++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XL - CRYSTAL STRUCTURE REFINEMENT - SHELXTL Ver. 6.12 W95/98/NT/2000/ME + + Copyright(c) 2001 Bruker Analytical X-ray Solutions All Rights Reserved + + 2007src1052 started at 13:03:02 on 16-Aug-2007 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src1052 in P2(1) CELL 0.71073 8.9411 11.0719 10.9373 90.000 99.810 90.000 ZERR 2.00 0.0003 0.0003 0.0004 0.000 0.002 0.000 LATT -1 SYMM -X, 0.5+Y, -Z SFAC C H N O S CL UNIT 44 56 2 4 2 2 V = 1066.91 F(000) = 432.0 Mu = 0.29 mm-1 Cell Wt = 811.93 Rho = 1.264 TEMP -153 SIZE 0.6x0.5x0.3 TWIN BOND $H OMIT -3 55 SHEL 7 0.77 ACTA OMIT 1 0 7 OMIT -1 -1 -2 OMIT 2 1 0 OMIT -1 1 2 OMIT 3 0 7 OMIT 0 -2 0 OMIT 1 1 7 OMIT 0 3 7 OMIT 0 -3 7 OMIT 2 -2 1 OMIT 1 -1 7 OMIT 1 -1 0 L.S. 8 FMAP 2 PLAN 20 WGHT 0.0566 0.1765 BASF 0.43965 FVAR 0.41596 S1 5 1.135931 -0.004210 0.665797 11.00000 0.02584 0.01448 = 0.04123 -0.00411 0.00355 0.00204 CL1 6 0.515579 0.132042 0.381657 11.00000 0.03308 0.04297 = 0.03647 0.00629 -0.01115 -0.00531 C1 1 0.707061 0.150203 0.466011 11.00000 0.02665 0.02790 = 0.02280 0.00356 -0.00388 -0.00634 AFIX 13 H1 2 0.730089 0.238643 0.469670 11.00000 -1.20000 AFIX 0 C2 1 0.818987 0.090395 0.395783 11.00000 0.03958 0.03698 = 0.01917 -0.00155 0.00489 -0.00970 AFIX 23 H2A 2 0.808779 0.125278 0.311424 11.00000 -1.20000 H2B 2 0.797363 0.002797 0.387647 11.00000 -1.20000 AFIX 0 C3 1 0.980000 0.110095 0.465314 11.00000 0.03206 0.03104 = 0.02530 -0.00117 0.01156 -0.00524 AFIX 23 H3A 2 1.053556 0.065659 0.423995 11.00000 -1.20000 H3B 2 1.005978 0.197057 0.466582 11.00000 -1.20000 AFIX 0 N1 3 0.985742 0.064770 0.593728 11.00000 0.02371 0.02052 = 0.02416 -0.00145 0.00656 0.00137 C4 1 0.883748 0.125622 0.667293 11.00000 0.02268 0.01822 = 0.01875 0.00061 0.00479 0.00112 AFIX 13 H4 2 0.894916 0.083857 0.749415 11.00000 -1.20000 AFIX 0 C5 1 0.718963 0.105276 0.599891 11.00000 0.02290 0.01913 = 0.02123 -0.00152 0.00382 -0.00254 AFIX 13 H5 2 0.651696 0.157815 0.641460 11.00000 -1.20000 AFIX 0 C6 1 0.667821 -0.025378 0.612613 11.00000 0.02922 0.02345 = 0.02639 0.00150 0.00712 -0.00804 AFIX 23 H6A 2 0.571225 -0.038856 0.554973 11.00000 -1.20000 H6B 2 0.744746 -0.080527 0.588161 11.00000 -1.20000 AFIX 0 C7 1 0.645315 -0.056221 0.744402 11.00000 0.03120 0.02351 = 0.03262 0.00850 0.00833 -0.00103 AFIX 137 H7A 2 0.744025 -0.057592 0.799432 11.00000 -1.50000 H7B 2 0.597221 -0.135725 0.744792 11.00000 -1.50000 H7C 2 0.580262 0.004867 0.773529 11.00000 -1.50000 AFIX 0 C8 1 0.924323 0.259504 0.692211 11.00000 0.02141 0.01740 = 0.02125 -0.00043 0.00410 -0.00070 AFIX 23 H8A 2 1.036050 0.268909 0.706183 11.00000 -1.20000 H8B 2 0.881612 0.307860 0.618342 11.00000 -1.20000 AFIX 0 C9 1 0.863197 0.307358 0.804844 11.00000 0.04570 0.03051 = 0.03181 -0.00822 0.01870 -0.01365 AFIX 23 H9A 2 0.750868 0.306499 0.786986 11.00000 -1.20000 H9B 2 0.896334 0.253276 0.876417 11.00000 -1.20000 AFIX 0 C10 1 0.916939 0.433623 0.838553 11.00000 0.03135 0.02128 = 0.01911 -0.00246 0.01221 0.00138 C11 1 1.054052 0.454383 0.917665 11.00000 0.03880 0.02182 = 0.02158 0.00134 0.00338 0.00648 AFIX 43 H11 2 1.111012 0.387743 0.955403 11.00000 -1.20000 AFIX 0 C12 1 1.108337 0.569724 0.942050 11.00000 0.04125 0.03049 = 0.02496 -0.00622 0.00447 -0.00454 AFIX 43 H12 2 1.202462 0.581814 0.995730 11.00000 -1.20000 AFIX 0 C13 1 1.026348 0.668706 0.888649 11.00000 0.07452 0.01552 = 0.02599 -0.00312 0.02169 -0.00395 AFIX 43 H13 2 1.064311 0.748295 0.904803 11.00000 -1.20000 AFIX 0 C14 1 0.888667 0.649686 0.811633 11.00000 0.05918 0.02792 = 0.02799 0.00828 0.01745 0.01875 AFIX 43 H14 2 