+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src1054 started at 15:33:05 on 03-Aug-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src1054 in P-1 CELL 0.71073 9.7504 10.2281 14.0530 95.766 107.842 96.617 ZERR 6.00 0.0003 0.0003 0.0005 0.002 0.002 0.002 LATT 1 SFAC C H N O UNIT 66 66 6 6 V = 1311.45 F(000) = 552.0 Mu = 0.08 mm-1 Cell Wt = 1039.25 Rho = 1.316 MERG 2 OMIT -3.00 55.00 OMIT 0 3 0 SHEL 7 0.77 EQIV $1 -x+2, -y, -z+1 EQIV $2 x+1, y, z+1 EQIV $3 x-1, y, z-1 HTAB N1 O1_$1 HTAB N101 O201_$2 HTAB N201 O101_$3 ACTA BOND $H SIZE 0.3 0.08 0.04 FMAP 2 PLAN 10 WGHT 0.02140 2.33100 L.S. 20 TEMP -153.00 FVAR 0.64896 MOLE 1 C1 1 0.914651 0.001524 0.348399 11.00000 0.02266 0.01591 = 0.01719 0.00086 0.00471 0.00254 C2 1 0.814492 0.003000 0.242478 11.00000 0.01958 0.01788 = 0.01530 0.00312 0.00125 0.00304 C3 1 0.669248 0.008048 0.252534 11.00000 0.02043 0.01884 = 0.01453 0.00256 0.00298 0.00382 C4 1 0.685122 0.009074 0.355372 11.00000 0.01896 0.02058 = 0.01715 0.00260 0.00203 0.00283 C5 1 0.569490 0.009831 0.392570 11.00000 0.02433 0.03237 = 0.01725 0.00260 0.00615 0.00196 AFIX 43 H5 2 0.583604 0.011253 0.462644 11.00000 -1.20000 AFIX 0 C6 1 0.431447 0.008440 0.323868 11.00000 0.02139 0.03374 = 0.02755 0.00408 0.00648 0.00613 AFIX 43 H6 2 0.349677 0.008829 0.347116 11.00000 -1.20000 AFIX 0 C7 1 0.412534 0.006496 0.222031 11.00000 0.01652 0.03524 = 0.02263 0.00369 -0.00167 0.00460 AFIX 43 H7 2 0.317527 0.004920 0.176158 11.00000 -1.20000 AFIX 0 C8 1 0.530386 0.006806 0.185469 11.00000 0.02413 0.03062 = 0.01423 0.00262 0.00090 0.00672 AFIX 43 H8 2 0.515912 0.006176 0.115415 11.00000 -1.20000 AFIX 0 C9 1 0.855934 0.000248 0.159060 11.00000 0.02288 0.01873 = 0.02058 0.00220 0.00498 0.00127 C10 1 0.750864 0.008552 0.057064 11.00000 0.02787 0.03502 = 0.01453 0.00498 0.00364 0.00597 AFIX 137 H10A 2 0.669216 -0.064636 0.039612 11.00000 -1.50000 H10B 2 0.800855 0.002077 0.006363 11.00000 -1.50000 H10C 2 0.713965 0.093632 0.058667 11.00000 -1.50000 AFIX 0 C11 1 1.008272 -0.011435 0.159548 11.00000 0.02308 0.04399 = 0.02027 0.00540 0.00652 0.00322 AFIX 137 H11A 2 1.070598 -0.013234 0.228795 11.00000 -1.50000 H11B 2 1.046470 0.064988 0.133325 11.00000 -1.50000 H11C 2 1.007155 -0.093682 0.116843 11.00000 -1.50000 AFIX 0 N1 3 0.830251 0.006700 0.409690 11.00000 0.01826 0.02882 = 0.01281 0.00376 0.00043 0.00343 AFIX 43 H1 2 0.863490 0.008340 0.475579 11.00000 -1.20000 AFIX 0 O1 4 1.046942 -0.000819 0.378387 11.00000 0.02044 0.02767 = 0.01838 0.00430 0.00242 0.00405 MOLE 2 C101 1 1.180409 0.313364 0.675007 11.00000 0.02278 0.01744 = 0.01563 0.00330 0.00451 0.00176 C102 1 1.082184 0.317222 0.569300 11.00000 0.02099 0.01850 = 0.01687 0.00379 0.00350 0.00356 C103 1 0.936263 0.321295 0.578641 11.00000 0.02113 0.01770 = 0.01845 0.00269 0.00555 0.00348 C104 1 0.950185 0.319011 0.681066 11.00000 0.02218 0.02124 = 0.01758 0.00247 0.00253 0.00403 C105 1 0.834033 0.320188 0.717404 11.00000 0.02496 0.03356 = 0.01951 0.00370 0.00784 0.00654 AFIX 43 H105 2 0.847161 0.319006 0.787129 11.00000 -1.20000 AFIX 0 C106 1 0.697346 0.323149 0.649291 11.00000 0.02435 0.03540 = 0.02505 0.00317 0.00970 0.00447 AFIX 43 H106 2 0.615488 0.323978 0.672405 11.00000 -1.20000 AFIX 0 C107 1 0.679596 0.324904 0.547719 11.00000 0.02362 0.03433 = 0.02650 0.00459 0.00340 0.00543 AFIX 43 H107 2 0.585415 0.326912 0.501946 11.00000 -1.20000 AFIX 0 C108 1 0.798348 0.323763 0.511522 11.00000 0.02562 0.03202 = 0.02054 0.00355 0.00418 0.00479 AFIX 43 H108 2 0.784783 0.324668 0.441716 11.00000 -1.20000 AFIX 0 C109 1 1.127559 0.319015 0.487384 11.00000 0.02401 0.02081 = 0.01844 0.00332 0.00516 0.00509 C110 1 1.027605 0.334657 0.385552 11.00000 0.03614 0.03843 = 0.01838 0.00609 0.00610 0.00673 AFIX 137 H11D 2 0.970236 0.248184 0.351609 11.00000 -1.50000 H11E 2 1.085452 0.368689 0.344782 11.00000 -1.50000 H11F 2 0.961833 0.397317 0.393745 11.00000 -1.50000 AFIX 0 C111 1 1.279749 0.305406 0.489642 11.00000 0.03013 0.03654 = 0.02391 0.00781 0.01207 0.00716 AFIX 137 H11G 2 1.333887 0.281196 0.554915 11.00000 -1.50000 H11H 2 1.328372 0.390142 0.480207 11.00000 -1.50000 H11I 2 1.276596 0.235974 0.435283 11.00000 -1.50000 AFIX 0 N101 3 1.095201 0.315270 0.735316 11.00000 0.01961 0.03005 = 0.01399 0.00481 0.00261 0.00533 AFIX 43 H101 2 1.127710 0.314263 0.800932 11.00000 -1.20000 AFIX 0 O101 4 1.312970 0.311694 0.706094 11.00000 0.01804 0.03234 = 0.02036 0.00399 0.00306 0.00544 MOLE 3 C201 1 0.346962 0.325027 -0.021125 11.00000 0.02456 0.01789 = 0.01765 0.00283 0.00610 0.00267 C202 1 0.447883 0.341659 0.086299 11.00000 0.01992 0.01761 = 0.01805 0.00251 0.00234 0.00332 C203 1 0.595913 0.347948 0.078704 11.00000 0.02122 0.01862 = 0.01792 0.00208 0.00375 0.00150 C204 1 0.580378 0.332962 -0.024932 11.00000 0.02209 0.01918 = 0.01987 0.00453 0.00618 0.00541 C205 1 0.697447 0.334507 -0.060253 11.00000 0.02644 0.02896 = 0.01868 0.00657 0.00789 0.00463 