+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2009src0001 started at 12:59:57 on 09-Jan-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2009src0001 in P-1 CELL 0.71073 10.0998 10.2807 11.7549 100.067 100.429 103.216 ZERR 2.00 0.0002 0.0002 0.0003 0.002 0.001 0.002 LATT 1 SFAC C H B N O UNIT 44 70 2 4 8 V = 1138.41 F(000) = 436.0 Mu = 0.08 mm-1 Cell Wt = 804.66 Rho = 1.174 MERG 2 OMIT -3.00 55.00 SHEL 7 0.77 FMAP 2 PLAN 10 SIZE 0.03 0.10 0.19 ACTA BOND $H WGHT 0.02020 0.89680 L.S. 4 TEMP -153.00 FVAR 0.90158 MOLE 1 C3 1 0.232433 0.148504 0.752071 11.00000 0.02482 0.02365 = 0.02736 0.00514 0.01170 0.00793 C4 1 0.267548 0.304347 0.752779 11.00000 0.02019 0.02348 = 0.02630 0.00414 0.00877 0.00726 C6 1 0.135333 0.060038 0.636467 11.00000 0.03616 0.02802 = 0.03395 -0.00385 0.01427 0.00179 AFIX 137 H6A 2 0.099030 -0.032985 0.646826 11.00000 -1.50000 H6B 2 0.187055 0.056609 0.573544 11.00000 -1.50000 H6C 2 0.057348 0.099488 0.614541 11.00000 -1.50000 AFIX 0 C7 1 0.357605 0.093433 0.786051 11.00000 0.03400 0.03657 = 0.05181 0.01738 0.02057 0.01902 AFIX 137 H7A 2 0.412496 0.144741 0.865269 11.00000 -1.50000 H7B 2 0.415875 0.103837 0.728272 11.00000 -1.50000 H7C 2 0.325297 -0.003853 0.786559 11.00000 -1.50000 AFIX 0 C8 1 0.395620 0.390201 0.848615 11.00000 0.02086 0.03464 = 0.03402 -0.00019 0.00567 0.00100 AFIX 137 H8A 2 0.400722 0.487719 0.855676 11.00000 -1.50000 H8B 2 0.480077 0.372121 0.827087 11.00000 -1.50000 H8C 2 0.388390 0.365952 0.924689 11.00000 -1.50000 AFIX 0 C9 1 0.277283 0.338726 0.633562 11.00000 0.03022 0.03555 = 0.03180 0.01199 0.01378 0.01006 AFIX 137 H9A 2 0.187627 0.295716 0.576335 11.00000 -1.50000 H9B 2 0.350841 0.304232 0.604911 11.00000 -1.50000 H9C 2 0.299666 0.438419 0.642498 11.00000 -1.50000 AFIX 0 C10 1 -0.017017 0.261834 0.924517 11.00000 0.01604 0.01956 = 0.01870 0.00059 0.00162 0.00171 C11 1 -0.022458 0.187094 1.013159 11.00000 0.02312 0.02188 = 0.02285 0.00355 0.00292 0.00380 AFIX 43 H11 2 0.038198 0.129495 1.022603 11.00000 -1.20000 AFIX 0 C12 1 -0.113634 0.194664 1.087450 11.00000 0.02859 0.02919 = 0.02243 0.00675 0.00700 0.00163 AFIX 43 H12 2 -0.114350 0.143774 1.147565 11.00000 -1.20000 AFIX 0 C13 1 -0.203884 0.277029 1.073500 11.00000 0.02349 0.03543 = 0.02346 -0.00075 0.01067 0.00173 AFIX 43 H13 2 -0.266610 0.283244 1.124200 11.00000 -1.20000 AFIX 0 C14 1 -0.201983 0.350241 0.985094 11.00000 0.01968 0.02668 = 0.02525 -0.00175 0.00305 0.00605 AFIX 43 H14 2 -0.264920 0.405540 0.975145 11.00000 -1.20000 AFIX 0 C15 1 -0.110105 0.344568 0.910707 11.00000 0.01770 0.01848 = 0.01947 -0.00125 0.00098 0.00241 C16 1 -0.111727 0.423809 0.813984 11.00000 0.02245 0.01911 = 0.02066 -0.00003 0.00095 0.00671 AFIX 23 H16A 2 -0.172381 0.486145 0.824366 11.00000 -1.20000 H16B 2 -0.015961 0.480623 0.820853 11.00000 -1.20000 AFIX 0 C18 1 -0.129135 0.404420 0.604041 11.00000 0.01776 0.02203 = 0.02417 0.00642 0.00441 0.00258 AFIX 23 H18A 2 -0.026978 0.445894 0.621466 11.00000 -1.20000 H18B 2 -0.175925 0.479177 0.604014 11.00000 -1.20000 AFIX 0 C19 1 -0.176378 0.306478 0.483104 11.00000 0.02007 0.02972 = 0.02395 0.00488 0.00432 0.00297 AFIX 23 H19A 2 -0.158482 0.357880 0.421186 11.00000 -1.20000 H19B 2 -0.122198 0.237445 0.480466 11.00000 -1.20000 AFIX 0 C21 1 -0.365427 0.169901 0.551375 11.00000 0.02361 0.02738 = 0.02175 0.00859 -0.00040 -0.00280 AFIX 23 H21A 2 -0.324493 0.091328 0.553506 11.00000 -1.20000 H21B 2 -0.468427 