+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2007src0763 started at 17:32:31 on 28-Jun-2007 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2007SRC0763 in Pna2(1) CELL 0.71073 15.4076 12.9924 9.3800 90.000 90.000 90.000 ZERR 4.00 0.0003 0.0004 0.0003 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, 1/2 + Z SYMM 1/2 - X, 1/2 + Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, Z SFAC C H N O S CL UNIT 76 112 4 8 4 4 V = 1877.70 F(000) = 792.0 Mu = 0.33 mm-1 Cell Wt = 1479.74 Rho = 1.309 MERG 2 OMIT -3.00 57.00 FMAP 2 PLAN 10 SIZE 0.10 0.10 0.24 TWIN BASF 0.4 ACTA BOND $H WGHT 0.06270 4.79270 L.S. 10 TEMP -153.00 FVAR 0.83136 C1 1 0.658799 0.008406 0.415472 11.00000 0.02690 0.01815 = 0.04607 -0.00010 0.00593 0.00489 AFIX 137 H1A 2 0.652714 0.007778 0.311477 11.00000 -1.50000 H1B 2 0.665667 -0.062267 0.450194 11.00000 -1.50000 H1C 2 0.709932 0.049001 0.441916 11.00000 -1.50000 AFIX 0 C2 1 0.578053 0.056165 0.482082 11.00000 0.02125 0.01594 = 0.03330 -0.00073 -0.00155 0.00082 AFIX 13 H2 2 0.581320 0.047335 0.587852 11.00000 -1.20000 AFIX 0 C3 1 0.566900 0.171492 0.448696 11.00000 0.02355 0.01789 = 0.02933 0.00055 -0.00007 -0.00008 AFIX 13 H3 2 0.617378 0.208095 0.492518 11.00000 -1.20000 AFIX 0 C4 1 0.483145 0.217725 0.516678 11.00000 0.02472 0.01658 = 0.01800 -0.00069 0.00111 -0.00135 AFIX 13 H4 2 0.451577 0.161778 0.568367 11.00000 -1.20000 AFIX 0 C5 1 0.471680 0.215944 0.255315 11.00000 0.02230 0.03069 = 0.01651 0.00086 0.00486 0.00509 AFIX 23 H5A 2 0.445693 0.150650 0.221581 11.00000 -1.20000 H5B 2 0.464517 0.268972 0.180440 11.00000 -1.20000 AFIX 0 C6 1 0.564667 0.201708 0.291558 11.00000 0.02880 0.03083 = 0.03549 -0.00290 0.00645 0.00462 AFIX 23 H6A 2 0.597330 0.266335 0.275815 11.00000 -1.20000 H6B 2 0.590654 0.146868 0.231997 11.00000 -1.20000 AFIX 0 C7 1 0.498927 0.307023 0.620101 11.00000 0.02253 0.01589 = 0.02108 -0.00405 0.00319 -0.00269 AFIX 13 H7 2 0.440610 0.334350 0.647614 11.00000 -1.20000 AFIX 0 C8 1 0.550592 0.398215 0.556762 11.00000 0.02748 0.01256 = 0.03073 -0.00201 -0.00139 -0.00011 AFIX 23 H8A 2 0.609263 0.374570 0.528849 11.00000 -1.20000 H8B 2 0.520826 0.423802 0.470200 11.00000 -1.20000 AFIX 0 C9 1 0.558442 0.485379 0.665201 11.00000 0.02143 0.01899 = 0.04275 -0.00966 0.00164 -0.00532 AFIX 23 H9A 2 0.499990 0.512477 0.687834 11.00000 -1.20000 H9B 2 0.593165 0.542136 0.623898 11.00000 -1.20000 AFIX 0 C10 1 0.601946 0.446892 0.802008 11.00000 0.02769 0.03142 = 0.03044 -0.00981 -0.00268 -0.00159 AFIX 23 H10A 2 0.662284 0.425833 0.780434 11.00000 -1.20000 H10B 2 0.604283 0.503710 0.872231 11.00000 -1.20000 AFIX 0 C11 1 0.553322 0.356263 0.866624 11.00000 0.03429 0.03313 = 0.03081 -0.00564 -0.00261 -0.00603 AFIX 23 H11A 2 0.495395 0.379286 0.899316 11.00000 -1.20000 H11B 2 0.585597 0.330234 0.950463 11.00000 -1.20000 AFIX 0 C12 1 0.542777 0.269873 0.757848 11.00000 0.03018 0.02226 = 0.02738 0.00113 -0.00349 -0.00151 AFIX 23 H12A 2 0.507561 0.214020 0.800372 11.00000 -1.20000 H12B 2 0.600611 0.241251 0.734540 11.00000 -1.20000 AFIX 0 C13 1 0.289805 0.119255 0.401269 11.00000 0.01512 0.01457 = 0.02236 0.00176 0.00174 -0.00020 C14 1 0.266702 0.071165 0.274551 11.00000 0.03832 0.02067 = 0.01503 0.00057 -0.00206 -0.00617 AFIX 43 H14 2 0.267754 0.108497 0.187484 11.00000 -1.20000 AFIX 0 C15 1 0.241991 -0.031956 0.275548 11.00000 0.04899 0.01995 = 0.01942 -0.00594 -0.00358 -0.01308 AFIX 43 H15 2 0.226616 -0.064947 0.188764 11.00000 -1.20000 AFIX 0 C16 1 0.239680 -0.086604 0.401836 11.00000 0.01861 0.01709 = 0.02684 -0.00407 -0.00373 -0.00196 C17 1 0.262288 -0.037808 0.528688 11.00000 0.03345 0.02036 = 0.02263 0.00104 0.00140 -0.00920 AFIX 43 H17 2 0.260671 -0.074893 0.615934 11.00000 -1.20000 AFIX 0 C18 1 0.287180 0.064864 0.528012 11.00000 0.02732 0.02310 = 