+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008src0988 started at 16:52:14 on 19-Sep-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src0988 in P-1 CELL 0.71073 5.4658 12.1791 15.8842 106.312 99.182 102.509 ZERR 2.00 0.0002 0.0004 0.0005 0.002 0.002 0.002 LATT 1 SFAC C H N O UNIT 46 52 4 4 V = 962.93 F(000) = 388.0 Mu = 0.08 mm-1 Cell Wt = 724.92 Rho = 1.250 MERG 2 OMIT -3.00 55.00 EXTI 0.03408 SHEL 7 0.77 FMAP 2 PLAN 10 SIZE 0.08 0.11 0.43 ACTA BOND $H WGHT 0.05410 0.15860 L.S. 4 TEMP -153.00 FVAR 1.01972 C1 1 0.150680 -0.075012 0.105619 11.00000 0.01362 0.02095 = 0.02098 0.00671 0.00243 0.00459 C2 1 0.226000 -0.081624 0.024381 11.00000 0.01791 0.02323 = 0.02227 0.01096 0.00490 0.00416 AFIX 43 H2 2 0.264648 -0.011726 0.007918 11.00000 -1.20000 AFIX 0 C3 1 0.245590 -0.186707 -0.032315 11.00000 0.02059 0.02762 = 0.02039 0.00703 0.00693 0.00468 AFIX 43 H3 2 0.294323 -0.189547 -0.087518 11.00000 -1.20000 AFIX 0 C4 1 0.192923 -0.288145 -0.007353 11.00000 0.02116 0.02141 = 0.02552 0.00450 0.00649 0.00488 AFIX 43 H4 2 0.211109 -0.360541 -0.044727 11.00000 -1.20000 AFIX 0 C5 1 0.114018 -0.284417 0.071724 11.00000 0.01986 0.01973 = 0.02615 0.00749 0.00581 0.00477 AFIX 43 H5 2 0.075676 -0.354984 0.087346 11.00000 -1.20000 AFIX 0 C6 1 0.089554 -0.178807 0.129152 11.00000 0.01346 0.02010 = 0.01974 0.00708 0.00287 0.00331 C8 1 -0.150776 -0.120008 0.246456 11.00000 0.02010 0.01728 = 0.02358 0.00478 0.00597 0.00122 C9 1 -0.225528 -0.034241 0.201289 11.00000 0.01789 0.02112 = 0.02433 0.00562 0.00581 0.00492 AFIX 23 H9A 2 -0.301260 -0.077316 0.136202 11.00000 -1.20000 H9B 2 -0.358601 -0.002770 0.227725 11.00000 -1.20000 AFIX 0 C11 1 0.179104 0.048416 0.166428 11.00000 0.01715 0.01960 = 0.02051 0.00972 0.00234 0.00484 C12 1 0.066392 -0.271491 0.250371 11.00000 0.02097 0.02295 = 0.02367 0.01196 0.00372 0.00620 AFIX 23 H12A 2 0.098706 -0.238093 0.316861 11.00000 -1.20000 H12B 2 0.225175 -0.290317 0.235774 11.00000 -1.20000 AFIX 0 C13 1 -0.151252 -0.385806 0.217317 11.00000 0.02273 0.02047 = 0.02211 0.00902 0.00974 0.00900 C14 1 -0.372591 -0.404287 0.152248 11.00000 0.02386 0.02097 = 0.02947 0.01290 0.00650 0.00700 AFIX 43 H14 2 -0.388966 -0.344220 0.126120 11.00000 -1.20000 AFIX 0 C15 1 -0.569589 -0.509066 0.124980 11.00000 0.02294 0.02506 = 0.03440 0.01158 0.00456 0.00467 AFIX 43 H15 2 -0.718221 -0.520415 0.079868 11.00000 -1.20000 AFIX 0 C16 1 -0.551951 -0.597166 0.162752 11.00000 0.02646 0.01937 = 0.03452 0.00813 0.01336 0.00506 AFIX 43 H16 2 -0.688584 -0.668324 0.144612 11.00000 -1.20000 AFIX 0 C17 1 -0.332666 -0.580420 0.227357 11.00000 0.03937 0.01902 = 0.02874 0.01089 0.01282 0.01024 AFIX 43 H17 2 -0.318749 -0.640454 0.253764 11.00000 -1.20000 AFIX 0 C18 1 -0.133089 -0.476579 0.253808 11.00000 0.02906 0.02351 = 0.02239 0.00964 0.00635 0.01041 AFIX 43 H18 2 0.017921 -0.466966 0.297273 11.00000 -1.20000 AFIX 0 C19 1 0.012951 0.182246 0.273771 11.00000 0.02518 0.01744 = 0.02532 0.00557 0.00662 0.00829 AFIX 23 H19A 2 -0.157279 0.198221 0.262634 11.00000 -1.20000 H19B 2 0.137583 0.242861 0.259836 11.00000 -1.20000 AFIX 0 C20 1 0.096344 0.196938 0.373711 11.00000 