+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 12:58:39 on 31-Mar-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh022 in P-1 CELL 0.71073 9.2339 11.9540 13.4630 64.502 87.652 76.670 ZERR 4.00 0.0003 0.0004 0.0004 0.002 0.002 0.002 LATT 1 SFAC C H N O UNIT 60 64 8 12 V = 1302.32 F(000) = 576.0 Mu = 0.10 mm-1 Cell Wt = 1089.19 Rho = 1.389 MERG 2 OMIT -3.00 55.00 DFIX 0.88 0.02 N1 H1N N2 H2N N3 H3N N4 H4N FMAP 2 PLAN 5 HTAB ACTA BOND $H SIZE 0.3 0.02 0.01 L.S. 8 TEMP -153.00 WGHT 0.018500 1.927500 FVAR 0.66027 MOLE 1 C1 1 0.257384 0.333658 0.162590 11.00000 0.01946 0.02774 = 0.02591 -0.01542 0.00689 -0.00716 C2 1 0.169241 0.392551 0.065635 11.00000 0.02449 0.02197 = 0.03023 -0.01114 0.00356 -0.00556 AFIX 43 H2 2 0.138304 0.482991 0.030612 11.00000 -1.20000 AFIX 0 C3 1 0.124319 0.322001 0.017651 11.00000 0.02174 0.02694 = 0.02613 -0.01115 -0.00168 -0.00325 AFIX 43 H3 2 0.062682 0.363878 -0.048950 11.00000 -1.20000 AFIX 0 C4 1 0.170913 0.190027 0.068549 11.00000 0.02638 0.02734 = 0.02967 -0.01752 0.00592 -0.00752 C5 1 0.264435 0.130806 0.164045 11.00000 0.03380 0.02127 = 0.03252 -0.01085 -0.00071 -0.00246 AFIX 43 H5 2 0.299679 0.040657 0.197322 11.00000 -1.20000 AFIX 0 C6 1 0.306935 0.201766 0.211352 11.00000 0.02756 0.03002 = 0.02808 -0.01386 0.00098 -0.00401 AFIX 43 H6 2 0.370050 0.160140 0.277228 11.00000 -1.20000 AFIX 0 C7 1 0.199006 0.486332 0.242903 11.00000 0.01766 0.02387 = 0.02260 -0.01104 0.00168 -0.00494 C8 1 0.179185 0.640922 0.322870 11.00000 0.01810 0.02356 = 0.02306 -0.01105 -0.00048 -0.00492 C9 1 0.054949 0.619600 0.382987 11.00000 0.02080 0.02405 = 0.02656 -0.01211 0.00228 -0.00788 AFIX 43 H9 2 0.015355 0.549534 0.391636 11.00000 -1.20000 AFIX 0 C10 1 -0.012860 0.699395 0.430988 11.00000 0.02003 0.02709 = 0.02643 -0.01258 0.00280 -0.00628 AFIX 43 H10 2 -0.098924 0.684288 0.471070 11.00000 -1.20000 AFIX 0 C11 1 0.045181 0.800692 0.420272 11.00000 0.02799 0.02497 = 0.02558 -0.01469 -0.00020 -0.00388 C12 1 0.170621 0.821691 0.360767 11.00000 0.03459 0.03341 = 0.03442 -0.02036 0.00705 -0.01813 AFIX 43 H12 2 0.211515 0.890664 0.353422 11.00000 -1.20000 AFIX 0 C13 1 0.236098 0.743682 0.312446 11.00000 0.02666 0.03306 = 0.03078 -0.01626 0.00726 -0.01471 AFIX 43 H13 2 0.321188 0.759906 0.271420 11.00000 -1.20000 AFIX 0 C14 1 0.026340 0.168705 -0.063097 11.00000 0.03454 0.03904 = 0.03394 -0.02115 0.00246 -0.01263 AFIX 137 H14A 2 -0.066330 0.212806 -0.044541 11.00000 -1.50000 H14B 2 0.006215 0.102464 -0.081307 11.00000 -1.50000 H14C 2 0.065743 0.230129 -0.126650 11.00000 -1.50000 AFIX 0 C15 1 -0.126315 0.855941 0.538550 11.00000 0.02842 0.03906 = 0.04147 -0.02769 0.00664 -0.00572 AFIX 137 H15A 2 -0.215580 0.861748 0.497980 11.00000 -1.50000 H15B 2 -0.149484 0.917200 0.570598 11.00000 -1.50000 H15C 2 -0.093614 0.769429 0.597588 11.00000 -1.50000 AFIX 0 N1 3 0.300961 0.408289 0.210423 11.00000 0.01414 0.02818 = 0.03402 -0.01865 0.00407 -0.00621 N2 3 0.257187 0.560226 0.276067 11.00000 0.01397 0.02769 = 0.02906 -0.01630 0.00234 -0.00543 O1 4 0.064659 0.487901 0.241986 11.00000 0.01454 0.03536 = 0.03744 -0.02362 0.00424 -0.00769 O2 4 0.133663 0.111261 0.029336 11.00000 0.04548 0.02926 = 0.03737 -0.01896 -0.00424 -0.00798 O3 4 -0.010839 0.884102 0.465388 11.00000 0.03643 0.03141 = 0.04064 -0.02440 0.01031 -0.01115 H1N 2 0.392536 0.409514 0.212266 11.00000 0.02471 H2N 2 0.351898 0.556251 0.269353 11.00000 0.03045 MOLE 2 C21 1 0.763421 0.321209 0.185735 11.00000 0.01930 0.02763 = 0.02852 -0.01520 0.00638 -0.01027 C22 1 0.657282 0.367427 0.099727 11.00000 0.02452 0.02324 = 0.03375 -0.01335 0.00152 -0.00394 AFIX 43 H22 2 0.606442 0.454932 0.068737 11.00000 -1.20000 AFIX 0 C23 1 0.623324 0.288191 0.057528 11.00000 0.02272 0.03062 = 0.02831 -0.01355 0.00089 -0.00623 AFIX 43 H23 2 0.548476 0.320830 -0.000776 11.00000 -1.20000 AFIX 0 C24 1 0.699882 0.160840 0.101430 11.00000 0.03085 0.02694 = 0.02686 -0.01517 0.00822 -0.01050 C25 1 0.807230 0.112926 0.188326 11.00000 0.03070 0.02348 = 0.03216 -0.01282 0.00172 -0.00381 AFIX 43 H25 2 0.859143 0.025711 0.218708 11.00000 -1.20000 AFIX 0 C26 1 0.838173 0.192788 0.230402 11.00000 0.02517 0.02889 = 0.02908 -0.01405 0.00096 -0.00278 AFIX 43 H26 2 0.910882 0.159832 0.290153 11.00000 -1.20000 AFIX 0 C27 1 0.698937 0.488193 0.250055 11.00000 0.01756 0.02629 = 0.02627 -0.01269 0.00213 -0.00656 C28 1 0.676545 0.652032 0.317452 11.00000 0.01481 0.02615 = 0.02861 -0.01587 0.00380 -0.00663 C29 1 0.626067 0.599605 0.422217 11.00000 0.02007 0.02230 = 0.02988 -0.01064 -0.00310 -0.00571 AFIX 43 H29 2 0.640587 0.509679 0.461170 11.00000 -1.20000 AFIX 0 C30 1 0.554298 0.677216 0.471064 11.00000 0.02567 0.02754 = 0.02496 -0.01246 0.00210 -0.00886 AFIX 43 H30 2 0.518629 0.640585 0.542468 11.00000 -1.20000 AFIX 0 C31 1 0.535177 0.808657 0.414668 11.00000 0.01874 0.02738 = 0.03066 -0.01688 -0.00038 -0.00581 C32 1 0.586816 0.861505 0.309836 11.00000 0.02368 0.02046 = 0.03032 -0.00979 0.00128 -0.00719 AFIX 43 H32 2 0.574728 0.951253 0.271568 11.00000 -1.20000 AFIX 0 C33 1 0.655765 0.783871 0.261009 11.00000 0.02129 0.02694 = 0.02604 -0.00995 0.00203 -0.00727 AFIX 43 H33 2 0.688996 0.820650 0.188791 11.00000 -1.20000 AFIX 0 C34 1 0.585254 0.128209 -0.035315 11.00000 0.04929 0.03953 = 0.03467 -0.02194 0.00344 -0.01587 AFIX 137 H34A 2 0.482645 0.160993 -0.021806 11.00000 -1.50000 H34B 2 0.587439 0.061571 -0.059725 11.00000 -1.50000 H34C 2 0.622127 0.197863 -0.092603 11.00000 -1.50000 AFIX 0 C35 1 0.406614 0.842902 0.560524 11.00000 0.04028 0.03659 = 0.02843 -0.01867 0.00407 -0.00492 AFIX 137 H35A 2 0.324689 0.805419 0.555991 11.00000 -1.50000 H35B 2 0.369264 0.911090 0.583653 11.00000 -1.50000 H35C 2 0.485114 0.776939 0.614401 11.00000 -1.50000 AFIX 0 N3 3 0.801299 0.403159 0.226034 11.00000 0.01325 0.02937 = 0.04041 -0.02174 0.00376 -0.00529 N4 3 0.756061 0.572199 0.269685 11.00000 0.01567 0.02834 = 0.03583 -0.01864 0.00498 -0.00750 O4 4 0.564346 0.488525 0.253893 11.00000 0.01700 0.04267 = 0.04829 -0.03115 0.00622 -0.01003 O5 4 0.677400 0.076299 0.063560 11.00000 0.04484 0.02818 = 0.03110 -0.01684 0.00198 -0.00920 O6 4 0.466158 0.894389 0.454697 11.00000 0.03104 0.02701 = 0.03471 -0.01862 0.00546 -0.00656 H3N 2 0.894822 0.402639 0.229086 11.00000 0.03031 H4N 2 0.850568 0.568178 0.261914 11.00000 0.03047 HKLF 4 Covalent radii and connectivity table for 2008lsh022 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 C1 - C2 C6 N1 C2 - C1 C3 C3 - C4 C2 C4 - O2 C3 C5 C5 - C6 C4 C6 - C5 C1 C7 - O1 N2 N1 C8 - C9 C13 N2 C9 - C8 C10 C10 - C11 C9 C11 - O3 C10 C12 C12 - C13 C11 C13 - C12 C8 C14 - O2 C15 - O3 N1 - C7 C1 N2 - C7 C8 O1 - C7 O2 - C4 C14 O3 - C11 C15 C21 - C22 C26 N3 C22 - C21 C23 C23 - C24 C22 C24 - O5 C23 C25 C25 - C26 C24 C26 - C25 C21 C27 - O4 N4 N3 C28 - C29 C33 N4 C29 - C28 C30 C30 - C31 C29 C31 - O6 C30 C32 C32 - C33 C31 C33 - C32 C28 C34 - O5 C35 - O6 N3 - C27 C21 N4 - C27 C28 O4 - C27 O5 - C24 C34 O6 - C31 C35 22896 Reflections read, of which 45 rejected -11 =< h =< 11, -15 =< k =< 15, -17 =< l =< 17, Max. 2-theta = 54.99 0 Systematic absence violations 0 Inconsistent equivalents 5928 Unique reflections, of which 0 suppressed R(int) = 0.0517 R(sigma) = 0.0556 Friedel opposites merged Maximum memory for data reduction = 3442 / 59283 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 = 4495 / 485910 wR2 = 0.1485 before cycle 1 for 5928 data and 381 / 381 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.103; Restrained GooF = 1.103 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0185 * P )^2 + 1.93 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.66027 0.00122 0.000 OSF Mean shift/esd = 0.001 Maximum = -0.005 for U12 O1 Max. shift = 0.000 A for H15C Max. dU = 0.000 for O4 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4495 / 485910 wR2 = 0.1485 before cycle 2 for 5928 data and 381 / 381 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.103; Restrained GooF = 1.103 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0185 * P )^2 + 1.93 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.66027 0.00122 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.002 for U12 O1 Max. shift = 0.000 A for H2N Max. dU = 0.000 for O4 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4495 / 485910 wR2 = 0.1485 before cycle 3 for 5928 data and 381 / 381 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.103; Restrained GooF = 1.103 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0185 * P )^2 + 1.93 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.66027 0.00122 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H4N Max. dU = 0.000 for H2N Least-squares cycle 4 Maximum vector length = 511 Memory required = 4495 / 485910 wR2 = 0.1485 before cycle 4 for 5928 data and 381 / 381 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.103; Restrained GooF = 1.103 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0185 * P )^2 + 1.93 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.66027 0.00122 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H4N Max. dU = 0.000 for N2 Least-squares cycle 5 Maximum vector length = 511 Memory required = 4495 / 485910 wR2 = 0.1485 before cycle 5 for 5928 data and 381 / 381 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.103; Restrained GooF = 1.103 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0185 * P )^2 + 1.93 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.66027 0.00122 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y O6 Max. shift = 0.000 A for H4N Max. dU = 0.000 for H2N Least-squares cycle 6 Maximum vector length = 511 Memory required = 4495 / 485910 wR2 = 0.1485 before cycle 6 for 5928 data and 381 / 381 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.103; Restrained GooF = 1.103 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0185 * P )^2 + 1.93 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.66027 0.00122 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H4N Max. dU = 0.000 for H1N Least-squares cycle 7 Maximum vector length = 511 Memory required = 4495 / 485910 wR2 = 0.1485 before cycle 7 for 5928 data and 381 / 381 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.103; Restrained GooF = 1.103 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0185 * P )^2 + 1.93 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.66027 0.00122 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O4 Max. shift = 0.000 A for C31 Max. dU = 0.000 for H1N Least-squares cycle 8 Maximum vector length = 511 Memory required = 4495 / 485910 wR2 = 0.1485 before cycle 8 for 5928 data and 381 / 381 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.103; Restrained GooF = 1.103 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0185 * P )^2 + 1.93 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.66027 0.00122 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H1N Max. dU = 0.000 for H3N Largest correlation matrix elements -0.618 U23 O4 / U22 O4 -0.589 U23 N3 / U22 N3 -0.570 U23 N1 / U22 N1 -0.618 U23 C15 / U33 C15 -0.585 U23 N3 / U33 N3 -0.570 U23 C12 / U22 C12 -0.617 U23 C15 / U22 C15 -0.576 U23 C14 / U33 C14 -0.569 U23 N4 / U33 N4 -0.616 U23 O4 / U33 O4 -0.574 U23 C34 / U33 C34 -0.568 U23 C14 / U22 C14 -0.601 U23 O3 / U22 O3 -0.573 U23 C12 / U33 C12 -0.567 U23 C4 / U33 C4 -0.596 U23 O3 / U33 O3 -0.572 U23 C34 / U22 C34 -0.567 U23 C31 / U22 C31 -0.593 U23 O1 / U33 O1 -0.571 U23 N1 / U33 N1 -0.566 U23 O6 / U33 O6 -0.590 U23 O1 / U22 O1 -0.571 U23 C4 / U22 C4 -0.565 U23 O6 / U22 O6 Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.1383 0.4830 0.0306 43 0.950 0.000 C2 C1 C3 H3 0.0627 0.3639 -0.0490 43 0.950 0.000 C3 C4 C2 H5 0.2997 0.0407 0.1973 43 0.950 0.000 C5 C6 C4 H6 0.3701 0.1601 0.2772 43 0.950 0.000 C6 C5 C1 H9 0.0154 0.5495 0.3916 43 0.950 0.000 C9 C8 C10 H10 -0.0989 0.6843 0.4711 43 0.950 0.000 C10 C11 C9 H12 0.2115 0.8907 0.3534 43 0.950 0.000 C12 C13 C11 H13 0.3212 0.7599 0.2714 43 