+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0239 started at 09:14:54 on 12-Mar-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0239 in P2(1)2(1)2(1) CELL 0.71073 8.9301 10.8793 23.2605 90.000 90.000 90.000 ZERR 4.00 0.0002 0.0002 0.0004 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N O I UNIT 72 112 16 8 8 V = 2259.83 F(000) = 1144.0 Mu = 2.80 mm-1 Cell Wt = 2344.98 Rho = 1.723 MERG 2 OMIT -3.00 55.00 OMIT 1 1 2 OMIT 5 8 8 SHEL 7 0.77 FMAP 2 PLAN 10 SIZE 0.15 0.35 0.43 ACTA HTAB 2.00000 BOND $H WGHT 0.02720 1.01550 L.S. 4 TEMP -153.00 FVAR 0.30078 C6 1 0.524080 1.045825 0.204487 11.00000 0.02753 0.04008 = 0.01762 -0.00877 0.00569 -0.02282 AFIX 13 H6 2 0.541331 1.037023 0.162209 11.00000 -1.20000 AFIX 0 C7 1 0.649957 0.981598 0.235878 11.00000 0.01705 0.04082 = 0.06048 -0.02159 0.00442 -0.00675 AFIX 137 H7A 2 0.633928 0.988329 0.277439 11.00000 -1.50000 H7B 2 0.745542 1.020142 0.225709 11.00000 -1.50000 H7C 2 0.652009 0.894683 0.224838 11.00000 -1.50000 AFIX 0 C8 1 0.516157 1.182949 0.218926 11.00000 0.04343 0.02866 = 0.03042 0.00688 -0.00802 -0.01944 AFIX 137 H8A 2 0.424498 1.218058 0.202582 11.00000 -1.50000 H8B 2 0.603506 1.224981 0.202678 11.00000 -1.50000 H8C 2 0.515394 1.193593 0.260761 11.00000 -1.50000 AFIX 0 C9 1 0.070073 0.782360 0.190155 11.00000 0.01213 0.01613 = 0.01559 -0.00089 -0.00225 0.00017 AFIX 13 H9 2 0.013101 0.745702 0.222955 11.00000 -1.20000 AFIX 0 C10 1 0.143507 0.681040 0.153901 11.00000 0.01361 0.01203 = 0.01465 -0.00022 0.00188 -0.00293 AFIX 13 H10 2 0.248496 0.663992 0.166550 11.00000 -1.20000 AFIX 0 C12 1 -0.036526 0.841551 0.147331 11.00000 0.01689 0.01737 = 0.01973 -0.00559 0.00033 0.00229 AFIX 23 H12A 2 -0.134130 0.798400 0.147210 11.00000 -1.20000 H12B 2 -0.053516 0.929003 0.157124 11.00000 -1.20000 AFIX 0 C13 1 0.023954 1.057761 0.398731 11.00000 0.01233 0.01812 = 0.02420 0.00224 0.00071 -0.00008 AFIX 23 H13A 2 0.123649 1.097486 0.397591 11.00000 -1.20000 H13B 2 0.036953 0.969634 0.408091 11.00000 -1.20000 AFIX 0 C15 1 -0.137574 1.229123 0.407994 11.00000 0.01004 0.01026 = 0.01808 0.00036 0.00173 0.00040 AFIX 13 H15 2 -0.239165 1.254165 0.421773 11.00000 -1.20000 AFIX 0 C16 1 -0.076955 1.120349 0.442645 11.00000 0.01058 0.01407 = 0.01640 0.00180 -0.00316 -0.00421 AFIX 13 H16 2 -0.018836 1.148648 0.476926 11.00000 -1.20000 AFIX 0 C22 1 -0.469503 0.797743 0.434167 11.00000 0.02802 0.03014 = 0.02197 -0.00013 -0.00018 -0.01333 AFIX 13 H22 2 -0.425970 0.770726 0.396627 11.00000 -1.20000 AFIX 0 C23 1 -0.467594 0.690102 0.473962 11.00000 0.09265 0.02609 = 0.06352 0.01165 -0.02867 -0.02875 AFIX 137 H23A 2 -0.364641 0.660283 0.478238 11.00000 -1.50000 H23B 2 -0.530386 0.624390 0.458173 11.00000 -1.50000 H23C 2 -0.506501 0.714971 0.511601 11.00000 -1.50000 AFIX 0 C24 1 -0.628306 0.844598 0.422734 11.00000 0.02884 0.04582 = 0.08784 -0.01192 -0.01393 -0.00901 AFIX 137 H24A 2 -0.670927 0.877226 0.458433 11.00000 -1.50000 H24B 2 -0.690653 0.776764 0.408751 11.00000 -1.50000 H24C 2 -0.625038 0.909810 0.393696 11.00000 -1.50000 AFIX 0 O11 4 0.036212 0.830614 0.091669 11.00000 0.02451 0.01378 = 0.02141 0.00087 -0.00512 0.00668 