+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008lsh011 started at 16:27:38 on 23-Jun-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh011 in P2(1) CELL 0.71073 9.7285 13.3392 12.9849 90.000 103.791 90.000 ZERR 8.00 0.0005 0.0007 0.0005 0.000 0.003 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N O UNIT 64 64 16 24 V = 1636.48 F(000) = 752.0 Mu = 0.11 mm-1 Cell Wt = 1441.31 Rho = 1.463 MERG 2 OMIT -3.00 55.00 OMIT 0 1 4 OMIT 0 -1 4 OMIT -2 1 2 OMIT 1 -1 3 OMIT 1 1 3 OMIT 0 -1 2 FMAP 2 PLAN 10 SIZE 0.20 0.20 0.30 ACTA EQIV $1 x + 1, y, z EQIV $2 x-1, y, z HTAB N1 O11_$1 HTAB N11 O1 HTAB N21 O31_$2 HTAB N31 O21 BOND $H L.S. 8 TEMP -153.00 WGHT 0.063900 0.511400 EXTI 0.022043 FVAR 0.96327 MOLE 1 C1 1 0.245382 1.300742 0.116855 11.00000 0.02501 0.02146 = 0.02334 0.00212 0.00509 0.00120 C2 1 0.121815 1.342117 0.138123 11.00000 0.02243 0.03045 = 0.03255 0.00270 0.00879 0.00017 AFIX 43 H2 2 0.044511 1.299917 0.141910 11.00000 -1.20000 AFIX 0 C3 1 0.113293 1.444155 0.153455 11.00000 0.02687 0.02887 = 0.03735 0.00142 0.01062 0.00754 AFIX 43 H3 2 0.028696 1.471296 0.166390 11.00000 -1.20000 AFIX 0 C4 1 0.223494 1.507514 0.150552 11.00000 0.03398 0.02170 = 0.02688 0.00136 0.00712 0.00227 AFIX 43 H4 2 0.216222 1.577757 0.160098 11.00000 -1.20000 AFIX 0 C5 1 0.345306 1.464932 0.133188 11.00000 0.02778 0.01723 = 0.02377 0.00389 0.00364 -0.00191 C6 1 0.359645 1.363443 0.115261 11.00000 0.02202 0.02542 = 0.02293 0.00479 0.00520 0.00170 AFIX 43 H6 2 0.444797 1.337348 0.102268 11.00000 -1.20000 AFIX 0 C7 1 0.166801 1.123950 0.080423 11.00000 0.02175 0.03232 = 0.02949 0.00338 0.00776 0.00016 C8 1 0.221082 1.022441 0.058190 11.00000 0.02491 0.02096 = 0.03795 -0.00202 0.00728 -0.00097 AFIX 137 H8A 2 0.238510 0.981571 0.122723 11.00000 -1.50000 H8B 2 0.309506 1.030425 0.035392 11.00000 -1.50000 H8C 2 0.150548 0.989277 0.001987 11.00000 -1.50000 AFIX 0 N1 3 0.263748 1.198867 0.096121 11.00000 0.02458 0.02007 = 0.03180 0.00130 0.01039 0.00082 AFIX 43 H1 2 0.349813 1.181313 0.092887 11.00000 -1.20000 AFIX 0 N2 3 0.466226 1.530391 0.131852 11.00000 0.02738 0.03044 = 0.03044 0.00353 0.00413 -0.00428 O1 4 0.042527 1.137593 0.083222 11.00000 0.02382 0.02997 = 0.05212 0.00083 0.01046 -0.00032 O2 4 0.454784 1.621050 0.148840 11.00000 0.04671 0.02489 = 0.06300 -0.00028 0.00766 -0.00798 O3 4 0.574013 1.493335 0.114310 11.00000 0.03104 0.04365 = 0.04388 -0.00066 0.01373 -0.00880 MOLE 2 C11 1 -0.249190 0.977998 0.131203 11.00000 0.02504 0.01959 = 0.02307 -0.00014 0.00463 0.00071 C12 1 -0.375078 0.938004 0.146703 11.00000 0.02472 0.02986 = 0.02848 0.00173 0.00524 0.00420 AFIX 43 H12 2 -0.453404 0.980636 0.146374 11.00000 -1.20000 AFIX 0 C13 1 -0.385669 0.835189 0.162696 11.00000 0.02618 0.03502 = 0.03003 0.00009 0.00824 -0.00289 AFIX 43 H13 2 -0.472090 0.808446 0.172636 11.00000 -1.20000 AFIX 0 C14 1 -0.272208 0.770713 0.164427 11.00000 0.03117 0.02065 = 0.02674 0.00074 0.00800 -0.00397 AFIX 43 H14 2 -0.279649 0.700393 0.173341 11.00000 -1.20000 AFIX 0 C15 1 -0.147876 0.814988 0.152408 11.00000 0.02196 0.02291 = 0.02327 -0.00251 0.00461 0.00149 C16 1 -0.133838 0.915820 0.135506 11.00000 0.02160 0.02062 = 0.02229 -0.00097 0.00564 -0.00080 AFIX 43 H16 2 -0.046648 0.942387 0.126932 11.00000 -1.20000 AFIX 0 C17 1 -0.325080 1.156401 0.097283 11.00000 0.02373 0.02646 = 0.03423 -0.00449 0.00445 0.00291 C18 1 -0.275248 1.254593 0.063501 11.00000 0.03009 0.02767 = 0.03770 0.00355 0.00764 0.00388 AFIX 137 H18A 2 -0.354549 1.289046 0.015961 11.00000 -1.50000 H18B 2 -0.200150 1.242645 0.026321 11.00000 -1.50000 H18C 2 -0.238446 1.296320 0.126124 11.00000 -1.50000 AFIX 0 N11 3 -0.231547 1.080940 0.107836 11.00000 0.02641 0.02476 = 0.03096 -0.00037 0.00771 0.00147 AFIX 43 H11 2 -0.147438 1.097314 0.099097 11.00000 -1.20000 AFIX 0 N12 3 -0.024333 0.749976 0.156276 11.00000 0.03210 0.02565 = 0.02723 -0.00129 0.00433 0.00764 O11 4 -0.444793 1.146305 0.113025 11.00000 0.02627 0.03190 = 0.06764 0.00406 0.02013 0.00156 O12 4 -0.037824 0.658925 0.171567 11.00000 0.04577 0.02064 = 0.04838 0.00318 0.01311 0.01016 O13 4 0.085252 0.787613 0.144182 11.00000 0.02888 0.03242 = 0.05016 0.00003 0.01291 0.00475 MOLE 3 C21 1 -0.284482 0.395985 0.630067 11.00000 0.02343 0.01620 = 0.02024 0.00058 0.00224 0.00081 C22 1 -0.156839 0.445364 0.633825 11.00000 0.02221 0.01617 = 0.02176 0.00091 0.00433 0.00123 AFIX 43 H22 2 -0.075937 0.409702 0.624922 11.00000 -1.20000 AFIX 0 C23 1 -0.151752 0.548200 0.650973 11.00000 0.02449 0.01768 = 0.01968 0.00081 0.00372 -0.00140 C24 1 -0.265608 0.604445 0.664192 11.00000 0.03392 0.01889 = 0.02425 -0.00097 0.00759 0.00416 AFIX 43 H24 2 -0.258473 0.674998 0.673993 11.00000 -1.20000 AFIX 0 C25 1 -0.390983 0.553792 0.662594 11.00000 0.02690 0.02659 = 0.02956 -0.00287 0.00823 0.00445 AFIX 43 H25 2 -0.471068 0.589841 0.672493 11.00000 -1.20000 AFIX 0 C26 1 -0.399822 0.451578 0.646734 11.00000 0.02052 0.02274 = 0.02762 0.00130 0.00667 0.00008 AFIX 43 H26 2 -0.485836 0.418015 0.647088 11.00000 -1.20000 AFIX 0 C27 1 -0.214491 0.224516 0.589214 11.00000 0.02222 0.01882 = 0.02589 0.00015 0.00732 -0.00053 C28 1 -0.276243 0.121796 0.558650 11.00000 0.02463 0.01997 = 0.04270 -0.00222 0.01146 -0.00150 AFIX 137 H28A 2 -0.238597 0.095114 0.500609 11.00000 -1.50000 H28B 2 -0.379532 0.126783 0.535564 11.00000 -1.50000 H28C 2 -0.250658 0.076857 0.619949 11.00000 -1.50000 AFIX 0 N21 3 -0.308317 0.293712 0.606691 11.00000 0.01659 0.01642 = 0.03191 -0.00120 0.00714 -0.00272 AFIX 43 H21 2 -0.394755 0.271931 0.602941 11.00000 -1.20000 AFIX 0 N22 3 -0.018354 0.600178 0.652112 11.00000 0.02841 0.01814 = 0.02847 0.00121 0.00575 -0.00601 O21 4 -0.088239 0.242543 0.596536 11.00000 0.02024 0.02268 = 0.04249 -0.00058 0.00987 0.00099 O22 4 -0.009038 0.689810 0.674413 11.00000 0.04637 0.01945 = 0.05366 -0.00556 0.01597 -0.00906 O23 4 0.079682 0.551517 0.631419 11.00000 0.02538 0.03065 = 0.04954 -0.00014 0.01255 -0.00491 MOLE 4 C31 1 0.213162 0.064525 0.616846 11.00000 0.02203 0.01658 = 0.02205 -0.00210 0.00601 -0.00156 C32 1 0.340809 0.015714 0.616129 11.00000 0.02013 0.02250 = 0.02224 -0.00078 0.00562 -0.00148 AFIX 43 H32 2 0.419139 0.051696 0.602953 11.00000 -1.20000 AFIX 0 C33 1 0.348885 -0.085493 0.635037 11.00000 0.02279 0.01778 = 0.02127 -0.00297 0.00524 0.00312 C34 1 0.239995 -0.143313 0.655553 11.00000 0.03329 0.01492 = 0.02787 -0.00273 0.00737 -0.00190 AFIX 43 H34 2 0.249964 -0.213495 0.667439 11.00000 -1.20000 AFIX 0 C35 1 0.114907 -0.092962 0.657826 11.00000 0.02729 0.02191 = 0.03358 -0.00195 0.01226 -0.00664 AFIX 43 H35 2 0.037640 -0.129137 0.672503 11.00000 -1.20000 AFIX 0 C36 1 0.102489 0.008398 0.639042 11.00000 0.02326 0.02004 = 0.03418 -0.00168 0.01050 -0.00205 AFIX 43 H36 2 0.016485 0.041114 0.641206 11.00000 -1.20000 AFIX 0 C37 1 0.279950 0.238911 0.579508 11.00000 0.02202 0.02148 = 0.02563 0.00037 0.00888 -0.00005 C38 1 0.214521 0.340110 0.551946 11.00000 0.02578 0.02138 = 0.03967 0.00718 0.01001 0.00112 AFIX 137 H38A 2 0.237972 0.383590 0.614527 11.00000 -1.50000 H38B 2 0.111506 0.333127 0.528422 11.00000 -1.50000 H38C 2 0.251308 0.369773 0.494869 11.00000 -1.50000 AFIX 0 N31 3 0.187014 0.166320 0.592547 11.00000 0.01919 0.01699 = 0.03150 0.00110 0.00724 0.00136 AFIX 43 H31A 2 0.098733 0.185898 0.584674 11.00000 -1.20000 AFIX 0 N32 3 0.482782 -0.137601 0.632405 11.00000 0.02706 0.02183 = 0.02633 -0.00228 0.00464 0.00533 O31 4 0.406994 0.222708 0.589876 11.00000 0.01901 0.02050 = 0.04423 0.00003 0.00879 -0.00146 O32 4 0.489875 -0.227682 0.649186 11.00000 0.03921 0.01860 = 0.05540 -0.00123 0.00686 0.00857 O33 4 0.579190 -0.087390 0.614391 11.00000 0.02847 0.03129 = 0.04134 0.00141 0.01210 0.00678 HKLF 4 Covalent radii and connectivity table for 2008lsh011 in P2(1) C 0.770 H 0.320 N 0.700 O 0.660 C1 - C6 N1 C2 C2 - C3 C1 C3 - C4 C2 C4 - C3 C5 C5 - C4 C6 N2 C6 - C5 C1 C7 - O1 N1 C8 C8 - C7 N1 - C7 C1 N2 - O3 O2 C5 O1 - C7 O2 - N2 O3 - N2 C11 - C16 C12 N11 C12 - C11 C13 C13 - C12 C14 C14 - C15 C13 C15 - C16 C14 N12 C16 - C15 C11 C17 - O11 N11 C18 C18 - C17 N11 - C17 C11 N12 - O13 O12 C15 O11 - C17 O12 - N12 O13 - N12 C21 - C22 C26 N21 C22 - C23 C21 C23 - C24 C22 N22 C24 - C23 C25 C25 - C26 C24 C26 - C25 C21 C27 - O21 N21 C28 C28 - C27 N21 - C27 C21 N22 - O22 O23 C23 O21 - C27 O22 - N22 O23 - N22 C31 - C36 N31 C32 C32 - C33 C31 C33 - C32 C34 N32 C34 - C33 C35 C35 - C36 C34 C36 - C35 C31 C37 - O31 N31 C38 C38 - C37 N31 - C37 C31 N32 - O33 O32 C33 O31 - C37 O32 - N32 O33 - N32 Operators for generating equivalent atoms: $1 x+1, y, z $2 x-1, y, z Floating origin restraints generated h k l Fo^2 Sigma Why rejected 0 9 0 21.49 5.36 observed but should be systematically absent 24487 Reflections read, of which 40 rejected -12 =< h =< 12, -17 =< k =< 17, -16 =< l =< 16, Max. 2-theta = 55.00 1 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -5 -4 14 17.37 1.56 3 8.38 -1 -2 15 17.41 2.08 2 11.36 2 Inconsistent equivalents 7352 Unique reflections, of which 0 suppressed R(int) = 0.0426 R(sigma) = 0.0490 Friedel opposites not merged Maximum memory for data reduction = 4125 / 73298 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 = 5397 / 620946 wR2 = 0.1287 before cycle 1 for 7352 data and 474 / 474 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0639 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96327 0.00199 0.001 OSF 2 0.02205 0.00313 0.001 EXTI Mean shift/esd = 0.001 Maximum = 0.005 for U12 O31 Max. shift = 0.000 A for H38C Max. dU = 0.000 for C31 Least-squares cycle 2 Maximum vector length = 511 Memory required = 5397 / 620946 wR2 = 0.1287 before cycle 2 for 7352 data and 474 / 