0.02259 0.02404 = 0.02271 0.00639 0.00565 0.00583 AFIX 13 H20 2 -0.043006 0.143949 0.389587 11.00000 -1.20000 AFIX 0 C21 1 0.347158 0.164170 0.397193 11.00000 0.02833 0.03478 = 0.02754 0.00989 0.00425 0.00919 AFIX 23 H21A 2 0.484869 0.212265 0.378271 11.00000 -1.20000 H21B 2 0.323019 0.079192 0.363790 11.00000 -1.20000 AFIX 0 C22 1 0.429412 0.186300 0.498781 11.00000 0.03675 0.05546 = 0.02906 0.01351 0.00201 0.01631 AFIX 23 H22A 2 0.299295 0.132546 0.516543 11.00000 -1.20000 H22B 2 0.595909 0.167718 0.512404 11.00000 -1.20000 AFIX 0 C23 1 0.457487 0.314762 0.553396 11.00000 0.03618 0.05592 = 0.02650 0.00521 0.00035 0.00539 AFIX 23 H23A 2 0.601414 0.367995 0.540880 11.00000 -1.20000 H23B 2 0.499664 0.324756 0.618555 11.00000 -1.20000 AFIX 0 C24 1 0.210175 0.349989 0.530243 11.00000 0.03894 0.04439 = 0.02783 -0.00048 0.00736 0.00614 AFIX 23 H24A 2 0.239127 0.435663 0.562741 11.00000 -1.20000 H24B 2 0.071941 0.304378 0.550549 11.00000 -1.20000 AFIX 0 C25 1 0.124451 0.325940 0.428911 11.00000 0.02972 0.03009 = 0.02854 0.00187 0.00614 0.00760 AFIX 23 H25A 2 0.252274 0.379712 0.410341 11.00000 -1.20000 H25B 2 -0.042904 0.343955 0.415789 11.00000 -1.20000 AFIX 0 N7 3 0.014266 -0.180801 0.210983 11.00000 0.01906 0.01784 = 0.02025 0.00836 0.00555 0.00425 N10 3 -0.005338 0.064617 0.211867 11.00000 0.01761 0.01881 = 0.02291 0.00593 0.00494 0.00573 O1 4 0.367147 0.130305 0.172410 11.00000 0.02337 0.01949 = 0.03096 0.00958 0.00681 0.00305 O2 4 -0.232522 -0.134466 0.310843 11.00000 0.03806 0.03310 = 0.03355 0.01444 0.01938 0.01128 HKLF 4 Covalent radii and connectivity table for 2008src0988 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 C1 - C2 C6 C11 C2 - C3 C1 C3 - C2 C4 C4 - C5 C3 C5 - C4 C6 C6 - C5 C1 N7 C8 - O2 N7 C9 C9 - N10 C8 C11 - O1 N10 C1 C12 - N7 C13 C13 - C14 C18 C12 C14 - C15 C13 C15 - C16 C14 C16 - C15 C17 C17 - C16 C18 C18 - C17 C13 C19 - N10 C20 C20 - C19 C21 C25 C21 - C20 C22 C22 - C23 C21 C23 - C22 C24 C24 - C23 C25 C25 - C24 C20 N7 - C8 C6 C12 N10 - C11 C9 C19 O1 - C11 O2 - C8 19667 Reflections read, of which 25 rejected -7 =< h =< 7, -15 =< k =< 15, -19 =< l =< 20, Max. 2-theta = 54.96 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 4 5 8 -10.46 6.55 2 42.19 2 -2 10 12.89 0.77 5 4.40 2 -13 15 5.31 3.33 3 19.03 1 -6 18 -3.82 1.65 3 14.13 1 -4 19 -16.03 6.29 2 51.73 5 Inconsistent equivalents 4394 Unique reflections, of which 0 suppressed R(int) = 0.0733 R(sigma) = 0.0689 Friedel opposites merged Maximum memory for data reduction = 2632 / 44035 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 = 3357 / 304010 wR2 = 0.1299 before cycle 1 for 4394 data and 245 / 245 parameters GooF = S = 1.053; Restrained GooF = 1.053 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0541 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.01971 0.00241 -0.003 OSF 2 0.03408 0.00412 0.000 EXTI Mean shift/su = 0.002 Maximum = -0.007 for U12 O1 Max. shift = 0.000 A for C12 Max. dU = 0.000 for C18 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3357 / 304010 wR2 = 0.1299 before cycle 2 for 4394 data and 245 / 245 parameters GooF = S = 1.053; Restrained GooF = 1.053 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0541 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.01971 0.00241 0.000 OSF 2 0.03408 0.00412 0.000 EXTI Mean shift/su = 0.001 Maximum = -0.002 for U12 O1 Max. shift = 0.000 A for H22B Max. dU = 0.000 for C18 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3357 / 304010 wR2 = 0.1299 before cycle 3 for 4394 data and 245 / 245 parameters GooF = S = 1.053; Restrained GooF = 1.053 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0541 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.01972 0.00241 0.000 OSF 2 0.03408 0.00412 0.001 EXTI Mean shift/su = 0.000 Maximum = 0.001 for EXTI Max. shift = 0.000 A for C17 Max. dU = 0.000 for C8 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3357 / 304010 wR2 = 0.1299 before cycle 4 for 4394 data and 245 / 245 parameters GooF = S = 1.053; Restrained GooF = 1.053 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0541 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 1.01971 0.00241 -0.001 OSF 2 0.03408 0.00412 0.000 EXTI Mean shift/su = 0.000 Maximum = -0.001 for OSF Max. shift = 0.000 A for C21 Max. dU = 0.000 for O2 Largest correlation matrix elements 0.535 EXTI / OSF Idealized hydrogen atom generation before cycle 5 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.2646 -0.0117 0.0079 43 0.950 0.000 C2 C3 C1 H3 0.2943 -0.1895 -0.0875 43 0.950 0.000 C3 C2 C4 H4 0.2111 -0.3605 -0.0447 43 0.950 0.000 C4 C5 C3 H5 0.0757 -0.3550 0.0873 43 0.950 0.000 C5 C4 C6 H9A -0.3013 -0.0773 0.1362 23 0.990 0.000 C9 N10 C8 H9B -0.3586 -0.0028 0.2277 23 0.990 0.000 C9 N10 C8 H12A 0.0987 -0.2381 0.3169 23 0.990 0.000 C12 N7 C13 H12B 0.2252 -0.2903 0.2358 23 0.990 0.000 C12 N7 C13 H14 -0.3890 -0.3442 0.1261 43 0.950 0.000 C14 C15 C13 H15 -0.7182 -0.5204 0.0799 43 0.950 0.000 C15 C16 C14 H16 -0.6886 -0.6683 0.1446 43 0.950 0.000 C16 C15 C17 H17 -0.3187 -0.6405 0.2538 43 0.950 0.000 C17 C16 C18 H18 0.0179 -0.4670 0.2973 43 0.950 0.000 C18 C17 C13 H19A -0.1573 0.1982 0.2626 23 0.990 0.000 C19 N10 C20 H19B 0.1376 0.2429 0.2598 23 0.990 0.000 C19 N10 C20 H20 -0.0430 0.1439 0.3896 13 1.000 0.000 C20 C19 C21 C25 H21A 0.4849 0.2123 0.3783 23 0.990 0.000 C21 C20 C22 H21B 0.3230 0.0792 0.3638 23 0.990 0.000 C21 C20 C22 H22A 0.2993 0.1325 0.5165 23 0.990 0.000 C22 C23 C21 H22B 0.5959 0.1677 0.5124 23 0.990 0.000 C22 C23 C21 H23A 0.6014 0.3680 0.5409 23 0.990 0.000 C23 C22 C24 H23B 0.4997 0.3248 0.6186 23 0.990 0.000 C23 C22 C24 H24A 0.2391 0.4357 0.5627 23 0.990 0.000 C24 C23 C25 H24B 0.0719 0.3044 0.5505 23 0.990 0.000 C24 C23 C25 H25A 0.2523 0.3797 0.4103 23 0.990 0.000 C25 C24 C20 H25B -0.0429 0.3440 0.4158 23 0.990 0.000 C25 C24 C20 2008src0988 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.15068 -0.07501 0.10562 1.00000 0.01362 0.02095 0.02098 0.00671 0.00243 0.00459 0.01877 0.00355 0.00029 0.00014 0.00011 0.00000 0.00077 0.00089 0.00081 0.00067 0.00063 0.00065 0.00036 C2 0.22600 -0.08162 0.02438 1.00000 0.01791 0.02323 0.02227 0.01096 0.00490 0.00416 0.02060 0.00368 0.00030 0.00015 0.00011 0.00000 0.00081 0.00093 0.00084 0.00070 0.00066 0.00068 0.00037 