++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XL - CRYSTAL STRUCTURE REFINEMENT - SHELXTL Ver. 6.12 W95/98/NT/2000/ME + + Copyright(c) 2001 Bruker Analytical X-ray Solutions All Rights Reserved + + 2007src1053 started at 11:03:56 on 20-Aug-2007 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src1053 in Pbca CELL 0.71073 13.0538 15.5288 19.1088 90.000 90.000 90.000 ZERR 8.00 0.0003 0.0003 0.0004 0.000 0.000 0.000 LATT 1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N O S CL UNIT 160 240 8 16 8 8 V = 3873.54 F(000) = 1648.0 Mu = 0.32 mm-1 Cell Wt = 3071.68 Rho = 1.317 BOND $H OMIT -3 55 SHEL 7 0.77 OMIT 2 0 0 OMIT 0 6 0 ACTA SIZE 0.6x0.5x0.5 TEMP -153 L.S. 8 FMAP 2 PLAN 20 WGHT 0.0508 3.0009 FVAR 0.11962 S1 5 0.27994 0.82924 0.09615 11.00000 0.01760 0.01001 = 0.02019 0.00097 0.00292 0.00112 CL1 6 0.06249 0.99941 0.19543 11.00000 0.03226 0.02219 = 0.03598 0.01086 0.01194 0.00487 O1 4 0.29180 0.80921 0.02315 11.00000 0.02862 0.01597 = 0.02229 -0.00335 0.00850 0.00063 O2 4 0.35023 0.79331 0.14609 11.00000 0.01930 0.01715 = 0.03254 0.00521 -0.00276 0.00325 N1 3 0.28752 0.93273 0.10536 11.00000 0.02044 0.01019 = 0.01734 0.00163 -0.00071 0.00000 C16 1 0.02928 0.76014 0.20594 11.00000 0.02444 0.01918 = 0.01776 0.00171 0.00276 0.00144 AFIX 43 H16 2 0.00945 0.75686 0.25370 11.00000 -1.20000 AFIX 0 C14 1 0.15541 0.79478 0.11896 11.00000 0.01743 0.00839 = 0.01872 0.00038 0.00048 0.00171 C18 1 -0.01107 0.74470 0.08428 11.00000 0.02243 0.02031 = 0.02134 0.00095 -0.00583 -0.00210 AFIX 43 H18 2 -0.05799 0.72960 0.04832 11.00000 -1.20000 AFIX 0 C15 1 0.12719 0.78770 0.18905 11.00000 0.02237 0.01581 = 0.01560 -0.00044 -0.00191 -0.00074 AFIX 43 H15 2 0.17469 0.80166 0.22497 11.00000 -1.20000 AFIX 0 C2 1 0.21092 1.07308 0.11083 11.00000 0.02114 0.00965 = 0.01988 0.00033 0.00080 -0.00019 AFIX 13 H2 2 0.22834 1.12400 0.08109 11.00000 -1.20000 AFIX 0 C9 1 0.19320 1.06197 -0.05546 11.00000 0.02132 0.01845 = 0.01950 0.00211 -0.00184 0.00017 AFIX 23 H9A 2 0.12590 1.03273 -0.05781 11.00000 -1.20000 H9B 2 0.18272 1.11952 -0.03435 11.00000 -1.20000 AFIX 0 C17 1 -0.04065 0.73711 0.15400 11.00000 0.01896 0.01382 = 0.02526 0.00304 0.00080 0.00168 C3 1 0.29648 1.06416 0.16551 11.00000 0.02571 0.01540 = 0.02374 -0.00327 -0.00273 -0.00112 AFIX 23 H3A 2 0.36021 1.09183 0.14868 11.00000 -1.20000 H3B 2 0.27598 1.09153 0.21016 11.00000 -1.20000 AFIX 0 C8 1 0.26628 1.00928 -0.00936 11.00000 0.02151 0.01080 = 0.01755 0.00034 0.00034 -0.00013 AFIX 13 H8 2 0.27585 0.95216 -0.03261 11.00000 -1.20000 AFIX 0 C19 1 0.08582 0.77395 0.06657 11.00000 0.02492 0.01642 = 0.01492 0.00159 -0.00116 0.00100 AFIX 43 H19 2 0.10462 0.77975 0.01878 11.00000 -1.20000 AFIX 0 C6 1 0.02197 1.11017 0.08807 11.00000 0.02150 0.01949 = 0.02323 -0.00115 0.00058 -0.00088 AFIX 23 H6A 2 0.04691 1.15701 0.05733 11.00000 -1.20000 H6B 2 0.01074 1.05869 0.05849 11.00000 -1.20000 AFIX 0 C5 1 0.10444 1.08969 0.14181 11.00000 0.02617 0.01265 = 0.02188 0.00042 0.00327 0.00027 AFIX 13 H5 2 0.11040 1.14083 0.17335 11.00000 -1.20000 AFIX 0 C4 1 0.31266 0.96769 0.17553 11.00000 0.02811 0.01741 = 0.02014 -0.00230 -0.00539 0.00055 AFIX 23 H4A 2 0.38439 0.95470 0.18862 11.00000 -1.20000 H4B 2 0.26615 0.94433 0.21179 11.00000 -1.20000 AFIX 0 C1 1 0.22050 0.99194 0.06361 11.00000 0.01777 0.00967 = 0.01882 0.00116 -0.00125 -0.00038 AFIX 13 H1 2 0.15136 0.96506 0.05807 11.00000 -1.20000 AFIX 0 C7 1 -0.07965 1.13716 0.11974 