474 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0639 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96327 0.00199 -0.002 OSF 2 0.02205 0.00313 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.002 for U12 O31 Max. shift = 0.000 A for H38C Max. dU = 0.000 for C18 Least-squares cycle 3 Maximum vector length = 511 Memory required = 5397 / 620946 wR2 = 0.1287 before cycle 3 for 7352 data and 474 / 474 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0639 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96327 0.00199 0.000 OSF 2 0.02205 0.00313 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H18A Max. dU = 0.000 for O2 Least-squares cycle 4 Maximum vector length = 511 Memory required = 5397 / 620946 wR2 = 0.1287 before cycle 4 for 7352 data and 474 / 474 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0639 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96327 0.00199 -0.001 OSF 2 0.02204 0.00313 -0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for H18B Max. dU = 0.000 for N11 Least-squares cycle 5 Maximum vector length = 511 Memory required = 5397 / 620946 wR2 = 0.1287 before cycle 5 for 7352 data and 474 / 474 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0639 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96327 0.00199 0.001 OSF 2 0.02204 0.00313 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H38B Max. dU = 0.000 for O32 Least-squares cycle 6 Maximum vector length = 511 Memory required = 5397 / 620946 wR2 = 0.1287 before cycle 6 for 7352 data and 474 / 474 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0639 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96327 0.00199 -0.001 OSF 2 0.02204 0.00313 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for H18B Max. dU = 0.000 for N31 Least-squares cycle 7 Maximum vector length = 511 Memory required = 5397 / 620946 wR2 = 0.1287 before cycle 7 for 7352 data and 474 / 474 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0639 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96327 0.00199 0.000 OSF 2 0.02204 0.00313 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C5 Max. dU = 0.000 for N11 Least-squares cycle 8 Maximum vector length = 511 Memory required = 5397 / 620946 wR2 = 0.1287 before cycle 8 for 7352 data and 474 / 474 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0639 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.96327 0.00199 0.000 OSF 2 0.02204 0.00313 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.000 for y N1 Max. shift = 0.000 A for C25 Max. dU = 0.000 for C38 Largest correlation matrix elements 0.575 EXTI / OSF Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.0445 1.2999 0.1419 43 0.950 0.000 C2 C3 C1 H3 0.0287 1.4713 0.1664 43 0.950 0.000 C3 C4 C2 H4 0.2162 1.5778 0.1601 43 0.950 0.000 C4 C3 C5 H6 0.4448 1.3373 0.1023 43 0.950 0.000 C6 C5 C1 H8A 0.2385 0.9816 0.1227 137 0.980 0.000 C8 C7 H8A H8B 0.3095 1.0304 0.0354 137 0.980 0.000 C8 C7 H8A H8C 0.1505 0.9893 0.0020 137 0.980 0.000 C8 C7 H8A H1 0.3498 1.1813 0.0929 43 0.880 0.000 N1 C7 C1 H12 -0.4534 0.9806 0.1464 43 0.950 0.000 C12 C11 C13 H13 -0.4721 0.8084 0.1726 43 0.950 0.000 C13 C12 C14 H14 -0.2796 0.7004 0.1733 43 0.950 0.000 C14 C15 C13 H16 -0.0466 0.9424 0.1269 43 0.950 0.000 C16 C15 C11 H18A -0.3545 1.2890 0.0160 137 0.980 0.000 C18 C17 H18A H18B -0.2002 1.2426 0.0263 137 0.980 0.000 C18 C17 H18A H18C -0.2384 1.2963 0.1261 137 0.980 0.000 C18 C17 H18A H11 -0.1474 1.0973 0.0991 43 0.880 0.000 N11 C17 C11 H22 -0.0759 0.4097 0.6249 43 0.950 0.000 C22 C23 C21 H24 -0.2585 0.6750 0.6740 43 0.950 0.000 C24 C23 C25 H25 -0.4711 0.5898 0.6725 43 0.950 0.000 C25 C26 C24 H26 -0.4858 0.4180 0.6471 43 0.950 0.000 C26 C25 C21 H28A -0.2386 0.0951 0.5006 137 0.980 0.000 C28 C27 H28A H28B -0.3795 0.1268 0.5356 137 0.980 0.000 C28 C27 H28A H28C -0.2507 0.0769 0.6199 137 0.980 0.000 C28 C27 H28A H21 -0.3948 0.2719 0.6029 43 0.880 0.000 N21 C27 C21 H32 0.4191 0.0517 0.6030 43 0.950 0.000 C32 C33 C31 H34 0.2500 -0.2135 0.6674 43 0.950 0.000 C34 C33 C35 H35 0.0376 -0.1291 0.6725 43 0.950 0.000 C35 C36 C34 H36 0.0165 0.0411 0.6412 43 0.950 0.000 C36 C35 C31 H38A 0.2380 0.3836 0.6145 137 0.980 0.000 C38 C37 H38A H38B 0.1115 0.3331 0.5284 137 0.980 0.000 C38 C37 H38A H38C 0.2513 0.3698 0.4949 137 0.980 0.000 C38 C37 H38A H31A 0.0987 0.1859 0.5847 43 0.880 0.000 N31 C37 C31 2008lsh011 in P2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.24538 1.30074 0.11686 1.00000 0.02501 0.02146 0.02334 0.00212 0.00509 0.00120 0.02338 0.00468 0.00027 0.00018 0.00019 0.00000 0.00129 0.00139 0.00120 0.00090 0.00094 0.00102 0.00053 C2 0.12181 1.34212 0.13812 1.00000 0.02243 0.03045 0.03255 0.00270 0.00879 0.00017 0.02810 0.00525 0.00028 0.00022 0.00020 0.00000 0.00126 0.00156 0.00134 0.00107 