+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2005slh0413 started at 11:34:08 on 22-Aug-2005 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2005slh0413 in P2(1)/c CELL 0.71073 10.7073 16.3214 19.5513 90.000 91.799 90.000 ZERR 4.00 0.0004 0.0004 0.0006 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O P S CD UNIT 116 136 8 16 8 16 4 V = 3415.06 F(000) = 1584.0 Mu = 1.01 mm-1 Cell Wt = 3108.65 Rho = 1.512 MERG 2 OMIT -3.00 55.00 OMIT 1 4 0 OMIT 0 0 4 OMIT 1 2 1 OMIT 1 3 0 OMIT -1 1 3 OMIT -5 10 5 OMIT 2 0 0 OMIT 1 2 2 OMIT -1 2 1 FMAP 2 PLAN 5 SIZE 0.2 0.2 0.07 ACTA BOND $H L.S. 6 TEMP -153.00 WGHT 0.029400 1.968900 EXTI 0.000960 FVAR 0.35859 C1 1 0.005919 0.620769 -0.033438 11.00000 0.03483 0.06148 = 0.03654 -0.00924 -0.00976 -0.01359 AFIX 137 H1A 2 -0.003973 0.565840 -0.014103 11.00000 -1.50000 H1B 2 -0.003738 0.618024 -0.083396 11.00000 -1.50000 H1C 2 -0.057786 0.657320 -0.015416 11.00000 -1.50000 AFIX 0 C2 1 0.313501 0.717205 0.053849 11.00000 0.01876 0.02007 = 0.02692 -0.00082 0.00311 0.00365 C3 1 0.396479 0.723993 0.109403 11.00000 0.02686 0.03169 = 0.03318 0.00370 -0.00143 -0.00061 AFIX 43 H3 2 0.375583 0.700411 0.151970 11.00000 -1.20000 AFIX 0 C4 1 0.509969 0.764790 0.103906 11.00000 0.02291 0.03249 = 0.04713 -0.00086 -0.00831 0.00153 AFIX 43 H4 2 0.566292 0.768987 0.142267 11.00000 -1.20000 AFIX 0 C5 1 0.539552 0.799201 0.041597 11.00000 0.01923 0.01887 = 0.05786 -0.00585 0.00939 0.00317 C6 1 0.457030 0.794012 -0.014008 11.00000 0.02760 0.02159 = 0.04030 -0.00117 0.01383 0.00175 AFIX 43 H6 2 0.477362 0.818716 -0.056224 11.00000 -1.20000 AFIX 0 C7 1 0.345032 0.752966 -0.008306 11.00000 0.02472 0.02074 = 0.02813 -0.00074 0.00618 0.00564 AFIX 43 H7 2 0.289057 0.748993 -0.046835 11.00000 -1.20000 AFIX 0 C8 1 0.740180 0.844869 0.084760 11.00000 0.02188 0.03687 = 0.13003 0.00852 -0.01704 -0.00085 AFIX 137 H8A 2 0.703454 0.871349 0.124373 11.00000 -1.50000 H8B 2 0.812206 0.876787 0.070247 11.00000 -1.50000 H8C 2 0.767368 0.789384 0.097293 11.00000 -1.50000 AFIX 0 C9 1 0.060499 0.630183 0.442923 11.00000 0.02593 0.05170 = 0.03000 -0.01684 0.00522 0.00833 AFIX 137 H9A 2 0.040028 0.681602 0.419239 11.00000 -1.50000 H9B 2 0.064235 0.639652 0.492442 11.00000 -1.50000 H9C 2 -0.003960 0.589257 0.431800 11.00000 -1.50000 AFIX 0 C10 1 0.359294 0.553334 0.343134 11.00000 0.02015 0.02121 = 0.02090 -0.00220 -0.00092 0.00114 C11 1 0.429327 0.557637 0.284447 11.00000 0.02712 0.04106 = 0.01840 0.00442 -0.00148 0.00444 AFIX 43 H11 2 0.392636 0.579982 0.243695 11.00000 -1.20000 AFIX 0 C12 1 0.550627 0.530118 0.284445 11.00000 0.02746 0.04408 = 0.02210 0.00432 0.00668 0.00451 AFIX 43 H12 2 0.597546 0.534258 0.244148 11.00000 -1.20000 AFIX 0 C13 1 0.604576 0.496170 0.343612 11.00000 0.01947 0.01996 = 0.02625 0.00019 0.00143 -0.00011 C14 1 0.535704 0.489745 0.402056 11.00000 0.02507 0.02464 = 0.02199 0.00478 -0.00296 0.00137 AFIX 43 H14 2 0.571745 0.465953 0.442390 11.00000 -1.20000 AFIX 0 C15 1 0.413396 0.518344 0.401355 11.00000 0.02396 0.02860 = 0.01995 0.00111 0.00385 -0.00079 AFIX 43 H15 2 0.366146 0.513802 0.441502 11.00000 -1.20000 AFIX 0 C16 1 0.786318 0.439472 0.398987 11.00000 0.02430 0.03787 = 0.04810 0.01754 -0.00258 0.00608 AFIX 137 H16A 2 0.783812 0.480047 0.435866 11.00000 -1.50000 H16B 2 0.873450 0.426515 0.389497 11.00000 -1.50000 H16C 2 0.743147 0.389528 0.412932 11.00000 -1.50000 AFIX 0 C17 1 -0.188018 0.668095 0.309972 11.00000 0.02345 0.01582 = 0.03601 0.00089 0.00598 0.00126 AFIX 43 H17 2 -0.188264 0.609953 0.312246 11.00000 -1.20000 AFIX 0 C18 1 -0.256760 0.711313 0.356624 11.00000 0.02019 0.01931 = 0.03446 0.00499 0.00951 0.00179 AFIX 43 H18 2 -0.302506 0.682907 0.390067 11.00000 -1.20000 AFIX 0 C19 1 -0.258694 0.796051 0.354435 11.00000 0.01388 0.01917 = 0.02229 0.00230 0.00021 0.00271 C20 1 -0.191207 0.833440 0.303721 11.00000 0.02937 0.01509 = 0.02647 0.00134 0.00457 0.00222 AFIX 43 H20 2 -0.191421 0.891421 0.299444 11.00000 -1.20000 AFIX 0 C21 1 -0.123614 0.786101 0.259403 11.00000 0.02804 0.01915 = 0.02364 0.00280 0.00561 0.00008 AFIX 43 H21 2 -0.076590 0.812907 0.225604 11.00000 -1.20000 AFIX 0 C22 1 -0.331616 0.846280 0.404032 11.00000 0.01926 0.01875 = 0.02229 0.00110 0.00245 0.00159 AFIX 23 H22A 2 -0.279816 