+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2005src1012 started at 17:39:35 on 09-Aug-2005 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2005src1012 in P2(1)/c CELL 0.71073 11.5255 14.0330 14.1939 90.000 113.615 90.000 ZERR 4.00 0.0006 0.0007 0.0005 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N CL TI UNIT 88 72 16 8 4 V = 2103.44 F(000) = 936.0 Mu = 0.68 mm-1 Cell Wt = 1828.82 Rho = 1.444 MERG 2 OMIT -3.00 55.00 OMIT -1 0 2 OMIT -6 6 9 OMIT -5 4 15 FMAP 2 PLAN 20 SIZE 0.01 0.04 0.34 ACTA BOND WGHT 0.02170 3.06250 L.S. 4 TEMP -153.00 FVAR 0.44722 C1 1 0.619642 0.756187 -0.175725 11.00000 0.02129 0.03039 = 0.02161 -0.00086 0.00899 0.00032 AFIX 43 H1 2 0.576372 0.697586 -0.199100 11.00000 -1.20000 AFIX 0 C2 1 0.575355 0.844370 -0.219198 11.00000 0.02551 0.03963 = 0.02357 0.00435 0.00891 0.00760 AFIX 43 H2 2 0.498278 0.856660 -0.276573 11.00000 -1.20000 AFIX 0 C3 1 0.665862 0.911970 -0.162449 11.00000 0.02954 0.02415 = 0.02648 0.00716 0.01207 0.00677 AFIX 43 H3 2 0.662168 0.978821 -0.173836 11.00000 -1.20000 AFIX 0 C4 1 0.761931 0.862051 -0.086358 11.00000 0.02493 0.02290 = 0.02045 0.00297 0.01228 0.00277 C5 1 0.877397 0.886748 -0.006696 11.00000 0.02574 0.01812 = 0.02506 0.00006 0.01394 0.00192 AFIX 43 H5 2 0.903038 0.951473 0.006211 11.00000 -1.20000 AFIX 0 C6 1 1.063684 0.843012 0.133363 11.00000 0.02096 0.02141 = 0.02103 -0.00033 0.00705 -0.00413 C7 1 1.063457 0.907045 0.207925 11.00000 0.02850 0.02372 = 0.02688 -0.00087 0.01078 -0.00121 AFIX 43 H7 2 0.986416 0.935822 0.202480 11.00000 -1.20000 AFIX 0 C8 1 1.175254 0.928886 0.289997 11.00000 0.04001 0.02631 = 0.02435 -0.00366 0.00834 -0.00949 AFIX 43 H8 2 1.174933 0.973092 0.340582 11.00000 -1.20000 AFIX 0 C9 1 1.287464 0.886784 0.298875 11.00000 0.02876 0.02803 = 0.03065 0.00587 -0.00215 -0.00662 AFIX 43 H9 2 1.364192 0.901256 0.355710 11.00000 -1.20000 AFIX 0 C10 1 1.286979 0.823102 0.223894 11.00000 0.02032 0.02872 = 0.05120 0.00812 0.01047 0.00064 AFIX 43 H10 2 1.364218 0.794776 0.229193 11.00000 -1.20000 AFIX 0 C11 1 1.176365 0.800443 0.142104 11.00000 0.02383 0.02617 = 0.03375 -0.00024 0.01202 0.00119 AFIX 43 H11 2 1.176950 0.755948 0.091854 11.00000 -1.20000 AFIX 0 C12 1 1.105026 0.591161 0.187590 11.00000 0.02302 0.01939 = 0.02829 0.00127 0.00895 0.00282 AFIX 43 H12 2 1.142681 0.562213 0.146214 11.00000 -1.20000 AFIX 0 C13 1 1.161371 0.597772 0.293852 11.00000 0.02295 0.02167 = 0.02587 0.00070 0.00141 0.00139 AFIX 43 H13 2 1.242887 0.574874 0.337364 11.00000 -1.20000 AFIX 0 C14 1 1.074768 0.644911 0.325074 11.00000 0.02787 0.02634 = 0.01638 -0.00092 0.00332 0.00173 AFIX 43 H14 2 1.086438 0.659595 0.393627 11.00000 -1.20000 AFIX 0 C15 1 0.969527 0.665672 0.236684 11.00000 0.02371 0.01882 = 0.01798 -0.00158 0.00683 -0.00087 C16 1 0.855692 0.714096 0.215033 11.00000 0.02318 0.01935 = 0.01794 -0.00168 0.00797 -0.00167 AFIX 43 H16 2 0.834440 0.737970 0.268721 11.00000 -1.20000 AFIX 0 C17 1 0.665732 0.778959 0.095557 11.00000 0.02120 0.02469 = 0.01785 0.00191 0.00972 0.00429 C18 1 0.550841 0.742643 0.027694 11.00000 0.02542 0.03106 = 0.02219 -0.00496 0.00859 0.00339 AFIX 43 H18 2 0.547946 0.682768 -0.004406 11.00000 -1.20000 AFIX 0 C19 1 0.440358 0.793372 