+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src1354 started at 10:49:21 on 19-Oct-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src1354 in P2(1)2(1)2(1) CELL 0.71073 9.7683 13.0654 16.8119 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 CL UNIT 88 100 8 20 4 V = 2145.65 F(000) = 912.0 Mu = 0.21 mm-1 Cell Wt = 1731.56 Rho = 1.340 MERG 2 OMIT -3.00 55.00 OMIT 1 3 1 OMIT 1 0 3 OMIT -1 3 1 OMIT -1 1 3 OMIT 0 3 2 OMIT 1 1 3 OMIT 1 3 0 OMIT -1 2 2 OMIT 1 2 2 OMIT 0 2 3 OMIT 2 0 8 OMIT 1 2 0 FMAP 2 PLAN 20 SIZE 0.20 0.25 0.35 ACTA BOND WPDB 1 WGHT 0.05390 0.64030 L.S. 4 TEMP -153.00 FVAR 0.26446 0.58388 O2 4 0.617310 0.042294 0.032638 11.00000 0.06165 0.15787 = 0.08474 0.06771 0.02824 -0.00452 O3 4 0.487374 -0.068099 0.112117 11.00000 0.09469 0.08006 = 0.04256 0.00211 -0.00252 -0.05091 PART 1 O4 4 0.705969 -0.037101 0.133162 21.00000 0.06141 0.05757 = 0.17442 0.06992 -0.07301 -0.02332 O5 4 0.565898 0.101023 0.151805 21.00000 0.15039 0.04571 = 0.12942 -0.03088 0.04592 -0.02529 PART 2 O4' 4 0.438677 0.083722 0.115234 -21.00000 0.05841 0.03931 = 0.06613 0.01832 0.01628 0.02254 O5' 4 0.627543 0.036802 0.186834 -21.00000 0.08240 0.06464 = 0.07217 0.02732 -0.05311 -0.05157 PART 0 CL1 5 0.575425 0.015080 0.108992 11.00000 0.05961 0.02903 = 0.03590 0.01369 -0.01342 -0.01183 C1 1 0.114795 0.211903 0.267376 11.00000 0.01723 0.02137 = 0.02164 0.00101 0.00209 0.00352 C2 1 0.053293 0.199680 0.342212 11.00000 0.02121 0.02854 = 0.01966 -0.00078 0.00305 0.00237 AFIX 43 H2 2 0.085499 0.238436 0.386210 11.00000 -1.20000 AFIX 0 C3 1 -0.054217 0.131440 0.352514 11.00000 0.02328 0.03331 = 0.02458 0.00156 0.00720 0.00165 AFIX 43 H3 2 -0.094430 0.122698 0.403514 11.00000 -1.20000 AFIX 0 C4 1 -0.102688 0.076006 0.287858 11.00000 0.01973 0.02882 = 0.03178 0.00534 0.00160 -0.00358 AFIX 43 H4 2 -0.176410 0.029406 0.294699 11.00000 -1.20000 AFIX 0 C5 1 -0.043732 0.088432 0.213109 11.00000 0.02208 0.02917 = 0.02536 -0.00168 -0.00189 -0.00205 AFIX 43 H5 2 -0.077738 0.050517 0.169126 11.00000 -1.20000 AFIX 0 C6 1 0.064163 0.155722 0.202505 11.00000 0.01905 0.02725 = 0.02135 0.00105 0.00049 0.00161 AFIX 43 H6 2 0.103980 0.163913 0.151345 11.00000 -1.20000 AFIX 0 C7 1 0.236372 0.275735 0.261686 11.00000 0.02036 0.02180 = 0.02189 -0.00207 -0.00166 0.00091 AFIX 43 H7 2 0.264525 0.309615 0.308932 11.00000 -1.20000 AFIX 0 C8 1 0.313665 0.291862 0.195882 11.00000 0.02241 0.02424 = 0.01742 -0.00253 -0.00111 -0.00120 AFIX 43 H8 2 0.283009 0.272065 0.144509 11.00000 -1.20000 AFIX 0 C9 1 0.442774 0.339812 0.207442 11.00000 0.02172 0.02055 = 0.01629 -0.00240 -0.00002 -0.00012 AFIX 43 H9 2 0.460985 0.367000 0.258772 11.00000 -1.20000 AFIX 0 C10 1 0.681617 0.381024 0.176082 11.00000 0.01689 0.01999 = 0.01852 0.00078 -0.00025 -0.00176 C11 1 0.689688 0.494668 0.194591 11.00000 0.02266 0.02140 = 0.02434 -0.00329 -0.00211 -0.00309 AFIX 137 H11A 2 0.783464 0.512344 0.210097 11.00000 -1.50000 H11B 2 0.627009 0.510946 0.238313 11.00000 -1.50000 H11C 2 0.663799 0.534028 0.147304 11.00000 -1.50000 AFIX 0 C12 1 0.731807 0.316350 0.245824 11.00000 0.02418 0.03087 = 0.02479 0.00384 -0.00386 0.00232 AFIX 137 H12A 2 0.709172 0.244318 0.236271 11.00000 -1.50000 H12B 2 0.687253 0.339441 0.294872 11.00000 -1.50000 H12C 2 0.831225 0.323762 0.251112 11.00000 -1.50000 AFIX 0 C13 1 0.898602 0.374029 0.092477 11.00000 0.01814 0.03645 = 0.03502 0.00006 0.00481 -0.00085 AFIX 137 H13A 2 0.926578 0.354849 0.038518 11.00000 -1.50000 H13B 2 0.950866 0.333881 0.131235 11.00000 -1.50000 H13C 2 0.916303 0.447063 