+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 04mbh0606 started at 12:57:46 on 14-Aug-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 04mbh0606 in P-1 CELL 0.71073 4.8651 9.4161 19.1274 98.133 95.126 97.982 ZERR 2.00 0.0021 0.0032 0.0119 0.030 0.069 0.031 LATT 1 SFAC C H O N UNIT 24 50 26 2 V = 853.69 F(000) = 416.0 Mu = 0.14 mm-1 Cell Wt = 782.66 Rho = 1.522 MERG 2 OMIT -3.00 55.00 DFIX 0.84 0.02 O1W H1W O1W H2W DANG 1.35 0.02 H1W H2W SHEL 7 0.77 HTAB O2 O1B HTAB O32 O4B HTAB O32 O31B EQIV_$1 -x+3, -y+1, -z+1 HTAB O1A O31A_$1 EQIV_$2 -x+2, -y+2, -z+1 HTAB O2 O3_$2 EQIV_$3 x+1, y, z HTAB O3 O2_$3 HTAB O33 O32_$3 EQIV_$4 x-1, y, z HTAB O4A O31B_$4 EQIV_$5 -x+2, -y+1, -z+1 HTAB N25 O4B_$5 HTAB N25 O3_$5 HTAB N25 O33_$5 HTAB O1W O34A_$5 HTAB O1W O33_$5 EQIV_$6 x-1, y-1, z HTAB N25 O1B_$6 EQIV_$7 x, y, z-1 HTAB O34B O1W_$7 EQIV_$8 -x+1, -y+1, -z+1 HTAB O1W O34A_$8 FMAP 2 PLAN 10 SIZE 0.02 0.10 0.20 ACTA BOND $H WGHT 0.05460 0.18280 L.S. 4 TEMP -153.00 FVAR 0.90493 MOLE 1 C1 1 1.167581 0.835653 0.607995 11.00000 0.01634 0.02132 = 0.01698 0.00395 0.00351 0.00595 C2 1 0.937825 0.775120 0.548008 11.00000 0.01692 0.01519 = 0.02049 0.00291 -0.00099 0.00284 AFIX 13 H2 2 0.817723 0.691888 0.562753 11.00000 -1.20000 AFIX 0 C3 1 1.065517 0.717794 0.481695 11.00000 0.01646 0.01608 = 0.01968 0.00464 0.00053 0.00133 AFIX 13 H3 2 1.170923 0.638074 0.492399 11.00000 -1.20000 AFIX 0 C4 1 0.838468 0.658255 0.421337 11.00000 0.01726 0.01478 = 0.02153 0.00186 0.00410 0.00560 O1A 3 1.289647 0.731623 0.627485 11.00000 0.02387 0.02448 = 0.02520 0.00155 -0.00932 0.00493 AFIX 147 H1 2 1.422719 0.766384 0.659020 11.00000 -1.50000 AFIX 0 O1B 3 1.219818 0.963899 0.631981 11.00000 0.02132 0.01997 = 0.02322 0.00050 -0.00137 0.00146 O2 3 0.766473 0.879608 0.532927 11.00000 0.01833 0.01854 = 0.02730 0.00179 -0.00203 0.00461 AFIX 147 H2O 2 0.856803 0.963377 0.545864 11.00000 -1.50000 AFIX 0 O3 3 1.248714 0.826620 0.457734 11.00000 0.01424 0.02353 = 0.02269 0.00679 0.00029 -0.00109 AFIX 147 H3O 2 1.405270 0.838878 0.481964 11.00000 -1.50000 AFIX 0 O4A 3 0.644434 0.564835 0.440346 11.00000 0.01998 0.01954 = 0.01966 0.00092 -0.00154 -0.00238 AFIX 147 H4 2 0.536617 0.523229 0.404312 11.00000 -1.50000 AFIX 0 O4B 3 0.840706 0.691942 0.362262 11.00000 0.02105 0.02255 = 0.01707 0.00454 0.00209 0.00157 MOLE 2 C21 1 0.696827 -0.028957 0.920828 11.00000 0.05574 0.03445 = 0.03067 0.01138 0.00630 0.00816 AFIX 137 H21A 2 0.626929 0.051120 0.948821 11.00000 -1.50000 H21B 2 0.817273 -0.073897 0.952200 11.00000 -1.50000 H21C 2 0.538917 -0.101502 0.897713 11.00000 -1.50000 AFIX 0 C22 1 0.862959 0.028926 0.864734 11.00000 0.03444 0.02474 = 0.02483 0.00305 -0.00036 0.00051 AFIX 23 H22A 2 1.009058 0.109842 0.887923 11.00000 -1.20000 H22B 2 0.957275 -0.048848 0.841632 11.00000 -1.20000 AFIX 0 C23 1 0.681009 0.082215 0.808558 11.00000 0.02482 0.02126 = 0.02424 0.00228 0.00407 0.00122 AFIX 23 H23A 2 0.530621 0.002478 0.786458 11.00000 -1.20000 H23B 2 0.592511 0.162771 0.831253 11.00000 -1.20000 AFIX 0 C24 1 0.847133 0.133832 0.752032 11.00000 0.01980 0.02533 = 0.02466 0.00522 0.00185 0.00345 AFIX 23 H24A 2 1.000383 0.211856 0.774346 11.00000 -1.20000 H24B 2 0.931980 0.052569 