+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 04mbh0607 started at 16:53:57 on 15-Jan-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 04mbh0607 in P2(1)/c CELL 0.71073 7.3883 14.2268 21.7440 90.000 93.867 90.000 ZERR 8.00 0.0026 0.0048 0.0077 0.000 0.030 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H O N UNIT 64 152 56 8 V = 2280.35 F(000) = 1040.0 Mu = 0.12 mm-1 Cell Wt = 1929.94 Rho = 1.405 MERG 2 OMIT -3.00 55.00 DFIX 0.84 0.02 O1W H1W O1W H2W O2W H21W O2W H22W DANG 1.35 0.02 H1W H2W H21W H22W SHEL 7 0.77 HTAB O2 O1W HTAB O3 O2W HTAB N25 O4A HTAB N25 O3 HTAB O33 O34A HTAB N45 O33 EQIV_$1 x+1, y, z HTAB O4B O1A_$1 HTAB O32 O1A_$1 EQIV_$2 -x+2, y-1/2, -z+1/2 HTAB N25 O32_$2 EQIV_$3 -x+1, y-1/2, -z+1/2 HTAB N25 O31B_$3 HTAB O2W O31B_$3 HTAB O2W O32_$3 EQIV _$4 x-1, y, z HTAB O31A O34B_$4 HTAB N45 O34A_$4 HTAB O2W O4A_$4 EQIV_$5 x+1, -y+3/2, z+1/2 HTAB O33 O1W_$5 EQIV_$6 -x, -y+1, -z HTAB O1W O1B_$6 EQIV_$7 -x+1, -y+1, -z HTAB O1W O2_$7 EQIV_$8 -x+1, y+1/2, -z+1/2 HTAB N45 O2_$8 HTAB N45 O1B_$8 HTAB N45 O3_$8 FMAP 2 PLAN 10 SIZE 0.03 0.03 0.12 ACTA BOND $H WGHT 0.04020 0.77990 L.S. 4 TEMP -153.00 FVAR 0.46027 MOLE 1 C1 1 0.106075 0.580213 0.115210 11.00000 0.01307 0.01557 = 0.01528 0.00457 -0.00133 0.00166 C2 1 0.313268 0.590320 0.115251 11.00000 0.01351 0.01666 = 0.01666 -0.00010 0.00116 0.00174 AFIX 13 H2 2 0.345293 0.657279 0.107163 11.00000 -1.20000 AFIX 0 C3 1 0.401948 0.559557 0.177481 11.00000 0.01243 0.01597 = 0.01722 -0.00116 0.00069 0.00086 AFIX 13 H3 2 0.366146 0.603686 0.210337 11.00000 -1.20000 AFIX 0 C4 1 0.607612 0.557114 0.176715 11.00000 0.01625 0.01846 = 0.01273 -0.00382 -0.00048 0.00087 O1A 3 0.025913 0.634284 0.151420 11.00000 0.01207 0.02018 = 0.02090 -0.00378 0.00091 0.00143 O1B 3 0.030950 0.521582 0.080314 11.00000 0.01346 0.02378 = 0.02274 -0.00579 -0.00280 0.00027 O2 3 0.385717 0.531638 0.070518 11.00000 0.01476 0.02829 = 0.01339 -0.00194 0.00058 0.00507 AFIX 147 H2O 2 0.340800 0.546480 0.035339 11.00000 -1.50000 AFIX 0 O3 3 0.347077 0.467631 0.191476 11.00000 0.01220 0.02113 = 0.02405 0.00595 0.00431 0.00002 AFIX 147 H3O 2 0.247782 0.469674 0.208107 11.00000 -1.50000 AFIX 0 O4A 3 0.696655 0.492152 0.197994 11.00000 0.01283 0.02525 = 0.03192 0.00791 0.00014 0.00282 O4B 3 0.676151 0.631933 0.151838 11.00000 0.00960 0.01948 = 0.03137 0.00248 -0.00006 -0.00040 AFIX 147 H4 2 0.789653 0.627128 0.153068 11.00000 -1.50000 AFIX 0 MOLE 2 C21 1 0.650916 0.354594 0.465036 11.00000 0.02603 0.04914 = 0.02201 -0.00301 -0.00021 -0.00265 AFIX 137 H21A 2 0.626198 0.382927 0.504687 11.00000 -1.50000 H21B 2 0.766546 0.320685 0.469244 11.00000 -1.50000 H21C 2 0.553249 0.310699 0.452302 11.00000 -1.50000 AFIX 0 C22 1 0.661392 0.431325 0.416762 11.00000 0.02910 0.03631 = 0.02276 -0.00577 0.00087 -0.00635 AFIX 23 H22A 2 0.763679 0.473614 0.429349 11.00000 -1.20000 H22B 2 0.548600 0.469001 0.415959 11.00000 -1.20000 AFIX 0 C23 1 0.686657 0.395795 0.351823 11.00000 0.02247 0.02775 = 0.02022 -0.00105 0.00082 -0.00473 AFIX 23 H23B 2 0.727980 0.448394 0.326457 11.00000 -1.20000 H23A 2 0.782358 0.346977 0.353658 11.00000 -1.20000 AFIX 0 C24 1 0.514530 0.355155 0.321343 11.00000 0.01937 0.02429 = 0.01720 -0.00161 0.00104 0.00042 AFIX 23 H24B 2 0.478537 0.299094 0.344574 11.00000 -1.20000 H24A 2 0.415868 0.402107 0.322318 11.00000 -1.20000 AFIX 0 N25 4 0.539276 0.328294 0.256456 11.00000 0.01352 0.01723 = 0.02038 0.00008 0.00004 0.00105 AFIX 137 H25A 2 0.641887 0.293245 0.254869 11.00000 0.01993 H25B 2 0.549112 0.381079 0.233282 11.00000 0.03902 H25C 2 0.441994 0.294096 0.241454 11.00000 0.03094 AFIX 0 MOLE 3 C31 1 0.873415 0.679769 0.303184 11.00000 0.01457 0.01713 = 0.01466 -0.00431 0.00138 -0.00238 C32 1 1.076748 0.664559 0.299893 11.00000 0.01235 0.01539 = 0.01869 -0.00008 0.00269 0.00010 AFIX 13 H32 2 1.099697 0.597374 0.289363 11.00000 -1.20000 AFIX 0 C33 1 1.176766 0.687785 0.361512 