0.893074 0.420222 11.00000 -1.20000 H22B 2 -0.350693 0.812162 0.444247 11.00000 -1.20000 AFIX 0 C23 1 -0.454048 0.878752 0.371462 11.00000 0.02048 0.02316 = 0.02191 -0.00142 0.00131 0.00518 AFIX 23 H23A 2 -0.435670 0.911194 0.330193 11.00000 -1.20000 H23B 2 -0.507900 0.832102 0.357177 11.00000 -1.20000 AFIX 0 C24 1 -0.523048 0.932393 0.422118 11.00000 0.02101 0.01977 = 0.02167 -0.00099 0.00060 0.00325 AFIX 23 H24A 2 -0.545837 0.898288 0.461699 11.00000 -1.20000 H24B 2 -0.465460 0.975717 0.439302 11.00000 -1.20000 AFIX 0 C25 1 -0.639642 0.972348 0.392693 11.00000 0.01992 0.01861 = 0.01561 0.00044 0.00431 0.00191 C26 1 -0.729918 0.929693 0.354484 11.00000 0.02192 0.01750 = 0.02950 0.00021 0.00073 0.00072 AFIX 43 H26 2 -0.720282 0.872645 0.346575 11.00000 -1.20000 AFIX 0 C27 1 -0.833663 0.970434 0.328042 11.00000 0.02098 0.01918 = 0.02907 0.00020 0.00008 -0.00265 AFIX 43 H27 2 -0.893158 0.940182 0.301276 11.00000 -1.20000 AFIX 0 C29 1 -0.768341 1.090833 0.375437 11.00000 0.03105 0.01866 = 0.03444 -0.00434 -0.00723 0.00699 AFIX 43 H29 2 -0.781417 1.147476 0.383804 11.00000 -1.20000 AFIX 0 C30 1 -0.661283 1.055031 0.402430 11.00000 0.02684 0.02212 = 0.02803 -0.00693 -0.00640 0.00204 AFIX 43 H30 2 -0.602149 1.087181 0.427798 11.00000 -1.20000 AFIX 0 N1 3 -0.121496 0.704119 0.262014 11.00000 0.01697 0.01881 = 0.02506 -0.00068 0.00266 0.00115 N2 3 -0.854834 1.050312 0.338131 11.00000 0.01909 0.01971 = 0.02344 -0.00010 0.00019 0.00084 O1 4 0.128290 0.651819 -0.014915 11.00000 0.02559 0.03921 = 0.02221 -0.00382 -0.00055 -0.00323 O2 4 0.648892 0.840612 0.029781 11.00000 0.02116 0.03212 = 0.07926 -0.00984 0.01123 -0.00469 O3 4 0.180693 0.600632 0.421143 11.00000 0.02273 0.04043 = 0.02145 -0.00927 -0.00042 0.00491 O4 4 0.725940 0.471989 0.338781 11.00000 0.02021 0.03262 = 0.03543 0.00780 0.00416 0.00517 P1 5 0.166742 0.665455 0.063938 11.00000 0.01905 0.02132 = 0.02048 0.00005 0.00175 0.00083 P2 5 0.202488 0.592463 0.340727 11.00000 0.02013 0.02308 = 0.01931 -0.00482 -0.00212 0.00257 S1 6 0.041574 0.738431 0.107645 11.00000 0.02049 0.02128 = 0.02618 0.00423 0.00598 0.00345 S2 6 0.190317 0.560366 0.114333 11.00000 0.02832 0.01882 = 0.03075 0.00143 0.00633 0.00370 S3 6 0.079419 0.511697 0.300530 11.00000 0.02249 0.01989 = 0.02174 -0.00142 -0.00188 -0.00011 S4 6 0.197534 0.700218 0.293308 11.00000 0.02750 0.01940 = 0.03636 -0.00235 -0.00844 0.00012 CD1 7 0.029336 0.624602 0.205228 11.00000 0.01620 0.01797 = 0.01987 -0.00020 0.00060 0.00036 HKLF 4 Covalent radii and connectivity table for 2005slh0413 in P2(1)/c C 0.770 H 0.320 N 0.700 O 0.660 P 1.100 S 1.030 CD 1.490 C1 - O1 C2 - C3 C7 P1 C3 - C2 C4 C4 - C5 C3 C5 - O2 C6 C4 C6 - C7 C5 C7 - C6 C2 C8 - O2 C9 - O3 C10 - C15 C11 P2 C11 - C12 C10 C12 - C11 C13 C13 - O4 C14 C12 C14 - C13 C15 C15 - C10 C14 C16 - O4 C17 - N1 C18 C18 - C17 C19 C19 - C18 C20 C22 C20 - C21 C19 C21 - N1 C20 C22 - C19 C23 C23 - C24 C22 C24 - C25 C23 C25 - C30 C26 C24 C26 - C27 C25 C27 - N2 C26 C29 - N2 C30 C30 - C29 C25 N1 - C17 C21 Cd1 N2 - C29 C27 Cd1_$2 O1 - C1 P1 O2 - C5 C8 O3 - C9 P2 O4 - C13 C16 P1 - O1 C2 S2 S1 P2 - O3 C10 S4 S3 S1 - P1 Cd1 S2 - P1 Cd1 S3 - P2 Cd1 S4 - P2 Cd1 Cd1 - N2_$1 N1 S3 S1 S2 S4 Operators for generating equivalent atoms: $1 -x-1, y-1/2, -z+1/2 $2 -x-1, y+1/2, -z+1/2 22610 Reflections read, of which 486 rejected -13 =< h =< 12, -21 =< k =< 18, -25 =< l =< 21, Max. 2-theta = 54.98 0 Systematic absence violations 0 Inconsistent equivalents 7757 Unique reflections, of which 0 suppressed R(int) = 0.0319 R(sigma) = 0.0449 Friedel opposites merged Maximum memory for data reduction = 3810 / 77002 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 = 4875 / 493197 wR2 = 0.0728 before cycle 1 for 7757 data and 384 / 384 parameters GooF = S = 1.022; Restrained GooF = 1.022 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0294 * P )^2 + 1.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.35859 0.00039 -0.010 OSF 2 0.00096 0.00019 0.001 EXTI Mean shift/esd = 0.002 Maximum = -0.046 for z Cd1 Max. shift = 0.000 A for H16C Max. dU = 0.000 for C8 Least-squares cycle 2 Maximum vector length = 511 Memory required = 4875 / 493197 wR2 = 0.0728 before cycle 2 for 7757 data and 384 / 384 parameters GooF = S = 1.022; Restrained GooF = 1.022 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0294 * P )^2 + 1.