+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 04mbh0608 started at 17:52:57 on 05-Sep-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 04mbh0608 in P-1 CELL 0.71073 6.1179 8.6720 15.1817 90.918 91.411 99.792 ZERR 2.00 0.0014 0.0024 0.0075 0.033 0.027 0.023 LATT 1 SFAC C H O N UNIT 20 56 18 4 V = 793.31 F(000) = 348.0 Mu = 0.12 mm-1 Cell Wt = 640.69 Rho = 1.341 MERG 2 OMIT -3.00 55.00 DFIX 0.84 0.02 O1W H1W O1W H2W O2W H21W O2W H22W O3W H31W O3W H32W DANG 1.35 0.02 H1W H2W H21W H22W H31W H32W SHEL 7 0.77 HTAB O2 O1A HTAB O3 O4A HTAB N25 O4B HTAB N25 O4A HTAB O1W O1B HTAB O1W O2W HTAB O2W O4B EQIV_$1 -x+1, -y, -z+1 HTAB O2 O1A_$1 EQIV_$2 x-1, y, z HTAB O3 O1B_$2 EQIV_$3 x-1, y+1, z HTAB N22 O1B_$3 HTAB N22 O1A_$3 HTAB O3W O1W_$3 EQIV_$4 -x, -y+1, -z+2 HTAB O2W O3W_$4 EQIV_$5 -x+1, -y+1, -z+2 HTAB O3W O1W_$5 FMAP 2 PLAN 10 SIZE 0.10 0.20 0.70 ACTA BOND $H WGHT 0.04790 0.38130 L.S. 4 TEMP -153.00 FVAR 1.11627 MOLE 1 C1 1 0.647531 0.019114 0.654165 11.00000 0.01576 0.01665 = 0.05229 0.00835 0.01529 0.00512 C2 1 0.568411 0.176225 0.661383 11.00000 0.01453 0.01515 = 0.02545 0.00282 0.00185 0.00349 AFIX 13 H2 2 0.693013 0.255453 0.686714 11.00000 -1.20000 AFIX 0 C3 1 0.374538 0.162916 0.723690 11.00000 0.01499 0.01364 = 0.02371 0.00225 0.00035 0.00197 AFIX 13 H3 2 0.427724 0.134834 0.783166 11.00000 -1.20000 AFIX 0 C4 1 0.289054 0.317593 0.732684 11.00000 0.01588 0.01554 = 0.01805 0.00181 0.00252 0.00309 O1A 3 0.618312 -0.053691 0.582394 11.00000 0.05915 0.02244 = 0.05761 -0.00616 0.02779 0.01339 O1B 3 0.740434 -0.028136 0.721030 11.00000 0.02173 0.02388 = 0.06975 0.01827 0.00434 0.00967 O2 3 0.506672 0.227127 0.577852 11.00000 0.03065 0.01730 = 0.02437 0.00096 0.00464 0.00657 AFIX 147 H2O 2 0.487434 0.151191 0.541824 11.00000 -1.50000 AFIX 0 O3 3 0.205188 0.041554 0.693370 11.00000 0.01410 0.01411 = 0.04248 -0.00285 0.00204 0.00134 AFIX 147 H3O 2 0.081280 0.069367 0.699241 11.00000 -1.50000 AFIX 0 O4A 3 0.095699 0.322234 0.710513 11.00000 0.01740 0.01898 = 0.03952 -0.00217 -0.00293 0.00619 O4B 3 0.427121 0.432861 0.766155 11.00000 0.01947 0.01534 = 0.02254 -0.00049 -0.00040 0.00192 MOLE 2 C21 1 0.014382 0.784393 0.523022 11.00000 0.02474 0.03117 = 0.02808 0.01330 0.00210 0.00530 AFIX 137 H21A 2 0.087095 0.702866 0.497008 11.00000 -1.50000 H21B 2 0.124658 0.878818 0.535080 11.00000 -1.50000 H21C 2 -0.100229 0.808734 0.481823 11.00000 -1.50000 AFIX 0 C23 1 0.083490 0.685858 0.668574 11.00000 0.01709 0.01680 = 0.02089 0.00199 0.00201 0.00645 AFIX 23 H23A 2 0.213221 0.771500 0.671208 11.00000 -1.20000 H23B 2 0.133544 0.590042 0.646408 11.00000 -1.20000 AFIX 0 C24 1 -0.005707 0.658221 0.759961 11.00000 0.01898 0.01954 = 0.02247 0.00073 0.00439 0.00590 AFIX 23 H24A 2 -0.069320 0.749963 0.779970 11.00000 -1.20000 H24B 2 -0.125344 0.565596 0.758628 11.00000 -1.20000 AFIX 0 C26 1 0.079599 0.550484 0.901796 11.00000 0.02868 0.03196 = 0.01976 0.00577 0.00687 0.00037 AFIX 137 H26A 2 0.199486 0.539207 0.943952 11.00000 -1.50000 