+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src0258 started at 17:53:17 on 28-Feb-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007src0258 in P4(3) CELL 0.71073 11.5009 11.5009 16.7834 90.000 90.000 90.000 ZERR 4.00 0.0001 0.0001 0.0001 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, 1/2 + Z SYMM - Y, X, 3/4 + Z SYMM Y, - X, 1/4 + Z SFAC C H N O P S UNIT 72 96 20 8 12 8 V = 2219.95 F(000) = 1040.0 Mu = 0.48 mm-1 Cell Wt = 1997.81 Rho = 1.494 MERG 2 OMIT -3.00 55.00 OMIT 1 2 -2 OMIT 1 2 2 OMIT 0 1 2 FMAP 2 PLAN 20 SIZE 0.02 0.05 0.60 ACTA BOND WGHT 0.02650 0.67230 L.S. 4 TEMP -153.00 FVAR 0.68730 C1 1 0.337208 0.208632 -0.137951 11.00000 0.02530 0.01892 = 0.01577 0.00389 0.00024 0.00034 C2 1 0.456750 0.208220 -0.151228 11.00000 0.02623 0.02417 = 0.02623 0.00754 0.00497 0.00505 AFIX 43 H2 2 0.493097 0.141621 -0.173607 11.00000 -1.20000 AFIX 0 C3 1 0.522723 0.305161 -0.131746 11.00000 0.02794 0.03238 = 0.03376 0.01089 0.00220 -0.00398 AFIX 43 H3 2 0.604300 0.304962 -0.140632 11.00000 -1.20000 AFIX 0 C4 1 0.469429 0.402127 -0.099344 11.00000 0.04545 0.02372 = 0.03069 0.00710 -0.00434 -0.00847 AFIX 43 H4 2 0.514656 0.468364 -0.085805 11.00000 -1.20000 AFIX 0 C5 1 0.350283 0.403054 -0.086542 11.00000 0.04788 0.02101 = 0.02958 0.00119 0.00190 0.00617 AFIX 43 H5 2 0.314283 0.470005 -0.064394 11.00000 -1.20000 AFIX 0 C6 1 0.283166 0.306362 -0.105985 11.00000 0.02851 0.02646 = 0.02523 0.00308 0.00390 0.00506 AFIX 43 H6 2 0.201492 0.307087 -0.097536 11.00000 -1.20000 AFIX 0 C7 1 0.330873 -0.209217 -0.120310 11.00000 0.01850 0.01400 = 0.01999 -0.00297 0.00074 -0.00298 C8 1 0.349983 -0.208397 -0.201924 11.00000 0.02855 0.02504 = 0.02316 -0.00186 0.00324 -0.00156 AFIX 43 H8 2 0.291387 -0.180392 -0.236901 11.00000 -1.20000 AFIX 0 C9 1 0.454910 -0.248569 -0.232524 11.00000 0.03654 0.02934 = 0.03054 -0.00590 0.01287 -0.00649 AFIX 43 H9 2 0.468451 -0.247795 -0.288360 11.00000 -1.20000 AFIX 0 C10 1 0.539417 -0.289655 -0.181112 11.00000 0.02218 0.02649 = 0.06158 -0.01764 0.01162 -0.00385 AFIX 43 H10 2 0.610992 -0.317597 -0.201888 11.00000 -1.20000 AFIX 0 C11 1 0.520686 -0.290430 -0.099830 11.00000 0.02408 0.02585 = 0.05481 -0.00773 -0.01021 0.00333 AFIX 43 H11 2 0.579796 -0.317978 -0.065089 11.00000 -1.20000 AFIX 0 C12 1 0.415859 -0.251145 -0.068514 11.00000 0.02830 0.02037 = 0.02440 -0.00336 -0.00518 -0.00015 AFIX 43 H12 2 0.402368 -0.252852 -0.012682 11.00000 -1.20000 AFIX 0 C13 1 0.608933 0.123142 0.029681 11.00000 0.01365 0.02397 = 0.02597 -0.00143 0.00154 -0.00262 AFIX 23 H13A 2 0.669216 0.182855 0.019747 11.00000 -1.20000 H13B 2 0.593889 0.081436 -0.020880 11.00000 -1.20000 AFIX 0 C14 1 0.651082 0.038032 0.092753 11.00000 0.01487 0.02681 = 0.02763 -0.00261 -0.00479 0.00195 AFIX 23 H14A 2 0.722904 -0.000365 0.073653 11.00000 -1.20000 H14B 2 0.670498 0.081430 0.141927 11.00000 -1.20000 AFIX 0 C15 1 0.561086 -0.054006 0.112093 11.00000 0.01889 0.02467 = 0.02746 0.00394 -0.00483 0.00582 AFIX 23 H15A 2 0.547314 -0.102979 0.064509 11.00000 -1.20000 H15B 2 0.590604 -0.104697 0.155263 11.00000 -1.20000 AFIX 0 C16 1 -0.054881 0.102284 0.141909 11.00000 0.01636 0.02146 = 0.02569 0.00180 -0.00087 -0.00173 AFIX 23 H16A 2 -0.097791 0.071644 0.188535 11.00000 -1.20000 H16B 2 -0.079511 0.057997 0.094227 11.00000 -1.20000 AFIX 0 C17 1 -0.082599 0.230651 0.130664 11.00000 0.01450 