+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 20:42:22 on 22-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh161 in Cc CELL 0.71073 4.5852 21.3953 9.4310 90.000 90.001 90.000 ZERR 4.00 0.0002 0.0010 0.0004 0.000 0.003 0.000 LATT -7 SYMM X, - Y, 1/2 + Z SFAC C H N O UNIT 40 52 4 4 V = 925.20 F(000) = 352.0 Mu = 0.08 mm-1 Cell Wt = 652.86 Rho = 1.172 MERG 2 OMIT -3.00 55.00 OMIT 1 3 0 OMIT -1 3 0 OMIT 0 0 -2 TWIN BASF 2.26846 EADP N1A N1B EXYZ N1A N1B EQIV $1 x, -y, z-1/2 EQIV $2 x, -y, z+1/2 HTAB N1A O1A_$1 HTAB N1B O1B_$2 FMAP 2 PLAN 5 SIZE 0.02 0.28 0.40 ACTA BOND $H WGHT 0.05630 0.14690 L.S. 16 TEMP -153.00 FVAR 0.40546 0.49704 C1 1 0.147715 0.091369 0.608930 11.00000 0.02112 0.01939 = 0.02238 -0.00027 -0.00010 -0.00435 C2 1 0.045551 0.116026 0.736389 11.00000 0.03114 0.03035 = 0.02137 0.00161 0.00235 0.00110 AFIX 43 H2 2 0.112851 0.099656 0.824122 11.00000 -1.20000 AFIX 0 C3 1 -0.154794 0.164565 0.734513 11.00000 0.03021 0.03140 = 0.03080 -0.00578 0.00631 0.00012 AFIX 43 H3 2 -0.223361 0.180845 0.822100 11.00000 -1.20000 AFIX 0 C4 1 -0.258545 0.190170 0.609164 11.00000 0.02169 0.02257 = 0.04125 -0.00025 0.00101 -0.00301 C5 1 -0.154843 0.164632 0.483223 11.00000 0.03140 0.03038 = 0.03053 0.00528 -0.00498 0.00141 AFIX 43 H5 2 -0.222993 0.180979 0.395624 11.00000 -1.20000 AFIX 0 C6 1 0.045452 0.115924 0.481829 11.00000 0.03129 0.02975 = 0.02197 -0.00036 -0.00071 0.00173 AFIX 43 H6 2 0.112438 0.099420 0.394168 11.00000 -1.20000 AFIX 0 PART 1 C7A 1 0.465777 0.007660 0.709960 21.00000 0.02771 0.02183 = 0.02406 0.00535 -0.00115 -0.00615 C8A 1 0.676568 -0.042647 0.665632 21.00000 0.03398 0.02451 = 0.03578 0.00405 -0.00549 0.00199 AFIX 137 H8A1 2 0.876188 -0.029235 0.686916 21.00000 -1.50000 H8A2 2 0.657404 -0.050222 0.563575 21.00000 -1.50000 H8A3 2 0.633300 -0.081224 0.717556 21.00000 -1.50000 AFIX 0 N1A 3 0.353142 0.042031 0.609147 21.00000 0.02568 0.02376 = 0.01910 -0.00023 0.00046 0.00017 AFIX 43 H1A 2 0.418496 0.032520 0.524109 21.00000 -1.20000 AFIX 0 O1A 4 0.404450 0.015881 0.836019 21.00000 0.04909 0.03343 = 0.02158 0.00869 0.00341 0.00346 PART 2 SAME C7A > O1A C7B 1 0.465617 0.007714 0.508038 -21.00000 0.03007 0.02253 = 0.02340 -0.00489 0.00218 -0.00599 C8B 1 0.678262 -0.042255 0.552487 -21.00000 0.03693 0.02493 = 0.03655 -0.00212 0.00594 0.00399 AFIX 137 H8B1 2 0.617747 -0.082501 0.512538 -21.00000 -1.50000 H8B2 2 0.681929 -0.045130 0.656179 -21.00000 -1.50000 H8B3 2 0.873445 -0.031640 0.517659 -21.00000 -1.50000 AFIX 0 N1B 3 0.353142 0.042031 0.609147 -21.00000 0.02568 0.02376 = 0.01910 -0.00023 0.00046 0.00017 AFIX 43 H1B 2 0.418331 0.032506 0.694207 -21.00000 -1.20000 AFIX 0 O1B 4 0.404575 0.015666 0.381680 -21.00000 0.04885 0.03495 = 0.02208 -0.00883 -0.00164 0.00403 PART 0 C9 1 -0.465735 0.244850 0.609009 11.00000 0.02712 0.02615 = 0.05877 -0.00015 -0.00073 0.00117 AFIX 23 H9A 2 -0.592634 0.242358 0.693750 11.00000 -1.20000 H9B 2 -0.592006 0.242374 0.524045 11.00000 -1.20000 AFIX 0 C10 1 -0.306458 0.307422 0.609179 11.00000 0.03788 0.02324 = 0.05560 0.00062 0.00051 0.00202 AFIX 137 H10A 2 -0.185726 0.310655 0.694611 11.00000 -1.50000 H10B 2 -0.449224 0.341506 0.608102 11.00000 -1.50000 H10C 2 -0.182068 0.310316 0.524934 11.00000 -1.50000 AFIX 0 HKLF 4 Covalent radii and