+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + p21n started at 18:00:42 on 03-Dec-2010 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL p21n in P2(1)/n CELL 0.71073 6.9836 13.2116 12.0495 90.000 91.532 90.000 ZERR 2.00 0.0001 0.0002 0.0002 0.000 0.001 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O F SI UNIT 32 88 4 4 12 2 V = 1111.34 F(000) = 476.0 Mu = 0.17 mm-1 Cell Wt = 877.24 Rho = 1.311 MERG 2 OMIT -3.00 55.00 OMIT 0 2 0 OMIT 0 2 2 OMIT -1 0 5 EXTI 0.37376 SHEL 7 0.77 simu delu dfix 0.85 0.02 o1 h1wa o1 h1wb dang 1.37 0.02 h1wa h1wb eadp n1 n11 EQIV $1 -X+1, -Y+1, -Z+1 HTAB O1 F3 HTAB O1 F1_$1 FMAP 2 PLAN 10 SIZE 0.28 0.38 0.42 ACTA BOND $H WGHT 0.09040 0.15730 L.S. 19 TEMP -153.00 FVAR 0.53107 0.89098 MOLE 1 F1 5 0.104010 0.384813 0.495001 11.00000 0.03809 0.02624 = 0.03404 -0.00290 0.00028 0.00642 F2 5 0.042998 0.516471 0.364719 11.00000 0.03656 0.03471 = 0.02288 -0.00002 0.00333 -0.00165 F3 5 0.215045 0.551752 0.534195 11.00000 0.02602 0.04143 = 0.03745 -0.00280 -0.00309 -0.00897 SI1 6 0.000000 0.500000 0.500000 10.50000 0.02088 0.02309 = 0.02185 -0.00181 0.00048 -0.00058 MOLE 2 PART 1 C1 1 0.397339 0.674706 0.349850 21.00000 0.03410 0.02556 = 0.02342 0.00345 0.00512 -0.00157 AFIX 23 H1A 2 0.349776 0.604112 0.348957 21.00000 -1.20000 H1B 2 0.484217 0.682252 0.415604 21.00000 -1.20000 AFIX 0 C2 1 0.228701 0.745164 0.362592 21.00000 0.03771 0.03541 = 0.03791 0.00079 0.01118 0.00497 AFIX 33 H2A 2 0.163102 0.728866 0.431225 21.00000 -1.50000 H2B 2 0.139500 0.736989 0.299052 21.00000 -1.50000 H2C 2 0.274211 0.815299 0.365758 21.00000 -1.50000 AFIX 0 C3 1 0.686482 0.624940 0.255986 21.00000 0.02691 0.02826 = 0.03115 0.00493 -0.00137 0.00327 AFIX 23 H3A 2 0.643499 0.554228 0.266238 21.00000 -1.20000 H3B 2 0.761598 0.644674 0.323395 21.00000 -1.20000 AFIX 0 C4 1 0.817013 0.628769 0.156956 21.00000 0.02936 0.03843 = 0.04877 0.00292 0.00866 0.00060 AFIX 33 H4A 2 0.926192 0.583314 0.170034 21.00000 -1.50000 H4B 2 0.863501 0.698095 0.147111 21.00000 -1.50000 H4C 2 0.745409 0.607365 0.089944 21.00000 -1.50000 AFIX 0 C5 1 0.568264 0.802457 0.236272 21.00000 0.03819 0.02176 = 0.03342 0.00717 0.00234 -0.00317 AFIX 23 H5A 2 0.640943 0.811411 0.167534 21.00000 -1.20000 H5B 2 0.450385 0.843800 0.228853 21.00000 -1.20000 AFIX 0 C6 1 0.687913 0.842118 0.333174 21.00000 0.05007 0.03333 = 0.04814 -0.00638 0.00305 -0.01453 AFIX 33 H6A 2 0.718164 0.913596 0.320778 21.00000 -1.50000 H6B 2 0.807027 0.803132 0.340020 21.00000 -1.50000 H6C 2 0.616136 0.835346 0.401562 21.00000 -1.50000 AFIX 0 C7 1 0.392517 0.667328 0.142578 21.00000 0.02995 0.03289 = 0.02483 0.00177 -0.00358 0.00166 AFIX 23 H7A 2 0.274097 0.708512 0.142774 21.00000 -1.20000 H7B 2 0.465188 0.687285 0.076630 21.00000 -1.20000 AFIX 0 C8 1 0.337276 0.556932 0.131215 21.00000 0.03654 0.03421 = 0.03609 -0.00656 -0.00388 -0.00182 AFIX 33 H8A 2 0.260816 0.547284 0.062647 21.00000 -1.50000 H8B 2 0.261913 0.536657 0.194963 21.00000 -1.50000 H8C 2 0.453339 0.515394 0.128679 21.00000 -1.50000 AFIX 0 N1 3 0.511811 0.692373 0.245907 21.00000 0.02628 0.02191 = 0.02256 0.00558 0.00076 -0.00009 PART 2 same c1 > n1 C11 1 0.350605 0.764862 0.239567 -21.00000 0.02532 AFIX 23 H11A 2 0.273031 0.740586 0.174945 -21.00000 -1.20000 H11B 2 0.393025 0.834481 0.222341 -21.00000 -1.20000 AFIX 0 C12 1 0.221578 0.770207 0.338449 -21.00000 0.04316 AFIX 33 H12A 2 0.110482 0.812936 0.320089 -21.00000 -1.50000 H12B 2 0.292748 0.799189 0.402040 -21.00000 -1.50000 H12C 2 0.178018 0.701953 0.357199 -21.00000 -1.50000 AFIX 0 C13 1 0.642374 0.713563 0.147898 -21.00000 0.02693 AFIX 23 H13A 2 0.673292 0.786324 0.140323 -21.00000 -1.20000 H13B 2 0.563662 0.693416 0.082004 -21.00000 -1.20000 AFIX 0 C14 1 0.828331 0.652786 0.149813 -21.00000 0.02337 AFIX 33 H14A 2 0.886623 0.656557 0.076844 -21.00000 -1.50000 H14B 2 0.800746 0.581973 0.167581 -21.00000 -1.50000 H14C 2 0.917008 0.680809 0.206243 -21.00000 -1.50000 AFIX 0 C15 1 0.644920 0.731013 0.352507 -21.00000 0.04016 AFIX 23 H15A 2 0.583912 0.704985 0.420021 -21.00000 -1.20000 H15B 2 0.774106 0.700521 0.348968 -21.00000 -1.20000 AFIX 0 C16 1 0.664067 0.844046 0.361126 -21.00000 0.03983 AFIX 33 H16A 2 0.724870 0.861720 0.432766 -21.00000 -1.50000 H16B 2 0.536819 0.875177 0.355344 -21.00000 -1.50000 H16C 2 0.742998 0.868957 0.300888 -21.00000 -1.50000 AFIX 0 C17 1 0.482185 0.588301 0.271746 -21.00000 0.03168 AFIX 23 H17A 2 0.405330 0.583198 0.339378 -21.00000 -1.20000 H17B 2 0.604086 0.551821 0.286387 -21.00000 -1.20000 AFIX 0 C18 1 0.373902 0.536007 0.176408 -21.00000 0.04004 AFIX 33 H18A 2 0.349533 0.465337 0.196315 -21.00000 -1.50000 H18B 2 0.450788 0.538322 0.109600 -21.00000 -1.50000 H18C 2 0.251750 0.570732 0.162002 -21.00000 -1.50000 AFIX 0 N11 3 0.526402 0.698715 0.250763 -21.00000 0.02628 0.02191 = 0.02256 0.00558 0.00076 -0.00009 MOLE 3 PART 0 O1 4 0.551381 0.621013 0.630275 11.00000 0.03069 0.06959 = 0.04775 -0.02591 -0.00046 -0.00014 H1WA 2 0.456488 0.588756 0.599450 11.00000 -1.50000 