AFIX 43 H205 2 0.683492 0.323012 -0.130688 11.00000 -1.20000 AFIX 0 C206 1 0.836663 0.353337 0.009874 11.00000 0.02115 0.02995 = 0.02821 0.00523 0.01052 0.00313 AFIX 43 H206 2 0.919372 0.355767 -0.012520 11.00000 -1.20000 AFIX 0 C207 1 0.855168 0.368616 0.112661 11.00000 0.02087 0.03128 = 0.02799 0.00369 0.00352 0.00214 AFIX 43 H207 2 0.950866 0.381254 0.159808 11.00000 -1.20000 AFIX 0 C208 1 0.736253 0.365761 0.147852 11.00000 0.02682 0.02738 = 0.01745 0.00248 0.00413 0.00466 AFIX 43 H208 2 0.750598 0.375857 0.218333 11.00000 -1.20000 AFIX 0 C209 1 0.405157 0.348453 0.169284 11.00000 0.02395 0.01773 = 0.01814 0.00208 0.00566 0.00106 C210 1 0.512814 0.365511 0.274392 11.00000 0.02456 0.03990 = 0.01585 0.00261 0.00198 -0.00017 AFIX 137 H21A 2 0.568392 0.291074 0.281098 11.00000 -1.50000 H21B 2 0.460331 0.367383 0.323748 11.00000 -1.50000 H21C 2 0.579745 0.449171 0.286698 11.00000 -1.50000 AFIX 0 C211 1 0.248572 0.340801 0.165024 11.00000 0.02591 0.03952 = 0.02027 0.00109 0.00818 0.00243 AFIX 137 H21D 2 0.185701 0.326126 0.094353 11.00000 -1.50000 H21E 2 0.234639 0.424317 0.198980 11.00000 -1.50000 H21F 2 0.223216 0.266969 0.198958 11.00000 -1.50000 AFIX 0 N201 3 0.432758 0.318369 -0.081135 11.00000 0.02015 0.02761 = 0.01456 0.00434 0.00273 0.00553 AFIX 43 H201 2 0.399158 0.306285 -0.147575 11.00000 -1.20000 AFIX 0 O201 4 0.212742 0.315151 -0.053344 11.00000 0.01694 0.03138 = 0.02010 0.00375 0.00241 0.00446 HKLF 4 Covalent radii and connectivity table for 2007src1054 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1 N1 C2 C2 - C9 C3 C1 C3 - C8 C4 C2 C4 - C5 N1 C3 C5 - C4 C6 C6 - C7 C5 C7 - C6 C8 C8 - C3 C7 C9 - C2 C11 C10 C10 - C9 C11 - C9 N1 - C1 C4 O1 - C1 C101 - O101 N101 C102 C102 - C109 C103 C101 C103 - C108 C104 C102 C104 - C105 N101 C103 C105 - C104 C106 C106 - C107 C105 C107 - C106 C108 C108 - C103 C107 C109 - C102 C111 C110 C110 - C109 C111 - C109 N101 - C101 C104 O101 - C101 C201 - O201 N201 C202 C202 - C209 C203 C201 C203 - C208 C204 C202 C204 - C205 N201 C203 C205 - C204 C206 C206 - C207 C205 C207 - C206 C208 C208 - C207 C203 C209 - C202 C211 C210 C210 - C209 C211 - C209 N201 - C201 C204 O201 - C201 Operators for generating equivalent atoms: $1 -x+2, -y, -z+1 $2 x+1, y, z+1 $3 x-1, y, z-1 21431 Reflections read, of which 41 rejected -12 =< h =< 12, -12 =< k =< 13, -18 =< l =< 18, Max. 2-theta = 54.96 0 Systematic absence violations 0 Inconsistent equivalents 5972 Unique reflections, of which 0 suppressed R(int) = 0.0592 R(sigma) = 0.0674 Friedel opposites merged Maximum memory for data reduction = 3586 / 59762 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 = 4607 / 453848 wR2 = 0.1681 before cycle 1 for 5972 data and 358 / 358 parameters GooF = S = 1.078; Restrained GooF = 1.078 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0214 * P )^2 + 2.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64897 0.00136 0.006 OSF Mean shift/esd = 0.002 Maximum = 0.006 for z C111 Max. shift = 0.000 A for H10C Max. dU = 0.000 for C9 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4607 / 453848 wR2 = 0.1681 before cycle 2 for 5972 data and 358 / 358 parameters GooF = S = 1.078; Restrained GooF = 1.078 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0214 * P )^2 + 2.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64897 0.00136 -0.001 OSF Mean shift/esd = 0.001 Maximum = 0.004 for tors H10A Max. shift = 0.000 A for H10B Max. dU = 0.000 for C9 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4607 / 453848 wR2 = 0.1681 before cycle 3 for 5972 data and 358 / 358 parameters GooF = S = 1.078; Restrained GooF = 1.078 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0214 * P )^2 + 2.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64897 0.00136 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.002 for tors H11D Max. shift = 0.000 A for H11D Max. dU = 0.000 for C203 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4607 / 453848 wR2 = 0.1681 before cycle 4 for 5972 data and 358 / 358 parameters GooF = S = 1.078; Restrained GooF = 1.078 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0214 * P )^2 + 2.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64897 0.00136 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.002 for tors H11D Max. shift = 0.000 A for H11D Max. dU = 0.000 for C204 Least-squares cycle 5 Maximum vector length = 511 Memory required = 4607 / 453848 wR2 = 0.1681 before cycle 5 for 5972 data and 358 / 358 parameters GooF = S = 1.078; Restrained GooF = 1.078 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0214 * P )^2 + 2.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64897 0.00136 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for tors H11D Max. shift = 0.000 A for H11D Max. dU = 0.000 for C109 Least-squares cycle 6 Maximum vector length = 511 Memory required = 4607 / 453848 wR2 = 0.1681 before cycle 6 for 5972 data and 358 / 358 parameters GooF = S = 1.078; Restrained GooF = 1.078 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0214 * P )^2 + 2.