0.006583 11.00000 0.02219 0.04336 = 0.02472 -0.00566 0.00733 0.00171 AFIX 43 H19 2 0.361497 0.767399 -0.038505 11.00000 -1.20000 AFIX 0 C20 1 0.444178 0.881525 0.050718 11.00000 0.02400 0.03919 = 0.03153 0.00194 0.01309 0.01201 AFIX 43 H20 2 0.368332 0.916743 0.035156 11.00000 -1.20000 AFIX 0 C21 1 0.558427 0.918298 0.117461 11.00000 0.03406 0.02444 = 0.03241 0.00072 0.01678 0.00594 AFIX 43 H21 2 0.560858 0.978707 0.148408 11.00000 -1.20000 AFIX 0 C22 1 0.670047 0.867914 0.139928 11.00000 0.01903 0.02751 = 0.02531 0.00080 0.00936 -0.00100 AFIX 43 H22 2 0.748702 0.894015 0.185241 11.00000 -1.20000 AFIX 0 N1 3 0.733653 0.765165 -0.094947 11.00000 0.02068 0.02047 = 0.02050 0.00010 0.00906 0.00201 N2 3 0.948576 0.818586 0.049145 11.00000 0.01881 0.01906 = 0.01981 0.00072 0.00817 0.00180 N3 3 0.987785 0.632110 0.150757 11.00000 0.01986 0.01831 = 0.02099 -0.00250 0.00735 0.00005 N4 3 0.779269 0.725501 0.118362 11.00000 0.01610 0.01946 = 0.02134 -0.00117 0.00718 0.00065 CL1 4 0.988679 0.634515 -0.065585 11.00000 0.02787 0.02514 = 0.02376 -0.00180 0.01364 0.00380 CL2 4 0.721066 0.553283 -0.045375 11.00000 0.02761 0.02201 = 0.02589 -0.00304 0.00843 -0.00221 TI1 5 0.858959 0.676053 0.011223 11.00000 0.02007 0.01789 = 0.01610 -0.00027 0.00682 0.00164 HKLF 4 Covalent radii and connectivity table for 2005src1012 in P2(1)/c C 0.770 H 0.320 N 0.700 CL 0.990 TI 1.450 C1 - N1 C2 C2 - C1 C3 C3 - C4 C2 C4 - C3 N1 C5 C5 - N2 C4 C6 - C7 C11 N2 C7 - C8 C6 C8 - C9 C7 C9 - C8 C10 C10 - C11 C9 C11 - C10 C6 C12 - N3 C13 C13 - C12 C14 C14 - C15 C13 C15 - C14 C16 N3 C16 - N4 C15 C17 - C18 C22 N4 C18 - C19 C17 C19 - C20 C18 C20 - C21 C19 C21 - C20 C22 C22 - C21 C17 N1 - C1 C4 Ti1 N2 - C5 C6 Ti1 N3 - C12 C15 Ti1 N4 - C16 C17 Ti1 Cl1 - Ti1 Cl2 - Ti1 Ti1 - N3 N1 N4 N2 Cl1 Cl2 24993 Reflections read, of which 575 rejected -14 =< h =< 14, -17 =< k =< 18, -18 =< l =< 17, Max. 2-theta = 54.99 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 7 11 3 120.18 15.54 4 90.24 1 Inconsistent equivalents 4806 Unique reflections, of which 0 suppressed R(int) = 0.0997 R(sigma) = 0.0835 Friedel opposites merged Maximum memory for data reduction = 2339 / 48119 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 = 3048 / 326758 wR2 = 0.1121 before cycle 1 for 4806 data and 262 / 262 parameters GooF = S = 1.035; Restrained GooF = 1.035 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0217 * P )^2 + 3.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.44604 0.00070 -1.673 OSF Mean shift/esd = 0.204 Maximum = -1.673 for OSF Max. shift = 0.003 A for C12 Max. dU =-0.001 for C10 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3048 / 326758 wR2 = 0.1117 before cycle 2 for 4806 data and 262 / 262 parameters GooF = S = 1.030; Restrained GooF = 1.030 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0217 * P )^2 + 3.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.44590 0.00070 -0.213 OSF Mean shift/esd = 0.068 Maximum = 0.226 for z C12 Max. shift = 0.001 A for C12 Max. dU = 0.000 for C10 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3048 / 326758 wR2 = 0.1117 before cycle 3 for 4806 data and 262 / 262 parameters GooF = S = 1.029; Restrained GooF = 1.029 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0217 * P )^2 + 3.