+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + shelxl started at 11:23:51 on 31-Mar-2009 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008lsh144 in P2(1)2(1)2 CELL 0.71073 11.5691 11.5772 4.6662 90.000 90.000 90.000 ZERR 2.00 0.0004 0.0004 0.0001 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, Z SYMM 1/2 - X, 1/2 + Y, - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N O BR UNIT 26 20 4 2 4 V = 624.98 F(000) = 360.0 Mu = 6.47 mm-1 Cell Wt = 740.10 Rho = 1.966 MERG 2 OMIT -3.00 55.00 TWIN EADP C1 C1B EADP C2 C2B EADP C3 C3B EADP C4 C4B EADP C5 C5B EADP C6 C6B EADP C7 C7B EADP N1 N1B EADP O1 O1B EQIV $1 x, y, z-1 EQIV $2 x, y, z+1 HTAB N1 O1_$1 HTAB N1B O1B_$2 FMAP 2 PLAN 5 SIZE 0.02 0.02 0.30 ACTA HTAB 2.00000 BOND $H L.S. 8 TEMP -153.00 WGHT 0.014000 0.825900 BASF 0.48348 FVAR 0.24317 0.86775 PART 1 C1 1 0.086489 0.306359 0.800209 21.00000 0.01772 0.01486 = 0.01103 -0.00119 -0.00246 0.00171 C2 1 0.188646 0.257942 0.697073 21.00000 0.01662 0.01695 = 0.01239 -0.00347 -0.00104 -0.00358 C3 1 0.225184 0.149595 0.791094 21.00000 0.01983 0.01949 = 0.01802 -0.00536 -0.00246 0.01000 AFIX 43 H3 2 0.292249 0.115020 0.710827 21.00000 -1.20000 AFIX 0 C4 1 0.163460 0.092884 1.001213 21.00000 0.02869 0.01220 = 0.02698 0.00066 -0.00326 0.00219 AFIX 43 H4 2 0.189528 0.020358 1.071162 21.00000 -1.20000 AFIX 0 C5 1 0.063338 0.141845 1.110204 21.00000 0.02640 0.01547 = 0.01640 0.00193 -0.00141 -0.00561 AFIX 43 H5 2 0.021282 0.102783 1.255752 21.00000 -1.20000 AFIX 0 C6 1 0.024249 0.246748 1.009219 21.00000 0.01741 0.01789 = 0.01767 -0.00232 0.00042 0.00127 AFIX 43 H6 2 -0.045441 0.278593 1.082381 21.00000 -1.20000 AFIX 0 C7 1 0.000000 0.500000 0.844414 20.50000 0.01794 0.01515 = 0.00840 0.00000 0.00000 -0.00252 N1 3 0.045567 0.412875 0.684897 21.00000 0.02560 0.01783 = 0.00990 -0.00155 0.00151 0.00709 AFIX 43 H1N 2 0.050103 0.422870 0.498283 21.00000 -1.20000 AFIX 0 O1 4 0.000000 0.500000 1.109327 20.50000 0.02835 0.01540 = 0.00639 0.00000 0.00000 0.00798 BR1 5 0.281616 0.338641 0.430103 21.00000 0.02165 0.02645 = 0.01736 -0.00171 0.00322 -0.00259 PART 2 AFIX 66 SAME C1 > BR1 C1B 1 0.087583 0.307272 1.195066 -21.00000 0.01772 0.01486 = 0.01103 -0.00119 -0.00246 0.00171 C2B 1 0.188397 0.259582 1.305789 -21.00000 0.01662 0.01695 = 0.01239 -0.00347 -0.00104 -0.00358 C3B 1 0.225353 0.151588 1.213331 -21.00000 0.01983 0.01949 = 0.01802 -0.00536 -0.00246 0.01000 AFIX 43 H3B 2 0.294255 0.118995 1.289006 -21.00000 -1.20000 AFIX 65 C4B 1 0.161495 0.091284 1.010149 -21.00000 0.02869 0.01220 = 0.02698 0.00066 -0.00326 0.00219 AFIX 43 H4B 2 0.186753 0.017475 0.946959 -21.00000 -1.20000 AFIX 65 C5B 1 0.060681 0.138973 0.899424 -21.00000 0.02640 0.01547 = 0.01640 0.00193 -0.00141 -0.00561 AFIX 43 H5B 2 0.017037 0.097757 0.760558 -21.00000 -1.20000 