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64897 0.00136 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for tors H11D Max. shift = 0.000 A for H11F Max. dU = 0.000 for C202 Least-squares cycle 7 Maximum vector length = 511 Memory required = 4607 / 453848 wR2 = 0.1681 before cycle 7 for 5972 data and 358 / 358 parameters GooF = S = 1.078; Restrained GooF = 1.078 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0214 * P )^2 + 2.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64897 0.00136 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for tors H11D Max. shift = 0.000 A for H11E Max. dU = 0.000 for C6 Least-squares cycle 8 Maximum vector length = 511 Memory required = 4607 / 453848 wR2 = 0.1681 before cycle 8 for 5972 data and 358 / 358 parameters GooF = S = 1.078; Restrained GooF = 1.078 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0214 * P )^2 + 2.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64897 0.00136 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for tors H11D Max. shift = 0.000 A for H11E Max. dU = 0.000 for C106 Least-squares cycle 9 Maximum vector length = 511 Memory required = 4607 / 453848 wR2 = 0.1681 before cycle 9 for 5972 data and 358 / 358 parameters GooF = S = 1.078; Restrained GooF = 1.078 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0214 * P )^2 + 2.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64897 0.00136 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for tors H11D Max. shift = 0.000 A for H11F Max. dU = 0.000 for C7 Least-squares cycle 10 Maximum vector length = 511 Memory required = 4607 / 453848 wR2 = 0.1681 before cycle 10 for 5972 data and 358 / 358 parameters GooF = S = 1.078; Restrained GooF = 1.078 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0214 * P )^2 + 2.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64897 0.00136 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O101 Max. shift = 0.000 A for H11E Max. dU = 0.000 for C10 Least-squares cycle 11 Maximum vector length = 511 Memory required = 4607 / 453848 wR2 = 0.1681 before cycle 11 for 5972 data and 358 / 358 parameters GooF = S = 1.078; Restrained GooF = 1.078 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0214 * P )^2 + 2.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64897 0.00136 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O101 Max. shift = 0.000 A for H11F Max. dU = 0.000 for C110 Least-squares cycle 12 Maximum vector length = 511 Memory required = 4607 / 453848 wR2 = 0.1681 before cycle 12 for 5972 data and 358 / 358 parameters GooF = S = 1.078; Restrained GooF = 1.078 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0214 * P )^2 + 2.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64897 0.00136 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x C102 Max. shift = 0.000 A for H11D Max. dU = 0.000 for O101 Least-squares cycle 13 Maximum vector length = 511 Memory required = 4607 / 453848 wR2 = 0.1681 before cycle 13 for 5972 data and 358 / 358 parameters GooF = S = 1.078; Restrained GooF = 1.078 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0214 * P )^2 + 2.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64897 0.00136 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O101 Max. shift = 0.000 A for H11F Max. dU = 0.000 for C110 Least-squares cycle 14 Maximum vector length = 511 Memory required = 4607 / 453848 wR2 = 0.1681 before cycle 14 for 5972 data and 358 / 358 parameters GooF = S = 1.078; Restrained GooF = 1.078 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0214 * P )^2 + 2.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64897 0.00136 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O101 Max. shift = 0.000 A for C106 Max. dU = 0.000 for O101 Least-squares cycle 15 Maximum vector length = 511 Memory required = 4607 / 453848 wR2 = 0.1681 before cycle 15 for 5972 data and 358 / 358 parameters GooF = S = 1.078; Restrained GooF = 1.078 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0214 * P )^2 + 2.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64897 0.00136 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H11F Max. dU = 0.000 for C106 Least-squares cycle 16 Maximum vector length = 511 Memory required = 4607 / 453848 wR2 = 0.1681 before cycle 16 for 5972 data and 358 / 358 parameters GooF = S = 1.078; Restrained GooF = 1.078 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0214 * P )^2 + 2.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64897 0.00136 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O101 Max. shift = 0.000 A for C101 Max. dU = 0.000 for C11 Least-squares cycle 17 Maximum vector length = 511 Memory required = 4607 / 453848 wR2 = 0.1681 before cycle 17 for 5972 data and 358 / 358 parameters GooF = S = 1.078; Restrained GooF = 1.078 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0214 * P )^2 + 2.