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.35858 0.00039 -0.004 OSF 2 0.00096 0.00019 0.000 EXTI Mean shift/esd = 0.001 Maximum = -0.015 for z Cd1 Max. shift = 0.000 A for H1B Max. dU = 0.000 for C8 Least-squares cycle 3 Maximum vector length = 511 Memory required = 4875 / 493197 wR2 = 0.0727 before cycle 3 for 7757 data and 384 / 384 parameters GooF = S = 1.022; Restrained GooF = 1.022 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0294 * P )^2 + 1.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.35859 0.00039 0.003 OSF 2 0.00096 0.00019 0.002 EXTI Mean shift/esd = 0.000 Maximum = 0.003 for OSF Max. shift = 0.000 A for H16C Max. dU = 0.000 for C19 Least-squares cycle 4 Maximum vector length = 511 Memory required = 4875 / 493197 wR2 = 0.0727 before cycle 4 for 7757 data and 384 / 384 parameters GooF = S = 1.022; Restrained GooF = 1.022 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0294 * P )^2 + 1.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.35859 0.00039 0.000 OSF 2 0.00096 0.00019 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for y Cd1 Max. shift = 0.000 A for H1A Max. dU = 0.000 for P2 Least-squares cycle 5 Maximum vector length = 511 Memory required = 4875 / 493197 wR2 = 0.0727 before cycle 5 for 7757 data and 384 / 384 parameters GooF = S = 1.022; Restrained GooF = 1.022 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0294 * P )^2 + 1.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.35859 0.00039 -0.001 OSF 2 0.00096 0.00019 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.002 for y Cd1 Max. shift = 0.000 A for N2 Max. dU = 0.000 for C12 Least-squares cycle 6 Maximum vector length = 511 Memory required = 4875 / 493197 wR2 = 0.0727 before cycle 6 for 7757 data and 384 / 384 parameters GooF = S = 1.022; Restrained GooF = 1.022 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0294 * P )^2 + 1.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.35859 0.00039 0.002 OSF 2 0.00096 0.00019 0.001 EXTI Mean shift/esd = 0.000 Maximum = 0.002 for OSF Max. shift = 0.000 A for H1B Max. dU = 0.000 for C1 Largest correlation matrix elements 0.635 EXTI / OSF 0.571 U22 Cd1 / OSF 0.578 U11 Cd1 / OSF 0.552 U33 Cd1 / OSF Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A -0.0040 0.5658 -0.0141 137 0.980 0.000 C1 O1 H1A H1B -0.0037 0.6180 -0.0834 137 0.980 0.000 C1 O1 H1A H1C -0.0578 0.6573 -0.0154 137 0.980 0.000 C1 O1 H1A H3 0.3756 0.7004 0.1520 43 0.950 0.000 C3 C2 C4 H4 0.5663 0.7690 0.1423 43 0.950 0.000 C4 C5 C3 H6 0.4774 0.8187 -0.0562 43 0.950 0.000 C6 C7 C5 H7 0.2891 0.7490 -0.0468 43 0.950 0.000 C7 C6 C2 H8A 0.7035 0.8713 0.1244 137 0.980 0.000 C8 O2 H8A H8B 0.8122 0.8768 0.0702 137 0.980 0.000 C8 O2 H8A H8C 0.7674 0.7894 0.0973 137 0.980 0.000 C8 O2 H8A H9A 0.0400 0.6816 0.4192 137 0.980 0.000 C9 O3 H9A H9B 0.0642 0.6397 0.4924 137 0.980 0.000 C9 O3 H9A H9C -0.0040 0.5893 0.4318 137 0.980 0.000 C9 O3 H9A H11 0.3926 0.5800 0.2437 43 0.950 0.000 C11 C12 C10 H12 0.5975 0.5343 0.2441 43 0.950 0.000 C12 C11 C13 H14 0.5717 0.4660 0.4424 43 0.950 0.000 C14 C13 C15 H15 0.3661 0.5138 0.4415 43 0.950 0.000 C15 C10 C14 H16A 0.7838 0.4800 0.4359 137 0.980 0.000 C16 O4 H16A H16B 0.8735 0.4265 0.3895 137 0.980 0.000 C16 O4 H16A H16C 0.7431 0.3895 0.4129 137 0.980 0.000 C16 O4 H16A H17 -0.1883 0.6100 0.3122 43 0.950 0.000 C17 N1 C18 H18 -0.3025 0.6829 0.3901 43 0.950 0.000 C18 C17 C19 H20 -0.1914 0.8914 0.2994 43 0.950 0.000 C20 C21 C19 H21 -0.0766 0.8129 0.2256 43 0.950 0.000 C21 N1 C20 H22A -0.2798 0.8931 0.4202 23 0.990 0.000 C22 C19 C23 H22B -0.3507 0.8122 0.4442 23 0.990 0.000 C22 C19 C23 H23A -0.4357 0.9112 0.3302 23 0.990 0.000 C23 C24 C22 H23B -0.5079 0.8321 0.3572 23 0.990 0.000 C23 C24 C22 H24A -0.5458 0.8983 0.4617 23 0.990 0.000 C24 C25 C23 H24B -0.4655 0.9757 0.4393 23 0.990 0.000 C24 C25 C23 H26 -0.7203 0.8726 0.3466 43 0.950 0.000 C26 C27 C25 H27 -0.8932 0.9402 0.3013 43 0.950 0.000 C27 N2 C26 H29 -0.7814 1.1475 0.3838 43 0.950 0.000 C29 N2 C30 H30 -0.6021 1.0872 0.4278 43 0.950 0.000 C30 C29 C25 2005slh0413 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.00592 0.62077 -0.03344 