+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2005slh0412 started at 10:27:40 on 22-Aug-2005 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2005slh0412 in P2(1)/c CELL 0.71073 15.2643 14.7356 10.5323 90.000 94.988 90.000 ZERR 2.00 0.0004 0.0003 0.0002 0.000 0.001 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H O P S HG UNIT 72 96 16 8 16 4 V = 2360.04 F(000) = 1352.0 Mu = 7.03 mm-1 Cell Wt = 2780.57 Rho = 1.956 MERG 2 OMIT -3.00 55.00 OMIT -1 2 1 FMAP 2 PLAN 5 ACTA BOND $H L.S. 6 TEMP -123.00 WGHT 0.018200 2.423200 EXTI 0.001641 FVAR 0.22767 C1 1 0.688602 0.346177 0.476918 11.00000 0.01211 0.01636 = 0.01900 0.00172 -0.00224 0.00352 AFIX 23 H1A 2 0.646091 0.344217 0.542700 11.00000 -1.20000 H1B 2 0.659193 0.322867 0.395954 11.00000 -1.20000 AFIX 0 C2 1 0.719739 0.442087 0.459562 11.00000 0.01860 0.01526 = 0.02980 0.00233 -0.00359 0.00343 AFIX 137 H2A 2 0.745298 0.465814 0.541486 11.00000 -1.50000 H2B 2 0.669857 0.480104 0.427942 11.00000 -1.50000 H2C 2 0.764308 0.442704 0.397975 11.00000 -1.50000 AFIX 0 C3 1 0.866118 0.161563 0.596962 11.00000 0.01255 0.01100 = 0.01215 0.00211 0.00120 0.00069 C4 1 0.934582 0.126727 0.532623 11.00000 0.01581 0.01708 = 0.01242 -0.00108 0.00121 0.00013 AFIX 43 H4 2 0.923483 0.107337 0.446707 11.00000 -1.20000 AFIX 0 C5 1 1.019239 0.120033 0.593061 11.00000 0.01389 0.02006 = 0.01840 -0.00101 0.00247 0.00381 AFIX 43 H5 2 1.065703 0.095956 0.548910 11.00000 -1.20000 AFIX 0 C6 1 1.034961 0.148820 0.718100 11.00000 0.01183 0.01236 = 0.01828 0.00301 -0.00114 0.00173 C7 1 0.966166 0.182094 0.783961 11.00000 0.01910 0.02289 = 0.01210 -0.00290 -0.00116 0.00318 AFIX 43 H7 2 0.976955 0.200440 0.870375 11.00000 -1.20000 AFIX 0 C8 1 0.882746 0.188276 0.723556 11.00000 0.01325 0.01934 = 0.01475 -0.00158 0.00069 0.00599 AFIX 43 H8 2 0.836110 0.210962 0.768617 11.00000 -1.20000 AFIX 0 C9 1 1.187639 0.110874 0.725631 11.00000 0.01111 0.02840 = 0.03127 -0.00101 0.00147 0.00543 AFIX 137 H9A 2 1.176997 0.046541 0.706393 11.00000 -1.50000 H9B 2 1.241458 0.117143 0.782843 11.00000 -1.50000 H9C 2 1.194301 0.144002 0.646364 11.00000 -1.50000 AFIX 0 C10 1 0.469382 0.293161 0.396361 11.00000 0.01507 0.01766 = 0.04394 -0.00175 -0.00801 -0.00695 AFIX 23 H10A 2 0.509747 0.283249 0.329014 11.00000 -1.20000 H10B 2 0.497073 0.268124 0.477374 11.00000 -1.20000 AFIX 0 C11 1 0.451793 0.391841 0.410528 11.00000 0.03050 0.01590 = 0.02085 0.00022 -0.00385 -0.00686 AFIX 137 H11A 2 0.421377 0.415146 0.331422 11.00000 -1.50000 H11B 2 0.507586 0.424195 0.428511 11.00000 -1.50000 H11C 2 0.414837 0.401149 0.480979 11.00000 -1.50000 AFIX 0 C12 1 0.270073 0.127721 0.287405 11.00000 0.00974 0.01063 = 0.01498 -0.00230 -0.00439 -0.00039 C13 1 0.256332 0.168045 0.167362 11.00000 0.01417 0.01353 = 0.01649 0.00145 0.00056 -0.00071 AFIX 43 H13 2 0.303024 0.199890 0.133168 11.00000 -1.20000 AFIX 0 C14 1 0.175847 0.162129 0.098080 11.00000 0.01556 0.01834 = 0.01313 0.00465 -0.00356 0.00094 AFIX 43 H14 2 0.166998 0.189197 0.016104 11.00000 -1.20000 AFIX 0 C15 1 0.106986 0.115706 0.149760 11.00000 0.01140 0.01447 = 0.01568 -0.00230 -0.00440 0.00039 C16 1 0.120619 0.072788 0.266977 11.00000 0.01259 0.01512 = 0.01523 0.00227 0.00080 -0.00196 AFIX 43 H16 2 0.074516 0.039282 0.299997 11.00000 -1.20000 