0.00100 0.00108 0.00056 H2 0.04451 1.29992 0.14191 1.00000 0.03372 0.00000 0.00000 C3 0.11329 1.44416 0.15346 1.00000 0.02687 0.02887 0.03735 0.00142 0.01062 0.00754 0.03053 0.00540 0.00028 0.00021 0.00021 0.00000 0.00138 0.00153 0.00153 0.00109 0.00110 0.00113 0.00060 H3 0.02870 1.47130 0.16639 1.00000 0.03663 0.00000 0.00000 C4 0.22349 1.50751 0.15055 1.00000 0.03398 0.02170 0.02688 0.00136 0.00712 0.00227 0.02755 0.00503 0.00028 0.00021 0.00020 0.00000 0.00146 0.00141 0.00133 0.00097 0.00104 0.00109 0.00058 H4 0.21622 1.57776 0.16010 1.00000 0.03305 0.00000 0.00000 C5 0.34531 1.46493 0.13319 1.00000 0.02778 0.01723 0.02377 0.00389 0.00364 -0.00191 0.02335 0.00474 0.00027 0.00018 0.00019 0.00000 0.00134 0.00128 0.00121 0.00090 0.00097 0.00100 0.00053 C6 0.35965 1.36344 0.11526 1.00000 0.02202 0.02542 0.02293 0.00479 0.00520 0.00170 0.02348 0.00467 0.00026 0.00019 0.00018 0.00000 0.00124 0.00132 0.00118 0.00096 0.00092 0.00101 0.00052 H6 0.44480 1.33735 0.10227 1.00000 0.02818 0.00000 0.00000 C7 0.16680 1.12395 0.08042 1.00000 0.02175 0.03232 0.02949 0.00338 0.00776 0.00016 0.02758 0.00495 0.00026 0.00020 0.00020 0.00000 0.00129 0.00155 0.00127 0.00105 0.00098 0.00108 0.00057 C8 0.22108 1.02244 0.05819 1.00000 0.02491 0.02096 0.03795 -0.00202 0.00728 -0.00097 0.02798 0.00487 0.00027 0.00020 0.00021 0.00000 0.00128 0.00132 0.00145 0.00102 0.00103 0.00107 0.00055 H8A 0.23851 0.98157 0.12272 1.00000 0.04196 0.00000 0.00000 H8B 0.30951 1.03043 0.03539 1.00000 0.04196 0.00000 0.00000 H8C 0.15055 0.98928 0.00199 1.00000 0.04196 0.00000 0.00000 N1 0.26375 1.19887 0.09612 1.00000 0.02458 0.02007 0.03180 0.00130 0.01039 0.00082 0.02486 0.00401 0.00023 0.00016 0.00016 0.00000 0.00109 0.00115 0.00110 0.00084 0.00084 0.00090 0.00046 H1 0.34981 1.18131 0.09289 1.00000 0.02984 0.00000 0.00000 N2 0.46623 1.53039 0.13185 1.00000 0.02738 0.03044 0.03044 0.00353 0.00413 -0.00428 0.02989 0.00426 0.00023 0.00018 0.00017 0.00000 0.00120 0.00129 0.00119 0.00093 0.00090 0.00099 0.00051 O1 0.04253 1.13759 0.08322 1.00000 0.02382 0.02997 0.05212 0.00083 0.01046 -0.00032 0.03507 0.00366 0.00019 0.00015 0.00015 0.00000 0.00099 0.00108 0.00115 0.00087 0.00083 0.00082 0.00045 O2 0.45478 1.62105 0.14884 1.00000 0.04671 0.02489 0.06300 -0.00028 0.00766 -0.00798 0.04578 0.00407 0.00024 0.00016 0.00018 0.00000 0.00134 0.00121 0.00141 0.00092 0.00105 0.00093 0.00055 O3 0.57401 1.49334 0.11431 1.00000 0.03104 0.04365 0.04388 -0.00066 0.01373 -0.00880 0.03871 0.00388 0.00020 0.00017 0.00016 0.00000 0.00109 0.00126 0.00117 0.00093 0.00089 0.00095 0.00050 C11 -0.24919 0.97800 0.13120 1.00000 0.02504 0.01959 0.02307 -0.00014 0.00463 0.00071 0.02275 0.00469 0.00026 0.00020 0.00018 0.00000 0.00128 0.00126 0.00119 0.00095 0.00095 0.00103 0.00052 C12 -0.37508 0.93800 0.14670 1.00000 0.02472 0.02986 0.02848 0.00173 0.00524 0.00420 0.02787 0.00501 0.00027 0.00021 0.00020 0.00000 0.00131 0.00150 0.00136 0.00103 0.00100 0.00112 0.00057 H12 -0.45340 0.98064 0.14637 1.00000 0.03344 0.00000 0.00000 C13 -0.38567 0.83519 0.16270 1.00000 0.02618 0.03502 0.03003 0.00009 0.00824 -0.00289 0.03015 0.00514 0.00028 0.00023 0.00019 0.00000 0.00135 0.00161 0.00135 0.00111 0.00103 0.00115 0.00059 H13 -0.47209 0.80845 0.17264 1.00000 0.03618 0.00000 0.00000 C14 -0.27221 0.77071 0.16443 1.00000 0.03117 0.02065 0.02674 0.00074 0.00800 -0.00397 0.02600 0.00486 0.00027 0.00020 0.00019 0.00000 0.00139 0.00131 0.00129 0.00096 0.00101 0.00105 0.00055 H14 -0.27965 0.70039 0.17334 1.00000 0.03120 0.00000 0.00000 C15 -0.14788 0.81499 0.15241 1.00000 0.02196 0.02291 0.02327 -0.00251 0.00461 0.00149 0.02284 0.00459 0.00026 0.00019 0.00018 0.00000 0.00120 0.00128 0.00121 0.00092 0.00090 0.00100 0.00051 C16 -0.13384 0.91582 0.13551 1.00000 0.02160 0.02062 0.02229 -0.00097 0.00564 -0.00080 0.02143 0.00455 0.00026 0.00019 0.00018 0.00000 0.00117 0.00125 0.00114 0.00089 0.00088 0.00095 0.00049 H16 -0.04665 0.94239 0.12693 1.00000 0.02572 0.00000 0.00000 C17 -0.32508 1.15640 0.09728 1.00000 0.02373 0.02646 0.03423 -0.00449 0.00445 0.00291 0.02855 0.00491 0.00027 0.00021 0.00020 0.00000 0.00130 0.00143 0.00133 0.00105 0.00103 0.00113 0.00056 C18 -0.27525 1.25459 0.06350 1.00000 0.03009 0.02767 0.03770 0.00355 0.00764 0.00388 0.03189 0.00545 0.00029 0.00021 0.00022 0.00000 0.00141 0.00152 0.00147 0.00110 0.00111 0.00118 0.00061 H18A -0.35455 1.28905 0.01596 1.00000 0.04784 0.00000 0.00000 H18B -0.20015 1.24265 0.02632 1.00000 0.04784 0.00000 0.00000 H18C -0.23845 1.29632 0.12612 1.00000 0.04784 0.00000 0.00000 N11 -0.23155 1.08094 0.10784 1.00000 0.02641 0.02476 0.03096 -0.00037 0.00771 0.00147 0.02723 0.00411 0.00024 0.00016 0.00016 0.00000 0.00118 0.00122 0.00116 0.00084 0.00088 0.00094 0.00048 H11 -0.14744 1.09731 0.09910 1.00000 0.03268 0.00000 0.00000 