1.00000 0.03483 0.06148 0.03654 -0.00924 -0.00976 -0.01359 0.04451 0.00472 0.00027 0.00020 0.00016 0.00000 0.00160 0.00206 0.00171 0.00142 0.00131 0.00146 0.00076 H1A -0.00397 0.56584 -0.01410 1.00000 0.06677 0.00000 0.00000 H1B -0.00374 0.61802 -0.08340 1.00000 0.06677 0.00000 0.00000 H1C -0.05779 0.65732 -0.01542 1.00000 0.06677 0.00000 0.00000 C2 0.31350 0.71721 0.05385 1.00000 0.01876 0.02007 0.02692 -0.00082 0.00311 0.00365 0.02187 0.00411 0.00021 0.00014 0.00012 0.00000 0.00114 0.00116 0.00131 0.00094 0.00097 0.00096 0.00050 C3 0.39648 0.72399 0.10940 1.00000 0.02686 0.03169 0.03318 0.00370 -0.00143 -0.00061 0.03062 0.00449 0.00023 0.00016 0.00014 0.00000 0.00135 0.00140 0.00149 0.00111 0.00111 0.00115 0.00058 H3 0.37558 0.70041 0.15197 1.00000 0.03675 0.00000 0.00000 C4 0.50997 0.76479 0.10391 1.00000 0.02291 0.03249 0.04713 -0.00086 -0.00831 0.00153 0.03437 0.00470 0.00024 0.00016 0.00015 0.00000 0.00131 0.00143 0.00176 0.00124 0.00118 0.00117 0.00063 H4 0.56629 0.76899 0.14227 1.00000 0.04125 0.00000 0.00000 C5 0.53955 0.79920 0.04160 1.00000 0.01923 0.01887 0.05786 -0.00585 0.00939 0.00317 0.03182 0.00470 0.00023 0.00015 0.00015 0.00000 0.00125 0.00123 0.00189 0.00117 0.00120 0.00103 0.00062 C6 0.45703 0.79401 -0.01401 1.00000 0.02760 0.02159 0.04030 -0.00117 0.01383 0.00175 0.02956 0.00461 0.00023 0.00015 0.00014 0.00000 0.00134 0.00123 0.00160 0.00108 0.00117 0.00108 0.00058 H6 0.47736 0.81872 -0.05622 1.00000 0.03547 0.00000 0.00000 C7 0.34503 0.75297 -0.00831 1.00000 0.02472 0.02074 0.02813 -0.00074 0.00618 0.00564 0.02441 0.00442 0.00023 0.00014 0.00013 0.00000 0.00123 0.00117 0.00135 0.00097 0.00100 0.00102 0.00052 H7 0.28906 0.74899 -0.04683 1.00000 0.02930 0.00000 0.00000 C8 0.74018 0.84487 0.08476 1.00000 0.02188 0.03687 0.13003 0.00852 -0.01704 -0.00085 0.06333 0.00607 0.00027 0.00020 0.00022 0.00000 0.00151 0.00176 0.00356 0.00196 0.00182 0.00138 0.00111 H8A 0.70345 0.87135 0.12437 1.00000 0.09499 0.00000 0.00000 H8B 0.81221 0.87679 0.07025 1.00000 0.09499 0.00000 0.00000 H8C 0.76737 0.78938 0.09729 1.00000 0.09499 0.00000 0.00000 C9 0.06050 0.63018 0.44292 1.00000 0.02593 0.05170 0.03000 -0.01684 0.00522 0.00833 0.03579 0.00482 0.00024 0.00018 0.00014 0.00000 0.00136 0.00178 0.00150 0.00125 0.00112 0.00126 0.00066 H9A 0.04003 0.68160 0.41924 1.00000 0.05368 0.00000 0.00000 H9B 0.06423 0.63965 0.49244 1.00000 0.05368 0.00000 0.00000 H9C -0.00396 0.58926 0.43180 1.00000 0.05368 0.00000 0.00000 C10 0.35929 0.55333 0.34313 1.00000 0.02015 0.02121 0.02090 -0.00220 -0.00092 0.00114 0.02078 0.00390 0.00021 0.00014 0.00012 0.00000 0.00114 0.00115 0.00123 0.00092 0.00093 0.00096 0.00049 C11 0.42933 0.55764 0.28445 1.00000 0.02712 0.04106 0.01840 0.00442 -0.00148 0.00444 0.02891 0.00454 0.00023 0.00016 0.00012 0.00000 0.00130 0.00154 0.00128 0.00107 0.00101 0.00117 0.00057 H11 0.39264 0.57998 0.24369 1.00000 0.03469 0.00000 0.00000 C12 0.55063 0.53012 0.28444 1.00000 0.02746 0.04408 0.02210 0.00432 0.00668 0.00451 0.03109 0.00469 0.00023 0.00017 0.00013 0.00000 0.00132 0.00159 0.00133 0.00112 0.00104 0.00122 0.00059 H12 0.59755 0.53426 0.24415 1.00000 0.03731 0.00000 0.00000 C13 0.60458 0.49617 0.34361 1.00000 0.01947 0.01996 0.02625 0.00019 0.00143 -0.00011 0.02188 0.00404 0.00021 0.00014 0.00012 0.00000 0.00115 0.00114 0.00129 0.00095 0.00095 0.00096 0.00049 C14 0.53570 0.48975 0.40206 1.00000 0.02507 0.02464 0.02199 0.00478 -0.00296 0.00137 0.02398 0.00413 0.00022 0.00014 0.00012 0.00000 0.00124 0.00125 0.00129 0.00096 0.00099 0.00103 0.00052 H14 0.57175 0.46595 0.44239 1.00000 0.02877 0.00000 0.00000 C15 0.41340 0.51834 0.40136 1.00000 0.02396 0.02860 0.01995 0.00111 0.00385 -0.00079 0.02410 0.00413 0.00022 0.00015 0.00012 0.00000 0.00122 0.00129 0.00125 0.00097 0.00096 0.00105 0.00051 H15 0.36615 0.51380 0.44150 1.00000 0.02892 0.00000 0.00000 C16 0.78632 0.43947 0.39899 1.00000 0.02430 0.03787 0.04810 0.01754 -0.00258 0.00608 0.03683 0.00522 0.00024 0.00018 0.00015 0.00000 0.00133 0.00156 0.00178 0.00130 0.00121 0.00120 0.00067 H16A 0.78381 0.48005 0.43587 1.00000 0.05525 0.00000 0.00000 H16B 0.87345 0.42652 0.38950 1.00000 0.05525 0.00000 0.00000 H16C 0.74315 0.38953 0.41293 1.00000 0.05525 0.00000 0.00000 C17 -0.18802 