+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2005src0502 started at 22:44:43 on 18-Apr-2005 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2005src0502 in P2(1)/c CELL 0.71073 14.5879 10.4825 12.6410 90.000 91.815 90.000 ZERR 4.00 0.0019 0.0009 0.0023 0.000 0.016 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 84 108 4 16 V = 1932.06 F(000) = 768.0 Mu = 0.08 mm-1 Cell Wt = 1429.74 Rho = 1.229 MERG 2 OMIT -3.00 55.00 OMIT -3 3 6 OMIT -1 1 2 OMIT 0 3 3 OMIT 0 1 3 OMIT 3 6 3 OMIT 0 6 6 OMIT -6 3 3 EXTI 0.00489 FMAP 2 PLAN 20 SIZE 0.01 0.30 0.34 ACTA BOND WGHT 0.05450 1.15300 L.S. 4 TEMP -123.00 FVAR 0.72199 C1 1 0.508709 0.452785 0.162353 11.00000 0.03332 0.03453 = 0.04780 -0.00572 0.00138 0.00538 AFIX 137 H1A 2 0.467734 0.381816 0.178553 11.00000 -1.50000 H1B 2 0.479529 0.507069 0.107892 11.00000 -1.50000 H1C 2 0.521069 0.503145 0.226546 11.00000 -1.50000 AFIX 0 C2 1 0.640984 0.320074 0.188699 11.00000 0.03188 0.02640 = 0.03609 -0.00102 0.00165 0.00020 C3 1 0.610519 0.272906 0.284319 11.00000 0.02751 0.03304 = 0.03519 -0.00443 0.00581 -0.00204 AFIX 43 H3 2 0.553667 0.300209 0.311142 11.00000 -1.20000 AFIX 0 C4 1 0.665168 0.184552 0.340186 11.00000 0.02844 0.03256 = 0.02778 -0.00069 0.00449 -0.00672 AFIX 43 H4 2 0.644485 0.151963 0.405373 11.00000 -1.20000 AFIX 0 C5 1 0.748078 0.143306 0.303610 11.00000 0.02873 0.02376 = 0.02696 -0.00392 0.00092 -0.00610 C6 1 0.778078 0.194002 0.209785 11.00000 0.02963 0.02905 = 0.03108 -0.00104 0.00544 0.00089 AFIX 43 H6 2 0.835604 0.168104 0.183887 11.00000 -1.20000 AFIX 0 C7 1 0.725509 0.281925 0.153063 11.00000 0.03514 0.02956 = 0.03274 0.00323 0.00991 0.00097 AFIX 43 H7 2 0.747589 0.316366 0.089189 11.00000 -1.20000 AFIX 0 C8 1 0.802880 0.039770 0.362013 11.00000 0.02901 0.02695 = 0.02658 -0.00249 0.00056 -0.00434 AFIX 13 H8 2 0.784171 0.042453 0.437404 11.00000 -1.20000 AFIX 0 C9 1 0.906349 0.061513 0.363130 11.00000 0.03147 0.02736 = 0.02407 0.00186 0.00119 0.00062 C10 1 0.965384 -0.014255 0.306235 11.00000 0.03851 0.03095 = 0.02855 -0.00703 -0.00224 0.00098 AFIX 43 H10 2 0.941488 -0.080787 0.262416 11.00000 -1.20000 AFIX 0 C11 1 1.058988 0.007100 0.313331 11.00000 0.03585 0.03902 = 0.03415 -0.00944 0.00529 0.00587 AFIX 43 H11 2 1.098770 -0.044473 0.273393 11.00000 -1.20000 AFIX 0 C12 1 1.095601 0.102301 0.377615 11.00000 0.02852 0.03480 = 0.03351 -0.00266 -0.00137 0.00152 AFIX 43 H12 2 1.160102 0.114900 0.381931 11.00000 -1.20000 AFIX 0 C13 1 1.038550 0.179591 0.435903 11.00000 0.03021 0.02453 = 0.02459 -0.00026 -0.00106 -0.00009 C14 1 0.944092 0.158983 0.426166 11.00000 0.03025 0.02509 = 0.02247 0.00087 0.00342 0.00117 C15 1 0.866795 0.357316 0.446122 11.00000 0.03738 0.02513 = 0.03875 -0.00089 0.00597 0.00047 AFIX 137 H15A 2 0.923334 0.395282 0.420511 11.00000 -1.50000 H15B 2 0.842766 0.410611 0.502593 11.00000 -1.50000 H15C 2 0.821207 0.351734 0.387677 11.00000 -1.50000 AFIX 0 C16 1 1.074279 0.280250 0.512932 11.00000 0.02902 0.03117 = 0.03185 -0.00406 0.00332 -0.00275 AFIX 23 H16A 2 1.054699 0.365146 0.486382 11.00000 -1.20000 H16B 2 1.045419 0.266688 0.581869 11.00000 -1.20000 AFIX 0 C17 1 1.227705 