A 0.54764 0.47685 0.37079 1.00000 0.02750 0.00000 0.00000 H12B 0.57240 0.36460 0.27153 1.00000 0.02750 0.00000 0.00000 C13 0.23712 0.48246 0.40965 1.00000 0.02965 0.02824 0.02976 -0.01527 -0.01231 0.01276 0.02699 0.00176 0.00014 0.00014 0.00012 0.00000 0.00058 0.00057 0.00059 0.00048 0.00047 0.00046 0.00025 H13A 0.13869 0.51161 0.37827 1.00000 0.03239 0.00000 0.00000 H13B 0.27548 0.57166 0.43575 1.00000 0.03239 0.00000 0.00000 C14 0.20883 0.34053 0.53237 1.00000 0.01984 0.03465 0.02542 -0.01355 -0.00201 0.00079 0.02591 0.00170 0.00013 0.00014 0.00012 0.00000 0.00051 0.00061 0.00055 0.00048 0.00042 0.00044 0.00024 H14A 0.13437 0.36537 0.60769 1.00000 0.03110 0.00000 0.00000 H14B 0.16293 0.25376 0.50810 1.00000 0.03110 0.00000 0.00000 C15 0.32145 0.16105 0.70213 1.00000 0.05540 0.02723 0.02474 0.00016 -0.01154 -0.00862 0.03664 0.00200 0.00018 0.00015 0.00013 0.00000 0.00083 0.00061 0.00059 0.00049 0.00056 0.00056 0.00030 H15A 0.27241 0.07347 0.68328 1.00000 0.05495 0.00000 0.00000 H15B 0.25209 0.19387 0.77466 1.00000 0.05495 0.00000 0.00000 H15C 0.41890 0.12807 0.73168 1.00000 0.05495 0.00000 0.00000 C16 0.38692 0.58755 0.17355 1.00000 0.07147 0.02234 0.02753 0.00092 -0.01742 -0.00671 0.04084 0.00210 0.00020 0.00015 0.00013 0.00000 0.00100 0.00059 0.00063 0.00050 0.00064 0.00060 0.00034 H16A 0.42842 0.67470 0.19864 1.00000 0.06126 0.00000 0.00000 H16B 0.29141 0.61827 0.13957 1.00000 0.06126 0.00000 0.00000 H16C 0.46317 0.56055 0.10185 1.00000 0.06126 0.00000 0.00000 N11 0.35268 0.29170 0.57815 1.00000 0.02483 0.02135 0.01858 -0.00458 -0.00590 -0.00084 0.02153 0.00133 0.00011 0.00011 0.00009 0.00000 0.00046 0.00044 0.00043 0.00035 0.00035 0.00035 0.00019 N12 0.35315 0.44951 0.29594 1.00000 0.03066 0.01758 0.01886 -0.00621 -0.00826 0.00064 0.02165 0.00133 0.00011 0.00010 0.00009 0.00000 0.00049 0.00042 0.00043 0.00035 0.00036 0.00035 0.00020 H12 0.31175 0.36950 0.26996 1.00000 0.02598 0.00000 0.00000 Final Structure Factor Calculation for 2008src0818 in P-1 Total number of l.s. parameters = 214 Maximum vector length = 511 Memory required = 2745 / 24017 wR2 = 0.0842 before cycle 9 for 3493 data and 0 / 214 parameters GooF = S = 1.051; Restrained GooF = 1.051 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0379 * P )^2 + 0.24 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0322 for 3204 Fo > 4sig(Fo) and 0.0358 for all 3493 data wR2 = 0.0842, GooF = S = 1.051, Restrained GooF = 1.051 for all data Occupancy sum of asymmetric unit = 23.00 for non-hydrogen and 19.00 for hydrogen atoms Principal mean square atomic displacements U 0.0180 0.0123 0.0098 B1 0.0246 0.0142 0.0126 B2 0.0200 0.0132 0.0125 B3 0.0194 0.0135 0.0134 B4 0.0203 0.0130 0.0127 B5 0.0244 0.0113 0.0109 O1 0.0415 0.0117 0.0110 O2 0.0224 0.0112 0.0107 O3 0.0194 0.0163 0.0111 O4 0.0276 0.0187 0.0106 O5 0.0196 0.0138 0.0113 O6 0.0605 0.0129 0.0113 O7 0.0390 0.0126 0.0113 O8 0.0289 0.0196 0.0115 O9 0.0299 0.0166 0.0118 O10 0.0305 0.0196 0.0170 C11 0.0316 0.0195 0.0177 C12 0.0424 0.0223 0.0163 C13 0.0362 0.0229 0.0186 C14 0.0601 0.0297 0.0201 C15 0.0744 0.0298 0.0183 C16 0.0261 0.0208 0.0177 N11 0.0311 0.0185 0.0154 N12 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.023 0.043 0.065 0.088 0.113 0.146 0.187 0.251 0.372 1.000 Number in group 356. 