11.00000 0.02650 0.02780 = 0.03019 -0.00394 -0.00095 0.00665 AFIX 137 H7A 2 -0.10225 1.09344 0.15335 11.00000 -1.50000 H7B 2 -0.13090 1.14298 0.08257 11.00000 -1.50000 H7C 2 -0.07143 1.19248 0.14376 11.00000 -1.50000 AFIX 0 C20 1 -0.14470 0.70220 0.17307 11.00000 0.02241 0.02931 = 0.03620 0.00471 0.00190 -0.00411 AFIX 137 H20A 2 -0.13914 0.64056 0.18342 11.00000 -1.50000 H20B 2 -0.19195 0.71075 0.13383 11.00000 -1.50000 H20C 2 -0.17067 0.73258 0.21438 11.00000 -1.50000 AFIX 0 C13 1 0.37107 1.05310 -0.00712 11.00000 0.02017 0.02249 = 0.02321 0.00487 0.00045 -0.00199 AFIX 23 H13A 2 0.41869 1.01799 0.02138 11.00000 -1.20000 H13B 2 0.36439 1.11022 0.01544 11.00000 -1.20000 AFIX 0 C11 1 0.34182 1.11415 -0.12778 11.00000 0.03409 0.03072 = 0.02683 0.01173 0.00352 -0.00210 AFIX 23 H11A 2 0.33543 1.17396 -0.11038 11.00000 -1.20000 H11B 2 0.37003 1.11644 -0.17583 11.00000 -1.20000 AFIX 0 C10 1 0.23643 1.07228 -0.12947 11.00000 0.03199 0.02450 = 0.01987 0.00528 -0.00132 0.00173 AFIX 23 H10A 2 0.24146 1.01504 -0.15203 11.00000 -1.20000 H10B 2 0.18929 1.10817 -0.15769 11.00000 -1.20000 AFIX 0 C12 1 0.41511 1.06423 -0.08072 11.00000 0.02492 0.03146 = 0.02767 0.00911 0.00508 -0.00262 AFIX 23 H12A 2 0.48118 1.09532 -0.07784 11.00000 -1.20000 H12B 2 0.42836 1.00686 -0.10143 11.00000 -1.20000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 2007src1053 in Pbca C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 CL 0.990 S1 - O2 O1 N1 C14 Cl1 - C5 O1 - S1 O2 - S1 N1 - C4 C1 S1 C16 - C15 C17 C14 - C19 C15 S1 C18 - C19 C17 C15 - C16 C14 C2 - C5 C3 C1 C9 - C10 C8 C17 - C18 C16 C20 C3 - C4 C2 C8 - C13 C9 C1 C19 - C18 C14 C6 - C7 C5 C5 - C6 C2 Cl1 C4 - N1 C3 C1 - N1 C8 C2 C7 - C6 C20 - C17 C13 - C8 C12 C11 - C10 C12 C10 - C11 C9 C12 - C11 C13 h k l Fo^2 Sigma Why rejected 11 8 0 0.20 0.05 observed but should be systematically absent 33620 Reflections read, of which 2202 rejected -16 =< h =< 16, -20 =< k =< 19, -24 =< l =< 24, Max. 2-theta = 54.97 1 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 13 7 3 4.28 0.24 3 1.31 1 Inconsistent equivalents 4422 Unique reflections, of which 0 suppressed R(int) = 0.0516 R(sigma) = 0.0367 Friedel opposites merged Maximum memory for data reduction = 2774 / 44015 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 = 3476 / 284617 wR2 = 0.1097 before cycle 1 for 4422 data and 228 / 228 parameters GooF = S = 1.027; Restrained GooF = 1.027 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0508 * P )^2 + 3.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.11986 0.00021 1.129 OSF Mean shift/esd = 0.120 Maximum = 1.129 for OSF Max. shift = 0.008 A for H7B Max. dU = 0.000 for C12 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3476 / 284617 wR2 = 0.1096 before cycle 2 for 4422 data and 228 / 228 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0508 * P )^2 + 3.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.11992 0.00021 0.287 OSF Mean shift/esd = 0.044 Maximum = 0.287 for OSF Max. shift = 0.004 A for H20B Max. dU = 0.000 for C12 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3476 / 284617 wR2 = 0.1096 before cycle 3 for 4422 data and 228 / 228 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0508 * P )^2 + 3.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.11992 0.00021 0.008 OSF Mean shift/esd = 0.003 Maximum = 0.077 for tors H20A Max. shift = 0.001 A for H20B Max. dU = 0.000 for C11 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3476 / 284617 wR2 = 0.1096 before cycle 4 for 4422 data and 228 / 228 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0508 * P )^2 + 3.