0.01776 -0.00163 -0.00005 -0.00715 AFIX 43 H18 2 0.302459 0.097885 0.614821 11.00000 -1.20000 AFIX 0 C19 1 0.213360 -0.198485 0.402951 11.00000 0.03384 0.01978 = 0.03202 0.00382 0.00438 -0.00455 AFIX 137 H19A 2 0.157645 -0.206411 0.353763 11.00000 -1.50000 H19B 2 0.207653 -0.222187 0.501692 11.00000 -1.50000 H19C 2 0.257691 -0.239508 0.354122 11.00000 -1.50000 AFIX 0 N1 3 0.430510 0.250179 0.393390 11.00000 0.01034 0.01800 = 0.02176 -0.00150 -0.00559 0.00007 O1 4 0.301244 0.291358 0.535638 11.00000 0.02527 0.02061 = 0.02356 -0.00749 0.00422 -0.00018 O2 4 0.293626 0.294282 0.270537 11.00000 0.01876 0.01874 = 0.03193 0.00581 -0.00384 0.00434 S1 5 0.324864 0.247882 0.400387 11.00000 0.01558 0.01339 = 0.02043 -0.00251 -0.00023 0.00075 CL1 6 0.485511 -0.017014 0.415575 11.00000 0.03025 0.01872 = 0.07443 -0.01196 0.00200 -0.00345 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 2007SRC0763 in Pna2(1) C 0.770 H 0.320 N 0.700 O 0.660 S 1.030 CL 0.990 C1 - C2 C2 - C1 C3 Cl1 C3 - C6 C2 C4 C4 - N1 C7 C3 C5 - C6 N1 C6 - C5 C3 C7 - C4 C12 C8 C8 - C9 C7 C9 - C8 C10 C10 - C11 C9 C11 - C10 C12 C12 - C11 C7 C13 - C18 C14 S1 C14 - C13 C15 C15 - C16 C14 C16 - C15 C17 C19 C17 - C18 C16 C18 - C13 C17 C19 - C16 N1 - C4 C5 S1 O1 - S1 O2 - S1 S1 - O1 O2 N1 C13 Cl1 - C2 Floating origin restraints generated h k l Fo^2 Sigma Why rejected 0 1 -2 21.36 3.19 observed but should be systematically absent 0 1 2 21.94 3.70 observed but should be systematically absent 0 3 2 15.98 3.39 observed but should be systematically absent 0 3 -2 18.88 3.50 observed but should be systematically absent 0 5 -8 13.52 2.76 observed but should be systematically absent 1 0 3 71.51 9.84 observed but should be systematically absent 1 0 3 70.28 7.85 observed but should be systematically absent 1 0 -3 57.07 7.23 observed but should be systematically absent 1 0 -3 86.31 9.43 observed but should be systematically absent 1 0 -5 97.95 12.69 observed but should be systematically absent 1 0 5 62.02 6.10 observed but should be systematically absent 1 0 5 81.43 9.26 observed but should be systematically absent 3 0 1 36.38 4.00 observed but should be systematically absent 3 0 1 41.97 4.24 observed but should be systematically absent 3 0 2 9.03 2.03 observed but should be systematically absent 3 0 3 38.33 4.06 observed but should be systematically absent 3 0 -3 42.67 7.55 observed but should be systematically absent 3 0 -3 37.83 5.50 observed but should be systematically absent 3 0 3 56.33 9.09 observed but should be systematically absent 3 0 5 37.19 6.58 observed but should be systematically absent 3 0 -5 43.70 5.67 observed but should be systematically absent 3 0 5 34.09 5.96 observed but should be systematically absent 5 0 0 13.67 2.84 observed but should be systematically absent 5 0 0 15.29 3.63 observed but should be systematically absent 5 0 1 12.65 2.56 observed but should be systematically absent 5 0 -3 24.10 3.74 observed but should be systematically absent 5 0 3 26.59 5.39 observed but should be systematically absent 5 0 3 23.55 4.75 observed but should be systematically absent 5 0 4 17.70 3.47 observed but should be systematically absent 5 0 5 40.18 4.94 observed but should be systematically absent 5 0 5 30.85 7.03 observed but should be systematically absent 5 0 6 18.16 3.51 observed but should be systematically absent 5 0 6 12.80 3.12 observed but should be systematically absent 7 0 1 12.92 2.99 observed but should be systematically absent 7 0 2 11.97 2.29 observed but should be systematically absent 7 0 3 10.87 2.70 observed but should be systematically absent 7 0 -4 15.91 3.21 observed but should be systematically absent 7 0 4 15.59 3.37 observed but should be systematically absent 7 0 7 26.10 6.38 observed but should be systematically