+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 19:50:05 on 18-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh010 in Pbca CELL 0.71073 11.9225 7.2026 17.4291 90.000 90.000 90.000 ZERR 8.00 0.0007 0.0002 0.0010 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N O UNIT 64 80 16 8 V = 1496.69 F(000) = 640.0 Mu = 0.09 mm-1 Cell Wt = 1201.44 Rho = 1.333 MERG 2 OMIT -3.00 55.00 OMIT 0 2 0 DFIX 0.88 0.02 N2 H2AN N2 H2BN DFIX 0.88 0.02 N1 H1N FMAP 2 PLAN 5 ACTA EQIV $1 x, -y+1/2, z+1/2 EQIV $2 x+1/2, y, -z+3/2 HTAB N2 O1_$1 HTAB N1 N2_$2 HTAB SIZE 0.12 0.08 0.08 BOND $H L.S. 16 TEMP -153.00 WGHT 0.0462 0.4555 FVAR 0.25498 C1 1 0.694069 0.258050 0.672813 11.00000 0.01712 0.02044 = 0.02138 -0.00046 0.00122 -0.00245 C2 1 0.588302 0.339311 0.665658 11.00000 0.01995 0.02108 = 0.02298 0.00389 -0.00380 -0.00314 AFIX 43 H2 2 0.559473 0.368047 0.616251 11.00000 -1.20000 AFIX 0 C3 1 0.525273 0.378141 0.730519 11.00000 0.01441 0.02146 = 0.02651 0.00180 -0.00125 -0.00127 AFIX 43 H3 2 0.453155 0.432640 0.725041 11.00000 -1.20000 AFIX 0 C4 1 0.566124 0.338400 0.803825 11.00000 0.01711 0.01852 = 0.02459 0.00088 0.00082 -0.00291 C5 1 0.670545 0.252539 0.810093 11.00000 0.01905 0.02164 = 0.02279 0.00306 -0.00258 -0.00195 AFIX 43 H5 2 0.698822 0.220822 0.859337 11.00000 -1.20000 AFIX 0 C6 1 0.733563 0.212933 0.745294 11.00000 0.01606 0.01989 = 0.02493 -0.00036 -0.00304 0.00017 AFIX 43 H6 2 0.804516 0.154295 0.750589 11.00000 -1.20000 AFIX 0 C7 1 0.738578 0.177247 0.537467 11.00000 0.02274 0.02156 = 0.02383 0.00186 -0.00059 0.00001 C8 1 0.837344 0.156823 0.483635 11.00000 0.02786 0.03571 = 0.02390 -0.00125 0.00058 0.00363 AFIX 137 H8A 2 0.818851 0.066941 0.443362 11.00000 -1.50000 H8B 2 0.902788 0.113014 0.512439 11.00000 -1.50000 H8C 2 0.854373 0.277284 0.460231 11.00000 -1.50000 AFIX 0 N1 3 0.766976 0.227402 0.609254 11.00000 0.01715 0.02722 = 0.02053 -0.00100 -0.00164 -0.00077 N2 3 0.501063 0.375850 0.869764 11.00000 0.01948 0.02966 = 0.02389 -0.00097 0.00160 0.00242 O1 4 0.640921 0.151395 0.516322 11.00000 0.02616 0.04223 = 0.02622 -0.00373 -0.00486 -0.00454 H2AN 2 0.463367 0.481380 0.867078 11.00000 0.04002 H2BN 2 0.543499 0.374303 0.911951 11.00000 0.03948 H1N 2 0.839615 0.243071 0.618335 11.00000 0.03666 HKLF 4 Covalent radii and connectivity table for 2008lsh010 in Pbca C 0.770 H 0.320 N 0.700 O 0.660 C1 - C6 C2 N1 C2 - C3 C1 C3 - C2 C4 C4 - C5 C3 N2 C5 - C6 C4 C6 - C5 C1 C7 - O1 N1 C8 C8 - C7 N1 - C7 C1 N2 - C4 O1 - C7 Operators for generating equivalent atoms: $1 x, -y+1/2, z+1/2 $2 x+1/2, y, -z+3/2 10907 Reflections read, of which 889 rejected -13 =< h =< 15, -9 =< k =< 8, -22 =< l =< 20, Max. 2-theta = 54.99 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 4 8 3 0.04 0.04 4 0.21 1 Inconsistent equivalents 1716 Unique reflections, of which 0 suppressed R(int) = 0.0834 R(sigma) = 0.0690 Friedel opposites merged Maximum memory for data reduction = 1344 / 17282 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 = 1646 / 145148 wR2 = 0.1240 before cycle 1 for 1716 data and 113 / 113 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.050 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0462 