H26B 2 -0.001496 0.446704 0.884332 11.00000 -1.50000 H26C 2 -0.022130 0.611601 0.929292 11.00000 -1.50000 AFIX 0 C27 1 -0.276791 0.596220 0.590385 11.00000 0.02370 0.02601 = 0.03438 0.00930 -0.00567 -0.00418 AFIX 137 H27A 2 -0.219246 0.503908 0.569305 11.00000 -1.50000 H27B 2 -0.379521 0.626161 0.545818 11.00000 -1.50000 H27C 2 -0.355128 0.571820 0.645301 11.00000 -1.50000 AFIX 0 C28 1 0.327220 0.779086 0.848696 11.00000 0.03208 0.02006 = 0.02802 -0.00281 -0.00080 -0.00300 AFIX 137 H28A 2 0.392448 0.829621 0.795936 11.00000 -1.50000 H28B 2 0.445566 0.754634 0.888010 11.00000 -1.50000 H28C 2 0.244052 0.849861 0.879315 11.00000 -1.50000 AFIX 0 N22 4 -0.089317 0.727914 0.606670 11.00000 0.01791 0.01425 = 0.02580 0.00555 0.00256 0.00481 AFIX 13 H22 2 -0.146293 0.810170 0.632369 11.00000 0.03718 AFIX 0 N25 4 0.175024 0.632269 0.822668 11.00000 0.01979 0.01590 = 0.01800 0.00036 0.00319 0.00170 AFIX 13 H25 2 0.258500 0.566935 0.794593 11.00000 0.03204 AFIX 0 MOLE 3 O1W 3 0.820400 0.083763 0.891582 11.00000 0.03084 0.04414 = 0.04643 0.01948 -0.00798 0.00748 H1W 2 0.785189 0.054303 0.837190 11.00000 0.09627 H2W 2 0.742699 0.153769 0.901175 11.00000 0.07655 MOLE 4 O2W 3 0.588224 0.323117 0.924463 11.00000 0.02837 0.04217 = 0.02867 0.00927 -0.00698 -0.00223 H21W 2 0.465106 0.280011 0.944941 11.00000 0.06701 H22W 2 0.551213 0.362661 0.876216 11.00000 0.05150 MOLE 5 O3W 3 -0.205724 0.829648 1.004074 11.00000 0.03166 0.03714 = 0.04692 0.01626 -0.00728 -0.00191 H31W 2 -0.202663 0.910316 0.972305 11.00000 0.06428 H32W 2 -0.094907 0.856225 1.040637 11.00000 0.06275 HKLF 4 Covalent radii and connectivity table for 04mbh0608 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 C2 C4 C4 - O4A O4B C3 O1A - C1 O1B - C1 O2 - C2 O3 - C3 O4A - C4 O4B - C4 C21 - N22 C23 - N22 C24 C24 - N25 C23 C26 - N25 C27 - N22 C28 - N25 N22 - C21 C27 C23 N25 - C28 C26 C24 O1W - no bonds found O2W - no bonds found O3W - no bonds found Operators for generating equivalent atoms: $1 -x+1, -y, -z+1 $2 x-1, y, z $3 x-1, y+1, z $4 -x, -y+1, -z+2 $5 -x+1, -y+1, -z+2 12979 Reflections read, of which 17 rejected -7 =< h =< 7, -11 =< k =< 11, -19 =< l =< 19, 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) 5 5 5 4.01 1.66 2 8.79 6 -3 6 188.77 5.17 2 26.23 2 Inconsistent equivalents 3575 Unique reflections, of which 0 suppressed R(int) = 0.0349 R(sigma) = 0.0366 Friedel opposites merged Maximum memory for data reduction = 2834 / 35358 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 = 3476 / 275076 wR2 = 0.1122 before cycle 1 for 3575 data and 222 / 222 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 6. 3. 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 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.032; Restrained GooF = 1.031 for 9 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0479 * P )^2 + 0.