O14 4 -0.052440 1.072396 0.344742 11.00000 0.02560 0.01385 = 0.01301 0.00255 0.00199 0.00713 MOLE 1 C2 1 0.307365 0.908773 0.184705 11.00000 0.02400 0.02231 = 0.01173 -0.00485 0.00136 -0.00207 AFIX 43 H2 2 0.338690 0.884762 0.147325 11.00000 -1.20000 AFIX 0 C4 1 0.176438 0.927145 0.264371 11.00000 0.02648 0.02451 = 0.01011 -0.00729 0.00452 0.00057 AFIX 43 H4 2 0.100610 0.916983 0.292619 11.00000 -1.20000 AFIX 0 C5 1 0.296736 0.999962 0.268346 11.00000 0.02802 0.01814 = 0.01747 -0.00328 0.00358 -0.00238 AFIX 43 H5 2 0.320655 1.051809 0.299901 11.00000 -1.20000 AFIX 0 C18 1 -0.261781 0.949187 0.428251 11.00000 0.01180 0.01625 = 0.01572 -0.00043 0.00168 0.00010 AFIX 43 H18 2 -0.227147 0.924184 0.391448 11.00000 -1.20000 AFIX 0 C20 1 -0.391000 0.962155 0.508543 11.00000 0.02602 0.03269 = 0.01539 0.00468 0.00579 -0.00433 AFIX 43 H20 2 -0.463779 0.946788 0.537451 11.00000 -1.20000 AFIX 0 C21 1 -0.282614 1.049024 0.510155 11.00000 0.01961 0.02513 = 0.01164 0.00037 -0.00017 -0.00010 AFIX 43 H21 2 -0.264605 1.105689 0.540451 11.00000 -1.20000 AFIX 0 N1 3 0.379894 0.986912 0.218914 11.00000 0.01872 0.01742 = 0.01595 -0.00513 0.00289 -0.00425 N3 3 0.183114 0.869353 0.211379 11.00000 0.01508 0.01375 = 0.01489 -0.00441 -0.00217 -0.00150 N17 3 -0.203428 1.039714 0.459585 11.00000 0.01204 0.01813 = 0.01078 0.00309 0.00128 0.00088 N19 3 -0.376034 0.899226 0.456465 11.00000 0.01852 0.01702 = 0.01898 0.00255 0.00111 -0.00561 I1 5 0.564672 0.710436 0.100494 11.00000 0.01224 0.02705 = 0.02023 0.00250 -0.00032 -0.00069 I2 5 -0.072270 0.694606 0.351235 11.00000 0.03356 0.01684 = 0.02160 -0.00093 0.00047 0.00041 HKLF 4 Covalent radii and connectivity table for 2009src0239 in P2(1)2(1)2(1) C 0.770 H 0.320 N 0.700 O 0.660 I 1.330 C6 - N1 C7 C8 C7 - C6 C8 - C6 C9 - N3 C12 C10 C10 - O14_$2 C15_$2 C9 C12 - O11 C9 C13 - O14 C16 C15 - O11_$1 C16 C10_$1 C16 - N17 C13 C15 C22 - N19 C23 C24 C23 - C22 C24 - C22 O11 - C15_$2 C12 O14 - C10_$1 C13 C2 - N1 N3 C4 - C5 N3 C5 - C4 N1 C18 - N19 N17 C20 - C21 N19 C21 - C20 N17 N1 - C2 C5 C6 N3 - C2 C4 C9 N17 - C18 C21 C16 N19 - C18 C20 C22 I1 - no bonds found I2 - no bonds found Operators for generating equivalent atoms: $1 -x, y+1/2, -z+1/2 $2 -x, y-1/2, -z+1/2 h k l Fo^2 Sigma Why rejected 0 0 5 16.31 2.98 observed but should be systematically absent 19290 Reflections read, of which 65 rejected -11 =< h =< 10, -14 =< k =< 12, -25 =< l =< 30, Max. 2-theta = 54.95 1 Systematic absence violations 0 Inconsistent equivalents 5180 Unique reflections, of which 0 suppressed R(int) = 0.0479 R(sigma) = 0.0518 Friedel opposites not merged Maximum memory for data reduction = 2779 / 51826 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 = 3492 / 297433 wR2 = 0.0723 before cycle 1 for 5180 data and 239 / 239 parameters GooF = S = 1.045; Restrained GooF = 1.045 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0272 * P )^2 + 1.02 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.30071 0.00030 -0.230 OSF Mean shift/su = 0.080 Maximum = -0.403 for U12 N17 Max. shift = 0.002 A for H23C Max. dU = 0.000 for C23 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3492 / 297433 wR2 = 0.0723 before cycle 2 for 5180 data and 239 / 239 parameters GooF = S = 1.045; Restrained GooF = 1.045 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0272 * P )^2 + 1.02 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.30068 0.00030 -0.095 OSF Mean shift/su = 0.026 Maximum = -0.129 for U12 N17 Max. shift = 0.001 A for H24A Max. dU = 0.000 for C23 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3492 / 297433 wR2 = 0.0723 before cycle 3 for 5180 data and 239 / 239 parameters GooF = S = 1.045; Restrained GooF = 1.045 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0272 * P )^2 + 1.02 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.30068 0.00030 0.000 OSF Mean shift/su = 0.001 Maximum = 0.009 for y C23 Max. shift = 0.000 A for H24A Max. dU = 0.000 for C24 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3492 / 297433 wR2 = 0.0723 before cycle 4 for 5180 data and 239 / 239 parameters GooF = S = 1.045; Restrained GooF = 1.045 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0272 * P )^2 + 1.02 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.30068 0.00030 0.000 OSF Mean shift/su = 0.000 Maximum = -0.003 for U12 C15 Max. shift = 0.000 A for H24A Max. dU = 0.000 for C10 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H6 0.5414 1.0371 0.1622 13 1.000 0.000 C6 N1 C7 C8 H7A 0.6339 0.9883 0.2775 137 0.980 0.000 C7 C6 H7A H7B 0.7456 1.0203 0.2258 137 0.980 0.000 C7 C6 H7A H7C 0.6521 0.8948 0.2248 137 0.980 0.000 C7 C6 H7A H8A 0.4247 1.2182 0.2025 137 0.980 0.000 C8 C6 H8A H8B 0.6038 1.2250 0.2027 137 0.980 0.000 C8 C6 H8A H8C 0.5155 1.1937 0.2607 137 0.980 0.000 C8 C6 H8A H9 0.0131 0.7457 0.2229 13 1.000 0.000 C9 N3 C12 C10 H10 0.2485 0.6640 0.1666 13 1.000 0.000 C10 O14_$2 C15_$2 C9 H12A -0.1342 0.7986 0.1472 23 0.990 0.000 C12 O11 C9 H12B -0.0534 0.9291 0.1571 23 0.990 0.000 C12 O11 C9 H13A 0.1237 1.0976 0.3976 23 0.990 0.000 C13 O14 C16 H13B 0.0371 0.9697 0.4081 23 0.990 0.000 C13 O14 C16 H15 -0.2392 1.2540 0.4218 13 1.000 0.000 C15 O11_$1 C16 C10_$1 H16 -0.0189 1.1487 0.4769 13 1.000 0.000 C16 N17 C13 C15 H22 -0.4260 0.7708 0.3967 13 1.000 0.000 C22 N19 C23 C24 H23A -0.3645 0.6603 0.4782 137 0.980 0.000 C23 C22 H23A H23B -0.5303 0.6244 0.4582 137 0.980 0.000 C23 C22 H23A H23C -0.5062 0.7149 0.5116 137 0.980 0.000 C23 C22 H23A H24A -0.6709 0.8775 0.4584 137 0.980 0.000 C24 C22 H24A H24B -0.6907 0.7770 0.4088 137 0.980 0.000 C24 C22 H24A H24C -0.6249 0.9099 0.3937 137 0.980 0.000 C24 C22 H24A H2 0.3386 0.8848 0.1473 43 0.950 0.000 C2 N1 N3 H4 0.1007 0.9169 0.2926 43 0.950 0.000 C4 C5 N3 H5 0.3207 1.0518 0.2999 43 0.950 0.000 C5 C4 N1 H18 -0.2272 0.9243 0.3915 43 0.950 0.000 C18 N19 N17 H20 -0.4638 0.9467 0.5375 43 0.950 0.000 C20 C21 N19 H21 -0.2648 1.1057 0.5404 43 0.950 0.000 C21 C20 N17 2009src0239 in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C6 0.52414 1.04592 0.20450 1.00000 0.02722 0.03970 0.01759 -0.00833 0.00582 -0.02225 0.02817 0.00728 0.00049 0.00044 0.00020 0.00000 0.00247 0.00284 0.00237 0.00212 0.00191 0.00216 0.00114 H6 0.54141 1.03709 0.16222 1.00000 0.03380 0.00000 0.00000 C7 0.64999 