H1WB 2 0.648222 0.602855 0.592821 11.00000 -1.50000 HKLF 4 Covalent radii and connectivity table for p21n in P2(1)/n C 0.770 H 0.320 N 0.700 O 0.660 F 0.640 SI 1.170 F1 - Si1 F2 - Si1 F3 - Si1 Si1 - F2 F2_$2 F1 F1_$2 F3_$2 F3 C1_a - C2_a N1_a C2_a - C1_a C3_a - N1_a C4_a C4_a - C3_a C5_a - C6_a N1_a C6_a - C5_a C7_a - C8_a N1_a C8_a - C7_a N1_a - C5_a C3_a C7_a C1_a C11_b - N11_b C12_b C12_b - C11_b C13_b - N11_b C14_b C14_b - C13_b C15_b - C16_b N11_b C16_b - C15_b C17_b - N11_b C18_b C18_b - C17_b N11_b - C11_b C13_b C17_b C15_b O1 - no bonds found Operators for generating equivalent atoms: $1 -x+1, -y+1, -z+1 $2 -x, -y+1, -z+1 26099 Reflections read, of which 889 rejected -9 =< h =< 8, -17 =< k =< 17, -15 =< l =< 15, Max. 2-theta = 54.97 0 Systematic absence violations Inconsistent equivalents etc. h k l Fo^2 Sigma(Fo^2) N Su of mean(Fo^2) 1 3 0 127.38 5.16 3 98.13 -1 2 1 199.62 2.64 7 136.88 1 4 1 253.51 13.32 3 103.24 3 Inconsistent equivalents 2536 Unique reflections, of which 0 suppressed R(int) = 0.0520 R(sigma) = 0.0304 Friedel opposites merged Maximum memory for data reduction = 3667 / 25505 Special position constraints for Si1 x = 0.0000 y = 0.5000 z = 0.5000 sof = 0.50000 Input constraints retained (at least in part) for sof 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 = 4305 / 210075 wR2 = 0.1577 before cycle 1 for 2536 data and 167 / 167 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 18. 0. 0. 0. 24. 214. 0. 0. rms sigma 0.000 0.020 0.020 0.033 0.000 0.000 0.000 0.010 0.060 0.000 0.000 rms deviation 0.000 0.011 0.014 0.018 0.000 0.000 0.000 0.001 0.010 0.000 0.000 GooF = S = 1.299; Restrained GooF = 1.237 for 259 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0904 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.53107 0.00252 -0.001 OSF 2 0.89098 0.00276 0.000 FVAR 2 3 0.37359 0.02426 -0.007 EXTI Mean shift/su = 0.002 Maximum = -0.019 for U12 Si1 Max. shift = 0.000 A for H1WA Max. dU = 0.000 for C16_b Least-squares cycle 2 Maximum vector length = 511 Memory required = 4305 / 210075 wR2 = 0.1577 before cycle 2 for 2536 data and 167 / 167 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 18. 0. 0. 0. 24. 214. 0. 0. rms sigma 0.000 0.020 0.020 0.033 0.000 0.000 0.000 0.010 0.060 0.000 0.000 rms deviation 0.000 0.011 0.014 0.018 0.000 0.000 0.000 0.001 0.010 0.000 0.000 GooF = S = 1.298; Restrained GooF = 1.237 for 259 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0904 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.53107 0.00252 0.001 OSF 2 0.89098 0.00276 0.000 FVAR 2 3 0.37359 0.02425 0.000 EXTI Mean shift/su = 0.001 Maximum = -0.007 for U12 Si1 Max. shift = 0.000 A for H12B_b Max. dU = 0.000 for C16_b Least-squares cycle 3 Maximum vector length = 511 Memory required = 4305 / 210075 wR2 = 0.1577 before cycle 3 for 2536 data and 167 / 167 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 18. 0. 0. 0. 24. 214. 0. 0. rms sigma 0.000 0.020 0.020 0.033 0.000 0.000 0.000 0.010 0.060 0.000 0.000 rms deviation 0.000 0.011 0.014 0.018 0.000 0.000 0.000 0.001 0.010 0.000 0.000 GooF = S = 1.298; Restrained GooF = 1.237 for 259 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0904 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.53107 0.00252 0.000 OSF 2 0.89098 0.00276 0.000 FVAR 2 3 0.37358 0.02425 0.000 EXTI Mean shift/su = 0.000 Maximum = -0.001 for x C6_a Max. shift = 0.000 A for C16_b Max. dU = 0.000 for C16_b Least-squares cycle 4 Maximum vector length = 511 Memory required = 4305 / 210075 wR2 = 0.1577 before cycle 4 for 2536 data and 167 / 167 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 18. 0. 0. 0. 24. 214. 0. 0. rms sigma 0.000 0.020 0.020 0.033 0.000 0.000 0.000 0.010 0.060 0.000 0.000 rms deviation 0.000 0.011 0.014 0.018 0.000 0.000 0.000 0.001 0.010 0.000 0.000 GooF = S = 1.299; Restrained GooF = 1.237 for 259 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0904 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.53107 0.00252 0.000 OSF 2 0.89098 0.00276 0.000 FVAR 2 3 0.37359 0.02425 0.000 EXTI Mean shift/su = 0.000 Maximum = -0.001 for x C6_a Max. shift = 0.000 A for C16_b Max. dU = 0.000 for C16_b Least-squares cycle 5 Maximum vector length = 511 Memory required = 4305 / 210075 wR2 = 0.1577 before cycle 5 for 2536 data and 167 / 167 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 18. 0. 0. 0. 24. 214. 0. 0. rms sigma 0.000 0.020 0.020 0.033 0.000 0.000 0.000 0.010 0.060 0.000 0.000 rms deviation 0.000 0.011 0.014 0.018 0.000 0.000 0.000 0.001 0.010 0.000 0.000 GooF = S = 1.299; Restrained GooF = 1.237 for 259 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0904 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.53107 0.00252 0.000 OSF 2 0.89098 0.00276 0.000 FVAR 2 3 0.37359 0.02425 0.000 EXTI Mean shift/su = 0.000 Maximum = -0.001 for x C6_a Max. shift = 0.000 A for C16_b Max. dU = 0.000 for C16_b Least-squares cycle 6 Maximum vector length = 511 Memory required = 4305 / 210075 wR2 = 0.1577 before cycle 6 for 2536 data and 167 / 167 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 18. 