+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 04mbh0601 started at 13:29:59 on 13-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 04mbh0601 in P-1 CELL 0.71073 7.3930 8.2154 23.3228 90.866 98.162 99.937 ZERR 4.00 0.0010 0.0040 0.0158 0.032 0.023 0.026 LATT 1 SFAC C H O N UNIT 44 92 28 4 V = 1380.02 F(000) = 608.0 Mu = 0.11 mm-1 Cell Wt = 1125.22 Rho = 1.354 MERG 2 OMIT -3.00 55.00 OMIT 0 -1 3 OMIT 0 1 3 EXTI 0.01307 SHEL 7 0.77 DFIX 0.84 0.02 O2W H21W O2W H22W DANG 1.35 0.02 H21W H22W HTAB O3 O1W HTAB O33 O2W EQIV_$1 x+1, y, z HTAB O1B O4B_$1 HTAB N21 O4A_$1 EQIV_$3 -x, -y+1, -z+1 HTAB N21 O1A_$3 HTAB N21 O2_$3 EQIV_$4 x-1, y, z HTAB O31A O34B_$4 HTAB N41 O34B_$4 HTAB N41 O33_$4 EQIV_$5 -x+2, -y, -z HTAB O32 O34A_$5 EQIV_$6 -x+1, -y+1, -z HTAB N41 O32_$6 HTAB N41 O31B_$6 HTAB N41 O2W_$6 HTAB O2W O31B_$6 EQIV_$8 -x+2, -y+1, -z HTAB O2W O32_$8 FMAP 2 PLAN 10 SIZE 0.06 0.20 0.20 ACTA BOND $H WGHT 0.05750 0.89630 L.S. 4 TEMP -153.00 FVAR 0.82476 MOLE 1 C1 1 -0.058858 0.660744 0.455817 11.00000 0.01998 0.02308 = 0.03115 0.00647 0.00610 0.00637 C2 1 -0.267269 0.611047 0.452075 11.00000 0.01883 0.03711 = 0.02743 0.00911 0.00709 0.00624 AFIX 13 H2 2 -0.300149 0.487610 0.449490 11.00000 -1.20000 AFIX 0 C3 1 -0.366527 0.680039 0.398330 11.00000 0.01735 0.02305 = 0.02105 -0.00131 0.00298 0.00073 AFIX 13 H3 2 -0.328172 0.630947 0.363447 11.00000 -1.20000 AFIX 0 C4 1 -0.574082 0.622414 0.396088 11.00000 0.01628 0.02869 = 0.02559 0.00354 0.00196 0.00235 O1A 3 0.038712 0.727385 0.499829 11.00000 0.02453 0.04139 = 0.02787 -0.00307 0.00222 0.00351 O1B 3 0.001445 0.624752 0.409089 11.00000 0.01323 0.03710 = 0.03661 -0.00683 0.00634 0.00146 AFIX 147 H1 2 0.115379 0.663309 0.411949 11.00000 -1.50000 AFIX 0 O2 3 -0.328956 0.670536 0.502200 11.00000 0.02958 0.13230 = 0.02481 0.01944 0.01062 0.02670 AFIX 87 H2A 2 -0.368381 0.590209 0.521614 11.00000 -1.50000 AFIX 0 O3 3 -0.313441 0.852822 0.397898 11.00000 0.02062 0.02300 = 0.04627 0.00443 0.00524 0.00188 AFIX 147 H3O 2 -0.383122 0.898487 0.415893 11.00000 -1.50000 AFIX 0 O4A 3 -0.635458 0.473817 0.387712 11.00000 0.01929 0.02633 = 0.13107 -0.01471 0.00696 -0.00198 O4B 3 -0.669087 0.731710 0.404952 11.00000 0.01881 0.02685 = 0.04020 0.00078 0.00615 0.00553 MOLE 2 C22 1 0.121306 0.077300 0.383243 11.00000 0.03316 0.03837 = 0.03010 0.00524 0.00007 0.00820 AFIX 23 H22A 2 0.063648 -0.003885 0.409191 11.00000 -1.20000 H22B 2 0.256259 0.101784 0.397401 11.00000 -1.20000 AFIX 0 C23 1 0.092339 -0.001758 0.323057 11.00000 0.04261 0.03045 = 0.04001 0.00408 0.00168 0.00539 AFIX 23 H23A 2 -0.042535 -0.023021 0.308712 11.00000 -1.20000 H23B 2 0.132865 -0.110441 0.326031 11.00000 -1.20000 AFIX 0 C24 1 0.190237 0.093821 0.278026 11.00000 0.05830 0.03334 = 0.03881 -0.00627 0.01549 0.00357 AFIX 23 H24A 2 0.173424 0.020823 0.242810 11.00000 -1.20000 H24B 2 0.324737 0.117299 0.292897 11.00000 -1.20000 AFIX 0 C25 1 0.130638 0.257661 0.259812 11.00000 0.06547 0.03024 = 0.02912 -0.00186 0.01895 -0.00243 AFIX 23 H25B 2 0.191085 0.344266 0.289750 11.00000 -1.20000 H25A 2 0.178581 0.288870 0.223238 11.00000 -1.20000 AFIX 0 C26 1 -0.077119 0.258529 0.250855 11.00000 0.06078 0.02590 = 0.02547 0.00054 -0.00166 0.00030 AFIX 23 H26A 2 -0.143286 0.143526 0.242069 11.00000 -1.20000 H26B 2 -0.107250 0.323460 0.216482 11.00000 -1.20000 AFIX 0 C27 1 -0.151383 0.328753 0.301684 11.00000 0.04072 0.03279 = 0.03106 0.00060 -0.00633 0.00256 AFIX 23 H27B 2 -0.079582 0.441361 0.311570 11.00000 -1.20000 H27A 2 -0.281553 0.340565 0.288386 11.00000 -1.20000 AFIX 0 C28 1 -0.147882 0.233417 0.356927 11.00000 0.02523 0.04471 = 0.03441 0.00423 0.00294 0.00424 AFIX 23 H28A 2 -0.219594 0.282368 0.383308 11.00000 -1.20000 H28B 2 -0.210316 0.117709 0.347250 11.00000 -1.20000 AFIX 0 N21 4 0.044578 0.232947 0.388162 11.00000 0.02715 0.04150 = 0.01948 0.00014 0.00322 0.00341 AFIX 23 H21A 2 0.124102 0.317449 0.374591 11.00000 -1.20000 H21B 2 0.045055 0.256854 0.426854 11.00000 -1.20000 AFIX 0 MOLE 3 C31 1 0.560094 0.189746 0.040428 11.00000 0.01576 0.01494 = 0.02643 -0.00296 0.00043 0.00067 C32 1 0.746906 0.139941 0.038506 11.00000 0.01566 0.01787 = 0.02072 -0.00077 0.00299 0.00357 AFIX 13 H32 2 0.729887 0.016506 0.035748 11.00000 -1.20000 AFIX 0 C33 1 0.878468 0.202350 0.093900 11.00000 0.01848 0.01390 = 0.01818 0.00054 0.00349 0.00286 AFIX 13 H33 2 