0.728629 11.00000 -1.20000 AFIX 0 N25 4 0.670893 0.189723 0.697468 11.00000 0.02118 0.02661 = 0.02431 0.00524 0.00394 0.00035 AFIX 137 H25B 2 0.772280 0.208916 0.661233 11.00000 -1.50000 H25C 2 0.613696 0.272588 0.717524 11.00000 -1.50000 H25A 2 0.519119 0.121784 0.680339 11.00000 -1.50000 AFIX 0 MOLE 3 C31 1 1.211592 0.365926 0.286689 11.00000 0.01343 0.02468 = 0.02143 0.00572 -0.00070 0.00030 C32 1 1.008649 0.380818 0.223796 11.00000 0.01643 0.01996 = 0.01947 0.00201 -0.00057 0.00384 AFIX 13 H32 2 0.882031 0.286433 0.207858 11.00000 -1.20000 AFIX 0 C33 1 1.171345 0.420190 0.162602 11.00000 0.01710 0.01692 = 0.02072 0.00043 0.00084 0.00295 AFIX 13 H33 2 1.270962 0.338205 0.145363 11.00000 -1.20000 AFIX 0 C34 1 0.969264 0.446260 0.102445 11.00000 0.02100 0.02659 = 0.01923 0.00127 0.00441 0.00428 O31A 3 1.317939 0.250546 0.280562 11.00000 0.02517 0.02263 = 0.02517 0.00351 -0.00627 0.00648 O31B 3 1.258616 0.468485 0.337352 11.00000 0.02035 0.02253 = 0.01909 0.00045 -0.00400 0.00284 O32 3 0.846351 0.491341 0.242189 11.00000 0.02188 0.02757 = 0.01782 -0.00014 -0.00088 0.00946 AFIX 147 H32O 2 0.891753 0.528455 0.284960 11.00000 -1.50000 AFIX 0 O33 3 1.367274 0.548344 0.183221 11.00000 0.01525 0.02427 = 0.02856 0.00423 -0.00202 0.00216 AFIX 147 H33O 2 1.521841 0.526756 0.197802 11.00000 -1.50000 AFIX 0 O34A 3 0.981582 0.559965 0.079482 11.00000 0.02681 0.02639 = 0.02318 0.00843 -0.00018 0.00379 O34B 3 0.781948 0.330901 0.079756 11.00000 0.02840 0.03053 = 0.02559 0.00771 -0.01017 -0.00337 AFIX 147 H34 2 0.683859 0.344475 0.043588 11.00000 -1.50000 AFIX 0 MOLE 4 O1W 3 0.496927 0.328406 0.961336 11.00000 0.02378 0.02867 = 0.02565 0.00667 -0.00116 0.00427 H1W 2 0.355427 0.365644 0.954681 11.00000 0.05325 H2W 2 0.611050 0.358668 0.932855 11.00000 0.07643 HKLF 4 Covalent radii and connectivity table for 04mbh0606 in P-1 C 0.770 H 0.320 O 0.660 N 0.700 C1 - O1B O1A C2 C2 - O2 C1 C3 C3 - O3 C4 C2 C4 - O4B O4A C3 O1A - C1 O1B - C1 O2 - C2 O3 - C3 O4A - C4 O4B - C4 C21 - C22 C22 - C23 C21 C23 - C24 C22 C24 - N25 C23 N25 - C24 C31 - O31B O31A C32 C32 - O32 C31 C33 C33 - O33 C34 C32 C34 - O34A O34B C33 O31A - C31 O31B - C31 O32 - C32 O33 - C33 O34A - C34 O34B - C34 O1W - no bonds found Operators for generating equivalent atoms: $1 -x+3, -y+1, -z+1 $2 -x+2, -y+2, -z+1 $3 x+1, y, z $4 x-1, y, z $5 -x+2, -y+1, -z+1 $6 x-1, y-1, z $7 x, y, z-1 $8 -x+1, -y+1, -z+1 15112 Reflections read, of which 49 rejected -5 =< h =< 6, -12 =< k =< 12, -24 =< l =< 24, Max. 2-theta = 54.96 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 4 -3 4 54.01 3.04 6 19.59 -4 3 6 18.75 10.99 2 55.31 5 -4 7 116.75 9.62 3 55.79 -4 6 7 54.40 17.28 2 115.50 4 Inconsistent equivalents 3899 Unique reflections, of which 0 suppressed R(int) = 0.0922 R(sigma) = 0.1090 Friedel opposites merged Maximum memory for data reduction = 3093 / 39168 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 = 3807 / 312921 wR2 = 0.1354 before cycle 1 for 3899 data and 252 / 252 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 0.019 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.021; Restrained GooF = 1.021 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0546 * P )^2 + 0.