0. 0. 0. 24. 214. 0. 0. rms sigma 0.000 0.020 0.020 0.033 0.000 0.000 0.000 0.010 0.060 0.000 0.000 rms deviation 0.000 0.011 0.014 0.018 0.000 0.000 0.000 0.001 0.010 0.000 0.000 GooF = S = 1.299; Restrained GooF = 1.237 for 259 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0904 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.53107 0.00252 0.000 OSF 2 0.89098 0.00276 0.000 FVAR 2 3 0.37359 0.02425 0.000 EXTI Mean shift/su = 0.000 Maximum = -0.001 for x C6_a Max. shift = 0.000 A for C16_b Max. dU = 0.000 for C16_b Least-squares cycle 7 Maximum vector length = 511 Memory required = 4305 / 210075 wR2 = 0.1577 before cycle 7 for 2536 data and 167 / 167 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 18. 0. 0. 0. 24. 214. 0. 0. rms sigma 0.000 0.020 0.020 0.033 0.000 0.000 0.000 0.010 0.060 0.000 0.000 rms deviation 0.000 0.011 0.014 0.018 0.000 0.000 0.000 0.001 0.010 0.000 0.000 GooF = S = 1.299; Restrained GooF = 1.237 for 259 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0904 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.53107 0.00252 0.001 OSF 2 0.89098 0.00276 0.000 FVAR 2 3 0.37360 0.02425 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for C16_b Max. dU = 0.000 for C16_b Least-squares cycle 8 Maximum vector length = 511 Memory required = 4305 / 210075 wR2 = 0.1577 before cycle 8 for 2536 data and 167 / 167 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 18. 0. 0. 0. 24. 214. 0. 0. rms sigma 0.000 0.020 0.020 0.033 0.000 0.000 0.000 0.010 0.060 0.000 0.000 rms deviation 0.000 0.011 0.014 0.018 0.000 0.000 0.000 0.001 0.010 0.000 0.000 GooF = S = 1.299; Restrained GooF = 1.237 for 259 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0904 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.53107 0.00252 0.000 OSF 2 0.89098 0.00276 0.000 FVAR 2 3 0.37359 0.02425 0.000 EXTI Mean shift/su = 0.000 Maximum = -0.001 for x C6_a Max. shift = 0.000 A for C16_b Max. dU = 0.000 for C16_b Least-squares cycle 9 Maximum vector length = 511 Memory required = 4305 / 210075 wR2 = 0.1577 before cycle 9 for 2536 data and 167 / 167 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 18. 0. 0. 0. 24. 214. 0. 0. rms sigma 0.000 0.020 0.020 0.033 0.000 0.000 0.000 0.010 0.060 0.000 0.000 rms deviation 0.000 0.011 0.014 0.018 0.000 0.000 0.000 0.001 0.010 0.000 0.000 GooF = S = 1.299; Restrained GooF = 1.237 for 259 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0904 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.53107 0.00252 0.000 OSF 2 0.89098 0.00276 0.000 FVAR 2 3 0.37359 0.02425 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.000 for x C6_a Max. shift = 0.000 A for C16_b Max. dU = 0.000 for C16_b Least-squares cycle 10 Maximum vector length = 511 Memory required = 4305 / 210075 wR2 = 0.1577 before cycle 10 for 2536 data and 167 / 167 parameters Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 18. 0. 0. 0. 24. 214. 0. 0. rms sigma 0.000 0.020 0.020 0.033 0.000 0.000 0.000 0.010 0.060 0.000 0.000 rms deviation 0.000 0.011 0.014 0.018 0.000 0.000 0.000 0.001 0.010 0.000 0.000 GooF = S = 1.299; Restrained GooF = 1.237 for 259 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0904 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.53107 0.00252 0.000 OSF 2 0.89098 0.00276 0.000 FVAR 2 3 0.37359 0.02425 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.000 for x C6_a Max. shift = 0.000 A for C16_b Max. dU = 0.000 for C16_b Least-squares cycle 11 Maximum vector length = 511 Memory required = 4305 / 210075 wR2 = 0.1577 before cycle 11 for 2536 data and 167 / 167 parameters Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 18. 0. 0. 0. 24. 214. 0. 0. rms sigma 0.000 0.020 0.020 0.033 0.000 0.000 0.000 0.010 0.060 0.000 0.000 rms deviation 0.000 0.011 0.014 0.018 0.000 0.000 0.000 0.001 0.010 0.000 0.000 GooF = S = 1.299; Restrained GooF = 1.237 for 259 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0904 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.53107 0.00252 0.000 OSF 2 0.89098 0.00276 0.000 FVAR 2 3 0.37359 0.02425 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.000 for x C6_a Max. shift = 0.000 A for C16_b Max. dU = 0.000 for C16_b Least-squares cycle 12 Maximum vector length = 511 Memory required = 4305 / 210075 wR2 = 0.1577 before cycle 12 for 2536 data and 167 / 167 parameters Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 18. 0. 0. 0. 24. 214. 0. 0. rms sigma 0.000 0.020 0.020 0.033 0.000 0.000 0.000 0.010 0.060 0.000 0.000 rms deviation 0.000 0.011 0.014 0.018 0.000 0.000 0.000 0.001 0.010 0.000 0.000 GooF = S = 1.299; Restrained GooF = 1.237 for 259 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0904 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.53107 0.00252 0.000 OSF 2 0.89098 0.00276 0.000 FVAR 2 3 0.37359 0.02425 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.000 for y F3 Max. shift = 0.000 A for C16_b Max. dU = 0.000 for C16_b Least-squares cycle 13 Maximum vector length = 511 Memory required = 4305 / 210075 wR2 = 0.1577 before cycle 13 for 2536 data and 167 / 167 parameters Summary of restraints applied in cycle 13 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 18. 