AFIX 65 C6B 1 0.023724 0.246966 0.991879 -21.00000 0.01741 0.01789 = 0.01767 -0.00232 0.00042 0.00127 AFIX 43 H6B 2 -0.045178 0.279560 0.916204 -21.00000 -1.20000 AFIX 0 C7B 1 0.000000 0.500000 1.164442 -20.50000 0.01794 0.01515 = 0.00840 0.00000 0.00000 -0.00252 N1B 3 0.047718 0.413075 1.316494 -21.00000 0.02560 0.01783 = 0.00990 -0.00155 0.00151 0.00709 AFIX 43 H1NB 2 0.054700 0.422277 1.502895 -21.00000 -1.20000 AFIX 0 O1B 4 0.000000 0.500000 0.901016 -20.50000 0.02835 0.01540 = 0.00639 0.00000 0.00000 0.00798 BR1B 5 0.278638 0.344160 1.567879 -21.00000 0.02907 0.02813 = 0.02390 0.00508 -0.00554 -0.00527 HKLF 4 1 0 1 0 0 0 1 1 0 0 Covalent radii and connectivity table for 2008lsh144 in P2(1)2(1)2 C 0.770 H 0.320 N 0.700 O 0.660 BR 1.140 C1_a - C2_a C6_a N1_a C2_a - C1_a C3_a Br1_a C3_a - C4_a C2_a C4_a - C3_a C5_a C5_a - C6_a C4_a C6_a - C5_a C1_a C7_a - O1_a N1_$3a N1_a N1_a - C7_a C1_a O1_a - C7_a Br1_a - C2_a C1B_b - C2B_b C6B_b N1B_b C2B_b - C1B_b C3B_b Br1B_b C3B_b - C4B_b C2B_b C4B_b - C3B_b C5B_b C5B_b - C6B_b C4B_b C6B_b - C5B_b C1B_b C7B_b - O1B_b N1B_$3b N1B_b N1B_b - C7B_b C1B_b O1B_b - C7B_b Br1B_b - C2B_b Operators for generating equivalent atoms: $1 x, y, z-1 $2 x, y, z+1 $3 -x, -y+1, z 7284 Reflections read, of which 34 rejected -15 =< h =< 13, -13 =< k =< 15, -6 =< l =< 5, Max. 2-theta = 54.95 0 Systematic absence violations 0 Inconsistent equivalents 1415 Unique reflections, of which 0 suppressed R(int) = 0.0432 R(sigma) = 0.0335 Friedel opposites not merged Maximum memory for data reduction = 1970 / 14003 Special position constraints for C7_a x = 0.0000 y = 0.5000 U23 = 0 U13 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for O1_a x = 0.0000 y = 0.5000 U23 = 0 U13 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for C7B_b x = 0.0000 y = 0.5000 U23 = 0 U13 = 0 sof = 0.50000 Input constraints retained (at least in part) for sof Special position constraints for O1B_b x = 0.0000 y = 0.5000 U23 = 0 U13 = 0 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 = 2375 / 137102 wR2 = 0.0554 before cycle 1 for 1415 data and 105 / 105 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. 22. 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 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 0.157; Restrained GooF = 0.156 for 22 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0140 * P )^2 + 0.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.76958 0.00148 355.263 OSF 2 0.86637 0.00265 -0.520 FVAR 2 3 0.48633 0.01468 0.194 BASF 1 Mean shift/esd = 3.633 Maximum = 355.263 for OSF Max. shift = 0.013 A for O1B_b Max. dU =-0.001 for C4_a Least-squares cycle 2 Maximum vector length = 511 Memory required = 2375 / 137102 wR2 = 0.0600 before cycle 2 for 1415 data and 105 / 105 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. 