+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2006src1540 started at 13:00:43 on 07-Feb-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2006src1540 in P2(1)/c CELL 0.71073 14.2194 10.2937 20.6731 90.000 95.272 90.000 ZERR 8.00 0.0003 0.0002 0.0005 0.000 0.001 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H B N O UNIT 152 144 8 8 8 V = 3013.13 F(000) = 1216.0 Mu = 0.08 mm-1 Cell Wt = 2297.23 Rho = 1.266 MERG 2 OMIT -3.00 55.00 OMIT 1 1 2 OMIT -1 1 2 EXTI 0.00237 SHEL 7 0.77 FMAP 2 PLAN 5 SIZE 0.08 0.15 0.38 ACTA BOND $H WGHT 0.01000 2.49210 L.S. 20 TEMP -153.00 FVAR 0.55613 MOLE 1 C1 1 0.492522 0.630028 0.142467 11.00000 0.03162 0.01625 = 0.02682 0.00090 0.00323 0.00124 AFIX 23 H1A 2 0.476001 0.642578 0.187533 11.00000 -1.20000 H1B 2 0.470500 0.706970 0.116620 11.00000 -1.20000 AFIX 0 C2 1 0.598626 0.616226 0.142170 11.00000 0.03125 0.02205 = 0.03692 0.00260 0.00457 -0.00514 AFIX 23 H2A 2 0.615029 0.613936 0.096669 11.00000 -1.20000 H2B 2 0.629738 0.693127 0.163449 11.00000 -1.20000 AFIX 0 C3 1 0.635552 0.495956 0.176494 11.00000 0.02462 0.02183 = 0.02262 -0.00360 0.00497 -0.00212 C4 1 0.728942 0.486574 0.203087 11.00000 0.02477 0.03316 = 0.03359 -0.00499 0.00241 -0.00643 AFIX 43 H4 2 0.770517 0.558036 0.199819 11.00000 -1.20000 AFIX 0 C5 1 0.761602 0.374657 0.234084 11.00000 0.02142 0.04240 = 0.02954 -0.00601 -0.00306 0.00252 AFIX 43 H5 2 0.825211 0.368559 0.252404 11.00000 -1.20000 AFIX 0 C6 1 0.700243 0.271415 0.238069 11.00000 0.02859 0.02712 = 0.02320 -0.00109 -0.00015 0.00626 AFIX 43 H6 2 0.720899 0.192772 0.258821 11.00000 -1.20000 AFIX 0 C7 1 0.608562 0.285151 0.211293 11.00000 0.02496 0.02097 = 0.01954 -0.00119 0.00333 0.00143 AFIX 43 H7 2 0.566283 0.214318 0.214024 11.00000 -1.20000 AFIX 0 C8 1 0.406913 0.412365 0.222633 11.00000 0.02252 0.01471 = 0.02263 0.00036 0.00382 0.00179 C9 1 0.308581 0.393364 0.217818 11.00000 0.02159 0.02753 = 0.02393 -0.00143 0.00240 0.00284 AFIX 43 H9 2 0.276898 0.371664 0.176777 11.00000 -1.20000 AFIX 0 C10 1 0.256166 0.405236 0.271019 11.00000 0.02120 0.02851 = 0.03264 0.00084 0.00700 0.00312 AFIX 43 H10 2 0.190171 0.388653 0.266186 11.00000 -1.20000 AFIX 0 C11 1 0.299686 0.441156 0.331117 11.00000 0.03188 0.02225 = 0.02410 0.00264 0.01167 0.00699 AFIX 43 H11 2 0.263829 0.450589 0.367406 11.00000 -1.20000 AFIX 0 C12 1 0.396194 0.463092 0.337489 11.00000 0.03198 0.01882 = 0.01971 0.00085 0.00403 0.00182 AFIX 43 H12 2 0.426789 0.489541 0.378142 11.00000 -1.20000 AFIX 0 C13 1 0.448558 0.446315 0.284112 11.00000 0.02317 0.01673 = 0.02204 0.00059 0.00292 -0.00053 AFIX 43 H13 2 0.515029 0.458470 0.289873 11.00000 -1.20000 AFIX 0 C14 1 0.435142 0.275533 0.112768 11.00000 0.01498 0.02143 = 0.02152 -0.00122 0.00109 0.00269 C15 1 0.392872 0.163475 0.135124 11.00000 0.01939 0.02329 = 0.02133 0.00029 0.00193 0.00168 AFIX 43 H15 2 0.377048 0.160785 0.178761 11.00000 -1.20000 AFIX 0 C16 1 0.373263 0.055772 0.095445 11.00000 0.01939 0.01965 = 0.03070 0.00055 -0.00172 0.00087 AFIX 43 H16 2 0.344906 -0.019100 0.112217 11.00000 -1.20000 AFIX 0 C17 1 0.395043 0.057721 0.031625 11.00000 0.02408 0.02300 = 0.02998 -0.00779 -0.00236 0.00388 AFIX 43 H17 2 0.381566 -0.015402 0.004300 11.00000 -1.20000 AFIX 0 C18 1 0.436727 0.167440 0.007945 11.00000 0.02857 0.02974 = 0.02268 -0.00487 0.00299 0.00311 AFIX 43 H18 2 0.451820 0.169585 -0.035864 11.00000 -1.20000 AFIX 0 C19 1 0.456562 0.274260 0.047884 11.00000 0.02261 0.02271 = 0.02320 -0.00114 0.00399 0.00051 AFIX 43 H19 2 0.485404 0.348448 0.030814 11.00000 -1.20000 AFIX 0 B1 3 0.461171 0.402985 0.156674 11.00000 0.01804 0.01885 = 0.01961 -0.00053 0.00134 0.00010 N1 4 0.576180 0.394760 0.181364 11.00000 0.02047 0.01922 = 0.01708 -0.00179 0.00367 0.00079 O1 5 0.447794 0.517072 0.115720 11.00000 0.02614 0.01913 = 0.02127 0.00079 0.00098 0.00125 MOLE 2 C21 1 -0.090363 0.039065 0.369013 11.00000 0.02612 0.02653 = 0.02566 -0.00451 0.00283 -0.00603 AFIX 23 H21A 2 -0.122282 -0.016493 0.334591 11.00000 -1.20000 H21B 2 -0.122715 0.027233 0.409011 11.00000 -1.20000 AFIX 0 C22 1 0.011999 -0.001037 0.381600 11.00000 0.03061 0.02392 = 0.03097 -0.00510 0.00087 0.00002 AFIX 23 H22A 2 0.015044 -0.088136 0.401993 11.00000 -1.20000 H22B 2 0.039831 -0.007810 0.339558 11.00000 -1.20000 AFIX 0 C23 1 0.070046 0.092075 0.424788 11.00000 0.02076 0.02617 = 0.02167 -0.00068 0.00409 -0.00064 C24 1 0.157481 0.053636 0.454125 11.00000 0.02367 0.02944 = 0.03021 0.00131 0.00440 0.00416 AFIX 43 H24 2 0.178899 -0.032712 0.448553 11.00000 -1.20000 AFIX 0 C25 1 0.213115 0.139875 0.491149 11.00000 0.02000 0.04415 = 0.02845 0.00025 0.00048 0.00162 AFIX 43 H25 2 0.272451 0.113499 0.511859 11.00000 -1.20000 AFIX 0 C26 1 0.181276 0.265719 0.497756 11.00000 0.02244 0.03851 = 0.03018 -0.00793 0.00142 -0.00548 AFIX 43 H26 2 0.219037 0.327870 0.522168 11.00000 -1.20000 AFIX 0 C27 1 0.093934 0.299262 0.468337 11.00000 0.02371 0.02850 = 0.02567 -0.00533 0.00387 -0.00224 AFIX 43 H27 2 0.071950 0.385552 0.473188 11.00000 -1.20000 AFIX 0 C28 1 -0.139252 0.259010 0.459583 11.00000 0.02203 0.02245 = 0.02200 0.00091 0.00341 0.00267 C29 1 -0.116808 0.302609 0.523338 11.00000 0.02332 0.02441 = 0.02507 -0.00040 0.00191 0.00017 AFIX 43 H29 