0.134502 0.533801 11.00000 -1.20000 AFIX 0 C22 1 -0.313981 0.271255 0.670885 11.00000 0.01723 0.02784 = 0.02307 0.00886 0.00284 0.00300 AFIX 23 H22A 2 -0.362555 0.344708 0.671111 11.00000 -1.20000 H22B 2 -0.336376 0.223692 0.734117 11.00000 -1.20000 AFIX 0 C23 1 -0.412585 0.239097 0.357945 11.00000 0.02334 0.02148 = 0.01950 0.00192 0.00591 0.00474 C26 1 -0.658178 0.164959 0.251099 11.00000 0.02287 0.02590 = 0.02106 0.00679 0.00006 0.00802 C27 1 -0.636146 0.095891 0.133423 11.00000 0.03084 0.05141 = 0.02319 0.00160 0.00092 0.01384 AFIX 137 H27A 2 -0.549348 0.148651 0.118961 11.00000 -1.50000 H27B 2 -0.714977 0.091761 0.069268 11.00000 -1.50000 H27C 2 -0.629900 0.002701 0.136123 11.00000 -1.50000 AFIX 0 C28 1 -0.669411 0.309810 0.254679 11.00000 0.03175 0.02916 = 0.05407 0.01312 0.00438 0.01110 AFIX 137 H28A 2 -0.672488 0.352823 0.335073 11.00000 -1.50000 H28B 2 -0.754931 0.307575 0.198618 11.00000 -1.50000 H28C 2 -0.588088 0.362852 0.232665 11.00000 -1.50000 AFIX 0 C29 1 -0.786435 0.079778 0.280249 11.00000 0.02361 0.03620 = 0.03031 0.01091 -0.00013 0.00386 AFIX 137 H29A 2 -0.776467 -0.012731 0.280801 11.00000 -1.50000 H29B 2 -0.869881 0.074184 0.220178 11.00000 -1.50000 H29C 2 -0.795671 0.122948 0.358568 11.00000 -1.50000 AFIX 0 B1 3 0.092702 0.249044 0.848606 11.00000 0.01887 0.02008 = 0.01880 0.00214 0.00129 0.00441 N17 4 -0.163132 0.331863 0.695336 11.00000 0.01643 0.02008 = 0.01847 0.00255 0.00157 0.00289 N20 4 -0.325040 0.237469 0.459155 11.00000 0.02150 0.03147 = 0.02024 0.00850 0.00088 -0.00292 O2 5 0.150608 0.140264 0.842409 11.00000 0.02592 0.02509 = 0.02889 0.00871 0.01240 0.00980 O5 5 0.147504 0.342368 0.787579 11.00000 0.01998 0.02240 = 0.02871 0.00618 0.00945 0.00694 O24 5 -0.375368 0.299815 0.284310 11.00000 0.02806 0.03686 = 0.02313 0.01077 0.00698 0.00544 O25 5 -0.544101 0.164462 0.349514 11.00000 0.02150 0.02724 = 0.01996 0.00701 -0.00105 0.00203 HKLF 4 Covalent radii and connectivity table for 2009src0001 in P-1 C 0.770 H 0.320 B 0.820 N 0.700 O 0.660 C3 - O2 C7 C6 C4 C4 - O5 C9 C8 C3 C6 - C3 C7 - C3 C8 - C4 C9 - C4 C10 - C11 C15 B1 C11 - C12 C10 C12 - C11 C13 C13 - C14 C12 C14 - C13 C15 C15 - C14 C10 C16 C16 - N17 C15 C18 - N17 C19 C19 - N20 C18 C21 - N20 C22 C22 - N17 C21 C23 - O24 O25 N20 C26 - O25 C28 C27 C29 C27 - C26 C28 - C26 C29 - C26 B1 - O5 O2 C10 N17 - C18 C22 C16 N20 - C23 C21 C19 O2 - B1 C3 O5 - B1 C4 O24 - C23 O25 - C23 C26 23230 Reflections read, of which 51 rejected -13 =< h =< 13, -13 =< k =< 13, -15 =< l =< 15, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 5193 Unique reflections, of which 0 suppressed R(int) = 0.0435 R(sigma) = 0.0408 Friedel opposites merged Maximum memory for data reduction = 3092 / 52423 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 = 3919 / 335788 wR2 = 0.1152 before cycle 1 for 5193 data and 269 / 269 parameters GooF = S = 1.070; Restrained GooF = 1.070 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0202 * P )^2 + 0.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.90136 0.00132 -0.164 OSF Mean shift/su = 0.017 Maximum = -0.164 for OSF Max. shift = 0.000 A for H27A Max. dU = 0.000 for C10 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3919 / 335788 wR2 = 0.1151 before cycle 2 for 5193 data and 269 / 269 parameters GooF = S = 1.070; Restrained GooF = 1.070 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0202 * P )^2 + 0.