connectivity table for 2008lsh161 in Cc C 0.770 H 0.320 N 0.700 O 0.660 C1 - C6 C2 N1B_b N1A_a C2 - C3 C1 C3 - C2 C4 C4 - C3 C5 C9 C5 - C6 C4 C6 - C5 C1 C7A_a - O1A_a N1A_a C8A_a C8A_a - C7A_a N1A_a - C7A_a C1 O1A_a - C7A_a C7B_b - O1B_b N1B_b C8B_b C8B_b - C7B_b N1B_b - C7B_b C1 O1B_b - C7B_b C9 - C4 C10 C10 - C9 Operators for generating equivalent atoms: $1 x, -y, z-1/2 $2 x, -y, z+1/2 Floating origin restraints generated 9660 Reflections read, of which 138 rejected -5 =< h =< 5, -27 =< k =< 27, -12 =< l =< 12, Max. 2-theta = 54.96 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Esd of mean(Fo^2) 3 7 8 0.88 0.20 3 1.24 1 Inconsistent equivalents 2019 Unique reflections, of which 0 suppressed R(int) = 0.0406 R(sigma) = 0.0330 Friedel opposites not merged Maximum memory for data reduction = 1843 / 23594 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 = 2269 / 177390 wR2 = 0.0970 before cycle 1 for 2019 data and 141 / 141 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.061; Restrained GooF = 1.059 for 8 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0563 * P )^2 + 0.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40546 0.00103 0.003 OSF 2 0.49704 0.00429 0.000 FVAR 2 3 2.26786 1.68960 0.000 BASF 1 Mean shift/esd = 0.003 Maximum = 0.011 for U22 C10 Max. shift = 0.000 A for H8B3_b Max. dU = 0.000 for C10 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2269 / 177390 wR2 = 0.0970 before cycle 2 for 2019 data and 141 / 141 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.061; Restrained GooF = 1.059 for 8 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0563 * P )^2 + 0.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40547 0.00103 0.004 OSF 2 0.49704 0.00429 0.000 FVAR 2 3 2.26772 1.68935 0.000 BASF 1 Mean shift/esd = 0.001 Maximum = 0.006 for tors H8B1_b Max. shift = 0.000 A for H8B3_b Max. dU = 0.000 for C10 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2269 / 177390 wR2 = 0.0970 before cycle 3 for 2019 data and 141 / 141 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.061; Restrained GooF = 1.059 for 8 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0563 * P )^2 + 0.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40547 0.00103 0.000 OSF 2 0.49704 0.00429 0.000 FVAR 2 3 2.26851 1.68945 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.004 for tors H8B1_b Max. shift = 0.000 A for H8B3_b Max. dU = 0.000 for C8B_b Least-squares cycle 4 Maximum vector length = 511 Memory required = 2269 / 177390 wR2 = 0.0970 before cycle 4 for 2019 data and 141 / 141 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.061; Restrained GooF = 1.059 for 8 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0563 * P )^2 + 0.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40547 0.00103 0.000 OSF 2 0.49704 0.00429 0.000 FVAR 2 3 2.26832 1.68943 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.003 for tors H8B1_b Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C8B_b Least-squares cycle 5 Maximum vector length = 511 Memory required = 2269 / 177390 wR2 = 0.0970 before cycle 5 for 2019 data and 141 / 141 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.061; Restrained GooF = 1.059 for 8 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0563 * P )^2 + 0.