absent 9 0 2 14.21 3.51 observed but should be systematically absent 9 0 4 20.58 4.45 observed but should be systematically absent 11 0 2 12.95 3.05 observed but should be systematically absent 11 0 4 25.53 5.20 observed but should be systematically absent 11 0 -4 35.65 6.81 observed but should be systematically absent 11 0 4 42.81 7.77 observed but should be systematically absent 11 0 6 27.44 5.30 observed but should be systematically absent 11 0 -6 25.28 4.70 observed but should be systematically absent 11136 Reflections read, of which 512 rejected -20 =< h =< 17, -14 =< k =< 17, -12 =< l =< 12, Max. 2-theta = 56.99 47 Systematic absence violations 0 Inconsistent equivalents 4506 Unique reflections, of which 0 suppressed R(int) = 0.0506 R(sigma) = 0.0598 Friedel opposites not merged Maximum memory for data reduction = 2638 / 45209 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 = 3314 / 274629 wR2 = 0.1762 before cycle 1 for 4506 data and 220 / 220 parameters GooF = S = 1.074; Restrained GooF = 1.074 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 4.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.83133 0.00226 -0.015 OSF 2 0.40278 0.12437 0.022 BASF 1 Mean shift/esd = 0.014 Maximum = -0.106 for U33 Cl1 Max. shift = 0.001 A for H19A Max. dU = 0.000 for C15 Least-squares cycle 2 Maximum vector length = 511 Memory required = 3314 / 274629 wR2 = 0.1762 before cycle 2 for 4506 data and 220 / 220 parameters GooF = S = 1.074; Restrained GooF = 1.074 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 4.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.83129 0.00226 -0.015 OSF 2 0.40426 0.12433 0.012 BASF 1 Mean shift/esd = 0.007 Maximum = -0.051 for U33 Cl1 Max. shift = 0.000 A for H19A Max. dU = 0.000 for C15 Least-squares cycle 3 Maximum vector length = 511 Memory required = 3314 / 274629 wR2 = 0.1762 before cycle 3 for 4506 data and 220 / 220 parameters GooF = S = 1.074; Restrained GooF = 1.074 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 4.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.83128 0.00226 -0.003 OSF 2 0.40455 0.12431 0.002 BASF 1 Mean shift/esd = 0.002 Maximum = -0.008 for U33 Cl1 Max. shift = 0.000 A for H19A Max. dU = 0.000 for C15 Least-squares cycle 4 Maximum vector length = 511 Memory required = 3314 / 274629 wR2 = 0.1762 before cycle 4 for 4506 data and 220 / 220 parameters GooF = S = 1.074; Restrained GooF = 1.074 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 4.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.83128 0.00226 -0.001 OSF 2 0.40460 0.12430 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = -0.003 for tors H19A Max. shift = 0.000 A for H19A Max. dU = 0.000 for C5 Least-squares cycle 5 Maximum vector length = 511 Memory required = 3314 / 274629 wR2 = 0.1761 before cycle 5 for 4506 data and 220 / 220 parameters GooF = S = 1.074; Restrained GooF = 1.074 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 4.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.83128 0.00226 0.000 OSF 2 0.40462 0.12430 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = -0.001 for tors H19A Max. shift = 0.000 A for H19A Max. dU = 0.000 for C5 Least-squares cycle 6 Maximum vector length = 511 Memory required = 3314 / 274629 wR2 = 0.1761 before cycle 6 for 4506 data and 220 / 220 parameters GooF = S = 1.074; Restrained GooF = 1.074 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 4.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.83128 0.00226 0.000 OSF 2 0.40462 0.12430 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = -0.001 for tors H19A Max. shift = 0.000 A for H19A Max. dU = 0.000 for C6 Least-squares cycle 7 Maximum vector length = 511 Memory required = 3314 / 274629 wR2 = 0.1761 before cycle 7 for 4506 data and 220 / 220 parameters GooF = S = 1.074; Restrained GooF = 1.074 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 4.