0.823306 0.147838 0.127010 11.00000 -1.20000 AFIX 0 C34 1 1.060840 0.141401 0.091081 11.00000 0.01725 0.01936 = 0.01706 0.00330 0.00288 0.00485 O31A 3 0.486542 0.130127 0.084552 11.00000 0.01660 0.02769 = 0.03794 0.00926 0.00947 0.00884 AFIX 147 H31 2 0.392744 0.172485 0.087862 11.00000 -1.50000 AFIX 0 O31B 3 0.491094 0.275634 0.004038 11.00000 0.01881 0.02473 = 0.02860 0.00048 -0.00068 0.00769 O32 3 0.823813 0.204611 -0.010641 11.00000 0.02051 0.01929 = 0.02021 -0.00110 0.00394 0.00536 AFIX 147 H32O 2 0.843804 0.126621 -0.031192 11.00000 -1.50000 AFIX 0 O33 3 0.901180 0.374690 0.104441 11.00000 0.02627 0.01866 = 0.02349 -0.00140 -0.00080 0.00648 AFIX 147 H33O 2 0.877673 0.420684 0.072998 11.00000 -1.50000 AFIX 0 O34A 3 1.049973 -0.007796 0.078989 11.00000 0.02038 0.01871 = 0.03257 -0.00068 0.00518 0.00656 O34B 3 1.210479 0.245810 0.101537 11.00000 0.01568 0.02243 = 0.03281 -0.00046 0.00385 0.00264 MOLE 4 C42 1 0.242121 0.710123 0.137334 11.00000 0.02241 0.02069 = 0.02574 0.00023 0.00228 0.00611 AFIX 23 H42A 2 0.117027 0.720230 0.117646 11.00000 -1.20000 H42B 2 0.321817 0.820318 0.137929 11.00000 -1.20000 AFIX 0 C43 1 0.226998 0.664367 0.199127 11.00000 0.02784 0.02580 = 0.02640 0.00027 0.00731 0.00326 AFIX 23 H43A 2 0.158485 0.549416 0.198222 11.00000 -1.20000 H43B 2 0.149567 0.736348 0.214769 11.00000 -1.20000 AFIX 0 C44 1 0.406289 0.675138 0.242328 11.00000 0.03663 0.04523 = 0.02204 0.00170 0.00401 -0.00040 AFIX 23 H44A 2 0.375075 0.684667 0.281999 11.00000 -1.20000 H44B 2 0.453019 0.569971 0.239068 11.00000 -1.20000 AFIX 0 C45 1 0.563392 0.817476 0.235220 11.00000 0.03449 0.04121 = 0.02522 -0.01061 0.00164 -0.00194 AFIX 23 H45A 2 0.625716 0.860614 0.274219 11.00000 -1.20000 H45B 2 0.508684 0.907767 0.215829 11.00000 -1.20000 AFIX 0 C46 1 0.710148 0.772555 0.200530 11.00000 0.02505 0.03341 = 0.03249 -0.00490 -0.00103 -0.00205 AFIX 23 H46A 2 0.815117 0.866809 0.204784 11.00000 -1.20000 H46B 2 0.757721 0.677206 0.218723 11.00000 -1.20000 AFIX 0 C47 1 0.652031 0.729192 0.135807 11.00000 0.02362 0.02630 = 0.02864 -0.00349 0.00430 0.00050 AFIX 23 H47A 2 0.596507 0.820779 0.117692 11.00000 -1.20000 H47B 2 0.764889 0.722268 0.118235 11.00000 -1.20000 AFIX 0 C48 1 0.514423 0.568334 0.120831 11.00000 0.02189 0.02482 = 0.02921 -0.00342 0.00111 0.00781 AFIX 23 H48A 2 0.554591 0.507533 0.089313 11.00000 -1.20000 H48B 2 0.517473 0.498896 0.155160 11.00000 -1.20000 AFIX 0 N41 4 0.318482 0.592513 0.102156 11.00000 0.02185 0.01908 = 0.02199 -0.00065 0.00014 0.00265 AFIX 23 H41A 2 0.310113 0.627452 0.064733 11.00000 -1.20000 H41B 2 0.242601 0.490927 0.101315 11.00000 -1.20000 AFIX 0 MOLE 5 O1W 3 -0.413366 1.119808 0.466070 11.00000 0.06193 0.05700 = 0.05436 0.00606 -0.01201 -0.02544 MOLE 6 O2W 3 0.835165 0.578681 0.016253 11.00000 0.01904 0.02227 = 0.03317 0.00351 0.00389 0.00497 H21W 2 0.745310 0.627703 0.012695 11.00000 0.05704 H22W 2 0.931931 0.642946 0.011032 11.00000 0.05681 HKLF 4 Covalent radii and connectivity table for 04mbh0601 in P-1 C 0.770 H 0.320 O 0.660 N 0.700 C1 - O1A O1B C2 C2 - O2 C1 C3 C3 - O3 C4 C2 C4 - O4A O4B C3 O1A - C1 O1B - C1 O2 - C2 O3 - C3 O4A - C4 O4B - C4 C22 - N21 C23 C23 - C22 C24 C24 - C23 C25 C25 - C26 C24 C26 - C27 C25 C27 - C28 C26 C28 - N21 C27 N21 - C22 C28 C31 - O31B O31A C32 C32 - O32 C31 C33 C33 - O33 C32 C34 C34 - O34A O34B C33 O31A - C31 O31B - C31 O32 - C32 O33 - C33 O34A - C34 O34B - C34 C42 - N41 C43 C43 - C42 C44 C44 - C45 C43 C45 - C44 C46 C46 - C47 C45 C47 - C48 C46 C48 - N41 C47 N41 - C42 C48 O1W - no bonds found O2W - no bonds found Operators for generating equivalent atoms: $1 x+1, y, z $3 -x, -y+1, -z+1 $4 x-1, y, z $5 -x+2, -y, -z $6 -x+1, -y+1, -z $8 -x+2, -y+1, -z 18909 Reflections read, of which 37 rejected -9 =< h =< 8, -10 =< k =< 10, -30 =< l =< 30, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 6189 Unique reflections, of which 0 suppressed R(int) = 0.0595 R(sigma) = 0.0835 Friedel opposites merged Maximum memory for data reduction = 4382 / 61700 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. ** Cell contents from UNIT instruction and atom list do not agree ** Unit-cell contents from UNIT instruction and atom list resp. C 44.00 44.00 H 92.00 88.00 O 28.00 28.00 N 4.00 4.00 Least-squares cycle 1 Maximum vector length = 511 Memory required = 5454 / 453848 wR2 = 0.1525 before cycle 1 for 6189 data and 358 / 358 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.008 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.028; Restrained GooF = 1.028 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0575 * P )^2 + 0.