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.11627 0.00216 0.000 OSF Mean shift/esd = 0.002 Maximum = 0.008 for U12 O3 Max. shift = 0.000 A for H21B Max. dU = 0.000 for O2W Least-squares cycle 2 Maximum vector length = 511 Memory required = 3476 / 275076 wR2 = 0.1122 before cycle 2 for 3575 data and 222 / 222 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 6. 3. 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 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.032; Restrained GooF = 1.031 for 9 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0479 * P )^2 + 0.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.11628 0.00216 0.002 OSF Mean shift/esd = 0.001 Maximum = 0.003 for U12 O3 Max. shift = 0.000 A for H32W Max. dU = 0.000 for H1W Least-squares cycle 3 Maximum vector length = 511 Memory required = 3476 / 275076 wR2 = 0.1122 before cycle 3 for 3575 data and 222 / 222 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 6. 3. 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 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.032; Restrained GooF = 1.031 for 9 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0479 * P )^2 + 0.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.11627 0.00216 -0.001 OSF Mean shift/esd = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for H31W Max. dU = 0.000 for H31W Least-squares cycle 4 Maximum vector length = 511 Memory required = 3476 / 275076 wR2 = 0.1122 before cycle 4 for 3575 data and 222 / 222 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 6. 3. 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 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.032; Restrained GooF = 1.031 for 9 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0479 * P )^2 + 0.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.11627 0.00216 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z N25 Max. shift = 0.000 A for H1W Max. dU = 0.000 for H1W Largest correlation matrix elements 0.579 y H2W / x H2W Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.6930 0.2555 0.6867 13 1.000 0.000 C2 O2 C1 C3 H3 0.4277 0.1348 0.7832 13 1.000 0.000 C3 O3 C2 C4 H2O 0.4874 0.1512 0.5418 147 0.840 0.000 O2 C2 H2O H3O 0.0813 0.0694 0.6992 147 0.840 0.000 O3 C3 H3O H21A 0.0871 0.7029 0.4970 137 0.980 0.000 C21 N22 H21A H21B 0.1247 0.8788 0.5351 137 0.980 0.000 C21 N22 H21A H21C -0.1002 0.8087 0.4818 137 0.980 0.000 C21 N22 H21A H23A 0.2132 0.7715 0.6712 23 0.990 0.000 C23 N22 C24 H23B 0.1335 0.5900 0.6464 23 0.990 0.000 C23 N22 C24 H24A -0.0693 0.7500 0.7800 23 0.990 0.000 C24 N25 C23 H24B -0.1253 0.5656 0.7586 23 0.990 0.000 C24 N25 C23 H26A 0.1995 0.5392 0.9440 137 0.980 0.000 C26 N25 H26A H26B -0.0015 0.4467 0.8843 137 0.980 0.000 C26 N25 H26A H26C -0.0221 0.6116 0.9293 137 0.980 0.000 C26 N25 H26A H27A -0.2192 0.5039 0.5693 137 0.980 0.000 C27 N22 H27A H27B -0.3795 0.6262 0.5458 137 0.980 0.000 C27 N22 H27A H27C -0.3551 0.5718 0.6453 137 0.980 0.000 C27 N22 H27A H28A 0.3924 0.8296 0.7959 137 0.980 0.000 C28 N25 H28A H28B 0.4456 0.7546 0.8880 137 0.980 0.000 C28 N25 H28A H28C 0.2441 0.8499 0.8793 137 