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64897 0.00136 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x C102 Max. shift = 0.000 A for H11E Max. dU = 0.000 for C101 Least-squares cycle 18 Maximum vector length = 511 Memory required = 4607 / 453848 wR2 = 0.1681 before cycle 18 for 5972 data and 358 / 358 parameters GooF = S = 1.078; Restrained GooF = 1.078 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0214 * P )^2 + 2.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64897 0.00136 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O101 Max. shift = 0.000 A for H11E Max. dU = 0.000 for C105 Least-squares cycle 19 Maximum vector length = 511 Memory required = 4607 / 453848 wR2 = 0.1681 before cycle 19 for 5972 data and 358 / 358 parameters GooF = S = 1.078; Restrained GooF = 1.078 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0214 * P )^2 + 2.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64897 0.00136 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z O101 Max. shift = 0.000 A for C2 Max. dU = 0.000 for N1 Least-squares cycle 20 Maximum vector length = 511 Memory required = 4607 / 453848 wR2 = 0.1681 before cycle 20 for 5972 data and 358 / 358 parameters GooF = S = 1.078; Restrained GooF = 1.078 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0214 * P )^2 + 2.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.64897 0.00136 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x C102 Max. shift = 0.000 A for C4 Max. dU = 0.000 for C110 Largest correlation matrix elements 0.519 U13 C111 / U33 C111 0.504 U13 C111 / U11 C111 0.511 U13 C206 / U33 C206 0.503 U13 C206 / U11 C206 Idealized hydrogen atom generation before cycle 21 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H5 0.5836 0.0113 0.4626 43 0.950 0.000 C5 C4 C6 H6 0.3497 0.0088 0.3471 43 0.950 0.000 C6 C7 C5 H7 0.3175 0.0049 0.1762 43 0.950 0.000 C7 C6 C8 H8 0.5159 0.0062 0.1154 43 0.950 0.000 C8 C3 C7 H10A 0.6692 -0.0646 0.0396 137 0.980 0.000 C10 C9 H10A H10B 0.8008 0.0021 0.0064 137 0.980 0.000 C10 C9 H10A H10C 0.7140 0.0936 0.0587 137 0.980 0.000 C10 C9 H10A H11A 1.0706 -0.0132 0.2288 137 0.980 0.000 C11 C9 H11A H11B 1.0465 0.0650 0.1333 137 0.980 0.000 C11 C9 H11A H11C 1.0072 -0.0937 0.1168 137 0.980 0.000 C11 C9 H11A H1 0.8635 0.0083 0.4756 43 0.880 0.000 N1 C1 C4 H105 0.8472 0.3190 0.7871 43 0.950 0.000 C105 C104 C106 H106 0.6155 0.3240 0.6724 43 0.950 0.000 C106 C107 C105 H107 0.5854 0.3269 0.5019 43 0.950 0.000 C107 C106 C108 H108 0.7848 0.3247 0.4417 43 0.950 0.000 C108 C103 C107 H11D 0.9703 0.2482 0.3516 137 0.980 0.000 C110 C109 H11D H11E 1.0855 0.3687 0.3448 137 0.980 0.000 C110 C109 H11D H11F 0.9618 0.3973 0.3937 137 0.980 0.000 C110 C109 H11D H11G 1.3339 0.2812 0.5549 137 0.980 0.000 C111 C109 H11G H11H 1.3284 0.3901 0.4802 137 0.980 0.000 C111 C109 H11G H11I 1.2766 0.2360 0.4353 137 0.980 0.000 C111 C109 H11G H101 1.1277 0.3143 0.8009 43 0.880 0.000 N101 C101 C104 H205 0.6835 0.3230 -0.1307 43 0.950 0.000 C205 C204 C206 H206 0.9194 0.3558 -0.0125 43 0.950 0.000 C206 C207 C205 H207 0.9509 0.3813 0.1598 43 0.950 0.000 C207 C206 C208 H208 0.7506 0.3759 0.2183 43 0.950 0.000 C208 C207 C203 H21A 0.5684 0.2911 0.2811 137 0.980 0.000 C210 C209 H21A H21B 0.4603 0.3674 0.3237 137 0.980 0.000 C210 C209 H21A H21C 0.5797 0.4492 0.2867 137 0.980 0.000 C210 C209 H21A H21D 0.1857 0.3261 0.0944 137 0.980 0.000 C211 C209 H21D H21E 0.2346 0.4243 0.1990 137 0.980 0.000 C211 C209 H21D H21F 0.2232 0.2670 0.1990 137 0.980 0.000 C211 C209 H21D H201 0.3992 0.3063 -0.1476 43 0.880 0.000 N201 C201 C204 2007src1054 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.91465 0.00152 0.34840 1.00000 0.02267 0.01591 0.01719 0.00086 0.00471 0.00253 0.01913 0.00565 0.00030 0.00023 0.00020 0.00000 0.00156 0.00117 0.00132 0.00093 0.00117 0.00098 0.00055 C2 0.81449 0.00300 0.24248 1.00000 0.01958 0.01788 0.01530 0.00312 0.00125 0.00304 0.01852 0.00552 0.00029 0.00024 0.00019 0.00000 0.00144 0.00119 0.00130 0.00093 0.00113 0.00098 0.00054 C3 0.66925 0.00805 0.25253 1.00000 0.02042 0.01884 0.01454 0.00256 0.00298 0.00382 0.01846 0.00557 0.00029 0.00024 0.00019 0.00000 0.00146 0.00120 0.00129 0.00093 0.00113 0.00098 0.00054 C4 0.68512 0.00907 0.35537 1.00000 0.01896 0.02057 0.01715 0.00260 0.00203 0.00283 0.01979 0.00569 0.00029 0.00024 0.00020 0.00000 0.00147 0.00124 0.00134 0.00097 0.00114 0.00100 0.00055 C5 0.56949 0.00983 0.39257 1.00000 0.02433 0.03237 0.01725 0.00260 0.00614 0.00195 0.02505 0.00610 0.00031 0.00027 0.00021 0.00000 0.00160 0.00147 0.00140 0.00108 0.00125 0.00114 0.00061 H5 0.58360 0.01125 0.46264 1.00000 0.03006 0.00000 0.00000 C6 0.43145 0.00844 0.32387 1.00000 0.02139 0.03373 0.02755 0.00408 0.00648 0.00613 0.02775 0.00639 