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.82475 0.00191 -0.004 OSF 2 0.01307 0.00187 -0.001 EXTI Mean shift/esd = 0.004 Maximum = 0.018 for y O2 Max. shift = 0.001 A for H21W Max. dU = 0.000 for H21W Least-squares cycle 2 Maximum vector length = 511 Memory required = 5454 / 453848 wR2 = 0.1525 before cycle 2 for 6189 data and 358 / 358 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.008 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.028; Restrained GooF = 1.028 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0575 * P )^2 + 0.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.82474 0.00191 -0.006 OSF 2 0.01307 0.00187 -0.001 EXTI Mean shift/esd = 0.001 Maximum = -0.006 for z H21W Max. shift = 0.000 A for H21W Max. dU = 0.000 for H22W Least-squares cycle 3 Maximum vector length = 511 Memory required = 5454 / 453848 wR2 = 0.1524 before cycle 3 for 6189 data and 358 / 358 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.008 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.028; Restrained GooF = 1.028 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0575 * P )^2 + 0.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.82474 0.00191 -0.001 OSF 2 0.01307 0.00187 -0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for tors H3O Max. shift = 0.000 A for H3O Max. dU = 0.000 for H22W Least-squares cycle 4 Maximum vector length = 511 Memory required = 5454 / 453848 wR2 = 0.1525 before cycle 4 for 6189 data and 358 / 358 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.008 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.028; Restrained GooF = 1.028 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0575 * P )^2 + 0.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.82474 0.00191 -0.001 OSF 2 0.01307 0.00187 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.001 for tors H3O Max. shift = 0.000 A for H3O Max. dU = 0.000 for H21W Largest correlation matrix elements 0.593 y H21W / x H21W 0.544 x H22W / x H21W 0.525 EXTI / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 -0.3002 0.4876 0.4495 13 1.000 0.000 C2 O2 C1 C3 H3 -0.3282 0.6309 0.3634 13 1.000 0.000 C3 O3 C4 C2 H1 0.1154 0.6633 0.4120 147 0.840 0.000 O1B C1 H1 H2A -0.3683 0.5902 0.5216 87 0.840 0.000 O2 C2 H2A H3O -0.3832 0.8985 0.4159 147 0.840 0.000 O3 C3 H3O H22A 0.0636 -0.0039 0.4092 23 0.990 0.000 C22 N21 C23 H22B 0.2563 0.1018 0.3974 23 0.990 0.000 C22 N21 C23 H23A -0.0425 -0.0230 0.3087 23 0.990 0.000 C23 C22 C24 H23B 0.1329 -0.1104 0.3260 23 0.990 0.000 C23 C22 C24 H24A 0.1734 0.0208 0.2428 23 0.990 0.000 C24 C23 C25 H24B 0.3247 0.1173 0.2929 23 0.990 0.000 C24 C23 C25 H25B 0.1911 0.3443 0.2897 23 0.990 0.000 C25 C26 C24 H25A 0.1786 0.2889 0.2232 23 0.990 0.000 C25 C26 C24 H26A -0.1072 0.3235 0.2165 23 0.990 0.000 C26 C27 C25 H26B -0.1433 0.1435 0.2421 23 0.990 0.000 C26 C27 C25 H27B -0.0796 0.4414 0.3116 23 0.990 0.000 C27 C28 C26 H27A -0.2816 0.3406 0.2884 23 0.990 0.000 C27 C28 C26 H28A -0.2196 0.2824 0.3833 23 0.990 0.000 C28 N21 C27 H28B -0.2103 0.1177 0.3473 23 0.990 0.000 C28 N21 C27 H21A 0.1241 0.3175 0.3746 23 0.920 0.000 N21 C22 C28 H21B 0.0451 0.2569 0.4269 23 0.920 0.000 N21 C22 C28 H32 0.7299 0.0165 0.0357 13 1.000 0.000 C32 O32 C31 C33 H33 0.8233 0.1478 0.1270 13 1.000 0.000 C33 O33 C32 C34 H31 0.3928 0.1725 0.0879 147 0.840 0.000 O31A C31 H31 H32O 0.8438 0.1266 -0.0312 147 0.840 0.000 O32 C32 H32O H33O 0.8777 0.4207 0.0730 147 0.840 0.000 O33 C33 H33O H42A 0.1170 0.7202 0.1176 23 0.990 0.000 C42 N41 C43 H42B 0.3218 0.8203 0.1379 23 0.990 0.000 C42 N41 C43 H43A 0.1585 0.5494 0.1982 23 0.990 0.000 C43 C42 C44 H43B 0.1496 0.7363 0.2148 23 0.990 0.000 C43 C42 C44 H44A 0.3751 0.6847 0.2820 23 0.990 0.000 C44 C45 C43 H44B 0.4530 0.5700 0.2391 23 0.990 0.000 C44 C45 C43 H45A 0.6257 0.8606 0.2742 23 0.990 0.000 C45 C44 C46 H45B 0.5087 0.9078 0.2158 23 0.990 0.000 C45 C44 C46 H46A 0.8151 0.8668 0.2048 23 0.990 0.000 C46 C47 C45 H46B 0.7577 0.6772 0.2187 23 0.990 0.000 C46 C47 C45 H47A 0.5965 0.8208 0.1177 23 0.990 0.000 C47 C48 C46 H47B 0.7649 0.7223 0.1182 23 0.990 0.000 C47 