+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 17:44:41 on 17-Nov-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh006 in Pna2(1) CELL 0.71073 9.6978 12.3874 6.5757 90.000 90.000 90.000 ZERR 4.00 0.0004 0.0004 0.0002 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, Z SYMM 1/2 - X, 1/2 + Y, 1/2 + Z SFAC C H N O CL UNIT 32 32 4 4 4 V = 789.94 F(000) = 352.0 Mu = 0.42 mm-1 Cell Wt = 678.42 Rho = 1.426 MERG 2 OMIT -3.00 55.00 OMIT 0 3 1 EADP C8A C8B EADP N1A N1B EADP C7A C7B EADP O1A O1B FMAP 2 PLAN 5 ACTA SIZE 0.4 0.2 0.1 EQIV $1 x-1/2, -y+3/2, z EQIV $2 x+1/2, -y+3/2, z HTAB N1A O1A_$1 HTAB N1B O1B_$2 HTAB BOND $H L.S. 16 TEMP -153.00 WGHT 0.031400 0.156200 FVAR 0.33343 0.78802 C1 1 0.739644 0.650230 0.272417 11.00000 0.03402 0.01675 = 0.01424 -0.00433 -0.00150 -0.00074 C2 1 0.866158 0.618898 0.353629 11.00000 0.02574 0.02034 = 0.02276 0.00154 0.00772 0.00181 AFIX 43 H2 2 0.949221 0.637217 0.285258 11.00000 -1.20000 AFIX 0 C3 1 0.871175 0.560572 0.535466 11.00000 0.02044 0.02153 = 0.02336 0.00089 0.00067 0.00276 AFIX 43 H3 2 0.957370 0.539529 0.591511 11.00000 -1.20000 AFIX 0 C4 1 0.749901 0.533832 0.632830 11.00000 0.02159 0.01349 = 0.01555 -0.00211 -0.00060 0.00007 C5 1 0.623041 0.564329 0.554582 11.00000 0.01941 0.02285 = 0.02547 0.00026 -0.00048 -0.00074 AFIX 43 H5 2 0.540260 0.545740 0.623437 11.00000 -1.20000 AFIX 0 C6 1 0.618651 0.622555 0.373754 11.00000 0.02409 0.02103 = 0.02674 0.00308 -0.00833 -0.00096 AFIX 43 H6 2 0.532147 0.643657 0.318835 11.00000 -1.20000 AFIX 0 PART 1 C7A 1 0.811757 0.751922 -0.033470 21.00000 0.01808 0.02047 = 0.01767 -0.00212 0.00209 -0.00442 C8A 1 0.758926 0.810562 -0.214783 21.00000 0.02040 0.01961 = 0.01765 0.00088 -0.00104 0.00053 AFIX 137 H8A1 2 0.786698 0.886521 -0.207169 21.00000 -1.50000 H8A2 2 0.658084 0.805792 -0.218313 21.00000 -1.50000 H8A3 2 0.797182 0.778014 -0.338349 21.00000 -1.50000 AFIX 0 N1A 3 0.715480 0.708496 0.090929 21.00000 0.01100 0.02191 = 0.01744 0.00181 0.00017 -0.00094 AFIX 43 H1A 2 0.628781 0.717435 0.055191 21.00000 -1.20000 AFIX 0 O1A 4 0.936803 0.743062 -0.001069 21.00000 0.01469 0.04843 = 0.02536 0.00721 -0.00219 -0.00558 PART 2 SAME C7A > O1A C7B 1 0.686480 0.751904 -0.037418 -21.00000 0.01808 0.02047 = 0.01767 -0.00212 0.00209 -0.00442 C8B 1 0.735247 0.814437 -0.215594 -21.00000 0.02040 0.01961 = 0.01765 0.00088 -0.00104 0.00053 AFIX 137 H8B1 2 0.705166 0.778661 -0.340898 -21.00000 -1.50000 H8B2 2 0.836156 0.818495 -0.213308 -21.00000 -1.50000 H8B3 2 0.696665 0.887505 -0.210397 -21.00000 -1.50000 AFIX 0 N1B 3 0.782794 0.710407 0.087548 -21.00000 0.01100 0.02191 = 0.01744 0.00181 0.00017 -0.00094 AFIX 43 H1B 2 0.870917 0.718874 0.059900 -21.00000 -1.20000 AFIX 0 O1B 4 0.562277 0.741309 -0.002352 -21.00000 0.01469 0.04843 = 0.02536 0.00721 -0.00219 -0.00558 PART 0 CL1 5 0.755604 0.459286 0.857546 11.00000 0.03000 0.02311 = 0.01699 0.00429 -0.00058 0.00028 HKLF 4 Covalent radii and connectivity table for 2008lsh006 in Pna2(1) C 0.770 H 0.320 N 0.700 O 0.660 CL 0.990 C1 - C6 C2 N1A_a N1B_b C2 - C1 C3 C3 - C4 C2 C4 - C3 C5 Cl1 C5 - C4 C6 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 Cl1 - C4 Operators for generating equivalent atoms: $1 