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40547 0.00103 0.000 OSF 2 0.49704 0.00429 0.000 FVAR 2 3 2.26806 1.68943 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.003 for tors H8B1_b Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C8A_a Least-squares cycle 6 Maximum vector length = 511 Memory required = 2269 / 177390 wR2 = 0.0970 before cycle 6 for 2019 data and 141 / 141 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.061; Restrained GooF = 1.059 for 8 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0563 * P )^2 + 0.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40547 0.00103 0.000 OSF 2 0.49704 0.00429 0.000 FVAR 2 3 2.26845 1.68933 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.002 for tors H8B1_b Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C8B_b Least-squares cycle 7 Maximum vector length = 511 Memory required = 2269 / 177390 wR2 = 0.0970 before cycle 7 for 2019 data and 141 / 141 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.061; Restrained GooF = 1.059 for 8 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0563 * P )^2 + 0.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40547 0.00103 0.000 OSF 2 0.49704 0.00429 0.000 FVAR 2 3 2.26841 1.68928 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.002 for tors H8B1_b Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C8A_a Least-squares cycle 8 Maximum vector length = 511 Memory required = 2269 / 177390 wR2 = 0.0970 before cycle 8 for 2019 data and 141 / 141 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.061; Restrained GooF = 1.059 for 8 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0563 * P )^2 + 0.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40547 0.00103 0.000 OSF 2 0.49704 0.00429 0.000 FVAR 2 3 2.26853 1.68940 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.002 for tors H8B1_b Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C8B_b Least-squares cycle 9 Maximum vector length = 511 Memory required = 2269 / 177390 wR2 = 0.0970 before cycle 9 for 2019 data and 141 / 141 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.061; Restrained GooF = 1.059 for 8 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0563 * P )^2 + 0.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40547 0.00103 0.000 OSF 2 0.49704 0.00429 0.000 FVAR 2 3 2.26880 1.68929 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.001 for tors H8B1_b Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C8A_a Least-squares cycle 10 Maximum vector length = 511 Memory required = 2269 / 177390 wR2 = 0.0970 before cycle 10 for 2019 data and 141 / 141 parameters Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.061; Restrained GooF = 1.059 for 8 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0563 * P )^2 + 0.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40547 0.00103 0.000 OSF 2 0.49704 0.00429 0.000 FVAR 2 3 2.26867 1.68934 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.001 for tors H8B1_b Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C8A_a Least-squares cycle 11 Maximum vector length = 511 Memory required = 2269 / 177390 wR2 = 0.0970 before cycle 11 for 2019 data and 141 / 141 parameters Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.061; Restrained GooF = 1.059 for 8 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0563 * P )^2 + 0.