+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 23:19:14 on 13-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh051 in P-1 CELL 0.71073 5.5061 7.2607 11.4567 103.709 93.064 100.528 ZERR 2.00 0.0002 0.0003 0.0005 0.002 0.003 0.003 LATT 1 SFAC C H N O UNIT 20 22 2 4 V = 435.23 F(000) = 188.0 Mu = 0.09 mm-1 Cell Wt = 354.40 Rho = 1.352 MERG 0 OMIT -3.00 55.00 OMIT 3 -8 1 OMIT -2 1 -1 FMAP 2 PLAN 5 SIZE 0.64 0.46 0.04 EQIV $1 -x, -y+1, -z+1 HTAB N1 O2_$1 HTAB ACTA BOND $H L.S. 16 TEMP -153.00 WGHT 0.053700 0.433200 BASF 0.36660 FVAR 1.06077 C1 1 0.269786 0.541662 0.259942 11.00000 0.01420 0.01533 = 0.01287 0.00473 0.00321 0.00481 C2 1 0.270634 0.597922 0.385577 11.00000 0.01436 0.01532 = 0.01529 0.00577 0.00516 0.00398 AFIX 43 H2 2 0.128575 0.553020 0.422330 11.00000 -1.20000 AFIX 0 C3 1 0.478213 0.719378 0.457396 11.00000 0.01652 0.01340 = 0.01330 0.00448 0.00215 0.00624 C4 1 0.685582 0.786067 0.403452 11.00000 0.01389 0.01731 = 0.01495 0.00179 0.00344 0.00012 AFIX 43 H4 2 0.828721 0.867006 0.451727 11.00000 -1.20000 AFIX 0 C5 1 0.681932 0.733188 0.277740 11.00000 0.01720 0.02194 = 0.02003 0.00622 0.00812 0.00308 AFIX 43 H5 2 0.822030 0.781230 0.240789 11.00000 -1.20000 AFIX 0 C6 1 0.477155 0.611905 0.206463 11.00000 0.01838 0.01891 = 0.01139 0.00415 0.00537 0.00554 AFIX 43 H6 2 0.477547 0.576392 0.121164 11.00000 -1.20000 AFIX 0 C7 1 0.020351 0.314586 0.075464 11.00000 0.02191 0.02163 = 0.01397 0.00471 0.00258 0.00840 C8 1 -0.227907 0.180354 0.040019 11.00000 0.02439 0.02595 = 0.01713 0.00096 0.00075 0.00261 AFIX 137 H8A 2 -0.266641 0.150033 -0.047766 11.00000 -1.50000 H8B 2 -0.355650 0.242669 0.079847 11.00000 -1.50000 H8C 2 -0.223641 0.060652 0.064815 11.00000 -1.50000 AFIX 0 C9 1 0.468930 0.771114 0.591409 11.00000 0.01909 0.01552 = 0.01638 0.00579 0.00296 0.00640 C10 1 0.693628 0.892570 0.671783 11.00000 0.02311 0.01905 = 0.01656 0.00398 0.00049 0.00315 AFIX 137 H10A 2 0.717510 1.025383 0.662741 11.00000 -1.50000 H10B 2 0.840178 0.838809 0.649114 11.00000 -1.50000 H10C 2 0.669968 0.892854 0.755996 11.00000 -1.50000 AFIX 0 N1 3 0.055525 0.415041 0.194837 11.00000 0.01321 0.02142 = 0.01135 0.00279 0.00497 0.00097 AFIX 43 H1 2 -0.073355 0.397850 0.236126 11.00000 -1.20000 AFIX 0 O1 4 0.178397 0.327451 0.005658 11.00000 0.02820 0.03748 = 0.01503 0.00065 0.00921 0.00029 O2 4 0.276674 0.716198 0.634501 11.00000 0.02310 0.02830 = 0.01611 0.00378 0.00504 0.00268 HKLF 5 Covalent radii and connectivity table for 2008lsh051 in P-1 C 0.770 H 0.320 N 0.700 O 0.660 C1 - C6 C2 N1 C2 - C3 C1 C3 - C4 C2 C9 C4 - C3 C5 C5 - C6 C4 C6 - C5 C1 C7 - O1 N1 C8 C8 - C7 C9 - O2 C3 C10 C10 - C9 N1 - C7 C1 O1 - C7 O2 - C9 Operators for generating equivalent atoms: $1 -x, -y+1, -z+1 6451 Reflections read, of which 26 rejected -7 =< h =< 7, -9 =< k =< 9, -14 =< l =< 14, Max. 2-theta = 54.94 0 Systematic absence violations 0 Data suppressed, R(sigma) = 0.0396 Maximum memory for data reduction = 1392 / 80 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 = 1729 / 154280 wR2 = 0.1428 before cycle 1 for 6434 data and 121 / 121 parameters GooF = S = 1.092; Restrained GooF = 1.092 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0537 * P )^2 + 0.43 