11.00000 0.01344 0.01896 = 0.01851 -0.00040 0.00120 0.00141 AFIX 13 H33 2 1.147760 0.638163 0.391899 11.00000 -1.20000 AFIX 0 C34 1 1.382403 0.690564 0.357363 11.00000 0.01302 0.02417 = 0.01345 0.00448 0.00046 0.00109 O31A 3 0.798008 0.620250 0.338652 11.00000 0.00980 0.02508 = 0.02907 0.00370 0.00315 0.00090 AFIX 147 H31 2 0.685329 0.629031 0.336468 11.00000 -1.50000 AFIX 0 O31B 3 0.795200 0.742682 0.274389 11.00000 0.01593 0.02733 = 0.03190 0.01017 0.00137 0.00391 O32 3 1.143280 0.723380 0.253727 11.00000 0.01668 0.02305 = 0.01341 -0.00183 0.00146 -0.00469 AFIX 147 H32O 2 1.111646 0.701520 0.218756 11.00000 -1.50000 AFIX 0 O33 3 1.114810 0.775276 0.382885 11.00000 0.01298 0.02506 = 0.02756 -0.01131 0.00108 -0.00090 AFIX 147 H33O 2 1.204102 0.808156 0.395573 11.00000 -1.50000 AFIX 0 O34A 3 1.459637 0.763719 0.375793 11.00000 0.01339 0.02457 = 0.02915 -0.00504 0.00110 -0.00223 O34B 3 1.457658 0.618938 0.335769 11.00000 0.01239 0.02259 = 0.03265 -0.00180 0.00303 0.00043 MOLE 4 C41 1 0.848439 0.571584 0.569242 11.00000 0.03636 0.03205 = 0.03270 0.00543 0.00547 0.00553 AFIX 137 H41A 2 0.872454 0.556439 0.612999 11.00000 -1.50000 H41B 2 0.944143 0.544614 0.545604 11.00000 -1.50000 H41C 2 0.730858 0.545295 0.554442 11.00000 -1.50000 AFIX 0 C42 1 0.845134 0.677391 0.561013 11.00000 0.02173 0.02869 = 0.01997 -0.00024 0.00303 0.00168 AFIX 23 H42A 2 0.960991 0.703893 0.578820 11.00000 -1.20000 H42B 2 0.746097 0.703932 0.584124 11.00000 -1.20000 AFIX 0 C43 1 0.817671 0.707132 0.494019 11.00000 0.01943 0.02300 = 0.02192 -0.00040 0.00274 0.00010 AFIX 23 H43A 2 0.922939 0.686254 0.471677 11.00000 -1.20000 H43B 2 0.708072 0.675843 0.474974 11.00000 -1.20000 AFIX 0 C44 1 0.796604 0.812321 0.487281 11.00000 0.02682 0.02336 = 0.01730 -0.00296 0.00170 -0.00118 AFIX 23 H44A 2 0.686714 0.832885 0.507214 11.00000 -1.20000 H44B 2 0.902712 0.843979 0.508419 11.00000 -1.20000 AFIX 0 N45 4 0.781366 0.840287 0.421373 11.00000 0.01627 0.01901 = 0.02133 -0.00167 0.00142 -0.00071 AFIX 137 H45A 2 0.682260 0.812342 0.402121 11.00000 0.03615 H45B 2 0.882735 0.821823 0.403091 11.00000 0.04240 H45C 2 0.769760 0.903843 0.418498 11.00000 0.03838 AFIX 0 MOLE 5 O1W 3 0.285884 0.566825 -0.047671 11.00000 0.01615 0.02563 = 0.01981 -0.00300 0.00064 -0.00056 H1W 2 0.189754 0.536583 -0.059792 11.00000 0.05101 H2W 2 0.373428 0.539210 -0.062553 11.00000 0.05872 MOLE 6 O2W 3 0.043039 0.429685 0.244535 11.00000 0.01566 0.02101 = 0.03343 0.00138 0.00331 0.00070 H21W 2 -0.056661 0.447283 0.228385 11.00000 0.05916 H22W 2 0.043622 0.370872 0.241686 11.00000 0.04937 HKLF 4 Covalent radii and connectivity table for 04mbh0607 in P2(1)/c C 0.770 H 0.320 O 0.660 N 0.700 C1 - O1B O1A C2 C2 - O2 C3 C1 C3 - O3 C4 C2 C4 - O4A O4B C3 O1A - C1 O1B - C1 O2 - C2 O3 - C3 O4A - C4 O4B - C4 C21 - C22 C22 - C21 C23 C23 - C24 C22 C24 - N25 C23 N25 - C24 C31 - O31B O31A C32 C32 - O32 C33 C31 C33 - O33 C32 C34 C34 - O34A O34B C33 O31A - C31 O31B - C31 O32 - C32 O33 - C33 O34A - C34 O34B - C34 C41 - C42 C42 - C41 C43 C43 - C44 C42 C44 - N45 C43 N45 - C44 O1W - no bonds found O2W - no bonds found Operators for generating equivalent atoms: $1 x+1, y, z $2 -x+2, y-1/2, -z+1/2 $3 -x+1, y-1/2, -z+1/2 $4 x-1, y, z $5 x+1, -y+3/2, z+1/2 $6 -x, -y+1, -z $7 -x+1, -y+1, -z $8 -x+1, y+1/2, -z+1/2 23934 Reflections read, of which 494 rejected -9 =< h =< 8, -18 =< k =< 18, -28 =< l =< 27, Max. 2-theta = 54.97 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 6 3 0 0.04 0.75 4 3.95 -6 9 3 45.89 3.22 6 16.27 7 7 6 14.45 2.82 5 14.88 -7 3 8 0.83 0.68 5 3.55 7 3 11 32.62 3.83 4 22.27 5 Inconsistent equivalents 5223 Unique reflections, of which 0 suppressed R(int) = 0.0618 R(sigma) = 0.0688 Friedel opposites merged Maximum memory for data reduction = 4026 / 51940 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 = 4959 / 403380 wR2 = 0.1099 before cycle 1 for 5223 data and 321 / 321 