N12 -0.02433 0.74998 0.15628 1.00000 0.03210 0.02565 0.02723 -0.00129 0.00433 0.00764 0.02879 0.00416 0.00024 0.00017 0.00016 0.00000 0.00124 0.00123 0.00113 0.00087 0.00091 0.00097 0.00050 O11 -0.44479 1.14630 0.11303 1.00000 0.02627 0.03190 0.06764 0.00406 0.02013 0.00156 0.04043 0.00412 0.00020 0.00016 0.00018 0.00000 0.00101 0.00114 0.00133 0.00100 0.00094 0.00089 0.00049 O12 -0.03782 0.65892 0.17157 1.00000 0.04577 0.02064 0.04838 0.00318 0.01311 0.01016 0.03794 0.00397 0.00022 0.00014 0.00016 0.00000 0.00122 0.00104 0.00115 0.00081 0.00092 0.00087 0.00048 O13 0.08525 0.78761 0.14418 1.00000 0.02888 0.03242 0.05016 0.00003 0.01291 0.00475 0.03657 0.00394 0.00020 0.00016 0.00016 0.00000 0.00105 0.00112 0.00120 0.00087 0.00087 0.00088 0.00047 C21 -0.28448 0.39599 0.63007 1.00000 0.02343 0.01620 0.02024 0.00058 0.00224 0.00081 0.02045 0.00439 0.00025 0.00019 0.00017 0.00000 0.00125 0.00115 0.00114 0.00089 0.00088 0.00098 0.00050 C22 -0.15684 0.44536 0.63382 1.00000 0.02221 0.01617 0.02176 0.00091 0.00433 0.00123 0.02020 0.00453 0.00025 0.00018 0.00018 0.00000 0.00123 0.00124 0.00113 0.00087 0.00089 0.00094 0.00050 H22 -0.07594 0.40970 0.62492 1.00000 0.02424 0.00000 0.00000 C23 -0.15175 0.54820 0.65097 1.00000 0.02449 0.01768 0.01968 0.00081 0.00372 -0.00140 0.02088 0.00449 0.00026 0.00019 0.00018 0.00000 0.00132 0.00128 0.00115 0.00088 0.00092 0.00096 0.00053 C24 -0.26561 0.60445 0.66419 1.00000 0.03392 0.01889 0.02425 -0.00097 0.00759 0.00416 0.02558 0.00488 0.00027 0.00021 0.00018 0.00000 0.00146 0.00123 0.00125 0.00098 0.00100 0.00109 0.00054 H24 -0.25847 0.67500 0.67399 1.00000 0.03069 0.00000 0.00000 C25 -0.39098 0.55379 0.66259 1.00000 0.02690 0.02659 0.02956 -0.00287 0.00823 0.00445 0.02743 0.00504 0.00029 0.00020 0.00020 0.00000 0.00141 0.00145 0.00133 0.00107 0.00103 0.00107 0.00057 H25 -0.47107 0.58984 0.67249 1.00000 0.03292 0.00000 0.00000 C26 -0.39982 0.45158 0.64673 1.00000 0.02052 0.02274 0.02762 0.00130 0.00667 0.00008 0.02347 0.00476 0.00026 0.00018 0.00019 0.00000 0.00124 0.00135 0.00127 0.00094 0.00094 0.00100 0.00053 H26 -0.48584 0.41801 0.64709 1.00000 0.02816 0.00000 0.00000 C27 -0.21449 0.22452 0.58921 1.00000 0.02222 0.01882 0.02589 0.00015 0.00732 -0.00053 0.02204 0.00462 0.00025 0.00019 0.00018 0.00000 0.00125 0.00124 0.00117 0.00094 0.00090 0.00100 0.00049 C28 -0.27624 0.12180 0.55865 1.00000 0.02463 0.01997 0.04270 -0.00222 0.01146 -0.00150 0.02852 0.00500 0.00028 0.00019 0.00022 0.00000 0.00137 0.00140 0.00154 0.00106 0.00110 0.00102 0.00058 H28A -0.23860 0.09511 0.50061 1.00000 0.04278 0.00000 0.00000 H28B -0.37953 0.12678 0.53556 1.00000 0.04278 0.00000 0.00000 H28C -0.25066 0.07686 0.61995 1.00000 0.04278 0.00000 0.00000 N21 -0.30832 0.29371 0.60669 1.00000 0.01659 0.01642 0.03191 -0.00120 0.00714 -0.00272 0.02141 0.00377 0.00021 0.00015 0.00016 0.00000 0.00100 0.00107 0.00107 0.00078 0.00079 0.00081 0.00044 H21 -0.39476 0.27193 0.60294 1.00000 0.02569 0.00000 0.00000 N22 -0.01835 0.60018 0.65211 1.00000 0.02841 0.01814 0.02847 0.00121 0.00575 -0.00601 0.02518 0.00397 0.00022 0.00016 0.00016 0.00000 0.00119 0.00112 0.00110 0.00086 0.00086 0.00092 0.00047 O21 -0.08824 0.24254 0.59654 1.00000 0.02024 0.02268 0.04249 -0.00058 0.00987 0.00099 0.02807 0.00338 0.00018 0.00014 0.00014 0.00000 0.00091 0.00096 0.00102 0.00077 0.00072 0.00077 0.00041 O22 -0.00904 0.68981 0.67441 1.00000 0.04637 0.01945 0.05366 -0.00556 0.01597 -0.00906 0.03914 0.00374 0.00022 0.00015 0.00016 0.00000 0.00127 0.00101 0.00127 0.00086 0.00098 0.00088 0.00050 O23 0.07968 0.55152 0.63142 1.00000 0.02538 0.03065 0.04954 -0.00014 0.01255 -0.00491 0.03458 0.00383 0.00021 0.00015 0.00016 0.00000 0.00103 0.00111 0.00115 0.00087 0.00083 0.00083 0.00046 C31 0.21316 0.06453 0.61685 1.00000 0.02203 0.01658 0.02205 -0.00210 0.00601 -0.00156 0.02010 0.00441 0.00026 0.00018 0.00018 0.00000 0.00126 0.00119 0.00117 0.00089 0.00090 0.00094 0.00050 C32 0.34081 0.01571 0.61613 1.00000 0.02013 0.02250 0.02224 -0.00078 0.00562 -0.00148 0.02153 0.00456 0.00025 0.00019 0.00018 0.00000 0.00119 0.00136 0.00120 0.00092 0.00090 0.00100 0.00052 H32 0.41914 0.05170 0.60295 1.00000 0.02583 0.00000 0.00000 C33 0.34888 -0.08549 0.63504 1.00000 0.02279 0.01778 0.02127 -0.00297 0.00524 0.00312 0.02061 0.00460 0.00025 0.00019 0.00018 0.00000 0.00126 0.00127 0.00115 0.00088 0.00089 0.00093 0.00051 C34 0.23999 -0.14331 0.65555 1.00000 0.03329 0.01492 0.02787 -0.00273 0.00737 -0.00190 0.02535 0.00474 0.00028 0.00020 0.00019 0.00000 0.00143 0.00122 0.00129 0.00097 0.00101 0.00107 0.00055 H34 0.24996 -0.21349 0.66744 1.00000 0.03042 0.00000 0.00000 C35 0.11491 -0.09296 0.65783 1.00000 0.02729 0.02191 0.03358 -0.00195 0.01226 -0.00664 0.02675 0.00488 0.00028 0.00020 0.00020 0.00000 0.00137 0.00138 0.00136 0.00103 