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.83128 0.00226 0.000 OSF 2 0.40462 0.12430 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for tors H19A Max. shift = 0.000 A for H19A Max. dU = 0.000 for C13 Least-squares cycle 8 Maximum vector length = 511 Memory required = 3314 / 274629 wR2 = 0.1761 before cycle 8 for 4506 data and 220 / 220 parameters GooF = S = 1.074; Restrained GooF = 1.074 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 4.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.83128 0.00226 0.000 OSF 2 0.40463 0.12430 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for x Cl1 Max. shift = 0.000 A for H19C Max. dU = 0.000 for C1 Least-squares cycle 9 Maximum vector length = 511 Memory required = 3314 / 274629 wR2 = 0.1761 before cycle 9 for 4506 data and 220 / 220 parameters GooF = S = 1.074; Restrained GooF = 1.074 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 4.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.83128 0.00226 0.000 OSF 2 0.40463 0.12430 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for x Cl1 Max. shift = 0.000 A for H19C Max. dU = 0.000 for C2 Least-squares cycle 10 Maximum vector length = 511 Memory required = 3314 / 274629 wR2 = 0.1761 before cycle 10 for 4506 data and 220 / 220 parameters GooF = S = 1.074; Restrained GooF = 1.074 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 4.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.83128 0.00226 0.000 OSF 2 0.40463 0.12430 0.000 BASF 1 Mean shift/esd = 0.000 Maximum = 0.000 for x Cl1 Max. shift = 0.000 A for H19A Max. dU = 0.000 for C6 No correlation matrix elements larger than 0.500 Idealized hydrogen atom generation before cycle 11 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H1A 0.6527 0.0078 0.3115 137 0.980 0.000 C1 C2 H1A H1B 0.6657 -0.0623 0.4503 137 0.980 0.000 C1 C2 H1A H1C 0.7099 0.0490 0.4420 137 0.980 0.000 C1 C2 H1A H2 0.5813 0.0473 0.5878 13 1.000 0.000 C2 C1 C3 Cl1 H3 0.6174 0.2081 0.4925 13 1.000 0.000 C3 C6 C2 C4 H4 0.4516 0.1618 0.5683 13 1.000 0.000 C4 N1 C7 C3 H5A 0.4457 0.1506 0.2216 23 0.990 0.000 C5 C6 N1 H5B 0.4645 0.2689 0.1804 23 0.990 0.000 C5 C6 N1 H6A 0.5973 0.2664 0.2758 23 0.990 0.000 C6 C5 C3 H6B 0.5907 0.1469 0.2320 23 0.990 0.000 C6 C5 C3 H7 0.4406 0.3343 0.6476 13 1.000 0.000 C7 C4 C12 C8 H8A 0.6093 0.3746 0.5289 23 0.990 0.000 C8 C9 C7 H8B 0.5208 0.4238 0.4702 23 0.990 0.000 C8 C9 C7 H9A 0.5000 0.5125 0.6878 23 0.990 0.000 C9 C8 C10 H9B 0.5932 0.5421 0.6239 23 0.990 0.000 C9 C8 C10 H10A 0.6623 0.4258 0.7804 23 0.990 0.000 C10 C11 C9 H10B 0.6043 0.5037 0.8722 23 0.990 0.000 C10 C11 C9 H11A 0.4954 0.3793 0.8993 23 0.990 0.000 C11 C10 C12 H11B 0.5856 0.3302 0.9505 23 0.990 0.000 C11 C10 C12 H12A 0.5076 0.2140 0.8004 23 0.990 0.000 C12 C11 C7 H12B 0.6006 0.2413 0.7345 23 0.990 0.000 C12 C11 C7 H14 0.2678 0.1085 0.1875 43 0.950 0.000 C14 C13 C15 H15 0.2265 -0.0649 0.1888 43 0.950 0.000 C15 C16 C14 H17 0.2607 -0.0749 0.6160 43 0.950 0.000 C17 C18 C16 H18 0.3025 0.0979 0.6148 43 0.950 0.000 C18 C13 C17 H19A 0.1576 -0.2064 0.3539 137 0.980 0.000 C19 C16 H19A H19B 0.2077 -0.2222 0.5017 137 0.980 0.000 C19 C16 H19A H19C 0.2576 -0.2395 0.3540 137 0.980 0.000 C19 C16 H19A 2007SRC0763 in Pna2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.65881 0.00841 0.41551 1.00000 0.02689 0.01814 0.04597 -0.00007 0.00596 0.00487 0.03033 0.00864 0.00026 0.00028 0.00066 0.00000 0.00180 0.00153 0.00276 0.00215 0.00228 0.00136 0.00091 H1A 0.65273 0.00776 0.31152 1.00000 0.04550 0.00000 0.00000 H1B 0.66569 -0.06225 0.45027 1.00000 0.04550 0.00000 0.00000 H1C 0.70993 0.04903 0.44195 1.00000 0.04550 0.00000 0.00000 C2 0.57805 