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.90505 0.00203 0.058 OSF Mean shift/esd = 0.010 Maximum = 0.058 for OSF Max. shift = 0.001 A for H2W Max. dU = 0.000 for O34B Least-squares cycle 2 Maximum vector length = 511 Memory required = 3807 / 312921 wR2 = 0.1354 before cycle 2 for 3899 data and 252 / 252 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 0.019 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.021; Restrained GooF = 1.020 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0546 * P )^2 + 0.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.90510 0.00203 0.027 OSF Mean shift/esd = 0.004 Maximum = 0.027 for OSF Max. shift = 0.000 A for H21C Max. dU = 0.000 for H1W Least-squares cycle 3 Maximum vector length = 511 Memory required = 3807 / 312921 wR2 = 0.1354 before cycle 3 for 3899 data and 252 / 252 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 0.019 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.021; Restrained GooF = 1.021 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0546 * P )^2 + 0.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.90511 0.00203 0.001 OSF Mean shift/esd = 0.000 Maximum = -0.002 for tors H21A Max. shift = 0.000 A for H1 Max. dU = 0.000 for H1W Least-squares cycle 4 Maximum vector length = 511 Memory required = 3807 / 312921 wR2 = 0.1354 before cycle 4 for 3899 data and 252 / 252 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 0.019 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.021; Restrained GooF = 1.021 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0546 * P )^2 + 0.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.90511 0.00203 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for H1 Max. dU = 0.000 for H1W Largest correlation matrix elements 0.664 z H2W / x H2W 0.624 y H1W / x H1W Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.8177 0.6919 0.5628 13 1.000 0.000 C2 O2 C1 C3 H3 1.1709 0.6381 0.4924 13 1.000 0.000 C3 O3 C4 C2 H1 1.4228 0.7664 0.6590 147 0.840 0.000 O1A C1 H1 H2O 0.8568 0.9634 0.5458 147 0.840 0.000 O2 C2 H2O H3O 1.4053 0.8388 0.4819 147 0.840 0.000 O3 C3 H3O H4 0.5366 0.5232 0.4043 147 0.840 0.000 O4A C4 H4 H21A 0.6270 0.0511 0.9488 137 0.980 0.000 C21 C22 H21A H21B 0.8172 -0.0740 0.9522 137 0.980 0.000 C21 C22 H21A H21C 0.5388 -0.1014 0.8977 137 0.980 0.000 C21 C22 H21A H22A 1.0090 0.1098 0.8879 23 0.990 0.000 C22 C23 C21 H22B 0.9572 -0.0488 0.8416 23 0.990 0.000 C22 C23 C21 H23A 0.5306 0.0025 0.7865 23 0.990 0.000 C23 C24 C22 H23B 0.5925 0.1628 0.8313 23 0.990 0.000 C23 C24 C22 H24A 1.0004 0.2119 0.7743 23 0.990 0.000 C24 N25 C23 H24B 0.9320 0.0526 0.7286 23 0.990 0.000 C24 N25 C23 H25B 0.7723 0.2089 0.6612 137 0.910 0.000 N25 C24 H25B H25C 0.6137 0.2726 0.7175 137 0.910 0.000 N25 C24 H25B H25A 0.5191 0.1218 0.6803 137 0.910 0.000 N25 C24 H25B H32 0.8821 0.2864 0.2079 13 1.000 0.000 C32 O32 C31 C33 H33 1.2710 0.3382 0.1454 13 1.000 0.000 C33 O33 C34 C32 H32O 0.8916 0.5284 0.2850 147 0.840 0.000 O32 C32 H32O H33O 1.5218 0.5268 0.1978 147 0.840 0.000 O33 C33 H33O H34 0.6838 0.3445 0.0436 147 0.840 0.000 O34B C34 H34 04mbh0606 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 1.16758 0.83566 0.60799 1.00000 