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40547 0.00103 0.000 OSF 2 0.49704 0.00429 0.000 FVAR 2 3 2.26865 1.68931 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.001 for tors H8B1_b Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C8A_a Least-squares cycle 12 Maximum vector length = 511 Memory required = 2269 / 177390 wR2 = 0.0970 before cycle 12 for 2019 data and 141 / 141 parameters Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.061; Restrained GooF = 1.059 for 8 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0563 * P )^2 + 0.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40547 0.00103 0.000 OSF 2 0.49705 0.00429 0.000 FVAR 2 3 2.26865 1.68938 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.001 for tors H8B1_b Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for O1B_b Least-squares cycle 13 Maximum vector length = 511 Memory required = 2269 / 177390 wR2 = 0.0970 before cycle 13 for 2019 data and 141 / 141 parameters Summary of restraints applied in cycle 13 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.061; Restrained GooF = 1.059 for 8 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0563 * P )^2 + 0.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40547 0.00103 0.000 OSF 2 0.49705 0.00429 0.000 FVAR 2 3 2.26839 1.68934 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.001 for tors H8B1_b Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C8A_a Least-squares cycle 14 Maximum vector length = 511 Memory required = 2269 / 177390 wR2 = 0.0970 before cycle 14 for 2019 data and 141 / 141 parameters Summary of restraints applied in cycle 14 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.061; Restrained GooF = 1.059 for 8 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0563 * P )^2 + 0.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40547 0.00103 0.000 OSF 2 0.49705 0.00429 0.000 FVAR 2 3 2.26854 1.68935 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.001 for tors H8B1_b Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C3 Least-squares cycle 15 Maximum vector length = 511 Memory required = 2269 / 177390 wR2 = 0.0970 before cycle 15 for 2019 data and 141 / 141 parameters Summary of restraints applied in cycle 15 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.061; Restrained GooF = 1.059 for 8 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0563 * P )^2 + 0.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40547 0.00103 0.000 OSF 2 0.49705 0.00429 0.000 FVAR 2 3 2.26898 1.68931 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.001 for tors H8B1_b Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C8A_a Least-squares cycle 16 Maximum vector length = 511 Memory required = 2269 / 177390 wR2 = 0.0970 before cycle 16 for 2019 data and 141 / 141 parameters Summary of restraints applied in cycle 16 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.061; Restrained GooF = 1.059 for 8 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0563 * P )^2 + 0.