0.05616 0.48208 1.00000 0.02123 0.01593 0.03325 -0.00069 -0.00150 0.00083 0.02347 0.00717 0.00026 0.00030 0.00049 0.00000 0.00188 0.00174 0.00232 0.00150 0.00156 0.00145 0.00084 H2 0.58131 0.04733 0.58785 1.00000 0.02817 0.00000 0.00000 C3 0.56690 0.17150 0.44871 1.00000 0.02362 0.01779 0.02939 0.00054 -0.00010 -0.00012 0.02360 0.00743 0.00026 0.00031 0.00048 0.00000 0.00186 0.00179 0.00219 0.00148 0.00159 0.00138 0.00084 H3 0.61737 0.20810 0.49254 1.00000 0.02832 0.00000 0.00000 C4 0.48315 0.21774 0.51666 1.00000 0.02473 0.01656 0.01807 -0.00073 0.00111 -0.00133 0.01979 0.00697 0.00027 0.00031 0.00044 0.00000 0.00197 0.00174 0.00192 0.00139 0.00161 0.00153 0.00079 H4 0.45158 0.16179 0.56834 1.00000 0.02375 0.00000 0.00000 C5 0.47169 0.21592 0.25534 1.00000 0.02232 0.03072 0.01641 0.00087 0.00484 0.00509 0.02315 0.00790 0.00028 0.00036 0.00045 0.00000 0.00204 0.00216 0.00189 0.00158 0.00152 0.00162 0.00085 H5A 0.44572 0.15061 0.22164 1.00000 0.02778 0.00000 0.00000 H5B 0.46450 0.26893 0.18044 1.00000 0.02778 0.00000 0.00000 C6 0.56467 0.20174 0.29155 1.00000 0.02876 0.03078 0.03552 -0.00285 0.00651 0.00458 0.03169 0.00865 0.00029 0.00038 0.00054 0.00000 0.00234 0.00233 0.00264 0.00194 0.00195 0.00176 0.00100 H6A 0.59730 0.26638 0.27582 1.00000 0.03802 0.00000 0.00000 H6B 0.59067 0.14691 0.23198 1.00000 0.03802 0.00000 0.00000 C7 0.49892 0.30702 0.62011 1.00000 0.02254 0.01588 0.02108 -0.00407 0.00320 -0.00271 0.01983 0.00669 0.00026 0.00029 0.00043 0.00000 0.00182 0.00162 0.00188 0.00138 0.00147 0.00134 0.00074 H7 0.44061 0.33434 0.64762 1.00000 0.02380 0.00000 0.00000 C8 0.55060 0.39821 0.55677 1.00000 0.02741 0.01256 0.03072 -0.00200 -0.00135 -0.00011 0.02356 0.00706 0.00028 0.00028 0.00048 0.00000 0.00201 0.00155 0.00214 0.00150 0.00172 0.00145 0.00080 H8A 0.60927 0.37457 0.52888 1.00000 0.02828 0.00000 0.00000 H8B 0.52084 0.42379 0.47020 1.00000 0.02828 0.00000 0.00000 C9 0.55844 0.48538 0.66518 1.00000 0.02143 0.01901 0.04278 -0.00968 0.00167 -0.00534 0.02774 0.00718 0.00028 0.00032 0.00052 0.00000 0.00207 0.00190 0.00265 0.00172 0.00181 0.00150 0.00094 H9A 0.49999 0.51248 0.68780 1.00000 0.03329 0.00000 0.00000 H9B 0.59317 0.54213 0.62388 1.00000 0.03329 0.00000 0.00000 C10 0.60193 0.44689 0.80200 1.00000 0.02765 0.03143 0.03039 -0.00983 -0.00268 -0.00164 0.02983 0.00753 0.00030 0.00036 0.00049 0.00000 0.00221 0.00224 0.00236 0.00177 0.00178 0.00175 0.00095 H10A 0.66227 0.42584 0.78043 1.00000 0.03579 0.00000 0.00000 H10B 0.60426 0.50371 0.87221 1.00000 0.03579 0.00000 0.00000 C11 0.55331 0.35627 0.86662 1.00000 0.03438 0.03316 0.03076 -0.00562 -0.00258 -0.00610 0.03277 0.00770 0.00032 0.00037 0.00049 0.00000 0.00237 0.00220 0.00272 0.00170 0.00178 0.00183 0.00105 H11A 0.49538 0.37929 0.89931 1.00000 0.03932 0.00000 0.00000 H11B 0.58559 0.33025 0.95046 1.00000 0.03932 0.00000 0.00000 C12 0.54278 0.26987 0.75785 1.00000 0.03023 0.02222 0.02742 0.00116 -0.00351 -0.00151 0.02662 0.00738 0.00030 0.00032 0.00047 0.00000 0.00219 0.00187 0.00212 0.00161 0.00175 0.00161 0.00085 H12A 0.50757 0.21401 0.80037 1.00000 0.03195 0.00000 0.00000 H12B 0.60062 0.24126 0.73454 1.00000 0.03195 0.00000 0.00000 C13 0.28981 0.11925 0.40127 1.00000 0.01514 0.01457 0.02236 0.00181 0.00166 -0.00020 0.01736 0.00672 0.00020 0.00023 0.00054 0.00000 0.00142 0.00130 0.00159 0.00180 0.00172 0.00111 0.00060 C14 0.26670 0.07117 0.27456 1.00000 0.03840 0.02061 0.01507 0.00057 -0.00199 -0.00614 0.02469 0.00740 0.00031 0.00033 0.00045 0.00000 0.00250 0.00197 0.00196 0.00150 0.00178 0.00172 0.00089 H14 0.26778 0.10850 0.18748 1.00000 0.02963 0.00000 0.00000 C15 0.24195 -0.03195 0.27556 1.00000 0.04885 0.01988 0.01947 -0.00592 -0.00361 -0.01303 0.02940 0.00763 0.00034 0.00035 0.00049 0.00000 0.00286 0.00198 0.00210 0.00156 