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25484 0.00080 -0.175 OSF Mean shift/esd = 0.130 Maximum = -0.392 for U33 C4 Max. shift = 0.006 A for H1N Max. dU = 0.002 for H2BN Least-squares cycle 2 Maximum vector length = 511 Memory required = 1646 / 145148 wR2 = 0.1238 before cycle 2 for 1716 data and 113 / 113 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.050; Restrained GooF = 1.049 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0462 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25477 0.00080 -0.081 OSF Mean shift/esd = 0.043 Maximum = 0.137 for U11 C8 Max. shift = 0.002 A for H1N Max. dU = 0.001 for H2BN Least-squares cycle 3 Maximum vector length = 511 Memory required = 1646 / 145148 wR2 = 0.1238 before cycle 3 for 1716 data and 113 / 113 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.050; Restrained GooF = 1.049 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0462 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25478 0.00080 0.003 OSF Mean shift/esd = 0.002 Maximum = -0.016 for z H1N Max. shift = 0.000 A for H1N Max. dU = 0.000 for H2BN Least-squares cycle 4 Maximum vector length = 511 Memory required = 1646 / 145148 wR2 = 0.1238 before cycle 4 for 1716 data and 113 / 113 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.050; Restrained GooF = 1.049 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0462 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25478 0.00080 0.006 OSF Mean shift/esd = 0.001 Maximum = 0.006 for OSF Max. shift = 0.000 A for H1N Max. dU = 0.000 for H2AN Least-squares cycle 5 Maximum vector length = 511 Memory required = 1646 / 145148 wR2 = 0.1238 before cycle 5 for 1716 data and 113 / 113 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.050; Restrained GooF = 1.049 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0462 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25478 0.00080 0.000 OSF Mean shift/esd = 0.000 Maximum = -0.001 for tors H8A Max. shift = 0.000 A for H8C Max. dU = 0.000 for H2AN Least-squares cycle 6 Maximum vector length = 511 Memory required = 1646 / 145148 wR2 = 0.1238 before cycle 6 for 1716 data and 113 / 113 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.050; Restrained GooF = 1.049 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0462 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25478 0.00080 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C3 Max. shift = 0.000 A for H2BN Max. dU = 0.000 for H2BN Least-squares cycle 7 Maximum vector length = 511 Memory required = 1646 / 145148 wR2 = 0.1238 before cycle 7 for 1716 data and 113 / 113 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.050; Restrained GooF = 1.049 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0462 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25478 0.00080 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for OSF Max. shift = 0.000 A for H1N Max. dU = 0.000 for H1N Least-squares cycle 8 Maximum vector length = 511 Memory required = 1646 / 145148 wR2 = 0.1238 before cycle 8 for 1716 data and 113 / 113 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.050; Restrained