AFIX 0 C17 1 0.202223 0.079209 0.335655 11.00000 0.01433 0.01507 = 0.01271 0.00093 -0.00173 0.00082 AFIX 43 H17 2 0.211786 0.050234 0.416244 11.00000 -1.20000 AFIX 0 C18 1 -0.045313 0.075191 0.123963 11.00000 0.01016 0.03061 = 0.03120 0.00455 -0.00507 -0.00497 AFIX 137 H18A 2 -0.034885 0.009849 0.133848 11.00000 -1.50000 H18B 2 -0.097192 0.085363 0.064088 11.00000 -1.50000 H18C 2 -0.055235 0.101706 0.206834 11.00000 -1.50000 AFIX 0 O1 3 0.765175 0.291225 0.516135 11.00000 0.01052 0.01124 = 0.01693 0.00095 -0.00306 -0.00046 O2 3 1.114646 0.147397 0.786111 11.00000 0.01188 0.02844 = 0.01842 -0.00224 -0.00375 0.00480 O3 3 0.385880 0.248714 0.362352 11.00000 0.01018 0.01127 = 0.02503 0.00200 -0.00476 -0.00256 O4 3 0.029550 0.116952 0.076044 11.00000 0.01262 0.02678 = 0.01915 0.00605 -0.00666 -0.00298 P1 4 0.759606 0.183215 0.517188 11.00000 0.01107 0.01133 = 0.00927 0.00048 -0.00113 -0.00113 P2 4 0.375101 0.141868 0.374694 11.00000 0.00933 0.01021 = 0.01250 -0.00004 -0.00254 0.00024 S1 5 0.742140 0.129938 0.343649 11.00000 0.01571 0.01868 = 0.00944 -0.00169 0.00101 -0.00437 S2 5 0.661949 0.144243 0.625856 11.00000 0.01533 0.02049 = 0.00954 -0.00158 0.00180 -0.00473 S3 5 0.465055 0.076339 0.276895 11.00000 0.01243 0.02165 = 0.01161 -0.00317 -0.00219 0.00349 S4 5 0.621155 -0.109861 0.440982 11.00000 0.01590 0.01558 = 0.01134 -0.00135 -0.00187 0.00176 HG1 6 0.590100 0.064829 0.438723 11.00000 0.01172 0.01739 = 0.01592 -0.00011 -0.00350 -0.00232 HKLF 4 1.0 0.00 0.00 1.00 0.00 -1.00 0.00 1.00 0.00 0.00 Covalent radii and connectivity table for 2005slh0412 in P2(1)/c C 0.770 H 0.320 O 0.660 P 1.100 S 1.030 HG 1.500 C1 - O1 C2 C2 - C1 C3 - C4 C8 P1 C4 - C3 C5 C5 - C6 C4 C6 - O2 C5 C7 C7 - C8 C6 C8 - C7 C3 C9 - O2 C10 - O3 C11 C11 - C10 C12 - C17 C13 P2 C13 - C14 C12 C14 - C13 C15 C15 - O4 C16 C14 C16 - C15 C17 C17 - C16 C12 C18 - O4 O1 - C1 P1 O2 - C6 C9 O3 - C10 P2 O4 - C15 C18 P1 - O1 C3 S1 S2 P2 - O3 C12 S4_$1 S3 S1 - P1 Hg1 S2 - P1 Hg1 S3 - P2 Hg1 S4 - P2_$1 Hg1 Hg1 - S3 S2 S4 S1 Operators for generating equivalent atoms: $1 -x+1, -y, -z+1 h k l Fo^2 Sigma Why rejected 5 0 3 12.97 2.60 observed but should be systematically absent -7 0 9 25.30 5.68 observed but should be systematically absent 22133 Reflections read, of which 523 rejected -19 =< h =< 19, -17 =< k =< 19, -13 =< l =< 13, Max. 2-theta = 54.99 2 Systematic absence violations 0 Inconsistent equivalents 5390 Unique reflections, of which 0 suppressed R(int) = 0.0320 R(sigma) = 0.0300 Friedel opposites merged Maximum memory for data reduction = 2725 / 53476 Default effective X-H distances for T = -123.0 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 = 3481 / 334225 wR2 = 0.0473 before cycle 1 for 5390 data and 267 / 267 parameters GooF = S = 1.043; Restrained GooF = 1.043 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0182 * P )^2 + 2.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22768 0.00021 0.030 OSF 2 0.00164 0.00008 -0.002 EXTI Mean shift/esd = 0.003 Maximum = -0.086 for U23 Hg1 Max. shift = 0.000 A for H18C Max. dU = 0.000 for O2 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3481 / 334225 wR2 = 0.0472 before cycle 2 for 5390 data and 267 / 267 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0182 * P )^2 + 2.