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.90129 0.00131 -0.054 OSF Mean shift/su = 0.006 Maximum = -0.054 for OSF Max. shift = 0.000 A for H27A Max. dU = 0.000 for O2 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3919 / 335788 wR2 = 0.1151 before cycle 3 for 5193 data and 269 / 269 parameters GooF = S = 1.070; Restrained GooF = 1.070 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0202 * P )^2 + 0.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.90129 0.00131 0.000 OSF Mean shift/su = 0.000 Maximum = 0.001 for U23 C18 Max. shift = 0.000 A for H27A Max. dU = 0.000 for C7 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3919 / 335788 wR2 = 0.1151 before cycle 4 for 5193 data and 269 / 269 parameters GooF = S = 1.070; Restrained GooF = 1.070 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0202 * P )^2 + 0.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.90129 0.00131 0.001 OSF Mean shift/su = 0.000 Maximum = 0.001 for z C12 Max. shift = 0.000 A for H29B Max. dU = 0.000 for C22 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H6A 0.0991 -0.0330 0.6468 137 0.980 0.000 C6 C3 H6A H6B 0.1870 0.0566 0.5735 137 0.980 0.000 C6 C3 H6A H6C 0.0573 0.0995 0.6146 137 0.980 0.000 C6 C3 H6A H7A 0.4125 0.1447 0.8653 137 0.980 0.000 C7 C3 H7A H7B 0.4159 0.1038 0.7283 137 0.980 0.000 C7 C3 H7A H7C 0.3253 -0.0039 0.7866 137 0.980 0.000 C7 C3 H7A H8A 0.4007 0.4877 0.8557 137 0.980 0.000 C8 C4 H8A H8B 0.4801 0.3721 0.8271 137 0.980 0.000 C8 C4 H8A H8C 0.3884 0.3660 0.9247 137 0.980 0.000 C8 C4 H8A H9A 0.1876 0.2957 0.5763 137 0.980 0.000 C9 C4 H9A H9B 0.3508 0.3042 0.6049 137 0.980 0.000 C9 C4 H9A H9C 0.2997 0.4384 0.6425 137 0.980 0.000 C9 C4 H9A H11 0.0382 0.1295 1.0226 43 0.950 0.000 C11 C12 C10 H12 -0.1144 0.1438 1.1476 43 0.950 0.000 C12 C11 C13 H13 -0.2666 0.2833 1.1242 43 0.950 0.000 C13 C14 C12 H14 -0.2649 0.4055 0.9751 43 0.950 0.000 C14 C13 C15 H16A -0.1724 0.4861 0.8244 23 0.990 0.000 C16 N17 C15 H16B -0.0160 0.4806 0.8209 23 0.990 0.000 C16 N17 C15 H18A -0.0270 0.4459 0.6215 23 0.990 0.000 C18 N17 C19 H18B -0.1759 0.4792 0.6040 23 0.990 0.000 C18 N17 C19 H19A -0.1585 0.3579 0.4212 23 0.990 0.000 C19 N20 C18 H19B -0.1222 0.2374 0.4805 23 0.990 0.000 C19 N20 C18 H21A -0.3245 0.0913 0.5535 23 0.990 0.000 C21 N20 C22 H21B -0.4684 0.1345 0.5338 23 0.990 0.000 C21 N20 C22 H22A -0.3626 0.3447 0.6711 23 0.990 0.000 C22 N17 C21 H22B -0.3364 0.2237 0.7341 23 0.990 0.000 C22 N17 C21 H27A -0.5494 0.1487 0.1189 137 0.980 0.000 C27 C26 H27A H27B -0.7150 0.0917 0.0693 137 0.980 0.000 C27 C26 H27A H27C -0.6298 0.0027 0.1361 137 0.980 0.000 C27 C26 H27A H28A -0.6725 0.3528 0.3351 137 0.980 0.000 C28 C26 H28A H28B -0.7549 0.3076 0.1986 137 0.980 0.000 C28 C26 H28A H28C -0.5881 0.3629 0.2326 137 0.980 0.000 C28 C26 H28A H29A -0.7765 -0.0127 0.2808 137 0.980 0.000 C29 C26 H29A H29B -0.8699 0.0742 0.2202 137 0.980 0.000 C29 C26 H29A H29C -0.7957 0.1229 0.3586 137 0.980 0.000 C29 C26 H29A 2009src0001 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C3 0.23244 0.14851 0.75207 1.00000 0.02478 0.02364 0.02733 0.00514 0.01169 0.00793 0.02433 0.00386 0.00018 0.00017 0.00015 0.00000 0.00087 0.00086 0.00088 0.00069 0.00071 0.00067 0.00036 C4 0.26755 0.30434 0.75277 1.00000 0.02016 0.02346 0.02628 0.00413 0.00877 0.00726 0.02280 0.00375 0.00017 0.00017 0.00015 0.00000 0.00082 0.00084 0.00086 0.00067 0.00067 0.00064 0.00035 C6 0.13533 0.06004 0.63646 1.00000 0.03614 0.02800 