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.44590 0.00070 0.006 OSF Mean shift/esd = 0.003 Maximum = 0.022 for U11 C4 Max. shift = 0.000 A for C19 Max. dU = 0.000 for C4 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3048 / 326758 wR2 = 0.1117 before cycle 4 for 4806 data and 262 / 262 parameters GooF = S = 1.029; Restrained GooF = 1.029 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0217 * P )^2 + 3.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.44591 0.00070 0.010 OSF Mean shift/esd = 0.001 Maximum = 0.010 for OSF Max. shift = 0.000 A for C20 Max. dU = 0.000 for C20 Largest correlation matrix elements 0.603 U13 Cl1 / U11 Cl1 0.571 U13 N1 / U11 N1 0.549 U13 C2 / U11 C2 0.603 U13 C21 / U11 C21 0.567 U13 C11 / U11 C11 0.547 U13 N4 / U11 N4 0.593 U13 C4 / U11 C4 0.566 U13 Ti1 / U11 Ti1 0.547 U13 N3 / U11 N3 0.589 U13 C5 / U11 C5 0.566 U13 N2 / U11 N2 0.545 U13 C21 / U33 C21 0.582 U13 C17 / U11 C17 0.563 U13 C16 / U11 C16 0.545 U13 C15 / U11 C15 0.575 U13 C3 / U11 C3 0.561 U13 C22 / U11 C22 0.544 U13 C18 / U11 C18 0.574 U13 C1 / U11 C1 0.560 U13 C7 / U11 C7 0.542 U13 Cl2 / U11 Cl2 0.572 U13 C20 / U11 C20 0.555 U13 C12 / U11 C12 0.540 U13 C6 / U11 C6 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.5763 0.6978 -0.1991 43 0.950 0.000 C1 N1 C2 H2 0.4984 0.8566 -0.2765 43 0.950 0.000 C2 C1 C3 H3 0.6625 0.9787 -0.1740 43 0.950 0.000 C3 C4 C2 H5 0.9030 0.9513 0.0063 43 0.950 0.000 C5 N2 C4 H7 0.9864 0.9357 0.2024 43 0.950 0.000 C7 C8 C6 H8 1.1749 0.9730 0.3405 43 0.950 0.000 C8 C9 C7 H9 1.3641 0.9013 0.3555 43 0.950 0.000 C9 C8 C10 H10 1.3641 0.7946 0.2294 43 0.950 0.000 C10 C11 C9 H11 1.1767 0.7560 0.0917 43 0.950 0.000 C11 C10 C6 H12 1.1425 0.5620 0.1465 43 0.950 0.000 C12 N3 C13 H13 1.2429 0.5749 0.3372 43 0.950 0.000 C13 C12 C14 H14 1.0866 0.6598 0.3936 43 0.950 0.000 C14 C15 C13 H16 0.8345 0.7379 0.2687 43 0.950 0.000 C16 N4 C15 H18 0.5480 0.6826 -0.0044 43 0.950 0.000 C18 C19 C17 H19 0.3618 0.7672 -0.0386 43 0.950 0.000 C19 C20 C18 H20 0.3682 0.9165 0.0354 43 0.950 0.000 C20 C21 C19 H21 0.5609 0.9787 0.1484 43 0.950 0.000 C21 C20 C22 H22 0.7488 0.8939 0.1851 43 0.950 0.000 C22 C21 C17 2005src1012 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.61965 0.75635 -0.17570 1.00000 0.02062 0.03026 0.02070 -0.00121 0.00866 -0.00012 0.02374 0.00677 0.00030 0.00024 0.00023 0.00000 0.00169 0.00189 0.00157 0.00133 0.00135 0.00142 0.00070 H1 0.57628 0.69778 -0.19908 1.00000 0.02849 0.00000 0.00000 C2 0.57548 0.84430 -0.21914 1.00000 0.02568 0.03933 0.02325 0.00407 0.00874 0.00778 0.02976 0.00744 0.00033 0.00026 0.00025 0.00000 0.00186 0.00223 0.00167 0.00145 0.00145 0.00158 0.00080 H2 0.49839 0.85660 -0.27649 1.00000 0.03571 0.00000 0.00000 C3 0.66609 0.91183 -0.16244 1.00000 0.02865 0.02450 0.02596 0.00758 0.01196 0.00694 0.02605 0.00726 0.00032 0.00024 0.00024 0.00000 0.00191 0.00181 0.00169 0.00136 0.00147 0.00146 0.00073 H3 0.66246 0.97866 -0.17395 1.00000 0.03125 0.00000 0.00000 C4 0.76201 0.86211 -0.08632 1.00000 0.02491 0.02190 0.02098 0.00229 0.01263 0.00177 0.02150 0.00672 0.00030 0.00023 0.00023 0.00000 0.00174 0.00166 0.00153 0.00126 0.00135 0.00136 