0.830903 0.716523 0.775276 11.00000 -1.20000 AFIX 0 C15 1 0.835137 0.533297 0.787581 11.00000 0.03009 0.04202 = 0.02422 0.00288 0.00651 0.00608 AFIX 43 H15 2 0.740208 0.521398 0.734964 11.00000 -1.20000 AFIX 0 C16 1 1.254104 0.106890 0.748086 11.00000 0.01979 0.01958 = 0.03186 -0.00100 0.00325 0.00554 C17 1 1.327342 0.188965 0.682143 11.00000 0.02122 0.02703 = 0.03024 -0.00366 0.00516 0.00264 AFIX 43 H17 2 1.321045 0.180733 0.594957 11.00000 -1.20000 AFIX 0 C18 1 1.409905 0.283226 0.745182 11.00000 0.02372 0.02199 = 0.04004 -0.00470 0.01123 -0.00080 AFIX 43 H18 2 1.457634 0.340834 0.700202 11.00000 -1.20000 AFIX 0 C19 1 1.423445 0.294150 0.873991 11.00000 0.02298 0.03158 = 0.03906 -0.01126 0.01178 -0.00187 C20 1 1.351044 0.208790 0.937546 11.00000 0.02886 0.03981 = 0.02834 -0.00435 0.00715 -0.00044 AFIX 43 H20 2 1.361113 0.214269 1.025249 11.00000 -1.20000 AFIX 0 C22 1 1.511873 0.396341 0.943194 11.00000 0.04146 0.05541 = 0.05385 -0.03157 0.01979 -0.01963 AFIX 137 H22A 2 1.610344 0.366258 0.985355 11.00000 -1.50000 H22B 2 1.454918 0.429160 1.004686 11.00000 -1.50000 H22C 2 1.527821 0.460011 0.884513 11.00000 -1.50000 AFIX 0 C21 1 1.265226 0.116659 0.876205 11.00000 0.02274 0.02684 = 0.03226 0.00600 0.00599 0.00416 AFIX 43 H21 2 1.214471 0.060711 0.920762 11.00000 -1.20000 AFIX 0 O1 4 1.213033 -0.053971 0.571797 11.00000 0.03291 0.03212 = 0.06077 -0.02360 0.01118 0.00602 O2 4 1.087247 -0.081834 0.756110 11.00000 0.03778 0.02019 = 0.05630 0.01389 0.00141 -0.00361 HKLF 4 Covalent radii and connectivity table for 2007src1052 in P2(1) C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 CL 0.990 S1 - O2 O1 N1 C16 Cl1 - C1 C1 - C2 C5 Cl1 C2 - C1 C3 C3 - N1 C2 N1 - C4 C3 S1 C4 - N1 C8 C5 C5 - C6 C1 C4 C6 - C7 C5 C7 - C6 C8 - C9 C4 C9 - C10 C8 C10 - C15 C11 C9 C11 - C12 C10 C12 - C11 C13 C13 - C14 C12 C14 - C13 C15 C15 - C14 C10 C16 - C17 C21 S1 C17 - C16 C18 C18 - C17 C19 C19 - C20 C18 C22 C20 - C21 C19 C22 - C19 C21 - C20 C16 O1 - S1 O2 - S1 Floating origin restraints generated 13274 Reflections read, of which 61 rejected -10 =< h =< 11, -13 =< k =< 14, -14 =< l =< 14, Max. 2-theta = 54.95 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 2 8 4 2.04 0.10 3 0.88 1 Inconsistent equivalents 4663 Unique reflections, of which 0 suppressed R(int) = 0.0367 R(sigma) = 0.0443 Friedel opposites not merged Maximum memory for data reduction = 2779 / 46331 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 = 3482 / 308595 wR2 = 0.1078 before cycle 1 for 4663 data and 247 / 247 parameters GooF = S = 1.120; Restrained GooF = 1.120 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0566 * P )^2 + 0.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41572 0.00072 -0.333 OSF 2 0.43880 0.05749 -0.015 BASF 1 Mean shift/esd = 0.033 Maximum = -0.333 for OSF Max. shift = 0.001 A for H22C Max. dU = 0.000 for C13 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3482 / 308595 wR2 = 0.1078 before cycle 2 for 4663 data and 247 / 247 parameters GooF = S = 1.121; Restrained GooF = 1.121 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0566 * P )^2 + 0.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41564 0.00072 -0.116 OSF 2 0.43848 0.05749 -0.006 BASF 1 Mean shift/esd = 0.011 Maximum = -0.116 for OSF Max. shift = 0.001 A for H22C Max. dU = 0.000 for C13 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3482 / 308595 wR2 = 0.1078 before cycle 3 for 4663 data and 247 / 247 parameters GooF = S = 1.121; Restrained GooF = 1.121 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0566 * P )^2 + 0.