0.03392 -0.00385 0.01427 0.00178 0.03441 0.00408 0.00021 0.00019 0.00017 0.00000 0.00106 0.00097 0.00103 0.00079 0.00085 0.00078 0.00044 H6A 0.09906 -0.03299 0.64682 1.00000 0.05162 0.00000 0.00000 H6B 0.18705 0.05663 0.57353 1.00000 0.05162 0.00000 0.00000 H6C 0.05733 0.09947 0.61455 1.00000 0.05162 0.00000 0.00000 C7 0.35761 0.09343 0.78605 1.00000 0.03395 0.03656 0.05178 0.01738 0.02058 0.01902 0.03677 0.00496 0.00021 0.00021 0.00020 0.00000 0.00107 0.00109 0.00126 0.00094 0.00095 0.00086 0.00046 H7A 0.41249 0.14473 0.86527 1.00000 0.05516 0.00000 0.00000 H7B 0.41588 0.10383 0.72828 1.00000 0.05516 0.00000 0.00000 H7C 0.32529 -0.00386 0.78655 1.00000 0.05516 0.00000 0.00000 C8 0.39562 0.39020 0.84861 1.00000 0.02085 0.03461 0.03400 -0.00018 0.00568 0.00100 0.03202 0.00389 0.00018 0.00020 0.00017 0.00000 0.00089 0.00102 0.00102 0.00080 0.00076 0.00074 0.00042 H8A 0.40072 0.48771 0.85567 1.00000 0.04803 0.00000 0.00000 H8B 0.48008 0.37211 0.82709 1.00000 0.04803 0.00000 0.00000 H8C 0.38839 0.36595 0.92469 1.00000 0.04803 0.00000 0.00000 C9 0.27729 0.33873 0.63357 1.00000 0.03019 0.03552 0.03177 0.01198 0.01378 0.01003 0.03085 0.00439 0.00020 0.00020 0.00017 0.00000 0.00098 0.00102 0.00099 0.00080 0.00079 0.00078 0.00041 H9A 0.18763 0.29573 0.57634 1.00000 0.04627 0.00000 0.00000 H9B 0.35084 0.30424 0.60491 1.00000 0.04627 0.00000 0.00000 H9C 0.29968 0.43843 0.64251 1.00000 0.04627 0.00000 0.00000 C10 -0.01702 0.26183 0.92452 1.00000 0.01600 0.01951 0.01867 0.00057 0.00161 0.00169 0.01938 0.00333 0.00016 0.00016 0.00014 0.00000 0.00075 0.00078 0.00077 0.00061 0.00061 0.00059 0.00033 C11 -0.02245 0.18710 1.01315 1.00000 0.02307 0.02184 0.02284 0.00354 0.00291 0.00380 0.02347 0.00358 0.00018 0.00017 0.00015 0.00000 0.00084 0.00083 0.00083 0.00066 0.00067 0.00065 0.00035 H11 0.03821 0.12950 1.02260 1.00000 0.02817 0.00000 0.00000 C12 -0.11364 0.19466 1.08745 1.00000 0.02855 0.02917 0.02240 0.00674 0.00699 0.00163 0.02748 0.00382 0.00018 0.00018 0.00015 0.00000 0.00093 0.00094 0.00086 0.00071 0.00072 0.00072 0.00038 H12 -0.11436 0.14377 1.14756 1.00000 0.03298 0.00000 0.00000 C13 -0.20388 0.27703 1.07350 1.00000 0.02348 0.03539 0.02343 -0.00077 0.01067 0.00173 0.02873 0.00381 0.00018 0.00019 0.00016 0.00000 0.00089 0.00101 0.00087 0.00074 0.00072 0.00073 0.00040 H13 -0.26660 0.28325 1.12420 1.00000 0.03448 0.00000 0.00000 C14 -0.20198 0.35024 0.98509 1.00000 0.01967 0.02665 0.02521 -0.00177 0.00303 0.00604 0.02514 0.00361 0.00017 0.00018 0.00015 0.00000 0.00083 0.00089 0.00087 0.00069 0.00068 0.00067 0.00037 H14 -0.26492 0.40554 0.97514 1.00000 0.03017 0.00000 0.00000 C15 -0.11011 0.34457 0.91071 1.00000 0.01768 0.01846 0.01943 -0.00126 0.00098 0.00239 0.02009 0.00335 0.00016 0.00016 0.00014 0.00000 0.00077 0.00078 0.00078 0.00061 0.00062 0.00060 0.00033 C16 -0.11173 0.42381 0.81399 1.00000 0.02239 0.01910 0.02066 -0.00003 0.00095 0.00670 0.02164 0.00349 0.00017 0.00016 0.00014 0.00000 0.00083 0.00081 0.00080 0.00063 0.00065 0.00063 0.00034 H16A -0.17239 0.48614 0.82437 1.00000 0.02597 0.00000 0.00000 H16B -0.01596 0.48063 0.82086 1.00000 0.02597 0.00000 0.00000 C18 -0.12913 0.40442 0.60404 1.00000 0.01774 0.02202 0.02414 0.00642 0.00442 0.00257 0.02167 0.00356 0.00017 0.00017 0.00014 0.00000 0.00078 0.00082 0.00084 0.00066 0.00065 0.00062 0.00034 H18A -0.02697 0.44589 0.62146 1.00000 0.02600 0.00000 0.00000 H18B -0.17592 0.47918 0.60401 1.00000 