0.343489 0.464260 11.00000 0.03110 0.02196 = 0.02445 -0.00355 -0.00159 -0.00069 C18 1 1.331457 0.339628 0.489118 11.00000 0.02827 0.02783 = 0.03177 0.00199 -0.00210 0.00075 C19 1 1.366890 0.209804 0.451997 11.00000 0.03463 0.04596 = 0.04666 -0.01051 -0.00131 0.00672 AFIX 137 H19A 2 1.336624 0.141540 0.490728 11.00000 -1.50000 H19B 2 1.433315 0.204950 0.465556 11.00000 -1.50000 H19C 2 1.353361 0.200012 0.375999 11.00000 -1.50000 AFIX 0 C20 1 1.353481 0.357525 0.607215 11.00000 0.03610 0.04400 = 0.03784 -0.00401 -0.00814 -0.00226 AFIX 137 H20A 2 1.326604 0.437764 0.631170 11.00000 -1.50000 H20B 2 1.420138 0.360017 0.619381 11.00000 -1.50000 H20C 2 1.327820 0.286268 0.646806 11.00000 -1.50000 AFIX 0 C21 1 1.377203 0.445843 0.426529 11.00000 0.03267 0.05376 = 0.05739 0.02185 -0.00374 -0.00898 AFIX 137 H21A 2 1.362009 0.435356 0.350957 11.00000 -1.50000 H21B 2 1.443859 0.441240 0.438153 11.00000 -1.50000 H21C 2 1.355018 0.528915 0.450416 11.00000 -1.50000 AFIX 0 N1 3 1.173395 0.281346 0.530098 11.00000 0.02896 0.02920 = 0.02773 0.00304 -0.00385 -0.00300 O1 4 0.592655 0.403869 0.124687 11.00000 0.03766 0.03858 = 0.04556 0.00906 0.00949 0.01202 O2 4 0.777081 -0.082996 0.321899 11.00000 0.04433 0.02900 = 0.02725 0.00040 -0.00263 -0.00652 AFIX 147 H2 2 0.782279 -0.084070 0.255915 11.00000 -1.50000 AFIX 0 O3 4 0.885973 0.231669 0.486577 11.00000 0.03069 0.02632 = 0.02832 -0.00197 0.00717 0.00066 O4 4 1.194514 0.401961 0.387280 11.00000 0.03604 0.03099 = 0.02945 0.00580 -0.00367 0.00196 H1N 2 1.196343 0.234172 0.581726 11.00000 0.03784 HKLF 4 1.0 0.00 0.00 1.00 0.00 -1.00 0.00 1.00 0.00 0.00 Covalent radii and connectivity table for 2005src0502 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 C1 - O1 C2 - O1 C7 C3 C3 - C2 C4 C4 - C5 C3 C5 - C4 C6 C8 C6 - C5 C7 C7 - C6 C2 C8 - O2 C5 C9 C9 - C10 C14 C8 C10 - C11 C9 C11 - C12 C10 C12 - C11 C13 C13 - C12 C14 C16 C14 - O3 C13 C9 C15 - O3 C16 - N1 C13 C17 - O4 N1 C18 C18 - C20 C21 C19 C17 C19 - C18 C20 - C18 C21 - C18 N1 - C17 C16 O1 - C2 C1 O2 - C8 O3 - C14 C15 O4 - C17 h k l Fo^2 Sigma Why rejected -14 0 7 11.75 2.18 observed but should be systematically absent 19473 Reflections read, of which 556 rejected -15 =< h =< 18, -11 =< k =< 12, -14 =< l =< 16, Max. 2-theta = 54.99 1 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -1 8 1 29.00 3.99 4 24.60 -7 1 2 -0.04 0.09 6 0.54 2 7 2 3.38 0.30 9 1.83 -10 6 6 22.37 6.55 3 42.61 4 Inconsistent equivalents 4288 Unique reflections, of which 0 suppressed R(int) = 0.0757 R(sigma) = 0.0692 Friedel opposites merged Maximum memory for data reduction = 2433 / 42129 Default effective X-H distances for T = -123.0 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 = 3132 / 305280 wR2 = 0.1516 before cycle 1 for 4288 data and 246 / 246 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0545 * P )^2 + 1.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72193 0.00208 -0.030 OSF 2 0.00486 0.00216 -0.016 EXTI Mean shift/esd = 0.015 Maximum = -0.058 for x C9 Max. shift = 0.001 A for H1N Max. dU = 0.000 for C9 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3132 / 305280 wR2 = 0.1516 before cycle 2 for 4288 data and 246 / 246 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0545 * P )^2 + 1.