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41563 0.00072 -0.003 OSF 2 0.43847 0.05748 0.000 BASF 1 Mean shift/esd = 0.001 Maximum = 0.016 for tors H22A Max. shift = 0.000 A for H22A Max. dU = 0.000 for O2 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3482 / 308595 wR2 = 0.1078 before cycle 4 for 4663 data and 247 / 247 parameters GooF = S = 1.121; Restrained GooF = 1.121 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0566 * P )^2 + 0.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41563 0.00072 0.000 OSF 2 0.43847 0.05749 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.008 for tors H22A Max. shift = 0.000 A for H22A Max. dU = 0.000 for C22 Least-squares cycle 5 Maximum vector length = 511 Memory required = 3482 / 308595 wR2 = 0.1078 before cycle 5 for 4663 data and 247 / 247 parameters GooF = S = 1.121; Restrained GooF = 1.121 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0566 * P )^2 + 0.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41563 0.00072 0.001 OSF 2 0.43846 0.05749 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.004 for tors H22A Max. shift = 0.000 A for H22A Max. dU = 0.000 for C22 Least-squares cycle 6 Maximum vector length = 511 Memory required = 3482 / 308595 wR2 = 0.1078 before cycle 6 for 4663 data and 247 / 247 parameters GooF = S = 1.121; Restrained GooF = 1.121 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0566 * P )^2 + 0.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41563 0.00072 0.001 OSF 2 0.43847 0.05748 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.002 for tors H22A Max. shift = 0.000 A for H22A Max. dU = 0.000 for C22 Least-squares cycle 7 Maximum vector length = 511 Memory required = 3482 / 308595 wR2 = 0.1078 before cycle 7 for 4663 data and 247 / 247 parameters GooF = S = 1.121; Restrained GooF = 1.121 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0566 * P )^2 + 0.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41563 0.00072 0.000 OSF 2 0.43846 0.05748 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.001 for tors H22A Max. shift = 0.000 A for H22B Max. dU = 0.000 for C1 Least-squares cycle 8 Maximum vector length = 511 Memory required = 3482 / 308595 wR2 = 0.1078 before cycle 8 for 4663 data and 247 / 247 parameters GooF = S = 1.121; Restrained GooF = 1.121 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0566 * P )^2 + 0.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.41563 0.00072 0.000 OSF 2 0.43846 0.05748 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.001 for x S1 Max. shift = 0.000 A for H22A Max. dU = 0.000 for O1 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1 0.7301 0.2386 0.4697 13 1.000 0.000 C1 C2 C5 Cl1 H2A 0.8088 0.1253 0.3114 23 0.990 0.000 C2 C1 C3 H2B 0.7974 0.0028 0.3876 23 0.990 0.000 C2 C1 C3 H3A 1.0535 0.0656 0.4240 23 0.990 0.000 C3 N1 C2 H3B 1.0060 0.1970 0.4666 23 0.990 0.000 C3 N1 C2 H4 0.8949 0.0838 0.7494 13 1.000 0.000 C4 N1 C8 C5 H5 0.6517 0.1578 0.6415 13 1.000 0.000 C5 C6 C1 C4 H6A 0.5712 -0.0388 0.5550 23 0.990 0.000 C6 C7 C5 H6B 0.7447 -0.0805 0.5881 23 0.990 0.000 C6 C7 C5 H7A 0.7440 -0.0575 0.7994 137 0.980 0.000 C7 C6 H7A H7B 0.5973 -0.1357 0.7448 137 0.980 0.000 C7 C6 H7A H7C 0.5802 0.0048 0.7735 137 0.980 0.000 C7 C6 H7A H8A 1.0361 0.2689 0.7062 23 0.990 0.000 C8 C9 C4 H8B 0.8816 0.3079 0.6183 23 0.990 0.000 C8 C9 C4 H9A 0.7509 0.3065 0.7870 23 0.990 0.000 C9 C10 C8 H9B 0.8963 0.2533 0.8764 23 0.990 0.000 C9 C10 C8 H11 1.1110 0.3877 0.9554 43 0.950 0.000 C11 C12 C10 H12 1.2024 0.5818 0.9957 43 0.950 0.000 C12 C11 C13 H13 1.0644 0.7483 0.9048 43 0.950 0.000 C13 C14 C12 H14 