0.00195 0.00185 0.00101 H15 0.22652 -0.06493 0.18879 1.00000 0.03528 0.00000 0.00000 C16 0.23968 -0.08661 0.40185 1.00000 0.01865 0.01711 0.02683 -0.00399 -0.00377 -0.00195 0.02086 0.00648 0.00021 0.00025 0.00053 0.00000 0.00155 0.00143 0.00179 0.00186 0.00196 0.00114 0.00067 C17 0.26231 -0.03782 0.52871 1.00000 0.03334 0.02040 0.02265 0.00100 0.00139 -0.00923 0.02546 0.00769 0.00031 0.00034 0.00049 0.00000 0.00231 0.00192 0.00219 0.00165 0.00175 0.00169 0.00090 H17 0.26072 -0.07492 0.61595 1.00000 0.03056 0.00000 0.00000 C18 0.28719 0.06484 0.52803 1.00000 0.02732 0.02312 0.01781 -0.00160 -0.00004 -0.00714 0.02275 0.00737 0.00028 0.00034 0.00048 0.00000 0.00215 0.00199 0.00201 0.00158 0.00157 0.00157 0.00086 H18 0.30246 0.09787 0.61484 1.00000 0.02730 0.00000 0.00000 C19 0.21335 -0.19848 0.40297 1.00000 0.03380 0.01979 0.03204 0.00387 0.00442 -0.00456 0.02854 0.00815 0.00026 0.00027 0.00064 0.00000 0.00199 0.00157 0.00197 0.00216 0.00223 0.00141 0.00078 H19A 0.15760 -0.20639 0.35391 1.00000 0.04281 0.00000 0.00000 H19B 0.20773 -0.22221 0.50172 1.00000 0.04281 0.00000 0.00000 H19C 0.25764 -0.23950 0.35402 1.00000 0.04281 0.00000 0.00000 N1 0.43052 0.25018 0.39342 1.00000 0.01030 0.01799 0.02184 -0.00149 -0.00565 0.00007 0.01671 0.00614 0.00016 0.00021 0.00054 0.00000 0.00112 0.00115 0.00144 0.00134 0.00150 0.00098 0.00055 O1 0.30125 0.29136 0.53566 1.00000 0.02525 0.02067 0.02359 -0.00744 0.00418 -0.00012 0.02317 0.00535 0.00020 0.00024 0.00034 0.00000 0.00151 0.00147 0.00160 0.00124 0.00124 0.00120 0.00065 O2 0.29362 0.29428 0.27055 1.00000 0.01878 0.01872 0.03185 0.00586 -0.00388 0.00432 0.02312 0.00551 0.00020 0.00023 0.00034 0.00000 0.00142 0.00145 0.00181 0.00126 0.00124 0.00111 0.00066 S1 0.32487 0.24788 0.40037 1.00000 0.01557 0.01338 0.02043 -0.00252 -0.00021 0.00075 0.01646 0.00161 0.00005 0.00006 0.00014 0.00000 0.00035 0.00031 0.00038 0.00038 0.00044 0.00026 0.00018 Cl1 0.48551 -0.01701 0.41558 1.00000 0.03027 0.01872 0.07428 -0.01194 0.00203 -0.00345 0.04109 0.00220 0.00007 0.00007 0.00019 0.00000 0.00049 0.00040 0.00092 0.00061 0.00066 0.00035 0.00033 Final Structure Factor Calculation for 2007SRC0763 in Pna2(1) Total number of l.s. parameters = 220 Maximum vector length = 511 Memory required = 3096 / 27090 wR2 = 0.1761 before cycle 11 for 4506 data and 2 / 220 parameters GooF = S = 1.074; Restrained GooF = 1.074 for 1 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0627 * P )^2 + 4.79 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0699 for 4215 Fo > 4sig(Fo) and 0.0743 for all 4506 data wR2 = 0.1761, GooF = S = 1.074, Restrained GooF = 1.074 for all data Occupancy sum of asymmetric unit = 24.00 for non-hydrogen and 28.00 for hydrogen atoms Principal mean square atomic displacements U 0.0477 0.0275 0.0157 C1 0.0335 0.0212 0.0158 C2 0.0294 0.0236 0.0178 C3 0.0251 0.0180 0.0162 C4 0.0336 0.0223 0.0135 C5 0.0395 0.0340 0.0216 C6 0.0271 0.0189 0.0136 C7 0.0314 0.0270 0.0123 C8 0.0467 0.0235 0.0131 C9 0.0408 0.0288 0.0199 C10 0.0404 0.0349 0.0230 C11 0.0329 0.0250 0.0219 C12 0.0231 0.0151 0.0139 C13 0.0405 0.0187 0.0149 C14 0.0539 0.0243 0.0100 C15 0.0291 0.0199 0.0135 C16 0.0382 0.0229 0.0153 C17 0.0327 0.0191 0.0165 C18 0.0375 0.0314 0.0168 C19 0.0244 0.0177 0.0080 N1 0.0315 0.0240 0.0139 O1 0.0344 0.0229 0.0120 O2 0.0213 0.0157 0.0124 S1 0.0769 0.0307 0.0157 Cl1 Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.034 0.053 0.069 0.086 0.106 0.130 0.161 0.202 0.292 1.000 Number in group 460. 459. 459. 429. 445. 451. 451. 449. 454. 449. GooF 1.329 1.211 1.049 0.971 0.981 0.976 1.092 0.963 1.031 1.064 K 2.212 1.389 1.120 1.058 1.021 1.016 0.998 0.991 1.006 1.013 Resolution(A) 0.74 0.78 0.81 0.84 0.89 0.95 1.02 1.13 1.29 1.62 inf Number in group 469. 437. 452. 448. 458. 