0.00101 0.00104 0.00056 H35 0.03764 -0.12914 0.67250 1.00000 0.03210 0.00000 0.00000 C36 0.10249 0.00840 0.63904 1.00000 0.02326 0.02004 0.03418 -0.00168 0.01050 -0.00205 0.02521 0.00483 0.00027 0.00019 0.00020 0.00000 0.00129 0.00136 0.00135 0.00098 0.00101 0.00103 0.00055 H36 0.01649 0.04111 0.64121 1.00000 0.03026 0.00000 0.00000 C37 0.27995 0.23891 0.57951 1.00000 0.02202 0.02148 0.02563 0.00037 0.00888 -0.00005 0.02250 0.00462 0.00025 0.00019 0.00018 0.00000 0.00124 0.00130 0.00118 0.00096 0.00091 0.00101 0.00050 C38 0.21452 0.34011 0.55195 1.00000 0.02578 0.02138 0.03967 0.00718 0.01001 0.00112 0.02857 0.00523 0.00027 0.00020 0.00021 0.00000 0.00132 0.00139 0.00144 0.00107 0.00105 0.00105 0.00056 H38A 0.23797 0.38359 0.61453 1.00000 0.04286 0.00000 0.00000 H38B 0.11151 0.33313 0.52842 1.00000 0.04286 0.00000 0.00000 H38C 0.25131 0.36977 0.49487 1.00000 0.04286 0.00000 0.00000 N31 0.18701 0.16632 0.59255 1.00000 0.01919 0.01699 0.03150 0.00110 0.00724 0.00136 0.02236 0.00382 0.00021 0.00015 0.00015 0.00000 0.00103 0.00106 0.00106 0.00079 0.00081 0.00082 0.00044 H31A 0.09873 0.18590 0.58467 1.00000 0.02683 0.00000 0.00000 N32 0.48278 -0.13760 0.63241 1.00000 0.02706 0.02183 0.02633 -0.00228 0.00464 0.00533 0.02536 0.00406 0.00023 0.00017 0.00016 0.00000 0.00117 0.00118 0.00108 0.00083 0.00083 0.00089 0.00047 O31 0.40699 0.22271 0.58988 1.00000 0.01901 0.02050 0.04423 0.00003 0.00879 -0.00146 0.02770 0.00333 0.00017 0.00013 0.00014 0.00000 0.00090 0.00092 0.00104 0.00077 0.00071 0.00073 0.00040 O32 0.48987 -0.22768 0.64919 1.00000 0.03921 0.01860 0.05540 -0.00123 0.00686 0.00857 0.03848 0.00395 0.00022 0.00015 0.00017 0.00000 0.00117 0.00105 0.00126 0.00086 0.00093 0.00084 0.00049 O33 0.57919 -0.08739 0.61439 1.00000 0.02847 0.03129 0.04134 0.00141 0.01210 0.00678 0.03306 0.00379 0.00020 0.00015 0.00015 0.00000 0.00100 0.00112 0.00106 0.00085 0.00080 0.00084 0.00045 Final Structure Factor Calculation for 2008lsh011 in P2(1) Total number of l.s. parameters = 474 Maximum vector length = 511 Memory required = 4925 / 25046 wR2 = 0.1287 before cycle 9 for 7352 data and 2 / 474 parameters GooF = S = 1.068; Restrained GooF = 1.068 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0639 * P )^2 + 0.51 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0503 for 6174 Fo > 4sig(Fo) and 0.0649 for all 7352 data wR2 = 0.1287, GooF = S = 1.068, Restrained GooF = 1.068 for all data Flack x parameter = 1.3721 with esd 0.9483 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 52.00 for non-hydrogen and 32.00 for hydrogen atoms Principal mean square atomic displacements U 0.0255 0.0247 0.0199 C1 0.0344 0.0287 0.0211 C2 0.0386 0.0335 0.0195 C3 0.0345 0.0270 0.0211 C4 0.0310 0.0238 0.0152 C5 0.0291 0.0222 0.0191 C6 0.0346 0.0274 0.0208 C7 0.0384 0.0249 0.0206 C8 0.0328 0.0219 0.0199 N1 0.0380 0.0274 0.0243 N2 0.0523 0.0300 0.0229 O1 0.0666 0.0484 0.0223 O2 0.0487 0.0434 0.0241 O3 0.0260 0.0228 0.0195 C11 0.0322 0.0291 0.0222 C12 0.0359 0.0302 0.0243 C13 0.0325 0.0266 0.0189 C14 0.0267 0.0218 0.0200 C15 0.0229 0.0213 0.0200 C16 0.0383 0.0258 0.0215 C17 0.0388 0.0323 0.0245 C18 0.0310 0.0271 0.0236 N11 0.0392 0.0267 0.0205 N12 0.0685 0.0314 0.0214 O11 0.0510 0.0458 0.0170 O12 0.0502 0.0353 0.0242 O13 0.0261 0.0192 0.0160 C21 0.0232 0.0215 0.0158 C22 0.0258 0.0196 0.0172 C23 0.0351 0.0243 0.0173 C24 0.0324 0.0297 0.0202 C25 0.0279 0.0224 0.0200 C26 0.0262 0.0213 0.0187 C27 0.0430 0.0230 0.0195 C28 0.0320 0.0187 0.0136 N21 0.0325 0.0280 0.0151 N22 0.0425 0.0230 0.0187 O21 0.0564 0.0444 0.0166 O22 0.0496 0.0332 0.0209 O23 0.0234 0.0211 0.0158 C31 0.0236 0.0217 0.0193 C32 0.0254 0.0219 0.0145 C33 0.0335 0.0282 0.0143 C34 0.0368 0.0268 0.0167 C35 0.0349 0.0219 0.0189 C36 0.0269 0.0215 0.0191 C37 0.0422 0.0248 0.0188 C38 0.0316 0.0192 0.0163 N31 0.0327 0.0254 0.0180 N32 0.0444 0.0213 0.0175 O31 0.0585 0.0415 0.0154 O32 0.0424 0.0350 0.0218 O33 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.025 0.039 0.051 0.063 0.076 0.095 0.116 0.150 0.217 1.000 Number in group 766. 731. 729. 751. 714. 753. 715. 725. 734. 734. GooF 1.140 1.036 1.076 1.062 1.080 1.075 1.037 0.931 1.013 1.203 K 1.592 1.072 0.997 0.987 1.002 0.983 0.997 1.006 1.012 1.023 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.64 inf Number in group 736. 756. 720. 726. 751. 737. 717. 738. 732. 