0. 0. 0. 24. 214. 0. 0. rms sigma 0.000 0.020 0.020 0.033 0.000 0.000 0.000 0.010 0.060 0.000 0.000 rms deviation 0.000 0.011 0.014 0.018 0.000 0.000 0.000 0.001 0.010 0.000 0.000 GooF = S = 1.299; Restrained GooF = 1.237 for 259 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0904 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.53107 0.00252 0.000 OSF 2 0.89098 0.00276 0.000 FVAR 2 3 0.37359 0.02425 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.000 for y F3 Max. shift = 0.000 A for C16_b Max. dU = 0.000 for C16_b Least-squares cycle 14 Maximum vector length = 511 Memory required = 4305 / 210075 wR2 = 0.1577 before cycle 14 for 2536 data and 167 / 167 parameters Summary of restraints applied in cycle 14 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 18. 0. 0. 0. 24. 214. 0. 0. rms sigma 0.000 0.020 0.020 0.033 0.000 0.000 0.000 0.010 0.060 0.000 0.000 rms deviation 0.000 0.011 0.014 0.018 0.000 0.000 0.000 0.001 0.010 0.000 0.000 GooF = S = 1.299; Restrained GooF = 1.237 for 259 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0904 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.53107 0.00252 0.000 OSF 2 0.89098 0.00276 0.000 FVAR 2 3 0.37359 0.02425 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.000 for y F3 Max. shift = 0.000 A for C16_b Max. dU = 0.000 for C16_b Least-squares cycle 15 Maximum vector length = 511 Memory required = 4305 / 210075 wR2 = 0.1577 before cycle 15 for 2536 data and 167 / 167 parameters Summary of restraints applied in cycle 15 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 18. 0. 0. 0. 24. 214. 0. 0. rms sigma 0.000 0.020 0.020 0.033 0.000 0.000 0.000 0.010 0.060 0.000 0.000 rms deviation 0.000 0.011 0.014 0.018 0.000 0.000 0.000 0.001 0.010 0.000 0.000 GooF = S = 1.299; Restrained GooF = 1.237 for 259 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0904 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.53107 0.00252 0.000 OSF 2 0.89098 0.00276 0.000 FVAR 2 3 0.37359 0.02425 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.000 for y F3 Max. shift = 0.000 A for C16_b Max. dU = 0.000 for C16_b Least-squares cycle 16 Maximum vector length = 511 Memory required = 4305 / 210075 wR2 = 0.1577 before cycle 16 for 2536 data and 167 / 167 parameters Summary of restraints applied in cycle 16 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 18. 0. 0. 0. 24. 214. 0. 0. rms sigma 0.000 0.020 0.020 0.033 0.000 0.000 0.000 0.010 0.060 0.000 0.000 rms deviation 0.000 0.011 0.014 0.018 0.000 0.000 0.000 0.001 0.010 0.000 0.000 GooF = S = 1.299; Restrained GooF = 1.237 for 259 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0904 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.53107 0.00252 0.000 OSF 2 0.89098 0.00276 0.000 FVAR 2 3 0.37359 0.02425 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.000 for y F3 Max. shift = 0.000 A for C16_b Max. dU = 0.000 for C16_b Least-squares cycle 17 Maximum vector length = 511 Memory required = 4305 / 210075 wR2 = 0.1577 before cycle 17 for 2536 data and 167 / 167 parameters Summary of restraints applied in cycle 17 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 18. 0. 0. 0. 24. 214. 0. 0. rms sigma 0.000 0.020 0.020 0.033 0.000 0.000 0.000 0.010 0.060 0.000 0.000 rms deviation 0.000 0.011 0.014 0.018 0.000 0.000 0.000 0.001 0.010 0.000 0.000 GooF = S = 1.299; Restrained GooF = 1.237 for 259 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0904 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.53107 0.00252 0.000 OSF 2 0.89098 0.00276 0.000 FVAR 2 3 0.37359 0.02425 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.000 for y F3 Max. shift = 0.000 A for C16_b Max. dU = 0.000 for C16_b Least-squares cycle 18 Maximum vector length = 511 Memory required = 4305 / 210075 wR2 = 0.1577 before cycle 18 for 2536 data and 167 / 167 parameters Summary of restraints applied in cycle 18 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 18. 0. 0. 0. 24. 214. 0. 0. rms sigma 0.000 0.020 0.020 0.033 0.000 0.000 0.000 0.010 0.060 0.000 0.000 rms deviation 0.000 0.011 0.014 0.018 0.000 0.000 0.000 0.001 0.010 0.000 0.000 GooF = S = 1.299; Restrained GooF = 1.237 for 259 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0904 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.53107 0.00252 0.000 OSF 2 0.89098 0.00276 0.000 FVAR 2 3 0.37360 0.02425 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.000 for y F3 Max. shift = 0.000 A for C16_b Max. dU = 0.000 for C16_b Least-squares cycle 19 Maximum vector length = 511 Memory required = 4305 / 210075 wR2 = 0.1577 before cycle 19 for 2536 data and 167 / 167 parameters Summary of restraints applied in cycle 19 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 18. 