H2 0.26465 -0.01173 0.00792 1.00000 0.02472 0.00000 0.00000 C3 0.24559 -0.18671 -0.03232 1.00000 0.02059 0.02762 0.02039 0.00703 0.00693 0.00468 0.02312 0.00375 0.00031 0.00015 0.00011 0.00000 0.00085 0.00099 0.00084 0.00072 0.00068 0.00073 0.00039 H3 0.29432 -0.18955 -0.08752 1.00000 0.02774 0.00000 0.00000 C4 0.19292 -0.28814 -0.00735 1.00000 0.02116 0.02141 0.02552 0.00450 0.00649 0.00488 0.02343 0.00381 0.00032 0.00015 0.00011 0.00000 0.00087 0.00094 0.00088 0.00071 0.00070 0.00071 0.00039 H4 0.21111 -0.36054 -0.04473 1.00000 0.02812 0.00000 0.00000 C5 0.11402 -0.28442 0.07172 1.00000 0.01986 0.01973 0.02615 0.00749 0.00581 0.00477 0.02198 0.00367 0.00031 0.00015 0.00011 0.00000 0.00084 0.00092 0.00087 0.00072 0.00069 0.00070 0.00038 H5 0.07568 -0.35498 0.08735 1.00000 0.02638 0.00000 0.00000 C6 0.08955 -0.17881 0.12915 1.00000 0.01346 0.02010 0.01974 0.00708 0.00287 0.00331 0.01799 0.00350 0.00029 0.00014 0.00010 0.00000 0.00076 0.00088 0.00080 0.00067 0.00062 0.00065 0.00036 C8 -0.15078 -0.12001 0.24646 1.00000 0.02010 0.01728 0.02358 0.00478 0.00597 0.00122 0.02129 0.00363 0.00031 0.00014 0.00011 0.00000 0.00084 0.00088 0.00087 0.00068 0.00068 0.00068 0.00038 C9 -0.22553 -0.03424 0.20129 1.00000 0.01789 0.02112 0.02433 0.00562 0.00581 0.00492 0.02148 0.00371 0.00031 0.00015 0.00011 0.00000 0.00082 0.00091 0.00086 0.00069 0.00066 0.00069 0.00037 H9A -0.30126 -0.07732 0.13620 1.00000 0.02578 0.00000 0.00000 H9B -0.35860 -0.00277 0.22772 1.00000 0.02578 0.00000 0.00000 C11 0.17910 0.04842 0.16643 1.00000 0.01715 0.01960 0.02051 0.00972 0.00234 0.00484 0.01869 0.00361 0.00030 0.00014 0.00011 0.00000 0.00081 0.00089 0.00081 0.00067 0.00064 0.00068 0.00036 C12 0.06639 -0.27149 0.25037 1.00000 0.02097 0.02295 0.02367 0.01196 0.00372 0.00620 0.02175 0.00375 0.00032 0.00015 0.00011 0.00000 0.00086 0.00093 0.00085 0.00071 0.00068 0.00071 0.00038 H12A 0.09871 -0.23809 0.31686 1.00000 0.02610 0.00000 0.00000 H12B 0.22518 -0.29032 0.23577 1.00000 0.02610 0.00000 0.00000 C13 -0.15125 -0.38581 0.21732 1.00000 0.02273 0.02047 0.02211 0.00902 0.00974 0.00900 0.02028 0.00378 0.00031 0.00015 0.00011 0.00000 0.00087 0.00090 0.00083 0.00068 0.00068 0.00070 0.00037 C14 -0.37259 -0.40429 0.15225 1.00000 0.02386 0.02097 0.02947 0.01290 0.00650 0.00700 0.02359 0.00385 0.00032 0.00015 0.00012 0.00000 0.00089 0.00093 0.00092 0.00073 0.00072 0.00073 0.00039 H14 -0.38897 -0.34422 0.12612 1.00000 0.02831 0.00000 0.00000 C15 -0.56959 -0.50907 0.12498 1.00000 0.02294 0.02506 0.03440 0.01158 0.00456 0.00467 0.02765 0.00406 0.00034 0.00016 0.00012 0.00000 0.00090 0.00100 0.00100 0.00080 0.00076 0.00075 0.00042 H15 -0.71822 -0.52042 0.07987 1.00000 0.03318 0.00000 0.00000 C16 -0.55195 -0.59717 0.16275 1.00000 0.02646 0.01937 0.03452 0.00813 0.01336 0.00506 0.02640 0.00413 0.00034 0.00016 0.00012 0.00000 0.00093 0.00094 0.00099 0.00076 0.00078 0.00073 0.00041 H16 -0.68858 -0.66832 0.14461 1.00000 0.03168 0.00000 0.00000 C17 -0.33267 -0.58042 0.22736 1.00000 0.03937 0.01902 0.02874 0.01089 0.01282 0.01024 0.02744 0.00409 0.00036 0.00016 0.00012 0.00000 0.00108 0.00095 0.00095 0.00074 0.00082 