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22767 0.00021 -0.007 OSF 2 0.00164 0.00008 -0.003 EXTI Mean shift/esd = 0.001 Maximum = -0.029 for U23 Hg1 Max. shift = 0.000 A for H2A Max. dU = 0.000 for C14 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3481 / 334225 wR2 = 0.0472 before cycle 3 for 5390 data and 267 / 267 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0182 * P )^2 + 2.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22768 0.00021 0.002 OSF 2 0.00164 0.00008 0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.004 for x Hg1 Max. shift = 0.000 A for H18B Max. dU = 0.000 for C1 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3481 / 334225 wR2 = 0.0472 before cycle 4 for 5390 data and 267 / 267 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0182 * P )^2 + 2.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22768 0.00021 0.001 OSF 2 0.00164 0.00008 0.002 EXTI Mean shift/esd = 0.000 Maximum = -0.004 for x Hg1 Max. shift = 0.000 A for H2B Max. dU = 0.000 for C1 Least-squares cycle 5 Maximum vector length = 511 Memory required = 3481 / 334225 wR2 = 0.0472 before cycle 5 for 5390 data and 267 / 267 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0182 * P )^2 + 2.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22768 0.00021 -0.001 OSF 2 0.00164 0.00008 -0.001 EXTI Mean shift/esd = 0.000 Maximum = -0.004 for x Hg1 Max. shift = 0.000 A for H2C Max. dU = 0.000 for C1 Least-squares cycle 6 Maximum vector length = 511 Memory required = 3481 / 334225 wR2 = 0.0472 before cycle 6 for 5390 data and 267 / 267 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0182 * P )^2 + 2.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.22768 0.00021 0.000 OSF 2 0.00164 0.00008 0.000 EXTI Mean shift/esd = 0.000 Maximum = -0.004 for x Hg1 Max. shift = 0.000 A for H2B Max. dU = 0.000 for C11 Largest correlation matrix elements 0.665 EXTI / OSF 0.641 U33 Hg1 / OSF 0.642 U22 Hg1 / OSF 0.633 U11 Hg1 / OSF Idealized hydrogen atom generation before cycle 7 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.6461 0.3442 0.5427 23 0.990 0.000 C1 O1 C2 H1B 0.6592 0.3229 0.3960 23 0.990 0.000 C1 O1 C2 H2A 0.7453 0.4658 0.5415 137 0.980 0.000 C2 C1 H2A H2B 0.6699 0.4801 0.4279 137 0.980 0.000 C2 C1 H2A H2C 0.7643 0.4427 0.3980 137 0.980 0.000 C2 C1 H2A H4 0.9235 0.1073 0.4467 43 0.950 0.000 C4 C3 C5 H5 1.0657 0.0960 0.5489 43 0.950 0.000 C5 C6 C4 H7 0.9770 0.2004 0.8704 43 0.950 0.000 C7 C8 C6 H8 0.8361 0.2110 0.7686 43 0.950 0.000 C8 C7 C3 H9A 1.1770 0.0465 0.7064 137 0.980 0.000 C9 O2 H9A H9B 1.2415 0.1171 0.7828 137 0.980 0.000 C9 O2 H9A H9C 1.1943 0.1440 0.6464 137 0.980 0.000 C9 O2 H9A H10A 0.5097 0.2832 0.3290 23 0.990 0.000 C10 O3 C11 H10B 0.4971 0.2681 0.4774 23 0.990 0.000 C10 O3 C11 H11A 0.4214 0.4151 0.3314 137 0.980 0.000 C11 C10 H11A H11B 0.5076 0.4242 0.4285 137 0.980 0.000 C11 C10 H11A H11C 0.4148 0.4011 0.4810 137 0.980 0.000 C11 C10 H11A H13 0.3030 0.1999 0.1332 43 0.950 0.000 C13 C14 C12 H14 0.1670 0.1892 0.0161 43 0.950 0.000 C14 C13 C15 H16 0.0745 0.0393 0.3000 43 0.950 0.000 C16 C15 C17 H17 0.2118 0.0502 0.4162 43 0.950 0.000 C17 C16 C12 H18A -0.0349 0.0098 0.1338 137 0.980 0.000 C18 O4 H18A H18B -0.0972 0.0854 0.0641 137 0.980 0.000 C18 O4 H18A