0.100887 11.00000 -1.50000 AFIX 0 C14 1 0.674226 0.316233 0.044039 11.00000 0.02643 0.01628 = 0.01937 0.00201 0.00191 -0.00002 C15 1 0.525946 0.318290 0.069795 11.00000 0.02233 0.01950 = 0.01694 -0.00388 -0.00058 -0.00441 AFIX 13 H15 2 0.485737 0.248054 0.066217 11.00000 -1.20000 AFIX 0 C16 1 0.441819 0.393697 0.018584 11.00000 0.01874 0.03135 = 0.01875 0.00080 -0.00286 -0.00510 AFIX 23 H16A 2 0.441962 0.369079 -0.037108 11.00000 -1.20000 H16B 2 0.345835 0.393003 0.037481 11.00000 -1.20000 AFIX 0 C17 1 0.493064 0.502352 0.019831 11.00000 0.02182 0.02495 = 0.01916 0.00211 -0.00391 0.00356 C18 1 0.612953 0.530965 -0.020013 11.00000 0.02849 0.02266 = 0.02159 0.00198 0.00199 0.00092 AFIX 43 H18 2 0.660053 0.482066 -0.051636 11.00000 -1.20000 AFIX 0 C19 1 0.664171 0.630304 -0.013901 11.00000 0.04064 0.02756 = 0.02644 0.00566 -0.00096 -0.00581 AFIX 43 H19 2 0.746590 0.648327 -0.040426 11.00000 -1.20000 AFIX 0 C20 1 0.594611 0.702918 0.031001 11.00000 0.05677 0.01959 = 0.02873 0.00268 -0.01267 0.00289 AFIX 43 H20 2 0.629574 0.770502 0.035662 11.00000 -1.20000 AFIX 0 C21 1 0.474482 0.676167 0.068738 11.00000 0.04920 0.02961 = 0.03091 -0.00433 -0.00640 0.01795 AFIX 43 H21 2 0.425634 0.725943 0.098590 11.00000 -1.20000 AFIX 0 C22 1 0.424456 0.576862 0.063365 11.00000 0.02908 0.03925 = 0.02593 0.00144 0.00247 0.01175 AFIX 43 H22 2 0.341812 0.559555 0.089942 11.00000 -1.20000 AFIX 0 N1 3 0.537815 0.349763 0.154276 11.00000 0.01843 0.01835 = 0.01726 -0.00052 -0.00107 -0.00213 N2 3 0.753034 0.353661 0.102568 11.00000 0.01973 0.01993 = 0.02230 -0.00201 0.00422 -0.00021 O1 4 0.713436 0.288916 -0.022240 11.00000 0.03437 0.02630 = 0.02004 -0.00278 0.00668 0.00307 HKLF 4 Covalent radii and connectivity table for 2007src1354 in P2(1)2(1)2(1) C 0.770 H 0.320 N 0.700 O 0.660 CL 0.990 O2 - Cl1 O3 - Cl1 O4_a - Cl1 O5_a - Cl1 O4'_b - Cl1 O5'_b - Cl1 Cl1 - O5_a O3 O2 O5'_b O4_a O4'_b C1 - C2 C6 C7 C2 - C3 C1 C3 - C2 C4 C4 - C3 C5 C5 - C6 C4 C6 - C5 C1 C7 - C8 C1 C8 - C7 C9 C9 - N1 C8 C10 - N2 N1 C11 C12 C11 - C10 C12 - C10 C13 - N2 C14 - O1 N2 C15 C15 - N1 C14 C16 C16 - C17 C15 C17 - C22 C18 C16 C18 - C19 C17 C19 - C20 C18 C20 - C21 C19 C21 - C20 C22 C22 - C21 C17 N1 - C9 C15 C10 N2 - C14 C13 C10 O1 - C14 20568 Reflections read, of which 92 rejected -12 =< h =< 12, -16 =< k =< 16, -21 =< l =< 21, Max. 2-theta = 54.98 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 4 10 11 4.44 0.25 3 1.39 0 10 15 9.07 0.51 2 2.67 2 Inconsistent equivalents 4898 Unique reflections, of which 0 suppressed R(int) = 0.0487 R(sigma) = 0.0419 Friedel opposites not merged Maximum memory for data reduction = 2707 / 48223 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 = 3498 / 367120 wR2 = 0.1052 before cycle 1 for 4898 data and 293 / 293 parameters GooF = S = 1.037; Restrained GooF = 1.037 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0539 * P )^2 + 0.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.26424 0.00045 -0.483 OSF 2 0.58536 0.00619 0.239 FVAR 2 Mean shift/esd = 0.066 Maximum = -0.483 for OSF Max. shift = 0.002 A for H12B Max. dU =-0.001 for O5'_b Least-squares cycle 2 Maximum vector length = 511 Memory required = 3498 / 367120 wR2 = 0.1051 before cycle 2 for 4898 data and 293 / 293 parameters GooF = S = 1.038; Restrained GooF = 1.038 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0539 * P )^2 + 0.