0.00066 C5 0.87732 0.88660 -0.00672 1.00000 0.02504 0.01756 0.02518 0.00037 0.01386 0.00184 0.02138 0.00680 0.00030 0.00022 0.00023 0.00000 0.00177 0.00165 0.00161 0.00125 0.00138 0.00134 0.00067 H5 0.90300 0.95131 0.00628 1.00000 0.02566 0.00000 0.00000 C6 1.06381 0.84298 0.13346 1.00000 0.02001 0.02056 0.02115 0.00017 0.00690 -0.00411 0.02100 0.00637 0.00030 0.00022 0.00023 0.00000 0.00164 0.00172 0.00153 0.00123 0.00128 0.00130 0.00066 C7 1.06347 0.90694 0.20789 1.00000 0.02776 0.02417 0.02733 -0.00144 0.01115 -0.00100 0.02638 0.00694 0.00033 0.00024 0.00024 0.00000 0.00187 0.00180 0.00171 0.00136 0.00146 0.00145 0.00072 H7 0.98639 0.93567 0.20242 1.00000 0.03166 0.00000 0.00000 C8 1.17522 0.92884 0.28996 1.00000 0.03983 0.02572 0.02406 -0.00373 0.00871 -0.00931 0.03117 0.00710 0.00035 0.00025 0.00025 0.00000 0.00223 0.00196 0.00171 0.00138 0.00157 0.00165 0.00081 H8 1.17490 0.97305 0.34055 1.00000 0.03740 0.00000 0.00000 C9 1.28734 0.88675 0.29876 1.00000 0.02851 0.02794 0.02970 0.00548 -0.00242 -0.00676 0.03320 0.00733 0.00035 0.00025 0.00026 0.00000 0.00203 0.00204 0.00184 0.00147 0.00151 0.00159 0.00084 H9 1.36409 0.90129 0.35553 1.00000 0.03984 0.00000 0.00000 C10 1.28687 0.82306 0.22397 1.00000 0.01995 0.02796 0.05010 0.00814 0.01002 0.00035 0.03394 0.00765 0.00033 0.00026 0.00028 0.00000 0.00181 0.00196 0.00222 0.00170 0.00163 0.00154 0.00082 H10 1.36409 0.79463 0.22937 1.00000 0.04073 0.00000 0.00000 C11 1.17619 0.80045 0.14205 1.00000 0.02389 0.02486 0.03347 -0.00086 0.01177 0.00062 0.02732 0.00716 0.00031 0.00024 0.00026 0.00000 0.00185 0.00188 0.00183 0.00140 0.00151 0.00142 0.00075 H11 1.17674 0.75602 0.09172 1.00000 0.03278 0.00000 0.00000 C12 1.10489 0.59113 0.18780 1.00000 0.02336 0.01930 0.02809 0.00066 0.00969 0.00250 0.02378 0.00680 0.00031 0.00022 0.00024 0.00000 0.00180 0.00169 0.00170 0.00131 0.00142 0.00137 0.00069 H12 1.14247 0.56197 0.14649 1.00000 0.02854 0.00000 0.00000 C13 1.16132 0.59782 0.29379 1.00000 0.02187 0.02212 0.02613 0.00083 0.00147 0.00200 0.02596 0.00678 0.00032 0.00023 0.00024 0.00000 0.00178 0.00178 0.00167 0.00134 0.00139 0.00139 0.00072 H13 1.24287 0.57493 0.33724 1.00000 0.03116 0.00000 0.00000 C14 1.07484 0.64505 0.32505 1.00000 0.02731 0.02545 0.01620 -0.00126 0.00328 0.00119 0.02472 0.00660 0.00031 0.00023 0.00023 0.00000 0.00182 0.00180 0.00148 0.00127 0.00133 0.00144 0.00070 H14 1.08660 0.65981 0.39361 1.00000 0.02966 0.00000 0.00000 C15 0.96951 0.66576 0.23666 1.00000 0.02300 0.01897 0.01781 -0.00146 0.00700 -0.00129 0.02030 0.00635 0.00030 0.00022 0.00022 0.00000 0.00169 0.00167 0.00146 0.00119 0.00126 0.00131 0.00065 C16 0.85579 0.71410 0.21504 1.00000 0.02295 0.01904 0.01823 -0.00190 0.00856 -0.00198 0.01997 0.00628 0.00029 0.00022 0.00022 0.00000 0.00170 0.00162 0.00150 0.00120 0.00132 0.00132 0.00065 H16 0.83453 0.73791 0.26875 1.00000 0.02397 0.00000 0.00000 C17 0.66571 0.77889 0.09557 1.00000 0.02050 0.02380 0.01766 0.00259 0.00936 0.00433 0.02011 0.00655 0.00029 0.00022 0.00022 0.00000 0.00166 0.00169 0.00148 0.00123 0.00129 0.00134 0.00065 C18 0.55086 0.74254 0.02771 1.00000 0.02537 0.03128 0.02159 -0.00477 0.00832 0.00405 0.02642 0.00686 0.00031 0.00025 0.00023 0.00000 