0.00032 0.00028 0.00022 0.00000 0.00160 0.00153 0.00161 0.00119 0.00133 0.00118 0.00064 H6 0.34968 0.00883 0.34711 1.00000 0.03329 0.00000 0.00000 C7 0.41253 0.00650 0.22203 1.00000 0.01652 0.03524 0.02262 0.00368 -0.00167 0.00460 0.02661 0.00621 0.00031 0.00028 0.00022 0.00000 0.00151 0.00153 0.00152 0.00115 0.00123 0.00113 0.00062 H7 0.31753 0.00492 0.17616 1.00000 0.03194 0.00000 0.00000 C8 0.53039 0.00681 0.18547 1.00000 0.02413 0.03062 0.01423 0.00262 0.00090 0.00672 0.02404 0.00596 0.00030 0.00027 0.00021 0.00000 0.00160 0.00144 0.00134 0.00104 0.00119 0.00114 0.00060 H8 0.51591 0.00618 0.11542 1.00000 0.02885 0.00000 0.00000 C9 0.85593 0.00025 0.15906 1.00000 0.02288 0.01872 0.02058 0.00220 0.00498 0.00127 0.02139 0.00573 0.00030 0.00024 0.00020 0.00000 0.00153 0.00123 0.00143 0.00099 0.00123 0.00102 0.00057 C10 0.75086 0.00855 0.05706 1.00000 0.02787 0.03503 0.01453 0.00498 0.00364 0.00597 0.02635 0.00619 0.00032 0.00028 0.00020 0.00000 0.00167 0.00154 0.00138 0.00109 0.00125 0.00120 0.00062 H10A 0.66920 -0.06462 0.03962 1.00000 0.03952 0.00000 0.00000 H10B 0.80085 0.00205 0.00636 1.00000 0.03952 0.00000 0.00000 H10C 0.71399 0.09364 0.05866 1.00000 0.03952 0.00000 0.00000 C11 1.00827 -0.01143 0.15955 1.00000 0.02308 0.04399 0.02027 0.00540 0.00652 0.00321 0.02932 0.00655 0.00032 0.00031 0.00022 0.00000 0.00163 0.00171 0.00151 0.00122 0.00129 0.00126 0.00065 H11A 1.07060 -0.01324 0.22879 1.00000 0.04398 0.00000 0.00000 H11B 1.04647 0.06499 0.13333 1.00000 0.04398 0.00000 0.00000 H11C 1.00716 -0.09368 0.11684 1.00000 0.04398 0.00000 0.00000 N1 0.83025 0.00670 0.40969 1.00000 0.01826 0.02882 0.01281 0.00376 0.00043 0.00343 0.02098 0.00480 0.00024 0.00021 0.00017 0.00000 0.00125 0.00118 0.00111 0.00086 0.00096 0.00090 0.00048 H1 0.86349 0.00834 0.47558 1.00000 0.02518 0.00000 0.00000 O1 1.04694 -0.00082 0.37839 1.00000 0.02044 0.02767 0.01838 0.00430 0.00242 0.00405 0.02295 0.00403 0.00020 0.00018 0.00014 0.00000 0.00112 0.00098 0.00100 0.00074 0.00085 0.00076 0.00042 C101 1.18041 0.31337 0.67501 1.00000 0.02278 0.01743 0.01563 0.00330 0.00451 0.00176 0.01904 0.00562 0.00030 0.00024 0.00019 0.00000 0.00154 0.00120 0.00132 0.00093 0.00116 0.00099 0.00055 C102 1.08218 0.31722 0.56930 1.00000 0.02099 0.01850 0.01687 0.00379 0.00351 0.00356 0.01925 0.00569 0.00029 0.00024 0.00020 0.00000 0.00146 0.00119 0.00133 0.00095 0.00115 0.00099 0.00054 C103 0.93626 0.32130 0.57864 1.00000 0.02113 0.01770 0.01845 0.00269 0.00554 0.00348 0.01923 0.00565 0.00029 0.00024 0.00019 0.00000 0.00149 0.00120 0.00137 0.00096 0.00118 0.00099 0.00055 C104 0.95019 0.31901 0.68106 1.00000 0.02219 0.02123 0.01759 0.00247 0.00254 0.00403 0.02119 0.00578 0.00030 0.00025 0.00020 0.00000 0.00152 0.00125 0.00138 0.00098 0.00120 0.00103 0.00057 C105 0.83403 0.32019 0.71740 1.00000 0.02496 0.03356 0.01950 0.00370 0.00784 0.00654 0.02569 0.00622 0.00031 0.00027 0.00021 0.00000 0.00162 0.00150 0.00144 0.00111 0.00127 0.00118 0.00061 H105 0.84716 0.31901 0.78713 1.00000 0.03083 0.00000 0.00000 C106 0.69734 0.32315 0.64929 1.00000 0.02435 0.03540 0.02505 0.00317 0.00970 0.00447 0.02796 0.00638 0.00033 0.00028 0.00022 0.00000 0.00164 0.00157 0.00159 0.00119 0.00133 0.00121 0.00064 H106 0.61549 0.32398 0.67240 1.00000 0.03355 0.00000 0.00000 C107 0.67960 0.32490 0.54772 1.00000 0.02362 0.03433 0.02649 0.00459 0.00340 0.00543 0.02913 0.00655 0.00033 0.00028 0.00023 0.00000 0.00163 0.00156 0.00160 0.00119 0.00132 0.00120 0.00065 H107 0.58542 0.32691 0.50195 1.00000 0.03495 0.00000 0.00000 C108 0.79835 0.32376 0.51152 1.00000 0.02562 0.03202 0.02054 0.00355 0.00418 0.00479 0.02680 0.00624 0.00032 0.00027 0.00022 0.00000 0.00166 0.00148 0.00147 0.00112 0.00129 0.00117 0.00062 H108 0.78478 0.32467 0.44172 1.00000 0.03216 0.00000 0.00000 C109 1.12756 0.31902 0.48738 1.00000 0.02401 0.02081 0.01844 0.00332 0.00516 0.00509 0.02130 0.00586 0.00030 0.00025 0.00020 0.00000 0.00153 0.00126 0.00138 0.00098 0.00119 0.00105 0.00057 C110 1.02761 0.33466 0.38555 1.00000 0.03614 0.03843 0.01838 0.00609 0.00610 0.00673 0.03137 0.00665 0.00035 0.00030 0.00021 0.00000 0.00185 0.00165 0.00148 0.00119 0.00137 0.00133 0.00068 H11D 0.97026 0.24818 0.35160 1.00000 0.04706 0.00000 0.00000 H11E 1.08545 0.36872 0.34479 1.00000 0.04706 0.00000 0.00000 H11F 0.96181 0.39729 0.39375 1.00000 0.04706 0.00000 0.00000 C111 1.27975 0.30541 0.48964 1.00000 0.03012 0.03654 0.02391 0.00781 0.01207 0.00716 0.02900 0.00671 0.00032 0.00029 0.00022 0.00000 0.00174 0.00158 0.00157 0.00119 0.00137 0.00125 0.00065 H11G 1.33389 0.28119 0.55491 1.00000 0.04349 0.00000 0.00000 H11H 1.32838 0.39015 0.48021 1.00000 0.04349 0.00000 0.00000 H11I 1.27660 0.23598 0.43528 1.00000 0.04349 0.00000 0.00000 N101 1.09520 0.31527 0.73532 1.00000 0.01961 0.03005 0.01399 0.00481 0.00261 0.00533 0.02162 0.00486 0.00024 0.00021 0.00017 0.00000 0.00126 0.00120 0.00113 0.00088 0.00098 