0.980 0.000 C28 N25 H28A H22 -0.1463 0.8102 0.6324 13 0.930 0.000 N22 C21 C27 C23 H25 0.2585 0.5669 0.7946 13 0.930 0.000 N25 C28 C26 C24 04mbh0608 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.64753 0.01911 0.65416 1.00000 0.01576 0.01665 0.05229 0.00835 0.01529 0.00512 0.02764 0.00345 0.00026 0.00019 0.00013 0.00000 0.00077 0.00078 0.00116 0.00077 0.00072 0.00059 0.00040 C2 0.56841 0.17622 0.66138 1.00000 0.01453 0.01515 0.02545 0.00282 0.00185 0.00349 0.01822 0.00283 0.00024 0.00017 0.00010 0.00000 0.00070 0.00072 0.00081 0.00059 0.00057 0.00054 0.00032 H2 0.69301 0.25545 0.68671 1.00000 0.02186 0.00000 0.00000 C3 0.37454 0.16292 0.72369 1.00000 0.01499 0.01364 0.02371 0.00225 0.00035 0.00197 0.01748 0.00270 0.00023 0.00017 0.00010 0.00000 0.00071 0.00071 0.00080 0.00058 0.00056 0.00053 0.00031 H3 0.42772 0.13483 0.78317 1.00000 0.02098 0.00000 0.00000 C4 0.28905 0.31759 0.73268 1.00000 0.01588 0.01554 0.01805 0.00181 0.00252 0.00309 0.01639 0.00270 0.00023 0.00017 0.00010 0.00000 0.00073 0.00072 0.00074 0.00056 0.00055 0.00054 0.00030 O1A 0.61831 -0.05369 0.58239 1.00000 0.05915 0.02244 0.05761 -0.00616 0.02779 0.01339 0.04529 0.00287 0.00025 0.00015 0.00010 0.00000 0.00093 0.00067 0.00096 0.00064 0.00073 0.00061 0.00039 O1B 0.74043 -0.02814 0.72103 1.00000 0.02173 0.02388 0.06975 0.01827 0.00434 0.00967 0.03754 0.00260 0.00020 0.00014 0.00010 0.00000 0.00063 0.00065 0.00098 0.00062 0.00059 0.00049 0.00034 O2 0.50667 0.22713 0.57785 1.00000 0.03065 0.01730 0.02437 0.00096 0.00464 0.00657 0.02375 0.00213 0.00019 0.00013 0.00007 0.00000 0.00063 0.00056 0.00060 0.00045 0.00046 0.00045 0.00026 H2O 0.48743 0.15119 0.54182 1.00000 0.03562 0.00000 0.00000 O3 0.20519 0.04155 0.69337 1.00000 0.01410 0.01411 0.04248 -0.00285 0.00204 0.00134 0.02370 0.00197 0.00017 0.00012 0.00008 0.00000 0.00053 0.00054 0.00071 0.00047 0.00047 0.00040 0.00027 H3O 0.08128 0.06937 0.69924 1.00000 0.03556 0.00000 0.00000 O4A 0.09570 0.32223 0.71051 1.00000 0.01740 0.01898 0.03952 -0.00217 -0.00293 0.00619 0.02503 0.00202 0.00017 0.00013 0.00008 0.00000 0.00058 0.00057 0.00070 0.00049 0.00046 0.00043 0.00027 O4B 0.42712 0.43286 0.76616 1.00000 0.01947 0.01534 0.02254 -0.00049 -0.00040 0.00192 0.01926 0.00187 0.00017 0.00012 0.00007 0.00000 0.00054 0.00053 0.00057 0.00042 0.00041 0.00040 0.00024 C21 0.01438 0.78439 0.52302 1.00000 0.02474 0.03117 0.02808 0.01330 0.00210 0.00530 0.02777 0.00340 0.00028 0.00021 0.00011 0.00000 0.00086 0.00093 0.00091 0.00072 0.00066 0.00068 0.00038 H21A 0.08709 0.70287 0.49701 1.00000 0.04166 0.00000 0.00000 H21B 0.12466 0.87882 0.53508 1.00000 0.04166 0.00000 0.00000 H21C -0.10023 0.80873 0.48182 1.00000 0.04166 0.00000 0.00000 C23 0.08349 0.68586 0.66857 1.00000 0.01709 0.01680 0.02089 0.00199 0.00201 0.00645 0.01780 0.00282 0.00024 0.00017 0.00010 0.00000 0.00072 0.00073 0.00078 0.00058 0.00056 0.00055 0.00031 H23A 0.21322 0.77150 0.67121 1.00000 0.02136 0.00000 0.00000 H23B 0.13354 0.59004 0.64641 1.00000 