2 -0.054314 0.331430 0.535871 11.00000 -1.20000 AFIX 0 C30 1 -0.183064 0.305128 0.568991 11.00000 0.03276 0.02698 = 0.02127 -0.00086 0.00450 0.00417 AFIX 43 H30 2 -0.165548 0.336179 0.611676 11.00000 -1.20000 AFIX 0 C31 1 -0.274429 0.262404 0.552196 11.00000 0.02839 0.03016 = 0.02586 0.00402 0.01078 0.00942 AFIX 43 H31 2 -0.319676 0.263375 0.583264 11.00000 -1.20000 AFIX 0 C32 1 -0.299167 0.218227 0.489609 11.00000 0.01951 0.03495 = 0.02823 0.00488 0.00422 0.00363 AFIX 43 H32 2 -0.361544 0.188250 0.477684 11.00000 -1.20000 AFIX 0 C33 1 -0.232779 0.217749 0.444277 11.00000 0.02274 0.03210 = 0.02191 0.00066 0.00156 0.00238 AFIX 43 H33 2 -0.251336 0.188470 0.401420 11.00000 -1.20000 AFIX 0 C34 1 -0.057224 0.404580 0.370656 11.00000 0.01940 0.02772 = 0.01955 -0.00288 0.00209 -0.00019 C35 1 -0.119025 0.506089 0.380527 11.00000 0.02428 0.03175 = 0.02532 0.00008 0.00576 0.00391 AFIX 43 H35 2 -0.166478 0.493249 0.409380 11.00000 -1.20000 AFIX 0 C36 1 -0.113807 0.625615 0.349675 11.00000 0.03520 0.02906 = 0.03305 0.00170 0.00478 0.00989 AFIX 43 H36 2 -0.157822 0.692209 0.357061 11.00000 -1.20000 AFIX 0 C37 1 -0.044448 0.647331 0.308241 11.00000 0.03784 0.02791 = 0.02709 0.00415 0.00103 0.00138 AFIX 43 H37 2 -0.040389 0.728866 0.287149 11.00000 -1.20000 AFIX 0 C38 1 0.019044 0.549275 0.297739 11.00000 0.03054 0.03513 = 0.02534 0.00080 0.00876 -0.00042 AFIX 43 H38 2 0.067283 0.563608 0.269656 11.00000 -1.20000 AFIX 0 C39 1 0.012161 0.430144 0.328246 11.00000 0.02758 0.02830 = 0.02814 -0.00179 0.00868 0.00347 AFIX 43 H39 2 0.055869 0.363590 0.320174 11.00000 -1.20000 AFIX 0 B21 3 -0.068595 0.261663 0.401689 11.00000 0.01722 0.02530 = 0.02219 -0.00208 0.00128 0.00166 N21 4 0.038232 0.214336 0.432836 11.00000 0.01817 0.02382 = 0.02072 -0.00175 0.00330 -0.00088 O21 5 -0.096329 0.170843 0.349430 11.00000 0.02145 0.02621 = 0.02152 -0.00213 0.00189 -0.00094 HKLF 4 Covalent radii and connectivity table for 2006src1540 in P2(1)/c C 0.770 H 0.320 B 0.820 N 0.700 O 0.660 C1 - O1 C2 C2 - C3 C1 C3 - N1 C4 C2 C4 - C5 C3 C5 - C4 C6 C6 - C7 C5 C7 - N1 C6 C8 - C13 C9 B1 C9 - C10 C8 C10 - C11 C9 C11 - C12 C10 C12 - C11 C13 C13 - C8 C12 C14 - C15 C19 B1 C15 - C16 C14 C16 - C17 C15 C17 - C16 C18 C18 - C17 C19 C19 - C18 C14 B1 - O1 C14 C8 N1 N1 - C7 C3 B1 O1 - C1 B1 C21 - O21 C22 C22 - C23 C21 C23 - N21 C24 C22 C24 - C25 C23 C25 - C24 C26 C26 - C27 C25 C27 - N21 C26 C28 - C29 C33 B21 C29 - C30 C28 C30 - C31 C29 C31 - C30 C32 C32 - C31 C33 C33 - C32 C28 C34 - C35 C39 B21 C35 - C36 C34 C36 - C37 C35 C37 - C36 C38 C38 - C37 C39 C39 - C38 C34 B21 - O21 C34 C28 N21 N21 - C27 C23 B21 O21 - C21 B21 h k l Fo^2 Sigma Why rejected 7 0 7 9.56 2.14 observed but should be systematically absent -5 0 15 1.95 0.44 observed but should be systematically absent 31275 Reflections read, of which 1099 rejected -18 =< h =< 18, -13 =< k =< 13, -26 =< l =< 26, Max. 2-theta = 54.97 2 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 3 3 2 51.68 1.60 8 13.39 -11 1 6 3.22 1.90 3 11.18 2 Inconsistent equivalents 6886 Unique reflections, of which 0 suppressed R(int) = 0.0437 R(sigma) = 0.0393 Friedel opposites merged Maximum memory for data reduction = 3869 / 68686 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 = 5005 / 510970 wR2 = 0.1113 before cycle 1 for 6886 data and 398 / 398 parameters GooF = S = 1.097; Restrained GooF = 1.097 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 2.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55603 0.00083 -0.119 OSF 2 0.00234 0.00048 -0.058 EXTI Mean shift/esd = 0.011 Maximum = -0.119 for OSF Max. shift = 0.000 A for C36 Max. dU = 0.000 for C19 Least-squares cycle 2 Maximum vector length = 511 Memory required = 5005 / 510970 wR2 = 0.1112 before cycle 2 for 6886 data and 398 / 398 parameters GooF = S = 1.097; Restrained GooF = 1.097 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 2.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55601 0.00083 -0.030 OSF 2 0.00233 0.00048 -0.020 EXTI Mean shift/esd = 0.004 Maximum = -0.030 for OSF Max. shift = 0.000 A for C36 Max. dU = 0.000 for B21 Least-squares cycle 3 Maximum vector length = 511 Memory required = 5005 / 510970 wR2 = 0.1113 before cycle 3 for 6886 data and 398 / 398 parameters GooF = S = 1.097; Restrained GooF = 1.097 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 2.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55600 0.00083 -0.003 OSF 2 0.00233 0.00048 -0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.003 for OSF Max. shift = 0.000 A for C37 Max. dU = 0.000 for B21 Least-squares cycle 4 Maximum vector length = 511 Memory required = 5005 / 510970 wR2 = 0.1113 before cycle 4 for 6886 data and 398 / 398 parameters GooF = S = 1.097; Restrained GooF = 1.097 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 2.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55600 0.00083 0.000 OSF 2 0.00233 0.00048 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z C29 Max. shift = 0.000 A for C7 Max. dU = 0.000 for C33 Least-squares cycle 5 Maximum vector length = 511 Memory required = 5005 / 510970 wR2 = 0.1113 before cycle 5 for 6886 data and 398 / 398 parameters GooF = S = 1.097; Restrained GooF = 1.097 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 2.