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.06077 0.00206 0.000 OSF 2 0.36660 0.00147 0.002 BASF 1 Mean shift/esd = 0.002 Maximum = -0.006 for U13 C8 Max. shift = 0.000 A for H8B Max. dU = 0.000 for C9 Least-squares cycle 2 Maximum vector length = 511 Memory required = 1729 / 154280 wR2 = 0.1428 before cycle 2 for 6434 data and 121 / 121 parameters GooF = S = 1.092; Restrained GooF = 1.092 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0537 * P )^2 + 0.43 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.06077 0.00206 0.000 OSF 2 0.36660 0.00147 0.001 BASF 1 Mean shift/esd = 0.001 Maximum = 0.005 for tors H8A Max. shift = 0.000 A for H8B Max. dU = 0.000 for C9 Least-squares cycle 3 Maximum vector length = 511 Memory required = 1729 / 154280 wR2 = 0.1428 before cycle 3 for 6434 data and 121 / 121 parameters GooF = S = 1.092; Restrained GooF = 1.092 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0537 * P )^2 + 0.43 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.06077 0.00206 0.000 OSF 2 0.36661 0.00147 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.003 for tors H8A Max. shift = 0.000 A for H8C Max. dU = 0.000 for O1 Least-squares cycle 4 Maximum vector length = 511 Memory required = 1729 / 154280 wR2 = 0.1428 before cycle 4 for 6434 data and 121 / 121 parameters GooF = S = 1.092; Restrained GooF = 1.092 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0537 * P )^2 + 0.43 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.06077 0.00206 0.000 OSF 2 0.36660 0.00147 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.002 for tors H8A Max. shift = 0.000 A for H8C Max. dU = 0.000 for O1 Least-squares cycle 5 Maximum vector length = 511 Memory required = 1729 / 154280 wR2 = 0.1428 before cycle 5 for 6434 data and 121 / 121 parameters GooF = S = 1.092; Restrained GooF = 1.092 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0537 * P )^2 + 0.43 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.06077 0.00206 0.001 OSF 2 0.36660 0.00147 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.001 for tors H8A Max. shift = 0.000 A for H8B Max. dU = 0.000 for C6 Least-squares cycle 6 Maximum vector length = 511 Memory required = 1729 / 154280 wR2 = 0.1428 before cycle 6 for 6434 data and 121 / 121 parameters GooF = S = 1.092; Restrained GooF = 1.092 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0537 * P )^2 + 0.43 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.06077 0.00206 0.000 OSF 2 0.36661 0.00147 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.001 for tors H8A Max. shift = 0.000 A for H8B Max. dU = 0.000 for N1 Least-squares cycle 7 Maximum vector length = 511 Memory required = 1729 / 154280 wR2 = 0.1428 before cycle 7 for 6434 data and 121 / 121 parameters GooF = S = 1.092; Restrained GooF = 1.092 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0537 * P )^2 + 0.43 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.06077 0.00206 0.000 OSF 2 0.36661 0.00147 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for tors H8A Max. shift = 0.000 A for H8C Max. dU = 0.000 for C4 Least-squares cycle 8 Maximum vector length = 511 Memory required = 1729 / 154280 wR2 = 0.1428 before cycle 8 for 6434 data and 121 / 