0.01635 0.02134 0.01701 0.00397 0.00352 0.00598 0.01774 0.00549 0.00052 0.00030 0.00014 0.00000 0.00139 0.00161 0.00144 0.00122 0.00108 0.00115 0.00059 C2 0.93783 0.77512 0.54801 1.00000 0.01695 0.01520 0.02049 0.00293 -0.00099 0.00282 0.01769 0.00523 0.00052 0.00028 0.00014 0.00000 0.00135 0.00144 0.00147 0.00117 0.00110 0.00109 0.00059 H2 0.81774 0.69188 0.56275 1.00000 0.02123 0.00000 0.00000 C3 1.06552 0.71780 0.48170 1.00000 0.01648 0.01609 0.01970 0.00464 0.00052 0.00132 0.01744 0.00506 0.00051 0.00028 0.00013 0.00000 0.00138 0.00141 0.00147 0.00117 0.00110 0.00109 0.00059 H3 1.17093 0.63808 0.49240 1.00000 0.02093 0.00000 0.00000 C4 0.83846 0.65825 0.42133 1.00000 0.01728 0.01478 0.02157 0.00185 0.00410 0.00561 0.01755 0.00533 0.00052 0.00028 0.00014 0.00000 0.00140 0.00141 0.00156 0.00120 0.00113 0.00111 0.00059 O1A 1.28964 0.73162 0.62749 1.00000 0.02388 0.02451 0.02522 0.00154 -0.00932 0.00491 0.02539 0.00374 0.00039 0.00020 0.00010 0.00000 0.00108 0.00111 0.00115 0.00089 0.00083 0.00086 0.00047 H1 1.42280 0.76639 0.65900 1.00000 0.03809 0.00000 0.00000 O1B 1.21983 0.96390 0.63198 1.00000 0.02136 0.01997 0.02324 0.00051 -0.00136 0.00146 0.02220 0.00363 0.00036 0.00020 0.00010 0.00000 0.00100 0.00113 0.00106 0.00088 0.00079 0.00082 0.00045 O2 0.76647 0.87961 0.53293 1.00000 0.01836 0.01857 0.02731 0.00179 -0.00202 0.00461 0.02170 0.00361 0.00035 0.00019 0.00010 0.00000 0.00100 0.00103 0.00112 0.00091 0.00080 0.00080 0.00045 H2O 0.85683 0.96338 0.54584 1.00000 0.03255 0.00000 0.00000 O3 1.24871 0.82662 0.45773 1.00000 0.01426 0.02356 0.02269 0.00679 0.00029 -0.00108 0.02035 0.00362 0.00035 0.00020 0.00009 0.00000 0.00095 0.00106 0.00109 0.00086 0.00078 0.00080 0.00044 H3O 1.40530 0.83885 0.48194 1.00000 0.03052 0.00000 0.00000 O4A 0.64444 0.56483 0.44035 1.00000 0.02000 0.01955 0.01968 0.00093 -0.00156 -0.00239 0.02071 0.00356 0.00037 0.00020 0.00009 0.00000 0.00100 0.00106 0.00104 0.00086 0.00079 0.00080 0.00044 H4 0.53663 0.52322 0.40431 1.00000 0.03106 0.00000 0.00000 O4B 0.84070 0.69194 0.36226 1.00000 0.02108 0.02255 0.01706 0.00456 0.00210 0.00157 0.02026 0.00354 0.00035 0.00019 0.00009 0.00000 0.00100 0.00107 0.00104 0.00084 0.00078 0.00080 0.00043 C21 0.69682 -0.02895 0.92083 1.00000 0.05574 0.03450 0.03070 0.01137 0.00628 0.00816 0.03949 0.00693 0.00072 0.00035 0.00017 0.00000 0.00219 0.00197 0.00186 0.00158 0.00162 0.00166 0.00083 H21A 0.62705 0.05114 0.94884 1.00000 0.05923 0.00000 0.00000 H21B 0.81724 -0.07395 0.95217 1.00000 0.05923 0.00000 0.00000 H21C 0.53883 -0.10144 0.89771 1.00000 0.05923 0.00000 0.00000 C22 0.86293 0.02893 0.86473 1.00000 0.03449 0.02474 0.02484 0.00307 -0.00037 0.00051 0.02872 0.00598 0.00062 0.00032 0.00015 0.00000 0.00171 0.00167 0.00165 0.00135 0.00134 0.00133 0.00070 H22A 1.00902 0.10985 0.88792 1.00000 0.03446 0.00000 0.00000 H22B 0.95725 -0.04884 0.84163 1.00000 0.03446 0.00000 0.00000 C23 0.68102 0.08221 0.80856 1.00000 0.02486 0.02128 0.02427 0.00227 0.00407 0.00124 0.02373 0.00575 0.00057 0.00031 0.00014 0.00000 0.00153 0.00155 0.00156 0.00126 0.00122 0.00120 0.00064 H23A 0.53064 0.00247 0.78646 1.00000 0.02848 0.00000 0.00000 H23B 0.59251 0.16276 0.83126 1.00000 0.02848 0.00000 