x-1/2, -y+3/2, z $2 x+1/2, -y+3/2, z Floating origin restraints generated 8699 Reflections read, of which 505 rejected -12 =< h =< 12, -16 =< k =< 16, -8 =< l =< 8, Max. 2-theta = 54.97 0 Systematic absence violations 0 Inconsistent equivalents 1821 Unique reflections, of which 0 suppressed R(int) = 0.0369 R(sigma) = 0.0353 Friedel opposites not merged Maximum memory for data reduction = 1664 / 18172 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 = 2028 / 148447 wR2 = 0.0771 before cycle 1 for 1821 data and 115 / 115 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.083; Restrained GooF = 1.081 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0314 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33343 0.00068 0.003 OSF 2 0.78802 0.00141 0.001 FVAR 2 Mean shift/esd = 0.002 Maximum = -0.015 for U23 Cl1 Max. shift = 0.000 A for H8B1_b Max. dU = 0.000 for C3 Least-squares cycle 2 Maximum vector length = 511 Memory required = 2028 / 148447 wR2 = 0.0771 before cycle 2 for 1821 data and 115 / 115 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.083; Restrained GooF = 1.081 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0314 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33343 0.00068 0.002 OSF 2 0.78802 0.00141 0.000 FVAR 2 Mean shift/esd = 0.001 Maximum = 0.005 for U22 Cl1 Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for Cl1 Least-squares cycle 3 Maximum vector length = 511 Memory required = 2028 / 148447 wR2 = 0.0771 before cycle 3 for 1821 data and 115 / 115 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.083; Restrained GooF = 1.081 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0314 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33343 0.00068 0.000 OSF 2 0.78802 0.00141 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for U23 C1 Max. shift = 0.000 A for H8A1_a Max. dU = 0.000 for C8A_a Least-squares cycle 4 Maximum vector length = 511 Memory required = 2028 / 148447 wR2 = 0.0771 before cycle 4 for 1821 data and 115 / 115 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.083; Restrained GooF = 1.081 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0314 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33343 0.00068 0.000 OSF 2 0.78802 0.00141 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = -0.001 for x Cl1 Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C5 Least-squares cycle 5 Maximum vector length = 511 Memory required = 2028 / 148447 wR2 = 0.0771 before cycle 5 for 1821 data and 115 / 115 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.083; Restrained GooF = 1.081 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0314 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33343 0.00068 0.000 OSF 2 0.78802 0.00141 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = -0.001 for x Cl1 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 = 2028 / 148447 wR2 = 0.0771 before cycle 6 for 1821 data and 115 / 115 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.083; Restrained GooF = 1.081 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0314 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33343 0.00068 0.000 OSF 2 0.78802 