0.00081 0.00042 H17 -0.31875 -0.64045 0.25376 1.00000 0.03292 0.00000 0.00000 C18 -0.13309 -0.47658 0.25381 1.00000 0.02906 0.02351 0.02239 0.00964 0.00635 0.01041 0.02397 0.00399 0.00034 0.00015 0.00011 0.00000 0.00094 0.00096 0.00085 0.00071 0.00072 0.00075 0.00039 H18 0.01792 -0.46697 0.29727 1.00000 0.02877 0.00000 0.00000 C19 0.01295 0.18225 0.27377 1.00000 0.02518 0.01744 0.02532 0.00557 0.00662 0.00829 0.02247 0.00374 0.00033 0.00015 0.00011 0.00000 0.00090 0.00088 0.00088 0.00069 0.00071 0.00071 0.00038 H19A -0.15728 0.19822 0.26263 1.00000 0.02697 0.00000 0.00000 H19B 0.13758 0.24286 0.25984 1.00000 0.02697 0.00000 0.00000 C20 0.09634 0.19694 0.37371 1.00000 0.02259 0.02404 0.02271 0.00639 0.00565 0.00583 0.02345 0.00380 0.00033 0.00015 0.00011 0.00000 0.00088 0.00095 0.00086 0.00071 0.00069 0.00072 0.00039 H20 -0.04301 0.14395 0.38959 1.00000 0.02814 0.00000 0.00000 C21 0.34716 0.16417 0.39719 1.00000 0.02833 0.03478 0.02754 0.00989 0.00425 0.00919 0.03048 0.00420 0.00035 0.00018 0.00012 0.00000 0.00099 0.00111 0.00096 0.00082 0.00078 0.00084 0.00044 H21A 0.48487 0.21226 0.37827 1.00000 0.03658 0.00000 0.00000 H21B 0.32302 0.07919 0.36379 1.00000 0.03658 0.00000 0.00000 C22 0.42941 0.18630 0.49878 1.00000 0.03675 0.05546 0.02906 0.01351 0.00201 0.01631 0.04059 0.00468 0.00041 0.00020 0.00013 0.00000 0.00116 0.00143 0.00104 0.00097 0.00087 0.00102 0.00053 H22A 0.29930 0.13255 0.51654 1.00000 0.04871 0.00000 0.00000 H22B 0.59591 0.16772 0.51240 1.00000 0.04871 0.00000 0.00000 C23 0.45749 0.31476 0.55340 1.00000 0.03618 0.05592 0.02650 0.00521 0.00035 0.00539 0.04339 0.00460 0.00041 0.00021 0.00014 0.00000 0.00116 0.00146 0.00100 0.00096 0.00086 0.00103 0.00056 H23A 0.60141 0.36799 0.54088 1.00000 0.05206 0.00000 0.00000 H23B 0.49966 0.32476 0.61855 1.00000 0.05206 0.00000 0.00000 C24 0.21018 0.34999 0.53024 1.00000 0.03894 0.04439 0.02783 -0.00048 0.00736 0.00614 0.04067 0.00447 0.00040 0.00020 0.00013 0.00000 0.00119 0.00130 0.00103 0.00090 0.00087 0.00098 0.00052 H24A 0.23913 0.43566 0.56274 1.00000 0.04880 0.00000 0.00000 H24B 0.07194 0.30438 0.55055 1.00000 0.04880 0.00000 0.00000 C25 0.12445 0.32594 0.42891 1.00000 0.02972 0.03009 0.02854 0.00187 0.00614 0.00760 0.03132 0.00409 0.00037 0.00017 0.00012 0.00000 0.00100 0.00107 0.00097 0.00080 0.00078 0.00082 0.00044 H25A 0.25227 0.37971 0.41034 1.00000 0.03759 0.00000 0.00000 H25B -0.04290 0.34396 0.41579 1.00000 0.03759 0.00000 0.00000 N7 0.01427 -0.18080 0.21098 1.00000 0.01906 0.01784 0.02025 0.00836 0.00555 0.00425 0.01862 0.00297 0.00025 0.00012 0.00009 0.00000 0.00070 0.00073 0.00070 0.00056 0.00055 0.00056 0.00031 N10 -0.00534 0.06462 0.21187 1.00000 0.01761 0.01881 0.02291 0.00593 0.00494 0.00573 0.01983 0.00300 0.00025 0.00012 0.00009 0.00000 0.00069 0.00076 0.00072 0.00058 0.00056 0.00057 0.00032 O1 0.36715 0.13031 0.17241 1.00000 0.02337 0.01949 0.03096 0.00958 0.00681 0.00305 0.02474 0.00259 0.00022 0.00010 0.00008 0.00000 0.00064 0.00066 0.00066 0.00052 0.00051 0.00052 0.00030 O2 -0.23252 -0.13447 0.31084 1.00000 0.03806 0.03310 0.03355 0.01444 0.01938 0.01128 0.03258 0.00300 0.00025 0.00011 