22. 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 0.014 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.095; Restrained GooF = 1.088 for 22 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0140 * P )^2 + 0.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.76953 0.00154 -0.029 OSF 2 0.86706 0.00283 0.244 FVAR 2 3 0.48493 0.01683 -0.083 BASF 1 Mean shift/esd = 0.120 Maximum = 0.414 for U12 C2_a Max. shift = 0.006 A for N1B_b Max. dU = 0.000 for C4_a Least-squares cycle 3 Maximum vector length = 511 Memory required = 2375 / 137102 wR2 = 0.0598 before cycle 3 for 1415 data and 105 / 105 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. 22. 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 0.014 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.093; Restrained GooF = 1.085 for 22 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0140 * P )^2 + 0.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.76900 0.00154 -0.345 OSF 2 0.86775 0.00283 0.243 FVAR 2 3 0.48356 0.01680 -0.081 BASF 1 Mean shift/esd = 0.122 Maximum = 0.402 for U12 C2_a Max. shift = 0.006 A for N1B_b Max. dU = 0.000 for C4_a Least-squares cycle 4 Maximum vector length = 511 Memory required = 2375 / 137102 wR2 = 0.0597 before cycle 4 for 1415 data and 105 / 105 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. 22. 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 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.092; Restrained GooF = 1.084 for 22 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0140 * P )^2 + 0.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.76897 0.00153 -0.022 OSF 2 0.86775 0.00283 0.000 FVAR 2 3 0.48358 0.01678 0.001 BASF 1 Mean shift/esd = 0.006 Maximum = -0.034 for y Br1B_b Max. shift = 0.000 A for O1B_b Max. dU = 0.000 for Br1B_b Least-squares cycle 5 Maximum vector length = 511 Memory required = 2375 / 137102 wR2 = 0.0597 before cycle 5 for 1415 data and 105 / 105 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. 22. 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 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.092; Restrained GooF = 1.084 for 22 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0140 * P )^2 + 0.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.76896 0.00153 -0.002 OSF 2 0.86775 0.00283 0.000 FVAR 2 3 0.48360 0.01678 0.001 BASF 1 Mean shift/esd = 0.002 Maximum = 0.010 for x Br1B_b Max. shift = 0.000 A for H5B_b Max. dU = 0.000 for C4_a Least-squares cycle 6 Maximum vector length = 511 Memory required = 2375 / 137102 wR2 = 0.0597 before cycle 6 for 1415 data and 105 / 105 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. 22. 