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 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 0.009 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.036 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0402 * P )^2 + 0.78 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.46026 0.00070 -0.008 OSF Mean shift/esd = 0.002 Maximum = -0.008 for OSF Max. shift = 0.000 A for H1W Max. dU = 0.000 for H1W Least-squares cycle 2 Maximum vector length = 511 Memory required = 4959 / 403380 wR2 = 0.1099 before cycle 2 for 5223 data and 321 / 321 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 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 0.009 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.036 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0402 * P )^2 + 0.78 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.46026 0.00070 -0.001 OSF Mean shift/esd = 0.001 Maximum = 0.002 for U12 O4B Max. shift = 0.000 A for H1W Max. dU = 0.000 for H1W Least-squares cycle 3 Maximum vector length = 511 Memory required = 4959 / 403380 wR2 = 0.1099 before cycle 3 for 5223 data and 321 / 321 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 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 0.009 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.036 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0402 * P )^2 + 0.78 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.46026 0.00070 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y C1 Max. shift = 0.000 A for H21W Max. dU = 0.000 for H21W Least-squares cycle 4 Maximum vector length = 511 Memory required = 4959 / 403380 wR2 = 0.1099 before cycle 4 for 5223 data and 321 / 321 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 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 0.009 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.036 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0402 * P )^2 + 0.78 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.46026 0.00070 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O32 Max. shift = 0.000 A for H1W Max. dU = 0.000 for H25A Largest correlation matrix elements 0.531 x H2W / x H1W Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.3453 0.6573 0.1072 13 1.000 0.000 C2 O2 C3 C1 H3 0.3661 0.6037 0.2103 13 1.000 0.000 C3 O3 C4 C2 H2O 0.3408 0.5465 0.0353 147 0.840 0.000 O2 C2 H2O H3O 0.2478 0.4697 0.2081 147 0.840 0.000 O3 C3 H3O H4 0.7897 0.6271 0.1531 147 0.840 0.000 O4B C4 H4 H21A 0.6262 0.3829 0.5047 137 0.980 0.000 C21 C22 H21A H21B 0.7665 0.3207 0.4692 137 0.980 0.000 C21 C22 H21A H21C 0.5533 0.3107 0.4523 137 0.980 0.000 C21 C22 H21A H22A 0.7637 0.4736 0.4293 23 0.990 0.000 C22 C21 C23 H22B 0.5486 0.4690 0.4160 23 0.990 0.000 C22 C21 C23 H23B 0.7280 0.4484 0.3265 23 0.990 0.000 C23 C24 C22 H23A 0.7824 0.3470 0.3537 23 0.990 0.000 C23 C24 C22 H24B 0.4785 0.2991 0.3446 23 0.990 0.000 C24 N25 C23 H24A 0.4159 0.4021 0.3223 23 0.990 0.000 C24 N25 C23 H25A 0.6419 0.2932 0.2549 137 0.910 0.000 N25 C24 H25A H25B 0.5491 0.3811 0.2333 137 0.910 0.000 N25 C24 H25A H25C 0.4420 0.2941 0.2415 137 0.910 0.000 N25 C24 H25A H32 1.0997 0.5974 0.2894 13 1.000 0.000 C32 O32 C33 C31 H33 1.1478 0.6382 0.3919 13 1.000 0.000 C33 O33 C32 C34 H31 0.6853 0.6290 0.3365 147 0.840 0.000 O31A C31 H31 H32O 1.1116 0.7015 0.2188 147 0.840 0.000 O32 C32 H32O H33O 1.2041 0.8082 0.3956 147 0.840 0.000 O33 C33 H33O H41A 0.8725 0.5564 0.6130 137 0.980 0.000 C41 C42 H41A H41B 0.9441 0.5446 0.5456 137 0.980 0.000 C41 C42 H41A H41C 0.7309 0.5453 0.5544 137 0.980 0.000 C41 C42 H41A H42A 0.9610 0.7039 0.5788 23 0.990 0.000 C42 C41 C43 H42B 0.7461 0.7039 0.5841 23 0.990 0.000 C42 C41 C43 H43A 0.9229 0.6863 0.4717 23 0.990 0.000 C43 C44 C42 H43B 0.7081 0.6758 0.4750 23 0.990 0.000 C43 C44 C42 H44A 0.6867 0.8329 0.5072 23 0.990 0.000 C44 N45 C43 H44B 0.9027 0.8440 0.5084 23 0.990 0.000 C44 N45 C43 