0.00000 C24 0.84711 0.13384 0.75203 1.00000 0.01984 0.02532 0.02470 0.00522 0.00184 0.00344 0.02320 0.00570 0.00055 0.00031 0.00014 0.00000 0.00147 0.00163 0.00159 0.00131 0.00118 0.00120 0.00064 H24A 1.00035 0.21187 0.77435 1.00000 0.02784 0.00000 0.00000 H24B 0.93197 0.05258 0.72863 1.00000 0.02784 0.00000 0.00000 N25 0.67091 0.18972 0.69747 1.00000 0.02118 0.02662 0.02435 0.00522 0.00395 0.00034 0.02416 0.00454 0.00044 0.00025 0.00012 0.00000 0.00126 0.00138 0.00133 0.00110 0.00102 0.00103 0.00056 H25B 0.77231 0.20891 0.66124 1.00000 0.03624 0.00000 0.00000 H25C 0.61370 0.27258 0.71753 1.00000 0.03624 0.00000 0.00000 H25A 0.51914 0.12178 0.68034 1.00000 0.03624 0.00000 0.00000 C31 1.21158 0.36593 0.28669 1.00000 0.01342 0.02471 0.02145 0.00571 -0.00070 0.00030 0.02007 0.00548 0.00053 0.00030 0.00014 0.00000 0.00134 0.00162 0.00156 0.00133 0.00109 0.00116 0.00062 C32 1.00867 0.38083 0.22380 1.00000 0.01642 0.01997 0.01950 0.00201 -0.00059 0.00383 0.01880 0.00539 0.00052 0.00029 0.00014 0.00000 0.00136 0.00148 0.00147 0.00119 0.00109 0.00112 0.00060 H32 0.88206 0.28644 0.20786 1.00000 0.02255 0.00000 0.00000 C33 1.17134 0.42019 0.16261 1.00000 0.01714 0.01691 0.02076 0.00042 0.00083 0.00296 0.01856 0.00514 0.00052 0.00028 0.00014 0.00000 0.00137 0.00147 0.00150 0.00119 0.00112 0.00112 0.00060 H33 1.27096 0.33820 0.14537 1.00000 0.02227 0.00000 0.00000 C34 0.96928 0.44626 0.10245 1.00000 0.02102 0.02661 0.01923 0.00124 0.00443 0.00428 0.02232 0.00571 0.00056 0.00032 0.00015 0.00000 0.00148 0.00172 0.00152 0.00133 0.00116 0.00127 0.00064 O31A 1.31795 0.25054 0.28056 1.00000 0.02521 0.02266 0.02517 0.00352 -0.00627 0.00649 0.02465 0.00368 0.00037 0.00020 0.00010 0.00000 0.00105 0.00110 0.00110 0.00089 0.00083 0.00087 0.00046 O31B 1.25861 0.46849 0.33735 1.00000 0.02037 0.02257 0.01910 0.00045 -0.00401 0.00285 0.02138 0.00363 0.00036 0.00020 0.00010 0.00000 0.00098 0.00109 0.00101 0.00088 0.00079 0.00081 0.00044 O32 0.84635 0.49134 0.24219 1.00000 0.02193 0.02758 0.01784 -0.00013 -0.00086 0.00947 0.02245 0.00373 0.00037 0.00020 0.00010 0.00000 0.00104 0.00115 0.00101 0.00088 0.00082 0.00086 0.00045 H32O 0.89163 0.52840 0.28497 1.00000 0.03367 0.00000 0.00000 O33 1.36727 0.54835 0.18322 1.00000 0.01525 0.02430 0.02860 0.00422 -0.00203 0.00217 0.02307 0.00360 0.00035 0.00019 0.00010 0.00000 0.00097 0.00110 0.00116 0.00090 0.00082 0.00081 0.00046 H33O 1.52185 0.52676 0.19780 1.00000 0.03460 0.00000 0.00000 O34A 0.98157 0.55996 0.07948 1.00000 0.02686 0.02639 0.02319 0.00844 -0.00017 0.00379 0.02524 0.00376 0.00037 0.00021 0.00010 0.00000 0.00110 0.00118 0.00110 0.00094 0.00086 0.00088 0.00047 O34B 0.78196 0.33090 0.07975 1.00000 0.02843 0.03056 0.02564 0.00771 -0.01016 -0.00337 0.02945 0.00379 0.00040 0.00021 0.00010 0.00000 0.00114 0.00122 0.00118 0.00095 0.00087 0.00095 0.00050 H34 0.68385 0.34448 0.04359 1.00000 0.04417 0.00000 0.00000 O1W 0.49692 0.32841 0.96134 1.00000 0.02379 0.02870 0.02568 0.00668 -0.00117 0.00428 0.02603 0.00403 0.00043 0.00022 0.00011 0.00000 0.00117 0.00122 0.00121 0.00095 0.00094 0.00095 0.00048 H1W 0.35546 0.36559 0.95468 1.00000 0.05321 0.06982 0.00479 0.00362 0.00175 0.00000 0.01166 H2W 0.61111 0.35858 