0.950 0.000 C13 C12 C8 H14A -0.0663 0.2128 -0.0445 137 0.980 0.000 C14 O2 H14A H14B 0.0062 0.1025 -0.0813 137 0.980 0.000 C14 O2 H14A H14C 0.0657 0.2301 -0.1267 137 0.980 0.000 C14 O2 H14A H15A -0.2156 0.8617 0.4980 137 0.980 0.000 C15 O3 H15A H15B -0.1495 0.9172 0.5706 137 0.980 0.000 C15 O3 H15A H15C -0.0936 0.7694 0.5976 137 0.980 0.000 C15 O3 H15A H22 0.6064 0.4549 0.0687 43 0.950 0.000 C22 C21 C23 H23 0.5485 0.3208 -0.0008 43 0.950 0.000 C23 C24 C22 H25 0.8591 0.0257 0.2187 43 0.950 0.000 C25 C26 C24 H26 0.9109 0.1598 0.2902 43 0.950 0.000 C26 C25 C21 H29 0.6406 0.5097 0.4612 43 0.950 0.000 C29 C28 C30 H30 0.5186 0.6406 0.5425 43 0.950 0.000 C30 C31 C29 H32 0.5747 0.9513 0.2716 43 0.950 0.000 C32 C33 C31 H33 0.6890 0.8206 0.1888 43 0.950 0.000 C33 C32 C28 H34A 0.4826 0.1610 -0.0218 137 0.980 0.000 C34 O5 H34A H34B 0.5874 0.0616 -0.0597 137 0.980 0.000 C34 O5 H34A H34C 0.6221 0.1979 -0.0926 137 0.980 0.000 C34 O5 H34A H35A 0.3247 0.8054 0.5560 137 0.980 0.000 C35 O6 H35A H35B 0.3693 0.9111 0.5837 137 0.980 0.000 C35 O6 H35A H35C 0.4851 0.7769 0.6144 137 0.980 0.000 C35 O6 H35A 2008lsh022 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.25738 0.33366 0.16259 1.00000 0.01946 0.02774 0.02591 -0.01542 0.00689 -0.00716 0.02287 0.00352 0.00027 0.00025 0.00021 0.00000 0.00116 0.00134 0.00127 0.00110 0.00099 0.00103 0.00052 C2 0.16924 0.39255 0.06563 1.00000 0.02449 0.02197 0.03023 -0.01114 0.00356 -0.00556 0.02566 0.00366 0.00028 0.00025 0.00022 0.00000 0.00126 0.00129 0.00138 0.00111 0.00107 0.00104 0.00055 H2 0.13830 0.48299 0.03061 1.00000 0.03080 0.00000 0.00000 C3 0.12432 0.32200 0.01765 1.00000 0.02174 0.02694 0.02613 -0.01115 -0.00168 -0.00325 0.02541 0.00363 0.00028 0.00025 0.00021 0.00000 0.00122 0.00135 0.00130 0.00111 0.00103 0.00105 0.00055 H3 0.06268 0.36388 -0.04895 1.00000 0.03049 0.00000 0.00000 C4 0.17091 0.19003 0.06855 1.00000 0.02638 0.02734 0.02967 -0.01752 0.00592 -0.00752 0.02583 0.00364 0.00029 0.00025 0.00022 0.00000 0.00129 0.00137 0.00136 0.00116 0.00109 0.00110 0.00055 C5 0.26444 0.13081 0.16404 1.00000 0.03380 0.02127 0.03252 -0.01085 -0.00071 -0.00246 0.03013 0.00390 0.00031 0.00026 0.00023 0.00000 0.00144 0.00133 0.00147 0.00117 0.00118 0.00113 0.00060 H5 0.29968 0.04066 0.19732 1.00000 0.03615 0.00000 0.00000 C6 0.30693 0.20177 0.21135 1.00000 0.02756 0.03002 0.02808 -0.01386 0.00098 -0.00401 0.02856 0.00386 0.00030 0.00026 0.00022 0.00000 0.00134 0.00144 0.00137 0.00118 0.00110 0.00113 0.00058 H6 0.37005 0.16014 0.27723 1.00000 0.03428 0.00000 0.00000 C7 0.19901 0.48633 0.24290 1.00000 0.01766 0.02387 0.02260 -0.01104 0.00168 -0.00494 0.02103 0.00336 0.00026 0.00024 0.00020 0.00000 0.00114 0.00126 0.00122 0.00104 0.00096 0.00099 0.00051 C8 0.17919 0.64092 0.32287 1.00000 0.01810 0.02356 0.02306 -0.01105 -0.00048 -0.00492 0.02117 0.00335 0.00026 0.00024 0.00020 0.00000 0.00114 0.00127 0.00123 0.00105 0.00096 0.00099 0.00051 C9 0.05495 0.61960 0.38299 1.00000 0.02080 0.02405 0.02656 -0.01211 0.00228 -0.00788 0.02294 0.00348 0.00027 0.00024 0.00020 0.00000 0.00118 0.00131 0.00129 0.00109 0.00100 0.00102 0.00053 H9 0.01536 0.54953 0.39164 1.00000 0.02753 0.00000 0.00000 C10 -0.01286 0.69939 0.43099 1.00000 0.02003 0.02709 0.02643 -0.01258 0.00280 -0.00628 0.02407 0.00350 0.00027 0.00024 0.00021 0.00000 0.00119 0.00135 0.00130 0.00111 0.00101 0.00104 0.00054 H10 -0.09892 0.68429 0.47107 1.00000 0.02888 0.00000 0.00000 C11 0.04518 0.80069 0.42027 1.00000 0.02799 0.02497 0.02558 -0.01469 -0.00020 -0.00388 0.02519 0.00357 0.00029 0.00025 0.00021 0.00000 0.00131 0.00133 0.00129 0.00111 0.00106 0.00108 0.00055 C12 0.17062 0.82169 0.36077 1.00000 0.03459 0.03341 0.03442 -0.02036 0.00705 -0.01813 0.03041 0.00372 0.00031 0.00027 0.00022 0.00000 0.00147 0.00152 0.00150 0.00128 0.00121 0.00125 0.00061 H12 0.21151 0.89066 0.35342 1.00000 0.03649 0.00000 0.00000 C13 0.23610 0.74368 0.31245 1.00000 0.02666 0.03306 0.03078 -0.01626 0.00726 -0.01471 0.02807 0.00365 