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.11992 0.00021 0.001 OSF Mean shift/esd = 0.001 Maximum = 0.023 for tors H20A Max. shift = 0.000 A for H20B Max. dU = 0.000 for C20 Least-squares cycle 5 Maximum vector length = 511 Memory required = 3476 / 284617 wR2 = 0.1096 before cycle 5 for 4422 data and 228 / 228 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0508 * P )^2 + 3.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.11992 0.00021 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.007 for tors H20A Max. shift = 0.000 A for H20B Max. dU = 0.000 for C6 Least-squares cycle 6 Maximum vector length = 511 Memory required = 3476 / 284617 wR2 = 0.1096 before cycle 6 for 4422 data and 228 / 228 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0508 * P )^2 + 3.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.11992 0.00021 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.002 for tors H20A Max. shift = 0.000 A for H20B Max. dU = 0.000 for C15 Least-squares cycle 7 Maximum vector length = 511 Memory required = 3476 / 284617 wR2 = 0.1096 before cycle 7 for 4422 data and 228 / 228 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0508 * P )^2 + 3.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.11992 0.00021 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for tors H20A Max. shift = 0.000 A for H20C Max. dU = 0.000 for C3 Least-squares cycle 8 Maximum vector length = 511 Memory required = 3476 / 284617 wR2 = 0.1096 before cycle 8 for 4422 data and 228 / 228 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0508 * P )^2 + 3.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.11992 0.00021 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for y C8 Max. shift = 0.000 A for H20B 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 H16 0.0095 0.7569 0.2537 43 0.950 0.000 C16 C15 C17 H18 -0.0580 0.7296 0.0483 43 0.950 0.000 C18 C19 C17 H15 0.1747 0.8017 0.2250 43 0.950 0.000 C15 C16 C14 H2 0.2284 1.1240 0.0811 13 1.000 0.000 C2 C5 C3 C1 H9A 0.1260 1.0327 -0.0578 23 0.990 0.000 C9 C10 C8 H9B 0.1827 1.1195 -0.0344 23 0.990 0.000 C9 C10 C8 H3A 0.3602 1.0918 0.1487 23 0.990 0.000 C3 C4 C2 H3B 0.2759 1.0915 0.2102 23 0.990 0.000 C3 C4 C2 H8 0.2758 0.9521 -0.0326 13 1.000 0.000 C8 C13 C9 C1 H19 0.1047 0.7798 0.0188 43 0.950 0.000 C19 C18 C14 H6A 0.0469 1.1571 0.0573 23 0.990 0.000 C6 C7 C5 H6B 0.0107 1.0588 0.0585 23 0.990 0.000 C6 C7 C5 H5 0.1105 1.1408 0.1734 13 1.000 0.000 C5 C6 C2 Cl1 H4A 0.3843 0.9548 0.1886 23 0.990 0.000 C4 N1 C3 H4B 0.2661 0.9444 0.2118 23 0.990 0.000 C4 N1 C3 H1 0.1514 0.9651 0.0581 13 1.000 0.000 C1 N1 C8 C2 H7A -0.1027 1.0932 0.1529 137 0.980 0.000 C7 C6 H7A H7B -0.1307 1.1437 0.0825 137 0.980 0.000 C7 C6 H7A H7C -0.0713 1.1922 0.1442 137 0.980 0.000 C7 C6 H7A H20A -0.1390 0.6406 0.1840 137 0.980 0.000 C20 C17 H20A H20B -0.1918 0.7100 0.1336 137 0.980 0.000 C20 C17 H20A H20C -0.1711 0.7330 0.2140 137 0.980 0.000 C20 C17 H20A H13A 0.4186 1.0179 0.0214 23 0.990 0.000 C13 C8 C12 H13B 0.3644 1.1101 0.0154 23 0.990 0.000 C13 C8 C12 H11A 0.3353 1.1740 -0.1103 23 0.990 0.000 C11 C10 C12 H11B 0.3699 1.1167 -0.1758 23 0.990 0.000 C11 C10 C12 H10A 0.2416 1.0150 -0.1520 23 0.990 0.000 C10 C11 C9 H10B 0.1892 1.1081 -0.1577 