0.02113 = 0.02584 -0.00190 -0.00063 0.00190 AFIX 23 H17A 2 -0.167039 0.239889 0.121110 11.00000 -1.20000 H17B 2 -0.062812 0.273388 0.180039 11.00000 -1.20000 AFIX 0 C18 1 -0.015673 0.282897 0.061133 11.00000 0.01930 0.01828 = 0.02273 0.00085 -0.00487 0.00435 AFIX 23 H18A 2 -0.041434 0.246161 0.010793 11.00000 -1.20000 H18B 2 -0.032204 0.367225 0.057682 11.00000 -1.20000 AFIX 0 N1 3 0.368888 0.010885 -0.005421 11.00000 0.01389 0.01787 = 0.01741 -0.00247 -0.00336 0.00060 N2 3 0.286458 0.146558 0.115310 11.00000 0.01542 0.02169 = 0.01640 -0.00290 -0.00274 -0.00047 N3 3 0.139462 0.065926 0.000830 11.00000 0.01464 0.02158 = 0.01913 -0.00428 -0.00553 0.00189 N4 3 0.499902 0.179691 0.058320 11.00000 0.01405 0.01656 = 0.02154 -0.00023 -0.00118 -0.00069 N5 3 0.071607 0.088011 0.154392 11.00000 0.01586 0.01580 = 0.02088 0.00380 -0.00293 0.00199 O1 4 0.452229 -0.000555 0.136951 11.00000 0.01673 0.02315 = 0.01878 0.00448 -0.00332 0.00109 O2 4 0.109633 0.264816 0.071473 11.00000 0.01777 0.01493 = 0.02046 0.00188 -0.00032 0.00084 P1 5 0.245524 0.010561 -0.047081 11.00000 0.01508 0.01532 = 0.01343 -0.00087 -0.00292 -0.00030 P2 5 0.393409 0.084563 0.073809 11.00000 0.01280 0.01492 = 0.01411 0.00044 -0.00265 -0.00053 P3 5 0.156961 0.136294 0.083223 11.00000 0.01359 0.01458 = 0.01466 -0.00049 -0.00216 0.00073 S1 6 0.254981 0.081682 -0.161899 11.00000 0.03043 0.02468 = 0.01469 0.00321 -0.00465 -0.00237 S2 6 0.196031 -0.158683 -0.080608 11.00000 0.01723 0.01961 = 0.01942 -0.00470 0.00198 -0.00431 H4N 2 0.480704 0.234375 0.028465 11.00000 0.02460 H5N 2 0.089384 0.029895 0.172199 11.00000 0.03062 HKLF 4 Covalent radii and connectivity table for 2007src0258 in P4(3) C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 S 1.030 C1 - C6 C2 S1 C2 - C3 C1 C3 - C4 C2 C4 - C3 C5 C5 - C4 C6 C6 - C1 C5 C7 - C8 C12 S2 C8 - C7 C9 C9 - C10 C8 C10 - C11 C9 C11 - C10 C12 C12 - C11 C7 C13 - N4 C14 C14 - C15 C13 C15 - O1 C14 C16 - N5 C17 C17 - C18 C16 C18 - O2 C17 N1 - P1 P2 N2 - P2 P3 N3 - P1 P3 N4 - C13 P2 N5 - C16 P3 O1 - C15 P2 O2 - C18 P3 P1 - N1 N3 S1 S2 P2 - N2 O1 N1 N4 P3 - O2 N2 N3 N5 S1 - C1 P1 S2 - C7 P1 Floating origin restraints generated 56868 Reflections read, of which 96 rejected -14 =< h =< 14, -14 =< k =< 14, -20 =< l =< 21, Max. 2-theta = 54.97 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) -1 2 -14 693.81 8.93 4 47.43 0 2 -14 323.81 5.29 2 43.28 2 Inconsistent equivalents 4987 Unique reflections, of which 0 suppressed R(int) = 0.0419 R(sigma) = 0.0228 Friedel opposites not merged Maximum memory for data reduction = 2592 / 52906 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 = 3366 / 349795 wR2 = 0.0539 before cycle 1 for 4987 data and 279 / 279 parameters GooF = S = 1.032; Restrained GooF = 1.032 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0265 * P )^2 + 0.67 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.68710 0.00057 -0.357 OSF Mean shift/esd = 0.042 Maximum = -0.357 for OSF Max. shift = 0.004 A for H5N Max. dU = 0.001 for H4N Least-squares cycle 2 Maximum vector length = 511 Memory required = 3366 / 349795 wR2 = 0.0539 before cycle 2 for 4987 data and 279 / 279 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0265 * P )^2 + 0.67 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.68701 0.00057 -0.155 OSF Mean shift/esd = 0.014 Maximum = -0.155 for OSF