0. 0. 0. 24. 214. 0. 0. rms sigma 0.000 0.020 0.020 0.033 0.000 0.000 0.000 0.010 0.060 0.000 0.000 rms deviation 0.000 0.011 0.014 0.018 0.000 0.000 0.000 0.001 0.010 0.000 0.000 GooF = S = 1.299; Restrained GooF = 1.237 for 259 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0904 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value su shift/su parameter 1 0.53107 0.00252 0.000 OSF 2 0.89098 0.00276 0.000 FVAR 2 3 0.37359 0.02425 0.000 EXTI Mean shift/su = 0.000 Maximum = 0.000 for y F3 Max. shift = 0.000 A for C16_b Max. dU = 0.000 for C16_b Largest correlation matrix elements -0.874 z N11_b / z N1_a -0.685 U11 C12_b / U23 C2_a 0.601 U11 C12_b / y C2_a -0.825 y N11_b / y N1_a 0.684 EXTI / OSF -0.600 x C16_b / x C6_a -0.773 x N11_b / x N1_a -0.663 z C16_b / U33 C6_a -0.595 U11 C12_b / z C2_a 0.754 U11 C14_b / y C4_a -0.626 x C14_b / x C4_a -0.594 x C14_b / U12 C4_a -0.751 z C14_b / z C4_a -0.620 U11 C16_b / U22 C6_a -0.574 U11 C16_b / U13 C6_a 0.732 U11 C16_b / z C6_a 0.618 U22 Si1 / OSF 0.574 U23 C4_a / z C4_a -0.701 y C14_b / U22 C4_a 0.617 U33 Si1 / OSF -0.571 y C16_b / y C6_a -0.695 z C14_b / U23 C4_a 0.609 U11 Si1 / OSF -0.558 U11 C14_b / U33 C4_a Idealized hydrogen atom generation before cycle 20 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.3498 0.6041 0.3490 23 0.990 0.000 C1_a C2_a N1_a H1B 0.4842 0.6823 0.4156 23 0.990 0.000 C1_a C2_a N1_a H2A 0.1631 0.7289 0.4312 33 0.980 0.000 C2_a C1_a H2A_a H2B 0.1395 0.7370 0.2991 33 0.980 0.000 C2_a C1_a H2A_a H2C 0.2742 0.8153 0.3658 33 0.980 0.000 C2_a C1_a H2A_a H3A 0.6435 0.5542 0.2662 23 0.990 0.000 C3_a N1_a C4_a H3B 0.7616 0.6447 0.3234 23 0.990 0.000 C3_a N1_a C4_a H4A 0.9262 0.5833 0.1700 33 0.980 0.000 C4_a C3_a H4A_a H4B 0.8635 0.6981 0.1471 33 0.980 0.000 C4_a C3_a H4A_a H4C 0.7454 0.6074 0.0899 33 0.980 0.000 C4_a C3_a H4A_a H5A 0.6409 0.8114 0.1675 23 0.990 0.000 C5_a C6_a N1_a H5B 0.4504 0.8438 0.2289 23 0.990 0.000 C5_a C6_a N1_a H6A 0.7182 0.9136 0.3208 33 0.980 0.000 C6_a C5_a H6A_a H6B 0.8070 0.8031 0.3400 33 0.980 0.000 C6_a C5_a H6A_a H6C 0.6161 0.8353 0.4016 33 0.980 0.000 C6_a C5_a H6A_a H7A 0.2741 0.7085 0.1428 23 0.990 0.000 C7_a C8_a N1_a H7B 0.4652 0.6873 0.0766 23 0.990 0.000 C7_a C8_a N1_a H8A 0.2608 0.5473 0.0626 33 0.980 0.000 C8_a C7_a H8A_a H8B 0.2619 0.5367 0.1950 33 0.980 0.000 C8_a C7_a H8A_a H8C 0.4533 0.5154 0.1287 33 0.980 0.000 C8_a C7_a H8A_a H11A 0.2730 0.7406 0.1749 23 0.990 0.000 C11_b N11_b C12_b H11B 0.3930 0.8345 0.2223 23 0.990 0.000 C11_b N11_b C12_b H12A 0.1105 0.8129 0.3201 33 0.980 0.000 C12_b C11_b H12A_b H12B 0.2927 0.7992 0.4020 33 0.980 0.000 C12_b C11_b H12A_b H12C 0.1780 0.7019 0.3572 33 0.980 0.000 C12_b C11_b H12A_b H13A 0.6733 0.7863 0.1403 23 0.990 0.000 C13_b N11_b C14_b H13B 0.5637 0.6934 0.0820 23 0.990 0.000 C13_b N11_b C14_b H14A 0.8866 0.6566 0.0768 33 0.980 0.000 C14_b C13_b H14A_b H14B 0.8008 0.5820 0.1676 33 0.980 0.000 C14_b C13_b H14A_b H14C 0.9170 0.6808 0.2062 33 0.980 0.000 C14_b C13_b H14A_b H15A 0.5839 0.7050 0.4200 23 0.990 0.000 C15_b C16_b N11_b H15B 0.7741 0.7005 0.3490 23 0.990 0.000 C15_b C16_b N11_b H16A 0.7249 0.8617 0.4328 33 0.980 0.000 C16_b C15_b H16A_b H16B 0.5369 0.8752 0.3554 33 0.980 0.000 C16_b C15_b H16A_b H16C 0.7430 0.8689 0.3009 33 0.980 0.000 C16_b C15_b H16A_b H17A 0.4053 0.5832 0.3394 23 0.990 0.000 C17_b N11_b C18_b H17B 0.6041 0.5518 0.2864 23 0.990 0.000 C17_b N11_b C18_b H18A 0.3495 0.4653 0.1963 33 0.980 0.000 C18_b C17_b H18A_b H18B 0.4508 0.5383 0.1096 33 0.980 0.000 C18_b C17_b H18A_b H18C 0.2518 0.5707 0.1620 33 0.980 0.000 C18_b C17_b H18A_b p21n in P2(1)/n ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq F1 0.10401 0.38481 0.49500 1.00000 0.03809 0.02624 0.03404 -0.00290 0.00028 0.00642 0.03280 0.00161 0.00013 0.00006 0.00008 0.00000 0.00053 0.00047 0.00050 0.00033 0.00037 0.00035 0.00028 F2 0.04300 0.51647 0.36472 1.00000 0.03656 0.03471 0.02288 -0.00002 0.00333 -0.00165 0.03134 0.00161 0.00014 0.00007 0.00007 0.00000 0.00052 0.00051 0.00045 0.00032 0.00036 0.00035 0.00028 F3 0.21504 0.55175 0.53419 1.00000 0.02602 0.04143 0.03745 -0.00280 -0.00309 -0.00897 0.03504 0.00153 0.00012 0.00007 0.00008 0.00000 0.00047 0.00056 0.00053 0.00039 0.00034 0.00037 0.00029 Si1 0.00000 0.50000 0.50000 0.50000 0.02088 0.02309 0.02185 -0.00181 0.00048 -0.00058 0.02194 0.00000 0.00000 0.00000 0.00000 0.00000 0.00032 0.00033 0.00032 0.00018 0.00020 0.00018 0.00023 C1_a 0.39734 0.67471 0.34985 0.89098 0.03410 0.02556 0.02342 0.00345 0.00512 -0.00157 0.02761 0.00295 0.00024 0.00012 0.00013 0.00276 0.00085 0.00077 0.00073 0.00057 0.00059 0.00061 0.00039 H1A_a 0.34978 0.60411 0.34896 0.89098 0.03314 0.00276 0.00000 H1B_a 0.48422 0.68225 0.41560 0.89098 0.03314 0.00276 0.00000 C2_a 0.22870 0.74516 0.36259 0.89098 0.03771 0.03541 0.03790 0.00079 0.01118 0.00497 0.03683 0.00434 0.00032 