739. GooF 0.949 0.933 1.004 0.986 1.026 1.010 0.999 0.969 1.156 1.520 K 1.022 1.037 1.006 1.000 1.007 1.017 1.039 1.029 1.043 0.999 R1 0.151 0.134 0.116 0.092 0.066 0.054 0.042 0.038 0.041 0.041 Recommended weighting scheme: WGHT 0.0629 0.5274 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 6 0 57.61 18.39 6.64 0.041 2.16 -10 -2 13 13.76 54.51 6.60 0.071 0.77 -4 1 2 222.06 121.89 6.57 0.106 2.37 -4 -1 2 214.65 121.63 6.10 0.106 2.37 1 -6 0 53.32 18.30 5.98 0.041 2.16 4 0 2 23.12 1.53 5.86 0.012 2.06 9 -4 8 2.94 55.60 5.72 0.072 0.77 -10 0 2 69.47 24.36 5.63 0.047 0.97 -4 0 4 77.37 39.46 5.36 0.060 2.15 -2 -5 1 464.62 302.84 5.32 0.167 2.33 -2 5 1 463.30 302.80 5.25 0.167 2.33 2 6 1 171.66 102.52 5.20 0.097 1.96 -6 -9 6 20.58 0.92 5.08 0.009 1.03 3 -6 4 24.83 5.71 4.96 0.023 1.49 2 -5 1 743.99 516.67 4.95 0.218 2.24 2 -6 1 169.26 102.28 4.93 0.097 1.96 2 5 1 739.06 516.83 4.77 0.218 2.24 0 -11 2 40.62 14.56 4.70 0.037 1.19 0 -2 0 162.30 260.58 4.25 0.155 6.67 -1 1 8 7.68 0.45 4.22 0.006 1.61 -1 -1 8 7.03 0.45 4.14 0.006 1.61 2 1 0 500.51 691.08 4.04 0.252 4.45 2 -1 0 498.98 690.23 3.89 0.252 4.45 3 6 4 34.02 5.68 3.86 0.023 1.49 -8 4 6 20.49 5.18 3.84 0.022 1.09 4 0 4 137.77 94.07 3.78 0.093 1.71 2 6 5 108.45 71.32 3.76 0.081 1.50 -2 11 2 141.73 93.96 3.68 0.093 1.17 -8 -7 3 121.51 184.28 3.63 0.130 1.02 10 0 2 68.23 38.56 3.62 0.060 0.90 -6 8 12 24.63 45.26 3.60 0.065 0.85 -5 -3 2 361.32 267.73 3.59 0.157 1.78 0 0 5 -0.86 4.93 3.55 0.021 2.52 -2 6 3 48.17 27.36 3.51 0.050 1.89 0 2 0 175.38 259.41 3.47 0.155 6.67 -7 9 4 22.13 46.04 3.42 0.065 1.00 2 -6 5 103.09 71.07 3.39 0.081 1.50 3 -6 0 100.33 68.45 3.36 0.079 1.82 -10 -5 2 52.98 87.70 3.36 0.090 0.91 -6 5 1 25.74 10.54 3.34 0.031 1.38 3 6 0 99.98 68.43 3.33 0.079 1.82 -8 -7 7 15.23 34.14 3.29 0.056 0.96 -6 9 2 126.22 86.24 3.26 0.089 1.09 -5 13 9 32.75 9.35 3.21 0.029 0.80 -5 3 2 351.31 267.70 3.21 0.157 1.78 -6 -10 1 111.94 162.90 3.18 0.122 1.03 4 -1 0 313.80 235.13 3.17 0.147 2.33 4 -5 0 123.28 168.74 3.12 0.125 1.77 4 1 0 304.39 234.79 3.11 0.147 2.33 0 11 2 33.59 14.70 3.09 0.037 1.19 Bond lengths and angles C1 - Distance Angles C6 1.3952 (0.0035) N1 1.4050 (0.0032) 116.03 (0.23) C2 1.4086 (0.0036) 119.22 (0.24) 124.75 (0.24) C1 - C6 N1 C2 - Distance Angles C3 1.3809 (0.0040) C1 1.4086 (0.0036) 119.86 (0.25) H2 0.9500 120.07 120.07 C2 - C3 C1 C3 - Distance Angles C4 1.3727 (0.0038) C2 1.3809 (0.0040) 121.92 (0.25) H3 0.9500 119.04 119.04 C3 - C4 C2 C4 - Distance Angles C3 1.3727 (0.0038) C5 1.3803 (0.0036) 117.24 (0.25) H4 0.9500 121.38 121.38 C4 - C3 C5 C5 - Distance Angles C4 1.3803 (0.0036) C6 1.3863 (0.0035) 123.64 (0.24) N2 1.4684 (0.0033) 118.60 (0.23) 117.76 (0.23) C5 - C4 C6 C6 - Distance Angles C5 1.3863 (0.0035) C1 1.3952 (0.0035) 118.07 (0.24) H6 0.9500 120.97 120.97 C6 - C5 C1 C7 - Distance Angles O1 1.2317 (0.0031) N1 1.3558 (0.0034) 122.63 (0.25) C8 1.5061 (0.0037) 122.00 (0.24) 115.36 (0.21) C7 - O1 N1 C8 - Distance Angles C7 1.5061 (0.0037) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - C7 H8A H8B N1 - Distance Angles C7 1.3558 (0.0034) C1 1.4050 (0.0032) 128.76 (0.23) H1 0.8800 115.62 115.62 N1 - C7 C1 N2 - Distance Angles O3 1.2287 (0.0030) O2 1.2390 (0.0032) 122.85 (0.24) C5 1.4684 (0.0033) 118.98 (0.23) 118.17 (0.23) N2 - O3 O2 O1 - Distance Angles C7 1.2317 (0.0031) O1 - O2 - Distance Angles N2 1.2390 (0.0032) O2 - O3 - Distance Angles N2 1.2287 (0.0030) O3 - C11 - Distance Angles C16 1.3858 (0.0035) C12 1.3937 (0.0035) 119.74 (0.24) N11 1.4255 (0.0033) 116.60 (0.23) 123.64 (0.23) C11 - C16 C12 C12 - Distance Angles C11 1.3937 (0.0035) C13 1.3946 (0.0040) 119.77 (0.24) H12 0.9500 120.11 120.11 C12 - C11 C13 C13 - Distance Angles C12 1.3946 (0.0040) C14 1.3953 (0.0039) 121.49 (0.25) H13 0.9500 119.26 119.26 C13 - C12 C14 C14 - Distance Angles C15 1.3879 (0.0035) C13 1.3953 (0.0039) 116.31 (0.24) H14 0.9500 121.85 121.85 C14 - C15 C13 C15 - Distance Angles C16 1.3748 (0.0036) C14 1.3879 (0.0035) 123.82 (0.24) N12 1.4732 (0.0032) 118.04 (0.23) 118.13 (0.23) C15 - C16 C14 C16 - Distance Angles C15 1.3748 (0.0036) C11 1.3858 (0.0035) 118.79 (0.23) H16 0.9500 120.60 120.60 C16 - C15 C11 C17 - Distance Angles O11 1.2368 (0.0032) N11 1.3418 (0.0034) 122.94 (0.26) C18 1.4981 (0.0039) 121.79 (0.24) 115.27 (0.23) C17 - O11 N11 C18 - Distance Angles C17 1.4981 (0.0039) H18A 0.9800 109.47 H18B 0.9800 109.47 109.47 H18C 0.9800 109.47 109.47 109.47 C18 - C17 H18A H18B N11 - Distance Angles C17 1.3418 (0.0034) C11 1.4255 (0.0033) 129.14 (0.23) H11 0.8800 115.43 115.43 N11 - C17 C11 N12 - Distance Angles O13 1.2219 (0.0030) O12 1.2427 (0.0030) 123.42 (0.23) C15 1.4732 (0.0032) 118.91 (0.22) 117.67 (0.23) N12 - O13 O12 O11 - Distance Angles C17 1.2368 (0.0032) O11 - O12 - Distance Angles N12 1.2427 (0.0030) O12 - O13 - Distance Angles N12 1.2219 (0.0030) O13 - C21 - Distance Angles C22 1.3962 (0.0034) C26 1.4041 (0.0034) 118.83 (0.23) N21 1.4048 (0.0031) 124.42 (0.22) 116.70 (0.22) C21 - C22 C26 C22 - Distance Angles C23 1.3887 (0.0033) C21 1.3962 (0.0034) 117.97 (0.23) H22 0.9500 121.01 121.01 C22 - C23 C21 C23 - Distance Angles C24 1.3820 (0.0036) C22 1.3887 (0.0033) 123.86 (0.24) N22 1.4683 (0.0031) 118.36 (0.22) 117.75 (0.22) C23 - C24 C22 