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55600 0.00083 0.000 OSF 2 0.00233 0.00048 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z C29 Max. shift = 0.000 A for C28 Max. dU = 0.000 for B1 Least-squares cycle 6 Maximum vector length = 511 Memory required = 5005 / 510970 wR2 = 0.1113 before cycle 6 for 6886 data and 398 / 398 parameters GooF = S = 1.097; Restrained GooF = 1.097 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 2.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55600 0.00083 0.000 OSF 2 0.00233 0.00048 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z C29 Max. shift = 0.000 A for C23 Max. dU = 0.000 for C25 Least-squares cycle 7 Maximum vector length = 511 Memory required = 5005 / 510970 wR2 = 0.1113 before cycle 7 for 6886 data and 398 / 398 parameters GooF = S = 1.097; Restrained GooF = 1.097 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 2.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55600 0.00083 0.000 OSF 2 0.00233 0.00048 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z C29 Max. shift = 0.000 A for C25 Max. dU = 0.000 for C19 Least-squares cycle 8 Maximum vector length = 511 Memory required = 5005 / 510970 wR2 = 0.1113 before cycle 8 for 6886 data and 398 / 398 parameters GooF = S = 1.097; Restrained GooF = 1.097 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 2.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55600 0.00083 0.000 OSF 2 0.00233 0.00048 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z C29 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C32 Least-squares cycle 9 Maximum vector length = 511 Memory required = 5005 / 510970 wR2 = 0.1113 before cycle 9 for 6886 data and 398 / 398 parameters GooF = S = 1.097; Restrained GooF = 1.097 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 2.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55600 0.00083 0.000 OSF 2 0.00233 0.00048 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z C29 Max. shift = 0.000 A for C39 Max. dU = 0.000 for C18 Least-squares cycle 10 Maximum vector length = 511 Memory required = 5005 / 510970 wR2 = 0.1113 before cycle 10 for 6886 data and 398 / 398 parameters GooF = S = 1.097; Restrained GooF = 1.097 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 2.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55600 0.00083 0.000 OSF 2 0.00233 0.00048 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z C29 Max. shift = 0.000 A for C9 Max. dU = 0.000 for C39 Least-squares cycle 11 Maximum vector length = 511 Memory required = 5005 / 510970 wR2 = 0.1113 before cycle 11 for 6886 data and 398 / 398 parameters GooF = S = 1.097; Restrained GooF = 1.097 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 2.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55600 0.00083 0.000 OSF 2 0.00233 0.00048 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z C29 Max. shift = 0.000 A for N21 Max. dU = 0.000 for C9 Least-squares cycle 12 Maximum vector length = 511 Memory required = 5005 / 510970 wR2 = 0.1113 before cycle 12 for 6886 data and 398 / 398 parameters GooF = S = 1.097; Restrained GooF = 1.097 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 2.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55600 0.00083 0.000 OSF 2 0.00233 0.00048 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z C29 Max. shift = 0.000 A for C19 Max. dU = 0.000 for B1 Least-squares cycle 13 Maximum vector length = 511 Memory required = 5005 / 510970 wR2 = 0.1113 before cycle 13 for 6886 data and 398 / 398 parameters GooF = S = 1.097; Restrained GooF = 1.097 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 2.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55600 0.00083 0.000 OSF 2 0.00233 0.00048 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z C29 Max. shift = 0.000 A for C21 Max. dU = 0.000 for C25 Least-squares cycle 14 Maximum vector length = 511 Memory required = 5005 / 510970 wR2 = 0.1113 before cycle 14 for 6886 data and 398 / 398 parameters GooF = S = 1.097; Restrained GooF = 1.097 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 2.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55600 0.00083 0.000 OSF 2 0.00233 0.00048 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z C29 Max. shift = 0.000 A for N21 Max. dU = 0.000 for C38 Least-squares cycle 15 Maximum vector length = 511 Memory required = 5005 / 510970 wR2 = 0.1113 before cycle 15 for 6886 data and 398 / 398 parameters GooF = S = 1.097; Restrained GooF = 1.097 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 2.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55600 0.00083 0.000 OSF 2 0.00233 0.00048 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z C29 Max. shift = 0.000 A for C24 Max. dU = 0.000 for C28 Least-squares cycle 16 Maximum vector length = 511 Memory required = 5005 / 510970 wR2 = 0.1113 before cycle 16 for 6886 data and 398 / 398 parameters GooF = S = 1.097; Restrained GooF = 1.097 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 2.