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72191 0.00208 -0.007 OSF 2 0.00484 0.00216 -0.007 EXTI Mean shift/esd = 0.006 Maximum = -0.023 for U22 C14 Max. shift = 0.001 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 3 Maximum vector length = 511 Memory required = 3132 / 305280 wR2 = 0.1516 before cycle 3 for 4288 data and 246 / 246 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0545 * P )^2 + 1.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72191 0.00208 0.000 OSF 2 0.00484 0.00216 0.000 EXTI Mean shift/esd = 0.001 Maximum = 0.005 for tors H15A Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 4 Maximum vector length = 511 Memory required = 3132 / 305280 wR2 = 0.1516 before cycle 4 for 4288 data and 246 / 246 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0545 * P )^2 + 1.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.72191 0.00208 0.001 OSF 2 0.00484 0.00216 0.000 EXTI Mean shift/esd = 0.000 Maximum = 0.002 for tors H15A Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Largest correlation matrix elements 0.564 EXTI / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.4677 0.3818 0.1785 137 0.980 0.000 C1 O1 H1A H1B 0.4795 0.5071 0.1079 137 0.980 0.000 C1 O1 H1A H1C 0.5211 0.5031 0.2266 137 0.980 0.000 C1 O1 H1A H3 0.5537 0.3002 0.3111 43 0.950 0.000 C3 C2 C4 H4 0.6445 0.1520 0.4054 43 0.950 0.000 C4 C5 C3 H6 0.8356 0.1681 0.1839 43 0.950 0.000 C6 C5 C7 H7 0.7476 0.3164 0.0892 43 0.950 0.000 C7 C6 C2 H8 0.7842 0.0425 0.4374 13 1.000 0.000 C8 O2 C5 C9 H10 0.9415 -0.0808 0.2624 43 0.950 0.000 C10 C11 C9 H11 1.0988 -0.0445 0.2734 43 0.950 0.000 C11 C12 C10 H12 1.1601 0.1149 0.3819 43 0.950 0.000 C12 C11 C13 H15A 0.9233 0.3953 0.4205 137 0.980 0.000 C15 O3 H15A H15B 0.8428 0.4106 0.5026 137 0.980 0.000 C15 O3 H15A H15C 0.8212 0.3517 0.3877 137 0.980 0.000 C15 O3 H15A H16A 1.0547 0.3651 0.4864 23 0.990 0.000 C16 N1 C13 H16B 1.0454 0.2667 0.5819 23 0.990 0.000 C16 N1 C13 H19A 1.3366 0.1415 0.4908 137 0.980 0.000 C19 C18 H19A H19B 1.4333 0.2050 0.4655 137 0.980 0.000 C19 C18 H19A H19C 1.3533 0.2000 0.3760 137 0.980 0.000 C19 C18 H19A H20A 1.3266 0.4378 0.6312 137 0.980 0.000 C20 C18 H20A H20B 1.4201 0.3600 0.6194 137 0.980 0.000 C20 C18 H20A H20C 1.3278 0.2863 0.6468 137 0.980 0.000 C20 C18 H20A H21A 1.3619 0.4354 0.3510 137 0.980 0.000 C21 C18 H21A H21B 1.4439 0.4412 0.4381 137 0.980 0.000 C21 C18 H21A H21C 1.3551 0.5289 0.4505 137 0.980 0.000 C21 C18 H21A H2 0.7822 -0.0841 0.2559 147 0.840 0.000 O2 C8 H2 2005src0502 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.50871 0.45279 0.16235 1.00000 0.03330 0.03452 0.04784 -0.00574 0.00140 0.00540 0.03855 0.00442 0.00016 0.00023 0.00021 0.00000 0.00133 0.00133 0.00159 0.00109 0.00111 0.00099 0.00059 H1A 0.46773 0.38183 0.17854 1.00000 0.05783 0.00000 0.00000 H1B 0.47954 0.50709 0.10790 1.00000 0.05783 0.00000 0.00000 H1C 0.52108 0.50314 0.22655 1.00000 0.05783 0.00000 0.00000 C2 0.64099 0.32008 0.18870 1.00000 0.03190 0.02633 0.03608 -0.00103 0.00162 0.00022 0.03143 