23 0.990 0.000 C10 C11 C9 H12A 0.4812 1.0952 -0.0779 23 0.990 0.000 C12 C11 C13 H12B 0.4282 1.0068 -0.1015 23 0.990 0.000 C12 C11 C13 2007src1053 in Pbca ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq S1 0.27994 0.82924 0.09615 1.00000 0.01772 0.01010 0.02033 0.00097 0.00292 0.00112 0.01605 0.00073 0.00003 0.00003 0.00002 0.00000 0.00022 0.00021 0.00021 0.00015 0.00016 0.00016 0.00012 Cl1 0.06250 0.99941 0.19543 1.00000 0.03243 0.02226 0.03612 0.01087 0.01195 0.00487 0.03027 0.00096 0.00004 0.00003 0.00003 0.00000 0.00028 0.00025 0.00027 0.00020 0.00020 0.00020 0.00014 O1 0.29179 0.80925 0.02315 1.00000 0.02874 0.01596 0.02251 -0.00335 0.00851 0.00060 0.02240 0.00222 0.00010 0.00008 0.00006 0.00000 0.00071 0.00064 0.00065 0.00050 0.00052 0.00054 0.00029 O2 0.35020 0.79336 0.14609 1.00000 0.01943 0.01728 0.03270 0.00518 -0.00272 0.00323 0.02313 0.00226 0.00010 0.00008 0.00007 0.00000 0.00066 0.00065 0.00070 0.00053 0.00052 0.00054 0.00029 N1 0.28751 0.93277 0.10536 1.00000 0.02051 0.01051 0.01744 0.00160 -0.00072 -0.00001 0.01615 0.00243 0.00011 0.00009 0.00007 0.00000 0.00074 0.00069 0.00069 0.00053 0.00055 0.00059 0.00031 C16 0.02929 0.76017 0.20594 1.00000 0.02454 0.01957 0.01779 0.00172 0.00275 0.00147 0.02064 0.00319 0.00014 0.00012 0.00009 0.00000 0.00094 0.00090 0.00080 0.00067 0.00068 0.00077 0.00037 H16 0.00946 0.75693 0.25370 1.00000 0.02476 0.00000 0.00000 C14 0.15544 0.79484 0.11896 1.00000 0.01752 0.00849 0.01887 0.00041 0.00048 0.00171 0.01496 0.00289 0.00013 0.00010 0.00008 0.00000 0.00083 0.00074 0.00078 0.00060 0.00064 0.00066 0.00033 C18 -0.01109 0.74468 0.08428 1.00000 0.02251 0.02072 0.02138 0.00095 -0.00582 -0.00213 0.02154 0.00310 0.00014 0.00012 0.00009 0.00000 0.00093 0.00094 0.00085 0.00069 0.00070 0.00077 0.00038 H18 -0.05799 0.72956 0.04831 1.00000 0.02585 0.00000 0.00000 C15 0.12725 0.78777 0.18905 1.00000 0.02249 0.01593 0.01574 -0.00043 -0.00191 -0.00077 0.01805 0.00300 0.00014 0.00011 0.00009 0.00000 0.00091 0.00084 0.00077 0.00063 0.00065 0.00073 0.00036 H15 0.17474 0.80174 0.22497 1.00000 0.02166 0.00000 0.00000 C2 0.21094 1.07306 0.11083 1.00000 0.02118 0.01005 0.01995 0.00035 0.00080 -0.00020 0.01706 0.00290 0.00013 0.00011 0.00009 0.00000 0.00088 0.00080 0.00081 0.00062 0.00065 0.00069 0.00035 H2 0.22839 1.12399 0.08110 1.00000 0.02047 0.00000 0.00000 C9 0.19325 1.06192 -0.05547 1.00000 0.02132 0.01877 0.01961 0.00211 -0.00181 0.00017 0.01990 0.00315 0.00014 0.00012 0.00009 0.00000 0.00090 0.00089 0.00083 0.00067 0.00067 0.00076 0.00037 H9A 0.12595 1.03267 -0.05782 1.00000 0.02388 0.00000 0.00000 H9B 0.18275 1.11946 -0.03435 1.00000 0.02388 0.00000 0.00000 C17 -0.04067 0.73708 0.15399 1.00000 0.01908 0.01414 0.02530 0.00306 0.00079 0.00169 0.01951 0.00318 0.00014 0.00011 0.00009 0.00000 0.00089 0.00084 0.00088 0.00068 0.00068 0.00072 0.00037 C3 0.29644 1.06412 0.16551 1.00000 0.02571 0.01578 0.02382 -0.00328 -0.00270 -0.00113 0.02177 0.00309 0.00014 0.00012 0.00010 0.00000 0.00096 0.00090 0.00088 0.00069 0.00072 0.00077 0.00038 H3A 0.36018 1.09180 0.14871 1.00000 0.02612 0.00000 0.00000 H3B 0.27591 1.09148 0.21016 1.00000 0.02612 0.00000 0.00000 C8 0.26627 1.00927 -0.00936 1.00000 0.02165 0.01072 0.01774 0.00034 0.00033 -0.00013 0.01670 0.00299 0.00014 0.00011 0.00008 0.00000 0.00093 0.00081 0.00077 0.00062 0.00066 0.00069 0.00036 H8 0.27583 0.95213 -0.03259 1.00000 0.02004 0.00000 0.00000 C19 0.08588 0.77401 