H18C -0.0552 0.1017 0.2068 137 0.980 0.000 C18 O4 H18A 2005slh0412 in P2(1)/c ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.68860 0.34618 0.47692 1.00000 0.01211 0.01636 0.01900 0.00172 -0.00224 0.00352 0.01603 0.00498 0.00018 0.00018 0.00026 0.00000 0.00130 0.00131 0.00135 0.00107 0.00106 0.00104 0.00055 H1A 0.64609 0.34422 0.54270 1.00000 0.01924 0.00000 0.00000 H1B 0.65919 0.32287 0.39595 1.00000 0.01924 0.00000 0.00000 C2 0.71974 0.44209 0.45956 1.00000 0.01860 0.01526 0.02980 0.00233 -0.00359 0.00343 0.02155 0.00543 0.00020 0.00018 0.00030 0.00000 0.00150 0.00139 0.00164 0.00115 0.00126 0.00111 0.00063 H2A 0.74530 0.46581 0.54149 1.00000 0.03233 0.00000 0.00000 H2B 0.66986 0.48010 0.42794 1.00000 0.03233 0.00000 0.00000 H2C 0.76431 0.44270 0.39798 1.00000 0.03233 0.00000 0.00000 C3 0.86612 0.16156 0.59696 1.00000 0.01255 0.01100 0.01215 0.00211 0.00120 0.00069 0.01189 0.00464 0.00017 0.00017 0.00024 0.00000 0.00126 0.00118 0.00120 0.00097 0.00099 0.00098 0.00050 C4 0.93458 0.12673 0.53262 1.00000 0.01581 0.01708 0.01242 -0.00108 0.00121 0.00013 0.01511 0.00485 0.00018 0.00018 0.00025 0.00000 0.00134 0.00133 0.00123 0.00105 0.00106 0.00108 0.00054 H4 0.92348 0.10734 0.44671 1.00000 0.01813 0.00000 0.00000 C5 1.01924 0.12003 0.59306 1.00000 0.01389 0.02006 0.01840 -0.00101 0.00247 0.00381 0.01739 0.00500 0.00018 0.00019 0.00026 0.00000 0.00137 0.00137 0.00135 0.00111 0.00110 0.00109 0.00056 H5 1.06570 0.09596 0.54891 1.00000 0.02086 0.00000 0.00000 C6 1.03496 0.14882 0.71810 1.00000 0.01183 0.01236 0.01828 0.00301 -0.00114 0.00173 0.01430 0.00478 0.00017 0.00017 0.00025 0.00000 0.00129 0.00124 0.00134 0.00103 0.00104 0.00100 0.00053 C7 0.96617 0.18209 0.78396 1.00000 0.01910 0.02289 0.01210 -0.00290 -0.00116 0.00318 0.01817 0.00501 0.00018 0.00019 0.00025 0.00000 0.00141 0.00146 0.00126 0.00110 0.00107 0.00116 0.00057 H7 0.97696 0.20044 0.87038 1.00000 0.02181 0.00000 0.00000 C8 0.88275 0.18828 0.72356 1.00000 0.01325 0.01934 0.01475 -0.00158 0.00069 0.00599 0.01581 0.00487 0.00017 0.00018 0.00025 0.00000 0.00131 0.00137 0.00126 0.00108 0.00103 0.00109 0.00054 H8 0.83611 0.21096 0.76862 1.00000 0.01897 0.00000 0.00000 C9 1.18764 0.11087 0.72563 1.00000 0.01111 0.02840 0.03127 -0.00101 0.00147 0.00543 0.02362 0.00560 0.00018 0.00021 0.00030 0.00000 0.00139 0.00160 0.00164 0.00133 0.00121 0.00119 0.00064 H9A 1.17700 0.04654 0.70639 1.00000 0.03543 0.00000 0.00000 H9B 1.24146 0.11714 0.78284 1.00000 0.03543 0.00000 0.00000 H9C 1.19430 0.14400 0.64636 1.00000 0.03543 0.00000 0.00000 C10 0.46938 0.29316 0.39636 1.00000 0.01507 0.01766 0.04394 -0.00175 -0.00801 -0.00695 0.02617 0.00518 0.00019 0.00019 0.00033 0.00000 0.00146 0.00143 0.00190 0.00133 0.00132 0.00115 0.00068 H10A 0.50975 0.28325 0.32901 1.00000 0.03141 0.00000 0.00000 H10B 0.49707 0.26812 0.47737 1.00000 0.03141 0.00000 0.00000 C11 0.45179 0.39184 0.41053 1.00000 0.03050 0.01590 0.02085 0.00022 -0.00385 -0.00686 0.02277 0.00513 0.00021 0.00019 0.00028 0.00000 0.00169 0.00140 0.00147 0.00115 0.00126 0.00123 0.00063 H11A 0.42138 0.41515 0.33142 1.00000 0.03416 0.00000 0.00000 H11B 0.50759 0.42420 0.42851 1.00000 0.03416 0.00000 0.00000 H11C 0.41484 0.40115 0.48098 1.00000 0.03416 0.00000 0.00000 C12 0.27007 0.12772 0.28741 