0.66809 0.30997 1.00000 0.02345 0.01582 0.03601 0.00089 0.00598 0.00126 0.02499 0.00430 0.00022 0.00014 0.00013 0.00000 0.00124 0.00112 0.00146 0.00100 0.00105 0.00100 0.00053 H17 -0.18826 0.60995 0.31225 1.00000 0.02998 0.00000 0.00000 C18 -0.25676 0.71131 0.35662 1.00000 0.02019 0.01931 0.03446 0.00499 0.00951 0.00179 0.02447 0.00432 0.00021 0.00014 0.00013 0.00000 0.00118 0.00117 0.00143 0.00100 0.00103 0.00098 0.00053 H18 -0.30251 0.68291 0.39007 1.00000 0.02937 0.00000 0.00000 C19 -0.25869 0.79605 0.35443 1.00000 0.01388 0.01917 0.02229 0.00230 0.00021 0.00271 0.01846 0.00388 0.00020 0.00013 0.00012 0.00000 0.00105 0.00111 0.00121 0.00090 0.00088 0.00091 0.00046 C20 -0.19121 0.83344 0.30372 1.00000 0.02937 0.01509 0.02647 0.00134 0.00457 0.00222 0.02357 0.00420 0.00022 0.00014 0.00012 0.00000 0.00130 0.00110 0.00132 0.00094 0.00102 0.00101 0.00051 H20 -0.19142 0.89142 0.29944 1.00000 0.02828 0.00000 0.00000 C21 -0.12361 0.78610 0.25940 1.00000 0.02804 0.01915 0.02364 0.00280 0.00561 0.00008 0.02351 0.00415 0.00022 0.00014 0.00012 0.00000 0.00128 0.00116 0.00129 0.00093 0.00101 0.00101 0.00051 H21 -0.07659 0.81291 0.22560 1.00000 0.02821 0.00000 0.00000 C22 -0.33162 0.84628 0.40403 1.00000 0.01926 0.01875 0.02229 0.00110 0.00245 0.00159 0.02006 0.00404 0.00021 0.00014 0.00012 0.00000 0.00114 0.00111 0.00123 0.00091 0.00092 0.00095 0.00048 H22A -0.27982 0.89307 0.42022 1.00000 0.02407 0.00000 0.00000 H22B -0.35069 0.81216 0.44425 1.00000 0.02407 0.00000 0.00000 C23 -0.45405 0.87875 0.37146 1.00000 0.02048 0.02316 0.02191 -0.00142 0.00131 0.00518 0.02184 0.00414 0.00022 0.00014 0.00012 0.00000 0.00116 0.00119 0.00124 0.00094 0.00095 0.00099 0.00050 H23A -0.43567 0.91119 0.33019 1.00000 0.02620 0.00000 0.00000 H23B -0.50790 0.83210 0.35718 1.00000 0.02620 0.00000 0.00000 C24 -0.52305 0.93239 0.42212 1.00000 0.02101 0.01977 0.02167 -0.00099 0.00060 0.00325 0.02082 0.00405 0.00021 0.00014 0.00012 0.00000 0.00116 0.00113 0.00124 0.00091 0.00094 0.00096 0.00049 H24A -0.54584 0.89829 0.46170 1.00000 0.02498 0.00000 0.00000 H24B -0.46546 0.97572 0.43930 1.00000 0.02498 0.00000 0.00000 C25 -0.63964 0.97235 0.39269 1.00000 0.01992 0.01861 0.01561 0.00044 0.00431 0.00191 0.01797 0.00389 0.00020 0.00013 0.00011 0.00000 0.00112 0.00110 0.00113 0.00086 0.00087 0.00094 0.00046 C26 -0.72992 0.92969 0.35448 1.00000 0.02192 0.01750 0.02950 0.00021 0.00073 0.00072 0.02297 0.00413 0.00021 0.00014 0.00012 0.00000 0.00120 0.00112 0.00134 0.00095 0.00099 0.00098 0.00050 H26 -0.72028 0.87265 0.34658 1.00000 0.02757 0.00000 0.00000 C27 -0.83366 0.97043 0.32804 1.00000 0.02098 0.01918 0.02907 0.00020 0.00008 -0.00265 0.02309 0.00418 0.00022 0.00014 0.00013 0.00000 0.00117 0.00115 0.00135 0.00096 0.00098 0.00099 0.00051 H27 -0.89316 0.94018 0.30128 1.00000 0.02771 0.00000 0.00000 C29 -0.76834 1.09083 0.37544 1.00000 0.03105 0.01866 0.03444 -0.00434 -0.00723 0.00699 0.02822 0.00425 0.00023 0.00015 0.00013 0.00000 0.00136 0.00120 0.00149 0.00104 0.00111 0.00110 0.00056 H29 -0.78142 1.14748 0.38380 1.00000 0.03387 0.00000 0.00000 C30 -0.66128 1.05503 0.40243 1.00000 0.02684 0.02212 0.02803 -0.00693 -0.00640 0.00204 0.02582 0.00420 0.00023 0.00015 0.00013 0.00000 0.00127 0.00121 0.00136 0.00100 0.00103 0.00105 0.00053 H30 -0.60215 1.08718 0.42780 1.00000 0.03098 0.00000 0.00000 N1 -0.12150 0.70412 0.26201 1.00000 0.01697 0.01881 0.02506 -0.00068 0.00266 0.00115 0.02024 0.00328 0.00017 0.00011 0.00010 0.00000 0.00094 0.00096 0.00109 0.00078 0.00079 0.00079 0.00041 N2 -0.85483 1.05031 0.33813 1.00000 0.01909 0.01971 0.02344 -0.00010 0.00019 0.00084 0.02076 0.00330 0.00017 0.00011 0.00010 0.00000 0.00096 0.00098 0.00106 0.00079 0.00080 0.00081 0.00041 O1 0.12829 0.65182 -0.01491 1.00000 0.02559 0.03921 0.02221 -0.00382 -0.00055 -0.00323 0.02903 0.00288 0.00015 0.00011 0.00008 0.00000 0.00091 0.00102 0.00092 0.00076 0.00072 0.00080 0.00039 O2 0.64889 0.84061 0.02978 1.00000 0.02116 0.03212 0.07926 -0.00984 0.01123 -0.00469 0.04398 0.00346 0.00016 0.00012 0.00012 0.00000 0.00096 0.00106 0.00161 0.00101 0.00098 0.00084 0.00053 O3 0.18069 0.60063 0.42114 1.00000 0.02273 0.04043 0.02145 -0.00927 -0.00042 0.00491 0.02823 0.00289 0.00015 0.00011 0.00008 0.00000 0.00087 