0.06657 1.00000 0.02501 0.01669 0.01501 0.00160 -0.00116 0.00094 0.01890 0.00305 0.00014 0.00011 0.00009 0.00000 0.00093 0.00086 0.00076 0.00064 0.00065 0.00074 0.00036 H19 0.10467 0.77984 0.01878 1.00000 0.02268 0.00000 0.00000 C6 0.02198 1.11023 0.08808 1.00000 0.02170 0.01975 0.02329 -0.00116 0.00056 -0.00093 0.02158 0.00317 0.00014 0.00012 0.00009 0.00000 0.00092 0.00091 0.00087 0.00070 0.00070 0.00076 0.00038 H6A 0.04694 1.15707 0.05734 1.00000 0.02590 0.00000 0.00000 H6B 0.01075 1.05876 0.05849 1.00000 0.02590 0.00000 0.00000 C5 0.10449 1.08971 0.14181 1.00000 0.02626 0.01301 0.02193 0.00041 0.00329 0.00023 0.02040 0.00318 0.00014 0.00011 0.00009 0.00000 0.00095 0.00084 0.00085 0.00066 0.00071 0.00076 0.00037 H5 0.11049 1.14084 0.17335 1.00000 0.02448 0.00000 0.00000 C4 0.31261 0.96777 0.17553 1.00000 0.02816 0.01752 0.02031 -0.00231 -0.00542 0.00053 0.02200 0.00309 0.00015 0.00012 0.00009 0.00000 0.00099 0.00091 0.00084 0.00069 0.00073 0.00079 0.00039 H4A 0.38435 0.95479 0.18863 1.00000 0.02639 0.00000 0.00000 H4B 0.26611 0.94441 0.21179 1.00000 0.02639 0.00000 0.00000 C1 0.22052 0.99197 0.06362 1.00000 0.01785 0.00960 0.01904 0.00117 -0.00125 -0.00041 0.01550 0.00288 0.00013 0.00011 0.00008 0.00000 0.00085 0.00078 0.00080 0.00062 0.00062 0.00066 0.00035 H1 0.15137 0.96509 0.05808 1.00000 0.01860 0.00000 0.00000 C7 -0.07971 1.13724 0.11974 1.00000 0.02673 0.02776 0.03032 -0.00392 -0.00093 0.00665 0.02827 0.00358 0.00015 0.00014 0.00011 0.00000 0.00105 0.00107 0.00099 0.00082 0.00079 0.00086 0.00044 H7A -0.10274 1.09319 0.15292 1.00000 0.04240 0.00000 0.00000 H7B -0.13073 1.14374 0.08249 1.00000 0.04240 0.00000 0.00000 H7C -0.07131 1.19222 0.14424 1.00000 0.04240 0.00000 0.00000 C20 -0.14477 0.70211 0.17307 1.00000 0.02257 0.02943 0.03634 0.00465 0.00190 -0.00411 0.02945 0.00365 0.00015 0.00014 0.00011 0.00000 0.00101 0.00109 0.00107 0.00087 0.00081 0.00086 0.00045 H20A -0.13903 0.64063 0.18397 1.00000 0.04417 0.00000 0.00000 H20B -0.19179 0.71001 0.13361 1.00000 0.04417 0.00000 0.00000 H20C -0.17113 0.73296 0.21402 1.00000 0.04417 0.00000 0.00000 C13 0.37102 1.05303 -0.00712 1.00000 0.02026 0.02277 0.02331 0.00487 0.00046 -0.00195 0.02211 0.00324 0.00014 0.00012 0.00009 0.00000 0.00092 0.00095 0.00088 0.00072 0.00069 0.00079 0.00039 H13A 0.41863 1.01791 0.02137 1.00000 0.02654 0.00000 0.00000 H13B 0.36436 1.11015 0.01544 1.00000 0.02654 0.00000 0.00000 C11 0.34173 1.11425 -0.12776 1.00000 0.03414 0.03108 0.02694 0.01181 0.00352 -0.00213 0.03072 0.00379 0.00016 0.00014 0.00010 0.00000 0.00113 0.00111 0.00096 0.00082 0.00083 0.00092 0.00046 H11A 0.33529 1.17401 -0.11026 1.00000 0.03687 0.00000 0.00000 H11B 0.36994 1.11666 -0.17581 1.00000 0.03687 0.00000 0.00000 C10 0.23645 1.07225 -0.12947 1.00000 0.03201 0.02495 0.01992 0.00532 -0.00134 0.00177 0.02563 0.00343 0.00015 0.00013 0.00009 0.00000 0.00106 0.00101 0.00087 0.00073 0.00076 0.00086 0.00042 H10A 0.24159 1.01501 -0.15202 1.00000 0.03075 0.00000 0.00000 H10B 0.18925 1.10808 -0.15770 1.00000 0.03075 0.00000 0.00000 C12 0.41504 1.06417 -0.08074 1.00000 0.02505 0.03189 0.02776 0.00918 0.00508 -0.00267 0.02823 0.00374 0.00015 0.00014 0.00010 0.00000 0.00099 0.00112 0.00097 0.00083 0.00077 0.00088 0.00044 H12A 0.48117 1.09518 -0.07786 1.00000 0.03388 0.00000 0.00000 H12B 0.42818 1.00680 -0.10148 1.00000 0.03388 0.00000 0.00000 Final Structure Factor Calculation for 2007src1053 in Pbca Total