0.00020 0.00023 0.00276 0.00112 0.00117 0.00113 0.00100 0.00085 0.00084 0.00052 H2A_a 0.16310 0.72887 0.43123 0.89098 0.05524 0.00276 0.00000 H2B_a 0.13950 0.73699 0.29905 0.89098 0.05524 0.00276 0.00000 H2C_a 0.27421 0.81530 0.36576 0.89098 0.05524 0.00276 0.00000 C3_a 0.68648 0.62494 0.25599 0.89098 0.02691 0.02826 0.03115 0.00493 -0.00137 0.00327 0.02881 0.00302 0.00023 0.00012 0.00014 0.00276 0.00080 0.00081 0.00083 0.00061 0.00060 0.00060 0.00041 H3A_a 0.64350 0.55423 0.26624 0.89098 0.03457 0.00276 0.00000 H3B_a 0.76160 0.64467 0.32339 0.89098 0.03457 0.00276 0.00000 C4_a 0.81701 0.62877 0.15696 0.89098 0.02936 0.03843 0.04877 0.00292 0.00866 0.00060 0.03872 0.00613 0.00037 0.00026 0.00029 0.00276 0.00111 0.00155 0.00146 0.00121 0.00080 0.00096 0.00071 H4A_a 0.92619 0.58331 0.17003 0.89098 0.05807 0.00276 0.00000 H4B_a 0.86350 0.69809 0.14711 0.89098 0.05807 0.00276 0.00000 H4C_a 0.74541 0.60737 0.08994 0.89098 0.05807 0.00276 0.00000 C5_a 0.56826 0.80246 0.23627 0.89098 0.03819 0.02176 0.03342 0.00716 0.00234 -0.00317 0.03110 0.00310 0.00026 0.00012 0.00014 0.00276 0.00092 0.00076 0.00087 0.00061 0.00069 0.00063 0.00042 H5A_a 0.64094 0.81141 0.16754 0.89098 0.03732 0.00276 0.00000 H5B_a 0.45038 0.84380 0.22885 0.89098 0.03732 0.00276 0.00000 C6_a 0.68791 0.84212 0.33318 0.89098 0.05007 0.03333 0.04814 -0.00638 0.00304 -0.01453 0.04382 0.00478 0.00051 0.00019 0.00032 0.00276 0.00154 0.00121 0.00169 0.00098 0.00135 0.00092 0.00070 H6A_a 0.71816 0.91360 0.32078 0.89098 0.06572 0.00276 0.00000 H6B_a 0.80702 0.80313 0.34002 0.89098 0.06572 0.00276 0.00000 H6C_a 0.61613 0.83535 0.40156 0.89098 0.06572 0.00276 0.00000 C7_a 0.39252 0.66733 0.14258 0.89098 0.02995 0.03289 0.02483 0.00177 -0.00358 0.00166 0.02930 0.00288 0.00024 0.00013 0.00013 0.00276 0.00082 0.00085 0.00077 0.00060 0.00059 0.00063 0.00041 H7A_a 0.27410 0.70851 0.14277 0.89098 0.03516 0.00276 0.00000 H7B_a 0.46519 0.68728 0.07663 0.89098 0.03516 0.00276 0.00000 C8_a 0.33728 0.55693 0.13121 0.89098 0.03654 0.03422 0.03609 -0.00656 -0.00388 -0.00182 0.03570 0.00332 0.00028 0.00014 0.00018 0.00276 0.00096 0.00096 0.00102 0.00076 0.00077 0.00074 0.00045 H8A_a 0.26082 0.54729 0.06265 0.89098 0.05355 0.00276 0.00000 H8B_a 0.26191 0.53666 0.19496 0.89098 0.05355 0.00276 0.00000 H8C_a 0.45334 0.51539 0.12868 0.89098 0.05355 0.00276 0.00000 N1_a 0.51181 0.69237 0.24591 0.89098 0.02628 0.02191 0.02256 0.00558 0.00076 -0.00009 0.02358 0.00373 0.00031 0.00018 0.00021 0.00276 0.00069 0.00064 0.00062 0.00045 0.00050 0.00048 0.00034 C11_b 0.35061 0.76486 0.23957 0.10902 0.02532 0.02196 0.00163 0.00092 0.00098 0.00276 0.00261 H11A_b 0.27304 0.74059 0.17494 0.10902 0.03039 0.00276 0.00000 H11B_b 0.39303 0.83448 0.22235 0.10902 0.03039 0.00276 0.00000 C12_b 0.22157 0.77020 0.33844 0.10902 0.04316 0.04715 0.00324 0.00190 0.00174 0.00276 0.00666 H12A_b 0.11047 0.81293 0.32008 0.10902 0.06474 0.00276 0.00000 H12B_b 0.29273 0.79918 0.40204 0.10902 0.06474 0.00276 0.00000 H12C_b 0.17801 0.70195 0.35719 0.10902 0.06474 0.00276 0.00000 C13_b 0.64237 0.71356 0.14790 0.10902 0.02693 0.02251 0.00169 0.00095 0.00097 0.00276 0.00270 H13A_b 0.67329 0.78632 0.14032 0.10902 0.03232 0.00276 0.00000 H13B_b 0.56366 0.69341 0.08200 0.10902 0.03232 0.00276 0.00000 C14_b 0.82833 0.65279 0.14981 0.10902 0.02337 0.04250 0.00266 0.00156 0.00204 0.00276 0.00492 H14A_b 0.88662 0.65656 0.07684 0.10902 0.03506 0.00276 0.00000 H14B_b 0.80075 0.58197 0.16758 0.10902 0.03506 0.00276 0.00000 H14C_b 0.91701 0.68081 0.20624 0.10902 0.03506 0.00276 0.00000 C15_b 0.64493 0.73101 0.35251 0.10902 0.04015 0.02384 0.00215 0.00112 0.00118 0.00276 0.00346 H15A_b 0.58391 0.70498 0.42002 0.10902 0.04818 0.00276 0.00000 H15B_b 0.77411 0.70051 0.34897 0.10902 0.04818 0.00276 0.00000 C16_b 0.66410 0.84404 0.36114 0.10902 0.03989 0.04320 0.00435 0.00152 0.00220 0.00276 0.00723 H16A_b 0.72490 0.86170 0.43278 0.10902 0.05983 0.00276 0.00000 H16B_b 0.53686 0.87518 0.35536 0.10902 0.05983 0.00276 0.00000 H16C_b 0.74304 0.86895 0.30090 0.10902 0.05983 0.00276 0.00000 C17_b 0.48218 0.58830 0.27174 0.10902 0.03169 0.02191 0.00196 0.00094 0.00109 0.00276 0.00288 H17A_b 0.40533 0.58320 0.33937 0.10902 0.03803 0.00276 0.00000 H17B_b 0.60408 0.55182 0.28638 0.10902 0.03803 0.00276 0.00000 C18_b 0.37390 0.53601 0.17640 0.10902 0.04004 0.02616 0.00252 0.00137 0.00152 0.00276 0.00409 H18A_b 0.34953 0.46534 0.19631 0.10902 0.06006 0.00276 0.00000 H18B_b 0.45079 0.53832 0.10960 0.10902 0.06006 0.00276 0.00000 H18C_b 0.25175 0.57073 0.16200 0.10902 0.06006 0.00276 0.00000 N11_b 0.52640 0.69872 0.25076 0.10902 0.02628 0.02191 0.02256 0.00558 0.00076 -0.00009 0.02358 0.02987 0.00237 0.00135 0.00165 0.00276 0.00069 0.00064 0.00062 0.00045 0.00050 0.00048 0.00034 O1 0.55138 0.62101 0.63027 1.00000 0.03069 0.06959 0.04775 -0.02591 -0.00046 -0.00014 0.04937 0.00229 0.00018 0.00012 0.00012 0.00000 0.00064 0.00095 0.00076 0.00065 0.00053 0.00059 0.00040 H1WA 0.45649 0.58876 0.59944 1.00000 0.07405 0.03206 0.00272 0.00207 0.00225 0.00000 0.00000 H1WB 0.64823 0.60286 0.59282 1.00000 0.07405 0.04617 0.00271 0.00206 0.00226 0.00000 0.00000 Final Structure Factor Calculation for p21n in P2(1)/n Total number of l.s. parameters = 167 Maximum vector length = 511 Memory required = 4138 / 25039 wR2 = 0.1577 before cycle 20 for 2536 data and 0 / 167 parameters Summary of restraints applied in cycle 20 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 2. 