0.00029 0.00026 0.00022 0.00000 0.00132 0.00148 0.00140 0.00121 0.00111 0.00116 0.00058 H13 0.32119 0.75991 0.27142 1.00000 0.03368 0.00000 0.00000 C14 0.02634 0.16871 -0.06310 1.00000 0.03454 0.03904 0.03394 -0.02115 0.00246 -0.01263 0.03319 0.00382 0.00032 0.00028 0.00023 0.00000 0.00148 0.00164 0.00151 0.00134 0.00122 0.00129 0.00064 H14A -0.06633 0.21281 -0.04454 1.00000 0.04979 0.00000 0.00000 H14B 0.00621 0.10246 -0.08131 1.00000 0.04979 0.00000 0.00000 H14C 0.06574 0.23013 -0.12665 1.00000 0.04979 0.00000 0.00000 C15 -0.12631 0.85594 0.53855 1.00000 0.02842 0.03906 0.04147 -0.02769 0.00664 -0.00572 0.03313 0.00401 0.00030 0.00028 0.00024 0.00000 0.00140 0.00165 0.00163 0.00141 0.00122 0.00123 0.00064 H15A -0.21558 0.86175 0.49798 1.00000 0.04970 0.00000 0.00000 H15B -0.14948 0.91720 0.57060 1.00000 0.04970 0.00000 0.00000 H15C -0.09361 0.76943 0.59759 1.00000 0.04970 0.00000 0.00000 N1 0.30096 0.40829 0.21042 1.00000 0.01414 0.02818 0.03402 -0.01865 0.00407 -0.00621 0.02342 0.00298 0.00022 0.00021 0.00018 0.00000 0.00098 0.00117 0.00121 0.00100 0.00088 0.00088 0.00046 N2 0.25719 0.56023 0.27607 1.00000 0.01397 0.02769 0.02906 -0.01630 0.00234 -0.00543 0.02205 0.00289 0.00022 0.00020 0.00017 0.00000 0.00096 0.00115 0.00114 0.00096 0.00085 0.00087 0.00045 O1 0.06466 0.48790 0.24199 1.00000 0.01454 0.03536 0.03744 -0.02362 0.00424 -0.00769 0.02601 0.00237 0.00018 0.00017 0.00015 0.00000 0.00081 0.00104 0.00104 0.00088 0.00073 0.00074 0.00041 O2 0.13366 0.11126 0.02934 1.00000 0.04548 0.02926 0.03737 -0.01896 -0.00424 -0.00798 0.03566 0.00266 0.00023 0.00018 0.00016 0.00000 0.00120 0.00105 0.00111 0.00091 0.00093 0.00091 0.00048 O3 -0.01084 0.88410 0.46539 1.00000 0.03643 0.03141 0.04064 -0.02440 0.01031 -0.01115 0.03264 0.00268 0.00021 0.00018 0.00016 0.00000 0.00106 0.00107 0.00113 0.00093 0.00088 0.00087 0.00045 H1N 0.39254 0.40951 0.21227 1.00000 0.02471 0.03249 0.00202 0.00260 0.00222 0.00000 0.00725 H2N 0.35190 0.55625 0.26935 1.00000 0.03045 0.03671 0.00202 0.00274 0.00232 0.00000 0.00775 C21 0.76342 0.32121 0.18574 1.00000 0.01930 0.02763 0.02852 -0.01520 0.00638 -0.01027 0.02334 0.00348 0.00027 0.00025 0.00021 0.00000 0.00117 0.00135 0.00133 0.00113 0.00101 0.00104 0.00053 C22 0.65728 0.36743 0.09973 1.00000 0.02452 0.02324 0.03375 -0.01335 0.00152 -0.00394 0.02710 0.00368 0.00028 0.00025 0.00022 0.00000 0.00128 0.00134 0.00145 0.00117 0.00112 0.00107 0.00057 H22 0.60644 0.45493 0.06874 1.00000 0.03251 0.00000 0.00000 C23 0.62332 0.28819 0.05753 1.00000 0.02272 0.03062 0.02831 -0.01355 0.00089 -0.00623 0.02692 0.00372 0.00028 0.00025 0.00022 0.00000 0.00126 0.00146 0.00136 0.00117 0.00106 0.00110 0.00057 H23 0.54848 0.32083 -0.00078 1.00000 0.03230 0.00000 0.00000 C24 0.69988 0.16084 0.10143 1.00000 0.03085 0.02694 0.02686 -0.01517 0.00822 -0.01050 0.02647 0.00372 0.00030 0.00025 0.00021 0.00000 0.00137 0.00137 0.00134 0.00114 0.00111 0.00113 0.00056 C25 0.80723 0.11293 0.18833 1.00000 0.03070 0.02348 0.03216 -0.01282 0.00172 -0.00381 0.02895 0.00383 0.00030 0.00026 0.00022 0.00000 0.00139 0.00134 0.00143 0.00116 0.00115 0.00112 0.00058 H25 0.85914 0.02571 0.21871 1.00000 0.03474 0.00000 0.00000 C26 0.83817 0.19279 0.23040 1.00000 0.02517 0.02889 0.02908 -0.01405 0.00096 -0.00278 0.02779 0.00384 0.00029 0.00026 0.00022 0.00000 0.00129 0.00142 0.00138 0.00117 0.00109 0.00110 0.00057 H26 0.91088 0.15983 0.29015 1.00000 0.03335 0.00000 0.00000 C27 0.69894 0.48819 0.25005 1.00000 0.01756 0.02629 0.02627 -0.01269 0.00213 -0.00656 0.02267 0.00343 0.00026 0.00024 0.00020 0.00000 0.00116 0.00132 0.00128 0.00109 0.00099 0.00102 0.00053 C28 0.67654 0.65203 0.31745 1.00000 0.01481 0.02615 0.02861 -0.01587 0.00380 -0.00663 0.02148 0.00335 0.00025 0.00024 0.00021 0.00000 0.00109 0.00131 0.00131 0.00111 0.00097 0.00098 0.00052 C29 0.62607 0.59960 0.42222 1.00000 0.02007 0.02230 0.02988 -0.01064 -0.00310 -0.00571 0.02405 0.00340 0.00027 0.00024 0.00021 0.00000 0.00118 0.00128 0.00135 