number of l.s. parameters = 228 Maximum vector length = 511 Memory required = 3248 / 25039 wR2 = 0.1096 before cycle 9 for 4422 data and 0 / 228 parameters GooF = S = 1.025; Restrained GooF = 1.025 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0508 * P )^2 + 3.00 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0406 for 3598 Fo > 4sig(Fo) and 0.0550 for all 4422 data wR2 = 0.1096, GooF = S = 1.025, Restrained GooF = 1.025 for all data Occupancy sum of asymmetric unit = 25.00 for non-hydrogen and 30.00 for hydrogen atoms Principal mean square atomic displacements U 0.0224 0.0158 0.0099 S1 0.0510 0.0238 0.0161 Cl1 0.0348 0.0193 0.0131 O1 0.0345 0.0217 0.0132 O2 0.0207 0.0176 0.0102 N1 0.0261 0.0194 0.0164 C16 0.0191 0.0176 0.0082 C14 0.0284 0.0202 0.0160 C18 0.0231 0.0162 0.0149 C15 0.0216 0.0196 0.0100 C2 0.0228 0.0203 0.0167 C9 0.0263 0.0192 0.0130 C17 0.0277 0.0233 0.0143 C3 0.0217 0.0177 0.0107 C8 0.0252 0.0177 0.0138 C19 0.0239 0.0216 0.0192 C6 0.0280 0.0202 0.0130 C5 0.0311 0.0193 0.0156 C4 0.0200 0.0171 0.0095 C1 0.0361 0.0285 0.0202 C7 0.0387 0.0299 0.0198 C20 0.0281 0.0211 0.0172 C13 0.0411 0.0350 0.0161 C11 0.0324 0.0282 0.0163 C10 0.0393 0.0287 0.0166 C12 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.013 0.024 0.035 0.049 0.064 0.083 0.103 0.136 0.190 1.000 Number in group 475. 449. 411. 441. 458. 421. 442. 442. 438. 445. GooF 1.050 1.017 1.011 1.140 1.059 1.033 1.066 0.976 0.925 0.953 K 1.871 1.085 0.969 0.984 0.994 0.995 0.993 1.011 1.010 1.000 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 458. 427. 447. 442. 439. 442. 450. 431. 444. 442. GooF 0.879 0.897 0.874 0.876 0.926 0.843 0.900 0.923 1.022 1.768 K 0.987 1.023 1.022 0.996 1.014 1.007 1.008 1.010 1.013 0.990 R1 0.126 0.097 0.081 0.080 0.060 0.044 0.038 0.031 0.031 0.042 Recommended weighting scheme: WGHT 0.0419 3.4245 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) 5 0 4 284.94 117.07 6.13 0.041 2.29 3 2 8 952.54 595.97 5.68 0.093 2.02 0 6 2 92.78 11.57 5.06 0.013 2.50 4 1 3 483.12 278.63 4.87 0.064 2.85 3 5 6 120.98 45.60 4.71 0.026 1.98 1 5 10 381.03 223.04 4.70 0.057 1.61 5 1 1 320.70 530.87 4.61 0.088 2.55 2 6 4 130.76 51.60 4.53 0.027 2.15 4 0 4 53.44 8.48 4.51 0.011 2.69 6 4 2 399.11 240.23 4.42 0.059 1.86 6 1 1 685.00 461.99 4.34 0.082 2.14 4 1 8 195.60 100.25 4.25 0.038 1.91 5 2 6 73.57 167.22 4.24 0.049 1.95 6 3 2 848.73 608.55 4.00 0.094 1.96 4 1 4 74.64 157.64 3.93 0.048 2.66 4 3 7 1731.14 2253.07 3.90 0.181 1.94 3 2 6 482.68 693.98 3.89 0.100 2.44 5 4 2 1782.21 1370.33 3.84 0.141 2.11 5 6 5 74.01 17.75 3.83 0.016 1.66 2 6 1 507.14 347.85 3.74 0.071 2.39 4 5 6 923.00 687.44 3.71 0.100 1.84 5 2 8 262.96 163.77 3.65 0.049 1.72 9 9 6 140.05 272.16 3.60 0.063 1.05 6 2 8 88.63 34.14 3.58 0.022 1.57 2 1 7 129.77 223.26 3.55 0.057 2.49 5 4 3 1302.67 1007.89 3.52 0.121 2.05 1 3 11 41.06 100.76 3.50 0.038 1.63 0 8 0 3681.51 2616.64 3.48 0.195 1.94 2 1 10 2579.87 2072.05 3.45 0.174 1.82 5 0 2 1886.52 2384.21 3.41 0.186 2.52 2 3 9 82.18 154.87 3.40 0.047 1.88 4 5 0 790.95 588.16 3.38 0.092 2.25 2 4 1 922.12 1199.99 3.36 0.132 3.29 14 6 3 116.13 438.53 3.32 0.080 0.87 6 5 0 138.25 72.71 3.30 0.033 1.78 10 15 0 185.67 676.97 3.28 0.099 0.81 2 0 6 311.29 210.18 3.18 0.055 2.86 6 0 2 1239.14 973.40 3.16 0.119 2.12 1 2 6 365.05 506.07 3.15 0.086 2.87 7 2 4 365.63 510.37 3.12 0.086 1.70 3 2 2 1061.76 1339.15 3.10 0.139 3.53 4 3 0 916.33 710.85 3.08 0.102 2.76 10 