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 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.092; Restrained GooF = 1.084 for 22 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0140 * P )^2 + 0.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.76896 0.00153 -0.001 OSF 2 0.86775 0.00283 0.001 FVAR 2 3 0.48360 0.01678 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.001 for FVAR 2 Max. shift = 0.000 A for C7B_b Max. dU = 0.000 for Br1B_b Least-squares cycle 7 Maximum vector length = 511 Memory required = 2375 / 137102 wR2 = 0.0597 before cycle 7 for 1415 data and 105 / 105 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. 22. 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 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.092; Restrained GooF = 1.084 for 22 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0140 * P )^2 + 0.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.76896 0.00153 0.000 OSF 2 0.86776 0.00283 0.000 FVAR 2 3 0.48360 0.01678 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.001 for z Br1B_b Max. shift = 0.000 A for O1B_b Max. dU = 0.000 for C7_a Least-squares cycle 8 Maximum vector length = 511 Memory required = 2375 / 137102 wR2 = 0.0597 before cycle 8 for 1415 data and 105 / 105 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. 22. 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 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.092; Restrained GooF = 1.084 for 22 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0140 * P )^2 + 0.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.76896 0.00153 0.001 OSF 2 0.86776 0.00283 0.000 FVAR 2 3 0.48360 0.01678 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.001 for OSF Max. shift = 0.000 A for O1B_b Max. dU = 0.000 for Br1B_b Largest correlation matrix elements 0.909 z Br1B_b / z Br1_a -0.731 U33 Br1B_b / z Br1_a -0.668 z O1B_b / z C7_a 0.901 z O1B_b / z C7B_b 0.726 U33 Br1_a / z Br1_a 0.629 U13 Br1B_b / U13 Br1_a -0.818 z C7B_b / U33 O1_a -0.717 z O1B_b / U33 C7_a -0.621 z C7B_b / U33 C7_a 0.816 z Br1_a / FVAR 2 -0.707 U33 Br1B_b / z Br1B_b 0.617 U33 O1_a / z C7_a 0.798 z Br1B_b / FVAR 2 -0.696 z C7B_b / z C7_a -0.566 y C1B_b / rotZ C1B_b -0.790 U33 Br1B_b / FVAR 2 -0.691 x C1B_b / rotZ C1B_b -0.540 x Br1B_b / U13 Br1_a -0.781 z O1B_b / U33 O1_a 0.690 z C1B_b / rotX C1B_b 0.524 U23 Br1B_b / U23 Br1_a 0.763 z Br1B_b / U33 Br1_a 0.680 U33 Br1_a / FVAR 2 0.520 U13 Br1B_b / x Br1_a Idealized hydrogen atom generation before cycle 9 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H3 0.2922 0.1150 0.7108 43 0.950 0.000 C3_a C4_a C2_a H4 0.1895 0.0204 1.0712 43 0.950 0.000 C4_a C3_a C5_a H5 0.0213 0.1028 1.2557 43 0.950 0.000 C5_a C6_a C4_a H6 -0.0454 0.2786 1.0824 43 0.950 0.000 C6_a C5_a C1_a H1N 0.0501 0.4229 0.4983 43 0.880 0.000 N1_a C7_a C1_a H3B 0.2943 0.1190 1.2890 43 0.950 0.000 C3B_b C4B_b