Max. shift = 0.001 A for H5N Max. dU = 0.000 for H5N Least-squares cycle 3 Maximum vector length = 511 Memory required = 3366 / 349795 wR2 = 0.0539 before cycle 3 for 4987 data and 279 / 279 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0265 * P )^2 + 0.67 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.68701 0.00057 0.001 OSF Mean shift/esd = 0.000 Maximum = 0.004 for U11 H5N Max. shift = 0.000 A for H5N Max. dU = 0.000 for H5N Least-squares cycle 4 Maximum vector length = 511 Memory required = 3366 / 349795 wR2 = 0.0539 before cycle 4 for 4987 data and 279 / 279 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0265 * P )^2 + 0.67 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.68701 0.00057 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.001 for z H5N Max. shift = 0.000 A for H5N Max. dU = 0.000 for H4N 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 H2 0.4931 0.1416 -0.1736 43 0.950 0.000 C2 C3 C1 H3 0.6043 0.3050 -0.1406 43 0.950 0.000 C3 C4 C2 H4 0.5147 0.4684 -0.0858 43 0.950 0.000 C4 C3 C5 H5 0.3142 0.4700 -0.0644 43 0.950 0.000 C5 C4 C6 H6 0.2015 0.3071 -0.0975 43 0.950 0.000 C6 C1 C5 H8 0.2914 -0.1804 -0.2369 43 0.950 0.000 C8 C7 C9 H9 0.4684 -0.2478 -0.2884 43 0.950 0.000 C9 C10 C8 H10 0.6110 -0.3176 -0.2019 43 0.950 0.000 C10 C11 C9 H11 0.5798 -0.3180 -0.0651 43 0.950 0.000 C11 C10 C12 H12 0.4024 -0.2528 -0.0127 43 0.950 0.000 C12 C11 C7 H13A 0.6692 0.1829 0.0198 23 0.990 0.000 C13 N4 C14 H13B 0.5939 0.0815 -0.0209 23 0.990 0.000 C13 N4 C14 H14A 0.7229 -0.0004 0.0736 23 0.990 0.000 C14 C15 C13 H14B 0.6705 0.0814 0.1419 23 0.990 0.000 C14 C15 C13 H15A 0.5473 -0.1030 0.0645 23 0.990 0.000 C15 O1 C14 H15B 0.5906 -0.1047 0.1553 23 0.990 0.000 C15 O1 C14 H16A -0.0978 0.0716 0.1885 23 0.990 0.000 C16 N5 C17 H16B -0.0795 0.0580 0.0942 23 0.990 0.000 C16 N5 C17 H17A -0.1670 0.2399 0.1211 23 0.990 0.000 C17 C18 C16 H17B -0.0628 0.2734 0.1800 23 0.990 0.000 C17 C18 C16 H18A -0.0414 0.2461 0.0108 23 0.990 0.000 C18 O2 C17 H18B -0.0322 0.3672 0.0577 23 0.990 0.000 C18 O2 C17 2007src0258 in P4(3) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.33720 0.20863 -0.13795 1.00000 0.02531 0.01885 0.01570 0.00392 0.00021 0.00037 0.01995 0.00289 0.00015 0.00014 0.00010 0.00000 0.00083 0.00080 0.00075 0.00058 0.00061 0.00064 0.00032 C2 0.45675 0.20822 -0.15123 1.00000 0.02625 0.02414 0.02612 0.00747 0.00493 0.00506 0.02550 0.00333 0.00015 0.00016 0.00011 0.00000 0.00090 0.00087 0.00088 0.00068 0.00069 0.00070 0.00036 H2 0.49310 0.14162 -0.17361 1.00000 0.03060 0.00000 0.00000 C3 0.52272 0.30517 -0.13175 1.00000 0.02793 0.03231 0.03370 0.01091 0.00222 -0.00397 0.03131 0.00363 0.00017 0.00018 0.00012 0.00000 0.00096 0.00106 0.00104 0.00080 0.00077 0.00081 0.00041 H3 0.60429 0.30497 -0.14065 1.00000 0.03757 0.00000 0.00000 C4 0.46944 0.40213 -0.09934 1.00000 0.04534 0.02373 0.03067 0.00710 -0.00429 -0.00848 0.03325 0.00361 0.00019 0.00017 0.00012 0.00000 0.00117 0.00093 0.00103 0.00074 0.00084 0.00086 0.00043 H4 0.51467 0.46836 -0.08578 1.00000 0.03990 0.00000 0.00000 C5 0.35026 0.40305 -0.08655 1.00000 0.04782 0.02101 0.02958 0.00114 0.00191 0.00615 0.03280 0.00367 0.00019 0.00016 0.00012 0.00000 0.00119 0.00087 0.00099 0.00073 0.00086 0.00082 0.00042 H5 0.31425 0.47001 -0.06442 1.00000 0.03936 0.00000 0.00000 C6 0.28317 0.30636 -0.10598 1.00000 0.02842 