0.00141 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for x Cl1 Max. shift = 0.000 A for H8B2_b Max. dU = 0.000 for C6 Least-squares cycle 7 Maximum vector length = 511 Memory required = 2028 / 148447 wR2 = 0.0771 before cycle 7 for 1821 data and 115 / 115 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.083; Restrained GooF = 1.081 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0314 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33343 0.00068 0.000 OSF 2 0.78802 0.00141 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for x Cl1 Max. shift = 0.000 A for H8B3_b Max. dU = 0.000 for C8A_a Least-squares cycle 8 Maximum vector length = 511 Memory required = 2028 / 148447 wR2 = 0.0771 before cycle 8 for 1821 data and 115 / 115 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.083; Restrained GooF = 1.081 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0314 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33343 0.00068 0.000 OSF 2 0.78802 0.00141 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for x Cl1 Max. shift = 0.000 A for H8B1_b Max. dU = 0.000 for C8A_a Least-squares cycle 9 Maximum vector length = 511 Memory required = 2028 / 148447 wR2 = 0.0771 before cycle 9 for 1821 data and 115 / 115 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.083; Restrained GooF = 1.081 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0314 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33343 0.00068 0.000 OSF 2 0.78802 0.00141 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = -0.001 for x Cl1 Max. shift = 0.000 A for H8B1_b Max. dU = 0.000 for C8A_a Least-squares cycle 10 Maximum vector length = 511 Memory required = 2028 / 148447 wR2 = 0.0771 before cycle 10 for 1821 data and 115 / 115 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.083; Restrained GooF = 1.081 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0314 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33343 0.00068 0.000 OSF 2 0.78802 0.00141 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = -0.001 for x Cl1 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 = 2028 / 148447 wR2 = 0.0771 before cycle 11 for 1821 data and 115 / 115 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.083; Restrained GooF = 1.081 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0314 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33343 0.00068 0.000 OSF 2 0.78802 0.00141 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = -0.001 for x Cl1 Max. shift = 0.000 A for H8B1_b Max. dU = 0.000 for C8A_a Least-squares cycle 12 Maximum vector length = 511 Memory required = 2028 / 148447 wR2 = 0.0771 before cycle 12 for 1821 data and 115 / 115 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.083; Restrained GooF = 1.081 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0314 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33343 0.00068 0.000 OSF 2 0.78802 0.00141 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for x Cl1 Max. shift = 0.000 A for H8B1_b Max. dU = 0.000 for C8A_a Least-squares cycle 13 Maximum vector length = 511 Memory required = 2028 / 148447 wR2 = 0.0771 before cycle 13 for 1821 data and 