0.00182 0.00198 0.00162 0.00137 0.00141 0.00151 0.00074 H18 0.54798 0.68265 -0.00435 1.00000 0.03171 0.00000 0.00000 C19 0.44055 0.79320 0.00658 1.00000 0.02266 0.04343 0.02361 -0.00557 0.00705 0.00220 0.03060 0.00742 0.00033 0.00027 0.00025 0.00000 0.00179 0.00222 0.00169 0.00151 0.00142 0.00160 0.00079 H19 0.36176 0.76724 -0.03865 1.00000 0.03673 0.00000 0.00000 C20 0.44413 0.88143 0.05086 1.00000 0.02351 0.03814 0.03099 0.00264 0.01268 0.01257 0.03032 0.00749 0.00033 0.00026 0.00025 0.00000 0.00185 0.00221 0.00184 0.00152 0.00152 0.00161 0.00081 H20 0.36821 0.91651 0.03543 1.00000 0.03638 0.00000 0.00000 C21 0.55839 0.91826 0.11749 1.00000 0.03333 0.02445 0.03215 0.00067 0.01685 0.00555 0.02879 0.00756 0.00034 0.00024 0.00026 0.00000 0.00205 0.00188 0.00185 0.00142 0.00161 0.00152 0.00077 H21 0.56085 0.97868 0.14842 1.00000 0.03455 0.00000 0.00000 C22 0.67010 0.86783 0.13987 1.00000 0.01926 0.02672 0.02488 0.00054 0.00925 -0.00113 0.02349 0.00685 0.00030 0.00024 0.00024 0.00000 0.00169 0.00180 0.00163 0.00134 0.00136 0.00140 0.00069 H22 0.74879 0.89395 0.18508 1.00000 0.02819 0.00000 0.00000 N1 0.73362 0.76512 -0.09498 1.00000 0.02056 0.02041 0.01995 -0.00016 0.00904 0.00201 0.02001 0.00530 0.00024 0.00018 0.00019 0.00000 0.00141 0.00144 0.00129 0.00104 0.00112 0.00111 0.00056 N2 0.94846 0.81848 0.04901 1.00000 0.01905 0.01876 0.01978 0.00085 0.00863 0.00178 0.01893 0.00526 0.00024 0.00018 0.00018 0.00000 0.00135 0.00137 0.00125 0.00103 0.00107 0.00112 0.00054 N3 0.98780 0.63217 0.15072 1.00000 0.01975 0.01756 0.02024 -0.00196 0.00716 0.00048 0.01946 0.00520 0.00024 0.00018 0.00018 0.00000 0.00138 0.00135 0.00129 0.00103 0.00108 0.00112 0.00054 N4 0.77942 0.72556 0.11849 1.00000 0.01656 0.01873 0.02054 -0.00123 0.00747 0.00016 0.01860 0.00521 0.00023 0.00018 0.00019 0.00000 0.00133 0.00138 0.00129 0.00103 0.00107 0.00108 0.00054 Cl1 0.98862 0.63454 -0.06559 1.00000 0.02772 0.02495 0.02384 -0.00170 0.01354 0.00392 0.02448 0.00167 0.00008 0.00006 0.00006 0.00000 0.00044 0.00042 0.00039 0.00031 0.00033 0.00034 0.00019 Cl2 0.72101 0.55331 -0.04537 1.00000 0.02743 0.02198 0.02562 -0.00287 0.00823 -0.00221 0.02577 0.00164 0.00008 0.00006 0.00006 0.00000 0.00044 0.00041 0.00040 0.00031 0.00033 0.00034 0.00019 Ti1 0.85897 0.67606 0.01122 1.00000 0.02011 0.01783 0.01613 -0.00034 0.00682 0.00170 0.01816 0.00115 0.00005 0.00004 0.00004 0.00000 0.00030 0.00029 0.00027 0.00022 0.00022 0.00024 0.00014 Final Structure Factor Calculation for 2005src1012 in P2(1)/c Total number of l.s. parameters = 262 Maximum vector length = 511 Memory required = 2786 / 24017 wR2 = 0.1117 before cycle 5 for 4806 data and 0 / 262 parameters GooF = S = 1.030; Restrained GooF = 1.030 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0217 * P )^2 + 3.06 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0571 for 3374 Fo > 4sig(Fo) and 0.0948 for all 4806 data wR2 = 0.1117, GooF = S = 1.030, Restrained GooF = 1.030 for all data Occupancy sum of asymmetric unit = 29.00 for non-hydrogen and 18.00 for hydrogen atoms Principal mean square atomic displacements U 0.0304 0.0209 0.0199 C1 0.0429 0.0254 0.0210 C2 0.0352 0.0258 0.0172 C3 0.0269 0.0211 0.0165 C4 0.0280 0.0196 0.0166 