0.00092 0.00049 H101 1.12771 0.31426 0.80093 1.00000 0.02594 0.00000 0.00000 O101 1.31297 0.31170 0.70609 1.00000 0.01804 0.03234 0.02036 0.00399 0.00306 0.00544 0.02415 0.00413 0.00021 0.00018 0.00014 0.00000 0.00107 0.00104 0.00102 0.00077 0.00085 0.00078 0.00043 C201 0.34696 0.32503 -0.02113 1.00000 0.02456 0.01788 0.01765 0.00283 0.00610 0.00267 0.02022 0.00577 0.00030 0.00024 0.00020 0.00000 0.00158 0.00121 0.00136 0.00095 0.00120 0.00100 0.00056 C202 0.44788 0.34166 0.08630 1.00000 0.01993 0.01761 0.01805 0.00251 0.00234 0.00332 0.01936 0.00558 0.00029 0.00024 0.00020 0.00000 0.00144 0.00118 0.00136 0.00095 0.00114 0.00098 0.00055 C203 0.59591 0.34795 0.07870 1.00000 0.02122 0.01862 0.01793 0.00208 0.00374 0.00150 0.02001 0.00562 0.00029 0.00024 0.00020 0.00000 0.00150 0.00121 0.00136 0.00096 0.00117 0.00100 0.00056 C204 0.58038 0.33296 -0.02493 1.00000 0.02209 0.01918 0.01987 0.00453 0.00617 0.00541 0.02020 0.00581 0.00029 0.00024 0.00020 0.00000 0.00152 0.00123 0.00141 0.00098 0.00120 0.00102 0.00056 C205 0.69745 0.33451 -0.06025 1.00000 0.02644 0.02896 0.01868 0.00657 0.00789 0.00463 0.02429 0.00616 0.00031 0.00026 0.00021 0.00000 0.00165 0.00141 0.00140 0.00106 0.00128 0.00114 0.00060 H205 0.68349 0.32301 -0.13069 1.00000 0.02915 0.00000 0.00000 C206 0.83666 0.35334 0.00987 1.00000 0.02114 0.02995 0.02821 0.00523 0.01052 0.00313 0.02583 0.00626 0.00031 0.00027 0.00022 0.00000 0.00158 0.00144 0.00159 0.00114 0.00133 0.00112 0.00062 H206 0.91937 0.35577 -0.01252 1.00000 0.03100 0.00000 0.00000 C207 0.85517 0.36861 0.11266 1.00000 0.02087 0.03128 0.02799 0.00369 0.00351 0.00214 0.02791 0.00642 0.00032 0.00028 0.00023 0.00000 0.00158 0.00148 0.00162 0.00118 0.00131 0.00115 0.00064 H207 0.95086 0.38125 0.15981 1.00000 0.03349 0.00000 0.00000 C208 0.73625 0.36576 0.14785 1.00000 0.02682 0.02738 0.01745 0.00248 0.00413 0.00465 0.02459 0.00602 0.00031 0.00026 0.00021 0.00000 0.00163 0.00140 0.00140 0.00104 0.00124 0.00113 0.00060 H208 0.75060 0.37586 0.21833 1.00000 0.02950 0.00000 0.00000 C209 0.40516 0.34845 0.16928 1.00000 0.02395 0.01773 0.01815 0.00208 0.00566 0.00106 0.02041 0.00572 0.00030 0.00024 0.00020 0.00000 0.00151 0.00120 0.00134 0.00095 0.00117 0.00101 0.00055 C210 0.51281 0.36551 0.27439 1.00000 0.02457 0.03990 0.01586 0.00261 0.00199 -0.00017 0.02834 0.00611 0.00032 0.00030 0.00021 0.00000 0.00161 0.00163 0.00141 0.00114 0.00123 0.00122 0.00064 H21A 0.56839 0.29107 0.28110 1.00000 0.04251 0.00000 0.00000 H21B 0.46033 0.36739 0.32375 1.00000 0.04251 0.00000 0.00000 H21C 0.57975 0.44917 0.28670 1.00000 0.04251 0.00000 0.00000 C211 0.24857 0.34080 0.16502 1.00000 0.02591 0.03952 0.02027 0.00109 0.00818 0.00243 0.02884 0.00645 0.00032 0.00030 0.00022 0.00000 0.00167 0.00162 0.00149 0.00117 0.00130 0.00124 0.00065 H21D 0.18570 0.32613 0.09435 1.00000 0.04326 0.00000 0.00000 H21E 0.23464 0.42432 0.19898 1.00000 0.04326 0.00000 0.00000 H21F 0.22321 0.26697 0.19896 1.00000 0.04326 0.00000 0.00000 N201 0.43276 0.31837 -0.08114 1.00000 0.02015 0.02761 0.01456 0.00434 0.00273 0.00553 0.02118 0.00485 0.00024 0.00021 0.00017 0.00000 0.00128 0.00116 0.00114 0.00087 0.00100 0.00091 0.00049 H201 0.39916 0.30629 -0.14757 1.00000 0.02542 0.00000 0.00000 O201 0.21274 0.31515 -0.05334 1.00000 0.01694 0.03138 0.02010 0.00375 0.00241 0.00446 0.02356 0.00405 0.00020 0.00018 0.00014 0.00000 0.00107 0.00102 0.00102 0.00077 0.00085 0.00077 0.00042 Final Structure Factor Calculation for 2007src1054 in P-1 Total number of l.s. parameters = 358 Maximum vector length = 511 Memory required = 4249 / 22995 wR2 = 0.1681 before cycle 21 for 5972 data and 0 / 358 parameters GooF = S = 1.078; Restrained GooF = 1.078 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0214 * P )^2 + 2.33 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0788 for 4122 Fo > 4sig(Fo) and 0.1204 for all 5972 data wR2 = 0.1681, GooF = S = 1.078, Restrained GooF = 1.078 for all data Occupancy sum of asymmetric unit = 39.00 for non-hydrogen and 33.00 for hydrogen atoms Principal mean square atomic displacements U 0.0240 0.0183 0.0151 C1 0.0244 0.0179 0.0132 C2 0.0228 0.0186 0.0140 C3 0.0237 0.0206 0.0150 C4 0.0335 0.0244 0.0172 C5 0.0340 0.0285 0.0207 C6 0.0355 0.0318 0.0126 C7 0.0329 0.0263 0.0130 C8 0.0254 0.0207 0.0181 C9 0.0351 0.0300 0.0140 C10 0.0446 0.0233 0.0200 C11 0.0289 0.0230 0.0110 N1 0.0278 0.0251 0.0159 O1 0.0246 0.0175 0.0151 C101 0.0235 0.0190 0.0153 C102 0.0218 0.0184 0.0175 C103 0.0264 0.0210 0.0162 C104 0.0339 0.0241 0.0190 C105 0.0358 0.0261 0.0220 C106 0.0344 0.0321 0.0209 C107 0.0322 0.0286 0.0196 C108 0.0257 0.0203 0.0179 C109 0.0389 0.0375 0.0178 C110 0.0373 0.0294 0.0203 C111 0.0301 0.0220 0.0128 N101 0.0325 0.0239 0.0161 O101 0.0252 0.0180 0.0174 C201 0.0247 0.0176 0.0158 C202 0.0242 0.0190 0.0169 C203 0.0231 0.0208 0.0167 C204 0.0295 0.0265 0.0169 C205 0.0305 0.0281 0.0189 C206 0.0328 0.0311 0.0198 C207 0.0296 0.0269 0.0172 C208 0.0256 0.0185 0.0172 C209 0.0425 0.0276 0.0150 C210 0.0412 0.0258 0.0196 C211 0.0279 0.0223 0.0134 N201 0.0314 0.0241 0.0152 O201 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.006 0.012 0.019 0.026 0.035 0.046 0.061 0.083 0.124 1.000 Number in group 644. 