C48 C46 H48A 0.5546 0.5075 0.0893 23 0.990 0.000 C48 N41 C47 H48B 0.5175 0.4989 0.1552 23 0.990 0.000 C48 N41 C47 H41A 0.3101 0.6275 0.0647 23 0.920 0.000 N41 C42 C48 H41B 0.2426 0.4909 0.1013 23 0.920 0.000 N41 C42 C48 04mbh0601 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 -0.05886 0.66074 0.45582 1.00000 0.01997 0.02308 0.03114 0.00647 0.00609 0.00636 0.02414 0.00518 0.00033 0.00032 0.00012 0.00000 0.00129 0.00142 0.00156 0.00117 0.00109 0.00102 0.00058 C2 -0.26727 0.61104 0.45207 1.00000 0.01883 0.03711 0.02742 0.00912 0.00710 0.00624 0.02719 0.00535 0.00033 0.00036 0.00011 0.00000 0.00130 0.00166 0.00148 0.00123 0.00102 0.00109 0.00061 H2 -0.30015 0.48761 0.44949 1.00000 0.03262 0.00000 0.00000 C3 -0.36653 0.68004 0.39833 1.00000 0.01734 0.02304 0.02104 -0.00131 0.00298 0.00073 0.02082 0.00458 0.00031 0.00031 0.00011 0.00000 0.00121 0.00141 0.00133 0.00107 0.00092 0.00097 0.00054 H3 -0.32817 0.63095 0.36345 1.00000 0.02499 0.00000 0.00000 C4 -0.57408 0.62242 0.39609 1.00000 0.01629 0.02869 0.02558 0.00354 0.00197 0.00236 0.02380 0.00495 0.00032 0.00033 0.00011 0.00000 0.00123 0.00159 0.00142 0.00116 0.00096 0.00107 0.00058 O1A 0.03871 0.72738 0.49983 1.00000 0.02452 0.04140 0.02787 -0.00307 0.00222 0.00350 0.03175 0.00355 0.00024 0.00024 0.00008 0.00000 0.00097 0.00121 0.00107 0.00090 0.00077 0.00082 0.00046 O1B 0.00145 0.62475 0.40909 1.00000 0.01322 0.03710 0.03659 -0.00683 0.00633 0.00146 0.02915 0.00335 0.00022 0.00023 0.00008 0.00000 0.00086 0.00115 0.00112 0.00088 0.00073 0.00075 0.00045 H1 0.11539 0.66327 0.41195 1.00000 0.04373 0.00000 0.00000 O2 -0.32896 0.67054 0.50220 1.00000 0.02957 0.13229 0.02481 0.01944 0.01062 0.02670 0.05991 0.00500 0.00029 0.00036 0.00009 0.00000 0.00120 0.00242 0.00119 0.00133 0.00087 0.00133 0.00076 H2A -0.36833 0.59022 0.52162 1.00000 0.08987 0.00000 0.00000 O3 -0.31344 0.85282 0.39790 1.00000 0.02061 0.02300 0.04626 0.00443 0.00524 0.00188 0.03013 0.00359 0.00023 0.00022 0.00009 0.00000 0.00095 0.00103 0.00124 0.00088 0.00078 0.00073 0.00045 H3O -0.38316 0.89849 0.41588 1.00000 0.04520 0.00000 0.00000 O4A -0.63546 0.47382 0.38771 1.00000 0.01928 0.02632 0.13107 -0.01471 0.00695 -0.00198 0.06020 0.00430 0.00026 0.00026 0.00013 0.00000 0.00106 0.00127 0.00236 0.00133 0.00117 0.00085 0.00075 O4B -0.66909 0.73171 0.40495 1.00000 0.01881 0.02686 0.04019 0.00079 0.00615 0.00553 0.02827 0.00346 0.00022 0.00022 0.00008 0.00000 0.00090 0.00105 0.00114 0.00085 0.00075 0.00075 0.00044 C22 0.12131 0.07730 0.38324 1.00000 0.03317 0.03836 0.03010 0.00524 0.00007 0.00820 0.03406 0.00556 0.00038 0.00036 0.00012 0.00000 0.00154 0.00178 0.00160 0.00133 0.00116 0.00125 0.00067 H22A 0.06365 -0.00389 0.40919 1.00000 0.04087 0.00000 0.00000 H22B 0.25626 0.10178 0.39740 1.00000 0.04087 0.00000 0.00000 C23 0.09234 -0.00176 0.32306 1.00000 0.04261 0.03044 0.03999 0.00407 0.00167 0.00540 0.03821 0.00581 0.00042 0.00037 0.00013 0.00000 0.00171 0.00170 0.00181 0.00138 0.00131 0.00129 0.00071 H23A -0.04254 -0.02302 0.30871 1.00000 0.04585 0.00000 0.00000 H23B 0.13286 -0.11044 0.32603 1.00000 0.04585 0.00000 0.00000 C24 0.19024 0.09382 0.27803 1.00000 0.05829 0.03333 0.03880 -0.00626 0.01548 0.00356 0.04328 0.00642 0.00047 0.00038 0.00014 0.00000 0.00201 0.00182 0.00186 0.00144 0.00148 0.00146 0.00078 H24A 0.17343 0.02082 0.24281 1.00000 0.05193 0.00000 0.00000 H24B 0.32474 0.11730 0.29290 1.00000 0.05193 0.00000 0.00000 C25 0.13063 0.25766 0.25981 1.00000 0.06545 0.03023 0.02912 -0.00186 0.01895 -0.00242 0.04176 0.00620 0.00045 0.00037 0.00013 0.00000 0.00213 0.00174 0.00166 0.00133 0.00145 0.00146 0.00078 H25B 0.19108 0.34426 0.28975 1.00000 0.05011 0.00000 0.00000 H25A 0.17857 0.28887 0.22324 1.00000 0.05011 0.00000 0.00000 C26 -0.07712 0.25853 0.25086 1.00000 0.06078 0.02589 0.02547 0.00055 -0.00165 0.00032 0.03905 0.00567 0.00043 0.00037 0.00012 0.00000 0.00201 0.00163 0.00160 0.00127 0.00134 0.00137 0.00074 H26A -0.10725 0.32346 0.21648 1.00000 0.04686 0.00000 0.00000 H26B -0.14329 0.14353 0.24207 1.00000 0.04686 0.00000 0.00000 C27 -0.15138 0.32875 0.30168 1.00000 0.04072 0.03279 0.03106 0.00060 -0.00633 0.00256 0.03647 0.00555 0.00040 0.00037 0.00012 0.00000 0.00168 0.00171 0.00167 0.00133 0.00124 0.00127 0.00071 H27B -0.07958 0.44136 0.31157 1.00000 0.04377 0.00000 0.00000 H27A -0.28155 0.34057 0.28839 1.00000 