0.02600 0.00000 0.00000 C19 -0.17637 0.30648 0.48310 1.00000 0.02006 0.02968 0.02394 0.00489 0.00433 0.00295 0.02544 0.00364 0.00017 0.00018 0.00015 0.00000 0.00084 0.00093 0.00087 0.00071 0.00068 0.00068 0.00037 H19A -0.15848 0.35788 0.42118 1.00000 0.03053 0.00000 0.00000 H19B -0.12220 0.23744 0.48046 1.00000 0.03053 0.00000 0.00000 C21 -0.36542 0.16990 0.55137 1.00000 0.02358 0.02735 0.02176 0.00860 -0.00041 -0.00280 0.02623 0.00365 0.00018 0.00018 0.00015 0.00000 0.00087 0.00091 0.00084 0.00070 0.00068 0.00068 0.00038 H21A -0.32449 0.09133 0.55350 1.00000 0.03147 0.00000 0.00000 H21B -0.46842 0.13450 0.53380 1.00000 0.03147 0.00000 0.00000 C22 -0.31398 0.27125 0.67088 1.00000 0.01721 0.02782 0.02305 0.00885 0.00285 0.00299 0.02305 0.00358 0.00016 0.00018 0.00015 0.00000 0.00080 0.00089 0.00084 0.00069 0.00065 0.00065 0.00035 H22A -0.36256 0.34470 0.67111 1.00000 0.02766 0.00000 0.00000 H22B -0.33638 0.22368 0.73411 1.00000 0.02766 0.00000 0.00000 C23 -0.41258 0.23910 0.35795 1.00000 0.02332 0.02145 0.01951 0.00190 0.00589 0.00475 0.02186 0.00356 0.00017 0.00017 0.00014 0.00000 0.00084 0.00082 0.00080 0.00064 0.00066 0.00064 0.00034 C26 -0.65818 0.16495 0.25109 1.00000 0.02283 0.02590 0.02103 0.00677 0.00005 0.00801 0.02348 0.00368 0.00017 0.00017 0.00015 0.00000 0.00085 0.00087 0.00082 0.00068 0.00067 0.00067 0.00036 C27 -0.63615 0.09590 0.13342 1.00000 0.03083 0.05137 0.02318 0.00158 0.00091 0.01383 0.03624 0.00436 0.00021 0.00023 0.00016 0.00000 0.00102 0.00125 0.00093 0.00084 0.00077 0.00089 0.00046 H27A -0.54938 0.14869 0.11894 1.00000 0.05436 0.00000 0.00000 H27B -0.71501 0.09172 0.06927 1.00000 0.05436 0.00000 0.00000 H27C -0.62984 0.00273 0.13614 1.00000 0.05436 0.00000 0.00000 C28 -0.66941 0.30982 0.25468 1.00000 0.03170 0.02914 0.05404 0.01310 0.00438 0.01109 0.03806 0.00462 0.00021 0.00020 0.00020 0.00000 0.00105 0.00102 0.00131 0.00093 0.00093 0.00081 0.00048 H28A -0.67247 0.35283 0.33508 1.00000 0.05708 0.00000 0.00000 H28B -0.75494 0.30759 0.19863 1.00000 0.05708 0.00000 0.00000 H28C -0.58810 0.36285 0.23265 1.00000 0.05708 0.00000 0.00000 C29 -0.78644 0.07977 0.28025 1.00000 0.02358 0.03620 0.03030 0.01090 -0.00015 0.00384 0.03114 0.00406 0.00018 0.00020 0.00017 0.00000 0.00091 0.00104 0.00097 0.00080 0.00074 0.00075 0.00041 H29A -0.77648 -0.01274 0.28079 1.00000 0.04672 0.00000 0.00000 H29B -0.86989 0.07419 0.22019 1.00000 0.04672 0.00000 0.00000 H29C -0.79566 0.12294 0.35857 1.00000 0.04672 0.00000 0.00000 B1 0.09270 0.24905 0.84861 1.00000 0.01884 0.02005 0.01877 0.00212 0.00126 0.00439 0.02006 0.00394 0.00019 0.00019 0.00016 0.00000 0.00088 0.00089 0.00087 0.00070 0.00070 0.00069 0.00037 N17 -0.16313 0.33185 0.69534 1.00000 0.01640 0.02004 0.01844 0.00255 0.00156 0.00287 0.01920 0.00284 0.00013 0.00013 0.00012 0.00000 0.00066 0.00068 0.00066 0.00053 0.00052 0.00051 0.00028 N20 -0.32504 0.23747 0.45915 1.00000 0.02146 0.03145 0.02020 0.00849 0.00085 -0.00294 0.02626 0.00310 0.00015 0.00015 0.00013 0.00000 0.00072 0.00081 0.00071 0.00060 0.00057 0.00059 0.00033 O2 0.15061 0.14027 0.84241 1.00000 0.02588 0.02506 0.02885 0.00870 0.01240 0.00979 0.02495 0.00267 0.00012 0.00012 0.00011 0.00000 0.00063 0.00062 0.00065 0.00050 0.00051 0.00049 0.00027 O5 0.14750 0.34237 0.78758 1.00000 0.01996 0.02238 0.02867 0.00617 0.00943 0.00695 0.02290 0.00255 0.00012 0.00012 0.00010 0.00000 0.00058 0.00060 0.00064 0.00049 0.00049 0.00045 0.00026 