0.00110 0.00104 0.00101 0.00054 H29 0.64059 0.50968 0.46117 1.00000 0.02886 0.00000 0.00000 C30 0.55430 0.67722 0.47106 1.00000 0.02567 0.02754 0.02496 -0.01246 0.00210 -0.00886 0.02521 0.00350 0.00028 0.00025 0.00021 0.00000 0.00129 0.00136 0.00129 0.00112 0.00105 0.00109 0.00055 H30 0.51863 0.64058 0.54247 1.00000 0.03025 0.00000 0.00000 C31 0.53518 0.80866 0.41467 1.00000 0.01874 0.02738 0.03066 -0.01688 -0.00038 -0.00581 0.02390 0.00341 0.00027 0.00025 0.00021 0.00000 0.00117 0.00136 0.00135 0.00115 0.00102 0.00103 0.00054 C32 0.58682 0.86150 0.30984 1.00000 0.02368 0.02046 0.03032 -0.00979 0.00128 -0.00719 0.02489 0.00356 0.00027 0.00024 0.00021 0.00000 0.00124 0.00125 0.00136 0.00109 0.00106 0.00103 0.00054 H32 0.57473 0.95125 0.27157 1.00000 0.02986 0.00000 0.00000 C33 0.65577 0.78387 0.26101 1.00000 0.02129 0.02694 0.02604 -0.00995 0.00203 -0.00727 0.02504 0.00356 0.00027 0.00025 0.00021 0.00000 0.00121 0.00136 0.00130 0.00111 0.00102 0.00105 0.00055 H33 0.68900 0.82065 0.18879 1.00000 0.03005 0.00000 0.00000 C34 0.58525 0.12821 -0.03531 1.00000 0.04929 0.03953 0.03467 -0.02194 0.00344 -0.01587 0.03808 0.00404 0.00036 0.00029 0.00024 0.00000 0.00182 0.00171 0.00157 0.00139 0.00138 0.00145 0.00070 H34A 0.48265 0.16099 -0.02181 1.00000 0.05712 0.00000 0.00000 H34B 0.58744 0.06157 -0.05972 1.00000 0.05712 0.00000 0.00000 H34C 0.62213 0.19786 -0.09260 1.00000 0.05712 0.00000 0.00000 C35 0.40661 0.84290 0.56052 1.00000 0.04028 0.03659 0.02843 -0.01867 0.00407 -0.00492 0.03424 0.00422 0.00034 0.00028 0.00023 0.00000 0.00160 0.00162 0.00143 0.00128 0.00123 0.00131 0.00065 H35A 0.32469 0.80542 0.55599 1.00000 0.05136 0.00000 0.00000 H35B 0.36926 0.91109 0.58365 1.00000 0.05136 0.00000 0.00000 H35C 0.48511 0.77694 0.61440 1.00000 0.05136 0.00000 0.00000 N3 0.80130 0.40316 0.22603 1.00000 0.01325 0.02937 0.04041 -0.02174 0.00376 -0.00529 0.02528 0.00303 0.00023 0.00021 0.00019 0.00000 0.00098 0.00120 0.00130 0.00106 0.00091 0.00089 0.00048 N4 0.75606 0.57220 0.26969 1.00000 0.01567 0.02834 0.03583 -0.01864 0.00498 -0.00750 0.02458 0.00300 0.00023 0.00021 0.00019 0.00000 0.00100 0.00118 0.00124 0.00101 0.00091 0.00090 0.00047 O4 0.56435 0.48852 0.25389 1.00000 0.01700 0.04267 0.04829 -0.03115 0.00622 -0.01003 0.03142 0.00250 0.00019 0.00019 0.00016 0.00000 0.00086 0.00116 0.00119 0.00100 0.00081 0.00081 0.00045 O5 0.67740 0.07630 0.06356 1.00000 0.04484 0.02818 0.03110 -0.01684 0.00198 -0.00920 0.03313 0.00266 0.00022 0.00018 0.00015 0.00000 0.00117 0.00104 0.00103 0.00087 0.00089 0.00089 0.00046 O6 0.46616 0.89439 0.45470 1.00000 0.03104 0.02701 0.03471 -0.01862 0.00546 -0.00656 0.02916 0.00256 0.00020 0.00017 0.00015 0.00000 0.00099 0.00100 0.00105 0.00086 0.00082 0.00081 0.00043 H3N 0.89482 0.40264 0.22909 1.00000 0.03031 0.03376 0.00204 0.00272 0.00233 0.00000 0.00774 H4N 0.85057 0.56818 0.26191 1.00000 0.03047 0.03697 0.00202 0.00275 0.00233 0.00000 0.00775 Final Structure Factor Calculation for 2008lsh022 in P-1 Total number of l.s. parameters = 381 Maximum vector length = 511 Memory required = 4114 / 22995 wR2 = 0.1485 before cycle 9 for 5928 data and 0 / 381 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.019 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.103; Restrained GooF = 1.103 for 4 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0185 * P )^2 + 1.93 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0731 for 4217 Fo > 4sig(Fo) and 0.1118 for all 5928 data wR2 = 0.1485, GooF = S = 1.103, Restrained GooF = 1.103 for all data Occupancy sum of asymmetric unit = 40.00 for non-hydrogen and 32.00 for hydrogen atoms Principal mean square atomic displacements U 0.0303 0.0227 0.0157 C1 0.0315 0.0239 0.0216 C2 0.0289 0.0271 0.0202 C3 0.0332 0.0252 0.0190 C4 0.0368 0.0330 0.0206 C5 0.0328 0.0271 0.0258 C6 0.0242 0.0214 0.0176 C7 0.0245 0.0222 0.0169 C8 0.0268 0.0239 0.0182 C9 0.0275 0.0251 0.0196 C10 0.0314 0.0256 0.0186 C11 0.0436 0.0299 0.0177 C12 0.0376 0.0274 