0.00102 0.00091 0.00075 0.00069 0.00079 0.00039 O4 0.72594 0.47199 0.33878 1.00000 0.02021 0.03262 0.03543 0.00780 0.00416 0.00517 0.02935 0.00312 0.00015 0.00011 0.00009 0.00000 0.00085 0.00097 0.00104 0.00077 0.00073 0.00077 0.00040 P1 0.16674 0.66545 0.06394 1.00000 0.01905 0.02132 0.02048 0.00005 0.00175 0.00083 0.02026 0.00105 0.00006 0.00004 0.00003 0.00000 0.00030 0.00030 0.00032 0.00024 0.00023 0.00025 0.00013 P2 0.20249 0.59246 0.34073 1.00000 0.02013 0.02308 0.01931 -0.00482 -0.00212 0.00257 0.02090 0.00103 0.00006 0.00004 0.00003 0.00000 0.00030 0.00031 0.00031 0.00024 0.00024 0.00025 0.00014 S1 0.04157 0.73843 0.10764 1.00000 0.02049 0.02128 0.02618 0.00423 0.00598 0.00345 0.02254 0.00108 0.00005 0.00004 0.00003 0.00000 0.00029 0.00029 0.00032 0.00023 0.00023 0.00024 0.00013 S2 0.19032 0.56037 0.11433 1.00000 0.02832 0.01882 0.03075 0.00143 0.00633 0.00370 0.02585 0.00112 0.00006 0.00004 0.00003 0.00000 0.00033 0.00029 0.00035 0.00024 0.00026 0.00025 0.00014 S3 0.07942 0.51170 0.30053 1.00000 0.02249 0.01989 0.02174 -0.00142 -0.00188 -0.00011 0.02143 0.00099 0.00005 0.00003 0.00003 0.00000 0.00029 0.00029 0.00031 0.00022 0.00023 0.00024 0.00013 S4 0.19753 0.70022 0.29331 1.00000 0.02750 0.01940 0.03636 -0.00235 -0.00844 0.00012 0.02795 0.00105 0.00006 0.00004 0.00003 0.00000 0.00033 0.00029 0.00037 0.00025 0.00027 0.00026 0.00015 Cd1 0.02934 0.62460 0.20523 1.00000 0.01620 0.01797 0.01987 -0.00020 0.00060 0.00036 0.01801 0.00028 0.00001 0.00001 0.00001 0.00000 0.00010 0.00010 0.00010 0.00006 0.00006 0.00007 0.00007 Final Structure Factor Calculation for 2005slh0413 in P2(1)/c Total number of l.s. parameters = 384 Maximum vector length = 511 Memory required = 4491 / 26061 wR2 = 0.0727 before cycle 7 for 7757 data and 0 / 384 parameters GooF = S = 1.022; Restrained GooF = 1.022 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0294 * P )^2 + 1.97 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0311 for 6284 Fo > 4sig(Fo) and 0.0461 for all 7757 data wR2 = 0.0727, GooF = S = 1.022, Restrained GooF = 1.022 for all data Occupancy sum of asymmetric unit = 42.00 for non-hydrogen and 34.00 for hydrogen atoms Principal mean square atomic displacements U 0.0678 0.0467 0.0190 C1 0.0275 0.0230 0.0151 C2 0.0368 0.0290 0.0261 C3 0.0508 0.0325 0.0199 C4 0.0599 0.0221 0.0134 C5 0.0478 0.0229 0.0180 C6 0.0326 0.0252 0.0154 C7 0.1348 0.0361 0.0191 C8 0.0618 0.0309 0.0146 C9 0.0242 0.0194 0.0187 C10 0.0429 0.0271 0.0168 C11 0.0465 0.0287 0.0181 C12 0.0263 0.0200 0.0193 C13 0.0289 0.0262 0.0168 C14 0.0288 0.0256 0.0179 C15 0.0613 0.0315 0.0177 C16 0.0377 0.0216 0.0156 C17 0.0396 0.0181 0.0157 C18 0.0236 0.0192 0.0126 C19 0.0322 0.0238 0.0147 C20 0.0312 0.0221 0.0173 C21 0.0236 0.0192 0.0174 C22 0.0273 0.0221 0.0161 C23 0.0240 0.0216 0.0169 C24 0.0228 0.0179 0.0132 C25 0.0295 0.0220 0.0174 C26 0.0292 0.0228 0.0173 C27 0.0440 0.0252 0.0155 C29 0.0378 0.0227 0.0169 C30 0.0255 0.0194 0.0159 N1 0.0235 0.0203 0.0185 N2 0.0406 0.0259 0.0206 O1 0.0827 0.0307 0.0186 O2 0.0454 0.0218 0.0175 O3 0.0433 0.0265 0.0183 O4 0.0217 0.0208 0.0182 P1 0.0282 0.0186 0.0159 P2 0.0318 0.0189 0.0169 S1 0.0356 0.0244 0.0175 S2 0.0250 0.0208 0.0185 S3 0.0428 0.0222 0.0188 S4 0.0199 0.0180 0.0161 Cd1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.020 0.038 0.058 0.080 0.103 0.133 0.166 0.211 0.283 1.000 Number in group 823. 733. 784. 762. 784. 791. 762. 769. 776. 773. GooF 0.928 1.021 1.089 1.082 1.029 1.017 1.018 0.982 0.996 1.056 K 1.068 0.899 0.921 0.942 0.969 0.977 0.986 1.007 1.018 1.012 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.32 1.64 inf Number in group 789. 779. 766. 766. 780. 792. 757. 786. 760. 