H45A 0.6823 0.8123 0.4021 137 0.910 0.000 N45 C44 H45A H45B 0.8827 0.8218 0.4031 137 0.910 0.000 N45 C44 H45A H45C 0.7698 0.9038 0.4185 137 0.910 0.000 N45 C44 H45A 04mbh0607 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.10608 0.58021 0.11521 1.00000 0.01307 0.01557 0.01528 0.00457 -0.00133 0.00166 0.01474 0.00317 0.00023 0.00012 0.00008 0.00000 0.00089 0.00097 0.00102 0.00078 0.00069 0.00069 0.00039 C2 0.31327 0.59032 0.11525 1.00000 0.01351 0.01666 0.01666 -0.00010 0.00116 0.00174 0.01560 0.00320 0.00023 0.00013 0.00008 0.00000 0.00090 0.00095 0.00102 0.00078 0.00068 0.00070 0.00039 H2 0.34529 0.65728 0.10716 1.00000 0.01872 0.00000 0.00000 C3 0.40195 0.55956 0.17748 1.00000 0.01243 0.01597 0.01722 -0.00116 0.00069 0.00086 0.01522 0.00313 0.00022 0.00013 0.00008 0.00000 0.00089 0.00094 0.00103 0.00077 0.00069 0.00068 0.00039 H3 0.36615 0.60369 0.21034 1.00000 0.01826 0.00000 0.00000 C4 0.60761 0.55711 0.17671 1.00000 0.01625 0.01846 0.01273 -0.00381 -0.00048 0.00087 0.01588 0.00308 0.00023 0.00013 0.00008 0.00000 0.00094 0.00098 0.00099 0.00078 0.00070 0.00074 0.00039 O1A 0.02591 0.63428 0.15142 1.00000 0.01207 0.02018 0.02089 -0.00378 0.00091 0.00143 0.01772 0.00217 0.00016 0.00009 0.00006 0.00000 0.00063 0.00069 0.00075 0.00057 0.00050 0.00050 0.00029 O1B 0.03095 0.52158 0.08031 1.00000 0.01346 0.02378 0.02274 -0.00579 -0.00280 0.00027 0.02018 0.00216 0.00016 0.00009 0.00006 0.00000 0.00065 0.00074 0.00077 0.00060 0.00052 0.00052 0.00030 O2 0.38572 0.53164 0.07052 1.00000 0.01476 0.02829 0.01339 -0.00194 0.00058 0.00507 0.01883 0.00225 0.00016 0.00009 0.00006 0.00000 0.00066 0.00076 0.00071 0.00059 0.00050 0.00052 0.00030 H2O 0.34080 0.54648 0.03534 1.00000 0.02824 0.00000 0.00000 O3 0.34708 0.46763 0.19148 1.00000 0.01220 0.02113 0.02404 0.00595 0.00431 0.00002 0.01898 0.00225 0.00016 0.00009 0.00006 0.00000 0.00066 0.00072 0.00079 0.00058 0.00052 0.00049 0.00030 H3O 0.24778 0.46967 0.20811 1.00000 0.02848 0.00000 0.00000 O4A 0.69665 0.49215 0.19799 1.00000 0.01283 0.02525 0.03192 0.00791 0.00014 0.00282 0.02340 0.00239 0.00016 0.00009 0.00006 0.00000 0.00065 0.00077 0.00085 0.00064 0.00054 0.00054 0.00032 O4B 0.67615 0.63193 0.15184 1.00000 0.00960 0.01948 0.03136 0.00248 -0.00006 -0.00040 0.02022 0.00227 0.00016 0.00009 0.00006 0.00000 0.00063 0.00072 0.00085 0.00060 0.00053 0.00049 0.00031 H4 0.78965 0.62713 0.15307 1.00000 0.03032 0.00000 0.00000 C21 0.65092 0.35459 0.46504 1.00000 0.02603 0.04914 0.02201 -0.00301 -0.00021 -0.00265 0.03248 0.00392 0.00028 0.00017 0.00010 0.00000 0.00114 0.00145 0.00123 0.00106 0.00085 0.00097 0.00052 H21A 0.62619 0.38293 0.50469 1.00000 0.04871 0.00000 0.00000 H21B 0.76655 0.32069 0.46925 1.00000 0.04871 0.00000 0.00000 H21C 0.55325 0.31070 0.45230 1.00000 0.04871 0.00000 0.00000 C22 0.66139 0.43133 0.41676 1.00000 0.02910 0.03631 0.02276 -0.00577 0.00087 -0.00635 0.02943 0.00367 0.00029 0.00015 0.00010 0.00000 0.00115 0.00129 0.00121 0.00099 0.00086 0.00091 0.00050 H22A 0.76368 0.47361 0.42935 1.00000 0.03532 0.00000 0.00000 H22B 0.54860 0.46900 0.41596 1.00000 0.03532 0.00000 0.00000 C23 0.68666 0.39580 0.35182 1.00000 0.02246 0.02775 0.02021 -0.00105 0.00082 -0.00473 0.02350 0.00339 0.00026 0.00015 0.00009 0.00000 0.00101 0.00112 0.00112 0.00089 0.00078 0.00082 0.00044 H23B 0.72798 0.44839 0.32646 1.00000 0.02820 0.00000 0.00000 H23A 0.78236 0.34698 0.35366 1.00000 0.02820 0.00000 0.00000 C24 0.51453 0.35515 0.32134 1.00000 0.01937 0.02429 0.01720 -0.00161 0.00104 0.00042 0.02030 0.00328 0.00025 0.00014 0.00009 0.00000 0.00097 0.00107 0.00108 0.00085 0.00074 0.00077 0.00042 H24B 0.47854 0.29909 0.34457 1.00000 0.02435 0.00000 0.00000 H24A 0.41587 0.40211 0.32232 1.00000 0.02435 0.00000 0.00000 N25 0.53928 0.32829 0.25646 1.00000 0.01352 0.01723 0.02038 0.00008 0.00004 0.00105 0.01709 0.00264 0.00019 0.00011 0.00007 0.00000 0.00078 0.00085 0.00092 0.00071 