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55600 0.00083 0.000 OSF 2 0.00233 0.00048 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z C29 Max. shift = 0.000 A for N21 Max. dU = 0.000 for B21 Least-squares cycle 17 Maximum vector length = 511 Memory required = 5005 / 510970 wR2 = 0.1113 before cycle 17 for 6886 data and 398 / 398 parameters GooF = S = 1.097; Restrained GooF = 1.097 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 2.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55600 0.00083 0.000 OSF 2 0.00233 0.00048 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z C29 Max. shift = 0.000 A for C2 Max. dU = 0.000 for C26 Least-squares cycle 18 Maximum vector length = 511 Memory required = 5005 / 510970 wR2 = 0.1113 before cycle 18 for 6886 data and 398 / 398 parameters GooF = S = 1.097; Restrained GooF = 1.097 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 2.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55600 0.00083 0.000 OSF 2 0.00233 0.00048 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z C29 Max. shift = 0.000 A for C38 Max. dU = 0.000 for C27 Least-squares cycle 19 Maximum vector length = 511 Memory required = 5005 / 510970 wR2 = 0.1113 before cycle 19 for 6886 data and 398 / 398 parameters GooF = S = 1.097; Restrained GooF = 1.097 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 2.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55600 0.00083 0.000 OSF 2 0.00233 0.00048 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z C29 Max. shift = 0.000 A for C2 Max. dU = 0.000 for C33 Least-squares cycle 20 Maximum vector length = 511 Memory required = 5005 / 510970 wR2 = 0.1113 before cycle 20 for 6886 data and 398 / 398 parameters GooF = S = 1.097; Restrained GooF = 1.097 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 2.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.55600 0.00083 0.000 OSF 2 0.00233 0.00048 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for z C29 Max. shift = 0.000 A for O21 Max. dU = 0.000 for C33 Largest correlation matrix elements 0.565 EXTI / OSF Idealized hydrogen atom generation before cycle 21 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.4760 0.6426 0.1875 23 0.990 0.000 C1 O1 C2 H1B 0.4705 0.7070 0.1166 23 0.990 0.000 C1 O1 C2 H2A 0.6150 0.6139 0.0967 23 0.990 0.000 C2 C3 C1 H2B 0.6297 0.6931 0.1635 23 0.990 0.000 C2 C3 C1 H4 0.7705 0.5580 0.1998 43 0.950 0.000 C4 C5 C3 H5 0.8252 0.3686 0.2524 43 0.950 0.000 C5 C4 C6 H6 0.7209 0.1928 0.2588 43 0.950 0.000 C6 C7 C5 H7 0.5663 0.2143 0.2140 43 0.950 0.000 C7 N1 C6 H9 0.2769 0.3717 0.1768 43 0.950 0.000 C9 C10 C8 H10 0.1902 0.3886 0.2662 43 0.950 0.000 C10 C11 C9 H11 0.2638 0.4506 0.3674 43 0.950 0.000 C11 C12 C10 H12 0.4268 0.4895 0.3781 43 0.950 0.000 C12 C11 C13 H13 0.5150 0.4585 0.2899 43 0.950 0.000 C13 C8 C12 H15 0.3771 0.1608 0.1788 43 0.950 0.000 C15 C16 C14 H16 0.3449 -0.0191 0.1122 43 0.950 0.000 C16 C17 C15 H17 0.3816 -0.0154 0.0043 43 0.950 0.000 C17 C16 C18 H18 0.4518 0.1696 -0.0359 43 0.950 0.000 C18 C17 C19 H19 0.4854 0.3485 0.0308 43 0.950 0.000 C19 C18 C14 H21A -0.1223 -0.0165 0.3346 23 0.990 0.000 C21 O21 C22 H21B -0.1227 0.0272 0.4090 23 0.990 0.000 C21 O21 C22 H22A 0.0150 -0.0881 0.4020 23 0.990 0.000 C22 C23 C21 H22B 0.0398 -0.0078 0.3396 23 0.990 0.000 C22 C23 C21 H24 0.1789 -0.0327 0.4486 43 0.950 0.000 C24 C25 C23 H25 0.2725 0.1135 0.5119 43 0.950 0.000 C25 C24 C26 H26 0.2190 0.3279 0.5222 43 0.950 0.000 C26 C27 C25 H27 0.0719 0.3855 0.4732 43 0.950 0.000 C27 N21 C26 H29 -0.0543 0.3314 0.5359 43 0.950 0.000 C29 C30 C28 H30 -0.1655 0.3362 0.6117 43 0.950 0.000 C30 C31 C29 H31 -0.3197 0.2634 0.5833 43 0.950 0.000 C31 C30 C32 H32 -0.3615 0.1883 0.4777 43 0.950 0.000 C32 C31 C33 H33 -0.2513 0.1885 0.4014 43 0.950 0.000 C33 C32 C28 H35 -0.1665 0.4932 0.4094 43 0.950 0.000 C35 C36 C34 H36 -0.1578 0.6922 0.3571 43 0.950 0.000 C36 C37 C35 H37 -0.0404 0.7289 0.2871 43 0.950 0.000 C37 C36 C38 H38 0.0673 0.5636 0.2697 43 0.950 0.000 C38 C37 C39 H39 0.0559 0.3636 0.3202 43 0.950 0.000 C39 C38 C34 2006src1540 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.49252 0.63003 0.14247 1.00000 0.03159 0.01625 0.02681 0.00090 0.00324 0.00125 0.02485 0.00299 0.00012 0.00016 0.00008 0.00000 0.00088 0.00078 0.00083 0.00064 0.00067 0.00066 0.00035 H1A 0.47600 0.64258 0.18753 1.00000 0.02982 0.00000 0.00000 H1B 0.47050 0.70697 0.11662 1.00000 0.02982 0.00000 0.00000 C2 0.59862 0.61623 0.14217 1.00000 0.03123 0.02206 0.03690 0.00260 0.00457 -0.00512 0.02997 0.00327 0.00012 0.00017 0.00009 0.00000 0.00092 0.00087 0.00098 0.00074 0.00075 0.00072 0.00039 H2A 0.61503 0.61394 0.09667 1.00000 0.03597 0.00000 0.00000 H2B 0.62974 0.69313 0.16345 1.00000 0.03597 0.00000 0.00000 C3 0.63555 0.49595 0.17649 1.00000 0.02461 0.02181 0.02261 -0.00360 0.00497 -0.00212 0.02284 0.00288 0.00011 0.00016 0.00008 0.00000 0.00079 0.00082 0.00079 0.00064 0.00063 0.00065 0.00034 C4 0.72895 0.48657 0.20309 1.00000 0.02475 0.03317 0.03358 -0.00500 0.00241 -0.00642 0.03052 0.00315 0.00012 0.00019 0.00009 0.00000 0.00085 0.00100 0.00095 0.00077 0.00071 0.00074 0.00040 H4 0.77052 0.55804 0.19982 1.00000 0.03663 0.00000 0.00000 C5 0.76161 0.37466 0.23408 1.00000 0.02140 0.04239 0.02953 -0.00601 -0.00306 0.00252 0.03144 0.00318 