1. 18. 0. 0. 0. 24. 214. 0. 0. rms sigma 0.000 0.020 0.020 0.033 0.000 0.000 0.000 0.010 0.060 0.000 0.000 rms deviation 0.000 0.011 0.014 0.018 0.000 0.000 0.000 0.001 0.010 0.000 0.000 GooF = S = 1.299; Restrained GooF = 1.237 for 259 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0904 * P )^2 + 0.16 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0660 for 2327 Fo > 4sig(Fo) and 0.0712 for all 2536 data wR2 = 0.1577, GooF = S = 1.299, Restrained GooF = 1.237 for all data Occupancy sum of asymmetric unit = 13.50 for non-hydrogen and 22.00 for hydrogen atoms Principal mean square atomic displacements U 0.0414 0.0341 0.0229 F1 0.0378 0.0339 0.0224 F2 0.0456 0.0388 0.0207 F3 0.0244 0.0211 0.0203 Si1 0.0356 0.0279 0.0194 C1_a 0.0489 0.0353 0.0263 C2_a 0.0348 0.0298 0.0218 C3_a 0.0518 0.0378 0.0265 C4_a 0.0388 0.0368 0.0177 C5_a 0.0602 0.0471 0.0241 C6_a 0.0337 0.0323 0.0220 C7_a 0.0431 0.0374 0.0265 C8_a 0.0278 0.0263 0.0166 N1_a 0.0278 0.0263 0.0166 N11_b 0.0868 0.0318 0.0295 O1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.014 0.030 0.044 0.060 0.078 0.096 0.127 0.166 0.254 1.000 Number in group 257. 261. 244. 271. 240. 248. 258. 251. 251. 255. GooF 1.303 1.323 1.161 1.101 1.096 0.907 0.912 0.900 0.733 2.567 K 2.124 1.062 1.003 0.977 0.973 0.990 1.003 1.008 1.016 1.010 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.14 1.31 1.65 inf Number in group 255. 254. 252. 254. 254. 254. 252. 252. 255. 254. GooF 0.911 0.913 0.828 0.930 0.901 0.980 1.008 1.171 1.384 2.749 K 1.042 1.045 1.041 1.035 1.016 1.006 1.007 1.028 1.097 0.956 R1 0.068 0.059 0.051 0.056 0.043 0.038 0.037 0.036 0.052 0.150 Recommended weighting scheme: WGHT 0.0904 0.1573 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)/su Fc/Fc(max) Resolution(A) 1 1 1 645.06 3621.94 9.07 0.728 5.44 -2 1 1 1276.10 5440.90 8.84 0.892 3.27 1 0 3 1268.14 6625.41 8.34 0.985 3.44 0 3 2 1224.63 4185.64 7.95 0.783 3.55 0 0 2 287.99 1041.86 7.00 0.390 6.02 0 0 6 1288.17 3650.62 6.44 0.731 2.01 0 2 1 586.36 2047.12 6.21 0.547 5.79 -1 0 1 1412.19 4339.63 6.14 0.797 6.11 -1 1 6 1461.69 3687.36 5.82 0.735 1.92 -1 1 1 995.82 3058.51 5.22 0.669 5.55 5 6 2 7.81 1.24 5.13 0.013 1.15 -3 4 5 13.75 5.28 4.85 0.028 1.51 1 6 0 2497.73 4943.82 4.67 0.851 2.10 1 4 1 1960.09 6832.43 4.19 1.000 2.89 -2 0 2 3066.72 1964.71 3.97 0.536 3.06 -2 1 2 4010.94 2648.11 3.80 0.623 2.98 1 3 0 933.12 4629.12 3.77 0.823 3.72 0 4 4 8.37 3.49 3.71 0.023 2.23 1 4 3 4130.19 2752.24 3.68 0.635 2.38 2 1 3 5418.80 3486.59 3.67 0.714 2.55 -1 1 4 5244.83 3481.51 3.64 0.714 2.73 -1 4 1 1.35 5.70 3.53 0.029 2.91 3 3 1 5065.91 3425.86 3.52 0.708 2.02 -4 4 3 0.45 3.54 3.44 0.023 1.45 -1 1 2 2870.02 1963.22 3.44 0.536 4.36 -2 2 1 20.75 36.35 3.40 0.073 3.01 0 4 2 112.35 175.97 3.30 0.160 2.90 -2 3 1 2560.23 1806.92 3.15 0.514 2.68 3 3 0 4208.75 2997.61 3.06 0.662 2.06 -1 5 1 3787.49 2704.28 3.04 0.629 2.43 -1 4 9 11.28 5.85 3.04 0.029 1.23 -3 0 3 3700.06 2636.27 3.00 0.621 2.04 3 4 1 3.01 0.74 2.95 0.010 1.87 1 1 3 2866.64 2066.05 2.95 0.550 3.33 -5 1 2 2.28 0.39 2.88 0.008 1.36 5 2 6 3.49 0.20 2.88 0.005 1.12 0 10 5 1.92 0.00 2.87 0.000 1.16 1 3 2 1608.80 1170.52 2.85 0.414 3.15 2 2 4 2900.53 2118.25 2.83 0.557 2.13 2 6 5 59.06 87.51 2.81 0.113 1.46 0 3 1 2152.33 1573.37 2.80 0.480 4.14 1 5 6 10.35 17.70 2.77 0.051 1.55 -2 4 3 2.28 5.66 2.77 0.029 2.08 1 0 5 168.61 120.43 2.74 0.133 2.26 0 4 6 13.76 5.53 2.71 0.028 1.72 3 2 2 2753.14 2039.95 2.70 0.546 2.05 6 0 8 20.18 34.09 2.68 0.071 0.91 -2 4 11 17.84 28.26 2.66 0.064 1.00 1 1 4 52.29 75.31 2.63 0.105 2.68 -1 4 2 2398.91 1789.05 2.63 0.512 2.69 Bond lengths and angles F1 - Distance Angles Si1 1.6880 (0.0008) F1 - F2 - Distance Angles Si1 1.6795 (0.0008) F2 - F3 - Distance Angles Si1 1.6910 (0.0008) F3 - Si1 - Distance Angles F2 1.6795 (0.0008) F2_$2 1.6795 (0.0008) 180.00 F1 1.6880 (0.0008) 89.65 (0.04) 90.35 (0.04) F1_$2 1.6880 (0.0008) 90.35 (0.04) 89.65 (0.04) 180.00 (0.06) F3_$2 1.6910 (0.0008) 89.80 (0.05) 90.20 (0.05) 90.40 (0.05) 89.60 (0.05) F3 1.6910 (0.0008) 90.20 (0.05) 89.80 (0.05) 89.60 (0.05) 90.40 (0.05) 180.00 (0.09) Si1 - F2 F2_$2 F1 F1_$2 F3_$2 C1_a - Distance Angles C2_a 1.5122 (0.0026) N1_a 1.5218 (0.0027) 114.64 (0.18) H1A_a 0.9900 108.60 108.60 H1B_a 0.9900 108.60 108.60 107.57 C1_a - C2_a N1_a H1A_a C2_a - Distance Angles C1_a 1.5122 (0.0026) H2A_a 0.9800 109.47 H2B_a 0.9800 109.47 109.47 H2C_a 0.9800 109.47 109.47 109.47 C2_a - C1_a H2A_a H2B_a C3_a - Distance Angles N1_a 1.5128 (0.0028) C4_a 1.5217 (0.0032) 114.59 (0.18) H3A_a 