0.93283 1.00000 0.07643 0.08062 0.00590 0.00415 0.00180 0.00000 0.01445 Final Structure Factor Calculation for 04mbh0606 in P-1 Total number of l.s. parameters = 252 Maximum vector length = 511 Memory required = 3555 / 22995 wR2 = 0.1354 before cycle 5 for 3899 data and 0 / 252 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 0.019 0.004 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.021; Restrained GooF = 1.021 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0546 * P )^2 + 0.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0596 for 2204 Fo > 4sig(Fo) and 0.1343 for all 3899 data wR2 = 0.1354, GooF = S = 1.021, Restrained GooF = 1.021 for all data Occupancy sum of asymmetric unit = 26.00 for non-hydrogen and 25.00 for hydrogen atoms Principal mean square atomic displacements U 0.0225 0.0168 0.0139 C1 0.0227 0.0159 0.0145 C2 0.0213 0.0161 0.0148 C3 0.0222 0.0187 0.0117 C4 0.0387 0.0241 0.0134 O1A 0.0271 0.0225 0.0171 O1B 0.0305 0.0189 0.0157 O2 0.0282 0.0196 0.0133 O3 0.0265 0.0219 0.0137 O4A 0.0242 0.0202 0.0163 O4B 0.0558 0.0378 0.0249 C21 0.0376 0.0257 0.0228 C22 0.0277 0.0231 0.0205 C23 0.0264 0.0235 0.0197 C24 0.0288 0.0247 0.0189 N25 0.0272 0.0202 0.0128 C31 0.0223 0.0191 0.0149 C32 0.0228 0.0169 0.0160 C33 0.0278 0.0222 0.0170 C34 0.0358 0.0229 0.0153 O31A 0.0275 0.0226 0.0140 O31B 0.0331 0.0179 0.0164 O32 0.0305 0.0243 0.0143 O33 0.0310 0.0264 0.0183 O34A 0.0468 0.0264 0.0151 O34B 0.0309 0.0272 0.0200 O1W 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 0.033 0.045 0.058 0.073 0.094 0.124 0.177 1.000 Number in group 411. 383. 400. 382. 373. 393. 395. 392. 378. 392. GooF 0.939 0.950 0.923 1.024 1.099 1.072 1.086 1.071 1.038 0.997 K 11.142 2.942 1.054 1.007 0.952 0.998 0.962 1.012 1.011 0.993 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.63 inf Number in group 391. 391. 395. 393. 387. 386. 386. 394. 383. 393. GooF 1.005 0.985 0.951 1.039 0.999 0.992 0.975 0.968 1.006 1.252 K 1.061 1.110 1.005 0.995 1.035 0.999 1.017 1.031 1.029 0.974 R1 0.376 0.331 0.261 0.242 0.194 0.103 0.071 0.065 0.050 0.036 Recommended weighting scheme: WGHT 0.0549 0.1806 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) 2 -9 3 93.13 32.56 5.74 0.051 1.00 3 -6 19 854.75 159.28 4.45 0.113 0.78 -2 2 0 106.29 77.30 4.11 0.079 2.27 -5 -1 15 513.27 4.90 4.07 0.020 0.80 0 -3 6 22.27 41.70 3.89 0.058 2.39 2 9 3 -34.14 69.62 3.88 0.075 0.86 -5 -2 14 532.03 4.08 3.86 0.018 0.81 -5 2 10 56.77 115.41 3.84 0.096 0.89 -3 -6 3 104.52 52.30 3.75 0.065 1.05 0 -1 4 66.88 36.84 3.62 0.054 4.48 -1 -6 6 31.55 0.07 3.47 0.002 1.37 0 -1 3 70.37 43.47 3.45 0.059 5.61 3 1 3 27.35 9.44 3.42 0.028 1.45 -1 -1 7 161.03 125.17 3.38 0.100 2.42 1 -1 3 190.59 239.45 3.35 0.138 3.63 0 -1 5 216.43 270.85 3.33 0.147 3.69 0 2 5 21.42 2.24 3.26 0.013 2.71 0 -1 6 155.32 197.68 3.22 0.126 3.12 2 2 6 19.68 0.02 3.21 0.001 1.58 1 -3 3 24.40 38.50 3.12 0.056 2.62 5 -2 3 310.16 197.96 3.08 0.126 0.95 -2 0 2 276.00 224.52 3.07 0.134 2.38 3 -1 6 19.43 4.52 3.04 0.019 1.39 4 3 2 187.06 244.28 3.00 0.140 1.04 -1 4 11 15.19 31.51 2.94 0.050 1.29 0 1 9 39.96 24.97 2.90 0.045 1.97 -5 0 9 97.24 146.46 2.87 0.108 0.91 0 4 4 438.12 362.49 2.87 0.170 1.95 0 7 13 12.06 52.17 