GooF = 1.049 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0462 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25478 0.00080 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O1 Max. shift = 0.000 A for H8B Max. dU = 0.000 for H2BN Least-squares cycle 9 Maximum vector length = 511 Memory required = 1646 / 145148 wR2 = 0.1238 before cycle 9 for 1716 data and 113 / 113 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.050; Restrained GooF = 1.049 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0462 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25478 0.00080 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C2 Max. shift = 0.000 A for C7 Max. dU = 0.000 for H2AN Least-squares cycle 10 Maximum vector length = 511 Memory required = 1646 / 145148 wR2 = 0.1238 before cycle 10 for 1716 data and 113 / 113 parameters Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.050; Restrained GooF = 1.049 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0462 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25478 0.00080 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C2 Max. shift = 0.000 A for H2BN Max. dU = 0.000 for H2AN Least-squares cycle 11 Maximum vector length = 511 Memory required = 1646 / 145148 wR2 = 0.1238 before cycle 11 for 1716 data and 113 / 113 parameters Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.050; Restrained GooF = 1.049 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0462 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25478 0.00080 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for x O1 Max. shift = 0.000 A for H1N Max. dU = 0.000 for H2AN Least-squares cycle 12 Maximum vector length = 511 Memory required = 1646 / 145148 wR2 = 0.1238 before cycle 12 for 1716 data and 113 / 113 parameters Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.050; Restrained GooF = 1.049 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0462 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25478 0.00080 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C2 Max. shift = 0.000 A for H2BN Max. dU = 0.000 for H2BN Least-squares cycle 13 Maximum vector length = 511 Memory required = 1646 / 145148 wR2 = 0.1238 before cycle 13 for 1716 data and 113 / 113 parameters Summary of restraints applied in cycle 13 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.050; Restrained GooF = 1.049 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0462 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25478 0.00080 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C3 Max. shift = 0.000 A for H2AN Max. dU = 0.000 for H2AN Least-squares cycle 14 Maximum vector length = 511 Memory required = 1646 / 145148 wR2 = 0.1238 before cycle 14 for 1716 data and 113 / 113 parameters Summary of restraints applied in cycle 14 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.050; Restrained GooF = 1.049 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0462 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25478 0.00080 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C3 Max. shift = 0.000 A for H2BN Max. dU = 0.000 for H1N Least-squares cycle 15 Maximum vector length = 511 Memory required = 1646 / 145148 wR2 = 0.1238 before cycle 15 for 1716 data and 113 / 113 parameters Summary of restraints applied in cycle 15 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.050; Restrained GooF = 1.049 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0462 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25478 0.00080 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C3 Max. shift = 0.000 A for H2AN Max. dU = 0.000 for H2AN Least-squares cycle 16 Maximum vector length = 511 Memory required = 1646 / 145148 wR2 = 0.1238 before cycle 16 for 1716 data and 113 / 113 parameters Summary of restraints applied in cycle 16 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.050; Restrained GooF = 1.049 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0462 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.25478 0.00080 0.000 OSF Mean shift/esd = 0.000 Maximum = 0.000 for z C2 Max. shift = 0.000 A for H2BN Max. dU = 0.000 for H2BN 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 0.5594 0.3678 0.6163 43 0.950 0.000 C2 C3 C1 H3 0.4532 0.4327 0.7251 43 0.950 0.000 C3 C2 C4 H5 0.6988 0.2208 0.8593 43 0.950 0.000 C5 C6 C4 H6 0.8045 0.1542 0.7506 43 0.950 0.000 C6 C5 C1 H8A 0.8189 0.0669 0.4434 137 0.980 0.000 C8 C7 H8A H8B 0.9028 0.1132 0.5124 137 0.980 0.000 C8 C7 H8A H8C 0.8543 0.2773 0.4602 137 0.980 0.000 C8 C7 H8A 2008lsh010 in Pbca ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.69407 0.25810 0.67280 1.00000 0.01688 0.02027 0.02132 -0.00051 0.00103 -0.00246 0.01949 0.00294 0.00015 0.00023 0.00010 0.00000 0.00095 0.00092 0.00096 0.00068 0.00074 0.00067 0.00041 C2 0.58829 0.33924 0.66566 1.00000 0.01970 0.02087 0.02273 0.00376 -0.00377 -0.00310 0.02110 0.00300 0.00015 0.00023 0.00010 0.00000 0.00097 0.00090 0.00095 0.00071 0.00080 0.00069 0.00041 H2 0.55941 0.36784 0.61625 1.00000 0.02532 0.00000 0.00000 C3 0.52530 0.37816 0.73054 1.00000 0.01435 0.02150 0.02663 0.00192 -0.00117 -0.00106 0.02083 0.00299 0.00015 0.00023 0.00010 0.00000 0.00095 0.00090 0.00103 0.00069 0.00076 0.00069 0.00041 H3 0.45321 0.43275 0.72508 1.00000 0.02500 0.00000 0.00000 C4 0.56615 0.33840 0.80382 1.00000 0.01692 0.01854 0.02409 0.00088 0.00071 -0.00301 0.01985 0.00297 0.00015 0.00023 0.00010 0.00000 0.00097 0.00087 0.00098 0.00069 0.00072 0.00066 0.00041 C5 0.67050 0.25256 0.81007 1.00000 0.01887 0.02137 0.02244 0.00307 -0.00234 -0.00188 0.02089 0.00304 0.00015 0.00024 0.00010 0.00000 0.00101 0.00095 0.00093 0.00069 0.00073 0.00070 0.00042 H5 0.69877 0.22084 0.85931 1.00000 0.02507 0.00000 0.00000 C6 0.73354 0.21291 0.74527 1.00000 0.01564 0.01995 0.02474 -0.00044 -0.00310 0.00043 0.02011 0.00296 0.00015 0.00024 0.00010 0.00000 0.00094 0.00089 0.00100 0.00073 0.00075 0.00067 0.00041 H6 0.80448 0.15422 0.75057 1.00000 0.02413 0.00000 0.00000 C7 0.73864 0.17731 0.53742 1.00000 0.02320 0.02127 0.02374 0.00174 -0.00072 -0.00016 0.02274 0.00325 0.00016 0.00025 0.00010 0.00000 0.00106 0.00094 0.00100 0.00072 0.00080 0.00070 0.00043 C8 0.83734 0.15689 0.48361 1.00000 0.02844 0.03527 0.02377 -0.00123 0.00042 