782. GooF 1.028 0.914 0.985 0.974 0.951 0.964 0.977 0.994 0.974 1.380 K 0.966 0.996 0.996 1.010 1.007 1.016 1.027 1.029 1.014 0.990 R1 0.120 0.089 0.079 0.064 0.051 0.039 0.033 0.028 0.021 0.022 Recommended weighting scheme: WGHT 0.0291 1.9894 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 4 0 2674.55 3294.95 4.73 0.200 4.08 0 8 0 4350.80 5329.03 4.65 0.255 2.04 1 9 0 503.57 337.92 4.55 0.064 1.79 -5 16 10 1598.49 2235.66 4.51 0.165 0.84 -4 3 6 309.56 132.42 4.49 0.040 1.96 0 1 5 1072.31 842.22 4.13 0.101 3.80 -4 1 10 56.55 149.75 4.10 0.043 1.59 -2 0 6 3656.82 3032.56 4.03 0.192 2.82 -1 8 2 7500.50 8688.84 4.03 0.325 1.97 -3 8 6 82.95 174.17 4.00 0.046 1.57 -2 6 3 964.01 1212.37 3.99 0.122 2.28 -4 2 1 1503.56 1823.56 3.96 0.149 2.53 -3 4 6 2752.68 3250.56 3.81 0.199 2.10 0 4 3 210.74 130.87 3.76 0.040 3.46 3 6 6 36.36 104.28 3.75 0.036 1.79 3 0 6 1692.41 1369.72 3.74 0.129 2.37 4 0 4 1314.33 1666.64 3.65 0.142 2.32 3 0 20 897.39 1404.33 3.64 0.131 0.93 3 5 1 416.41 312.75 3.35 0.062 2.38 3 4 7 1794.77 2096.93 3.27 0.160 1.91 -2 5 8 5632.20 4948.80 3.26 0.246 1.85 2 6 6 422.18 550.22 3.22 0.082 1.93 -3 16 11 17.14 186.25 3.17 0.048 0.86 1 10 2 196.83 113.09 3.16 0.037 1.59 -3 4 9 67.11 140.75 3.14 0.041 1.71 2 3 8 786.85 634.13 3.14 0.088 2.04 2 10 0 47.05 9.55 3.08 0.011 1.56 3 12 8 -4.25 62.70 3.05 0.028 1.12 2 6 8 137.14 221.61 3.05 0.052 1.71 -2 4 10 82.74 161.19 3.05 0.044 1.69 -11 7 4 870.17 1108.95 3.04 0.116 0.89 -4 1 18 -29.66 149.33 3.02 0.043 1.02 6 15 10 3134.03 2407.23 3.02 0.171 0.83 3 8 3 67.16 27.33 3.00 0.018 1.70 0 5 22 88.79 233.49 3.00 0.053 0.86 5 9 13 233.35 363.27 2.98 0.067 1.01 4 2 1 7932.10 8844.81 2.98 0.328 2.51 2 0 8 1996.64 1663.32 2.98 0.142 2.20 -1 4 12 397.78 522.10 2.96 0.080 1.50 3 3 6 4297.27 4848.63 2.94 0.243 2.17 -3 7 9 153.15 233.90 2.93 0.053 1.46 2 8 3 352.52 458.16 2.93 0.075 1.82 -1 9 3 5976.75 6673.29 2.93 0.285 1.73 5 6 2 2281.62 2675.69 2.93 0.181 1.65 4 5 20 19.49 184.27 2.92 0.047 0.88 3 3 9 270.24 373.71 2.92 0.067 1.73 -3 1 5 5163.73 5781.71 2.91 0.265 2.64 1 12 16 998.27 1269.59 2.91 0.124 0.90 5 5 3 2467.18 2159.40 2.90 0.162 1.71 0 1 3 17.88 65.45 2.89 0.028 6.05 Bond lengths and angles C1 - Distance Angles O1 1.4405 (0.0031) H1A 0.9800 109.47 H1B 0.9800 109.47 109.47 H1C 0.9800 109.47 109.47 109.47 C1 - O1 H1A H1B C2 - Distance Angles C3 1.3859 (0.0034) C7 1.3990 (0.0033) 118.76 (0.23) P1 1.8003 (0.0024) 119.47 (0.19) 121.75 (0.18) C2 - C3 C7 C3 - Distance Angles C2 1.3859 (0.0034) C4 1.3928 (0.0036) 121.14 (0.25) H3 0.9500 119.43 119.43 C3 - C2 C4 C4 - Distance Angles C5 1.3871 (0.0040) C3 1.3928 (0.0036) 119.03 (0.25) H4 0.9500 120.49 120.49 C4 - C5 C3 C5 - Distance Angles O2 1.3776 (0.0030) C6 1.3818 (0.0038) 115.08 (0.25) C4 1.3871 (0.0040) 124.38 (0.26) 120.54 (0.24) C5 - O2 C6 C6 - Distance Angles C7 1.3812 (0.0034) C5 1.3818 (0.0038) 120.10 (0.25) H6 0.9500 119.95 119.95 C6 - C7 C5 C7 - Distance Angles C6 1.3812 (0.0034) C2 1.3990 (0.0033) 120.42 (0.24) H7 0.9500 119.79 119.79 C7 - C6 C2 C8 - Distance Angles O2 1.4317 (0.0039) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - O2 H8A H8B C9 - Distance Angles O3 1.4507 (0.0029) H9A 0.9800 109.47 H9B 0.9800 109.47 109.47 H9C 0.9800 109.47 109.47 109.47 C9 - O3 H9A H9B C10 - Distance Angles C15 1.3842 (0.0032) C11 1.3921 (0.0033) 118.44 (0.22) P2 1.7956 (0.0023) 122.35 (0.18) 119.20 (0.18) C10 - C15 C11 C11 - Distance Angles C12 1.3743 (0.0034) C10 1.3921 (0.0033) 121.14 (0.23) H11 0.9500 119.43 119.43 C11 - C12 C10 C12 - Distance Angles C11 1.3743 (0.0034) C13 1.3917 (0.0034) 119.85 (0.23) H12 0.9500 120.08 120.08 C12 - C11 C13 C13 - Distance Angles O4 1.3642 (0.0027) C14 1.3832 (0.0033) 124.68 (0.21) C12 1.3917 (0.0034) 115.41 (0.21) 119.91 (0.22) C13 - O4 C14 C14 - Distance Angles C13 1.3832 (0.0033) C15 1.3900 (0.0032) 119.54 (0.22) H14 0.9500 120.23 120.23 C14 - C13 C15 C15 - Distance Angles C10 1.3842 (0.0032) C14 1.3900 (0.0032) 121.10 (0.22) H15 0.9500 119.45 119.45 C15 - C10 C14 C16 - Distance Angles O4 1.4274 (0.0030) H16A 0.9800 109.47 H16B 0.9800 109.47 109.47 H16C 0.9800 109.47 109.47 109.47 C16 - O4 H16A H16B C17 - Distance Angles N1 1.3320 (0.0030) C18 1.3833 (0.0032) 123.12 (0.21) H17 0.9500 118.44 118.44 C17 - N1 C18 C18 - Distance Angles C17 1.3833 (0.0033) C19 1.3838 (0.0031) 119.80 (0.21) H18 0.9500 120.10 120.10 C18 - C17 C19 C19 - Distance Angles C18 1.3838 (0.0031) C20 1.3866 (0.0031) 117.02 (0.21) C22 1.5065 (0.0030) 122.11 (0.20) 120.87 (0.20) C19 - C18 C20 C20 - Distance Angles C21 1.3824 (0.0032) C19 1.3866 (0.0031) 119.81 (0.21) H20 0.9500 120.10 120.10 C20 - C21 C19 C21 - Distance Angles N1 1.3392 (0.0028) C20 1.3824 (0.0032) 122.90 (0.22) H21 0.9500 118.55 118.55 C21 - N1 C20 C22 - Distance Angles C19 1.5065 (0.0030) C23 1.5338 (0.0031) 