437. 455. 448. 452. 450. GooF 0.997 0.897 0.974 0.994 1.019 1.016 1.001 0.975 1.093 1.605 K 1.026 1.028 1.030 1.039 1.027 1.007 1.001 1.009 1.001 1.022 R1 0.124 0.104 0.105 0.095 0.090 0.078 0.061 0.052 0.052 0.061 Recommended weighting scheme: WGHT 0.0590 4.7970 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) 4 0 -4 717.56 316.11 5.86 0.159 2.00 4 0 4 654.34 319.65 4.91 0.160 2.00 2 1 1 1178.95 1895.40 4.71 0.389 5.41 2 1 -1 1213.42 1907.15 4.57 0.390 5.41 17 1 0 317.29 120.90 4.56 0.098 0.90 16 2 0 330.23 122.72 4.52 0.099 0.95 6 0 0 149.15 51.61 4.08 0.064 2.57 1 2 3 468.53 265.17 4.05 0.145 2.77 4 4 4 1369.14 917.87 3.97 0.271 1.70 1 2 -3 468.47 264.71 3.96 0.145 2.77 9 6 3 59.58 11.04 3.92 0.030 1.23 2 1 -5 129.63 44.03 3.79 0.059 1.81 4 9 3 80.93 19.71 3.78 0.040 1.24 4 7 0 36.84 2.68 3.75 0.015 1.67 6 3 2 610.62 944.34 3.74 0.274 2.00 8 1 0 334.37 168.81 3.71 0.116 1.91 4 4 -4 1411.21 912.85 3.69 0.270 1.70 4 3 0 53.89 10.39 3.65 0.029 2.88 4 4 2 164.72 76.67 3.48 0.078 2.19 2 1 5 112.95 42.68 3.45 0.058 1.81 3 4 -2 47.41 132.58 3.45 0.103 2.37 2 3 5 65.30 15.90 3.44 0.036 1.68 19 1 0 202.14 81.92 3.44 0.081 0.81 5 4 -4 87.13 25.69 3.42 0.045 1.62 3 4 -5 811.51 554.45 3.27 0.210 1.55 4 4 -2 160.18 75.48 3.23 0.078 2.19 3 4 2 52.29 132.98 3.23 0.103 2.37 16 2 4 313.84 152.56 3.21 0.110 0.88 6 3 -2 647.88 940.04 3.19 0.274 2.00 5 5 -7 73.73 163.90 3.16 0.114 1.11 2 0 2 1277.28 906.23 3.15 0.269 4.01 4 0 1 4922.81 6561.07 3.14 0.723 3.56 17 3 0 171.07 50.76 3.12 0.064 0.89 16 11 0 165.34 311.58 3.11 0.158 0.75 15 6 3 76.23 168.91 3.10 0.116 0.89 6 4 -10 435.10 253.50 3.10 0.142 0.85 7 2 -4 117.10 47.94 3.07 0.062 1.56 5 16 0 45.61 2.25 3.07 0.013 0.79 1 1 4 1660.34 2210.88 3.07 0.420 2.28 7 1 -9 34.57 103.50 3.04 0.091 0.94 17 9 2 37.90 1.68 3.04 0.012 0.76 9 6 -3 53.18 10.57 3.04 0.029 1.23 8 1 2 91.11 36.30 3.00 0.054 1.77 18 2 0 80.97 21.96 2.99 0.042 0.85 1 1 -4 1668.22 2199.33 2.96 0.419 2.28 8 1 -2 89.31 35.32 2.95 0.053 1.77 12 3 -4 87.24 34.39 2.95 0.052 1.09 14 10 -5 43.39 2.03 2.93 0.013 0.77 5 2 0 15.92 0.06 2.93 0.002 2.78 1 12 -3 52.72 10.82 2.93 0.029 1.02 Bond lengths and angles C1 - Distance Angles C2 1.5241 (0.0057) H1A 0.9800 109.47 H1B 0.9800 109.47 109.47 H1C 0.9800 109.47 109.47 109.47 C1 - C2 H1A H1B C2 - Distance Angles C1 1.5241 (0.0057) C3 1.5405 (0.0055) 113.81 (0.34) Cl1 1.8237 (0.0042) 106.62 (0.29) 110.51 (0.28) H2 1.0000 108.59 108.59 108.59 C2 - C1 C3 Cl1 C3 - Distance Angles C6 1.5260 (0.0071) C2 1.5405 (0.0055) 116.69 (0.36) C4 1.5596 (0.0057) 106.08 (0.34) 112.58 (0.34) H3 1.0000 106.99 106.99 106.99 C3 - C6 C2 C4 C4 - Distance Angles N1 1.4736 (0.0057) C7 1.5317 (0.0054) 111.57 (0.32) C3 1.5596 (0.0057) 104.17 (0.33) 114.79 (0.34) H4 1.0000 108.70 108.70 108.70 C4 - N1 C7 C3 C5 - Distance Angles C6 1.4837 (0.0062) N1 1.5093 (0.0059) 104.24 (0.34) H5A 0.9900 110.91 110.91 H5B 0.9900 110.91 110.91 108.93 C5 - C6 N1 H5A C6 - Distance Angles C5 1.4837 (0.0062) C3 1.5260 (0.0071) 105.95 (0.37) H6A 0.9900 110.54 110.54 H6B 0.9900 110.54 110.54 108.70 C6 - C5 C3 H6A C7 - Distance Angles C4 1.5317 (0.0054) C12 1.5358 (0.0058) 111.39 (0.33) C8 1.5462 (0.0053) 114.75 (0.34) 109.72 (0.34) H7 1.0000 106.84 106.84 106.84 C7 - C4 C12 C8 C8 - Distance Angles C9 1.5268 (0.0055) C7 1.5462 (0.0053) 110.69 (0.35) H8A 0.9900 109.51 109.51 H8B 0.9900 109.51 109.51 108.08 C8 - C9 C7 H8A C9 - Distance Angles C8 1.5268 (0.0055) C10 1.5316 (0.0068) 110.52 (0.35) H9A 0.9900 109.55 109.55 H9B 0.9900 109.55 109.55 108.10 C9 - C8 C10 H9A C10 - Distance Angles C11 1.5215 (0.0065) C9 1.5316 (0.0068) 111.78 (0.37) H10A 0.9900 109.26 109.26 H10B 0.9900 109.26 109.26 107.93 C10 - C11 C9 H10A C11 - Distance Angles C10 1.5215 (0.0065) C12 1.5256 (0.0060) 110.81 (0.37) H11A 0.9900 