115 / 115 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.083; Restrained GooF = 1.081 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0314 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33343 0.00068 0.000 OSF 2 0.78802 0.00141 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = -0.001 for x Cl1 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 = 2028 / 148447 wR2 = 0.0771 before cycle 14 for 1821 data and 115 / 115 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.083; Restrained GooF = 1.081 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0314 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33343 0.00068 0.000 OSF 2 0.78802 0.00141 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = -0.001 for x Cl1 Max. shift = 0.000 A for H8B1_b Max. dU = 0.000 for C8A_a Least-squares cycle 15 Maximum vector length = 511 Memory required = 2028 / 148447 wR2 = 0.0771 before cycle 15 for 1821 data and 115 / 115 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.083; Restrained GooF = 1.081 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0314 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33343 0.00068 0.000 OSF 2 0.78802 0.00141 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = 0.000 for x Cl1 Max. shift = 0.000 A for H8B1_b Max. dU = 0.000 for C8A_a Least-squares cycle 16 Maximum vector length = 511 Memory required = 2028 / 148447 wR2 = 0.0771 before cycle 16 for 1821 data and 115 / 115 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.083; Restrained GooF = 1.081 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0314 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.33343 0.00068 0.000 OSF 2 0.78802 0.00141 0.000 FVAR 2 Mean shift/esd = 0.000 Maximum = -0.001 for x Cl1 Max. shift = 0.000 A for H8B1_b Max. dU = 0.000 for C8A_a Largest correlation matrix elements -0.948 y C8B_b / y C8A_a 0.791 U13 Cl1 / z O1A_a -0.735 U13 Cl1 / U13 C1 0.922 x C8B_b / U11 C8A_a 0.790 U13 Cl1 / z N1A_a -0.728 U13 C8A_a / z C8A_a -0.910 z C8B_b / z C8A_a -0.783 U13 Cl1 / z N1B_b -0.724 z C7B_b / z O1A_a -0.904 x C8B_b / x C8A_a 0.765 z O1B_b / z C7B_b -0.721 z N1B_b / z N1A_a -0.867 U11 C8A_a / x C8A_a 0.760 z C8B_b / U13 C8A_a 0.710 z O1A_a / z N1A_a 0.859 y C8B_b / U12 C8A_a -0.747 U13 Cl1 / z C7B_b -0.705 z O1B_b / z O1A_a -0.823 U12 C8A_a / y C8A_a -0.745 z O1B_b / z N1A_a -0.705 z N1B_b / z O1A_a -0.822 U13 Cl1 / z O1B_b 0.738 z O1B_b / z N1B_b -0.703 z O1B_b / z C7A_a Idealized hydrogen atom generation before cycle 17 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.9492 0.6372 0.2853 43 0.950 0.000 C2 C1 C3 H3 0.9574 0.5395 0.5915 43 0.950 0.000 C3 C4 C2 H5 0.5403 0.5457 0.6234 43 0.950 0.000 C5 C4 C6 H6 0.5321 0.6437 0.3188 43 0.950 0.000 C6 C5 C1 H8A1 0.7867 0.8865 -0.2072 137 0.980 0.000 C8A_a C7A_a H8A1_a H8A2 0.6581 0.8058 -0.2183 137 0.980 0.000 C8A_a C7A_a H8A1_a H8A3 0.7972 0.7780 -0.3383 137 0.980 0.000 C8A_a C7A_a H8A1_a H1A 0.6288 0.7174 0.0552 43 0.880 0.000 N1A_a C7A_a C1 H8B1 0.7052 0.7787 -0.3409 137 0.980 0.000 C8B_b C7B_b H8B1_b H8B2 0.8362 0.8185 -0.2133 137 0.980 0.000 C8B_b C7B_b H8B1_b H8B3 0.6967 0.8875 -0.2104 137 0.980 0.000 C8B_b C7B_b H8B1_b H1B 0.8709 