2.87 0.065 0.91 -1 -9 5 71.03 22.11 2.86 0.042 0.98 -4 7 3 8.94 29.98 2.86 0.049 0.95 4 -3 7 38.05 69.08 2.85 0.074 1.06 -2 -8 8 204.71 138.69 2.85 0.105 0.97 5 0 8 49.17 89.76 2.83 0.085 0.85 3 -4 20 53.83 120.51 2.82 0.098 0.78 4 7 4 -21.71 18.78 2.82 0.039 0.79 -3 10 8 -25.30 45.13 2.81 0.060 0.78 1 -7 18 61.72 115.84 2.81 0.096 0.88 -4 1 2 166.90 106.74 2.78 0.092 1.22 -2 -1 20 29.53 76.80 2.78 0.078 0.91 -1 -7 1 105.89 72.99 2.74 0.076 1.23 4 2 8 91.71 59.32 2.73 0.069 0.96 2 -4 21 102.48 40.87 2.73 0.057 0.82 -1 3 4 9.86 2.24 2.70 0.013 2.32 -5 7 2 1.81 61.75 2.70 0.070 0.83 0 -6 16 1.03 28.87 2.69 0.048 1.01 -1 -4 6 499.06 420.17 2.68 0.183 1.81 0 7 14 56.46 0.36 2.65 0.005 0.87 0 -3 2 304.00 366.37 2.65 0.171 3.06 0 2 6 475.72 562.39 2.64 0.212 2.42 Bond lengths and angles C1 - Distance Angles O1B 1.2126 (0.0031) O1A 1.2948 (0.0030) 127.63 (0.25) C2 1.5165 (0.0038) 122.44 (0.23) 109.92 (0.23) C1 - O1B O1A C2 - Distance Angles O2 1.4183 (0.0029) C1 1.5165 (0.0038) 112.15 (0.21) C3 1.5251 (0.0036) 110.42 (0.21) 109.74 (0.20) H2 1.0000 108.14 108.14 108.14 C2 - O2 C1 C3 C3 - Distance Angles O3 1.4166 (0.0030) C4 1.5115 (0.0038) 106.98 (0.21) C2 1.5251 (0.0036) 112.76 (0.21) 110.21 (0.20) H3 1.0000 108.94 108.94 108.94 C3 - O3 C4 C2 C4 - Distance Angles O4B 1.2166 (0.0030) O4A 1.3108 (0.0031) 124.79 (0.25) C3 1.5115 (0.0038) 123.54 (0.24) 111.66 (0.22) C4 - O4B O4A O1A - Distance Angles C1 1.2948 (0.0031) H1 0.8400 109.47 O1A - C1 O1B - Distance Angles C1 1.2126 (0.0031) O1B - O2 - Distance Angles C2 1.4183 (0.0029) H2O 0.8400 109.47 O2 - C2 O3 - Distance Angles C3 1.4166 (0.0030) H3O 0.8400 109.47 O3 - C3 O4A - Distance Angles C4 1.3108 (0.0032) H4 0.8400 109.47 O4A - C4 O4B - Distance Angles C4 1.2166 (0.0030) O4B - C21 - Distance Angles C22 1.5163 (0.0041) H21A 0.9800 109.47 H21B 0.9800 109.47 109.47 H21C 0.9800 109.47 109.47 109.47 C21 - C22 H21A H21B C22 - Distance Angles C23 1.5150 (0.0039) C21 1.5163 (0.0041) 112.35 (0.25) H22A 0.9900 109.13 109.13 H22B 0.9900 109.13 109.13 107.86 C22 - C23 C21 H22A C23 - Distance Angles C24 1.5014 (0.0038) C22 1.5150 (0.0039) 111.58 (0.23) H23A 0.9900 109.31 109.31 H23B 0.9900 109.31 109.31 107.96 C23 - C24 C22 H23A C24 - Distance Angles N25 1.4905 (0.0034) C23 1.5014 (0.0038) 111.91 (0.22) H24A 0.9900 109.23 109.23 H24B 0.9900 109.23 109.23 107.92 C24 - N25 C23 H24A N25 - Distance Angles C24 1.4905 (0.0034) H25B 0.9100 109.47 H25C 0.9100 109.47 109.47 H25A 0.9100 109.47 109.47 109.47 N25 - C24 H25B H25C C31 - Distance Angles O31B 1.2483 (0.0032) O31A 1.2621 (0.0032) 127.39 (0.25) C32 1.5216 (0.0037) 117.36 (0.23) 115.23 (0.24) C31 - O31B O31A C32 - Distance Angles O32 1.4158 (0.0030) C31 1.5216 (0.0037) 111.13 (0.21) C33 1.5298 (0.0037) 108.25 (0.21) 109.64 (0.21) H32 1.0000 109.26 109.26 109.26 C32 - O32 C31 C33 C33 - Distance Angles O33 1.4139 (0.0031) C34 1.5151 (0.0038) 107.58 (0.22) C32 1.5298 (0.0037) 111.97 (0.21) 109.22 (0.21) H33 1.0000 109.34 109.34 109.34 C33 - O33 C34 C32 C34 - Distance Angles O34A 1.2094 (0.0033) O34B 1.3114 (0.0034) 125.34 (0.26) C33 1.5151 (0.0038) 123.48 (0.26) 111.18 (0.24) C34 - O34A O34B O31A - Distance Angles C31 1.2621 (0.0032) O31A - O31B - Distance Angles C31 1.2483 (0.0032) O31B - O32 - Distance Angles C32 1.4158 (0.0030) H32O 0.8400 109.47 O32 - C32 O33 - Distance Angles C33 1.4139 (0.0031) H33O 0.8400 109.47 O33 - C33 O34A - Distance Angles C34 1.2094 (0.0033) O34A - O34B - Distance Angles C34 1.3114 (0.0034) H34 0.8400 109.47 O34B - C34 O1W - Distance Angles H1W 0.8224 (0.0173) H2W 0.8607 (0.0177) 107.12 (2.45) O1W - H1W Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 2.30 2.725(3) 111.4 O2-H2O...O1B 0.84 2.04 2.764(3) 144.7 O32-H32O...O4B 0.84 2.15 2.638(3) 116.7 O32-H32O...O31B 0.84 1.67 2.448(3) 152.2 O1A-H1...O31A_$1 0.84 2.12 2.758(3) 132.6 O2-H2O...O3_$2 0.84 1.89 2.732(3) 175.4 O3-H3O...O2_$3 0.84 1.82 2.654(3) 171.6 O33-H33O...O32_$3 0.84 1.75 2.567(3) 165.4 O4A-H4...O31B_$4 0.91 2.10 2.881(3) 143.6 N25-H25B...O4B_$5 0.91 2.24 3.014(3) 142.1 N25-H25B...O3_$5 0.91 2.34 3.152(3) 148.5 N25-H25C...O33_$5 0.861(18) 2.07(2) 2.828(3) 147(3) O1W-H2W...O34A_$5 0.861(18) 2.50(3) 3.233(3) 143(3) O1W-H2W...O33_$5 0.91 1.99 2.892(3) 171.8 N25-H25A...O1B_$6 0.84 1.72 2.543(3) 165.4 O34B-H34...O1W_$7 0.822(17) 1.966(19) 2.779(3) 170(3) O1W-H1W...O34A_$8 FMAP and GRID set by program FMAP 2 1 24 GRID -4.762 -2 -1 4.762 2 1 R1 = 0.1342 for 3899 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.32 at 0.5374 0.2902 0.2298 [ 1.55 A from O31A ] Deepest hole -0.40 at 0.6003 0.1834 0.3489 [ 0.54 A from H1 ] Mean = 0.00, Rms deviation from mean = 0.07 e/A^3, Highest memory used = 3740 / 31332 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 1.5374 0.2902 0.2298 1.00000 0.05 0.32 1.55 O31A 1.77 H32 2.12 H33 2.15 C31 Q2 1 1.0645 0.1505 0.3107 1.00000 0.05 0.26 1.64 O31A 1.96 H24B 2.00 C1 2.11 O1B Q3 1 0.6305 0.4803 0.3166 1.00000 0.05 0.26 1.50 H32O 1.78 H4 1.85 O32 1.88 O31B Q4 1 1.0182 0.2001 0.2698 1.00000 0.05 0.25 1.46 O31A 1.67 H32 1.68 C31 2.03 C32 Q5 1 1.5221 0.7962 0.4494 1.00000 0.05 0.25 0.96 H3O 1.42 O3 1.91 O2 2.20 C4 Q6 1 1.2471 0.7723 0.4068 1.00000 0.05 0.25 1.03 O3 1.33 H25B 1.57 H3O 1.85 C3 Q7 1 1.1354 -0.1374 0.8473 1.00000 0.05 0.25 1.29 H22B 1.62 H32 2.07 H21C 2.20 C22 Q8 1 1.3920 0.6713 0.2073 1.00000 0.05 0.24 1.17 O33 1.46 H25C 1.57 H33O 1.82 H23B Q9 1 1.1429 0.1355 0.2361 1.00000 0.05 0.24 1.41 O31A 1.59 H22B 1.98 H24B 2.13 H32 Q10 1 0.8075 0.2174 0.2564 1.00000 0.05 0.24 1.26 H32 1.92 C32 2.05 H1 2.23 C31 Shortest distances between peaks (including symmetry equivalents) 2 4 0.99 4 10 1.07 4 9 1.10 5 6 1.47 2 9 1.50 1 10 1.64 2 10 1.79 9 10 1.95 7 9 2.00 7 10 2.08 1 3 2.23 4 7 2.26 1 9 2.27 1 4 2.68 1 7 2.69 3 10 2.86 Time profile in seconds ----------------------- 0.11: Read and process instructions 0.00: Fit rigid groups 0.02: Interpret restraints etc. 0.00: Generate connectivity array 0.00: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.00: Analyse other restraints etc. 0.73: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.75: Structure factors and derivatives 1.58: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.20: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.08: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 04mbh0606 finished at 12:57:49 Total CPU time: 3.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++