0.00060 0.00061 0.00035 H25A 0.64189 0.29325 0.25487 1.00000 0.01993 0.00000 0.00521 H25B 0.54911 0.38108 0.23328 1.00000 0.03902 0.00000 0.00681 H25C 0.44199 0.29410 0.24145 1.00000 0.03094 0.00000 0.00601 C31 0.87342 0.67977 0.30318 1.00000 0.01457 0.01713 0.01466 -0.00430 0.00138 -0.00238 0.01544 0.00304 0.00023 0.00013 0.00008 0.00000 0.00091 0.00097 0.00100 0.00080 0.00070 0.00072 0.00039 C32 1.07675 0.66456 0.29989 1.00000 0.01235 0.01539 0.01869 -0.00008 0.00269 0.00010 0.01540 0.00315 0.00022 0.00013 0.00008 0.00000 0.00090 0.00095 0.00103 0.00078 0.00069 0.00067 0.00039 H32 1.09970 0.59737 0.28936 1.00000 0.01849 0.00000 0.00000 C33 1.17677 0.68778 0.36151 1.00000 0.01344 0.01896 0.01851 -0.00040 0.00120 0.00141 0.01696 0.00319 0.00023 0.00013 0.00009 0.00000 0.00090 0.00099 0.00105 0.00079 0.00070 0.00070 0.00040 H33 1.14776 0.63816 0.39190 1.00000 0.02036 0.00000 0.00000 C34 1.38240 0.69056 0.35736 1.00000 0.01302 0.02417 0.01345 0.00448 0.00046 0.00109 0.01690 0.00329 0.00023 0.00013 0.00009 0.00000 0.00090 0.00107 0.00100 0.00082 0.00068 0.00076 0.00040 O31A 0.79801 0.62025 0.33865 1.00000 0.00980 0.02508 0.02906 0.00370 0.00315 0.00090 0.02123 0.00238 0.00016 0.00009 0.00006 0.00000 0.00063 0.00077 0.00083 0.00061 0.00052 0.00051 0.00031 H31 0.68533 0.62903 0.33647 1.00000 0.03185 0.00000 0.00000 O31B 0.79520 0.74268 0.27439 1.00000 0.01593 0.02733 0.03190 0.01017 0.00137 0.00391 0.02507 0.00247 0.00017 0.00010 0.00007 0.00000 0.00070 0.00079 0.00088 0.00066 0.00056 0.00055 0.00033 O32 1.14328 0.72338 0.25373 1.00000 0.01668 0.02305 0.01341 -0.00183 0.00146 -0.00469 0.01769 0.00215 0.00016 0.00009 0.00006 0.00000 0.00065 0.00073 0.00070 0.00057 0.00051 0.00051 0.00029 H32O 1.11165 0.70152 0.21876 1.00000 0.02654 0.00000 0.00000 O33 1.11481 0.77528 0.38289 1.00000 0.01298 0.02506 0.02756 -0.01131 0.00108 -0.00090 0.02188 0.00221 0.00016 0.00009 0.00006 0.00000 0.00065 0.00076 0.00083 0.00061 0.00054 0.00051 0.00032 H33O 1.20410 0.80816 0.39557 1.00000 0.03282 0.00000 0.00000 O34A 1.45964 0.76372 0.37579 1.00000 0.01339 0.02457 0.02915 -0.00504 0.00110 -0.00223 0.02239 0.00225 0.00016 0.00009 0.00006 0.00000 0.00067 0.00077 0.00084 0.00062 0.00054 0.00053 0.00032 O34B 1.45766 0.61894 0.33577 1.00000 0.01239 0.02259 0.03265 -0.00180 0.00303 0.00043 0.02247 0.00231 0.00016 0.00009 0.00007 0.00000 0.00066 0.00075 0.00087 0.00062 0.00055 0.00052 0.00032 C41 0.84844 0.57158 0.56924 1.00000 0.03636 0.03205 0.03270 0.00543 0.00547 0.00553 0.03356 0.00421 0.00031 0.00015 0.00011 0.00000 0.00126 0.00130 0.00136 0.00104 0.00096 0.00095 0.00053 H41A 0.87245 0.55644 0.61300 1.00000 0.05034 0.00000 0.00000 H41B 0.94414 0.54461 0.54560 1.00000 0.05034 0.00000 0.00000 H41C 0.73086 0.54530 0.55444 1.00000 0.05034 0.00000 0.00000 C42 0.84513 0.67739 0.56101 1.00000 0.02173 0.02869 0.01997 -0.00024 0.00303 0.00168 0.02339 0.00356 0.00026 0.00014 0.00009 0.00000 0.00101 0.00114 0.00112 0.00090 0.00077 0.00081 0.00044 H42A 0.96099 0.70389 0.57882 1.00000 0.02807 0.00000 0.00000 H42B 0.74610 0.70393 0.58412 1.00000 0.02807 0.00000 0.00000 C43 0.81767 0.70713 0.49402 1.00000 0.01943 0.02300 0.02192 -0.00040 0.00274 0.00010 0.02139 0.00343 0.00025 0.00013 0.00009 0.00000 0.00097 0.00107 0.00112 0.00086 0.00076 0.00076 0.00043 H43A 0.92294 0.68625 0.47168 1.00000 0.02566 0.00000 0.00000 H43B 0.70807 0.67584 0.47497 1.00000 0.02566 0.00000 0.00000 C44 0.79660 0.81232 0.48728 1.00000 0.02682 0.02336 0.01730 -0.00296 0.00170 -0.00118 0.02249 0.00343 0.00027 0.00014 0.00009 0.00000 0.00105 0.00109 0.00109 0.00085 0.00078 0.00081 0.00044 H44A 0.68671 0.83289 0.50721 1.00000 0.02698 0.00000 0.00000 H44B 0.90271 0.84398 0.50842 1.00000 0.02698 0.00000 0.00000 N45 0.78137 0.84029 0.42137 1.00000 0.01627 0.01900 0.02133 -0.00167 0.00142 -0.00071 0.01886 0.00275 0.00020 0.00011 0.00007 0.00000 0.00083 0.00092 0.00092 0.00071 