0.8309 0.7165 0.7753 43 0.950 0.000 C14 C13 C15 H15 0.7402 0.5214 0.7350 43 0.950 0.000 C15 C14 C10 H17 1.3211 0.1808 0.5950 43 0.950 0.000 C17 C16 C18 H18 1.4577 0.3408 0.7002 43 0.950 0.000 C18 C17 C19 H20 1.3611 0.2143 1.0253 43 0.950 0.000 C20 C21 C19 H22A 1.6104 0.3663 0.9852 137 0.980 0.000 C22 C19 H22A H22B 1.4550 0.4290 1.0048 137 0.980 0.000 C22 C19 H22A H22C 1.5276 0.4601 0.8845 137 0.980 0.000 C22 C19 H22A H21 1.2145 0.0607 0.9208 43 0.950 0.000 C21 C20 C16 2007src1052 in P2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq S1 1.13593 -0.00421 0.66579 1.00000 0.02578 0.01444 0.04119 -0.00412 0.00355 0.00205 0.02739 0.00103 0.00007 0.00005 0.00006 0.00000 0.00028 0.00024 0.00032 0.00024 0.00023 0.00022 0.00014 Cl1 0.51558 0.13204 0.38166 1.00000 0.03303 0.04293 0.03644 0.00630 -0.01117 -0.00532 0.03947 0.00106 0.00007 0.00006 0.00006 0.00000 0.00032 0.00036 0.00030 0.00028 0.00024 0.00027 0.00017 C1 0.70706 0.15020 0.46600 1.00000 0.02660 0.02784 0.02277 0.00355 -0.00389 -0.00633 0.02668 0.00392 0.00026 0.00022 0.00020 0.00000 0.00112 0.00123 0.00098 0.00093 0.00086 0.00096 0.00049 H1 0.73008 0.23864 0.46966 1.00000 0.03202 0.00000 0.00000 C2 0.81901 0.09041 0.39579 1.00000 0.03950 0.03689 0.01913 -0.00157 0.00491 -0.00968 0.03185 0.00424 0.00029 0.00024 0.00020 0.00000 0.00140 0.00141 0.00099 0.00095 0.00096 0.00108 0.00056 H2A 0.80882 0.12531 0.31144 1.00000 0.03822 0.00000 0.00000 H2B 0.79738 0.00281 0.38763 1.00000 0.03822 0.00000 0.00000 C3 0.97998 0.11008 0.46534 1.00000 0.03199 0.03096 0.02522 -0.00121 0.01159 -0.00525 0.02860 0.00419 0.00028 0.00023 0.00020 0.00000 0.00123 0.00129 0.00105 0.00099 0.00093 0.00099 0.00051 H3A 1.05353 0.06564 0.42402 1.00000 0.03432 0.00000 0.00000 H3B 1.00597 0.19704 0.46660 1.00000 0.03432 0.00000 0.00000 N1 0.98574 0.06478 0.59373 1.00000 0.02365 0.02042 0.02411 -0.00140 0.00654 0.00139 0.02244 0.00337 0.00021 0.00017 0.00017 0.00000 0.00096 0.00093 0.00088 0.00075 0.00075 0.00076 0.00040 C4 0.88374 0.12561 0.66729 1.00000 0.02264 0.01818 0.01869 0.00059 0.00476 0.00116 0.01969 0.00375 0.00023 0.00020 0.00018 0.00000 0.00099 0.00098 0.00086 0.00084 0.00075 0.00084 0.00040 H4 0.89491 0.08385 0.74942 1.00000 0.02363 0.00000 0.00000 C5 0.71896 0.10528 0.59990 1.00000 0.02282 0.01911 0.02118 -0.00148 0.00386 -0.00256 0.02102 0.00367 0.00025 0.00019 0.00018 0.00000 0.00104 0.00107 0.00094 0.00082 0.00080 0.00080 0.00044 H5 0.65170 0.15782 0.64146 1.00000 0.02523 0.00000 0.00000 C6 0.66779 -0.02537 0.61261 1.00000 0.02912 0.02338 0.02628 0.00156 0.00702 -0.00801 0.02599 0.00417 0.00028 0.00020 0.00021 0.00000 0.00116 0.00126 0.00105 0.00090 0.00090 0.00091 0.00049 H6A 0.57118 -0.03883 0.55499 1.00000 0.03119 0.00000 0.00000 H6B 0.74469 -0.08053 0.58813 1.00000 0.03119 0.00000 0.00000 C7 0.64533 -0.05622 0.74441 1.00000 0.03117 0.02343 0.03251 0.00842 0.00835 -0.00105 0.02870 0.00466 0.00029 0.00023 0.00022 0.00000 0.00127 0.00111 0.00119 0.00096 0.00100 0.00093 0.00050 H7A 0.74405 -0.05754 0.79943 1.00000 0.04304 0.00000 0.00000 H7B 0.59730 -0.13575 0.74481 1.00000 0.04304 0.00000 0.00000 H7C 0.58023 0.00484 0.77353 1.00000 0.04304 0.00000 0.00000 C8 0.92433 0.25951 0.69222 1.00000 0.02136 0.01736 0.02119 -0.00038 0.00411 -0.00071 0.01991 0.00390 0.00025 0.00019 0.00019 0.00000 0.00104 0.00099 0.00096 0.00082 0.00080 0.00081 0.00042 H8A 1.03605 0.26891 0.70619 1.00000 0.02390 0.00000 0.00000 H8B 0.88162 0.30786 0.61835 1.00000 0.02390 0.00000 0.00000 C9 0.86320 0.30735 0.80483 1.00000 0.04566 0.03045 0.03173 -0.00824 0.01867 -0.01366 0.03453 0.00480 0.00034 0.00024 