0.98165 0.23589 1.00000 0.01708 0.04001 0.06076 -0.02242 0.00434 -0.00677 0.03928 0.00851 0.00051 0.00051 0.00025 0.00000 0.00242 0.00319 0.00375 0.00287 0.00245 0.00230 0.00137 H7A 0.63386 0.98826 0.27745 1.00000 0.05892 0.00000 0.00000 H7B 0.74557 1.02027 0.22578 1.00000 0.05892 0.00000 0.00000 H7C 0.65212 0.89477 0.22480 1.00000 0.05892 0.00000 0.00000 C8 0.51633 1.18302 0.21890 1.00000 0.04322 0.02795 0.03049 0.00689 -0.00798 -0.01899 0.03389 0.00798 0.00057 0.00042 0.00021 0.00000 0.00287 0.00268 0.00272 0.00220 0.00227 0.00236 0.00123 H8A 0.42474 1.21818 0.20253 1.00000 0.05083 0.00000 0.00000 H8B 0.60375 1.22498 0.20267 1.00000 0.05083 0.00000 0.00000 H8C 0.51551 1.19370 0.26074 1.00000 0.05083 0.00000 0.00000 C9 0.07009 0.78235 0.19014 1.00000 0.01216 0.01609 0.01553 -0.00134 -0.00219 0.00029 0.01459 0.00630 0.00043 0.00033 0.00016 0.00000 0.00170 0.00184 0.00181 0.00149 0.00171 0.00197 0.00075 H9 0.01311 0.74571 0.22295 1.00000 0.01751 0.00000 0.00000 C10 0.14347 0.68102 0.15390 1.00000 0.01392 0.01263 0.01443 -0.00027 0.00184 -0.00299 0.01366 0.00663 0.00043 0.00035 0.00017 0.00000 0.00181 0.00188 0.00194 0.00165 0.00162 0.00156 0.00080 H10 0.24846 0.66398 0.16655 1.00000 0.01639 0.00000 0.00000 C12 -0.03653 0.84167 0.14734 1.00000 0.01690 0.01745 0.01965 -0.00527 0.00039 0.00198 0.01800 0.00694 0.00043 0.00037 0.00018 0.00000 0.00211 0.00193 0.00213 0.00174 0.00184 0.00163 0.00087 H12A -0.13419 0.79861 0.14724 1.00000 0.02160 0.00000 0.00000 H12B -0.05338 0.92914 0.15714 1.00000 0.02160 0.00000 0.00000 C13 0.02406 1.05778 0.39875 1.00000 0.01216 0.01738 0.02425 0.00231 0.00102 0.00006 0.01793 0.00705 0.00042 0.00037 0.00019 0.00000 0.00192 0.00203 0.00230 0.00184 0.00177 0.00155 0.00088 H13A 0.12371 1.09758 0.39760 1.00000 0.02151 0.00000 0.00000 H13B 0.03714 0.96968 0.40813 1.00000 0.02151 0.00000 0.00000 C15 -0.13756 1.22899 0.40799 1.00000 0.01011 0.01055 0.01795 0.00035 0.00164 0.00072 0.01287 0.00652 0.00041 0.00034 0.00017 0.00000 0.00171 0.00187 0.00203 0.00159 0.00156 0.00151 0.00080 H15 -0.23917 1.25398 0.42177 1.00000 0.01544 0.00000 0.00000 C16 -0.07695 1.12034 0.44262 1.00000 0.01057 0.01421 0.01642 0.00169 -0.00353 -0.00414 0.01373 0.00649 0.00043 0.00032 0.00016 0.00000 0.00180 0.00181 0.00190 0.00150 0.00176 0.00179 0.00077 H16 -0.01887 1.14869 0.47691 1.00000 0.01648 0.00000 0.00000 C22 -0.46951 0.79775 0.43420 1.00000 0.02794 0.03013 0.02203 0.00025 0.00009 -0.01343 0.02670 0.00753 0.00048 0.00043 0.00020 0.00000 0.00243 0.00253 0.00229 0.00204 0.00186 0.00214 0.00104 H22 -0.42598 0.77076 0.39666 1.00000 0.03204 0.00000 0.00000 C23 -0.46744 0.69010 0.47396 1.00000 0.09160 0.02546 0.06368 0.01198 -0.02878 -0.02920 0.06025 0.00963 0.00080 0.00046 0.00027 0.00000 0.00487 0.00284 0.00412 0.00274 0.00375 0.00332 0.00191 H23A -0.36446 0.66027 0.47817 1.00000 0.09037 0.00000 0.00000 H23B -0.53030 0.62440 0.45820 1.00000 0.09037 0.00000 0.00000 H23C -0.50618 0.71493 0.51163 1.00000 0.09037 0.00000 0.00000 C24 -0.62830 0.84476 0.42273 1.00000 0.02889 0.04532 0.08803 -0.01251 -0.01393 -0.00994 0.05408 0.00955 0.00057 0.00056 0.00030 0.00000 0.00287 