0.00398 0.00016 0.00020 0.00019 0.00000 0.00125 0.00119 0.00136 0.00093 0.00100 0.00088 0.00052 C3 0.61052 0.27290 0.28431 1.00000 0.02752 0.03301 0.03515 -0.00444 0.00580 -0.00204 0.03179 0.00390 0.00015 0.00021 0.00019 0.00000 0.00118 0.00126 0.00136 0.00098 0.00097 0.00092 0.00052 H3 0.55367 0.30019 0.31113 1.00000 0.03815 0.00000 0.00000 C4 0.66517 0.18455 0.34018 1.00000 0.02843 0.03251 0.02780 -0.00066 0.00447 -0.00671 0.02950 0.00376 0.00015 0.00020 0.00018 0.00000 0.00119 0.00120 0.00123 0.00090 0.00093 0.00088 0.00050 H4 0.64448 0.15195 0.40536 1.00000 0.03541 0.00000 0.00000 C5 0.74808 0.14331 0.30361 1.00000 0.02872 0.02373 0.02695 -0.00391 0.00092 -0.00609 0.02646 0.00354 0.00014 0.00020 0.00017 0.00000 0.00116 0.00110 0.00122 0.00085 0.00090 0.00083 0.00048 C6 0.77807 0.19401 0.20978 1.00000 0.02967 0.02904 0.03106 -0.00105 0.00545 0.00090 0.02983 0.00390 0.00015 0.00020 0.00018 0.00000 0.00120 0.00118 0.00129 0.00091 0.00095 0.00087 0.00051 H6 0.83560 0.16812 0.18388 1.00000 0.03580 0.00000 0.00000 C7 0.72551 0.28192 0.15307 1.00000 0.03515 0.02952 0.03273 0.00326 0.00993 0.00097 0.03228 0.00410 0.00015 0.00021 0.00019 0.00000 0.00131 0.00122 0.00132 0.00096 0.00101 0.00095 0.00053 H7 0.74759 0.31636 0.08920 1.00000 0.03873 0.00000 0.00000 C8 0.80288 0.03978 0.36201 1.00000 0.02901 0.02692 0.02660 -0.00251 0.00051 -0.00436 0.02752 0.00360 0.00014 0.00020 0.00018 0.00000 0.00118 0.00115 0.00120 0.00087 0.00091 0.00085 0.00049 H8 0.78417 0.04246 0.43740 1.00000 0.03302 0.00000 0.00000 C9 0.90634 0.06152 0.36313 1.00000 0.03142 0.02732 0.02405 0.00182 0.00120 0.00061 0.02759 0.00379 0.00015 0.00020 0.00017 0.00000 0.00120 0.00112 0.00117 0.00086 0.00091 0.00087 0.00049 C10 0.96539 -0.01425 0.30622 1.00000 0.03849 0.03095 0.02855 -0.00705 -0.00226 0.00101 0.03274 0.00401 0.00016 0.00022 0.00019 0.00000 0.00137 0.00125 0.00126 0.00093 0.00099 0.00094 0.00054 H10 0.94150 -0.08077 0.26240 1.00000 0.03928 0.00000 0.00000 C11 1.05898 0.00711 0.31332 1.00000 0.03584 0.03896 0.03415 -0.00943 0.00530 0.00585 0.03623 0.00418 0.00016 0.00023 0.00019 0.00000 0.00135 0.00135 0.00140 0.00103 0.00105 0.00102 0.00057 H11 1.09876 -0.04446 0.27337 1.00000 0.04347 0.00000 0.00000 C12 1.09560 0.10231 0.37762 1.00000 0.02851 0.03482 0.03347 -0.00264 -0.00135 0.00151 0.03232 0.00401 0.00016 0.00021 0.00019 0.00000 0.00120 0.00126 0.00134 0.00098 0.00097 0.00092 0.00053 H12 1.16010 0.11491 0.38193 1.00000 0.03878 0.00000 0.00000 C13 1.03855 0.17958 0.43590 1.00000 0.03015 0.02448 0.02459 -0.00025 -0.00104 -0.00010 0.02645 0.00367 0.00015 0.00019 0.00017 0.00000 0.00119 0.00111 0.00117 0.00083 0.00090 0.00084 0.00048 C14 0.94410 0.15898 0.42616 1.00000 0.03029 0.02500 0.02248 0.00085 0.00343 0.00118 0.02587 0.00376 0.00014 0.00020 0.00017 0.00000 0.00119 0.00113 0.00115 0.00083 0.00089 0.00083 0.00048 C15 0.86680 0.35732 0.44612 1.00000 0.03738 0.02509 0.03880 -0.00088 0.00596 0.00051 0.03366 0.00422 0.00016 0.00020 0.00020 0.00000 0.00130 0.00119 0.00141 0.00095 0.00105 0.00093 0.00054 H15A 0.92333 0.39526 0.42047 1.00000 0.05048 0.00000 0.00000 H15B 0.84280 0.41063 0.50261 