C5 0.0259 0.0210 0.0161 C6 0.0282 0.0274 0.0236 C7 0.0471 0.0271 0.0192 C8 0.0569 0.0238 0.0189 C9 0.0567 0.0253 0.0198 C10 0.0339 0.0252 0.0229 C11 0.0287 0.0245 0.0181 C12 0.0379 0.0227 0.0172 C13 0.0337 0.0250 0.0154 C14 0.0242 0.0199 0.0168 C15 0.0238 0.0195 0.0167 C16 0.0270 0.0176 0.0157 C17 0.0369 0.0236 0.0187 C18 0.0462 0.0242 0.0214 C19 0.0454 0.0306 0.0149 C20 0.0369 0.0290 0.0205 C21 0.0272 0.0248 0.0185 C22 0.0225 0.0202 0.0174 N1 0.0211 0.0188 0.0169 N2 0.0226 0.0194 0.0164 N3 0.0214 0.0181 0.0163 N4 0.0305 0.0260 0.0170 Cl1 0.0307 0.0267 0.0199 Cl2 0.0216 0.0170 0.0159 Ti1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.014 0.026 0.039 0.054 0.070 0.088 0.112 0.144 0.202 1.000 Number in group 525. 457. 476. 469. 502. 458. 478. 476. 484. 481. GooF 1.067 1.039 1.013 0.997 1.070 1.097 1.030 0.999 0.968 1.004 K 6.809 1.976 1.431 1.121 1.034 1.033 1.003 1.009 1.005 1.003 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.31 1.64 inf Number in group 484. 487. 486. 469. 482. 484. 476. 474. 481. 483. GooF 1.016 1.004 1.051 1.051 0.959 0.973 0.938 0.882 1.005 1.344 K 1.058 1.086 1.052 1.078 1.020 1.015 1.016 1.016 1.007 1.000 R1 0.265 0.224 0.179 0.136 0.099 0.074 0.061 0.053 0.040 0.038 Recommended weighting scheme: WGHT 0.0138 3.2127 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) 0 6 0 394.86 25.18 5.33 0.024 2.34 0 4 2 769.15 495.33 5.08 0.106 3.09 -5 10 13 1151.26 332.17 4.95 0.087 0.86 -6 0 16 4666.18 2687.66 4.47 0.247 0.89 -5 4 1 1780.96 2278.25 4.46 0.228 1.88 -4 3 7 92.30 195.24 4.05 0.067 1.78 -4 6 12 146.01 17.26 3.83 0.020 1.06 -7 7 15 1371.82 839.41 3.74 0.138 0.84 3 0 0 1600.94 1050.61 3.67 0.154 3.52 4 2 1 82.55 198.19 3.54 0.067 2.28 2 2 6 1628.24 1315.21 3.44 0.173 1.72 6 11 5 212.44 4.42 3.35 0.010 0.89 3 9 3 118.98 16.18 3.30 0.019 1.29 0 14 0 155.44 60.13 3.28 0.037 1.00 2 15 1 451.77 770.02 3.24 0.132 0.91 -11 6 15 -207.84 241.33 3.20 0.074 0.78 -5 8 14 498.30 195.00 3.18 0.067 0.88 1 3 6 256.51 159.69 3.08 0.060 1.82 -4 12 11 551.68 320.64 3.08 0.085 0.87 3 5 2 36.47 153.99 3.07 0.059 1.94 -4 3 3 660.87 836.32 3.07 0.138 2.41 -6 3 17 974.09 417.13 3.07 0.097 0.82 4 6 0 20.12 102.92 3.07 0.048 1.75 3 1 15 187.88 26.95 3.06 0.025 0.77 -1 9 4 3089.83 2578.07 3.05 0.242 1.43 -3 4 6 1088.17 885.91 3.04 0.142 1.93 -3 3 6 1242.03 1019.50 3.04 0.152 2.07 0 2 9 34.84 101.42 3.03 0.048 1.42 -6 6 3 142.00 62.24 3.01 0.038 1.48 -6 2 17 366.01 37.09 3.00 0.029 0.83 1 4 4 183.21 98.98 3.00 0.047 2.19 1 0 4 702.67 507.70 3.00 0.107 2.81 -6 10 14 560.93 262.91 2.98 0.077 0.82 -5 5 15 129.42 14.98 2.95 0.018 0.90 -9 14 8 178.80 2.12 2.91 0.007 0.77 -2 4 3 3126.27 2668.29 2.88 0.246 2.72 -1 4 2 1409.44 1168.81 2.87 0.163 3.13 -4 5 1 757.26 939.58 2.87 0.146 1.99 -5 1 2 377.66 510.14 2.86 0.108 2.27 -5 3 7 497.72 378.11 2.82 0.093 1.68 11 4 0 298.57 10.75 2.80 0.016 0.93 -1 7 4 21843.11 18628.20 2.74 0.651 1.74 -12 5 2 2185.40 1697.82 2.74 0.196 0.88 -3 6 4 362.68 254.03 2.73 0.076 1.86 3 11 7 297.15 455.06 2.72 0.102 0.95 -1 5 15 460.74 47.44 2.72 0.033 0.85 9 6 4 2410.27 49.61 2.71 0.034 0.91 -6 12 6 441.58 306.37 2.69 0.083 0.97 -3 3 7 1462.51 1691.09 2.68 0.196 1.85 -4 6 14 20.00 92.81 2.67 0.046 0.93 Bond