109.48 109.48 H11B 0.9900 109.48 109.48 108.06 C11 - C10 C12 H11A C12 - Distance Angles C11 1.5256 (0.0060) C7 1.5358 (0.0058) 112.22 (0.35) H12A 0.9900 109.16 109.16 H12B 0.9900 109.16 109.16 107.88 C12 - C11 C7 H12A C13 - Distance Angles C18 1.3839 (0.0060) C14 1.3891 (0.0058) 119.86 (0.30) S1 1.7563 (0.0031) 119.94 (0.33) 120.17 (0.34) C13 - C18 C14 C14 - Distance Angles C13 1.3891 (0.0058) C15 1.3931 (0.0060) 119.79 (0.38) H14 0.9500 120.10 120.10 C14 - C13 C15 C15 - Distance Angles C16 1.3815 (0.0067) C14 1.3931 (0.0060) 120.47 (0.38) H15 0.9500 119.77 119.77 C15 - C16 C14 C16 - Distance Angles C15 1.3815 (0.0067) C17 1.3926 (0.0061) 119.50 (0.31) C19 1.5091 (0.0045) 120.52 (0.42) 119.98 (0.43) C16 - C15 C17 C17 - Distance Angles C18 1.3878 (0.0059) C16 1.3926 (0.0061) 120.18 (0.41) H17 0.9500 119.91 119.91 C17 - C18 C16 C18 - Distance Angles C13 1.3839 (0.0060) C17 1.3878 (0.0059) 120.20 (0.39) H18 0.9500 119.90 119.90 C18 - C13 C17 C19 - Distance Angles C16 1.5091 (0.0045) H19A 0.9800 109.47 H19B 0.9800 109.47 109.47 H19C 0.9800 109.47 109.47 109.47 C19 - C16 H19A H19B N1 - Distance Angles C4 1.4736 (0.0057) C5 1.5093 (0.0059) 110.95 (0.28) S1 1.6294 (0.0026) 120.87 (0.33) 116.67 (0.30) N1 - C4 C5 O1 - Distance Angles S1 1.4360 (0.0033) O1 - O2 - Distance Angles S1 1.4415 (0.0032) O2 - S1 - Distance Angles O1 1.4360 (0.0033) O2 1.4415 (0.0032) 119.83 (0.15) N1 1.6294 (0.0026) 106.34 (0.21) 106.99 (0.21) C13 1.7563 (0.0031) 106.99 (0.21) 107.42 (0.21) 108.96 (0.15) S1 - O1 O2 N1 Cl1 - Distance Angles C2 1.8237 (0.0042) Cl1 - FMAP and GRID set by program FMAP 2 1 20 GRID -1.471 -2 -2 1.471 2 2 R1 = 0.0730 for 2512 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 1.19 at 0.0251 0.4748 0.7991 [ 1.11 A from CL1 ] Deepest hole -0.77 at 0.0009 0.5151 0.3576 [ 0.59 A from CL1 ] Mean = 0.00, Rms deviation from mean = 0.10 e/A^3, Highest memory used = 3110 / 22423 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.4749 -0.0252 0.2991 1.00000 0.05 1.19 1.11 CL1 2.18 H2 2.44 H5A 2.47 H12A Q2 1 0.4763 -0.0239 0.5138 1.00000 0.05 1.04 0.94 CL1 1.90 C2 1.99 H2 2.50 H4 Q3 1 0.4569 0.6066 0.7473 1.00000 0.05 0.60 1.50 H9A 1.87 H6A 2.12 H5B 2.16 H8B Q4 1 0.5717 0.0541 0.3081 1.00000 0.05 0.46 1.39 H1A 1.43 H6B 1.64 C2 1.78 C1 Q5 1 0.6080 0.4243 0.9921 1.00000 0.05 0.43 1.33 H11B 1.53 H10B 1.70 C11 1.81 C10 Q6 1 0.5300 0.1441 0.3020 1.00000 0.05 0.43 0.92 C6 1.14 H6B 1.37 C5 1.50 H5A Q7 1 0.3114 0.2782 0.4533 1.00000 0.05 0.42 0.67 S1 0.81 O1 1.75 O2 1.95 N1 Q8 1 0.4717 0.2665 0.2333 1.00000 0.05 0.41 0.51 H5B 0.69 C5 1.56 H5A 1.64 N1 Q9 1 0.5592 0.1484 0.3429 1.00000 0.05 0.41 0.85 C6 1.04 C3 1.15 H6B 1.76 H6A Q10 1 0.5352 0.2554 1.0365 1.00000 0.05 0.40 1.48 H11B 1.74 H5B 2.08 C11 2.15 H11A Shortest distances between peaks (including symmetry equivalents) 6 9 0.59 4 9 1.28 4 6 1.33 1 4 1.81 6 8 1.94 3 8 1.99 1 2 2.01 8 10 2.09 8 9 2.29 1 6 2.36 5 10 2.50 3 5 2.62 2 4 2.63 1 9 2.64 3 10 2.67 1 2 2.85 6 10 2.88 2 4 2.88 Time profile in seconds ----------------------- 0.09: 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 0.02: Analyse other restraints etc. 1.72: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.00: OSF, H-atoms from difference map 0.05: Set up l.s. refinement 0.00: Generate idealized H-atoms 11.52: Structure factors and derivatives 4.64: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.03: Apply other restraints 0.75: Solve l.s. equations 0.00: Generate HTAB table 0.06: Other dependent quantities, CIF, tables 0.11: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.09: Fourier summations 0.06: Peaksearch 0.02: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2007src0763 finished at 17:33:02 Total CPU time: 19.2 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++