0.02644 0.02519 0.00309 0.00388 0.00500 0.02668 0.00342 0.00017 0.00016 0.00011 0.00000 0.00093 0.00094 0.00091 0.00069 0.00069 0.00074 0.00038 H6 0.20150 0.30707 -0.09751 1.00000 0.03202 0.00000 0.00000 C7 0.33088 -0.20922 -0.12030 1.00000 0.01847 0.01397 0.01991 -0.00295 0.00076 -0.00300 0.01745 0.00270 0.00014 0.00014 0.00010 0.00000 0.00076 0.00073 0.00077 0.00056 0.00059 0.00059 0.00031 C8 0.34999 -0.20840 -0.20191 1.00000 0.02853 0.02496 0.02314 -0.00181 0.00321 -0.00156 0.02554 0.00315 0.00016 0.00016 0.00011 0.00000 0.00093 0.00090 0.00088 0.00065 0.00068 0.00073 0.00037 H8 0.29141 -0.18038 -0.23689 1.00000 0.03065 0.00000 0.00000 C9 0.45492 -0.24859 -0.23251 1.00000 0.03650 0.02922 0.03054 -0.00594 0.01289 -0.00644 0.03209 0.00346 0.00018 0.00017 0.00012 0.00000 0.00108 0.00100 0.00101 0.00077 0.00081 0.00082 0.00042 H9 0.46844 -0.24784 -0.28835 1.00000 0.03851 0.00000 0.00000 C10 0.53941 -0.28965 -0.18112 1.00000 0.02213 0.02643 0.06155 -0.01760 0.01165 -0.00386 0.03670 0.00350 0.00017 0.00017 0.00015 0.00000 0.00090 0.00097 0.00142 0.00093 0.00090 0.00074 0.00049 H10 0.61099 -0.31758 -0.20190 1.00000 0.04404 0.00000 0.00000 C11 0.52069 -0.29044 -0.09984 1.00000 0.02414 0.02581 0.05477 -0.00773 -0.01022 0.00334 0.03490 0.00344 0.00017 0.00017 0.00014 0.00000 0.00095 0.00096 0.00134 0.00088 0.00085 0.00076 0.00046 H11 0.57980 -0.31799 -0.06511 1.00000 0.04189 0.00000 0.00000 C12 0.41585 -0.25114 -0.06853 1.00000 0.02821 0.02038 0.02436 -0.00341 -0.00514 -0.00016 0.02432 0.00294 0.00016 0.00015 0.00011 0.00000 0.00091 0.00082 0.00090 0.00064 0.00066 0.00068 0.00036 H12 0.40236 -0.25285 -0.01269 1.00000 0.02918 0.00000 0.00000 C13 0.60893 0.12316 0.02968 1.00000 0.01364 0.02392 0.02592 -0.00142 0.00156 -0.00259 0.02116 0.00294 0.00014 0.00015 0.00010 0.00000 0.00075 0.00085 0.00087 0.00067 0.00061 0.00063 0.00033 H13A 0.66921 0.18288 0.01976 1.00000 0.02539 0.00000 0.00000 H13B 0.59389 0.08146 -0.02089 1.00000 0.02539 0.00000 0.00000 C14 0.65109 0.03802 0.09275 1.00000 0.01485 0.02680 0.02750 -0.00252 -0.00474 0.00199 0.02305 0.00290 0.00014 0.00015 0.00011 0.00000 0.00074 0.00087 0.00088 0.00069 0.00064 0.00064 0.00034 H14A 0.72290 -0.00039 0.07364 1.00000 0.02766 0.00000 0.00000 H14B 0.67052 0.08141 0.14193 1.00000 0.02766 0.00000 0.00000 C15 0.56108 -0.05399 0.11209 1.00000 0.01880 0.02466 0.02746 0.00394 -0.00483 0.00582 0.02364 0.00306 0.00015 0.00015 0.00011 0.00000 0.00082 0.00086 0.00089 0.00068 0.00066 0.00067 0.00036 H15A 0.54730 -0.10297 0.06451 1.00000 0.02837 0.00000 0.00000 H15B 0.59059 -0.10469 0.15527 1.00000 0.02837 0.00000 0.00000 C16 -0.05487 0.10229 0.14191 1.00000 0.01630 0.02140 0.02563 0.00181 -0.00090 -0.00172 0.02111 0.00293 0.00014 0.00015 0.00010 0.00000 0.00078 0.00082 0.00085 0.00063 0.00062 0.00065 0.00033 H16A -0.09778 0.07165 0.18853 1.00000 0.02533 0.00000 0.00000 H16B -0.07950 0.05801 0.09422 1.00000 0.02533 0.00000 0.00000 C17 -0.08260 0.23064 0.13067 1.00000 0.01443 0.02111 0.02581 -0.00190 -0.00062 0.00193 0.02045 0.00287 0.00014 0.00015 0.00010 0.00000 0.00075 0.00079 0.00087 0.00063 0.00060 0.00065 0.00033 H17A -0.16704 0.23987 0.12111 1.00000 0.02454 0.00000 0.00000 H17B -0.06281 0.27338 0.18004 1.00000 0.02454 0.00000 0.00000 C18 -0.01568 0.28288 0.06114 1.00000 0.01917 0.01826 0.02271 0.00085 -0.00489 0.00439 0.02005 0.00288 