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.26416 0.00045 -0.185 OSF 2 0.58552 0.00618 0.026 FVAR 2 Mean shift/esd = 0.022 Maximum = -0.185 for OSF Max. shift = 0.001 A for H13A Max. dU = 0.000 for O4_a Least-squares cycle 3 Maximum vector length = 511 Memory required = 3498 / 367120 wR2 = 0.1051 before cycle 3 for 4898 data and 293 / 293 parameters GooF = S = 1.038; Restrained GooF = 1.038 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0539 * P )^2 + 0.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.26416 0.00045 0.000 OSF 2 0.58550 0.00617 -0.003 FVAR 2 Mean shift/esd = 0.002 Maximum = 0.025 for U23 O5'_b Max. shift = 0.000 A for H13C Max. dU = 0.000 for O5'_b Least-squares cycle 4 Maximum vector length = 511 Memory required = 3498 / 367120 wR2 = 0.1051 before cycle 4 for 4898 data and 293 / 293 parameters GooF = S = 1.038; Restrained GooF = 1.038 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0539 * P )^2 + 0.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.26416 0.00045 0.001 OSF 2 0.58548 0.00617 -0.003 FVAR 2 Mean shift/esd = 0.001 Maximum = -0.013 for tors H13A Max. shift = 0.000 A for H13C Max. dU = 0.000 for O5'_b Largest correlation matrix elements 0.646 U23 O4_a / U33 O4_a -0.585 U22 O5'_b / FVAR 2 -0.512 U13 O5'_b / U33 O5'_b -0.635 U13 O4_a / U33 O4_a 0.541 z O4_a / y O4_a -0.508 z O4_a / x O4_a 0.629 U23 O4_a / U22 O4_a -0.540 y O5'_b / x O5'_b 0.504 U13 O5_a / U11 O5_a -0.619 U12 O5'_b / U22 O5'_b -0.538 U12 O4_a / U23 O4_a 0.500 U23 O2 / U22 O2 -0.589 U13 O4_a / U11 O4_a 0.538 U12 O4_a / U13 O4_a -0.588 U12 O5'_b / U11 O5'_b -0.534 U13 O5'_b / U11 O5'_b Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.0855 0.2384 0.3862 43 0.950 0.000 C2 C3 C1 H3 -0.0945 0.1227 0.4035 43 0.950 0.000 C3 C2 C4 H4 -0.1764 0.0294 0.2947 43 0.950 0.000 C4 C3 C5 H5 -0.0777 0.0505 0.1691 43 0.950 0.000 C5 C6 C4 H6 0.1040 0.1640 0.1513 43 0.950 0.000 C6 C5 C1 H7 0.2645 0.3096 0.3089 43 0.950 0.000 C7 C8 C1 H8 0.2830 0.2721 0.1445 43 0.950 0.000 C8 C7 C9 H9 0.4610 0.3670 0.2588 43 0.950 0.000 C9 N1 C8 H11A 0.7835 0.5123 0.2101 137 0.980 0.000 C11 C10 H11A H11B 0.6270 0.5110 0.2383 137 0.980 0.000 C11 C10 H11A H11C 0.6639 0.5340 0.1473 137 0.980 0.000 C11 C10 H11A H12A 0.7093 0.2443 0.2362 137 0.980 0.000 C12 C10 H12A H12B 0.6870 0.3393 0.2949 137 0.980 0.000 C12 C10 H12A H12C 0.8312 0.3239 0.2512 137 0.980 0.000 C12 C10 H12A H13A 0.9266 0.3547 0.0385 137 0.980 0.000 C13 N2 H13A H13B 0.9509 0.3340 0.1313 137 0.980 0.000 C13 N2 H13A H13C 0.9163 0.4471 0.1008 137 0.980 0.000 C13 N2 H13A H15 0.4857 0.2481 0.0662 13 1.000 0.000 C15 N1 C14 C16 H16A 0.4419 0.3691 -0.0371 23 0.990 0.000 C16 C17 C15 H16B 0.3458 0.3930 0.0375 23 0.990 0.000 C16 C17 C15 H18 0.6601 0.4820 -0.0516 43 0.950 0.000 C18 C19 C17 H19 0.7465 0.6483 -0.0405 43 0.950 0.000 C19 C20 C18 H20 0.6296 0.7705 0.0357 43 0.950 0.000 C20 C21 C19 H21 0.4256 0.7259 0.0986 43 0.950 0.000 C21 C20 C22 H22 0.3418 0.5596 0.0899 43 0.950 0.000 C22 C21 C17 2007src1354 in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq O2 0.61731 0.04231 0.03264 1.00000 0.06167 0.15795 0.08455 0.06789 0.02843 -0.00445 0.10139 0.00589 0.00027 0.00026 0.00016 0.00000 0.00152 0.00270 0.00172 0.00180 0.00134 0.00165 0.00104 O3 0.48745 -0.06810 0.11211 1.00000 0.09475 0.08009 0.04255 0.00203 -0.00252 -0.05135 0.07246 0.00348 0.00027 0.00018 0.00012 0.00000 0.00172 0.00150 0.00106 0.00104 0.00112 0.00135 0.00071 O4_a 0.70605 -0.03712 0.13315 0.58548 0.06122 0.05756 0.17413 0.06953 -0.07290 -0.02290 0.09764 0.00800 0.00044 0.00033 0.00036 0.00617 0.00271 0.00264 0.00581 0.00325 0.00322 0.00201 0.00259 O5_a 0.56590 0.10102 0.15185 0.58548 0.15109 0.04553 0.13042 -0.03162 