0.00024 0.00000 0.00158 0.00134 0.00121 0.00107 0.00115 0.00113 0.00060 H9A 0.75087 0.30650 0.78697 1.00000 0.04144 0.00000 0.00000 H9B 0.89633 0.25327 0.87640 1.00000 0.04144 0.00000 0.00000 C10 0.91694 0.43362 0.83856 1.00000 0.03128 0.02120 0.01908 -0.00245 0.01223 0.00138 0.02292 0.00425 0.00027 0.00020 0.00019 0.00000 0.00121 0.00115 0.00095 0.00085 0.00088 0.00092 0.00046 C11 1.05403 0.45437 0.91765 1.00000 0.03869 0.02175 0.02153 0.00134 0.00339 0.00648 0.02752 0.00448 0.00030 0.00022 0.00020 0.00000 0.00135 0.00109 0.00102 0.00088 0.00098 0.00097 0.00050 H11 1.11100 0.38773 0.95538 1.00000 0.03303 0.00000 0.00000 C12 1.10832 0.56974 0.94204 1.00000 0.04126 0.03044 0.02489 -0.00623 0.00446 -0.00454 0.03233 0.00455 0.00030 0.00025 0.00022 0.00000 0.00148 0.00127 0.00111 0.00101 0.00102 0.00110 0.00055 H12 1.20243 0.58183 0.99573 1.00000 0.03880 0.00000 0.00000 C13 1.02638 0.66870 0.88865 1.00000 0.07431 0.01549 0.02592 -0.00313 0.02166 -0.00395 0.03704 0.00505 0.00036 0.00022 0.00022 0.00000 0.00205 0.00113 0.00116 0.00090 0.00127 0.00113 0.00066 H13 1.06435 0.74829 0.90480 1.00000 0.04444 0.00000 0.00000 C14 0.88867 0.64968 0.81163 1.00000 0.05922 0.02781 0.02794 0.00830 0.01745 0.01882 0.03715 0.00542 0.00034 0.00024 0.00023 0.00000 0.00171 0.00141 0.00112 0.00103 0.00117 0.00124 0.00063 H14 0.83090 0.71652 0.77527 1.00000 0.04458 0.00000 0.00000 C15 0.83514 0.53329 0.78758 1.00000 0.02996 0.04194 0.02420 0.00291 0.00651 0.00604 0.03181 0.00487 0.00030 0.00024 0.00022 0.00000 0.00129 0.00152 0.00114 0.00101 0.00099 0.00102 0.00057 H15 0.74022 0.52139 0.73495 1.00000 0.03817 0.00000 0.00000 C16 1.25408 0.10688 0.74809 1.00000 0.01966 0.01948 0.03185 -0.00098 0.00323 0.00552 0.02380 0.00402 0.00024 0.00020 0.00020 0.00000 0.00104 0.00105 0.00109 0.00089 0.00088 0.00081 0.00046 C17 1.32735 0.18899 0.68215 1.00000 0.02118 0.02693 0.03017 -0.00363 0.00518 0.00265 0.02600 0.00423 0.00025 0.00021 0.00022 0.00000 0.00110 0.00118 0.00111 0.00097 0.00091 0.00091 0.00048 H17 1.32105 0.18077 0.59496 1.00000 0.03120 0.00000 0.00000 C18 1.40992 0.28322 0.74519 1.00000 0.02364 0.02194 0.03995 -0.00463 0.01121 -0.00078 0.02783 0.00441 0.00027 0.00022 0.00023 0.00000 0.00113 0.00114 0.00131 0.00100 0.00099 0.00089 0.00050 H18 1.45767 0.34082 0.70022 1.00000 0.03340 0.00000 0.00000 C19 1.42342 0.29415 0.87399 1.00000 0.02286 0.03157 0.03896 -0.01122 0.01174 -0.00187 0.03037 0.00443 0.00028 0.00023 0.00023 0.00000 0.00112 0.00128 0.00131 0.00109 0.00101 0.00097 0.00053 C20 1.35105 0.20879 0.93755 1.00000 0.02875 0.03978 0.02828 -0.00436 0.00709 -0.00041 0.03201 0.00472 0.00028 0.00025 0.00023 0.00000 0.00124 0.00139 0.00114 0.00106 0.00099 0.00108 0.00053 H20 1.36114 0.21426 1.02525 1.00000 0.03841 0.00000 0.00000 C22 1.51187 0.39636 0.94320 1.00000 0.04144 0.05535 0.05378 -0.03156 0.01981 -0.01956 0.04882 0.00497 0.00035 0.00030 0.00030 0.00000 0.00161 0.00189 0.00169 0.00152 0.00137 0.00141 0.00080 H22A 1.61045 0.36632 0.98518 1.00000 0.07323 0.00000 0.00000 H22B 1.45504 0.42904 1.00484 1.00000 0.07323 0.00000 0.00000 H22C 1.52758 0.46011 0.88454 1.00000 0.07323 0.00000 0.00000 C21 1.26523 0.11664 0.87620 1.00000 0.02269 0.02673 0.03223 0.00599 0.00599 0.00415 0.02707 0.00442 0.00026 0.00023 0.00021 0.00000 0.00106 0.00115 0.00107 0.00099 0.00088 0.00092 0.00047 H21 1.21448 0.06069 0.92076 1.00000 0.03248 0.00000 0.00000 O1 1.21302 -0.05397 0.57177 1.00000 0.03284 0.03206 0.06068 -0.02360 0.01116 0.00606 0.04149 0.00348 0.00021 0.00017 0.00019 0.00000 0.00099 0.00092 0.00122 0.00092 0.00088 0.00078 0.00047 O2 1.08724 -0.08184 0.75612 