0.00366 0.00514 0.00340 0.00308 0.00265 0.00180 H24A -0.67090 0.87748 0.45841 1.00000 0.08112 0.00000 0.00000 H24B -0.69074 0.77696 0.40876 1.00000 0.08112 0.00000 0.00000 H24C -0.62492 0.90992 0.39367 1.00000 0.08112 0.00000 0.00000 O11 0.03617 0.83067 0.09167 1.00000 0.02463 0.01397 0.02130 0.00084 -0.00502 0.00684 0.01997 0.00483 0.00031 0.00024 0.00012 0.00000 0.00161 0.00136 0.00154 0.00118 0.00133 0.00121 0.00065 O14 -0.05240 1.07233 0.34473 1.00000 0.02520 0.01335 0.01311 0.00252 0.00201 0.00705 0.01722 0.00485 0.00034 0.00023 0.00011 0.00000 0.00151 0.00128 0.00137 0.00106 0.00140 0.00129 0.00059 C2 0.30735 0.90876 0.18471 1.00000 0.02386 0.02219 0.01165 -0.00476 0.00145 -0.00233 0.01923 0.00701 0.00046 0.00039 0.00017 0.00000 0.00229 0.00229 0.00201 0.00170 0.00183 0.00190 0.00093 H2 0.33863 0.88477 0.14732 1.00000 0.02308 0.00000 0.00000 C4 0.17654 0.92710 0.26436 1.00000 0.02650 0.02505 0.01005 -0.00742 0.00479 0.00105 0.02053 0.00740 0.00050 0.00040 0.00018 0.00000 0.00239 0.00240 0.00203 0.00175 0.00186 0.00195 0.00096 H4 0.10073 0.91689 0.29261 1.00000 0.02464 0.00000 0.00000 C5 0.29679 0.99996 0.26835 1.00000 0.02806 0.01807 0.01739 -0.00340 0.00378 -0.00225 0.02118 0.00765 0.00050 0.00041 0.00018 0.00000 0.00241 0.00217 0.00218 0.00180 0.00189 0.00202 0.00095 H5 0.32068 1.05183 0.29990 1.00000 0.02541 0.00000 0.00000 C18 -0.26184 0.94924 0.42828 1.00000 0.01198 0.01670 0.01566 -0.00075 0.00189 0.00024 0.01478 0.00680 0.00043 0.00036 0.00017 0.00000 0.00192 0.00207 0.00202 0.00163 0.00163 0.00168 0.00084 H18 -0.22723 0.92427 0.39147 1.00000 0.01774 0.00000 0.00000 C20 -0.39103 0.96209 0.50854 1.00000 0.02585 0.03271 0.01536 0.00450 0.00592 -0.00487 0.02464 0.00795 0.00048 0.00043 0.00019 0.00000 0.00246 0.00254 0.00219 0.00193 0.00182 0.00206 0.00102 H20 -0.46378 0.94669 0.53745 1.00000 0.02957 0.00000 0.00000 C21 -0.28273 1.04897 0.51013 1.00000 0.01962 0.02543 0.01155 0.00011 -0.00048 -0.00024 0.01887 0.00744 0.00046 0.00040 0.00017 0.00000 0.00212 0.00232 0.00200 0.00176 0.00173 0.00192 0.00091 H21 -0.26479 1.10566 0.54042 1.00000 0.02264 0.00000 0.00000 N1 0.37995 0.98688 0.21892 1.00000 0.01889 0.01780 0.01581 -0.00514 0.00281 -0.00373 0.01750 0.00570 0.00037 0.00032 0.00015 0.00000 0.00176 0.00181 0.00180 0.00145 0.00143 0.00147 0.00076 N3 0.18321 0.86935 0.21138 1.00000 0.01500 0.01425 0.01482 -0.00449 -0.00208 -0.00130 0.01469 0.00548 0.00036 0.00030 0.00014 0.00000 0.00166 0.00173 0.00172 0.00137 0.00146 0.00141 0.00072 N17 -0.20347 1.03973 0.45959 1.00000 0.01208 0.01806 0.01074 0.00314 0.00126 0.00012 0.01363 0.00551 0.00035 0.00030 0.00013 0.00000 0.00162 0.00174 0.00162 0.00138 0.00136 0.00144 0.00070 N19 -0.37604 0.89918 0.45648 1.00000 0.01842 0.01672 0.01903 0.00231 0.00113 -0.00616 0.01806 0.00588 0.00036 0.00032 0.00015 0.00000 0.00172 0.00178 0.00189 0.00149 0.00151 0.00146 0.00076 I1 0.56467 0.71043 0.10049 1.00000 0.01221 0.02702 0.02021 0.00251 -0.00032 -0.00065 0.01982 0.00045 0.00003 0.00002 0.00001 0.00000 0.00012 0.00015 0.00014 0.00011 0.00012 0.00013 0.00008 I2 -0.07227 0.69460 0.35123 1.00000 0.03353 0.01678 0.02158 -0.00092 