0.04623 -0.02574 0.10901 0.01049 0.00076 0.00034 0.00037 0.00617 0.00633 0.00234 0.00489 0.00278 0.00478 0.00326 0.00276 O4'_b 0.43869 0.08368 0.11519 0.41452 0.05812 0.03912 0.06554 0.01836 0.01628 0.02284 0.05426 0.01081 0.00056 0.00034 0.00031 0.00617 0.00336 0.00247 0.00315 0.00210 0.00271 0.00227 0.00179 O5'_b 0.62767 0.03670 0.18683 0.41452 0.08190 0.06392 0.07178 0.02728 -0.05335 -0.05119 0.07253 0.00750 0.00068 0.00048 0.00033 0.00617 0.00439 0.00443 0.00345 0.00294 0.00320 0.00353 0.00252 Cl1 0.57542 0.01509 0.10899 1.00000 0.05954 0.02897 0.03577 0.01364 -0.01338 -0.01180 0.04143 0.00097 0.00007 0.00004 0.00003 0.00000 0.00038 0.00025 0.00027 0.00021 0.00026 0.00025 0.00016 C1 0.11480 0.21191 0.26738 1.00000 0.01712 0.02131 0.02157 0.00096 0.00205 0.00350 0.02000 0.00319 0.00018 0.00014 0.00011 0.00000 0.00083 0.00084 0.00084 0.00070 0.00070 0.00068 0.00036 C2 0.05330 0.19968 0.34222 1.00000 0.02114 0.02854 0.01954 -0.00078 0.00302 0.00232 0.02307 0.00339 0.00020 0.00014 0.00011 0.00000 0.00093 0.00091 0.00083 0.00071 0.00073 0.00077 0.00038 H2 0.08551 0.23842 0.38622 1.00000 0.02769 0.00000 0.00000 C3 -0.05421 0.13146 0.35250 1.00000 0.02314 0.03316 0.02450 0.00160 0.00722 0.00167 0.02693 0.00357 0.00021 0.00015 0.00012 0.00000 0.00099 0.00102 0.00091 0.00080 0.00078 0.00082 0.00042 H3 -0.09445 0.12274 0.40349 1.00000 0.03232 0.00000 0.00000 C4 -0.10267 0.07601 0.28788 1.00000 0.01969 0.02864 0.03168 0.00525 0.00165 -0.00352 0.02667 0.00347 0.00020 0.00015 0.00012 0.00000 0.00091 0.00096 0.00102 0.00079 0.00078 0.00076 0.00041 H4 -0.17637 0.02940 0.29474 1.00000 0.03200 0.00000 0.00000 C5 -0.04373 0.08842 0.21310 1.00000 0.02206 0.02917 0.02517 -0.00163 -0.00187 -0.00212 0.02547 0.00334 0.00020 0.00015 0.00012 0.00000 0.00093 0.00093 0.00092 0.00075 0.00075 0.00076 0.00040 H5 -0.07772 0.05049 0.16912 1.00000 0.03056 0.00000 0.00000 C6 0.06416 0.15575 0.20250 1.00000 0.01897 0.02701 0.02123 0.00102 0.00040 0.00160 0.02241 0.00322 0.00019 0.00014 0.00011 0.00000 0.00087 0.00088 0.00084 0.00072 0.00072 0.00073 0.00037 H6 0.10395 0.16397 0.15134 1.00000 0.02689 0.00000 0.00000 C7 0.23636 0.27574 0.26168 1.00000 0.02029 0.02168 0.02176 -0.00209 -0.00164 0.00091 0.02124 0.00318 0.00019 0.00014 0.00011 0.00000 0.00089 0.00083 0.00086 0.00072 0.00070 0.00071 0.00037 H7 0.26451 0.30962 0.30893 1.00000 0.02549 0.00000 0.00000 C8 0.31366 0.29187 0.19589 1.00000 0.02225 0.02412 0.01737 -0.00244 -0.00115 -0.00126 0.02124 0.00316 0.00019 0.00014 0.00011 0.00000 0.00091 0.00089 0.00081 0.00070 0.00070 0.00073 0.00036 H8 0.28301 0.27208 0.14452 1.00000 0.02549 0.00000 0.00000 C9 0.44275 0.33980 0.20745 1.00000 0.02165 0.02044 0.01624 -0.00238 0.00003 -0.00012 0.01945 0.00301 0.00019 0.00013 0.00010 0.00000 0.00089 0.00079 0.00077 0.00065 0.00069 0.00070 0.00035 H9 0.46096 0.36697 0.25879 1.00000 0.02333 0.00000 0.00000 C10 0.68159 0.38102 0.17608 1.00000 0.01687 0.01995 0.01843 0.00078 -0.00020 -0.00178 0.01842 0.00305 0.00019 0.00014 0.00010 0.00000 0.00086 0.00083 0.00082 0.00067 0.00067 0.00067 0.00036 C11 0.68970 0.49468 0.19458 1.00000 0.02266 0.02140 0.02415 -0.00330 -0.00211 -0.00318 0.02274 0.00309 0.00020 0.00014 0.00011 0.00000 0.00089 0.00087 0.00085 0.00074 0.00073 0.00072 0.00037 H11A 0.78346 0.51232 0.21014 1.00000 0.03410 0.00000 0.00000 H11B 0.62696 0.51099 0.23826 1.00000 0.03410 0.00000 0.00000 H11C 0.66392 0.53404 0.14727 1.00000 0.03410 0.00000 0.00000 C12 0.73177 0.31634 0.24584 1.00000 0.02418 0.03083 0.02473 0.00388 -0.00385 0.00231 0.02658 