0.00012 0.00020 0.00009 0.00000 0.00083 0.00112 0.00090 0.00080 0.00068 0.00076 0.00041 H5 0.82521 0.36856 0.25241 1.00000 0.03773 0.00000 0.00000 C6 0.70024 0.27141 0.23807 1.00000 0.02860 0.02711 0.02320 -0.00111 -0.00015 0.00626 0.02646 0.00305 0.00012 0.00018 0.00008 0.00000 0.00086 0.00089 0.00081 0.00068 0.00067 0.00071 0.00036 H6 0.72090 0.19277 0.25882 1.00000 0.03175 0.00000 0.00000 C7 0.60856 0.28516 0.21129 1.00000 0.02494 0.02096 0.01954 -0.00119 0.00331 0.00143 0.02173 0.00289 0.00011 0.00016 0.00007 0.00000 0.00079 0.00079 0.00073 0.00062 0.00061 0.00064 0.00033 H7 0.56628 0.21432 0.21403 1.00000 0.02608 0.00000 0.00000 C8 0.40691 0.41237 0.22263 1.00000 0.02251 0.01471 0.02261 0.00035 0.00383 0.00178 0.01984 0.00281 0.00011 0.00015 0.00008 0.00000 0.00076 0.00073 0.00076 0.00060 0.00060 0.00059 0.00032 C9 0.30858 0.39336 0.21782 1.00000 0.02156 0.02754 0.02393 -0.00144 0.00241 0.00285 0.02432 0.00304 0.00011 0.00017 0.00008 0.00000 0.00079 0.00088 0.00080 0.00068 0.00062 0.00067 0.00035 H9 0.27690 0.37166 0.17678 1.00000 0.02919 0.00000 0.00000 C10 0.25616 0.40523 0.27102 1.00000 0.02120 0.02851 0.03262 0.00084 0.00699 0.00312 0.02716 0.00323 0.00012 0.00017 0.00008 0.00000 0.00079 0.00091 0.00091 0.00073 0.00067 0.00069 0.00037 H10 0.19017 0.38864 0.26619 1.00000 0.03260 0.00000 0.00000 C11 0.29968 0.44116 0.33112 1.00000 0.03185 0.02225 0.02408 0.00263 0.01167 0.00697 0.02550 0.00319 0.00012 0.00016 0.00008 0.00000 0.00088 0.00084 0.00082 0.00066 0.00068 0.00070 0.00036 H11 0.26382 0.45059 0.36741 1.00000 0.03060 0.00000 0.00000 C12 0.39620 0.46309 0.33749 1.00000 0.03196 0.01881 0.01970 0.00085 0.00404 0.00182 0.02339 0.00302 0.00012 0.00016 0.00008 0.00000 0.00087 0.00080 0.00076 0.00062 0.00065 0.00067 0.00034 H12 0.42679 0.48954 0.37814 1.00000 0.02806 0.00000 0.00000 C13 0.44856 0.44631 0.28411 1.00000 0.02316 0.01672 0.02202 0.00059 0.00290 -0.00053 0.02058 0.00281 0.00011 0.00015 0.00007 0.00000 0.00077 0.00074 0.00076 0.00061 0.00061 0.00062 0.00032 H13 0.51503 0.45847 0.28987 1.00000 0.02470 0.00000 0.00000 C14 0.43514 0.27553 0.11277 1.00000 0.01498 0.02141 0.02150 -0.00123 0.00109 0.00269 0.01933 0.00274 0.00010 0.00016 0.00007 0.00000 0.00069 0.00080 0.00074 0.00062 0.00057 0.00059 0.00032 C15 0.39287 0.16347 0.13513 1.00000 0.01937 0.02327 0.02133 0.00029 0.00192 0.00166 0.02132 0.00282 0.00011 0.00016 0.00008 0.00000 0.00074 0.00082 0.00076 0.00063 0.00059 0.00063 0.00033 H15 0.37705 0.16078 0.17876 1.00000 0.02558 0.00000 0.00000 C16 0.37326 0.05577 0.09545 1.00000 0.01939 0.01964 0.03068 0.00053 -0.00171 0.00087 0.02349 0.00288 0.00011 0.00016 0.00008 0.00000 0.00075 0.00079 0.00086 0.00067 0.00064 0.00063 0.00034 H16 0.34491 -0.01911 0.11222 1.00000 0.02818 0.00000 0.00000 C17 0.39504 0.05772 0.03162 1.00000 0.02406 0.02300 0.02996 -0.00778 -0.00235 0.00388 0.02597 0.00298 0.00012 0.00017 0.00008 0.00000 0.00081 0.00084 0.00086 0.00070 0.00066 0.00067 0.00036 H17 0.38156 -0.01540 0.00430 1.00000 0.03117 0.00000 0.00000 C18 0.43673 0.16744 0.00794 1.00000 0.02857 0.02971 0.02267 -0.00488 0.00299 0.00309 0.02694 0.00306 0.00012 0.00018 0.00008 0.00000 0.00086 0.00093 0.00081 0.00069 0.00066 0.00072 0.00037 H18 0.45182 0.16958 -0.03587 1.00000 0.03233 0.00000 0.00000 C19 0.45656 0.27427 0.04788 1.00000 0.02261 0.02269 0.02317 -0.00115 0.00399 0.00052 0.02271 0.00291 0.00011 0.00016 0.00008 0.00000 0.00078 0.00082 0.00077 0.00065 0.00062 0.00064 0.00033 H19 0.48541 0.34845 0.03082 1.00000 0.02725 0.00000 0.00000 B1 0.46118 0.40299 0.15668 1.00000 0.01804 0.01883 0.01958 -0.00054 0.00135 0.00009 0.01884 0.00312 0.00012 0.00018 0.00008 0.00000 0.00080 0.00085 0.00081 0.00067 0.00063 0.00066 0.00035 N1 0.57618 0.39476 0.18137 1.00000 0.02046 0.01923 0.01707 -0.00180 0.00368 0.00079 0.01880 0.00229 0.00009 0.00013 0.00006 0.00000 0.00064 0.00065 0.00061 0.00051 0.00049 0.00052 0.00027 O1 0.44779 0.51708 0.11572 1.00000 0.02612 0.01914 0.02126 0.00079 0.00099 0.00126 0.02224 0.00198 0.00008 0.00011 0.00005 0.00000 0.00058 0.00057 0.00055 0.00044 0.00044 0.00046 0.00025 C21 -0.09036 0.03906 0.36901 1.00000 0.02610 0.02651 0.02566 -0.00451 0.00283 -0.00603 0.02606 0.00295 0.00012 0.00017 0.00008 0.00000 0.00084 0.00088 0.00083 0.00069 0.00066 0.00069 0.00036 H21A -0.12228 -0.01649 0.33459 1.00000 0.03127 0.00000 0.00000 H21B -0.12271 0.02723 0.40901 1.00000 0.03127 0.00000 0.00000 C22 0.01199 -0.00104 0.38160 1.00000 0.03060 0.02391 0.03096 -0.00509 0.00087 0.00003 0.02861 0.00303 0.00012 0.00017 0.00009 0.00000 0.00090 0.00088 0.00091 0.00072 0.00072 0.00072 0.00038 H22A 0.01504 -0.08814 0.40199 1.00000 0.03433 0.00000 0.00000 H22B 0.03982 -0.00781 0.33956 1.00000 0.03433 0.00000 0.00000 C23 0.07005 0.09208 0.42479 1.00000 0.02075 0.02616 0.02166 -0.00068 0.00407 -0.00064 0.02273 0.00291 0.00011 0.00017 0.00008 0.00000 0.00077 0.00086 0.00077 0.00065 0.00061 0.00064 0.00034 C24 0.15748 0.05363 0.45412 1.00000 0.02366 0.02943 0.03021 0.00130 0.00441 0.00415 0.02765 0.00318 0.00012 0.00018 0.00008 0.00000 0.00082 0.00092 0.00088 0.00073 0.00068 0.00071 0.00037 H24 0.17890 -0.03272 0.44855 1.00000 0.03317 0.00000 0.00000 C25 0.21312 0.13988 0.49115 