121 parameters GooF = S = 1.092; Restrained GooF = 1.092 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0537 * P )^2 + 0.43 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.06077 0.00206 0.000 OSF 2 0.36661 0.00147 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for tors H8A Max. shift = 0.000 A for H8A Max. dU = 0.000 for C9 Least-squares cycle 9 Maximum vector length = 511 Memory required = 1729 / 154280 wR2 = 0.1428 before cycle 9 for 6434 data and 121 / 121 parameters GooF = S = 1.092; Restrained GooF = 1.092 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0537 * P )^2 + 0.43 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.06077 0.00206 0.000 OSF 2 0.36661 0.00147 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for z C9 Max. shift = 0.000 A for H8B Max. dU = 0.000 for C2 Least-squares cycle 10 Maximum vector length = 511 Memory required = 1729 / 154280 wR2 = 0.1428 before cycle 10 for 6434 data and 121 / 121 parameters GooF = S = 1.092; Restrained GooF = 1.092 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0537 * P )^2 + 0.43 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.06077 0.00206 0.000 OSF 2 0.36660 0.00147 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H8B Max. dU = 0.000 for C8 Least-squares cycle 11 Maximum vector length = 511 Memory required = 1729 / 154280 wR2 = 0.1428 before cycle 11 for 6434 data and 121 / 121 parameters GooF = S = 1.092; Restrained GooF = 1.092 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0537 * P )^2 + 0.43 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.06077 0.00206 0.000 OSF 2 0.36660 0.00147 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for z C9 Max. shift = 0.000 A for H8C Max. dU = 0.000 for C6 Least-squares cycle 12 Maximum vector length = 511 Memory required = 1729 / 154280 wR2 = 0.1428 before cycle 12 for 6434 data and 121 / 121 parameters GooF = S = 1.092; Restrained GooF = 1.092 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0537 * P )^2 + 0.43 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.06077 0.00206 0.000 OSF 2 0.36660 0.00147 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H8B Max. dU = 0.000 for C1 Least-squares cycle 13 Maximum vector length = 511 Memory required = 1729 / 154280 wR2 = 0.1428 before cycle 13 for 6434 data and 121 / 121 parameters GooF = S = 1.092; Restrained GooF = 1.092 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0537 * P )^2 + 0.43 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.06077 0.00206 0.000 OSF 2 0.36660 0.00147 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C5 Max. dU = 0.000 for O2 Least-squares cycle 14 Maximum vector length = 511 Memory required = 1729 / 154280 wR2 = 0.1428 before cycle 14 for 6434 data and 121 / 121 parameters GooF = S = 1.092; Restrained GooF = 1.092 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0537 * P )^2 + 0.43 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.06077 0.00206 0.000 OSF 2 0.36660 0.00147 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for z C9 Max. shift = 0.000 A for H10C Max. dU = 0.000 for N1 Least-squares cycle 15 Maximum vector length = 511 Memory required = 1729 / 154280 wR2 = 0.1428 before cycle 15 for 