0.00014 0.00014 0.00010 0.00000 0.00079 0.00076 0.00083 0.00061 0.00061 0.00062 0.00033 H18A -0.04144 0.24615 0.01080 1.00000 0.02406 0.00000 0.00000 H18B -0.03222 0.36721 0.05769 1.00000 0.02406 0.00000 0.00000 N1 0.36889 0.01090 -0.00542 1.00000 0.01386 0.01778 0.01739 -0.00248 -0.00338 0.00059 0.01635 0.00222 0.00011 0.00011 0.00008 0.00000 0.00061 0.00064 0.00064 0.00050 0.00049 0.00050 0.00026 N2 0.28645 0.14655 0.11531 1.00000 0.01534 0.02158 0.01634 -0.00292 -0.00272 -0.00042 0.01775 0.00224 0.00012 0.00012 0.00008 0.00000 0.00065 0.00068 0.00064 0.00051 0.00049 0.00052 0.00027 N3 0.13947 0.06592 0.00083 1.00000 0.01461 0.02150 0.01904 -0.00428 -0.00553 0.00187 0.01838 0.00232 0.00011 0.00012 0.00008 0.00000 0.00063 0.00067 0.00068 0.00050 0.00051 0.00051 0.00028 N4 0.49990 0.17968 0.05832 1.00000 0.01398 0.01651 0.02152 -0.00021 -0.00114 -0.00070 0.01734 0.00231 0.00012 0.00012 0.00008 0.00000 0.00065 0.00066 0.00069 0.00054 0.00050 0.00051 0.00027 N5 0.07161 0.08802 0.15439 1.00000 0.01580 0.01577 0.02086 0.00382 -0.00292 0.00201 0.01748 0.00232 0.00012 0.00013 0.00008 0.00000 0.00066 0.00068 0.00071 0.00053 0.00051 0.00053 0.00027 O1 0.45222 -0.00054 0.13695 1.00000 0.01671 0.02308 0.01873 0.00447 -0.00331 0.00113 0.01951 0.00197 0.00010 0.00010 0.00007 0.00000 0.00055 0.00058 0.00055 0.00044 0.00043 0.00046 0.00024 O2 0.10964 0.26481 0.07147 1.00000 0.01762 0.01493 0.02047 0.00190 -0.00035 0.00085 0.01767 0.00190 0.00009 0.00009 0.00007 0.00000 0.00055 0.00053 0.00057 0.00043 0.00043 0.00043 0.00022 P1 0.24553 0.01056 -0.04708 1.00000 0.01505 0.01530 0.01340 -0.00087 -0.00292 -0.00030 0.01458 0.00067 0.00003 0.00003 0.00002 0.00000 0.00018 0.00019 0.00017 0.00014 0.00014 0.00015 0.00008 P2 0.39341 0.08456 0.07381 1.00000 0.01277 0.01489 0.01409 0.00043 -0.00265 -0.00053 0.01391 0.00064 0.00003 0.00003 0.00002 0.00000 0.00018 0.00018 0.00018 0.00014 0.00014 0.00014 0.00008 P3 0.15696 0.13630 0.08322 1.00000 0.01356 0.01454 0.01463 -0.00049 -0.00215 0.00074 0.01424 0.00064 0.00003 0.00003 0.00002 0.00000 0.00018 0.00018 0.00018 0.00014 0.00014 0.00014 0.00008 S1 0.25498 0.08168 -0.16190 1.00000 0.03039 0.02464 0.01467 0.00321 -0.00466 -0.00238 0.02323 0.00073 0.00004 0.00004 0.00002 0.00000 0.00023 0.00021 0.00019 0.00015 0.00015 0.00017 0.00009 S2 0.19603 -0.15868 -0.08061 1.00000 0.01720 0.01957 0.01940 -0.00470 0.00197 -0.00432 0.01872 0.00067 0.00003 0.00003 0.00002 0.00000 0.00019 0.00019 0.00019 0.00014 0.00015 0.00015 0.00008 H4N 0.48062 0.23425 0.02842 1.00000 0.02536 0.03704 0.00186 0.00190 0.00133 0.00000 0.00541 H5N 0.08969 0.02989 0.17203 1.00000 0.03137 0.03883 0.00199 0.00203 0.00139 0.00000 0.00613 Final Structure Factor Calculation for 2007src0258 in P4(3) Total number of l.s. parameters = 279 Maximum vector length = 511 Memory required = 3089 / 27090 wR2 = 0.0539 before cycle 5 for 4987 data and 2 / 279 parameters GooF = S = 1.033; Restrained GooF = 1.033 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0265 * P )^2 + 0.67 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0218 for 4844 Fo > 4sig(Fo) and 0.0231 for all 4987 data wR2 = 0.0539, GooF = S = 1.033, Restrained GooF = 1.033 for all data Flack x parameter = 0.0091 with esd 0.0410 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Occupancy sum of asymmetric unit = 30.00 for non-hydrogen