1.00000 0.01998 0.04414 0.02844 0.00024 0.00048 0.00161 0.03096 0.00325 0.00012 0.00020 0.00009 0.00000 0.00080 0.00113 0.00089 0.00079 0.00067 0.00076 0.00040 H25 0.27245 0.11350 0.51186 1.00000 0.03715 0.00000 0.00000 C26 0.18128 0.26572 0.49776 1.00000 0.02243 0.03851 0.03017 -0.00792 0.00142 -0.00546 0.03043 0.00312 0.00012 0.00019 0.00009 0.00000 0.00083 0.00105 0.00090 0.00079 0.00069 0.00075 0.00040 H26 0.21904 0.32788 0.52217 1.00000 0.03652 0.00000 0.00000 C27 0.09393 0.29926 0.46834 1.00000 0.02369 0.02850 0.02564 -0.00532 0.00385 -0.00225 0.02585 0.00293 0.00011 0.00018 0.00008 0.00000 0.00081 0.00091 0.00083 0.00070 0.00065 0.00069 0.00036 H27 0.07194 0.38554 0.47319 1.00000 0.03102 0.00000 0.00000 C28 -0.13925 0.25901 0.45958 1.00000 0.02201 0.02246 0.02197 0.00091 0.00341 0.00267 0.02206 0.00292 0.00011 0.00016 0.00008 0.00000 0.00077 0.00081 0.00076 0.00063 0.00061 0.00064 0.00033 C29 -0.11681 0.30262 0.52334 1.00000 0.02330 0.02442 0.02505 -0.00042 0.00192 0.00017 0.02427 0.00298 0.00012 0.00016 0.00008 0.00000 0.00079 0.00085 0.00081 0.00067 0.00064 0.00066 0.00035 H29 -0.05431 0.33144 0.53587 1.00000 0.02913 0.00000 0.00000 C30 -0.18306 0.30513 0.56899 1.00000 0.03274 0.02698 0.02126 -0.00086 0.00451 0.00417 0.02687 0.00317 0.00012 0.00017 0.00008 0.00000 0.00091 0.00091 0.00079 0.00067 0.00068 0.00072 0.00037 H30 -0.16555 0.33618 0.61168 1.00000 0.03224 0.00000 0.00000 C31 -0.27443 0.26240 0.55220 1.00000 0.02838 0.03016 0.02585 0.00402 0.01078 0.00942 0.02762 0.00332 0.00012 0.00018 0.00008 0.00000 0.00087 0.00094 0.00083 0.00071 0.00068 0.00073 0.00038 H31 -0.31967 0.26337 0.58327 1.00000 0.03315 0.00000 0.00000 C32 -0.29917 0.21823 0.48961 1.00000 0.01949 0.03495 0.02823 0.00486 0.00423 0.00361 0.02743 0.00327 0.00012 0.00018 0.00008 0.00000 0.00077 0.00098 0.00086 0.00075 0.00065 0.00070 0.00037 H32 -0.36155 0.18825 0.47768 1.00000 0.03292 0.00000 0.00000 C33 -0.23278 0.21775 0.44428 1.00000 0.02272 0.03210 0.02190 0.00066 0.00157 0.00237 0.02561 0.00309 0.00011 0.00018 0.00008 0.00000 0.00080 0.00094 0.00078 0.00069 0.00063 0.00070 0.00036 H33 -0.25134 0.18847 0.40142 1.00000 0.03073 0.00000 0.00000 C34 -0.05722 0.40458 0.37066 1.00000 0.01939 0.02772 0.01956 -0.00288 0.00209 -0.00019 0.02220 0.00284 0.00011 0.00017 0.00008 0.00000 0.00074 0.00086 0.00075 0.00065 0.00059 0.00064 0.00033 C35 -0.11903 0.50608 0.38053 1.00000 0.02427 0.03173 0.02532 0.00007 0.00577 0.00392 0.02689 0.00315 0.00012 0.00018 0.00008 0.00000 0.00082 0.00095 0.00085 0.00071 0.00066 0.00071 0.00037 H35 -0.16648 0.49324 0.40938 1.00000 0.03227 0.00000 0.00000 C36 -0.11381 0.62562 0.34967 1.00000 0.03520 0.02905 0.03303 0.00170 0.00477 0.00990 0.03233 0.00347 0.00013 0.00019 0.00009 0.00000 0.00097 0.00098 0.00095 0.00077 0.00076 0.00078 0.00041 H36 -0.15783 0.69221 0.35706 1.00000 0.03879 0.00000 0.00000 C37 -0.04445 0.64733 0.30824 1.00000 0.03782 0.02791 0.02707 0.00414 0.00104 0.00140 0.03105 0.00329 0.00013 0.00018 0.00009 0.00000 0.00098 0.00094 0.00089 0.00073 0.00074 0.00078 0.00040 H37 -0.04039 0.72887 0.28715 1.00000 0.03726 0.00000 0.00000 C38 0.01905 0.54928 0.29774 1.00000 0.03052 0.03511 0.02533 0.00080 0.00876 -0.00041 0.02994 0.00327 0.00013 0.00019 0.00008 0.00000 0.00091 0.00101 0.00085 0.00075 0.00070 0.00077 0.00039 H38 0.06729 0.56361 0.26966 1.00000 0.03593 0.00000 0.00000 C39 0.01216 0.43015 0.32824 1.00000 0.02756 0.02828 0.02814 -0.00178 0.00869 0.00346 0.02761 0.00317 0.00012 0.00018 0.00008 0.00000 0.00086 0.00092 0.00087 0.00071 0.00069 0.00072 0.00037 H39 0.05587 0.36360 0.32017 1.00000 0.03314 0.00000 0.00000 B21 -0.06859 0.26166 0.40169 1.00000 0.01721 0.02527 0.02218 -0.00207 0.00128 0.00165 0.02158 0.00326 0.00012 0.00019 0.00009 0.00000 0.00081 0.00095 0.00085 0.00072 0.00066 0.00070 0.00037 N21 0.03823 0.21434 0.43284 1.00000 0.01816 0.02380 0.02072 -0.00174 0.00329 -0.00088 0.02080 0.00234 0.00009 0.00013 0.00006 0.00000 0.00063 0.00071 0.00064 0.00055 0.00050 0.00054 0.00028 O21 -0.09633 0.17084 0.34943 1.00000 0.02142 0.02620 0.02150 -0.00214 0.00189 -0.00094 0.02305 0.00196 0.00008 0.00011 0.00005 0.00000 0.00055 0.00062 0.00056 0.00047 0.00043 0.00047 0.00025 Final Structure Factor Calculation for 2006src1540 in P2(1)/c Total number of l.s. parameters = 398 Maximum vector length = 511 Memory required = 4607 / 24017 wR2 = 0.1113 before cycle 21 for 6886 data and 0 / 398 parameters GooF = S = 1.097; Restrained GooF = 1.097 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0100 * P )^2 + 2.49 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0518 for 5640 Fo > 4sig(Fo) and 0.0678 for all 6886 data wR2 = 0.1113, GooF = S = 1.097, Restrained GooF = 1.097 for all data Occupancy sum of asymmetric unit = 44.00 for non-hydrogen and 36.00 for hydrogen atoms Principal mean square atomic displacements U 0.0317 0.0267 0.0161 C1 0.0374 0.0335 0.0191 C2 0.0285 0.0216 0.0185 C3 0.0394 0.0312 0.0209 C4 0.0459 0.0293 0.0192 C5 0.0351 0.0230 0.0213 C6 0.0255 0.0216 0.0182 C7 0.0244 0.0208 0.0143 C8 0.0291 0.0238 0.0201 C9 0.0343 0.0287 0.0184 C10 0.0399 0.0204 0.0162 C11 0.0323 0.0196 0.0183 C12 0.0235 0.0216 0.0166 C13 0.0235 0.0205 0.0140 C14 