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.40547 0.00103 0.000 OSF 2 0.49705 0.00429 0.000 FVAR 2 3 2.26890 1.68933 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.001 for tors H8B1_b Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C3 Largest correlation matrix elements -0.722 y O1B_b / y O1A_a -0.594 U33 C8B_b / U33 C8A_a -0.530 z O1B_b / y O1A_a 0.615 U23 O1B_b / U23 O1A_a 0.573 y O1B_b / FVAR 2 0.530 y O1B_b / z O1A_a -0.614 y O1B_b / U23 O1A_a -0.567 y O1A_a / FVAR 2 0.523 U23 O1A_a / y O1A_a 0.605 U23 O1B_b / y O1A_a 0.559 z O1A_a / FVAR 2 -0.519 U23 O1B_b / y O1B_b -0.603 U22 O1B_b / FVAR 2 0.553 z O1B_b / FVAR 2 -0.506 U22 O1B_b / z O1A_a 0.603 U22 O1A_a / FVAR 2 0.535 z O1B_b / z O1A_a 0.502 z O1B_b / U22 O1A_a Idealized hydrogen atom generation before cycle 17 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.1129 0.0997 0.8241 43 0.950 0.000 C2 C3 C1 H3 -0.2234 0.1808 0.8221 43 0.950 0.000 C3 C2 C4 H5 -0.2230 0.1810 0.3956 43 0.950 0.000 C5 C6 C4 H6 0.1124 0.0994 0.3942 43 0.950 0.000 C6 C5 C1 H8A1 0.8762 -0.0292 0.6869 137 0.980 0.000 C8A_a C7A_a H8A1_a H8A2 0.6574 -0.0502 0.5636 137 0.980 0.000 C8A_a C7A_a H8A1_a H8A3 0.6333 -0.0812 0.7176 137 0.980 0.000 C8A_a C7A_a H8A1_a H1A 0.4185 0.0325 0.5241 43 0.880 0.000 N1A_a C7A_a C1 H8B1 0.6179 -0.0825 0.5125 137 0.980 0.000 C8B_b C7B_b H8B1_b H8B2 0.6818 -0.0452 0.6562 137 0.980 0.000 C8B_b C7B_b H8B1_b H8B3 0.8735 -0.0316 0.5177 137 0.980 0.000 C8B_b C7B_b H8B1_b H1B 0.4183 0.0325 0.6942 43 0.880 0.000 N1B_b C7B_b C1 H9A -0.5926 0.2424 0.6937 23 0.990 0.000 C9 C4 C10 H9B -0.5920 0.2424 0.5240 23 0.990 0.000 C9 C4 C10 H10A -0.1857 0.3107 0.6946 137 0.980 0.000 C10 C9 H10A H10B -0.4492 0.3415 0.6081 137 0.980 0.000 C10 C9 H10A H10C -0.1821 0.3103 0.5249 137 0.980 0.000 C10 C9 H10A 2008lsh161 in Cc ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.14772 0.09137 0.60893 1.00000 0.02112 0.01938 0.02239 -0.00027 -0.00010 -0.00435 0.02097 0.00214 0.00025 0.00005 0.00015 0.00000 0.00060 0.00058 0.00058 0.00052 0.00050 0.00046 0.00027 C2 0.04555 0.11603 0.73639 1.00000 0.03115 0.03035 0.02137 0.00161 0.00235 0.00110 0.02762 0.00243 0.00029 0.00007 0.00014 0.00000 0.00074 0.00076 0.00066 0.00053 0.00055 0.00054 0.00032 H2 0.11285 0.09966 0.82412 1.00000 0.03315 0.00000 0.00000 C3 -0.15479 0.16457 0.73451 1.00000 0.03021 0.03140 0.03080 -0.00578 0.00631 0.00012 0.03081 0.00249 0.00030 0.00007 0.00016 0.00000 0.00072 0.00080 0.00079 0.00061 0.00058 0.00056 0.00034 H3 -0.22336 0.18084 0.82210 1.00000 0.03697 0.00000 0.00000 C4 -0.25854 0.19017 0.60916 1.00000 0.02169 0.02258 0.04125 -0.00025 0.00101 -0.00301 0.02851 0.00248 0.00030 0.00006 0.00017 0.00000 0.00065 0.00062 0.00075 0.00064 0.00062 0.00053 0.00031 C5 -0.15484 0.16463 0.48322 1.00000 0.03141 0.03038 0.03053 0.00528 -0.00499 0.00141 0.03077 0.00256 0.00030 0.00007 0.00016 0.00000 0.00075 0.00080 0.00078 0.00060 0.00059 0.00056 0.00034 H5 -0.22299 0.18098 0.39562 1.00000 0.03692 0.00000 0.00000 C6 0.04545 0.11592 0.48183 1.00000 0.03129 0.02975 0.02198 -0.00036 -0.00071 0.00173 0.02767 0.00240 0.00029 0.00006 0.00015 0.00000 0.00075 0.00075 0.00065 0.00054 0.00056 0.00054 0.00032 H6 0.11244 0.09942 0.39417 1.00000 0.03321 0.00000 0.00000 C7A_a 0.46578 0.00766 0.70996 0.49705 0.02771 0.02183 0.02406 0.00535 -0.00116 -0.00615 0.02454 0.00468 0.00058 0.00012 0.00029 0.00429 0.00152 0.00136 0.00148 0.00099 0.00105 0.00098 