lengths and angles C1 - Distance Angles N1 1.3592 (0.0040) C2 1.3825 (0.0046) 110.73 (0.30) C1 - N1 C2 - Distance Angles C1 1.3825 (0.0046) C3 1.4010 (0.0049) 106.93 (0.30) C2 - C1 C3 - Distance Angles C4 1.3855 (0.0044) C2 1.4010 (0.0049) 106.60 (0.30) C3 - C4 C4 - Distance Angles C3 1.3855 (0.0044) N1 1.3938 (0.0040) 109.70 (0.29) C5 1.3992 (0.0045) 135.16 (0.31) 115.12 (0.27) C4 - C3 N1 C5 - Distance Angles N2 1.3008 (0.0039) C4 1.3992 (0.0045) 118.29 (0.29) C5 - N2 C6 - Distance Angles C7 1.3874 (0.0043) C11 1.3865 (0.0045) 119.94 (0.31) N2 1.4303 (0.0039) 120.56 (0.28) 119.48 (0.28) C6 - C7 C11 C7 - Distance Angles C8 1.3814 (0.0048) C6 1.3874 (0.0044) 120.00 (0.32) C7 - C8 C8 - Distance Angles C9 1.3802 (0.0052) C7 1.3814 (0.0048) 120.26 (0.33) C8 - C9 C9 - Distance Angles C8 1.3802 (0.0052) C10 1.3860 (0.0051) 119.37 (0.33) C9 - C8 C10 - Distance Angles C11 1.3754 (0.0048) C9 1.3860 (0.0051) 120.93 (0.34) C10 - C11 C11 - Distance Angles C10 1.3754 (0.0048) C6 1.3865 (0.0045) 119.49 (0.32) C11 - C10 C12 - Distance Angles N3 1.3641 (0.0040) C13 1.3824 (0.0045) 110.65 (0.28) C12 - N3 C13 - Distance Angles C12 1.3824 (0.0045) C14 1.4085 (0.0045) 106.91 (0.29) C13 - C12 C14 - Distance Angles C15 1.3828 (0.0043) C13 1.4085 (0.0045) 106.73 (0.27) C14 - C15 C15 - Distance Angles C14 1.3828 (0.0043) C16 1.3964 (0.0043) 135.00 (0.28) N3 1.4002 (0.0036) 109.62 (0.27) 115.33 (0.26) C15 - C14 C16 C16 - Distance Angles N4 1.3086 (0.0038) C15 1.3964 (0.0043) 117.91 (0.26) C16 - N4 C17 - Distance Angles C18 1.3852 (0.0045) C22 1.3893 (0.0044) 119.79 (0.29) N4 1.4290 (0.0038) 119.95 (0.28) 120.25 (0.28) C17 - C18 C22 C18 - Distance Angles C19 1.3806 (0.0046) C17 1.3852 (0.0045) 120.12 (0.32) C18 - C19 C19 - Distance Angles C20 1.3816 (0.0049) C18 1.3806 (0.0046) 120.37 (0.33) C19 - C20 C20 - Distance Angles C21 1.3777 (0.0050) C19 1.3816 (0.0049) 119.64 (0.31) C20 - C21 C21 - Distance Angles C20 1.3777 (0.0050) C22 1.3899 (0.0046) 120.60 (0.32) C21 - C20 C22 - Distance Angles C21 1.3899 (0.0046) C17 1.3893 (0.0044) 119.45 (0.31) C22 - C21 N1 - Distance Angles C1 1.3592 (0.0040) C4 1.3938 (0.0040) 106.04 (0.26) Ti1 2.0437 (0.0026) 136.49 (0.22) 117.42 (0.20) N1 - C1 C4 N2 - Distance Angles C5 1.3008 (0.0039) C6 1.4303 (0.0039) 118.74 (0.27) Ti1 2.2142 (0.0026) 113.39 (0.21) 127.33 (0.19) N2 - C5 C6 N3 - Distance Angles C12 1.3641 (0.0040) C15 1.4002 (0.0036) 106.08 (0.25) Ti1 2.0369 (0.0025) 136.55 (0.20) 116.07 (0.20) N3 - C12 C15 N4 - Distance Angles C16 1.3086 (0.0038) C17 1.4290 (0.0038) 118.26 (0.24) Ti1 2.1815 (0.0023) 113.41 (0.20) 127.69 (0.18) N4 - C16 C17 Cl1 - Distance Angles Ti1 2.2509 (0.0009) Cl1 - Cl2 - Distance Angles Ti1 2.2622 (0.0010) Cl2 - Ti1 - Distance Angles N3 2.0369 (0.0025) N1 2.0437 (0.0026) 157.90 (0.10) N4 2.1815 (0.0023) 76.37 (0.10) 87.11 (0.09) N2 2.2142 (0.0026) 87.13 (0.10) 75.51 (0.10) 80.14 (0.09) Cl1 2.2509 (0.0009) 91.47 (0.07) 102.20 (0.07) 165.15 (0.07) 90.90 (0.07) Cl2 2.2622 (0.0010) 104.48 (0.08) 90.86 (0.08) 93.34 (0.07) 165.08 (0.07) 98.02 (0.04) Ti1 - N3 N1 N4 N2 Cl1 FMAP and GRID set by program FMAP 2 3 21 GRID -1.389 -2 -2 1.389 2 2 R1 = 0.0930 for 4806 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.36 