0.00374 0.02916 0.00356 0.00017 0.00028 0.00011 0.00000 0.00117 0.00113 0.00102 0.00079 0.00087 0.00082 0.00048 H8A 0.81886 0.06693 0.44336 1.00000 0.04374 0.00000 0.00000 H8B 0.90281 0.11317 0.51241 1.00000 0.04374 0.00000 0.00000 H8C 0.85433 0.27732 0.46017 1.00000 0.04374 0.00000 0.00000 N1 0.76699 0.22743 0.60926 1.00000 0.01706 0.02714 0.02038 -0.00110 -0.00178 -0.00089 0.02153 0.00263 0.00013 0.00021 0.00008 0.00000 0.00087 0.00085 0.00085 0.00061 0.00065 0.00064 0.00038 N2 0.50107 0.37580 0.86978 1.00000 0.01940 0.02946 0.02403 -0.00087 0.00156 0.00255 0.02430 0.00291 0.00014 0.00023 0.00009 0.00000 0.00087 0.00092 0.00092 0.00066 0.00069 0.00066 0.00040 O1 0.64090 0.15142 0.51636 1.00000 0.02595 0.04230 0.02628 -0.00361 -0.00490 -0.00439 0.03151 0.00226 0.00012 0.00019 0.00008 0.00000 0.00083 0.00085 0.00075 0.00058 0.00062 0.00059 0.00038 H2AN 0.46302 0.48090 0.86695 1.00000 0.04020 0.03787 0.00177 0.00246 0.00124 0.00000 0.00678 H2BN 0.54318 0.37422 0.91221 1.00000 0.04214 0.03224 0.00182 0.00299 0.00106 0.00000 0.00682 H1N 0.83958 0.24422 0.61833 1.00000 0.03643 0.03284 0.00140 0.00300 0.00127 0.00000 0.00619 Final Structure Factor Calculation for 2008lsh010 in Pbca Total number of l.s. parameters = 113 Maximum vector length = 511 Memory required = 1533 / 22995 wR2 = 0.1238 before cycle 17 for 1716 data and 0 / 113 parameters Summary of restraints applied in cycle 17 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 3. 0. 0. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.020 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.009 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.050; Restrained GooF = 1.049 for 3 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0462 * P )^2 + 0.46 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0526 for 1195 Fo > 4sig(Fo) and 0.0888 for all 1716 data wR2 = 0.1238, GooF = S = 1.050, Restrained GooF = 1.049 for all data Occupancy sum of asymmetric unit = 11.00 for non-hydrogen and 10.00 for hydrogen atoms Principal mean square atomic displacements U 0.0224 0.0205 0.0155 C1 0.0284 0.0179 0.0170 C2 0.0274 0.0209 0.0141 C3 0.0242 0.0208 0.0145 C4 0.0262 0.0188 0.0176 C5 0.0257 0.0199 0.0147 C6 0.0249 0.0229 0.0204 C7 0.0370 0.0270 0.0235 C8 0.0273 0.0211 0.0161 N1 0.0301 0.0245 0.0183 N2 0.0437 0.0310 0.0198 O1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.011 0.021 0.031 0.044 0.057 0.071 0.091 0.122 0.176 1.000 Number in group 175. 181. 160. 174. 173. 167. 175. 167. 173. 171. GooF 1.003 0.981 1.098 1.053 1.102 1.032 1.146 0.988 0.930 1.146 K 4.361 1.427 1.218 0.992 0.970 1.018 1.012 1.003 1.009 0.973 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.04 1.15 1.31 1.64 inf Number in group 173. 178. 164. 174. 171. 169. 173. 176. 165. 