1.00000 0.00974 0.01063 0.01498 -0.00230 -0.00439 -0.00039 0.01210 0.00445 0.00017 0.00017 0.00024 0.00000 0.00121 0.00118 0.00126 0.00099 0.00099 0.00097 0.00050 C13 0.25633 0.16804 0.16736 1.00000 0.01417 0.01353 0.01649 0.00145 0.00056 -0.00071 0.01477 0.00474 0.00018 0.00018 0.00025 0.00000 0.00132 0.00126 0.00129 0.00104 0.00105 0.00102 0.00053 H13 0.30302 0.19989 0.13317 1.00000 0.01773 0.00000 0.00000 C14 0.17585 0.16213 0.09808 1.00000 0.01556 0.01834 0.01313 0.00465 -0.00356 0.00094 0.01595 0.00483 0.00018 0.00018 0.00025 0.00000 0.00135 0.00133 0.00128 0.00106 0.00105 0.00108 0.00055 H14 0.16700 0.18920 0.01610 1.00000 0.01915 0.00000 0.00000 C15 0.10699 0.11571 0.14976 1.00000 0.01141 0.01447 0.01568 -0.00230 -0.00440 0.00039 0.01418 0.00461 0.00017 0.00018 0.00025 0.00000 0.00128 0.00129 0.00129 0.00104 0.00103 0.00103 0.00053 C16 0.12062 0.07279 0.26698 1.00000 0.01259 0.01512 0.01523 0.00227 0.00080 -0.00196 0.01434 0.00485 0.00018 0.00017 0.00025 0.00000 0.00133 0.00129 0.00130 0.00102 0.00105 0.00101 0.00054 H16 0.07452 0.03928 0.30000 1.00000 0.01720 0.00000 0.00000 C17 0.20222 0.07921 0.33565 1.00000 0.01433 0.01507 0.01271 0.00093 -0.00173 0.00082 0.01421 0.00477 0.00018 0.00018 0.00025 0.00000 0.00133 0.00125 0.00126 0.00102 0.00105 0.00104 0.00053 H17 0.21179 0.05023 0.41624 1.00000 0.01705 0.00000 0.00000 C18 -0.04531 0.07519 0.12396 1.00000 0.01016 0.03061 0.03120 0.00455 -0.00507 -0.00497 0.02439 0.00559 0.00019 0.00021 0.00031 0.00000 0.00137 0.00165 0.00169 0.00131 0.00122 0.00118 0.00066 H18A -0.03489 0.00985 0.13385 1.00000 0.03659 0.00000 0.00000 H18B -0.09719 0.08536 0.06409 1.00000 0.03659 0.00000 0.00000 H18C -0.05523 0.10171 0.20683 1.00000 0.03659 0.00000 0.00000 O1 0.76518 0.29123 0.51614 1.00000 0.01052 0.01124 0.01693 0.00095 -0.00306 -0.00046 0.01314 0.00313 0.00011 0.00011 0.00017 0.00000 0.00089 0.00087 0.00091 0.00072 0.00072 0.00070 0.00037 O2 1.11465 0.14740 0.78611 1.00000 0.01188 0.02844 0.01842 -0.00224 -0.00375 0.00480 0.01988 0.00347 0.00012 0.00014 0.00018 0.00000 0.00098 0.00111 0.00098 0.00083 0.00078 0.00082 0.00043 O3 0.38588 0.24871 0.36235 1.00000 0.01018 0.01127 0.02503 0.00200 -0.00476 -0.00256 0.01586 0.00323 0.00012 0.00012 0.00018 0.00000 0.00091 0.00091 0.00101 0.00077 0.00077 0.00071 0.00039 O4 0.02955 0.11695 0.07604 1.00000 0.01262 0.02678 0.01915 0.00605 -0.00666 -0.00298 0.01999 0.00343 0.00012 0.00014 0.00018 0.00000 0.00096 0.00108 0.00099 0.00083 0.00078 0.00081 0.00042 P1 0.75961 0.18322 0.51719 1.00000 0.01107 0.01133 0.00927 0.00048 -0.00113 -0.00113 0.01068 0.00115 0.00004 0.00004 0.00006 0.00000 0.00031 0.00031 0.00029 0.00025 0.00024 0.00025 0.00013 P2 0.37510 0.14187 0.37469 1.00000 0.00933 0.01021 0.01250 -0.00004 -0.00254 0.00024 0.01088 0.00116 0.00004 0.00004 0.00006 0.00000 0.00031 0.00031 0.00031 0.00025 0.00025 0.00024 0.00013 S1 0.74214 0.12994 0.34365 1.00000 0.01571 0.01868 0.00944 -0.00169 0.00101 -0.00437 0.01462 0.00115 0.00004 0.00005 0.00006 0.00000 0.00033 0.00033 0.00029 0.00025 0.00025 0.00026 0.00014 S2 0.66195 0.14424 0.62586 1.00000 0.01533 0.02049 0.00954 -0.00158 0.00180 -0.00473 0.01508 0.00116 0.00004 0.00005 0.00006 0.00000 0.00033 0.00034 0.00029 0.00025 0.00025 0.00026 0.00014 S3 0.46505 0.07634 