6434 data and 121 / 121 parameters GooF = S = 1.092; Restrained GooF = 1.092 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0537 * P )^2 + 0.43 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.06077 0.00206 0.000 OSF 2 0.36660 0.00147 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H10B Max. dU = 0.000 for C5 Least-squares cycle 16 Maximum vector length = 511 Memory required = 1729 / 154280 wR2 = 0.1428 before cycle 16 for 6434 data and 121 / 121 parameters GooF = S = 1.092; Restrained GooF = 1.092 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0537 * P )^2 + 0.43 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 1.06077 0.00206 0.000 OSF 2 0.36660 0.00147 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for C1 Max. dU = 0.000 for C5 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 17 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.1286 0.5530 0.4223 43 0.950 0.000 C2 C3 C1 H4 0.8287 0.8670 0.4517 43 0.950 0.000 C4 C3 C5 H5 0.8220 0.7812 0.2408 43 0.950 0.000 C5 C6 C4 H6 0.4775 0.5764 0.1212 43 0.950 0.000 C6 C5 C1 H8A -0.2666 0.1500 -0.0478 137 0.980 0.000 C8 C7 H8A H8B -0.3557 0.2427 0.0798 137 0.980 0.000 C8 C7 H8A H8C -0.2237 0.0607 0.0648 137 0.980 0.000 C8 C7 H8A H10A 0.7175 1.0254 0.6627 137 0.980 0.000 C10 C9 H10A H10B 0.8402 0.8388 0.6491 137 0.980 0.000 C10 C9 H10A H10C 0.6700 0.8928 0.7560 137 0.980 0.000 C10 C9 H10A H1 -0.0734 0.3978 0.2361 43 0.880 0.000 N1 C7 C1 2008lsh051 in P-1 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.26979 0.54166 0.25994 1.00000 0.01420 0.01533 0.01287 0.00473 0.00321 0.00481 0.01362 0.00312 0.00025 0.00021 0.00013 0.00000 0.00078 0.00084 0.00078 0.00066 0.00061 0.00068 0.00034 C2 0.27063 0.59792 0.38558 1.00000 0.01436 0.01532 0.01529 0.00577 0.00516 0.00398 0.01439 0.00323 0.00026 0.00021 0.00014 0.00000 0.00076 0.00083 0.00078 0.00064 0.00062 0.00066 0.00033 H2 0.12857 0.55302 0.42233 1.00000 0.01727 0.00000 0.00000 C3 0.47821 0.71938 0.45740 1.00000 0.01652 0.01340 0.01330 0.00448 0.00215 0.00624 0.01376 0.00307 0.00026 0.00020 0.00013 0.00000 0.00081 0.00080 0.00074 0.00066 0.00063 0.00067 0.00033 C4 0.68558 0.78607 0.40345 1.00000 0.01388 0.01731 0.01495 0.00179 0.00344 0.00012 0.01609 0.00330 0.00027 0.00022 0.00014 0.00000 0.00077 0.00085 0.00079 0.00068 0.00060 0.00065 0.00034 H4 0.82872 0.86701 0.45173 1.00000 0.01931 0.00000 0.00000 C5 0.68193 0.73319 0.27774 1.00000 0.01720 0.02195 0.02003 0.00622 0.00812 0.00308 0.01944 0.00354 0.00028 0.00024 0.00015 0.00000 0.00080 0.00092 0.00083 0.00073 0.00066 0.00073 0.00037 H5 0.82203 0.78123 0.24079 1.00000 0.02333 0.00000 0.00000 C6 0.47716 0.61191 0.20646 1.00000 0.01838 0.01891 0.01139 0.00415 0.00537 0.00554 0.01579 0.00314 0.00025 0.00021 0.00013 0.00000 0.00080 0.00090 0.00078 0.00071 0.00064 0.00071 0.00035 H6 0.47755 0.57639 0.12116 1.00000 0.01895 0.00000 0.00000 C7 0.02035 0.31459 0.07546 1.00000 0.02191 0.02163 0.01397 0.00471 0.00258 0.00840 0.01858 0.00347 0.00028 0.00024 0.00014 0.00000 0.00084 0.00087 0.00079 0.00069 0.00068 0.00072 0.00036 C8 -0.22791 0.18035 0.04002 1.00000 0.02439 0.02595 0.01713 0.00096 0.00074 0.00261 0.02363 0.00339 0.00028 0.00025 0.00015 0.00000 0.00089 0.00097 0.00086 0.00074 