0.00354 0.00021 0.00015 0.00011 0.00000 0.00098 0.00098 0.00096 0.00081 0.00076 0.00078 0.00042 H12A 0.70934 0.24428 0.23622 1.00000 0.03987 0.00000 0.00000 H12B 0.68703 0.33932 0.29486 1.00000 0.03987 0.00000 0.00000 H12C 0.83116 0.32389 0.25122 1.00000 0.03987 0.00000 0.00000 C13 0.89864 0.37401 0.09247 1.00000 0.01813 0.03627 0.03504 0.00011 0.00486 -0.00082 0.02982 0.00369 0.00020 0.00017 0.00013 0.00000 0.00097 0.00105 0.00107 0.00087 0.00081 0.00080 0.00044 H13A 0.92664 0.35469 0.03854 1.00000 0.04472 0.00000 0.00000 H13B 0.95089 0.33396 0.13129 1.00000 0.04472 0.00000 0.00000 H13C 0.91633 0.44706 0.10077 1.00000 0.04472 0.00000 0.00000 C14 0.67420 0.31622 0.04404 1.00000 0.02632 0.01613 0.01939 0.00199 0.00184 0.00000 0.02061 0.00316 0.00020 0.00013 0.00010 0.00000 0.00095 0.00079 0.00087 0.00068 0.00074 0.00068 0.00037 C15 0.52595 0.31830 0.06978 1.00000 0.02224 0.01937 0.01678 -0.00384 -0.00052 -0.00434 0.01946 0.00301 0.00019 0.00013 0.00011 0.00000 0.00092 0.00081 0.00079 0.00065 0.00068 0.00067 0.00036 H15 0.48574 0.24806 0.06621 1.00000 0.02335 0.00000 0.00000 C16 0.44181 0.39368 0.01860 1.00000 0.01878 0.03124 0.01869 0.00071 -0.00287 -0.00509 0.02290 0.00311 0.00019 0.00014 0.00011 0.00000 0.00088 0.00094 0.00079 0.00072 0.00071 0.00074 0.00037 H16A 0.44192 0.36906 -0.03710 1.00000 0.02748 0.00000 0.00000 H16B 0.34584 0.39299 0.03751 1.00000 0.02748 0.00000 0.00000 C17 0.49308 0.50235 0.01983 1.00000 0.02185 0.02478 0.01899 0.00217 -0.00395 0.00353 0.02187 0.00316 0.00018 0.00015 0.00011 0.00000 0.00089 0.00089 0.00078 0.00073 0.00069 0.00072 0.00037 C18 0.61296 0.53096 -0.01999 1.00000 0.02840 0.02245 0.02155 0.00196 0.00189 0.00095 0.02413 0.00328 0.00021 0.00014 0.00011 0.00000 0.00100 0.00090 0.00085 0.00074 0.00077 0.00073 0.00039 H18 0.66010 0.48205 -0.05158 1.00000 0.02896 0.00000 0.00000 C19 0.66413 0.63030 -0.01392 1.00000 0.04056 0.02744 0.02632 0.00572 -0.00097 -0.00575 0.03144 0.00373 0.00025 0.00016 0.00012 0.00000 0.00123 0.00099 0.00096 0.00081 0.00089 0.00087 0.00046 H19 0.74650 0.64833 -0.04050 1.00000 0.03773 0.00000 0.00000 C20 0.59464 0.70292 0.03100 1.00000 0.05667 0.01946 0.02870 0.00262 -0.01259 0.00286 0.03495 0.00376 0.00027 0.00015 0.00012 0.00000 0.00147 0.00089 0.00102 0.00078 0.00102 0.00093 0.00051 H20 0.62962 0.77050 0.03567 1.00000 0.04194 0.00000 0.00000 C21 0.47446 0.67614 0.06875 1.00000 0.04908 0.02963 0.03080 -0.00434 -0.00644 0.01801 0.03650 0.00409 0.00026 0.00017 0.00013 0.00000 0.00142 0.00105 0.00104 0.00085 0.00100 0.00097 0.00052 H21 0.42561 0.72591 0.09861 1.00000 0.04381 0.00000 0.00000 C22 0.42444 0.57691 0.06338 1.00000 0.02902 0.03907 0.02584 0.00146 0.00247 0.01176 0.03131 0.00383 0.00023 0.00016 0.00012 0.00000 0.00105 0.00111 0.00094 0.00083 0.00086 0.00090 0.00045 H22 0.34178 0.55962 0.08994 1.00000 0.03758 0.00000 0.00000 N1 0.53782 0.34978 0.15427 1.00000 0.01834 0.01826 0.01711 -0.00053 -0.00094 -0.00210 0.01790 0.00256 0.00016 0.00011 0.00009 0.00000 0.00076 0.00066 0.00068 0.00056 0.00057 0.00059 0.00030 N2 0.75301 0.35365 0.10258 1.00000 0.01960 0.01979 0.02217 -0.00202 0.00420 -0.00028 0.02052 0.00267 0.00016 0.00011 0.00009 0.00000 0.00078 0.00073 0.00075 0.00063 0.00062 0.00060 0.00032 O1 0.71343 0.28891 -0.02224 1.00000 0.03427 0.02626 0.01999 -0.00276 0.00668 0.00302 0.02684 0.00241 0.00015 0.00010 0.00008 0.00000 0.00077 0.00068 0.00064 0.00054 0.00057 0.00057 0.00031 Final Structure Factor Calculation for 2007src1354 in P2(1)2(1)2(1) Total number of l.s. parameters = 293 