3 5 1433.67 1131.56 3.07 0.128 1.20 14 8 5 200.96 401.44 3.06 0.076 0.82 4 4 2 14.62 0.55 3.05 0.003 2.42 1 14 8 211.02 122.55 3.05 0.042 1.00 6 1 7 423.09 574.48 3.04 0.091 1.69 4 1 22 -21.75 25.95 2.95 0.019 0.84 1 11 7 65.67 23.89 2.94 0.019 1.25 4 4 3 463.56 612.19 2.93 0.094 2.33 Bond lengths and angles S1 - Distance Angles O2 1.4360 (0.0013) O1 1.4376 (0.0013) 119.50 (0.08) N1 1.6203 (0.0015) 105.89 (0.08) 108.24 (0.07) C14 1.7654 (0.0017) 107.85 (0.08) 105.86 (0.08) 109.24 (0.08) S1 - O2 O1 N1 Cl1 - Distance Angles C5 1.8212 (0.0018) Cl1 - O1 - Distance Angles S1 1.4376 (0.0013) O1 - O2 - Distance Angles S1 1.4360 (0.0013) O2 - N1 - Distance Angles C4 1.4834 (0.0021) C1 1.4987 (0.0021) 112.66 (0.13) S1 1.6203 (0.0015) 118.37 (0.11) 121.01 (0.11) N1 - C4 C1 C16 - Distance Angles C15 1.3867 (0.0026) C17 1.3958 (0.0025) 121.15 (0.16) H16 0.9500 119.43 119.43 C16 - C15 C17 C14 - Distance Angles C19 1.3896 (0.0024) C15 1.3934 (0.0023) 120.10 (0.16) S1 1.7654 (0.0017) 119.62 (0.13) 120.28 (0.13) C14 - C19 C15 C18 - Distance Angles C19 1.3872 (0.0026) C17 1.3920 (0.0025) 120.96 (0.16) H18 0.9500 119.52 119.52 C18 - C19 C17 C15 - Distance Angles C16 1.3867 (0.0026) C14 1.3934 (0.0023) 119.45 (0.16) H15 0.9500 120.28 120.28 C15 - C16 C14 C2 - Distance Angles C5 1.5323 (0.0024) C3 1.5352 (0.0024) 114.30 (0.14) C1 1.5542 (0.0023) 115.71 (0.14) 105.27 (0.13) H2 1.0000 107.02 107.02 107.02 C2 - C5 C3 C1 C9 - Distance Angles C10 1.5308 (0.0024) C8 1.5341 (0.0024) 110.95 (0.15) H9A 0.9900 109.45 109.45 H9B 0.9900 109.45 109.45 108.04 C9 - C10 C8 H9A C17 - Distance Angles C18 1.3920 (0.0025) C16 1.3958 (0.0025) 118.51 (0.17) C20 1.5080 (0.0026) 120.78 (0.17) 120.68 (0.16) C17 - C18 C16 C3 - Distance Angles C4 1.5231 (0.0025) C2 1.5352 (0.0024) 105.97 (0.14) H3A 0.9900 110.54 110.54 H3B 0.9900 110.54 110.54 108.70 C3 - C4 C2 H3A C8 - Distance Angles C13 1.5275 (0.0025) C9 1.5341 (0.0024) 109.58 (0.14) C1 1.5406 (0.0023) 113.54 (0.14) 111.84 (0.14) H8 1.0000 107.18 107.18 107.18 C8 - C13 C9 C1 C19 - Distance Angles C18 1.3872 (0.0026) C14 1.3896 (0.0024) 119.80 (0.16) H19 0.9500 120.10 120.10 C19 - C18 C14 C6 - Distance Angles C7 1.5179 (0.0026) C5 1.5217 (0.0025) 114.08 (0.15) H6A 0.9900 108.73 108.73 H6B 0.9900 108.73 108.73 107.64 C6 - C7 C5 H6A C5 - Distance Angles C6 1.5217 (0.0025) C2 1.5323 (0.0024) 114.62 (0.14) Cl1 1.8212 (0.0018) 109.13 (0.13) 111.13 (0.12) H5 1.0000 107.21 107.21 107.21 C5 - C6 C2 Cl1 C4 - Distance Angles N1 1.4834 (0.0021) C3 1.5231 (0.0025) 102.46 (0.14) H4A 0.9900 111.28 111.28 H4B 0.9900 111.28 111.28 109.18 C4 - N1 C3 H4A C1 - Distance Angles N1 1.4987 (0.0021) C8 1.5406 (0.0023) 111.26 (0.14) C2 1.5542 (0.0023) 103.59 (0.13) 114.53 (0.13) H1 1.0000 109.09 109.09 109.09 C1 - N1 C8 C2 C7 - Distance Angles C6 1.5179 (0.0026) 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 C20 - Distance Angles C17 1.5080 (0.0026) H20A 0.9800 109.47 H20B 0.9800 109.47 109.47 H20C 0.9800 109.47 109.47 109.47 C20 - C17 H20A H20B C13 - Distance Angles C8 1.5275 (0.0025) C12 1.5294 (0.0025) 111.16 (0.15) H13A 0.9900 109.40 109.40 H13B 0.9900 109.40 109.40 108.01 C13 - C8 C12 H13A C11 - Distance Angles C10 1.5217 (0.0029) C12 1.5258 (0.0028) 111.14 (0.16) H11A 0.9900 109.41 109.41 H11B 0.9900 109.41 109.41 108.02 C11 - C10 C12 H11A C10 - Distance Angles C11 1.5217 (0.0029) C9 1.5308 (0.0024) 110.96 (0.16) H10A 0.9900 109.45 109.45 H10B 0.9900 109.45 