173. GooF 0.940 0.925 1.089 1.014 1.005 1.091 1.055 0.982 1.111 1.257 K 1.067 1.073 1.044 1.006 1.005 0.992 1.004 1.021 1.032 0.953 R1 0.220 0.216 0.171 0.151 0.103 0.081 0.057 0.045 0.050 0.039 Recommended weighting scheme: WGHT 0.0425 0.4831 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 6 2 14 83.60 138.53 4.00 0.089 1.01 2 2 0 14412.49 17599.71 3.37 1.000 3.08 0 2 1 7844.95 9834.48 3.12 0.748 3.53 10 3 13 6.51 37.75 3.09 0.046 0.84 5 0 14 0.07 28.28 2.99 0.040 1.10 2 1 8 1687.69 1443.50 2.94 0.286 1.97 2 6 14 123.44 61.91 2.92 0.059 0.86 6 7 3 107.57 142.43 2.87 0.090 0.90 9 5 4 31.90 7.18 2.87 0.020 0.95 9 2 15 31.22 72.08 2.83 0.064 0.85 6 1 13 63.27 37.07 2.83 0.046 1.10 6 2 18 -11.90 20.63 2.81 0.034 0.85 6 6 7 27.31 12.77 2.79 0.027 0.95 2 5 4 16.21 4.89 2.77 0.017 1.33 11 3 5 732.55 601.54 2.69 0.185 0.95 6 3 2 33.23 18.43 2.69 0.032 1.51 10 4 0 20.50 0.07 2.66 0.002 0.99 8 6 12 38.29 8.80 2.65 0.022 0.79 6 7 6 12.86 27.63 2.59 0.040 0.87 10 1 12 13.11 29.11 2.58 0.041 0.91 3 4 4 22.16 9.21 2.55 0.023 1.54 3 2 13 20.37 38.15 2.51 0.047 1.20 5 1 14 125.10 162.93 2.51 0.096 1.09 4 1 12 81.62 112.19 2.47 0.080 1.28 7 7 4 77.34 118.05 2.47 0.082 0.86 7 1 14 94.91 59.68 2.44 0.058 1.00 3 5 15 150.16 111.48 2.41 0.080 0.88 0 0 22 12.17 61.57 2.39 0.059 0.79 6 3 10 145.20 112.40 2.39 0.080 1.15 3 2 6 20.71 9.52 2.35 0.023 1.97 0 0 10 362.42 266.14 2.34 0.123 1.74 13 3 4 -10.19 11.67 2.32 0.026 0.84 2 2 3 11.94 4.53 2.32 0.016 2.72 13 1 11 136.69 74.39 2.32 0.065 0.79 1 2 11 26.03 12.62 2.31 0.027 1.44 7 5 14 95.16 46.75 2.30 0.052 0.82 1 1 10 39.37 60.79 2.30 0.059 1.68 3 2 8 212.34 178.79 2.29 0.101 1.69 6 4 5 628.64 545.20 2.29 0.176 1.25 11 2 12 142.69 98.23 2.28 0.075 0.84 10 2 4 154.11 192.69 2.28 0.105 1.10 12 3 2 54.51 89.57 2.27 0.071 0.91 2 7 3 91.28 117.32 2.26 0.082 1.00 4 2 16 18.25 0.05 2.26 0.002 0.98 8 7 1 1.75 17.35 2.26 0.031 0.85 4 2 0 666.93 570.90 2.24 0.180 2.30 3 4 3 11.60 3.51 2.24 0.014 1.58 0 4 9 1436.27 1245.71 2.23 0.266 1.32 3 3 13 82.88 106.86 2.22 0.078 1.12 8 5 11 9.35 26.44 2.20 0.039 0.87 Bond lengths and angles C1 - Distance Angles C6 1.3867 (0.0024) C2 1.3955 (0.0026) 119.10 (0.16) N1 1.4252 (0.0023) 117.67 (0.16) 123.15 (0.16) C1 - C6 C2 C2 - Distance Angles C3 1.3862 (0.0025) C1 1.3955 (0.0026) 120.10 (0.16) H2 0.9500 119.95 119.95 C2 - C3 C1 C3 - Distance Angles C2 1.3862 (0.0025) C4 1.3965 (0.0025) 121.04 (0.17) H3 0.9500 119.48 119.48 C3 - C2 C4 C4 - Distance Angles C5 1.3935 (0.0025) C3 1.3965 (0.0025) 118.28 (0.17) N2 1.4130 (0.0024) 120.74 (0.16) 120.90 (0.17) C4 - C5 C3 C5 - Distance Angles C6 1.3863 (0.0025) C4 1.3935 (0.0025) 120.78 (0.17) H5 0.9500 119.61 119.61 C5 - C6 C4 C6 - Distance Angles C5 1.3863 (0.0025) C1 1.3867 (0.0024) 120.64 (0.17) H6 0.9500 119.68 119.68 C6 - C5 C1 C7 - Distance Angles O1 1.2359 (0.0022) N1 1.3461 (0.0024) 123.61 (0.17) C8 1.5120 (0.0027) 122.33 (0.17) 114.06 (0.17) C7 - O1 N1 C8 - Distance Angles C7 1.5120 (0.0027) 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 N1 - Distance Angles C7 1.3461 (0.0024) C1 1.4252 (0.0023) 127.67 (0.16) H1N 0.8881 (0.0159) 116.53 (1.47) 115.79 (1.47) N1 - C7 C1 N2 - Distance Angles C4 1.4130 (0.0024) H2AN 0.8839 (0.0156) 113.56 (1.44) H2BN 0.8938 (0.0160) 111.24 (1.53) 110.20 (2.03) N2 - C4 H2AN O1 - Distance Angles C7 1.2359 (0.0022) O1 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.894(16) 2.165(17) 3.057(2) 176(2) N2-H2BN...O1_$1 0.888(16) 2.156(17) 3.011(2) 161(2) N1-H1N...N2_$2 Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)