C2B_b H4B 0.1867 0.0175 0.9470 43 0.950 0.000 C4B_b C3B_b C5B_b H5B 0.0170 0.0978 0.7606 43 0.950 0.000 C5B_b C6B_b C4B_b H6B -0.0452 0.2796 0.9162 43 0.950 0.000 C6B_b C5B_b C1B_b H1NB 0.0547 0.4223 1.5029 43 0.880 0.000 N1B_b C7B_b C1B_b 2008lsh144 in P2(1)2(1)2 ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1_a 0.08649 0.30636 0.80021 0.86776 0.01772 0.01487 0.01103 -0.00119 -0.00245 0.00171 0.01454 0.00598 0.00030 0.00029 0.00075 0.00283 0.00167 0.00157 0.00158 0.00116 0.00133 0.00125 0.00069 C2_a 0.18865 0.25794 0.69707 0.86776 0.01662 0.01697 0.01238 -0.00347 -0.00104 -0.00359 0.01532 0.00579 0.00028 0.00030 0.00074 0.00283 0.00165 0.00161 0.00153 0.00128 0.00122 0.00126 0.00069 C3_a 0.22519 0.14960 0.79109 0.86776 0.01983 0.01949 0.01802 -0.00536 -0.00245 0.01001 0.01911 0.00599 0.00033 0.00029 0.00069 0.00283 0.00162 0.00165 0.00153 0.00132 0.00144 0.00165 0.00068 H3_a 0.29225 0.11502 0.71082 0.86776 0.02293 0.00283 0.00000 C4_a 0.16346 0.09288 1.00121 0.86776 0.02870 0.01220 0.02697 0.00066 -0.00326 0.00220 0.02262 0.00713 0.00041 0.00033 0.00098 0.00283 0.00163 0.00143 0.00195 0.00118 0.00141 0.00128 0.00073 H4_a 0.18953 0.02036 1.07116 0.86776 0.02715 0.00283 0.00000 C5_a 0.06334 0.14185 1.11020 0.86776 0.02641 0.01548 0.01640 0.00193 -0.00141 -0.00561 0.01943 0.00591 0.00032 0.00029 0.00074 0.00283 0.00178 0.00170 0.00170 0.00138 0.00142 0.00137 0.00076 H5_a 0.02129 0.10278 1.25575 0.86776 0.02332 0.00283 0.00000 C6_a 0.02425 0.24675 1.00922 0.86776 0.01741 0.01789 0.01767 -0.00232 0.00042 0.00126 0.01766 0.00721 0.00036 0.00038 0.00100 0.00283 0.00140 0.00139 0.00154 0.00108 0.00106 0.00110 0.00061 H6_a -0.04544 0.27859 1.08238 0.86776 0.02119 0.00283 0.00000 C7_a 0.00000 0.50000 0.84441 0.43388 0.01792 0.01515 0.00841 0.00000 0.00000 -0.00252 0.01383 0.00635 0.00000 0.00000 0.00136 0.00141 0.00257 0.00262 0.00328 0.00000 0.00000 0.00211 0.00139 N1_a 0.04557 0.41287 0.68490 0.86776 0.02561 0.01783 0.00991 -0.00156 0.00151 0.00709 0.01778 0.00560 0.00027 0.00026 0.00068 0.00283 0.00158 0.00151 0.00142 0.00114 0.00121 0.00124 0.00065 H1N_a 0.05010 0.42287 0.49829 0.86776 0.02134 0.00283 0.00000 O1_a 0.00000 0.50000 1.10933 0.43388 0.02836 0.01540 0.00639 0.00000 0.00000 0.00798 0.01672 0.00354 0.00000 0.00000 0.00076 0.00141 0.00198 0.00179 0.00278 0.00000 0.00000 0.00155 0.00103 Br1_a 0.28162 0.33864 0.43010 0.86776 0.02165 0.02645 0.01736 -0.00171 0.00322 -0.00259 0.02182 0.00116 0.00004 0.00004 0.00020 0.00283 0.00018 0.00019 0.00033 0.00020 0.00021 0.00018 0.00014 C1B_b 0.08758 0.30727 1.19506 0.13224 0.01772 0.01487 0.01103 -0.00119 -0.00245 0.00171 0.01454 0.02225 0.00130 0.00107 0.00374 0.00283 0.00167 0.00157 0.00158 0.00116 0.00133 0.00125 0.00069 C2B_b 0.18840 0.25959 1.30578 0.13224 0.01662 0.01697 0.01238 -0.00347 -0.00104 -0.00359 0.01532 0.01687 0.00111 0.00112 0.00293 0.00283 0.00165 0.00161 0.00153 0.00128 0.00122 0.00126 0.00069 C3B_b 0.22535 0.15159 1.21333 0.13224 0.01983 0.01949 0.01802 -0.00536 -0.00245 0.01001 0.01911 0.02442 0.00127 0.00126 0.00357 0.00283 0.00162 0.00165 0.00153 0.00132 0.00144 0.00165 0.00068 H3B_b 0.29425 0.11900 1.28900 0.13224 0.02293 0.00283 0.00000 C4B_b 0.16149 0.09128 1.01016 0.13224 0.02870 0.01220 0.02697 0.00066 -0.00326 0.00220 0.02262 0.02420 0.00168 0.00115 0.00396 0.00283 0.00163 0.00143 0.00195 0.00118 0.00141 0.00128 0.00073 H4B_b 0.18674 0.01747 0.94697 0.13224 0.02715 0.00283 0.00000 C5B_b 0.06067 0.13897 0.89944 0.13224 0.02641 0.01548 0.01640 0.00193 -0.00141 -0.00561 0.01943 0.01715 0.00157 0.00137 0.00373 0.00283 0.00178 0.00170 0.00170 0.00138 0.00142 0.00137 0.00076 H5B_b 0.01703 0.09775 0.76059 0.13224 0.02332 0.00283 0.00000 C6B_b 0.02372 0.24696 0.99189 0.13224 0.01741 0.01789 0.01767 -0.00232 0.00042 0.00126 0.01766 0.02269 0.00131 0.00143 0.00406 0.00283 0.00140 0.00139 0.00154 0.00108 0.00106 0.00110 0.00061 H6B_b -0.04519 0.27956 0.91622 0.13224 0.02119 0.00283 0.00000 C7B_b 0.00000 0.50000 1.16443 0.06612 0.01792 0.01515 0.00841 0.00000 0.00000 -0.00252 0.01383 0.04370 0.00000 0.00000 0.00936 0.00141 0.00257 0.00262 0.00328 0.00000 0.00000 0.00211 0.00139 N1B_b 0.04771 0.41307 1.31648 0.13224 0.02561 0.01783 0.00991 -0.00156 0.00151 0.00709 0.01778 0.03330 0.00172 0.00133 0.00411 0.00283 0.00158 0.00151 0.00142 0.00114 0.00121 0.00124 0.00065 H1NB_b 0.05469 0.42227 1.50288 0.13224 0.02134 0.00283 0.00000 O1B_b 0.00000 0.50000 0.90101 0.06612 0.02836 0.01540 0.00639 0.00000 0.00000 0.00798 0.01672 0.04044 0.00000 0.00000 0.00867 0.00141 0.00198 0.00179 0.00278 0.00000 0.00000 0.00155 0.00103 Br1B_b 0.27864 0.34416 1.56788 0.13224 0.02907 0.02813 0.02390 0.00508 -0.00554 -0.00528 0.02703 0.00798 0.00028 0.00027 0.00145 0.00283 0.00153 0.00146 0.00252 0.00165 0.00179 0.00149 0.00105 Final Structure Factor Calculation for 2008lsh144 in P2(1)2(1)2 Total number of l.s. parameters = 105 Maximum vector length = 511 Memory required = 2272 / 26068 wR2 = 0.0597 before cycle 9 for 1415 data and 2 / 105 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. 22. 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 0.013 0.000 0.000 0.000 0.000 0.000 0.000 0.000 GooF = S = 1.092; Restrained GooF = 1.084 for 22 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0140 * P )^2 + 0.83 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0276 for 1376 Fo > 4sig(Fo) and 0.0295 for all 1415 data wR2 = 0.0597, GooF = S = 1.092, Restrained GooF = 1.084 for all data Occupancy sum of asymmetric unit = 9.00 for non-hydrogen and 5.00 for hydrogen atoms Principal mean square atomic displacements U 0.0194 