0.27690 1.00000 0.01243 0.02165 0.01161 -0.00317 -0.00219 0.00349 0.01542 0.00120 0.00004 0.00005 0.00006 0.00000 0.00032 0.00033 0.00031 0.00025 0.00025 0.00026 0.00014 S4 0.62116 -0.10986 0.44098 1.00000 0.01590 0.01558 0.01134 -0.00135 -0.00187 0.00176 0.01445 0.00118 0.00004 0.00004 0.00006 0.00000 0.00033 0.00032 0.00030 0.00024 0.00025 0.00026 0.00014 Hg1 0.59010 0.06483 0.43872 1.00000 0.01172 0.01739 0.01592 -0.00011 -0.00350 -0.00232 0.01528 0.00017 0.00001 0.00001 0.00001 0.00000 0.00007 0.00007 0.00007 0.00004 0.00004 0.00004 0.00005 Final Structure Factor Calculation for 2005slh0412 in P2(1)/c Total number of l.s. parameters = 267 Maximum vector length = 511 Memory required = 3214 / 25039 wR2 = 0.0472 before cycle 7 for 5390 data and 0 / 267 parameters GooF = S = 1.042; Restrained GooF = 1.042 for 0 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0182 * P )^2 + 2.42 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0211 for 4941 Fo > 4sig(Fo) and 0.0253 for all 5390 data wR2 = 0.0472, GooF = S = 1.042, Restrained GooF = 1.042 for all data Occupancy sum of asymmetric unit = 29.00 for non-hydrogen and 24.00 for hydrogen atoms Principal mean square atomic displacements U 0.0209 0.0183 0.0089 C1 0.0328 0.0199 0.0120 C2 0.0139 0.0124 0.0093 C3 0.0173 0.0158 0.0122 C4 0.0220 0.0185 0.0116 C5 0.0201 0.0138 0.0090 C6 0.0260 0.0174 0.0111 C7 0.0235 0.0145 0.0095 C8 0.0321 0.0292 0.0095 C9 0.0484 0.0225 0.0076 C10 0.0361 0.0194 0.0128 C11 0.0193 0.0108 0.0062 C12 0.0175 0.0141 0.0128 C13 0.0220 0.0178 0.0081 C14 0.0208 0.0138 0.0079 C15 0.0181 0.0136 0.0112 C16 0.0168 0.0154 0.0104 C17 0.0387 0.0264 0.0080 C18 0.0196 0.0111 0.0087 O1 0.0311 0.0196 0.0090 O2 0.0284 0.0117 0.0075 O3 0.0331 0.0191 0.0078 O4 0.0133 0.0106 0.0081 P1 0.0151 0.0102 0.0074 P2 0.0219 0.0129 0.0091 S1 0.0234 0.0125 0.0093 S2 0.0244 0.0128 0.0090 S3 0.0192 0.0142 0.0100 S4 0.0201 0.0172 0.0086 Hg1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.026 0.046 0.068 0.092 0.122 0.153 0.190 0.234 0.299 1.000 Number in group 567. 531. 522. 542. 545. 529. 545. 537. 533. 539. GooF 1.103 1.018 1.046 1.053 1.035 0.995 1.009 0.960 1.028 1.159 K 1.292 1.039 0.997 0.979 0.979 0.987 0.994 1.004 1.006 1.009 Resolution(A) 0.77 0.80 0.83 0.87 0.91 0.97 1.05 1.15 1.31 1.65 inf Number in group 572. 507. 568. 515. 532. 552. 525. 538. 545. 536. GooF 0.994 0.934 0.932 0.957 0.927 0.978 0.986 1.027 1.116 1.460 K 0.972 0.993 1.003 1.002 1.008 1.015 1.020 1.017 1.005 0.994 R1 0.054 0.043 0.034 0.033 0.024 0.022 0.018 0.016 0.015 0.018 Recommended weighting scheme: WGHT 0.0180 2.4626 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) 3 2 0 111.69 23.09 4.88 0.011 4.18 0 1 9 14573.92 13053.87 4.02 0.253 1.16 3 4 4 8984.87 10055.32 3.96 0.222 1.92 0 1 2 4426.38 5045.48 3.87 0.157 4.94 -6 4 2 1900.86 1597.85 3.75 0.088 1.99 6 2 5 1209.50 943.01 3.68 0.068 1.52 2 3 3 1161.93 1421.63 3.68 0.083 2.61 -6 6 2 8079.84 7187.99 3.66 0.187 1.70 1 4 0 422.18 306.60 3.59 0.039 3.58 1 3 1 13161.51 14554.51 3.58 0.267 4.23 -1 2 3 821.75 650.16 3.54 0.056 3.14 0 1 4 648.25 487.41 3.53 0.049 2.58 0 2 3 13324.52 14609.24 3.48 0.267 3.16 10 7 4 1603.37 1949.42 3.48 0.098 1.09 12 7 7 1672.15 2182.48 3.28 0.103 0.85 7 1 2 962.83 766.73 3.28 0.061 