0.02136 0.00000 0.00000 C24 -0.00571 0.65822 0.75996 1.00000 0.01898 0.01954 0.02247 0.00073 0.00439 0.00590 0.01996 0.00292 0.00025 0.00018 0.00010 0.00000 0.00075 0.00076 0.00081 0.00061 0.00059 0.00058 0.00033 H24A -0.06932 0.74996 0.77997 1.00000 0.02395 0.00000 0.00000 H24B -0.12534 0.56560 0.75863 1.00000 0.02395 0.00000 0.00000 C26 0.07960 0.55048 0.90180 1.00000 0.02868 0.03196 0.01976 0.00577 0.00687 0.00037 0.02720 0.00326 0.00028 0.00021 0.00011 0.00000 0.00089 0.00093 0.00083 0.00069 0.00065 0.00069 0.00037 H26A 0.19949 0.53921 0.94395 1.00000 0.04081 0.00000 0.00000 H26B -0.00150 0.44670 0.88433 1.00000 0.04081 0.00000 0.00000 H26C -0.02213 0.61160 0.92929 1.00000 0.04081 0.00000 0.00000 C27 -0.27679 0.59622 0.59038 1.00000 0.02370 0.02601 0.03438 0.00930 -0.00567 -0.00418 0.02903 0.00309 0.00028 0.00020 0.00012 0.00000 0.00086 0.00090 0.00098 0.00073 0.00069 0.00066 0.00039 H27A -0.21925 0.50391 0.56931 1.00000 0.04354 0.00000 0.00000 H27B -0.37952 0.62616 0.54582 1.00000 0.04354 0.00000 0.00000 H27C -0.35513 0.57182 0.64530 1.00000 0.04354 0.00000 0.00000 C28 0.32722 0.77909 0.84870 1.00000 0.03208 0.02006 0.02802 -0.00281 -0.00080 -0.00300 0.02765 0.00294 0.00029 0.00019 0.00012 0.00000 0.00092 0.00082 0.00091 0.00067 0.00069 0.00066 0.00037 H28A 0.39245 0.82962 0.79594 1.00000 0.04148 0.00000 0.00000 H28B 0.44557 0.75463 0.88801 1.00000 0.04148 0.00000 0.00000 H28C 0.24405 0.84986 0.87931 1.00000 0.04148 0.00000 0.00000 N22 -0.08932 0.72791 0.60667 1.00000 0.01791 0.01425 0.02580 0.00555 0.00256 0.00481 0.01899 0.00239 0.00020 0.00014 0.00009 0.00000 0.00064 0.00063 0.00071 0.00051 0.00051 0.00048 0.00028 H22 -0.14629 0.81017 0.63237 1.00000 0.03718 0.00000 0.00548 N25 0.17502 0.63227 0.82267 1.00000 0.01979 0.01590 0.01800 0.00036 0.00319 0.00170 0.01801 0.00228 0.00020 0.00014 0.00008 0.00000 0.00065 0.00063 0.00065 0.00049 0.00049 0.00048 0.00028 H25 0.25850 0.56694 0.79459 1.00000 0.03204 0.00000 0.00510 O1W 0.82040 0.08376 0.89158 1.00000 0.03084 0.04414 0.04643 0.01948 -0.00798 0.00748 0.04030 0.00290 0.00023 0.00018 0.00010 0.00000 0.00073 0.00086 0.00092 0.00069 0.00062 0.00062 0.00035 H1W 0.78519 0.05430 0.83719 1.00000 0.09628 0.04653 0.00524 0.00362 0.00132 0.00000 0.01161 H2W 0.74270 0.15377 0.90117 1.00000 0.07655 0.05113 0.00443 0.00283 0.00179 0.00000 0.00967 O2W 0.58822 0.32312 0.92446 1.00000 0.02837 0.04217 0.02867 0.00927 -0.00698 -0.00223 0.03407 0.00236 0.00021 0.00016 0.00009 0.00000 0.00071 0.00078 0.00071 0.00058 0.00053 0.00056 0.00031 H21W 0.46511 0.28001 0.94494 1.00000 0.06701 0.04532 0.00330 0.00290 0.00150 0.00000 0.00830 H22W 0.55121 0.36266 0.87622 1.00000 0.05150 0.04268 0.00372 0.00263 0.00118 0.00000 0.00687 O3W -0.20572 0.82965 1.00407 1.00000 0.03166 0.03714 0.04692 0.01626 -0.00728 -0.00191 0.03945 0.00261 0.00023 0.00017 0.00010 0.00000 0.00075 0.00080 0.00087 0.00067 0.00062 0.00057 0.00034 H31W -0.20266 0.91032 0.97230 1.00000 0.06428 0.04520 0.00416 0.00245 0.00144 0.00000 0.00809 H32W -0.09491 0.85622 1.04064 1.00000 0.06275 0.03540 0.00357 0.00285 0.00142 0.00000 0.00791 Final Structure Factor Calculation for 04mbh0608 in P-1 Total number of l.s. parameters = 222 Maximum vector length = 511 Memory required = 3254 / 22995 wR2 = 0.1122 before cycle 5 for 3575 data and 0 / 222 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 6. 