1.00000 0.05048 0.00000 0.00000 H15C 0.82118 0.35174 0.38771 1.00000 0.05048 0.00000 0.00000 C16 1.07427 0.28025 0.51293 1.00000 0.02899 0.03118 0.03183 -0.00408 0.00334 -0.00277 0.03062 0.00375 0.00015 0.00021 0.00018 0.00000 0.00120 0.00121 0.00131 0.00094 0.00096 0.00091 0.00051 H16A 1.05469 0.36514 0.48638 1.00000 0.03674 0.00000 0.00000 H16B 1.04541 0.26669 0.58186 1.00000 0.03674 0.00000 0.00000 C17 1.22771 0.34349 0.46426 1.00000 0.03112 0.02197 0.02445 -0.00355 -0.00158 -0.00069 0.02590 0.00360 0.00015 0.00019 0.00017 0.00000 0.00117 0.00107 0.00119 0.00085 0.00090 0.00084 0.00047 C18 1.33146 0.33963 0.48912 1.00000 0.02821 0.02782 0.03177 0.00201 -0.00206 0.00074 0.02933 0.00382 0.00015 0.00020 0.00018 0.00000 0.00119 0.00120 0.00130 0.00092 0.00095 0.00086 0.00051 C19 1.36688 0.20980 0.45201 1.00000 0.03465 0.04597 0.04666 -0.01050 -0.00133 0.00676 0.04248 0.00448 0.00017 0.00024 0.00022 0.00000 0.00136 0.00153 0.00161 0.00120 0.00116 0.00109 0.00063 H19A 1.33663 0.14154 0.49076 1.00000 0.06372 0.00000 0.00000 H19B 1.43331 0.20495 0.46554 1.00000 0.06372 0.00000 0.00000 H19C 1.35333 0.19999 0.37601 1.00000 0.06372 0.00000 0.00000 C20 1.35348 0.35752 0.60722 1.00000 0.03609 0.04400 0.03786 -0.00404 -0.00813 -0.00222 0.03951 0.00415 0.00017 0.00025 0.00020 0.00000 0.00137 0.00146 0.00148 0.00110 0.00109 0.00106 0.00060 H20A 1.32664 0.43778 0.63116 1.00000 0.05927 0.00000 0.00000 H20B 1.42014 0.35996 0.61938 1.00000 0.05927 0.00000 0.00000 H20C 1.32779 0.28629 0.64681 1.00000 0.05927 0.00000 0.00000 C21 1.37720 0.44584 0.42653 1.00000 0.03266 0.05377 0.05739 0.02187 -0.00374 -0.00899 0.04805 0.00501 0.00017 0.00027 0.00024 0.00000 0.00139 0.00166 0.00185 0.00135 0.00125 0.00115 0.00072 H21A 1.36195 0.43542 0.35097 1.00000 0.07208 0.00000 0.00000 H21B 1.44387 0.44116 0.43809 1.00000 0.07208 0.00000 0.00000 H21C 1.35508 0.52891 0.45048 1.00000 0.07208 0.00000 0.00000 N1 1.17339 0.28135 0.53010 1.00000 0.02892 0.02920 0.02775 0.00309 -0.00385 -0.00300 0.02873 0.00320 0.00013 0.00018 0.00016 0.00000 0.00101 0.00104 0.00107 0.00082 0.00081 0.00076 0.00043 O1 0.59265 0.40387 0.12469 1.00000 0.03768 0.03856 0.04563 0.00911 0.00952 0.01203 0.04045 0.00318 0.00011 0.00015 0.00014 0.00000 0.00098 0.00097 0.00109 0.00077 0.00079 0.00072 0.00045 O2 0.77709 -0.08300 0.32190 1.00000 0.04435 0.02899 0.02725 0.00038 -0.00264 -0.00653 0.03361 0.00265 0.00012 0.00014 0.00012 0.00000 0.00098 0.00087 0.00089 0.00064 0.00075 0.00067 0.00040 H2 0.78223 -0.08406 0.25591 1.00000 0.05041 0.00000 0.00000 O3 0.88598 0.23167 0.48658 1.00000 0.03071 0.02629 0.02832 -0.00196 0.00718 0.00068 0.02831 0.00256 0.00010 0.00013 0.00012 0.00000 0.00085 0.00081 0.00087 0.00061 0.00065 0.00060 0.00037 O4 1.19451 0.40196 0.38728 1.00000 0.03604 0.03100 0.02945 0.00581 -0.00367 0.00194 0.03226 0.00270 0.00011 0.00014 0.00012 0.00000 0.00090 0.00086 0.00091 0.00067 0.00070 0.00065 0.00039 H1N 1.19639 0.23406 0.58160 1.00000 0.03789 0.04417 0.00169 0.00241 0.00216 0.00000 0.00708 Final Structure Factor Calculation for 2005src0502 in P2(1)/c Total number of l.s. parameters = 246 Maximum vector length = 511 Memory required = 2886 / 22995 wR2 = 0.1516 before cycle 5 for 4288 data and 0 / 246 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0545 * P )^2 + 1.