0.04377 0.00000 0.00000 C28 -0.14788 0.23342 0.35693 1.00000 0.02523 0.04470 0.03439 0.00422 0.00295 0.00424 0.03512 0.00562 0.00036 0.00039 0.00012 0.00000 0.00146 0.00188 0.00167 0.00139 0.00115 0.00123 0.00069 H28A -0.21959 0.28237 0.38331 1.00000 0.04215 0.00000 0.00000 H28B -0.21032 0.11771 0.34725 1.00000 0.04215 0.00000 0.00000 N21 0.04457 0.23295 0.38816 1.00000 0.02715 0.04150 0.01947 0.00014 0.00322 0.00342 0.02972 0.00427 0.00029 0.00029 0.00009 0.00000 0.00119 0.00147 0.00117 0.00103 0.00087 0.00099 0.00054 H21A 0.12410 0.31745 0.37459 1.00000 0.03567 0.00000 0.00000 H21B 0.04505 0.25686 0.42685 1.00000 0.03567 0.00000 0.00000 C31 0.56010 0.18975 0.04043 1.00000 0.01575 0.01494 0.02643 -0.00296 0.00043 0.00066 0.01959 0.00450 0.00031 0.00029 0.00011 0.00000 0.00116 0.00128 0.00140 0.00107 0.00096 0.00092 0.00053 C32 0.74691 0.13994 0.03851 1.00000 0.01565 0.01787 0.02071 -0.00077 0.00299 0.00356 0.01799 0.00452 0.00030 0.00030 0.00010 0.00000 0.00117 0.00129 0.00130 0.00101 0.00091 0.00091 0.00051 H32 0.72989 0.01651 0.03575 1.00000 0.02159 0.00000 0.00000 C33 0.87847 0.20235 0.09390 1.00000 0.01846 0.01390 0.01818 0.00054 0.00348 0.00286 0.01677 0.00437 0.00030 0.00028 0.00010 0.00000 0.00119 0.00124 0.00126 0.00097 0.00090 0.00090 0.00050 H33 0.82331 0.14784 0.12701 1.00000 0.02012 0.00000 0.00000 C34 1.06084 0.14140 0.09108 1.00000 0.01724 0.01936 0.01705 0.00330 0.00288 0.00485 0.01763 0.00463 0.00030 0.00030 0.00010 0.00000 0.00120 0.00139 0.00126 0.00102 0.00089 0.00096 0.00052 O31A 0.48654 0.13013 0.08455 1.00000 0.01660 0.02769 0.03793 0.00925 0.00947 0.00884 0.02619 0.00356 0.00022 0.00022 0.00008 0.00000 0.00090 0.00106 0.00111 0.00085 0.00074 0.00072 0.00043 H31 0.39276 0.17250 0.08787 1.00000 0.03929 0.00000 0.00000 O31B 0.49109 0.27564 0.00404 1.00000 0.01880 0.02473 0.02860 0.00048 -0.00068 0.00769 0.02400 0.00324 0.00021 0.00021 0.00007 0.00000 0.00087 0.00099 0.00101 0.00081 0.00070 0.00071 0.00041 O32 0.82381 0.20461 -0.01064 1.00000 0.02051 0.01929 0.02021 -0.00110 0.00394 0.00537 0.01970 0.00322 0.00022 0.00020 0.00007 0.00000 0.00085 0.00093 0.00092 0.00072 0.00066 0.00068 0.00038 H32O 0.84385 0.12663 -0.03119 1.00000 0.02956 0.00000 0.00000 O33 0.90118 0.37469 0.10444 1.00000 0.02627 0.01865 0.02348 -0.00140 -0.00080 0.00647 0.02296 0.00316 0.00022 0.00020 0.00007 0.00000 0.00092 0.00095 0.00096 0.00074 0.00072 0.00071 0.00040 H33O 0.87769 0.42069 0.07300 1.00000 0.03444 0.00000 0.00000 O34A 1.04997 -0.00780 0.07899 1.00000 0.02038 0.01871 0.03257 -0.00068 0.00518 0.00656 0.02341 0.00327 0.00021 0.00021 0.00007 0.00000 0.00088 0.00100 0.00105 0.00079 0.00071 0.00068 0.00041 O34B 1.21048 0.24581 0.10154 1.00000 0.01568 0.02242 0.03280 -0.00046 0.00385 0.00264 0.02371 0.00321 0.00021 0.00021 0.00007 0.00000 0.00086 0.00098 0.00104 0.00078 0.00068 0.00069 0.00041 C42 0.24212 0.71012 0.13733 1.00000 0.02242 0.02069 0.02573 0.00022 0.00228 0.00611 0.02280 0.00486 0.00033 0.00031 0.00011 0.00000 0.00129 0.00139 0.00142 0.00110 0.00098 0.00101 0.00056 H42A 0.11702 0.72023 0.11764 1.00000 0.02736 0.00000 0.00000 H42B 0.32181 0.82032 0.13793 1.00000 0.02736 0.00000 0.00000 C43 0.22700 0.66437 0.19913 1.00000 0.02784 0.02580 0.02640 0.00027 0.00732 0.00327 0.02654 0.00508 0.00034 0.00034 0.00011 0.00000 0.00139 0.00151 0.00147 0.00116 0.00107 0.00109 0.00060 H43A 0.15848 0.54942 0.19822 1.00000 0.03184 0.00000 0.00000 H43B 0.14957 0.73635 0.21477 1.00000 0.03184 0.00000 0.00000 C44 0.40629 0.67514 0.24233 1.00000 0.03662 0.04523 0.02204 0.00171 0.00400 -0.00041 0.03557 0.00541 0.00038 0.00039 0.00012 0.00000 0.00160 0.00189 0.00149 0.00132 0.00114 0.00131 0.00070 H44A 0.37508 0.68467 0.28200 1.00000 0.04269 0.00000 0.00000 H44B 0.45302 0.56997 0.23907 1.00000 0.04269 0.00000 0.00000 C45 0.56339 0.81748 0.23522 1.00000 0.03449 0.04119 0.02521 -0.01060 0.00164 -0.00195 0.03506 0.00520 0.00037 0.00037 0.00012 0.00000 0.00157 0.00185 0.00152 0.00133 0.00114 0.00127 0.00070 H45A 0.62572 0.86062 0.27422 1.00000 0.04207 0.00000 0.00000 H45B 0.50868 0.90777 0.21583 1.00000 0.04207 0.00000 0.00000 C46 0.71015 0.77256 0.20053 1.00000 0.02504 0.03340 0.03249 -0.00490 -0.00103 -0.00206 0.03176 0.00508 0.00035 0.00036 0.00012 0.00000 0.00140 0.00165 0.00159 0.00128 0.00111 0.00113 0.00065 H46A 0.81512 0.86681 0.20478 1.00000 