and 24.00 for hydrogen atoms Principal mean square atomic displacements U 0.0254 0.0215 0.0131 C1 0.0372 0.0218 0.0175 C2 0.0440 0.0302 0.0197 C3 0.0504 0.0311 0.0183 C4 0.0494 0.0294 0.0196 C5 0.0350 0.0227 0.0223 C6 0.0222 0.0183 0.0118 C7 0.0308 0.0245 0.0213 C8 0.0504 0.0257 0.0202 C9 0.0719 0.0200 0.0182 C10 0.0599 0.0240 0.0207 C11 0.0321 0.0233 0.0176 C12 0.0272 0.0234 0.0129 C13 0.0312 0.0248 0.0132 C14 0.0303 0.0280 0.0126 C15 0.0265 0.0211 0.0158 C16 0.0266 0.0208 0.0139 C17 0.0266 0.0209 0.0126 C18 0.0212 0.0161 0.0117 N1 0.0230 0.0178 0.0125 N2 0.0268 0.0176 0.0108 N3 0.0217 0.0167 0.0136 N4 0.0233 0.0178 0.0114 N5 0.0260 0.0197 0.0129 O1 0.0211 0.0179 0.0141 O2 0.0173 0.0154 0.0110 P1 0.0164 0.0146 0.0107 P2 0.0167 0.0142 0.0118 P3 0.0329 0.0239 0.0129 S1 0.0264 0.0163 0.0134 S2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.051 0.076 0.098 0.122 0.143 0.168 0.197 0.240 0.316 1.000 Number in group 510. 490. 512. 500. 480. 507. 493. 498. 494. 503. GooF 1.011 1.046 1.063 1.084 1.075 0.982 0.975 0.998 1.002 1.077 K 0.989 0.975 0.980 0.983 0.993 0.994 1.006 1.009 1.010 0.998 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.65 inf Number in group 505. 521. 478. 505. 484. 501. 495. 502. 494. 502. GooF 0.968 0.962 1.019 0.868 0.885 0.942 0.870 0.864 0.993 1.682 K 0.985 0.996 1.001 1.007 1.010 1.017 1.010 1.009 1.001 0.989 R1 0.046 0.036 0.033 0.025 0.023 0.021 0.017 0.014 0.015 0.022 Recommended weighting scheme: WGHT 0.0259 0.6856 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) 0 1 -2 2393.61 4456.82 5.37 0.465 6.78 4 4 0 875.27 1074.22 5.03 0.229 2.03 4 5 3 173.74 119.13 4.84 0.076 1.71 1 3 -3 1683.21 1992.21 4.73 0.311 3.05 0 0 8 2747.28 3216.68 4.54 0.395 2.10 0 5 0 413.99 325.02 4.46 0.126 2.30 1 3 3 1742.61 2042.84 4.43 0.315 3.05 0 3 9 836.90 996.17 4.35 0.220 1.68 -1 5 -4 1206.34 1021.82 4.34 0.223 1.99 -1 5 0 251.25 326.43 4.27 0.126 2.26 0 3 -9 885.98 1048.08 4.19 0.226 1.68 4 9 -2 14.91 38.58 4.17 0.043 1.16 1 6 0 6471.59 5716.83 4.09 0.527 1.89 -3 5 0 431.85 524.14 3.90 0.160 1.97 -2 5 0 28.73 11.72 3.90 0.024 2.14 0 2 4 462.11 382.24 3.86 0.136 3.39 1 1 -7 1299.41 1499.96 3.83 0.270 2.30 1 4 -8 298.05 238.89 3.74 0.108 1.68 -2 6 4 153.42 112.19 3.73 0.074 1.67 0 3 -5 486.46 406.65 3.69 0.141 2.53 3 5 0 506.49 424.18 3.64 0.144 1.97 4 5 -3 162.60 121.54 3.64 0.077 1.71 1 5 -5 1647.18 1873.24 3.63 0.302 1.87 1 1 7 1329.07 1511.69 3.59 0.271 2.30 1 4 8 308.99 251.24 3.57 0.111 1.68 2 5 0 207.37 160.19 3.56 0.088 2.14 -1 5 4 1187.93 1033.04 3.53 0.224 1.99 -4 6 -11 47.68 26.95 3.53 0.036 1.10 0 2 -4 475.02 401.21 3.48 0.140 3.39 0 6 -2 204.45 255.53 3.44 0.111 1.87 0 3 5 440.64 370.23 3.43 0.134 2.53 -1 5 1 1347.35 1183.04 3.42 0.240 2.24 -2 6 -4 154.97 117.23 3.35 0.075 1.67 -1 14 -4 210.50 282.44 3.33 0.117 0.80 1 1 3 2903.12 3248.00 3.29 0.397 4.61 5 6 0 337.05 401.98 3.21 0.140 1.47 3 5 -6 553.90 644.51 3.21 0.177 1.61 -5 8 9 89.12 121.65 3.19 0.077 1.02 3 3 4 462.16 394.62 3.17 0.138 2.28 2 7 0 641.31 737.71 3.14 0.189 1.58 -1 3 19 1040.77 910.67 3.12 0.210 0.86 -2 4 2 574.94 662.60 3.07 0.179 2.46 -1 5 -1 1350.83 1202.62 3.06 0.242 2.24 3 5 6 554.15 637.15 3.06 0.176 1.61 -1 5 -5 72.93 51.51 3.04 0.050 1.87 2 12 -4 266.15 322.49 3.03 0.125 0.92 9 11 3 147.38 206.35 2.99 0.100 0.80 3 5 2 7080.29 6476.79 2.98 0.561 1.92 3 3 5 748.76 660.43 