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0615 for 2899 Fo > 4sig(Fo) and 0.1023 for all 4288 data wR2 = 0.1516, GooF = S = 1.032, Restrained GooF = 1.032 for all data Occupancy sum of asymmetric unit = 26.00 for non-hydrogen and 27.00 for hydrogen atoms Principal mean square atomic displacements U 0.0502 0.0379 0.0275 C1 0.0362 0.0318 0.0262 C2 0.0405 0.0299 0.0250 C3 0.0381 0.0283 0.0221 C4 0.0335 0.0274 0.0185 C5 0.0348 0.0295 0.0252 C6 0.0432 0.0296 0.0240 C7 0.0327 0.0275 0.0224 C8 0.0315 0.0280 0.0232 C9 0.0410 0.0348 0.0224 C10 0.0469 0.0390 0.0228 C11 0.0377 0.0316 0.0276 C12 0.0308 0.0246 0.0239 C13 0.0313 0.0248 0.0216 C14 0.0428 0.0332 0.0250 C15 0.0371 0.0277 0.0271 C16 0.0320 0.0265 0.0192 C17 0.0339 0.0287 0.0254 C18 0.0589 0.0377 0.0309 C19 0.0475 0.0442 0.0268 C20 0.0800 0.0357 0.0285 C21 0.0361 0.0264 0.0237 N1 0.0600 0.0353 0.0261 O1 0.0475 0.0275 0.0258 O2 0.0357 0.0272 0.0220 O3 0.0389 0.0352 0.0228 O4 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 0.027 0.037 0.049 0.063 0.083 0.110 0.169 1.000 Number in group 446. 436. 424. 411. 449. 416. 427. 428. 421. 430. GooF 1.101 0.986 1.038 1.040 1.037 1.027 0.985 1.105 0.993 1.002 K 11.960 2.161 1.460 1.240 1.086 1.035 1.006 1.013 1.002 1.004 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.98 1.05 1.16 1.33 1.66 inf Number in group 434. 424. 436. 426. 425. 437. 421. 430. 424. 431. GooF 0.942 1.003 0.965 0.972 1.003 1.052 0.864 0.993 1.057 1.385 K 1.095 1.189 1.066 1.070 1.027 1.000 1.011 1.007 1.006 1.006 R1 0.271 0.268 0.201 0.179 0.129 0.098 0.058 0.060 0.053 0.042 Recommended weighting scheme: WGHT 0.0537 1.1640 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) 6 6 9 78.56 1.07 6.71 0.008 0.99 0 3 9 1002.03 550.95 6.50 0.179 1.30 -3 0 6 145.59 31.64 5.63 0.043 1.95 0 2 6 250.39 158.14 4.45 0.096 1.95 3 0 0 544.21 363.15 4.39 0.146 4.86 3 3 3 117.40 62.22 4.34 0.060 2.33 6 3 6 370.82 231.56 4.33 0.116 1.43 5 12 4 65.80 0.22 4.29 0.004 0.81 1 2 5 649.41 890.91 4.25 0.228 2.24 9 6 6 111.89 55.39 4.23 0.057 1.02 -6 6 3 32.60 5.88 4.17 0.019 1.35 5 2 3 37.86 9.09 4.16 0.023 2.15 -6 2 3 51.46 20.71 4.16 0.035 1.98 -3 6 6 250.47 158.74 4.10 0.096 1.30 3 6 6 609.58 443.85 3.95 0.161 1.29 -12 2 9 84.64 31.56 3.61 0.043 0.92 5 2 4 218.00 148.30 3.52 0.093 1.96 1 5 0 16.92 0.03 3.47 0.001 2.08 0 6 0 87.21 0.11 3.40 0.003 1.75 -2 5 6 46.57 20.25 3.40 0.034 1.46 -1 2 6 23.88 4.83 3.32 0.017 1.94 -11 2 11 270.82 176.00 3.27 0.101 0.87 0 6 12 52.93 0.98 3.21 0.008 0.90 -4 1 13 102.89 2.20 3.21 0.011 0.94 8 4 0 16.72 2.50 3.17 0.012 1.50 -9 6 9 37.19 8.54 3.17 0.022 0.92 2 1 3 273.45 201.49 3.16 0.108 3.40 13 7 6 29.47 3.47 3.12 0.014 0.82 -6 9 3 57.01 27.69 3.12 0.040 1.02 9 3 3 57.58 26.39 3.06 0.039 1.38 -11 9 2 209.04 127.24 3.06 0.086 0.87 4 1 14 164.33 260.83 3.05 0.123 0.87 -15 5 4 -5.19 19.97 3.04 0.034 0.86 -3 3 3 1311.11 1043.66 3.01 0.247 2.37 -2 3 15 77.04 12.85 2.99 0.027 0.82 -7 5 4 57.20 31.98 2.96 0.043 1.35 4 4 0 