349. 346. 352. 345. 353. 345. 348. 349. 350. GooF 1.032 1.074 1.036 1.065 1.193 1.036 0.926 1.044 0.969 1.113 K 1.381 0.934 0.964 0.981 0.977 0.990 1.008 1.014 1.006 1.007 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.14 1.30 1.62 inf Number in group 362. 347. 351. 342. 346. 347. 349. 352. 347. 350. GooF 0.977 0.989 0.916 0.913 0.917 0.962 1.033 0.894 1.119 1.598 K 1.038 1.034 1.031 1.018 1.005 0.998 0.997 1.000 1.019 0.999 R1 0.069 0.062 0.061 0.048 0.035 0.032 0.026 0.022 0.026 0.030 Recommended weighting scheme: WGHT 0.0359 0.2457 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) -3 1 0 32.85 19.16 5.18 0.087 2.76 1 -3 3 3.65 0.39 4.98 0.012 1.91 0 3 3 11.19 20.48 4.22 0.090 2.52 -6 4 4 18.33 29.73 4.02 0.109 1.08 0 2 1 797.62 955.72 3.89 0.617 4.39 1 2 1 1021.62 1215.82 3.87 0.696 3.99 3 4 2 11.96 20.57 3.85 0.091 1.79 6 1 1 68.18 51.01 3.77 0.143 1.45 5 2 2 43.45 31.06 3.67 0.111 1.65 3 0 3 32.77 46.18 3.66 0.136 2.40 -1 2 1 733.24 854.76 3.41 0.584 3.83 0 1 2 31.03 42.90 3.40 0.131 4.86 -5 5 5 18.10 27.12 3.36 0.104 1.08 1 1 2 136.06 165.31 3.31 0.257 4.59 4 -2 3 74.73 59.22 3.21 0.154 1.72 1 0 4 2.19 0.49 3.16 0.014 2.48 2 8 4 13.66 21.00 3.13 0.092 1.08 -1 3 3 24.41 16.96 3.10 0.082 2.34 -1 0 1 794.73 916.01 3.08 0.604 5.92 -1 1 4 23.67 16.56 3.05 0.081 2.32 1 5 3 33.22 24.50 3.03 0.099 1.71 -1 11 1 3.11 7.63 3.02 0.055 0.79 1 -4 7 66.34 83.85 2.97 0.183 1.06 -4 1 1 9.09 5.17 2.96 0.045 2.01 -2 -2 3 150.70 126.76 2.93 0.225 1.91 3 2 4 1.12 0.04 2.93 0.004 2.04 -2 -1 2 27.59 37.09 2.92 0.122 2.64 5 0 4 476.27 416.08 2.89 0.407 1.56 -1 -3 11 17.12 9.86 2.87 0.063 0.77 2 -3 3 737.73 650.93 2.86 0.510 1.84 0 -2 4 662.34 582.00 2.85 0.482 1.91 5 -3 2 178.25 152.26 2.84 0.246 1.45 -4 5 0 90.07 108.70 2.84 0.208 1.37 2 7 6 -0.23 1.03 2.84 0.020 1.13 0 -4 7 44.06 33.36 2.84 0.115 1.04 1 1 10 44.70 56.95 2.81 0.151 1.02 5 -1 1 36.50 27.90 2.81 0.105 1.72 9 -3 3 28.59 20.18 2.79 0.090 0.91 2 6 7 15.16 21.79 2.79 0.093 1.17 -2 0 3 0.72 2.77 2.77 0.033 2.39 2 5 0 28.99 21.59 2.77 0.093 1.57 -2 3 0 4.59 2.13 2.77 0.029 2.42 -3 -5 2 49.21 38.59 2.76 0.124 1.28 1 -7 5 5.74 2.45 2.76 0.031 0.93 -1 0 6 72.89 59.56 2.75 0.154 1.55 6 9 8 76.05 59.18 2.75 0.154 0.79 4 -2 2 45.94 36.19 2.74 0.120 1.85 3 3 0 2.87 1.01 2.74 0.020 1.99 -1 -8 4 31.48 22.03 2.73 0.094 0.88 -6 6 2 1.42 3.91 2.71 0.039 1.02 Bond lengths and angles B1 - Distance Angles O1 1.4653 (0.0012) O3 1.4725 (0.0012) 111.17 (0.07) O6 1.4734 (0.0012) 108.26 (0.08) 109.99 (0.08) O4 1.4752 (0.0012) 108.52 (0.08) 108.34 (0.08) 110.56 (0.07) B1 - O1 O3 O6 B2 - Distance Angles O7 1.3538 (0.0013) O1 1.3609 (0.0012) 122.58 (0.09) O2 1.3851 (0.0013) 116.89 (0.09) 120.52 (0.09) B2 - O7 O1 B3 - Distance Angles O8 1.3578 (0.0013) O3 1.3604 (0.0012) 123.04 (0.09) O2 1.3838 (0.0013) 116.22 (0.09) 120.73 (0.09) B3 - O8 O3 B4 - Distance Angles O9 1.3585 (0.0013) O4 1.3638 (0.0012) 117.17 (0.09) O5 1.3782 (0.0013) 122.17 (0.09) 120.65 (0.09) B4 - O9 O4 B5 - Distance Angles O6 1.3588 (0.0012) O10 1.3637 (0.0013) 123.31 (0.09) O5 1.3806 (0.0013) 121.69 (0.09) 114.97 (0.09) B5 - O6 O10 O1 - Distance Angles B2 1.3609 (0.0012) B1 1.4653 (0.0012) 123.94 (0.08) O1 - B2 O2 - Distance Angles B3 1.3838 (0.0013) B2 1.3851 (0.0013) 119.84 (0.08) O2 - B3 O3 - Distance Angles B3 1.3604 (0.0012) B1 1.4725 (0.0012) 123.55 (0.08) O3 - B3 O4 - Distance Angles B4 1.3638 (0.0012) B1 1.4752 (0.0012) 123.50 (0.08) O4 - B4 O5 - Distance Angles B4 1.3782 (0.0013) B5 1.3806 (0.0013) 118.78 (0.08) O5 - B4 O6 - Distance Angles B5 1.3588 (0.0012) B1 1.4734 (0.0012) 122.66 (0.08) O6 - B5 O7 - Distance Angles B2 1.3538 (0.0013) H7 0.8400 109.47 O7 - B2 O8 - Distance Angles B3 1.3578 (0.0013) H8 0.8400 109.47 O8 - B3 O9 - Distance Angles B4 1.3585 (0.0013) H9 0.8400 109.47 O9 - B4 O10 - Distance Angles B5 1.3637 (0.0013) H10 0.8400 109.47 O10 - B5 C11 - Distance Angles N11 1.4571 (0.0014) C12 1.5089 (0.0016) 110.29 (0.09) H11A 0.9900 109.60 109.60 H11B 0.9900 109.60 109.60 108.13 C11 - N11 C12 H11A C12 - Distance Angles N12 1.4995 (0.0014) C11 1.5089 (0.0016) 109.65 (0.09) H12A 0.9900 109.74 109.74 H12B 0.9900 109.74 109.74 108.21 C12 - N12 C11 H12A C13 - Distance Angles N12 1.4944 (0.0014) C14 1.5097 (0.0017) 110.51 (0.09) H13A 0.9900 109.55 109.55 H13B 0.9900 109.55 109.55 108.10 C13 - N12 C14 H13A C14 - Distance Angles N11 1.4561 (0.0014) C13 1.5097 (0.0017) 110.81 (0.09) H14A 0.9900 109.48 109.48 H14B 0.9900 109.48 109.48 108.06 C14 - N11 C13 H14A C15 - Distance Angles N11 1.4597 (0.0015) H15A 0.9800 109.47 H15B 0.9800 109.47 109.47 H15C 0.9800 109.47 109.47 109.47 C15 - N11 H15A H15B C16 - Distance Angles N12 1.4886 (0.0015) H16A 0.9800 109.47 H16B 0.9800 109.47 109.47 H16C 0.9800 109.47 109.47 109.47 C16 - N12 H16A H16B N11 - Distance Angles C14 1.4561 (0.0014) C11 1.4571 (0.0014) 109.32 (0.08) C15 1.4597 (0.0015) 109.96 (0.10) 111.93 (0.09) N11 - C14 C11 N12 - Distance Angles C16 1.4886 (0.0015) C13 1.4944 (0.0014) 112.35 (0.10) C12 1.4995 (0.0014) 110.99 (0.10) 110.07 (0.08) H12 0.9300 107.75 107.75 107.75 N12 - C16 C13 C12 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.90 2.7422(10) 175.0 O7-H7...O1_$1 0.84 1.91 2.7466(10) 172.6 O8-H8...O3_$2 0.84 2.09 2.8508(10) 150.6 O9-H9...O10_$3 0.84 1.92 2.7570(10) 171.0 O10-H10...O6_$4 0.93 1.84 2.7548(11) 169.2 N12-H12...O4 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)