0.0192 C13 0.0415 0.0342 0.0239 C14 0.0475 0.0317 0.0202 C15 0.0355 0.0213 0.0135 N1 0.0313 0.0213 0.0136 N2 0.0420 0.0225 0.0136 O1 0.0502 0.0352 0.0216 O2 0.0468 0.0318 0.0193 O3 0.0317 0.0227 0.0156 C21 0.0339 0.0259 0.0215 C22 0.0308 0.0276 0.0224 C23 0.0354 0.0236 0.0204 C24 0.0324 0.0323 0.0222 C25 0.0324 0.0277 0.0233 C26 0.0272 0.0240 0.0168 C27 0.0304 0.0201 0.0139 C28 0.0328 0.0224 0.0170 C29 0.0289 0.0247 0.0220 C30 0.0329 0.0223 0.0165 C31 0.0318 0.0242 0.0187 C32 0.0292 0.0255 0.0204 C33 0.0507 0.0393 0.0243 C34 0.0444 0.0360 0.0223 C35 0.0416 0.0214 0.0129 N3 0.0369 0.0224 0.0145 N4 0.0538 0.0250 0.0155 O4 0.0450 0.0327 0.0217 O5 0.0366 0.0307 0.0202 O6 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.007 0.013 0.020 0.028 0.037 0.047 0.062 0.082 0.123 1.000 Number in group 630. 557. 595. 644. 579. 565. 604. 565. 597. 592. GooF 1.204 1.211 1.197 1.150 1.124 1.061 1.035 1.000 0.923 1.082 K 9.441 2.097 1.355 1.096 1.033 1.009 0.998 0.995 0.997 1.005 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.66 inf Number in group 619. 593. 574. 589. 600. 579. 602. 591. 588. 593. GooF 1.182 1.239 1.209 1.195 1.110 1.077 0.999 0.866 0.999 1.100 K 1.163 1.120 1.083 1.024 1.007 0.997 1.000 1.003 1.020 0.997 R1 0.268 0.256 0.218 0.173 0.138 0.101 0.070 0.053 0.059 0.038 Recommended weighting scheme: WGHT 0.0143 1.9252 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) -6 -3 6 59.42 11.90 4.32 0.023 1.14 6 12 4 6.13 46.48 3.91 0.045 0.91 6 0 6 50.25 15.49 3.91 0.026 1.17 5 -3 11 53.84 3.14 3.53 0.012 0.79 6 13 6 40.04 3.89 3.51 0.013 0.86 4 12 0 33.85 1.18 3.38 0.007 0.89 -4 -12 1 25.70 2.45 3.35 0.010 0.86 7 4 13 85.95 36.38 3.32 0.040 0.81 -5 11 5 -9.47 18.89 3.32 0.029 0.83 6 13 1 50.51 119.84 3.21 0.072 0.81 4 13 9 4.25 29.42 3.16 0.036 0.89 0 6 6 562.35 443.99 3.15 0.139 1.75 6 2 0 944.55 775.51 3.14 0.183 1.54 -4 -1 11 -1.61 20.29 3.11 0.030 0.98 -5 -5 9 86.73 24.95 3.11 0.033 0.91 8 0 4 3.55 29.67 3.08 0.036 1.03 7 -1 10 35.18 0.60 3.04 0.005 0.82 8 6 3 61.08 104.85 3.03 0.067 1.08 -10 -7 1 35.51 7.11 3.02 0.018 0.85 -3 -1 15 52.14 13.43 3.02 0.024 0.77 -4 2 12 175.74 247.56 3.02 0.104 0.98 8 -1 3 24.88 4.78 3.01 0.014 1.02 -4 6 15 -9.21 14.98 3.00 0.025 0.82 7 14 7 82.57 35.45 3.00 0.039 0.78 -5 -1 3 28.18 7.03 3.00 0.017 1.67 -5 11 1 29.85 1.20 3.00 0.007 0.79 -8 -2 6 -5.87 25.73 2.98 0.033 0.99 -8 1 8 12.88 0.00 2.98 0.000 0.93 -2 4 5 5292.97 4734.48 2.97 0.453 1.97 -7 -4 9 44.52 1.07 2.96 0.007 0.87 -5 1 14 52.53 0.01 2.94 0.001 0.82 -9 1 10 30.48 77.00 2.93 0.058 0.80 -3 -2 11 107.46 55.08 2.91 0.049 0.98 0 6 0 797.70 662.25 2.90 0.169 1.75 -7 8 7 25.84 0.05 2.89 0.002 0.86 -7 -7 7 28.35 0.51 2.89 0.005 0.84 -5 4 0 14.93 0.27 2.88 0.003 1.34 -6 -2 10 75.25 125.49 2.83 0.074 0.93 0 11 2 16.92 0.82 2.83 0.006 1.01 -4 -6 9 2.42 29.08 2.83 0.036 0.88 4 10 8 10.56 33.78 2.82 0.038 1.09 -9 -4 8 47.48 1.02 2.82 0.007 0.81 -6 2 12 -10.23 13.87 2.81 0.025 0.89 -1 -5 12 50.81 8.10 2.81 0.019 0.79 -3 -3 5 13.28 0.23 2.80 0.003 1.58 8 3 11 4.35 31.45 2.76 0.037 0.83 2 0 0 2400.82 2691.99 2.76 0.342 4.48 4 1 2 3552.78 3183.70 2.73 0.372 2.17 -2 -12 4 62.05 22.98 2.73 0.032 0.77 -3 3 12 19.03 0.94 2.72 0.006 1.04 Bond lengths and angles C1 - Distance Angles C2 1.3761 (0.0035) C6 1.3881 (0.0037) 119.16 (0.24) N1 1.4332 (0.0032) 120.17 (0.23) 120.64 (0.23) C1 - C2 C6 C2 - Distance Angles C1 1.3761 (0.0036) C3 1.3975 (0.0035) 121.33 (0.24) H2 0.9500 119.34 119.34 C2 - C1 C3 C3 - Distance Angles C4 1.3871 (0.0036) C2 1.3975 (0.0035) 119.13 (0.24) H3 0.9500 120.44 120.44 C3 - C4 C2 C4 - Distance Angles O2 1.3696 (0.0030) C3 1.3871 (0.0036) 124.25 (0.24) C5 1.3876 (0.0037) 116.15 (0.23) 119.58 (0.24) C4 - O2 C3 C5 - Distance Angles C6 1.3850 (0.0037) C4 1.3876 (0.0037) 120.68 (0.25) H5 0.9500 119.66 119.66 C5 - C6 C4 C6 - Distance Angles C5 1.3850 (0.0037) C1 1.3881 (0.0037) 120.06 (0.25) H6 0.9500 119.97 119.97 C6 - C5 C1 C7 - Distance Angles O1 1.2368 (0.0028) N2 1.3588 (0.0031) 