13.64 3.30 2.93 0.014 2.13 7 7 7 26.33 3.26 2.90 0.014 1.00 -6 4 14 170.71 61.00 2.90 0.060 0.81 -2 2 5 47.48 23.47 2.89 0.037 2.19 9 3 0 170.87 124.20 2.88 0.085 1.47 -3 12 7 1.25 46.25 2.86 0.052 0.78 -5 2 9 17.72 0.72 2.84 0.006 1.24 -11 4 7 36.78 10.12 2.84 0.024 1.00 3 3 6 420.33 327.62 2.82 0.138 1.68 7 9 1 34.58 15.33 2.81 0.030 1.01 -8 2 2 167.95 117.92 2.79 0.083 1.67 -1 0 4 27.93 56.66 2.77 0.057 3.11 9 1 1 33.85 16.11 2.75 0.031 1.58 5 7 8 269.77 348.46 2.74 0.143 1.01 Bond lengths and angles C1 - Distance Angles O1 1.4234 (0.0028) C1 - C2 - Distance Angles O1 1.3738 (0.0027) C7 1.3850 (0.0031) 116.02 (0.21) C3 1.3917 (0.0033) 124.52 (0.21) 119.46 (0.22) C2 - O1 C7 C3 - Distance Angles C2 1.3917 (0.0033) C4 1.3987 (0.0032) 118.76 (0.21) C3 - C2 C4 - Distance Angles C5 1.3780 (0.0030) C3 1.3987 (0.0032) 122.05 (0.21) C4 - C5 C5 - Distance Angles C4 1.3780 (0.0030) C6 1.3833 (0.0031) 118.16 (0.21) C8 1.5247 (0.0030) 120.88 (0.19) 120.89 (0.19) C5 - C4 C6 C6 - Distance Angles C5 1.3833 (0.0031) C7 1.3843 (0.0031) 120.98 (0.21) C6 - C5 C7 - Distance Angles C6 1.3843 (0.0031) C2 1.3850 (0.0031) 120.53 (0.21) C7 - C6 C8 - Distance Angles O2 1.4293 (0.0025) C5 1.5247 (0.0030) 109.94 (0.17) C9 1.5260 (0.0030) 112.76 (0.17) 113.67 (0.17) C8 - O2 C5 C9 - Distance Angles C10 1.3891 (0.0031) C14 1.3980 (0.0030) 118.25 (0.20) C8 1.5260 (0.0030) 122.63 (0.20) 119.09 (0.19) C9 - C10 C14 C10 - Distance Angles C11 1.3836 (0.0033) C9 1.3891 (0.0031) 120.05 (0.21) C10 - C11 C11 - Distance Angles C12 1.3837 (0.0032) C10 1.3836 (0.0033) 121.10 (0.21) C11 - C12 C12 - Distance Angles C11 1.3837 (0.0032) C13 1.3893 (0.0031) 120.36 (0.21) C12 - C11 C13 - Distance Angles C12 1.3893 (0.0031) C14 1.3963 (0.0030) 117.97 (0.20) C16 1.5169 (0.0029) 123.14 (0.20) 118.82 (0.19) C13 - C12 C14 C14 - Distance Angles O3 1.3870 (0.0025) C13 1.3963 (0.0030) 119.03 (0.19) C9 1.3980 (0.0030) 118.59 (0.19) 122.22 (0.19) C14 - O3 C13 C15 - Distance Angles O3 1.4372 (0.0026) C15 - C16 - Distance Angles N1 1.4554 (0.0028) C13 1.5169 (0.0029) 114.88 (0.18) C16 - N1 C17 - Distance Angles O4 1.2359 (0.0026) N1 1.3366 (0.0028) 120.45 (0.20) C18 1.5365 (0.0030) 122.21 (0.19) 117.35 (0.19) C17 - O4 N1 C18 - Distance Angles C20 1.5286 (0.0033) C21 1.5311 (0.0032) 109.50 (0.20) C19 1.5345 (0.0032) 110.18 (0.19) 109.29 (0.21) C17 1.5365 (0.0030) 111.82 (0.19) 108.53 (0.18) 107.45 (0.18) C18 - C20 C21 C19 C19 - Distance Angles C18 1.5345 (0.0032) C19 - C20 - Distance Angles C18 1.5286 (0.0033) C20 - C21 - Distance Angles C18 1.5311 (0.0032) C21 - N1 - Distance Angles C17 1.3366 (0.0028) C16 1.4554 (0.0028) 121.11 (0.19) N1 - C17 O1 - Distance Angles C2 1.3738 (0.0027) C1 1.4234 (0.0028) 117.66 (0.19) O1 - C2 O2 - Distance Angles C8 1.4293 (0.0025) O2 - O3 - Distance Angles C14 1.3870 (0.0025) C15 1.4372 (0.0026) 115.03 (0.16) O3 - C14 O4 - Distance Angles C17 1.2359 (0.0026) O4 - FMAP and GRID set by program FMAP 2 2 15 GRID -2.083 -2 -2 2.083 2 2 R1 = 0.1023 for 4288 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.29 at 0.0068 0.0385 0.2745 [ 0.92 A from C10 ] Deepest hole -0.20 at 0.0962 0.0031 0.6784 [ 0.86 A from C9 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 3057 / 23166 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 1.0068 0.0385 0.2745 1.00000 0.05 0.29 0.92 C10 0.95 C11 1.58 H10 1.60 H11 Q2 1 0.7713 -0.0030 0.4279 1.00000 0.05 0.29 0.52 H8 1.06 C8 1.59 O2 2.21 C5 Q3 1 1.2250 0.2037 0.4774 1.00000 0.05 0.23 1.31 N1 1.43 H1N 1.48 C17 1.76 H19A Q4 1 0.9159 0.1488 0.3638 1.00000 0.05 0.22 0.88 C14 0.93 C9 1.84 O3 2.00 C10 Q5 1 1.2837 0.3484 0.4879 1.00000 0.05 0.21 0.70 C18 0.86 C17 1.80 C20 1.85 N1 Q6 1 0.9628 0.3319 0.4954 1.00000 0.05 0.20 1.28 H15A 1.39 H16A 1.54 C15 1.54 O3 Q7 1 1.3399 0.3480 0.5397 1.00000 0.05 0.20 0.65 C18 0.88 C20 1.51 H20A 1.52 H20C Q8 1 0.7189 0.2154 0.3395 1.00000 0.05 0.20 0.85 C4 0.98 C5 1.54 H4 1.81 C3 Q9 1 0.6349 0.2975 0.2419 1.00000 0.05 0.18 0.70 C3 0.72 C2 1.50 H3 1.76 C4 Q10 1 1.1878 0.1526 0.4116 1.00000 0.05 0.18 0.67 H12 1.49 C12 2.03 N1 2.18 C17 Q11 1 0.8585 0.0660 0.3605 1.00000 0.05 0.18 0.70 C9 0.86 C8 1.50 H8 1.77 C14 Q12 1 1.3414 0.3000 0.4779 1.00000 0.05 0.18 0.46 C18 1.07 C19 1.67 H19A 1.67 H19C Q13 1 0.9021 0.4077 0.5084 1.00000 0.05 0.17 0.87 H15B 1.07 C15 1.17 H15A 1.88 O3 Q14 1 1.0582 0.2271 0.4672 1.00000 0.05 0.17 0.69 C13 0.83 C16 1.47 H16A 1.53 H16B Q15 1 1.2588 0.3844 0.6862 1.00000 0.05 0.17 1.35 H20A 1.53 H20C 1.75 C20 2.23 H1N Q16 1 1.2418 0.3156 0.3235 1.00000 0.05 0.17 1.41 O4 1.49 H2 1.82 C17 2.12 H19C Q17 1 1.0574 0.1833 0.3951 1.00000 0.05 0.16 0.59 C13 1.04 C12 1.67 H12 1.73 C14 Q18 1 1.2618 0.3690 0.3771 1.00000 0.05 0.16 1.05 O4 1.25 C17 1.66 H21A 1.74 C18 Q19 1 0.6151 0.2291 0.4347 1.00000 0.05 0.16 0.99 H4 1.50 C4 1.93 H3 1.96 C3 Q20 1 1.0221 0.3579 0.5331 1.00000 0.05 0.16 0.77 H16A 1.15 C16 1.18 H16B 2.03 H15A Shortest distances between peaks (including symmetry equivalents) 16 18 0.92 7 12 0.93 5 12 0.99 6 20 1.01 14 17 1.02 5 7 1.03 3 10 1.12 6 13 1.20 4 11 1.21 5 18 1.44 14 20 1.70 2 11 1.71 3 5 1.74 6 14 1.82 13 20 1.84 12 18 1.84 8 9 1.92 10 17 1.93 8 19 1.97 3 12 1.97 1 4 2.11 4 17 2.12 5 16 2.17 10 14 2.18 10 16 2.20 3 18 2.22 1 17 2.26 7 15 2.26 3 16 2.29 7 18 2.33 3 7 2.37 12 16 2.40 2 3 2.42 3 14 2.44 6 17 2.46 1 11 2.47 4 14 2.55 10 18 2.56 9 19 2.57 5 15 2.57 8 11 2.58 17 20 2.59 4 6 2.62 2 10 2.62 3 17 2.64 2 8 2.65 5 10 2.65 15 16 2.74 13 20 2.75 2 4 2.78 10 12 2.83 4 8 2.96 Time profile in seconds ----------------------- 0.02: 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 0.01: Analyse other restraints etc. 1.09: Read intensity data, sort/merge etc. 0.01: Set up constraints 0.00: OSF, H-atoms from difference map 0.01: Set up l.s. refinement 0.00: Generate idealized H-atoms 1.70: Structure factors and derivatives 2.42: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.01: Apply other restraints 0.23: Solve l.s. equations 0.00: Generate HTAB table 0.03: Other dependent quantities, CIF, tables 0.13: Analysis of variance 0.05: Merge reflections for Fourier and .fcf 0.04: Fourier summations 0.04: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2005src0502 finished at 22:44:48 Total CPU time: 5.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++