0.00068 0.00079 0.00039 H8A -0.26662 0.15001 -0.04777 1.00000 0.03544 0.00000 0.00000 H8B -0.35565 0.24268 0.07983 1.00000 0.03544 0.00000 0.00000 H8C -0.22365 0.06066 0.06483 1.00000 0.03544 0.00000 0.00000 C9 0.46893 0.77111 0.59141 1.00000 0.01909 0.01552 0.01638 0.00579 0.00296 0.00640 0.01626 0.00330 0.00028 0.00022 0.00013 0.00000 0.00081 0.00082 0.00083 0.00069 0.00064 0.00070 0.00035 C10 0.69363 0.89257 0.67178 1.00000 0.02311 0.01904 0.01656 0.00398 0.00049 0.00315 0.01986 0.00321 0.00026 0.00023 0.00014 0.00000 0.00083 0.00087 0.00082 0.00071 0.00069 0.00072 0.00036 H10A 0.71751 1.02538 0.66274 1.00000 0.02979 0.00000 0.00000 H10B 0.84018 0.83881 0.64911 1.00000 0.02979 0.00000 0.00000 H10C 0.66997 0.89285 0.75600 1.00000 0.02979 0.00000 0.00000 N1 0.05552 0.41504 0.19484 1.00000 0.01321 0.02142 0.01135 0.00279 0.00497 0.00097 0.01575 0.00258 0.00021 0.00018 0.00011 0.00000 0.00064 0.00072 0.00064 0.00058 0.00052 0.00056 0.00030 H1 -0.07335 0.39785 0.23613 1.00000 0.01890 0.00000 0.00000 O1 0.17840 0.32745 0.00566 1.00000 0.02820 0.03748 0.01503 0.00065 0.00921 0.00029 0.02849 0.00244 0.00020 0.00018 0.00010 0.00000 0.00068 0.00075 0.00063 0.00058 0.00055 0.00058 0.00031 O2 0.27667 0.71620 0.63450 1.00000 0.02310 0.02830 0.01611 0.00378 0.00504 0.00268 0.02302 0.00237 0.00019 0.00017 0.00010 0.00000 0.00060 0.00067 0.00060 0.00052 0.00048 0.00053 0.00028 Final Structure Factor Calculation for 2008lsh051 in P-1 Total number of l.s. parameters = 121 Maximum vector length = 511 Memory required = 1608 / 22995 wR2 = 0.1428 before cycle 17 for 6434 data and 0 / 121 parameters GooF = S = 1.092; Restrained GooF = 1.092 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0537 * P )^2 + 0.43 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0547 for 4879 Fo > 4sig(Fo) and 0.0867 for all 6434 data wR2 = 0.1428, GooF = S = 1.092, Restrained GooF = 1.092 for all data Occupancy sum of asymmetric unit = 13.00 for non-hydrogen and 11.00 for hydrogen atoms Principal mean square atomic displacements U 0.0168 0.0127 0.0114 C1 0.0185 0.0141 0.0106 C2 0.0180 0.0131 0.0102 C3 0.0223 0.0141 0.0119 C4 0.0249 0.0221 0.0113 C5 0.0204 0.0177 0.0092 C6 0.0252 0.0168 0.0137 C7 0.0303 0.0246 0.0160 C8 0.0205 0.0159 0.0124 C9 0.0239 0.0193 0.0163 C10 0.0242 0.0151 0.0079 N1 0.0476 0.0267 0.0111 O1 0.0315 0.0229 0.0146 O2 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.020 0.028 0.036 0.047 0.057 0.072 0.094 0.131 1.000 Number in group 666. 637. 647. 662. 662. 606. 648. 618. 641. 647. GooF 1.136 1.106 1.142 1.128 1.012 0.955 1.122 1.080 1.045 1.169 K 1.315 0.773 0.897 0.939 0.988 1.013 1.009 1.012 1.003 1.006 Resolution(A) 0.77 0.82 0.87 0.93 1.02 1.10 1.20 1.34 1.54 1.94 inf Number in group 648. 648. 635. 649. 635. 652. 679. 602. 637. 