O24 -0.37537 0.29982 0.28431 1.00000 0.02801 0.03683 0.02312 0.01078 0.00699 0.00544 0.02922 0.00274 0.00013 0.00013 0.00011 0.00000 0.00067 0.00072 0.00063 0.00054 0.00052 0.00054 0.00029 O25 -0.54410 0.16446 0.34952 1.00000 0.02146 0.02723 0.01994 0.00702 -0.00105 0.00202 0.02420 0.00247 0.00012 0.00012 0.00010 0.00000 0.00060 0.00063 0.00058 0.00048 0.00047 0.00047 0.00026 Final Structure Factor Calculation for 2009src0001 in P-1 Total number of l.s. parameters = 269 Maximum vector length = 511 Memory required = 3650 / 24017 wR2 = 0.1151 before cycle 5 for 5193 data and 0 / 269 parameters GooF = S = 1.070; Restrained GooF = 1.070 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0202 * P )^2 + 0.90 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0555 for 4127 Fo > 4sig(Fo) and 0.0740 for all 5193 data wR2 = 0.1151, GooF = S = 1.070, Restrained GooF = 1.070 for all data Occupancy sum of asymmetric unit = 29.00 for non-hydrogen and 35.00 for hydrogen atoms Principal mean square atomic displacements U 0.0312 0.0240 0.0178 C3 0.0281 0.0237 0.0166 C4 0.0531 0.0289 0.0213 C6 0.0563 0.0328 0.0213 C7 0.0460 0.0304 0.0196 C8 0.0383 0.0323 0.0219 C9 0.0242 0.0202 0.0137 C10 0.0264 0.0243 0.0198 C11 0.0372 0.0249 0.0203 C12 0.0460 0.0237 0.0165 C13 0.0359 0.0204 0.0192 C14 0.0262 0.0207 0.0134 C15 0.0289 0.0199 0.0161 C16 0.0258 0.0225 0.0167 C18 0.0325 0.0243 0.0195 C19 0.0416 0.0196 0.0175 C21 0.0316 0.0206 0.0170 C22 0.0258 0.0221 0.0177 C23 0.0285 0.0261 0.0159 C26 0.0555 0.0318 0.0214 C27 0.0572 0.0330 0.0240 C28 0.0429 0.0297 0.0208 C29 0.0233 0.0208 0.0161 B1 0.0219 0.0208 0.0149 N17 0.0426 0.0190 0.0172 N20 0.0328 0.0230 0.0190 O2 0.0295 0.0222 0.0170 O5 0.0397 0.0279 0.0201 O24 0.0339 0.0229 0.0158 O25 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.009 0.018 0.026 0.036 0.048 0.062 0.081 0.106 0.153 1.000 Number in group 555. 532. 478. 520. 515. 516. 533. 504. 520. 520. GooF 1.100 1.115 1.148 1.088 1.122 1.096 1.008 0.939 1.007 1.061 K 4.260 1.460 1.077 1.016 1.005 1.001 1.004 1.005 1.008 0.996 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.65 inf Number in group 537. 509. 520. 511. 517. 526. 515. 520. 517. 521. GooF 1.137 1.162 1.132 1.117 1.027 0.951 1.010 0.907 0.990 1.221 K 1.072 1.069 1.073 1.028 1.001 0.991 0.984 0.994 1.019 0.993 R1 0.184 0.173 0.152 0.132 0.092 0.063 0.054 0.039 0.041 0.030 Recommended weighting scheme: WGHT 0.0199 0.8990 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/su Fc/Fc(max) Resolution(A) 4 -4 1 264.40 201.87 3.82 0.126 1.96 -5 0 3 357.82 283.05 3.75 0.149 1.89 -9 1 10 49.06 19.70 3.59 0.039 0.88 -5 1 12 25.97 4.20 3.51 0.018 0.92 11 -8 2 18.98 1.08 3.48 0.009 0.80 -1 1 1 4970.86 5687.86 3.41 0.669 6.54 2 4 7 8.88 24.94 3.40 0.044 1.10 8 0 6 49.99 23.30 3.34 0.043 0.92 1 3 8 34.22 59.61 3.30 0.068 1.15 -7 2 0 20.26 6.92 3.15 0.023 1.42 5 6 6 -3.02 6.05 3.14 0.022 0.85 -8 -1 10 9.56 26.61 3.13 0.046 0.93 -9 -2 10 194.13 142.05 3.13 0.106 0.86 -1 -1 2 7338.04 8077.83 3.13 0.797 4.88 -1 -6 10 11.51 0.10 3.12 0.003 1.04 5 -1 4 2.13 11.36 3.09 0.030 1.49 -7 -8 3 -1.25 10.31 3.07 0.028 0.84 5 -13 1 2.88 27.28 3.02 0.046 0.78 5 -2 4 8.74 1.91 3.00 0.012 1.51 2 -13 6 110.67 60.47 2.97 0.069 0.77 -1 -1 6 4.02 13.92 2.94 0.033 1.96 9 -11 2 68.47 38.49 2.94 0.055 0.79 5 1 0 141.35 107.42 2.94 0.092 1.79 -2 -11 8 136.93 90.99 2.93 0.085 0.81 -12 5 2 13.84 0.29 2.93 0.005 0.83 -1 -1 1 4478.91 