0.0239 0.0213 0.0188 C15 0.0324 0.0202 0.0179 C16 0.0384 0.0218 0.0177 C17 0.0338 0.0276 0.0195 C18 0.0248 0.0231 0.0202 C19 0.0200 0.0186 0.0180 B1 0.0212 0.0202 0.0150 N1 0.0267 0.0215 0.0186 O1 0.0336 0.0253 0.0192 C21 0.0347 0.0299 0.0212 C22 0.0264 0.0229 0.0188 C23 0.0328 0.0289 0.0212 C24 0.0443 0.0290 0.0197 C25 0.0438 0.0277 0.0198 C26 0.0331 0.0229 0.0215 C27 0.0255 0.0213 0.0194 C28 0.0254 0.0242 0.0233 C29 0.0350 0.0255 0.0201 C30 0.0423 0.0239 0.0166 C31 0.0382 0.0257 0.0184 C32 0.0327 0.0227 0.0215 C33 0.0286 0.0195 0.0185 C34 0.0336 0.0270 0.0201 C35 0.0428 0.0324 0.0218 C36 0.0384 0.0316 0.0231 C37 0.0352 0.0341 0.0205 C38 0.0337 0.0298 0.0194 C39 0.0267 0.0211 0.0169 B21 0.0248 0.0203 0.0173 N21 0.0271 0.0215 0.0205 O21 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.010 0.019 0.028 0.039 0.051 0.065 0.083 0.108 0.153 1.000 Number in group 766. 654. 661. 692. 704. 697. 672. 662. 696. 682. GooF 1.175 1.177 1.214 1.204 1.056 1.099 0.961 1.022 0.936 1.083 K 3.072 1.202 1.083 1.039 0.993 1.011 1.003 1.000 1.005 1.006 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.65 inf Number in group 705. 692. 678. 690. 695. 676. 680. 696. 680. 694. GooF 1.271 1.176 1.166 1.058 1.041 1.051 0.998 0.962 1.064 1.145 K 1.109 1.061 1.032 1.007 0.993 0.991 0.989 0.984 1.008 1.011 R1 0.154 0.140 0.121 0.097 0.086 0.070 0.050 0.040 0.046 0.027 Recommended weighting scheme: WGHT 0.0000 2.4911 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 9 0 116.02 0.03 5.36 0.001 1.11 9 0 6 580.56 266.60 5.08 0.087 1.38 -7 0 14 775.30 337.72 4.49 0.097 1.25 12 0 12 80.63 20.06 4.20 0.024 0.93 0 6 12 92.18 26.13 4.13 0.027 1.21 -3 0 18 113.57 26.60 4.02 0.027 1.14 -6 4 3 3968.57 3389.32 3.94 0.309 1.71 -4 8 20 31.24 0.88 3.65 0.005 0.80 -7 2 24 201.03 111.37 3.60 0.056 0.81 3 12 6 40.62 105.26 3.57 0.054 0.82 7 0 4 5061.39 4357.97 3.57 0.350 1.83 -9 2 22 109.66 44.56 3.53 0.035 0.83 0 2 11 7.43 43.14 3.48 0.035 1.76 -7 7 8 27.13 0.08 3.37 0.001 1.10 9 11 5 40.91 1.49 3.34 0.006 0.78 6 0 18 215.99 133.12 3.32 0.061 0.99 -16 1 5 40.19 98.81 3.28 0.053 0.88 9 1 20 -4.39 20.61 3.27 0.024 0.82 -5 10 3 23.30 0.00 3.21 0.000 0.96 8 8 15 525.70 371.35 3.19 0.102 0.81 6 6 0 46.33 16.34 3.17 0.021 1.39 12 7 5 -8.41 23.28 3.17 0.026 0.88 8 7 15 65.47 134.91 3.16 0.062 0.85 -8 6 14 28.97 0.16 3.12 0.002 0.98 -17 1 11 107.75 46.50 3.10 0.036 0.79 13 3 16 50.50 1.37 3.10 0.006 0.78 -5 10 16 131.16 71.94 3.06 0.045 0.79 3 0 18 30.93 4.32 3.05 0.011 1.09 4 9 13 42.04 6.09 3.04 0.013 0.89 11 3 16 146.47 228.54 3.04 0.080 0.84 -6 0 12 2072.40 1437.70 3.03 0.201 1.45 3 1 25 69.40 24.86 3.00 0.026 0.80 6 9 14 5.09 38.56 2.99 0.033 0.83 -7 2 16 6.23 35.82 2.99 0.032 1.11 10 3 17 48.33 10.98 2.98 0.018 0.85 6 9 6 29.31 0.25 2.97 0.003 0.98 7 0 0 4846.22 4153.06 2.96 0.342 2.02 -10 8 5 24.47 2.13 2.96 0.008 0.94 4 10 6 94.83 165.33 2.93 0.068 0.94 0 7 7 751.83 589.19 2.90 0.129 1.32 -6 2 23 50.28 16.92 2.90 0.022 0.85 9 9 2 28.59 1.64 2.88 0.007 0.92 -6 3 12 60.53 26.81 2.88 0.027 1.34 -9 9 13 30.87 83.16 2.87 0.048 0.82 -2 10 13 43.62 9.02 2.86 0.016 0.86 12 2 4 183.04 259.50 2.85 0.085 1.10 -2 5 8 41.90 13.74 2.83 0.020 1.59 -5 2 21 29.33 69.34 2.82 0.044 0.94 -11 10 7 107.41 52.55 2.82 0.038 0.79 10 5 18 52.05 11.76 2.81 0.018 0.79 Bond lengths and angles C1 - Distance Angles O1 1.4133 (0.0019) C2 1.5160 (0.0024) 109.48 (0.13) H1A 0.9900 109.78 109.78 H1B 0.9900 109.78 109.78 108.23 C1 - O1 C2 H1A C2 - Distance Angles C3 1.4978 (0.0024) C1 1.5160 (0.0024) 112.41 (0.14) H2A 0.9900 109.12 109.12 H2B 0.9900 109.12 109.12 107.85 C2 - C3 C1 H2A C3 - Distance Angles N1 1.3504 (0.0021) C4 1.3932 (0.0024) 119.79 (0.16) C2 1.4978 (0.0024) 118.60 (0.14) 121.61 (0.16) C3 - N1 C4 C4 - Distance Angles C5 1.3779 (0.0027) C3 1.3932 (0.0024) 120.65 (0.17) H4 0.9500 119.68 119.68 C4 - C5 C3 C5 - Distance Angles C4 1.3779 (0.0027) C6 1.3823 (0.0026) 118.87 (0.16) H5 0.9500 120.56 120.56 C5 - C4 C6 C6 - Distance Angles C7 1.3759 (0.0023) C5 1.3823 (0.0026) 118.48 (0.16) H6 0.9500 120.76 120.76 C6 - C7 C5 C7 - Distance Angles N1 1.3473 (0.0020) C6 1.3759 (0.0023) 122.82 (0.16) H7 0.9500 118.59 118.59 C7 - N1 C6 C8 - Distance Angles C13 1.3964 (0.0022) C9 1.4063 (0.0022) 115.79 (0.14) B1 1.6301 (0.0023) 125.62 (0.14) 118.46 (0.14) C8 - C13 C9 C9 - Distance Angles C10 1.3896 (0.0023) C8 1.4063 (0.0022) 122.27 (0.16) H9 0.9500 118.87 118.87 C9 - C10 C8 C10 - Distance Angles C11 1.3864 (0.0024) C9 1.3896 (0.0023) 120.34 (0.16) H10 0.9500 119.83 119.83 C10 - C11 C9 C11 - Distance Angles C12 1.3851 (0.0024) C10 1.3864 (0.0024) 119.04 (0.15) H11 0.9500 120.48 120.48 C11 - C12 C10 C12 - Distance Angles C11 1.3851 (0.0024) C13 1.3975 (0.0022) 119.99 (0.15) H12 0.9500 120.00 120.00 C12 - C11 C13 C13 - Distance Angles C8 1.3964 (0.0022) C12 1.3975 (0.0022) 122.51 (0.15) H13 0.9500 118.74 118.74 C13 - C8 C12 C14 - Distance Angles C15 1.3988 (0.0022) C19 1.4026 (0.0022) 116.49 (0.15) B1 1.6188 (0.0023) 124.48 (0.14) 119.03 (0.14) C14 - C15 C19 C15 - Distance Angles C16 1.3921 (0.0023) C14 1.3988 (0.0022) 122.07 (0.15) H15 0.9500 118.97 118.97 C15 - C16 C14 C16 - Distance Angles C17 1.3828 (0.0024) C15 1.3921 (0.0023) 120.03 (0.16) H16 0.9500 119.99 119.99 C16 - C17 C15 C17 - Distance Angles C16 1.3828 (0.0024) C18 1.3856 (0.0025) 119.31 (0.16) H17 0.9500 120.35 120.35 C17 - C16 C18 C18 - Distance Angles C17 1.3856 (0.0025) C19 1.3884 (0.0023) 120.37 (0.16) H18 0.9500 119.82 119.82 C18 - C17 C19 C19 - Distance Angles C18 1.3884 (0.0023) C14 1.4026 (0.0022) 121.73 (0.16) H19 0.9500 119.13 119.13 C19 - C18 C14 B1 - Distance Angles O1 1.4500 (0.0021) C14 1.6188 (0.0023) 108.54 (0.13) C8 1.6301 (0.0023) 113.18 (0.13) 114.56 (0.13) N1 1.6699 (0.0021) 106.97 (0.12) 107.30 (0.12) 105.83 (0.12) B1 - O1 C14 C8 N1 - Distance Angles C7 1.3473 (0.0020) C3 1.3504 (0.0021) 119.38 (0.14) B1 1.6699 (0.0021) 117.81 (0.13) 122.64 (0.13) N1 - C7 C3 O1 - Distance Angles C1 1.4133 (0.0019) B1 1.4500 (0.0021) 114.06 (0.12) O1 - C1 C21 - Distance Angles O21 1.4159 (0.0021) C22 1.5122 (0.0024) 110.01 (0.14) H21A 0.9900 109.66 109.66 H21B 0.9900 109.66 109.66 108.16 C21 - O21 C22 H21A C22 - Distance Angles C23 1.5039 (0.0023) C21 1.5122 (0.0024) 113.28 (0.14) H22A 0.9900 108.92 108.92 H22B 0.9900 108.92 108.92 107.74 C22 - C23 C21 H22A C23 - Distance Angles N21 1.3528 (0.0021) C24 1.3898 (0.0023) 120.47 (0.15) C22 1.5039 (0.0023) 119.63 (0.14) 119.85 (0.16) C23 - N21 C24 C24 - Distance Angles C25 1.3743 (0.0025) C23 1.3898 (0.0023) 120.34 (0.17) H24 0.9500 119.83 119.83 C24 - C25 C23 C25 - Distance Angles C24 1.3743 (0.0025) C26 1.3831 (0.0027) 118.89 (0.16) H25 0.9500 120.55 120.55 C25 - C24 C26 C26 - Distance Angles C27 1.3758 (0.0024) C25 1.3831 (0.0027) 118.80 (0.16) H26 0.9500 120.60 120.60 C26 - C27 C25 C27 - Distance Angles N21 1.3503 (0.0021) C26 1.3758 (0.0024) 122.58 (0.17) H27 0.9500 118.71 118.71 C27 - N21 C26 C28 - Distance Angles C29 1.4012 (0.0022) C33 1.4042 (0.0023) 115.98 (0.15) B21 1.6320 (0.0024) 125.60 (0.14) 118.29 (0.14) C28 - C29 C33 C29 - Distance Angles C30 1.3937 (0.0023) C28 1.4012 (0.0022) 122.22 (0.16) H29 0.9500 118.89 118.89 C29 - C30 C28 C30 - Distance Angles C31 1.3852 (0.0025) C29 1.3937 (0.0023) 120.07 (0.16) H30 0.9500 119.96 119.96 C30 - C31 C29 C31 - Distance Angles C30 1.3852 (0.0025) C32 1.3860 (0.0024) 119.34 (0.15) H31 0.9500 120.33 120.33 C31 - C30 C32 C32 - Distance Angles C31 1.3860 (0.0024) C33 1.3900 (0.0023) 120.05 (0.16) H32 0.9500 119.98 119.98 C32 - C31 C33 C33 - Distance Angles C32 1.3900 (0.0023) C28 1.4042 (0.0023) 122.33 (0.16) H33 0.9500 118.83 118.83 C33 - C32 C28 C34 - Distance Angles C35 1.3924 (0.0023) C39 1.4037 (0.0022) 116.12 (0.16) B21 1.6190 (0.0025) 122.44 (0.14) 121.29 (0.15) C34 - C35 C39 C35 - Distance Angles C36 1.3911 (0.0025) C34 1.3924 (0.0023) 122.38 (0.16) H35 0.9500 118.81 118.81 C35 - C36 C34 C36 - Distance Angles C37 1.3826 (0.0026) C35 1.3911 (0.0025) 119.88 (0.17) H36 0.9500 120.06 120.06 C36 - C37 C35 C37 - Distance Angles C36 1.3826 (0.0026) C38 1.3846 (0.0026) 119.46 (0.17) H37 0.9500 120.27 120.27 C37 - C36 C38 C38 - Distance Angles C37 1.3846 (0.0026) C39 1.3865 (0.0025) 119.94 (0.16) H38 0.9500 120.03 120.03 C38 - C37 C39 C39 - Distance Angles C38 1.3865 (0.0025) C34 1.4037 (0.0022) 122.20 (0.16) H39 0.9500 118.90 118.90 C39 - C38 C34 B21 - Distance Angles O21 1.4555 (0.0021) C34 1.6190 (0.0025) 108.64 (0.13) C28 1.6320 (0.0024) 112.99 (0.14) 113.35 (0.14) N21 1.6672 (0.0022) 105.91 (0.13) 107.33 (0.13) 108.21 (0.13) B21 - O21 C34 C28 N21 - Distance Angles C27 1.3503 (0.0021) C23 1.3528 (0.0021) 118.88 (0.14) B21 1.6672 (0.0022) 119.27 (0.14) 121.83 (0.13) N21 - C27 C23 O21 - Distance Angles C21 1.4159 (0.0021) B21 1.4555 (0.0021) 113.46 (0.13) O21 - C21 FMAP and GRID set by program FMAP 2 1 33 GRID -1.667 -2 -1 1.667 2 1 R1 = 0.0678 for 6886 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.36 at 0.4431 0.3367 0.1359 [ 0.79 A from C14 ] Deepest hole -0.21 at 0.3183 0.8658 0.2988 [ 1.25 A from C6 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 4613 / 44901 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4431 0.3367 0.1359 1.00000 0.05 0.36 0.79 C14 0.83 B1 1.91 O1 1.92 C15 Q2 1 0.4349 0.4009 0.1939 1.00000 0.05 0.31 0.75 C8 0.89 B1 1.91 C9 1.92 C13 Q3 1 0.0376 0.0526 0.3998 1.00000 0.05 0.25 0.74 C22 0.78 C23 1.39 H22B 1.49 H22A Q4 1 -0.1039 0.2598 0.4322 1.00000 0.05 0.25 0.79 C28 0.84 B21 1.92 C33 1.95 O21 Q5 1 -0.2625 0.1882 0.4672 1.00000 0.05 0.24 0.73 C33 0.79 C32 1.38 H33 1.45 H32 Shortest distances between peaks (including symmetry equivalents) 1 2 1.38 4 5 2.54 Time profile in seconds ----------------------- 0.06: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.00: 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. 3.65: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.04: Set up l.s. refinement 0.00: Generate idealized H-atoms 14.27: Structure factors and derivatives 33.28: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.09: Apply other restraints 3.11: Solve l.s. equations 0.00: Generate HTAB table 0.10: Other dependent quantities, CIF, tables 0.17: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.12: Fourier summations 0.07: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2006src1540 finished at 13:02:17 Total CPU time: 55.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++