1.00000 0.03771 0.02009 0.05630 0.01393 0.00144 -0.00361 0.03880 0.00344 0.00022 0.00016 0.00019 0.00000 0.00103 0.00085 0.00116 0.00084 0.00088 0.00073 0.00045 Final Structure Factor Calculation for 2007src1052 in P2(1) Total number of l.s. parameters = 247 Maximum vector length = 511 Memory required = 3237 / 27090 wR2 = 0.1078 before cycle 9 for 4663 data and 2 / 247 parameters GooF = S = 1.121; Restrained GooF = 1.121 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0566 * P )^2 + 0.18 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0404 for 4248 Fo > 4sig(Fo) and 0.0470 for all 4663 data wR2 = 0.1078, GooF = S = 1.121, Restrained GooF = 1.121 for all data Occupancy sum of asymmetric unit = 27.00 for non-hydrogen and 28.00 for hydrogen atoms Principal mean square atomic displacements U 0.0428 0.0260 0.0134 S1 0.0602 0.0382 0.0200 Cl1 0.0398 0.0228 0.0174 C1 0.0480 0.0286 0.0189 C2 0.0384 0.0282 0.0193 C3 0.0260 0.0228 0.0185 N1 0.0231 0.0182 0.0178 C4 0.0242 0.0213 0.0175 C5 0.0348 0.0269 0.0163 C6 0.0377 0.0310 0.0174 C7 0.0218 0.0207 0.0172 C8 0.0587 0.0228 0.0220 C9 0.0341 0.0223 0.0125 C10 0.0414 0.0223 0.0190 C11 0.0429 0.0334 0.0207 C12 0.0761 0.0204 0.0146 C13 0.0698 0.0232 0.0185 C14 0.0447 0.0275 0.0232 C15 0.0326 0.0248 0.0140 C16 0.0328 0.0260 0.0192 C17 0.0420 0.0218 0.0197 C18 0.0477 0.0252 0.0182 C19 0.0413 0.0297 0.0250 C20 0.0920 0.0320 0.0225 C22 0.0364 0.0248 0.0200 C21 0.0744 0.0362 0.0138 O1 0.0649 0.0366 0.0149 O2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.027 0.041 0.051 0.063 0.075 0.090 0.110 0.139 0.191 1.000 Number in group 467. 488. 444. 485. 457. 466. 467. 470. 450. 469. GooF 1.116 1.093 1.178 1.171 1.162 1.115 0.931 0.953 0.951 1.441 K 1.161 0.986 0.976 0.999 0.991 1.010 1.015 1.022 1.013 0.960 Resolution(A) 0.77 0.80 0.84 0.88 0.93 0.98 1.06 1.16 1.33 1.68 inf Number in group 467. 470. 462. 470. 465. 469. 458. 472. 463. 467. GooF 0.927 0.970 0.986 1.065 1.009 1.164 0.979 0.993 1.167 1.724 K 0.980 0.997 0.997 1.011 1.007 1.015 1.017 1.015 1.017 0.943 R1 0.101 0.090 0.071 0.063 0.046 0.043 0.030 0.027 0.029 0.040 ** Extinction (EXTI) or solvent water (SWAT) correction may be required ** Recommended weighting scheme: WGHT 0.0562 0.1764 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 2 598.55 13160.67 22.43 1.000 4.55 0 10 4 27.99 6.63 5.04 0.022 1.02 -4 0 7 44.39 11.48 4.95 0.030 1.38 -5 3 11 31.66 3.90 4.73 0.017 0.90 -4 -7 7 90.06 52.36 4.71 0.063 1.04 -4 2 3 96.90 52.03 4.55 0.063 1.91 -1 -5 4 160.87 102.79 4.46 0.088 1.71 1 -8 7 64.65 37.40 4.21 0.053 1.01 -4 3 7 75.75 50.50 4.04 0.062 1.29 -2 7 9 51.06 77.98 3.97 0.077 0.96 -4 7 7 89.26 52.34 3.86 0.063 1.04 1 7 7 246.56 175.70 3.86 0.116 1.08 -4 4 7 247.01 180.97 3.78 0.117 1.23 5 -3 7 43.42 26.37 3.76 0.045 1.03 1 -2 6 48.46 32.47 3.73 0.050 1.63 0 -10 4 26.57 6.76 3.72 0.023 1.02 -5 3 4 76.43 40.77 3.69 0.056 1.47 -4 3 4 43.31 26.83 3.67 0.045 1.67 -4 6 7 107.58 68.85 3.67 0.072 1.10 5 -5 7 40.62 22.70 3.65 0.042 0.97 -5 -3 11 21.77 3.87 3.63 0.017 0.90 3 -8 4 61.79 38.61 3.56 0.054 1.11 -2 9 8 28.13 49.74 3.55 0.061 0.91 -1 5 4 151.20 102.91 3.49 0.088 1.71 8 1 5 17.47 32.82 3.42 0.050 0.92 -4 -6 7 96.42 68.86 3.35 0.072 1.10 -5 -3 7 31.41 12.37 3.35 0.031 1.20 -4 0 11 21.96 10.01 3.30 0.028 0.96 -1 0 7 5.61 12.01 3.29 0.030 1.56 -1 -3 10 37.98 22.47 3.25 0.041 1.05 10 2 4 2.89 17.51 3.22 0.036 0.79 1 0 5 0.34 4.02 3.13 0.017 2.02 -7 6 10 15.65 31.49 3.10 0.049 0.81 -5 7 7 77.11 54.74 3.09 0.064 0.99 1 -7 7 228.29 175.97 3.08 0.116 1.08 -6 -10 2 8.45 21.10 3.06 0.040 0.89 3 4 4 203.11 155.12 3.05 0.109 