at 0.9531 0.6409 0.0996 [ 0.68 A from N3 ] Deepest hole -0.42 at 0.9156 0.6396 0.0331 [ 0.79 A from TI1 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 2901 / 26586 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.9531 0.6409 0.0996 1.00000 0.05 0.36 0.68 N3 1.38 TI1 1.83 C12 1.91 C15 Q2 1 0.7582 0.6342 -0.0855 1.00000 0.05 0.34 1.41 CL2 1.52 TI1 1.86 N1 2.25 H1 Q3 1 0.8485 0.7427 0.3186 1.00000 0.05 0.34 0.66 H16 1.56 C16 2.14 N1 2.40 C15 Q4 1 0.5929 0.5525 -0.0953 1.00000 0.05 0.32 1.36 CL2 2.41 H18 2.48 H1 2.53 H9 Q5 1 0.9354 0.6710 -0.0243 1.00000 0.05 0.32 1.13 CL1 1.18 TI1 2.29 N2 2.37 N3 Q6 1 1.2973 0.9578 0.3325 1.00000 0.05 0.31 1.06 H9 1.09 C9 1.35 C8 1.48 H8 Q7 1 0.9618 1.0493 0.0393 1.00000 0.05 0.30 1.52 H5 1.91 H5 2.01 H14 2.27 C5 Q8 1 0.7225 0.7568 0.1008 1.00000 0.05 0.30 0.70 C17 0.74 N4 1.83 C16 1.84 C22 Q9 1 0.9734 0.6796 0.0474 1.00000 0.05 0.29 1.21 TI1 1.56 N3 1.80 CL1 1.97 N2 Q10 1 1.2826 0.6013 0.3121 1.00000 0.05 0.29 0.78 H13 1.32 C13 2.11 C12 2.32 H12 Q11 1 0.9393 0.6710 -0.1508 1.00000 0.05 0.29 1.22 CL1 1.81 H16 2.38 C16 2.64 H22 Q12 1 0.8272 0.6250 -0.1265 1.00000 0.05 0.28 1.71 CL1 1.97 TI1 2.23 CL2 2.37 N1 Q13 1 1.1374 0.9016 0.2417 1.00000 0.05 0.28 0.75 C8 0.80 C7 1.60 C9 1.64 H8 Q14 1 0.6211 0.7602 0.1089 1.00000 0.05 0.28 0.67 C17 1.14 C18 1.61 C22 1.84 N4 Q15 1 1.1596 0.6443 0.2914 1.00000 0.05 0.28 0.65 C13 1.25 C14 1.34 H13 1.54 C12 Q16 1 1.0476 0.6212 0.1631 1.00000 0.05 0.28 0.66 N3 0.74 C12 1.47 H12 1.74 C15 Q17 1 0.9213 0.5535 -0.0259 1.00000 0.05 0.28 1.60 CL1 2.01 TI1 2.21 CL2 2.25 H12 Q18 1 0.8013 0.6906 0.0693 1.00000 0.05 0.28 0.97 N4 1.27 TI1 1.93 C16 2.14 C17 Q19 1 0.6936 0.6697 -0.0435 1.00000 0.05 0.27 1.67 CL2 1.68 N1 1.75 TI1 1.98 H18 Q20 1 0.7571 0.6791 -0.0277 1.00000 0.05 0.27 1.08 TI1 1.50 N1 1.81 CL2 2.09 N4 Shortest distances between peaks (including symmetry equivalents) 19 20 0.69 5 9 0.94 1 9 1.02 2 20 1.04 1 16 1.13 2 12 1.16 8 14 1.22 2 19 1.23 18 20 1.27 10 15 1.46 8 18 1.49 3 11 1.54 11 12 1.60 18 19 1.61 5 12 1.62 5 17 1.66 9 16 1.72 12 17 1.73 1 5 1.74 1 18 1.77 15 16 1.79 5 11 1.81 2 5 1.94 6 13 1.94 4 19 1.98 9 17 2.02 12 20 2.02 5 20 2.04 2 17 2.06 3 12 2.07 1 17 2.07 9 18 2.13 7 7 2.17 2 4 2.18 2 18 2.20 17 17 2.24 9 20 2.28 8 19 2.29 8 20 2.29 1 20 2.32 12 19 2.37 3 5 2.38 5 18 2.42 9 12 2.49 11 17 2.49 4 20 2.49 2 9 2.52 5 16 2.55 14 18 2.55 17 20 2.58 2 11 2.65 2 3 2.66 16 17 2.66 9 11 2.68 1 2 2.69 5 19 2.69 10 16 2.70 16 18 2.78 1 15 2.81 3 8 2.85 1 19 2.89 14 19 2.90 1 12 2.95 9 19 2.96 3 20 2.99 17 18 2.99 Time profile in seconds ----------------------- 0.03: Read and process instructions 0.00: Fit rigid groups 0.00: 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. 1.38: 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 1.85: Structure factors and derivatives 2.98: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.01: Apply other restraints 0.27: Solve l.s. equations 0.00: Generate HTAB table 0.01: Other dependent quantities, CIF, tables 0.18: Analysis of variance 0.06: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2005src1012 finished at 17:39:42 Total CPU time: 7.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++