0.00074 C8A_a 0.67658 -0.04264 0.66563 0.49705 0.03400 0.02450 0.03578 0.00405 -0.00550 0.00200 0.03143 0.00602 0.00073 0.00015 0.00035 0.00429 0.00176 0.00148 0.00192 0.00121 0.00129 0.00114 0.00082 H8A1_a 0.87619 -0.02923 0.68692 0.49705 0.04714 0.00429 0.00000 H8A2_a 0.65742 -0.05022 0.56357 0.49705 0.04714 0.00429 0.00000 H8A3_a 0.63331 -0.08122 0.71755 0.49705 0.04714 0.00429 0.00000 N1A_a 0.35314 0.04203 0.60915 0.49705 0.02568 0.02376 0.01911 -0.00023 0.00046 0.00017 0.02285 0.00192 0.00023 0.00005 0.00013 0.00429 0.00052 0.00050 0.00046 0.00049 0.00042 0.00043 0.00024 H1A_a 0.41849 0.03252 0.52411 0.49705 0.02742 0.00429 0.00000 O1A_a 0.40445 0.01588 0.83602 0.49705 0.04909 0.03343 0.02158 0.00869 0.00341 0.00346 0.03470 0.00393 0.00048 0.00016 0.00027 0.00429 0.00149 0.00147 0.00118 0.00117 0.00095 0.00098 0.00068 C7B_b 0.46562 0.00771 0.50804 0.50295 0.03007 0.02254 0.02340 -0.00489 0.00218 -0.00599 0.02534 0.00440 0.00058 0.00012 0.00028 0.00429 0.00156 0.00137 0.00147 0.00099 0.00108 0.00100 0.00075 C8B_b 0.67826 -0.04225 0.55249 0.50295 0.03694 0.02493 0.03654 -0.00212 0.00594 0.00399 0.03280 0.00599 0.00071 0.00014 0.00036 0.00429 0.00182 0.00151 0.00192 0.00120 0.00131 0.00118 0.00083 H8B1_b 0.61786 -0.08249 0.51246 0.50295 0.04921 0.00429 0.00000 H8B2_b 0.68178 -0.04516 0.65618 0.50295 0.04921 0.00429 0.00000 H8B3_b 0.87348 -0.03162 0.51774 0.50295 0.04921 0.00429 0.00000 N1B_b 0.35314 0.04203 0.60915 0.50295 0.02568 0.02376 0.01911 -0.00023 0.00046 0.00017 0.02285 0.00192 0.00023 0.00005 0.00013 0.00429 0.00052 0.00050 0.00046 0.00049 0.00042 0.00043 0.00024 H1B_b 0.41833 0.03250 0.69421 0.50295 0.02742 0.00429 0.00000 O1B_b 0.40457 0.01567 0.38168 0.50295 0.04885 0.03495 0.02209 -0.00883 -0.00164 0.00403 0.03530 0.00555 0.00048 0.00016 0.00027 0.00429 0.00147 0.00150 0.00118 0.00118 0.00095 0.00099 0.00068 C9 -0.46574 0.24485 0.60901 1.00000 0.02712 0.02616 0.05877 -0.00015 -0.00073 0.00118 0.03735 0.00290 0.00034 0.00006 0.00021 0.00000 0.00070 0.00071 0.00099 0.00075 0.00069 0.00056 0.00036 H9A -0.59263 0.24236 0.69375 1.00000 0.04482 0.00000 0.00000 H9B -0.59201 0.24237 0.52404 1.00000 0.04482 0.00000 0.00000 C10 -0.30646 0.30742 0.60918 1.00000 0.03788 0.02325 0.05560 0.00063 0.00051 0.00202 0.03891 0.00305 0.00037 0.00006 0.00022 0.00000 0.00086 0.00068 0.00093 0.00076 0.00075 0.00062 0.00037 H10A -0.18573 0.31065 0.69461 1.00000 0.05837 0.00000 0.00000 H10B -0.44923 0.34151 0.60810 1.00000 0.05837 0.00000 0.00000 H10C -0.18207 0.31032 0.52493 1.00000 0.05837 0.00000 0.00000 Final Structure Factor Calculation for 2008lsh161 in Cc Total number of l.s. parameters = 141 Maximum vector length = 511 Memory required = 2130 / 25046 wR2 = 0.0970 before cycle 17 for 2019 data and 2 / 141 parameters Summary of restraints applied in cycle 17 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 0. 0. 6. 0. 0. 0. 0. 0. 0. 