0.00047 0.00039 0.02396 0.00047 0.00003 0.00002 0.00001 0.00000 0.00016 0.00013 0.00014 0.00011 0.00014 0.00014 0.00008 Final Structure Factor Calculation for 2009src0239 in P2(1)2(1)2(1) Total number of l.s. parameters = 239 Maximum vector length = 511 Memory required = 3255 / 26068 wR2 = 0.0723 before cycle 5 for 5180 data and 2 / 239 parameters GooF = S = 1.045; Restrained GooF = 1.045 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0272 * P )^2 + 1.02 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0313 for 4674 Fo > 4sig(Fo) and 0.0374 for all 5180 data wR2 = 0.0723, GooF = S = 1.045, Restrained GooF = 1.045 for all data Flack x parameter = -0.0094 with su 0.0235 Expected values are 0 (within 3 su's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Occupancy sum of asymmetric unit = 26.00 for non-hydrogen and 28.00 for hydrogen atoms Principal mean square atomic displacements U 0.0591 0.0151 0.0103 C6 0.0760 0.0267 0.0151 C7 0.0598 0.0269 0.0150 C8 0.0177 0.0150 0.0111 C9 0.0173 0.0137 0.0100 C10 0.0241 0.0175 0.0124 C12 0.0250 0.0167 0.0121 C13 0.0183 0.0109 0.0094 C15 0.0202 0.0137 0.0073 C16 0.0425 0.0220 0.0155 C22 0.1199 0.0464 0.0144 C23 0.0933 0.0494 0.0195 C24 0.0300 0.0201 0.0098 O11 0.0290 0.0132 0.0094 O14 0.0266 0.0213 0.0098 C2 0.0287 0.0270 0.0059 C4 0.0301 0.0192 0.0142 C5 0.0172 0.0160 0.0111 C18 0.0353 0.0276 0.0110 C20 0.0254 0.0196 0.0115 C21 0.0254 0.0155 0.0116 N1 0.0191 0.0158 0.0091 N3 0.0193 0.0125 0.0091 N17 0.0239 0.0197 0.0106 N19 0.0279 0.0194 0.0122 I1 0.0336 0.0217 0.0166 I2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.036 0.057 0.075 0.094 0.115 0.140 0.169 0.208 0.276 1.000 Number in group 529. 525. 503. 524. 520. 504. 518. 525. 515. 517. GooF 0.937 1.121 1.125 1.080 1.092 1.104 0.972 1.007 1.001 0.993 K 1.007 0.952 0.972 0.984 0.987 0.990 1.013 1.012 1.017 0.985 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.66 inf Number in group 541. 494. 520. 525. 525. 516. 505. 520. 515. 519. GooF 1.021 0.989 0.902 1.011 0.996 0.987 0.972 0.826 0.961 1.594 K 0.956 0.980 1.004 1.029 1.031 1.014 1.012 1.008 1.004 0.970 R1 0.081 0.077 0.058 0.052 0.046 0.033 0.028 0.019 0.016 0.024 Recommended weighting scheme: WGHT 0.0268 1.0033 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)/su Fc/Fc(max) Resolution(A) 1 1 0 -6.71 79.89 6.67 0.026 6.90 -1 1 2 22312.55 39024.54 6.54 0.572 5.94 1 1 1 2756.49 5297.85 6.43 0.211 6.62 -1 1 1 3309.92 4712.34 6.38 0.199 6.62 6 9 8 245.81 849.03 6.07 0.084 0.89 2 0 0 75942.77 92766.75 5.10 0.882 4.47 0 5 7 727.00 513.46 4.99 0.066 1.82 0 2 2 1552.05 2005.09 4.69 0.130 4.93 1 0 6 1549.94 1225.83 4.48 0.101 3.56 0 0 6 2708.42 3265.93 4.33 0.165 3.88 0 0 4 47666.08 56601.21 4.32 0.689 5.82 2 0 2 176.14 262.02 4.30 0.047 4.17 4 4 4 461.36 308.96 4.25 0.051 1.65 0 0 10 -17.50 61.01 4.21 0.023 2.33 0 1 6 566.39 439.77 3.75 0.061 3.65 1 1 10 2188.24 1643.10 3.72 0.117 2.20 4 2 0 1224.40 1012.06 3.67 0.092 2.07 1 1 4 2317.88 2752.41 3.58 0.152 4.45 0 1 12 1063.62 1296.57 3.56 0.104 1.91 4 4 0 122.15 58.89 3.56 0.022 1.73 0 2 6 432.35 329.84 3.53 0.053 3.16 -2 12 14 47.83 244.29 3.49 0.045 