0.00063 0.00063 0.00036 H45A 0.68226 0.81234 0.40212 1.00000 0.03615 0.00000 0.00635 H45B 0.88273 0.82182 0.40309 1.00000 0.04240 0.00000 0.00685 H45C 0.76976 0.90384 0.41850 1.00000 0.03838 0.00000 0.00673 O1W 0.28588 0.56683 -0.04767 1.00000 0.01615 0.02563 0.01981 -0.00300 0.00064 -0.00056 0.02056 0.00236 0.00018 0.00009 0.00006 0.00000 0.00072 0.00079 0.00079 0.00061 0.00055 0.00059 0.00031 H1W 0.18976 0.53658 -0.05979 1.00000 0.05100 0.03299 0.00233 0.00165 0.00117 0.00000 0.00796 H2W 0.37343 0.53921 -0.06255 1.00000 0.05871 0.04350 0.00245 0.00173 0.00119 0.00000 0.00894 O2W 0.04304 0.42968 0.24454 1.00000 0.01566 0.02100 0.03343 0.00138 0.00331 0.00070 0.02329 0.00247 0.00018 0.00010 0.00007 0.00000 0.00075 0.00084 0.00091 0.00066 0.00059 0.00056 0.00033 H21W -0.05666 0.44728 0.22838 1.00000 0.05917 0.04220 0.00269 0.00164 0.00121 0.00000 0.00889 H22W 0.04362 0.37087 0.24169 1.00000 0.04937 0.04050 0.00317 0.00113 0.00122 0.00000 0.00827 Final Structure Factor Calculation for 04mbh0607 in P2(1)/c Total number of l.s. parameters = 321 Maximum vector length = 511 Memory required = 4638 / 22995 wR2 = 0.1099 before cycle 5 for 5223 data and 0 / 321 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 4. 2. 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 0.009 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.037; Restrained GooF = 1.036 for 6 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0402 * P )^2 + 0.78 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0516 for 3511 Fo > 4sig(Fo) and 0.0954 for all 5223 data wR2 = 0.1099, GooF = S = 1.037, Restrained GooF = 1.036 for all data Occupancy sum of asymmetric unit = 32.00 for non-hydrogen and 38.00 for hydrogen atoms Principal mean square atomic displacements U 0.0201 0.0150 0.0092 C1 0.0174 0.0167 0.0127 C2 0.0181 0.0154 0.0122 C3 0.0209 0.0160 0.0107 C4 0.0245 0.0169 0.0117 O1A 0.0298 0.0187 0.0119 O1B 0.0303 0.0134 0.0128 O2 0.0289 0.0171 0.0109 O3 0.0372 0.0211 0.0119 O4A 0.0321 0.0190 0.0096 O4B 0.0497 0.0268 0.0209 C21 0.0410 0.0276 0.0197 C22 0.0305 0.0210 0.0190 C23 0.0247 0.0193 0.0169 C24 0.0206 0.0175 0.0131 N25 0.0209 0.0142 0.0111 C31 0.0190 0.0154 0.0118 C32 0.0195 0.0183 0.0131 C33 0.0258 0.0134 0.0115 C34 0.0314 0.0229 0.0095 O31A 0.0401 0.0210 0.0141 O31B 0.0257 0.0143 0.0130 O32 0.0377 0.0151 0.0128 O33 0.0324 0.0218 0.0129 O34A 0.0330 0.0223 0.0121 O34B 0.0429 0.0312 0.0266 C41 0.0291 0.0223 0.0188 C42 0.0232 0.0223 0.0187 C43 0.0273 0.0241 0.0161 C44 0.0222 0.0183 0.0161 N45 0.0269 0.0188 0.0160 O1W 0.0336 0.0209 0.0153 O2W Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.008 0.017 0.025 0.034 0.044 0.057 0.073 0.096 0.139 1.000 Number in group 539. 573. 490. 532. 486. 525. 521. 523. 513. 521. GooF 1.015 1.040 1.048 1.012 1.060 1.065 0.994 1.064 0.975 1.090 K 6.818 1.968 1.212 1.017 1.103 1.031 1.005 1.001 1.012 0.992 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.32 1.65 inf Number in group 534. 523. 516. 524. 523. 511. 527. 523. 516. 526. GooF 0.959 0.971 1.025 1.059 0.978 1.001 1.009 0.951 0.993 1.357 K 1.125 1.106 1.039 1.024 1.011 1.014 1.011 1.014 1.025 0.977 R1 0.273 0.221 0.166 0.177 0.108 0.095 0.056 0.041 0.042 0.033 Recommended weighting scheme: WGHT 0.0402 0.7758 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 1 1 2 1732.82 2220.89 5.01 0.210 5.46 -7 1 2 171.38 385.46 4.75 0.088 1.05 -1 0 2 2748.27 3703.19 3.90 0.271 6.30 -1 3 3 829.16 682.85 3.65 0.117 3.55 -1 2 1 1782.78 2124.87 3.62 0.206 5.03 -5 2 13 32.34 0.38 3.57 0.003 1.13 2 0 0 2540.43 3023.63 3.57 0.245 3.69 -5 3 4 140.48 4.63 3.55 0.010 1.38 0 4 0 1741.28 2078.24 3.53 0.203 3.56 -3 0 20 90.22 1.26 3.40 0.005 1.02 0 14 4 83.29 3.22 3.37 0.008 1.00 2 0 4 3470.82 4083.90 3.31 0.285 2.96 -1 4 7 127.20 87.12 3.21 0.042 2.26 -1 3 2 4869.45 5623.98 3.21 0.335 3.79 7 10 8 65.52 163.93 3.10 0.057 0.80 4 1 22 134.97 241.78 3.10 0.069 