0.0141 0.0101 C1_a 0.0208 0.0157 0.0094 C2_a 0.0319 0.0164 0.0091 C3_a 0.0313 0.0247 0.0118 C4_a 0.0291 0.0165 0.0127 C5_a 0.0203 0.0178 0.0149 C6_a 0.0194 0.0137 0.0084 C7_a 0.0298 0.0146 0.0089 N1_a 0.0322 0.0116 0.0064 O1_a 0.0284 0.0215 0.0156 Br1_a 0.0194 0.0141 0.0101 C1B_b 0.0208 0.0157 0.0094 C2B_b 0.0319 0.0164 0.0091 C3B_b 0.0313 0.0247 0.0118 C4B_b 0.0291 0.0165 0.0127 C5B_b 0.0203 0.0178 0.0149 C6B_b 0.0194 0.0137 0.0084 C7B_b 0.0298 0.0146 0.0089 N1B_b 0.0322 0.0116 0.0064 O1B_b 0.0379 0.0233 0.0199 Br1B_b Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.055 0.080 0.102 0.121 0.141 0.166 0.194 0.235 0.325 1.000 Number in group 142. 142. 142. 144. 137. 147. 140. 138. 141. 142. GooF 1.430 0.998 1.109 1.131 1.159 0.920 1.008 0.990 1.019 1.073 K 1.200 0.983 0.966 0.975 0.977 0.994 1.012 1.007 1.012 1.002 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.98 1.05 1.15 1.34 1.68 inf Number in group 145. 139. 146. 141. 139. 141. 140. 142. 143. 139. GooF 1.171 1.088 1.151 1.026 1.039 1.082 0.893 1.012 1.044 1.350 K 0.975 0.981 1.004 1.015 1.018 1.015 1.010 1.007 1.003 0.998 R1 0.062 0.067 0.047 0.040 0.032 0.028 0.022 0.019 0.017 0.016 Recommended weighting scheme: WGHT 0.0121 0.8602 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) 1 6 0 18.82 3.62 4.03 0.015 1.90 3 0 2 356.67 445.12 3.82 0.167 2.00 -6 5 4 35.35 3.39 3.68 0.015 0.92 14 4 0 205.66 366.71 3.65 0.152 0.79 1 0 1 609.73 728.54 3.61 0.214 4.33 -1 14 2 122.33 195.61 3.40 0.111 0.78 3 0 1 802.33 933.65 3.26 0.242 2.97 13 4 0 317.31 223.69 3.26 0.119 0.85 0 14 1 60.96 5.87 3.19 0.019 0.81 0 8 0 85.87 47.95 3.04 0.055 1.45 -10 9 1 191.45 274.72 3.04 0.132 0.85 6 0 2 22.85 3.31 2.94 0.014 1.49 6 1 0 1318.78 1461.73 2.92 0.303 1.90 7 12 2 202.63 277.80 2.91 0.132 0.78 -11 8 1 213.80 283.45 2.87 0.134 0.84 6 5 4 28.41 3.32 2.86 0.014 0.92 8 8 1 123.87 170.84 2.79 0.104 1.00 -6 3 5 73.37 118.48 2.77 0.086 0.82 1 5 3 2474.57 2266.59 2.65 0.378 1.28 -7 7 2 342.97 287.10 2.59 0.134 1.05 3 6 0 586.30 519.93 2.58 0.181 1.73 5 6 0 41.40 24.71 2.56 0.039 1.48 -1 9 4 66.09 102.96 2.56 0.081 0.86 8 0 2 37.47 17.82 2.54 0.033 1.23 4 12 3 8.84 40.39 2.51 0.050 0.79 3 11 1 27.34 50.20 2.50 0.056 0.99 3 1 3 1082.59 1203.48 2.49 0.275 1.43 -13 7 1 127.42 178.69 2.47 0.106 0.77 -7 11 1 34.16 57.60 2.46 0.060 0.87 -13 6 1 123.61 173.91 2.46 0.105 0.80 0 8 2 24.83 12.25 2.44 0.028 1.23 10 8 0 23.78 1.50 2.44 0.010 0.90 2 1 0 859.61 774.25 2.42 0.221 5.17 8 7 4 64.05 100.15 2.42 0.079 0.80 5 11 0 46.93 22.38 2.40 0.038 0.96 12 1 3 60.58 102.96 2.37 0.081 0.82 2 11 4 -12.80 9.94 2.36 0.025 0.77 0 1 2 571.10 646.58 2.35 0.202 2.29 -1 5 3 2451.92 2276.56 2.34 0.379 1.28 6 0 4 98.64 71.87 2.30 0.067 1.00 8 1 1 2201.11 2370.85 2.30 0.386 1.37 0 5 2 525.17 463.12 2.27 0.171 1.64 -1 5 1 