0.7189 0.0599 43 0.880 0.000 N1B_b C7B_b C1 2008lsh006 in Pna2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.73964 0.65023 0.27242 1.00000 0.03402 0.01675 0.01424 -0.00433 -0.00150 -0.00074 0.02167 0.00296 0.00018 0.00014 0.00028 0.00000 0.00102 0.00089 0.00080 0.00075 0.00102 0.00069 0.00040 C2 0.86616 0.61890 0.35363 1.00000 0.02574 0.02034 0.02276 0.00154 0.00772 0.00181 0.02295 0.00324 0.00017 0.00013 0.00029 0.00000 0.00083 0.00084 0.00115 0.00083 0.00107 0.00060 0.00046 H2 0.94922 0.63722 0.28526 1.00000 0.02754 0.00000 0.00000 C3 0.87117 0.56057 0.53547 1.00000 0.02044 0.02153 0.02336 0.00089 0.00067 0.00276 0.02177 0.00304 0.00018 0.00014 0.00026 0.00000 0.00087 0.00085 0.00131 0.00071 0.00074 0.00066 0.00049 H3 0.95737 0.53953 0.59151 1.00000 0.02613 0.00000 0.00000 C4 0.74990 0.53383 0.63283 1.00000 0.02159 0.01349 0.01555 -0.00211 -0.00060 0.00007 0.01688 0.00292 0.00016 0.00014 0.00029 0.00000 0.00087 0.00082 0.00089 0.00060 0.00062 0.00061 0.00037 C5 0.62304 0.56433 0.55458 1.00000 0.01941 0.02285 0.02547 0.00026 -0.00048 -0.00074 0.02258 0.00296 0.00017 0.00014 0.00027 0.00000 0.00084 0.00088 0.00133 0.00077 0.00074 0.00067 0.00050 H5 0.54026 0.54574 0.62344 1.00000 0.02709 0.00000 0.00000 C6 0.61865 0.62255 0.37375 1.00000 0.02409 0.02103 0.02674 0.00308 -0.00833 -0.00096 0.02395 0.00291 0.00017 0.00013 0.00028 0.00000 0.00083 0.00085 0.00136 0.00085 0.00097 0.00061 0.00049 H6 0.53215 0.64366 0.31883 1.00000 0.02874 0.00000 0.00000 C7A_a 0.81176 0.75192 -0.03347 0.78802 0.01808 0.02047 0.01767 -0.00212 0.00209 -0.00442 0.01874 0.00439 0.00022 0.00018 0.00049 0.00141 0.00092 0.00105 0.00110 0.00087 0.00093 0.00094 0.00044 C8A_a 0.75893 0.81056 -0.21478 0.78802 0.02040 0.01961 0.01765 0.00088 -0.00104 0.00053 0.01922 0.01302 0.00052 0.00060 0.00087 0.00141 0.00248 0.00110 0.00084 0.00075 0.00109 0.00141 0.00085 H8A1_a 0.78670 0.88652 -0.20717 0.78802 0.02883 0.00141 0.00000 H8A2_a 0.65808 0.80579 -0.21831 0.78802 0.02883 0.00141 0.00000 H8A3_a 0.79718 0.77801 -0.33835 0.78802 0.02883 0.00141 0.00000 N1A_a 0.71548 0.70850 0.09093 0.78802 0.01100 0.02191 0.01744 0.00181 0.00017 -0.00094 0.01678 0.00417 0.00019 0.00015 0.00051 0.00141 0.00086 0.00083 0.00085 0.00068 0.00094 0.00092 0.00038 H1A_a 0.62878 0.71744 0.05519 0.78802 0.02014 0.00141 0.00000 O1A_a 0.93680 0.74306 -0.00107 0.78802 0.01469 0.04843 0.02536 0.00721 -0.00219 -0.00558 0.02949 0.00382 0.00015 0.00015 0.00046 0.00141 0.00071 0.00102 0.00086 0.00069 0.00071 0.00062 0.00039 C7B_b 0.68648 0.75190 -0.03742 0.21198 0.01808 0.02047 0.01767 -0.00212 0.00209 -0.00442 0.01874 0.01714 0.00074 0.00066 0.00204 0.00141 0.00092 0.00105 0.00110 0.00087 0.00093 0.00094 0.00044 C8B_b 0.73525 0.81444 -0.21559 0.21198 0.02040 0.01961 0.01765 0.00088 -0.00104 0.00053 0.01922 0.05444 0.00250 0.00243 0.00363 0.00141 0.00248 0.00110 0.00084 0.00075 0.00109 0.00141 0.00085 H8B1_b 0.70517 0.77866 -0.34090 0.21198 0.02883 0.00141 0.00000 H8B2_b 0.83616 0.81850 -0.21331 0.21198 0.02883 0.00141 0.00000 H8B3_b 0.69667 0.88750 -0.21040 0.21198 0.02883 0.00141 0.00000 N1B_b 0.78279 0.71041 0.08755 0.21198 0.01100 0.02191 0.01744 0.00181 0.00017 -0.00094 0.01678 0.01727 0.00074 