Maximum vector length = 511 Memory required = 3207 / 26068 wR2 = 0.1051 before cycle 5 for 4898 data and 2 / 293 parameters GooF = S = 1.038; Restrained GooF = 1.038 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0539 * P )^2 + 0.64 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0418 for 4406 Fo > 4sig(Fo) and 0.0490 for all 4898 data wR2 = 0.1051, GooF = S = 1.038, Restrained GooF = 1.038 for all data Flack x parameter = -0.0398 with esd 0.0591 Expected values are 0 (within 3 esd'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 = 30.00 for non-hydrogen and 25.00 for hydrogen atoms Principal mean square atomic displacements U 0.1993 0.0804 0.0245 O2 0.1394 0.0424 0.0355 O3 0.2389 0.0365 0.0175 O4_a may be split into 0.6970 -0.0307 0.1444 and 0.7151 -0.0435 0.1219 0.1986 0.0945 0.0340 O5_a 0.0937 0.0464 0.0227 O4'_b 0.1629 0.0405 0.0142 O5'_b 0.0720 0.0340 0.0183 Cl1 0.0245 0.0206 0.0149 C1 0.0292 0.0232 0.0169 C2 0.0347 0.0296 0.0166 C3 0.0357 0.0267 0.0176 C4 0.0300 0.0260 0.0204 C5 0.0275 0.0211 0.0186 C6 0.0246 0.0200 0.0191 C7 0.0252 0.0224 0.0162 C8 0.0217 0.0214 0.0152 C9 0.0210 0.0182 0.0160 C10 0.0263 0.0251 0.0167 C11 0.0327 0.0280 0.0190 C12 0.0364 0.0362 0.0168 C13 0.0268 0.0199 0.0151 C14 0.0258 0.0196 0.0129 C15 0.0332 0.0203 0.0152 C16 0.0272 0.0237 0.0147 C17 0.0292 0.0233 0.0199 C18 0.0433 0.0305 0.0206 C19 0.0616 0.0258 0.0175 C20 0.0618 0.0289 0.0189 C21 0.0472 0.0259 0.0209 C22 0.0204 0.0178 0.0155 N1 0.0258 0.0195 0.0162 N2 0.0372 0.0273 0.0160 O1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.030 0.044 0.059 0.072 0.086 0.104 0.128 0.162 0.226 1.000 Number in group 499. 485. 533. 479. 456. 503. 496. 469. 484. 494. GooF 1.000 1.099 1.089 1.060 1.049 0.968 1.092 1.014 0.991 1.003 K 1.113 1.029 0.984 0.994 0.989 1.001 0.999 1.006 1.016 0.982 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.31 1.62 inf Number in group 505. 484. 495. 476. 498. 482. 493. 491. 481. 493. GooF 0.969 0.958 1.009 1.010 0.974 0.977 0.967 0.925 1.158 1.356 K 0.982 0.986 0.987 0.999 1.005 1.012 1.027 1.019 1.022 0.964 R1 0.108 0.102 0.085 0.072 0.051 0.040 0.035 0.030 0.032 0.034 Recommended weighting scheme: WGHT 0.0522 0.6734 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 5 3 271.00 183.89 4.90 0.112 2.13 1 0 7 13.78 1.84 4.72 0.011 2.33 -5 1 4 151.39 98.36 4.25 0.082 1.76 4 3 0 174.81 118.14 4.16 0.090 2.13 2 5 3 271.92 198.52 4.07 0.117 2.13 0 2 2 2204.13 2863.74 4.03 0.443 5.16 7 0 3 39.98 14.50 3.99 0.032 1.35 4 2 13 42.50 20.38 3.99 0.037 1.13 0 7 6 159.97 110.41 3.91 0.087 1.55 -4 1 7 11.60 29.32 3.79 0.045 1.70 5 8 0 148.43 102.60 3.76 0.084 1.25 0 4 9 1015.66 803.74 3.71 0.235 1.62 2 8 0 18.46 6.56 3.68 0.021 1.55 -4 2 13 41.16 19.43 3.63 0.036 1.13 -3 1 11 248.74 185.45 3.62 0.113 1.38 -1 1 2 2011.41 2524.40 3.54 0.416 5.73 0 3 10 16.07 4.47 3.53 0.018 1.57 10 0 8 86.69 49.96 3.52 0.059 0.89 3 5 0 789.69 641.35 3.25 0.210 2.04 -3 1 1 16.80 33.47 3.25 0.048 3.11 0 2 1 118.62 170.64 3.22 0.108 6.09 0 7 5 86.37 121.62 3.19 0.091 1.63 6 3 0 197.71 261.69 3.13 0.134 1.52 0 1 3 912.48 1129.63 3.05 0.278 5.15 -9 1 5 225.71 172.36 3.04 0.109 1.03 4 1 7 19.26 35.14 3.04 0.049 1.70 -3 14 7 32.64 15.08 2.99 0.032 0.84 1 4 6 451.48 367.07 2.99 0.159 2.08 3 3 19 8.80 30.91 2.97 0.046 0.84 3 16 4 33.39 71.08 2.96 0.070 0.78 -3 2 11 530.06 432.03 2.93 0.172 1.35 1 15 10 7.45 32.90 2.92 0.047 0.77 5 1 4 132.88 99.19 2.91 0.082 1.76 0 6 4 116.66 154.53 2.90 0.103 1.93 11 0 7 233.67 173.17 2.89 0.109 0.83 3 6 2 302.26 375.46 2.88 0.160 1.77 