0.78 -1 10 20 1575.90 1998.81 3.44 0.129 0.79 2 4 0 3040.23 3487.15 3.41 0.171 2.32 0 2 4 104667.47 119246.50 3.36 1.000 3.97 -1 1 10 2032.01 1756.23 3.34 0.121 2.20 -6 3 25 640.37 1023.73 3.33 0.093 0.77 -4 9 18 294.85 629.88 3.29 0.073 0.82 0 3 6 817.89 653.14 3.27 0.074 2.65 3 1 0 5224.41 5893.23 3.24 0.222 2.87 6 9 10 1542.67 2125.79 3.20 0.134 0.87 -1 1 4 2209.29 2553.94 3.17 0.146 4.45 4 3 1 2395.80 2088.59 3.16 0.132 1.89 5 8 6 572.03 783.37 3.16 0.081 1.04 0 1 4 32531.70 37691.96 3.15 0.562 5.13 10 5 4 697.55 1255.47 3.13 0.103 0.82 2 6 8 554.17 444.15 3.12 0.061 1.45 11 3 7 1178.25 2134.29 3.09 0.134 0.77 -2 2 4 6995.39 7956.34 3.08 0.258 2.97 6 0 2 1366.89 1161.48 3.07 0.099 1.48 7 9 14 954.79 1435.78 3.04 0.110 0.78 3 9 0 2070.85 1644.82 3.03 0.117 1.12 -4 7 21 175.82 381.51 3.02 0.057 0.84 4 1 8 714.15 567.69 2.92 0.069 1.75 7 2 18 1445.31 859.73 2.92 0.085 0.90 -2 5 1 429.15 545.59 2.90 0.068 1.95 -8 2 11 164.70 317.68 2.89 0.052 0.97 4 2 20 944.56 1294.57 2.86 0.104 1.01 6 6 22 1121.31 1833.11 2.86 0.124 0.78 3 2 12 19570.07 22322.81 2.85 0.433 1.56 Bond lengths and angles C6 - Distance Angles N1 1.4775 (0.0051) C7 1.5117 (0.0069) 109.70 (0.37) C8 1.5304 (0.0065) 109.53 (0.38) 112.26 (0.39) H6 1.0000 108.42 108.42 108.42 C6 - N1 C7 C8 C7 - Distance Angles C6 1.5117 (0.0069) H7A 0.9800 109.47 H7B 0.9800 109.47 109.47 H7C 0.9800 109.47 109.47 109.47 C7 - C6 H7A H7B C8 - Distance Angles C6 1.5304 (0.0065) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - C6 H8A H8B C9 - Distance Angles N3 1.4698 (0.0047) C12 1.5212 (0.0052) 112.14 (0.31) C10 1.5347 (0.0052) 110.72 (0.31) 102.27 (0.31) H9 1.0000 110.49 110.49 110.49 C9 - N3 C12 C10 C10 - Distance Angles O14_$2 1.4355 (0.0045) C15_$2 1.5323 (0.0054) 106.37 (0.29) C9 1.5347 (0.0052) 109.73 (0.29) 104.88 (0.30) H10 1.0000 111.83 111.83 111.83 C10 - O14_$2 C15_$2 C9 C12 - Distance Angles O11 1.4536 (0.0049) C9 1.5212 (0.0052) 105.58 (0.29) H12A 0.9900 110.62 110.62 H12B 0.9900 110.62 110.62 108.75 C12 - O11 C9 H12A C13 - Distance Angles O14 1.4387 (0.0049) C16 1.5226 (0.0055) 104.78 (0.29) H13A 0.9900 110.79 110.79 H13B 0.9900 110.79 110.79 108.86 C13 - O14 C16 H13A C15 - Distance Angles O11_$1 1.4295 (0.0044) C16 1.5293 (0.0051) 111.78 (0.29) C10_$1 1.5323 (0.0054) 106.89 (0.30) 104.11 (0.30) H15 1.0000 111.26 111.26 111.26 C15 - O11_$1 C16 C10_$1 C16 - Distance Angles N17 1.4837 (0.0048) C13 1.5226 (0.0055) 111.42 (0.30) C15 1.5293 (0.0051) 109.11 (0.30) 101.66 (0.31) H16 1.0000 111.42 111.42 111.42 C16 - N17 C13 C15 C22 - Distance Angles N19 1.4775 (0.0054) C23 1.4924 (0.0067) 111.21 (0.38) C24 1.5308 (0.0068) 109.57 (0.40) 112.44 (0.47) H22 1.0000 107.82 107.82 107.82 C22 - N19 C23 C24 C23 - Distance Angles C22 1.4924 (0.0067) H23A 0.9800 109.47 H23B 0.9800 109.47 109.47 H23C 0.9800 109.47 109.47 109.47 C23 - C22 H23A H23B C24 - Distance Angles C22 1.5308 (0.0068) H24A 0.9800 109.47 H24B 0.9800 109.47 109.47 H24C 0.9800 109.47 109.47 109.47 C24 - C22 H24A H24B O11 - Distance Angles C15_$2 1.4295 (0.0044) C12 1.4536 (0.0049) 109.98 (0.28) O11 - C15_$2 O14 - Distance Angles C10_$1 1.4355 (0.0045) C13 1.4387 (0.0049) 109.88 (0.28) O14 - C10_$1 C2 - Distance Angles N1 1.3326 (0.0051) N3 1.3408 (0.0051) 109.26 (0.35) H2 0.9500 125.37 125.37 C2 - N1 N3 C4 - Distance Angles C5 1.3379 (0.0060) N3 1.3844 (0.0049) 107.23 (0.37) H4 0.9500 126.39 126.39 C4 - C5 N3 C5 - Distance Angles C4 1.3379 (0.0060) N1 1.3762 (0.0051) 108.29 (0.37) H5 0.9500 125.86 125.86 C5 - C4 N1 C18 - Distance Angles N19 1.3292 (0.0049) N17 1.3309 (0.0048) 109.48 (0.35) H18 0.9500 125.26 125.26 C18 - N19 N17 C20 - Distance Angles C21 1.3528 (0.0060) N19 1.3974 (0.0056) 107.30 (0.36) H20 0.9500 126.35 126.35 C20 - C21 N19 C21 - Distance Angles C20 1.3528 (0.0060) N17 1.3760 (0.0049) 107.05 (0.37) H21 0.9500 126.47 126.47 C21 - C20 N17 N1 - Distance Angles C2 1.3326 (0.0051) C5 1.3762 (0.0051) 107.60 (0.34) C6 1.4775 (0.0052) 124.45 (0.35) 127.95 (0.35) N1 - C2 C5 N3 - Distance Angles C2 1.3408 (0.0051) C4 1.3844 (0.0049) 107.60 (0.34) C9 1.4698 (0.0047) 128.22 (0.33) 124.18 (0.33) N3 - C2 C4 N17 - Distance Angles C18 1.3309 (0.0048) C21 1.3760 (0.0049) 108.67 (0.33) C16 1.4837 (0.0048) 126.15 (0.32) 125.15 (0.33) N17 - C18 C21 N19 - Distance Angles C18 1.3292 (0.0049) C20 1.3974 (0.0056) 107.49 (0.35) C22 1.4775 (0.0054) 124.50 (0.36) 127.99 (0.35) N19 - C18 C20 FMAP and GRID set by program FMAP 2 3 28 GRID -1.000 -2 -2 1.000 2 2 R1 = 0.0313 for 2948 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.06 at 0.2558 0.9566 0.0196 [ 2.42 A from H23A ] Deepest hole -0.85 at 0.5636 0.7781 0.1044 [ 0.74 A from I1 ] Mean = 0.00, Rms deviation from mean = 0.13 e/A^3, Highest memory used = 3141 / 23149 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.2558 0.4566 0.4804 1.00000 0.05 1.06 2.42 H23A 2.42 H24A 2.60 H15 2.80 H16 Q2 1 0.1046 0.6842 0.2412 1.00000 0.05 0.44 1.14 H9 1.63 C9 2.06 C10 2.17 H10 Q3 1 0.8355 1.1798 0.2215 1.00000 0.05 0.41 1.91 H7B 2.00 H9 2.17 H8B 2.49 C9 Q4 1 0.2958 0.6271 0.1595 1.00000 0.05 0.41 0.61 H10 1.49 C10 2.20 H7A 2.26 O14 Q5 1 -0.0679 1.0042 0.3415 1.00000 0.05 0.41 0.76 O14 1.67 C13 1.85 H13B 2.03 H18 Q6 1 0.0747 1.0726 0.3992 1.00000 0.05 0.40 0.48 C13 0.52 H13A 1.19 H13B 1.70 O14 Q7 1 0.4167 0.6041 0.1555 1.00000 0.05 0.40 1.66 H10 2.05 H7A 2.17 I1 2.26 H8C Q8 1 -0.5142 0.6162 0.4294 1.00000 0.05 0.40 0.69 H23B 1.38 C23 1.82 H23A 2.01 H22 Q9 1 0.6401 1.1019 0.1511 1.00000 0.05 0.39 1.16 H6 1.73 C6 1.83 H8B 2.12 C8 Q10 1 0.6082 1.2808 0.2809 1.00000 0.05 0.39 1.34 H8C 1.77 C2 1.92 H8B 1.97 C8 Shortest distances between peaks (including symmetry equivalents) 2 3 1.02 4 7 1.11 5 6 1.99 8 9 2.19 4 10 2.33 7 10 2.44 4 5 2.44 3 9 2.54 2 4 2.63 3 10 2.69 2 5 2.76 2 10 2.82 Time profile in seconds ----------------------- 0.03: 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. 0.94: 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 0.02: Generate idealized H-atoms 2.39: Structure factors and derivatives 1.94: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.17: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.09: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0239 finished at 09:14:59 Total CPU time: 5.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++