0.9900 108.62 108.62 H3B_a 0.9900 108.62 108.62 107.57 C3_a - N1_a C4_a H3A_a C4_a - Distance Angles C3_a 1.5217 (0.0032) H4A_a 0.9800 109.47 H4B_a 0.9800 109.47 109.47 H4C_a 0.9800 109.47 109.47 109.47 C4_a - C3_a H4A_a H4B_a C5_a - Distance Angles C6_a 1.5113 (0.0036) N1_a 1.5121 (0.0027) 114.46 (0.18) H5A_a 0.9900 108.65 108.65 H5B_a 0.9900 108.65 108.65 107.59 C5_a - C6_a N1_a H5A_a C6_a - Distance Angles C5_a 1.5113 (0.0035) H6A_a 0.9800 109.47 H6B_a 0.9800 109.47 109.47 H6C_a 0.9800 109.47 109.47 109.47 C6_a - C5_a H6A_a H6B_a C7_a - Distance Angles C8_a 1.5139 (0.0024) N1_a 1.5160 (0.0028) 114.69 (0.16) H7A_a 0.9900 108.59 108.59 H7B_a 0.9900 108.59 108.59 107.56 C7_a - C8_a N1_a H7A_a C8_a - Distance Angles C7_a 1.5139 (0.0024) H8A_a 0.9800 109.47 H8B_a 0.9800 109.47 109.47 H8C_a 0.9800 109.47 109.47 109.47 C8_a - C7_a H8A_a H8B_a N1_a - Distance Angles C5_a 1.5121 (0.0027) C3_a 1.5128 (0.0028) 111.18 (0.16) C7_a 1.5160 (0.0028) 106.59 (0.19) 111.20 (0.16) C1_a 1.5218 (0.0027) 110.76 (0.16) 106.49 (0.19) 110.68 (0.16) N1_a - C5_a C3_a C7_a C11_b - Distance Angles N11_b 1.5101 (0.0164) C12_b 1.5146 (0.0154) 117.13 (1.34) H11A_b 0.9900 108.02 108.02 H11B_b 0.9900 108.02 108.02 107.25 C11_b - N11_b C12_b H11A_b C12_b - Distance Angles C11_b 1.5146 (0.0153) H12A_b 0.9800 109.47 H12B_b 0.9800 109.47 109.47 H12C_b 0.9800 109.47 109.47 109.47 C12_b - C11_b H12A_b H12B_b C13_b - Distance Angles N11_b 1.5114 (0.0164) C14_b 1.5265 (0.0155) 113.18 (1.29) H13A_b 0.9900 108.94 108.94 H13B_b 0.9900 108.94 108.94 107.75 C13_b - N11_b C14_b H13A_b C14_b - Distance Angles C13_b 1.5265 (0.0154) H14A_b 0.9800 109.47 H14B_b 0.9800 109.47 109.47 H14C_b 0.9800 109.47 109.47 109.47 C14_b - C13_b H14A_b H14B_b C15_b - Distance Angles C16_b 1.5026 (0.0167) N11_b 1.5218 (0.0168) 112.33 (1.54) H15A_b 0.9900 109.14 109.14 H15B_b 0.9900 109.14 109.14 107.86 C15_b - C16_b N11_b H15A_b C16_b - Distance Angles C15_b 1.5026 (0.0167) H16A_b 0.9800 109.47 H16B_b 0.9800 109.47 109.47 H16C_b 0.9800 109.47 109.47 109.47 C16_b - C15_b H16A_b H16B_b C17_b - Distance Angles N11_b 1.5137 (0.0167) C18_b 1.5239 (0.0150) 114.23 (1.28) H17A_b 0.9900 108.70 108.70 H17B_b 0.9900 108.70 108.70 107.62 C17_b - N11_b C18_b H17A_b C18_b - Distance Angles C17_b 1.5239 (0.0150) H18A_b 0.9800 109.47 H18B_b 0.9800 109.47 109.47 H18C_b 0.9800 109.47 109.47 109.47 C18_b - C17_b H18A_b H18B_b N11_b - Distance Angles C11_b 1.5101 (0.0163) C13_b 1.5114 (0.0164) 107.69 (1.43) C17_b 1.5137 (0.0167) 113.80 (1.22) 112.22 (1.17) C15_b 1.5218 (0.0167) 109.46 (1.17) 109.42 (1.22) 104.16 (1.45) N11_b - C11_b C13_b C17_b O1 - Distance Angles H1WA 0.8634 (0.0161) H1WB 0.8573 (0.0161) 104.05 (2.06) O1 - H1WA Specified hydrogen bonds (with su's except fixed and riding H) D-H H...A D...A <(DHA) 0.863(16) 1.905(17) 2.7476(15) 165(3) O1-H1WA...F3 0.857(16) 2.059(17) 2.8759(16) 159(3) O1-H1WB...F1_$1 FMAP and GRID set by program FMAP 2 1 11 GRID -3.125 -2 -2 3.125 2 2 R1 = 0.0710 for 2536 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.60 at 0.0887 0.2749 0.9334 [ 0.93 A from H14A ] Deepest hole -0.68 at 0.0187 0.5416 0.5343 [ 0.70 A from SI1 ] Mean = 0.00, Rms deviation from mean = 0.20 e/A^3, Highest memory used = 4235 / 17972 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.9113 0.7251 0.0666 1.00000 0.05 0.60 0.93 H14A 1.09 H4B 1.51 C14 1.78 H14C Q2 1 0.1388 0.6206 0.2788 1.00000 0.05 0.59 1.45 H12C 1.56 H2B 1.69 H1A 1.74 H8B Q3 1 0.6084 0.4953 0.3437 1.00000 0.05 0.54 1.02 H17B 1.25 H3A 1.39 H1WA 1.73 C17 Q4 1 0.2915 0.5045 0.6011 1.00000 0.05 0.50 1.14 F3 1.60 H1WA 1.69 H17B 1.82 H3A Q5 1 0.9879 0.4968 0.0450 1.00000 0.05 0.50 1.95 H4A 2.02 H16B 2.03 H8A 2.22 H8A Q6 1 0.6863 0.5237 0.3835 1.00000 0.05 0.50 1.34 H17B 1.49 H3A 1.55 F3 1.80 H1WA Q7 1 0.1169 0.3630 0.4659 1.00000 0.05 0.50 0.47 F1 1.86 H1WB 2.03 SI1 2.30 H11B Q8 1 0.2290 0.4444 0.5531 1.00000 0.05 0.48 1.36 F1 1.44 F3 1.86 SI1 1.90 H3B Q9 1 0.1952 0.4323 0.2633 1.00000 0.05 0.46 1.43 H18A 1.44 H11B 1.55 H5B 1.68 H8B Q10 1 0.1153 0.3631 0.5578 1.00000 0.05 0.39 0.81 F1 1.59 H15B 1.65 H3B 2.09 SI1 Shortest distances between peaks (including symmetry equivalents) 4 6 0.44 3 6 0.81 3 4 0.95 6 8 1.04 4 8 1.07 5 5 1.10 7 10 1.11 8 10 1.34 7 8 1.68 3 8 1.84 6 10 2.15 4 10 2.29 2 9 2.53 7 9 2.68 2 10 2.69 6 7 2.70 4 7 2.74 3 10 2.92 Time profile in seconds ----------------------- 0.02: 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. 0.72: 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 1.64: Structure factors and derivatives 1.27: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.11: Apply other restraints 0.20: Solve l.s. equations 0.00: Generate HTAB table 0.17: Other dependent quantities, CIF, tables 0.02: Analysis of variance 0.02: Merge reflections for Fourier and .fcf 0.02: Fourier summations 0.02: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + p21n finished at 18:00:47 Total CPU time: 4.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++