0.03811 0.00000 0.00000 H46B 0.75772 0.67721 0.21872 1.00000 0.03811 0.00000 0.00000 C47 0.65203 0.72919 0.13581 1.00000 0.02362 0.02628 0.02862 -0.00349 0.00430 0.00050 0.02665 0.00478 0.00034 0.00033 0.00011 0.00000 0.00134 0.00151 0.00149 0.00117 0.00104 0.00106 0.00060 H47A 0.59651 0.82078 0.11769 1.00000 0.03198 0.00000 0.00000 H47B 0.76489 0.72227 0.11824 1.00000 0.03198 0.00000 0.00000 C48 0.51442 0.56834 0.12083 1.00000 0.02189 0.02482 0.02920 -0.00342 0.00111 0.00781 0.02517 0.00483 0.00032 0.00032 0.00012 0.00000 0.00130 0.00147 0.00148 0.00116 0.00102 0.00104 0.00058 H48A 0.55459 0.50753 0.08931 1.00000 0.03020 0.00000 0.00000 H48B 0.51747 0.49890 0.15516 1.00000 0.03020 0.00000 0.00000 N41 0.31848 0.59251 0.10216 1.00000 0.02185 0.01907 0.02199 -0.00066 0.00014 0.00264 0.02140 0.00385 0.00026 0.00025 0.00009 0.00000 0.00105 0.00114 0.00114 0.00090 0.00081 0.00082 0.00046 H41A 0.31011 0.62745 0.06473 1.00000 0.02568 0.00000 0.00000 H41B 0.24260 0.49093 0.10132 1.00000 0.02568 0.00000 0.00000 O1W -0.41336 1.11981 0.46607 1.00000 0.06193 0.05699 0.05437 0.00606 -0.01201 -0.02544 0.06405 0.00422 0.00033 0.00031 0.00011 0.00000 0.00156 0.00162 0.00154 0.00126 0.00117 0.00121 0.00074 O2W 0.83517 0.57868 0.01625 1.00000 0.01903 0.02227 0.03316 0.00352 0.00388 0.00497 0.02463 0.00349 0.00024 0.00022 0.00008 0.00000 0.00099 0.00102 0.00109 0.00081 0.00076 0.00079 0.00042 H21W 0.74532 0.62771 0.01266 1.00000 0.05708 0.06306 0.00297 0.00373 0.00147 0.00000 0.01094 H22W 0.93194 0.64293 0.01103 1.00000 0.05674 0.05476 0.00281 0.00348 0.00146 0.00000 0.01077 Final Structure Factor Calculation for 04mbh0601 in P-1 Total number of l.s. parameters = 358 Maximum vector length = 511 Memory required = 5096 / 22995 wR2 = 0.1525 before cycle 5 for 6189 data and 0 / 358 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.008 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.028; Restrained GooF = 1.028 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0575 * P )^2 + 0.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0588 for 3715 Fo > 4sig(Fo) and 0.1192 for all 6189 data wR2 = 0.1525, GooF = S = 1.028, Restrained GooF = 1.028 for all data Occupancy sum of asymmetric unit = 38.00 for non-hydrogen and 44.00 for hydrogen atoms Principal mean square atomic displacements U 0.0337 0.0207 0.0180 C1 0.0412 0.0236 0.0168 C2 0.0257 0.0202 0.0166 C3 0.0310 0.0242 0.0163 C4 0.0434 0.0281 0.0238 O1A 0.0462 0.0289 0.0124 O1B 0.1341 0.0266 0.0190 O2 0.0467 0.0243 0.0193 O3 0.1354 0.0285 0.0166 O4A 0.0403 0.0269 0.0176 O4B 0.0400 0.0369 0.0253 C22 0.0476 0.0375 0.0296 C23 0.0634 0.0394 0.0270 C24 0.0732 0.0287 0.0234 C25 0.0669 0.0262 0.0241 C26 0.0517 0.0331 0.0246 C27 0.0463 0.0339 0.0252 C28 0.0426 0.0271 0.0194 N21 0.0282 0.0178 0.0127 C31 0.0215 0.0174 0.0151 C32 0.0191 0.0174 0.0139 C33 0.0211 0.0168 0.0150 C34 0.0424 0.0232 0.0130 O31A 0.0313 0.0252 0.0155 O31B 0.0220 0.0212 0.0160 O32 0.0309 0.0208 0.0172 O33 0.0329 0.0223 0.0151 O34A 0.0331 0.0225 0.0155 O34B 0.0267 0.0231 0.0186 C42 0.0310 0.0254 0.0231 C43 0.0514 0.0333 0.0219 C44 0.0516 0.0350 0.0186 C45 0.0402 0.0357 0.0194 C46 0.0335 0.0254 0.0211 C47 0.0338 0.0233 0.0184 C48 0.0255 0.0208 0.0179 N41 0.1136 0.0516 0.0270 O1W 0.0337 0.0219 0.0183 O2W Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.010 0.020 0.029 0.039 0.051 0.066 0.083 0.112 0.162 1.000 Number in group 673. 615. 609. 582. 616. 642. 593. 626. 615. 618. GooF 0.905 0.902 0.973 1.053 1.112 1.055 1.068 1.094 1.115 0.987 K 3.124 1.114 0.940 0.988 0.938 0.971 1.012 1.002 1.016 1.013 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.98 1.05 1.16 1.32 1.65 inf Number in group 635. 613. 611. 618. 625. 612. 634. 605. 618. 