649. GooF 1.136 1.119 1.119 1.045 1.006 0.998 0.976 0.951 1.183 1.331 K 0.969 0.992 1.000 0.979 1.004 0.998 1.015 1.023 1.041 0.987 R1 0.224 0.172 0.135 0.108 0.072 0.062 0.058 0.053 0.052 0.043 Recommended weighting scheme: WGHT 0.0622 0.4173 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) -2 -1 -1 119.90 228.01 7.20 0.158 2.22 -4 2 1 4.81 30.77 7.00 0.058 1.34 2 -1 1 58.97 110.45 5.81 0.110 2.62 2 -1 1 63.79 110.45 5.25 0.110 2.62 2 -1 1 65.14 110.45 5.08 0.110 2.62 -3 0 3 188.51 282.89 5.03 0.176 1.68 1 0 0 114.67 171.67 4.54 0.137 5.39 1 -3 -1 34.11 63.11 4.29 0.083 2.16 -3 4 -13 -6.08 14.86 4.22 0.040 0.77 -1 2 5 93.20 61.46 4.13 0.082 1.69 1 0 0 119.76 171.67 4.11 0.137 5.39 1 0 0 121.57 171.67 3.95 0.137 5.39 -3 1 2 98.68 68.92 3.73 0.087 1.76 -4 -2 -4 30.64 51.55 3.67 0.075 1.02 2 -2 -1 4.90 0.42 3.65 0.007 2.28 0 7 6 16.01 1.38 3.59 0.012 0.79 2 -4 0 4.98 0.13 3.52 0.004 1.61 -4 1 -5 34.10 57.75 3.49 0.079 1.14 -1 0 0 127.56 171.67 3.44 0.137 5.39 -2 4 0 4.27 0.13 3.41 0.004 1.61 -4 2 -10 15.41 30.31 3.41 0.058 0.85 -3 -6 1 3.94 16.24 3.37 0.042 0.91 3 1 7 97.73 180.40 3.33 0.140 1.07 -6 -2 4 56.69 35.14 3.32 0.062 0.83 0 -8 0 -6.69 10.44 3.30 0.034 0.86 -2 6 -11 -0.12 8.41 3.26 0.030 0.85 -5 4 7 14.81 33.85 3.24 0.061 0.83 -3 8 2 -1.71 9.18 3.21 0.032 0.81 0 -4 0 7.29 1.73 3.18 0.014 1.73 -4 -4 -2 20.45 7.69 3.18 0.029 0.92 -2 0 9 16.37 5.86 3.18 0.025 1.16 0 2 13 22.35 7.65 3.16 0.029 0.78 5 -5 3 -3.89 7.31 3.15 0.028 0.94 -2 1 12 39.48 21.77 3.13 0.049 0.87 4 -1 1 7.47 0.20 3.12 0.005 1.36 -4 -3 0 10.71 23.00 3.09 0.050 1.07 1 8 -4 138.52 105.42 3.08 0.107 0.85 -2 -1 5 13.61 5.89 3.08 0.025 1.77 -6 1 6 -2.83 6.40 3.08 0.026 0.84 0 1 1 61.37 85.07 3.07 0.096 5.29 3 -1 -2 92.94 68.92 3.07 0.087 1.76 -1 7 -11 27.07 44.06 3.06 0.069 0.82 2 7 -5 -5.77 9.63 3.06 0.032 0.89 2 1 -4 24.70 39.75 3.06 0.066 1.97 2 -4 0 6.42 0.13 3.05 0.004 1.61 -4 1 7 85.08 60.95 3.04 0.082 1.07 -2 1 0 4.27 0.31 3.03 0.006 2.70 1 0 -8 58.90 40.63 3.02 0.067 1.37 0 0 -5 1128.57 939.58 3.01 0.321 2.21 -2 8 4 -4.17 5.84 3.01 0.025 0.79 Bond lengths and angles C1 - Distance Angles C6 1.3962 (0.0020) C2 1.3995 (0.0020) 119.30 (0.13) N1 1.4064 (0.0019) 123.85 (0.13) 116.85 (0.13) C1 - C6 C2 C2 - Distance Angles C3 1.3958 (0.0021) C1 1.3995 (0.0020) 120.63 (0.14) H2 0.9500 119.69 119.69 C2 - C3 C1 C3 - Distance Angles C4 1.3912 (0.0021) C2 1.3958 (0.0021) 119.65 (0.13) C9 1.4977 (0.0020) 122.38 (0.13) 117.96 (0.13) C3 - C4 C2 C4 - Distance Angles C3 1.3912 (0.0021) C5 1.3979 (0.0022) 119.56 (0.15) H4 0.9500 120.22 120.22 C4 - C3 C5 C5 - Distance Angles C6 1.3826 (0.0022) C4 1.3979 (0.0022) 120.88 (0.15) H5 0.9500 119.56 119.56 C5 - C6 C4 C6 - Distance Angles C5 1.3826 (0.0022) C1 1.3962 (0.0020) 119.95 (0.13) H6 0.9500 120.03 120.03 C6 - C5 C1 C7 - Distance Angles O1 1.2189 (0.0019) N1 1.3737 (0.0019) 123.48 (0.15) C8 1.4998 (0.0023) 122.89 (0.15) 113.58 (0.13) C7 - O1 N1 C8 - Distance Angles C7 1.4998 (0.0023) H8A 0.9800 109.47 H8B 0.9800 109.47 109.47 H8C 0.9800 109.47 109.47 109.47 C8 - C7 H8A H8B C9 - Distance Angles O2 1.2322 (0.0018) C3 1.4977 (0.0020) 119.92 (0.14) C10 1.5003 (0.0021) 120.66 (0.14) 119.41 (0.13) C9 - O2 C3 C10 - Distance Angles C9 1.5003 (0.0021) H10A 0.9800 109.47 H10B 0.9800 109.47 109.47 H10C 0.9800 109.47 109.47 109.47 C10 - C9 H10A H10B N1 - Distance Angles C7 1.3737 (0.0019) C1 1.4064 (0.0019) 128.72 (0.13) H1 0.8800 115.64 115.64 N1 - C7 C1 O1 - Distance Angles C7 1.2189 (0.0019) O1 - O2 - Distance Angles C9 1.2322 (0.0018) O2 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 2.13 2.9504(17) 153.9 N1-H1...O2_$1 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)