3. 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 0.005 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.032; Restrained GooF = 1.031 for 9 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0479 * P )^2 + 0.38 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0436 for 2759 Fo > 4sig(Fo) and 0.0635 for all 3575 data wR2 = 0.1122, GooF = S = 1.032, Restrained GooF = 1.031 for all data Occupancy sum of asymmetric unit = 21.00 for non-hydrogen and 28.00 for hydrogen atoms Principal mean square atomic displacements U 0.0576 0.0150 0.0104 C1 0.0260 0.0150 0.0136 C2 0.0241 0.0152 0.0132 C3 0.0195 0.0152 0.0145 C4 0.0845 0.0379 0.0135 O1A 0.0752 0.0239 0.0135 O1B 0.0325 0.0225 0.0163 O2 0.0431 0.0149 0.0132 O3 0.0406 0.0202 0.0143 O4A 0.0229 0.0198 0.0151 O4B 0.0422 0.0246 0.0166 C21 0.0224 0.0184 0.0126 C23 0.0250 0.0200 0.0148 C24 0.0364 0.0308 0.0144 C26 0.0467 0.0230 0.0175 C27 0.0372 0.0291 0.0167 C28 0.0279 0.0174 0.0116 N22 0.0221 0.0166 0.0153 N25 0.0662 0.0355 0.0192 O1W 0.0537 0.0278 0.0207 O2W 0.0647 0.0282 0.0255 O3W Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.020 0.032 0.043 0.056 0.073 0.093 0.126 0.181 1.000 Number in group 384. 334. 377. 345. 353. 361. 351. 354. 358. 358. GooF 0.994 1.026 1.095 1.049 1.058 0.971 1.034 1.031 1.058 0.997 K 2.129 1.011 1.037 0.952 0.963 0.988 0.990 1.004 1.024 0.991 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.33 1.66 inf Number in group 363. 353. 369. 346. 359. 353. 360. 362. 350. 360. GooF 0.895 0.929 0.939 0.923 1.002 1.069 0.951 0.992 1.139 1.385 K 1.017 1.012 1.008 1.005 0.995 1.005 1.011 1.015 1.033 0.975 R1 0.162 0.137 0.122 0.102 0.083 0.061 0.042 0.037 0.035 0.033 Recommended weighting scheme: WGHT 0.0479 0.3813 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) 4 1 5 73.26 146.57 6.32 0.129 1.29 -4 2 7 15.83 3.87 5.53 0.021 1.25 -1 1 1 239.42 323.41 4.65 0.191 5.09 1 -1 9 163.93 117.62 4.60 0.115 1.60 0 -3 8 10.34 0.85 4.54 0.010 1.59 -3 8 0 4.56 20.42 4.53 0.048 1.02 -3 0 4 9.77 2.42 4.46 0.017 1.80 1 0 0 0.10 9.36 4.42 0.033 6.03 6 -3 6 151.50 255.98 4.13 0.170 0.93 2 0 2 231.90 179.55 3.92 0.142 2.77 1 0 9 7.76 1.67 3.76 0.014 1.61 5 -3 2 93.31 65.46 3.70 0.086 1.17 0 -3 6 179.47 141.03 3.48 0.126 1.91 -1 2 0 4.44 0.47 3.47 0.007 3.80 -1 1 2 1319.87 1579.72 3.38 0.422 4.41 0 2 4 16.27 27.36 3.37 0.056 2.81 -2 -2 7 251.38 203.34 3.30 0.151 1.60 3 0 11 43.78 29.91 3.17 0.058 1.12 -1 -3 5 77.82 57.88 3.12 0.081 1.92 4 -2 10 30.84 45.66 3.05 0.072 1.06 2 -1 7 25.67 16.34 3.04 0.043 1.74 -1 -3 8 14.58 7.56 3.01 0.029 1.51 -1 0 1 70.26 91.49 2.99 0.102 5.65 -2 4 4 42.20 29.44 