0. rms sigma 0.000 0.000 0.000 0.032 0.000 0.000 0.000 0.000 0.000 0.000 0.000 rms deviation 0.000 0.000 0.000 0.003 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.061; Restrained GooF = 1.059 for 8 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0563 * P )^2 + 0.15 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0376 for 1833 Fo > 4sig(Fo) and 0.0433 for all 2019 data wR2 = 0.0970, GooF = S = 1.061, Restrained GooF = 1.059 for all data Occupancy sum of asymmetric unit = 12.00 for non-hydrogen and 13.00 for hydrogen atoms Principal mean square atomic displacements U 0.0247 0.0224 0.0158 C1 0.0326 0.0296 0.0207 C2 0.0393 0.0310 0.0221 C3 0.0413 0.0251 0.0191 C4 0.0373 0.0323 0.0227 C5 0.0325 0.0286 0.0219 C6 0.0334 0.0244 0.0159 C7A_a 0.0407 0.0316 0.0220 C8A_a 0.0257 0.0238 0.0191 N1A_a 0.0508 0.0363 0.0169 O1A_a 0.0350 0.0238 0.0172 C7B_b 0.0428 0.0330 0.0226 C8B_b 0.0257 0.0238 0.0191 N1B_b 0.0505 0.0378 0.0176 O1B_b 0.0588 0.0279 0.0254 C9 0.0556 0.0381 0.0230 C10 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.025 0.040 0.056 0.072 0.086 0.105 0.132 0.170 0.233 1.000 Number in group 210. 198. 202. 216. 184. 205. 199. 203. 202. 200. GooF 1.051 1.087 0.982 1.112 1.136 0.967 1.055 1.120 0.983 1.108 K 1.499 1.072 1.024 1.008 0.971 0.990 1.009 1.006 1.018 0.983 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.97 1.05 1.15 1.32 1.67 inf Number in group 211. 197. 205. 195. 203. 200. 202. 204. 199. 203. GooF 1.002 1.068 1.040 1.049 0.965 1.015 0.862 0.947 1.065 1.484 K 1.053 1.042 1.013 1.025 0.989 1.004 1.016 1.012 1.024 0.968 R1 0.113 0.082 0.068 0.056 0.045 0.035 0.028 0.025 0.027 0.036 Recommended weighting scheme: WGHT 0.0564 0.1470 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 0 208.21 396.02 6.74 0.248 5.35 0 4 2 219.90 294.99 4.30 0.214 3.54 0 4 6 117.24 154.51 3.83 0.155 1.51 -1 3 4 107.15 82.62 3.64 0.113 2.01 0 4 -2 231.76 295.01 3.55 0.214 3.54 3 3 5 8.88 2.74 3.42 0.021 1.17 0 4 -6 120.43 154.47 3.42 0.155 1.51 0 10 11 18.34 8.76 3.13 0.037 0.80 3 21 -3 31.70 19.16 3.08 0.055 0.82 4 14 2 -0.61 2.75 3.03 0.021 0.90 -1 7 -10 41.58 28.36 2.99 0.066 0.88 0 8 10 12.53 3.89 2.95 0.025 0.89 -1 3 1 5361.23 6440.44 2.90 1.000 3.57 -5 9 -1 13.48 20.37 2.87 0.056 0.85 3 15 -1 93.93 116.76 2.86 0.135 1.04 1 3 12 1.82 12.13 2.83 0.043 0.77 5 3 4 91.67 71.76 2.79 0.106 0.85 1 3 4 102.36 82.52 2.77 0.113 2.01 -3 3 5 7.29 3.48 2.76 0.023 1.17 3 5 8 25.34 34.36 2.75 0.073 0.91 -1 3 -4 101.10 81.51 2.75 0.112 2.01 -3 3 8 22.53 32.91 2.74 0.071 0.93 -1 11 1 146.05 121.04 2.70 0.137 1.76 5 9 -3 15.01 6.11 2.57 0.031 0.83 3 7 -8 -2.31 2.42 2.56 0.019 0.89 -1 3 6 43.38 34.47 2.55 0.073 1.46 0 12 0 105.22 86.04 2.53 0.116 1.78 -1 11 9 21.33 29.83 2.51 0.068 0.90 0 6 6 273.69 232.37 2.50 0.190 1.44 1 3 -4 100.47 83.63 2.50 0.114 2.01 2 18 1 56.20 70.19 2.49 0.104 1.05 2 22 4 10.16 21.45 2.49 0.058 0.84 -2 26 0 34.16 21.95 2.38 0.058 0.77 2 18 -1 58.17 71.54 2.38 0.105 1.05 -1 9 8 35.84 44.96 2.37 0.084 1.03 0 6 -6 271.24 232.31 2.36 0.190 1.44 5 9 1 13.88 20.25 2.36 0.056 0.85 5 9 4 9.00 1.60 2.35 0.016 0.80 2 8 5 46.25 58.12 2.34 0.095 1.28 2 2 -1 133.33 157.69 2.34 0.156 2.18 -1 3 -1 5411.15 6430.47 2.33 0.999 3.57 -1 5 -1 4619.11 5341.97 2.33 0.910 2.97 0 0 4 537.09 464.51 2.33 0.268 2.36 0 6 5 745.11 645.63 2.32 0.317 1.67 1 9 -10 15.43 8.35 2.31 0.036 0.86 1 11 1 143.35 121.50 2.29 0.137 1.76 4 10 4 84.57 103.69 2.26 0.127 0.93 0 4 1 22.48 28.70 2.26 0.067 4.65 3 15 1 94.60 113.15 2.26 0.133 1.04 -2 2 -5 150.73 124.79 2.24 0.139 1.44 Bond lengths and angles C1 - Distance Angles C6 1.3902 (0.0019) C2 1.3938 (0.0018) 119.16 (0.11) N1A_a 1.4148 (0.0015) 120.51 (0.12) 120.33 (0.12) C1 - C6 C2 C2 - Distance Angles C3 1.3866 (0.0021) C1 1.3938 (0.0018) 119.68 (0.12) H2 0.9500 120.16 120.16 C2 - C3 C1 C3 - Distance Angles C2 1.3866 (0.0021) C4 1.3871 (0.0022) 122.27 (0.13) H3 0.9500 118.87 118.87 C3 - C2 C4 C4 - Distance Angles C3 1.3871 (0.0022) C5 1.3912 (0.0021) 117.08 (0.12) C9 1.5070 (0.0019) 121.58 (0.14) 121.30 (0.15) C4 - C3 C5 C5 - Distance Angles C6 1.3891 (0.0021) C4 1.3912 (0.0021) 121.92 (0.13) H5 0.9500 119.04 119.04 C5 - C6 C4 C6 - Distance Angles C5 1.3891 (0.0021) C1 1.3902 (0.0019) 119.89 (0.12) H6 0.9500 120.06 120.06 C6 - C5 C1 C7A_a - Distance Angles O1A_a 1.2343 (0.0037) N1A_a 1.3082 (0.0028) 122.00 (0.26) C8A_a 1.5058 (0.0040) 121.03 (0.27) 116.96 (0.23) C7A_a - O1A_a N1A_a C8A_a - Distance Angles C7A_a 1.5058 (0.0040) H8A1_a 0.9800 109.47 H8A2_a 0.9800 109.47 109.47 H8A3_a 0.9800 109.47 109.47 109.47 C8A_a - C7A_a H8A1_a H8A2_a N1A_a - Distance Angles C7A_a 1.3082 (0.0028) C1 1.4148 (0.0015) 133.10 (0.16) H1A_a 0.8800 113.45 113.45 N1A_a - C7A_a C1 O1A_a - Distance Angles C7A_a 1.2343 (0.0037) O1A_a - C7B_b - Distance Angles O1B_b 1.2359 (0.0037) C8B_b 1.5064 (0.0041) 120.84 (0.26) C7B_b - O1B_b C8B_b - Distance Angles C7B_b 1.5064 (0.0041) H8B1_b 0.9800 109.47 H8B2_b 0.9800 109.47 109.47 H8B3_b 0.9800 109.47 109.47 109.47 C8B_b - C7B_b H8B1_b H8B2_b O1B_b - Distance Angles C7B_b 1.2359 (0.0037) O1B_b - C9 - Distance Angles C4 1.5070 (0.0019) C10 1.5250 (0.0019) 112.31 (0.13) H9A 0.9900 109.14 109.14 H9B 0.9900 109.14 109.14 107.87 C9 - C4 C10 H9A C10 - Distance Angles C9 1.5250 (0.0019) 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 Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 2.06 2.868(4) 153.2 N1A_a-H1A_a...O1A_$1a 0.88 2.05 2.861(4) 153.3 N1B_b-H1B_b...O1B_$2b FMAP and GRID set by program FMAP 2 1 13 GRID -5.000 -1 -2 5.000 1 2 R1 = 0.0398 for 1064 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.14 at 0.0640 0.4140 0.1167 [ 1.35 A from N1B ] Deepest hole -0.16 at 0.1844 0.0686 0.6763 [ 0.82 A from C1 ] Mean = 0.00, Rms deviation from mean = 0.04 e/A^3, Highest memory used = 2556 / 22202 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5640 0.0860 0.6167 1.00000 0.05 0.14 1.35 N1A 1.35 N1B 1.51 H1B 1.59 H1A Q2 1 0.7271 0.0779 0.5620 1.00000 0.05 0.13 1.75 H1A 1.83 C6 1.93 N1A 1.93 N1B Q3 1 -0.2428 0.0789 0.6666 1.00000 0.05 0.13 1.68 C2 1.86 H1B 1.89 C1 1.98 C3 Q4 1 1.2083 -0.0750 0.6173 1.00000 0.05 0.12 1.93 H8A1 1.93 H10B 2.02 H8B3 2.13 H8B1 Q5 1 -0.3912 0.1138 0.7204 1.00000 0.05 0.12 1.54 C3 1.89 H3 1.96 H1B 2.01 C2 Shortest distances between peaks (including symmetry equivalents) 1 2 0.92 2 3 1.00 1 3 1.01 3 5 1.13 1 5 1.16 2 5 1.77 Time profile in seconds ----------------------- 0.11: 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 0.00: Analyse other restraints etc. 0.47: 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 2.69: Structure factors and derivatives 0.98: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.25: Solve l.s. equations 0.00: Generate HTAB table 0.06: Other dependent quantities, CIF, tables 0.03: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + shelxl finished at 20:42:27 Total CPU time: 4.7 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++