3 3 16 24.44 11.49 2.86 0.028 0.97 5 14 3 205.46 317.82 2.83 0.148 0.83 9 1 5 223.19 172.28 2.81 0.109 1.03 3 11 14 45.74 19.16 2.79 0.036 0.82 3 0 2 506.54 629.51 2.77 0.208 3.04 5 12 4 6.16 16.34 2.77 0.033 0.93 11 3 5 50.60 86.26 2.77 0.077 0.84 6 2 16 44.01 68.76 2.76 0.069 0.87 1 1 2 2111.84 2536.94 2.76 0.417 5.73 0 5 17 19.62 35.96 2.75 0.050 0.92 -9 8 9 62.90 31.90 2.74 0.047 0.81 -4 6 19 11.03 43.40 2.72 0.055 0.78 7 1 8 191.15 242.15 2.72 0.129 1.16 -10 2 2 11.19 31.17 2.69 0.046 0.96 Bond lengths and angles O2 - Distance Angles Cl1 1.3934 (0.0022) O2 - O3 - Distance Angles Cl1 1.3865 (0.0020) O3 - O4_a - Distance Angles Cl1 1.5028 (0.0038) O4_a - O5_a - Distance Angles Cl1 1.3373 (0.0041) O5_a - O4'_b - Distance Angles Cl1 1.6118 (0.0043) O4'_b - O5'_b - Distance Angles Cl1 1.4327 (0.0048) O5'_b - Cl1 - Distance Angles O5_a 1.3373 (0.0041) O3 1.3865 (0.0020) 126.49 (0.28) O2 1.3934 (0.0022) 107.61 (0.29) 114.63 (0.17) O5'_b 1.4327 (0.0048) 50.74 (0.38) 109.93 (0.21) 133.35 (0.25) O4_a 1.5028 (0.0038) 107.13 (0.40) 99.22 (0.18) 96.63 (0.26) 62.62 (0.34) O4'_b 1.6118 (0.0043) 56.00 (0.34) 85.40 (0.23) 99.26 (0.20) 97.27 (0.38) 159.80 (0.32) Cl1 - O5_a O3 O2 O5'_b O4_a C1 - Distance Angles C2 1.4034 (0.0024) C6 1.4045 (0.0026) 119.08 (0.17) C7 1.4542 (0.0025) 118.29 (0.17) 122.41 (0.17) C1 - C2 C6 C2 - Distance Angles C3 1.3883 (0.0027) C1 1.4034 (0.0025) 120.57 (0.17) C2 - C3 C3 - Distance Angles C2 1.3883 (0.0027) C4 1.3889 (0.0029) 119.69 (0.18) C3 - C2 C4 - Distance Angles C3 1.3889 (0.0029) C5 1.3922 (0.0027) 120.30 (0.18) C4 - C3 C5 - Distance Angles C6 1.3842 (0.0026) C4 1.3922 (0.0027) 120.34 (0.18) C5 - C6 C6 - Distance Angles C5 1.3842 (0.0026) C1 1.4045 (0.0026) 120.01 (0.17) C6 - C5 C7 - Distance Angles C8 1.3557 (0.0026) C1 1.4542 (0.0025) 126.70 (0.17) C7 - C8 C8 - Distance Angles C7 1.3557 (0.0026) C9 1.4213 (0.0025) 116.81 (0.16) C8 - C7 C9 - Distance Angles N1 1.2957 (0.0023) C8 1.4213 (0.0025) 125.86 (0.16) C9 - N1 C10 - Distance Angles N2 1.4634 (0.0023) N1 1.5078 (0.0023) 99.93 (0.13) C11 1.5192 (0.0025) 112.76 (0.15) 111.28 (0.15) C12 1.5264 (0.0025) 111.13 (0.15) 109.64 (0.15) 111.54 (0.15) C10 - N2 N1 C11 C11 - Distance Angles C10 1.5192 (0.0025) C11 - C12 - Distance Angles C10 1.5264 (0.0025) C12 - C13 - Distance Angles N2 1.4572 (0.0024) C13 - C14 - Distance Angles O1 1.2311 (0.0022) N2 1.3418 (0.0025) 126.22 (0.18) C15 1.5116 (0.0027) 124.23 (0.17) 109.46 (0.15) C14 - O1 N2 C15 - Distance Angles N1 1.4833 (0.0022) C14 1.5116 (0.0027) 101.79 (0.14) C16 1.5447 (0.0025) 113.46 (0.15) 111.20 (0.15) C15 - N1 C14 C16 - Distance Angles C17 1.5056 (0.0026) C15 1.5447 (0.0025) 114.62 (0.15) C16 - C17 C17 - Distance Angles C22 1.3909 (0.0027) C18 1.3998 (0.0027) 117.90 (0.18) C16 1.5056 (0.0026) 120.49 (0.17) 121.57 (0.17) C17 - C22 C18 C18 - Distance Angles C19 1.3946 (0.0027) C17 1.3998 (0.0027) 120.89 (0.19) C18 - C19 C19 - Distance Angles C20 1.3897 (0.0032) C18 1.3946 (0.0027) 120.01 (0.21) C19 - C20 C20 - Distance Angles C21 1.3796 (0.0036) C19 1.3897 (0.0032) 119.50 (0.19) C20 - C21 C21 - Distance Angles C20 1.3796 (0.0036) C22 1.3884 (0.0031) 120.42 (0.20) C21 - C20 C22 - Distance Angles C21 1.3884 (0.0031) C17 1.3909 (0.0027) 121.24 (0.20) C22 - C21 N1 - Distance Angles C9 1.2957 (0.0023) C15 1.4833 (0.0022) 125.23 (0.15) C10 1.5078 (0.0023) 121.80 (0.15) 112.38 (0.14) N1 - C9 C15 N2 - Distance Angles C14 1.3418 (0.0025) C13 1.4572 (0.0024) 122.76 (0.16) C10 1.4634 (0.0023) 115.78 (0.15) 121.28 (0.15) N2 - C14 C13 O1 - Distance Angles C14 1.2311 (0.0022) O1 - FMAP and GRID set by program FMAP 2 3 21 GRID -1.389 -2 -2 1.389 2 2 R1 = 0.0459 for 2773 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.38 at 0.5740 0.9184 0.1107 [ 0.86 A from O3 ] Deepest hole -0.46 at 0.6018 0.9789 0.0823 [ 0.70 A from CL1 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 3118 / 22752 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5740 -0.0816 0.1107 1.00000 0.05 0.38 0.86 O3 1.26 CL1 1.46 O4 2.07 O5' Q2 1 0.6689 0.0855 0.0735 1.00000 0.05 0.26 1.02 O2 1.43 CL1 1.67 O5 1.92 O4 Q3 1 0.7407 -0.0548 0.1348 1.00000 0.05 0.22 0.41 O4 1.85 O5' 1.90 CL1 2.01 H7 Q4 1 0.6814 0.0001 0.1627 1.00000 0.05 0.22 0.74 O4 0.82 O5' 1.39 CL1 1.75 O5 Q5 1 0.7260 -0.0295 0.0920 1.00000 0.05 0.21 0.72 O4 1.61 CL1 1.73 O2 2.05 O5' Q6 1 0.1009 0.1830 0.3050 1.00000 0.05 0.19 0.75 C1 0.81 C2 1.55 H2 1.80 C6 Q7 1 0.6171 0.3634 0.1716 1.00000 0.05 0.18 0.68 C10 0.85 N1 1.77 N2 1.79 C12 Q8 1 0.2967 0.2303 0.1403 1.00000 0.05 0.17 0.57 H8 1.24 C8 2.08 H6 2.16 O1 Q9 1 0.6401 0.0357 0.2177 1.00000 0.05 0.16 0.53 O5' 1.57 O5 1.83 O4 1.95 CL1 Q10 1 0.8083 0.2188 0.1547 1.00000 0.05 0.16 1.71 H12A 2.04 N2 2.09 H13B 2.13 C12 Q11 1 0.0257 0.2215 0.0820 1.00000 0.05 0.16 1.58 H6 1.62 H16A 1.84 H13B 2.10 O1 Q12 1 0.5926 0.3169 0.0627 1.00000 0.05 0.15 0.66 C15 0.86 C14 1.38 H15 1.69 N1 Q13 1 0.5799 0.2628 -0.0278 1.00000 0.05 0.15 1.35 O1 1.67 C14 1.84 H15 1.87 C15 Q14 1 0.7016 0.3600 0.2083 1.00000 0.05 0.15 0.64 C10 0.90 C12 1.49 H12B 1.53 H12C Q15 1 0.4698 -0.0993 0.1153 1.00000 0.05 0.15 0.45 O3 1.82 CL1 2.27 H9 2.30 H12B Q16 1 0.7117 0.4981 0.3329 1.00000 0.05 0.15 1.80 H11B 2.04 O4' 2.18 H12B 2.19 H11A Q17 1 0.4482 -0.0313 0.0810 1.00000 0.05 0.15 0.81 O3 1.46 CL1 1.61 O4' 2.08 O2 Q18 1 0.7251 0.3629 0.1268 1.00000 0.05 0.15 0.51 N2 0.96 C10 1.60 C14 1.80 C13 Q19 1 0.4549 -0.0216 0.0991 1.00000 0.05 0.14 0.72 O3 1.28 CL1 1.41 O4' 2.11 O2 Q20 1 0.6692 -0.0811 0.1495 1.00000 0.05 0.14 0.73 O4 1.70 CL1 1.71 O5' 1.72 H7 Shortest distances between peaks (including symmetry equivalents) 17 19 0.34 3 5 0.80 3 20 0.82 7 14 1.03 3 4 1.03 1 15 1.05 15 19 1.06 11 13 1.07 15 17 1.08 4 20 1.09 4 9 1.11 1 20 1.14 7 18 1.30 5 20 1.30 4 5 1.32 14 18 1.39 1 19 1.42 1 17 1.48 2 5 1.63 1 5 1.66 12 13 1.68 1 3 1.71 1 4 1.73 12 18 1.79 2 4 1.87 9 20 1.93 7 12 1.94 16 19 2.00 15 20 2.04 3 9 2.08 10 18 2.10 16 17 2.16 2 3 2.22 10 14 2.30 15 16 2.35 19 20 2.39 5 9 2.43 1 9 2.45 10 11 2.45 1 2 2.45 4 19 2.47 2 20 2.52 2 9 2.53 17 20 2.53 2 19 2.55 4 15 2.57 11 12 2.57 2 10 2.60 2 17 2.64 5 19 2.65 7 10 2.67 5 15 2.69 4 17 2.69 5 17 2.72 12 14 2.73 3 15 2.73 14 16 2.77 9 19 2.79 8 11 2.83 8 13 2.84 3 19 2.89 10 12 2.91 9 15 2.97 Time profile in seconds ----------------------- 0.07: Read and process instructions 0.00: Fit rigid groups 0.01: Interpret restraints etc. 0.01: 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. 3.55: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.01: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 3.99: Structure factors and derivatives 4.25: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.01: Apply other restraints 0.52: Solve l.s. equations 0.00: Generate HTAB table 0.04: Other dependent quantities, CIF, tables 0.11: Analysis of variance 0.07: Merge reflections for Fourier and .fcf 0.05: Fourier summations 0.05: Peaksearch 0.01: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src1354 finished at 10:49:43 Total CPU time: 12.8 secs + 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