1.53 5 5 7 47.31 23.00 3.04 0.042 0.97 6 -9 3 48.22 71.97 3.01 0.074 0.89 0 -7 10 121.74 163.56 3.01 0.111 0.89 -4 -10 5 13.72 23.85 3.01 0.043 0.93 -6 3 6 33.88 21.22 3.00 0.040 1.18 -7 4 7 56.93 38.60 3.00 0.054 1.00 -4 -2 3 84.48 51.72 2.97 0.063 1.91 -4 -1 7 148.03 105.61 2.96 0.090 1.37 5 3 7 39.34 26.05 2.96 0.044 1.03 1 -8 11 50.54 23.11 2.89 0.042 0.79 3 0 1 8.53 14.37 2.87 0.033 2.72 3 13 1 27.73 41.82 2.86 0.056 0.81 -4 -3 7 69.28 49.80 2.85 0.062 1.29 Bond lengths and angles S1 - Distance Angles O2 1.4321 (0.0019) O1 1.4414 (0.0019) 120.08 (0.12) N1 1.6271 (0.0019) 107.05 (0.11) 106.82 (0.11) C16 1.7649 (0.0023) 107.00 (0.11) 108.23 (0.11) 107.02 (0.10) S1 - O2 O1 N1 Cl1 - Distance Angles C1 1.8122 (0.0022) Cl1 - C1 - Distance Angles C2 1.5139 (0.0036) C5 1.5331 (0.0029) 113.48 (0.19) Cl1 1.8122 (0.0022) 110.01 (0.15) 110.86 (0.16) H1 1.0000 107.41 107.41 107.41 C1 - C2 C5 Cl1 C2 - Distance Angles C1 1.5139 (0.0036) C3 1.5246 (0.0033) 109.51 (0.18) H2A 0.9900 109.77 109.77 H2B 0.9900 109.77 109.77 108.23 C2 - C1 C3 H2A C3 - Distance Angles N1 1.4838 (0.0029) C2 1.5246 (0.0033) 107.55 (0.19) H3A 0.9900 110.20 110.20 H3B 0.9900 110.20 110.20 108.49 C3 - N1 C2 H3A N1 - Distance Angles C4 1.4774 (0.0027) C3 1.4838 (0.0029) 115.86 (0.18) S1 1.6271 (0.0019) 119.03 (0.14) 120.65 (0.16) N1 - C4 C3 C4 - Distance Angles N1 1.4774 (0.0027) C8 1.5395 (0.0030) 112.75 (0.18) C5 1.5475 (0.0028) 107.47 (0.16) 113.64 (0.17) H4 1.0000 107.57 107.57 107.57 C4 - N1 C8 C5 C5 - Distance Angles C6 1.5306 (0.0031) C1 1.5331 (0.0029) 114.85 (0.18) C4 1.5475 (0.0028) 111.67 (0.18) 108.26 (0.18) H5 1.0000 107.24 107.24 107.24 C5 - C6 C1 C4 C6 - Distance Angles C7 1.5276 (0.0032) C5 1.5306 (0.0031) 112.73 (0.19) H6A 0.9900 109.04 109.04 H6B 0.9900 109.04 109.04 107.81 C6 - C7 C5 H6A C7 - Distance Angles C6 1.5276 (0.0032) 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 C9 1.5251 (0.0032) C4 1.5395 (0.0030) 111.80 (0.18) H8A 0.9900 109.26 109.26 H8B 0.9900 109.26 109.26 107.93 C8 - C9 C4 H8A C9 - Distance Angles C10 1.5036 (0.0034) C8 1.5251 (0.0032) 112.18 (0.20) H9A 0.9900 109.17 109.17 H9B 0.9900 109.17 109.17 107.88 C9 - C10 C8 H9A C10 - Distance Angles C15 1.3874 (0.0033) C11 1.3936 (0.0034) 117.78 (0.21) C9 1.5036 (0.0034) 121.09 (0.22) 121.07 (0.22) C10 - C15 C11 C11 - Distance Angles C12 1.3763 (0.0036) C10 1.3936 (0.0034) 121.14 (0.22) H11 0.9500 119.43 119.43 C11 - C12 C10 C12 - Distance Angles C11 1.3763 (0.0036) C13 1.3901 (0.0037) 120.46 (0.23) H12 0.9500 119.77 119.77 C12 - C11 C13 C13 - Distance Angles C14 1.3844 (0.0041) C12 1.3901 (0.0037) 119.09 (0.23) H13 0.9500 120.46 120.46 C13 - C14 C12 C14 - Distance Angles C13 1.3844 (0.0041) C15 1.3841 (0.0040) 120.01 (0.23) H14 0.9500 120.00 120.00 C14 - C13 C15 C15 - Distance Angles C14 1.3841 (0.0040) C10 1.3874 (0.0033) 121.51 (0.24) H15 0.9500 119.24 119.24 C15 - C14 C10 C16 - Distance Angles C17 1.3917 (0.0033) C21 1.3919 (0.0032) 120.78 (0.21) S1 1.7649 (0.0023) 118.99 (0.17) 120.10 (0.18) C16 - C17 C21 C17 - Distance Angles C16 1.3917 (0.0033) C18 1.3912 (0.0033) 119.33 (0.22) H17 0.9500 120.33 120.33 C17 - C16 C18 C18 - Distance Angles C17 1.3912 (0.0033) C19 1.3985 (0.0035) 120.77 (0.23) H18 0.9500 119.62 119.62 C18 - C17 C19 C19 - Distance Angles C20 1.3958 (0.0037) C18 1.3985 (0.0035) 118.38 (0.22) C22 1.5083 (0.0035) 120.40 (0.23) 121.22 (0.24) C19 - C20 C18 C20 - Distance Angles C21 1.3801 (0.0036) C19 1.3958 (0.0037) 121.66 (0.23) H20 0.9500 119.17 119.17 C20 - C21 C19 C22 - Distance Angles C19 1.5083 (0.0035) H22A 0.9800 109.47 H22B 0.9800 109.47 109.47 H22C 