585. 615. 553. 603. 584. 613. 595. 582. 598. GooF 1.114 1.201 1.100 1.115 1.035 1.049 1.059 1.027 0.942 1.112 K 13.692 2.787 1.479 1.226 1.034 1.042 1.002 1.004 1.009 1.007 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.64 inf Number in group 620. 592. 586. 596. 607. 585. 593. 600. 592. 601. GooF 1.156 1.198 1.106 1.153 1.085 1.043 1.009 0.906 0.988 1.097 K 1.096 1.081 1.066 1.060 1.013 1.012 0.990 1.000 1.025 1.009 R1 0.266 0.246 0.205 0.196 0.151 0.105 0.085 0.063 0.070 0.043 Recommended weighting scheme: WGHT 0.0214 2.3373 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 0 1 165.61 452.30 8.59 0.141 6.61 0 8 0 57.63 0.98 4.84 0.007 1.26 5 4 10 104.85 15.58 4.19 0.026 0.83 2 11 2 1.00 39.09 3.75 0.042 0.84 0 11 5 0.36 34.82 3.61 0.039 0.83 -2 0 8 40.53 90.45 3.54 0.063 1.75 4 6 10 58.36 4.55 3.38 0.014 0.81 5 2 6 125.04 239.99 3.36 0.103 1.15 0 -6 6 48.90 16.98 3.30 0.027 1.44 -8 -2 8 1060.88 1288.37 3.26 0.238 1.09 -7 -1 17 63.82 15.03 3.25 0.026 0.79 7 6 6 -4.23 50.92 3.25 0.047 0.79 0 11 0 45.27 0.28 3.22 0.004 0.91 -10 -3 11 40.88 1.08 3.21 0.007 0.84 2 -1 12 252.20 368.03 3.16 0.127 1.01 -6 -4 16 29.30 0.17 3.13 0.003 0.82 2 -5 11 63.68 143.20 3.13 0.080 1.03 -2 5 14 16.14 54.12 3.12 0.049 0.85 5 -4 12 66.92 133.58 3.05 0.077 0.84 -11 -2 8 117.08 59.25 3.04 0.051 0.84 -1 0 16 33.80 2.04 2.97 0.009 0.85 0 -6 15 33.93 3.34 2.96 0.012 0.83 -12 -2 5 3.93 40.42 2.95 0.042 0.78 -11 -5 7 30.10 0.75 2.94 0.006 0.77 7 5 3 23.46 2.86 2.94 0.011 0.94 -5 -3 17 22.68 2.33 2.93 0.010 0.81 -5 -2 9 122.35 184.50 2.92 0.090 1.34 1 5 11 46.25 98.46 2.91 0.066 0.94 -10 0 9 24.90 2.20 2.91 0.010 0.92 4 -3 3 2375.87 2055.41 2.89 0.301 1.73 5 6 7 68.25 27.80 2.84 0.035 0.87 -4 1 14 5.10 31.13 2.82 0.037 0.98 -2 0 14 3.92 25.35 2.81 0.033 0.99 -9 5 3 56.65 22.24 2.79 0.031 1.00 3 -1 5 1676.75 1429.80 2.77 0.251 1.77 2 -2 7 119.58 186.22 2.77 0.091 1.59 1 7 10 205.16 126.41 2.76 0.075 0.88 -9 0 11 23.88 1.01 2.73 0.007 0.94 -7 -5 5 25.99 1.01 2.72 0.007 1.08 -5 12 1 39.37 91.25 2.72 0.063 0.81 -3 4 12 26.24 0.96 2.70 0.007 1.02 -7 6 10 5.71 28.90 2.70 0.036 0.94 -11 6 6 38.04 1.20 2.69 0.007 0.81 -6 6 15 28.71 3.11 2.69 0.012 0.78 -3 10 3 10.77 41.42 2.67 0.043 0.97 -1 0 7 1600.90 1377.91 2.67 0.247 1.98 3 -1 12 42.74 8.96 2.67 0.020 0.96 -1 -1 8 43.00 80.17 2.66 0.059 1.74 9 5 2 -0.92 29.63 2.66 0.036 0.82 3 -6 8 95.05 53.54 2.65 0.049 1.12 Bond lengths and angles C1 - Distance Angles O1 1.2321 (0.0032) N1 1.3628 (0.0033) 124.22 (0.24) C2 1.5122 (0.0037) 129.38 (0.24) 106.38 (0.22) C1 - O1 N1 C2 - Distance Angles C9 1.3508 (0.0036) C3 1.4718 (0.0036) 129.56 (0.25) C1 1.5122 (0.0037) 125.19 (0.25) 105.26 (0.21) C2 - C9 C3 C3 - Distance Angles C8 1.3904 (0.0038) C4 1.4043 (0.0035) 118.20 (0.24) C2 1.4718 (0.0036) 134.89 (0.24) 106.85 (0.23) C3 - C8 C4 C4 - Distance Angles C5 1.3809 (0.0038) N1 1.3912 (0.0034) 127.27 (0.25) C3 1.4043 (0.0035) 122.96 (0.25) 109.76 (0.23) C4 - C5 N1 C5 - Distance Angles C4 1.3809 (0.0038) C6 1.3930 (0.0041) 117.75 (0.26) H5 0.9500 121.13 121.13 C5 - C4 C6 C6 - Distance Angles C7 1.3836 (0.0039) C5 1.3930 (0.0041) 120.50 (0.26) H6 0.9500 119.75 119.75 C6 - C7 C5 C7 - Distance Angles C6 1.3836 (0.0039) C8 1.3949 (0.0039) 121.22 (0.27) H7 0.9500 119.39 119.39 C7 - C6 C8 C8 - Distance Angles C3 1.3904 (0.0038) C7 1.3949 (0.0039) 119.37 (0.25) H8 0.9500 120.32 120.32 C8 - C3 C7 C9 - Distance Angles C2 1.3508 (0.0036) C11 1.5018 (0.0038) 123.66 (0.25) C10 1.5020 (0.0037) 121.90 (0.25) 114.44 (0.23) C9 - C2 C11 C10 - Distance Angles C9 1.5020 (0.0037) H10A 0.9800 109.47 H10B 0.9800 109.47 109.47 H10C 0.9800 109.47 109.47 109.47 C10 - C9 H10A H10B C11 - Distance Angles C9 1.5018 (0.0038) H11A 0.9800 109.47 H11B 0.9800 109.47 109.47 H11C 0.9800 109.47 109.47 109.47 C11 - C9 H11A H11B N1 - Distance Angles C1 1.3628 (0.0033) C4 1.3912 (0.0034) 111.74 (0.22) H1 0.8800 124.13 124.13 N1 - C1 C4 O1 - Distance Angles C1 1.2321 (0.0032) O1 - C101 - Distance Angles O101 1.2338 (0.0032) N101 1.3568 (0.0033) 123.84 (0.24) C102 1.5080 (0.0036) 129.48 (0.24) 106.66 (0.22) C101 - O101 N101 C102 - Distance Angles C109 1.3549 (0.0036) C103 1.4732 (0.0037) 130.41 (0.25) C101 1.5080 (0.0036) 124.52 (0.25) 105.05 (0.21) C102 - C109 C103 C103 - Distance Angles C108 1.3907 (0.0039) C104 1.4066 (0.0035) 118.00 (0.24) C102 1.4732 (0.0037) 134.96 (0.24) 107.02 (0.23) C103 - C108 C104 C104 - Distance Angles C105 1.3784 (0.0038) N101 1.3927 (0.0035) 127.74 (0.25) C103 1.4066 (0.0035) 122.98 (0.26) 109.27 (0.23) C104 - C105 N101 C105 - Distance Angles C104 1.3784 (0.0038) C106 1.3881 (0.0041) 