0.84 -2 2 1 5323.91 6113.87 3.09 0.349 3.26 7 5 5 22.09 46.61 3.09 0.030 0.95 -1 10 22 519.46 342.04 3.06 0.083 0.81 5 9 2 33.51 2.51 3.06 0.007 1.07 -2 5 1 90.32 59.86 3.03 0.035 2.25 -2 5 2 12.06 30.55 3.03 0.025 2.22 -8 3 9 1257.44 942.87 3.03 0.137 0.87 0 2 3 584.16 695.27 3.03 0.118 5.07 0 8 9 96.79 58.95 3.01 0.034 1.43 1 3 5 84.70 52.85 3.00 0.032 2.88 -3 10 6 172.41 230.34 3.00 0.068 1.18 1 1 1 66.16 43.46 2.99 0.029 6.16 -2 5 18 106.82 166.30 2.98 0.058 1.08 8 6 9 111.09 28.06 2.97 0.024 0.79 4 10 7 184.04 248.89 2.96 0.070 1.04 8 2 2 171.23 290.42 2.94 0.076 0.91 -2 13 7 195.26 269.30 2.90 0.073 1.00 -4 1 25 369.97 75.61 2.90 0.039 0.81 4 14 0 64.69 12.94 2.90 0.016 0.89 -3 14 8 59.26 135.61 2.90 0.052 0.89 5 3 9 529.97 438.41 2.89 0.093 1.18 1 7 0 69.16 41.81 2.87 0.029 1.96 8 0 0 195.57 366.10 2.87 0.085 0.92 5 5 8 66.16 34.58 2.87 0.026 1.15 2 0 8 388.18 296.18 2.86 0.077 2.12 -1 11 15 69.50 5.26 2.84 0.010 0.96 -2 3 19 168.43 243.08 2.84 0.070 1.08 2 2 6 120.17 86.79 2.83 0.042 2.36 0 5 15 74.27 37.30 2.80 0.027 1.29 -4 4 4 255.28 313.47 2.80 0.079 1.59 5 15 0 49.64 158.83 2.79 0.056 0.80 4 9 15 246.80 337.93 2.79 0.082 0.90 2 7 1 56.69 24.73 2.78 0.022 1.77 1 2 5 593.15 502.89 2.77 0.100 3.24 Bond lengths and angles C1 - Distance Angles O1B 1.2340 (0.0022) O1A 1.2749 (0.0022) 125.39 (0.16) C2 1.5375 (0.0024) 118.04 (0.16) 116.56 (0.16) C1 - O1B O1A C2 - Distance Angles O2 1.4142 (0.0022) C3 1.5272 (0.0026) 106.29 (0.14) C1 1.5375 (0.0024) 111.56 (0.15) 109.96 (0.15) H2 1.0000 109.66 109.66 109.66 C2 - O2 C3 C1 C3 - Distance Angles O3 1.4085 (0.0022) C4 1.5211 (0.0024) 106.47 (0.14) C2 1.5272 (0.0026) 110.18 (0.15) 111.47 (0.15) H3 1.0000 109.56 109.56 109.56 C3 - O3 C4 C2 C4 - Distance Angles O4A 1.2083 (0.0022) O4B 1.3111 (0.0022) 124.30 (0.17) C3 1.5211 (0.0024) 122.13 (0.17) 113.57 (0.15) C4 - O4A O4B O1A - Distance Angles C1 1.2749 (0.0022) O1A - O1B - Distance Angles C1 1.2340 (0.0022) O1B - O2 - Distance Angles C2 1.4142 (0.0022) H2O 0.8400 109.47 O2 - C2 O3 - Distance Angles C3 1.4085 (0.0022) H3O 0.8400 109.47 O3 - C3 O4A - Distance Angles C4 1.2083 (0.0022) O4A - O4B - Distance Angles C4 1.3111 (0.0022) H4 0.8400 109.47 O4B - C4 C21 - Distance Angles C22 1.5200 (0.0031) 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 C21 1.5200 (0.0031) C23 1.5231 (0.0029) 114.65 (0.18) H22A 0.9900 108.60 108.60 H22B 0.9900 108.60 108.60 107.57 C22 - C21 C23 H22A C23 - Distance Angles C24 1.5090 (0.0026) C22 1.5231 (0.0029) 112.46 (0.16) H23B 0.9900 109.11 109.11 H23A 0.9900 109.11 109.11 107.85 C23 - C24 C22 H23B C24 - Distance Angles N25 1.4849 (0.0025) C23 1.5090 (0.0026) 111.21 (0.15) H24B 0.9900 109.39 109.39 H24A 0.9900 109.39 109.39 108.01 C24 - N25 C23 H24B N25 - Distance Angles C24 1.4849 (0.0025) H25A 0.9100 109.47 H25B 0.9100 109.47 109.47 H25C 0.9100 109.47 109.47 109.47 N25 - C24 H25A H25B C31 - Distance Angles O31B 1.2158 (0.0022) O31A 1.2962 (0.0022) 125.37 (0.17) C32 1.5242 (0.0025) 121.07 (0.16) 113.56 (0.16) C31 - O31B O31A C32 - Distance Angles O32 1.4199 (0.0022) C33 1.5221 (0.0026) 108.89 (0.14) C31 1.5242 (0.0025) 109.80 (0.15) 110.45 (0.15) H32 1.0000 109.23 109.23 109.23 C32 - O32 C33 C31 C33 - Distance Angles O33 1.4155 (0.0022) C32 1.5221 (0.0026) 109.35 (0.15) C34 1.5286 (0.0025) 109.96 (0.15) 112.28 (0.15) H33 1.0000 108.39 108.39 108.39 C33 - O33 C32 C34 C34 - Distance Angles O34A 1.2404 (0.0022) O34B 1.2662 (0.0022) 126.24 (0.17) C33 1.5286 (0.0025) 116.11 (0.16) 117.65 (0.16) C34 - O34A O34B O31A - Distance Angles C31 1.2962 (0.0022) H31 0.8400 109.47 O31A - C31 O31B - Distance Angles C31 1.2158 (0.0022) O31B - O32 - Distance Angles C32 1.4199 (0.0022) H32O 0.8400 109.47 O32 - C32 O33 - Distance Angles C33 1.4155 (0.0022) H33O 0.8400 109.47 O33 - C33 O34A - Distance Angles C34 1.2404 (0.0022) O34A - O34B - Distance Angles C34 1.2662 (0.0022) O34B - C41 - Distance