C24 - Distance Angles C23 1.3820 (0.0036) C25 1.3902 (0.0039) 117.43 (0.24) H24 0.9500 121.29 121.29 C24 - C23 C25 C25 - Distance Angles C26 1.3785 (0.0037) C24 1.3902 (0.0039) 120.41 (0.25) H25 0.9500 119.79 119.79 C25 - C26 C24 C26 - Distance Angles C25 1.3785 (0.0037) C21 1.4041 (0.0034) 121.45 (0.24) H26 0.9500 119.28 119.28 C26 - C25 C21 C27 - Distance Angles O21 1.2328 (0.0029) N21 1.3548 (0.0032) 123.56 (0.23) C28 1.5107 (0.0036) 121.58 (0.23) 114.86 (0.21) C27 - O21 N21 C28 - Distance Angles C27 1.5107 (0.0036) H28A 0.9800 109.47 H28B 0.9800 109.47 109.47 H28C 0.9800 109.47 109.47 109.47 C28 - C27 H28A H28B N21 - Distance Angles C27 1.3548 (0.0032) C21 1.4048 (0.0031) 127.93 (0.21) H21 0.8800 116.03 116.03 N21 - C27 C21 N22 - Distance Angles O22 1.2284 (0.0029) O23 1.2350 (0.0029) 123.05 (0.22) C23 1.4683 (0.0031) 118.51 (0.22) 118.43 (0.21) N22 - O22 O23 O21 - Distance Angles C27 1.2328 (0.0029) O21 - O22 - Distance Angles N22 1.2284 (0.0029) O22 - O23 - Distance Angles N22 1.2350 (0.0029) O23 - C31 - Distance Angles C36 1.3967 (0.0033) N31 1.4035 (0.0031) 117.24 (0.22) C32 1.4042 (0.0034) 118.64 (0.22) 124.08 (0.21) C31 - C36 N31 C32 - Distance Angles C33 1.3711 (0.0036) C31 1.4042 (0.0034) 117.93 (0.23) H32 0.9500 121.03 121.03 C32 - C33 C31 C33 - Distance Angles C32 1.3711 (0.0036) C34 1.3866 (0.0035) 124.63 (0.23) N32 1.4840 (0.0031) 118.05 (0.22) 117.32 (0.22) C33 - C32 C34 C34 - Distance Angles C33 1.3866 (0.0035) C35 1.3964 (0.0037) 116.49 (0.23) H34 0.9500 121.75 121.75 C34 - C33 C35 C35 - Distance Angles C36 1.3741 (0.0038) C34 1.3964 (0.0037) 120.64 (0.25) H35 0.9500 119.68 119.68 C35 - C36 C34 C36 - Distance Angles C35 1.3741 (0.0038) C31 1.3967 (0.0033) 121.64 (0.25) H36 0.9500 119.18 119.18 C36 - C35 C31 C37 - Distance Angles O31 1.2301 (0.0029) N31 1.3626 (0.0031) 122.73 (0.23) C38 1.4990 (0.0035) 122.87 (0.22) 114.40 (0.20) C37 - O31 N31 C38 - Distance Angles C37 1.4990 (0.0035) H38A 0.9800 109.47 H38B 0.9800 109.47 109.47 H38C 0.9800 109.47 109.47 109.47 C38 - C37 H38A H38B N31 - Distance Angles C37 1.3626 (0.0031) C31 1.4035 (0.0031) 128.71 (0.21) H31A 0.8800 115.64 115.64 N31 - C37 C31 N32 - Distance Angles O33 1.2197 (0.0029) O32 1.2202 (0.0029) 124.17 (0.23) C33 1.4840 (0.0031) 117.81 (0.20) 118.01 (0.22) N32 - O33 O32 O31 - Distance Angles C37 1.2301 (0.0029) O31 - O32 - Distance Angles N32 1.2202 (0.0029) O32 - O33 - Distance Angles N32 1.2197 (0.0029) O33 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 2.01 2.878(3) 169.9 N1-H1...O11_$1 0.88 1.98 2.862(3) 178.1 N11-H11...O1 0.88 2.01 2.886(3) 178.4 N21-H21...O31_$2 0.88 2.01 2.876(3) 168.2 N31-H31A...O21 FMAP and GRID set by program FMAP 2 1 25 GRID -2.273 -2 -2 2.273 2 2 R1 = 0.0591 for 3892 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.56 at 0.0844 0.6260 0.9095 [ 0.75 A from H11 ] Deepest hole -0.25 at 0.0243 0.7243 0.1369 [ 0.68 A from N12 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 4719 / 31679 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.0844 1.1260 0.0905 1.00000 0.05 0.56 0.75 H11 1.27 O1 1.62 N11 1.98 H18B Q2 1 0.4042 1.1468 0.0889 1.00000 0.05 0.48 0.71 H1 1.43 O11 1.56 N1 1.85 H8B Q3 1 -0.2098 1.1422 0.0883 1.00000 0.05 0.35 0.84 H11 0.90 N11 1.17 C17 1.58 H18B Q4 1 -0.3203 1.0753 0.1051 1.00000 0.05 0.33 0.86 N11 1.09 C17 1.47 C11 1.56 O11 Q5 1 0.1739 1.2056 0.0895 1.00000 0.05 0.33 0.86 N1 1.10 C7 1.45 C1 1.55 O1 Q6 1 0.2949 1.3279 0.1021 1.00000 0.05 0.32 0.67 C1 0.77 C6 1.46 H6 1.75 N1 Q7 1 0.4109 1.3330 0.1005 1.00000 0.05 0.27 0.33 H6 0.70 C6 1.73 C1 1.95 C5 Q8 1 0.0302 0.2275 0.5823 1.00000 0.05 0.27 0.86 H31A 1.23 O21 1.71 N31 1.83 H38B Q9 1 -0.0306 0.8630 0.1438 1.00000 0.05 0.26 1.09 H16 1.21 C16 1.34 C15 1.51 O13 Q10 1 -0.3128 0.9576 0.1238 1.00000 0.05 0.25 0.66 C11 0.78 C12 1.50 H12 1.80 C16 Shortest distances between peaks (including symmetry equivalents) 6 7 1.14 1 3 1.23 3 4 1.45 4 10 1.59 5 6 1.99 2 5 2.38 1 4 2.44 2 7 2.49 2 6 2.66 1 5 2.73 3 10 2.74 2 4 2.81 5 7 2.84 9 10 2.98 Time profile in seconds ----------------------- 0.19: Read and process instructions 0.00: Fit rigid groups 0.01: Interpret restraints etc. 0.00: Generate connectivity array 0.02: 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. 1.70: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.05: Set up l.s. refinement 0.00: Generate idealized H-atoms 5.45: Structure factors and derivatives 19.30: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.05: Apply other restraints 1.42: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.11: Analysis of variance 0.04: Merge reflections for Fourier and .fcf 0.04: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008lsh011 finished at 16:28:10 Total CPU time: 28.5 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++