109.45 108.04 C10 - C11 C9 H10A C12 - Distance Angles C11 1.5258 (0.0028) C13 1.5294 (0.0024) 111.32 (0.16) H12A 0.9900 109.37 109.37 H12B 0.9900 109.37 109.37 107.99 C12 - C11 C13 H12A FMAP and GRID set by program FMAP 2 2 20 GRID -1.471 24 -2 1.471 1 2 R1 = 0.0545 for 4422 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.88 at 0.4569 0.0531 0.2881 [ 1.50 A from H7A ] Deepest hole -0.42 at 0.2244 0.2173 0.5926 [ 0.73 A from S1 ] Mean = 0.00, Rms deviation from mean = 0.06 e/A^3, Highest memory used = 3611 / 34472 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.0431 1.0531 0.2119 1.00000 0.05 0.88 1.50 H7A 1.64 CL1 2.24 C7 2.41 C5 Q2 1 0.2146 1.0303 0.0892 1.00000 0.05 0.37 0.77 C1 0.78 C2 1.44 H1 1.47 H2 Q3 1 -0.0200 0.7265 0.1197 1.00000 0.05 0.30 0.73 C17 0.74 C18 1.45 H18 1.84 C16 Q4 1 0.2178 1.0685 -0.0927 1.00000 0.05 0.28 0.75 C10 0.79 C9 1.44 H10B 1.44 H10A Q5 1 0.1594 1.0642 0.1323 1.00000 0.05 0.28 0.80 C2 0.84 C5 1.56 H5 1.62 H2 Q6 1 0.2400 1.0022 0.0270 1.00000 0.05 0.27 0.76 C1 0.78 C8 1.42 H1 1.46 H8 Q7 1 0.2164 0.8051 0.1090 1.00000 0.05 0.27 0.83 C14 0.94 S1 1.89 O2 1.91 O1 Q8 1 0.2319 1.0366 -0.0328 1.00000 0.05 0.27 0.76 C8 0.77 C9 1.43 H8 1.44 H9B Q9 1 0.3149 1.0321 -0.0121 1.00000 0.05 0.26 0.73 C8 0.81 C13 1.40 H8 1.47 H13B Q10 1 0.2432 1.0579 0.1389 1.00000 0.05 0.26 0.72 C2 0.87 C3 1.52 H3B 1.52 H2 Q11 1 0.2551 0.9582 0.0848 1.00000 0.05 0.26 0.70 N1 0.80 C1 1.45 H1 1.89 C4 Q12 1 0.1385 0.8060 0.1487 1.00000 0.05 0.26 0.63 C14 0.83 C15 1.53 H15 1.78 C19 Q13 1 -0.0224 1.1318 0.1047 1.00000 0.05 0.23 0.74 C6 0.81 C7 1.34 H6A 1.36 H7C Q14 1 0.0001 0.7400 0.1795 1.00000 0.05 0.21 0.71 C16 0.72 C17 1.45 H16 1.83 C15 Q15 1 0.2943 0.9463 0.1328 1.00000 0.05 0.21 0.57 N1 0.91 C4 1.55 H4B 1.59 H4A Q16 1 -0.0817 0.7212 0.1591 1.00000 0.05 0.20 0.60 C17 0.91 C20 1.53 H20B 1.53 H20A Q17 1 0.3418 0.9215 0.0959 1.00000 0.05 0.20 0.75 N1 1.64 S1 1.72 C4 1.93 H4A Q18 1 0.1754 0.7807 0.1185 1.00000 0.05 0.19 0.34 C14 1.49 C15 1.54 C19 1.62 S1 Q19 1 0.1181 0.7856 0.0953 1.00000 0.05 0.19 0.68 C14 0.72 C19 1.48 H19 1.79 C15 Q20 1 0.3385 0.8095 -0.0277 1.00000 0.05 0.19 1.15 O1 1.53 H18 2.08 H20B 2.36 H8 Shortest distances between peaks (including symmetry equivalents) 7 18 0.68 12 18 0.85 18 19 0.87 15 17 1.01 11 15 1.07 12 19 1.10 5 10 1.11 2 10 1.11 3 16 1.11 8 9 1.15 14 16 1.17 3 14 1.19 2 5 1.21 2 11 1.24 4 8 1.26 6 8 1.27 7 12 1.27 11 17 1.28 2 6 1.31 6 11 1.31 6 9 1.32 7 19 1.34 10 15 1.86 2 15 1.87 10 11 1.87 4 9 2.07 3 19 2.08 12 14 2.16 6 17 2.25 5 11 2.26 6 10 2.31 6 15 2.31 9 11 2.31 14 19 2.34 2 9 2.34 2 8 2.34 2 17 2.37 1 13 2.40 7 17 2.45 7 15 2.46 5 6 2.47 3 12 2.47 7 11 2.47 4 6 2.52 5 15 2.54 8 11 2.57 10 17 2.61 3 20 2.61 14 18 2.65 5 13 2.65 3 18 2.69 9 17 2.71 16 20 2.76 17 20 2.93 12 15 3.00 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 0.00: 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. 0.22: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.02: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.02: Generate idealized H-atoms 2.47: Structure factors and derivatives 1.91: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.08: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.05: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.08: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src1053 finished at 11:04:01 Total CPU time: 5.0 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++