118.15 (0.26) H105 0.9500 120.92 120.92 C105 - C104 C106 C106 - Distance Angles C107 1.3864 (0.0040) C105 1.3881 (0.0041) 120.38 (0.27) H106 0.9500 119.81 119.81 C106 - C107 C105 C107 - Distance Angles C106 1.3864 (0.0040) C108 1.4009 (0.0040) 121.04 (0.28) H107 0.9500 119.48 119.48 C107 - C106 C108 C108 - Distance Angles C103 1.3907 (0.0039) C107 1.4009 (0.0040) 119.44 (0.26) H108 0.9500 120.28 120.28 C108 - C103 C107 C109 - Distance Angles C102 1.3549 (0.0036) C111 1.4973 (0.0038) 123.66 (0.25) C110 1.5002 (0.0039) 122.24 (0.26) 114.10 (0.23) C109 - C102 C111 C110 - Distance Angles C109 1.5002 (0.0039) H11D 0.9800 109.47 H11E 0.9800 109.47 109.47 H11F 0.9800 109.47 109.47 109.47 C110 - C109 H11D H11E C111 - Distance Angles C109 1.4973 (0.0038) H11G 0.9800 109.47 H11H 0.9800 109.47 109.47 H11I 0.9800 109.47 109.47 109.47 C111 - C109 H11G H11H N101 - Distance Angles C101 1.3568 (0.0033) C104 1.3927 (0.0035) 111.99 (0.22) H101 0.8800 124.01 124.01 N101 - C101 C104 O101 - Distance Angles C101 1.2338 (0.0032) O101 - C201 - Distance Angles O201 1.2350 (0.0032) N201 1.3600 (0.0033) 124.05 (0.24) C202 1.5086 (0.0037) 129.56 (0.24) 106.37 (0.23) C201 - O201 N201 C202 - Distance Angles C209 1.3515 (0.0036) C203 1.4742 (0.0037) 129.45 (0.25) C201 1.5086 (0.0037) 125.13 (0.25) 105.42 (0.21) C202 - C209 C203 C203 - Distance Angles C208 1.3936 (0.0038) C204 1.4079 (0.0035) 118.15 (0.24) C202 1.4742 (0.0037) 135.02 (0.24) 106.82 (0.23) C203 - C208 C204 C204 - Distance Angles C205 1.3763 (0.0037) N201 1.3957 (0.0034) 127.90 (0.25) C203 1.4079 (0.0035) 122.78 (0.26) 109.32 (0.23) C204 - C205 N201 C205 - Distance Angles C204 1.3763 (0.0037) C206 1.3902 (0.0040) 118.24 (0.26) H205 0.9500 120.88 120.88 C205 - C204 C206 C206 - Distance Angles C207 1.3899 (0.0040) C205 1.3902 (0.0040) 120.18 (0.26) H206 0.9500 119.91 119.91 C206 - C207 C205 C207 - Distance Angles C206 1.3899 (0.0040) C208 1.3915 (0.0039) 121.28 (0.27) H207 0.9500 119.36 119.36 C207 - C206 C208 C208 - Distance Angles C207 1.3915 (0.0039) C203 1.3936 (0.0038) 119.36 (0.26) H208 0.9500 120.32 120.32 C208 - C207 C203 C209 - Distance Angles C202 1.3515 (0.0036) C211 1.5021 (0.0039) 123.37 (0.25) C210 1.5066 (0.0038) 122.04 (0.25) 114.59 (0.23) C209 - C202 C211 C210 - Distance Angles C209 1.5066 (0.0038) H21A 0.9800 109.47 H21B 0.9800 109.47 109.47 H21C 0.9800 109.47 109.47 109.47 C210 - C209 H21A H21B C211 - Distance Angles C209 1.5021 (0.0039) H21D 0.9800 109.47 H21E 0.9800 109.47 109.47 H21F 0.9800 109.47 109.47 109.47 C211 - C209 H21D H21E N201 - Distance Angles C201 1.3600 (0.0033) C204 1.3957 (0.0034) 112.04 (0.22) H201 0.8800 123.98 123.98 N201 - C201 C204 O201 - Distance Angles C201 1.2350 (0.0032) O201 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 1.98 2.859(3) 174.2 N1-H1...O1_$1 0.88 1.96 2.837(3) 176.3 N101-H101...O201_$2 0.88 1.98 2.848(3) 169.5 N201-H201...O101_$3 FMAP and GRID set by program FMAP 2 3 35 GRID -1.563 -2 -2 1.563 2 2 R1 = 0.1203 for 5972 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.36 at 0.0590 0.2808 0.3385 [ 0.89 A from H11E ] Deepest hole -0.31 at 0.1012 0.3590 0.3466 [ 0.19 A from H11E ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 3955 / 27123 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 1.0590 0.2808 0.3385 1.00000 0.05 0.36 0.89 H11E 0.96 C110 0.97 H11D 1.86 H11F Q2 1 0.7391 -0.0061 0.2443 1.00000 0.05 0.31 0.74 C2 0.75 C3 1.79 C4 1.87 C1 Q3 1 0.9171 0.2938 0.3659 1.00000 0.05 0.29 0.79 H11D 1.05 C110 1.08 H11F 1.85 H11E Q4 1 0.8182 -0.0456 0.2046 1.00000 0.05 0.27 0.70 C2 0.96 C9 1.89 C3 1.93 C1 Q5 1 0.5965 0.3747 0.0274 1.00000 0.05 0.26 0.77 C204 0.80 C203 1.82 N201 1.84 C208 Q6 1 0.6294 0.5552 0.2966 1.00000 0.05 0.26 1.11 H21C 1.42 O101 2.07 C101 2.08 C210 Q7 1 1.4172 0.3192 0.5846 1.00000 0.05 0.25 0.82 H11G 1.56 C111 1.74 H11H 1.94 H106 Q8 1 0.6663 0.0047 0.3011 1.00000 0.05 0.25 0.70 C3 0.72 C4 1.76 C8 1.81 C5 Q9 1 1.0075 0.3177 0.5704 1.00000 0.05 0.25 0.73 C102 0.74 C103 1.81 C104 1.87 C101 Q10 1 0.9391 0.3102 0.6277 1.00000 0.05 0.25 0.70 C103 0.72 C104 1.78 N101 1.81 C108 Shortest distances between peaks (including symmetry equivalents) 2 4 1.17 9 10 1.19 2 8 1.22 1 3 1.56 6 7 2.19 4 8 2.36 3 9 2.71 Time profile in seconds ----------------------- 0.14: 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. 3.38: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.06: Set up l.s. refinement 0.00: Generate idealized H-atoms 9.28: Structure factors and derivatives 25.64: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.14: Apply other restraints 3.72: Solve l.s. equations 0.00: Generate HTAB table 0.08: Other dependent quantities, CIF, tables 0.23: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.08: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src1054 finished at 15:34:13 Total CPU time: 42.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++