0.9800 109.47 109.47 109.47 C22 - C19 H22A H22B C21 - Distance Angles C20 1.3801 (0.0036) C16 1.3919 (0.0032) 119.04 (0.23) H21 0.9500 120.48 120.48 C21 - C20 C16 O1 - Distance Angles S1 1.4414 (0.0019) O1 - O2 - Distance Angles S1 1.4321 (0.0019) O2 - FMAP and GRID set by program FMAP 2 1 23 GRID -2.500 -2 -2 2.500 2 2 R1 = 0.0443 for 2566 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.59 at 0.1350 1.0015 0.9408 [ 1.02 A from H21 ] Deepest hole -0.52 at 0.4511 0.0967 0.3572 [ 0.71 A from CL1 ] Mean = 0.00, Rms deviation from mean = 0.18 e/A^3, Highest memory used = 3198 / 23542 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 1.1350 0.0015 0.9408 1.00000 0.05 0.59 1.02 H21 1.94 C21 2.20 O2 2.53 C11 Q2 1 1.5256 0.1385 1.1105 1.00000 0.05 0.54 1.81 H20 2.03 H22C 2.37 C20 2.66 H22B Q3 1 0.5153 0.1344 0.6587 1.00000 0.05 0.54 1.29 H5 1.83 H17 1.84 C17 1.93 H7C Q4 1 0.9743 0.0903 0.8623 1.00000 0.05 0.49 1.32 H4 1.95 H9B 2.16 H21 2.18 C4 Q5 1 1.2433 0.1158 1.0294 1.00000 0.05 0.46 1.32 H21 1.52 H20 1.72 C21 1.82 C20 Q6 1 0.7010 0.1501 0.7415 1.00000 0.05 0.45 1.11 H5 1.66 C5 1.84 H9A 1.87 H4 Q7 1 1.1335 -0.0037 0.3953 1.00000 0.05 0.44 1.13 H3A 1.98 H15 2.02 O1 2.09 H8B Q8 1 1.2249 0.1049 0.4645 1.00000 0.05 0.44 1.58 H3A 1.75 H17 2.13 O1 2.19 C3 Q9 1 1.2783 0.1153 0.5010 1.00000 0.05 0.43 1.26 H17 2.12 H3A 2.12 C17 2.15 O1 Q10 1 1.1141 0.1053 0.4290 1.00000 0.05 0.43 0.69 H3A 1.33 C3 1.51 H3B 2.34 N1 Q11 1 0.9564 0.1421 0.8350 1.00000 0.05 0.43 1.19 H4 1.45 H9B 1.85 C4 2.01 C8 Q12 1 1.3226 0.0636 0.5548 1.00000 0.05 0.43 1.37 H17 1.66 O1 1.96 C17 2.35 S1 Q13 1 1.1108 0.1626 0.4513 1.00000 0.05 0.42 1.05 H3B 1.20 H3A 1.34 C3 2.24 H17 Q14 1 0.7921 0.1073 0.7885 1.00000 0.05 0.41 1.11 H4 1.68 C4 1.88 H7A 1.95 H5 Q15 1 1.3716 0.0828 0.5495 1.00000 0.05 0.41 1.31 H17 1.96 C17 2.12 O1 2.23 H6A Q16 1 1.3755 0.5847 0.8143 1.00000 0.05 0.41 2.00 H22C 2.01 H2A 2.56 CL1 2.63 H2B Q17 1 0.8910 0.1219 0.3000 1.00000 0.05 0.41 0.77 H2A 1.36 C2 1.85 C3 1.91 H2B Q18 1 1.1900 0.0466 0.4801 1.00000 0.05 0.41 1.29 H3A 1.49 O1 1.99 C3 2.16 H17 Q19 1 0.6902 0.1482 0.2422 1.00000 0.05 0.40 1.22 H2A 1.97 C2 2.35 H2B 2.37 CL1 Q20 1 1.1276 0.1416 0.9220 1.00000 0.05 0.40 1.19 H21 1.43 C21 2.11 C20 2.34 H20 Shortest distances between peaks (including symmetry equivalents) 12 15 0.50 8 9 0.58 4 11 0.65 10 13 0.68 8 18 0.75 9 12 0.87 9 15 0.98 8 10 1.00 6 14 1.00 10 18 1.03 16 19 1.05 9 18 1.09 7 18 1.12 8 13 1.19 2 16 1.25 7 10 1.28 8 12 1.29 12 18 1.33 5 20 1.45 13 18 1.47 8 15 1.49 11 14 1.52 4 20 1.52 9 10 1.55 1 20 1.56 7 8 1.57 9 13 1.59 11 20 1.66 3 15 1.70 4 14 1.70 15 18 1.72 3 6 1.76 1 5 1.78 17 19 1.82 1 4 1.83 2 19 1.88 7 13 1.96 3 12 2.05 7 9 2.06 10 12 2.17 10 17 2.25 12 13 2.31 7 12 2.34 6 11 2.34 1 11 2.38 13 17 2.39 10 15 2.46 3 9 2.50 16 17 2.53 2 5 2.54 13 15 2.55 7 17 2.64 3 14 2.65 4 6 2.66 7 15 2.66 4 5 2.78 Time profile in seconds ----------------------- 0.02: Read and process instructions 0.00: Fit rigid groups 0.00: Interpret restraints etc. 0.00: Generate connectivity array 0.02: 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. 0.11: 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 0.00: Generate idealized H-atoms 3.38: Structure factors and derivatives 2.39: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.09: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.08: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.00: Fourier summations 0.03: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src1052 finished at 13:03:08 Total CPU time: 6.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++