1.93 16 5 6 625.12 1065.65 3.25 0.072 0.78 9 4 2 1631.95 1361.83 3.23 0.082 1.44 -17 8 5 448.33 711.97 3.22 0.059 0.77 15 1 7 8077.86 9456.22 3.19 0.215 0.81 0 3 1 392.42 289.47 3.19 0.038 4.45 -2 11 11 1630.05 2461.01 3.19 0.110 0.78 -2 1 2 6377.05 7006.94 3.18 0.185 4.31 3 1 1 141.49 77.00 3.12 0.019 4.23 2 6 8 208.81 95.39 3.10 0.022 1.13 8 4 3 246.90 123.11 3.08 0.025 1.48 13 9 4 -63.83 279.97 3.08 0.037 0.88 8 4 2 9355.44 8498.32 3.07 0.204 1.57 -1 5 6 549.60 409.41 3.06 0.045 1.51 6 5 11 773.40 1160.42 3.03 0.075 0.83 -1 3 7 2383.01 2078.79 3.02 0.101 1.44 2 5 5 10759.93 11683.93 2.98 0.239 1.64 -7 2 3 8535.89 9282.84 2.97 0.213 1.86 0 9 10 1343.89 1685.20 2.94 0.091 0.88 12 4 2 303.57 167.37 2.91 0.029 1.15 -10 12 3 11961.82 10589.85 2.91 0.228 0.93 1 5 7 1934.55 1661.47 2.90 0.090 1.32 7 15 5 1130.18 1560.92 2.90 0.087 0.81 0 7 5 270.89 172.46 2.89 0.029 1.49 1 10 3 447.96 325.61 2.87 0.040 1.35 2 0 10 28165.15 25000.01 2.83 0.350 1.03 0 2 7 2752.74 2436.24 2.83 0.109 1.47 15 6 5 247.22 630.25 2.82 0.056 0.83 -3 16 1 1262.18 1964.47 2.82 0.098 0.90 -1 2 5 10096.14 10908.24 2.79 0.231 2.02 0 3 5 90.51 25.92 2.78 0.011 1.93 5 14 2 198.68 108.89 2.78 0.023 0.97 8 3 3 3041.60 2696.70 2.77 0.115 1.53 -11 5 11 -56.56 161.68 2.76 0.028 0.79 4 1 3 12734.95 13753.62 2.73 0.259 2.44 Bond lengths and angles C1 - Distance Angles O1 1.4521 (0.0031) C2 1.5073 (0.0037) 107.63 (0.22) H1A 0.9900 110.18 110.18 H1B 0.9900 110.18 110.18 108.48 C1 - O1 C2 H1A C2 - Distance Angles C1 1.5073 (0.0037) H2A 0.9800 109.47 H2B 0.9800 109.47 109.47 H2C 0.9800 109.47 109.47 109.47 C2 - C1 H2A H2B C3 - Distance Angles C4 1.3921 (0.0036) C8 1.3922 (0.0036) 119.23 (0.24) P1 1.7926 (0.0027) 121.74 (0.20) 118.75 (0.19) C3 - C4 C8 C4 - Distance Angles C3 1.3921 (0.0036) C5 1.3935 (0.0038) 120.62 (0.25) H4 0.9500 119.69 119.69 C4 - C3 C5 C5 - Distance Angles C6 1.3845 (0.0038) C4 1.3935 (0.0038) 119.34 (0.24) H5 0.9500 120.33 120.33 C5 - C6 C4 C6 - Distance Angles O2 1.3570 (0.0032) C5 1.3845 (0.0038) 124.79 (0.23) C7 1.3968 (0.0037) 114.92 (0.23) 120.28 (0.25) C6 - O2 C5 C7 - Distance Angles C8 1.3761 (0.0039) C6 1.3968 (0.0037) 119.94 (0.25) H7 0.9500 120.03 120.03 C7 - C8 C6 C8 - Distance Angles C7 1.3761 (0.0039) C3 1.3922 (0.0036) 120.56 (0.24) H8 0.9500 119.72 119.72 C8 - C7 C3 C9 - Distance Angles O2 1.4354 (0.0032) H9A 0.9800 109.47 H9B 0.9800 109.47 109.47 H9C 0.9800 109.47 109.47 109.47 C9 - O2 H9A H9B C10 - Distance Angles O3 1.4500 (0.0032) C11 1.4885 (0.0039) 107.68 (0.24) H10A 0.9900 110.17 110.17 H10B 0.9900 110.17 110.17 108.47 C10 - O3 C11 H10A C11 - Distance Angles C10 1.4885 (0.0039) H11A 0.9800 109.47 H11B 0.9800 109.47 109.47 H11C 0.9800 109.47 109.47 109.47 C11 - C10 H11A H11B C12 - Distance Angles C17 1.3905 (0.0037) C13 1.3962 (0.0036) 119.45 (0.24) P2 1.7896 (0.0026) 122.32 (0.20) 118.23 (0.19) C12 - C17 C13 C13 - Distance Angles C14 1.3760 (0.0038) C12 1.3962 (0.0036) 120.67 (0.24) H13 0.9500 119.66 119.66 C13 - C14 C12 C14 - Distance Angles C13 1.3760 (0.0038) C15 1.4031 (0.0037) 119.31 (0.24) H14 0.9500 120.34 120.34 C14 - C13 C15 C15 - Distance Angles O4 1.3567 (0.0032) C16 1.3866 (0.0037) 124.86 (0.24) C14 1.4031 (0.0037) 114.59 (0.23) 120.55 (0.24) C15 - O4 C16 C16 - Distance Angles C15 1.3866 (0.0037) C17 1.3882 (0.0039) 119.42 (0.24) H16 0.9500 120.29 120.29 C16 - C15 C17 C17 - Distance Angles C16 1.3882 (0.0039) C12 1.3905 (0.0037) 120.51 (0.24) H17 0.9500 119.74 119.74 C17 - C16 C12 C18 - Distance Angles O4 1.4281 (0.0034) H18A 0.9800 109.47 H18B 0.9800 109.47 109.47 H18C 0.9800 109.47 109.47 109.47 C18 - O4 H18A H18B O1 - Distance Angles C1 1.4521 (0.0031) P1 1.5939 (0.0018) 121.11 (0.16) O1 - C1 O2 - Distance Angles C6 1.3570 (0.0032) C9 1.4354 (0.0032) 117.79 (0.21) O2 - C6 O3 - Distance Angles C10 1.4500 (0.0033) P2 1.5895 (0.0018) 121.48 (0.17) O3 - C10 O4 - Distance Angles C15 1.3567 (0.0032) C18 1.4281 (0.0034) 118.43 (0.21) O4 - C15 P1 - Distance Angles O1 1.5939 (0.0018) C3 1.7926 (0.0027) 97.71 (0.11) S1 1.9858 (0.0009) 113.04 (0.07) 113.88 (0.09) S2 2.0392 (0.0009) 109.10 (0.07) 111.36 (0.09) 111.04 (0.04) P1 - O1 C3 S1 P2 - Distance Angles O3 1.5895 (0.0018) C12 1.7896 (0.0026) 99.66 (0.11) S4_$1 1.9938 (0.0009) 108.63 (0.08) 114.91 (0.09) S3 2.0309 (0.0009) 110.49 (0.08) 107.40 (0.09) 114.71 (0.04) P2 - O3 C12 S4_$1 S1 - Distance Angles P1 1.9858 (0.0009) Hg1 2.7773 (0.0006) 81.62 (0.03) S1 - P1 S2 - Distance Angles P1 2.0392 (0.0009) Hg1 2.4659 (0.0007) 88.92 (0.03) S2 - P1 S3 - Distance Angles P2 2.0309 (0.0009) Hg1 2.4518 (0.0007) 101.54 (0.03) S3 - P2 S4 - Distance Angles P2_$1 1.9938 (0.0009) Hg1 2.6172 (0.0007) 103.38 (0.03) S4 - P2_$1 Hg1 - Distance Angles S3 2.4518 (0.0007) S2 2.4659 (0.0007) 142.00 (0.02) S4 2.6172 (0.0007) 101.76 (0.02) 113.07 (0.02) S1 2.7773 (0.0006) 110.48 (0.02) 78.27 (0.02) 100.76 (0.02) Hg1 - S3 S2 S4 FMAP and GRID set by program FMAP 2 2 19 GRID -1.563 -2 -2 1.563 2 2 R1 = 0.0241 for 5390 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.92 at 0.4109 0.1937 0.5623 [ 1.33 A from S4 ] Deepest hole -1.32 at 0.5540 0.0670 0.4942 [ 0.84 A from HG1 ] Mean = 0.00, Rms deviation from mean = 0.11 e/A^3, Highest memory used = 3283 / 24584 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.5891 -0.1937 0.4377 1.00000 0.05 0.92 1.33 S4 1.98 H10B 2.14 P2 2.26 O3 Q2 1 1.2312 0.0636 0.6792 1.00000 0.05 0.71 0.93 H9A 1.11 C9 1.34 H9C 1.35 H9B Q3 1 0.6152 0.0613 0.3191 1.00000 0.05 0.62 1.35 HG1 2.18 S1 2.31 S3 2.70 H11A Q4 1 0.6227 -0.0189 0.4242 1.00000 0.05 0.56 1.34 HG1 1.35 S4 2.79 P2 2.89 H11A Q5 1 0.5802 0.0557 0.5440 1.00000 0.05 0.55 1.14 HG1 1.95 S2 2.76 S4 2.84 S3 Shortest distances between peaks (including symmetry equivalents) 3 4 1.62 4 5 1.83 3 5 2.47 1 4 2.63 2 4 2.65 2 3 2.98 Time profile in seconds ----------------------- 0.05: 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 0.01: Analyse other restraints etc. 1.77: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.01: OSF, H-atoms from difference map 0.02: Set up l.s. refinement 0.00: Generate idealized H-atoms 4.68: Structure factors and derivatives 6.89: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.01: Apply other restraints 0.50: Solve l.s. equations 0.00: Generate HTAB table 0.05: Other dependent quantities, CIF, tables 0.17: Analysis of variance 0.08: Merge reflections for Fourier and .fcf 0.12: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2005slh0412 finished at 10:27:55 Total CPU time: 14.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++