Angles C42 1.5159 (0.0030) H41A 0.9800 109.47 H41B 0.9800 109.47 109.47 H41C 0.9800 109.47 109.47 109.47 C41 - C42 H41A H41B C42 - Distance Angles C41 1.5159 (0.0030) C43 1.5174 (0.0028) 112.97 (0.17) H42A 0.9900 108.99 108.99 H42B 0.9900 108.99 108.99 107.78 C42 - C41 C43 H42A C43 - Distance Angles C44 1.5107 (0.0028) C42 1.5174 (0.0028) 112.06 (0.16) H43A 0.9900 109.20 109.20 H43B 0.9900 109.20 109.20 107.90 C43 - C44 C42 H43A C44 - Distance Angles N45 1.4842 (0.0025) C43 1.5107 (0.0028) 111.09 (0.16) H44A 0.9900 109.42 109.42 H44B 0.9900 109.42 109.42 108.02 C44 - N45 C43 H44A N45 - Distance Angles C44 1.4842 (0.0025) H45A 0.9100 109.47 H45B 0.9100 109.47 109.47 H45C 0.9100 109.47 109.47 109.47 N45 - C44 H45A H45B O1W - Distance Angles H1W 0.8566 (0.0157) H2W 0.8400 (0.0158) 106.89 (2.00) O1W - H1W O2W - Distance Angles H21W 0.8329 (0.0159) H22W 0.8390 (0.0157) 106.11 (1.98) O2W - H21W Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.84 1.85 2.673(2) 167.7 O2-H2O...O1W 0.84 1.84 2.649(2) 160.0 O3-H3O...O2W 0.91 2.09 2.933(2) 152.7 N25-H25B...O4A 0.91 2.09 2.770(2) 130.1 N25-H25B...O3 0.84 2.06 2.5680(19) 118.0 O33-H33O...O34A 0.91 1.92 2.811(2) 167.2 N45-H45B...O33 0.84 1.75 2.5850(19) 171.5 O4B-H4...O1A_$1 0.84 1.83 2.6546(19) 168.5 O32-H32O...O1A_$1 0.91 1.89 2.801(2) 176.2 N25-H25A...O32_$2 0.91 1.91 2.796(2) 164.3 N25-H25C...O31B_$3 0.839(16) 2.219(18) 2.957(2) 147(2) O2W-H22W...O31B_$3 0.839(16) 2.52(2) 3.243(2) 145(2) O2W-H22W...O32_$3 0.84 1.69 2.5112(19) 166.3 O31A-H31...O34B_$4 0.91 1.84 2.739(2) 169.2 N45-H45A...O34A_$4 0.833(16) 2.001(16) 2.831(2) 174(3) O2W-H21W...O4A_$4 0.84 2.23 2.944(2) 143.6 O33-H33O...O1W_$5 0.857(16) 1.856(16) 2.7095(19) 174(2) O1W-H1W...O1B_$6 0.840(16) 2.063(17) 2.8738(19) 162(3) O1W-H2W...O2_$7 0.91 2.17 2.999(2) 150.7 N45-H45C...O2_$8 0.91 2.23 2.930(2) 133.4 N45-H45C...O1B_$8 0.91 2.65 3.145(2) 115.2 N45-H45C...O3_$8 FMAP and GRID set by program FMAP 2 1 19 GRID -3.125 -2 -1 3.125 2 1 R1 = 0.0953 for 5223 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.29 at 0.4958 0.0582 0.3278 [ 0.76 A from C4 ] Deepest hole -0.32 at 0.3054 0.0564 0.3323 [ 0.68 A from C4 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 5115 / 39455 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5042 0.5582 0.1722 1.00000 0.05 0.29 0.76 C4 0.77 C3 1.50 H3 1.73 O4B Q2 1 0.2137 0.5764 0.1152 1.00000 0.05 0.26 0.76 C2 0.80 C1 1.52 H2 1.69 O1B Q3 1 0.5734 0.6288 0.3262 1.00000 0.05 0.26 0.84 H31 0.90 O34B 1.67 O31A 1.83 C34 Q4 1 1.3116 0.6914 0.2486 1.00000 0.05 0.24 1.34 O32 1.49 H25A 1.57 H3 1.58 H32O Q5 1 0.6275 0.6009 0.4821 1.00000 0.05 0.24 1.24 H43B 1.88 H41C 1.93 H21A 2.07 C43 Q6 1 1.5597 0.7580 0.3779 1.00000 0.05 0.23 0.74 O34A 1.28 H45A 1.66 C34 2.18 N45 Q7 1 1.2817 0.6916 0.3551 1.00000 0.05 0.22 0.74 C34 0.80 C33 1.52 H33 1.70 O34A Q8 1 0.9767 0.6789 0.3046 1.00000 0.05 0.20 0.76 C31 0.78 C32 1.52 H32 1.71 O31B Q9 1 1.1240 0.6720 0.3285 1.00000 0.05 0.20 0.70 C32 0.82 C33 1.37 H32 1.46 H33 Q10 1 0.8569 0.9260 0.3671 1.00000 0.05 0.19 1.36 H45C 1.68 H45B 1.81 N45 1.87 H3O Shortest distances between peaks (including symmetry equivalents) 8 9 1.18 7 9 1.30 3 6 2.16 2 10 2.24 6 7 2.28 4 9 2.31 4 7 2.34 1 2 2.42 7 8 2.45 3 7 2.45 3 4 2.63 4 8 2.84 1 4 2.95 Time profile in seconds ----------------------- 0.04: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.01: 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. 0.98: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.01: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.88: Structure factors and derivatives 3.19: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.01: Apply other restraints 0.29: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.08: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 04mbh0607 finished at 16:54:04 Total CPU time: 6.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++