1900.12 1775.00 2.27 0.334 2.04 13 0 2 13.11 42.03 2.23 0.051 0.83 -8 8 1 134.19 171.76 2.22 0.104 1.00 2 4 1 571.95 637.21 2.22 0.200 2.26 -6 1 5 428.52 363.48 2.22 0.151 0.84 4 13 1 323.54 260.25 2.21 0.128 0.84 8 5 3 198.81 161.90 2.20 0.101 0.96 14 2 0 94.76 61.42 2.18 0.062 0.82 Bond lengths and angles C1_a - Distance Angles C2_a 1.3938 (0.0047) C6_a 1.3950 (0.0056) 118.69 (0.32) N1_a 1.4263 (0.0043) 119.93 (0.31) 121.34 (0.33) C1_a - C2_a C6_a C2_a - Distance Angles C1_a 1.3938 (0.0047) C3_a 1.3945 (0.0047) 120.68 (0.33) Br1_a 1.8925 (0.0034) 120.71 (0.26) 118.61 (0.26) C2_a - C1_a C3_a C3_a - Distance Angles C4_a 1.3792 (0.0057) C2_a 1.3945 (0.0047) 119.66 (0.34) H3_a 0.9500 120.17 120.17 C3_a - C4_a C2_a C4_a - Distance Angles C3_a 1.3792 (0.0057) C5_a 1.3862 (0.0055) 119.92 (0.36) H4_a 0.9500 120.04 120.04 C4_a - C3_a C5_a C5_a - Distance Angles C6_a 1.3790 (0.0052) C4_a 1.3862 (0.0055) 120.58 (0.38) H5_a 0.9500 119.71 119.71 C5_a - C6_a C4_a C6_a - Distance Angles C5_a 1.3790 (0.0052) C1_a 1.3950 (0.0056) 120.35 (0.37) H6_a 0.9500 119.82 119.82 C6_a - C5_a C1_a C7_a - Distance Angles O1_a 1.2362 (0.0064) N1_$3a 1.3599 (0.0047) 123.18 (0.25) N1_a 1.3599 (0.0047) 123.18 (0.25) 113.63 (0.51) C7_a - O1_a N1_$3a N1_a - Distance Angles C7_a 1.3599 (0.0047) C1_a 1.4263 (0.0043) 124.30 (0.35) H1N_a 0.8800 117.85 117.85 N1_a - C7_a C1_a O1_a - Distance Angles C7_a 1.2362 (0.0064) O1_a - Br1_a - Distance Angles C2_a 1.8925 (0.0035) Br1_a - C1B_b - Distance Angles C2B_b 1.3900 C6B_b 1.3900 120.00 N1B_b 1.4262 (0.0137) 117.70 (1.11) 122.03 (1.12) C1B_b - C2B_b C6B_b C2B_b - Distance Angles C1B_b 1.3900 C3B_b 1.3900 120.00 Br1B_b 1.8827 (0.0100) 120.01 (0.74) 119.92 (0.74) C2B_b - C1B_b C3B_b C3B_b - Distance Angles C4B_b 1.3900 C2B_b 1.3900 120.00 H3B_b 0.9500 120.00 120.00 C3B_b - C4B_b C2B_b C4B_b - Distance Angles C3B_b 1.3900 C5B_b 1.3900 120.00 H4B_b 0.9500 120.00 120.00 C4B_b - C3B_b C5B_b C5B_b - Distance Angles C6B_b 1.3900 C4B_b 1.3900 120.00 H5B_b 0.9500 120.00 120.00 C5B_b - C6B_b C4B_b C6B_b - Distance Angles C5B_b 1.3900 C1B_b 1.3900 120.00 H6B_b 0.9500 120.00 120.00 C6B_b - C5B_b C1B_b C7B_b - Distance Angles O1B_b 1.2292 (0.0190) N1B_$3b 1.3494 (0.0177) 121.72 (1.54) N1B_b 1.3494 (0.0177) 121.72 (1.54) 116.56 (3.08) C7B_b - O1B_b N1B_$3b N1B_b - Distance Angles C7B_b 1.3494 (0.0177) C1B_b 1.4262 (0.0137) 124.33 (1.60) H1NB_b 0.8800 117.84 117.84 N1B_b - C7B_b C1B_b O1B_b - Distance Angles C7B_b 1.2292 (0.0190) O1B_b - Br1B_b - Distance Angles C2B_b 1.8827 (0.0100) Br1B_b - Specified hydrogen bonds (with esds except fixed and riding H) D-H H...A D...A <(DHA) 0.88 2.10 2.917(5) 153.2 N1_a-H1N_a...O1_$1a 0.88 2.16 2.96(3) 150.9 N1B_b-H1NB_b...O1B_$2b Hydrogen bonds with H..A < r(A) + 2.000 Angstroms and 110 deg. D-H d(D-H) d(H..A)