0.00062 0.00220 0.00141 0.00086 0.00083 0.00085 0.00068 0.00094 0.00092 0.00038 H1B_b 0.87092 0.71887 0.05990 0.21198 0.02014 0.00141 0.00000 O1B_b 0.56228 0.74131 -0.00235 0.21198 0.01469 0.04843 0.02536 0.00721 -0.00219 -0.00558 0.02949 0.01516 0.00056 0.00054 0.00198 0.00141 0.00071 0.00102 0.00086 0.00069 0.00071 0.00062 0.00039 Cl1 0.75560 0.45929 0.85755 1.00000 0.03000 0.02311 0.01699 0.00429 -0.00058 0.00028 0.02337 0.00074 0.00004 0.00003 0.00008 0.00000 0.00022 0.00022 0.00020 0.00018 0.00049 0.00015 0.00013 Final Structure Factor Calculation for 2008lsh006 in Pna2(1) Total number of l.s. parameters = 115 Maximum vector length = 511 Memory required = 1915 / 26068 wR2 = 0.0771 before cycle 17 for 1821 data and 2 / 115 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 0.010 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.083; Restrained GooF = 1.081 for 7 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0314 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0315 for 1536 Fo > 4sig(Fo) and 0.0407 for all 1821 data wR2 = 0.0771, GooF = S = 1.083, Restrained GooF = 1.081 for all data Flack x parameter = 0.0563 with esd 0.0590 Expected values are 0 (within 3 esd's) for correct and +1 for inverted absolute structure. Note that this rough estimate ignores correlation with other parameters; if the above value differs significantly from zero, it is ESSENTIAL to test the inverted structure or refine x as a full-matrix parameter using TWIN and BASF Occupancy sum of asymmetric unit = 11.00 for non-hydrogen and 8.00 for hydrogen atoms Principal mean square atomic displacements U 0.0341 0.0200 0.0109 C1 0.0326 0.0199 0.0164 C2 0.0247 0.0224 0.0182 C3 0.0217 0.0168 0.0122 C4 0.0255 0.0230 0.0192 C5 0.0345 0.0208 0.0166 C6 0.0250 0.0165 0.0146 C7A_a 0.0208 0.0199 0.0169 C8A_a 0.0226 0.0168 0.0109 N1A_a 0.0515 0.0233 0.0137 O1A_a 0.0250 0.0165 0.0146 C7B_b 0.0208 0.0199 0.0169 C8B_b 0.0226 0.0168 0.0109 N1B_b 0.0515 0.0233 0.0137 O1B_b 0.0300 0.0253 0.0148 Cl1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.017 0.027 0.039 0.053 0.071 0.096 0.128 0.174 0.250 1.000 Number in group 190. 185. 180. 180. 184. 174. 186. 184. 176. 182. GooF 0.901 1.011 1.082 1.134 1.089 1.299 1.155 1.048 0.926 1.143 K 0.736 0.883 0.919 0.921 0.994 0.996 1.004 1.016 1.013 0.993 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.31 1.64 inf Number in group 184. 189. 174. 189. 181. 182. 176. 181. 186. 179. GooF 1.053 0.943 1.128 1.200 1.110 1.050 0.911 0.991 1.047 1.337 K 0.963 1.031 1.014 1.004 1.006 1.011 1.009 1.021 1.011 0.976 R1 0.093 0.080 0.065 0.057 0.042 0.038 0.024 0.022 0.022 0.025 Recommended weighting scheme: WGHT 0.0286 0.1977 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) 9 7 -1 47.26 74.12 4.61 0.088 0.91 4 2 0 90.96 113.05 3.69 0.108 2.26 4 1 1 363.71 309.01 3.53 0.179 2.24 0 1 -1 1116.41 1484.55 3.36 0.393 5.81 8 0 1 273.20 214.13 3.35 0.149 1.19 6 1 -6 -0.47 6.11 3.15 0.025 0.90 7 11 2 6.42 13.96 3.14 0.038 0.84 4 6 0 928.40 825.33 3.11 0.293 1.57 4 1 -1 368.74 316.97 3.10 0.181 2.24 12 3 -1 36.61 53.86 3.01 0.075 0.79 8 0 5 20.92 33.87 3.00 0.059 0.89 11 1 -2 47.97 34.37 2.99 0.060 0.85 1 4 0 201.21 231.32 