2.98 0.179 2.11 -1 3 -7 221.86 266.67 2.96 0.114 2.00 Bond lengths and angles C1 - Distance Angles C6 1.3918 (0.0024) C2 1.3930 (0.0024) 120.33 (0.17) S1 1.7853 (0.0017) 120.72 (0.14) 118.95 (0.13) C1 - C6 C2 C2 - Distance Angles C3 1.3877 (0.0028) C1 1.3930 (0.0024) 119.95 (0.17) C2 - C3 C3 - Distance Angles C4 1.3838 (0.0030) C2 1.3877 (0.0028) 119.87 (0.18) C3 - C4 C4 - Distance Angles C3 1.3838 (0.0030) C5 1.3874 (0.0030) 120.30 (0.19) C4 - C3 C5 - Distance Angles C4 1.3874 (0.0030) C6 1.3923 (0.0029) 120.34 (0.18) C5 - C4 C6 - Distance Angles C1 1.3918 (0.0024) C5 1.3923 (0.0029) 119.21 (0.18) C6 - C1 C7 - Distance Angles C8 1.3873 (0.0024) C12 1.3938 (0.0024) 120.45 (0.17) S2 1.7851 (0.0016) 120.26 (0.14) 119.28 (0.13) C7 - C8 C12 C8 - Distance Angles C7 1.3873 (0.0024) C9 1.3906 (0.0027) 120.00 (0.18) C8 - C7 C9 - Distance Angles C10 1.3825 (0.0032) C8 1.3906 (0.0027) 119.54 (0.19) C9 - C10 C10 - Distance Angles C11 1.3810 (0.0033) C9 1.3825 (0.0032) 120.59 (0.19) C10 - C11 C11 - Distance Angles C10 1.3810 (0.0033) C12 1.3908 (0.0028) 120.42 (0.19) C11 - C10 C12 - Distance Angles C11 1.3908 (0.0028) C7 1.3938 (0.0024) 118.99 (0.18) C12 - C11 C13 - Distance Angles N4 1.4920 (0.0021) C14 1.5213 (0.0024) 108.91 (0.13) C13 - N4 C14 - Distance Angles C15 1.5156 (0.0024) C13 1.5213 (0.0024) 112.38 (0.13) C14 - C15 C15 - Distance Angles O1 1.4557 (0.0020) C14 1.5156 (0.0024) 110.73 (0.13) C15 - O1 C16 - Distance Angles N5 1.4788 (0.0021) C17 1.5219 (0.0023) 109.35 (0.13) C16 - N5 C17 - Distance Angles C18 1.5215 (0.0024) C16 1.5219 (0.0023) 111.85 (0.14) C17 - C18 C18 - Distance Angles O2 1.4665 (0.0019) C17 1.5215 (0.0024) 110.52 (0.13) C18 - O2 N1 - Distance Angles P1 1.5817 (0.0013) P2 1.6018 (0.0013) 121.75 (0.08) N1 - P1 N2 - Distance Angles P2 1.5832 (0.0014) P3 1.5880 (0.0013) 123.10 (0.09) N2 - P2 N3 - Distance Angles P1 1.5937 (0.0014) P3 1.6148 (0.0014) 122.47 (0.08) N3 - P1 N4 - Distance Angles C13 1.4920 (0.0021) P2 1.6626 (0.0014) 112.51 (0.11) N4 - C13 N5 - Distance Angles C16 1.4788 (0.0021) P3 1.6427 (0.0014) 116.57 (0.11) N5 - C16 O1 - Distance Angles C15 1.4557 (0.0020) P2 1.5933 (0.0011) 115.72 (0.10) O1 - C15 O2 - Distance Angles C18 1.4665 (0.0019) P3 1.5874 (0.0011) 118.92 (0.10) O2 - C18 P1 - Distance Angles N1 1.5817 (0.0013) N3 1.5937 (0.0014) 117.55 (0.07) S1 2.0963 (0.0006) 111.03 (0.05) 110.35 (0.06) S2 2.1046 (0.0006) 111.29 (0.05) 107.30 (0.06) 97.42 (0.02) P1 - N1 N3 S1 P2 - Distance Angles N2 1.5832 (0.0014) O1 1.5933 (0.0011) 108.29 (0.07) N1 1.6018 (0.0013) 117.81 (0.07) 107.58 (0.07) N4 1.6626 (0.0014) 110.17 (0.07) 101.27 (0.07) 110.36 (0.07) P2 - N2 O1 N1 P3 - Distance Angles O2 1.5874 (0.0011) N2 1.5880 (0.0013) 107.13 (0.07) N3 1.6148 (0.0014) 108.52 (0.07) 116.39 (0.07) N5 1.6427 (0.0014) 101.55 (0.07) 109.81 (0.07) 112.26 (0.07) P3 - O2 N2 N3 S1 - Distance Angles C1 1.7853 (0.0017) P1 2.0963 (0.0006) 98.02 (0.06) S1 - C1 S2 - Distance Angles C7 1.7851 (0.0016) P1 2.1046 (0.0006) 99.55 (0.05) S2 - C7 FMAP and GRID set by program FMAP 2 3 21 GRID -1.389 -2 -2 1.389 2 2 R1 = 0.0212 for 2629 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.17 at 0.9578 0.7600 -0.0023 [ 1.72 A from H8 ] Deepest hole -0.27 at 0.3784 0.1380 0.0505 [ 0.75 A from P2 ] Mean = 0.00, Rms deviation from mean = 0.04 e/A^3, Highest memory used = 2922 / 20559 