111.98 (0.18) H22A 0.9900 109.22 109.22 H22B 0.9900 109.22 109.22 107.91 C22 - C19 C23 H22A C23 - Distance Angles C24 1.5294 (0.0031) C22 1.5338 (0.0031) 110.66 (0.19) H23A 0.9900 109.51 109.51 H23B 0.9900 109.51 109.51 108.08 C23 - C24 C22 H23A C24 - Distance Angles C25 1.5065 (0.0031) C23 1.5294 (0.0031) 114.32 (0.19) H24A 0.9900 108.68 108.68 H24B 0.9900 108.68 108.68 107.61 C24 - C25 C23 H24A C25 - Distance Angles C30 1.3834 (0.0031) C26 1.3899 (0.0032) 116.48 (0.21) C24 1.5065 (0.0031) 120.67 (0.20) 122.85 (0.20) C25 - C30 C26 C26 - Distance Angles C27 1.3811 (0.0032) C25 1.3899 (0.0032) 119.85 (0.21) H26 0.9500 120.08 120.08 C26 - C27 C25 C27 - Distance Angles N2 1.3389 (0.0029) C26 1.3811 (0.0032) 123.47 (0.22) H27 0.9500 118.26 118.26 C27 - N2 C26 C29 - Distance Angles N2 1.3359 (0.0030) C30 1.3770 (0.0033) 123.62 (0.21) H29 0.9500 118.19 118.19 C29 - N2 C30 C30 - Distance Angles C29 1.3770 (0.0033) C25 1.3834 (0.0031) 120.15 (0.22) H30 0.9500 119.93 119.93 C30 - C29 C25 N1 - Distance Angles C17 1.3320 (0.0030) C21 1.3392 (0.0028) 117.33 (0.20) Cd1 2.3744 (0.0018) 118.33 (0.14) 122.63 (0.15) N1 - C17 C21 N2 - Distance Angles C29 1.3359 (0.0030) C27 1.3389 (0.0029) 116.41 (0.20) Cd1_$2 2.3623 (0.0019) 117.95 (0.15) 125.63 (0.15) N2 - C29 C27 O1 - Distance Angles C1 1.4405 (0.0031) P1 1.5987 (0.0017) 119.74 (0.17) O1 - C1 O2 - Distance Angles C5 1.3776 (0.0030) C8 1.4317 (0.0039) 117.50 (0.25) O2 - C5 O3 - Distance Angles C9 1.4507 (0.0029) P2 1.6023 (0.0018) 118.27 (0.16) O3 - C9 O4 - Distance Angles C13 1.3642 (0.0027) C16 1.4274 (0.0030) 117.27 (0.19) O4 - C13 P1 - Distance Angles O1 1.5987 (0.0017) C2 1.8003 (0.0024) 99.14 (0.10) S2 1.9902 (0.0008) 112.47 (0.07) 111.16 (0.08) S1 2.0042 (0.0008) 109.78 (0.07) 111.44 (0.08) 112.16 (0.04) P1 - O1 C2 S2 P2 - Distance Angles O3 1.6023 (0.0018) C10 1.7956 (0.0023) 99.71 (0.10) S4 1.9880 (0.0009) 112.42 (0.07) 109.76 (0.08) S3 2.0067 (0.0008) 108.96 (0.07) 112.25 (0.08) 113.01 (0.04) P2 - O3 C10 S4 S1 - Distance Angles P1 2.0042 (0.0008) Cd1 2.6692 (0.0006) 86.54 (0.03) S1 - P1 S2 - Distance Angles P1 1.9902 (0.0008) Cd1 2.7241 (0.0006) 85.31 (0.03) S2 - P1 S3 - Distance Angles P2 2.0067 (0.0008) Cd1 2.6632 (0.0006) 86.26 (0.03) S3 - P2 S4 - Distance Angles P2 1.9880 (0.0009) Cd1 2.7454 (0.0006) 84.39 (0.03) S4 - P2 Cd1 - Distance Angles N2_$1 2.3623 (0.0019) N1 2.3744 (0.0018) 84.63 (0.06) S3 2.6632 (0.0006) 92.04 (0.05) 100.14 (0.05) S1 2.6692 (0.0006) 99.02 (0.05) 90.18 (0.05) 165.56 (0.02) S2 2.7241 (0.0006) 94.47 (0.05) 165.70 (0.05) 94.16 (0.02) 75.84 (0.02) S4 2.7454 (0.0006) 162.12 (0.05) 84.46 (0.05) 76.02 (0.02) 95.13 (0.02) 99.57 (0.02) Cd1 - N2_$1 N1 S3 S1 S2 FMAP and GRID set by program FMAP 2 3 24 GRID -1.190 -2 -2 1.190 2 2 R1 = 0.0454 for 7757 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.65 at 0.0904 0.1238 0.1166 [ 1.42 A from H9C ] Deepest hole -0.85 at -0.0029 0.6267 0.1640 [ 0.87 A from CD1 ] Mean = 0.00, Rms deviation from mean = 0.08 e/A^3, Highest memory used = 4398 / 30687 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 -0.0904 0.6238 0.3834 1.00000 0.05 0.65 1.42 H9C 1.73 H17 1.81 H9A 1.89 C17 Q2 1 -0.0326 0.6258 0.2944 1.00000 0.05 0.50 1.70 N1 1.73 H17 1.84 C17 1.88 CD1 Q3 1 0.1018 0.6214 0.1177 1.00000 0.05 0.41 1.38 S2 1.47 P1 1.90 CD1 2.02 S1 Q4 1 -0.0811 0.7440 0.2033 1.00000 0.05 0.40 1.21 H21 1.38 C21 1.40 N1 2.28 CD1 Q5 1 -0.0989 0.7617 -0.0128 1.00000 0.05 0.39 1.76 H1C 2.23 H9A 2.38 H9B 2.60 C1 Shortest distances between peaks (including symmetry equivalents) 1 2 1.87 2 4 2.67 1 5 2.76 Time profile in seconds ----------------------- 0.06: 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. 1.80: 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 9.75: Structure factors and derivatives 20.88: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.01: Apply other restraints 1.21: Solve l.s. equations 0.00: Generate HTAB table 0.06: Other dependent quantities, CIF, tables 0.38: Analysis of variance 0.13: Merge reflections for Fourier and .fcf 0.12: Fourier summations 0.17: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2005slh0413 finished at 11:34:44 Total CPU time: 34.6 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++