123.59 (0.23) N1 1.3640 (0.0032) 121.68 (0.22) 114.73 (0.21) C7 - O1 N2 C8 - Distance Angles C9 1.3846 (0.0034) C13 1.3957 (0.0034) 118.36 (0.23) N2 1.4185 (0.0033) 123.74 (0.22) 117.81 (0.22) C8 - C9 C13 C9 - Distance Angles C8 1.3846 (0.0034) C10 1.3935 (0.0036) 120.98 (0.23) H9 0.9500 119.51 119.51 C9 - C8 C10 C10 - Distance Angles C11 1.3845 (0.0035) C9 1.3935 (0.0036) 120.01 (0.24) H10 0.9500 120.00 120.00 C10 - C11 C9 C11 - Distance Angles O3 1.3742 (0.0031) C10 1.3845 (0.0035) 125.04 (0.24) C12 1.3897 (0.0037) 115.81 (0.23) 119.15 (0.24) C11 - O3 C10 C12 - Distance Angles C13 1.3742 (0.0038) C11 1.3897 (0.0037) 120.66 (0.24) H12 0.9500 119.67 119.67 C12 - C13 C11 C13 - Distance Angles C12 1.3742 (0.0038) C8 1.3957 (0.0034) 120.84 (0.25) H13 0.9500 119.58 119.58 C13 - C12 C8 C14 - Distance Angles O2 1.4331 (0.0033) H14A 0.9800 109.47 H14B 0.9800 109.47 109.47 H14C 0.9800 109.47 109.47 109.47 C14 - O2 H14A H14B C15 - Distance Angles O3 1.4193 (0.0033) H15A 0.9800 109.47 H15B 0.9800 109.47 109.47 H15C 0.9800 109.47 109.47 109.47 C15 - O3 H15A H15B N1 - Distance Angles C7 1.3640 (0.0032) C1 1.4332 (0.0032) 122.04 (0.20) H1N 0.8506 (0.0168) 119.20 (1.88) 118.46 (1.89) N1 - C7 C1 N2 - Distance Angles C7 1.3588 (0.0031) C8 1.4185 (0.0033) 126.45 (0.21) H2N 0.8680 (0.0171) 116.72 (1.96) 116.82 (1.95) N2 - C7 C8 O1 - Distance Angles C7 1.2368 (0.0028) O1 - O2 - Distance Angles C4 1.3696 (0.0030) C14 1.4331 (0.0033) 117.27 (0.21) O2 - C4 O3 - Distance Angles C11 1.3742 (0.0031) C15 1.4193 (0.0033) 117.37 (0.21) O3 - C11 C21 - Distance Angles C22 1.3781 (0.0036) C26 1.3948 (0.0036) 119.10 (0.24) N3 1.4169 (0.0032) 120.95 (0.23) 119.90 (0.23) C21 - C22 C26 C22 - Distance Angles C21 1.3781 (0.0036) C23 1.3904 (0.0036) 121.13 (0.24) H22 0.9500 119.43 119.43 C22 - C21 C23 C23 - Distance Angles C24 1.3892 (0.0037) C22 1.3904 (0.0036) 119.38 (0.24) H23 0.9500 120.31 120.31 C23 - C24 C22 C24 - Distance Angles O5 1.3687 (0.0031) C23 1.3892 (0.0037) 123.73 (0.24) C25 1.3912 (0.0037) 116.20 (0.23) 120.07 (0.24) C24 - O5 C23 C25 - Distance Angles C26 1.3851 (0.0037) C24 1.3912 (0.0037) 119.79 (0.25) H25 0.9500 120.11 120.11 C25 - C26 C24 C26 - Distance Angles C25 1.3851 (0.0037) C21 1.3948 (0.0036) 120.52 (0.25) H26 0.9500 119.74 119.74 C26 - C25 C21 C27 - Distance Angles O4 1.2409 (0.0028) N4 1.3567 (0.0032) 122.91 (0.23) N3 1.3587 (0.0033) 122.58 (0.23) 114.51 (0.21) C27 - O4 N4 C28 - Distance Angles C29 1.3853 (0.0035) C33 1.3927 (0.0035) 119.37 (0.23) N4 1.4248 (0.0033) 120.64 (0.23) 119.90 (0.23) C28 - C29 C33 C29 - Distance Angles C28 1.3853 (0.0035) C30 1.3923 (0.0036) 120.75 (0.24) H29 0.9500 119.63 119.63 C29 - C28 C30 C30 - Distance Angles C31 1.3901 (0.0036) C29 1.3923 (0.0036) 119.57 (0.24) H30 0.9500 120.22 120.22 C30 - C31 C29 C31 - Distance Angles O6 1.3759 (0.0031) C30 1.3901 (0.0036) 124.62 (0.24) C32 1.3909 (0.0036) 115.57 (0.23) 119.81 (0.24) C31 - O6 C30 C32 - Distance Angles C33 1.3846 (0.0037) C31 1.3909 (0.0036) 120.28 (0.24) H32 0.9500 119.86 119.86 C32 - C33 C31 C33 - Distance Angles C32 1.3846 (0.0037) C28 1.3927 (0.0035) 120.20 (0.24) H33 0.9500 119.90 119.90 C33 - C32 C28 C34 - Distance Angles O5 1.4210 (0.0034) H34A 0.9800 109.47 H34B 0.9800 109.47 109.47 H34C 0.9800 109.47 109.47 109.47 C34 - O5 H34A H34B C35 - Distance Angles O6 1.4311 (0.0033) H35A 0.9800 109.47 H35B 0.9800 109.47 109.47 H35C 0.9800 109.47 109.47 109.47 C35 - O6 H35A H35B N3 - Distance Angles C27 1.3587 (0.0033) C21 1.4169 (0.0032) 123.64 (0.21) H3N 0.8647 (0.0170) 119.50 (1.94) 116.59 (1.94) N3 - C27 C21 N4 - Distance Angles C27 1.3567 (0.0032) C28 1.4248 (0.0033) 123.95 (0.21) H4N 0.8674 (0.0171) 117.16 (1.97) 118.20 (1.96) N4 - C27 C28 O4 - Distance Angles C27 1.2409 (0.0028) O4 - O5 - Distance Angles C24 1.3687 (0.0031) C34 1.4210 (0.0034) 116.53 (0.21) O5 - C24 O6 - Distance Angles C31 1.3759 (0.0031) C35 1.4311 (0.0033) 116.69 (0.21) O6 - C31 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)