618. GooF 0.975 0.961 0.931 0.970 0.999 1.008 1.001 0.986 1.034 1.354 K 0.985 1.033 1.019 0.992 1.002 0.998 1.016 1.028 1.030 1.002 R1 0.347 0.283 0.238 0.194 0.149 0.109 0.072 0.063 0.051 0.037 Recommended weighting scheme: WGHT 0.0575 0.8945 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) 0 0 5 -3.58 22.50 5.38 0.037 4.61 1 0 1 792.92 1182.19 5.20 0.266 6.61 -1 2 7 59.59 24.94 4.58 0.039 2.55 -1 1 3 29.30 65.11 4.53 0.062 4.91 -1 -1 2 547.91 756.62 4.36 0.212 4.78 2 -1 7 30.16 10.52 4.11 0.025 2.27 -1 1 0 281.27 391.70 3.97 0.153 5.92 3 -9 10 453.69 262.97 3.90 0.125 0.83 4 6 0 -4.25 32.39 3.87 0.044 1.00 -1 -2 3 368.22 501.17 3.87 0.173 3.14 -2 1 2 647.92 857.78 3.83 0.226 3.50 0 0 7 66.40 34.78 3.81 0.046 3.30 0 -1 2 -1.76 7.41 3.79 0.021 6.75 0 -3 22 -12.44 25.33 3.70 0.039 0.99 5 3 13 46.69 106.43 3.60 0.080 0.93 4 0 0 20.56 67.99 3.55 0.064 1.80 -1 2 5 2.48 18.68 3.54 0.033 3.00 -1 -1 10 13.77 34.48 3.52 0.045 2.20 0 2 9 142.25 95.08 3.49 0.075 2.13 -1 -1 11 147.54 96.35 3.46 0.076 2.03 2 1 4 1.28 13.96 3.44 0.029 2.58 0 -1 9 120.96 173.42 3.30 0.102 2.47 0 8 7 304.57 423.37 3.30 0.159 0.96 -5 8 17 -35.86 47.71 3.28 0.053 0.77 9 -2 6 489.41 287.13 3.28 0.131 0.77 -2 1 3 201.29 270.42 3.28 0.127 3.37 -2 -3 7 125.22 177.78 3.22 0.103 1.80 2 0 4 362.03 279.96 3.22 0.129 2.87 -1 -8 7 100.48 175.81 3.16 0.102 0.95 -6 -3 19 108.48 0.40 3.08 0.005 0.85 2 -2 3 16.10 3.92 3.07 0.015 2.68 0 2 28 80.14 1.11 3.06 0.008 0.80 5 6 6 65.70 16.31 3.02 0.031 0.86 1 -8 6 -5.05 42.97 3.02 0.051 1.00 0 -7 18 19.36 70.95 3.00 0.065 0.88 -1 -2 5 29.55 53.01 3.00 0.056 2.81 6 1 1 -3.54 37.91 3.00 0.048 1.15 -6 2 14 8.73 30.85 2.98 0.043 1.05 4 0 13 76.10 116.76 2.93 0.083 1.18 6 -5 4 10.78 35.11 2.91 0.046 1.02 1 1 0 668.74 821.96 2.90 0.221 4.96 -7 4 4 273.75 207.95 2.90 0.111 1.00 -5 7 14 123.48 202.23 2.89 0.110 0.87 -4 5 2 106.16 156.52 2.87 0.097 1.33 -2 -5 6 279.71 211.78 2.86 0.112 1.34 -1 6 9 728.95 587.95 2.83 0.187 1.20 0 -4 9 31.62 60.77 2.82 0.060 1.62 1 2 20 57.01 22.37 2.82 0.037 1.06 -3 4 9 298.33 230.20 2.82 0.117 1.47 -6 5 0 4.79 22.14 2.80 0.036 1.06 Bond lengths and angles C1 - Distance Angles O1A 1.2289 (0.0031) O1B 1.2836 (0.0031) 124.97 (0.23) C2 1.5139 (0.0034) 122.06 (0.23) 112.97 (0.23) C1 - O1A O1B C2 - Distance Angles O2 1.4229 (0.0033) C1 1.5139 (0.0034) 110.57 (0.23) C3 1.5280 (0.0036) 108.98 (0.21) 110.69 (0.20) H2 1.0000 108.85 108.85 108.85 C2 - O2 C1 C3 C3 - Distance Angles O3 1.4065 (0.0031) C4 1.5189 (0.0033) 113.85 (0.20) C2 1.5280 (0.0036) 110.89 (0.21) 108.24 (0.20) H3 1.0000 107.89 107.89 107.89 C3 - O3 C4 C2 C4 - Distance Angles O4A 1.2292 (0.0033) O4B 1.2632 (0.0030) 125.21 (0.23) C3 1.5189 (0.0033) 117.98 (0.23) 116.77 (0.23) C4 - O4A O4B O1A - Distance Angles C1 1.2289 (0.0031) O1A - O1B - Distance Angles C1 1.2836 (0.0031) H1 0.8400 109.47 O1B - C1 O2 - Distance Angles C2 1.4229 (0.0033) H2A 0.8400 109.47 O2 - C2 O3 - Distance Angles C3 1.4065 (0.0031) H3O 0.8400 109.47 O3 - C3 O4A - Distance Angles C4 1.2292 (0.0033) O4A - O4B - Distance Angles C4 1.2632 (0.0030) O4B - C22 - Distance Angles N21 1.4948 (0.0036) C23 1.5090 (0.0041) 115.40 (0.23) H22A 0.9900 108.42 108.42 H22B 0.9900 108.42 108.42 107.47 C22 - N21 C23 H22A C23 - Distance Angles C22 1.5090 (0.0041) C24 1.5127 (0.0042) 117.05 (0.26) H23A 0.9900 108.04 108.04 H23B 0.9900 108.04 108.04 107.26 C23 - C22 C24 H23A C24 - Distance Angles C23 1.5127 (0.0041) C25 1.5346 (0.0044) 117.73 (0.26) H24A 0.9900 107.87 107.87 H24B 0.9900 107.87 107.87 107.18 C24 - C23 C25 H24A C25 - Distance Angles C26 1.5217 (0.0044) C24 1.5346 (0.0044) 116.20 (0.26) H25B 0.9900 108.24 108.24 H25A 0.9900 108.24 108.24 107.37 C25 - C26 C24 H25B C26 - Distance Angles C27 1.5208 (0.0041) C25 1.5217 (0.0044) 115.53 (0.24) H26A 0.9900 108.40 108.40 H26B 0.9900 108.40 108.40 107.45 C26 - C27 C25 H26A C27 - Distance Angles C28 1.5173 (0.0041) C26 1.5208 (0.0041) 118.00 (0.26) H27B 0.9900 107.81 107.81 H27A 0.9900 107.81 107.81 107.15 C27 - C28 C26 H27B C28 - Distance Angles N21 1.5043 (0.0033) C27 1.5173 (0.0041) 113.68 (0.22) H28A 0.9900 108.83 108.83 H28B 0.9900 108.83 108.83 107.69 C28 - N21 C27 H28A N21 - Distance Angles C22 1.4948 (0.0036) C28 1.5043 (0.0033) 117.02 (0.22) H21A 0.9200 108.04 108.04 H21B 0.9200 108.04 108.04 107.27 N21 - C22 C28 H21A C31 - Distance Angles O31B 1.2238 (0.0029) O31A 1.2950 (0.0030) 125.79 (0.22) C32 1.5129 (0.0032) 122.73 (0.22) 111.49 (0.21) C31 - O31B O31A C32 - Distance Angles O32 1.4208 (0.0028) C31 1.5129 (0.0032) 110.55 (0.19) C33 1.5262 (0.0032) 110.02 (0.19) 109.83 (0.19) H32 1.0000 108.80 108.80 108.80 C32 - O32 C31 C33 C33 - Distance Angles O33 1.4103 (0.0029) C32 1.5262 (0.0032) 113.55 (0.19) C34 1.5264 (0.0031) 113.43 (0.18) 107.65 (0.19) H33 1.0000 107.29 107.29 107.29 C33 - O33 C32 C34 C34 - Distance Angles O34A 1.2400 (0.0029) O34B 1.2683 (0.0028) 125.26 (0.20) C33 1.5264 (0.0031) 116.76 (0.20) 117.98 (0.21) C34 - O34A O34B O31A - Distance Angles C31 1.2950 (0.0030) H31 0.8400 109.47 O31A - C31 O31B - Distance Angles C31 1.2238 (0.0029) O31B - O32 - Distance Angles C32 1.4208 (0.0028) H32O 0.8400 109.47 O32 - C32 O33 - Distance Angles C33 1.4103 (0.0029) H33O 0.8400 109.47 O33 - C33 O34A - Distance Angles C34 1.2400 (0.0029) O34A - O34B - Distance Angles C34 1.2683 (0.0028) O34B - C42 - Distance Angles N41 1.4904 (0.0031) C43 1.5095 (0.0036) 115.72 (0.21) H42A 0.9900 108.35 108.35 H42B 0.9900 108.35 108.35 107.43 C42 - N41 C43 H42A C43 - Distance Angles C42 1.5095 (0.0036) C44 1.5354 (0.0037) 118.53 (0.21) H43A 0.9900 107.68 107.68 H43B 0.9900 107.68 107.68 107.08 C43 - C42 C44 H43A C44 - Distance Angles C45 1.5283 (0.0039) C43 1.5354 (0.0037) 116.26 (0.24) H44A 0.9900 108.22 108.22 H44B 0.9900 108.22 108.22 107.36 C44 - C45 C43 H44A C45 - Distance Angles C44 1.5283 (0.0039) C46 1.5318 (0.0038) 115.02 (0.24) H45A 0.9900 108.52 108.51 H45B 0.9900 108.51 108.51 107.52 C45 - C44 C46 H45A C46 - Distance Angles C47 1.5287 (0.0038) C45 1.5318 (0.0038) 117.92 (0.22) H46A 0.9900 107.83 107.83 H46B 0.9900 107.83 107.83 107.16 C46 - C47 C45 H46A C47 - Distance Angles C48 1.5246 (0.0035) C46 1.5287 (0.0038) 115.50 (0.22) H47A 0.9900 108.40 108.40 H47B 0.9900 108.40 108.40 107.46 C47 - C48 C46 H47A C48 - Distance Angles N41 1.5001 (0.0030) C47 1.5246 (0.0035) 113.87 (0.21) H48A 0.9900 108.78 108.78 H48B 0.9900 108.78 108.78 107.67 C48 - N41 C47 H48A N41 - Distance Angles C42 1.4904 (0.0031) C48 1.5001 (0.0030) 118.04 (0.19) H41A 0.9200 107.80 107.80 H41B 0.9200 107.80 107.80 107.14 N41 - C42 C48 H41A O2W - Distance Angles H21W 0.8295 (0.0169) H22W 0.8377 (0.0171) 110.49 (2.48) O2W - H21W Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 2.21 2.945(4) 146.4 O3-H3O...O1W 0.84 1.90 2.716(3) 163.7 O33-H33O...O2W 0.84 1.63 2.459(2) 169.7 O1B-H1...O4B_$1 0.92 1.99 2.811(3) 148.2 N21-H21A...O4A_$1 0.92 1.91 2.795(3) 160.8 N21-H21B...O1A_$3 0.92 2.46 3.070(3) 123.9 N21-H21B...O2_$3 0.84 1.64 2.472(2) 173.5 O31A-H31...O34B_$4 0.92 1.99 2.822(3) 150.1 N41-H41B...O34B_$4 0.92 2.55 3.297(3) 138.4 N41-H41B...O33_$4 0.84 1.81 2.625(3) 161.6 O32-H32O...O34A_$5 0.92 2.16 2.918(3) 139.7 N41-H41A...O32_$6 0.92 2.38 3.136(3) 139.2 N41-H41A...O31B_$6 0.92 2.51 3.055(3) 118.5 N41-H41A...O2W_$6 0.829(17) 2.033(17) 2.857(2) 173(3) O2W-H21W...O31B_$6 0.838(17) 2.013(18) 2.845(2) 172(3) O2W-H22W...O32_$8 FMAP and GRID set by program FMAP 2 1 35 GRID -3.125 -2 -1 3.125 2 1 R1 = 0.1191 for 6189 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.69 at 0.6306 0.5592 0.4950 [ 0.67 A from H2A ] Deepest hole -0.45 at 0.2995 0.2228 0.4928 [ 0.87 A from O2 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 5051 / 44163 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.3694 0.5592 0.4950 1.00000 0.05 0.69 0.67 H2A 0.92 O2 1.37 C2 1.40 H2 Q2 1 -0.4689 1.1916 0.4748 1.00000 0.05 0.57 0.81 O1W 2.14 O2 2.33 H2A 2.52 H22B Q3 1 -0.3004 1.1516 0.4816 1.00000 0.05 0.51 0.86 O1W 2.00 O1A 2.50 H3O 2.65 H28A Q4 1 -0.3999 1.1029 0.4483 1.00000 0.05 0.44 0.46 O1W 1.86 H3O 2.49 H28A 2.57 O3 Q5 1 0.2555 0.0879 0.3435 1.00000 0.05 0.31 1.26 H22B 1.32 C23 1.36 H24B 1.44 C22 Q6 1 0.9785 0.1836 0.0918 1.00000 0.05 0.28 0.75 C34 0.79 C33 1.50 H33 1.68 O34B Q7 1 -0.6509 0.4741 0.4066 1.00000 0.05 0.28 0.47 O4A 1.30 C4 1.76 H2A 1.96 H21A Q8 1 -0.6521 0.4890 0.3618 1.00000 0.05 0.27 0.62 O4A 1.34 C4 2.04 H21A 2.12 H25B Q9 1 0.3432 0.2352 0.0885 1.00000 0.05 0.24 0.68 H31 1.08 O34B 1.49 O31A 2.11 C34 Q10 1 0.3050 0.8229 0.1202 1.00000 0.05 0.23 0.42 H42B 1.07 C42 1.49 H42A 1.96 N41 Shortest distances between peaks (including symmetry equivalents) 3 4 1.02 7 8 1.05 2 4 1.17 2 3 1.33 1 1 2.05 1 7 2.30 6 9 2.67 1 2 2.67 1 7 2.70 1 2 3.00 Time profile in seconds ----------------------- 0.09: Read and process instructions 0.00: Fit rigid groups 0.02: 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. 0.91: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.88: Structure factors and derivatives 5.28: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.39: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.11: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.13: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 04mbh0601 finished at 13:30:07 Total CPU time: 8.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++