2.98 0.058 1.70 -3 1 14 3.71 10.62 2.97 0.035 0.97 -2 2 15 6.41 15.69 2.96 0.042 0.95 -2 -5 11 1.35 9.59 2.95 0.033 0.99 3 7 1 47.88 65.65 2.95 0.086 0.97 0 -4 8 13.21 4.81 2.93 0.023 1.43 2 1 13 618.95 520.53 2.92 0.242 1.06 -2 -4 1 259.36 215.86 2.91 0.156 1.61 2 4 4 7.89 3.26 2.91 0.019 1.47 -4 3 8 4.49 0.01 2.90 0.001 1.15 1 -2 9 59.88 43.96 2.90 0.070 1.54 -1 1 0 103.16 129.13 2.86 0.121 5.38 0 -4 3 34.70 23.93 2.84 0.052 1.98 4 -3 9 77.79 59.79 2.83 0.082 1.08 0 2 1 1062.85 1234.85 2.80 0.373 4.09 3 -8 5 11.33 0.58 2.79 0.008 0.97 1 9 6 -1.75 5.16 2.78 0.024 0.85 2 0 9 90.46 114.17 2.76 0.113 1.45 -1 -1 2 9.09 3.68 2.73 0.020 3.97 1 2 1 120.12 146.94 2.70 0.129 3.14 3 3 1 124.07 101.18 2.68 0.107 1.51 2 -2 4 88.55 70.64 2.65 0.089 2.18 3 -4 17 15.80 28.78 2.65 0.057 0.78 -3 7 4 16.56 8.01 2.64 0.030 1.08 1 0 2 527.20 615.93 2.63 0.264 4.66 -2 0 18 16.34 30.88 2.62 0.059 0.82 4 2 12 17.92 28.51 2.62 0.057 0.91 Bond lengths and angles C1 - Distance Angles O1A 1.2441 (0.0024) O1B 1.2592 (0.0024) 124.07 (0.16) C2 1.5247 (0.0022) 118.02 (0.17) 117.90 (0.16) C1 - O1A O1B C2 - Distance Angles O2 1.4131 (0.0020) C1 1.5247 (0.0022) 111.28 (0.13) C3 1.5255 (0.0021) 110.59 (0.12) 109.59 (0.12) H2 1.0000 108.43 108.43 108.43 C2 - O2 C1 C3 C3 - Distance Angles O3 1.4082 (0.0018) C2 1.5255 (0.0021) 109.24 (0.12) C4 1.5257 (0.0021) 111.29 (0.12) 111.45 (0.12) H3 1.0000 108.25 108.25 108.25 C3 - O3 C2 C4 C4 - Distance Angles O4A 1.2293 (0.0018) O4B 1.2831 (0.0018) 125.14 (0.14) C3 1.5257 (0.0021) 118.92 (0.13) 115.91 (0.12) C4 - O4A O4B O1A - Distance Angles C1 1.2441 (0.0024) O1A - O1B - Distance Angles C1 1.2592 (0.0024) O1B - O2 - Distance Angles C2 1.4131 (0.0020) H2O 0.8400 109.47 O2 - C2 O3 - Distance Angles C3 1.4082 (0.0018) H3O 0.8400 109.47 O3 - C3 O4A - Distance Angles C4 1.2293 (0.0018) O4A - O4B - Distance Angles C4 1.2831 (0.0018) O4B - C21 - Distance Angles N22 1.4863 (0.0022) H21A 0.9800 109.47 H21B 0.9800 109.47 109.47 H21C 0.9800 109.47 109.47 109.47 C21 - N22 H21A H21B C23 - Distance Angles N22 1.4924 (0.0019) C24 1.5111 (0.0022) 111.10 (0.12) H23A 0.9900 109.42 109.42 H23B 0.9900 109.42 109.42 108.02 C23 - N22 C24 H23A C24 - Distance Angles N25 1.4897 (0.0020) C23 1.5111 (0.0022) 110.25 (0.12) H24A 0.9900 109.61 109.61 H24B 0.9900 109.61 109.61 108.13 C24 - N25 C23 H24A C26 - Distance Angles N25 1.4859 (0.0021) H26A 0.9800 109.47 H26B 0.9800 109.47 109.47 H26C 0.9800 109.47 109.47 109.47 C26 - N25 H26A H26B C27 - Distance Angles N22 1.4874 (0.0020) H27A 0.9800 109.47 H27B 0.9800 109.47 109.47 H27C 0.9800 109.47 109.47 109.47 C27 - N22 H27A H27B C28 - Distance Angles N25 1.4855 (0.0020) H28A 0.9800 109.47 H28B 0.9800 109.47 109.47 H28C 0.9800 109.47 109.47 109.47 C28 - N25 H28A H28B N22 - Distance Angles C21 1.4863 (0.0022) C27 1.4874 (0.0020) 111.43 (0.13) C23 1.4924 (0.0019) 109.67 (0.12) 112.39 (0.12) H22 0.9300 107.72 107.72 107.72 N22 - C21 C27 C23 N25 - Distance Angles C28 1.4855 (0.0020) C26 1.4859 (0.0021) 