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.2400 -0.0422 -0.2523 1.00000 0.05 0.17 1.72 H8 1.94 H16A 2.09 S1 2.10 H14B Q2 1 0.5408 -0.1631 -0.2508 1.00000 0.05 0.17 1.43 C9 1.43 H9 1.87 C10 2.09 H18B Q3 1 0.4212 0.0221 0.2188 1.00000 0.05 0.16 1.44 O1 1.62 H18B 2.14 H18A 2.22 C18 Q4 1 0.3023 0.1640 -0.1495 1.00000 0.05 0.15 0.68 C1 1.11 S1 1.81 C6 1.85 C2 Q5 1 0.2784 0.1355 0.1640 1.00000 0.05 0.15 0.83 N2 1.95 P3 1.99 H18A 2.09 P2 Q6 1 0.3982 0.0003 -0.1869 1.00000 0.05 0.15 1.94 S1 1.97 H2 2.48 C8 2.56 C2 Q7 1 0.3353 -0.2159 -0.1574 1.00000 0.05 0.14 0.63 C7 0.77 C8 1.48 H8 1.80 C12 Q8 1 0.3995 -0.2070 -0.2059 1.00000 0.05 0.14 0.57 C8 0.91 C9 1.38 H8 1.64 C7 Q9 1 -0.0836 0.4684 -0.0197 1.00000 0.05 0.14 1.84 H18B 1.85 O1 2.05 H9 2.18 C9 Q10 1 0.3264 0.0099 -0.2306 1.00000 0.05 0.14 1.64 S1 2.23 H8 2.38 H14B 2.40 H15B Q11 1 0.5421 -0.0938 0.1676 1.00000 0.05 0.14 0.61 H15B 1.06 C15 1.58 O1 1.73 H15A Q12 1 0.5712 -0.0189 0.2536 1.00000 0.05 0.14 1.94 H15B 2.01 H2 2.40 O1 2.41 C15 Q13 1 0.6286 0.0266 0.2326 1.00000 0.05 0.14 1.72 H14B 2.04 H15B 2.06 H8 2.36 C15 Q14 1 0.4374 -0.1064 0.1963 1.00000 0.05 0.13 1.58 O1 1.89 H15B 2.00 H6 2.09 C15 Q15 1 0.4785 0.3391 -0.1100 1.00000 0.05 0.13 0.74 C3 0.75 C4 1.59 H3 1.60 H4 Q16 1 0.4853 0.2639 -0.1522 1.00000 0.05 0.13 0.72 C2 0.73 C3 1.45 H2 1.46 H3 Q17 1 -0.1395 0.4082 -0.0240 1.00000 0.05 0.13 1.90 H18B 1.90 H9 2.13 C9 2.25 H18A Q18 1 0.3125 0.1083 0.1215 1.00000 0.05 0.13 0.54 N2 1.26 P2 1.93 P3 2.05 O1 Q19 1 0.6023 0.0022 0.0964 1.00000 0.05 0.13 0.70 C14 0.84 C15 1.42 H14B 1.44 H14A Q20 1 0.4603 0.1030 -0.1896 1.00000 0.05 0.13 0.64 H2 1.37 C2 2.06 C1 2.42 S1 Shortest distances between peaks (including symmetry equivalents) 2 17 0.75 5 18 0.87 10 13 0.91 3 9 0.91 12 13 0.91 9 17 0.95 2 9 0.97 6 12 1.08 7 8 1.10 6 10 1.11 15 16 1.12 10 12 1.21 1 10 1.22 11 14 1.30 3 17 1.36 6 20 1.38 12 20 1.40 6 13 1.42 3 14 1.54 1 13 1.54 11 12 1.71 9 12 1.71 2 3 1.76 11 19 1.77 5 17 1.82 2 8 1.86 3 12 1.88 9 13 1.96 16 20 1.97 10 20 2.00 11 13 2.02 4 20 2.06 12 14 2.07 17 18 2.10 3 11 2.11 1 6 2.18 13 20 2.23 14 20 2.25 4 10 2.25 4 6 2.27 3 18 2.28 6 9 2.28 1 12 2.28 9 14 2.29 3 5 2.29 13 19 2.32 8 9 2.34 8 13 2.34 3 13 2.40 4 16 2.40 11 20 2.40 6 8 2.41 9 11 2.45 2 12 2.46 10 11 2.48 3 20 2.51 2 13 2.52 5 9 2.52 2 5 2.54 9 18 2.57 8 17 2.61 3 6 2.62 6 7 2.64 12 17 2.65 9 20 2.66 8 10 2.66 12 19 2.67 9 10 2.68 8 12 2.71 2 6 2.71 4 12 2.75 13 14 2.75 1 8 2.75 6 11 2.75 1 7 2.78 2 18 2.80 14 19 2.82 13 17 2.85 7 10 2.87 9 19 2.88 7 13 2.88 14 17 2.89 2 7 2.90 4 15 2.93 3 19 2.93 6 14 2.98 Time profile in seconds ----------------------- 0.07: 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 0.01: Analyse other restraints etc. 8.31: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.01: OSF, H-atoms from difference map 0.00: Set up l.s. refinement 0.00: Generate idealized H-atoms 3.64: Structure factors and derivatives 3.94: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.04: Apply other restraints 0.49: Solve l.s. equations 0.00: Generate HTAB table 0.01: Other dependent quantities, CIF, tables 0.10: Analysis of variance 0.07: Merge reflections for Fourier and .fcf 0.09: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src0258 finished at 17:55:14 Total CPU time: 16.8 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++