4915.56 2.92 0.622 6.12 9 3 5 72.08 41.24 2.90 0.057 0.79 1 7 10 40.65 18.39 2.87 0.038 0.77 -6 3 4 10.69 24.41 2.87 0.044 1.48 -11 9 0 31.60 3.45 2.85 0.016 0.79 -1 2 0 4469.12 4891.43 2.85 0.620 4.91 -9 2 10 103.07 149.15 2.85 0.108 0.87 1 -2 1 2691.03 2955.60 2.84 0.482 4.69 -12 3 1 33.46 62.15 2.84 0.070 0.84 -4 -5 12 62.34 34.54 2.84 0.052 0.90 0 -2 1 2623.28 2882.77 2.83 0.476 4.89 -8 -4 3 36.98 18.71 2.83 0.038 1.01 3 -12 4 22.44 6.13 2.81 0.022 0.85 3 -6 6 6.00 0.60 2.81 0.007 1.31 -4 -6 14 25.89 9.03 2.80 0.027 0.78 1 9 6 -3.67 5.41 2.75 0.021 0.83 -7 -7 6 16.86 4.59 2.74 0.019 0.89 1 5 11 10.18 1.60 2.74 0.011 0.81 -4 0 8 21.18 9.74 2.73 0.028 1.36 0 6 10 7.47 0.20 2.72 0.004 0.84 -2 12 3 20.77 2.06 2.71 0.013 0.79 -7 0 10 1.95 11.54 2.69 0.030 0.99 8 2 4 11.95 26.53 2.69 0.046 0.94 -9 -3 1 28.00 48.65 2.69 0.062 0.96 -3 3 3 10.50 3.03 2.69 0.015 2.18 Bond lengths and angles C3 - Distance Angles O2 1.4612 (0.0020) C7 1.5172 (0.0025) 109.15 (0.14) C6 1.5210 (0.0025) 106.00 (0.14) 110.84 (0.16) C4 1.5578 (0.0024) 102.03 (0.12) 115.33 (0.15) 112.66 (0.15) C3 - O2 C7 C6 C4 - Distance Angles O5 1.4597 (0.0019) C9 1.5184 (0.0024) 108.67 (0.14) C8 1.5245 (0.0024) 106.23 (0.13) 110.46 (0.15) C3 1.5578 (0.0024) 101.99 (0.12) 115.19 (0.15) 113.47 (0.15) C4 - O5 C9 C8 C6 - Distance Angles C3 1.5210 (0.0025) H6A 0.9800 109.47 H6B 0.9800 109.47 109.47 H6C 0.9800 109.47 109.47 109.47 C6 - C3 H6A H6B C7 - Distance Angles C3 1.5172 (0.0025) H7A 0.9800 109.47 H7B 0.9800 109.47 109.47 H7C 0.9800 109.47 109.47 109.47 C7 - C3 H7A H7B C8 - Distance Angles C4 1.5245 (0.0024) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - C4 H8A H8B C9 - Distance Angles C4 1.5184 (0.0024) H9A 0.9800 109.47 H9B 0.9800 109.47 109.47 H9C 0.9800 109.47 109.47 109.47 C9 - C4 H9A H9B C10 - Distance Angles C11 1.4001 (0.0023) C15 1.4115 (0.0022) 117.96 (0.15) B1 1.5573 (0.0024) 117.61 (0.15) 124.43 (0.15) C10 - C11 C15 C11 - Distance Angles C12 1.3846 (0.0024) C10 1.4001 (0.0023) 121.94 (0.16) H11 0.9500 119.03 119.03 C11 - C12 C10 C12 - Distance Angles C11 1.3846 (0.0024) C13 1.3863 (0.0026) 119.54 (0.16) H12 0.9500 120.23 120.23 C12 - C11 C13 C13 - Distance Angles C14 1.3860 (0.0026) C12 1.3863 (0.0026) 119.56 (0.16) H13 0.9500 120.22 120.22 C13 - C14 C12 C14 - Distance Angles C13 1.3860 (0.0026) C15 1.3891 (0.0023) 121.47 (0.16) H14 0.9500 119.26 119.26 C14 - C13 C15 C15 - Distance Angles C14 1.3891 (0.0023) C10 1.4115 (0.0022) 119.52 (0.15) C16 1.5098 (0.0023) 120.35 (0.15) 120.12 (0.14) C15 - C14 C10 C16 - Distance Angles N17 1.4701 (0.0020) C15 1.5098 (0.0023) 111.60 (0.13) H16A 0.9900 109.30 109.30 H16B 0.9900 109.30 109.30 107.96 C16 - N17 C15 H16A C18 - Distance Angles N17 1.4569 (0.0020) C19 1.5155 (0.0023) 110.22 (0.13) H18A 0.9900 109.61 109.61 H18B 0.9900 109.61 109.61 108.14 C18 - N17 C19 H18A C19 - Distance Angles N20 1.4585 (0.0021) C18 1.5155 (0.0023) 110.43 (0.14) H19A 0.9900 109.57 109.57 H19B 0.9900 109.57 109.57 108.11 C19 - N20 C18 H19A C21 - Distance Angles N20 1.4553 (0.0021) C22 1.5184 (0.0023) 109.62 (0.14) H21A 0.9900 109.75 109.75 H21B 0.9900 109.75 109.75 108.22 C21 - N20 C22 H21A C22 - Distance Angles N17 1.4618 (0.0020) C21 1.5184 (0.0023) 110.79 (0.14) H22A 0.9900 109.49 109.49 H22B 0.9900 109.49 109.49 108.06 C22 - N17 C21 H22A C23 - Distance Angles O24 1.2164 (0.0020) O25 1.3501 (0.0020) 125.07 (0.15) N20 1.3528 (0.0021) 123.47 (0.15) 111.46 (0.14) C23 - O24 O25 C26 - Distance Angles O25 1.4793 (0.0019) C28 1.5132 (0.0025) 110.07 (0.14) C27 1.5189 (0.0024) 110.01 (0.14) 113.05 (0.16) C29 1.5196 (0.0024) 102.46 (0.13) 110.10 (0.15) 110.64 (0.15) C26 - O25 C28 C27 C27 - Distance Angles C26 1.5189 (0.0024) H27A 0.9800 109.47 H27B 0.9800 109.47 109.47 H27C 0.9800 109.47 109.47 109.47 C27 - C26 H27A H27B C28 - Distance Angles C26 1.5132 (0.0025) H28A 0.9800 109.47 H28B 0.9800 109.47 109.47 H28C 0.9800 109.47 109.47 109.47 C28 - C26 H28A H28B C29 - Distance Angles C26 1.5196 (0.0024) H29A 0.9800 109.47 H29B 0.9800 109.47 109.47 H29C 0.9800 109.47 109.47 109.47 C29 - C26 H29A H29B B1 - Distance Angles O5 1.3722 (0.0022) O2 1.3726 (0.0021) 112.76 (0.15) C10 1.5573 (0.0024) 126.37 (0.15) 120.78 (0.15) B1 - O5 O2 N17 - Distance Angles C18 1.4569 (0.0020) C22 1.4618 (0.0020) 110.00 (0.12) C16 1.4701 (0.0020) 110.97 (0.12) 110.90 (0.13) N17 - C18 C22 N20 - Distance Angles C23 1.3528 (0.0021) C21 1.4553 (0.0021) 125.44 (0.14) C19 1.4585 (0.0021) 120.38 (0.14) 114.19 (0.13) N20 - C23 C21 O2 - Distance Angles B1 1.3726 (0.0022) C3 1.4612 (0.0020) 106.89 (0.13) O2 - B1 O5 - Distance Angles B1 1.3722 (0.0022) C4 1.4597 (0.0019) 107.16 (0.13) O5 - B1 O24 - Distance Angles C23 1.2164 (0.0020) O24 - O25 - Distance Angles C23 1.3501 (0.0020) C26 1.4793 (0.0019) 119.61 (0.13) O25 - C23 FMAP and GRID set by program FMAP 2 1 26 GRID -2.174 -2 -2 2.174 2 2 R1 = 0.0740 for 5193 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.27 at 0.2476 0.2214 0.7457 [ 0.75 A from C3 ] Deepest hole -0.25 at 0.4778 0.7540 0.6811 [ 0.76 A from C23 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 3545 / 25103 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2476 0.2214 0.7457 1.00000 0.05 0.27 0.75 C3 0.82 C4 1.82 O2 1.83 O5 Q2 1 0.0468 0.2736 0.9003 1.00000 0.05 0.22 0.74 C10 0.87 B1 1.87 C11 1.90 C15 Q3 1 -0.1209 0.3795 0.8622 1.00000 0.05 0.21 0.73 C15 0.79 C16 1.42 H16A 1.52 H16B Q4 1 -0.0446 0.3151 0.9227 1.00000 0.05 0.20 0.67 C10 0.79 C15 1.86 C11 1.95 C14 Q5 1 0.0022 0.2539 0.9839 1.00000 0.05 0.19 0.71 C10 0.83 C11 1.53 H11 1.82 C15 Q6 1 -0.2381 0.3055 0.6805 1.00000 0.05 0.19 0.72 N17 0.74 C22 1.40 H22A 1.46 H22B Q7 1 -0.1780 0.3334 1.0496 1.00000 0.05 0.19 0.71 C13 0.81 C14 1.44 H13 1.53 H14 Q8 1 0.0794 0.1068 1.0395 1.00000 0.05 0.19 0.55 H11 1.48 C11 2.09 H27B 2.20 H29B Q9 1 -0.0841 0.2862 0.8919 1.00000 0.05 0.18 0.72 C15 0.83 C10 1.86 C16 1.91 C14 Q10 1 -0.1297 0.2641 1.0956 1.00000 0.05 0.18 0.76 C12 0.80 C13 1.50 H12 1.53 H13 Shortest distances between peaks (including symmetry equivalents) 4 9 0.48 7 10 1.11 4 5 1.14 2 4 1.15 2 5 1.18 3 9 1.19 3 4 1.32 2 9 1.35 5 9 1.40 5 8 2.01 5 10 2.04 3 6 2.16 4 7 2.19 2 3 2.23 7 9 2.26 8 8 2.32 5 7 2.35 4 10 2.44 3 5 2.45 3 7 2.47 9 10 2.56 2 8 2.60 6 9 2.75 Time profile in seconds ----------------------- 0.03: 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. 1.08: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.19: Structure factors and derivatives 2.42: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.00: Apply other restraints 0.25: Solve l.s. equations 0.00: Generate HTAB table 0.02: Other dependent quantities, CIF, tables 0.13: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.06: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2009src0001 finished at 13:00:02 Total CPU time: 5.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++