110.56 (0.13) C24 1.4897 (0.0020) 113.00 (0.13) 110.22 (0.12) H25 0.9300 107.61 107.61 107.61 N25 - C28 C26 C24 O1W - Distance Angles H1W 0.8714 (0.0169) H2W 0.8453 (0.0164) 103.47 (2.07) O1W - H1W O2W - Distance Angles H21W 0.8504 (0.0162) H22W 0.8554 (0.0156) 103.82 (1.88) O2W - H21W O3W - Distance Angles H31W 0.8539 (0.0163) H32W 0.8632 (0.0161) 103.48 (1.98) O3W - H31W Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 2.16 2.6402(18) 116.0 O2-H2O...O1A 0.84 2.18 2.6427(16) 114.3 O3-H3O...O4A 0.93 1.74 2.6514(18) 167.1 N25-H25...O4B 0.93 2.50 3.120(2) 124.1 N25-H25...O4A 0.871(17) 1.888(17) 2.753(3) 172(3) O1W-H1W...O1B 0.845(16) 1.910(17) 2.753(2) 176(3) O1W-H2W...O2W 0.855(16) 1.966(16) 2.816(2) 172(2) O2W-H22W...O4B 0.84 2.10 2.858(2) 150.6 O2-H2O...O1A_$1 0.84 2.15 2.8475(17) 140.5 O3-H3O...O1B_$2 0.93 2.14 3.049(2) 165.8 N22-H22...O1B_$3 0.93 2.14 2.840(2) 130.7 N22-H22...O1A_$3 0.854(16) 1.944(17) 2.795(2) 174(3) O3W-H31W...O1W_$3 0.850(16) 1.895(16) 2.743(2) 175(2) O2W-H21W...O3W_$4 0.863(16) 1.937(17) 2.794(2) 172(3) O3W-H32W...O1W_$5 FMAP and GRID set by program FMAP 2 1 17 GRID -3.571 -2 -2 3.571 2 2 R1 = 0.0635 for 3575 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.26 at 0.2330 0.9734 0.2405 [ 0.74 A from O1B ] Deepest hole -0.38 at 0.2998 0.0557 0.3399 [ 0.78 A from C1 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 3317 / 20474 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.7670 0.0266 0.7595 1.00000 0.05 0.26 0.74 O1B 1.20 H1W 1.74 C1 2.06 O1W Q2 1 0.4754 0.1762 0.6956 1.00000 0.05 0.26 0.75 C3 0.78 C2 1.40 H2 1.41 H3 Q3 1 0.3486 0.2457 0.7245 1.00000 0.05 0.23 0.76 C3 0.78 C4 1.45 H3 1.72 O4B Q4 1 0.7274 -0.0255 0.6974 1.00000 0.05 0.21 0.37 O1B 0.94 C1 1.85 O1A 1.99 H22 Q5 1 0.0370 0.6629 0.7152 1.00000 0.05 0.20 0.73 C24 0.79 C23 1.38 H24B 1.41 H23B Q6 1 0.6091 -0.0721 0.5597 1.00000 0.05 0.19 0.38 O1A 1.62 C1 1.73 H2O 2.21 H2O Q7 1 0.5810 0.0800 0.6595 1.00000 0.05 0.18 0.72 C1 0.85 C2 1.60 H2 1.68 O1A Q8 1 0.7788 -0.0672 0.7121 1.00000 0.05 0.18 0.46 O1B 1.47 C1 1.72 H22 2.04 H3O Q9 1 0.6786 -0.0322 0.6146 1.00000 0.05 0.18 0.61 O1A 0.79 C1 1.65 O1B 1.89 H22 Q10 1 -0.0613 0.8063 0.8854 1.00000 0.05 0.17 1.66 H24A 1.85 H28C 1.88 H26C 1.89 H31W Shortest distances between peaks (including symmetry equivalents) 4 8 0.56 6 9 0.96 1 4 1.04 1 8 1.09 2 3 1.15 2 7 1.26 4 9 1.28 7 9 1.40 4 7 1.50 8 9 1.64 1 7 1.98 6 7 2.02 7 8 2.06 4 6 2.20 1 9 2.28 3 7 2.40 6 8 2.51 2 4 2.52 1 2 2.56 2 9 2.66 6 6 2.67 5 10 2.97 Time profile in seconds ----------------------- 0.06: 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 0.03: Set up l.s. refinement 0.00: Generate idealized H-atoms 0.64: Structure factors and derivatives 1.16: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.16: Solve l.s. equations 0.00: Generate HTAB table 0.00: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 04mbh0608 finished at 17:53:00 Total CPU time: 3.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++