0.00008 0.00000 0.00077 0.00079 0.00073 0.00061 0.00060 0.00060 0.00033 Final Structure Factor Calculation for 2008src0988 in P-1 Total number of l.s. parameters = 245 Maximum vector length = 511 Memory required = 3112 / 22995 wR2 = 0.1299 before cycle 5 for 4394 data and 0 / 245 parameters GooF = S = 1.053; Restrained GooF = 1.053 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0541 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0505 for 2915 Fo > 4sig(Fo) and 0.0896 for all 4394 data wR2 = 0.1299, GooF = S = 1.053, Restrained GooF = 1.053 for all data Occupancy sum of asymmetric unit = 27.00 for non-hydrogen and 26.00 for hydrogen atoms Principal mean square atomic displacements U 0.0219 0.0211 0.0134 C1 0.0264 0.0190 0.0165 C2 0.0297 0.0220 0.0176 C3 0.0292 0.0206 0.0205 C4 0.0263 0.0207 0.0189 C5 0.0215 0.0191 0.0134 C6 0.0270 0.0216 0.0152 C8 0.0262 0.0208 0.0175 C9 0.0240 0.0177 0.0144 C11 0.0276 0.0213 0.0163 C12 0.0264 0.0181 0.0164 C13 0.0305 0.0237 0.0165 C14 0.0358 0.0252 0.0220 C15 0.0386 0.0221 0.0186 C16 0.0404 0.0255 0.0164 C17 0.0299 0.0231 0.0189 C18 0.0264 0.0253 0.0157 C19 0.0257 0.0225 0.0221 C20 0.0351 0.0309 0.0254 C21 0.0569 0.0401 0.0248 C22 0.0642 0.0420 0.0239 C23 0.0589 0.0389 0.0242 C24 0.0408 0.0299 0.0233 C25 0.0210 0.0198 0.0151 N7 0.0236 0.0190 0.0169 N10 0.0310 0.0260 0.0172 O1 0.0450 0.0322 0.0206 O2 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 0.038 0.050 0.063 0.081 0.108 0.160 1.000 Number in group 450. 476. 393. 448. 461. 412. 445. 439. 428. 442. GooF 0.818 0.852 0.947 1.129 1.157 1.188 1.232 1.088 1.065 0.979 K 0.793 0.991 1.003 0.914 0.950 0.977 0.979 1.016 1.024 1.017 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.66 inf Number in group 449. 437. 448. 430. 435. 437. 438. 444. 433. 443. GooF 0.983 0.971 1.039 1.111 1.053 1.105 1.080 0.982 1.044 1.150 K 1.045 1.037 0.987 1.011 1.001 1.007 1.026 1.029 1.024 1.005 R1 0.231 0.211 0.187 0.154 0.109 0.081 0.057 0.050 0.043 0.031 Recommended weighting scheme: WGHT 0.0541 0.1585 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) -3 -3 18 35.34 67.98 4.21 0.079 0.84 6 -5 3 75.32 130.79 4.14 0.110 0.86 -1 9 6 43.27 66.32 3.98 0.078 1.04 -4 2 14 2.43 20.88 3.95 0.044 0.91 -6 4 5 119.88 81.68 3.76 0.087 0.90 -2 9 6 29.63 51.52 3.35 0.069 1.04 3 -7 14 475.80 344.15 3.33 0.179 0.88 4 7 4 332.60 245.68 3.23 0.151 0.81 0 -1 4 62.02 46.78 3.19 0.066 3.92 -1 0 2 932.41 1134.79 3.17 0.324 4.81 1 2 6 6.58 1.06 3.16 0.010 1.73 0 -10 16 7.52 20.01 3.15 0.043 0.87 4 1 10 17.10 41.26 3.14 0.062 0.85 1 -7 3 50.23 36.60 3.13 0.058 1.73 -1 -5 3 38.97 27.44 3.12 0.050 2.02 6 -6 6 6.99 39.80 3.12 0.061 0.81 4 -12 3 19.13 35.14 3.11 0.057 0.89 0 -15 4 10.13 35.90 3.09 0.058 0.79 -3 13 4 10.01 31.23 3.07 0.054 0.81 1 -9 11 8.21 16.03 3.06 0.039 1.10 0 -15 9 1.81 20.64 3.05 0.044 0.79 1 -1 13 44.61 59.87 3.00 0.074 1.10 -6 11 1 35.80 70.81 2.98 0.081 0.77 2 -6 9 22.79 41.16 2.96 0.062 1.31 -1 -6 4 265.18 217.36 2.96 0.142 1.73 -1 -1 16 28.95 45.14 2.94 0.065 0.97 -1 0 19 367.45 269.98 2.94 0.158 0.80 1 -10 18 72.49 43.14 2.93 0.063 0.79 5 -1 8 -1.05 17.72 2.92 0.041 0.85 3 -13 5 0.10 13.49 2.92 0.035 0.89 -3 -2 12 4.56 11.25 2.90 0.032 1.14 2 -2 10 12.40 26.55 2.90 0.050 1.25 -4 -8 14 18.50 38.85 2.89 0.060 0.81 -1 -1 2 460.02 551.30 2.89 0.226 4.36 -1 -2 8 10.37 3.90 2.89 0.019 1.93 1 2 7 128.18 103.36 2.89 0.098 1.56 -1 -12 6 12.83 3.80 2.86 0.019 0.94 6 -7 2 27.34 48.53 2.85 0.067 0.86 3 -8 13 26.59 68.61 2.85 0.080 0.91 1 -11 9 37.67 51.61 2.84 0.069 1.04 -2 -4 8 41.83 29.31 2.82 0.052 1.54 0 -11 11 44.24 61.64 2.80 0.076 0.98 0 -2 17 35.25 52.24 2.79 0.070 0.91 -1 -5 11 26.93 38.47 2.79 0.060 1.35 -2 -8 1 81.01 103.72 2.78 0.098 1.14 -3 -6 7 63.51 46.02 2.78 0.065 1.18 3 -13 13 21.08 36.24 2.78 0.058 0.78 4 -7 2 132.21 105.86 2.77 0.099 1.17 -4 3 13 5.59 12.85 2.76 0.034 0.93 -2 7 7 151.75 190.12 2.76 0.133 1.17 Bond lengths and angles C1 - Distance Angles C2 1.4024 (0.0023) C6 1.4042 (0.0023) 118.99 (0.15) C11 1.5007 (0.0023) 115.31 (0.14) 125.13 (0.15) C1 - C2 C6 C2 - Distance Angles C3 1.3795 (0.0024) C1 1.4024 (0.0023) 121.90 (0.15) H2 0.9500 119.05 119.05 C2 - C3 C1 C3 - Distance Angles C2 1.3795 (0.0024) C4 1.3870 (0.0024) 118.87 (0.15) H3 0.9500 120.56 120.56 C3 - C2 C4 C4 - Distance Angles C5 1.3839 (0.0024) C3 1.3870 (0.0024) 120.33 (0.16) H4 0.9500 119.84 119.84 C4 - C5 C3 C5 - Distance Angles C4 1.3839 (0.0024) C6 1.3995 (0.0023) 121.34 (0.15) H5 0.9500 119.33 119.33 C5 - C4 C6 C6 - Distance Angles C5 1.3995 (0.0023) C1 1.4042 (0.0023) 118.52 (0.15) N7 1.4295 (0.0020) 118.27 (0.14) 123.15 (0.15) C6 - C5 C1 C8 - Distance Angles O2 1.2205 (0.0020) N7 1.3772 (0.0022) 121.92 (0.15) C9 1.5116 (0.0023) 121.71 (0.16) 116.37 (0.14) C8 - O2 N7 C9 - Distance Angles N10 1.4562 (0.0021) C8 1.5116 (0.0023) 111.92 (0.13) H9A 0.9900 109.23 109.23 H9B 0.9900 109.23 109.23 107.92 C9 - N10 C8 H9A C11 - Distance Angles O1 1.2376 (0.0019) N10 1.3471 (0.0021) 122.98 (0.15) C1 1.5007 (0.0023) 119.37 (0.15) 117.64 (0.14) C11 - O1 N10 C12 - Distance Angles N7 1.4698 (0.0020) C13 1.5172 (0.0023) 113.69 (0.13) H12A 0.9900 108.82 108.82 H12B 0.9900 108.82 108.82 107.69 C12 - N7 C13 H12A C13 - Distance Angles C14 1.3910 (0.0023) C18 1.3990 (0.0022) 117.92 (0.15) C12 1.5172 (0.0023) 122.62 (0.14) 119.46 (0.14) C13 - C14 C18 C14 - Distance Angles C15 1.3860 (0.0024) C13 1.3910 (0.0023) 120.96 (0.16) H14 0.9500 119.52 119.52 C14 - C15 C13 C15 - Distance Angles C16 1.3815 (0.0024) C14 1.3860 (0.0024) 120.65 (0.16) H15 0.9500 119.67 119.67 C15 - C16 C14 C16 - Distance Angles C15 1.3815 (0.0024) C17 1.3839 (0.0026) 119.14 (0.16) H16 0.9500 120.43 120.43 C16 - C15 C17 C17 - Distance Angles C16 1.3839 (0.0026) C18 1.3869 (0.0024) 120.44 (0.16) H17 0.9500 119.78 119.78 C17 - C16 C18 C18 - Distance Angles C17 1.3869 (0.0024) C13 1.3990 (0.0022) 120.86 (0.16) H18 0.9500 119.57 119.57 C18 - C17 C13 C19 - Distance Angles N10 1.4644 (0.0021) C20 1.5278 (0.0022) 114.63 (0.13) H19A 0.9900 108.61 108.61 H19B 0.9900 108.61 108.61 107.57 C19 - N10 C20 H19A C20 - Distance Angles C19 1.5278 (0.0022) C21 1.5281 (0.0025) 113.12 (0.15) C25 1.5295 (0.0025) 108.33 (0.14) 110.27 (0.14) H20 1.0000 108.33 108.34 108.34 C20 - C19 C21 C25 C21 - Distance Angles C20 1.5281 (0.0025) C22 1.5331 (0.0025) 111.07 (0.16) H21A 0.9900 109.42 109.42 H21B 0.9900 109.42 109.42 108.03 C21 - C20 C22 H21A C22 - Distance Angles C23 1.5215 (0.0031) C21 1.5331 (0.0025) 111.44 (0.17) H22A 0.9900 109.34 109.34 H22B 0.9900 109.34 109.34 107.98 C22 - C23 C21 H22A C23 - Distance Angles C22 1.5215 (0.0031) C24 1.5257 (0.0030) 111.26 (0.16) H23A 0.9900 109.38 109.38 H23B 0.9900 109.38 109.38 108.00 C23 - C22 C24 H23A C24 - Distance Angles C23 1.5257 (0.0030) C25 1.5268 (0.0026) 111.31 (0.17) H24A 0.9900 109.37 109.37 H24B 0.9900 109.37 109.37 108.00 C24 - C23 C25 H24A C25 - Distance Angles C24 1.5268 (0.0026) C20 1.5295 (0.0025) 112.32 (0.16) H25A 0.9900 109.14 109.14 H25B 0.9900 109.14 109.14 107.86 C25 - C24 C20 H25A N7 - Distance Angles C8 1.3772 (0.0022) C6 1.4295 (0.0020) 124.13 (0.13) C12 1.4698 (0.0020) 115.60 (0.13) 118.90 (0.14) N7 - C8 C6 N10 - Distance Angles C11 1.3471 (0.0021) C9 1.4562 (0.0021) 120.92 (0.14) C19 1.4644 (0.0021) 120.52 (0.14) 118.55 (0.14) N10 - C11 C9 O1 - Distance Angles C11 1.2376 (0.0019) O1 - O2 - Distance Angles C8 1.2205 (0.0020) O2 - FMAP and GRID set by program FMAP 2 1 28 GRID -4.000 -2 -1 4.000 2 1 R1 = 0.0896 for 4394 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.22 at 0.8788 0.0784 0.3505 [ 0.83 A from H20 ] Deepest hole -0.26 at 0.9662 0.1763 0.2312 [ 0.66 A from C19 ] Mean = 0.00, Rms deviation from mean = 0.05 e/A^3, Highest memory used = 3302 / 36026 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.1212 0.0784 0.3505 1.00000 0.05 0.22 0.83 H20 1.57 C20 2.00 H9B 2.09 C19 Q2 1 -0.4159 -0.6165 0.1599 1.00000 0.05 0.22 0.83 C16 1.02 C17 1.44 H16 1.63 H17 Q3 1 -0.0408 -0.3811 0.1460 1.00000 0.05 0.21 1.28 H5 1.37 C13 1.73 C12 1.77 H12B Q4 1 0.2492 -0.2554 0.0457 1.00000 0.05 0.21 0.80 C4 0.95 C5 1.58 H4 1.68 C3 Q5 1 0.1621 -0.1176 0.1189 1.00000 0.05 0.20 0.62 C1 0.84 C6 1.74 C2 1.90 C5 Q6 1 0.0938 0.2158 0.3386 1.00000 0.05 0.20 0.66 C20 0.98 C19 1.42 H19B 1.51 H20 Q7 1 0.0355 0.3996 0.3694 1.00000 0.05 0.20 1.20 H25B 1.36 H25A 1.57 C25 2.25 H18 Q8 1 0.2929 -0.0789 0.1901 1.00000 0.05 0.19 1.44 C6 1.46 C1 1.85 H9B 1.88 N7 Q9 1 0.0777 -0.2944 0.0203 1.00000 0.05 0.19 0.78 C5 0.83 C4 1.46 H5 1.51 H4 Q10 1 0.1492 -0.2521 -0.0312 1.00000 0.05 0.19 0.71 C4 0.86 C3 1.40 H4 1.53 H3 Shortest distances between peaks (including symmetry equivalents) 4 9 0.92 5 8 1.14 9 10 1.16 4 10 1.27 1 6 1.90 4 5 1.95 5 9 2.18 6 7 2.26 5 10 2.46 4 8 2.60 3 9 2.61 3 4 2.92 2 10 3.00 Time profile in seconds ----------------------- 0.03: Read and process instructions 0.00: Fit rigid groups 0.02: 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. 0.91: 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 0.88: Structure factors and derivatives 1.69: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.02: Apply other restraints 0.17: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.06: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.09: Fourier summations 0.00: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008src0988 finished at 16:52:18 Total CPU time: 3.9 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++