2.96 0.155 2.95 9 3 0 180.24 149.70 2.91 0.125 1.04 8 10 -1 12.85 22.39 2.89 0.048 0.86 0 2 8 48.12 75.22 2.86 0.088 0.81 4 12 -2 -1.63 5.04 2.83 0.023 0.91 9 9 1 59.78 78.17 2.75 0.090 0.84 4 5 -1 733.55 815.28 2.75 0.291 1.68 1 11 -2 -1.30 1.65 2.72 0.013 1.06 0 6 4 100.70 84.83 2.70 0.094 1.29 1 3 -1 8650.77 9632.49 2.66 1.000 3.29 3 8 0 113.48 131.75 2.65 0.117 1.40 6 13 -1 16.02 27.17 2.64 0.053 0.81 9 7 1 57.21 72.36 2.64 0.087 0.91 11 1 0 40.68 28.32 2.63 0.054 0.88 0 13 -5 93.88 124.23 2.62 0.114 0.77 2 11 4 7.04 14.26 2.62 0.038 0.91 6 3 6 106.58 87.20 2.61 0.095 0.89 7 6 0 583.47 518.76 2.61 0.232 1.15 1 3 1 8539.36 9539.35 2.58 0.995 3.29 7 9 0 11.08 19.40 2.57 0.045 0.98 3 5 -1 139.27 121.68 2.54 0.112 1.88 1 15 -3 43.52 58.37 2.54 0.078 0.77 2 4 2 56.06 70.35 2.53 0.085 2.04 4 6 -5 5.37 9.17 2.52 0.031 1.01 8 12 -1 14.32 24.47 2.49 0.050 0.78 10 6 2 8.92 16.72 2.48 0.042 0.85 4 2 -2 906.33 997.38 2.48 0.322 1.86 7 1 5 247.45 216.76 2.46 0.150 0.95 2 12 -3 14.44 22.81 2.46 0.049 0.92 0 2 0 57.50 68.89 2.41 0.085 6.19 7 3 -5 99.45 115.98 2.33 0.110 0.93 0 8 2 283.41 250.20 2.33 0.161 1.40 2 1 5 89.87 77.68 2.32 0.090 1.26 6 1 1 48.42 39.92 2.28 0.064 1.56 5 2 3 6.22 9.82 2.26 0.032 1.41 4 11 4 -1.72 3.98 2.26 0.020 0.87 6 12 2 123.93 100.08 2.25 0.102 0.84 9 8 -4 28.69 67.94 2.25 0.084 0.78 Bond lengths and angles C1 - Distance Angles C6 1.3923 (0.0024) C2 1.3932 (0.0023) 119.35 (0.16) N1A_a 1.4142 (0.0035) 112.95 (0.16) 127.70 (0.17) N1B_b 1.4861 (0.0131) 138.79 (0.32) 101.85 (0.32) 25.89 (0.26) C1 - C6 C2 N1A_a C2 - Distance Angles C1 1.3932 (0.0023) C3 1.3979 (0.0025) 120.16 (0.15) H2 0.9500 119.92 119.92 C2 - C1 C3 C3 - Distance Angles C4 1.3794 (0.0023) C2 1.3979 (0.0025) 119.44 (0.15) H3 0.9500 120.28 120.28 C3 - C4 C2 C4 - Distance Angles C3 1.3794 (0.0023) C5 1.3860 (0.0023) 121.27 (0.18) Cl1 1.7433 (0.0019) 119.57 (0.12) 119.16 (0.13) C4 - C3 C5 C5 - Distance Angles C4 1.3860 (0.0023) C6 1.3914 (0.0025) 119.06 (0.15) H5 0.9500 120.47 120.47 C5 - C4 C6 C6 - Distance Angles C5 1.3914 (0.0025) C1 1.3923 (0.0024) 120.72 (0.15) H6 0.9500 119.64 119.64 C6 - C5 C1 C7A_a - Distance Angles O1A_a 1.2361 (0.0026) N1A_a 1.3529 (0.0029) 122.52 (0.21) C8A_a 1.4872 (0.0047) 121.30 (0.25) 116.18 (0.25) C7A_a - O1A_a N1A_a C8A_a - Distance Angles C7A_a 1.4872 (0.0048) 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 1.3529 (0.0029) C1 1.4142 (0.0035) 126.78 (0.18) H1A_a 0.8800 116.61 116.61 N1A_a - C7A_a C1 O1A_a - Distance Angles C7A_a 1.2361 (0.0026) O1A_a - C7B_b - Distance Angles O1B_b 1.2334 (0.0087) N1B_b 1.3461 (0.0100) 121.53 (0.75) C8B_b 1.4820 (0.0141) 121.00 (1.15) 117.44 (1.10) C7B_b - O1B_b N1B_b C8B_b - Distance Angles C7B_b 1.4820 (0.0141) 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 N1B_b - Distance Angles C7B_b 1.3461 (0.0100) C1 1.4861 (0.0131) 119.70 (0.64) H1B_b 0.8800 120.15 120.15 N1B_b - C7B_b C1 O1B_b - Distance Angles C7B_b 1.2334 (0.0087) O1B_b - Cl1 - Distance Angles C4 1.7433 (0.0019) Cl1 - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 1.96 2.834(2) 171.6 N1A_a-H1A_a...O1A_$1a 0.88 1.96 2.838(9) 172.3 N1B_b-H1B_b...O1B_$2b Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)